file_name stringlengths 11 11 | content stringlengths 1.16k 56.6M |
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1100793.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100793.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100793
loop_
_publ_author_name
'Tomlinson, Susan'
'Zheng, Chong'
'Hosmane, Narayan S.'
'Yang, Jimin'
'Wang, Ying'
'Zhang, Hongming'
'Gray, Thomas G.'
'Demissie, Temesgen'
'Maguire, John A.'
'Baumann, Frank'
'Klein, Axel'
'Sarkar, Biprajit'
'Kaim, Wolfgang'
'Lipscomb, William N.'
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural,
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2177
_journal_page_last 2187
_journal_paper_doi 10.1021/om048982u
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C22 H60 B8 Fe2 N2 Si4'
_chemical_formula_weight 663.26
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 92.06(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.574(1)
_cell_length_b 16.472(1)
_cell_length_c 18.363(2)
_cell_measurement_reflns_used 39
_cell_measurement_temperature 228(2)
_cell_measurement_theta_max 10.0
_cell_measurement_theta_min 5.0
_cell_volume 3800.9(6)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 228(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.026
_diffrn_reflns_av_sigmaI/netI 0.041
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 4887
_diffrn_reflns_theta_full 22.00
_diffrn_reflns_theta_max 22.00
_diffrn_reflns_theta_min 2.04
_diffrn_standards_decay_% 3.26
_diffrn_standards_interval_count 147
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.905
_exptl_absorpt_correction_T_max 0.876
_exptl_absorpt_correction_T_min 0.742
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Siemens XEMP'
_exptl_crystal_colour dark-green
_exptl_crystal_density_diffrn 1.159
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.286
_refine_diff_density_min -0.250
_refine_diff_density_rms 0.057
_refine_ls_extinction_coef 0.00142(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 360
_refine_ls_number_reflns 4635
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.051
_refine_ls_R_factor_gt 0.037
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+5.7999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.084
_refine_ls_wR_factor_ref 0.090
_reflns_number_gt 3807
_reflns_number_total 4635
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060287
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100793
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.73819(4) 0.94669(3) 0.19113(3) 0.02561(16) Uani 1 1 d . . .
Fe2 Fe 0.73834(4) 1.01867(3) 0.06237(3) 0.02873(17) Uani 1 1 d . . .
Si1 Si 0.82445(10) 0.73621(8) 0.15495(6) 0.0458(3) Uani 1 1 d . . .
Si2 Si 0.93747(10) 0.84823(9) 0.33074(7) 0.0534(4) Uani 1 1 d . . .
Si3 Si 0.67281(10) 1.09418(8) 0.32953(6) 0.0429(3) Uani 1 1 d . . .
Si4 Si 0.53339(10) 0.87922(8) 0.33203(7) 0.0465(3) Uani 1 1 d . . .
C1 C 0.8377(3) 0.8472(2) 0.1787(2) 0.0333(9) Uani 1 1 d . . .
C2 C 0.8742(3) 0.8929(2) 0.2452(2) 0.0343(10) Uani 1 1 d . . .
B3 B 0.8930(3) 0.9853(3) 0.2282(3) 0.0385(12) Uani 1 1 d . . .
H3 H 0.9193 1.0326 0.2672 0.046 Uiso 1 1 calc R . .
B4 B 0.8773(3) 0.9943(3) 0.1384(2) 0.0320(11) Uani 1 1 d . . .
H4 H 0.8964 1.0524 0.1059 0.038 Uiso 1 1 d . . .
B5 B 0.8373(3) 0.9021(3) 0.1086(2) 0.0323(11) Uani 1 1 d . . .
H5 H 0.8288 0.8761 0.0513 0.039 Uiso 1 1 d . . .
B6 B 0.9490(4) 0.9101(3) 0.1697(2) 0.0399(12) Uani 1 1 d . . .
H6 H 1.0328 0.8963 0.1597 0.048 Uiso 1 1 calc R . .
C11 C 0.6462(3) 1.0196(2) 0.25416(19) 0.0283(9) Uani 1 1 d . . .
C12 C 0.6020(3) 0.9356(2) 0.25715(19) 0.0291(9) Uani 1 1 d . . .
B13 B 0.5763(3) 0.9000(3) 0.1794(2) 0.0312(10) Uani 1 1 d . . .
H13 H 0.5436 0.8396 0.1662 0.037 Uiso 1 1 calc R . .
B14 B 0.5979(3) 0.9752(3) 0.1215(2) 0.0298(10) Uani 1 1 d . . .
H14 H 0.5756 0.9740 0.0590 0.036 Uiso 1 1 d . . .
B15 B 0.6466(3) 1.0525(3) 0.1732(2) 0.0320(10) Uani 1 1 d . . .
H15 H 0.6609 1.1222 0.1599 0.038 Uiso 1 1 d . . .
B16 B 0.5314(3) 1.0012(3) 0.2005(2) 0.0338(11) Uani 1 1 d . . .
H16 H 0.4500 1.0253 0.2034 0.041 Uiso 1 1 calc R . .
C21 C 0.7110(4) 0.7248(3) 0.0879(2) 0.0565(13) Uani 1 1 d . . .
H21A H 0.6956 0.6682 0.0809 0.085 Uiso 1 1 calc R . .
H21B H 0.7293 0.7486 0.0423 0.085 Uiso 1 1 calc R . .
H21C H 0.6495 0.7517 0.1059 0.085 Uiso 1 1 calc R . .
C22 C 0.9490(4) 0.7033(3) 0.1102(3) 0.0717(16) Uani 1 1 d . . .
H22A H 0.9424 0.6474 0.0957 0.108 Uiso 1 1 calc R . .
H22B H 1.0087 0.7092 0.1438 0.108 Uiso 1 1 calc R . .
H22C H 0.9597 0.7363 0.0680 0.108 Uiso 1 1 calc R . .
C23 C 0.7989(5) 0.6648(3) 0.2314(3) 0.0840(19) Uani 1 1 d . . .
H23A H 0.7294 0.6748 0.2494 0.126 Uiso 1 1 calc R . .
H23B H 0.8514 0.6730 0.2700 0.126 Uiso 1 1 calc R . .
H23C H 0.8028 0.6099 0.2142 0.126 Uiso 1 1 calc R . .
C24 C 1.0350(5) 0.7689(4) 0.3037(3) 0.103(2) Uani 1 1 d . . .
H24A H 1.0656 0.7435 0.3466 0.154 Uiso 1 1 calc R . .
H24B H 1.0903 0.7937 0.2767 0.154 Uiso 1 1 calc R . .
H24C H 0.9991 0.7287 0.2739 0.154 Uiso 1 1 calc R . .
C25 C 1.0167(4) 0.9260(4) 0.3826(3) 0.093(2) Uani 1 1 d . . .
H25A H 0.9708 0.9695 0.3964 0.140 Uiso 1 1 calc R . .
H25B H 1.0712 0.9469 0.3525 0.140 Uiso 1 1 calc R . .
H25C H 1.0488 0.9017 0.4255 0.140 Uiso 1 1 calc R . .
C26 C 0.8404(4) 0.8038(3) 0.3935(3) 0.0764(17) Uani 1 1 d . . .
H26A H 0.8781 0.7778 0.4335 0.115 Uiso 1 1 calc R . .
H26B H 0.7970 0.7645 0.3677 0.115 Uiso 1 1 calc R . .
H26C H 0.7960 0.8460 0.4117 0.115 Uiso 1 1 calc R . .
C27 C 0.7616(4) 1.0531(4) 0.4045(3) 0.0732(16) Uani 1 1 d . . .
H27A H 0.8346 1.0617 0.3929 0.110 Uiso 1 1 calc R . .
H27B H 0.7488 0.9961 0.4100 0.110 Uiso 1 1 calc R . .
H27C H 0.7471 1.0806 0.4492 0.110 Uiso 1 1 calc R . .
C28 C 0.7431(4) 1.1834(3) 0.2917(3) 0.0687(15) Uani 1 1 d . . .
H28A H 0.7731 1.2155 0.3309 0.103 Uiso 1 1 calc R . .
H28B H 0.6936 1.2157 0.2632 0.103 Uiso 1 1 calc R . .
H28C H 0.7989 1.1649 0.2614 0.103 Uiso 1 1 calc R . .
C29 C 0.5419(4) 1.1282(3) 0.3645(3) 0.0623(14) Uani 1 1 d . . .
H29A H 0.5540 1.1664 0.4034 0.093 Uiso 1 1 calc R . .
H29B H 0.5040 1.0821 0.3823 0.093 Uiso 1 1 calc R . .
H29C H 0.5007 1.1534 0.3258 0.093 Uiso 1 1 calc R . .
C30 C 0.5579(4) 0.7682(3) 0.3211(3) 0.0731(16) Uani 1 1 d . . .
H30A H 0.6259 0.7601 0.3001 0.110 Uiso 1 1 calc R . .
H30B H 0.5032 0.7453 0.2896 0.110 Uiso 1 1 calc R . .
H30C H 0.5571 0.7422 0.3678 0.110 Uiso 1 1 calc R . .
C31 C 0.5664(5) 0.9068(4) 0.4288(2) 0.0773(17) Uani 1 1 d . . .
H31A H 0.5263 0.8732 0.4605 0.116 Uiso 1 1 calc R . .
H31B H 0.5489 0.9628 0.4367 0.116 Uiso 1 1 calc R . .
H31C H 0.6411 0.8987 0.4390 0.116 Uiso 1 1 calc R . .
C32 C 0.3870(4) 0.8982(4) 0.3185(3) 0.0774(17) Uani 1 1 d . . .
H32A H 0.3486 0.8645 0.3512 0.116 Uiso 1 1 calc R . .
H32B H 0.3653 0.8857 0.2691 0.116 Uiso 1 1 calc R . .
H32C H 0.3721 0.9542 0.3283 0.116 Uiso 1 1 calc R . .
N41 N 0.7552(2) 0.98390(19) -0.05319(15) 0.0319(7) Uani 1 1 d . . .
N42 N 0.7149(3) 1.14032(19) 0.01132(16) 0.0359(8) Uani 1 1 d . . .
C43 C 0.7157(3) 1.0542(3) -0.0969(2) 0.0422(11) Uani 1 1 d . . .
H43A H 0.6385 1.0533 -0.0998 0.051 Uiso 1 1 calc R . .
H43B H 0.7411 1.0501 -0.1460 0.051 Uiso 1 1 calc R . .
C44 C 0.7526(4) 1.1323(3) -0.0636(2) 0.0484(11) Uani 1 1 d . . .
H44A H 0.8297 1.1343 -0.0626 0.058 Uiso 1 1 calc R . .
H44B H 0.7259 1.1772 -0.0931 0.058 Uiso 1 1 calc R . .
C45 C 0.8678(3) 0.9676(3) -0.0701(2) 0.0475(12) Uani 1 1 d . . .
H45A H 0.8922 0.9202 -0.0442 0.071 Uiso 1 1 calc R . .
H45B H 0.9109 1.0133 -0.0556 0.071 Uiso 1 1 calc R . .
H45C H 0.8730 0.9588 -0.1216 0.071 Uiso 1 1 calc R . .
C46 C 0.6909(3) 0.9123(3) -0.0739(2) 0.0431(11) Uani 1 1 d . . .
H46A H 0.6172 0.9233 -0.0660 0.065 Uiso 1 1 calc R . .
H46B H 0.7137 0.8666 -0.0448 0.065 Uiso 1 1 calc R . .
H46C H 0.6999 0.9002 -0.1245 0.065 Uiso 1 1 calc R . .
C47 C 0.7772(4) 1.2051(3) 0.0490(3) 0.0586(13) Uani 1 1 d . . .
H47A H 0.8514 1.1915 0.0494 0.088 Uiso 1 1 calc R . .
H47B H 0.7546 1.2102 0.0982 0.088 Uiso 1 1 calc R . .
H47C H 0.7659 1.2556 0.0239 0.088 Uiso 1 1 calc R . .
C48 C 0.6012(3) 1.1646(3) 0.0090(2) 0.0492(12) Uani 1 1 d . . .
H48A H 0.5937 1.2167 -0.0141 0.074 Uiso 1 1 calc R . .
H48B H 0.5763 1.1677 0.0577 0.074 Uiso 1 1 calc R . .
H48C H 0.5601 1.1251 -0.0183 0.074 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0226(3) 0.0321(3) 0.0222(3) 0.0028(2) 0.0015(2) 0.0005(2)
Fe2 0.0287(3) 0.0350(3) 0.0226(3) 0.0051(2) 0.0022(2) -0.0001(2)
Si1 0.0610(8) 0.0385(7) 0.0388(7) 0.0045(6) 0.0128(6) 0.0109(6)
Si2 0.0478(7) 0.0786(10) 0.0332(7) 0.0123(7) -0.0065(6) 0.0197(7)
Si3 0.0456(7) 0.0488(8) 0.0346(6) -0.0133(6) 0.0035(5) -0.0010(6)
Si4 0.0465(7) 0.0547(8) 0.0394(7) 0.0154(6) 0.0154(6) -0.0008(6)
C1 0.028(2) 0.043(3) 0.030(2) 0.0082(19) 0.0049(17) 0.0081(18)
C2 0.028(2) 0.048(3) 0.027(2) 0.0047(19) 0.0016(17) 0.0069(19)
B3 0.024(2) 0.056(3) 0.036(3) 0.002(2) -0.002(2) -0.004(2)
B4 0.021(2) 0.041(3) 0.035(3) 0.011(2) 0.0057(19) -0.001(2)
B5 0.028(2) 0.044(3) 0.025(2) 0.006(2) 0.0057(19) 0.008(2)
B6 0.029(3) 0.060(3) 0.031(3) 0.011(2) 0.003(2) -0.001(2)
C11 0.0225(19) 0.033(2) 0.029(2) 0.0016(18) 0.0007(16) 0.0027(17)
C12 0.024(2) 0.036(2) 0.027(2) 0.0052(18) 0.0038(16) 0.0004(17)
B13 0.026(2) 0.034(3) 0.033(3) -0.002(2) 0.0027(19) 0.000(2)
B14 0.024(2) 0.043(3) 0.023(2) -0.001(2) -0.0012(18) 0.003(2)
B15 0.026(2) 0.039(3) 0.031(2) 0.001(2) 0.0049(19) 0.003(2)
B16 0.026(2) 0.046(3) 0.030(2) 0.002(2) -0.001(2) 0.003(2)
C21 0.062(3) 0.050(3) 0.058(3) -0.014(2) 0.015(2) -0.006(2)
C22 0.082(4) 0.073(4) 0.060(3) -0.008(3) 0.008(3) 0.033(3)
C23 0.149(6) 0.044(3) 0.061(3) 0.012(3) 0.026(4) 0.010(3)
C24 0.092(4) 0.153(6) 0.062(4) 0.015(4) -0.014(3) 0.078(4)
C25 0.074(4) 0.133(6) 0.069(4) 0.013(4) -0.038(3) 0.003(4)
C26 0.094(4) 0.091(4) 0.044(3) 0.027(3) 0.004(3) 0.007(3)
C27 0.073(4) 0.100(4) 0.046(3) -0.016(3) -0.009(3) 0.001(3)
C28 0.077(4) 0.054(3) 0.076(4) -0.025(3) 0.010(3) -0.019(3)
C29 0.071(3) 0.068(4) 0.049(3) -0.015(3) 0.016(3) 0.009(3)
C30 0.095(4) 0.056(3) 0.070(4) 0.026(3) 0.012(3) -0.014(3)
C31 0.098(4) 0.092(4) 0.043(3) 0.019(3) 0.023(3) 0.012(4)
C32 0.050(3) 0.103(5) 0.082(4) 0.035(3) 0.032(3) -0.005(3)
N41 0.0323(18) 0.0380(19) 0.0255(17) 0.0033(15) 0.0028(14) -0.0020(15)
N42 0.044(2) 0.0311(19) 0.0325(19) 0.0019(15) -0.0021(15) -0.0062(16)
C43 0.048(3) 0.051(3) 0.028(2) 0.005(2) -0.0020(19) -0.001(2)
C44 0.060(3) 0.049(3) 0.037(2) 0.014(2) 0.005(2) -0.007(2)
C45 0.036(2) 0.075(3) 0.033(2) 0.004(2) 0.0116(19) 0.000(2)
C46 0.050(3) 0.048(3) 0.031(2) -0.009(2) 0.001(2) -0.004(2)
C47 0.080(4) 0.040(3) 0.055(3) 0.000(2) -0.006(3) -0.020(3)
C48 0.059(3) 0.039(3) 0.049(3) 0.012(2) 0.002(2) 0.012(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt1 Fe1 Cnt2 174.4 . . y
C11 Fe1 C1 151.20(14) . . ?
C11 Fe1 B15 44.70(15) . . ?
C1 Fe1 B15 164.09(15) . . ?
C11 Fe1 B5 163.73(16) . . ?
C1 Fe1 B5 43.87(15) . . ?
B15 Fe1 B5 120.32(17) . . ?
C11 Fe1 B3 99.86(17) . . ?
C1 Fe1 B3 74.02(18) . . ?
B15 Fe1 B3 106.86(19) . . ?
B5 Fe1 B3 77.25(18) . . ?
C11 Fe1 C2 115.93(14) . . ?
C1 Fe1 C2 41.47(14) . . ?
B15 Fe1 C2 146.93(17) . . ?
B5 Fe1 C2 73.07(15) . . ?
B3 Fe1 C2 43.18(17) . . ?
C11 Fe1 C12 41.64(14) . . ?
C1 Fe1 C12 119.44(15) . . ?
B15 Fe1 C12 73.49(15) . . ?
B5 Fe1 C12 151.02(17) . . ?
B3 Fe1 C12 125.66(16) . . ?
C2 Fe1 C12 110.11(14) . . ?
C11 Fe1 B4 121.21(16) . . ?
C1 Fe1 B4 74.83(16) . . ?
B15 Fe1 B4 94.35(17) . . ?
B5 Fe1 B4 46.09(18) . . ?
B3 Fe1 B4 45.28(17) . . ?
C2 Fe1 B4 73.35(15) . . ?
C12 Fe1 B4 162.72(16) . . ?
C11 Fe1 B13 73.70(16) . . ?
C1 Fe1 B13 105.92(16) . . ?
B15 Fe1 B13 76.92(17) . . ?
B5 Fe1 B13 112.13(17) . . ?
B3 Fe1 B13 166.86(17) . . ?
C2 Fe1 B13 128.91(16) . . ?
C12 Fe1 B13 42.51(15) . . ?
B4 Fe1 B13 147.81(16) . . ?
C11 Fe1 B14 75.29(15) . . ?
C1 Fe1 B14 125.39(16) . . ?
B15 Fe1 B14 46.24(17) . . ?
B5 Fe1 B14 97.94(16) . . ?
B3 Fe1 B14 145.82(18) . . ?
C2 Fe1 B14 166.64(16) . . ?
C12 Fe1 B14 72.88(14) . . ?
B4 Fe1 B14 107.85(16) . . ?
B13 Fe1 B14 44.67(16) . . ?
C11 Fe1 Fe2 105.09(10) . . ?
C1 Fe1 Fe2 103.59(10) . . ?
B15 Fe1 Fe2 60.50(12) . . ?
B5 Fe1 Fe2 59.92(12) . . ?
B3 Fe1 Fe2 96.99(13) . . ?
C2 Fe1 Fe2 125.08(10) . . ?
C12 Fe1 Fe2 124.80(10) . . ?
B4 Fe1 Fe2 54.16(11) . . ?
B13 Fe1 Fe2 95.77(11) . . ?
B14 Fe1 Fe2 53.77(11) . . ?
N41 Fe2 B14 119.27(13) . . ?
N41 Fe2 N42 81.10(11) . . ?
B14 Fe2 N42 113.55(14) . . ?
N41 Fe2 B4 116.94(14) . . ?
B14 Fe2 B4 104.71(15) . . ?
N42 Fe2 B4 120.91(14) . . ?
N41 Fe2 B5 93.73(13) . . ?
B14 Fe2 B5 88.90(15) . . ?
N42 Fe2 B5 156.66(14) . . ?
B4 Fe2 B5 42.15(16) . . ?
N41 Fe2 B15 157.28(13) . . ?
B14 Fe2 B15 42.19(15) . . ?
N42 Fe2 B15 94.95(14) . . ?
B4 Fe2 B15 84.37(15) . . ?
B5 Fe2 B15 98.10(14) . . ?
N41 Fe2 Fe1 138.03(9) . . ?
B14 Fe2 Fe1 52.66(11) . . ?
N42 Fe2 Fe1 140.81(8) . . ?
B4 Fe2 Fe1 52.13(11) . . ?
B5 Fe2 Fe1 49.39(10) . . ?
B15 Fe2 Fe1 48.78(11) . . ?
C21 Si1 C23 106.6(3) . . ?
C21 Si1 C22 108.3(2) . . ?
C23 Si1 C22 108.4(3) . . ?
C21 Si1 C1 108.05(19) . . ?
C23 Si1 C1 116.9(2) . . ?
C22 Si1 C1 108.3(2) . . ?
C26 Si2 C25 107.7(3) . . ?
C26 Si2 C24 109.9(3) . . ?
C25 Si2 C24 105.8(3) . . ?
C26 Si2 C2 113.8(2) . . ?
C25 Si2 C2 111.0(2) . . ?
C24 Si2 C2 108.2(2) . . ?
C28 Si3 C27 106.4(3) . . ?
C28 Si3 C11 108.44(19) . . ?
C27 Si3 C11 113.2(2) . . ?
C28 Si3 C29 109.1(2) . . ?
C27 Si3 C29 111.4(2) . . ?
C11 Si3 C29 108.29(19) . . ?
C30 Si4 C31 108.0(2) . . ?
C30 Si4 C32 108.3(3) . . ?
C31 Si4 C32 105.6(3) . . ?
C30 Si4 C12 108.7(2) . . ?
C31 Si4 C12 118.7(2) . . ?
C32 Si4 C12 107.03(19) . . ?
C2 C1 B5 111.8(3) . . ?
C2 C1 B6 63.7(3) . . ?
B5 C1 B6 64.0(3) . . ?
C2 C1 Si1 134.4(3) . . ?
B5 C1 Si1 111.8(3) . . ?
B6 C1 Si1 128.0(3) . . ?
C2 C1 Fe1 71.4(2) . . ?
B5 C1 Fe1 69.7(2) . . ?
B6 C1 Fe1 91.7(2) . . ?
Si1 C1 Fe1 137.8(2) . . ?
C1 C2 B3 111.7(3) . . ?
C1 C2 B6 65.5(3) . . ?
B3 C2 B6 65.9(3) . . ?
C1 C2 Si2 126.4(3) . . ?
B3 C2 Si2 118.8(3) . . ?
B6 C2 Si2 120.5(3) . . ?
C1 C2 Fe1 67.14(19) . . ?
B3 C2 Fe1 68.3(2) . . ?
B6 C2 Fe1 90.5(2) . . ?
Si2 C2 Fe1 148.8(2) . . ?
C2 B3 B4 105.7(4) . . ?
C2 B3 B6 61.2(3) . . ?
B4 B3 B6 60.2(3) . . ?
C2 B3 Fe1 68.5(2) . . ?
B4 B3 Fe1 68.6(2) . . ?
B6 B3 Fe1 88.6(3) . . ?
B3 B4 B5 105.4(3) . . ?
B3 B4 B6 63.9(3) . . ?
B5 B4 B6 62.2(3) . . ?
B3 B4 Fe1 66.1(2) . . ?
B5 B4 Fe1 65.5(2) . . ?
B6 B4 Fe1 89.0(2) . . ?
B3 B4 Fe2 134.4(3) . . ?
B5 B4 Fe2 75.0(2) . . ?
B6 B4 Fe2 137.2(3) . . ?
Fe1 B4 Fe2 73.71(13) . . ?
C1 B5 B4 105.1(3) . . ?
C1 B5 B6 63.0(3) . . ?
B4 B5 B6 60.4(3) . . ?
C1 B5 Fe1 66.4(2) . . ?
B4 B5 Fe1 68.4(2) . . ?
B6 B5 Fe1 89.7(2) . . ?
C1 B5 Fe2 136.7(3) . . ?
B4 B5 Fe2 62.8(2) . . ?
B6 B5 Fe2 123.2(3) . . ?
Fe1 B5 Fe2 70.69(13) . . ?
C2 B6 B4 96.0(3) . . ?
C2 B6 C1 50.8(2) . . ?
B4 B6 C1 95.5(3) . . ?
C2 B6 B5 93.1(3) . . ?
B4 B6 B5 57.4(3) . . ?
C1 B6 B5 53.0(2) . . ?
C2 B6 B3 52.9(2) . . ?
B4 B6 B3 55.9(3) . . ?
C1 B6 B3 91.1(3) . . ?
B5 B6 B3 96.4(3) . . ?
C12 C11 B15 111.4(3) . . ?
C12 C11 B16 63.8(2) . . ?
B15 C11 B16 63.8(2) . . ?
C12 C11 Si3 129.6(3) . . ?
B15 C11 Si3 117.6(3) . . ?
B16 C11 Si3 130.8(3) . . ?
C12 C11 Fe1 72.4(2) . . ?
B15 C11 Fe1 69.5(2) . . ?
B16 C11 Fe1 93.0(2) . . ?
Si3 C11 Fe1 135.37(19) . . ?
C11 C12 B13 112.2(3) . . ?
C11 C12 B16 65.2(2) . . ?
B13 C12 B16 66.4(3) . . ?
C11 C12 Si4 131.4(3) . . ?
B13 C12 Si4 113.2(3) . . ?
B16 C12 Si4 120.5(2) . . ?
C11 C12 Fe1 66.01(19) . . ?
B13 C12 Fe1 70.0(2) . . ?
B16 C12 Fe1 90.5(2) . . ?
Si4 C12 Fe1 148.0(2) . . ?
C12 B13 B14 105.8(3) . . ?
C12 B13 B16 61.0(2) . . ?
B14 B13 B16 60.6(3) . . ?
C12 B13 Fe1 67.5(2) . . ?
B14 B13 Fe1 68.1(2) . . ?
B16 B13 Fe1 87.2(2) . . ?
B13 B14 B15 105.4(3) . . ?
B13 B14 B16 63.8(3) . . ?
B15 B14 B16 61.6(2) . . ?
B13 B14 Fe1 67.2(2) . . ?
B15 B14 Fe1 64.2(2) . . ?
B16 B14 Fe1 88.1(2) . . ?
B13 B14 Fe2 134.7(3) . . ?
B15 B14 Fe2 75.7(2) . . ?
B16 B14 Fe2 137.3(3) . . ?
Fe1 B14 Fe2 73.57(13) . . ?
C11 B15 B14 104.9(3) . . ?
C11 B15 B16 62.6(2) . . ?
B14 B15 B16 60.9(3) . . ?
C11 B15 Fe1 65.8(2) . . ?
B14 B15 Fe1 69.5(2) . . ?
B16 B15 Fe1 90.6(2) . . ?
C11 B15 Fe2 136.3(3) . . ?
B14 B15 Fe2 62.1(2) . . ?
B16 B15 Fe2 123.0(3) . . ?
Fe1 B15 Fe2 70.72(13) . . ?
C12 B16 C11 51.0(2) . . ?
C12 B16 B14 95.5(3) . . ?
C11 B16 B14 95.7(3) . . ?
C12 B16 B15 93.5(3) . . ?
C11 B16 B15 53.6(2) . . ?
B14 B16 B15 57.4(2) . . ?
C12 B16 B13 52.6(2) . . ?
C11 B16 B13 91.3(3) . . ?
B14 B16 B13 55.6(2) . . ?
B15 B16 B13 96.6(3) . . ?
C46 N41 C43 108.4(3) . . ?
C46 N41 C45 108.7(3) . . ?
C43 N41 C45 109.3(3) . . ?
C46 N41 Fe2 112.6(2) . . ?
C43 N41 Fe2 105.9(2) . . ?
C45 N41 Fe2 111.8(2) . . ?
C44 N42 C47 108.6(3) . . ?
C44 N42 C48 109.8(3) . . ?
C47 N42 C48 108.2(3) . . ?
C44 N42 Fe2 105.6(2) . . ?
C47 N42 Fe2 113.1(2) . . ?
C48 N42 Fe2 111.6(2) . . ?
N41 C43 C44 111.0(3) . . ?
N42 C44 C43 110.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Cnt1 1.643 . y
Fe1 C1 2.079(4) . y
Fe1 C2 2.138(4) . y
Fe1 B3 2.136(4) . y
Fe1 B4 2.175(4) . y
Fe1 B5 2.128(4) . y
Fe1 Cnt2 1.647 . y
Fe1 C11 2.053(4) . y
Fe1 C12 2.141(4) . y
Fe1 B13 2.179(4) . y
Fe1 B14 2.192(4) . y
Fe1 B15 2.108(5) . y
Fe1 Fe2 2.6450(7) . ?
Fe2 N41 2.215(3) . ?
Fe2 B14 2.224(4) . ?
Fe2 N42 2.227(3) . ?
Fe2 B4 2.234(4) . ?
Fe2 B5 2.425(4) . ?
Fe2 B15 2.439(4) . ?
Si1 C21 1.860(5) . ?
Si1 C23 1.868(5) . ?
Si1 C22 1.875(5) . ?
Si1 C1 1.886(4) . ?
Si2 C26 1.859(5) . ?
Si2 C25 1.863(6) . ?
Si2 C24 1.871(5) . ?
Si2 C2 1.884(4) . ?
Si3 C28 1.862(5) . ?
Si3 C27 1.868(5) . ?
Si3 C11 1.872(4) . ?
Si3 C29 1.874(5) . ?
Si4 C30 1.866(5) . ?
Si4 C31 1.867(5) . ?
Si4 C32 1.875(5) . ?
Si4 C12 1.893(4) . ?
C1 C2 1.494(5) . ?
C1 B5 1.572(6) . ?
C1 B6 1.754(6) . ?
C2 B3 1.573(6) . ?
C2 B6 1.728(6) . ?
B3 B4 1.660(6) . ?
B3 B6 1.800(7) . ?
B4 B5 1.685(7) . ?
B4 B6 1.740(6) . ?
B5 B6 1.770(6) . ?
C11 C12 1.493(5) . ?
C11 B15 1.583(6) . ?
C11 B16 1.746(5) . ?
C12 B13 1.567(6) . ?
C12 B16 1.725(5) . ?
B13 B14 1.661(6) . ?
B13 B16 1.807(6) . ?
B14 B15 1.690(6) . ?
B14 B16 1.754(6) . ?
B15 B16 1.765(6) . ?
N41 C46 1.472(5) . ?
N41 C43 1.485(5) . ?
N41 C45 1.485(5) . ?
N42 C44 1.478(5) . ?
N42 C47 1.481(5) . ?
N42 C48 1.483(5) . ?
C43 C44 1.490(6) . ?
|
1100794.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100794.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100794
loop_
_publ_author_name
'Tomlinson, Susan'
'Zheng, Chong'
'Hosmane, Narayan S.'
'Yang, Jimin'
'Wang, Ying'
'Zhang, Hongming'
'Gray, Thomas G.'
'Demissie, Temesgen'
'Maguire, John A.'
'Baumann, Frank'
'Klein, Axel'
'Sarkar, Biprajit'
'Kaim, Wolfgang'
'Lipscomb, William N.'
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural,
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2177
_journal_page_last 2187
_journal_paper_doi 10.1021/om048982u
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C16 H44 B8 Fe Si4'
_chemical_formula_weight 491.20
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.932(2)
_cell_length_b 12.939(3)
_cell_length_c 22.815(5)
_cell_measurement_reflns_used 30
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 10.0
_cell_measurement_theta_min 5.0
_cell_volume 3227.2(11)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 220(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type 'Siemens P3'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.262
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 1731
_diffrn_reflns_theta_full 20.04
_diffrn_reflns_theta_max 20.04
_diffrn_reflns_theta_min 1.79
_diffrn_standards_decay_% 5.30
_diffrn_standards_interval_count 147
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.619
_exptl_absorpt_correction_T_max 0.941
_exptl_absorpt_correction_T_min 0.747
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Siemens XEMP'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.011
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 1048
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.668
_refine_diff_density_min -0.377
_refine_diff_density_rms 0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.33(15)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 154
_refine_ls_number_reflns 1731
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.222
_refine_ls_R_factor_gt 0.097
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.9810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.186
_refine_ls_wR_factor_ref 0.246
_reflns_number_gt 793
_reflns_number_total 1731
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060288
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)2(1)2(1)
_cod_database_code 1100794
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.1055(4) 0.4641(3) 0.83269(17) 0.0337(12) Uani 1 1 d . . .
Si1 Si 0.2505(10) 0.6658(7) 0.9337(4) 0.065(3) Uani 1 1 d . . .
Si2 Si 0.3091(9) 0.4461(7) 0.7035(4) 0.058(3) Uani 1 1 d . . .
Si3 Si -0.2289(7) 0.4899(6) 0.8587(4) 0.054(3) Uani 1 1 d . . .
Si4 Si 0.2078(9) 0.2461(7) 0.9324(4) 0.059(3) Uani 1 1 d . . .
C1 C 0.209(2) 0.5989(18) 0.8632(10) 0.029(7) Uiso 1 1 d . . .
B2 B 0.297(3) 0.515(2) 0.8304(14) 0.049(10) Uiso 1 1 d . . .
H2 H 0.3828 0.4806 0.8458 0.058 Uiso 1 1 calc R . .
C3 C 0.235(2) 0.5072(17) 0.7668(9) 0.028(7) Uiso 1 1 d . . .
B4 B 0.103(3) 0.567(2) 0.7628(14) 0.048(10) Uiso 1 1 d . . .
H4 H 0.0416 0.5740 0.7248 0.057 Uiso 1 1 calc R . .
B5 B 0.097(3) 0.623(2) 0.8265(14) 0.027(9) Uiso 1 1 d . . .
H5 H 0.0244 0.6766 0.8405 0.032 Uiso 1 1 calc R . .
B6 B 0.234(3) 0.630(3) 0.7938(14) 0.045(10) Uiso 1 1 d . . .
H6 H 0.2818 0.6986 0.7768 0.054 Uiso 1 1 calc R . .
C11 C -0.074(2) 0.4234(18) 0.8528(10) 0.037(8) Uiso 1 1 d . . .
B12 B 0.009(3) 0.397(3) 0.9043(17) 0.053(12) Uiso 1 1 d . . .
H12 H -0.0032 0.4218 0.9500 0.064 Uiso 1 1 calc R . .
C13 C 0.107(3) 0.3231(19) 0.8832(10) 0.034(7) Uiso 1 1 d . . .
B14 B 0.100(4) 0.305(3) 0.8157(14) 0.050(11) Uiso 1 1 d . . .
H14 H 0.1591 0.2540 0.7898 0.059 Uiso 1 1 calc R . .
B15 B -0.030(3) 0.376(3) 0.7902(16) 0.052(11) Uiso 1 1 d . . .
H15 H -0.0718 0.3805 0.7465 0.063 Uiso 1 1 calc R . .
B16 B -0.036(3) 0.294(3) 0.8597(14) 0.050(11) Uiso 1 1 d . . .
H16 H -0.0938 0.2260 0.8684 0.060 Uiso 1 1 calc R . .
C21 C 0.130(3) 0.646(2) 0.9892(12) 0.079(11) Uiso 1 1 d . . .
H21A H 0.1511 0.6825 1.0244 0.119 Uiso 1 1 calc R . .
H21B H 0.1224 0.5736 0.9976 0.119 Uiso 1 1 calc R . .
H21C H 0.0534 0.6717 0.9745 0.119 Uiso 1 1 calc R . .
C22 C 0.393(4) 0.620(3) 0.9635(14) 0.115(15) Uiso 1 1 d . . .
H22A H 0.3828 0.5508 0.9779 0.173 Uiso 1 1 calc R . .
H22B H 0.4183 0.6643 0.9950 0.173 Uiso 1 1 calc R . .
H22C H 0.4546 0.6204 0.9334 0.173 Uiso 1 1 calc R . .
C23 C 0.252(4) 0.806(3) 0.9155(15) 0.113(15) Uiso 1 1 d . . .
H23A H 0.3036 0.8176 0.8821 0.170 Uiso 1 1 calc R . .
H23B H 0.2831 0.8444 0.9483 0.170 Uiso 1 1 calc R . .
H23C H 0.1704 0.8286 0.9068 0.170 Uiso 1 1 calc R . .
C24 C 0.424(3) 0.342(3) 0.7257(14) 0.102(13) Uiso 1 1 d . . .
H24A H 0.4929 0.3736 0.7443 0.153 Uiso 1 1 calc R . .
H24B H 0.4502 0.3051 0.6915 0.153 Uiso 1 1 calc R . .
H24C H 0.3854 0.2947 0.7525 0.153 Uiso 1 1 calc R . .
C25 C 0.387(3) 0.549(2) 0.6616(13) 0.104(11) Uiso 1 1 d . . .
H25A H 0.4506 0.5783 0.6852 0.156 Uiso 1 1 calc R . .
H25B H 0.3288 0.6012 0.6513 0.156 Uiso 1 1 calc R . .
H25C H 0.4216 0.5197 0.6267 0.156 Uiso 1 1 calc R . .
C26 C 0.196(3) 0.381(2) 0.6563(13) 0.087(11) Uiso 1 1 d . . .
H26A H 0.2368 0.3359 0.6296 0.131 Uiso 1 1 calc R . .
H26B H 0.1506 0.4323 0.6346 0.131 Uiso 1 1 calc R . .
H26C H 0.1401 0.3422 0.6802 0.131 Uiso 1 1 calc R . .
C27 C -0.220(3) 0.586(2) 0.9195(12) 0.082(12) Uiso 1 1 d . . .
H27A H -0.3000 0.6123 0.9277 0.122 Uiso 1 1 calc R . .
H27B H -0.1670 0.6416 0.9082 0.122 Uiso 1 1 calc R . .
H27C H -0.1877 0.5529 0.9539 0.122 Uiso 1 1 calc R . .
C29 C -0.264(3) 0.557(3) 0.7878(13) 0.110(14) Uiso 1 1 d . . .
H29A H -0.2000 0.6056 0.7793 0.165 Uiso 1 1 calc R . .
H29B H -0.3405 0.5919 0.7908 0.165 Uiso 1 1 calc R . .
H29C H -0.2677 0.5064 0.7569 0.165 Uiso 1 1 calc R . .
C28 C -0.347(3) 0.386(2) 0.8750(13) 0.077(12) Uiso 1 1 d . . .
H28A H -0.3599 0.3819 0.9165 0.116 Uiso 1 1 calc R . .
H28B H -0.3173 0.3204 0.8610 0.116 Uiso 1 1 calc R . .
H28C H -0.4222 0.4026 0.8558 0.116 Uiso 1 1 calc R . .
C30 C 0.360(3) 0.215(3) 0.8971(16) 0.128(17) Uiso 1 1 d . . .
H30A H 0.4100 0.1776 0.9242 0.192 Uiso 1 1 calc R . .
H30B H 0.4004 0.2787 0.8866 0.192 Uiso 1 1 calc R . .
H30C H 0.3468 0.1746 0.8625 0.192 Uiso 1 1 calc R . .
C31 C 0.243(3) 0.323(2) 0.9999(14) 0.096(13) Uiso 1 1 d . . .
H31A H 0.2921 0.2826 1.0260 0.145 Uiso 1 1 calc R . .
H31B H 0.1675 0.3413 1.0192 0.145 Uiso 1 1 calc R . .
H31C H 0.2858 0.3848 0.9892 0.145 Uiso 1 1 calc R . .
C32 C 0.130(4) 0.123(3) 0.9479(16) 0.138(17) Uiso 1 1 d . . .
H32A H 0.1293 0.0809 0.9132 0.206 Uiso 1 1 calc R . .
H32B H 0.0475 0.1361 0.9601 0.206 Uiso 1 1 calc R . .
H32C H 0.1727 0.0869 0.9786 0.206 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe 0.034(2) 0.035(2) 0.032(2) 0.000(3) 0.001(2) 0.002(3)
Si1 0.075(8) 0.063(7) 0.056(7) -0.029(6) -0.007(6) -0.016(6)
Si2 0.069(7) 0.054(7) 0.050(5) 0.004(6) 0.018(5) -0.018(6)
Si3 0.032(5) 0.052(7) 0.077(6) 0.012(5) 0.006(5) 0.000(5)
Si4 0.048(6) 0.057(7) 0.071(7) 0.011(6) 0.000(6) 0.022(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt1 Fe Cnt2 175.1 . . y
B5 Fe B4 46.2(12) . . ?
B5 Fe C11 102.8(12) . . ?
B4 Fe C11 108.6(12) . . ?
B5 Fe B14 164.8(11) . . ?
B4 Fe B14 119.2(13) . . ?
C11 Fe B14 76.4(13) . . ?
B5 Fe B15 118.4(14) . . ?
B4 Fe B15 89.2(14) . . ?
C11 Fe B15 45.8(11) . . ?
B14 Fe B15 50.3(14) . . ?
B5 Fe B12 115.9(14) . . ?
B4 Fe B12 147.6(14) . . ?
C11 Fe B12 42.5(11) . . ?
B14 Fe B12 74.0(14) . . ?
B15 Fe B12 77.6(14) . . ?
B5 Fe C3 73.9(11) . . ?
B4 Fe C3 45.7(11) . . ?
C11 Fe C3 147.5(9) . . ?
B14 Fe C3 98.4(12) . . ?
B15 Fe C3 106.4(11) . . ?
B12 Fe C3 166.7(12) . . ?
B5 Fe C13 151.6(12) . . ?
B4 Fe C13 162.2(11) . . ?
C11 Fe C13 71.2(10) . . ?
B14 Fe C13 43.0(10) . . ?
B15 Fe C13 78.0(12) . . ?
B12 Fe C13 41.3(11) . . ?
C3 Fe C13 126.3(10) . . ?
B5 Fe C1 41.6(11) . . ?
B4 Fe C1 74.9(11) . . ?
C11 Fe C1 128.1(10) . . ?
B14 Fe C1 148.9(13) . . ?
B15 Fe C1 160.1(12) . . ?
B12 Fe C1 109.7(12) . . ?
C3 Fe C1 71.0(9) . . ?
C13 Fe C1 120.0(9) . . ?
B5 Fe B2 75.1(13) . . ?
B4 Fe B2 78.5(14) . . ?
C11 Fe B2 168.4(11) . . ?
B14 Fe B2 108.7(14) . . ?
B15 Fe B2 145.3(13) . . ?
B12 Fe B2 127.8(13) . . ?
C3 Fe B2 43.5(10) . . ?
C13 Fe B2 105.1(11) . . ?
C1 Fe B2 43.6(10) . . ?
C22 Si1 C21 108.3(15) . . ?
C22 Si1 C23 113.4(18) . . ?
C21 Si1 C23 107.1(16) . . ?
C22 Si1 C1 112.3(14) . . ?
C21 Si1 C1 110.5(13) . . ?
C23 Si1 C1 105.1(14) . . ?
C3 Si2 C25 107.6(13) . . ?
C3 Si2 C26 110.9(13) . . ?
C25 Si2 C26 109.6(14) . . ?
C3 Si2 C24 112.6(13) . . ?
C25 Si2 C24 110.1(16) . . ?
C26 Si2 C24 106.0(14) . . ?
C27 Si3 C29 110.3(14) . . ?
C27 Si3 C28 111.3(14) . . ?
C29 Si3 C28 111.0(15) . . ?
C27 Si3 C11 107.9(13) . . ?
C29 Si3 C11 109.1(13) . . ?
C28 Si3 C11 107.1(12) . . ?
C32 Si4 C13 107.9(15) . . ?
C32 Si4 C31 113.3(16) . . ?
C13 Si4 C31 109.3(13) . . ?
C32 Si4 C30 107.9(17) . . ?
C13 Si4 C30 112.1(15) . . ?
C31 Si4 C30 106.4(16) . . ?
B5 C1 B2 111(2) . . ?
B5 C1 B6 63.7(19) . . ?
B2 C1 B6 68.1(18) . . ?
B5 C1 Si1 125(2) . . ?
B2 C1 Si1 123.8(19) . . ?
B6 C1 Si1 131.6(19) . . ?
B5 C1 Fe 64.5(14) . . ?
B2 C1 Fe 68.2(14) . . ?
B6 C1 Fe 88.7(16) . . ?
Si1 C1 Fe 139.6(13) . . ?
C3 B2 C1 102(2) . . ?
C3 B2 B6 58.9(17) . . ?
C1 B2 B6 56.6(16) . . ?
C3 B2 Fe 66.4(14) . . ?
C1 B2 Fe 68.2(14) . . ?
B6 B2 Fe 84.2(17) . . ?
B2 C3 B4 113(2) . . ?
B2 C3 B6 67.4(18) . . ?
B4 C3 B6 64.7(19) . . ?
B2 C3 Si2 123.5(18) . . ?
B4 C3 Si2 123.2(18) . . ?
B6 C3 Si2 133.4(19) . . ?
B2 C3 Fe 70.1(14) . . ?
B4 C3 Fe 65.3(14) . . ?
B6 C3 Fe 89.2(16) . . ?
Si2 C3 Fe 137.2(13) . . ?
B5 B4 C3 101(2) . . ?
B5 B4 B6 58.6(19) . . ?
C3 B4 B6 59.5(18) . . ?
B5 B4 Fe 66.3(15) . . ?
C3 B4 Fe 69.0(14) . . ?
B6 B4 Fe 88.8(19) . . ?
C1 B5 B4 112(3) . . ?
C1 B5 B6 62.2(18) . . ?
B4 B5 B6 66(2) . . ?
C1 B5 Fe 73.8(16) . . ?
B4 B5 Fe 67.5(15) . . ?
B6 B5 Fe 93(2) . . ?
C1 B6 B5 54.1(18) . . ?
C1 B6 C3 97(2) . . ?
B5 B6 C3 96(2) . . ?
C1 B6 B4 98(2) . . ?
B5 B6 B4 55.7(18) . . ?
C3 B6 B4 55.7(17) . . ?
C1 B6 B2 55.3(15) . . ?
B5 B6 B2 95(2) . . ?
C3 B6 B2 53.6(16) . . ?
B4 B6 B2 96(2) . . ?
B12 C11 B15 114(2) . . ?
B12 C11 B16 64(2) . . ?
B15 C11 B16 69(2) . . ?
B12 C11 Si3 125(2) . . ?
B15 C11 Si3 120.1(19) . . ?
B16 C11 Si3 130.2(18) . . ?
B12 C11 Fe 70.2(17) . . ?
B15 C11 Fe 67.6(16) . . ?
B16 C11 Fe 92.1(17) . . ?
Si3 C11 Fe 137.6(13) . . ?
C13 B12 C11 109(3) . . ?
C13 B12 B16 62(2) . . ?
C11 B12 B16 63(2) . . ?
C13 B12 Fe 70.3(17) . . ?
C11 B12 Fe 67.3(16) . . ?
B16 B12 Fe 90(2) . . ?
B12 C13 B14 112(3) . . ?
B12 C13 B16 66(2) . . ?
B14 C13 B16 67(2) . . ?
B12 C13 Si4 124(2) . . ?
B14 C13 Si4 123(2) . . ?
B16 C13 Si4 128.2(19) . . ?
B12 C13 Fe 68.4(17) . . ?
B14 C13 Fe 66.3(16) . . ?
B16 C13 Fe 90.6(17) . . ?
Si4 C13 Fe 141.2(15) . . ?
C13 B14 B15 107(3) . . ?
C13 B14 B16 60(2) . . ?
B15 B14 B16 64(2) . . ?
C13 B14 Fe 70.7(16) . . ?
B15 B14 Fe 65.1(16) . . ?
B16 B14 Fe 90(2) . . ?
C11 B15 B14 98(2) . . ?
C11 B15 B16 57.9(18) . . ?
B14 B15 B16 58.3(19) . . ?
C11 B15 Fe 66.6(16) . . ?
B14 B15 Fe 64.6(16) . . ?
B16 B15 Fe 86.9(18) . . ?
C13 B16 C11 92(2) . . ?
C13 B16 B12 52.0(17) . . ?
C11 B16 B12 52.2(17) . . ?
C13 B16 B14 52.8(17) . . ?
C11 B16 B14 94(2) . . ?
B12 B16 B14 92(2) . . ?
C13 B16 B15 96(2) . . ?
C11 B16 B15 53.0(16) . . ?
B12 B16 B15 93(2) . . ?
B14 B16 B15 57.4(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe Cnt1 1.642 . y
Fe C1 2.19(2) . y
Fe B2 2.19(3) . y
Fe C3 2.14(2) . y
Fe B4 2.08(3) . y
Fe B5 2.06(3) . y
Fe Cnt2 1.618 . y
Fe C11 2.09(3) . y
Fe B12 2.13(4) . y
Fe C13 2.16(2) . y
Fe B14 2.09(3) . y
Fe B15 2.10(4) . y
Si1 C22 1.80(4) . ?
Si1 C21 1.85(3) . ?
Si1 C23 1.86(3) . ?
Si1 C1 1.88(3) . ?
Si2 C3 1.84(2) . ?
Si2 C25 1.84(3) . ?
Si2 C26 1.84(3) . ?
Si2 C24 1.91(3) . ?
Si3 C27 1.86(3) . ?
Si3 C29 1.87(3) . ?
Si3 C28 1.90(3) . ?
Si3 C11 1.90(3) . ?
Si4 C32 1.84(4) . ?
Si4 C13 1.86(3) . ?
Si4 C31 1.87(3) . ?
Si4 C30 1.89(4) . ?
C1 B5 1.52(4) . ?
C1 B2 1.63(4) . ?
C1 B6 1.66(4) . ?
B2 C3 1.60(4) . ?
B2 B6 1.84(5) . ?
C3 B4 1.64(4) . ?
C3 B6 1.71(4) . ?
B4 B5 1.62(4) . ?
B4 B6 1.79(5) . ?
B5 B6 1.68(5) . ?
C11 B12 1.53(4) . ?
C11 B15 1.63(4) . ?
C11 B16 1.73(4) . ?
B12 C13 1.51(4) . ?
B12 B16 1.75(5) . ?
C13 B14 1.56(4) . ?
C13 B16 1.70(4) . ?
B14 B15 1.78(5) . ?
B14 B16 1.80(5) . ?
B15 B16 1.91(5) . ?
|
1100795.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100795.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100795
loop_
_publ_author_name
'Tomlinson, Susan'
'Zheng, Chong'
'Hosmane, Narayan S.'
'Yang, Jimin'
'Wang, Ying'
'Zhang, Hongming'
'Gray, Thomas G.'
'Demissie, Temesgen'
'Maguire, John A.'
'Baumann, Frank'
'Klein, Axel'
'Sarkar, Biprajit'
'Kaim, Wolfgang'
'Lipscomb, William N.'
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural,
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2177
_journal_page_last 2187
_journal_paper_doi 10.1021/om048982u
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety '[C34 H92 B8 Cl5 Co4 N6 Si4] . 1/2[C6 H6]'
_chemical_formula_sum 'C37 H95 B8 Cl5 Co4 N6 Si4'
_chemical_formula_weight 1236.00
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 89.85(2)
_cell_angle_beta 76.21(2)
_cell_angle_gamma 86.52(2)
_cell_formula_units_Z 2
_cell_length_a 11.562(2)
_cell_length_b 15.644(4)
_cell_length_c 17.925(4)
_cell_measurement_reflns_used 30
_cell_measurement_temperature 230(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 10.0
_cell_volume 3142.7(12)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 230(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Siemens P3'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.016
_diffrn_reflns_av_sigmaI/netI 0.023
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 7143
_diffrn_reflns_theta_full 21.00
_diffrn_reflns_theta_max 21.00
_diffrn_reflns_theta_min 1.76
_diffrn_standards_decay_% n/a
_diffrn_standards_interval_count 200
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.357
_exptl_absorpt_correction_T_max 0.963
_exptl_absorpt_correction_T_min 0.780
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Siemens XEMP'
_exptl_crystal_colour redish
_exptl_crystal_density_diffrn 1.306
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 1296
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.542
_refine_diff_density_min -0.382
_refine_diff_density_rms 0.047
_refine_ls_extinction_coef 0.0029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 602
_refine_ls_number_reflns 6714
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.027
_refine_ls_R_factor_all 0.038
_refine_ls_R_factor_gt 0.030
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+3.6846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.071
_refine_ls_wR_factor_ref 0.076
_reflns_number_gt 5781
_reflns_number_total 6714
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060289
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum '[C34 H92 B8 Cl5 Co4 N6 Si4] . 0.5[C6 H6]'
_cod_database_code 1100795
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.13218(4) 0.25114(3) 0.68496(2) 0.02812(14) Uani 1 1 d . . .
Co2 Co 0.40799(4) 0.76167(4) 0.89868(3) 0.04456(17) Uani 1 1 d . . .
Co3 Co 0.48591(4) 0.80122(3) 0.71852(3) 0.03621(15) Uani 1 1 d . . .
Co4 Co 0.65633(4) 0.68205(3) 0.79876(3) 0.03829(15) Uani 1 1 d . . .
Cl1 Cl 0.30733(9) 0.84965(7) 0.81645(5) 0.0507(3) Uani 1 1 d . . .
Cl2 Cl 0.56419(9) 0.66866(8) 0.93708(6) 0.0585(3) Uani 1 1 d . . .
Cl3 Cl 0.67792(9) 0.72440(7) 0.66603(5) 0.0517(3) Uani 1 1 d . . .
Cl4 Cl 0.58662(8) 0.83555(6) 0.82558(6) 0.0476(3) Uani 1 1 d . . .
Cl5 Cl 0.44623(8) 0.66006(6) 0.78735(5) 0.0431(2) Uani 1 1 d . . .
Si1 Si 0.31000(10) 0.43213(7) 0.62821(7) 0.0494(3) Uani 1 1 d . . .
Si2 Si 0.33248(10) 0.29385(8) 0.80456(6) 0.0517(3) Uani 1 1 d . . .
Si3 Si -0.05470(11) 0.07473(7) 0.69036(7) 0.0518(3) Uani 1 1 d . . .
Si4 Si -0.06330(11) 0.27302(9) 0.55598(7) 0.0591(4) Uani 1 1 d . . .
C1 C 0.2785(3) 0.3171(2) 0.64530(19) 0.0344(9) Uani 1 1 d . . .
C2 C 0.2864(3) 0.2664(2) 0.7147(2) 0.0355(9) Uani 1 1 d . . .
B3 B 0.2715(4) 0.1687(3) 0.7022(3) 0.0406(11) Uani 1 1 d . . .
H3 H 0.2760 0.1158 0.7422 0.049 Uiso 1 1 calc R . .
B4 B 0.2574(4) 0.1601(3) 0.6131(3) 0.0429(11) Uani 1 1 d . . .
H4 H 0.2509 0.1009 0.5819 0.052 Uiso 1 1 calc R . .
B5 B 0.2589(4) 0.2583(3) 0.5795(2) 0.0393(11) Uani 1 1 d . . .
H5 H 0.2532 0.2773 0.5213 0.047 Uiso 1 1 calc R . .
B6 B 0.3693(4) 0.2227(3) 0.6280(3) 0.0444(12) Uani 1 1 d . . .
H6 H 0.4662 0.2113 0.6054 0.053 Uiso 1 1 calc R . .
C11 C -0.0184(3) 0.1886(2) 0.69926(19) 0.0327(9) Uani 1 1 d . . .
C12 C -0.0213(3) 0.2656(2) 0.6503(2) 0.0357(9) Uani 1 1 d . . .
B13 B -0.0030(4) 0.3490(3) 0.6933(2) 0.0387(11) Uani 1 1 d . . .
H13 H -0.0041 0.4151 0.6724 0.046 Uiso 1 1 calc R . .
B14 B 0.0093(4) 0.3190(3) 0.7795(2) 0.0378(11) Uani 1 1 d . . .
H14 H 0.0178 0.3605 0.8271 0.045 Uiso 1 1 calc R . .
B15 B 0.0020(4) 0.2134(3) 0.7798(2) 0.0364(10) Uani 1 1 d . . .
H15 H 0.0049 0.1709 0.8283 0.044 Uiso 1 1 calc R . .
B16 B -0.1048(4) 0.2771(3) 0.7453(2) 0.0405(11) Uani 1 1 d . . .
H16 H -0.2014 0.2871 0.7697 0.049 Uiso 1 1 calc R . .
C21 C 0.2954(5) 0.4624(3) 0.5305(3) 0.0773(15) Uani 1 1 d . . .
H21A H 0.3081 0.5222 0.5228 0.116 Uiso 1 1 calc R . .
H21B H 0.2168 0.4515 0.5253 0.116 Uiso 1 1 calc R . .
H21C H 0.3536 0.4292 0.4929 0.116 Uiso 1 1 calc R . .
C22 C 0.4671(4) 0.4434(3) 0.6336(3) 0.0755(15) Uani 1 1 d . . .
H22A H 0.5197 0.4084 0.5945 0.113 Uiso 1 1 calc R . .
H22B H 0.4766 0.4255 0.6832 0.113 Uiso 1 1 calc R . .
H22C H 0.4859 0.5022 0.6261 0.113 Uiso 1 1 calc R . .
C23 C 0.2055(4) 0.5075(3) 0.6965(3) 0.0694(14) Uani 1 1 d . . .
H23A H 0.2504 0.5462 0.7181 0.104 Uiso 1 1 calc R . .
H23B H 0.1574 0.4757 0.7369 0.104 Uiso 1 1 calc R . .
H23C H 0.1549 0.5395 0.6696 0.104 Uiso 1 1 calc R . .
C24 C 0.4965(4) 0.2677(3) 0.7848(3) 0.0768(15) Uani 1 1 d . . .
H24A H 0.5255 0.2845 0.8281 0.115 Uiso 1 1 calc R . .
H24B H 0.5358 0.2979 0.7401 0.115 Uiso 1 1 calc R . .
H24C H 0.5126 0.2072 0.7758 0.115 Uiso 1 1 calc R . .
C25 C 0.2554(4) 0.2269(3) 0.8844(2) 0.0777(15) Uani 1 1 d . . .
H25A H 0.2736 0.2445 0.9314 0.117 Uiso 1 1 calc R . .
H25B H 0.2819 0.1679 0.8738 0.117 Uiso 1 1 calc R . .
H25C H 0.1708 0.2336 0.8894 0.117 Uiso 1 1 calc R . .
C26 C 0.3015(5) 0.4056(3) 0.8413(3) 0.0836(16) Uani 1 1 d . . .
H26A H 0.2173 0.4203 0.8513 0.125 Uiso 1 1 calc R . .
H26B H 0.3433 0.4437 0.8036 0.125 Uiso 1 1 calc R . .
H26C H 0.3277 0.4108 0.8879 0.125 Uiso 1 1 calc R . .
C27 C 0.0633(5) 0.0023(3) 0.7155(4) 0.111(2) Uani 1 1 d . . .
H27A H 0.0366 -0.0548 0.7220 0.166 Uiso 1 1 calc R . .
H27B H 0.0797 0.0219 0.7624 0.166 Uiso 1 1 calc R . .
H27C H 0.1346 0.0024 0.6749 0.166 Uiso 1 1 calc R . .
C28 C -0.1958(5) 0.0590(3) 0.7621(3) 0.0883(18) Uani 1 1 d . . .
H28A H -0.2571 0.0992 0.7532 0.132 Uiso 1 1 calc R . .
H28B H -0.1846 0.0680 0.8128 0.132 Uiso 1 1 calc R . .
H28C H -0.2190 0.0017 0.7576 0.132 Uiso 1 1 calc R . .
C29 C -0.0702(6) 0.0368(4) 0.5965(3) 0.113(2) Uani 1 1 d . . .
H29A H -0.0911 -0.0218 0.6004 0.170 Uiso 1 1 calc R . .
H29B H 0.0040 0.0410 0.5591 0.170 Uiso 1 1 calc R . .
H29C H -0.1317 0.0714 0.5810 0.170 Uiso 1 1 calc R . .
C30 C 0.0306(4) 0.2008(3) 0.4804(2) 0.0672(13) Uani 1 1 d . . .
H30A H -0.0181 0.1784 0.4494 0.101 Uiso 1 1 calc R . .
H30B H 0.0662 0.1544 0.5040 0.101 Uiso 1 1 calc R . .
H30C H 0.0921 0.2323 0.4486 0.101 Uiso 1 1 calc R . .
C31 C -0.2249(4) 0.2534(5) 0.5748(3) 0.124(3) Uani 1 1 d . . .
H31A H -0.2698 0.2942 0.6122 0.186 Uiso 1 1 calc R . .
H31B H -0.2374 0.1965 0.5939 0.186 Uiso 1 1 calc R . .
H31C H -0.2509 0.2595 0.5279 0.186 Uiso 1 1 calc R . .
C32 C -0.0450(7) 0.3826(4) 0.5178(3) 0.118(2) Uani 1 1 d . . .
H32A H -0.0667 0.3857 0.4694 0.177 Uiso 1 1 calc R . .
H32B H 0.0366 0.3963 0.5109 0.177 Uiso 1 1 calc R . .
H32C H -0.0956 0.4227 0.5535 0.177 Uiso 1 1 calc R . .
N41 N 0.3705(3) 0.8464(3) 0.9955(2) 0.0768(12) Uani 1 1 d . . .
N42 N 0.2561(3) 0.6975(3) 0.9622(2) 0.0656(11) Uani 1 1 d . . .
C43 C 0.2664(8) 0.8103(8) 1.0463(5) 0.231(7) Uani 1 1 d . . .
H43A H 0.2894 0.7969 1.0938 0.277 Uiso 1 1 calc R . .
H43B H 0.2054 0.8569 1.0583 0.277 Uiso 1 1 calc R . .
C44 C 0.2161(8) 0.7482(6) 1.0311(4) 0.165(4) Uani 1 1 d . . .
H44A H 0.1345 0.7684 1.0329 0.198 Uiso 1 1 calc R . .
H44B H 0.2125 0.7090 1.0735 0.198 Uiso 1 1 calc R . .
C45 C 0.4674(5) 0.8496(4) 1.0342(3) 0.0959(19) Uani 1 1 d . . .
H45A H 0.5353 0.8722 1.0000 0.144 Uiso 1 1 calc R . .
H45B H 0.4885 0.7929 1.0492 0.144 Uiso 1 1 calc R . .
H45C H 0.4422 0.8858 1.0790 0.144 Uiso 1 1 calc R . .
C46 C 0.3432(7) 0.9342(5) 0.9768(4) 0.147(4) Uani 1 1 d . . .
H46A H 0.3263 0.9690 1.0226 0.221 Uiso 1 1 calc R . .
H46B H 0.2749 0.9370 0.9549 0.221 Uiso 1 1 calc R . .
H46C H 0.4103 0.9550 0.9404 0.221 Uiso 1 1 calc R . .
C47 C 0.2841(5) 0.6095(4) 0.9819(4) 0.103(2) Uani 1 1 d . . .
H47A H 0.3459 0.6084 1.0094 0.154 Uiso 1 1 calc R . .
H47B H 0.3108 0.5756 0.9358 0.154 Uiso 1 1 calc R . .
H47C H 0.2141 0.5865 1.0135 0.154 Uiso 1 1 calc R . .
C48 C 0.1596(5) 0.6971(5) 0.9231(4) 0.129(3) Uani 1 1 d . . .
H48A H 0.0916 0.6731 0.9561 0.193 Uiso 1 1 calc R . .
H48B H 0.1850 0.6633 0.8768 0.193 Uiso 1 1 calc R . .
H48C H 0.1384 0.7548 0.9106 0.193 Uiso 1 1 calc R . .
N51 N 0.5197(3) 0.9199(2) 0.6608(2) 0.0539(9) Uani 1 1 d . . .
N52 N 0.3959(3) 0.7759(2) 0.62924(17) 0.0438(8) Uani 1 1 d . . .
C53 C 0.4341(6) 0.9271(4) 0.6131(4) 0.115(3) Uani 1 1 d . . .
H53A H 0.3574 0.9481 0.6447 0.139 Uiso 1 1 calc R . .
H53B H 0.4596 0.9691 0.5737 0.139 Uiso 1 1 calc R . .
C54 C 0.4196(6) 0.8502(3) 0.5777(3) 0.0949(19) Uani 1 1 d . . .
H54A H 0.4912 0.8361 0.5378 0.114 Uiso 1 1 calc R . .
H54B H 0.3540 0.8592 0.5528 0.114 Uiso 1 1 calc R . .
C55 C 0.4925(5) 0.9946(3) 0.7142(3) 0.0946(19) Uani 1 1 d . . .
H55A H 0.4999 1.0465 0.6852 0.142 Uiso 1 1 calc R . .
H55B H 0.5475 0.9928 0.7468 0.142 Uiso 1 1 calc R . .
H55C H 0.4126 0.9929 0.7451 0.142 Uiso 1 1 calc R . .
C56 C 0.6436(4) 0.9252(3) 0.6177(3) 0.0798(15) Uani 1 1 d . . .
H56A H 0.6658 0.8776 0.5825 0.120 Uiso 1 1 calc R . .
H56B H 0.6948 0.9238 0.6528 0.120 Uiso 1 1 calc R . .
H56C H 0.6515 0.9777 0.5897 0.120 Uiso 1 1 calc R . .
C57 C 0.4458(4) 0.6978(3) 0.5849(2) 0.0652(13) Uani 1 1 d . . .
H57A H 0.4319 0.6490 0.6176 0.098 Uiso 1 1 calc R . .
H57B H 0.5301 0.7017 0.5650 0.098 Uiso 1 1 calc R . .
H57C H 0.4081 0.6918 0.5431 0.098 Uiso 1 1 calc R . .
C58 C 0.2679(4) 0.7679(4) 0.6583(3) 0.0780(15) Uani 1 1 d . . .
H58A H 0.2319 0.8204 0.6834 0.117 Uiso 1 1 calc R . .
H58B H 0.2548 0.7219 0.6943 0.117 Uiso 1 1 calc R . .
H58C H 0.2327 0.7562 0.6163 0.117 Uiso 1 1 calc R . .
N61 N 0.8368(3) 0.7031(2) 0.80700(19) 0.0529(9) Uani 1 1 d . . .
N62 N 0.7202(3) 0.5509(2) 0.7817(2) 0.0573(10) Uani 1 1 d . . .
C63 C 0.9000(4) 0.6189(4) 0.7859(4) 0.0980(19) Uani 1 1 d . . .
H63A H 0.9330 0.6176 0.7308 0.118 Uiso 1 1 calc R . .
H63B H 0.9664 0.6136 0.8103 0.118 Uiso 1 1 calc R . .
C64 C 0.8319(5) 0.5469(4) 0.8053(4) 0.104(2) Uani 1 1 d . . .
H64A H 0.8148 0.5400 0.8605 0.125 Uiso 1 1 calc R . .
H64B H 0.8796 0.4964 0.7820 0.125 Uiso 1 1 calc R . .
C65 C 0.8409(4) 0.7275(4) 0.8846(3) 0.097(2) Uani 1 1 d . . .
H65A H 0.9219 0.7357 0.8862 0.145 Uiso 1 1 calc R . .
H65B H 0.8102 0.6832 0.9195 0.145 Uiso 1 1 calc R . .
H65C H 0.7932 0.7799 0.8992 0.145 Uiso 1 1 calc R . .
C66 C 0.8951(4) 0.7664(4) 0.7535(3) 0.099(2) Uani 1 1 d . . .
H66A H 0.8510 0.8208 0.7642 0.148 Uiso 1 1 calc R . .
H66B H 0.8978 0.7486 0.7019 0.148 Uiso 1 1 calc R . .
H66C H 0.9748 0.7715 0.7593 0.148 Uiso 1 1 calc R . .
C67 C 0.7365(5) 0.5218(3) 0.7019(3) 0.0771(15) Uani 1 1 d . . .
H67A H 0.7929 0.5560 0.6686 0.116 Uiso 1 1 calc R . .
H67B H 0.6615 0.5275 0.6876 0.116 Uiso 1 1 calc R . .
H67C H 0.7659 0.4628 0.6971 0.116 Uiso 1 1 calc R . .
C68 C 0.6403(6) 0.4907(3) 0.8295(4) 0.104(2) Uani 1 1 d . . .
H68A H 0.6756 0.4334 0.8205 0.156 Uiso 1 1 calc R . .
H68B H 0.5646 0.4942 0.8161 0.156 Uiso 1 1 calc R . .
H68C H 0.6291 0.5056 0.8828 0.156 Uiso 1 1 calc R . .
C71 C -0.0613(5) 0.9280(3) 0.9996(4) 0.0799(15) Uani 1 1 d . . .
H71 H -0.1029 0.8790 0.9992 0.096 Uiso 1 1 calc R . .
C72 C 0.0091(5) 0.9569(4) 0.9325(3) 0.0818(16) Uani 1 1 d . . .
H72 H 0.0153 0.9276 0.8865 0.098 Uiso 1 1 calc R . .
C73 C 0.0701(5) 1.0289(4) 0.9336(3) 0.0774(15) Uani 1 1 d . . .
H73 H 0.1179 1.0485 0.8882 0.093 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0255(3) 0.0308(3) 0.0262(3) 0.0005(2) -0.0032(2) 0.0016(2)
Co2 0.0373(3) 0.0669(4) 0.0261(3) -0.0035(3) -0.0049(2) 0.0134(3)
Co3 0.0332(3) 0.0444(3) 0.0294(3) 0.0015(2) -0.0069(2) 0.0079(2)
Co4 0.0330(3) 0.0472(3) 0.0333(3) -0.0011(2) -0.0087(2) 0.0108(2)
Cl1 0.0421(6) 0.0691(7) 0.0365(6) -0.0034(5) -0.0064(4) 0.0206(5)
Cl2 0.0519(6) 0.0859(8) 0.0356(6) 0.0072(5) -0.0114(5) 0.0168(6)
Cl3 0.0409(6) 0.0753(7) 0.0327(5) 0.0047(5) -0.0014(4) 0.0175(5)
Cl4 0.0433(6) 0.0499(6) 0.0509(6) -0.0073(5) -0.0156(5) 0.0065(5)
Cl5 0.0417(6) 0.0484(6) 0.0389(5) 0.0016(4) -0.0102(4) 0.0011(4)
Si1 0.0410(7) 0.0404(7) 0.0598(8) 0.0130(6) 0.0021(6) -0.0046(5)
Si2 0.0458(7) 0.0733(8) 0.0410(7) 0.0086(6) -0.0166(5) -0.0189(6)
Si3 0.0553(7) 0.0469(7) 0.0465(7) -0.0126(5) 0.0049(6) -0.0183(6)
Si4 0.0534(8) 0.0872(10) 0.0408(7) -0.0023(6) -0.0230(6) 0.0115(7)
C1 0.025(2) 0.041(2) 0.034(2) 0.0035(17) -0.0016(16) 0.0011(16)
C2 0.024(2) 0.046(2) 0.034(2) 0.0050(18) -0.0034(16) -0.0004(17)
B3 0.032(2) 0.038(3) 0.048(3) 0.008(2) -0.005(2) 0.006(2)
B4 0.035(3) 0.041(3) 0.047(3) -0.007(2) 0.000(2) 0.006(2)
B5 0.028(2) 0.055(3) 0.029(2) 0.000(2) 0.0022(19) 0.004(2)
B6 0.034(3) 0.052(3) 0.042(3) 0.006(2) -0.002(2) 0.010(2)
C11 0.026(2) 0.036(2) 0.032(2) -0.0033(17) 0.0009(16) -0.0024(16)
C12 0.025(2) 0.047(2) 0.033(2) -0.0038(18) -0.0051(16) 0.0055(17)
B13 0.031(2) 0.038(3) 0.043(3) -0.003(2) -0.003(2) 0.008(2)
B14 0.031(2) 0.044(3) 0.034(2) -0.011(2) 0.000(2) 0.001(2)
B15 0.028(2) 0.047(3) 0.030(2) -0.001(2) 0.0003(19) -0.001(2)
B16 0.032(2) 0.048(3) 0.037(3) -0.006(2) -0.001(2) 0.004(2)
C21 0.083(4) 0.070(3) 0.066(3) 0.033(3) 0.005(3) 0.005(3)
C22 0.053(3) 0.056(3) 0.112(4) 0.016(3) -0.005(3) -0.019(2)
C23 0.067(3) 0.043(3) 0.090(4) -0.004(2) 0.000(3) -0.007(2)
C24 0.055(3) 0.107(4) 0.079(4) 0.020(3) -0.036(3) -0.014(3)
C25 0.080(4) 0.116(4) 0.044(3) 0.022(3) -0.022(3) -0.035(3)
C26 0.098(4) 0.095(4) 0.062(3) -0.016(3) -0.023(3) -0.023(3)
C27 0.109(5) 0.041(3) 0.183(7) 0.012(4) -0.035(5) -0.009(3)
C28 0.094(4) 0.083(4) 0.071(3) -0.023(3) 0.024(3) -0.049(3)
C29 0.180(7) 0.096(4) 0.055(3) -0.027(3) 0.001(4) -0.068(4)
C30 0.077(3) 0.088(3) 0.035(2) 0.000(2) -0.008(2) -0.014(3)
C31 0.051(3) 0.251(9) 0.076(4) -0.041(5) -0.032(3) 0.015(4)
C32 0.196(7) 0.094(4) 0.073(4) 0.019(3) -0.062(4) 0.033(4)
N41 0.062(3) 0.117(4) 0.047(2) -0.035(2) -0.010(2) 0.019(2)
N42 0.048(2) 0.098(3) 0.041(2) 0.010(2) 0.0062(18) 0.007(2)
C43 0.174(9) 0.351(16) 0.115(7) -0.155(9) 0.102(6) -0.143(10)
C44 0.171(8) 0.175(8) 0.097(6) -0.030(6) 0.083(6) -0.049(7)
C45 0.114(5) 0.123(5) 0.060(3) -0.035(3) -0.046(3) 0.025(4)
C46 0.194(8) 0.142(6) 0.124(6) -0.094(5) -0.104(6) 0.109(6)
C47 0.072(4) 0.109(5) 0.120(5) 0.055(4) -0.007(3) -0.010(3)
C48 0.049(3) 0.210(8) 0.136(6) 0.086(6) -0.032(4) -0.036(4)
N51 0.050(2) 0.052(2) 0.065(2) 0.0174(19) -0.0232(19) -0.0039(17)
N52 0.048(2) 0.051(2) 0.0333(18) 0.0002(16) -0.0143(15) 0.0054(16)
C53 0.139(6) 0.103(5) 0.144(6) 0.077(5) -0.103(5) -0.049(4)
C54 0.168(6) 0.076(4) 0.062(3) 0.015(3) -0.071(4) -0.006(4)
C55 0.095(4) 0.045(3) 0.131(5) 0.013(3) -0.005(4) 0.013(3)
C56 0.075(4) 0.071(3) 0.083(4) 0.021(3) 0.005(3) -0.013(3)
C57 0.067(3) 0.081(3) 0.051(3) -0.021(2) -0.024(2) 0.010(3)
C58 0.047(3) 0.134(5) 0.057(3) -0.017(3) -0.022(2) 0.004(3)
N61 0.0355(19) 0.068(2) 0.055(2) -0.0045(19) -0.0144(17) 0.0121(18)
N62 0.059(2) 0.052(2) 0.065(2) -0.0093(19) -0.0292(19) 0.0212(18)
C63 0.043(3) 0.100(5) 0.151(6) -0.014(4) -0.030(3) 0.020(3)
C64 0.097(4) 0.076(4) 0.160(6) -0.046(4) -0.084(4) 0.050(4)
C65 0.055(3) 0.165(6) 0.080(4) -0.036(4) -0.038(3) 0.008(3)
C66 0.053(3) 0.134(5) 0.114(5) 0.040(4) -0.024(3) -0.034(3)
C67 0.091(4) 0.069(3) 0.076(4) -0.027(3) -0.035(3) 0.028(3)
C68 0.135(5) 0.054(3) 0.115(5) 0.015(3) -0.021(4) 0.021(3)
C71 0.072(4) 0.073(4) 0.087(4) 0.029(4) -0.005(3) -0.004(3)
C72 0.082(4) 0.081(4) 0.073(4) 0.022(3) -0.003(3) 0.006(3)
C73 0.068(3) 0.074(4) 0.077(4) 0.035(3) 0.004(3) 0.004(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt1 Co1 Cnt2 178.9 . . y
C2 Co1 C11 148.63(14) . . ?
C2 Co1 C12 166.49(15) . . ?
C11 Co1 C12 43.49(14) . . ?
C2 Co1 C1 43.51(14) . . ?
C11 Co1 C1 166.56(14) . . ?
C12 Co1 C1 125.61(14) . . ?
C2 Co1 B3 45.14(16) . . ?
C11 Co1 B3 110.32(16) . . ?
C12 Co1 B3 147.71(16) . . ?
C1 Co1 B3 76.25(16) . . ?
C2 Co1 B15 110.53(15) . . ?
C11 Co1 B15 44.93(15) . . ?
C12 Co1 B15 75.89(16) . . ?
C1 Co1 B15 147.76(15) . . ?
B3 Co1 B15 97.14(17) . . ?
C2 Co1 B13 123.61(16) . . ?
C11 Co1 B13 75.79(16) . . ?
C12 Co1 B13 44.74(16) . . ?
C1 Co1 B13 100.75(16) . . ?
B3 Co1 B13 165.37(17) . . ?
B15 Co1 B13 77.65(17) . . ?
C2 Co1 B5 75.61(16) . . ?
C11 Co1 B5 123.98(16) . . ?
C12 Co1 B5 101.02(15) . . ?
C1 Co1 B5 44.51(16) . . ?
B3 Co1 B5 77.94(17) . . ?
B15 Co1 B5 165.74(17) . . ?
B13 Co1 B5 110.22(17) . . ?
C2 Co1 B4 75.85(16) . . ?
C11 Co1 B4 100.21(16) . . ?
C12 Co1 B4 111.40(16) . . ?
C1 Co1 B4 75.68(16) . . ?
B3 Co1 B4 45.75(17) . . ?
B15 Co1 B4 122.18(17) . . ?
B13 Co1 B4 148.01(17) . . ?
B5 Co1 B4 45.49(17) . . ?
C2 Co1 B14 99.82(15) . . ?
C11 Co1 B14 76.07(15) . . ?
C12 Co1 B14 75.87(15) . . ?
C1 Co1 B14 111.03(15) . . ?
B3 Co1 B14 121.78(17) . . ?
B15 Co1 B14 45.75(16) . . ?
B13 Co1 B14 45.46(17) . . ?
B5 Co1 B14 147.67(17) . . ?
B4 Co1 B14 165.40(17) . . ?
N41 Co2 N42 84.40(16) . . ?
N41 Co2 Cl1 97.53(12) . . ?
N42 Co2 Cl1 98.51(11) . . ?
N41 Co2 Cl2 97.22(12) . . ?
N42 Co2 Cl2 97.39(11) . . ?
Cl1 Co2 Cl2 159.24(4) . . ?
N41 Co2 Cl5 178.18(12) . . ?
N42 Co2 Cl5 93.79(11) . . ?
Cl1 Co2 Cl5 82.63(4) . . ?
Cl2 Co2 Cl5 83.09(4) . . ?
N41 Co2 Cl4 95.49(13) . . ?
N42 Co2 Cl4 179.30(11) . . ?
Cl1 Co2 Cl4 82.19(4) . . ?
Cl2 Co2 Cl4 81.93(4) . . ?
Cl5 Co2 Cl4 86.32(4) . . ?
N51 Co3 N52 83.93(13) . . ?
N51 Co3 Cl3 98.90(10) . . ?
N52 Co3 Cl3 99.99(9) . . ?
N51 Co3 Cl1 98.26(10) . . ?
N52 Co3 Cl1 96.66(9) . . ?
Cl3 Co3 Cl1 157.19(4) . . ?
N51 Co3 Cl5 179.83(10) . . ?
N52 Co3 Cl5 96.22(9) . . ?
Cl3 Co3 Cl5 81.01(4) . . ?
Cl1 Co3 Cl5 81.79(4) . . ?
N51 Co3 Cl4 95.17(10) . . ?
N52 Co3 Cl4 177.96(9) . . ?
Cl3 Co3 Cl4 81.95(4) . . ?
Cl1 Co3 Cl4 81.64(4) . . ?
Cl5 Co3 Cl4 84.68(4) . . ?
N62 Co4 N61 84.45(13) . . ?
N62 Co4 Cl3 99.70(10) . . ?
N61 Co4 Cl3 97.63(10) . . ?
N62 Co4 Cl2 95.35(11) . . ?
N61 Co4 Cl2 98.32(10) . . ?
Cl3 Co4 Cl2 159.00(4) . . ?
N62 Co4 Cl4 176.61(10) . . ?
N61 Co4 Cl4 93.39(10) . . ?
Cl3 Co4 Cl4 83.16(4) . . ?
Cl2 Co4 Cl4 82.36(4) . . ?
N62 Co4 Cl5 96.34(10) . . ?
N61 Co4 Cl5 178.84(10) . . ?
Cl3 Co4 Cl5 81.41(4) . . ?
Cl2 Co4 Cl5 82.46(4) . . ?
Cl4 Co4 Cl5 85.86(4) . . ?
Co3 Cl1 Co2 81.65(4) . . ?
Co4 Cl2 Co2 80.18(4) . . ?
Co4 Cl3 Co3 82.64(4) . . ?
Co4 Cl4 Co2 78.90(4) . . ?
Co4 Cl4 Co3 79.16(4) . . ?
Co2 Cl4 Co3 78.77(4) . . ?
Co2 Cl5 Co4 78.63(4) . . ?
Co2 Cl5 Co3 79.21(4) . . ?
Co4 Cl5 Co3 78.64(4) . . ?
C21 Si1 C22 108.7(2) . . ?
C21 Si1 C23 106.4(2) . . ?
C22 Si1 C23 111.0(2) . . ?
C21 Si1 C1 109.7(2) . . ?
C22 Si1 C1 107.20(18) . . ?
C23 Si1 C1 113.72(18) . . ?
C26 Si2 C25 105.2(2) . . ?
C26 Si2 C24 108.4(2) . . ?
C25 Si2 C24 109.4(2) . . ?
C26 Si2 C2 117.9(2) . . ?
C25 Si2 C2 109.54(19) . . ?
C24 Si2 C2 106.31(19) . . ?
C29 Si3 C28 108.2(3) . . ?
C29 Si3 C27 105.8(3) . . ?
C28 Si3 C27 107.6(3) . . ?
C29 Si3 C11 118.1(2) . . ?
C28 Si3 C11 107.26(19) . . ?
C27 Si3 C11 109.5(2) . . ?
C32 Si4 C30 105.7(3) . . ?
C32 Si4 C31 107.3(3) . . ?
C30 Si4 C31 112.8(3) . . ?
C32 Si4 C12 110.1(2) . . ?
C30 Si4 C12 113.76(19) . . ?
C31 Si4 C12 107.0(2) . . ?
C2 C1 B5 111.3(3) . . ?
C2 C1 B6 64.4(2) . . ?
B5 C1 B6 64.5(3) . . ?
C2 C1 Si1 127.0(3) . . ?
B5 C1 Si1 121.2(3) . . ?
B6 C1 Si1 132.6(2) . . ?
C2 C1 Co1 67.87(18) . . ?
B5 C1 Co1 70.7(2) . . ?
B6 C1 Co1 91.4(2) . . ?
Si1 C1 Co1 135.97(19) . . ?
C1 C2 B3 111.5(3) . . ?
C1 C2 B6 64.9(2) . . ?
B3 C2 B6 64.7(3) . . ?
C1 C2 Si2 132.3(3) . . ?
B3 C2 Si2 115.4(3) . . ?
B6 C2 Si2 130.6(2) . . ?
C1 C2 Co1 68.62(19) . . ?
B3 C2 Co1 70.0(2) . . ?
B6 C2 Co1 92.0(2) . . ?
Si2 C2 Co1 136.37(19) . . ?
C2 B3 B4 105.4(3) . . ?
C2 B3 B6 62.1(2) . . ?
B4 B3 B6 60.8(3) . . ?
C2 B3 Co1 64.84(19) . . ?
B4 B3 Co1 69.5(2) . . ?
B6 B3 Co1 88.3(2) . . ?
B5 B4 B3 106.0(3) . . ?
B5 B4 B6 63.0(3) . . ?
B3 B4 B6 63.2(3) . . ?
B5 B4 Co1 65.6(2) . . ?
B3 B4 Co1 64.7(2) . . ?
B6 B4 Co1 87.0(2) . . ?
C1 B5 B4 105.8(3) . . ?
C1 B5 B6 62.7(3) . . ?
B4 B5 B6 61.0(3) . . ?
C1 B5 Co1 64.74(19) . . ?
B4 B5 Co1 68.9(2) . . ?
B6 B5 Co1 87.8(2) . . ?
C2 B6 B4 95.0(3) . . ?
C2 B6 C1 50.7(2) . . ?
B4 B6 C1 94.8(3) . . ?
C2 B6 B5 91.9(3) . . ?
B4 B6 B5 56.0(3) . . ?
C1 B6 B5 52.8(2) . . ?
C2 B6 B3 53.1(2) . . ?
B4 B6 B3 56.0(3) . . ?
C1 B6 B3 92.0(3) . . ?
B5 B6 B3 95.9(3) . . ?
C12 C11 B15 111.2(3) . . ?
C12 C11 B16 65.0(2) . . ?
B15 C11 B16 64.0(2) . . ?
C12 C11 Si3 133.6(3) . . ?
B15 C11 Si3 114.5(3) . . ?
B16 C11 Si3 131.4(2) . . ?
C12 C11 Co1 68.39(18) . . ?
B15 C11 Co1 70.3(2) . . ?
B16 C11 Co1 91.7(2) . . ?
Si3 C11 Co1 135.51(19) . . ?
C11 C12 B13 111.2(3) . . ?
C11 C12 B16 64.5(2) . . ?
B13 C12 B16 64.4(2) . . ?
C11 C12 Si4 127.9(3) . . ?
B13 C12 Si4 120.2(3) . . ?
B16 C12 Si4 132.5(2) . . ?
C11 C12 Co1 68.12(18) . . ?
B13 C12 Co1 70.5(2) . . ?
B16 C12 Co1 91.4(2) . . ?
Si4 C12 Co1 135.95(19) . . ?
C12 B13 B14 106.2(3) . . ?
C12 B13 B16 62.8(2) . . ?
B14 B13 B16 61.0(3) . . ?
C12 B13 Co1 64.81(19) . . ?
B14 B13 Co1 69.4(2) . . ?
B16 B13 Co1 88.0(2) . . ?
B13 B14 B15 105.3(3) . . ?
B13 B14 B16 63.0(3) . . ?
B15 B14 B16 62.4(3) . . ?
B13 B14 Co1 65.1(2) . . ?
B15 B14 Co1 64.82(19) . . ?
B16 B14 Co1 86.7(2) . . ?
C11 B15 B14 105.9(3) . . ?
C11 B15 B16 62.8(2) . . ?
B14 B15 B16 61.1(3) . . ?
C11 B15 Co1 64.76(19) . . ?
B14 B15 Co1 69.4(2) . . ?
B16 B15 Co1 88.5(2) . . ?
B14 B16 C11 95.4(3) . . ?
B14 B16 C12 94.9(3) . . ?
C11 B16 C12 50.6(2) . . ?
B14 B16 B15 56.4(2) . . ?
C11 B16 B15 53.2(2) . . ?
C12 B16 B15 92.0(3) . . ?
B14 B16 B13 55.9(2) . . ?
C11 B16 B13 91.8(3) . . ?
C12 B16 B13 52.8(2) . . ?
B15 B16 B13 96.0(3) . . ?
C46 N41 C45 105.5(5) . . ?
C46 N41 C43 110.9(7) . . ?
C45 N41 C43 110.4(6) . . ?
C46 N41 Co2 113.4(3) . . ?
C45 N41 Co2 114.1(3) . . ?
C43 N41 Co2 102.6(4) . . ?
C44 N42 C48 108.5(6) . . ?
C44 N42 C47 109.5(5) . . ?
C48 N42 C47 108.0(5) . . ?
C44 N42 Co2 103.5(4) . . ?
C48 N42 Co2 113.1(3) . . ?
C47 N42 Co2 114.0(3) . . ?
C44 C43 N41 125.4(6) . . ?
C43 C44 N42 124.0(7) . . ?
C53 N51 C56 113.7(4) . . ?
C53 N51 C55 106.5(4) . . ?
C56 N51 C55 106.3(4) . . ?
C53 N51 Co3 104.1(3) . . ?
C56 N51 Co3 113.5(3) . . ?
C55 N51 Co3 112.6(3) . . ?
C58 N52 C57 107.9(4) . . ?
C58 N52 C54 111.0(4) . . ?
C57 N52 C54 108.4(4) . . ?
C58 N52 Co3 113.1(2) . . ?
C57 N52 Co3 112.3(2) . . ?
C54 N52 Co3 104.0(3) . . ?
C54 C53 N51 114.2(5) . . ?
C53 C54 N52 115.5(4) . . ?
C65 N61 C66 109.0(4) . . ?
C65 N61 C63 110.5(4) . . ?
C66 N61 C63 108.6(4) . . ?
C65 N61 Co4 111.8(3) . . ?
C66 N61 Co4 113.8(3) . . ?
C63 N61 Co4 103.0(3) . . ?
C64 N62 C67 111.8(4) . . ?
C64 N62 C68 108.2(4) . . ?
C67 N62 C68 106.0(4) . . ?
C64 N62 Co4 104.4(3) . . ?
C67 N62 Co4 112.7(3) . . ?
C68 N62 Co4 113.8(3) . . ?
C64 C63 N61 116.4(4) . . ?
C63 C64 N62 114.8(5) . . ?
C73 C71 C72 119.9(5) 2_577 . ?
C73 C72 C71 119.7(5) . . ?
C71 C73 C72 120.4(5) 2_577 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Cnt1 1.577 . y
Co1 C1 2.016(3) . y
Co1 C2 2.006(3) . y
Co1 B3 2.083(4) . y
Co1 B4 2.157(4) . y
Co1 B5 2.105(4) . y
Co1 Cnt2 1.580 . y
Co1 C11 2.012(3) . y
Co1 C12 2.016(3) . y
Co1 B13 2.099(4) . y
Co1 B14 2.167(4) . y
Co1 B15 2.094(4) . y
Co2 N41 2.130(4) . ?
Co2 N42 2.155(4) . ?
Co2 Cl1 2.4565(12) . ?
Co2 Cl2 2.4740(12) . ?
Co2 Cl5 2.4930(12) . ?
Co2 Cl4 2.5120(13) . ?
Co3 N51 2.135(3) . ?
Co3 N52 2.156(3) . ?
Co3 Cl3 2.4380(12) . ?
Co3 Cl1 2.4511(12) . ?
Co3 Cl5 2.5393(12) . ?
Co3 Cl4 2.5442(12) . ?
Co4 N62 2.135(3) . ?
Co4 N61 2.172(3) . ?
Co4 Cl3 2.4271(12) . ?
Co4 Cl2 2.4680(13) . ?
Co4 Cl4 2.4967(13) . ?
Co4 Cl5 2.5297(11) . ?
Si1 C21 1.857(5) . ?
Si1 C22 1.861(5) . ?
Si1 C23 1.865(4) . ?
Si1 C1 1.868(4) . ?
Si2 C26 1.854(5) . ?
Si2 C25 1.854(4) . ?
Si2 C24 1.864(5) . ?
Si2 C2 1.873(4) . ?
Si3 C29 1.837(5) . ?
Si3 C28 1.851(4) . ?
Si3 C27 1.857(6) . ?
Si3 C11 1.871(4) . ?
Si4 C32 1.850(6) . ?
Si4 C30 1.857(4) . ?
Si4 C31 1.863(5) . ?
Si4 C12 1.868(4) . ?
C1 C2 1.491(5) . ?
C1 B5 1.563(6) . ?
C1 B6 1.743(5) . ?
C2 B3 1.571(6) . ?
C2 B6 1.737(6) . ?
B3 B4 1.650(6) . ?
B3 B6 1.777(6) . ?
B4 B5 1.649(6) . ?
B4 B6 1.738(7) . ?
B5 B6 1.770(6) . ?
C11 C12 1.492(5) . ?
C11 B15 1.571(5) . ?
C11 B16 1.744(5) . ?
C12 B13 1.568(6) . ?
C12 B16 1.751(5) . ?
B13 B14 1.649(6) . ?
B13 B16 1.775(6) . ?
B14 B15 1.658(6) . ?
B14 B16 1.742(6) . ?
B15 B16 1.763(6) . ?
N41 C46 1.448(8) . ?
N41 C45 1.456(6) . ?
N41 C43 1.467(9) . ?
N42 C44 1.434(8) . ?
N42 C48 1.453(6) . ?
N42 C47 1.457(6) . ?
C43 C44 1.225(9) . ?
N51 C53 1.453(6) . ?
N51 C56 1.463(5) . ?
N51 C55 1.482(6) . ?
N52 C58 1.461(5) . ?
N52 C57 1.468(5) . ?
N52 C54 1.481(6) . ?
C53 C54 1.399(7) . ?
N61 C65 1.455(6) . ?
N61 C66 1.457(6) . ?
N61 C63 1.471(6) . ?
N62 C64 1.450(6) . ?
N62 C67 1.468(5) . ?
N62 C68 1.482(6) . ?
C63 C64 1.409(8) . ?
C71 C73 1.355(7) 2_577 ?
C71 C72 1.375(7) . ?
C72 C73 1.368(7) . ?
C73 C71 1.355(7) 2_577 ?
|
1100796.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100796.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100796
loop_
_publ_author_name
'Tomlinson, Susan'
'Zheng, Chong'
'Hosmane, Narayan S.'
'Yang, Jimin'
'Wang, Ying'
'Zhang, Hongming'
'Gray, Thomas G.'
'Demissie, Temesgen'
'Maguire, John A.'
'Baumann, Frank'
'Klein, Axel'
'Sarkar, Biprajit'
'Kaim, Wolfgang'
'Lipscomb, William N.'
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural,
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2177
_journal_page_last 2187
_journal_paper_doi 10.1021/om048982u
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C14 H38 B4 Co N2 Si2'
_chemical_formula_weight 392.81
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 94.38(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.329(2)
_cell_length_b 19.648(6)
_cell_length_c 14.570(4)
_cell_measurement_reflns_used 30
_cell_measurement_temperature 230(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 10.0
_cell_volume 2377.4(11)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 230(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Siemens P3'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.000
_diffrn_reflns_av_sigmaI/netI 0.051
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 2566
_diffrn_reflns_theta_full 21.02
_diffrn_reflns_theta_max 21.02
_diffrn_reflns_theta_min 2.50
_diffrn_standards_decay_% n/a
_diffrn_standards_interval_count 200
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.821
_exptl_absorpt_correction_T_max 0.583
_exptl_absorpt_correction_T_min 0.544
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Siemens XEMP'
_exptl_crystal_colour dark-orange
_exptl_crystal_density_diffrn 1.097
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 844
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.287
_refine_diff_density_min -0.268
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef 0.0002(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 218
_refine_ls_number_reflns 2566
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.065
_refine_ls_R_factor_gt 0.041
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+1.2173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.089
_refine_ls_wR_factor_ref 0.101
_reflns_number_gt 1815
_reflns_number_total 2566
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060290
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100796
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.19564(7) 0.20324(3) 0.53046(4) 0.0390(2) Uani 1 1 d . . .
Si1 Si 0.29753(18) 0.37891(7) 0.45866(10) 0.0556(4) Uani 1 1 d . . .
Si2 Si 0.30362(19) 0.09058(7) 0.33742(10) 0.0584(5) Uani 1 1 d . . .
C1 C 0.3078(5) 0.2854(2) 0.4654(3) 0.0404(11) Uani 1 1 d . . .
B2 B 0.2255(6) 0.2342(3) 0.3960(4) 0.0426(14) Uani 1 1 d . . .
H2 H 0.1358 0.2462 0.3389 0.051 Uiso 1 1 calc R . .
C3 C 0.3107(5) 0.1641(2) 0.4147(3) 0.0388(11) Uani 1 1 d . . .
B4 B 0.4227(6) 0.1671(3) 0.5039(4) 0.0429(14) Uani 1 1 d . . .
H4 H 0.4953 0.1248 0.5343 0.051 Uiso 1 1 calc R . .
B5 B 0.4223(6) 0.2492(3) 0.5374(4) 0.0450(15) Uani 1 1 d . . .
H5 H 0.4950 0.2733 0.5946 0.054 Uiso 1 1 calc R . .
B6 B 0.4384(6) 0.2310(3) 0.4210(4) 0.0433(14) Uani 1 1 d . . .
H6 H 0.5390 0.2420 0.3786 0.052 Uiso 1 1 calc R . .
C7 C 0.1582(8) 0.4079(3) 0.3597(4) 0.100(2) Uani 1 1 d . . .
H7A H 0.0502 0.3942 0.3696 0.150 Uiso 1 1 calc R . .
H7B H 0.1900 0.3878 0.3039 0.150 Uiso 1 1 calc R . .
H7C H 0.1629 0.4566 0.3550 0.150 Uiso 1 1 calc R . .
C8 C 0.5021(7) 0.4124(3) 0.4413(4) 0.0802(19) Uani 1 1 d . . .
H8A H 0.4948 0.4598 0.4256 0.120 Uiso 1 1 calc R . .
H8B H 0.5467 0.3877 0.3923 0.120 Uiso 1 1 calc R . .
H8C H 0.5703 0.4069 0.4969 0.120 Uiso 1 1 calc R . .
C9 C 0.2319(7) 0.4141(3) 0.5670(4) 0.089(2) Uani 1 1 d . . .
H9A H 0.1249 0.3985 0.5758 0.134 Uiso 1 1 calc R . .
H9B H 0.2325 0.4629 0.5641 0.134 Uiso 1 1 calc R . .
H9C H 0.3040 0.3992 0.6175 0.134 Uiso 1 1 calc R . .
C10 C 0.1715(11) 0.1034(4) 0.2338(5) 0.179(5) Uani 1 1 d . . .
H10A H 0.1672 0.0624 0.1977 0.268 Uiso 1 1 calc R . .
H10B H 0.2121 0.1399 0.1984 0.268 Uiso 1 1 calc R . .
H10C H 0.0653 0.1146 0.2504 0.268 Uiso 1 1 calc R . .
C11 C 0.5123(8) 0.0717(4) 0.3046(5) 0.131(3) Uani 1 1 d . . .
H11A H 0.5105 0.0315 0.2671 0.197 Uiso 1 1 calc R . .
H11B H 0.5822 0.0646 0.3592 0.197 Uiso 1 1 calc R . .
H11C H 0.5510 0.1094 0.2707 0.197 Uiso 1 1 calc R . .
C12 C 0.2409(9) 0.0149(3) 0.3992(5) 0.113(3) Uani 1 1 d . . .
H12A H 0.1296 0.0191 0.4112 0.170 Uiso 1 1 calc R . .
H12B H 0.3054 0.0107 0.4564 0.170 Uiso 1 1 calc R . .
H12C H 0.2548 -0.0249 0.3622 0.170 Uiso 1 1 calc R . .
N21 N -0.0509(4) 0.2069(2) 0.5182(3) 0.0617(12) Uani 1 1 d . . .
N22 N 0.1724(5) 0.1674(2) 0.6577(3) 0.0624(12) Uani 1 1 d . . .
C23 C -0.1037(8) 0.1821(4) 0.6053(6) 0.128(3) Uani 1 1 d . . .
H23A H -0.1906 0.2112 0.6225 0.154 Uiso 1 1 calc R . .
H23B H -0.1483 0.1369 0.5949 0.154 Uiso 1 1 calc R . .
C24 C 0.0004(8) 0.1788(6) 0.6734(5) 0.164(5) Uani 1 1 d . . .
H24A H -0.0321 0.1424 0.7131 0.197 Uiso 1 1 calc R . .
H24B H -0.0059 0.2208 0.7078 0.197 Uiso 1 1 calc R . .
C25 C -0.1210(6) 0.1633(3) 0.4434(5) 0.108(3) Uani 1 1 d . . .
H25A H -0.0810 0.1178 0.4519 0.161 Uiso 1 1 calc R . .
H25B H -0.0917 0.1806 0.3854 0.161 Uiso 1 1 calc R . .
H25C H -0.2362 0.1632 0.4442 0.161 Uiso 1 1 calc R . .
C26 C -0.1083(6) 0.2766(3) 0.5016(4) 0.0723(17) Uani 1 1 d . . .
H26A H -0.0720 0.2928 0.4446 0.108 Uiso 1 1 calc R . .
H26B H -0.0667 0.3054 0.5510 0.108 Uiso 1 1 calc R . .
H26C H -0.2238 0.2772 0.4983 0.108 Uiso 1 1 calc R . .
C27 C 0.2181(11) 0.0965(3) 0.6654(5) 0.140(3) Uani 1 1 d . . .
H27A H 0.3283 0.0915 0.6517 0.209 Uiso 1 1 calc R . .
H27B H 0.1503 0.0701 0.6228 0.209 Uiso 1 1 calc R . .
H27C H 0.2059 0.0810 0.7270 0.209 Uiso 1 1 calc R . .
C28 C 0.2663(7) 0.2057(3) 0.7290(3) 0.089(2) Uani 1 1 d . . .
H28A H 0.2426 0.1893 0.7885 0.133 Uiso 1 1 calc R . .
H28B H 0.2391 0.2531 0.7238 0.133 Uiso 1 1 calc R . .
H28C H 0.3790 0.1999 0.7215 0.133 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0277(4) 0.0447(4) 0.0447(4) 0.0055(3) 0.0033(3) -0.0042(3)
Si1 0.0663(10) 0.0359(8) 0.0661(10) -0.0033(7) 0.0141(8) -0.0091(8)
Si2 0.0775(11) 0.0406(9) 0.0564(9) -0.0072(7) 0.0005(8) -0.0029(8)
C1 0.036(2) 0.042(3) 0.043(3) 0.002(2) 0.007(2) -0.006(2)
B2 0.040(3) 0.043(3) 0.044(3) 0.000(3) 0.002(3) -0.006(3)
C3 0.039(3) 0.039(3) 0.038(3) 0.002(2) 0.004(2) -0.004(2)
B4 0.037(3) 0.047(3) 0.045(4) 0.003(3) 0.007(3) 0.004(3)
B5 0.035(3) 0.054(4) 0.046(4) -0.002(3) 0.003(3) -0.008(3)
B6 0.038(3) 0.045(3) 0.048(3) 0.001(3) 0.012(3) -0.005(3)
C7 0.121(6) 0.051(4) 0.125(6) 0.032(4) -0.014(4) 0.005(4)
C8 0.102(5) 0.054(4) 0.090(4) -0.018(3) 0.045(4) -0.033(3)
C9 0.096(5) 0.061(4) 0.116(5) -0.028(4) 0.048(4) -0.017(3)
C10 0.300(12) 0.110(6) 0.107(6) -0.052(5) -0.116(7) 0.078(7)
C11 0.128(6) 0.120(6) 0.153(7) -0.076(5) 0.056(5) -0.012(5)
C12 0.156(7) 0.046(4) 0.142(6) -0.014(4) 0.034(5) -0.025(4)
N21 0.035(2) 0.067(3) 0.084(3) 0.028(3) 0.011(2) 0.001(2)
N22 0.047(3) 0.094(4) 0.047(3) 0.002(3) 0.010(2) -0.009(3)
C23 0.055(4) 0.177(8) 0.159(8) 0.097(7) 0.047(5) 0.024(5)
C24 0.044(4) 0.393(16) 0.058(4) 0.026(7) 0.017(4) -0.048(6)
C25 0.037(3) 0.083(5) 0.199(8) -0.026(5) -0.013(4) -0.012(3)
C26 0.037(3) 0.074(4) 0.105(5) 0.008(4) 0.003(3) 0.001(3)
C27 0.254(11) 0.085(6) 0.086(5) 0.044(4) 0.055(6) -0.006(6)
C28 0.079(4) 0.143(6) 0.045(3) 0.000(4) 0.004(3) -0.008(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt1 Co N21 135.4 . . y
Cnt1 Co N22 138.8 . . y
N22 Co N21 85.75(17) . . ?
N22 Co B4 101.84(19) . . ?
N21 Co B4 156.0(2) . . ?
N22 Co B2 176.3(2) . . ?
N21 Co B2 95.65(19) . . ?
B4 Co B2 75.5(2) . . ?
N22 Co B5 104.94(19) . . ?
N21 Co B5 152.3(2) . . ?
B4 Co B5 47.7(2) . . ?
B2 Co B5 75.3(2) . . ?
N22 Co C1 139.10(18) . . ?
N21 Co C1 113.97(17) . . ?
B4 Co C1 74.93(19) . . ?
B2 Co C1 43.16(18) . . ?
B5 Co C1 42.80(18) . . ?
N22 Co C3 132.95(18) . . ?
N21 Co C3 116.70(18) . . ?
B4 Co C3 42.72(18) . . ?
B2 Co C3 43.38(18) . . ?
B5 Co C3 74.71(19) . . ?
C1 Co C3 71.54(16) . . ?
C1 Si1 C9 110.1(2) . . ?
C1 Si1 C8 108.7(2) . . ?
C9 Si1 C8 108.6(3) . . ?
C1 Si1 C7 111.7(2) . . ?
C9 Si1 C7 109.8(3) . . ?
C8 Si1 C7 107.9(3) . . ?
C10 Si2 C3 113.0(3) . . ?
C10 Si2 C12 110.0(4) . . ?
C3 Si2 C12 109.6(3) . . ?
C10 Si2 C11 109.3(4) . . ?
C3 Si2 C11 109.0(2) . . ?
C12 Si2 C11 105.6(3) . . ?
B5 C1 B2 111.5(4) . . ?
B5 C1 B6 65.4(3) . . ?
B2 C1 B6 66.7(3) . . ?
B5 C1 Si1 121.4(3) . . ?
B2 C1 Si1 126.6(3) . . ?
B6 C1 Si1 129.7(3) . . ?
B5 C1 Co 67.4(2) . . ?
B2 C1 Co 67.1(2) . . ?
B6 C1 Co 90.5(3) . . ?
Si1 C1 Co 139.6(2) . . ?
C1 B2 C3 106.6(4) . . ?
C1 B2 B6 60.4(3) . . ?
C3 B2 B6 60.2(3) . . ?
C1 B2 Co 69.8(3) . . ?
C3 B2 Co 70.4(3) . . ?
B6 B2 Co 89.2(3) . . ?
B4 C3 B2 110.6(4) . . ?
B4 C3 B6 65.6(3) . . ?
B2 C3 B6 66.4(3) . . ?
B4 C3 Si2 122.5(3) . . ?
B2 C3 Si2 126.5(3) . . ?
B6 C3 Si2 129.7(3) . . ?
B4 C3 Co 66.5(2) . . ?
B2 C3 Co 66.3(2) . . ?
B6 C3 Co 89.7(3) . . ?
Si2 C3 Co 140.5(2) . . ?
C3 B4 B5 105.4(4) . . ?
C3 B4 B6 61.2(3) . . ?
B5 B4 B6 61.0(3) . . ?
C3 B4 Co 70.7(3) . . ?
B5 B4 Co 66.3(3) . . ?
B6 B4 Co 90.0(3) . . ?
C1 B5 B4 105.1(4) . . ?
C1 B5 B6 61.4(3) . . ?
B4 B5 B6 61.4(3) . . ?
C1 B5 Co 69.8(3) . . ?
B4 B5 Co 66.0(3) . . ?
B6 B5 Co 90.0(3) . . ?
C1 B6 C3 95.3(3) . . ?
C1 B6 B5 53.1(3) . . ?
C3 B6 B5 96.7(3) . . ?
C1 B6 B4 96.1(3) . . ?
C3 B6 B4 53.1(3) . . ?
B5 B6 B4 57.6(3) . . ?
C1 B6 B2 52.9(3) . . ?
C3 B6 B2 53.4(3) . . ?
B5 B6 B2 92.4(3) . . ?
B4 B6 B2 92.3(3) . . ?
C23 N21 C26 109.9(5) . . ?
C23 N21 C25 108.7(5) . . ?
C26 N21 C25 108.4(4) . . ?
C23 N21 Co 106.2(3) . . ?
C26 N21 Co 111.1(3) . . ?
C25 N21 Co 112.5(3) . . ?
C27 N22 C28 108.5(5) . . ?
C27 N22 C24 112.6(6) . . ?
C28 N22 C24 106.5(5) . . ?
C27 N22 Co 111.5(4) . . ?
C28 N22 Co 113.1(3) . . ?
C24 N22 Co 104.7(4) . . ?
C24 C23 N21 117.7(6) . . ?
C23 C24 N22 119.8(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co Cnt1 1.624 . y
Co C1 2.124(4) . y
Co B2 2.084(5) . y
Co C3 2.145(4) . y
Co B4 2.084(5) . y
Co B5 2.088(5) . y
Co N21 2.049(4) . y
Co N22 2.006(4) . y
Si1 C1 1.842(4) . ?
Si1 C9 1.844(5) . ?
Si1 C8 1.862(5) . ?
Si1 C7 1.869(6) . ?
Si2 C10 1.817(6) . ?
Si2 C3 1.830(4) . ?
Si2 C12 1.835(6) . ?
Si2 C11 1.874(6) . ?
C1 B5 1.537(7) . ?
C1 B2 1.548(7) . ?
C1 B6 1.688(7) . ?
B2 C3 1.564(7) . ?
B2 B6 1.784(7) . ?
C3 B4 1.541(7) . ?
C3 B6 1.689(7) . ?
B4 B5 1.686(8) . ?
B4 B6 1.754(8) . ?
B5 B6 1.748(8) . ?
N21 C23 1.459(7) . ?
N21 C26 1.464(6) . ?
N21 C25 1.471(7) . ?
N22 C27 1.446(7) . ?
N22 C28 1.460(6) . ?
N22 C24 1.484(7) . ?
C23 C24 1.269(8) . ?
|
1100797.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100797.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100797
loop_
_publ_author_name
'Tomlinson, Susan'
'Zheng, Chong'
'Hosmane, Narayan S.'
'Yang, Jimin'
'Wang, Ying'
'Zhang, Hongming'
'Gray, Thomas G.'
'Demissie, Temesgen'
'Maguire, John A.'
'Baumann, Frank'
'Klein, Axel'
'Sarkar, Biprajit'
'Kaim, Wolfgang'
'Lipscomb, William N.'
_publ_section_title
;
Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 31. New Insights
into Reaction Pathways of Carborane Ligand Systems: Synthetic, Structural,
Spectroscopic, and Electrochemical Studies on Sandwich and Half-Sandwich
Metallacarboranes of Iron, Cobalt, and Nickel
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2177
_journal_page_last 2187
_journal_paper_doi 10.1021/om048982u
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C21 H55 B8 N2 Ni Si4'
_chemical_formula_weight 593.22
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 112.33(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 17.788(5)
_cell_length_b 10.130(2)
_cell_length_c 21.049(5)
_cell_measurement_reflns_used 30
_cell_measurement_temperature 230(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 10.0
_cell_volume 3508.4(15)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 230(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Siemens P3'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.017
_diffrn_reflns_av_sigmaI/netI 0.032
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -2
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 4475
_diffrn_reflns_theta_full 22.00
_diffrn_reflns_theta_max 22.00
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% n/a
_diffrn_standards_interval_count 200
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.704
_exptl_absorpt_correction_T_max 0.899
_exptl_absorpt_correction_T_min 0.802
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'Siemens XEMP'
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.123
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 1276
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.563
_refine_diff_density_min -0.214
_refine_diff_density_rms 0.047
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.034
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 340
_refine_ls_number_reflns 4308
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.034
_refine_ls_R_factor_all 0.051
_refine_ls_R_factor_gt 0.034
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+2.5132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.080
_refine_ls_wR_factor_ref 0.089
_reflns_number_gt 3488
_reflns_number_total 4308
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060291
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100797
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.72816(2) 0.13974(4) 0.261017(19) 0.02664(14) Uani 1 1 d . . .
Si1 Si 0.81991(7) -0.10587(10) 0.41327(5) 0.0457(3) Uani 1 1 d . . .
Si2 Si 0.72475(6) -0.07295(10) 0.11620(5) 0.0425(3) Uani 1 1 d . . .
Si3 Si 0.92885(6) 0.33543(10) 0.30213(6) 0.0472(3) Uani 1 1 d . . .
Si4 Si 0.59347(6) 0.37828(10) 0.12039(5) 0.0413(3) Uani 1 1 d . . .
C1 C 0.76194(19) -0.0412(3) 0.32575(16) 0.0319(8) Uani 1 1 d . . .
B2 B 0.7933(2) -0.0416(4) 0.26692(19) 0.0327(9) Uani 1 1 d . . .
H2 H 0.8565 -0.0599 0.2724 0.039 Uiso 1 1 calc R . .
C3 C 0.71535(18) -0.0286(3) 0.19823(15) 0.0310(7) Uani 1 1 d . . .
B4 B 0.6370(2) -0.0038(4) 0.2114(2) 0.0348(9) Uani 1 1 d . . .
H4 H 0.5747 0.0048 0.1730 0.042 Uiso 1 1 calc R . .
B5 B 0.6701(2) -0.0032(4) 0.2990(2) 0.0353(9) Uani 1 1 d . . .
H5 H 0.6341 0.0091 0.3311 0.042 Uiso 1 1 calc R . .
B6 B 0.7015(2) -0.1298(4) 0.25772(19) 0.0364(9) Uani 1 1 d . . .
H6 H 0.6877 -0.2360 0.2551 0.044 Uiso 1 1 calc R . .
C11 C 0.81980(18) 0.3009(3) 0.28530(16) 0.0311(8) Uani 1 1 d . . .
B12 B 0.7594(2) 0.2907(4) 0.20744(19) 0.0323(9) Uani 1 1 d . . .
H12 H 0.7772 0.2798 0.1631 0.039 Uiso 1 1 calc R . .
C13 C 0.67107(18) 0.3235(3) 0.20407(15) 0.0304(7) Uani 1 1 d . . .
B14 B 0.6746(2) 0.3105(3) 0.27791(18) 0.0281(8) Uani 1 1 d . . .
B15 B 0.7734(2) 0.3061(3) 0.33382(19) 0.0310(9) Uani 1 1 d . . .
B16 B 0.7442(2) 0.4166(4) 0.26126(19) 0.0321(9) Uani 1 1 d . . .
H16 H 0.7490 0.5248 0.2613 0.038 Uiso 1 1 calc R . .
C21 C 0.9290(3) -0.1234(5) 0.4285(2) 0.0928(17) Uani 1 1 d . . .
H21A H 0.9523 -0.0376 0.4296 0.139 Uiso 1 1 calc R . .
H21B H 0.9346 -0.1747 0.3922 0.139 Uiso 1 1 calc R . .
H21C H 0.9565 -0.1670 0.4716 0.139 Uiso 1 1 calc R . .
C22 C 0.8071(4) -0.0006(4) 0.4800(2) 0.0933(18) Uani 1 1 d . . .
H22A H 0.8383 -0.0362 0.5246 0.140 Uiso 1 1 calc R . .
H22B H 0.7507 0.0020 0.4736 0.140 Uiso 1 1 calc R . .
H22C H 0.8256 0.0872 0.4766 0.140 Uiso 1 1 calc R . .
C23 C 0.7799(3) -0.2726(4) 0.4201(2) 0.0769(14) Uani 1 1 d . . .
H23A H 0.8091 -0.3076 0.4652 0.115 Uiso 1 1 calc R . .
H23B H 0.7868 -0.3301 0.3864 0.115 Uiso 1 1 calc R . .
H23C H 0.7232 -0.2663 0.4122 0.115 Uiso 1 1 calc R . .
C24 C 0.6322(2) -0.0242(5) 0.04144(19) 0.0743(14) Uani 1 1 d . . .
H24A H 0.6381 -0.0499 -0.0003 0.111 Uiso 1 1 calc R . .
H24B H 0.6252 0.0697 0.0417 0.111 Uiso 1 1 calc R . .
H24C H 0.5856 -0.0673 0.0444 0.111 Uiso 1 1 calc R . .
C25 C 0.8145(2) 0.0097(4) 0.10985(18) 0.0555(10) Uani 1 1 d . . .
H25A H 0.8617 -0.0096 0.1502 0.083 Uiso 1 1 calc R . .
H25B H 0.8057 0.1033 0.1062 0.083 Uiso 1 1 calc R . .
H25C H 0.8227 -0.0219 0.0699 0.083 Uiso 1 1 calc R . .
C26 C 0.7398(4) -0.2533(4) 0.1151(3) 0.0953(18) Uani 1 1 d . . .
H26A H 0.7881 -0.2778 0.1533 0.143 Uiso 1 1 calc R . .
H26B H 0.7454 -0.2778 0.0730 0.143 Uiso 1 1 calc R . .
H26C H 0.6938 -0.2979 0.1184 0.143 Uiso 1 1 calc R . .
C27 C 0.9538(3) 0.4995(4) 0.3446(3) 0.0913(17) Uani 1 1 d . . .
H27A H 0.9469 0.4965 0.3876 0.137 Uiso 1 1 calc R . .
H27B H 0.9183 0.5651 0.3155 0.137 Uiso 1 1 calc R . .
H27C H 1.0092 0.5215 0.3525 0.137 Uiso 1 1 calc R . .
C28 C 0.9468(3) 0.3448(5) 0.2212(2) 0.0902(16) Uani 1 1 d . . .
H28A H 1.0028 0.3658 0.2313 0.135 Uiso 1 1 calc R . .
H28B H 0.9129 0.4121 0.1922 0.135 Uiso 1 1 calc R . .
H28C H 0.9341 0.2613 0.1979 0.135 Uiso 1 1 calc R . .
C29 C 0.9963(2) 0.2045(5) 0.3553(3) 0.0835(15) Uani 1 1 d . . .
H29A H 0.9765 0.1197 0.3357 0.125 Uiso 1 1 calc R . .
H29B H 0.9972 0.2087 0.4011 0.125 Uiso 1 1 calc R . .
H29C H 1.0504 0.2171 0.3565 0.125 Uiso 1 1 calc R . .
C30 C 0.5047(2) 0.2642(4) 0.0876(2) 0.0656(12) Uani 1 1 d . . .
H30A H 0.4708 0.2885 0.0415 0.098 Uiso 1 1 calc R . .
H30B H 0.4739 0.2702 0.1164 0.098 Uiso 1 1 calc R . .
H30C H 0.5235 0.1753 0.0881 0.098 Uiso 1 1 calc R . .
C31 C 0.5531(2) 0.5449(4) 0.12811(19) 0.0595(11) Uani 1 1 d . . .
H31A H 0.5964 0.5989 0.1581 0.089 Uiso 1 1 calc R . .
H31B H 0.5116 0.5363 0.1466 0.089 Uiso 1 1 calc R . .
H31C H 0.5304 0.5853 0.0836 0.089 Uiso 1 1 calc R . .
C32 C 0.6399(3) 0.3907(4) 0.05514(18) 0.0647(12) Uani 1 1 d . . .
H32A H 0.6546 0.3042 0.0452 0.097 Uiso 1 1 calc R . .
H32B H 0.6876 0.4451 0.0726 0.097 Uiso 1 1 calc R . .
H32C H 0.6016 0.4292 0.0139 0.097 Uiso 1 1 calc R . .
N41 N 0.61168(14) 0.3450(2) 0.31051(13) 0.0324(6) Uani 1 1 d . . .
N42 N 0.79170(15) 0.3203(3) 0.40539(13) 0.0381(7) Uani 1 1 d . . .
C43 C 0.6457(2) 0.2973(3) 0.38409(16) 0.0409(9) Uani 1 1 d . . .
H43A H 0.6071 0.3187 0.4049 0.049 Uiso 1 1 calc R . .
H43B H 0.6503 0.2019 0.3839 0.049 Uiso 1 1 calc R . .
C44 C 0.7271(2) 0.3530(3) 0.42846(17) 0.0433(9) Uani 1 1 d . . .
H44A H 0.7226 0.4483 0.4297 0.052 Uiso 1 1 calc R . .
H44B H 0.7414 0.3205 0.4749 0.052 Uiso 1 1 calc R . .
C45 C 0.5989(2) 0.4911(3) 0.30903(19) 0.0457(9) Uani 1 1 d . . .
H45A H 0.5753 0.5206 0.2622 0.069 Uiso 1 1 calc R . .
H45B H 0.6501 0.5344 0.3319 0.069 Uiso 1 1 calc R . .
H45C H 0.5630 0.5120 0.3320 0.069 Uiso 1 1 calc R . .
C46 C 0.53209(19) 0.2794(4) 0.27416(19) 0.0464(9) Uani 1 1 d . . .
H46A H 0.4968 0.2966 0.2982 0.070 Uiso 1 1 calc R . .
H46B H 0.5401 0.1860 0.2725 0.070 Uiso 1 1 calc R . .
H46C H 0.5079 0.3134 0.2282 0.070 Uiso 1 1 calc R . .
C47 C 0.8725(2) 0.3357(4) 0.45844(18) 0.0628(12) Uani 1 1 d . . .
H47A H 0.9118 0.2950 0.4437 0.094 Uiso 1 1 calc R . .
H47B H 0.8742 0.2945 0.5000 0.094 Uiso 1 1 calc R . .
H47C H 0.8847 0.4280 0.4666 0.094 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0263(2) 0.0235(2) 0.0331(2) -0.00045(18) 0.01465(18) -0.00096(18)
Si1 0.0638(7) 0.0342(6) 0.0368(6) 0.0044(5) 0.0164(5) -0.0007(5)
Si2 0.0507(6) 0.0423(6) 0.0412(6) -0.0109(5) 0.0249(5) -0.0080(5)
Si3 0.0263(5) 0.0456(6) 0.0721(7) -0.0002(5) 0.0214(5) -0.0036(5)
Si4 0.0390(6) 0.0421(6) 0.0362(5) 0.0017(5) 0.0068(4) 0.0018(5)
C1 0.042(2) 0.0213(17) 0.0368(19) -0.0004(14) 0.0194(16) -0.0005(15)
B2 0.032(2) 0.025(2) 0.041(2) -0.0014(17) 0.0152(18) 0.0007(17)
C3 0.0353(18) 0.0244(17) 0.0355(19) -0.0013(15) 0.0159(15) -0.0052(14)
B4 0.034(2) 0.027(2) 0.044(2) 0.0001(18) 0.0151(18) -0.0065(17)
B5 0.042(2) 0.024(2) 0.046(2) 0.0013(18) 0.025(2) -0.0018(17)
B6 0.042(2) 0.029(2) 0.042(2) -0.0023(18) 0.0203(19) -0.0063(18)
C11 0.0257(18) 0.0226(17) 0.047(2) 0.0018(15) 0.0160(15) -0.0008(14)
B12 0.037(2) 0.025(2) 0.040(2) 0.0013(17) 0.0197(19) 0.0012(17)
C13 0.0304(18) 0.0243(17) 0.0370(18) -0.0006(14) 0.0135(15) -0.0020(14)
B14 0.027(2) 0.0237(19) 0.036(2) -0.0018(16) 0.0155(17) -0.0013(16)
B15 0.027(2) 0.022(2) 0.045(2) -0.0009(17) 0.0144(18) -0.0016(16)
B16 0.029(2) 0.024(2) 0.043(2) 0.0014(18) 0.0140(18) -0.0007(16)
C21 0.063(3) 0.128(5) 0.067(3) 0.031(3) 0.002(2) 0.006(3)
C22 0.180(6) 0.059(3) 0.047(3) 0.002(2) 0.051(3) 0.019(3)
C23 0.115(4) 0.047(3) 0.061(3) 0.017(2) 0.025(3) -0.013(3)
C24 0.062(3) 0.113(4) 0.040(2) -0.018(2) 0.011(2) -0.014(3)
C25 0.053(2) 0.078(3) 0.044(2) -0.001(2) 0.0281(19) -0.003(2)
C26 0.169(5) 0.052(3) 0.113(4) -0.018(3) 0.108(4) -0.008(3)
C27 0.055(3) 0.065(3) 0.156(5) -0.029(3) 0.043(3) -0.025(2)
C28 0.055(3) 0.128(5) 0.108(4) 0.003(3) 0.054(3) -0.015(3)
C29 0.041(2) 0.086(4) 0.119(4) 0.014(3) 0.024(3) 0.016(2)
C30 0.051(3) 0.068(3) 0.057(3) -0.003(2) -0.004(2) -0.011(2)
C31 0.060(3) 0.055(3) 0.051(2) 0.008(2) 0.007(2) 0.011(2)
C32 0.073(3) 0.080(3) 0.036(2) 0.008(2) 0.015(2) 0.005(2)
N41 0.0296(15) 0.0293(15) 0.0435(16) -0.0023(13) 0.0198(13) 0.0017(12)
N42 0.0332(16) 0.0443(17) 0.0319(16) -0.0052(13) 0.0068(13) -0.0022(13)
C43 0.047(2) 0.041(2) 0.045(2) -0.0013(17) 0.0286(18) -0.0014(17)
C44 0.051(2) 0.042(2) 0.039(2) -0.0063(17) 0.0189(18) -0.0029(18)
C45 0.047(2) 0.032(2) 0.067(2) -0.0010(18) 0.032(2) 0.0092(17)
C46 0.0280(19) 0.050(2) 0.065(2) -0.0062(19) 0.0221(18) -0.0054(17)
C47 0.050(2) 0.086(3) 0.044(2) -0.006(2) 0.0073(19) 0.000(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B14 Ni B12 73.50(14) . . ?
B14 Ni B5 100.68(14) . . ?
B12 Ni B5 167.09(15) . . ?
B14 Ni C3 146.46(13) . . ?
B12 Ni C3 103.87(13) . . ?
B5 Ni C3 74.39(13) . . ?
B14 Ni B4 109.87(14) . . ?
B12 Ni B4 122.79(15) . . ?
B5 Ni B4 47.57(15) . . ?
C3 Ni B4 42.55(13) . . ?
B14 Ni B2 167.75(14) . . ?
B12 Ni B2 114.01(14) . . ?
B5 Ni B2 73.87(14) . . ?
C3 Ni B2 43.57(13) . . ?
B4 Ni B2 74.87(14) . . ?
B14 Ni B15 46.75(13) . . ?
B12 Ni B15 73.50(14) . . ?
B5 Ni B15 111.27(14) . . ?
C3 Ni B15 166.05(12) . . ?
B4 Ni B15 150.12(14) . . ?
B2 Ni B15 124.33(14) . . ?
B14 Ni C11 72.08(12) . . ?
B12 Ni C11 42.91(13) . . ?
B5 Ni C11 147.13(14) . . ?
C3 Ni C11 129.08(11) . . ?
B4 Ni C11 165.29(13) . . ?
B2 Ni C11 106.34(13) . . ?
B15 Ni C11 40.56(12) . . ?
B14 Ni C1 128.16(13) . . ?
B12 Ni C1 149.87(13) . . ?
B5 Ni C1 42.13(13) . . ?
C3 Ni C1 70.03(12) . . ?
B4 Ni C1 73.53(13) . . ?
B2 Ni C1 41.15(12) . . ?
B15 Ni C1 105.11(12) . . ?
C11 Ni C1 117.37(11) . . ?
B14 Ni C13 41.58(12) . . ?
B12 Ni C13 42.61(12) . . ?
B5 Ni C13 125.97(13) . . ?
C3 Ni C13 114.62(12) . . ?
B4 Ni C13 101.48(13) . . ?
B2 Ni C13 150.04(13) . . ?
B15 Ni C13 73.09(12) . . ?
C11 Ni C13 69.91(11) . . ?
C1 Ni C13 167.12(11) . . ?
C22 Si1 C21 110.4(3) . . ?
C22 Si1 C1 111.66(18) . . ?
C21 Si1 C1 110.88(17) . . ?
C22 Si1 C23 107.7(2) . . ?
C21 Si1 C23 107.8(2) . . ?
C1 Si1 C23 108.23(17) . . ?
C26 Si2 C3 108.43(18) . . ?
C26 Si2 C25 108.2(2) . . ?
C3 Si2 C25 110.09(15) . . ?
C26 Si2 C24 109.7(2) . . ?
C3 Si2 C24 111.08(17) . . ?
C25 Si2 C24 109.22(19) . . ?
C28 Si3 C29 107.0(2) . . ?
C28 Si3 C27 107.7(2) . . ?
C29 Si3 C27 111.6(2) . . ?
C28 Si3 C11 111.41(18) . . ?
C29 Si3 C11 111.62(18) . . ?
C27 Si3 C11 107.46(17) . . ?
C32 Si4 C13 109.97(16) . . ?
C32 Si4 C30 108.71(19) . . ?
C13 Si4 C30 112.63(16) . . ?
C32 Si4 C31 107.32(19) . . ?
C13 Si4 C31 111.02(15) . . ?
C30 Si4 C31 107.00(19) . . ?
B2 C1 B5 111.1(3) . . ?
B2 C1 B6 68.0(2) . . ?
B5 C1 B6 65.4(2) . . ?
B2 C1 Si1 124.3(2) . . ?
B5 C1 Si1 123.8(2) . . ?
B6 C1 Si1 126.2(2) . . ?
B2 C1 Ni 66.77(17) . . ?
B5 C1 Ni 64.77(17) . . ?
B6 C1 Ni 88.96(19) . . ?
Si1 C1 Ni 144.81(17) . . ?
C1 B2 C3 105.9(3) . . ?
C1 B2 B6 59.9(2) . . ?
C3 B2 B6 60.0(2) . . ?
C1 B2 Ni 72.07(18) . . ?
C3 B2 Ni 67.08(17) . . ?
B6 B2 Ni 88.3(2) . . ?
B4 C3 B2 112.8(3) . . ?
B4 C3 B6 64.8(2) . . ?
B2 C3 B6 66.5(2) . . ?
B4 C3 Si2 128.0(2) . . ?
B2 C3 Si2 118.2(2) . . ?
B6 C3 Si2 128.9(2) . . ?
B4 C3 Ni 69.28(18) . . ?
B2 C3 Ni 69.35(17) . . ?
B6 C3 Ni 92.14(19) . . ?
Si2 C3 Ni 138.68(16) . . ?
C3 B4 B5 103.3(3) . . ?
C3 B4 B6 62.2(2) . . ?
B5 B4 B6 61.1(2) . . ?
C3 B4 Ni 68.17(17) . . ?
B5 B4 Ni 65.37(18) . . ?
B6 B4 Ni 90.5(2) . . ?
C1 B5 B4 105.8(3) . . ?
C1 B5 B6 60.8(2) . . ?
B4 B5 B6 60.5(2) . . ?
C1 B5 Ni 73.10(18) . . ?
B4 B5 Ni 67.06(17) . . ?
B6 B5 Ni 91.2(2) . . ?
C1 B6 C3 94.6(2) . . ?
C1 B6 B4 99.0(3) . . ?
C3 B6 B4 53.03(19) . . ?
C1 B6 B5 53.9(2) . . ?
C3 B6 B5 94.9(3) . . ?
B4 B6 B5 58.4(2) . . ?
C1 B6 B2 52.18(19) . . ?
C3 B6 B2 53.50(19) . . ?
B4 B6 B2 94.2(2) . . ?
B5 B6 B2 91.7(2) . . ?
B15 C11 B12 111.4(3) . . ?
B15 C11 B16 67.2(2) . . ?
B12 C11 B16 65.8(2) . . ?
B15 C11 Si3 130.4(2) . . ?
B12 C11 Si3 117.1(2) . . ?
B16 C11 Si3 124.8(2) . . ?
B15 C11 Ni 69.32(17) . . ?
B12 C11 Ni 64.22(16) . . ?
B16 C11 Ni 90.56(18) . . ?
Si3 C11 Ni 142.99(16) . . ?
C13 B12 C11 107.7(3) . . ?
C13 B12 B16 59.6(2) . . ?
C11 B12 B16 60.4(2) . . ?
C13 B12 Ni 73.48(18) . . ?
C11 B12 Ni 72.87(18) . . ?
B16 B12 Ni 92.6(2) . . ?
B14 C13 B12 106.2(3) . . ?
B14 C13 B16 66.5(2) . . ?
B12 C13 B16 66.5(2) . . ?
B14 C13 Si4 135.5(2) . . ?
B12 C13 Si4 118.2(2) . . ?
B16 C13 Si4 127.1(2) . . ?
B14 C13 Ni 63.34(17) . . ?
B12 C13 Ni 63.90(17) . . ?
B16 C13 Ni 90.72(18) . . ?
Si4 C13 Ni 140.97(16) . . ?
C13 B14 N41 131.7(3) . . ?
C13 B14 B15 109.6(3) . . ?
N41 B14 B15 115.3(3) . . ?
C13 B14 B16 60.7(2) . . ?
N41 B14 B16 128.6(3) . . ?
B15 B14 B16 62.5(2) . . ?
C13 B14 Ni 75.07(18) . . ?
N41 B14 Ni 135.8(2) . . ?
B15 B14 Ni 71.06(17) . . ?
B16 B14 Ni 94.06(19) . . ?
N42 B15 C11 137.9(3) . . ?
N42 B15 B14 119.3(3) . . ?
C11 B15 B14 102.4(3) . . ?
N42 B15 B16 135.3(3) . . ?
C11 B15 B16 60.9(2) . . ?
B14 B15 B16 60.6(2) . . ?
N42 B15 Ni 133.4(2) . . ?
C11 B15 Ni 70.12(18) . . ?
B14 B15 Ni 62.20(16) . . ?
B16 B15 Ni 88.52(19) . . ?
C13 B16 C11 97.8(2) . . ?
C13 B16 B14 52.73(19) . . ?
C11 B16 B14 93.2(2) . . ?
C13 B16 B12 53.95(19) . . ?
C11 B16 B12 53.78(19) . . ?
B14 B16 B12 88.7(2) . . ?
C13 B16 B15 98.8(2) . . ?
C11 B16 B15 51.87(18) . . ?
B14 B16 B15 56.93(19) . . ?
B12 B16 B15 91.7(2) . . ?
C46 N41 C45 108.9(3) . . ?
C46 N41 C43 108.5(2) . . ?
C45 N41 C43 109.6(3) . . ?
C46 N41 B14 112.1(2) . . ?
C45 N41 B14 110.0(2) . . ?
C43 N41 B14 107.7(2) . . ?
B15 N42 C44 119.2(3) . . ?
B15 N42 C47 125.8(3) . . ?
C44 N42 C47 113.4(3) . . ?
C44 C43 N41 115.6(3) . . ?
N42 C44 C43 113.9(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni C1 2.226(3) . y
Ni B2 2.150(4) . y
Ni C3 2.116(3) . y
Ni B4 2.132(4) . y
Ni B5 2.105(4) . y
Ni C11 2.225(3) . y
Ni B12 2.096(4) . y
Ni C13 2.238(3) . y
Ni B14 2.070(3) . y
Ni B15 2.213(4) . y
Si1 C22 1.846(4) . ?
Si1 C21 1.850(5) . ?
Si1 C1 1.855(3) . ?
Si1 C23 1.860(4) . ?
Si2 C26 1.848(4) . ?
Si2 C3 1.852(3) . ?
Si2 C25 1.852(4) . ?
Si2 C24 1.861(4) . ?
Si3 C28 1.852(4) . ?
Si3 C29 1.852(4) . ?
Si3 C27 1.859(4) . ?
Si3 C11 1.868(3) . ?
Si4 C32 1.857(4) . ?
Si4 C13 1.862(3) . ?
Si4 C30 1.865(4) . ?
Si4 C31 1.866(4) . ?
C1 B2 1.540(5) . ?
C1 B5 1.561(5) . ?
C1 B6 1.686(5) . ?
B2 C3 1.584(5) . ?
B2 B6 1.807(5) . ?
C3 B4 1.542(5) . ?
C3 B6 1.707(5) . ?
B4 B5 1.709(6) . ?
B4 B6 1.746(5) . ?
B5 B6 1.756(5) . ?
C11 B15 1.539(5) . ?
C11 B12 1.585(5) . ?
C11 B16 1.709(5) . ?
B12 C13 1.581(5) . ?
B12 B16 1.793(5) . ?
C13 B14 1.537(5) . ?
C13 B16 1.685(5) . ?
B14 N41 1.559(4) . ?
B14 B15 1.704(5) . ?
B14 B16 1.772(5) . ?
B15 N42 1.422(4) . ?
B15 B16 1.803(5) . ?
N41 C46 1.486(4) . ?
N41 C45 1.495(4) . ?
N41 C43 1.512(4) . ?
N42 C44 1.447(4) . ?
N42 C47 1.455(4) . ?
C43 C44 1.503(5) . ?
|
1100798.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100798.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100798
loop_
_publ_author_name
'Cano, Jes\'us'
'Sudupe, Mar\'ia'
'Royo, Pascual'
'Mosquera, Marta E. G.'
_publ_section_title
;
Insertion Reactions into the Metal--Alkyl and Metal--Amido Bonds of
1,3-Di(silyl-\h-amido)cyclopentadienyl Titanium and Zirconium Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2424
_journal_page_last 2432
_journal_paper_doi 10.1021/om048984e
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C18 H36 N2 Si2 Zr1'
_chemical_formula_sum 'C18 H36 N2 Si2 Zr'
_chemical_formula_weight 427.89
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 108.131(12)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.3691(15)
_cell_length_b 13.9028(9)
_cell_length_c 15.137(2)
_cell_measurement_reflns_used 87
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 20.963
_cell_measurement_theta_min 3.315
_cell_volume 2273.8(4)
_diffrn_ambient_temperature 200(2)
_diffrn_detector 'CCD plate'
_diffrn_measurement_device '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD rotation images, thick slices'
_diffrn_orient_matrix_type X=UH
_diffrn_orient_matrix_UB_11 0.01
_diffrn_orient_matrix_UB_12 0
_diffrn_orient_matrix_UB_13 0
_diffrn_orient_matrix_UB_21 0
_diffrn_orient_matrix_UB_22 0.01
_diffrn_orient_matrix_UB_23 0
_diffrn_orient_matrix_UB_31 0
_diffrn_orient_matrix_UB_32 0
_diffrn_orient_matrix_UB_33 0.01
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0799
_diffrn_reflns_av_sigmaI/netI 0.0622
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 18635
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 3.06
_diffrn_source 'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu 0.591
_exptl_absorpt_correction_T_max 1.258
_exptl_absorpt_correction_T_min 0.826
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.250
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description blocK
_exptl_crystal_F_000 904
_exptl_crystal_size_max 0.71
_exptl_crystal_size_mid 0.479
_exptl_crystal_size_min 0.433
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 208
_refine_ls_number_reflns 5211
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.065
_refine_ls_R_factor_all 0.0683
_refine_ls_R_factor_gt 0.0402
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.8463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0886
_refine_ls_wR_factor_ref 0.1001
_reflns_number_gt 3843
_reflns_number_total 5211
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100798
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.4473(4) 0.4577(3) 0.3492(3) 0.0549(10) Uani 1 1 d . . .
H9A H 0.4490 0.4426 0.4129 0.082 Uiso 1 1 calc R . .
H9B H 0.3612 0.4612 0.3089 0.082 Uiso 1 1 calc R . .
H9C H 0.4880 0.5197 0.3486 0.082 Uiso 1 1 calc R . .
Zr1 Zr 0.75090(2) 0.418728(19) 0.242124(17) 0.02164(9) Uani 1 1 d . . .
Si1 Si 0.79033(9) 0.34443(6) 0.06332(6) 0.0327(2) Uani 1 1 d . . .
Si2 Si 0.53047(8) 0.36155(7) 0.30600(6) 0.0335(2) Uani 1 1 d . . .
N1 N 0.8785(2) 0.36275(18) 0.17851(16) 0.0274(5) Uani 1 1 d . . .
N2 N 0.6906(2) 0.36530(18) 0.35132(16) 0.0269(5) Uani 1 1 d . . .
C10 C 0.8101(3) 0.5766(2) 0.28131(19) 0.0279(6) Uani 1 1 d . . .
H10A H 0.8392 0.6053 0.2328 0.042 Uiso 1 1 calc R . .
H10B H 0.8768 0.5779 0.3407 0.042 Uiso 1 1 calc R . .
H10C H 0.7391 0.6132 0.2870 0.042 Uiso 1 1 calc R . .
C1 C 0.6402(3) 0.3816(2) 0.07908(19) 0.0316(7) Uani 1 1 d . . .
C5 C 0.5855(3) 0.3281(2) 0.13688(19) 0.0291(7) Uani 1 1 d . . .
H5 H 0.5881 0.2601 0.1427 0.035 Uiso 1 1 calc R . .
C2 C 0.6116(3) 0.4795(2) 0.0906(2) 0.0344(7) Uani 1 1 d . . .
H2 H 0.6353 0.5329 0.0607 0.041 Uiso 1 1 calc R . .
C3 C 0.5431(3) 0.4848(2) 0.1531(2) 0.0343(7) Uani 1 1 d . . .
H3 H 0.5124 0.5424 0.1716 0.041 Uiso 1 1 calc R . .
C13 C 1.0736(3) 0.4178(3) 0.2901(3) 0.0508(10) Uani 1 1 d . . .
H13A H 1.0350 0.4165 0.3396 0.076 Uiso 1 1 calc R . .
H13B H 1.0623 0.4816 0.2610 0.076 Uiso 1 1 calc R . .
H13C H 1.1622 0.4041 0.3164 0.076 Uiso 1 1 calc R . .
C21 C 0.7648(3) 0.3408(2) 0.4479(2) 0.0349(7) Uani 1 1 d . . .
C7 C 0.8225(4) 0.4275(3) -0.0239(2) 0.0526(10) Uani 1 1 d . . .
H7A H 0.8259 0.4939 -0.0016 0.079 Uiso 1 1 calc R . .
H7B H 0.7565 0.4215 -0.0834 0.079 Uiso 1 1 calc R . .
H7C H 0.9020 0.4105 -0.0323 0.079 Uiso 1 1 calc R . .
C6 C 0.7842(4) 0.2175(3) 0.0211(2) 0.0498(9) Uani 1 1 d . . .
H6A H 0.8640 0.2003 0.0134 0.075 Uiso 1 1 calc R . .
H6B H 0.7187 0.2114 -0.0386 0.075 Uiso 1 1 calc R . .
H6C H 0.7666 0.1742 0.0666 0.075 Uiso 1 1 calc R . .
C11 C 1.0133(3) 0.3420(2) 0.2170(2) 0.0369(8) Uani 1 1 d . . .
C4 C 0.5263(3) 0.3909(2) 0.1847(2) 0.0320(7) Uani 1 1 d . . .
C8 C 0.4550(3) 0.2436(3) 0.3109(3) 0.0537(10) Uani 1 1 d . . .
H8A H 0.4583 0.2300 0.3752 0.081 Uiso 1 1 calc R . .
H8B H 0.4985 0.1928 0.2887 0.081 Uiso 1 1 calc R . .
H8C H 0.3685 0.2460 0.2714 0.081 Uiso 1 1 calc R . .
C14 C 1.0311(3) 0.2420(3) 0.2614(3) 0.0513(10) Uani 1 1 d . . .
H14A H 0.9914 0.2396 0.3102 0.077 Uiso 1 1 calc R . .
H14B H 1.1198 0.2288 0.2885 0.077 Uiso 1 1 calc R . .
H14C H 0.9937 0.1936 0.2139 0.077 Uiso 1 1 calc R . .
C24 C 0.8968(4) 0.3753(4) 0.4632(3) 0.0714(14) Uani 1 1 d . . .
H24A H 0.8967 0.4451 0.4537 0.107 Uiso 1 1 calc R . .
H24B H 0.9309 0.3432 0.4189 0.107 Uiso 1 1 calc R . .
H24C H 0.9478 0.3599 0.5267 0.107 Uiso 1 1 calc R . .
C12 C 1.0766(4) 0.3457(4) 0.1419(3) 0.0649(12) Uani 1 1 d . . .
H12A H 1.0397 0.2974 0.0941 0.097 Uiso 1 1 calc R . .
H12B H 1.1651 0.3323 0.1697 0.097 Uiso 1 1 calc R . .
H12C H 1.0658 0.4098 0.1135 0.097 Uiso 1 1 calc R . .
C23 C 0.7672(4) 0.2336(3) 0.4634(3) 0.0649(13) Uani 1 1 d . . .
H23A H 0.7995 0.2015 0.4181 0.097 Uiso 1 1 calc R . .
H23B H 0.6831 0.2106 0.4557 0.097 Uiso 1 1 calc R . .
H23C H 0.8206 0.2188 0.5264 0.097 Uiso 1 1 calc R . .
C22 C 0.7150(5) 0.3915(4) 0.5185(3) 0.0805(16) Uani 1 1 d . . .
H22A H 0.7134 0.4611 0.5080 0.121 Uiso 1 1 calc R . .
H22B H 0.7687 0.3772 0.5816 0.121 Uiso 1 1 calc R . .
H22C H 0.6309 0.3686 0.5113 0.121 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C9 0.045(2) 0.057(3) 0.072(3) -0.005(2) 0.032(2) 0.0099(19)
Zr1 0.01990(14) 0.02195(15) 0.01984(14) -0.00172(11) 0.00149(10) -0.00176(12)
Si1 0.0417(5) 0.0336(5) 0.0224(4) -0.0015(3) 0.0091(4) -0.0005(4)
Si2 0.0252(4) 0.0356(5) 0.0417(5) -0.0008(4) 0.0133(4) 0.0004(4)
N1 0.0230(12) 0.0325(14) 0.0265(12) 0.0002(10) 0.0075(10) 0.0000(11)
N2 0.0279(13) 0.0293(13) 0.0231(12) 0.0014(10) 0.0071(10) 0.0012(11)
C10 0.0309(16) 0.0188(15) 0.0313(14) -0.0011(12) 0.0057(12) -0.0025(12)
C1 0.0325(16) 0.0333(17) 0.0202(13) -0.0038(12) -0.0046(12) -0.0025(13)
C5 0.0217(14) 0.0296(16) 0.0276(14) -0.0043(12) -0.0044(12) -0.0075(12)
C2 0.0339(16) 0.0331(17) 0.0268(14) 0.0056(13) -0.0042(13) 0.0010(14)
C3 0.0264(15) 0.0320(17) 0.0355(16) 0.0009(13) -0.0032(13) 0.0086(13)
C13 0.0270(17) 0.055(2) 0.059(2) 0.0034(19) -0.0020(16) -0.0072(17)
C21 0.0450(19) 0.0384(19) 0.0207(14) 0.0009(12) 0.0093(13) 0.0043(15)
C7 0.068(3) 0.057(2) 0.0372(18) 0.0098(17) 0.0230(18) 0.001(2)
C6 0.071(3) 0.043(2) 0.0369(18) -0.0088(16) 0.0189(18) -0.0030(19)
C11 0.0296(16) 0.042(2) 0.0403(17) 0.0065(14) 0.0123(14) 0.0043(14)
C4 0.0179(14) 0.0360(17) 0.0346(16) -0.0030(13) -0.0027(12) 0.0009(12)
C8 0.039(2) 0.050(2) 0.074(3) -0.001(2) 0.0199(19) -0.0094(18)
C14 0.041(2) 0.040(2) 0.065(2) 0.0063(18) 0.0052(18) 0.0084(17)
C24 0.048(2) 0.101(4) 0.049(2) 0.027(2) -0.0082(19) -0.019(2)
C12 0.038(2) 0.096(4) 0.069(3) 0.015(2) 0.028(2) 0.012(2)
C23 0.081(3) 0.046(2) 0.049(2) 0.0138(18) -0.006(2) 0.003(2)
C22 0.101(4) 0.105(4) 0.034(2) -0.006(2) 0.020(2) 0.035(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100799.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100799.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100799
loop_
_publ_author_name
'Cano, Jes\'us'
'Sudupe, Mar\'ia'
'Royo, Pascual'
'Mosquera, Marta E. G.'
_publ_section_title
;
Insertion Reactions into the Metal--Alkyl and Metal--Amido Bonds of
1,3-Di(silyl-\h-amido)cyclopentadienyl Titanium and Zirconium Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2424
_journal_page_last 2432
_journal_paper_doi 10.1021/om048984e
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C33 H49 N3 Si2 Zr'
_chemical_formula_weight 635.15
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 106.355(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.119(2)
_cell_length_b 19.430(4)
_cell_length_c 15.805(2)
_cell_measurement_reflns_used 40
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 17.209
_cell_measurement_theta_min 3.96
_cell_volume 3276.4(10)
_diffrn_ambient_temperature 200(2)
_diffrn_detector 'CCD plate'
_diffrn_measurement_device '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD rotation images, thick slices'
_diffrn_orient_matrix_type X=UH
_diffrn_orient_matrix_UB_11 0.01
_diffrn_orient_matrix_UB_12 0
_diffrn_orient_matrix_UB_13 0
_diffrn_orient_matrix_UB_21 0
_diffrn_orient_matrix_UB_22 0.01
_diffrn_orient_matrix_UB_23 0
_diffrn_orient_matrix_UB_31 0
_diffrn_orient_matrix_UB_32 0
_diffrn_orient_matrix_UB_33 0.01
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1751
_diffrn_reflns_av_sigmaI/netI 0.1321
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 27467
_diffrn_reflns_theta_max 27.53
_diffrn_reflns_theta_min 3.01
_diffrn_source 'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu 0.434
_exptl_absorpt_correction_T_max 0.954
_exptl_absorpt_correction_T_min 0.794
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.288
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1344
_exptl_crystal_size_max 0.561
_exptl_crystal_size_mid 0.443
_exptl_crystal_size_min 0.108
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 350
_refine_ls_number_reflns 7529
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.1359
_refine_ls_R_factor_gt 0.0636
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+5.5411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1210
_refine_ls_wR_factor_ref 0.1446
_reflns_number_gt 4388
_reflns_number_total 7529
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1100799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.16570(4) 0.11245(2) 0.23597(3) 0.01799(12) Uani 1 1 d . . .
C1 C 0.2279(5) 0.0594(2) 0.1091(3) 0.0248(11) Uani 1 1 d . . .
C2 C 0.1012(5) 0.0810(3) 0.0764(3) 0.0279(11) Uani 1 1 d . . .
H2 H 0.0328 0.0519 0.0556 0.034 Uiso 1 1 calc R . .
C3 C 0.0951(5) 0.1535(3) 0.0803(3) 0.0240(10) Uani 1 1 d . . .
H3 H 0.0223 0.1797 0.0622 0.029 Uiso 1 1 calc R . .
C4 C 0.2186(5) 0.1803(2) 0.1164(3) 0.0230(10) Uani 1 1 d . . .
C5 C 0.2979(5) 0.1214(3) 0.1314(3) 0.0253(11) Uani 1 1 d . . .
H5 H 0.3847 0.1232 0.1532 0.030 Uiso 1 1 calc R . .
Si1 Si 0.28551(13) -0.01848(7) 0.17817(9) 0.0267(3) Uani 1 1 d . . .
N1 N 0.2559(4) 0.0136(2) 0.2723(2) 0.0240(9) Uani 1 1 d . . .
C11 C 0.1969(6) -0.0980(3) 0.1282(4) 0.0401(14) Uani 1 1 d . . .
H11A H 0.2289 -0.1370 0.1649 0.060 Uiso 1 1 calc R . .
H11B H 0.2070 -0.1054 0.0705 0.060 Uiso 1 1 calc R . .
H11C H 0.1096 -0.0922 0.1237 0.060 Uiso 1 1 calc R . .
C12 C 0.4537(5) -0.0323(3) 0.1829(4) 0.0422(15) Uani 1 1 d . . .
H12A H 0.4848 -0.0723 0.2180 0.063 Uiso 1 1 calc R . .
H12B H 0.5019 0.0072 0.2088 0.063 Uiso 1 1 calc R . .
H12C H 0.4607 -0.0391 0.1243 0.063 Uiso 1 1 calc R . .
C13 C 0.2745(5) -0.0289(3) 0.3543(3) 0.0296(12) Uani 1 1 d . . .
C14 C 0.1581(5) -0.0720(3) 0.3497(4) 0.0383(13) Uani 1 1 d . . .
H14A H 0.1409 -0.1014 0.2989 0.057 Uiso 1 1 calc R . .
H14B H 0.0879 -0.0421 0.3453 0.057 Uiso 1 1 calc R . .
H14C H 0.1723 -0.0995 0.4020 0.057 Uiso 1 1 calc R . .
C15 C 0.3029(6) 0.0182(3) 0.4354(3) 0.0407(14) Uani 1 1 d . . .
H15A H 0.3761 0.0452 0.4379 0.061 Uiso 1 1 calc R . .
H15B H 0.3176 -0.0093 0.4878 0.061 Uiso 1 1 calc R . .
H15C H 0.2329 0.0482 0.4314 0.061 Uiso 1 1 calc R . .
C16 C 0.3861(5) -0.0785(3) 0.3674(4) 0.0422(14) Uani 1 1 d . . .
H16A H 0.4609 -0.0527 0.3706 0.063 Uiso 1 1 calc R . .
H16B H 0.3704 -0.1099 0.3186 0.063 Uiso 1 1 calc R . .
H16C H 0.3966 -0.1039 0.4211 0.063 Uiso 1 1 calc R . .
Si2 Si 0.26229(13) 0.25520(7) 0.19222(9) 0.0240(3) Uani 1 1 d . . .
N2 N 0.2358(4) 0.2134(2) 0.2827(2) 0.0224(9) Uani 1 1 d . . .
C21 C 0.1616(5) 0.3317(3) 0.1502(3) 0.0369(13) Uani 1 1 d . . .
H21A H 0.1868 0.3692 0.1909 0.055 Uiso 1 1 calc R . .
H21B H 0.0756 0.3203 0.1443 0.055 Uiso 1 1 calc R . .
H21C H 0.1707 0.3448 0.0937 0.055 Uiso 1 1 calc R . .
C22 C 0.4266(5) 0.2800(3) 0.2007(4) 0.0393(14) Uani 1 1 d . . .
H22A H 0.4502 0.3186 0.2397 0.059 Uiso 1 1 calc R . .
H22B H 0.4334 0.2922 0.1433 0.059 Uiso 1 1 calc R . .
H22C H 0.4813 0.2419 0.2233 0.059 Uiso 1 1 calc R . .
C23 C 0.2395(5) 0.2498(2) 0.3666(3) 0.0250(11) Uani 1 1 d . . .
C24 C 0.1099(5) 0.2803(3) 0.3601(4) 0.0348(13) Uani 1 1 d . . .
H24A H 0.0869 0.3118 0.3114 0.052 Uiso 1 1 calc R . .
H24B H 0.1126 0.3043 0.4137 0.052 Uiso 1 1 calc R . .
H24C H 0.0492 0.2439 0.3511 0.052 Uiso 1 1 calc R . .
C25 C 0.3357(5) 0.3094(3) 0.3856(4) 0.0371(13) Uani 1 1 d . . .
H25A H 0.3147 0.3416 0.3376 0.056 Uiso 1 1 calc R . .
H25B H 0.4181 0.2914 0.3919 0.056 Uiso 1 1 calc R . .
H25C H 0.3339 0.3323 0.4391 0.056 Uiso 1 1 calc R . .
C26 C 0.2767(6) 0.2002(3) 0.4437(3) 0.0422(15) Uani 1 1 d . . .
H26A H 0.3579 0.1814 0.4477 0.063 Uiso 1 1 calc R . .
H26B H 0.2164 0.1636 0.4349 0.063 Uiso 1 1 calc R . .
H26C H 0.2792 0.2242 0.4972 0.063 Uiso 1 1 calc R . .
N3 N -0.0325(3) 0.1080(2) 0.2283(2) 0.0220(8) Uani 1 1 d . . .
C30 C 0.0205(5) 0.0982(2) 0.3108(3) 0.0268(11) Uani 1 1 d . . .
C31 C -0.0474(6) 0.0769(4) 0.3775(4) 0.061(2) Uani 1 1 d . . .
H31A H -0.0707 0.0289 0.3665 0.073 Uiso 1 1 calc R . .
H31B H 0.0125 0.0792 0.4354 0.073 Uiso 1 1 calc R . .
C32 C -0.1616(4) 0.1151(3) 0.3818(3) 0.0284(11) Uani 1 1 d D B .
C33 C -0.1512(9) 0.1766(4) 0.4271(5) 0.073(3) Uani 1 1 d D . .
H33 H -0.0689 0.1923 0.4459 0.088 Uiso 1 1 calc R A 1
C34 C -0.2224(15) 0.2144(7) 0.4479(9) 0.047(4) Uiso 0.511(18) 1 d PD B 1
H34 H -0.1978 0.2521 0.4850 0.057 Uiso 0.511(18) 1 calc PR B 1
C35 C -0.3460(19) 0.1957(10) 0.4106(11) 0.056(5) Uiso 0.511(18) 1 d PD B 1
H35 H -0.4083 0.2242 0.4196 0.068 Uiso 0.511(18) 1 calc PR B 1
C36 C -0.3816(15) 0.1376(11) 0.3613(10) 0.052(4) Uiso 0.511(18) 1 d PD B 1
H36 H -0.4660 0.1276 0.3367 0.063 Uiso 0.511(18) 1 calc PR B 1
C34' C -0.2932(19) 0.2087(8) 0.4202(10) 0.047(4) Uiso 0.489(18) 1 d P B 2
H34' H -0.3044 0.2520 0.4419 0.056 Uiso 0.489(18) 1 calc PR B 2
C35' C -0.3911(14) 0.1671(9) 0.3806(10) 0.043(4) Uiso 0.489(18) 1 d P B 2
H35' H -0.4701 0.1857 0.3746 0.052 Uiso 0.489(18) 1 calc PR B 2
C36' C -0.3905(11) 0.1003(8) 0.3475(8) 0.036(4) Uiso 0.489(18) 1 d P B 2
H36' H -0.4587 0.0708 0.3296 0.044 Uiso 0.489(18) 1 calc PR B 2
C37 C -0.2772(6) 0.0877(4) 0.3466(4) 0.060(2) Uani 1 1 d D . .
H37 H -0.2928 0.0454 0.3180 0.072 Uiso 1 1 calc R B 1
C38 C -0.1591(4) 0.1046(3) 0.1727(3) 0.0255(11) Uani 1 1 d . . .
C39 C -0.2299(5) 0.1651(3) 0.1521(3) 0.0267(11) Uani 1 1 d . . .
C40 C -0.3494(5) 0.1600(3) 0.0939(3) 0.0330(12) Uani 1 1 d . . .
H40 H -0.3982 0.1994 0.0796 0.040 Uiso 1 1 calc R . .
C41 C -0.3970(5) 0.0986(3) 0.0572(4) 0.0395(14) Uani 1 1 d . . .
H41 H -0.4777 0.0963 0.0191 0.047 Uiso 1 1 calc R . .
C42 C -0.3240(5) 0.0398(3) 0.0772(4) 0.0375(13) Uani 1 1 d . . .
H42 H -0.3555 -0.0016 0.0506 0.045 Uiso 1 1 calc R . .
C43 C -0.2057(5) 0.0414(3) 0.1357(4) 0.0291(12) Uani 1 1 d . . .
C44 C -0.1299(5) -0.0242(3) 0.1565(4) 0.0394(13) Uani 1 1 d . . .
H44A H -0.0504 -0.0146 0.1981 0.059 Uiso 1 1 calc R . .
H44B H -0.1168 -0.0424 0.1033 0.059 Uiso 1 1 calc R . .
H44C H -0.1745 -0.0573 0.1813 0.059 Uiso 1 1 calc R . .
C45 C -0.1787(5) 0.2334(3) 0.1903(4) 0.0386(13) Uani 1 1 d . . .
H45A H -0.0956 0.2273 0.2289 0.058 Uiso 1 1 calc R . .
H45B H -0.2317 0.2524 0.2230 0.058 Uiso 1 1 calc R . .
H45C H -0.1758 0.2643 0.1435 0.058 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.0230(2) 0.0147(2) 0.0170(2) -0.0002(2) 0.00688(15) -0.0007(2)
C1 0.037(3) 0.017(2) 0.024(3) -0.003(2) 0.014(2) 0.001(2)
C2 0.037(3) 0.029(3) 0.017(2) -0.004(2) 0.006(2) -0.005(2)
C3 0.033(3) 0.022(3) 0.016(2) -0.003(2) 0.006(2) 0.002(2)
C4 0.036(3) 0.021(3) 0.015(2) -0.0004(19) 0.011(2) 0.001(2)
C5 0.031(3) 0.029(3) 0.019(2) -0.005(2) 0.0122(19) -0.005(2)
Si1 0.0339(8) 0.0172(7) 0.0321(8) -0.0007(6) 0.0144(6) 0.0027(6)
N1 0.032(2) 0.019(2) 0.022(2) 0.0010(17) 0.0084(17) 0.0031(17)
C11 0.059(4) 0.022(3) 0.045(3) -0.005(2) 0.023(3) -0.004(3)
C12 0.047(4) 0.040(4) 0.049(4) 0.005(3) 0.027(3) 0.009(3)
C13 0.039(3) 0.026(3) 0.025(3) 0.009(2) 0.013(2) 0.008(2)
C14 0.045(3) 0.035(3) 0.038(3) 0.008(3) 0.017(3) 0.002(3)
C15 0.053(4) 0.037(3) 0.030(3) 0.009(3) 0.008(3) 0.007(3)
C16 0.053(4) 0.027(3) 0.046(3) 0.009(3) 0.013(3) 0.014(3)
Si2 0.0358(8) 0.0152(7) 0.0237(7) -0.0005(5) 0.0127(6) -0.0026(6)
N2 0.028(2) 0.022(2) 0.0194(19) -0.0049(17) 0.0111(17) -0.0034(17)
C21 0.057(4) 0.023(3) 0.034(3) 0.004(2) 0.018(3) 0.005(3)
C22 0.044(3) 0.036(3) 0.043(3) -0.005(3) 0.020(3) -0.016(3)
C23 0.036(3) 0.022(3) 0.017(2) -0.009(2) 0.009(2) -0.004(2)
C24 0.041(3) 0.033(3) 0.036(3) -0.016(3) 0.020(2) -0.004(2)
C25 0.043(3) 0.031(3) 0.036(3) -0.016(3) 0.009(3) -0.005(2)
C26 0.070(4) 0.036(3) 0.021(3) -0.001(2) 0.013(3) 0.004(3)
N3 0.028(2) 0.017(2) 0.0227(19) 0.0012(18) 0.0103(16) -0.0007(17)
C30 0.031(3) 0.022(3) 0.029(3) 0.006(2) 0.011(2) 0.004(2)
C31 0.051(4) 0.095(6) 0.050(4) 0.039(4) 0.034(3) 0.028(4)
C32 0.028(3) 0.037(3) 0.023(2) 0.008(3) 0.0119(19) 0.004(2)
C33 0.138(7) 0.043(4) 0.069(5) -0.009(4) 0.078(5) -0.024(5)
C37 0.057(4) 0.095(6) 0.034(3) -0.004(4) 0.021(3) -0.023(4)
C38 0.026(2) 0.027(3) 0.026(2) 0.008(2) 0.0109(19) 0.000(2)
C39 0.031(3) 0.026(3) 0.025(3) 0.001(2) 0.012(2) 0.002(2)
C40 0.030(3) 0.037(3) 0.034(3) 0.003(3) 0.012(2) 0.010(2)
C41 0.024(3) 0.048(4) 0.042(3) 0.002(3) 0.001(2) -0.007(2)
C42 0.033(3) 0.037(3) 0.038(3) -0.003(3) 0.004(2) -0.011(2)
C43 0.027(3) 0.022(3) 0.041(3) 0.005(2) 0.013(2) -0.006(2)
C44 0.040(3) 0.026(3) 0.053(4) 0.002(3) 0.012(3) -0.002(2)
C45 0.048(3) 0.027(3) 0.038(3) 0.000(2) 0.007(3) 0.012(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100800.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100800.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100800
loop_
_publ_author_name
'Cano, Jes\'us'
'Sudupe, Mar\'ia'
'Royo, Pascual'
'Mosquera, Marta E. G.'
_publ_section_title
;
Insertion Reactions into the Metal--Alkyl and Metal--Amido Bonds of
1,3-Di(silyl-\h-amido)cyclopentadienyl Titanium and Zirconium Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2424
_journal_page_last 2432
_journal_paper_doi 10.1021/om048984e
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C36 H54 N4 Si2 Ti1'
_chemical_formula_sum 'C36 H54 N4 Si2 Ti'
_chemical_formula_weight 646.91
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 98.372(6)
_cell_angle_beta 102.866(10)
_cell_angle_gamma 99.863(7)
_cell_formula_units_Z 2
_cell_length_a 9.7722(10)
_cell_length_b 11.3369(4)
_cell_length_c 17.0066(16)
_cell_measurement_reflns_used 120
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 21.149
_cell_measurement_theta_min 5.123
_cell_volume 1776.2(3)
_diffrn_ambient_temperature 200(2)
_diffrn_detector 'CCD plate'
_diffrn_measurement_device '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD rotation images, thick slices'
_diffrn_orient_matrix_type X=UH
_diffrn_orient_matrix_UB_11 0.01
_diffrn_orient_matrix_UB_12 0
_diffrn_orient_matrix_UB_13 0
_diffrn_orient_matrix_UB_21 0
_diffrn_orient_matrix_UB_22 0.01
_diffrn_orient_matrix_UB_23 0
_diffrn_orient_matrix_UB_31 0
_diffrn_orient_matrix_UB_32 0
_diffrn_orient_matrix_UB_33 0.01
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0663
_diffrn_reflns_av_sigmaI/netI 0.0986
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 15135
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 3.04
_diffrn_source 'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu 0.338
_exptl_absorpt_correction_T_max 1.242
_exptl_absorpt_correction_T_min 0.825
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.210
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 696
_exptl_crystal_size_max 0.412
_exptl_crystal_size_mid 0.396
_exptl_crystal_size_min 0.194
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 388
_refine_ls_number_reflns 8058
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.1097
_refine_ls_R_factor_gt 0.0614
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+1.4230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1466
_refine_ls_wR_factor_ref 0.1654
_reflns_number_gt 5192
_reflns_number_total 8058
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100800
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.2452(3) 0.2792(3) 0.1986(2) 0.0265(7) Uani 1 1 d . . .
H10A H 0.1793 0.2011 0.1928 0.040 Uiso 1 1 calc R . .
H10B H 0.2140 0.3167 0.1511 0.040 Uiso 1 1 calc R . .
H10C H 0.2452 0.3336 0.2490 0.040 Uiso 1 1 calc R . .
C6 C 0.6224(4) 0.6787(3) 0.3835(2) 0.0356(8) Uani 1 1 d . . .
H6A H 0.5913 0.7424 0.3550 0.053 Uiso 1 1 calc R . .
H6B H 0.7201 0.6739 0.3799 0.053 Uiso 1 1 calc R . .
H6C H 0.6211 0.6985 0.4413 0.053 Uiso 1 1 calc R . .
Ti1 Ti 0.59675(6) 0.23075(5) 0.30176(3) 0.01901(15) Uani 1 1 d . . .
Si1 Si 0.49779(10) 0.52856(8) 0.33424(6) 0.0236(2) Uani 1 1 d . . .
Si2 Si 0.81571(12) 0.16891(9) 0.42846(6) 0.0337(2) Uani 1 1 d . . .
N3 N 0.6500(3) 0.3256(2) 0.22320(15) 0.0171(5) Uani 1 1 d . . .
N1 N 0.4972(3) 0.4790(2) 0.23103(16) 0.0200(5) Uani 1 1 d . . .
N4 N 0.4210(3) 0.1426(2) 0.21100(16) 0.0222(6) Uani 1 1 d . . .
N2 N 0.7401(3) 0.1270(2) 0.32307(16) 0.0233(6) Uani 1 1 d . . .
C31 C 0.7562(3) 0.3754(3) 0.18271(19) 0.0185(6) Uani 1 1 d . . .
C36 C 0.7407(3) 0.3244(3) 0.0997(2) 0.0224(7) Uani 1 1 d . . .
C37 C 0.6184(4) 0.2214(3) 0.0530(2) 0.0273(7) Uani 1 1 d . . .
H37A H 0.6269 0.1990 -0.0034 0.041 Uiso 1 1 calc R . .
H37B H 0.5272 0.2470 0.0517 0.041 Uiso 1 1 calc R . .
H37C H 0.6212 0.1509 0.0800 0.041 Uiso 1 1 calc R . .
C11 C 0.4762(3) 0.5526(3) 0.1639(2) 0.0229(7) Uani 1 1 d . . .
C30 C 0.5130(3) 0.3544(3) 0.21154(18) 0.0184(6) Uani 1 1 d . . .
C32 C 0.8778(3) 0.4677(3) 0.2246(2) 0.0234(7) Uani 1 1 d . . .
C41 C 0.3067(3) 0.0371(3) 0.1773(2) 0.0249(7) Uani 1 1 d . . .
C22 C 0.7935(4) 0.0448(3) 0.2651(2) 0.0260(7) Uani 1 1 d . . .
C5 C 0.6969(4) 0.3870(3) 0.41899(19) 0.0279(7) Uani 1 1 d . . .
H5 H 0.7825 0.4433 0.4215 0.034 Uiso 1 1 calc R . .
C13 C 0.3992(4) 0.4693(3) 0.0806(2) 0.0336(8) Uani 1 1 d . . .
H13A H 0.3080 0.4218 0.0845 0.050 Uiso 1 1 calc R . .
H13B H 0.4599 0.4137 0.0658 0.050 Uiso 1 1 calc R . .
H13C H 0.3806 0.5191 0.0385 0.050 Uiso 1 1 calc R . .
C2 C 0.4616(4) 0.3005(3) 0.3997(2) 0.0309(8) Uani 1 1 d . . .
H2 H 0.3597 0.2864 0.3856 0.037 Uiso 1 1 calc R . .
C33 C 0.9768(3) 0.5090(3) 0.1818(2) 0.0299(8) Uani 1 1 d . . .
H33 H 1.0574 0.5723 0.2097 0.036 Uiso 1 1 calc R . .
C25 C 0.6681(4) -0.0236(3) 0.1928(2) 0.0391(9) Uani 1 1 d . . .
H25A H 0.5950 -0.0714 0.2134 0.059 Uiso 1 1 calc R . .
H25B H 0.7028 -0.0783 0.1553 0.059 Uiso 1 1 calc R . .
H25C H 0.6260 0.0352 0.1635 0.059 Uiso 1 1 calc R . .
C35 C 0.8438(4) 0.3693(3) 0.0596(2) 0.0289(7) Uani 1 1 d . . .
H35 H 0.8324 0.3360 0.0034 0.035 Uiso 1 1 calc R . .
C43 C 0.1562(4) -0.1463(3) 0.1933(3) 0.0400(10) Uani 1 1 d . . .
H43 H 0.1316 -0.2020 0.2271 0.048 Uiso 1 1 calc R . .
C7 C 0.3205(4) 0.5450(3) 0.3556(2) 0.0350(8) Uani 1 1 d . . .
H7A H 0.2492 0.4691 0.3311 0.053 Uiso 1 1 calc R . .
H7B H 0.2883 0.6123 0.3318 0.053 Uiso 1 1 calc R . .
H7C H 0.3316 0.5621 0.4151 0.053 Uiso 1 1 calc R . .
C1 C 0.5555(4) 0.4047(3) 0.3880(2) 0.0261(7) Uani 1 1 d . . .
C4 C 0.6922(4) 0.2726(3) 0.4459(2) 0.0309(8) Uani 1 1 d . . .
C34 C 0.9612(4) 0.4607(3) 0.1003(2) 0.0332(8) Uani 1 1 d . . .
H34 H 1.0305 0.4901 0.0725 0.040 Uiso 1 1 calc R . .
C46 C 0.2307(4) 0.0150(3) 0.0938(2) 0.0303(8) Uani 1 1 d . . .
C3 C 0.5436(4) 0.2232(3) 0.4349(2) 0.0316(8) Uani 1 1 d . . .
H3 H 0.5059 0.1488 0.4494 0.038 Uiso 1 1 calc R . .
C42 C 0.2716(4) -0.0475(3) 0.2267(2) 0.0336(8) Uani 1 1 d . . .
C14 C 0.3807(4) 0.6419(3) 0.1829(2) 0.0336(8) Uani 1 1 d . . .
H14A H 0.2889 0.5961 0.1871 0.050 Uiso 1 1 calc R . .
H14B H 0.3635 0.6882 0.1386 0.050 Uiso 1 1 calc R . .
H14C H 0.4289 0.6982 0.2349 0.050 Uiso 1 1 calc R . .
C12 C 0.6189(4) 0.6260(3) 0.1577(2) 0.0327(8) Uani 1 1 d . . .
H12A H 0.6685 0.6792 0.2108 0.049 Uiso 1 1 calc R . .
H12B H 0.6005 0.6758 0.1155 0.049 Uiso 1 1 calc R . .
H12C H 0.6790 0.5700 0.1428 0.049 Uiso 1 1 calc R . .
C47 C 0.2707(4) 0.0898(3) 0.0320(2) 0.0383(9) Uani 1 1 d . . .
H47A H 0.3510 0.1580 0.0601 0.057 Uiso 1 1 calc R . .
H47B H 0.1879 0.1213 0.0064 0.057 Uiso 1 1 calc R . .
H47C H 0.2990 0.0381 -0.0104 0.057 Uiso 1 1 calc R . .
C48 C 0.3511(5) -0.0343(4) 0.3149(3) 0.0460(10) Uani 1 1 d . . .
H48A H 0.4287 0.0385 0.3303 0.069 Uiso 1 1 calc R . .
H48B H 0.3917 -0.1065 0.3221 0.069 Uiso 1 1 calc R . .
H48C H 0.2848 -0.0265 0.3500 0.069 Uiso 1 1 calc R . .
C9 C 0.7926(6) 0.0453(4) 0.4897(3) 0.0568(12) Uani 1 1 d . . .
H9A H 0.8572 -0.0097 0.4810 0.085 Uiso 1 1 calc R . .
H9B H 0.6930 -0.0008 0.4720 0.085 Uiso 1 1 calc R . .
H9C H 0.8154 0.0819 0.5482 0.085 Uiso 1 1 calc R . .
C45 C 0.1167(4) -0.0866(3) 0.0634(3) 0.0417(10) Uani 1 1 d . . .
H45 H 0.0652 -0.1018 0.0073 0.050 Uiso 1 1 calc R . .
C23 C 0.8607(4) -0.0493(3) 0.3078(3) 0.0392(9) Uani 1 1 d . . .
H23A H 0.7889 -0.0986 0.3284 0.059 Uiso 1 1 calc R . .
H23B H 0.9423 -0.0070 0.3538 0.059 Uiso 1 1 calc R . .
H23C H 0.8939 -0.1024 0.2685 0.059 Uiso 1 1 calc R . .
C38 C 0.9023(4) 0.5273(4) 0.3128(2) 0.0439(10) Uani 1 1 d . . .
H38A H 0.8250 0.4895 0.3350 0.066 Uiso 1 1 calc R . .
H38B H 0.9032 0.6145 0.3163 0.066 Uiso 1 1 calc R . .
H38C H 0.9947 0.5168 0.3446 0.066 Uiso 1 1 calc R . .
C44 C 0.0775(4) -0.1656(3) 0.1138(3) 0.0471(11) Uani 1 1 d . . .
H44 H -0.0029 -0.2318 0.0931 0.057 Uiso 1 1 calc R . .
C8 C 1.0076(5) 0.2521(4) 0.4596(3) 0.0576(12) Uani 1 1 d . . .
H8A H 1.0692 0.1948 0.4497 0.086 Uiso 1 1 calc R . .
H8B H 1.0338 0.2891 0.5181 0.086 Uiso 1 1 calc R . .
H8C H 1.0205 0.3161 0.4273 0.086 Uiso 1 1 calc R . .
C24 C 0.9079(4) 0.1204(3) 0.2331(3) 0.0427(10) Uani 1 1 d . . .
H24A H 0.8667 0.1812 0.2057 0.064 Uiso 1 1 calc R . .
H24B H 0.9404 0.0664 0.1940 0.064 Uiso 1 1 calc R . .
H24C H 0.9896 0.1618 0.2793 0.064 Uiso 1 1 calc R . .
C40 C 0.3949(3) 0.2582(3) 0.20313(19) 0.0213(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C10 0.0189(16) 0.0292(17) 0.0325(19) 0.0034(14) 0.0097(14) 0.0064(13)
C6 0.038(2) 0.0329(18) 0.033(2) -0.0022(15) 0.0080(17) 0.0081(15)
Ti1 0.0198(3) 0.0217(3) 0.0173(3) 0.0044(2) 0.0074(2) 0.0051(2)
Si1 0.0254(5) 0.0251(4) 0.0207(5) 0.0000(3) 0.0076(4) 0.0075(4)
Si2 0.0388(6) 0.0399(6) 0.0244(5) 0.0097(4) 0.0032(4) 0.0166(4)
N3 0.0165(12) 0.0192(12) 0.0164(13) 0.0034(10) 0.0061(10) 0.0040(9)
N1 0.0231(14) 0.0182(12) 0.0192(13) 0.0020(10) 0.0061(11) 0.0058(10)
N4 0.0192(14) 0.0230(13) 0.0256(15) 0.0032(11) 0.0094(11) 0.0041(10)
N2 0.0244(14) 0.0259(13) 0.0248(15) 0.0103(11) 0.0106(12) 0.0090(11)
C31 0.0168(15) 0.0220(15) 0.0219(16) 0.0096(12) 0.0087(12) 0.0083(12)
C36 0.0232(16) 0.0254(16) 0.0235(17) 0.0091(13) 0.0098(13) 0.0097(13)
C37 0.0286(18) 0.0293(17) 0.0235(17) 0.0005(13) 0.0091(14) 0.0053(14)
C11 0.0248(17) 0.0223(15) 0.0258(17) 0.0088(13) 0.0092(14) 0.0089(12)
C30 0.0193(15) 0.0212(14) 0.0158(15) 0.0032(11) 0.0062(12) 0.0056(12)
C32 0.0175(16) 0.0273(16) 0.0265(17) 0.0077(13) 0.0061(13) 0.0046(12)
C41 0.0185(16) 0.0207(15) 0.0365(19) 0.0000(13) 0.0129(14) 0.0037(12)
C22 0.0295(18) 0.0250(16) 0.0308(18) 0.0112(13) 0.0134(15) 0.0131(13)
C5 0.0344(19) 0.0322(18) 0.0155(16) -0.0012(13) 0.0057(14) 0.0079(14)
C13 0.043(2) 0.0340(19) 0.0251(18) 0.0085(15) 0.0067(16) 0.0128(16)
C2 0.036(2) 0.0371(19) 0.0243(18) 0.0049(14) 0.0172(15) 0.0090(15)
C33 0.0167(16) 0.0348(18) 0.038(2) 0.0123(15) 0.0074(15) 0.0004(13)
C25 0.043(2) 0.040(2) 0.035(2) 0.0016(16) 0.0104(18) 0.0179(17)
C35 0.0305(19) 0.0391(19) 0.0238(18) 0.0107(14) 0.0140(15) 0.0126(15)
C43 0.034(2) 0.0218(17) 0.070(3) 0.0076(17) 0.026(2) 0.0053(15)
C7 0.037(2) 0.040(2) 0.032(2) 0.0013(16) 0.0163(17) 0.0153(16)
C1 0.0319(19) 0.0307(17) 0.0173(16) 0.0008(13) 0.0096(14) 0.0095(14)
C4 0.041(2) 0.0374(19) 0.0156(16) 0.0039(14) 0.0072(15) 0.0136(16)
C34 0.0239(18) 0.045(2) 0.036(2) 0.0159(16) 0.0161(16) 0.0040(15)
C46 0.0216(17) 0.0263(17) 0.039(2) -0.0036(14) 0.0073(15) 0.0028(13)
C3 0.048(2) 0.0323(18) 0.0215(18) 0.0087(14) 0.0181(16) 0.0118(16)
C42 0.0301(19) 0.0248(17) 0.049(2) 0.0028(15) 0.0203(17) 0.0049(14)
C14 0.038(2) 0.0351(19) 0.035(2) 0.0114(15) 0.0139(17) 0.0199(16)
C12 0.0319(19) 0.0326(18) 0.041(2) 0.0168(16) 0.0150(17) 0.0105(15)
C47 0.029(2) 0.043(2) 0.035(2) 0.0009(17) 0.0030(16) -0.0021(16)
C48 0.059(3) 0.033(2) 0.053(3) 0.0209(18) 0.026(2) 0.0023(18)
C9 0.085(4) 0.065(3) 0.038(2) 0.028(2) 0.020(2) 0.041(3)
C45 0.028(2) 0.034(2) 0.053(3) -0.0088(17) 0.0059(18) 0.0010(15)
C23 0.043(2) 0.034(2) 0.050(2) 0.0175(17) 0.0177(19) 0.0204(17)
C38 0.031(2) 0.054(2) 0.034(2) -0.0088(18) 0.0109(17) -0.0122(17)
C44 0.028(2) 0.0246(19) 0.082(3) -0.0041(19) 0.015(2) -0.0027(15)
C8 0.042(3) 0.062(3) 0.055(3) -0.004(2) -0.011(2) 0.018(2)
C24 0.045(2) 0.039(2) 0.060(3) 0.0208(19) 0.033(2) 0.0168(18)
C40 0.0224(16) 0.0227(15) 0.0205(16) 0.0020(12) 0.0095(13) 0.0061(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100801.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 07:52:51 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180561 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100801.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100801
loop_
_publ_author_name
'Mebi, Charles A.'
'Frost, Brian J.'
_publ_section_title
;
Effect of pH on the Biphasic Catalytic Hydrogenation of Benzylidene
Acetone Using CpRu(PTA)~2~H
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2339
_journal_page_last 2346
_journal_paper_doi 10.1021/om048987r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C34 H62 Cl2 F24 N12 O4 P8 Ru2'
_chemical_formula_weight 1679.76
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 75.545(2)
_cell_angle_beta 81.394(2)
_cell_angle_gamma 82.551(2)
_cell_formula_units_Z 1
_cell_length_a 6.5764(9)
_cell_length_b 13.4764(19)
_cell_length_c 17.321(2)
_cell_measurement_reflns_used 1904
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.17
_cell_measurement_theta_min 2.20
_cell_volume 1462.9(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1425
_diffrn_reflns_av_sigmaI/netI 0.1788
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 14049
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.75
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.953
_exptl_absorpt_correction_T_max 0.9858
_exptl_absorpt_correction_T_min 0.9183
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.907
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 840
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.02
_refine_diff_density_max 1.049
_refine_diff_density_min -1.039
_refine_diff_density_rms 0.180
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.929
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 388
_refine_ls_number_reflns 5149
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.929
_refine_ls_R_factor_all 0.1534
_refine_ls_R_factor_gt 0.0669
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1353
_refine_ls_wR_factor_ref 0.1524
_reflns_number_gt 2715
_reflns_number_total 5149
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om048987rsi20041221_041543.cif
_cod_data_source_block bjf070abs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P1
_cod_database_code 1100801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.55007(13) 0.39688(6) 0.32923(5) 0.0142(2) Uani 1 1 d . . .
Cl1 Cl 0.8200(4) 0.33779(17) 0.23208(13) 0.0199(6) Uani 1 1 d . . .
P1 P 0.4166(4) 0.24704(19) 0.34157(14) 0.0164(6) Uani 1 1 d . . .
P2 P 0.3992(4) 0.49249(19) 0.22243(14) 0.0164(6) Uani 1 1 d . . .
P3 P 0.0283(4) 0.2184(2) 0.64208(16) 0.0219(6) Uani 1 1 d . . .
P4 P 0.1778(5) 0.1593(2) 0.05518(16) 0.0260(7) Uani 1 1 d . . .
F1 F 0.2497(9) 0.1874(5) 0.5981(3) 0.0365(16) Uani 1 1 d . . .
F2 F 0.0148(8) 0.3263(4) 0.5787(3) 0.0279(14) Uani 1 1 d . . .
F3 F -0.1935(9) 0.2492(4) 0.6842(3) 0.0325(15) Uani 1 1 d . . .
F4 F 0.0404(10) 0.1090(4) 0.7070(3) 0.0391(17) Uani 1 1 d . . .
F5 F -0.0793(10) 0.1693(4) 0.5853(3) 0.0346(16) Uani 1 1 d . . .
F6 F 0.1371(9) 0.2646(4) 0.6996(3) 0.0298(14) Uani 1 1 d . . .
F7 F 0.4195(9) 0.1474(5) 0.0633(4) 0.0376(16) Uani 1 1 d . . .
F8 F 0.2186(9) 0.2300(4) -0.0344(3) 0.0306(15) Uani 1 1 d . . .
F9 F -0.0641(9) 0.1710(5) 0.0485(3) 0.0365(16) Uani 1 1 d . . .
F10 F 0.1368(10) 0.0892(5) 0.1449(3) 0.0430(18) Uani 1 1 d . . .
F11 F 0.2035(10) 0.0601(4) 0.0206(3) 0.0382(17) Uani 1 1 d . . .
F12 F 0.1520(10) 0.2599(5) 0.0901(3) 0.0393(17) Uani 1 1 d . . .
N1 N 0.4539(12) 0.0370(6) 0.4116(4) 0.0165(18) Uani 1 1 d . . .
N2 N 0.1042(12) 0.1179(6) 0.3916(5) 0.021(2) Uani 1 1 d . . .
N3 N 0.3478(12) 0.0866(6) 0.2761(5) 0.0184(19) Uani 1 1 d . . .
H3C H 0.3565 0.0616 0.2302 0.022 Uiso 1 1 calc R . .
N4 N 0.0577(12) 0.6082(6) 0.1559(4) 0.0184(19) Uani 1 1 d . . .
N5 N 0.3869(11) 0.6823(6) 0.1126(4) 0.0171(18) Uani 1 1 d . . .
H5C H 0.4405 0.7458 0.0946 0.020 Uiso 1 1 calc R . .
N6 N 0.3214(13) 0.5367(6) 0.0638(4) 0.023(2) Uani 1 1 d . . .
C1 C 0.5436(14) 0.1344(7) 0.4076(5) 0.016(2) Uani 1 1 d . . .
H1A H 0.6926 0.1271 0.3876 0.019 Uiso 1 1 calc R . .
H1B H 0.5304 0.1461 0.4624 0.019 Uiso 1 1 calc R . .
C2 C 0.1469(14) 0.2255(7) 0.3838(6) 0.020(2) Uani 1 1 d . . .
H2A H 0.1191 0.2417 0.4373 0.024 Uiso 1 1 calc R . .
H2B H 0.0525 0.2728 0.3485 0.024 Uiso 1 1 calc R . .
C3 C 0.4263(15) 0.1932(7) 0.2534(5) 0.019(2) Uani 1 1 d . . .
H3A H 0.3409 0.2401 0.2143 0.023 Uiso 1 1 calc R . .
H3B H 0.5704 0.1883 0.2271 0.023 Uiso 1 1 calc R . .
C4 C 0.2351(14) 0.0438(7) 0.4455(5) 0.016(2) Uani 1 1 d . . .
H4A H 0.2229 0.0643 0.4971 0.019 Uiso 1 1 calc R . .
H4B H 0.1845 -0.0251 0.4567 0.019 Uiso 1 1 calc R . .
C5 C 0.1252(14) 0.0917(7) 0.3149(6) 0.021(2) Uani 1 1 d . . .
H5A H 0.0405 0.1438 0.2787 0.026 Uiso 1 1 calc R . .
H5B H 0.0718 0.0242 0.3222 0.026 Uiso 1 1 calc R . .
C6 C 0.4767(16) 0.0138(8) 0.3353(5) 0.023(2) Uani 1 1 d . . .
H6A H 0.4390 -0.0569 0.3423 0.028 Uiso 1 1 calc R . .
H6B H 0.6240 0.0150 0.3125 0.028 Uiso 1 1 calc R . .
C7 C 0.1206(14) 0.5361(8) 0.2316(5) 0.021(2) Uani 1 1 d . . .
H7A H 0.0406 0.4755 0.2448 0.025 Uiso 1 1 calc R . .
H7B H 0.0865 0.5714 0.2763 0.025 Uiso 1 1 calc R . .
C8 C 0.4979(14) 0.6197(7) 0.1823(5) 0.013(2) Uani 1 1 d . . .
H8A H 0.4789 0.6576 0.2254 0.016 Uiso 1 1 calc R . .
H8B H 0.6477 0.6104 0.1641 0.016 Uiso 1 1 calc R . .
C9 C 0.4220(15) 0.4545(7) 0.1253(5) 0.019(2) Uani 1 1 d . . .
H9A H 0.5698 0.4413 0.1056 0.023 Uiso 1 1 calc R . .
H9B H 0.3562 0.3900 0.1335 0.023 Uiso 1 1 calc R . .
C10 C 0.1555(14) 0.7009(7) 0.1386(6) 0.020(2) Uani 1 1 d . . .
H10A H 0.1343 0.7293 0.1870 0.024 Uiso 1 1 calc R . .
H10B H 0.0913 0.7523 0.0953 0.024 Uiso 1 1 calc R . .
C11 C 0.4215(16) 0.6289(7) 0.0441(5) 0.022(2) Uani 1 1 d . . .
H11A H 0.3683 0.6761 -0.0038 0.026 Uiso 1 1 calc R . .
H11B H 0.5717 0.6123 0.0305 0.026 Uiso 1 1 calc R . .
C12 C 0.0975(14) 0.5578(7) 0.0888(5) 0.019(2) Uani 1 1 d . . .
H12A H 0.0324 0.6023 0.0425 0.022 Uiso 1 1 calc R . .
H12B H 0.0330 0.4921 0.1045 0.022 Uiso 1 1 calc R . .
C13 C 0.4325(16) 0.4012(8) 0.4533(6) 0.025(2) Uani 1 1 d . . .
H13A H 0.3131 0.3658 0.4865 0.030 Uiso 1 1 calc R . .
C14 C 0.4231(17) 0.5040(8) 0.4028(6) 0.029(3) Uani 1 1 d . . .
H14A H 0.2962 0.5532 0.3951 0.035 Uiso 1 1 calc R . .
C15 C 0.6284(16) 0.5271(8) 0.3755(5) 0.022(2) Uani 1 1 d . . .
H15A H 0.6711 0.5945 0.3415 0.026 Uiso 1 1 calc R . .
C16 C 0.7648(15) 0.4385(8) 0.4031(5) 0.023(2) Uani 1 1 d . . .
H16A H 0.9191 0.4330 0.3926 0.028 Uiso 1 1 calc R . .
C17 C 0.6442(16) 0.3623(8) 0.4519(6) 0.024(2) Uani 1 1 d . . .
H17A H 0.6987 0.2933 0.4825 0.029 Uiso 1 1 calc R . .
O2S O 0.4139(12) 0.8806(5) 0.1214(4) 0.040(2) Uani 1 1 d . . .
O1S O 0.6970(12) -0.0061(6) 0.1656(4) 0.038(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0219(5) 0.0106(4) 0.0097(4) -0.0006(3) -0.0029(3) -0.0022(3)
Cl1 0.0242(14) 0.0168(13) 0.0175(13) -0.0019(10) -0.0027(10) -0.0009(11)
P1 0.0210(15) 0.0160(13) 0.0102(12) 0.0008(10) -0.0026(11) -0.0013(11)
P2 0.0224(15) 0.0136(13) 0.0115(13) 0.0006(10) -0.0025(11) -0.0021(11)
P3 0.0284(17) 0.0148(14) 0.0199(14) -0.0017(11) -0.0003(12) 0.0000(12)
P4 0.0344(18) 0.0237(16) 0.0186(15) -0.0018(12) -0.0056(13) -0.0019(13)
F1 0.031(4) 0.039(4) 0.033(4) -0.009(3) 0.000(3) 0.016(3)
F2 0.027(3) 0.018(3) 0.034(4) -0.004(3) 0.000(3) 0.006(3)
F3 0.028(4) 0.037(4) 0.030(3) -0.010(3) 0.007(3) -0.003(3)
F4 0.068(5) 0.023(3) 0.025(3) 0.008(3) -0.016(3) -0.012(3)
F5 0.063(5) 0.023(3) 0.020(3) -0.006(3) -0.010(3) -0.007(3)
F6 0.039(4) 0.025(3) 0.028(3) -0.008(3) -0.003(3) -0.010(3)
F7 0.041(4) 0.035(4) 0.035(4) 0.000(3) -0.016(3) 0.000(3)
F8 0.033(4) 0.034(4) 0.022(3) -0.001(3) -0.005(3) 0.000(3)
F9 0.033(4) 0.044(4) 0.024(3) 0.013(3) -0.010(3) -0.010(3)
F10 0.061(5) 0.048(4) 0.013(3) 0.009(3) -0.015(3) -0.003(3)
F11 0.064(5) 0.022(3) 0.026(3) 0.000(3) -0.009(3) -0.002(3)
F12 0.053(4) 0.039(4) 0.029(4) -0.012(3) -0.013(3) 0.004(3)
N1 0.024(5) 0.010(4) 0.015(4) 0.000(3) -0.007(4) -0.001(4)
N2 0.022(5) 0.018(5) 0.018(4) 0.007(4) -0.009(4) 0.005(4)
N3 0.027(5) 0.015(4) 0.013(4) -0.001(3) -0.002(4) -0.004(4)
N4 0.026(5) 0.014(4) 0.014(4) -0.001(3) -0.002(4) -0.002(4)
N5 0.017(5) 0.019(4) 0.018(4) 0.000(3) -0.008(4) -0.010(4)
N6 0.036(6) 0.022(5) 0.010(4) -0.004(4) -0.002(4) -0.001(4)
C1 0.017(5) 0.015(5) 0.013(5) -0.002(4) 0.003(4) 0.000(4)
C2 0.025(6) 0.004(5) 0.028(6) 0.000(4) -0.003(5) 0.002(4)
C3 0.023(6) 0.014(5) 0.021(5) 0.003(4) -0.014(4) -0.005(4)
C4 0.021(6) 0.011(5) 0.012(5) 0.002(4) -0.003(4) 0.005(4)
C5 0.018(6) 0.011(5) 0.036(6) -0.001(4) -0.012(5) -0.003(4)
C6 0.033(7) 0.025(6) 0.012(5) -0.001(4) 0.003(5) -0.015(5)
C7 0.020(6) 0.028(6) 0.011(5) 0.000(4) -0.004(4) 0.004(5)
C8 0.019(5) 0.014(5) 0.007(5) 0.000(4) -0.004(4) 0.000(4)
C9 0.029(6) 0.007(5) 0.022(5) -0.002(4) -0.013(5) 0.005(4)
C10 0.023(6) 0.022(6) 0.018(5) -0.008(4) -0.002(4) -0.003(5)
C11 0.039(7) 0.012(5) 0.012(5) 0.002(4) -0.003(5) 0.001(5)
C12 0.019(6) 0.024(6) 0.016(5) -0.009(4) -0.005(4) -0.001(4)
C13 0.023(6) 0.027(6) 0.026(6) -0.006(5) -0.004(5) -0.005(5)
C14 0.031(7) 0.036(7) 0.024(6) -0.014(5) -0.008(5) 0.001(5)
C15 0.036(7) 0.025(6) 0.008(5) 0.000(4) -0.007(4) -0.020(5)
C16 0.018(6) 0.036(6) 0.015(5) -0.008(5) -0.007(4) 0.008(5)
C17 0.037(7) 0.024(6) 0.016(5) -0.007(4) -0.009(5) -0.010(5)
O2S 0.059(6) 0.016(4) 0.039(5) -0.005(3) 0.010(4) -0.002(4)
O1S 0.045(5) 0.039(5) 0.030(4) -0.009(4) -0.001(4) -0.005(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 Ru1 C13 38.7(4) . . ?
C14 Ru1 C17 63.4(4) . . ?
C13 Ru1 C17 37.6(4) . . ?
C14 Ru1 C15 37.2(4) . . ?
C13 Ru1 C15 62.3(4) . . ?
C17 Ru1 C15 61.4(3) . . ?
C14 Ru1 C16 63.0(4) . . ?
C13 Ru1 C16 62.4(4) . . ?
C17 Ru1 C16 36.6(3) . . ?
C15 Ru1 C16 36.9(3) . . ?
C14 Ru1 P1 122.4(3) . . ?
C13 Ru1 P1 92.0(3) . . ?
C17 Ru1 P1 97.0(3) . . ?
C15 Ru1 P1 154.2(2) . . ?
C16 Ru1 P1 130.2(3) . . ?
C14 Ru1 P2 92.4(3) . . ?
C13 Ru1 P2 123.4(3) . . ?
C17 Ru1 P2 155.6(3) . . ?
C15 Ru1 P2 97.8(2) . . ?
C16 Ru1 P2 130.7(3) . . ?
P1 Ru1 P2 99.05(10) . . ?
C14 Ru1 Cl1 151.4(3) . . ?
C13 Ru1 Cl1 149.6(3) . . ?
C17 Ru1 Cl1 112.6(3) . . ?
C15 Ru1 Cl1 114.6(3) . . ?
C16 Ru1 Cl1 96.4(3) . . ?
P1 Ru1 Cl1 85.86(9) . . ?
P2 Ru1 Cl1 86.80(9) . . ?
C3 P1 C1 98.3(4) . . ?
C3 P1 C2 97.8(4) . . ?
C1 P1 C2 97.7(4) . . ?
C3 P1 Ru1 120.2(3) . . ?
C1 P1 Ru1 114.9(3) . . ?
C2 P1 Ru1 122.9(3) . . ?
C8 P2 C7 98.0(4) . . ?
C8 P2 C9 97.2(4) . . ?
C7 P2 C9 98.6(4) . . ?
C8 P2 Ru1 113.3(3) . . ?
C7 P2 Ru1 121.3(3) . . ?
C9 P2 Ru1 123.3(3) . . ?
F3 P3 F2 89.3(3) . . ?
F3 P3 F6 91.4(3) . . ?
F2 P3 F6 91.4(3) . . ?
F3 P3 F1 178.9(4) . . ?
F2 P3 F1 90.3(3) . . ?
F6 P3 F1 89.6(3) . . ?
F3 P3 F5 89.0(3) . . ?
F2 P3 F5 89.8(3) . . ?
F6 P3 F5 178.7(3) . . ?
F1 P3 F5 89.9(3) . . ?
F3 P3 F4 90.3(3) . . ?
F2 P3 F4 179.5(4) . . ?
F6 P3 F4 88.4(3) . . ?
F1 P3 F4 90.1(3) . . ?
F5 P3 F4 90.3(3) . . ?
F11 P4 F9 89.5(4) . . ?
F11 P4 F12 179.9(5) . . ?
F9 P4 F12 90.6(4) . . ?
F11 P4 F7 91.0(4) . . ?
F9 P4 F7 179.1(3) . . ?
F12 P4 F7 89.0(3) . . ?
F11 P4 F8 90.2(3) . . ?
F9 P4 F8 90.3(3) . . ?
F12 P4 F8 89.7(3) . . ?
F7 P4 F8 90.5(3) . . ?
F11 P4 F10 90.0(3) . . ?
F9 P4 F10 89.7(3) . . ?
F12 P4 F10 90.0(3) . . ?
F7 P4 F10 89.5(3) . . ?
F8 P4 F10 179.7(4) . . ?
C6 N1 C4 110.8(8) . . ?
C6 N1 C1 111.6(7) . . ?
C4 N1 C1 110.0(7) . . ?
C5 N2 C4 110.1(7) . . ?
C5 N2 C2 112.2(7) . . ?
C4 N2 C2 112.0(7) . . ?
C6 N3 C5 108.1(7) . . ?
C6 N3 C3 110.0(7) . . ?
C5 N3 C3 110.6(7) . . ?
C6 N3 H3C 109.4 . . ?
C5 N3 H3C 109.4 . . ?
C3 N3 H3C 109.4 . . ?
C10 N4 C12 112.1(7) . . ?
C10 N4 C7 110.9(8) . . ?
C12 N4 C7 111.0(7) . . ?
C11 N5 C8 110.6(7) . . ?
C11 N5 C10 109.8(7) . . ?
C8 N5 C10 111.1(7) . . ?
C11 N5 H5C 108.4 . . ?
C8 N5 H5C 108.4 . . ?
C10 N5 H5C 108.4 . . ?
C11 N6 C12 110.8(8) . . ?
C11 N6 C9 112.0(8) . . ?
C12 N6 C9 112.0(7) . . ?
N1 C1 P1 112.7(6) . . ?
N1 C1 H1A 109.0 . . ?
P1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
P1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 P1 111.9(6) . . ?
N2 C2 H2A 109.2 . . ?
P1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
P1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N3 C3 P1 111.8(6) . . ?
N3 C3 H3A 109.2 . . ?
P1 C3 H3A 109.2 . . ?
N3 C3 H3B 109.2 . . ?
P1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 N2 112.7(7) . . ?
N1 C4 H4A 109.1 . . ?
N2 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
N2 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 N3 112.3(7) . . ?
N2 C5 H5A 109.1 . . ?
N3 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
N3 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
N1 C6 N3 114.2(8) . . ?
N1 C6 H6A 108.7 . . ?
N3 C6 H6A 108.7 . . ?
N1 C6 H6B 108.7 . . ?
N3 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
N4 C7 P2 112.4(6) . . ?
N4 C7 H7A 109.1 . . ?
P2 C7 H7A 109.1 . . ?
N4 C7 H7B 109.1 . . ?
P2 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N5 C8 P2 111.3(6) . . ?
N5 C8 H8A 109.4 . . ?
P2 C8 H8A 109.4 . . ?
N5 C8 H8B 109.4 . . ?
P2 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N6 C9 P2 111.2(6) . . ?
N6 C9 H9A 109.4 . . ?
P2 C9 H9A 109.4 . . ?
N6 C9 H9B 109.4 . . ?
P2 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N4 C10 N5 111.4(8) . . ?
N4 C10 H10A 109.4 . . ?
N5 C10 H10A 109.4 . . ?
N4 C10 H10B 109.4 . . ?
N5 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N6 C11 N5 111.8(7) . . ?
N6 C11 H11A 109.2 . . ?
N5 C11 H11A 109.2 . . ?
N6 C11 H11B 109.2 . . ?
N5 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 N6 112.4(7) . . ?
N4 C12 H12A 109.1 . . ?
N6 C12 H12A 109.1 . . ?
N4 C12 H12B 109.1 . . ?
N6 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C17 C13 C14 107.4(9) . . ?
C17 C13 Ru1 72.7(6) . . ?
C14 C13 Ru1 69.9(6) . . ?
C17 C13 H13A 126.2 . . ?
C14 C13 H13A 126.2 . . ?
Ru1 C13 H13A 126.2 . . ?
C15 C14 C13 107.1(9) . . ?
C15 C14 Ru1 74.5(6) . . ?
C13 C14 Ru1 71.4(6) . . ?
C15 C14 H14A 126.2 . . ?
C13 C14 H14A 126.2 . . ?
Ru1 C14 H14A 126.2 . . ?
C14 C15 C16 109.0(9) . . ?
C14 C15 Ru1 68.3(5) . . ?
C16 C15 Ru1 71.6(6) . . ?
C14 C15 H15A 125.5 . . ?
C16 C15 H15A 125.5 . . ?
Ru1 C15 H15A 125.5 . . ?
C17 C16 C15 107.6(9) . . ?
C17 C16 Ru1 70.7(6) . . ?
C15 C16 Ru1 71.5(5) . . ?
C17 C16 H16A 126.2 . . ?
C15 C16 H16A 126.2 . . ?
Ru1 C16 H16A 126.2 . . ?
C16 C17 C13 108.8(9) . . ?
C16 C17 Ru1 72.6(6) . . ?
C13 C17 Ru1 69.7(6) . . ?
C16 C17 H17A 125.6 . . ?
C13 C17 H17A 125.6 . . ?
Ru1 C17 H17A 125.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C14 2.166(10) . ?
Ru1 C13 2.185(10) . ?
Ru1 C17 2.223(9) . ?
Ru1 C15 2.246(9) . ?
Ru1 C16 2.247(10) . ?
Ru1 P1 2.254(3) . ?
Ru1 P2 2.257(3) . ?
Ru1 Cl1 2.455(2) . ?
P1 C3 1.838(9) . ?
P1 C1 1.844(9) . ?
P1 C2 1.845(10) . ?
P2 C8 1.845(9) . ?
P2 C7 1.846(9) . ?
P2 C9 1.857(9) . ?
P3 F3 1.583(6) . ?
P3 F2 1.589(6) . ?
P3 F6 1.590(6) . ?
P3 F1 1.595(6) . ?
P3 F5 1.600(6) . ?
P3 F4 1.617(6) . ?
P4 F11 1.578(6) . ?
P4 F9 1.596(6) . ?
P4 F12 1.598(6) . ?
P4 F7 1.601(6) . ?
P4 F8 1.609(6) . ?
P4 F10 1.609(6) . ?
N1 C6 1.414(11) . ?
N1 C4 1.471(11) . ?
N1 C1 1.489(11) . ?
N2 C5 1.441(12) . ?
N2 C4 1.471(10) . ?
N2 C2 1.481(11) . ?
N3 C6 1.508(12) . ?
N3 C5 1.517(12) . ?
N3 C3 1.527(11) . ?
N3 H3C 0.9300 . ?
N4 C10 1.425(11) . ?
N4 C12 1.462(11) . ?
N4 C7 1.502(10) . ?
N5 C11 1.510(11) . ?
N5 C8 1.515(10) . ?
N5 C10 1.528(11) . ?
N5 H5C 0.9300 . ?
N6 C11 1.424(12) . ?
N6 C12 1.482(12) . ?
N6 C9 1.494(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C17 1.421(14) . ?
C13 C14 1.442(14) . ?
C13 H13A 1.0000 . ?
C14 C15 1.409(13) . ?
C14 H14A 1.0000 . ?
C15 C16 1.423(13) . ?
C15 H15A 1.0000 . ?
C16 C17 1.405(13) . ?
C16 H16A 1.0000 . ?
C17 H17A 1.0000 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C O1S 0.93 2.52 3.104(10) 121.4 .
N5 H5C O2S 0.93 1.96 2.743(10) 140.1 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 Ru1 P1 C3 148.0(5) . . . . ?
C13 Ru1 P1 C3 173.4(5) . . . . ?
C17 Ru1 P1 C3 -149.2(5) . . . . ?
C15 Ru1 P1 C3 179.3(7) . . . . ?
C16 Ru1 P1 C3 -131.8(5) . . . . ?
P2 Ru1 P1 C3 49.2(4) . . . . ?
Cl1 Ru1 P1 C3 -36.9(4) . . . . ?
C14 Ru1 P1 C1 -95.0(5) . . . . ?
C13 Ru1 P1 C1 -69.5(4) . . . . ?
C17 Ru1 P1 C1 -32.1(4) . . . . ?
C15 Ru1 P1 C1 -63.7(7) . . . . ?
C16 Ru1 P1 C1 -14.7(5) . . . . ?
P2 Ru1 P1 C1 166.3(3) . . . . ?
Cl1 Ru1 P1 C1 80.2(3) . . . . ?
C14 Ru1 P1 C2 23.6(5) . . . . ?
C13 Ru1 P1 C2 49.1(5) . . . . ?
C17 Ru1 P1 C2 86.5(5) . . . . ?
C15 Ru1 P1 C2 54.9(7) . . . . ?
C16 Ru1 P1 C2 103.8(5) . . . . ?
P2 Ru1 P1 C2 -75.2(4) . . . . ?
Cl1 Ru1 P1 C2 -161.3(4) . . . . ?
C14 Ru1 P2 C8 64.9(4) . . . . ?
C13 Ru1 P2 C8 89.8(5) . . . . ?
C17 Ru1 P2 C8 57.5(7) . . . . ?
C15 Ru1 P2 C8 27.9(4) . . . . ?
C16 Ru1 P2 C8 9.2(5) . . . . ?
P1 Ru1 P2 C8 -171.8(3) . . . . ?
Cl1 Ru1 P2 C8 -86.5(3) . . . . ?
C14 Ru1 P2 C7 -51.2(5) . . . . ?
C13 Ru1 P2 C7 -26.3(5) . . . . ?
C17 Ru1 P2 C7 -58.6(8) . . . . ?
C15 Ru1 P2 C7 -88.2(5) . . . . ?
C16 Ru1 P2 C7 -106.9(5) . . . . ?
P1 Ru1 P2 C7 72.1(4) . . . . ?
Cl1 Ru1 P2 C7 157.4(4) . . . . ?
C14 Ru1 P2 C9 -178.6(5) . . . . ?
C13 Ru1 P2 C9 -153.7(5) . . . . ?
C17 Ru1 P2 C9 174.0(7) . . . . ?
C15 Ru1 P2 C9 144.4(5) . . . . ?
C16 Ru1 P2 C9 125.7(5) . . . . ?
P1 Ru1 P2 C9 -55.3(4) . . . . ?
Cl1 Ru1 P2 C9 30.0(4) . . . . ?
C6 N1 C1 P1 61.4(9) . . . . ?
C4 N1 C1 P1 -62.0(8) . . . . ?
C3 P1 C1 N1 -49.3(7) . . . . ?
C2 P1 C1 N1 49.9(7) . . . . ?
Ru1 P1 C1 N1 -178.2(5) . . . . ?
C5 N2 C2 P1 -63.6(9) . . . . ?
C4 N2 C2 P1 60.8(9) . . . . ?
C3 P1 C2 N2 51.0(7) . . . . ?
C1 P1 C2 N2 -48.6(7) . . . . ?
Ru1 P1 C2 N2 -175.1(5) . . . . ?
C6 N3 C3 P1 -59.2(9) . . . . ?
C5 N3 C3 P1 60.2(8) . . . . ?
C1 P1 C3 N3 48.9(7) . . . . ?
C2 P1 C3 N3 -50.1(7) . . . . ?
Ru1 P1 C3 N3 174.2(5) . . . . ?
C6 N1 C4 N2 -55.2(10) . . . . ?
C1 N1 C4 N2 68.6(9) . . . . ?
C5 N2 C4 N1 56.7(10) . . . . ?
C2 N2 C4 N1 -68.9(10) . . . . ?
C4 N2 C5 N3 -56.7(10) . . . . ?
C2 N2 C5 N3 68.8(9) . . . . ?
C6 N3 C5 N2 53.9(9) . . . . ?
C3 N3 C5 N2 -66.6(9) . . . . ?
C4 N1 C6 N3 54.3(10) . . . . ?
C1 N1 C6 N3 -68.7(10) . . . . ?
C5 N3 C6 N1 -53.2(10) . . . . ?
C3 N3 C6 N1 67.7(10) . . . . ?
C10 N4 C7 P2 -64.1(9) . . . . ?
C12 N4 C7 P2 61.1(9) . . . . ?
C8 P2 C7 N4 50.0(7) . . . . ?
C9 P2 C7 N4 -48.6(7) . . . . ?
Ru1 P2 C7 N4 173.6(5) . . . . ?
C11 N5 C8 P2 -61.7(8) . . . . ?
C10 N5 C8 P2 60.5(8) . . . . ?
C7 P2 C8 N5 -48.8(7) . . . . ?
C9 P2 C8 N5 50.9(7) . . . . ?
Ru1 P2 C8 N5 -178.0(5) . . . . ?
C11 N6 C9 P2 64.3(9) . . . . ?
C12 N6 C9 P2 -60.9(9) . . . . ?
C8 P2 C9 N6 -51.1(7) . . . . ?
C7 P2 C9 N6 48.2(7) . . . . ?
Ru1 P2 C9 N6 -175.2(5) . . . . ?
C12 N4 C10 N5 -54.4(10) . . . . ?
C7 N4 C10 N5 70.3(9) . . . . ?
C11 N5 C10 N4 53.2(9) . . . . ?
C8 N5 C10 N4 -69.5(9) . . . . ?
C12 N6 C11 N5 55.9(10) . . . . ?
C9 N6 C11 N5 -69.9(10) . . . . ?
C8 N5 C11 N6 68.5(10) . . . . ?
C10 N5 C11 N6 -54.5(10) . . . . ?
C10 N4 C12 N6 55.8(10) . . . . ?
C7 N4 C12 N6 -68.8(10) . . . . ?
C11 N6 C12 N4 -56.2(10) . . . . ?
C9 N6 C12 N4 69.6(10) . . . . ?
C14 Ru1 C13 C17 -116.6(9) . . . . ?
C15 Ru1 C13 C17 -78.2(6) . . . . ?
C16 Ru1 C13 C17 -36.3(6) . . . . ?
P1 Ru1 C13 C17 98.9(6) . . . . ?
P2 Ru1 C13 C17 -158.9(5) . . . . ?
Cl1 Ru1 C13 C17 13.8(9) . . . . ?
C17 Ru1 C13 C14 116.6(9) . . . . ?
C15 Ru1 C13 C14 38.4(6) . . . . ?
C16 Ru1 C13 C14 80.3(6) . . . . ?
P1 Ru1 C13 C14 -144.5(6) . . . . ?
P2 Ru1 C13 C14 -42.3(7) . . . . ?
Cl1 Ru1 C13 C14 130.3(6) . . . . ?
C17 C13 C14 C15 -3.0(11) . . . . ?
Ru1 C13 C14 C15 -66.5(7) . . . . ?
C17 C13 C14 Ru1 63.4(7) . . . . ?
C13 Ru1 C14 C15 114.6(8) . . . . ?
C17 Ru1 C14 C15 76.9(6) . . . . ?
C16 Ru1 C14 C15 35.7(5) . . . . ?
P1 Ru1 C14 C15 158.0(5) . . . . ?
P2 Ru1 C14 C15 -99.7(5) . . . . ?
Cl1 Ru1 C14 C15 -11.9(10) . . . . ?
C17 Ru1 C14 C13 -37.6(6) . . . . ?
C15 Ru1 C14 C13 -114.6(8) . . . . ?
C16 Ru1 C14 C13 -78.8(6) . . . . ?
P1 Ru1 C14 C13 43.4(7) . . . . ?
P2 Ru1 C14 C13 145.8(6) . . . . ?
Cl1 Ru1 C14 C13 -126.4(6) . . . . ?
C13 C14 C15 C16 4.1(11) . . . . ?
Ru1 C14 C15 C16 -60.3(7) . . . . ?
C13 C14 C15 Ru1 64.4(7) . . . . ?
C13 Ru1 C15 C14 -40.0(6) . . . . ?
C17 Ru1 C15 C14 -82.8(6) . . . . ?
C16 Ru1 C15 C14 -120.1(8) . . . . ?
P1 Ru1 C15 C14 -46.5(9) . . . . ?
P2 Ru1 C15 C14 83.7(6) . . . . ?
Cl1 Ru1 C15 C14 173.8(5) . . . . ?
C14 Ru1 C15 C16 120.1(8) . . . . ?
C13 Ru1 C15 C16 80.1(6) . . . . ?
C17 Ru1 C15 C16 37.3(6) . . . . ?
P1 Ru1 C15 C16 73.5(9) . . . . ?
P2 Ru1 C15 C16 -156.2(5) . . . . ?
Cl1 Ru1 C15 C16 -66.1(6) . . . . ?
C14 C15 C16 C17 -3.7(11) . . . . ?
Ru1 C15 C16 C17 -61.9(7) . . . . ?
C14 C15 C16 Ru1 58.2(6) . . . . ?
C14 Ru1 C16 C17 81.0(6) . . . . ?
C13 Ru1 C16 C17 37.3(6) . . . . ?
C15 Ru1 C16 C17 117.0(8) . . . . ?
P1 Ru1 C16 C17 -29.8(7) . . . . ?
P2 Ru1 C16 C17 148.9(5) . . . . ?
Cl1 Ru1 C16 C17 -119.8(6) . . . . ?
C14 Ru1 C16 C15 -36.0(6) . . . . ?
C13 Ru1 C16 C15 -79.8(6) . . . . ?
C17 Ru1 C16 C15 -117.0(8) . . . . ?
P1 Ru1 C16 C15 -146.8(5) . . . . ?
P2 Ru1 C16 C15 31.9(7) . . . . ?
Cl1 Ru1 C16 C15 123.2(5) . . . . ?
C15 C16 C17 C13 1.7(11) . . . . ?
Ru1 C16 C17 C13 -60.7(7) . . . . ?
C15 C16 C17 Ru1 62.4(6) . . . . ?
C14 C13 C17 C16 0.8(11) . . . . ?
Ru1 C13 C17 C16 62.5(7) . . . . ?
C14 C13 C17 Ru1 -61.7(7) . . . . ?
C14 Ru1 C17 C16 -79.7(6) . . . . ?
C13 Ru1 C17 C16 -118.4(9) . . . . ?
C15 Ru1 C17 C16 -37.5(6) . . . . ?
P1 Ru1 C17 C16 157.5(5) . . . . ?
P2 Ru1 C17 C16 -71.5(9) . . . . ?
Cl1 Ru1 C17 C16 69.1(6) . . . . ?
C14 Ru1 C17 C13 38.7(6) . . . . ?
C15 Ru1 C17 C13 80.8(6) . . . . ?
C16 Ru1 C17 C13 118.4(9) . . . . ?
P1 Ru1 C17 C13 -84.1(6) . . . . ?
P2 Ru1 C17 C13 46.9(10) . . . . ?
Cl1 Ru1 C17 C13 -172.5(5) . . . . ?
|
1100802.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 07:52:51 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180561 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100802.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100802
loop_
_publ_author_name
'Mebi, Charles A.'
'Frost, Brian J.'
_publ_section_title
;
Effect of pH on the Biphasic Catalytic Hydrogenation of Benzylidene
Acetone Using CpRu(PTA)~2~H
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2339
_journal_page_last 2346
_journal_paper_doi 10.1021/om048987r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C17 H30 Cl F6 N6 O3 P3 Ru'
_chemical_formula_weight 709.90
_space_group_IT_number 33
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 26.2152(19)
_cell_length_b 14.9540(11)
_cell_length_c 6.4535(5)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 2529.9(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 123(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0845
_diffrn_reflns_av_sigmaI/netI 0.1061
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -33
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 14733
_diffrn_reflns_theta_full 27.89
_diffrn_reflns_theta_max 27.89
_diffrn_reflns_theta_min 1.55
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.994
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 1.864
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rod
_exptl_crystal_F_000 1432
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_refine_diff_density_max 1.164
_refine_diff_density_min -0.583
_refine_diff_density_rms 0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.07(4)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.928
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 338
_refine_ls_number_reflns 5488
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.928
_refine_ls_R_factor_all 0.0745
_refine_ls_R_factor_gt 0.0471
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0918
_refine_ls_wR_factor_ref 0.0984
_reflns_number_gt 3830
_reflns_number_total 5488
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om048987rsi20041221_041543.cif
_cod_data_source_block bjf019b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Pna2(1)
_cod_database_code 1100802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.487140(17) 0.28176(3) 0.46164(6) 0.01026(11) Uani 1 1 d . . .
P1 P 0.42100(6) 0.21910(10) 0.2885(2) 0.0108(3) Uani 1 1 d . . .
P2 P 0.55227(6) 0.21814(10) 0.2838(2) 0.0111(3) Uani 1 1 d . . .
P3 P 0.29328(7) 0.49840(11) 1.2764(3) 0.0186(4) Uani 1 1 d . . .
Cl1 Cl 0.48665(6) 0.14645(9) 0.6807(2) 0.0150(3) Uani 1 1 d . . .
N1 N 0.36758(19) 0.0701(3) 0.1556(8) 0.0130(11) Uani 1 1 d . . .
N2 N 0.31606(19) 0.1871(3) 0.3217(7) 0.0122(11) Uani 1 1 d . . .
N3 N 0.35000(17) 0.2097(3) -0.0265(10) 0.0135(10) Uani 1 1 d . . .
N4 N 0.60748(19) 0.0718(3) 0.1457(8) 0.0136(12) Uani 1 1 d . . .
N5 N 0.6571(2) 0.1931(3) 0.3023(8) 0.0131(11) Uani 1 1 d . . .
H5N H 0.691(3) 0.203(4) 0.362(10) 0.03(2) Uiso 1 1 d . . .
N6 N 0.62118(15) 0.2133(3) -0.0435(10) 0.0127(9) Uani 1 1 d . . .
F1 F 0.34376(13) 0.4617(2) 1.4113(5) 0.0229(9) Uani 1 1 d . . .
F2 F 0.26266(14) 0.4005(2) 1.3271(6) 0.0240(9) Uani 1 1 d . . .
F3 F 0.26829(14) 0.5427(2) 1.4931(6) 0.0290(10) Uani 1 1 d . . .
F4 F 0.24290(14) 0.5342(2) 1.1391(6) 0.0227(9) Uani 1 1 d . . .
F5 F 0.31739(15) 0.4514(3) 1.0572(5) 0.0240(9) Uani 1 1 d . . .
F6 F 0.32397(13) 0.5953(2) 1.2224(6) 0.0214(9) Uani 1 1 d . . .
C1 C 0.4173(2) 0.0977(4) 0.2418(10) 0.0137(14) Uani 1 1 d . . .
H1A H 0.4447 0.0802 0.1444 0.016 Uiso 1 1 calc R . .
H1B H 0.4232 0.0658 0.3740 0.016 Uiso 1 1 calc R . .
C2 C 0.3600(2) 0.2326(4) 0.4278(9) 0.0106(14) Uani 1 1 d . . .
H2A H 0.3636 0.2079 0.5693 0.013 Uiso 1 1 calc R . .
H2B H 0.3523 0.2972 0.4409 0.013 Uiso 1 1 calc R . .
C3 C 0.3977(2) 0.2575(4) 0.0328(9) 0.0147(15) Uani 1 1 d . . .
H3A H 0.3911 0.3226 0.0379 0.018 Uiso 1 1 calc R . .
H3B H 0.4243 0.2465 -0.0733 0.018 Uiso 1 1 calc R . .
C4 C 0.3259(2) 0.0878(4) 0.2963(9) 0.0143(14) Uani 1 1 d . . .
H4A H 0.3339 0.0615 0.4333 0.017 Uiso 1 1 calc R . .
H4B H 0.2946 0.0586 0.2434 0.017 Uiso 1 1 calc R . .
C5 C 0.3577(2) 0.1133(3) -0.0453(12) 0.0138(12) Uani 1 1 d . . .
H5A H 0.3869 0.1019 -0.1390 0.017 Uiso 1 1 calc R . .
H5B H 0.3270 0.0861 -0.1087 0.017 Uiso 1 1 calc R . .
C6 C 0.3077(2) 0.2269(4) 0.1071(9) 0.0147(14) Uani 1 1 d . . .
H6A H 0.2764 0.2010 0.0457 0.018 Uiso 1 1 calc R . .
H6B H 0.3027 0.2923 0.1196 0.018 Uiso 1 1 calc R . .
C7 C 0.5575(2) 0.0959(4) 0.2366(10) 0.0160(14) Uani 1 1 d . . .
H7A H 0.5529 0.0636 0.3692 0.019 Uiso 1 1 calc R . .
H7B H 0.5299 0.0770 0.1414 0.019 Uiso 1 1 calc R . .
C8 C 0.6132(2) 0.2346(4) 0.4189(9) 0.0128(15) Uani 1 1 d . . .
H8A H 0.6196 0.2994 0.4359 0.015 Uiso 1 1 calc R . .
H8B H 0.6111 0.2076 0.5587 0.015 Uiso 1 1 calc R . .
C9 C 0.5733(2) 0.2575(4) 0.0253(9) 0.0155(15) Uani 1 1 d . . .
H9A H 0.5461 0.2453 -0.0771 0.019 Uiso 1 1 calc R . .
H9B H 0.5788 0.3229 0.0303 0.019 Uiso 1 1 calc R . .
C10 C 0.6498(2) 0.0920(4) 0.2793(10) 0.0160(14) Uani 1 1 d . . .
H10A H 0.6813 0.0653 0.2214 0.019 Uiso 1 1 calc R . .
H10B H 0.6438 0.0653 0.4174 0.019 Uiso 1 1 calc R . .
C11 C 0.6153(2) 0.1158(3) -0.0546(12) 0.0169(13) Uani 1 1 d . . .
H11A H 0.5859 0.1019 -0.1454 0.020 Uiso 1 1 calc R . .
H11B H 0.6462 0.0902 -0.1203 0.020 Uiso 1 1 calc R . .
C12 C 0.6640(2) 0.2338(4) 0.0866(9) 0.0148(15) Uani 1 1 d . . .
H12A H 0.6676 0.2995 0.0988 0.018 Uiso 1 1 calc R . .
H12B H 0.6955 0.2099 0.0229 0.018 Uiso 1 1 calc R . .
C13 C 0.4447(2) 0.3937(4) 0.6103(10) 0.0149(15) Uani 1 1 d . . .
H13A H 0.4087 0.3916 0.6611 0.018 Uiso 1 1 calc R . .
C14 C 0.4882(3) 0.3774(4) 0.7281(10) 0.0162(13) Uani 1 1 d . . .
H14A H 0.4885 0.3602 0.8778 0.019 Uiso 1 1 calc R . .
C15 C 0.5316(3) 0.3922(4) 0.6063(10) 0.0177(15) Uani 1 1 d . . .
H15A H 0.5678 0.3890 0.6540 0.021 Uiso 1 1 calc R . .
C16 C 0.5146(3) 0.4170(4) 0.4045(9) 0.0172(15) Uani 1 1 d . . .
H16A H 0.5367 0.4364 0.2865 0.021 Uiso 1 1 calc R . .
C17 C 0.4607(3) 0.4166(4) 0.4073(9) 0.0148(15) Uani 1 1 d . . .
H17A H 0.4380 0.4362 0.2914 0.018 Uiso 1 1 calc R . .
O1W O 0.36676(17) 0.5620(3) 0.7667(7) 0.0226(11) Uani 1 1 d . . .
O2W O 0.74774(17) 0.1141(3) 0.7693(7) 0.0217(11) Uani 1 1 d . . .
O3W O 0.73222(15) 0.2693(3) 0.5583(6) 0.0141(10) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0093(2) 0.00893(19) 0.0125(2) -0.0012(2) 0.0002(4) -0.0003(2)
P1 0.0093(8) 0.0107(7) 0.0123(8) -0.0006(7) 0.0004(7) -0.0004(7)
P2 0.0090(8) 0.0108(8) 0.0135(8) 0.0002(7) -0.0004(7) 0.0002(7)
P3 0.0166(9) 0.0203(8) 0.0187(8) 0.0007(7) -0.0008(8) 0.0015(7)
Cl1 0.0159(8) 0.0151(7) 0.0139(7) 0.0008(5) -0.0009(8) -0.0004(7)
N1 0.012(3) 0.014(3) 0.013(3) 0.005(2) -0.002(2) -0.002(2)
N2 0.011(3) 0.015(2) 0.011(3) -0.002(2) -0.004(2) 0.000(2)
N3 0.013(2) 0.017(2) 0.010(2) 0.003(3) -0.005(3) -0.005(2)
N4 0.009(3) 0.014(3) 0.017(3) 0.000(2) 0.001(2) 0.001(2)
N5 0.007(3) 0.017(3) 0.016(3) 0.004(2) -0.002(2) 0.001(2)
N6 0.009(2) 0.017(2) 0.012(2) 0.002(3) -0.004(3) 0.000(2)
F1 0.017(2) 0.025(2) 0.027(3) -0.0026(16) -0.0072(17) 0.0067(16)
F2 0.018(2) 0.0217(19) 0.032(2) 0.0090(17) 0.0006(18) -0.0008(17)
F3 0.031(2) 0.037(2) 0.019(2) -0.0029(19) 0.006(2) 0.0147(17)
F4 0.015(2) 0.026(2) 0.026(2) 0.0088(18) -0.0090(18) -0.0057(17)
F5 0.034(2) 0.023(2) 0.0157(19) -0.0019(16) 0.0063(18) 0.0010(19)
F6 0.015(2) 0.0155(19) 0.034(2) 0.0033(16) -0.0051(17) -0.0036(16)
C1 0.010(3) 0.010(3) 0.021(4) 0.001(3) -0.001(3) 0.003(3)
C2 0.008(3) 0.015(3) 0.008(4) -0.002(3) 0.001(3) -0.002(2)
C3 0.017(4) 0.017(3) 0.010(3) 0.002(2) -0.001(3) -0.006(3)
C4 0.017(4) 0.017(3) 0.009(3) 0.000(3) 0.000(3) -0.007(3)
C5 0.013(3) 0.018(3) 0.009(3) -0.001(3) 0.002(4) 0.000(2)
C6 0.018(4) 0.017(3) 0.010(3) 0.002(3) -0.002(3) 0.001(3)
C7 0.011(3) 0.013(3) 0.023(4) 0.000(3) 0.005(3) 0.000(3)
C8 0.012(3) 0.012(3) 0.014(4) -0.001(2) -0.003(3) -0.002(2)
C9 0.014(3) 0.013(3) 0.019(4) -0.001(2) -0.001(3) 0.002(3)
C10 0.015(3) 0.017(3) 0.016(3) 0.002(3) -0.003(3) 0.005(3)
C11 0.011(3) 0.019(3) 0.020(4) -0.006(3) -0.001(4) 0.001(2)
C12 0.012(3) 0.019(4) 0.013(3) -0.001(3) 0.006(3) -0.002(3)
C13 0.011(4) 0.012(3) 0.022(4) -0.007(3) -0.001(3) 0.003(3)
C14 0.016(3) 0.007(3) 0.026(4) -0.008(2) 0.001(3) -0.003(3)
C15 0.016(4) 0.011(3) 0.026(4) -0.007(3) 0.007(3) -0.003(3)
C16 0.016(3) 0.010(3) 0.026(4) -0.004(2) 0.005(3) -0.001(3)
C17 0.015(3) 0.013(3) 0.017(4) -0.002(2) -0.003(3) 0.002(3)
O1W 0.020(3) 0.022(2) 0.026(3) 0.001(2) 0.000(2) -0.004(2)
O2W 0.024(3) 0.022(2) 0.019(2) -0.002(2) 0.001(2) 0.006(2)
O3W 0.012(2) 0.014(3) 0.016(2) -0.0003(16) 0.0002(19) -0.0026(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 Ru1 C16 38.0(2) . . ?
C17 Ru1 C15 62.8(2) . . ?
C16 Ru1 C15 37.7(2) . . ?
C17 Ru1 C13 37.7(2) . . ?
C16 Ru1 C13 62.6(2) . . ?
C15 Ru1 C13 61.5(2) . . ?
C17 Ru1 C14 62.1(2) . . ?
C16 Ru1 C14 62.1(2) . . ?
C15 Ru1 C14 36.6(2) . . ?
C13 Ru1 C14 36.3(2) . . ?
C17 Ru1 P1 93.47(18) . . ?
C16 Ru1 P1 123.61(18) . . ?
C15 Ru1 P1 156.08(18) . . ?
C13 Ru1 P1 98.13(17) . . ?
C14 Ru1 P1 130.79(18) . . ?
C17 Ru1 P2 123.43(17) . . ?
C16 Ru1 P2 93.13(18) . . ?
C15 Ru1 P2 97.44(18) . . ?
C13 Ru1 P2 155.48(18) . . ?
C14 Ru1 P2 130.41(18) . . ?
P1 Ru1 P2 98.81(5) . . ?
C17 Ru1 Cl1 148.91(17) . . ?
C16 Ru1 Cl1 149.29(17) . . ?
C15 Ru1 Cl1 111.77(18) . . ?
C13 Ru1 Cl1 111.51(17) . . ?
C14 Ru1 Cl1 94.81(16) . . ?
P1 Ru1 Cl1 86.53(5) . . ?
P2 Ru1 Cl1 87.13(5) . . ?
C1 P1 C2 98.2(3) . . ?
C1 P1 C3 98.2(3) . . ?
C2 P1 C3 96.6(3) . . ?
C1 P1 Ru1 121.9(2) . . ?
C2 P1 Ru1 112.20(18) . . ?
C3 P1 Ru1 124.3(2) . . ?
C8 P2 C9 97.2(3) . . ?
C8 P2 C7 98.3(3) . . ?
C9 P2 C7 98.2(3) . . ?
C8 P2 Ru1 111.01(19) . . ?
C9 P2 Ru1 123.2(2) . . ?
C7 P2 Ru1 123.5(2) . . ?
F1 P3 F4 179.3(2) . . ?
F1 P3 F3 90.2(2) . . ?
F4 P3 F3 90.4(2) . . ?
F1 P3 F6 90.67(19) . . ?
F4 P3 F6 89.55(19) . . ?
F3 P3 F6 91.1(2) . . ?
F1 P3 F2 89.49(19) . . ?
F4 P3 F2 90.28(19) . . ?
F3 P3 F2 89.7(2) . . ?
F6 P3 F2 179.2(2) . . ?
F1 P3 F5 90.19(19) . . ?
F4 P3 F5 89.2(2) . . ?
F3 P3 F5 178.5(2) . . ?
F6 P3 F5 90.4(2) . . ?
F2 P3 F5 88.8(2) . . ?
C4 N1 C5 109.9(5) . . ?
C4 N1 C1 112.3(5) . . ?
C5 N1 C1 111.4(5) . . ?
C2 N2 C4 111.2(4) . . ?
C2 N2 C6 110.3(5) . . ?
C4 N2 C6 108.0(4) . . ?
C6 N3 C5 109.6(5) . . ?
C6 N3 C3 114.2(5) . . ?
C5 N3 C3 112.2(4) . . ?
C10 N4 C11 109.0(5) . . ?
C10 N4 C7 113.2(5) . . ?
C11 N4 C7 111.3(5) . . ?
C8 N5 C12 112.4(4) . . ?
C8 N5 C10 111.1(5) . . ?
C12 N5 C10 108.6(5) . . ?
C8 N5 H5N 116(4) . . ?
C12 N5 H5N 101(4) . . ?
C10 N5 H5N 108(4) . . ?
C12 N6 C11 108.8(5) . . ?
C12 N6 C9 113.0(5) . . ?
C11 N6 C9 111.6(4) . . ?
N1 C1 P1 112.6(4) . . ?
N1 C1 H1A 109.1 . . ?
P1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
P1 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 P1 113.1(4) . . ?
N2 C2 H2A 109.0 . . ?
P1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
P1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C3 P1 110.9(4) . . ?
N3 C3 H3A 109.5 . . ?
P1 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 108.0 . . ?
N1 C4 N2 112.1(5) . . ?
N1 C4 H4A 109.2 . . ?
N2 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
N2 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N3 C5 N1 112.6(6) . . ?
N3 C5 H5A 109.1 . . ?
N1 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
N1 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N3 C6 N2 111.6(5) . . ?
N3 C6 H6A 109.3 . . ?
N2 C6 H6A 109.3 . . ?
N3 C6 H6B 109.3 . . ?
N2 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 P2 111.8(4) . . ?
N4 C7 H7A 109.3 . . ?
P2 C7 H7A 109.3 . . ?
N4 C7 H7B 109.3 . . ?
P2 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
N5 C8 P2 111.8(4) . . ?
N5 C8 H8A 109.3 . . ?
P2 C8 H8A 109.3 . . ?
N5 C8 H8B 109.3 . . ?
P2 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N6 C9 P2 112.3(4) . . ?
N6 C9 H9A 109.1 . . ?
P2 C9 H9A 109.1 . . ?
N6 C9 H9B 109.1 . . ?
P2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N4 C10 N5 111.3(5) . . ?
N4 C10 H10A 109.4 . . ?
N5 C10 H10A 109.4 . . ?
N4 C10 H10B 109.4 . . ?
N5 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N4 C11 N6 114.7(6) . . ?
N4 C11 H11A 108.6 . . ?
N6 C11 H11A 108.6 . . ?
N4 C11 H11B 108.6 . . ?
N6 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N6 C12 N5 110.8(5) . . ?
N6 C12 H12A 109.5 . . ?
N5 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C14 C13 C17 107.8(6) . . ?
C14 C13 Ru1 72.2(3) . . ?
C17 C13 Ru1 68.6(4) . . ?
C14 C13 H13A 126.1 . . ?
C17 C13 H13A 126.1 . . ?
Ru1 C13 H13A 126.1 . . ?
C13 C14 C15 109.3(6) . . ?
C13 C14 Ru1 71.4(3) . . ?
C15 C14 Ru1 71.3(3) . . ?
C13 C14 H14A 125.3 . . ?
C15 C14 H14A 125.3 . . ?
Ru1 C14 H14A 125.3 . . ?
C14 C15 C16 107.5(6) . . ?
C14 C15 Ru1 72.1(3) . . ?
C16 C15 Ru1 69.3(4) . . ?
C14 C15 H15A 126.2 . . ?
C16 C15 H15A 126.2 . . ?
Ru1 C15 H15A 126.2 . . ?
C17 C16 C15 107.4(6) . . ?
C17 C16 Ru1 70.3(4) . . ?
C15 C16 Ru1 73.0(4) . . ?
C17 C16 H16A 126.2 . . ?
C15 C16 H16A 126.2 . . ?
Ru1 C16 H16A 126.2 . . ?
C16 C17 C13 107.9(6) . . ?
C16 C17 Ru1 71.6(3) . . ?
C13 C17 Ru1 73.7(4) . . ?
C16 C17 H17A 125.8 . . ?
C13 C17 H17A 125.8 . . ?
Ru1 C17 H17A 125.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C17 2.161(6) . ?
Ru1 C16 2.178(6) . ?
Ru1 C15 2.226(6) . ?
Ru1 C13 2.226(6) . ?
Ru1 C14 2.237(6) . ?
Ru1 P1 2.2656(17) . ?
Ru1 P2 2.2668(16) . ?
Ru1 Cl1 2.4683(14) . ?
P1 C1 1.842(6) . ?
P1 C2 1.846(6) . ?
P1 C3 1.850(6) . ?
P2 C8 1.837(6) . ?
P2 C9 1.852(6) . ?
P2 C7 1.858(6) . ?
P3 F1 1.676(4) . ?
P3 F4 1.678(4) . ?
P3 F3 1.681(4) . ?
P3 F6 1.694(4) . ?
P3 F2 1.701(4) . ?
P3 F5 1.701(4) . ?
N1 C4 1.445(7) . ?
N1 C5 1.472(8) . ?
N1 C1 1.477(7) . ?
N2 C2 1.502(7) . ?
N2 C4 1.516(7) . ?
N2 C6 1.523(7) . ?
N3 C6 1.428(8) . ?
N3 C5 1.461(6) . ?
N3 C3 1.491(7) . ?
N4 C10 1.437(8) . ?
N4 C11 1.465(9) . ?
N4 C7 1.480(7) . ?
N5 C8 1.508(7) . ?
N5 C12 1.530(7) . ?
N5 C10 1.531(7) . ?
N5 H5N 0.98(7) . ?
N6 C12 1.435(8) . ?
N6 C11 1.467(7) . ?
N6 C9 1.486(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.391(9) . ?
C13 C17 1.418(9) . ?
C13 H13A 1.0000 . ?
C14 C15 1.400(9) . ?
C14 H14A 1.0000 . ?
C15 C16 1.425(9) . ?
C15 H15A 1.0000 . ?
C16 C17 1.413(8) . ?
C16 H16A 1.0000 . ?
C17 H17A 1.0000 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C17 Ru1 P1 C1 174.8(3) . . . . ?
C16 Ru1 P1 C1 149.9(3) . . . . ?
C15 Ru1 P1 C1 -177.6(5) . . . . ?
C13 Ru1 P1 C1 -147.7(3) . . . . ?
C14 Ru1 P1 C1 -129.8(3) . . . . ?
P2 Ru1 P1 C1 50.2(3) . . . . ?
Cl1 Ru1 P1 C1 -36.4(3) . . . . ?
C17 Ru1 P1 C2 -69.5(3) . . . . ?
C16 Ru1 P1 C2 -94.3(3) . . . . ?
C15 Ru1 P1 C2 -61.8(5) . . . . ?
C13 Ru1 P1 C2 -31.9(3) . . . . ?
C14 Ru1 P1 C2 -14.0(3) . . . . ?
P2 Ru1 P1 C2 165.9(2) . . . . ?
Cl1 Ru1 P1 C2 79.4(2) . . . . ?
C17 Ru1 P1 C3 45.9(3) . . . . ?
C16 Ru1 P1 C3 21.0(3) . . . . ?
C15 Ru1 P1 C3 53.5(5) . . . . ?
C13 Ru1 P1 C3 83.5(3) . . . . ?
C14 Ru1 P1 C3 101.4(3) . . . . ?
P2 Ru1 P1 C3 -78.7(3) . . . . ?
Cl1 Ru1 P1 C3 -165.3(3) . . . . ?
C17 Ru1 P2 C8 92.5(3) . . . . ?
C16 Ru1 P2 C8 67.9(3) . . . . ?
C15 Ru1 P2 C8 30.2(3) . . . . ?
C13 Ru1 P2 C8 59.4(5) . . . . ?
C14 Ru1 P2 C8 12.5(3) . . . . ?
P1 Ru1 P2 C8 -167.4(2) . . . . ?
Cl1 Ru1 P2 C8 -81.4(2) . . . . ?
C17 Ru1 P2 C9 -21.9(3) . . . . ?
C16 Ru1 P2 C9 -46.5(3) . . . . ?
C15 Ru1 P2 C9 -84.1(3) . . . . ?
C13 Ru1 P2 C9 -54.9(5) . . . . ?
C14 Ru1 P2 C9 -101.8(3) . . . . ?
P1 Ru1 P2 C9 78.2(2) . . . . ?
Cl1 Ru1 P2 C9 164.3(2) . . . . ?
C17 Ru1 P2 C7 -151.4(3) . . . . ?
C16 Ru1 P2 C7 -176.0(3) . . . . ?
C15 Ru1 P2 C7 146.3(3) . . . . ?
C13 Ru1 P2 C7 175.5(5) . . . . ?
C14 Ru1 P2 C7 128.6(3) . . . . ?
P1 Ru1 P2 C7 -51.3(3) . . . . ?
Cl1 Ru1 P2 C7 34.7(3) . . . . ?
C4 N1 C1 P1 -62.9(6) . . . . ?
C5 N1 C1 P1 60.8(6) . . . . ?
C2 P1 C1 N1 48.5(5) . . . . ?
C3 P1 C1 N1 -49.4(5) . . . . ?
Ru1 P1 C1 N1 171.1(3) . . . . ?
C4 N2 C2 P1 58.3(5) . . . . ?
C6 N2 C2 P1 -61.4(5) . . . . ?
C1 P1 C2 N2 -47.4(4) . . . . ?
C3 P1 C2 N2 51.9(4) . . . . ?
Ru1 P1 C2 N2 -176.8(3) . . . . ?
C6 N3 C3 P1 64.0(6) . . . . ?
C5 N3 C3 P1 -61.5(7) . . . . ?
C1 P1 C3 N3 48.8(5) . . . . ?
C2 P1 C3 N3 -50.5(5) . . . . ?
Ru1 P1 C3 N3 -173.1(3) . . . . ?
C5 N1 C4 N2 -55.6(6) . . . . ?
C1 N1 C4 N2 69.0(6) . . . . ?
C2 N2 C4 N1 -66.3(6) . . . . ?
C6 N2 C4 N1 54.9(6) . . . . ?
C6 N3 C5 N1 -59.2(6) . . . . ?
C3 N3 C5 N1 68.8(7) . . . . ?
C4 N1 C5 N3 57.3(6) . . . . ?
C1 N1 C5 N3 -67.7(6) . . . . ?
C5 N3 C6 N2 58.9(7) . . . . ?
C3 N3 C6 N2 -68.0(6) . . . . ?
C2 N2 C6 N3 65.2(6) . . . . ?
C4 N2 C6 N3 -56.6(6) . . . . ?
C10 N4 C7 P2 62.5(6) . . . . ?
C11 N4 C7 P2 -60.8(6) . . . . ?
C8 P2 C7 N4 -49.0(5) . . . . ?
C9 P2 C7 N4 49.6(5) . . . . ?
Ru1 P2 C7 N4 -171.1(3) . . . . ?
C12 N5 C8 P2 60.9(5) . . . . ?
C10 N5 C8 P2 -61.0(5) . . . . ?
C9 P2 C8 N5 -49.9(4) . . . . ?
C7 P2 C8 N5 49.5(4) . . . . ?
Ru1 P2 C8 N5 -179.7(3) . . . . ?
C12 N6 C9 P2 -64.0(6) . . . . ?
C11 N6 C9 P2 59.1(7) . . . . ?
C8 P2 C9 N6 50.7(4) . . . . ?
C7 P2 C9 N6 -48.8(5) . . . . ?
Ru1 P2 C9 N6 171.7(3) . . . . ?
C11 N4 C10 N5 55.9(6) . . . . ?
C7 N4 C10 N5 -68.6(6) . . . . ?
C8 N5 C10 N4 67.5(6) . . . . ?
C12 N5 C10 N4 -56.6(6) . . . . ?
C10 N4 C11 N6 -57.9(6) . . . . ?
C7 N4 C11 N6 67.7(6) . . . . ?
C12 N6 C11 N4 58.8(6) . . . . ?
C9 N6 C11 N4 -66.6(7) . . . . ?
C11 N6 C12 N5 -57.4(7) . . . . ?
C9 N6 C12 N5 67.2(6) . . . . ?
C8 N5 C12 N6 -66.0(6) . . . . ?
C10 N5 C12 N6 57.3(6) . . . . ?
C17 Ru1 C13 C14 -118.0(5) . . . . ?
C16 Ru1 C13 C14 -79.4(4) . . . . ?
C15 Ru1 C13 C14 -36.4(4) . . . . ?
P1 Ru1 C13 C14 156.9(3) . . . . ?
P2 Ru1 C13 C14 -69.8(6) . . . . ?
Cl1 Ru1 C13 C14 67.4(4) . . . . ?
C16 Ru1 C13 C17 38.6(3) . . . . ?
C15 Ru1 C13 C17 81.6(4) . . . . ?
C14 Ru1 C13 C17 118.0(5) . . . . ?
P1 Ru1 C13 C17 -85.1(4) . . . . ?
P2 Ru1 C13 C17 48.2(6) . . . . ?
Cl1 Ru1 C13 C17 -174.6(3) . . . . ?
C17 C13 C14 C15 1.9(6) . . . . ?
Ru1 C13 C14 C15 61.6(4) . . . . ?
C17 C13 C14 Ru1 -59.7(4) . . . . ?
C17 Ru1 C14 C13 37.6(4) . . . . ?
C16 Ru1 C14 C13 80.9(4) . . . . ?
C15 Ru1 C14 C13 118.8(5) . . . . ?
P1 Ru1 C14 C13 -30.9(4) . . . . ?
P2 Ru1 C14 C13 149.2(3) . . . . ?
Cl1 Ru1 C14 C13 -120.4(4) . . . . ?
C17 Ru1 C14 C15 -81.2(4) . . . . ?
C16 Ru1 C14 C15 -37.9(4) . . . . ?
C13 Ru1 C14 C15 -118.8(5) . . . . ?
P1 Ru1 C14 C15 -149.7(3) . . . . ?
P2 Ru1 C14 C15 30.4(4) . . . . ?
Cl1 Ru1 C14 C15 120.7(4) . . . . ?
C13 C14 C15 C16 -1.1(6) . . . . ?
Ru1 C14 C15 C16 60.6(4) . . . . ?
C13 C14 C15 Ru1 -61.7(4) . . . . ?
C17 Ru1 C15 C14 79.0(4) . . . . ?
C16 Ru1 C15 C14 117.4(5) . . . . ?
C13 Ru1 C15 C14 36.2(4) . . . . ?
P1 Ru1 C15 C14 70.4(6) . . . . ?
P2 Ru1 C15 C14 -157.1(3) . . . . ?
Cl1 Ru1 C15 C14 -67.2(4) . . . . ?
C17 Ru1 C15 C16 -38.4(3) . . . . ?
C13 Ru1 C15 C16 -81.2(4) . . . . ?
C14 Ru1 C15 C16 -117.4(5) . . . . ?
P1 Ru1 C15 C16 -47.0(6) . . . . ?
P2 Ru1 C15 C16 85.5(4) . . . . ?
Cl1 Ru1 C15 C16 175.4(3) . . . . ?
C14 C15 C16 C17 -0.1(7) . . . . ?
Ru1 C15 C16 C17 62.3(4) . . . . ?
C14 C15 C16 Ru1 -62.4(4) . . . . ?
C15 Ru1 C16 C17 -116.2(5) . . . . ?
C13 Ru1 C16 C17 -38.3(4) . . . . ?
C14 Ru1 C16 C17 -79.5(4) . . . . ?
P1 Ru1 C16 C17 42.9(4) . . . . ?
P2 Ru1 C16 C17 145.7(3) . . . . ?
Cl1 Ru1 C16 C17 -124.7(4) . . . . ?
C17 Ru1 C16 C15 116.2(5) . . . . ?
C13 Ru1 C16 C15 77.9(4) . . . . ?
C14 Ru1 C16 C15 36.7(4) . . . . ?
P1 Ru1 C16 C15 159.1(3) . . . . ?
P2 Ru1 C16 C15 -98.1(3) . . . . ?
Cl1 Ru1 C16 C15 -8.5(6) . . . . ?
C15 C16 C17 C13 1.2(7) . . . . ?
Ru1 C16 C17 C13 65.2(4) . . . . ?
C15 C16 C17 Ru1 -64.0(4) . . . . ?
C14 C13 C17 C16 -1.9(7) . . . . ?
Ru1 C13 C17 C16 -63.9(4) . . . . ?
C14 C13 C17 Ru1 62.0(4) . . . . ?
C15 Ru1 C17 C16 38.1(4) . . . . ?
C13 Ru1 C17 C16 115.8(5) . . . . ?
C14 Ru1 C17 C16 79.5(4) . . . . ?
P1 Ru1 C17 C16 -145.4(3) . . . . ?
P2 Ru1 C17 C16 -42.4(4) . . . . ?
Cl1 Ru1 C17 C16 125.6(4) . . . . ?
C16 Ru1 C17 C13 -115.8(5) . . . . ?
C15 Ru1 C17 C13 -77.7(4) . . . . ?
C14 Ru1 C17 C13 -36.3(3) . . . . ?
P1 Ru1 C17 C13 98.8(3) . . . . ?
P2 Ru1 C17 C13 -158.3(3) . . . . ?
Cl1 Ru1 C17 C13 9.8(6) . . . . ?
|
1100803.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 07:38:26 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180560 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100803.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100803
loop_
_publ_author_name
'Vicente, Jos\'e'
'Arcas, Aurelia'
'Fern\'andez-Hern\'andez, Jes\'us M.'
'Bautista, Delia'
'Jones, Peter G.'
_publ_section_title
;
Reactivity of [Pd{CH~2~C(O)Me}Cl]~n~ toward Isocyanides
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2516
_journal_page_last 2527
_journal_paper_doi 10.1021/om048999c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C13 H23 Cl N2 O Pd'
_chemical_formula_weight 365.18
_space_group_IT_number 29
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2ac'
_symmetry_space_group_name_H-M 'P c a 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 18.2636(11)
_cell_length_b 9.3501(4)
_cell_length_c 9.2895(4)
_cell_measurement_reflns_used 7094
_cell_measurement_temperature 133(2)
_cell_measurement_theta_max 30.47
_cell_measurement_theta_min 2.45
_cell_volume 1586.34(14)
_computing_cell_refinement 'Bruker Saint'
_computing_data_collection 'Bruker Smart'
_computing_data_reduction 'Bruker Saint'
_computing_molecular_graphics 'Siemens XP'
_computing_publication_material Shelxl-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker smart 1000 CCD'
_diffrn_measurement_method '\w- & \f-scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0289
_diffrn_reflns_av_sigmaI/netI 0.0163
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 31977
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.03
_diffrn_reflns_theta_min 2.18
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.330
_exptl_absorpt_correction_T_max 0.8799
_exptl_absorpt_correction_T_min 0.6419
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details XPREP
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.529
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description tablet
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.387
_refine_diff_density_min -0.201
_refine_diff_density_rms 0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.020(16)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment
;
NH free with DFIX, methyls rigid, others riding
;
_refine_ls_matrix_type full
_refine_ls_number_parameters 174
_refine_ls_number_reflns 4637
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0166
_refine_ls_R_factor_gt 0.0152
_refine_ls_shift/su_max 0.077
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0381
_refine_ls_wR_factor_ref 0.0386
_reflns_number_gt 4447
_reflns_number_total 4637
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om048999csi20041220_105555.cif
_cod_data_source_block traidos
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Pca21
_cod_database_code 1100803
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.894076(4) 0.618848(8) 0.74628(2) 0.01817(3) Uani 1 1 d . . .
Cl Cl 0.94570(2) 0.71392(4) 0.96038(4) 0.02777(7) Uani 1 1 d . . .
O O 0.83158(6) 0.79624(10) 0.71227(11) 0.0248(2) Uani 1 1 d . . .
C1 C 0.84585(8) 0.55467(15) 0.56498(15) 0.0207(3) Uani 1 1 d . . .
C2 C 0.79308(8) 0.65563(16) 0.51966(18) 0.0242(3) Uani 1 1 d . . .
H2 H 0.7625 0.6402 0.4385 0.029 Uiso 1 1 calc R . .
C3 C 0.78927(8) 0.77854(15) 0.60211(17) 0.0239(3) Uani 1 1 d . . .
N1 N 0.86133(7) 0.43315(14) 0.49802(13) 0.0221(2) Uani 1 1 d D . .
H01 H 0.9010(10) 0.395(3) 0.521(4) 0.061(10) Uiso 1 1 d D . .
N2 N 0.95833(7) 0.32290(13) 0.80924(14) 0.0222(2) Uani 1 1 d . . .
C4 C 0.73723(10) 0.89860(17) 0.5688(2) 0.0342(4) Uani 1 1 d . . .
H4A H 0.7082 0.9209 0.6547 0.041 Uiso 1 1 calc R . .
H4B H 0.7045 0.8698 0.4904 0.041 Uiso 1 1 calc R . .
H4C H 0.7650 0.9834 0.5397 0.041 Uiso 1 1 calc R . .
C5 C 0.83110(8) 0.37294(15) 0.36133(16) 0.0220(3) Uani 1 1 d . . .
C6 C 0.86537(9) 0.22455(17) 0.34627(18) 0.0275(3) Uani 1 1 d . . .
H6A H 0.9187 0.2338 0.3392 0.033 Uiso 1 1 calc R . .
H6B H 0.8465 0.1782 0.2593 0.033 Uiso 1 1 calc R . .
H6C H 0.8529 0.1666 0.4307 0.033 Uiso 1 1 calc R . .
C7 C 0.74815(9) 0.35358(18) 0.3726(2) 0.0310(3) Uani 1 1 d . . .
H7A H 0.7366 0.2964 0.4580 0.037 Uiso 1 1 calc R . .
H7B H 0.7301 0.3045 0.2864 0.037 Uiso 1 1 calc R . .
H7C H 0.7246 0.4475 0.3806 0.037 Uiso 1 1 calc R . .
C8 C 0.85330(8) 0.46777(17) 0.2358(2) 0.0328(3) Uani 1 1 d . . .
H8A H 0.8336 0.5642 0.2503 0.039 Uiso 1 1 calc R . .
H8B H 0.8338 0.4279 0.1461 0.039 Uiso 1 1 calc R . .
H8C H 0.9068 0.4723 0.2301 0.039 Uiso 1 1 calc R . .
C9 C 0.93967(7) 0.43716(16) 0.78196(14) 0.0213(3) Uani 1 1 d . . .
C10 C 0.97263(8) 0.17277(15) 0.84504(16) 0.0225(3) Uani 1 1 d . . .
C11 C 1.05497(9) 0.14802(19) 0.8375(2) 0.0322(3) Uani 1 1 d . . .
H11A H 1.0724 0.1687 0.7399 0.039 Uiso 1 1 calc R . .
H11B H 1.0658 0.0482 0.8615 0.039 Uiso 1 1 calc R . .
H11C H 1.0797 0.2112 0.9061 0.039 Uiso 1 1 calc R . .
C12 C 0.94246(12) 0.1488(2) 0.9961(2) 0.0396(4) Uani 1 1 d . . .
H12A H 0.9680 0.2114 1.0641 0.048 Uiso 1 1 calc R . .
H12B H 0.9499 0.0487 1.0239 0.048 Uiso 1 1 calc R . .
H12C H 0.8900 0.1707 0.9973 0.048 Uiso 1 1 calc R . .
C13 C 0.93160(9) 0.08318(16) 0.7352(3) 0.0328(3) Uani 1 1 d . . .
H13A H 0.8792 0.1052 0.7403 0.039 Uiso 1 1 calc R . .
H13B H 0.9392 -0.0185 0.7559 0.039 Uiso 1 1 calc R . .
H13C H 0.9499 0.1050 0.6385 0.039 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.01994(4) 0.01501(4) 0.01957(5) -0.00072(6) -0.00061(6) -0.00074(3)
Cl 0.03078(16) 0.02726(17) 0.02527(16) -0.00669(14) -0.00447(15) -0.00052(14)
O 0.0253(5) 0.0168(4) 0.0323(6) -0.0022(4) -0.0029(4) 0.0019(4)
C1 0.0210(6) 0.0192(6) 0.0218(6) 0.0014(5) 0.0015(5) -0.0024(5)
C2 0.0221(6) 0.0231(7) 0.0275(7) -0.0004(6) -0.0036(6) 0.0000(5)
C3 0.0202(6) 0.0207(6) 0.0308(8) 0.0032(6) 0.0013(6) -0.0009(5)
N1 0.0245(6) 0.0213(6) 0.0204(6) -0.0022(5) -0.0056(5) 0.0023(5)
N2 0.0242(6) 0.0213(6) 0.0211(5) -0.0002(5) -0.0018(5) 0.0005(5)
C4 0.0287(8) 0.0253(8) 0.0487(11) -0.0021(7) -0.0053(8) 0.0068(6)
C5 0.0218(6) 0.0250(7) 0.0192(7) -0.0039(5) -0.0035(5) -0.0002(5)
C6 0.0285(8) 0.0273(8) 0.0266(7) -0.0073(6) -0.0009(6) 0.0016(6)
C7 0.0236(7) 0.0333(8) 0.0359(9) -0.0088(7) -0.0016(6) -0.0025(6)
C8 0.0387(8) 0.0356(7) 0.0240(8) 0.0037(9) -0.0033(8) -0.0054(6)
C9 0.0215(6) 0.0235(7) 0.0188(7) -0.0026(5) -0.0012(5) -0.0015(5)
C10 0.0265(7) 0.0174(6) 0.0236(7) 0.0020(5) -0.0005(6) 0.0033(5)
C11 0.0257(7) 0.0320(8) 0.0388(9) 0.0038(7) -0.0040(7) 0.0067(6)
C12 0.0497(11) 0.0404(10) 0.0287(9) 0.0113(7) 0.0094(8) 0.0142(8)
C13 0.0346(7) 0.0219(6) 0.0418(10) -0.0044(9) -0.0071(9) -0.0041(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.1900
0.00 -1.00 0.00 0.0420
0.00 1.00 0.00 0.0560
1.00 0.00 0.00 0.1880
-1.00 0.00 0.00 0.1550
-2.00 0.00 -1.00 0.1720
3.00 0.00 -2.00 0.1950
2.00 -1.00 3.00 0.1530
-1.00 0.00 1.00 0.2340
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Pd C1 94.08(6) . . ?
C9 Pd O 171.63(5) . . ?
C1 Pd O 82.33(5) . . ?
C9 Pd Cl 90.83(4) . . ?
C1 Pd Cl 175.05(4) . . ?
O Pd Cl 92.72(3) . . ?
C3 O Pd 110.68(9) . . ?
N1 C1 C2 125.32(14) . . ?
N1 C1 Pd 124.07(11) . . ?
C2 C1 Pd 110.61(10) . . ?
C3 C2 C1 115.12(14) . . ?
O C3 C2 120.98(13) . . ?
O C3 C4 116.44(14) . . ?
C2 C3 C4 122.58(15) . . ?
C1 N1 C5 129.98(12) . . ?
C9 N2 C10 173.02(14) . . ?
N1 C5 C8 109.48(12) . . ?
N1 C5 C6 105.57(12) . . ?
C8 C5 C6 110.49(13) . . ?
N1 C5 C7 110.63(13) . . ?
C8 C5 C7 112.69(13) . . ?
C6 C5 C7 107.73(12) . . ?
N2 C9 Pd 171.28(12) . . ?
N2 C10 C13 106.73(12) . . ?
N2 C10 C11 108.11(12) . . ?
C13 C10 C11 111.86(13) . . ?
N2 C10 C12 106.59(13) . . ?
C13 C10 C12 111.05(15) . . ?
C11 C10 C12 112.16(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C9 1.9207(15) . ?
Pd C1 1.9931(14) . ?
Pd O 2.0380(10) . ?
Pd Cl 2.3738(4) . ?
O C3 1.2929(18) . ?
C1 N1 1.3258(19) . ?
C1 C2 1.413(2) . ?
C2 C3 1.383(2) . ?
C3 C4 1.503(2) . ?
N1 C5 1.4948(19) . ?
N2 C9 1.150(2) . ?
N2 C10 1.4661(18) . ?
C5 C8 1.520(3) . ?
C5 C6 1.528(2) . ?
C5 C7 1.529(2) . ?
C10 C13 1.518(2) . ?
C10 C11 1.523(2) . ?
C10 C12 1.524(2) . ?
|
1100804.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 07:38:26 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180560 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100804.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100804
loop_
_publ_author_name
'Vicente, Jos\'e'
'Arcas, Aurelia'
'Fern\'andez-Hern\'andez, Jes\'us M.'
'Bautista, Delia'
'Jones, Peter G.'
_publ_section_title
;
Reactivity of [Pd{CH~2~C(O)Me}Cl]~n~ toward Isocyanides
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2516
_journal_page_last 2527
_journal_paper_doi 10.1021/om048999c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C32 H33 Cl3 F3 N3 O4 Pd S'
_chemical_formula_weight 825.42
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary Patterson
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 83.546(5)
_cell_angle_beta 87.742(5)
_cell_angle_gamma 70.234(4)
_cell_formula_units_Z 2
_cell_length_a 8.6505(5)
_cell_length_b 11.8001(5)
_cell_length_c 18.7442(14)
_cell_measurement_reflns_used 85
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 12.4
_cell_measurement_theta_min 5.3
_cell_volume 1789.20(19)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens XSCANS'
_computing_molecular_graphics 'Bruker ShelxTL'
_computing_publication_material 'Bruker ShelxTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0181
_diffrn_reflns_av_sigmaI/netI 0.0287
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 6735
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 3.01
_diffrn_standards_decay_% 0.7
_diffrn_standards_interval_count 247
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.856
_exptl_absorpt_correction_T_max 0.910
_exptl_absorpt_correction_T_min 0.743
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.532
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 836
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.17
_refine_diff_density_max 0.693
_refine_diff_density_min -0.554
_refine_diff_density_rms 0.060
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment
'ordered methyls rigid,hydrogens at C3 free, others riding'
_refine_ls_matrix_type full
_refine_ls_number_parameters 455
_refine_ls_number_reflns 6278
_refine_ls_number_restraints 39
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0361
_refine_ls_R_factor_gt 0.0290
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.6583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0684
_refine_ls_wR_factor_ref 0.0705
_reflns_number_gt 5432
_reflns_number_total 6278
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om048999csi20041220_105555.cif
_cod_data_source_block jm300
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_database_code 1100804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.64574(2) 0.908779(17) 0.689302(10) 0.02155(7) Uani 1 1 d . . .
O1 O 0.6859(3) 0.75021(18) 0.51907(11) 0.0419(5) Uani 1 1 d . . .
N1 N 0.6976(3) 0.9102(2) 0.85565(12) 0.0292(5) Uani 1 1 d . . .
N2 N 0.5565(3) 1.18920(19) 0.66640(11) 0.0271(5) Uani 1 1 d . . .
N3 N 0.8073(3) 0.62751(19) 0.69476(11) 0.0253(5) Uani 1 1 d . . .
C1 C 0.5728(3) 0.9214(2) 0.58288(13) 0.0318(6) Uani 1 1 d . . .
H1A H 0.4715 0.9001 0.5826 0.038 Uiso 1 1 calc R . .
H1B H 0.5453 1.0066 0.5617 0.038 Uiso 1 1 calc R . .
C2 C 0.6966(3) 0.8433(2) 0.53701(13) 0.0301(6) Uani 1 1 d . . .
C3 C 0.8376(5) 0.8852(4) 0.51182(19) 0.0442(8) Uani 1 1 d D . .
H3A H 0.911(10) 0.809(4) 0.516(6) 0.09(4) Uiso 0.54(8) 1 d PD A 1
H3B H 0.811(7) 0.920(5) 0.4663(17) 0.03(2) Uiso 0.54(8) 1 d PD A 1
H3C H 0.881(12) 0.925(9) 0.540(4) 0.08(3) Uiso 0.54(8) 1 d PD A 1
H3A' H 0.924(7) 0.857(9) 0.543(3) 0.04(3) Uiso 0.46(8) 1 d PD A 2
H3B' H 0.899(8) 0.843(7) 0.477(3) 0.04(2) Uiso 0.46(8) 1 d PD A 2
H3C' H 0.822(8) 0.966(2) 0.510(4) 0.02(2) Uiso 0.46(8) 1 d PD A 2
C4 C 0.6882(3) 0.9059(2) 0.79515(14) 0.0272(6) Uani 1 1 d . . .
C5 C 0.5826(3) 1.0868(2) 0.67577(13) 0.0268(6) Uani 1 1 d . . .
C6 C 0.7393(3) 0.7304(2) 0.69186(13) 0.0251(6) Uani 1 1 d . . .
C11 C 0.7092(4) 0.9137(3) 0.93002(14) 0.0328(6) Uani 1 1 d D . .
C12 C 0.6611(4) 0.8303(3) 0.97616(15) 0.0405(7) Uani 1 1 d D . .
C13 C 0.6762(4) 0.8354(3) 1.04894(16) 0.0531(9) Uani 1 1 d D . .
H13 H 0.6454 0.7804 1.0826 0.064 Uiso 1 1 calc R . .
C14 C 0.7356(4) 0.9194(4) 1.07366(17) 0.0544(9) Uani 1 1 d D . .
H14 H 0.7459 0.9208 1.1238 0.065 Uiso 1 1 calc R . .
C15 C 0.7796(4) 1.0009(3) 1.02588(16) 0.0465(8) Uani 1 1 d D . .
H15 H 0.8194 1.0581 1.0436 0.056 Uiso 1 1 calc R . .
C16 C 0.7670(4) 1.0009(3) 0.95240(15) 0.0366(7) Uani 1 1 d D . .
C17 C 0.8085(4) 1.0910(3) 0.89907(17) 0.0440(8) Uani 1 1 d . . .
H17A H 0.8514 1.1423 0.9244 0.053 Uiso 1 1 calc R . .
H17B H 0.7095 1.1415 0.8724 0.053 Uiso 1 1 calc R . .
H17C H 0.8919 1.0480 0.8655 0.053 Uiso 1 1 calc R . .
C18 C 0.5957(5) 0.7411(3) 0.94832(18) 0.0536(9) Uani 1 1 d . . .
H18A H 0.6873 0.6733 0.9326 0.064 Uiso 1 1 calc R . .
H18B H 0.5223 0.7809 0.9077 0.064 Uiso 1 1 calc R . .
H18C H 0.5347 0.7107 0.9865 0.064 Uiso 1 1 calc R . .
C21 C 0.5283(3) 1.3146(2) 0.65580(13) 0.0260(6) Uani 1 1 d D . .
C22 C 0.4339(3) 1.3860(2) 0.70653(14) 0.0310(6) Uani 1 1 d D . .
C23 C 0.4091(4) 1.5096(2) 0.69499(15) 0.0359(7) Uani 1 1 d D . .
H23 H 0.3433 1.5624 0.7275 0.043 Uiso 1 1 calc R . .
C24 C 0.4795(4) 1.5560(2) 0.63645(16) 0.0375(7) Uani 1 1 d D . .
H24 H 0.4629 1.6403 0.6297 0.045 Uiso 1 1 calc R . .
C25 C 0.5735(4) 1.4819(2) 0.58761(15) 0.0344(7) Uani 1 1 d D . .
H25 H 0.6212 1.5159 0.5480 0.041 Uiso 1 1 calc R . .
C26 C 0.5997(3) 1.3583(2) 0.59541(14) 0.0287(6) Uani 1 1 d D . .
C27 C 0.3670(4) 1.3317(3) 0.77148(16) 0.0442(8) Uani 1 1 d . . .
H27A H 0.3217 1.2718 0.7573 0.053 Uiso 1 1 calc R . .
H27B H 0.2801 1.3957 0.7932 0.053 Uiso 1 1 calc R . .
H27C H 0.4554 1.2922 0.8064 0.053 Uiso 1 1 calc R . .
C28 C 0.6993(4) 1.2743(3) 0.54332(16) 0.0410(7) Uani 1 1 d . . .
H28A H 0.7484 1.3190 0.5074 0.049 Uiso 1 1 calc R . .
H28B H 0.6281 1.2411 0.5193 0.049 Uiso 1 1 calc R . .
H28C H 0.7865 1.2080 0.5692 0.049 Uiso 1 1 calc R . .
C31 C 0.8889(3) 0.5022(2) 0.69463(14) 0.0292(6) Uani 1 1 d D . .
C32 C 0.8489(4) 0.4252(3) 0.74904(16) 0.0376(7) Uani 1 1 d D . .
C33 C 0.9278(5) 0.3009(3) 0.7448(2) 0.0560(10) Uani 1 1 d D . .
H33 H 0.9052 0.2440 0.7800 0.067 Uiso 1 1 calc R . .
C34 C 1.0379(5) 0.2599(3) 0.6902(2) 0.0571(10) Uani 1 1 d D . .
H34 H 1.0881 0.1753 0.6880 0.068 Uiso 1 1 calc R . .
C35 C 1.0760(4) 0.3390(3) 0.6393(2) 0.0488(8) Uani 1 1 d D . .
H35 H 1.1537 0.3085 0.6029 0.059 Uiso 1 1 calc R . .
C36 C 1.0024(4) 0.4631(2) 0.64015(16) 0.0343(6) Uani 1 1 d D . .
C37 C 0.7310(4) 0.4727(3) 0.80761(17) 0.0475(8) Uani 1 1 d . . .
H37A H 0.7867 0.4987 0.8439 0.057 Uiso 1 1 calc R . .
H37B H 0.6905 0.4089 0.8298 0.057 Uiso 1 1 calc R . .
H37C H 0.6385 0.5419 0.7876 0.057 Uiso 1 1 calc R . .
C38 C 1.0455(4) 0.5507(3) 0.58539(16) 0.0404(7) Uani 1 1 d . . .
H38A H 1.1363 0.5062 0.5554 0.049 Uiso 1 1 calc R . .
H38B H 1.0787 0.6079 0.6099 0.049 Uiso 1 1 calc R . .
H38C H 0.9497 0.5951 0.5551 0.049 Uiso 1 1 calc R . .
S S 0.25070(9) 0.87868(6) 0.76549(4) 0.02947(15) Uani 1 1 d . . .
C99 C 0.1227(4) 0.8781(3) 0.69072(16) 0.0375(7) Uani 1 1 d . . .
F1 F 0.2053(3) 0.8675(2) 0.62904(10) 0.0644(6) Uani 1 1 d . . .
F2 F -0.0072(2) 0.97890(17) 0.68221(13) 0.0624(6) Uani 1 1 d . . .
F3 F 0.0661(2) 0.78549(16) 0.70069(10) 0.0493(5) Uani 1 1 d . . .
O2 O 0.2974(3) 0.98350(17) 0.74548(12) 0.0421(5) Uani 1 1 d . . .
O3 O 0.3809(3) 0.76457(17) 0.76560(12) 0.0458(5) Uani 1 1 d . . .
O4 O 0.1408(3) 0.8881(2) 0.82572(11) 0.0503(6) Uani 1 1 d . . .
C90 C 0.1714(4) 0.6404(3) 0.91241(17) 0.0457(8) Uani 1 1 d . . .
H90 H 0.1771 0.7190 0.8885 0.055 Uiso 1 1 calc R . .
Cl1 Cl 0.37043(13) 0.53571(9) 0.91684(6) 0.0686(3) Uani 1 1 d . . .
Cl2 Cl 0.04443(12) 0.59402(10) 0.86074(6) 0.0701(3) Uani 1 1 d . . .
Cl3 Cl 0.09008(19) 0.66470(13) 0.99809(6) 0.0979(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.02698(11) 0.01841(10) 0.01852(10) 0.00002(7) -0.00042(7) -0.00722(8)
O1 0.0536(14) 0.0372(12) 0.0359(11) -0.0113(9) -0.0044(10) -0.0138(10)
N1 0.0373(14) 0.0296(12) 0.0227(12) -0.0040(9) -0.0009(10) -0.0133(10)
N2 0.0318(13) 0.0213(12) 0.0262(11) 0.0000(9) -0.0008(9) -0.0070(10)
N3 0.0324(13) 0.0222(12) 0.0229(11) -0.0004(8) -0.0053(9) -0.0115(10)
C1 0.0339(16) 0.0349(15) 0.0218(13) -0.0019(11) -0.0081(11) -0.0050(12)
C2 0.0341(16) 0.0344(15) 0.0180(13) 0.0039(11) -0.0078(11) -0.0077(12)
C3 0.044(2) 0.054(2) 0.0359(19) -0.0034(16) 0.0055(16) -0.0192(18)
C4 0.0325(15) 0.0207(13) 0.0293(15) -0.0009(10) -0.0003(11) -0.0107(11)
C5 0.0281(14) 0.0281(15) 0.0222(13) -0.0011(10) 0.0017(11) -0.0075(11)
C6 0.0313(15) 0.0299(15) 0.0166(12) -0.0003(10) -0.0038(10) -0.0138(12)
C11 0.0385(17) 0.0426(16) 0.0198(13) -0.0090(11) 0.0011(12) -0.0154(14)
C12 0.0476(19) 0.0515(19) 0.0283(15) -0.0032(13) 0.0010(13) -0.0246(16)
C13 0.059(2) 0.080(3) 0.0245(16) 0.0004(16) 0.0054(15) -0.031(2)
C14 0.056(2) 0.090(3) 0.0230(15) -0.0185(16) 0.0015(15) -0.028(2)
C15 0.0452(19) 0.065(2) 0.0369(17) -0.0258(16) 0.0029(14) -0.0224(17)
C16 0.0342(16) 0.0464(17) 0.0332(15) -0.0147(13) 0.0028(12) -0.0159(14)
C17 0.0469(19) 0.0428(18) 0.0502(19) -0.0132(14) 0.0034(15) -0.0230(15)
C18 0.077(3) 0.058(2) 0.0393(18) 0.0014(15) -0.0004(17) -0.041(2)
C21 0.0291(14) 0.0181(12) 0.0293(14) -0.0016(10) -0.0069(11) -0.0056(11)
C22 0.0330(15) 0.0300(14) 0.0276(14) -0.0036(11) -0.0048(12) -0.0070(12)
C23 0.0403(17) 0.0272(14) 0.0361(16) -0.0081(12) -0.0111(13) -0.0033(13)
C24 0.0476(18) 0.0209(13) 0.0447(17) 0.0002(12) -0.0199(14) -0.0113(13)
C25 0.0383(17) 0.0323(15) 0.0353(16) 0.0067(12) -0.0109(13) -0.0173(13)
C26 0.0300(15) 0.0282(14) 0.0277(14) 0.0011(11) -0.0059(11) -0.0098(12)
C27 0.052(2) 0.0425(18) 0.0345(16) -0.0078(13) 0.0078(14) -0.0104(15)
C28 0.0447(19) 0.0402(17) 0.0351(16) -0.0005(13) 0.0074(14) -0.0121(14)
C31 0.0333(15) 0.0164(12) 0.0387(15) -0.0012(11) -0.0137(12) -0.0084(11)
C32 0.0403(17) 0.0317(15) 0.0451(18) 0.0048(13) -0.0146(14) -0.0186(13)
C33 0.061(2) 0.0305(17) 0.079(3) 0.0176(17) -0.024(2) -0.0244(17)
C34 0.054(2) 0.0216(15) 0.092(3) -0.0083(17) -0.013(2) -0.0059(15)
C35 0.045(2) 0.0298(16) 0.070(2) -0.0162(16) -0.0085(17) -0.0064(14)
C36 0.0345(16) 0.0272(14) 0.0411(16) -0.0082(12) -0.0107(13) -0.0076(12)
C37 0.054(2) 0.054(2) 0.0413(18) 0.0140(15) -0.0148(16) -0.0318(17)
C38 0.0409(18) 0.0411(17) 0.0361(16) -0.0078(13) 0.0003(13) -0.0085(14)
S 0.0326(4) 0.0237(3) 0.0318(4) -0.0037(3) -0.0025(3) -0.0087(3)
C99 0.0330(17) 0.0396(17) 0.0410(17) 0.0005(13) -0.0034(13) -0.0147(14)
F1 0.0678(14) 0.1025(17) 0.0322(10) -0.0035(10) -0.0025(9) -0.0417(13)
F2 0.0414(11) 0.0409(11) 0.0996(17) 0.0086(10) -0.0304(11) -0.0086(9)
F3 0.0483(11) 0.0439(10) 0.0659(12) -0.0110(9) -0.0061(9) -0.0265(9)
O2 0.0385(12) 0.0315(11) 0.0598(14) -0.0009(9) -0.0058(10) -0.0168(9)
O3 0.0434(13) 0.0298(11) 0.0572(14) -0.0076(10) -0.0143(11) -0.0006(10)
O4 0.0669(16) 0.0517(14) 0.0397(12) -0.0159(10) 0.0153(11) -0.0279(12)
C90 0.060(2) 0.0372(17) 0.0417(18) -0.0015(14) -0.0098(16) -0.0184(16)
Cl1 0.0562(6) 0.0643(6) 0.0832(7) -0.0006(5) -0.0217(5) -0.0174(5)
Cl2 0.0547(6) 0.0912(8) 0.0734(7) -0.0280(6) -0.0099(5) -0.0289(5)
Cl3 0.1280(11) 0.1098(10) 0.0542(6) -0.0354(6) 0.0115(7) -0.0307(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 Pd C6 170.53(11) . . ?
C5 Pd C4 91.20(10) . . ?
C6 Pd C4 93.05(10) . . ?
C5 Pd C1 86.36(11) . . ?
C6 Pd C1 90.30(10) . . ?
C4 Pd C1 173.28(11) . . ?
C4 N1 C11 179.2(3) . . ?
C5 N2 C21 178.5(3) . . ?
C6 N3 C31 177.1(2) . . ?
C2 C1 Pd 114.57(18) . . ?
O1 C2 C1 122.4(3) . . ?
O1 C2 C3 120.9(3) . . ?
C1 C2 C3 116.7(3) . . ?
N1 C4 Pd 173.8(2) . . ?
N2 C5 Pd 175.4(2) . . ?
N3 C6 Pd 173.7(2) . . ?
C12 C11 C16 124.6(3) . . ?
C12 C11 N1 117.8(2) . . ?
C16 C11 N1 117.6(2) . . ?
C13 C12 C11 116.1(3) . . ?
C13 C12 C18 122.1(3) . . ?
C11 C12 C18 121.7(3) . . ?
C12 C13 C14 121.3(3) . . ?
C15 C14 C13 120.4(3) . . ?
C14 C15 C16 121.3(3) . . ?
C15 C16 C11 116.3(3) . . ?
C15 C16 C17 122.6(3) . . ?
C11 C16 C17 121.1(3) . . ?
C22 C21 C26 124.6(2) . . ?
C22 C21 N2 117.9(2) . . ?
C26 C21 N2 117.5(2) . . ?
C21 C22 C23 116.6(3) . . ?
C21 C22 C27 121.5(2) . . ?
C23 C22 C27 121.9(3) . . ?
C24 C23 C22 120.5(3) . . ?
C25 C24 C23 121.1(3) . . ?
C24 C25 C26 121.1(3) . . ?
C25 C26 C21 116.1(2) . . ?
C25 C26 C28 123.0(3) . . ?
C21 C26 C28 120.9(2) . . ?
C36 C31 C32 124.5(2) . . ?
C36 C31 N3 117.9(2) . . ?
C32 C31 N3 117.6(3) . . ?
C31 C32 C33 115.5(3) . . ?
C31 C32 C37 122.0(3) . . ?
C33 C32 C37 122.5(3) . . ?
C34 C33 C32 121.0(3) . . ?
C35 C34 C33 121.3(3) . . ?
C34 C35 C36 120.8(3) . . ?
C35 C36 C31 116.9(3) . . ?
C35 C36 C38 121.3(3) . . ?
C31 C36 C38 121.8(2) . . ?
O3 S O2 115.45(14) . . ?
O3 S O4 114.79(14) . . ?
O2 S O4 114.94(13) . . ?
O3 S C99 103.03(13) . . ?
O2 S C99 103.17(13) . . ?
O4 S C99 102.93(14) . . ?
F1 C99 F2 107.7(3) . . ?
F1 C99 F3 106.6(2) . . ?
F2 C99 F3 107.1(2) . . ?
F1 C99 S 112.0(2) . . ?
F2 C99 S 111.7(2) . . ?
F3 C99 S 111.5(2) . . ?
Cl3 C90 Cl1 110.90(18) . . ?
Cl3 C90 Cl2 111.0(2) . . ?
Cl1 C90 Cl2 111.07(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C5 1.972(3) . ?
Pd C6 1.979(3) . ?
Pd C4 2.027(3) . ?
Pd C1 2.090(2) . ?
O1 C2 1.218(3) . ?
N1 C4 1.148(3) . ?
N1 C11 1.408(3) . ?
N2 C5 1.146(3) . ?
N2 C21 1.408(3) . ?
N3 C6 1.152(3) . ?
N3 C31 1.407(3) . ?
C1 C2 1.475(4) . ?
C2 C3 1.505(4) . ?
C11 C12 1.395(4) . ?
C11 C16 1.396(4) . ?
C12 C13 1.386(4) . ?
C12 C18 1.500(4) . ?
C13 C14 1.388(5) . ?
C14 C15 1.378(5) . ?
C15 C16 1.386(4) . ?
C16 C17 1.500(4) . ?
C21 C22 1.391(4) . ?
C21 C26 1.399(4) . ?
C22 C23 1.393(4) . ?
C22 C27 1.499(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.380(4) . ?
C25 C26 1.389(4) . ?
C26 C28 1.501(4) . ?
C31 C36 1.393(4) . ?
C31 C32 1.400(4) . ?
C32 C33 1.403(4) . ?
C32 C37 1.491(5) . ?
C33 C34 1.383(5) . ?
C34 C35 1.368(5) . ?
C35 C36 1.387(4) . ?
C36 C38 1.501(4) . ?
S O3 1.434(2) . ?
S O2 1.434(2) . ?
S O4 1.436(2) . ?
S C99 1.822(3) . ?
C99 F1 1.330(4) . ?
C99 F2 1.331(3) . ?
C99 F3 1.333(3) . ?
C90 Cl3 1.742(3) . ?
C90 Cl1 1.746(4) . ?
C90 Cl2 1.747(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C37 H37A Cl2 0.98 2.86 3.680(3) 142.1 1_655
C17 H17C O4 0.98 2.49 3.415(4) 157.3 1_655
C34 H34 O2 0.95 2.53 3.350(4) 144.8 1_645
|
1100805.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100805.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100805
loop_
_publ_author_name
'Ionescu, Emanuel'
'von Frantzius, Gerd'
'Jones, Peter G.'
'Streubel, Rainer'
_publ_section_title
;
Photochemical and Thermal Reactions of a 2H-Azaphosphirene Complex
with Isonitriles
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2237
_journal_page_last 2240
_journal_paper_doi 10.1021/om049014u
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C13 H20 N O5 P Si2 W'
_chemical_formula_weight 541.30
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 73.219(3)
_cell_angle_beta 89.975(3)
_cell_angle_gamma 81.823(3)
_cell_formula_units_Z 2
_cell_length_a 6.9618(4)
_cell_length_b 9.6073(8)
_cell_length_c 16.1541(9)
_cell_measurement_reflns_used 7126
_cell_measurement_temperature 133(2)
_cell_measurement_theta_max 30.539
_cell_measurement_theta_min 2.242
_cell_volume 1022.98(12)
_computing_cell_refinement 'Bruker Saint'
_computing_data_collection 'Bruker Smart'
_computing_data_reduction 'Bruker Saint'
_computing_molecular_graphics 'Siemens XP'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker AXS Smart 1000CCD'
_diffrn_measurement_method '\w- & \f-scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0234
_diffrn_reflns_av_sigmaI/netI 0.0240
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 19997
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.03
_diffrn_reflns_theta_min 1.32
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.860
_exptl_absorpt_correction_T_max 0.9281
_exptl_absorpt_correction_T_min 0.7289
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details sadabs
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.757
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 524
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.946
_refine_diff_density_min -0.552
_refine_diff_density_rms 0.085
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.998
_refine_ls_hydrogen_treatment 'PH free, rigid methyls, others riding'
_refine_ls_matrix_type full
_refine_ls_number_parameters 218
_refine_ls_number_reflns 5954
_refine_ls_number_restraints 21
_refine_ls_restrained_S_all 0.997
_refine_ls_R_factor_all 0.0185
_refine_ls_R_factor_gt 0.0159
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0341
_refine_ls_wR_factor_ref 0.0346
_reflns_number_gt 5515
_reflns_number_total 5954
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060308
_cod_data_source_file om049014usi20050215_124817.cif
_cod_data_source_block ch
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_database_code 1100805
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.261181(10) 0.716083(8) 0.116808(5) 0.01703(2) Uani 1 1 d . . .
N N -0.1900(3) 0.4336(2) 0.24210(13) 0.0367(4) Uani 1 1 d . . .
P P 0.21119(6) 0.46014(5) 0.18983(3) 0.01652(9) Uani 1 1 d . . .
H0 H 0.208(3) 0.382(2) 0.1354(14) 0.025(6) Uiso 1 1 d . . .
Si1 Si 0.27506(8) 0.35607(6) 0.39420(3) 0.02167(10) Uani 1 1 d U . .
Si2 Si 0.41973(8) 0.14789(6) 0.27166(3) 0.02091(10) Uani 1 1 d U . .
O1 O 0.0283(2) 0.70023(19) -0.04908(10) 0.0380(4) Uani 1 1 d . . .
O2 O -0.1250(2) 0.83559(19) 0.19606(12) 0.0451(4) Uani 1 1 d . . .
O3 O 0.2884(2) 1.04673(17) 0.01445(12) 0.0412(4) Uani 1 1 d . . .
O4 O 0.6480(2) 0.59289(17) 0.03919(10) 0.0328(3) Uani 1 1 d . . .
O5 O 0.5215(2) 0.72042(18) 0.27815(10) 0.0349(3) Uani 1 1 d . . .
C1 C 0.1083(3) 0.7053(2) 0.01169(13) 0.0244(4) Uani 1 1 d . . .
C2 C 0.0128(3) 0.7923(2) 0.16746(14) 0.0271(4) Uani 1 1 d . . .
C3 C 0.2853(3) 0.9260(2) 0.05228(14) 0.0273(4) Uani 1 1 d . . .
C4 C 0.5099(3) 0.6370(2) 0.06706(12) 0.0221(4) Uani 1 1 d . . .
C5 C 0.4272(3) 0.7202(2) 0.21995(13) 0.0236(4) Uani 1 1 d . . .
C6 C 0.3553(2) 0.34070(19) 0.28357(11) 0.0174(3) Uani 1 1 d U . .
H6 H 0.4825 0.3789 0.2774 0.021 Uiso 1 1 calc R . .
C7 C 0.1395(3) 0.5418(2) 0.38876(14) 0.0310(4) Uani 1 1 d U . .
H7A H 0.0142 0.5562 0.3575 0.037 Uiso 1 1 calc R . .
H7B H 0.2157 0.6179 0.3584 0.037 Uiso 1 1 calc R . .
H7C H 0.1175 0.5483 0.4475 0.037 Uiso 1 1 calc R . .
C8 C 0.5040(3) 0.3274(3) 0.46181(14) 0.0328(5) Uani 1 1 d U . .
H8A H 0.4714 0.3325 0.5200 0.039 Uiso 1 1 calc R . .
H8B H 0.5828 0.4040 0.4351 0.039 Uiso 1 1 calc R . .
H8C H 0.5775 0.2307 0.4657 0.039 Uiso 1 1 calc R . .
C9 C 0.1132(3) 0.2172(2) 0.44494(14) 0.0307(4) Uani 1 1 d U . .
H9A H 0.1818 0.1181 0.4512 0.037 Uiso 1 1 calc R . .
H9B H -0.0047 0.2345 0.4081 0.037 Uiso 1 1 calc R . .
H9C H 0.0778 0.2265 0.5020 0.037 Uiso 1 1 calc R . .
C10 C 0.5860(3) 0.0301(2) 0.36344(14) 0.0320(5) Uani 1 1 d U . .
H10A H 0.6244 -0.0668 0.3549 0.038 Uiso 1 1 calc R . .
H10B H 0.5190 0.0190 0.4178 0.038 Uiso 1 1 calc R . .
H10C H 0.7018 0.0763 0.3658 0.038 Uiso 1 1 calc R . .
C11 C 0.1942(3) 0.0656(2) 0.26610(15) 0.0321(5) Uani 1 1 d U . .
H11A H 0.1051 0.1326 0.2201 0.039 Uiso 1 1 calc R . .
H11B H 0.1312 0.0498 0.3217 0.039 Uiso 1 1 calc R . .
H11C H 0.2279 -0.0286 0.2536 0.039 Uiso 1 1 calc R . .
C12 C 0.5538(3) 0.1627(3) 0.17020(14) 0.0342(5) Uani 1 1 d U . .
H12A H 0.6622 0.2175 0.1704 0.041 Uiso 1 1 calc R . .
H12B H 0.4656 0.2144 0.1201 0.041 Uiso 1 1 calc R . .
H12C H 0.6041 0.0640 0.1668 0.041 Uiso 1 1 calc R . .
C13 C -0.0360(3) 0.4402(2) 0.22160(13) 0.0235(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W 0.01575(4) 0.01504(4) 0.01936(4) -0.00395(3) 0.00147(2) -0.00150(2)
N 0.0265(10) 0.0383(11) 0.0426(12) -0.0068(9) -0.0004(8) -0.0061(8)
P 0.0159(2) 0.0161(2) 0.0177(2) -0.00515(17) 0.00028(15) -0.00250(17)
Si1 0.0244(3) 0.0239(3) 0.0178(3) -0.0074(2) 0.00223(18) -0.0045(2)
Si2 0.0241(3) 0.0172(2) 0.0201(3) -0.00514(19) -0.00080(18) 0.0010(2)
O1 0.0322(8) 0.0521(10) 0.0302(9) -0.0128(7) -0.0067(6) -0.0063(7)
O2 0.0320(9) 0.0371(10) 0.0631(12) -0.0138(9) 0.0178(8) 0.0038(7)
O3 0.0368(9) 0.0211(8) 0.0566(11) 0.0025(7) 0.0051(7) -0.0038(7)
O4 0.0272(8) 0.0378(9) 0.0299(8) -0.0083(7) 0.0064(6) 0.0036(6)
O5 0.0323(8) 0.0460(10) 0.0323(9) -0.0185(7) -0.0017(6) -0.0096(7)
C1 0.0202(9) 0.0243(10) 0.0268(10) -0.0049(8) 0.0033(7) -0.0026(7)
C2 0.0250(10) 0.0196(10) 0.0349(12) -0.0056(8) 0.0033(8) -0.0024(8)
C3 0.0216(9) 0.0256(11) 0.0331(11) -0.0069(8) 0.0015(7) -0.0009(8)
C4 0.0237(9) 0.0211(9) 0.0190(9) -0.0021(7) 0.0000(7) -0.0029(7)
C5 0.0237(9) 0.0220(10) 0.0274(10) -0.0105(8) 0.0069(7) -0.0042(7)
C6 0.0163(8) 0.0184(9) 0.0168(9) -0.0040(6) 0.0000(6) -0.0024(6)
C7 0.0384(12) 0.0295(11) 0.0285(11) -0.0142(9) 0.0097(8) -0.0042(9)
C8 0.0379(12) 0.0372(12) 0.0264(11) -0.0129(9) -0.0059(8) -0.0074(9)
C9 0.0336(11) 0.0331(12) 0.0245(11) -0.0059(9) 0.0069(8) -0.0074(9)
C10 0.0368(12) 0.0248(11) 0.0296(11) -0.0051(8) -0.0078(8) 0.0050(9)
C11 0.0366(12) 0.0234(11) 0.0397(13) -0.0141(9) -0.0020(9) -0.0051(9)
C12 0.0405(12) 0.0335(12) 0.0267(11) -0.0110(9) 0.0070(9) 0.0053(10)
C13 0.0227(9) 0.0196(9) 0.0264(10) -0.0034(7) -0.0038(7) -0.0042(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 W C1 88.37(8) . . ?
C3 W C5 92.40(8) . . ?
C1 W C5 176.79(7) . . ?
C3 W C2 88.45(8) . . ?
C1 W C2 91.28(8) . . ?
C5 W C2 91.86(8) . . ?
C3 W C4 92.28(8) . . ?
C1 W C4 88.83(7) . . ?
C5 W C4 88.03(7) . . ?
C2 W C4 179.26(8) . . ?
C3 W P 176.07(6) . . ?
C1 W P 88.08(6) . . ?
C5 W P 91.24(6) . . ?
C2 W P 89.97(6) . . ?
C4 W P 89.30(5) . . ?
C6 P C13 102.82(8) . . ?
C6 P W 123.84(6) . . ?
C13 P W 114.40(6) . . ?
C8 Si1 C7 107.94(10) . . ?
C8 Si1 C9 111.32(10) . . ?
C7 Si1 C9 107.19(10) . . ?
C8 Si1 C6 105.90(9) . . ?
C7 Si1 C6 112.79(9) . . ?
C9 Si1 C6 111.69(9) . . ?
C10 Si2 C12 107.43(10) . . ?
C10 Si2 C11 110.91(10) . . ?
C12 Si2 C11 110.08(11) . . ?
C10 Si2 C6 110.10(9) . . ?
C12 Si2 C6 108.03(9) . . ?
C11 Si2 C6 110.21(9) . . ?
O1 C1 W 177.51(17) . . ?
O2 C2 W 179.4(2) . . ?
O3 C3 W 176.26(18) . . ?
O4 C4 W 179.78(18) . . ?
O5 C5 W 179.02(17) . . ?
P C6 Si2 110.32(9) . . ?
P C6 Si1 116.77(9) . . ?
Si2 C6 Si1 117.34(9) . . ?
N C13 P 176.91(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C3 2.016(2) . ?
W C1 2.040(2) . ?
W C5 2.041(2) . ?
W C2 2.045(2) . ?
W C4 2.0491(19) . ?
W P 2.4753(5) . ?
N C13 1.127(3) . ?
P C6 1.8129(18) . ?
P C13 1.816(2) . ?
Si1 C8 1.874(2) . ?
Si1 C7 1.874(2) . ?
Si1 C9 1.875(2) . ?
Si1 C6 1.9121(18) . ?
Si2 C10 1.865(2) . ?
Si2 C12 1.865(2) . ?
Si2 C11 1.869(2) . ?
Si2 C6 1.9076(18) . ?
O1 C1 1.146(2) . ?
O2 C2 1.142(2) . ?
O3 C3 1.148(3) . ?
O4 C4 1.140(2) . ?
O5 C5 1.148(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
P H0 O1 1.32(2) 2.50(2) 3.6168(16) 140.4(13) 2_565
C12 H12C O2 0.98 2.61 3.507(3) 151.9 1_645
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 W P C6 -173.4(9) . . . . ?
C1 W P C6 161.68(9) . . . . ?
C5 W P C6 -15.18(9) . . . . ?
C2 W P C6 -107.04(9) . . . . ?
C4 W P C6 72.83(9) . . . . ?
C3 W P C13 -46.7(9) . . . . ?
C1 W P C13 -71.63(9) . . . . ?
C5 W P C13 111.51(9) . . . . ?
C2 W P C13 19.65(9) . . . . ?
C4 W P C13 -160.48(9) . . . . ?
C3 W C1 O1 61(4) . . . . ?
C5 W C1 O1 -43(5) . . . . ?
C2 W C1 O1 150(4) . . . . ?
C4 W C1 O1 -31(4) . . . . ?
P W C1 O1 -120(4) . . . . ?
C3 W C2 O2 -60(23) . . . . ?
C1 W C2 O2 -148(23) . . . . ?
C5 W C2 O2 32(23) . . . . ?
C4 W C2 O2 113(22) . . . . ?
P W C2 O2 124(23) . . . . ?
C1 W C3 O3 48(3) . . . . ?
C5 W C3 O3 -135(3) . . . . ?
C2 W C3 O3 -43(3) . . . . ?
C4 W C3 O3 137(3) . . . . ?
P W C3 O3 23(4) . . . . ?
C3 W C4 O4 -102(100) . . . . ?
C1 W C4 O4 -13(78) . . . . ?
C5 W C4 O4 166(100) . . . . ?
C2 W C4 O4 85(79) . . . . ?
P W C4 O4 75(78) . . . . ?
C3 W C5 O5 -149(10) . . . . ?
C1 W C5 O5 -45(11) . . . . ?
C2 W C5 O5 122(10) . . . . ?
C4 W C5 O5 -57(10) . . . . ?
P W C5 O5 32(10) . . . . ?
C13 P C6 Si2 91.28(10) . . . . ?
W P C6 Si2 -137.22(6) . . . . ?
C13 P C6 Si1 -46.06(12) . . . . ?
W P C6 Si1 85.45(10) . . . . ?
C10 Si2 C6 P 175.00(10) . . . . ?
C12 Si2 C6 P 57.97(12) . . . . ?
C11 Si2 C6 P -62.33(12) . . . . ?
C10 Si2 C6 Si1 -47.93(13) . . . . ?
C12 Si2 C6 Si1 -164.96(11) . . . . ?
C11 Si2 C6 Si1 74.74(12) . . . . ?
C8 Si1 C6 P -144.32(11) . . . . ?
C7 Si1 C6 P -26.47(13) . . . . ?
C9 Si1 C6 P 94.34(12) . . . . ?
C8 Si1 C6 Si2 81.36(12) . . . . ?
C7 Si1 C6 Si2 -160.79(10) . . . . ?
C9 Si1 C6 Si2 -39.98(13) . . . . ?
C6 P C13 N 101(4) . . . . ?
W P C13 N -36(4) . . . . ?
|
1100806.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 08:41:18 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180562 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100806.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100806
loop_
_publ_author_name
'Dorcier, Antoine'
'Dyson, Paul J.'
'Gossens, Christian'
'Rothlisberger, Ursula'
'Scopelliti, Rosario'
'Tavernelli, Ivano'
_publ_section_title
;
Binding of Organometallic Ruthenium(II) and Osmium(II) Complexes to
an Oligonucleotide: A Combined Mass Spectrometric and Theoretical Study
;
_cod_duplicate_entry 4060315
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2114
_journal_page_last 2123
_journal_paper_doi 10.1021/om049022a
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C17 H29 Cl2 N3 P Ru, 0.5(C H4 O), Cl'
_chemical_formula_sum 'C17.5 H31 Cl3 N3 O0.5 P Ru'
_chemical_formula_weight 529.84
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 113.411(9)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.4320(13)
_cell_length_b 10.5988(10)
_cell_length_c 16.2393(15)
_cell_measurement_reflns_used 5348
_cell_measurement_temperature 140(2)
_cell_measurement_theta_max 26.8249
_cell_measurement_theta_min 2.3858
_cell_volume 2121.6(3)
_computing_cell_refinement 'Oxford Diffraction CrysAlis RED'
_computing_data_collection 'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction 'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 140(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type 'Oxford Diffraction KM4/Sapphire CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0738
_diffrn_reflns_av_sigmaI/netI 0.0526
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 12048
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 3.18
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.203
_exptl_absorpt_correction_T_max 0.852
_exptl_absorpt_correction_T_min 0.527
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.659
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1084
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.697
_refine_diff_density_min -0.907
_refine_diff_density_rms 0.127
_refine_ls_extinction_coef 0.0002(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.022
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 239
_refine_ls_number_reflns 3373
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.022
_refine_ls_R_factor_all 0.0513
_refine_ls_R_factor_gt 0.0426
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1101
_refine_ls_wR_factor_ref 0.1147
_reflns_number_gt 2819
_reflns_number_total 3373
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om049022asi20041210_041724.cif
_cod_data_source_block 2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_original_formula_sum 'C17.50 H31 Cl3 N3 O0.50 P Ru'
_cod_database_code 1100806
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.16735(2) 0.05648(3) 0.35285(2) 0.01820(16) Uani 1 1 d . . .
Cl1 Cl 0.17994(9) -0.15280(10) 0.30298(7) 0.0300(3) Uani 1 1 d . . .
Cl2 Cl -0.00231(8) -0.00577(11) 0.35866(8) 0.0301(3) Uani 1 1 d . . .
P1 P 0.24332(8) -0.04294(10) 0.48779(7) 0.0191(3) Uani 1 1 d . . .
N1 N 0.3043(3) -0.0363(3) 0.6718(2) 0.0264(9) Uani 1 1 d . . .
N2 N 0.2544(3) -0.2410(3) 0.5972(3) 0.0299(9) Uani 1 1 d . . .
N3 N 0.4256(3) -0.1434(4) 0.6149(2) 0.0288(9) Uani 1 1 d . . .
C1 C 0.2464(3) 0.0388(4) 0.5870(3) 0.0213(10) Uani 1 1 d . . .
H1A H 0.2833 0.1211 0.5922 0.026 Uiso 1 1 calc R . .
H1B H 0.1711 0.0557 0.5804 0.026 Uiso 1 1 calc R . .
C2 C 0.1904(4) -0.1936(4) 0.5070(3) 0.0307(11) Uani 1 1 d . . .
H2A H 0.1140 -0.1829 0.4994 0.037 Uiso 1 1 calc R . .
H2B H 0.1921 -0.2558 0.4621 0.037 Uiso 1 1 calc R . .
C3 C 0.3870(3) -0.0817(4) 0.5268(3) 0.0266(10) Uani 1 1 d . . .
H3A H 0.3986 -0.1385 0.4830 0.032 Uiso 1 1 calc R . .
H3B H 0.4292 -0.0036 0.5311 0.032 Uiso 1 1 calc R . .
C4 C 0.2482(4) -0.1631(4) 0.6657(3) 0.0318(11) Uani 1 1 d . . .
H4A H 0.2821 -0.2074 0.7240 0.038 Uiso 1 1 calc R . .
H4B H 0.1709 -0.1484 0.6541 0.038 Uiso 1 1 calc R . .
C5 C 0.3675(4) -0.2606(4) 0.6121(3) 0.0333(11) Uani 1 1 d . . .
H5A H 0.3708 -0.3146 0.5635 0.040 Uiso 1 1 calc R . .
H5B H 0.4043 -0.3062 0.6695 0.040 Uiso 1 1 calc R . .
C6 C 0.4219(3) -0.0634(4) 0.6830(3) 0.0277(11) Uani 1 1 d . . .
H6A H 0.4583 0.0172 0.6816 0.033 Uiso 1 1 calc R . .
H6B H 0.4619 -0.1033 0.7422 0.033 Uiso 1 1 calc R . .
C7 C 0.3051(4) 0.0356(5) 0.7502(3) 0.0420(14) Uani 1 1 d . . .
H7A H 0.2304 0.0520 0.7431 0.063 Uiso 1 1 calc R . .
H7B H 0.3430 0.1159 0.7543 0.063 Uiso 1 1 calc R . .
H7C H 0.3426 -0.0136 0.8050 0.063 Uiso 1 1 calc R . .
C8 C 0.2297(4) 0.1236(4) 0.2528(3) 0.0296(11) Uani 1 1 d . . .
C9 C 0.1242(4) 0.1700(4) 0.2274(3) 0.0322(12) Uani 1 1 d . . .
H9 H 0.0722 0.1574 0.1679 0.039 Uiso 1 1 calc R . .
C10 C 0.0954(4) 0.2352(4) 0.2898(3) 0.0283(10) Uani 1 1 d . . .
H10 H 0.0224 0.2623 0.2726 0.034 Uiso 1 1 calc R . .
C11 C 0.1711(4) 0.2615(4) 0.3769(3) 0.0263(10) Uani 1 1 d . . .
C12 C 0.2759(3) 0.2141(4) 0.4008(3) 0.0267(10) Uani 1 1 d . . .
H12 H 0.3282 0.2279 0.4600 0.032 Uiso 1 1 calc R . .
C13 C 0.3059(3) 0.1475(4) 0.3407(3) 0.0284(11) Uani 1 1 d . . .
H13 H 0.3782 0.1178 0.3590 0.034 Uiso 1 1 calc R . .
C14 C 0.2626(5) 0.0482(5) 0.1897(4) 0.0480(15) Uani 1 1 d . . .
H14A H 0.1981 0.0101 0.1435 0.072 Uiso 1 1 calc R . .
H14B H 0.3130 -0.0184 0.2231 0.072 Uiso 1 1 calc R . .
H14C H 0.2981 0.1036 0.1613 0.072 Uiso 1 1 calc R . .
C15 C 0.1464(4) 0.3423(4) 0.4438(3) 0.0337(11) Uani 1 1 d . . .
H15 H 0.2040 0.3255 0.5047 0.040 Uiso 1 1 calc R . .
C16 C 0.1552(5) 0.4796(5) 0.4213(4) 0.0502(15) Uani 1 1 d . . .
H16A H 0.2277 0.4957 0.4227 0.075 Uiso 1 1 calc R . .
H16B H 0.1431 0.5336 0.4654 0.075 Uiso 1 1 calc R . .
H16C H 0.1005 0.4982 0.3612 0.075 Uiso 1 1 calc R . .
C17 C 0.0395(4) 0.3142(5) 0.4474(4) 0.0502(15) Uani 1 1 d . . .
H17A H -0.0187 0.3317 0.3887 0.075 Uiso 1 1 calc R . .
H17B H 0.0300 0.3672 0.4931 0.075 Uiso 1 1 calc R . .
H17C H 0.0369 0.2251 0.4626 0.075 Uiso 1 1 calc R . .
Cl3 Cl 0.47269(12) 0.23843(13) 0.62974(8) 0.0522(4) Uani 1 1 d . . .
O1 O 0.5907(7) 0.3987(8) 0.5531(6) 0.063(2) Uani 0.50 1 d P A -1
H1 H 0.5593 0.3379 0.5659 0.095 Uiso 0.50 1 calc PR A -1
C18 C 0.5143(16) 0.4813(16) 0.4977(16) 0.063(2) Uani 0.50 1 d P A -1
H18A H 0.5273 0.5656 0.5247 0.095 Uiso 0.50 1 calc PR A -1
H18B H 0.4416 0.4526 0.4897 0.095 Uiso 0.50 1 calc PR A -1
H18C H 0.5195 0.4845 0.4392 0.095 Uiso 0.50 1 calc PR A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0179(2) 0.0215(2) 0.0165(2) -0.00085(13) 0.00816(15) -0.00038(13)
Cl1 0.0371(6) 0.0267(6) 0.0313(6) -0.0094(4) 0.0188(5) -0.0021(5)
Cl2 0.0209(5) 0.0313(6) 0.0416(6) 0.0013(5) 0.0161(5) -0.0004(4)
P1 0.0192(6) 0.0210(6) 0.0187(5) 0.0003(4) 0.0093(5) -0.0012(4)
N1 0.0274(19) 0.034(2) 0.0193(18) 0.0063(16) 0.0111(16) 0.0020(16)
N2 0.032(2) 0.030(2) 0.031(2) 0.0121(17) 0.0166(18) 0.0019(16)
N3 0.0233(18) 0.037(2) 0.028(2) 0.0091(17) 0.0116(16) 0.0074(16)
C1 0.023(2) 0.024(2) 0.019(2) 0.0082(17) 0.0108(19) 0.0032(17)
C2 0.032(2) 0.029(2) 0.031(2) 0.002(2) 0.012(2) -0.006(2)
C3 0.025(2) 0.035(3) 0.026(2) 0.0046(19) 0.017(2) 0.0043(19)
C4 0.032(2) 0.037(3) 0.032(2) 0.015(2) 0.019(2) 0.001(2)
C5 0.039(3) 0.028(2) 0.039(3) 0.013(2) 0.022(2) 0.008(2)
C6 0.019(2) 0.042(3) 0.020(2) 0.0104(19) 0.0053(19) 0.0011(19)
C7 0.049(3) 0.061(4) 0.019(2) -0.003(2) 0.016(2) 0.004(3)
C8 0.043(3) 0.028(2) 0.031(2) 0.000(2) 0.028(2) -0.002(2)
C9 0.036(3) 0.033(3) 0.021(2) 0.0047(19) 0.005(2) -0.001(2)
C10 0.029(2) 0.027(2) 0.033(2) 0.006(2) 0.017(2) 0.0061(19)
C11 0.037(3) 0.021(2) 0.026(2) 0.0055(18) 0.019(2) -0.0027(19)
C12 0.028(2) 0.025(2) 0.024(2) 0.0045(19) 0.008(2) -0.0115(19)
C13 0.022(2) 0.028(2) 0.042(3) 0.009(2) 0.019(2) 0.0001(18)
C14 0.065(4) 0.051(3) 0.050(3) -0.004(3) 0.046(3) -0.002(3)
C15 0.045(3) 0.025(2) 0.033(2) -0.005(2) 0.018(2) 0.001(2)
C16 0.077(4) 0.024(3) 0.070(4) -0.007(3) 0.051(4) -0.004(3)
C17 0.051(3) 0.050(3) 0.066(4) -0.022(3) 0.041(3) -0.006(3)
Cl3 0.0665(9) 0.0457(8) 0.0309(6) -0.0076(5) 0.0051(6) -0.0219(7)
O1 0.081(6) 0.060(5) 0.065(4) 0.000(4) 0.046(4) 0.000(4)
C18 0.081(6) 0.060(5) 0.065(4) 0.000(4) 0.046(4) 0.000(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Ru1 C13 37.43(18) . . ?
C12 Ru1 C10 66.84(16) . . ?
C13 Ru1 C10 78.94(17) . . ?
C12 Ru1 C11 37.38(17) . . ?
C13 Ru1 C11 67.56(17) . . ?
C10 Ru1 C11 37.26(16) . . ?
C12 Ru1 C8 67.50(17) . . ?
C13 Ru1 C8 37.43(16) . . ?
C10 Ru1 C8 66.74(17) . . ?
C11 Ru1 C8 79.92(17) . . ?
C12 Ru1 C9 78.74(16) . . ?
C13 Ru1 C9 66.39(17) . . ?
C10 Ru1 C9 36.95(17) . . ?
C11 Ru1 C9 67.05(16) . . ?
C8 Ru1 C9 36.58(17) . . ?
C12 Ru1 P1 91.77(11) . . ?
C13 Ru1 P1 102.73(12) . . ?
C10 Ru1 P1 142.91(12) . . ?
C11 Ru1 P1 108.43(12) . . ?
C8 Ru1 P1 134.26(12) . . ?
C9 Ru1 P1 169.05(12) . . ?
C12 Ru1 Cl1 135.64(13) . . ?
C13 Ru1 Cl1 101.72(13) . . ?
C10 Ru1 Cl1 136.26(12) . . ?
C11 Ru1 Cl1 167.12(13) . . ?
C8 Ru1 Cl1 87.21(12) . . ?
C9 Ru1 Cl1 102.61(12) . . ?
P1 Ru1 Cl1 80.30(4) . . ?
C12 Ru1 Cl2 135.58(13) . . ?
C13 Ru1 Cl2 169.12(12) . . ?
C10 Ru1 Cl2 90.37(12) . . ?
C11 Ru1 Cl2 102.61(12) . . ?
C8 Ru1 Cl2 138.94(12) . . ?
C9 Ru1 Cl2 106.05(12) . . ?
P1 Ru1 Cl2 84.53(4) . . ?
Cl1 Ru1 Cl2 87.39(4) . . ?
C1 P1 C3 98.7(2) . . ?
C1 P1 C2 98.0(2) . . ?
C3 P1 C2 100.0(2) . . ?
C1 P1 Ru1 118.50(13) . . ?
C3 P1 Ru1 116.55(15) . . ?
C2 P1 Ru1 120.95(14) . . ?
C7 N1 C1 109.7(3) . . ?
C7 N1 C4 110.2(4) . . ?
C1 N1 C4 110.1(3) . . ?
C7 N1 C6 109.7(3) . . ?
C1 N1 C6 109.7(3) . . ?
C4 N1 C6 107.4(3) . . ?
C4 N2 C5 109.7(4) . . ?
C4 N2 C2 113.1(4) . . ?
C5 N2 C2 112.1(4) . . ?
C6 N3 C5 110.6(4) . . ?
C6 N3 C3 112.8(3) . . ?
C5 N3 C3 111.8(3) . . ?
N1 C1 P1 112.3(3) . . ?
N1 C1 H1A 109.2 . . ?
P1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
P1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 P1 111.0(3) . . ?
N2 C2 H2A 109.4 . . ?
P1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
P1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N3 C3 P1 110.7(3) . . ?
N3 C3 H3A 109.5 . . ?
P1 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N2 C4 N1 112.5(4) . . ?
N2 C4 H4A 109.1 . . ?
N1 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
N1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 N3 113.2(4) . . ?
N2 C5 H5A 108.9 . . ?
N3 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N3 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
N3 C6 N1 111.9(3) . . ?
N3 C6 H6A 109.2 . . ?
N1 C6 H6A 109.2 . . ?
N3 C6 H6B 109.2 . . ?
N1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 118.5(4) . . ?
C9 C8 C14 121.7(4) . . ?
C13 C8 C14 119.8(4) . . ?
C9 C8 Ru1 72.3(3) . . ?
C13 C8 Ru1 69.5(3) . . ?
C14 C8 Ru1 129.0(4) . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 Ru1 71.1(3) . . ?
C10 C9 Ru1 69.7(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
Ru1 C9 H9 132.1 . . ?
C9 C10 C11 121.9(4) . . ?
C9 C10 Ru1 73.4(3) . . ?
C11 C10 Ru1 72.0(2) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
Ru1 C10 H10 127.7 . . ?
C12 C11 C10 117.1(4) . . ?
C12 C11 C15 119.1(4) . . ?
C10 C11 C15 123.8(4) . . ?
C12 C11 Ru1 69.2(2) . . ?
C10 C11 Ru1 70.7(3) . . ?
C15 C11 Ru1 133.3(3) . . ?
C13 C12 C11 122.0(4) . . ?
C13 C12 Ru1 72.2(2) . . ?
C11 C12 Ru1 73.5(2) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
Ru1 C12 H12 127.5 . . ?
C12 C13 C8 120.5(4) . . ?
C12 C13 Ru1 70.4(3) . . ?
C8 C13 Ru1 73.1(3) . . ?
C12 C13 H13 119.8 . . ?
C8 C13 H13 119.8 . . ?
Ru1 C13 H13 129.1 . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C16 111.7(4) . . ?
C17 C15 C11 113.8(4) . . ?
C16 C15 C11 107.9(4) . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C11 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 O1 H1 109.5 . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C12 2.150(4) . ?
Ru1 C13 2.173(4) . ?
Ru1 C10 2.187(4) . ?
Ru1 C11 2.205(4) . ?
Ru1 C8 2.221(5) . ?
Ru1 C9 2.235(4) . ?
Ru1 P1 2.2753(11) . ?
Ru1 Cl1 2.3903(11) . ?
Ru1 Cl2 2.4101(11) . ?
P1 C1 1.816(4) . ?
P1 C3 1.823(4) . ?
P1 C2 1.824(5) . ?
N1 C7 1.479(6) . ?
N1 C1 1.511(5) . ?
N1 C4 1.525(6) . ?
N1 C6 1.543(6) . ?
N2 C4 1.414(6) . ?
N2 C5 1.455(6) . ?
N2 C2 1.461(6) . ?
N3 C6 1.410(6) . ?
N3 C5 1.458(6) . ?
N3 C3 1.468(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.398(6) . ?
C8 C13 1.411(6) . ?
C8 C14 1.497(7) . ?
C9 C10 1.402(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.403(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(6) . ?
C11 C15 1.520(7) . ?
C12 C13 1.387(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.490(7) . ?
C15 C16 1.517(7) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O1 C18 1.38(2) . ?
O1 H1 0.8400 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl3 0.84 2.12 2.917(9) 158.3 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 Ru1 P1 C1 56.9(2) . . . . ?
C13 Ru1 P1 C1 93.0(2) . . . . ?
C10 Ru1 P1 C1 4.6(3) . . . . ?
C11 Ru1 P1 C1 22.7(2) . . . . ?
C8 Ru1 P1 C1 116.6(2) . . . . ?
C9 Ru1 P1 C1 86.6(7) . . . . ?
Cl1 Ru1 P1 C1 -167.04(17) . . . . ?
Cl2 Ru1 P1 C1 -78.76(17) . . . . ?
C12 Ru1 P1 C3 -60.8(2) . . . . ?
C13 Ru1 P1 C3 -24.6(2) . . . . ?
C10 Ru1 P1 C3 -113.1(3) . . . . ?
C11 Ru1 P1 C3 -94.9(2) . . . . ?
C8 Ru1 P1 C3 -1.1(2) . . . . ?
C9 Ru1 P1 C3 -31.1(7) . . . . ?
Cl1 Ru1 P1 C3 75.30(17) . . . . ?
Cl2 Ru1 P1 C3 163.58(17) . . . . ?
C12 Ru1 P1 C2 177.5(2) . . . . ?
C13 Ru1 P1 C2 -146.4(2) . . . . ?
C10 Ru1 P1 C2 125.2(3) . . . . ?
C11 Ru1 P1 C2 143.4(2) . . . . ?
C8 Ru1 P1 C2 -122.8(3) . . . . ?
C9 Ru1 P1 C2 -152.8(7) . . . . ?
Cl1 Ru1 P1 C2 -46.4(2) . . . . ?
Cl2 Ru1 P1 C2 41.9(2) . . . . ?
C7 N1 C1 P1 179.4(3) . . . . ?
C4 N1 C1 P1 -59.2(4) . . . . ?
C6 N1 C1 P1 58.8(4) . . . . ?
C3 P1 C1 N1 -50.3(3) . . . . ?
C2 P1 C1 N1 51.1(3) . . . . ?
Ru1 P1 C1 N1 -177.1(2) . . . . ?
C4 N2 C2 P1 64.6(5) . . . . ?
C5 N2 C2 P1 -60.0(5) . . . . ?
C1 P1 C2 N2 -51.8(4) . . . . ?
C3 P1 C2 N2 48.6(4) . . . . ?
Ru1 P1 C2 N2 178.0(3) . . . . ?
C6 N3 C3 P1 -65.1(4) . . . . ?
C5 N3 C3 P1 60.3(4) . . . . ?
C1 P1 C3 N3 51.1(3) . . . . ?
C2 P1 C3 N3 -48.7(4) . . . . ?
Ru1 P1 C3 N3 179.1(2) . . . . ?
C5 N2 C4 N1 57.3(4) . . . . ?
C2 N2 C4 N1 -68.6(5) . . . . ?
C7 N1 C4 N2 -174.2(4) . . . . ?
C1 N1 C4 N2 64.7(5) . . . . ?
C6 N1 C4 N2 -54.7(4) . . . . ?
C4 N2 C5 N3 -58.2(5) . . . . ?
C2 N2 C5 N3 68.3(5) . . . . ?
C6 N3 C5 N2 58.2(5) . . . . ?
C3 N3 C5 N2 -68.5(5) . . . . ?
C5 N3 C6 N1 -55.9(4) . . . . ?
C3 N3 C6 N1 70.2(5) . . . . ?
C7 N1 C6 N3 173.5(4) . . . . ?
C1 N1 C6 N3 -65.9(4) . . . . ?
C4 N1 C6 N3 53.8(4) . . . . ?
C12 Ru1 C8 C9 -101.7(3) . . . . ?
C13 Ru1 C8 C9 -130.9(4) . . . . ?
C10 Ru1 C8 C9 -28.3(3) . . . . ?
C11 Ru1 C8 C9 -64.9(3) . . . . ?
P1 Ru1 C8 C9 -170.8(2) . . . . ?
Cl1 Ru1 C8 C9 115.6(3) . . . . ?
Cl2 Ru1 C8 C9 32.8(4) . . . . ?
C12 Ru1 C8 C13 29.2(3) . . . . ?
C10 Ru1 C8 C13 102.6(3) . . . . ?
C11 Ru1 C8 C13 66.1(3) . . . . ?
C9 Ru1 C8 C13 130.9(4) . . . . ?
P1 Ru1 C8 C13 -39.9(3) . . . . ?
Cl1 Ru1 C8 C13 -113.5(3) . . . . ?
Cl2 Ru1 C8 C13 163.7(2) . . . . ?
C12 Ru1 C8 C14 141.4(5) . . . . ?
C13 Ru1 C8 C14 112.3(5) . . . . ?
C10 Ru1 C8 C14 -145.1(5) . . . . ?
C11 Ru1 C8 C14 178.3(5) . . . . ?
C9 Ru1 C8 C14 -116.8(6) . . . . ?
P1 Ru1 C8 C14 72.4(5) . . . . ?
Cl1 Ru1 C8 C14 -1.2(4) . . . . ?
Cl2 Ru1 C8 C14 -84.0(5) . . . . ?
C13 C8 C9 C10 -2.0(7) . . . . ?
C14 C8 C9 C10 177.0(4) . . . . ?
Ru1 C8 C9 C10 51.6(4) . . . . ?
C13 C8 C9 Ru1 -53.6(4) . . . . ?
C14 C8 C9 Ru1 125.4(5) . . . . ?
C12 Ru1 C9 C8 67.3(3) . . . . ?
C13 Ru1 C9 C8 30.1(3) . . . . ?
C10 Ru1 C9 C8 133.5(4) . . . . ?
C11 Ru1 C9 C8 104.6(3) . . . . ?
P1 Ru1 C9 C8 37.0(8) . . . . ?
Cl1 Ru1 C9 C8 -67.3(3) . . . . ?
Cl2 Ru1 C9 C8 -158.3(2) . . . . ?
C12 Ru1 C9 C10 -66.3(3) . . . . ?
C13 Ru1 C9 C10 -103.5(3) . . . . ?
C11 Ru1 C9 C10 -29.0(3) . . . . ?
C8 Ru1 C9 C10 -133.5(4) . . . . ?
P1 Ru1 C9 C10 -96.6(7) . . . . ?
Cl1 Ru1 C9 C10 159.1(2) . . . . ?
Cl2 Ru1 C9 C10 68.2(3) . . . . ?
C8 C9 C10 C11 3.3(7) . . . . ?
Ru1 C9 C10 C11 55.6(4) . . . . ?
C8 C9 C10 Ru1 -52.3(4) . . . . ?
C12 Ru1 C10 C9 102.4(3) . . . . ?
C13 Ru1 C10 C9 65.2(3) . . . . ?
C11 Ru1 C10 C9 132.5(4) . . . . ?
C8 Ru1 C10 C9 28.0(3) . . . . ?
P1 Ru1 C10 C9 161.8(2) . . . . ?
Cl1 Ru1 C10 C9 -30.2(3) . . . . ?
Cl2 Ru1 C10 C9 -116.8(3) . . . . ?
C12 Ru1 C10 C11 -30.1(3) . . . . ?
C13 Ru1 C10 C11 -67.3(3) . . . . ?
C8 Ru1 C10 C11 -104.5(3) . . . . ?
C9 Ru1 C10 C11 -132.5(4) . . . . ?
P1 Ru1 C10 C11 29.2(4) . . . . ?
Cl1 Ru1 C10 C11 -162.8(2) . . . . ?
Cl2 Ru1 C10 C11 110.6(3) . . . . ?
C9 C10 C11 C12 -3.3(7) . . . . ?
Ru1 C10 C11 C12 52.9(4) . . . . ?
C9 C10 C11 C15 174.0(4) . . . . ?
Ru1 C10 C11 C15 -129.7(4) . . . . ?
C9 C10 C11 Ru1 -56.2(4) . . . . ?
C13 Ru1 C11 C12 -29.0(3) . . . . ?
C10 Ru1 C11 C12 -130.6(4) . . . . ?
C8 Ru1 C11 C12 -66.0(3) . . . . ?
C9 Ru1 C11 C12 -101.8(3) . . . . ?
P1 Ru1 C11 C12 67.5(3) . . . . ?
Cl1 Ru1 C11 C12 -63.8(6) . . . . ?
Cl2 Ru1 C11 C12 155.9(2) . . . . ?
C12 Ru1 C11 C10 130.6(4) . . . . ?
C13 Ru1 C11 C10 101.6(3) . . . . ?
C8 Ru1 C11 C10 64.6(3) . . . . ?
C9 Ru1 C11 C10 28.7(3) . . . . ?
P1 Ru1 C11 C10 -161.9(3) . . . . ?
Cl1 Ru1 C11 C10 66.7(6) . . . . ?
Cl2 Ru1 C11 C10 -73.6(3) . . . . ?
C12 Ru1 C11 C15 -110.8(5) . . . . ?
C13 Ru1 C11 C15 -139.8(5) . . . . ?
C10 Ru1 C11 C15 118.6(5) . . . . ?
C8 Ru1 C11 C15 -176.8(4) . . . . ?
C9 Ru1 C11 C15 147.4(5) . . . . ?
P1 Ru1 C11 C15 -43.3(4) . . . . ?
Cl1 Ru1 C11 C15 -174.6(3) . . . . ?
Cl2 Ru1 C11 C15 45.1(4) . . . . ?
C10 C11 C12 C13 2.2(6) . . . . ?
C15 C11 C12 C13 -175.3(4) . . . . ?
Ru1 C11 C12 C13 55.9(4) . . . . ?
C10 C11 C12 Ru1 -53.7(4) . . . . ?
C15 C11 C12 Ru1 128.9(4) . . . . ?
C10 Ru1 C12 C13 -102.5(3) . . . . ?
C11 Ru1 C12 C13 -132.5(4) . . . . ?
C8 Ru1 C12 C13 -29.2(3) . . . . ?
C9 Ru1 C12 C13 -65.7(3) . . . . ?
P1 Ru1 C12 C13 108.8(2) . . . . ?
Cl1 Ru1 C12 C13 30.9(3) . . . . ?
Cl2 Ru1 C12 C13 -167.2(2) . . . . ?
C13 Ru1 C12 C11 132.5(4) . . . . ?
C10 Ru1 C12 C11 30.0(3) . . . . ?
C8 Ru1 C12 C11 103.3(3) . . . . ?
C9 Ru1 C12 C11 66.8(3) . . . . ?
P1 Ru1 C12 C11 -118.7(3) . . . . ?
Cl1 Ru1 C12 C11 163.4(2) . . . . ?
Cl2 Ru1 C12 C11 -34.7(3) . . . . ?
C11 C12 C13 C8 -1.0(7) . . . . ?
Ru1 C12 C13 C8 55.4(4) . . . . ?
C11 C12 C13 Ru1 -56.4(4) . . . . ?
C9 C8 C13 C12 0.9(7) . . . . ?
C14 C8 C13 C12 -178.1(4) . . . . ?
Ru1 C8 C13 C12 -54.1(4) . . . . ?
C9 C8 C13 Ru1 55.0(4) . . . . ?
C14 C8 C13 Ru1 -124.0(4) . . . . ?
C10 Ru1 C13 C12 66.2(3) . . . . ?
C11 Ru1 C13 C12 29.0(2) . . . . ?
C8 Ru1 C13 C12 132.2(4) . . . . ?
C9 Ru1 C13 C12 102.7(3) . . . . ?
P1 Ru1 C13 C12 -75.9(2) . . . . ?
Cl1 Ru1 C13 C12 -158.5(2) . . . . ?
Cl2 Ru1 C13 C12 55.2(8) . . . . ?
C12 Ru1 C13 C8 -132.2(4) . . . . ?
C10 Ru1 C13 C8 -66.0(3) . . . . ?
C11 Ru1 C13 C8 -103.2(3) . . . . ?
C9 Ru1 C13 C8 -29.4(3) . . . . ?
P1 Ru1 C13 C8 151.9(2) . . . . ?
Cl1 Ru1 C13 C8 69.3(3) . . . . ?
Cl2 Ru1 C13 C8 -77.0(8) . . . . ?
C12 C11 C15 C17 -138.8(5) . . . . ?
C10 C11 C15 C17 43.9(6) . . . . ?
Ru1 C11 C15 C17 -50.9(6) . . . . ?
C12 C11 C15 C16 96.6(5) . . . . ?
C10 C11 C15 C16 -80.7(6) . . . . ?
Ru1 C11 C15 C16 -175.4(4) . . . . ?
|
1100807.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 08:41:18 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180562 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100807.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100807
loop_
_publ_author_name
'Dorcier, Antoine'
'Dyson, Paul J.'
'Gossens, Christian'
'Rothlisberger, Ursula'
'Scopelliti, Rosario'
'Tavernelli, Ivano'
_publ_section_title
;
Binding of Organometallic Ruthenium(II) and Osmium(II) Complexes to
an Oligonucleotide: A Combined Mass Spectrometric and Theoretical Study
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2114
_journal_page_last 2123
_journal_paper_doi 10.1021/om049022a
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C16 H26 Cl2 N3 Os P, 2(C H Cl3)'
_chemical_formula_sum 'C18 H28 Cl8 N3 Os P'
_chemical_formula_weight 791.20
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 101.171(16)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.579(2)
_cell_length_b 12.7402(9)
_cell_length_c 20.977(4)
_cell_measurement_reflns_used 4157
_cell_measurement_temperature 140(2)
_cell_measurement_theta_max 25.64935
_cell_measurement_theta_min 1.86985
_cell_volume 2773.7(8)
_computing_cell_refinement 'Oxford Diffraction CrysAlis RED'
_computing_data_collection 'marresearch mar345'
_computing_data_reduction 'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 140(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type 'marresearch mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg. and exp. time = 180 sec.'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71070
_diffrn_reflns_av_R_equivalents 0.0534
_diffrn_reflns_av_sigmaI/netI 0.0381
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 16359
_diffrn_reflns_theta_full 25.02
_diffrn_reflns_theta_max 25.02
_diffrn_reflns_theta_min 2.85
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.439
_exptl_absorpt_correction_T_max 0.744
_exptl_absorpt_correction_T_min 0.306
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.895
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1536
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.11
_refine_diff_density_max 1.208
_refine_diff_density_min -1.444
_refine_diff_density_rms 0.190
_refine_ls_extinction_coef 0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 281
_refine_ls_number_reflns 4836
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.128
_refine_ls_R_factor_all 0.0460
_refine_ls_R_factor_gt 0.0426
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+10.5637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1106
_refine_ls_wR_factor_ref 0.1139
_reflns_number_gt 4353
_reflns_number_total 4836
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060316
_cod_data_source_file om049022asi20041210_041724.cif
_cod_data_source_block 3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.28369(2) 0.436995(18) 0.207975(11) 0.02626(14) Uani 1 1 d . . .
Cl1 Cl 0.44239(14) 0.31660(12) 0.26770(7) 0.0324(3) Uani 1 1 d . . .
Cl2 Cl 0.12769(15) 0.29913(12) 0.21101(7) 0.0331(3) Uani 1 1 d . . .
P1 P 0.25893(15) 0.47990(13) 0.31296(7) 0.0273(3) Uani 1 1 d . . .
N1 N 0.1479(6) 0.5926(5) 0.3990(3) 0.0377(13) Uani 1 1 d . . .
N2 N 0.2233(5) 0.4151(4) 0.4338(3) 0.0318(11) Uani 1 1 d . . .
N3 N 0.3799(6) 0.5575(4) 0.4320(3) 0.0334(12) Uani 1 1 d . . .
C1 C 0.1381(7) 0.5761(5) 0.3291(3) 0.0324(14) Uani 1 1 d . . .
H1A H 0.1514 0.6437 0.3081 0.039 Uiso 1 1 calc R . .
H1B H 0.0506 0.5504 0.3100 0.039 Uiso 1 1 calc R . .
C2 C 0.2238(6) 0.3743(5) 0.3679(3) 0.0324(13) Uani 1 1 d . . .
H2A H 0.1388 0.3429 0.3499 0.039 Uiso 1 1 calc R . .
H2B H 0.2897 0.3184 0.3705 0.039 Uiso 1 1 calc R . .
C3 C 0.4027(6) 0.5359(6) 0.3656(3) 0.0331(13) Uani 1 1 d . . .
H3A H 0.4755 0.4862 0.3684 0.040 Uiso 1 1 calc R . .
H3B H 0.4268 0.6020 0.3462 0.040 Uiso 1 1 calc R . .
C4 C 0.1228(7) 0.4960(6) 0.4330(3) 0.0387(15) Uani 1 1 d . . .
H4A H 0.0386 0.4668 0.4116 0.046 Uiso 1 1 calc R . .
H4B H 0.1172 0.5136 0.4783 0.046 Uiso 1 1 calc R . .
C5 C 0.3476(7) 0.4605(6) 0.4635(3) 0.0368(14) Uani 1 1 d . . .
H5A H 0.4159 0.4079 0.4622 0.044 Uiso 1 1 calc R . .
H5B H 0.3471 0.4758 0.5098 0.044 Uiso 1 1 calc R . .
C6 C 0.2751(7) 0.6338(6) 0.4295(3) 0.0394(16) Uani 1 1 d . . .
H6A H 0.2942 0.6963 0.4049 0.047 Uiso 1 1 calc R . .
H6B H 0.2722 0.6566 0.4743 0.047 Uiso 1 1 calc R . .
C7 C 0.4362(7) 0.4998(5) 0.1585(3) 0.0347(14) Uani 1 1 d . . .
C8 C 0.3575(7) 0.4295(5) 0.1143(3) 0.0344(15) Uani 1 1 d . . .
H8 H 0.3965 0.3744 0.0945 0.041 Uiso 1 1 calc R . .
C9 C 0.2233(7) 0.4416(5) 0.1002(3) 0.0302(14) Uani 1 1 d . . .
H9 H 0.1728 0.3937 0.0712 0.036 Uiso 1 1 calc R . .
C10 C 0.1596(6) 0.5248(5) 0.1287(3) 0.0308(13) Uani 1 1 d . . .
C11 C 0.2395(6) 0.5954(5) 0.1721(3) 0.0298(13) Uani 1 1 d . . .
H11 H 0.2012 0.6505 0.1922 0.036 Uiso 1 1 calc R . .
C12 C 0.3762(7) 0.5837(5) 0.1852(3) 0.0312(13) Uani 1 1 d . . .
H12 H 0.4279 0.6333 0.2124 0.037 Uiso 1 1 calc R . .
C13 C 0.5783(7) 0.4850(6) 0.1757(4) 0.0452(17) Uani 1 1 d . . .
H13A H 0.6186 0.5165 0.1419 0.068 Uiso 1 1 calc R . .
H13B H 0.5982 0.4098 0.1789 0.068 Uiso 1 1 calc R . .
H13C H 0.6118 0.5189 0.2175 0.068 Uiso 1 1 calc R . .
C14 C 0.0144(7) 0.5378(6) 0.1097(3) 0.0371(15) Uani 1 1 d . . .
H14 H -0.0208 0.4740 0.0846 0.045 Uiso 1 1 calc R . .
C15 C -0.0128(8) 0.6334(7) 0.0636(4) 0.0495(19) Uani 1 1 d . . .
H15A H 0.0123 0.6980 0.0882 0.074 Uiso 1 1 calc R . .
H15B H -0.1049 0.6360 0.0444 0.074 Uiso 1 1 calc R . .
H15C H 0.0369 0.6267 0.0289 0.074 Uiso 1 1 calc R . .
C16 C -0.0543(7) 0.5492(6) 0.1668(4) 0.0396(16) Uani 1 1 d . . .
H16A H -0.0318 0.4899 0.1966 0.059 Uiso 1 1 calc R . .
H16B H -0.1476 0.5503 0.1508 0.059 Uiso 1 1 calc R . .
H16C H -0.0275 0.6149 0.1899 0.059 Uiso 1 1 calc R . .
Cl3 Cl 0.07819(17) 0.29167(14) 0.57101(8) 0.0412(4) Uani 1 1 d . . .
Cl4 Cl 0.34964(19) 0.23377(17) 0.59780(10) 0.0520(5) Uani 1 1 d . . .
Cl5 Cl 0.1648(2) 0.10681(18) 0.51076(11) 0.0618(6) Uani 1 1 d . . .
C17 C 0.2051(7) 0.2366(6) 0.5391(3) 0.0407(16) Uani 1 1 d . . .
H17 H 0.2192 0.2805 0.5016 0.049 Uiso 1 1 calc R . .
Cl6 Cl 0.7593(2) 0.4619(2) 0.36050(12) 0.0671(6) Uani 1 1 d . . .
Cl7 Cl 0.8508(3) 0.3112(2) 0.27763(11) 0.0705(7) Uani 1 1 d . . .
Cl8 Cl 0.8521(3) 0.2586(2) 0.41131(11) 0.0699(6) Uani 1 1 d . . .
C18 C 0.7700(7) 0.3278(7) 0.3421(4) 0.0516(19) Uani 1 1 d . . .
H18 H 0.6809 0.2986 0.3292 0.062 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.02813(18) 0.0254(2) 0.02553(18) -0.00013(8) 0.00601(11) -0.00019(8)
Cl1 0.0307(7) 0.0292(8) 0.0367(8) 0.0015(6) 0.0051(6) 0.0017(6)
Cl2 0.0327(8) 0.0313(8) 0.0348(8) 0.0007(6) 0.0054(6) -0.0040(6)
P1 0.0280(8) 0.0283(8) 0.0260(7) 0.0006(6) 0.0060(6) -0.0005(6)
N1 0.038(3) 0.043(3) 0.036(3) 0.003(3) 0.014(2) 0.006(3)
N2 0.033(3) 0.037(3) 0.026(3) 0.003(2) 0.008(2) 0.000(2)
N3 0.033(3) 0.040(3) 0.027(3) -0.003(2) 0.005(2) -0.006(2)
C1 0.036(4) 0.032(3) 0.031(3) 0.001(2) 0.011(3) 0.008(3)
C2 0.036(3) 0.029(3) 0.034(3) -0.001(3) 0.013(3) 0.003(3)
C3 0.027(3) 0.040(4) 0.033(3) -0.001(3) 0.009(3) -0.005(3)
C4 0.032(3) 0.050(4) 0.034(3) 0.004(3) 0.008(3) 0.001(3)
C5 0.037(4) 0.044(4) 0.030(3) 0.001(3) 0.007(3) 0.005(3)
C6 0.054(4) 0.037(4) 0.029(3) -0.006(3) 0.014(3) 0.002(3)
C7 0.039(4) 0.034(3) 0.034(3) 0.007(3) 0.016(3) -0.006(3)
C8 0.044(4) 0.041(4) 0.021(3) 0.001(2) 0.014(3) 0.006(3)
C9 0.046(4) 0.030(3) 0.015(3) -0.002(2) 0.006(3) 0.000(3)
C10 0.035(3) 0.027(3) 0.029(3) 0.006(2) 0.003(3) -0.003(3)
C11 0.037(3) 0.024(3) 0.029(3) 0.006(2) 0.010(3) 0.001(3)
C12 0.038(4) 0.025(3) 0.032(3) 0.006(2) 0.009(3) -0.001(3)
C13 0.037(4) 0.049(5) 0.053(4) 0.008(3) 0.017(3) 0.000(3)
C14 0.034(4) 0.040(4) 0.035(3) -0.004(3) 0.002(3) 0.001(3)
C15 0.041(4) 0.065(5) 0.039(4) 0.011(4) -0.001(3) 0.007(4)
C16 0.034(4) 0.040(4) 0.045(4) 0.003(3) 0.009(3) 0.002(3)
Cl3 0.0423(9) 0.0403(9) 0.0438(9) -0.0009(7) 0.0156(7) 0.0025(7)
Cl4 0.0426(10) 0.0566(11) 0.0545(11) -0.0003(9) 0.0037(8) 0.0061(8)
Cl5 0.0750(15) 0.0509(12) 0.0596(12) -0.0202(10) 0.0132(11) 0.0030(10)
C17 0.046(4) 0.043(4) 0.036(4) 0.004(3) 0.015(3) 0.009(3)
Cl6 0.0482(12) 0.0822(15) 0.0673(14) -0.0220(12) 0.0025(10) 0.0068(11)
Cl7 0.0766(15) 0.0914(18) 0.0500(12) 0.0082(11) 0.0283(11) 0.0312(13)
Cl8 0.0736(15) 0.0850(17) 0.0503(12) 0.0045(11) 0.0094(11) -0.0106(12)
C18 0.034(4) 0.073(6) 0.049(4) -0.014(4) 0.009(3) -0.001(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Os1 C12 38.0(2) . . ?
C11 Os1 C10 38.1(2) . . ?
C12 Os1 C10 68.4(2) . . ?
C11 Os1 C9 67.9(2) . . ?
C12 Os1 C9 79.0(2) . . ?
C10 Os1 C9 38.0(2) . . ?
C11 Os1 C7 68.4(2) . . ?
C12 Os1 C7 37.2(2) . . ?
C10 Os1 C7 81.2(2) . . ?
C9 Os1 C7 67.0(3) . . ?
C11 Os1 C8 79.9(2) . . ?
C12 Os1 C8 66.6(2) . . ?
C10 Os1 C8 67.8(2) . . ?
C9 Os1 C8 36.5(3) . . ?
C7 Os1 C8 37.3(3) . . ?
C11 Os1 P1 93.08(17) . . ?
C12 Os1 P1 98.15(18) . . ?
C10 Os1 P1 115.59(18) . . ?
C9 Os1 P1 152.79(18) . . ?
C7 Os1 P1 125.39(18) . . ?
C8 Os1 P1 162.71(19) . . ?
C11 Os1 Cl2 125.54(18) . . ?
C12 Os1 Cl2 162.71(18) . . ?
C10 Os1 Cl2 94.49(17) . . ?
C9 Os1 Cl2 89.00(17) . . ?
C7 Os1 Cl2 146.29(18) . . ?
C8 Os1 Cl2 110.22(18) . . ?
P1 Os1 Cl2 86.75(5) . . ?
C11 Os1 Cl1 147.58(18) . . ?
C12 Os1 Cl1 110.79(18) . . ?
C10 Os1 Cl1 162.79(18) . . ?
C9 Os1 Cl1 124.92(17) . . ?
C7 Os1 Cl1 88.66(18) . . ?
C8 Os1 Cl1 95.80(18) . . ?
P1 Os1 Cl1 81.61(6) . . ?
Cl2 Os1 Cl1 86.27(5) . . ?
C3 P1 C1 98.8(3) . . ?
C3 P1 C2 98.6(3) . . ?
C1 P1 C2 97.9(3) . . ?
C3 P1 Os1 115.3(2) . . ?
C1 P1 Os1 122.4(2) . . ?
C2 P1 Os1 119.3(2) . . ?
C1 N1 C6 111.5(5) . . ?
C1 N1 C4 112.3(6) . . ?
C6 N1 C4 108.9(5) . . ?
C5 N2 C2 111.9(5) . . ?
C5 N2 C4 108.3(5) . . ?
C2 N2 C4 111.6(5) . . ?
C6 N3 C5 109.4(5) . . ?
C6 N3 C3 110.4(5) . . ?
C5 N3 C3 111.1(5) . . ?
N1 C1 P1 111.2(4) . . ?
N1 C1 H1A 109.4 . . ?
P1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
P1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 P1 111.3(4) . . ?
N2 C2 H2A 109.4 . . ?
P1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
P1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N3 C3 P1 111.7(4) . . ?
N3 C3 H3A 109.3 . . ?
P1 C3 H3A 109.3 . . ?
N3 C3 H3B 109.3 . . ?
P1 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 N2 113.0(5) . . ?
N1 C4 H4A 109.0 . . ?
N2 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
N2 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 N3 114.1(5) . . ?
N2 C5 H5A 108.7 . . ?
N3 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
N3 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N3 C6 N1 113.6(6) . . ?
N3 C6 H6A 108.8 . . ?
N1 C6 H6A 108.8 . . ?
N3 C6 H6B 108.8 . . ?
N1 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C12 C7 C8 118.7(6) . . ?
C12 C7 C13 120.7(6) . . ?
C8 C7 C13 120.7(6) . . ?
C12 C7 Os1 70.5(4) . . ?
C8 C7 Os1 72.2(4) . . ?
C13 C7 Os1 129.1(5) . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 Os1 70.8(4) . . ?
C7 C8 Os1 70.5(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
Os1 C8 H8 131.8 . . ?
C8 C9 C10 121.8(6) . . ?
C8 C9 Os1 72.7(4) . . ?
C10 C9 Os1 70.4(3) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
Os1 C9 H9 130.5 . . ?
C11 C10 C9 117.2(6) . . ?
C11 C10 C14 122.7(6) . . ?
C9 C10 C14 120.0(6) . . ?
C11 C10 Os1 69.5(3) . . ?
C9 C10 Os1 71.5(3) . . ?
C14 C10 Os1 132.5(5) . . ?
C12 C11 C10 120.6(6) . . ?
C12 C11 Os1 72.2(4) . . ?
C10 C11 Os1 72.4(4) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
Os1 C11 H11 127.8 . . ?
C7 C12 C11 121.3(6) . . ?
C7 C12 Os1 72.3(4) . . ?
C11 C12 Os1 69.8(4) . . ?
C7 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
Os1 C12 H12 131.4 . . ?
C7 C13 H13A 109.5 . . ?
C7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C16 114.5(6) . . ?
C10 C14 C15 107.9(6) . . ?
C16 C14 C15 110.9(6) . . ?
C10 C14 H14 107.8 . . ?
C16 C14 H14 107.8 . . ?
C15 C14 H14 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Cl3 C17 Cl4 111.4(4) . . ?
Cl3 C17 Cl5 110.3(4) . . ?
Cl4 C17 Cl5 109.4(4) . . ?
Cl3 C17 H17 108.6 . . ?
Cl4 C17 H17 108.6 . . ?
Cl5 C17 H17 108.6 . . ?
Cl7 C18 Cl6 110.4(5) . . ?
Cl7 C18 Cl8 109.7(4) . . ?
Cl6 C18 Cl8 110.2(4) . . ?
Cl7 C18 H18 108.8 . . ?
Cl6 C18 H18 108.8 . . ?
Cl8 C18 H18 108.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C11 2.173(6) . ?
Os1 C12 2.205(6) . ?
Os1 C10 2.212(6) . ?
Os1 C9 2.227(6) . ?
Os1 C7 2.229(6) . ?
Os1 C8 2.252(6) . ?
Os1 P1 2.3324(16) . ?
Os1 Cl2 2.4194(15) . ?
Os1 Cl1 2.4344(15) . ?
P1 C3 1.842(7) . ?
P1 C1 1.849(6) . ?
P1 C2 1.856(6) . ?
N1 C1 1.465(9) . ?
N1 C6 1.470(10) . ?
N1 C4 1.472(9) . ?
N2 C5 1.461(9) . ?
N2 C2 1.477(8) . ?
N2 C4 1.479(9) . ?
N3 C6 1.467(9) . ?
N3 C5 1.473(9) . ?
N3 C3 1.483(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.413(9) . ?
C7 C8 1.434(10) . ?
C7 C13 1.489(10) . ?
C8 C9 1.401(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.447(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.433(9) . ?
C10 C14 1.519(9) . ?
C11 C12 1.426(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.525(10) . ?
C14 C15 1.547(10) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
Cl3 C17 1.758(7) . ?
Cl4 C17 1.768(8) . ?
Cl5 C17 1.781(8) . ?
C17 H17 1.0000 . ?
Cl6 C18 1.760(9) . ?
Cl7 C18 1.747(8) . ?
Cl8 C18 1.775(9) . ?
C18 H18 1.0000 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 Os1 P1 C3 -85.1(3) . . . . ?
C12 Os1 P1 C3 -47.2(3) . . . . ?
C10 Os1 P1 C3 -117.1(3) . . . . ?
C9 Os1 P1 C3 -129.1(4) . . . . ?
C7 Os1 P1 C3 -19.6(3) . . . . ?
C8 Os1 P1 C3 -19.8(7) . . . . ?
Cl2 Os1 P1 C3 149.5(3) . . . . ?
Cl1 Os1 P1 C3 62.8(3) . . . . ?
C11 Os1 P1 C1 35.0(3) . . . . ?
C12 Os1 P1 C1 72.8(3) . . . . ?
C10 Os1 P1 C1 2.9(3) . . . . ?
C9 Os1 P1 C1 -9.0(5) . . . . ?
C7 Os1 P1 C1 100.5(3) . . . . ?
C8 Os1 P1 C1 100.2(6) . . . . ?
Cl2 Os1 P1 C1 -90.5(3) . . . . ?
Cl1 Os1 P1 C1 -177.2(3) . . . . ?
C11 Os1 P1 C2 157.9(3) . . . . ?
C12 Os1 P1 C2 -164.2(3) . . . . ?
C10 Os1 P1 C2 125.9(3) . . . . ?
C9 Os1 P1 C2 113.9(4) . . . . ?
C7 Os1 P1 C2 -136.6(3) . . . . ?
C8 Os1 P1 C2 -136.8(6) . . . . ?
Cl2 Os1 P1 C2 32.5(3) . . . . ?
Cl1 Os1 P1 C2 -54.2(3) . . . . ?
C6 N1 C1 P1 60.7(6) . . . . ?
C4 N1 C1 P1 -61.8(6) . . . . ?
C3 P1 C1 N1 -49.2(5) . . . . ?
C2 P1 C1 N1 50.8(5) . . . . ?
Os1 P1 C1 N1 -176.8(4) . . . . ?
C5 N2 C2 P1 -60.2(6) . . . . ?
C4 N2 C2 P1 61.3(6) . . . . ?
C3 P1 C2 N2 49.4(5) . . . . ?
C1 P1 C2 N2 -50.9(5) . . . . ?
Os1 P1 C2 N2 174.8(3) . . . . ?
C6 N3 C3 P1 -60.9(6) . . . . ?
C5 N3 C3 P1 60.7(6) . . . . ?
C1 P1 C3 N3 49.6(5) . . . . ?
C2 P1 C3 N3 -49.9(5) . . . . ?
Os1 P1 C3 N3 -178.1(4) . . . . ?
C1 N1 C4 N2 67.4(7) . . . . ?
C6 N1 C4 N2 -56.7(7) . . . . ?
C5 N2 C4 N1 56.8(7) . . . . ?
C2 N2 C4 N1 -66.9(7) . . . . ?
C2 N2 C5 N3 67.8(7) . . . . ?
C4 N2 C5 N3 -55.7(7) . . . . ?
C6 N3 C5 N2 54.6(7) . . . . ?
C3 N3 C5 N2 -67.6(7) . . . . ?
C5 N3 C6 N1 -53.8(7) . . . . ?
C3 N3 C6 N1 68.7(7) . . . . ?
C1 N1 C6 N3 -69.4(7) . . . . ?
C4 N1 C6 N3 55.2(7) . . . . ?
C11 Os1 C7 C12 28.3(4) . . . . ?
C10 Os1 C7 C12 65.7(4) . . . . ?
C9 Os1 C7 C12 102.6(4) . . . . ?
C8 Os1 C7 C12 130.4(6) . . . . ?
P1 Os1 C7 C12 -49.5(4) . . . . ?
Cl2 Os1 C7 C12 150.5(3) . . . . ?
Cl1 Os1 C7 C12 -128.2(4) . . . . ?
C11 Os1 C7 C8 -102.0(4) . . . . ?
C12 Os1 C7 C8 -130.4(6) . . . . ?
C10 Os1 C7 C8 -64.7(4) . . . . ?
C9 Os1 C7 C8 -27.8(4) . . . . ?
P1 Os1 C7 C8 -179.9(3) . . . . ?
Cl2 Os1 C7 C8 20.2(6) . . . . ?
Cl1 Os1 C7 C8 101.4(4) . . . . ?
C11 Os1 C7 C13 142.5(7) . . . . ?
C12 Os1 C7 C13 114.2(8) . . . . ?
C10 Os1 C7 C13 179.9(7) . . . . ?
C9 Os1 C7 C13 -143.2(7) . . . . ?
C8 Os1 C7 C13 -115.4(8) . . . . ?
P1 Os1 C7 C13 64.7(7) . . . . ?
Cl2 Os1 C7 C13 -95.3(7) . . . . ?
Cl1 Os1 C7 C13 -14.0(6) . . . . ?
C12 C7 C8 C9 -2.7(9) . . . . ?
C13 C7 C8 C9 177.6(6) . . . . ?
Os1 C7 C8 C9 52.2(5) . . . . ?
C12 C7 C8 Os1 -54.9(5) . . . . ?
C13 C7 C8 Os1 125.4(6) . . . . ?
C11 Os1 C8 C9 -66.3(4) . . . . ?
C12 Os1 C8 C9 -103.7(4) . . . . ?
C10 Os1 C8 C9 -28.5(3) . . . . ?
C7 Os1 C8 C9 -133.8(6) . . . . ?
P1 Os1 C8 C9 -133.4(5) . . . . ?
Cl2 Os1 C8 C9 58.0(4) . . . . ?
Cl1 Os1 C8 C9 146.2(3) . . . . ?
C11 Os1 C8 C7 67.5(4) . . . . ?
C12 Os1 C8 C7 30.1(4) . . . . ?
C10 Os1 C8 C7 105.2(4) . . . . ?
C9 Os1 C8 C7 133.8(6) . . . . ?
P1 Os1 C8 C7 0.3(8) . . . . ?
Cl2 Os1 C8 C7 -168.2(3) . . . . ?
Cl1 Os1 C8 C7 -80.1(4) . . . . ?
C7 C8 C9 C10 0.6(9) . . . . ?
Os1 C8 C9 C10 52.7(5) . . . . ?
C7 C8 C9 Os1 -52.1(5) . . . . ?
C11 Os1 C9 C8 103.4(4) . . . . ?
C12 Os1 C9 C8 65.3(4) . . . . ?
C10 Os1 C9 C8 134.2(5) . . . . ?
C7 Os1 C9 C8 28.4(4) . . . . ?
P1 Os1 C9 C8 151.8(3) . . . . ?
Cl2 Os1 C9 C8 -127.3(4) . . . . ?
Cl1 Os1 C9 C8 -42.5(4) . . . . ?
C11 Os1 C9 C10 -30.8(4) . . . . ?
C12 Os1 C9 C10 -68.9(4) . . . . ?
C7 Os1 C9 C10 -105.8(4) . . . . ?
C8 Os1 C9 C10 -134.2(5) . . . . ?
P1 Os1 C9 C10 17.7(6) . . . . ?
Cl2 Os1 C9 C10 98.6(3) . . . . ?
Cl1 Os1 C9 C10 -176.7(3) . . . . ?
C8 C9 C10 C11 0.3(9) . . . . ?
Os1 C9 C10 C11 54.0(5) . . . . ?
C8 C9 C10 C14 177.2(6) . . . . ?
Os1 C9 C10 C14 -129.0(6) . . . . ?
C8 C9 C10 Os1 -53.7(5) . . . . ?
C12 Os1 C10 C11 -29.8(4) . . . . ?
C9 Os1 C10 C11 -129.8(5) . . . . ?
C7 Os1 C10 C11 -66.1(4) . . . . ?
C8 Os1 C10 C11 -102.4(4) . . . . ?
P1 Os1 C10 C11 59.1(4) . . . . ?
Cl2 Os1 C10 C11 147.6(3) . . . . ?
Cl1 Os1 C10 C11 -120.5(5) . . . . ?
C11 Os1 C10 C9 129.8(5) . . . . ?
C12 Os1 C10 C9 100.0(4) . . . . ?
C7 Os1 C10 C9 63.7(4) . . . . ?
C8 Os1 C10 C9 27.4(4) . . . . ?
P1 Os1 C10 C9 -171.2(3) . . . . ?
Cl2 Os1 C10 C9 -82.6(4) . . . . ?
Cl1 Os1 C10 C9 9.3(8) . . . . ?
C11 Os1 C10 C14 -116.1(8) . . . . ?
C12 Os1 C10 C14 -145.9(7) . . . . ?
C9 Os1 C10 C14 114.1(8) . . . . ?
C7 Os1 C10 C14 177.8(7) . . . . ?
C8 Os1 C10 C14 141.5(7) . . . . ?
P1 Os1 C10 C14 -57.0(7) . . . . ?
Cl2 Os1 C10 C14 31.5(6) . . . . ?
Cl1 Os1 C10 C14 123.4(6) . . . . ?
C9 C10 C11 C12 0.9(8) . . . . ?
C14 C10 C11 C12 -176.0(6) . . . . ?
Os1 C10 C11 C12 56.0(5) . . . . ?
C9 C10 C11 Os1 -55.0(5) . . . . ?
C14 C10 C11 Os1 128.1(6) . . . . ?
C10 Os1 C11 C12 -131.5(5) . . . . ?
C9 Os1 C11 C12 -100.7(4) . . . . ?
C7 Os1 C11 C12 -27.7(4) . . . . ?
C8 Os1 C11 C12 -64.8(4) . . . . ?
P1 Os1 C11 C12 99.3(4) . . . . ?
Cl2 Os1 C11 C12 -172.5(3) . . . . ?
Cl1 Os1 C11 C12 20.1(5) . . . . ?
C12 Os1 C11 C10 131.5(5) . . . . ?
C9 Os1 C11 C10 30.7(4) . . . . ?
C7 Os1 C11 C10 103.7(4) . . . . ?
C8 Os1 C11 C10 66.7(4) . . . . ?
P1 Os1 C11 C10 -129.2(3) . . . . ?
Cl2 Os1 C11 C10 -41.0(4) . . . . ?
Cl1 Os1 C11 C10 151.6(3) . . . . ?
C8 C7 C12 C11 3.9(9) . . . . ?
C13 C7 C12 C11 -176.4(6) . . . . ?
Os1 C7 C12 C11 -51.9(5) . . . . ?
C8 C7 C12 Os1 55.8(5) . . . . ?
C13 C7 C12 Os1 -124.6(6) . . . . ?
C10 C11 C12 C7 -3.0(9) . . . . ?
Os1 C11 C12 C7 53.0(5) . . . . ?
C10 C11 C12 Os1 -56.1(5) . . . . ?
C11 Os1 C12 C7 -134.2(6) . . . . ?
C10 Os1 C12 C7 -104.4(4) . . . . ?
C9 Os1 C12 C7 -66.2(4) . . . . ?
C8 Os1 C12 C7 -30.2(4) . . . . ?
P1 Os1 C12 C7 141.2(4) . . . . ?
Cl2 Os1 C12 C7 -113.3(6) . . . . ?
Cl1 Os1 C12 C7 57.1(4) . . . . ?
C10 Os1 C12 C11 29.8(4) . . . . ?
C9 Os1 C12 C11 68.0(4) . . . . ?
C7 Os1 C12 C11 134.2(6) . . . . ?
C8 Os1 C12 C11 104.0(4) . . . . ?
P1 Os1 C12 C11 -84.5(4) . . . . ?
Cl2 Os1 C12 C11 21.0(8) . . . . ?
Cl1 Os1 C12 C11 -168.6(3) . . . . ?
C11 C10 C14 C16 -52.0(9) . . . . ?
C9 C10 C14 C16 131.2(6) . . . . ?
Os1 C10 C14 C16 39.3(9) . . . . ?
C11 C10 C14 C15 72.0(8) . . . . ?
C9 C10 C14 C15 -104.8(7) . . . . ?
Os1 C10 C14 C15 163.3(5) . . . . ?
|
1100808.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 08:41:18 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180562 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100808.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100808
loop_
_publ_author_name
'Dorcier, Antoine'
'Dyson, Paul J.'
'Gossens, Christian'
'Rothlisberger, Ursula'
'Scopelliti, Rosario'
'Tavernelli, Ivano'
_publ_section_title
;
Binding of Organometallic Ruthenium(II) and Osmium(II) Complexes to
an Oligonucleotide: A Combined Mass Spectrometric and Theoretical Study
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2114
_journal_page_last 2123
_journal_paper_doi 10.1021/om049022a
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C17 H29 Cl2 N3 Os P, 0.5(C H4 O), Cl'
_chemical_formula_sum 'C17.5 H31 Cl3 N3 O0.5 Os P'
_chemical_formula_weight 618.97
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 113.142(14)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.5918(20)
_cell_length_b 10.7345(9)
_cell_length_c 16.442(2)
_cell_measurement_reflns_used 3519
_cell_measurement_temperature 140(2)
_cell_measurement_theta_max 21.63555
_cell_measurement_theta_min 2.32765
_cell_volume 2205.9(5)
_computing_cell_refinement 'Oxford Diffraction, CrysAlis RED'
_computing_data_collection 'Oxford Diffraction, CrysAlis CCD'
_computing_data_reduction 'Oxford Diffraction, CrysAlis RED'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 140(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type 'Oxford Diffraction, KM4/Sapphire CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0772
_diffrn_reflns_av_sigmaI/netI 0.0625
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 12057
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 3.17
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 6.227
_exptl_absorpt_correction_T_max 0.685
_exptl_absorpt_correction_T_min 0.220
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.864
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 1212
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.11
_refine_diff_density_max 4.421
_refine_diff_density_min -2.583
_refine_diff_density_rms 0.268
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.196
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 3764
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.195
_refine_ls_R_factor_all 0.0865
_refine_ls_R_factor_gt 0.0774
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+99.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1656
_refine_ls_wR_factor_ref 0.1700
_reflns_number_gt 3220
_reflns_number_total 3764
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060317
_cod_data_source_file om049022asi20041210_041724.cif
_cod_data_source_block 4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_original_formula_sum 'C17.50 H31 Cl3 N3 O0.50 Os P'
_cod_database_code 1100808
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.16908(4) 0.05850(6) 0.35360(4) 0.0234(2) Uani 1 1 d . . .
Cl1 Cl 0.1789(3) -0.1522(4) 0.3023(3) 0.0341(9) Uani 1 1 d . . .
Cl2 Cl -0.0012(3) -0.0052(4) 0.3572(3) 0.0326(9) Uani 1 1 d . . .
P1 P 0.2443(3) -0.0424(4) 0.4888(2) 0.0244(8) Uani 1 1 d . . .
N1 N 0.3040(10) -0.0351(14) 0.6719(8) 0.031(3) Uani 1 1 d . . .
N2 N 0.2544(11) -0.2409(15) 0.5992(9) 0.036(3) Uani 1 1 d . . .
N3 N 0.4255(11) -0.1453(15) 0.6152(9) 0.040(4) Uani 1 1 d . . .
C1 C 0.2469(12) 0.0419(16) 0.5884(9) 0.027(4) Uani 1 1 d . . .
H1A H 0.2842 0.1226 0.5936 0.033 Uiso 1 1 calc R . .
H1B H 0.1727 0.0594 0.5821 0.033 Uiso 1 1 calc R . .
C2 C 0.1893(14) -0.1912(17) 0.5070(11) 0.038(4) Uani 1 1 d . . .
H2A H 0.1141 -0.1792 0.4998 0.046 Uiso 1 1 calc R . .
H2B H 0.1901 -0.2526 0.4623 0.046 Uiso 1 1 calc R . .
C3 C 0.3880(12) -0.0787(18) 0.5286(10) 0.035(4) Uani 1 1 d . . .
H3A H 0.4012 -0.1314 0.4845 0.041 Uiso 1 1 calc R . .
H3B H 0.4291 -0.0005 0.5353 0.041 Uiso 1 1 calc R . .
C4 C 0.2487(13) -0.1614(17) 0.6678(11) 0.034(4) Uani 1 1 d . . .
H4A H 0.2829 -0.2040 0.7256 0.041 Uiso 1 1 calc R . .
H4B H 0.1727 -0.1470 0.6571 0.041 Uiso 1 1 calc R . .
C5 C 0.3682(14) -0.2621(18) 0.6141(11) 0.039(4) Uani 1 1 d . . .
H5A H 0.4045 -0.3058 0.6711 0.047 Uiso 1 1 calc R . .
H5B H 0.3715 -0.3167 0.5667 0.047 Uiso 1 1 calc R . .
C6 C 0.4211(12) -0.0627(18) 0.6834(10) 0.034(4) Uani 1 1 d . . .
H6A H 0.4572 0.0166 0.6815 0.041 Uiso 1 1 calc R . .
H6B H 0.4601 -0.1012 0.7421 0.041 Uiso 1 1 calc R . .
C7 C 0.3074(16) 0.0346(19) 0.7519(11) 0.045(5) Uani 1 1 d . . .
H7A H 0.2344 0.0465 0.7484 0.068 Uiso 1 1 calc R . .
H7B H 0.3412 0.1159 0.7543 0.068 Uiso 1 1 calc R . .
H7C H 0.3489 -0.0131 0.8052 0.068 Uiso 1 1 calc R . .
C8 C 0.2309(13) 0.1264(16) 0.2532(11) 0.031(4) Uani 1 1 d . . .
C9 C 0.1231(12) 0.1711(17) 0.2281(10) 0.030(4) Uani 1 1 d . . .
H9 H 0.0706 0.1555 0.1705 0.036 Uiso 1 1 calc R . .
C10 C 0.0965(13) 0.2382(16) 0.2901(10) 0.032(4) Uani 1 1 d . . .
H10 H 0.0250 0.2671 0.2726 0.038 Uiso 1 1 calc R . .
C11 C 0.1703(11) 0.2654(14) 0.3775(9) 0.023(3) Uani 1 1 d . . .
C12 C 0.2794(13) 0.2171(16) 0.4034(11) 0.033(4) Uani 1 1 d . . .
H12 H 0.3306 0.2315 0.4617 0.040 Uiso 1 1 calc R . .
C13 C 0.3104(12) 0.1473(14) 0.3411(11) 0.027(3) Uani 1 1 d . . .
H13 H 0.3812 0.1164 0.3579 0.033 Uiso 1 1 calc R . .
C14 C 0.2642(16) 0.0470(19) 0.1905(12) 0.043(4) Uani 1 1 d . . .
H14A H 0.2001 0.0149 0.1424 0.065 Uiso 1 1 calc R . .
H14B H 0.3084 -0.0229 0.2234 0.065 Uiso 1 1 calc R . .
H14C H 0.3053 0.0983 0.1658 0.065 Uiso 1 1 calc R . .
C15 C 0.1460(14) 0.3433(15) 0.4432(11) 0.032(4) Uani 1 1 d . . .
H15 H 0.2032 0.3266 0.5029 0.039 Uiso 1 1 calc R . .
C16 C 0.1549(15) 0.4836(18) 0.4207(13) 0.044(5) Uani 1 1 d . . .
H16A H 0.2304 0.5060 0.4387 0.067 Uiso 1 1 calc R . .
H16B H 0.1226 0.5359 0.4525 0.067 Uiso 1 1 calc R . .
H16C H 0.1172 0.4967 0.3569 0.067 Uiso 1 1 calc R . .
C17 C 0.0381(15) 0.311(2) 0.4475(13) 0.047(5) Uani 1 1 d . . .
H17A H -0.0176 0.3080 0.3875 0.071 Uiso 1 1 calc R . .
H17B H 0.0198 0.3743 0.4821 0.071 Uiso 1 1 calc R . .
H17C H 0.0432 0.2293 0.4758 0.071 Uiso 1 1 calc R . .
Cl3 Cl 0.4742(5) 0.2389(5) 0.6297(3) 0.0580(14) Uani 1 1 d . . .
O1 O 0.593(2) 0.403(3) 0.5555(16) 0.052(8) Uani 0.50 1 d P A -1
H1 H 0.5864 0.3854 0.6029 0.079 Uiso 0.50 1 calc PR A -1
C18 C 0.522(6) 0.486(8) 0.513(4) 0.079(19) Uani 0.50 1 d PU A -1
H18A H 0.5464 0.5679 0.5390 0.118 Uiso 0.50 1 calc PR A -1
H18B H 0.4541 0.4652 0.5167 0.118 Uiso 0.50 1 calc PR A -1
H18C H 0.5134 0.4863 0.4508 0.118 Uiso 0.50 1 calc PR A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.0211(3) 0.0271(4) 0.0216(3) -0.0012(3) 0.0080(2) -0.0003(3)
Cl1 0.039(2) 0.030(2) 0.035(2) -0.0067(17) 0.0178(17) 0.0011(18)
Cl2 0.0236(18) 0.031(2) 0.046(2) -0.0003(18) 0.0159(17) -0.0013(17)
P1 0.0231(19) 0.027(2) 0.0242(18) 0.0045(16) 0.0103(15) -0.0004(17)
N1 0.029(7) 0.042(9) 0.024(6) 0.004(6) 0.012(5) -0.005(6)
N2 0.032(7) 0.041(9) 0.033(7) 0.011(7) 0.010(6) -0.007(7)
N3 0.032(8) 0.052(11) 0.038(8) 0.016(7) 0.015(6) 0.012(7)
C1 0.030(8) 0.037(10) 0.020(7) 0.011(7) 0.015(6) 0.011(7)
C2 0.037(9) 0.032(11) 0.040(9) 0.008(8) 0.010(8) -0.002(8)
C3 0.027(8) 0.045(11) 0.029(8) 0.005(8) 0.007(7) 0.005(8)
C4 0.032(9) 0.035(10) 0.042(9) 0.017(8) 0.021(7) 0.000(8)
C5 0.044(10) 0.039(11) 0.036(9) 0.007(8) 0.017(8) 0.013(9)
C6 0.025(8) 0.047(11) 0.025(7) 0.013(8) 0.005(6) 0.010(8)
C7 0.063(12) 0.049(13) 0.027(8) -0.001(8) 0.021(8) 0.010(10)
C8 0.043(10) 0.028(9) 0.037(9) -0.004(7) 0.032(8) -0.004(8)
C9 0.019(7) 0.039(10) 0.026(8) 0.003(7) 0.001(6) 0.008(7)
C10 0.032(9) 0.028(10) 0.035(9) 0.011(7) 0.013(7) 0.008(7)
C11 0.018(7) 0.011(8) 0.032(8) -0.001(6) 0.001(6) -0.007(6)
C12 0.038(9) 0.027(10) 0.034(8) -0.001(7) 0.013(7) -0.021(8)
C13 0.028(8) 0.015(8) 0.046(9) 0.001(7) 0.022(7) -0.009(6)
C14 0.058(12) 0.040(12) 0.041(9) -0.011(9) 0.030(9) -0.005(10)
C15 0.046(10) 0.017(9) 0.038(9) 0.000(7) 0.022(8) -0.003(7)
C16 0.049(11) 0.035(11) 0.064(12) -0.015(9) 0.038(10) 0.000(9)
C17 0.051(11) 0.049(13) 0.056(11) -0.017(10) 0.037(10) -0.013(10)
Cl3 0.076(4) 0.049(3) 0.032(2) -0.007(2) 0.003(2) -0.020(3)
O1 0.047(15) 0.07(2) 0.032(13) -0.003(14) 0.006(12) -0.019(15)
C18 0.10(6) 0.11(5) 0.02(3) 0.04(3) 0.02(3) 0.03(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Os1 C13 38.5(6) . . ?
C12 Os1 C10 67.5(6) . . ?
C13 Os1 C10 79.9(6) . . ?
C12 Os1 C8 68.1(6) . . ?
C13 Os1 C8 37.6(6) . . ?
C10 Os1 C8 66.4(6) . . ?
C12 Os1 C11 38.4(6) . . ?
C13 Os1 C11 69.3(6) . . ?
C10 Os1 C11 37.0(6) . . ?
C8 Os1 C11 80.2(6) . . ?
C12 Os1 C9 80.2(6) . . ?
C13 Os1 C9 68.0(6) . . ?
C10 Os1 C9 36.5(6) . . ?
C8 Os1 C9 37.3(6) . . ?
C11 Os1 C9 67.2(6) . . ?
C12 Os1 P1 91.4(4) . . ?
C13 Os1 P1 102.6(4) . . ?
C10 Os1 P1 143.2(4) . . ?
C8 Os1 P1 134.8(5) . . ?
C11 Os1 P1 108.8(4) . . ?
C9 Os1 P1 170.4(4) . . ?
C12 Os1 Cl2 136.2(5) . . ?
C13 Os1 Cl2 170.2(4) . . ?
C10 Os1 Cl2 90.2(4) . . ?
C8 Os1 Cl2 137.9(5) . . ?
C11 Os1 Cl2 102.4(4) . . ?
C9 Os1 Cl2 104.3(4) . . ?
P1 Os1 Cl2 84.89(14) . . ?
C12 Os1 Cl1 136.4(5) . . ?
C13 Os1 Cl1 101.4(4) . . ?
C10 Os1 Cl1 135.6(4) . . ?
C8 Os1 Cl1 87.7(4) . . ?
C11 Os1 Cl1 167.8(4) . . ?
C9 Os1 Cl1 102.3(5) . . ?
P1 Os1 Cl1 80.50(14) . . ?
Cl2 Os1 Cl1 85.99(14) . . ?
C2 P1 C3 101.6(8) . . ?
C2 P1 C1 98.5(8) . . ?
C3 P1 C1 98.0(7) . . ?
C2 P1 Os1 120.5(6) . . ?
C3 P1 Os1 116.5(5) . . ?
C1 P1 Os1 117.8(5) . . ?
C7 N1 C1 110.4(13) . . ?
C7 N1 C4 109.0(13) . . ?
C1 N1 C4 111.7(12) . . ?
C7 N1 C6 108.1(13) . . ?
C1 N1 C6 110.3(11) . . ?
C4 N1 C6 107.2(13) . . ?
C4 N2 C5 109.6(13) . . ?
C4 N2 C2 112.6(14) . . ?
C5 N2 C2 112.2(13) . . ?
C6 N3 C5 110.4(13) . . ?
C6 N3 C3 110.0(14) . . ?
C5 N3 C3 114.5(14) . . ?
N1 C1 P1 110.8(11) . . ?
N1 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 P1 110.6(12) . . ?
N2 C2 H2A 109.5 . . ?
P1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N3 C3 P1 111.0(11) . . ?
N3 C3 H3A 109.4 . . ?
P1 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
P1 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N2 C4 N1 112.4(12) . . ?
N2 C4 H4A 109.1 . . ?
N1 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
N1 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
N3 C5 N2 112.5(14) . . ?
N3 C5 H5A 109.1 . . ?
N2 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
N2 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N3 C6 N1 112.0(13) . . ?
N3 C6 H6A 109.2 . . ?
N1 C6 H6A 109.2 . . ?
N3 C6 H6B 109.2 . . ?
N1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 120.9(14) . . ?
C9 C8 C14 121.8(15) . . ?
C13 C8 C14 117.1(15) . . ?
C9 C8 Os1 71.7(9) . . ?
C13 C8 Os1 70.4(8) . . ?
C14 C8 Os1 127.4(12) . . ?
C10 C9 C8 119.0(14) . . ?
C10 C9 Os1 70.7(9) . . ?
C8 C9 Os1 71.0(9) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
Os1 C9 H9 130.3 . . ?
C9 C10 C11 123.8(15) . . ?
C9 C10 Os1 72.8(10) . . ?
C11 C10 Os1 72.4(9) . . ?
C9 C10 H10 118.1 . . ?
C11 C10 H10 118.1 . . ?
Os1 C10 H10 129.5 . . ?
C10 C11 C12 116.9(14) . . ?
C10 C11 C15 125.0(14) . . ?
C12 C11 C15 118.1(13) . . ?
C10 C11 Os1 70.6(9) . . ?
C12 C11 Os1 68.9(9) . . ?
C15 C11 Os1 133.3(11) . . ?
C13 C12 C11 121.0(14) . . ?
C13 C12 Os1 71.6(8) . . ?
C11 C12 Os1 72.7(8) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
Os1 C12 H12 128.5 . . ?
C8 C13 C12 118.3(14) . . ?
C8 C13 Os1 72.0(8) . . ?
C12 C13 Os1 69.9(8) . . ?
C8 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
Os1 C13 H13 129.5 . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 113.0(14) . . ?
C11 C15 C16 107.9(13) . . ?
C17 C15 C16 113.1(15) . . ?
C11 C15 H15 107.5 . . ?
C17 C15 H15 107.5 . . ?
C16 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 O1 H1 109.5 . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C12 2.203(15) . ?
Os1 C13 2.226(14) . ?
Os1 C10 2.230(16) . ?
Os1 C8 2.247(14) . ?
Os1 C11 2.254(15) . ?
Os1 C9 2.257(16) . ?
Os1 P1 2.318(4) . ?
Os1 Cl2 2.436(4) . ?
Os1 Cl1 2.436(4) . ?
P1 C2 1.838(18) . ?
P1 C3 1.842(16) . ?
P1 C1 1.859(15) . ?
N1 C7 1.50(2) . ?
N1 C1 1.527(18) . ?
N1 C4 1.54(2) . ?
N1 C6 1.556(19) . ?
N2 C4 1.44(2) . ?
N2 C5 1.49(2) . ?
N2 C2 1.52(2) . ?
N3 C6 1.45(2) . ?
N3 C5 1.47(2) . ?
N3 C3 1.49(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.44(2) . ?
C8 C13 1.44(2) . ?
C8 C14 1.54(2) . ?
C9 C10 1.41(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.42(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.47(2) . ?
C11 C15 1.50(2) . ?
C12 C13 1.46(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.54(2) . ?
C15 C16 1.57(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O1 C18 1.29(6) . ?
O1 H1 0.8400 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl3 0.84 2.35 2.96(3) 129.7 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 Os1 P1 C2 176.7(9) . . . . ?
C13 Os1 P1 C2 -146.1(8) . . . . ?
C10 Os1 P1 C2 123.9(10) . . . . ?
C8 Os1 P1 C2 -123.4(9) . . . . ?
C11 Os1 P1 C2 141.7(8) . . . . ?
C9 Os1 P1 C2 -154(3) . . . . ?
Cl2 Os1 P1 C2 40.4(7) . . . . ?
Cl1 Os1 P1 C2 -46.4(7) . . . . ?
C12 Os1 P1 C3 -59.7(8) . . . . ?
C13 Os1 P1 C3 -22.5(8) . . . . ?
C10 Os1 P1 C3 -112.4(10) . . . . ?
C8 Os1 P1 C3 0.2(9) . . . . ?
C11 Os1 P1 C3 -94.6(8) . . . . ?
C9 Os1 P1 C3 -31(3) . . . . ?
Cl2 Os1 P1 C3 164.0(7) . . . . ?
Cl1 Os1 P1 C3 77.2(7) . . . . ?
C12 Os1 P1 C1 56.3(8) . . . . ?
C13 Os1 P1 C1 93.6(7) . . . . ?
C10 Os1 P1 C1 3.6(10) . . . . ?
C8 Os1 P1 C1 116.2(8) . . . . ?
C11 Os1 P1 C1 21.4(7) . . . . ?
C9 Os1 P1 C1 85(3) . . . . ?
Cl2 Os1 P1 C1 -80.0(6) . . . . ?
Cl1 Os1 P1 C1 -166.7(6) . . . . ?
C7 N1 C1 P1 179.0(11) . . . . ?
C4 N1 C1 P1 -59.6(14) . . . . ?
C6 N1 C1 P1 59.5(15) . . . . ?
C2 P1 C1 N1 51.6(12) . . . . ?
C3 P1 C1 N1 -51.4(12) . . . . ?
Os1 P1 C1 N1 -177.1(8) . . . . ?
C4 N2 C2 P1 64.5(16) . . . . ?
C5 N2 C2 P1 -59.7(18) . . . . ?
C3 P1 C2 N2 47.5(14) . . . . ?
C1 P1 C2 N2 -52.6(13) . . . . ?
Os1 P1 C2 N2 178.0(9) . . . . ?
C6 N3 C3 P1 -67.3(16) . . . . ?
C5 N3 C3 P1 57.7(17) . . . . ?
C2 P1 C3 N3 -46.1(14) . . . . ?
C1 P1 C3 N3 54.4(14) . . . . ?
Os1 P1 C3 N3 -179.0(10) . . . . ?
C5 N2 C4 N1 58.2(17) . . . . ?
C2 N2 C4 N1 -67.4(17) . . . . ?
C7 N1 C4 N2 -172.5(14) . . . . ?
C1 N1 C4 N2 65.2(16) . . . . ?
C6 N1 C4 N2 -55.7(16) . . . . ?
C6 N3 C5 N2 58.1(17) . . . . ?
C3 N3 C5 N2 -66.7(18) . . . . ?
C4 N2 C5 N3 -58.7(17) . . . . ?
C2 N2 C5 N3 67.1(19) . . . . ?
C5 N3 C6 N1 -56.5(17) . . . . ?
C3 N3 C6 N1 70.9(17) . . . . ?
C7 N1 C6 N3 171.7(14) . . . . ?
C1 N1 C6 N3 -67.5(18) . . . . ?
C4 N1 C6 N3 54.4(16) . . . . ?
C12 Os1 C8 C9 -103.1(11) . . . . ?
C13 Os1 C8 C9 -133.8(14) . . . . ?
C10 Os1 C8 C9 -29.0(10) . . . . ?
C11 Os1 C8 C9 -65.0(10) . . . . ?
P1 Os1 C8 C9 -171.9(8) . . . . ?
Cl2 Os1 C8 C9 32.6(12) . . . . ?
Cl1 Os1 C8 C9 114.0(9) . . . . ?
C12 Os1 C8 C13 30.7(9) . . . . ?
C10 Os1 C8 C13 104.8(11) . . . . ?
C11 Os1 C8 C13 68.7(9) . . . . ?
C9 Os1 C8 C13 133.8(14) . . . . ?
P1 Os1 C8 C13 -38.1(12) . . . . ?
Cl2 Os1 C8 C13 166.4(7) . . . . ?
Cl1 Os1 C8 C13 -112.2(9) . . . . ?
C12 Os1 C8 C14 140.4(17) . . . . ?
C13 Os1 C8 C14 109.7(19) . . . . ?
C10 Os1 C8 C14 -145.6(17) . . . . ?
C11 Os1 C8 C14 178.4(16) . . . . ?
C9 Os1 C8 C14 -116.5(19) . . . . ?
P1 Os1 C8 C14 71.6(16) . . . . ?
Cl2 Os1 C8 C14 -83.9(16) . . . . ?
Cl1 Os1 C8 C14 -2.6(15) . . . . ?
C13 C8 C9 C10 1(2) . . . . ?
C14 C8 C9 C10 176.9(16) . . . . ?
Os1 C8 C9 C10 53.8(14) . . . . ?
C13 C8 C9 Os1 -52.5(14) . . . . ?
C14 C8 C9 Os1 123.2(16) . . . . ?
C12 Os1 C9 C10 -65.2(10) . . . . ?
C13 Os1 C9 C10 -103.3(11) . . . . ?
C8 Os1 C9 C10 -131.6(15) . . . . ?
C11 Os1 C9 C10 -27.4(9) . . . . ?
P1 Os1 C9 C10 -94(3) . . . . ?
Cl2 Os1 C9 C10 70.2(10) . . . . ?
Cl1 Os1 C9 C10 159.2(9) . . . . ?
C12 Os1 C9 C8 66.5(10) . . . . ?
C13 Os1 C9 C8 28.4(9) . . . . ?
C10 Os1 C9 C8 131.6(15) . . . . ?
C11 Os1 C9 C8 104.3(10) . . . . ?
P1 Os1 C9 C8 37(3) . . . . ?
Cl2 Os1 C9 C8 -158.1(9) . . . . ?
Cl1 Os1 C9 C8 -69.1(9) . . . . ?
C8 C9 C10 C11 0(3) . . . . ?
Os1 C9 C10 C11 53.9(15) . . . . ?
C8 C9 C10 Os1 -53.9(14) . . . . ?
C12 Os1 C10 C9 104.5(11) . . . . ?
C13 Os1 C10 C9 66.4(10) . . . . ?
C8 Os1 C10 C9 29.6(9) . . . . ?
C11 Os1 C10 C9 135.2(14) . . . . ?
P1 Os1 C10 C9 164.0(7) . . . . ?
Cl2 Os1 C10 C9 -114.2(9) . . . . ?
Cl1 Os1 C10 C9 -29.7(12) . . . . ?
C12 Os1 C10 C11 -30.7(9) . . . . ?
C13 Os1 C10 C11 -68.8(9) . . . . ?
C8 Os1 C10 C11 -105.6(10) . . . . ?
C9 Os1 C10 C11 -135.2(14) . . . . ?
P1 Os1 C10 C11 28.7(13) . . . . ?
Cl2 Os1 C10 C11 110.5(9) . . . . ?
Cl1 Os1 C10 C11 -165.0(7) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
Os1 C10 C11 C12 52.7(12) . . . . ?
C9 C10 C11 C15 176.1(16) . . . . ?
Os1 C10 C11 C15 -129.8(15) . . . . ?
C9 C10 C11 Os1 -54.1(15) . . . . ?
C12 Os1 C11 C10 130.5(13) . . . . ?
C13 Os1 C11 C10 101.0(10) . . . . ?
C8 Os1 C11 C10 63.6(10) . . . . ?
C9 Os1 C11 C10 27.0(9) . . . . ?
P1 Os1 C11 C10 -162.3(8) . . . . ?
Cl2 Os1 C11 C10 -73.5(9) . . . . ?
Cl1 Os1 C11 C10 59(2) . . . . ?
C13 Os1 C11 C12 -29.5(9) . . . . ?
C10 Os1 C11 C12 -130.5(13) . . . . ?
C8 Os1 C11 C12 -66.9(9) . . . . ?
C9 Os1 C11 C12 -103.5(10) . . . . ?
P1 Os1 C11 C12 67.2(9) . . . . ?
Cl2 Os1 C11 C12 156.0(8) . . . . ?
Cl1 Os1 C11 C12 -71(2) . . . . ?
C12 Os1 C11 C15 -109.3(17) . . . . ?
C13 Os1 C11 C15 -138.8(16) . . . . ?
C10 Os1 C11 C15 120.2(18) . . . . ?
C8 Os1 C11 C15 -176.2(15) . . . . ?
C9 Os1 C11 C15 147.3(16) . . . . ?
P1 Os1 C11 C15 -42.0(15) . . . . ?
Cl2 Os1 C11 C15 46.7(15) . . . . ?
Cl1 Os1 C11 C15 179.2(12) . . . . ?
C10 C11 C12 C13 1(2) . . . . ?
C15 C11 C12 C13 -176.2(14) . . . . ?
Os1 C11 C12 C13 55.0(13) . . . . ?
C10 C11 C12 Os1 -53.5(12) . . . . ?
C15 C11 C12 Os1 128.8(13) . . . . ?
C10 Os1 C12 C13 -102.6(10) . . . . ?
C8 Os1 C12 C13 -30.0(9) . . . . ?
C11 Os1 C12 C13 -132.3(13) . . . . ?
C9 Os1 C12 C13 -66.8(10) . . . . ?
P1 Os1 C12 C13 108.5(9) . . . . ?
Cl2 Os1 C12 C13 -167.4(7) . . . . ?
Cl1 Os1 C12 C13 30.8(12) . . . . ?
C13 Os1 C12 C11 132.3(13) . . . . ?
C10 Os1 C12 C11 29.7(9) . . . . ?
C8 Os1 C12 C11 102.3(10) . . . . ?
C9 Os1 C12 C11 65.5(9) . . . . ?
P1 Os1 C12 C11 -119.2(8) . . . . ?
Cl2 Os1 C12 C11 -35.1(11) . . . . ?
Cl1 Os1 C12 C11 163.1(7) . . . . ?
C9 C8 C13 C12 -1(2) . . . . ?
C14 C8 C13 C12 -177.0(14) . . . . ?
Os1 C8 C13 C12 -54.2(12) . . . . ?
C9 C8 C13 Os1 53.1(14) . . . . ?
C14 C8 C13 Os1 -122.8(14) . . . . ?
C11 C12 C13 C8 0(2) . . . . ?
Os1 C12 C13 C8 55.2(12) . . . . ?
C11 C12 C13 Os1 -55.5(12) . . . . ?
C12 Os1 C13 C8 -130.5(14) . . . . ?
C10 Os1 C13 C8 -64.2(10) . . . . ?
C11 Os1 C13 C8 -101.0(10) . . . . ?
C9 Os1 C13 C8 -28.2(9) . . . . ?
P1 Os1 C13 C8 153.3(9) . . . . ?
Cl2 Os1 C13 C8 -68(3) . . . . ?
Cl1 Os1 C13 C8 70.7(9) . . . . ?
C10 Os1 C13 C12 66.3(10) . . . . ?
C8 Os1 C13 C12 130.5(14) . . . . ?
C11 Os1 C13 C12 29.4(9) . . . . ?
C9 Os1 C13 C12 102.3(11) . . . . ?
P1 Os1 C13 C12 -76.2(9) . . . . ?
Cl2 Os1 C13 C12 63(3) . . . . ?
Cl1 Os1 C13 C12 -158.9(9) . . . . ?
C10 C11 C15 C17 45(2) . . . . ?
C12 C11 C15 C17 -137.3(16) . . . . ?
Os1 C11 C15 C17 -51(2) . . . . ?
C10 C11 C15 C16 -80.6(19) . . . . ?
C12 C11 C15 C16 96.9(17) . . . . ?
Os1 C11 C15 C16 -176.4(12) . . . . ?
|
1100809.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100809.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100809
loop_
_publ_author_name
'Boyd, Catherine L.'
'Clot, Eric'
'Guiducci, Aldo E.'
'Mountford, Philip'
_publ_section_title
;
Pendant Arm Functionalized Benzamidinate Titanium Imido Compounds:
Experimental and Computational Studies of Their Reactions with CO~2~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2347
_journal_page_last 2367
_journal_paper_doi 10.1021/om049026f
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety ' C30 H50 N4 O2 Si1 Ti1 '
_chemical_formula_sum 'C30 H50 N4 O2 Si Ti'
_chemical_formula_weight 574.74
_chemical_name_systematic
;
[Ti{Me3SiNC(Ph)CH2CH2CH2NMe2}{OC(O)N-t-Bu}]
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_cell_angle_alpha 90.00
_cell_angle_beta 104.140(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.0352(3)
_cell_length_b 20.1007(8)
_cell_length_c 18.2507(7)
_cell_measurement_reflns_used 4526
_cell_measurement_temperature 150
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 2.910
_cell_volume 3214.2(2)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)'
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution 'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature 150
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.03
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 9624
_diffrn_reflns_theta_max 27.485
_diffrn_reflns_theta_min 2.91
_diffrn_standards_decay_% 'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time 'not measured'
_diffrn_standards_number 'not measured'
_exptl_absorpt_coefficient_mu 0.33
_exptl_absorpt_correction_T_max 0.968
_exptl_absorpt_correction_T_min 0.968
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour block
_exptl_crystal_density_diffrn 1.19
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description red
_exptl_crystal_F_000 1241.43
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.49
_refine_diff_density_min -0.44
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 204(33)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref 1.0724
_refine_ls_hydrogen_treatment 'riding model'
_refine_ls_matrix_type full
_refine_ls_number_parameters 344
_refine_ls_number_reflns 2377
_refine_ls_number_restraints 0
_refine_ls_R_factor_gt 0.0597
_refine_ls_shift/su_max 0.000194
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979,
0.416 -.575 0.123 -.286
;
_refine_ls_weighting_scheme 'Chebychev polynomial'
_refine_ls_wR_factor_ref 0.0496
_reflns_limit_h_max 11
_reflns_limit_h_min -11
_reflns_limit_k_max 26
_reflns_limit_k_min 0
_reflns_limit_l_max 23
_reflns_limit_l_min 0
_reflns_number_gt 2377
_reflns_number_total 6497
_reflns_threshold_expression >3.00\s(I)
_cod_data_source_file om049026fsi20041209_070538.cif
_cod_data_source_block compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.
'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M 'P 1 21/n 1 '
_cod_original_formula_sum ' C30 H50 N4 O2 Si1 Ti1 '
_cod_database_code 1100809
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Ti1 0.65879(11) 0.43276(6) 0.32422(6) 0.0334 1.0000 Uani
N1 0.6046(5) 0.3472(2) 0.2583(3) 0.0362 1.0000 Uani
N2 0.7554(4) 0.4249(2) 0.2291(2) 0.0326 1.0000 Uani
N3 0.8879(5) 0.5698(3) 0.0327(3) 0.0431 1.0000 Uani
N4 0.5150(5) 0.5066(3) 0.2840(3) 0.0394 1.0000 Uani
Si1 0.44899(19) 0.2921(1) 0.24149(11) 0.0466 1.0000 Uani
C1 0.6916(6) 0.3665(3) 0.2112(3) 0.0331 1.0000 Uani
C2 0.7155(6) 0.3255(3) 0.1473(3) 0.0382 1.0000 Uani
C3 0.8224(7) 0.2743(3) 0.1598(4) 0.0509 1.0000 Uani
C4 0.8485(8) 0.2382(4) 0.0986(5) 0.0609 1.0000 Uani
C5 0.7690(9) 0.2520(4) 0.0268(5) 0.0675 1.0000 Uani
C6 0.6624(9) 0.3026(4) 0.0143(4) 0.0620 1.0000 Uani
C7 0.6370(7) 0.3393(3) 0.0740(4) 0.0494 1.0000 Uani
C8 0.8745(6) 0.4501(3) 0.1935(3) 0.0370 1.0000 Uani
C9 0.8129(6) 0.4900(3) 0.1214(3) 0.0344 1.0000 Uani
C10 0.9373(6) 0.5333(3) 0.1035(3) 0.0380 1.0000 Uani
C11 0.7698(8) 0.6174(4) 0.0371(5) 0.0777 1.0000 Uani
C12 1.0188(7) 0.6052(3) 0.0167(4) 0.0480 1.0000 Uani
C13 0.4111(7) 0.2684(4) 0.3335(4) 0.0593 1.0000 Uani
C14 0.2776(7) 0.3351(4) 0.1836(4) 0.0678 1.0000 Uani
C15 0.4841(9) 0.2154(4) 0.1923(5) 0.0912 1.0000 Uani
C16 0.3977(7) 0.4748(3) 0.3059(4) 0.0450 1.0000 Uani
C17 0.4840(6) 0.5645(3) 0.2317(3) 0.0417 1.0000 Uani
C18 0.6358(7) 0.5988(3) 0.2367(4) 0.0499 1.0000 Uani
C19 0.4122(7) 0.5379(3) 0.1522(4) 0.0555 1.0000 Uani
C20 0.3752(8) 0.6145(4) 0.2550(5) 0.0720 1.0000 Uani
C21 0.9180(6) 0.4059(3) 0.3876(3) 0.0345 1.0000 Uani
C22 0.8954(6) 0.4744(3) 0.3974(3) 0.0336 1.0000 Uani
C23 0.7840(7) 0.4804(4) 0.4401(4) 0.0497 1.0000 Uani
C24 0.7407(6) 0.4160(4) 0.4567(3) 0.0489 1.0000 Uani
C25 0.8225(6) 0.3694(3) 0.4239(3) 0.0419 1.0000 Uani
C26 1.0365(6) 0.3735(3) 0.3530(3) 0.0399 1.0000 Uani
C27 0.9820(7) 0.5316(3) 0.3751(4) 0.0451 1.0000 Uani
C28 0.7300(8) 0.5460(4) 0.4658(4) 0.0696 1.0000 Uani
C29 0.6340(7) 0.3996(5) 0.5063(4) 0.0760 1.0000 Uani
C30 0.8191(7) 0.2947(4) 0.4312(4) 0.0646 1.0000 Uani
O1 0.4615(4) 0.4250(2) 0.3516(2) 0.0458 1.0000 Uani
O2 0.2623(4) 0.4872(2) 0.2909(3) 0.0578 1.0000 Uani
H31 0.8796(7) 0.2638(3) 0.2127(4) 0.0710 1.0000 Uiso
H41 0.9254(8) 0.2014(4) 0.1075(5) 0.0836 1.0000 Uiso
H51 0.7885(9) 0.2257(4) -0.0164(5) 0.0858 1.0000 Uiso
H61 0.6039(9) 0.3121(4) -0.0387(4) 0.0807 1.0000 Uiso
H71 0.5612(7) 0.3765(3) 0.0643(4) 0.0638 1.0000 Uiso
H81 0.9430(6) 0.4802(3) 0.2304(3) 0.0557 1.0000 Uiso
H82 0.9348(6) 0.4115(3) 0.1819(3) 0.0557 1.0000 Uiso
H91 0.7258(6) 0.5185(3) 0.1272(3) 0.0477 1.0000 Uiso
H92 0.7768(6) 0.4584(3) 0.0785(3) 0.0477 1.0000 Uiso
H101 0.9692(6) 0.5661(3) 0.1456(3) 0.0501 1.0000 Uiso
H102 1.0263(6) 0.5045(3) 0.1009(3) 0.0501 1.0000 Uiso
H111 0.7367(8) 0.6413(4) -0.0123(5) 0.1042 1.0000 Uiso
H112 0.8118(8) 0.6502(4) 0.0781(5) 0.1042 1.0000 Uiso
H113 0.6803(8) 0.5940(4) 0.0484(5) 0.1042 1.0000 Uiso
H121 0.9855(7) 0.6301(3) -0.0320(4) 0.0663 1.0000 Uiso
H122 1.0612(7) 0.6371(3) 0.0585(4) 0.0663 1.0000 Uiso
H123 1.0992(7) 0.5721(3) 0.0127(4) 0.0663 1.0000 Uiso
H131 0.3230(7) 0.2368(4) 0.3249(4) 0.0823 1.0000 Uiso
H132 0.3860(7) 0.3094(4) 0.3592(4) 0.0823 1.0000 Uiso
H133 0.5037(7) 0.2467(4) 0.3659(4) 0.0823 1.0000 Uiso
H141 0.1883(7) 0.3041(4) 0.1737(4) 0.0840 1.0000 Uiso
H142 0.2544(7) 0.3750(4) 0.2115(4) 0.0840 1.0000 Uiso
H143 0.2981(7) 0.3493(4) 0.1345(4) 0.0840 1.0000 Uiso
H151 0.3929(9) 0.1856(4) 0.1843(5) 0.1206 1.0000 Uiso
H152 0.5756(9) 0.1915(4) 0.2229(5) 0.1206 1.0000 Uiso
H153 0.5024(9) 0.2281(4) 0.1423(5) 0.1206 1.0000 Uiso
H181 0.6197(7) 0.6383(3) 0.2024(4) 0.0681 1.0000 Uiso
H182 0.6773(7) 0.6138(3) 0.2901(4) 0.0681 1.0000 Uiso
H183 0.7098(7) 0.5676(3) 0.2220(4) 0.0681 1.0000 Uiso
H191 0.3902(7) 0.5762(3) 0.1161(4) 0.0667 1.0000 Uiso
H192 0.4846(7) 0.5066(3) 0.1363(4) 0.0667 1.0000 Uiso
H193 0.3150(7) 0.5140(3) 0.1520(4) 0.0667 1.0000 Uiso
H201 0.3563(8) 0.6529(4) 0.2190(5) 0.1039 1.0000 Uiso
H202 0.4225(8) 0.6311(4) 0.3071(5) 0.1039 1.0000 Uiso
H203 0.2763(8) 0.5920(4) 0.2544(5) 0.1039 1.0000 Uiso
H261 1.0257(6) 0.3241(3) 0.3547(3) 0.0552 1.0000 Uiso
H262 1.1410(6) 0.3867(3) 0.3824(3) 0.0552 1.0000 Uiso
H263 1.0211(6) 0.3883(3) 0.2994(3) 0.0552 1.0000 Uiso
H271 0.9391(7) 0.5745(3) 0.3885(4) 0.0535 1.0000 Uiso
H272 1.0921(7) 0.5283(3) 0.4024(4) 0.0535 1.0000 Uiso
H273 0.9725(7) 0.5299(3) 0.3194(4) 0.0535 1.0000 Uiso
H281 0.6522(8) 0.5375(4) 0.4953(4) 0.0857 1.0000 Uiso
H282 0.8188(8) 0.5703(4) 0.4982(4) 0.0857 1.0000 Uiso
H283 0.6836(8) 0.5736(4) 0.4204(4) 0.0857 1.0000 Uiso
H291 0.6224(7) 0.3502(5) 0.5079(4) 0.1003 1.0000 Uiso
H292 0.6774(7) 0.4168(5) 0.5586(4) 0.1003 1.0000 Uiso
H293 0.5319(7) 0.4204(5) 0.4852(4) 0.1003 1.0000 Uiso
H301 0.7412(7) 0.2811(4) 0.4589(4) 0.0781 1.0000 Uiso
H302 0.9219(7) 0.2782(4) 0.4590(4) 0.0781 1.0000 Uiso
H303 0.7920(7) 0.2752(4) 0.3792(4) 0.0781 1.0000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0229(5) 0.0398(7) 0.0406(6) 0.0052(6) 0.0135(4) 0.0013(5)
N1 0.030(2) 0.043(3) 0.037(3) 0.005(2) 0.011(2) -0.003(2)
N2 0.025(2) 0.035(3) 0.042(3) 0.007(3) 0.015(2) 0.002(2)
N3 0.041(3) 0.047(3) 0.043(3) 0.013(3) 0.015(2) 0.000(3)
N4 0.023(2) 0.048(3) 0.050(3) 0.003(3) 0.014(2) 0.002(2)
Si1 0.0367(9) 0.0509(12) 0.0563(12) -0.001(1) 0.0194(9) -0.0131(9)
C1 0.028(3) 0.030(4) 0.043(4) 0.009(3) 0.010(3) 0.006(3)
C2 0.031(3) 0.038(4) 0.050(4) -0.002(3) 0.018(3) -0.012(3)
C3 0.045(4) 0.055(5) 0.055(5) -0.007(4) 0.018(3) -0.002(3)
C4 0.059(4) 0.057(5) 0.075(6) -0.020(4) 0.032(4) -0.011(4)
C5 0.076(6) 0.074(6) 0.062(5) -0.025(5) 0.035(5) -0.039(5)
C6 0.087(6) 0.057(5) 0.041(4) -0.010(4) 0.013(4) -0.034(5)
C7 0.046(4) 0.052(4) 0.045(4) 0.004(4) 0.002(3) -0.020(3)
C8 0.031(3) 0.033(4) 0.051(4) 0.004(3) 0.018(3) -0.000(2)
C9 0.027(3) 0.043(4) 0.035(3) -0.005(3) 0.011(3) -0.003(3)
C10 0.036(3) 0.036(4) 0.044(4) -0.003(3) 0.015(3) -0.007(3)
C11 0.068(5) 0.084(7) 0.089(6) 0.052(5) 0.036(5) 0.022(5)
C12 0.056(4) 0.047(4) 0.048(4) 0.005(3) 0.024(3) -0.012(3)
C13 0.044(4) 0.066(5) 0.074(5) 0.019(4) 0.026(4) -0.014(4)
C14 0.034(4) 0.100(6) 0.066(5) 0.002(5) 0.005(3) -0.020(4)
C15 0.084(6) 0.073(6) 0.133(8) -0.044(6) 0.058(6) -0.049(5)
C16 0.033(3) 0.059(5) 0.044(4) 0.007(4) 0.013(3) 0.007(3)
C17 0.030(3) 0.046(4) 0.049(4) 0.009(4) 0.010(3) 0.011(3)
C18 0.040(3) 0.047(4) 0.067(4) 0.012(4) 0.020(3) 0.001(3)
C19 0.033(3) 0.066(5) 0.066(5) 0.027(4) 0.009(3) -0.000(3)
C20 0.058(5) 0.049(5) 0.119(7) 0.015(5) 0.041(5) 0.025(4)
C21 0.029(3) 0.037(4) 0.039(3) 0.004(3) 0.012(3) 0.007(3)
C22 0.026(3) 0.043(4) 0.032(3) 0.000(3) 0.006(3) 0.003(3)
C23 0.034(3) 0.072(5) 0.043(4) 0.003(4) 0.008(3) 0.019(3)
C24 0.029(3) 0.077(6) 0.042(4) 0.014(4) 0.010(3) 0.000(3)
C25 0.035(3) 0.041(4) 0.048(4) 0.016(3) 0.005(3) 0.002(3)
C26 0.024(3) 0.043(4) 0.053(4) 0.004(3) 0.008(3) 0.008(3)
C27 0.041(3) 0.034(4) 0.055(4) 0.001(3) 0.003(3) -0.002(3)
C28 0.061(5) 0.093(7) 0.050(4) -0.020(4) 0.004(4) 0.039(4)
C29 0.045(4) 0.132(8) 0.060(5) 0.020(5) 0.029(4) 0.002(5)
C30 0.035(4) 0.064(5) 0.088(6) 0.028(5) 0.001(4) -0.007(4)
O1 0.032(2) 0.059(3) 0.053(3) 0.012(2) 0.0220(19) 0.004(2)
O2 0.025(2) 0.072(3) 0.080(3) 0.011(3) 0.020(2) 0.009(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ti1 . N2 . 63.56(18) yes
N1 . Ti1 . N4 . 111.20(19) yes
N2 . Ti1 . N4 . 96.60(18) yes
N1 . Ti1 . C16 . 97.1(2) yes
N2 . Ti1 . C16 . 119.12(19) yes
N4 . Ti1 . C16 . 34.2(2) yes
N1 . Ti1 . C21 . 98.95(19) yes
N2 . Ti1 . C21 . 80.25(17) yes
N4 . Ti1 . C21 . 144.6(2) yes
C16 . Ti1 . C21 . 159.1(2) yes
N1 . Ti1 . C22 . 131.73(19) yes
N2 . Ti1 . C22 . 89.59(18) yes
N4 . Ti1 . C22 . 111.1(2) yes
C16 . Ti1 . C22 . 131.2(2) yes
C21 . Ti1 . C22 . 34.28(19) yes
N1 . Ti1 . C23 . 148.1(2) yes
N2 . Ti1 . C23 . 124.2(2) yes
N4 . Ti1 . C23 . 99.0(2) yes
C16 . Ti1 . C23 . 102.6(2) yes
C21 . Ti1 . C23 . 57.3(2) yes
N1 . Ti1 . C24 . 116.2(2) yes
N2 . Ti1 . C24 . 137.03(18) yes
N4 . Ti1 . C24 . 119.6(2) yes
C16 . Ti1 . C24 . 103.8(2) yes
C21 . Ti1 . C24 . 56.90(19) yes
N1 . Ti1 . C25 . 90.8(2) yes
N2 . Ti1 . C25 . 106.14(19) yes
N4 . Ti1 . C25 . 153.8(2) yes
C16 . Ti1 . C25 . 132.7(2) yes
C21 . Ti1 . C25 . 34.16(19) yes
N1 . Ti1 . O1 . 88.92(18) yes
N2 . Ti1 . O1 . 140.90(18) yes
N4 . Ti1 . O1 . 66.64(18) yes
C16 . Ti1 . O1 . 33.06(18) yes
C21 . Ti1 . O1 . 134.00(18) yes
C22 . Ti1 . C23 . 34.98(19) yes
C22 . Ti1 . C24 . 57.6(2) yes
C23 . Ti1 . C24 . 34.6(2) yes
C22 . Ti1 . C25 . 57.3(2) yes
C23 . Ti1 . C25 . 57.5(2) yes
C24 . Ti1 . C25 . 34.4(2) yes
C22 . Ti1 . O1 . 129.03(18) yes
C23 . Ti1 . O1 . 94.1(2) yes
C24 . Ti1 . O1 . 78.88(18) yes
C25 . Ti1 . O1 . 101.14(19) yes
Ti1 . N1 . Si1 . 133.3(3) yes
Ti1 . N1 . C1 . 92.2(4) yes
Si1 . N1 . C1 . 129.2(4) yes
Ti1 . N2 . C1 . 91.5(3) yes
Ti1 . N2 . C8 . 145.2(4) yes
C1 . N2 . C8 . 121.4(5) yes
C10 . N3 . C11 . 110.7(5) yes
C10 . N3 . C12 . 109.4(5) yes
C11 . N3 . C12 . 109.2(5) yes
Ti1 . N4 . C16 . 91.5(4) yes
Ti1 . N4 . C17 . 145.4(3) yes
C16 . N4 . C17 . 120.8(5) yes
N1 . Si1 . C13 . 108.7(3) yes
N1 . Si1 . C14 . 109.1(3) yes
C13 . Si1 . C14 . 108.7(3) yes
N1 . Si1 . C15 . 112.7(3) yes
C13 . Si1 . C15 . 108.4(4) yes
C14 . Si1 . C15 . 109.2(4) yes
N1 . C1 . N2 . 112.7(5) yes
N1 . C1 . C2 . 123.8(5) yes
N2 . C1 . C2 . 123.5(5) yes
C1 . C2 . C3 . 120.7(6) yes
C1 . C2 . C7 . 120.7(6) yes
C3 . C2 . C7 . 118.6(6) yes
C2 . C3 . C4 . 119.9(7) yes
C3 . C4 . C5 . 120.7(7) yes
C4 . C5 . C6 . 119.5(7) yes
C5 . C6 . C7 . 120.4(7) yes
C2 . C7 . C6 . 120.9(7) yes
N2 . C8 . C9 . 114.1(4) yes
C8 . C9 . C10 . 110.7(4) yes
N3 . C10 . C9 . 113.3(5) yes
Ti1 . C16 . N4 . 54.3(3) yes
Ti1 . C16 . O1 . 53.4(3) yes
N4 . C16 . O1 . 106.4(5) yes
Ti1 . C16 . O2 . 170.5(5) yes
N4 . C16 . O2 . 130.1(6) yes
O1 . C16 . O2 . 123.5(6) yes
N4 . C17 . C18 . 106.9(4) yes
N4 . C17 . C19 . 107.7(5) yes
C18 . C17 . C19 . 112.5(5) yes
N4 . C17 . C20 . 111.6(5) yes
C18 . C17 . C20 . 108.4(6) yes
C19 . C17 . C20 . 109.8(5) yes
Ti1 . C21 . C22 . 71.8(3) yes
Ti1 . C21 . C25 . 73.0(3) yes
C22 . C21 . C25 . 108.8(5) yes
Ti1 . C21 . C26 . 126.9(4) yes
C22 . C21 . C26 . 127.6(5) yes
C25 . C21 . C26 . 123.2(5) yes
Ti1 . C22 . C21 . 73.9(3) yes
Ti1 . C22 . C23 . 71.2(3) yes
C21 . C22 . C23 . 107.2(5) yes
Ti1 . C22 . C27 . 125.0(4) yes
C21 . C22 . C27 . 127.7(5) yes
C23 . C22 . C27 . 124.8(6) yes
Ti1 . C23 . C22 . 73.8(3) yes
Ti1 . C23 . C24 . 73.8(4) yes
C22 . C23 . C24 . 108.2(6) yes
Ti1 . C23 . C28 . 120.8(4) yes
C22 . C23 . C28 . 124.5(7) yes
C24 . C23 . C28 . 127.3(6) yes
Ti1 . C24 . C23 . 71.6(4) yes
Ti1 . C24 . C25 . 74.2(4) yes
C23 . C24 . C25 . 108.4(5) yes
Ti1 . C24 . C29 . 123.7(4) yes
C23 . C24 . C29 . 125.6(7) yes
C25 . C24 . C29 . 125.8(7) yes
Ti1 . C25 . C21 . 72.8(3) yes
Ti1 . C25 . C24 . 71.5(3) yes
C21 . C25 . C24 . 107.3(6) yes
Ti1 . C25 . C30 . 124.8(4) yes
C21 . C25 . C30 . 125.8(6) yes
C24 . C25 . C30 . 126.8(6) yes
Ti1 . O1 . C16 . 93.5(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . N1 . 2.087(5) yes
Ti1 . N2 . 2.131(4) yes
Ti1 . N4 . 1.991(5) yes
Ti1 . C16 . 2.450(6) yes
Ti1 . C21 . 2.406(5) yes
Ti1 . C22 . 2.379(5) yes
Ti1 . C23 . 2.346(7) yes
Ti1 . C24 . 2.374(6) yes
Ti1 . C25 . 2.409(6) yes
Ti1 . O1 . 1.971(4) yes
N1 . Si1 . 1.757(5) yes
N1 . C1 . 1.356(7) yes
N2 . C1 . 1.313(7) yes
N2 . C8 . 1.475(6) yes
N3 . C10 . 1.457(7) yes
N3 . C11 . 1.451(8) yes
N3 . C12 . 1.470(7) yes
N4 . C16 . 1.378(7) yes
N4 . C17 . 1.487(8) yes
Si1 . C13 . 1.856(6) yes
Si1 . C14 . 1.860(7) yes
Si1 . C15 . 1.851(8) yes
C1 . C2 . 1.487(8) yes
C2 . C3 . 1.392(8) yes
C2 . C7 . 1.380(8) yes
C3 . C4 . 1.400(9) yes
C4 . C5 . 1.36(1) yes
C5 . C6 . 1.381(11) yes
C6 . C7 . 1.381(9) yes
C8 . C9 . 1.527(8) yes
C9 . C10 . 1.518(7) yes
C16 . O1 . 1.339(7) yes
C16 . O2 . 1.213(7) yes
C17 . C18 . 1.518(8) yes
C17 . C19 . 1.534(9) yes
C17 . C20 . 1.537(8) yes
C21 . C22 . 1.410(8) yes
C21 . C25 . 1.414(8) yes
C21 . C26 . 1.516(7) yes
C22 . C23 . 1.420(8) yes
C22 . C27 . 1.502(8) yes
C23 . C24 . 1.41(1) yes
C23 . C28 . 1.520(9) yes
C24 . C25 . 1.414(9) yes
C24 . C29 . 1.511(8) yes
C25 . C30 . 1.509(9) yes
|
1100810.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100810.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100810
loop_
_publ_author_name
'Boyd, Catherine L.'
'Clot, Eric'
'Guiducci, Aldo E.'
'Mountford, Philip'
_publ_section_title
;
Pendant Arm Functionalized Benzamidinate Titanium Imido Compounds:
Experimental and Computational Studies of Their Reactions with CO~2~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2347
_journal_page_last 2367
_journal_paper_doi 10.1021/om049026f
_journal_volume 24
_journal_year 2005
_chemical_compound_source
;
[Ti(N-t-Bu){Me3SiNC(C6H5)NCH2CH2NMe2}Cl] + CO2
;
_chemical_formula_moiety ' C40 H62 N6 O2 Si2 Ti2 '
_chemical_formula_sum 'C40 H62 N6 O2 Si2 Ti2'
_chemical_formula_weight 810.95
_chemical_melting_point ?
_chemical_name_systematic
;
[Ti2(mu-O)2(C5H4Me)2{Me3SiNC(C6H5)NCH2CH2NMe2}2]
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary 'Fourier difference maps'
_cell_angle_alpha 108.200(1)
_cell_angle_beta 94.168(1)
_cell_angle_gamma 90.162(2)
_cell_formula_units_Z 4
_cell_length_a 12.7045(4)
_cell_length_b 16.1774(4)
_cell_length_c 22.8120(8)
_cell_measurement_reflns_used 13497
_cell_measurement_temperature 150
_cell_measurement_theta_max 24.108
_cell_measurement_theta_min 2.910
_cell_volume 4440.5
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution 'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature 150
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.037
_diffrn_reflns_av_sigmaI/netI 0.235
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 26452
_diffrn_reflns_theta_max 24.06
_diffrn_reflns_theta_min 2.98
_diffrn_standards_decay_% 'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time 'not measured'
_diffrn_standards_number 'not measured'
_exptl_absorpt_coefficient_mu 0.45
_exptl_absorpt_correction_T_max 0.980
_exptl_absorpt_correction_T_min 0.980
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.21
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description block
_exptl_crystal_F_000 1728
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.34
_refine_diff_density_min -0.34
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 51.9(74)
_refine_ls_extinction_method
;
Larson 1970 Crystallographic Computing eq 22
;
_refine_ls_goodness_of_fit_ref 0.2534
_refine_ls_hydrogen_treatment 'riding model'
_refine_ls_matrix_type blocked
_refine_ls_number_parameters 939
_refine_ls_number_reflns 6099
_refine_ls_number_restraints 0
_refine_ls_R_factor_gt 0.0522
_refine_ls_shift/su_max 0.0025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme unit
_refine_ls_wR_factor_ref 0.0575
_reflns_limit_h_max 14
_reflns_limit_h_min -14
_reflns_limit_k_max 17
_reflns_limit_k_min -18
_reflns_limit_l_max 26
_reflns_limit_l_min 0
_reflns_number_gt 6099
_reflns_number_total 13969
_reflns_threshold_expression >2.00\s(I)
_cod_data_source_file om049026fsi20041209_070538.cif
_cod_data_source_block 10a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'unit weights' was changed to
'unit'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
The following automatic conversions were performed:
'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.
'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M 'P -1 '
_cod_original_formula_sum ' C40 H62 N6 O2 Si2 Ti2 '
_cod_database_code 1100810
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Ti1 1.4510(1) 0.91902(9) 0.28799(6) 0.0254 1.0000 Uani
Ti2 1.3004(1) 0.81735(9) 0.20091(6) 0.0266 1.0000 Uani
N1 1.4014(5) 1.0359(4) 0.3573(3) 0.0308 1.0000 Uani
N2 1.4735(5) 1.0409(4) 0.2733(3) 0.0302 1.0000 Uani
N3 1.4686(5) 1.0976(5) 0.1263(3) 0.0453 1.0000 Uani
N4 1.3458(5) 0.6996(4) 0.1289(3) 0.0302 1.0000 Uani
N5 1.2792(5) 0.6954(4) 0.2150(3) 0.0320 1.0000 Uani
N6 1.2783(5) 0.6386(4) 0.3618(3) 0.0384 1.0000 Uani
O1 1.3253(4) 0.8658(3) 0.2880(2) 0.0260 1.0000 Uani
O2 1.4274(4) 0.8689(3) 0.2012(2) 0.0286 1.0000 Uani
Si1 1.32857(18) 1.06241(15) 0.4209(1) 0.0337 1.0000 Uani
Si2 1.42551(19) 0.67834(16) 0.06846(11) 0.0392 1.0000 Uani
C1 1.4370(6) 1.0867(5) 0.3259(3) 0.0292 1.0000 Uani
C2 1.4419(6) 1.1847(5) 0.3493(3) 0.0273 1.0000 Uani
C3 1.3659(7) 1.2332(6) 0.3306(5) 0.0546 1.0000 Uani
C4 1.3696(7) 1.3233(6) 0.3536(5) 0.0657 1.0000 Uani
C5 1.4537(7) 1.3635(6) 0.3957(4) 0.0462 1.0000 Uani
C6 1.5296(8) 1.3145(6) 0.4142(4) 0.0516 1.0000 Uani
C7 1.5248(7) 1.2270(6) 0.3905(4) 0.0483 1.0000 Uani
C8 1.5146(6) 1.0784(5) 0.2287(3) 0.0322 1.0000 Uani
C9 1.4379(6) 1.0575(5) 0.1710(3) 0.0346 1.0000 Uani
C10 1.4144(8) 1.0535(7) 0.0648(4) 0.0660 1.0000 Uani
C11 1.4418(8) 1.1887(6) 0.1453(5) 0.0662 1.0000 Uani
C12 1.3961(8) 1.1443(6) 0.4894(4) 0.0569 1.0000 Uani
C13 1.1982(7) 1.1052(7) 0.4028(5) 0.0639 1.0000 Uani
C14 1.3066(7) 0.9597(5) 0.4400(4) 0.0481 1.0000 Uani
C15 1.6330(6) 0.8728(6) 0.2753(4) 0.0410 1.0000 Uani
C16 1.6376(6) 0.9468(6) 0.3290(4) 0.0410 1.0000 Uani
C17 1.5779(6) 0.9243(6) 0.3730(4) 0.0401 1.0000 Uani
C18 1.5384(6) 0.8398(5) 0.3474(4) 0.0377 1.0000 Uani
C19 1.5707(6) 0.8084(6) 0.2876(4) 0.0392 1.0000 Uani
C20 1.6857(7) 0.8663(7) 0.2183(4) 0.0619 1.0000 Uani
C21 1.3151(6) 0.6500(5) 0.1615(4) 0.0298 1.0000 Uani
C22 1.3145(6) 0.5527(5) 0.1395(4) 0.0311 1.0000 Uani
C23 1.3862(7) 0.5074(6) 0.1651(5) 0.0547 1.0000 Uani
C24 1.3835(7) 0.4165(6) 0.1440(5) 0.0628 1.0000 Uani
C25 1.3144(8) 0.3720(6) 0.0978(4) 0.0542 1.0000 Uani
C26 1.2429(9) 0.4150(6) 0.0721(5) 0.0688 1.0000 Uani
C27 1.2430(8) 0.5058(7) 0.0921(4) 0.0585 1.0000 Uani
C28 1.2375(6) 0.6573(6) 0.2587(3) 0.0371 1.0000 Uani
C29 1.3108(6) 0.6821(5) 0.3183(3) 0.0335 1.0000 Uani
C30 1.3150(7) 0.5490(6) 0.3456(4) 0.0524 1.0000 Uani
C31 1.3196(8) 0.6850(6) 0.4243(4) 0.0602 1.0000 Uani
C32 1.372(1) 0.5915(7) -0.0014(4) 0.0843 1.0000 Uani
C33 1.5577(8) 0.6434(8) 0.0917(5) 0.0755 1.0000 Uani
C34 1.4412(8) 0.7796(6) 0.0498(4) 0.0572 1.0000 Uani
C35 1.1219(6) 0.8682(6) 0.2164(4) 0.0371 1.0000 Uani
C36 1.1847(6) 0.9308(5) 0.2024(4) 0.0375 1.0000 Uani
C37 1.2121(6) 0.8967(6) 0.1413(4) 0.0400 1.0000 Uani
C38 1.1702(6) 0.8113(5) 0.1180(4) 0.0343 1.0000 Uani
C39 1.1141(6) 0.7947(5) 0.1644(4) 0.0350 1.0000 Uani
C40 1.0739(7) 0.8779(7) 0.2768(4) 0.0617 1.0000 Uani
H31 1.3093(7) 1.2037(6) 0.3012(5) 0.0706 1.0000 Uiso
H41 1.3163(7) 1.3572(6) 0.3405(5) 0.0838 1.0000 Uiso
H51 1.4584(7) 1.4258(6) 0.4121(4) 0.0630 1.0000 Uiso
H61 1.5862(8) 1.3424(6) 0.4442(4) 0.0715 1.0000 Uiso
H71 1.5801(7) 1.1931(6) 0.4017(4) 0.0624 1.0000 Uiso
H81 1.5219(6) 1.1404(5) 0.2468(3) 0.0486 1.0000 Uiso
H82 1.5821(6) 1.0547(5) 0.2174(3) 0.0486 1.0000 Uiso
H91 1.3695(6) 1.0771(5) 0.1837(3) 0.0506 1.0000 Uiso
H92 1.4350(6) 0.9955(5) 0.1519(3) 0.0506 1.0000 Uiso
H101 1.4353(8) 1.0811(7) 0.0356(4) 0.0850 1.0000 Uiso
H102 1.4335(8) 0.9935(7) 0.0514(4) 0.0850 1.0000 Uiso
H103 1.3393(8) 1.0570(7) 0.0672(4) 0.0850 1.0000 Uiso
H111 1.4627(8) 1.2150(6) 0.1154(5) 0.0890 1.0000 Uiso
H112 1.4789(8) 1.2173(6) 0.1847(5) 0.0890 1.0000 Uiso
H113 1.3671(8) 1.1945(6) 0.1489(5) 0.0890 1.0000 Uiso
H121 1.3520(8) 1.1566(6) 0.5234(4) 0.0718 1.0000 Uiso
H122 1.4090(8) 1.1967(6) 0.4795(4) 0.0718 1.0000 Uiso
H123 1.4620(8) 1.1223(6) 0.5007(4) 0.0718 1.0000 Uiso
H131 1.1584(7) 1.1195(7) 0.4387(5) 0.0889 1.0000 Uiso
H132 1.2095(7) 1.1564(7) 0.3911(5) 0.0889 1.0000 Uiso
H133 1.1599(7) 1.0619(7) 0.3693(5) 0.0889 1.0000 Uiso
H141 1.2658(7) 0.9712(5) 0.4754(4) 0.0690 1.0000 Uiso
H142 1.3734(7) 0.9370(5) 0.4489(4) 0.0690 1.0000 Uiso
H143 1.2692(7) 0.9179(5) 0.4051(4) 0.0690 1.0000 Uiso
H161 1.6733(6) 1.0014(6) 0.3343(4) 0.0543 1.0000 Uiso
H171 1.5678(6) 0.9619(6) 0.4140(4) 0.0548 1.0000 Uiso
H181 1.4959(6) 0.8089(5) 0.3672(4) 0.0546 1.0000 Uiso
H191 1.5538(6) 0.7516(6) 0.2588(4) 0.0530 1.0000 Uiso
H201 1.6707(7) 0.8096(7) 0.1890(4) 0.0860 1.0000 Uiso
H202 1.7606(7) 0.8746(7) 0.2278(4) 0.0860 1.0000 Uiso
H203 1.6595(7) 0.9098(7) 0.2009(4) 0.0860 1.0000 Uiso
H231 1.4375(7) 0.5387(6) 0.1975(5) 0.0696 1.0000 Uiso
H241 1.4324(7) 0.3855(6) 0.1628(5) 0.0800 1.0000 Uiso
H251 1.3149(8) 0.3096(6) 0.0830(4) 0.0732 1.0000 Uiso
H261 1.1919(9) 0.3830(6) 0.0398(5) 0.0877 1.0000 Uiso
H271 1.1932(8) 0.5360(7) 0.0731(4) 0.0788 1.0000 Uiso
H281 1.2345(6) 0.5950(6) 0.2411(3) 0.0547 1.0000 Uiso
H282 1.1679(6) 0.6780(6) 0.2679(3) 0.0547 1.0000 Uiso
H291 1.3815(6) 0.6662(5) 0.3080(3) 0.0511 1.0000 Uiso
H292 1.3087(6) 0.7439(5) 0.3374(3) 0.0511 1.0000 Uiso
H301 1.2918(7) 0.5218(6) 0.3744(4) 0.0773 1.0000 Uiso
H302 1.3906(7) 0.5492(6) 0.3468(4) 0.0773 1.0000 Uiso
H303 1.2861(7) 0.5171(6) 0.3046(4) 0.0773 1.0000 Uiso
H311 1.2975(8) 0.6558(6) 0.4523(4) 0.0842 1.0000 Uiso
H312 1.3953(8) 0.6869(6) 0.4258(4) 0.0842 1.0000 Uiso
H313 1.2940(8) 0.7432(6) 0.4363(4) 0.0842 1.0000 Uiso
H321 1.420(1) 0.5828(7) -0.0334(4) 0.0971 1.0000 Uiso
H322 1.364(1) 0.5385(7) 0.0085(4) 0.0971 1.0000 Uiso
H323 1.305(1) 0.6080(7) -0.0154(4) 0.0971 1.0000 Uiso
H331 1.6021(8) 0.6317(8) 0.0579(5) 0.0980 1.0000 Uiso
H332 1.5896(8) 0.6891(8) 0.1263(5) 0.0980 1.0000 Uiso
H333 1.5492(8) 0.5918(8) 0.1033(5) 0.0980 1.0000 Uiso
H341 1.4854(8) 0.7703(6) 0.0160(4) 0.0746 1.0000 Uiso
H342 1.4730(8) 0.8238(6) 0.0854(4) 0.0746 1.0000 Uiso
H343 1.3732(8) 0.7980(6) 0.0383(4) 0.0746 1.0000 Uiso
H361 1.2045(6) 0.9877(5) 0.2300(4) 0.0506 1.0000 Uiso
H371 1.2519(6) 0.9262(6) 0.1192(4) 0.0576 1.0000 Uiso
H381 1.1791(6) 0.7712(5) 0.0777(4) 0.0491 1.0000 Uiso
H391 1.0759(6) 0.7418(5) 0.1606(4) 0.0475 1.0000 Uiso
H401 1.0362(7) 0.8249(7) 0.2733(4) 0.0833 1.0000 Uiso
H402 1.1284(7) 0.8891(7) 0.3100(4) 0.0833 1.0000 Uiso
H403 1.0260(7) 0.9252(7) 0.2852(4) 0.0833 1.0000 Uiso
Ti101 0.7970(1) 0.44156(9) 0.26711(6) 0.0277 1.0000 Uani
Ti102 0.9509(1) 0.31746(9) 0.24209(6) 0.0289 1.0000 Uani
N101 0.8066(5) 0.5536(4) 0.3528(3) 0.0281 1.0000 Uani
N102 0.8730(5) 0.5561(4) 0.2672(3) 0.0326 1.0000 Uani
N103 0.9259(5) 0.6254(5) 0.1303(3) 0.0429 1.0000 Uani
N104 0.9425(5) 0.2052(4) 0.1563(3) 0.0299 1.0000 Uani
N105 0.8739(5) 0.2031(4) 0.2421(3) 0.0345 1.0000 Uani
N106 0.8266(5) 0.1318(5) 0.3783(3) 0.0388 1.0000 Uani
O101 0.8611(4) 0.3733(3) 0.3060(2) 0.0280 1.0000 Uani
O102 0.8848(4) 0.3845(3) 0.2027(2) 0.0311 1.0000 Uani
Si101 0.76795(19) 0.57674(15) 0.4276(1) 0.0363 1.0000 Uani
Si102 0.97921(18) 0.18242(16) 0.0814(1) 0.0356 1.0000 Uani
C101 0.8607(6) 0.5996(5) 0.3263(4) 0.0310 1.0000 Uani
C102 0.8998(6) 0.6916(5) 0.3578(3) 0.0295 1.0000 Uani
C103 1.0063(7) 0.7102(5) 0.3774(4) 0.0379 1.0000 Uani
C104 1.0388(6) 0.7939(6) 0.4091(4) 0.0383 1.0000 Uani
C105 0.9673(7) 0.8613(5) 0.4200(4) 0.0434 1.0000 Uani
C106 0.8606(7) 0.8425(6) 0.3988(4) 0.0486 1.0000 Uani
C107 0.8286(6) 0.7575(6) 0.3679(4) 0.0396 1.0000 Uani
C108 0.9345(6) 0.5870(6) 0.2263(4) 0.0410 1.0000 Uani
C109 0.8665(7) 0.6075(7) 0.1778(4) 0.0503 1.0000 Uani
C110 0.8707(8) 0.6821(7) 0.1026(5) 0.0665 1.0000 Uani
C111 0.9479(11) 0.5476(8) 0.0821(6) 0.1021 1.0000 Uani
C112 0.8580(8) 0.6574(6) 0.4877(4) 0.0566 1.0000 Uani
C113 0.6289(7) 0.6164(7) 0.4304(5) 0.0659 1.0000 Uani
C114 0.7700(7) 0.4727(5) 0.4466(4) 0.0454 1.0000 Uani
C115 0.6627(6) 0.3659(6) 0.1858(4) 0.0412 1.0000 Uani
C116 0.6486(6) 0.4553(7) 0.1972(4) 0.0477 1.0000 Uani
C117 0.6217(6) 0.4927(7) 0.2583(4) 0.0506 1.0000 Uani
C118 0.6173(6) 0.4256(7) 0.2849(4) 0.0513 1.0000 Uani
C119 0.6431(6) 0.3490(6) 0.2403(4) 0.0421 1.0000 Uani
C120 0.6913(7) 0.3040(6) 0.1265(4) 0.0545 1.0000 Uani
C121 0.8873(6) 0.1578(5) 0.1826(4) 0.0309 1.0000 Uani
C122 0.8485(6) 0.0681(5) 0.1521(3) 0.0286 1.0000 Uani
C123 0.7443(6) 0.0476(5) 0.1286(3) 0.0310 1.0000 Uani
C124 0.7129(7) -0.0373(6) 0.0967(4) 0.0462 1.0000 Uani
C125 0.7834(8) -0.1032(6) 0.0879(4) 0.0495 1.0000 Uani
C126 0.8861(7) -0.0844(6) 0.1114(4) 0.0454 1.0000 Uani
C127 0.9181(6) -0.0005(5) 0.1425(4) 0.0358 1.0000 Uani
C128 0.8134(6) 0.1708(6) 0.2830(3) 0.0365 1.0000 Uani
C129 0.8827(7) 0.1393(6) 0.3270(4) 0.0454 1.0000 Uani
C130 0.8207(9) 0.2123(7) 0.4253(4) 0.0740 1.0000 Uani
C131 0.8783(8) 0.0700(7) 0.4049(5) 0.0680 1.0000 Uani
C132 0.8916(7) 0.1030(6) 0.0218(4) 0.0469 1.0000 Uani
C133 0.9780(8) 0.2854(6) 0.0624(4) 0.0597 1.0000 Uani
C134 1.1159(7) 0.1406(7) 0.0770(4) 0.0560 1.0000 Uani
C135 1.0850(6) 0.3865(6) 0.3238(4) 0.0400 1.0000 Uani
C136 1.1004(6) 0.4117(6) 0.2715(4) 0.0463 1.0000 Uani
C137 1.1297(6) 0.3383(7) 0.2245(4) 0.0523 1.0000 Uani
C138 1.1286(6) 0.2691(7) 0.2479(5) 0.0525 1.0000 Uani
C139 1.1006(6) 0.2978(6) 0.3089(4) 0.0447 1.0000 Uani
C140 1.0555(7) 0.4476(7) 0.3858(4) 0.0682 1.0000 Uani
H1031 1.0562(7) 0.6643(5) 0.3688(4) 0.0504 1.0000 Uiso
H1041 1.1115(6) 0.8068(6) 0.4240(4) 0.0550 1.0000 Uiso
H1051 0.9905(7) 0.9202(5) 0.4417(4) 0.0601 1.0000 Uiso
H1061 0.8106(7) 0.8883(6) 0.4057(4) 0.0680 1.0000 Uiso
H1071 0.7558(6) 0.7437(6) 0.3536(4) 0.0518 1.0000 Uiso
H1081 0.9739(6) 0.6386(6) 0.2504(4) 0.0608 1.0000 Uiso
H1082 0.9823(6) 0.5428(6) 0.2068(4) 0.0608 1.0000 Uiso
H1091 0.8267(7) 0.6579(7) 0.1969(4) 0.0747 1.0000 Uiso
H1092 0.8190(7) 0.5588(7) 0.1585(4) 0.0747 1.0000 Uiso
H1101 0.9115(8) 0.6930(7) 0.0718(5) 0.1007 1.0000 Uiso
H1102 0.8600(8) 0.7360(7) 0.1342(5) 0.1007 1.0000 Uiso
H1103 0.8035(8) 0.6562(7) 0.0837(5) 0.1007 1.0000 Uiso
H1111 0.9880(11) 0.5616(8) 0.0523(6) 0.1279 1.0000 Uiso
H1112 0.9871(11) 0.5091(8) 0.0995(6) 0.1279 1.0000 Uiso
H1113 0.8822(11) 0.5196(8) 0.0623(6) 0.1279 1.0000 Uiso
H1121 0.8322(8) 0.6671(6) 0.5277(4) 0.0720 1.0000 Uiso
H1122 0.9277(8) 0.6347(6) 0.4875(4) 0.0720 1.0000 Uiso
H1123 0.8602(8) 0.7115(6) 0.4786(4) 0.0720 1.0000 Uiso
H1131 0.6075(7) 0.6291(7) 0.4717(5) 0.0869 1.0000 Uiso
H1132 0.6260(7) 0.6682(7) 0.4184(5) 0.0869 1.0000 Uiso
H1133 0.5824(7) 0.5724(7) 0.4024(5) 0.0869 1.0000 Uiso
H1141 0.7489(7) 0.4832(5) 0.4879(4) 0.0636 1.0000 Uiso
H1142 0.8403(7) 0.4509(5) 0.4442(4) 0.0636 1.0000 Uiso
H1143 0.7223(7) 0.4306(5) 0.4179(4) 0.0636 1.0000 Uiso
H1161 0.6564(6) 0.4858(7) 0.1678(4) 0.0646 1.0000 Uiso
H1171 0.6084(6) 0.5530(7) 0.2783(4) 0.0610 1.0000 Uiso
H1181 0.5994(6) 0.4313(7) 0.3262(4) 0.0690 1.0000 Uiso
H1191 0.6471(6) 0.2929(6) 0.2463(4) 0.0598 1.0000 Uiso
H1201 0.6961(7) 0.2469(6) 0.1308(4) 0.0667 1.0000 Uiso
H1202 0.7581(7) 0.3212(6) 0.1162(4) 0.0667 1.0000 Uiso
H1203 0.6380(7) 0.3032(6) 0.0943(4) 0.0667 1.0000 Uiso
H1231 0.6944(6) 0.0934(5) 0.1343(3) 0.0423 1.0000 Uiso
H1241 0.6406(7) -0.0506(6) 0.0810(4) 0.0557 1.0000 Uiso
H1251 0.7616(8) -0.1621(6) 0.0655(4) 0.0630 1.0000 Uiso
H1261 0.9359(7) -0.1302(6) 0.1058(4) 0.0607 1.0000 Uiso
H1271 0.9904(6) 0.0122(5) 0.1584(4) 0.0501 1.0000 Uiso
H1281 0.7721(6) 0.2172(6) 0.3068(3) 0.0542 1.0000 Uiso
H1282 0.7673(6) 0.1236(6) 0.2585(3) 0.0542 1.0000 Uiso
H1291 0.9410(7) 0.1801(6) 0.3428(4) 0.0661 1.0000 Uiso
H1292 0.9087(7) 0.0835(6) 0.3050(4) 0.0661 1.0000 Uiso
H1301 0.7828(9) 0.2050(7) 0.4583(4) 0.0913 1.0000 Uiso
H1302 0.8909(9) 0.2343(7) 0.4411(4) 0.0913 1.0000 Uiso
H1303 0.7849(9) 0.2528(7) 0.4083(4) 0.0913 1.0000 Uiso
H1311 0.8408(8) 0.0649(7) 0.4388(5) 0.0982 1.0000 Uiso
H1312 0.9495(8) 0.0900(7) 0.4196(5) 0.0982 1.0000 Uiso
H1313 0.8789(8) 0.0142(7) 0.3737(5) 0.0982 1.0000 Uiso
H1321 0.9172(7) 0.0938(6) -0.0182(4) 0.0607 1.0000 Uiso
H1322 0.8903(7) 0.0488(6) 0.0308(4) 0.0607 1.0000 Uiso
H1323 0.8216(7) 0.1252(6) 0.0221(4) 0.0607 1.0000 Uiso
H1331 0.9981(8) 0.2746(6) 0.0209(4) 0.0815 1.0000 Uiso
H1332 1.0272(8) 0.3265(6) 0.0908(4) 0.0815 1.0000 Uiso
H1333 0.9085(8) 0.3087(6) 0.0655(4) 0.0815 1.0000 Uiso
H1341 1.1363(7) 0.1277(7) 0.0355(4) 0.0687 1.0000 Uiso
H1342 1.1640(7) 0.1834(7) 0.1047(4) 0.0687 1.0000 Uiso
H1343 1.1174(7) 0.0885(7) 0.0887(4) 0.0687 1.0000 Uiso
H1361 1.0918(6) 0.4693(6) 0.2688(4) 0.0648 1.0000 Uiso
H1371 1.1481(6) 0.3367(7) 0.1841(4) 0.0680 1.0000 Uiso
H1381 1.1444(6) 0.2102(7) 0.2255(5) 0.0635 1.0000 Uiso
H1391 1.0929(6) 0.2631(6) 0.3358(4) 0.0604 1.0000 Uiso
H1401 1.0491(7) 0.4158(7) 0.4146(4) 0.0778 1.0000 Uiso
H1402 1.1095(7) 0.4923(7) 0.4018(4) 0.0778 1.0000 Uiso
H1403 0.9895(7) 0.4738(7) 0.3800(4) 0.0778 1.0000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0239(7) 0.0272(8) 0.0250(7) 0.0085(6) -0.0009(6) 0.0021(6)
Ti2 0.0229(7) 0.0298(8) 0.0276(8) 0.0101(6) 0.0000(6) 0.0040(6)
N1 0.037(4) 0.026(4) 0.031(4) 0.011(3) 0.003(3) -0.001(3)
N2 0.031(4) 0.030(4) 0.033(4) 0.015(3) 0.003(3) 0.000(3)
N3 0.034(4) 0.068(6) 0.051(5) 0.042(4) 0.010(3) -0.000(4)
N4 0.039(4) 0.023(4) 0.028(4) 0.007(3) 0.005(3) 0.002(3)
N5 0.037(4) 0.030(4) 0.032(4) 0.015(3) 0.003(3) 0.003(3)
N6 0.039(4) 0.040(4) 0.044(4) 0.023(4) 0.004(3) 0.006(3)
O1 0.026(3) 0.030(3) 0.023(3) 0.011(2) 0.001(2) 0.001(2)
O2 0.035(3) 0.024(3) 0.026(3) 0.005(2) 0.007(2) 0.000(2)
Si1 0.0403(14) 0.0320(13) 0.0290(12) 0.009(1) 0.007(1) 0.0041(11)
Si2 0.0484(15) 0.0328(14) 0.0355(13) 0.0074(11) 0.0112(11) 0.0008(11)
C1 0.030(4) 0.032(5) 0.021(4) 0.002(4) 0.001(3) 0.000(4)
C2 0.029(4) 0.024(4) 0.027(4) 0.006(3) 0.001(3) -0.001(3)
C3 0.048(6) 0.032(6) 0.077(7) 0.011(5) -0.009(5) 0.002(4)
C4 0.039(6) 0.045(7) 0.108(9) 0.018(6) -0.005(6) 0.017(5)
C5 0.043(5) 0.037(5) 0.056(6) 0.008(5) 0.014(5) -0.013(4)
C6 0.066(7) 0.046(6) 0.044(6) 0.020(5) -0.014(5) -0.021(5)
C7 0.049(6) 0.039(6) 0.058(6) 0.020(5) -0.018(5) -0.006(4)
C8 0.038(5) 0.039(5) 0.026(4) 0.019(4) 0.006(4) -0.003(4)
C9 0.038(5) 0.032(5) 0.034(5) 0.010(4) 0.006(4) 0.000(4)
C10 0.081(8) 0.091(9) 0.026(5) 0.018(5) 0.010(5) 0.022(6)
C11 0.065(7) 0.063(8) 0.087(8) 0.053(6) -0.024(6) -0.010(6)
C12 0.077(7) 0.052(6) 0.034(5) 0.002(5) 0.007(5) -0.015(5)
C13 0.047(6) 0.078(8) 0.073(7) 0.031(6) 0.017(5) 0.020(6)
C14 0.069(7) 0.034(5) 0.049(5) 0.019(4) 0.024(5) -0.003(5)
C15 0.039(5) 0.052(6) 0.043(5) 0.028(5) 0.013(4) 0.010(4)
C16 0.025(5) 0.050(6) 0.043(5) 0.010(5) -0.008(4) 0.000(4)
C17 0.032(5) 0.052(6) 0.036(5) 0.016(4) -0.008(4) 0.012(4)
C18 0.039(5) 0.032(5) 0.047(5) 0.021(4) -0.005(4) 0.001(4)
C19 0.034(5) 0.046(6) 0.034(5) 0.009(4) -0.001(4) 0.013(4)
C20 0.042(6) 0.091(8) 0.059(6) 0.029(6) 0.021(5) 0.029(6)
C21 0.022(4) 0.027(5) 0.039(5) 0.011(4) -0.005(3) -0.001(3)
C22 0.030(4) 0.028(5) 0.040(5) 0.018(4) -0.001(4) -0.004(4)
C23 0.031(5) 0.036(6) 0.087(7) 0.011(5) -0.021(5) -0.001(4)
C24 0.047(6) 0.033(6) 0.097(8) 0.008(6) -0.008(6) 0.000(5)
C25 0.067(7) 0.031(5) 0.063(6) 0.012(5) 0.006(5) 0.008(5)
C26 0.099(9) 0.039(6) 0.062(7) 0.017(5) -0.039(6) -0.033(6)
C27 0.061(6) 0.062(7) 0.061(6) 0.040(6) -0.028(5) -0.015(5)
C28 0.029(4) 0.050(6) 0.037(5) 0.020(4) 0.001(4) 0.006(4)
C29 0.030(4) 0.042(5) 0.039(5) 0.026(4) 0.007(4) 0.006(4)
C30 0.050(6) 0.045(6) 0.069(6) 0.029(5) -0.007(5) -0.001(5)
C31 0.081(7) 0.068(7) 0.045(6) 0.034(5) 0.017(5) 0.033(6)
C32 0.135(11) 0.068(8) 0.038(6) -0.003(6) 0.024(6) -0.012(7)
C33 0.060(7) 0.081(9) 0.086(8) 0.023(7) 0.024(6) 0.023(6)
C34 0.074(7) 0.054(7) 0.037(5) 0.003(5) 0.019(5) 0.003(5)
C35 0.020(4) 0.056(6) 0.036(5) 0.018(4) -0.002(4) 0.005(4)
C36 0.026(4) 0.030(5) 0.051(6) 0.010(4) -0.018(4) 0.000(4)
C37 0.028(5) 0.053(6) 0.049(5) 0.031(5) -0.006(4) 0.004(4)
C38 0.041(5) 0.031(5) 0.028(4) 0.008(4) -0.009(4) -0.002(4)
C39 0.017(4) 0.038(5) 0.048(5) 0.013(4) -0.009(4) 0.000(4)
C40 0.043(6) 0.076(8) 0.069(7) 0.022(6) 0.017(5) 0.020(5)
Ti101 0.0257(8) 0.0316(9) 0.0263(8) 0.0098(7) 0.0015(6) -0.0001(6)
Ti102 0.0259(8) 0.0331(9) 0.0253(8) 0.0061(7) -0.0000(6) 0.0013(6)
N101 0.033(4) 0.024(4) 0.027(4) 0.007(3) 0.007(3) -0.006(3)
N102 0.039(4) 0.031(4) 0.028(4) 0.010(3) 0.003(3) -0.007(3)
N103 0.043(4) 0.053(5) 0.038(4) 0.021(4) 0.007(3) -0.009(4)
N104 0.027(4) 0.033(4) 0.029(4) 0.007(3) 0.007(3) 0.001(3)
N105 0.043(4) 0.043(4) 0.019(3) 0.011(3) 0.004(3) 0.005(3)
N106 0.039(4) 0.055(5) 0.031(4) 0.027(4) -0.000(3) -0.006(4)
O101 0.028(3) 0.029(3) 0.028(3) 0.012(2) 0.002(2) 0.005(2)
O102 0.027(3) 0.039(3) 0.028(3) 0.010(2) 0.006(2) 0.003(2)
Si101 0.0438(14) 0.0334(14) 0.0302(12) 0.0066(11) 0.008(1) -0.0006(11)
Si102 0.0363(13) 0.0423(15) 0.0278(12) 0.0090(11) 0.009(1) 0.0012(11)
C101 0.019(4) 0.042(5) 0.034(5) 0.017(4) -0.008(3) 0.001(4)
C102 0.019(4) 0.034(5) 0.035(4) 0.011(4) -0.004(3) -0.005(3)
C103 0.050(6) 0.030(5) 0.034(5) 0.010(4) 0.002(4) 0.003(4)
C104 0.036(5) 0.042(6) 0.044(5) 0.024(4) -0.001(4) -0.005(4)
C105 0.062(6) 0.024(5) 0.047(5) 0.016(4) -0.001(4) -0.005(4)
C106 0.041(6) 0.041(6) 0.070(6) 0.025(5) 0.010(5) 0.008(4)
C107 0.028(5) 0.038(6) 0.051(5) 0.013(4) 0.000(4) 0.000(4)
C108 0.041(5) 0.050(6) 0.038(5) 0.022(4) 0.004(4) -0.007(4)
C109 0.040(5) 0.064(7) 0.059(6) 0.035(5) 0.010(5) -0.006(5)
C110 0.059(7) 0.078(8) 0.078(8) 0.045(7) 0.014(6) 0.011(6)
C111 0.141(12) 0.08(1) 0.09(1) 0.031(8) 0.039(9) 0.033(9)
C112 0.089(8) 0.035(6) 0.046(6) 0.012(5) 0.005(5) -0.015(5)
C113 0.061(7) 0.072(8) 0.063(7) 0.013(6) 0.026(5) 0.012(6)
C114 0.064(6) 0.032(5) 0.041(5) 0.013(4) 0.007(4) -0.016(4)
C115 0.027(5) 0.060(7) 0.031(5) 0.009(4) -0.007(4) 0.002(4)
C116 0.029(5) 0.069(7) 0.055(6) 0.036(5) -0.006(4) -0.002(5)
C117 0.030(5) 0.053(6) 0.052(6) -0.003(5) -0.016(4) 0.004(4)
C118 0.023(5) 0.088(8) 0.042(5) 0.018(6) 0.005(4) -0.016(5)
C119 0.037(5) 0.039(6) 0.053(6) 0.019(5) -0.003(4) -0.018(4)
C120 0.048(6) 0.070(7) 0.042(5) 0.014(5) -0.010(4) 0.005(5)
C121 0.034(5) 0.025(5) 0.034(5) 0.010(4) -0.000(4) 0.007(4)
C122 0.037(5) 0.029(5) 0.025(4) 0.015(4) 0.005(3) 0.001(4)
C123 0.031(5) 0.037(5) 0.027(4) 0.013(4) 0.002(3) 0.004(4)
C124 0.041(5) 0.063(7) 0.024(4) -0.002(5) 0.003(4) -0.000(5)
C125 0.070(7) 0.036(6) 0.035(5) -0.002(4) 0.015(5) -0.009(5)
C126 0.056(6) 0.025(5) 0.059(6) 0.017(5) 0.012(5) 0.004(4)
C127 0.032(5) 0.036(5) 0.045(5) 0.022(4) -0.001(4) 0.007(4)
C128 0.033(5) 0.046(5) 0.032(4) 0.012(4) 0.007(4) -0.004(4)
C129 0.046(5) 0.056(6) 0.045(5) 0.029(5) 0.015(4) 0.017(5)
C130 0.110(9) 0.064(8) 0.040(6) 0.005(6) 0.006(6) 0.012(7)
C131 0.067(7) 0.084(8) 0.074(7) 0.055(7) 0.005(6) 0.004(6)
C132 0.057(6) 0.052(6) 0.028(5) 0.008(4) -0.001(4) -0.013(5)
C133 0.065(7) 0.073(8) 0.048(6) 0.027(5) 0.015(5) 0.003(6)
C134 0.049(6) 0.074(7) 0.039(5) 0.006(5) 0.012(4) 0.012(5)
C135 0.029(5) 0.049(6) 0.041(5) 0.013(4) -0.003(4) -0.002(4)
C136 0.033(5) 0.063(7) 0.044(6) 0.023(5) -0.019(4) -0.017(4)
C137 0.029(5) 0.079(8) 0.045(6) 0.015(6) 0.002(4) -0.010(5)
C138 0.015(4) 0.062(7) 0.060(7) -0.007(6) -0.009(4) 0.004(4)
C139 0.031(5) 0.047(6) 0.063(6) 0.031(5) -0.014(4) 0.001(4)
C140 0.046(6) 0.098(9) 0.037(5) -0.009(6) -0.019(4) 0.009(6)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ti2 . Ti1 . N1 . 118.88(17) yes
Ti2 . Ti1 . N2 . 110.52(17) yes
N1 . Ti1 . N2 . 61.7(2) yes
Ti2 . Ti1 . O1 . 42.75(14) yes
N1 . Ti1 . O1 . 90.1(2) yes
N2 . Ti1 . O1 . 126.2(2) yes
Ti2 . Ti1 . O2 . 40.42(15) yes
N1 . Ti1 . O2 . 135.8(2) yes
N2 . Ti1 . O2 . 87.8(2) yes
O1 . Ti1 . O2 . 83.2(2) yes
Ti2 . Ti1 . C15 . 115.6(2) yes
N1 . Ti1 . C15 . 125.4(3) yes
N2 . Ti1 . C15 . 96.3(3) yes
O1 . Ti1 . C15 . 135.5(3) yes
O2 . Ti1 . C15 . 86.5(2) yes
Ti2 . Ti1 . C16 . 149.2(2) yes
N1 . Ti1 . C16 . 91.9(3) yes
N2 . Ti1 . C16 . 81.8(3) yes
O1 . Ti1 . C16 . 148.2(3) yes
O2 . Ti1 . C16 . 116.0(2) yes
Ti2 . Ti1 . C17 . 145.6(2) yes
N1 . Ti1 . C17 . 79.9(3) yes
N2 . Ti1 . C17 . 103.7(3) yes
O1 . Ti1 . C17 . 115.7(3) yes
O2 . Ti1 . C17 . 141.6(2) yes
Ti2 . Ti1 . C18 . 112.0(2) yes
N1 . Ti1 . C18 . 103.7(3) yes
N2 . Ti1 . C18 . 136.5(3) yes
O1 . Ti1 . C18 . 92.0(3) yes
O2 . Ti1 . C18 . 120.1(3) yes
Ti2 . Ti1 . C19 . 97.4(2) yes
N1 . Ti1 . C19 . 135.5(3) yes
N2 . Ti1 . C19 . 130.5(3) yes
O1 . Ti1 . C19 . 102.1(3) yes
O2 . Ti1 . C19 . 88.4(2) yes
C15 . Ti1 . C16 . 33.6(3) yes
C15 . Ti1 . C17 . 56.2(3) yes
C16 . Ti1 . C17 . 34.1(3) yes
C15 . Ti1 . C18 . 57.0(3) yes
C16 . Ti1 . C18 . 56.7(3) yes
C17 . Ti1 . C18 . 33.7(3) yes
C15 . Ti1 . C19 . 34.3(3) yes
C16 . Ti1 . C19 . 56.3(3) yes
C17 . Ti1 . C19 . 56.1(3) yes
C18 . Ti1 . C19 . 34.4(3) yes
Ti1 . Ti2 . N4 . 120.65(17) yes
Ti1 . Ti2 . N5 . 110.52(18) yes
N4 . Ti2 . N5 . 61.7(2) yes
Ti1 . Ti2 . O1 . 40.44(15) yes
N4 . Ti2 . O1 . 136.7(2) yes
N5 . Ti2 . O1 . 87.3(2) yes
Ti1 . Ti2 . O2 . 42.60(15) yes
N4 . Ti2 . O2 . 90.5(2) yes
N5 . Ti2 . O2 . 124.8(2) yes
O1 . Ti2 . O2 . 83.0(2) yes
Ti1 . Ti2 . C35 . 113.6(2) yes
N4 . Ti2 . C35 . 125.7(3) yes
N5 . Ti2 . C35 . 98.0(3) yes
O1 . Ti2 . C35 . 85.6(2) yes
O2 . Ti2 . C35 . 134.8(3) yes
Ti1 . Ti2 . C36 . 96.0(2) yes
N4 . Ti2 . C36 . 134.5(3) yes
N5 . Ti2 . C36 . 132.4(3) yes
O1 . Ti2 . C36 . 88.6(2) yes
O2 . Ti2 . C36 . 101.6(3) yes
Ti1 . Ti2 . C37 . 112.2(2) yes
N4 . Ti2 . C37 . 102.0(3) yes
N5 . Ti2 . C37 . 136.5(3) yes
O1 . Ti2 . C37 . 121.0(3) yes
O2 . Ti2 . C37 . 93.2(3) yes
Ti1 . Ti2 . C38 . 146.4(2) yes
N4 . Ti2 . C38 . 78.7(2) yes
N5 . Ti2 . C38 . 102.9(3) yes
O1 . Ti2 . C38 . 141.3(2) yes
O2 . Ti2 . C38 . 118.0(3) yes
Ti1 . Ti2 . C39 . 146.74(19) yes
N4 . Ti2 . C39 . 92.6(3) yes
N5 . Ti2 . C39 . 82.9(3) yes
O1 . Ti2 . C39 . 114.1(2) yes
O2 . Ti2 . C39 . 149.3(3) yes
C35 . Ti2 . C36 . 34.4(3) yes
C35 . Ti2 . C37 . 56.9(3) yes
C36 . Ti2 . C37 . 34.5(3) yes
C35 . Ti2 . C38 . 56.2(3) yes
C36 . Ti2 . C38 . 56.8(3) yes
C37 . Ti2 . C38 . 34.2(3) yes
C35 . Ti2 . C39 . 33.2(3) yes
C36 . Ti2 . C39 . 56.2(3) yes
C37 . Ti2 . C39 . 56.4(3) yes
C38 . Ti2 . C39 . 33.9(3) yes
Ti1 . N1 . Si1 . 138.3(4) yes
Ti1 . N1 . C1 . 91.4(4) yes
Si1 . N1 . C1 . 129.7(5) yes
Ti1 . N2 . C1 . 94.7(5) yes
Ti1 . N2 . C8 . 140.9(5) yes
C1 . N2 . C8 . 124.4(7) yes
C9 . N3 . C10 . 110.6(7) yes
C9 . N3 . C11 . 110.2(7) yes
C10 . N3 . C11 . 108.9(7) yes
Ti2 . N4 . Si2 . 135.4(4) yes
Ti2 . N4 . C21 . 90.6(4) yes
Si2 . N4 . C21 . 131.1(5) yes
Ti2 . N5 . C21 . 94.5(5) yes
Ti2 . N5 . C28 . 140.8(5) yes
C21 . N5 . C28 . 124.6(7) yes
C29 . N6 . C30 . 111.4(7) yes
C29 . N6 . C31 . 111.0(7) yes
C30 . N6 . C31 . 108.4(7) yes
Ti1 . O1 . Ti2 . 96.8(2) yes
Ti1 . O2 . Ti2 . 97.0(2) yes
N1 . Si1 . C12 . 113.1(4) yes
N1 . Si1 . C13 . 110.5(4) yes
C12 . Si1 . C13 . 108.5(5) yes
N1 . Si1 . C14 . 106.8(3) yes
C12 . Si1 . C14 . 108.9(4) yes
C13 . Si1 . C14 . 109.0(5) yes
N4 . Si2 . C32 . 113.7(4) yes
N4 . Si2 . C33 . 110.3(4) yes
C32 . Si2 . C33 . 107.0(5) yes
N4 . Si2 . C34 . 107.2(4) yes
C32 . Si2 . C34 . 109.4(5) yes
C33 . Si2 . C34 . 109.2(5) yes
N1 . C1 . N2 . 112.1(7) yes
N1 . C1 . C2 . 124.7(6) yes
N2 . C1 . C2 . 123.1(7) yes
C1 . C2 . C3 . 121.5(7) yes
C1 . C2 . C7 . 119.5(7) yes
C3 . C2 . C7 . 119.0(8) yes
C2 . C3 . C4 . 121.1(9) yes
C3 . C4 . C5 . 118.0(9) yes
C4 . C5 . C6 . 120.6(9) yes
C5 . C6 . C7 . 120.1(9) yes
C2 . C7 . C6 . 121.1(8) yes
N2 . C8 . C9 . 109.6(6) yes
N3 . C9 . C8 . 113.3(7) yes
Ti1 . C15 . C16 . 74.4(4) yes
Ti1 . C15 . C19 . 69.3(4) yes
C16 . C15 . C19 . 107.0(7) yes
Ti1 . C15 . C20 . 122.2(6) yes
C16 . C15 . C20 . 125.2(9) yes
C19 . C15 . C20 . 127.8(9) yes
Ti1 . C16 . C15 . 72.0(4) yes
Ti1 . C16 . C17 . 70.6(4) yes
C15 . C16 . C17 . 106.5(8) yes
Ti1 . C17 . C16 . 75.3(4) yes
Ti1 . C17 . C18 . 71.3(4) yes
C16 . C17 . C18 . 109.3(8) yes
Ti1 . C18 . C17 . 75.0(5) yes
Ti1 . C18 . C19 . 72.3(5) yes
C17 . C18 . C19 . 107.5(8) yes
Ti1 . C19 . C15 . 76.4(5) yes
Ti1 . C19 . C18 . 73.4(4) yes
C15 . C19 . C18 . 109.7(8) yes
N4 . C21 . N5 . 113.1(7) yes
N4 . C21 . C22 . 124.3(7) yes
N5 . C21 . C22 . 122.5(7) yes
C21 . C22 . C23 . 121.1(7) yes
C21 . C22 . C27 . 120.7(7) yes
C23 . C22 . C27 . 118.2(8) yes
C22 . C23 . C24 . 119.9(8) yes
C23 . C24 . C25 . 121.2(10) yes
C24 . C25 . C26 . 119.9(9) yes
C25 . C26 . C27 . 120.5(9) yes
C22 . C27 . C26 . 120.2(9) yes
N5 . C28 . C29 . 109.3(6) yes
N6 . C29 . C28 . 111.7(7) yes
Ti2 . C35 . C36 . 69.8(4) yes
Ti2 . C35 . C39 . 73.8(4) yes
C36 . C35 . C39 . 107.1(7) yes
Ti2 . C35 . C40 . 120.6(5) yes
C36 . C35 . C40 . 126.8(8) yes
C39 . C35 . C40 . 126.0(9) yes
Ti2 . C36 . C35 . 75.9(4) yes
Ti2 . C36 . C37 . 73.7(4) yes
C35 . C36 . C37 . 108.8(7) yes
Ti2 . C37 . C36 . 71.8(4) yes
Ti2 . C37 . C38 . 73.9(4) yes
C36 . C37 . C38 . 107.4(8) yes
Ti2 . C38 . C37 . 71.9(4) yes
Ti2 . C38 . C39 . 74.6(4) yes
C37 . C38 . C39 . 107.9(7) yes
Ti2 . C39 . C35 . 73.0(4) yes
Ti2 . C39 . C38 . 71.5(4) yes
C35 . C39 . C38 . 108.7(8) yes
Ti102 . Ti101 . N101 . 122.15(16) yes
Ti102 . Ti101 . N102 . 104.73(18) yes
N101 . Ti101 . N102 . 61.4(2) yes
Ti102 . Ti101 . O101 . 43.48(15) yes
N101 . Ti101 . O101 . 91.7(2) yes
N102 . Ti101 . O101 . 119.5(2) yes
Ti102 . Ti101 . O102 . 39.91(15) yes
N101 . Ti101 . O102 . 138.6(2) yes
N102 . Ti101 . O102 . 85.5(2) yes
O101 . Ti101 . O102 . 83.4(2) yes
Ti102 . Ti101 . C115 . 98.6(2) yes
N101 . Ti101 . C115 . 137.7(3) yes
N102 . Ti101 . C115 . 122.1(3) yes
O101 . Ti101 . C115 . 114.0(3) yes
O102 . Ti101 . C115 . 79.8(2) yes
Ti102 . Ti101 . C116 . 126.9(2) yes
N101 . Ti101 . C116 . 110.6(3) yes
N102 . Ti101 . C116 . 94.2(3) yes
O101 . Ti101 . C116 . 145.9(3) yes
O102 . Ti101 . C116 . 94.9(3) yes
Ti102 . Ti101 . C117 . 154.2(2) yes
N101 . Ti101 . C117 . 81.6(3) yes
N102 . Ti101 . C117 . 95.5(3) yes
O101 . Ti101 . C117 . 135.7(3) yes
O102 . Ti101 . C117 . 128.7(3) yes
Ti102 . Ti101 . C118 . 129.0(3) yes
N101 . Ti101 . C118 . 86.6(3) yes
N102 . Ti101 . C118 . 126.3(3) yes
O101 . Ti101 . C118 . 102.1(3) yes
O102 . Ti101 . C118 . 134.6(3) yes
Ti102 . Ti101 . C119 . 99.7(2) yes
N101 . Ti101 . C119 . 119.5(3) yes
N102 . Ti101 . C119 . 148.8(3) yes
O101 . Ti101 . C119 . 91.6(3) yes
O102 . Ti101 . C119 . 101.7(3) yes
C115 . Ti101 . C116 . 33.4(3) yes
C115 . Ti101 . C117 . 56.4(3) yes
C116 . Ti101 . C117 . 33.8(3) yes
C115 . Ti101 . C118 . 56.5(3) yes
C116 . Ti101 . C118 . 56.0(3) yes
C117 . Ti101 . C118 . 34.2(3) yes
C115 . Ti101 . C119 . 33.5(3) yes
C116 . Ti101 . C119 . 55.2(3) yes
C117 . Ti101 . C119 . 56.2(3) yes
C118 . Ti101 . C119 . 34.1(3) yes
Ti101 . Ti102 . N104 . 122.52(16) yes
Ti101 . Ti102 . N105 . 104.39(18) yes
N104 . Ti102 . N105 . 61.8(2) yes
Ti101 . Ti102 . O101 . 39.85(15) yes
N104 . Ti102 . O101 . 138.1(2) yes
N105 . Ti102 . O101 . 84.5(2) yes
Ti101 . Ti102 . O102 . 43.32(15) yes
N104 . Ti102 . O102 . 91.4(2) yes
N105 . Ti102 . O102 . 118.3(2) yes
O101 . Ti102 . O102 . 83.2(2) yes
Ti101 . Ti102 . C135 . 100.4(2) yes
N104 . Ti102 . C135 . 136.1(3) yes
N105 . Ti102 . C135 . 119.8(3) yes
O101 . Ti102 . C135 . 81.0(2) yes
O102 . Ti102 . C135 . 117.4(3) yes
Ti101 . Ti102 . C136 . 98.4(2) yes
N104 . Ti102 . C136 . 121.1(3) yes
N105 . Ti102 . C136 . 149.2(3) yes
O101 . Ti102 . C136 . 100.7(3) yes
O102 . Ti102 . C136 . 92.5(3) yes
Ti101 . Ti102 . C137 . 127.1(3) yes
N104 . Ti102 . C137 . 87.3(3) yes
N105 . Ti102 . C137 . 128.5(3) yes
O101 . Ti102 . C137 . 134.5(3) yes
O102 . Ti102 . C137 . 101.3(3) yes
Ti101 . Ti102 . C138 . 153.6(2) yes
N104 . Ti102 . C138 . 80.8(3) yes
N105 . Ti102 . C138 . 97.6(3) yes
O101 . Ti102 . C138 . 130.8(3) yes
O102 . Ti102 . C138 . 134.1(3) yes
Ti101 . Ti102 . C139 . 129.3(2) yes
N104 . Ti102 . C139 . 107.8(3) yes
N105 . Ti102 . C139 . 93.1(3) yes
O101 . Ti102 . C139 . 97.4(3) yes
O102 . Ti102 . C139 . 148.5(3) yes
C135 . Ti102 . C136 . 34.1(3) yes
C135 . Ti102 . C137 . 56.5(3) yes
C136 . Ti102 . C137 . 34.5(3) yes
C135 . Ti102 . C138 . 55.3(3) yes
C136 . Ti102 . C138 . 56.1(3) yes
C137 . Ti102 . C138 . 33.7(3) yes
C135 . Ti102 . C139 . 33.2(3) yes
C136 . Ti102 . C139 . 56.3(3) yes
C137 . Ti102 . C139 . 56.4(3) yes
C138 . Ti102 . C139 . 33.5(3) yes
Ti101 . N101 . Si101 . 137.3(4) yes
Ti101 . N101 . C101 . 90.8(4) yes
Si101 . N101 . C101 . 131.8(5) yes
Ti101 . N102 . C101 . 95.8(5) yes
Ti101 . N102 . C108 . 138.5(5) yes
C101 . N102 . C108 . 125.2(7) yes
C109 . N103 . C110 . 111.5(7) yes
C109 . N103 . C111 . 112.3(8) yes
C110 . N103 . C111 . 108.2(8) yes
Ti102 . N104 . Si102 . 137.6(4) yes
Ti102 . N104 . C121 . 91.2(4) yes
Si102 . N104 . C121 . 131.0(5) yes
Ti102 . N105 . C121 . 96.2(5) yes
Ti102 . N105 . C128 . 139.3(5) yes
C121 . N105 . C128 . 124.3(7) yes
C129 . N106 . C130 . 112.4(8) yes
C129 . N106 . C131 . 110.1(7) yes
C130 . N106 . C131 . 108.8(7) yes
Ti101 . O101 . Ti102 . 96.7(2) yes
Ti101 . O102 . Ti102 . 96.8(2) yes
N101 . Si101 . C112 . 113.8(4) yes
N101 . Si101 . C113 . 109.5(4) yes
C112 . Si101 . C113 . 110.2(5) yes
N101 . Si101 . C114 . 107.1(3) yes
C112 . Si101 . C114 . 107.7(4) yes
C113 . Si101 . C114 . 108.4(5) yes
N104 . Si102 . C132 . 114.8(4) yes
N104 . Si102 . C133 . 107.7(4) yes
C132 . Si102 . C133 . 107.6(4) yes
N104 . Si102 . C134 . 109.6(4) yes
C132 . Si102 . C134 . 108.4(4) yes
C133 . Si102 . C134 . 108.7(5) yes
N101 . C101 . N102 . 111.9(7) yes
N101 . C101 . C102 . 124.2(7) yes
N102 . C101 . C102 . 123.9(7) yes
C101 . C102 . C103 . 120.8(7) yes
C101 . C102 . C107 . 118.9(7) yes
C103 . C102 . C107 . 120.3(7) yes
C102 . C103 . C104 . 119.6(8) yes
C103 . C104 . C105 . 120.7(8) yes
C104 . C105 . C106 . 119.4(8) yes
C105 . C106 . C107 . 119.3(8) yes
C102 . C107 . C106 . 120.6(8) yes
N102 . C108 . C109 . 111.8(7) yes
N103 . C109 . C108 . 113.1(7) yes
Ti101 . C115 . C116 . 73.1(5) yes
Ti101 . C115 . C119 . 71.0(4) yes
C116 . C115 . C119 . 106.3(8) yes
Ti101 . C115 . C120 . 121.6(5) yes
C116 . C115 . C120 . 125.3(9) yes
C119 . C115 . C120 . 128.5(9) yes
Ti101 . C116 . C115 . 73.5(5) yes
Ti101 . C116 . C117 . 71.5(5) yes
C115 . C116 . C117 . 109.2(8) yes
Ti101 . C117 . C116 . 74.7(5) yes
Ti101 . C117 . C118 . 72.2(5) yes
C116 . C117 . C118 . 107.4(8) yes
Ti101 . C118 . C117 . 73.7(5) yes
Ti101 . C118 . C119 . 73.3(5) yes
C117 . C118 . C119 . 107.3(8) yes
Ti101 . C119 . C115 . 75.5(5) yes
Ti101 . C119 . C118 . 72.7(5) yes
C115 . C119 . C118 . 109.9(8) yes
N104 . C121 . N105 . 110.7(7) yes
N104 . C121 . C122 . 125.1(7) yes
N105 . C121 . C122 . 124.1(7) yes
C121 . C122 . C123 . 122.6(7) yes
C121 . C122 . C127 . 120.1(7) yes
C123 . C122 . C127 . 117.1(7) yes
C122 . C123 . C124 . 120.6(7) yes
C123 . C124 . C125 . 120.8(8) yes
C124 . C125 . C126 . 119.4(8) yes
C125 . C126 . C127 . 120.2(8) yes
C122 . C127 . C126 . 121.8(8) yes
N105 . C128 . C129 . 112.4(6) yes
N106 . C129 . C128 . 111.9(6) yes
Ti102 . C135 . C136 . 70.4(5) yes
Ti102 . C135 . C139 . 74.1(5) yes
C136 . C135 . C139 . 108.3(8) yes
Ti102 . C135 . C140 . 121.1(5) yes
C136 . C135 . C140 . 124.9(9) yes
C139 . C135 . C140 . 126.8(9) yes
Ti102 . C136 . C135 . 75.5(5) yes
Ti102 . C136 . C137 . 73.7(5) yes
C135 . C136 . C137 . 108.1(9) yes
Ti102 . C137 . C136 . 71.9(5) yes
Ti102 . C137 . C138 . 74.1(5) yes
C136 . C137 . C138 . 106.7(8) yes
Ti102 . C138 . C137 . 72.3(5) yes
Ti102 . C138 . C139 . 74.6(5) yes
C137 . C138 . C139 . 109.8(8) yes
Ti102 . C139 . C135 . 72.8(5) yes
Ti102 . C139 . C138 . 71.8(5) yes
C135 . C139 . C138 . 107.0(9) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . Ti2 . 2.7749(18) yes
Ti1 . N1 . 2.180(6) yes
Ti1 . N2 . 2.123(6) yes
Ti1 . O1 . 1.813(5) yes
Ti1 . O2 . 1.892(5) yes
Ti1 . C15 . 2.441(8) yes
Ti1 . C16 . 2.472(8) yes
Ti1 . C17 . 2.410(7) yes
Ti1 . C18 . 2.364(8) yes
Ti1 . C19 . 2.350(8) yes
Ti2 . N4 . 2.202(6) yes
Ti2 . N5 . 2.116(7) yes
Ti2 . O1 . 1.897(5) yes
Ti2 . O2 . 1.813(5) yes
Ti2 . C35 . 2.428(7) yes
Ti2 . C36 . 2.349(7) yes
Ti2 . C37 . 2.374(8) yes
Ti2 . C38 . 2.399(7) yes
Ti2 . C39 . 2.439(7) yes
N1 . Si1 . 1.720(6) yes
N1 . C1 . 1.34(1) yes
N2 . C1 . 1.317(9) yes
N2 . C8 . 1.460(9) yes
N3 . C9 . 1.44(1) yes
N3 . C10 . 1.478(11) yes
N3 . C11 . 1.450(11) yes
N4 . Si2 . 1.717(6) yes
N4 . C21 . 1.33(1) yes
N5 . C21 . 1.327(9) yes
N5 . C28 . 1.45(1) yes
N6 . C29 . 1.46(1) yes
N6 . C30 . 1.47(1) yes
N6 . C31 . 1.448(11) yes
Si1 . C12 . 1.854(8) yes
Si1 . C13 . 1.864(9) yes
Si1 . C14 . 1.869(8) yes
Si2 . C32 . 1.85(1) yes
Si2 . C33 . 1.87(1) yes
Si2 . C34 . 1.83(1) yes
C1 . C2 . 1.50(1) yes
C2 . C3 . 1.373(11) yes
C2 . C7 . 1.383(11) yes
C3 . C4 . 1.386(13) yes
C4 . C5 . 1.395(12) yes
C5 . C6 . 1.375(12) yes
C6 . C7 . 1.347(12) yes
C8 . C9 . 1.53(1) yes
C15 . C16 . 1.419(11) yes
C15 . C19 . 1.414(12) yes
C15 . C20 . 1.481(11) yes
C16 . C17 . 1.433(12) yes
C17 . C18 . 1.385(11) yes
C18 . C19 . 1.393(11) yes
C21 . C22 . 1.495(11) yes
C22 . C23 . 1.380(11) yes
C22 . C27 . 1.382(11) yes
C23 . C24 . 1.395(12) yes
C24 . C25 . 1.337(13) yes
C25 . C26 . 1.353(13) yes
C26 . C27 . 1.395(13) yes
C28 . C29 . 1.53(1) yes
C35 . C36 . 1.414(12) yes
C35 . C39 . 1.390(11) yes
C35 . C40 . 1.512(11) yes
C36 . C37 . 1.400(11) yes
C37 . C38 . 1.403(11) yes
C38 . C39 . 1.410(11) yes
Ti101 . Ti102 . 2.7653(17) yes
Ti101 . N101 . 2.207(6) yes
Ti101 . N102 . 2.086(7) yes
Ti101 . O101 . 1.784(5) yes
Ti101 . O102 . 1.910(5) yes
Ti101 . C115 . 2.440(8) yes
Ti101 . C116 . 2.436(8) yes
Ti101 . C117 . 2.395(8) yes
Ti101 . C118 . 2.375(8) yes
Ti101 . C119 . 2.383(8) yes
Ti102 . N104 . 2.211(6) yes
Ti102 . N105 . 2.091(7) yes
Ti102 . O101 . 1.916(5) yes
Ti102 . O102 . 1.787(5) yes
Ti102 . C135 . 2.419(8) yes
Ti102 . C136 . 2.354(8) yes
Ti102 . C137 . 2.377(9) yes
Ti102 . C138 . 2.400(8) yes
Ti102 . C139 . 2.435(8) yes
N101 . Si101 . 1.737(6) yes
N101 . C101 . 1.32(1) yes
N102 . C101 . 1.332(9) yes
N102 . C108 . 1.46(1) yes
N103 . C109 . 1.46(1) yes
N103 . C110 . 1.426(11) yes
N103 . C111 . 1.432(12) yes
N104 . Si102 . 1.730(6) yes
N104 . C121 . 1.34(1) yes
N105 . C121 . 1.349(9) yes
N105 . C128 . 1.46(1) yes
N106 . C129 . 1.45(1) yes
N106 . C130 . 1.412(11) yes
N106 . C131 . 1.458(11) yes
Si101 . C112 . 1.881(9) yes
Si101 . C113 . 1.879(9) yes
Si101 . C114 . 1.865(8) yes
Si102 . C132 . 1.849(8) yes
Si102 . C133 . 1.85(1) yes
Si102 . C134 . 1.863(8) yes
C101 . C102 . 1.501(11) yes
C102 . C103 . 1.40(1) yes
C102 . C107 . 1.38(1) yes
C103 . C104 . 1.367(11) yes
C104 . C105 . 1.395(11) yes
C105 . C106 . 1.404(12) yes
C106 . C107 . 1.379(12) yes
C108 . C109 . 1.475(11) yes
C115 . C116 . 1.401(12) yes
C115 . C119 . 1.392(12) yes
C115 . C120 . 1.481(11) yes
C116 . C117 . 1.404(12) yes
C117 . C118 . 1.401(13) yes
C118 . C119 . 1.394(12) yes
C121 . C122 . 1.466(11) yes
C122 . C123 . 1.39(1) yes
C122 . C127 . 1.39(1) yes
C123 . C124 . 1.381(11) yes
C124 . C125 . 1.370(12) yes
C125 . C126 . 1.370(12) yes
C126 . C127 . 1.365(11) yes
C128 . C129 . 1.496(11) yes
C135 . C136 . 1.401(12) yes
C135 . C139 . 1.386(12) yes
C135 . C140 . 1.526(11) yes
C136 . C137 . 1.401(12) yes
C137 . C138 . 1.383(13) yes
C138 . C139 . 1.395(12) yes
|
1100811.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100811.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100811
loop_
_publ_author_name
'Boyd, Catherine L.'
'Clot, Eric'
'Guiducci, Aldo E.'
'Mountford, Philip'
_publ_section_title
;
Pendant Arm Functionalized Benzamidinate Titanium Imido Compounds:
Experimental and Computational Studies of Their Reactions with CO~2~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2347
_journal_page_last 2367
_journal_paper_doi 10.1021/om049026f
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C42 H66 N6 O2 Si2 Ti2'
_chemical_formula_sum 'C42 H66 N6 O2 Si2 Ti2'
_chemical_formula_weight 838.99
_chemical_name_systematic
;
[Ti2(mu-O)2(C5H4Me)2{Me3SiNC(C6H5)NCH2CH2CH2NMe2}2]
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_cell_angle_alpha 72.8419(8)
_cell_angle_beta 76.2046(8)
_cell_angle_gamma 72.8192(9)
_cell_formula_units_Z 1
_cell_length_a 9.3597(2)
_cell_length_b 10.7886(2)
_cell_length_c 12.1749(3)
_cell_measurement_reflns_used 4378
_cell_measurement_temperature 150
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 2.910
_cell_volume 1106.74(4)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al, 1996)'
_computing_structure_solution 'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature 150
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method 2\q/\w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.02
_diffrn_reflns_av_sigmaI/netI 0.069
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 9040
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 3.01
_diffrn_standards_decay_% 'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time 'not measured'
_diffrn_standards_number 'not measured'
_exptl_absorpt_coefficient_mu 0.45
_exptl_absorpt_correction_T_max 0.914
_exptl_absorpt_correction_T_min 0.874
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.26
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description plate
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.31
_refine_diff_density_min -0.31
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 127.4(354)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs 1.076
_refine_ls_hydrogen_treatment 'riding model'
_refine_ls_matrix_type full
_refine_ls_number_parameters 245
_refine_ls_number_reflns 3814
_refine_ls_number_restraints 0
_refine_ls_R_factor_obs 0.0367
_refine_ls_shift/esd_max 0.0025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme 'Chebychev polynomial'
_refine_ls_wR_factor_obs 0.0387
_reflns_limit_h_max 12
_reflns_limit_h_min -11
_reflns_limit_k_max 13
_reflns_limit_k_min -13
_reflns_limit_l_max 15
_reflns_limit_l_min 0
_reflns_number_observed 3814
_reflns_number_total 4955
_reflns_observed_criterion >3.00\s(I)
_cod_data_source_file om049026fsi20041209_070538.cif
_cod_data_source_block 11a
_cod_depositor_comments
;
Changing the values of the _chemical_formula_sum and _chemical_formula_moiety
from ' C44 H66 N6 O2 Si2 Ti2' to 'C42 H66 N6 O2 Si2 Ti2' after consulting the
original publication.
Antanas Vaitkus,
2017-09-09
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.
'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M 'P -1 '
_cod_original_formula_moiety ' C44 H66 N6 O2 Si2 Ti2'
_cod_original_formula_sum ' C44 H66 N6 O2 Si2 Ti2'
_cod_database_code 1100811
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0229(2) 0.0208(2) 0.0183(2) -0.0063(1) -0.0034(1) -0.0054(1)
N1 0.0243(7) 0.0263(8) 0.0218(7) -0.0077(6) -0.0052(6) -0.0040(6)
N2 0.0233(7) 0.0276(8) 0.0197(7) -0.0069(6) -0.0019(6) -0.0048(6)
N3 0.0336(8) 0.0343(9) 0.0235(8) -0.0084(6) -0.0017(6) -0.0084(7)
O1 0.0222(6) 0.0237(6) 0.0229(6) -0.0048(5) -0.0014(5) -0.0049(5)
Si1 0.0225(2) 0.0302(3) 0.0252(3) -0.0087(2) -0.0036(2) -0.0051(2)
C1 0.0275(8) 0.0185(8) 0.0206(8) -0.0053(6) -0.0036(6) -0.0057(7)
C2 0.0244(8) 0.0269(9) 0.0214(8) -0.0078(7) -0.0026(6) -0.0060(7)
C3 0.038(1) 0.028(1) 0.030(1) -0.0065(8) -0.0100(8) -0.0075(8)
C4 0.046(1) 0.041(1) 0.030(1) -0.0003(8) -0.0144(9) -0.009(1)
C5 0.040(1) 0.057(1) 0.026(1) -0.0130(9) -0.0107(8) -0.011(1)
C6 0.043(1) 0.046(1) 0.039(1) -0.025(1) -0.0083(9) -0.009(1)
C7 0.039(1) 0.030(1) 0.031(1) -0.0112(8) -0.0082(8) -0.0059(8)
C8 0.0261(9) 0.0288(9) 0.0232(8) -0.0097(7) -0.0001(7) -0.0047(7)
C9 0.0299(9) 0.0294(9) 0.0298(9) -0.0102(7) -0.0020(7) -0.0068(8)
C10 0.0297(9) 0.032(1) 0.0270(9) -0.0079(7) -0.0001(7) -0.0105(8)
C11 0.044(1) 0.045(1) 0.029(1) -0.0139(9) 0.0029(9) -0.011(1)
C12 0.050(1) 0.050(1) 0.034(1) -0.010(1) -0.014(1) -0.005(1)
C13 0.030(1) 0.044(1) 0.056(1) -0.003(1) -0.004(1) -0.0004(9)
C14 0.030(1) 0.069(2) 0.032(1) -0.020(1) 0.0022(8) -0.017(1)
C15 0.032(1) 0.051(1) 0.057(1) -0.026(1) -0.001(1) -0.015(1)
C16 0.055(1) 0.0234(9) 0.035(1) -0.0112(8) -0.0204(9) -0.0081(9)
C17 0.032(1) 0.040(1) 0.049(1) -0.025(1) -0.0066(9) -0.0119(9)
C18 0.063(2) 0.033(1) 0.051(1) -0.016(1) -0.036(1) -0.000(1)
C19 0.097(2) 0.046(1) 0.023(1) -0.0153(9) -0.002(1) -0.036(1)
C20 0.030(1) 0.057(1) 0.075(2) -0.054(1) -0.002(1) -0.006(1)
C21 0.155(3) 0.026(1) 0.068(2) -0.002(1) -0.065(2) -0.018(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
Ti1 0.03615(3) 0.36211(3) 0.54027(3) 0.0203 1.0000 Uani
N1 0.2182(2) 0.2654(1) 0.6459(1) 0.0240 1.0000 Uani
N2 -0.0241(2) 0.3221(1) 0.7222(1) 0.0238 1.0000 Uani
N3 -0.3255(2) 0.3319(2) 1.0535(1) 0.0307 1.0000 Uani
O1 0.1359(1) 0.4893(1) 0.4595(1) 0.0237 1.0000 Uani
Si1 0.41383(5) 0.24223(5) 0.62235(4) 0.0259 1.0000 Uani
C1 0.1169(2) 0.2844(2) 0.7408(1) 0.0221 1.0000 Uani
C2 0.1591(2) 0.2667(2) 0.8567(1) 0.0241 1.0000 Uani
C3 0.1997(2) 0.1391(2) 0.9280(2) 0.0316 1.0000 Uani
C4 0.2407(3) 0.1226(2) 1.0346(2) 0.0397 1.0000 Uani
C5 0.2407(2) 0.2319(2) 1.0709(2) 0.0395 1.0000 Uani
C6 0.2002(3) 0.3594(2) 1.0010(2) 0.0395 1.0000 Uani
C7 0.1586(2) 0.3769(2) 0.8943(2) 0.0326 1.0000 Uani
C8 -0.1557(2) 0.3559(2) 0.8101(2) 0.0264 1.0000 Uani
C9 -0.2174(2) 0.2350(2) 0.8792(2) 0.0297 1.0000 Uani
C10 -0.3531(2) 0.2662(2) 0.9741(2) 0.0297 1.0000 Uani
C11 -0.4642(3) 0.3664(2) 1.1348(2) 0.0399 1.0000 Uani
C12 -0.2052(3) 0.2475(2) 1.1184(2) 0.0448 1.0000 Uani
C13 0.5084(3) 0.0768(2) 0.7094(2) 0.0480 1.0000 Uani
C14 0.4835(2) 0.2473(3) 0.4653(2) 0.0421 1.0000 Uani
C15 0.4675(2) 0.3775(2) 0.6586(2) 0.0441 1.0000 Uani
C16 0.0324(3) 0.1333(2) 0.5455(2) 0.0351 1.0000 Uani
C17 -0.1075(2) 0.2171(2) 0.5242(2) 0.0369 1.0000 Uani
C18 -0.0900(3) 0.3104(2) 0.4196(2) 0.0455 1.0000 Uani
C19 0.0606(4) 0.2870(2) 0.3726(2) 0.0513 1.0000 Uani
C20 0.1397(2) 0.1776(3) 0.4496(2) 0.0477 1.0000 Uani
C21 0.0639(5) 0.0204(2) 0.6490(3) 0.0774 1.0000 Uani
H31 0.1997(2) 0.0628(2) 0.9028(2) 0.0424 1.0000 Uiso
H41 0.2690(3) 0.0345(2) 1.0837(2) 0.0532 1.0000 Uiso
H51 0.2688(2) 0.2199(2) 1.1449(2) 0.0530 1.0000 Uiso
H61 0.2008(3) 0.4354(2) 1.0264(2) 0.0559 1.0000 Uiso
H71 0.1291(2) 0.4653(2) 0.8462(2) 0.0464 1.0000 Uiso
H81 -0.1263(2) 0.3909(2) 0.8630(2) 0.0353 1.0000 Uiso
H82 -0.2341(2) 0.4226(2) 0.7722(2) 0.0353 1.0000 Uiso
H91 -0.1380(2) 0.1681(2) 0.9157(2) 0.0409 1.0000 Uiso
H92 -0.2475(2) 0.2010(2) 0.8260(2) 0.0409 1.0000 Uiso
H101 -0.3792(2) 0.1840(2) 1.0188(2) 0.0419 1.0000 Uiso
H102 -0.4367(2) 0.3241(2) 0.9367(2) 0.0419 1.0000 Uiso
H111 -0.4459(3) 0.4094(2) 1.1870(2) 0.0529 1.0000 Uiso
H112 -0.4968(3) 0.2869(2) 1.1788(2) 0.0529 1.0000 Uiso
H113 -0.5417(3) 0.4262(2) 1.0918(2) 0.0529 1.0000 Uiso
H121 -0.1900(3) 0.2936(2) 1.1694(2) 0.0602 1.0000 Uiso
H122 -0.2323(3) 0.1658(2) 1.1635(2) 0.0602 1.0000 Uiso
H123 -0.1134(3) 0.2274(2) 1.0644(2) 0.0602 1.0000 Uiso
H131 0.6161(3) 0.0672(2) 0.6943(2) 0.0566 1.0000 Uiso
H132 0.4711(3) 0.0715(2) 0.7908(2) 0.0566 1.0000 Uiso
H133 0.4862(3) 0.0066(2) 0.6878(2) 0.0566 1.0000 Uiso
H141 0.5917(2) 0.2347(3) 0.4492(2) 0.0550 1.0000 Uiso
H142 0.4372(2) 0.3323(3) 0.4192(2) 0.0550 1.0000 Uiso
H143 0.4573(2) 0.1774(3) 0.4463(2) 0.0550 1.0000 Uiso
H151 0.5759(2) 0.3623(2) 0.6448(2) 0.0641 1.0000 Uiso
H152 0.4291(2) 0.3777(2) 0.7391(2) 0.0641 1.0000 Uiso
H153 0.4248(2) 0.4623(2) 0.6103(2) 0.0641 1.0000 Uiso
H171 -0.2022(2) 0.2102(2) 0.5747(2) 0.0543 1.0000 Uiso
H181 -0.1698(3) 0.3801(2) 0.3862(2) 0.0635 1.0000 Uiso
H191 0.1049(4) 0.3364(2) 0.2995(2) 0.0658 1.0000 Uiso
H201 0.2471(2) 0.1395(3) 0.4392(2) 0.0685 1.0000 Uiso
H211 0.1707(5) -0.0202(2) 0.6413(3) 0.0858 1.0000 Uiso
H212 0.0311(5) 0.0532(2) 0.7184(3) 0.0858 1.0000 Uiso
H213 0.0100(5) -0.0448(2) 0.6540(3) 0.0858 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ti1 2_566 Ti1 . N1 . 119.31(4) yes
Ti1 2_566 Ti1 . N2 . 106.40(4) yes
N1 . Ti1 . N2 . 61.86(6) yes
Ti1 2_566 Ti1 . O1 . 43.14(4) yes
N1 . Ti1 . O1 . 89.88(6) yes
N2 . Ti1 . O1 . 121.90(6) yes
Ti1 2_566 Ti1 . O1 2_566 40.23(4) yes
N1 . Ti1 . O1 2_566 135.49(5) yes
N2 . Ti1 . O1 2_566 84.89(5) yes
O1 . Ti1 . O1 2_566 83.37(5) yes
Ti1 2_566 Ti1 . C16 . 154.47(5) yes
N1 . Ti1 . C16 . 85.51(6) yes
N2 . Ti1 . C16 . 90.08(6) yes
O1 . Ti1 . C16 . 140.37(7) yes
O1 2_566 Ti1 . C16 . 125.68(7) yes
Ti1 2_566 Ti1 . C17 . 124.53(6) yes
N1 . Ti1 . C17 . 115.70(7) yes
N2 . Ti1 . C17 . 92.84(7) yes
O1 . Ti1 . C17 . 144.41(7) yes
O1 2_566 Ti1 . C17 . 93.17(6) yes
Ti1 2_566 Ti1 . C18 . 98.47(6) yes
N1 . Ti1 . C18 . 139.58(7) yes
N2 . Ti1 . C18 . 123.21(8) yes
O1 . Ti1 . C18 . 111.26(8) yes
O1 2_566 Ti1 . C18 . 82.61(7) yes
Ti1 2_566 Ti1 . C19 . 103.16(6) yes
N1 . Ti1 . C19 . 116.48(9) yes
N2 . Ti1 . C19 . 145.74(7) yes
O1 . Ti1 . C19 . 91.64(7) yes
O1 2_566 Ti1 . C19 . 107.68(8) yes
Ti1 2_566 Ti1 . C20 . 134.80(7) yes
N1 . Ti1 . C20 . 85.22(7) yes
N2 . Ti1 . C20 . 118.79(8) yes
O1 . Ti1 . C20 . 106.67(7) yes
O1 2_566 Ti1 . C20 . 138.82(7) yes
C16 . Ti1 . C17 . 33.01(7) yes
C16 . Ti1 . C18 . 56.00(7) yes
C17 . Ti1 . C18 . 33.55(8) yes
C16 . Ti1 . C19 . 56.46(8) yes
C17 . Ti1 . C19 . 55.61(8) yes
C18 . Ti1 . C19 . 33.77(9) yes
C16 . Ti1 . C20 . 33.75(8) yes
C17 . Ti1 . C20 . 55.31(7) yes
C18 . Ti1 . C20 . 56.36(8) yes
C19 . Ti1 . C20 . 34.46(9) yes
Ti1 . N1 . Si1 . 136.15(8) yes
Ti1 . N1 . C1 . 89.1(1) yes
Si1 . N1 . C1 . 129.4(1) yes
Ti1 . N2 . C1 . 94.3(1) yes
Ti1 . N2 . C8 . 139.0(1) yes
C1 . N2 . C8 . 124.1(1) yes
C10 . N3 . C11 . 109.7(2) yes
C10 . N3 . C12 . 111.8(2) yes
C11 . N3 . C12 . 109.4(2) yes
Ti1 . O1 . Ti1 2_566 96.63(5) yes
N1 . Si1 . C13 . 111.82(9) yes
N1 . Si1 . C14 . 107.46(8) yes
C13 . Si1 . C14 . 108.3(1) yes
N1 . Si1 . C15 . 111.35(9) yes
C13 . Si1 . C15 . 108.9(1) yes
C14 . Si1 . C15 . 108.9(1) yes
N1 . C1 . N2 . 113.2(1) yes
N1 . C1 . C2 . 123.6(2) yes
N2 . C1 . C2 . 123.2(2) yes
C1 . C2 . C3 . 120.0(2) yes
C1 . C2 . C7 . 120.8(2) yes
C3 . C2 . C7 . 119.2(2) yes
C2 . C3 . C4 . 120.0(2) yes
C3 . C4 . C5 . 120.4(2) yes
C4 . C5 . C6 . 120.2(2) yes
C5 . C6 . C7 . 119.8(2) yes
C2 . C7 . C6 . 120.3(2) yes
N2 . C8 . C9 . 112.1(1) yes
C8 . C9 . C10 . 113.4(2) yes
N3 . C10 . C9 . 113.8(2) yes
Ti1 . C16 . C17 . 71.7(1) yes
Ti1 . C16 . C20 . 70.8(1) yes
C17 . C16 . C20 . 106.1(2) yes
Ti1 . C16 . C21 . 121.7(1) yes
C17 . C16 . C21 . 127.1(3) yes
C20 . C16 . C21 . 126.8(3) yes
Ti1 . C17 . C16 . 75.2(1) yes
Ti1 . C17 . C18 . 70.9(1) yes
C16 . C17 . C18 . 109.9(2) yes
Ti1 . C18 . C17 . 75.5(1) yes
Ti1 . C18 . C19 . 72.7(1) yes
C17 . C18 . C19 . 108.1(2) yes
Ti1 . C19 . C18 . 73.5(1) yes
Ti1 . C19 . C20 . 74.8(1) yes
C18 . C19 . C20 . 108.2(2) yes
Ti1 . C20 . C16 . 75.4(1) yes
Ti1 . C20 . C19 . 70.7(1) yes
C16 . C20 . C19 . 107.7(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . Ti1 2_566 2.7709(6) yes
Ti1 . N1 . 2.203(1) yes
Ti1 . N2 . 2.096(1) yes
Ti1 . O1 . 1.802(1) yes
Ti1 . O1 2_566 1.907(1) yes
Ti1 . C16 . 2.461(2) yes
Ti1 . C17 . 2.417(2) yes
Ti1 . C18 . 2.359(2) yes
Ti1 . C19 . 2.349(2) yes
Ti1 . C20 . 2.402(2) yes
N1 . Si1 . 1.737(2) yes
N1 . C1 . 1.333(2) yes
N2 . C1 . 1.315(2) yes
N2 . C8 . 1.460(2) yes
N3 . C10 . 1.461(2) yes
N3 . C11 . 1.457(3) yes
N3 . C12 . 1.454(3) yes
Si1 . C13 . 1.868(2) yes
Si1 . C14 . 1.857(2) yes
Si1 . C15 . 1.870(2) yes
C1 . C2 . 1.498(2) yes
C2 . C3 . 1.391(3) yes
C2 . C7 . 1.392(3) yes
C3 . C4 . 1.387(3) yes
C4 . C5 . 1.376(3) yes
C5 . C6 . 1.385(3) yes
C6 . C7 . 1.388(3) yes
C8 . C9 . 1.519(3) yes
C9 . C10 . 1.529(3) yes
C16 . C17 . 1.386(3) yes
C16 . C20 . 1.413(3) yes
C16 . C21 . 1.489(3) yes
C17 . C18 . 1.379(3) yes
C18 . C19 . 1.367(4) yes
C19 . C20 . 1.408(4) yes
|
1100812.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 10:15:27 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180564 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100812.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100812
loop_
_publ_author_name
'Humphries, Martin J.'
'Tellmann, Kilian P.'
'Gibson, Vernon C.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
Investigations into the Mechanism of Activation and Initiation of
Ethylene Polymerization by Bis(imino)pyridine Cobalt Catalysts:
Synthesis, Structures, and Deuterium Labeling Studies
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2039
_journal_page_last 2050
_journal_paper_doi 10.1021/om049032b
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C34 H46 Co N3'
_chemical_formula_weight 555.67
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.92(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.882(2)
_cell_length_b 14.823(2)
_cell_length_c 15.492(6)
_cell_measurement_reflns_used 31
_cell_measurement_temperature 203(2)
_cell_measurement_theta_max 12.52
_cell_measurement_theta_min 5.05
_cell_volume 3187.4(14)
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 203(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0467
_diffrn_reflns_av_sigmaI/netI 0.0916
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 5844
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.563
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour 'Very dark green'
_exptl_crystal_density_diffrn 1.158
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'platy blocks'
_exptl_crystal_F_000 1192
_exptl_crystal_size_max 0.73
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.23
_refine_diff_density_max 0.414
_refine_diff_density_min -0.330
_refine_diff_density_rms 0.064
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.978
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 346
_refine_ls_number_reflns 5600
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.978
_refine_ls_R_factor_all 0.0999
_refine_ls_R_factor_gt 0.0543
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1026
_refine_ls_wR_factor_ref 0.1142
_reflns_number_gt 3750
_reflns_number_total 5600
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060323
_cod_data_source_file om049032bsi20041208_063138.cif
_cod_data_source_block Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100812
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.74598(3) 0.85927(3) 0.56799(3) 0.02506(11) Uani 1 1 d . . .
C C 0.8468(3) 0.9518(3) 0.5719(3) 0.0451(9) Uani 1 1 d . . .
H0A H 0.8869 0.9462 0.5215 0.068 Uiso 1 1 calc R . .
H0B H 0.8861 0.9440 0.6237 0.068 Uiso 1 1 calc R . .
H0C H 0.8173 1.0111 0.5725 0.068 Uiso 1 1 calc R . .
N1 N 0.6506(2) 0.77377(17) 0.56261(17) 0.0265(5) Uani 1 1 d . . .
C2 C 0.5759(2) 0.7790(2) 0.6187(2) 0.0272(6) Uani 1 1 d . . .
C3 C 0.5018(2) 0.7157(2) 0.6135(2) 0.0331(7) Uani 1 1 d . . .
H3A H 0.4503 0.7181 0.6522 0.040 Uiso 1 1 calc R . .
C4 C 0.5047(3) 0.6486(3) 0.5504(2) 0.0378(7) Uani 1 1 d . . .
H4A H 0.4544 0.6063 0.5461 0.045 Uiso 1 1 calc R . .
C5 C 0.5809(3) 0.6437(3) 0.4941(2) 0.0381(7) Uani 1 1 d . . .
H5A H 0.5831 0.5984 0.4517 0.046 Uiso 1 1 calc R . .
C6 C 0.6547(3) 0.7077(2) 0.5014(2) 0.0312(7) Uani 1 1 d . . .
C7 C 0.5870(2) 0.8567(3) 0.67409(18) 0.0282(6) Uani 1 1 d . . .
N7 N 0.66658(19) 0.90384(18) 0.65783(17) 0.0257(5) Uani 1 1 d . . .
C8 C 0.5145(3) 0.8800(3) 0.7408(2) 0.0406(8) Uani 1 1 d . . .
H8A H 0.5425 0.9226 0.7816 0.061 Uiso 1 1 calc R . .
H8B H 0.4956 0.8257 0.7711 0.061 Uiso 1 1 calc R . .
H8C H 0.4583 0.9068 0.7130 0.061 Uiso 1 1 calc R . .
C9 C 0.7407(3) 0.7178(2) 0.4523(2) 0.0386(8) Uani 1 1 d . . .
N9 N 0.7941(2) 0.78826(19) 0.47590(19) 0.0330(6) Uani 1 1 d . . .
C10 C 0.7643(4) 0.6541(3) 0.3806(3) 0.0631(13) Uani 1 1 d . . .
H10A H 0.8295 0.6651 0.3617 0.095 Uiso 1 1 calc R . .
H10B H 0.7196 0.6633 0.3327 0.095 Uiso 1 1 calc R . .
H10C H 0.7591 0.5924 0.4011 0.095 Uiso 1 1 calc R . .
C11 C 0.6823(2) 0.9876(2) 0.7037(2) 0.0267(6) Uani 1 1 d . . .
C12 C 0.6376(2) 1.0664(2) 0.6708(2) 0.0319(7) Uani 1 1 d . . .
C13 C 0.6565(3) 1.1478(3) 0.7126(2) 0.0388(7) Uani 1 1 d . . .
H13A H 0.6271 1.2008 0.6916 0.047 Uiso 1 1 calc R . .
C14 C 0.7170(3) 1.1529(2) 0.7838(2) 0.0354(7) Uani 1 1 d . . .
H14A H 0.7285 1.2085 0.8113 0.042 Uiso 1 1 calc R . .
C15 C 0.7609(3) 1.0744(3) 0.8143(2) 0.0375(8) Uani 1 1 d . . .
H15A H 0.8026 1.0776 0.8626 0.045 Uiso 1 1 calc R . .
C16 C 0.7444(2) 0.9916(2) 0.7750(2) 0.0301(6) Uani 1 1 d . . .
C17 C 0.5723(3) 1.0656(2) 0.5911(3) 0.0443(9) Uani 1 1 d . . .
H17A H 0.5604 1.0017 0.5756 0.053 Uiso 1 1 calc R . .
C18 C 0.6220(4) 1.1099(4) 0.5152(3) 0.0715(15) Uani 1 1 d . . .
H18A H 0.6835 1.0808 0.5060 0.107 Uiso 1 1 calc R . .
H18B H 0.6323 1.1734 0.5275 0.107 Uiso 1 1 calc R . .
H18C H 0.5818 1.1038 0.4637 0.107 Uiso 1 1 calc R . .
C19 C 0.4748(4) 1.1091(4) 0.6077(4) 0.0653(14) Uani 1 1 d . . .
H19A H 0.4445 1.0792 0.6559 0.098 Uiso 1 1 calc R . .
H19B H 0.4340 1.1033 0.5565 0.098 Uiso 1 1 calc R . .
H19C H 0.4838 1.1725 0.6211 0.098 Uiso 1 1 calc R . .
C20 C 0.7939(3) 0.9079(2) 0.8116(3) 0.0428(9) Uani 1 1 d . . .
H20A H 0.7788 0.8569 0.7725 0.051 Uiso 1 1 calc R . .
C21 C 0.7546(5) 0.8850(4) 0.9001(4) 0.0825(19) Uani 1 1 d . . .
H21A H 0.6850 0.8795 0.8962 0.124 Uiso 1 1 calc R . .
H21B H 0.7715 0.9325 0.9406 0.124 Uiso 1 1 calc R . .
H21C H 0.7821 0.8284 0.9200 0.124 Uiso 1 1 calc R . .
C22 C 0.9026(4) 0.9173(3) 0.8171(4) 0.0596(12) Uani 1 1 d . . .
H22A H 0.9272 0.9311 0.7604 0.089 Uiso 1 1 calc R . .
H22B H 0.9306 0.8611 0.8376 0.089 Uiso 1 1 calc R . .
H22C H 0.9195 0.9655 0.8568 0.089 Uiso 1 1 calc R . .
C23 C 0.8840(3) 0.8043(2) 0.4331(2) 0.0390(8) Uani 1 1 d . . .
C24 C 0.9697(3) 0.7701(3) 0.4715(3) 0.0469(9) Uani 1 1 d . . .
C25 C 1.0553(3) 0.7887(3) 0.4310(3) 0.0572(12) Uani 1 1 d . . .
H25A H 1.1133 0.7666 0.4551 0.069 Uiso 1 1 calc R . .
C26 C 1.0582(3) 0.8393(3) 0.3556(3) 0.0602(13) Uani 1 1 d . . .
H26A H 1.1171 0.8493 0.3281 0.072 Uiso 1 1 calc R . .
C27 C 0.9740(4) 0.8748(3) 0.3212(3) 0.0555(11) Uani 1 1 d . . .
H27A H 0.9767 0.9102 0.2709 0.067 Uiso 1 1 calc R . .
C28 C 0.8849(3) 0.8595(3) 0.3593(3) 0.0462(8) Uani 1 1 d . . .
C29 C 0.9683(4) 0.7172(4) 0.5559(3) 0.0607(12) Uani 1 1 d . . .
H29A H 0.9035 0.7250 0.5806 0.073 Uiso 1 1 calc R . .
C30 C 1.0414(6) 0.7526(6) 0.6222(5) 0.104(3) Uani 1 1 d . . .
H30A H 1.0376 0.7171 0.6746 0.156 Uiso 1 1 calc R . .
H30B H 1.0273 0.8152 0.6350 0.156 Uiso 1 1 calc R . .
H30C H 1.1057 0.7479 0.5991 0.156 Uiso 1 1 calc R . .
C31 C 0.9826(8) 0.6178(5) 0.5411(6) 0.115(3) Uani 1 1 d . . .
H31A H 0.9355 0.5964 0.4990 0.173 Uiso 1 1 calc R . .
H31B H 0.9747 0.5856 0.5950 0.173 Uiso 1 1 calc R . .
H31C H 1.0470 0.6073 0.5197 0.173 Uiso 1 1 calc R . .
C32 C 0.7942(4) 0.9036(4) 0.3237(3) 0.0635(13) Uani 1 1 d . . .
H32A H 0.7401 0.8858 0.3608 0.076 Uiso 1 1 calc R . .
C33 C 0.8011(7) 1.0061(5) 0.3249(5) 0.104(3) Uani 1 1 d . . .
H33A H 0.8153 1.0264 0.3833 0.156 Uiso 1 1 calc R . .
H33B H 0.7403 1.0317 0.3053 0.156 Uiso 1 1 calc R . .
H33C H 0.8520 1.0254 0.2870 0.156 Uiso 1 1 calc R . .
C34 C 0.7702(5) 0.8728(7) 0.2311(5) 0.101(3) Uani 1 1 d . . .
H34A H 0.7117 0.9023 0.2110 0.152 Uiso 1 1 calc R . .
H34B H 0.7609 0.8079 0.2303 0.152 Uiso 1 1 calc R . .
H34C H 0.8229 0.8886 0.1935 0.152 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.02706(19) 0.02061(17) 0.02747(19) -0.00239(19) -0.00121(13) -0.0035(2)
C 0.047(2) 0.0380(18) 0.051(2) -0.0219(17) 0.0129(17) -0.0172(16)
N1 0.0323(14) 0.0212(12) 0.0258(12) 0.0007(10) -0.0065(10) -0.0018(10)
C2 0.0259(14) 0.0262(15) 0.0293(15) 0.0069(12) -0.0044(12) -0.0018(12)
C3 0.0297(16) 0.0346(17) 0.0350(16) 0.0057(14) -0.0027(13) -0.0041(13)
C4 0.0368(17) 0.0331(17) 0.0432(18) 0.0064(16) -0.0096(14) -0.0122(15)
C5 0.0457(18) 0.0280(14) 0.0401(17) -0.0008(16) -0.0120(14) -0.0091(16)
C6 0.0391(18) 0.0250(14) 0.0294(15) -0.0032(12) -0.0072(13) -0.0050(13)
C7 0.0289(14) 0.0291(14) 0.0264(13) 0.0023(14) -0.0036(11) 0.0011(14)
N7 0.0264(13) 0.0235(12) 0.0271(12) -0.0005(10) -0.0033(10) 0.0002(10)
C8 0.0368(18) 0.042(2) 0.0429(19) -0.0026(15) 0.0061(15) -0.0025(15)
C9 0.047(2) 0.0325(17) 0.0367(19) -0.0076(14) -0.0010(16) -0.0039(15)
N9 0.0360(15) 0.0279(13) 0.0351(14) -0.0044(11) 0.0028(12) -0.0037(11)
C10 0.073(3) 0.050(3) 0.066(3) -0.033(2) 0.019(2) -0.018(2)
C11 0.0287(15) 0.0255(14) 0.0258(14) -0.0033(12) 0.0003(12) -0.0003(12)
C12 0.0350(17) 0.0239(15) 0.0367(17) -0.0025(13) -0.0063(14) 0.0049(13)
C13 0.0425(17) 0.0274(15) 0.0462(18) -0.0069(16) -0.0054(14) 0.0052(15)
C14 0.0402(17) 0.0265(16) 0.0394(17) -0.0108(14) -0.0013(14) -0.0002(14)
C15 0.0414(19) 0.0382(18) 0.0328(17) -0.0069(14) -0.0062(14) -0.0014(15)
C16 0.0329(16) 0.0303(16) 0.0270(15) 0.0004(12) -0.0023(13) -0.0015(13)
C17 0.055(2) 0.0297(17) 0.048(2) -0.0032(15) -0.0196(18) 0.0064(16)
C18 0.086(4) 0.086(4) 0.041(2) 0.007(2) -0.022(2) 0.004(3)
C19 0.052(3) 0.069(3) 0.074(3) -0.002(2) -0.031(2) 0.016(2)
C20 0.056(2) 0.0281(17) 0.044(2) 0.0012(15) -0.0199(18) -0.0002(16)
C21 0.085(4) 0.078(4) 0.084(4) 0.048(3) -0.002(3) 0.008(3)
C22 0.054(3) 0.051(3) 0.073(3) 0.008(2) -0.017(2) 0.013(2)
C23 0.0409(19) 0.0339(17) 0.0425(19) -0.0162(15) 0.0114(15) -0.0081(15)
C24 0.044(2) 0.043(2) 0.054(2) -0.0165(18) 0.0091(18) 0.0016(17)
C25 0.039(2) 0.064(3) 0.069(3) -0.025(2) 0.010(2) -0.003(2)
C26 0.052(2) 0.058(3) 0.072(3) -0.029(2) 0.029(2) -0.023(2)
C27 0.070(3) 0.044(2) 0.053(2) -0.0108(18) 0.026(2) -0.016(2)
C28 0.055(2) 0.0349(16) 0.049(2) -0.0058(19) 0.0185(17) -0.0068(19)
C29 0.049(2) 0.072(3) 0.061(3) -0.002(2) 0.007(2) 0.018(2)
C30 0.105(6) 0.118(6) 0.088(5) 0.015(4) -0.033(4) 0.004(5)
C31 0.168(9) 0.063(4) 0.116(6) 0.017(4) 0.036(6) 0.002(4)
C32 0.066(3) 0.064(3) 0.061(3) 0.011(2) 0.019(2) 0.009(2)
C33 0.161(8) 0.069(4) 0.081(4) 0.016(3) -0.006(5) 0.033(5)
C34 0.075(4) 0.132(7) 0.096(5) -0.017(5) -0.020(3) 0.021(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co N9 81.11(12) . . ?
N1 Co N7 81.22(12) . . ?
N9 Co N7 162.32(12) . . ?
N1 Co C 178.94(17) . . ?
N9 Co C 98.70(15) . . ?
N7 Co C 98.95(14) . . ?
C6 N1 C2 121.5(3) . . ?
C6 N1 Co 119.3(2) . . ?
C2 N1 Co 119.1(2) . . ?
N1 C2 C3 119.5(3) . . ?
N1 C2 C7 110.4(3) . . ?
C3 C2 C7 130.0(3) . . ?
C2 C3 C4 119.3(3) . . ?
C5 C4 C3 120.7(3) . . ?
C4 C5 C6 118.7(3) . . ?
N1 C6 C5 120.3(3) . . ?
N1 C6 C9 109.8(3) . . ?
C5 C6 C9 130.0(3) . . ?
N7 C7 C2 112.7(3) . . ?
N7 C7 C8 125.3(3) . . ?
C2 C7 C8 122.0(3) . . ?
C7 N7 C11 118.4(3) . . ?
C7 N7 Co 116.5(2) . . ?
C11 N7 Co 124.9(2) . . ?
N9 C9 C6 113.6(3) . . ?
N9 C9 C10 124.9(4) . . ?
C6 C9 C10 121.4(3) . . ?
C9 N9 C23 119.1(3) . . ?
C9 N9 Co 116.1(2) . . ?
C23 N9 Co 124.8(2) . . ?
C16 C11 C12 120.9(3) . . ?
C16 C11 N7 120.9(3) . . ?
C12 C11 N7 118.1(3) . . ?
C13 C12 C11 118.1(3) . . ?
C13 C12 C17 119.3(3) . . ?
C11 C12 C17 122.6(3) . . ?
C14 C13 C12 121.8(3) . . ?
C13 C14 C15 118.9(3) . . ?
C16 C15 C14 121.5(3) . . ?
C15 C16 C11 118.8(3) . . ?
C15 C16 C20 119.2(3) . . ?
C11 C16 C20 122.0(3) . . ?
C12 C17 C18 110.6(4) . . ?
C12 C17 C19 112.3(4) . . ?
C18 C17 C19 111.2(4) . . ?
C22 C20 C21 109.9(4) . . ?
C22 C20 C16 112.9(3) . . ?
C21 C20 C16 110.5(4) . . ?
C28 C23 C24 122.1(4) . . ?
C28 C23 N9 119.3(4) . . ?
C24 C23 N9 118.4(4) . . ?
C25 C24 C23 117.5(4) . . ?
C25 C24 C29 121.0(4) . . ?
C23 C24 C29 121.4(4) . . ?
C24 C25 C26 121.8(5) . . ?
C27 C26 C25 119.7(4) . . ?
C26 C27 C28 121.6(4) . . ?
C27 C28 C23 117.2(4) . . ?
C27 C28 C32 120.8(4) . . ?
C23 C28 C32 122.0(4) . . ?
C31 C29 C24 111.7(5) . . ?
C31 C29 C30 110.6(6) . . ?
C24 C29 C30 112.5(5) . . ?
C28 C32 C33 112.0(6) . . ?
C28 C32 C34 112.2(5) . . ?
C33 C32 C34 108.7(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N1 1.833(3) . ?
Co N9 1.903(3) . ?
Co N7 1.907(3) . ?
Co C 1.960(4) . ?
N1 C6 1.365(4) . ?
N1 C2 1.366(4) . ?
C2 C3 1.394(5) . ?
C2 C7 1.443(5) . ?
C3 C4 1.396(5) . ?
C4 C5 1.384(5) . ?
C5 C6 1.399(5) . ?
C6 C9 1.434(5) . ?
C7 N7 1.335(4) . ?
C7 C8 1.494(5) . ?
N7 C11 1.445(4) . ?
C9 N9 1.329(5) . ?
C9 C10 1.498(5) . ?
N9 C23 1.441(5) . ?
C11 C16 1.393(4) . ?
C11 C12 1.413(4) . ?
C12 C13 1.393(5) . ?
C12 C17 1.520(5) . ?
C13 C14 1.378(5) . ?
C14 C15 1.393(5) . ?
C15 C16 1.387(5) . ?
C16 C20 1.523(5) . ?
C17 C18 1.522(7) . ?
C17 C19 1.525(6) . ?
C20 C22 1.516(6) . ?
C20 C21 1.523(7) . ?
C23 C28 1.406(6) . ?
C23 C24 1.416(6) . ?
C24 C25 1.381(6) . ?
C24 C29 1.525(7) . ?
C25 C26 1.389(8) . ?
C26 C27 1.381(8) . ?
C27 C28 1.398(6) . ?
C28 C32 1.514(7) . ?
C29 C31 1.505(9) . ?
C29 C30 1.525(9) . ?
C32 C33 1.522(9) . ?
C32 C34 1.537(8) . ?
|
1100813.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 10:15:27 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180564 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100813.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100813
loop_
_publ_author_name
'Humphries, Martin J.'
'Tellmann, Kilian P.'
'Gibson, Vernon C.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
Investigations into the Mechanism of Activation and Initiation of
Ethylene Polymerization by Bis(imino)pyridine Cobalt Catalysts:
Synthesis, Structures, and Deuterium Labeling Studies
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2039
_journal_page_last 2050
_journal_paper_doi 10.1021/om049032b
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C27 H31 Cl Co N3'
_chemical_formula_weight 491.93
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 101.91(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 36.945(11)
_cell_length_b 8.062(3)
_cell_length_c 17.718(5)
_cell_measurement_reflns_used 30
_cell_measurement_temperature 203(2)
_cell_measurement_theta_max 12.47
_cell_measurement_theta_min 5.17
_cell_volume 5164(3)
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 203(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0284
_diffrn_reflns_av_sigmaI/netI 0.0623
_diffrn_reflns_limit_h_max 43
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 4574
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 2.25
_diffrn_standards_decay_% 14.37
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.786
_exptl_absorpt_correction_T_max 0.9206
_exptl_absorpt_correction_T_min 0.7184
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour Claret
_exptl_crystal_density_diffrn 1.265
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'platy needles'
_exptl_crystal_F_000 2064
_exptl_crystal_size_max 0.93
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.17
_refine_diff_density_max 0.310
_refine_diff_density_min -0.334
_refine_diff_density_rms 0.061
_refine_ls_extinction_coef 0.00002(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 0.975
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 298
_refine_ls_number_reflns 4500
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.975
_refine_ls_R_factor_all 0.0830
_refine_ls_R_factor_gt 0.0444
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0942
_refine_ls_wR_factor_ref 0.1053
_reflns_number_gt 3089
_reflns_number_total 4500
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060324
_cod_data_source_file om049032bsi20041208_063138.cif
_cod_data_source_block Compound_10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100813
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.375079(12) 0.53216(6) 0.61068(2) 0.02937(14) Uani 1 1 d . . .
Cl Cl 0.39217(4) 0.38751(19) 0.71506(6) 0.0771(5) Uani 1 1 d . . .
N1 N 0.35959(7) 0.6412(3) 0.52171(15) 0.0291(6) Uani 1 1 d . . .
C2 C 0.33080(9) 0.7502(4) 0.51405(19) 0.0337(7) Uani 1 1 d . . .
C3 C 0.31732(10) 0.8309(5) 0.4437(2) 0.0426(9) Uani 1 1 d . . .
H3A H 0.2976 0.9065 0.4387 0.051 Uiso 1 1 calc R . .
C4 C 0.33384(11) 0.7965(5) 0.3813(2) 0.0461(9) Uani 1 1 d . . .
H4A H 0.3249 0.8480 0.3335 0.055 Uiso 1 1 calc R . .
C5 C 0.36329(11) 0.6869(5) 0.3895(2) 0.0433(9) Uani 1 1 d . . .
H5A H 0.3746 0.6652 0.3476 0.052 Uiso 1 1 calc R . .
C6 C 0.37597(10) 0.6092(5) 0.46021(18) 0.0339(7) Uani 1 1 d . . .
C7 C 0.31841(9) 0.7605(5) 0.5853(2) 0.0352(7) Uani 1 1 d . . .
N7 N 0.33664(7) 0.6608(4) 0.63982(15) 0.0315(6) Uani 1 1 d . . .
C8 C 0.28786(11) 0.8760(6) 0.5958(3) 0.0522(10) Uani 1 1 d . . .
H8A H 0.2673 0.8120 0.6066 0.078 Uiso 1 1 calc R . .
H8B H 0.2797 0.9400 0.5490 0.078 Uiso 1 1 calc R . .
H8C H 0.2969 0.9506 0.6385 0.078 Uiso 1 1 calc R . .
C9 C 0.40577(9) 0.4923(4) 0.48264(18) 0.0354(8) Uani 1 1 d . . .
N9 N 0.40971(7) 0.4415(4) 0.55502(15) 0.0328(6) Uani 1 1 d . . .
C10 C 0.42985(12) 0.4387(6) 0.4286(2) 0.0526(11) Uani 1 1 d . . .
H10A H 0.4522 0.5056 0.4374 0.079 Uiso 1 1 calc R . .
H10B H 0.4166 0.4529 0.3757 0.079 Uiso 1 1 calc R . .
H10C H 0.4364 0.3228 0.4376 0.079 Uiso 1 1 calc R . .
C11 C 0.32660(8) 0.6620(4) 0.71397(19) 0.0321(7) Uani 1 1 d . . .
C12 C 0.34455(9) 0.7690(5) 0.7713(2) 0.0376(8) Uani 1 1 d . . .
C13 C 0.33403(10) 0.7684(5) 0.8421(2) 0.0400(8) Uani 1 1 d . . .
H13A H 0.3461 0.8405 0.8810 0.048 Uiso 1 1 calc R . .
C14 C 0.30651(9) 0.6657(5) 0.85749(19) 0.0357(8) Uani 1 1 d . . .
C15 C 0.28927(9) 0.5592(5) 0.7997(2) 0.0394(8) Uani 1 1 d . . .
H15A H 0.2704 0.4890 0.8092 0.047 Uiso 1 1 calc R . .
C16 C 0.29912(9) 0.5531(5) 0.72776(19) 0.0369(8) Uani 1 1 d . . .
C17 C 0.37507(12) 0.8829(6) 0.7563(3) 0.0591(12) Uani 1 1 d . . .
H17A H 0.3940 0.8175 0.7397 0.089 Uiso 1 1 calc R . .
H17B H 0.3858 0.9419 0.8033 0.089 Uiso 1 1 calc R . .
H17C H 0.3648 0.9620 0.7164 0.089 Uiso 1 1 calc R . .
C18 C 0.29591(11) 0.6673(6) 0.9362(2) 0.0468(9) Uani 1 1 d . . .
H18A H 0.2733 0.7303 0.9331 0.070 Uiso 1 1 calc R . .
H18B H 0.3156 0.7181 0.9738 0.070 Uiso 1 1 calc R . .
H18C H 0.2921 0.5544 0.9518 0.070 Uiso 1 1 calc R . .
C19 C 0.28107(13) 0.4319(6) 0.6668(3) 0.0597(13) Uani 1 1 d . . .
H19A H 0.2701 0.4917 0.6202 0.090 Uiso 1 1 calc R . .
H19B H 0.2619 0.3710 0.6852 0.090 Uiso 1 1 calc R . .
H19C H 0.2995 0.3550 0.6559 0.090 Uiso 1 1 calc R . .
C20 C 0.44035(9) 0.3336(4) 0.5858(2) 0.0343(7) Uani 1 1 d . . .
C21 C 0.47326(10) 0.4047(5) 0.6249(2) 0.0387(8) Uani 1 1 d . . .
C22 C 0.50317(11) 0.3012(6) 0.6540(3) 0.0516(10) Uani 1 1 d . . .
H22A H 0.5256 0.3478 0.6802 0.062 Uiso 1 1 calc R . .
C23 C 0.50030(13) 0.1313(6) 0.6449(3) 0.0665(13) Uani 1 1 d . . .
C24 C 0.46723(13) 0.0654(5) 0.6082(3) 0.0683(15) Uani 1 1 d . . .
H24A H 0.4653 -0.0504 0.6025 0.082 Uiso 1 1 calc R . .
C25 C 0.43618(11) 0.1617(5) 0.5786(2) 0.0458(9) Uani 1 1 d . . .
C26 C 0.47702(13) 0.5897(5) 0.6344(3) 0.0574(11) Uani 1 1 d . . .
H26A H 0.4725 0.6419 0.5840 0.086 Uiso 1 1 calc R . .
H26B H 0.5018 0.6166 0.6621 0.086 Uiso 1 1 calc R . .
H26C H 0.4591 0.6300 0.6631 0.086 Uiso 1 1 calc R . .
C27 C 0.53421(15) 0.0228(8) 0.6757(5) 0.106(2) Uani 1 1 d . . .
H27A H 0.5275 -0.0639 0.7082 0.160 Uiso 1 1 calc R . .
H27B H 0.5537 0.0906 0.7055 0.160 Uiso 1 1 calc R . .
H27C H 0.5428 -0.0269 0.6327 0.160 Uiso 1 1 calc R . .
C28 C 0.39994(13) 0.0846(6) 0.5409(3) 0.0717(15) Uani 1 1 d . . .
H28A H 0.3803 0.1309 0.5632 0.108 Uiso 1 1 calc R . .
H28B H 0.4011 -0.0344 0.5493 0.108 Uiso 1 1 calc R . .
H28C H 0.3950 0.1074 0.4860 0.108 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0279(2) 0.0352(2) 0.0269(2) 0.0033(2) 0.00996(15) 0.0062(2)
Cl 0.0848(8) 0.1090(10) 0.0475(6) 0.0408(6) 0.0371(6) 0.0582(8)
N1 0.0271(13) 0.0308(15) 0.0293(13) -0.0014(11) 0.0054(10) 0.0025(11)
C2 0.0278(17) 0.0352(19) 0.0372(17) 0.0009(15) 0.0044(13) 0.0009(14)
C3 0.042(2) 0.037(2) 0.045(2) 0.0024(16) 0.0010(16) 0.0082(17)
C4 0.058(2) 0.042(2) 0.0353(19) 0.0089(16) 0.0020(17) 0.0019(19)
C5 0.058(2) 0.043(2) 0.0307(17) 0.0024(16) 0.0129(16) -0.0002(18)
C6 0.0414(19) 0.0346(18) 0.0274(16) -0.0017(14) 0.0113(14) -0.0005(15)
C7 0.0297(17) 0.037(2) 0.0387(18) -0.0022(15) 0.0056(13) 0.0045(15)
N7 0.0261(13) 0.0370(16) 0.0333(14) -0.0013(12) 0.0101(11) 0.0013(12)
C8 0.042(2) 0.055(3) 0.062(2) 0.001(2) 0.0155(18) 0.0143(19)
C9 0.0415(18) 0.035(2) 0.0339(16) -0.0014(14) 0.0172(14) 0.0007(15)
N9 0.0318(14) 0.0328(17) 0.0357(14) 0.0002(12) 0.0113(11) 0.0042(12)
C10 0.061(2) 0.057(3) 0.046(2) -0.0006(19) 0.0262(19) 0.017(2)
C11 0.0239(15) 0.0335(18) 0.0408(18) -0.0030(15) 0.0111(13) 0.0020(14)
C12 0.0284(17) 0.043(2) 0.0446(19) -0.0043(16) 0.0139(14) -0.0040(15)
C13 0.0358(19) 0.044(2) 0.0404(19) -0.0106(16) 0.0081(15) -0.0012(16)
C14 0.0318(17) 0.041(2) 0.0373(18) 0.0036(15) 0.0151(14) 0.0084(15)
C15 0.0309(17) 0.044(2) 0.0478(19) 0.0046(17) 0.0178(15) -0.0039(16)
C16 0.0289(16) 0.041(2) 0.0412(18) -0.0070(16) 0.0081(14) -0.0060(16)
C17 0.050(2) 0.069(3) 0.065(3) -0.021(2) 0.028(2) -0.030(2)
C18 0.049(2) 0.057(3) 0.0382(19) 0.0060(18) 0.0165(17) 0.0068(19)
C19 0.058(3) 0.067(3) 0.057(2) -0.013(2) 0.018(2) -0.027(2)
C20 0.0324(17) 0.0335(19) 0.0395(18) 0.0020(15) 0.0132(14) 0.0060(15)
C21 0.0330(18) 0.037(2) 0.048(2) -0.0045(16) 0.0128(15) 0.0009(15)
C22 0.0301(19) 0.051(3) 0.071(3) -0.003(2) 0.0048(18) 0.0015(17)
C23 0.041(2) 0.047(3) 0.102(4) 0.001(3) -0.006(2) 0.013(2)
C24 0.050(3) 0.030(3) 0.115(4) -0.004(2) -0.006(3) 0.0077(19)
C25 0.038(2) 0.033(2) 0.062(2) -0.0010(18) -0.0001(17) 0.0010(16)
C26 0.052(3) 0.039(2) 0.081(3) -0.011(2) 0.015(2) -0.0033(19)
C27 0.058(3) 0.068(4) 0.174(7) -0.003(4) -0.021(4) 0.023(3)
C28 0.050(3) 0.038(3) 0.113(4) -0.004(2) -0.014(3) -0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co N7 81.46(12) . . ?
N1 Co N9 81.96(12) . . ?
N7 Co N9 163.35(12) . . ?
N1 Co Cl 176.65(11) . . ?
N7 Co Cl 99.40(9) . . ?
N9 Co Cl 97.25(9) . . ?
C2 N1 C6 120.2(3) . . ?
C2 N1 Co 120.3(2) . . ?
C6 N1 Co 119.5(2) . . ?
N1 C2 C3 120.9(3) . . ?
N1 C2 C7 109.5(3) . . ?
C3 C2 C7 129.6(3) . . ?
C4 C3 C2 118.6(3) . . ?
C5 C4 C3 120.4(3) . . ?
C4 C5 C6 119.5(3) . . ?
N1 C6 C5 120.5(3) . . ?
N1 C6 C9 109.9(3) . . ?
C5 C6 C9 129.6(3) . . ?
N7 C7 C2 113.6(3) . . ?
N7 C7 C8 124.5(3) . . ?
C2 C7 C8 122.0(3) . . ?
C7 N7 C11 118.2(3) . . ?
C7 N7 Co 115.1(2) . . ?
C11 N7 Co 126.6(2) . . ?
N9 C9 C6 113.2(3) . . ?
N9 C9 C10 124.6(3) . . ?
C6 C9 C10 122.2(3) . . ?
C9 N9 C20 118.2(3) . . ?
C9 N9 Co 115.4(2) . . ?
C20 N9 Co 126.2(2) . . ?
C12 C11 C16 120.9(3) . . ?
C12 C11 N7 119.8(3) . . ?
C16 C11 N7 119.2(3) . . ?
C13 C12 C11 118.5(3) . . ?
C13 C12 C17 121.1(3) . . ?
C11 C12 C17 120.4(3) . . ?
C14 C13 C12 122.4(3) . . ?
C13 C14 C15 118.0(3) . . ?
C13 C14 C18 121.0(3) . . ?
C15 C14 C18 121.0(3) . . ?
C14 C15 C16 121.9(3) . . ?
C15 C16 C11 118.1(3) . . ?
C15 C16 C19 121.1(3) . . ?
C11 C16 C19 120.7(3) . . ?
C21 C20 C25 121.5(3) . . ?
C21 C20 N9 118.5(3) . . ?
C25 C20 N9 120.0(3) . . ?
C20 C21 C22 118.8(4) . . ?
C20 C21 C26 121.0(4) . . ?
C22 C21 C26 120.2(4) . . ?
C23 C22 C21 120.9(4) . . ?
C24 C23 C22 118.7(4) . . ?
C24 C23 C27 122.2(5) . . ?
C22 C23 C27 119.1(5) . . ?
C23 C24 C25 123.2(4) . . ?
C24 C25 C20 116.8(4) . . ?
C24 C25 C28 121.6(4) . . ?
C20 C25 C28 121.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N1 1.793(3) . ?
Co N7 1.914(3) . ?
Co N9 1.914(3) . ?
Co Cl 2.1672(13) . ?
N1 C2 1.365(4) . ?
N1 C6 1.375(4) . ?
C2 C3 1.403(5) . ?
C2 C7 1.432(5) . ?
C3 C4 1.397(6) . ?
C4 C5 1.386(6) . ?
C5 C6 1.393(5) . ?
C6 C9 1.442(5) . ?
C7 N7 1.328(5) . ?
C7 C8 1.504(5) . ?
N7 C11 1.437(4) . ?
C9 N9 1.325(4) . ?
C9 C10 1.500(4) . ?
N9 C20 1.443(4) . ?
C11 C12 1.392(5) . ?
C11 C16 1.401(5) . ?
C12 C13 1.387(5) . ?
C12 C17 1.520(5) . ?
C13 C14 1.381(5) . ?
C14 C15 1.387(5) . ?
C14 C18 1.524(5) . ?
C15 C16 1.396(5) . ?
C16 C19 1.505(5) . ?
C20 C21 1.392(5) . ?
C20 C25 1.397(5) . ?
C21 C22 1.396(6) . ?
C21 C26 1.505(6) . ?
C22 C23 1.381(7) . ?
C23 C24 1.367(7) . ?
C23 C27 1.533(7) . ?
C24 C25 1.395(6) . ?
C25 C28 1.502(6) . ?
|
1100814.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 10:38:59 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180565 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100814.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100814
loop_
_publ_author_name
'Soleimannejad, Janet'
'White, Colin'
_publ_section_title
;
A Convenient One-Pot Synthesis of a Functionalized-Arene Ruthenium
Half-Sandwich Compound [RuCl~2~(\h^6^-C~6~H~5~OCH~2~CH~2~OH)]~2~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2538
_journal_page_last 2541
_journal_paper_doi 10.1021/om049044x
_journal_volume 24
_chemical_formula_moiety 'C16 H20 Cl3 O2 Ru2 +, C24 H20 B -, C3 H6 O'
_chemical_formula_sum 'C43 H46 B Cl3 O3 Ru2'
_chemical_formula_weight 930.10
_chemical_name_systematic
'tri-\m-chloro-bis{(\h^6^-ethoxybenzene)ruthenium(II)}(1+)tetraphenylborate(1-) 1 acetone solvate'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 98.977(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.0185(12)
_cell_length_b 17.180(2)
_cell_length_c 23.544(3)
_cell_measurement_reflns_used 40
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 28.38
_cell_measurement_theta_min 1.47
_cell_volume 4002.7(8)
_computing_cell_refinement SMART
_computing_data_collection 'SMART (Bruker, 1997-2001)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker SMART1000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0475
_diffrn_reflns_av_sigmaI/netI 0.0550
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 21238
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.75
_diffrn_standards_decay_% 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.993
_exptl_absorpt_correction_T_max 0.8817
_exptl_absorpt_correction_T_min 0.6746
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.543
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1888
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.13
_refine_diff_density_max 1.072
_refine_diff_density_min -0.552
_refine_diff_density_rms 0.095
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.976
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 503
_refine_ls_number_reflns 7008
_refine_ls_number_restraints 47
_refine_ls_restrained_S_all 0.973
_refine_ls_R_factor_all 0.0760
_refine_ls_R_factor_gt 0.0443
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1062
_refine_ls_wR_factor_ref 0.1208
_reflns_number_gt 4626
_reflns_number_total 7008
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om049044xsi20050310_111544.cif
_cod_data_source_block iwh31m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100814
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.20830(4) 0.959222(19) 0.330513(16) 0.03477(13) Uani 1 1 d . . .
Ru2 Ru 0.26604(5) 0.95404(2) 0.198023(16) 0.04480(15) Uani 1 1 d . . .
Cl1 Cl 0.39855(14) 1.00589(8) 0.28583(5) 0.0464(3) Uani 1 1 d . . .
Cl2 Cl 0.23052(19) 0.85276(7) 0.26602(6) 0.0680(5) Uani 1 1 d . . .
Cl3 Cl 0.08868(16) 1.01460(9) 0.24185(6) 0.0586(4) Uani 1 1 d . . .
B B 0.0835(6) 1.2593(3) 0.5055(2) 0.0312(12) Uani 1 1 d . . .
C1 C 0.2879(6) 1.0153(3) 0.4156(2) 0.0445(13) Uani 1 1 d . . .
C2 C 0.3075(6) 0.9320(3) 0.4170(2) 0.0483(14) Uani 1 1 d . . .
H2 H 0.3955 0.9113 0.4283 0.058 Uiso 1 1 calc R . .
C3 C 0.1975(6) 0.8812(3) 0.4017(2) 0.0466(14) Uani 1 1 d . . .
H3 H 0.2110 0.8265 0.4046 0.056 Uiso 1 1 calc R . .
C4 C 0.0664(6) 0.9114(3) 0.3819(2) 0.0504(15) Uani 1 1 d . . .
H4 H -0.0081 0.8772 0.3721 0.061 Uiso 1 1 calc R . .
C5 C 0.0482(6) 0.9917(3) 0.3770(2) 0.0472(13) Uani 1 1 d . . .
H5 H -0.0392 1.0117 0.3630 0.057 Uiso 1 1 calc R . .
C6 C 0.1574(5) 1.0444(3) 0.3924(2) 0.0395(12) Uani 1 1 d . . .
H6 H 0.1436 1.0988 0.3871 0.047 Uiso 1 1 calc R . .
C7 C 0.3882(6) 1.1416(3) 0.4209(2) 0.0478(13) Uani 1 1 d . . .
H7A H 0.3182 1.1649 0.4410 0.057 Uiso 1 1 calc R . .
H7B H 0.3633 1.1516 0.3792 0.057 Uiso 1 1 calc R . .
C8 C 0.5222(6) 1.1760(4) 0.4425(3) 0.0638(17) Uani 1 1 d . . .
H8A H 0.5465 1.1650 0.4836 0.096 Uiso 1 1 calc R . .
H8B H 0.5185 1.2325 0.4365 0.096 Uiso 1 1 calc R . .
H8C H 0.5903 1.1535 0.4217 0.096 Uiso 1 1 calc R . .
C9 C 0.4280(9) 0.9762(4) 0.1449(3) 0.0662(19) Uani 1 1 d . A .
C10 C 0.3988(11) 0.8963(4) 0.1463(3) 0.088(3) Uani 1 1 d . . .
H10 H 0.4689 0.8598 0.1581 0.105 Uiso 1 1 calc R . .
C11 C 0.2649(12) 0.8709(4) 0.1302(3) 0.098(3) Uani 1 1 d . . .
H11 H 0.2462 0.8167 0.1298 0.118 Uiso 1 1 calc R . .
C12 C 0.1579(9) 0.9233(4) 0.1145(2) 0.084(3) Uani 1 1 d . . .
H12 H 0.0681 0.9048 0.1036 0.101 Uiso 1 1 calc R . .
C13 C 0.1865(8) 1.0049(4) 0.1152(2) 0.0688(19) Uani 1 1 d . . .
H13 H 0.1160 1.0417 0.1053 0.083 Uiso 1 1 calc R . .
C14 C 0.3237(7) 1.0298(3) 0.1313(2) 0.0568(17) Uani 1 1 d . . .
H14 H 0.3439 1.0838 0.1326 0.068 Uiso 1 1 calc R . .
C15A C 0.6916(11) 0.9674(8) 0.1796(5) 0.077(3) Uani 0.611(8) 1 d PDU A 1
H15A H 0.7626 1.0017 0.1685 0.093 Uiso 0.611(8) 1 calc PR A 1
H15B H 0.6954 0.9172 0.1592 0.093 Uiso 0.611(8) 1 calc PR A 1
C15B C 0.6345(17) 0.9333(7) 0.1835(8) 0.077(3) Uani 0.389(8) 1 d PDU A 2
H15C H 0.6459 0.8962 0.1524 0.092 Uiso 0.389(8) 1 calc PR A 2
H15D H 0.5930 0.9063 0.2136 0.092 Uiso 0.389(8) 1 calc PR A 2
C16A C 0.7206(13) 0.9531(7) 0.2438(5) 0.079(3) Uani 0.611(8) 1 d PDU A 1
H16A H 0.7203 1.0028 0.2642 0.119 Uiso 0.611(8) 1 calc PR A 1
H16B H 0.8093 0.9283 0.2537 0.119 Uiso 0.611(8) 1 calc PR A 1
H16C H 0.6509 0.9189 0.2550 0.119 Uiso 0.611(8) 1 calc PR A 1
C16B C 0.7659(18) 0.9728(11) 0.2080(9) 0.079(3) Uani 0.389(8) 1 d PDU A 2
H16D H 0.8188 0.9825 0.1770 0.119 Uiso 0.389(8) 1 calc PR A 2
H16E H 0.8174 0.9392 0.2371 0.119 Uiso 0.389(8) 1 calc PR A 2
H16F H 0.7465 1.0224 0.2256 0.119 Uiso 0.389(8) 1 calc PR A 2
C17 C 0.0136(5) 1.2318(2) 0.44032(19) 0.0329(11) Uani 1 1 d . . .
C18 C 0.0602(5) 1.2566(3) 0.3900(2) 0.0412(12) Uani 1 1 d . . .
H18 H 0.1347 1.2914 0.3938 0.049 Uiso 1 1 calc R . .
C19 C 0.0033(6) 1.2330(3) 0.3348(2) 0.0485(14) Uani 1 1 d . . .
H19 H 0.0385 1.2521 0.3023 0.058 Uiso 1 1 calc R . .
C20 C -0.1046(6) 1.1819(3) 0.3276(2) 0.0488(14) Uani 1 1 d . . .
H20 H -0.1435 1.1648 0.2903 0.059 Uiso 1 1 calc R . .
C21 C -0.1540(5) 1.1564(3) 0.3755(2) 0.0429(13) Uani 1 1 d . . .
H21 H -0.2285 1.1215 0.3708 0.051 Uiso 1 1 calc R . .
C22 C -0.0989(5) 1.1799(2) 0.4302(2) 0.0361(11) Uani 1 1 d . . .
H22 H -0.1369 1.1610 0.4621 0.043 Uiso 1 1 calc R . .
C23 C -0.0320(5) 1.2846(2) 0.54555(19) 0.0320(11) Uani 1 1 d . . .
C24 C -0.1681(5) 1.2987(2) 0.5249(2) 0.0368(12) Uani 1 1 d . . .
H24 H -0.1991 1.2920 0.4850 0.044 Uiso 1 1 calc R . .
C25 C -0.2608(6) 1.3222(2) 0.5599(2) 0.0423(13) Uani 1 1 d . . .
H25 H -0.3525 1.3310 0.5437 0.051 Uiso 1 1 calc R . .
C26 C -0.2185(6) 1.3327(3) 0.6185(2) 0.0484(15) Uani 1 1 d . . .
H26 H -0.2812 1.3481 0.6427 0.058 Uiso 1 1 calc R . .
C27 C -0.0844(6) 1.3205(3) 0.6412(2) 0.0516(15) Uani 1 1 d . . .
H27 H -0.0534 1.3283 0.6810 0.062 Uiso 1 1 calc R . .
C28 C 0.0052(6) 1.2965(3) 0.6044(2) 0.0462(13) Uani 1 1 d . . .
H28 H 0.0968 1.2879 0.6207 0.055 Uiso 1 1 calc R . .
C29 C 0.1776(5) 1.3357(2) 0.49797(19) 0.0318(11) Uani 1 1 d . . .
C30 C 0.1224(5) 1.4104(2) 0.48969(18) 0.0326(11) Uani 1 1 d . . .
H30 H 0.0309 1.4176 0.4946 0.039 Uiso 1 1 calc R . .
C31 C 0.1938(5) 1.4745(2) 0.4747(2) 0.0369(11) Uani 1 1 d . . .
H31 H 0.1505 1.5237 0.4688 0.044 Uiso 1 1 calc R . .
C32 C 0.3286(5) 1.4666(3) 0.4683(2) 0.0398(12) Uani 1 1 d . . .
H32 H 0.3786 1.5103 0.4586 0.048 Uiso 1 1 calc R . .
C33 C 0.3886(5) 1.3949(3) 0.4762(2) 0.0429(12) Uani 1 1 d . . .
H33 H 0.4802 1.3886 0.4711 0.051 Uiso 1 1 calc R . .
C34 C 0.3156(5) 1.3312(3) 0.4917(2) 0.0402(12) Uani 1 1 d . . .
H34 H 0.3606 1.2827 0.4982 0.048 Uiso 1 1 calc R . .
C35 C 0.1731(5) 1.1864(2) 0.53770(19) 0.0334(11) Uani 1 1 d . . .
C36 C 0.2822(5) 1.1989(3) 0.5823(2) 0.0418(12) Uani 1 1 d . . .
H36 H 0.3070 1.2510 0.5928 0.050 Uiso 1 1 calc R . .
C37 C 0.3556(6) 1.1380(3) 0.6121(2) 0.0483(13) Uani 1 1 d . . .
H37 H 0.4276 1.1491 0.6423 0.058 Uiso 1 1 calc R . .
C38 C 0.3226(6) 1.0613(3) 0.5972(2) 0.0486(14) Uani 1 1 d . . .
H38 H 0.3714 1.0194 0.6169 0.058 Uiso 1 1 calc R . .
C39 C 0.2177(5) 1.0473(3) 0.5532(2) 0.0400(12) Uani 1 1 d . . .
H39 H 0.1945 0.9953 0.5422 0.048 Uiso 1 1 calc R . .
C40 C 0.1455(5) 1.1084(2) 0.52463(19) 0.0336(11) Uani 1 1 d . . .
H40 H 0.0734 1.0965 0.4946 0.040 Uiso 1 1 calc R . .
C41 C 0.5295(8) 1.1909(5) 0.2305(4) 0.101(3) Uani 1 1 d . B .
H41A H 0.6177 1.2103 0.2488 0.152 Uiso 1 1 calc R . .
H41B H 0.5099 1.2105 0.1910 0.152 Uiso 1 1 calc R . .
H41C H 0.5308 1.1339 0.2300 0.152 Uiso 1 1 calc R . .
C42 C 0.4221(9) 1.2184(3) 0.2638(3) 0.075(2) Uani 1 1 d D . .
C43 C 0.2827(7) 1.2103(4) 0.2358(3) 0.079(2) Uani 1 1 d . B .
H43A H 0.2217 1.2254 0.2626 0.118 Uiso 1 1 calc R . .
H43B H 0.2654 1.1560 0.2241 0.118 Uiso 1 1 calc R . .
H43C H 0.2671 1.2439 0.2018 0.118 Uiso 1 1 calc R . .
O1 O 0.3973(4) 1.05783(19) 0.43172(14) 0.0461(9) Uani 1 1 d . . .
O2 O 0.5553(6) 1.0044(3) 0.16101(19) 0.0863(15) Uani 1 1 d D . .
O3A O 0.4769(18) 1.2410(7) 0.3121(3) 0.094(4) Uani 0.66(2) 1 d PDU B 1
O3B O 0.394(3) 1.2527(13) 0.3071(7) 0.096(5) Uani 0.34(2) 1 d PDU B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0522(3) 0.02454(19) 0.0296(2) 0.00365(15) 0.01262(18) 0.00500(18)
Ru2 0.0826(4) 0.0282(2) 0.0238(2) 0.00148(16) 0.0090(2) -0.0036(2)
Cl1 0.0524(9) 0.0595(8) 0.0281(6) 0.0033(6) 0.0090(6) -0.0041(7)
Cl2 0.1486(17) 0.0257(6) 0.0349(7) -0.0003(5) 0.0304(9) -0.0039(8)
Cl3 0.0602(10) 0.0677(9) 0.0468(8) 0.0229(7) 0.0052(7) 0.0094(7)
B 0.037(3) 0.025(2) 0.031(3) -0.001(2) 0.005(2) -0.001(2)
C1 0.069(4) 0.045(3) 0.024(2) 0.001(2) 0.021(3) 0.007(3)
C2 0.079(4) 0.043(3) 0.025(3) 0.010(2) 0.019(3) 0.021(3)
C3 0.082(4) 0.033(3) 0.030(3) 0.007(2) 0.026(3) 0.008(3)
C4 0.068(4) 0.036(3) 0.055(3) 0.002(2) 0.034(3) -0.003(3)
C5 0.051(3) 0.041(3) 0.055(3) -0.005(2) 0.025(3) -0.001(3)
C6 0.056(3) 0.033(2) 0.035(3) -0.003(2) 0.021(2) 0.006(2)
C7 0.057(4) 0.047(3) 0.041(3) -0.001(2) 0.013(3) 0.001(3)
C8 0.054(4) 0.078(4) 0.060(4) -0.015(3) 0.012(3) -0.004(3)
C9 0.109(6) 0.058(4) 0.036(3) 0.008(3) 0.026(4) 0.010(4)
C10 0.181(9) 0.055(4) 0.037(4) 0.002(3) 0.048(5) 0.028(5)
C11 0.235(12) 0.043(4) 0.025(3) -0.009(3) 0.043(5) -0.024(6)
C12 0.146(8) 0.073(4) 0.028(3) 0.006(3) 0.000(4) -0.051(5)
C13 0.120(6) 0.060(4) 0.023(3) 0.014(3) 0.000(3) 0.000(4)
C14 0.101(5) 0.041(3) 0.031(3) 0.004(2) 0.016(3) -0.015(3)
C15A 0.087(7) 0.078(5) 0.067(5) 0.013(5) 0.013(5) 0.003(5)
C15B 0.086(7) 0.077(6) 0.067(5) 0.013(5) 0.011(5) 0.002(5)
C16A 0.088(7) 0.082(5) 0.068(5) 0.010(5) 0.013(5) 0.001(5)
C16B 0.087(8) 0.079(6) 0.071(6) 0.014(5) 0.011(5) -0.002(5)
C17 0.040(3) 0.028(2) 0.033(2) -0.0022(19) 0.010(2) 0.001(2)
C18 0.047(3) 0.037(3) 0.042(3) -0.004(2) 0.011(3) -0.002(2)
C19 0.061(4) 0.054(3) 0.032(3) -0.002(2) 0.013(3) 0.002(3)
C20 0.058(4) 0.049(3) 0.038(3) -0.012(2) 0.000(3) 0.008(3)
C21 0.041(3) 0.031(2) 0.053(3) -0.008(2) -0.005(3) -0.001(2)
C22 0.048(3) 0.025(2) 0.036(3) -0.0001(19) 0.007(2) 0.003(2)
C23 0.045(3) 0.018(2) 0.035(3) 0.0006(18) 0.009(2) -0.003(2)
C24 0.043(3) 0.029(2) 0.040(3) 0.009(2) 0.011(2) 0.003(2)
C25 0.048(3) 0.030(2) 0.051(3) 0.010(2) 0.014(3) 0.007(2)
C26 0.060(4) 0.029(2) 0.064(4) -0.005(2) 0.033(3) 0.001(2)
C27 0.061(4) 0.052(3) 0.045(3) -0.016(3) 0.020(3) -0.005(3)
C28 0.046(3) 0.050(3) 0.043(3) -0.014(2) 0.009(3) -0.007(3)
C29 0.038(3) 0.031(2) 0.027(2) -0.0058(19) 0.006(2) -0.003(2)
C30 0.041(3) 0.030(2) 0.028(2) -0.0061(19) 0.009(2) -0.003(2)
C31 0.049(3) 0.027(2) 0.035(3) 0.000(2) 0.010(2) 0.001(2)
C32 0.048(3) 0.032(2) 0.040(3) -0.004(2) 0.008(2) -0.013(2)
C33 0.035(3) 0.047(3) 0.048(3) -0.003(2) 0.008(2) -0.006(2)
C34 0.047(3) 0.028(2) 0.046(3) -0.002(2) 0.008(3) 0.002(2)
C35 0.042(3) 0.030(2) 0.030(2) -0.0007(19) 0.011(2) 0.004(2)
C36 0.046(3) 0.034(2) 0.043(3) -0.007(2) 0.001(3) 0.005(2)
C37 0.048(3) 0.049(3) 0.045(3) -0.003(3) -0.005(3) 0.006(3)
C38 0.059(4) 0.043(3) 0.042(3) 0.004(2) 0.004(3) 0.017(3)
C39 0.054(3) 0.029(2) 0.040(3) 0.001(2) 0.014(3) 0.005(2)
C40 0.043(3) 0.032(2) 0.026(2) -0.0019(19) 0.009(2) 0.001(2)
C41 0.069(5) 0.094(5) 0.140(8) 0.022(6) 0.014(5) 0.005(4)
C42 0.137(7) 0.046(3) 0.040(4) 0.011(3) 0.002(4) -0.038(4)
C43 0.081(6) 0.078(5) 0.084(5) 0.007(4) 0.033(5) 0.004(4)
O1 0.058(3) 0.045(2) 0.0350(19) 0.0002(16) 0.0065(18) 0.0067(18)
O2 0.117(5) 0.093(3) 0.053(3) 0.013(3) 0.024(3) 0.042(3)
O3A 0.118(11) 0.105(5) 0.050(4) 0.009(4) -0.019(5) -0.066(8)
O3B 0.120(12) 0.105(6) 0.053(5) 0.010(5) -0.022(7) -0.070(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 Ru1 C3 68.6(2) . . ?
C5 Ru1 C4 37.67(19) . . ?
C3 Ru1 C4 38.3(2) . . ?
C5 Ru1 C2 81.2(2) . . ?
C3 Ru1 C2 37.9(2) . . ?
C4 Ru1 C2 68.8(2) . . ?
C5 Ru1 C6 38.35(19) . . ?
C3 Ru1 C6 81.58(18) . . ?
C4 Ru1 C6 68.86(18) . . ?
C2 Ru1 C6 68.85(18) . . ?
C5 Ru1 C1 68.0(2) . . ?
C3 Ru1 C1 68.26(19) . . ?
C4 Ru1 C1 80.6(2) . . ?
C2 Ru1 C1 38.04(18) . . ?
C6 Ru1 C1 37.47(19) . . ?
C5 Ru1 Cl2 131.83(15) . . ?
C3 Ru1 Cl2 92.19(13) . . ?
C4 Ru1 Cl2 101.39(14) . . ?
C2 Ru1 Cl2 110.69(13) . . ?
C6 Ru1 Cl2 169.94(14) . . ?
C1 Ru1 Cl2 146.11(14) . . ?
C5 Ru1 Cl3 91.62(16) . . ?
C3 Ru1 Cl3 146.11(17) . . ?
C4 Ru1 Cl3 110.44(17) . . ?
C2 Ru1 Cl3 168.63(13) . . ?
C6 Ru1 Cl3 100.10(14) . . ?
C1 Ru1 Cl3 130.86(13) . . ?
Cl2 Ru1 Cl3 80.66(5) . . ?
C5 Ru1 Cl1 145.55(14) . . ?
C3 Ru1 Cl1 132.20(17) . . ?
C4 Ru1 Cl1 170.18(17) . . ?
C2 Ru1 Cl1 101.54(16) . . ?
C6 Ru1 Cl1 110.21(13) . . ?
C1 Ru1 Cl1 92.92(14) . . ?
Cl2 Ru1 Cl1 79.83(5) . . ?
Cl3 Ru1 Cl1 79.38(5) . . ?
C11 Ru2 C12 38.1(3) . . ?
C11 Ru2 C13 68.9(3) . . ?
C12 Ru2 C13 38.6(2) . . ?
C11 Ru2 C10 38.0(3) . . ?
C12 Ru2 C10 69.1(3) . . ?
C13 Ru2 C10 81.5(3) . . ?
C11 Ru2 C14 80.3(2) . . ?
C12 Ru2 C14 69.0(2) . . ?
C13 Ru2 C14 38.4(2) . . ?
C10 Ru2 C14 67.4(2) . . ?
C11 Ru2 C9 67.4(3) . . ?
C12 Ru2 C9 80.6(3) . . ?
C13 Ru2 C9 68.0(3) . . ?
C10 Ru2 C9 37.1(3) . . ?
C14 Ru2 C9 36.7(2) . . ?
C11 Ru2 Cl3 133.2(3) . . ?
C12 Ru2 Cl3 101.3(3) . . ?
C13 Ru2 Cl3 91.1(2) . . ?
C10 Ru2 Cl3 170.3(3) . . ?
C14 Ru2 Cl3 110.13(18) . . ?
C9 Ru2 Cl3 144.21(16) . . ?
C11 Ru2 Cl2 91.69(17) . . ?
C12 Ru2 Cl2 108.71(17) . . ?
C13 Ru2 Cl2 144.0(2) . . ?
C10 Ru2 Cl2 101.98(17) . . ?
C14 Ru2 Cl2 169.36(17) . . ?
C9 Ru2 Cl2 133.32(18) . . ?
Cl3 Ru2 Cl2 80.47(5) . . ?
C11 Ru2 Cl1 144.4(3) . . ?
C12 Ru2 Cl1 171.68(17) . . ?
C13 Ru2 Cl1 133.45(17) . . ?
C10 Ru2 Cl1 109.9(3) . . ?
C14 Ru2 Cl1 102.80(16) . . ?
C9 Ru2 Cl1 93.7(2) . . ?
Cl3 Ru2 Cl1 79.69(5) . . ?
Cl2 Ru2 Cl1 79.61(5) . . ?
Ru2 Cl1 Ru1 83.55(4) . . ?
Ru1 Cl2 Ru2 84.78(4) . . ?
Ru2 Cl3 Ru1 84.36(5) . . ?
C29 B C35 112.0(4) . . ?
C29 B C17 107.2(4) . . ?
C35 B C17 109.3(3) . . ?
C29 B C23 108.3(3) . . ?
C35 B C23 108.3(4) . . ?
C17 B C23 111.7(4) . . ?
O1 C1 C6 125.8(4) . . ?
O1 C1 C2 115.9(5) . . ?
C6 C1 C2 118.0(5) . . ?
O1 C1 Ru1 130.8(3) . . ?
C6 C1 Ru1 68.4(3) . . ?
C2 C1 Ru1 67.9(3) . . ?
C3 C2 C1 120.7(5) . . ?
C3 C2 Ru1 70.7(3) . . ?
C1 C2 Ru1 74.1(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
Ru1 C2 H2 127.7 . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 Ru1 71.4(3) . . ?
C4 C3 Ru1 71.0(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
Ru1 C3 H3 130.2 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 Ru1 70.6(3) . . ?
C3 C4 Ru1 70.7(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
Ru1 C4 H4 131.2 . . ?
C4 C5 C6 121.5(5) . . ?
C4 C5 Ru1 71.7(3) . . ?
C6 C5 Ru1 71.9(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
Ru1 C5 H5 129.7 . . ?
C5 C6 C1 119.8(4) . . ?
C5 C6 Ru1 69.8(3) . . ?
C1 C6 Ru1 74.1(3) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
Ru1 C6 H6 128.2 . . ?
O1 C7 C8 107.7(5) . . ?
O1 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
O1 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 C14 117.7(6) . . ?
O2 C9 C10 122.1(7) . . ?
C14 C9 C10 120.0(8) . . ?
O2 C9 Ru2 129.5(4) . . ?
C14 C9 Ru2 69.9(4) . . ?
C10 C9 Ru2 69.4(4) . . ?
C9 C10 C11 119.4(8) . . ?
C9 C10 Ru2 73.5(4) . . ?
C11 C10 Ru2 69.7(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
Ru2 C10 H10 128.8 . . ?
C12 C11 C10 121.9(6) . . ?
C12 C11 Ru2 71.6(4) . . ?
C10 C11 Ru2 72.4(4) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
Ru2 C11 H11 129.7 . . ?
C11 C12 C13 118.8(7) . . ?
C11 C12 Ru2 70.3(4) . . ?
C13 C12 Ru2 71.2(3) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
Ru2 C12 H12 130.3 . . ?
C12 C13 C14 118.6(7) . . ?
C12 C13 Ru2 70.2(3) . . ?
C14 C13 Ru2 71.4(3) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
Ru2 C13 H13 130.1 . . ?
C9 C14 C13 121.2(6) . . ?
C9 C14 Ru2 73.3(3) . . ?
C13 C14 Ru2 70.2(3) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
Ru2 C14 H14 129.6 . . ?
O2 C15A C16A 112.5(9) . . ?
O2 C15A H15A 109.1 . . ?
C16A C15A H15A 109.1 . . ?
O2 C15A H15B 109.1 . . ?
C16A C15A H15B 109.1 . . ?
H15A C15A H15B 107.8 . . ?
O2 C15B C16B 98.5(12) . . ?
O2 C15B H15C 112.1 . . ?
C16B C15B H15C 112.1 . . ?
O2 C15B H15D 112.1 . . ?
C16B C15B H15D 112.1 . . ?
H15C C15B H15D 109.7 . . ?
C15B C16B H16D 109.5 . . ?
C15B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C18 C17 C22 114.0(4) . . ?
C18 C17 B 123.2(4) . . ?
C22 C17 B 122.8(4) . . ?
C19 C18 C17 123.8(5) . . ?
C19 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C20 C19 C18 119.8(5) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C22 122.0(5) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C17 121.9(4) . . ?
C21 C22 H22 119.1 . . ?
C17 C22 H22 119.1 . . ?
C24 C23 C28 114.6(5) . . ?
C24 C23 B 125.2(4) . . ?
C28 C23 B 120.1(5) . . ?
C23 C24 C25 123.3(5) . . ?
C23 C24 H24 118.3 . . ?
C25 C24 H24 118.3 . . ?
C26 C25 C24 119.7(5) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C27 C26 C25 119.5(5) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 118.9(5) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
C23 C28 C27 124.1(6) . . ?
C23 C28 H28 118.0 . . ?
C27 C28 H28 118.0 . . ?
C30 C29 C34 114.0(4) . . ?
C30 C29 B 121.8(4) . . ?
C34 C29 B 123.7(4) . . ?
C31 C30 C29 123.7(4) . . ?
C31 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
C30 C31 C32 119.9(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C33 C32 C31 119.1(4) . . ?
C33 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C32 C33 C34 120.3(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C29 123.0(4) . . ?
C33 C34 H34 118.5 . . ?
C29 C34 H34 118.5 . . ?
C40 C35 C36 114.6(4) . . ?
C40 C35 B 123.5(4) . . ?
C36 C35 B 121.9(4) . . ?
C37 C36 C35 122.9(4) . . ?
C37 C36 H36 118.5 . . ?
C35 C36 H36 118.5 . . ?
C38 C37 C36 119.8(5) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C39 C38 C37 118.6(5) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?
C38 C39 C40 120.8(4) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C39 C40 C35 123.4(5) . . ?
C39 C40 H40 118.3 . . ?
C35 C40 H40 118.3 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O3A C42 O3B 39.5(9) . . ?
O3A C42 C43 134.3(12) . . ?
O3B C42 C43 95.4(14) . . ?
O3A C42 C41 109.0(12) . . ?
O3B C42 C41 147.7(14) . . ?
C43 C42 C41 116.6(6) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C1 O1 C7 117.8(4) . . ?
C9 O2 C15B 103.2(8) . . ?
C9 O2 C15A 134.2(8) . . ?
C15B O2 C15A 32.1(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C5 2.152(5) . ?
Ru1 C3 2.162(4) . ?
Ru1 C4 2.167(5) . ?
Ru1 C2 2.172(5) . ?
Ru1 C6 2.180(4) . ?
Ru1 C1 2.254(5) . ?
Ru1 Cl2 2.4095(13) . ?
Ru1 Cl3 2.4328(14) . ?
Ru1 Cl1 2.4512(13) . ?
Ru2 C11 2.142(6) . ?
Ru2 C12 2.158(6) . ?
Ru2 C13 2.171(5) . ?
Ru2 C10 2.177(7) . ?
Ru2 C14 2.186(5) . ?
Ru2 C9 2.230(7) . ?
Ru2 Cl3 2.4242(16) . ?
Ru2 Cl2 2.4280(13) . ?
Ru2 Cl1 2.4441(13) . ?
B C29 1.642(7) . ?
B C35 1.654(7) . ?
B C17 1.653(7) . ?
B C23 1.661(7) . ?
C1 O1 1.322(6) . ?
C1 C6 1.426(8) . ?
C1 C2 1.445(7) . ?
C2 C3 1.408(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.422(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.423(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O1 1.461(6) . ?
C7 C8 1.483(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O2 1.362(8) . ?
C9 C14 1.392(9) . ?
C9 C10 1.404(9) . ?
C10 C11 1.406(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.404(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.430(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.433(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15A O2 1.508(10) . ?
C15A C16A 1.513(11) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15B O2 1.507(10) . ?
C15B C16B 1.513(11) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17 C18 1.406(6) . ?
C17 C22 1.428(6) . ?
C18 C19 1.395(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(7) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.395(7) . ?
C23 C28 1.393(7) . ?
C24 C25 1.394(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.382(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.402(7) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.398(6) . ?
C29 C34 1.416(7) . ?
C30 C31 1.389(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.389(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.370(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.395(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.393(6) . ?
C35 C36 1.409(7) . ?
C36 C37 1.402(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.390(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.377(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.503(11) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O3A 1.245(8) . ?
C42 O3B 1.246(8) . ?
C42 C43 1.455(9) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 Ru2 Cl1 Ru1 -118.9(3) . . . . ?
C12 Ru2 Cl1 Ru1 138.9(18) . . . . ?
C13 Ru2 Cl1 Ru1 123.0(3) . . . . ?
C10 Ru2 Cl1 Ru1 -139.75(19) . . . . ?
C14 Ru2 Cl1 Ru1 149.92(18) . . . . ?
C9 Ru2 Cl1 Ru1 -174.05(17) . . . . ?
Cl3 Ru2 Cl1 Ru1 41.42(4) . . . . ?
Cl2 Ru2 Cl1 Ru1 -40.66(5) . . . . ?
C5 Ru1 Cl1 Ru2 -118.4(3) . . . . ?
C3 Ru1 Cl1 Ru2 124.67(18) . . . . ?
C4 Ru1 Cl1 Ru2 139.0(8) . . . . ?
C2 Ru1 Cl1 Ru2 150.25(13) . . . . ?
C6 Ru1 Cl1 Ru2 -138.25(15) . . . . ?
C1 Ru1 Cl1 Ru2 -172.35(13) . . . . ?
Cl2 Ru1 Cl1 Ru2 41.00(5) . . . . ?
Cl3 Ru1 Cl1 Ru2 -41.29(5) . . . . ?
C5 Ru1 Cl2 Ru2 123.3(2) . . . . ?
C3 Ru1 Cl2 Ru2 -173.76(17) . . . . ?
C4 Ru1 Cl2 Ru2 148.70(17) . . . . ?
C2 Ru1 Cl2 Ru2 -139.81(17) . . . . ?
C6 Ru1 Cl2 Ru2 134.8(8) . . . . ?
C1 Ru1 Cl2 Ru2 -121.2(2) . . . . ?
Cl3 Ru1 Cl2 Ru2 39.56(5) . . . . ?
Cl1 Ru1 Cl2 Ru2 -41.22(5) . . . . ?
C11 Ru2 Cl2 Ru1 -173.4(3) . . . . ?
C12 Ru2 Cl2 Ru1 -138.5(3) . . . . ?
C13 Ru2 Cl2 Ru1 -118.3(3) . . . . ?
C10 Ru2 Cl2 Ru1 149.8(3) . . . . ?
C14 Ru2 Cl2 Ru1 145.5(10) . . . . ?
C9 Ru2 Cl2 Ru1 126.7(3) . . . . ?
Cl3 Ru2 Cl2 Ru1 -39.75(5) . . . . ?
Cl1 Ru2 Cl2 Ru1 41.40(5) . . . . ?
C11 Ru2 Cl3 Ru1 122.6(2) . . . . ?
C12 Ru2 Cl3 Ru1 146.68(17) . . . . ?
C13 Ru2 Cl3 Ru1 -175.82(18) . . . . ?
C10 Ru2 Cl3 Ru1 144.9(11) . . . . ?
C14 Ru2 Cl3 Ru1 -141.71(18) . . . . ?
C9 Ru2 Cl3 Ru1 -123.7(4) . . . . ?
Cl2 Ru2 Cl3 Ru1 39.33(5) . . . . ?
Cl1 Ru2 Cl3 Ru1 -41.73(4) . . . . ?
C5 Ru1 Cl3 Ru2 -171.85(14) . . . . ?
C3 Ru1 Cl3 Ru2 -119.6(2) . . . . ?
C4 Ru1 Cl3 Ru2 -138.42(14) . . . . ?
C2 Ru1 Cl3 Ru2 137.4(8) . . . . ?
C6 Ru1 Cl3 Ru2 150.51(14) . . . . ?
C1 Ru1 Cl3 Ru2 126.26(19) . . . . ?
Cl2 Ru1 Cl3 Ru2 -39.67(5) . . . . ?
Cl1 Ru1 Cl3 Ru2 41.63(5) . . . . ?
C5 Ru1 C1 O1 -149.7(5) . . . . ?
C3 Ru1 C1 O1 135.5(5) . . . . ?
C4 Ru1 C1 O1 173.3(5) . . . . ?
C2 Ru1 C1 O1 105.8(6) . . . . ?
C6 Ru1 C1 O1 -119.4(6) . . . . ?
Cl2 Ru1 C1 O1 76.8(5) . . . . ?
Cl3 Ru1 C1 O1 -77.7(5) . . . . ?
Cl1 Ru1 C1 O1 0.8(5) . . . . ?
C5 Ru1 C1 C6 -30.3(3) . . . . ?
C3 Ru1 C1 C6 -105.1(3) . . . . ?
C4 Ru1 C1 C6 -67.3(3) . . . . ?
C2 Ru1 C1 C6 -134.8(5) . . . . ?
Cl2 Ru1 C1 C6 -163.8(2) . . . . ?
Cl3 Ru1 C1 C6 41.7(3) . . . . ?
Cl1 Ru1 C1 C6 120.1(3) . . . . ?
C5 Ru1 C1 C2 104.5(4) . . . . ?
C3 Ru1 C1 C2 29.7(3) . . . . ?
C4 Ru1 C1 C2 67.5(3) . . . . ?
C6 Ru1 C1 C2 134.8(5) . . . . ?
Cl2 Ru1 C1 C2 -29.0(5) . . . . ?
Cl3 Ru1 C1 C2 176.5(3) . . . . ?
Cl1 Ru1 C1 C2 -105.1(3) . . . . ?
O1 C1 C2 C3 178.9(4) . . . . ?
C6 C1 C2 C3 -6.9(6) . . . . ?
Ru1 C1 C2 C3 -55.2(4) . . . . ?
O1 C1 C2 Ru1 -125.9(4) . . . . ?
C6 C1 C2 Ru1 48.3(4) . . . . ?
C5 Ru1 C2 C3 66.3(3) . . . . ?
C4 Ru1 C2 C3 29.3(3) . . . . ?
C6 Ru1 C2 C3 104.0(3) . . . . ?
C1 Ru1 C2 C3 131.5(5) . . . . ?
Cl2 Ru1 C2 C3 -65.3(3) . . . . ?
Cl3 Ru1 C2 C3 117.9(8) . . . . ?
Cl1 Ru1 C2 C3 -148.6(3) . . . . ?
C5 Ru1 C2 C1 -65.3(3) . . . . ?
C3 Ru1 C2 C1 -131.5(5) . . . . ?
C4 Ru1 C2 C1 -102.2(3) . . . . ?
C6 Ru1 C2 C1 -27.6(3) . . . . ?
Cl2 Ru1 C2 C1 163.2(3) . . . . ?
Cl3 Ru1 C2 C1 -13.7(10) . . . . ?
Cl1 Ru1 C2 C1 79.8(3) . . . . ?
C1 C2 C3 C4 3.2(7) . . . . ?
Ru1 C2 C3 C4 -53.7(4) . . . . ?
C1 C2 C3 Ru1 56.9(4) . . . . ?
C5 Ru1 C3 C2 -103.7(3) . . . . ?
C4 Ru1 C3 C2 -132.6(4) . . . . ?
C6 Ru1 C3 C2 -66.2(3) . . . . ?
C1 Ru1 C3 C2 -29.8(3) . . . . ?
Cl2 Ru1 C3 C2 121.8(3) . . . . ?
Cl3 Ru1 C3 C2 -161.8(2) . . . . ?
Cl1 Ru1 C3 C2 43.5(3) . . . . ?
C5 Ru1 C3 C4 28.9(3) . . . . ?
C2 Ru1 C3 C4 132.6(4) . . . . ?
C6 Ru1 C3 C4 66.4(3) . . . . ?
C1 Ru1 C3 C4 102.8(3) . . . . ?
Cl2 Ru1 C3 C4 -105.7(3) . . . . ?
Cl3 Ru1 C3 C4 -29.2(4) . . . . ?
Cl1 Ru1 C3 C4 176.1(2) . . . . ?
C2 C3 C4 C5 0.9(7) . . . . ?
Ru1 C3 C4 C5 -52.9(4) . . . . ?
C2 C3 C4 Ru1 53.8(4) . . . . ?
C3 Ru1 C4 C5 132.6(5) . . . . ?
C2 Ru1 C4 C5 103.6(4) . . . . ?
C6 Ru1 C4 C5 28.9(3) . . . . ?
C1 Ru1 C4 C5 65.9(4) . . . . ?
Cl2 Ru1 C4 C5 -148.5(3) . . . . ?
Cl3 Ru1 C4 C5 -64.3(4) . . . . ?
Cl1 Ru1 C4 C5 115.4(8) . . . . ?
C5 Ru1 C4 C3 -132.6(5) . . . . ?
C2 Ru1 C4 C3 -29.0(3) . . . . ?
C6 Ru1 C4 C3 -103.6(3) . . . . ?
C1 Ru1 C4 C3 -66.6(3) . . . . ?
Cl2 Ru1 C4 C3 78.9(3) . . . . ?
Cl3 Ru1 C4 C3 163.1(3) . . . . ?
Cl1 Ru1 C4 C3 -17.2(10) . . . . ?
C3 C4 C5 C6 -1.2(7) . . . . ?
Ru1 C4 C5 C6 -54.2(4) . . . . ?
C3 C4 C5 Ru1 52.9(4) . . . . ?
C3 Ru1 C5 C4 -29.4(3) . . . . ?
C2 Ru1 C5 C4 -66.5(4) . . . . ?
C6 Ru1 C5 C4 -133.3(5) . . . . ?
C1 Ru1 C5 C4 -103.7(4) . . . . ?
Cl2 Ru1 C5 C4 43.5(4) . . . . ?
Cl3 Ru1 C5 C4 122.4(3) . . . . ?
Cl1 Ru1 C5 C4 -164.2(3) . . . . ?
C3 Ru1 C5 C6 104.0(4) . . . . ?
C4 Ru1 C5 C6 133.3(5) . . . . ?
C2 Ru1 C5 C6 66.8(3) . . . . ?
C1 Ru1 C5 C6 29.7(3) . . . . ?
Cl2 Ru1 C5 C6 176.8(2) . . . . ?
Cl3 Ru1 C5 C6 -104.3(3) . . . . ?
Cl1 Ru1 C5 C6 -30.8(5) . . . . ?
C4 C5 C6 C1 -2.7(7) . . . . ?
Ru1 C5 C6 C1 -56.8(4) . . . . ?
C4 C5 C6 Ru1 54.1(4) . . . . ?
O1 C1 C6 C5 -179.8(4) . . . . ?
C2 C1 C6 C5 6.6(6) . . . . ?
Ru1 C1 C6 C5 54.7(4) . . . . ?
O1 C1 C6 Ru1 125.5(4) . . . . ?
C2 C1 C6 Ru1 -48.1(4) . . . . ?
C3 Ru1 C6 C5 -66.0(3) . . . . ?
C4 Ru1 C6 C5 -28.5(3) . . . . ?
C2 Ru1 C6 C5 -103.1(3) . . . . ?
C1 Ru1 C6 C5 -131.0(4) . . . . ?
Cl2 Ru1 C6 C5 -13.8(10) . . . . ?
Cl3 Ru1 C6 C5 79.7(3) . . . . ?
Cl1 Ru1 C6 C5 162.0(3) . . . . ?
C5 Ru1 C6 C1 131.0(4) . . . . ?
C3 Ru1 C6 C1 65.0(3) . . . . ?
C4 Ru1 C6 C1 102.6(3) . . . . ?
C2 Ru1 C6 C1 28.0(3) . . . . ?
Cl2 Ru1 C6 C1 117.2(8) . . . . ?
Cl3 Ru1 C6 C1 -149.3(3) . . . . ?
Cl1 Ru1 C6 C1 -67.0(3) . . . . ?
C11 Ru2 C9 O2 -145.4(7) . . . . ?
C12 Ru2 C9 O2 177.3(6) . . . . ?
C13 Ru2 C9 O2 139.3(6) . . . . ?
C10 Ru2 C9 O2 -115.2(8) . . . . ?
C14 Ru2 C9 O2 109.9(7) . . . . ?
Cl3 Ru2 C9 O2 81.0(7) . . . . ?
Cl2 Ru2 C9 O2 -75.8(6) . . . . ?
Cl1 Ru2 C9 O2 3.5(6) . . . . ?
C11 Ru2 C9 C14 104.7(5) . . . . ?
C12 Ru2 C9 C14 67.4(4) . . . . ?
C13 Ru2 C9 C14 29.3(4) . . . . ?
C10 Ru2 C9 C14 134.9(7) . . . . ?
Cl3 Ru2 C9 C14 -29.0(6) . . . . ?
Cl2 Ru2 C9 C14 174.3(3) . . . . ?
Cl1 Ru2 C9 C14 -106.5(4) . . . . ?
C11 Ru2 C9 C10 -30.2(5) . . . . ?
C12 Ru2 C9 C10 -67.5(5) . . . . ?
C13 Ru2 C9 C10 -105.6(5) . . . . ?
C14 Ru2 C9 C10 -134.9(7) . . . . ?
Cl3 Ru2 C9 C10 -163.9(4) . . . . ?
Cl2 Ru2 C9 C10 39.4(6) . . . . ?
Cl1 Ru2 C9 C10 118.6(5) . . . . ?
O2 C9 C10 C11 178.9(5) . . . . ?
C14 C9 C10 C11 4.1(8) . . . . ?
Ru2 C9 C10 C11 54.3(5) . . . . ?
O2 C9 C10 Ru2 124.5(6) . . . . ?
C14 C9 C10 Ru2 -50.2(5) . . . . ?
C11 Ru2 C10 C9 131.0(7) . . . . ?
C12 Ru2 C10 C9 102.5(5) . . . . ?
C13 Ru2 C10 C9 64.6(5) . . . . ?
C14 Ru2 C10 C9 27.3(4) . . . . ?
Cl3 Ru2 C10 C9 104.4(12) . . . . ?
Cl2 Ru2 C10 C9 -151.8(4) . . . . ?
Cl1 Ru2 C10 C9 -68.7(5) . . . . ?
C12 Ru2 C10 C11 -28.5(4) . . . . ?
C13 Ru2 C10 C11 -66.5(4) . . . . ?
C14 Ru2 C10 C11 -103.7(5) . . . . ?
C9 Ru2 C10 C11 -131.0(7) . . . . ?
Cl3 Ru2 C10 C11 -26.6(14) . . . . ?
Cl2 Ru2 C10 C11 77.1(4) . . . . ?
Cl1 Ru2 C10 C11 160.3(4) . . . . ?
C9 C10 C11 C12 -2.3(9) . . . . ?
Ru2 C10 C11 C12 53.9(5) . . . . ?
C9 C10 C11 Ru2 -56.2(5) . . . . ?
C13 Ru2 C11 C12 -30.1(4) . . . . ?
C10 Ru2 C11 C12 -133.7(6) . . . . ?
C14 Ru2 C11 C12 -68.2(4) . . . . ?
C9 Ru2 C11 C12 -104.2(4) . . . . ?
Cl3 Ru2 C11 C12 40.3(5) . . . . ?
Cl2 Ru2 C11 C12 118.8(4) . . . . ?
Cl1 Ru2 C11 C12 -166.8(3) . . . . ?
C12 Ru2 C11 C10 133.7(6) . . . . ?
C13 Ru2 C11 C10 103.6(4) . . . . ?
C14 Ru2 C11 C10 65.5(4) . . . . ?
C9 Ru2 C11 C10 29.6(4) . . . . ?
Cl3 Ru2 C11 C10 174.1(3) . . . . ?
Cl2 Ru2 C11 C10 -107.4(4) . . . . ?
Cl1 Ru2 C11 C10 -33.0(5) . . . . ?
C10 C11 C12 C13 -0.2(9) . . . . ?
Ru2 C11 C12 C13 54.1(5) . . . . ?
C10 C11 C12 Ru2 -54.2(5) . . . . ?
C13 Ru2 C12 C11 131.4(7) . . . . ?
C10 Ru2 C12 C11 28.4(4) . . . . ?
C14 Ru2 C12 C11 101.4(5) . . . . ?
C9 Ru2 C12 C11 65.1(5) . . . . ?
Cl3 Ru2 C12 C11 -151.2(4) . . . . ?
Cl2 Ru2 C12 C11 -67.6(5) . . . . ?
Cl1 Ru2 C12 C11 112.8(18) . . . . ?
C11 Ru2 C12 C13 -131.4(7) . . . . ?
C10 Ru2 C12 C13 -103.0(5) . . . . ?
C14 Ru2 C12 C13 -30.1(4) . . . . ?
C9 Ru2 C12 C13 -66.3(5) . . . . ?
Cl3 Ru2 C12 C13 77.3(4) . . . . ?
Cl2 Ru2 C12 C13 161.0(4) . . . . ?
Cl1 Ru2 C12 C13 -19(2) . . . . ?
C11 C12 C13 C14 0.8(8) . . . . ?
Ru2 C12 C13 C14 54.4(5) . . . . ?
C11 C12 C13 Ru2 -53.6(5) . . . . ?
C11 Ru2 C13 C12 29.7(5) . . . . ?
C10 Ru2 C13 C12 66.9(5) . . . . ?
C14 Ru2 C13 C12 131.1(6) . . . . ?
C9 Ru2 C13 C12 103.0(5) . . . . ?
Cl3 Ru2 C13 C12 -106.9(5) . . . . ?
Cl2 Ru2 C13 C12 -31.7(6) . . . . ?
Cl1 Ru2 C13 C12 176.4(4) . . . . ?
C11 Ru2 C13 C14 -101.3(5) . . . . ?
C12 Ru2 C13 C14 -131.1(6) . . . . ?
C10 Ru2 C13 C14 -64.1(4) . . . . ?
C9 Ru2 C13 C14 -28.1(3) . . . . ?
Cl3 Ru2 C13 C14 122.0(3) . . . . ?
Cl2 Ru2 C13 C14 -162.8(3) . . . . ?
Cl1 Ru2 C13 C14 45.3(5) . . . . ?
O2 C9 C14 C13 -178.5(5) . . . . ?
C10 C9 C14 C13 -3.6(8) . . . . ?
Ru2 C9 C14 C13 -53.5(5) . . . . ?
O2 C9 C14 Ru2 -125.0(5) . . . . ?
C10 C9 C14 Ru2 49.9(5) . . . . ?
C12 C13 C14 C9 1.1(8) . . . . ?
Ru2 C13 C14 C9 54.9(5) . . . . ?
C12 C13 C14 Ru2 -53.9(4) . . . . ?
C11 Ru2 C14 C9 -64.9(5) . . . . ?
C12 Ru2 C14 C9 -102.8(5) . . . . ?
C13 Ru2 C14 C9 -133.0(5) . . . . ?
C10 Ru2 C14 C9 -27.6(4) . . . . ?
Cl3 Ru2 C14 C9 162.4(4) . . . . ?
Cl2 Ru2 C14 C9 -23.1(12) . . . . ?
Cl1 Ru2 C14 C9 78.9(4) . . . . ?
C11 Ru2 C14 C13 68.1(5) . . . . ?
C12 Ru2 C14 C13 30.2(4) . . . . ?
C10 Ru2 C14 C13 105.4(5) . . . . ?
C9 Ru2 C14 C13 133.0(5) . . . . ?
Cl3 Ru2 C14 C13 -64.5(4) . . . . ?
Cl2 Ru2 C14 C13 109.9(10) . . . . ?
Cl1 Ru2 C14 C13 -148.1(3) . . . . ?
C29 B C17 C18 16.5(6) . . . . ?
C35 B C17 C18 -105.2(5) . . . . ?
C23 B C17 C18 135.0(4) . . . . ?
C29 B C17 C22 -164.3(4) . . . . ?
C35 B C17 C22 74.0(5) . . . . ?
C23 B C17 C22 -45.8(5) . . . . ?
C22 C17 C18 C19 -0.2(7) . . . . ?
B C17 C18 C19 179.1(5) . . . . ?
C17 C18 C19 C20 -0.6(8) . . . . ?
C18 C19 C20 C21 0.9(8) . . . . ?
C19 C20 C21 C22 -0.4(8) . . . . ?
C20 C21 C22 C17 -0.4(7) . . . . ?
C18 C17 C22 C21 0.7(6) . . . . ?
B C17 C22 C21 -178.6(4) . . . . ?
C29 B C23 C24 104.0(5) . . . . ?
C35 B C23 C24 -134.2(4) . . . . ?
C17 B C23 C24 -13.8(6) . . . . ?
C29 B C23 C28 -73.2(5) . . . . ?
C35 B C23 C28 48.5(5) . . . . ?
C17 B C23 C28 168.9(4) . . . . ?
C28 C23 C24 C25 -0.6(6) . . . . ?
B C23 C24 C25 -178.0(4) . . . . ?
C23 C24 C25 C26 0.2(7) . . . . ?
C24 C25 C26 C27 0.7(7) . . . . ?
C25 C26 C27 C28 -1.1(7) . . . . ?
C24 C23 C28 C27 0.2(7) . . . . ?
B C23 C28 C27 177.7(4) . . . . ?
C26 C27 C28 C23 0.6(8) . . . . ?
C35 B C29 C30 -158.9(4) . . . . ?
C17 B C29 C30 81.2(5) . . . . ?
C23 B C29 C30 -39.5(6) . . . . ?
C35 B C29 C34 29.7(6) . . . . ?
C17 B C29 C34 -90.2(5) . . . . ?
C23 B C29 C34 149.1(4) . . . . ?
C34 C29 C30 C31 2.1(6) . . . . ?
B C29 C30 C31 -170.0(4) . . . . ?
C29 C30 C31 C32 -1.4(7) . . . . ?
C30 C31 C32 C33 0.9(7) . . . . ?
C31 C32 C33 C34 -1.4(8) . . . . ?
C32 C33 C34 C29 2.3(8) . . . . ?
C30 C29 C34 C33 -2.5(7) . . . . ?
B C29 C34 C33 169.4(5) . . . . ?
C29 B C35 C40 -145.4(4) . . . . ?
C17 B C35 C40 -26.7(6) . . . . ?
C23 B C35 C40 95.2(5) . . . . ?
C29 B C35 C36 36.7(6) . . . . ?
C17 B C35 C36 155.3(4) . . . . ?
C23 B C35 C36 -82.7(5) . . . . ?
C40 C35 C36 C37 -1.1(7) . . . . ?
B C35 C36 C37 177.0(5) . . . . ?
C35 C36 C37 C38 0.9(8) . . . . ?
C36 C37 C38 C39 0.0(8) . . . . ?
C37 C38 C39 C40 -0.6(8) . . . . ?
C38 C39 C40 C35 0.4(7) . . . . ?
C36 C35 C40 C39 0.5(7) . . . . ?
B C35 C40 C39 -177.6(4) . . . . ?
C6 C1 O1 C7 -5.1(6) . . . . ?
C2 C1 O1 C7 168.6(4) . . . . ?
Ru1 C1 O1 C7 86.3(5) . . . . ?
C8 C7 O1 C1 180.0(4) . . . . ?
C14 C9 O2 C15B 169.0(9) . . . . ?
C10 C9 O2 C15B -5.8(10) . . . . ?
Ru2 C9 O2 C15B 83.0(10) . . . . ?
C14 C9 O2 C15A 178.8(7) . . . . ?
C10 C9 O2 C15A 4.0(11) . . . . ?
Ru2 C9 O2 C15A 92.7(9) . . . . ?
C16B C15B O2 C9 -171.9(12) . . . . ?
C16B C15B O2 C15A 21.3(13) . . . . ?
C16A C15A O2 C9 -88.2(13) . . . . ?
C16A C15A O2 C15B -70.1(16) . . . . ?
|
1100815.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 10:38:59 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180565 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100815.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100815
loop_
_publ_author_name
'Soleimannejad, Janet'
'White, Colin'
_publ_section_title
;
A Convenient One-Pot Synthesis of a Functionalized-Arene Ruthenium
Half-Sandwich Compound [RuCl~2~(\h^6^-C~6~H~5~OCH~2~CH~2~OH)]~2~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2538
_journal_page_last 2541
_journal_paper_doi 10.1021/om049044x
_journal_volume 24
_chemical_formula_moiety 'C16 H20 Cl4 O4 Ru2'
_chemical_formula_sum 'C16 H20 Cl4 O4 Ru2'
_chemical_formula_weight 620.26
_chemical_name_systematic
;
di-\m-chloro-bis{chloro(\h^6^-2-hydroxyethoxybenzene)ruthenium(II)}
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 116.519(11)
_cell_angle_beta 108.648(9)
_cell_angle_gamma 91.492(8)
_cell_formula_units_Z 1
_cell_length_a 6.149(3)
_cell_length_b 9.548(4)
_cell_length_c 9.604(5)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 28.37
_cell_measurement_theta_min 2.43
_cell_volume 468.4(4)
_computing_cell_refinement SMART
_computing_data_collection 'SMART (Bruker, 1997-2001)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type 'Bruker SMART1000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0619
_diffrn_reflns_av_sigmaI/netI 0.1160
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 2335
_diffrn_reflns_theta_full 24.99
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 2.43
_diffrn_standards_decay_% 0.00
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.203
_exptl_absorpt_correction_T_max 0.8435
_exptl_absorpt_correction_T_min 0.7479
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details sadabs
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.199
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 304
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.08
_refine_diff_density_max 1.358
_refine_diff_density_min -2.053
_refine_diff_density_rms 0.242
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.950
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 118
_refine_ls_number_reflns 1622
_refine_ls_number_restraints 55
_refine_ls_restrained_S_all 0.936
_refine_ls_R_factor_all 0.1107
_refine_ls_R_factor_gt 0.0727
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1678
_refine_ls_wR_factor_ref 0.1857
_reflns_number_gt 1101
_reflns_number_total 1622
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om049044xsi20050310_111611.cif
_cod_data_source_block iwh72jm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.
'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru -0.38857(19) 0.21613(11) -0.39112(13) 0.0287(4) Uani 1 1 d . . .
Cl1 Cl -0.7314(6) 0.2265(4) -0.5901(4) 0.0432(9) Uani 1 1 d . . .
Cl2 Cl -0.3652(6) -0.0233(3) -0.6216(4) 0.0341(8) Uani 1 1 d . . .
O1 O -0.3051(17) 0.3242(11) -0.0039(12) 0.048(3) Uani 1 1 d . . .
O2 O -0.576(2) 0.1841(16) 0.1045(18) 0.085(4) Uani 1 1 d . . .
H2A H -0.6171 0.1944 0.1842 0.102 Uiso 1 1 d R . .
C1 C -0.338(3) 0.4410(15) -0.1688(15) 0.0407(18) Uani 1 1 d U . .
H1 H -0.4507 0.4936 -0.1276 0.049 Uiso 1 1 calc R . .
C2 C -0.273(3) 0.4668(15) -0.2882(15) 0.0416(18) Uani 1 1 d U . .
H2 H -0.3426 0.5384 -0.3241 0.050 Uiso 1 1 calc R . .
C3 C -0.118(3) 0.3945(15) -0.3496(16) 0.0427(18) Uani 1 1 d U . .
H3 H -0.0776 0.4132 -0.4282 0.051 Uiso 1 1 calc R . .
C4 C -0.015(3) 0.2870(15) -0.2936(16) 0.0440(18) Uani 1 1 d U . .
H4 H 0.0982 0.2351 -0.3347 0.053 Uiso 1 1 calc R . .
C5 C -0.073(3) 0.2577(15) -0.1839(16) 0.0423(18) Uani 1 1 d U . .
H5 H -0.0066 0.1828 -0.1523 0.051 Uiso 1 1 calc R . .
C6 C -0.234(2) 0.3382(14) -0.1158(15) 0.0401(18) Uani 1 1 d U . .
C7 C -0.227(3) 0.2048(19) 0.048(2) 0.060(3) Uani 1 1 d U . .
H7A H -0.2845 0.0960 -0.0489 0.072 Uiso 1 1 calc R . .
H7B H -0.0541 0.2249 0.0970 0.072 Uiso 1 1 calc R . .
C8 C -0.323(3) 0.2194(19) 0.171(2) 0.061(3) Uani 1 1 d U . .
H8A H -0.2663 0.3297 0.2657 0.073 Uiso 1 1 calc R . .
H8B H -0.2644 0.1457 0.2146 0.073 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0384(7) 0.0212(5) 0.0290(6) 0.0150(4) 0.0117(4) -0.0029(4)
Cl1 0.047(2) 0.052(2) 0.045(2) 0.0347(17) 0.0171(17) 0.0091(16)
Cl2 0.0445(19) 0.0289(15) 0.0328(16) 0.0165(13) 0.0172(14) -0.0038(13)
O1 0.057(7) 0.050(6) 0.048(6) 0.034(5) 0.018(5) 0.000(5)
O2 0.100(11) 0.085(9) 0.096(10) 0.060(8) 0.044(9) 0.005(8)
C1 0.055(4) 0.028(3) 0.028(3) 0.010(3) 0.010(3) -0.012(3)
C2 0.055(4) 0.029(3) 0.030(3) 0.010(3) 0.010(3) -0.015(3)
C3 0.055(4) 0.031(3) 0.030(3) 0.009(3) 0.011(3) -0.017(3)
C4 0.053(4) 0.030(3) 0.031(3) 0.006(3) 0.009(3) -0.015(3)
C5 0.053(4) 0.028(3) 0.029(3) 0.007(3) 0.007(3) -0.013(3)
C6 0.054(4) 0.028(3) 0.027(3) 0.010(3) 0.009(3) -0.012(3)
C7 0.069(8) 0.057(7) 0.056(7) 0.040(6) 0.007(6) -0.014(6)
C8 0.070(8) 0.058(7) 0.056(7) 0.041(6) 0.007(6) -0.016(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ru1 C4 67.0(6) . . ?
C2 Ru1 C5 80.0(5) . . ?
C4 Ru1 C5 36.5(5) . . ?
C2 Ru1 C3 35.9(5) . . ?
C4 Ru1 C3 39.0(5) . . ?
C5 Ru1 C3 68.6(5) . . ?
C2 Ru1 C1 39.2(5) . . ?
C4 Ru1 C1 79.8(6) . . ?
C5 Ru1 C1 67.6(6) . . ?
C3 Ru1 C1 68.2(5) . . ?
C2 Ru1 C6 68.0(5) . . ?
C4 Ru1 C6 67.0(5) . . ?
C5 Ru1 C6 37.9(5) . . ?
C3 Ru1 C6 80.5(5) . . ?
C1 Ru1 C6 36.8(5) . . ?
C2 Ru1 Cl1 89.1(4) . . ?
C4 Ru1 Cl1 140.7(4) . . ?
C5 Ru1 Cl1 168.5(4) . . ?
C3 Ru1 Cl1 104.5(4) . . ?
C1 Ru1 Cl1 101.5(4) . . ?
C6 Ru1 Cl1 133.8(4) . . ?
C2 Ru1 Cl2 135.6(4) . . ?
C4 Ru1 Cl2 89.4(4) . . ?
C5 Ru1 Cl2 103.5(4) . . ?
C3 Ru1 Cl2 103.3(4) . . ?
C1 Ru1 Cl2 169.2(4) . . ?
C6 Ru1 Cl2 137.6(4) . . ?
Cl1 Ru1 Cl2 86.85(13) . . ?
C2 Ru1 Cl2 142.5(4) . 2_454 ?
C4 Ru1 Cl2 130.6(4) . 2_454 ?
C5 Ru1 Cl2 98.9(3) . 2_454 ?
C3 Ru1 Cl2 167.3(4) . 2_454 ?
C1 Ru1 Cl2 105.4(3) . 2_454 ?
C6 Ru1 Cl2 88.0(3) . 2_454 ?
Cl1 Ru1 Cl2 87.44(12) . 2_454 ?
Cl2 Ru1 Cl2 81.50(12) . 2_454 ?
Ru1 Cl2 Ru1 98.50(12) . 2_454 ?
C6 O1 C7 119.1(12) . . ?
C8 O2 H2A 106.4 . . ?
C6 C1 C2 118.6(14) . . ?
C6 C1 Ru1 72.7(8) . . ?
C2 C1 Ru1 69.1(7) . . ?
C6 C1 H1 120.7 . . ?
C2 C1 H1 120.7 . . ?
Ru1 C1 H1 129.8 . . ?
C3 C2 C1 122.5(14) . . ?
C3 C2 Ru1 72.8(8) . . ?
C1 C2 Ru1 71.7(7) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
Ru1 C2 H2 129.3 . . ?
C2 C3 C4 117.8(13) . . ?
C2 C3 Ru1 71.3(8) . . ?
C4 C3 Ru1 70.1(7) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
Ru1 C3 H3 129.8 . . ?
C5 C4 C3 121.7(15) . . ?
C5 C4 Ru1 72.3(9) . . ?
C3 C4 Ru1 70.9(8) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
Ru1 C4 H4 130.3 . . ?
C4 C5 C6 120.2(14) . . ?
C4 C5 Ru1 71.1(8) . . ?
C6 C5 Ru1 72.6(8) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
Ru1 C5 H5 128.6 . . ?
O1 C6 C1 113.8(13) . . ?
O1 C6 C5 126.9(12) . . ?
C1 C6 C5 119.2(12) . . ?
O1 C6 Ru1 131.1(9) . . ?
C1 C6 Ru1 70.5(8) . . ?
C5 C6 Ru1 69.5(8) . . ?
C8 C7 O1 106.9(14) . . ?
C8 C7 H7A 110.3 . . ?
O1 C7 H7A 110.3 . . ?
C8 C7 H7B 110.3 . . ?
O1 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?
C7 C8 O2 112.7(13) . . ?
C7 C8 H8A 109.0 . . ?
O2 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
O2 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C2 2.136(12) . ?
Ru1 C4 2.144(14) . ?
Ru1 C5 2.159(14) . ?
Ru1 C3 2.155(12) . ?
Ru1 C1 2.171(13) . ?
Ru1 C6 2.199(12) . ?
Ru1 Cl1 2.390(4) . ?
Ru1 Cl2 2.418(3) . ?
Ru1 Cl2 2.423(3) 2_454 ?
Cl2 Ru1 2.423(3) 2_454 ?
O1 C6 1.337(15) . ?
O1 C7 1.472(17) . ?
O2 C8 1.45(2) . ?
O2 H2A 0.8471 . ?
C1 C6 1.38(2) . ?
C1 C2 1.444(17) . ?
C1 H1 0.9500 . ?
C2 C3 1.32(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.43(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.349(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.42(2) . ?
C5 H5 0.9500 . ?
C7 C8 1.43(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A Cl1 0.85 2.38 3.230(14) 179.3 1_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Ru1 Cl2 Ru1 -173.4(6) . . . 2_454 ?
C4 Ru1 Cl2 Ru1 131.2(4) . . . 2_454 ?
C5 Ru1 Cl2 Ru1 97.2(4) . . . 2_454 ?
C3 Ru1 Cl2 Ru1 168.0(4) . . . 2_454 ?
C1 Ru1 Cl2 Ru1 130.9(18) . . . 2_454 ?
C6 Ru1 Cl2 Ru1 77.5(5) . . . 2_454 ?
Cl1 Ru1 Cl2 Ru1 -87.88(13) . . . 2_454 ?
Cl2 Ru1 Cl2 Ru1 0.0 2_454 . . 2_454 ?
C2 Ru1 C1 C6 -130.9(13) . . . . ?
C4 Ru1 C1 C6 -64.9(9) . . . . ?
C5 Ru1 C1 C6 -28.9(8) . . . . ?
C3 Ru1 C1 C6 -103.8(9) . . . . ?
Cl1 Ru1 C1 C6 155.0(8) . . . . ?
Cl2 Ru1 C1 C6 -65(2) . . . . ?
Cl2 Ru1 C1 C6 64.5(9) 2_454 . . . ?
C4 Ru1 C1 C2 65.9(9) . . . . ?
C5 Ru1 C1 C2 102.0(9) . . . . ?
C3 Ru1 C1 C2 27.1(9) . . . . ?
C6 Ru1 C1 C2 130.9(13) . . . . ?
Cl1 Ru1 C1 C2 -74.1(9) . . . . ?
Cl2 Ru1 C1 C2 66(2) . . . . ?
Cl2 Ru1 C1 C2 -164.6(8) 2_454 . . . ?
C6 C1 C2 C3 0.7(19) . . . . ?
Ru1 C1 C2 C3 -54.6(11) . . . . ?
C6 C1 C2 Ru1 55.3(11) . . . . ?
C4 Ru1 C2 C3 31.4(8) . . . . ?
C5 Ru1 C2 C3 67.2(9) . . . . ?
C1 Ru1 C2 C3 133.9(13) . . . . ?
C6 Ru1 C2 C3 104.7(9) . . . . ?
Cl1 Ru1 C2 C3 -116.5(8) . . . . ?
Cl2 Ru1 C2 C3 -31.9(11) . . . . ?
Cl2 Ru1 C2 C3 158.8(7) 2_454 . . . ?
C4 Ru1 C2 C1 -102.5(9) . . . . ?
C5 Ru1 C2 C1 -66.7(9) . . . . ?
C3 Ru1 C2 C1 -133.9(13) . . . . ?
C6 Ru1 C2 C1 -29.2(9) . . . . ?
Cl1 Ru1 C2 C1 109.6(8) . . . . ?
Cl2 Ru1 C2 C1 -165.8(7) . . . . ?
Cl2 Ru1 C2 C1 24.9(12) 2_454 . . . ?
C1 C2 C3 C4 -0.1(18) . . . . ?
Ru1 C2 C3 C4 -54.2(10) . . . . ?
C1 C2 C3 Ru1 54.1(11) . . . . ?
C4 Ru1 C3 C2 -130.3(12) . . . . ?
C5 Ru1 C3 C2 -102.8(9) . . . . ?
C1 Ru1 C3 C2 -29.3(8) . . . . ?
C6 Ru1 C3 C2 -65.4(9) . . . . ?
Cl1 Ru1 C3 C2 67.5(8) . . . . ?
Cl2 Ru1 C3 C2 157.7(7) . . . . ?
Cl2 Ru1 C3 C2 -92(2) 2_454 . . . ?
C2 Ru1 C3 C4 130.3(12) . . . . ?
C5 Ru1 C3 C4 27.4(8) . . . . ?
C1 Ru1 C3 C4 101.0(9) . . . . ?
C6 Ru1 C3 C4 64.9(8) . . . . ?
Cl1 Ru1 C3 C4 -162.2(7) . . . . ?
Cl2 Ru1 C3 C4 -72.1(8) . . . . ?
Cl2 Ru1 C3 C4 39(2) 2_454 . . . ?
C2 C3 C4 C5 1.0(18) . . . . ?
Ru1 C3 C4 C5 -53.8(11) . . . . ?
C2 C3 C4 Ru1 54.8(10) . . . . ?
C2 Ru1 C4 C5 104.8(9) . . . . ?
C3 Ru1 C4 C5 133.9(12) . . . . ?
C1 Ru1 C4 C5 66.0(9) . . . . ?
C6 Ru1 C4 C5 29.9(8) . . . . ?
Cl1 Ru1 C4 C5 161.8(7) . . . . ?
Cl2 Ru1 C4 C5 -113.9(8) . . . . ?
Cl2 Ru1 C4 C5 -35.7(10) 2_454 . . . ?
C2 Ru1 C4 C3 -29.1(8) . . . . ?
C5 Ru1 C4 C3 -133.9(12) . . . . ?
C1 Ru1 C4 C3 -67.9(8) . . . . ?
C6 Ru1 C4 C3 -104.0(9) . . . . ?
Cl1 Ru1 C4 C3 27.9(11) . . . . ?
Cl2 Ru1 C4 C3 112.2(8) . . . . ?
Cl2 Ru1 C4 C3 -169.6(6) 2_454 . . . ?
C3 C4 C5 C6 -2.5(19) . . . . ?
Ru1 C4 C5 C6 -55.6(11) . . . . ?
C3 C4 C5 Ru1 53.2(11) . . . . ?
C2 Ru1 C5 C4 -64.7(9) . . . . ?
C3 Ru1 C5 C4 -29.1(9) . . . . ?
C1 Ru1 C5 C4 -103.5(9) . . . . ?
C6 Ru1 C5 C4 -131.6(11) . . . . ?
Cl1 Ru1 C5 C4 -84(2) . . . . ?
Cl2 Ru1 C5 C4 70.0(8) . . . . ?
Cl2 Ru1 C5 C4 153.4(8) 2_454 . . . ?
C2 Ru1 C5 C6 67.0(7) . . . . ?
C4 Ru1 C5 C6 131.6(11) . . . . ?
C3 Ru1 C5 C6 102.5(8) . . . . ?
C1 Ru1 C5 C6 28.1(7) . . . . ?
Cl1 Ru1 C5 C6 48(2) . . . . ?
Cl2 Ru1 C5 C6 -158.3(6) . . . . ?
Cl2 Ru1 C5 C6 -75.0(7) 2_454 . . . ?
C7 O1 C6 C1 173.2(11) . . . . ?
C7 O1 C6 C5 -5.3(19) . . . . ?
C7 O1 C6 Ru1 88.9(16) . . . . ?
C2 C1 C6 O1 179.2(10) . . . . ?
Ru1 C1 C6 O1 -127.3(10) . . . . ?
C2 C1 C6 C5 -2.1(18) . . . . ?
Ru1 C1 C6 C5 51.4(11) . . . . ?
C2 C1 C6 Ru1 -53.5(10) . . . . ?
C4 C5 C6 O1 -178.5(12) . . . . ?
Ru1 C5 C6 O1 126.6(13) . . . . ?
C4 C5 C6 C1 3.0(18) . . . . ?
Ru1 C5 C6 C1 -51.9(11) . . . . ?
C4 C5 C6 Ru1 54.9(11) . . . . ?
C2 Ru1 C6 O1 136.1(15) . . . . ?
C4 Ru1 C6 O1 -150.6(15) . . . . ?
C5 Ru1 C6 O1 -121.7(16) . . . . ?
C3 Ru1 C6 O1 171.2(14) . . . . ?
C1 Ru1 C6 O1 105.1(17) . . . . ?
Cl1 Ru1 C6 O1 70.2(14) . . . . ?
Cl2 Ru1 C6 O1 -89.5(14) . . . . ?
Cl2 Ru1 C6 O1 -14.4(13) 2_454 . . . ?
C2 Ru1 C6 C1 31.0(9) . . . . ?
C4 Ru1 C6 C1 104.3(9) . . . . ?
C5 Ru1 C6 C1 133.2(11) . . . . ?
C3 Ru1 C6 C1 66.1(9) . . . . ?
Cl1 Ru1 C6 C1 -34.9(10) . . . . ?
Cl2 Ru1 C6 C1 165.5(6) . . . . ?
Cl2 Ru1 C6 C1 -119.5(8) 2_454 . . . ?
C2 Ru1 C6 C5 -102.3(8) . . . . ?
C4 Ru1 C6 C5 -28.9(7) . . . . ?
C3 Ru1 C6 C5 -67.1(8) . . . . ?
C1 Ru1 C6 C5 -133.2(11) . . . . ?
Cl1 Ru1 C6 C5 -168.2(6) . . . . ?
Cl2 Ru1 C6 C5 32.2(9) . . . . ?
Cl2 Ru1 C6 C5 107.3(7) 2_454 . . . ?
C6 O1 C7 C8 178.3(11) . . . . ?
O1 C7 C8 O2 62.6(16) . . . . ?
|
1100816.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-01 10:45:47 +0200 (Tue, 01 Nov 2016) $
#$Revision: 187722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100816.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100816
loop_
_publ_author_name
'Li, Xiao-Fang'
'Li, Yang-Guo'
'Li, Yue-Sheng'
'Chen, Yan-Xiang'
'Hu, Ning-Hai'
_publ_section_title
;
Copolymerization of Ethylene with Methyl Methacrylate with Neutral
Nickel(II) Complexes Bearing \b-Ketoiminato Chelate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2502
_journal_page_last 2510
_journal_paper_doi 10.1021/om049080w
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C46 H43 F3 N Ni O P'
_chemical_formula_weight 772.49
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 72.302(12)
_cell_angle_beta 70.461(13)
_cell_angle_gamma 68.172(15)
_cell_formula_units_Z 2
_cell_length_a 12.611(3)
_cell_length_b 12.665(2)
_cell_length_c 14.887(2)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 9.31
_cell_measurement_theta_min 5.20
_cell_volume 2035.8(6)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0251
_diffrn_reflns_av_sigmaI/netI 0.0889
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 8418
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_min 1.77
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.564
_exptl_absorpt_correction_T_max 0.54954
_exptl_absorpt_correction_T_min 0.49629
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.260
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rod-like
_exptl_crystal_F_000 808
_exptl_crystal_size_max 0.52
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.28
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.872
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 482
_refine_ls_number_reflns 7098
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.872
_refine_ls_R_factor_all 0.0781
_refine_ls_R_factor_gt 0.0405
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0643
_refine_ls_wR_factor_ref 0.0696
_reflns_number_gt 4218
_reflns_number_total 7098
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100816
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.82357(3) 0.81734(3) 0.73541(3) 0.04088(11) Uani 1 1 d . . .
P P 0.68644(7) 0.73837(6) 0.75567(5) 0.0431(2) Uani 1 1 d . . .
O O 0.70004(15) 0.96034(15) 0.74550(13) 0.0489(5) Uani 1 1 d . . .
N N 0.93982(19) 0.87770(17) 0.74653(15) 0.0420(6) Uani 1 1 d . . .
F1 F 1.11005(17) 0.96791(16) 0.76664(17) 0.1017(7) Uani 1 1 d . . .
F2 F 1.00778(19) 1.13373(17) 0.7100(2) 0.1279(10) Uani 1 1 d . . .
F3 F 0.9557(2) 1.0592(2) 0.8594(2) 0.1350(11) Uani 1 1 d . . .
C1 C 0.9342(2) 0.6816(2) 0.6910(2) 0.0478(8) Uani 1 1 d . . .
C2 C 0.9955(3) 0.5804(3) 0.7451(2) 0.0634(9) Uani 1 1 d . . .
H2 H 0.9850 0.5755 0.8109 0.063 Uiso 1 1 calc R . .
C3 C 1.0714(3) 0.4870(3) 0.7033(3) 0.0893(13) Uani 1 1 d . . .
H3 H 1.1103 0.4203 0.7415 0.089 Uiso 1 1 calc R . .
C4 C 1.0903(3) 0.4915(4) 0.6064(4) 0.1083(17) Uani 1 1 d . . .
H4 H 1.1421 0.4284 0.5788 0.108 Uiso 1 1 calc R . .
C5 C 1.0321(3) 0.5899(4) 0.5501(3) 0.0915(13) Uani 1 1 d . . .
H5 H 1.0446 0.5940 0.4841 0.091 Uiso 1 1 calc R . .
C6 C 0.9545(3) 0.6833(3) 0.5925(2) 0.0613(9) Uani 1 1 d . . .
H6 H 0.9148 0.7490 0.5540 0.061 Uiso 1 1 calc R . .
C7 C 0.5488(2) 0.8067(2) 0.8375(2) 0.0442(7) Uani 1 1 d . . .
C8 C 0.4387(3) 0.8336(3) 0.8212(2) 0.0611(9) Uani 1 1 d . . .
H8 H 0.4324 0.8164 0.7671 0.061 Uiso 1 1 calc R . .
C9 C 0.3381(3) 0.8860(3) 0.8859(3) 0.0784(11) Uani 1 1 d . . .
H9 H 0.2647 0.9046 0.8742 0.078 Uiso 1 1 calc R . .
C10 C 0.3450(3) 0.9110(3) 0.9663(3) 0.0773(11) Uani 1 1 d . . .
H10 H 0.2768 0.9464 1.0090 0.077 Uiso 1 1 calc R . .
C11 C 0.4528(3) 0.8836(3) 0.9839(2) 0.0696(10) Uani 1 1 d . . .
H11 H 0.4580 0.8995 1.0390 0.070 Uiso 1 1 calc R . .
C12 C 0.5542(3) 0.8324(2) 0.9198(2) 0.0566(8) Uani 1 1 d . . .
H12 H 0.6272 0.8148 0.9320 0.057 Uiso 1 1 calc R . .
C13 C 0.6450(2) 0.7594(3) 0.6442(2) 0.0524(8) Uani 1 1 d . . .
C14 C 0.6544(3) 0.8569(3) 0.5730(3) 0.0860(12) Uani 1 1 d . . .
H14 H 0.6824 0.9101 0.5823 0.086 Uiso 1 1 calc R . .
C15 C 0.6229(4) 0.8765(4) 0.4882(3) 0.1312(19) Uani 1 1 d . . .
H15 H 0.6286 0.9434 0.4411 0.131 Uiso 1 1 calc R . .
C16 C 0.5832(4) 0.7982(5) 0.4724(3) 0.126(2) Uani 1 1 d . . .
H16 H 0.5628 0.8114 0.4145 0.126 Uiso 1 1 calc R . .
C17 C 0.5739(4) 0.7020(5) 0.5413(3) 0.1097(16) Uani 1 1 d . . .
H17 H 0.5473 0.6484 0.5309 0.110 Uiso 1 1 calc R . .
C18 C 0.6035(3) 0.6830(3) 0.6263(3) 0.0787(11) Uani 1 1 d . . .
H18 H 0.5955 0.6168 0.6735 0.079 Uiso 1 1 calc R . .
C19 C 0.7090(3) 0.5833(2) 0.8072(2) 0.0498(8) Uani 1 1 d . . .
C20 C 0.7856(3) 0.5024(3) 0.7507(2) 0.0668(10) Uani 1 1 d . . .
H20 H 0.8245 0.5282 0.6870 0.067 Uiso 1 1 calc R . .
C21 C 0.8050(3) 0.3847(3) 0.7872(3) 0.0862(12) Uani 1 1 d . . .
H21 H 0.8570 0.3318 0.7485 0.086 Uiso 1 1 calc R . .
C22 C 0.7478(3) 0.3462(3) 0.8799(3) 0.0860(12) Uani 1 1 d . . .
H22 H 0.7607 0.2669 0.9042 0.086 Uiso 1 1 calc R . .
C23 C 0.6709(3) 0.4236(3) 0.9382(3) 0.0759(10) Uani 1 1 d . . .
H23 H 0.6317 0.3967 1.0014 0.076 Uiso 1 1 calc R . .
C24 C 0.6524(3) 0.5422(3) 0.9016(2) 0.0613(9) Uani 1 1 d . . .
H24 H 0.6014 0.5946 0.9411 0.061 Uiso 1 1 calc R . .
C25 C 1.0462(2) 0.7931(2) 0.7719(2) 0.0429(7) Uani 1 1 d . . .
C26 C 1.0416(3) 0.7423(2) 0.8699(2) 0.0482(7) Uani 1 1 d . . .
C27 C 1.1441(3) 0.6614(3) 0.8926(2) 0.0657(9) Uani 1 1 d . . .
H27 H 1.1438 0.6259 0.9573 0.066 Uiso 1 1 calc R . .
C28 C 1.2461(3) 0.6329(3) 0.8211(3) 0.0732(10) Uani 1 1 d . . .
H28 H 1.3140 0.5793 0.8380 0.073 Uiso 1 1 calc R . .
C29 C 1.2484(3) 0.6830(3) 0.7251(3) 0.0673(9) Uani 1 1 d . . .
H29 H 1.3181 0.6627 0.6776 0.067 Uiso 1 1 calc R . .
C30 C 1.1489(3) 0.7632(2) 0.6976(2) 0.0509(8) Uani 1 1 d . . .
C31 C 0.9304(3) 0.7726(3) 0.9516(2) 0.0610(9) Uani 1 1 d . . .
H31 H 0.8739 0.8414 0.9233 0.061 Uiso 1 1 calc R . .
C32 C 0.8730(3) 0.6750(3) 0.9917(2) 0.0927(12) Uani 1 1 d . . .
H32A H 0.8566 0.6589 0.9395 0.093 Uiso 1 1 calc R . .
H32B H 0.8007 0.6985 1.0396 0.093 Uiso 1 1 calc R . .
H32C H 0.9256 0.6064 1.0211 0.093 Uiso 1 1 calc R . .
C33 C 0.9523(3) 0.8034(3) 1.0338(2) 0.1060(14) Uani 1 1 d . . .
H33A H 1.0031 0.7360 1.0662 0.106 Uiso 1 1 calc R . .
H33B H 0.8785 0.8294 1.0794 0.106 Uiso 1 1 calc R . .
H33C H 0.9891 0.8641 1.0074 0.106 Uiso 1 1 calc R . .
C34 C 1.1521(3) 0.8145(3) 0.5902(2) 0.0725(10) Uani 1 1 d . . .
H34 H 1.0723 0.8320 0.5835 0.073 Uiso 1 1 calc R . .
C35 C 1.1834(4) 0.9276(3) 0.5523(3) 0.1392(18) Uani 1 1 d . . .
H35A H 1.1207 0.9875 0.5821 0.139 Uiso 1 1 calc R . .
H35B H 1.1943 0.9493 0.4829 0.139 Uiso 1 1 calc R . .
H35C H 1.2550 0.9174 0.5679 0.139 Uiso 1 1 calc R . .
C36 C 1.2346(3) 0.7296(3) 0.5241(2) 0.1039(14) Uani 1 1 d . . .
H36A H 1.3148 0.7262 0.5148 0.104 Uiso 1 1 calc R . .
H36B H 1.2154 0.7555 0.4622 0.104 Uiso 1 1 calc R . .
H36C H 1.2254 0.6537 0.5536 0.104 Uiso 1 1 calc R . .
C37 C 0.9152(3) 0.9880(2) 0.7501(2) 0.0509(8) Uani 1 1 d . . .
C38 C 0.8090(3) 1.0758(2) 0.7421(2) 0.0551(8) Uani 1 1 d . . .
H38 H 0.8074 1.1517 0.7360 0.055 Uiso 1 1 calc R . .
C39 C 0.7071(3) 1.0594(2) 0.74253(18) 0.0425(7) Uani 1 1 d . . .
C40 C 0.9992(3) 1.0333(3) 0.7730(3) 0.0819(12) Uani 1 1 d . . .
C41 C 0.5952(3) 1.1582(2) 0.74503(19) 0.0449(7) Uani 1 1 d . . .
C42 C 0.5928(3) 1.2729(2) 0.7266(2) 0.0717(10) Uani 1 1 d . . .
H42 H 0.6629 1.2906 0.7113 0.072 Uiso 1 1 calc R . .
C43 C 0.4872(3) 1.3614(3) 0.7308(3) 0.0912(13) Uani 1 1 d . . .
H43 H 0.4872 1.4381 0.7173 0.091 Uiso 1 1 calc R . .
C44 C 0.3818(3) 1.3375(3) 0.7546(3) 0.0808(11) Uani 1 1 d . . .
H44 H 0.3108 1.3972 0.7584 0.081 Uiso 1 1 calc R . .
C45 C 0.3837(3) 1.2246(3) 0.7724(2) 0.0700(10) Uani 1 1 d . . .
H45 H 0.3134 1.2071 0.7884 0.070 Uiso 1 1 calc R . .
C46 C 0.4894(3) 1.1361(3) 0.7669(2) 0.0541(8) Uani 1 1 d . . .
H46 H 0.4890 1.0598 0.7783 0.054 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0406(2) 0.0370(2) 0.0500(2) -0.01385(17) -0.01054(19) -0.01383(18)
P 0.0433(5) 0.0421(4) 0.0500(5) -0.0141(4) -0.0115(4) -0.0161(4)
O 0.0397(12) 0.0370(11) 0.0709(14) -0.0164(10) -0.0129(11) -0.0092(10)
N 0.0400(15) 0.0349(13) 0.0543(15) -0.0122(11) -0.0144(12) -0.0100(12)
F1 0.0665(14) 0.0660(13) 0.205(2) -0.0483(14) -0.0661(15) -0.0111(11)
F2 0.0953(18) 0.0587(14) 0.255(3) -0.0174(16) -0.0739(19) -0.0359(13)
F3 0.113(2) 0.172(2) 0.188(3) -0.117(2) -0.0511(19) -0.0410(18)
C1 0.0416(19) 0.0463(18) 0.067(2) -0.0223(16) -0.0132(17) -0.0173(15)
C2 0.058(2) 0.053(2) 0.092(3) -0.0304(19) -0.027(2) -0.0109(18)
C3 0.061(3) 0.056(2) 0.162(4) -0.046(3) -0.042(3) 0.002(2)
C4 0.062(3) 0.098(3) 0.179(5) -0.103(4) -0.001(3) -0.005(3)
C5 0.077(3) 0.111(3) 0.107(3) -0.077(3) 0.006(3) -0.033(3)
C6 0.053(2) 0.069(2) 0.073(2) -0.0341(19) -0.0041(18) -0.0241(18)
C7 0.0427(19) 0.0444(17) 0.0477(19) -0.0104(14) -0.0064(15) -0.0192(15)
C8 0.052(2) 0.070(2) 0.066(2) -0.0230(18) -0.0123(19) -0.0182(19)
C9 0.044(2) 0.087(3) 0.101(3) -0.030(2) -0.013(2) -0.012(2)
C10 0.065(3) 0.068(2) 0.077(3) -0.023(2) 0.014(2) -0.019(2)
C11 0.086(3) 0.073(2) 0.050(2) -0.0202(18) -0.001(2) -0.033(2)
C12 0.055(2) 0.063(2) 0.055(2) -0.0179(17) -0.0088(18) -0.0214(18)
C13 0.0418(19) 0.068(2) 0.0517(19) -0.0213(17) -0.0106(16) -0.0145(17)
C14 0.104(3) 0.093(3) 0.074(3) 0.006(2) -0.047(2) -0.041(3)
C15 0.157(5) 0.167(5) 0.079(3) 0.020(3) -0.066(3) -0.062(4)
C16 0.118(4) 0.212(7) 0.065(3) -0.042(4) -0.041(3) -0.042(4)
C17 0.093(3) 0.182(5) 0.095(3) -0.071(3) -0.031(3) -0.046(4)
C18 0.084(3) 0.101(3) 0.078(3) -0.036(2) -0.023(2) -0.041(2)
C19 0.047(2) 0.0453(18) 0.065(2) -0.0138(16) -0.0134(17) -0.0209(16)
C20 0.071(2) 0.051(2) 0.085(3) -0.0221(19) -0.007(2) -0.0301(19)
C21 0.081(3) 0.048(2) 0.131(4) -0.032(2) -0.010(3) -0.025(2)
C22 0.087(3) 0.046(2) 0.132(4) -0.007(2) -0.037(3) -0.028(2)
C23 0.084(3) 0.064(2) 0.079(3) 0.009(2) -0.025(2) -0.037(2)
C24 0.060(2) 0.051(2) 0.074(2) -0.0104(18) -0.019(2) -0.0184(18)
C25 0.0382(18) 0.0405(16) 0.058(2) -0.0173(15) -0.0169(16) -0.0107(14)
C26 0.0435(19) 0.0501(18) 0.055(2) -0.0235(16) -0.0155(17) -0.0058(16)
C27 0.064(2) 0.063(2) 0.067(2) -0.0197(18) -0.028(2) -0.0019(19)
C28 0.054(2) 0.067(2) 0.097(3) -0.034(2) -0.038(2) 0.0142(19)
C29 0.043(2) 0.077(2) 0.084(3) -0.036(2) -0.009(2) -0.0112(19)
C30 0.043(2) 0.0542(19) 0.060(2) -0.0172(17) -0.0096(18) -0.0177(17)
C31 0.052(2) 0.069(2) 0.056(2) -0.0237(18) -0.0161(18) -0.0008(18)
C32 0.084(3) 0.112(3) 0.078(3) -0.032(2) 0.004(2) -0.036(3)
C33 0.093(3) 0.152(4) 0.087(3) -0.073(3) -0.010(2) -0.025(3)
C34 0.058(2) 0.088(3) 0.067(2) -0.011(2) -0.003(2) -0.034(2)
C35 0.190(5) 0.132(4) 0.098(3) 0.004(3) 0.001(3) -0.106(4)
C36 0.077(3) 0.158(4) 0.076(3) -0.043(3) 0.006(2) -0.042(3)
C37 0.048(2) 0.0408(18) 0.075(2) -0.0167(16) -0.0226(17) -0.0159(16)
C38 0.053(2) 0.0303(17) 0.089(2) -0.0133(16) -0.0305(19) -0.0086(16)
C39 0.050(2) 0.0386(17) 0.0395(17) -0.0102(14) -0.0096(15) -0.0133(15)
C40 0.073(3) 0.049(2) 0.151(4) -0.030(3) -0.054(3) -0.017(2)
C41 0.0435(19) 0.0407(17) 0.0453(18) -0.0122(14) -0.0097(15) -0.0055(15)
C42 0.054(2) 0.0433(19) 0.107(3) -0.0202(19) -0.008(2) -0.0087(18)
C43 0.071(3) 0.044(2) 0.146(4) -0.032(2) -0.017(3) -0.002(2)
C44 0.054(2) 0.063(2) 0.110(3) -0.036(2) -0.021(2) 0.013(2)
C45 0.044(2) 0.070(2) 0.088(3) -0.025(2) -0.0115(19) -0.0056(19)
C46 0.049(2) 0.0504(19) 0.059(2) -0.0123(16) -0.0126(17) -0.0109(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100817.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-01 10:45:47 +0200 (Tue, 01 Nov 2016) $
#$Revision: 187722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100817.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100817
loop_
_publ_author_name
'Li, Xiao-Fang'
'Li, Yang-Guo'
'Li, Yue-Sheng'
'Chen, Yan-Xiang'
'Hu, Ning-Hai'
_publ_section_title
;
Copolymerization of Ethylene with Methyl Methacrylate with Neutral
Nickel(II) Complexes Bearing \b-Ketoiminato Chelate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2502
_journal_page_last 2510
_journal_paper_doi 10.1021/om049080w
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C46 H46 N Ni O P'
_chemical_formula_weight 718.52
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 114.18(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.782(3)
_cell_length_b 38.013(11)
_cell_length_c 10.424(3)
_cell_measurement_reflns_used 45
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 11.69
_cell_measurement_theta_min 4.98
_cell_volume 3897.5(19)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0277
_diffrn_reflns_av_sigmaI/netI 0.1180
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -46
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 9536
_diffrn_reflns_theta_max 25.98
_diffrn_reflns_theta_min 2.07
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.574
_exptl_absorpt_correction_T_max 0.7205
_exptl_absorpt_correction_T_min 0.5631
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.225
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1520
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.28
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.915
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 456
_refine_ls_number_reflns 7656
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.915
_refine_ls_R_factor_all 0.0998
_refine_ls_R_factor_gt 0.0438
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0723
_refine_ls_wR_factor_ref 0.0790
_reflns_number_gt 4019
_reflns_number_total 7656
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100817
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.57075(4) 0.871396(10) 0.38721(4) 0.03179(11) Uani 1 1 d . . .
P P 0.76716(8) 0.86565(2) 0.56788(9) 0.0355(2) Uani 1 1 d . . .
O O 0.52279(19) 0.82689(5) 0.4354(2) 0.0458(6) Uani 1 1 d . . .
N N 0.3859(2) 0.88322(6) 0.2610(3) 0.0317(6) Uani 1 1 d . . .
C1 C 0.6577(3) 0.90515(8) 0.3166(3) 0.0348(8) Uani 1 1 d . . .
C2 C 0.6593(3) 0.94169(9) 0.3264(4) 0.0459(9) Uani 1 1 d . . .
H2 H 0.6121 0.9526 0.3727 0.046 Uiso 1 1 calc R . .
C3 C 0.7302(4) 0.96236(10) 0.2683(4) 0.0617(12) Uani 1 1 d . . .
H3 H 0.7303 0.9867 0.2770 0.062 Uiso 1 1 calc R . .
C4 C 0.7997(4) 0.94693(12) 0.1985(5) 0.0744(14) Uani 1 1 d . . .
H4 H 0.8468 0.9608 0.1601 0.074 Uiso 1 1 calc R . .
C5 C 0.7998(3) 0.91059(12) 0.1850(4) 0.0667(12) Uani 1 1 d . . .
H5 H 0.8462 0.9000 0.1372 0.067 Uiso 1 1 calc R . .
C6 C 0.7300(3) 0.89031(9) 0.2437(3) 0.0476(9) Uani 1 1 d . . .
H6 H 0.7307 0.8660 0.2347 0.048 Uiso 1 1 calc R . .
C7 C 0.8851(3) 0.83909(9) 0.5239(4) 0.0414(9) Uani 1 1 d . . .
C8 C 0.8320(4) 0.80865(9) 0.4487(4) 0.0637(12) Uani 1 1 d . . .
H8 H 0.7418 0.8027 0.4265 0.064 Uiso 1 1 calc R . .
C9 C 0.9115(5) 0.78674(11) 0.4057(5) 0.0852(15) Uani 1 1 d . . .
H9 H 0.8740 0.7668 0.3524 0.085 Uiso 1 1 calc R . .
C10 C 1.0465(5) 0.79509(12) 0.4433(5) 0.0883(16) Uani 1 1 d . . .
H10 H 1.1020 0.7801 0.4194 0.088 Uiso 1 1 calc R . .
C11 C 1.0977(4) 0.82531(13) 0.5153(5) 0.0820(15) Uani 1 1 d . . .
H11 H 1.1875 0.8314 0.5366 0.082 Uiso 1 1 calc R . .
C12 C 1.0186(3) 0.84706(10) 0.5573(4) 0.0596(11) Uani 1 1 d . . .
H12 H 1.0563 0.8673 0.6088 0.060 Uiso 1 1 calc R . .
C13 C 0.8620(3) 0.90515(8) 0.6577(4) 0.0383(8) Uani 1 1 d . . .
C14 C 0.9214(3) 0.92720(8) 0.5930(4) 0.0478(9) Uani 1 1 d . . .
H14 H 0.9179 0.9214 0.5049 0.048 Uiso 1 1 calc R . .
C15 C 0.9859(3) 0.95781(9) 0.6591(5) 0.0577(11) Uani 1 1 d . . .
H15 H 1.0247 0.9726 0.6146 0.058 Uiso 1 1 calc R . .
C16 C 0.9930(4) 0.96658(10) 0.7895(5) 0.0674(13) Uani 1 1 d . . .
H16 H 1.0365 0.9871 0.8335 0.067 Uiso 1 1 calc R . .
C17 C 0.9352(3) 0.94467(10) 0.8547(4) 0.0601(11) Uani 1 1 d . . .
H17 H 0.9409 0.9502 0.9439 0.060 Uiso 1 1 calc R . .
C18 C 0.8685(3) 0.91437(9) 0.7884(4) 0.0493(10) Uani 1 1 d . . .
H18 H 0.8276 0.9001 0.8323 0.049 Uiso 1 1 calc R . .
C19 C 0.7553(3) 0.84206(8) 0.7157(3) 0.0431(9) Uani 1 1 d . . .
C20 C 0.6424(4) 0.84596(10) 0.7436(4) 0.0601(11) Uani 1 1 d . . .
H20 H 0.5691 0.8590 0.6821 0.060 Uiso 1 1 calc R . .
C21 C 0.6350(5) 0.83090(13) 0.8618(5) 0.0923(16) Uani 1 1 d . . .
H21 H 0.5583 0.8340 0.8803 0.092 Uiso 1 1 calc R . .
C22 C 0.7437(7) 0.81135(12) 0.9509(5) 0.102(2) Uani 1 1 d . . .
H22 H 0.7401 0.8010 1.0301 0.102 Uiso 1 1 calc R . .
C23 C 0.8556(5) 0.80708(12) 0.9247(5) 0.0853(15) Uani 1 1 d . . .
H23 H 0.9284 0.7939 0.9862 0.085 Uiso 1 1 calc R . .
C24 C 0.8629(4) 0.82218(10) 0.8069(4) 0.0609(11) Uani 1 1 d . . .
H24 H 0.9399 0.8190 0.7892 0.061 Uiso 1 1 calc R . .
C25 C 0.3560(3) 0.91921(8) 0.2158(3) 0.0321(8) Uani 1 1 d . . .
C26 C 0.3303(3) 0.94292(9) 0.3042(4) 0.0387(8) Uani 1 1 d . . .
C27 C 0.3060(3) 0.97804(9) 0.2639(4) 0.0485(10) Uani 1 1 d . . .
H27 H 0.2882 0.9941 0.3215 0.049 Uiso 1 1 calc R . .
C28 C 0.3084(3) 0.98911(9) 0.1388(4) 0.0539(10) Uani 1 1 d . . .
H28 H 0.2924 1.0126 0.1124 0.054 Uiso 1 1 calc R . .
C29 C 0.3343(3) 0.96553(9) 0.0533(4) 0.0475(9) Uani 1 1 d . . .
H29 H 0.3361 0.9734 -0.0304 0.048 Uiso 1 1 calc R . .
C30 C 0.3582(3) 0.92987(8) 0.0885(3) 0.0353(8) Uani 1 1 d . . .
C31 C 0.3344(3) 0.93227(10) 0.4469(4) 0.0509(10) Uani 1 1 d . . .
H31 H 0.3361 0.9065 0.4511 0.051 Uiso 1 1 calc R . .
C32 C 0.2116(4) 0.94454(12) 0.4713(4) 0.1003(17) Uani 1 1 d . . .
H32A H 0.2168 0.9695 0.4862 0.100 Uiso 1 1 calc R . .
H32B H 0.2105 0.9329 0.5526 0.100 Uiso 1 1 calc R . .
H32C H 0.1300 0.9389 0.3905 0.100 Uiso 1 1 calc R . .
C33 C 0.4648(4) 0.94554(12) 0.5642(4) 0.0859(15) Uani 1 1 d . . .
H33A H 0.5415 0.9379 0.5473 0.086 Uiso 1 1 calc R . .
H33B H 0.4716 0.9364 0.6527 0.086 Uiso 1 1 calc R . .
H33C H 0.4634 0.9708 0.5667 0.086 Uiso 1 1 calc R . .
C34 C 0.3879(3) 0.90436(9) -0.0070(3) 0.0457(9) Uani 1 1 d . . .
H34 H 0.4464 0.8858 0.0529 0.046 Uiso 1 1 calc R . .
C35 C 0.2607(4) 0.88672(10) -0.1104(4) 0.0788(14) Uani 1 1 d . . .
H35A H 0.2219 0.8724 -0.0603 0.079 Uiso 1 1 calc R . .
H35B H 0.2832 0.8722 -0.1732 0.079 Uiso 1 1 calc R . .
H35C H 0.1962 0.9043 -0.1634 0.079 Uiso 1 1 calc R . .
C36 C 0.4655(4) 0.92162(11) -0.0842(4) 0.0838(14) Uani 1 1 d . . .
H36A H 0.4115 0.9402 -0.1429 0.084 Uiso 1 1 calc R . .
H36B H 0.4841 0.9044 -0.1413 0.084 Uiso 1 1 calc R . .
H36C H 0.5495 0.9311 -0.0170 0.084 Uiso 1 1 calc R . .
C37 C 0.2807(3) 0.86208(8) 0.2350(3) 0.0396(9) Uani 1 1 d . . .
C38 C 0.2912(3) 0.82697(8) 0.2801(4) 0.0436(9) Uani 1 1 d . . .
H38 H 0.2132 0.8132 0.2419 0.044 Uiso 1 1 calc R . .
C39 C 0.4070(3) 0.81102(8) 0.3759(4) 0.0372(8) Uani 1 1 d . . .
C40 C 0.1366(3) 0.87537(9) 0.1591(4) 0.0622(11) Uani 1 1 d . . .
H40A H 0.1031 0.8831 0.2267 0.062 Uiso 1 1 calc R . .
H40B H 0.0799 0.8568 0.1032 0.062 Uiso 1 1 calc R . .
H40C H 0.1353 0.8947 0.0993 0.062 Uiso 1 1 calc R . .
C41 C 0.4042(3) 0.77390(8) 0.4226(4) 0.0402(9) Uani 1 1 d . . .
C42 C 0.3124(4) 0.74915(9) 0.3388(4) 0.0599(11) Uani 1 1 d . . .
H42 H 0.2517 0.7552 0.2483 0.060 Uiso 1 1 calc R . .
C43 C 0.3102(4) 0.71551(10) 0.3882(5) 0.0732(14) Uani 1 1 d . . .
H43 H 0.2466 0.6994 0.3311 0.073 Uiso 1 1 calc R . .
C44 C 0.3990(5) 0.70560(11) 0.5180(5) 0.0791(15) Uani 1 1 d . . .
H44 H 0.3969 0.6828 0.5497 0.079 Uiso 1 1 calc R . .
C45 C 0.4922(4) 0.72944(10) 0.6024(5) 0.0759(13) Uani 1 1 d . . .
H45 H 0.5533 0.7228 0.6919 0.076 Uiso 1 1 calc R . .
C46 C 0.4960(4) 0.76331(9) 0.5551(4) 0.0632(11) Uani 1 1 d . . .
H46 H 0.5606 0.7791 0.6127 0.063 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.02706(19) 0.0327(2) 0.0321(2) 0.0065(2) 0.00852(17) -0.0007(2)
P 0.0306(4) 0.0365(5) 0.0360(5) 0.0057(5) 0.0101(4) 0.0010(4)
O 0.0371(12) 0.0403(13) 0.0526(17) 0.0145(13) 0.0108(12) -0.0055(11)
N 0.0277(13) 0.0326(15) 0.0316(16) 0.0033(13) 0.0090(13) 0.0025(11)
C1 0.0275(16) 0.040(2) 0.032(2) 0.0110(17) 0.0076(16) -0.0012(15)
C2 0.0391(19) 0.043(2) 0.049(2) 0.0133(19) 0.0118(18) -0.0017(16)
C3 0.059(2) 0.051(2) 0.062(3) 0.017(2) 0.013(2) -0.013(2)
C4 0.066(3) 0.088(4) 0.075(3) 0.029(3) 0.035(3) -0.015(3)
C5 0.059(3) 0.088(3) 0.065(3) 0.019(3) 0.038(2) 0.004(2)
C6 0.044(2) 0.051(2) 0.046(2) 0.010(2) 0.0167(19) 0.0035(18)
C7 0.0384(19) 0.044(2) 0.037(2) 0.0057(19) 0.0107(18) 0.0044(17)
C8 0.052(2) 0.052(2) 0.089(3) -0.008(3) 0.030(2) 0.002(2)
C9 0.102(4) 0.051(3) 0.112(4) -0.014(3) 0.053(3) 0.009(3)
C10 0.087(4) 0.082(3) 0.121(5) 0.004(3) 0.068(4) 0.029(3)
C11 0.051(3) 0.100(4) 0.101(4) -0.004(3) 0.037(3) 0.010(3)
C12 0.044(2) 0.067(3) 0.063(3) -0.015(2) 0.017(2) 0.000(2)
C13 0.0259(17) 0.0387(19) 0.042(2) 0.0053(18) 0.0050(16) 0.0013(15)
C14 0.0335(17) 0.056(2) 0.043(2) 0.007(2) 0.0044(18) -0.0028(18)
C15 0.042(2) 0.042(2) 0.075(3) 0.012(2) 0.011(2) -0.0057(18)
C16 0.049(2) 0.040(2) 0.092(4) -0.018(3) 0.007(3) -0.0057(19)
C17 0.061(3) 0.051(3) 0.056(3) -0.015(2) 0.012(2) 0.007(2)
C18 0.051(2) 0.040(2) 0.054(3) 0.001(2) 0.018(2) 0.0032(18)
C19 0.058(2) 0.037(2) 0.031(2) 0.0022(18) 0.0151(19) -0.0032(18)
C20 0.069(3) 0.067(3) 0.054(3) 0.009(2) 0.034(2) 0.000(2)
C21 0.130(5) 0.098(4) 0.082(4) -0.005(3) 0.076(4) -0.029(3)
C22 0.195(6) 0.065(3) 0.055(4) 0.020(3) 0.059(4) -0.010(4)
C23 0.128(4) 0.064(3) 0.050(3) 0.014(3) 0.022(3) 0.012(3)
C24 0.076(3) 0.056(3) 0.043(3) 0.018(2) 0.017(2) 0.008(2)
C25 0.0239(15) 0.0339(19) 0.032(2) 0.0034(17) 0.0053(15) 0.0054(14)
C26 0.0333(18) 0.040(2) 0.039(2) 0.0019(18) 0.0114(17) 0.0030(15)
C27 0.052(2) 0.040(2) 0.051(3) -0.005(2) 0.018(2) 0.0113(17)
C28 0.062(2) 0.035(2) 0.053(3) 0.010(2) 0.012(2) 0.0135(18)
C29 0.054(2) 0.047(2) 0.033(2) 0.0118(19) 0.0093(19) 0.0071(19)
C30 0.0328(17) 0.0376(19) 0.0266(19) 0.0033(17) 0.0031(16) 0.0034(15)
C31 0.059(2) 0.055(2) 0.046(2) -0.004(2) 0.028(2) 0.0029(19)
C32 0.087(3) 0.151(5) 0.090(4) 0.003(4) 0.063(3) 0.013(3)
C33 0.087(3) 0.133(4) 0.036(3) 0.010(3) 0.024(2) -0.012(3)
C34 0.054(2) 0.049(2) 0.027(2) 0.0082(18) 0.0100(18) 0.0175(18)
C35 0.079(3) 0.077(3) 0.056(3) -0.032(3) 0.004(2) 0.022(2)
C36 0.116(4) 0.096(4) 0.057(3) 0.014(3) 0.053(3) 0.022(3)
C37 0.0316(17) 0.041(2) 0.042(2) 0.0005(18) 0.0107(16) -0.0029(15)
C38 0.0286(17) 0.039(2) 0.058(3) 0.000(2) 0.0122(18) -0.0066(15)
C39 0.0420(19) 0.0332(18) 0.044(2) -0.0024(18) 0.0260(18) -0.0059(16)
C40 0.0318(18) 0.062(2) 0.072(3) 0.012(2) 0.0003(19) -0.0019(18)
C41 0.0414(19) 0.034(2) 0.051(2) 0.0040(19) 0.0255(19) -0.0026(16)
C42 0.068(3) 0.041(2) 0.074(3) -0.003(2) 0.032(2) -0.0081(19)
C43 0.090(3) 0.035(2) 0.105(4) -0.011(3) 0.051(3) -0.019(2)
C44 0.125(4) 0.038(2) 0.103(4) 0.011(3) 0.076(4) -0.001(3)
C45 0.117(4) 0.049(3) 0.067(3) 0.018(3) 0.042(3) 0.006(3)
C46 0.082(3) 0.046(2) 0.066(3) 0.001(2) 0.035(3) -0.011(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100818.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-01 10:45:47 +0200 (Tue, 01 Nov 2016) $
#$Revision: 187722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100818.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100818
loop_
_publ_author_name
'Li, Xiao-Fang'
'Li, Yang-Guo'
'Li, Yue-Sheng'
'Chen, Yan-Xiang'
'Hu, Ning-Hai'
_publ_section_title
;
Copolymerization of Ethylene with Methyl Methacrylate with Neutral
Nickel(II) Complexes Bearing \b-Ketoiminato Chelate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2502
_journal_page_last 2510
_journal_paper_doi 10.1021/om049080w
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C41 H41 F3 N Ni O P'
_chemical_formula_weight 710.43
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 96.70(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.299(3)
_cell_length_b 21.609(6)
_cell_length_c 18.370(13)
_cell_measurement_reflns_used 34
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.30
_cell_measurement_theta_min 5.21
_cell_volume 3666(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0377
_diffrn_reflns_av_sigmaI/netI 0.0867
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 8303
_diffrn_reflns_theta_max 24.99
_diffrn_reflns_theta_min 1.46
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.620
_exptl_absorpt_correction_T_max 0.5419
_exptl_absorpt_correction_T_min 0.4412
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.287
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description tabular
_exptl_crystal_F_000 1488
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.51
_exptl_crystal_size_min 0.23
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 438
_refine_ls_number_reflns 6407
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.020
_refine_ls_R_factor_all 0.1164
_refine_ls_R_factor_gt 0.0677
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1763
_refine_ls_wR_factor_ref 0.1924
_reflns_number_gt 3724
_reflns_number_total 6407
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.33418(6) 0.45323(3) 0.26059(4) 0.0408(2) Uani 1 1 d . . .
P P 0.17835(13) 0.52612(6) 0.22702(8) 0.0410(3) Uani 1 1 d . . .
O O 0.4340(4) 0.51268(16) 0.3237(2) 0.0535(10) Uani 1 1 d . . .
N N 0.4353(4) 0.38306(18) 0.3099(2) 0.0409(10) Uani 1 1 d . . .
C1 C 0.2648(6) 0.4123(2) 0.1710(3) 0.0480(13) Uani 1 1 d . . .
C2 C 0.3271(6) 0.4333(3) 0.1114(3) 0.0573(15) Uani 1 1 d . . .
H2 H 0.3947 0.4651 0.1176 0.057 Uiso 1 1 calc R . .
C3 C 0.2919(8) 0.4082(3) 0.0423(4) 0.079(2) Uani 1 1 d . . .
H3 H 0.3352 0.4232 0.0027 0.079 Uiso 1 1 calc R . .
C4 C 0.1922(10) 0.3611(3) 0.0327(4) 0.093(3) Uani 1 1 d . . .
H4 H 0.1695 0.3434 -0.0133 0.093 Uiso 1 1 calc R . .
C5 C 0.1266(9) 0.3402(3) 0.0908(5) 0.089(2) Uani 1 1 d . . .
H5 H 0.0575 0.3090 0.0837 0.089 Uiso 1 1 calc R . .
C6 C 0.1615(7) 0.3648(3) 0.1595(4) 0.0653(17) Uani 1 1 d . . .
H6 H 0.1166 0.3499 0.1987 0.065 Uiso 1 1 calc R . .
C7 C 0.2418(6) 0.5831(2) 0.1634(3) 0.0505(14) Uani 1 1 d . . .
C8 C 0.3889(7) 0.5929(3) 0.1683(4) 0.0676(17) Uani 1 1 d . . .
H8 H 0.4509 0.5718 0.2031 0.068 Uiso 1 1 calc R . .
C9 C 0.4449(9) 0.6347(4) 0.1208(5) 0.093(3) Uani 1 1 d . . .
H9 H 0.5443 0.6410 0.1235 0.093 Uiso 1 1 calc R . .
C10 C 0.3543(12) 0.6657(3) 0.0712(4) 0.099(3) Uani 1 1 d . . .
H10 H 0.3920 0.6932 0.0394 0.099 Uiso 1 1 calc R . .
C11 C 0.2081(11) 0.6575(3) 0.0668(4) 0.096(3) Uani 1 1 d . . .
H11 H 0.1464 0.6796 0.0327 0.096 Uiso 1 1 calc R . .
C12 C 0.1530(7) 0.6164(3) 0.1134(4) 0.0687(18) Uani 1 1 d . . .
H12 H 0.0532 0.6111 0.1109 0.069 Uiso 1 1 calc R . .
C13 C 0.1419(5) 0.5718(3) 0.3067(3) 0.0475(13) Uani 1 1 d . . .
C14 C 0.1385(7) 0.5439(3) 0.3738(3) 0.0677(17) Uani 1 1 d . . .
H14 H 0.1582 0.5018 0.3781 0.068 Uiso 1 1 calc R . .
C15 C 0.1075(7) 0.5755(4) 0.4345(4) 0.086(2) Uani 1 1 d . . .
H15 H 0.1021 0.5552 0.4787 0.086 Uiso 1 1 calc R . .
C16 C 0.0847(8) 0.6380(5) 0.4284(5) 0.099(3) Uani 1 1 d . . .
H16 H 0.0650 0.6605 0.4693 0.099 Uiso 1 1 calc R . .
C17 C 0.0902(9) 0.6667(4) 0.3652(5) 0.101(3) Uani 1 1 d . . .
H17 H 0.0769 0.7093 0.3626 0.101 Uiso 1 1 calc R . .
C18 C 0.1157(7) 0.6340(3) 0.3020(4) 0.0723(18) Uani 1 1 d . . .
H18 H 0.1148 0.6544 0.2573 0.072 Uiso 1 1 calc R . .
C19 C -0.0034(5) 0.5044(2) 0.1847(3) 0.0468(13) Uani 1 1 d . . .
C20 C -0.1188(6) 0.5003(3) 0.2263(3) 0.0633(16) Uani 1 1 d . . .
H20 H -0.1063 0.5118 0.2755 0.063 Uiso 1 1 calc R . .
C21 C -0.2517(7) 0.4794(4) 0.1949(5) 0.084(2) Uani 1 1 d . . .
H21 H -0.3285 0.4770 0.2230 0.084 Uiso 1 1 calc R . .
C22 C -0.2718(7) 0.4622(3) 0.1230(5) 0.081(2) Uani 1 1 d . . .
H22 H -0.3617 0.4477 0.1026 0.081 Uiso 1 1 calc R . .
C23 C -0.1599(6) 0.4660(3) 0.0807(3) 0.0602(16) Uani 1 1 d . . .
H23 H -0.1741 0.4549 0.0314 0.060 Uiso 1 1 calc R . .
C24 C -0.0258(6) 0.4864(3) 0.1120(3) 0.0546(15) Uani 1 1 d . . .
H24 H 0.0507 0.4880 0.0837 0.055 Uiso 1 1 calc R . .
C25 C 0.3780(6) 0.3209(2) 0.2926(3) 0.0510(14) Uani 1 1 d . . .
C26 C 0.4368(6) 0.2857(3) 0.2379(4) 0.0603(16) Uani 1 1 d . . .
C27 C 0.3755(7) 0.2290(3) 0.2222(4) 0.0734(19) Uani 1 1 d . . .
H27 H 0.4120 0.2044 0.1871 0.073 Uiso 1 1 calc R . .
C28 C 0.2611(8) 0.2067(3) 0.2566(4) 0.079(2) Uani 1 1 d . . .
H28 H 0.2211 0.1681 0.2442 0.079 Uiso 1 1 calc R . .
C29 C 0.2073(7) 0.2425(3) 0.3093(4) 0.0715(19) Uani 1 1 d . . .
H29 H 0.1304 0.2274 0.3322 0.072 Uiso 1 1 calc R . .
C30 C 0.2640(6) 0.3003(2) 0.3294(3) 0.0524(14) Uani 1 1 d . . .
C31 C 0.5601(7) 0.3105(3) 0.1989(4) 0.0670(17) Uani 1 1 d . . .
H31 H 0.5514 0.3557 0.1972 0.067 Uiso 1 1 calc R . .
C32 C 0.7059(7) 0.2950(5) 0.2397(4) 0.114(3) Uani 1 1 d . . .
H32A H 0.7144 0.3138 0.2874 0.114 Uiso 1 1 calc R . .
H32B H 0.7811 0.3105 0.2129 0.114 Uiso 1 1 calc R . .
H32C H 0.7152 0.2509 0.2448 0.114 Uiso 1 1 calc R . .
C33 C 0.5532(8) 0.2873(4) 0.1195(4) 0.093(2) Uani 1 1 d . . .
H33A H 0.5775 0.2441 0.1196 0.093 Uiso 1 1 calc R . .
H33B H 0.6208 0.3101 0.0943 0.093 Uiso 1 1 calc R . .
H33C H 0.4571 0.2931 0.0951 0.093 Uiso 1 1 calc R . .
C34 C 0.2023(7) 0.3371(3) 0.3866(4) 0.0634(17) Uani 1 1 d . . .
H34 H 0.2642 0.3736 0.3961 0.063 Uiso 1 1 calc R . .
C35 C 0.0517(8) 0.3602(4) 0.3637(5) 0.097(3) Uani 1 1 d . . .
H35A H 0.0485 0.3804 0.3170 0.097 Uiso 1 1 calc R . .
H35B H 0.0248 0.3891 0.3995 0.097 Uiso 1 1 calc R . .
H35C H -0.0145 0.3260 0.3599 0.097 Uiso 1 1 calc R . .
C36 C 0.2061(9) 0.3020(4) 0.4590(4) 0.102(3) Uani 1 1 d . . .
H36A H 0.1504 0.2647 0.4514 0.102 Uiso 1 1 calc R . .
H36B H 0.1658 0.3275 0.4943 0.102 Uiso 1 1 calc R . .
H36C H 0.3044 0.2918 0.4767 0.102 Uiso 1 1 calc R . .
C37 C 0.5337(6) 0.3869(3) 0.3656(4) 0.0556(15) Uani 1 1 d . . .
C38 C 0.5926(6) 0.4444(2) 0.3936(3) 0.0572(15) Uani 1 1 d . . .
H38 H 0.6720 0.4432 0.4295 0.057 Uiso 1 1 calc R . .
C39 C 0.5406(6) 0.5004(2) 0.3715(3) 0.0476(13) Uani 1 1 d . . .
C40 C 0.5918(7) 0.3313(2) 0.4103(4) 0.0722(19) Uani 1 1 d . . .
H40A H 0.5530 0.3312 0.4565 0.072 Uiso 1 1 calc R . .
H40B H 0.6956 0.3335 0.4187 0.072 Uiso 1 1 calc R . .
H40C H 0.5636 0.2940 0.3841 0.072 Uiso 1 1 calc R . .
C41 C 0.6130(7) 0.5582(3) 0.4071(4) 0.0638(17) Uani 1 1 d . . .
F1 F 0.5180(5) 0.5991(2) 0.4256(3) 0.1241(19) Uani 1 1 d . . .
F2 F 0.7022(6) 0.54837(18) 0.4664(3) 0.126(2) Uani 1 1 d . . .
F3 F 0.6850(6) 0.5879(2) 0.3610(3) 0.1164(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0352(3) 0.0333(3) 0.0540(4) -0.0013(3) 0.0059(3) 0.0026(3)
P 0.0367(7) 0.0369(7) 0.0504(9) 0.0021(6) 0.0092(6) 0.0050(6)
O 0.048(2) 0.038(2) 0.071(3) -0.0106(18) -0.006(2) -0.0019(17)
N 0.035(2) 0.033(2) 0.053(3) 0.0011(19) -0.001(2) 0.0026(18)
C1 0.048(3) 0.037(3) 0.058(4) -0.004(3) -0.002(3) 0.008(2)
C2 0.052(3) 0.056(3) 0.065(4) -0.009(3) 0.013(3) 0.011(3)
C3 0.098(5) 0.076(5) 0.061(4) -0.002(4) 0.004(4) 0.029(4)
C4 0.139(7) 0.064(5) 0.066(5) -0.013(4) -0.034(5) 0.023(5)
C5 0.119(6) 0.046(4) 0.087(6) -0.009(4) -0.043(5) -0.009(4)
C6 0.070(4) 0.049(3) 0.071(4) 0.004(3) -0.019(3) -0.004(3)
C7 0.056(3) 0.036(3) 0.061(4) -0.002(3) 0.015(3) -0.007(3)
C8 0.066(4) 0.068(4) 0.070(4) 0.000(3) 0.013(3) -0.016(3)
C9 0.094(5) 0.106(6) 0.084(6) -0.015(5) 0.030(5) -0.059(5)
C10 0.166(9) 0.072(5) 0.060(5) -0.001(4) 0.023(6) -0.055(6)
C11 0.147(8) 0.059(4) 0.079(6) 0.011(4) 0.000(5) -0.022(5)
C12 0.072(4) 0.052(4) 0.077(5) 0.017(3) -0.011(3) -0.010(3)
C13 0.037(3) 0.052(3) 0.054(4) -0.011(3) 0.009(2) 0.007(2)
C14 0.069(4) 0.074(4) 0.063(4) 0.007(4) 0.019(3) 0.010(4)
C15 0.072(5) 0.125(7) 0.065(5) -0.006(5) 0.020(4) 0.010(5)
C16 0.074(5) 0.146(9) 0.083(6) -0.050(6) 0.029(4) 0.002(5)
C17 0.109(6) 0.077(5) 0.123(8) -0.039(5) 0.036(6) 0.016(5)
C18 0.082(4) 0.063(4) 0.076(5) -0.009(4) 0.024(4) 0.010(4)
C19 0.035(3) 0.040(3) 0.067(4) 0.001(3) 0.012(3) 0.008(2)
C20 0.052(3) 0.086(4) 0.054(4) 0.002(3) 0.012(3) 0.003(3)
C21 0.042(3) 0.117(6) 0.096(6) 0.002(5) 0.024(4) -0.005(4)
C22 0.040(3) 0.095(5) 0.106(6) 0.000(5) 0.010(4) -0.006(4)
C23 0.048(3) 0.073(4) 0.057(4) -0.005(3) -0.007(3) 0.001(3)
C24 0.038(3) 0.061(4) 0.065(4) 0.001(3) 0.009(3) 0.003(3)
C25 0.046(3) 0.030(3) 0.076(4) -0.001(3) 0.002(3) 0.001(2)
C26 0.056(3) 0.040(3) 0.086(5) 0.000(3) 0.012(3) 0.012(3)
C27 0.082(5) 0.049(4) 0.089(5) -0.018(4) 0.010(4) 0.009(4)
C28 0.082(5) 0.038(3) 0.116(6) -0.011(4) 0.003(4) -0.009(3)
C29 0.069(4) 0.044(3) 0.102(5) 0.010(4) 0.015(4) -0.009(3)
C30 0.052(3) 0.037(3) 0.067(4) 0.006(3) 0.004(3) -0.005(3)
C31 0.066(4) 0.061(4) 0.078(5) -0.007(3) 0.024(3) 0.012(3)
C32 0.067(5) 0.178(10) 0.096(7) 0.002(6) 0.013(5) 0.015(6)
C33 0.104(6) 0.107(6) 0.071(5) 0.003(4) 0.024(4) 0.030(5)
C34 0.066(4) 0.052(4) 0.076(5) 0.003(3) 0.025(3) -0.013(3)
C35 0.091(5) 0.091(6) 0.112(7) 0.002(5) 0.027(5) 0.028(5)
C36 0.107(6) 0.096(6) 0.108(7) 0.020(5) 0.039(5) 0.009(5)
C37 0.051(3) 0.042(3) 0.074(4) 0.006(3) 0.009(3) 0.009(3)
C38 0.056(3) 0.050(4) 0.061(4) -0.002(3) -0.015(3) -0.003(3)
C39 0.051(3) 0.035(3) 0.058(4) -0.003(3) 0.009(3) -0.008(2)
C40 0.077(4) 0.042(3) 0.093(5) 0.003(3) -0.013(4) 0.006(3)
C41 0.068(4) 0.040(3) 0.080(5) -0.001(3) -0.008(4) -0.008(3)
F1 0.117(4) 0.080(3) 0.172(5) -0.069(3) 0.003(3) 0.003(3)
F2 0.165(5) 0.062(3) 0.126(4) 0.007(3) -0.085(4) -0.022(3)
F3 0.142(4) 0.079(3) 0.130(4) -0.002(3) 0.023(3) -0.058(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100819.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-16 04:05:44 +0300 (Mon, 16 Jul 2018) $
#$Revision: 209049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100819.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100819
loop_
_publ_author_name
'Prabusankar, Ganesan'
'Murugavel, Ramaswamy'
'Butcher, Ray J.'
_publ_section_title
;
Synthesis, Spectral Studies, and Structural Characterization of a New
Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic
Aluminosilicate
;
_journal_coden_ASTM JOCEAH
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2124
_journal_page_last 2128
_journal_paper_doi 10.1021/om049254+
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C111 H208 N8 O24 Si16'
_chemical_formula_sum 'C111 H208 N8 O24 Si16'
_chemical_formula_weight 2488.29
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 102.68(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.342(3)
_cell_length_b 30.139(6)
_cell_length_c 29.457(6)
_cell_measurement_temperature 293(2)
_cell_volume 14155(5)
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1051
_diffrn_reflns_av_sigmaI/netI 0.0769
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 35
_diffrn_reflns_limit_k_min -35
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 138951
_diffrn_reflns_theta_max 24.94
_diffrn_reflns_theta_min 1.35
_exptl_absorpt_coefficient_mu 0.206
_exptl_absorpt_correction_T_max 0.9797
_exptl_absorpt_correction_T_min 0.9407
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.168
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 5384
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.000
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1528
_refine_ls_number_reflns 24498
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.000
_refine_ls_R_factor_all 0.1082
_refine_ls_R_factor_gt 0.0634
_refine_ls_shift/su_max 0.756
_refine_ls_shift/su_mean 0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1525
_refine_ls_wR_factor_ref 0.1709
_reflns_number_gt 15478
_reflns_number_total 24498
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060451
_cod_depositor_comments
;
Merging entries 1100819-1100822 with entries 4060451-4060454.
Marking entries 1100819-1100822 as duplicates of entries 4060451-4060454.
Antanas Vaitkus,
2018-07-16
;
_cod_database_code 1100819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.19388(8) 0.55328(4) 0.37594(4) 0.0307(3) Uani 1 1 d . . .
Si2 Si 0.25695(9) 0.56784(4) 0.48105(4) 0.0401(3) Uani 1 1 d . . .
Si3 Si 0.04866(6) 0.56411(3) 0.20683(3) 0.0225(2) Uani 1 1 d . . .
Si4 Si -0.09007(7) 0.50010(4) 0.16085(4) 0.0328(3) Uani 1 1 d . . .
Si5 Si 0.25160(6) 0.56790(3) 0.10370(3) 0.0222(2) Uani 1 1 d . . .
Si6 Si 0.24922(7) 0.59121(4) 0.00300(3) 0.0276(2) Uani 1 1 d . . .
Si7 Si 0.37047(6) 0.55524(3) 0.27815(3) 0.0211(2) Uani 1 1 d . . .
Si8 Si 0.52013(7) 0.50224(4) 0.33451(4) 0.0340(3) Uani 1 1 d . . .
Si9 Si 0.39005(6) 0.69802(3) 0.17720(3) 0.0215(2) Uani 1 1 d . . .
Si10 Si 0.45440(8) 0.76213(4) 0.11332(4) 0.0343(3) Uani 1 1 d . . .
Si11 Si 0.49403(7) 0.70014(4) 0.34687(4) 0.0304(3) Uani 1 1 d . . .
Si12 Si 0.55960(8) 0.68208(4) 0.45104(4) 0.0367(3) Uani 1 1 d . . .
Si13 Si 0.20877(7) 0.70499(3) 0.30194(3) 0.0231(2) Uani 1 1 d . . .
Si14 Si 0.19708(9) 0.77777(5) 0.37422(5) 0.0522(4) Uani 1 1 d . . .
Si15 Si 0.07084(7) 0.70826(4) 0.13510(4) 0.0279(3) Uani 1 1 d . . .
Si16 Si 0.02572(8) 0.77068(5) 0.05226(5) 0.0451(3) Uani 1 1 d . . .
N1 N 0.2002(2) 0.53896(11) 0.43255(11) 0.0306(8) Uani 1 1 d . . .
N2 N -0.00815(19) 0.51664(10) 0.20750(10) 0.0256(7) Uani 1 1 d . . .
N3 N 0.28687(19) 0.56004(10) 0.05383(10) 0.0240(7) Uani 1 1 d . . .
N4 N 0.43939(19) 0.51181(10) 0.28518(10) 0.0247(7) Uani 1 1 d . . .
N5 N 0.4386(2) 0.74662(11) 0.16828(10) 0.0255(7) Uani 1 1 d . . .
N6 N 0.5613(2) 0.70996(11) 0.39897(11) 0.0293(8) Uani 1 1 d . . .
N7 N 0.15654(19) 0.74608(10) 0.32390(10) 0.0245(7) Uani 1 1 d . . .
N8 N -0.00170(19) 0.73114(11) 0.09030(11) 0.0284(7) Uani 1 1 d . . .
O1 O 0.1030(2) 0.57446(11) 0.35316(11) 0.0396(8) Uani 1 1 d . . .
O2 O 0.2674(2) 0.58900(10) 0.37398(10) 0.0338(7) Uani 1 1 d . . .
O3 O 0.2141(2) 0.51143(10) 0.34395(10) 0.0343(7) Uani 1 1 d . . .
O4 O 0.06464(18) 0.58799(10) 0.25792(9) 0.0273(6) Uani 1 1 d . . .
O5 O 0.1378(2) 0.55644(10) 0.19247(11) 0.0291(7) Uani 1 1 d . . .
O6 O -0.00189(19) 0.59635(10) 0.16587(10) 0.0281(6) Uani 1 1 d . . .
O7 O 0.2362(2) 0.62050(10) 0.10811(10) 0.0274(7) Uani 1 1 d . . .
O8 O 0.3257(2) 0.55464(12) 0.14912(10) 0.0315(7) Uani 1 1 d . . .
O9 O 0.16760(18) 0.54002(10) 0.10403(11) 0.0320(7) Uani 1 1 d . . .
O10 O 0.27281(17) 0.53923(9) 0.26616(10) 0.0247(6) Uani 1 1 d . . .
O11 O 0.39147(16) 0.58340(8) 0.32657(8) 0.0261(6) Uani 1 1 d . . .
O12 O 0.3800(2) 0.58903(10) 0.23665(11) 0.0268(7) Uani 1 1 d . . .
O13 O 0.3774(2) 0.67062(10) 0.12929(10) 0.0296(7) Uani 1 1 d . . .
O14 O 0.29772(16) 0.70491(9) 0.18876(10) 0.0248(6) Uani 1 1 d . . .
O15 O 0.44846(19) 0.67150(12) 0.22116(10) 0.0277(7) Uani 1 1 d . . .
O16 O 0.43672(19) 0.74318(11) 0.32570(10) 0.0310(7) Uani 1 1 d . . .
O17 O 0.42429(19) 0.66541(10) 0.35620(10) 0.0365(7) Uani 1 1 d . . .
O18 O 0.54451(19) 0.68160(11) 0.30943(10) 0.0417(8) Uani 1 1 d . . .
O19 O 0.2570(2) 0.67337(9) 0.34444(9) 0.0312(6) Uani 1 1 d . . .
O20 O 0.2777(2) 0.72412(12) 0.27488(11) 0.0300(8) Uani 1 1 d . . .
O21 O 0.1443(2) 0.67405(10) 0.26519(10) 0.0283(7) Uani 1 1 d . . .
O22 O 0.0906(2) 0.65597(11) 0.12983(11) 0.0297(7) Uani 1 1 d . . .
O23 O 0.1539(2) 0.73670(11) 0.13660(13) 0.0462(10) Uani 1 1 d . . .
O24 O 0.03956(19) 0.71027(11) 0.18505(10) 0.0363(7) Uani 1 1 d . . .
C1 C 0.1513(3) 0.50040(16) 0.43969(14) 0.0438(12) Uani 1 1 d . . .
C2 C 0.1916(5) 0.45826(17) 0.44451(17) 0.0665(19) Uani 1 1 d . . .
C3 C 0.1438(8) 0.4219(2) 0.4511(2) 0.116(4) Uani 1 1 d . . .
H3 H 0.1687 0.3940 0.4550 0.140 Uiso 1 1 calc R . .
C4 C 0.0626(9) 0.4257(3) 0.4521(3) 0.127(5) Uani 1 1 d . . .
H4 H 0.0320 0.4003 0.4553 0.152 Uiso 1 1 calc R . .
C5 C 0.0229(6) 0.4666(4) 0.4484(2) 0.107(4) Uani 1 1 d . . .
H5 H -0.0332 0.4683 0.4499 0.129 Uiso 1 1 calc R . .
C6 C 0.0674(4) 0.5061(2) 0.44229(16) 0.0636(18) Uani 1 1 d . . .
C7 C 0.2852(5) 0.45356(19) 0.4452(2) 0.080(2) Uani 1 1 d . . .
H7A H 0.3028 0.4791 0.4298 0.096 Uiso 1 1 calc R . .
H7B H 0.3162 0.4540 0.4773 0.096 Uiso 1 1 calc R . .
C8 C 0.3085(7) 0.4120(3) 0.4223(3) 0.123(4) Uani 1 1 d . . .
H8A H 0.3679 0.4117 0.4242 0.184 Uiso 1 1 calc R . .
H8B H 0.2795 0.4116 0.3902 0.184 Uiso 1 1 calc R . .
H8C H 0.2931 0.3864 0.4379 0.184 Uiso 1 1 calc R . .
C9 C 0.0273(4) 0.5508(3) 0.44055(19) 0.077(2) Uani 1 1 d . . .
H9A H 0.0467 0.5685 0.4175 0.093 Uiso 1 1 calc R . .
H9B H 0.0472 0.5651 0.4705 0.093 Uiso 1 1 calc R . .
C10 C -0.0690(4) 0.5520(4) 0.4292(2) 0.140(5) Uani 1 1 d . . .
H10A H -0.0877 0.5822 0.4292 0.210 Uiso 1 1 calc R . .
H10B H -0.0895 0.5353 0.4522 0.210 Uiso 1 1 calc R . .
H10C H -0.0900 0.5392 0.3990 0.210 Uiso 1 1 calc R . .
C11 C 0.2231(4) 0.62662(19) 0.4785(2) 0.0703(17) Uani 1 1 d . . .
H11A H 0.1639 0.6280 0.4771 0.105 Uiso 1 1 calc R . .
H11B H 0.2350 0.6404 0.4513 0.105 Uiso 1 1 calc R . .
H11C H 0.2528 0.6419 0.5057 0.105 Uiso 1 1 calc R . .
C12 C 0.2351(4) 0.5416(2) 0.53425(16) 0.0669(17) Uani 1 1 d . . .
H12A H 0.1758 0.5423 0.5329 0.100 Uiso 1 1 calc R . .
H12B H 0.2641 0.5575 0.5612 0.100 Uiso 1 1 calc R . .
H12C H 0.2540 0.5113 0.5361 0.100 Uiso 1 1 calc R . .
C13 C 0.3713(4) 0.5665(2) 0.48379(19) 0.0655(16) Uani 1 1 d . . .
H13A H 0.3827 0.5803 0.4564 0.098 Uiso 1 1 calc R . .
H13B H 0.3902 0.5363 0.4855 0.098 Uiso 1 1 calc R . .
H13C H 0.4002 0.5823 0.5109 0.098 Uiso 1 1 calc R . .
C14 C 0.0217(2) 0.48524(12) 0.24515(13) 0.0256(8) Uani 1 1 d . . .
C15 C -0.0105(3) 0.48873(13) 0.28580(14) 0.0300(9) Uani 1 1 d . . .
C16 C 0.0204(3) 0.45964(14) 0.32246(14) 0.0342(10) Uani 1 1 d . . .
H16 H 0.0006 0.4618 0.3497 0.041 Uiso 1 1 calc R . .
C17 C 0.0793(3) 0.42791(15) 0.31934(16) 0.0393(11) Uani 1 1 d . . .
H17 H 0.0992 0.4091 0.3443 0.047 Uiso 1 1 calc R . .
C18 C 0.1085(3) 0.42401(14) 0.27923(16) 0.0371(10) Uani 1 1 d . . .
H18 H 0.1473 0.4020 0.2771 0.044 Uiso 1 1 calc R . .
C19 C 0.0809(2) 0.45270(13) 0.24148(14) 0.0301(9) Uani 1 1 d . . .
C20 C -0.0777(3) 0.52120(15) 0.29101(15) 0.0367(10) Uani 1 1 d . . .
H20A H -0.0895 0.5405 0.2640 0.044 Uiso 1 1 calc R . .
H20B H -0.0571 0.5395 0.3182 0.044 Uiso 1 1 calc R . .
C21 C -0.1589(3) 0.49872(19) 0.2960(2) 0.0588(14) Uani 1 1 d . . .
H21A H -0.1994 0.5209 0.2992 0.088 Uiso 1 1 calc R . .
H21B H -0.1480 0.4800 0.3230 0.088 Uiso 1 1 calc R . .
H21C H -0.1804 0.4811 0.2689 0.088 Uiso 1 1 calc R . .
C22 C 0.1154(3) 0.44661(15) 0.19824(16) 0.0376(10) Uani 1 1 d . . .
H22A H 0.1738 0.4556 0.2052 0.045 Uiso 1 1 calc R . .
H22B H 0.0854 0.4663 0.1742 0.045 Uiso 1 1 calc R . .
C23 C 0.1094(4) 0.39940(17) 0.1790(2) 0.0573(14) Uani 1 1 d . . .
H23A H 0.1325 0.3985 0.1517 0.086 Uiso 1 1 calc R . .
H23B H 0.0516 0.3904 0.1710 0.086 Uiso 1 1 calc R . .
H23C H 0.1402 0.3796 0.2021 0.086 Uiso 1 1 calc R . .
C24 C -0.1228(3) 0.44331(17) 0.17400(19) 0.0588(15) Uani 1 1 d . . .
H24A H -0.0757 0.4236 0.1775 0.088 Uiso 1 1 calc R . .
H24B H -0.1668 0.4332 0.1490 0.088 Uiso 1 1 calc R . .
H24C H -0.1427 0.4438 0.2023 0.088 Uiso 1 1 calc R . .
C25 C -0.1820(3) 0.53704(17) 0.15410(17) 0.0463(12) Uani 1 1 d . . .
H25A H -0.2015 0.5375 0.1825 0.069 Uiso 1 1 calc R . .
H25B H -0.2258 0.5263 0.1293 0.069 Uiso 1 1 calc R . .
H25C H -0.1664 0.5665 0.1470 0.069 Uiso 1 1 calc R . .
C26 C -0.0547(3) 0.5002(2) 0.10505(16) 0.0563(14) Uani 1 1 d . . .
H26A H -0.0067 0.4812 0.1077 0.084 Uiso 1 1 calc R . .
H26B H -0.0398 0.5299 0.0981 0.084 Uiso 1 1 calc R . .
H26C H -0.0991 0.4896 0.0805 0.084 Uiso 1 1 calc R . .
C27 C 0.3435(3) 0.52349(13) 0.05150(12) 0.0278(9) Uani 1 1 d . . .
C28 C 0.4307(3) 0.53186(15) 0.06040(13) 0.0316(9) Uani 1 1 d . . .
C29 C 0.4837(3) 0.49657(16) 0.05587(14) 0.0397(11) Uani 1 1 d . . .
H29 H 0.5412 0.5015 0.0612 0.048 Uiso 1 1 calc R . .
C30 C 0.4532(3) 0.45486(16) 0.04375(15) 0.0422(11) Uani 1 1 d . . .
H30 H 0.4901 0.4319 0.0414 0.051 Uiso 1 1 calc R . .
C31 C 0.3679(3) 0.44680(15) 0.03505(14) 0.0389(11) Uani 1 1 d . . .
H31 H 0.3477 0.4185 0.0266 0.047 Uiso 1 1 calc R . .
C32 C 0.3112(3) 0.48105(13) 0.03892(13) 0.0307(9) Uani 1 1 d . . .
C33 C 0.4640(3) 0.57789(16) 0.07209(15) 0.0381(10) Uani 1 1 d . . .
H33A H 0.4411 0.5888 0.0977 0.046 Uiso 1 1 calc R . .
H33B H 0.4427 0.5968 0.0455 0.046 Uiso 1 1 calc R . .
C34 C 0.5595(3) 0.58331(19) 0.08542(17) 0.0505(13) Uani 1 1 d . . .
H34A H 0.5732 0.6139 0.0921 0.076 Uiso 1 1 calc R . .
H34B H 0.5834 0.5737 0.0601 0.076 Uiso 1 1 calc R . .
H34C H 0.5818 0.5657 0.1125 0.076 Uiso 1 1 calc R . .
C35 C 0.2189(3) 0.47009(14) 0.02876(15) 0.0388(11) Uani 1 1 d . . .
H35A H 0.2036 0.4559 -0.0015 0.047 Uiso 1 1 calc R . .
H35B H 0.1872 0.4975 0.0271 0.047 Uiso 1 1 calc R . .
C36 C 0.1940(3) 0.43999(16) 0.0647(2) 0.0537(13) Uani 1 1 d . . .
H36A H 0.1348 0.4343 0.0562 0.081 Uiso 1 1 calc R . .
H36B H 0.2074 0.4542 0.0946 0.081 Uiso 1 1 calc R . .
H36C H 0.2241 0.4125 0.0661 0.081 Uiso 1 1 calc R . .
C37 C 0.1326(3) 0.59229(16) -0.00929(15) 0.0394(11) Uani 1 1 d . . .
H37A H 0.1115 0.5625 -0.0121 0.059 Uiso 1 1 calc R . .
H37B H 0.1115 0.6079 -0.0379 0.059 Uiso 1 1 calc R . .
H37C H 0.1145 0.6070 0.0157 0.059 Uiso 1 1 calc R . .
C38 C 0.2868(3) 0.56363(16) -0.04515(13) 0.0395(11) Uani 1 1 d . . .
H38A H 0.2676 0.5334 -0.0480 0.059 Uiso 1 1 calc R . .
H38B H 0.3470 0.5641 -0.0386 0.059 Uiso 1 1 calc R . .
H38C H 0.2652 0.5791 -0.0738 0.059 Uiso 1 1 calc R . .
C39 C 0.2866(3) 0.64953(15) 0.00790(15) 0.0419(11) Uani 1 1 d . . .
H39A H 0.2675 0.6640 0.0327 0.063 Uiso 1 1 calc R . .
H39B H 0.2647 0.6648 -0.0208 0.063 Uiso 1 1 calc R . .
H39C H 0.3467 0.6500 0.0143 0.063 Uiso 1 1 calc R . .
C40 C 0.4275(2) 0.48261(12) 0.24499(12) 0.0243(8) Uani 1 1 d . . .
C41 C 0.3726(3) 0.44634(13) 0.24211(13) 0.0293(9) Uani 1 1 d . . .
C42 C 0.3539(3) 0.42170(14) 0.20072(14) 0.0346(10) Uani 1 1 d . . .
H42 H 0.3169 0.3979 0.1981 0.042 Uiso 1 1 calc R . .
C43 C 0.3895(3) 0.43231(14) 0.16401(14) 0.0372(11) Uani 1 1 d . . .
H43 H 0.3749 0.4164 0.1364 0.045 Uiso 1 1 calc R . .
C44 C 0.4463(3) 0.46609(15) 0.16797(14) 0.0361(10) Uani 1 1 d . . .
H44 H 0.4715 0.4722 0.1432 0.043 Uiso 1 1 calc R . .
C45 C 0.4675(3) 0.49181(13) 0.20848(13) 0.0294(9) Uani 1 1 d . . .
C46 C 0.3341(3) 0.43345(14) 0.28257(15) 0.0379(10) Uani 1 1 d . . .
H46A H 0.2777 0.4454 0.2773 0.045 Uiso 1 1 calc R . .
H46B H 0.3665 0.4469 0.3107 0.045 Uiso 1 1 calc R . .
C47 C 0.3302(3) 0.38374(15) 0.29008(17) 0.0470(12) Uani 1 1 d . . .
H47A H 0.3056 0.3780 0.3162 0.070 Uiso 1 1 calc R . .
H47B H 0.3859 0.3716 0.2960 0.070 Uiso 1 1 calc R . .
H47C H 0.2967 0.3702 0.2628 0.070 Uiso 1 1 calc R . .
C48 C 0.5329(3) 0.52810(15) 0.21079(16) 0.0376(10) Uani 1 1 d . . .
H48A H 0.5153 0.5481 0.1847 0.045 Uiso 1 1 calc R . .
H48B H 0.5366 0.5451 0.2391 0.045 Uiso 1 1 calc R . .
C49 C 0.6187(3) 0.5094(2) 0.2098(2) 0.0654(16) Uani 1 1 d . . .
H49A H 0.6581 0.5332 0.2113 0.098 Uiso 1 1 calc R . .
H49B H 0.6155 0.4930 0.1815 0.098 Uiso 1 1 calc R . .
H49C H 0.6368 0.4900 0.2360 0.098 Uiso 1 1 calc R . .
C50 C 0.6024(3) 0.54612(17) 0.34124(17) 0.0485(12) Uani 1 1 d . . .
H50A H 0.5782 0.5743 0.3459 0.073 Uiso 1 1 calc R . .
H50B H 0.6245 0.5473 0.3137 0.073 Uiso 1 1 calc R . .
H50C H 0.6467 0.5393 0.3676 0.073 Uiso 1 1 calc R . .
C51 C 0.4790(3) 0.49970(18) 0.38882(15) 0.0503(13) Uani 1 1 d . . .
H51A H 0.4545 0.5277 0.3937 0.075 Uiso 1 1 calc R . .
H51B H 0.5242 0.4932 0.4148 0.075 Uiso 1 1 calc R . .
H51C H 0.4372 0.4769 0.3858 0.075 Uiso 1 1 calc R . .
C52 C 0.5677(4) 0.44794(17) 0.32565(18) 0.0583(15) Uani 1 1 d . . .
H52A H 0.5256 0.4252 0.3221 0.087 Uiso 1 1 calc R . .
H52B H 0.6119 0.4413 0.3521 0.087 Uiso 1 1 calc R . .
H52C H 0.5901 0.4492 0.2982 0.087 Uiso 1 1 calc R . .
C53 C 0.4570(3) 0.77765(13) 0.20665(13) 0.0291(9) Uani 1 1 d . . .
C54 C 0.3959(3) 0.80775(13) 0.21447(14) 0.0326(9) Uani 1 1 d . . .
C55 C 0.4153(3) 0.83606(15) 0.25305(16) 0.0420(11) Uani 1 1 d . . .
H55 H 0.3751 0.8558 0.2588 0.050 Uiso 1 1 calc R . .
C56 C 0.4936(3) 0.83492(15) 0.28253(16) 0.0423(11) Uani 1 1 d . . .
H56 H 0.5056 0.8538 0.3081 0.051 Uiso 1 1 calc R . .
C57 C 0.5540(3) 0.80605(15) 0.27429(15) 0.0394(11) Uani 1 1 d . . .
H57 H 0.6066 0.8058 0.2943 0.047 Uiso 1 1 calc R . .
C58 C 0.5373(3) 0.77717(15) 0.23634(13) 0.0333(10) Uani 1 1 d . . .
C59 C 0.3092(3) 0.81150(14) 0.18269(17) 0.0412(11) Uani 1 1 d . . .
H59A H 0.2673 0.8060 0.2008 0.049 Uiso 1 1 calc R . .
H59B H 0.3033 0.7887 0.1589 0.049 Uiso 1 1 calc R . .
C60 C 0.2925(3) 0.85665(16) 0.1592(2) 0.0618(16) Uani 1 1 d . . .
H60A H 0.2370 0.8571 0.1398 0.093 Uiso 1 1 calc R . .
H60B H 0.3328 0.8620 0.1405 0.093 Uiso 1 1 calc R . .
H60C H 0.2972 0.8794 0.1825 0.093 Uiso 1 1 calc R . .
C61 C 0.6042(3) 0.74729(19) 0.22574(17) 0.0494(13) Uani 1 1 d . . .
H61A H 0.5847 0.7169 0.2263 0.059 Uiso 1 1 calc R . .
H61B H 0.6094 0.7535 0.1942 0.059 Uiso 1 1 calc R . .
C62 C 0.6871(4) 0.7497(2) 0.2555(2) 0.0777(19) Uani 1 1 d . . .
H62A H 0.7235 0.7291 0.2447 0.117 Uiso 1 1 calc R . .
H62B H 0.6842 0.7423 0.2868 0.117 Uiso 1 1 calc R . .
H62C H 0.7087 0.7792 0.2548 0.117 Uiso 1 1 calc R . .
C63 C 0.3526(3) 0.76745(17) 0.07006(15) 0.0453(12) Uani 1 1 d . . .
H63A H 0.3176 0.7887 0.0811 0.068 Uiso 1 1 calc R . .
H63B H 0.3248 0.7392 0.0661 0.068 Uiso 1 1 calc R . .
H63C H 0.3629 0.7772 0.0408 0.068 Uiso 1 1 calc R . .
C64 C 0.5223(3) 0.72089(18) 0.09178(16) 0.0497(13) Uani 1 1 d . . .
H64A H 0.5747 0.7182 0.1140 0.075 Uiso 1 1 calc R . .
H64B H 0.5326 0.7307 0.0625 0.075 Uiso 1 1 calc R . .
H64C H 0.4947 0.6926 0.0878 0.075 Uiso 1 1 calc R . .
C65 C 0.5084(3) 0.81763(17) 0.11938(16) 0.0500(13) Uani 1 1 d . . .
H65A H 0.5610 0.8154 0.1415 0.075 Uiso 1 1 calc R . .
H65B H 0.4736 0.8392 0.1300 0.075 Uiso 1 1 calc R . .
H65C H 0.5182 0.8266 0.0898 0.075 Uiso 1 1 calc R . .
C66 C 0.6231(3) 0.74401(14) 0.39755(13) 0.0329(10) Uani 1 1 d . . .
C67 C 0.7000(3) 0.73164(19) 0.38647(16) 0.0488(12) Uani 1 1 d . . .
C68 C 0.7571(4) 0.7651(3) 0.3846(2) 0.0730(19) Uani 1 1 d . . .
H68 H 0.8079 0.7578 0.3771 0.088 Uiso 1 1 calc R . .
C69 C 0.7418(4) 0.8084(2) 0.39336(19) 0.0722(19) Uani 1 1 d . . .
H69 H 0.7813 0.8301 0.3912 0.087 Uiso 1 1 calc R . .
C70 C 0.6675(4) 0.82003(18) 0.40542(18) 0.0600(16) Uani 1 1 d . . .
H70 H 0.6577 0.8495 0.4120 0.072 Uiso 1 1 calc R . .
C71 C 0.6066(3) 0.78774(15) 0.40779(14) 0.0399(11) Uani 1 1 d . . .
C72 C 0.7200(3) 0.6842(2) 0.37612(19) 0.0588(15) Uani 1 1 d . . .
H72A H 0.7445 0.6843 0.3490 0.071 Uiso 1 1 calc R . .
H72B H 0.6675 0.6680 0.3678 0.071 Uiso 1 1 calc R . .
C73 C 0.7783(4) 0.6589(2) 0.4145(2) 0.080(2) Uani 1 1 d . . .
H73A H 0.7861 0.6294 0.4040 0.121 Uiso 1 1 calc R . .
H73B H 0.7542 0.6575 0.4414 0.121 Uiso 1 1 calc R . .
H73C H 0.8314 0.6738 0.4224 0.121 Uiso 1 1 calc R . .
C74 C 0.5256(4) 0.80233(19) 0.4199(2) 0.0624(16) Uani 1 1 d . . .
H74A H 0.4968 0.8219 0.3954 0.075 Uiso 1 1 calc R . .
H74B H 0.4906 0.7763 0.4196 0.075 Uiso 1 1 calc R . .
C75 C 0.5315(5) 0.8244(3) 0.4631(3) 0.103(3) Uani 1 1 d . . .
H75A H 0.4762 0.8321 0.4668 0.155 Uiso 1 1 calc R . .
H75B H 0.5643 0.8509 0.4638 0.155 Uiso 1 1 calc R . .
H75C H 0.5578 0.8052 0.4881 0.155 Uiso 1 1 calc R . .
C76 C 0.6469(3) 0.70415(16) 0.49737(15) 0.0489(13) Uani 1 1 d . . .
H76A H 0.6400 0.7356 0.5004 0.073 Uiso 1 1 calc R . .
H76B H 0.6995 0.6983 0.4891 0.073 Uiso 1 1 calc R . .
H76C H 0.6459 0.6899 0.5264 0.073 Uiso 1 1 calc R . .
C77 C 0.5719(4) 0.62087(15) 0.44468(16) 0.0502(13) Uani 1 1 d . . .
H77A H 0.5266 0.6098 0.4209 0.075 Uiso 1 1 calc R . .
H77B H 0.5711 0.6065 0.4737 0.075 Uiso 1 1 calc R . .
H77C H 0.6242 0.6149 0.4362 0.075 Uiso 1 1 calc R . .
C78 C 0.4591(4) 0.6911(2) 0.46916(19) 0.0629(15) Uani 1 1 d . . .
H78A H 0.4136 0.6799 0.4456 0.094 Uiso 1 1 calc R . .
H78B H 0.4511 0.7223 0.4733 0.094 Uiso 1 1 calc R . .
H78C H 0.4605 0.6759 0.4980 0.094 Uiso 1 1 calc R . .
C79 C 0.0718(3) 0.75511(15) 0.30001(15) 0.0394(11) Uani 1 1 d . . .
C80 C 0.0061(3) 0.72806(18) 0.30913(19) 0.0515(13) Uani 1 1 d . . .
C81 C -0.0752(3) 0.7388(2) 0.2874(2) 0.0622(15) Uani 1 1 d . . .
H81 H -0.1190 0.7219 0.2937 0.075 Uiso 1 1 calc R . .
C82 C -0.0930(3) 0.7732(2) 0.2572(2) 0.0587(14) Uani 1 1 d . . .
H82 H -0.1486 0.7797 0.2434 0.070 Uiso 1 1 calc R . .
C83 C -0.0279(3) 0.79927(18) 0.24640(18) 0.0541(14) Uani 1 1 d . . .
H83 H -0.0397 0.8227 0.2254 0.065 Uiso 1 1 calc R . .
C84 C 0.0532(3) 0.78912(14) 0.26769(14) 0.0331(10) Uani 1 1 d . . .
C85 C 0.0239(4) 0.6889(2) 0.3428(2) 0.0698(17) Uani 1 1 d . . .
H85A H 0.0106 0.6617 0.3252 0.084 Uiso 1 1 calc R . .
H85B H 0.0835 0.6884 0.3567 0.084 Uiso 1 1 calc R . .
C86 C -0.0216(7) 0.6890(4) 0.3801(4) 0.172(6) Uani 1 1 d . . .
H86A H -0.0066 0.6632 0.3992 0.258 Uiso 1 1 calc R . .
H86B H -0.0808 0.6888 0.3670 0.258 Uiso 1 1 calc R . .
H86C H -0.0073 0.7152 0.3987 0.258 Uiso 1 1 calc R . .
C87 C 0.1248(4) 0.8183(2) 0.2585(2) 0.0637(15) Uani 1 1 d . . .
H87A H 0.1518 0.8324 0.2876 0.076 Uiso 1 1 calc R . .
H87B H 0.1660 0.7992 0.2492 0.076 Uiso 1 1 calc R . .
C88 C 0.1009(4) 0.8529(2) 0.2231(2) 0.0727(18) Uani 1 1 d . . .
H88A H 0.1498 0.8692 0.2201 0.109 Uiso 1 1 calc R . .
H88B H 0.0614 0.8727 0.2323 0.109 Uiso 1 1 calc R . .
H88C H 0.0757 0.8394 0.1939 0.109 Uiso 1 1 calc R . .
C89 C 0.2353(5) 0.7418(2) 0.42499(18) 0.090(3) Uani 1 1 d . . .
H89A H 0.2793 0.7231 0.4191 0.136 Uiso 1 1 calc R . .
H89B H 0.1900 0.7238 0.4305 0.136 Uiso 1 1 calc R . .
H89C H 0.2565 0.7599 0.4519 0.136 Uiso 1 1 calc R . .
C90 C 0.2889(4) 0.8119(3) 0.3657(3) 0.122(4) Uani 1 1 d . . .
H90A H 0.2714 0.8311 0.3394 0.183 Uiso 1 1 calc R . .
H90B H 0.3325 0.7926 0.3604 0.183 Uiso 1 1 calc R . .
H90C H 0.3096 0.8294 0.3931 0.183 Uiso 1 1 calc R . .
C91 C 0.1124(3) 0.81426(18) 0.38608(17) 0.0533(14) Uani 1 1 d . . .
H91A H 0.0924 0.8331 0.3597 0.080 Uiso 1 1 calc R . .
H91B H 0.1340 0.8322 0.4130 0.080 Uiso 1 1 calc R . .
H91C H 0.0671 0.7963 0.3917 0.080 Uiso 1 1 calc R . .
C92 C -0.0871(2) 0.71365(13) 0.08049(13) 0.0299(9) Uani 1 1 d . . .
C93 C -0.1063(3) 0.67504(15) 0.05338(16) 0.0433(12) Uani 1 1 d . . .
C94 C -0.1886(3) 0.65932(17) 0.0451(2) 0.0588(15) Uani 1 1 d . . .
H94 H -0.2024 0.6335 0.0278 0.071 Uiso 1 1 calc R . .
C95 C -0.2499(3) 0.68117(19) 0.06186(19) 0.0552(14) Uani 1 1 d . . .
H95 H -0.3042 0.6699 0.0562 0.066 Uiso 1 1 calc R . .
C96 C -0.2308(3) 0.71932(17) 0.08676(16) 0.0429(11) Uani 1 1 d . . .
H96 H -0.2728 0.7343 0.0973 0.052 Uiso 1 1 calc R . .
C97 C -0.1499(3) 0.73627(14) 0.09669(14) 0.0328(10) Uani 1 1 d . . .
C98 C -0.0451(3) 0.65138(19) 0.03084(19) 0.0633(17) Uani 1 1 d . . .
H98A H -0.0487 0.6197 0.0358 0.076 Uiso 1 1 calc R . .
H98B H 0.0114 0.6609 0.0451 0.076 Uiso 1 1 calc R . .
C99 C -0.0632(4) 0.6612(3) -0.0230(2) 0.094(3) Uani 1 1 d . . .
H99A H -0.0237 0.6454 -0.0366 0.141 Uiso 1 1 calc R . .
H99B H -0.0580 0.6925 -0.0279 0.141 Uiso 1 1 calc R . .
H99C H -0.1191 0.6517 -0.0372 0.141 Uiso 1 1 calc R . .
C100 C -0.1296(3) 0.77931(18) 0.12387(17) 0.0492(13) Uani 1 1 d . . .
H10D H -0.0881 0.7727 0.1521 0.059 Uiso 1 1 calc R . .
H10E H -0.1035 0.7993 0.1054 0.059 Uiso 1 1 calc R . .
C101 C -0.2007(4) 0.8037(2) 0.1375(2) 0.077(2) Uani 1 1 d . . .
H10D H -0.1799 0.8303 0.1539 0.115 Uiso 1 1 calc R . .
H10E H -0.2256 0.7851 0.1573 0.115 Uiso 1 1 calc R . .
H10F H -0.2421 0.8112 0.1101 0.115 Uiso 1 1 calc R . .
C102 C 0.1048(4) 0.7479(3) 0.0216(2) 0.080(2) Uani 1 1 d . . .
H10G H 0.0830 0.7215 0.0051 0.120 Uiso 1 1 calc R . .
H10H H 0.1553 0.7409 0.0440 0.120 Uiso 1 1 calc R . .
H10I H 0.1167 0.7695 0.0000 0.120 Uiso 1 1 calc R . .
C103 C 0.0707(4) 0.82137(19) 0.0834(2) 0.0706(18) Uani 1 1 d . . .
H10J H 0.0312 0.8339 0.0995 0.106 Uiso 1 1 calc R . .
H10K H 0.0828 0.8425 0.0614 0.106 Uiso 1 1 calc R . .
H10L H 0.1215 0.8140 0.1054 0.106 Uiso 1 1 calc R . .
C104 C -0.0719(3) 0.7869(2) 0.00893(19) 0.0657(17) Uani 1 1 d . . .
H10M H -0.0964 0.7610 -0.0077 0.099 Uiso 1 1 calc R . .
H10N H -0.0580 0.8080 -0.0126 0.099 Uiso 1 1 calc R . .
H10O H -0.1112 0.8000 0.0249 0.099 Uiso 1 1 calc R . .
C105 C 0.8753(2) 0.65423(13) 0.18158(14) 0.0276(9) Uani 1 1 d . . .
H10P H 0.9292 0.6522 0.2025 0.041 Uiso 1 1 calc R . .
H10Q H 0.8672 0.6838 0.1692 0.041 Uiso 1 1 calc R . .
H10R H 0.8724 0.6335 0.1566 0.041 Uiso 1 1 calc R . .
C106 C 0.8120(3) 0.64434(14) 0.20587(16) 0.0380(10) Uani 1 1 d . . .
C107 C 0.8336(3) 0.63203(16) 0.25294(17) 0.0487(12) Uani 1 1 d . . .
H107 H 0.8897 0.6307 0.2684 0.058 Uiso 1 1 calc R . .
C108 C 0.7713(4) 0.62197(18) 0.27615(19) 0.0617(16) Uani 1 1 d . . .
H108 H 0.7856 0.6138 0.3073 0.074 Uiso 1 1 calc R . .
C109 C 0.6882(4) 0.62387(18) 0.2535(2) 0.0634(16) Uani 1 1 d . . .
H109 H 0.6465 0.6179 0.2696 0.076 Uiso 1 1 calc R . .
C110 C 0.6669(3) 0.63446(17) 0.2075(2) 0.0536(13) Uani 1 1 d . . .
H110 H 0.6108 0.6348 0.1920 0.064 Uiso 1 1 calc R . .
C111 C 0.7276(3) 0.64462(16) 0.18395(17) 0.0421(11) Uani 1 1 d . . .
H111 H 0.7122 0.6519 0.1525 0.050 Uiso 1 1 calc R . .
H1 H 0.085(4) 0.577(2) 0.329(2) 0.08(2) Uiso 1 1 d . . .
H2 H 0.314(3) 0.5742(14) 0.3885(14) 0.026(11) Uiso 1 1 d . . .
H3 H 0.181(3) 0.4947(16) 0.3381(16) 0.033(14) Uiso 1 1 d . . .
H4 H 0.090(3) 0.6074(15) 0.2596(15) 0.026(13) Uiso 1 1 d . . .
H5 H 0.169(3) 0.5499(16) 0.2071(16) 0.024(15) Uiso 1 1 d . . .
H6 H -0.035(3) 0.6075(17) 0.1726(17) 0.038(16) Uiso 1 1 d . . .
H7 H 0.203(3) 0.6274(15) 0.1119(16) 0.019(15) Uiso 1 1 d . . .
H8 H 0.340(3) 0.5351(14) 0.1486(15) 0.017(14) Uiso 1 1 d . . .
H9 H 0.150(4) 0.540(2) 0.126(2) 0.07(2) Uiso 1 1 d . . .
H10 H 0.257(3) 0.5310(15) 0.2868(16) 0.029(13) Uiso 1 1 d . . .
H11 H 0.420(5) 0.630(3) 0.334(3) 0.16(3) Uiso 1 1 d . . .
H12 H 0.364(3) 0.5795(15) 0.2200(15) 0.014(14) Uiso 1 1 d . . .
H13 H 0.342(3) 0.6593(18) 0.1257(18) 0.039(17) Uiso 1 1 d . . .
H14 H 0.296(3) 0.7105(16) 0.2126(17) 0.039(15) Uiso 1 1 d . . .
H15 H 0.434(3) 0.6538(16) 0.2261(16) 0.023(16) Uiso 1 1 d . . .
H16 H 0.456(3) 0.7606(14) 0.3193(14) 0.013(13) Uiso 1 1 d . . .
H17 H 0.393(2) 0.6735(11) 0.3797(12) 0.009(8) Uiso 1 1 d . . .
H18 H 0.519(4) 0.685(2) 0.278(2) 0.09(2) Uiso 1 1 d . . .
H19 H 0.313(5) 0.670(2) 0.346(2) 0.09(2) Uiso 1 1 d . . .
H20 H 0.308(3) 0.7290(15) 0.2841(15) 0.006(14) Uiso 1 1 d . . .
H21 H 0.121(3) 0.6828(15) 0.2466(16) 0.026(14) Uiso 1 1 d . . .
H22 H 0.068(3) 0.6426(17) 0.1359(18) 0.034(18) Uiso 1 1 d . . .
H23 H 0.187(3) 0.7270(17) 0.1472(18) 0.037(16) Uiso 1 1 d . . .
H24 H 0.031(3) 0.7351(19) 0.1897(19) 0.055(18) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.0457(7) 0.0266(6) 0.0226(5) 0.0014(4) 0.0134(5) -0.0072(5)
Si2 0.0524(8) 0.0431(7) 0.0257(6) -0.0026(5) 0.0104(5) -0.0152(6)
Si3 0.0214(5) 0.0272(5) 0.0184(5) -0.0011(4) 0.0036(4) -0.0026(4)
Si4 0.0289(6) 0.0382(6) 0.0281(6) -0.0079(5) -0.0002(5) -0.0067(5)
Si5 0.0238(5) 0.0268(5) 0.0160(5) -0.0029(4) 0.0045(4) -0.0001(4)
Si6 0.0303(6) 0.0344(6) 0.0172(5) 0.0009(4) 0.0034(4) 0.0014(5)
Si7 0.0230(5) 0.0213(5) 0.0180(5) -0.0004(4) 0.0024(4) 0.0024(4)
Si8 0.0350(6) 0.0351(6) 0.0267(6) -0.0006(5) -0.0045(5) 0.0115(5)
Si9 0.0192(5) 0.0276(5) 0.0174(5) -0.0025(4) 0.0034(4) -0.0039(4)
Si10 0.0359(6) 0.0446(7) 0.0232(6) -0.0013(5) 0.0082(5) -0.0168(5)
Si11 0.0304(6) 0.0315(6) 0.0243(5) -0.0054(4) -0.0050(5) 0.0023(5)
Si12 0.0482(7) 0.0369(7) 0.0221(6) -0.0051(5) 0.0015(5) -0.0023(6)
Si13 0.0268(5) 0.0244(5) 0.0179(5) -0.0018(4) 0.0042(4) 0.0050(4)
Si14 0.0518(8) 0.0565(9) 0.0420(8) -0.0181(6) -0.0033(6) 0.0169(7)
Si15 0.0217(5) 0.0253(6) 0.0313(6) 0.0026(4) -0.0058(4) 0.0017(4)
Si16 0.0317(7) 0.0604(9) 0.0394(7) 0.0182(6) -0.0002(5) 0.0029(6)
N1 0.041(2) 0.0276(18) 0.0251(17) 0.0028(13) 0.0118(15) -0.0086(15)
N2 0.0244(17) 0.0285(17) 0.0227(16) -0.0006(13) 0.0027(13) -0.0032(14)
N3 0.0244(16) 0.0292(17) 0.0187(15) -0.0024(12) 0.0056(13) 0.0008(14)
N4 0.0272(17) 0.0248(17) 0.0203(15) -0.0015(12) 0.0015(13) 0.0046(13)
N5 0.0256(17) 0.0315(18) 0.0202(15) -0.0029(13) 0.0066(13) -0.0069(14)
N6 0.0331(18) 0.0289(18) 0.0216(16) -0.0033(13) -0.0032(14) 0.0008(15)
N7 0.0198(16) 0.0302(17) 0.0229(16) -0.0028(13) 0.0033(13) 0.0053(13)
N8 0.0203(16) 0.0317(18) 0.0288(17) 0.0006(14) -0.0045(13) 0.0017(14)
O1 0.049(2) 0.0475(19) 0.0228(16) 0.0029(14) 0.0080(15) 0.0024(15)
O2 0.0392(17) 0.0346(16) 0.0296(15) 0.0001(12) 0.0118(13) -0.0018(14)
O3 0.0438(18) 0.0301(17) 0.0317(16) -0.0048(13) 0.0140(14) -0.0104(15)
O4 0.0300(16) 0.0301(16) 0.0219(14) -0.0023(12) 0.0060(11) -0.0086(14)
O5 0.0235(16) 0.0405(18) 0.0228(15) 0.0009(13) 0.0039(13) 0.0005(14)
O6 0.0237(15) 0.0337(16) 0.0266(15) 0.0013(12) 0.0050(12) 0.0027(13)
O7 0.0218(16) 0.0326(17) 0.0287(16) -0.0043(12) 0.0076(13) 0.0006(14)
O8 0.0349(17) 0.0361(19) 0.0218(15) -0.0004(13) 0.0026(12) 0.0117(15)
O9 0.0337(16) 0.0366(17) 0.0294(16) -0.0050(13) 0.0147(14) -0.0074(13)
O10 0.0247(14) 0.0290(15) 0.0219(14) 0.0010(11) 0.0081(12) -0.0004(11)
O11 0.0290(14) 0.0246(14) 0.0221(13) -0.0035(10) 0.0000(11) 0.0010(11)
O12 0.0307(17) 0.0250(16) 0.0232(16) -0.0008(13) 0.0026(14) 0.0009(13)
O13 0.0303(17) 0.0381(17) 0.0223(14) -0.0074(12) 0.0098(12) -0.0106(15)
O14 0.0255(14) 0.0304(15) 0.0183(14) -0.0017(11) 0.0042(11) -0.0043(11)
O15 0.0238(15) 0.0309(18) 0.0260(15) 0.0012(13) 0.0004(11) -0.0030(14)
O16 0.0290(16) 0.0301(18) 0.0309(16) 0.0007(13) 0.0001(13) -0.0035(14)
O17 0.0362(17) 0.0375(17) 0.0349(16) -0.0039(13) 0.0058(14) 0.0047(14)
O18 0.0351(17) 0.063(2) 0.0249(16) -0.0072(14) 0.0013(13) 0.0095(15)
O19 0.0406(18) 0.0292(15) 0.0240(14) 0.0027(11) 0.0074(13) 0.0097(13)
O20 0.0229(18) 0.043(2) 0.0233(16) -0.0046(13) 0.0024(14) 0.0030(15)
O21 0.0348(17) 0.0275(16) 0.0210(15) -0.0007(12) 0.0030(13) 0.0010(13)
O22 0.0243(16) 0.0284(17) 0.0382(18) 0.0056(13) 0.0106(13) 0.0018(14)
O23 0.0284(18) 0.0371(19) 0.062(2) 0.0194(16) -0.0140(16) -0.0032(15)
O24 0.0405(18) 0.0331(18) 0.0293(16) -0.0041(13) -0.0052(13) 0.0107(14)
C1 0.069(3) 0.046(3) 0.019(2) -0.0018(18) 0.015(2) -0.029(2)
C2 0.134(6) 0.037(3) 0.030(3) 0.001(2) 0.021(3) -0.031(3)
C3 0.256(13) 0.057(4) 0.057(4) -0.016(3) 0.079(6) -0.068(6)
C4 0.231(13) 0.099(7) 0.073(5) -0.048(5) 0.080(7) -0.115(8)
C5 0.122(6) 0.175(9) 0.036(3) -0.032(4) 0.044(4) -0.106(7)
C6 0.071(4) 0.101(5) 0.023(2) -0.011(3) 0.020(2) -0.045(4)
C7 0.138(7) 0.044(3) 0.056(4) 0.009(3) 0.020(4) 0.022(4)
C8 0.192(10) 0.074(5) 0.093(6) -0.022(4) 0.009(6) 0.034(6)
C9 0.046(3) 0.153(7) 0.037(3) 0.008(4) 0.019(2) -0.003(4)
C10 0.048(4) 0.319(15) 0.055(4) -0.026(6) 0.016(3) 0.005(6)
C11 0.100(5) 0.052(3) 0.062(4) -0.021(3) 0.025(3) -0.015(3)
C12 0.087(4) 0.088(4) 0.024(2) -0.001(2) 0.008(3) -0.035(4)
C13 0.058(3) 0.085(4) 0.048(3) 0.000(3) -0.001(3) -0.017(3)
C14 0.024(2) 0.026(2) 0.026(2) -0.0004(15) 0.0021(16) -0.0077(16)
C15 0.033(2) 0.027(2) 0.030(2) -0.0037(16) 0.0049(17) -0.0124(17)
C16 0.040(2) 0.035(2) 0.028(2) 0.0000(17) 0.0081(18) -0.011(2)
C17 0.041(3) 0.033(2) 0.040(3) 0.0105(19) 0.001(2) -0.011(2)
C18 0.033(2) 0.028(2) 0.048(3) 0.0094(19) 0.006(2) 0.0002(18)
C19 0.027(2) 0.027(2) 0.038(2) -0.0020(17) 0.0084(17) -0.0059(17)
C20 0.044(3) 0.039(2) 0.031(2) -0.0030(18) 0.0156(19) -0.003(2)
C21 0.040(3) 0.061(3) 0.079(4) -0.002(3) 0.021(3) -0.004(3)
C22 0.035(2) 0.037(2) 0.045(3) 0.0038(19) 0.019(2) 0.0019(19)
C23 0.071(4) 0.048(3) 0.061(3) -0.014(3) 0.031(3) -0.011(3)
C24 0.057(3) 0.051(3) 0.058(3) -0.008(2) -0.011(3) -0.019(3)
C25 0.026(2) 0.053(3) 0.052(3) -0.010(2) -0.008(2) -0.002(2)
C26 0.052(3) 0.081(4) 0.032(3) -0.018(2) 0.000(2) -0.008(3)
C27 0.033(2) 0.034(2) 0.0169(18) 0.0004(15) 0.0069(16) 0.0066(18)
C28 0.030(2) 0.047(3) 0.0196(19) -0.0013(17) 0.0089(16) 0.0037(19)
C29 0.034(2) 0.058(3) 0.028(2) 0.001(2) 0.0099(18) 0.010(2)
C30 0.048(3) 0.052(3) 0.030(2) -0.001(2) 0.018(2) 0.021(2)
C31 0.051(3) 0.038(2) 0.028(2) -0.0065(18) 0.010(2) 0.007(2)
C32 0.038(2) 0.033(2) 0.0200(19) -0.0022(16) 0.0027(17) 0.0077(18)
C33 0.029(2) 0.052(3) 0.034(2) -0.003(2) 0.0084(18) 0.000(2)
C34 0.031(2) 0.075(4) 0.047(3) -0.013(2) 0.011(2) -0.007(2)
C35 0.037(2) 0.033(2) 0.041(2) -0.0117(19) -0.004(2) 0.0031(19)
C36 0.040(3) 0.038(3) 0.083(4) 0.006(3) 0.013(3) -0.004(2)
C37 0.036(2) 0.050(3) 0.030(2) 0.0041(19) 0.0023(19) 0.007(2)
C38 0.044(3) 0.056(3) 0.020(2) 0.0023(19) 0.0080(18) 0.007(2)
C39 0.052(3) 0.042(3) 0.029(2) 0.0105(19) 0.004(2) -0.001(2)
C40 0.027(2) 0.0203(19) 0.0228(19) -0.0005(15) 0.0002(15) 0.0093(16)
C41 0.032(2) 0.026(2) 0.028(2) -0.0034(16) 0.0030(17) 0.0088(17)
C42 0.039(2) 0.030(2) 0.032(2) -0.0069(17) 0.0018(19) 0.0038(19)
C43 0.048(3) 0.034(2) 0.025(2) -0.0064(17) -0.0022(19) 0.014(2)
C44 0.045(3) 0.040(3) 0.024(2) 0.0017(18) 0.0102(18) 0.013(2)
C45 0.032(2) 0.031(2) 0.027(2) 0.0002(16) 0.0077(17) 0.0131(17)
C46 0.044(3) 0.029(2) 0.042(2) -0.0040(18) 0.011(2) -0.0013(19)
C47 0.061(3) 0.034(3) 0.048(3) 0.011(2) 0.019(2) 0.014(2)
C48 0.038(2) 0.040(3) 0.039(2) 0.0005(19) 0.017(2) 0.005(2)
C49 0.043(3) 0.068(4) 0.092(4) -0.012(3) 0.029(3) 0.005(3)
C50 0.031(2) 0.061(3) 0.048(3) -0.012(2) -0.003(2) 0.003(2)
C51 0.063(3) 0.056(3) 0.027(2) 0.006(2) -0.001(2) 0.003(3)
C52 0.062(3) 0.054(3) 0.047(3) -0.004(2) -0.015(3) 0.029(3)
C53 0.035(2) 0.029(2) 0.024(2) -0.0047(16) 0.0085(17) -0.0128(18)
C54 0.037(2) 0.025(2) 0.037(2) -0.0001(17) 0.0107(19) -0.0077(18)
C55 0.050(3) 0.029(2) 0.052(3) -0.009(2) 0.022(2) -0.008(2)
C56 0.057(3) 0.037(3) 0.037(2) -0.013(2) 0.020(2) -0.024(2)
C57 0.037(2) 0.048(3) 0.032(2) -0.0102(19) 0.0038(19) -0.023(2)
C58 0.029(2) 0.045(3) 0.024(2) -0.0035(18) 0.0045(17) -0.0107(19)
C59 0.032(2) 0.029(2) 0.061(3) 0.001(2) 0.009(2) -0.0028(19)
C60 0.043(3) 0.035(3) 0.096(4) 0.013(3) -0.008(3) -0.005(2)
C61 0.029(2) 0.071(3) 0.046(3) -0.016(2) 0.002(2) -0.011(2)
C62 0.044(3) 0.076(4) 0.105(5) -0.017(4) -0.003(3) -0.005(3)
C63 0.051(3) 0.051(3) 0.031(2) 0.005(2) 0.004(2) -0.019(2)
C64 0.047(3) 0.069(3) 0.037(3) -0.008(2) 0.021(2) -0.017(3)
C65 0.057(3) 0.060(3) 0.033(2) 0.006(2) 0.008(2) -0.025(3)
C66 0.033(2) 0.043(3) 0.0186(19) -0.0014(17) -0.0029(17) -0.0023(19)
C67 0.040(3) 0.074(4) 0.032(2) -0.011(2) 0.009(2) -0.003(3)
C68 0.055(4) 0.115(6) 0.054(3) -0.024(3) 0.022(3) -0.026(4)
C69 0.084(5) 0.090(5) 0.044(3) -0.006(3) 0.017(3) -0.047(4)
C70 0.081(4) 0.047(3) 0.042(3) -0.006(2) -0.007(3) -0.023(3)
C71 0.045(3) 0.039(3) 0.029(2) -0.0044(18) -0.0059(19) -0.004(2)
C72 0.041(3) 0.081(4) 0.056(3) -0.016(3) 0.014(2) 0.011(3)
C73 0.053(4) 0.099(5) 0.083(5) -0.017(4) 0.002(3) 0.013(3)
C74 0.056(3) 0.056(3) 0.067(4) -0.029(3) -0.005(3) 0.011(3)
C75 0.099(5) 0.118(6) 0.107(6) -0.072(5) 0.053(5) -0.049(5)
C76 0.067(3) 0.047(3) 0.025(2) -0.0001(19) -0.009(2) 0.000(2)
C77 0.072(4) 0.034(3) 0.038(3) 0.005(2) -0.002(2) -0.004(2)
C78 0.069(4) 0.076(4) 0.051(3) -0.012(3) 0.029(3) -0.011(3)
C79 0.037(2) 0.046(3) 0.034(2) -0.010(2) 0.0057(19) 0.009(2)
C80 0.039(3) 0.056(3) 0.063(3) -0.001(3) 0.018(2) 0.002(2)
C81 0.031(3) 0.089(4) 0.064(4) 0.012(3) 0.006(2) -0.001(3)
C82 0.030(3) 0.074(4) 0.069(4) -0.001(3) 0.004(2) 0.006(3)
C83 0.054(3) 0.055(3) 0.047(3) -0.008(2) -0.003(2) 0.021(3)
C84 0.033(2) 0.038(2) 0.027(2) -0.0038(17) 0.0037(17) 0.0124(19)
C85 0.063(4) 0.078(4) 0.072(4) 0.015(3) 0.023(3) -0.002(3)
C86 0.198(11) 0.210(12) 0.152(9) 0.116(9) 0.134(9) 0.112(10)
C87 0.052(3) 0.065(4) 0.075(4) 0.013(3) 0.015(3) 0.012(3)
C88 0.084(4) 0.055(4) 0.080(4) 0.022(3) 0.020(4) 0.015(3)
C89 0.147(7) 0.067(4) 0.038(3) -0.022(3) -0.021(4) 0.053(4)
C90 0.045(4) 0.154(8) 0.170(8) -0.112(7) 0.031(4) -0.026(4)
C91 0.055(3) 0.063(3) 0.038(3) -0.023(2) 0.001(2) 0.024(3)
C92 0.023(2) 0.033(2) 0.029(2) 0.0011(17) -0.0062(16) 0.0005(17)
C93 0.031(2) 0.037(3) 0.051(3) -0.004(2) -0.014(2) 0.005(2)
C94 0.045(3) 0.041(3) 0.076(4) -0.006(3) -0.018(3) -0.007(2)
C95 0.026(2) 0.061(3) 0.069(3) 0.016(3) -0.011(2) -0.008(2)
C96 0.024(2) 0.059(3) 0.042(3) 0.014(2) -0.0014(19) 0.006(2)
C97 0.029(2) 0.037(2) 0.029(2) 0.0065(17) 0.0012(17) 0.0067(18)
C98 0.046(3) 0.060(3) 0.068(4) -0.034(3) -0.021(3) 0.018(3)
C99 0.059(4) 0.124(6) 0.085(5) -0.060(4) -0.015(3) 0.023(4)
C100 0.040(3) 0.062(3) 0.043(3) -0.011(2) 0.002(2) 0.013(2)
C101 0.063(4) 0.083(5) 0.076(4) -0.020(3) -0.004(3) 0.034(3)
C102 0.048(3) 0.145(7) 0.049(3) 0.005(4) 0.014(3) -0.004(4)
C103 0.050(3) 0.054(3) 0.096(5) 0.034(3) -0.010(3) -0.004(3)
C104 0.049(3) 0.090(4) 0.051(3) 0.033(3) -0.003(3) 0.005(3)
C105 0.0161(18) 0.029(2) 0.038(2) 0.0067(17) 0.0073(16) 0.0078(16)
C106 0.038(2) 0.031(2) 0.045(3) -0.0063(19) 0.010(2) 0.0045(19)
C107 0.053(3) 0.047(3) 0.044(3) -0.008(2) 0.005(2) 0.010(2)
C108 0.104(5) 0.046(3) 0.045(3) -0.005(2) 0.036(3) 0.009(3)
C109 0.074(4) 0.047(3) 0.086(5) -0.011(3) 0.054(4) -0.003(3)
C110 0.043(3) 0.052(3) 0.070(4) -0.016(3) 0.022(3) -0.005(2)
C111 0.035(3) 0.045(3) 0.047(3) -0.002(2) 0.011(2) 0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O1 1.620(4) . ?
Si1 O2 1.624(3) . ?
Si1 O3 1.651(3) . ?
Si1 N1 1.704(3) . ?
Si2 N1 1.754(3) . ?
Si2 C11 1.853(6) . ?
Si2 C13 1.853(6) . ?
Si2 C12 1.859(5) . ?
Si3 O5 1.621(3) . ?
Si3 O6 1.626(3) . ?
Si3 O4 1.637(3) . ?
Si3 N2 1.708(3) . ?
Si4 N2 1.767(3) . ?
Si4 C25 1.845(5) . ?
Si4 C26 1.859(5) . ?
Si4 C24 1.859(5) . ?
Si5 O9 1.611(3) . ?
Si5 O7 1.615(3) . ?
Si5 O8 1.644(3) . ?
Si5 N3 1.708(3) . ?
Si6 N3 1.760(3) . ?
Si6 C39 1.856(5) . ?
Si6 C38 1.861(4) . ?
Si6 C37 1.861(4) . ?
Si7 O12 1.625(3) . ?
Si7 O11 1.630(3) . ?
Si7 O10 1.630(3) . ?
Si7 N4 1.709(3) . ?
Si7 H12 1.84(4) . ?
Si8 N4 1.759(3) . ?
Si8 C52 1.854(5) . ?
Si8 C50 1.865(5) . ?
Si8 C51 1.868(5) . ?
Si9 O13 1.609(3) . ?
Si9 O14 1.631(3) . ?
Si9 O15 1.638(3) . ?
Si9 N5 1.713(3) . ?
Si9 H13 1.94(5) . ?
Si9 H15 1.98(5) . ?
Si10 N5 1.758(3) . ?
Si10 C64 1.868(5) . ?
Si10 C63 1.868(5) . ?
Si10 C65 1.881(5) . ?
Si11 O18 1.615(3) . ?
Si11 O17 1.615(3) . ?
Si11 O16 1.641(3) . ?
Si11 N6 1.706(3) . ?
Si12 N6 1.754(3) . ?
Si12 C78 1.856(6) . ?
Si12 C76 1.867(5) . ?
Si12 C77 1.869(5) . ?
Si13 O20 1.622(4) . ?
Si13 O21 1.629(3) . ?
Si13 O19 1.632(3) . ?
Si13 N7 1.710(3) . ?
Si13 H20 1.95(4) . ?
Si14 N7 1.766(3) . ?
Si14 C89 1.841(6) . ?
Si14 C91 1.860(5) . ?
Si14 C90 1.880(8) . ?
Si15 O23 1.598(4) . ?
Si15 O22 1.623(3) . ?
Si15 O24 1.661(3) . ?
Si15 N8 1.713(3) . ?
Si15 H22 1.98(5) . ?
Si15 H23 1.93(5) . ?
Si16 N8 1.760(4) . ?
Si16 C103 1.849(6) . ?
Si16 C102 1.862(6) . ?
Si16 C104 1.876(5) . ?
N1 C1 1.452(5) . ?
N2 C14 1.458(5) . ?
N3 C27 1.450(5) . ?
N4 C40 1.454(5) . ?
N5 C53 1.447(5) . ?
N6 C66 1.447(5) . ?
N7 C79 1.435(5) . ?
N8 C92 1.460(5) . ?
O1 H1 0.71(6) . ?
O2 H2 0.90(4) . ?
O3 H3 0.73(5) . ?
O4 H4 0.71(5) . ?
O5 H5 0.62(4) . ?
O6 H6 0.70(5) . ?
O7 H7 0.62(4) . ?
O8 H8 0.64(4) . ?
O9 H9 0.76(6) . ?
O10 H10 0.75(5) . ?
O12 H12 0.58(4) . ?
O13 H13 0.65(5) . ?
O14 H14 0.73(5) . ?
O15 H15 0.62(5) . ?
O16 H16 0.66(4) . ?
O17 H11 1.24(9) . ?
O17 H17 0.98(4) . ?
O18 H18 0.92(6) . ?
O19 H19 0.90(7) . ?
O20 H20 0.53(4) . ?
O21 H21 0.65(4) . ?
O22 H22 0.60(5) . ?
O23 H23 0.63(5) . ?
O24 H24 0.78(6) . ?
C1 C6 1.401(8) . ?
C1 C2 1.424(8) . ?
C2 C3 1.385(9) . ?
C2 C7 1.531(10) . ?
C3 C4 1.338(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.427(9) . ?
C5 H5 0.9300 . ?
C6 C9 1.493(10) . ?
C7 C8 1.510(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.537(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C19 1.399(6) . ?
C14 C15 1.413(6) . ?
C15 C16 1.396(6) . ?
C15 C20 1.504(6) . ?
C16 C17 1.374(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.374(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.403(6) . ?
C18 H18 0.9300 . ?
C19 C22 1.513(6) . ?
C20 C21 1.525(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.527(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C32 1.402(6) . ?
C27 C28 1.413(6) . ?
C28 C29 1.397(6) . ?
C28 C33 1.502(6) . ?
C29 C30 1.370(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.408(6) . ?
C31 H31 0.9300 . ?
C32 C35 1.510(6) . ?
C33 C34 1.533(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.516(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C45 1.404(6) . ?
C40 C41 1.404(6) . ?
C41 C42 1.403(5) . ?
C41 C46 1.516(6) . ?
C42 C43 1.374(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.365(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.401(6) . ?
C44 H44 0.9300 . ?
C45 C48 1.519(6) . ?
C46 C47 1.518(6) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 C49 1.519(7) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 C54 1.405(6) . ?
C53 C58 1.409(6) . ?
C54 C55 1.401(6) . ?
C54 C59 1.521(6) . ?
C55 C56 1.379(7) . ?
C55 H55 0.9300 . ?
C56 C57 1.377(7) . ?
C56 H56 0.9300 . ?
C57 C58 1.396(6) . ?
C57 H57 0.9300 . ?
C58 C61 1.501(7) . ?
C59 C60 1.524(6) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 C62 1.445(7) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 C71 1.391(6) . ?
C66 C67 1.417(7) . ?
C67 C68 1.383(8) . ?
C67 C72 1.513(8) . ?
C68 C69 1.364(10) . ?
C68 H68 0.9300 . ?
C69 C70 1.384(9) . ?
C69 H69 0.9300 . ?
C70 C71 1.404(7) . ?
C70 H70 0.9300 . ?
C71 C74 1.509(7) . ?
C72 C73 1.514(8) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 C75 1.423(8) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C79 C84 1.386(6) . ?
C79 C80 1.420(7) . ?
C80 C81 1.379(7) . ?
C80 C85 1.528(8) . ?
C81 C82 1.358(8) . ?
C81 H81 0.9300 . ?
C82 C83 1.414(8) . ?
C82 H82 0.9300 . ?
C83 C84 1.370(6) . ?
C83 H83 0.9300 . ?
C84 C87 1.534(7) . ?
C85 C86 1.454(10) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C87 C88 1.465(8) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C89 H89A 0.9600 . ?
C89 H89B 0.9600 . ?
C89 H89C 0.9600 . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 C97 1.400(6) . ?
C92 C93 1.407(6) . ?
C93 C94 1.396(7) . ?
C93 C98 1.497(7) . ?
C94 C95 1.377(8) . ?
C94 H94 0.9300 . ?
C95 C96 1.363(7) . ?
C95 H95 0.9300 . ?
C96 C97 1.388(6) . ?
C96 H96 0.9300 . ?
C97 C100 1.522(6) . ?
C98 C99 1.576(9) . ?
C98 H98A 0.9700 . ?
C98 H98B 0.9700 . ?
C99 H99A 0.9600 . ?
C99 H99B 0.9600 . ?
C99 H99C 0.9600 . ?
C100 C101 1.503(7) . ?
C100 H10D 0.9700 . ?
C100 H10E 0.9700 . ?
C101 H10D 0.9600 . ?
C101 H10E 0.9600 . ?
C101 H10F 0.9600 . ?
C102 H10G 0.9600 . ?
C102 H10H 0.9600 . ?
C102 H10I 0.9600 . ?
C103 H10J 0.9600 . ?
C103 H10K 0.9600 . ?
C103 H10L 0.9600 . ?
C104 H10M 0.9600 . ?
C104 H10N 0.9600 . ?
C104 H10O 0.9600 . ?
C105 C106 1.413(6) . ?
C105 H10P 0.9600 . ?
C105 H10Q 0.9600 . ?
C105 H10R 0.9600 . ?
C106 C111 1.388(6) . ?
C106 C107 1.404(7) . ?
C107 C108 1.379(8) . ?
C107 H107 0.9300 . ?
C108 C109 1.377(9) . ?
C108 H108 0.9300 . ?
C109 C110 1.361(8) . ?
C109 H109 0.9300 . ?
C110 C111 1.365(7) . ?
C110 H110 0.9300 . ?
C111 H111 0.9300 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30659590
|
1100820.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-16 04:05:44 +0300 (Mon, 16 Jul 2018) $
#$Revision: 209049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100820.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100820
loop_
_publ_author_name
'Prabusankar, Ganesan'
'Murugavel, Ramaswamy'
'Butcher, Ray J.'
_publ_section_title
;
Synthesis, Spectral Studies, and Structural Characterization of a New
Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic
Aluminosilicate
;
_journal_coden_ASTM JOCEAH
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2124
_journal_page_last 2128
_journal_paper_doi 10.1021/om049254+
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C17 H35 N3 O3 Si2'
_chemical_formula_weight 385.66
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 77.332(10)
_cell_angle_beta 74.774(13)
_cell_angle_gamma 64.301(16)
_cell_formula_units_Z 2
_cell_length_a 9.728(3)
_cell_length_b 9.696(3)
_cell_length_c 13.710(2)
_cell_measurement_temperature 294(2)
_cell_volume 1116.1(5)
_diffrn_ambient_temperature 294(2)
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0433
_diffrn_reflns_av_sigmaI/netI 0.0319
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 3986
_diffrn_reflns_theta_max 25.22
_diffrn_reflns_theta_min 1.55
_exptl_absorpt_coefficient_mu 0.178
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.148
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needles
_exptl_crystal_F_000 420
_exptl_crystal_size_max 0.84
_exptl_crystal_size_mid 0.45
_exptl_crystal_size_min 0.25
_refine_ls_extinction_coef 0.025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 259
_refine_ls_number_reflns 3768
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.039
_refine_ls_R_factor_all 0.0747
_refine_ls_R_factor_gt 0.0647
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+0.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1801
_refine_ls_wR_factor_ref 0.1924
_reflns_number_gt 3137
_reflns_number_total 3768
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060452
_cod_depositor_comments
;
Merging entries 1100819-1100822 with entries 4060451-4060454.
Marking entries 1100819-1100822 as duplicates of entries 4060451-4060454.
Antanas Vaitkus,
2018-07-16
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100820
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.67532(8) 0.08389(8) 0.88626(6) 0.0456(3) Uani 1 1 d . . .
Si2 Si 0.74374(11) -0.04502(10) 0.68666(7) 0.0623(3) Uani 1 1 d . . .
O1 O 0.8209(3) 0.1229(3) 0.88626(19) 0.0649(6) Uani 1 1 d . . .
O2 O 0.5170(2) 0.1891(2) 0.95620(16) 0.0536(5) Uani 1 1 d . . .
O3 O 0.7164(3) -0.0938(2) 0.93411(17) 0.0594(6) Uani 1 1 d . . .
N1 N 0.6522(3) 0.1047(3) 0.76293(18) 0.0483(6) Uani 1 1 d . . .
N2 N 0.3429(3) 0.4925(3) 0.9189(2) 0.0610(7) Uani 1 1 d . . .
N3 N 0.1310(3) 0.8049(3) 0.9455(2) 0.0673(8) Uani 1 1 d . . .
C1 C 0.5593(3) 0.2565(3) 0.7181(2) 0.0513(7) Uani 1 1 d . . .
C2 C 0.4009(4) 0.2954(4) 0.7222(2) 0.0613(8) Uani 1 1 d . . .
C3 C 0.3126(5) 0.4422(5) 0.6798(3) 0.0771(11) Uani 1 1 d . . .
C4 C 0.3767(5) 0.5462(5) 0.6355(3) 0.0799(11) Uani 1 1 d . . .
C5 C 0.5297(6) 0.5082(4) 0.6309(3) 0.0764(10) Uani 1 1 d . . .
C6 C 0.6256(4) 0.3625(4) 0.6717(3) 0.0640(8) Uani 1 1 d . . .
C7 C 0.3255(4) 0.1839(5) 0.7720(3) 0.0827(11) Uani 1 1 d . . .
H7A H 0.4040 0.0806 0.7634 0.099 Uiso 1 1 calc R . .
H7B H 0.2967 0.1921 0.8445 0.099 Uiso 1 1 calc R . .
C8 C 0.1927(10) 0.1974(11) 0.7393(8) 0.237(6) Uani 1 1 d . . .
H8A H 0.1583 0.1189 0.7778 0.355 Uiso 1 1 calc R . .
H8B H 0.2190 0.1852 0.6683 0.355 Uiso 1 1 calc R . .
H8C H 0.1110 0.2971 0.7498 0.355 Uiso 1 1 calc R . .
C9 C 0.7958(5) 0.3251(6) 0.6649(4) 0.0944(14) Uani 1 1 d . . .
H9A H 0.8038 0.3651 0.7212 0.113 Uiso 1 1 calc R . .
H9B H 0.8495 0.2138 0.6754 0.113 Uiso 1 1 calc R . .
C10 C 0.8783(7) 0.3810(9) 0.5728(4) 0.139(2) Uani 1 1 d . . .
H10A H 0.9839 0.3502 0.5792 0.208 Uiso 1 1 calc R . .
H10B H 0.8292 0.4914 0.5617 0.208 Uiso 1 1 calc R . .
H10C H 0.8769 0.3386 0.5163 0.208 Uiso 1 1 calc R . .
C11 C 0.9541(5) -0.1320(7) 0.6859(4) 0.1127(17) Uani 1 1 d . . .
H11A H 0.9952 -0.0542 0.6620 0.169 Uiso 1 1 calc R . .
H11B H 1.0050 -0.2114 0.6417 0.169 Uiso 1 1 calc R . .
H11C H 0.9719 -0.1758 0.7537 0.169 Uiso 1 1 calc R . .
C12 C 0.6728(8) -0.2018(6) 0.7342(4) 0.125(2) Uani 1 1 d . . .
H12A H 0.5630 -0.1608 0.7358 0.187 Uiso 1 1 calc R . .
H12B H 0.6928 -0.2447 0.8017 0.187 Uiso 1 1 calc R . .
H12C H 0.7258 -0.2809 0.6899 0.187 Uiso 1 1 calc R . .
C14 C 0.2038(4) 0.5308(4) 0.9989(3) 0.0740(10) Uani 1 1 d . . .
H14A H 0.2302 0.5376 1.0606 0.089 Uiso 1 1 calc R . .
H14B H 0.1670 0.4488 1.0132 0.089 Uiso 1 1 calc R . .
C13 C 0.7070(6) 0.0318(6) 0.5563(3) 0.1055(15) Uani 1 1 d . . .
H13A H 0.5972 0.0763 0.5577 0.158 Uiso 1 1 calc R . .
H13B H 0.7569 -0.0503 0.5142 0.158 Uiso 1 1 calc R . .
H13C H 0.7480 0.1093 0.5290 0.158 Uiso 1 1 calc R . .
C15 C 0.0742(4) 0.6823(4) 0.9693(4) 0.0789(11) Uani 1 1 d . . .
H15A H 0.0416 0.6743 0.9104 0.095 Uiso 1 1 calc R . .
H15B H -0.0145 0.7055 1.0250 0.095 Uiso 1 1 calc R . .
C16 C 0.2672(4) 0.7717(4) 0.8636(3) 0.0713(9) Uani 1 1 d . . .
H16A H 0.3045 0.8531 0.8507 0.086 Uiso 1 1 calc R . .
H16B H 0.2394 0.7673 0.8017 0.086 Uiso 1 1 calc R . .
C17 C 0.3935(4) 0.6192(4) 0.8933(3) 0.0623(8) Uani 1 1 d . . .
H17A H 0.4819 0.5962 0.8373 0.075 Uiso 1 1 calc R . .
H17B H 0.4272 0.6280 0.9514 0.075 Uiso 1 1 calc R . .
H3 H 0.203(5) 0.475(5) 0.687(3) 0.101(14) Uiso 1 1 d . . .
H4 H 0.313(5) 0.644(5) 0.610(3) 0.087(12) Uiso 1 1 d . . .
H5 H 0.582(5) 0.572(5) 0.602(3) 0.089(13) Uiso 1 1 d . . .
H2N H 0.325(5) 0.475(5) 0.869(3) 0.077(12) Uiso 1 1 d . . .
H3N H 0.056(5) 0.884(5) 0.929(3) 0.083(12) Uiso 1 1 d . . .
H1O H 0.831(6) 0.141(6) 0.942(4) 0.122(18) Uiso 1 1 d . . .
H2O H 0.468(5) 0.289(6) 0.932(3) 0.098(14) Uiso 1 1 d . . .
H3O H 0.631(6) -0.109(6) 0.961(4) 0.116(17) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.0391(4) 0.0390(5) 0.0538(5) -0.0081(3) -0.0020(3) -0.0139(3)
Si2 0.0648(6) 0.0487(6) 0.0631(6) -0.0181(4) -0.0037(4) -0.0126(4)
O1 0.0564(13) 0.0822(17) 0.0656(14) -0.0173(12) -0.0019(10) -0.0380(12)
O2 0.0510(11) 0.0406(12) 0.0602(12) -0.0106(9) 0.0015(9) -0.0149(9)
O3 0.0494(12) 0.0393(12) 0.0699(13) -0.0013(9) -0.0037(10) -0.0068(9)
N1 0.0453(12) 0.0388(13) 0.0556(13) -0.0076(10) -0.0054(10) -0.0135(10)
N2 0.0610(16) 0.0418(15) 0.0774(18) -0.0164(13) -0.0158(14) -0.0124(12)
N3 0.0578(16) 0.0464(17) 0.090(2) -0.0214(14) -0.0229(15) -0.0023(13)
C1 0.0522(16) 0.0436(17) 0.0520(15) -0.0109(12) -0.0037(12) -0.0147(13)
C2 0.0510(16) 0.062(2) 0.0595(17) -0.0111(14) -0.0103(13) -0.0099(15)
C3 0.063(2) 0.073(3) 0.072(2) -0.0108(19) -0.0137(17) -0.0046(19)
C4 0.083(3) 0.055(2) 0.072(2) -0.0050(18) -0.0211(19) 0.003(2)
C5 0.104(3) 0.050(2) 0.070(2) 0.0038(16) -0.018(2) -0.030(2)
C6 0.070(2) 0.052(2) 0.0666(19) -0.0020(15) -0.0097(15) -0.0256(16)
C7 0.058(2) 0.095(3) 0.095(3) -0.001(2) -0.0175(19) -0.034(2)
C8 0.222(9) 0.238(10) 0.340(13) 0.136(10) -0.198(10) -0.172(9)
C9 0.079(3) 0.095(3) 0.110(3) 0.030(3) -0.022(2) -0.053(2)
C10 0.104(4) 0.193(7) 0.108(4) 0.030(4) -0.014(3) -0.076(4)
C11 0.070(3) 0.119(4) 0.107(4) -0.044(3) -0.004(2) 0.008(3)
C12 0.177(6) 0.079(3) 0.132(4) -0.039(3) 0.003(4) -0.069(4)
C14 0.0577(19) 0.058(2) 0.100(3) -0.0083(19) -0.0058(18) -0.0236(17)
C13 0.127(4) 0.095(3) 0.079(3) -0.033(2) -0.022(3) -0.018(3)
C15 0.0488(17) 0.070(2) 0.116(3) -0.025(2) -0.0139(18) -0.0164(16)
C16 0.079(2) 0.0454(19) 0.081(2) -0.0042(16) -0.0158(18) -0.0189(17)
C17 0.0551(17) 0.0462(18) 0.079(2) -0.0133(15) -0.0042(15) -0.0164(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O3 1.613(2) . ?
Si1 O1 1.616(2) . ?
Si1 O2 1.620(2) . ?
Si1 N1 1.721(2) . ?
Si2 N1 1.746(2) . ?
Si2 C11 1.843(5) . ?
Si2 C13 1.843(5) . ?
Si2 C12 1.858(5) . ?
O1 H1O 0.86(5) . ?
O2 H2O 0.91(5) . ?
O3 H3O 0.87(5) . ?
N1 C1 1.450(4) . ?
N2 C17 1.455(4) . ?
N2 C14 1.462(4) . ?
N2 H2N 0.81(4) . ?
N3 C16 1.458(5) . ?
N3 C15 1.460(5) . ?
N3 H3N 0.84(4) . ?
C1 C6 1.397(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.393(5) . ?
C2 C7 1.507(5) . ?
C3 C4 1.361(6) . ?
C3 H3 0.95(5) . ?
C4 C5 1.356(6) . ?
C4 H4 0.93(4) . ?
C5 C6 1.401(5) . ?
C5 H5 0.93(4) . ?
C6 C9 1.514(5) . ?
C7 C8 1.421(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.441(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 C15 1.520(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.511(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21153112
|
1100821.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-16 04:05:44 +0300 (Mon, 16 Jul 2018) $
#$Revision: 209049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100821.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100821
loop_
_publ_author_name
'Prabusankar, Ganesan'
'Murugavel, Ramaswamy'
'Butcher, Ray J.'
_publ_section_title
;
Synthesis, Spectral Studies, and Structural Characterization of a New
Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic
Aluminosilicate
;
_journal_coden_ASTM JOCEAH
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2124
_journal_page_last 2128
_journal_paper_doi 10.1021/om049254+
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C23 H33 N3 O3 Si2'
_chemical_formula_sum 'C23 H33 N3 O3 Si2'
_chemical_formula_weight 455.70
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 114.812(12)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.8490(16)
_cell_length_b 15.3410(15)
_cell_length_c 13.394(2)
_cell_measurement_temperature 293(2)
_cell_volume 2583.0(5)
_diffrn_ambient_temperature 293(2)
_diffrn_measurement_device_type 'Enraf Nonius TurboCAD4'
_diffrn_measurement_method 'non-profiled omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0348
_diffrn_reflns_av_sigmaI/netI 0.1145
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 6121
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 1.62
_diffrn_standards_decay_% 1
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.164
_exptl_absorpt_correction_T_max 0.9601
_exptl_absorpt_correction_T_min 0.9372
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.172
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 976
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.25
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.998
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 292
_refine_ls_number_reflns 5886
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.998
_refine_ls_R_factor_all 0.1919
_refine_ls_R_factor_gt 0.0612
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1499
_refine_ls_wR_factor_ref 0.1879
_reflns_number_gt 2594
_reflns_number_total 5886
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060453
_cod_depositor_comments
;
Merging entries 1100819-1100822 with entries 4060451-4060454.
Marking entries 1100819-1100822 as duplicates of entries 4060451-4060454.
Antanas Vaitkus,
2018-07-16
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H1 H 0.141(3) 0.485(2) 0.436(3) 0.059(12) Uiso 1 1 d . . .
H2 H 0.046(2) 0.554(2) 0.610(3) 0.039(11) Uiso 1 1 d . . .
H3 H 0.134(3) 0.657(3) 0.447(3) 0.084(16) Uiso 1 1 d . . .
Si1 Si 0.16288(6) 0.56859(6) 0.55959(6) 0.0493(3) Uani 1 1 d . . .
Si2 Si 0.39602(8) 0.61640(9) 0.63974(8) 0.0793(4) Uani 1 1 d . . .
N1 N 0.29331(18) 0.55526(17) 0.64860(18) 0.0545(7) Uani 1 1 d . . .
N2 N -0.0423(3) 0.3342(2) 0.7269(2) 0.0796(9) Uani 1 1 d . . .
N3 N 0.1557(3) 0.4376(2) 1.2938(2) 0.0844(9) Uani 1 1 d . . .
O1 O 0.11303(18) 0.49120(16) 0.46942(19) 0.0597(7) Uani 1 1 d . . .
O2 O 0.0933(2) 0.56895(19) 0.62940(19) 0.0652(8) Uani 1 1 d . . .
O3 O 0.1586(2) 0.66014(18) 0.4996(2) 0.0667(7) Uani 1 1 d . . .
C1 C 0.3185(2) 0.4919(2) 0.7362(3) 0.0606(9) Uani 1 1 d . . .
C2 C 0.3353(3) 0.4046(3) 0.7189(3) 0.0773(11) Uani 1 1 d . . .
C3 C 0.3605(3) 0.3463(3) 0.8067(5) 0.1035(15) Uani 1 1 d . . .
H3A H 0.3696 0.2875 0.7960 0.124 Uiso 1 1 calc R . .
C4 C 0.3721(3) 0.3746(4) 0.9082(5) 0.1059(16) Uani 1 1 d . . .
H4A H 0.3895 0.3349 0.9656 0.127 Uiso 1 1 calc R . .
C5 C 0.3585(3) 0.4594(3) 0.9257(3) 0.0894(13) Uani 1 1 d . . .
H5A H 0.3687 0.4777 0.9957 0.107 Uiso 1 1 calc R . .
C6 C 0.3296(2) 0.5196(3) 0.8411(3) 0.0644(9) Uani 1 1 d . . .
C7 C 0.3887(4) 0.6098(4) 0.4982(4) 0.1124(16) Uani 1 1 d . . .
H7A H 0.3922 0.5498 0.4793 0.169 Uiso 1 1 calc R . .
H7B H 0.4471 0.6413 0.4949 0.169 Uiso 1 1 calc R . .
H7C H 0.3229 0.6348 0.4472 0.169 Uiso 1 1 calc R . .
C8 C 0.5245(3) 0.5679(4) 0.7374(4) 0.129(2) Uani 1 1 d . . .
H8A H 0.5283 0.5083 0.7177 0.194 Uiso 1 1 calc R . .
H8B H 0.5288 0.5705 0.8108 0.194 Uiso 1 1 calc R . .
H8C H 0.5825 0.6001 0.7341 0.194 Uiso 1 1 calc R . .
C9 C 0.3899(4) 0.7323(3) 0.6773(3) 0.1106(16) Uani 1 1 d . . .
H9A H 0.3240 0.7575 0.6269 0.166 Uiso 1 1 calc R . .
H9B H 0.4483 0.7638 0.6738 0.166 Uiso 1 1 calc R . .
H9C H 0.3943 0.7353 0.7507 0.166 Uiso 1 1 calc R . .
C11 C 0.0416(4) 0.3829(3) 0.7749(3) 0.0803(11) Uani 1 1 d . . .
H11 H 0.0725 0.4068 0.7315 0.096 Uiso 1 1 calc R . .
C12 C 0.0878(3) 0.4014(2) 0.8864(3) 0.0729(10) Uani 1 1 d . . .
H12 H 0.1483 0.4360 0.9160 0.087 Uiso 1 1 calc R . .
C13 C 0.0435(3) 0.3682(2) 0.9529(2) 0.0590(8) Uani 1 1 d . . .
C14 C -0.0439(3) 0.3158(3) 0.9033(3) 0.0827(11) Uani 1 1 d . . .
H14 H -0.0761 0.2908 0.9449 0.099 Uiso 1 1 calc R . .
C15 C -0.0837(3) 0.3003(3) 0.7928(3) 0.0905(13) Uani 1 1 d . . .
H15 H -0.1428 0.2642 0.7614 0.109 Uiso 1 1 calc R . .
C16 C 0.1870(3) 0.4790(3) 1.2266(3) 0.0835(12) Uani 1 1 d . . .
H16 H 0.2343 0.5251 1.2545 0.100 Uiso 1 1 calc R . .
C17 C 0.1539(3) 0.4579(3) 1.1177(3) 0.0812(11) Uani 1 1 d . . .
H17 H 0.1784 0.4903 1.0744 0.097 Uiso 1 1 calc R . .
C18 C 0.0856(3) 0.3902(2) 1.0718(2) 0.0582(8) Uani 1 1 d . . .
C19 C 0.0560(4) 0.3467(3) 1.1428(3) 0.1068(16) Uani 1 1 d . . .
H19 H 0.0108 0.2989 1.1178 0.128 Uiso 1 1 calc R . .
C20 C 0.0916(5) 0.3718(4) 1.2508(4) 0.1209(19) Uani 1 1 d . . .
H20 H 0.0688 0.3401 1.2961 0.145 Uiso 1 1 calc R . .
C21 C 0.3306(4) 0.3718(3) 0.6107(4) 0.1013(14) Uani 1 1 d . . .
H21A H 0.3120 0.4202 0.5593 0.122 Uiso 1 1 calc R . .
H21B H 0.4009 0.3519 0.6220 0.122 Uiso 1 1 calc R . .
C22 C 0.2525(5) 0.2991(4) 0.5596(5) 0.164(2) Uani 1 1 d . . .
H22A H 0.2546 0.2820 0.4916 0.245 Uiso 1 1 calc R . .
H22B H 0.1822 0.3186 0.5457 0.245 Uiso 1 1 calc R . .
H22C H 0.2710 0.2502 0.6089 0.245 Uiso 1 1 calc R . .
C61 C 0.3116(3) 0.6127(3) 0.8635(3) 0.0828(11) Uani 1 1 d . . .
H61A H 0.3801 0.6390 0.9075 0.099 Uiso 1 1 calc R . .
H61B H 0.2812 0.6436 0.7940 0.099 Uiso 1 1 calc R . .
C62 C 0.2416(5) 0.6262(3) 0.9205(4) 0.141(2) Uani 1 1 d . . .
H62A H 0.2350 0.6875 0.9307 0.211 Uiso 1 1 calc R . .
H62B H 0.2718 0.5978 0.9909 0.211 Uiso 1 1 calc R . .
H62C H 0.1726 0.6021 0.8770 0.211 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.0421(5) 0.0640(6) 0.0376(4) -0.0055(4) 0.0127(3) -0.0058(4)
Si2 0.0495(6) 0.1206(10) 0.0631(6) 0.0057(6) 0.0188(5) -0.0190(6)
N1 0.0440(14) 0.0709(18) 0.0450(13) 0.0020(13) 0.0151(11) -0.0024(13)
N2 0.101(2) 0.076(2) 0.0520(17) 0.0057(16) 0.0223(17) -0.0002(19)
N3 0.094(2) 0.099(3) 0.0667(19) -0.0201(19) 0.0397(18) -0.009(2)
O1 0.0540(14) 0.0761(17) 0.0517(13) -0.0185(12) 0.0250(12) -0.0124(12)
O2 0.0421(14) 0.105(2) 0.0477(13) -0.0198(13) 0.0178(11) -0.0112(15)
O3 0.0703(16) 0.0691(18) 0.0483(15) 0.0001(13) 0.0127(13) -0.0081(12)
C1 0.0383(16) 0.079(3) 0.0564(19) 0.0054(18) 0.0113(14) -0.0008(16)
C2 0.058(2) 0.079(3) 0.091(3) 0.005(2) 0.027(2) 0.0120(19)
C3 0.082(3) 0.082(3) 0.140(4) 0.034(3) 0.040(3) 0.025(2)
C4 0.084(3) 0.120(5) 0.107(4) 0.058(3) 0.033(3) 0.027(3)
C5 0.075(3) 0.112(4) 0.074(3) 0.029(3) 0.025(2) 0.017(3)
C6 0.0484(19) 0.085(3) 0.0503(19) 0.0090(19) 0.0114(15) 0.0001(17)
C7 0.089(3) 0.179(5) 0.086(3) 0.013(3) 0.053(3) -0.004(3)
C8 0.042(2) 0.216(6) 0.110(3) 0.037(4) 0.013(2) -0.011(3)
C9 0.110(3) 0.111(4) 0.101(3) -0.008(3) 0.034(3) -0.060(3)
C11 0.100(3) 0.089(3) 0.061(2) 0.006(2) 0.044(2) -0.004(2)
C12 0.076(2) 0.088(3) 0.059(2) 0.0027(19) 0.0314(19) -0.013(2)
C13 0.069(2) 0.058(2) 0.0506(18) 0.0049(16) 0.0248(17) 0.0032(17)
C14 0.100(3) 0.092(3) 0.054(2) 0.000(2) 0.030(2) -0.026(2)
C15 0.106(3) 0.091(3) 0.061(2) -0.006(2) 0.022(2) -0.034(3)
C16 0.073(3) 0.105(3) 0.070(2) -0.023(2) 0.028(2) -0.023(2)
C17 0.084(3) 0.102(3) 0.060(2) -0.009(2) 0.033(2) -0.024(2)
C18 0.063(2) 0.062(2) 0.0507(18) -0.0026(16) 0.0246(16) 0.0005(17)
C19 0.151(4) 0.117(4) 0.070(3) -0.030(2) 0.063(3) -0.066(3)
C20 0.180(5) 0.133(4) 0.069(3) -0.031(3) 0.071(3) -0.067(4)
C21 0.088(3) 0.092(3) 0.114(4) -0.013(3) 0.033(3) 0.019(3)
C22 0.192(6) 0.102(4) 0.156(5) -0.022(4) 0.033(5) -0.013(4)
C61 0.093(3) 0.097(3) 0.050(2) -0.004(2) 0.022(2) -0.015(2)
C62 0.235(7) 0.099(4) 0.141(5) -0.011(3) 0.131(5) -0.008(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O2 1.600(3) . ?
Si1 O3 1.607(3) . ?
Si1 O1 1.626(2) . ?
Si1 N1 1.708(2) . ?
Si1 H3 1.94(4) . ?
Si2 N1 1.749(3) . ?
Si2 C7 1.859(4) . ?
Si2 C9 1.859(5) . ?
Si2 C8 1.864(4) . ?
N1 C1 1.449(4) . ?
N2 C11 1.302(5) . ?
N2 C15 1.341(5) . ?
N3 C20 1.308(5) . ?
N3 C16 1.315(5) . ?
O1 H1 0.71(3) . ?
O2 H2 0.64(3) . ?
O3 H3 0.64(4) . ?
C1 C2 1.396(5) . ?
C1 C6 1.413(4) . ?
C2 C3 1.400(6) . ?
C2 C21 1.508(6) . ?
C3 C4 1.371(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.349(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.385(5) . ?
C5 H5A 0.9300 . ?
C6 C61 1.501(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 C12 1.384(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(5) . ?
C13 C18 1.487(4) . ?
C14 C15 1.367(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.371(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.365(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.358(5) . ?
C19 C20 1.373(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.504(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C61 C62 1.478(6) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21153113
|
1100822.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-16 04:05:44 +0300 (Mon, 16 Jul 2018) $
#$Revision: 209049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100822.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100822
loop_
_publ_author_name
'Prabusankar, Ganesan'
'Murugavel, Ramaswamy'
'Butcher, Ray J.'
_publ_section_title
;
Synthesis, Spectral Studies, and Structural Characterization of a New
Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic
Aluminosilicate
;
_journal_coden_ASTM JOCEAH
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2124
_journal_page_last 2128
_journal_paper_doi 10.1021/om049254+
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C20 H20 Al1 N1 O3 Si2'
_chemical_formula_sum 'C40 H72 Al2 N6 O7 Si4'
_chemical_formula_weight 915.36
_space_group_IT_number 80
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I 4bw'
_symmetry_space_group_name_H-M 'I 41'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 14.4980(17)
_cell_length_b 14.4980(17)
_cell_length_c 52.767(3)
_cell_measurement_reflns_used 0
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 0
_cell_measurement_theta_min 0
_cell_volume 11091.2(19)
_diffrn_ambient_temperature 293(2)
_diffrn_measurement_device_type 'Enraf Nonius TurboCAD4'
_diffrn_measurement_method 'non-profiled omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1155
_diffrn_reflns_av_sigmaI/netI 0.2538
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -62
_diffrn_reflns_number 5313
_diffrn_reflns_theta_max 24.97
_diffrn_reflns_theta_min 1.54
_diffrn_standards_decay_% 29
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.184
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.096
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 3936
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.25
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 532
_refine_ls_number_reflns 4907
_refine_ls_number_restraints 109
_refine_ls_restrained_S_all 1.052
_refine_ls_R_factor_all 0.3304
_refine_ls_R_factor_gt 0.1155
_refine_ls_shift/su_max 0.026
_refine_ls_shift/su_mean 0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2932
_refine_ls_wR_factor_ref 0.3987
_reflns_number_gt 1769
_reflns_number_total 4907
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060454
_cod_depositor_comments
;
Merging entries 1100819-1100822 with entries 4060451-4060454.
Marking entries 1100819-1100822 as duplicates of entries 4060451-4060454.
Antanas Vaitkus,
2018-07-16
;
_cod_database_code 1100822
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.1278(5) 0.0681(5) 0.91725(16) 0.049(2) Uani 1 1 d . . .
Al2 Al 0.0713(5) -0.1295(6) 0.86022(19) 0.055(2) Uani 1 1 d . . .
Si1 Si 0.1433(5) 0.0743(5) 0.85801(17) 0.052(2) Uani 1 1 d . . .
Si2 Si 0.3391(5) 0.0989(6) 0.83641(17) 0.059(2) Uani 1 1 d . . .
Si3 Si -0.0719(5) 0.1400(5) 0.91872(17) 0.0469(19) Uani 1 1 d . . .
Si4 Si -0.0908(7) 0.3414(6) 0.9383(2) 0.086(3) Uani 1 1 d . . .
N1 N 0.2219(12) 0.1271(11) 0.8388(4) 0.036(4) Uani 1 1 d . . .
N2 N -0.124(2) 0.2302(18) 0.9390(5) 0.087(8) Uani 1 1 d . . .
N3 N 0.2243(13) 0.1175(16) 0.9399(4) 0.054(6) Uani 1 1 d . . .
N4 N 0.353(3) 0.174(3) 0.9728(7) 0.115(11) Uani 1 1 d . . .
N5 N 0.1108(15) -0.2327(17) 0.8372(6) 0.076(8) Uani 1 1 d . . .
N6 N 0.163(2) -0.361(3) 0.8102(7) 0.106(10) Uani 1 1 d U . .
O1 O 0.1748(12) 0.0930(11) 0.8870(4) 0.063(5) Uani 1 1 d . . .
O2 O 0.1380(10) -0.0379(10) 0.8521(3) 0.048(4) Uani 1 1 d . . .
O3 O 0.0447(13) 0.1232(16) 0.8516(4) 0.088(7) Uani 1 1 d . . .
O4 O 0.0351(13) 0.1348(13) 0.9252(4) 0.076(6) Uani 1 1 d . . .
O5 O 0.1173(9) -0.0438(10) 0.9246(3) 0.040(4) Uani 1 1 d . . .
O6 O -0.0841(12) 0.1702(10) 0.8896(4) 0.057(5) Uani 1 1 d . . .
C1 C 0.1971(16) 0.2086(18) 0.8235(4) 0.061(8) Uani 1 1 d DU . .
C2 C 0.1690(18) 0.1976(17) 0.7997(4) 0.112(15) Uani 1 1 d D . .
C3 C 0.150(2) 0.268(2) 0.7847(6) 0.14(2) Uani 1 1 d D . .
H3 H 0.1319 0.2585 0.7680 0.174 Uiso 1 1 calc R . .
C4 C 0.156(2) 0.353(2) 0.7939(7) 0.19(3) Uani 1 1 d DU . .
H4 H 0.1373 0.4022 0.7839 0.231 Uiso 1 1 calc R . .
C5 C 0.189(2) 0.3701(19) 0.8168(6) 0.110(15) Uani 1 1 d D . .
H5 H 0.2019 0.4295 0.8224 0.132 Uiso 1 1 calc R . .
C6 C 0.203(2) 0.2957(16) 0.8311(7) 0.114(16) Uani 1 1 d DU . .
C7 C 0.163(4) 0.111(5) 0.7897(7) 0.21(3) Uani 1 1 d . . .
H7A H 0.1205 0.0782 0.8009 0.250 Uiso 1 1 calc R . .
H7B H 0.2227 0.0833 0.7925 0.250 Uiso 1 1 calc R . .
C8 C 0.135(3) 0.080(5) 0.7633(7) 0.22(3) Uani 1 1 d . . .
H8A H 0.1498 0.0159 0.7612 0.333 Uiso 1 1 calc R . .
H8B H 0.1691 0.1157 0.7510 0.333 Uiso 1 1 calc R . .
H8C H 0.0705 0.0895 0.7609 0.333 Uiso 1 1 calc R . .
C9 C 0.241(3) 0.321(3) 0.8562(12) 0.16(2) Uani 1 1 d . . .
H9A H 0.2481 0.2641 0.8655 0.197 Uiso 1 1 calc R . .
H9B H 0.3021 0.3451 0.8532 0.197 Uiso 1 1 calc R . .
C10 C 0.201(4) 0.379(2) 0.8719(12) 0.27(4) Uani 1 1 d . . .
H10A H 0.2381 0.3866 0.8867 0.406 Uiso 1 1 calc R . .
H10B H 0.1411 0.3559 0.8766 0.406 Uiso 1 1 calc R . .
H10C H 0.1933 0.4380 0.8637 0.406 Uiso 1 1 calc R . .
C11 C 0.389(2) 0.166(3) 0.8101(7) 0.103(12) Uani 1 1 d . . .
H11A H 0.3573 0.1515 0.7946 0.154 Uiso 1 1 calc R . .
H11B H 0.4533 0.1509 0.8083 0.154 Uiso 1 1 calc R . .
H11C H 0.3830 0.2308 0.8136 0.154 Uiso 1 1 calc R . .
C12 C 0.3853(18) 0.113(4) 0.8677(6) 0.16(2) Uani 1 1 d . . .
H12A H 0.3563 0.0693 0.8790 0.240 Uiso 1 1 calc R . .
H12B H 0.3739 0.1742 0.8736 0.240 Uiso 1 1 calc R . .
H12C H 0.4506 0.1013 0.8674 0.240 Uiso 1 1 calc R . .
C13 C 0.350(3) -0.037(2) 0.8306(10) 0.16(2) Uani 1 1 d . . .
H13A H 0.3223 -0.0693 0.8445 0.243 Uiso 1 1 calc R . .
H13B H 0.4140 -0.0533 0.8294 0.243 Uiso 1 1 calc R . .
H13C H 0.3191 -0.0529 0.8151 0.243 Uiso 1 1 calc R . .
C21 C -0.2028(19) 0.1982(18) 0.9547(6) 0.105(15) Uani 1 1 d DU . .
C22 C -0.2883(18) 0.2076(18) 0.9461(5) 0.106(15) Uani 1 1 d D . .
C23 C -0.356(2) 0.180(3) 0.9614(6) 0.25(3) Uani 1 1 d DU . .
H23 H -0.4156 0.1845 0.9552 0.304 Uiso 1 1 calc R . .
C24 C -0.345(3) 0.146(3) 0.9845(6) 0.41(9) Uani 1 1 d D . .
H24 H -0.3942 0.1278 0.9949 0.488 Uiso 1 1 calc R . .
C25 C -0.258(3) 0.141(2) 0.9912(8) 0.51(12) Uani 1 1 d D . .
H25 H -0.2457 0.1248 1.0079 0.609 Uiso 1 1 calc R . .
C26 C -0.185(3) 0.157(2) 0.9767(6) 0.14(2) Uani 1 1 d D . .
C27 C -0.306(2) 0.235(3) 0.9160(8) 0.124(16) Uani 1 1 d . . .
H27A H -0.3477 0.2871 0.9152 0.149 Uiso 1 1 calc R . .
H27B H -0.2479 0.2538 0.9085 0.149 Uiso 1 1 calc R . .
C28 C -0.345(2) 0.160(2) 0.9006(6) 0.110(11) Uani 1 1 d . . .
H28A H -0.3533 0.1811 0.8835 0.165 Uiso 1 1 calc R . .
H28B H -0.4032 0.1415 0.9075 0.165 Uiso 1 1 calc R . .
H28C H -0.3033 0.1084 0.9007 0.165 Uiso 1 1 calc R . .
C29 C -0.088(2) 0.145(3) 0.9856(9) 0.111(15) Uani 1 1 d . . .
H29A H -0.0498 0.1284 0.9713 0.134 Uiso 1 1 calc R . .
H29B H -0.0657 0.2038 0.9921 0.134 Uiso 1 1 calc R . .
C30 C -0.079(5) 0.079(3) 1.0042(16) 0.27(4) Uani 1 1 d . . .
H30A H -0.0155 0.0732 1.0089 0.399 Uiso 1 1 calc R . .
H30B H -0.1015 0.0211 0.9980 0.399 Uiso 1 1 calc R . .
H30C H -0.1145 0.0970 1.0188 0.399 Uiso 1 1 calc R . .
C31 C -0.119(3) 0.4136(17) 0.9076(8) 0.117(13) Uani 1 1 d U . .
H31A H -0.1839 0.4133 0.9046 0.176 Uiso 1 1 calc R . .
H31B H -0.0874 0.3868 0.8933 0.176 Uiso 1 1 calc R . .
H31C H -0.0978 0.4760 0.9099 0.176 Uiso 1 1 calc R . .
C32 C 0.023(2) 0.3506(18) 0.9461(10) 0.135(18) Uani 1 1 d . . .
H32A H 0.0597 0.3202 0.9334 0.202 Uiso 1 1 calc R . .
H32B H 0.0337 0.3223 0.9622 0.202 Uiso 1 1 calc R . .
H32C H 0.0400 0.4146 0.9469 0.202 Uiso 1 1 calc R . .
C33 C -0.155(3) 0.406(3) 0.9619(9) 0.16(2) Uani 1 1 d . . .
H33A H -0.2195 0.3964 0.9594 0.247 Uiso 1 1 calc R . .
H33B H -0.1404 0.4700 0.9604 0.247 Uiso 1 1 calc R . .
H33C H -0.1378 0.3843 0.9785 0.247 Uiso 1 1 calc R . .
C41 C 0.275(3) 0.206(2) 0.9296(8) 0.141(18) Uani 1 1 d . . .
H41A H 0.3160 0.1920 0.9156 0.169 Uiso 1 1 calc R . .
H41B H 0.2319 0.2537 0.9244 0.169 Uiso 1 1 calc R . .
C42 C 0.330(3) 0.236(2) 0.9533(10) 0.134(16) Uani 1 1 d U . .
H42A H 0.3871 0.2621 0.9474 0.161 Uiso 1 1 calc R . .
H42B H 0.2952 0.2855 0.9611 0.161 Uiso 1 1 calc R . .
C43 C 0.1955(19) 0.1216(17) 0.9655(5) 0.060(7) Uani 1 1 d . . .
H43A H 0.1719 0.0615 0.9703 0.073 Uiso 1 1 calc R . .
H43B H 0.1449 0.1652 0.9668 0.073 Uiso 1 1 calc R . .
C44 C 0.271(2) 0.150(3) 0.9851(7) 0.097(12) Uani 1 1 d . . .
H44A H 0.2497 0.2021 0.9950 0.117 Uiso 1 1 calc R . .
H44B H 0.2831 0.0993 0.9966 0.117 Uiso 1 1 calc R . .
C45 C 0.3055(19) 0.055(2) 0.9375(6) 0.087(11) Uani 1 1 d U . .
H45A H 0.3255 0.0512 0.9200 0.104 Uiso 1 1 calc R . .
H45B H 0.2894 -0.0070 0.9431 0.104 Uiso 1 1 calc R . .
C46 C 0.3844(18) 0.096(3) 0.9546(9) 0.126(16) Uani 1 1 d U . .
H46A H 0.4109 0.0463 0.9646 0.151 Uiso 1 1 calc R . .
H46B H 0.4327 0.1196 0.9436 0.151 Uiso 1 1 calc R . .
C51 C 0.100(2) -0.192(3) 0.8080(7) 0.115(15) Uani 1 1 d . . .
H51A H 0.0365 -0.1802 0.8037 0.138 Uiso 1 1 calc R . .
H51B H 0.1366 -0.1367 0.8055 0.138 Uiso 1 1 calc R . .
C52 C 0.140(4) -0.274(4) 0.7928(9) 0.19(3) Uani 1 1 d U . .
H52A H 0.1952 -0.2542 0.7841 0.227 Uiso 1 1 calc R . .
H52B H 0.0951 -0.2921 0.7800 0.227 Uiso 1 1 calc R . .
C53 C 0.0487(18) -0.3110(19) 0.8377(6) 0.077(10) Uani 1 1 d . . .
H53A H -0.0102 -0.2923 0.8306 0.092 Uiso 1 1 calc R . .
H53B H 0.0384 -0.3289 0.8552 0.092 Uiso 1 1 calc R . .
C54 C 0.084(2) -0.396(3) 0.8228(10) 0.17(2) Uani 1 1 d . . .
H54A H 0.1007 -0.4460 0.8341 0.204 Uiso 1 1 calc R . .
H54B H 0.0386 -0.4177 0.8108 0.204 Uiso 1 1 calc R . .
C55 C 0.2114(15) -0.2555(14) 0.8433(5) 0.053(7) Uani 1 1 d U . .
H55A H 0.2171 -0.2648 0.8614 0.063 Uiso 1 1 calc R . .
H55B H 0.2494 -0.2030 0.8388 0.063 Uiso 1 1 calc R . .
C56 C 0.251(4) -0.346(3) 0.8289(11) 0.19(3) Uani 1 1 d . . .
H56A H 0.2598 -0.3974 0.8403 0.223 Uiso 1 1 calc R . .
H56B H 0.3072 -0.3333 0.8197 0.223 Uiso 1 1 calc R . .
O101 O 0.065(3) 0.433(4) 0.7321(7) 0.214(18) Uani 1 1 d U . .
C102 C 0.067(5) 0.527(4) 0.7436(10) 0.21(3) Uani 1 1 d U . .
H10D H 0.0403 0.5227 0.7604 0.255 Uiso 1 1 calc R . .
H10E H 0.1314 0.5438 0.7457 0.255 Uiso 1 1 calc R . .
C103 C -0.032(5) 0.417(2) 0.7332(10) 0.17(2) Uani 1 1 d U . .
H10F H -0.0566 0.4137 0.7161 0.198 Uiso 1 1 calc R . .
H10G H -0.0442 0.3591 0.7416 0.198 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.046(5) 0.047(5) 0.054(5) -0.007(4) -0.012(4) 0.009(4)
Al2 0.038(5) 0.046(5) 0.082(6) 0.004(4) -0.005(4) 0.018(4)
Si1 0.042(4) 0.048(5) 0.065(5) 0.014(4) -0.007(4) 0.004(3)
Si2 0.048(5) 0.070(5) 0.059(4) 0.001(4) -0.001(4) -0.004(4)
Si3 0.040(4) 0.036(4) 0.065(5) -0.012(4) -0.008(3) 0.005(3)
Si4 0.083(7) 0.050(5) 0.125(8) -0.024(5) 0.035(6) -0.020(5)
N1 0.033(10) 0.025(9) 0.051(11) 0.006(8) 0.009(9) 0.010(8)
N2 0.12(2) 0.061(16) 0.076(17) -0.007(13) 0.013(16) -0.002(16)
N3 0.030(11) 0.083(17) 0.051(12) -0.029(11) -0.023(9) 0.022(10)
N4 0.14(3) 0.11(3) 0.10(2) -0.03(2) -0.04(2) 0.01(2)
N5 0.036(12) 0.063(16) 0.13(2) 0.002(15) -0.018(13) 0.015(11)
N6 0.08(2) 0.12(2) 0.12(2) -0.05(2) 0.006(19) 0.029(19)
O1 0.058(11) 0.057(11) 0.075(13) 0.023(10) -0.008(10) 0.021(8)
O2 0.031(8) 0.033(9) 0.079(11) -0.005(8) -0.021(8) 0.007(7)
O3 0.047(12) 0.124(18) 0.093(15) 0.032(13) -0.013(11) 0.016(12)
O4 0.075(14) 0.072(13) 0.082(13) -0.049(10) 0.009(11) 0.020(10)
O5 0.031(8) 0.053(10) 0.035(8) 0.009(7) 0.004(6) 0.007(7)
O6 0.072(12) 0.035(9) 0.064(11) -0.017(9) -0.008(9) 0.023(8)
C1 0.050(16) 0.08(2) 0.056(16) 0.011(14) 0.016(13) -0.017(15)
C2 0.24(4) 0.052(18) 0.048(18) 0.004(14) 0.04(2) 0.06(2)
C3 0.17(4) 0.11(3) 0.15(3) 0.11(3) 0.08(3) 0.07(3)
C4 0.11(3) 0.19(4) 0.28(6) 0.22(5) 0.11(4) 0.08(3)
C5 0.08(2) 0.062(19) 0.18(4) 0.09(2) 0.08(2) 0.018(16)
C6 0.10(3) 0.05(2) 0.19(4) 0.00(3) 0.07(3) 0.039(19)
C7 0.22(6) 0.35(9) 0.05(2) -0.03(4) -0.04(3) 0.14(6)
C8 0.16(5) 0.42(9) 0.09(3) -0.07(4) 0.02(3) -0.10(5)
C9 0.15(4) 0.09(3) 0.26(6) 0.04(3) 0.10(4) 0.10(3)
C10 0.32(7) 0.07(3) 0.43(9) -0.11(4) 0.29(7) -0.08(3)
C11 0.051(18) 0.11(3) 0.15(3) 0.06(2) 0.018(18) -0.009(18)
C12 0.021(15) 0.38(7) 0.08(2) -0.06(3) -0.028(14) 0.03(2)
C13 0.23(5) 0.05(2) 0.21(5) -0.02(2) -0.09(4) 0.01(2)
C21 0.08(2) 0.07(2) 0.17(4) -0.07(2) 0.08(2) -0.055(19)
C22 0.07(2) 0.08(2) 0.16(3) 0.05(2) 0.10(2) 0.034(18)
C23 0.04(2) 0.23(6) 0.49(9) -0.02(6) 0.05(4) -0.05(3)
C24 0.84(19) 0.16(6) 0.22(7) -0.10(5) 0.40(11) -0.25(9)
C25 1.4(4) 0.02(2) 0.06(3) 0.000(18) -0.04(9) -0.02(7)
C26 0.25(6) 0.042(18) 0.12(3) 0.039(19) 0.13(3) 0.01(2)
C27 0.07(2) 0.15(4) 0.16(3) -0.04(3) -0.03(2) 0.07(2)
C28 0.059(19) 0.16(3) 0.11(2) -0.04(2) 0.031(17) 0.016(19)
C29 0.041(17) 0.11(3) 0.18(4) 0.04(3) -0.01(2) 0.016(18)
C30 0.29(8) 0.08(3) 0.43(12) 0.00(5) -0.02(8) -0.01(4)
C31 0.16(3) 0.014(13) 0.18(3) 0.014(16) -0.03(2) 0.003(15)
C32 0.07(2) 0.033(15) 0.30(6) -0.04(2) -0.01(3) -0.019(15)
C33 0.21(5) 0.09(3) 0.19(4) -0.09(3) 0.12(4) -0.07(3)
C41 0.21(4) 0.035(17) 0.18(4) -0.04(2) -0.09(3) 0.03(2)
C42 0.13(3) 0.06(2) 0.21(4) -0.05(2) 0.01(3) -0.08(2)
C43 0.067(17) 0.039(14) 0.076(19) 0.022(12) 0.002(13) -0.014(12)
C44 0.06(2) 0.12(3) 0.11(3) 0.03(2) -0.032(18) -0.038(19)
C45 0.052(18) 0.10(2) 0.11(2) 0.031(19) 0.030(17) 0.036(16)
C46 0.015(13) 0.15(3) 0.21(4) 0.01(3) 0.005(19) -0.022(18)
C51 0.07(2) 0.18(4) 0.09(2) -0.02(3) 0.044(19) -0.05(2)
C52 0.20(5) 0.27(6) 0.09(3) -0.06(4) 0.10(3) -0.09(4)
C53 0.051(17) 0.066(18) 0.11(2) -0.061(17) 0.004(16) -0.001(14)
C54 0.06(2) 0.17(4) 0.28(5) -0.18(4) 0.06(3) -0.03(2)
C55 0.051(15) 0.026(11) 0.081(16) -0.004(10) -0.028(13) 0.026(10)
C56 0.19(5) 0.13(4) 0.24(6) -0.14(4) 0.07(4) -0.04(3)
O101 0.13(2) 0.30(5) 0.21(3) -0.06(3) 0.02(2) 0.08(3)
C102 0.33(6) 0.14(4) 0.17(4) -0.02(3) -0.19(4) -0.01(4)
C103 0.28(6) 0.05(2) 0.17(4) 0.02(2) 0.03(4) -0.02(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O5 1.676(16) . ?
Al1 O4 1.709(18) . ?
Al1 O1 1.77(2) . ?
Al1 N3 1.97(2) . ?
Al2 O6 1.67(2) 6_444 ?
Al2 O2 1.698(17) . ?
Al2 O3 1.75(2) 6_444 ?
Al2 N5 2.01(3) . ?
Si1 O1 1.62(2) . ?
Si1 O3 1.631(19) . ?
Si1 O2 1.659(16) . ?
Si1 N1 1.705(19) . ?
Si2 N1 1.753(18) . ?
Si2 C12 1.79(3) . ?
Si2 C11 1.85(3) . ?
Si2 C13 2.00(3) . ?
Si3 O5 1.573(16) 6_444 ?
Si3 O4 1.59(2) . ?
Si3 O6 1.61(2) . ?
Si3 N2 1.85(3) . ?
Si4 N2 1.68(3) . ?
Si4 C32 1.71(3) . ?
Si4 C33 1.81(4) . ?
Si4 C31 1.97(4) . ?
N1 C1 1.47(3) . ?
N2 C21 1.48(4) . ?
N3 C43 1.42(3) . ?
N3 C45 1.49(3) . ?
N3 C41 1.58(4) . ?
N4 C42 1.40(5) . ?
N4 C44 1.39(5) . ?
N4 C46 1.56(5) . ?
N5 C53 1.45(3) . ?
N5 C55 1.53(3) . ?
N5 C51 1.65(4) . ?
N6 C54 1.42(5) . ?
N6 C52 1.60(7) . ?
N6 C56 1.62(6) . ?
O3 Al2 1.75(2) 6_444 ?
O5 Si3 1.573(16) 6_444 ?
O6 Al2 1.67(2) 6_444 ?
C1 C6 1.327(10) . ?
C1 C2 1.331(10) . ?
C2 C3 1.325(10) . ?
C2 C7 1.37(6) . ?
C3 C4 1.323(10) . ?
C4 C5 1.322(10) . ?
C5 C6 1.331(10) . ?
C6 C9 1.48(7) . ?
C7 C8 1.51(5) . ?
C9 C10 1.31(5) . ?
C21 C22 1.327(10) . ?
C21 C26 1.329(10) . ?
C22 C23 1.329(10) . ?
C22 C27 1.66(5) . ?
C23 C24 1.325(10) . ?
C24 C25 1.322(11) . ?
C25 C26 1.323(10) . ?
C26 C29 1.49(5) . ?
C27 C28 1.47(5) . ?
C29 C30 1.38(7) . ?
C41 C42 1.54(6) . ?
C43 C44 1.56(4) . ?
C45 C46 1.57(5) . ?
C51 C52 1.54(6) . ?
C53 C54 1.55(4) . ?
C55 C56 1.62(4) . ?
O101 C103 1.42(6) . ?
O101 C102 1.49(5) . ?
C102 C103 1.10(5) 6_454 ?
C103 C102 1.10(5) 6_454 ?
|
1100823.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100823.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100823
loop_
_publ_author_name
'Evans, William J.'
'Kozimor, Stosh A.'
'Brady, Jason C.'
'Davis, Benjamin L.'
'Nyce, Gregory W.'
'Seibel, Christopher A.'
'Ziller, Joseph W.'
'Doedens, Robert J.'
_publ_section_title
;
Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to
Cyclopentadienyl Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2269
_journal_page_last 2278
_journal_paper_doi 10.1021/om049286x
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C31 H51 Si2 Y'
_chemical_formula_weight 568.81
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.0582(5)
_cell_length_b 10.9779(6)
_cell_length_c 28.1698(15)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 163(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 3110.5(3)
_diffrn_ambient_temperature 163(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0770
_diffrn_reflns_av_sigmaI/netI 0.0795
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 36
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_number 33375
_diffrn_reflns_theta_max 28.29
_diffrn_reflns_theta_min 1.45
_diffrn_standards_decay_% '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_interval_time ?
_diffrn_standards_number '50 frames'
_exptl_absorpt_coefficient_mu 1.969
_exptl_absorpt_correction_T_max 0.8275
_exptl_absorpt_correction_T_min 0.6942
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.215
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 1216
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.008(5)
_refine_ls_extinction_coef 0.0006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 308
_refine_ls_number_reflns 7602
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.024
_refine_ls_R_factor_all 0.0681
_refine_ls_R_factor_gt 0.0426
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0861
_refine_ls_wR_factor_ref 0.0968
_reflns_number_gt 6043
_reflns_number_total 7602
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M P2(1)2(1)2(1)
_cod_database_code 1100823
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.70514(3) 0.61192(3) 0.148960(11) 0.01908(9) Uani 1 1 d . . .
Si1 Si 1.01992(9) 0.83802(10) 0.14040(4) 0.0260(2) Uani 1 1 d . . .
Si2 Si 0.46653(10) 0.35318(10) 0.09749(4) 0.0272(2) Uani 1 1 d . . .
C1 C 0.7385(3) 0.8499(3) 0.16628(12) 0.0226(8) Uani 1 1 d . . .
C2 C 0.6117(3) 0.8434(3) 0.14485(13) 0.0208(7) Uani 1 1 d . . .
C3 C 0.6289(3) 0.8040(3) 0.09751(13) 0.0209(8) Uani 1 1 d . . .
C4 C 0.7655(3) 0.7893(3) 0.08833(12) 0.0196(8) Uani 1 1 d . . .
C5 C 0.8376(3) 0.8144(3) 0.13141(12) 0.0204(8) Uani 1 1 d . . .
C6 C 0.7663(3) 0.9033(4) 0.21461(12) 0.0312(9) Uani 1 1 d . . .
H6A H 0.7746 0.9920 0.2120 0.047 Uiso 1 1 calc R . .
H6B H 0.8493 0.8692 0.2271 0.047 Uiso 1 1 calc R . .
H6C H 0.6930 0.8833 0.2362 0.047 Uiso 1 1 calc R . .
C7 C 0.4818(3) 0.8847(4) 0.16642(13) 0.0294(8) Uani 1 1 d . . .
H7A H 0.4696 0.9719 0.1605 0.044 Uiso 1 1 calc R . .
H7B H 0.4833 0.8697 0.2007 0.044 Uiso 1 1 calc R . .
H7C H 0.4083 0.8392 0.1520 0.044 Uiso 1 1 calc R . .
C8 C 0.5193(4) 0.7952(4) 0.06064(13) 0.0288(9) Uani 1 1 d . . .
H8A H 0.5063 0.8749 0.0457 0.043 Uiso 1 1 calc R . .
H8B H 0.4365 0.7695 0.0760 0.043 Uiso 1 1 calc R . .
H8C H 0.5443 0.7354 0.0364 0.043 Uiso 1 1 calc R . .
C9 C 0.8253(3) 0.7728(3) 0.03951(12) 0.0255(8) Uani 1 1 d . . .
H9A H 0.8376 0.8526 0.0246 0.038 Uiso 1 1 calc R . .
H9B H 0.7655 0.7232 0.0200 0.038 Uiso 1 1 calc R . .
H9C H 0.9115 0.7318 0.0423 0.038 Uiso 1 1 calc R . .
C10 C 1.1212(3) 0.8181(4) 0.08543(14) 0.0336(9) Uani 1 1 d . . .
H10A H 1.1108 0.7347 0.0736 0.050 Uiso 1 1 calc R . .
H10B H 1.2151 0.8333 0.0927 0.050 Uiso 1 1 calc R . .
H10C H 1.0910 0.8758 0.0612 0.050 Uiso 1 1 calc R . .
C11 C 1.0891(4) 0.7336(4) 0.18690(15) 0.0415(11) Uani 1 1 d . . .
H11A H 1.0743 0.6488 0.1774 0.062 Uiso 1 1 calc R . .
H11B H 1.0445 0.7490 0.2172 0.062 Uiso 1 1 calc R . .
H11C H 1.1847 0.7483 0.1904 0.062 Uiso 1 1 calc R . .
C12 C 1.0489(4) 1.0015(4) 0.15879(14) 0.0354(10) Uani 1 1 d . . .
H12A H 1.0173 1.0136 0.1917 0.043 Uiso 1 1 calc R . .
H12B H 1.1453 1.0196 0.1579 0.043 Uiso 1 1 calc R . .
C13 C 0.9765(4) 1.0871(4) 0.12620(15) 0.0402(11) Uani 1 1 d . . .
H13A H 0.8856 1.1024 0.1331 0.048 Uiso 1 1 calc R . .
C14 C 1.0271(5) 1.1429(4) 0.08911(17) 0.0543(13) Uani 1 1 d . . .
H14A H 1.1176 1.1305 0.0808 0.065 Uiso 1 1 calc R . .
H14B H 0.9731 1.1956 0.0706 0.065 Uiso 1 1 calc R . .
C15 C 0.7333(3) 0.4503(3) 0.07945(13) 0.0230(8) Uani 1 1 d . . .
C16 C 0.8602(3) 0.4556(3) 0.10128(14) 0.0237(8) Uani 1 1 d . . .
C17 C 0.8497(3) 0.4058(3) 0.14723(13) 0.0231(8) Uani 1 1 d . . .
C18 C 0.7168(3) 0.3659(3) 0.15471(12) 0.0234(7) Uani 1 1 d . . .
C19 C 0.6418(3) 0.3962(4) 0.11294(12) 0.0209(7) Uani 1 1 d . . .
C20 C 0.7048(4) 0.4756(3) 0.02799(12) 0.0290(8) Uani 1 1 d . . .
H20A H 0.7228 0.4023 0.0092 0.043 Uiso 1 1 calc R . .
H20B H 0.7617 0.5423 0.0169 0.043 Uiso 1 1 calc R . .
H20C H 0.6112 0.4988 0.0243 0.043 Uiso 1 1 calc R . .
C21 C 0.9902(3) 0.4870(4) 0.07732(14) 0.0300(9) Uani 1 1 d . . .
H21A H 1.0271 0.4139 0.0623 0.045 Uiso 1 1 calc R . .
H21B H 1.0531 0.5180 0.1010 0.045 Uiso 1 1 calc R . .
H21C H 0.9747 0.5495 0.0531 0.045 Uiso 1 1 calc R . .
C22 C 0.9648(3) 0.3857(4) 0.18157(13) 0.0336(9) Uani 1 1 d . . .
H22A H 1.0052 0.3060 0.1755 0.050 Uiso 1 1 calc R . .
H22B H 0.9316 0.3885 0.2143 0.050 Uiso 1 1 calc R . .
H22C H 1.0315 0.4497 0.1770 0.050 Uiso 1 1 calc R . .
C23 C 0.6719(4) 0.2911(4) 0.19583(14) 0.0312(9) Uani 1 1 d . . .
H23A H 0.6868 0.2046 0.1889 0.047 Uiso 1 1 calc R . .
H23B H 0.5769 0.3051 0.2014 0.047 Uiso 1 1 calc R . .
H23C H 0.7224 0.3142 0.2242 0.047 Uiso 1 1 calc R . .
C24 C 0.3678(4) 0.4886(4) 0.07636(17) 0.0484(12) Uani 1 1 d . . .
H24A H 0.3649 0.5503 0.1015 0.073 Uiso 1 1 calc R . .
H24B H 0.2771 0.4628 0.0686 0.073 Uiso 1 1 calc R . .
H24C H 0.4101 0.5231 0.0481 0.073 Uiso 1 1 calc R . .
C25 C 0.3697(4) 0.2852(4) 0.14719(16) 0.0388(10) Uani 1 1 d . . .
H25A H 0.4166 0.2135 0.1594 0.058 Uiso 1 1 calc R . .
H25B H 0.2816 0.2610 0.1357 0.058 Uiso 1 1 calc R . .
H25C H 0.3598 0.3453 0.1727 0.058 Uiso 1 1 calc R . .
C26 C 0.4716(4) 0.2365(4) 0.04884(16) 0.0425(11) Uani 1 1 d . . .
H26A H 0.3801 0.2074 0.0425 0.051 Uiso 1 1 calc R . .
H26B H 0.5052 0.2753 0.0195 0.051 Uiso 1 1 calc R . .
C27 C 0.5554(6) 0.1329(4) 0.06044(16) 0.0529(13) Uani 1 1 d . . .
H27A H 0.5204 0.0768 0.0829 0.063 Uiso 1 1 calc R . .
C28 C 0.6733(5) 0.1078(5) 0.0436(2) 0.0697(16) Uani 1 1 d . . .
H28A H 0.7133 0.1606 0.0210 0.084 Uiso 1 1 calc R . .
H28B H 0.7189 0.0368 0.0539 0.084 Uiso 1 1 calc R . .
C29 C 0.5000(4) 0.5806(4) 0.20300(13) 0.0315(9) Uani 1 1 d . . .
H29A H 0.4208 0.6301 0.1951 0.038 Uiso 1 1 calc R . .
H29B H 0.4777 0.4950 0.2108 0.038 Uiso 1 1 calc R . .
C30 C 0.5928(4) 0.6357(4) 0.23209(12) 0.0310(9) Uani 1 1 d . . .
H30A H 0.5725 0.7207 0.2425 0.037 Uiso 1 1 calc R . .
C31 C 0.7222(4) 0.5946(4) 0.24027(12) 0.0334(9) Uani 1 1 d . . .
H31A H 0.7303 0.5109 0.2531 0.040 Uiso 1 1 calc R . .
H31B H 0.7828 0.6532 0.2559 0.040 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01588(14) 0.02598(16) 0.01539(14) -0.00056(15) 0.00150(13) 0.00092(15)
Si1 0.0154(4) 0.0360(6) 0.0265(6) -0.0020(5) -0.0018(4) -0.0018(4)
Si2 0.0197(5) 0.0347(7) 0.0271(6) 0.0003(5) -0.0005(4) -0.0048(4)
C1 0.0162(17) 0.031(2) 0.0202(17) -0.0038(15) -0.0006(13) -0.0009(14)
C2 0.0169(15) 0.0244(17) 0.0211(18) -0.0035(17) 0.0012(15) 0.0017(13)
C3 0.0159(16) 0.027(2) 0.0200(19) -0.0035(16) -0.0042(14) -0.0001(15)
C4 0.0176(18) 0.0249(19) 0.0164(18) -0.0011(14) -0.0013(13) -0.0004(14)
C5 0.0184(17) 0.027(2) 0.0159(17) -0.0027(15) 0.0008(13) -0.0013(14)
C6 0.029(2) 0.040(2) 0.0241(19) -0.0075(18) 0.0034(15) -0.0035(17)
C7 0.0192(17) 0.037(2) 0.0314(19) -0.0019(19) 0.0045(14) 0.0070(18)
C8 0.0265(19) 0.035(2) 0.025(2) 0.0028(17) -0.0097(16) 0.0014(17)
C9 0.0232(19) 0.035(2) 0.0188(19) 0.0017(16) 0.0004(14) -0.0032(15)
C10 0.0182(18) 0.045(3) 0.037(2) -0.001(2) 0.0044(17) -0.0048(17)
C11 0.029(2) 0.056(3) 0.039(3) -0.001(2) -0.0089(19) 0.005(2)
C12 0.026(2) 0.045(2) 0.035(3) -0.009(2) -0.0032(16) -0.0151(18)
C13 0.044(2) 0.034(3) 0.043(3) -0.008(2) -0.002(2) -0.0042(19)
C14 0.075(3) 0.042(3) 0.046(3) -0.005(2) 0.010(3) -0.012(3)
C15 0.0214(19) 0.0268(19) 0.0208(19) -0.0021(15) 0.0018(14) 0.0039(14)
C16 0.0150(17) 0.026(2) 0.030(2) -0.0041(17) 0.0042(15) 0.0007(14)
C17 0.0188(15) 0.026(2) 0.0246(18) 0.0017(19) -0.0064(15) 0.0044(13)
C18 0.0256(17) 0.0221(18) 0.0224(18) 0.0001(14) 0.0036(16) 0.0003(15)
C19 0.0208(16) 0.0233(18) 0.0187(17) 0.0006(17) 0.0013(13) 0.0001(16)
C20 0.0316(19) 0.033(2) 0.0225(18) -0.0042(15) 0.0048(17) -0.0053(19)
C21 0.0211(19) 0.034(2) 0.035(2) -0.0042(18) 0.0058(16) 0.0001(16)
C22 0.0220(17) 0.044(2) 0.035(2) 0.001(2) -0.0049(15) 0.003(2)
C23 0.033(2) 0.032(2) 0.028(2) 0.0090(18) 0.0006(16) -0.0043(17)
C24 0.023(2) 0.057(3) 0.066(3) 0.015(3) -0.007(2) -0.005(2)
C25 0.032(2) 0.044(2) 0.040(2) -0.001(2) 0.003(2) -0.0129(18)
C26 0.037(2) 0.051(3) 0.040(3) -0.004(2) -0.006(2) -0.019(2)
C27 0.090(4) 0.030(3) 0.039(3) -0.003(2) 0.007(3) -0.007(3)
C28 0.063(3) 0.041(3) 0.105(5) -0.017(3) -0.011(3) 0.002(3)
C29 0.027(2) 0.036(2) 0.031(2) 0.0023(17) 0.0105(16) 0.0010(16)
C30 0.037(2) 0.039(3) 0.0178(18) -0.0001(17) 0.0131(15) 0.0018(18)
C31 0.039(2) 0.039(2) 0.0220(18) 0.0027(17) 0.0017(16) -0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100824.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100824.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100824
loop_
_publ_author_name
'Evans, William J.'
'Kozimor, Stosh A.'
'Brady, Jason C.'
'Davis, Benjamin L.'
'Nyce, Gregory W.'
'Seibel, Christopher A.'
'Ziller, Joseph W.'
'Doedens, Robert J.'
_publ_section_title
;
Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to
Cyclopentadienyl Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2269
_journal_page_last 2278
_journal_paper_doi 10.1021/om049286x
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C64 H116 Al2 Si4 Y2'
_chemical_formula_weight 1229.71
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 93.695(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 11.0875(10)
_cell_length_b 19.7843(18)
_cell_length_c 15.6311(14)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 171(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 3421.7(5)
_diffrn_ambient_temperature 171(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1320
_diffrn_reflns_av_sigmaI/netI 0.1034
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 28964
_diffrn_reflns_theta_max 24.71
_diffrn_reflns_theta_min 1.66
_diffrn_standards_decay_% '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_interval_time ?
_diffrn_standards_number '50 frames'
_exptl_absorpt_coefficient_mu 1.818
_exptl_absorpt_correction_T_max 0.8833
_exptl_absorpt_correction_T_min 0.5769
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.194
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Irregular
_exptl_crystal_F_000 1320
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.07
_refine_ls_extinction_coef 0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXTL
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 350
_refine_ls_number_reflns 5819
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.1233
_refine_ls_R_factor_gt 0.0531
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+2.2823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1111
_refine_ls_wR_factor_ref 0.1381
_reflns_number_gt 3423
_reflns_number_total 5819
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
The following automatic conversions were performed:
'_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to
'mixed'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100824
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.60017(5) 0.13404(3) 0.86845(3) 0.02667(18) Uani 1 1 d . . .
Si1 Si 0.45240(15) 0.32158(8) 0.91390(11) 0.0402(4) Uani 1 1 d . . .
Si2 Si 0.33404(16) 0.10396(9) 0.67591(11) 0.0408(4) Uani 1 1 d . . .
Al1 Al 0.76207(15) -0.05838(8) 1.01587(11) 0.0308(4) Uani 1 1 d . . .
C1 C 0.5825(5) 0.1535(3) 0.6992(3) 0.0350(14) Uani 1 1 d . . .
C2 C 0.7000(5) 0.1290(3) 0.7167(3) 0.0408(15) Uani 1 1 d . . .
C3 C 0.6928(5) 0.0609(3) 0.7435(3) 0.0401(15) Uani 1 1 d . . .
C4 C 0.5691(5) 0.0429(3) 0.7434(3) 0.0332(14) Uani 1 1 d . . .
C5 C 0.4966(5) 0.1012(3) 0.7157(3) 0.0323(13) Uani 1 1 d . . .
C6 C 0.5522(6) 0.2193(3) 0.6553(4) 0.0545(18) Uani 1 1 d . . .
H6A H 0.5510 0.2131 0.5930 0.082 Uiso 1 1 calc R . .
H6B H 0.6132 0.2532 0.6732 0.082 Uiso 1 1 calc R . .
H6C H 0.4725 0.2347 0.6710 0.082 Uiso 1 1 calc R . .
C7 C 0.8166(6) 0.1640(4) 0.6957(4) 0.0592(19) Uani 1 1 d . . .
H7A H 0.8334 0.1545 0.6362 0.089 Uiso 1 1 calc R . .
H7B H 0.8834 0.1473 0.7341 0.089 Uiso 1 1 calc R . .
H7C H 0.8081 0.2129 0.7035 0.089 Uiso 1 1 calc R . .
C8 C 0.8003(5) 0.0145(4) 0.7591(4) 0.0549(18) Uani 1 1 d . . .
H8A H 0.8189 -0.0071 0.7050 0.082 Uiso 1 1 calc R . .
H8B H 0.7814 -0.0203 0.8008 0.082 Uiso 1 1 calc R . .
H8C H 0.8704 0.0407 0.7815 0.082 Uiso 1 1 calc R . .
C9 C 0.5250(5) -0.0275(3) 0.7587(4) 0.0422(15) Uani 1 1 d . . .
H9A H 0.5200 -0.0526 0.7046 0.063 Uiso 1 1 calc R . .
H9B H 0.4448 -0.0255 0.7816 0.063 Uiso 1 1 calc R . .
H9C H 0.5814 -0.0504 0.8001 0.063 Uiso 1 1 calc R . .
C10 C 0.6907(5) 0.2571(3) 0.8923(3) 0.0331(14) Uani 1 1 d . . .
C11 C 0.7716(5) 0.2133(3) 0.9396(4) 0.0347(14) Uani 1 1 d . . .
C12 C 0.7110(5) 0.1888(3) 1.0102(4) 0.0368(14) Uani 1 1 d . . .
C13 C 0.5938(5) 0.2154(3) 1.0062(3) 0.0326(14) Uani 1 1 d . . .
C14 C 0.5769(5) 0.2574(3) 0.9317(4) 0.0325(13) Uani 1 1 d . . .
C15 C 0.7301(5) 0.3061(3) 0.8259(4) 0.0480(17) Uani 1 1 d . . .
H15A H 0.7601 0.3475 0.8542 0.072 Uiso 1 1 calc R . .
H15B H 0.6613 0.3169 0.7857 0.072 Uiso 1 1 calc R . .
H15C H 0.7947 0.2857 0.7945 0.072 Uiso 1 1 calc R . .
C16 C 0.9034(5) 0.2028(3) 0.9262(4) 0.0511(17) Uani 1 1 d . . .
H16A H 0.9513 0.2374 0.9578 0.077 Uiso 1 1 calc R . .
H16B H 0.9166 0.2063 0.8650 0.077 Uiso 1 1 calc R . .
H16C H 0.9283 0.1579 0.9471 0.077 Uiso 1 1 calc R . .
C17 C 0.7734(6) 0.1508(3) 1.0835(4) 0.0530(18) Uani 1 1 d . . .
H17A H 0.8059 0.1829 1.1268 0.080 Uiso 1 1 calc R . .
H17B H 0.8396 0.1239 1.0624 0.080 Uiso 1 1 calc R . .
H17C H 0.7154 0.1207 1.1091 0.080 Uiso 1 1 calc R . .
C18 C 0.5088(5) 0.2060(3) 1.0774(4) 0.0447(16) Uani 1 1 d . . .
H18A H 0.5233 0.2417 1.1204 0.067 Uiso 1 1 calc R . .
H18B H 0.5231 0.1618 1.1044 0.067 Uiso 1 1 calc R . .
H18C H 0.4250 0.2086 1.0535 0.067 Uiso 1 1 calc R . .
C19 C 0.4372(7) 0.3569(4) 0.8050(4) 0.069(2) Uani 1 1 d . . .
H19A H 0.5143 0.3768 0.7908 0.103 Uiso 1 1 calc R . .
H19B H 0.3744 0.3918 0.8021 0.103 Uiso 1 1 calc R . .
H19C H 0.4147 0.3209 0.7640 0.103 Uiso 1 1 calc R . .
C20 C 0.4806(6) 0.3939(3) 0.9875(4) 0.0554(18) Uani 1 1 d . . .
H20A H 0.5577 0.4152 0.9760 0.083 Uiso 1 1 calc R . .
H20B H 0.4839 0.3779 1.0469 0.083 Uiso 1 1 calc R . .
H20C H 0.4151 0.4269 0.9785 0.083 Uiso 1 1 calc R . .
C21 C 0.3020(6) 0.2847(3) 0.9383(5) 0.062(2) Uani 1 1 d . . .
H21A H 0.2872 0.2439 0.9027 0.075 Uiso 1 1 calc R . .
H21B H 0.3061 0.2704 0.9991 0.075 Uiso 1 1 calc R . .
C22 C 0.1977(7) 0.3315(4) 0.9230(7) 0.095(3) Uani 1 1 d . . .
H22A H 0.1976 0.3695 0.9602 0.114 Uiso 1 1 calc R . .
C23 C 0.1153(9) 0.3286(6) 0.8717(8) 0.144(5) Uani 1 1 d . . .
H23A H 0.1092 0.2920 0.8322 0.172 Uiso 1 1 calc R . .
H23B H 0.0550 0.3627 0.8698 0.172 Uiso 1 1 calc R . .
C24 C 0.2538(5) 0.0236(3) 0.6899(4) 0.0533(18) Uani 1 1 d . . .
H24A H 0.2573 0.0117 0.7508 0.080 Uiso 1 1 calc R . .
H24B H 0.2921 -0.0121 0.6578 0.080 Uiso 1 1 calc R . .
H24C H 0.1692 0.0285 0.6685 0.080 Uiso 1 1 calc R . .
C25 C 0.2465(6) 0.1719(3) 0.7274(4) 0.0549(18) Uani 1 1 d . . .
H25A H 0.2489 0.1643 0.7894 0.082 Uiso 1 1 calc R . .
H25B H 0.1624 0.1710 0.7039 0.082 Uiso 1 1 calc R . .
H25C H 0.2823 0.2160 0.7158 0.082 Uiso 1 1 calc R . .
C26 C 0.3243(6) 0.1225(3) 0.5579(4) 0.0574(19) Uani 1 1 d . . .
H26A H 0.2381 0.1261 0.5377 0.069 Uiso 1 1 calc R . .
H26B H 0.3627 0.1668 0.5484 0.069 Uiso 1 1 calc R . .
C27 C 0.3820(7) 0.0714(4) 0.5064(4) 0.070(2) Uani 1 1 d . . .
H27A H 0.4675 0.0730 0.5050 0.084 Uiso 1 1 calc R . .
C28 C 0.3239(8) 0.0232(4) 0.4616(5) 0.078(2) Uani 1 1 d . . .
H28A H 0.2384 0.0201 0.4614 0.094 Uiso 1 1 calc R . .
H28B H 0.3677 -0.0081 0.4297 0.094 Uiso 1 1 calc R . .
C29 C 0.6946(6) 0.0265(3) 0.9557(4) 0.0306(14) Uani 1 1 d . . .
C30 C 0.6112(5) -0.0925(3) 1.0722(4) 0.0308(14) Uani 1 1 d . . .
C31 C 0.8113(5) -0.1249(3) 0.9294(4) 0.0414(15) Uani 1 1 d . . .
H31A H 0.8832 -0.1083 0.9027 0.062 Uiso 1 1 calc R . .
H31B H 0.7453 -0.1309 0.8853 0.062 Uiso 1 1 calc R . .
H31C H 0.8296 -0.1683 0.9575 0.062 Uiso 1 1 calc R . .
C32 C 0.8973(5) -0.0363(3) 1.1009(3) 0.0401(15) Uani 1 1 d . . .
H32A H 0.9668 -0.0203 1.0708 0.060 Uiso 1 1 calc R . .
H32B H 0.9203 -0.0768 1.1341 0.060 Uiso 1 1 calc R . .
H32C H 0.8716 -0.0009 1.1396 0.060 Uiso 1 1 calc R . .
H29A H 0.759(5) 0.051(3) 0.935(3) 0.044(17) Uiso 1 1 d . . .
H29B H 0.653(4) 0.050(3) 0.997(3) 0.032(15) Uiso 1 1 d . . .
H29C H 0.645(4) 0.009(3) 0.916(3) 0.028(16) Uiso 1 1 d . . .
H30A H 0.619(4) -0.135(3) 1.096(3) 0.037(16) Uiso 1 1 d . . .
H30B H 0.602(4) -0.063(3) 1.114(3) 0.037(16) Uiso 1 1 d . . .
H30C H 0.548(5) -0.097(3) 1.022(4) 0.047(17) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.0354(3) 0.0201(3) 0.0242(3) 0.0005(3) -0.0006(2) -0.0020(3)
Si1 0.0446(10) 0.0261(9) 0.0490(11) -0.0024(8) -0.0038(8) 0.0032(8)
Si2 0.0475(11) 0.0387(10) 0.0350(10) 0.0002(8) -0.0074(8) -0.0010(8)
Al1 0.0347(10) 0.0244(9) 0.0333(10) 0.0020(7) 0.0021(8) 0.0037(7)
C1 0.052(4) 0.030(3) 0.022(3) 0.005(2) 0.001(3) -0.005(3)
C2 0.050(4) 0.049(4) 0.025(3) -0.001(3) 0.010(3) -0.015(3)
C3 0.052(4) 0.050(4) 0.019(3) -0.006(3) 0.001(3) 0.010(3)
C4 0.052(4) 0.027(3) 0.020(3) -0.002(2) -0.004(3) -0.003(3)
C5 0.042(3) 0.032(3) 0.023(3) -0.005(3) -0.003(3) 0.004(3)
C6 0.092(5) 0.042(4) 0.028(4) 0.007(3) -0.010(3) -0.015(4)
C7 0.055(4) 0.079(5) 0.045(4) -0.013(4) 0.014(3) -0.020(4)
C8 0.055(4) 0.074(5) 0.035(4) -0.015(3) 0.006(3) 0.014(4)
C9 0.058(4) 0.033(4) 0.034(3) -0.005(3) -0.011(3) 0.004(3)
C10 0.047(4) 0.020(3) 0.032(3) -0.007(3) 0.001(3) -0.009(3)
C11 0.040(4) 0.025(3) 0.038(4) -0.014(3) -0.006(3) -0.002(3)
C12 0.048(4) 0.025(3) 0.036(4) -0.010(3) -0.009(3) -0.001(3)
C13 0.050(4) 0.020(3) 0.027(3) -0.003(2) -0.001(3) -0.007(3)
C14 0.038(3) 0.020(3) 0.039(3) -0.004(3) 0.001(3) -0.005(2)
C15 0.051(4) 0.040(4) 0.053(4) 0.003(3) 0.001(3) -0.016(3)
C16 0.040(4) 0.050(4) 0.062(5) -0.017(3) -0.004(3) -0.002(3)
C17 0.074(5) 0.034(4) 0.048(4) -0.008(3) -0.022(4) 0.003(3)
C18 0.058(4) 0.042(4) 0.035(4) -0.006(3) 0.004(3) -0.003(3)
C19 0.085(5) 0.065(5) 0.056(5) 0.010(4) -0.002(4) 0.031(4)
C20 0.060(4) 0.035(4) 0.071(5) -0.006(3) -0.002(4) 0.011(3)
C21 0.051(4) 0.042(4) 0.093(6) 0.006(4) -0.008(4) 0.008(3)
C22 0.051(5) 0.036(4) 0.198(11) -0.004(6) -0.006(6) -0.002(4)
C23 0.071(7) 0.111(9) 0.245(15) 0.106(9) -0.010(8) -0.006(6)
C24 0.049(4) 0.058(4) 0.052(4) -0.011(3) -0.003(3) -0.008(3)
C25 0.051(4) 0.051(4) 0.061(5) 0.002(4) -0.006(3) 0.008(3)
C26 0.066(5) 0.057(5) 0.048(4) 0.008(4) -0.011(4) 0.000(4)
C27 0.073(5) 0.094(7) 0.041(4) 0.004(4) -0.003(4) 0.003(5)
C28 0.108(7) 0.081(6) 0.045(5) 0.000(4) 0.008(4) 0.016(5)
C29 0.034(4) 0.027(3) 0.032(4) -0.005(3) 0.006(3) -0.005(3)
C30 0.042(4) 0.023(4) 0.027(3) 0.000(3) -0.002(3) 0.000(3)
C31 0.051(4) 0.029(3) 0.046(4) 0.003(3) 0.008(3) 0.009(3)
C32 0.045(4) 0.043(4) 0.032(3) 0.010(3) -0.002(3) -0.002(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100825.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100825.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100825
loop_
_publ_author_name
'Evans, William J.'
'Kozimor, Stosh A.'
'Brady, Jason C.'
'Davis, Benjamin L.'
'Nyce, Gregory W.'
'Seibel, Christopher A.'
'Ziller, Joseph W.'
'Doedens, Robert J.'
_publ_section_title
;
Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to
Cyclopentadienyl Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2269
_journal_page_last 2278
_journal_paper_doi 10.1021/om049286x
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C23 H35 Si Y'
_chemical_formula_weight 428.51
_space_group_IT_number 110
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I 4bw -2c'
_symmetry_space_group_name_H-M 'I 41 c d'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 29.2318(15)
_cell_length_b 29.2318(15)
_cell_length_c 10.1105(7)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 163(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 8639.4(9)
_diffrn_ambient_temperature 163(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0586
_diffrn_reflns_av_sigmaI/netI 0.0465
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_k_max 38
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 45278
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 1.39
_diffrn_standards_decay_% '< 1.0'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.759
_exptl_absorpt_correction_T_max 0.5573
_exptl_absorpt_correction_T_min 0.4452
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.318
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rods
_exptl_crystal_F_000 3616
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.24
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.023(6)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.074
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 5325
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0485
_refine_ls_R_factor_gt 0.0361
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+6.9213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0896
_refine_ls_wR_factor_ref 0.0965
_reflns_number_gt 4611
_reflns_number_total 5325
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M I4(1)cd
_cod_database_code 1100825
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.887047(10) 0.372793(10) 0.63242(3) 0.01784(8) Uani 1 1 d . . .
Si1 Si 0.85816(3) 0.37562(3) 0.94942(9) 0.0219(2) Uani 1 1 d . . .
C1 C 0.81010(11) 0.40954(12) 0.7113(4) 0.0224(7) Uani 1 1 d . . .
C2 C 0.79834(11) 0.39287(12) 0.5841(4) 0.0236(7) Uani 1 1 d . . .
C3 C 0.80047(11) 0.34425(12) 0.5884(3) 0.0225(7) Uani 1 1 d . . .
C4 C 0.81418(11) 0.33139(12) 0.7176(3) 0.0218(7) Uani 1 1 d . . .
C5 C 0.82001(11) 0.37205(11) 0.7975(3) 0.0192(7) Uani 1 1 d . . .
C6 C 0.80711(13) 0.45993(12) 0.7467(4) 0.0314(8) Uani 1 1 d . . .
H6A H 0.8167 0.4643 0.8387 0.047 Uiso 1 1 calc R . .
H6B H 0.7755 0.4705 0.7361 0.047 Uiso 1 1 calc R . .
H6C H 0.8272 0.4776 0.6882 0.047 Uiso 1 1 calc R . .
C7 C 0.78185(13) 0.42087(13) 0.4679(4) 0.0320(8) Uani 1 1 d . . .
H7A H 0.7763 0.4007 0.3922 0.048 Uiso 1 1 calc R . .
H7B H 0.8052 0.4435 0.4443 0.048 Uiso 1 1 calc R . .
H7C H 0.7534 0.4366 0.4917 0.048 Uiso 1 1 calc R . .
C8 C 0.78666(13) 0.31192(13) 0.4789(4) 0.0319(8) Uani 1 1 d . . .
H8A H 0.7786 0.3295 0.3998 0.048 Uiso 1 1 calc R . .
H8B H 0.7602 0.2938 0.5074 0.048 Uiso 1 1 calc R . .
H8C H 0.8122 0.2914 0.4585 0.048 Uiso 1 1 calc R . .
C9 C 0.81790(13) 0.28166(12) 0.7604(4) 0.0278(8) Uani 1 1 d . . .
H9A H 0.8282 0.2802 0.8525 0.042 Uiso 1 1 calc R . .
H9B H 0.8400 0.2658 0.7038 0.042 Uiso 1 1 calc R . .
H9C H 0.7879 0.2669 0.7523 0.042 Uiso 1 1 calc R . .
C10 C 0.93671(11) 0.41606(11) 0.8060(3) 0.0206(7) Uani 1 1 d . . .
C11 C 0.97007(11) 0.40090(12) 0.7137(4) 0.0242(7) Uani 1 1 d . . .
C12 C 0.97177(11) 0.35265(11) 0.7178(3) 0.0215(7) Uani 1 1 d . . .
C13 C 0.93969(11) 0.33727(11) 0.8123(4) 0.0213(7) Uani 1 1 d . . .
C14 C 0.91666(12) 0.37667(10) 0.8702(4) 0.0208(7) Uani 1 1 d . . .
C15 C 0.92873(12) 0.46581(11) 0.8362(4) 0.0280(8) Uani 1 1 d . . .
H15A H 0.9044 0.4687 0.9022 0.042 Uiso 1 1 calc R . .
H15B H 0.9197 0.4818 0.7551 0.042 Uiso 1 1 calc R . .
H15C H 0.9569 0.4794 0.8709 0.042 Uiso 1 1 calc R . .
C16 C 1.00138(12) 0.43159(11) 0.6338(5) 0.0309(7) Uani 1 1 d . . .
H16A H 0.9930 0.4636 0.6486 0.046 Uiso 1 1 calc R . .
H16B H 0.9983 0.4243 0.5397 0.046 Uiso 1 1 calc R . .
H16C H 1.0331 0.4267 0.6616 0.046 Uiso 1 1 calc R . .
C17 C 1.00551(12) 0.32344(12) 0.6440(4) 0.0312(8) Uani 1 1 d . . .
H17A H 0.9995 0.2911 0.6630 0.047 Uiso 1 1 calc R . .
H17B H 1.0366 0.3312 0.6721 0.047 Uiso 1 1 calc R . .
H17C H 1.0024 0.3289 0.5488 0.047 Uiso 1 1 calc R . .
C18 C 0.93417(12) 0.28743(11) 0.8481(4) 0.0280(8) Uani 1 1 d . . .
H18A H 0.9103 0.2843 0.9155 0.042 Uiso 1 1 calc R . .
H18B H 0.9631 0.2756 0.8829 0.042 Uiso 1 1 calc R . .
H18C H 0.9255 0.2700 0.7692 0.042 Uiso 1 1 calc R . .
C19 C 0.84725(13) 0.42763(14) 1.0542(4) 0.0341(9) Uani 1 1 d . . .
H19A H 0.8510 0.4552 1.0003 0.051 Uiso 1 1 calc R . .
H19B H 0.8691 0.4283 1.1277 0.051 Uiso 1 1 calc R . .
H19C H 0.8160 0.4265 1.0892 0.051 Uiso 1 1 calc R . .
C20 C 0.84979(14) 0.32746(15) 1.0686(4) 0.0371(10) Uani 1 1 d . . .
H20A H 0.8189 0.3290 1.1059 0.056 Uiso 1 1 calc R . .
H20B H 0.8723 0.3298 1.1399 0.056 Uiso 1 1 calc R . .
H20C H 0.8537 0.2983 1.0223 0.056 Uiso 1 1 calc R . .
C21 C 0.90790(15) 0.32500(15) 0.4272(4) 0.0355(9) Uani 1 1 d . . .
C22 C 0.9270(2) 0.3675(2) 0.4047(5) 0.0618(15) Uani 1 1 d . . .
C23 C 0.90550(14) 0.40963(15) 0.4054(4) 0.0393(10) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01680(14) 0.01938(15) 0.01734(14) 0.00066(13) -0.00025(13) 0.00163(11)
Si1 0.0227(5) 0.0266(5) 0.0164(5) 0.0014(4) 0.0008(4) 0.0014(4)
C1 0.0196(16) 0.0242(18) 0.0235(18) 0.0039(14) 0.0021(13) 0.0047(13)
C2 0.0141(15) 0.0321(19) 0.0247(18) 0.0072(14) 0.0005(13) 0.0045(13)
C3 0.0156(15) 0.0299(19) 0.0221(17) -0.0002(14) -0.0027(12) 0.0003(13)
C4 0.0195(16) 0.0230(17) 0.0230(18) -0.0005(13) -0.0004(13) -0.0006(13)
C5 0.0174(16) 0.0223(17) 0.0179(16) 0.0016(13) 0.0026(12) 0.0003(12)
C6 0.0312(19) 0.0251(19) 0.038(2) 0.0042(16) -0.0004(17) 0.0074(14)
C7 0.0263(19) 0.043(2) 0.0266(19) 0.0071(17) -0.0036(15) 0.0092(16)
C8 0.027(2) 0.037(2) 0.032(2) -0.0016(17) -0.0051(16) -0.0034(15)
C9 0.0298(18) 0.0219(18) 0.032(2) 0.0011(15) -0.0029(16) -0.0004(14)
C10 0.0225(17) 0.0180(16) 0.0214(17) -0.0008(13) -0.0020(13) -0.0005(13)
C11 0.0215(17) 0.0240(17) 0.0270(18) 0.0004(14) -0.0031(14) -0.0002(13)
C12 0.0165(15) 0.0242(17) 0.0238(17) -0.0034(14) -0.0041(13) 0.0044(12)
C13 0.0214(17) 0.0185(16) 0.0241(17) -0.0032(13) -0.0071(14) 0.0026(13)
C14 0.0260(17) 0.0212(16) 0.0154(16) -0.0005(14) -0.0074(15) 0.0005(11)
C15 0.0266(18) 0.0210(17) 0.036(2) -0.0038(15) 0.0014(15) -0.0016(13)
C16 0.0244(15) 0.0309(16) 0.0376(18) -0.004(2) 0.0028(16) -0.0060(15)
C17 0.0246(17) 0.0367(18) 0.032(2) -0.0051(19) -0.0005(17) 0.0102(14)
C18 0.0321(19) 0.0218(17) 0.030(2) 0.0011(14) -0.0055(14) 0.0047(14)
C19 0.030(2) 0.046(2) 0.027(2) -0.0096(17) 0.0028(16) 0.0052(17)
C20 0.030(2) 0.050(3) 0.031(2) 0.0164(19) -0.0024(17) -0.0071(18)
C21 0.042(2) 0.041(2) 0.0229(19) -0.0102(16) 0.0078(17) -0.0020(18)
C22 0.072(4) 0.075(4) 0.039(3) -0.002(3) 0.008(3) -0.003(3)
C23 0.040(2) 0.045(2) 0.034(3) 0.0055(18) 0.0086(18) -0.0017(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100826.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100826.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100826
loop_
_publ_author_name
'Evans, William J.'
'Kozimor, Stosh A.'
'Brady, Jason C.'
'Davis, Benjamin L.'
'Nyce, Gregory W.'
'Seibel, Christopher A.'
'Ziller, Joseph W.'
'Doedens, Robert J.'
_publ_section_title
;
Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to
Cyclopentadienyl Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2269
_journal_page_last 2278
_journal_paper_doi 10.1021/om049286x
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C23 H35 Lu'
_chemical_formula_weight 486.48
_space_group_IT_number 82
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'I -4'
_symmetry_space_group_name_H-M 'I -4'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 22.5779(5)
_cell_length_b 22.5779(5)
_cell_length_c 8.4111(3)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 163(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 4287.7(2)
_diffrn_ambient_temperature 163(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0325
_diffrn_reflns_av_sigmaI/netI 0.0277
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 23139
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 1.28
_diffrn_standards_decay_% ' 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_interval_time ?
_diffrn_standards_number '50 frames'
_exptl_absorpt_coefficient_mu 4.606
_exptl_absorpt_correction_T_max 0.5450
_exptl_absorpt_correction_T_min 0.3805
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.507
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 1952
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.15
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.006(11)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.073
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 247
_refine_ls_number_reflns 5217
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.073
_refine_ls_R_factor_all 0.0237
_refine_ls_R_factor_gt 0.0214
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+4.7003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0492
_refine_ls_wR_factor_ref 0.0504
_reflns_number_gt 4967
_reflns_number_total 5217
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
The following automatic conversions were performed:
'_atom_sites_solution_hydrogens' value 'geom/difmap' was changed to
'mixed'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M I-4
_cod_database_code 1100826
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.055404(6) 0.255802(6) 0.065318(17) 0.02239(4) Uani 1 1 d . . .
C1 C 0.05508(17) 0.34267(17) 0.2671(5) 0.0270(8) Uani 1 1 d . . .
C2 C 0.11531(16) 0.32734(16) 0.2466(4) 0.0248(7) Uani 1 1 d . . .
C3 C 0.13211(16) 0.34245(16) 0.0874(5) 0.0251(8) Uani 1 1 d . . .
C4 C 0.08168(17) 0.36748(17) 0.0120(5) 0.0275(8) Uani 1 1 d . . .
C5 C 0.03429(17) 0.36830(18) 0.1236(5) 0.0291(8) Uani 1 1 d . . .
C6 C 0.0220(2) 0.3388(2) 0.4220(7) 0.0473(11) Uani 1 1 d . . .
H6A H -0.0173(12) 0.3514(4) 0.4068(8) 0.071 Uiso 1 1 calc R . .
H6B H 0.0405(6) 0.3632(8) 0.498(2) 0.071 Uiso 1 1 calc R . .
H6C H 0.0221(2) 0.2994(12) 0.4582(13) 0.071 Uiso 1 1 calc R . .
C7 C 0.1567(2) 0.30978(19) 0.3776(5) 0.0366(10) Uani 1 1 d . . .
H7A H 0.1925(11) 0.3019(3) 0.3368(12) 0.055 Uiso 1 1 calc R . .
H7B H 0.1426(5) 0.2775(10) 0.4266(16) 0.055 Uiso 1 1 calc R . .
H7C H 0.1596(2) 0.3395(9) 0.448(2) 0.055 Uiso 1 1 calc R . .
C8 C 0.19271(17) 0.34448(19) 0.0161(5) 0.0369(10) Uani 1 1 d . . .
H8A H 0.2188(8) 0.3262(6) 0.082(2) 0.055 Uiso 1 1 calc R . .
H8B H 0.2038(4) 0.3828(11) 0.0022(7) 0.055 Uiso 1 1 calc R . .
H8C H 0.19241(17) 0.3257(6) -0.079(3) 0.055 Uiso 1 1 calc R . .
C9 C 0.0804(2) 0.3939(2) -0.1518(5) 0.0464(12) Uani 1 1 d . . .
H9A H 0.0453(12) 0.4063(5) -0.1725(9) 0.070 Uiso 1 1 calc R . .
H9B H 0.0905(4) 0.3676(9) -0.220(2) 0.070 Uiso 1 1 calc R . .
H9C H 0.1048(8) 0.4231(10) -0.1563(6) 0.070 Uiso 1 1 calc R . .
C10 C -0.02355(18) 0.4004(2) 0.1027(6) 0.0459(13) Uani 1 1 d . . .
H10A H -0.0267(2) 0.4122(4) 0.006(3) 0.069 Uiso 1 1 calc R . .
H10B H -0.02460(19) 0.4304(10) 0.165(2) 0.069 Uiso 1 1 calc R . .
H10C H -0.0522(10) 0.3771(8) 0.1247(9) 0.069 Uiso 1 1 calc R . .
C11 C 0.05270(16) 0.13959(16) 0.0764(6) 0.0284(8) Uani 1 1 d . . .
C12 C 0.10082(17) 0.15810(17) 0.1741(5) 0.0265(8) Uani 1 1 d . . .
C13 C 0.14451(15) 0.18363(15) 0.0735(6) 0.0260(7) Uani 1 1 d . . .
C14 C 0.12257(16) 0.18272(16) -0.0843(5) 0.0257(7) Uani 1 1 d . . .
C15 C 0.06614(16) 0.15478(16) -0.0824(5) 0.0259(7) Uani 1 1 d . . .
C16 C 0.0010(2) 0.1030(2) 0.1329(6) 0.0422(11) Uani 1 1 d . . .
H16A H 0.0025(2) 0.0994(2) 0.241(3) 0.063 Uiso 1 1 calc R . .
H16B H 0.0027(2) 0.0662(12) 0.0873(15) 0.063 Uiso 1 1 calc R . .
H16C H -0.0337(11) 0.1212(6) 0.1043(11) 0.063 Uiso 1 1 calc R . .
C17 C 0.1071(3) 0.1463(2) 0.3497(5) 0.0461(12) Uani 1 1 d . . .
H17A H 0.1410(11) 0.1623(6) 0.3849(13) 0.069 Uiso 1 1 calc R . .
H17B H 0.1075(3) 0.1072(13) 0.3670(8) 0.069 Uiso 1 1 calc R . .
H17C H 0.0765(10) 0.1626(6) 0.4017(18) 0.069 Uiso 1 1 calc R . .
C18 C 0.20740(18) 0.19764(19) 0.1219(6) 0.0366(10) Uani 1 1 d . . .
H18A H 0.2105(2) 0.1955(2) 0.222(3) 0.055 Uiso 1 1 calc R . .
H18B H 0.2162(3) 0.2322(10) 0.0917(10) 0.055 Uiso 1 1 calc R . .
H18C H 0.2307(7) 0.1731(7) 0.0792(13) 0.055 Uiso 1 1 calc R . .
C19 C 0.1547(2) 0.2025(2) -0.2321(5) 0.0385(10) Uani 1 1 d . . .
H19A H 0.1920(11) 0.2199(6) -0.2031(9) 0.058 Uiso 1 1 calc R . .
H19B H 0.1311(7) 0.2312(9) -0.2877(17) 0.058 Uiso 1 1 calc R . .
H19C H 0.1615(3) 0.1689(10) -0.300(2) 0.058 Uiso 1 1 calc R . .
C20 C 0.0314(2) 0.1369(2) -0.2290(5) 0.0386(11) Uani 1 1 d . . .
H20A H -0.0042(11) 0.1194(6) -0.1983(10) 0.058 Uiso 1 1 calc R . .
H20B H 0.0535(7) 0.1099(9) -0.2883(19) 0.058 Uiso 1 1 calc R . .
H20C H 0.0237(3) 0.1702(10) -0.291(2) 0.058 Uiso 1 1 calc R . .
C21 C -0.0530(2) 0.2452(2) 0.1443(9) 0.0460(14) Uani 1 1 d . . .
C22 C -0.0511(2) 0.2348(2) -0.0175(8) 0.0487(16) Uani 1 1 d . . .
C23 C -0.0278(2) 0.2711(2) -0.1345(7) 0.0484(13) Uani 1 1 d . . .
H21A H -0.070(3) 0.217(3) 0.224(8) 0.067(19) Uiso 1 1 d . . .
H21B H -0.057(2) 0.285(2) 0.195(6) 0.042(13) Uiso 1 1 d . . .
H22 H -0.061(2) 0.194(2) -0.055(8) 0.063(16) Uiso 1 1 d . . .
H23A H -0.029(2) 0.259(2) -0.253(7) 0.049(15) Uiso 1 1 d . . .
H23B H -0.033(3) 0.310(3) -0.112(7) 0.062(18) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Lu1 0.01678(7) 0.02266(8) 0.02772(7) -0.00494(6) -0.00119(6) -0.00041(6)
C1 0.0229(18) 0.0261(18) 0.032(2) -0.0115(16) 0.0045(15) -0.0037(14)
C2 0.0250(18) 0.0221(17) 0.0273(18) -0.0026(14) -0.0047(14) -0.0038(14)
C3 0.0213(16) 0.0250(17) 0.029(2) -0.0026(16) -0.0008(15) -0.0015(13)
C4 0.0263(19) 0.0281(19) 0.0282(18) -0.0021(15) -0.0056(15) -0.0025(15)
C5 0.0213(18) 0.0263(19) 0.040(2) -0.0090(16) -0.0046(16) 0.0023(15)
C6 0.048(3) 0.054(3) 0.040(2) -0.012(2) 0.013(2) -0.012(2)
C7 0.046(2) 0.029(2) 0.036(2) -0.0006(17) -0.0154(18) -0.0040(18)
C8 0.0255(19) 0.034(2) 0.051(3) -0.0057(18) 0.0107(18) -0.0042(16)
C9 0.065(3) 0.042(3) 0.032(2) 0.007(2) -0.010(2) -0.009(2)
C10 0.029(2) 0.038(2) 0.070(4) -0.012(2) -0.010(2) 0.0088(18)
C11 0.0282(18) 0.0235(17) 0.034(2) -0.0020(18) 0.0012(18) -0.0026(14)
C12 0.032(2) 0.0267(18) 0.0209(17) -0.0032(15) -0.0029(15) 0.0014(15)
C13 0.0233(16) 0.0226(16) 0.0322(18) -0.0062(18) -0.0039(18) 0.0035(13)
C14 0.0249(17) 0.0267(17) 0.0255(18) -0.0022(15) 0.0025(15) 0.0034(14)
C15 0.0278(17) 0.0255(17) 0.0245(19) -0.0063(16) -0.0011(16) 0.0015(14)
C16 0.040(2) 0.032(2) 0.054(3) -0.002(2) 0.010(2) -0.0144(19)
C17 0.070(3) 0.042(3) 0.026(2) 0.0012(19) -0.005(2) -0.005(2)
C18 0.029(2) 0.035(2) 0.046(2) -0.0113(18) -0.0064(18) 0.0049(17)
C19 0.044(2) 0.041(2) 0.031(2) -0.0034(18) 0.0099(18) -0.0016(19)
C20 0.043(3) 0.040(2) 0.033(2) -0.0083(19) -0.0110(19) -0.002(2)
C21 0.023(2) 0.037(3) 0.078(4) -0.009(3) 0.008(2) -0.0029(18)
C22 0.019(2) 0.045(3) 0.081(5) -0.017(3) -0.013(2) 0.0014(19)
C23 0.042(3) 0.037(3) 0.067(3) -0.011(2) -0.028(2) 0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100827.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100827.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100827
loop_
_publ_author_name
'Evans, William J.'
'Kozimor, Stosh A.'
'Brady, Jason C.'
'Davis, Benjamin L.'
'Nyce, Gregory W.'
'Seibel, Christopher A.'
'Ziller, Joseph W.'
'Doedens, Robert J.'
_publ_section_title
;
Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to
Cyclopentadienyl Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2269
_journal_page_last 2278
_journal_paper_doi 10.1021/om049286x
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C23 H35 Y'
_chemical_formula_weight 400.42
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.066(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.9218(11)
_cell_length_b 17.632(2)
_cell_length_c 13.6181(17)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 163(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 2142.3(5)
_diffrn_ambient_temperature 163(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0433
_diffrn_reflns_av_sigmaI/netI 0.0401
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 22410
_diffrn_reflns_theta_max 28.31
_diffrn_reflns_theta_min 1.89
_diffrn_standards_decay_% '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_interval_time ?
_diffrn_standards_number '50 frames'
_exptl_absorpt_coefficient_mu 2.724
_exptl_absorpt_correction_T_max 0.7185
_exptl_absorpt_correction_T_min 0.4088
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS'
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 1.242
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description MFP
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.13
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 357
_refine_ls_number_reflns 5189
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0499
_refine_ls_R_factor_gt 0.0304
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.6295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0671
_refine_ls_wR_factor_ref 0.0732
_reflns_number_gt 4053
_reflns_number_total 5189
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.22989(2) 0.183735(10) 0.275151(13) 0.01507(6) Uani 1 1 d . . .
C1 C 0.2136(2) 0.25558(12) 0.44700(15) 0.0206(4) Uani 1 1 d . . .
C2 C 0.1382(2) 0.18552(12) 0.45998(14) 0.0204(4) Uani 1 1 d . . .
C3 C 0.0053(2) 0.18813(12) 0.40236(15) 0.0221(4) Uani 1 1 d . . .
C4 C 0.0007(2) 0.25949(13) 0.35427(15) 0.0224(4) Uani 1 1 d . . .
C5 C 0.1278(2) 0.30201(11) 0.38301(15) 0.0210(4) Uani 1 1 d . . .
C6 C 0.3553(3) 0.2779(2) 0.4996(2) 0.0391(7) Uani 1 1 d . . .
C7 C 0.1816(4) 0.12653(16) 0.53431(18) 0.0342(6) Uani 1 1 d . . .
C8 C -0.1215(3) 0.13210(18) 0.4026(2) 0.0380(7) Uani 1 1 d . . .
C9 C -0.1265(3) 0.2874(2) 0.2921(2) 0.0450(8) Uani 1 1 d . . .
C10 C 0.1558(4) 0.38392(14) 0.3620(2) 0.0416(7) Uani 1 1 d . . .
C11 C 0.4119(2) 0.08410(12) 0.18747(15) 0.0203(4) Uani 1 1 d . . .
C12 C 0.3751(2) 0.05360(12) 0.28073(15) 0.0223(4) Uani 1 1 d . . .
C13 C 0.2207(2) 0.03426(11) 0.28026(15) 0.0220(4) Uani 1 1 d . . .
C14 C 0.1612(2) 0.05475(12) 0.18759(15) 0.0204(4) Uani 1 1 d . . .
C15 C 0.2791(2) 0.08492(12) 0.12990(14) 0.0193(4) Uani 1 1 d . . .
C16 C 0.5673(3) 0.10189(16) 0.1526(2) 0.0306(5) Uani 1 1 d . . .
C17 C 0.4856(4) 0.03597(19) 0.3609(2) 0.0391(7) Uani 1 1 d . . .
C18 C 0.1431(4) -0.01435(15) 0.3547(2) 0.0354(6) Uani 1 1 d . . .
C19 C 0.0055(3) 0.03775(17) 0.1512(2) 0.0329(6) Uani 1 1 d . . .
C20 C 0.2696(3) 0.10357(15) 0.02224(17) 0.0289(5) Uani 1 1 d . . .
C21 C 0.4423(3) 0.27820(14) 0.23491(18) 0.0275(5) Uani 1 1 d . . .
C22 C 0.3650(3) 0.26897(13) 0.14692(16) 0.0245(5) Uani 1 1 d . . .
C23 C 0.2122(3) 0.28020(14) 0.13293(17) 0.0272(5) Uani 1 1 d . . .
H6A H 0.403(4) 0.320(2) 0.469(3) 0.077(12) Uiso 1 1 d . . .
H6B H 0.416(5) 0.239(2) 0.510(3) 0.097(15) Uiso 1 1 d . . .
H6C H 0.337(4) 0.2982(19) 0.561(3) 0.070(11) Uiso 1 1 d . . .
H7A H 0.129(4) 0.0840(19) 0.532(2) 0.061(10) Uiso 1 1 d . . .
H7B H 0.173(3) 0.1459(16) 0.600(2) 0.042(7) Uiso 1 1 d . . .
H7C H 0.282(3) 0.1094(17) 0.529(2) 0.048(9) Uiso 1 1 d . . .
H8A H -0.086(5) 0.091(3) 0.440(3) 0.119(17) Uiso 1 1 d . . .
H8B H -0.141(3) 0.1112(15) 0.340(2) 0.040(8) Uiso 1 1 d . . .
H8C H -0.208(4) 0.152(2) 0.431(3) 0.075(11) Uiso 1 1 d . . .
H9A H -0.163(4) 0.254(2) 0.243(3) 0.078(11) Uiso 1 1 d . . .
H9B H -0.103(4) 0.328(2) 0.256(3) 0.067(12) Uiso 1 1 d . . .
H9C H -0.203(4) 0.3004(19) 0.328(3) 0.069(11) Uiso 1 1 d . . .
H10A H 0.256(4) 0.397(2) 0.371(3) 0.087(13) Uiso 1 1 d . . .
H10B H 0.107(4) 0.4151(19) 0.407(2) 0.064(10) Uiso 1 1 d . . .
H10C H 0.125(4) 0.3989(19) 0.304(3) 0.067(11) Uiso 1 1 d . . .
H16A H 0.566(3) 0.1371(17) 0.099(2) 0.050(9) Uiso 1 1 d . . .
H16B H 0.612(3) 0.0551(19) 0.132(2) 0.061(9) Uiso 1 1 d . . .
H16C H 0.629(3) 0.1213(16) 0.201(2) 0.046(8) Uiso 1 1 d . . .
H17A H 0.438(3) 0.0181(18) 0.419(2) 0.060(10) Uiso 1 1 d . . .
H17B H 0.527(5) 0.075(2) 0.386(3) 0.099(15) Uiso 1 1 d . . .
H17C H 0.553(4) 0.002(3) 0.343(3) 0.096(14) Uiso 1 1 d . . .
H18A H 0.187(4) -0.0131(19) 0.417(3) 0.069(11) Uiso 1 1 d . . .
H18B H 0.143(3) -0.0636(18) 0.341(2) 0.051(9) Uiso 1 1 d . . .
H18C H 0.044(4) -0.0004(18) 0.366(2) 0.060(10) Uiso 1 1 d . . .
H19A H -0.023(5) 0.066(3) 0.109(3) 0.119(18) Uiso 1 1 d . . .
H19B H -0.056(4) 0.031(2) 0.198(3) 0.074(12) Uiso 1 1 d . . .
H19C H -0.005(4) -0.010(2) 0.122(3) 0.083(12) Uiso 1 1 d . . .
H20A H 0.345(3) 0.1371(17) 0.001(2) 0.045(8) Uiso 1 1 d . . .
H20B H 0.174(3) 0.1270(16) 0.004(2) 0.049(8) Uiso 1 1 d . . .
H20C H 0.282(4) 0.058(2) -0.014(2) 0.071(10) Uiso 1 1 d . . .
H21A H 0.406(3) 0.3152(14) 0.282(2) 0.036(7) Uiso 1 1 d . . .
H21B H 0.545(3) 0.2633(14) 0.2364(17) 0.030(7) Uiso 1 1 d . . .
H22A H 0.418(2) 0.2406(12) 0.0942(16) 0.018(6) Uiso 1 1 d . . .
H23A H 0.159(3) 0.3155(15) 0.175(2) 0.042(8) Uiso 1 1 d . . .
H23B H 0.169(3) 0.2669(14) 0.0687(19) 0.036(7) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01683(10) 0.01398(9) 0.01441(10) 0.00050(8) 0.00297(6) -0.00195(8)
C1 0.0204(11) 0.0250(11) 0.0165(10) -0.0065(8) 0.0028(8) -0.0039(8)
C2 0.0258(11) 0.0206(10) 0.0150(9) -0.0011(9) 0.0052(8) 0.0014(9)
C3 0.0215(10) 0.0255(11) 0.0194(10) -0.0074(9) 0.0083(8) -0.0049(9)
C4 0.0199(11) 0.0296(11) 0.0178(10) -0.0040(9) 0.0040(8) 0.0054(9)
C5 0.0281(11) 0.0170(10) 0.0179(10) -0.0038(8) 0.0079(8) -0.0001(8)
C6 0.0307(14) 0.0573(19) 0.0293(14) -0.0142(14) -0.0037(11) -0.0116(14)
C7 0.0533(18) 0.0297(14) 0.0197(12) 0.0040(10) 0.0068(11) 0.0113(13)
C8 0.0296(14) 0.0445(16) 0.0399(15) -0.0210(14) 0.0186(12) -0.0179(12)
C9 0.0327(16) 0.073(2) 0.0289(14) -0.0049(16) -0.0036(12) 0.0246(15)
C10 0.069(2) 0.0169(12) 0.0395(16) -0.0010(11) 0.0204(15) 0.0002(13)
C11 0.0199(10) 0.0198(10) 0.0213(10) -0.0022(8) 0.0030(8) 0.0029(8)
C12 0.0281(12) 0.0179(10) 0.0208(10) 0.0007(9) 0.0007(9) 0.0055(9)
C13 0.0309(12) 0.0122(9) 0.0230(10) -0.0003(8) 0.0077(9) 0.0001(9)
C14 0.0220(11) 0.0156(10) 0.0235(10) -0.0048(8) 0.0036(8) -0.0009(8)
C15 0.0232(11) 0.0179(10) 0.0170(10) -0.0042(8) 0.0021(8) 0.0014(8)
C16 0.0226(12) 0.0353(14) 0.0339(14) -0.0018(12) 0.0061(10) 0.0025(10)
C17 0.0454(17) 0.0442(17) 0.0278(13) 0.0032(13) -0.0072(12) 0.0135(14)
C18 0.0519(18) 0.0193(13) 0.0352(15) 0.0017(11) 0.0186(13) -0.0032(12)
C19 0.0269(13) 0.0332(15) 0.0387(15) -0.0064(12) -0.0012(11) -0.0069(11)
C20 0.0387(15) 0.0304(13) 0.0176(11) -0.0013(10) 0.0018(10) 0.0013(11)
C21 0.0227(12) 0.0279(12) 0.0320(13) 0.0029(10) 0.0070(10) -0.0090(10)
C22 0.0275(12) 0.0215(11) 0.0244(11) 0.0057(9) 0.0066(9) -0.0076(9)
C23 0.0329(13) 0.0268(12) 0.0219(11) 0.0059(10) 0.0022(10) -0.0024(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100828.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 20:09:12 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210313 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100828.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100828
loop_
_publ_author_name
'Suzuki, Noriyuki'
'Watanabe, Takaaki'
'Iwasaki, Masakazu'
'Chihara, Teiji'
_publ_section_title
;
Reaction of 1-Zirconacyclopent-3-yne with "Zirconocene":
Synthesis and Structure of Bimetallic 1,2,3-Butatriene Complexes
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2065
_journal_page_last 2069
_journal_paper_doi 10.1021/om049288h
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C14 H14 Zr'
_chemical_formula_sum 'C14 H14 Zr'
_chemical_formula_weight 273.48
_chemical_melting_point ?
_space_group_IT_number 9
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 9
_symmetry_space_group_name_Hall 'C -2yc'
_symmetry_space_group_name_H-M 'C 1 c 1'
_cell_angle_alpha 90
_cell_angle_beta 91.525(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.1150(4)
_cell_length_b 9.2921(3)
_cell_length_c 9.9839(2)
_cell_measurement_reflns_used 13461
_cell_measurement_temperature 113.2
_cell_measurement_theta_max 30.0
_cell_measurement_theta_min 2.0
_cell_volume 1123.52(5)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9550
_diffrn_measured_fraction_theta_max 0.9550
_diffrn_measurement_device_type 'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.017
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 3688
_diffrn_reflns_theta_full 30.03
_diffrn_reflns_theta_max 30.03
_exptl_absorpt_coefficient_mu 0.939
_exptl_absorpt_correction_T_max 0.954
_exptl_absorpt_correction_T_min 0.774
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details '(Higashi, 1999)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.617
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.050
_exptl_crystal_size_rad ?
_refine_diff_density_max 0.38
_refine_diff_density_min -1.18
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-8'
_refine_ls_abs_structure_Flack 0.43(5)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.929
_refine_ls_hydrogen_treatment ?
_refine_ls_number_parameters 153
_refine_ls_number_reflns 2965
_refine_ls_R_factor_gt 0.0242
_refine_ls_shift/su_max 0.0022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0677
_reflns_number_gt 2780
_reflns_number_total 1573
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_duplicate_entry 4060460
_cod_database_code 1100828
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.111(2) 0.22802(2) 0.402(2) 0.01115(5) Uani 1.00 d . . .
C1 C -0.018(2) 0.2994(4) 0.569(2) 0.0184(7) Uani 1.00 d . . .
C2 C -0.054(2) 0.1741(4) 0.502(2) 0.0178(6) Uani 1.00 d . . .
C3 C -0.041(2) 0.0782(4) 0.418(2) 0.0197(7) Uani 1.00 d . . .
C4 C 0.020(2) 0.0127(4) 0.316(2) 0.0248(8) Uani 1.00 d . . .
C5 C 0.063(2) 0.3053(4) 0.163(2) 0.0247(8) Uani 1.00 d . . .
C6 C 0.175(2) 0.3447(5) 0.187(2) 0.0294(8) Uani 1.00 d . . .
C7 C 0.176(2) 0.4525(4) 0.287(2) 0.0290(8) Uani 1.00 d . . .
C8 C 0.067(2) 0.4787(4) 0.326(2) 0.0251(7) Uani 1.00 d . . .
C9 C -0.003(2) 0.3877(4) 0.249(2) 0.0195(7) Uani 1.00 d . . .
C10 C 0.291(2) 0.2756(5) 0.526(2) 0.0326(9) Uani 1.00 d . . .
C11 C 0.225(2) 0.2007(4) 0.618(2) 0.0225(8) Uani 1.00 d . . .
C12 C 0.207(2) 0.0610(4) 0.568(2) 0.0193(7) Uani 1.00 d . . .
C13 C 0.263(2) 0.0478(5) 0.447(2) 0.0291(9) Uani 1.00 d . . .
C14 C 0.315(2) 0.1808(6) 0.421(2) 0.0357(9) Uani 1.00 d . . .
H1a H 0.004(5) 0.275(5) 0.662(6) 0.03(1) Uiso 1.00 calc . . .
H1b H -0.060(4) 0.381(6) 0.563(4) 0.026(9) Uiso 1.00 calc . . .
H4a H 0.047(4) -0.087(6) 0.333(5) 0.04(1) Uiso 1.00 calc . . .
H4b H -0.015(5) 0.008(6) 0.219(6) 0.05(1) Uiso 1.00 calc . . .
H5 H 0.0348 0.2362 0.0989 0.0299 Uiso 1.00 calc . . .
H6 H 0.2359 0.3055 0.1431 0.0356 Uiso 1.00 calc . . .
H7 H 0.2391 0.4990 0.3237 0.0350 Uiso 1.00 calc . . .
H8 H 0.0428 0.5463 0.3907 0.0304 Uiso 1.00 calc . . .
H9 H -0.0830 0.3822 0.2541 0.0237 Uiso 1.00 calc . . .
H10 H 0.3116 0.3738 0.5333 0.0398 Uiso 1.00 calc . . .
H11 H 0.1953 0.2381 0.6984 0.0270 Uiso 1.00 calc . . .
H12 H 0.1639 -0.0130 0.6104 0.0229 Uiso 1.00 calc . . .
H13 H 0.2628 -0.0360 0.3902 0.0350 Uiso 1.00 calc . . .
H14 H 0.3582 0.2026 0.3458 0.0431 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Zr Zr -2.967 0.560
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100829.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 20:09:12 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210313 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100829.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100829
loop_
_publ_author_name
'Suzuki, Noriyuki'
'Watanabe, Takaaki'
'Iwasaki, Masakazu'
'Chihara, Teiji'
_publ_section_title
;
Reaction of 1-Zirconacyclopent-3-yne with "Zirconocene":
Synthesis and Structure of Bimetallic 1,2,3-Butatriene Complexes
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2065
_journal_page_last 2069
_journal_paper_doi 10.1021/om049288h
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C24 H24 Zr2 '
_chemical_formula_sum 'C24 H24 Zr2'
_chemical_formula_weight 494.89
_chemical_melting_point ?
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 91.116(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.7249(6)
_cell_length_b 7.9789(6)
_cell_length_c 13.8141(8)
_cell_measurement_reflns_used 25483
_cell_measurement_temperature 93.2
_cell_measurement_theta_max 25.0
_cell_measurement_theta_min 1.5
_cell_volume 961.5(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9906
_diffrn_measured_fraction_theta_max 0.9906
_diffrn_measurement_device_type 'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.056
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 8284
_diffrn_reflns_theta_full 25.02
_diffrn_reflns_theta_max 25.02
_exptl_absorpt_coefficient_mu 1.088
_exptl_absorpt_correction_T_max 0.897
_exptl_absorpt_correction_T_min 0.512
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(Higashi, 1995)'
_exptl_crystal_colour dark
_exptl_crystal_density_diffrn 1.709
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description cubic
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_exptl_crystal_size_rad ?
_refine_diff_density_max 0.76
_refine_diff_density_min -1.21
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack ?
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.575
_refine_ls_hydrogen_treatment ?
_refine_ls_number_parameters 126
_refine_ls_number_reflns 1687
_refine_ls_R_factor_gt 0.0558
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1353
_reflns_number_gt 1511
_reflns_number_total 1687
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_duplicate_entry 4060461
_cod_original_formula_sum 'C24 H24 Zr2 '
_cod_database_code 1100829
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.19494(6) 0.17288(8) 0.01246(4) 0.0195(2) Uani 1.00 d . . .
C1 C 0.2030(6) -0.1028(9) 0.0389(4) 0.021(2) Uani 1.00 d . . .
C2 C 0.0369(7) -0.0732(8) 0.0133(4) 0.019(2) Uani 1.00 d . . .
C3 C 0.247(1) 0.103(1) -0.1609(5) 0.051(3) Uani 1.00 d . . .
C4 C 0.1825(8) 0.268(1) -0.1611(5) 0.035(2) Uani 1.00 d . . .
C5 C 0.2892(9) 0.3691(10) -0.1167(5) 0.040(2) Uani 1.00 d . . .
C6 C 0.4150(8) 0.277(1) -0.0860(5) 0.044(2) Uani 1.00 d . . .
C7 C 0.3924(9) 0.119(1) -0.1138(5) 0.044(2) Uani 1.00 d . . .
C8 C 0.2853(10) 0.200(1) 0.1864(5) 0.049(3) Uani 1.00 d . . .
C9 C 0.328(1) 0.340(1) 0.1414(6) 0.060(3) Uani 1.00 d . . .
C10 C 0.190(2) 0.4303(9) 0.1122(6) 0.073(3) Uani 1.00 d . . .
C11 C 0.0694(9) 0.3284(10) 0.1490(5) 0.038(2) Uani 1.00 d . . .
C12 C 0.1316(9) 0.195(1) 0.1903(5) 0.040(2) Uani 1.00 d . . .
H1a H 0.265(9) -0.177(9) -0.007(5) 0.04(2) Uiso 1.00 d . . .
H1b H 0.208(8) -0.151(8) 0.110(5) 0.04(2) Uiso 1.00 d . . .
H3 H 0.1984 0.0027 -0.1870 0.0627 Uiso 1.00 calc . . .
H4 H 0.0840 0.3014 -0.1865 0.0446 Uiso 1.00 calc . . .
H5 H 0.2777 0.4888 -0.1075 0.0471 Uiso 1.00 calc . . .
H6 H 0.5036 0.3174 -0.0507 0.0538 Uiso 1.00 calc . . .
H7 H 0.4652 0.0294 -0.1042 0.0536 Uiso 1.00 calc . . .
H8 H 0.3543 0.1140 0.2111 0.0597 Uiso 1.00 calc . . .
H9 H 0.4329 0.3745 0.1301 0.0693 Uiso 1.00 calc . . .
H10 H 0.1825 0.5329 0.0769 0.0832 Uiso 1.00 calc . . .
H11 H -0.0390 0.3538 0.1444 0.0466 Uiso 1.00 calc . . .
H12 H 0.0726 0.1052 0.2193 0.0499 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Zr Zr -2.967 0.560
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100830.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100830.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100830
loop_
_publ_author_name
'Schuster, Oliver'
'Schmidbaur, Hubert'
_publ_section_title
;
Preparative Routes to the First Tri- and Tetra(alkynyl)gold(III)
Compounds:  (L)Au(C⋮CR) <sub>3</sub> and [ER <sub>4</sub> ]
<sup>+</sup> [Au(C⋮CR) <sub>4</sub> ] <sup>-</sup>
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2289
_journal_page_last 2296
_journal_paper_doi 10.1021/om050038q
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C28 H26 Au Cl2 P'
_chemical_formula_weight 661.32
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 117.6930(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.1163(2)
_cell_length_b 16.2269(3)
_cell_length_c 14.1022(3)
_cell_measurement_reflns_used 67806
_cell_measurement_temperature 143(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 2657.65(9)
_diffrn_ambient_temperature 143(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'NONIUS DIP 2020'
_diffrn_measurement_method phi-rotation
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.084
_diffrn_reflns_av_sigmaI/netI 0.0373
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 67806
_diffrn_reflns_theta_max 25.39
_diffrn_reflns_theta_min 2.51
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.810
_exptl_absorpt_correction_T_max 0.8160
_exptl_absorpt_correction_T_min 0.4440
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.653
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1288
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.124
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 292
_refine_ls_number_reflns 4834
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.124
_refine_ls_R_factor_all 0.0407
_refine_ls_R_factor_gt 0.0371
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+4.6670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0937
_refine_ls_wR_factor_ref 0.0961
_reflns_number_gt 4444
_reflns_number_total 4834
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100830
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C33 C 0.7871(4) 0.5388(3) 0.2908(4) 0.0278(11) Uani 1 1 d . . .
C32 C 0.6994(4) 0.4948(3) 0.2004(4) 0.0272(11) Uani 1 1 d . . .
C34 C 0.7595(6) 0.5802(4) 0.3623(5) 0.0426(14) Uani 1 1 d . . .
H34 H 0.6818 0.5824 0.3497 0.051 Uiso 1 1 calc R . .
C31 C 0.6301(5) 0.4542(3) 0.1280(4) 0.0316(12) Uani 1 1 d . . .
C35 C 0.8454(8) 0.6183(4) 0.4520(6) 0.055(2) Uani 1 1 d . . .
H35 H 0.8267 0.6461 0.5012 0.067 Uiso 1 1 calc R . .
C36 C 0.9592(8) 0.6157(4) 0.4697(6) 0.057(2) Uani 1 1 d . . .
H36 H 1.0181 0.6413 0.5314 0.069 Uiso 1 1 calc R . .
C38 C 0.9007(5) 0.5377(4) 0.3102(5) 0.0413(14) Uani 1 1 d . . .
H38 H 0.9204 0.5097 0.2618 0.050 Uiso 1 1 calc R . .
C41 C 0.2514(5) 0.4110(4) 0.0099(5) 0.0399(13) Uani 1 1 d . . .
H41A H 0.2039 0.4070 0.0467 0.060 Uiso 1 1 calc R . .
H41B H 0.2217 0.3732 -0.0512 0.060 Uiso 1 1 calc R . .
H41C H 0.2487 0.4676 -0.0155 0.060 Uiso 1 1 calc R . .
C42 C 0.3957(5) 0.2834(4) 0.1553(5) 0.0393(13) Uani 1 1 d . . .
H42A H 0.4744 0.2673 0.2063 0.059 Uiso 1 1 calc R . .
H42B H 0.3637 0.2432 0.0968 0.059 Uiso 1 1 calc R . .
H42C H 0.3479 0.2852 0.1918 0.059 Uiso 1 1 calc R . .
C37 C 0.9861(6) 0.5767(4) 0.3990(6) 0.0569(19) Uani 1 1 d . . .
H37 H 1.0635 0.5761 0.4104 0.068 Uiso 1 1 calc R . .
C43 C 0.4405(5) 0.4559(4) 0.2105(5) 0.0377(13) Uani 1 1 d . . .
H43A H 0.3880 0.4513 0.2420 0.057 Uiso 1 1 calc R . .
H43B H 0.4374 0.5121 0.1839 0.057 Uiso 1 1 calc R . .
H43C H 0.5192 0.4435 0.2652 0.057 Uiso 1 1 calc R . .
Cl1 Cl 0.68889(13) 0.41723(10) 0.48934(13) 0.0464(4) Uani 1 1 d . . .
Cl2 Cl 0.54787(16) 0.40403(11) 0.59865(14) 0.0531(4) Uani 1 1 d . . .
C1 C 0.6222(6) 0.3504(4) 0.5416(6) 0.0508(16) Uani 1 1 d . . .
H1A H 0.6815 0.3148 0.5968 0.061 Uiso 1 1 calc R . .
H1B H 0.5676 0.3143 0.4836 0.061 Uiso 1 1 calc R . .
Au1 Au 0.516441(15) 0.376592(11) 0.020292(14) 0.02341(10) Uani 1 1 d . . .
P1 P 0.39795(13) 0.38413(8) 0.10140(12) 0.0270(3) Uani 1 1 d . . .
C11 C 0.6201(5) 0.3555(3) -0.0479(4) 0.0285(11) Uani 1 1 d . . .
C21 C 0.4006(5) 0.2954(3) -0.0783(4) 0.0288(11) Uani 1 1 d . . .
C13 C 0.7573(4) 0.3152(3) -0.1301(4) 0.0282(11) Uani 1 1 d . . .
C18 C 0.8429(5) 0.3684(3) -0.1230(5) 0.0324(12) Uani 1 1 d . . .
H28 H 0.8516 0.4201 -0.0884 0.039 Uiso 1 1 calc R . .
C27 C 0.0544(5) 0.1658(4) -0.3495(5) 0.0381(13) Uani 1 1 d . . .
H15 H -0.0099 0.1864 -0.4115 0.046 Uiso 1 1 calc R . .
C12 C 0.6819(5) 0.3364(3) -0.0852(4) 0.0314(11) Uani 1 1 d . . .
C22 C 0.3268(4) 0.2455(3) -0.1287(4) 0.0254(10) Uani 1 1 d . . .
C17 C 0.9160(5) 0.3481(4) -0.1650(5) 0.0374(13) Uani 1 1 d . . .
H27 H 0.9744 0.3855 -0.1590 0.045 Uiso 1 1 calc R . .
C16 C 0.9040(5) 0.2724(4) -0.2164(5) 0.0396(14) Uani 1 1 d . . .
H26 H 0.9546 0.2579 -0.2447 0.047 Uiso 1 1 calc R . .
C14 C 0.7459(4) 0.2392(3) -0.1820(4) 0.0319(11) Uani 1 1 d . . .
H24 H 0.6883 0.2014 -0.1871 0.038 Uiso 1 1 calc R . .
C15 C 0.8182(5) 0.2189(4) -0.2258(5) 0.0377(13) Uani 1 1 d . . .
H25 H 0.8084 0.1680 -0.2623 0.045 Uiso 1 1 calc R . .
C26 C 0.0608(5) 0.0826(4) -0.3241(5) 0.0405(14) Uani 1 1 d . . .
H16 H 0.0012 0.0460 -0.3686 0.049 Uiso 1 1 calc R . .
C23 C 0.2367(4) 0.1896(3) -0.1936(4) 0.0258(10) Uani 1 1 d . . .
C24 C 0.2431(5) 0.1059(4) -0.1680(4) 0.0350(12) Uani 1 1 d . . .
H18 H 0.3074 0.0851 -0.1062 0.042 Uiso 1 1 calc R . .
C28 C 0.1415(4) 0.2184(3) -0.2848(4) 0.0297(11) Uani 1 1 d . . .
H14 H 0.1365 0.2752 -0.3025 0.036 Uiso 1 1 calc R . .
C25 C 0.1548(6) 0.0537(4) -0.2334(5) 0.0437(15) Uani 1 1 d . . .
H17 H 0.1589 -0.0031 -0.2156 0.052 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C33 0.027(3) 0.026(3) 0.028(3) 0.002(2) 0.011(2) -0.001(2)
C32 0.021(2) 0.027(3) 0.034(3) -0.001(2) 0.012(2) -0.003(2)
C34 0.050(4) 0.042(3) 0.043(3) -0.004(3) 0.028(3) -0.010(3)
C31 0.026(3) 0.038(3) 0.038(3) 0.001(2) 0.020(2) 0.002(2)
C35 0.089(6) 0.046(4) 0.032(3) -0.007(3) 0.028(4) -0.015(3)
C36 0.061(5) 0.045(4) 0.034(4) 0.002(3) -0.005(3) -0.012(3)
C38 0.031(3) 0.032(3) 0.054(4) -0.005(3) 0.013(3) 0.002(2)
C41 0.029(3) 0.054(4) 0.042(3) -0.003(3) 0.021(3) 0.001(3)
C42 0.043(3) 0.045(3) 0.041(3) 0.003(3) 0.028(3) -0.003(3)
C37 0.027(3) 0.045(4) 0.069(5) 0.002(3) -0.003(3) 0.001(3)
C43 0.040(3) 0.046(3) 0.037(3) -0.012(3) 0.026(3) -0.002(3)
Cl1 0.0384(8) 0.0547(9) 0.0461(8) -0.0046(7) 0.0196(7) -0.0063(7)
Cl2 0.0578(10) 0.0575(10) 0.0531(9) -0.0127(8) 0.0335(8) -0.0082(8)
C1 0.044(4) 0.041(3) 0.069(4) 0.004(3) 0.028(3) 0.005(3)
Au1 0.02207(14) 0.02626(14) 0.02561(15) -0.00191(7) 0.01419(11) -0.00243(7)
P1 0.0264(7) 0.0320(7) 0.0279(7) -0.0030(5) 0.0170(6) -0.0025(5)
C11 0.030(3) 0.025(3) 0.038(3) -0.002(2) 0.023(3) -0.001(2)
C21 0.033(3) 0.035(3) 0.027(3) 0.002(2) 0.021(2) 0.005(2)
C13 0.025(3) 0.037(3) 0.024(2) 0.005(2) 0.013(2) 0.004(2)
C18 0.031(3) 0.032(3) 0.036(3) 0.002(2) 0.018(3) 0.003(2)
C27 0.029(3) 0.049(4) 0.034(3) -0.005(3) 0.013(2) -0.001(3)
C12 0.032(3) 0.034(3) 0.031(3) 0.003(2) 0.017(2) -0.002(2)
C22 0.026(3) 0.026(2) 0.027(2) -0.003(2) 0.015(2) -0.005(2)
C17 0.032(3) 0.045(3) 0.042(3) 0.011(3) 0.023(3) 0.003(3)
C16 0.035(3) 0.050(4) 0.046(3) 0.007(3) 0.029(3) 0.010(3)
C14 0.025(3) 0.033(3) 0.036(3) 0.003(2) 0.013(2) 0.003(2)
C15 0.043(3) 0.037(3) 0.039(3) 0.001(2) 0.024(3) 0.011(3)
C26 0.038(3) 0.041(3) 0.040(3) -0.008(3) 0.016(3) -0.012(3)
C23 0.024(3) 0.032(3) 0.027(2) -0.004(2) 0.016(2) -0.003(2)
C24 0.037(3) 0.038(3) 0.026(3) -0.001(2) 0.012(2) -0.005(2)
C28 0.030(3) 0.029(3) 0.030(3) -0.001(2) 0.015(2) 0.004(2)
C25 0.057(4) 0.032(3) 0.040(3) -0.004(2) 0.021(3) -0.011(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100831.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100831.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100831
loop_
_publ_author_name
'Schuster, Oliver'
'Schmidbaur, Hubert'
_publ_section_title
;
Preparative Routes to the First Tri- and Tetra(alkynyl)gold(III)
Compounds:  (L)Au(C⋮CR) <sub>3</sub> and [ER <sub>4</sub> ]
<sup>+</sup> [Au(C⋮CR) <sub>4</sub> ] <sup>-</sup>
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2289
_journal_page_last 2296
_journal_paper_doi 10.1021/om050038q
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C32 H46 Au N'
_chemical_formula_weight 641.66
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 17.27720(10)
_cell_length_b 18.3213(2)
_cell_length_c 18.6586(2)
_cell_measurement_reflns_used 124873
_cell_measurement_temperature 143(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 5906.21(10)
_diffrn_ambient_temperature 143(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'NONIUS DIP 2020'
_diffrn_measurement_method phi-rotation
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.072
_diffrn_reflns_av_sigmaI/netI 0.0223
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 124873
_diffrn_reflns_theta_max 25.40
_diffrn_reflns_theta_min 2.36
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.000
_exptl_absorpt_correction_T_max 0.743
_exptl_absorpt_correction_T_min 0.305
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.443
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2592
_exptl_crystal_size_max 1.00
_exptl_crystal_size_mid 1.00
_exptl_crystal_size_min 0.20
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 311
_refine_ls_number_reflns 5427
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0426
_refine_ls_R_factor_gt 0.0400
_refine_ls_shift/su_max 0.070
_refine_ls_shift/su_mean 0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+6.5974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1229
_refine_ls_wR_factor_ref 0.1260
_reflns_number_gt 5040
_reflns_number_total 5427
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M Pbca
_cod_database_code 1100831
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C132 C 0.5433(2) -0.0971(2) 0.0939(2) 0.0294(9) Uani 1 1 d . . .
H32A H 0.5816 -0.0999 0.0545 0.035 Uiso 1 1 calc R . .
H32B H 0.5440 -0.1441 0.1200 0.035 Uiso 1 1 calc R . .
C141 C 0.6599(2) 0.0263(2) 0.2232(2) 0.0261(8) Uani 1 1 d . . .
H44A H 0.6531 0.0689 0.1912 0.031 Uiso 1 1 calc R . .
H44B H 0.7146 0.0258 0.2390 0.031 Uiso 1 1 calc R . .
C122 C 0.7225(2) -0.1248(2) 0.2653(2) 0.0304(8) Uani 1 1 d . . .
H12A H 0.7396 -0.0803 0.2909 0.036 Uiso 1 1 calc R . .
H12B H 0.7626 -0.1377 0.2296 0.036 Uiso 1 1 calc R . .
C21 C 0.8346(3) 0.1522(2) 0.4282(2) 0.0367(9) Uani 1 1 d . . .
C11 C 0.8836(2) 0.0172(3) 0.2671(2) 0.0364(9) Uani 1 1 d . . .
C142 C 0.6085(2) 0.0370(2) 0.2894(2) 0.0322(9) Uani 1 1 d . . .
H42A H 0.5533 0.0350 0.2753 0.039 Uiso 1 1 calc R . .
H42B H 0.6183 -0.0024 0.3245 0.039 Uiso 1 1 calc R . .
C112 C 0.7089(2) 0.0068(2) 0.0647(2) 0.0298(8) Uani 1 1 d . . .
H11A H 0.6646 -0.0019 0.0322 0.036 Uiso 1 1 calc R . .
H11B H 0.7035 0.0563 0.0854 0.036 Uiso 1 1 calc R . .
C24 C 0.8645(2) 0.2753(3) 0.5739(3) 0.0376(10) Uani 1 1 d . . .
H24 H 0.9149 0.2753 0.5536 0.045 Uiso 1 1 calc R . .
C12 C 0.9056(2) -0.0294(3) 0.2261(2) 0.0365(9) Uani 1 1 d . . .
C124 C 0.7903(3) -0.2092(3) 0.3516(2) 0.0410(11) Uani 1 1 d . . .
H12C H 0.8221 -0.2336 0.3153 0.062 Uiso 1 1 calc R . .
H12D H 0.7813 -0.2426 0.3917 0.062 Uiso 1 1 calc R . .
H12E H 0.8172 -0.1656 0.3689 0.062 Uiso 1 1 calc R . .
C13 C 0.9390(3) -0.0889(3) 0.1849(3) 0.0398(12) Uani 1 1 d . . .
C28 C 0.7314(3) 0.2379(3) 0.5713(3) 0.0395(10) Uani 1 1 d . . .
H28 H 0.6900 0.2121 0.5494 0.047 Uiso 1 1 calc R . .
C133 C 0.4629(3) -0.0841(2) 0.0628(2) 0.0322(9) Uani 1 1 d . . .
H33A H 0.4243 -0.0838 0.1020 0.039 Uiso 1 1 calc R . .
H33B H 0.4615 -0.0357 0.0391 0.039 Uiso 1 1 calc R . .
C23 C 0.8055(3) 0.2351(2) 0.5411(2) 0.0341(9) Uani 1 1 d . . .
C114 C 0.7862(3) 0.0545(3) -0.0397(3) 0.0461(11) Uani 1 1 d . . .
H11C H 0.7460 0.0413 -0.0744 0.069 Uiso 1 1 calc R . .
H11D H 0.8371 0.0522 -0.0629 0.069 Uiso 1 1 calc R . .
H11E H 0.7770 0.1042 -0.0223 0.069 Uiso 1 1 calc R . .
C113 C 0.7841(3) 0.0015(3) 0.0231(2) 0.0389(10) Uani 1 1 d . . .
H11F H 0.7905 -0.0489 0.0050 0.047 Uiso 1 1 calc R . .
H11G H 0.8280 0.0121 0.0557 0.047 Uiso 1 1 calc R . .
C22 C 0.8211(3) 0.1902(2) 0.4791(2) 0.0342(9) Uani 1 1 d . . .
C123 C 0.7131(2) -0.1872(2) 0.3187(2) 0.0305(8) Uani 1 1 d . . .
H12F H 0.6772 -0.1721 0.3573 0.037 Uiso 1 1 calc R . .
H12G H 0.6901 -0.2299 0.2940 0.037 Uiso 1 1 calc R . .
C18 C 0.9646(3) -0.0785(3) 0.1147(3) 0.0543(15) Uani 1 1 d . . .
H18 H 0.9570 -0.0328 0.0917 0.065 Uiso 1 1 calc R . .
C134 C 0.4418(3) -0.1425(3) 0.0090(3) 0.0424(11) Uani 1 1 d . . .
H34A H 0.4782 -0.1409 -0.0313 0.064 Uiso 1 1 calc R . .
H34B H 0.3891 -0.1339 -0.0086 0.064 Uiso 1 1 calc R . .
H34C H 0.4443 -0.1905 0.0320 0.064 Uiso 1 1 calc R . .
C143 C 0.6263(3) 0.1106(3) 0.3232(3) 0.0421(10) Uani 1 1 d . . .
H43A H 0.6145 0.1498 0.2883 0.051 Uiso 1 1 calc R . .
H43B H 0.6821 0.1132 0.3347 0.051 Uiso 1 1 calc R . .
C144 C 0.5795(3) 0.1231(3) 0.3912(3) 0.0530(13) Uani 1 1 d . . .
H44C H 0.5241 0.1210 0.3799 0.080 Uiso 1 1 calc R . .
H44D H 0.5921 0.1711 0.4111 0.080 Uiso 1 1 calc R . .
H44E H 0.5921 0.0851 0.4263 0.080 Uiso 1 1 calc R . .
C14 C 0.9497(3) -0.1563(3) 0.2174(3) 0.0521(13) Uani 1 1 d . . .
H14 H 0.9317 -0.1642 0.2649 0.062 Uiso 1 1 calc R . .
C26 C 0.7771(3) 0.3154(3) 0.6655(3) 0.0430(11) Uani 1 1 d . . .
H26 H 0.7677 0.3415 0.7087 0.052 Uiso 1 1 calc R . .
C25 C 0.8501(3) 0.3153(3) 0.6359(3) 0.0438(11) Uani 1 1 d . . .
H25 H 0.8906 0.3424 0.6577 0.053 Uiso 1 1 calc R . .
C27 C 0.7182(3) 0.2784(3) 0.6331(3) 0.0484(12) Uani 1 1 d . . .
H27 H 0.6676 0.2803 0.6530 0.058 Uiso 1 1 calc R . .
C15 C 0.9872(3) -0.2129(4) 0.1801(4) 0.0643(16) Uani 1 1 d . . .
H15 H 0.9949 -0.2588 0.2025 0.077 Uiso 1 1 calc R . .
C17 C 1.0011(3) -0.1346(4) 0.0786(3) 0.0682(18) Uani 1 1 d . . .
H17 H 1.0186 -0.1270 0.0309 0.082 Uiso 1 1 calc R . .
C16 C 1.0126(3) -0.2015(4) 0.1109(4) 0.0686(19) Uani 1 1 d . . .
H16 H 1.0380 -0.2396 0.0856 0.082 Uiso 1 1 calc R . .
Au1 Au 0.857107(10) 0.086225(9) 0.345702(9) 0.03317(12) Uani 1 1 d . . .
N1 N 0.64500(15) -0.04252(19) 0.18002(18) 0.0236(7) Uani 1 1 d . . .
C121 C 0.6462(2) -0.1100(3) 0.2273(2) 0.0279(8) Uani 1 1 d . . .
H12H H 0.6332 -0.1529 0.1975 0.033 Uiso 1 1 calc R . .
H12I H 0.6051 -0.1049 0.2640 0.033 Uiso 1 1 calc R . .
C131 C 0.5654(2) -0.0354(2) 0.1450(2) 0.0266(8) Uani 1 1 d . . .
H31A H 0.5259 -0.0327 0.1833 0.032 Uiso 1 1 calc R . .
H31B H 0.5637 0.0112 0.1182 0.032 Uiso 1 1 calc R . .
C111 C 0.7087(2) -0.0497(2) 0.1243(2) 0.0266(8) Uani 1 1 d . . .
H11H H 0.7592 -0.0472 0.1493 0.032 Uiso 1 1 calc R . .
H11I H 0.7047 -0.0987 0.1022 0.032 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C132 0.029(2) 0.025(2) 0.035(2) -0.0074(16) -0.0034(17) 0.0042(15)
C141 0.0269(17) 0.0207(19) 0.0308(19) -0.0014(15) 0.0021(16) -0.0026(14)
C122 0.0274(18) 0.028(2) 0.036(2) 0.0036(16) -0.0010(17) -0.0028(15)
C21 0.038(2) 0.034(2) 0.038(2) 0.0071(19) -0.0023(19) 0.0021(18)
C11 0.0259(19) 0.044(3) 0.039(2) -0.002(2) -0.0072(18) -0.0010(17)
C142 0.033(2) 0.035(2) 0.0288(19) -0.0032(16) 0.0035(16) -0.0033(17)
C112 0.032(2) 0.028(2) 0.0285(19) 0.0027(15) 0.0018(16) 0.0024(16)
C24 0.039(2) 0.033(2) 0.041(2) 0.004(2) 0.0083(18) 0.0032(17)
C12 0.0256(18) 0.046(3) 0.038(2) -0.010(2) -0.0035(17) 0.0000(18)
C124 0.033(2) 0.043(3) 0.047(3) 0.0143(19) -0.0020(19) 0.003(2)
C13 0.020(2) 0.051(3) 0.048(3) -0.015(2) -0.005(2) -0.0033(16)
C28 0.038(2) 0.035(2) 0.046(2) 0.0041(19) -0.003(2) 0.0027(18)
C133 0.030(2) 0.032(2) 0.035(2) -0.0044(16) -0.0040(19) 0.0005(15)
C23 0.042(2) 0.027(2) 0.034(2) 0.0067(16) 0.0002(18) 0.0057(17)
C114 0.057(3) 0.038(3) 0.044(2) 0.007(2) 0.015(2) 0.000(2)
C113 0.037(2) 0.039(2) 0.040(2) 0.0091(19) 0.0098(19) 0.0029(18)
C22 0.041(2) 0.030(2) 0.031(2) 0.0060(17) -0.0017(18) 0.0058(17)
C123 0.0304(19) 0.029(2) 0.032(2) 0.0026(16) 0.0025(17) -0.0031(16)
C18 0.040(3) 0.079(4) 0.045(3) -0.016(3) -0.008(2) 0.010(2)
C134 0.035(2) 0.045(3) 0.047(3) -0.009(2) -0.011(2) 0.0034(19)
C143 0.049(2) 0.032(3) 0.046(3) -0.013(2) 0.007(2) -0.007(2)
C144 0.053(3) 0.059(4) 0.047(3) -0.021(2) 0.008(2) 0.001(2)
C14 0.034(2) 0.050(3) 0.072(3) -0.010(3) 0.008(2) -0.012(2)
C26 0.053(3) 0.035(3) 0.041(2) -0.0009(19) 0.004(2) 0.013(2)
C25 0.047(3) 0.037(3) 0.048(3) -0.002(2) -0.003(2) 0.0021(19)
C27 0.044(3) 0.047(3) 0.055(3) 0.003(2) 0.013(2) 0.014(2)
C15 0.040(3) 0.053(3) 0.101(5) -0.028(3) 0.000(3) -0.008(2)
C17 0.045(3) 0.108(6) 0.051(3) -0.034(3) -0.009(3) 0.015(3)
C16 0.038(3) 0.087(5) 0.081(4) -0.051(4) -0.006(3) 0.004(3)
Au1 0.03299(16) 0.03280(17) 0.03373(16) 0.00065(6) -0.00257(6) 0.00486(6)
N1 0.0210(16) 0.0224(17) 0.0276(17) 0.0011(14) 0.0034(12) -0.0009(11)
C121 0.0244(19) 0.027(2) 0.032(2) 0.0026(18) -0.0028(15) -0.0058(14)
C131 0.0191(18) 0.029(2) 0.0314(19) -0.0037(15) -0.0014(15) 0.0015(15)
C111 0.0224(18) 0.025(2) 0.032(2) 0.0002(16) 0.0035(16) 0.0042(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100832.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100832.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100832
loop_
_publ_author_name
'Schuster, Oliver'
'Schmidbaur, Hubert'
_publ_section_title
;
Preparative Routes to the First Tri- and Tetra(alkynyl)gold(III)
Compounds:  (L)Au(C⋮CR) <sub>3</sub> and [ER <sub>4</sub> ]
<sup>+</sup> [Au(C⋮CR) <sub>4</sub> ] <sup>-</sup>
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2289
_journal_page_last 2296
_journal_paper_doi 10.1021/om050038q
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C82 H106 Au2 Cl4 N2'
_chemical_formula_weight 1655.42
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 78.1633(12)
_cell_angle_beta 84.1125(13)
_cell_angle_gamma 78.1765(19)
_cell_formula_units_Z 1
_cell_length_a 8.9747(2)
_cell_length_b 12.4383(3)
_cell_length_c 17.9334(5)
_cell_measurement_reflns_used 53832
_cell_measurement_temperature 143(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1913.93(8)
_diffrn_ambient_temperature 143(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'NONIUS DIP 2020'
_diffrn_measurement_method phi-rotation
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0615
_diffrn_reflns_av_sigmaI/netI 0.0513
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 25970
_diffrn_reflns_theta_max 25.35
_diffrn_reflns_theta_min 2.32
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 4.011
_exptl_absorpt_correction_T_max 0.797
_exptl_absorpt_correction_T_min 0.404
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.436
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 838
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.111
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 413
_refine_ls_number_reflns 6583
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.111
_refine_ls_R_factor_all 0.0668
_refine_ls_R_factor_gt 0.0400
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+4.6269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0763
_refine_ls_wR_factor_ref 0.0848
_reflns_number_gt 4641
_reflns_number_total 6583
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100832
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.6744(6) 0.7191(4) 0.2618(3) 0.0294(12) Uani 1 1 d . . .
Au1 Au 0.0000 0.0000 0.0000 0.03089(11) Uani 1 2 d S . .
Au2 Au 1.5000 0.5000 0.5000 0.03588(12) Uani 1 2 d S . .
C11 C 0.0693(7) -0.1473(5) 0.0700(3) 0.0350(14) Uani 1 1 d . . .
C12 C 0.1114(7) -0.2349(5) 0.1110(3) 0.0337(14) Uani 1 1 d . . .
C13 C 0.1475(7) -0.3402(5) 0.1630(4) 0.0374(15) Uani 1 1 d . . .
C14 C 0.2012(7) -0.3469(6) 0.2338(4) 0.0397(15) Uani 1 1 d . . .
H14 H 0.2226 -0.2819 0.2473 0.048 Uiso 1 1 calc R . .
C15 C 0.2244(9) -0.4485(7) 0.2856(4) 0.055(2) Uani 1 1 d . . .
H15 H 0.2595 -0.4518 0.3343 0.066 Uiso 1 1 calc R . .
C16 C 0.1970(9) -0.5426(6) 0.2666(5) 0.059(2) Uani 1 1 d . . .
H16 H 0.2106 -0.6108 0.3027 0.071 Uiso 1 1 calc R . .
C17 C 0.1493(9) -0.5402(6) 0.1949(4) 0.056(2) Uani 1 1 d . . .
H17 H 0.1347 -0.6070 0.1813 0.068 Uiso 1 1 calc R . .
C18 C 0.1231(8) -0.4390(6) 0.1432(4) 0.0421(17) Uani 1 1 d . . .
H18 H 0.0888 -0.4365 0.0944 0.051 Uiso 1 1 calc R . .
C21 C -0.2070(7) 0.0212(5) 0.0566(3) 0.0334(13) Uani 1 1 d . . .
C22 C -0.3305(7) 0.0388(5) 0.0891(3) 0.0343(14) Uani 1 1 d . . .
C23 C -0.4774(7) 0.0664(5) 0.1281(3) 0.0317(13) Uani 1 1 d . . .
C24 C -0.4941(7) 0.1303(5) 0.1858(4) 0.0356(14) Uani 1 1 d . . .
H24 H -0.4078 0.1545 0.1986 0.043 Uiso 1 1 calc R . .
C25 C -0.6332(8) 0.1584(5) 0.2239(4) 0.0430(16) Uani 1 1 d . . .
H25 H -0.6424 0.2023 0.2623 0.052 Uiso 1 1 calc R . .
C26 C -0.7599(8) 0.1231(6) 0.2065(4) 0.0455(17) Uani 1 1 d . . .
H26 H -0.8557 0.1421 0.2331 0.055 Uiso 1 1 calc R . .
C27 C -0.7460(7) 0.0599(6) 0.1501(4) 0.0429(16) Uani 1 1 d . . .
H27 H -0.8326 0.0350 0.1383 0.052 Uiso 1 1 calc R . .
C28 C -0.6071(7) 0.0328(5) 0.1108(3) 0.0367(14) Uani 1 1 d . . .
H28 H -0.5997 -0.0093 0.0715 0.044 Uiso 1 1 calc R . .
C31 C 1.3401(8) 0.4151(5) 0.4890(4) 0.0399(15) Uani 1 1 d . . .
C32 C 1.2447(7) 0.3648(5) 0.4819(4) 0.0375(14) Uani 1 1 d . . .
C33 C 1.1312(7) 0.3013(5) 0.4737(3) 0.0361(14) Uani 1 1 d . . .
C34 C 1.1738(8) 0.1985(5) 0.4499(4) 0.0409(16) Uani 1 1 d . . .
H34 H 1.2784 0.1707 0.4379 0.049 Uiso 1 1 calc R . .
C35 C 1.0652(9) 0.1364(6) 0.4437(4) 0.0485(17) Uani 1 1 d . . .
H35 H 1.0965 0.0664 0.4279 0.058 Uiso 1 1 calc R . .
C36 C 0.9135(8) 0.1745(6) 0.4601(4) 0.0461(17) Uani 1 1 d . . .
H36 H 0.8393 0.1323 0.4551 0.055 Uiso 1 1 calc R . .
C37 C 0.8702(8) 0.2775(6) 0.4843(4) 0.0495(18) Uani 1 1 d . . .
H37 H 0.7654 0.3052 0.4960 0.059 Uiso 1 1 calc R . .
C38 C 0.9767(8) 0.3384(5) 0.4913(4) 0.0397(15) Uani 1 1 d . . .
H38 H 0.9449 0.4073 0.5086 0.048 Uiso 1 1 calc R . .
C111 C 0.6064(7) 0.7359(5) 0.1846(3) 0.0298(14) Uani 1 1 d . . .
H11A H 0.5185 0.6972 0.1917 0.036 Uiso 1 1 calc R . .
H11B H 0.5668 0.8167 0.1676 0.036 Uiso 1 1 calc R . .
C112 C 0.7141(8) 0.6947(6) 0.1223(4) 0.0407(15) Uani 1 1 d . . .
H11C H 0.7491 0.6128 0.1365 0.049 Uiso 1 1 calc R . .
H11D H 0.8046 0.7306 0.1154 0.049 Uiso 1 1 calc R . .
C113 C 0.6340(9) 0.7223(6) 0.0478(4) 0.0444(16) Uani 1 1 d . . .
H11E H 0.5429 0.6870 0.0550 0.053 Uiso 1 1 calc R . .
H11F H 0.5996 0.8042 0.0336 0.053 Uiso 1 1 calc R . .
C114 C 0.7395(10) 0.6808(7) -0.0157(4) 0.058(2) Uani 1 1 d . . .
H11G H 0.8360 0.7071 -0.0179 0.087 Uiso 1 1 calc R . .
H11H H 0.6918 0.7097 -0.0644 0.087 Uiso 1 1 calc R . .
H11I H 0.7593 0.5989 -0.0059 0.087 Uiso 1 1 calc R . .
C121 C 0.7937(8) 0.7930(6) 0.2531(4) 0.0368(16) Uani 1 1 d . . .
H12A H 0.8776 0.7668 0.2170 0.044 Uiso 1 1 calc R . .
H12B H 0.7466 0.8705 0.2304 0.044 Uiso 1 1 calc R . .
C122 C 0.8609(8) 0.7946(6) 0.3274(4) 0.0424(18) Uani 1 1 d . . .
H12C H 0.9244 0.7206 0.3459 0.051 Uiso 1 1 calc R . .
H12D H 0.7775 0.8095 0.3667 0.051 Uiso 1 1 calc R . .
C123 C 0.9590(8) 0.8853(6) 0.3151(4) 0.0464(17) Uani 1 1 d . . .
H12E H 1.0208 0.8730 0.3598 0.056 Uiso 1 1 calc R . .
H12F H 1.0302 0.8776 0.2697 0.056 Uiso 1 1 calc R . .
C131 C 0.5473(7) 0.7472(5) 0.3220(3) 0.0317(13) Uani 1 1 d . . .
H13A H 0.4729 0.6976 0.3248 0.038 Uiso 1 1 calc R . .
H13B H 0.5916 0.7314 0.3723 0.038 Uiso 1 1 calc R . .
C132 C 0.4638(8) 0.8673(5) 0.3067(4) 0.0414(16) Uani 1 1 d . . .
H13C H 0.4008 0.8798 0.2624 0.050 Uiso 1 1 calc R . .
H13D H 0.5386 0.9178 0.2941 0.050 Uiso 1 1 calc R . .
C133 C 0.3615(8) 0.8942(6) 0.3769(4) 0.0444(17) Uani 1 1 d . . .
H13E H 0.2897 0.9657 0.3618 0.053 Uiso 1 1 calc R . .
H13F H 0.3004 0.8349 0.3947 0.053 Uiso 1 1 calc R . .
C141 C 0.7520(7) 0.5964(5) 0.2866(3) 0.0361(14) Uani 1 1 d . . .
H14A H 0.8404 0.5795 0.2502 0.043 Uiso 1 1 calc R . .
H14B H 0.7921 0.5876 0.3374 0.043 Uiso 1 1 calc R . .
C142 C 0.6513(8) 0.5109(5) 0.2911(4) 0.0403(15) Uani 1 1 d . . .
H14C H 0.5752 0.5163 0.3349 0.048 Uiso 1 1 calc R . .
H14D H 0.5956 0.5274 0.2440 0.048 Uiso 1 1 calc R . .
C143 C 0.7438(10) 0.3942(6) 0.3006(5) 0.058(2) Uani 1 1 d . . .
H14E H 0.8109 0.3815 0.3433 0.070 Uiso 1 1 calc R . .
H14F H 0.8094 0.3856 0.2535 0.070 Uiso 1 1 calc R . .
C144 C 0.6402(11) 0.3069(6) 0.3167(5) 0.066(2) Uani 1 1 d . . .
H14G H 0.5740 0.3163 0.3628 0.099 Uiso 1 1 calc R . .
H14H H 0.7031 0.2317 0.3243 0.099 Uiso 1 1 calc R . .
H14I H 0.5774 0.3171 0.2733 0.099 Uiso 1 1 calc R . .
Cl98 Cl 0.5427(3) 0.42483(19) 0.10324(13) 0.0703(6) Uani 1 1 d . . .
Cl99 Cl 0.8613(3) 0.3239(4) 0.0962(2) 0.1350(15) Uani 1 1 d . . .
C99 C 0.6905(10) 0.3434(8) 0.0552(5) 0.067(2) Uani 1 1 d . . .
H99A H 0.6637 0.2698 0.0562 0.080 Uiso 1 1 calc R . .
H99B H 0.7013 0.3810 0.0012 0.080 Uiso 1 1 calc R . .
C134 C 0.4495(9) 0.9036(7) 0.4422(4) 0.058(2) Uani 1 1 d . . .
H13G H 0.5137 0.8310 0.4608 0.087 Uiso 1 1 calc R . .
H13H H 0.3778 0.9261 0.4837 0.087 Uiso 1 1 calc R . .
H13I H 0.5139 0.9597 0.4244 0.087 Uiso 1 1 calc R . .
C124 C 0.8669(10) 1.0026(7) 0.3039(6) 0.070(3) Uani 1 1 d . . .
H12G H 0.8015 1.0143 0.2613 0.105 Uiso 1 1 calc R . .
H12H H 0.9359 1.0564 0.2927 0.105 Uiso 1 1 calc R . .
H12I H 0.8033 1.0133 0.3506 0.105 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.030(3) 0.030(3) 0.026(3) -0.005(2) -0.008(2) 0.000(2)
Au1 0.0326(2) 0.0297(2) 0.0283(2) -0.00178(16) -0.00261(17) -0.00442(16)
Au2 0.0355(2) 0.0349(2) 0.0346(2) -0.00263(18) -0.00327(18) -0.00398(18)
C11 0.036(4) 0.038(3) 0.031(3) -0.008(3) 0.003(3) -0.007(3)
C12 0.030(3) 0.035(3) 0.033(3) -0.004(3) -0.001(3) -0.001(3)
C13 0.029(3) 0.040(4) 0.035(3) -0.001(3) 0.001(3) 0.004(3)
C14 0.032(3) 0.047(4) 0.035(3) -0.001(3) -0.008(3) 0.001(3)
C15 0.051(5) 0.062(5) 0.037(4) 0.003(3) -0.009(3) 0.012(4)
C16 0.056(5) 0.042(4) 0.058(5) 0.010(4) 0.006(4) 0.016(4)
C17 0.071(5) 0.036(4) 0.052(5) -0.008(3) 0.008(4) 0.004(4)
C18 0.043(4) 0.045(4) 0.033(4) -0.004(3) -0.004(3) 0.002(3)
C21 0.032(3) 0.032(3) 0.034(3) -0.003(3) -0.003(3) -0.005(3)
C22 0.039(4) 0.029(3) 0.032(3) 0.000(2) -0.013(3) -0.002(3)
C23 0.030(3) 0.032(3) 0.027(3) 0.002(2) -0.005(3) 0.002(2)
C24 0.038(4) 0.030(3) 0.037(3) 0.000(3) -0.006(3) -0.008(3)
C25 0.050(4) 0.035(3) 0.041(4) -0.008(3) -0.004(3) 0.001(3)
C26 0.035(4) 0.046(4) 0.046(4) 0.001(3) 0.002(3) 0.000(3)
C27 0.030(4) 0.045(4) 0.050(4) 0.003(3) -0.016(3) -0.005(3)
C28 0.040(4) 0.037(3) 0.031(3) -0.001(3) -0.002(3) -0.007(3)
C31 0.038(4) 0.037(4) 0.038(4) 0.002(3) -0.008(3) 0.001(3)
C32 0.036(4) 0.039(4) 0.033(3) -0.002(3) -0.004(3) -0.001(3)
C33 0.043(4) 0.036(3) 0.027(3) -0.002(3) -0.004(3) -0.006(3)
C34 0.040(4) 0.039(4) 0.038(4) -0.010(3) 0.001(3) 0.006(3)
C35 0.055(5) 0.041(4) 0.052(4) -0.015(3) -0.006(4) -0.009(3)
C36 0.046(4) 0.044(4) 0.050(4) -0.004(3) -0.011(3) -0.013(3)
C37 0.039(4) 0.046(4) 0.055(4) -0.003(3) 0.005(3) 0.000(3)
C38 0.042(4) 0.038(4) 0.038(4) -0.007(3) 0.001(3) -0.007(3)
C111 0.031(3) 0.030(3) 0.027(3) -0.005(3) -0.003(3) -0.003(3)
C112 0.044(4) 0.041(4) 0.033(3) -0.001(3) -0.003(3) -0.005(3)
C113 0.062(5) 0.038(4) 0.033(3) -0.003(3) -0.009(3) -0.010(3)
C114 0.084(6) 0.058(5) 0.029(4) -0.007(3) -0.007(4) -0.006(4)
C121 0.033(4) 0.036(4) 0.040(4) -0.005(3) -0.006(3) -0.006(3)
C122 0.038(4) 0.045(4) 0.044(4) -0.006(3) -0.010(3) -0.006(3)
C123 0.036(4) 0.053(4) 0.054(4) -0.013(3) -0.013(3) -0.009(3)
C131 0.033(3) 0.036(3) 0.024(3) -0.004(2) -0.002(3) -0.004(3)
C132 0.044(4) 0.034(3) 0.039(4) 0.000(3) 0.000(3) 0.000(3)
C133 0.041(4) 0.043(4) 0.043(4) -0.005(3) 0.001(3) 0.001(3)
C141 0.043(4) 0.027(3) 0.031(3) 0.000(2) -0.006(3) 0.007(3)
C142 0.053(4) 0.028(3) 0.037(4) -0.004(3) -0.006(3) -0.003(3)
C143 0.077(6) 0.034(4) 0.061(5) -0.006(3) -0.023(4) 0.000(4)
C144 0.104(7) 0.034(4) 0.062(5) -0.007(4) -0.016(5) -0.013(4)
Cl98 0.0853(16) 0.0649(13) 0.0604(13) -0.0083(10) -0.0066(11) -0.0159(11)
Cl99 0.0608(17) 0.244(4) 0.127(3) -0.104(3) -0.0104(18) -0.018(2)
C99 0.080(6) 0.080(6) 0.048(5) -0.018(4) -0.001(4) -0.027(5)
C134 0.048(4) 0.076(5) 0.058(5) -0.040(4) 0.003(4) -0.002(4)
C124 0.055(5) 0.062(5) 0.107(7) -0.042(5) -0.008(5) -0.019(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100833.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-14 15:39:52 +0300 (Fri, 14 Apr 2023) $
#$Revision: 282633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100833.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100833
loop_
_publ_author_name
'Schuster, Oliver'
'Schmidbaur, Hubert'
_publ_section_title
;
Preparative Routes to the First Tri- and Tetra(alkynyl)gold(III)
Compounds:  (L)Au(C⋮CR) <sub>3</sub> and [ER <sub>4</sub> ]
<sup>+</sup> [Au(C⋮CR) <sub>4</sub> ] <sup>-</sup>
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2289
_journal_page_last 2296
_journal_paper_doi 10.1021/om050038q
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C36 H28 Au Cl2 P'
_chemical_formula_weight 759.42
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 83.782(5)
_cell_angle_beta 79.915(5)
_cell_angle_gamma 78.659(2)
_cell_formula_units_Z 2
_cell_length_a 8.9539(5)
_cell_length_b 12.9892(8)
_cell_length_c 15.4944(11)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 143(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1734.47(19)
_diffrn_ambient_temperature 143(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'NONIUS DIP 2020'
_diffrn_measurement_method phi-rotation
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.076
_diffrn_reflns_av_sigmaI/netI 0.0611
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 69364
_diffrn_reflns_theta_max 25.27
_diffrn_reflns_theta_min 2.51
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 4.462
_exptl_absorpt_correction_T_max 0.720
_exptl_absorpt_correction_T_min 0.269
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.454
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.182
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 373
_refine_ls_number_reflns 5443
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.182
_refine_ls_R_factor_all 0.0719
_refine_ls_R_factor_gt 0.0597
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+1.9151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1361
_refine_ls_wR_factor_ref 0.1434
_reflns_number_gt 4711
_reflns_number_total 5443
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100833
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.67197(4) 0.90662(3) 0.53982(3) 0.04972(16) Uani 1 1 d . . .
P1 P 0.8842(3) 0.7816(2) 0.37459(18) 0.0550(6) Uani 1 1 d . . .
C31 C 0.7240(11) 1.0552(8) 0.4811(7) 0.055(2) Uani 1 1 d . . .
C3 C 0.9533(13) 0.6576(8) 0.4427(8) 0.067(3) Uani 1 1 d . . .
H4A H 0.8851 0.6069 0.4432 0.100 Uiso 1 1 calc R . .
H4B H 0.9521 0.6745 0.5029 0.100 Uiso 1 1 calc R . .
H4C H 1.0587 0.6269 0.4172 0.100 Uiso 1 1 calc R . .
C21 C 0.6410(11) 0.7514(8) 0.5929(7) 0.057(2) Uani 1 1 d . . .
C12 C 0.6409(12) 0.9923(7) 0.7328(7) 0.054(2) Uani 1 1 d . . .
C2 C 1.0159(13) 0.8767(8) 0.3629(8) 0.064(3) Uani 1 1 d . . .
H9A H 1.1170 0.8459 0.3317 0.096 Uiso 1 1 calc R . .
H9B H 1.0271 0.8938 0.4213 0.096 Uiso 1 1 calc R . .
H9C H 0.9736 0.9411 0.3295 0.096 Uiso 1 1 calc R . .
C11 C 0.6474(12) 0.9644(8) 0.6609(8) 0.060(3) Uani 1 1 d . . .
C22 C 0.6360(12) 0.6556(8) 0.6212(7) 0.059(3) Uani 1 1 d . . .
C32 C 0.7696(12) 1.1373(7) 0.4423(7) 0.053(2) Uani 1 1 d . . .
C34 C 0.7437(12) 1.3390(7) 0.3888(7) 0.058(2) Uani 1 1 d . . .
H003 H 0.6411 1.3515 0.4195 0.070 Uiso 1 1 calc R . .
C42 C 0.8762(13) 0.7111(9) 0.2001(8) 0.067(3) Uani 1 1 d . . .
C43 C 0.8639(14) 0.6753(8) 0.1165(7) 0.063(3) Uani 1 1 d . . .
C33 C 0.8315(11) 1.2307(7) 0.3920(7) 0.052(2) Uani 1 1 d . . .
C23 C 0.6333(12) 0.5377(8) 0.6526(8) 0.064(3) Uani 1 1 d . . .
C38 C 0.9803(12) 1.2140(8) 0.3470(7) 0.060(3) Uani 1 1 d . . .
H008 H 1.0407 1.1451 0.3472 0.072 Uiso 1 1 calc R . .
C36 C 0.9540(13) 1.4095(8) 0.2941(8) 0.065(3) Uani 1 1 d . . .
H009 H 0.9970 1.4645 0.2592 0.078 Uiso 1 1 calc R . .
C37 C 1.0441(13) 1.3016(8) 0.2994(8) 0.066(3) Uani 1 1 d . . .
H010 H 1.1480 1.2892 0.2704 0.079 Uiso 1 1 calc R . .
C41 C 0.8873(13) 0.7392(8) 0.2724(7) 0.062(3) Uani 1 1 d . . .
C24 C 0.6223(13) 0.4614(8) 0.5915(9) 0.072(3) Uani 1 1 d . . .
H012 H 0.6213 0.4859 0.5315 0.086 Uiso 1 1 calc R . .
C46 C 0.8377(18) 0.6091(11) -0.0465(9) 0.092(4) Uani 1 1 d . . .
H013 H 0.8334 0.5862 -0.1020 0.110 Uiso 1 1 calc R . .
C35 C 0.8065(13) 1.4293(8) 0.3404(8) 0.068(3) Uani 1 1 d . . .
H014 H 0.7474 1.4986 0.3411 0.081 Uiso 1 1 calc R . .
C18 C 0.5122(16) 1.0971(9) 0.8624(8) 0.074(3) Uani 1 1 d . . .
H015 H 0.4216 1.1165 0.8360 0.089 Uiso 1 1 calc R . .
C13 C 0.6423(13) 1.0278(8) 0.8175(8) 0.063(3) Uani 1 1 d . . .
C44 C 0.7705(16) 0.5962(10) 0.1142(8) 0.079(3) Uani 1 1 d . . .
H017 H 0.7184 0.5670 0.1671 0.094 Uiso 1 1 calc R . .
C14 C 0.7758(17) 0.9998(11) 0.8571(8) 0.083(4) Uani 1 1 d . . .
H018 H 0.8646 0.9541 0.8309 0.100 Uiso 1 1 calc R . .
C48 C 0.9413(16) 0.7218(10) 0.0387(8) 0.083(4) Uani 1 1 d . . .
H019 H 1.0028 0.7730 0.0409 0.100 Uiso 1 1 calc R . .
C28 C 0.6381(15) 0.4973(11) 0.7387(9) 0.085(4) Uani 1 1 d . . .
H020 H 0.6466 0.5415 0.7820 0.102 Uiso 1 1 calc R . .
C45 C 0.7582(19) 0.5630(12) 0.0314(10) 0.095(4) Uani 1 1 d . . .
H021 H 0.6982 0.5112 0.0282 0.113 Uiso 1 1 calc R . .
C25 C 0.6128(16) 0.3498(10) 0.6161(11) 0.090(4) Uani 1 1 d . . .
H022 H 0.6045 0.3051 0.5732 0.108 Uiso 1 1 calc R . .
C17 C 0.512(2) 1.1369(11) 0.9415(8) 0.088(4) Uani 1 1 d . . .
H023 H 0.4233 1.1810 0.9695 0.105 Uiso 1 1 calc R . .
C27 C 0.6296(18) 0.3812(14) 0.7638(11) 0.106(5) Uani 1 1 d . . .
H024 H 0.6333 0.3541 0.8230 0.127 Uiso 1 1 calc R . .
C26 C 0.6161(16) 0.3120(12) 0.7006(13) 0.099(5) Uani 1 1 d . . .
H025 H 0.6095 0.2404 0.7180 0.119 Uiso 1 1 calc R . .
C47 C 0.9230(18) 0.6888(12) -0.0419(9) 0.092(4) Uani 1 1 d . . .
H026 H 0.9696 0.7211 -0.0951 0.111 Uiso 1 1 calc R . .
C15 C 0.772(2) 1.0431(14) 0.9383(10) 0.106(5) Uani 1 1 d . . .
H027 H 0.8601 1.0253 0.9667 0.127 Uiso 1 1 calc R . .
C16 C 0.642(3) 1.1111(14) 0.9778(10) 0.112(6) Uani 1 1 d . . .
H028 H 0.6458 1.1394 1.0312 0.134 Uiso 1 1 calc R . .
C1 C 0.6929(11) 0.8462(8) 0.4153(7) 0.056(2) Uani 1 1 d . . .
H02A H 0.6218 0.7956 0.4200 0.067 Uiso 1 1 calc R . .
H02B H 0.6604 0.9049 0.3723 0.067 Uiso 1 1 calc R . .
C99 C 0.6452(15) 1.1715(11) 0.2252(8) 0.081(3) Uani 1 1 d . . .
Cl2 Cl 0.7943(4) 1.0559(3) 0.1961(2) 0.0955(10) Uani 1 1 d . A .
Cl1 Cl 0.6845(6) 1.2929(3) 0.1623(3) 0.091(2) Uani 0.814(13) 1 d P A 1
Cl3 Cl 0.542(5) 1.266(3) 0.141(2) 0.18(2) Uani 0.186(13) 1 d P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0509(2) 0.0481(2) 0.0517(2) -0.00066(14) -0.01571(15) -0.00766(14)
P1 0.0578(15) 0.0557(14) 0.0541(16) -0.0038(11) -0.0177(12) -0.0090(11)
C31 0.055(6) 0.067(6) 0.048(6) -0.017(5) -0.026(4) 0.000(5)
C3 0.065(7) 0.067(6) 0.069(7) 0.003(5) -0.027(5) -0.005(5)
C21 0.048(5) 0.071(7) 0.053(6) -0.011(5) -0.015(4) -0.004(5)
C12 0.060(6) 0.056(5) 0.050(6) -0.003(4) -0.016(5) -0.013(4)
C2 0.060(6) 0.063(6) 0.067(7) 0.000(5) -0.009(5) -0.010(5)
C11 0.050(6) 0.060(6) 0.069(8) 0.002(5) -0.021(5) -0.008(4)
C22 0.052(6) 0.060(6) 0.065(7) 0.006(5) -0.017(5) -0.014(5)
C32 0.061(6) 0.043(5) 0.060(6) 0.010(4) -0.028(5) -0.014(4)
C34 0.059(6) 0.052(5) 0.065(7) -0.011(4) -0.014(5) -0.008(4)
C42 0.058(6) 0.068(7) 0.069(8) 0.004(5) -0.008(5) -0.004(5)
C43 0.083(8) 0.068(6) 0.040(6) -0.005(4) -0.017(5) -0.015(5)
C33 0.049(5) 0.053(5) 0.060(6) 0.000(4) -0.020(4) -0.016(4)
C23 0.048(6) 0.057(6) 0.083(8) 0.010(5) -0.012(5) -0.008(5)
C38 0.055(6) 0.062(6) 0.062(7) 0.008(5) -0.022(5) -0.001(5)
C36 0.067(7) 0.060(6) 0.069(7) 0.008(5) -0.018(6) -0.015(5)
C37 0.059(6) 0.067(6) 0.074(8) -0.007(5) -0.015(5) -0.012(5)
C41 0.067(7) 0.066(6) 0.056(7) -0.003(5) -0.021(5) -0.010(5)
C24 0.059(7) 0.060(6) 0.095(9) -0.004(6) -0.008(6) -0.013(5)
C46 0.114(12) 0.107(10) 0.055(8) -0.018(7) -0.017(8) -0.013(9)
C35 0.065(7) 0.047(5) 0.093(9) 0.005(5) -0.025(6) -0.010(5)
C18 0.089(9) 0.070(7) 0.059(7) 0.003(5) -0.007(6) -0.012(6)
C13 0.072(7) 0.056(6) 0.065(7) 0.009(5) -0.018(5) -0.022(5)
C44 0.084(9) 0.092(8) 0.063(8) -0.004(6) -0.018(6) -0.022(7)
C14 0.091(9) 0.101(9) 0.064(8) 0.004(6) -0.028(7) -0.024(7)
C48 0.093(9) 0.092(9) 0.062(8) -0.008(6) 0.005(7) -0.024(7)
C28 0.079(8) 0.091(9) 0.072(8) 0.027(7) -0.006(6) -0.010(7)
C45 0.109(11) 0.098(10) 0.082(11) -0.022(8) -0.026(9) -0.015(8)
C25 0.077(9) 0.068(8) 0.112(12) -0.001(7) 0.009(8) -0.011(6)
C17 0.126(12) 0.098(9) 0.042(7) -0.013(6) -0.019(7) -0.022(8)
C27 0.088(10) 0.122(12) 0.088(11) 0.034(10) -0.002(8) -0.004(9)
C26 0.074(9) 0.081(9) 0.125(14) 0.007(9) 0.008(9) -0.002(7)
C47 0.103(11) 0.121(11) 0.057(8) -0.010(7) -0.010(7) -0.030(9)
C15 0.131(14) 0.137(13) 0.072(10) 0.022(9) -0.054(10) -0.058(11)
C16 0.174(19) 0.115(12) 0.058(9) -0.013(8) -0.018(11) -0.048(12)
C1 0.049(5) 0.056(5) 0.063(7) 0.002(4) -0.020(5) -0.005(4)
C99 0.078(8) 0.105(9) 0.064(8) -0.001(6) -0.017(6) -0.027(7)
Cl2 0.087(2) 0.126(3) 0.073(2) -0.0063(19) -0.0282(17) -0.007(2)
Cl1 0.117(4) 0.078(3) 0.081(3) -0.0102(19) 0.001(3) -0.036(2)
Cl3 0.21(4) 0.19(3) 0.12(2) -0.07(2) -0.10(2) 0.10(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100834.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100834.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100834
loop_
_publ_author_name
'Schuster, Oliver'
'Schmidbaur, Hubert'
_publ_section_title
;
Preparative Routes to the First Tri- and Tetra(alkynyl)gold(III)
Compounds:  (L)Au(C⋮CR) <sub>3</sub> and [ER <sub>4</sub> ]
<sup>+</sup> [Au(C⋮CR) <sub>4</sub> ] <sup>-</sup>
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2289
_journal_page_last 2296
_journal_paper_doi 10.1021/om050038q
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C27 H24 Au P'
_chemical_formula_weight 576.40
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 82.9382(6)
_cell_angle_beta 73.8315(6)
_cell_angle_gamma 78.4370(9)
_cell_formula_units_Z 2
_cell_length_a 9.26320(10)
_cell_length_b 11.1278(2)
_cell_length_c 12.1561(2)
_cell_measurement_reflns_used 25643
_cell_measurement_temperature 143(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1176.05(3)
_diffrn_ambient_temperature 143(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'NONIUS DIP 2020'
_diffrn_measurement_method phi-rotation
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.042
_diffrn_reflns_av_sigmaI/netI 0.0316
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 25643
_diffrn_reflns_theta_max 25.47
_diffrn_reflns_theta_min 2.32
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 6.332
_exptl_absorpt_correction_T_max 0.785
_exptl_absorpt_correction_T_min 0.380
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.628
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 560
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.122
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 265
_refine_ls_number_reflns 4054
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.122
_refine_ls_R_factor_all 0.0232
_refine_ls_R_factor_gt 0.0231
_refine_ls_shift/su_max 0.041
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.6137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.0617
_reflns_number_gt 4021
_reflns_number_total 4054
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100834
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.426784(11) 0.333438(9) 0.068133(9) 0.02349(7) Uani 1 1 d . . .
P1 P 0.32273(11) 0.37522(9) -0.08817(8) 0.0279(2) Uani 1 1 d . . .
C11 C 0.5106(4) 0.2890(3) 0.2071(3) 0.0234(7) Uani 1 1 d . . .
C12 C 0.5555(4) 0.2605(3) 0.2916(3) 0.0281(7) Uani 1 1 d . . .
C13 C 0.6165(3) 0.2266(3) 0.3895(3) 0.0246(6) Uani 1 1 d . . .
C14 C 0.6406(4) 0.1042(3) 0.4331(3) 0.0312(7) Uani 1 1 d . . .
H14A H 0.6123 0.0429 0.3995 0.037 Uiso 1 1 calc R . .
C15 C 0.7053(5) 0.0715(3) 0.5244(3) 0.0383(8) Uani 1 1 d . . .
H15A H 0.7190 -0.0119 0.5539 0.046 Uiso 1 1 calc R . .
C16 C 0.7500(4) 0.1582(3) 0.5730(3) 0.0361(8) Uani 1 1 d . . .
H16A H 0.7966 0.1347 0.6346 0.043 Uiso 1 1 calc R . .
C17 C 0.7263(5) 0.2810(4) 0.5312(3) 0.0350(8) Uani 1 1 d . . .
H17A H 0.7568 0.3415 0.5645 0.042 Uiso 1 1 calc R . .
C18 C 0.6585(4) 0.3149(3) 0.4417(3) 0.0294(7) Uani 1 1 d . . .
H18A H 0.6401 0.3991 0.4152 0.035 Uiso 1 1 calc R . .
C21 C 0.5849(4) 0.2027(3) -0.0179(3) 0.0273(7) Uani 1 1 d . . .
C22 C 0.6711(4) 0.1179(3) -0.0659(3) 0.0286(8) Uani 1 1 d . . .
C23 C 0.7783(4) 0.0189(3) -0.1246(3) 0.0275(7) Uani 1 1 d . . .
C24 C 0.9312(4) -0.0017(3) -0.1233(3) 0.0319(7) Uani 1 1 d . . .
H24A H 0.9650 0.0509 -0.0836 0.038 Uiso 1 1 calc R . .
C25 C 1.0350(4) -0.0976(4) -0.1789(3) 0.0401(9) Uani 1 1 d . . .
H25A H 1.1386 -0.1111 -0.1764 0.048 Uiso 1 1 calc R . .
C26 C 0.9860(5) -0.1740(4) -0.2386(4) 0.0428(10) Uani 1 1 d . . .
H26A H 1.0567 -0.2393 -0.2777 0.051 Uiso 1 1 calc R . .
C27 C 0.8347(5) -0.1550(3) -0.2409(3) 0.0365(8) Uani 1 1 d . . .
H27A H 0.8017 -0.2073 -0.2815 0.044 Uiso 1 1 calc R . .
C28 C 0.7293(4) -0.0583(3) -0.1833(3) 0.0296(7) Uani 1 1 d . . .
H28A H 0.6252 -0.0458 -0.1845 0.036 Uiso 1 1 calc R . .
C31 C 0.2615(4) 0.4554(3) 0.1591(3) 0.0273(7) Uani 1 1 d . . .
C32 C 0.1575(4) 0.5179(3) 0.2220(3) 0.0290(8) Uani 1 1 d . . .
C33 C 0.0333(4) 0.5931(3) 0.2969(3) 0.0266(7) Uani 1 1 d . . .
C34 C 0.0204(4) 0.7207(3) 0.2862(3) 0.0288(7) Uani 1 1 d . . .
H34A H 0.0943 0.7584 0.2292 0.035 Uiso 1 1 calc R . .
C35 C -0.0994(4) 0.7929(3) 0.3581(3) 0.0364(8) Uani 1 1 d . . .
H35A H -0.1067 0.8797 0.3508 0.044 Uiso 1 1 calc R . .
C36 C -0.2090(4) 0.7390(4) 0.4410(4) 0.0410(9) Uani 1 1 d . . .
H36A H -0.2921 0.7889 0.4893 0.049 Uiso 1 1 calc R . .
C37 C -0.1965(5) 0.6124(4) 0.4528(4) 0.0435(9) Uani 1 1 d . . .
H37A H -0.2703 0.5750 0.5101 0.052 Uiso 1 1 calc R . .
C38 C -0.0760(4) 0.5400(4) 0.3809(3) 0.0380(8) Uani 1 1 d . . .
H38A H -0.0681 0.4531 0.3892 0.046 Uiso 1 1 calc R . .
C111 C 0.1969(4) 0.5213(3) -0.0922(3) 0.0353(8) Uani 1 1 d . . .
H11A H 0.1423 0.5234 -0.1511 0.053 Uiso 1 1 calc R . .
H11B H 0.2569 0.5877 -0.1107 0.053 Uiso 1 1 calc R . .
H11C H 0.1232 0.5320 -0.0172 0.053 Uiso 1 1 calc R . .
C112 C 0.2129(6) 0.2581(4) -0.0825(4) 0.0499(10) Uani 1 1 d . . .
H11D H 0.1634 0.2749 -0.1456 0.075 Uiso 1 1 calc R . .
H11E H 0.1350 0.2576 -0.0090 0.075 Uiso 1 1 calc R . .
H11F H 0.2803 0.1779 -0.0897 0.075 Uiso 1 1 calc R . .
C113 C 0.4609(5) 0.3714(4) -0.2258(3) 0.0417(9) Uani 1 1 d . . .
H11G H 0.4083 0.3807 -0.2868 0.063 Uiso 1 1 calc R . .
H11H H 0.5314 0.2926 -0.2301 0.063 Uiso 1 1 calc R . .
H11I H 0.5182 0.4387 -0.2354 0.063 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.02212(10) 0.02549(10) 0.02381(10) -0.00215(6) -0.00765(6) -0.00374(7)
P1 0.0299(5) 0.0306(4) 0.0258(4) 0.0022(3) -0.0110(4) -0.0088(4)
C11 0.0243(16) 0.0295(16) 0.0196(15) -0.0009(12) -0.0108(12) -0.0052(14)
C12 0.0192(14) 0.0276(16) 0.0362(18) -0.0051(13) -0.0021(13) -0.0067(13)
C13 0.0172(14) 0.0322(16) 0.0238(15) -0.0032(12) -0.0017(11) -0.0076(13)
C14 0.0353(18) 0.0284(16) 0.0317(17) -0.0036(13) -0.0093(14) -0.0084(14)
C15 0.051(2) 0.0301(18) 0.0366(19) 0.0012(14) -0.0168(17) -0.0087(17)
C16 0.044(2) 0.040(2) 0.0291(18) 0.0053(15) -0.0165(15) -0.0128(17)
C17 0.044(2) 0.0360(19) 0.0298(18) -0.0015(14) -0.0108(15) -0.0172(17)
C18 0.0318(17) 0.0276(15) 0.0290(17) 0.0001(12) -0.0052(13) -0.0106(14)
C21 0.0253(17) 0.0294(17) 0.0243(17) -0.0007(13) -0.0052(13) -0.0005(15)
C22 0.0296(17) 0.0307(17) 0.0255(16) 0.0028(13) -0.0076(13) -0.0078(16)
C23 0.0293(17) 0.0233(15) 0.0254(16) 0.0025(12) -0.0019(13) -0.0041(14)
C24 0.0296(17) 0.0332(17) 0.0325(18) 0.0023(14) -0.0083(14) -0.0068(15)
C25 0.0284(17) 0.041(2) 0.045(2) 0.0014(16) -0.0034(15) -0.0039(17)
C26 0.040(2) 0.034(2) 0.043(2) -0.0050(16) 0.0059(17) -0.0027(17)
C27 0.048(2) 0.0289(17) 0.0303(18) -0.0012(14) -0.0041(16) -0.0101(17)
C28 0.0282(16) 0.0373(18) 0.0205(15) 0.0012(13) -0.0028(12) -0.0060(15)
C31 0.0262(17) 0.0277(17) 0.0276(18) -0.0025(14) -0.0093(14) -0.0007(15)
C32 0.0310(18) 0.0267(17) 0.0348(18) -0.0010(14) -0.0167(15) -0.0068(15)
C33 0.0244(15) 0.0305(17) 0.0283(16) -0.0069(13) -0.0116(13) -0.0029(14)
C34 0.0273(16) 0.0282(17) 0.0330(18) -0.0026(13) -0.0094(13) -0.0074(14)
C35 0.0355(19) 0.0283(18) 0.047(2) -0.0074(15) -0.0105(16) -0.0065(16)
C36 0.0317(18) 0.0374(19) 0.051(2) -0.0163(16) -0.0009(16) -0.0047(16)
C37 0.038(2) 0.040(2) 0.048(2) -0.0101(17) 0.0051(17) -0.0150(18)
C38 0.040(2) 0.0295(18) 0.043(2) -0.0066(15) -0.0050(16) -0.0089(17)
C111 0.0302(17) 0.0388(19) 0.0372(19) 0.0052(15) -0.0123(14) -0.0064(15)
C112 0.068(3) 0.049(2) 0.048(2) 0.0131(18) -0.035(2) -0.027(2)
C113 0.047(2) 0.045(2) 0.0277(18) 0.0008(15) -0.0079(16) -0.0018(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100835.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100835.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100835
loop_
_publ_author_name
'Schaefer, Carsten'
'Werz, Daniel B.'
'Staeb, Tobias H.'
'Gleiter, Rolf'
'Rominger, Frank'
_publ_section_title
;
CpCo-Stabilized Cyclopentadienones from Cyclobutadiene Complexes:
Experimental and Theoretical Investigations
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2113
_journal_paper_doi 10.1021/om050048r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C19 H25 Co O S4 Si'
_chemical_formula_weight 484.65
_chemical_name_common in_paper_11
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 76.2750(10)
_cell_angle_beta 86.0300(10)
_cell_angle_gamma 84.9640(10)
_cell_formula_units_Z 2
_cell_length_a 8.81940(10)
_cell_length_b 8.89640(10)
_cell_length_c 14.4346(2)
_cell_measurement_temperature 200(2)
_cell_volume 1094.59(2)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0214
_diffrn_reflns_av_sigmaI/netI 0.0253
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 11392
_diffrn_reflns_theta_full 27.45
_diffrn_reflns_theta_max 27.45
_diffrn_reflns_theta_min 2.32
_exptl_absorpt_coefficient_mu 1.227
_exptl_absorpt_correction_T_max 0.8871
_exptl_absorpt_correction_T_min 0.6268
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.470
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description polyhedron
_exptl_crystal_F_000 504
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.481
_refine_diff_density_min -0.389
_refine_diff_density_rms 0.055
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 251
_refine_ls_number_reflns 4985
_refine_ls_number_restraints 11
_refine_ls_restrained_S_all 1.098
_refine_ls_R_factor_all 0.0314
_refine_ls_R_factor_gt 0.0263
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.5059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.0673
_reflns_number_gt 4434
_reflns_number_total 4985
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060509
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100835
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.11298(2) 0.70412(2) 0.281851(14) 0.01793(7) Uani 1 1 d . A .
S3 S 0.45482(5) 0.60979(5) 0.17082(4) 0.02941(11) Uani 1 1 d . . .
S4 S 0.08002(5) 0.49873(5) 0.11605(3) 0.02725(10) Uani 1 1 d . . .
Si1 Si 0.30572(7) 0.82077(8) 0.45815(4) 0.04005(14) Uani 1 1 d . . .
C1 C 0.1672(2) 0.7029(2) 0.42022(12) 0.0305(4) Uani 1 1 d . . .
C2 C 0.1979(2) 0.5524(2) 0.40021(13) 0.0340(4) Uani 1 1 d . . .
H2 H 0.2949 0.4964 0.4023 0.041 Uiso 1 1 calc R . .
C3 C 0.0604(3) 0.4998(2) 0.37677(14) 0.0384(5) Uani 1 1 d . . .
H3 H 0.0503 0.4034 0.3611 0.046 Uiso 1 1 calc R . .
C4 C -0.0575(2) 0.6156(3) 0.38089(14) 0.0383(5) Uani 1 1 d . . .
H4 H -0.1614 0.6112 0.3689 0.046 Uiso 1 1 calc R . .
C5 C 0.0072(2) 0.7408(2) 0.40636(13) 0.0339(4) Uani 1 1 d . . .
H5 H -0.0472 0.8349 0.4131 0.041 Uiso 1 1 calc R . .
C6 C 0.26048(19) 0.87108(18) 0.17645(11) 0.0220(3) Uani 1 1 d . A .
O6 O 0.36490(15) 0.95034(15) 0.18459(10) 0.0346(3) Uani 1 1 d . . .
C9 C 0.27291(17) 0.70679(18) 0.17079(11) 0.0190(3) Uani 1 1 d . . .
C10 C 0.12809(17) 0.66467(17) 0.15001(11) 0.0182(3) Uani 1 1 d . . .
C11 C 0.5001(3) 0.7582(4) 0.41699(19) 0.0567(6) Uani 1 1 d . . .
H11A H 0.5238 0.6486 0.4472 0.085 Uiso 1 1 calc R . .
H11B H 0.5745 0.8209 0.4345 0.085 Uiso 1 1 calc R . .
H11C H 0.5047 0.7722 0.3475 0.085 Uiso 1 1 calc R . .
C12 C 0.2569(3) 1.0307(3) 0.40702(19) 0.0588(7) Uani 1 1 d . . .
H12A H 0.2777 1.0539 0.3377 0.088 Uiso 1 1 calc R . .
H12B H 0.3187 1.0928 0.4353 0.088 Uiso 1 1 calc R . .
H12C H 0.1486 1.0559 0.4211 0.088 Uiso 1 1 calc R . .
C13 C 0.2924(4) 0.7807(4) 0.59225(17) 0.0663(8) Uani 1 1 d . . .
H13A H 0.1887 0.8103 0.6139 0.099 Uiso 1 1 calc R . .
H13B H 0.3648 0.8410 0.6138 0.099 Uiso 1 1 calc R . .
H13C H 0.3167 0.6699 0.6189 0.099 Uiso 1 1 calc R . .
S1 S 0.02959(11) 1.09871(8) 0.19192(6) 0.02609(18) Uani 0.794(3) 1 d PD A 1
S2 S -0.16826(7) 0.79142(8) 0.12457(7) 0.0268(2) Uani 0.794(3) 1 d PD A 1
C14 C -0.1110(2) 1.1498(2) 0.10120(15) 0.0356(4) Uani 1 1 d D . .
H14A H -0.1215 1.2643 0.0799 0.043 Uiso 0.794(3) 1 calc PR A 1
H14B H -0.0698 1.1093 0.0456 0.043 Uiso 0.794(3) 1 calc PR A 1
H14C H -0.1132 1.2644 0.0826 0.043 Uiso 0.206(3) 1 calc PR A 2
H14D H -0.0601 1.1061 0.0491 0.043 Uiso 0.206(3) 1 calc PR A 2
C15 C -0.2679(2) 1.0944(3) 0.1276(2) 0.0545(7) Uani 1 1 d D A .
H15A H -0.3214 1.1026 0.0683 0.065 Uiso 0.794(3) 1 calc PR A 1
H15B H -0.3257 1.1639 0.1641 0.065 Uiso 0.794(3) 1 calc PR A 1
H15C H -0.3480 1.1743 0.0998 0.065 Uiso 0.206(3) 1 calc PR A 2
H15D H -0.2868 1.0633 0.1977 0.065 Uiso 0.206(3) 1 calc PR A 2
C16 C -0.2688(3) 0.9277(3) 0.18685(19) 0.0348(6) Uani 0.794(3) 1 d PD A 1
H16A H -0.3755 0.9002 0.2020 0.042 Uiso 0.794(3) 1 calc PR A 1
H16B H -0.2205 0.9199 0.2479 0.042 Uiso 0.794(3) 1 calc PR A 1
C7 C 0.09504(19) 0.91095(18) 0.18109(12) 0.0217(3) Uani 1 1 d D . .
C8 C 0.01668(18) 0.79139(18) 0.15744(11) 0.0208(3) Uani 1 1 d D A .
C17 C 0.4106(2) 0.4082(2) 0.19638(14) 0.0315(4) Uani 1 1 d . . .
H17A H 0.4983 0.3429 0.2272 0.038 Uiso 1 1 calc R . .
H17B H 0.3220 0.3941 0.2428 0.038 Uiso 1 1 calc R . .
C18 C 0.3747(2) 0.3501(2) 0.10975(14) 0.0306(4) Uani 1 1 d . . .
H18A H 0.4693 0.3438 0.0693 0.037 Uiso 1 1 calc R . .
H18B H 0.3401 0.2441 0.1318 0.037 Uiso 1 1 calc R . .
C19 C 0.2532(2) 0.4525(2) 0.04932(13) 0.0291(4) Uani 1 1 d . . .
H19A H 0.2262 0.3996 0.0003 0.035 Uiso 1 1 calc R . .
H19B H 0.2970 0.5506 0.0156 0.035 Uiso 1 1 calc R . .
S1B S -0.0205(4) 1.0710(4) 0.2147(2) 0.0292(7) Uiso 0.206(3) 1 d PD A 2
S2B S -0.1954(3) 0.7583(3) 0.1684(3) 0.0229(6) Uiso 0.206(3) 1 d PD A 2
C16B C -0.2565(9) 0.9292(8) 0.0738(6) 0.0241(18) Uiso 0.206(3) 1 d PD A 2
H16C H -0.1815 0.9433 0.0187 0.029 Uiso 0.206(3) 1 calc PR A 2
H16D H -0.3570 0.9159 0.0515 0.029 Uiso 0.206(3) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01869(11) 0.01882(11) 0.01591(11) -0.00272(8) -0.00115(8) -0.00281(8)
S3 0.01551(19) 0.0324(2) 0.0441(3) -0.0168(2) -0.00214(17) 0.00056(16)
S4 0.0209(2) 0.0234(2) 0.0431(3) -0.01818(18) -0.00468(17) -0.00127(15)
Si1 0.0448(3) 0.0532(4) 0.0270(3) -0.0154(2) -0.0119(2) -0.0060(3)
C1 0.0366(10) 0.0383(10) 0.0166(8) -0.0051(7) -0.0038(7) -0.0033(8)
C2 0.0449(11) 0.0323(10) 0.0197(8) 0.0043(7) -0.0060(8) 0.0006(8)
C3 0.0565(13) 0.0304(10) 0.0250(9) 0.0040(8) 0.0024(9) -0.0174(9)
C4 0.0352(10) 0.0527(12) 0.0259(9) -0.0040(8) 0.0083(8) -0.0191(9)
C5 0.0347(10) 0.0467(11) 0.0208(8) -0.0101(8) 0.0051(7) -0.0038(8)
C6 0.0256(8) 0.0188(7) 0.0209(8) -0.0025(6) -0.0001(6) -0.0046(6)
O6 0.0297(7) 0.0264(6) 0.0505(8) -0.0113(6) 0.0014(6) -0.0129(5)
C9 0.0176(7) 0.0189(7) 0.0204(7) -0.0047(6) -0.0004(6) -0.0018(6)
C10 0.0194(7) 0.0168(7) 0.0184(7) -0.0039(6) -0.0035(6) -0.0002(6)
C11 0.0412(13) 0.0828(19) 0.0530(14) -0.0249(13) -0.0128(11) -0.0089(12)
C12 0.0790(18) 0.0496(14) 0.0575(15) -0.0235(12) -0.0214(14) -0.0123(13)
C13 0.0775(19) 0.098(2) 0.0313(12) -0.0227(13) -0.0155(12) -0.0163(16)
S1 0.0267(4) 0.0161(3) 0.0372(4) -0.0102(2) -0.0048(3) 0.0029(2)
S2 0.0163(3) 0.0311(3) 0.0380(5) -0.0170(3) -0.0091(3) 0.0032(2)
C14 0.0408(11) 0.0234(9) 0.0398(11) -0.0021(8) -0.0116(8) 0.0055(8)
C15 0.0302(11) 0.0348(11) 0.092(2) -0.0062(12) -0.0062(11) 0.0138(9)
C16 0.0191(10) 0.0401(13) 0.0496(15) -0.0219(12) 0.0023(10) 0.0017(9)
C7 0.0268(8) 0.0160(7) 0.0227(8) -0.0057(6) -0.0046(6) 0.0023(6)
C8 0.0199(7) 0.0216(8) 0.0221(8) -0.0077(6) -0.0063(6) 0.0035(6)
C17 0.0304(9) 0.0254(9) 0.0370(10) -0.0058(7) -0.0086(8) 0.0091(7)
C18 0.0277(9) 0.0219(8) 0.0425(11) -0.0107(8) -0.0015(8) 0.0047(7)
C19 0.0283(9) 0.0298(9) 0.0336(9) -0.0177(8) -0.0049(7) 0.0047(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Co1 C10 42.39(6) . . ?
C8 Co1 C5 120.37(7) . . ?
C10 Co1 C5 156.80(7) . . ?
C8 Co1 C2 162.51(7) . . ?
C10 Co1 C2 124.47(7) . . ?
C5 Co1 C2 67.58(8) . . ?
C8 Co1 C9 69.96(6) . . ?
C10 Co1 C9 41.23(6) . . ?
C5 Co1 C9 160.93(7) . . ?
C2 Co1 C9 107.55(7) . . ?
C8 Co1 C7 41.43(6) . . ?
C10 Co1 C7 69.84(6) . . ?
C5 Co1 C7 107.60(7) . . ?
C2 Co1 C7 155.10(8) . . ?
C9 Co1 C7 68.58(6) . . ?
C8 Co1 C3 125.06(8) . . ?
C10 Co1 C3 107.62(7) . . ?
C5 Co1 C3 67.49(9) . . ?
C2 Co1 C3 40.53(8) . . ?
C9 Co1 C3 121.68(8) . . ?
C7 Co1 C3 162.41(8) . . ?
C8 Co1 C4 107.49(8) . . ?
C10 Co1 C4 121.22(7) . . ?
C5 Co1 C4 40.50(8) . . ?
C2 Co1 C4 67.54(9) . . ?
C9 Co1 C4 156.63(8) . . ?
C7 Co1 C4 125.71(8) . . ?
C3 Co1 C4 39.71(9) . . ?
C8 Co1 C1 155.15(7) . . ?
C10 Co1 C1 160.90(7) . . ?
C5 Co1 C1 40.71(8) . . ?
C2 Co1 C1 40.61(8) . . ?
C9 Co1 C1 123.58(7) . . ?
C7 Co1 C1 119.60(7) . . ?
C3 Co1 C1 68.55(8) . . ?
C4 Co1 C1 68.60(8) . . ?
C8 Co1 C6 67.08(6) . . ?
C10 Co1 C6 66.94(6) . . ?
C5 Co1 C6 126.36(7) . . ?
C2 Co1 C6 122.60(7) . . ?
C9 Co1 C6 39.38(6) . . ?
C7 Co1 C6 39.22(6) . . ?
C3 Co1 C6 157.05(8) . . ?
C4 Co1 C6 162.46(8) . . ?
C1 Co1 C6 108.84(7) . . ?
C9 S3 C17 102.05(8) . . ?
C10 S4 C19 101.04(8) . . ?
C11 Si1 C12 111.59(14) . . ?
C11 Si1 C1 108.13(10) . . ?
C12 Si1 C1 109.66(10) . . ?
C11 Si1 C13 109.60(13) . . ?
C12 Si1 C13 109.72(14) . . ?
C1 Si1 C13 108.06(11) . . ?
C2 C1 C5 105.10(17) . . ?
C2 C1 Si1 126.94(15) . . ?
C5 C1 Si1 127.96(15) . . ?
C2 C1 Co1 68.51(10) . . ?
C5 C1 Co1 68.38(10) . . ?
Si1 C1 Co1 127.97(10) . . ?
C3 C2 C1 109.52(18) . . ?
C3 C2 Co1 70.35(10) . . ?
C1 C2 Co1 70.88(10) . . ?
C4 C3 C2 108.05(18) . . ?
C4 C3 Co1 70.38(11) . . ?
C2 C3 Co1 69.12(10) . . ?
C3 C4 C5 107.60(18) . . ?
C3 C4 Co1 69.91(11) . . ?
C5 C4 Co1 68.82(10) . . ?
C4 C5 C1 109.70(18) . . ?
C4 C5 Co1 70.68(11) . . ?
C1 C5 Co1 70.91(10) . . ?
O6 C6 C7 128.56(15) . . ?
O6 C6 C9 127.42(15) . . ?
C7 C6 C9 103.69(13) . . ?
O6 C6 Co1 134.25(13) . . ?
C7 C6 Co1 62.17(8) . . ?
C9 C6 Co1 62.11(8) . . ?
C10 C9 C6 109.57(13) . . ?
C10 C9 S3 131.17(12) . . ?
C6 C9 S3 118.36(11) . . ?
C10 C9 Co1 67.56(9) . . ?
C6 C9 Co1 78.51(9) . . ?
S3 C9 Co1 129.36(9) . . ?
C9 C10 C8 107.61(13) . . ?
C9 C10 S4 130.17(12) . . ?
C8 C10 S4 122.18(12) . . ?
C9 C10 Co1 71.21(9) . . ?
C8 C10 Co1 68.32(9) . . ?
S4 C10 Co1 127.54(9) . . ?
C7 S1 C14 100.87(9) . . ?
C8 S2 C16 101.75(10) . . ?
C15 C14 S1 117.90(17) . . ?
C15 C14 S1B 99.9(2) . . ?
S1 C14 S1B 17.98(10) . . ?
C14 C15 C16 113.97(17) . . ?
C14 C15 C16B 100.5(3) . . ?
C16 C15 C16B 57.5(3) . . ?
C15 C16 S2 111.88(19) . . ?
C8 C7 C6 109.60(13) . . ?
C8 C7 S1 130.76(13) . . ?
C6 C7 S1 118.50(12) . . ?
C8 C7 S1B 117.47(17) . . ?
C6 C7 S1B 132.86(17) . . ?
S1 C7 S1B 18.24(10) . . ?
C8 C7 Co1 66.94(9) . . ?
C6 C7 Co1 78.61(9) . . ?
S1 C7 Co1 130.91(10) . . ?
S1B C7 Co1 117.16(14) . . ?
C7 C8 C10 107.75(13) . . ?
C7 C8 S2 130.80(12) . . ?
C10 C8 S2 120.84(12) . . ?
C7 C8 S2B 130.10(14) . . ?
C10 C8 S2B 119.80(13) . . ?
S2 C8 S2B 20.44(8) . . ?
C7 C8 Co1 71.63(9) . . ?
C10 C8 Co1 69.30(9) . . ?
S2 C8 Co1 131.10(10) . . ?
S2B C8 Co1 110.71(13) . . ?
C18 C17 S3 115.01(13) . . ?
C19 C18 C17 113.67(14) . . ?
C18 C19 S4 114.64(13) . . ?
C7 S1B C14 98.12(16) . . ?
C16B S2B C8 97.0(3) . . ?
C15 C16B S2B 106.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C8 1.9957(15) . ?
Co1 C10 2.0090(15) . ?
Co1 C5 2.0491(18) . ?
Co1 C2 2.0513(17) . ?
Co1 C9 2.0578(15) . ?
Co1 C7 2.0584(16) . ?
Co1 C3 2.0676(18) . ?
Co1 C4 2.0738(18) . ?
Co1 C1 2.0829(17) . ?
Co1 C6 2.2817(16) . ?
S3 C9 1.7537(16) . ?
S3 C17 1.8147(19) . ?
S4 C10 1.7555(16) . ?
S4 C19 1.8175(18) . ?
Si1 C11 1.858(3) . ?
Si1 C12 1.862(3) . ?
Si1 C1 1.866(2) . ?
Si1 C13 1.880(2) . ?
C1 C2 1.435(3) . ?
C1 C5 1.438(3) . ?
C2 C3 1.427(3) . ?
C3 C4 1.407(3) . ?
C4 C5 1.427(3) . ?
C6 O6 1.236(2) . ?
C6 C7 1.472(2) . ?
C6 C9 1.477(2) . ?
C9 C10 1.433(2) . ?
C10 C8 1.448(2) . ?
S1 C7 1.7578(16) . ?
S1 C14 1.817(2) . ?
S2 C8 1.7299(16) . ?
S2 C16 1.812(2) . ?
C14 C15 1.503(3) . ?
C14 S1B 1.831(3) . ?
C15 C16 1.527(3) . ?
C15 C16B 1.811(8) . ?
C7 C8 1.435(2) . ?
C7 S1B 1.818(3) . ?
C8 S2B 1.909(3) . ?
C17 C18 1.523(3) . ?
C18 C19 1.523(2) . ?
S2B C16B 1.854(8) . ?
|
1100836.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100836.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100836
loop_
_publ_author_name
'Schaefer, Carsten'
'Werz, Daniel B.'
'Staeb, Tobias H.'
'Gleiter, Rolf'
'Rominger, Frank'
_publ_section_title
;
CpCo-Stabilized Cyclopentadienones from Cyclobutadiene Complexes:
Experimental and Theoretical Investigations
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2113
_journal_paper_doi 10.1021/om050048r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C14 H17 Co O S4'
_chemical_formula_weight 388.45
_chemical_name_common in_paper_14
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 79.0220(10)
_cell_angle_beta 83.8000(10)
_cell_angle_gamma 79.2260(10)
_cell_formula_units_Z 6
_cell_length_a 9.1494(3)
_cell_length_b 12.4455(5)
_cell_length_c 22.3392(8)
_cell_measurement_temperature 200(2)
_cell_volume 2446.25(15)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0874
_diffrn_reflns_av_sigmaI/netI 0.1461
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 23034
_diffrn_reflns_theta_full 25.97
_diffrn_reflns_theta_max 25.97
_diffrn_reflns_theta_min 0.93
_exptl_absorpt_coefficient_mu 1.556
_exptl_absorpt_correction_T_max 0.9696
_exptl_absorpt_correction_T_min 0.7359
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.582
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description polyhedron
_exptl_crystal_F_000 1200
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.492
_refine_diff_density_min -0.443
_refine_diff_density_rms 0.098
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.951
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 553
_refine_ls_number_reflns 9560
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.951
_refine_ls_R_factor_all 0.1305
_refine_ls_R_factor_gt 0.0492
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+0.0566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0668
_refine_ls_wR_factor_ref 0.0858
_reflns_number_gt 5088
_reflns_number_total 9560
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060510
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100836
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1_1 Co 0.63311(7) 0.21893(5) 0.01799(3) 0.02327(18) Uani 1 1 d . . .
S1_1 S 0.83125(15) 0.01510(11) 0.12126(6) 0.0326(3) Uani 1 1 d . . .
S2_1 S 0.86729(14) 0.28559(11) 0.10521(6) 0.0346(4) Uani 1 1 d . . .
S3_1 S 0.83290(15) 0.41050(10) -0.04950(7) 0.0405(4) Uani 1 1 d . . .
S4_1 S 0.78905(15) 0.21282(11) -0.12944(6) 0.0376(4) Uani 1 1 d . . .
C1_1 C 0.4336(5) 0.1632(4) 0.0214(2) 0.0296(13) Uani 1 1 d . . .
H1_1 H 0.4218 0.0921 0.0150 0.035 Uiso 1 1 calc R . .
C2_1 C 0.4513(5) 0.1917(5) 0.0774(2) 0.0365(14) Uani 1 1 d . . .
H2_1 H 0.4553 0.1430 0.1157 0.044 Uiso 1 1 calc R . .
C3_1 C 0.4622(5) 0.3063(5) 0.0670(3) 0.0443(16) Uani 1 1 d . . .
H3_1 H 0.4737 0.3477 0.0973 0.053 Uiso 1 1 calc R . .
C4_1 C 0.4531(5) 0.3472(4) 0.0048(3) 0.0401(15) Uani 1 1 d . . .
H4_1 H 0.4573 0.4214 -0.0149 0.048 Uiso 1 1 calc R . .
C5_1 C 0.4364(5) 0.2587(4) -0.0238(2) 0.0316(13) Uani 1 1 d . . .
H5_1 H 0.4285 0.2629 -0.0663 0.038 Uiso 1 1 calc R . .
C6_1 C 0.8240(5) 0.0770(4) -0.0094(2) 0.0221(12) Uani 1 1 d . . .
O6_1 O 0.8316(3) -0.0161(3) -0.02306(14) 0.0304(9) Uani 1 1 d . . .
C7_1 C 0.8160(5) 0.1067(4) 0.0517(2) 0.0217(12) Uani 1 1 d . . .
C8_1 C 0.8297(5) 0.2216(4) 0.0459(2) 0.0224(12) Uani 1 1 d . . .
C9_1 C 0.8213(5) 0.2713(4) -0.0174(2) 0.0242(12) Uani 1 1 d . . .
C10_1 C 0.7989(5) 0.1865(4) -0.0497(2) 0.0228(12) Uani 1 1 d . . .
C11_1 C 0.7381(6) -0.0933(4) 0.1092(2) 0.0564(18) Uani 1 1 d . . .
H11A_1 H 0.6398 -0.0605 0.0943 0.085 Uiso 1 1 calc R . .
H11B_1 H 0.7259 -0.1446 0.1478 0.085 Uiso 1 1 calc R . .
H11C_1 H 0.7978 -0.1339 0.0788 0.085 Uiso 1 1 calc R . .
C12_1 C 1.0666(5) 0.2412(5) 0.1034(2) 0.0573(18) Uani 1 1 d . . .
H12A_1 H 1.0912 0.1641 0.0967 0.086 Uiso 1 1 calc R . .
H12B_1 H 1.1022 0.2464 0.1424 0.086 Uiso 1 1 calc R . .
H12C_1 H 1.1148 0.2890 0.0701 0.086 Uiso 1 1 calc R . .
C13_1 C 1.0312(6) 0.3985(4) -0.0683(3) 0.065(2) Uani 1 1 d . . .
H13A_1 H 1.0835 0.3745 -0.0308 0.098 Uiso 1 1 calc R . .
H13B_1 H 1.0546 0.4707 -0.0891 0.098 Uiso 1 1 calc R . .
H13C_1 H 1.0632 0.3437 -0.0954 0.098 Uiso 1 1 calc R . .
C14_1 C 0.6981(6) 0.1028(4) -0.1409(2) 0.0547(17) Uani 1 1 d . . .
H14A_1 H 0.7676 0.0322 -0.1346 0.082 Uiso 1 1 calc R . .
H14B_1 H 0.6665 0.1182 -0.1827 0.082 Uiso 1 1 calc R . .
H14C_1 H 0.6106 0.0982 -0.1116 0.082 Uiso 1 1 calc R . .
Co1_2 Co 0.47283(7) 0.60655(5) 0.33671(3) 0.02015(17) Uani 1 1 d . . .
S1_2 S 0.62642(14) 0.37669(11) 0.43526(6) 0.0332(4) Uani 1 1 d . . .
S2_2 S 0.69585(15) 0.63938(11) 0.43626(6) 0.0377(4) Uani 1 1 d . . .
S3_2 S 0.70268(15) 0.78433(10) 0.28497(6) 0.0350(4) Uani 1 1 d . . .
S4_2 S 0.64182(15) 0.61200(11) 0.19113(6) 0.0353(4) Uani 1 1 d . . .
C1_2 C 0.2624(5) 0.5716(4) 0.3334(3) 0.0386(15) Uani 1 1 d . . .
H1_2 H 0.2387 0.5057 0.3242 0.046 Uiso 1 1 calc R . .
C2_2 C 0.2823(5) 0.5910(4) 0.3919(3) 0.0365(15) Uani 1 1 d . . .
H2_2 H 0.2763 0.5393 0.4289 0.044 Uiso 1 1 calc R . .
C3_2 C 0.3126(5) 0.6993(4) 0.3867(2) 0.0309(13) Uani 1 1 d . . .
H3_2 H 0.3290 0.7337 0.4193 0.037 Uiso 1 1 calc R . .
C4_2 C 0.3141(5) 0.7474(4) 0.3243(2) 0.0282(13) Uani 1 1 d . . .
H4_2 H 0.3319 0.8202 0.3075 0.034 Uiso 1 1 calc R . .
C5_2 C 0.2845(5) 0.6688(4) 0.2908(2) 0.0352(14) Uani 1 1 d . . .
H5_2 H 0.2802 0.6792 0.2477 0.042 Uiso 1 1 calc R . .
C6_2 C 0.6492(5) 0.4602(4) 0.3062(2) 0.0219(12) Uani 1 1 d . . .
O6_2 O 0.6492(3) 0.3726(2) 0.28750(14) 0.0284(8) Uani 1 1 d . . .
C7_2 C 0.6366(5) 0.4786(4) 0.3697(2) 0.0237(12) Uani 1 1 d . . .
C8_2 C 0.6667(5) 0.5883(4) 0.3708(2) 0.0249(12) Uani 1 1 d . . .
C9_2 C 0.6708(5) 0.6465(3) 0.3088(2) 0.0205(12) Uani 1 1 d . . .
C10_2 C 0.6429(5) 0.5740(4) 0.2698(2) 0.0195(11) Uani 1 1 d . . .
C11_2 C 0.4919(5) 0.3012(4) 0.4166(2) 0.0388(14) Uani 1 1 d . . .
H11A_2 H 0.3967 0.3514 0.4100 0.058 Uiso 1 1 calc R . .
H11B_2 H 0.4775 0.2402 0.4504 0.058 Uiso 1 1 calc R . .
H11C_2 H 0.5286 0.2709 0.3793 0.058 Uiso 1 1 calc R . .
C12_2 C 0.8910(6) 0.5948(5) 0.4408(3) 0.083(2) Uani 1 1 d . . .
H12A_2 H 0.9166 0.5160 0.4374 0.125 Uiso 1 1 calc R . .
H12B_2 H 0.9195 0.6052 0.4801 0.125 Uiso 1 1 calc R . .
H12C_2 H 0.9447 0.6386 0.4074 0.125 Uiso 1 1 calc R . .
C13_2 C 0.8984(5) 0.7586(4) 0.2597(2) 0.0529(17) Uani 1 1 d . . .
H13A_2 H 0.9563 0.7222 0.2946 0.079 Uiso 1 1 calc R . .
H13B_2 H 0.9311 0.8293 0.2419 0.079 Uiso 1 1 calc R . .
H13C_2 H 0.9139 0.7104 0.2288 0.079 Uiso 1 1 calc R . .
C14_2 C 0.5332(6) 0.5175(4) 0.1711(2) 0.0467(16) Uani 1 1 d . . .
H14A_2 H 0.5967 0.4451 0.1697 0.070 Uiso 1 1 calc R . .
H14B_2 H 0.4949 0.5479 0.1309 0.070 Uiso 1 1 calc R . .
H14C_2 H 0.4494 0.5085 0.2018 0.070 Uiso 1 1 calc R . .
Co1_3 Co 0.09322(7) 1.12361(5) 0.33486(3) 0.02138(18) Uani 1 1 d . . .
S1_3 S 0.19981(14) 1.35277(11) 0.23651(6) 0.0331(4) Uani 1 1 d . . .
S2_3 S 0.40674(14) 1.08961(11) 0.24767(6) 0.0338(4) Uani 1 1 d . . .
S3_3 S 0.37937(14) 0.95866(10) 0.40186(7) 0.0354(4) Uani 1 1 d . . .
S4_3 S 0.15105(15) 1.13759(11) 0.48382(6) 0.0355(4) Uani 1 1 d . . .
C1_3 C -0.1347(5) 1.1482(4) 0.3367(3) 0.0330(14) Uani 1 1 d . . .
H1_3 H -0.2009 1.2092 0.3497 0.040 Uiso 1 1 calc R . .
C2_3 C -0.0728(6) 1.1424(5) 0.2769(3) 0.0454(16) Uani 1 1 d . . .
H2_3 H -0.0887 1.1996 0.2423 0.054 Uiso 1 1 calc R . .
C3_3 C 0.0172(6) 1.0375(5) 0.2770(3) 0.0498(17) Uani 1 1 d . . .
H3_3 H 0.0717 1.0114 0.2424 0.060 Uiso 1 1 calc R . .
C4_3 C 0.0125(6) 0.9779(4) 0.3371(3) 0.0418(16) Uani 1 1 d . . .
H4_3 H 0.0629 0.9046 0.3505 0.050 Uiso 1 1 calc R . .
C5_3 C -0.0806(5) 1.0467(4) 0.3737(2) 0.0329(14) Uani 1 1 d . . .
H5_3 H -0.1033 1.0278 0.4165 0.039 Uiso 1 1 calc R . .
C6_3 C 0.1563(5) 1.2777(4) 0.3656(2) 0.0232(12) Uani 1 1 d . . .
O6_3 O 0.0915(3) 1.3654(3) 0.38150(14) 0.0323(9) Uani 1 1 d . . .
C7_3 C 0.2086(5) 1.2553(4) 0.3035(2) 0.0201(11) Uani 1 1 d . . .
C8_3 C 0.3008(5) 1.1465(4) 0.3077(2) 0.0199(11) Uani 1 1 d . . .
C9_3 C 0.2888(5) 1.0923(4) 0.3710(2) 0.0226(12) Uani 1 1 d . . .
C10_3 C 0.1897(5) 1.1666(4) 0.4046(2) 0.0191(11) Uani 1 1 d . . .
C11_3 C 0.0176(5) 1.4343(4) 0.2448(2) 0.0482(16) Uani 1 1 d . . .
H11A_3 H -0.0578 1.3861 0.2500 0.072 Uiso 1 1 calc R . .
H11B_3 H 0.0007 1.4913 0.2083 0.072 Uiso 1 1 calc R . .
H11C_3 H 0.0103 1.4700 0.2808 0.072 Uiso 1 1 calc R . .
C12_3 C 0.5644(5) 1.1596(5) 0.2386(3) 0.070(2) Uani 1 1 d . . .
H12A_3 H 0.5304 1.2400 0.2292 0.105 Uiso 1 1 calc R . .
H12B_3 H 0.6336 1.1358 0.2052 0.105 Uiso 1 1 calc R . .
H12C_3 H 0.6151 1.1413 0.2767 0.105 Uiso 1 1 calc R . .
C13_3 C 0.5648(6) 0.9829(4) 0.4057(3) 0.067(2) Uani 1 1 d . . .
H13A_3 H 0.6000 1.0219 0.3660 0.101 Uiso 1 1 calc R . .
H13B_3 H 0.6313 0.9117 0.4163 0.101 Uiso 1 1 calc R . .
H13C_3 H 0.5646 1.0283 0.4371 0.101 Uiso 1 1 calc R . .
C14_3 C -0.0428(5) 1.2049(4) 0.4937(2) 0.0452(15) Uani 1 1 d . . .
H14A_3 H -0.0573 1.2777 0.4670 0.068 Uiso 1 1 calc R . .
H14B_3 H -0.0668 1.2144 0.5364 0.068 Uiso 1 1 calc R . .
H14C_3 H -0.1083 1.1587 0.4830 0.068 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1_1 0.0187(4) 0.0267(4) 0.0249(4) -0.0049(3) -0.0015(3) -0.0048(3)
S1_1 0.0353(8) 0.0353(8) 0.0262(8) 0.0019(6) -0.0055(7) -0.0089(7)
S2_1 0.0304(8) 0.0405(9) 0.0381(9) -0.0175(7) -0.0024(7) -0.0083(7)
S3_1 0.0396(9) 0.0250(8) 0.0543(11) 0.0010(7) 0.0006(8) -0.0093(7)
S4_1 0.0433(9) 0.0448(9) 0.0225(8) 0.0007(7) -0.0007(7) -0.0092(7)
C1_1 0.022(3) 0.040(3) 0.029(3) -0.006(3) -0.002(3) -0.013(3)
C2_1 0.016(3) 0.067(4) 0.024(3) -0.001(3) 0.004(2) -0.010(3)
C3_1 0.026(3) 0.065(4) 0.048(4) -0.033(4) -0.002(3) 0.001(3)
C4_1 0.030(3) 0.031(3) 0.058(4) -0.008(3) -0.009(3) 0.000(3)
C5_1 0.022(3) 0.041(3) 0.032(3) -0.011(3) -0.006(3) 0.001(3)
C6_1 0.013(3) 0.023(3) 0.028(3) -0.002(3) 0.000(2) -0.001(2)
O6_1 0.035(2) 0.028(2) 0.030(2) -0.0089(17) -0.0013(17) -0.0062(17)
C7_1 0.019(3) 0.025(3) 0.019(3) -0.001(2) -0.001(2) -0.001(2)
C8_1 0.016(3) 0.026(3) 0.027(3) -0.012(3) -0.002(2) -0.003(2)
C9_1 0.021(3) 0.020(3) 0.030(3) 0.000(3) 0.000(3) -0.006(2)
C10_1 0.017(3) 0.033(3) 0.018(3) -0.006(2) 0.000(2) -0.002(2)
C11_1 0.087(5) 0.049(4) 0.036(4) 0.016(3) -0.010(4) -0.039(4)
C12_1 0.028(3) 0.097(5) 0.056(4) -0.031(4) -0.015(3) -0.009(3)
C13_1 0.047(4) 0.050(4) 0.092(5) 0.007(4) 0.014(4) -0.025(3)
C14_1 0.087(5) 0.052(4) 0.032(4) -0.014(3) -0.024(3) -0.012(4)
Co1_2 0.0154(4) 0.0195(4) 0.0257(4) -0.0051(3) -0.0011(3) -0.0025(3)
S1_2 0.0331(8) 0.0356(8) 0.0285(8) 0.0047(7) -0.0075(7) -0.0074(7)
S2_2 0.0312(9) 0.0531(10) 0.0365(9) -0.0235(8) -0.0043(7) -0.0094(7)
S3_2 0.0329(8) 0.0267(8) 0.0465(10) -0.0064(7) 0.0041(7) -0.0117(7)
S4_2 0.0455(9) 0.0387(9) 0.0227(8) -0.0021(7) 0.0012(7) -0.0154(7)
C1_2 0.018(3) 0.043(4) 0.062(5) -0.024(3) -0.008(3) -0.005(3)
C2_2 0.018(3) 0.028(3) 0.053(4) 0.006(3) 0.009(3) 0.003(2)
C3_2 0.031(3) 0.024(3) 0.038(4) -0.012(3) 0.001(3) -0.002(3)
C4_2 0.019(3) 0.022(3) 0.038(4) -0.002(3) 0.004(3) 0.004(2)
C5_2 0.020(3) 0.042(4) 0.042(4) -0.006(3) -0.011(3) 0.002(3)
C6_2 0.011(3) 0.030(3) 0.026(3) -0.009(3) -0.003(2) 0.000(2)
O6_2 0.035(2) 0.0220(19) 0.028(2) -0.0072(16) -0.0029(17) -0.0014(16)
C7_2 0.016(3) 0.029(3) 0.026(3) -0.005(2) 0.000(2) -0.006(2)
C8_2 0.011(3) 0.034(3) 0.030(3) -0.009(3) 0.002(2) -0.004(2)
C9_2 0.015(3) 0.019(3) 0.027(3) -0.002(2) 0.005(2) -0.005(2)
C10_2 0.019(3) 0.019(3) 0.021(3) -0.003(2) 0.002(2) -0.007(2)
C11_2 0.043(4) 0.034(3) 0.041(4) -0.005(3) 0.005(3) -0.016(3)
C12_2 0.045(4) 0.114(6) 0.106(6) -0.070(5) -0.047(4) 0.021(4)
C13_2 0.036(4) 0.051(4) 0.071(5) 0.003(3) 0.004(3) -0.025(3)
C14_2 0.066(4) 0.047(4) 0.036(4) -0.010(3) -0.019(3) -0.020(3)
Co1_3 0.0148(4) 0.0241(4) 0.0261(4) -0.0028(3) -0.0031(3) -0.0062(3)
S1_3 0.0350(9) 0.0350(8) 0.0281(8) 0.0039(7) -0.0042(7) -0.0117(7)
S2_3 0.0288(8) 0.0429(9) 0.0341(9) -0.0194(7) 0.0069(7) -0.0098(7)
S3_3 0.0265(8) 0.0250(8) 0.0522(10) 0.0007(7) -0.0087(7) -0.0024(6)
S4_3 0.0303(8) 0.0483(9) 0.0234(8) 0.0002(7) -0.0015(7) -0.0018(7)
C1_3 0.012(3) 0.024(3) 0.066(4) -0.009(3) -0.006(3) -0.005(2)
C2_3 0.040(4) 0.061(4) 0.040(4) 0.016(3) -0.025(3) -0.033(3)
C3_3 0.040(4) 0.078(5) 0.048(4) -0.036(4) 0.007(3) -0.033(4)
C4_3 0.027(3) 0.024(3) 0.078(5) -0.017(3) -0.010(3) -0.003(3)
C5_3 0.028(3) 0.042(4) 0.031(3) 0.006(3) -0.005(3) -0.022(3)
C6_3 0.014(3) 0.024(3) 0.035(3) -0.003(3) -0.009(2) -0.008(2)
O6_3 0.035(2) 0.023(2) 0.039(2) -0.0098(18) 0.0048(18) -0.0042(17)
C7_3 0.014(3) 0.025(3) 0.024(3) -0.003(2) -0.002(2) -0.010(2)
C8_3 0.015(3) 0.022(3) 0.026(3) -0.008(2) -0.001(2) -0.006(2)
C9_3 0.012(3) 0.022(3) 0.034(3) -0.006(2) -0.003(2) -0.003(2)
C10_3 0.011(3) 0.032(3) 0.016(3) -0.004(2) 0.000(2) -0.009(2)
C11_3 0.047(4) 0.041(4) 0.051(4) 0.004(3) -0.022(3) 0.005(3)
C12_3 0.028(4) 0.132(6) 0.072(5) -0.056(5) 0.022(3) -0.044(4)
C13_3 0.038(4) 0.043(4) 0.124(6) -0.013(4) -0.047(4) 0.005(3)
C14_3 0.038(4) 0.059(4) 0.038(4) -0.019(3) 0.013(3) -0.005(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8_1 Co1_1 C9_1 42.48(17) . . ?
C8_1 Co1_1 C2_1 122.7(2) . . ?
C9_1 Co1_1 C2_1 160.6(2) . . ?
C8_1 Co1_1 C5_1 164.17(19) . . ?
C9_1 Co1_1 C5_1 124.51(19) . . ?
C2_1 Co1_1 C5_1 67.03(19) . . ?
C8_1 Co1_1 C1_1 155.28(19) . . ?
C9_1 Co1_1 C1_1 158.96(19) . . ?
C2_1 Co1_1 C1_1 39.70(17) . . ?
C5_1 Co1_1 C1_1 40.06(17) . . ?
C8_1 Co1_1 C10_1 69.95(18) . . ?
C9_1 Co1_1 C10_1 41.68(16) . . ?
C2_1 Co1_1 C10_1 156.4(2) . . ?
C5_1 Co1_1 C10_1 106.03(19) . . ?
C1_1 Co1_1 C10_1 120.52(19) . . ?
C8_1 Co1_1 C3_1 111.49(19) . . ?
C9_1 Co1_1 C3_1 125.4(2) . . ?
C2_1 Co1_1 C3_1 40.38(19) . . ?
C5_1 Co1_1 C3_1 66.8(2) . . ?
C1_1 Co1_1 C3_1 67.1(2) . . ?
C10_1 Co1_1 C3_1 159.8(2) . . ?
C8_1 Co1_1 C4_1 128.51(19) . . ?
C9_1 Co1_1 C4_1 110.49(19) . . ?
C2_1 Co1_1 C4_1 67.1(2) . . ?
C5_1 Co1_1 C4_1 40.11(17) . . ?
C1_1 Co1_1 C4_1 67.23(19) . . ?
C10_1 Co1_1 C4_1 123.1(2) . . ?
C3_1 Co1_1 C4_1 39.31(19) . . ?
C8_1 Co1_1 C7_1 41.50(16) . . ?
C9_1 Co1_1 C7_1 69.68(17) . . ?
C2_1 Co1_1 C7_1 107.51(19) . . ?
C5_1 Co1_1 C7_1 152.38(19) . . ?
C1_1 Co1_1 C7_1 118.22(19) . . ?
C10_1 Co1_1 C7_1 67.56(17) . . ?
C3_1 Co1_1 C7_1 127.7(2) . . ?
C4_1 Co1_1 C7_1 165.1(2) . . ?
C8_1 Co1_1 C6_1 65.91(17) . . ?
C9_1 Co1_1 C6_1 65.95(16) . . ?
C2_1 Co1_1 C6_1 124.27(19) . . ?
C5_1 Co1_1 C6_1 120.91(18) . . ?
C1_1 Co1_1 C6_1 107.25(18) . . ?
C10_1 Co1_1 C6_1 38.26(15) . . ?
C3_1 Co1_1 C6_1 161.8(2) . . ?
C4_1 Co1_1 C6_1 156.5(2) . . ?
C7_1 Co1_1 C6_1 38.06(15) . . ?
C7_1 S1_1 C11_1 102.1(2) . . ?
C8_1 S2_1 C12_1 98.8(2) . . ?
C9_1 S3_1 C13_1 100.1(2) . . ?
C10_1 S4_1 C14_1 102.1(2) . . ?
C2_1 C1_1 C5_1 107.8(5) . . ?
C2_1 C1_1 Co1_1 69.8(3) . . ?
C5_1 C1_1 Co1_1 69.7(3) . . ?
C1_1 C2_1 C3_1 108.1(5) . . ?
C1_1 C2_1 Co1_1 70.5(3) . . ?
C3_1 C2_1 Co1_1 70.4(3) . . ?
C4_1 C3_1 C2_1 108.1(5) . . ?
C4_1 C3_1 Co1_1 70.5(3) . . ?
C2_1 C3_1 Co1_1 69.2(3) . . ?
C3_1 C4_1 C5_1 107.8(5) . . ?
C3_1 C4_1 Co1_1 70.2(3) . . ?
C5_1 C4_1 Co1_1 69.2(3) . . ?
C1_1 C5_1 C4_1 108.3(5) . . ?
C1_1 C5_1 Co1_1 70.3(3) . . ?
C4_1 C5_1 Co1_1 70.7(3) . . ?
O6_1 C6_1 C7_1 128.6(4) . . ?
O6_1 C6_1 C10_1 128.2(4) . . ?
C7_1 C6_1 C10_1 102.7(4) . . ?
O6_1 C6_1 Co1_1 136.7(3) . . ?
C7_1 C6_1 Co1_1 60.5(2) . . ?
C10_1 C6_1 Co1_1 59.9(2) . . ?
C8_1 C7_1 C6_1 109.7(4) . . ?
C8_1 C7_1 S1_1 122.1(4) . . ?
C6_1 C7_1 S1_1 126.7(3) . . ?
C8_1 C7_1 Co1_1 65.4(2) . . ?
C6_1 C7_1 Co1_1 81.5(3) . . ?
S1_1 C7_1 Co1_1 129.7(2) . . ?
C9_1 C8_1 C7_1 107.9(4) . . ?
C9_1 C8_1 S2_1 126.4(3) . . ?
C7_1 C8_1 S2_1 125.5(4) . . ?
C9_1 C8_1 Co1_1 69.2(3) . . ?
C7_1 C8_1 Co1_1 73.1(2) . . ?
S2_1 C8_1 Co1_1 127.6(2) . . ?
C8_1 C9_1 C10_1 107.2(4) . . ?
C8_1 C9_1 S3_1 126.5(4) . . ?
C10_1 C9_1 S3_1 126.3(4) . . ?
C8_1 C9_1 Co1_1 68.3(2) . . ?
C10_1 C9_1 Co1_1 72.1(2) . . ?
S3_1 C9_1 Co1_1 124.0(2) . . ?
C9_1 C10_1 C6_1 109.7(4) . . ?
C9_1 C10_1 S4_1 121.5(3) . . ?
C6_1 C10_1 S4_1 127.2(3) . . ?
C9_1 C10_1 Co1_1 66.2(2) . . ?
C6_1 C10_1 Co1_1 81.8(3) . . ?
S4_1 C10_1 Co1_1 129.2(2) . . ?
C8_2 Co1_2 C9_2 42.77(17) . . ?
C8_2 Co1_2 C2_2 121.4(2) . . ?
C9_2 Co1_2 C2_2 158.7(2) . . ?
C8_2 Co1_2 C5_2 163.8(2) . . ?
C9_2 Co1_2 C5_2 124.1(2) . . ?
C2_2 Co1_2 C5_2 67.8(2) . . ?
C8_2 Co1_2 C4_2 127.45(19) . . ?
C9_2 Co1_2 C4_2 109.03(18) . . ?
C2_2 Co1_2 C4_2 67.32(18) . . ?
C5_2 Co1_2 C4_2 40.48(17) . . ?
C8_2 Co1_2 C7_2 42.17(17) . . ?
C9_2 Co1_2 C7_2 70.32(17) . . ?
C2_2 Co1_2 C7_2 107.65(19) . . ?
C5_2 Co1_2 C7_2 152.1(2) . . ?
C4_2 Co1_2 C7_2 165.35(19) . . ?
C8_2 Co1_2 C3_2 109.61(19) . . ?
C9_2 Co1_2 C3_2 123.45(18) . . ?
C2_2 Co1_2 C3_2 40.14(17) . . ?
C5_2 Co1_2 C3_2 67.94(19) . . ?
C4_2 Co1_2 C3_2 40.05(17) . . ?
C7_2 Co1_2 C3_2 127.37(19) . . ?
C8_2 Co1_2 C1_2 154.9(2) . . ?
C9_2 Co1_2 C1_2 160.0(2) . . ?
C2_2 Co1_2 C1_2 40.15(19) . . ?
C5_2 Co1_2 C1_2 40.47(18) . . ?
C4_2 Co1_2 C1_2 67.65(19) . . ?
C7_2 Co1_2 C1_2 118.12(19) . . ?
C3_2 Co1_2 C1_2 67.65(19) . . ?
C8_2 Co1_2 C10_2 70.49(18) . . ?
C9_2 Co1_2 C10_2 41.56(16) . . ?
C2_2 Co1_2 C10_2 158.83(19) . . ?
C5_2 Co1_2 C10_2 105.54(19) . . ?
C4_2 Co1_2 C10_2 121.52(18) . . ?
C7_2 Co1_2 C10_2 68.29(17) . . ?
C3_2 Co1_2 C10_2 158.01(18) . . ?
C1_2 Co1_2 C10_2 121.88(19) . . ?
C8_2 Co1_2 C6_2 66.34(17) . . ?
C9_2 Co1_2 C6_2 66.01(16) . . ?
C2_2 Co1_2 C6_2 126.09(18) . . ?
C5_2 Co1_2 C6_2 120.81(18) . . ?
C4_2 Co1_2 C6_2 155.79(18) . . ?
C7_2 Co1_2 C6_2 38.20(16) . . ?
C3_2 Co1_2 C6_2 162.71(18) . . ?
C1_2 Co1_2 C6_2 108.38(18) . . ?
C10_2 Co1_2 C6_2 38.63(15) . . ?
C7_2 S1_2 C11_2 101.9(2) . . ?
C8_2 S2_2 C12_2 101.0(2) . . ?
C9_2 S3_2 C13_2 100.1(2) . . ?
C10_2 S4_2 C14_2 102.8(2) . . ?
C2_2 C1_2 C5_2 107.4(5) . . ?
C2_2 C1_2 Co1_2 69.1(3) . . ?
C5_2 C1_2 Co1_2 69.3(3) . . ?
C3_2 C2_2 C1_2 109.1(5) . . ?
C3_2 C2_2 Co1_2 70.6(3) . . ?
C1_2 C2_2 Co1_2 70.8(3) . . ?
C2_2 C3_2 C4_2 107.5(5) . . ?
C2_2 C3_2 Co1_2 69.3(3) . . ?
C4_2 C3_2 Co1_2 69.7(3) . . ?
C3_2 C4_2 C5_2 108.6(4) . . ?
C3_2 C4_2 Co1_2 70.2(3) . . ?
C5_2 C4_2 Co1_2 69.7(3) . . ?
C4_2 C5_2 C1_2 107.4(5) . . ?
C4_2 C5_2 Co1_2 69.8(3) . . ?
C1_2 C5_2 Co1_2 70.2(3) . . ?
O6_2 C6_2 C7_2 128.2(4) . . ?
O6_2 C6_2 C10_2 128.0(4) . . ?
C7_2 C6_2 C10_2 103.4(4) . . ?
O6_2 C6_2 Co1_2 137.7(3) . . ?
C7_2 C6_2 Co1_2 59.9(2) . . ?
C10_2 C6_2 Co1_2 60.7(2) . . ?
C8_2 C7_2 C6_2 109.5(4) . . ?
C8_2 C7_2 S1_2 123.3(4) . . ?
C6_2 C7_2 S1_2 126.0(4) . . ?
C8_2 C7_2 Co1_2 65.5(2) . . ?
C6_2 C7_2 Co1_2 81.9(3) . . ?
S1_2 C7_2 Co1_2 128.4(2) . . ?
C9_2 C8_2 C7_2 107.2(4) . . ?
C9_2 C8_2 S2_2 126.7(4) . . ?
C7_2 C8_2 S2_2 126.1(4) . . ?
C9_2 C8_2 Co1_2 69.0(3) . . ?
C7_2 C8_2 Co1_2 72.3(3) . . ?
S2_2 C8_2 Co1_2 124.7(2) . . ?
C8_2 C9_2 C10_2 108.5(4) . . ?
C8_2 C9_2 S3_2 125.5(4) . . ?
C10_2 C9_2 S3_2 126.0(4) . . ?
C8_2 C9_2 Co1_2 68.2(2) . . ?
C10_2 C9_2 Co1_2 73.1(2) . . ?
S3_2 C9_2 Co1_2 123.9(2) . . ?
C9_2 C10_2 C6_2 108.6(4) . . ?
C9_2 C10_2 S4_2 123.0(3) . . ?
C6_2 C10_2 S4_2 127.2(3) . . ?
C9_2 C10_2 Co1_2 65.4(2) . . ?
C6_2 C10_2 Co1_2 80.7(3) . . ?
S4_2 C10_2 Co1_2 129.1(2) . . ?
C9_3 Co1_3 C8_3 42.78(17) . . ?
C9_3 Co1_3 C5_3 122.29(19) . . ?
C8_3 Co1_3 C5_3 160.0(2) . . ?
C9_3 Co1_3 C1_3 155.4(2) . . ?
C8_3 Co1_3 C1_3 158.7(2) . . ?
C5_3 Co1_3 C1_3 40.30(17) . . ?
C9_3 Co1_3 C2_3 164.0(2) . . ?
C8_3 Co1_3 C2_3 124.2(2) . . ?
C5_3 Co1_3 C2_3 67.1(2) . . ?
C1_3 Co1_3 C2_3 40.01(19) . . ?
C9_3 Co1_3 C10_3 41.23(16) . . ?
C8_3 Co1_3 C10_3 70.03(17) . . ?
C5_3 Co1_3 C10_3 107.40(18) . . ?
C1_3 Co1_3 C10_3 118.5(2) . . ?
C2_3 Co1_3 C10_3 153.1(2) . . ?
C9_3 Co1_3 C4_3 110.89(19) . . ?
C8_3 Co1_3 C4_3 125.01(19) . . ?
C5_3 Co1_3 C4_3 39.93(18) . . ?
C1_3 Co1_3 C4_3 67.45(19) . . ?
C2_3 Co1_3 C4_3 67.0(2) . . ?
C10_3 Co1_3 C4_3 126.8(2) . . ?
C9_3 Co1_3 C3_3 128.4(2) . . ?
C8_3 Co1_3 C3_3 110.2(2) . . ?
C5_3 Co1_3 C3_3 66.7(2) . . ?
C1_3 Co1_3 C3_3 67.1(2) . . ?
C2_3 Co1_3 C3_3 39.9(2) . . ?
C10_3 Co1_3 C3_3 164.5(2) . . ?
C4_3 Co1_3 C3_3 39.6(2) . . ?
C9_3 Co1_3 C7_3 69.94(17) . . ?
C8_3 Co1_3 C7_3 41.59(16) . . ?
C5_3 Co1_3 C7_3 157.2(2) . . ?
C1_3 Co1_3 C7_3 120.63(18) . . ?
C2_3 Co1_3 C7_3 106.28(19) . . ?
C10_3 Co1_3 C7_3 67.97(17) . . ?
C4_3 Co1_3 C7_3 159.8(2) . . ?
C3_3 Co1_3 C7_3 123.2(2) . . ?
C9_3 Co1_3 C6_3 66.30(16) . . ?
C8_3 Co1_3 C6_3 66.47(16) . . ?
C5_3 Co1_3 C6_3 124.54(19) . . ?
C1_3 Co1_3 C6_3 107.01(18) . . ?
C2_3 Co1_3 C6_3 120.9(2) . . ?
C10_3 Co1_3 C6_3 38.76(15) . . ?
C4_3 Co1_3 C6_3 161.5(2) . . ?
C3_3 Co1_3 C6_3 156.5(2) . . ?
C7_3 Co1_3 C6_3 38.45(16) . . ?
C7_3 S1_3 C11_3 103.3(2) . . ?
C8_3 S2_3 C12_3 100.9(2) . . ?
C9_3 S3_3 C13_3 101.5(2) . . ?
C10_3 S4_3 C14_3 102.7(2) . . ?
C2_3 C1_3 C5_3 107.2(5) . . ?
C2_3 C1_3 Co1_3 70.2(3) . . ?
C5_3 C1_3 Co1_3 69.5(3) . . ?
C1_3 C2_3 C3_3 108.3(5) . . ?
C1_3 C2_3 Co1_3 69.8(3) . . ?
C3_3 C2_3 Co1_3 70.9(3) . . ?
C4_3 C3_3 C2_3 108.2(5) . . ?
C4_3 C3_3 Co1_3 70.2(3) . . ?
C2_3 C3_3 Co1_3 69.2(3) . . ?
C5_3 C4_3 C3_3 107.3(5) . . ?
C5_3 C4_3 Co1_3 68.7(3) . . ?
C3_3 C4_3 Co1_3 70.3(3) . . ?
C4_3 C5_3 C1_3 108.9(5) . . ?
C4_3 C5_3 Co1_3 71.4(3) . . ?
C1_3 C5_3 Co1_3 70.2(3) . . ?
O6_3 C6_3 C7_3 129.2(4) . . ?
O6_3 C6_3 C10_3 127.5(4) . . ?
C7_3 C6_3 C10_3 103.1(4) . . ?
O6_3 C6_3 Co1_3 137.9(3) . . ?
C7_3 C6_3 Co1_3 61.3(2) . . ?
C10_3 C6_3 Co1_3 60.7(2) . . ?
C8_3 C7_3 C6_3 109.6(4) . . ?
C8_3 C7_3 S1_3 123.0(3) . . ?
C6_3 C7_3 S1_3 125.9(3) . . ?
C8_3 C7_3 Co1_3 65.6(2) . . ?
C6_3 C7_3 Co1_3 80.3(3) . . ?
S1_3 C7_3 Co1_3 131.0(2) . . ?
C7_3 C8_3 C9_3 107.3(4) . . ?
C7_3 C8_3 S2_3 126.7(4) . . ?
C9_3 C8_3 S2_3 125.9(3) . . ?
C7_3 C8_3 Co1_3 72.8(2) . . ?
C9_3 C8_3 Co1_3 68.6(2) . . ?
S2_3 C8_3 Co1_3 123.6(2) . . ?
C10_3 C9_3 C8_3 108.0(4) . . ?
C10_3 C9_3 S3_3 125.5(4) . . ?
C8_3 C9_3 S3_3 126.5(3) . . ?
C10_3 C9_3 Co1_3 72.6(2) . . ?
C8_3 C9_3 Co1_3 68.7(2) . . ?
S3_3 C9_3 Co1_3 124.3(2) . . ?
C9_3 C10_3 C6_3 109.7(4) . . ?
C9_3 C10_3 S4_3 123.4(4) . . ?
C6_3 C10_3 S4_3 125.4(3) . . ?
C9_3 C10_3 Co1_3 66.1(2) . . ?
C6_3 C10_3 Co1_3 80.5(3) . . ?
S4_3 C10_3 Co1_3 130.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1_1 C8_1 1.973(4) . ?
Co1_1 C9_1 1.986(4) . ?
Co1_1 C2_1 2.050(5) . ?
Co1_1 C5_1 2.052(5) . ?
Co1_1 C1_1 2.059(4) . ?
Co1_1 C10_1 2.064(4) . ?
Co1_1 C3_1 2.067(5) . ?
Co1_1 C4_1 2.072(5) . ?
Co1_1 C7_1 2.077(4) . ?
Co1_1 C6_1 2.361(5) . ?
S1_1 C7_1 1.746(5) . ?
S1_1 C11_1 1.799(5) . ?
S2_1 C8_1 1.764(4) . ?
S2_1 C12_1 1.802(5) . ?
S3_1 C9_1 1.762(4) . ?
S3_1 C13_1 1.802(5) . ?
S4_1 C10_1 1.757(5) . ?
S4_1 C14_1 1.799(5) . ?
C1_1 C2_1 1.396(6) . ?
C1_1 C5_1 1.408(6) . ?
C2_1 C3_1 1.421(7) . ?
C3_1 C4_1 1.392(7) . ?
C4_1 C5_1 1.414(6) . ?
C6_1 O6_1 1.241(5) . ?
C6_1 C7_1 1.472(6) . ?
C6_1 C10_1 1.477(6) . ?
C7_1 C8_1 1.439(6) . ?
C8_1 C9_1 1.434(6) . ?
C9_1 C10_1 1.443(6) . ?
Co1_2 C8_2 1.962(4) . ?
Co1_2 C9_2 1.973(4) . ?
Co1_2 C2_2 2.041(5) . ?
Co1_2 C5_2 2.051(5) . ?
Co1_2 C4_2 2.051(4) . ?
Co1_2 C7_2 2.055(5) . ?
Co1_2 C3_2 2.058(5) . ?
Co1_2 C1_2 2.063(5) . ?
Co1_2 C10_2 2.076(4) . ?
Co1_2 C6_2 2.350(5) . ?
S1_2 C7_2 1.753(5) . ?
S1_2 C11_2 1.806(4) . ?
S2_2 C8_2 1.765(5) . ?
S2_2 C12_2 1.776(5) . ?
S3_2 C9_2 1.765(4) . ?
S3_2 C13_2 1.807(5) . ?
S4_2 C10_2 1.732(5) . ?
S4_2 C14_2 1.818(5) . ?
C1_2 C2_2 1.409(7) . ?
C1_2 C5_2 1.423(6) . ?
C2_2 C3_2 1.407(6) . ?
C3_2 C4_2 1.407(6) . ?
C4_2 C5_2 1.419(6) . ?
C6_2 O6_2 1.239(5) . ?
C6_2 C7_2 1.468(6) . ?
C6_2 C10_2 1.487(6) . ?
C7_2 C8_2 1.448(6) . ?
C8_2 C9_2 1.435(6) . ?
C9_2 C10_2 1.440(6) . ?
Co1_3 C9_3 1.984(4) . ?
Co1_3 C8_3 1.985(4) . ?
Co1_3 C5_3 2.038(4) . ?
Co1_3 C1_3 2.048(4) . ?
Co1_3 C2_3 2.053(5) . ?
Co1_3 C10_3 2.070(4) . ?
Co1_3 C4_3 2.073(5) . ?
Co1_3 C3_3 2.074(5) . ?
Co1_3 C7_3 2.083(4) . ?
Co1_3 C6_3 2.341(4) . ?
S1_3 C7_3 1.737(4) . ?
S1_3 C11_3 1.794(5) . ?
S2_3 C8_3 1.750(4) . ?
S2_3 C12_3 1.794(5) . ?
S3_3 C9_3 1.761(4) . ?
S3_3 C13_3 1.792(5) . ?
S4_3 C10_3 1.747(4) . ?
S4_3 C14_3 1.824(5) . ?
C1_3 C2_3 1.403(7) . ?
C1_3 C5_3 1.407(6) . ?
C2_3 C3_3 1.408(7) . ?
C3_3 C4_3 1.405(7) . ?
C4_3 C5_3 1.404(6) . ?
C6_3 O6_3 1.237(5) . ?
C6_3 C7_3 1.477(6) . ?
C6_3 C10_3 1.486(6) . ?
C7_3 C8_3 1.447(6) . ?
C8_3 C9_3 1.448(6) . ?
C9_3 C10_3 1.430(6) . ?
|
1100837.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100837.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100837
loop_
_publ_author_name
'Schaefer, Carsten'
'Werz, Daniel B.'
'Staeb, Tobias H.'
'Gleiter, Rolf'
'Rominger, Frank'
_publ_section_title
;
CpCo-Stabilized Cyclopentadienones from Cyclobutadiene Complexes:
Experimental and Theoretical Investigations
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2113
_journal_paper_doi 10.1021/om050048r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C16 H19 Co O3 S4'
_chemical_formula_weight 446.48
_chemical_name_common in_paper_15
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 114.3310(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.4714(6)
_cell_length_b 8.3209(3)
_cell_length_c 15.0158(5)
_cell_measurement_temperature 200(2)
_cell_volume 1875.23(11)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0469
_diffrn_reflns_av_sigmaI/netI 0.0423
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 18886
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 1.36
_exptl_absorpt_coefficient_mu 1.372
_exptl_absorpt_correction_T_max 0.9101
_exptl_absorpt_correction_T_min 0.6032
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.581
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description polyhedron
_exptl_crystal_F_000 920
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.312
_refine_diff_density_min -0.332
_refine_diff_density_rms 0.063
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 222
_refine_ls_number_reflns 4300
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0566
_refine_ls_R_factor_gt 0.0319
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.7781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0613
_refine_ls_wR_factor_ref 0.0715
_reflns_number_gt 3175
_reflns_number_total 4300
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060511
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100837
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.226839(19) 0.64161(4) 0.28911(2) 0.02232(9) Uani 1 1 d . . .
S1 S 0.39385(4) 0.83717(8) 0.48104(5) 0.03962(17) Uani 1 1 d . . .
S2 S 0.42996(4) 0.66697(9) 0.29515(5) 0.04067(17) Uani 1 1 d . . .
S3 S 0.29799(5) 0.31121(8) 0.22161(5) 0.03733(17) Uani 1 1 d . . .
S4 S 0.18538(5) 0.26717(8) 0.36029(5) 0.04007(17) Uani 1 1 d . . .
C1 C 0.11153(15) 0.7620(3) 0.26510(16) 0.0268(5) Uani 1 1 d . . .
C2 C 0.17344(15) 0.8670(3) 0.25090(17) 0.0304(5) Uani 1 1 d . . .
H2 H 0.1975 0.9626 0.2867 0.037 Uiso 1 1 calc R . .
C3 C 0.19295(16) 0.8045(3) 0.17425(17) 0.0329(6) Uani 1 1 d . . .
H3 H 0.2320 0.8511 0.1494 0.039 Uiso 1 1 calc R . .
C4 C 0.14422(16) 0.6607(3) 0.14127(16) 0.0340(6) Uani 1 1 d . . .
H4 H 0.1449 0.5940 0.0902 0.041 Uiso 1 1 calc R . .
C5 C 0.09433(14) 0.6327(3) 0.19699(16) 0.0308(5) Uani 1 1 d . . .
H5 H 0.0561 0.5438 0.1904 0.037 Uiso 1 1 calc R . .
C6 C 0.28551(14) 0.5541(3) 0.45112(16) 0.0264(5) Uani 1 1 d . . .
O6 O 0.26757(11) 0.5653(2) 0.52290(12) 0.0378(4) Uani 1 1 d . . .
C7 C 0.33833(14) 0.6660(3) 0.41949(15) 0.0261(5) Uani 1 1 d . . .
C8 C 0.35571(14) 0.5929(3) 0.34237(16) 0.0262(5) Uani 1 1 d . . .
C9 C 0.30309(15) 0.4486(3) 0.31317(16) 0.0258(5) Uani 1 1 d . . .
C10 C 0.25383(14) 0.4334(3) 0.37220(16) 0.0247(5) Uani 1 1 d . . .
C11 C 0.31917(19) 0.9212(3) 0.52847(19) 0.0463(7) Uani 1 1 d . . .
H11A H 0.2619 0.9457 0.4743 0.069 Uiso 1 1 calc R . .
H11B H 0.3450 1.0200 0.5645 0.069 Uiso 1 1 calc R . .
H11C H 0.3099 0.8436 0.5725 0.069 Uiso 1 1 calc R . .
C12 C 0.53402(17) 0.6196(5) 0.3956(2) 0.0653(10) Uani 1 1 d . . .
H12A H 0.5355 0.6685 0.4556 0.098 Uiso 1 1 calc R . .
H12B H 0.5834 0.6617 0.3821 0.098 Uiso 1 1 calc R . .
H12C H 0.5399 0.5027 0.4038 0.098 Uiso 1 1 calc R . .
C13 C 0.3764(2) 0.1622(3) 0.2963(2) 0.0521(8) Uani 1 1 d . . .
H13A H 0.4367 0.2073 0.3227 0.078 Uiso 1 1 calc R . .
H13B H 0.3740 0.0676 0.2565 0.078 Uiso 1 1 calc R . .
H13C H 0.3609 0.1308 0.3503 0.078 Uiso 1 1 calc R . .
C14 C 0.1324(2) 0.3047(3) 0.4404(2) 0.0484(7) Uani 1 1 d . . .
H14A H 0.1774 0.3086 0.5080 0.073 Uiso 1 1 calc R . .
H14B H 0.0898 0.2185 0.4338 0.073 Uiso 1 1 calc R . .
H14C H 0.1009 0.4077 0.4235 0.073 Uiso 1 1 calc R . .
C15 C 0.07436(15) 0.7844(3) 0.33808(17) 0.0282(5) Uani 1 1 d . . .
O15 O 0.08958(12) 0.8976(2) 0.39254(13) 0.0391(4) Uani 1 1 d . . .
O16 O 0.01952(11) 0.6634(2) 0.33556(12) 0.0378(4) Uani 1 1 d . . .
C16 C -0.02300(18) 0.6764(4) 0.40244(19) 0.0452(7) Uani 1 1 d . . .
H16A H 0.0225 0.6917 0.4690 0.068 Uiso 1 1 calc R . .
H16B H -0.0565 0.5778 0.3996 0.068 Uiso 1 1 calc R . .
H16C H -0.0638 0.7683 0.3840 0.068 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.02006(15) 0.02445(16) 0.02069(15) 0.00107(13) 0.00663(12) 0.00298(13)
S1 0.0363(4) 0.0378(4) 0.0373(4) -0.0056(3) 0.0077(3) -0.0104(3)
S2 0.0274(3) 0.0625(5) 0.0343(3) 0.0119(3) 0.0149(3) 0.0001(3)
S3 0.0476(4) 0.0371(4) 0.0302(3) -0.0022(3) 0.0188(3) 0.0109(3)
S4 0.0531(4) 0.0288(3) 0.0477(4) -0.0068(3) 0.0302(3) -0.0098(3)
C1 0.0216(11) 0.0296(12) 0.0249(12) 0.0045(10) 0.0054(10) 0.0072(10)
C2 0.0305(13) 0.0272(12) 0.0309(12) 0.0061(11) 0.0099(10) 0.0064(11)
C3 0.0322(13) 0.0415(15) 0.0261(12) 0.0122(11) 0.0130(11) 0.0107(11)
C4 0.0319(13) 0.0447(15) 0.0201(11) -0.0005(11) 0.0052(10) 0.0070(12)
C5 0.0199(11) 0.0382(14) 0.0264(12) -0.0015(11) 0.0017(9) -0.0001(11)
C6 0.0234(12) 0.0300(13) 0.0239(12) 0.0013(10) 0.0080(10) 0.0037(10)
O6 0.0472(11) 0.0435(11) 0.0303(9) -0.0061(8) 0.0238(8) -0.0059(9)
C7 0.0226(11) 0.0288(13) 0.0224(11) 0.0021(10) 0.0049(9) 0.0022(10)
C8 0.0206(11) 0.0335(13) 0.0234(12) 0.0068(10) 0.0081(9) 0.0044(10)
C9 0.0269(12) 0.0275(13) 0.0225(11) 0.0026(10) 0.0096(10) 0.0071(10)
C10 0.0260(12) 0.0235(12) 0.0241(12) 0.0026(9) 0.0098(10) 0.0038(9)
C11 0.0636(19) 0.0368(15) 0.0364(15) -0.0066(12) 0.0186(14) 0.0021(14)
C12 0.0252(14) 0.109(3) 0.0566(19) 0.0218(19) 0.0116(14) -0.0004(17)
C13 0.0615(19) 0.0424(17) 0.0577(18) 0.0083(15) 0.0299(16) 0.0224(15)
C14 0.0529(18) 0.0460(17) 0.0592(19) -0.0049(14) 0.0361(15) -0.0137(14)
C15 0.0228(12) 0.0316(13) 0.0274(13) 0.0070(11) 0.0073(10) 0.0090(10)
O15 0.0452(11) 0.0369(10) 0.0409(10) -0.0046(8) 0.0235(9) 0.0020(8)
O16 0.0337(9) 0.0464(11) 0.0373(10) -0.0031(8) 0.0187(8) -0.0062(8)
C16 0.0452(16) 0.0589(19) 0.0394(15) 0.0008(14) 0.0254(13) -0.0081(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Co1 C9 42.66(9) . . ?
C8 Co1 C1 159.48(10) . . ?
C9 Co1 C1 154.71(9) . . ?
C8 Co1 C5 158.96(10) . . ?
C9 Co1 C5 120.92(10) . . ?
C1 Co1 C5 40.90(9) . . ?
C8 Co1 C2 124.47(10) . . ?
C9 Co1 C2 163.84(9) . . ?
C1 Co1 C2 40.71(9) . . ?
C5 Co1 C2 68.23(10) . . ?
C8 Co1 C7 41.53(9) . . ?
C9 Co1 C7 69.98(9) . . ?
C1 Co1 C7 121.12(9) . . ?
C5 Co1 C7 157.77(9) . . ?
C2 Co1 C7 106.63(9) . . ?
C8 Co1 C10 69.94(9) . . ?
C9 Co1 C10 41.34(9) . . ?
C1 Co1 C10 117.97(9) . . ?
C5 Co1 C10 106.31(9) . . ?
C2 Co1 C10 153.33(9) . . ?
C7 Co1 C10 68.04(9) . . ?
C8 Co1 C4 124.69(9) . . ?
C9 Co1 C4 110.14(9) . . ?
C1 Co1 C4 67.79(9) . . ?
C5 Co1 C4 40.05(9) . . ?
C2 Co1 C4 67.33(10) . . ?
C7 Co1 C4 159.81(9) . . ?
C10 Co1 C4 126.19(10) . . ?
C8 Co1 C3 110.21(9) . . ?
C9 Co1 C3 127.84(9) . . ?
C1 Co1 C3 67.79(9) . . ?
C5 Co1 C3 67.44(10) . . ?
C2 Co1 C3 40.07(9) . . ?
C7 Co1 C3 123.41(10) . . ?
C10 Co1 C3 163.91(9) . . ?
C4 Co1 C3 39.70(10) . . ?
C8 Co1 C6 66.42(8) . . ?
C9 Co1 C6 66.25(8) . . ?
C1 Co1 C6 107.01(8) . . ?
C5 Co1 C6 124.14(9) . . ?
C2 Co1 C6 121.51(9) . . ?
C7 Co1 C6 38.69(8) . . ?
C10 Co1 C6 38.55(8) . . ?
C4 Co1 C6 160.99(9) . . ?
C3 Co1 C6 157.19(9) . . ?
C7 S1 C11 103.49(12) . . ?
C8 S2 C12 99.54(12) . . ?
C9 S3 C13 99.70(12) . . ?
C10 S4 C14 105.51(12) . . ?
C2 C1 C5 107.3(2) . . ?
C2 C1 C15 125.3(2) . . ?
C5 C1 C15 127.4(2) . . ?
C2 C1 Co1 69.91(13) . . ?
C5 C1 Co1 69.72(12) . . ?
C15 C1 Co1 124.93(15) . . ?
C3 C2 C1 108.2(2) . . ?
C3 C2 Co1 71.11(13) . . ?
C1 C2 Co1 69.37(13) . . ?
C4 C3 C2 108.1(2) . . ?
C4 C3 Co1 70.03(13) . . ?
C2 C3 Co1 68.82(13) . . ?
C3 C4 C5 108.5(2) . . ?
C3 C4 Co1 70.27(13) . . ?
C5 C4 Co1 68.86(12) . . ?
C4 C5 C1 107.9(2) . . ?
C4 C5 Co1 71.10(13) . . ?
C1 C5 Co1 69.37(12) . . ?
O6 C6 C10 128.4(2) . . ?
O6 C6 C7 128.1(2) . . ?
C10 C6 C7 103.34(18) . . ?
O6 C6 Co1 137.94(17) . . ?
C10 C6 Co1 61.15(11) . . ?
C7 C6 Co1 60.98(11) . . ?
C8 C7 C6 109.32(19) . . ?
C8 C7 S1 122.63(17) . . ?
C6 C7 S1 126.50(16) . . ?
C8 C7 Co1 65.80(12) . . ?
C6 C7 Co1 80.33(13) . . ?
S1 C7 Co1 130.58(12) . . ?
C7 C8 C9 107.68(19) . . ?
C7 C8 S2 125.36(18) . . ?
C9 C8 S2 126.95(17) . . ?
C7 C8 Co1 72.67(12) . . ?
C9 C8 Co1 68.68(12) . . ?
S2 C8 Co1 125.02(12) . . ?
C10 C9 C8 107.99(19) . . ?
C10 C9 S3 124.58(17) . . ?
C8 C9 S3 127.42(17) . . ?
C10 C9 Co1 72.91(12) . . ?
C8 C9 Co1 68.66(12) . . ?
S3 C9 Co1 124.15(12) . . ?
C9 C10 C6 109.49(19) . . ?
C9 C10 S4 120.87(17) . . ?
C6 C10 S4 128.41(17) . . ?
C9 C10 Co1 65.76(12) . . ?
C6 C10 Co1 80.30(13) . . ?
S4 C10 Co1 129.11(12) . . ?
O15 C15 O16 123.7(2) . . ?
O15 C15 C1 124.8(2) . . ?
O16 C15 C1 111.5(2) . . ?
C15 O16 C16 115.92(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C8 1.978(2) . ?
Co1 C9 1.978(2) . ?
Co1 C1 2.043(2) . ?
Co1 C5 2.048(2) . ?
Co1 C2 2.051(2) . ?
Co1 C7 2.070(2) . ?
Co1 C10 2.073(2) . ?
Co1 C4 2.078(2) . ?
Co1 C3 2.081(2) . ?
Co1 C6 2.333(2) . ?
S1 C7 1.739(2) . ?
S1 C11 1.797(3) . ?
S2 C8 1.759(2) . ?
S2 C12 1.799(3) . ?
S3 C9 1.763(2) . ?
S3 C13 1.809(3) . ?
S4 C10 1.746(2) . ?
S4 C14 1.781(3) . ?
C1 C2 1.424(3) . ?
C1 C5 1.430(3) . ?
C1 C15 1.471(3) . ?
C2 C3 1.416(3) . ?
C3 C4 1.412(4) . ?
C4 C5 1.413(3) . ?
C6 O6 1.233(3) . ?
C6 C10 1.475(3) . ?
C6 C7 1.480(3) . ?
C7 C8 1.438(3) . ?
C8 C9 1.439(3) . ?
C9 C10 1.433(3) . ?
C15 O15 1.205(3) . ?
C15 O16 1.343(3) . ?
O16 C16 1.446(3) . ?
|
1100838.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100838.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100838
loop_
_publ_author_name
'Schaefer, Carsten'
'Werz, Daniel B.'
'Staeb, Tobias H.'
'Gleiter, Rolf'
'Rominger, Frank'
_publ_section_title
;
CpCo-Stabilized Cyclopentadienones from Cyclobutadiene Complexes:
Experimental and Theoretical Investigations
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2113
_journal_paper_doi 10.1021/om050048r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C17 H25 Co O S4 Si'
_chemical_formula_weight 460.63
_chemical_name_common in_paper_16
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 95.8050(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 7.97110(10)
_cell_length_b 14.6145(2)
_cell_length_c 17.77560(10)
_cell_measurement_temperature 200(2)
_cell_volume 2060.13(4)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0365
_diffrn_reflns_av_sigmaI/netI 0.0304
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 21109
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 1.81
_exptl_absorpt_coefficient_mu 1.299
_exptl_absorpt_correction_T_max 0.8811
_exptl_absorpt_correction_T_min 0.5627
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.485
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.319
_refine_diff_density_min -0.272
_refine_diff_density_rms 0.057
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 224
_refine_ls_number_reflns 4731
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.041
_refine_ls_R_factor_all 0.0411
_refine_ls_R_factor_gt 0.0268
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.6995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0573
_refine_ls_wR_factor_ref 0.0621
_reflns_number_gt 3843
_reflns_number_total 4731
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060512
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100838
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.05866(3) 0.889570(15) 0.173130(13) 0.01816(7) Uani 1 1 d . . .
Si1 Si -0.17283(6) 0.69726(3) 0.09671(3) 0.02426(12) Uani 1 1 d . . .
S1 S -0.03012(7) 0.83297(4) 0.34831(3) 0.03380(12) Uani 1 1 d . . .
S2 S 0.27363(6) 0.99813(3) 0.31828(3) 0.03010(12) Uani 1 1 d . . .
S3 S 0.14866(6) 1.10791(3) 0.14678(3) 0.03116(12) Uani 1 1 d . . .
S4 S -0.24401(6) 1.01596(3) 0.07591(3) 0.03033(12) Uani 1 1 d . . .
C1 C 0.0236(2) 0.76736(12) 0.11466(10) 0.0218(4) Uani 1 1 d . . .
C2 C 0.1519(2) 0.75979(12) 0.17729(10) 0.0236(4) Uani 1 1 d . . .
H2 H 0.1487 0.7192 0.2189 0.028 Uiso 1 1 calc R . .
C3 C 0.2846(2) 0.82273(13) 0.16727(11) 0.0272(4) Uani 1 1 d . . .
H3 H 0.3847 0.8308 0.2004 0.033 Uiso 1 1 calc R . .
C4 C 0.2405(2) 0.87056(13) 0.09970(11) 0.0278(4) Uani 1 1 d . . .
H4 H 0.3062 0.9166 0.0788 0.033 Uiso 1 1 calc R . .
C5 C 0.0809(2) 0.83830(12) 0.06790(10) 0.0255(4) Uani 1 1 d . . .
H5 H 0.0212 0.8604 0.0226 0.031 Uiso 1 1 calc R . .
C6 C -0.1915(2) 0.92528(12) 0.21886(10) 0.0218(4) Uani 1 1 d . . .
O6 O -0.33014(16) 0.88808(9) 0.21799(8) 0.0295(3) Uani 1 1 d . . .
C7 C -0.0404(2) 0.91131(12) 0.27316(10) 0.0219(4) Uani 1 1 d . . .
C8 C 0.0871(2) 0.97652(12) 0.25939(10) 0.0218(4) Uani 1 1 d . . .
C9 C 0.0323(2) 1.02368(12) 0.18969(10) 0.0215(4) Uani 1 1 d . . .
C10 C -0.1283(2) 0.98633(12) 0.16156(10) 0.0210(4) Uani 1 1 d . . .
C11 C -0.1972(3) 0.87612(16) 0.39927(13) 0.0478(6) Uani 1 1 d . . .
H11A H -0.1646 0.9358 0.4213 0.072 Uiso 1 1 calc R . .
H11B H -0.2179 0.8332 0.4397 0.072 Uiso 1 1 calc R . .
H11C H -0.3001 0.8829 0.3646 0.072 Uiso 1 1 calc R . .
C12 C 0.1800(3) 1.06472(15) 0.38882(11) 0.0355(5) Uani 1 1 d . . .
H12A H 0.1286 1.1200 0.3654 0.053 Uiso 1 1 calc R . .
H12B H 0.2674 1.0821 0.4291 0.053 Uiso 1 1 calc R . .
H12C H 0.0934 1.0282 0.4103 0.053 Uiso 1 1 calc R . .
C13 C 0.0161(3) 1.20625(14) 0.15323(14) 0.0445(6) Uani 1 1 d . . .
H13A H -0.0898 1.1972 0.1210 0.067 Uiso 1 1 calc R . .
H13B H 0.0737 1.2607 0.1364 0.067 Uiso 1 1 calc R . .
H13C H -0.0080 1.2146 0.2058 0.067 Uiso 1 1 calc R . .
C14 C -0.4259(3) 1.06913(16) 0.11018(13) 0.0429(5) Uani 1 1 d . . .
H14A H -0.4713 1.0289 0.1473 0.064 Uiso 1 1 calc R . .
H14B H -0.5122 1.0796 0.0678 0.064 Uiso 1 1 calc R . .
H14C H -0.3930 1.1277 0.1341 0.064 Uiso 1 1 calc R . .
C15 C -0.2195(3) 0.64814(16) 0.18841(12) 0.0416(5) Uani 1 1 d . . .
H15A H -0.2371 0.6978 0.2239 0.062 Uiso 1 1 calc R . .
H15B H -0.1245 0.6102 0.2091 0.062 Uiso 1 1 calc R . .
H15C H -0.3216 0.6105 0.1808 0.062 Uiso 1 1 calc R . .
C16 C -0.3477(3) 0.76785(14) 0.05105(13) 0.0370(5) Uani 1 1 d . . .
H16A H -0.4486 0.7298 0.0406 0.055 Uiso 1 1 calc R . .
H16B H -0.3152 0.7930 0.0035 0.055 Uiso 1 1 calc R . .
H16C H -0.3719 0.8180 0.0849 0.055 Uiso 1 1 calc R . .
C17 C -0.1315(3) 0.60402(14) 0.02921(13) 0.0409(5) Uani 1 1 d . . .
H17A H -0.0624 0.5564 0.0560 0.061 Uiso 1 1 calc R . .
H17B H -0.0715 0.6292 -0.0116 0.061 Uiso 1 1 calc R . .
H17C H -0.2389 0.5776 0.0078 0.061 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01812(12) 0.01771(12) 0.01843(12) -0.00011(9) 0.00076(9) 0.00041(9)
Si1 0.0236(3) 0.0230(3) 0.0257(3) -0.0028(2) 0.0002(2) -0.0025(2)
S1 0.0432(3) 0.0333(3) 0.0250(2) 0.0089(2) 0.0036(2) 0.0000(2)
S2 0.0242(2) 0.0352(3) 0.0293(3) -0.0045(2) -0.00540(19) -0.0018(2)
S3 0.0306(3) 0.0246(2) 0.0393(3) 0.0066(2) 0.0085(2) -0.0024(2)
S4 0.0315(3) 0.0352(3) 0.0229(2) 0.0032(2) -0.0041(2) 0.0066(2)
C1 0.0235(9) 0.0201(9) 0.0221(9) -0.0033(7) 0.0037(7) 0.0020(7)
C2 0.0229(9) 0.0201(9) 0.0276(10) 0.0000(7) 0.0021(7) 0.0048(7)
C3 0.0182(9) 0.0290(10) 0.0339(10) -0.0056(8) 0.0009(8) 0.0022(8)
C4 0.0252(10) 0.0284(10) 0.0314(10) -0.0029(8) 0.0100(8) -0.0032(8)
C5 0.0291(10) 0.0273(10) 0.0208(9) -0.0026(8) 0.0057(7) 0.0007(8)
C6 0.0222(9) 0.0223(9) 0.0208(9) -0.0043(7) 0.0014(7) 0.0020(7)
O6 0.0208(7) 0.0342(7) 0.0336(7) -0.0027(6) 0.0036(6) -0.0062(6)
C7 0.0251(9) 0.0224(9) 0.0181(8) -0.0002(7) 0.0016(7) 0.0007(7)
C8 0.0214(9) 0.0220(9) 0.0216(9) -0.0042(7) 0.0006(7) 0.0001(7)
C9 0.0231(9) 0.0188(8) 0.0226(9) 0.0000(7) 0.0029(7) 0.0009(7)
C10 0.0206(9) 0.0208(8) 0.0211(9) -0.0005(7) 0.0004(7) 0.0034(7)
C11 0.0632(16) 0.0469(14) 0.0372(13) -0.0025(11) 0.0233(12) -0.0115(12)
C12 0.0376(12) 0.0381(12) 0.0295(11) -0.0069(9) -0.0027(9) -0.0057(9)
C13 0.0546(15) 0.0203(10) 0.0599(15) 0.0043(10) 0.0126(12) 0.0012(10)
C14 0.0348(12) 0.0464(13) 0.0448(13) -0.0021(11) -0.0083(10) 0.0153(10)
C15 0.0386(12) 0.0483(13) 0.0381(12) 0.0043(10) 0.0041(10) -0.0142(10)
C16 0.0290(11) 0.0362(11) 0.0440(12) -0.0034(10) -0.0050(9) 0.0014(9)
C17 0.0427(13) 0.0340(12) 0.0448(13) -0.0145(10) -0.0012(10) -0.0020(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Co1 C9 42.58(7) . . ?
C8 Co1 C2 123.72(7) . . ?
C9 Co1 C2 162.35(7) . . ?
C8 Co1 C5 158.31(7) . . ?
C9 Co1 C5 121.08(7) . . ?
C2 Co1 C5 68.02(7) . . ?
C8 Co1 C7 41.63(7) . . ?
C9 Co1 C7 70.32(7) . . ?
C2 Co1 C7 106.57(7) . . ?
C5 Co1 C7 158.90(7) . . ?
C8 Co1 C10 70.20(7) . . ?
C9 Co1 C10 41.51(7) . . ?
C2 Co1 C10 154.89(7) . . ?
C5 Co1 C10 106.93(7) . . ?
C7 Co1 C10 68.83(7) . . ?
C8 Co1 C3 108.06(7) . . ?
C9 Co1 C3 125.34(7) . . ?
C2 Co1 C3 40.76(7) . . ?
C5 Co1 C3 67.79(8) . . ?
C7 Co1 C3 122.32(7) . . ?
C10 Co1 C3 162.23(7) . . ?
C8 Co1 C4 122.76(7) . . ?
C9 Co1 C4 108.43(7) . . ?
C2 Co1 C4 67.71(7) . . ?
C5 Co1 C4 40.46(7) . . ?
C7 Co1 C4 158.31(8) . . ?
C10 Co1 C4 125.38(7) . . ?
C3 Co1 C4 39.77(8) . . ?
C8 Co1 C1 159.71(7) . . ?
C9 Co1 C1 155.49(7) . . ?
C2 Co1 C1 40.97(7) . . ?
C5 Co1 C1 40.78(7) . . ?
C7 Co1 C1 121.78(7) . . ?
C10 Co1 C1 119.00(7) . . ?
C3 Co1 C1 68.91(7) . . ?
C4 Co1 C1 68.57(7) . . ?
C8 Co1 C6 67.40(7) . . ?
C9 Co1 C6 67.38(7) . . ?
C2 Co1 C6 121.83(7) . . ?
C5 Co1 C6 124.70(7) . . ?
C7 Co1 C6 39.44(7) . . ?
C10 Co1 C6 39.42(7) . . ?
C3 Co1 C6 157.43(7) . . ?
C4 Co1 C6 161.39(7) . . ?
C1 Co1 C6 107.25(7) . . ?
C15 Si1 C16 113.06(11) . . ?
C15 Si1 C17 110.29(11) . . ?
C16 Si1 C17 107.36(10) . . ?
C15 Si1 C1 107.52(9) . . ?
C16 Si1 C1 110.43(9) . . ?
C17 Si1 C1 108.08(9) . . ?
C7 S1 C11 100.07(10) . . ?
C8 S2 C12 97.26(9) . . ?
C9 S3 C13 101.13(10) . . ?
C10 S4 C14 100.58(9) . . ?
C5 C1 C2 105.15(15) . . ?
C5 C1 Si1 127.44(14) . . ?
C2 C1 Si1 127.39(13) . . ?
C5 C1 Co1 68.42(10) . . ?
C2 C1 Co1 68.18(10) . . ?
Si1 C1 Co1 128.75(9) . . ?
C3 C2 C1 109.40(16) . . ?
C3 C2 Co1 70.56(10) . . ?
C1 C2 Co1 70.84(10) . . ?
C4 C3 C2 107.67(16) . . ?
C4 C3 Co1 70.29(11) . . ?
C2 C3 Co1 68.68(10) . . ?
C3 C4 C5 108.17(16) . . ?
C3 C4 Co1 69.93(10) . . ?
C5 C4 Co1 68.79(10) . . ?
C4 C5 C1 109.58(16) . . ?
C4 C5 Co1 70.75(11) . . ?
C1 C5 Co1 70.81(10) . . ?
O6 C6 C7 128.19(17) . . ?
O6 C6 C10 128.73(16) . . ?
C7 C6 C10 102.73(14) . . ?
O6 C6 Co1 135.12(13) . . ?
C7 C6 Co1 61.25(9) . . ?
C10 C6 Co1 61.54(9) . . ?
C8 C7 C6 109.99(15) . . ?
C8 C7 S1 125.79(14) . . ?
C6 C7 S1 123.97(13) . . ?
C8 C7 Co1 67.12(10) . . ?
C6 C7 Co1 79.31(10) . . ?
S1 C7 Co1 124.68(10) . . ?
C7 C8 C9 107.78(15) . . ?
C7 C8 S2 126.14(14) . . ?
C9 C8 S2 126.05(13) . . ?
C7 C8 Co1 71.25(10) . . ?
C9 C8 Co1 69.06(10) . . ?
S2 C8 Co1 126.74(10) . . ?
C10 C9 C8 107.39(15) . . ?
C10 C9 S3 127.27(14) . . ?
C8 C9 S3 125.29(13) . . ?
C10 C9 Co1 71.23(10) . . ?
C8 C9 Co1 68.36(10) . . ?
S3 C9 Co1 123.70(9) . . ?
C9 C10 C6 110.10(15) . . ?
C9 C10 S4 125.56(13) . . ?
C6 C10 S4 124.09(13) . . ?
C9 C10 Co1 67.26(9) . . ?
C6 C10 Co1 79.04(10) . . ?
S4 C10 Co1 124.83(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C8 1.9868(17) . ?
Co1 C9 1.9962(17) . ?
Co1 C2 2.0355(17) . ?
Co1 C5 2.0393(18) . ?
Co1 C7 2.0419(17) . ?
Co1 C10 2.0494(17) . ?
Co1 C3 2.0605(18) . ?
Co1 C4 2.0651(19) . ?
Co1 C1 2.0711(17) . ?
Co1 C6 2.2887(18) . ?
Si1 C15 1.853(2) . ?
Si1 C16 1.854(2) . ?
Si1 C17 1.867(2) . ?
Si1 C1 1.8711(18) . ?
S1 C7 1.7549(18) . ?
S1 C11 1.799(2) . ?
S2 C8 1.7579(18) . ?
S2 C12 1.807(2) . ?
S3 C9 1.7606(18) . ?
S3 C13 1.794(2) . ?
S4 C10 1.7529(18) . ?
S4 C14 1.804(2) . ?
C1 C5 1.432(3) . ?
C1 C2 1.438(2) . ?
C2 C3 1.426(3) . ?
C3 C4 1.403(3) . ?
C4 C5 1.420(3) . ?
C6 O6 1.230(2) . ?
C6 C7 1.480(2) . ?
C6 C10 1.480(2) . ?
C7 C8 1.432(2) . ?
C8 C9 1.446(2) . ?
C9 C10 1.434(2) . ?
|
1100839.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100839.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100839
loop_
_publ_author_name
'Schaefer, Carsten'
'Werz, Daniel B.'
'Staeb, Tobias H.'
'Gleiter, Rolf'
'Rominger, Frank'
_publ_section_title
;
CpCo-Stabilized Cyclopentadienones from Cyclobutadiene Complexes:
Experimental and Theoretical Investigations
;
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2113
_journal_paper_doi 10.1021/om050048r
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C35 H27 Co O2 S4'
_chemical_formula_weight 666.74
_chemical_name_common in_paper_30
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 93.5300(10)
_cell_angle_beta 93.9120(10)
_cell_angle_gamma 102.0420(10)
_cell_formula_units_Z 2
_cell_length_a 10.3437(6)
_cell_length_b 10.4068(6)
_cell_length_c 14.8969(9)
_cell_measurement_reflns_used 6753
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 28.22
_cell_measurement_theta_min 2.34
_cell_volume 1559.90(16)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0216
_diffrn_reflns_av_sigmaI/netI 0.0313
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 16316
_diffrn_reflns_theta_full 28.28
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 2.01
_exptl_absorpt_coefficient_mu 0.849
_exptl_absorpt_correction_T_max 0.8832
_exptl_absorpt_correction_T_min 0.7788
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_density_diffrn 1.420
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 688
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.483
_refine_diff_density_min -0.261
_refine_diff_density_rms 0.053
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 380
_refine_ls_number_reflns 7629
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.024
_refine_ls_R_factor_all 0.0499
_refine_ls_R_factor_gt 0.0381
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.2878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.1046
_reflns_number_gt 6124
_reflns_number_total 7629
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060513
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100839
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.10465(5) 0.07202(5) 0.77770(4) 0.06182(15) Uani 1 1 d . . .
Co1 Co 0.40046(2) 0.23139(2) 0.851459(16) 0.04229(8) Uani 1 1 d . . .
S2 S 0.40079(6) 0.19908(6) 0.63217(4) 0.06269(15) Uani 1 1 d . . .
S3 S 0.49507(5) 0.52664(5) 0.78883(4) 0.05730(14) Uani 1 1 d . . .
S4 S 0.19994(6) 0.39685(6) 0.93541(4) 0.06094(15) Uani 1 1 d . . .
O1 O 0.2895(2) 0.1519(2) 1.09060(12) 0.0836(5) Uani 1 1 d . . .
O2 O 0.23317(16) -0.02770(17) 0.99450(11) 0.0670(4) Uani 1 1 d . . .
C1 C 0.22882(17) 0.21343(18) 0.78230(13) 0.0434(4) Uani 1 1 d . . .
C2 C 0.33904(18) 0.26011(18) 0.72821(12) 0.0434(4) Uani 1 1 d . . .
C3 C 0.37439(18) 0.38264(17) 0.78617(13) 0.0444(4) Uani 1 1 d . . .
C4 C 0.26394(18) 0.33612(18) 0.84017(12) 0.0436(4) Uani 1 1 d . . .
C11 C 0.41334(19) 0.13203(19) 0.96492(13) 0.0478(4) Uani 1 1 d . . .
C12 C 0.4473(2) 0.0593(2) 0.88978(14) 0.0516(5) Uani 1 1 d . . .
H12 H 0.4044 -0.0253 0.8671 0.062 Uiso 1 1 calc R . .
C13 C 0.5583(2) 0.1388(3) 0.85568(17) 0.0649(6) Uani 1 1 d . . .
H13 H 0.6017 0.1155 0.8065 0.078 Uiso 1 1 calc R . .
C14 C 0.5918(2) 0.2594(3) 0.90897(18) 0.0688(7) Uani 1 1 d . . .
H14 H 0.6612 0.3293 0.9008 0.083 Uiso 1 1 calc R . .
C15 C 0.5033(2) 0.2566(2) 0.97657(15) 0.0595(5) Uani 1 1 d . . .
H15 H 0.5034 0.3238 1.0208 0.071 Uiso 1 1 calc R . .
C16 C 0.3059(2) 0.0894(2) 1.02364(14) 0.0550(5) Uani 1 1 d . . .
C17 C 0.1287(3) -0.0813(3) 1.0498(2) 0.0911(9) Uani 1 1 d . . .
H17A H 0.1669 -0.1032 1.1059 0.137 Uiso 1 1 calc R . .
H17B H 0.0734 -0.1591 1.0188 0.137 Uiso 1 1 calc R . .
H17C H 0.0762 -0.0171 1.0616 0.137 Uiso 1 1 calc R . .
C21 C -0.03057(19) 0.1176(2) 0.71805(14) 0.0553(5) Uani 1 1 d . . .
C22 C -0.0362(3) 0.2437(3) 0.7025(2) 0.0830(8) Uani 1 1 d . . .
H22 H 0.0344 0.3128 0.7229 0.100 Uiso 1 1 calc R . .
C23 C -0.1480(4) 0.2684(4) 0.6560(3) 0.1155(13) Uani 1 1 d . . .
H23 H -0.1527 0.3547 0.6459 0.139 Uiso 1 1 calc R . .
C24 C -0.2505(3) 0.1683(6) 0.6252(2) 0.1256(18) Uani 1 1 d . . .
H24 H -0.3248 0.1855 0.5935 0.151 Uiso 1 1 calc R . .
C25 C -0.2440(3) 0.0443(6) 0.6409(3) 0.1331(18) Uani 1 1 d . . .
H25 H -0.3141 -0.0245 0.6195 0.160 Uiso 1 1 calc R . .
C26 C -0.1365(3) 0.0178(4) 0.6874(2) 0.0958(10) Uani 1 1 d . . .
H26 H -0.1344 -0.0687 0.6986 0.115 Uiso 1 1 calc R . .
C31 C 0.3038(2) 0.2526(2) 0.54480(14) 0.0594(5) Uani 1 1 d . . .
C32 C 0.3652(3) 0.3369(3) 0.48559(19) 0.0852(8) Uani 1 1 d . . .
H32 H 0.4569 0.3658 0.4909 0.102 Uiso 1 1 calc R . .
C33 C 0.2874(6) 0.3783(4) 0.4173(2) 0.1178(14) Uani 1 1 d . . .
H33 H 0.3276 0.4337 0.3758 0.141 Uiso 1 1 calc R . .
C34 C 0.1553(5) 0.3385(5) 0.4114(2) 0.1282(17) Uani 1 1 d . . .
H34 H 0.1045 0.3688 0.3668 0.154 Uiso 1 1 calc R . .
C35 C 0.0955(4) 0.2564(5) 0.4681(3) 0.1292(16) Uani 1 1 d . . .
H35 H 0.0035 0.2301 0.4630 0.155 Uiso 1 1 calc R . .
C36 C 0.1694(3) 0.2099(4) 0.5349(2) 0.0946(9) Uani 1 1 d . . .
H36 H 0.1275 0.1497 0.5729 0.114 Uiso 1 1 calc R . .
C41 C 0.4157(2) 0.62553(19) 0.72001(13) 0.0502(4) Uani 1 1 d . . .
C42 C 0.4686(3) 0.7590(2) 0.72910(17) 0.0661(6) Uani 1 1 d . . .
H42 H 0.5427 0.7931 0.7690 0.079 Uiso 1 1 calc R . .
C43 C 0.4102(3) 0.8420(2) 0.6782(2) 0.0805(8) Uani 1 1 d . . .
H43 H 0.4453 0.9322 0.6844 0.097 Uiso 1 1 calc R . .
C44 C 0.3021(3) 0.7931(3) 0.6191(2) 0.0843(8) Uani 1 1 d . . .
H44 H 0.2637 0.8496 0.5853 0.101 Uiso 1 1 calc R . .
C45 C 0.2503(3) 0.6603(3) 0.60991(19) 0.0805(8) Uani 1 1 d . . .
H45 H 0.1767 0.6265 0.5695 0.097 Uiso 1 1 calc R . .
C46 C 0.3070(2) 0.5760(2) 0.66030(16) 0.0649(6) Uani 1 1 d . . .
H46 H 0.2715 0.4858 0.6538 0.078 Uiso 1 1 calc R . .
C51 C 0.1068(2) 0.5071(2) 0.88898(13) 0.0510(4) Uani 1 1 d . . .
C52 C -0.0293(2) 0.4722(3) 0.87934(19) 0.0719(7) Uani 1 1 d . . .
H52 H -0.0729 0.3888 0.8925 0.086 Uiso 1 1 calc R . .
C53 C -0.1008(3) 0.5622(3) 0.8499(2) 0.0841(8) Uani 1 1 d . . .
H53 H -0.1930 0.5398 0.8443 0.101 Uiso 1 1 calc R . .
C54 C -0.0370(3) 0.6827(3) 0.82926(18) 0.0809(8) Uani 1 1 d . . .
H54 H -0.0858 0.7426 0.8092 0.097 Uiso 1 1 calc R . .
C55 C 0.0973(3) 0.7168(3) 0.8377(2) 0.0857(8) Uani 1 1 d . . .
H55 H 0.1401 0.7992 0.8222 0.103 Uiso 1 1 calc R . .
C56 C 0.1706(3) 0.6303(2) 0.86880(18) 0.0685(6) Uani 1 1 d . . .
H56 H 0.2627 0.6549 0.8762 0.082 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0521(3) 0.0467(3) 0.0858(4) 0.0241(3) -0.0004(3) 0.0051(2)
Co1 0.03786(13) 0.04575(14) 0.04683(15) 0.01650(10) -0.00077(10) 0.01470(10)
S2 0.0661(3) 0.0792(4) 0.0553(3) 0.0126(3) 0.0096(2) 0.0406(3)
S3 0.0469(3) 0.0516(3) 0.0708(3) 0.0232(2) -0.0085(2) 0.0036(2)
S4 0.0728(4) 0.0735(3) 0.0484(3) 0.0154(2) 0.0089(2) 0.0385(3)
O1 0.0965(14) 0.1033(14) 0.0590(10) 0.0049(10) 0.0167(9) 0.0366(11)
O2 0.0672(10) 0.0748(10) 0.0609(9) 0.0229(8) 0.0119(7) 0.0121(8)
C1 0.0377(8) 0.0456(9) 0.0498(10) 0.0162(7) -0.0016(7) 0.0133(7)
C2 0.0419(9) 0.0482(9) 0.0447(9) 0.0157(8) 0.0015(7) 0.0173(7)
C3 0.0414(9) 0.0427(9) 0.0513(10) 0.0169(8) -0.0003(7) 0.0116(7)
C4 0.0429(9) 0.0456(9) 0.0468(9) 0.0133(8) 0.0006(7) 0.0175(7)
C11 0.0509(10) 0.0529(10) 0.0438(9) 0.0148(8) -0.0056(8) 0.0204(8)
C12 0.0543(11) 0.0536(11) 0.0544(11) 0.0166(9) 0.0003(9) 0.0268(9)
C13 0.0500(11) 0.0904(17) 0.0671(14) 0.0294(12) 0.0076(10) 0.0365(11)
C14 0.0430(11) 0.0766(15) 0.0861(17) 0.0299(13) -0.0117(11) 0.0098(10)
C15 0.0565(12) 0.0622(12) 0.0589(12) 0.0084(10) -0.0169(10) 0.0166(10)
C16 0.0596(12) 0.0673(13) 0.0452(11) 0.0186(9) 0.0005(9) 0.0270(10)
C17 0.0677(16) 0.121(2) 0.090(2) 0.0527(18) 0.0198(14) 0.0156(16)
C21 0.0392(10) 0.0727(13) 0.0523(11) 0.0032(10) 0.0037(8) 0.0084(9)
C22 0.0655(15) 0.0855(18) 0.100(2) 0.0029(15) -0.0223(14) 0.0315(13)
C23 0.097(2) 0.154(3) 0.111(3) 0.004(2) -0.022(2) 0.074(3)
C24 0.0529(17) 0.254(6) 0.076(2) -0.005(3) -0.0094(15) 0.057(3)
C25 0.0545(18) 0.217(5) 0.103(3) -0.013(3) -0.0185(18) -0.013(3)
C26 0.0702(17) 0.107(2) 0.091(2) 0.0018(17) -0.0075(15) -0.0184(16)
C31 0.0702(14) 0.0735(14) 0.0431(10) 0.0086(10) 0.0087(9) 0.0325(11)
C32 0.109(2) 0.0881(19) 0.0676(16) 0.0242(14) 0.0246(15) 0.0314(17)
C33 0.190(4) 0.123(3) 0.0662(19) 0.0430(19) 0.039(2) 0.073(3)
C34 0.171(4) 0.190(4) 0.0540(17) 0.012(2) -0.003(2) 0.111(4)
C35 0.095(2) 0.225(5) 0.081(2) 0.019(3) -0.0123(19) 0.070(3)
C36 0.0727(18) 0.147(3) 0.0695(17) 0.0232(18) 0.0039(14) 0.0312(18)
C41 0.0564(11) 0.0473(10) 0.0492(10) 0.0151(8) 0.0022(8) 0.0133(8)
C42 0.0768(15) 0.0471(11) 0.0700(14) 0.0128(10) -0.0046(12) 0.0044(10)
C43 0.110(2) 0.0440(11) 0.0880(18) 0.0191(12) -0.0016(16) 0.0167(13)
C44 0.114(2) 0.0663(15) 0.0807(18) 0.0224(13) -0.0099(16) 0.0391(15)
C45 0.0936(19) 0.0694(15) 0.0784(17) 0.0111(13) -0.0267(14) 0.0269(14)
C46 0.0748(15) 0.0457(11) 0.0722(14) 0.0096(10) -0.0150(12) 0.0138(10)
C51 0.0570(11) 0.0581(11) 0.0451(10) 0.0076(8) 0.0071(8) 0.0269(9)
C52 0.0547(13) 0.0800(16) 0.0872(17) 0.0269(13) 0.0168(12) 0.0194(11)
C53 0.0565(14) 0.119(2) 0.0885(19) 0.0235(17) 0.0103(13) 0.0406(15)
C54 0.103(2) 0.0914(19) 0.0676(15) 0.0119(14) 0.0052(14) 0.0643(18)
C55 0.103(2) 0.0570(14) 0.102(2) 0.0156(14) 0.0009(17) 0.0286(14)
C56 0.0657(14) 0.0570(12) 0.0832(16) 0.0058(11) -0.0014(12) 0.0166(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C21 103.08(9) . . ?
C3 Co1 C1 63.48(7) . . ?
C3 Co1 C4 43.75(7) . . ?
C1 Co1 C4 43.77(8) . . ?
C3 Co1 C2 43.75(8) . . ?
C1 Co1 C2 43.67(7) . . ?
C4 Co1 C2 63.67(8) . . ?
C3 Co1 C11 153.94(8) . . ?
C1 Co1 C11 119.85(8) . . ?
C4 Co1 C11 118.18(8) . . ?
C2 Co1 C11 157.16(8) . . ?
C3 Co1 C12 165.23(8) . . ?
C1 Co1 C12 115.96(8) . . ?
C4 Co1 C12 146.72(8) . . ?
C2 Co1 C12 124.55(8) . . ?
C11 Co1 C12 40.46(8) . . ?
C3 Co1 C15 121.16(9) . . ?
C1 Co1 C15 147.08(9) . . ?
C4 Co1 C15 113.77(9) . . ?
C2 Co1 C15 162.19(9) . . ?
C11 Co1 C15 40.58(8) . . ?
C12 Co1 C15 68.13(9) . . ?
C3 Co1 C14 111.28(9) . . ?
C1 Co1 C14 172.39(9) . . ?
C4 Co1 C14 136.69(10) . . ?
C2 Co1 C14 128.72(9) . . ?
C11 Co1 C14 67.40(9) . . ?
C12 Co1 C14 67.54(9) . . ?
C15 Co1 C14 39.92(10) . . ?
C3 Co1 C13 129.47(9) . . ?
C1 Co1 C13 138.30(10) . . ?
C4 Co1 C13 173.09(9) . . ?
C2 Co1 C13 112.89(9) . . ?
C11 Co1 C13 67.49(8) . . ?
C12 Co1 C13 40.16(9) . . ?
C15 Co1 C13 67.48(10) . . ?
C14 Co1 C13 39.99(11) . . ?
C2 S2 C31 101.49(9) . . ?
C3 S3 C41 102.14(9) . . ?
C4 S4 C51 102.15(9) . . ?
C16 O2 C17 115.8(2) . . ?
C2 C1 C4 90.28(14) . . ?
C2 C1 S1 134.74(15) . . ?
C4 C1 S1 134.97(15) . . ?
C2 C1 Co1 68.30(10) . . ?
C4 C1 Co1 68.17(10) . . ?
S1 C1 Co1 122.76(9) . . ?
C1 C2 C3 89.75(15) . . ?
C1 C2 S2 135.58(15) . . ?
C3 C2 S2 134.64(14) . . ?
C1 C2 Co1 68.03(10) . . ?
C3 C2 Co1 67.89(10) . . ?
S2 C2 Co1 123.32(9) . . ?
C4 C3 C2 90.27(14) . . ?
C4 C3 S3 134.51(15) . . ?
C2 C3 S3 135.20(15) . . ?
C4 C3 Co1 68.28(9) . . ?
C2 C3 Co1 68.36(9) . . ?
S3 C3 Co1 122.58(10) . . ?
C3 C4 C1 89.70(15) . . ?
C3 C4 S4 136.07(15) . . ?
C1 C4 S4 134.21(14) . . ?
C3 C4 Co1 67.97(9) . . ?
C1 C4 Co1 68.06(10) . . ?
S4 C4 Co1 121.02(9) . . ?
C12 C11 C15 108.30(19) . . ?
C12 C11 C16 127.52(19) . . ?
C15 C11 C16 124.2(2) . . ?
C12 C11 Co1 70.08(10) . . ?
C15 C11 Co1 70.08(11) . . ?
C16 C11 Co1 126.26(13) . . ?
C13 C12 C11 107.4(2) . . ?
C13 C12 Co1 70.19(12) . . ?
C11 C12 Co1 69.46(10) . . ?
C14 C13 C12 108.2(2) . . ?
C14 C13 Co1 69.88(13) . . ?
C12 C13 Co1 69.65(11) . . ?
C15 C14 C13 108.8(2) . . ?
C15 C14 Co1 69.96(12) . . ?
C13 C14 Co1 70.13(12) . . ?
C14 C15 C11 107.3(2) . . ?
C14 C15 Co1 70.12(13) . . ?
C11 C15 Co1 69.33(11) . . ?
O1 C16 O2 124.6(2) . . ?
O1 C16 C11 124.0(2) . . ?
O2 C16 C11 111.37(18) . . ?
C22 C21 C26 119.0(3) . . ?
C22 C21 S1 124.17(18) . . ?
C26 C21 S1 116.9(2) . . ?
C21 C22 C23 119.4(3) . . ?
C24 C23 C22 120.7(4) . . ?
C25 C24 C23 119.5(3) . . ?
C24 C25 C26 120.9(4) . . ?
C25 C26 C21 120.6(4) . . ?
C36 C31 C32 119.5(3) . . ?
C36 C31 S2 120.9(2) . . ?
C32 C31 S2 119.6(2) . . ?
C31 C32 C33 118.9(3) . . ?
C34 C33 C32 120.2(3) . . ?
C35 C34 C33 121.2(3) . . ?
C34 C35 C36 120.4(4) . . ?
C31 C36 C35 119.8(3) . . ?
C46 C41 C42 119.90(19) . . ?
C46 C41 S3 123.69(16) . . ?
C42 C41 S3 116.41(17) . . ?
C41 C42 C43 119.3(2) . . ?
C44 C43 C42 120.9(2) . . ?
C43 C44 C45 119.6(2) . . ?
C44 C45 C46 120.4(2) . . ?
C41 C46 C45 119.9(2) . . ?
C52 C51 C56 120.0(2) . . ?
C52 C51 S4 119.81(17) . . ?
C56 C51 S4 120.07(17) . . ?
C51 C52 C53 119.4(2) . . ?
C54 C53 C52 120.2(3) . . ?
C53 C54 C55 120.5(2) . . ?
C54 C55 C56 120.4(3) . . ?
C55 C56 C51 119.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.7341(19) . ?
S1 C21 1.769(2) . ?
Co1 C3 1.9560(16) . ?
Co1 C1 1.9587(17) . ?
Co1 C4 1.9602(17) . ?
Co1 C2 1.9625(17) . ?
Co1 C11 2.0459(17) . ?
Co1 C12 2.0542(18) . ?
Co1 C15 2.056(2) . ?
Co1 C14 2.058(2) . ?
Co1 C13 2.061(2) . ?
S2 C2 1.744(2) . ?
S2 C31 1.776(2) . ?
S3 C3 1.7352(18) . ?
S3 C41 1.7751(19) . ?
S4 C4 1.744(2) . ?
S4 C51 1.7863(19) . ?
O1 C16 1.198(3) . ?
O2 C16 1.322(3) . ?
O2 C17 1.444(3) . ?
C1 C2 1.458(3) . ?
C1 C4 1.461(3) . ?
C2 C3 1.460(3) . ?
C3 C4 1.459(3) . ?
C11 C12 1.418(3) . ?
C11 C15 1.423(3) . ?
C11 C16 1.474(3) . ?
C12 C13 1.413(3) . ?
C13 C14 1.408(4) . ?
C14 C15 1.404(4) . ?
C21 C22 1.359(4) . ?
C21 C26 1.373(3) . ?
C22 C23 1.386(4) . ?
C23 C24 1.354(6) . ?
C24 C25 1.340(6) . ?
C25 C26 1.356(5) . ?
C31 C36 1.363(4) . ?
C31 C32 1.375(3) . ?
C32 C33 1.399(5) . ?
C33 C34 1.337(6) . ?
C34 C35 1.329(6) . ?
C35 C36 1.385(4) . ?
C41 C46 1.374(3) . ?
C41 C42 1.377(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.363(4) . ?
C44 C45 1.369(4) . ?
C45 C46 1.383(3) . ?
C51 C52 1.374(3) . ?
C51 C56 1.375(3) . ?
C52 C53 1.383(4) . ?
C53 C54 1.354(4) . ?
C54 C55 1.356(4) . ?
C55 C56 1.374(4) . ?
|
1100840.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100840.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100840
loop_
_publ_author_name
'Major, Quinn'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
Substituents Effects in POP Pincer Complexes of Ruthenium
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2492
_journal_page_last 2501
_journal_paper_doi 10.1021/om050053v
_journal_volume 24
_journal_year 2005
_chemical_absolute_configuration rmad
_chemical_formula_moiety 'C20 H44 Cl2 O P2 Ru'
_chemical_formula_sum 'C20 H44 Cl2 O P2 Ru'
_chemical_formula_weight 534.46
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.8430(12)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 7.35610(10)
_cell_length_b 14.3852(3)
_cell_length_c 11.9104(2)
_cell_measurement_reflns_used 13690
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.6
_cell_volume 1260.21(4)
_diffrn_ambient_temperature 150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0401
_diffrn_reflns_av_sigmaI/netI 0.0480
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 11339
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 2.77
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.969
_exptl_absorpt_correction_T_max 0.834
_exptl_absorpt_correction_T_min 0.612
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.408
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 560
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.18
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.04(2)
_refine_ls_extinction_coef none
_refine_ls_extinction_expression ?
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.017
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 236
_refine_ls_number_reflns 5249
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.017
_refine_ls_R_factor_all 0.0327
_refine_ls_R_factor_gt 0.0286
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0487P)2^] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0727
_refine_ls_wR_factor_ref 0.0752
_reflns_number_gt 5032
_reflns_number_total 5249
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 1100840
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.72350(3) 0.154152(14) 0.249683(17) 0.01308(8) Uani 1 1 d . . .
Cl1 Cl 0.62770(12) 0.27299(6) 0.37066(6) 0.02374(18) Uani 1 1 d . . .
Cl2 Cl 0.41974(9) 0.11747(6) 0.19109(6) 0.02080(16) Uani 1 1 d . . .
P1 P 0.75325(10) 0.03821(6) 0.39432(6) 0.01599(16) Uani 1 1 d . . .
P2 P 0.79675(11) 0.25644(5) 0.10668(7) 0.01546(16) Uani 1 1 d . . .
O1 O 1.0031(3) 0.17467(14) 0.28896(17) 0.0182(5) Uani 1 1 d . . .
C1 C 1.0058(4) 0.0391(3) 0.4057(3) 0.0238(7) Uani 1 1 d . . .
H1A H 1.0438 0.0150 0.4803 0.029 Uiso 1 1 calc R . .
H1B H 1.0566 -0.0026 0.3479 0.029 Uiso 1 1 calc R . .
C2 C 1.0809(4) 0.1361(2) 0.3904(3) 0.0227(8) Uani 1 1 d . . .
H2A H 1.0493 0.1754 0.4555 0.027 Uiso 1 1 calc R . .
H2B H 1.2149 0.1337 0.3850 0.027 Uiso 1 1 calc R . .
C3 C 1.0719(4) 0.2672(2) 0.2654(3) 0.0216(7) Uani 1 1 d . . .
H3A H 1.2036 0.2709 0.2832 0.026 Uiso 1 1 calc R . .
H3B H 1.0077 0.3142 0.3108 0.026 Uiso 1 1 calc R . .
C4 C 1.0378(4) 0.2841(2) 0.1422(3) 0.0229(7) Uani 1 1 d . . .
H4A H 1.1194 0.2445 0.0974 0.028 Uiso 1 1 calc R . .
H4B H 1.0634 0.3499 0.1239 0.028 Uiso 1 1 calc R . .
C5 C 0.7006(5) -0.0858(2) 0.3521(3) 0.0246(7) Uani 1 1 d . . .
C6 C 0.8127(6) -0.1615(3) 0.4128(3) 0.0393(10) Uani 1 1 d . . .
H6A H 0.7751 -0.2229 0.3854 0.059 Uiso 1 1 calc R . .
H6B H 0.7923 -0.1576 0.4938 0.059 Uiso 1 1 calc R . .
H6C H 0.9421 -0.1522 0.3980 0.059 Uiso 1 1 calc R . .
C7 C 0.7403(5) -0.0940(3) 0.2258(3) 0.0310(8) Uani 1 1 d . . .
H7A H 0.7143 -0.1575 0.2004 0.047 Uiso 1 1 calc R . .
H7B H 0.8685 -0.0795 0.2129 0.047 Uiso 1 1 calc R . .
H7C H 0.6633 -0.0502 0.1837 0.047 Uiso 1 1 calc R . .
C8 C 0.4974(6) -0.1051(3) 0.3649(3) 0.0352(9) Uani 1 1 d . . .
H8A H 0.4712 -0.1695 0.3429 0.053 Uiso 1 1 calc R . .
H8B H 0.4275 -0.0626 0.3166 0.053 Uiso 1 1 calc R . .
H8C H 0.4634 -0.0957 0.4433 0.053 Uiso 1 1 calc R . .
C9 C 0.6782(4) 0.0575(2) 0.5448(3) 0.0196(6) Uani 1 1 d . . .
C10 C 0.7134(5) -0.0256(2) 0.6239(3) 0.0270(7) Uani 1 1 d . . .
H10A H 0.6717 -0.0103 0.6994 0.041 Uiso 1 1 calc R . .
H10B H 0.8439 -0.0393 0.6267 0.041 Uiso 1 1 calc R . .
H10C H 0.6471 -0.0801 0.5957 0.041 Uiso 1 1 calc R . .
C11 C 0.4768(4) 0.0831(3) 0.5448(3) 0.0286(8) Uani 1 1 d . . .
H11A H 0.4378 0.0933 0.6221 0.043 Uiso 1 1 calc R . .
H11B H 0.4056 0.0324 0.5112 0.043 Uiso 1 1 calc R . .
H11C H 0.4577 0.1401 0.5010 0.043 Uiso 1 1 calc R . .
C12 C 0.7860(4) 0.1411(3) 0.5938(3) 0.0266(8) Uani 1 1 d . . .
H12A H 0.7490 0.1522 0.6714 0.040 Uiso 1 1 calc R . .
H12B H 0.7608 0.1966 0.5486 0.040 Uiso 1 1 calc R . .
H12C H 0.9165 0.1274 0.5925 0.040 Uiso 1 1 calc R . .
C13 C 0.8188(5) 0.1755(2) -0.0162(3) 0.0259(8) Uani 1 1 d . . .
C14 C 0.9630(6) 0.1985(3) -0.1042(3) 0.0422(10) Uani 1 1 d . . .
H14A H 0.9614 0.1506 -0.1628 0.063 Uiso 1 1 calc R . .
H14B H 1.0834 0.2003 -0.0680 0.063 Uiso 1 1 calc R . .
H14C H 0.9360 0.2591 -0.1380 0.063 Uiso 1 1 calc R . .
C15 C 0.8700(5) 0.0856(3) 0.0460(3) 0.0342(9) Uani 1 1 d . . .
H15A H 0.8872 0.0355 -0.0085 0.051 Uiso 1 1 calc R . .
H15B H 0.7724 0.0687 0.0973 0.051 Uiso 1 1 calc R . .
H15C H 0.9831 0.0953 0.0890 0.051 Uiso 1 1 calc R . .
C16 C 0.6330(4) 0.1609(3) -0.0751(3) 0.0311(7) Uani 1 1 d . . .
H16A H 0.6470 0.1183 -0.1385 0.047 Uiso 1 1 calc R . .
H16B H 0.5868 0.2208 -0.1025 0.047 Uiso 1 1 calc R . .
H16C H 0.5471 0.1345 -0.0217 0.047 Uiso 1 1 calc R . .
C17 C 0.6883(4) 0.3699(2) 0.0682(3) 0.0222(7) Uani 1 1 d . . .
C18 C 0.4820(5) 0.3567(3) 0.0698(3) 0.0314(9) Uani 1 1 d . . .
H18A H 0.4220 0.4154 0.0499 0.047 Uiso 1 1 calc R . .
H18B H 0.4452 0.3375 0.1451 0.047 Uiso 1 1 calc R . .
H18C H 0.4466 0.3086 0.0153 0.047 Uiso 1 1 calc R . .
C19 C 0.7398(5) 0.4410(2) 0.1594(3) 0.0328(8) Uani 1 1 d . . .
H19A H 0.6841 0.5011 0.1412 0.049 Uiso 1 1 calc R . .
H19B H 0.8723 0.4478 0.1630 0.049 Uiso 1 1 calc R . .
H19C H 0.6959 0.4193 0.2322 0.049 Uiso 1 1 calc R . .
C20 C 0.7503(5) 0.4059(3) -0.0466(3) 0.0330(9) Uani 1 1 d . . .
H20A H 0.6899 0.4652 -0.0632 0.050 Uiso 1 1 calc R . .
H20B H 0.7182 0.3605 -0.1049 0.050 Uiso 1 1 calc R . .
H20C H 0.8823 0.4151 -0.0449 0.050 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01334(11) 0.01340(12) 0.01248(11) -0.00047(9) -0.00050(7) 0.00056(11)
Cl1 0.0312(5) 0.0206(4) 0.0196(4) -0.0043(3) 0.0031(3) 0.0067(3)
Cl2 0.0150(3) 0.0240(4) 0.0234(4) 0.0002(3) -0.0020(3) -0.0025(3)
P1 0.0167(4) 0.0178(4) 0.0134(4) 0.0021(3) -0.0021(3) 0.0014(3)
P2 0.0144(4) 0.0159(4) 0.0161(4) 0.0040(3) 0.0002(3) 0.0001(3)
O1 0.0162(10) 0.0184(13) 0.0199(11) 0.0024(8) -0.0032(8) -0.0010(8)
C1 0.0199(15) 0.0280(17) 0.0234(17) 0.0084(14) -0.0006(12) 0.0042(14)
C2 0.0142(13) 0.036(2) 0.0177(14) 0.0049(13) -0.0048(10) -0.0017(13)
C3 0.0181(15) 0.0192(16) 0.0274(17) -0.0009(13) -0.0022(12) -0.0069(13)
C4 0.0164(15) 0.0232(17) 0.0292(18) 0.0050(14) 0.0011(12) -0.0038(13)
C5 0.0381(19) 0.0161(16) 0.0196(16) 0.0045(12) -0.0021(13) 0.0003(14)
C6 0.060(3) 0.0236(18) 0.034(2) 0.0056(16) -0.0130(19) 0.0086(18)
C7 0.043(2) 0.024(2) 0.0257(17) -0.0009(15) -0.0016(15) 0.0043(16)
C8 0.047(2) 0.030(2) 0.028(2) 0.0074(15) -0.0054(16) -0.0143(17)
C9 0.0207(14) 0.0242(17) 0.0139(15) 0.0034(12) -0.0011(11) -0.0010(13)
C10 0.0311(17) 0.0314(19) 0.0185(16) 0.0082(14) -0.0028(13) 0.0001(15)
C11 0.0215(16) 0.039(2) 0.0256(18) 0.0006(15) 0.0020(13) 0.0021(15)
C12 0.0324(16) 0.033(2) 0.0146(14) -0.0002(14) -0.0036(11) -0.0009(16)
C13 0.0282(16) 0.031(2) 0.0191(15) -0.0036(13) 0.0067(12) -0.0033(14)
C14 0.040(2) 0.055(3) 0.032(2) -0.0136(19) 0.0181(17) -0.011(2)
C15 0.0326(19) 0.0226(18) 0.047(2) -0.0056(17) 0.0055(17) 0.0018(16)
C16 0.0364(17) 0.0365(19) 0.0204(15) -0.0077(18) 0.0004(12) -0.011(2)
C17 0.0211(16) 0.0193(16) 0.0262(17) 0.0075(13) -0.0018(12) 0.0004(13)
C18 0.0216(17) 0.0226(18) 0.050(2) 0.0100(17) -0.0047(16) 0.0034(15)
C19 0.038(2) 0.0166(17) 0.044(2) -0.0020(15) 0.0054(17) 0.0007(15)
C20 0.0330(19) 0.030(2) 0.036(2) 0.0182(16) -0.0025(16) -0.0035(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100841.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100841.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100841
loop_
_publ_author_name
'Major, Quinn'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
Substituents Effects in POP Pincer Complexes of Ruthenium
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2492
_journal_page_last 2501
_journal_paper_doi 10.1021/om050053v
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C32 H72 Cl3 O2 P4 Ru2, F6 P'
_chemical_formula_sum 'C32 H72 Cl3 F6 O2 P5 Ru2'
_chemical_formula_weight 1066.24
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 68.844(4)
_cell_angle_beta 89.075(5)
_cell_angle_gamma 83.462(5)
_cell_formula_units_Z 2
_cell_length_a 10.9035(8)
_cell_length_b 14.2678(11)
_cell_length_c 15.5810(13)
_cell_measurement_reflns_used 59141
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.3
_cell_volume 2245.0(3)
_diffrn_ambient_temperature 150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.1758
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 23484
_diffrn_reflns_theta_max 27.62
_diffrn_reflns_theta_min 2.57
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.082
_exptl_absorpt_correction_T_max 0.981
_exptl_absorpt_correction_T_min 0.720
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.577
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1096.0
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.02
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 452
_refine_ls_number_reflns 23484
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.1860
_refine_ls_R_factor_gt 0.1039
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+14.1036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2273
_refine_ls_wR_factor_ref 0.2738
_reflns_number_gt 12819
_reflns_number_total 23484
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100841
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.21797(6) 0.08521(5) 0.16997(5) 0.02934(18) Uani 1 1 d . . .
Ru2 Ru 0.20905(6) -0.13186(5) 0.34176(5) 0.02893(18) Uani 1 1 d . . .
Cl1 Cl 0.38547(18) -0.04137(15) 0.26488(15) 0.0349(5) Uani 1 1 d . . .
Cl2 Cl 0.12934(19) 0.05192(14) 0.31782(14) 0.0320(4) Uani 1 1 d . . .
Cl3 Cl 0.13857(19) -0.08110(15) 0.18576(14) 0.0328(5) Uani 1 1 d . . .
P1 P 0.3316(2) 0.21391(16) 0.15850(16) 0.0347(5) Uani 1 1 d . . .
P2 P 0.0542(2) 0.16860(16) 0.07305(16) 0.0332(5) Uani 1 1 d . . .
P3 P 0.3160(2) -0.28444(15) 0.36361(15) 0.0304(5) Uani 1 1 d . . .
P4 P 0.0352(2) -0.17938(16) 0.42249(16) 0.0343(5) Uani 1 1 d . . .
O1 O 0.3059(5) 0.0879(4) 0.0458(4) 0.0357(14) Uani 1 1 d . . .
O2 O 0.2813(5) -0.1529(4) 0.4757(4) 0.0355(13) Uani 1 1 d . . .
C1 C 0.4150(9) 0.2241(6) 0.0520(6) 0.040(2) Uani 1 1 d . . .
H1A H 0.3698 0.2772 -0.0013 0.048 Uiso 1 1 calc R . .
H1B H 0.4983 0.2436 0.0562 0.048 Uiso 1 1 calc R . .
C2 C 0.4264(8) 0.1231(7) 0.0379(7) 0.038(2) Uani 1 1 d . . .
H2A H 0.4593 0.1315 -0.0237 0.046 Uiso 1 1 calc R . .
H2B H 0.4843 0.0729 0.0848 0.046 Uiso 1 1 calc R . .
C3 C 0.2324(8) 0.1345(7) -0.0399(6) 0.041(2) Uani 1 1 d . . .
H3A H 0.2612 0.1021 -0.0843 0.050 Uiso 1 1 calc R . .
H3B H 0.2427 0.2073 -0.0676 0.050 Uiso 1 1 calc R . .
C4 C 0.0985(8) 0.1220(7) -0.0205(6) 0.039(2) Uani 1 1 d . . .
H4A H 0.0857 0.0498 -0.0019 0.047 Uiso 1 1 calc R . .
H4B H 0.0469 0.1610 -0.0765 0.047 Uiso 1 1 calc R . .
C5 C 0.4608(8) 0.1781(7) 0.2453(6) 0.041(2) Uani 1 1 d . . .
H5A H 0.5121 0.1190 0.2377 0.049 Uiso 1 1 calc R . .
C6 C 0.4174(9) 0.1399(7) 0.3476(6) 0.042(2) Uani 1 1 d . . .
H6A H 0.4895 0.1220 0.3896 0.064 Uiso 1 1 calc R . .
H6B H 0.3738 0.0803 0.3592 0.064 Uiso 1 1 calc R . .
H6C H 0.3618 0.1936 0.3579 0.064 Uiso 1 1 calc R . .
C7 C 0.5490(8) 0.2584(7) 0.2331(7) 0.043(2) Uani 1 1 d . . .
H7A H 0.6132 0.2323 0.2820 0.064 Uiso 1 1 calc R . .
H7B H 0.5025 0.3199 0.2367 0.064 Uiso 1 1 calc R . .
H7C H 0.5875 0.2743 0.1730 0.064 Uiso 1 1 calc R . .
C8 C 0.2652(9) 0.3458(6) 0.1408(6) 0.042(2) Uani 1 1 d . . .
H8A H 0.1913 0.3594 0.0992 0.051 Uiso 1 1 calc R . .
C9 C 0.2145(10) 0.3508(7) 0.2310(8) 0.056(3) Uani 1 1 d . . .
H9A H 0.1789 0.4202 0.2213 0.085 Uiso 1 1 calc R . .
H9B H 0.2814 0.3301 0.2775 0.085 Uiso 1 1 calc R . .
H9C H 0.1504 0.3052 0.2521 0.085 Uiso 1 1 calc R . .
C10 C 0.3445(11) 0.4309(7) 0.0928(7) 0.058(3) Uani 1 1 d . . .
H10A H 0.2985 0.4961 0.0869 0.086 Uiso 1 1 calc R . .
H10B H 0.3651 0.4305 0.0314 0.086 Uiso 1 1 calc R . .
H10C H 0.4207 0.4205 0.1292 0.086 Uiso 1 1 calc R . .
C11 C 0.0269(9) 0.3081(6) 0.0134(6) 0.041(2) Uani 1 1 d . . .
H11A H 0.1104 0.3321 0.0019 0.049 Uiso 1 1 calc R . .
C12 C -0.0405(10) 0.3454(7) -0.0818(7) 0.062(3) Uani 1 1 d . . .
H12A H -0.0499 0.4195 -0.1077 0.094 Uiso 1 1 calc R . .
H12B H -0.1221 0.3215 -0.0747 0.094 Uiso 1 1 calc R . .
H12C H 0.0080 0.3188 -0.1233 0.094 Uiso 1 1 calc R . .
C13 C -0.0380(10) 0.3600(7) 0.0751(7) 0.055(3) Uani 1 1 d . . .
H13A H -0.0503 0.4333 0.0417 0.082 Uiso 1 1 calc R . .
H13B H 0.0131 0.3450 0.1307 0.082 Uiso 1 1 calc R . .
H13C H -0.1182 0.3350 0.0925 0.082 Uiso 1 1 calc R . .
C14 C -0.0982(8) 0.1210(7) 0.1104(6) 0.038(2) Uani 1 1 d . . .
H14A H -0.0804 0.0456 0.1361 0.045 Uiso 1 1 calc R . .
C15 C -0.1523(8) 0.1496(7) 0.1881(6) 0.043(2) Uani 1 1 d . . .
H15A H -0.2305 0.1208 0.2055 0.065 Uiso 1 1 calc R . .
H15B H -0.1674 0.2235 0.1684 0.065 Uiso 1 1 calc R . .
H15C H -0.0945 0.1233 0.2411 0.065 Uiso 1 1 calc R . .
C16 C -0.1967(9) 0.1446(7) 0.0331(7) 0.049(3) Uani 1 1 d . . .
H16A H -0.2720 0.1154 0.0596 0.074 Uiso 1 1 calc R . .
H16B H -0.1653 0.1153 -0.0121 0.074 Uiso 1 1 calc R . .
H16C H -0.2155 0.2181 0.0028 0.074 Uiso 1 1 calc R . .
C17 C 0.3800(8) -0.3188(6) 0.4809(6) 0.036(2) Uani 1 1 d . . .
H17A H 0.3235 -0.3587 0.5263 0.044 Uiso 1 1 calc R . .
H17B H 0.4608 -0.3607 0.4877 0.044 Uiso 1 1 calc R . .
C18 C 0.3959(8) -0.2237(7) 0.4980(7) 0.041(2) Uani 1 1 d . . .
H18A H 0.4196 -0.2412 0.5635 0.049 Uiso 1 1 calc R . .
H18B H 0.4634 -0.1904 0.4600 0.049 Uiso 1 1 calc R . .
C19 C 0.1976(8) -0.1766(7) 0.5524(6) 0.039(2) Uani 1 1 d . . .
H19A H 0.2209 -0.1462 0.5968 0.047 Uiso 1 1 calc R . .
H19B H 0.2027 -0.2508 0.5846 0.047 Uiso 1 1 calc R . .
C20 C 0.0685(9) -0.1350(6) 0.5159(6) 0.038(2) Uani 1 1 d . . .
H20A H 0.0601 -0.0602 0.4924 0.046 Uiso 1 1 calc R . .
H20B H 0.0091 -0.1582 0.5658 0.046 Uiso 1 1 calc R . .
C21 C 0.4531(8) -0.2942(7) 0.2925(6) 0.038(2) Uani 1 1 d . . .
H21A H 0.4719 -0.3677 0.3028 0.045 Uiso 1 1 calc R . .
C22 C 0.5722(8) -0.2625(7) 0.3204(8) 0.052(3) Uani 1 1 d . . .
H22A H 0.6386 -0.2704 0.2795 0.078 Uiso 1 1 calc R . .
H22B H 0.5960 -0.3053 0.3841 0.078 Uiso 1 1 calc R . .
H22C H 0.5579 -0.1916 0.3152 0.078 Uiso 1 1 calc R . .
C23 C 0.4256(9) -0.2410(7) 0.1891(6) 0.047(2) Uani 1 1 d . . .
H23A H 0.5002 -0.2485 0.1551 0.071 Uiso 1 1 calc R . .
H23B H 0.3994 -0.1689 0.1754 0.071 Uiso 1 1 calc R . .
H23C H 0.3596 -0.2714 0.1704 0.071 Uiso 1 1 calc R . .
C24 C 0.2458(8) -0.3992(6) 0.3707(6) 0.038(2) Uani 1 1 d . . .
H24A H 0.1718 -0.4017 0.4099 0.045 Uiso 1 1 calc R . .
C25 C 0.3292(9) -0.4987(7) 0.4174(7) 0.050(3) Uani 1 1 d . . .
H25A H 0.2858 -0.5556 0.4187 0.076 Uiso 1 1 calc R . .
H25B H 0.3498 -0.5055 0.4806 0.076 Uiso 1 1 calc R . .
H25C H 0.4051 -0.4984 0.3829 0.076 Uiso 1 1 calc R . .
C26 C 0.1975(10) -0.3891(7) 0.2748(6) 0.053(3) Uani 1 1 d . . .
H26A H 0.1604 -0.4502 0.2796 0.080 Uiso 1 1 calc R . .
H26B H 0.2662 -0.3807 0.2323 0.080 Uiso 1 1 calc R . .
H26C H 0.1352 -0.3300 0.2516 0.080 Uiso 1 1 calc R . .
C27 C 0.0060(9) -0.3130(7) 0.4850(7) 0.045(2) Uani 1 1 d . . .
H27A H 0.0892 -0.3535 0.4994 0.054 Uiso 1 1 calc R . .
C28 C -0.0621(8) -0.3549(6) 0.4241(7) 0.044(2) Uani 1 1 d . . .
H28A H -0.0752 -0.4252 0.4593 0.067 Uiso 1 1 calc R . .
H28B H -0.0125 -0.3523 0.3704 0.067 Uiso 1 1 calc R . .
H28C H -0.1420 -0.3141 0.4035 0.067 Uiso 1 1 calc R . .
C29 C -0.0580(10) -0.3347(8) 0.5783(7) 0.058(3) Uani 1 1 d . . .
H29A H -0.0679 -0.4069 0.6056 0.087 Uiso 1 1 calc R . .
H29B H -0.1394 -0.2948 0.5685 0.087 Uiso 1 1 calc R . .
H29C H -0.0075 -0.3162 0.6198 0.087 Uiso 1 1 calc R . .
C30 C -0.1121(8) -0.1030(6) 0.3698(6) 0.039(2) Uani 1 1 d . . .
H30A H -0.0926 -0.0314 0.3458 0.047 Uiso 1 1 calc R . .
C31 C -0.2185(9) -0.1046(8) 0.4375(8) 0.058(3) Uani 1 1 d . . .
H31A H -0.2921 -0.0626 0.4033 0.086 Uiso 1 1 calc R . .
H31B H -0.1933 -0.0779 0.4835 0.086 Uiso 1 1 calc R . .
H31C H -0.2374 -0.1743 0.4685 0.086 Uiso 1 1 calc R . .
C32 C -0.1566(8) -0.1211(7) 0.2857(6) 0.045(2) Uani 1 1 d . . .
H32A H -0.2340 -0.0777 0.2615 0.067 Uiso 1 1 calc R . .
H32B H -0.1705 -0.1922 0.3031 0.067 Uiso 1 1 calc R . .
H32C H -0.0940 -0.1052 0.2383 0.067 Uiso 1 1 calc R . .
P5 P 0.2516(3) -0.5069(2) 0.7688(2) 0.0604(8) Uani 1 1 d . . .
F1 F 0.3959(8) -0.5211(8) 0.7711(9) 0.145(4) Uani 1 1 d . . .
F2 F 0.1054(8) -0.4924(7) 0.7616(7) 0.125(3) Uani 1 1 d . . .
F3 F 0.2537(12) -0.5025(7) 0.6669(6) 0.150(5) Uani 1 1 d . . .
F4 F 0.2417(11) -0.5162(8) 0.8696(6) 0.144(4) Uani 1 1 d . . .
F5 F 0.2535(11) -0.6261(5) 0.8039(7) 0.143(4) Uani 1 1 d . . .
F6 F 0.2509(8) -0.3881(5) 0.7338(6) 0.105(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0334(4) 0.0267(3) 0.0294(4) -0.0108(3) 0.0008(3) -0.0071(3)
Ru2 0.0321(4) 0.0269(3) 0.0292(4) -0.0109(3) -0.0003(3) -0.0064(3)
Cl1 0.0319(10) 0.0314(10) 0.0405(12) -0.0107(9) 0.0009(9) -0.0077(9)
Cl2 0.0376(11) 0.0300(10) 0.0310(10) -0.0138(8) 0.0041(9) -0.0056(9)
Cl3 0.0400(11) 0.0318(10) 0.0294(10) -0.0132(8) -0.0003(9) -0.0084(9)
P1 0.0396(13) 0.0326(11) 0.0359(13) -0.0152(10) 0.0007(11) -0.0109(10)
P2 0.0361(12) 0.0293(11) 0.0331(12) -0.0096(9) -0.0005(10) -0.0049(10)
P3 0.0324(11) 0.0278(11) 0.0318(12) -0.0113(9) 0.0001(10) -0.0057(9)
P4 0.0357(12) 0.0300(11) 0.0357(12) -0.0096(10) 0.0031(10) -0.0055(10)
O1 0.039(3) 0.035(3) 0.032(3) -0.011(3) -0.003(3) -0.007(3)
O2 0.044(3) 0.028(3) 0.035(3) -0.015(3) 0.000(3) 0.001(3)
C1 0.048(5) 0.034(5) 0.037(5) -0.011(4) -0.010(4) -0.005(4)
C2 0.033(5) 0.043(5) 0.046(5) -0.024(4) 0.009(4) -0.010(4)
C3 0.052(6) 0.059(6) 0.020(4) -0.022(4) -0.003(4) -0.006(5)
C4 0.043(5) 0.039(5) 0.037(5) -0.014(4) -0.004(4) -0.008(4)
C5 0.043(5) 0.046(5) 0.036(5) -0.015(4) 0.002(4) -0.018(5)
C6 0.055(6) 0.045(5) 0.031(5) -0.014(4) -0.004(5) -0.021(5)
C7 0.040(5) 0.047(5) 0.049(6) -0.022(5) 0.002(5) -0.019(5)
C8 0.057(6) 0.029(4) 0.041(5) -0.011(4) -0.006(5) -0.008(4)
C9 0.065(7) 0.039(5) 0.070(7) -0.030(5) -0.011(6) 0.015(5)
C10 0.081(8) 0.032(5) 0.056(7) -0.008(5) -0.010(6) -0.020(5)
C11 0.053(6) 0.027(4) 0.043(5) -0.011(4) -0.007(5) -0.012(4)
C12 0.065(7) 0.040(6) 0.064(7) 0.004(5) -0.029(6) -0.005(5)
C13 0.059(6) 0.029(5) 0.069(7) -0.012(5) 0.013(6) 0.001(5)
C14 0.038(5) 0.039(5) 0.037(5) -0.011(4) -0.008(4) -0.012(4)
C15 0.036(5) 0.040(5) 0.046(6) -0.011(4) -0.005(4) 0.009(4)
C16 0.041(5) 0.054(6) 0.056(6) -0.020(5) -0.003(5) -0.014(5)
C17 0.035(5) 0.035(5) 0.032(5) -0.006(4) 0.001(4) 0.004(4)
C18 0.032(5) 0.041(5) 0.051(6) -0.020(4) -0.013(4) 0.006(4)
C19 0.050(6) 0.038(5) 0.026(4) -0.008(4) 0.002(4) -0.003(4)
C20 0.054(6) 0.033(4) 0.029(5) -0.014(4) 0.006(4) -0.003(4)
C21 0.038(5) 0.038(5) 0.039(5) -0.016(4) 0.000(4) -0.003(4)
C22 0.041(5) 0.040(5) 0.083(8) -0.031(5) 0.021(6) -0.013(5)
C23 0.058(6) 0.045(5) 0.044(6) -0.024(5) 0.010(5) -0.005(5)
C24 0.037(5) 0.033(4) 0.041(5) -0.010(4) 0.001(4) -0.011(4)
C25 0.054(6) 0.036(5) 0.059(7) -0.013(5) 0.000(5) -0.009(5)
C26 0.075(7) 0.048(6) 0.045(6) -0.018(5) -0.010(6) -0.028(6)
C27 0.047(5) 0.039(5) 0.047(6) -0.014(4) 0.005(5) -0.004(5)
C28 0.038(5) 0.033(5) 0.058(6) -0.013(4) -0.003(5) -0.005(4)
C29 0.056(6) 0.050(6) 0.056(7) -0.003(5) 0.007(6) -0.007(5)
C30 0.035(5) 0.035(5) 0.039(5) -0.002(4) 0.003(4) -0.011(4)
C31 0.039(5) 0.069(7) 0.065(7) -0.025(6) 0.007(5) -0.005(5)
C32 0.038(5) 0.049(6) 0.040(5) -0.006(4) -0.004(4) -0.012(5)
P5 0.081(2) 0.0415(15) 0.0531(18) -0.0127(13) 0.0124(16) -0.0015(15)
F1 0.079(6) 0.120(8) 0.217(12) -0.045(8) 0.011(7) 0.016(5)
F2 0.086(6) 0.107(7) 0.150(9) -0.003(6) -0.012(6) -0.031(5)
F3 0.269(14) 0.123(8) 0.077(6) -0.042(5) 0.053(8) -0.087(9)
F4 0.208(11) 0.147(8) 0.068(5) -0.054(5) -0.017(7) 0.071(8)
F5 0.226(11) 0.041(4) 0.136(8) -0.009(4) 0.096(8) -0.005(6)
F6 0.125(7) 0.046(4) 0.143(8) -0.031(4) -0.012(6) -0.017(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100842.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100842.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100842
loop_
_publ_author_name
'Major, Quinn'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
Substituents Effects in POP Pincer Complexes of Ruthenium
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2492
_journal_page_last 2501
_journal_paper_doi 10.1021/om050053v
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C20 H44 Cl N2 O P2 Ru, C24 H20 B, C H2 Cl2'
_chemical_formula_sum 'C45 H66 B Cl3 N2 O P2 Ru'
_chemical_formula_weight 931.17
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 79.4740(15)
_cell_angle_beta 87.0280(14)
_cell_angle_gamma 73.8070(13)
_cell_formula_units_Z 2
_cell_length_a 11.8290(3)
_cell_length_b 13.4628(4)
_cell_length_c 15.2504(3)
_cell_measurement_reflns_used 20707
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.6
_cell_volume 2293.05(10)
_diffrn_ambient_temperature 150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0689
_diffrn_reflns_av_sigmaI/netI 0.0966
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 22136
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 2.71
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.622
_exptl_absorpt_correction_T_max 0.943
_exptl_absorpt_correction_T_min 0.737
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour plate
_exptl_crystal_density_diffrn 1.349
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description lilac
_exptl_crystal_F_000 976
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.08
_refine_ls_extinction_coef none
_refine_ls_extinction_expression ?
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 497
_refine_ls_number_reflns 10364
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.046
_refine_ls_R_factor_all 0.1021
_refine_ls_R_factor_gt 0.0559
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+2.0371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1234
_refine_ls_wR_factor_ref 0.1488
_reflns_number_gt 6953
_reflns_number_total 10364
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100842
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.26211(3) 0.50383(2) 0.66025(2) 0.02209(12) Uani 1 1 d . . .
Cl1 Cl 0.11288(9) 0.44555(8) 0.60967(7) 0.0333(3) Uani 1 1 d . . .
P1 P 0.36583(9) 0.33346(8) 0.74398(7) 0.0230(2) Uani 1 1 d . . .
P2 P 0.15256(9) 0.67952(8) 0.62275(7) 0.0222(2) Uani 1 1 d . . .
O1 O 0.1721(2) 0.5169(2) 0.78309(17) 0.0235(6) Uani 1 1 d . . .
N1 N 0.3422(3) 0.4868(2) 0.5470(2) 0.0227(7) Uani 1 1 d . . .
N2 N 0.3803(4) 0.4745(3) 0.4845(3) 0.0406(10) Uani 1 1 d . . .
C1 C 0.2865(4) 0.3440(3) 0.8509(3) 0.0259(9) Uani 1 1 d . . .
H1A H 0.2817 0.2734 0.8805 0.031 Uiso 1 1 calc R . .
H1B H 0.3310 0.3701 0.8905 0.031 Uiso 1 1 calc R . .
C2 C 0.1644(4) 0.4169(3) 0.8375(3) 0.0293(10) Uani 1 1 d . . .
H2A H 0.1148 0.3853 0.8070 0.035 Uiso 1 1 calc R . .
H2B H 0.1281 0.4291 0.8960 0.035 Uiso 1 1 calc R . .
C3 C 0.0565(4) 0.5950(3) 0.7778(3) 0.0310(10) Uani 1 1 d . . .
H3A H 0.0253 0.6023 0.8384 0.037 Uiso 1 1 calc R . .
H3B H 0.0002 0.5726 0.7454 0.037 Uiso 1 1 calc R . .
C4 C 0.0723(4) 0.6984(3) 0.7289(3) 0.0278(9) Uani 1 1 d . . .
H4A H 0.1170 0.7267 0.7667 0.033 Uiso 1 1 calc R . .
H4B H -0.0057 0.7498 0.7162 0.033 Uiso 1 1 calc R . .
C5 C 0.3494(4) 0.2115(3) 0.7072(3) 0.0303(10) Uani 1 1 d . . .
C6 C 0.4346(5) 0.1085(4) 0.7531(3) 0.0475(13) Uani 1 1 d . . .
H6A H 0.4204 0.0492 0.7309 0.071 Uiso 1 1 calc R . .
H6B H 0.4218 0.1000 0.8177 0.071 Uiso 1 1 calc R . .
H6C H 0.5159 0.1107 0.7398 0.071 Uiso 1 1 calc R . .
C7 C 0.3718(5) 0.2222(4) 0.6065(3) 0.0389(11) Uani 1 1 d . . .
H7A H 0.3634 0.1599 0.5858 0.058 Uiso 1 1 calc R . .
H7B H 0.4517 0.2288 0.5936 0.058 Uiso 1 1 calc R . .
H7C H 0.3147 0.2849 0.5755 0.058 Uiso 1 1 calc R . .
C8 C 0.2243(5) 0.2021(4) 0.7273(3) 0.0423(12) Uani 1 1 d . . .
H8A H 0.2159 0.1388 0.7082 0.063 Uiso 1 1 calc R . .
H8B H 0.1676 0.2641 0.6951 0.063 Uiso 1 1 calc R . .
H8C H 0.2092 0.1973 0.7915 0.063 Uiso 1 1 calc R . .
C9 C 0.5221(4) 0.3147(3) 0.7781(3) 0.0321(10) Uani 1 1 d . . .
C10 C 0.5319(4) 0.4200(4) 0.7979(3) 0.0407(11) Uani 1 1 d . . .
H10A H 0.6126 0.4123 0.8160 0.061 Uiso 1 1 calc R . .
H10B H 0.4774 0.4410 0.8461 0.061 Uiso 1 1 calc R . .
H10C H 0.5119 0.4739 0.7441 0.061 Uiso 1 1 calc R . .
C11 C 0.6077(4) 0.2879(4) 0.7013(3) 0.0389(11) Uani 1 1 d . . .
H11A H 0.6883 0.2785 0.7206 0.058 Uiso 1 1 calc R . .
H11B H 0.5878 0.3453 0.6500 0.058 Uiso 1 1 calc R . .
H11C H 0.6015 0.2229 0.6843 0.058 Uiso 1 1 calc R . .
C12 C 0.5610(4) 0.2321(4) 0.8636(3) 0.0390(11) Uani 1 1 d . . .
H12A H 0.6428 0.2266 0.8775 0.059 Uiso 1 1 calc R . .
H12B H 0.5549 0.1638 0.8541 0.059 Uiso 1 1 calc R . .
H12C H 0.5100 0.2538 0.9134 0.059 Uiso 1 1 calc R . .
C13 C 0.0466(4) 0.7424(3) 0.5292(3) 0.0301(10) Uani 1 1 d . . .
C14 C -0.0695(4) 0.7130(4) 0.5536(3) 0.0351(10) Uani 1 1 d . . .
H14A H -0.1262 0.7454 0.5050 0.053 Uiso 1 1 calc R . .
H14B H -0.1015 0.7384 0.6084 0.053 Uiso 1 1 calc R . .
H14C H -0.0544 0.6364 0.5628 0.053 Uiso 1 1 calc R . .
C15 C 0.0206(4) 0.8629(3) 0.5121(3) 0.0380(11) Uani 1 1 d . . .
H15A H -0.0352 0.8931 0.4625 0.057 Uiso 1 1 calc R . .
H15B H 0.0939 0.8826 0.4969 0.057 Uiso 1 1 calc R . .
H15C H -0.0136 0.8899 0.5659 0.057 Uiso 1 1 calc R . .
C16 C 0.0982(4) 0.6969(4) 0.4458(3) 0.0369(11) Uani 1 1 d . . .
H16A H 0.0439 0.7289 0.3956 0.055 Uiso 1 1 calc R . .
H16B H 0.1097 0.6207 0.4575 0.055 Uiso 1 1 calc R . .
H16C H 0.1741 0.7120 0.4311 0.055 Uiso 1 1 calc R . .
C17 C 0.2750(4) 0.7412(3) 0.6259(3) 0.0274(9) Uani 1 1 d . . .
C18 C 0.2450(4) 0.8478(3) 0.6555(3) 0.0324(10) Uani 1 1 d . . .
H18A H 0.3163 0.8715 0.6543 0.049 Uiso 1 1 calc R . .
H18B H 0.2132 0.8415 0.7163 0.049 Uiso 1 1 calc R . .
H18C H 0.1862 0.8989 0.6151 0.049 Uiso 1 1 calc R . .
C19 C 0.3560(4) 0.6563(3) 0.6967(3) 0.0312(10) Uani 1 1 d . . .
H19A H 0.4263 0.6781 0.7060 0.047 Uiso 1 1 calc R . .
H19B H 0.3796 0.5890 0.6754 0.047 Uiso 1 1 calc R . .
H19C H 0.3132 0.6485 0.7531 0.047 Uiso 1 1 calc R . .
C20 C 0.3414(4) 0.7477(3) 0.5368(3) 0.0312(10) Uani 1 1 d . . .
H20A H 0.4049 0.7804 0.5409 0.047 Uiso 1 1 calc R . .
H20B H 0.2869 0.7900 0.4892 0.047 Uiso 1 1 calc R . .
H20C H 0.3749 0.6768 0.5236 0.047 Uiso 1 1 calc R . .
C21 C 0.6572(3) 0.8290(3) 0.7464(2) 0.0227(8) Uani 1 1 d . . .
C22 C 0.7375(4) 0.8895(3) 0.7280(3) 0.0265(9) Uani 1 1 d . . .
H22A H 0.7928 0.8844 0.7728 0.032 Uiso 1 1 calc R . .
C23 C 0.7403(4) 0.9562(3) 0.6477(3) 0.0327(10) Uani 1 1 d . . .
H23A H 0.7954 0.9967 0.6391 0.039 Uiso 1 1 calc R . .
C24 C 0.6632(4) 0.9639(3) 0.5801(3) 0.0337(10) Uani 1 1 d . . .
H24A H 0.6654 1.0087 0.5245 0.040 Uiso 1 1 calc R . .
C25 C 0.5831(4) 0.9054(3) 0.5949(3) 0.0328(10) Uani 1 1 d . . .
H25A H 0.5293 0.9097 0.5493 0.039 Uiso 1 1 calc R . .
C26 C 0.5808(4) 0.8400(3) 0.6765(3) 0.0290(10) Uani 1 1 d . . .
H26A H 0.5243 0.8009 0.6851 0.035 Uiso 1 1 calc R . .
C31 C 0.7358(4) 0.6273(3) 0.8266(3) 0.0259(9) Uani 1 1 d . . .
C32 C 0.7834(4) 0.5478(3) 0.8987(3) 0.0327(10) Uani 1 1 d . . .
H32A H 0.7741 0.5638 0.9573 0.039 Uiso 1 1 calc R . .
C33 C 0.8438(4) 0.4461(4) 0.8872(4) 0.0432(13) Uani 1 1 d . . .
H33A H 0.8756 0.3947 0.9376 0.052 Uiso 1 1 calc R . .
C34 C 0.8576(4) 0.4198(4) 0.8041(4) 0.0453(13) Uani 1 1 d . . .
H34A H 0.8980 0.3502 0.7967 0.054 Uiso 1 1 calc R . .
C35 C 0.8123(4) 0.4952(4) 0.7311(3) 0.0399(12) Uani 1 1 d . . .
H35A H 0.8219 0.4780 0.6729 0.048 Uiso 1 1 calc R . .
C36 C 0.7524(4) 0.5969(3) 0.7432(3) 0.0303(10) Uani 1 1 d . . .
H36A H 0.7214 0.6477 0.6922 0.036 Uiso 1 1 calc R . .
C41 C 0.5232(4) 0.7411(3) 0.8702(2) 0.0235(9) Uani 1 1 d . . .
C42 C 0.4260(4) 0.8308(3) 0.8584(3) 0.0266(9) Uani 1 1 d . . .
H42A H 0.4385 0.8957 0.8297 0.032 Uiso 1 1 calc R . .
C43 C 0.3131(4) 0.8295(3) 0.8866(3) 0.0314(10) Uani 1 1 d . . .
H43A H 0.2509 0.8927 0.8770 0.038 Uiso 1 1 calc R . .
C44 C 0.2901(4) 0.7369(4) 0.9285(3) 0.0327(10) Uani 1 1 d . . .
H44A H 0.2128 0.7356 0.9480 0.039 Uiso 1 1 calc R . .
C45 C 0.3822(4) 0.6466(3) 0.9411(3) 0.0319(10) Uani 1 1 d . . .
H45A H 0.3684 0.5822 0.9698 0.038 Uiso 1 1 calc R . .
C46 C 0.4957(4) 0.6485(3) 0.9122(3) 0.0255(9) Uani 1 1 d . . .
H46A H 0.5569 0.5847 0.9213 0.031 Uiso 1 1 calc R . .
C51 C 0.7149(4) 0.7906(3) 0.9160(2) 0.0242(9) Uani 1 1 d . . .
C52 C 0.6504(4) 0.8782(3) 0.9522(3) 0.0263(9) Uani 1 1 d . . .
H52A H 0.5686 0.9044 0.9392 0.032 Uiso 1 1 calc R . .
C53 C 0.6984(4) 0.9288(3) 1.0058(3) 0.0289(9) Uani 1 1 d . . .
H53A H 0.6504 0.9888 1.0272 0.035 Uiso 1 1 calc R . .
C54 C 0.8162(4) 0.8916(3) 1.0281(3) 0.0323(10) Uani 1 1 d . . .
H54A H 0.8500 0.9252 1.0652 0.039 Uiso 1 1 calc R . .
C55 C 0.8843(4) 0.8045(3) 0.9953(3) 0.0310(10) Uani 1 1 d . . .
H55A H 0.9653 0.7776 1.0104 0.037 Uiso 1 1 calc R . .
C56 C 0.8342(4) 0.7560(3) 0.9401(3) 0.0273(9) Uani 1 1 d . . .
H56A H 0.8831 0.6970 0.9179 0.033 Uiso 1 1 calc R . .
B1 B 0.6588(4) 0.7454(3) 0.8407(3) 0.0218(9) Uani 1 1 d . . .
Cl2 Cl 0.99426(16) 1.0108(2) 0.75849(14) 0.1024(7) Uani 1 1 d . . .
Cl3 Cl 0.89029(14) 1.13028(13) 0.89702(13) 0.0758(5) Uani 1 1 d . . .
C1S C 0.8772(5) 1.0435(4) 0.8298(4) 0.0566(15) Uani 1 1 d . . .
H1SA H 0.8685 0.9784 0.8684 0.068 Uiso 1 1 calc R . .
H1SB H 0.8044 1.0750 0.7940 0.068 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.02270(19) 0.02109(19) 0.02372(18) -0.00695(13) 0.00462(13) -0.00690(14)
Cl1 0.0294(6) 0.0316(6) 0.0426(6) -0.0108(5) -0.0027(5) -0.0111(5)
P1 0.0217(6) 0.0215(5) 0.0242(5) -0.0058(4) 0.0022(4) -0.0027(4)
P2 0.0210(5) 0.0213(5) 0.0255(5) -0.0068(4) 0.0016(4) -0.0061(4)
O1 0.0195(14) 0.0226(14) 0.0277(14) -0.0063(11) 0.0066(11) -0.0045(12)
N1 0.0271(19) 0.0196(17) 0.0235(18) -0.0049(14) 0.0002(15) -0.0090(15)
N2 0.039(2) 0.033(2) 0.048(3) -0.0076(19) 0.008(2) -0.0084(19)
C1 0.023(2) 0.029(2) 0.024(2) -0.0074(17) 0.0023(16) -0.0033(18)
C2 0.030(2) 0.029(2) 0.027(2) -0.0025(18) 0.0083(18) -0.0097(19)
C3 0.021(2) 0.028(2) 0.041(2) -0.0093(19) 0.0073(18) -0.0009(18)
C4 0.028(2) 0.027(2) 0.026(2) -0.0066(17) 0.0048(18) -0.0040(19)
C5 0.040(3) 0.022(2) 0.029(2) -0.0049(17) 0.0050(19) -0.009(2)
C6 0.072(4) 0.026(2) 0.041(3) -0.005(2) 0.000(3) -0.007(2)
C7 0.052(3) 0.035(3) 0.033(2) -0.016(2) 0.002(2) -0.012(2)
C8 0.060(3) 0.034(3) 0.041(3) -0.008(2) 0.006(2) -0.025(3)
C9 0.025(2) 0.036(2) 0.030(2) -0.0062(19) 0.0011(18) 0.001(2)
C10 0.028(3) 0.042(3) 0.049(3) -0.009(2) -0.007(2) -0.005(2)
C11 0.028(3) 0.042(3) 0.040(3) -0.006(2) 0.004(2) -0.001(2)
C12 0.035(3) 0.043(3) 0.033(2) -0.007(2) -0.002(2) 0.000(2)
C13 0.028(2) 0.027(2) 0.033(2) -0.0032(18) -0.0072(18) -0.0053(19)
C14 0.028(2) 0.034(3) 0.044(3) -0.012(2) -0.005(2) -0.005(2)
C15 0.036(3) 0.030(2) 0.044(3) -0.004(2) -0.007(2) -0.003(2)
C16 0.034(3) 0.043(3) 0.032(2) -0.007(2) -0.005(2) -0.006(2)
C17 0.028(2) 0.024(2) 0.034(2) -0.0076(18) 0.0027(18) -0.0112(19)
C18 0.031(2) 0.029(2) 0.041(2) -0.0118(19) -0.001(2) -0.010(2)
C19 0.031(2) 0.023(2) 0.039(2) -0.0059(18) -0.0065(19) -0.0057(19)
C20 0.033(2) 0.026(2) 0.037(2) -0.0054(19) 0.0045(19) -0.013(2)
C21 0.022(2) 0.022(2) 0.0241(19) -0.0076(16) 0.0010(16) -0.0042(17)
C22 0.030(2) 0.026(2) 0.026(2) -0.0075(17) -0.0006(17) -0.0092(19)
C23 0.031(3) 0.029(2) 0.039(2) -0.0023(19) 0.003(2) -0.013(2)
C24 0.042(3) 0.026(2) 0.028(2) 0.0026(18) 0.001(2) -0.007(2)
C25 0.036(3) 0.032(2) 0.028(2) -0.0011(19) -0.0046(19) -0.009(2)
C26 0.034(3) 0.028(2) 0.029(2) -0.0061(18) -0.0003(18) -0.014(2)
C31 0.020(2) 0.024(2) 0.035(2) -0.0071(18) 0.0046(17) -0.0077(18)
C32 0.027(2) 0.025(2) 0.042(3) -0.0024(19) 0.0060(19) -0.0029(19)
C33 0.026(3) 0.024(2) 0.073(4) 0.001(2) 0.005(2) -0.003(2)
C34 0.029(3) 0.024(2) 0.087(4) -0.024(3) 0.014(3) -0.006(2)
C35 0.034(3) 0.038(3) 0.058(3) -0.026(2) 0.015(2) -0.017(2)
C36 0.026(2) 0.029(2) 0.040(2) -0.0136(19) 0.0049(19) -0.0111(19)
C41 0.028(2) 0.020(2) 0.0226(19) -0.0068(16) -0.0015(17) -0.0053(18)
C42 0.030(2) 0.024(2) 0.027(2) -0.0046(17) 0.0004(18) -0.0088(19)
C43 0.026(2) 0.033(2) 0.035(2) -0.0097(19) -0.0024(18) -0.005(2)
C44 0.028(2) 0.042(3) 0.034(2) -0.015(2) 0.0071(19) -0.014(2)
C45 0.036(3) 0.029(2) 0.033(2) -0.0019(18) 0.0036(19) -0.015(2)
C46 0.031(2) 0.021(2) 0.025(2) -0.0028(16) -0.0025(17) -0.0090(18)
C51 0.025(2) 0.025(2) 0.0205(19) -0.0031(16) -0.0015(16) -0.0048(18)
C52 0.025(2) 0.024(2) 0.028(2) -0.0064(17) -0.0003(17) -0.0024(18)
C53 0.033(3) 0.025(2) 0.030(2) -0.0102(17) 0.0022(18) -0.0067(19)
C54 0.038(3) 0.034(2) 0.029(2) -0.0119(19) 0.0028(19) -0.016(2)
C55 0.020(2) 0.038(3) 0.035(2) -0.009(2) -0.0029(18) -0.0053(19)
C56 0.026(2) 0.027(2) 0.026(2) -0.0088(17) 0.0048(17) -0.0020(18)
B1 0.022(2) 0.019(2) 0.025(2) -0.0061(18) 0.0003(18) -0.0042(19)
Cl2 0.0539(11) 0.175(2) 0.1008(14) -0.0765(15) 0.0295(10) -0.0388(13)
Cl3 0.0481(9) 0.0665(10) 0.1279(15) -0.0590(10) -0.0111(9) -0.0111(8)
C1S 0.057(4) 0.049(3) 0.074(4) -0.027(3) 0.016(3) -0.025(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100843.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100843.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100843
loop_
_publ_author_name
'Major, Quinn'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
Substituents Effects in POP Pincer Complexes of Ruthenium
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2492
_journal_page_last 2501
_journal_paper_doi 10.1021/om050053v
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C16 H38 Cl2 O P2 Ru'
_chemical_formula_sum 'C16 H38 Cl2 O P2 Ru'
_chemical_formula_weight 480.37
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 109.7360(14)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.7468(4)
_cell_length_b 16.5738(4)
_cell_length_c 12.9615(5)
_cell_measurement_reflns_used 25511
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.6
_cell_volume 2173.03(13)
_diffrn_ambient_temperature 150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0703
_diffrn_reflns_av_sigmaI/netI 0.0699
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 18568
_diffrn_reflns_theta_max 27.47
_diffrn_reflns_theta_min 2.97
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.115
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.883
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.468
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1000
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.04
_refine_ls_extinction_coef ?
_refine_ls_extinction_expression ?
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 214
_refine_ls_number_reflns 4953
_refine_ls_number_restraints 11
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.0741
_refine_ls_R_factor_gt 0.0403
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0812
_refine_ls_wR_factor_ref 0.0944
_reflns_number_gt 3540
_reflns_number_total 4953
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100843
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.53880(3) 0.068803(15) 0.75439(2) 0.01728(10) Uani 1 1 d D . .
H1RU H 0.531(3) 0.0145(13) 0.6431(16) 0.026 Uiso 1 1 d D . .
H2RU H 0.610(3) 0.0391(15) 0.6650(19) 0.026 Uiso 1 1 d D . .
Cl1 Cl 0.43948(9) 0.18269(5) 0.64093(8) 0.0283(2) Uani 1 1 d D . .
Cl2 Cl 0.63537(9) -0.04182(5) 0.87532(7) 0.0235(2) Uani 1 1 d D . .
P1 P 0.33161(9) 0.00734(5) 0.72007(8) 0.0206(2) Uani 1 1 d D . .
P2 P 0.73679(9) 0.14074(5) 0.83612(7) 0.0192(2) Uani 1 1 d D . .
O1 O 0.4901(2) 0.12153(13) 0.88896(19) 0.0199(5) Uani 1 1 d . . .
C1 C 0.2911(4) 0.0452(2) 0.8383(3) 0.0233(8) Uani 1 1 d . . .
H1A H 0.1939 0.0481 0.8190 0.028 Uiso 1 1 calc R . .
H1B H 0.3256 0.0072 0.9004 0.028 Uiso 1 1 calc R . .
C2 C 0.3503(4) 0.1281(2) 0.8726(3) 0.0248(8) Uani 1 1 d . . .
H2A H 0.3082 0.1683 0.8149 0.030 Uiso 1 1 calc R . .
H2B H 0.3369 0.1451 0.9413 0.030 Uiso 1 1 calc R . .
C3 C 0.5634(4) 0.19372(19) 0.9373(3) 0.0239(8) Uani 1 1 d . . .
H3A H 0.5475 0.2075 1.0062 0.029 Uiso 1 1 calc R . .
H3B H 0.5348 0.2398 0.8861 0.029 Uiso 1 1 calc R . .
C4 C 0.7071(4) 0.1764(2) 0.9601(3) 0.0233(8) Uani 1 1 d . . .
H4A H 0.7371 0.1349 1.0181 0.028 Uiso 1 1 calc R . .
H4B H 0.7591 0.2261 0.9871 0.028 Uiso 1 1 calc R . .
C5 C 0.3246(4) -0.1030(2) 0.7404(3) 0.0243(8) Uani 1 1 d . . .
H5A H 0.3871 -0.1140 0.8160 0.029 Uiso 1 1 calc R . .
C6 C 0.3762(5) -0.1524(2) 0.6631(4) 0.0427(11) Uani 1 1 d . . .
H6A H 0.3870 -0.2088 0.6870 0.064 Uiso 1 1 calc R . .
H6B H 0.4617 -0.1307 0.6648 0.064 Uiso 1 1 calc R . .
H6C H 0.3130 -0.1491 0.5883 0.064 Uiso 1 1 calc R . .
C7 C 0.1906(4) -0.1338(2) 0.7389(3) 0.0338(10) Uani 1 1 d . . .
H7A H 0.2006 -0.1881 0.7707 0.051 Uiso 1 1 calc R . .
H7B H 0.1296 -0.1356 0.6631 0.051 Uiso 1 1 calc R . .
H7C H 0.1554 -0.0974 0.7820 0.051 Uiso 1 1 calc R . .
C8 C 0.1859(4) 0.0293(2) 0.5969(3) 0.0329(10) Uani 1 1 d . . .
H8A H 0.1178 -0.0127 0.5933 0.039 Uiso 1 1 calc R . .
C9 C 0.2229(5) 0.0204(3) 0.4927(3) 0.0431(12) Uani 1 1 d . . .
H9A H 0.1437 0.0277 0.4279 0.065 Uiso 1 1 calc R . .
H9B H 0.2595 -0.0336 0.4909 0.065 Uiso 1 1 calc R . .
H9C H 0.2888 0.0612 0.4928 0.065 Uiso 1 1 calc R . .
C10 C 0.1216(4) 0.1119(2) 0.5988(4) 0.0396(11) Uani 1 1 d . . .
H10A H 0.0427 0.1175 0.5335 0.059 Uiso 1 1 calc R . .
H10B H 0.1846 0.1548 0.5996 0.059 Uiso 1 1 calc R . .
H10C H 0.0965 0.1160 0.6647 0.059 Uiso 1 1 calc R . .
C11 C 0.7872(4) 0.2307(2) 0.7742(3) 0.0251(8) Uani 1 1 d . . .
H11A H 0.8823 0.2414 0.8168 0.030 Uiso 1 1 calc R . .
C12 C 0.7096(4) 0.3078(2) 0.7802(3) 0.0338(10) Uani 1 1 d . . .
H12A H 0.7389 0.3523 0.7442 0.051 Uiso 1 1 calc R . .
H12B H 0.7257 0.3216 0.8571 0.051 Uiso 1 1 calc R . .
H12C H 0.6149 0.2984 0.7431 0.051 Uiso 1 1 calc R . .
C13 C 0.7776(4) 0.2142(2) 0.6554(3) 0.0349(10) Uani 1 1 d . . .
H13A H 0.8089 0.2616 0.6260 0.052 Uiso 1 1 calc R . .
H13B H 0.6855 0.2032 0.6111 0.052 Uiso 1 1 calc R . .
H13C H 0.8324 0.1675 0.6532 0.052 Uiso 1 1 calc R . .
C14 C 0.8907(4) 0.0820(2) 0.8962(3) 0.0235(8) Uani 1 1 d . . .
H14A H 0.8739 0.0448 0.9508 0.028 Uiso 1 1 calc R . .
C15 C 0.9207(4) 0.0277(2) 0.8122(3) 0.0301(9) Uani 1 1 d . . .
H15A H 0.9961 -0.0071 0.8496 0.045 Uiso 1 1 calc R . .
H15B H 0.9418 0.0611 0.7580 0.045 Uiso 1 1 calc R . .
H15C H 0.8432 -0.0057 0.7752 0.045 Uiso 1 1 calc R . .
C16 C 1.0121(4) 0.1328(2) 0.9610(3) 0.0333(10) Uani 1 1 d . . .
H16A H 1.0842 0.0969 1.0022 0.050 Uiso 1 1 calc R . .
H16B H 0.9887 0.1684 1.0121 0.050 Uiso 1 1 calc R . .
H16C H 1.0406 0.1655 0.9100 0.050 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01816(17) 0.01558(15) 0.01728(16) -0.00012(10) 0.00488(12) -0.00021(11)
Cl1 0.0242(5) 0.0233(5) 0.0324(5) 0.0093(4) 0.0031(4) 0.0012(4)
Cl2 0.0229(5) 0.0194(4) 0.0258(5) 0.0039(3) 0.0052(4) 0.0019(3)
P1 0.0195(5) 0.0189(5) 0.0216(5) 0.0005(3) 0.0046(4) -0.0028(4)
P2 0.0170(5) 0.0173(4) 0.0214(5) 0.0004(3) 0.0039(4) -0.0015(3)
O1 0.0194(13) 0.0177(12) 0.0235(14) -0.0034(9) 0.0083(11) 0.0014(9)
C1 0.018(2) 0.0244(18) 0.028(2) 0.0029(14) 0.0084(17) -0.0001(14)
C2 0.022(2) 0.0278(19) 0.029(2) -0.0007(15) 0.0138(17) 0.0012(15)
C3 0.025(2) 0.0202(18) 0.026(2) -0.0080(14) 0.0083(17) -0.0030(14)
C4 0.024(2) 0.0245(19) 0.0190(19) -0.0047(14) 0.0041(16) -0.0032(15)
C5 0.025(2) 0.0182(18) 0.027(2) 0.0037(14) 0.0047(17) -0.0010(14)
C6 0.055(3) 0.025(2) 0.055(3) -0.0062(18) 0.028(3) -0.0011(19)
C7 0.035(2) 0.027(2) 0.033(2) 0.0025(16) 0.0037(19) -0.0075(17)
C8 0.026(2) 0.030(2) 0.033(2) 0.0065(16) -0.0020(19) -0.0099(16)
C9 0.054(3) 0.042(3) 0.023(2) 0.0012(18) -0.002(2) -0.006(2)
C10 0.024(2) 0.037(2) 0.050(3) 0.0155(19) 0.002(2) 0.0027(18)
C11 0.023(2) 0.0192(18) 0.033(2) 0.0060(14) 0.0097(17) -0.0016(14)
C12 0.038(3) 0.020(2) 0.042(3) 0.0032(16) 0.011(2) -0.0010(16)
C13 0.041(3) 0.033(2) 0.037(2) 0.0118(17) 0.021(2) 0.0017(18)
C14 0.019(2) 0.0224(18) 0.027(2) 0.0014(14) 0.0049(16) -0.0013(14)
C15 0.026(2) 0.029(2) 0.038(2) -0.0020(16) 0.0138(19) 0.0020(16)
C16 0.022(2) 0.028(2) 0.040(3) -0.0023(17) -0.0021(19) -0.0011(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100844.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100844.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100844
loop_
_publ_author_name
'Major, Quinn'
'Lough, Alan J.'
'Gusev, Dmitry G.'
_publ_section_title
;
Substituents Effects in POP Pincer Complexes of Ruthenium
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2492
_journal_page_last 2501
_journal_paper_doi 10.1021/om050053v
_journal_volume 24
_journal_year 2005
_chemical_absolute_configuration ad
_chemical_formula_moiety 'C16 H36 Cl2 N2 O P2 Ru'
_chemical_formula_sum 'C16 H36 Cl2 N2 O P2 Ru'
_chemical_formula_weight 506.38
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.7245(2)
_cell_length_b 13.8487(4)
_cell_length_c 15.4083(4)
_cell_measurement_reflns_used 25033
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.6
_cell_volume 2288.45(10)
_diffrn_ambient_temperature 150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0540
_diffrn_reflns_av_sigmaI/netI 0.0523
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 18260
_diffrn_reflns_theta_max 27.47
_diffrn_reflns_theta_min 2.64
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.065
_exptl_absorpt_correction_T_max 0.922
_exptl_absorpt_correction_T_min 0.845
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour needle
_exptl_crystal_density_diffrn 1.470
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description orange
_exptl_crystal_F_000 1048
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.08
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.07(4)
_refine_ls_extinction_coef none
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc2^\l3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method ?
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 227
_refine_ls_number_reflns 5220
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.085
_refine_ls_R_factor_all 0.0493
_refine_ls_R_factor_gt 0.0360
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0365P)2^+0.7371P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0751
_refine_ls_wR_factor_ref 0.0815
_reflns_number_gt 4532
_reflns_number_total 5220
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100844
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.51984(2) 0.52530(2) -0.081730(19) 0.01904(9) Uani 1 1 d . A .
Cl1 Cl 0.46227(9) 0.38706(7) -0.16605(6) 0.0301(2) Uani 1 1 d . . .
Cl2 Cl 0.56889(8) 0.66998(7) -0.00059(7) 0.0271(2) Uani 1 1 d . . .
P1 P 0.67327(9) 0.56508(7) -0.18627(7) 0.0235(2) Uani 1 1 d . A .
P2 P 0.32994(9) 0.50818(7) -0.00558(7) 0.0247(2) Uani 1 1 d . . .
O1 O 0.4061(2) 0.6134(2) -0.16463(18) 0.0263(6) Uani 1 1 d . . .
N1 N 0.6194(3) 0.4471(2) -0.0086(2) 0.0223(7) Uani 1 1 d . . .
N2 N 0.6764(4) 0.4010(3) 0.0340(3) 0.0395(9) Uani 1 1 d . A .
C1 C 0.5739(4) 0.6302(3) -0.2643(3) 0.0350(10) Uani 1 1 d . . .
H1A H 0.6251 0.6765 -0.2978 0.042 Uiso 1 1 calc R A .
H1B H 0.5362 0.5838 -0.3055 0.042 Uiso 1 1 calc R . .
C2 C 0.4726(4) 0.6837(3) -0.2166(3) 0.0329(9) Uani 1 1 d . A .
H2A H 0.5093 0.7342 -0.1789 0.039 Uiso 1 1 calc R . .
H2B H 0.4152 0.7150 -0.2583 0.039 Uiso 1 1 calc R . .
C3 C 0.2954(4) 0.6544(3) -0.1234(3) 0.0377(11) Uani 1 1 d . A .
H3A H 0.2419 0.6862 -0.1673 0.045 Uiso 1 1 calc R . .
H3B H 0.3198 0.7030 -0.0795 0.045 Uiso 1 1 calc R . .
C4 C 0.2269(3) 0.5732(3) -0.0813(3) 0.0369(10) Uani 1 1 d . A .
H4A H 0.1962 0.5280 -0.1264 0.044 Uiso 1 1 calc R . .
H4B H 0.1538 0.5987 -0.0495 0.044 Uiso 1 1 calc R . .
C5 C 0.7592(4) 0.4738(3) -0.2507(3) 0.0330(9) Uani 1 1 d . . .
H5A H 0.8371 0.5054 -0.2723 0.040 Uiso 1 1 calc R A .
C6 C 0.6894(5) 0.4353(3) -0.3301(3) 0.0426(11) Uani 1 1 d . A .
H6A H 0.7414 0.3877 -0.3601 0.064 Uiso 1 1 calc R . .
H6B H 0.6707 0.4889 -0.3696 0.064 Uiso 1 1 calc R . .
H6C H 0.6114 0.4048 -0.3114 0.064 Uiso 1 1 calc R . .
C7 C 0.7991(4) 0.3895(3) -0.1927(3) 0.0392(11) Uani 1 1 d . A .
H7A H 0.8441 0.3416 -0.2276 0.059 Uiso 1 1 calc R . .
H7B H 0.7251 0.3595 -0.1670 0.059 Uiso 1 1 calc R . .
H7C H 0.8537 0.4134 -0.1465 0.059 Uiso 1 1 calc R . .
C8 C 0.7943(4) 0.6537(3) -0.1535(3) 0.0354(11) Uani 1 1 d . . .
H8A H 0.7486 0.7089 -0.1263 0.042 Uiso 1 1 calc R A .
C9 C 0.8767(4) 0.6112(4) -0.0824(4) 0.0512(13) Uani 1 1 d . A .
H9A H 0.9400 0.6587 -0.0656 0.077 Uiso 1 1 calc R . .
H9B H 0.9177 0.5528 -0.1041 0.077 Uiso 1 1 calc R . .
H9C H 0.8253 0.5949 -0.0319 0.077 Uiso 1 1 calc R . .
C10 C 0.8697(6) 0.6967(4) -0.2283(4) 0.0662(19) Uani 1 1 d . A .
H10A H 0.9311 0.7424 -0.2052 0.099 Uiso 1 1 calc R . .
H10B H 0.8134 0.7305 -0.2681 0.099 Uiso 1 1 calc R . .
H10C H 0.9128 0.6449 -0.2594 0.099 Uiso 1 1 calc R . .
C11 C 0.3128(4) 0.5736(3) 0.0976(3) 0.0324(10) Uani 1 1 d . A .
H11A H 0.3433 0.6407 0.0861 0.039 Uiso 1 1 calc R . .
C12 C 0.3993(5) 0.5327(4) 0.1668(3) 0.0561(14) Uani 1 1 d . . .
H12A H 0.3892 0.5694 0.2208 0.084 Uiso 1 1 calc R A .
H12B H 0.4859 0.5375 0.1470 0.084 Uiso 1 1 calc R . .
H12C H 0.3784 0.4648 0.1773 0.084 Uiso 1 1 calc R . .
C13 C 0.1800(5) 0.5848(4) 0.1310(4) 0.0601(16) Uani 1 1 d . . .
H13A H 0.1809 0.6206 0.1859 0.090 Uiso 1 1 calc R A .
H13B H 0.1434 0.5208 0.1405 0.090 Uiso 1 1 calc R . .
H13C H 0.1302 0.6201 0.0882 0.090 Uiso 1 1 calc R . .
C14 C 0.2605(4) 0.3869(4) 0.0054(4) 0.0535(15) Uani 1 1 d D A 1
H14 H 0.2118 0.4020 0.0590 0.064 Uiso 1 1 calc R A 1
C15 C 0.3447(6) 0.3159(4) 0.0473(4) 0.0611(16) Uani 1 1 d . A 1
H15A H 0.4097 0.3501 0.0797 0.092 Uiso 1 1 calc R A 1
H15B H 0.3834 0.2752 0.0028 0.092 Uiso 1 1 calc R A 1
H15C H 0.2965 0.2753 0.0873 0.092 Uiso 1 1 calc R A 1
C16 C 0.1527(12) 0.3588(10) -0.0467(10) 0.088(5) Uani 0.50 1 d PD A 1
H16A H 0.1277 0.2929 -0.0315 0.131 Uiso 0.50 1 calc PR A 1
H16B H 0.1746 0.3615 -0.1084 0.131 Uiso 0.50 1 calc PR A 1
H16C H 0.0835 0.4032 -0.0352 0.131 Uiso 0.50 1 calc PR A 1
C14A C 0.2605(4) 0.3869(4) 0.0054(4) 0.0535(15) Uani 0.00 1 d PD A 2
H14A H 0.2662 0.3645 -0.0562 0.064 Uiso 0.00 1 calc PR A 2
C15A C 0.3447(6) 0.3159(4) 0.0473(4) 0.0611(16) Uani 0.00 1 d P A 2
H15D H 0.4313 0.3309 0.0324 0.092 Uiso 0.00 1 calc PR A 2
H15E H 0.3241 0.2507 0.0269 0.092 Uiso 0.00 1 calc PR A 2
H15F H 0.3341 0.3190 0.1105 0.092 Uiso 0.00 1 calc PR A 2
C16A C 0.1260(8) 0.3790(10) 0.0188(11) 0.070(4) Uani 0.50 1 d PD A 2
H16D H 0.1030 0.3108 0.0245 0.105 Uiso 0.50 1 calc PR A 2
H16E H 0.0821 0.4071 -0.0310 0.105 Uiso 0.50 1 calc PR A 2
H16F H 0.1026 0.4137 0.0717 0.105 Uiso 0.50 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01879(13) 0.01659(14) 0.02173(15) -0.00004(13) -0.00071(11) 0.00046(11)
Cl1 0.0355(5) 0.0268(5) 0.0279(5) -0.0063(4) 0.0007(4) -0.0074(4)
Cl2 0.0265(4) 0.0213(5) 0.0335(5) -0.0063(4) 0.0019(4) -0.0008(4)
P1 0.0242(5) 0.0188(5) 0.0275(5) -0.0007(4) 0.0052(4) -0.0013(4)
P2 0.0200(4) 0.0248(5) 0.0294(5) 0.0014(4) 0.0037(4) -0.0006(4)
O1 0.0247(13) 0.0244(14) 0.0298(15) 0.0038(13) -0.0005(11) 0.0016(12)
N1 0.0252(15) 0.0166(16) 0.0249(17) -0.0043(14) 0.0001(14) 0.0013(13)
N2 0.047(2) 0.033(2) 0.038(2) -0.0015(18) -0.0094(18) 0.0057(19)
C1 0.040(2) 0.032(2) 0.032(2) 0.012(2) 0.0062(19) 0.0042(19)
C2 0.038(2) 0.024(2) 0.036(2) 0.0109(17) -0.002(2) 0.0003(19)
C3 0.025(2) 0.040(3) 0.047(3) 0.011(2) -0.0016(19) 0.0139(19)
C4 0.0226(18) 0.044(3) 0.044(2) 0.004(3) 0.001(2) 0.0030(18)
C5 0.033(2) 0.027(2) 0.039(2) -0.004(2) 0.0141(17) -0.003(2)
C6 0.060(3) 0.035(3) 0.032(3) -0.006(2) 0.011(2) -0.006(2)
C7 0.040(2) 0.028(2) 0.049(3) -0.007(2) -0.001(2) 0.0058(19)
C8 0.031(2) 0.024(2) 0.051(3) -0.011(2) 0.011(2) -0.0086(17)
C9 0.033(2) 0.037(3) 0.083(4) -0.017(3) -0.014(3) -0.0040(19)
C10 0.070(4) 0.048(3) 0.081(4) -0.020(3) 0.044(3) -0.035(3)
C11 0.032(2) 0.032(2) 0.033(2) -0.0005(19) 0.0110(17) 0.0031(18)
C12 0.077(4) 0.055(3) 0.037(3) -0.004(3) -0.006(2) 0.014(3)
C13 0.048(3) 0.065(4) 0.067(4) -0.016(3) 0.038(3) -0.005(3)
C14 0.034(2) 0.031(3) 0.095(5) 0.005(3) 0.010(3) -0.012(2)
C15 0.078(4) 0.035(3) 0.070(4) 0.011(3) -0.006(3) -0.016(3)
C16 0.089(10) 0.040(7) 0.134(15) -0.004(8) -0.031(10) -0.022(7)
C14A 0.034(2) 0.031(3) 0.095(5) 0.005(3) 0.010(3) -0.012(2)
C15A 0.078(4) 0.035(3) 0.070(4) 0.011(3) -0.006(3) -0.016(3)
C16A 0.046(6) 0.057(8) 0.107(12) -0.025(8) 0.036(7) -0.031(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100845.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100845.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100845
loop_
_publ_author_name
'Henry, Renee M.'
'Shoemaker, Richard K.'
'Newell, Rachel H.'
'Jacobsen, George M.'
'DuBois, Daniel L.'
'Rakowski DuBois, M.'
_publ_section_title
;
Stereochemical Control of Iron(II) Complexes Containing a Diphosphine
Ligand with a Pendant Nitrogen Base
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2481
_journal_page_last 2491
_journal_paper_doi 10.1021/om050071c
_journal_volume 24
_chemical_formula_sum 'C44 H68 B Fe N3 P4'
_chemical_formula_weight 829.55
_chemical_name_common '[HFe(CH3CN)(PNP)(dmpm)][BPh4]'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 105.7990(10)
_cell_angle_beta 95.9700(10)
_cell_angle_gamma 98.8340(10)
_cell_formula_units_Z 2
_cell_length_a 11.7581(5)
_cell_length_b 12.0235(6)
_cell_length_c 17.3035(8)
_cell_measurement_reflns_used 17440
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 1.79
_cell_volume 2298.40(18)
_diffrn_ambient_temperature 153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0468
_diffrn_reflns_av_sigmaI/netI 0.0876
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 17440
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 1.79
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.500
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.427291
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details
;
absorption correction applied
using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51,
33-38)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.199
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description cubes
_exptl_crystal_F_000 888
_exptl_crystal_size_max 0.97
_exptl_crystal_size_mid 0.49
_exptl_crystal_size_min 0.25
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 493
_refine_ls_number_reflns 10414
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.016
_refine_ls_R_factor_all 0.0658
_refine_ls_R_factor_gt 0.0540
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.7231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1403
_refine_ls_wR_factor_ref 0.1515
_reflns_number_gt 8537
_reflns_number_total 10414
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.27378(2) 0.39035(2) 0.281973(17) 0.02157(10) Uani 1 1 d . . .
P1 P 0.41351(5) 0.31845(5) 0.21882(4) 0.02741(14) Uani 1 1 d . . .
P2 P 0.41923(5) 0.54105(5) 0.30210(4) 0.02876(14) Uani 1 1 d . . .
P3 P 0.16067(5) 0.48048(5) 0.36310(3) 0.02364(13) Uani 1 1 d . . .
P4 P 0.15771(5) 0.22052(5) 0.26548(3) 0.02326(13) Uani 1 1 d . . .
N2 N -0.03370(16) 0.30184(17) 0.32515(12) 0.0293(4) Uani 1 1 d . . .
N1 N 0.19063(15) 0.42361(15) 0.19202(11) 0.0247(4) Uani 1 1 d . . .
N3 N 0.3736(4) -0.1414(5) -0.4787(5) 0.216(4) Uani 1 1 d . . .
B1 B 0.1770(2) 0.2315(2) -0.17683(15) 0.0251(5) Uani 1 1 d . . .
H1 H 0.344(2) 0.367(2) 0.3533(16) 0.030(6) Uiso 1 1 d . . .
C1 C 0.14519(18) 0.45286(18) 0.14075(13) 0.0263(4) Uani 1 1 d . . .
C2 C 0.0888(2) 0.4924(2) 0.07688(14) 0.0331(5) Uani 1 1 d . . .
H2A H 0.0785 0.5736 0.0996 0.046 Uiso 1 1 calc R . .
H2B H 0.0127 0.4414 0.0541 0.046 Uiso 1 1 calc R . .
H2C H 0.1375 0.4889 0.0339 0.046 Uiso 1 1 calc R . .
C3 C 0.4861(2) 0.2036(2) 0.24008(19) 0.0460(6) Uani 1 1 d . . .
H3A H 0.4337 0.1270 0.2176 0.064 Uiso 1 1 calc R . .
H3B H 0.5064 0.2199 0.2990 0.064 Uiso 1 1 calc R . .
H3C H 0.5571 0.2024 0.2150 0.064 Uiso 1 1 calc R . .
C4 C 0.4070(2) 0.2853(3) 0.10943(16) 0.0451(6) Uani 1 1 d . . .
H4A H 0.4859 0.2864 0.0957 0.063 Uiso 1 1 calc R . .
H4B H 0.3726 0.3445 0.0907 0.063 Uiso 1 1 calc R . .
H4C H 0.3590 0.2072 0.0829 0.063 Uiso 1 1 calc R . .
C5 C 0.5254(2) 0.4527(2) 0.26065(17) 0.0386(6) Uani 1 1 d . . .
H5A H 0.5625 0.4794 0.2184 0.054 Uiso 1 1 calc R . .
H5B H 0.5853 0.4464 0.3031 0.054 Uiso 1 1 calc R . .
C6 C 0.4925(2) 0.6387(2) 0.40026(17) 0.0423(6) Uani 1 1 d . . .
H6A H 0.5670 0.6816 0.3937 0.059 Uiso 1 1 calc R . .
H6B H 0.5066 0.5923 0.4376 0.059 Uiso 1 1 calc R . .
H6C H 0.4435 0.6949 0.4224 0.059 Uiso 1 1 calc R . .
C7 C 0.4164(2) 0.6417(3) 0.2404(2) 0.0493(7) Uani 1 1 d . . .
H7A H 0.3631 0.6953 0.2587 0.069 Uiso 1 1 calc R . .
H7B H 0.3896 0.5967 0.1833 0.069 Uiso 1 1 calc R . .
H7C H 0.4949 0.6875 0.2460 0.069 Uiso 1 1 calc R . .
C8 C 0.1692(2) 0.4755(2) 0.46839(13) 0.0331(5) Uani 1 1 d . . .
H8A H 0.1162 0.5245 0.4956 0.046 Uiso 1 1 calc R . .
H8B H 0.1403 0.3934 0.4679 0.046 Uiso 1 1 calc R . .
C9 C 0.2896(2) 0.5171(3) 0.51847(16) 0.0523(8) Uani 1 1 d . . .
H9A H 0.3438 0.4714 0.4912 0.073 Uiso 1 1 calc R . .
H9B H 0.2867 0.5062 0.5724 0.073 Uiso 1 1 calc R . .
H9C H 0.3161 0.6007 0.5242 0.073 Uiso 1 1 calc R . .
C10 C 0.1680(2) 0.63750(19) 0.37084(15) 0.0309(5) Uani 1 1 d . . .
H10A H 0.2490 0.6788 0.3935 0.043 Uiso 1 1 calc R . .
H10B H 0.1525 0.6437 0.3150 0.043 Uiso 1 1 calc R . .
C11 C 0.0873(2) 0.7049(2) 0.42114(18) 0.0436(6) Uani 1 1 d . . .
H11A H 0.0060 0.6696 0.3974 0.061 Uiso 1 1 calc R . .
H11B H 0.1029 0.7873 0.4211 0.061 Uiso 1 1 calc R . .
H11C H 0.1012 0.7010 0.4771 0.061 Uiso 1 1 calc R . .
C12 C 0.00236(18) 0.4260(2) 0.33029(14) 0.0288(5) Uani 1 1 d . . .
H12A H -0.0401 0.4738 0.3692 0.040 Uiso 1 1 calc R . .
H12B H -0.0197 0.4367 0.2764 0.040 Uiso 1 1 calc R . .
C13 C -0.1610(2) 0.2729(2) 0.32118(17) 0.0415(6) Uani 1 1 d . . .
H13A H -0.1995 0.2869 0.2726 0.058 Uiso 1 1 calc R . .
H13B H -0.1840 0.3226 0.3698 0.058 Uiso 1 1 calc R . .
H13C H -0.1841 0.1899 0.3185 0.058 Uiso 1 1 calc R . .
C14 C 0.00029(18) 0.2247(2) 0.25400(14) 0.0278(4) Uani 1 1 d . . .
H14A H -0.0206 0.2518 0.2062 0.039 Uiso 1 1 calc R . .
H14B H -0.0445 0.1440 0.2434 0.039 Uiso 1 1 calc R . .
C15 C 0.1686(2) 0.1477(2) 0.34556(14) 0.0303(5) Uani 1 1 d . . .
H15A H 0.1482 0.1989 0.3954 0.042 Uiso 1 1 calc R . .
H15B H 0.1103 0.0734 0.3285 0.042 Uiso 1 1 calc R . .
C16 C 0.2885(2) 0.1193(3) 0.36618(17) 0.0413(6) Uani 1 1 d . . .
H16A H 0.3093 0.0675 0.3175 0.058 Uiso 1 1 calc R . .
H16B H 0.2865 0.0798 0.4088 0.058 Uiso 1 1 calc R . .
H16C H 0.3467 0.1925 0.3855 0.058 Uiso 1 1 calc R . .
C17 C 0.1543(2) 0.09675(19) 0.17422(14) 0.0302(5) Uani 1 1 d . . .
H17A H 0.2339 0.0795 0.1725 0.042 Uiso 1 1 calc R . .
H17B H 0.1034 0.0261 0.1791 0.042 Uiso 1 1 calc R . .
C18 C 0.1113(2) 0.1182(2) 0.09429(14) 0.0344(5) Uani 1 1 d . . .
H18A H 0.0283 0.1216 0.0911 0.048 Uiso 1 1 calc R . .
H18B H 0.1230 0.0539 0.0488 0.048 Uiso 1 1 calc R . .
H18C H 0.1551 0.1930 0.0916 0.048 Uiso 1 1 calc R . .
C19 C 0.22882(18) 0.3733(2) -0.13491(14) 0.0279(4) Uani 1 1 d . . .
C20 C 0.1780(2) 0.4571(2) -0.16191(15) 0.0337(5) Uani 1 1 d . . .
H20 H 0.1172 0.4299 -0.2071 0.040 Uiso 1 1 calc R . .
C21 C 0.2124(2) 0.5779(2) -0.12567(17) 0.0375(5) Uani 1 1 d . . .
H21 H 0.1757 0.6311 -0.1464 0.045 Uiso 1 1 calc R . .
C22 C 0.3003(2) 0.6203(2) -0.05927(17) 0.0386(6) Uani 1 1 d . . .
H22 H 0.3243 0.7026 -0.0340 0.046 Uiso 1 1 calc R . .
C23 C 0.3528(2) 0.5413(2) -0.03031(16) 0.0383(6) Uani 1 1 d . . .
H23 H 0.4131 0.5693 0.0152 0.046 Uiso 1 1 calc R . .
C24 C 0.3173(2) 0.4206(2) -0.06764(14) 0.0324(5) Uani 1 1 d . . .
H24 H 0.3547 0.3681 -0.0465 0.039 Uiso 1 1 calc R . .
C25 C 0.25137(18) 0.14832(19) -0.13902(13) 0.0271(4) Uani 1 1 d . . .
C26 C 0.3726(2) 0.1611(2) -0.13777(16) 0.0353(5) Uani 1 1 d . . .
H26 H 0.4115 0.2224 -0.1558 0.042 Uiso 1 1 calc R . .
C27 C 0.4380(2) 0.0876(3) -0.11119(18) 0.0433(6) Uani 1 1 d . . .
H27 H 0.5198 0.1004 -0.1108 0.052 Uiso 1 1 calc R . .
C28 C 0.3848(2) -0.0038(2) -0.08531(16) 0.0392(6) Uani 1 1 d . . .
H28 H 0.4292 -0.0542 -0.0673 0.047 Uiso 1 1 calc R . .
C29 C 0.2657(2) -0.0200(2) -0.08636(15) 0.0365(5) Uani 1 1 d . . .
H29 H 0.2275 -0.0825 -0.0691 0.044 Uiso 1 1 calc R . .
C30 C 0.2013(2) 0.0546(2) -0.11262(14) 0.0303(5) Uani 1 1 d . . .
H30 H 0.1195 0.0412 -0.1126 0.036 Uiso 1 1 calc R . .
C31 C 0.17706(18) 0.18809(19) -0.27557(13) 0.0267(4) Uani 1 1 d . . .
C32 C 0.1316(2) 0.0687(2) -0.31675(15) 0.0342(5) Uani 1 1 d . . .
H32 H 0.1086 0.0177 -0.2855 0.041 Uiso 1 1 calc R . .
C33 C 0.1188(2) 0.0217(2) -0.40010(15) 0.0381(5) Uani 1 1 d . . .
H33 H 0.0865 -0.0594 -0.4248 0.046 Uiso 1 1 calc R . .
C34 C 0.1531(2) 0.0931(2) -0.44753(15) 0.0372(5) Uani 1 1 d . . .
H34 H 0.1439 0.0621 -0.5050 0.045 Uiso 1 1 calc R . .
C35 C 0.2012(2) 0.2106(2) -0.40947(15) 0.0356(5) Uani 1 1 d . . .
H35 H 0.2264 0.2604 -0.4411 0.043 Uiso 1 1 calc R . .
C36 C 0.21313(19) 0.2568(2) -0.32513(14) 0.0295(5) Uani 1 1 d . . .
H36 H 0.2469 0.3375 -0.3006 0.035 Uiso 1 1 calc R . .
C37 C 0.04058(18) 0.21374(18) -0.16005(14) 0.0260(4) Uani 1 1 d . . .
C38 C 0.0143(2) 0.22160(19) -0.08152(14) 0.0296(5) Uani 1 1 d . . .
H38 H 0.0763 0.2332 -0.0386 0.035 Uiso 1 1 calc R . .
C39 C -0.0993(2) 0.2130(2) -0.06424(16) 0.0353(5) Uani 1 1 d . . .
H39 H -0.1134 0.2188 -0.0103 0.042 Uiso 1 1 calc R . .
C40 C -0.1921(2) 0.1960(2) -0.12571(18) 0.0387(6) Uani 1 1 d . . .
H40 H -0.2697 0.1895 -0.1144 0.046 Uiso 1 1 calc R . .
C41 C -0.1696(2) 0.1888(2) -0.20328(18) 0.0379(6) Uani 1 1 d . . .
H41 H -0.2322 0.1781 -0.2456 0.046 Uiso 1 1 calc R . .
C42 C -0.05548(19) 0.1972(2) -0.22022(15) 0.0310(5) Uani 1 1 d . . .
H42 H -0.0424 0.1915 -0.2743 0.037 Uiso 1 1 calc R . .
C43 C 0.3986(3) -0.0628(4) -0.4237(3) 0.0965(17) Uani 1 1 d . . .
C44 C 0.4300(3) 0.0367(3) -0.3553(3) 0.0765(12) Uani 1 1 d . . .
H44A H 0.3725 0.0877 -0.3553 0.107 Uiso 1 1 calc R . .
H44B H 0.5070 0.0801 -0.3571 0.107 Uiso 1 1 calc R . .
H44C H 0.4325 0.0119 -0.3058 0.107 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.02110(16) 0.02084(17) 0.02293(17) 0.00580(12) 0.00379(11) 0.00531(12)
P1 0.0248(3) 0.0277(3) 0.0300(3) 0.0064(2) 0.0082(2) 0.0067(2)
P2 0.0225(3) 0.0248(3) 0.0371(3) 0.0072(2) 0.0034(2) 0.0033(2)
P3 0.0231(3) 0.0235(3) 0.0233(3) 0.0041(2) 0.0029(2) 0.0068(2)
P4 0.0247(3) 0.0214(3) 0.0236(3) 0.0060(2) 0.0048(2) 0.0047(2)
N2 0.0250(9) 0.0298(10) 0.0312(10) 0.0049(8) 0.0083(7) 0.0039(7)
N1 0.0238(8) 0.0223(9) 0.0268(9) 0.0054(7) 0.0048(7) 0.0033(7)
N3 0.075(3) 0.155(5) 0.284(8) -0.150(5) -0.008(4) 0.031(3)
B1 0.0242(11) 0.0258(12) 0.0259(12) 0.0079(9) 0.0055(9) 0.0051(9)
C1 0.0248(10) 0.0238(10) 0.0293(11) 0.0065(9) 0.0044(8) 0.0038(8)
C2 0.0377(12) 0.0312(12) 0.0319(12) 0.0116(10) 0.0003(9) 0.0098(10)
C3 0.0402(14) 0.0435(15) 0.0642(18) 0.0185(14) 0.0211(13) 0.0237(12)
C4 0.0361(13) 0.0628(18) 0.0300(13) 0.0054(12) 0.0123(10) 0.0007(12)
C5 0.0239(11) 0.0363(13) 0.0495(15) 0.0033(11) 0.0072(10) 0.0035(9)
C6 0.0306(12) 0.0354(13) 0.0479(15) -0.0050(11) -0.0014(10) 0.0034(10)
C7 0.0401(14) 0.0464(16) 0.070(2) 0.0340(15) 0.0107(13) 0.0014(12)
C8 0.0414(13) 0.0364(12) 0.0230(11) 0.0070(9) 0.0073(9) 0.0134(10)
C9 0.0463(15) 0.081(2) 0.0282(13) 0.0047(14) 0.0006(11) 0.0304(15)
C10 0.0308(11) 0.0227(10) 0.0381(12) 0.0052(9) 0.0043(9) 0.0088(9)
C11 0.0484(15) 0.0327(13) 0.0508(16) 0.0052(12) 0.0126(12) 0.0199(11)
C12 0.0236(10) 0.0288(11) 0.0321(11) 0.0049(9) 0.0049(8) 0.0065(8)
C13 0.0270(11) 0.0449(15) 0.0496(15) 0.0077(12) 0.0151(10) 0.0022(10)
C14 0.0245(10) 0.0272(11) 0.0305(11) 0.0068(9) 0.0044(8) 0.0036(8)
C15 0.0350(11) 0.0303(11) 0.0300(11) 0.0134(9) 0.0100(9) 0.0083(9)
C16 0.0406(13) 0.0490(15) 0.0464(15) 0.0282(13) 0.0098(11) 0.0163(12)
C17 0.0366(12) 0.0196(10) 0.0318(12) 0.0026(9) 0.0073(9) 0.0047(9)
C18 0.0403(13) 0.0309(12) 0.0270(11) 0.0019(9) 0.0065(9) 0.0033(10)
C19 0.0247(10) 0.0298(11) 0.0295(11) 0.0085(9) 0.0078(8) 0.0034(8)
C20 0.0296(11) 0.0298(12) 0.0392(13) 0.0068(10) 0.0027(9) 0.0055(9)
C21 0.0365(12) 0.0285(12) 0.0496(15) 0.0103(11) 0.0118(11) 0.0110(10)
C22 0.0354(12) 0.0274(12) 0.0476(15) 0.0010(11) 0.0160(11) 0.0016(10)
C23 0.0313(12) 0.0404(14) 0.0356(13) 0.0034(11) 0.0048(10) -0.0015(10)
C24 0.0298(11) 0.0348(12) 0.0307(12) 0.0081(10) 0.0042(9) 0.0033(9)
C25 0.0265(10) 0.0285(11) 0.0258(10) 0.0055(9) 0.0055(8) 0.0072(8)
C26 0.0287(11) 0.0404(13) 0.0407(13) 0.0146(11) 0.0112(10) 0.0094(10)
C27 0.0283(12) 0.0522(16) 0.0512(16) 0.0119(13) 0.0082(11) 0.0176(11)
C28 0.0432(13) 0.0383(14) 0.0378(13) 0.0080(11) 0.0033(10) 0.0204(11)
C29 0.0426(13) 0.0311(12) 0.0387(13) 0.0117(10) 0.0071(10) 0.0126(10)
C30 0.0286(11) 0.0294(11) 0.0335(12) 0.0084(9) 0.0066(9) 0.0075(9)
C31 0.0221(9) 0.0296(11) 0.0283(11) 0.0079(9) 0.0047(8) 0.0049(8)
C32 0.0365(12) 0.0320(12) 0.0324(12) 0.0085(10) 0.0089(10) 0.0007(10)
C33 0.0369(12) 0.0364(13) 0.0335(13) 0.0011(10) 0.0071(10) 0.0002(10)
C34 0.0308(11) 0.0509(15) 0.0269(11) 0.0065(11) 0.0051(9) 0.0074(11)
C35 0.0277(11) 0.0502(15) 0.0340(12) 0.0205(11) 0.0075(9) 0.0054(10)
C36 0.0252(10) 0.0309(11) 0.0327(12) 0.0113(9) 0.0039(8) 0.0028(9)
C37 0.0253(10) 0.0204(10) 0.0328(11) 0.0079(9) 0.0061(8) 0.0045(8)
C38 0.0311(11) 0.0232(10) 0.0353(12) 0.0076(9) 0.0091(9) 0.0070(9)
C39 0.0390(13) 0.0250(11) 0.0445(14) 0.0086(10) 0.0191(10) 0.0079(9)
C40 0.0276(11) 0.0274(12) 0.0624(17) 0.0110(11) 0.0170(11) 0.0063(9)
C41 0.0264(11) 0.0281(12) 0.0566(16) 0.0090(11) 0.0011(10) 0.0068(9)
C42 0.0296(11) 0.0282(11) 0.0357(12) 0.0103(9) 0.0040(9) 0.0058(9)
C43 0.0470(19) 0.065(2) 0.140(4) -0.034(3) 0.004(2) 0.0192(18)
C44 0.062(2) 0.054(2) 0.096(3) -0.006(2) -0.007(2) 0.0241(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100846.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100846.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100846
loop_
_publ_author_name
'Henry, Renee M.'
'Shoemaker, Richard K.'
'Newell, Rachel H.'
'Jacobsen, George M.'
'DuBois, Daniel L.'
'Rakowski DuBois, M.'
_publ_section_title
;
Stereochemical Control of Iron(II) Complexes Containing a Diphosphine
Ligand with a Pendant Nitrogen Base
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2481
_journal_page_last 2491
_journal_paper_doi 10.1021/om050071c
_journal_volume 24
_chemical_formula_sum 'C73 H97 B2 Fe N3 O P4'
_chemical_formula_weight 1233.89
_chemical_name_common '[Fe(PNP)2(CH3CN)(CO)](BPh4)2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 109.824(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 21.873(10)
_cell_length_b 13.629(6)
_cell_length_c 24.754(11)
_cell_measurement_reflns_used 3425
_cell_measurement_temperature 154(2)
_cell_measurement_theta_max 20.361
_cell_measurement_theta_min 2.136
_cell_volume 6942(6)
_diffrn_ambient_temperature 154(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.3327
_diffrn_reflns_av_sigmaI/netI 0.3926
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 53474
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 1.73
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.353
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.026852
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details
;
absorption correction applied
using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51,
33-38)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.181
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 2640
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.5
_exptl_crystal_size_min 0.55
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.896
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 768
_refine_ls_number_reflns 15911
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.896
_refine_ls_R_factor_all 0.2638
_refine_ls_R_factor_gt 0.1074
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2230
_refine_ls_wR_factor_ref 0.3062
_reflns_number_gt 5699
_reflns_number_total 15911
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100846
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.98805(4) 1.24470(6) 0.75957(4) 0.0259(3) Uani 1 1 d . . .
P1 P 1.07739(9) 1.35492(13) 0.79270(8) 0.0339(5) Uani 1 1 d . . .
P2 P 1.00813(9) 1.20189(13) 0.85400(8) 0.0334(5) Uani 1 1 d . . .
P3 P 1.04361(9) 1.11490(12) 0.73923(8) 0.0292(4) Uani 1 1 d . . .
P4 P 0.95749(9) 1.29848(12) 0.66516(8) 0.0319(4) Uani 1 1 d . . .
N1 N 0.9314(3) 1.3527(4) 0.7693(3) 0.0407(16) Uani 1 1 d . . .
N2 N 1.1154(3) 1.3167(4) 0.9079(2) 0.0386(15) Uani 1 1 d . . .
N3 N 1.0109(3) 1.1491(4) 0.6219(2) 0.0341(14) Uani 1 1 d . . .
O1 O 0.8721(2) 1.1200(3) 0.7324(2) 0.0422(12) Uani 1 1 d . . .
B1 B 1.3706(4) 1.2301(5) 0.8912(3) 0.0310(19) Uani 1 1 d . . .
B2 B 0.9078(4) 0.7480(6) 0.8548(3) 0.0341(19) Uani 1 1 d . . .
C1 C 0.8907(4) 1.4044(5) 0.7662(3) 0.0370(17) Uani 1 1 d . . .
C2 C 0.8378(4) 1.4725(5) 0.7679(3) 0.047(2) Uani 1 1 d . . .
H2A H 0.8380 1.4780 0.8075 0.066 Uiso 1 1 calc R . .
H2B H 0.7957 1.4467 0.7434 0.066 Uiso 1 1 calc R . .
H2C H 0.8449 1.5373 0.7541 0.066 Uiso 1 1 calc R . .
C3 C 0.9180(3) 1.1664(5) 0.7419(3) 0.0318(16) Uani 1 1 d . . .
C4 C 1.0516(4) 1.4806(5) 0.8052(4) 0.050(2) Uani 1 1 d . . .
H4A H 1.0484 1.5205 0.7710 0.070 Uiso 1 1 calc R . .
H4B H 1.0072 1.4755 0.8071 0.070 Uiso 1 1 calc R . .
C5 C 1.0930(5) 1.5379(6) 0.8581(4) 0.082(3) Uani 1 1 d . . .
H5A H 1.0951 1.5018 0.8929 0.115 Uiso 1 1 calc R . .
H5B H 1.0734 1.6025 0.8585 0.115 Uiso 1 1 calc R . .
H5C H 1.1369 1.5462 0.8568 0.115 Uiso 1 1 calc R . .
C6 C 1.1269(3) 1.3699(5) 0.7458(3) 0.0407(18) Uani 1 1 d . . .
H6A H 1.1520 1.3088 0.7478 0.057 Uiso 1 1 calc R . .
H6B H 1.0969 1.3767 0.7057 0.057 Uiso 1 1 calc R . .
C7 C 1.1741(4) 1.4556(6) 0.7584(3) 0.057(2) Uani 1 1 d . . .
H7A H 1.1499 1.5171 0.7475 0.079 Uiso 1 1 calc R . .
H7B H 1.2036 1.4481 0.7364 0.079 Uiso 1 1 calc R . .
H7C H 1.1995 1.4569 0.7996 0.079 Uiso 1 1 calc R . .
C8 C 1.1416(3) 1.3299(5) 0.8621(3) 0.0349(17) Uani 1 1 d . . .
H8A H 1.1655 1.2700 0.8586 0.049 Uiso 1 1 calc R . .
H8B H 1.1728 1.3852 0.8718 0.049 Uiso 1 1 calc R . .
C9 C 1.1638(4) 1.3413(6) 0.9643(3) 0.050(2) Uani 1 1 d . . .
H9A H 1.2002 1.2952 0.9732 0.070 Uiso 1 1 calc R . .
H9B H 1.1435 1.3369 0.9940 0.070 Uiso 1 1 calc R . .
H9C H 1.1797 1.4083 0.9632 0.070 Uiso 1 1 calc R . .
C10 C 1.0900(3) 1.2182(5) 0.9076(3) 0.0382(18) Uani 1 1 d . . .
H10A H 1.0884 1.2031 0.9462 0.053 Uiso 1 1 calc R . .
H10B H 1.1201 1.1708 0.8995 0.053 Uiso 1 1 calc R . .
C11 C 0.9588(3) 1.2753(5) 0.8860(3) 0.0402(19) Uani 1 1 d . . .
H11A H 0.9764 1.2670 0.9283 0.056 Uiso 1 1 calc R . .
H11B H 0.9634 1.3454 0.8776 0.056 Uiso 1 1 calc R . .
C12 C 0.8867(3) 1.2494(5) 0.8651(3) 0.0413(18) Uani 1 1 d . . .
H12A H 0.8694 1.2529 0.8231 0.058 Uiso 1 1 calc R . .
H12B H 0.8634 1.2959 0.8813 0.058 Uiso 1 1 calc R . .
H12C H 0.8811 1.1827 0.8775 0.058 Uiso 1 1 calc R . .
C13 C 0.9917(4) 1.0764(5) 0.8683(3) 0.0378(18) Uani 1 1 d . . .
H13A H 0.9470 1.0605 0.8431 0.053 Uiso 1 1 calc R . .
H13B H 1.0215 1.0337 0.8563 0.053 Uiso 1 1 calc R . .
C14 C 0.9978(4) 1.0481(5) 0.9294(3) 0.0392(18) Uani 1 1 d . . .
H14A H 1.0426 1.0587 0.9549 0.055 Uiso 1 1 calc R . .
H14B H 0.9864 0.9787 0.9305 0.055 Uiso 1 1 calc R . .
H14C H 0.9683 1.0886 0.9422 0.055 Uiso 1 1 calc R . .
C15 C 1.0023(3) 0.9940(4) 0.7314(3) 0.0363(17) Uani 1 1 d . . .
H15A H 1.0361 0.9425 0.7393 0.051 Uiso 1 1 calc R . .
H15B H 0.9823 0.9891 0.7617 0.051 Uiso 1 1 calc R . .
C16 C 0.9498(4) 0.9696(5) 0.6739(3) 0.052(2) Uani 1 1 d . . .
H16A H 0.9144 1.0174 0.6660 0.073 Uiso 1 1 calc R . .
H16B H 0.9328 0.9036 0.6757 0.073 Uiso 1 1 calc R . .
H16C H 0.9685 0.9722 0.6432 0.073 Uiso 1 1 calc R . .
C17 C 1.1244(3) 1.0858(5) 0.7921(3) 0.0324(16) Uani 1 1 d . . .
H17A H 1.1490 1.1480 0.8029 0.045 Uiso 1 1 calc R . .
H17B H 1.1178 1.0598 0.8271 0.045 Uiso 1 1 calc R . .
C18 C 1.1664(4) 1.0135(5) 0.7739(3) 0.0439(19) Uani 1 1 d . . .
H18A H 1.1404 0.9558 0.7565 0.062 Uiso 1 1 calc R . .
H18B H 1.2030 0.9933 0.8076 0.062 Uiso 1 1 calc R . .
H18C H 1.1828 1.0446 0.7459 0.062 Uiso 1 1 calc R . .
C19 C 1.0647(3) 1.1193(5) 0.6733(3) 0.0345(17) Uani 1 1 d . . .
H19A H 1.1012 1.1657 0.6792 0.048 Uiso 1 1 calc R . .
H19B H 1.0800 1.0536 0.6665 0.048 Uiso 1 1 calc R . .
C20 C 1.0227(4) 1.1129(5) 0.5707(3) 0.048(2) Uani 1 1 d . . .
H20A H 1.0666 1.1313 0.5725 0.068 Uiso 1 1 calc R . .
H20B H 0.9909 1.1420 0.5364 0.068 Uiso 1 1 calc R . .
H20C H 1.0184 1.0413 0.5689 0.068 Uiso 1 1 calc R . .
C21 C 1.0023(3) 1.2556(5) 0.6191(3) 0.0364(17) Uani 1 1 d . . .
H21A H 0.9785 1.2751 0.5789 0.051 Uiso 1 1 calc R . .
H21B H 1.0455 1.2876 0.6311 0.051 Uiso 1 1 calc R . .
C22 C 0.8742(3) 1.2640(5) 0.6205(3) 0.0413(18) Uani 1 1 d . . .
H22A H 0.8685 1.2810 0.5802 0.058 Uiso 1 1 calc R . .
H22B H 0.8705 1.1917 0.6223 0.058 Uiso 1 1 calc R . .
C23 C 0.8190(4) 1.3084(6) 0.6347(4) 0.067(3) Uani 1 1 d . . .
H23A H 0.8195 1.2840 0.6721 0.093 Uiso 1 1 calc R . .
H23B H 0.7778 1.2903 0.6051 0.093 Uiso 1 1 calc R . .
H23C H 0.8235 1.3800 0.6362 0.093 Uiso 1 1 calc R . .
C24 C 0.9573(4) 1.4322(5) 0.6557(3) 0.0448(19) Uani 1 1 d . . .
H24A H 0.9303 1.4615 0.6766 0.063 Uiso 1 1 calc R . .
H24B H 1.0023 1.4562 0.6743 0.063 Uiso 1 1 calc R . .
C25 C 0.9322(5) 1.4712(6) 0.5932(4) 0.076(3) Uani 1 1 d . . .
H25A H 0.9597 1.4458 0.5723 0.106 Uiso 1 1 calc R . .
H25B H 0.9338 1.5431 0.5936 0.106 Uiso 1 1 calc R . .
H25C H 0.8873 1.4495 0.5742 0.106 Uiso 1 1 calc R . .
C26 C 1.3447(3) 1.3324(5) 0.9120(3) 0.0344(17) Uani 1 1 d . . .
C27 C 1.3224(3) 1.4141(5) 0.8763(3) 0.0392(18) Uani 1 1 d . . .
H27 H 1.3183 1.4096 0.8370 0.047 Uiso 1 1 calc R . .
C28 C 1.3060(4) 1.5027(6) 0.8972(4) 0.050(2) Uani 1 1 d . . .
H28 H 1.2904 1.5562 0.8716 0.060 Uiso 1 1 calc R . .
C29 C 1.3119(4) 1.5130(6) 0.9539(4) 0.055(2) Uani 1 1 d . . .
H29 H 1.3005 1.5727 0.9679 0.066 Uiso 1 1 calc R . .
C30 C 1.3350(4) 1.4338(7) 0.9901(4) 0.063(2) Uani 1 1 d . . .
H30 H 1.3403 1.4395 1.0297 0.075 Uiso 1 1 calc R . .
C31 C 1.3509(4) 1.3448(6) 0.9690(3) 0.052(2) Uani 1 1 d . . .
H31 H 1.3663 1.2916 0.9948 0.062 Uiso 1 1 calc R . .
C32 C 1.3334(3) 1.1308(5) 0.9039(3) 0.0337(17) Uani 1 1 d . . .
C33 C 1.2854(4) 1.1295(6) 0.9300(3) 0.053(2) Uani 1 1 d . . .
H33 H 1.2719 1.1895 0.9420 0.064 Uiso 1 1 calc R . .
C34 C 1.2567(4) 1.0407(7) 0.9387(4) 0.060(3) Uani 1 1 d . . .
H34 H 1.2254 1.0421 0.9576 0.072 Uiso 1 1 calc R . .
C35 C 1.2733(4) 0.9521(6) 0.9205(4) 0.059(2) Uani 1 1 d . . .
H35 H 1.2530 0.8931 0.9259 0.071 Uiso 1 1 calc R . .
C36 C 1.3198(4) 0.9509(5) 0.8943(3) 0.046(2) Uani 1 1 d . . .
H36 H 1.3328 0.8905 0.8823 0.055 Uiso 1 1 calc R . .
C37 C 1.3471(4) 1.0372(5) 0.8858(3) 0.0405(19) Uani 1 1 d . . .
H37 H 1.3777 1.0341 0.8662 0.049 Uiso 1 1 calc R . .
C38 C 1.3542(3) 1.2294(4) 0.8210(3) 0.0322(16) Uani 1 1 d . . .
C39 C 1.2895(3) 1.2303(5) 0.7843(3) 0.0368(18) Uani 1 1 d . . .
H39 H 1.2561 1.2305 0.8008 0.044 Uiso 1 1 calc R . .
C40 C 1.2716(4) 1.2309(5) 0.7243(3) 0.0423(19) Uani 1 1 d . . .
H40 H 1.2270 1.2306 0.7010 0.051 Uiso 1 1 calc R . .
C41 C 1.3189(4) 1.2320(5) 0.6996(3) 0.0405(18) Uani 1 1 d . . .
H41 H 1.3072 1.2331 0.6590 0.049 Uiso 1 1 calc R . .
C42 C 1.3831(4) 1.2314(5) 0.7336(3) 0.0424(19) Uani 1 1 d . . .
H42 H 1.4161 1.2316 0.7166 0.051 Uiso 1 1 calc R . .
C43 C 1.4000(4) 1.2305(5) 0.7934(3) 0.0375(18) Uani 1 1 d . . .
H43 H 1.4448 1.2306 0.8162 0.045 Uiso 1 1 calc R . .
C44 C 1.4486(3) 1.2231(5) 0.9265(3) 0.0333(17) Uani 1 1 d . . .
C45 C 1.4915(3) 1.2972(5) 0.9207(3) 0.0382(18) Uani 1 1 d . . .
H45 H 1.4734 1.3512 0.8962 0.046 Uiso 1 1 calc R . .
C46 C 1.5585(4) 1.2957(5) 0.9487(3) 0.0431(19) Uani 1 1 d . . .
H46 H 1.5854 1.3448 0.9411 0.052 Uiso 1 1 calc R . .
C47 C 1.5852(4) 1.2216(5) 0.9875(3) 0.0440(19) Uani 1 1 d . . .
H47 H 1.6305 1.2210 1.0082 0.053 Uiso 1 1 calc R . .
C48 C 1.5464(4) 1.1491(5) 0.9963(3) 0.0406(18) Uani 1 1 d . . .
H48 H 1.5652 1.0980 1.0229 0.049 Uiso 1 1 calc R . .
C49 C 1.4801(3) 1.1494(5) 0.9668(3) 0.0313(16) Uani 1 1 d . . .
H49 H 1.4545 1.0979 0.9739 0.038 Uiso 1 1 calc R . .
C50 C 0.8689(3) 0.8453(5) 0.8680(3) 0.0359(17) Uani 1 1 d . . .
C51 C 0.8613(3) 0.8559(5) 0.9215(3) 0.0394(18) Uani 1 1 d . . .
H51 H 0.8757 0.8049 0.9490 0.047 Uiso 1 1 calc R . .
C52 C 0.8331(4) 0.9402(6) 0.9355(4) 0.050(2) Uani 1 1 d . . .
H52 H 0.8299 0.9459 0.9727 0.060 Uiso 1 1 calc R . .
C53 C 0.8095(4) 1.0158(6) 0.8959(4) 0.050(2) Uani 1 1 d . . .
H53 H 0.7892 1.0719 0.9051 0.059 Uiso 1 1 calc R . .
C54 C 0.8166(3) 1.0063(5) 0.8433(4) 0.0428(19) Uani 1 1 d . . .
H54 H 0.8010 1.0569 0.8156 0.051 Uiso 1 1 calc R . .
C55 C 0.8461(3) 0.9241(5) 0.8293(3) 0.0367(17) Uani 1 1 d . . .
H55 H 0.8511 0.9209 0.7927 0.044 Uiso 1 1 calc R . .
C56 C 0.8834(4) 0.6494(5) 0.8822(3) 0.0397(19) Uani 1 1 d . . .
C57 C 0.9248(4) 0.5747(6) 0.9130(4) 0.053(2) Uani 1 1 d . . .
H57 H 0.9700 0.5796 0.9193 0.064 Uiso 1 1 calc R . .
C58 C 0.9013(5) 0.4910(6) 0.9352(4) 0.063(3) Uani 1 1 d . . .
H58 H 0.9305 0.4417 0.9560 0.076 Uiso 1 1 calc R . .
C59 C 0.8357(6) 0.4836(6) 0.9256(4) 0.068(3) Uani 1 1 d . . .
H59 H 0.8198 0.4299 0.9414 0.082 Uiso 1 1 calc R . .
C60 C 0.7926(6) 0.5534(6) 0.8932(5) 0.074(3) Uani 1 1 d . . .
H60 H 0.7471 0.5457 0.8849 0.089 Uiso 1 1 calc R . .
C61 C 0.8170(4) 0.6362(5) 0.8725(4) 0.049(2) Uani 1 1 d . . .
H61 H 0.7872 0.6846 0.8513 0.059 Uiso 1 1 calc R . .
C62 C 0.8879(4) 0.7262(5) 0.7857(3) 0.0393(18) Uani 1 1 d . . .
C63 C 0.8249(4) 0.7423(5) 0.7465(4) 0.049(2) Uani 1 1 d . . .
H63 H 0.7927 0.7676 0.7605 0.059 Uiso 1 1 calc R . .
C64 C 0.8074(4) 0.7225(6) 0.6873(4) 0.056(2) Uani 1 1 d . . .
H64 H 0.7639 0.7323 0.6626 0.067 Uiso 1 1 calc R . .
C65 C 0.8534(5) 0.6888(6) 0.6652(4) 0.059(2) Uani 1 1 d . . .
H65 H 0.8427 0.6782 0.6251 0.071 Uiso 1 1 calc R . .
C66 C 0.9160(4) 0.6706(5) 0.7027(4) 0.047(2) Uani 1 1 d . . .
H66 H 0.9479 0.6450 0.6884 0.057 Uiso 1 1 calc R . .
C67 C 0.9320(4) 0.6896(5) 0.7610(3) 0.0408(18) Uani 1 1 d . . .
H67 H 0.9752 0.6771 0.7854 0.049 Uiso 1 1 calc R . .
C68 C 0.9849(4) 0.7745(5) 0.8871(3) 0.0370(17) Uani 1 1 d . . .
C69 C 1.0225(4) 0.8211(5) 0.8594(3) 0.0371(18) Uani 1 1 d . . .
H69 H 1.0031 0.8344 0.8195 0.045 Uiso 1 1 calc R . .
C70 C 1.0869(4) 0.8496(5) 0.8866(3) 0.0418(19) Uani 1 1 d . . .
H70 H 1.1098 0.8814 0.8652 0.050 Uiso 1 1 calc R . .
C71 C 1.1176(4) 0.8318(6) 0.9448(3) 0.050(2) Uani 1 1 d . . .
H71 H 1.1618 0.8493 0.9636 0.060 Uiso 1 1 calc R . .
C72 C 1.0811(4) 0.7873(6) 0.9744(4) 0.057(2) Uani 1 1 d . . .
H72 H 1.1005 0.7756 1.0144 0.068 Uiso 1 1 calc R . .
C73 C 1.0173(4) 0.7599(5) 0.9467(3) 0.048(2) Uani 1 1 d . . .
H73 H 0.9941 0.7300 0.9686 0.058 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0255(6) 0.0341(5) 0.0116(5) -0.0021(4) -0.0025(4) -0.0006(4)
P1 0.0300(11) 0.0441(11) 0.0210(11) -0.0048(8) 0.0000(9) -0.0033(8)
P2 0.0356(12) 0.0402(10) 0.0178(10) 0.0013(8) 0.0002(9) -0.0009(8)
P3 0.0294(11) 0.0384(10) 0.0124(10) 0.0012(8) -0.0025(8) 0.0044(7)
P4 0.0346(11) 0.0368(10) 0.0176(10) 0.0010(8) 0.0001(9) 0.0035(8)
N1 0.017(3) 0.032(3) 0.068(5) 0.006(3) 0.008(3) 0.007(2)
N2 0.039(4) 0.053(4) 0.016(3) -0.001(3) -0.001(3) -0.012(3)
N3 0.049(4) 0.040(3) 0.002(3) 0.003(2) -0.006(3) 0.013(3)
O1 0.038(3) 0.054(3) 0.026(3) -0.007(2) 0.000(3) -0.009(2)
B1 0.035(5) 0.036(4) 0.020(5) 0.003(3) 0.007(4) -0.003(3)
B2 0.036(5) 0.043(5) 0.018(4) -0.001(4) 0.002(4) 0.005(4)
C1 0.043(5) 0.050(5) 0.012(4) 0.005(3) 0.002(4) 0.001(4)
C2 0.046(5) 0.050(5) 0.033(5) -0.006(4) -0.003(4) 0.009(4)
C3 0.030(4) 0.043(4) 0.012(4) 0.003(3) -0.007(3) -0.002(3)
C4 0.047(5) 0.039(4) 0.054(6) -0.012(4) 0.005(5) -0.003(3)
C5 0.124(10) 0.056(6) 0.042(6) -0.006(5) -0.002(6) 0.012(5)
C6 0.036(5) 0.049(4) 0.024(4) 0.000(3) -0.006(4) -0.001(3)
C7 0.049(6) 0.090(6) 0.021(5) 0.006(4) 0.000(4) -0.021(4)
C8 0.037(4) 0.040(4) 0.013(4) -0.008(3) -0.010(3) -0.005(3)
C9 0.047(5) 0.065(5) 0.027(5) -0.009(4) 0.001(4) -0.013(4)
C10 0.029(4) 0.044(4) 0.029(5) 0.006(3) -0.006(4) 0.001(3)
C11 0.040(5) 0.057(5) 0.027(5) -0.002(3) 0.016(4) -0.003(3)
C12 0.044(5) 0.049(4) 0.028(4) -0.003(4) 0.009(4) 0.000(3)
C13 0.047(5) 0.040(4) 0.023(4) 0.005(3) 0.008(4) 0.005(3)
C14 0.052(5) 0.032(4) 0.027(5) 0.006(3) 0.004(4) -0.005(3)
C15 0.047(5) 0.032(4) 0.020(4) -0.004(3) -0.001(4) 0.005(3)
C16 0.069(6) 0.043(4) 0.032(5) -0.016(4) 0.001(5) -0.006(4)
C17 0.027(4) 0.044(4) 0.015(4) 0.002(3) -0.007(3) 0.001(3)
C18 0.044(5) 0.063(5) 0.015(4) 0.004(4) -0.003(4) 0.021(4)
C19 0.033(4) 0.041(4) 0.022(4) -0.001(3) 0.000(3) 0.010(3)
C20 0.067(6) 0.057(5) 0.013(4) 0.002(3) 0.002(4) 0.020(4)
C21 0.039(4) 0.051(4) 0.012(4) 0.002(3) -0.002(3) 0.005(3)
C22 0.036(5) 0.055(5) 0.022(4) 0.001(3) -0.004(4) -0.006(3)
C23 0.032(5) 0.085(6) 0.063(7) 0.016(5) -0.011(5) 0.003(4)
C24 0.054(5) 0.047(4) 0.029(5) 0.008(4) 0.009(4) 0.008(4)
C25 0.133(10) 0.050(5) 0.039(6) 0.024(4) 0.025(6) 0.022(5)
C26 0.030(4) 0.048(4) 0.018(4) 0.002(3) -0.002(3) 0.000(3)
C27 0.033(5) 0.057(5) 0.022(4) 0.005(4) 0.002(4) -0.005(3)
C28 0.037(5) 0.058(5) 0.045(6) 0.010(4) 0.003(4) -0.001(4)
C29 0.047(6) 0.057(5) 0.052(6) -0.009(5) 0.006(5) -0.001(4)
C30 0.062(7) 0.093(7) 0.020(5) -0.012(5) -0.004(5) 0.009(5)
C31 0.060(6) 0.067(5) 0.014(4) 0.000(4) -0.005(4) 0.020(4)
C32 0.022(4) 0.057(5) 0.014(4) 0.013(3) -0.005(3) 0.004(3)
C33 0.044(5) 0.084(6) 0.028(5) 0.026(4) 0.008(4) 0.017(4)
C34 0.042(6) 0.097(7) 0.045(6) 0.031(5) 0.021(5) 0.006(5)
C35 0.038(5) 0.071(6) 0.049(6) 0.031(5) -0.008(5) -0.001(4)
C36 0.044(5) 0.055(5) 0.021(5) 0.008(4) -0.014(4) 0.003(4)
C37 0.044(5) 0.050(5) 0.018(4) 0.007(3) -0.002(4) -0.012(4)
C38 0.030(4) 0.041(4) 0.020(4) 0.001(3) 0.002(3) 0.000(3)
C39 0.020(4) 0.060(5) 0.028(5) -0.003(3) 0.006(4) -0.004(3)
C40 0.039(5) 0.062(5) 0.013(4) 0.006(3) -0.008(4) -0.009(3)
C41 0.055(6) 0.047(4) 0.014(4) 0.004(3) 0.005(4) -0.007(3)
C42 0.038(5) 0.056(5) 0.033(5) 0.006(4) 0.011(4) -0.002(3)
C43 0.034(5) 0.051(5) 0.025(4) 0.005(3) 0.006(4) 0.006(3)
C44 0.040(5) 0.038(4) 0.012(4) 0.003(3) -0.004(3) 0.003(3)
C45 0.040(5) 0.045(4) 0.020(4) 0.009(3) -0.002(4) -0.004(3)
C46 0.030(5) 0.060(5) 0.033(5) 0.001(4) 0.002(4) -0.012(3)
C47 0.028(4) 0.066(5) 0.025(5) -0.004(4) -0.008(4) 0.003(4)
C48 0.040(5) 0.041(4) 0.028(5) 0.006(3) -0.005(4) 0.010(3)
C49 0.027(4) 0.037(4) 0.025(4) -0.004(3) 0.003(3) 0.002(3)
C50 0.033(4) 0.042(4) 0.028(5) -0.011(3) 0.005(4) -0.009(3)
C51 0.034(5) 0.044(4) 0.040(5) -0.012(4) 0.014(4) -0.010(3)
C52 0.047(5) 0.071(6) 0.034(5) -0.018(4) 0.016(5) -0.016(4)
C53 0.042(5) 0.050(5) 0.049(6) -0.019(4) 0.006(5) -0.003(4)
C54 0.031(5) 0.041(4) 0.039(5) 0.001(4) -0.011(4) -0.007(3)
C55 0.039(5) 0.044(4) 0.022(4) -0.004(3) 0.003(4) -0.003(3)
C56 0.058(6) 0.039(4) 0.018(4) -0.010(3) 0.007(4) 0.006(4)
C57 0.064(6) 0.054(5) 0.039(6) -0.001(4) 0.014(5) -0.010(4)
C58 0.111(9) 0.045(5) 0.035(6) -0.005(4) 0.027(6) -0.001(5)
C59 0.107(9) 0.052(6) 0.064(7) -0.006(5) 0.054(7) -0.014(6)
C60 0.104(9) 0.056(6) 0.074(8) -0.027(5) 0.046(7) -0.027(6)
C61 0.061(6) 0.040(4) 0.047(6) -0.006(4) 0.019(5) -0.003(4)
C62 0.033(5) 0.043(4) 0.038(5) 0.001(3) 0.008(4) -0.007(3)
C63 0.043(5) 0.057(5) 0.040(5) -0.010(4) 0.004(4) 0.005(4)
C64 0.042(5) 0.071(6) 0.038(6) -0.004(4) -0.009(4) -0.009(4)
C65 0.076(7) 0.065(6) 0.034(5) -0.016(4) 0.014(5) -0.014(5)
C66 0.056(6) 0.049(5) 0.040(6) -0.006(4) 0.021(5) -0.004(4)
C67 0.038(5) 0.053(5) 0.027(5) -0.006(4) 0.006(4) -0.002(3)
C68 0.042(5) 0.042(4) 0.027(4) 0.004(3) 0.011(4) 0.003(3)
C69 0.047(5) 0.039(4) 0.020(4) 0.000(3) 0.004(4) 0.004(3)
C70 0.049(5) 0.051(5) 0.025(5) -0.004(4) 0.011(4) -0.009(4)
C71 0.039(5) 0.073(5) 0.026(5) -0.004(4) -0.003(4) -0.005(4)
C72 0.039(5) 0.097(7) 0.023(5) 0.001(4) -0.004(4) 0.000(4)
C73 0.048(5) 0.073(5) 0.021(5) 0.004(4) 0.010(4) -0.007(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100847.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100847.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100847
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C20 H38 B4 Cl2 Ru2'
_chemical_formula_weight 594.78
_space_group_IT_number 88
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_atom_sites_solution_hydrogens 'geom, except difmap for M-H'
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 33.5236(10)
_cell_length_b 33.5236(10)
_cell_length_c 8.7943(4)
_cell_measurement_reflns_used 8697
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.27
_cell_measurement_theta_min 2.40
_cell_volume 9883.3(6)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0268
_diffrn_reflns_av_sigmaI/netI 0.0145
_diffrn_reflns_limit_h_max 44
_diffrn_reflns_limit_h_min -44
_diffrn_reflns_limit_k_max 43
_diffrn_reflns_limit_k_min -44
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 51363
_diffrn_reflns_theta_max 28.27
_diffrn_reflns_theta_min 2.39
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.443
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8865
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.599
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rod
_exptl_crystal_F_000 4800
_exptl_crystal_size_max 0.51
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.13
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.132
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 261
_refine_ls_number_reflns 6119
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.132
_refine_ls_R_factor_all 0.0260
_refine_ls_R_factor_gt 0.0241
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+23.6615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0576
_refine_ls_wR_factor_ref 0.0586
_reflns_number_gt 5794
_reflns_number_total 6119
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_atom_sites_solution_primary' value 'heavy atom' was changed to
'heavy'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M I4(1)/a
_cod_database_code 1100847
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.640029(5) 0.325160(5) 0.057441(18) 0.01698(5) Uani 1 1 d . . .
H8 H 0.6840 0.3285 -0.0191 0.060(10) Uiso 1 1 d R . .
Cl1 Cl 0.635526(18) 0.403240(18) -0.21056(8) 0.03745(14) Uani 1 1 d . . .
C1 C 0.58496(7) 0.28808(7) 0.0650(3) 0.0286(5) Uani 1 1 d . . .
B1 B 0.64981(7) 0.38490(7) -0.0216(3) 0.0250(5) Uani 1 1 d . . .
H1 H 0.6824 0.4052 0.0423 0.037(8) Uiso 1 1 d R . .
Ru2 Ru 0.713823(5) 0.367863(5) 0.036022(18) 0.01665(5) Uani 1 1 d . . .
Cl2 Cl 0.705862(18) 0.300389(18) 0.35237(6) 0.03025(12) Uani 1 1 d . . .
C2 C 0.59143(7) 0.29892(6) -0.0907(3) 0.0272(5) Uani 1 1 d . . .
B2 B 0.61044(8) 0.37912(8) 0.1168(4) 0.0314(6) Uani 1 1 d . . .
H3 H 0.5790 0.3824 0.1074 0.041(8) Uiso 1 1 d R . .
H2 H 0.6286 0.4093 0.0796 0.036(8) Uiso 1 1 d R . .
C3 C 0.62841(6) 0.28247(6) -0.1366(2) 0.0219(4) Uani 1 1 d . . .
B3 B 0.63014(8) 0.35063(8) 0.2768(3) 0.0307(6) Uani 1 1 d . . .
H6 H 0.6608 0.3614 0.3369 0.039(8) Uiso 1 1 d R . .
H5 H 0.6109 0.3390 0.3619 0.041(8) Uiso 1 1 d R . .
H4 H 0.6189 0.3875 0.2588 0.042(8) Uiso 1 1 d R . .
C4 C 0.64445(6) 0.26027(6) -0.0096(2) 0.0204(4) Uani 1 1 d . . .
B4 B 0.68175(7) 0.33832(7) 0.2340(3) 0.0221(5) Uani 1 1 d . . .
H7 H 0.7058 0.3697 0.2244 0.033(7) Uiso 1 1 d R . .
C5 C 0.61723(7) 0.26327(6) 0.1125(2) 0.0250(4) Uani 1 1 d . . .
C6 C 0.54775(8) 0.29568(9) 0.1553(4) 0.0554(9) Uani 1 1 d . . .
H6A H 0.5284 0.2744 0.1354 0.066 Uiso 1 1 calc R . .
H6B H 0.5363 0.3214 0.1256 0.066 Uiso 1 1 calc R . .
H6C H 0.5543 0.2961 0.2639 0.066 Uiso 1 1 calc R . .
C7 C 0.56287(9) 0.32136(8) -0.1887(4) 0.0527(9) Uani 1 1 d . . .
H7A H 0.5450 0.3025 -0.2401 0.063 Uiso 1 1 calc R . .
H7B H 0.5777 0.3367 -0.2648 0.063 Uiso 1 1 calc R . .
H7C H 0.5471 0.3396 -0.1256 0.063 Uiso 1 1 calc R . .
C8 C 0.64494(9) 0.28442(9) -0.2948(3) 0.0413(7) Uani 1 1 d . . .
H8A H 0.6347 0.2620 -0.3544 0.050 Uiso 1 1 calc R . .
H8B H 0.6741 0.2830 -0.2907 0.050 Uiso 1 1 calc R . .
H8C H 0.6368 0.3095 -0.3426 0.050 Uiso 1 1 calc R . .
C9 C 0.68069(7) 0.23415(7) -0.0147(4) 0.0371(6) Uani 1 1 d . . .
H9A H 0.6731 0.2073 -0.0484 0.045 Uiso 1 1 calc R . .
H9B H 0.6926 0.2326 0.0869 0.045 Uiso 1 1 calc R . .
H9C H 0.7001 0.2454 -0.0860 0.045 Uiso 1 1 calc R . .
C10 C 0.62085(10) 0.24160(8) 0.2614(3) 0.0447(7) Uani 1 1 d . . .
H10A H 0.6084 0.2153 0.2527 0.054 Uiso 1 1 calc R . .
H10B H 0.6074 0.2570 0.3412 0.054 Uiso 1 1 calc R . .
H10C H 0.6491 0.2384 0.2873 0.054 Uiso 1 1 calc R . .
C21 C 0.77775(6) 0.36214(7) 0.0813(3) 0.0249(4) Uani 1 1 d . . .
C22 C 0.76963(6) 0.40141(7) 0.0248(2) 0.0223(4) Uani 1 1 d . . .
C23 C 0.75451(6) 0.39698(6) -0.1275(2) 0.0219(4) Uani 1 1 d . . .
C24 C 0.75259(6) 0.35583(7) -0.1622(2) 0.0236(4) Uani 1 1 d . . .
C25 C 0.76712(6) 0.33407(7) -0.0321(3) 0.0252(4) Uani 1 1 d . . .
C26 C 0.79555(8) 0.35277(11) 0.2336(3) 0.0452(7) Uani 1 1 d . . .
H26A H 0.8247 0.3516 0.2247 0.054 Uiso 1 1 calc R . .
H26B H 0.7855 0.3270 0.2692 0.054 Uiso 1 1 calc R . .
H26C H 0.7881 0.3736 0.3064 0.054 Uiso 1 1 calc R . .
C27 C 0.78048(8) 0.43987(8) 0.1016(3) 0.0390(6) Uani 1 1 d . . .
H27A H 0.8078 0.4474 0.0734 0.047 Uiso 1 1 calc R . .
H27B H 0.7788 0.4365 0.2121 0.047 Uiso 1 1 calc R . .
H27C H 0.7620 0.4609 0.0694 0.047 Uiso 1 1 calc R . .
C28 C 0.74473(8) 0.42966(8) -0.2377(3) 0.0365(6) Uani 1 1 d . . .
H28A H 0.7687 0.4368 -0.2955 0.044 Uiso 1 1 calc R . .
H28B H 0.7352 0.4531 -0.1819 0.044 Uiso 1 1 calc R . .
H28C H 0.7239 0.4205 -0.3078 0.044 Uiso 1 1 calc R . .
C29 C 0.74207(8) 0.33879(9) -0.3146(3) 0.0396(6) Uani 1 1 d . . .
H29A H 0.7661 0.3371 -0.3775 0.048 Uiso 1 1 calc R . .
H29B H 0.7224 0.3561 -0.3645 0.048 Uiso 1 1 calc R . .
H29C H 0.7307 0.3121 -0.3013 0.048 Uiso 1 1 calc R . .
C30 C 0.77470(8) 0.29015(8) -0.0220(4) 0.0443(7) Uani 1 1 d . . .
H30A H 0.8013 0.2842 -0.0619 0.053 Uiso 1 1 calc R . .
H30B H 0.7546 0.2758 -0.0819 0.053 Uiso 1 1 calc R . .
H30C H 0.7731 0.2817 0.0845 0.053 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01626(8) 0.01598(8) 0.01869(8) -0.00254(6) 0.00086(6) 0.00014(5)
Cl1 0.0313(3) 0.0314(3) 0.0496(4) 0.0163(3) -0.0150(3) -0.0015(2)
C1 0.0220(10) 0.0239(10) 0.0398(13) -0.0127(9) 0.0069(9) -0.0074(8)
B1 0.0205(11) 0.0194(11) 0.0350(13) 0.0015(10) -0.0014(10) 0.0018(8)
Ru2 0.01663(8) 0.01759(8) 0.01573(8) -0.00129(6) -0.00004(6) -0.00049(5)
Cl2 0.0390(3) 0.0354(3) 0.0163(2) 0.0055(2) -0.0066(2) -0.0099(2)
C2 0.0225(10) 0.0200(10) 0.0391(13) -0.0002(9) -0.0118(9) -0.0004(8)
B2 0.0216(11) 0.0207(11) 0.0519(17) -0.0087(11) 0.0066(11) 0.0004(9)
C3 0.0258(10) 0.0215(9) 0.0185(9) -0.0028(8) -0.0036(8) -0.0057(8)
B3 0.0290(13) 0.0299(13) 0.0332(14) -0.0140(11) 0.0111(11) -0.0071(10)
C4 0.0222(9) 0.0152(9) 0.0237(10) -0.0035(7) -0.0043(8) -0.0006(7)
B4 0.0251(11) 0.0250(11) 0.0161(10) -0.0047(9) 0.0026(9) -0.0055(9)
C5 0.0337(11) 0.0219(10) 0.0193(10) -0.0015(8) -0.0016(9) -0.0102(9)
C6 0.0317(14) 0.0466(16) 0.088(3) -0.0329(17) 0.0268(15) -0.0167(12)
C7 0.0414(15) 0.0309(13) 0.086(2) 0.0083(14) -0.0387(16) 0.0000(11)
C8 0.0583(17) 0.0479(15) 0.0176(11) -0.0069(10) 0.0020(11) -0.0231(13)
C9 0.0290(12) 0.0219(11) 0.0604(17) -0.0056(11) -0.0094(12) 0.0053(9)
C10 0.072(2) 0.0402(15) 0.0223(12) 0.0067(10) -0.0059(12) -0.0290(14)
C21 0.0165(9) 0.0367(12) 0.0215(10) 0.0046(9) -0.0001(8) -0.0006(8)
C22 0.0170(9) 0.0284(11) 0.0215(10) -0.0039(8) 0.0032(8) -0.0038(8)
C23 0.0180(9) 0.0274(10) 0.0202(10) 0.0038(8) 0.0028(8) -0.0009(8)
C24 0.0181(9) 0.0325(11) 0.0201(10) -0.0033(8) 0.0032(8) -0.0031(8)
C25 0.0187(10) 0.0247(10) 0.0323(12) 0.0013(9) 0.0057(8) 0.0014(8)
C26 0.0234(12) 0.086(2) 0.0260(12) 0.0192(14) -0.0043(10) 0.0010(13)
C27 0.0288(12) 0.0425(14) 0.0458(15) -0.0201(12) 0.0111(11) -0.0123(10)
C28 0.0287(12) 0.0423(14) 0.0384(14) 0.0192(12) 0.0071(10) 0.0036(10)
C29 0.0318(13) 0.0613(18) 0.0258(12) -0.0184(12) 0.0044(10) -0.0085(12)
C30 0.0321(13) 0.0286(12) 0.072(2) 0.0069(13) 0.0185(13) 0.0084(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100848.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100848.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100848
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C20 H36 B4 Cl2 Ru2'
_chemical_formula_weight 592.77
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens 'geom except difmap for B-H'
_atom_sites_solution_primary patterson
_atom_sites_solution_secondary difmap
_cell_angle_alpha 76.6780(10)
_cell_angle_beta 79.1590(10)
_cell_angle_gamma 67.7320(10)
_cell_formula_units_Z 2
_cell_length_a 9.0023(3)
_cell_length_b 9.5781(4)
_cell_length_c 16.0270(6)
_cell_measurement_reflns_used 9819
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.29
_cell_measurement_theta_min 2.46
_cell_volume 1236.64(8)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0185
_diffrn_reflns_av_sigmaI/netI 0.0276
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 13410
_diffrn_reflns_theta_max 28.29
_diffrn_reflns_theta_min 2.33
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.442
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8916
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.592
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 596
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 337
_refine_ls_number_reflns 6132
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0251
_refine_ls_R_factor_gt 0.0225
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.6118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0556
_refine_ls_wR_factor_ref 0.0570
_reflns_number_gt 5625
_reflns_number_total 6132
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100848
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.891521(16) 0.841324(16) 0.825640(9) 0.01421(4) Uani 1 1 d . . .
H6 H 0.8850 0.8451 0.7158 0.017 Uiso 1 1 d R . .
Cl1 Cl 0.85386(7) 1.34071(6) 0.64218(3) 0.03022(12) Uani 1 1 d . . .
C1 C 0.7960(2) 0.6734(2) 0.91757(12) 0.0186(4) Uani 1 1 d . . .
B1 B 0.9749(3) 1.0406(3) 0.78630(14) 0.0208(4) Uani 1 1 d . . .
H1 H 1.0632 1.0835 0.8326 0.025 Uiso 1 1 d R . .
H3 H 1.0185 1.0784 0.7069 0.025 Uiso 1 1 d R . .
H2 H 1.0445 0.9016 0.7761 0.025 Uiso 1 1 d R . .
Ru2 Ru 0.724639(18) 1.013837(17) 0.678124(9) 0.01754(5) Uani 1 1 d . . .
Cl2 Cl 0.63630(6) 1.24762(5) 0.85080(3) 0.02190(10) Uani 1 1 d . . .
C2 C 0.9344(2) 0.5897(2) 0.86484(12) 0.0194(4) Uani 1 1 d . . .
B2 B 0.8725(3) 1.1450(3) 0.69173(14) 0.0225(4) Uani 1 1 d . A .
H4 H 0.8851 1.0589 0.6366 0.027 Uiso 1 1 d R . .
C3 C 1.0695(2) 0.6206(2) 0.87867(12) 0.0187(4) Uani 1 1 d . . .
B3 B 0.7663(3) 1.0934(2) 0.78947(13) 0.0181(4) Uani 1 1 d . A .
C4 C 1.0170(2) 0.7223(2) 0.94075(12) 0.0180(4) Uani 1 1 d . . .
B4 B 0.6569(3) 0.9640(2) 0.80753(14) 0.0176(4) Uani 1 1 d . A .
H5 H 0.5414 0.9720 0.8404 0.021 Uiso 1 1 d R . .
C5 C 0.8476(2) 0.7553(2) 0.96469(12) 0.0185(4) Uani 1 1 d . . .
C6 C 0.6333(2) 0.6570(2) 0.93201(14) 0.0262(4) Uani 1 1 d . . .
H6A H 0.6332 0.5701 0.9783 0.031 Uiso 1 1 calc R . .
H6B H 0.6100 0.6394 0.8788 0.031 Uiso 1 1 calc R . .
H6C H 0.5505 0.7510 0.9483 0.031 Uiso 1 1 calc R . .
C7 C 0.9374(3) 0.4838(2) 0.80841(14) 0.0263(4) Uani 1 1 d . . .
H7A H 0.9582 0.3804 0.8422 0.032 Uiso 1 1 calc R . .
H7B H 1.0231 0.4818 0.7604 0.032 Uiso 1 1 calc R . .
H7C H 0.8330 0.5199 0.7857 0.032 Uiso 1 1 calc R . .
C8 C 1.2404(2) 0.5507(2) 0.83919(14) 0.0261(4) Uani 1 1 d . . .
H8A H 1.2938 0.4525 0.8752 0.031 Uiso 1 1 calc R . .
H8B H 1.2991 0.6202 0.8354 0.031 Uiso 1 1 calc R . .
H8C H 1.2396 0.5340 0.7812 0.031 Uiso 1 1 calc R . .
C9 C 1.1239(2) 0.7759(2) 0.97705(14) 0.0251(4) Uani 1 1 d . . .
H9A H 1.1649 0.7031 1.0287 0.030 Uiso 1 1 calc R . .
H9B H 1.0618 0.8772 0.9924 0.030 Uiso 1 1 calc R . .
H9C H 1.2149 0.7825 0.9338 0.030 Uiso 1 1 calc R . .
C10 C 0.7431(2) 0.8528(2) 1.02958(13) 0.0238(4) Uani 1 1 d . . .
H10A H 0.7425 0.7887 1.0869 0.029 Uiso 1 1 calc R . .
H10B H 0.6326 0.9010 1.0136 0.029 Uiso 1 1 calc R . .
H10C H 0.7858 0.9324 1.0306 0.029 Uiso 1 1 calc R . .
C21 C 0.5635(8) 1.1526(7) 0.5777(4) 0.0179(12) Uani 0.51 1 d P A 1
C21A C 0.5375(9) 1.1880(8) 0.6021(4) 0.0177(12) Uani 0.49 1 d P A 2
C22 C 0.6714(6) 1.0158(9) 0.5467(4) 0.0179(10) Uani 0.51 1 d P A 1
C22A C 0.6628(6) 1.1054(8) 0.5444(3) 0.0210(8) Uani 0.49 1 d P A 2
C23 C 0.6384(7) 0.8892(5) 0.6001(4) 0.0181(8) Uani 0.51 1 d P A 1
C23A C 0.6817(7) 0.9472(9) 0.5659(4) 0.0208(12) Uani 0.49 1 d P A 2
C24 C 0.5107(6) 0.9454(7) 0.6657(4) 0.0181(10) Uani 0.51 1 d P A 1
C24A C 0.5671(8) 0.9283(7) 0.6386(5) 0.0203(11) Uani 0.49 1 d P A 2
C25 C 0.4700(2) 1.0946(3) 0.65581(14) 0.0255(4) Uani 1 1 d . A .
C26 C 0.5432(6) 1.3151(5) 0.5362(3) 0.0316(10) Uani 0.51 1 d P A 1
H26A H 0.4650 1.3510 0.4940 0.038 Uiso 0.51 1 calc PR A 1
H26B H 0.6474 1.3204 0.5070 0.038 Uiso 0.51 1 calc PR A 1
H26C H 0.5039 1.3802 0.5805 0.038 Uiso 0.51 1 calc PR A 1
C26A C 0.4720(5) 1.3579(5) 0.6010(3) 0.0287(9) Uani 0.49 1 d P A 2
H26D H 0.3901 1.4077 0.5606 0.034 Uiso 0.49 1 calc PR A 2
H26E H 0.5601 1.3986 0.5826 0.034 Uiso 0.49 1 calc PR A 2
H26F H 0.4231 1.3782 0.6590 0.034 Uiso 0.49 1 calc PR A 2
C27 C 0.7933(5) 1.0079(6) 0.4681(3) 0.0330(10) Uani 0.51 1 d P A 1
H27A H 0.7437 1.0108 0.4180 0.040 Uiso 0.51 1 calc PR A 1
H27B H 0.8859 0.9124 0.4772 0.040 Uiso 0.51 1 calc PR A 1
H27C H 0.8296 1.0954 0.4577 0.040 Uiso 0.51 1 calc PR A 1
C27A C 0.7576(6) 1.1792(6) 0.4706(3) 0.0344(11) Uani 0.49 1 d P A 2
H27D H 0.7014 1.2121 0.4188 0.041 Uiso 0.49 1 calc PR A 2
H27E H 0.8659 1.1047 0.4588 0.041 Uiso 0.49 1 calc PR A 2
H27F H 0.7665 1.2683 0.4866 0.041 Uiso 0.49 1 calc PR A 2
C28 C 0.7161(6) 0.7247(5) 0.5874(3) 0.0327(10) Uani 0.51 1 d P A 1
H28A H 0.6520 0.7028 0.5524 0.039 Uiso 0.51 1 calc PR A 1
H28B H 0.7212 0.6568 0.6436 0.039 Uiso 0.51 1 calc PR A 1
H28C H 0.8256 0.7075 0.5578 0.039 Uiso 0.51 1 calc PR A 1
C28A C 0.7951(6) 0.8233(6) 0.5171(3) 0.0395(13) Uani 0.49 1 d P A 2
H28D H 0.7427 0.8193 0.4698 0.047 Uiso 0.49 1 calc PR A 2
H28E H 0.8225 0.7243 0.5562 0.047 Uiso 0.49 1 calc PR A 2
H28F H 0.8938 0.8458 0.4935 0.047 Uiso 0.49 1 calc PR A 2
C29 C 0.4269(5) 0.8478(5) 0.7294(3) 0.0288(9) Uani 0.51 1 d P A 1
H29A H 0.3411 0.8405 0.7028 0.035 Uiso 0.51 1 calc PR A 1
H29B H 0.3799 0.8947 0.7810 0.035 Uiso 0.51 1 calc PR A 1
H29C H 0.5054 0.7450 0.7456 0.035 Uiso 0.51 1 calc PR A 1
C29A C 0.5344(6) 0.7860(6) 0.6800(4) 0.0380(12) Uani 0.49 1 d P A 2
H29D H 0.4591 0.7726 0.6483 0.046 Uiso 0.49 1 calc PR A 2
H29E H 0.4867 0.7933 0.7398 0.046 Uiso 0.49 1 calc PR A 2
H29F H 0.6357 0.6980 0.6794 0.046 Uiso 0.49 1 calc PR A 2
C30 C 0.3271(5) 1.2142(6) 0.7022(3) 0.0280(9) Uani 0.51 1 d P A 1
H30A H 0.2260 1.2304 0.6804 0.034 Uiso 0.51 1 calc PR A 1
H30B H 0.3462 1.3114 0.6908 0.034 Uiso 0.51 1 calc PR A 1
H30C H 0.3193 1.1759 0.7645 0.034 Uiso 0.51 1 calc PR A 1
C30A C 0.3292(5) 1.1235(7) 0.7250(3) 0.0279(9) Uani 0.49 1 d P A 2
H30D H 0.2283 1.1590 0.6988 0.034 Uiso 0.49 1 calc PR A 2
H30E H 0.3289 1.2020 0.7550 0.034 Uiso 0.49 1 calc PR A 2
H30F H 0.3386 1.0284 0.7664 0.034 Uiso 0.49 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01365(7) 0.01399(7) 0.01434(8) -0.00352(5) -0.00210(5) -0.00327(6)
Cl1 0.0464(3) 0.0209(2) 0.0237(2) -0.00143(19) -0.0017(2) -0.0147(2)
C1 0.0199(9) 0.0155(8) 0.0191(9) -0.0002(7) -0.0032(7) -0.0059(7)
B1 0.0208(10) 0.0212(10) 0.0196(10) -0.0048(8) 0.0002(8) -0.0070(8)
Ru2 0.01830(8) 0.01723(8) 0.01368(8) -0.00541(6) -0.00335(6) -0.00016(6)
Cl2 0.0224(2) 0.0199(2) 0.0221(2) -0.01029(17) -0.00105(17) -0.00275(18)
C2 0.0223(9) 0.0156(8) 0.0186(9) -0.0009(7) -0.0046(7) -0.0049(7)
B2 0.0299(12) 0.0176(10) 0.0182(10) -0.0039(8) -0.0005(9) -0.0069(9)
C3 0.0187(9) 0.0153(8) 0.0188(9) -0.0025(7) -0.0040(7) -0.0017(7)
B3 0.0215(10) 0.0155(9) 0.0153(9) -0.0049(8) -0.0016(8) -0.0032(8)
C4 0.0199(9) 0.0155(8) 0.0178(9) -0.0018(7) -0.0050(7) -0.0044(7)
B4 0.0172(10) 0.0169(9) 0.0171(10) -0.0052(8) -0.0041(8) -0.0020(8)
C5 0.0192(9) 0.0167(9) 0.0174(9) -0.0016(7) -0.0029(7) -0.0043(7)
C6 0.0229(10) 0.0273(10) 0.0295(11) -0.0017(9) -0.0027(8) -0.0121(8)
C7 0.0340(11) 0.0207(10) 0.0259(10) -0.0078(8) -0.0054(9) -0.0085(9)
C8 0.0185(9) 0.0237(10) 0.0307(11) -0.0056(8) -0.0019(8) -0.0012(8)
C9 0.0253(10) 0.0259(10) 0.0264(10) -0.0054(8) -0.0088(8) -0.0082(8)
C10 0.0253(10) 0.0235(10) 0.0199(9) -0.0062(8) 0.0016(8) -0.0061(8)
C21 0.020(4) 0.014(3) 0.019(3) -0.0040(19) -0.007(3) -0.002(2)
C21A 0.011(2) 0.022(3) 0.018(3) -0.006(2) -0.004(2) -0.001(2)
C22 0.017(2) 0.023(3) 0.012(2) -0.007(3) -0.0029(16) -0.003(3)
C22A 0.018(2) 0.032(3) 0.013(2) -0.008(2) -0.0053(18) -0.006(2)
C23 0.019(2) 0.017(2) 0.020(2) -0.007(2) -0.0090(19) -0.003(2)
C23A 0.018(2) 0.023(3) 0.022(4) -0.012(3) -0.007(2) -0.001(3)
C24 0.012(3) 0.022(2) 0.021(3) -0.006(2) -0.0066(19) -0.003(2)
C24A 0.017(3) 0.020(3) 0.026(4) -0.008(3) -0.008(2) -0.005(3)
C25 0.0176(9) 0.0402(12) 0.0241(10) -0.0157(9) -0.0017(8) -0.0107(9)
C26 0.037(2) 0.021(2) 0.036(2) 0.0059(18) -0.017(2) -0.0092(18)
C26A 0.026(2) 0.022(2) 0.035(2) -0.0014(18) -0.0134(19) -0.0039(17)
C27 0.024(2) 0.057(3) 0.0150(18) -0.0107(19) -0.0025(16) -0.008(2)
C27A 0.027(2) 0.058(3) 0.017(2) 0.001(2) -0.0039(17) -0.017(2)
C28 0.035(2) 0.020(2) 0.045(3) -0.0180(19) -0.015(2) -0.0003(18)
C28A 0.028(2) 0.050(3) 0.044(3) -0.034(2) -0.014(2) 0.002(2)
C29 0.029(2) 0.033(2) 0.031(2) 0.0033(18) -0.0101(18) -0.0192(19)
C29A 0.040(3) 0.033(3) 0.051(3) -0.002(2) -0.025(2) -0.019(2)
C30 0.020(2) 0.032(2) 0.028(2) -0.014(2) -0.0026(17) -0.0005(19)
C30A 0.015(2) 0.043(3) 0.024(2) -0.003(2) -0.0042(16) -0.008(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100849.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100849.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100849
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C20 H35 B4 Cl3 Ru2'
_chemical_formula_weight 627.21
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens 'geom, except difmap for M-H'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 105.0630(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.5503(4)
_cell_length_b 13.9118(5)
_cell_length_c 17.6855(7)
_cell_measurement_reflns_used 8780
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.29
_cell_measurement_theta_min 2.39
_cell_volume 2506.58(16)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0262
_diffrn_reflns_av_sigmaI/netI 0.0228
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 26582
_diffrn_reflns_theta_max 28.31
_diffrn_reflns_theta_min 1.89
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.531
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9141
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.662
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rectangular
_exptl_crystal_F_000 1256
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 262
_refine_ls_number_reflns 6228
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.025
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0228
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.8061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0575
_refine_ls_wR_factor_ref 0.0589
_reflns_number_gt 5712
_reflns_number_total 6228
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100849
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.465532(14) 0.394409(11) 0.270331(8) 0.01292(5) Uani 1 1 d . . .
Cl1 Cl 0.20009(5) 0.50750(4) 0.12306(3) 0.02264(10) Uani 1 1 d . . .
C1 C 0.34484(19) 0.44528(15) 0.34647(11) 0.0191(4) Uani 1 1 d . . .
B1 B 0.3627(2) 0.45712(15) 0.15531(13) 0.0153(4) Uani 1 1 d . . .
H1 H 0.4377 0.4978 0.2176 0.018 Uiso 1 1 d R . .
Ru2 Ru 0.602636(14) 0.315078(11) 0.163249(8) 0.01293(5) Uani 1 1 d . . .
H5 H 0.6190 0.3990 0.2430 0.016 Uiso 1 1 d R . .
Cl2 Cl 0.38099(5) 0.40164(4) -0.01695(3) 0.02031(10) Uani 1 1 d . . .
C2 C 0.34945(19) 0.34279(15) 0.34871(11) 0.0184(4) Uani 1 1 d . . .
B2 B 0.4486(2) 0.40628(15) 0.08815(12) 0.0155(4) Uani 1 1 d . . .
H3 H 0.5670 0.4187 0.1106 0.019 Uiso 1 1 d R . .
H2 H 0.4264 0.4949 0.1073 0.019 Uiso 1 1 d R . .
Cl3 Cl 0.24154(4) 0.25963(3) 0.10786(3) 0.01892(10) Uani 1 1 d . . .
B3 B 0.3883(2) 0.33335(15) 0.15090(12) 0.0142(4) Uani 1 1 d . . .
C3 C 0.4844(2) 0.31376(15) 0.38155(11) 0.0188(4) Uani 1 1 d . . .
B4 B 0.4840(2) 0.26005(16) 0.22732(13) 0.0157(4) Uani 1 1 d . . .
H4 H 0.4388 0.1556 0.2535 0.019 Uiso 1 1 d R . .
C4 C 0.56166(19) 0.40018(15) 0.39931(11) 0.0191(4) Uani 1 1 d . . .
C5 C 0.4777(2) 0.48057(15) 0.37831(11) 0.0197(4) Uani 1 1 d . . .
C6 C 0.2226(2) 0.50477(17) 0.32371(13) 0.0251(4) Uani 1 1 d . . .
H6A H 0.1898 0.5164 0.3699 0.030 Uiso 1 1 calc R . .
H6B H 0.1557 0.4705 0.2840 0.030 Uiso 1 1 calc R . .
H6C H 0.2422 0.5663 0.3023 0.030 Uiso 1 1 calc R . .
C7 C 0.2321(2) 0.27822(16) 0.32226(12) 0.0227(4) Uani 1 1 d . . .
H7A H 0.1956 0.2642 0.3667 0.027 Uiso 1 1 calc R . .
H7B H 0.2586 0.2181 0.3019 0.027 Uiso 1 1 calc R . .
H7C H 0.1654 0.3103 0.2809 0.027 Uiso 1 1 calc R . .
C8 C 0.5323(2) 0.21436(16) 0.40618(13) 0.0250(4) Uani 1 1 d . . .
H8A H 0.5268 0.2028 0.4599 0.030 Uiso 1 1 calc R . .
H8B H 0.6236 0.2079 0.4037 0.030 Uiso 1 1 calc R . .
H8C H 0.4776 0.1674 0.3710 0.030 Uiso 1 1 calc R . .
C9 C 0.7060(2) 0.40344(17) 0.43908(12) 0.0241(4) Uani 1 1 d . . .
H9A H 0.7187 0.4059 0.4959 0.029 Uiso 1 1 calc R . .
H9B H 0.7447 0.4608 0.4219 0.029 Uiso 1 1 calc R . .
H9C H 0.7486 0.3458 0.4253 0.029 Uiso 1 1 calc R . .
C10 C 0.5164(2) 0.58383(16) 0.39257(13) 0.0252(4) Uani 1 1 d . . .
H10A H 0.5125 0.6022 0.4454 0.030 Uiso 1 1 calc R . .
H10B H 0.4560 0.6242 0.3540 0.030 Uiso 1 1 calc R . .
H10C H 0.6060 0.5927 0.3876 0.030 Uiso 1 1 calc R . .
C21 C 0.6511(2) 0.19185(15) 0.09737(14) 0.0241(4) Uani 1 1 d . . .
C22 C 0.7227(2) 0.27379(16) 0.08391(12) 0.0209(4) Uani 1 1 d . . .
C23 C 0.81049(19) 0.30301(15) 0.15699(12) 0.0186(4) Uani 1 1 d . . .
C24 C 0.79170(19) 0.23902(16) 0.21548(12) 0.0211(4) Uani 1 1 d . . .
C25 C 0.6942(2) 0.16982(15) 0.17926(14) 0.0235(4) Uani 1 1 d . . .
C26 C 0.5536(3) 0.1361(2) 0.03537(18) 0.0411(7) Uani 1 1 d . . .
H26A H 0.5994 0.0850 0.0149 0.049 Uiso 1 1 calc R . .
H26B H 0.5110 0.1794 -0.0073 0.049 Uiso 1 1 calc R . .
H26C H 0.4872 0.1076 0.0583 0.049 Uiso 1 1 calc R . .
C27 C 0.7170(3) 0.3200(2) 0.00630(14) 0.0353(6) Uani 1 1 d . . .
H27A H 0.7804 0.2888 -0.0175 0.042 Uiso 1 1 calc R . .
H27B H 0.7383 0.3884 0.0141 0.042 Uiso 1 1 calc R . .
H27C H 0.6284 0.3128 -0.0283 0.042 Uiso 1 1 calc R . .
C28 C 0.9117(2) 0.38068(17) 0.16604(16) 0.0306(5) Uani 1 1 d . . .
H28A H 0.9940 0.3531 0.1601 0.037 Uiso 1 1 calc R . .
H28B H 0.9265 0.4098 0.2181 0.037 Uiso 1 1 calc R . .
H28C H 0.8808 0.4300 0.1259 0.037 Uiso 1 1 calc R . .
C29 C 0.8683(2) 0.2370(2) 0.29979(14) 0.0351(6) Uani 1 1 d . . .
H29A H 0.9475 0.1979 0.3052 0.042 Uiso 1 1 calc R . .
H29B H 0.8141 0.2092 0.3316 0.042 Uiso 1 1 calc R . .
H29C H 0.8934 0.3027 0.3176 0.042 Uiso 1 1 calc R . .
C30 C 0.6616(3) 0.08028(18) 0.21762(19) 0.0403(7) Uani 1 1 d . . .
H30A H 0.7236 0.0293 0.2136 0.048 Uiso 1 1 calc R . .
H30B H 0.5722 0.0597 0.1914 0.048 Uiso 1 1 calc R . .
H30C H 0.6679 0.0934 0.2729 0.048 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01261(8) 0.01407(8) 0.01186(8) -0.00005(5) 0.00279(5) -0.00193(5)
Cl1 0.0197(2) 0.0218(2) 0.0266(3) 0.00432(19) 0.00635(19) 0.00553(18)
C1 0.0175(9) 0.0256(10) 0.0155(9) -0.0029(8) 0.0068(7) -0.0025(8)
B1 0.0149(10) 0.0136(10) 0.0174(10) 0.0017(8) 0.0040(8) 0.0014(8)
Ru2 0.01245(8) 0.01306(8) 0.01316(8) 0.00118(5) 0.00311(6) 0.00011(5)
Cl2 0.0229(2) 0.0231(2) 0.0137(2) 0.00194(17) 0.00258(18) -0.00125(18)
C2 0.0169(9) 0.0246(10) 0.0141(9) 0.0008(8) 0.0047(7) -0.0041(8)
B2 0.0164(10) 0.0159(10) 0.0140(9) 0.0003(8) 0.0037(8) 0.0001(8)
Cl3 0.0170(2) 0.0192(2) 0.0182(2) -0.00051(17) 0.00043(17) -0.00506(17)
B3 0.0129(9) 0.0148(9) 0.0146(9) 0.0004(8) 0.0030(8) -0.0018(8)
C3 0.0180(9) 0.0259(10) 0.0119(9) 0.0025(7) 0.0027(7) -0.0042(8)
B4 0.0132(9) 0.0169(10) 0.0157(10) -0.0001(8) 0.0014(8) 0.0007(8)
C4 0.0160(9) 0.0291(11) 0.0115(9) -0.0007(8) 0.0025(7) -0.0060(8)
C5 0.0214(10) 0.0244(10) 0.0149(9) -0.0052(8) 0.0074(7) -0.0070(8)
C6 0.0201(10) 0.0297(11) 0.0272(11) -0.0061(9) 0.0093(9) 0.0011(8)
C7 0.0183(10) 0.0285(11) 0.0205(10) 0.0023(8) 0.0036(8) -0.0072(8)
C8 0.0235(10) 0.0282(11) 0.0207(10) 0.0092(9) 0.0010(8) -0.0042(9)
C9 0.0193(10) 0.0335(12) 0.0166(10) 0.0023(8) -0.0003(8) -0.0075(9)
C10 0.0252(11) 0.0258(11) 0.0260(11) -0.0098(9) 0.0093(9) -0.0063(9)
C21 0.0180(10) 0.0198(10) 0.0326(12) -0.0061(9) 0.0032(9) 0.0048(8)
C22 0.0213(10) 0.0234(10) 0.0188(10) -0.0007(8) 0.0065(8) 0.0067(8)
C23 0.0150(9) 0.0205(10) 0.0221(10) -0.0025(8) 0.0077(8) 0.0014(7)
C24 0.0163(9) 0.0267(11) 0.0204(10) 0.0025(8) 0.0046(8) 0.0066(8)
C25 0.0178(10) 0.0182(10) 0.0365(12) 0.0066(9) 0.0110(9) 0.0069(8)
C26 0.0288(12) 0.0311(13) 0.0555(17) -0.0223(12) -0.0034(12) 0.0060(10)
C27 0.0417(14) 0.0464(15) 0.0217(11) 0.0063(10) 0.0151(10) 0.0176(12)
C28 0.0226(11) 0.0276(12) 0.0450(14) -0.0069(10) 0.0147(10) -0.0057(9)
C29 0.0229(11) 0.0582(17) 0.0220(11) 0.0051(11) 0.0021(9) 0.0122(11)
C30 0.0314(13) 0.0236(12) 0.071(2) 0.0184(12) 0.0221(13) 0.0098(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100850.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100850.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100850
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C24.5 H43.84 B5 Cl3 Ru2 S'
_chemical_formula_weight 733.03
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 22.027(3)
_cell_length_b 12.4145(14)
_cell_length_c 23.813(3)
_cell_measurement_reflns_used 8306
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.31
_cell_measurement_theta_min 2.47
_cell_volume 6511.5(13)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_sigmaI/netI 0.0176
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 66921
_diffrn_reflns_theta_max 28.32
_diffrn_reflns_theta_min 1.85
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.252
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8722
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.495
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 2967
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.163
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 343
_refine_ls_number_reflns 8094
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.163
_refine_ls_R_factor_all 0.0372
_refine_ls_R_factor_gt 0.0348
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+14.9294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1026
_refine_ls_wR_factor_ref 0.1041
_reflns_number_gt 7540
_reflns_number_total 8094
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Pbca
_cod_original_formula_sum 'C24.50 H43.84 B5 Cl3 Ru2 S'
_cod_database_code 1100850
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru -0.045507(10) 0.295288(17) 0.108988(9) 0.01298(7) Uani 1 1 d . . .
S1 S -0.10678(4) 0.32457(6) 0.26012(3) 0.01903(15) Uani 1 1 d . . .
Cl1 Cl 0.06797(3) 0.25099(6) 0.21487(3) 0.02425(16) Uani 1 1 d . . .
C1 C 0.02806(14) 0.3419(2) 0.05003(13) 0.0189(6) Uani 1 1 d . . .
B1 B -0.00337(15) 0.2201(3) 0.18004(14) 0.0161(6) Uani 1 1 d . . .
C1S C -0.2607(4) 0.3135(14) 0.3794(4) 0.074(4) Uani 0.50 1 d P . .
Ru2 Ru -0.124200(10) 0.129405(17) 0.140341(9) 0.01274(7) Uani 1 1 d . . .
C2 C 0.01791(14) 0.4282(2) 0.08866(13) 0.0191(6) Uani 1 1 d . . .
Cl2 Cl -0.19192(3) 0.38686(6) 0.14630(3) 0.02000(15) Uani 1 1 d . . .
B2 B -0.07885(14) 0.2509(3) 0.19446(13) 0.0149(6) Uani 1 1 d . . .
C2S C -0.2204(4) 0.4195(12) 0.3728(3) 0.063(4) Uani 0.50 1 d P . .
Cl3 Cl 0.02558(3) 0.02633(6) 0.09640(3) 0.02152(15) Uani 1 1 d . . .
B3 B -0.05202(15) 0.1196(3) 0.19983(14) 0.0167(6) Uani 1 1 d . . .
H1 H -0.0392 0.0415 0.2418 0.020 Uiso 1 1 d R . .
C3 C -0.04291(14) 0.4671(2) 0.07972(13) 0.0189(6) Uani 1 1 d . . .
C3S C -0.2558(4) 0.5177(14) 0.3839(3) 0.075(5) Uani 0.50 1 d P . .
C4 C -0.06990(14) 0.4040(2) 0.03624(13) 0.0200(6) Uani 1 1 d . . .
B4 B -0.13178(15) 0.2921(3) 0.13966(14) 0.0162(6) Uani 1 1 d . . .
C4S C -0.2251(5) 0.6161(12) 0.3744(4) 0.066(3) Uani 0.50 1 d P . .
B5 B -0.02325(15) 0.1228(3) 0.13247(14) 0.0161(6) Uani 1 1 d . . .
H2 H -0.0576 0.1817 0.0965 0.019 Uiso 1 1 d R . .
C5 C -0.02641(14) 0.3253(2) 0.01838(12) 0.0189(6) Uani 1 1 d . . .
C5S C -0.2685(6) 0.7109(13) 0.3782(4) 0.069(4) Uani 0.50 1 d P . .
C6 C 0.08609(15) 0.2798(3) 0.04342(15) 0.0267(7) Uani 1 1 d . . .
H6A H 0.1117 0.3149 0.0152 0.032 Uiso 1 1 calc R . .
H6B H 0.0769 0.2062 0.0313 0.032 Uiso 1 1 calc R . .
H6C H 0.1076 0.2778 0.0794 0.032 Uiso 1 1 calc R . .
C7 C 0.06415(16) 0.4781(3) 0.12716(14) 0.0250(6) Uani 1 1 d . . .
H7A H 0.0860 0.5351 0.1071 0.030 Uiso 1 1 calc R . .
H7B H 0.0930 0.4228 0.1395 0.030 Uiso 1 1 calc R . .
H7C H 0.0436 0.5087 0.1600 0.030 Uiso 1 1 calc R . .
C8 C -0.07057(16) 0.5649(2) 0.10610(15) 0.0255(7) Uani 1 1 d . . .
H8A H -0.0612 0.6284 0.0832 0.031 Uiso 1 1 calc R . .
H8B H -0.0540 0.5746 0.1439 0.031 Uiso 1 1 calc R . .
H8C H -0.1147 0.5558 0.1084 0.031 Uiso 1 1 calc R . .
C9 C -0.13121(16) 0.4234(3) 0.01066(15) 0.0278(7) Uani 1 1 d . . .
H9A H -0.1274 0.4745 -0.0205 0.033 Uiso 1 1 calc R . .
H9B H -0.1586 0.4532 0.0391 0.033 Uiso 1 1 calc R . .
H9C H -0.1477 0.3552 -0.0033 0.033 Uiso 1 1 calc R . .
C10 C -0.03549(17) 0.2440(3) -0.02764(14) 0.0283(7) Uani 1 1 d . . .
H10A H -0.0239 0.2759 -0.0637 0.034 Uiso 1 1 calc R . .
H10B H -0.0783 0.2225 -0.0289 0.034 Uiso 1 1 calc R . .
H10C H -0.0102 0.1806 -0.0203 0.034 Uiso 1 1 calc R . .
C11 C -0.0597(2) 0.2756(3) 0.31598(14) 0.0350(9) Uani 1 1 d . . .
H11A H -0.0715 0.3103 0.3513 0.042 Uiso 1 1 calc R . .
H11B H -0.0171 0.2923 0.3077 0.042 Uiso 1 1 calc R . .
H11C H -0.0646 0.1974 0.3194 0.042 Uiso 1 1 calc R . .
C12 C -0.07781(18) 0.4592(3) 0.25304(15) 0.0279(7) Uani 1 1 d . . .
H12A H -0.0904 0.5023 0.2855 0.034 Uiso 1 1 calc R . .
H12B H -0.0939 0.4917 0.2186 0.034 Uiso 1 1 calc R . .
H12C H -0.0334 0.4570 0.2512 0.034 Uiso 1 1 calc R . .
C21 C -0.21495(13) 0.0985(2) 0.09860(13) 0.0184(6) Uani 1 1 d . . .
C22 C -0.22110(13) 0.0920(2) 0.15824(13) 0.0175(5) Uani 1 1 d . . .
C23 C -0.18291(13) 0.0053(2) 0.17787(13) 0.0180(5) Uani 1 1 d . . .
C24 C -0.15412(13) -0.0413(2) 0.13006(13) 0.0187(6) Uani 1 1 d . . .
C25 C -0.17289(14) 0.0172(2) 0.08134(13) 0.0192(6) Uani 1 1 d . . .
C26 C -0.25037(16) 0.1711(3) 0.06034(14) 0.0267(7) Uani 1 1 d . . .
H26A H -0.2879 0.1349 0.0489 0.032 Uiso 1 1 calc R . .
H26B H -0.2260 0.1877 0.0270 0.032 Uiso 1 1 calc R . .
H26C H -0.2603 0.2380 0.0801 0.032 Uiso 1 1 calc R . .
C27 C -0.26452(14) 0.1548(3) 0.19400(15) 0.0241(6) Uani 1 1 d . . .
H27A H -0.3041 0.1189 0.1941 0.029 Uiso 1 1 calc R . .
H27B H -0.2689 0.2277 0.1788 0.029 Uiso 1 1 calc R . .
H27C H -0.2489 0.1588 0.2325 0.029 Uiso 1 1 calc R . .
C28 C -0.18082(16) -0.0353(3) 0.23717(14) 0.0255(7) Uani 1 1 d . . .
H28A H -0.2120 -0.0908 0.2424 0.031 Uiso 1 1 calc R . .
H28B H -0.1884 0.0245 0.2631 0.031 Uiso 1 1 calc R . .
H28C H -0.1407 -0.0663 0.2448 0.031 Uiso 1 1 calc R . .
C29 C -0.11281(16) -0.1375(3) 0.13032(17) 0.0263(7) Uani 1 1 d . . .
H29A H -0.1368 -0.2031 0.1250 0.032 Uiso 1 1 calc R . .
H29B H -0.0914 -0.1413 0.1664 0.032 Uiso 1 1 calc R . .
H29C H -0.0832 -0.1308 0.0998 0.032 Uiso 1 1 calc R . .
C30 C -0.15528(18) -0.0095(3) 0.02197(14) 0.0307(7) Uani 1 1 d . . .
H30A H -0.1847 -0.0604 0.0061 0.037 Uiso 1 1 calc R . .
H30B H -0.1147 -0.0420 0.0216 0.037 Uiso 1 1 calc R . .
H30C H -0.1549 0.0565 -0.0006 0.037 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01396(12) 0.01072(11) 0.01426(12) -0.00030(7) 0.00080(8) 0.00003(7)
S1 0.0241(4) 0.0173(3) 0.0157(3) -0.0023(3) 0.0020(3) -0.0014(3)
Cl1 0.0194(3) 0.0238(4) 0.0295(4) 0.0007(3) -0.0083(3) -0.0040(3)
C1 0.0218(14) 0.0170(13) 0.0178(13) 0.0028(11) 0.0050(11) -0.0015(11)
B1 0.0161(14) 0.0143(14) 0.0180(14) -0.0006(11) -0.0035(12) 0.0008(11)
C1S 0.026(4) 0.166(14) 0.030(4) 0.009(6) 0.010(4) -0.010(6)
Ru2 0.01297(12) 0.01083(12) 0.01442(12) -0.00054(7) -0.00083(8) -0.00016(7)
C2 0.0227(14) 0.0145(13) 0.0201(14) 0.0012(11) 0.0034(11) -0.0037(11)
Cl2 0.0175(3) 0.0159(3) 0.0266(4) 0.0002(3) 0.0012(3) 0.0041(2)
B2 0.0176(14) 0.0131(14) 0.0140(13) -0.0016(11) -0.0005(11) 0.0001(11)
C2S 0.031(4) 0.150(11) 0.008(3) -0.027(5) -0.010(3) 0.019(6)
Cl3 0.0220(3) 0.0171(3) 0.0254(3) -0.0025(3) 0.0035(3) 0.0041(3)
B3 0.0165(14) 0.0149(14) 0.0186(15) -0.0004(12) -0.0015(12) -0.0003(11)
C3 0.0253(15) 0.0133(13) 0.0182(13) 0.0028(11) 0.0038(11) -0.0008(11)
C3S 0.028(4) 0.188(15) 0.010(3) -0.024(5) -0.002(3) -0.002(6)
C4 0.0240(15) 0.0181(14) 0.0179(13) 0.0054(11) 0.0019(11) 0.0005(11)
B4 0.0174(15) 0.0141(15) 0.0171(15) -0.0002(11) -0.0003(11) 0.0007(11)
C4S 0.057(6) 0.122(11) 0.018(4) 0.007(5) -0.021(4) -0.007(7)
B5 0.0158(14) 0.0149(14) 0.0177(14) -0.0012(11) -0.0003(12) 0.0006(11)
C5 0.0247(14) 0.0190(14) 0.0131(12) -0.0003(11) 0.0048(11) -0.0028(12)
C5S 0.057(7) 0.128(12) 0.022(4) 0.007(5) 0.015(4) 0.001(7)
C6 0.0226(15) 0.0251(16) 0.0323(17) 0.0008(13) 0.0094(13) 0.0041(13)
C7 0.0284(16) 0.0206(15) 0.0260(15) -0.0004(12) -0.0001(13) -0.0093(13)
C8 0.0317(17) 0.0125(13) 0.0323(17) 0.0011(12) 0.0108(14) 0.0011(12)
C9 0.0280(16) 0.0297(17) 0.0258(16) 0.0087(13) -0.0051(13) 0.0013(13)
C10 0.0391(19) 0.0284(17) 0.0175(14) -0.0051(13) 0.0030(13) -0.0088(15)
C11 0.061(3) 0.0292(18) 0.0143(14) 0.0016(13) -0.0071(15) 0.0084(17)
C12 0.0415(19) 0.0183(14) 0.0241(15) -0.0032(12) -0.0030(14) -0.0055(14)
C21 0.0157(13) 0.0171(13) 0.0223(14) 0.0003(11) -0.0022(11) -0.0029(11)
C22 0.0128(12) 0.0167(13) 0.0230(14) -0.0015(11) -0.0003(10) -0.0030(10)
C23 0.0157(13) 0.0151(13) 0.0231(14) 0.0015(11) -0.0011(11) -0.0039(10)
C24 0.0159(13) 0.0145(13) 0.0256(15) -0.0028(11) -0.0013(11) -0.0023(10)
C25 0.0182(13) 0.0169(13) 0.0225(14) -0.0053(11) -0.0030(11) -0.0049(11)
C26 0.0243(15) 0.0264(16) 0.0294(16) 0.0051(13) -0.0087(13) -0.0012(13)
C27 0.0196(14) 0.0228(15) 0.0299(16) -0.0025(13) 0.0041(12) -0.0003(12)
C28 0.0261(16) 0.0257(16) 0.0246(16) 0.0063(13) -0.0001(13) -0.0047(13)
C29 0.0220(15) 0.0142(14) 0.0427(19) -0.0018(13) 0.0007(14) 0.0013(12)
C30 0.040(2) 0.0313(18) 0.0210(15) -0.0093(13) 0.0012(14) -0.0060(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100851.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100851.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100851
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C22 H38 B5 Cl3 Ru2 S'
_chemical_formula_weight 697.12
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 91.4140(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.4861(4)
_cell_length_b 20.9284(10)
_cell_length_c 15.9540(7)
_cell_measurement_reflns_used 7914
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.31
_cell_measurement_theta_min 2.33
_cell_volume 2832.6(2)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0223
_diffrn_reflns_av_sigmaI/netI 0.0184
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 30747
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 1.61
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.434
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7441
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.635
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rod
_exptl_crystal_F_000 1400
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 336
_refine_ls_number_reflns 7044
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0217
_refine_ls_R_factor_gt 0.0203
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+2.2221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0478
_refine_ls_wR_factor_ref 0.0484
_reflns_number_gt 6743
_reflns_number_total 7044
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100851
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.569374(14) 0.080244(6) 0.777240(8) 0.00928(4) Uani 1 1 d . . .
S1 S 0.63738(5) 0.05897(2) 0.54063(3) 0.01572(8) Uani 1 1 d . . .
C1 C 0.7274(2) 0.00581(8) 0.83643(10) 0.0152(3) Uani 1 1 d . . .
B1 B 0.7391(2) 0.12166(9) 0.70691(11) 0.0125(3) Uani 1 1 d . . .
H1 H 0.8626 0.1163 0.6989 0.024(6) Uiso 1 1 d R . .
Cl1 Cl 0.24906(5) 0.01400(2) 0.65635(3) 0.01917(9) Uani 1 1 d . . .
Ru2 Ru 0.587124(14) 0.197618(6) 0.695230(8) 0.00921(4) Uani 1 1 d . . .
B2 B 0.5706(2) 0.10018(9) 0.64043(11) 0.0121(3) Uani 1 1 d . . .
C2 C 0.5685(2) -0.01765(8) 0.82961(11) 0.0153(3) Uani 1 1 d . . .
Cl2 Cl 0.28215(5) 0.16951(2) 0.54035(2) 0.01766(8) Uani 1 1 d . . .
C3 C 0.47251(19) 0.02224(8) 0.88074(10) 0.0138(3) Uani 1 1 d . . .
B3 B 0.3905(2) 0.07679(9) 0.68275(11) 0.0128(3) Uani 1 1 d . . .
Cl3 Cl 0.21104(5) 0.17481(2) 0.80013(3) 0.01704(8) Uani 1 1 d . . .
C4 C 0.57097(19) 0.07107(8) 0.91645(10) 0.0136(3) Uani 1 1 d . . .
B4 B 0.4019(2) 0.14802(9) 0.63188(11) 0.0128(3) Uani 1 1 d . . .
B5 B 0.3728(2) 0.14645(9) 0.73839(11) 0.0122(3) Uani 1 1 d . . .
H2 H 0.5185 0.1612 0.7841 0.046(8) Uiso 1 1 d R . .
C5 C 0.72884(19) 0.06031(8) 0.88964(10) 0.0141(3) Uani 1 1 d . . .
C6 C 0.8710(2) -0.02598(10) 0.80248(13) 0.0248(4) Uani 1 1 d . . .
H6A H 0.8353 -0.0539 0.7590 0.045(8) Uiso 1 1 d R . .
H6B H 0.9288 -0.0479 0.8464 0.055(9) Uiso 1 1 d R . .
H6C H 0.9407 0.0067 0.7836 0.042(7) Uiso 1 1 d R . .
C7 C 0.5171(3) -0.07751(8) 0.78521(13) 0.0237(4) Uani 1 1 d . . .
H7A H 0.5483 -0.1130 0.8115 0.053(8) Uiso 1 1 d R . .
H7B H 0.4087 -0.0767 0.7782 0.046(8) Uiso 1 1 d R . .
H7C H 0.5651 -0.0828 0.7443 0.060(10) Uiso 1 1 d R . .
C8 C 0.2999(2) 0.01396(9) 0.89509(12) 0.0215(4) Uani 1 1 d . . .
H8A H 0.2571 0.0527 0.8992 0.030(6) Uiso 1 1 d R . .
H8B H 0.2884 -0.0065 0.9436 0.036(7) Uiso 1 1 d R . .
H8C H 0.2435 -0.0069 0.8444 0.046(8) Uiso 1 1 d R . .
C9 C 0.5193(2) 0.12177(9) 0.97637(11) 0.0210(4) Uani 1 1 d . . .
H9A H 0.4236 0.1373 0.9603 0.026(6) Uiso 1 1 d R . .
H9B H 0.5943 0.1549 0.9727 0.040(7) Uiso 1 1 d R . .
H9C H 0.5331 0.1066 1.0333 0.040(7) Uiso 1 1 d R . .
C10 C 0.8727(2) 0.09636(9) 0.91800(12) 0.0216(4) Uani 1 1 d . . .
H10A H 0.9531 0.0987 0.8773 0.023(6) Uiso 1 1 d R . .
H10B H 0.8567 0.1386 0.9336 0.027(6) Uiso 1 1 d R . .
H10C H 0.9248 0.0793 0.9620 0.041(7) Uiso 1 1 d R . .
C21 C 0.5849(2) 0.29467(8) 0.75438(11) 0.0143(3) Uani 1 1 d . . .
C22 C 0.5222(2) 0.29910(7) 0.67075(11) 0.0143(3) Uani 1 1 d . . .
C23 C 0.64294(19) 0.28036(8) 0.61459(10) 0.0136(3) Uani 1 1 d . . .
C24 C 0.78212(19) 0.26542(8) 0.66402(10) 0.0122(3) Uani 1 1 d . . .
C25 C 0.74592(19) 0.27435(8) 0.75024(10) 0.0132(3) Uani 1 1 d . . .
C26 C 0.5012(2) 0.31367(9) 0.83226(12) 0.0218(4) Uani 1 1 d . . .
H26A H 0.5479 0.2948 0.8784 0.037(7) Uiso 1 1 d R . .
H26B H 0.3968 0.3081 0.8285 0.037(7) Uiso 1 1 d R . .
H26C H 0.5044 0.3591 0.8365 0.045(8) Uiso 1 1 d R . .
C27 C 0.3603(2) 0.32201(9) 0.64616(12) 0.0205(4) Uani 1 1 d . . .
H27A H 0.2919 0.3145 0.6866 0.030(6) Uiso 1 1 d R . .
H27B H 0.3269 0.3020 0.5954 0.028(6) Uiso 1 1 d R . .
H27C H 0.3580 0.3641 0.6374 0.035(7) Uiso 1 1 d R . .
C28 C 0.6302(2) 0.28410(9) 0.52068(11) 0.0189(3) Uani 1 1 d . . .
H28A H 0.5408 0.2685 0.4983 0.023(6) Uiso 1 1 d R . .
H28B H 0.7215 0.2645 0.4933 0.030(6) Uiso 1 1 d R . .
H28C H 0.6356 0.3277 0.5042 0.036(7) Uiso 1 1 d R . .
C29 C 0.94063(19) 0.24922(8) 0.63099(11) 0.0152(3) Uani 1 1 d . . .
H29A H 0.9939 0.2208 0.6618 0.034(7) Uiso 1 1 d R . .
H29B H 0.9406 0.2301 0.5782 0.031(6) Uiso 1 1 d R . .
H29C H 0.9990 0.2875 0.6241 0.026(6) Uiso 1 1 d R . .
C30 C 0.8581(2) 0.26778(9) 0.82337(11) 0.0189(3) Uani 1 1 d . . .
H30A H 0.8029 0.2584 0.8767 0.040(7) Uiso 1 1 d R . .
H30B H 0.9082 0.3044 0.8350 0.040(7) Uiso 1 1 d R . .
H30C H 0.9410 0.2387 0.8167 0.049(8) Uiso 1 1 d R . .
C31 C 0.7955(3) 0.10663(12) 0.50230(15) 0.0467(7) Uani 1 1 d . . .
H31A H 0.8379 0.0893 0.4571 0.047(8) Uiso 1 1 d R . .
H31B H 0.8722 0.1118 0.5430 0.055(9) Uiso 1 1 d R . .
H31C H 0.7637 0.1505 0.4936 0.069(10) Uiso 1 1 d R . .
C32 C 0.7422(3) -0.01071(10) 0.57553(13) 0.0317(5) Uani 1 1 d . . .
H32A H 0.7673 -0.0318 0.5266 0.036(7) Uiso 1 1 d R . .
H32B H 0.8159 0.0025 0.6152 0.037(7) Uiso 1 1 d R . .
H32C H 0.6719 -0.0367 0.6071 0.057(9) Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.00982(6) 0.00899(6) 0.00908(6) 0.00068(4) 0.00115(4) 0.00023(4)
S1 0.0206(2) 0.01486(19) 0.01191(18) -0.00257(15) 0.00487(15) -0.00273(15)
C1 0.0161(8) 0.0151(8) 0.0145(8) 0.0050(6) 0.0020(6) 0.0041(6)
B1 0.0133(8) 0.0114(8) 0.0130(8) 0.0004(6) 0.0024(6) 0.0004(6)
Cl1 0.0211(2) 0.0200(2) 0.01649(19) -0.00233(15) 0.00008(15) -0.00968(16)
Ru2 0.00954(6) 0.00911(6) 0.00901(6) 0.00068(4) 0.00081(4) 0.00010(4)
B2 0.0130(8) 0.0134(8) 0.0099(8) -0.0003(6) 0.0027(6) -0.0004(6)
C2 0.0199(8) 0.0109(7) 0.0151(8) 0.0033(6) -0.0001(6) 0.0001(6)
Cl2 0.01782(19) 0.0229(2) 0.01208(18) 0.00290(15) -0.00373(14) -0.00025(15)
C3 0.0148(8) 0.0139(8) 0.0129(7) 0.0063(6) 0.0012(6) 0.0009(6)
B3 0.0133(8) 0.0136(8) 0.0117(8) -0.0013(6) 0.0017(6) -0.0029(6)
Cl3 0.01305(18) 0.0222(2) 0.01606(18) 0.00189(15) 0.00393(14) 0.00467(15)
C4 0.0151(8) 0.0152(8) 0.0104(7) 0.0038(6) -0.0003(6) 0.0026(6)
B4 0.0125(8) 0.0147(8) 0.0113(8) 0.0019(6) 0.0008(6) 0.0007(6)
B5 0.0105(8) 0.0147(8) 0.0114(8) -0.0003(6) 0.0022(6) 0.0006(6)
C5 0.0140(8) 0.0157(8) 0.0127(7) 0.0053(6) -0.0007(6) 0.0015(6)
C6 0.0225(9) 0.0254(10) 0.0269(10) 0.0043(8) 0.0061(8) 0.0122(8)
C7 0.0348(11) 0.0124(8) 0.0239(10) 0.0008(7) 0.0006(8) -0.0021(7)
C8 0.0144(8) 0.0274(10) 0.0231(9) 0.0124(7) 0.0036(7) -0.0012(7)
C9 0.0290(10) 0.0217(9) 0.0124(8) -0.0008(7) 0.0021(7) 0.0077(7)
C10 0.0179(8) 0.0256(10) 0.0210(9) 0.0056(7) -0.0064(7) -0.0049(7)
C21 0.0156(8) 0.0105(7) 0.0170(8) -0.0022(6) 0.0023(6) -0.0001(6)
C22 0.0141(8) 0.0086(7) 0.0201(8) 0.0021(6) 0.0005(6) 0.0007(6)
C23 0.0141(8) 0.0109(7) 0.0159(8) 0.0036(6) 0.0009(6) -0.0018(6)
C24 0.0119(7) 0.0099(7) 0.0149(8) 0.0013(6) 0.0008(6) -0.0018(6)
C25 0.0142(7) 0.0099(7) 0.0154(8) -0.0003(6) 0.0001(6) -0.0020(6)
C26 0.0234(9) 0.0192(9) 0.0232(9) -0.0052(7) 0.0075(7) 0.0011(7)
C27 0.0149(8) 0.0160(8) 0.0304(10) 0.0035(7) 0.0001(7) 0.0038(6)
C28 0.0173(8) 0.0224(9) 0.0170(8) 0.0066(7) -0.0016(6) -0.0011(7)
C29 0.0129(7) 0.0148(8) 0.0178(8) 0.0016(6) 0.0021(6) -0.0010(6)
C30 0.0202(9) 0.0201(9) 0.0163(8) -0.0013(7) -0.0036(7) -0.0023(7)
C31 0.0660(17) 0.0421(14) 0.0339(13) -0.0202(11) 0.0358(12) -0.0334(13)
C32 0.0470(13) 0.0270(11) 0.0210(10) -0.0072(8) -0.0021(9) 0.0175(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100852.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100852.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100852
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C20 H33 B6 Cl3 Ru2'
_chemical_formula_weight 646.81
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 111.4440(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.0660(5)
_cell_length_b 32.7224(17)
_cell_length_c 9.1682(5)
_cell_measurement_reflns_used 6869
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.29
_cell_measurement_theta_min 2.47
_cell_volume 2531.6(2)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0410
_diffrn_reflns_av_sigmaI/netI 0.0345
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 43
_diffrn_reflns_limit_k_min -42
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 27077
_diffrn_reflns_theta_max 28.31
_diffrn_reflns_theta_min 2.41
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.518
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9289
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.697
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1288
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.122
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 280
_refine_ls_number_reflns 6285
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.122
_refine_ls_R_factor_all 0.0510
_refine_ls_R_factor_gt 0.0436
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+8.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1052
_refine_ls_wR_factor_ref 0.1086
_reflns_number_gt 5586
_reflns_number_total 6285
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100852
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.27105(4) 0.090719(9) 0.17322(4) 0.01705(9) Uani 1 1 d . . .
Cl1 Cl 0.00360(14) 0.17492(4) 0.07090(15) 0.0340(3) Uani 1 1 d . . .
B1 B 0.1868(6) 0.14973(15) 0.1638(6) 0.0226(9) Uani 1 1 d . . .
C1 C 0.0661(5) 0.06464(13) -0.0249(5) 0.0241(8) Uani 1 1 d . . .
Ru2 Ru 0.39345(4) 0.156446(9) 0.35890(4) 0.01768(9) Uani 1 1 d . . .
Cl2 Cl 0.71344(16) 0.17843(4) 0.23305(16) 0.0414(3) Uani 1 1 d . . .
B2 B 0.3508(6) 0.15018(14) 0.0975(5) 0.0207(9) Uani 1 1 d . . .
H1 H 0.2971 0.1730 -0.0049 0.025 Uiso 1 1 d R . .
C2 C 0.0202(5) 0.06405(13) 0.1097(5) 0.0242(9) Uani 1 1 d . . .
Cl3 Cl 0.69329(14) 0.07172(4) 0.43528(13) 0.0322(2) Uani 1 1 d . . .
C3 C 0.1310(5) 0.03837(12) 0.2253(5) 0.0230(8) Uani 1 1 d . . .
B3 B 0.5451(6) 0.14901(15) 0.2288(5) 0.0207(9) Uani 1 1 d . . .
C4 C 0.2421(5) 0.02269(13) 0.1602(5) 0.0220(8) Uani 1 1 d . . .
B4 B 0.4688(6) 0.10719(14) 0.1124(5) 0.0206(9) Uani 1 1 d . . .
H2 H 0.5344 0.0857 -0.0070 0.025 Uiso 1 1 d R . .
B5 B 0.5282(5) 0.10282(14) 0.3137(5) 0.0201(9) Uani 1 1 d . . .
C5 C 0.1998(5) 0.03860(13) 0.0052(5) 0.0231(8) Uani 1 1 d . . .
B6 B 0.3793(6) 0.09600(15) 0.4081(5) 0.0217(9) Uani 1 1 d . . .
H3 H 0.3925 0.0782 0.5307 0.026 Uiso 1 1 d R . .
C6 C -0.0251(6) 0.08557(15) -0.1788(5) 0.0323(10) Uani 1 1 d . . .
H6A H -0.0586 0.1098 -0.1493 0.039 Uiso 1 1 d R . .
H6B H 0.0378 0.0892 -0.2378 0.039 Uiso 1 1 d R . .
H6C H -0.1011 0.0653 -0.2465 0.039 Uiso 1 1 d R . .
C7 C -0.1238(6) 0.08283(14) 0.1226(7) 0.0326(10) Uani 1 1 d . . .
H7A H -0.0891 0.0923 0.2429 0.039 Uiso 1 1 d R . .
H7B H -0.1940 0.0661 0.1012 0.039 Uiso 1 1 d R . .
H7C H -0.1665 0.1031 0.0491 0.039 Uiso 1 1 d R . .
C8 C 0.1174(6) 0.02625(14) 0.3776(6) 0.0297(10) Uani 1 1 d . . .
H8A H 0.2004 0.0197 0.4443 0.036 Uiso 1 1 d R . .
H8B H 0.0486 0.0068 0.3410 0.036 Uiso 1 1 d R . .
H8C H 0.0761 0.0480 0.4189 0.036 Uiso 1 1 d R . .
C9 C 0.3744(5) -0.00675(14) 0.2381(5) 0.0275(9) Uani 1 1 d . . .
H9A H 0.4746 0.0045 0.2369 0.033 Uiso 1 1 d R . .
H9B H 0.3823 -0.0112 0.3360 0.033 Uiso 1 1 d R . .
H9C H 0.3475 -0.0357 0.2088 0.033 Uiso 1 1 d R . .
C10 C 0.2763(6) 0.02774(15) -0.1092(5) 0.0301(10) Uani 1 1 d . . .
H10A H 0.3781 0.0256 -0.0555 0.036 Uiso 1 1 d R . .
H10B H 0.2394 0.0056 -0.1679 0.036 Uiso 1 1 d R . .
H10C H 0.2920 0.0486 -0.1565 0.036 Uiso 1 1 d R . .
C21 C 0.5517(5) 0.19397(14) 0.5589(5) 0.0269(9) Uani 1 1 d . . .
C22 C 0.4651(6) 0.16665(13) 0.6182(5) 0.0281(10) Uani 1 1 d . . .
C23 C 0.3019(6) 0.17658(13) 0.5477(5) 0.0258(9) Uani 1 1 d . . .
C24 C 0.2870(5) 0.21042(13) 0.4438(5) 0.0250(9) Uani 1 1 d . . .
C25 C 0.4423(5) 0.22065(13) 0.4502(5) 0.0252(9) Uani 1 1 d . . .
C26 C 0.7300(6) 0.19648(19) 0.6149(6) 0.0422(13) Uani 1 1 d . . .
H26A H 0.7666 0.2128 0.5354 0.051 Uiso 1 1 d R . .
H26B H 0.7715 0.1736 0.6217 0.051 Uiso 1 1 d R . .
H26C H 0.7640 0.2135 0.6994 0.051 Uiso 1 1 d R . .
C27 C 0.5392(8) 0.13697(16) 0.7495(6) 0.0417(13) Uani 1 1 d . . .
H27A H 0.4648 0.1186 0.7590 0.050 Uiso 1 1 d R . .
H27B H 0.5745 0.1531 0.8464 0.050 Uiso 1 1 d R . .
H27C H 0.6329 0.1222 0.7442 0.050 Uiso 1 1 d R . .
C28 C 0.1678(7) 0.15772(16) 0.5845(7) 0.0403(13) Uani 1 1 d . . .
H28A H 0.0824 0.1560 0.4938 0.048 Uiso 1 1 d R . .
H28B H 0.1809 0.1294 0.5944 0.048 Uiso 1 1 d R . .
H28C H 0.1635 0.1692 0.6741 0.048 Uiso 1 1 d R . .
C29 C 0.1420(6) 0.23574(17) 0.3662(7) 0.0405(12) Uani 1 1 d . . .
H29A H 0.0606 0.2233 0.3722 0.049 Uiso 1 1 d R . .
H29B H 0.1461 0.2435 0.2582 0.049 Uiso 1 1 d R . .
H29C H 0.1260 0.2574 0.4246 0.049 Uiso 1 1 d R . .
C30 C 0.4844(7) 0.25581(15) 0.3677(6) 0.0369(11) Uani 1 1 d . . .
H30A H 0.5652 0.2533 0.3315 0.044 Uiso 1 1 d R . .
H30B H 0.3854 0.2594 0.2767 0.044 Uiso 1 1 d R . .
H30C H 0.5036 0.2811 0.4356 0.044 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01903(16) 0.01618(15) 0.01680(16) 0.00174(11) 0.00756(12) 0.00086(11)
Cl1 0.0287(6) 0.0293(6) 0.0382(6) 0.0021(5) 0.0053(5) 0.0050(4)
B1 0.020(2) 0.023(2) 0.023(2) 0.0013(18) 0.0056(18) 0.0000(17)
C1 0.022(2) 0.024(2) 0.024(2) -0.0001(16) 0.0061(17) -0.0016(16)
Ru2 0.02123(16) 0.01678(16) 0.01551(15) 0.00174(11) 0.00727(12) 0.00062(12)
Cl2 0.0378(7) 0.0443(7) 0.0446(7) -0.0004(6) 0.0181(6) -0.0046(5)
B2 0.024(2) 0.019(2) 0.019(2) -0.0004(16) 0.0072(18) -0.0027(17)
C2 0.022(2) 0.022(2) 0.029(2) -0.0010(17) 0.0095(17) -0.0015(16)
Cl3 0.0289(6) 0.0374(6) 0.0269(5) 0.0067(5) 0.0060(4) 0.0084(5)
C3 0.025(2) 0.0171(19) 0.027(2) 0.0035(16) 0.0098(17) -0.0005(15)
B3 0.020(2) 0.023(2) 0.019(2) 0.0006(17) 0.0074(18) -0.0012(17)
C4 0.022(2) 0.0210(19) 0.025(2) -0.0009(16) 0.0112(17) 0.0004(15)
B4 0.022(2) 0.024(2) 0.015(2) 0.0005(17) 0.0066(17) -0.0029(18)
B5 0.019(2) 0.022(2) 0.019(2) 0.0023(17) 0.0052(17) 0.0029(17)
C5 0.025(2) 0.021(2) 0.022(2) -0.0023(16) 0.0077(17) -0.0020(16)
B6 0.026(2) 0.022(2) 0.019(2) 0.0022(17) 0.0106(18) 0.0022(18)
C6 0.032(2) 0.034(3) 0.025(2) 0.0017(19) 0.0030(19) 0.003(2)
C7 0.026(2) 0.026(2) 0.050(3) 0.005(2) 0.019(2) -0.0007(18)
C8 0.034(2) 0.029(2) 0.030(2) 0.0021(18) 0.015(2) -0.0025(19)
C9 0.030(2) 0.024(2) 0.030(2) 0.0043(18) 0.0132(19) 0.0048(18)
C10 0.038(3) 0.030(2) 0.026(2) -0.0028(18) 0.015(2) -0.001(2)
C21 0.028(2) 0.026(2) 0.022(2) -0.0030(17) 0.0045(17) 0.0019(17)
C22 0.045(3) 0.021(2) 0.019(2) 0.0002(16) 0.0128(19) 0.0048(19)
C23 0.037(2) 0.023(2) 0.021(2) -0.0039(16) 0.0148(19) -0.0023(18)
C24 0.029(2) 0.021(2) 0.024(2) -0.0057(16) 0.0092(18) 0.0010(17)
C25 0.033(2) 0.022(2) 0.020(2) -0.0026(16) 0.0096(18) -0.0049(17)
C26 0.032(3) 0.054(3) 0.035(3) -0.011(2) 0.006(2) -0.001(2)
C27 0.068(4) 0.032(3) 0.021(2) 0.0040(19) 0.013(2) 0.009(3)
C28 0.055(3) 0.035(3) 0.046(3) -0.011(2) 0.036(3) -0.010(2)
C29 0.036(3) 0.037(3) 0.042(3) -0.008(2) 0.006(2) 0.011(2)
C30 0.051(3) 0.027(2) 0.038(3) 0.000(2) 0.023(2) -0.007(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100853.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100853.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100853
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C21 H42 B6 Cl4 Ru2'
_chemical_formula_weight 703.35
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens 'geom, except difmap for M-H and B-H'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 94.3710(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.5799(9)
_cell_length_b 11.3893(7)
_cell_length_c 17.7889(11)
_cell_measurement_reflns_used 5492
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.35
_cell_measurement_theta_min 2.27
_cell_volume 2945.3(3)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0419
_diffrn_reflns_av_sigmaI/netI 0.0336
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 24378
_diffrn_reflns_theta_max 25.37
_diffrn_reflns_theta_min 2.13
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.399
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8166
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details SADABS
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.586
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rod
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_hydrogen_treatment riding
_refine_ls_matrix_type full
_refine_ls_number_parameters 298
_refine_ls_number_reflns 5399
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.027
_refine_ls_R_factor_all 0.0437
_refine_ls_R_factor_gt 0.0323
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+7.3090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0736
_refine_ls_wR_factor_ref 0.0786
_reflns_number_gt 4509
_reflns_number_total 5399
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100853
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.66121(2) 0.63291(3) 0.030202(17) 0.01657(9) Uani 1 1 d . . .
Cl1 Cl 0.77241(6) 0.70341(8) -0.13582(5) 0.0222(2) Uani 1 1 d . . .
Cl1S Cl 0.97043(10) 0.39670(10) -0.41467(8) 0.0504(3) Uani 1 1 d . . .
C1 C 0.7598(3) 0.7787(3) 0.0643(2) 0.0203(8) Uani 1 1 d . . .
C1S C 0.9730(3) 0.2449(4) -0.3969(2) 0.0289(10) Uani 1 1 d . . .
H1SA H 1.0376 0.2174 -0.3930 0.035 Uiso 1 1 calc R . .
H1SB H 0.9398 0.2033 -0.4396 0.035 Uiso 1 1 calc R . .
B1 B 0.5862(3) 0.6446(4) -0.0824(3) 0.0223(9) Uani 1 1 d . . .
H2 H 0.5437 0.7621 -0.0995 0.027 Uiso 1 1 d R . .
H1 H 0.5633 0.6132 -0.0146 0.027 Uiso 1 1 d R . .
Ru2 Ru 0.70892(2) 0.40041(3) -0.131263(17) 0.01695(9) Uani 1 1 d . . .
Cl2 Cl 0.88274(6) 0.51792(8) -0.00193(5) 0.0219(2) Uani 1 1 d . . .
Cl2S Cl 0.92182(8) 0.21026(10) -0.31282(7) 0.0386(3) Uani 1 1 d . . .
B2 B 0.6068(3) 0.5437(4) -0.1528(3) 0.0233(10) Uani 1 1 d . . .
H4 H 0.5681 0.5668 -0.2226 0.028 Uiso 1 1 d R . .
H5 H 0.6015 0.4248 -0.1475 0.028 Uiso 1 1 d R . .
H3 H 0.5388 0.5615 -0.1156 0.028 Uiso 1 1 d R . .
C2 C 0.7507(3) 0.7039(3) 0.1278(2) 0.0203(8) Uani 1 1 d . . .
C3 C 0.6561(3) 0.7084(3) 0.1462(2) 0.0189(8) Uani 1 1 d . . .
B3 B 0.7001(3) 0.5924(4) -0.0902(2) 0.0190(9) Uani 1 1 d . . .
C4 C 0.6079(3) 0.7850(3) 0.0934(2) 0.0208(8) Uani 1 1 d . . .
B4 B 0.7562(3) 0.4980(4) -0.0219(2) 0.0186(9) Uani 1 1 d . . .
B5 B 0.7014(3) 0.4505(4) 0.0591(3) 0.0224(9) Uani 1 1 d . . .
H9 H 0.7370 0.4271 0.1275 0.027 Uiso 1 1 d R . .
H10 H 0.6317 0.5170 0.0692 0.027 Uiso 1 1 d R . .
C5 C 0.6721(3) 0.8276(3) 0.0424(2) 0.0208(8) Uani 1 1 d . . .
B6 B 0.7224(3) 0.3487(4) -0.0105(3) 0.0243(10) Uani 1 1 d . . .
H7 H 0.7545 0.2473 0.0209 0.029 Uiso 1 1 d R . .
H8 H 0.6633 0.3501 0.0348 0.029 Uiso 1 1 d R . .
H6 H 0.6639 0.3218 -0.0666 0.029 Uiso 1 1 d R . .
C6 C 0.8488(3) 0.8150(4) 0.0346(2) 0.0262(9) Uani 1 1 d . . .
H6A H 0.8737 0.8830 0.0631 0.031 Uiso 1 1 calc R . .
H6B H 0.8383 0.8359 -0.0188 0.031 Uiso 1 1 calc R . .
H6C H 0.8927 0.7499 0.0401 0.031 Uiso 1 1 calc R . .
C7 C 0.8282(3) 0.6468(4) 0.1743(2) 0.0251(9) Uani 1 1 d . . .
H7A H 0.8536 0.7023 0.2126 0.030 Uiso 1 1 calc R . .
H7B H 0.8763 0.6237 0.1417 0.030 Uiso 1 1 calc R . .
H7C H 0.8053 0.5771 0.1992 0.030 Uiso 1 1 calc R . .
C8 C 0.6175(3) 0.6486(4) 0.2116(2) 0.0243(9) Uani 1 1 d . . .
H8A H 0.6238 0.7002 0.2558 0.029 Uiso 1 1 calc R . .
H8B H 0.6510 0.5753 0.2228 0.029 Uiso 1 1 calc R . .
H8C H 0.5523 0.6311 0.1992 0.029 Uiso 1 1 calc R . .
C9 C 0.5101(3) 0.8259(4) 0.0948(2) 0.0266(9) Uani 1 1 d . . .
H9A H 0.5078 0.8947 0.1276 0.032 Uiso 1 1 calc R . .
H9B H 0.4727 0.7628 0.1140 0.032 Uiso 1 1 calc R . .
H9C H 0.4861 0.8468 0.0436 0.032 Uiso 1 1 calc R . .
C10 C 0.6524(3) 0.9195(4) -0.0174(2) 0.0287(9) Uani 1 1 d . . .
H10A H 0.6635 0.9976 0.0045 0.034 Uiso 1 1 calc R . .
H10B H 0.5880 0.9134 -0.0373 0.034 Uiso 1 1 calc R . .
H10C H 0.6927 0.9073 -0.0583 0.034 Uiso 1 1 calc R . .
C21 C 0.8345(3) 0.4048(3) -0.1977(2) 0.0211(8) Uani 1 1 d . . .
C22 C 0.7544(3) 0.4105(3) -0.2480(2) 0.0225(8) Uani 1 1 d . . .
C23 C 0.7032(3) 0.3035(3) -0.2406(2) 0.0220(8) Uani 1 1 d . . .
C24 C 0.7522(3) 0.2339(3) -0.1849(2) 0.0236(9) Uani 1 1 d . . .
C25 C 0.8330(3) 0.2965(3) -0.1575(2) 0.0213(8) Uani 1 1 d . . .
C26 C 0.9144(3) 0.4877(4) -0.1956(2) 0.0287(10) Uani 1 1 d . . .
H26A H 0.9571 0.4628 -0.2324 0.034 Uiso 1 1 calc R . .
H26B H 0.9461 0.4875 -0.1450 0.034 Uiso 1 1 calc R . .
H26C H 0.8921 0.5671 -0.2080 0.034 Uiso 1 1 calc R . .
C27 C 0.7349(3) 0.5020(4) -0.3076(2) 0.0346(11) Uani 1 1 d . . .
H27A H 0.7648 0.4800 -0.3531 0.042 Uiso 1 1 calc R . .
H27B H 0.7589 0.5780 -0.2891 0.042 Uiso 1 1 calc R . .
H27C H 0.6684 0.5080 -0.3196 0.042 Uiso 1 1 calc R . .
C28 C 0.6185(3) 0.2689(5) -0.2883(3) 0.0365(11) Uani 1 1 d . . .
H28A H 0.6361 0.2269 -0.3331 0.044 Uiso 1 1 calc R . .
H28B H 0.5835 0.3394 -0.3039 0.044 Uiso 1 1 calc R . .
H28C H 0.5804 0.2176 -0.2592 0.044 Uiso 1 1 calc R . .
C29 C 0.7294(3) 0.1114(4) -0.1616(3) 0.0339(11) Uani 1 1 d . . .
H29A H 0.7570 0.0549 -0.1948 0.041 Uiso 1 1 calc R . .
H29B H 0.6625 0.1010 -0.1652 0.041 Uiso 1 1 calc R . .
H29C H 0.7539 0.0981 -0.1094 0.041 Uiso 1 1 calc R . .
C30 C 0.9109(3) 0.2485(4) -0.1067(2) 0.0298(10) Uani 1 1 d . . .
H30A H 0.9542 0.2072 -0.1369 0.036 Uiso 1 1 calc R . .
H30B H 0.8867 0.1936 -0.0706 0.036 Uiso 1 1 calc R . .
H30C H 0.9428 0.3131 -0.0793 0.036 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01601(15) 0.01522(15) 0.01896(16) -0.00081(12) 0.00437(12) -0.00144(11)
Cl1 0.0249(5) 0.0186(5) 0.0238(5) 0.0035(4) 0.0065(4) -0.0008(4)
Cl1S 0.0714(9) 0.0265(6) 0.0572(8) 0.0039(5) 0.0293(7) 0.0120(6)
C1 0.022(2) 0.0165(19) 0.023(2) -0.0050(16) 0.0059(16) -0.0037(15)
C1S 0.035(2) 0.026(2) 0.028(2) -0.0025(18) 0.0111(19) 0.0064(18)
B1 0.019(2) 0.024(2) 0.025(2) -0.0040(19) 0.0021(18) -0.0015(18)
Ru2 0.01734(16) 0.01584(16) 0.01814(16) -0.00080(12) 0.00440(12) -0.00140(11)
Cl2 0.0185(5) 0.0221(5) 0.0249(5) -0.0027(4) 0.0013(4) 0.0017(4)
Cl2S 0.0463(7) 0.0364(6) 0.0356(6) -0.0009(5) 0.0201(5) 0.0078(5)
B2 0.020(2) 0.026(2) 0.025(2) -0.0019(19) 0.0036(18) 0.0012(18)
C2 0.0204(19) 0.018(2) 0.023(2) -0.0070(16) 0.0028(16) -0.0011(15)
C3 0.0211(19) 0.0170(19) 0.019(2) -0.0058(15) 0.0035(15) -0.0019(15)
B3 0.022(2) 0.017(2) 0.019(2) 0.0010(17) 0.0065(17) 0.0000(17)
C4 0.023(2) 0.0141(18) 0.026(2) -0.0034(16) 0.0056(17) -0.0007(15)
B4 0.016(2) 0.018(2) 0.022(2) 0.0005(17) 0.0032(17) -0.0005(16)
B5 0.028(2) 0.014(2) 0.026(2) -0.0017(18) 0.0080(19) -0.0034(18)
C5 0.024(2) 0.0136(18) 0.026(2) -0.0032(16) 0.0072(16) -0.0035(15)
B6 0.033(3) 0.020(2) 0.021(2) 0.0005(18) 0.008(2) -0.0071(19)
C6 0.025(2) 0.023(2) 0.032(2) -0.0040(18) 0.0092(18) -0.0028(17)
C7 0.021(2) 0.029(2) 0.025(2) -0.0037(17) -0.0002(17) 0.0004(17)
C8 0.025(2) 0.029(2) 0.020(2) 0.0006(17) 0.0048(16) -0.0009(17)
C9 0.020(2) 0.023(2) 0.037(2) -0.0013(18) 0.0053(18) -0.0001(17)
C10 0.034(2) 0.020(2) 0.033(2) 0.0038(18) 0.0072(19) 0.0040(17)
C21 0.023(2) 0.022(2) 0.020(2) -0.0031(16) 0.0108(16) 0.0008(16)
C22 0.023(2) 0.025(2) 0.021(2) 0.0015(16) 0.0081(16) 0.0043(16)
C23 0.0176(19) 0.027(2) 0.022(2) -0.0067(17) 0.0054(16) 0.0035(16)
C24 0.028(2) 0.020(2) 0.025(2) -0.0053(16) 0.0130(17) -0.0024(16)
C25 0.021(2) 0.024(2) 0.019(2) -0.0031(16) 0.0077(16) 0.0028(16)
C26 0.026(2) 0.027(2) 0.035(2) -0.0048(18) 0.0141(19) -0.0045(17)
C27 0.042(3) 0.035(3) 0.028(2) 0.0101(19) 0.013(2) 0.012(2)
C28 0.025(2) 0.055(3) 0.030(2) -0.019(2) 0.0051(19) -0.001(2)
C29 0.043(3) 0.018(2) 0.043(3) -0.0049(19) 0.017(2) -0.0062(19)
C30 0.031(2) 0.032(2) 0.026(2) -0.0024(18) 0.0038(18) 0.0096(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100854.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-09 22:39:32 +0300 (Sat, 09 Sep 2017) $
#$Revision: 200397 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100854.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100854
loop_
_publ_author_name
'Ghosh, Sundargopal'
'Fehlner, Thomas P.'
'Beatty, Alicia M.'
'Noll, Bruce C.'
_publ_section_title
;
Insertion of B-X (X = Cl, SMe~2~) Moieties into Ruthenaborane Frameworks:
Synthesis and Characterization of (\h^5^-C~5~Me~5~Ru)~2~(\m-H)B~4~H~m~Cl~n~,
(m, n = 4, 3; 5, 2; 7, 2),
closo-1-(SMe~2~)-2,3-(\h^5^-C~5~Me~5~Ru)~2~(\m~3~-H)B~5~HCl~3~, and
closo-2,3-(\h^5^-C~5~Me~5~Ru)~2~B~6~H~3~Cl~3~
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2473
_journal_page_last 2480
_journal_paper_doi 10.1021/om050083y
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C20 H41 B8 Cl Ru2'
_chemical_formula_sum 'C20 H41 B8 Cl Ru2'
_chemical_formula_weight 605.60
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.705(4)
_cell_length_b 13.701(4)
_cell_length_c 19.123(6)
_cell_measurement_reflns_used 8827
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 31.521
_cell_measurement_theta_min 2.353
_cell_volume 2542.8(15)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0388
_diffrn_reflns_av_sigmaI/netI 0.0249
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 27057
_diffrn_reflns_theta_max 31.56
_diffrn_reflns_theta_min 2.13
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.300
_exptl_absorpt_correction_T_max 0.9261
_exptl_absorpt_correction_T_min 0.6810
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. Acta Cryst. (1995) A51. 33-8'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.582
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1224
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.06
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.59(7)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.219
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 323
_refine_ls_number_reflns 4724
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.219
_refine_ls_R_factor_all 0.0476
_refine_ls_R_factor_gt 0.0451
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+6.1462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1095
_refine_ls_wR_factor_ref 0.1108
_reflns_number_gt 4511
_reflns_number_total 4724
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)2(1)2(1)
_cod_database_code 1100854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.03895(4) -0.52564(3) -0.05163(2) 0.01513(9) Uani 1 1 d . A .
Ru2 Ru 0.03254(4) -0.53339(3) 0.09994(2) 0.01549(9) Uani 1 1 d . A .
Cl1 Cl -0.29946(16) -0.42116(12) -0.07089(9) 0.0221(4) Uani 0.850(5) 1 d P A 1
Cl1' Cl -0.2953(12) -0.4196(10) 0.1117(7) 0.037(3) Uani 0.150(5) 1 d P A 2
B1 B -0.0458(6) -0.4322(4) 0.0259(4) 0.0195(10) Uani 1 1 d . A .
H1 H -0.031(9) -0.343(6) 0.028(4) 0.03(2) Uiso 1 1 d . . .
B2 B -0.1786(7) -0.4943(5) -0.0194(4) 0.0248(13) Uani 1 1 d . . .
B3 B -0.1851(7) -0.4853(5) 0.0726(4) 0.0221(12) Uani 1 1 d . A .
B4 B 0.1187(6) -0.6274(4) 0.0212(3) 0.0171(10) Uani 1 1 d . . .
H4 H 0.223(9) -0.652(6) 0.026(4) 0.03(2) Uiso 1 1 d . . .
H45 H 0.0334 -0.6976 0.0388 0.030 Uiso 1 1 d . . .
B5 B 0.0056(7) -0.6823(5) -0.0416(4) 0.0240(13) Uani 1 1 d . A .
H5 H 0.034(10) -0.742(7) -0.086(5) 0.05(3) Uiso 1 1 d . . .
H56 H -0.124(8) -0.707(6) -0.017(4) 0.03(2) Uiso 1 1 d . . .
B6 B -0.1504(7) -0.6108(5) -0.0558(4) 0.0236(12) Uani 1 1 d . A .
H6 H -0.204(8) -0.626(5) -0.101(4) 0.019(18) Uiso 1 1 d . . .
B7 B -0.2663(7) -0.5833(5) 0.0293(4) 0.0270(13) Uani 1 1 d . A .
H7 H -0.368(9) -0.587(7) 0.008(4) 0.04(2) Uiso 1 1 d . . .
H78 H -0.198(7) -0.655(5) 0.069(3) 0.012(16) Uiso 1 1 d . . .
B8 B -0.1726(8) -0.6026(5) 0.1073(4) 0.0262(14) Uani 1 1 d . . .
H8 H -0.212(11) -0.613(7) 0.149(5) 0.05(3) Uiso 1 1 d . . .
C1 C 0.0830(7) -0.3958(5) -0.1228(3) 0.0257(12) Uani 1 1 d . . .
C2 C 0.0388(6) -0.4767(5) -0.1632(3) 0.0279(12) Uani 1 1 d . A .
C3 C 0.1382(6) -0.5510(4) -0.1567(3) 0.0220(11) Uani 1 1 d . . .
C4 C 0.2424(6) -0.5191(4) -0.1100(3) 0.0196(10) Uani 1 1 d . A .
C5 C 0.2110(6) -0.4211(4) -0.0906(3) 0.0215(11) Uani 1 1 d . A .
C6 C 0.0205(10) -0.2955(5) -0.1206(5) 0.050(2) Uani 1 1 d . A .
H6A H 0.0492 -0.2587 -0.1621 0.060 Uiso 1 1 calc R . .
H6B H 0.0518 -0.2614 -0.0784 0.060 Uiso 1 1 calc R . .
H6C H -0.0801 -0.3009 -0.1199 0.060 Uiso 1 1 calc R . .
C7 C -0.0817(8) -0.4755(9) -0.2125(4) 0.049(2) Uani 1 1 d . . .
H7A H -0.1615 -0.4463 -0.1892 0.058 Uiso 1 1 calc R A .
H7B H -0.1040 -0.5425 -0.2266 0.058 Uiso 1 1 calc R . .
H7C H -0.0583 -0.4370 -0.2541 0.058 Uiso 1 1 calc R . .
C8 C 0.1364(9) -0.6437(6) -0.1984(4) 0.0379(17) Uani 1 1 d . A .
H8A H 0.1766 -0.6317 -0.2446 0.045 Uiso 1 1 calc R . .
H8B H 0.0412 -0.6662 -0.2038 0.045 Uiso 1 1 calc R . .
H8C H 0.1903 -0.6937 -0.1740 0.045 Uiso 1 1 calc R . .
C9 C 0.3750(6) -0.5714(5) -0.0941(4) 0.0286(13) Uani 1 1 d . . .
H9A H 0.3643 -0.6411 -0.1042 0.034 Uiso 1 1 calc R A .
H9B H 0.3980 -0.5627 -0.0445 0.034 Uiso 1 1 calc R . .
H9C H 0.4491 -0.5444 -0.1230 0.034 Uiso 1 1 calc R . .
C10 C 0.3041(9) -0.3492(5) -0.0540(4) 0.0364(16) Uani 1 1 d . . .
H10A H 0.3861 -0.3832 -0.0367 0.044 Uiso 1 1 calc R A .
H10B H 0.2547 -0.3197 -0.0146 0.044 Uiso 1 1 calc R . .
H10C H 0.3319 -0.2981 -0.0869 0.044 Uiso 1 1 calc R . .
C11 C 0.1460(6) -0.4111(4) 0.1534(3) 0.0186(10) Uani 1 1 d . . .
C12 C 0.0434(7) -0.4463(3) 0.1997(3) 0.0193(9) Uani 1 1 d . A .
C13 C 0.0728(7) -0.5463(4) 0.2142(3) 0.0231(11) Uani 1 1 d . . .
C14 C 0.1968(7) -0.5715(4) 0.1784(3) 0.0218(11) Uani 1 1 d . A .
C15 C 0.2438(6) -0.4871(4) 0.1402(3) 0.0199(10) Uani 1 1 d . A .
C16 C 0.1618(7) -0.3051(4) 0.1319(3) 0.0241(12) Uani 1 1 d . A .
H16A H 0.2119 -0.2696 0.1684 0.029 Uiso 1 1 calc R . .
H16B H 0.0705 -0.2759 0.1255 0.029 Uiso 1 1 calc R . .
H16C H 0.2133 -0.3015 0.0879 0.029 Uiso 1 1 calc R . .
C17 C -0.0725(7) -0.3875(4) 0.2306(3) 0.0255(12) Uani 1 1 d . . .
H17A H -0.1434 -0.4317 0.2487 0.031 Uiso 1 1 calc R A .
H17B H -0.1125 -0.3456 0.1944 0.031 Uiso 1 1 calc R . .
H17C H -0.0370 -0.3470 0.2688 0.031 Uiso 1 1 calc R . .
C18 C -0.0020(8) -0.6101(4) 0.2651(3) 0.0289(14) Uani 1 1 d . A .
H18A H 0.0481 -0.6112 0.3096 0.035 Uiso 1 1 calc R . .
H18B H -0.0080 -0.6765 0.2463 0.035 Uiso 1 1 calc R . .
H18C H -0.0950 -0.5844 0.2727 0.035 Uiso 1 1 calc R . .
C19 C 0.2747(8) -0.6661(5) 0.1860(4) 0.0292(13) Uani 1 1 d . . .
H19A H 0.3105 -0.6715 0.2338 0.035 Uiso 1 1 calc R A .
H19B H 0.3515 -0.6672 0.1528 0.035 Uiso 1 1 calc R . .
H19C H 0.2127 -0.7209 0.1764 0.035 Uiso 1 1 calc R . .
C20 C 0.3790(6) -0.4793(5) 0.1044(3) 0.0277(12) Uani 1 1 d . . .
H20A H 0.3831 -0.4178 0.0783 0.033 Uiso 1 1 calc R A .
H20B H 0.3900 -0.5341 0.0719 0.033 Uiso 1 1 calc R . .
H20C H 0.4531 -0.4808 0.1392 0.033 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01325(16) 0.00957(16) 0.02258(18) -0.00047(14) 0.00014(15) 0.00082(16)
Ru2 0.01596(17) 0.00840(15) 0.02210(18) -0.00196(13) -0.00037(15) 0.00076(16)
Cl1 0.0161(7) 0.0168(7) 0.0334(8) 0.0053(6) -0.0053(6) 0.0026(5)
Cl1' 0.026(5) 0.044(7) 0.041(6) 0.001(5) 0.004(5) -0.003(5)
B1 0.014(2) 0.010(2) 0.034(3) -0.001(2) -0.005(3) 0.0024(19)
B2 0.023(3) 0.016(3) 0.035(3) -0.004(3) 0.001(3) -0.001(2)
B3 0.020(3) 0.017(3) 0.029(3) 0.001(2) 0.002(2) 0.000(2)
B4 0.022(3) 0.009(2) 0.020(2) -0.006(2) 0.004(2) 0.0018(19)
B5 0.026(3) 0.017(3) 0.029(3) 0.000(2) -0.002(2) 0.001(2)
B6 0.019(3) 0.015(3) 0.036(3) -0.002(2) 0.000(3) -0.004(2)
B7 0.019(3) 0.023(3) 0.039(4) -0.003(3) 0.001(3) -0.001(2)
B8 0.027(3) 0.013(3) 0.039(4) 0.000(3) -0.001(3) -0.005(2)
C1 0.027(3) 0.020(3) 0.030(3) 0.012(2) 0.005(2) 0.009(2)
C2 0.017(2) 0.043(3) 0.024(2) 0.014(2) 0.000(2) -0.001(3)
C3 0.026(3) 0.019(2) 0.021(2) 0.0000(19) 0.004(2) -0.004(2)
C4 0.016(2) 0.016(2) 0.026(2) 0.007(2) 0.0003(19) 0.0024(19)
C5 0.026(3) 0.018(2) 0.021(2) 0.003(2) 0.003(2) -0.005(2)
C6 0.055(5) 0.024(3) 0.071(5) 0.026(3) 0.026(4) 0.023(4)
C7 0.030(3) 0.084(7) 0.032(3) 0.013(4) -0.007(3) 0.001(4)
C8 0.054(5) 0.031(3) 0.028(3) -0.009(3) 0.011(3) -0.014(3)
C9 0.023(3) 0.030(3) 0.034(3) 0.008(3) 0.009(2) 0.008(2)
C10 0.050(4) 0.028(3) 0.031(3) -0.006(3) 0.008(3) -0.021(3)
C11 0.023(2) 0.009(2) 0.023(2) -0.0044(19) -0.006(2) -0.0003(18)
C12 0.028(3) 0.0090(18) 0.021(2) -0.0030(16) -0.002(2) -0.003(2)
C13 0.032(3) 0.009(2) 0.028(3) -0.0040(19) 0.002(2) 0.0014(19)
C14 0.024(3) 0.016(2) 0.026(3) -0.004(2) -0.005(2) 0.004(2)
C15 0.017(2) 0.019(3) 0.024(2) -0.005(2) -0.0032(19) -0.001(2)
C16 0.030(3) 0.012(2) 0.030(3) -0.002(2) -0.007(2) -0.007(2)
C17 0.034(3) 0.011(2) 0.031(3) -0.002(2) 0.006(2) 0.004(2)
C18 0.045(4) 0.016(2) 0.025(3) 0.000(2) 0.008(3) 0.000(2)
C19 0.035(3) 0.017(3) 0.036(3) -0.003(2) -0.008(3) 0.010(2)
C20 0.023(2) 0.032(3) 0.029(3) -0.005(3) -0.002(2) -0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100855.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100855.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100855
loop_
_publ_author_name
'Busetto, Luigi'
'Marchetti, Fabio'
'Zacchini, Stefano'
'Zanotti, Valerio'
_publ_section_title
;
Deprotonation of \m-Vinyliminium Ligands in Diiron Complexes:  A
Route for the Synthesis of Mono- and Polynuclear Species Containing Novel
Multidentate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2297
_journal_page_last 2306
_journal_paper_doi 10.1021/om050095j
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C39 H40 Cl2 Fe4 N2 O8'
_chemical_formula_weight 959.03
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 105.50(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 18.032(4)
_cell_length_b 10.346(2)
_cell_length_c 21.479(4)
_cell_measurement_reflns_used 7752
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 35.4035
_cell_measurement_theta_min 2.291
_cell_volume 3861.2(13)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0771
_diffrn_reflns_av_sigmaI/netI 0.0455
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 37213
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 1.31
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.667
_exptl_absorpt_correction_T_max 0.7881
_exptl_absorpt_correction_T_min 0.6905
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.650
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1960
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.15
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 502
_refine_ls_number_reflns 7877
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0584
_refine_ls_R_factor_gt 0.0502
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+7.6004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1353
_refine_ls_wR_factor_ref 0.1416
_reflns_number_gt 6609
_reflns_number_total 7877
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100855
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.82757(3) 0.50596(5) 0.60562(2) 0.01519(13) Uani 1 1 d . . .
Fe2 Fe 0.77914(3) 0.27656(5) 0.60345(2) 0.01515(13) Uani 1 1 d . . .
Fe3 Fe 1.10922(3) 0.12373(5) 0.76770(2) 0.01413(13) Uani 1 1 d . . .
Fe4 Fe 1.11953(3) 0.09957(5) 0.65310(2) 0.01425(13) Uani 1 1 d . . .
C1 C 0.8636(2) 0.6856(4) 0.57742(18) 0.0244(8) Uani 1 1 d . . .
H1 H 0.9052 0.7342 0.6034 0.029 Uiso 1 1 calc R . .
C2 C 0.8690(2) 0.5933(4) 0.53109(18) 0.0227(8) Uani 1 1 d . . .
H2 H 0.9145 0.5694 0.5198 0.027 Uiso 1 1 calc R . .
C3 C 0.7945(2) 0.5419(4) 0.50412(18) 0.0254(8) Uani 1 1 d . . .
H3 H 0.7813 0.4764 0.4721 0.030 Uiso 1 1 calc R . .
C4 C 0.7431(2) 0.6059(4) 0.5336(2) 0.0275(9) Uani 1 1 d . . .
H4 H 0.6892 0.5913 0.5242 0.033 Uiso 1 1 calc R . .
C5 C 0.7851(2) 0.6941(4) 0.5789(2) 0.0272(9) Uani 1 1 d . . .
H5 H 0.7650 0.7495 0.6057 0.033 Uiso 1 1 calc R . .
C6 C 0.7363(2) 0.2127(4) 0.50597(19) 0.0248(8) Uani 1 1 d . . .
H6 H 0.7531 0.2461 0.4709 0.030 Uiso 1 1 calc R . .
C7 C 0.6747(2) 0.2598(4) 0.5277(2) 0.0256(8) Uani 1 1 d . . .
H7 H 0.6423 0.3302 0.5094 0.031 Uiso 1 1 calc R . .
C8 C 0.6689(2) 0.1854(4) 0.58129(19) 0.0265(9) Uani 1 1 d . . .
H8 H 0.6322 0.1971 0.6054 0.032 Uiso 1 1 calc R . .
C9 C 0.7270(2) 0.0907(4) 0.5926(2) 0.0264(9) Uani 1 1 d . . .
H9 H 0.7367 0.0272 0.6258 0.032 Uiso 1 1 calc R . .
C10 C 0.7689(2) 0.1068(4) 0.5455(2) 0.0249(8) Uani 1 1 d . . .
H10 H 0.8112 0.0558 0.5414 0.030 Uiso 1 1 calc R . .
C11 C 1.1534(2) 0.1134(4) 0.56710(19) 0.0245(8) Uani 1 1 d . . .
H11 H 1.1184 0.1096 0.5253 0.029 Uiso 1 1 calc R . .
C12 C 1.1768(2) 0.2266(4) 0.60353(18) 0.0222(8) Uani 1 1 d . . .
H12 H 1.1608 0.3122 0.5907 0.027 Uiso 1 1 calc R . .
C13 C 1.2287(2) 0.1894(4) 0.66261(18) 0.0203(7) Uani 1 1 d . . .
H13 H 1.2537 0.2463 0.6964 0.024 Uiso 1 1 calc R . .
C14 C 1.2373(2) 0.0526(4) 0.66301(19) 0.0214(8) Uani 1 1 d . . .
H14 H 1.2685 0.0023 0.6970 0.026 Uiso 1 1 calc R . .
C15 C 1.1910(2) 0.0054(4) 0.60371(19) 0.0233(8) Uani 1 1 d . . .
H15 H 1.1857 -0.0825 0.5905 0.028 Uiso 1 1 calc R . .
C16 C 1.2100(2) 0.2256(4) 0.82074(17) 0.0220(8) Uani 1 1 d . . .
H16 H 1.2425 0.2760 0.8021 0.026 Uiso 1 1 calc R . .
C17 C 1.2182(2) 0.0932(4) 0.83532(19) 0.0264(9) Uani 1 1 d . . .
H17 H 1.2576 0.0386 0.8282 0.032 Uiso 1 1 calc R . .
C18 C 1.1584(2) 0.0546(4) 0.86223(19) 0.0284(9) Uani 1 1 d . . .
H18 H 1.1502 -0.0300 0.8762 0.034 Uiso 1 1 calc R . .
C19 C 1.1126(2) 0.1658(5) 0.86455(18) 0.0280(9) Uani 1 1 d . . .
H19 H 1.0685 0.1686 0.8807 0.034 Uiso 1 1 calc R . .
C20 C 1.1444(2) 0.2707(4) 0.83873(18) 0.0250(8) Uani 1 1 d . . .
H20 H 1.1252 0.3567 0.8342 0.030 Uiso 1 1 calc R . .
C21 C 0.8664(2) 0.5358(3) 0.68829(18) 0.0181(7) Uani 1 1 d . . .
O21 O 0.88784(16) 0.5609(3) 0.74228(13) 0.0273(6) Uani 1 1 d . . .
C22 C 0.7414(2) 0.4247(4) 0.63185(17) 0.0198(7) Uani 1 1 d . . .
O22 O 0.69095(15) 0.4662(3) 0.65232(14) 0.0258(6) Uani 1 1 d . . .
C23 C 1.0321(2) 0.0305(4) 0.61104(18) 0.0214(8) Uani 1 1 d . . .
O23 O 0.97551(17) -0.0164(3) 0.58154(15) 0.0345(7) Uani 1 1 d . . .
C24 C 1.1218(2) -0.0252(3) 0.72320(17) 0.0177(7) Uani 1 1 d . . .
O24 O 1.12900(16) -0.1388(2) 0.72778(14) 0.0249(6) Uani 1 1 d . . .
C25 C 0.88727(19) 0.3404(3) 0.60910(16) 0.0152(7) Uani 1 1 d . . .
C26 C 0.91470(19) 0.2658(3) 0.66919(16) 0.0143(7) Uani 1 1 d . . .
C27 C 0.8440(2) 0.2549(3) 0.68851(17) 0.0154(7) Uani 1 1 d . . .
C28 C 0.9339(2) 0.3364(3) 0.56099(17) 0.0167(7) Uani 1 1 d . . .
O1 O 0.99937(14) 0.3729(3) 0.56990(13) 0.0225(6) Uani 1 1 d . . .
O2 O 0.89324(15) 0.2918(3) 0.50274(13) 0.0234(6) Uani 1 1 d . . .
C29 C 0.9324(3) 0.3001(5) 0.4523(2) 0.0320(10) Uani 1 1 d . . .
H29A H 0.9430 0.3909 0.4449 0.048 Uiso 1 1 calc R . .
H29B H 0.8998 0.2627 0.4124 0.048 Uiso 1 1 calc R . .
H29C H 0.9810 0.2522 0.4654 0.048 Uiso 1 1 calc R . .
N1 N 0.83702(17) 0.2488(3) 0.74734(15) 0.0184(6) Uani 1 1 d . . .
C30 C 0.7618(2) 0.2361(4) 0.7601(2) 0.0275(9) Uani 1 1 d . . .
H30A H 0.7221 0.2264 0.7191 0.041 Uiso 1 1 calc R . .
H30B H 0.7511 0.3135 0.7825 0.041 Uiso 1 1 calc R . .
H30C H 0.7616 0.1599 0.7871 0.041 Uiso 1 1 calc R . .
C31 C 0.9013(2) 0.2647(4) 0.80611(18) 0.0249(8) Uani 1 1 d . . .
H31A H 0.9474 0.2930 0.7940 0.037 Uiso 1 1 calc R . .
H31B H 0.9116 0.1820 0.8291 0.037 Uiso 1 1 calc R . .
H31C H 0.8874 0.3296 0.8343 0.037 Uiso 1 1 calc R . .
C32 C 1.06331(19) 0.2320(3) 0.68989(16) 0.0136(7) Uani 1 1 d . . .
C33 C 0.98421(19) 0.1985(3) 0.69395(16) 0.0140(7) Uani 1 1 d . . .
C34 C 1.00251(19) 0.0907(3) 0.73838(16) 0.0144(7) Uani 1 1 d . . .
C35 C 1.0872(2) 0.3713(3) 0.69610(16) 0.0152(7) Uani 1 1 d . . .
O3 O 1.14840(15) 0.4137(3) 0.69228(14) 0.0246(6) Uani 1 1 d . . .
O4 O 1.03498(14) 0.4501(2) 0.71171(13) 0.0193(5) Uani 1 1 d . . .
C36 C 1.0571(2) 0.5842(4) 0.7174(2) 0.0259(8) Uani 1 1 d . . .
H36A H 1.1030 0.5950 0.7538 0.039 Uiso 1 1 calc R . .
H36B H 1.0149 0.6362 0.7249 0.039 Uiso 1 1 calc R . .
H36C H 1.0686 0.6126 0.6774 0.039 Uiso 1 1 calc R . .
N2 N 0.95685(18) -0.0036(3) 0.74752(15) 0.0190(6) Uani 1 1 d . . .
C37 C 0.8811(2) -0.0308(4) 0.70490(19) 0.0223(8) Uani 1 1 d . . .
H37A H 0.8722 0.0240 0.6664 0.034 Uiso 1 1 calc R . .
H37B H 0.8418 -0.0129 0.7276 0.034 Uiso 1 1 calc R . .
H37C H 0.8783 -0.1219 0.6920 0.034 Uiso 1 1 calc R . .
C38 C 0.9832(2) -0.0994(4) 0.7991(2) 0.0279(9) Uani 1 1 d . . .
H38A H 1.0395 -0.0981 0.8139 0.042 Uiso 1 1 calc R . .
H38B H 0.9658 -0.1856 0.7825 0.042 Uiso 1 1 calc R . .
H38C H 0.9617 -0.0786 0.8353 0.042 Uiso 1 1 calc R . .
C39 C 0.1059(6) 0.5771(10) 0.9542(4) 0.115(4) Uani 1 1 d . . .
H39A H 0.1524 0.6185 0.9469 0.137 Uiso 1 1 calc R . .
H39B H 0.1200 0.4885 0.9705 0.137 Uiso 1 1 calc R . .
Cl1 Cl 0.03519(16) 0.5692(3) 0.88203(10) 0.1158(10) Uani 1 1 d . . .
Cl2 Cl 0.07401(17) 0.6671(3) 1.01292(12) 0.1191(9) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0146(3) 0.0160(3) 0.0147(3) 0.00187(19) 0.0034(2) 0.00160(18)
Fe2 0.0125(3) 0.0178(3) 0.0145(3) -0.00026(19) 0.00261(19) -0.00021(18)
Fe3 0.0133(3) 0.0146(3) 0.0132(2) 0.00045(18) 0.00153(19) 0.00089(18)
Fe4 0.0132(3) 0.0147(3) 0.0143(3) -0.00064(18) 0.00287(19) 0.00063(18)
C1 0.033(2) 0.0184(18) 0.0207(19) 0.0074(15) 0.0042(16) 0.0001(16)
C2 0.0248(19) 0.0237(19) 0.0220(19) 0.0092(15) 0.0105(15) 0.0028(15)
C3 0.031(2) 0.025(2) 0.0179(18) 0.0094(15) 0.0015(16) 0.0012(16)
C4 0.0209(19) 0.030(2) 0.028(2) 0.0158(17) 0.0019(16) 0.0063(16)
C5 0.039(2) 0.0198(19) 0.025(2) 0.0090(16) 0.0140(18) 0.0101(17)
C6 0.0229(19) 0.032(2) 0.0172(18) -0.0069(16) 0.0019(15) -0.0058(16)
C7 0.0144(18) 0.031(2) 0.027(2) -0.0036(17) -0.0026(15) -0.0022(15)
C8 0.0161(18) 0.037(2) 0.025(2) -0.0077(17) 0.0046(15) -0.0099(16)
C9 0.024(2) 0.0221(19) 0.028(2) -0.0035(16) -0.0009(16) -0.0112(16)
C10 0.0210(19) 0.024(2) 0.028(2) -0.0084(16) 0.0028(16) -0.0034(15)
C11 0.0205(19) 0.035(2) 0.0205(19) -0.0038(16) 0.0094(15) -0.0010(16)
C12 0.0249(19) 0.0225(19) 0.0228(19) 0.0054(15) 0.0125(16) 0.0009(15)
C13 0.0150(17) 0.0236(19) 0.0244(19) -0.0015(15) 0.0090(14) -0.0017(14)
C14 0.0148(17) 0.0251(19) 0.0259(19) 0.0016(15) 0.0080(15) 0.0030(14)
C15 0.023(2) 0.0235(19) 0.026(2) -0.0044(15) 0.0118(16) 0.0017(15)
C16 0.0223(19) 0.026(2) 0.0148(17) -0.0050(15) 0.0003(14) -0.0063(15)
C17 0.0164(18) 0.035(2) 0.0205(19) -0.0044(16) -0.0078(15) 0.0081(16)
C18 0.032(2) 0.029(2) 0.0168(18) 0.0082(16) -0.0048(16) -0.0045(17)
C19 0.0207(19) 0.048(3) 0.0137(17) -0.0043(17) 0.0012(15) -0.0005(18)
C20 0.026(2) 0.026(2) 0.0180(18) -0.0059(15) -0.0025(15) 0.0041(16)
C21 0.0131(17) 0.0170(17) 0.024(2) 0.0016(14) 0.0045(14) 0.0026(13)
O21 0.0245(14) 0.0357(16) 0.0199(14) -0.0054(12) 0.0029(11) 0.0036(12)
C22 0.0204(18) 0.0224(18) 0.0156(17) 0.0011(14) 0.0032(14) 0.0001(15)
O22 0.0212(14) 0.0272(14) 0.0332(16) -0.0011(12) 0.0144(12) 0.0030(11)
C23 0.024(2) 0.0214(18) 0.0190(18) -0.0044(15) 0.0063(15) 0.0032(15)
O23 0.0223(15) 0.0452(19) 0.0331(16) -0.0168(14) 0.0022(13) -0.0059(13)
C24 0.0151(17) 0.0187(18) 0.0190(17) 0.0015(14) 0.0039(14) 0.0012(13)
O24 0.0299(15) 0.0145(13) 0.0303(15) 0.0017(11) 0.0078(12) 0.0018(11)
C25 0.0114(15) 0.0184(17) 0.0148(16) -0.0007(13) 0.0020(13) 0.0002(13)
C26 0.0142(16) 0.0142(16) 0.0130(16) -0.0008(13) 0.0012(13) -0.0016(13)
C27 0.0165(17) 0.0114(16) 0.0182(17) -0.0010(13) 0.0046(14) 0.0000(13)
C28 0.0185(17) 0.0143(16) 0.0174(17) 0.0048(13) 0.0052(14) 0.0032(13)
O1 0.0151(13) 0.0328(15) 0.0194(13) 0.0035(11) 0.0042(10) -0.0007(11)
O2 0.0243(14) 0.0306(15) 0.0179(13) -0.0063(11) 0.0101(11) -0.0070(11)
C29 0.040(2) 0.042(3) 0.0202(19) -0.0089(18) 0.0190(18) -0.014(2)
N1 0.0169(15) 0.0219(16) 0.0173(15) 0.0047(12) 0.0060(12) 0.0032(12)
C30 0.0210(19) 0.036(2) 0.030(2) 0.0079(18) 0.0147(17) 0.0077(16)
C31 0.027(2) 0.033(2) 0.0140(17) -0.0014(16) 0.0032(15) 0.0044(16)
C32 0.0131(16) 0.0132(16) 0.0131(16) -0.0004(12) 0.0012(13) -0.0004(12)
C33 0.0138(16) 0.0135(16) 0.0146(16) -0.0032(13) 0.0036(13) -0.0018(12)
C34 0.0126(16) 0.0167(16) 0.0148(16) -0.0028(13) 0.0051(13) 0.0019(13)
C35 0.0185(17) 0.0133(16) 0.0118(16) 0.0007(12) 0.0008(13) -0.0006(13)
O3 0.0188(13) 0.0178(13) 0.0390(16) -0.0031(12) 0.0109(12) -0.0060(10)
O4 0.0180(13) 0.0133(12) 0.0281(14) -0.0030(10) 0.0087(11) -0.0006(10)
C36 0.025(2) 0.0130(17) 0.039(2) -0.0058(16) 0.0084(17) -0.0010(15)
N2 0.0183(15) 0.0157(15) 0.0226(16) 0.0030(12) 0.0049(13) -0.0010(11)
C37 0.0172(18) 0.0193(18) 0.030(2) -0.0044(16) 0.0054(15) -0.0053(14)
C38 0.029(2) 0.023(2) 0.032(2) 0.0119(17) 0.0092(17) -0.0009(16)
C39 0.130(8) 0.113(7) 0.076(6) -0.001(5) -0.015(5) 0.062(6)
Cl1 0.139(2) 0.145(2) 0.0542(11) 0.0056(12) 0.0108(12) 0.0817(18)
Cl2 0.134(2) 0.135(2) 0.0874(16) -0.0371(16) 0.0292(15) -0.0386(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100856.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100856.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100856
loop_
_publ_author_name
'Busetto, Luigi'
'Marchetti, Fabio'
'Zacchini, Stefano'
'Zanotti, Valerio'
_publ_section_title
;
Deprotonation of \m-Vinyliminium Ligands in Diiron Complexes:  A
Route for the Synthesis of Mono- and Polynuclear Species Containing Novel
Multidentate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2297
_journal_page_last 2306
_journal_paper_doi 10.1021/om050095j
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C20 H21 Fe N O2'
_chemical_formula_weight 363.23
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 109.83(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.3991(19)
_cell_length_b 19.964(4)
_cell_length_c 10.132(2)
_cell_measurement_reflns_used 3988
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 22.7305
_cell_measurement_theta_min 2.3035
_cell_volume 1788.5(6)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0644
_diffrn_reflns_av_sigmaI/netI 0.0472
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 21148
_diffrn_reflns_theta_max 28.70
_diffrn_reflns_theta_min 2.04
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.854
_exptl_absorpt_correction_T_max 0.9119
_exptl_absorpt_correction_T_min 0.8213
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 1.349
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 760
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.11
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.963
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 221
_refine_ls_number_reflns 4625
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.963
_refine_ls_R_factor_all 0.0892
_refine_ls_R_factor_gt 0.0494
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1252
_refine_ls_wR_factor_ref 0.1452
_reflns_number_gt 2757
_reflns_number_total 4625
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22846(4) 0.082484(19) 0.39792(4) 0.04807(15) Uani 1 1 d . . .
C1 C 0.3359(4) 0.05144(19) 0.6082(4) 0.0746(10) Uani 1 1 d . . .
H1 H 0.3575 0.0070 0.6348 0.090 Uiso 1 1 calc R . .
C2 C 0.4301(4) 0.09582(19) 0.5674(4) 0.0751(10) Uani 1 1 d . . .
H2 H 0.5254 0.0862 0.5636 0.090 Uiso 1 1 calc R . .
C3 C 0.3527(4) 0.15782(18) 0.5332(4) 0.0708(9) Uani 1 1 d . . .
H3 H 0.3877 0.1961 0.5017 0.085 Uiso 1 1 calc R . .
C4 C 0.2143(4) 0.15121(19) 0.5552(4) 0.0720(9) Uani 1 1 d . . .
H4 H 0.1418 0.1847 0.5411 0.086 Uiso 1 1 calc R . .
C5 C 0.2026(5) 0.08654(19) 0.6014(4) 0.0730(10) Uani 1 1 d . . .
H5 H 0.1217 0.0694 0.6239 0.088 Uiso 1 1 calc R . .
C6 C 0.1792(4) 0.00276(17) 0.3321(4) 0.0627(8) Uani 1 1 d . . .
O1 O 0.1444(4) -0.04950(13) 0.2880(4) 0.1033(10) Uani 1 1 d . . .
C7 C 0.3390(3) 0.09768(14) 0.2701(4) 0.0562(7) Uani 1 1 d . . .
O2 O 0.4727(3) 0.08943(13) 0.2891(3) 0.0883(8) Uani 1 1 d . . .
C8 C 0.2425(3) 0.12579(15) 0.1302(3) 0.0564(7) Uani 1 1 d . . .
C9 C 0.1007(3) 0.13829(15) 0.1226(3) 0.0571(7) Uani 1 1 d . . .
H9 H 0.0299 0.1573 0.0438 0.069 Uiso 1 1 calc R . .
C10 C 0.0647(3) 0.11976(13) 0.2478(3) 0.0443(6) Uani 1 1 d . . .
C11 C 0.3078(4) 0.1385(2) 0.0163(4) 0.0859(12) Uani 1 1 d . . .
H11A H 0.2311 0.1569 -0.0642 0.129 Uiso 1 1 calc R . .
H11B H 0.3437 0.0971 -0.0091 0.129 Uiso 1 1 calc R . .
H11C H 0.3903 0.1696 0.0494 0.129 Uiso 1 1 calc R . .
N1 N -0.0778(2) 0.13019(11) 0.2390(2) 0.0457(5) Uani 1 1 d . . .
C12 C -0.1370(3) 0.10839(17) 0.3491(3) 0.0634(8) Uani 1 1 d . . .
H12A H -0.0862 0.0682 0.3921 0.095 Uiso 1 1 calc R . .
H12B H -0.2435 0.0999 0.3083 0.095 Uiso 1 1 calc R . .
H12C H -0.1199 0.1429 0.4188 0.095 Uiso 1 1 calc R . .
C13 C -0.1859(3) 0.16528(14) 0.1240(3) 0.0488(6) Uani 1 1 d . . .
C14 C -0.2829(3) 0.12907(18) 0.0127(3) 0.0642(8) Uani 1 1 d . . .
C15 C -0.3851(4) 0.1655(3) -0.0965(4) 0.0914(13) Uani 1 1 d . . .
H15 H -0.4505 0.1430 -0.1737 0.110 Uiso 1 1 calc R . .
C16 C -0.3898(5) 0.2347(3) -0.0904(5) 0.0935(15) Uani 1 1 d . . .
H16 H -0.4588 0.2582 -0.1636 0.112 Uiso 1 1 calc R . .
C17 C -0.2962(4) 0.2683(2) 0.0197(5) 0.0802(12) Uani 1 1 d . . .
H17 H -0.3028 0.3148 0.0219 0.096 Uiso 1 1 calc R . .
C18 C -0.1893(3) 0.23524(16) 0.1306(4) 0.0590(8) Uani 1 1 d . . .
C19 C -0.2771(5) 0.0542(2) 0.0112(5) 0.1018(14) Uani 1 1 d . . .
H19A H -0.1743 0.0398 0.0325 0.153 Uiso 1 1 calc R . .
H19B H -0.3370 0.0381 -0.0800 0.153 Uiso 1 1 calc R . .
H19C H -0.3163 0.0366 0.0801 0.153 Uiso 1 1 calc R . .
C20 C -0.0820(4) 0.27365(17) 0.2499(4) 0.0785(10) Uani 1 1 d . . .
H20A H -0.0986 0.2620 0.3354 0.118 Uiso 1 1 calc R . .
H20B H -0.0986 0.3208 0.2329 0.118 Uiso 1 1 calc R . .
H20C H 0.0201 0.2628 0.2579 0.118 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0404(2) 0.0465(2) 0.0575(3) 0.00726(19) 0.01689(18) 0.00137(16)
C1 0.079(2) 0.068(2) 0.064(2) 0.0179(17) 0.0080(18) 0.0004(19)
C2 0.0498(19) 0.089(3) 0.074(2) 0.0033(19) 0.0044(17) 0.0012(17)
C3 0.072(2) 0.065(2) 0.071(2) -0.0027(17) 0.0177(18) -0.0165(17)
C4 0.079(2) 0.072(2) 0.0621(19) -0.0079(17) 0.0196(18) 0.0088(18)
C5 0.072(2) 0.091(3) 0.0565(19) 0.0045(18) 0.0215(17) -0.0092(19)
C6 0.0573(18) 0.0578(19) 0.077(2) 0.0062(16) 0.0284(17) 0.0007(15)
O1 0.120(2) 0.0537(15) 0.145(3) -0.0126(17) 0.056(2) -0.0130(15)
C7 0.0425(15) 0.0488(16) 0.080(2) 0.0074(14) 0.0242(15) 0.0035(12)
O2 0.0468(13) 0.116(2) 0.112(2) 0.0323(16) 0.0395(14) 0.0215(13)
C8 0.0509(17) 0.0578(17) 0.0713(19) 0.0105(15) 0.0347(15) 0.0098(13)
C9 0.0500(16) 0.0670(19) 0.0604(17) 0.0153(15) 0.0266(14) 0.0187(14)
C10 0.0395(13) 0.0404(14) 0.0556(16) -0.0022(11) 0.0196(12) -0.0005(10)
C11 0.078(2) 0.103(3) 0.100(3) 0.029(2) 0.061(2) 0.022(2)
N1 0.0390(11) 0.0482(12) 0.0542(13) 0.0019(10) 0.0216(10) 0.0006(9)
C12 0.0508(17) 0.075(2) 0.074(2) 0.0151(16) 0.0332(16) 0.0035(15)
C13 0.0341(12) 0.0574(16) 0.0594(17) 0.0041(13) 0.0217(12) 0.0078(11)
C14 0.0455(16) 0.085(2) 0.064(2) -0.0076(17) 0.0201(15) -0.0053(15)
C15 0.0474(19) 0.166(5) 0.058(2) 0.009(3) 0.0150(17) -0.007(2)
C16 0.062(2) 0.144(4) 0.085(3) 0.051(3) 0.037(2) 0.041(3)
C17 0.067(2) 0.090(3) 0.102(3) 0.043(2) 0.052(2) 0.034(2)
C18 0.0526(16) 0.0568(17) 0.080(2) 0.0125(15) 0.0386(16) 0.0119(13)
C19 0.108(3) 0.088(3) 0.108(3) -0.037(3) 0.035(3) -0.028(2)
C20 0.089(3) 0.0543(19) 0.105(3) -0.0078(19) 0.049(2) -0.0044(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100857.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100857.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100857
loop_
_publ_author_name
'Busetto, Luigi'
'Marchetti, Fabio'
'Zacchini, Stefano'
'Zanotti, Valerio'
_publ_section_title
;
Deprotonation of \m-Vinyliminium Ligands in Diiron Complexes:  A
Route for the Synthesis of Mono- and Polynuclear Species Containing Novel
Multidentate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2297
_journal_page_last 2306
_journal_paper_doi 10.1021/om050095j
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C36 H38 Fe4 N2 O4'
_chemical_formula_weight 786.08
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 112.80(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.735(3)
_cell_length_b 27.480(6)
_cell_length_c 10.206(2)
_cell_measurement_reflns_used 1005
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.3545
_cell_measurement_theta_min 2.3095
_cell_volume 3292.8(11)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1083
_diffrn_reflns_av_sigmaI/netI 0.0885
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 32
_diffrn_reflns_limit_k_min -32
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 26427
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 1.48
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.770
_exptl_absorpt_correction_T_max 0.8291
_exptl_absorpt_correction_T_min 0.7298
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 1.586
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1616
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.11
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 417
_refine_ls_number_reflns 5811
_refine_ls_number_restraints 178
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.0956
_refine_ls_R_factor_gt 0.0564
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.0384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1226
_refine_ls_wR_factor_ref 0.1398
_reflns_number_gt 3922
_reflns_number_total 5811
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.10977(7) 0.33641(3) 0.83271(9) 0.0338(2) Uani 1 1 d . A .
Fe2 Fe -0.07356(6) 0.40645(3) 0.69728(8) 0.0261(2) Uani 1 1 d . . .
Fe3 Fe 0.42836(6) 0.34921(3) 1.06538(8) 0.0262(2) Uani 1 1 d . A .
Fe4 Fe 0.38669(6) 0.40276(3) 1.23901(8) 0.0244(2) Uani 1 1 d . . .
C1 C -0.1661(16) 0.2873(6) 0.945(3) 0.058(4) Uiso 0.51(2) 1 d PDU A 1
H1 H -0.1305 0.2574 0.9747 0.070 Uiso 0.51(2) 1 calc PR A 1
C2 C -0.1423(12) 0.3321(9) 1.0186(14) 0.046(3) Uiso 0.51(2) 1 d PDU A 1
H2 H -0.0885 0.3364 1.1105 0.055 Uiso 0.51(2) 1 calc PR A 1
C3 C -0.2097(16) 0.3689(6) 0.935(2) 0.049(4) Uiso 0.51(2) 1 d PDU A 1
H3 H -0.2047 0.4015 0.9610 0.059 Uiso 0.51(2) 1 calc PR A 1
C4 C -0.2845(11) 0.3505(6) 0.8095(15) 0.035(3) Uiso 0.51(2) 1 d PDU A 1
H4 H -0.3395 0.3681 0.7376 0.042 Uiso 0.51(2) 1 calc PR A 1
C5 C -0.2636(15) 0.3000(6) 0.8079(19) 0.050(3) Uiso 0.51(2) 1 d PDU A 1
H5 H -0.3029 0.2784 0.7351 0.059 Uiso 0.51(2) 1 calc PR A 1
C1' C -0.2828(12) 0.3332(8) 0.7908(15) 0.046(3) Uiso 0.49(2) 1 d PDU A 2
H1' H -0.3384 0.3374 0.7000 0.055 Uiso 0.49(2) 1 calc PR A 2
C2' C -0.2310(19) 0.2890(6) 0.853(2) 0.054(3) Uiso 0.49(2) 1 d PDU A 2
H2' H -0.2452 0.2583 0.8111 0.064 Uiso 0.49(2) 1 calc PR A 2
C3' C -0.1546(12) 0.3005(8) 0.9892(19) 0.045(3) Uiso 0.49(2) 1 d PDU A 2
H3' H -0.1104 0.2772 1.0530 0.054 Uiso 0.49(2) 1 calc PR A 2
C4' C -0.1503(13) 0.3484(7) 1.0208(14) 0.046(3) Uiso 0.49(2) 1 d PDU A 2
H4' H -0.1036 0.3629 1.1058 0.055 Uiso 0.49(2) 1 calc PR A 2
C5' C -0.2301(15) 0.3726(5) 0.901(2) 0.041(3) Uiso 0.49(2) 1 d PDU A 2
H5' H -0.2466 0.4057 0.8913 0.049 Uiso 0.49(2) 1 calc PR A 2
C6 C -0.1279(5) 0.4744(2) 0.7480(8) 0.0466(16) Uani 1 1 d U A .
H6 H -0.1227 0.4827 0.8386 0.056 Uiso 1 1 calc R . .
C7 C -0.2212(6) 0.4524(2) 0.6428(8) 0.0504(16) Uani 1 1 d U A .
H7 H -0.2888 0.4434 0.6510 0.060 Uiso 1 1 calc R . .
C8 C -0.1954(6) 0.4460(2) 0.5233(8) 0.0548(18) Uani 1 1 d U A .
H8 H -0.2427 0.4326 0.4369 0.066 Uiso 1 1 calc R . .
C9 C -0.0859(6) 0.4635(2) 0.5574(8) 0.0548(17) Uani 1 1 d U A .
H9 H -0.0466 0.4629 0.4973 0.066 Uiso 1 1 calc R . .
C10 C -0.0439(6) 0.4820(2) 0.6947(8) 0.0501(17) Uani 1 1 d U A .
H10 H 0.0266 0.4967 0.7418 0.060 Uiso 1 1 calc R . .
C11 C 0.4140(7) 0.2773(3) 0.9907(9) 0.067(2) Uani 1 1 d U . .
H11 H 0.3451 0.2635 0.9318 0.080 Uiso 1 1 calc R . .
C12 C 0.4602(7) 0.2764(3) 1.1381(9) 0.0616(19) Uani 1 1 d U . .
H12 H 0.4279 0.2616 1.1955 0.074 Uiso 1 1 calc R . .
C13 C 0.5642(7) 0.3017(3) 1.1863(9) 0.072(2) Uani 1 1 d U . .
H13 H 0.6121 0.3072 1.2805 0.087 Uiso 1 1 calc R . .
C14 C 0.5822(7) 0.3172(3) 1.0654(9) 0.065(2) Uani 1 1 d U . .
H14 H 0.6452 0.3342 1.0648 0.078 Uiso 1 1 calc R . .
C15 C 0.4894(7) 0.3025(3) 0.9476(9) 0.0631(19) Uani 1 1 d U . .
H15 H 0.4791 0.3085 0.8537 0.076 Uiso 1 1 calc R . .
C16 C 0.5194(5) 0.3883(2) 1.4381(6) 0.0406(15) Uani 1 1 d U . .
H16 H 0.5934 0.3803 1.4494 0.049 Uiso 1 1 calc R . .
C17 C 0.4301(5) 0.3551(2) 1.4162(6) 0.0412(15) Uani 1 1 d U . .
H17 H 0.4348 0.3214 1.4112 0.049 Uiso 1 1 calc R . .
C18 C 0.3333(6) 0.3818(3) 1.4035(6) 0.0506(16) Uani 1 1 d U . .
H18 H 0.2623 0.3690 1.3905 0.061 Uiso 1 1 calc R . .
C19 C 0.3623(6) 0.4313(3) 1.4137(6) 0.0523(17) Uani 1 1 d U . .
H19 H 0.3133 0.4573 1.4049 0.063 Uiso 1 1 calc R . .
C20 C 0.4791(6) 0.4345(3) 1.4398(6) 0.0502(17) Uani 1 1 d U . .
H20 H 0.5215 0.4630 1.4556 0.060 Uiso 1 1 calc R . .
C21 C -0.0252(5) 0.2906(2) 0.8137(6) 0.0408(16) Uani 1 1 d . A .
O21 O 0.0294(4) 0.25828(17) 0.8015(6) 0.0664(15) Uani 1 1 d . . .
C22 C -0.1522(5) 0.3493(2) 0.6293(7) 0.0336(14) Uani 1 1 d . A .
O22 O -0.2063(4) 0.32785(16) 0.5235(5) 0.0519(12) Uani 1 1 d . . .
C23 C 0.3326(5) 0.4549(2) 1.1409(6) 0.0296(13) Uani 1 1 d . . .
O23 O 0.3013(4) 0.49107(15) 1.0823(5) 0.0501(12) Uani 1 1 d . . .
C24 C 0.5027(5) 0.4040(2) 1.1540(6) 0.0327(14) Uani 1 1 d . . .
O24 O 0.5817(4) 0.43026(17) 1.1740(5) 0.0519(12) Uani 1 1 d . . .
C25 C 0.0193(4) 0.38281(19) 0.8938(5) 0.0255(12) Uani 1 1 d U A .
C26 C 0.1150(4) 0.37502(18) 0.8491(5) 0.0219(11) Uani 1 1 d U A .
C27 C 0.0575(4) 0.37499(19) 0.6955(6) 0.0277(12) Uani 1 1 d U A .
C28 C 0.0440(5) 0.4151(2) 1.0238(6) 0.0391(15) Uani 1 1 d U . .
H28A H 0.0801 0.3961 1.1085 0.059 Uiso 1 1 calc R A .
H28B H -0.0261 0.4283 1.0229 0.059 Uiso 1 1 calc R . .
H28C H 0.0936 0.4412 1.0220 0.059 Uiso 1 1 calc R . .
N1 N 0.0932(4) 0.35604(18) 0.6021(5) 0.0339(12) Uani 1 1 d . . .
C30 C 0.0257(6) 0.3611(3) 0.4495(6) 0.0537(19) Uani 1 1 d . A .
H30A H -0.0520 0.3682 0.4343 0.081 Uiso 1 1 calc R . .
H30B H 0.0288 0.3313 0.4021 0.081 Uiso 1 1 calc R . .
H30C H 0.0560 0.3871 0.4120 0.081 Uiso 1 1 calc R . .
C31 C 0.1926(5) 0.3243(3) 0.6386(7) 0.0513(18) Uani 1 1 d . A .
H31A H 0.2540 0.3419 0.6283 0.077 Uiso 1 1 calc R . .
H31B H 0.1736 0.2966 0.5764 0.077 Uiso 1 1 calc R . .
H31C H 0.2154 0.3135 0.7352 0.077 Uiso 1 1 calc R . .
C32 C 0.2806(4) 0.36053(18) 1.0868(5) 0.0235(11) Uani 1 1 d U A .
C33 C 0.2325(4) 0.37823(17) 0.9398(5) 0.0209(11) Uani 1 1 d U . .
C34 C 0.3333(4) 0.38878(19) 0.9142(6) 0.0257(12) Uani 1 1 d U A .
C35 C 0.2168(5) 0.3192(2) 1.1241(6) 0.0374(15) Uani 1 1 d U . .
H35A H 0.1505 0.3320 1.1351 0.056 Uiso 1 1 calc R A .
H35B H 0.2658 0.3042 1.2114 0.056 Uiso 1 1 calc R . .
H35C H 0.1940 0.2954 1.0493 0.056 Uiso 1 1 calc R . .
N2 N 0.3468(4) 0.41890(17) 0.8220(5) 0.0313(11) Uani 1 1 d . . .
C37 C 0.2603(5) 0.4537(2) 0.7361(7) 0.0451(17) Uani 1 1 d . A .
H37A H 0.1964 0.4529 0.7640 0.068 Uiso 1 1 calc R . .
H37B H 0.2355 0.4452 0.6375 0.068 Uiso 1 1 calc R . .
H37C H 0.2922 0.4859 0.7507 0.068 Uiso 1 1 calc R . .
C38 C 0.4566(5) 0.4245(3) 0.8106(7) 0.0527(19) Uani 1 1 d . A .
H38A H 0.5123 0.4047 0.8810 0.079 Uiso 1 1 calc R . .
H38B H 0.4797 0.4580 0.8255 0.079 Uiso 1 1 calc R . .
H38C H 0.4503 0.4146 0.7176 0.079 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0279(5) 0.0339(5) 0.0354(5) 0.0063(4) 0.0075(4) -0.0091(4)
Fe2 0.0234(4) 0.0224(4) 0.0298(5) 0.0006(3) 0.0073(3) -0.0024(3)
Fe3 0.0267(4) 0.0264(4) 0.0267(5) 0.0011(4) 0.0117(3) 0.0052(3)
Fe4 0.0245(4) 0.0262(4) 0.0214(4) 0.0002(3) 0.0074(3) 0.0020(3)
C6 0.042(3) 0.034(3) 0.057(4) -0.005(3) 0.012(3) 0.008(3)
C7 0.037(3) 0.045(4) 0.065(4) 0.014(3) 0.015(3) 0.012(3)
C8 0.051(4) 0.042(4) 0.055(4) 0.015(3) 0.002(3) 0.002(3)
C9 0.064(4) 0.038(3) 0.072(4) 0.019(3) 0.037(4) 0.007(3)
C10 0.040(3) 0.021(3) 0.078(4) 0.004(3) 0.010(3) -0.001(3)
C11 0.075(5) 0.038(4) 0.076(5) -0.010(4) 0.015(4) 0.024(4)
C12 0.080(4) 0.044(4) 0.076(5) 0.019(4) 0.046(4) 0.033(4)
C13 0.074(4) 0.060(4) 0.065(5) -0.005(4) 0.007(4) 0.053(4)
C14 0.053(4) 0.065(4) 0.091(5) 0.003(4) 0.042(4) 0.026(4)
C15 0.089(5) 0.051(4) 0.064(4) 0.000(3) 0.045(4) 0.032(4)
C16 0.035(3) 0.054(4) 0.025(3) -0.009(3) 0.004(3) 0.001(3)
C17 0.054(4) 0.048(4) 0.018(3) 0.003(3) 0.010(3) -0.004(3)
C18 0.049(4) 0.079(4) 0.029(3) 0.005(3) 0.021(3) -0.003(3)
C19 0.064(4) 0.065(4) 0.026(3) 0.002(3) 0.016(3) 0.028(4)
C20 0.059(4) 0.052(4) 0.029(3) -0.007(3) 0.005(3) 0.002(3)
C21 0.047(4) 0.023(3) 0.039(4) 0.005(3) 0.002(3) -0.013(3)
O21 0.072(4) 0.032(3) 0.084(4) -0.002(3) 0.018(3) 0.004(3)
C22 0.026(3) 0.030(3) 0.040(4) 0.002(3) 0.006(3) 0.000(3)
O22 0.056(3) 0.039(3) 0.043(3) -0.006(2) -0.001(2) -0.011(2)
C23 0.029(3) 0.027(3) 0.029(3) -0.007(3) 0.007(3) -0.005(3)
O23 0.055(3) 0.032(3) 0.065(3) 0.012(2) 0.026(3) 0.008(2)
C24 0.028(3) 0.041(4) 0.026(3) 0.010(3) 0.007(2) 0.006(3)
O24 0.039(3) 0.062(3) 0.056(3) -0.004(2) 0.020(2) -0.023(2)
C25 0.024(3) 0.030(3) 0.020(3) -0.004(2) 0.006(2) -0.003(2)
C26 0.022(2) 0.021(2) 0.021(3) 0.002(2) 0.007(2) 0.000(2)
C27 0.029(3) 0.022(3) 0.031(3) 0.001(2) 0.010(2) -0.004(2)
C28 0.026(3) 0.051(4) 0.041(4) -0.018(3) 0.014(3) 0.001(3)
N1 0.036(3) 0.043(3) 0.021(3) -0.005(2) 0.010(2) 0.004(2)
C30 0.061(5) 0.067(5) 0.029(4) -0.005(3) 0.013(3) 0.006(4)
C31 0.054(4) 0.061(5) 0.038(4) -0.005(3) 0.017(3) 0.017(4)
C32 0.026(3) 0.024(3) 0.023(3) 0.004(2) 0.012(2) 0.002(2)
C33 0.024(2) 0.017(2) 0.021(3) 0.000(2) 0.007(2) 0.000(2)
C34 0.025(3) 0.030(3) 0.022(3) -0.002(2) 0.008(2) -0.001(2)
C35 0.033(3) 0.035(3) 0.039(4) 0.005(3) 0.009(3) -0.010(3)
N2 0.029(3) 0.038(3) 0.031(3) 0.010(2) 0.016(2) -0.002(2)
C37 0.042(4) 0.045(4) 0.044(4) 0.020(3) 0.013(3) 0.001(3)
C38 0.036(4) 0.080(5) 0.050(4) 0.014(4) 0.026(3) -0.004(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100858.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100858.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100858
loop_
_publ_author_name
'Busetto, Luigi'
'Marchetti, Fabio'
'Zacchini, Stefano'
'Zanotti, Valerio'
_publ_section_title
;
Deprotonation of \m-Vinyliminium Ligands in Diiron Complexes:  A
Route for the Synthesis of Mono- and Polynuclear Species Containing Novel
Multidentate Ligands
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2297
_journal_page_last 2306
_journal_paper_doi 10.1021/om050095j
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C27 H31 Fe2 N O2 Si'
_chemical_formula_weight 541.32
_space_group_IT_number 41
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'A 2 -2ab'
_symmetry_space_group_name_H-M 'A b a 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 9.920(2)
_cell_length_b 34.927(7)
_cell_length_c 14.849(3)
_cell_measurement_reflns_used 4532
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.9105
_cell_measurement_theta_min 2.333
_cell_volume 5144.6(18)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0769
_diffrn_reflns_av_sigmaI/netI 0.0590
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 22038
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 1.17
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.198
_exptl_absorpt_correction_T_max 0.8502
_exptl_absorpt_correction_T_min 0.7619
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour red-orange
_exptl_crystal_density_diffrn 1.398
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2256
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.14
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.50(3)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 297
_refine_ls_number_reflns 4551
_refine_ls_number_restraints 85
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0692
_refine_ls_R_factor_gt 0.0478
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1113
_refine_ls_wR_factor_ref 0.1212
_reflns_number_gt 3572
_reflns_number_total 4551
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Aba2
_cod_database_code 1100858
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.52566(8) 0.17030(2) 0.07571(6) 0.0367(2) Uani 1 1 d . . .
Fe2 Fe 0.56609(8) 0.17937(2) 0.24100(6) 0.0362(2) Uani 1 1 d . . .
C1 C 0.5226(8) 0.1801(2) -0.0618(5) 0.065(2) Uani 1 1 d D . .
H1 H 0.5783 0.1671 -0.1020 0.079 Uiso 1 1 calc R . .
C2 C 0.5528(7) 0.21498(19) -0.0195(5) 0.0605(19) Uani 1 1 d D . .
H2 H 0.6313 0.2293 -0.0260 0.073 Uiso 1 1 calc R . .
C3 C 0.4433(8) 0.2239(2) 0.0335(5) 0.070(2) Uani 1 1 d D . .
H3 H 0.4348 0.2458 0.0689 0.084 Uiso 1 1 calc R . .
C4 C 0.3467(7) 0.1949(3) 0.0257(6) 0.080(3) Uani 1 1 d D . .
H4 H 0.2641 0.1938 0.0553 0.096 Uiso 1 1 calc R . .
C5 C 0.3964(9) 0.1681(2) -0.0339(6) 0.082(3) Uani 1 1 d D . .
H5 H 0.3527 0.1458 -0.0522 0.098 Uiso 1 1 calc R . .
C6 C 0.5813(10) 0.2381(3) 0.2734(6) 0.048(3) Uiso 0.642(14) 1 d PD A 1
H6 H 0.6196 0.2563 0.2354 0.058 Uiso 0.642(14) 1 calc PR A 1
C7 C 0.6492(10) 0.2165(3) 0.3393(7) 0.050(3) Uiso 0.642(14) 1 d PD A 1
H7 H 0.7398 0.2185 0.3549 0.060 Uiso 0.642(14) 1 calc PR A 1
C8 C 0.5550(14) 0.1918(4) 0.3765(9) 0.066(4) Uiso 0.642(14) 1 d PD A 1
H8 H 0.5747 0.1733 0.4196 0.079 Uiso 0.642(14) 1 calc PR A 1
C9 C 0.4296(14) 0.1981(4) 0.3418(10) 0.069(4) Uiso 0.642(14) 1 d PD A 1
H9 H 0.3504 0.1858 0.3584 0.083 Uiso 0.642(14) 1 calc PR A 1
C10 C 0.4427(11) 0.2271(3) 0.2756(6) 0.045(3) Uiso 0.642(14) 1 d PD A 1
H10 H 0.3739 0.2370 0.2401 0.054 Uiso 0.642(14) 1 calc PR A 1
C6' C 0.495(2) 0.2340(5) 0.2815(14) 0.066(7) Uiso 0.358(14) 1 d PD A 2
H6' H 0.4778 0.2525 0.2378 0.079 Uiso 0.358(14) 1 calc PR A 2
C7' C 0.618(2) 0.2271(6) 0.3237(17) 0.073(8) Uiso 0.358(14) 1 d PD A 2
H7' H 0.6966 0.2413 0.3159 0.088 Uiso 0.358(14) 1 calc PR A 2
C8' C 0.6032(16) 0.1957(5) 0.3791(12) 0.038(5) Uiso 0.358(14) 1 d PD A 2
H8' H 0.6720 0.1841 0.4118 0.046 Uiso 0.358(14) 1 calc PR A 2
C9' C 0.4701(17) 0.1842(4) 0.3783(11) 0.039(5) Uiso 0.358(14) 1 d PD A 2
H9' H 0.4326 0.1645 0.4122 0.047 Uiso 0.358(14) 1 calc PR A 2
C10' C 0.4012(13) 0.2079(5) 0.3166(11) 0.030(5) Uiso 0.358(14) 1 d PD A 2
H10' H 0.3102 0.2065 0.3019 0.036 Uiso 0.358(14) 1 calc PR A 2
C11 C 0.6303(6) 0.13070(17) 0.0549(4) 0.0466(16) Uani 1 1 d . . .
O11 O 0.6986(5) 0.10621(14) 0.0325(3) 0.0686(14) Uani 1 1 d . . .
C12 C 0.6832(7) 0.19020(16) 0.1481(5) 0.0479(16) Uani 1 1 d . A .
O12 O 0.7878(5) 0.20303(14) 0.1282(4) 0.0722(15) Uani 1 1 d . . .
C13 C 0.4516(5) 0.14800(14) 0.1794(4) 0.0324(13) Uani 1 1 d . A .
N1 N 0.3629(5) 0.12174(13) 0.2000(3) 0.0355(11) Uani 1 1 d . . .
C14 C 0.3507(7) 0.1053(2) 0.2926(4) 0.0592(19) Uani 1 1 d . A .
H14A H 0.4378 0.1050 0.3208 0.089 Uiso 1 1 calc R . .
H14B H 0.3162 0.0797 0.2889 0.089 Uiso 1 1 calc R . .
H14C H 0.2902 0.1208 0.3276 0.089 Uiso 1 1 calc R . .
C15 C 0.2585(14) 0.1097(4) 0.1366(10) 0.040(5) Uiso 0.59(2) 1 d PD A 1
C16 C 0.1347(11) 0.1300(4) 0.1351(8) 0.042(4) Uiso 0.59(2) 1 d PD A 1
C17 C 0.0375(12) 0.1174(4) 0.0744(11) 0.057(3) Uiso 0.59(2) 1 d PD A 1
H17 H -0.0452 0.1298 0.0700 0.068 Uiso 0.59(2) 1 calc PR A 1
C18 C 0.0663(13) 0.0861(4) 0.0207(8) 0.049(3) Uiso 0.59(2) 1 d PD A 1
H18 H 0.0007 0.0786 -0.0205 0.058 Uiso 0.59(2) 1 calc PR A 1
C19 C 0.1837(16) 0.0650(4) 0.0230(8) 0.053(4) Uiso 0.59(2) 1 d PD A 1
H19 H 0.1961 0.0433 -0.0125 0.064 Uiso 0.59(2) 1 calc PR A 1
C20 C 0.2820(14) 0.0780(4) 0.0814(9) 0.048(4) Uiso 0.59(2) 1 d PD A 1
C21 C 0.4070(16) 0.0545(4) 0.0884(12) 0.071(4) Uiso 0.59(2) 1 d PD A 1
H21A H 0.3889 0.0290 0.0674 0.106 Uiso 0.59(2) 1 calc PR A 1
H21B H 0.4357 0.0535 0.1501 0.106 Uiso 0.59(2) 1 calc PR A 1
H21C H 0.4767 0.0658 0.0523 0.106 Uiso 0.59(2) 1 calc PR A 1
C22 C 0.1089(14) 0.1617(4) 0.1984(11) 0.060(4) Uiso 0.59(2) 1 d PD A 1
H22A H 0.1931 0.1711 0.2215 0.090 Uiso 0.59(2) 1 calc PR A 1
H22B H 0.0543 0.1527 0.2474 0.090 Uiso 0.59(2) 1 calc PR A 1
H22C H 0.0626 0.1820 0.1676 0.090 Uiso 0.59(2) 1 calc PR A 1
C15' C 0.2764(16) 0.1038(5) 0.1339(12) 0.027(6) Uiso 0.41(2) 1 d PD A 2
C16' C 0.1454(13) 0.1194(5) 0.1207(11) 0.035(5) Uiso 0.41(2) 1 d PD A 2
C17' C 0.0629(14) 0.1036(5) 0.0542(11) 0.039(4) Uiso 0.41(2) 1 d PD A 2
H17' H -0.0201 0.1143 0.0393 0.047 Uiso 0.41(2) 1 calc PR A 2
C18' C 0.1113(18) 0.0714(5) 0.0119(10) 0.044(5) Uiso 0.41(2) 1 d PD A 2
H18' H 0.0558 0.0600 -0.0308 0.053 Uiso 0.41(2) 1 calc PR A 2
C19' C 0.235(2) 0.0545(5) 0.0272(10) 0.051(5) Uiso 0.41(2) 1 d PD A 2
H19' H 0.2621 0.0329 -0.0049 0.061 Uiso 0.41(2) 1 calc PR A 2
C20' C 0.3174(16) 0.0707(4) 0.0914(9) 0.030(4) Uiso 0.41(2) 1 d PD A 2
C21' C 0.4486(17) 0.0523(4) 0.1136(13) 0.044(4) Uiso 0.41(2) 1 d PD A 2
H21D H 0.4328 0.0271 0.1374 0.067 Uiso 0.41(2) 1 calc PR A 2
H21E H 0.4952 0.0674 0.1577 0.067 Uiso 0.41(2) 1 calc PR A 2
H21F H 0.5025 0.0504 0.0601 0.067 Uiso 0.41(2) 1 calc PR A 2
C22' C 0.094(2) 0.1529(6) 0.1717(17) 0.065(6) Uiso 0.41(2) 1 d PD A 2
H22D H -0.0012 0.1505 0.1800 0.097 Uiso 0.41(2) 1 calc PR A 2
H22E H 0.1134 0.1759 0.1387 0.097 Uiso 0.41(2) 1 calc PR A 2
H22F H 0.1380 0.1540 0.2293 0.097 Uiso 0.41(2) 1 calc PR A 2
C23 C 0.6696(5) 0.13487(15) 0.2621(4) 0.0373(14) Uani 1 1 d . A .
C24 C 0.7339(6) 0.10480(16) 0.2734(4) 0.0473(16) Uani 1 1 d . . .
Si1 Si 0.81128(18) 0.05828(5) 0.28554(13) 0.0462(4) Uani 1 1 d . A .
C25 C 0.978(2) 0.0594(7) 0.3346(16) 0.063(6) Uiso 0.51(4) 1 d P A 1
H25A H 0.9843 0.0804 0.3761 0.095 Uiso 0.51(4) 1 calc PR A 1
H25B H 1.0440 0.0625 0.2878 0.095 Uiso 0.51(4) 1 calc PR A 1
H25C H 0.9946 0.0358 0.3661 0.095 Uiso 0.51(4) 1 calc PR A 1
C26 C 0.730(2) 0.0316(5) 0.3808(16) 0.062(6) Uiso 0.51(4) 1 d P A 1
H26A H 0.7690 0.0064 0.3849 0.094 Uiso 0.51(4) 1 calc PR A 1
H26B H 0.6353 0.0295 0.3701 0.094 Uiso 0.51(4) 1 calc PR A 1
H26C H 0.7457 0.0451 0.4361 0.094 Uiso 0.51(4) 1 calc PR A 1
C27 C 0.825(2) 0.0345(6) 0.1670(15) 0.055(5) Uiso 0.51(4) 1 d P A 1
H27A H 0.8699 0.0517 0.1263 0.082 Uiso 0.51(4) 1 calc PR A 1
H27B H 0.7367 0.0289 0.1446 0.082 Uiso 0.51(4) 1 calc PR A 1
H27C H 0.8762 0.0112 0.1716 0.082 Uiso 0.51(4) 1 calc PR A 1
C25' C 0.997(2) 0.0670(7) 0.3213(16) 0.063(7) Uiso 0.49(4) 1 d P A 2
H25D H 1.0461 0.0433 0.3180 0.094 Uiso 0.49(4) 1 calc PR A 2
H25E H 0.9994 0.0765 0.3819 0.094 Uiso 0.49(4) 1 calc PR A 2
H25F H 1.0375 0.0854 0.2816 0.094 Uiso 0.49(4) 1 calc PR A 2
C26' C 0.694(2) 0.0268(5) 0.3506(16) 0.054(5) Uiso 0.49(4) 1 d P A 2
H26D H 0.6029 0.0311 0.3306 0.081 Uiso 0.49(4) 1 calc PR A 2
H26E H 0.7006 0.0327 0.4136 0.081 Uiso 0.49(4) 1 calc PR A 2
H26F H 0.7174 0.0005 0.3409 0.081 Uiso 0.49(4) 1 calc PR A 2
C27' C 0.804(2) 0.0298(7) 0.1869(18) 0.064(7) Uiso 0.49(4) 1 d P A 2
H27D H 0.7748 0.0044 0.2023 0.096 Uiso 0.49(4) 1 calc PR A 2
H27E H 0.8922 0.0285 0.1600 0.096 Uiso 0.49(4) 1 calc PR A 2
H27F H 0.7421 0.0409 0.1449 0.096 Uiso 0.49(4) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0325(4) 0.0363(4) 0.0413(4) 0.0070(4) -0.0021(4) 0.0002(3)
Fe2 0.0328(4) 0.0288(3) 0.0471(5) -0.0049(4) -0.0096(4) 0.0032(3)
C1 0.075(5) 0.062(5) 0.059(5) -0.009(4) 0.010(4) 0.002(4)
C2 0.072(5) 0.054(4) 0.055(4) 0.023(3) 0.004(4) 0.013(4)
C3 0.096(6) 0.052(4) 0.062(5) 0.027(4) 0.016(4) 0.036(4)
C4 0.038(4) 0.121(7) 0.082(6) 0.061(6) -0.002(4) 0.026(5)
C5 0.076(6) 0.086(6) 0.082(6) 0.015(5) -0.054(5) -0.012(5)
C11 0.045(4) 0.053(4) 0.042(4) -0.003(3) -0.004(3) -0.004(3)
O11 0.064(3) 0.077(3) 0.065(3) -0.008(3) 0.005(3) 0.022(3)
C12 0.048(4) 0.028(3) 0.068(5) 0.005(3) -0.014(3) 0.003(3)
O12 0.038(3) 0.077(3) 0.102(4) 0.016(3) -0.005(3) -0.031(3)
C13 0.024(3) 0.029(3) 0.044(4) -0.002(2) -0.003(2) 0.006(2)
N1 0.035(3) 0.037(3) 0.034(2) 0.000(2) 0.001(2) -0.005(2)
C14 0.062(4) 0.078(5) 0.038(4) 0.011(3) 0.001(3) -0.029(4)
C23 0.036(3) 0.035(3) 0.041(4) 0.000(2) -0.012(2) -0.004(2)
C24 0.046(3) 0.037(3) 0.059(4) 0.003(3) -0.004(3) 0.010(3)
Si1 0.0432(9) 0.0368(9) 0.0586(11) 0.0083(8) 0.0006(8) 0.0072(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100859.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100859.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100859
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C21 H24 Au Cl N2'
_chemical_formula_weight 536.84
_space_group_IT_number 43
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'F 2 -2d'
_symmetry_space_group_name_H-M 'F d d 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 14.7275(5)
_cell_length_b 28.8178(9)
_cell_length_c 9.7016(3)
_cell_measurement_reflns_used 18538
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 35.068
_cell_measurement_theta_min 2.612
_cell_volume 4117.5(2)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0295
_diffrn_reflns_av_sigmaI/netI 0.0198
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 45
_diffrn_reflns_limit_k_min -45
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 21578
_diffrn_reflns_theta_max 35.10
_diffrn_reflns_theta_min 2.61
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 7.281
_exptl_absorpt_correction_T_max 0.892117
_exptl_absorpt_correction_T_min 0.627756
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.732
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 2080
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.057(6)
_refine_ls_extinction_coef 0.000122(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 164
_refine_ls_number_reflns 4415
_refine_ls_number_restraints 106
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0184
_refine_ls_R_factor_gt 0.0161
_refine_ls_shift/su_max 0.018
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+11.6731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0387
_refine_ls_wR_factor_ref 0.0396
_reflns_number_gt 4093
_reflns_number_total 4415
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Fdd2
_cod_database_code 1100859
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.0000 0.0000 0.73805(2) 0.01692(3) Uani 1 2 d SU . .
C1 C 0.0000 0.0000 0.5320(5) 0.0172(7) Uani 1 2 d SU . .
Cl1 Cl 0.0000 0.0000 0.97263(12) 0.0285(3) Uani 1 2 d SU . .
N2 N 0.05778(12) -0.02277(6) 0.44997(18) 0.0175(3) Uani 1 1 d U . .
C3 C 0.03656(15) -0.01455(8) 0.3127(2) 0.0207(3) Uani 1 1 d U . .
H3 H 0.0694(19) -0.0280(10) 0.231(3) 0.016(6) Uiso 1 1 d . . .
C4 C 0.13181(13) -0.05051(7) 0.5009(2) 0.0175(3) Uani 1 1 d U . .
C5 C 0.11634(14) -0.09706(8) 0.5314(2) 0.0197(3) Uani 1 1 d U . .
C6 C 0.18719(16) -0.12222(8) 0.5914(3) 0.0242(4) Uani 1 1 d U . .
H6 H 0.180(2) -0.1539(12) 0.609(4) 0.023(8) Uiso 1 1 d . . .
C7 C 0.27123(16) -0.10150(9) 0.6179(3) 0.0260(4) Uani 1 1 d U . .
C8 C 0.28441(16) -0.05564(9) 0.5823(3) 0.0257(4) Uani 1 1 d U . .
H8 H 0.336(3) -0.0436(14) 0.597(4) 0.037(10) Uiso 1 1 d . . .
C9 C 0.21526(16) -0.02875(8) 0.5239(2) 0.0223(4) Uani 1 1 d U . .
C10 C 0.02676(17) -0.11994(9) 0.5004(3) 0.0288(5) Uani 1 1 d U . .
H10A H 0.012(3) -0.118(2) 0.409(7) 0.059(15) Uiso 1 1 d . . .
H10B H -0.025(3) -0.0988(17) 0.531(5) 0.053(13) Uiso 1 1 d . . .
H10C H 0.023(3) -0.1480(19) 0.522(6) 0.058(14) Uiso 1 1 d . . .
C11 C 0.3464(2) -0.12882(14) 0.6860(4) 0.0403(7) Uani 1 1 d U . .
H11A H 0.333(4) -0.1398(17) 0.759(7) 0.064(16) Uiso 1 1 d . . .
H11B H 0.397(4) -0.1129(18) 0.704(6) 0.070(17) Uiso 1 1 d . . .
H11C H 0.358(5) -0.153(3) 0.639(7) 0.11(2) Uiso 1 1 d . . .
C12 C 0.23062(18) 0.02139(9) 0.4892(6) 0.0368(6) Uani 1 1 d U . .
H12C H 0.212(3) 0.0284(15) 0.398(5) 0.045(11) Uiso 1 1 d . . .
H12B H 0.200(4) 0.0453(18) 0.562(6) 0.065(15) Uiso 1 1 d . . .
H11A H 0.297(2) 0.0303(12) 0.504(5) 0.023(8) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01845(4) 0.02242(4) 0.00989(4) 0.000 0.000 0.00178(5)
C1 0.0177(13) 0.0156(13) 0.0183(18) 0.000 0.000 0.0003(8)
Cl1 0.0304(5) 0.0421(6) 0.0129(4) 0.000 0.000 -0.0013(3)
N2 0.0192(7) 0.0219(7) 0.0114(6) 0.0003(5) -0.0001(5) 0.0026(6)
C3 0.0250(9) 0.0262(9) 0.0110(7) -0.0003(7) 0.0007(7) 0.0054(8)
C4 0.0179(7) 0.0214(7) 0.0133(8) 0.0001(6) 0.0008(6) 0.0024(6)
C5 0.0189(8) 0.0225(8) 0.0177(8) 0.0010(6) -0.0003(6) -0.0001(6)
C6 0.0229(9) 0.0227(9) 0.0271(11) 0.0028(8) -0.0010(8) 0.0021(7)
C7 0.0215(9) 0.0307(11) 0.0257(11) 0.0025(8) -0.0037(8) 0.0053(8)
C8 0.0182(9) 0.0309(10) 0.0282(11) -0.0006(8) -0.0041(8) -0.0017(8)
C9 0.0205(9) 0.0229(9) 0.0235(10) 0.0002(7) -0.0002(7) -0.0025(7)
C10 0.0240(9) 0.0296(10) 0.0329(13) 0.0031(10) -0.0055(10) -0.0051(8)
C11 0.0298(13) 0.0454(16) 0.0458(17) 0.0104(14) -0.0112(12) 0.0081(12)
C12 0.0303(13) 0.0235(9) 0.0565(18) 0.0032(15) -0.003(2) -0.0045(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100860.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100860.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100860
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C21 H26 Au Cl N2'
_chemical_formula_weight 538.85
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 91.0600(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.4242(3)
_cell_length_b 21.9330(9)
_cell_length_c 11.2534(5)
_cell_measurement_reflns_used 25014
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 35.672
_cell_measurement_theta_min 2.417
_cell_volume 2078.91(15)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0325
_diffrn_reflns_av_sigmaI/netI 0.0152
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 24387
_diffrn_reflns_theta_max 22.50
_diffrn_reflns_theta_min 1.86
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 7.210
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.116724
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.722
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1048
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.12
_refine_ls_extinction_coef 0.00033(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.187
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 233
_refine_ls_number_reflns 2701
_refine_ls_number_restraints 217
_refine_ls_restrained_S_all 1.144
_refine_ls_R_factor_all 0.0179
_refine_ls_R_factor_gt 0.0173
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+3.7440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0438
_refine_ls_wR_factor_ref 0.0441
_reflns_number_gt 2619
_reflns_number_total 2701
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100860
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.448060(17) 0.194101(6) 0.032337(13) 0.03299(8) Uani 1 1 d U . .
Cl1 Cl 0.19950(12) 0.17306(5) -0.03919(10) 0.0493(3) Uani 1 1 d U . .
N1 N 0.7422(4) 0.26304(14) 0.0871(3) 0.0339(7) Uani 1 1 d U . .
C1 C 0.6618(4) 0.21145(17) 0.1011(3) 0.0318(8) Uani 1 1 d U . .
N2 N 0.7451(4) 0.17402(14) 0.1727(3) 0.0336(7) Uani 1 1 d U . .
C2 C 0.8930(5) 0.26371(18) 0.1558(4) 0.0392(9) Uani 1 1 d U . .
H2A H 0.8904 0.2942 0.2205 0.047 Uiso 1 1 calc R . .
H2B H 0.9839 0.2726 0.1040 0.047 Uiso 1 1 calc R . .
C3 C 0.9027(5) 0.19915(17) 0.2052(4) 0.0366(9) Uani 1 1 d U . .
H3A H 0.9889 0.1757 0.1678 0.044 Uiso 1 1 calc R . .
H3B H 0.9201 0.1994 0.2925 0.044 Uiso 1 1 calc R . .
C4 C 0.7007(5) 0.31246(16) 0.0070(3) 0.0332(8) Uani 1 1 d U . .
C5 C 0.6166(5) 0.36239(17) 0.0471(3) 0.0382(9) Uani 1 1 d U . .
C6 C 0.5942(5) 0.41123(19) -0.0313(4) 0.0439(10) Uani 1 1 d U . .
H6 H 0.5358 0.4457 -0.0057 0.053 Uiso 1 1 calc R . .
C7 C 0.6541(5) 0.41102(18) -0.1446(4) 0.0421(9) Uani 1 1 d U . .
C8 C 0.7360(5) 0.36000(18) -0.1816(3) 0.0374(9) Uani 1 1 d U . .
H8 H 0.7789 0.3596 -0.2591 0.045 Uiso 1 1 calc R . .
C9 C 0.7576(5) 0.30936(17) -0.1093(4) 0.0350(9) Uani 1 1 d U . .
C10 C 0.8334(5) 0.25213(19) -0.1556(4) 0.0451(10) Uani 1 1 d U . .
H10A H 0.7524 0.2204 -0.1658 0.068 Uiso 1 1 calc R . .
H10B H 0.9151 0.2381 -0.0988 0.068 Uiso 1 1 calc R . .
H10C H 0.8822 0.2606 -0.2322 0.068 Uiso 1 1 calc R . .
C11 C 0.6298(6) 0.4648(2) -0.2277(4) 0.0605(13) Uani 1 1 d U . .
H11A H 0.5164 0.4746 -0.2337 0.091 Uiso 1 1 calc R . .
H11B H 0.6690 0.4544 -0.3066 0.091 Uiso 1 1 calc R . .
H11C H 0.6882 0.5001 -0.1966 0.091 Uiso 1 1 calc R . .
C12 C 0.5462(6) 0.3643(2) 0.1702(4) 0.0533(12) Uani 1 1 d U . .
H12A H 0.4381 0.3479 0.1668 0.080 Uiso 1 1 calc R . .
H12B H 0.5436 0.4066 0.1984 0.080 Uiso 1 1 calc R . .
H12C H 0.6116 0.3397 0.2249 0.080 Uiso 1 1 calc R . .
C13 C 0.7006(4) 0.11230(17) 0.2007(3) 0.0346(8) Uani 1 1 d U . .
C14 C 0.7067(5) 0.06749(17) 0.1115(3) 0.0382(9) Uani 1 1 d U . .
C15 C 0.6584(5) 0.00865(18) 0.1410(4) 0.0438(10) Uani 1 1 d U . .
H15 H 0.6593 -0.0221 0.0816 0.053 Uiso 1 1 calc R . .
C16 C 0.6089(5) -0.00641(18) 0.2542(4) 0.0417(9) Uani 1 1 d U . .
C17 C 0.6122(5) 0.03844(18) 0.3406(4) 0.0415(9) Uani 1 1 d U . .
H17 H 0.5824 0.0281 0.4191 0.050 Uiso 1 1 calc R . .
C18 C 0.6578(5) 0.09839(17) 0.3169(3) 0.0360(9) Uani 1 1 d U . .
C19 C 0.6619(5) 0.14522(19) 0.4150(4) 0.0433(10) Uani 1 1 d U . .
H19A H 0.7675 0.1456 0.4530 0.065 Uiso 1 1 calc R . .
H19B H 0.5822 0.1349 0.4741 0.065 Uiso 1 1 calc R . .
H19C H 0.6386 0.1856 0.3816 0.065 Uiso 1 1 calc R . .
C20 C 0.5522(6) -0.06994(19) 0.2823(4) 0.0552(12) Uani 1 1 d U . .
H20A H 0.5976 -0.0830 0.3590 0.083 Uiso 1 1 calc R . .
H20B H 0.5859 -0.0980 0.2200 0.083 Uiso 1 1 calc R . .
H20C H 0.4360 -0.0701 0.2863 0.083 Uiso 1 1 calc R . .
C21 C 0.7657(6) 0.0815(2) -0.0111(4) 0.0507(11) Uani 1 1 d U . .
H21A H 0.7839 0.0433 -0.0539 0.076 Uiso 1 1 calc R . .
H21B H 0.8654 0.1044 -0.0046 0.076 Uiso 1 1 calc R . .
H21C H 0.6863 0.1059 -0.0545 0.076 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.03464(11) 0.03313(11) 0.03118(11) 0.00081(6) 0.00042(7) 0.00059(6)
Cl1 0.0370(6) 0.0642(7) 0.0467(6) -0.0043(5) -0.0049(5) -0.0017(5)
N1 0.0369(17) 0.0301(16) 0.0345(17) 0.0033(13) -0.0022(13) -0.0005(13)
C1 0.036(2) 0.0319(19) 0.0274(19) -0.0015(16) 0.0047(15) 0.0014(16)
N2 0.0349(17) 0.0282(16) 0.0378(18) 0.0024(14) 0.0004(14) 0.0003(13)
C2 0.039(2) 0.037(2) 0.042(2) 0.0035(18) -0.0056(17) -0.0028(17)
C3 0.034(2) 0.040(2) 0.036(2) 0.0041(17) -0.0029(17) -0.0007(16)
C4 0.034(2) 0.0280(19) 0.038(2) 0.0050(15) -0.0035(16) -0.0041(15)
C5 0.045(2) 0.033(2) 0.037(2) 0.0020(16) -0.0015(17) -0.0012(17)
C6 0.051(2) 0.030(2) 0.051(2) 0.0027(17) 0.0036(19) 0.0036(18)
C7 0.048(2) 0.036(2) 0.042(2) 0.0076(17) -0.0037(18) -0.0056(18)
C8 0.036(2) 0.042(2) 0.035(2) 0.0068(17) -0.0006(17) -0.0052(17)
C9 0.031(2) 0.035(2) 0.039(2) 0.0032(16) -0.0001(17) -0.0043(15)
C10 0.050(3) 0.044(2) 0.042(2) 0.0023(19) 0.0073(19) 0.004(2)
C11 0.079(3) 0.044(3) 0.058(3) 0.019(2) 0.001(3) 0.003(2)
C12 0.070(3) 0.045(3) 0.045(2) 0.004(2) 0.011(2) 0.014(2)
C13 0.035(2) 0.0291(19) 0.040(2) 0.0030(16) -0.0010(17) 0.0035(16)
C14 0.044(2) 0.033(2) 0.038(2) 0.0003(16) 0.0005(17) 0.0044(17)
C15 0.051(2) 0.033(2) 0.047(2) -0.0056(18) -0.0040(19) 0.0034(18)
C16 0.044(2) 0.031(2) 0.050(2) 0.0061(17) -0.0018(19) 0.0038(18)
C17 0.047(2) 0.038(2) 0.040(2) 0.0085(17) 0.0039(18) 0.0022(18)
C18 0.036(2) 0.035(2) 0.037(2) 0.0051(16) -0.0007(17) 0.0064(17)
C19 0.049(2) 0.042(2) 0.040(2) 0.0012(18) 0.0049(19) 0.001(2)
C20 0.066(3) 0.034(2) 0.066(3) 0.007(2) 0.003(2) 0.001(2)
C21 0.072(3) 0.041(2) 0.039(2) -0.0063(19) 0.006(2) 0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100861.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100861.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100861
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C27 H38 Au Cl N2'
_chemical_formula_weight 623.01
_space_group_IT_number 56
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ab 2ac'
_symmetry_space_group_name_H-M 'P c c n'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.9098(5)
_cell_length_b 12.5994(6)
_cell_length_c 19.3635(9)
_cell_measurement_reflns_used 26455
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 30.517
_cell_measurement_theta_min 2.104
_cell_volume 2661.6(2)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0378
_diffrn_reflns_av_sigmaI/netI 0.0164
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 42383
_diffrn_reflns_theta_max 30.52
_diffrn_reflns_theta_min 2.68
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.643
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.317014
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.555
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1240
_exptl_crystal_size_max 0.7
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.25
_refine_ls_extinction_coef 0.00066(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 147
_refine_ls_number_reflns 4060
_refine_ls_number_restraints 130
_refine_ls_restrained_S_all 1.046
_refine_ls_R_factor_all 0.0263
_refine_ls_R_factor_gt 0.0187
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+2.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0426
_refine_ls_wR_factor_ref 0.0467
_reflns_number_gt 3276
_reflns_number_total 4060
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M Pccn
_cod_database_code 1100861
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.7500 0.2500 0.278399(4) 0.02355(4) Uani 1 2 d SU . .
Cl1 Cl 0.7500 0.2500 0.16086(4) 0.0473(2) Uani 1 2 d SU . .
C1 C 0.7500 0.2500 0.38075(12) 0.0207(4) Uani 1 2 d SU . .
N1 N 0.78298(15) 0.16876(12) 0.42063(8) 0.0232(3) Uani 1 1 d U . .
C2 C 0.77768(17) 0.19399(14) 0.49540(9) 0.0242(4) Uani 1 1 d U . .
H2A H 0.8604 0.1936 0.5164 0.029 Uiso 1 1 calc R . .
H2B H 0.7246 0.1433 0.5205 0.029 Uiso 1 1 calc R . .
C3 C 0.82662(17) 0.06895(13) 0.39486(9) 0.0230(3) Uani 1 1 d U . .
C4 C 0.74169(18) -0.01134(15) 0.38034(10) 0.0288(4) Uani 1 1 d U . .
C5 C 0.7873(2) -0.10597(16) 0.35284(12) 0.0368(5) Uani 1 1 d U . .
H5 H 0.7319 -0.1611 0.3408 0.044 Uiso 1 1 calc R . .
C6 C 0.9113(2) -0.12081(16) 0.34280(12) 0.0383(5) Uani 1 1 d U . .
H6 H 0.9403 -0.1860 0.3243 0.046 Uiso 1 1 calc R . .
C7 C 0.9935(2) -0.04136(16) 0.35948(11) 0.0345(4) Uani 1 1 d U . .
H7 H 1.0788 -0.0531 0.3533 0.041 Uiso 1 1 calc R . .
C8 C 0.95284(18) 0.05581(15) 0.38531(10) 0.0276(4) Uani 1 1 d U . .
C9 C 1.04347(19) 0.14426(16) 0.39964(11) 0.0330(4) Uani 1 1 d U . .
H9 H 0.9988 0.2014 0.4252 0.040 Uiso 1 1 calc R . .
C10 C 1.0899(2) 0.1922(2) 0.33181(13) 0.0454(6) Uani 1 1 d U . .
H10A H 1.1399 0.1397 0.3073 0.068 Uiso 1 1 calc R . .
H10B H 1.1396 0.2551 0.3418 0.068 Uiso 1 1 calc R . .
H10C H 1.0199 0.2124 0.3030 0.068 Uiso 1 1 calc R . .
C11 C 1.1493(3) 0.1078(2) 0.44499(15) 0.0558(7) Uani 1 1 d U . .
H11A H 1.1169 0.0774 0.4878 0.084 Uiso 1 1 calc R . .
H11B H 1.2019 0.1686 0.4560 0.084 Uiso 1 1 calc R . .
H11C H 1.1973 0.0540 0.4204 0.084 Uiso 1 1 calc R . .
C12 C 0.60563(19) 0.00121(17) 0.39298(12) 0.0350(4) Uani 1 1 d U . .
H12 H 0.5935 0.0686 0.4194 0.042 Uiso 1 1 calc R . .
C13 C 0.5347(3) 0.0116(2) 0.32485(14) 0.0544(7) Uani 1 1 d U . .
H13A H 0.5668 0.0719 0.2985 0.082 Uiso 1 1 calc R . .
H13B H 0.4476 0.0230 0.3347 0.082 Uiso 1 1 calc R . .
H13C H 0.5445 -0.0536 0.2978 0.082 Uiso 1 1 calc R . .
C14 C 0.5538(2) -0.0892(2) 0.43656(14) 0.0490(6) Uani 1 1 d U . .
H14A H 0.5635 -0.1564 0.4117 0.073 Uiso 1 1 calc R . .
H14B H 0.4666 -0.0763 0.4454 0.073 Uiso 1 1 calc R . .
H14C H 0.5979 -0.0928 0.4806 0.073 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.02730(6) 0.02596(6) 0.01740(5) 0.000 0.000 -0.00346(4)
Cl1 0.0612(5) 0.0622(5) 0.0184(3) 0.000 0.000 -0.0228(4)
C1 0.0213(10) 0.0192(9) 0.0217(10) 0.000 0.000 -0.0039(9)
N1 0.0316(8) 0.0198(7) 0.0183(6) -0.0002(5) -0.0007(6) 0.0018(5)
C2 0.0336(10) 0.0212(8) 0.0179(7) 0.0008(6) 0.0003(6) -0.0008(6)
C3 0.0317(9) 0.0179(7) 0.0193(7) 0.0018(6) 0.0016(6) 0.0014(6)
C4 0.0335(9) 0.0236(8) 0.0294(8) -0.0039(7) 0.0025(8) -0.0024(7)
C5 0.0447(11) 0.0226(9) 0.0432(12) -0.0092(8) 0.0094(9) -0.0038(8)
C6 0.0492(12) 0.0216(8) 0.0441(12) -0.0036(8) 0.0162(10) 0.0037(8)
C7 0.0359(11) 0.0272(9) 0.0403(11) 0.0036(8) 0.0130(9) 0.0058(8)
C8 0.0328(9) 0.0231(8) 0.0269(9) 0.0044(7) 0.0051(7) -0.0018(7)
C9 0.0306(10) 0.0292(9) 0.0393(11) 0.0055(8) 0.0036(8) -0.0037(8)
C10 0.0321(11) 0.0498(14) 0.0544(14) 0.0224(12) -0.0019(10) -0.0107(10)
C11 0.0557(16) 0.0546(16) 0.0570(16) 0.0195(13) -0.0208(13) -0.0161(13)
C12 0.0311(10) 0.0336(10) 0.0404(11) -0.0115(9) 0.0006(8) -0.0033(8)
C13 0.0454(14) 0.0648(17) 0.0531(16) -0.0020(13) -0.0140(12) -0.0064(13)
C14 0.0444(13) 0.0498(14) 0.0527(14) -0.0066(12) 0.0155(11) -0.0089(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100862.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100862.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100862
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C11 H20 Au Cl N2'
_chemical_formula_weight 412.71
_space_group_IT_number 96
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4nw 2abw'
_symmetry_space_group_name_H-M 'P 43 21 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.0840(3)
_cell_length_b 8.0840(3)
_cell_length_c 20.6310(15)
_cell_measurement_reflns_used 19915
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 34.785
_cell_measurement_theta_min 2.520
_cell_volume 1348.26(12)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0463
_diffrn_reflns_av_sigmaI/netI 0.0234
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 8694
_diffrn_reflns_theta_full 22.49
_diffrn_reflns_theta_max 22.49
_diffrn_reflns_theta_min 2.71
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 11.083
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.392856
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.033
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 784
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.189
_refine_diff_density_min -0.851
_refine_diff_density_rms 0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.06(2)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.155
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 110
_refine_ls_number_reflns 889
_refine_ls_number_restraints 53
_refine_ls_restrained_S_all 1.123
_refine_ls_R_factor_all 0.0206
_refine_ls_R_factor_gt 0.0201
_refine_ls_shift/su_max 0.060
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+8.4025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0494
_refine_ls_wR_factor_ref 0.0497
_reflns_number_gt 878
_reflns_number_total 889
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P4(3)2(1)2
_cod_database_code 1100862
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.10776(3) 0.10776(3) 0.0000 0.01354(14) Uani 1 2 d SU . .
Cl1 Cl -0.0916(2) -0.0916(2) 0.0000 0.0204(5) Uani 1 2 d SU . .
C1 C 0.2823(8) 0.2823(8) 0.0000 0.0145(18) Uani 1 2 d SU . .
N1 N 0.2952(8) 0.4120(8) 0.0408(3) 0.0166(13) Uani 1 1 d U . .
C2 C 0.4346(9) 0.5059(9) 0.0257(3) 0.0217(18) Uani 1 1 d U . .
C3 C 0.4816(14) 0.6608(11) 0.0618(4) 0.032(2) Uani 1 1 d U . .
H3A H 0.606(16) 0.685(13) 0.051(5) 0.07(4) Uiso 1 1 d . . .
H3B H 0.488(14) 0.629(13) 0.110(6) 0.07(4) Uiso 1 1 d . . .
H3C H 0.373(12) 0.748(11) 0.059(4) 0.05(3) Uiso 1 1 d . . .
C4 C 0.1780(11) 0.4526(9) 0.0941(3) 0.0223(17) Uani 1 1 d U . .
H4 H 0.231(9) 0.544(10) 0.114(3) 0.010(18) Uiso 1 1 d . . .
C5 C 0.1651(12) 0.3105(12) 0.1430(4) 0.0246(19) Uani 1 1 d U . .
H5A H 0.127(9) 0.214(10) 0.124(4) 0.01(2) Uiso 1 1 d . . .
H5B H 0.099(13) 0.345(12) 0.177(5) 0.05(3) Uiso 1 1 d . . .
H5C H 0.264(11) 0.280(10) 0.157(4) 0.02(2) Uiso 1 1 d . . .
C6 C 0.0121(12) 0.5001(12) 0.0670(5) 0.032(2) Uani 1 1 d U . .
H6A H 0.030(9) 0.587(11) 0.049(3) 0.01(2) Uiso 1 1 d . . .
H6B H -0.087(11) 0.513(11) 0.101(4) 0.04(2) Uiso 1 1 d . . .
H6C H -0.046(11) 0.415(13) 0.048(4) 0.03(3) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01557(16) 0.01557(16) 0.00949(19) -0.00243(16) 0.00243(16) -0.00103(17)
Cl1 0.0192(8) 0.0192(8) 0.0228(12) 0.0043(11) -0.0043(11) -0.0027(11)
C1 0.020(3) 0.020(3) 0.003(4) -0.004(3) 0.004(3) -0.003(3)
N1 0.026(3) 0.016(3) 0.007(3) -0.002(2) 0.002(2) -0.005(2)
C2 0.030(4) 0.024(4) 0.011(3) 0.002(3) -0.005(3) -0.011(3)
C3 0.054(6) 0.028(5) 0.014(4) 0.002(3) 0.001(4) -0.018(5)
C4 0.040(4) 0.016(4) 0.010(3) -0.008(3) 0.005(3) -0.004(3)
C5 0.029(5) 0.034(5) 0.012(4) 0.003(3) 0.004(4) -0.002(4)
C6 0.042(5) 0.014(5) 0.038(5) 0.005(4) 0.008(4) 0.007(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Cl1 180.0 . . ?
N1 C1 N1 105.6(8) . 7 ?
N1 C1 Au1 127.2(4) . . ?
N1 C1 Au1 127.2(4) 7 . ?
C1 N1 C2 110.3(6) . . ?
C1 N1 C4 125.7(6) . . ?
C2 N1 C4 124.0(6) . . ?
C2 C2 N1 106.9(4) 7 . ?
C2 C2 C3 129.9(5) 7 . ?
N1 C2 C3 123.1(7) . . ?
N1 C4 C6 110.4(6) . . ?
N1 C4 C5 111.4(7) . . ?
C6 C4 C5 112.1(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 1.995(9) . ?
Au1 Cl1 2.279(2) . ?
C1 N1 1.348(9) . ?
C1 N1 1.348(9) 7 ?
N1 C2 1.393(9) . ?
N1 C4 1.489(10) . ?
C2 C2 1.337(15) 7 ?
C2 C3 1.506(11) . ?
C4 C6 1.503(12) . ?
C4 C5 1.532(11) . ?
|
1100863.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100863.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100863
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C7 H12 Au Cl N2'
_chemical_formula_weight 356.60
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.405(2)
_cell_length_b 8.4073(18)
_cell_length_c 11.068(2)
_cell_measurement_reflns_used 8143
_cell_measurement_temperature 396(2)
_cell_measurement_theta_max 30.714
_cell_measurement_theta_min 2.423
_cell_volume 968.3(4)
_diffrn_ambient_temperature 396(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1007
_diffrn_reflns_av_sigmaI/netI 0.0679
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 16002
_diffrn_reflns_theta_full 30.73
_diffrn_reflns_theta_max 30.73
_diffrn_reflns_theta_min 2.69
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 15.411
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.474615
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.446
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 656
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.4
_refine_diff_density_max 3.124
_refine_diff_density_min -5.229
_refine_diff_density_rms 0.354
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.080
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 104
_refine_ls_number_reflns 2962
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.0698
_refine_ls_R_factor_gt 0.0477
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+14.7563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1035
_refine_ls_wR_factor_ref 0.1102
_reflns_number_gt 2282
_reflns_number_total 2962
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100863
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.07137(3) 0.22170(4) 0.11976(3) 0.01399(11) Uani 1 1 d . . .
N1 N -0.0002(7) 0.2250(9) -0.1416(6) 0.0137(13) Uani 1 1 d . . .
Cl1 Cl 0.0574(2) 0.2876(3) 0.3199(2) 0.0264(5) Uani 1 1 d . . .
C1 C 0.0809(8) 0.1717(11) -0.0554(7) 0.0141(16) Uani 1 1 d . . .
N2 N 0.1676(7) 0.0774(9) -0.1146(6) 0.0139(14) Uani 1 1 d . . .
C4 C -0.1086(9) 0.3309(13) -0.1199(9) 0.024(2) Uani 1 1 d . . .
H4A H -0.1144 0.3539 -0.0351 0.035 Uiso 1 1 calc R . .
H4B H -0.1864 0.2806 -0.1464 0.035 Uiso 1 1 calc R . .
H4C H -0.0962 0.4281 -0.1639 0.035 Uiso 1 1 calc R . .
C2 C 0.0356(9) 0.1657(12) -0.2553(8) 0.0163(17) Uani 1 1 d . . .
C5 C 0.2701(9) -0.0103(12) -0.0571(9) 0.022(2) Uani 1 1 d . . .
H5A H 0.3515 0.0282 -0.0858 0.033 Uiso 1 1 calc R . .
H5B H 0.2619 -0.1212 -0.0761 0.033 Uiso 1 1 calc R . .
H5C H 0.2652 0.0039 0.0288 0.033 Uiso 1 1 calc R . .
C3 C 0.1411(8) 0.0751(11) -0.2376(8) 0.0160(17) Uani 1 1 d . . .
C7 C 0.2197(10) -0.0178(14) -0.3238(10) 0.028(2) Uani 1 1 d . . .
H7A H 0.1802 -0.0152 -0.4021 0.042 Uiso 1 1 calc R . .
H7B H 0.2258 -0.1259 -0.2966 0.042 Uiso 1 1 calc R . .
H7C H 0.3043 0.0275 -0.3287 0.042 Uiso 1 1 calc R . .
C6 C -0.0416(12) 0.2022(14) -0.3650(9) 0.030(2) Uani 1 1 d . . .
H6A H -0.0599 0.3141 -0.3676 0.046 Uiso 1 1 calc R . .
H6B H -0.1208 0.1436 -0.3625 0.046 Uiso 1 1 calc R . .
H6C H 0.0060 0.1725 -0.4358 0.046 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01401(16) 0.01681(17) 0.01115(15) -0.00087(13) 0.00056(10) -0.00388(14)
N1 0.016(3) 0.015(3) 0.010(3) -0.002(3) -0.002(3) 0.001(3)
Cl1 0.0269(11) 0.0401(14) 0.0123(9) -0.0057(9) 0.0008(8) 0.0014(11)
C1 0.016(4) 0.014(4) 0.012(4) 0.001(3) -0.002(3) -0.006(3)
N2 0.010(3) 0.020(4) 0.011(3) 0.001(3) 0.001(3) -0.002(3)
C4 0.020(4) 0.017(4) 0.034(5) 0.002(4) -0.003(4) 0.004(4)
C2 0.021(4) 0.016(4) 0.011(4) 0.000(3) 0.002(3) -0.009(4)
C5 0.017(4) 0.025(5) 0.025(5) 0.003(4) -0.002(4) 0.003(4)
C3 0.015(4) 0.020(5) 0.014(4) 0.001(3) 0.002(3) -0.008(3)
C7 0.023(5) 0.037(6) 0.024(5) -0.005(4) 0.009(4) -0.003(4)
C6 0.041(6) 0.032(7) 0.018(5) 0.000(4) -0.010(4) -0.006(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Cl1 178.0(3) . . ?
C1 N1 C2 110.4(8) . . ?
C1 N1 C4 124.8(8) . . ?
C2 N1 C4 124.8(8) . . ?
N1 C1 N2 105.5(7) . . ?
N1 C1 Au1 126.0(7) . . ?
N2 C1 Au1 128.5(6) . . ?
C1 N2 C3 110.3(7) . . ?
C1 N2 C5 124.9(7) . . ?
C3 N2 C5 124.8(8) . . ?
C3 C2 N1 106.6(7) . . ?
C3 C2 C6 132.4(9) . . ?
N1 C2 C6 121.0(9) . . ?
C2 C3 N2 107.2(8) . . ?
C2 C3 C7 130.8(9) . . ?
N2 C3 C7 122.0(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 1.987(8) . ?
Au1 Cl1 2.288(2) . ?
N1 C1 1.350(11) . ?
N1 C2 1.404(11) . ?
N1 C4 1.456(12) . ?
C1 N2 1.368(11) . ?
N2 C3 1.389(11) . ?
N2 C5 1.444(12) . ?
C2 C3 1.351(13) . ?
C2 C6 1.488(13) . ?
C3 C7 1.480(13) . ?
|
1100864.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100864.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100864
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C30 H48 Au2 Cl2 N4'
_chemical_formula_weight 929.56
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.1440(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.5570(5)
_cell_length_b 19.4416(10)
_cell_length_c 17.6956(9)
_cell_measurement_reflns_used 32924
_cell_measurement_temperature 396(2)
_cell_measurement_theta_max 30.660
_cell_measurement_theta_min 2.189
_cell_volume 3201.8(3)
_diffrn_ambient_temperature 396(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0476
_diffrn_reflns_av_sigmaI/netI 0.0291
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 19002
_diffrn_reflns_theta_full 20.00
_diffrn_reflns_theta_max 20.00
_diffrn_reflns_theta_min 2.19
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 9.346
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.360949
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.928
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1792
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.5
_exptl_crystal_size_min 0.4
_refine_diff_density_max 3.072
_refine_diff_density_min -1.914
_refine_diff_density_rms 0.167
_refine_ls_extinction_coef 0.00210(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 154
_refine_ls_number_reflns 2987
_refine_ls_number_restraints 38
_refine_ls_restrained_S_all 1.073
_refine_ls_R_factor_all 0.0386
_refine_ls_R_factor_gt 0.0371
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+63.5851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0881
_refine_ls_wR_factor_ref 0.0888
_reflns_number_gt 2894
_reflns_number_total 2987
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100864
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.02105(5) 0.22950(2) 0.27731(2) 0.0136(2) Uiso 1 1 d U . .
Cl1 Cl 0.2468(3) 0.18267(15) 0.28974(16) 0.0179(7) Uiso 1 1 d U . .
N1 N -0.2916(10) 0.2336(5) 0.2829(5) 0.021(2) Uiso 1 1 d U . .
C1 C -0.1749(13) 0.2676(6) 0.2684(7) 0.021(3) Uiso 1 1 d U . .
Au2 Au 0.25424(5) 0.38135(2) 0.36014(2) 0.0133(2) Uiso 1 1 d U . .
Cl2 Cl 0.2697(3) 0.37187(15) 0.23383(16) 0.0182(7) Uiso 1 1 d U . .
N2 N -0.2235(9) 0.3311(5) 0.2469(5) 0.014(2) Uiso 1 1 d U . .
C2 C -0.4097(13) 0.2771(6) 0.2699(7) 0.021(3) Uiso 1 1 d U . .
H2 H -0.5017 0.2662 0.2752 0.025 Uiso 1 1 calc R . .
N3 N 0.2582(9) 0.4475(5) 0.5154(5) 0.014(2) Uiso 1 1 d U . .
C3 C -0.3654(13) 0.3379(7) 0.2483(7) 0.020(3) Uiso 1 1 d U . .
H3 H -0.4208 0.3775 0.2364 0.025 Uiso 1 1 calc R . .
N4 N 0.2441(10) 0.3371(5) 0.5210(5) 0.015(2) Uiso 1 1 d U . .
C4 C -0.2946(13) 0.1610(6) 0.3047(6) 0.018(3) Uiso 1 1 d U . .
H4 H -0.1988 0.1416 0.3079 0.021 Uiso 1 1 calc R . .
C5 C -0.4013(13) 0.1213(6) 0.2429(7) 0.023(3) Uiso 1 1 d U . .
H5A H -0.4965 0.1408 0.2373 0.027 Uiso 1 1 calc R . .
H5B H -0.3744 0.1254 0.1934 0.027 Uiso 1 1 calc R . .
C6 C -0.4039(14) 0.0459(7) 0.2649(7) 0.028(3) Uiso 1 1 d U . .
H6A H -0.4754 0.0221 0.2260 0.034 Uiso 1 1 calc R . .
H6B H -0.3110 0.0255 0.2654 0.034 Uiso 1 1 calc R . .
C7 C -0.4379(14) 0.0364(7) 0.3429(7) 0.031(3) Uiso 1 1 d U . .
H7A H -0.4323 -0.0120 0.3563 0.037 Uiso 1 1 calc R . .
H7B H -0.5353 0.0519 0.3407 0.037 Uiso 1 1 calc R . .
C8 C -0.3347(14) 0.0765(7) 0.4045(7) 0.028(3) Uiso 1 1 d U . .
H8A H -0.2390 0.0574 0.4107 0.034 Uiso 1 1 calc R . .
H8B H -0.3627 0.0716 0.4536 0.034 Uiso 1 1 calc R . .
C9 C -0.3314(14) 0.1525(7) 0.3844(7) 0.025(3) Uiso 1 1 d U . .
H9A H -0.2599 0.1760 0.4237 0.030 Uiso 1 1 calc R . .
H9B H -0.4243 0.1731 0.3833 0.030 Uiso 1 1 calc R . .
C10 C -0.1329(13) 0.3866(6) 0.2239(6) 0.015(3) Uiso 1 1 d U . .
H10 H -0.0331 0.3705 0.2367 0.018 Uiso 1 1 calc R . .
C11 C -0.1744(13) 0.3992(6) 0.1366(7) 0.020(3) Uiso 1 1 d U . .
H11A H -0.1641 0.3570 0.1091 0.024 Uiso 1 1 calc R . .
H11B H -0.2740 0.4137 0.1215 0.024 Uiso 1 1 calc R . .
C12 C -0.0769(13) 0.4552(6) 0.1150(7) 0.020(3) Uiso 1 1 d U . .
H12A H -0.1074 0.4651 0.0600 0.024 Uiso 1 1 calc R . .
H12B H 0.0211 0.4383 0.1250 0.024 Uiso 1 1 calc R . .
C13 C -0.0809(12) 0.5215(6) 0.1609(6) 0.015(3) Uiso 1 1 d U . .
H13A H -0.1759 0.5418 0.1457 0.018 Uiso 1 1 calc R . .
H13B H -0.0126 0.5541 0.1485 0.018 Uiso 1 1 calc R . .
C14 C -0.0444(12) 0.5079(6) 0.2492(6) 0.019(3) Uiso 1 1 d U . .
H14A H 0.0555 0.4942 0.2657 0.023 Uiso 1 1 calc R . .
H14B H -0.0575 0.5499 0.2763 0.023 Uiso 1 1 calc R . .
C15 C -0.1396(12) 0.4518(6) 0.2699(6) 0.015(3) Uiso 1 1 d U . .
H15A H -0.2381 0.4680 0.2596 0.018 Uiso 1 1 calc R . .
H15B H -0.1095 0.4417 0.3249 0.018 Uiso 1 1 calc R . .
C16 C 0.2509(11) 0.3894(6) 0.4725(6) 0.011(3) Uiso 1 1 d U . .
C17 C 0.2597(12) 0.4304(6) 0.5911(7) 0.018(3) Uiso 1 1 d U . .
H17 H 0.2672 0.4609 0.6323 0.022 Uiso 1 1 calc R . .
C18 C 0.2484(12) 0.3612(6) 0.5947(7) 0.020(3) Uiso 1 1 d U . .
H18 H 0.2443 0.3351 0.6382 0.024 Uiso 1 1 calc R . .
C19 C 0.2688(12) 0.5179(6) 0.4847(6) 0.017(3) Uiso 1 1 d U . .
H19 H 0.3113 0.5137 0.4394 0.020 Uiso 1 1 calc R . .
C20 C 0.1225(12) 0.5519(6) 0.4573(7) 0.020(3) Uiso 1 1 d U . .
H20A H 0.0774 0.5575 0.5008 0.024 Uiso 1 1 calc R . .
H20B H 0.0609 0.5229 0.4190 0.024 Uiso 1 1 calc R . .
C21 C 0.1403(14) 0.6219(6) 0.4218(7) 0.027(3) Uiso 1 1 d U . .
H21A H 0.1778 0.6156 0.3757 0.032 Uiso 1 1 calc R . .
H21B H 0.0472 0.6440 0.4063 0.032 Uiso 1 1 calc R . .
C22 C 0.2418(14) 0.6681(7) 0.4788(8) 0.036(3) Uiso 1 1 d U . .
H22A H 0.2555 0.7109 0.4533 0.043 Uiso 1 1 calc R . .
H22B H 0.1987 0.6789 0.5220 0.043 Uiso 1 1 calc R . .
C23 C 0.3862(13) 0.6342(6) 0.5092(7) 0.025(3) Uiso 1 1 d U . .
H23A H 0.4448 0.6630 0.5489 0.030 Uiso 1 1 calc R . .
H23B H 0.4355 0.6292 0.4673 0.030 Uiso 1 1 calc R . .
C24 C 0.3672(13) 0.5639(6) 0.5431(7) 0.020(3) Uiso 1 1 d U . .
H24A H 0.4604 0.5420 0.5596 0.023 Uiso 1 1 calc R . .
H24B H 0.3273 0.5696 0.5884 0.023 Uiso 1 1 calc R . .
C25 C 0.2409(12) 0.2627(6) 0.5003(7) 0.015(3) Uiso 1 1 d U . .
H25 H 0.2417 0.2596 0.4451 0.018 Uiso 1 1 calc R . .
C26 C 0.1023(13) 0.2290(6) 0.5107(7) 0.019(3) Uiso 1 1 d U . .
H26A H 0.0200 0.2536 0.4806 0.023 Uiso 1 1 calc R . .
H26B H 0.0978 0.2308 0.5649 0.023 Uiso 1 1 calc R . .
C27 C 0.0989(13) 0.1537(6) 0.4835(7) 0.021(3) Uiso 1 1 d U . .
H27A H 0.0143 0.1313 0.4936 0.025 Uiso 1 1 calc R . .
H27B H 0.0917 0.1527 0.4280 0.025 Uiso 1 1 calc R . .
C28 C 0.2324(12) 0.1142(6) 0.5244(7) 0.022(3) Uiso 1 1 d U . .
H28A H 0.2307 0.0687 0.5018 0.026 Uiso 1 1 calc R . .
H28B H 0.2315 0.1088 0.5788 0.026 Uiso 1 1 calc R . .
C29 C 0.3694(13) 0.1509(6) 0.5177(7) 0.025(3) Uiso 1 1 d U . .
H29A H 0.3776 0.1498 0.4641 0.030 Uiso 1 1 calc R . .
H29B H 0.4515 0.1267 0.5487 0.030 Uiso 1 1 calc R . .
C30 C 0.3723(13) 0.2256(6) 0.5449(7) 0.019(3) Uiso 1 1 d U . .
H30A H 0.3744 0.2269 0.5999 0.023 Uiso 1 1 calc R . .
H30B H 0.4581 0.2481 0.5367 0.023 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Cl1 178.3(4) . . ?
C1 N1 C2 110.0(10) . . ?
C1 N1 C4 125.4(10) . . ?
C2 N1 C4 124.5(10) . . ?
N2 C1 N1 104.6(10) . . ?
N2 C1 Au1 128.6(9) . . ?
N1 C1 Au1 126.8(9) . . ?
C16 Au2 Cl2 177.3(3) . . ?
C1 N2 C3 111.4(10) . . ?
C1 N2 C10 123.8(9) . . ?
C3 N2 C10 124.8(10) . . ?
C3 C2 N1 106.7(11) . . ?
C16 N3 C17 109.3(9) . . ?
C16 N3 C19 124.3(9) . . ?
C17 N3 C19 126.3(9) . . ?
C2 C3 N2 107.3(11) . . ?
C16 N4 C18 110.5(9) . . ?
C16 N4 C25 125.5(9) . . ?
C18 N4 C25 123.9(9) . . ?
N1 C4 C5 110.4(9) . . ?
N1 C4 C9 111.4(9) . . ?
C5 C4 C9 110.5(10) . . ?
C6 C5 C4 110.6(10) . . ?
C7 C6 C5 112.0(11) . . ?
C6 C7 C8 111.0(11) . . ?
C7 C8 C9 112.1(11) . . ?
C8 C9 C4 109.8(10) . . ?
C15 C10 N2 111.1(9) . . ?
C15 C10 C11 112.1(10) . . ?
N2 C10 C11 111.0(9) . . ?
C12 C11 C10 109.5(9) . . ?
C11 C12 C13 112.1(9) . . ?
C12 C13 C14 111.5(10) . . ?
C15 C14 C13 110.9(9) . . ?
C14 C15 C10 111.8(9) . . ?
N4 C16 N3 106.2(9) . . ?
N4 C16 Au2 126.1(8) . . ?
N3 C16 Au2 127.6(8) . . ?
C18 C17 N3 107.6(10) . . ?
C17 C18 N4 106.3(10) . . ?
N3 C19 C24 112.1(9) . . ?
N3 C19 C20 112.5(9) . . ?
C24 C19 C20 110.0(10) . . ?
C19 C20 C21 109.7(10) . . ?
C22 C21 C20 111.5(11) . . ?
C23 C22 C21 111.7(11) . . ?
C22 C23 C24 110.5(10) . . ?
C19 C24 C23 111.8(10) . . ?
N4 C25 C30 111.6(9) . . ?
N4 C25 C26 110.9(9) . . ?
C30 C25 C26 112.0(10) . . ?
C25 C26 C27 109.1(9) . . ?
C28 C27 C26 112.0(10) . . ?
C27 C28 C29 111.7(10) . . ?
C28 C29 C30 112.1(10) . . ?
C25 C30 C29 109.7(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 1.987(12) . ?
Au1 Cl1 2.306(3) . ?
N1 C1 1.370(15) . ?
N1 C2 1.386(16) . ?
N1 C4 1.467(15) . ?
C1 N2 1.343(15) . ?
Au2 C16 2.003(11) . ?
Au2 Cl2 2.281(3) . ?
N2 C3 1.368(15) . ?
N2 C10 1.496(15) . ?
C2 C3 1.341(17) . ?
N3 C16 1.354(14) . ?
N3 C17 1.378(14) . ?
N3 C19 1.483(15) . ?
N4 C16 1.341(14) . ?
N4 C18 1.378(15) . ?
N4 C25 1.490(15) . ?
C4 C5 1.524(17) . ?
C4 C9 1.538(17) . ?
C5 C6 1.517(17) . ?
C6 C7 1.500(18) . ?
C7 C8 1.510(18) . ?
C8 C9 1.524(18) . ?
C10 C15 1.515(16) . ?
C10 C11 1.526(16) . ?
C11 C12 1.537(17) . ?
C12 C13 1.527(16) . ?
C13 C14 1.544(16) . ?
C14 C15 1.519(16) . ?
C17 C18 1.352(17) . ?
C19 C24 1.521(16) . ?
C19 C20 1.523(16) . ?
C20 C21 1.525(17) . ?
C21 C22 1.523(18) . ?
C22 C23 1.514(18) . ?
C23 C24 1.519(17) . ?
C25 C30 1.506(16) . ?
C25 C26 1.526(16) . ?
C26 C27 1.540(17) . ?
C27 C28 1.524(17) . ?
C28 C29 1.519(17) . ?
C29 C30 1.527(17) . ?
|
1100865.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100865.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100865
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C23 H32 Au Cl N2'
_chemical_formula_weight 568.92
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 111.4490(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.5735(7)
_cell_length_b 11.7626(6)
_cell_length_c 12.9098(6)
_cell_measurement_reflns_used 28583
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 30.466
_cell_measurement_theta_min 2.292
_cell_volume 2059.76(17)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0364
_diffrn_reflns_av_sigmaI/netI 0.0230
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 32039
_diffrn_reflns_theta_full 30.47
_diffrn_reflns_theta_max 30.47
_diffrn_reflns_theta_min 2.29
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 7.283
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.287418
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.835
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1120
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_refine_diff_density_max 2.094
_refine_diff_density_min -1.338
_refine_diff_density_rms 0.115
_refine_ls_extinction_coef 0.00428(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 245
_refine_ls_number_reflns 6242
_refine_ls_number_restraints 273
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0225
_refine_ls_R_factor_gt 0.0207
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+3.4771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0524
_refine_ls_wR_factor_ref 0.0535
_reflns_number_gt 5883
_reflns_number_total 6242
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.195987(6) 0.052787(7) 0.361363(6) 0.01650(4) Uani 1 1 d U . .
Cl1 Cl 0.23231(5) -0.04848(5) 0.52166(5) 0.02295(11) Uani 1 1 d U . .
C4 C -0.02174(16) 0.1305(2) 0.14926(19) 0.0175(4) Uani 1 1 d U . .
N1 N 0.07522(14) 0.16829(17) 0.14611(16) 0.0172(3) Uani 1 1 d U . .
N2 N 0.23134(14) 0.20234(17) 0.19072(16) 0.0170(3) Uani 1 1 d U . .
C12 C -0.02789(17) 0.0004(2) 0.14720(19) 0.0191(4) Uani 1 1 d U . .
H12A H 0.0259 -0.0313 0.2124 0.023 Uiso 1 1 calc R . .
H12B H -0.0202 -0.0289 0.0789 0.023 Uiso 1 1 calc R . .
C13 C -0.12866(19) -0.0366(2) 0.1498(2) 0.0216(4) Uani 1 1 d U . .
H13 H -0.1326 -0.1215 0.1490 0.026 Uiso 1 1 calc R . .
C7 C -0.21069(19) 0.0109(2) 0.0474(2) 0.0262(5) Uani 1 1 d U . .
H7A H -0.2757 -0.0141 0.0469 0.031 Uiso 1 1 calc R . .
H7B H -0.2030 -0.0177 -0.0211 0.031 Uiso 1 1 calc R . .
C6 C -0.20481(18) 0.1412(2) 0.0507(2) 0.0255(5) Uani 1 1 d U . .
H6 H -0.2587 0.1726 -0.0161 0.031 Uiso 1 1 calc R . .
C8 C -0.2172(2) 0.1861(2) 0.1554(3) 0.0295(5) Uani 1 1 d U . .
H8A H -0.2818 0.1621 0.1568 0.035 Uiso 1 1 calc R . .
H8B H -0.2148 0.2702 0.1562 0.035 Uiso 1 1 calc R . .
C9 C -0.13364(19) 0.1387(2) 0.2578(2) 0.0254(5) Uani 1 1 d U . .
H9 H -0.1411 0.1679 0.3271 0.030 Uiso 1 1 calc R . .
C10 C -0.13785(19) 0.0085(2) 0.2569(2) 0.0250(5) Uani 1 1 d U . .
H10A H -0.0835 -0.0219 0.3224 0.030 Uiso 1 1 calc R . .
H10B H -0.2010 -0.0170 0.2614 0.030 Uiso 1 1 calc R . .
C11 C -0.03412(18) 0.1771(2) 0.2549(2) 0.0214(4) Uani 1 1 d U . .
H11A H 0.0200 0.1486 0.3218 0.026 Uiso 1 1 calc R . .
H11B H -0.0309 0.2611 0.2552 0.026 Uiso 1 1 calc R . .
C5 C -0.10501(17) 0.1784(2) 0.0477(2) 0.0219(4) Uani 1 1 d U . .
H5A H -0.0980 0.1503 -0.0214 0.026 Uiso 1 1 calc R . .
H5B H -0.1012 0.2624 0.0480 0.026 Uiso 1 1 calc R . .
C1 C 0.16563(16) 0.14601(19) 0.22436(18) 0.0175(4) Uani 1 1 d U . .
C2 C 0.08535(17) 0.2382(2) 0.06427(19) 0.0208(4) Uani 1 1 d U . .
H2 H 0.0334 0.2660 0.0005 0.025 Uiso 1 1 calc R . .
C3 C 0.18193(17) 0.2592(2) 0.09174(19) 0.0205(4) Uani 1 1 d U . .
H3 H 0.2110 0.3045 0.0510 0.025 Uiso 1 1 calc R . .
C15 C 0.33924(16) 0.21345(19) 0.25489(18) 0.0166(4) Uani 1 1 d U . .
C23 C 0.39011(17) 0.0967(2) 0.2761(2) 0.0195(4) Uani 1 1 d U . .
H23A H 0.3600 0.0475 0.3173 0.023 Uiso 1 1 calc R . .
H23B H 0.3811 0.0595 0.2043 0.023 Uiso 1 1 calc R . .
C20 C 0.50048(17) 0.1113(2) 0.3440(2) 0.0215(4) Uani 1 1 d U . .
H20 H 0.5331 0.0351 0.3587 0.026 Uiso 1 1 calc R . .
C21 C 0.51430(18) 0.1699(2) 0.4553(2) 0.0240(5) Uani 1 1 d U . .
H21A H 0.4843 0.1229 0.4982 0.029 Uiso 1 1 calc R . .
H21B H 0.5855 0.1782 0.4999 0.029 Uiso 1 1 calc R . .
C22 C 0.46526(18) 0.2874(2) 0.4330(2) 0.0234(4) Uani 1 1 d U . .
H22 H 0.4747 0.3255 0.5054 0.028 Uiso 1 1 calc R . .
C18 C 0.51118(19) 0.3607(2) 0.3664(2) 0.0262(5) Uani 1 1 d U . .
H18A H 0.4791 0.4362 0.3517 0.031 Uiso 1 1 calc R . .
H18B H 0.5823 0.3718 0.4096 0.031 Uiso 1 1 calc R . .
C17 C 0.49721(17) 0.3012(2) 0.2564(2) 0.0231(5) Uani 1 1 d U . .
H17 H 0.5274 0.3486 0.2129 0.028 Uiso 1 1 calc R . .
C19 C 0.54744(18) 0.1849(2) 0.2792(2) 0.0240(5) Uani 1 1 d U . .
H19A H 0.5401 0.1474 0.2079 0.029 Uiso 1 1 calc R . .
H19B H 0.6187 0.1943 0.3228 0.029 Uiso 1 1 calc R . .
C16 C 0.38644(17) 0.2866(2) 0.1888(2) 0.0214(4) Uani 1 1 d U . .
H16A H 0.3771 0.2494 0.1169 0.026 Uiso 1 1 calc R . .
H16B H 0.3541 0.3620 0.1733 0.026 Uiso 1 1 calc R . .
C24 C 0.35473(17) 0.2732(2) 0.36595(19) 0.0203(4) Uani 1 1 d U . .
H24A H 0.3225 0.3487 0.3515 0.024 Uiso 1 1 calc R . .
H24B H 0.3242 0.2276 0.4093 0.024 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01526(5) 0.01949(5) 0.01472(5) 0.00229(3) 0.00545(3) -0.00028(3)
Cl1 0.0275(3) 0.0235(3) 0.0171(2) 0.00447(18) 0.0074(2) 0.0004(2)
C4 0.0142(9) 0.0205(10) 0.0186(9) 0.0009(7) 0.0068(7) -0.0011(7)
N1 0.0144(8) 0.0210(9) 0.0160(8) 0.0024(7) 0.0052(6) -0.0001(7)
N2 0.0148(8) 0.0211(9) 0.0156(8) 0.0017(7) 0.0060(6) 0.0000(7)
C12 0.0186(10) 0.0193(10) 0.0196(10) -0.0004(8) 0.0070(8) -0.0024(8)
C13 0.0203(10) 0.0209(10) 0.0238(11) 0.0008(8) 0.0083(9) -0.0050(8)
C7 0.0190(10) 0.0318(13) 0.0252(11) 0.0028(10) 0.0050(9) -0.0062(9)
C6 0.0143(9) 0.0318(13) 0.0289(12) 0.0083(10) 0.0060(9) 0.0001(9)
C8 0.0209(11) 0.0271(12) 0.0451(15) 0.0031(11) 0.0175(11) 0.0027(9)
C9 0.0222(11) 0.0301(12) 0.0291(12) -0.0027(9) 0.0156(9) -0.0027(9)
C10 0.0231(11) 0.0306(12) 0.0239(11) 0.0024(9) 0.0115(9) -0.0042(9)
C11 0.0196(10) 0.0236(11) 0.0237(10) -0.0028(8) 0.0111(9) -0.0023(8)
C5 0.0157(9) 0.0253(11) 0.0235(11) 0.0073(8) 0.0056(8) 0.0004(8)
C1 0.0155(9) 0.0190(10) 0.0179(9) 0.0005(7) 0.0061(8) -0.0007(7)
C2 0.0179(10) 0.0255(11) 0.0181(10) 0.0046(8) 0.0055(8) -0.0003(8)
C3 0.0177(9) 0.0247(11) 0.0183(10) 0.0046(8) 0.0055(8) 0.0005(8)
C15 0.0138(9) 0.0196(10) 0.0162(9) 0.0007(7) 0.0053(7) 0.0004(7)
C23 0.0178(9) 0.0195(10) 0.0212(10) 0.0011(8) 0.0071(8) 0.0016(8)
C20 0.0170(10) 0.0233(11) 0.0239(11) 0.0023(8) 0.0070(8) 0.0018(8)
C21 0.0192(10) 0.0318(12) 0.0185(10) 0.0041(9) 0.0041(8) 0.0003(9)
C22 0.0183(10) 0.0294(12) 0.0204(10) -0.0038(9) 0.0045(8) -0.0032(9)
C18 0.0182(10) 0.0245(12) 0.0334(13) -0.0002(9) 0.0065(9) -0.0039(9)
C17 0.0156(10) 0.0281(12) 0.0256(11) 0.0064(9) 0.0074(9) -0.0007(9)
C19 0.0169(10) 0.0311(12) 0.0256(11) 0.0030(9) 0.0095(9) 0.0032(9)
C16 0.0160(9) 0.0273(11) 0.0210(10) 0.0063(8) 0.0069(8) 0.0003(8)
C24 0.0166(9) 0.0238(11) 0.0201(10) -0.0038(8) 0.0063(8) -0.0006(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Cl1 178.07(7) . . ?
N1 C4 C12 110.27(18) . . ?
N1 C4 C5 109.13(18) . . ?
C12 C4 C5 109.24(19) . . ?
N1 C4 C11 109.62(18) . . ?
C12 C4 C11 110.22(18) . . ?
C5 C4 C11 108.33(19) . . ?
C1 N1 C2 109.59(19) . . ?
C1 N1 C4 126.18(19) . . ?
C2 N1 C4 124.13(19) . . ?
C1 N2 C3 109.88(19) . . ?
C1 N2 C15 126.02(18) . . ?
C3 N2 C15 123.79(19) . . ?
C4 C12 C13 109.36(19) . . ?
C7 C13 C10 110.8(2) . . ?
C7 C13 C12 109.1(2) . . ?
C10 C13 C12 108.7(2) . . ?
C13 C7 C6 108.9(2) . . ?
C8 C6 C5 110.2(2) . . ?
C8 C6 C7 110.3(2) . . ?
C5 C6 C7 109.2(2) . . ?
C6 C8 C9 108.9(2) . . ?
C10 C9 C11 109.3(2) . . ?
C10 C9 C8 109.8(2) . . ?
C11 C9 C8 109.3(2) . . ?
C13 C10 C9 109.7(2) . . ?
C9 C11 C4 109.6(2) . . ?
C4 C5 C6 109.60(19) . . ?
N2 C1 N1 105.84(19) . . ?
N2 C1 Au1 126.81(16) . . ?
N1 C1 Au1 127.34(16) . . ?
C3 C2 N1 107.5(2) . . ?
C2 C3 N2 107.2(2) . . ?
N2 C15 C24 108.88(17) . . ?
N2 C15 C23 111.26(18) . . ?
C24 C15 C23 110.18(18) . . ?
N2 C15 C16 109.59(18) . . ?
C24 C15 C16 108.57(19) . . ?
C23 C15 C16 108.30(18) . . ?
C20 C23 C15 109.75(19) . . ?
C19 C20 C23 109.7(2) . . ?
C19 C20 C21 109.0(2) . . ?
C23 C20 C21 109.61(19) . . ?
C22 C21 C20 109.56(19) . . ?
C24 C22 C18 109.2(2) . . ?
C24 C22 C21 109.2(2) . . ?
C18 C22 C21 110.1(2) . . ?
C17 C18 C22 109.0(2) . . ?
C18 C17 C19 109.8(2) . . ?
C18 C17 C16 109.5(2) . . ?
C19 C17 C16 109.8(2) . . ?
C20 C19 C17 109.5(2) . . ?
C17 C16 C15 109.71(19) . . ?
C22 C24 C15 109.99(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 1.989(2) . ?
Au1 Cl1 2.2761(6) . ?
C4 N1 1.496(3) . ?
C4 C12 1.532(3) . ?
C4 C5 1.532(3) . ?
C4 C11 1.541(3) . ?
N1 C1 1.361(3) . ?
N1 C2 1.388(3) . ?
N2 C1 1.360(3) . ?
N2 C3 1.388(3) . ?
N2 C15 1.491(3) . ?
C12 C13 1.544(3) . ?
C13 C7 1.528(4) . ?
C13 C10 1.532(4) . ?
C7 C6 1.534(4) . ?
C6 C8 1.522(4) . ?
C6 C5 1.533(3) . ?
C8 C9 1.537(4) . ?
C9 C10 1.532(4) . ?
C9 C11 1.533(3) . ?
C2 C3 1.343(3) . ?
C15 C24 1.537(3) . ?
C15 C23 1.537(3) . ?
C15 C16 1.539(3) . ?
C23 C20 1.534(3) . ?
C20 C19 1.529(3) . ?
C20 C21 1.539(4) . ?
C21 C22 1.533(4) . ?
C22 C24 1.534(3) . ?
C22 C18 1.533(4) . ?
C18 C17 1.529(4) . ?
C17 C19 1.528(4) . ?
C17 C16 1.538(3) . ?
|
1100866.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100866.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100866
loop_
_publ_author_name
'de Fr\'emont, Pierre'
'Scott, Natalie M.'
'Stevens, Edwin D.'
'Nolan, Steven P.'
_publ_section_title
;
Synthesis and Structural Characterization of <i>N</i> -Heterocyclic
Carbene Gold(I) Complexes
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2411
_journal_page_last 2418
_journal_paper_doi 10.1021/om050111c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C11 H11 Au Cl N3'
_chemical_formula_weight 417.64
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 91.9290(10)
_cell_angle_beta 91.3230(10)
_cell_angle_gamma 101.5470(10)
_cell_formula_units_Z 4
_cell_length_a 7.3539(4)
_cell_length_b 10.8603(5)
_cell_length_c 14.5517(7)
_cell_measurement_reflns_used 17736
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 30.728
_cell_measurement_theta_min 2.329
_cell_volume 1137.48(10)
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0420
_diffrn_reflns_av_sigmaI/netI 0.0368
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 10117
_diffrn_reflns_theta_full 22.50
_diffrn_reflns_theta_max 22.50
_diffrn_reflns_theta_min 2.33
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 13.141
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.384732
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.439
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 776
_exptl_crystal_size_max 0.8
_exptl_crystal_size_mid 0.5
_exptl_crystal_size_min 0.4
_refine_diff_density_max 1.036
_refine_diff_density_min -1.294
_refine_diff_density_rms 0.147
_refine_ls_extinction_coef 0.0040(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 290
_refine_ls_number_reflns 2972
_refine_ls_number_restraints 278
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0218
_refine_ls_R_factor_gt 0.0214
_refine_ls_shift/su_max 0.186
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+3.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0634
_refine_ls_wR_factor_ref 0.0637
_reflns_number_gt 2924
_reflns_number_total 2972
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100866
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.20267(3) 0.036777(17) 0.074184(13) 0.01374(12) Uani 1 1 d U . .
Cl1 Cl 0.16155(19) 0.22419(12) 0.13824(9) 0.0202(3) Uani 1 1 d U . .
N1 N 0.2896(6) -0.1246(4) -0.0782(3) 0.0139(9) Uani 1 1 d U . .
C1 C 0.2484(7) -0.1179(5) 0.0111(4) 0.0137(10) Uani 1 1 d U . .
Au2 Au 0.26622(3) 0.521694(18) 0.548074(13) 0.01682(12) Uani 1 1 d U . .
Cl2 Cl 0.2656(2) 0.73160(12) 0.54384(9) 0.0253(3) Uani 1 1 d U . .
N2 N 0.2476(6) -0.2371(4) 0.0375(3) 0.0155(9) Uani 1 1 d U . .
C2 C 0.3043(7) -0.2426(5) -0.1039(4) 0.0160(11) Uani 1 1 d U . .
N3 N 0.2804(6) -0.3165(4) -0.0349(3) 0.0179(10) Uani 1 1 d U . .
C3 C 0.3406(8) -0.2527(5) -0.2043(4) 0.0213(12) Uani 1 1 d U . .
H3A H 0.2312 -0.3021 -0.2390 0.026 Uiso 1 1 calc R . .
H3B H 0.4495 -0.2914 -0.2153 0.026 Uiso 1 1 calc R . .
N4 N 0.2453(6) 0.2526(4) 0.4843(3) 0.0172(9) Uani 1 1 d U . .
C4 C 0.3792(9) -0.1125(5) -0.2307(4) 0.0246(13) Uani 1 1 d U . .
H4A H 0.5143 -0.0800 -0.2350 0.030 Uiso 1 1 calc R . .
H4B H 0.3184 -0.1034 -0.2908 0.030 Uiso 1 1 calc R . .
N5 N 0.2915(6) 0.2725(4) 0.6280(3) 0.0168(9) Uani 1 1 d U . .
C5 C 0.2997(8) -0.0403(5) -0.1547(4) 0.0182(12) Uani 1 1 d U . .
H5A H 0.3828 0.0417 -0.1391 0.022 Uiso 1 1 calc R . .
H5B H 0.1752 -0.0260 -0.1729 0.022 Uiso 1 1 calc R . .
N6 N 0.2848(7) 0.1454(4) 0.6068(3) 0.0202(10) Uani 1 1 d U . .
C6 C 0.2128(7) -0.2877(5) 0.1261(4) 0.0143(10) Uani 1 1 d U . .
C7 C 0.2692(7) -0.2136(5) 0.2051(4) 0.0170(11) Uani 1 1 d U . .
H7 H 0.3339 -0.1292 0.2006 0.020 Uiso 1 1 calc R . .
C8 C 0.2303(8) -0.2636(5) 0.2909(4) 0.0201(12) Uani 1 1 d U . .
H8 H 0.2670 -0.2131 0.3453 0.024 Uiso 1 1 calc R . .
C9 C 0.1376(8) -0.3878(5) 0.2968(4) 0.0216(12) Uani 1 1 d U . .
H9 H 0.1105 -0.4223 0.3552 0.026 Uiso 1 1 calc R . .
C10 C 0.0849(7) -0.4611(5) 0.2170(4) 0.0204(12) Uani 1 1 d U . .
H10 H 0.0223 -0.5461 0.2211 0.024 Uiso 1 1 calc R . .
C11 C 0.1227(7) -0.4118(5) 0.1316(4) 0.0168(11) Uani 1 1 d U . .
H11 H 0.0872 -0.4626 0.0772 0.020 Uiso 1 1 calc R . .
C12 C 0.2685(7) 0.3409(5) 0.5546(4) 0.0160(11) Uani 1 1 d U . .
C13 C 0.2589(8) 0.1389(5) 0.5181(4) 0.0200(11) Uani 1 1 d U . .
C14 C 0.2404(9) 0.0412(6) 0.4425(4) 0.0278(13) Uani 1 1 d U . .
H14A H 0.1595 -0.0386 0.4594 0.033 Uiso 1 1 calc R . .
H14B H 0.3628 0.0249 0.4247 0.033 Uiso 1 1 calc R . .
C15 C 0.1482(9) 0.1062(6) 0.3643(4) 0.0292(13) Uani 1 1 d U . .
H15A H 0.1885 0.0815 0.3032 0.035 Uiso 1 1 calc R . .
H15B H 0.0111 0.0825 0.3658 0.035 Uiso 1 1 calc R . .
C16 C 0.2141(9) 0.2477(6) 0.3842(4) 0.0247(13) Uani 1 1 d U . .
H16A H 0.3300 0.2809 0.3522 0.030 Uiso 1 1 calc R . .
H16B H 0.1178 0.2950 0.3663 0.030 Uiso 1 1 calc R . .
C17 C 0.3100(8) 0.3133(5) 0.7227(4) 0.0154(11) Uani 1 1 d U . .
C18 C 0.2116(8) 0.2357(5) 0.7862(4) 0.0179(12) Uani 1 1 d U . .
H18 H 0.1312 0.1593 0.7663 0.021 Uiso 1 1 calc R . .
C19 C 0.2314(8) 0.2704(5) 0.8789(4) 0.0201(12) Uani 1 1 d U . .
H19 H 0.1660 0.2174 0.9230 0.024 Uiso 1 1 calc R . .
C20 C 0.3476(8) 0.3835(5) 0.9073(4) 0.0217(12) Uani 1 1 d U . .
H20 H 0.3603 0.4081 0.9707 0.026 Uiso 1 1 calc R . .
C21 C 0.4446(8) 0.4601(5) 0.8433(4) 0.0218(12) Uani 1 1 d U . .
H21 H 0.5237 0.5371 0.8631 0.026 Uiso 1 1 calc R . .
C22 C 0.4274(7) 0.4257(5) 0.7512(4) 0.0161(11) Uani 1 1 d U . .
H22 H 0.4951 0.4781 0.7075 0.019 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.02066(17) 0.01180(16) 0.00957(16) 0.00014(10) 0.00355(10) 0.00490(10)
Cl1 0.0307(8) 0.0154(7) 0.0155(7) -0.0040(5) 0.0040(5) 0.0073(6)
N1 0.021(2) 0.014(2) 0.009(2) -0.0015(16) 0.0021(17) 0.0078(18)
C1 0.013(2) 0.014(2) 0.013(2) 0.002(2) 0.002(2) 0.002(2)
Au2 0.02904(17) 0.01346(16) 0.00879(16) 0.00327(10) 0.00351(10) 0.00545(11)
Cl2 0.0473(9) 0.0150(7) 0.0151(7) 0.0015(6) 0.0012(6) 0.0093(6)
N2 0.023(2) 0.015(2) 0.009(2) 0.0006(17) 0.0034(18) 0.0059(19)
C2 0.021(3) 0.016(3) 0.012(2) 0.000(2) 0.001(2) 0.006(2)
N3 0.030(3) 0.015(2) 0.011(2) -0.0003(18) 0.0038(19) 0.0079(19)
C3 0.034(3) 0.021(3) 0.010(3) 0.002(2) 0.006(2) 0.008(2)
N4 0.025(2) 0.018(2) 0.010(2) 0.0022(18) 0.0046(18) 0.0060(19)
C4 0.038(3) 0.019(3) 0.017(3) 0.000(2) 0.002(2) 0.007(3)
N5 0.027(2) 0.014(2) 0.011(2) 0.0010(17) 0.0051(18) 0.0073(19)
C5 0.026(3) 0.014(3) 0.015(3) 0.004(2) 0.002(2) 0.006(2)
N6 0.031(3) 0.014(2) 0.017(2) 0.0001(19) 0.003(2) 0.005(2)
C6 0.016(3) 0.016(2) 0.013(2) 0.002(2) 0.005(2) 0.007(2)
C7 0.020(3) 0.016(3) 0.014(3) 0.002(2) 0.000(2) 0.005(2)
C8 0.024(3) 0.020(3) 0.016(3) -0.003(2) 0.003(2) 0.006(2)
C9 0.024(3) 0.024(3) 0.018(3) 0.006(2) 0.007(2) 0.008(2)
C10 0.020(3) 0.018(3) 0.022(3) 0.005(2) 0.002(2) 0.001(2)
C11 0.024(3) 0.014(3) 0.012(3) -0.003(2) -0.003(2) 0.006(2)
C12 0.019(3) 0.020(2) 0.010(2) 0.002(2) 0.006(2) 0.006(2)
C13 0.027(3) 0.017(3) 0.016(3) 0.003(2) 0.004(2) 0.005(2)
C14 0.043(4) 0.022(3) 0.019(3) -0.002(2) 0.004(3) 0.009(3)
C15 0.042(3) 0.028(3) 0.017(3) -0.001(2) 0.005(2) 0.004(3)
C16 0.035(3) 0.028(3) 0.011(3) 0.001(2) 0.007(2) 0.005(3)
C17 0.024(3) 0.015(3) 0.010(2) 0.004(2) 0.003(2) 0.010(2)
C18 0.022(3) 0.016(3) 0.017(3) 0.002(2) 0.003(2) 0.008(2)
C19 0.023(3) 0.025(3) 0.016(3) 0.008(2) 0.004(2) 0.010(2)
C20 0.032(3) 0.028(3) 0.008(3) -0.004(2) -0.001(2) 0.015(2)
C21 0.032(3) 0.016(3) 0.019(3) -0.002(2) -0.006(2) 0.009(2)
C22 0.021(3) 0.015(3) 0.014(2) 0.004(2) 0.002(2) 0.007(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 Cl1 175.59(15) . . ?
C1 N1 C2 110.6(4) . . ?
C1 N1 C5 135.4(4) . . ?
C2 N1 C5 113.4(4) . . ?
N1 C1 N2 102.3(4) . . ?
N1 C1 Au1 123.4(4) . . ?
N2 C1 Au1 134.3(4) . . ?
C12 Au2 Cl2 178.74(16) . . ?
C1 N2 N3 112.7(4) . . ?
C1 N2 C6 128.4(4) . . ?
N3 N2 C6 118.8(4) . . ?
N3 C2 N1 111.3(5) . . ?
N3 C2 C3 137.6(5) . . ?
N1 C2 C3 111.2(4) . . ?
C2 N3 N2 103.0(4) . . ?
C2 C3 C4 101.9(4) . . ?
C13 N4 C12 109.5(5) . . ?
C13 N4 C16 113.0(5) . . ?
C12 N4 C16 137.5(5) . . ?
C5 C4 C3 106.6(5) . . ?
C12 N5 N6 114.3(4) . . ?
C12 N5 C17 127.8(4) . . ?
N6 N5 C17 117.8(4) . . ?
N1 C5 C4 102.5(4) . . ?
C13 N6 N5 102.4(4) . . ?
C11 C6 C7 120.7(5) . . ?
C11 C6 N2 118.9(5) . . ?
C7 C6 N2 120.4(5) . . ?
C6 C7 C8 119.7(5) . . ?
C9 C8 C7 119.8(5) . . ?
C8 C9 C10 119.8(5) . . ?
C11 C10 C9 120.7(5) . . ?
C10 C11 C6 119.4(5) . . ?
N5 C12 N4 102.0(4) . . ?
N5 C12 Au2 129.9(4) . . ?
N4 C12 Au2 128.1(4) . . ?
N6 C13 N4 111.8(5) . . ?
N6 C13 C14 137.4(5) . . ?
N4 C13 C14 110.8(5) . . ?
C13 C14 C15 100.7(5) . . ?
C16 C15 C14 105.3(5) . . ?
N4 C16 C15 101.4(4) . . ?
C18 C17 C22 120.7(5) . . ?
C18 C17 N5 118.2(5) . . ?
C22 C17 N5 121.1(5) . . ?
C17 C18 C19 119.6(5) . . ?
C20 C19 C18 119.7(5) . . ?
C21 C20 C19 120.2(5) . . ?
C22 C21 C20 120.5(5) . . ?
C21 C22 C17 119.4(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 1.979(5) . ?
Au1 Cl1 2.2880(13) . ?
N1 C1 1.344(7) . ?
N1 C2 1.349(7) . ?
N1 C5 1.459(7) . ?
C1 N2 1.361(7) . ?
Au2 C12 1.972(5) . ?
Au2 Cl2 2.2835(13) . ?
N2 N3 1.395(6) . ?
N2 C6 1.426(7) . ?
C2 N3 1.299(7) . ?
C2 C3 1.496(8) . ?
C3 C4 1.555(8) . ?
N4 C13 1.365(7) . ?
N4 C12 1.363(7) . ?
N4 C16 1.467(7) . ?
C4 C5 1.527(8) . ?
N5 C12 1.347(7) . ?
N5 N6 1.395(6) . ?
N5 C17 1.429(7) . ?
N6 C13 1.298(7) . ?
C6 C11 1.384(8) . ?
C6 C7 1.387(8) . ?
C7 C8 1.392(8) . ?
C8 C9 1.390(8) . ?
C9 C10 1.388(8) . ?
C10 C11 1.381(8) . ?
C13 C14 1.487(8) . ?
C14 C15 1.570(9) . ?
C15 C16 1.531(8) . ?
C17 C18 1.388(8) . ?
C17 C22 1.391(8) . ?
C18 C19 1.385(8) . ?
C19 C20 1.392(8) . ?
C20 C21 1.384(8) . ?
C21 C22 1.374(8) . ?
|
1100867.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100867.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100867
loop_
_publ_author_name
'Slugovc, Christian'
'Burtscher, Daniel'
'Stelzer, Franz'
'Mereiter, Kurt'
_publ_section_title
;
Thermally Switchable Olefin Metathesis Initiators Bearing Chelating
Carbenes:  Influence of the Chelate's Ring Size
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2255
_journal_page_last 2258
_journal_paper_doi 10.1021/om050141f
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C35 H37 Cl2 N3 Ru'
_chemical_formula_sum 'C35 H37 Cl2 N3 Ru'
_chemical_formula_weight 671.65
_chemical_name_common RuCl2(H2IMes)(=CH-Ph-CH=N-Ph)
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.486(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 38.8057(19)
_cell_length_b 10.9768(6)
_cell_length_c 15.7674(8)
_cell_measurement_reflns_used 5927
_cell_measurement_temperature 297(2)
_cell_measurement_theta_max 26.42
_cell_measurement_theta_min 2.16
_cell_volume 6531.1(6)
_diffrn_ambient_temperature 297(2)
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0285
_diffrn_reflns_av_sigmaI/netI 0.0234
_diffrn_reflns_limit_h_max 54
_diffrn_reflns_limit_h_min -54
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 47727
_diffrn_reflns_theta_max 30.01
_diffrn_reflns_theta_min 2.16
_diffrn_standards_decay_% 0
_exptl_absorpt_coefficient_mu 0.671
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_correction_T_min 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'program SADABS, V2.10'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.366
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2768
_exptl_crystal_size_max 0.65
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.03
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 377
_refine_ls_number_reflns 9398
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.046
_refine_ls_R_factor_all 0.0742
_refine_ls_R_factor_gt 0.0498
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+7.7415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1207
_refine_ls_wR_factor_ref 0.1342
_reflns_number_gt 6673
_reflns_number_total 9398
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100867
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.121135(7) 0.24779(3) 0.412208(17) 0.04263(9) Uani 0.750(2) 1 d P A 1
Cl1 Cl 0.09246(3) 0.12789(10) 0.29337(6) 0.0611(3) Uani 0.750(2) 1 d P A 1
Cl2 Cl 0.13789(3) 0.38916(10) 0.52809(7) 0.0694(3) Uani 0.750(2) 1 d P A 1
C41 C 0.16598(11) 0.2175(4) 0.3998(3) 0.0564(9) Uani 0.750(2) 1 d P A 1
H41A H 0.1819 0.1869 0.4486 0.068 Uiso 0.750(2) 1 calc PR A 1
C42 C 0.17976(10) 0.2358(3) 0.3219(2) 0.0505(8) Uani 0.750(2) 1 d P A 1
C43 C 0.20790(12) 0.1719(4) 0.3083(3) 0.0706(12) Uani 0.750(2) 1 d P A 1
H43A H 0.2193 0.1167 0.3503 0.085 Uiso 0.750(2) 1 calc PR A 1
C44 C 0.22012(13) 0.1873(5) 0.2327(4) 0.0827(15) Uani 0.750(2) 1 d P A 1
H44A H 0.2388 0.1397 0.2238 0.099 Uiso 0.750(2) 1 calc PR A 1
C45 C 0.20536(17) 0.2695(6) 0.1728(4) 0.0879(18) Uani 0.750(2) 1 d P A 1
H45A H 0.2142 0.2800 0.1232 0.105 Uiso 0.750(2) 1 calc PR A 1
C46 C 0.17746(14) 0.3381(5) 0.1839(3) 0.0728(12) Uani 0.750(2) 1 d P A 1
H46A H 0.1675 0.3959 0.1421 0.087 Uiso 0.750(2) 1 calc PR A 1
C47 C 0.16379(10) 0.3224(4) 0.2574(2) 0.0534(8) Uani 0.750(2) 1 d P A 1
C48 C 0.13520(11) 0.3997(4) 0.2642(3) 0.0590(9) Uani 0.750(2) 1 d P A 1
H48A H 0.1284 0.4603 0.2224 0.071 Uiso 0.750(2) 1 calc PR A 1
N49 N 0.11821(9) 0.3911(3) 0.3242(2) 0.0538(7) Uani 0.750(2) 1 d P A 1
C51 C 0.09119(11) 0.4812(4) 0.3290(3) 0.0562(9) Uani 0.750(2) 1 d P A 1
C52 C 0.05787(12) 0.4439(4) 0.3324(3) 0.0714(12) Uani 0.750(2) 1 d P A 1
H52A H 0.0525 0.3613 0.3324 0.086 Uiso 0.750(2) 1 calc PR A 1
C53 C 0.03252(15) 0.5290(5) 0.3358(4) 0.0882(16) Uani 0.750(2) 1 d P A 1
H53A H 0.0096 0.5039 0.3358 0.106 Uiso 0.750(2) 1 calc PR A 1
C54 C 0.04046(17) 0.6510(5) 0.3392(4) 0.0878(16) Uani 0.750(2) 1 d P A 1
H54A H 0.0231 0.7079 0.3431 0.105 Uiso 0.750(2) 1 calc PR A 1
C55 C 0.07412(15) 0.6894(4) 0.3369(3) 0.0733(12) Uani 0.750(2) 1 d P A 1
H55A H 0.0795 0.7720 0.3385 0.088 Uiso 0.750(2) 1 calc PR A 1
C56 C 0.09952(13) 0.6043(4) 0.3322(3) 0.0715(12) Uani 0.750(2) 1 d P A 1
H56A H 0.1223 0.6291 0.3311 0.086 Uiso 0.750(2) 1 calc PR A 1
C11 C 0.11484(8) 0.1093(3) 0.49779(18) 0.0530(6) Uani 1 1 d . . .
N12 N 0.13789(7) 0.0290(3) 0.54283(18) 0.0667(7) Uani 1 1 d . A .
C13 C 0.12205(10) -0.0564(4) 0.5949(3) 0.0930(14) Uani 1 1 d . . .
H13A H 0.1344 -0.0539 0.6559 0.112 Uiso 1 1 calc R A .
H13B H 0.1224 -0.1392 0.5736 0.112 Uiso 1 1 calc R . .
C14 C 0.08474(10) -0.0099(4) 0.5819(3) 0.0913(14) Uani 1 1 d . A .
H14A H 0.0676 -0.0736 0.5602 0.110 Uiso 1 1 calc R . .
H14B H 0.0804 0.0222 0.6358 0.110 Uiso 1 1 calc R . .
N15 N 0.08313(7) 0.0870(2) 0.51678(17) 0.0620(7) Uani 1 1 d . A .
C21 C 0.17457(8) 0.0146(3) 0.5419(2) 0.0611(8) Uani 1 1 d . . .
C22 C 0.18388(9) -0.0618(3) 0.4802(2) 0.0648(8) Uani 1 1 d . A .
C23 C 0.21994(9) -0.0764(3) 0.4842(3) 0.0743(9) Uani 1 1 d . . .
H23A H 0.2268 -0.1272 0.4439 0.089 Uiso 1 1 calc R A .
C24 C 0.24586(9) -0.0178(4) 0.5460(3) 0.0791(10) Uani 1 1 d . A .
C25 C 0.23539(10) 0.0560(4) 0.6048(3) 0.0785(10) Uani 1 1 d . . .
H25A H 0.2527 0.0966 0.6459 0.094 Uiso 1 1 calc R A .
C26 C 0.20028(9) 0.0730(3) 0.6061(2) 0.0697(9) Uani 1 1 d . A .
C27 C 0.15681(11) -0.1275(4) 0.4138(3) 0.0933(13) Uani 1 1 d . . .
H27A H 0.1415 -0.0696 0.3778 0.140 Uiso 1 1 calc R A .
H27B H 0.1430 -0.1789 0.4425 0.140 Uiso 1 1 calc R . .
H27C H 0.1684 -0.1765 0.3783 0.140 Uiso 1 1 calc R . .
C28 C 0.28482(11) -0.0359(5) 0.5472(4) 0.1198(19) Uani 1 1 d . . .
H28A H 0.2984 -0.0382 0.6065 0.180 Uiso 1 1 calc R A .
H28B H 0.2929 0.0303 0.5171 0.180 Uiso 1 1 calc R . .
H28C H 0.2878 -0.1113 0.5189 0.180 Uiso 1 1 calc R . .
C29 C 0.19010(12) 0.1520(5) 0.6744(3) 0.0972(13) Uani 1 1 d . . .
H29A H 0.1736 0.1090 0.7004 0.146 Uiso 1 1 calc R A .
H29B H 0.1793 0.2256 0.6477 0.146 Uiso 1 1 calc R . .
H29C H 0.2109 0.1720 0.7185 0.146 Uiso 1 1 calc R . .
C31 C 0.05053(8) 0.1506(3) 0.48547(19) 0.0539(6) Uani 1 1 d . . .
C32 C 0.02525(9) 0.1023(3) 0.4164(2) 0.0596(7) Uani 1 1 d . A .
C33 C -0.00614(9) 0.1656(3) 0.3876(2) 0.0661(8) Uani 1 1 d . . .
H33A H -0.0229 0.1359 0.3399 0.079 Uiso 1 1 calc R A .
C34 C -0.01337(9) 0.2720(3) 0.4277(3) 0.0709(9) Uani 1 1 d . A .
C35 C 0.01135(9) 0.3137(3) 0.4977(2) 0.0693(9) Uani 1 1 d . . .
H35A H 0.0065 0.3841 0.5256 0.083 Uiso 1 1 calc R A .
C36 C 0.04360(9) 0.2551(3) 0.5292(2) 0.0623(8) Uani 1 1 d . A .
C37 C 0.03051(11) -0.0194(3) 0.3774(3) 0.0825(11) Uani 1 1 d . . .
H37A H 0.0221 -0.0827 0.4095 0.124 Uiso 1 1 calc R A .
H37B H 0.0553 -0.0315 0.3803 0.124 Uiso 1 1 calc R . .
H37C H 0.0175 -0.0216 0.3177 0.124 Uiso 1 1 calc R . .
C38 C -0.04864(11) 0.3366(4) 0.3947(4) 0.1020(15) Uani 1 1 d . . .
H38A H -0.0597 0.3502 0.4424 0.153 Uiso 1 1 calc R A .
H38B H -0.0638 0.2871 0.3514 0.153 Uiso 1 1 calc R . .
H38C H -0.0447 0.4134 0.3694 0.153 Uiso 1 1 calc R . .
C39 C 0.06877(12) 0.3021(5) 0.6092(3) 0.0932(13) Uani 1 1 d . . .
H39A H 0.0556 0.3381 0.6474 0.140 Uiso 1 1 calc R A .
H39B H 0.0840 0.3624 0.5928 0.140 Uiso 1 1 calc R . .
H39C H 0.0829 0.2361 0.6386 0.140 Uiso 1 1 calc R . .
Ru' Ru 0.1243 0.2217 0.4085 0.060 Uiso 0.25 1 d P A 2
Cl1' Cl 0.1549 0.3492 0.5189 0.071 Uiso 0.25 1 d P A 2
Cl2' Cl 0.1059 0.0761 0.2966 0.066 Uiso 0.25 1 d P A 2
C41' C 0.0930 0.3293 0.3819 0.117 Uiso 0.25 1 d P A 2
H41' H 0.0727 0.2839 0.3804 0.141 Uiso 0.25 1 d P A 2
C42' C 0.0784 0.4469 0.3601 0.049 Uiso 0.25 1 d P A 2
C43' C 0.0494 0.5146 0.3707 0.066 Uiso 0.25 1 d P A 2
H43' H 0.0310 0.4765 0.3890 0.080 Uiso 0.25 1 d P A 2
C44' C 0.0480 0.6390 0.3541 0.090 Uiso 0.25 1 d P A 2
H44' H 0.0286 0.6843 0.3612 0.108 Uiso 0.25 1 d P A 2
C45' C 0.0756 0.6958 0.3268 0.132 Uiso 0.25 1 d P A 2
H45' H 0.0746 0.7791 0.3157 0.158 Uiso 0.25 1 d P A 2
C46' C 0.1045 0.6282 0.3162 0.076 Uiso 0.25 1 d P A 2
H46' H 0.1230 0.6662 0.2979 0.092 Uiso 0.25 1 d P A 2
C47' C 0.1060 0.5037 0.3328 0.052 Uiso 0.25 1 d P A 2
C48' C 0.1337 0.4440 0.2988 0.058 Uiso 0.25 1 d P A 2
H48' H 0.1439 0.4859 0.2596 0.070 Uiso 0.25 1 d P A 2
N49' N 0.1445 0.3343 0.3217 0.051 Uiso 0.25 1 d P A 2
C51' C 0.1742 0.2796 0.2933 0.056 Uiso 0.25 1 d P A 2
C52' C 0.1974 0.2095 0.3547 0.097 Uiso 0.25 1 d P A 2
H52' H 0.1935 0.1997 0.4103 0.117 Uiso 0.25 1 d P A 2
C53' C 0.2264 0.1542 0.3329 0.140 Uiso 0.25 1 d P A 2
H53' H 0.2419 0.1073 0.3740 0.168 Uiso 0.25 1 d P A 2
C54' C 0.2322 0.1689 0.2498 0.077 Uiso 0.25 1 d P A 2
H54' H 0.2516 0.1319 0.2352 0.092 Uiso 0.25 1 d P A 2
C55' C 0.2090 0.2390 0.1884 0.104 Uiso 0.25 1 d P A 2
H55' H 0.2128 0.2488 0.1328 0.125 Uiso 0.25 1 d P A 2
C56' C 0.1800 0.2943 0.2102 0.078 Uiso 0.25 1 d P A 2
H56' H 0.1645 0.3412 0.1691 0.094 Uiso 0.25 1 d P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru 0.04841(16) 0.03979(14) 0.04327(15) -0.00041(11) 0.01797(11) -0.00544(11)
Cl1 0.0705(6) 0.0625(6) 0.0472(5) -0.0065(4) 0.0078(4) -0.0120(5)
Cl2 0.0875(8) 0.0591(6) 0.0631(6) -0.0166(5) 0.0201(5) -0.0180(5)
C41 0.057(2) 0.055(2) 0.060(2) 0.0049(17) 0.0198(18) -0.0040(17)
C42 0.056(2) 0.0443(18) 0.0516(19) 0.0002(15) 0.0139(16) -0.0132(15)
C43 0.065(3) 0.056(2) 0.093(3) -0.004(2) 0.022(2) -0.009(2)
C44 0.063(3) 0.080(3) 0.113(4) -0.027(3) 0.036(3) -0.003(2)
C45 0.104(4) 0.102(4) 0.077(3) -0.020(3) 0.061(3) -0.032(3)
C46 0.090(3) 0.073(3) 0.056(2) 0.003(2) 0.018(2) -0.015(3)
C47 0.054(2) 0.057(2) 0.0497(19) -0.0056(16) 0.0126(16) -0.0122(17)
C48 0.068(2) 0.052(2) 0.061(2) -0.0017(17) 0.0231(19) -0.0067(18)
N49 0.0600(18) 0.0467(16) 0.0551(17) 0.0038(13) 0.0144(14) -0.0129(14)
C51 0.057(2) 0.057(2) 0.054(2) -0.0054(17) 0.0131(17) -0.0047(17)
C52 0.072(3) 0.055(2) 0.097(3) 0.002(2) 0.038(2) -0.004(2)
C53 0.073(3) 0.086(4) 0.117(4) -0.001(3) 0.045(3) 0.002(3)
C54 0.113(4) 0.057(3) 0.104(4) -0.004(3) 0.047(3) 0.014(3)
C55 0.098(4) 0.044(2) 0.075(3) -0.007(2) 0.014(3) -0.001(2)
C56 0.073(3) 0.063(3) 0.076(3) -0.006(2) 0.012(2) -0.010(2)
C11 0.0598(16) 0.0511(15) 0.0510(15) 0.0010(12) 0.0189(13) -0.0054(12)
N12 0.0561(15) 0.0723(17) 0.0745(17) 0.0245(14) 0.0209(13) 0.0018(13)
C13 0.062(2) 0.107(3) 0.116(3) 0.059(3) 0.033(2) 0.012(2)
C14 0.067(2) 0.102(3) 0.111(3) 0.062(3) 0.035(2) 0.014(2)
N15 0.0561(14) 0.0666(16) 0.0663(15) 0.0222(13) 0.0207(12) 0.0057(12)
C21 0.0534(16) 0.0634(18) 0.0684(19) 0.0131(15) 0.0180(14) 0.0000(14)
C22 0.0625(18) 0.0538(17) 0.078(2) 0.0015(15) 0.0150(16) -0.0051(14)
C23 0.067(2) 0.069(2) 0.092(3) -0.0072(19) 0.0302(18) -0.0028(17)
C24 0.058(2) 0.082(2) 0.099(3) -0.004(2) 0.0204(19) -0.0100(17)
C25 0.062(2) 0.082(2) 0.088(3) -0.010(2) 0.0104(18) -0.0133(18)
C26 0.068(2) 0.075(2) 0.067(2) -0.0019(17) 0.0175(16) -0.0026(17)
C27 0.073(2) 0.093(3) 0.104(3) -0.021(2) 0.002(2) -0.003(2)
C28 0.063(2) 0.136(4) 0.168(5) -0.027(4) 0.042(3) -0.011(3)
C29 0.093(3) 0.118(4) 0.078(3) -0.019(2) 0.014(2) 0.012(3)
C31 0.0552(16) 0.0523(15) 0.0558(16) 0.0062(12) 0.0165(13) 0.0005(12)
C32 0.0657(18) 0.0477(15) 0.0666(18) 0.0020(13) 0.0179(15) -0.0026(13)
C33 0.0630(18) 0.0583(18) 0.073(2) 0.0043(15) 0.0075(15) -0.0062(15)
C34 0.0612(19) 0.0564(19) 0.097(3) 0.0159(17) 0.0221(18) 0.0060(14)
C35 0.071(2) 0.0560(18) 0.088(2) -0.0087(17) 0.0338(19) -0.0023(15)
C36 0.0635(18) 0.0683(19) 0.0602(17) -0.0044(15) 0.0249(14) -0.0082(15)
C37 0.087(3) 0.0561(19) 0.106(3) -0.0153(19) 0.024(2) -0.0095(18)
C38 0.070(2) 0.077(3) 0.156(4) 0.021(3) 0.021(3) 0.016(2)
C39 0.094(3) 0.121(3) 0.067(2) -0.029(2) 0.022(2) -0.016(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100868.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100868.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100868
loop_
_publ_author_name
'Slugovc, Christian'
'Burtscher, Daniel'
'Stelzer, Franz'
'Mereiter, Kurt'
_publ_section_title
;
Thermally Switchable Olefin Metathesis Initiators Bearing Chelating
Carbenes:  Influence of the Chelate's Ring Size
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2255
_journal_page_last 2258
_journal_paper_doi 10.1021/om050141f
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C35 H37 Cl2 N3 Ru'
_chemical_formula_sum 'C35 H37 Cl2 N3 Ru'
_chemical_formula_weight 671.65
_chemical_name_common RuCl2(H2IMes)(=CH-Ph-N=CH-Ph).solv
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 92.59(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 27.76(4)
_cell_length_b 15.49(2)
_cell_length_c 17.149(5)
_cell_measurement_reflns_used 8020
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.02
_cell_measurement_theta_min 2.58
_cell_volume 7366(15)
_diffrn_ambient_temperature 296(2)
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0596
_diffrn_reflns_av_sigmaI/netI 0.0610
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 20346
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 2.38
_diffrn_standards_decay_% ?
_exptl_absorpt_coefficient_mu 0.595
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_correction_T_min 0.86
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'program SADABS'
_exptl_crystal_colour darkgreen
_exptl_crystal_density_diffrn 1.211
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2768
_exptl_crystal_size_max 0.75
_exptl_crystal_size_mid 0.70
_exptl_crystal_size_min 0.65
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.176
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 401
_refine_ls_number_reflns 6369
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.176
_refine_ls_R_factor_all 0.0996
_refine_ls_R_factor_gt 0.0586
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+41.3157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1214
_refine_ls_wR_factor_ref 0.1692
_reflns_number_gt 4290
_reflns_number_total 6369
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100868
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.159305(19) 0.57300(4) 0.05088(3) 0.05459(18) Uani 1 1 d . . .
Cl1 Cl 0.20587(7) 0.66486(12) 0.13205(11) 0.0706(5) Uani 1 1 d . . .
Cl2 Cl 0.14251(7) 0.45126(13) -0.02697(10) 0.0732(5) Uani 1 1 d . . .
C11 C 0.1292(2) 0.5294(4) 0.1499(3) 0.0529(14) Uani 1 1 d . . .
N12 N 0.09413(19) 0.5663(4) 0.1904(3) 0.0623(14) Uani 1 1 d . . .
C13 C 0.0908(3) 0.5312(7) 0.2694(4) 0.094(3) Uani 1 1 d . . .
H13A H 0.0590 0.5078 0.2770 0.113 Uiso 1 1 calc R . .
H13B H 0.0978 0.5753 0.3085 0.113 Uiso 1 1 calc R . .
C14 C 0.1280(3) 0.4620(6) 0.2739(4) 0.088(3) Uani 1 1 d . . .
H14A H 0.1513 0.4718 0.3167 0.105 Uiso 1 1 calc R . .
H14B H 0.1134 0.4056 0.2799 0.105 Uiso 1 1 calc R . .
N15 N 0.1504(2) 0.4701(4) 0.1972(3) 0.0635(14) Uani 1 1 d . . .
C21 C 0.0564(3) 0.6223(5) 0.1614(4) 0.0703(19) Uani 1 1 d . . .
C22 C 0.0588(3) 0.7097(6) 0.1763(5) 0.077(2) Uani 1 1 d . . .
C23 C 0.0213(3) 0.7616(6) 0.1458(5) 0.090(2) Uani 1 1 d . . .
H23 H 0.0228 0.8209 0.1544 0.108 Uiso 1 1 calc R . .
C24 C -0.0178(3) 0.7286(6) 0.1037(5) 0.083(2) Uani 1 1 d . . .
C25 C -0.0200(3) 0.6414(7) 0.0915(5) 0.082(2) Uani 1 1 d . . .
H25 H -0.0464 0.6185 0.0633 0.098 Uiso 1 1 calc R . .
C26 C 0.0165(3) 0.5854(5) 0.1202(4) 0.0687(18) Uani 1 1 d . . .
C27 C 0.1010(3) 0.7484(6) 0.2219(6) 0.105(3) Uani 1 1 d . . .
H27A H 0.0957 0.7445 0.2767 0.157 Uiso 1 1 calc R . .
H27B H 0.1045 0.8079 0.2075 0.157 Uiso 1 1 calc R . .
H27C H 0.1299 0.7175 0.2105 0.157 Uiso 1 1 calc R . .
C28 C -0.0573(4) 0.7886(8) 0.0709(6) 0.124(4) Uani 1 1 d . . .
H28A H -0.0614 0.8357 0.1063 0.186 Uiso 1 1 calc R . .
H28B H -0.0870 0.7571 0.0645 0.186 Uiso 1 1 calc R . .
H28C H -0.0484 0.8106 0.0213 0.186 Uiso 1 1 calc R . .
C29 C 0.0130(3) 0.4916(6) 0.1039(5) 0.086(2) Uani 1 1 d . . .
H29A H -0.0190 0.4781 0.0838 0.129 Uiso 1 1 calc R . .
H29B H 0.0197 0.4599 0.1513 0.129 Uiso 1 1 calc R . .
H29C H 0.0359 0.4760 0.0661 0.129 Uiso 1 1 calc R . .
C31 C 0.1853(3) 0.4057(4) 0.1778(4) 0.0605(17) Uani 1 1 d . . .
C32 C 0.2334(3) 0.4156(5) 0.2045(4) 0.0684(18) Uani 1 1 d . . .
C33 C 0.2650(3) 0.3492(6) 0.1897(5) 0.088(2) Uani 1 1 d . . .
H33 H 0.2970 0.3549 0.2074 0.106 Uiso 1 1 calc R . .
C34 C 0.2514(3) 0.2754(6) 0.1502(5) 0.087(2) Uani 1 1 d . . .
C35 C 0.2030(4) 0.2668(5) 0.1277(5) 0.086(2) Uani 1 1 d . . .
H35 H 0.1926 0.2165 0.1024 0.103 Uiso 1 1 calc R . .
C36 C 0.1695(3) 0.3307(5) 0.1417(4) 0.0720(19) Uani 1 1 d . . .
C37 C 0.2508(3) 0.4927(6) 0.2494(5) 0.096(3) Uani 1 1 d . . .
H37A H 0.2592 0.4762 0.3022 0.143 Uiso 1 1 calc R . .
H37B H 0.2257 0.5354 0.2492 0.143 Uiso 1 1 calc R . .
H37C H 0.2785 0.5163 0.2258 0.143 Uiso 1 1 calc R . .
C38 C 0.2859(4) 0.2034(7) 0.1313(7) 0.125(4) Uani 1 1 d . . .
H38A H 0.3020 0.1833 0.1786 0.187 Uiso 1 1 calc R . .
H38B H 0.3093 0.2246 0.0965 0.187 Uiso 1 1 calc R . .
H38C H 0.2682 0.1567 0.1068 0.187 Uiso 1 1 calc R . .
C39 C 0.1166(3) 0.3150(6) 0.1208(5) 0.093(3) Uani 1 1 d . . .
H39A H 0.1124 0.2574 0.1009 0.140 Uiso 1 1 calc R . .
H39B H 0.1056 0.3557 0.0817 0.140 Uiso 1 1 calc R . .
H39C H 0.0982 0.3219 0.1665 0.140 Uiso 1 1 calc R . .
C41 C 0.1096(2) 0.6390(5) 0.0112(4) 0.0643(17) Uani 1 1 d . . .
H41 H 0.0801 0.6378 0.0347 0.077 Uiso 1 1 calc R . .
C42 C 0.1157(2) 0.6925(5) -0.0556(4) 0.0654(18) Uani 1 1 d . . .
C43 C 0.0799(3) 0.7427(5) -0.0922(5) 0.083(2) Uani 1 1 d . . .
H43 H 0.0490 0.7424 -0.0735 0.100 Uiso 1 1 calc R . .
C44 C 0.0896(4) 0.7929(7) -0.1562(6) 0.103(3) Uani 1 1 d . . .
H44 H 0.0656 0.8274 -0.1794 0.123 Uiso 1 1 calc R . .
C45 C 0.1352(4) 0.7915(6) -0.1856(5) 0.092(3) Uani 1 1 d . . .
H45 H 0.1414 0.8248 -0.2291 0.110 Uiso 1 1 calc R . .
C46 C 0.1718(3) 0.7419(5) -0.1517(4) 0.076(2) Uani 1 1 d . . .
H46 H 0.2023 0.7419 -0.1719 0.092 Uiso 1 1 calc R . .
C47 C 0.1622(2) 0.6916(4) -0.0865(4) 0.0583(15) Uani 1 1 d . . .
N48 N 0.19543(19) 0.6345(4) -0.0458(3) 0.0584(13) Uani 1 1 d . . .
C49 C 0.2404(3) 0.6394(5) -0.0595(4) 0.0639(17) Uani 1 1 d . . .
H49 H 0.2492 0.6829 -0.0934 0.077 Uiso 1 1 calc R . .
C51 C 0.2791(3) 0.5843(5) -0.0279(4) 0.0683(18) Uani 1 1 d . . .
C52 C 0.2717(3) 0.5048(6) 0.0049(6) 0.093(3) Uani 1 1 d . . .
H52 H 0.2406 0.4846 0.0112 0.111 Uiso 1 1 calc R . .
C53 C 0.3112(4) 0.4553(8) 0.0282(7) 0.121(4) Uani 1 1 d . . .
H53 H 0.3071 0.4001 0.0483 0.146 Uiso 1 1 calc R . .
C54 C 0.3573(4) 0.4893(10) 0.0212(7) 0.128(4) Uani 1 1 d . . .
H54 H 0.3839 0.4567 0.0381 0.154 Uiso 1 1 calc R . .
C55 C 0.3644(4) 0.5690(8) -0.0098(9) 0.129(4) Uani 1 1 d . . .
H55 H 0.3953 0.5913 -0.0132 0.155 Uiso 1 1 calc R . .
C56 C 0.3252(3) 0.6152(6) -0.0357(6) 0.093(3) Uani 1 1 d . . .
H56 H 0.3296 0.6686 -0.0591 0.111 Uiso 1 1 calc R . .
C1S C 0.007(4) 0.975(2) -0.197(9) 1.01(14) Uani 1 1 d . . .
C2S C 0.050(2) 0.949(3) -0.334(4) 0.53(4) Uani 1 1 d . . .
C3S C -0.022(2) 0.926(4) 0.155(3) 0.100 Uiso 0.179(19) 1 d P . .
C4S C 0.0000 0.931(3) -0.2500 0.135(18) Uiso 0.62(8) 2 d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru 0.0562(3) 0.0549(3) 0.0529(3) 0.0006(2) 0.0048(2) -0.0029(2)
Cl1 0.0756(11) 0.0648(10) 0.0709(10) 0.0004(8) -0.0026(8) -0.0143(9)
Cl2 0.0855(12) 0.0740(11) 0.0605(10) -0.0087(8) 0.0079(9) -0.0136(9)
C11 0.060(4) 0.052(3) 0.047(3) 0.000(3) 0.005(3) 0.002(3)
N12 0.062(3) 0.075(4) 0.050(3) 0.006(3) 0.005(2) 0.011(3)
C13 0.105(6) 0.120(7) 0.059(4) 0.019(5) 0.023(4) 0.040(6)
C14 0.113(6) 0.098(6) 0.055(4) 0.015(4) 0.026(4) 0.034(5)
N15 0.068(3) 0.070(4) 0.053(3) 0.006(3) 0.011(3) 0.017(3)
C21 0.070(4) 0.082(5) 0.060(4) 0.005(4) 0.009(3) 0.015(4)
C22 0.081(5) 0.081(5) 0.070(4) -0.006(4) 0.003(4) 0.020(4)
C23 0.098(6) 0.083(6) 0.089(6) -0.009(5) 0.001(5) 0.026(5)
C24 0.076(5) 0.100(7) 0.075(5) 0.012(5) 0.010(4) 0.020(5)
C25 0.062(4) 0.111(7) 0.073(5) 0.006(5) 0.008(4) 0.003(5)
C26 0.067(4) 0.083(5) 0.057(4) 0.003(4) 0.017(3) -0.008(4)
C27 0.109(7) 0.092(7) 0.112(7) -0.021(6) -0.014(6) 0.021(6)
C28 0.104(7) 0.143(10) 0.123(8) 0.018(7) -0.008(6) 0.064(7)
C29 0.076(5) 0.100(6) 0.083(5) -0.002(5) 0.014(4) -0.013(5)
C31 0.077(4) 0.057(4) 0.047(3) 0.005(3) 0.005(3) 0.012(3)
C32 0.070(4) 0.069(4) 0.065(4) 0.007(4) -0.005(3) 0.011(4)
C33 0.087(6) 0.084(6) 0.093(6) 0.007(5) 0.002(5) 0.024(5)
C34 0.097(6) 0.083(6) 0.081(5) 0.011(5) 0.016(5) 0.030(5)
C35 0.127(8) 0.055(4) 0.076(5) -0.003(4) 0.013(5) 0.017(5)
C36 0.089(5) 0.066(5) 0.061(4) 0.011(3) 0.002(4) 0.008(4)
C37 0.103(6) 0.081(6) 0.099(6) -0.008(5) -0.032(5) 0.001(5)
C38 0.135(9) 0.103(8) 0.139(9) 0.010(7) 0.039(7) 0.060(7)
C39 0.108(7) 0.084(6) 0.085(6) 0.004(5) -0.011(5) -0.011(5)
C41 0.058(4) 0.064(4) 0.071(4) 0.001(3) 0.008(3) 0.002(3)
C42 0.056(4) 0.071(4) 0.069(4) -0.017(4) 0.000(3) 0.011(3)
C43 0.075(5) 0.087(6) 0.088(5) 0.026(4) -0.003(4) 0.029(4)
C44 0.112(7) 0.103(7) 0.093(6) 0.027(5) -0.008(5) 0.036(6)
C45 0.119(7) 0.086(6) 0.071(5) 0.025(4) 0.011(5) 0.004(5)
C46 0.086(5) 0.072(5) 0.071(5) 0.011(4) 0.008(4) -0.009(4)
C47 0.068(4) 0.052(4) 0.055(3) -0.001(3) -0.002(3) -0.006(3)
N48 0.060(3) 0.057(3) 0.059(3) 0.004(2) 0.003(2) -0.001(3)
C49 0.076(5) 0.058(4) 0.058(4) 0.003(3) 0.005(3) -0.011(3)
C51 0.072(4) 0.071(5) 0.063(4) -0.003(4) 0.013(3) 0.005(4)
C52 0.075(5) 0.091(6) 0.114(7) 0.029(5) 0.029(5) 0.019(5)
C53 0.095(7) 0.130(9) 0.141(10) 0.040(7) 0.030(7) 0.033(7)
C54 0.088(7) 0.150(11) 0.147(10) 0.028(9) 0.012(7) 0.051(8)
C55 0.070(6) 0.110(9) 0.206(14) 0.001(9) 0.004(7) 0.017(6)
C56 0.059(4) 0.085(6) 0.136(8) 0.008(5) 0.022(5) -0.001(4)
C1S 0.89(16) 0.13(2) 1.9(3) -0.27(7) -0.98(19) 0.19(5)
C2S 0.54(7) 0.41(6) 0.66(8) 0.36(6) 0.34(6) 0.22(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100869.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100869.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100869
loop_
_publ_author_name
'Ruiz, J.'
'Quesada, R.'
'Vivanco, M.'
'Castellano, E. E.'
'Piro, O. E.'
_publ_section_title
;
Stepwise Formation of \s-Alkynyl, Vinylidene, and Vinylphosphonium
Complexes of Manganese(I)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2542
_journal_page_last 2545
_journal_paper_doi 10.1021/om050146c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C64 H50 Mn2 O10 P4'
_chemical_formula_weight 1212.80
_chemical_name_systematic
'fac-[(2-methoxycarbonylethynil)tricarbonyl(bis(diphenylphosphanyl)methane) manganese(I)]'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 69.7090(5)
_cell_angle_beta 88.5567(5)
_cell_angle_gamma 89.6242(5)
_cell_formula_units_Z 2
_cell_length_a 9.5092(1)
_cell_length_b 17.3418(2)
_cell_length_c 18.1765(2)
_cell_measurement_reflns_used 45152
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.00
_cell_measurement_theta_min 1.19
_cell_volume 2810.52(5)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD with \f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0452
_diffrn_reflns_av_sigmaI/netI 0.0315
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 45152
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 1.19
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.624
_exptl_absorpt_correction_T_max 0.945
_exptl_absorpt_correction_T_min 0.770
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.433
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1248
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.20
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 723
_refine_ls_number_reflns 11005
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0394
_refine_ls_R_factor_gt 0.0320
_refine_ls_shift/su_max 0.011
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.3205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0939
_refine_ls_wR_factor_ref 0.1016
_reflns_number_gt 9477
_reflns_number_total 11005
_reflns_threshold_expression >2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.3205P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.3205P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100869
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.30073(2) 0.647735(13) -0.000238(13) 0.01378(8) Uani 1 d . . .
P11 P 0.43691(4) 0.64401(2) 0.10483(2) 0.01402(9) Uani 1 d . . .
P12 P 0.40707(4) 0.77466(2) -0.03221(2) 0.01370(9) Uani 1 d . . .
O11 O 0.51806(13) 0.58521(8) -0.08568(7) 0.0282(3) Uani 1 d . . .
O12 O 0.11833(15) 0.69412(9) -0.13880(8) 0.0391(3) Uani 1 d . . .
O13 O 0.17600(13) 0.48184(7) 0.07763(7) 0.0261(3) Uani 1 d . . .
O14 O -0.14650(13) 0.79924(8) 0.06368(8) 0.0313(3) Uani 1 d . . .
O15 O -0.10978(13) 0.71785(9) 0.18347(7) 0.0345(3) Uani 1 d . . .
C11 C 0.43648(17) 0.60952(10) -0.05136(9) 0.0183(3) Uani 1 d . . .
C12 C 0.18901(17) 0.67542(10) -0.08562(10) 0.0222(3) Uani 1 d . . .
C13 C 0.22580(16) 0.54518(10) 0.04668(9) 0.0190(3) Uani 1 d . . .
C14 C 0.14933(16) 0.68841(9) 0.05356(9) 0.0160(3) Uani 1 d . . .
C15 C 0.04961(17) 0.71236(10) 0.08206(9) 0.0188(3) Uani 1 d . . .
C16 C -0.07314(17) 0.74567(10) 0.10703(10) 0.0207(3) Uani 1 d . . .
C17 C -0.0260(2) 0.65471(13) 0.23614(11) 0.0389(5) Uani 1 d . . .
H17A H -0.0590 0.6444 0.2902 0.058 Uiso 1 calc R . .
H17B H 0.0726 0.6723 0.2303 0.058 Uiso 1 calc R . .
H17C H -0.0343 0.6042 0.2240 0.058 Uiso 1 calc R . .
C18 C 0.48299(17) 0.75460(9) 0.06578(9) 0.0166(3) Uani 1 d . . .
H18A H 0.5858 0.7643 0.0630 0.020 Uiso 1 calc R . .
H18B H 0.4357 0.7862 0.0953 0.020 Uiso 1 calc R . .
C111 C 0.35926(16) 0.62226(10) 0.20240(9) 0.0170(3) Uani 1 d . . .
C112 C 0.38218(17) 0.67228(11) 0.24709(9) 0.0222(3) Uani 1 d . . .
H112 H 0.4338 0.7221 0.2250 0.027 Uiso 1 calc R . .
C113 C 0.32959(18) 0.64921(12) 0.32375(10) 0.0266(4) Uani 1 d . . .
H113 H 0.3451 0.6835 0.3537 0.032 Uiso 1 calc R . .
C114 C 0.25506(18) 0.57687(11) 0.35656(10) 0.0271(4) Uani 1 d . . .
H114 H 0.2199 0.5612 0.4091 0.033 Uiso 1 calc R . .
C115 C 0.23173(19) 0.52714(11) 0.31252(10) 0.0287(4) Uani 1 d . . .
H115 H 0.1807 0.4772 0.3350 0.034 Uiso 1 calc R . .
C116 C 0.28257(18) 0.54999(10) 0.23585(10) 0.0242(3) Uani 1 d . . .
H116 H 0.2649 0.5160 0.2058 0.029 Uiso 1 calc R . .
C121 C 0.60300(16) 0.58787(10) 0.12573(9) 0.0172(3) Uani 1 d . . .
C122 C 0.70693(16) 0.60331(10) 0.06683(9) 0.0202(3) Uani 1 d . . .
H122 H 0.6919 0.6440 0.0169 0.024 Uiso 1 calc R . .
C123 C 0.83206(17) 0.55968(11) 0.08076(10) 0.0230(3) Uani 1 d . . .
H123 H 0.9030 0.5713 0.0406 0.028 Uiso 1 calc R . .
C124 C 0.85429(18) 0.49911(12) 0.15293(11) 0.0297(4) Uani 1 d . . .
H124 H 0.9394 0.4687 0.1620 0.036 Uiso 1 calc R . .
C125 C 0.7521(2) 0.48335(13) 0.21147(12) 0.0374(5) Uani 1 d . . .
H125 H 0.7672 0.4421 0.2611 0.045 Uiso 1 calc R . .
C126 C 0.62700(19) 0.52755(11) 0.19824(10) 0.0293(4) Uani 1 d . . .
H126 H 0.5574 0.5165 0.2390 0.035 Uiso 1 calc R . .
C131 C 0.31150(16) 0.87155(9) -0.05377(9) 0.0165(3) Uani 1 d . . .
C132 C 0.38456(18) 0.94227(10) -0.05738(9) 0.0204(3) Uani 1 d . . .
H132 H 0.4836 0.9403 -0.0512 0.024 Uiso 1 calc R . .
C133 C 0.3129(2) 1.01585(10) -0.07005(10) 0.0263(4) Uani 1 d . . .
H133 H 0.3631 1.0639 -0.0724 0.032 Uiso 1 calc R . .
C134 C 0.1683(2) 1.01918(11) -0.07916(10) 0.0274(4) Uani 1 d . . .
H134 H 0.1195 1.0693 -0.0873 0.033 Uiso 1 calc R . .
C135 C 0.09522(18) 0.94938(11) -0.07635(10) 0.0254(4) Uani 1 d . . .
H135 H -0.0037 0.9520 -0.0831 0.030 Uiso 1 calc R . .
C136 C 0.16575(17) 0.87530(10) -0.06375(9) 0.0202(3) Uani 1 d . . .
H136 H 0.1151 0.8276 -0.0619 0.024 Uiso 1 calc R . .
C141 C 0.54908(16) 0.80261(9) -0.10607(9) 0.0158(3) Uani 1 d . . .
C142 C 0.68763(17) 0.81551(11) -0.09019(10) 0.0244(4) Uani 1 d . . .
H142 H 0.7130 0.8097 -0.0383 0.029 Uiso 1 calc R . .
C143 C 0.78930(18) 0.83700(12) -0.15064(11) 0.0295(4) Uani 1 d . . .
H143 H 0.8840 0.8452 -0.1395 0.035 Uiso 1 calc R . .
C144 C 0.75365(18) 0.84644(11) -0.22644(10) 0.0259(4) Uani 1 d . . .
H144 H 0.8233 0.8615 -0.2674 0.031 Uiso 1 calc R . .
C145 C 0.61551(18) 0.83379(10) -0.24251(10) 0.0226(3) Uani 1 d . . .
H145 H 0.5905 0.8405 -0.2946 0.027 Uiso 1 calc R . .
C146 C 0.51420(16) 0.81143(10) -0.18295(9) 0.0193(3) Uani 1 d . . .
H146 H 0.4202 0.8020 -0.1943 0.023 Uiso 1 calc R . .
Mn2 Mn 0.79715(2) 0.150083(13) 0.494096(13) 0.01372(8) Uani 1 d . . .
P21 P 0.92082(4) 0.14016(2) 0.60527(2) 0.01402(9) Uani 1 d . . .
P22 P 0.90938(4) 0.27406(2) 0.46936(2) 0.01351(9) Uani 1 d . . .
O21 O 1.02543(13) 0.08505(8) 0.41722(7) 0.0272(3) Uani 1 d . . .
O22 O 0.63848(15) 0.20610(9) 0.34651(8) 0.0377(3) Uani 1 d . . .
O23 O 0.65916(13) -0.01343(7) 0.56358(7) 0.0274(3) Uani 1 d . . .
O24 O 0.33350(12) 0.28021(8) 0.58971(7) 0.0276(3) Uani 1 d . . .
O25 O 0.42922(13) 0.18796(8) 0.69612(7) 0.0296(3) Uani 1 d . . .
C21 C 0.93888(17) 0.11031(10) 0.44795(9) 0.0179(3) Uani 1 d . . .
C22 C 0.69948(17) 0.18300(10) 0.40370(10) 0.0218(3) Uani 1 d . . .
C23 C 0.71417(16) 0.04884(10) 0.53556(9) 0.0193(3) Uani 1 d . . .
C24 C 0.64101(16) 0.19043(9) 0.54526(9) 0.0169(3) Uani 1 d . . .
C25 C 0.54187(17) 0.21057(10) 0.57742(9) 0.0202(3) Uani 1 d . . .
C26 C 0.42515(16) 0.23073(10) 0.61868(9) 0.0192(3) Uani 1 d . . .
C27 C 0.3140(2) 0.20343(14) 0.74204(11) 0.0388(5) Uani 1 d . . .
H27A H 0.3304 0.1745 0.7979 0.058 Uiso 1 calc R . .
H27B H 0.2262 0.1836 0.7276 0.058 Uiso 1 calc R . .
H27C H 0.3069 0.2626 0.7319 0.058 Uiso 1 calc R . .
C28 C 0.97401(16) 0.25012(9) 0.57005(8) 0.0158(3) Uani 1 d . . .
H28A H 0.9246 0.2818 0.5989 0.019 Uiso 1 calc R . .
H28B H 1.0770 0.2575 0.5711 0.019 Uiso 1 calc R . .
C211 C 0.83290(16) 0.11874(9) 0.70044(9) 0.0171(3) Uani 1 d . . .
C212 C 0.88275(17) 0.15210(11) 0.75472(10) 0.0237(3) Uani 1 d . . .
H212 H 0.9604 0.1890 0.7410 0.028 Uiso 1 calc R . .
C213 C 0.81933(19) 0.13161(11) 0.82848(10) 0.0266(4) Uani 1 d . . .
H213 H 0.8533 0.1546 0.8651 0.032 Uiso 1 calc R . .
C214 C 0.70653(19) 0.07769(11) 0.84886(10) 0.0273(4) Uani 1 d . . .
H214 H 0.6639 0.0633 0.8997 0.033 Uiso 1 calc R . .
C215 C 0.6554(2) 0.04455(11) 0.79533(10) 0.0304(4) Uani 1 d . . .
H215 H 0.5777 0.0077 0.8094 0.037 Uiso 1 calc R . .
C216 C 0.71831(18) 0.06554(10) 0.72115(10) 0.0255(4) Uani 1 d . . .
H216 H 0.6828 0.0434 0.6843 0.031 Uiso 1 calc R . .
C221 C 1.08362(16) 0.08151(9) 0.63067(9) 0.0172(3) Uani 1 d . . .
C222 C 1.19453(16) 0.09819(10) 0.57570(9) 0.0193(3) Uani 1 d . . .
H222 H 1.1842 0.1395 0.5256 0.023 Uiso 1 calc R . .
C223 C 1.31967(17) 0.05506(10) 0.59351(10) 0.0226(3) Uani 1 d . . .
H223 H 1.3952 0.0675 0.5560 0.027 Uiso 1 calc R . .
C224 C 1.33480(19) -0.00600(12) 0.66570(11) 0.0301(4) Uani 1 d . . .
H224 H 1.4205 -0.0357 0.6778 0.036 Uiso 1 calc R . .
C225 C 1.2252(2) -0.02388(13) 0.72029(11) 0.0390(5) Uani 1 d . . .
H225 H 1.2355 -0.0661 0.7698 0.047 Uiso 1 calc R . .
C226 C 1.0996(2) 0.01965(11) 0.70315(10) 0.0290(4) Uani 1 d . . .
H226 H 1.0246 0.0071 0.7410 0.035 Uiso 1 calc R . .
C231 C 1.05889(16) 0.29815(9) 0.40023(9) 0.0157(3) Uani 1 d . . .
C232 C 1.19791(17) 0.30162(10) 0.42103(10) 0.0211(3) Uani 1 d . . .
H232 H 1.2197 0.2932 0.4740 0.025 Uiso 1 calc R . .
C233 C 1.30529(18) 0.31757(11) 0.36380(11) 0.0270(4) Uani 1 d . . .
H233 H 1.4003 0.3190 0.3782 0.032 Uiso 1 calc R . .
C234 C 1.27452(18) 0.33129(10) 0.28625(10) 0.0264(4) Uani 1 d . . .
H234 H 1.3481 0.3426 0.2476 0.032 Uiso 1 calc R . .
C235 C 1.13567(19) 0.32843(10) 0.26500(10) 0.0242(4) Uani 1 d . . .
H235 H 1.1142 0.3382 0.2118 0.029 Uiso 1 calc R . .
C236 C 1.02886(17) 0.31123(10) 0.32160(9) 0.0203(3) Uani 1 d . . .
H236 H 0.9343 0.3083 0.3071 0.024 Uiso 1 calc R . .
C241 C 0.82083(16) 0.37339(9) 0.44502(9) 0.0165(3) Uani 1 d . . .
C242 C 0.89765(17) 0.44347(10) 0.44047(9) 0.0205(3) Uani 1 d . . .
H242 H 0.9965 0.4399 0.4474 0.025 Uiso 1 calc R . .
C243 C 0.8296(2) 0.51846(10) 0.42587(10) 0.0258(4) Uani 1 d . . .
H243 H 0.8821 0.5658 0.4232 0.031 Uiso 1 calc R . .
C244 C 0.6854(2) 0.52444(11) 0.41522(10) 0.0294(4) Uani 1 d . . .
H244 H 0.6393 0.5756 0.4056 0.035 Uiso 1 calc R . .
C245 C 0.60914(19) 0.45549(11) 0.41871(11) 0.0298(4) Uani 1 d . . .
H245 H 0.5106 0.4597 0.4109 0.036 Uiso 1 calc R . .
C246 C 0.67581(17) 0.38010(10) 0.43354(10) 0.0226(3) Uani 1 d . . .
H246 H 0.6226 0.3331 0.4359 0.027 Uiso 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.01335(13) 0.01496(13) 0.01374(13) -0.00592(10) 0.00049(9) -0.00017(9)
P11 0.01464(19) 0.01480(19) 0.01192(19) -0.00380(15) 0.00036(14) 0.00090(14)
P12 0.01389(19) 0.01436(19) 0.01210(19) -0.00362(15) -0.00044(14) -0.00003(14)
O11 0.0267(6) 0.0324(7) 0.0296(7) -0.0164(6) 0.0071(5) 0.0041(5)
O12 0.0418(8) 0.0437(8) 0.0355(8) -0.0170(6) -0.0219(6) 0.0092(6)
O13 0.0277(6) 0.0206(6) 0.0299(6) -0.0090(5) 0.0077(5) -0.0055(5)
O14 0.0277(6) 0.0334(7) 0.0386(7) -0.0192(6) -0.0135(5) 0.0125(5)
O15 0.0280(7) 0.0498(8) 0.0263(7) -0.0146(6) 0.0056(5) 0.0095(6)
C11 0.0193(8) 0.0182(8) 0.0175(7) -0.0062(6) -0.0014(6) -0.0021(6)
C12 0.0222(8) 0.0215(8) 0.0253(9) -0.0110(7) -0.0018(7) 0.0011(6)
C13 0.0163(7) 0.0236(9) 0.0201(8) -0.0114(7) 0.0015(6) 0.0017(6)
C14 0.0168(7) 0.0146(7) 0.0164(7) -0.0050(6) -0.0019(6) -0.0028(6)
C15 0.0199(8) 0.0187(8) 0.0176(8) -0.0058(6) -0.0004(6) -0.0011(6)
C16 0.0176(8) 0.0250(8) 0.0251(8) -0.0156(7) -0.0020(6) 0.0005(6)
C17 0.0407(11) 0.0455(12) 0.0243(9) -0.0047(8) 0.0063(8) 0.0074(9)
C18 0.0207(8) 0.0153(7) 0.0132(7) -0.0040(6) -0.0013(6) -0.0002(6)
C111 0.0176(7) 0.0192(7) 0.0133(7) -0.0046(6) -0.0004(6) 0.0050(6)
C112 0.0200(8) 0.0291(9) 0.0185(8) -0.0097(7) 0.0002(6) -0.0032(6)
C113 0.0250(9) 0.0397(10) 0.0188(8) -0.0150(7) -0.0009(7) 0.0033(7)
C114 0.0297(9) 0.0335(9) 0.0141(8) -0.0034(7) 0.0035(6) 0.0065(7)
C115 0.0332(9) 0.0234(9) 0.0238(9) -0.0016(7) 0.0081(7) 0.0019(7)
C116 0.0297(9) 0.0201(8) 0.0214(8) -0.0059(7) 0.0040(7) 0.0008(7)
C121 0.0169(7) 0.0186(7) 0.0174(7) -0.0081(6) -0.0015(6) 0.0011(6)
C122 0.0189(8) 0.0219(8) 0.0198(8) -0.0074(6) -0.0013(6) 0.0000(6)
C123 0.0167(8) 0.0290(9) 0.0282(9) -0.0161(7) 0.0015(6) -0.0011(6)
C124 0.0212(8) 0.0325(10) 0.0358(10) -0.0120(8) -0.0053(7) 0.0091(7)
C125 0.0327(10) 0.0380(11) 0.0291(10) 0.0040(8) -0.0017(8) 0.0151(8)
C126 0.0258(9) 0.0324(10) 0.0218(9) 0.0002(7) 0.0027(7) 0.0089(7)
C131 0.0198(8) 0.0164(7) 0.0118(7) -0.0032(6) 0.0008(6) 0.0014(6)
C132 0.0244(8) 0.0185(8) 0.0162(7) -0.0034(6) -0.0001(6) -0.0016(6)
C133 0.0383(10) 0.0171(8) 0.0232(8) -0.0062(7) -0.0026(7) -0.0015(7)
C134 0.0374(10) 0.0201(8) 0.0240(9) -0.0070(7) -0.0005(7) 0.0093(7)
C135 0.0230(8) 0.0251(9) 0.0249(9) -0.0047(7) 0.0004(7) 0.0060(7)
C136 0.0207(8) 0.0185(8) 0.0193(8) -0.0041(6) 0.0001(6) 0.0007(6)
C141 0.0171(7) 0.0139(7) 0.0151(7) -0.0037(6) 0.0019(6) -0.0001(6)
C142 0.0190(8) 0.0324(9) 0.0213(8) -0.0085(7) -0.0009(6) -0.0047(7)
C143 0.0173(8) 0.0389(10) 0.0318(10) -0.0117(8) 0.0023(7) -0.0061(7)
C144 0.0233(8) 0.0264(9) 0.0280(9) -0.0099(7) 0.0090(7) -0.0022(7)
C145 0.0276(9) 0.0229(8) 0.0175(8) -0.0073(6) 0.0028(6) 0.0013(7)
C146 0.0175(7) 0.0217(8) 0.0187(8) -0.0068(6) -0.0018(6) 0.0009(6)
Mn2 0.01272(13) 0.01558(13) 0.01374(13) -0.00627(10) 0.00077(9) -0.00054(9)
P21 0.01478(19) 0.01475(19) 0.01194(19) -0.00392(15) 0.00035(14) 0.00037(14)
P22 0.01259(18) 0.01467(19) 0.01246(19) -0.00367(15) -0.00034(14) -0.00004(14)
O21 0.0250(6) 0.0306(7) 0.0295(7) -0.0155(5) 0.0067(5) 0.0034(5)
O22 0.0394(8) 0.0453(8) 0.0302(7) -0.0145(6) -0.0176(6) 0.0063(6)
O23 0.0303(7) 0.0225(6) 0.0314(7) -0.0123(5) 0.0091(5) -0.0085(5)
O24 0.0229(6) 0.0324(7) 0.0312(7) -0.0155(5) -0.0059(5) 0.0094(5)
O25 0.0260(6) 0.0377(7) 0.0220(6) -0.0069(5) 0.0069(5) 0.0062(5)
C21 0.0197(8) 0.0180(8) 0.0161(7) -0.0057(6) -0.0011(6) -0.0028(6)
C22 0.0201(8) 0.0246(8) 0.0242(9) -0.0128(7) -0.0009(7) -0.0003(6)
C23 0.0175(7) 0.0239(9) 0.0194(8) -0.0115(7) 0.0017(6) 0.0014(6)
C24 0.0173(7) 0.0166(7) 0.0171(7) -0.0060(6) -0.0016(6) -0.0030(6)
C25 0.0210(8) 0.0206(8) 0.0198(8) -0.0079(6) -0.0004(6) -0.0003(6)
C26 0.0172(7) 0.0233(8) 0.0206(8) -0.0119(7) 0.0007(6) -0.0016(6)
C27 0.0295(10) 0.0576(13) 0.0290(10) -0.0158(9) 0.0110(8) 0.0024(9)
C28 0.0184(7) 0.0151(7) 0.0137(7) -0.0048(6) -0.0007(6) -0.0002(6)
C211 0.0190(7) 0.0172(7) 0.0135(7) -0.0034(6) 0.0011(6) 0.0023(6)
C212 0.0210(8) 0.0316(9) 0.0210(8) -0.0125(7) 0.0011(6) -0.0027(7)
C213 0.0294(9) 0.0341(10) 0.0198(8) -0.0139(7) 0.0011(7) 0.0002(7)
C214 0.0351(10) 0.0278(9) 0.0169(8) -0.0057(7) 0.0067(7) 0.0015(7)
C215 0.0350(10) 0.0318(10) 0.0214(8) -0.0056(7) 0.0069(7) -0.0107(8)
C216 0.0308(9) 0.0260(9) 0.0186(8) -0.0067(7) 0.0026(7) -0.0072(7)
C221 0.0184(7) 0.0168(7) 0.0178(7) -0.0077(6) -0.0035(6) 0.0026(6)
C222 0.0193(8) 0.0186(8) 0.0198(8) -0.0063(6) -0.0004(6) -0.0009(6)
C223 0.0187(8) 0.0239(8) 0.0292(9) -0.0142(7) -0.0014(6) 0.0005(6)
C224 0.0278(9) 0.0340(10) 0.0307(9) -0.0138(8) -0.0089(7) 0.0142(8)
C225 0.0454(12) 0.0398(11) 0.0228(9) 0.0004(8) -0.0032(8) 0.0227(9)
C226 0.0324(9) 0.0303(9) 0.0188(8) -0.0021(7) 0.0036(7) 0.0101(8)
C231 0.0162(7) 0.0128(7) 0.0165(7) -0.0031(6) 0.0021(6) -0.0003(5)
C232 0.0189(8) 0.0217(8) 0.0208(8) -0.0050(6) -0.0005(6) -0.0019(6)
C233 0.0159(8) 0.0286(9) 0.0361(10) -0.0110(8) 0.0042(7) -0.0017(7)
C234 0.0267(9) 0.0230(8) 0.0296(9) -0.0099(7) 0.0121(7) -0.0026(7)
C235 0.0312(9) 0.0221(8) 0.0186(8) -0.0065(7) 0.0049(7) -0.0008(7)
C236 0.0197(8) 0.0220(8) 0.0185(8) -0.0062(6) -0.0015(6) 0.0018(6)
C241 0.0187(7) 0.0164(7) 0.0130(7) -0.0036(6) 0.0007(6) 0.0012(6)
C242 0.0234(8) 0.0206(8) 0.0160(7) -0.0046(6) 0.0017(6) -0.0022(6)
C243 0.0412(10) 0.0160(8) 0.0191(8) -0.0046(6) 0.0014(7) -0.0025(7)
C244 0.0417(11) 0.0210(9) 0.0231(9) -0.0048(7) 0.0001(7) 0.0121(8)
C245 0.0261(9) 0.0281(9) 0.0315(9) -0.0056(8) -0.0024(7) 0.0094(7)
C246 0.0203(8) 0.0203(8) 0.0246(8) -0.0044(7) -0.0025(6) 0.0023(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100870.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100870.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100870
loop_
_publ_author_name
'Ruiz, J.'
'Quesada, R.'
'Vivanco, M.'
'Castellano, E. E.'
'Piro, O. E.'
_publ_section_title
;
Stepwise Formation of \s-Alkynyl, Vinylidene, and Vinylphosphonium
Complexes of Manganese(I)
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2542
_journal_page_last 2545
_journal_paper_doi 10.1021/om050146c
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C32 H26 B F4 Mn O5 P2'
_chemical_formula_weight 694.22
_chemical_name_systematic
'fac-[tricarbonyl(2-methoxycarbonylvinyliden(diphenylphosphanylmethyl)diphenylphosphorane)maganese(I)] tetrafluoroborate'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 95.650(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.2407(2)
_cell_length_b 16.6566(4)
_cell_length_c 18.3683(4)
_cell_measurement_reflns_used 22022
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.00
_cell_measurement_theta_min 1.65
_cell_volume 3118.0(1)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD with \f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0685
_diffrn_reflns_av_sigmaI/netI 0.0517
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 22022
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.65
_diffrn_standards_decay_% 0
_exptl_absorpt_coefficient_mu 0.590
_exptl_absorpt_correction_T_max 0.849
_exptl_absorpt_correction_T_min 0.617
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.479
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description fragment
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.20
_refine_ls_extinction_coef 0.0047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 408
_refine_ls_number_reflns 5480
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0472
_refine_ls_R_factor_gt 0.0373
_refine_ls_shift/su_max 0.010
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0945
_refine_ls_wR_factor_ref 0.1010
_reflns_number_gt 4655
_reflns_number_total 5480
_reflns_threshold_expression >2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.0141P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.0141P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M P2~1~/c
_cod_database_code 1100870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.93171(3) 0.181639(19) 0.221905(17) 0.01814(12) Uani 1 d . . .
P1 P 0.85675(5) 0.21032(3) 0.33392(3) 0.01820(15) Uani 1 d . . .
P2 P 0.66605(5) 0.09088(3) 0.26595(3) 0.01868(15) Uani 1 d . . .
B B 0.3918(3) 0.23558(19) 0.39605(16) 0.0302(6) Uani 1 d . . .
F1 F 0.49390(16) 0.22549(12) 0.45046(8) 0.0519(5) Uani 1 d . . .
F2 F 0.43176(17) 0.28708(12) 0.34391(11) 0.0606(5) Uani 1 d . . .
F3 F 0.36634(19) 0.16121(12) 0.36386(12) 0.0662(6) Uani 1 d . . .
F4 F 0.28007(15) 0.26384(12) 0.42347(10) 0.0544(5) Uani 1 d . . .
O1 O 0.72166(17) 0.29027(11) 0.16291(10) 0.0325(4) Uani 1 d . . .
O2 O 1.12908(18) 0.31370(11) 0.22474(11) 0.0368(4) Uani 1 d . . .
O3 O 0.9473(2) 0.14554(13) 0.06452(10) 0.0446(5) Uani 1 d . . .
O4 O 1.08137(14) 0.09876(9) 0.25177(8) 0.0208(3) Uani 1 d . . .
O5 O 1.12072(14) -0.02942(9) 0.28548(8) 0.0228(3) Uani 1 d . . .
C1 C 0.8043(2) 0.24757(14) 0.18727(12) 0.0230(5) Uani 1 d . . .
C2 C 1.0531(2) 0.26297(14) 0.22409(12) 0.0244(5) Uani 1 d . . .
C3 C 0.9470(2) 0.15711(14) 0.12572(13) 0.0262(5) Uani 1 d . . .
C4 C 1.0416(2) 0.03060(13) 0.26513(11) 0.0198(5) Uani 1 d . . .
C5 C 1.2601(2) -0.01051(15) 0.29511(14) 0.0284(5) Uani 1 d . . .
H5A H 1.3095 -0.0581 0.3130 0.043 Uiso 1 calc R . .
H5B H 1.2755 0.0332 0.3307 0.043 Uiso 1 calc R . .
H5C H 1.2891 0.0062 0.2481 0.043 Uiso 1 calc R . .
C6 C 0.9012(2) 0.01577(13) 0.26313(11) 0.0202(5) Uani 1 d . . .
H6 H 0.8644 -0.0345 0.2747 0.024 Uiso 1 calc R . .
C7 C 0.8297(2) 0.08106(13) 0.24312(11) 0.0191(5) Uani 1 d . . .
C8 C 0.6810(2) 0.18078(13) 0.32201(12) 0.0201(5) Uani 1 d . . .
H8A H 0.6491 0.1701 0.3702 0.024 Uiso 1 calc R . .
H8B H 0.6276 0.2246 0.2979 0.024 Uiso 1 calc R . .
C111 C 0.9247(2) 0.15961(14) 0.41680(12) 0.0229(5) Uani 1 d . . .
C112 C 1.0557(2) 0.13675(16) 0.42124(13) 0.0295(5) Uani 1 d . . .
H112 H 1.1044 0.1436 0.3802 0.035 Uiso 1 calc R . .
C113 C 1.1154(3) 0.10396(19) 0.48530(15) 0.0430(7) Uani 1 d . . .
H113 H 1.2054 0.0891 0.4884 0.052 Uiso 1 calc R . .
C114 C 1.0446(3) 0.09278(19) 0.54475(15) 0.0480(8) Uani 1 d . . .
H114 H 1.0853 0.0688 0.5882 0.058 Uiso 1 calc R . .
C115 C 0.9152(3) 0.11625(18) 0.54122(14) 0.0426(7) Uani 1 d . . .
H115 H 0.8674 0.1091 0.5825 0.051 Uiso 1 calc R . .
C116 C 0.8539(3) 0.15029(15) 0.47768(13) 0.0305(6) Uani 1 d . . .
H116 H 0.7649 0.1670 0.4756 0.037 Uiso 1 calc R . .
C121 C 0.8541(2) 0.31486(13) 0.36354(12) 0.0209(5) Uani 1 d . . .
C122 C 0.9758(2) 0.35225(14) 0.37964(12) 0.0236(5) Uani 1 d . . .
H122 H 1.0545 0.3236 0.3743 0.028 Uiso 1 calc R . .
C123 C 0.9811(2) 0.43139(15) 0.40344(12) 0.0269(5) Uani 1 d . . .
H123 H 1.0638 0.4567 0.4146 0.032 Uiso 1 calc R . .
C124 C 0.8667(2) 0.47390(15) 0.41099(13) 0.0297(6) Uani 1 d . . .
H124 H 0.8710 0.5281 0.4270 0.036 Uiso 1 calc R . .
C125 C 0.7465(3) 0.43693(15) 0.39507(14) 0.0315(6) Uani 1 d . . .
H125 H 0.6682 0.4660 0.4003 0.038 Uiso 1 calc R . .
C126 C 0.7392(2) 0.35751(14) 0.37143(13) 0.0277(5) Uani 1 d . . .
H126 H 0.6562 0.3325 0.3607 0.033 Uiso 1 calc R . .
C211 C 0.5556(2) 0.10817(13) 0.18566(12) 0.0213(5) Uani 1 d . . .
C212 C 0.4302(2) 0.13814(14) 0.19287(13) 0.0252(5) Uani 1 d . . .
H212 H 0.4038 0.1490 0.2400 0.030 Uiso 1 calc R . .
C213 C 0.3449(2) 0.15195(15) 0.13128(15) 0.0328(6) Uani 1 d . . .
H213 H 0.2594 0.1722 0.1361 0.039 Uiso 1 calc R . .
C214 C 0.3832(3) 0.13639(17) 0.06245(15) 0.0377(6) Uani 1 d . . .
H214 H 0.3244 0.1464 0.0202 0.045 Uiso 1 calc R . .
C215 C 0.5073(3) 0.10622(18) 0.05518(14) 0.0395(7) Uani 1 d . . .
H215 H 0.5330 0.0953 0.0079 0.047 Uiso 1 calc R . .
C216 C 0.5938(2) 0.09187(16) 0.11638(13) 0.0309(6) Uani 1 d . . .
H216 H 0.6788 0.0710 0.1113 0.037 Uiso 1 calc R . .
C221 C 0.6121(2) 0.00610(14) 0.31530(12) 0.0208(5) Uani 1 d . . .
C222 C 0.5938(2) 0.00841(15) 0.38952(13) 0.0265(5) Uani 1 d . . .
H222 H 0.6013 0.0578 0.4155 0.032 Uiso 1 calc R . .
C223 C 0.5645(2) -0.06166(15) 0.42519(13) 0.0285(5) Uani 1 d . . .
H223 H 0.5513 -0.0600 0.4756 0.034 Uiso 1 calc R . .
C224 C 0.5543(2) -0.13398(15) 0.38811(14) 0.0280(5) Uani 1 d . . .
H224 H 0.5356 -0.1818 0.4132 0.034 Uiso 1 calc R . .
C225 C 0.5715(2) -0.13657(15) 0.31415(14) 0.0270(5) Uani 1 d . . .
H225 H 0.5641 -0.1862 0.2886 0.032 Uiso 1 calc R . .
C226 C 0.5995(2) -0.06695(14) 0.27762(13) 0.0239(5) Uani 1 d . . .
H226 H 0.6101 -0.0687 0.2269 0.029 Uiso 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn 0.0198(2) 0.0142(2) 0.0209(2) 0.00117(13) 0.00428(14) 0.00124(13)
P1 0.0197(3) 0.0143(3) 0.0209(3) -0.0007(2) 0.0038(2) -0.0011(2)
P2 0.0181(3) 0.0155(3) 0.0227(3) -0.0008(2) 0.0032(2) 0.0000(2)
B 0.0285(14) 0.0331(16) 0.0303(14) -0.0094(12) 0.0086(12) -0.0049(12)
F1 0.0426(9) 0.0822(14) 0.0314(8) -0.0029(8) 0.0068(7) 0.0086(9)
F2 0.0403(10) 0.0620(12) 0.0805(13) 0.0357(11) 0.0107(9) 0.0079(9)
F3 0.0628(12) 0.0566(12) 0.0827(14) -0.0410(11) 0.0246(10) -0.0173(10)
F4 0.0296(8) 0.0734(13) 0.0618(11) -0.0362(10) 0.0131(8) -0.0045(8)
O1 0.0301(9) 0.0263(10) 0.0409(10) 0.0061(8) 0.0028(8) 0.0094(8)
O2 0.0353(10) 0.0241(10) 0.0524(12) -0.0002(8) 0.0110(9) -0.0099(8)
O3 0.0644(13) 0.0454(12) 0.0251(10) -0.0026(8) 0.0098(9) 0.0158(10)
O4 0.0208(8) 0.0165(8) 0.0255(8) 0.0011(6) 0.0048(6) -0.0011(6)
O5 0.0205(8) 0.0166(8) 0.0312(8) 0.0032(7) 0.0024(6) 0.0023(6)
C1 0.0255(12) 0.0190(12) 0.0258(11) -0.0014(9) 0.0092(10) -0.0027(10)
C2 0.0266(12) 0.0216(13) 0.0257(12) 0.0005(9) 0.0057(10) 0.0053(10)
C3 0.0297(12) 0.0188(12) 0.0305(13) 0.0018(10) 0.0051(10) 0.0046(10)
C4 0.0234(11) 0.0177(12) 0.0186(10) -0.0019(9) 0.0041(9) 0.0031(9)
C5 0.0182(11) 0.0235(13) 0.0428(14) 0.0035(11) 0.0002(10) 0.0012(9)
C6 0.0223(11) 0.0172(11) 0.0217(11) -0.0004(9) 0.0045(9) -0.0019(9)
C7 0.0209(11) 0.0180(11) 0.0190(10) -0.0023(9) 0.0043(9) -0.0011(9)
C8 0.0198(11) 0.0152(11) 0.0259(11) -0.0010(9) 0.0053(9) 0.0002(8)
C111 0.0285(12) 0.0165(11) 0.0236(11) -0.0007(9) 0.0026(9) -0.0029(9)
C112 0.0293(13) 0.0323(14) 0.0263(12) -0.0028(10) -0.0003(10) 0.0024(11)
C113 0.0396(16) 0.0535(19) 0.0335(14) 0.0008(13) -0.0077(12) 0.0132(14)
C114 0.068(2) 0.0485(19) 0.0254(14) 0.0072(13) -0.0053(14) 0.0143(16)
C115 0.068(2) 0.0359(16) 0.0250(13) 0.0055(12) 0.0109(13) -0.0018(14)
C116 0.0380(14) 0.0278(14) 0.0265(12) -0.0004(10) 0.0081(11) -0.0002(11)
C121 0.0286(12) 0.0162(11) 0.0183(10) -0.0005(9) 0.0048(9) -0.0012(9)
C122 0.0257(12) 0.0227(12) 0.0225(11) -0.0019(9) 0.0028(9) -0.0021(10)
C123 0.0329(13) 0.0239(13) 0.0235(11) -0.0011(10) 0.0002(10) -0.0090(10)
C124 0.0427(15) 0.0180(12) 0.0291(12) -0.0026(10) 0.0075(11) -0.0040(11)
C125 0.0351(14) 0.0201(13) 0.0407(14) -0.0053(11) 0.0109(11) 0.0032(10)
C126 0.0284(13) 0.0192(12) 0.0365(13) -0.0016(10) 0.0078(10) -0.0023(10)
C211 0.0232(11) 0.0156(11) 0.0248(11) 0.0004(9) 0.0015(9) -0.0040(9)
C212 0.0253(12) 0.0180(12) 0.0319(12) -0.0016(10) 0.0015(10) -0.0006(9)
C213 0.0282(13) 0.0220(13) 0.0466(15) 0.0048(11) -0.0050(11) 0.0008(10)
C214 0.0407(15) 0.0302(15) 0.0389(15) 0.0144(12) -0.0124(12) -0.0106(12)
C215 0.0473(17) 0.0461(17) 0.0248(13) 0.0044(12) 0.0021(12) -0.0157(13)
C216 0.0282(13) 0.0354(15) 0.0296(13) -0.0026(11) 0.0050(10) -0.0052(11)
C221 0.0159(10) 0.0197(12) 0.0268(11) 0.0021(9) 0.0018(9) 0.0003(9)
C222 0.0272(12) 0.0243(13) 0.0285(12) -0.0016(10) 0.0054(10) -0.0042(10)
C223 0.0273(12) 0.0313(14) 0.0272(12) 0.0042(10) 0.0041(10) -0.0021(10)
C224 0.0200(11) 0.0261(13) 0.0377(13) 0.0092(11) 0.0017(10) -0.0012(10)
C225 0.0226(12) 0.0184(12) 0.0397(14) 0.0007(10) 0.0023(10) -0.0012(9)
C226 0.0228(11) 0.0199(12) 0.0293(12) -0.0002(10) 0.0036(10) -0.0007(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100871.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100871.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100871
loop_
_publ_author_name
'Jamison, Gregory M.'
'Wheeler, David R.'
'Loy, Douglas A.'
'Ziller, Joseph W.'
_publ_section_title
;
Double Phosphaalkyne Insertion to a Tungsten Alkylidene: 
Formation of a Diphosphametallabicyclobutane
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2245
_journal_page_last 2247
_journal_paper_doi 10.1021/om050150o
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C35 H51 F12 N O2 P2 W'
_chemical_formula_weight 991.56
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 117.670(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 42.110(5)
_cell_length_b 10.6323(9)
_cell_length_c 20.577(2)
_cell_measurement_reflns_used 37
_cell_measurement_temperature 163
_cell_measurement_theta_max 11.70
_cell_measurement_theta_min 5.10
_cell_volume 8159.4(14)
_diffrn_ambient_temperature 163
_diffrn_measurement_device 'Siemens P4'
_diffrn_measurement_method '2\q/\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0201
_diffrn_reflns_av_sigmaI/netI 0.0393
_diffrn_reflns_limit_h_max 45
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 5419
_diffrn_reflns_theta_max 22.50
_diffrn_reflns_theta_min 2.16
_diffrn_standards_decay_% '< 1.0'
_diffrn_standards_interval_count 99
_diffrn_standards_interval_time ?
_diffrn_standards_number 1
_exptl_absorpt_coefficient_mu 2.996
_exptl_absorpt_correction_T_max 0.6052
_exptl_absorpt_correction_T_min 0.4794
_exptl_absorpt_correction_type empirical
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.614
_exptl_crystal_density_meas ?
_exptl_crystal_density_method none
_exptl_crystal_description Prism
_exptl_crystal_F_000 3968
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.17
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.060
_refine_ls_goodness_of_fit_obs 1.085
_refine_ls_hydrogen_treatment ?
_refine_ls_matrix_type full
_refine_ls_number_parameters 478
_refine_ls_number_reflns 5325
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.075
_refine_ls_restrained_S_obs 1.085
_refine_ls_R_factor_all 0.0467
_refine_ls_R_factor_obs 0.0317
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.0714
_refine_ls_wR_factor_obs 0.0650
_reflns_number_observed 4385
_reflns_number_total 5334
_reflns_observed_criterion >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100871
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.02018(14) 0.01523(13) 0.01433(13) -0.00049(12) 0.00685(10) 0.00020(12)
P1 0.0245(9) 0.0219(9) 0.0237(9) 0.0023(7) 0.0102(7) -0.0023(8)
P2 0.0324(10) 0.0205(9) 0.0216(9) 0.0021(7) 0.0134(8) 0.0018(8)
N1 0.023(3) 0.019(3) 0.028(3) 0.003(2) 0.014(2) 0.001(2)
O1 0.024(2) 0.023(3) 0.035(3) -0.002(2) -0.002(2) 0.003(2)
O2 0.020(2) 0.017(2) 0.023(2) -0.001(2) 0.009(2) 0.000(2)
C1 0.029(4) 0.018(3) 0.020(3) -0.001(3) 0.012(3) -0.003(3)
C2 0.034(4) 0.019(3) 0.030(3) 0.006(3) 0.016(3) 0.007(3)
C3 0.043(4) 0.017(3) 0.038(4) -0.003(3) 0.022(3) -0.001(3)
C4 0.036(4) 0.036(5) 0.032(4) 0.009(3) 0.017(3) 0.011(3)
C5 0.053(5) 0.022(4) 0.045(4) 0.013(3) 0.030(4) 0.011(3)
C6 0.040(4) 0.018(4) 0.023(4) 0.001(3) 0.014(3) 0.005(3)
C7 0.040(4) 0.021(4) 0.035(4) 0.000(3) 0.022(3) 0.005(3)
C8 0.034(4) 0.038(4) 0.022(3) 0.002(3) 0.009(3) 0.006(3)
C9 0.073(7) 0.119(9) 0.045(5) 0.015(6) 0.013(5) -0.007(7)
C10 0.046(5) 0.103(8) 0.036(4) -0.013(5) 0.011(4) -0.019(5)
C11 0.060(6) 0.055(6) 0.089(7) -0.036(6) 0.020(5) -0.006(5)
C12 0.028(4) 0.022(4) 0.025(3) 0.000(3) 0.012(3) -0.001(3)
C13 0.046(4) 0.034(4) 0.037(4) 0.010(3) 0.024(3) 0.003(4)
C14 0.040(4) 0.029(4) 0.031(4) -0.004(3) 0.014(3) -0.010(3)
C15 0.029(4) 0.039(4) 0.033(4) 0.003(3) 0.016(3) 0.000(3)
C16 0.030(4) 0.017(3) 0.015(3) -0.001(3) 0.012(3) 0.001(3)
C17 0.027(4) 0.021(4) 0.027(3) 0.007(3) 0.016(3) 0.005(3)
C18 0.039(4) 0.024(4) 0.035(4) 0.001(3) 0.025(3) 0.002(3)
C19 0.048(5) 0.031(4) 0.026(4) -0.008(3) 0.021(4) -0.001(4)
C20 0.034(4) 0.031(4) 0.027(4) 0.001(3) 0.011(3) -0.001(3)
C21 0.030(4) 0.019(3) 0.019(3) -0.002(3) 0.010(3) -0.002(3)
C22 0.021(3) 0.034(4) 0.026(3) 0.003(3) 0.011(3) 0.008(3)
C23 0.029(4) 0.041(4) 0.042(4) 0.005(4) 0.017(3) 0.005(3)
C24 0.035(4) 0.027(4) 0.053(4) 0.000(4) 0.019(3) -0.003(4)
C25 0.028(4) 0.046(5) 0.018(3) -0.005(3) 0.007(3) -0.003(3)
C26 0.041(5) 0.069(6) 0.056(5) -0.017(5) 0.025(4) -0.010(4)
C27 0.046(5) 0.077(6) 0.031(4) 0.010(4) 0.011(4) 0.021(4)
C28 0.026(4) 0.024(4) 0.029(4) -0.010(3) 0.008(3) -0.006(3)
C29 0.037(4) 0.042(5) 0.035(4) -0.002(4) 0.007(4) -0.008(4)
C30 0.040(5) 0.030(4) 0.065(5) 0.004(4) 0.022(4) -0.003(4)
C31 0.063(5) 0.080(7) 0.045(5) -0.023(5) 0.024(4) 0.003(5)
C32 0.021(3) 0.020(3) 0.025(3) -0.002(3) 0.009(3) 0.004(3)
C33 0.049(5) 0.023(4) 0.041(4) 0.004(4) 0.015(4) 0.006(4)
C34 0.032(4) 0.033(4) 0.037(4) -0.001(4) 0.020(3) 0.005(4)
C35 0.035(4) 0.032(4) 0.034(4) -0.004(3) 0.011(3) 0.005(3)
F1 0.044(3) 0.072(4) 0.067(3) 0.001(3) 0.021(2) 0.023(2)
F2 0.033(2) 0.053(3) 0.079(3) -0.009(3) -0.004(2) -0.016(2)
F3 0.045(3) 0.057(3) 0.055(3) 0.021(3) -0.004(2) 0.002(2)
F4 0.057(3) 0.043(3) 0.172(6) 0.022(4) 0.015(4) -0.026(3)
F5 0.043(3) 0.031(2) 0.077(3) 0.016(2) 0.021(2) 0.009(2)
F6 0.114(4) 0.114(5) 0.108(4) 0.069(4) 0.091(4) 0.054(4)
F7 0.110(4) 0.050(3) 0.039(3) 0.016(2) 0.039(3) 0.020(3)
F8 0.056(3) 0.038(3) 0.078(3) 0.021(2) 0.020(3) -0.008(2)
F9 0.056(3) 0.043(3) 0.068(3) 0.029(2) 0.017(2) 0.028(2)
F10 0.055(3) 0.045(3) 0.064(3) -0.012(2) 0.031(2) 0.016(2)
F11 0.100(4) 0.051(3) 0.042(2) 0.001(2) 0.048(3) 0.016(3)
F12 0.040(3) 0.068(3) 0.054(3) -0.039(2) 0.018(2) -0.012(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.626961(6) 0.39317(2) -0.225787(12) 0.01704(9) Uani 1 d . .
P1 P 0.57991(4) 0.2435(2) -0.23887(9) 0.0237(4) Uani 1 d . .
P2 P 0.60800(4) 0.2972(2) -0.12310(8) 0.0245(4) Uani 1 d . .
N1 N 0.63148(12) 0.3427(5) -0.3007(3) 0.0228(12) Uani 1 d . .
O1 O 0.67039(11) 0.4656(4) -0.1530(2) 0.0336(11) Uani 1 d . .
O2 O 0.59600(10) 0.5366(4) -0.2549(2) 0.0206(9) Uani 1 d . .
C1 C 0.6278(2) 0.2171(6) -0.1770(3) 0.0221(14) Uani 1 d . .
C2 C 0.6501(2) 0.0997(6) -0.1668(3) 0.0269(14) Uani 1 d . .
C3 C 0.6407(2) 0.0437(6) -0.2425(3) 0.031(2) Uani 1 d . .
H3A H 0.6551(2) -0.0322(6) -0.2362(3) 0.047 Uiso 1 calc R .
H3B H 0.6460(2) 0.1056(6) -0.2715(3) 0.047 Uiso 1 calc R .
H3C H 0.6152(2) 0.0221(6) -0.2680(3) 0.047 Uiso 1 calc R .
C4 C 0.6899(2) 0.1316(6) -0.1274(3) 0.034(2) Uani 1 d . .
H4A H 0.7039(2) 0.0550(6) -0.1212(3) 0.051 Uiso 1 calc R .
H4B H 0.6960(2) 0.1676(6) -0.0792(3) 0.051 Uiso 1 calc R .
H4C H 0.6953(2) 0.1928(6) -0.1565(3) 0.051 Uiso 1 calc R .
C5 C 0.6421(2) 0.0007(6) -0.1227(4) 0.037(2) Uani 1 d . .
H5A H 0.6568(2) -0.0742(6) -0.1168(4) 0.056 Uiso 1 calc R .
H5B H 0.6167(2) -0.0222(6) -0.1486(4) 0.056 Uiso 1 calc R .
H5C H 0.6477(2) 0.0348(6) -0.0743(4) 0.056 Uiso 1 calc R .
C6 C 0.5946(2) 0.1970(6) -0.0655(3) 0.027(2) Uani 1 d . .
C7 C 0.6156(2) 0.1960(6) 0.0057(3) 0.030(2) Uani 1 d . .
H7A H 0.6060(2) 0.1465(6) 0.0309(3) 0.036 Uiso 1 calc R .
C8 C 0.6512(2) 0.2542(7) 0.0574(3) 0.033(2) Uani 1 d . .
C9 C 0.6654(2) 0.1845(11) 0.1305(4) 0.085(3) Uani 1 d . .
H9A H 0.6473(2) 0.1865(11) 0.1478(4) 0.127 Uiso 1 calc R .
H9B H 0.6874(2) 0.2253(11) 0.1667(4) 0.127 Uiso 1 calc R .
H9C H 0.6706(2) 0.0970(11) 0.1238(4) 0.127 Uiso 1 calc R .
C10 C 0.6799(2) 0.2484(9) 0.0334(4) 0.064(3) Uani 1 d . .
H10A H 0.7018(2) 0.2885(9) 0.0705(4) 0.096 Uiso 1 calc R .
H10B H 0.6717(2) 0.2926(9) -0.0135(4) 0.096 Uiso 1 calc R .
H10C H 0.6849(2) 0.1603(9) 0.0274(4) 0.096 Uiso 1 calc R .
C11 C 0.6441(2) 0.3898(8) 0.0691(5) 0.074(3) Uani 1 d . .
H11A H 0.6254(2) 0.3931(8) 0.0847(5) 0.111 Uiso 1 calc R .
H11B H 0.6361(2) 0.4365(8) 0.0231(5) 0.111 Uiso 1 calc R .
H11C H 0.6662(2) 0.4277(8) 0.1070(5) 0.111 Uiso 1 calc R .
C12 C 0.5557(2) 0.1419(6) -0.0983(3) 0.0249(15) Uani 1 d . .
C13 C 0.5463(2) 0.0919(7) -0.0393(3) 0.037(2) Uani 1 d . .
H13A H 0.5629(2) 0.0244(7) -0.0116(3) 0.055 Uiso 1 calc R .
H13B H 0.5217(2) 0.0590(7) -0.0629(3) 0.055 Uiso 1 calc R .
H13C H 0.5481(2) 0.1603(7) -0.0058(3) 0.055 Uiso 1 calc R .
C14 C 0.5503(2) 0.0313(6) -0.1505(3) 0.035(2) Uani 1 d . .
H14A H 0.5678(2) -0.0350(6) -0.1241(3) 0.052 Uiso 1 calc R .
H14B H 0.5538(2) 0.0604(6) -0.1919(3) 0.052 Uiso 1 calc R .
H14C H 0.5260(2) -0.0022(6) -0.1687(3) 0.052 Uiso 1 calc R .
C15 C 0.5286(2) 0.2461(6) -0.1387(3) 0.033(2) Uani 1 d . .
H15A H 0.5335(2) 0.2813(6) -0.1772(3) 0.049 Uiso 1 calc R .
H15B H 0.5307(2) 0.3125(6) -0.1039(3) 0.049 Uiso 1 calc R .
H15C H 0.5043(2) 0.2112(6) -0.1610(3) 0.049 Uiso 1 calc R .
C16 C 0.6338(2) 0.3034(5) -0.3643(3) 0.0201(14) Uani 1 d . .
C17 C 0.6667(2) 0.2655(6) -0.3585(3) 0.0234(15) Uani 1 d . .
C18 C 0.6670(2) 0.2162(6) -0.4209(3) 0.030(2) Uani 1 d . .
H18A H 0.6890(2) 0.1894(6) -0.4186(3) 0.035 Uiso 1 calc R .
C19 C 0.6356(2) 0.2055(6) -0.4863(3) 0.033(2) Uani 1 d . .
H19A H 0.6360(2) 0.1692(6) -0.5280(3) 0.040 Uiso 1 calc R .
C20 C 0.6041(2) 0.2473(6) -0.4905(3) 0.032(2) Uani 1 d . .
H20A H 0.5830(2) 0.2416(6) -0.5362(3) 0.038 Uiso 1 calc R .
C21 C 0.6016(2) 0.2977(6) -0.4310(3) 0.0231(14) Uani 1 d . .
C22 C 0.7020(2) 0.2794(6) -0.2885(3) 0.027(2) Uani 1 d . .
H22A H 0.6962(2) 0.3068(6) -0.2487(3) 0.032 Uiso 1 calc R .
C23 C 0.7223(2) 0.1558(6) -0.2646(4) 0.037(2) Uani 1 d . .
H23A H 0.7068(2) 0.0918(6) -0.2596(4) 0.056 Uiso 1 calc R .
H23B H 0.7437(2) 0.1673(6) -0.2173(4) 0.056 Uiso 1 calc R .
H23C H 0.7294(2) 0.1285(6) -0.3015(4) 0.056 Uiso 1 calc R .
C24 C 0.7252(2) 0.3800(6) -0.2967(4) 0.039(2) Uani 1 d . .
H24A H 0.7117(2) 0.4589(6) -0.3121(4) 0.059 Uiso 1 calc R .
H24B H 0.7323(2) 0.3539(6) -0.3337(4) 0.059 Uiso 1 calc R .
H24C H 0.7466(2) 0.3926(6) -0.2495(4) 0.059 Uiso 1 calc R .
C25 C 0.5664(2) 0.3454(7) -0.4389(3) 0.032(2) Uani 1 d . .
H25A H 0.5713(2) 0.3932(7) -0.3933(3) 0.038 Uiso 1 calc R .
C26 C 0.5414(2) 0.2363(8) -0.4455(4) 0.054(2) Uani 1 d . .
H26A H 0.5186(2) 0.2696(8) -0.4506(4) 0.082 Uiso 1 calc R .
H26B H 0.5526(2) 0.1837(8) -0.4014(4) 0.082 Uiso 1 calc R .
H26C H 0.5369(2) 0.1856(8) -0.4888(4) 0.082 Uiso 1 calc R .
C27 C 0.5480(2) 0.4349(8) -0.5040(4) 0.054(2) Uani 1 d . .
H27A H 0.5252(2) 0.4636(8) -0.5070(4) 0.081 Uiso 1 calc R .
H27B H 0.5434(2) 0.3911(8) -0.5494(4) 0.081 Uiso 1 calc R .
H27C H 0.5635(2) 0.5076(8) -0.4972(4) 0.081 Uiso 1 calc R .
C28 C 0.6956(2) 0.5498(6) -0.1080(3) 0.028(2) Uani 1 d . .
C29 C 0.7320(2) 0.4828(7) -0.0729(4) 0.042(2) Uani 1 d . .
C30 C 0.6958(2) 0.6589(7) -0.1562(4) 0.045(2) Uani 1 d . .
C31 C 0.6869(2) 0.5998(9) -0.0489(4) 0.063(2) Uani 1 d . .
H31A H 0.6868(2) 0.5300(9) -0.0178(4) 0.094 Uiso 1 calc R .
H31B H 0.6632(2) 0.6397(9) -0.0720(4) 0.094 Uiso 1 calc R .
H31C H 0.7050(2) 0.6617(9) -0.0188(4) 0.094 Uiso 1 calc R .
C32 C 0.56384(15) 0.5989(6) -0.2732(3) 0.0228(14) Uani 1 d . .
C33 C 0.5608(2) 0.7018(7) -0.3287(4) 0.040(2) Uani 1 d . .
C34 C 0.5667(2) 0.6590(7) -0.2030(4) 0.032(2) Uani 1 d . .
C35 C 0.5310(2) 0.5152(6) -0.3071(4) 0.036(2) Uani 1 d . .
H35A H 0.5292(2) 0.4767(6) -0.3520(4) 0.054 Uiso 1 calc R .
H35B H 0.5095(2) 0.5656(6) -0.3190(4) 0.054 Uiso 1 calc R .
H35C H 0.5331(2) 0.4490(6) -0.2721(4) 0.054 Uiso 1 calc R .
F1 F 0.73995(11) 0.4316(5) -0.1221(2) 0.0626(13) Uani 1 d . .
F2 F 0.75844(11) 0.5604(4) -0.0321(3) 0.0670(14) Uani 1 d . .
F3 F 0.73181(11) 0.3914(5) -0.0294(2) 0.0633(13) Uani 1 d . .
F4 F 0.71911(14) 0.7472(5) -0.1180(4) 0.106(2) Uani 1 d . .
F5 F 0.66368(11) 0.7128(4) -0.1892(2) 0.0527(12) Uani 1 d . .
F6 F 0.7035(2) 0.6214(6) -0.2079(3) 0.096(2) Uani 1 d . .
F7 F 0.55970(14) 0.6502(4) -0.3878(2) 0.0647(14) Uani 1 d . .
F8 F 0.58844(12) 0.7803(4) -0.3018(3) 0.0620(13) Uani 1 d . .
F9 F 0.53139(12) 0.7710(4) -0.3498(2) 0.0608(13) Uani 1 d . .
F10 F 0.53921(11) 0.7328(4) -0.2148(2) 0.0533(12) Uani 1 d . .
F11 F 0.56757(13) 0.5711(4) -0.1565(2) 0.0589(13) Uani 1 d . .
F12 F 0.59603(11) 0.7281(4) -0.1676(2) 0.0558(12) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100872.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100872.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100872
loop_
_publ_author_name
'Wang, Jun'
'Amos, Ruth I. J.'
'Frey, Alistair S. P.'
'Gardiner, Michael G.'
'Cole, Marcus L.'
'Junk, Peter C.'
_publ_section_title
;
Reversible Sm(III)/Sm(II) Redox Chemistry of an Organosamarium(III)
Complex
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2259
_journal_page_last 2261
_journal_paper_doi 10.1021/om050172a
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C92 H134 N10 Sm2'
_chemical_formula_weight 1680.79
_space_group_IT_number 2
_symmetry_cell_setting ?
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 113.7890(10)
_cell_angle_beta 93.1120(10)
_cell_angle_gamma 95.3020(10)
_cell_formula_units_Z 2
_cell_length_a 14.6994(4)
_cell_length_b 17.0733(5)
_cell_length_c 18.7037(6)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 4255.2(2)
_diffrn_ambient_temperature 123(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0761
_diffrn_reflns_av_sigmaI/netI 0.0875
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 50584
_diffrn_reflns_theta_max 27.63
_diffrn_reflns_theta_min 2.57
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.417
_exptl_absorpt_correction_T_max 0.7648
_exptl_absorpt_correction_T_min 0.7648
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details none
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.312
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 1760
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 934
_refine_ls_number_reflns 19363
_refine_ls_number_restraints 9
_refine_ls_restrained_S_all 1.015
_refine_ls_R_factor_all 0.0821
_refine_ls_R_factor_gt 0.0436
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.8935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0935
_refine_ls_wR_factor_ref 0.1075
_reflns_number_gt 13492
_reflns_number_total 19363
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100872
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.203692(13) 1.275778(12) 0.442472(11) 0.01341(6) Uani 1 1 d . . .
Sm2 Sm 0.311827(13) 0.877359(12) 0.138658(11) 0.01356(6) Uani 1 1 d . . .
N1 N 0.0512(2) 1.2444(2) 0.36352(18) 0.0176(7) Uani 1 1 d . . .
N2 N 0.1764(2) 1.4365(2) 0.43249(18) 0.0171(7) Uani 1 1 d . . .
N3 N 0.2331(2) 1.3924(2) 0.58163(18) 0.0175(7) Uani 1 1 d . . .
N4 N 0.0761(2) 1.2266(2) 0.53020(18) 0.0170(7) Uani 1 1 d . . .
N5 N 0.2595(2) 0.7451(2) 0.01185(18) 0.0193(8) Uani 1 1 d . . .
N6 N 0.4734(2) 0.8368(2) 0.06315(18) 0.0190(8) Uani 1 1 d . . .
N7 N 0.4297(2) 0.8781(2) 0.24193(18) 0.0161(7) Uani 1 1 d . . .
N8 N 0.2366(2) 0.7474(2) 0.18290(18) 0.0172(7) Uani 1 1 d . . .
N9 N 0.3059(2) 1.18983(19) 0.37705(17) 0.0150(7) Uani 1 1 d . . .
N10 N 0.2546(2) 1.0030(2) 0.17046(18) 0.0162(7) Uani 1 1 d . . .
C1 C -0.0269(3) 1.1980(3) 0.3737(2) 0.0184(9) Uani 1 1 d . . .
C2 C -0.1052(3) 1.2270(3) 0.3549(2) 0.0245(10) Uani 1 1 d . . .
H2 H -0.1666 1.2066 0.3581 0.029 Uiso 1 1 calc R . .
C3 C -0.0779(3) 1.2920(3) 0.3300(2) 0.0267(10) Uani 1 1 d . . .
H3 H -0.1168 1.3240 0.3132 0.032 Uiso 1 1 calc R . .
C4 C 0.0172(3) 1.3003(3) 0.3348(2) 0.0195(9) Uani 1 1 d . . .
C5 C 0.0804(3) 1.3490(3) 0.3016(2) 0.0201(9) Uani 1 1 d . . .
C6 C 0.1001(3) 1.2852(3) 0.2182(2) 0.0230(9) Uani 1 1 d . . .
H6A H 0.1362 1.3182 0.1939 0.028 Uiso 1 1 calc R . .
H6B H 0.1385 1.2431 0.2241 0.028 Uiso 1 1 calc R . .
C7 C 0.0140(3) 1.2354(3) 0.1621(3) 0.0304(11) Uani 1 1 d . . .
H7A H -0.0203 1.1995 0.1837 0.046 Uiso 1 1 calc R . .
H7B H 0.0324 1.1987 0.1108 0.046 Uiso 1 1 calc R . .
H7C H -0.0249 1.2764 0.1560 0.046 Uiso 1 1 calc R . .
C8 C 0.0363(3) 1.4252(3) 0.2941(2) 0.0246(10) Uani 1 1 d . . .
H8A H -0.0148 1.4011 0.2516 0.030 Uiso 1 1 calc R . .
H8B H 0.0098 1.4572 0.3437 0.030 Uiso 1 1 calc R . .
C9 C 0.1015(3) 1.4886(3) 0.2770(3) 0.0361(12) Uani 1 1 d . . .
H9A H 0.1492 1.5174 0.3211 0.054 Uiso 1 1 calc R . .
H9B H 0.0672 1.5318 0.2697 0.054 Uiso 1 1 calc R . .
H9C H 0.1302 1.4575 0.2291 0.054 Uiso 1 1 calc R . .
C10 C 0.1701(3) 1.3796(2) 0.3531(2) 0.0165(8) Uani 1 1 d . . .
C11 C 0.0993(3) 1.4764(3) 0.4737(2) 0.0235(10) Uani 1 1 d . . .
H11A H 0.0951 1.5314 0.4695 0.035 Uiso 1 1 calc R . .
H11B H 0.1093 1.4866 0.5291 0.035 Uiso 1 1 calc R . .
H11C H 0.0421 1.4378 0.4498 0.035 Uiso 1 1 calc R . .
C12 C 0.2680(3) 1.4543(2) 0.4648(2) 0.0188(9) Uani 1 1 d . . .
C13 C 0.3176(3) 1.4059(2) 0.4063(2) 0.0178(9) Uani 1 1 d . . .
H13 H 0.3819 1.4040 0.4113 0.021 Uiso 1 1 calc R . .
C14 C 0.2574(3) 1.3596(2) 0.3372(2) 0.0194(9) Uani 1 1 d . . .
H14 H 0.2744 1.3212 0.2882 0.023 Uiso 1 1 calc R . .
C15 C 0.2965(3) 1.5143(2) 0.5490(2) 0.0178(9) Uani 1 1 d . . .
C16 C 0.4021(3) 1.5151(3) 0.5667(2) 0.0217(9) Uani 1 1 d . . .
H16A H 0.4162 1.4548 0.5454 0.026 Uiso 1 1 calc R . .
H16B H 0.4356 1.5449 0.5385 0.026 Uiso 1 1 calc R . .
C17 C 0.4379(3) 1.5585(3) 0.6533(2) 0.0306(11) Uani 1 1 d . . .
H17A H 0.4311 1.6201 0.6737 0.046 Uiso 1 1 calc R . .
H17B H 0.5029 1.5516 0.6595 0.046 Uiso 1 1 calc R . .
H17C H 0.4027 1.5319 0.6826 0.046 Uiso 1 1 calc R . .
C18 C 0.2772(3) 1.6078(2) 0.5654(2) 0.0226(9) Uani 1 1 d . . .
H18A H 0.2106 1.6108 0.5691 0.027 Uiso 1 1 calc R . .
H18B H 0.3096 1.6476 0.6170 0.027 Uiso 1 1 calc R . .
C19 C 0.3064(3) 1.6390(3) 0.5040(3) 0.0319(11) Uani 1 1 d . . .
H19A H 0.3719 1.6347 0.4986 0.048 Uiso 1 1 calc R . .
H19B H 0.2954 1.6992 0.5201 0.048 Uiso 1 1 calc R . .
H19C H 0.2707 1.6033 0.4535 0.048 Uiso 1 1 calc R . .
C20 C 0.2468(3) 1.4803(2) 0.6007(2) 0.0175(9) Uani 1 1 d . . .
C21 C 0.2183(3) 1.5261(3) 0.6735(2) 0.0208(9) Uani 1 1 d . . .
H21 H 0.2193 1.5869 0.6986 0.025 Uiso 1 1 calc R . .
C22 C 0.1876(3) 1.4662(2) 0.7033(2) 0.0211(9) Uani 1 1 d . . .
H22 H 0.1638 1.4785 0.7524 0.025 Uiso 1 1 calc R . .
C23 C 0.1986(3) 1.3860(2) 0.6475(2) 0.0179(9) Uani 1 1 d . . .
C24 C 0.1888(3) 1.3002(2) 0.6538(2) 0.0207(9) Uani 1 1 d . . .
C25 C 0.2841(3) 1.2844(3) 0.6807(2) 0.0271(10) Uani 1 1 d . . .
H25A H 0.2788 1.2254 0.6791 0.032 Uiso 1 1 calc R . .
H25B H 0.3272 1.2863 0.6423 0.032 Uiso 1 1 calc R . .
C26 C 0.3260(4) 1.3479(3) 0.7628(3) 0.0451(14) Uani 1 1 d . . .
H26A H 0.3246 1.4071 0.7676 0.068 Uiso 1 1 calc R . .
H26B H 0.3897 1.3383 0.7709 0.068 Uiso 1 1 calc R . .
H26C H 0.2906 1.3390 0.8023 0.068 Uiso 1 1 calc R . .
C27 C 0.1199(3) 1.2986(3) 0.7130(2) 0.0292(11) Uani 1 1 d . . .
H27A H 0.1446 1.3421 0.7659 0.035 Uiso 1 1 calc R . .
H27B H 0.0616 1.3159 0.6986 0.035 Uiso 1 1 calc R . .
C28 C 0.0993(5) 1.2115(3) 0.7172(3) 0.0573(18) Uani 1 1 d . . .
H28A H 0.0754 1.1676 0.6651 0.086 Uiso 1 1 calc R . .
H28B H 0.0534 1.2154 0.7542 0.086 Uiso 1 1 calc R . .
H28C H 0.1557 1.1955 0.7351 0.086 Uiso 1 1 calc R . .
C29 C 0.1586(3) 1.2306(2) 0.5728(2) 0.0173(9) Uani 1 1 d . . .
C30 C 0.0090(3) 1.2896(3) 0.5566(2) 0.0231(10) Uani 1 1 d . . .
H30A H -0.0241 1.2921 0.5108 0.035 Uiso 1 1 calc R . .
H30B H 0.0415 1.3468 0.5901 0.035 Uiso 1 1 calc R . .
H30C H -0.0348 1.2717 0.5865 0.035 Uiso 1 1 calc R . .
C31 C 0.0657(3) 1.1531(2) 0.4591(2) 0.0168(8) Uani 1 1 d . . .
C32 C 0.1452(3) 1.1147(2) 0.4562(2) 0.0171(9) Uani 1 1 d . . .
H32 H 0.1589 1.0646 0.4139 0.021 Uiso 1 1 calc R . .
C33 C 0.2026(3) 1.1626(2) 0.5267(2) 0.0174(9) Uani 1 1 d . . .
H33 H 0.2612 1.1501 0.5400 0.021 Uiso 1 1 calc R . .
C34 C -0.0179(3) 1.1269(2) 0.4011(2) 0.0178(9) Uani 1 1 d . . .
C35 C -0.0017(3) 1.0428(3) 0.3305(2) 0.0207(9) Uani 1 1 d . . .
H35A H 0.0545 1.0550 0.3079 0.025 Uiso 1 1 calc R . .
H35B H 0.0097 0.9986 0.3504 0.025 Uiso 1 1 calc R . .
C36 C -0.0803(3) 1.0056(3) 0.2654(2) 0.0281(10) Uani 1 1 d . . .
H36A H -0.1349 0.9882 0.2858 0.042 Uiso 1 1 calc R . .
H36B H -0.0629 0.9552 0.2222 0.042 Uiso 1 1 calc R . .
H36C H -0.0936 1.0493 0.2463 0.042 Uiso 1 1 calc R . .
C37 C -0.1056(3) 1.1103(3) 0.4366(2) 0.0207(9) Uani 1 1 d . . .
H37A H -0.1176 1.1654 0.4784 0.025 Uiso 1 1 calc R . .
H37B H -0.1578 1.0909 0.3953 0.025 Uiso 1 1 calc R . .
C38 C -0.1023(3) 1.0435(3) 0.4711(3) 0.0327(11) Uani 1 1 d . . .
H38A H -0.0877 0.9893 0.4310 0.049 Uiso 1 1 calc R . .
H38B H -0.1622 1.0336 0.4888 0.049 Uiso 1 1 calc R . .
H38C H -0.0550 1.0646 0.5159 0.049 Uiso 1 1 calc R . .
C39 C 0.1978(3) 0.6740(3) 0.0033(2) 0.0218(10) Uani 1 1 d . . .
C40 C 0.2118(3) 0.6025(3) -0.0614(2) 0.0288(11) Uani 1 1 d . . .
H40 H 0.1798 0.5461 -0.0785 0.035 Uiso 1 1 calc R . .
C41 C 0.2830(3) 0.6287(3) -0.0979(2) 0.0281(11) Uani 1 1 d . . .
H41 H 0.3073 0.5936 -0.1447 0.034 Uiso 1 1 calc R . .
C42 C 0.3103(3) 0.7143(3) -0.0530(2) 0.0217(9) Uani 1 1 d . . .
C43 C 0.3772(3) 0.7750(3) -0.0708(2) 0.0226(10) Uani 1 1 d . . .
C44 C 0.3249(3) 0.8185(3) -0.1168(2) 0.0267(10) Uani 1 1 d . . .
H44A H 0.2772 0.8489 -0.0848 0.032 Uiso 1 1 calc R . .
H44B H 0.3688 0.8627 -0.1227 0.032 Uiso 1 1 calc R . .
C45 C 0.2793(4) 0.7580(3) -0.1976(3) 0.0420(13) Uani 1 1 d . . .
H45A H 0.3265 0.7345 -0.2326 0.063 Uiso 1 1 calc R . .
H45B H 0.2418 0.7897 -0.2188 0.063 Uiso 1 1 calc R . .
H45C H 0.2401 0.7106 -0.1935 0.063 Uiso 1 1 calc R . .
C46 C 0.4516(3) 0.7255(3) -0.1193(2) 0.0280(11) Uani 1 1 d . . .
H46A H 0.4820 0.6966 -0.0899 0.034 Uiso 1 1 calc R . .
H46B H 0.4212 0.6800 -0.1692 0.034 Uiso 1 1 calc R . .
C47 C 0.5249(4) 0.7811(3) -0.1384(3) 0.0445(15) Uani 1 1 d . . .
H47A H 0.4963 0.8069 -0.1708 0.067 Uiso 1 1 calc R . .
H47B H 0.5704 0.7453 -0.1672 0.067 Uiso 1 1 calc R . .
H47C H 0.5552 0.8269 -0.0895 0.067 Uiso 1 1 calc R . .
C48 C 0.4196(3) 0.8482(3) 0.0053(2) 0.0193(9) Uani 1 1 d . . .
C49 C 0.4974(3) 0.7539(3) 0.0602(2) 0.0254(10) Uani 1 1 d . . .
H49A H 0.4476 0.7081 0.0301 0.038 Uiso 1 1 calc R . .
H49B H 0.5067 0.7573 0.1137 0.038 Uiso 1 1 calc R . .
H49C H 0.5541 0.7412 0.0347 0.038 Uiso 1 1 calc R . .
C50 C 0.5044(3) 0.9186(2) 0.1243(2) 0.0176(9) Uani 1 1 d . . .
C51 C 0.4651(3) 0.9780(3) 0.1053(2) 0.0175(9) Uani 1 1 d . . .
H51 H 0.4716 1.0384 0.1366 0.021 Uiso 1 1 calc R . .
C52 C 0.4131(3) 0.9348(3) 0.0315(2) 0.0188(9) Uani 1 1 d . . .
H52 H 0.3795 0.9613 0.0045 0.023 Uiso 1 1 calc R . .
C53 C 0.5695(3) 0.9312(3) 0.1941(2) 0.0205(9) Uani 1 1 d . . .
C54 C 0.5856(3) 1.0304(3) 0.2455(2) 0.0223(10) Uani 1 1 d . . .
H54A H 0.6086 1.0597 0.2127 0.027 Uiso 1 1 calc R . .
H54B H 0.5257 1.0502 0.2616 0.027 Uiso 1 1 calc R . .
C55 C 0.6531(3) 1.0589(3) 0.3195(2) 0.0341(12) Uani 1 1 d . . .
H55A H 0.6346 1.0261 0.3500 0.051 Uiso 1 1 calc R . .
H55B H 0.6527 1.1206 0.3514 0.051 Uiso 1 1 calc R . .
H55C H 0.7150 1.0482 0.3043 0.051 Uiso 1 1 calc R . .
C56 C 0.6621(3) 0.8985(3) 0.1682(2) 0.0272(10) Uani 1 1 d . . .
H56A H 0.7048 0.9127 0.2157 0.033 Uiso 1 1 calc R . .
H56B H 0.6518 0.8349 0.1399 0.033 Uiso 1 1 calc R . .
C57 C 0.7077(3) 0.9359(4) 0.1156(3) 0.0428(13) Uani 1 1 d . . .
H57A H 0.6652 0.9242 0.0692 0.064 Uiso 1 1 calc R . .
H57B H 0.7635 0.9091 0.0990 0.064 Uiso 1 1 calc R . .
H57C H 0.7238 0.9983 0.1447 0.064 Uiso 1 1 calc R . .
C58 C 0.5249(3) 0.8868(3) 0.2406(2) 0.0195(9) Uani 1 1 d . . .
C59 C 0.5650(3) 0.8557(3) 0.2891(3) 0.0318(11) Uani 1 1 d . . .
H59 H 0.6289 0.8539 0.2973 0.038 Uiso 1 1 calc R . .
C60 C 0.4962(3) 0.8268(3) 0.3250(3) 0.0319(11) Uani 1 1 d . . .
H60 H 0.5040 0.8019 0.3617 0.038 Uiso 1 1 calc R . .
C61 C 0.4144(3) 0.8421(3) 0.2956(2) 0.0211(9) Uani 1 1 d . . .
C62 C 0.3199(3) 0.8318(3) 0.3211(2) 0.0194(9) Uani 1 1 d . . .
C63 C 0.3043(3) 0.9157(3) 0.3916(2) 0.0226(9) Uani 1 1 d . . .
H63A H 0.3134 0.9643 0.3756 0.027 Uiso 1 1 calc R . .
H63B H 0.2395 0.9101 0.4027 0.027 Uiso 1 1 calc R . .
C64 C 0.3655(3) 0.9387(3) 0.4675(2) 0.0333(12) Uani 1 1 d . . .
H64A H 0.3507 0.8955 0.4885 0.050 Uiso 1 1 calc R . .
H64B H 0.3552 0.9957 0.5060 0.050 Uiso 1 1 calc R . .
H64C H 0.4300 0.9399 0.4567 0.050 Uiso 1 1 calc R . .
C65 C 0.3079(3) 0.7541(3) 0.3449(2) 0.0252(10) Uani 1 1 d . . .
H65A H 0.3255 0.7026 0.3020 0.030 Uiso 1 1 calc R . .
H65B H 0.3503 0.7671 0.3922 0.030 Uiso 1 1 calc R . .
C66 C 0.2104(3) 0.7332(3) 0.3616(3) 0.0342(11) Uani 1 1 d . . .
H66A H 0.1921 0.7840 0.4037 0.051 Uiso 1 1 calc R . .
H66B H 0.2082 0.6852 0.3779 0.051 Uiso 1 1 calc R . .
H66C H 0.1683 0.7168 0.3141 0.051 Uiso 1 1 calc R . .
C67 C 0.2493(3) 0.8196(2) 0.2546(2) 0.0158(8) Uani 1 1 d . . .
C68 C 0.2934(3) 0.6769(3) 0.1597(2) 0.0230(10) Uani 1 1 d . . .
H68A H 0.3568 0.6996 0.1827 0.034 Uiso 1 1 calc R . .
H68B H 0.2916 0.6499 0.1024 0.034 Uiso 1 1 calc R . .
H68C H 0.2697 0.6338 0.1786 0.034 Uiso 1 1 calc R . .
C69 C 0.1612(3) 0.7537(2) 0.1376(2) 0.0176(9) Uani 1 1 d . . .
C70 C 0.1305(3) 0.8315(2) 0.1794(2) 0.0175(9) Uani 1 1 d . . .
H70 H 0.0809 0.8537 0.1621 0.021 Uiso 1 1 calc R . .
C71 C 0.1846(3) 0.8729(3) 0.2522(2) 0.0186(9) Uani 1 1 d . . .
H71 H 0.1780 0.9275 0.2923 0.022 Uiso 1 1 calc R . .
C72 C 0.1246(3) 0.6837(3) 0.0583(2) 0.0202(9) Uani 1 1 d . . .
C73 C 0.0383(3) 0.7133(3) 0.0277(2) 0.0250(10) Uani 1 1 d . . .
H73A H -0.0033 0.7315 0.0698 0.030 Uiso 1 1 calc R . .
H73B H 0.0587 0.7643 0.0174 0.030 Uiso 1 1 calc R . .
C74 C -0.0154(3) 0.6446(3) -0.0465(2) 0.0334(12) Uani 1 1 d . . .
H74A H 0.0271 0.6190 -0.0857 0.050 Uiso 1 1 calc R . .
H74B H -0.0601 0.6711 -0.0675 0.050 Uiso 1 1 calc R . .
H74C H -0.0477 0.5996 -0.0339 0.050 Uiso 1 1 calc R . .
C75 C 0.0949(3) 0.5980(3) 0.0666(2) 0.0218(9) Uani 1 1 d . . .
H75A H 0.0682 0.5538 0.0146 0.026 Uiso 1 1 calc R . .
H75B H 0.1502 0.5776 0.0824 0.026 Uiso 1 1 calc R . .
C76 C 0.0250(3) 0.6061(3) 0.1262(2) 0.0316(11) Uani 1 1 d . . .
H76A H 0.0491 0.6524 0.1771 0.047 Uiso 1 1 calc R . .
H76B H 0.0141 0.5515 0.1320 0.047 Uiso 1 1 calc R . .
H76C H -0.0328 0.6195 0.1077 0.047 Uiso 1 1 calc R . .
C77 C 0.4042(3) 1.1940(2) 0.4019(2) 0.0171(9) Uani 1 1 d . . .
C78 C 0.4299(3) 1.1131(2) 0.4108(2) 0.0204(9) Uani 1 1 d . . .
H78A H 0.3880 1.0984 0.4438 0.031 Uiso 1 1 calc R . .
H78B H 0.4930 1.1243 0.4355 0.031 Uiso 1 1 calc R . .
H78C H 0.4250 1.0650 0.3590 0.031 Uiso 1 1 calc R . .
C79 C 0.4644(3) 1.2174(3) 0.3478(2) 0.0230(10) Uani 1 1 d . . .
H79A H 0.4498 1.1738 0.2938 0.035 Uiso 1 1 calc R . .
H79B H 0.5292 1.2195 0.3648 0.035 Uiso 1 1 calc R . .
H79C H 0.4530 1.2739 0.3499 0.035 Uiso 1 1 calc R . .
C80 C 0.4216(3) 1.2674(3) 0.4842(2) 0.0216(9) Uani 1 1 d . . .
H80A H 0.4092 1.3216 0.4815 0.032 Uiso 1 1 calc R . .
H80B H 0.4858 1.2728 0.5047 0.032 Uiso 1 1 calc R . .
H80C H 0.3811 1.2548 0.5191 0.032 Uiso 1 1 calc R . .
C81 C 0.2664(3) 1.1307(2) 0.3023(2) 0.0185(9) Uani 1 1 d . . .
H81 H 0.2082 1.1431 0.2879 0.022 Uiso 1 1 calc R . .
C82 C 0.2936(3) 1.0603(2) 0.2470(2) 0.0206(9) Uani 1 1 d . . .
H82 H 0.3503 1.0460 0.2622 0.025 Uiso 1 1 calc R . .
C83 C 0.1898(3) 1.0288(3) 0.1241(2) 0.0203(9) Uani 1 1 d . . .
C84 C 0.1698(3) 0.9529(3) 0.0432(2) 0.0257(10) Uani 1 1 d . . .
H84A H 0.2268 0.9423 0.0179 0.039 Uiso 1 1 calc R . .
H84B H 0.1252 0.9667 0.0105 0.039 Uiso 1 1 calc R . .
H84C H 0.1445 0.9011 0.0495 0.039 Uiso 1 1 calc R . .
C85 C 0.0967(3) 1.0448(3) 0.1576(2) 0.0227(9) Uani 1 1 d . . .
H85A H 0.0708 0.9943 0.1655 0.034 Uiso 1 1 calc R . .
H85B H 0.0545 1.0549 0.1206 0.034 Uiso 1 1 calc R . .
H85C H 0.1053 1.0955 0.2079 0.034 Uiso 1 1 calc R . .
C86 C 0.2335(3) 1.1076(3) 0.1125(2) 0.0242(10) Uani 1 1 d . . .
H86A H 0.2565 1.1538 0.1637 0.036 Uiso 1 1 calc R . .
H86B H 0.1873 1.1278 0.0864 0.036 Uiso 1 1 calc R . .
H86C H 0.2844 1.0915 0.0799 0.036 Uiso 1 1 calc R . .
C87 C 0.4354(9) 0.5092(8) 0.0890(8) 0.160(5) Uiso 1 1 d D . .
H87 H 0.4851 0.5462 0.0847 0.192 Uiso 1 1 calc RD . .
C88 C 0.3696(9) 0.4754(7) 0.0337(7) 0.147(4) Uiso 1 1 d D . .
H88 H 0.3765 0.4954 -0.0065 0.177 Uiso 1 1 calc RD . .
C89 C 0.2967(9) 0.4213(8) 0.0187(8) 0.160(5) Uiso 1 1 d D . .
H89 H 0.2513 0.4028 -0.0249 0.191 Uiso 1 1 calc RD . .
C90 C 0.2998(10) 0.3932(10) 0.0874(9) 0.189(6) Uiso 1 1 d D . .
H90 H 0.2579 0.3460 0.0845 0.227 Uiso 1 1 calc RD . .
C91 C 0.3589(11) 0.4329(9) 0.1500(9) 0.184(5) Uiso 1 1 d D . .
H91 H 0.3508 0.4211 0.1949 0.221 Uiso 1 1 calc RD . .
C92 C 0.4337(10) 0.4922(9) 0.1531(9) 0.182(5) Uiso 1 1 d D . .
H92 H 0.4791 0.5179 0.1967 0.218 Uiso 1 1 calc RD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.01131(11) 0.01311(11) 0.01473(11) 0.00442(8) 0.00173(8) 0.00226(8)
Sm2 0.01261(11) 0.01399(11) 0.01121(10) 0.00291(8) -0.00050(8) -0.00052(8)
N1 0.0154(17) 0.0197(17) 0.0198(17) 0.0100(15) 0.0024(14) 0.0039(13)
N2 0.0175(18) 0.0155(17) 0.0196(17) 0.0081(14) 0.0043(14) 0.0030(13)
N3 0.0147(17) 0.0175(17) 0.0188(17) 0.0058(14) 0.0023(13) 0.0021(13)
N4 0.0153(17) 0.0156(17) 0.0177(17) 0.0042(14) 0.0020(14) 0.0027(13)
N5 0.0205(18) 0.0201(18) 0.0154(16) 0.0067(15) 0.0016(14) -0.0041(14)
N6 0.0152(17) 0.0208(18) 0.0175(17) 0.0046(15) 0.0032(14) -0.0010(14)
N7 0.0144(17) 0.0171(17) 0.0156(16) 0.0058(14) -0.0006(13) 0.0023(13)
N8 0.0206(18) 0.0156(17) 0.0144(16) 0.0056(14) 0.0029(14) -0.0004(14)
N9 0.0161(17) 0.0110(16) 0.0146(16) 0.0017(13) 0.0028(13) 0.0022(13)
N10 0.0145(17) 0.0161(17) 0.0152(16) 0.0043(14) 0.0010(13) -0.0013(13)
C1 0.0100(19) 0.021(2) 0.021(2) 0.0068(18) -0.0020(16) -0.0024(16)
C2 0.009(2) 0.029(2) 0.037(2) 0.016(2) -0.0014(18) 0.0022(17)
C3 0.019(2) 0.031(2) 0.033(2) 0.017(2) -0.0039(19) 0.0062(18)
C4 0.018(2) 0.020(2) 0.024(2) 0.0123(18) 0.0022(17) 0.0050(16)
C5 0.018(2) 0.019(2) 0.025(2) 0.0101(18) -0.0008(17) 0.0019(16)
C6 0.029(2) 0.020(2) 0.022(2) 0.0107(18) -0.0008(18) 0.0035(18)
C7 0.033(3) 0.026(2) 0.029(2) 0.010(2) -0.006(2) 0.0020(19)
C8 0.030(2) 0.022(2) 0.023(2) 0.0111(19) -0.0054(19) 0.0075(18)
C9 0.039(3) 0.029(3) 0.043(3) 0.020(2) -0.006(2) 0.000(2)
C10 0.017(2) 0.015(2) 0.020(2) 0.0096(17) 0.0008(16) 0.0029(15)
C11 0.017(2) 0.023(2) 0.028(2) 0.0071(19) 0.0074(18) 0.0081(17)
C12 0.023(2) 0.014(2) 0.021(2) 0.0093(17) 0.0028(17) 0.0004(16)
C13 0.016(2) 0.014(2) 0.025(2) 0.0088(18) 0.0070(17) 0.0008(15)
C14 0.022(2) 0.016(2) 0.019(2) 0.0065(17) 0.0038(17) -0.0021(16)
C15 0.018(2) 0.0128(19) 0.018(2) 0.0015(17) 0.0039(16) 0.0032(15)
C16 0.019(2) 0.021(2) 0.024(2) 0.0083(19) 0.0022(17) 0.0029(17)
C17 0.026(2) 0.033(3) 0.024(2) 0.005(2) -0.0012(19) -0.004(2)
C18 0.027(2) 0.015(2) 0.024(2) 0.0067(18) 0.0013(18) 0.0033(17)
C19 0.039(3) 0.018(2) 0.038(3) 0.012(2) 0.003(2) 0.0012(19)
C20 0.017(2) 0.015(2) 0.019(2) 0.0059(17) 0.0028(16) -0.0004(15)
C21 0.021(2) 0.014(2) 0.023(2) 0.0023(18) 0.0040(17) 0.0019(16)
C22 0.022(2) 0.022(2) 0.017(2) 0.0042(18) 0.0045(17) 0.0047(17)
C23 0.015(2) 0.020(2) 0.0160(19) 0.0052(17) 0.0013(16) 0.0035(16)
C24 0.027(2) 0.016(2) 0.017(2) 0.0049(17) 0.0029(17) 0.0015(17)
C25 0.036(3) 0.021(2) 0.021(2) 0.0055(19) -0.0073(19) 0.0068(19)
C26 0.049(3) 0.040(3) 0.034(3) 0.004(2) -0.014(2) 0.010(2)
C27 0.043(3) 0.026(2) 0.019(2) 0.010(2) 0.009(2) 0.001(2)
C28 0.094(5) 0.033(3) 0.049(3) 0.017(3) 0.041(3) 0.008(3)
C29 0.017(2) 0.018(2) 0.018(2) 0.0083(17) 0.0006(16) 0.0002(16)
C30 0.016(2) 0.021(2) 0.026(2) 0.0033(19) 0.0045(17) 0.0049(17)
C31 0.016(2) 0.017(2) 0.018(2) 0.0089(17) 0.0029(16) 0.0005(16)
C32 0.023(2) 0.0134(19) 0.0146(19) 0.0057(17) 0.0033(16) 0.0000(16)
C33 0.018(2) 0.015(2) 0.024(2) 0.0123(18) 0.0036(17) 0.0034(16)
C34 0.0111(19) 0.019(2) 0.023(2) 0.0096(18) 0.0015(16) -0.0012(15)
C35 0.015(2) 0.022(2) 0.022(2) 0.0059(18) 0.0025(17) 0.0020(16)
C36 0.021(2) 0.028(2) 0.026(2) 0.004(2) -0.0016(18) -0.0010(18)
C37 0.018(2) 0.022(2) 0.021(2) 0.0079(18) 0.0021(17) 0.0001(16)
C38 0.029(3) 0.034(3) 0.041(3) 0.020(2) 0.016(2) 0.004(2)
C39 0.022(2) 0.018(2) 0.016(2) 0.0009(18) 0.0010(17) -0.0082(17)
C40 0.036(3) 0.020(2) 0.021(2) 0.0010(19) 0.0050(19) -0.0099(19)
C41 0.036(3) 0.021(2) 0.019(2) -0.0005(19) 0.0082(19) -0.0024(19)
C42 0.025(2) 0.020(2) 0.0132(19) 0.0006(17) 0.0030(17) -0.0020(17)
C43 0.026(2) 0.024(2) 0.0122(19) 0.0034(18) 0.0047(17) -0.0057(18)
C44 0.032(3) 0.025(2) 0.016(2) 0.0038(19) -0.0013(18) -0.0076(19)
C45 0.055(3) 0.037(3) 0.021(2) 0.002(2) -0.012(2) -0.003(2)
C46 0.033(3) 0.024(2) 0.018(2) 0.0006(19) 0.0061(19) -0.0041(19)
C47 0.049(3) 0.033(3) 0.038(3) 0.000(2) 0.029(3) -0.003(2)
C48 0.018(2) 0.022(2) 0.0135(19) 0.0044(17) 0.0003(16) -0.0056(16)
C49 0.026(2) 0.022(2) 0.025(2) 0.0050(19) 0.0043(19) 0.0051(18)
C50 0.012(2) 0.020(2) 0.0148(19) 0.0021(17) 0.0063(16) -0.0028(16)
C51 0.015(2) 0.017(2) 0.0162(19) 0.0038(17) 0.0035(16) -0.0044(16)
C52 0.017(2) 0.023(2) 0.0158(19) 0.0086(18) 0.0021(16) -0.0028(16)
C53 0.016(2) 0.025(2) 0.019(2) 0.0070(18) 0.0000(16) 0.0035(17)
C54 0.016(2) 0.025(2) 0.017(2) 0.0021(18) -0.0035(16) -0.0042(17)
C55 0.024(2) 0.039(3) 0.023(2) -0.002(2) -0.0082(19) 0.001(2)
C56 0.013(2) 0.037(3) 0.026(2) 0.007(2) 0.0018(17) 0.0050(18)
C57 0.019(2) 0.070(4) 0.043(3) 0.024(3) 0.013(2) 0.011(2)
C58 0.012(2) 0.024(2) 0.021(2) 0.0062(18) -0.0008(16) 0.0079(16)
C59 0.018(2) 0.046(3) 0.036(3) 0.022(2) -0.002(2) 0.008(2)
C60 0.028(3) 0.047(3) 0.031(2) 0.027(2) -0.003(2) 0.008(2)
C61 0.025(2) 0.021(2) 0.017(2) 0.0085(18) -0.0016(17) 0.0024(17)
C62 0.020(2) 0.021(2) 0.019(2) 0.0099(18) 0.0017(17) 0.0012(17)
C63 0.026(2) 0.023(2) 0.016(2) 0.0071(18) 0.0020(17) -0.0038(18)
C64 0.046(3) 0.031(3) 0.015(2) 0.004(2) -0.005(2) -0.004(2)
C65 0.029(2) 0.026(2) 0.023(2) 0.0148(19) 0.0002(19) -0.0019(19)
C66 0.035(3) 0.037(3) 0.038(3) 0.025(2) 0.005(2) -0.004(2)
C67 0.016(2) 0.018(2) 0.0139(19) 0.0078(17) 0.0037(16) -0.0037(16)
C68 0.024(2) 0.018(2) 0.021(2) 0.0029(18) -0.0017(18) 0.0031(17)
C69 0.017(2) 0.018(2) 0.019(2) 0.0098(17) 0.0000(16) -0.0044(16)
C70 0.0111(19) 0.021(2) 0.020(2) 0.0097(18) 0.0018(16) -0.0012(16)
C71 0.019(2) 0.022(2) 0.0135(19) 0.0069(17) 0.0025(16) 0.0001(17)
C72 0.018(2) 0.021(2) 0.017(2) 0.0066(18) -0.0012(17) -0.0073(17)
C73 0.019(2) 0.031(2) 0.023(2) 0.010(2) -0.0015(18) -0.0059(18)
C74 0.035(3) 0.033(3) 0.026(2) 0.011(2) -0.010(2) -0.015(2)
C75 0.025(2) 0.019(2) 0.016(2) 0.0054(18) -0.0013(17) -0.0078(17)
C76 0.039(3) 0.031(3) 0.024(2) 0.013(2) 0.006(2) -0.006(2)
C77 0.013(2) 0.016(2) 0.019(2) 0.0043(17) 0.0022(16) 0.0022(15)
C78 0.017(2) 0.021(2) 0.021(2) 0.0061(18) -0.0013(17) 0.0050(16)
C79 0.019(2) 0.020(2) 0.028(2) 0.0070(19) 0.0045(18) 0.0008(17)
C80 0.013(2) 0.022(2) 0.024(2) 0.0054(18) -0.0049(17) -0.0007(16)
C81 0.013(2) 0.020(2) 0.021(2) 0.0059(18) 0.0012(16) 0.0073(16)
C82 0.020(2) 0.018(2) 0.020(2) 0.0049(18) -0.0044(17) 0.0021(16)
C83 0.018(2) 0.021(2) 0.021(2) 0.0080(18) 0.0011(17) -0.0005(16)
C84 0.027(2) 0.029(2) 0.019(2) 0.0083(19) -0.0066(18) 0.0003(19)
C85 0.019(2) 0.023(2) 0.025(2) 0.0085(19) 0.0017(17) 0.0018(17)
C86 0.026(2) 0.025(2) 0.020(2) 0.0084(19) 0.0042(18) 0.0016(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100873.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100873.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100873
loop_
_publ_author_name
'Adams, Richard D.'
'Captain, Burjor'
'Zhu, Lei'
_publ_section_title
;
Platinum Participation in the Hydrogenation of Phenylacetylene by
Ru~5~(CO)~15~(C)[Pt(PBut~3~)]
;
_journal_coden_ASTM JACSAT
_journal_issue 10
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 3042
_journal_page_last 3043
_journal_paper_doi 10.1021/ja049955y
_journal_volume 126
_journal_year 2004
_chemical_formula_sum 'C38 H42 O13 P Pt Ru5'
_chemical_formula_weight 1438.13
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 92.6780(10)
_cell_angle_beta 91.0510(10)
_cell_angle_gamma 109.9580(10)
_cell_formula_units_Z 2
_cell_length_a 12.6218(5)
_cell_length_b 13.3776(5)
_cell_length_c 14.3654(5)
_cell_measurement_reflns_used 9203
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.15
_cell_measurement_theta_min 2.19
_cell_volume 2275.91(15)
_computing_cell_refinement 'SAINT+ V6.2 (Bruker, 2001)'
_computing_data_collection 'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction 'SAINT+ V6.2'
_computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material 'SHELXTL V6.1'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0247
_diffrn_reflns_av_sigmaI/netI 0.0372
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 24147
_diffrn_reflns_theta_full 28.33
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 1.62
_diffrn_standards_decay_% <1
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 4.771
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.794
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details '(SADABS, Bruker, 1997)'
_exptl_crystal_colour DarkRed
_exptl_crystal_density_diffrn 2.099
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 1374
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_refine_diff_density_max 5.424
_refine_diff_density_min -2.445
_refine_diff_density_rms 0.147
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 515
_refine_ls_number_reflns 11222
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0578
_refine_ls_R_factor_gt 0.0454
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+7.9341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1139
_refine_ls_wR_factor_ref 0.1227
_reflns_number_gt 9150
_reflns_number_total 11222
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om050175nsi20050310_030426.cif
_cod_data_source_block bcru5pts
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100873
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.75970(2) 0.46562(2) 0.224446(17) 0.05137(9) Uani 1 1 d . . .
Ru1 Ru 0.78415(5) 0.56492(4) 0.39389(3) 0.04791(13) Uani 1 1 d . . .
Ru2 Ru 0.91658(4) 0.67774(4) 0.23658(3) 0.04235(12) Uani 1 1 d . . .
Ru3 Ru 0.70108(4) 0.66478(4) 0.23858(3) 0.04232(12) Uani 1 1 d . . .
Ru4 Ru 0.72579(5) 0.74594(5) 0.43174(4) 0.05234(14) Uani 1 1 d . . .
Ru5 Ru 0.95839(5) 0.75695(4) 0.42943(4) 0.05042(13) Uani 1 1 d . . .
P1 P 0.70796(18) 0.30196(15) 0.14298(14) 0.0582(4) Uani 1 1 d . . .
O11 O 0.9486(6) 0.4411(5) 0.3904(4) 0.0821(17) Uani 1 1 d . . .
O12 O 0.7804(7) 0.5528(6) 0.6049(4) 0.094(2) Uani 1 1 d . . .
O13 O 0.5365(5) 0.4245(6) 0.3847(5) 0.0872(18) Uani 1 1 d . . .
O21 O 1.1056(6) 0.5836(6) 0.2244(6) 0.102(2) Uani 1 1 d . . .
O22 O 1.0693(6) 0.8864(5) 0.1729(5) 0.095(2) Uani 1 1 d . . .
O31 O 0.4559(5) 0.5285(6) 0.2010(5) 0.098(2) Uani 1 1 d . . .
O32 O 0.6501(7) 0.8553(5) 0.1800(5) 0.100(2) Uani 1 1 d . . .
O41 O 0.4710(6) 0.6544(7) 0.4098(5) 0.102(2) Uani 1 1 d . . .
O42 O 0.7137(6) 0.7709(7) 0.6439(4) 0.100(2) Uani 1 1 d . . .
O43 O 0.7668(7) 0.9773(6) 0.3954(6) 0.104(2) Uani 1 1 d . . .
O51 O 1.0817(7) 0.9886(5) 0.3950(6) 0.103(2) Uani 1 1 d . . .
O52 O 0.9679(6) 0.7961(6) 0.6407(4) 0.095(2) Uani 1 1 d . . .
O53 O 1.1596(6) 0.6798(6) 0.4365(5) 0.097(2) Uani 1 1 d . . .
C1 C 0.8277(5) 0.7190(5) 0.3384(4) 0.0428(12) Uani 1 1 d . . .
C2 C 0.7900(6) 0.6473(5) 0.1203(4) 0.0475(14) Uani 1 1 d . . .
C3 C 0.8248(7) 0.5611(6) 0.1233(5) 0.0589(17) Uani 1 1 d . . .
C11 C 0.8856(7) 0.4844(6) 0.3845(5) 0.0614(18) Uani 1 1 d . . .
C12 C 0.7833(8) 0.5626(7) 0.5265(5) 0.070(2) Uani 1 1 d . . .
C13 C 0.6289(7) 0.4745(7) 0.3802(5) 0.0655(19) Uani 1 1 d . . .
C21 C 1.0371(7) 0.6200(7) 0.2283(6) 0.0659(19) Uani 1 1 d . . .
C22 C 1.0117(7) 0.8069(6) 0.1955(5) 0.0603(17) Uani 1 1 d . . .
C31 C 0.5478(7) 0.5800(7) 0.2140(6) 0.0642(19) Uani 1 1 d . . .
C32 C 0.6700(7) 0.7822(6) 0.2005(5) 0.0612(18) Uani 1 1 d . . .
C41 C 0.5658(8) 0.6888(8) 0.4151(6) 0.074(2) Uani 1 1 d . . .
C42 C 0.7183(7) 0.7601(8) 0.5656(5) 0.072(2) Uani 1 1 d . . .
C43 C 0.7464(7) 0.8906(7) 0.4105(6) 0.069(2) Uani 1 1 d . . .
C51 C 1.0373(7) 0.9026(6) 0.4088(5) 0.0659(19) Uani 1 1 d . . .
C52 C 0.9625(7) 0.7798(7) 0.5617(5) 0.0654(19) Uani 1 1 d . . .
C53 C 1.0855(7) 0.7092(7) 0.4329(6) 0.068(2) Uani 1 1 d . . .
C61 C 0.8023(6) 0.7098(6) 0.0352(4) 0.0568(17) Uani 1 1 d . . .
C62 C 0.8388(8) 0.8202(6) 0.0379(5) 0.073(2) Uani 1 1 d . . .
H62 H 0.8562 0.8577 0.0955 0.088 Uiso 1 1 calc R . .
C63 C 0.8504(10) 0.8762(8) -0.0416(6) 0.090(3) Uani 1 1 d . . .
H63 H 0.8754 0.9503 -0.0375 0.108 Uiso 1 1 calc R . .
C64 C 0.8242(11) 0.8208(9) -0.1275(7) 0.104(4) Uani 1 1 d . . .
H64 H 0.8317 0.8575 -0.1818 0.125 Uiso 1 1 calc R . .
C65 C 0.7877(10) 0.7133(9) -0.1322(5) 0.095(3) Uani 1 1 d . . .
H65 H 0.7705 0.6764 -0.1901 0.114 Uiso 1 1 calc R . .
C66 C 0.7755(8) 0.6569(7) -0.0523(5) 0.072(2) Uani 1 1 d . . .
H66 H 0.7491 0.5828 -0.0573 0.086 Uiso 1 1 calc R . .
C71 C 0.6041(17) 0.2850(12) 0.0447(16) 0.218(13) Uani 1 1 d . . .
C72 C 0.5411(14) 0.3563(13) 0.0510(11) 0.165(8) Uani 1 1 d . . .
H72A H 0.5099 0.3607 -0.0095 0.248 Uiso 1 1 calc R . .
H72B H 0.5901 0.4257 0.0734 0.248 Uiso 1 1 calc R . .
H72C H 0.4812 0.3301 0.0934 0.248 Uiso 1 1 calc R . .
C73 C 0.7016(16) 0.3478(12) -0.0513(8) 0.148(6) Uani 1 1 d . . .
H73A H 0.6623 0.3259 -0.1107 0.223 Uiso 1 1 calc R . .
H73B H 0.7662 0.3253 -0.0494 0.223 Uiso 1 1 calc R . .
H73C H 0.7258 0.4239 -0.0424 0.223 Uiso 1 1 calc R . .
C74 C 0.5394(12) 0.1725(10) 0.0074(11) 0.141(6) Uani 1 1 d . . .
H74A H 0.4648 0.1501 0.0311 0.211 Uiso 1 1 calc R . .
H74B H 0.5776 0.1257 0.0270 0.211 Uiso 1 1 calc R . .
H74C H 0.5348 0.1704 -0.0595 0.211 Uiso 1 1 calc R . .
C75 C 0.8363(11) 0.2703(10) 0.1002(8) 0.105(4) Uani 1 1 d . . .
C76 C 0.9256(11) 0.3603(12) 0.0682(13) 0.149(6) Uani 1 1 d . . .
H76A H 0.9847 0.3372 0.0449 0.223 Uiso 1 1 calc R . .
H76B H 0.9550 0.4122 0.1191 0.223 Uiso 1 1 calc R . .
H76C H 0.8965 0.3914 0.0194 0.223 Uiso 1 1 calc R . .
C77 C 0.8119(11) 0.1688(10) 0.0366(9) 0.117(4) Uani 1 1 d . . .
H77A H 0.7693 0.1736 -0.0180 0.175 Uiso 1 1 calc R . .
H77B H 0.7694 0.1080 0.0696 0.175 Uiso 1 1 calc R . .
H77C H 0.8818 0.1614 0.0185 0.175 Uiso 1 1 calc R . .
C78 C 0.8959(14) 0.2464(15) 0.1971(10) 0.165(7) Uani 1 1 d . . .
H78A H 0.9448 0.2073 0.1811 0.248 Uiso 1 1 calc R . .
H78B H 0.8383 0.2054 0.2365 0.248 Uiso 1 1 calc R . .
H78C H 0.9390 0.3127 0.2295 0.248 Uiso 1 1 calc R . .
C79 C 0.6444(15) 0.2002(8) 0.2297(10) 0.138(6) Uani 1 1 d . . .
C80 C 0.4963(15) 0.2129(15) 0.2204(18) 0.267(16) Uani 1 1 d . . .
H80A H 0.4401 0.1464 0.2338 0.400 Uiso 1 1 calc R . .
H80B H 0.4827 0.2307 0.1584 0.400 Uiso 1 1 calc R . .
H80C H 0.4926 0.2679 0.2643 0.400 Uiso 1 1 calc R . .
C81 C 0.6776(17) 0.2260(9) 0.3218(8) 0.167(8) Uani 1 1 d . . .
H81A H 0.6223 0.1803 0.3603 0.250 Uiso 1 1 calc R . .
H81B H 0.6848 0.2988 0.3366 0.250 Uiso 1 1 calc R . .
H81C H 0.7490 0.2170 0.3329 0.250 Uiso 1 1 calc R . .
C82 C 0.6164(13) 0.0840(8) 0.2023(10) 0.127(5) Uani 1 1 d . . .
H82A H 0.6843 0.0705 0.1874 0.191 Uiso 1 1 calc R . .
H82B H 0.5653 0.0652 0.1488 0.191 Uiso 1 1 calc R . .
H82C H 0.5817 0.0422 0.2531 0.191 Uiso 1 1 calc R . .
H1 H 0.879(5) 0.550(5) 0.067(4) 0.036(15) Uiso 1 1 d . . .
C90 C 0.668(2) 0.156(2) 0.7428(18) 0.277(14) Uiso 1 1 d D . .
H90A H 0.6347 0.2029 0.7158 0.415 Uiso 1 1 calc R . .
H90B H 0.7433 0.1961 0.7658 0.415 Uiso 1 1 calc R . .
H90C H 0.6237 0.1215 0.7932 0.415 Uiso 1 1 calc R . .
C91 C 0.672(3) 0.073(3) 0.670(2) 0.321(17) Uiso 1 1 d D . .
H91A H 0.6411 0.0010 0.6894 0.386 Uiso 1 1 calc R . .
H91B H 0.7466 0.0869 0.6450 0.386 Uiso 1 1 calc R . .
C92 C 0.592(3) 0.106(2) 0.6067(19) 0.294(15) Uiso 1 1 d D . .
H92A H 0.5327 0.1194 0.6425 0.352 Uiso 1 1 calc R . .
H92B H 0.6320 0.1702 0.5751 0.352 Uiso 1 1 calc R . .
C93 C 0.544(2) 0.013(2) 0.5389(19) 0.270(14) Uiso 1 1 d D . .
H93A H 0.5175 -0.0467 0.5780 0.324 Uiso 1 1 calc R . .
H93B H 0.6096 0.0067 0.5092 0.324 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.06937(18) 0.04269(14) 0.04202(14) 0.00791(10) 0.00151(11) 0.01849(12)
Ru1 0.0603(3) 0.0474(3) 0.0345(2) 0.01078(19) -0.0006(2) 0.0155(2)
Ru2 0.0453(3) 0.0454(3) 0.0357(2) 0.00817(19) 0.00172(18) 0.0140(2)
Ru3 0.0490(3) 0.0469(3) 0.0348(2) 0.00582(18) -0.00357(18) 0.0211(2)
Ru4 0.0611(3) 0.0612(3) 0.0376(3) 0.0019(2) 0.0039(2) 0.0247(3)
Ru5 0.0573(3) 0.0522(3) 0.0392(3) 0.0037(2) -0.0099(2) 0.0159(2)
P1 0.0686(11) 0.0447(9) 0.0638(11) 0.0002(8) -0.0041(9) 0.0234(8)
O11 0.094(4) 0.090(4) 0.077(4) 0.015(3) -0.010(3) 0.049(4)
O12 0.139(6) 0.105(5) 0.039(3) 0.021(3) 0.001(3) 0.039(4)
O13 0.074(4) 0.091(5) 0.083(4) 0.015(3) 0.012(3) 0.009(3)
O21 0.076(4) 0.120(6) 0.127(6) 0.010(5) 0.018(4) 0.056(4)
O22 0.108(5) 0.069(4) 0.080(4) 0.023(3) 0.012(4) -0.010(4)
O31 0.065(4) 0.100(5) 0.117(6) 0.009(4) -0.025(4) 0.013(4)
O32 0.147(6) 0.075(4) 0.103(5) 0.007(4) -0.028(4) 0.069(4)
O41 0.069(4) 0.135(7) 0.096(5) 0.000(5) -0.002(4) 0.028(4)
O42 0.105(5) 0.159(7) 0.041(3) -0.005(4) 0.005(3) 0.052(5)
O43 0.138(7) 0.075(5) 0.112(6) 0.004(4) 0.008(5) 0.053(5)
O51 0.119(6) 0.052(4) 0.117(6) 0.004(4) 0.001(4) 0.002(4)
O52 0.108(5) 0.142(6) 0.043(3) -0.007(3) -0.021(3) 0.055(5)
O53 0.084(4) 0.116(6) 0.106(5) 0.017(4) 0.001(4) 0.052(4)
C1 0.048(3) 0.044(3) 0.036(3) 0.004(2) -0.002(2) 0.014(3)
C2 0.062(4) 0.049(3) 0.033(3) 0.005(2) -0.004(3) 0.022(3)
C3 0.075(5) 0.059(4) 0.043(3) 0.008(3) 0.002(3) 0.021(4)
C11 0.072(5) 0.057(4) 0.054(4) 0.015(3) -0.004(3) 0.020(4)
C12 0.093(6) 0.069(5) 0.045(4) 0.010(3) 0.000(4) 0.021(4)
C13 0.066(5) 0.067(5) 0.057(4) 0.016(4) 0.003(3) 0.012(4)
C21 0.059(4) 0.072(5) 0.068(5) 0.013(4) 0.008(4) 0.022(4)
C22 0.067(4) 0.057(4) 0.049(4) 0.011(3) 0.005(3) 0.011(3)
C31 0.058(4) 0.069(5) 0.066(5) 0.006(4) -0.014(3) 0.023(4)
C32 0.074(5) 0.066(5) 0.052(4) 0.000(3) -0.012(3) 0.036(4)
C41 0.071(5) 0.089(6) 0.062(5) 0.005(4) 0.001(4) 0.025(5)
C42 0.066(5) 0.102(7) 0.049(4) -0.001(4) 0.001(3) 0.033(5)
C43 0.081(5) 0.069(5) 0.064(5) -0.005(4) 0.003(4) 0.037(4)
C51 0.075(5) 0.055(4) 0.058(4) -0.001(3) -0.008(4) 0.011(4)
C52 0.063(4) 0.083(5) 0.053(4) 0.002(4) -0.013(3) 0.030(4)
C53 0.070(5) 0.067(5) 0.066(5) 0.008(4) -0.007(4) 0.020(4)
C61 0.075(5) 0.060(4) 0.038(3) 0.013(3) -0.005(3) 0.025(4)
C62 0.115(7) 0.053(4) 0.050(4) 0.011(3) -0.007(4) 0.025(4)
C63 0.133(9) 0.066(5) 0.063(5) 0.027(4) -0.008(5) 0.023(5)
C64 0.151(10) 0.095(8) 0.057(5) 0.039(5) -0.008(6) 0.025(7)
C65 0.140(9) 0.110(8) 0.033(4) 0.011(4) -0.012(4) 0.038(7)
C66 0.100(6) 0.070(5) 0.037(3) 0.006(3) -0.008(4) 0.019(4)
C71 0.245(19) 0.114(10) 0.32(3) -0.133(14) -0.24(2) 0.123(13)
C72 0.207(16) 0.172(14) 0.158(13) -0.076(11) -0.117(12) 0.136(13)
C73 0.26(2) 0.130(12) 0.066(7) 0.009(7) -0.006(10) 0.082(13)
C74 0.147(11) 0.102(9) 0.170(14) -0.062(9) -0.084(10) 0.053(9)
C75 0.121(9) 0.103(8) 0.098(8) -0.021(6) 0.026(7) 0.047(7)
C76 0.096(9) 0.130(12) 0.208(18) -0.029(12) 0.039(10) 0.027(8)
C77 0.142(11) 0.113(9) 0.113(9) -0.039(7) -0.004(8) 0.074(8)
C78 0.181(15) 0.24(2) 0.120(11) -0.041(12) -0.063(10) 0.145(15)
C79 0.227(16) 0.045(5) 0.119(10) 0.009(6) 0.073(11) 0.015(7)
C80 0.167(16) 0.165(16) 0.40(4) -0.083(19) 0.20(2) -0.032(13)
C81 0.33(2) 0.062(6) 0.077(8) 0.029(6) -0.029(11) 0.021(10)
C82 0.190(14) 0.056(6) 0.131(11) 0.007(6) 0.022(10) 0.037(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Pt1 P1 100.2(2) . . ?
C3 Pt1 Ru1 114.2(2) . . ?
P1 Pt1 Ru1 145.02(5) . . ?
C3 Pt1 Ru2 50.7(2) . . ?
P1 Pt1 Ru2 144.80(6) . . ?
Ru1 Pt1 Ru2 65.318(16) . . ?
C3 Pt1 Ru3 68.0(2) . . ?
P1 Pt1 Ru3 141.09(5) . . ?
Ru1 Pt1 Ru3 63.557(15) . . ?
Ru2 Pt1 Ru3 54.208(15) . . ?
C12 Ru1 C13 92.6(4) . . ?
C12 Ru1 C11 92.8(4) . . ?
C13 Ru1 C11 111.9(4) . . ?
C12 Ru1 C1 115.9(3) . . ?
C13 Ru1 C1 116.9(3) . . ?
C11 Ru1 C1 120.7(3) . . ?
C12 Ru1 Pt1 151.2(3) . . ?
C13 Ru1 Pt1 73.8(2) . . ?
C11 Ru1 Pt1 70.2(2) . . ?
C1 Ru1 Pt1 92.95(15) . . ?
C12 Ru1 Ru5 83.5(3) . . ?
C13 Ru1 Ru5 154.8(3) . . ?
C11 Ru1 Ru5 93.2(2) . . ?
C1 Ru1 Ru5 45.73(15) . . ?
Pt1 Ru1 Ru5 119.39(2) . . ?
C12 Ru1 Ru4 81.6(3) . . ?
C13 Ru1 Ru4 92.2(3) . . ?
C11 Ru1 Ru4 155.5(2) . . ?
C1 Ru1 Ru4 44.89(16) . . ?
Pt1 Ru1 Ru4 123.32(2) . . ?
Ru5 Ru1 Ru4 62.56(2) . . ?
C12 Ru1 Ru2 142.9(3) . . ?
C13 Ru1 Ru2 123.3(2) . . ?
C11 Ru1 Ru2 82.8(2) . . ?
C1 Ru1 Ru2 42.75(16) . . ?
Pt1 Ru1 Ru2 60.072(15) . . ?
Ru5 Ru1 Ru2 60.196(18) . . ?
Ru4 Ru1 Ru2 87.51(2) . . ?
C12 Ru1 Ru3 139.8(3) . . ?
C13 Ru1 Ru3 78.6(2) . . ?
C11 Ru1 Ru3 127.0(2) . . ?
C1 Ru1 Ru3 42.79(15) . . ?
Pt1 Ru1 Ru3 63.408(15) . . ?
Ru5 Ru1 Ru3 88.35(2) . . ?
Ru4 Ru1 Ru3 59.997(17) . . ?
Ru2 Ru1 Ru3 52.893(16) . . ?
C22 Ru2 C21 90.2(3) . . ?
C22 Ru2 C1 104.8(3) . . ?
C21 Ru2 C1 137.4(3) . . ?
C22 Ru2 C3 114.2(3) . . ?
C21 Ru2 C3 88.4(3) . . ?
C1 Ru2 C3 119.0(3) . . ?
C22 Ru2 C2 95.4(3) . . ?
C21 Ru2 C2 120.1(3) . . ?
C1 Ru2 C2 98.3(2) . . ?
C3 Ru2 C2 36.0(3) . . ?
C22 Ru2 Ru3 113.0(3) . . ?
C21 Ru2 Ru3 154.4(3) . . ?
C1 Ru2 Ru3 49.24(16) . . ?
C3 Ru2 Ru3 72.6(2) . . ?
C2 Ru2 Ru3 49.94(17) . . ?
C22 Ru2 Pt1 158.1(2) . . ?
C21 Ru2 Pt1 88.6(2) . . ?
C1 Ru2 Pt1 90.66(17) . . ?
C3 Ru2 Pt1 43.87(19) . . ?
C2 Ru2 Pt1 66.66(17) . . ?
Ru3 Ru2 Pt1 65.772(16) . . ?
C22 Ru2 Ru5 91.7(2) . . ?
C21 Ru2 Ru5 97.5(3) . . ?
C1 Ru2 Ru5 43.56(16) . . ?
C3 Ru2 Ru5 153.40(19) . . ?
C2 Ru2 Ru5 141.59(17) . . ?
Ru3 Ru2 Ru5 92.72(2) . . ?
Pt1 Ru2 Ru5 110.089(19) . . ?
C22 Ru2 Ru1 146.3(2) . . ?
C21 Ru2 Ru1 103.0(2) . . ?
C1 Ru2 Ru1 45.81(17) . . ?
C3 Ru2 Ru1 97.18(19) . . ?
C2 Ru2 Ru1 104.04(17) . . ?
Ru3 Ru2 Ru1 63.865(18) . . ?
Pt1 Ru2 Ru1 54.611(14) . . ?
Ru5 Ru2 Ru1 56.214(17) . . ?
C32 Ru3 C31 89.5(3) . . ?
C32 Ru3 C1 106.8(3) . . ?
C31 Ru3 C1 145.1(3) . . ?
C32 Ru3 C2 95.8(3) . . ?
C31 Ru3 C2 107.1(3) . . ?
C1 Ru3 C2 101.7(2) . . ?
C32 Ru3 Ru2 116.3(3) . . ?
C31 Ru3 Ru2 147.5(3) . . ?
C1 Ru3 Ru2 48.83(17) . . ?
C2 Ru3 Ru2 53.77(17) . . ?
C32 Ru3 Ru4 91.2(2) . . ?
C31 Ru3 Ru4 108.1(3) . . ?
C1 Ru3 Ru4 42.91(17) . . ?
C2 Ru3 Ru4 144.09(18) . . ?
Ru2 Ru3 Ru4 91.69(2) . . ?
C32 Ru3 Pt1 158.8(2) . . ?
C31 Ru3 Pt1 88.7(2) . . ?
C1 Ru3 Pt1 86.26(17) . . ?
C2 Ru3 Pt1 64.69(17) . . ?
Ru2 Ru3 Pt1 60.021(15) . . ?
Ru4 Ru3 Pt1 109.434(18) . . ?
C32 Ru3 Ru1 146.9(2) . . ?
C31 Ru3 Ru1 106.3(2) . . ?
C1 Ru3 Ru1 45.48(17) . . ?
C2 Ru3 Ru1 106.59(16) . . ?
Ru2 Ru3 Ru1 63.241(17) . . ?
Ru4 Ru3 Ru1 56.464(17) . . ?
Pt1 Ru3 Ru1 53.035(14) . . ?
C43 Ru4 C41 98.4(4) . . ?
C43 Ru4 C42 95.9(4) . . ?
C41 Ru4 C42 92.6(4) . . ?
C43 Ru4 C1 99.8(3) . . ?
C41 Ru4 C1 122.2(3) . . ?
C42 Ru4 C1 138.6(3) . . ?
C43 Ru4 Ru1 149.4(3) . . ?
C41 Ru4 Ru1 101.3(3) . . ?
C42 Ru4 Ru1 106.2(3) . . ?
C1 Ru4 Ru1 49.78(17) . . ?
C43 Ru4 Ru5 99.1(3) . . ?
C41 Ru4 Ru5 159.4(3) . . ?
C42 Ru4 Ru5 96.3(2) . . ?
C1 Ru4 Ru5 43.56(16) . . ?
Ru1 Ru4 Ru5 58.307(19) . . ?
C43 Ru4 Ru3 98.2(3) . . ?
C41 Ru4 Ru3 78.8(3) . . ?
C42 Ru4 Ru3 164.4(3) . . ?
C1 Ru4 Ru3 44.58(17) . . ?
Ru1 Ru4 Ru3 63.539(17) . . ?
Ru5 Ru4 Ru3 88.04(2) . . ?
C51 Ru5 C52 94.1(4) . . ?
C51 Ru5 C53 98.1(4) . . ?
C52 Ru5 C53 92.7(3) . . ?
C51 Ru5 C1 102.9(3) . . ?
C52 Ru5 C1 129.6(3) . . ?
C53 Ru5 C1 130.1(3) . . ?
C51 Ru5 Ru1 153.1(2) . . ?
C52 Ru5 Ru1 104.0(3) . . ?
C53 Ru5 Ru1 100.6(3) . . ?
C1 Ru5 Ru1 50.24(17) . . ?
C51 Ru5 Ru4 103.1(3) . . ?
C52 Ru5 Ru4 87.0(2) . . ?
C53 Ru5 Ru4 158.8(3) . . ?
C1 Ru5 Ru4 43.13(17) . . ?
Ru1 Ru5 Ru4 59.13(2) . . ?
C51 Ru5 Ru2 98.1(2) . . ?
C52 Ru5 Ru2 167.5(3) . . ?
C53 Ru5 Ru2 88.3(3) . . ?
C1 Ru5 Ru2 44.47(17) . . ?
Ru1 Ru5 Ru2 63.589(18) . . ?
Ru4 Ru5 Ru2 87.539(19) . . ?
C71 P1 C79 109.1(10) . . ?
C71 P1 C75 110.2(8) . . ?
C79 P1 C75 104.8(7) . . ?
C71 P1 Pt1 114.4(3) . . ?
C79 P1 Pt1 106.0(4) . . ?
C75 P1 Pt1 111.8(4) . . ?
Ru4 C1 Ru5 93.3(2) . . ?
Ru4 C1 Ru2 173.5(3) . . ?
Ru5 C1 Ru2 92.0(2) . . ?
Ru4 C1 Ru3 92.5(2) . . ?
Ru5 C1 Ru3 172.5(3) . . ?
Ru2 C1 Ru3 81.9(2) . . ?
Ru4 C1 Ru1 85.3(2) . . ?
Ru5 C1 Ru1 84.0(2) . . ?
Ru2 C1 Ru1 91.4(2) . . ?
Ru3 C1 Ru1 91.7(2) . . ?
C3 C2 C61 121.6(6) . . ?
C3 C2 Ru3 112.3(5) . . ?
C61 C2 Ru3 125.6(5) . . ?
C3 C2 Ru2 71.8(4) . . ?
C61 C2 Ru2 125.9(5) . . ?
Ru3 C2 Ru2 76.29(19) . . ?
C2 C3 Pt1 114.2(5) . . ?
C2 C3 Ru2 72.1(4) . . ?
Pt1 C3 Ru2 85.4(3) . . ?
C2 C3 H1 117(3) . . ?
Pt1 C3 H1 128(3) . . ?
Ru2 C3 H1 114(3) . . ?
O11 C11 Ru1 171.4(7) . . ?
O12 C12 Ru1 174.7(8) . . ?
O13 C13 Ru1 170.6(7) . . ?
O21 C21 Ru2 178.0(8) . . ?
O22 C22 Ru2 178.2(7) . . ?
O31 C31 Ru3 178.6(8) . . ?
O32 C32 Ru3 177.7(7) . . ?
O41 C41 Ru4 176.6(8) . . ?
O42 C42 Ru4 178.2(9) . . ?
O43 C43 Ru4 174.6(8) . . ?
O51 C51 Ru5 178.2(8) . . ?
O52 C52 Ru5 177.9(9) . . ?
O53 C53 Ru5 178.5(8) . . ?
C62 C61 C66 116.8(7) . . ?
C62 C61 C2 123.5(6) . . ?
C66 C61 C2 119.7(7) . . ?
C63 C62 C61 122.5(8) . . ?
C63 C62 H62 118.8 . . ?
C61 C62 H62 118.8 . . ?
C62 C63 C64 119.1(9) . . ?
C62 C63 H63 120.4 . . ?
C64 C63 H63 120.4 . . ?
C65 C64 C63 119.7(8) . . ?
C65 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C64 C65 C66 121.2(9) . . ?
C64 C65 H65 119.4 . . ?
C66 C65 H65 119.4 . . ?
C65 C66 C61 120.7(8) . . ?
C65 C66 H66 119.7 . . ?
C61 C66 H66 119.7 . . ?
C72 C71 C74 116.0(13) . . ?
C72 C71 P1 114.5(10) . . ?
C74 C71 P1 117.3(10) . . ?
C72 C71 C73 99.3(15) . . ?
C74 C71 C73 105.2(15) . . ?
P1 C71 C73 100.7(11) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 C77 113.3(11) . . ?
C76 C75 C78 101.3(13) . . ?
C77 C75 C78 104.9(11) . . ?
C76 C75 P1 114.6(9) . . ?
C77 C75 P1 116.4(9) . . ?
C78 C75 P1 104.0(8) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C75 C78 H78A 109.5 . . ?
C75 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C75 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C81 C79 C82 113.7(12) . . ?
C81 C79 P1 118.0(9) . . ?
C82 C79 P1 119.5(9) . . ?
C81 C79 C80 104.6(13) . . ?
C82 C79 C80 100.7(12) . . ?
P1 C79 C80 94.8(10) . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C79 C81 H81A 109.5 . . ?
C79 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C79 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C79 C82 H82A 109.5 . . ?
C79 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C79 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C91 C90 H90A 109.5 . . ?
C91 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C91 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C90 C91 C92 89.3(17) . . ?
C90 C91 H91A 113.8 . . ?
C92 C91 H91A 113.8 . . ?
C90 C91 H91B 113.8 . . ?
C92 C91 H91B 113.8 . . ?
H91A C91 H91B 111.0 . . ?
C93 C92 C91 104(2) . . ?
C93 C92 H92A 111.0 . . ?
C91 C92 H92A 111.0 . . ?
C93 C92 H92B 111.0 . . ?
C91 C92 H92B 111.0 . . ?
H92A C92 H92B 109.0 . . ?
C92 C93 C93 134(4) . 2_656 ?
C92 C93 H93A 103.7 . . ?
C93 C93 H93A 103.7 2_656 . ?
C92 C93 H93B 103.7 . . ?
C93 C93 H93B 103.7 2_656 . ?
H93A C93 H93B 105.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C3 1.980(7) . ?
Pt1 P1 2.3122(19) . ?
Pt1 Ru1 2.6787(6) . ?
Pt1 Ru2 2.8476(6) . ?
Pt1 Ru3 2.9979(5) . ?
Ru1 C12 1.907(7) . ?
Ru1 C13 1.920(8) . ?
Ru1 C11 1.938(8) . ?
Ru1 C1 2.141(6) . ?
Ru1 Ru5 2.7705(8) . ?
Ru1 Ru4 2.7949(8) . ?
Ru1 Ru2 2.9856(7) . ?
Ru1 Ru3 3.0018(7) . ?
Ru2 C22 1.865(7) . ?
Ru2 C21 1.930(8) . ?
Ru2 C1 2.027(6) . ?
Ru2 C3 2.210(7) . ?
Ru2 C2 2.214(6) . ?
Ru2 Ru3 2.6666(7) . ?
Ru2 Ru5 2.8926(7) . ?
Ru3 C32 1.847(7) . ?
Ru3 C31 1.896(8) . ?
Ru3 C1 2.040(6) . ?
Ru3 C2 2.101(6) . ?
Ru3 Ru4 2.9037(7) . ?
Ru4 C43 1.903(9) . ?
Ru4 C41 1.905(10) . ?
Ru4 C42 1.931(8) . ?
Ru4 C1 1.979(6) . ?
Ru4 Ru5 2.8898(8) . ?
Ru5 C51 1.901(8) . ?
Ru5 C52 1.907(8) . ?
Ru5 C53 1.919(9) . ?
Ru5 C1 1.995(6) . ?
P1 C71 1.861(11) . ?
P1 C79 1.870(11) . ?
P1 C75 1.913(11) . ?
O11 C11 1.136(9) . ?
O12 C12 1.141(9) . ?
O13 C13 1.134(9) . ?
O21 C21 1.129(9) . ?
O22 C22 1.131(9) . ?
O31 C31 1.135(9) . ?
O32 C32 1.139(9) . ?
O41 C41 1.125(10) . ?
O42 C42 1.132(9) . ?
O43 C43 1.132(10) . ?
O51 C51 1.124(10) . ?
O52 C52 1.142(9) . ?
O53 C53 1.133(10) . ?
C2 C3 1.369(10) . ?
C2 C61 1.494(8) . ?
C3 H1 1.11(6) . ?
C61 C62 1.386(10) . ?
C61 C66 1.391(10) . ?
C62 C63 1.378(10) . ?
C62 H62 0.9300 . ?
C63 C64 1.384(14) . ?
C63 H63 0.9300 . ?
C64 C65 1.350(14) . ?
C64 H64 0.9300 . ?
C65 C66 1.384(11) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C71 C72 1.437(16) . ?
C71 C74 1.512(16) . ?
C71 C73 1.89(3) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 C76 1.440(18) . ?
C75 C77 1.537(14) . ?
C75 C78 1.664(18) . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C79 C81 1.372(18) . ?
C79 C82 1.503(14) . ?
C79 C80 1.94(3) . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C81 H81A 0.9600 . ?
C81 H81B 0.9600 . ?
C81 H81C 0.9600 . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C90 C91 1.499(18) . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
C91 C92 1.541(18) . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C92 C93 1.488(18) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C93 C93 1.50(4) 2_656 ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
|
1100874.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 20:40:01 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180566 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100874.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100874
loop_
_publ_author_name
'Adams, Richard D.'
'Captain, Burjor'
'Zhu, Lei'
_publ_section_title
;
New High Nuclearity Platinum--Ruthenium Carbonyl Cluster Complexes
Containing a Phenylacetylene Ligand: Structures and Properties
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2419
_journal_page_last 2423
_journal_paper_doi 10.1021/om050175n
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C52 H74 O13 P2 Pt2 Ru5'
_chemical_formula_weight 1864.58
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 126.0050(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 39.0570(13)
_cell_length_b 18.0757(6)
_cell_length_c 22.9961(7)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 13133.4(7)
_computing_cell_refinement 'SAINT+ V6.2 (Bruker, 2001)'
_computing_data_collection 'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction 'SAINT+ V6.2'
_computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material 'SHELXTL V6.1'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0565
_diffrn_reflns_av_sigmaI/netI 0.0594
_diffrn_reflns_limit_h_max 39
_diffrn_reflns_limit_h_min -46
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 38947
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 1.29
_diffrn_standards_decay_% <1
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 5.463
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.340
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS, Bruker, 1997)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.886
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 7168
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.02
_refine_diff_density_max 1.973
_refine_diff_density_min -1.355
_refine_diff_density_rms 0.588
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.095
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 655
_refine_ls_number_reflns 11613
_refine_ls_number_restraints 9
_refine_ls_restrained_S_all 1.098
_refine_ls_R_factor_all 0.0731
_refine_ls_R_factor_gt 0.0509
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+7.0392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1155
_refine_ls_wR_factor_ref 0.1240
_reflns_number_gt 8843
_reflns_number_total 11613
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om050175nsi20050310_030517.cif
_cod_data_source_block ru5ptpps
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100874
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.183705(12) 0.34982(2) 0.775939(19) 0.03740(11) Uani 1 1 d . . .
Pt2 Pt 0.323604(13) 0.38279(2) 0.69285(2) 0.04282(12) Uani 1 1 d . . .
Ru1 Ru 0.24209(3) 0.41029(4) 0.64686(4) 0.03723(19) Uani 1 1 d . . .
Ru2 Ru 0.29073(3) 0.28806(4) 0.74546(4) 0.0392(2) Uani 1 1 d . . .
Ru3 Ru 0.21334(2) 0.24178(4) 0.72370(4) 0.03414(19) Uani 1 1 d . . .
Ru4 Ru 0.16832(2) 0.35190(4) 0.63173(4) 0.03423(19) Uani 1 1 d . . .
Ru5 Ru 0.24901(2) 0.39117(4) 0.77503(4) 0.03696(19) Uani 1 1 d . . .
P1 P 0.14380(9) 0.36994(15) 0.81915(14) 0.0439(7) Uani 1 1 d . . .
P2 P 0.37484(9) 0.40387(17) 0.67399(16) 0.0511(7) Uani 1 1 d . . .
O11 O 0.1804(3) 0.5379(4) 0.5760(4) 0.062(2) Uani 1 1 d . . .
O12 O 0.2224(3) 0.3478(5) 0.5084(4) 0.080(3) Uani 1 1 d . . .
O13 O 0.3072(3) 0.5370(5) 0.7100(5) 0.083(3) Uani 1 1 d . . .
O21 O 0.3834(3) 0.3363(5) 0.8406(4) 0.080(3) Uani 1 1 d . . .
O22 O 0.2878(3) 0.1746(5) 0.6460(5) 0.094(3) Uani 1 1 d . . .
O23 O 0.3355(3) 0.1952(6) 0.8810(5) 0.103(4) Uani 1 1 d . . .
O31 O 0.2090(3) 0.1061(4) 0.6436(4) 0.065(2) Uani 1 1 d . . .
O32 O 0.2529(3) 0.1586(4) 0.8645(4) 0.064(2) Uani 1 1 d . . .
O41 O 0.1284(3) 0.3203(5) 0.4773(4) 0.080(3) Uani 1 1 d . . .
O42 O 0.1064(3) 0.4763(5) 0.5908(5) 0.088(3) Uani 1 1 d . . .
O51 O 0.3358(3) 0.4621(6) 0.8580(5) 0.096(3) Uani 1 1 d . . .
O52 O 0.2039(3) 0.5408(4) 0.7393(4) 0.069(2) Uani 1 1 d . . .
O53 O 0.2808(3) 0.3375(5) 0.9253(4) 0.082(3) Uani 1 1 d . . .
C1 C 0.2306(3) 0.3227(5) 0.6851(5) 0.033(2) Uani 1 1 d . . .
C2 C 0.1580(3) 0.2565(5) 0.7228(5) 0.040(2) Uani 1 1 d . . .
H2 H 0.1482 0.2181 0.7399 0.047 Uiso 1 1 calc . . .
C3 C 0.1434(3) 0.2612(5) 0.6512(5) 0.032(2) Uani 1 1 d . . .
C4 C 0.1109(3) 0.2076(6) 0.5966(5) 0.045(2) Uani 1 1 d . . .
C5 C 0.1125(3) 0.1333(6) 0.6107(6) 0.049(3) Uani 1 1 d . . .
H5 H 0.1348 0.1155 0.6553 0.059 Uiso 1 1 calc R . .
C6 C 0.0823(4) 0.0844(7) 0.5615(6) 0.063(3) Uani 1 1 d . . .
H6 H 0.0852 0.0340 0.5714 0.076 Uiso 1 1 calc R . .
C7 C 0.0471(4) 0.1117(8) 0.4958(6) 0.079(4) Uani 1 1 d . . .
H7 H 0.0254 0.0800 0.4629 0.095 Uiso 1 1 calc R . .
C8 C 0.0449(4) 0.1866(7) 0.4808(6) 0.066(3) Uani 1 1 d . . .
H8 H 0.0225 0.2051 0.4366 0.080 Uiso 1 1 calc R . .
C9 C 0.0764(3) 0.2336(6) 0.5320(6) 0.058(3) Uani 1 1 d . . .
H9 H 0.0742 0.2840 0.5224 0.070 Uiso 1 1 calc R . .
C11 C 0.2019(3) 0.4887(6) 0.6023(5) 0.043(2) Uani 1 1 d . . .
C12 C 0.2313(3) 0.3739(6) 0.5598(6) 0.049(3) Uani 1 1 d . . .
C13 C 0.2918(3) 0.4794(6) 0.6854(6) 0.057(3) Uani 1 1 d . . .
C21 C 0.3493(4) 0.3315(6) 0.7874(6) 0.050(3) Uani 1 1 d . . .
C22 C 0.2906(4) 0.2174(6) 0.6851(6) 0.056(3) Uani 1 1 d . . .
C23 C 0.3183(4) 0.2284(7) 0.8307(7) 0.060(3) Uani 1 1 d . . .
C31 C 0.2106(3) 0.1569(5) 0.6747(5) 0.042(2) Uani 1 1 d . . .
C32 C 0.2385(3) 0.1871(5) 0.8104(5) 0.045(3) Uani 1 1 d . . .
C41 C 0.1436(4) 0.3315(6) 0.5364(6) 0.053(3) Uani 1 1 d . . .
C42 C 0.1292(3) 0.4293(6) 0.6056(5) 0.048(3) Uani 1 1 d . . .
C51 C 0.3033(4) 0.4342(7) 0.8235(6) 0.062(3) Uani 1 1 d . . .
C52 C 0.2185(3) 0.4830(6) 0.7520(5) 0.048(3) Uani 1 1 d . . .
C53 C 0.2634(4) 0.3547(6) 0.8658(6) 0.058(3) Uani 1 1 d . . .
C60 C 0.1622(4) 0.3107(6) 0.8993(5) 0.054(3) Uani 1 1 d . . .
C61 C 0.1703(5) 0.2308(7) 0.8854(7) 0.077(4) Uani 1 1 d . . .
H61A H 0.1791 0.2003 0.9262 0.115 Uiso 1 1 calc R . .
H61B H 0.1920 0.2315 0.8780 0.115 Uiso 1 1 calc R . .
H61C H 0.1447 0.2113 0.8434 0.115 Uiso 1 1 calc R . .
C62 C 0.1336(5) 0.3072(8) 0.9241(7) 0.087(5) Uani 1 1 d . . .
H62A H 0.1072 0.2846 0.8874 0.131 Uiso 1 1 calc R . .
H62B H 0.1285 0.3564 0.9332 0.131 Uiso 1 1 calc R . .
H62C H 0.1471 0.2785 0.9674 0.131 Uiso 1 1 calc R . .
C63 C 0.2068(4) 0.3372(7) 0.9655(5) 0.068(4) Uani 1 1 d . . .
H63A H 0.2180 0.3018 1.0038 0.102 Uiso 1 1 calc R . .
H63B H 0.2040 0.3844 0.9816 0.102 Uiso 1 1 calc R . .
H63C H 0.2256 0.3417 0.9517 0.102 Uiso 1 1 calc R . .
C64 C 0.0846(4) 0.3523(7) 0.7491(6) 0.059(3) Uani 1 1 d . . .
C65 C 0.0722(4) 0.3780(7) 0.6752(6) 0.069(4) Uani 1 1 d . . .
H65A H 0.0882 0.3508 0.6629 0.103 Uiso 1 1 calc R . .
H65B H 0.0781 0.4299 0.6771 0.103 Uiso 1 1 calc R . .
H65C H 0.0425 0.3695 0.6394 0.103 Uiso 1 1 calc R . .
C66 C 0.0742(4) 0.2709(7) 0.7393(7) 0.073(4) Uani 1 1 d . . .
H66A H 0.0813 0.2504 0.7837 0.110 Uiso 1 1 calc R . .
H66B H 0.0901 0.2462 0.7255 0.110 Uiso 1 1 calc R . .
H66C H 0.0445 0.2642 0.7026 0.110 Uiso 1 1 calc R . .
C67 C 0.0557(4) 0.3896(8) 0.7642(7) 0.087(4) Uani 1 1 d . . .
H67A H 0.0286 0.3657 0.7370 0.130 Uiso 1 1 calc R . .
H67B H 0.0523 0.4408 0.7506 0.130 Uiso 1 1 calc R . .
H67C H 0.0680 0.3860 0.8145 0.130 Uiso 1 1 calc R . .
C68 C 0.1517(4) 0.4720(6) 0.8470(6) 0.051(3) Uani 1 1 d . . .
C69 C 0.1282(4) 0.5195(7) 0.7796(6) 0.071(4) Uani 1 1 d . . .
H69A H 0.1351 0.5706 0.7927 0.106 Uiso 1 1 calc R . .
H69B H 0.0983 0.5125 0.7542 0.106 Uiso 1 1 calc R . .
H69C H 0.1365 0.5054 0.7492 0.106 Uiso 1 1 calc R . .
C70 C 0.1982(4) 0.4906(6) 0.8880(6) 0.061(3) Uani 1 1 d . . .
H70A H 0.2081 0.4767 0.8600 0.092 Uiso 1 1 calc R . .
H70B H 0.2138 0.4641 0.9327 0.092 Uiso 1 1 calc R . .
H70C H 0.2021 0.5428 0.8973 0.092 Uiso 1 1 calc R . .
C71 C 0.1373(4) 0.4915(7) 0.8940(6) 0.076(4) Uani 1 1 d . . .
H71A H 0.1514 0.4600 0.9356 0.114 Uiso 1 1 calc R . .
H71B H 0.1072 0.4845 0.8671 0.114 Uiso 1 1 calc R . .
H71C H 0.1441 0.5422 0.9090 0.114 Uiso 1 1 calc R . .
C72 C 0.4083(4) 0.3161(7) 0.6964(7) 0.063(3) Uani 1 1 d . . .
C73 C 0.4313(5) 0.3116(8) 0.6609(8) 0.092(5) Uani 1 1 d . . .
H73A H 0.4472 0.2664 0.6749 0.137 Uiso 1 1 calc R . .
H73B H 0.4501 0.3529 0.6759 0.137 Uiso 1 1 calc R . .
H73C H 0.4109 0.3126 0.6096 0.137 Uiso 1 1 calc R . .
C74 C 0.3797(5) 0.2497(7) 0.6741(9) 0.092(5) Uani 1 1 d . . .
H74A H 0.3589 0.2501 0.6228 0.138 Uiso 1 1 calc R . .
H74B H 0.3657 0.2514 0.6971 0.138 Uiso 1 1 calc R . .
H74C H 0.3962 0.2053 0.6880 0.138 Uiso 1 1 calc R . .
C75 C 0.4427(4) 0.3098(8) 0.7786(7) 0.087(4) Uani 1 1 d . . .
H75A H 0.4298 0.3156 0.8033 0.131 Uiso 1 1 calc R . .
H75B H 0.4635 0.3477 0.7938 0.131 Uiso 1 1 calc R . .
H75C H 0.4560 0.2621 0.7895 0.131 Uiso 1 1 calc R . .
C76 C 0.4121(4) 0.4848(7) 0.7294(8) 0.076(4) Uani 1 1 d . . .
C77 C 0.3907(6) 0.5574(8) 0.7014(11) 0.136(8) Uani 1 1 d . . .
H77A H 0.3663 0.5592 0.7021 0.204 Uiso 1 1 calc R . .
H77B H 0.3819 0.5637 0.6529 0.204 Uiso 1 1 calc R . .
H77C H 0.4099 0.5963 0.7310 0.204 Uiso 1 1 calc R . .
C78 C 0.4524(4) 0.4861(8) 0.7338(7) 0.085(4) Uani 1 1 d . . .
H78A H 0.4464 0.4694 0.6890 0.127 Uiso 1 1 calc R . .
H78B H 0.4730 0.4540 0.7718 0.127 Uiso 1 1 calc R . .
H78C H 0.4633 0.5356 0.7433 0.127 Uiso 1 1 calc R . .
C79 C 0.4213(5) 0.4802(9) 0.8034(8) 0.102(5) Uani 1 1 d . . .
H79A H 0.4351 0.5248 0.8296 0.153 Uiso 1 1 calc R . .
H79B H 0.4395 0.4387 0.8290 0.153 Uiso 1 1 calc R . .
H79C H 0.3953 0.4741 0.7984 0.153 Uiso 1 1 calc R . .
C80 C 0.3464(4) 0.4242(11) 0.5741(8) 0.095(5) Uani 1 1 d . . .
C81 C 0.3735(5) 0.4529(12) 0.5511(9) 0.132(8) Uani 1 1 d . . .
H81A H 0.3571 0.4533 0.4996 0.199 Uiso 1 1 calc R . .
H81B H 0.3976 0.4212 0.5701 0.199 Uiso 1 1 calc R . .
H81C H 0.3829 0.5022 0.5691 0.199 Uiso 1 1 calc R . .
C82 C 0.3106(5) 0.4774(10) 0.5479(9) 0.125(7) Uani 1 1 d . . .
H82A H 0.2984 0.4905 0.4989 0.188 Uiso 1 1 calc R . .
H82B H 0.3210 0.5211 0.5772 0.188 Uiso 1 1 calc R . .
H82C H 0.2894 0.4546 0.5508 0.188 Uiso 1 1 calc R . .
C83 C 0.3229(6) 0.3515(11) 0.5321(8) 0.124(7) Uani 1 1 d . . .
H83A H 0.3079 0.3317 0.5498 0.186 Uiso 1 1 calc R . .
H83B H 0.3433 0.3159 0.5391 0.186 Uiso 1 1 calc R . .
H83C H 0.3033 0.3624 0.4818 0.186 Uiso 1 1 calc R . .
C1S C 0.0120(8) 0.5992(14) 0.6045(14) 0.224(13) Uiso 1 1 d D . .
H1S1 H 0.0394 0.5969 0.6498 0.335 Uiso 1 1 calc R . .
H1S2 H -0.0046 0.5575 0.6002 0.335 Uiso 1 1 calc R . .
H1S3 H -0.0020 0.6441 0.6020 0.335 Uiso 1 1 calc R . .
C2S C 0.0167(11) 0.5977(12) 0.5450(14) 0.32(2) Uiso 1 1 d D . .
H2S1 H 0.0257 0.5487 0.5420 0.380 Uiso 1 1 calc R . .
H2S2 H -0.0105 0.6077 0.5000 0.380 Uiso 1 1 calc R . .
C3S C 0.0476(7) 0.652(2) 0.5552(14) 0.34(2) Uiso 1 1 d D . .
H3S1 H 0.0689 0.6276 0.5530 0.403 Uiso 1 1 calc R . .
H3S2 H 0.0617 0.6749 0.6022 0.403 Uiso 1 1 calc R . .
C4S C 0.0261(8) 0.7100(16) 0.499(2) 0.40(3) Uiso 1 1 d D . .
H4S1 H 0.0003 0.6898 0.4562 0.477 Uiso 1 1 calc R . .
H4S2 H 0.0184 0.7512 0.5157 0.477 Uiso 1 1 calc R . .
C5S C 0.0541(10) 0.7362(15) 0.4795(18) 0.293(18) Uiso 1 1 d D . .
H5S1 H 0.0511 0.7045 0.4428 0.351 Uiso 1 1 calc R . .
H5S2 H 0.0833 0.7344 0.5215 0.351 Uiso 1 1 calc R . .
C6S C 0.0421(11) 0.8145(14) 0.4521(19) 0.33(2) Uiso 1 1 d D . .
H6S1 H 0.0664 0.8396 0.4607 0.488 Uiso 1 1 calc R . .
H6S2 H 0.0325 0.8398 0.4767 0.488 Uiso 1 1 calc R . .
H6S3 H 0.0199 0.8138 0.4014 0.488 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0413(2) 0.0426(2) 0.0309(2) -0.00356(16) 0.02270(18) -0.00306(17)
Pt2 0.0410(2) 0.0467(2) 0.0457(2) 0.00101(18) 0.0283(2) 0.00185(17)
Ru1 0.0396(5) 0.0387(4) 0.0377(4) 0.0056(3) 0.0251(4) 0.0035(3)
Ru2 0.0400(5) 0.0400(4) 0.0386(4) 0.0049(3) 0.0237(4) 0.0064(3)
Ru3 0.0397(5) 0.0328(4) 0.0290(4) 0.0008(3) 0.0196(4) 0.0002(3)
Ru4 0.0360(4) 0.0369(4) 0.0288(4) 0.0018(3) 0.0185(3) 0.0028(3)
Ru5 0.0407(5) 0.0377(4) 0.0344(4) -0.0051(3) 0.0232(4) -0.0036(3)
P1 0.0479(17) 0.0534(17) 0.0363(14) -0.0026(12) 0.0279(13) 0.0000(12)
P2 0.0452(17) 0.0595(18) 0.0542(17) 0.0033(14) 0.0323(15) 0.0012(13)
O11 0.066(6) 0.055(5) 0.066(5) 0.020(4) 0.038(4) 0.017(4)
O12 0.099(8) 0.102(7) 0.057(5) -0.012(5) 0.055(5) -0.004(5)
O13 0.063(6) 0.052(5) 0.129(8) -0.006(5) 0.055(6) 0.000(4)
O21 0.051(6) 0.131(8) 0.045(5) 0.005(5) 0.021(4) -0.007(5)
O22 0.110(8) 0.074(6) 0.123(8) -0.043(6) 0.083(7) -0.005(5)
O23 0.075(7) 0.117(8) 0.089(7) 0.062(6) 0.031(6) 0.014(6)
O31 0.090(7) 0.045(5) 0.064(5) -0.014(4) 0.047(5) -0.002(4)
O32 0.074(6) 0.055(5) 0.043(4) 0.007(4) 0.023(4) 0.002(4)
O41 0.085(7) 0.117(8) 0.038(5) -0.007(5) 0.036(5) -0.007(5)
O42 0.085(7) 0.072(6) 0.107(7) 0.028(5) 0.056(6) 0.041(5)
O51 0.064(7) 0.115(8) 0.118(8) -0.058(7) 0.058(6) -0.036(6)
O52 0.095(7) 0.049(5) 0.063(5) 0.003(4) 0.046(5) 0.018(4)
O53 0.091(7) 0.095(7) 0.040(5) 0.011(4) 0.028(5) -0.001(5)
C1 0.033(5) 0.030(5) 0.036(5) 0.000(4) 0.021(4) 0.001(4)
C2 0.046(6) 0.033(5) 0.033(5) -0.003(4) 0.020(5) 0.000(4)
C3 0.034(5) 0.032(5) 0.033(5) -0.003(4) 0.021(4) -0.004(4)
C4 0.042(6) 0.055(7) 0.043(6) -0.004(5) 0.027(5) -0.003(5)
C5 0.055(7) 0.046(6) 0.045(6) -0.003(5) 0.029(6) -0.010(5)
C6 0.072(9) 0.055(7) 0.059(7) -0.006(6) 0.036(7) -0.018(6)
C7 0.060(9) 0.117(12) 0.040(7) -0.031(7) 0.018(6) -0.032(8)
C8 0.061(8) 0.057(8) 0.056(7) 0.003(6) 0.020(6) -0.003(6)
C9 0.044(7) 0.057(7) 0.052(7) 0.001(6) 0.016(6) -0.003(5)
C11 0.046(6) 0.041(6) 0.046(6) 0.006(5) 0.030(5) 0.008(5)
C12 0.051(7) 0.061(7) 0.042(6) 0.010(5) 0.030(6) 0.013(5)
C13 0.044(7) 0.040(6) 0.078(8) -0.003(6) 0.031(6) 0.001(5)
C21 0.045(7) 0.056(7) 0.052(7) 0.006(5) 0.030(6) 0.001(5)
C22 0.057(8) 0.045(7) 0.077(8) -0.005(6) 0.046(7) -0.003(5)
C23 0.050(7) 0.059(7) 0.074(8) 0.016(6) 0.038(7) 0.009(6)
C31 0.049(6) 0.039(6) 0.034(5) 0.006(4) 0.022(5) -0.001(5)
C32 0.052(7) 0.042(6) 0.029(5) 0.002(5) 0.017(5) 0.001(5)
C41 0.053(7) 0.065(7) 0.040(6) -0.002(5) 0.026(6) 0.001(5)
C42 0.043(7) 0.051(7) 0.045(6) 0.009(5) 0.023(5) 0.002(5)
C51 0.062(8) 0.081(9) 0.064(7) -0.038(7) 0.048(7) -0.024(7)
C52 0.060(7) 0.039(6) 0.046(6) -0.012(5) 0.033(6) -0.007(5)
C53 0.081(9) 0.042(6) 0.049(7) -0.006(5) 0.038(7) -0.002(6)
C60 0.066(8) 0.064(7) 0.045(6) 0.002(5) 0.040(6) -0.003(6)
C61 0.110(12) 0.071(9) 0.070(8) 0.005(7) 0.063(9) -0.006(8)
C62 0.106(12) 0.121(12) 0.071(8) -0.007(8) 0.071(9) -0.018(9)
C63 0.080(10) 0.075(9) 0.037(6) 0.006(6) 0.029(6) 0.000(7)
C64 0.046(7) 0.090(9) 0.050(6) 0.008(6) 0.032(6) 0.004(6)
C65 0.042(7) 0.106(10) 0.044(6) -0.005(6) 0.018(6) 0.005(6)
C66 0.060(8) 0.088(10) 0.076(9) -0.023(7) 0.042(7) -0.024(7)
C67 0.058(9) 0.132(13) 0.088(10) 0.006(9) 0.053(8) 0.014(8)
C68 0.059(8) 0.058(7) 0.048(6) -0.006(5) 0.039(6) -0.006(5)
C69 0.081(10) 0.073(8) 0.071(8) -0.006(7) 0.052(8) 0.004(7)
C70 0.080(9) 0.054(7) 0.053(7) -0.013(6) 0.040(7) -0.007(6)
C71 0.083(10) 0.088(10) 0.064(8) -0.019(7) 0.047(8) 0.005(7)
C72 0.062(8) 0.071(8) 0.071(8) -0.013(6) 0.047(7) 0.001(6)
C73 0.091(11) 0.090(11) 0.131(13) -0.031(9) 0.085(10) -0.013(8)
C74 0.098(12) 0.062(9) 0.151(14) -0.011(9) 0.093(11) 0.006(8)
C75 0.067(10) 0.117(12) 0.073(9) 0.007(8) 0.039(8) 0.025(8)
C76 0.063(9) 0.059(8) 0.116(12) -0.001(8) 0.057(9) 0.003(6)
C77 0.139(17) 0.080(12) 0.26(2) 0.013(14) 0.157(18) 0.012(11)
C78 0.051(8) 0.106(11) 0.107(11) -0.016(9) 0.052(8) -0.016(7)
C79 0.092(12) 0.130(14) 0.099(11) -0.060(10) 0.065(10) -0.049(10)
C80 0.059(9) 0.168(16) 0.073(9) 0.060(10) 0.046(8) 0.022(10)
C81 0.073(12) 0.24(2) 0.097(12) 0.049(13) 0.056(10) 0.014(13)
C82 0.075(11) 0.173(17) 0.129(14) 0.108(13) 0.060(10) 0.041(11)
C83 0.099(14) 0.20(2) 0.065(10) -0.013(12) 0.044(10) -0.021(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pt1 P1 100.0(3) . . ?
C2 Pt1 C53 118.0(4) . . ?
P1 Pt1 C53 117.3(3) . . ?
C2 Pt1 Ru5 112.0(3) . . ?
P1 Pt1 Ru5 147.78(7) . . ?
C53 Pt1 Ru5 43.5(3) . . ?
C2 Pt1 Ru3 49.0(3) . . ?
P1 Pt1 Ru3 145.58(7) . . ?
C53 Pt1 Ru3 76.1(2) . . ?
Ru5 Pt1 Ru3 64.21(2) . . ?
C2 Pt1 Ru4 68.2(3) . . ?
P1 Pt1 Ru4 136.32(7) . . ?
C53 Pt1 Ru4 104.7(3) . . ?
Ru5 Pt1 Ru4 63.88(2) . . ?
Ru3 Pt1 Ru4 54.14(2) . . ?
C21 Pt2 C13 111.7(5) . . ?
C21 Pt2 P2 110.0(3) . . ?
C13 Pt2 P2 112.6(3) . . ?
C21 Pt2 Ru1 103.3(3) . . ?
C13 Pt2 Ru1 47.1(3) . . ?
P2 Pt2 Ru1 146.32(8) . . ?
C21 Pt2 Ru2 46.8(3) . . ?
C13 Pt2 Ru2 98.3(3) . . ?
P2 Pt2 Ru2 147.83(8) . . ?
Ru1 Pt2 Ru2 63.62(2) . . ?
C12 Ru1 C11 95.1(4) . . ?
C12 Ru1 C1 102.8(4) . . ?
C11 Ru1 C1 120.2(4) . . ?
C12 Ru1 C13 103.6(5) . . ?
C11 Ru1 C13 92.9(4) . . ?
C1 Ru1 C13 135.0(4) . . ?
C12 Ru1 Pt2 80.3(3) . . ?
C11 Ru1 Pt2 138.0(3) . . ?
C1 Ru1 Pt2 101.4(3) . . ?
C13 Ru1 Pt2 49.2(3) . . ?
C12 Ru1 Ru5 152.0(3) . . ?
C11 Ru1 Ru5 101.3(3) . . ?
C1 Ru1 Ru5 49.3(2) . . ?
C13 Ru1 Ru5 98.1(4) . . ?
Pt2 Ru1 Ru5 101.43(3) . . ?
C12 Ru1 Ru4 99.2(3) . . ?
C11 Ru1 Ru4 76.1(3) . . ?
C1 Ru1 Ru4 45.1(3) . . ?
C13 Ru1 Ru4 155.5(3) . . ?
Pt2 Ru1 Ru4 145.89(3) . . ?
Ru5 Ru1 Ru4 63.72(3) . . ?
C12 Ru1 Ru2 101.2(3) . . ?
C11 Ru1 Ru2 158.8(3) . . ?
C1 Ru1 Ru2 42.9(3) . . ?
C13 Ru1 Ru2 96.2(3) . . ?
Pt2 Ru1 Ru2 59.17(2) . . ?
Ru5 Ru1 Ru2 58.51(3) . . ?
Ru4 Ru1 Ru2 87.98(3) . . ?
C22 Ru2 C23 97.4(5) . . ?
C22 Ru2 C1 102.0(4) . . ?
C23 Ru2 C1 127.6(4) . . ?
C22 Ru2 C21 97.2(5) . . ?
C23 Ru2 C21 86.2(5) . . ?
C1 Ru2 C21 137.6(4) . . ?
C22 Ru2 Pt2 84.3(3) . . ?
C23 Ru2 Pt2 131.2(4) . . ?
C1 Ru2 Pt2 99.1(3) . . ?
C21 Ru2 Pt2 45.6(3) . . ?
C22 Ru2 Ru5 151.3(4) . . ?
C23 Ru2 Ru5 100.5(4) . . ?
C1 Ru2 Ru5 49.4(2) . . ?
C21 Ru2 Ru5 106.1(3) . . ?
Pt2 Ru2 Ru5 100.19(3) . . ?
C22 Ru2 Ru3 97.3(3) . . ?
C23 Ru2 Ru3 85.2(4) . . ?
C1 Ru2 Ru3 44.5(3) . . ?
C21 Ru2 Ru3 163.9(3) . . ?
Pt2 Ru2 Ru3 143.26(3) . . ?
Ru5 Ru2 Ru3 62.38(3) . . ?
C22 Ru2 Ru1 102.8(4) . . ?
C23 Ru2 Ru1 159.1(4) . . ?
C1 Ru2 Ru1 42.5(3) . . ?
C21 Ru2 Ru1 96.4(3) . . ?
Pt2 Ru2 Ru1 57.21(2) . . ?
Ru5 Ru2 Ru1 58.81(3) . . ?
Ru3 Ru2 Ru1 87.01(3) . . ?
C31 Ru3 C32 91.0(4) . . ?
C31 Ru3 C1 104.1(4) . . ?
C32 Ru3 C1 137.4(4) . . ?
C31 Ru3 C2 113.1(4) . . ?
C32 Ru3 C2 88.4(4) . . ?
C1 Ru3 C2 119.7(3) . . ?
C31 Ru3 C3 93.9(4) . . ?
C32 Ru3 C3 121.0(4) . . ?
C1 Ru3 C3 97.8(3) . . ?
C2 Ru3 C3 36.8(3) . . ?
C31 Ru3 Ru4 110.8(3) . . ?
C32 Ru3 Ru4 155.6(3) . . ?
C1 Ru3 Ru4 49.3(2) . . ?
C2 Ru3 Ru4 73.3(2) . . ?
C3 Ru3 Ru4 49.3(2) . . ?
C31 Ru3 Pt1 156.5(3) . . ?
C32 Ru3 Pt1 90.1(3) . . ?
C1 Ru3 Pt1 90.7(2) . . ?
C2 Ru3 Pt1 43.5(2) . . ?
C3 Ru3 Pt1 65.7(2) . . ?
Ru4 Ru3 Pt1 65.48(2) . . ?
C31 Ru3 Ru2 91.4(3) . . ?
C32 Ru3 Ru2 97.2(3) . . ?
C1 Ru3 Ru2 43.9(2) . . ?
C2 Ru3 Ru2 154.8(2) . . ?
C3 Ru3 Ru2 141.3(2) . . ?
Ru4 Ru3 Ru2 93.21(3) . . ?
Pt1 Ru3 Ru2 111.70(3) . . ?
C31 Ru3 Ru5 147.0(3) . . ?
C32 Ru3 Ru5 103.0(3) . . ?
C1 Ru3 Ru5 46.5(2) . . ?
C2 Ru3 Ru5 97.2(2) . . ?
C3 Ru3 Ru5 103.7(2) . . ?
Ru4 Ru3 Ru5 64.61(3) . . ?
Pt1 Ru3 Ru5 54.62(2) . . ?
Ru2 Ru3 Ru5 57.59(3) . . ?
C41 Ru4 C42 90.6(5) . . ?
C41 Ru4 C1 105.5(4) . . ?
C42 Ru4 C1 146.6(4) . . ?
C41 Ru4 C3 96.6(4) . . ?
C42 Ru4 C3 104.9(4) . . ?
C1 Ru4 C3 102.1(3) . . ?
C41 Ru4 Ru3 115.7(3) . . ?
C42 Ru4 Ru3 146.6(3) . . ?
C1 Ru4 Ru3 48.5(2) . . ?
C3 Ru4 Ru3 54.4(2) . . ?
C41 Ru4 Ru1 90.2(4) . . ?
C42 Ru4 Ru1 109.3(3) . . ?
C1 Ru4 Ru1 43.3(2) . . ?
C3 Ru4 Ru1 145.0(2) . . ?
Ru3 Ru4 Ru1 91.79(3) . . ?
C41 Ru4 Pt1 159.7(4) . . ?
C42 Ru4 Pt1 87.7(3) . . ?
C1 Ru4 Pt1 86.5(2) . . ?
C3 Ru4 Pt1 64.4(2) . . ?
Ru3 Ru4 Pt1 60.37(2) . . ?
Ru1 Ru4 Pt1 109.47(3) . . ?
C41 Ru4 Ru5 145.9(4) . . ?
C42 Ru4 Ru5 107.7(3) . . ?
C1 Ru4 Ru5 45.2(2) . . ?
C3 Ru4 Ru5 105.7(2) . . ?
Ru3 Ru4 Ru5 62.09(3) . . ?
Ru1 Ru4 Ru5 56.96(3) . . ?
Pt1 Ru4 Ru5 52.68(2) . . ?
C51 Ru5 C52 96.1(5) . . ?
C51 Ru5 C53 89.4(5) . . ?
C52 Ru5 C53 109.3(5) . . ?
C51 Ru5 C1 115.6(4) . . ?
C52 Ru5 C1 115.5(4) . . ?
C53 Ru5 C1 124.5(4) . . ?
C51 Ru5 Pt1 149.0(3) . . ?
C52 Ru5 Pt1 78.7(3) . . ?
C53 Ru5 Pt1 64.4(4) . . ?
C1 Ru5 Pt1 93.8(2) . . ?
C51 Ru5 Ru2 78.9(4) . . ?
C52 Ru5 Ru2 149.1(3) . . ?
C53 Ru5 Ru2 101.2(3) . . ?
C1 Ru5 Ru2 45.2(2) . . ?
Pt1 Ru5 Ru2 120.58(3) . . ?
C51 Ru5 Ru1 87.2(3) . . ?
C52 Ru5 Ru1 86.7(3) . . ?
C53 Ru5 Ru1 163.8(3) . . ?
C1 Ru5 Ru1 44.7(2) . . ?
Pt1 Ru5 Ru1 122.53(3) . . ?
Ru2 Ru5 Ru1 62.68(3) . . ?
C51 Ru5 Ru3 135.7(4) . . ?
C52 Ru5 Ru3 127.5(3) . . ?
C53 Ru5 Ru3 83.6(3) . . ?
C1 Ru5 Ru3 43.3(2) . . ?
Pt1 Ru5 Ru3 61.17(2) . . ?
Ru2 Ru5 Ru3 60.02(3) . . ?
Ru1 Ru5 Ru3 87.79(3) . . ?
C51 Ru5 Ru4 146.3(4) . . ?
C52 Ru5 Ru4 79.8(3) . . ?
C53 Ru5 Ru4 123.7(4) . . ?
C1 Ru5 Ru4 42.8(2) . . ?
Pt1 Ru5 Ru4 63.44(2) . . ?
Ru2 Ru5 Ru4 87.80(3) . . ?
Ru1 Ru5 Ru4 59.31(3) . . ?
Ru3 Ru5 Ru4 53.29(2) . . ?
C60 P1 C64 107.9(5) . . ?
C60 P1 C68 109.2(5) . . ?
C64 P1 C68 108.6(5) . . ?
C60 P1 Pt1 111.5(4) . . ?
C64 P1 Pt1 113.4(4) . . ?
C68 P1 Pt1 106.1(3) . . ?
C80 P2 C72 107.8(7) . . ?
C80 P2 C76 109.2(7) . . ?
C72 P2 C76 108.7(6) . . ?
C80 P2 Pt2 107.5(4) . . ?
C72 P2 Pt2 109.9(4) . . ?
C76 P2 Pt2 113.7(4) . . ?
Ru1 C1 Ru2 94.5(4) . . ?
Ru1 C1 Ru3 172.5(5) . . ?
Ru2 C1 Ru3 91.6(3) . . ?
Ru1 C1 Ru4 91.6(3) . . ?
Ru2 C1 Ru4 173.2(5) . . ?
Ru3 C1 Ru4 82.1(3) . . ?
Ru1 C1 Ru5 86.1(3) . . ?
Ru2 C1 Ru5 85.4(3) . . ?
Ru3 C1 Ru5 90.1(3) . . ?
Ru4 C1 Ru5 92.0(4) . . ?
C3 C2 Pt1 112.7(7) . . ?
C3 C2 Ru3 74.4(6) . . ?
Pt1 C2 Ru3 87.6(4) . . ?
C2 C3 C4 120.5(8) . . ?
C2 C3 Ru4 112.5(6) . . ?
C4 C3 Ru4 126.9(6) . . ?
C2 C3 Ru3 68.8(5) . . ?
C4 C3 Ru3 125.8(6) . . ?
Ru4 C3 Ru3 76.3(3) . . ?
C9 C4 C5 117.9(10) . . ?
C9 C4 C3 119.6(9) . . ?
C5 C4 C3 122.3(9) . . ?
C6 C5 C4 122.5(10) . . ?
C5 C6 C7 118.9(11) . . ?
C8 C7 C6 119.2(11) . . ?
C9 C8 C7 119.6(11) . . ?
C4 C9 C8 121.7(11) . . ?
O11 C11 Ru1 174.8(10) . . ?
O12 C12 Ru1 173.3(11) . . ?
O13 C13 Ru1 148.4(10) . . ?
O13 C13 Pt2 126.2(9) . . ?
Ru1 C13 Pt2 83.7(4) . . ?
O21 C21 Pt2 129.6(9) . . ?
O21 C21 Ru2 142.5(9) . . ?
Pt2 C21 Ru2 87.6(4) . . ?
O22 C22 Ru2 175.6(11) . . ?
O23 C23 Ru2 177.7(12) . . ?
O31 C31 Ru3 178.4(9) . . ?
O32 C32 Ru3 174.8(9) . . ?
O41 C41 Ru4 178.7(11) . . ?
O42 C42 Ru4 178.8(12) . . ?
O51 C51 Ru5 173.6(10) . . ?
O52 C52 Ru5 173.1(10) . . ?
O53 C53 Ru5 164.9(11) . . ?
O53 C53 Pt1 122.9(10) . . ?
Ru5 C53 Pt1 72.1(4) . . ?
C62 C60 C61 108.7(10) . . ?
C62 C60 C63 106.8(9) . . ?
C61 C60 C63 104.0(10) . . ?
C62 C60 P1 116.7(9) . . ?
C61 C60 P1 109.7(7) . . ?
C63 C60 P1 110.2(8) . . ?
C66 C64 C67 107.3(11) . . ?
C66 C64 C65 104.4(10) . . ?
C67 C64 C65 108.9(10) . . ?
C66 C64 P1 112.0(8) . . ?
C67 C64 P1 115.2(9) . . ?
C65 C64 P1 108.5(8) . . ?
C70 C68 C69 107.1(9) . . ?
C70 C68 C71 108.4(9) . . ?
C69 C68 C71 109.9(10) . . ?
C70 C68 P1 108.7(8) . . ?
C69 C68 P1 108.7(7) . . ?
C71 C68 P1 113.9(8) . . ?
C74 C72 C73 109.0(11) . . ?
C74 C72 C75 107.1(12) . . ?
C73 C72 C75 106.7(11) . . ?
C74 C72 P2 108.4(9) . . ?
C73 C72 P2 114.9(10) . . ?
C75 C72 P2 110.6(8) . . ?
C77 C76 C78 108.3(12) . . ?
C77 C76 C79 103.7(13) . . ?
C78 C76 C79 111.8(12) . . ?
C77 C76 P2 111.8(11) . . ?
C78 C76 P2 114.0(9) . . ?
C79 C76 P2 106.8(9) . . ?
C82 C80 C81 108.4(13) . . ?
C82 C80 C83 102.7(14) . . ?
C81 C80 C83 110.1(15) . . ?
C82 C80 P2 110.7(11) . . ?
C81 C80 P2 116.8(11) . . ?
C83 C80 P2 107.2(10) . . ?
C3S C2S C1S 112.2(11) . . ?
C2S C3S C4S 110.1(10) . . ?
C5S C4S C3S 110.4(10) . . ?
C4S C5S C6S 108.9(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C2 1.976(9) . ?
Pt1 P1 2.317(3) . ?
Pt1 C53 2.531(13) . ?
Pt1 Ru5 2.6699(9) . ?
Pt1 Ru3 2.8689(8) . ?
Pt1 Ru4 3.0028(8) . ?
Pt2 C21 2.008(11) . ?
Pt2 C13 2.092(11) . ?
Pt2 P2 2.315(3) . ?
Pt2 Ru1 2.7465(9) . ?
Pt2 Ru2 2.8055(9) . ?
Ru1 C12 1.906(11) . ?
Ru1 C11 1.906(10) . ?
Ru1 C1 1.985(9) . ?
Ru1 C13 2.022(11) . ?
Ru1 Ru5 2.8181(11) . ?
Ru1 Ru4 2.8909(11) . ?
Ru1 Ru2 2.9270(11) . ?
Ru2 C22 1.884(12) . ?
Ru2 C23 1.919(12) . ?
Ru2 C1 1.999(9) . ?
Ru2 C21 2.047(11) . ?
Ru2 Ru5 2.8094(11) . ?
Ru2 Ru3 2.8824(12) . ?
Ru3 C31 1.870(10) . ?
Ru3 C32 1.900(10) . ?
Ru3 C1 2.023(9) . ?
Ru3 C2 2.166(10) . ?
Ru3 C3 2.238(9) . ?
Ru3 Ru4 2.6748(10) . ?
Ru3 Ru5 2.9484(11) . ?
Ru4 C41 1.840(11) . ?
Ru4 C42 1.890(11) . ?
Ru4 C1 2.048(9) . ?
Ru4 C3 2.086(9) . ?
Ru4 Ru5 3.0142(10) . ?
Ru5 C51 1.886(12) . ?
Ru5 C52 1.927(11) . ?
Ru5 C53 1.932(12) . ?
Ru5 C1 2.140(9) . ?
P1 C60 1.872(10) . ?
P1 C64 1.915(12) . ?
P1 C68 1.918(11) . ?
P2 C80 1.909(13) . ?
P2 C72 1.923(12) . ?
P2 C76 1.923(13) . ?
O11 C11 1.124(11) . ?
O12 C12 1.120(12) . ?
O13 C13 1.169(12) . ?
O21 C21 1.166(12) . ?
O22 C22 1.142(13) . ?
O23 C23 1.112(12) . ?
O31 C31 1.141(11) . ?
O32 C32 1.143(11) . ?
O41 C41 1.136(11) . ?
O42 C42 1.130(12) . ?
O51 C51 1.147(13) . ?
O52 C52 1.143(12) . ?
O53 C53 1.156(12) . ?
C2 C3 1.391(12) . ?
C3 C4 1.500(13) . ?
C4 C9 1.375(14) . ?
C4 C5 1.375(14) . ?
C5 C6 1.372(14) . ?
C6 C7 1.405(16) . ?
C7 C8 1.387(17) . ?
C8 C9 1.386(15) . ?
C60 C62 1.526(16) . ?
C60 C61 1.549(16) . ?
C60 C63 1.569(15) . ?
C64 C66 1.507(16) . ?
C64 C67 1.519(16) . ?
C64 C65 1.541(15) . ?
C68 C70 1.511(15) . ?
C68 C69 1.520(15) . ?
C68 C71 1.526(15) . ?
C72 C74 1.510(17) . ?
C72 C73 1.529(17) . ?
C72 C75 1.550(16) . ?
C76 C77 1.484(19) . ?
C76 C78 1.519(17) . ?
C76 C79 1.521(19) . ?
C80 C82 1.50(2) . ?
C80 C81 1.527(19) . ?
C80 C83 1.57(2) . ?
C1S C2S 1.484(10) . ?
C2S C3S 1.466(10) . ?
C3S C4S 1.487(10) . ?
C4S C5S 1.474(10) . ?
C5S C6S 1.507(10) . ?
|
1100875.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 20:40:01 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180566 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100875.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100875
loop_
_publ_author_name
'Adams, Richard D.'
'Captain, Burjor'
'Zhu, Lei'
_publ_section_title
;
New High Nuclearity Platinum--Ruthenium Carbonyl Cluster Complexes
Containing a Phenylacetylene Ligand: Structures and Properties
;
_journal_coden_ASTM ORGND7
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2419
_journal_page_last 2423
_journal_paper_doi 10.1021/om050175n
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C61 H90 O13 P3 Pt3 Ru5'
_chemical_formula_weight 2214.86
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 80.3400(10)
_cell_angle_beta 66.3240(10)
_cell_angle_gamma 71.6450(10)
_cell_formula_units_Z 2
_cell_length_a 14.7755(8)
_cell_length_b 16.3794(9)
_cell_length_c 17.3720(10)
_cell_measurement_reflns_used 6335
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.24
_cell_measurement_theta_min 2.30
_cell_volume 3650.4(4)
_computing_cell_refinement 'SAINT+ V6.2 (Bruker, 2001)'
_computing_data_collection 'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction 'SAINT+ V6.2'
_computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material 'SHELXTL V6.1'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0317
_diffrn_reflns_av_sigmaI/netI 0.0469
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 38713
_diffrn_reflns_theta_full 28.34
_diffrn_reflns_theta_max 28.34
_diffrn_reflns_theta_min 1.56
_diffrn_standards_decay_% <1
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 6.849
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.553
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details '(SADABS, Bruker, 1997)'
_exptl_crystal_colour DarkRed
_exptl_crystal_density_diffrn 2.015
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Rectangular
_exptl_crystal_F_000 2118
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_refine_diff_density_max 7.503
_refine_diff_density_min -2.375
_refine_diff_density_rms 0.210
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 778
_refine_ls_number_reflns 18034
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.019
_refine_ls_R_factor_all 0.0673
_refine_ls_R_factor_gt 0.0485
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+11.0362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1275
_refine_ls_wR_factor_ref 0.1401
_reflns_number_gt 13974
_reflns_number_total 18034
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file om050175nsi20050310_030557.cif
_cod_data_source_block ru5ptcos
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.31972(2) 0.025020(19) 0.258238(19) 0.04080(8) Uani 1 1 d . . .
Pt2 Pt 0.44640(2) 0.28122(2) 0.23944(2) 0.04504(9) Uani 1 1 d . . .
Pt3 Pt 0.06278(2) 0.449576(19) 0.240517(19) 0.03982(8) Uani 1 1 d . . .
Ru1 Ru 0.24781(4) 0.33156(4) 0.24081(4) 0.03647(13) Uani 1 1 d . . .
Ru2 Ru 0.04940(4) 0.28977(4) 0.31251(4) 0.04094(14) Uani 1 1 d . . .
Ru3 Ru 0.14372(4) 0.13539(4) 0.38917(4) 0.03662(13) Uani 1 1 d . . .
Ru4 Ru 0.32394(4) 0.17255(4) 0.32934(3) 0.03213(12) Uani 1 1 d . . .
Ru5 Ru 0.22926(5) 0.17832(4) 0.20444(4) 0.03858(14) Uani 1 1 d . . .
P1 P 0.38620(18) -0.12270(14) 0.23942(15) 0.0486(5) Uani 1 1 d . . .
P2 P 0.58747(19) 0.33173(17) 0.21016(18) 0.0574(6) Uani 1 1 d . . .
P3 P -0.03079(17) 0.59150(14) 0.22915(14) 0.0455(5) Uani 1 1 d . . .
O11 O 0.2318(7) 0.4449(5) 0.3690(5) 0.082(2) Uani 1 1 d . . .
O12 O 0.4346(5) 0.3158(5) 0.0734(4) 0.071(2) Uani 1 1 d . . .
O13 O 0.2423(5) 0.4610(5) 0.0911(5) 0.076(2) Uani 1 1 d . . .
O21 O -0.0604(10) 0.3889(7) 0.4721(6) 0.137(5) Uani 1 1 d . . .
O22 O -0.1089(6) 0.1909(6) 0.3608(7) 0.110(4) Uani 1 1 d . . .
O23 O -0.0425(6) 0.3665(5) 0.1768(5) 0.077(2) Uani 1 1 d . . .
O31 O 0.0054(6) 0.2016(5) 0.5599(4) 0.079(2) Uani 1 1 d . . .
O32 O 0.0275(6) 0.0064(6) 0.4041(6) 0.090(3) Uani 1 1 d . . .
O41 O 0.3228(7) 0.2612(5) 0.4677(5) 0.080(2) Uani 1 1 d . . .
O42 O 0.5562(5) 0.0971(5) 0.2347(5) 0.076(2) Uani 1 1 d . . .
O51 O 0.2122(8) 0.2911(5) 0.0510(5) 0.094(3) Uani 1 1 d . . .
O52 O 0.0858(7) 0.0818(6) 0.1999(6) 0.095(3) Uani 1 1 d . . .
O53 O 0.4546(6) 0.1047(5) 0.0921(4) 0.077(2) Uani 1 1 d . . .
C1 C 0.1892(5) 0.2400(5) 0.3169(4) 0.0356(15) Uani 1 1 d . . .
C2 C 0.3556(6) 0.0344(5) 0.3542(5) 0.0426(17) Uani 1 1 d . . .
H2 H 0.4201 -0.0007 0.3600 0.051 Uiso 1 1 calc . . .
C3 C 0.2700(5) 0.0712(5) 0.4226(5) 0.0381(15) Uani 1 1 d . . .
C4 C 0.2725(6) 0.0535(6) 0.5090(5) 0.0459(18) Uani 1 1 d . . .
C5 C 0.1930(8) 0.0285(7) 0.5744(6) 0.061(2) Uani 1 1 d . . .
H5 H 0.1380 0.0232 0.5643 0.073 Uiso 1 1 calc R . .
C6 C 0.1946(10) 0.0113(8) 0.6550(7) 0.078(3) Uani 1 1 d . . .
H6 H 0.1404 -0.0051 0.6986 0.094 Uiso 1 1 calc R . .
C7 C 0.2758(9) 0.0183(7) 0.6702(6) 0.071(3) Uani 1 1 d . . .
H7 H 0.2762 0.0071 0.7244 0.086 Uiso 1 1 calc R . .
C8 C 0.3547(9) 0.0411(7) 0.6079(7) 0.071(3) Uani 1 1 d . . .
H8 H 0.4092 0.0463 0.6190 0.085 Uiso 1 1 calc R . .
C9 C 0.3552(7) 0.0573(6) 0.5256(6) 0.055(2) Uani 1 1 d . . .
H9 H 0.4115 0.0705 0.4821 0.065 Uiso 1 1 calc R . .
C11 C 0.2390(7) 0.4051(6) 0.3183(6) 0.054(2) Uani 1 1 d . . .
C12 C 0.3897(6) 0.3174(6) 0.1469(6) 0.052(2) Uani 1 1 d . . .
C13 C 0.2087(6) 0.4277(5) 0.1576(6) 0.0495(19) Uani 1 1 d . . .
C21 C -0.0217(9) 0.3555(8) 0.4108(7) 0.074(3) Uani 1 1 d . . .
C22 C -0.0448(7) 0.2246(7) 0.3431(8) 0.070(3) Uani 1 1 d . . .
C23 C -0.0053(6) 0.3622(6) 0.2253(6) 0.053(2) Uani 1 1 d . . .
C31 C 0.0590(7) 0.1740(6) 0.4959(6) 0.052(2) Uani 1 1 d . . .
C32 C 0.0701(7) 0.0557(6) 0.4022(6) 0.055(2) Uani 1 1 d . . .
C41 C 0.3251(7) 0.2265(6) 0.4138(5) 0.0484(19) Uani 1 1 d . . .
C42 C 0.4792(6) 0.1488(5) 0.2638(5) 0.0441(17) Uani 1 1 d . . .
C51 C 0.2164(8) 0.2547(6) 0.1125(6) 0.056(2) Uani 1 1 d . . .
C52 C 0.1411(8) 0.1150(7) 0.2051(7) 0.068(3) Uani 1 1 d . . .
C53 C 0.3725(7) 0.1224(6) 0.1410(6) 0.054(2) Uani 1 1 d . . .
C60 C 0.3506(10) -0.1922(7) 0.3419(8) 0.077(3) Uani 1 1 d . . .
C61 C 0.2410(11) -0.1472(8) 0.4006(8) 0.092(4) Uani 1 1 d . . .
H61A H 0.1942 -0.1382 0.3725 0.138 Uiso 1 1 calc R . .
H61B H 0.2399 -0.0926 0.4149 0.138 Uiso 1 1 calc R . .
H61C H 0.2206 -0.1826 0.4510 0.138 Uiso 1 1 calc R . .
C62 C 0.4174(12) -0.1930(8) 0.3905(9) 0.097(4) Uani 1 1 d . . .
H62A H 0.3891 -0.2163 0.4467 0.145 Uiso 1 1 calc R . .
H62B H 0.4189 -0.1353 0.3926 0.145 Uiso 1 1 calc R . .
H62C H 0.4859 -0.2279 0.3627 0.145 Uiso 1 1 calc R . .
C63 C 0.3535(12) -0.2835(7) 0.3337(9) 0.097(4) Uani 1 1 d . . .
H63A H 0.4223 -0.3145 0.3009 0.146 Uiso 1 1 calc R . .
H63B H 0.3083 -0.2827 0.3062 0.146 Uiso 1 1 calc R . .
H63C H 0.3317 -0.3114 0.3886 0.146 Uiso 1 1 calc R . .
C64 C 0.5325(7) -0.1553(6) 0.1829(7) 0.059(2) Uani 1 1 d . . .
C65 C 0.5802(8) -0.1131(7) 0.2233(8) 0.073(3) Uani 1 1 d . . .
H65A H 0.6537 -0.1324 0.1975 0.110 Uiso 1 1 calc R . .
H65B H 0.5590 -0.1288 0.2824 0.110 Uiso 1 1 calc R . .
H65C H 0.5578 -0.0517 0.2154 0.110 Uiso 1 1 calc R . .
C66 C 0.5846(10) -0.2534(7) 0.1824(9) 0.091(4) Uani 1 1 d . . .
H66A H 0.5592 -0.2806 0.1535 0.136 Uiso 1 1 calc R . .
H66B H 0.5692 -0.2769 0.2392 0.136 Uiso 1 1 calc R . .
H66C H 0.6576 -0.2637 0.1541 0.136 Uiso 1 1 calc R . .
C67 C 0.5622(9) -0.1191(9) 0.0919(7) 0.083(3) Uani 1 1 d . . .
H67A H 0.5421 -0.0574 0.0913 0.124 Uiso 1 1 calc R . .
H67B H 0.5279 -0.1378 0.0643 0.124 Uiso 1 1 calc R . .
H67C H 0.6352 -0.1395 0.0630 0.124 Uiso 1 1 calc R . .
C68 C 0.3288(9) -0.1458(7) 0.1674(8) 0.071(3) Uani 1 1 d . . .
C69 C 0.2123(9) -0.1399(9) 0.2210(9) 0.089(4) Uani 1 1 d . . .
H69A H 0.1770 -0.0828 0.2409 0.134 Uiso 1 1 calc R . .
H69B H 0.2071 -0.1807 0.2681 0.134 Uiso 1 1 calc R . .
H69C H 0.1816 -0.1525 0.1866 0.134 Uiso 1 1 calc R . .
C70 C 0.3311(10) -0.0758(8) 0.0960(7) 0.079(3) Uani 1 1 d . . .
H70A H 0.4003 -0.0833 0.0562 0.119 Uiso 1 1 calc R . .
H70B H 0.3058 -0.0200 0.1190 0.119 Uiso 1 1 calc R . .
H70C H 0.2884 -0.0804 0.0682 0.119 Uiso 1 1 calc R . .
C71 C 0.3818(13) -0.2349(8) 0.1281(10) 0.105(5) Uani 1 1 d . . .
H71A H 0.3481 -0.2419 0.0936 0.158 Uiso 1 1 calc R . .
H71B H 0.3777 -0.2793 0.1721 0.158 Uiso 1 1 calc R . .
H71C H 0.4526 -0.2386 0.0943 0.158 Uiso 1 1 calc R . .
C72 C 0.5704(10) 0.4433(8) 0.1542(12) 0.106(5) Uani 1 1 d . . .
C73 C 0.5943(13) 0.4352(11) 0.0610(10) 0.125(7) Uani 1 1 d . . .
H73A H 0.5575 0.3986 0.0560 0.187 Uiso 1 1 calc R . .
H73B H 0.6667 0.4107 0.0328 0.187 Uiso 1 1 calc R . .
H73C H 0.5735 0.4912 0.0358 0.187 Uiso 1 1 calc R . .
C74 C 0.6348(13) 0.4981(11) 0.1661(14) 0.147(8) Uani 1 1 d . . .
H74A H 0.6286 0.5508 0.1323 0.221 Uiso 1 1 calc R . .
H74B H 0.7058 0.4657 0.1490 0.221 Uiso 1 1 calc R . .
H74C H 0.6092 0.5110 0.2243 0.221 Uiso 1 1 calc R . .
C75 C 0.4571(11) 0.4942(8) 0.1881(14) 0.133(7) Uani 1 1 d . . .
H75A H 0.4475 0.5475 0.1556 0.200 Uiso 1 1 calc R . .
H75B H 0.4368 0.5062 0.2459 0.200 Uiso 1 1 calc R . .
H75C H 0.4160 0.4611 0.1843 0.200 Uiso 1 1 calc R . .
C76 C 0.7133(8) 0.2585(8) 0.1435(8) 0.076(3) Uani 1 1 d . . .
C77 C 0.6965(9) 0.2241(9) 0.0754(8) 0.086(4) Uani 1 1 d . . .
H77A H 0.6623 0.2711 0.0469 0.130 Uiso 1 1 calc R . .
H77B H 0.6549 0.1848 0.1008 0.130 Uiso 1 1 calc R . .
H77C H 0.7617 0.1946 0.0357 0.130 Uiso 1 1 calc R . .
C78 C 0.8043(9) 0.3003(10) 0.1030(10) 0.104(5) Uani 1 1 d . . .
H78A H 0.8594 0.2647 0.0599 0.156 Uiso 1 1 calc R . .
H78B H 0.8280 0.3057 0.1454 0.156 Uiso 1 1 calc R . .
H78C H 0.7815 0.3563 0.0788 0.156 Uiso 1 1 calc R . .
C79 C 0.7491(9) 0.1784(8) 0.1967(10) 0.098(5) Uani 1 1 d . . .
H79A H 0.6907 0.1591 0.2345 0.146 Uiso 1 1 calc R . .
H79B H 0.7814 0.1932 0.2284 0.146 Uiso 1 1 calc R . .
H79C H 0.7972 0.1332 0.1601 0.146 Uiso 1 1 calc R . .
C80 C 0.5954(11) 0.3401(11) 0.3155(9) 0.096(4) Uani 1 1 d . . .
C81 C 0.5826(12) 0.2587(12) 0.3696(8) 0.112(6) Uani 1 1 d . . .
H81A H 0.5985 0.2587 0.4180 0.168 Uiso 1 1 calc R . .
H81B H 0.6282 0.2095 0.3376 0.168 Uiso 1 1 calc R . .
H81C H 0.5129 0.2564 0.3875 0.168 Uiso 1 1 calc R . .
C82 C 0.6944(12) 0.3580(12) 0.3112(11) 0.127(6) Uani 1 1 d . . .
H82A H 0.7031 0.4099 0.2775 0.191 Uiso 1 1 calc R . .
H82B H 0.7527 0.3107 0.2865 0.191 Uiso 1 1 calc R . .
H82C H 0.6887 0.3647 0.3670 0.191 Uiso 1 1 calc R . .
C83 C 0.5036(14) 0.4146(16) 0.3614(12) 0.165(10) Uani 1 1 d . . .
H83A H 0.4409 0.3988 0.3774 0.247 Uiso 1 1 calc R . .
H83B H 0.5019 0.4652 0.3245 0.247 Uiso 1 1 calc R . .
H83C H 0.5109 0.4260 0.4107 0.247 Uiso 1 1 calc R . .
C84 C -0.0641(7) 0.6171(6) 0.1302(6) 0.050(2) Uani 1 1 d . . .
C85 C -0.0960(10) 0.7150(6) 0.1058(7) 0.072(3) Uani 1 1 d . . .
H85A H -0.1100 0.7225 0.0554 0.108 Uiso 1 1 calc R . .
H85B H -0.0411 0.7394 0.0965 0.108 Uiso 1 1 calc R . .
H85C H -0.1565 0.7434 0.1506 0.108 Uiso 1 1 calc R . .
C86 C -0.1498(8) 0.5795(7) 0.1402(7) 0.063(2) Uani 1 1 d . . .
H86A H -0.1602 0.5874 0.0880 0.095 Uiso 1 1 calc R . .
H86B H -0.2119 0.6082 0.1835 0.095 Uiso 1 1 calc R . .
H86C H -0.1316 0.5192 0.1554 0.095 Uiso 1 1 calc R . .
C87 C 0.0323(8) 0.5711(7) 0.0558(6) 0.065(3) Uani 1 1 d . . .
H87A H 0.0441 0.5098 0.0654 0.097 Uiso 1 1 calc R . .
H87B H 0.0912 0.5869 0.0522 0.097 Uiso 1 1 calc R . .
H87C H 0.0207 0.5883 0.0042 0.097 Uiso 1 1 calc R . .
C88 C -0.1565(8) 0.6115(7) 0.3263(6) 0.065(3) Uani 1 1 d . . .
C89 C -0.2048(8) 0.5384(8) 0.3391(8) 0.086(4) Uani 1 1 d . . .
H89A H -0.2543 0.5377 0.3956 0.128 Uiso 1 1 calc R . .
H89B H -0.1523 0.4845 0.3299 0.128 Uiso 1 1 calc R . .
H89C H -0.2383 0.5467 0.3000 0.128 Uiso 1 1 calc R . .
C90 C -0.2374(10) 0.6957(8) 0.3232(8) 0.088(4) Uani 1 1 d . . .
H90A H -0.2467 0.7021 0.2707 0.132 Uiso 1 1 calc R . .
H90B H -0.2152 0.7431 0.3281 0.132 Uiso 1 1 calc R . .
H90C H -0.3013 0.6950 0.3688 0.132 Uiso 1 1 calc R . .
C91 C -0.1288(10) 0.6085(10) 0.4037(7) 0.100(5) Uani 1 1 d . . .
H91A H -0.1858 0.6019 0.4541 0.150 Uiso 1 1 calc R . .
H91B H -0.1134 0.6610 0.4044 0.150 Uiso 1 1 calc R . .
H91C H -0.0699 0.5606 0.4006 0.150 Uiso 1 1 calc R . .
C92 C 0.0448(9) 0.6684(6) 0.2293(7) 0.065(3) Uani 1 1 d . . .
C93 C -0.0217(11) 0.7594(7) 0.2556(9) 0.087(4) Uani 1 1 d . . .
H93A H 0.0200 0.7988 0.2335 0.130 Uiso 1 1 calc R . .
H93B H -0.0512 0.7603 0.3159 0.130 Uiso 1 1 calc R . .
H93C H -0.0756 0.7761 0.2339 0.130 Uiso 1 1 calc R . .
C94 C 0.1032(11) 0.6293(7) 0.2894(9) 0.085(4) Uani 1 1 d . . .
H94A H 0.1409 0.5706 0.2762 0.127 Uiso 1 1 calc R . .
H94B H 0.0549 0.6312 0.3465 0.127 Uiso 1 1 calc R . .
H94C H 0.1499 0.6618 0.2828 0.127 Uiso 1 1 calc R . .
C95 C 0.1265(9) 0.6729(7) 0.1422(8) 0.076(3) Uani 1 1 d . . .
H95A H 0.0943 0.6948 0.1019 0.115 Uiso 1 1 calc R . .
H95B H 0.1718 0.6164 0.1278 0.115 Uiso 1 1 calc R . .
H95C H 0.1652 0.7105 0.1419 0.115 Uiso 1 1 calc R . .
C1S C 1.021(2) 0.9883(19) 0.062(2) 0.200(11) Uiso 1 1 d . . .
H1S H 1.0383 0.9731 0.1089 0.240 Uiso 1 1 calc R . .
C2S C 0.932(2) 0.9547(18) 0.069(2) 0.200(11) Uiso 1 1 d . . .
H2S H 0.8916 0.9297 0.1179 0.240 Uiso 1 1 calc R . .
C3S C 0.921(3) 0.967(2) -0.005(2) 0.228(14) Uiso 1 1 d . . .
H3S H 0.8764 0.9460 -0.0158 0.273 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.03999(16) 0.04183(16) 0.04074(16) -0.00272(12) -0.01968(13) -0.00492(12)
Pt2 0.03539(15) 0.05087(19) 0.05497(19) 0.00188(14) -0.02086(14) -0.01686(13)
Pt3 0.03358(14) 0.04020(16) 0.04547(17) -0.00280(12) -0.01779(12) -0.00542(11)
Ru1 0.0268(3) 0.0364(3) 0.0462(3) -0.0008(2) -0.0150(2) -0.0073(2)
Ru2 0.0263(3) 0.0441(3) 0.0494(3) 0.0031(3) -0.0150(2) -0.0072(2)
Ru3 0.0280(3) 0.0426(3) 0.0415(3) 0.0015(2) -0.0147(2) -0.0120(2)
Ru4 0.0259(2) 0.0384(3) 0.0352(3) -0.0021(2) -0.0141(2) -0.0093(2)
Ru5 0.0389(3) 0.0411(3) 0.0425(3) -0.0003(2) -0.0242(3) -0.0089(2)
P1 0.0512(12) 0.0457(12) 0.0556(12) -0.0092(10) -0.0293(10) -0.0059(9)
P2 0.0499(13) 0.0599(14) 0.0784(16) 0.0089(12) -0.0349(12) -0.0280(11)
P3 0.0459(11) 0.0418(11) 0.0517(12) -0.0059(9) -0.0275(10) -0.0018(9)
O11 0.104(6) 0.074(5) 0.077(5) -0.024(4) -0.045(5) -0.009(4)
O12 0.044(3) 0.111(6) 0.054(4) 0.006(4) -0.017(3) -0.022(4)
O13 0.051(4) 0.073(5) 0.071(5) 0.022(4) -0.010(3) -0.005(3)
O21 0.177(12) 0.092(7) 0.071(6) -0.017(5) -0.027(7) 0.037(7)
O22 0.066(5) 0.106(7) 0.177(10) 0.049(7) -0.064(6) -0.051(5)
O23 0.089(5) 0.073(5) 0.101(6) 0.014(4) -0.072(5) -0.026(4)
O31 0.076(5) 0.089(5) 0.049(4) -0.013(4) -0.009(4) -0.005(4)
O32 0.078(5) 0.095(6) 0.116(7) 0.000(5) -0.032(5) -0.057(5)
O41 0.108(6) 0.077(5) 0.071(5) -0.024(4) -0.045(5) -0.019(5)
O42 0.031(3) 0.062(4) 0.115(6) 0.001(4) -0.011(4) -0.009(3)
O51 0.137(8) 0.085(6) 0.060(4) 0.008(4) -0.056(5) -0.010(5)
O52 0.086(6) 0.110(7) 0.122(7) -0.021(6) -0.054(5) -0.045(5)
O53 0.055(4) 0.091(5) 0.054(4) 0.006(4) -0.005(3) -0.004(4)
C1 0.026(3) 0.040(4) 0.038(4) 0.000(3) -0.014(3) -0.003(3)
C2 0.043(4) 0.044(4) 0.053(4) 0.002(3) -0.028(4) -0.017(3)
C3 0.034(3) 0.047(4) 0.040(4) 0.002(3) -0.020(3) -0.012(3)
C4 0.043(4) 0.055(5) 0.047(4) -0.004(4) -0.025(4) -0.010(4)
C5 0.063(6) 0.070(6) 0.059(5) 0.018(5) -0.037(5) -0.024(5)
C6 0.083(8) 0.102(9) 0.047(5) 0.022(5) -0.029(5) -0.028(7)
C7 0.088(8) 0.080(7) 0.045(5) 0.010(5) -0.040(5) -0.007(6)
C8 0.080(7) 0.085(7) 0.075(7) 0.005(6) -0.061(6) -0.019(6)
C9 0.060(5) 0.066(6) 0.049(5) 0.002(4) -0.033(4) -0.018(4)
C11 0.047(5) 0.051(5) 0.064(5) -0.012(4) -0.024(4) -0.004(4)
C12 0.037(4) 0.055(5) 0.064(6) -0.005(4) -0.021(4) -0.010(4)
C13 0.038(4) 0.043(4) 0.059(5) 0.000(4) -0.015(4) -0.004(3)
C21 0.067(7) 0.072(7) 0.057(6) -0.006(5) -0.016(5) 0.007(5)
C22 0.046(5) 0.071(6) 0.097(8) 0.026(6) -0.035(5) -0.026(5)
C23 0.041(4) 0.053(5) 0.072(6) 0.006(4) -0.032(4) -0.011(4)
C31 0.045(4) 0.058(5) 0.050(5) 0.000(4) -0.015(4) -0.015(4)
C32 0.040(4) 0.065(6) 0.062(5) 0.001(4) -0.016(4) -0.023(4)
C41 0.051(5) 0.047(5) 0.045(4) -0.009(4) -0.018(4) -0.008(4)
C42 0.034(4) 0.047(4) 0.053(4) -0.002(4) -0.016(3) -0.012(3)
C51 0.077(6) 0.045(5) 0.052(5) 0.003(4) -0.039(5) -0.006(4)
C52 0.064(6) 0.078(7) 0.071(6) -0.012(5) -0.029(5) -0.021(5)
C53 0.044(5) 0.064(6) 0.046(5) -0.009(4) -0.014(4) -0.004(4)
C60 0.102(9) 0.046(5) 0.088(8) 0.013(5) -0.042(7) -0.030(6)
C61 0.114(11) 0.077(8) 0.070(7) 0.001(6) -0.014(7) -0.037(8)
C62 0.145(13) 0.067(7) 0.094(9) 0.026(7) -0.079(9) -0.020(8)
C63 0.132(12) 0.050(6) 0.112(11) 0.002(6) -0.054(10) -0.020(7)
C64 0.041(4) 0.054(5) 0.078(6) -0.019(5) -0.028(4) 0.007(4)
C65 0.052(5) 0.075(7) 0.100(8) -0.022(6) -0.040(6) -0.004(5)
C66 0.080(8) 0.066(7) 0.125(11) -0.031(7) -0.059(8) 0.023(6)
C67 0.056(6) 0.100(9) 0.077(8) -0.013(7) -0.017(6) -0.006(6)
C68 0.070(6) 0.069(6) 0.097(8) -0.023(6) -0.053(6) -0.009(5)
C69 0.066(7) 0.097(9) 0.127(11) -0.034(8) -0.049(7) -0.020(6)
C70 0.086(8) 0.088(8) 0.078(7) -0.025(6) -0.055(7) 0.000(6)
C71 0.145(13) 0.074(8) 0.142(13) -0.033(8) -0.103(12) -0.010(8)
C72 0.074(8) 0.071(8) 0.193(17) 0.030(9) -0.065(10) -0.044(7)
C73 0.126(13) 0.155(15) 0.125(13) 0.084(12) -0.077(11) -0.088(12)
C74 0.116(12) 0.108(12) 0.26(2) 0.048(14) -0.100(15) -0.083(11)
C75 0.087(10) 0.059(8) 0.26(2) 0.025(11) -0.085(13) -0.022(7)
C76 0.046(5) 0.090(8) 0.098(8) 0.001(7) -0.018(5) -0.039(5)
C77 0.059(6) 0.113(10) 0.081(8) -0.020(7) -0.007(6) -0.033(7)
C78 0.055(6) 0.133(12) 0.125(12) 0.011(9) -0.019(7) -0.054(8)
C79 0.061(7) 0.089(9) 0.144(13) 0.030(8) -0.052(8) -0.022(6)
C80 0.088(9) 0.146(13) 0.095(9) -0.015(9) -0.049(8) -0.061(9)
C81 0.098(10) 0.203(18) 0.073(8) 0.012(10) -0.047(8) -0.080(11)
C82 0.119(12) 0.179(17) 0.154(15) -0.007(12) -0.091(12) -0.081(12)
C83 0.098(12) 0.28(3) 0.141(16) -0.117(18) -0.021(11) -0.065(16)
C84 0.054(5) 0.049(5) 0.059(5) -0.001(4) -0.036(4) -0.010(4)
C85 0.101(9) 0.054(6) 0.078(7) 0.010(5) -0.058(7) -0.018(6)
C86 0.064(6) 0.061(6) 0.081(7) -0.003(5) -0.045(5) -0.017(5)
C87 0.077(7) 0.074(7) 0.052(5) -0.004(5) -0.029(5) -0.026(5)
C88 0.056(5) 0.057(6) 0.061(6) -0.012(4) -0.016(5) 0.009(4)
C89 0.048(6) 0.083(8) 0.084(8) 0.005(6) -0.002(5) 0.002(5)
C90 0.075(8) 0.079(8) 0.091(8) -0.016(6) -0.040(7) 0.023(6)
C91 0.080(8) 0.113(11) 0.061(7) -0.020(7) -0.013(6) 0.024(7)
C92 0.086(7) 0.044(5) 0.084(7) -0.001(5) -0.059(6) -0.008(5)
C93 0.112(10) 0.043(5) 0.133(11) -0.014(6) -0.079(9) -0.010(6)
C94 0.112(10) 0.067(7) 0.117(10) -0.004(6) -0.088(9) -0.021(6)
C95 0.071(7) 0.056(6) 0.117(10) 0.010(6) -0.046(7) -0.031(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pt1 P1 100.6(2) . . ?
C2 Pt1 C53 114.3(3) . . ?
P1 Pt1 C53 118.9(2) . . ?
C2 Pt1 Ru5 111.6(2) . . ?
P1 Pt1 Ru5 147.70(6) . . ?
C53 Pt1 Ru5 44.9(2) . . ?
C2 Pt1 Ru4 47.9(2) . . ?
P1 Pt1 Ru4 145.99(5) . . ?
C53 Pt1 Ru4 74.6(2) . . ?
Ru5 Pt1 Ru4 64.701(18) . . ?
C2 Pt1 Ru3 68.4(2) . . ?
P1 Pt1 Ru3 135.05(6) . . ?
C53 Pt1 Ru3 104.7(2) . . ?
Ru5 Pt1 Ru3 63.749(19) . . ?
Ru4 Pt1 Ru3 53.806(16) . . ?
C12 Pt2 C42 111.5(3) . . ?
C12 Pt2 P2 111.5(3) . . ?
C42 Pt2 P2 111.9(2) . . ?
C12 Pt2 Ru4 96.5(3) . . ?
C42 Pt2 Ru4 47.3(2) . . ?
P2 Pt2 Ru4 151.00(6) . . ?
C12 Pt2 Ru1 47.3(3) . . ?
C42 Pt2 Ru1 105.2(2) . . ?
P2 Pt2 Ru1 142.57(7) . . ?
Ru4 Pt2 Ru1 63.801(18) . . ?
C13 Pt3 C23 109.7(4) . . ?
C13 Pt3 P3 111.5(2) . . ?
C23 Pt3 P3 112.1(2) . . ?
C13 Pt3 Ru2 103.6(2) . . ?
C23 Pt3 Ru2 47.5(2) . . ?
P3 Pt3 Ru2 144.42(6) . . ?
C13 Pt3 Ru1 47.1(2) . . ?
C23 Pt3 Ru1 98.0(2) . . ?
P3 Pt3 Ru1 148.87(6) . . ?
Ru2 Pt3 Ru1 64.096(18) . . ?
C11 Ru1 C1 102.1(4) . . ?
C11 Ru1 C12 106.6(4) . . ?
C1 Ru1 C12 128.0(3) . . ?
C11 Ru1 C13 96.3(4) . . ?
C1 Ru1 C13 137.4(3) . . ?
C12 Ru1 C13 81.1(3) . . ?
C11 Ru1 Pt2 77.5(3) . . ?
C1 Ru1 Pt2 101.53(18) . . ?
C12 Ru1 Pt2 46.6(3) . . ?
C13 Ru1 Pt2 120.0(2) . . ?
C11 Ru1 Ru5 151.0(3) . . ?
C1 Ru1 Ru5 49.2(2) . . ?
C12 Ru1 Ru5 92.4(3) . . ?
C13 Ru1 Ru5 108.3(3) . . ?
Pt2 Ru1 Ru5 101.93(2) . . ?
C11 Ru1 Pt3 84.4(3) . . ?
C1 Ru1 Pt3 98.14(19) . . ?
C12 Ru1 Pt3 126.8(3) . . ?
C13 Ru1 Pt3 45.7(2) . . ?
Pt2 Ru1 Pt3 155.61(3) . . ?
Ru5 Ru1 Pt3 101.81(2) . . ?
C11 Ru1 Ru4 94.4(3) . . ?
C1 Ru1 Ru4 43.58(18) . . ?
C12 Ru1 Ru4 91.3(3) . . ?
C13 Ru1 Ru4 168.3(3) . . ?
Pt2 Ru1 Ru4 58.071(16) . . ?
Ru5 Ru1 Ru4 62.79(2) . . ?
Pt3 Ru1 Ru4 140.71(2) . . ?
C11 Ru1 Ru2 104.6(3) . . ?
C1 Ru1 Ru2 42.50(18) . . ?
C12 Ru1 Ru2 148.8(3) . . ?
C13 Ru1 Ru2 95.8(2) . . ?
Pt2 Ru1 Ru2 143.99(3) . . ?
Ru5 Ru1 Ru2 58.91(2) . . ?
Pt3 Ru1 Ru2 56.742(17) . . ?
Ru4 Ru1 Ru2 86.06(2) . . ?
C22 Ru2 C21 94.6(6) . . ?
C22 Ru2 C1 122.2(4) . . ?
C21 Ru2 C1 101.9(4) . . ?
C22 Ru2 C23 92.1(4) . . ?
C21 Ru2 C23 104.6(4) . . ?
C1 Ru2 C23 134.3(3) . . ?
C22 Ru2 Pt3 137.0(3) . . ?
C21 Ru2 Pt3 80.5(4) . . ?
C1 Ru2 Pt3 100.5(2) . . ?
C23 Ru2 Pt3 49.4(3) . . ?
C22 Ru2 Ru5 101.4(4) . . ?
C21 Ru2 Ru5 150.6(4) . . ?
C1 Ru2 Ru5 48.8(2) . . ?
C23 Ru2 Ru5 99.3(3) . . ?
Pt3 Ru2 Ru5 103.09(2) . . ?
C22 Ru2 Ru3 77.2(3) . . ?
C21 Ru2 Ru3 97.3(3) . . ?
C1 Ru2 Ru3 46.1(2) . . ?
C23 Ru2 Ru3 156.4(3) . . ?
Pt3 Ru2 Ru3 145.76(3) . . ?
Ru5 Ru2 Ru3 63.23(2) . . ?
C22 Ru2 Ru1 159.2(4) . . ?
C21 Ru2 Ru1 102.3(4) . . ?
C1 Ru2 Ru1 42.5(2) . . ?
C23 Ru2 Ru1 95.3(2) . . ?
Pt3 Ru2 Ru1 59.163(17) . . ?
Ru5 Ru2 Ru1 58.15(2) . . ?
Ru3 Ru2 Ru1 88.55(2) . . ?
C31 Ru3 C32 90.8(4) . . ?
C31 Ru3 C1 106.6(3) . . ?
C32 Ru3 C1 144.4(3) . . ?
C31 Ru3 C3 94.5(3) . . ?
C32 Ru3 C3 107.6(4) . . ?
C1 Ru3 C3 101.8(3) . . ?
C31 Ru3 Ru4 113.9(3) . . ?
C32 Ru3 Ru4 148.5(3) . . ?
C1 Ru3 Ru4 48.65(18) . . ?
C3 Ru3 Ru4 53.8(2) . . ?
C31 Ru3 Ru2 91.3(3) . . ?
C32 Ru3 Ru2 106.5(3) . . ?
C1 Ru3 Ru2 44.01(18) . . ?
C3 Ru3 Ru2 145.3(2) . . ?
Ru4 Ru3 Ru2 92.65(2) . . ?
C31 Ru3 Pt1 157.7(3) . . ?
C32 Ru3 Pt1 87.7(3) . . ?
C1 Ru3 Pt1 86.96(19) . . ?
C3 Ru3 Pt1 64.9(2) . . ?
Ru4 Ru3 Pt1 61.975(18) . . ?
Ru2 Ru3 Pt1 110.39(2) . . ?
C31 Ru3 Ru5 147.7(3) . . ?
C32 Ru3 Ru5 105.8(3) . . ?
C1 Ru3 Ru5 45.5(2) . . ?
C3 Ru3 Ru5 106.1(2) . . ?
Ru4 Ru3 Ru5 63.57(2) . . ?
Ru2 Ru3 Ru5 57.69(2) . . ?
Pt1 Ru3 Ru5 52.903(17) . . ?
C41 Ru4 C1 103.2(3) . . ?
C41 Ru4 C42 93.9(4) . . ?
C1 Ru4 C42 140.3(3) . . ?
C41 Ru4 C2 111.4(3) . . ?
C1 Ru4 C2 119.6(3) . . ?
C42 Ru4 C2 85.4(3) . . ?
C41 Ru4 C3 89.5(3) . . ?
C1 Ru4 C3 99.0(3) . . ?
C42 Ru4 C3 117.0(3) . . ?
C2 Ru4 C3 36.9(3) . . ?
C41 Ru4 Ru3 106.1(3) . . ?
C1 Ru4 Ru3 50.1(2) . . ?
C42 Ru4 Ru3 154.7(2) . . ?
C2 Ru4 Ru3 73.1(2) . . ?
C3 Ru4 Ru3 49.52(18) . . ?
C41 Ru4 Pt2 77.7(3) . . ?
C1 Ru4 Pt2 100.7(2) . . ?
C42 Ru4 Pt2 48.1(2) . . ?
C2 Ru4 Pt2 133.5(2) . . ?
C3 Ru4 Pt2 158.50(17) . . ?
Ru3 Ru4 Pt2 150.79(3) . . ?
C41 Ru4 Pt1 153.2(3) . . ?
C1 Ru4 Pt1 89.4(2) . . ?
C42 Ru4 Pt1 91.0(2) . . ?
C2 Ru4 Pt1 42.8(2) . . ?
C3 Ru4 Pt1 64.96(19) . . ?
Ru3 Ru4 Pt1 64.219(19) . . ?
Pt2 Ru4 Pt1 123.64(2) . . ?
C41 Ru4 Ru1 95.6(3) . . ?
C1 Ru4 Ru1 42.7(2) . . ?
C42 Ru4 Ru1 100.8(2) . . ?
C2 Ru4 Ru1 151.93(19) . . ?
C3 Ru4 Ru1 141.48(18) . . ?
Ru3 Ru4 Ru1 92.71(2) . . ?
Pt2 Ru4 Ru1 58.128(17) . . ?
Pt1 Ru4 Ru1 109.34(2) . . ?
C41 Ru4 Ru5 147.4(3) . . ?
C1 Ru4 Ru5 45.4(2) . . ?
C42 Ru4 Ru5 106.8(2) . . ?
C2 Ru4 Ru5 95.45(19) . . ?
C3 Ru4 Ru5 102.52(18) . . ?
Ru3 Ru4 Ru5 63.42(2) . . ?
Pt2 Ru4 Ru5 97.44(2) . . ?
Pt1 Ru4 Ru5 53.412(16) . . ?
Ru1 Ru4 Ru5 56.510(19) . . ?
C51 Ru5 C52 96.4(5) . . ?
C51 Ru5 C53 92.5(4) . . ?
C52 Ru5 C53 111.6(4) . . ?
C51 Ru5 C1 114.5(3) . . ?
C52 Ru5 C1 117.0(4) . . ?
C53 Ru5 C1 119.7(3) . . ?
C51 Ru5 Pt1 148.2(3) . . ?
C52 Ru5 Pt1 80.7(3) . . ?
C53 Ru5 Pt1 60.3(3) . . ?
C1 Ru5 Pt1 94.53(18) . . ?
C51 Ru5 Ru1 76.1(3) . . ?
C52 Ru5 Ru1 147.7(3) . . ?
C53 Ru5 Ru1 100.2(3) . . ?
C1 Ru5 Ru1 45.13(19) . . ?
Pt1 Ru5 Ru1 121.84(2) . . ?
C51 Ru5 Ru2 88.9(3) . . ?
C52 Ru5 Ru2 85.8(3) . . ?
C53 Ru5 Ru2 162.2(3) . . ?
C1 Ru5 Ru2 44.74(17) . . ?
Pt1 Ru5 Ru2 122.18(3) . . ?
Ru1 Ru5 Ru2 62.94(2) . . ?
C51 Ru5 Ru3 148.0(3) . . ?
C52 Ru5 Ru3 81.2(3) . . ?
C53 Ru5 Ru3 118.2(3) . . ?
C1 Ru5 Ru3 43.85(19) . . ?
Pt1 Ru5 Ru3 63.349(18) . . ?
Ru1 Ru5 Ru3 88.87(2) . . ?
Ru2 Ru5 Ru3 59.08(2) . . ?
C51 Ru5 Ru4 133.2(3) . . ?
C52 Ru5 Ru4 129.6(3) . . ?
C53 Ru5 Ru4 79.1(3) . . ?
C1 Ru5 Ru4 42.61(17) . . ?
Pt1 Ru5 Ru4 61.887(17) . . ?
Ru1 Ru5 Ru4 60.70(2) . . ?
Ru2 Ru5 Ru4 87.02(2) . . ?
Ru3 Ru5 Ru4 53.007(18) . . ?
C68 P1 C64 107.4(5) . . ?
C68 P1 C60 109.1(5) . . ?
C64 P1 C60 108.8(5) . . ?
C68 P1 Pt1 105.2(3) . . ?
C64 P1 Pt1 112.1(3) . . ?
C60 P1 Pt1 113.9(4) . . ?
C76 P2 C80 108.0(6) . . ?
C76 P2 C72 108.4(6) . . ?
C80 P2 C72 109.1(8) . . ?
C76 P2 Pt2 113.7(3) . . ?
C80 P2 Pt2 107.0(4) . . ?
C72 P2 Pt2 110.6(4) . . ?
C84 P3 C88 108.5(4) . . ?
C84 P3 C92 109.1(4) . . ?
C88 P3 C92 108.3(5) . . ?
C84 P3 Pt3 113.3(3) . . ?
C88 P3 Pt3 107.7(3) . . ?
C92 P3 Pt3 109.8(3) . . ?
Ru1 C1 Ru2 95.0(3) . . ?
Ru1 C1 Ru4 93.7(3) . . ?
Ru2 C1 Ru4 171.0(4) . . ?
Ru1 C1 Ru3 173.7(4) . . ?
Ru2 C1 Ru3 89.9(3) . . ?
Ru4 C1 Ru3 81.3(2) . . ?
Ru1 C1 Ru5 85.6(3) . . ?
Ru2 C1 Ru5 86.5(3) . . ?
Ru4 C1 Ru5 92.0(3) . . ?
Ru3 C1 Ru5 90.6(3) . . ?
C3 C2 Pt1 112.4(5) . . ?
C3 C2 Ru4 73.4(5) . . ?
Pt1 C2 Ru4 89.3(3) . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 Ru3 112.0(5) . . ?
C4 C3 Ru3 127.6(5) . . ?
C2 C3 Ru4 69.6(4) . . ?
C4 C3 Ru4 126.9(5) . . ?
Ru3 C3 Ru4 76.6(2) . . ?
C5 C4 C9 118.0(8) . . ?
C5 C4 C3 120.0(7) . . ?
C9 C4 C3 121.9(8) . . ?
C4 C5 C6 120.7(9) . . ?
C7 C6 C5 120.0(10) . . ?
C8 C7 C6 120.7(9) . . ?
C7 C8 C9 120.0(9) . . ?
C4 C9 C8 120.5(9) . . ?
O11 C11 Ru1 175.2(9) . . ?
O12 C12 Pt2 128.8(7) . . ?
O12 C12 Ru1 144.4(7) . . ?
Pt2 C12 Ru1 86.2(4) . . ?
O13 C13 Pt3 129.6(7) . . ?
O13 C13 Ru1 143.1(7) . . ?
Pt3 C13 Ru1 87.3(3) . . ?
O21 C21 Ru2 174.6(10) . . ?
O22 C22 Ru2 174.1(9) . . ?
O23 C23 Ru2 148.2(8) . . ?
O23 C23 Pt3 128.1(7) . . ?
Ru2 C23 Pt3 83.1(3) . . ?
O31 C31 Ru3 176.7(9) . . ?
O32 C32 Ru3 175.2(9) . . ?
O41 C41 Ru4 178.0(8) . . ?
O42 C42 Ru4 146.3(7) . . ?
O42 C42 Pt2 128.1(7) . . ?
Ru4 C42 Pt2 84.6(3) . . ?
O51 C51 Ru5 170.7(9) . . ?
O52 C52 Ru5 173.9(11) . . ?
O53 C53 Ru5 165.2(8) . . ?
O53 C53 Pt1 119.9(7) . . ?
Ru5 C53 Pt1 74.9(3) . . ?
C63 C60 C62 109.6(10) . . ?
C63 C60 C61 107.7(11) . . ?
C62 C60 C61 103.6(11) . . ?
C63 C60 P1 116.6(9) . . ?
C62 C60 P1 110.1(8) . . ?
C61 C60 P1 108.5(8) . . ?
C65 C64 C67 104.9(10) . . ?
C65 C64 C66 108.3(8) . . ?
C67 C64 C66 108.3(9) . . ?
C65 C64 P1 109.4(7) . . ?
C67 C64 P1 110.2(7) . . ?
C66 C64 P1 115.2(8) . . ?
C70 C68 C71 108.6(10) . . ?
C70 C68 C69 106.7(9) . . ?
C71 C68 C69 108.8(10) . . ?
C70 C68 P1 110.4(7) . . ?
C71 C68 P1 114.5(8) . . ?
C69 C68 P1 107.5(8) . . ?
C75 C72 C73 103.8(14) . . ?
C75 C72 C74 107.9(13) . . ?
C73 C72 C74 111.7(13) . . ?
C75 C72 P2 109.6(10) . . ?
C73 C72 P2 110.1(11) . . ?
C74 C72 P2 113.3(11) . . ?
C77 C76 C79 105.8(11) . . ?
C77 C76 C78 110.1(11) . . ?
C79 C76 C78 106.1(10) . . ?
C77 C76 P2 108.8(8) . . ?
C79 C76 P2 110.6(9) . . ?
C78 C76 P2 115.0(9) . . ?
C81 C80 C83 107.0(15) . . ?
C81 C80 C82 108.7(13) . . ?
C83 C80 C82 107.4(13) . . ?
C81 C80 P2 109.7(9) . . ?
C83 C80 P2 107.5(11) . . ?
C82 C80 P2 116.2(11) . . ?
C86 C84 C85 108.3(8) . . ?
C86 C84 C87 106.5(8) . . ?
C85 C84 C87 109.0(8) . . ?
C86 C84 P3 110.7(7) . . ?
C85 C84 P3 114.4(6) . . ?
C87 C84 P3 107.6(6) . . ?
C89 C88 C90 107.6(10) . . ?
C89 C88 C91 107.3(10) . . ?
C90 C88 C91 109.3(9) . . ?
C89 C88 P3 109.1(7) . . ?
C90 C88 P3 115.7(8) . . ?
C91 C88 P3 107.6(8) . . ?
C95 C92 C93 109.5(10) . . ?
C95 C92 C94 106.1(10) . . ?
C93 C92 C94 108.8(9) . . ?
C95 C92 P3 108.9(7) . . ?
C93 C92 P3 114.4(8) . . ?
C94 C92 P3 108.9(7) . . ?
C3S C1S C2S 136(3) 2_775 . ?
C3S C2S C1S 109(3) . . ?
C1S C3S C2S 115(4) 2_775 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C2 1.983(7) . ?
Pt1 P1 2.332(2) . ?
Pt1 C53 2.391(10) . ?
Pt1 Ru5 2.6583(7) . ?
Pt1 Ru4 2.9201(6) . ?
Pt1 Ru3 2.9788(7) . ?
Pt2 C12 2.022(9) . ?
Pt2 C42 2.077(8) . ?
Pt2 P2 2.320(2) . ?
Pt2 Ru4 2.7762(6) . ?
Pt2 Ru1 2.7780(6) . ?
Pt3 C13 2.011(8) . ?
Pt3 C23 2.093(9) . ?
Pt3 P3 2.323(2) . ?
Pt3 Ru2 2.7356(7) . ?
Pt3 Ru1 2.8090(6) . ?
Ru1 C11 1.893(9) . ?
Ru1 C1 1.995(7) . ?
Ru1 C12 2.046(9) . ?
Ru1 C13 2.059(9) . ?
Ru1 Ru5 2.8069(9) . ?
Ru1 Ru4 2.9351(8) . ?
Ru1 Ru2 2.9428(8) . ?
Ru2 C22 1.873(10) . ?
Ru2 C21 1.908(11) . ?
Ru2 C1 1.996(6) . ?
Ru2 C23 2.033(8) . ?
Ru2 Ru5 2.8297(9) . ?
Ru2 Ru3 2.8723(8) . ?
Ru3 C31 1.854(9) . ?
Ru3 C32 1.881(9) . ?
Ru3 C1 2.071(7) . ?
Ru3 C3 2.087(7) . ?
Ru3 Ru4 2.6696(8) . ?
Ru3 Ru5 2.9891(9) . ?
Ru4 C41 1.844(8) . ?
Ru4 C1 2.028(6) . ?
Ru4 C42 2.049(8) . ?
Ru4 C2 2.167(8) . ?
Ru4 C3 2.215(7) . ?
Ru4 Ru5 2.9932(8) . ?
Ru5 C51 1.890(8) . ?
Ru5 C52 1.899(11) . ?
Ru5 C53 1.943(9) . ?
Ru5 C1 2.132(7) . ?
P1 C68 1.909(10) . ?
P1 C64 1.915(9) . ?
P1 C60 1.920(11) . ?
P2 C76 1.889(12) . ?
P2 C80 1.911(13) . ?
P2 C72 1.913(13) . ?
P3 C84 1.918(8) . ?
P3 C88 1.921(10) . ?
P3 C92 1.929(11) . ?
O11 C11 1.135(11) . ?
O12 C12 1.179(11) . ?
O13 C13 1.173(11) . ?
O21 C21 1.128(13) . ?
O22 C22 1.156(12) . ?
O23 C23 1.159(10) . ?
O31 C31 1.142(11) . ?
O32 C32 1.158(11) . ?
O41 C41 1.157(10) . ?
O42 C42 1.158(10) . ?
O51 C51 1.148(10) . ?
O52 C52 1.152(12) . ?
O53 C53 1.145(11) . ?
C2 C3 1.388(11) . ?
C3 C4 1.493(10) . ?
C4 C5 1.383(13) . ?
C4 C9 1.385(11) . ?
C5 C6 1.389(13) . ?
C6 C7 1.370(16) . ?
C7 C8 1.340(16) . ?
C8 C9 1.406(12) . ?
C60 C63 1.512(15) . ?
C60 C62 1.530(17) . ?
C60 C61 1.543(18) . ?
C64 C65 1.527(14) . ?
C64 C67 1.528(16) . ?
C64 C66 1.547(14) . ?
C68 C70 1.538(17) . ?
C68 C71 1.547(16) . ?
C68 C69 1.574(17) . ?
C72 C75 1.53(2) . ?
C72 C73 1.53(2) . ?
C72 C74 1.585(18) . ?
C76 C77 1.525(17) . ?
C76 C79 1.551(17) . ?
C76 C78 1.558(14) . ?
C80 C81 1.51(2) . ?
C80 C83 1.54(2) . ?
C80 C82 1.552(16) . ?
C84 C86 1.512(13) . ?
C84 C85 1.559(13) . ?
C84 C87 1.562(14) . ?
C88 C89 1.522(17) . ?
C88 C90 1.523(13) . ?
C88 C91 1.544(16) . ?
C92 C95 1.518(16) . ?
C92 C93 1.530(14) . ?
C92 C94 1.548(13) . ?
C1S C3S 1.30(4) 2_775 ?
C1S C2S 1.53(4) . ?
C2S C3S 1.34(4) . ?
C3S C1S 1.30(4) 2_775 ?
|
1100876.cif | #------------------------------------------------------------------------------
#$Date: 2019-10-02 14:34:28 +0300 (Wed, 02 Oct 2019) $
#$Revision: 219028 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100876.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100876
loop_
_publ_author_name
'Baya, Miguel'
'Buil, Mar\'ia L.'
'Esteruelas, Miguel A.'
'O\~nate, Enrique'
_publ_section_title
;
Ene-Type Reactions between an \a-Alkenylphosphine and Terminal Alkynes
Promoted by Osmium-Cyclopentadienyl Fragments
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2030
_journal_page_last 2038
_journal_paper_doi 10.1021/om0489857
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C22 H30 Cl Os P'
_chemical_formula_weight 551.08
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 95.913(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.3343(10)
_cell_length_b 12.6118(10)
_cell_length_c 13.4358(11)
_cell_measurement_reflns_used 2872
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 20
_cell_measurement_theta_min 2.5
_cell_volume 2078.9(3)
_computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\w rotations with narrow frames'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0729
_diffrn_reflns_av_sigmaI/netI 0.0965
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 24944
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.57
_diffrn_reflns_theta_min 2.13
_diffrn_standards_decay_% 'no decay'
_exptl_absorpt_coefficient_mu 6.342
_exptl_absorpt_correction_T_max 0.746
_exptl_absorpt_correction_T_min 0.545
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
SADABS: Area-Detector Absorption Correction. Bruker-AXS
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.761
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular blok'
_exptl_crystal_F_000 1080
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.521
_refine_diff_density_min -0.820
_refine_diff_density_rms 0.103
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.655
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 254
_refine_ls_number_reflns 4983
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.655
_refine_ls_R_factor_all 0.0576
_refine_ls_R_factor_gt 0.0297
_refine_ls_shift/su_max 0.016
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0365
_refine_ls_wR_factor_ref 0.0402
_reflns_number_gt 3232
_reflns_number_total 4983
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060292
_cod_depositor_comments
;
Updated bibliographic information.
Antanas Vaitkus,
2019-10-02
;
_cod_original_sg_symbol_H-M P21/n
_cod_database_code 1100876
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.840105(14) 0.216209(14) 0.836456(14) 0.03316(6) Uani 1 1 d . . .
Cl Cl 0.88837(10) 0.40251(9) 0.83097(9) 0.0497(3) Uani 1 1 d . . .
P P 0.75584(9) 0.25483(9) 0.97695(9) 0.0375(3) Uani 1 1 d . . .
C1 C 0.6197(3) 0.2903(4) 0.9243(3) 0.0423(12) Uani 1 1 d . . .
C2 C 0.5825(4) 0.2051(5) 0.8499(4) 0.0486(14) Uani 1 1 d . . .
H2A H 0.563(3) 0.134(3) 0.894(3) 0.052(14) Uiso 1 1 d . . .
H2B H 0.514(3) 0.223(3) 0.810(3) 0.048(13) Uiso 1 1 d . . .
C3 C 0.6697(4) 0.1820(4) 0.7798(3) 0.0368(12) Uani 1 1 d . . .
H3 H 0.671(3) 0.109(3) 0.753(3) 0.045(14) Uiso 1 1 d . . .
C4 C 0.7101(3) 0.2659(4) 0.7234(3) 0.0343(12) Uani 1 1 d . . .
H4 H 0.686(3) 0.326(3) 0.738(3) 0.022(12) Uiso 1 1 d . . .
C5 C 0.7370(3) 0.2573(3) 0.6206(3) 0.0367(12) Uani 1 1 d . . .
C6 C 0.7126(4) 0.1689(4) 0.5609(3) 0.0465(13) Uani 1 1 d . . .
H6 H 0.6770 0.1117 0.5867 0.056 Uiso 1 1 calc R . .
C7 C 0.7403(4) 0.1640(4) 0.4635(4) 0.0588(15) Uani 1 1 d . . .
H7 H 0.7232 0.1039 0.4248 0.071 Uiso 1 1 calc R . .
C8 C 0.7928(4) 0.2471(4) 0.4242(4) 0.0583(16) Uani 1 1 d . . .
H8 H 0.8120 0.2434 0.3591 0.070 Uiso 1 1 calc R . .
C9 C 0.8173(4) 0.3366(4) 0.4815(4) 0.0546(14) Uani 1 1 d . . .
H9 H 0.8522 0.3938 0.4550 0.065 Uiso 1 1 calc R . .
C10 C 0.7897(4) 0.3406(4) 0.5784(3) 0.0489(14) Uani 1 1 d . . .
H10 H 0.8069 0.4009 0.6166 0.059 Uiso 1 1 calc R . .
C11 C 0.5697(5) 0.3796(5) 0.9332(5) 0.0592(17) Uani 1 1 d . . .
H11A H 0.598(3) 0.433(3) 0.972(3) 0.042(16) Uiso 1 1 d . . .
H11B H 0.505(3) 0.397(3) 0.892(3) 0.040(13) Uiso 1 1 d . . .
C12 C 0.7317(4) 0.1366(3) 1.0554(3) 0.0472(13) Uani 1 1 d . . .
H12 H 0.7185 0.0781 1.0077 0.057 Uiso 1 1 calc R . .
C13 C 0.6300(4) 0.1410(4) 1.1112(3) 0.0656(16) Uani 1 1 d . . .
H13A H 0.6090 0.0704 1.1276 0.098 Uiso 1 1 calc R . .
H13B H 0.5717 0.1741 1.0696 0.098 Uiso 1 1 calc R . .
H13C H 0.6454 0.1814 1.1716 0.098 Uiso 1 1 calc R . .
C14 C 0.8321(4) 0.1036(4) 1.1237(3) 0.0695(17) Uani 1 1 d . . .
H14A H 0.8397 0.1484 1.1817 0.104 Uiso 1 1 calc R . .
H14B H 0.8956 0.1102 1.0884 0.104 Uiso 1 1 calc R . .
H14C H 0.8244 0.0312 1.1440 0.104 Uiso 1 1 calc R . .
C15 C 0.8073(4) 0.3652(3) 1.0594(3) 0.0463(13) Uani 1 1 d . . .
H15 H 0.7948 0.4295 1.0189 0.056 Uiso 1 1 calc R . .
C16 C 0.7483(4) 0.3837(4) 1.1519(3) 0.0709(18) Uani 1 1 d . . .
H16A H 0.7619 0.3252 1.1972 0.106 Uiso 1 1 calc R . .
H16B H 0.6714 0.3895 1.1325 0.106 Uiso 1 1 calc R . .
H16C H 0.7744 0.4480 1.1842 0.106 Uiso 1 1 calc R . .
C17 C 0.9311(4) 0.3593(4) 1.0860(3) 0.0690(17) Uani 1 1 d . . .
H17A H 0.9558 0.4220 1.1219 0.104 Uiso 1 1 calc R . .
H17B H 0.9664 0.3541 1.0257 0.104 Uiso 1 1 calc R . .
H17C H 0.9487 0.2980 1.1269 0.104 Uiso 1 1 calc R . .
C18 C 0.9057(4) 0.0602(4) 0.8757(4) 0.0532(14) Uani 1 1 d . . .
H18 H 0.8716 0.0161 0.9184 0.064 Uiso 1 1 calc R . .
C19 C 0.9898(4) 0.1328(4) 0.9042(4) 0.0484(14) Uani 1 1 d . . .
H19 H 1.0214 0.1458 0.9688 0.058 Uiso 1 1 calc R . .
C20 C 1.0173(4) 0.1823(4) 0.8151(4) 0.0524(14) Uani 1 1 d . . .
H20 H 1.0711 0.2335 0.8122 0.063 Uiso 1 1 calc R . .
C21 C 0.9512(4) 0.1424(4) 0.7325(4) 0.0472(13) Uani 1 1 d . . .
H21 H 0.9524 0.1620 0.6659 0.057 Uiso 1 1 calc R . .
C22 C 0.8824(4) 0.0664(4) 0.7711(4) 0.0538(15) Uani 1 1 d . . .
H22 H 0.8298 0.0266 0.7331 0.065 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os 0.03366(10) 0.03158(10) 0.03445(10) -0.00006(11) 0.00445(7) 0.00095(11)
Cl 0.0605(9) 0.0351(7) 0.0533(9) 0.0003(6) 0.0042(7) -0.0115(6)
P 0.0422(8) 0.0361(8) 0.0346(7) -0.0007(6) 0.0059(6) 0.0007(6)
C1 0.039(3) 0.047(3) 0.042(3) 0.001(3) 0.010(2) 0.002(3)
C2 0.039(3) 0.061(4) 0.046(3) -0.001(3) 0.003(3) -0.007(3)
C3 0.032(3) 0.042(3) 0.036(3) -0.002(2) 0.002(2) 0.000(2)
C4 0.029(3) 0.033(3) 0.040(3) -0.008(2) 0.000(2) 0.004(2)
C5 0.028(3) 0.040(3) 0.040(3) 0.009(2) -0.005(2) 0.001(2)
C6 0.050(3) 0.047(3) 0.042(3) 0.002(3) 0.005(3) -0.005(3)
C7 0.083(4) 0.060(4) 0.034(3) -0.004(3) 0.006(3) 0.009(3)
C8 0.072(4) 0.064(4) 0.041(3) 0.014(3) 0.014(3) 0.020(3)
C9 0.059(4) 0.058(4) 0.047(4) 0.018(3) 0.003(3) -0.004(3)
C10 0.058(4) 0.052(3) 0.037(3) 0.009(3) 0.007(3) 0.001(3)
C11 0.047(4) 0.068(5) 0.062(5) -0.005(4) 0.001(3) 0.015(4)
C12 0.062(4) 0.034(3) 0.048(3) 0.004(2) 0.015(3) 0.004(3)
C13 0.081(4) 0.065(4) 0.057(4) 0.004(3) 0.032(3) 0.000(3)
C14 0.093(5) 0.067(4) 0.050(4) 0.020(3) 0.015(3) 0.023(3)
C15 0.064(4) 0.041(3) 0.034(3) -0.009(2) 0.007(3) 0.000(3)
C16 0.114(5) 0.061(4) 0.040(4) -0.016(3) 0.022(3) -0.009(3)
C17 0.060(4) 0.090(4) 0.053(4) -0.011(3) -0.016(3) -0.020(3)
C18 0.061(4) 0.045(3) 0.057(4) -0.002(3) 0.023(3) 0.008(3)
C19 0.045(3) 0.054(4) 0.047(4) -0.004(3) 0.003(3) 0.017(3)
C20 0.031(3) 0.059(4) 0.069(4) -0.005(3) 0.014(3) 0.011(3)
C21 0.041(3) 0.059(4) 0.043(3) 0.000(3) 0.006(3) 0.013(3)
C22 0.054(4) 0.035(3) 0.072(4) -0.010(3) 0.005(3) -0.001(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 Os C18 37.85(16) . . ?
C22 Os C4 99.09(18) . . ?
C18 Os C4 131.09(19) . . ?
C22 Os C3 87.15(18) . . ?
C18 Os C3 103.01(19) . . ?
C4 Os C3 37.78(15) . . ?
C22 Os C19 62.08(18) . . ?
C18 Os C19 37.18(15) . . ?
C4 Os C19 159.13(17) . . ?
C3 Os C19 140.09(19) . . ?
C22 Os C21 37.20(15) . . ?
C18 Os C21 62.73(17) . . ?
C4 Os C21 97.88(17) . . ?
C3 Os C21 108.92(18) . . ?
C19 Os C21 61.87(16) . . ?
C22 Os C20 60.71(18) . . ?
C18 Os C20 61.40(18) . . ?
C4 Os C20 127.78(18) . . ?
C3 Os C20 144.56(17) . . ?
C19 Os C20 36.71(14) . . ?
C21 Os C20 36.02(14) . . ?
C22 Os P 131.66(15) . . ?
C18 Os P 100.42(13) . . ?
C4 Os P 98.56(12) . . ?
C3 Os P 80.18(12) . . ?
C19 Os P 100.95(13) . . ?
C21 Os P 161.91(12) . . ?
C20 Os P 131.68(13) . . ?
C22 Os Cl 139.54(14) . . ?
C18 Os Cl 142.95(14) . . ?
C4 Os Cl 82.31(12) . . ?
C3 Os Cl 114.03(13) . . ?
C19 Os Cl 105.85(14) . . ?
C21 Os Cl 102.36(13) . . ?
C20 Os Cl 86.36(13) . . ?
P Os Cl 87.30(4) . . ?
C1 P C15 107.2(2) . . ?
C1 P C12 102.9(2) . . ?
C15 P C12 109.1(2) . . ?
C1 P Os 102.17(15) . . ?
C15 P Os 119.63(15) . . ?
C12 P Os 113.95(15) . . ?
C11 C1 C2 124.5(5) . . ?
C11 C1 P 127.6(5) . . ?
C2 C1 P 106.9(4) . . ?
C1 C2 C3 111.1(4) . . ?
C1 C2 H2A 107(2) . . ?
C3 C2 H2A 112(2) . . ?
C1 C2 H2B 112(2) . . ?
C3 C2 H2B 109(2) . . ?
H2A C2 H2B 105(3) . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 Os 70.4(3) . . ?
C2 C3 Os 117.1(3) . . ?
C4 C3 H3 119(2) . . ?
C2 C3 H3 116(2) . . ?
Os C3 H3 105(2) . . ?
C3 C4 C5 125.2(4) . . ?
C3 C4 Os 71.8(3) . . ?
C5 C4 Os 114.6(3) . . ?
C3 C4 H4 113(3) . . ?
C5 C4 H4 114(3) . . ?
Os C4 H4 110(2) . . ?
C10 C5 C6 117.0(5) . . ?
C10 C5 C4 119.6(4) . . ?
C6 C5 C4 123.4(4) . . ?
C7 C6 C5 121.4(5) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C8 C7 C6 120.2(5) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.7(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 119.6(5) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C5 122.0(5) . . ?
C9 C10 H10 119.0 . . ?
C5 C10 H10 119.0 . . ?
C1 C11 H11A 123(3) . . ?
C1 C11 H11B 121(2) . . ?
H11A C11 H11B 115(4) . . ?
C14 C12 C13 111.9(4) . . ?
C14 C12 P 113.1(3) . . ?
C13 C12 P 115.8(3) . . ?
C14 C12 H12 105.0 . . ?
C13 C12 H12 105.0 . . ?
P C12 H12 105.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 111.4(4) . . ?
C16 C15 P 116.1(3) . . ?
C17 C15 P 112.0(3) . . ?
C16 C15 H15 105.4 . . ?
C17 C15 H15 105.4 . . ?
P C15 H15 105.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C22 107.7(5) . . ?
C19 C18 Os 73.9(3) . . ?
C22 C18 Os 71.0(3) . . ?
C19 C18 H18 126.1 . . ?
C22 C18 H18 126.1 . . ?
Os C18 H18 120.7 . . ?
C18 C19 C20 106.9(5) . . ?
C18 C19 Os 68.9(3) . . ?
C20 C19 Os 73.1(3) . . ?
C18 C19 H19 126.6 . . ?
C20 C19 H19 126.6 . . ?
Os C19 H19 123.1 . . ?
C21 C20 C19 109.9(5) . . ?
C21 C20 Os 71.3(3) . . ?
C19 C20 Os 70.2(3) . . ?
C21 C20 H20 125.1 . . ?
C19 C20 H20 125.1 . . ?
Os C20 H20 125.0 . . ?
C20 C21 C22 106.0(5) . . ?
C20 C21 Os 72.7(3) . . ?
C22 C21 Os 68.1(3) . . ?
C20 C21 H21 127.0 . . ?
C22 C21 H21 127.0 . . ?
Os C21 H21 123.9 . . ?
C18 C22 C21 109.6(5) . . ?
C18 C22 Os 71.1(3) . . ?
C21 C22 Os 74.7(3) . . ?
C18 C22 H22 125.2 . . ?
C21 C22 H22 125.2 . . ?
Os C22 H22 120.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C22 2.170(4) . ?
Os C18 2.171(5) . ?
Os C4 2.184(4) . ?
Os C3 2.203(4) . ?
Os C19 2.236(4) . ?
Os C21 2.256(4) . ?
Os C20 2.274(4) . ?
Os P 2.2990(12) . ?
Os Cl 2.4268(11) . ?
P C1 1.810(4) . ?
P C15 1.850(4) . ?
P C12 1.867(4) . ?
C1 C11 1.296(6) . ?
C1 C2 1.506(6) . ?
C2 C3 1.529(6) . ?
C2 H2A 1.11(4) . ?
C2 H2B 0.98(3) . ?
C3 C4 1.421(6) . ?
C3 H3 0.99(3) . ?
C4 C5 1.456(6) . ?
C4 H4 0.85(3) . ?
C5 C10 1.387(5) . ?
C5 C6 1.389(5) . ?
C6 C7 1.388(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.90(4) . ?
C11 H11B 0.95(4) . ?
C12 C14 1.522(6) . ?
C12 C13 1.528(5) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.522(5) . ?
C15 C17 1.533(6) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.406(6) . ?
C18 C22 1.408(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.421(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.400(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.414(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
|
1100877.cif | #------------------------------------------------------------------------------
#$Date: 2019-10-02 14:34:28 +0300 (Wed, 02 Oct 2019) $
#$Revision: 219028 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100877.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100877
loop_
_publ_author_name
'Baya, Miguel'
'Buil, Mar\'ia L.'
'Esteruelas, Miguel A.'
'O\~nate, Enrique'
_publ_section_title
;
Ene-Type Reactions between an \a-Alkenylphosphine and Terminal Alkynes
Promoted by Osmium-Cyclopentadienyl Fragments
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2030
_journal_page_last 2038
_journal_paper_doi 10.1021/om0489857
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C24.5 H34 Cl Os P'
_chemical_formula_weight 585.14
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 103.7850(10)
_cell_angle_beta 95.9700(10)
_cell_angle_gamma 91.4870(10)
_cell_formula_units_Z 2
_cell_length_a 7.6298(5)
_cell_length_b 11.3416(7)
_cell_length_c 14.0086(8)
_cell_measurement_reflns_used 6550
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27
_cell_measurement_theta_min 2.5
_cell_volume 1169.30(12)
_computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\w rotations with narrow frames'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0283
_diffrn_reflns_av_sigmaI/netI 0.0491
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 14372
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.64
_diffrn_reflns_theta_min 1.51
_diffrn_standards_decay_% 'no decay'
_exptl_absorpt_coefficient_mu 5.643
_exptl_absorpt_correction_T_max 0.526
_exptl_absorpt_correction_T_min 0.396
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
SADABS: Area-Detector Absorption Correction. Bruker-AXS
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.662
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 578
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.16
_refine_diff_density_max 1.844
_refine_diff_density_min -0.706
_refine_diff_density_rms 0.132
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.002
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 257
_refine_ls_number_reflns 5449
_refine_ls_number_restraints 7
_refine_ls_restrained_S_all 1.009
_refine_ls_R_factor_all 0.0321
_refine_ls_R_factor_gt 0.0285
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0627
_refine_ls_wR_factor_ref 0.0636
_reflns_number_gt 4917
_reflns_number_total 5449
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060293
_cod_depositor_comments
;
Updated bibliographic information.
Antanas Vaitkus,
2019-10-02
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.21702(2) 0.115328(15) 0.188806(12) 0.02046(6) Uani 1 1 d . A .
Cl Cl -0.05632(13) 0.21374(11) 0.19494(9) 0.0330(3) Uani 1 1 d . . .
P P 0.29625(14) 0.21829(10) 0.35097(8) 0.0217(2) Uani 1 1 d . . .
C1 C 0.1706(5) -0.0208(4) 0.2307(3) 0.0267(10) Uani 1 1 d . . .
C2 C 0.1558(6) -0.1289(4) 0.2511(3) 0.0270(10) Uani 1 1 d . A .
H2 H 0.258(5) -0.162(4) 0.275(3) 0.026(12) Uiso 1 1 d . . .
C3 C -0.0080(6) -0.2020(4) 0.2425(3) 0.0257(9) Uani 1 1 d . . .
C4 C -0.0036(6) -0.3209(4) 0.2531(4) 0.0365(11) Uani 1 1 d . A .
H4 H 0.1071 -0.3525 0.2685 0.044 Uiso 1 1 calc R . .
C5 C -0.1551(7) -0.3941(5) 0.2419(4) 0.0438(13) Uani 1 1 d . . .
H5 H -0.1478 -0.4755 0.2483 0.053 Uiso 1 1 calc R A .
C6 C -0.3145(7) -0.3497(4) 0.2218(4) 0.0386(12) Uani 1 1 d . A .
H6 H -0.4192 -0.3997 0.2146 0.046 Uiso 1 1 calc R . .
C7 C -0.3246(6) -0.2314(4) 0.2116(3) 0.0353(11) Uani 1 1 d . . .
H7 H -0.4364 -0.2004 0.1976 0.042 Uiso 1 1 calc R A .
C8 C -0.1731(6) -0.1583(4) 0.2218(3) 0.0288(10) Uani 1 1 d . A .
H8 H -0.1815 -0.0774 0.2146 0.035 Uiso 1 1 calc R . .
C9 C 0.3958(6) 0.3734(4) 0.3707(3) 0.0307(10) Uani 1 1 d . A .
H9 H 0.4042 0.4116 0.4433 0.037 Uiso 1 1 calc R . .
C10 C 0.5802(6) 0.3759(4) 0.3413(4) 0.0367(11) Uani 1 1 d . . .
H10A H 0.5771 0.3398 0.2702 0.055 Uiso 1 1 calc R A .
H10B H 0.6555 0.3293 0.3781 0.055 Uiso 1 1 calc R . .
H10C H 0.6278 0.4602 0.3564 0.055 Uiso 1 1 calc R . .
C11 C 0.2792(6) 0.4513(4) 0.3186(4) 0.0359(11) Uani 1 1 d . . .
H11A H 0.3328 0.5340 0.3331 0.054 Uiso 1 1 calc R A .
H11B H 0.1624 0.4537 0.3420 0.054 Uiso 1 1 calc R . .
H11C H 0.2673 0.4162 0.2470 0.054 Uiso 1 1 calc R . .
C12 C 0.4598(6) 0.1448(4) 0.4204(3) 0.0308(10) Uani 1 1 d . A .
C13 C 0.5265(7) 0.2130(5) 0.5243(3) 0.0395(12) Uani 1 1 d . . .
H13A H 0.6102 0.1640 0.5539 0.059 Uiso 1 1 calc R A .
H13B H 0.4271 0.2291 0.5637 0.059 Uiso 1 1 calc R . .
H13C H 0.5858 0.2902 0.5230 0.059 Uiso 1 1 calc R . .
C14 C 0.5561(9) 0.0586(6) 0.3720(5) 0.062(2) Uani 1 1 d . . .
H14A H 0.633(6) 0.025(4) 0.406(3) 0.033(13) Uiso 1 1 d . . .
H14B H 0.525(6) 0.019(4) 0.308(4) 0.040(14) Uiso 1 1 d . . .
C15A C 0.1031(12) 0.2385(7) 0.4241(6) 0.029(2) Uiso 0.74(2) 1 d PD A 1
C16A C 0.1074(13) 0.3494(7) 0.5059(7) 0.043(2) Uiso 0.74(2) 1 d PD A 1
C17A C 0.0602(12) 0.1193(6) 0.4564(7) 0.038(2) Uiso 0.74(2) 1 d PD A 1
C15B C 0.141(3) 0.2328(17) 0.4438(18) 0.029(6) Uiso 0.26(2) 1 d PD A 2
C16B C -0.001(2) 0.1307(14) 0.4257(14) 0.021(5) Uiso 0.26(2) 1 d PD A 2
C17B C 0.061(3) 0.3526(15) 0.4801(18) 0.030(6) Uiso 0.26(2) 1 d PD A 2
C18 C 0.3838(5) 0.0102(4) 0.0844(3) 0.0278(10) Uani 1 1 d . . .
H18 H 0.4209 -0.0667 0.0920 0.033 Uiso 1 1 calc R A .
C19 C 0.2329(6) 0.0301(4) 0.0247(3) 0.0316(11) Uani 1 1 d . A .
H19 H 0.1496 -0.0303 -0.0148 0.038 Uiso 1 1 calc R . .
C20 C 0.2289(6) 0.1560(5) 0.0347(3) 0.0352(11) Uani 1 1 d . . .
H20 H 0.1398 0.1955 0.0034 0.042 Uiso 1 1 calc R A .
C21 C 0.3757(6) 0.2148(4) 0.0978(3) 0.0337(11) Uani 1 1 d . A .
H21 H 0.4055 0.2996 0.1149 0.040 Uiso 1 1 calc R . .
C22 C 0.4716(5) 0.1247(4) 0.1315(3) 0.0305(10) Uani 1 1 d . A .
H22 H 0.5756 0.1381 0.1771 0.037 Uiso 1 1 calc R . .
C23 C 1.0000 0.5000 1.0000 0.076(3) Uiso 1 2 d SD . .
C24A C 0.8086(11) 0.4667(9) 0.9757(8) 0.046(3) Uiso 0.50 1 d PD . .
C25A C 0.7210(15) 0.3524(10) 0.9864(9) 0.049(3) Uiso 0.50 1 d PD . .
C24B C 0.8933(13) 0.3982(10) 1.0005(10) 0.065(3) Uiso 0.50 1 d PD . .
C25B C 0.7014(15) 0.4031(14) 0.9694(10) 0.063(4) Uiso 0.50 1 d PD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os 0.01852(9) 0.02152(10) 0.02139(9) 0.00522(6) 0.00296(6) -0.00098(6)
Cl 0.0207(5) 0.0354(6) 0.0418(7) 0.0086(5) -0.0001(5) 0.0041(4)
P 0.0248(5) 0.0176(5) 0.0230(6) 0.0046(4) 0.0051(4) -0.0002(4)
C1 0.019(2) 0.033(3) 0.023(2) -0.0024(19) -0.0001(17) -0.0023(18)
C2 0.029(2) 0.023(2) 0.030(2) 0.0072(19) 0.0053(19) 0.0032(19)
C3 0.034(2) 0.021(2) 0.023(2) 0.0051(18) 0.0082(18) -0.0002(18)
C4 0.038(3) 0.032(3) 0.044(3) 0.016(2) 0.007(2) 0.005(2)
C5 0.051(3) 0.028(3) 0.056(3) 0.017(3) 0.009(3) -0.004(2)
C6 0.042(3) 0.031(3) 0.044(3) 0.009(2) 0.010(2) -0.009(2)
C7 0.032(2) 0.036(3) 0.038(3) 0.009(2) 0.004(2) -0.001(2)
C8 0.033(2) 0.024(2) 0.031(2) 0.009(2) 0.007(2) 0.0009(19)
C9 0.039(3) 0.020(2) 0.031(2) 0.0041(19) 0.002(2) -0.0065(19)
C10 0.039(3) 0.027(3) 0.043(3) 0.008(2) 0.006(2) -0.010(2)
C11 0.050(3) 0.020(2) 0.039(3) 0.010(2) 0.007(2) 0.000(2)
C12 0.036(3) 0.033(3) 0.025(2) 0.010(2) 0.0004(19) 0.005(2)
C13 0.047(3) 0.037(3) 0.031(3) 0.007(2) -0.008(2) -0.003(2)
C14 0.078(5) 0.050(4) 0.044(4) -0.004(3) -0.030(3) 0.032(3)
C18 0.029(2) 0.032(3) 0.022(2) 0.0027(19) 0.0098(18) 0.0035(19)
C19 0.026(2) 0.045(3) 0.020(2) 0.000(2) 0.0048(18) -0.004(2)
C20 0.038(3) 0.050(3) 0.024(2) 0.018(2) 0.010(2) 0.007(2)
C21 0.045(3) 0.031(3) 0.029(2) 0.010(2) 0.017(2) -0.006(2)
C22 0.020(2) 0.043(3) 0.027(2) 0.005(2) 0.0077(18) -0.0052(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os C22 115.37(18) . . ?
C1 Os C18 88.99(18) . . ?
C22 Os C18 37.90(16) . . ?
C1 Os C19 99.76(18) . . ?
C22 Os C19 61.68(16) . . ?
C18 Os C19 36.50(15) . . ?
C1 Os C21 149.59(18) . . ?
C22 Os C21 36.59(16) . . ?
C18 Os C21 61.05(17) . . ?
C19 Os C21 59.89(17) . . ?
C1 Os P 89.05(13) . . ?
C22 Os P 99.47(12) . . ?
C18 Os P 128.15(12) . . ?
C19 Os P 161.13(11) . . ?
C21 Os P 104.90(12) . . ?
C1 Os C20 134.30(18) . . ?
C22 Os C20 60.23(17) . . ?
C18 Os C20 59.89(17) . . ?
C19 Os C20 35.42(16) . . ?
C21 Os C20 35.19(16) . . ?
P Os C20 136.11(13) . . ?
C1 Os Cl 103.35(13) . . ?
C22 Os Cl 140.45(13) . . ?
C18 Os Cl 141.89(12) . . ?
C19 Os Cl 105.41(12) . . ?
C21 Os Cl 103.90(13) . . ?
P Os Cl 88.51(4) . . ?
C20 Os Cl 87.33(12) . . ?
C15B P C12 93.6(8) . . ?
C15B P C9 104.1(6) . . ?
C12 P C9 102.8(2) . . ?
C15B P C15A 12.3(8) . . ?
C12 P C15A 105.3(3) . . ?
C9 P C15A 104.3(3) . . ?
C15B P Os 121.7(7) . . ?
C12 P Os 114.99(15) . . ?
C9 P Os 116.05(15) . . ?
C15A P Os 112.1(3) . . ?
C2 C1 Os 170.4(4) . . ?
C1 C2 C3 125.9(4) . . ?
C1 C2 H2 119(3) . . ?
C3 C2 H2 115(3) . . ?
C4 C3 C8 117.3(4) . . ?
C4 C3 C2 120.3(4) . . ?
C8 C3 C2 122.4(4) . . ?
C5 C4 C3 121.9(5) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C3 120.6(4) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C10 C9 C11 110.3(4) . . ?
C10 C9 P 113.3(3) . . ?
C11 C9 P 111.5(3) . . ?
C10 C9 H9 107.1 . . ?
C11 C9 H9 107.1 . . ?
P C9 H9 107.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 119.3(4) . . ?
C14 C12 P 120.0(4) . . ?
C13 C12 P 117.1(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 119(3) . . ?
C12 C14 H14B 122(3) . . ?
H14A C14 H14B 116(4) . . ?
C16A C15A C17A 113.1(7) . . ?
C16A C15A P 117.1(6) . . ?
C17A C15A P 109.9(6) . . ?
C17B C15B C16B 109.2(15) . . ?
C17B C15B P 119.7(15) . . ?
C16B C15B P 115.8(14) . . ?
C19 C18 C22 108.5(4) . . ?
C19 C18 Os 75.4(2) . . ?
C22 C18 Os 70.8(2) . . ?
C19 C18 H18 125.8 . . ?
C22 C18 H18 125.8 . . ?
Os C18 H18 119.8 . . ?
C20 C19 C18 106.9(4) . . ?
C20 C19 Os 73.6(3) . . ?
C18 C19 Os 68.1(2) . . ?
C20 C19 H19 126.5 . . ?
C18 C19 H19 126.5 . . ?
Os C19 H19 123.4 . . ?
C21 C20 C19 109.8(4) . . ?
C21 C20 Os 71.6(2) . . ?
C19 C20 Os 71.0(2) . . ?
C21 C20 H20 125.1 . . ?
C19 C20 H20 125.1 . . ?
Os C20 H20 123.9 . . ?
C20 C21 C22 107.4(4) . . ?
C20 C21 Os 73.2(3) . . ?
C22 C21 Os 67.3(2) . . ?
C20 C21 H21 126.3 . . ?
C22 C21 H21 126.3 . . ?
Os C21 H21 124.7 . . ?
C21 C22 C18 107.4(4) . . ?
C21 C22 Os 76.1(2) . . ?
C18 C22 Os 71.3(2) . . ?
C21 C22 H22 126.3 . . ?
C18 C22 H22 126.3 . . ?
Os C22 H22 118.2 . . ?
C24B C23 C24B 180.000(2) 2_767 . ?
C24B C23 C24A 45.6(6) 2_767 2_767 ?
C24B C23 C24A 134.4(6) . 2_767 ?
C24B C23 C24A 134.4(6) 2_767 . ?
C24B C23 C24A 45.6(6) . . ?
C24A C23 C24A 180.000(2) 2_767 . ?
C25B C24A C24B 86.3(9) . . ?
C25B C24A C23 149.5(11) . . ?
C24B C24A C23 63.2(6) . . ?
C25B C24A C25A 24.6(8) . . ?
C24B C24A C25A 61.8(8) . . ?
C23 C24A C25A 125.0(8) . . ?
C25B C25A C24B 85.4(13) . . ?
C25B C25A C24A 39.9(12) . . ?
C24B C25A C24A 45.7(6) . . ?
C24A C24B C25A 72.5(8) . . ?
C24A C24B C23 71.2(7) . . ?
C25A C24B C23 143.6(10) . . ?
C24A C24B C25B 45.2(7) . . ?
C25A C24B C25B 27.4(6) . . ?
C23 C24B C25B 116.4(10) . . ?
C25A C25B C24A 115.5(17) . . ?
C25A C25B C24B 67.2(13) . . ?
C24A C25B C24B 48.5(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C1 1.817(5) . ?
Os C22 2.188(4) . ?
Os C18 2.195(4) . ?
Os C19 2.289(4) . ?
Os C21 2.302(4) . ?
Os P 2.3028(11) . ?
Os C20 2.322(4) . ?
Os Cl 2.3906(10) . ?
P C15B 1.83(2) . ?
P C12 1.840(4) . ?
P C9 1.845(4) . ?
P C15A 1.869(8) . ?
C1 C2 1.328(6) . ?
C2 C3 1.460(6) . ?
C2 H2 0.94(4) . ?
C3 C4 1.392(6) . ?
C3 C8 1.394(6) . ?
C4 C5 1.379(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.357(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.508(6) . ?
C9 C11 1.523(6) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.334(7) . ?
C12 C13 1.505(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.87(5) . ?
C14 H14B 0.90(5) . ?
C15A C16A 1.483(10) . ?
C15A C17A 1.562(11) . ?
C15B C17B 1.503(19) . ?
C15B C16B 1.521(19) . ?
C18 C19 1.407(6) . ?
C18 C22 1.423(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.403(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.413(6) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24B 1.398(9) 2_767 ?
C23 C24B 1.398(9) . ?
C23 C24A 1.483(8) 2_767 ?
C23 C24A 1.483(8) . ?
C24A C25B 1.059(14) . ?
C24A C24B 1.119(15) . ?
C24A C25A 1.490(9) . ?
C25A C25B 0.687(16) . ?
C25A C24B 1.378(14) . ?
C24B C25B 1.490(10) . ?
|
1100878.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100878.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100878
loop_
_publ_author_name
'Osintseva, Svetlana V.'
'Dolgushin, Fedor M.'
'Shtel'tser, Nikolay A.'
'Petrovskii, Pavel V.'
'Kreindlin, Arkadii Z.'
'Rybin, Leonid V.'
'Antipin, Mikhail Yu.'
_publ_section_title
;
Reaction of Ru <sub>3</sub> (CO) <sub>12</sub> with Dibenzylideneacetone
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2279
_journal_page_last 2288
_journal_paper_doi 10.1021/om0489958
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C40 H26 O8 Ru3, 0.5(C6 H14)'
_chemical_formula_sum 'C43 H33 O8 Ru3'
_chemical_formula_weight 980.90
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.92(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.120(4)
_cell_length_b 24.452(7)
_cell_length_c 11.080(3)
_cell_measurement_reflns_used 24
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 12
_cell_measurement_theta_min 10
_cell_volume 3825(2)
_diffrn_ambient_temperature 153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Syntex P2(1)'
_diffrn_measurement_method \q/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0503
_diffrn_reflns_av_sigmaI/netI 0.1077
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -3
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 3512
_diffrn_reflns_theta_max 25.05
_diffrn_reflns_theta_min 2.46
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time ?
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 1.223
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.703
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1948
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.917
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 292
_refine_ls_number_reflns 3368
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.917
_refine_ls_R_factor_all 0.0721
_refine_ls_R_factor_gt 0.0367
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0788
_refine_ls_wR_factor_ref 0.0827
_reflns_number_gt 2483
_reflns_number_total 3368
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.0000 0.24547(2) 0.7500 0.01729(14) Uani 1 2 d S . .
Ru2 Ru -0.01659(3) 0.321935(15) 0.94145(3) 0.01717(12) Uani 1 1 d . . .
O1 O -0.0787(3) 0.15683(17) 0.9116(4) 0.0479(11) Uani 1 1 d . . .
O2 O -0.1472(3) 0.25565(16) 1.0944(4) 0.0391(10) Uani 1 1 d . . .
O3 O 0.0749(3) 0.3759(2) 1.1609(4) 0.0619(14) Uani 1 1 d . . .
O4 O 0.0691(2) 0.36654(12) 0.8254(3) 0.0184(7) Uani 1 1 d . . .
C1 C -0.0511(4) 0.1901(2) 0.8505(5) 0.0285(12) Uani 1 1 d . . .
C2 C -0.0957(4) 0.2802(2) 1.0377(5) 0.0249(11) Uani 1 1 d . . .
C3 C 0.0403(4) 0.3561(2) 1.0784(5) 0.0307(12) Uani 1 1 d . . .
C4 C 0.1180(3) 0.33294(18) 0.7603(4) 0.0183(10) Uani 1 1 d . . .
C5 C 0.1398(3) 0.27922(19) 0.8105(4) 0.0167(10) Uani 1 1 d . . .
C6 C 0.0891(3) 0.26430(18) 0.9131(4) 0.0179(10) Uani 1 1 d . . .
C7 C 0.1229(3) 0.21784(19) 0.9924(4) 0.0177(10) Uani 1 1 d . . .
C8 C 0.1815(3) 0.1770(2) 0.9475(4) 0.0233(11) Uani 1 1 d . . .
C9 C 0.2081(4) 0.1325(2) 1.0169(5) 0.0287(12) Uani 1 1 d . . .
C10 C 0.1775(4) 0.1280(2) 1.1343(5) 0.0265(12) Uani 1 1 d . . .
C11 C 0.1225(4) 0.1684(2) 1.1815(5) 0.0266(12) Uani 1 1 d . . .
C12 C 0.0949(3) 0.2135(2) 1.1116(4) 0.0218(11) Uani 1 1 d . . .
C13 C 0.1542(3) 0.35122(19) 0.6448(4) 0.0187(10) Uani 1 1 d . . .
C14 C 0.1166(3) 0.3978(2) 0.5884(4) 0.0213(10) Uani 1 1 d . . .
C15 C 0.1559(3) 0.42609(19) 0.4835(4) 0.0206(10) Uani 1 1 d . . .
C16 C 0.1272(4) 0.4793(2) 0.4590(5) 0.0294(12) Uani 1 1 d . . .
C17 C 0.1589(4) 0.5074(2) 0.3586(5) 0.0312(13) Uani 1 1 d . . .
C18 C 0.2232(4) 0.4829(2) 0.2835(5) 0.0325(13) Uani 1 1 d . . .
C19 C 0.2543(4) 0.4304(2) 0.3080(5) 0.0310(13) Uani 1 1 d . . .
C20 C 0.2209(4) 0.4022(2) 0.4069(4) 0.0239(11) Uani 1 1 d . . .
H5 H 0.190(4) 0.2601(19) 0.780(4) 0.024(14) Uiso 1 1 d . . .
H8 H 0.202(3) 0.1808(18) 0.869(4) 0.014(12) Uiso 1 1 d . . .
H9 H 0.247(3) 0.105(2) 0.981(4) 0.022(13) Uiso 1 1 d . . .
H10 H 0.200(4) 0.099(2) 1.177(5) 0.036(15) Uiso 1 1 d . . .
H11 H 0.101(3) 0.1671(18) 1.252(4) 0.016(13) Uiso 1 1 d . . .
H12 H 0.055(3) 0.2441(17) 1.145(4) 0.009(10) Uiso 1 1 d . . .
H13 H 0.205(3) 0.3287(18) 0.613(4) 0.012(11) Uiso 1 1 d . . .
H14 H 0.077(4) 0.420(2) 0.629(4) 0.024(14) Uiso 1 1 d . . .
H16 H 0.077(3) 0.4940(18) 0.514(4) 0.018(12) Uiso 1 1 d . . .
H17 H 0.133(4) 0.544(2) 0.351(5) 0.045(17) Uiso 1 1 d . . .
H18 H 0.243(4) 0.499(2) 0.210(5) 0.045(17) Uiso 1 1 d . . .
H19 H 0.295(3) 0.4133(18) 0.252(4) 0.020(13) Uiso 1 1 d . . .
H20 H 0.237(3) 0.3670(18) 0.413(4) 0.008(11) Uiso 1 1 d . . .
C1S C -0.006(2) 0.0109(10) 1.185(2) 0.212(12) Uiso 0.75 1 d P . .
C2S C -0.026(3) 0.0001(16) 1.087(4) 0.200(15) Uiso 0.50 1 d P . .
C3S C 0.0000 0.0000 1.0000 0.22(3) Uiso 0.50 2 d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0161(3) 0.0156(3) 0.0200(3) 0.000 -0.0049(2) 0.000
Ru2 0.0152(2) 0.0176(2) 0.0187(2) 0.00047(16) -0.00225(14) 0.00045(16)
O1 0.042(3) 0.043(2) 0.058(3) 0.026(2) -0.014(2) -0.021(2)
O2 0.031(2) 0.045(2) 0.041(2) 0.022(2) 0.0054(18) -0.0022(19)
O3 0.043(3) 0.106(4) 0.036(3) -0.031(3) -0.005(2) -0.018(3)
O4 0.0212(17) 0.0126(16) 0.0215(17) 0.0004(13) -0.0016(14) 0.0002(14)
C1 0.021(3) 0.026(3) 0.038(3) 0.000(2) -0.013(2) -0.002(2)
C2 0.021(3) 0.024(3) 0.030(3) 0.004(2) -0.006(2) 0.006(2)
C3 0.021(3) 0.042(3) 0.029(3) -0.001(3) -0.002(2) -0.002(2)
C4 0.013(2) 0.016(2) 0.026(3) -0.004(2) -0.0049(19) -0.0059(19)
C5 0.012(2) 0.019(2) 0.019(2) -0.004(2) -0.0044(19) 0.001(2)
C6 0.017(2) 0.021(3) 0.016(2) -0.0059(19) -0.0056(19) -0.0025(19)
C7 0.012(2) 0.020(2) 0.020(2) -0.001(2) -0.0055(19) -0.0033(19)
C8 0.021(3) 0.031(3) 0.018(3) 0.002(2) -0.002(2) 0.001(2)
C9 0.026(3) 0.026(3) 0.034(3) 0.000(2) -0.006(2) 0.004(2)
C10 0.029(3) 0.017(3) 0.033(3) 0.001(2) -0.010(2) 0.001(2)
C11 0.025(3) 0.035(3) 0.020(3) 0.005(2) -0.003(2) -0.005(2)
C12 0.010(2) 0.028(3) 0.027(3) 0.000(2) -0.005(2) 0.001(2)
C13 0.016(2) 0.018(2) 0.022(3) 0.002(2) 0.000(2) -0.001(2)
C14 0.020(3) 0.015(2) 0.029(3) -0.001(2) 0.003(2) -0.005(2)
C15 0.016(2) 0.021(3) 0.024(3) 0.000(2) -0.004(2) -0.002(2)
C16 0.020(3) 0.027(3) 0.041(3) 0.001(2) -0.001(2) -0.002(2)
C17 0.032(3) 0.023(3) 0.038(3) 0.010(2) 0.001(3) 0.000(2)
C18 0.038(3) 0.028(3) 0.031(3) 0.012(2) -0.004(3) -0.008(3)
C19 0.029(3) 0.031(3) 0.034(3) -0.006(2) 0.000(2) -0.002(2)
C20 0.026(3) 0.019(3) 0.026(3) 0.001(2) 0.005(2) 0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100879.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100879.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100879
loop_
_publ_author_name
'Osintseva, Svetlana V.'
'Dolgushin, Fedor M.'
'Shtel'tser, Nikolay A.'
'Petrovskii, Pavel V.'
'Kreindlin, Arkadii Z.'
'Rybin, Leonid V.'
'Antipin, Mikhail Yu.'
_publ_section_title
;
Reaction of Ru <sub>3</sub> (CO) <sub>12</sub> with Dibenzylideneacetone
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2279
_journal_page_last 2288
_journal_paper_doi 10.1021/om0489958
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C75 H56 O11 Ru3'
_chemical_formula_weight 1436.41
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 88.432(3)
_cell_angle_beta 83.478(3)
_cell_angle_gamma 73.940(4)
_cell_formula_units_Z 2
_cell_length_a 10.6747(13)
_cell_length_b 12.9415(16)
_cell_length_c 23.694(3)
_cell_measurement_reflns_used 877
_cell_measurement_temperature 110(2)
_cell_measurement_theta_max 22.5
_cell_measurement_theta_min 2.2
_cell_volume 3125.1(7)
_diffrn_ambient_temperature 110(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0532
_diffrn_reflns_av_sigmaI/netI 0.1542
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 30794
_diffrn_reflns_theta_max 28.02
_diffrn_reflns_theta_min 1.85
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.779
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.526
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1452
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.946
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 802
_refine_ls_number_reflns 14876
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.946
_refine_ls_R_factor_all 0.1234
_refine_ls_R_factor_gt 0.0597
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1071
_refine_ls_wR_factor_ref 0.1187
_reflns_number_gt 7052
_reflns_number_total 14876
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100879
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.25168(4) 0.79697(3) 0.215451(18) 0.02721(12) Uani 1 1 d . . .
Ru2 Ru 0.14058(4) 0.57948(4) 0.214613(19) 0.02847(13) Uani 1 1 d . . .
Ru3 Ru 0.01847(5) 0.65187(4) 0.394347(19) 0.03398(14) Uani 1 1 d . . .
O1 O 0.0249(4) 0.9876(3) 0.19735(16) 0.0394(10) Uani 1 1 d . . .
O2 O 0.4135(4) 0.9030(3) 0.13546(17) 0.0465(11) Uani 1 1 d . . .
O3 O 0.3974(4) 0.4160(3) 0.22509(17) 0.0445(11) Uani 1 1 d . . .
O4 O 0.0175(4) 0.4315(3) 0.28686(16) 0.0451(11) Uani 1 1 d . . .
O5 O -0.1195(5) 0.7647(4) 0.50565(19) 0.0732(16) Uani 1 1 d . . .
O6 O -0.2173(4) 0.6940(4) 0.3264(2) 0.0585(13) Uani 1 1 d . . .
O7 O 0.0021(5) 0.4237(3) 0.42430(19) 0.0604(14) Uani 1 1 d . . .
O8 O 0.4063(3) 0.6669(3) 0.23464(15) 0.0309(9) Uani 1 1 d . . .
O9 O 0.0290(3) 0.7510(3) 0.11977(15) 0.0298(9) Uani 1 1 d . . .
O10 O 0.2202(3) 0.6780(3) 0.16100(14) 0.0266(9) Uani 1 1 d . . .
O11 O 0.1333(3) 0.7170(3) 0.26986(14) 0.0262(9) Uani 1 1 d . . .
C1 C 0.1088(6) 0.9142(4) 0.2049(2) 0.0287(13) Uani 1 1 d . . .
C2 C 0.3512(5) 0.8613(4) 0.1650(2) 0.0303(14) Uani 1 1 d . . .
C3 C 0.2993(6) 0.4819(4) 0.2226(2) 0.0320(14) Uani 1 1 d . . .
C4 C 0.0629(5) 0.4913(4) 0.2607(2) 0.0314(14) Uani 1 1 d . . .
C5 C -0.0675(7) 0.7188(5) 0.4648(3) 0.0489(18) Uani 1 1 d . . .
C6 C -0.1284(7) 0.6768(5) 0.3526(3) 0.0420(16) Uani 1 1 d . . .
C7 C 0.0081(6) 0.5090(5) 0.4132(2) 0.0410(16) Uani 1 1 d . . .
C8 C 0.4535(5) 0.6827(4) 0.2792(2) 0.0279(13) Uani 1 1 d . . .
C9 C 0.4113(5) 0.7876(4) 0.3042(2) 0.0346(14) Uani 1 1 d . . .
H9A H 0.4486 0.8046 0.3360 0.042 Uiso 1 1 calc R . .
C10 C 0.3151(5) 0.8623(4) 0.2803(2) 0.0287(13) Uani 1 1 d . . .
C11 C 0.2734(5) 0.9733(4) 0.3029(2) 0.0311(14) Uani 1 1 d . . .
C12 C 0.2375(5) 1.0618(4) 0.2675(2) 0.0362(15) Uani 1 1 d . . .
H12A H 0.2369 1.0511 0.2280 0.043 Uiso 1 1 calc R . .
C13 C 0.2026(6) 1.1652(5) 0.2892(3) 0.0474(17) Uani 1 1 d . . .
H13A H 0.1784 1.2245 0.2643 0.057 Uiso 1 1 calc R . .
C14 C 0.2023(6) 1.1835(5) 0.3462(3) 0.0487(18) Uani 1 1 d . . .
H14A H 0.1805 1.2546 0.3609 0.058 Uiso 1 1 calc R . .
C15 C 0.2351(7) 1.0947(6) 0.3818(3) 0.059(2) Uani 1 1 d . . .
H15A H 0.2327 1.1054 0.4214 0.071 Uiso 1 1 calc R . .
C16 C 0.2705(6) 0.9927(5) 0.3605(3) 0.0411(16) Uani 1 1 d . . .
H16A H 0.2936 0.9336 0.3856 0.049 Uiso 1 1 calc R . .
C17 C 0.5496(5) 0.5939(4) 0.3032(2) 0.0354(14) Uani 1 1 d . . .
H17A H 0.5710 0.5997 0.3406 0.042 Uiso 1 1 calc R . .
C18 C 0.6082(5) 0.5039(5) 0.2724(2) 0.0361(15) Uani 1 1 d . . .
H18A H 0.5882 0.5043 0.2343 0.043 Uiso 1 1 calc R . .
C19 C 0.6987(6) 0.4060(5) 0.2912(3) 0.0400(15) Uani 1 1 d . . .
C20 C 0.7123(7) 0.3822(5) 0.3473(3) 0.072(2) Uani 1 1 d . . .
H20A H 0.6642 0.4329 0.3756 0.086 Uiso 1 1 calc R . .
C21 C 0.7944(7) 0.2863(6) 0.3637(3) 0.076(2) Uani 1 1 d . . .
H21A H 0.8003 0.2704 0.4029 0.091 Uiso 1 1 calc R . .
C22 C 0.8671(7) 0.2142(5) 0.3231(3) 0.0551(19) Uani 1 1 d . . .
H22A H 0.9251 0.1487 0.3341 0.066 Uiso 1 1 calc R . .
C23 C 0.8564(7) 0.2362(5) 0.2677(3) 0.062(2) Uani 1 1 d . . .
H23A H 0.9072 0.1866 0.2395 0.074 Uiso 1 1 calc R . .
C24 C 0.7701(6) 0.3327(5) 0.2518(3) 0.0521(18) Uani 1 1 d . . .
H24A H 0.7614 0.3469 0.2127 0.062 Uiso 1 1 calc R . .
C25 C -0.0494(5) 0.7041(4) 0.1556(2) 0.0292(13) Uani 1 1 d . . .
C26 C -0.0252(5) 0.5948(4) 0.1598(2) 0.0289(13) Uani 1 1 d . . .
H26A H -0.0991 0.5638 0.1738 0.035 Uiso 1 1 calc R . .
C27 C 0.0994(5) 0.5233(4) 0.1376(2) 0.0314(14) Uani 1 1 d . . .
C28 C 0.1124(6) 0.4060(5) 0.1298(2) 0.0360(15) Uani 1 1 d . . .
C29 C 0.2344(6) 0.3307(5) 0.1279(3) 0.0473(17) Uani 1 1 d . . .
H29A H 0.3107 0.3545 0.1289 0.057 Uiso 1 1 calc R . .
C30 C 0.2463(8) 0.2221(5) 0.1247(3) 0.0558(19) Uani 1 1 d . . .
H30A H 0.3299 0.1716 0.1250 0.067 Uiso 1 1 calc R . .
C31 C 0.1389(8) 0.1878(5) 0.1210(3) 0.056(2) Uani 1 1 d . . .
H31A H 0.1476 0.1130 0.1186 0.067 Uiso 1 1 calc R . .
C32 C 0.0164(8) 0.2603(6) 0.1208(3) 0.058(2) Uani 1 1 d . . .
H32A H -0.0587 0.2358 0.1180 0.070 Uiso 1 1 calc R . .
C33 C 0.0052(6) 0.3687(5) 0.1248(2) 0.0433(16) Uani 1 1 d . . .
H33A H -0.0786 0.4188 0.1242 0.052 Uiso 1 1 calc R . .
C34 C -0.1621(5) 0.7820(4) 0.1845(2) 0.0306(14) Uani 1 1 d . . .
H34A H -0.2181 0.7577 0.2126 0.037 Uiso 1 1 calc R . .
C35 C -0.1892(5) 0.8870(5) 0.1725(2) 0.0363(15) Uani 1 1 d . . .
H35A H -0.1351 0.9058 0.1415 0.044 Uiso 1 1 calc R . .
C36 C -0.2898(6) 0.9766(5) 0.2002(3) 0.0377(15) Uani 1 1 d . . .
C37 C -0.3120(6) 1.0781(5) 0.1761(3) 0.060(2) Uani 1 1 d . . .
H37A H -0.2633 1.0869 0.1411 0.072 Uiso 1 1 calc R . .
C38 C -0.4021(7) 1.1664(5) 0.2014(3) 0.065(2) Uani 1 1 d . . .
H38A H -0.4189 1.2343 0.1832 0.079 Uiso 1 1 calc R . .
C39 C -0.4673(6) 1.1549(5) 0.2534(3) 0.058(2) Uani 1 1 d . . .
H39A H -0.5273 1.2161 0.2718 0.069 Uiso 1 1 calc R . .
C40 C -0.4473(6) 1.0563(5) 0.2792(3) 0.0515(18) Uani 1 1 d . . .
H40A H -0.4939 1.0493 0.3151 0.062 Uiso 1 1 calc R . .
C41 C -0.3595(6) 0.9676(5) 0.2529(3) 0.0450(17) Uani 1 1 d . . .
H41A H -0.3460 0.8994 0.2708 0.054 Uiso 1 1 calc R . .
C42 C 0.1656(5) 0.6877(4) 0.1096(2) 0.0302(13) Uani 1 1 d . . .
C43 C 0.1720(5) 0.5751(4) 0.0895(2) 0.0295(13) Uani 1 1 d . . .
H43A H 0.2663 0.5325 0.0855 0.035 Uiso 1 1 calc R . .
C44 C 0.1208(6) 0.5734(5) 0.0315(2) 0.0384(15) Uani 1 1 d . . .
H44A H 0.0567 0.5304 0.0349 0.046 Uiso 1 1 calc R . .
H44B H 0.0736 0.6478 0.0217 0.046 Uiso 1 1 calc R . .
C45 C 0.2256(6) 0.5279(5) -0.0166(2) 0.0344(14) Uani 1 1 d . . .
C46 C 0.2663(7) 0.4197(5) -0.0276(3) 0.0530(18) Uani 1 1 d . . .
H46A H 0.2274 0.3731 -0.0046 0.064 Uiso 1 1 calc R . .
C47 C 0.3626(7) 0.3767(6) -0.0713(3) 0.065(2) Uani 1 1 d . . .
H47A H 0.3865 0.3016 -0.0788 0.077 Uiso 1 1 calc R . .
C48 C 0.4241(7) 0.4414(6) -0.1038(3) 0.059(2) Uani 1 1 d . . .
H48A H 0.4925 0.4118 -0.1329 0.071 Uiso 1 1 calc R . .
C49 C 0.3849(7) 0.5493(6) -0.0933(3) 0.057(2) Uani 1 1 d . . .
H49A H 0.4256 0.5954 -0.1158 0.068 Uiso 1 1 calc R . .
C50 C 0.2867(6) 0.5926(5) -0.0504(2) 0.0465(17) Uani 1 1 d . . .
H50A H 0.2607 0.6681 -0.0440 0.056 Uiso 1 1 calc R . .
C51 C 0.2309(5) 0.7537(4) 0.0683(2) 0.0297(13) Uani 1 1 d . . .
H51A H 0.3205 0.7236 0.0546 0.036 Uiso 1 1 calc R . .
C52 C 0.1716(6) 0.8498(5) 0.0504(2) 0.0347(14) Uani 1 1 d . . .
H52A H 0.0806 0.8764 0.0626 0.042 Uiso 1 1 calc R . .
C53 C 0.2319(6) 0.9207(5) 0.0133(2) 0.0361(15) Uani 1 1 d . . .
C54 C 0.3601(6) 0.8902(5) -0.0121(2) 0.0482(17) Uani 1 1 d . . .
H54A H 0.4134 0.8191 -0.0072 0.058 Uiso 1 1 calc R . .
C55 C 0.4108(7) 0.9620(6) -0.0442(3) 0.058(2) Uani 1 1 d . . .
H55A H 0.4981 0.9397 -0.0623 0.070 Uiso 1 1 calc R . .
C56 C 0.3363(7) 1.0663(6) -0.0506(3) 0.058(2) Uani 1 1 d . . .
H56A H 0.3735 1.1158 -0.0720 0.070 Uiso 1 1 calc R . .
C57 C 0.2083(6) 1.0991(5) -0.0262(3) 0.0446(16) Uani 1 1 d . . .
H57A H 0.1555 1.1703 -0.0312 0.054 Uiso 1 1 calc R . .
C58 C 0.1589(6) 1.0256(5) 0.0059(2) 0.0361(15) Uani 1 1 d . . .
H58A H 0.0713 1.0480 0.0237 0.043 Uiso 1 1 calc R . .
C59 C 0.1437(5) 0.7135(4) 0.3263(2) 0.0261(13) Uani 1 1 d . . .
C60 C 0.2183(5) 0.6204(4) 0.3520(2) 0.0273(13) Uani 1 1 d . . .
H60A H 0.2575 0.5533 0.3290 0.033 Uiso 1 1 calc R . .
C61 C 0.2238(5) 0.6179(4) 0.4119(2) 0.0337(14) Uani 1 1 d . . .
H61A H 0.2446 0.6826 0.4261 0.040 Uiso 1 1 calc R . .
C62 C 0.2918(6) 0.5173(5) 0.4403(2) 0.0426(16) Uani 1 1 d . . .
C63 C 0.3068(10) 0.5192(6) 0.4960(3) 0.122(4) Uani 1 1 d . . .
H63A H 0.2739 0.5848 0.5167 0.146 Uiso 1 1 calc R . .
C64 C 0.3694(13) 0.4266(8) 0.5233(4) 0.173(6) Uani 1 1 d . . .
H64A H 0.3790 0.4306 0.5625 0.208 Uiso 1 1 calc R . .
C65 C 0.4169(8) 0.3322(7) 0.4967(4) 0.091(3) Uani 1 1 d . . .
H65A H 0.4605 0.2696 0.5160 0.109 Uiso 1 1 calc R . .
C66 C 0.4008(7) 0.3294(5) 0.4422(3) 0.058(2) Uani 1 1 d . . .
H66A H 0.4318 0.2630 0.4222 0.070 Uiso 1 1 calc R . .
C67 C 0.3407(7) 0.4202(5) 0.4141(3) 0.059(2) Uani 1 1 d . . .
H67A H 0.3327 0.4150 0.3748 0.071 Uiso 1 1 calc R . .
C68 C 0.0691(5) 0.7987(4) 0.3636(2) 0.0322(14) Uani 1 1 d . . .
H68A H 0.1257 0.8208 0.3891 0.039 Uiso 1 1 calc R . .
C69 C -0.0314(5) 0.8958(4) 0.3427(2) 0.0318(14) Uani 1 1 d . . .
H69A H 0.0148 0.9456 0.3232 0.038 Uiso 1 1 calc R . .
H69B H -0.0796 0.8717 0.3147 0.038 Uiso 1 1 calc R . .
C70 C -0.1283(6) 0.9551(4) 0.3905(2) 0.0372(15) Uani 1 1 d . . .
C71 C -0.2576(7) 0.9519(5) 0.3969(3) 0.0540(19) Uani 1 1 d . . .
H71A H -0.2870 0.9126 0.3704 0.065 Uiso 1 1 calc R . .
C72 C -0.3451(7) 1.0054(6) 0.4417(3) 0.073(2) Uani 1 1 d . . .
H72A H -0.4340 1.0034 0.4454 0.087 Uiso 1 1 calc R . .
C73 C -0.3030(8) 1.0606(6) 0.4800(3) 0.071(2) Uani 1 1 d . . .
H73A H -0.3624 1.0965 0.5109 0.085 Uiso 1 1 calc R . .
C74 C -0.1744(8) 1.0648(5) 0.4744(3) 0.064(2) Uani 1 1 d . . .
H74A H -0.1443 1.1029 0.5012 0.077 Uiso 1 1 calc R . .
C75 C -0.0914(6) 1.0132(5) 0.4296(2) 0.0437(16) Uani 1 1 d . . .
H75A H -0.0036 1.0178 0.4254 0.052 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0319(3) 0.0223(3) 0.0244(3) -0.0001(2) -0.0003(2) -0.0035(2)
Ru2 0.0358(3) 0.0223(3) 0.0245(3) -0.0003(2) -0.0001(2) -0.0046(2)
Ru3 0.0411(3) 0.0287(3) 0.0274(3) 0.0019(2) 0.0035(2) -0.0049(2)
O1 0.038(3) 0.026(2) 0.051(3) 0.005(2) -0.010(2) -0.002(2)
O2 0.051(3) 0.055(3) 0.038(3) 0.005(2) 0.005(2) -0.025(2)
O3 0.043(3) 0.031(3) 0.051(3) 0.002(2) -0.004(2) 0.002(2)
O4 0.063(3) 0.035(3) 0.040(3) 0.002(2) 0.002(2) -0.021(2)
O5 0.110(4) 0.050(3) 0.037(3) -0.004(2) 0.024(3) 0.003(3)
O6 0.053(3) 0.059(3) 0.070(4) 0.010(3) -0.018(3) -0.021(3)
O7 0.085(4) 0.034(3) 0.062(3) 0.008(2) 0.000(3) -0.021(3)
O8 0.036(2) 0.028(2) 0.027(2) -0.0042(18) -0.0030(18) -0.0046(18)
O9 0.028(2) 0.028(2) 0.032(2) 0.0054(18) -0.0030(18) -0.0066(18)
O10 0.037(2) 0.025(2) 0.0186(19) -0.0005(16) -0.0034(17) -0.0089(17)
O11 0.036(2) 0.021(2) 0.022(2) 0.0016(16) -0.0017(17) -0.0081(17)
C1 0.040(4) 0.028(3) 0.022(3) -0.003(3) -0.003(3) -0.016(3)
C2 0.030(3) 0.033(3) 0.028(3) -0.003(3) -0.003(3) -0.007(3)
C3 0.043(4) 0.027(3) 0.025(3) 0.000(3) 0.001(3) -0.008(3)
C4 0.040(4) 0.026(3) 0.028(3) -0.004(3) -0.008(3) -0.006(3)
C5 0.067(5) 0.041(4) 0.036(4) 0.012(3) 0.001(4) -0.013(4)
C6 0.050(4) 0.030(4) 0.045(4) -0.002(3) 0.013(3) -0.017(3)
C7 0.048(4) 0.042(4) 0.031(4) -0.003(3) -0.002(3) -0.009(3)
C8 0.032(3) 0.025(3) 0.024(3) 0.000(3) 0.001(3) -0.005(3)
C9 0.042(4) 0.031(4) 0.031(3) -0.003(3) -0.005(3) -0.009(3)
C10 0.034(3) 0.026(3) 0.024(3) -0.002(3) 0.002(3) -0.006(3)
C11 0.027(3) 0.030(3) 0.035(3) -0.001(3) -0.002(3) -0.006(3)
C12 0.038(4) 0.031(4) 0.041(4) -0.011(3) -0.004(3) -0.009(3)
C13 0.046(4) 0.021(4) 0.071(5) -0.004(3) -0.004(4) -0.003(3)
C14 0.049(4) 0.027(4) 0.066(5) -0.021(4) 0.001(4) -0.004(3)
C15 0.078(5) 0.057(5) 0.038(4) -0.016(4) 0.002(4) -0.013(4)
C16 0.051(4) 0.029(4) 0.041(4) -0.007(3) 0.005(3) -0.011(3)
C17 0.039(4) 0.036(4) 0.030(3) 0.008(3) -0.008(3) -0.006(3)
C18 0.032(3) 0.037(4) 0.037(4) 0.002(3) -0.005(3) -0.005(3)
C19 0.036(4) 0.029(4) 0.053(4) 0.004(3) -0.008(3) -0.004(3)
C20 0.095(6) 0.047(5) 0.046(5) 0.007(4) -0.003(4) 0.022(4)
C21 0.087(6) 0.056(5) 0.058(5) 0.023(4) -0.007(5) 0.021(4)
C22 0.050(5) 0.037(4) 0.074(5) 0.008(4) -0.011(4) -0.004(3)
C23 0.058(5) 0.037(4) 0.078(6) -0.017(4) 0.000(4) 0.007(4)
C24 0.064(5) 0.035(4) 0.053(4) -0.004(3) -0.022(4) 0.002(4)
C25 0.032(3) 0.031(3) 0.023(3) 0.001(3) -0.005(3) -0.006(3)
C26 0.032(3) 0.032(3) 0.025(3) -0.002(3) -0.003(3) -0.012(3)
C27 0.035(4) 0.026(3) 0.030(3) -0.004(3) -0.002(3) -0.005(3)
C28 0.050(4) 0.039(4) 0.018(3) 0.003(3) -0.001(3) -0.014(3)
C29 0.054(4) 0.034(4) 0.050(4) -0.013(3) 0.001(3) -0.008(3)
C30 0.082(6) 0.028(4) 0.045(4) -0.010(3) -0.006(4) 0.005(4)
C31 0.101(6) 0.029(4) 0.040(4) -0.005(3) -0.007(4) -0.021(4)
C32 0.074(6) 0.053(5) 0.059(5) -0.001(4) -0.007(4) -0.038(4)
C33 0.058(4) 0.033(4) 0.044(4) -0.001(3) -0.009(3) -0.018(3)
C34 0.023(3) 0.035(4) 0.032(3) 0.003(3) -0.001(3) -0.006(3)
C35 0.028(3) 0.041(4) 0.037(4) 0.005(3) 0.000(3) -0.006(3)
C36 0.034(4) 0.025(3) 0.052(4) -0.003(3) -0.010(3) -0.004(3)
C37 0.045(4) 0.041(4) 0.090(6) 0.014(4) -0.001(4) -0.008(4)
C38 0.051(5) 0.032(4) 0.099(6) 0.007(4) 0.011(4) 0.004(4)
C39 0.039(4) 0.033(4) 0.090(6) -0.010(4) 0.009(4) 0.002(3)
C40 0.037(4) 0.044(4) 0.064(5) -0.008(4) 0.005(3) 0.001(3)
C41 0.038(4) 0.035(4) 0.060(5) 0.003(3) -0.006(3) -0.006(3)
C42 0.031(3) 0.028(3) 0.029(3) 0.001(3) -0.003(3) -0.004(3)
C43 0.034(3) 0.026(3) 0.025(3) -0.004(3) -0.001(3) -0.003(3)
C44 0.046(4) 0.036(4) 0.032(3) 0.006(3) -0.005(3) -0.009(3)
C45 0.048(4) 0.038(4) 0.021(3) -0.006(3) -0.006(3) -0.015(3)
C46 0.076(5) 0.041(4) 0.039(4) -0.006(3) 0.005(4) -0.014(4)
C47 0.087(6) 0.046(5) 0.043(4) -0.002(4) 0.007(4) 0.006(4)
C48 0.062(5) 0.060(5) 0.035(4) -0.007(4) 0.006(4) 0.014(4)
C49 0.066(5) 0.077(6) 0.030(4) 0.001(4) 0.005(4) -0.027(4)
C50 0.058(5) 0.050(4) 0.033(4) -0.002(3) -0.005(3) -0.018(4)
C51 0.033(3) 0.029(3) 0.022(3) -0.004(3) 0.002(3) -0.001(3)
C52 0.034(4) 0.041(4) 0.029(3) -0.001(3) -0.004(3) -0.009(3)
C53 0.048(4) 0.033(4) 0.020(3) 0.006(3) -0.001(3) 0.000(3)
C54 0.049(4) 0.045(4) 0.041(4) 0.007(3) 0.005(3) -0.001(3)
C55 0.050(4) 0.057(5) 0.055(5) 0.019(4) 0.013(4) -0.004(4)
C56 0.065(5) 0.057(5) 0.058(5) 0.009(4) 0.006(4) -0.031(4)
C57 0.052(4) 0.039(4) 0.045(4) 0.005(3) -0.004(3) -0.017(3)
C58 0.041(4) 0.038(4) 0.032(3) 0.002(3) -0.002(3) -0.017(3)
C59 0.036(3) 0.021(3) 0.025(3) -0.001(3) -0.003(3) -0.014(3)
C60 0.038(3) 0.018(3) 0.023(3) 0.001(2) -0.002(3) -0.003(3)
C61 0.045(4) 0.023(3) 0.029(3) 0.000(3) -0.001(3) -0.004(3)
C62 0.059(4) 0.029(4) 0.030(4) 0.001(3) -0.003(3) 0.004(3)
C63 0.227(12) 0.055(6) 0.047(5) -0.003(4) -0.060(6) 0.039(6)
C64 0.348(17) 0.068(7) 0.055(6) -0.008(5) -0.103(9) 0.055(9)
C65 0.119(8) 0.058(6) 0.075(6) 0.025(5) -0.041(6) 0.020(5)
C66 0.071(5) 0.041(4) 0.052(5) 0.010(4) -0.004(4) 0.002(4)
C67 0.087(6) 0.045(5) 0.037(4) 0.011(4) -0.019(4) -0.002(4)
C68 0.037(3) 0.036(4) 0.022(3) 0.005(3) -0.003(3) -0.007(3)
C69 0.043(4) 0.021(3) 0.027(3) 0.000(3) 0.002(3) -0.005(3)
C70 0.047(4) 0.029(4) 0.026(3) 0.005(3) -0.002(3) 0.004(3)
C71 0.053(5) 0.052(5) 0.045(4) -0.004(3) 0.005(4) 0.003(4)
C72 0.056(5) 0.086(6) 0.055(5) 0.002(5) 0.014(4) 0.008(4)
C73 0.071(6) 0.073(6) 0.035(4) 0.000(4) 0.011(4) 0.030(5)
C74 0.076(6) 0.056(5) 0.036(4) -0.001(4) -0.008(4) 0.023(4)
C75 0.051(4) 0.035(4) 0.036(4) -0.002(3) -0.001(3) 0.002(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100880.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100880.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100880
loop_
_publ_author_name
'Osintseva, Svetlana V.'
'Dolgushin, Fedor M.'
'Shtel'tser, Nikolay A.'
'Petrovskii, Pavel V.'
'Kreindlin, Arkadii Z.'
'Rybin, Leonid V.'
'Antipin, Mikhail Yu.'
_publ_section_title
;
Reaction of Ru <sub>3</sub> (CO) <sub>12</sub> with Dibenzylideneacetone
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2279
_journal_page_last 2288
_journal_paper_doi 10.1021/om0489958
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C76 H56 O12 Ru4'
_chemical_formula_weight 1565.49
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 75.860(3)
_cell_angle_beta 83.084(3)
_cell_angle_gamma 76.385(3)
_cell_formula_units_Z 1
_cell_length_a 10.4959(17)
_cell_length_b 12.347(2)
_cell_length_c 12.762(2)
_cell_measurement_reflns_used 1778
_cell_measurement_temperature 110(2)
_cell_measurement_theta_max 21.85
_cell_measurement_theta_min 2.35
_cell_volume 1555.2(4)
_diffrn_ambient_temperature 110(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0618
_diffrn_reflns_av_sigmaI/netI 0.1172
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 9165
_diffrn_reflns_theta_max 22.07
_diffrn_reflns_theta_min 1.65
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.020
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.672
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 784
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.986
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 415
_refine_ls_number_reflns 3837
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.986
_refine_ls_R_factor_all 0.0777
_refine_ls_R_factor_gt 0.0437
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1042
_refine_ls_wR_factor_ref 0.1227
_reflns_number_gt 2675
_reflns_number_total 3837
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100880
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.61687(6) 0.53595(5) 0.40342(5) 0.0263(2) Uani 1 1 d . . .
Ru2 Ru 0.31854(6) 0.60048(6) 0.26194(5) 0.0272(2) Uani 1 1 d . . .
O1 O 0.8229(6) 0.6775(5) 0.3501(5) 0.0410(16) Uani 1 1 d . . .
O2 O 0.8314(6) 0.3291(5) 0.4652(5) 0.0404(16) Uani 1 1 d . . .
O3 O 0.4807(5) 0.4303(4) 0.4366(4) 0.0277(13) Uani 1 1 d . . .
O4 O 0.4583(5) 0.6651(4) 0.3362(4) 0.0260(13) Uani 1 1 d . . .
O5 O 0.0894(6) 0.5090(6) 0.4004(5) 0.0491(17) Uani 1 1 d . . .
O6 O 0.2123(6) 0.5601(5) 0.0724(5) 0.0448(16) Uani 1 1 d . . .
C1 C 0.7418(8) 0.6253(7) 0.3706(6) 0.029(2) Uani 1 1 d . . .
C2 C 0.7505(10) 0.4094(8) 0.4456(7) 0.035(2) Uani 1 1 d . . .
C5 C 0.1785(9) 0.5422(7) 0.3557(6) 0.034(2) Uani 1 1 d . . .
C6 C 0.2486(8) 0.5752(7) 0.1484(7) 0.033(2) Uani 1 1 d . . .
C7 C 0.6240(8) 0.5151(7) 0.2443(7) 0.032(2) Uani 1 1 d . . .
C8 C 0.5031(8) 0.4637(6) 0.2459(6) 0.027(2) Uani 1 1 d . . .
H8A H 0.5050 0.4239 0.1860 0.032 Uiso 1 1 calc R . .
C9 C 0.4460(8) 0.4129(7) 0.3457(6) 0.028(2) Uani 1 1 d . . .
C10 C 0.3758(8) 0.3216(7) 0.3549(7) 0.033(2) Uani 1 1 d . . .
H10A H 0.3288 0.3224 0.2955 0.040 Uiso 1 1 calc R . .
C11 C 0.3748(9) 0.2378(7) 0.4425(7) 0.040(2) Uani 1 1 d . . .
H11A H 0.4216 0.2384 0.5015 0.048 Uiso 1 1 calc R . .
C12 C 0.3056(8) 0.1433(7) 0.4546(7) 0.035(2) Uani 1 1 d . . .
C13 C 0.2021(8) 0.1504(8) 0.3922(7) 0.043(2) Uani 1 1 d . . .
H13A H 0.1720 0.2192 0.3409 0.052 Uiso 1 1 calc R . .
C14 C 0.1431(10) 0.0599(8) 0.4037(8) 0.054(3) Uani 1 1 d . . .
H14A H 0.0728 0.0667 0.3604 0.064 Uiso 1 1 calc R . .
C15 C 0.1844(9) -0.0392(8) 0.4764(7) 0.045(3) Uani 1 1 d . . .
H15A H 0.1448 -0.1024 0.4827 0.054 Uiso 1 1 calc R . .
C16 C 0.2825(10) -0.0479(8) 0.5402(8) 0.053(3) Uani 1 1 d . . .
H16A H 0.3109 -0.1170 0.5917 0.064 Uiso 1 1 calc R . .
C17 C 0.3409(10) 0.0432(8) 0.5303(7) 0.047(3) Uani 1 1 d . . .
H17A H 0.4076 0.0366 0.5771 0.057 Uiso 1 1 calc R . .
C18 C 0.7488(7) 0.4365(7) 0.2100(6) 0.025(2) Uani 1 1 d . . .
C19 C 0.7575(8) 0.3201(7) 0.2235(6) 0.029(2) Uani 1 1 d . . .
H19A H 0.6818 0.2898 0.2506 0.035 Uiso 1 1 calc R . .
C20 C 0.8710(8) 0.2477(8) 0.1993(7) 0.034(2) Uani 1 1 d . . .
H20A H 0.8732 0.1684 0.2097 0.041 Uiso 1 1 calc R . .
C21 C 0.9831(9) 0.2890(8) 0.1595(7) 0.043(2) Uani 1 1 d . . .
H21A H 1.0624 0.2385 0.1432 0.052 Uiso 1 1 calc R . .
C22 C 0.9783(8) 0.4050(8) 0.1439(7) 0.037(2) Uani 1 1 d . . .
H22A H 1.0547 0.4342 0.1165 0.044 Uiso 1 1 calc R . .
C23 C 0.8634(8) 0.4781(7) 0.1679(6) 0.030(2) Uani 1 1 d . . .
H23A H 0.8611 0.5576 0.1560 0.036 Uiso 1 1 calc R . .
C24 C 0.2380(8) 0.7859(6) 0.2422(6) 0.029(2) Uani 1 1 d . . .
H24A H 0.2488 0.8142 0.3069 0.034 Uiso 1 1 calc R . .
C25 C 0.3579(8) 0.7687(7) 0.1745(7) 0.030(2) Uani 1 1 d . . .
H25A H 0.3575 0.7929 0.0938 0.035 Uiso 1 1 calc R . .
C26 C 0.4706(8) 0.6951(6) 0.2257(6) 0.026(2) Uani 1 1 d . . .
C27 C 0.5980(8) 0.6386(6) 0.1712(6) 0.026(2) Uani 1 1 d . . .
H27A H 0.6699 0.6771 0.1769 0.031 Uiso 1 1 calc R . .
C28 C 0.5877(8) 0.6395(7) 0.0518(6) 0.029(2) Uani 1 1 d . . .
H28A H 0.6657 0.5857 0.0287 0.035 Uiso 1 1 calc R . .
H28B H 0.5095 0.6095 0.0470 0.035 Uiso 1 1 calc R . .
C29 C 0.1089(8) 0.8373(7) 0.1976(7) 0.030(2) Uani 1 1 d . . .
C30 C 0.0837(9) 0.8397(7) 0.0917(7) 0.042(2) Uani 1 1 d . . .
H30A H 0.1528 0.8098 0.0445 0.050 Uiso 1 1 calc R . .
C31 C -0.0383(9) 0.8843(8) 0.0558(8) 0.047(3) Uani 1 1 d . . .
H31A H -0.0530 0.8865 -0.0168 0.056 Uiso 1 1 calc R . .
C32 C -0.1409(9) 0.9263(8) 0.1222(8) 0.044(2) Uani 1 1 d . . .
H32A H -0.2256 0.9579 0.0957 0.053 Uiso 1 1 calc R . .
C33 C -0.1200(9) 0.9221(7) 0.2275(7) 0.040(2) Uani 1 1 d . . .
H33A H -0.1907 0.9490 0.2750 0.048 Uiso 1 1 calc R . .
C34 C 0.0046(8) 0.8785(7) 0.2637(7) 0.030(2) Uani 1 1 d . . .
H34A H 0.0188 0.8769 0.3362 0.036 Uiso 1 1 calc R . .
C35 C 0.5778(7) 0.7535(6) -0.0279(6) 0.0231(19) Uani 1 1 d . . .
C36 C 0.6675(8) 0.8199(7) -0.0351(7) 0.038(2) Uani 1 1 d . . .
H36A H 0.7357 0.7956 0.0135 0.045 Uiso 1 1 calc R . .
C37 C 0.6607(9) 0.9221(7) -0.1118(7) 0.043(2) Uani 1 1 d . . .
H37A H 0.7245 0.9664 -0.1151 0.052 Uiso 1 1 calc R . .
C38 C 0.5638(9) 0.9597(7) -0.1826(7) 0.041(2) Uani 1 1 d . . .
H38A H 0.5604 1.0291 -0.2358 0.049 Uiso 1 1 calc R . .
C39 C 0.4699(8) 0.8948(7) -0.1756(7) 0.035(2) Uani 1 1 d . . .
H39A H 0.4009 0.9201 -0.2235 0.042 Uiso 1 1 calc R . .
C40 C 0.4778(8) 0.7932(7) -0.0985(6) 0.031(2) Uani 1 1 d . . .
H40A H 0.4130 0.7496 -0.0939 0.038 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0336(4) 0.0261(4) 0.0225(4) -0.0012(3) -0.0085(3) -0.0141(3)
Ru2 0.0320(4) 0.0291(5) 0.0237(4) -0.0042(3) -0.0060(3) -0.0126(4)
O1 0.041(4) 0.046(4) 0.045(4) -0.007(3) -0.006(3) -0.029(3)
O2 0.052(4) 0.030(4) 0.037(4) -0.003(3) -0.016(3) -0.002(3)
O3 0.043(3) 0.026(3) 0.020(3) 0.001(2) -0.013(3) -0.017(3)
O4 0.034(3) 0.029(3) 0.017(3) -0.001(2) -0.004(2) -0.016(3)
O5 0.044(4) 0.065(5) 0.045(4) -0.009(3) -0.002(3) -0.029(4)
O6 0.049(4) 0.053(4) 0.041(4) -0.016(3) -0.017(3) -0.015(3)
C1 0.037(5) 0.029(5) 0.022(5) -0.006(4) -0.018(4) -0.001(5)
C2 0.058(7) 0.034(6) 0.024(5) -0.006(4) -0.018(5) -0.022(5)
C5 0.038(5) 0.043(6) 0.022(5) -0.002(4) -0.008(4) -0.016(5)
C6 0.023(5) 0.037(6) 0.043(6) -0.011(5) -0.004(4) -0.011(4)
C7 0.041(5) 0.027(5) 0.035(5) -0.003(4) -0.017(4) -0.018(4)
C8 0.040(5) 0.015(4) 0.028(5) -0.008(4) -0.008(4) -0.004(4)
C9 0.036(5) 0.026(5) 0.021(5) 0.001(4) -0.008(4) -0.009(4)
C10 0.042(5) 0.040(6) 0.028(5) -0.012(4) -0.013(4) -0.020(5)
C11 0.053(6) 0.033(6) 0.039(6) 0.005(5) -0.019(5) -0.024(5)
C12 0.047(6) 0.032(5) 0.028(5) 0.000(4) -0.006(4) -0.021(5)
C13 0.041(6) 0.040(6) 0.045(6) 0.011(5) -0.018(5) -0.016(5)
C14 0.063(7) 0.042(7) 0.064(7) -0.005(6) -0.012(6) -0.031(6)
C15 0.062(7) 0.035(6) 0.046(6) -0.008(5) 0.000(5) -0.028(5)
C16 0.075(7) 0.039(6) 0.048(6) 0.002(5) -0.011(6) -0.027(6)
C17 0.068(7) 0.050(7) 0.031(5) -0.006(5) -0.002(5) -0.030(6)
C18 0.027(5) 0.025(5) 0.022(5) 0.004(4) -0.014(4) -0.007(4)
C19 0.037(5) 0.033(5) 0.021(4) -0.004(4) -0.009(4) -0.014(5)
C20 0.038(6) 0.030(5) 0.035(5) -0.008(4) -0.004(4) -0.005(5)
C21 0.033(6) 0.054(7) 0.041(6) -0.016(5) -0.006(5) 0.002(5)
C22 0.027(5) 0.042(6) 0.043(6) -0.010(5) 0.001(4) -0.012(5)
C23 0.038(5) 0.026(5) 0.026(5) 0.003(4) -0.009(4) -0.014(5)
C24 0.036(5) 0.023(5) 0.030(5) -0.008(4) -0.012(4) -0.004(4)
C25 0.035(5) 0.030(5) 0.026(5) -0.004(4) -0.008(4) -0.012(4)
C26 0.034(5) 0.022(5) 0.028(5) -0.005(4) -0.002(4) -0.017(4)
C27 0.033(5) 0.023(5) 0.026(5) -0.002(4) -0.009(4) -0.015(4)
C28 0.037(5) 0.021(5) 0.025(5) 0.004(4) -0.009(4) -0.006(4)
C29 0.032(5) 0.028(5) 0.034(5) -0.011(4) -0.005(4) -0.006(4)
C30 0.045(6) 0.042(6) 0.036(6) -0.007(5) -0.012(5) -0.001(5)
C31 0.036(6) 0.057(7) 0.052(6) -0.017(5) -0.016(5) -0.008(5)
C32 0.030(6) 0.038(6) 0.067(7) -0.013(5) -0.017(5) -0.004(5)
C33 0.044(6) 0.039(6) 0.041(6) -0.014(5) 0.003(5) -0.013(5)
C34 0.037(5) 0.031(5) 0.027(5) -0.008(4) -0.008(4) -0.013(4)
C35 0.026(5) 0.029(5) 0.017(4) -0.008(4) -0.001(4) -0.007(4)
C36 0.028(5) 0.041(6) 0.039(5) 0.003(5) -0.009(4) -0.008(5)
C37 0.045(6) 0.038(6) 0.048(6) 0.013(5) -0.015(5) -0.028(5)
C38 0.050(6) 0.033(6) 0.034(5) 0.006(4) -0.001(5) -0.011(5)
C39 0.037(5) 0.035(6) 0.029(5) -0.005(4) -0.010(4) 0.001(5)
C40 0.034(5) 0.039(6) 0.024(5) -0.004(4) -0.006(4) -0.014(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100881.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100881.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100881
loop_
_publ_author_name
'Osintseva, Svetlana V.'
'Dolgushin, Fedor M.'
'Shtel'tser, Nikolay A.'
'Petrovskii, Pavel V.'
'Kreindlin, Arkadii Z.'
'Rybin, Leonid V.'
'Antipin, Mikhail Yu.'
_publ_section_title
;
Reaction of Ru <sub>3</sub> (CO) <sub>12</sub> with Dibenzylideneacetone
;
_journal_issue 10
_journal_name_full Organometallics
_journal_page_first 2279
_journal_page_last 2288
_journal_paper_doi 10.1021/om0489958
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C41 H34 O7 Ru2, C3 H6 O '
_chemical_formula_sum 'C44 H40 O8 Ru2'
_chemical_formula_weight 898.90
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 65.566(2)
_cell_angle_beta 80.367(2)
_cell_angle_gamma 70.567(2)
_cell_formula_units_Z 2
_cell_length_a 11.2554(12)
_cell_length_b 14.1456(15)
_cell_length_c 14.1740(15)
_cell_measurement_reflns_used 904
_cell_measurement_temperature 110(2)
_cell_measurement_theta_max 29.1
_cell_measurement_theta_min 2.5
_cell_volume 1936.4(4)
_diffrn_ambient_temperature 110(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0323
_diffrn_reflns_av_sigmaI/netI 0.0601
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 23459
_diffrn_reflns_theta_max 30.05
_diffrn_reflns_theta_min 1.58
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.834
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.542
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 912
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 647
_refine_ls_number_reflns 11238
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0729
_refine_ls_R_factor_gt 0.0514
_refine_ls_shift/su_max 0.043
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1139
_refine_ls_wR_factor_ref 0.1225
_reflns_number_gt 7767
_reflns_number_total 11238
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100881
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.31692(3) 0.37029(2) 0.31446(2) 0.02073(8) Uani 1 1 d . . .
Ru2 Ru -0.01329(3) 0.51741(2) 0.28065(2) 0.02111(8) Uani 1 1 d . . .
O1 O 0.5208(3) 0.4691(2) 0.1922(2) 0.0389(7) Uani 1 1 d . . .
O2 O 0.4923(3) 0.1525(2) 0.3293(2) 0.0339(6) Uani 1 1 d . . .
O3 O -0.1210(3) 0.4200(2) 0.5001(2) 0.0405(7) Uani 1 1 d . . .
O4 O -0.2483(3) 0.5452(3) 0.1884(2) 0.0393(7) Uani 1 1 d . . .
O5 O 0.3412(3) 0.3669(2) 0.4678(2) 0.0324(6) Uani 1 1 d . . .
O6 O 0.1785(2) 0.29422(19) 0.39122(18) 0.0228(5) Uani 1 1 d . . .
O7 O 0.1761(2) 0.52031(19) 0.29068(18) 0.0226(5) Uani 1 1 d . . .
C1 C 0.4423(3) 0.4335(3) 0.2403(3) 0.0256(7) Uani 1 1 d . . .
C2 C 0.4261(3) 0.2361(3) 0.3259(3) 0.0247(7) Uani 1 1 d . . .
C3 C -0.0816(3) 0.4565(3) 0.4187(3) 0.0284(8) Uani 1 1 d . . .
C4 C -0.1596(3) 0.5359(3) 0.2241(3) 0.0280(8) Uani 1 1 d . . .
C5 C 0.4305(4) 0.3485(3) 0.5195(3) 0.0324(8) Uani 1 1 d . . .
C6 C 0.4067(5) 0.3523(5) 0.6256(4) 0.0445(11) Uani 1 1 d . . .
C7 C 0.5630(5) 0.3204(5) 0.4835(5) 0.0565(14) Uani 1 1 d . . .
C8 C -0.0117(3) 0.1872(3) 0.4614(3) 0.0237(7) Uani 1 1 d . . .
C9 C -0.0031(3) 0.2579(3) 0.3643(3) 0.0246(7) Uani 1 1 d . . .
C10 C 0.0939(3) 0.3152(3) 0.3274(3) 0.0216(7) Uani 1 1 d . . .
C11 C 0.1005(3) 0.3842(3) 0.2219(3) 0.0197(6) Uani 1 1 d . . .
C12 C 0.2299(3) 0.4024(3) 0.1781(3) 0.0202(6) Uani 1 1 d . . .
C13 C -0.1070(3) 0.1267(3) 0.5006(3) 0.0255(7) Uani 1 1 d . . .
C14 C -0.1357(4) 0.0869(3) 0.6057(3) 0.0352(9) Uani 1 1 d . . .
C15 C -0.2277(5) 0.0333(4) 0.6436(4) 0.0450(11) Uani 1 1 d . . .
C16 C -0.2866(4) 0.0158(4) 0.5775(4) 0.0430(11) Uani 1 1 d . . .
C17 C -0.2546(4) 0.0524(3) 0.4730(4) 0.0365(9) Uani 1 1 d . . .
C18 C -0.1658(4) 0.1089(3) 0.4341(3) 0.0304(8) Uani 1 1 d . . .
C19 C 0.3018(3) 0.3310(3) 0.1198(3) 0.0213(7) Uani 1 1 d . . .
C20 C 0.2808(3) 0.2313(3) 0.1425(3) 0.0243(7) Uani 1 1 d . . .
C21 C 0.3471(4) 0.1642(3) 0.0912(3) 0.0280(8) Uani 1 1 d . . .
C22 C 0.4382(4) 0.1936(3) 0.0162(3) 0.0306(8) Uani 1 1 d . . .
C23 C 0.4616(4) 0.2911(3) -0.0069(3) 0.0298(8) Uani 1 1 d . . .
C24 C 0.3949(4) 0.3581(3) 0.0442(3) 0.0268(7) Uani 1 1 d . . .
C25 C -0.0333(3) 0.6853(3) 0.2638(3) 0.0243(7) Uani 1 1 d . . .
C26 C 0.0327(4) 0.6669(3) 0.1746(3) 0.0250(7) Uani 1 1 d . . .
C27 C 0.1372(3) 0.5756(3) 0.1910(3) 0.0216(7) Uani 1 1 d . . .
C28 C 0.2090(3) 0.5252(3) 0.1144(3) 0.0204(6) Uani 1 1 d . . .
C29 C 0.1400(4) 0.5700(3) 0.0126(3) 0.0233(7) Uani 1 1 d . . .
C30 C -0.1546(4) 0.7712(3) 0.2569(3) 0.0267(7) Uani 1 1 d . . .
C31 C -0.2242(4) 0.8288(3) 0.1670(3) 0.0353(9) Uani 1 1 d . . .
C32 C -0.3356(4) 0.9093(3) 0.1643(4) 0.0401(10) Uani 1 1 d . . .
C33 C -0.3821(4) 0.9343(3) 0.2508(4) 0.0378(9) Uani 1 1 d . . .
C34 C -0.3131(4) 0.8773(3) 0.3398(3) 0.0343(9) Uani 1 1 d . . .
C35 C -0.2004(4) 0.7977(3) 0.3433(3) 0.0301(8) Uani 1 1 d . . .
C36 C 0.1396(3) 0.6853(3) -0.0582(3) 0.0240(7) Uani 1 1 d . . .
C37 C 0.2517(4) 0.7125(3) -0.0902(3) 0.0304(8) Uani 1 1 d . . .
C38 C 0.2505(4) 0.8190(4) -0.1512(3) 0.0369(9) Uani 1 1 d . . .
C39 C 0.1384(4) 0.8997(3) -0.1819(3) 0.0362(9) Uani 1 1 d . . .
C40 C 0.0267(4) 0.8733(3) -0.1527(3) 0.0344(9) Uani 1 1 d . . .
C41 C 0.0276(4) 0.7670(3) -0.0915(3) 0.0291(8) Uani 1 1 d . . .
H6A H 0.475(6) 0.409(5) 0.609(5) 0.09(2) Uiso 1 1 d . . .
H6B H 0.456(4) 0.275(4) 0.687(4) 0.045(13) Uiso 1 1 d . . .
H6C H 0.322(6) 0.383(5) 0.634(5) 0.09(2) Uiso 1 1 d . . .
H7A H 0.566(4) 0.336(3) 0.415(4) 0.030(11) Uiso 1 1 d . . .
H7B H 0.631(7) 0.337(6) 0.510(5) 0.09(2) Uiso 1 1 d . . .
H7C H 0.628(11) 0.244(10) 0.524(9) 0.20(5) Uiso 1 1 d . . .
H8 H 0.051(4) 0.173(3) 0.509(3) 0.023(10) Uiso 1 1 d . . .
H9 H -0.059(4) 0.271(3) 0.320(3) 0.032(11) Uiso 1 1 d . . .
H11 H 0.052(3) 0.378(3) 0.175(3) 0.013(8) Uiso 1 1 d . . .
H14 H -0.089(4) 0.093(3) 0.656(3) 0.021(9) Uiso 1 1 d . . .
H15 H -0.247(4) 0.015(4) 0.713(4) 0.042(13) Uiso 1 1 d . . .
H16 H -0.345(4) -0.022(4) 0.604(3) 0.037(12) Uiso 1 1 d . . .
H17 H -0.297(4) 0.045(3) 0.426(3) 0.022(10) Uiso 1 1 d . . .
H18 H -0.140(4) 0.132(3) 0.363(3) 0.023(10) Uiso 1 1 d . . .
H20 H 0.224(4) 0.210(3) 0.188(3) 0.032(11) Uiso 1 1 d . . .
H21 H 0.328(3) 0.093(3) 0.112(3) 0.011(8) Uiso 1 1 d . . .
H22 H 0.484(3) 0.154(3) -0.017(3) 0.012(8) Uiso 1 1 d . . .
H23 H 0.517(3) 0.312(3) -0.051(3) 0.013(9) Uiso 1 1 d . . .
H24 H 0.415(4) 0.421(3) 0.032(3) 0.029(11) Uiso 1 1 d . . .
H25 H 0.014(4) 0.668(3) 0.316(3) 0.033(11) Uiso 1 1 d . . .
H26 H 0.006(3) 0.709(3) 0.108(3) 0.015(9) Uiso 1 1 d . . .
H28 H 0.286(3) 0.540(3) 0.098(3) 0.014(9) Uiso 1 1 d . . .
H29A H 0.060(4) 0.567(3) 0.027(3) 0.025(10) Uiso 1 1 d . . .
H29B H 0.184(5) 0.525(4) -0.025(4) 0.055(15) Uiso 1 1 d . . .
H31 H -0.190(5) 0.818(4) 0.098(4) 0.059(15) Uiso 1 1 d . . .
H32 H -0.377(4) 0.951(3) 0.099(3) 0.033(11) Uiso 1 1 d . . .
H33 H -0.467(5) 0.987(4) 0.250(4) 0.047(13) Uiso 1 1 d . . .
H34 H -0.345(4) 0.893(3) 0.397(3) 0.020(9) Uiso 1 1 d . . .
H35 H -0.149(4) 0.758(3) 0.401(3) 0.032(11) Uiso 1 1 d . . .
H37 H 0.321(4) 0.659(3) -0.069(3) 0.016(9) Uiso 1 1 d . . .
H38 H 0.322(4) 0.835(4) -0.170(3) 0.034(12) Uiso 1 1 d . . .
H39 H 0.143(4) 0.973(4) -0.220(3) 0.041(13) Uiso 1 1 d . . .
H40 H -0.049(4) 0.933(3) -0.171(3) 0.030(11) Uiso 1 1 d . . .
H41 H -0.043(4) 0.752(3) -0.071(3) 0.021(10) Uiso 1 1 d . . .
O1S O -0.3130(4) 1.0788(3) -0.1292(3) 0.0674(11) Uani 1 1 d . . .
C1S C -0.2515(5) 1.1388(4) -0.1419(4) 0.0468(12) Uani 1 1 d . . .
C2S C -0.1404(7) 1.1056(5) -0.0800(5) 0.0588(15) Uani 1 1 d . . .
C3S C -0.2842(6) 1.2517(5) -0.2231(5) 0.0596(14) Uani 1 1 d . . .
H2SA H -0.152(5) 1.156(4) -0.045(4) 0.056(15) Uiso 1 1 d . . .
H2SB H -0.134(6) 1.035(6) -0.031(5) 0.10(2) Uiso 1 1 d . . .
H2SC H -0.066(6) 1.108(5) -0.118(5) 0.09(2) Uiso 1 1 d . . .
H3SA H -0.356(8) 1.291(6) -0.278(6) 0.12(3) Uiso 1 1 d . . .
H3SB H -0.204(7) 1.258(6) -0.283(6) 0.11(2) Uiso 1 1 d . . .
H3SC H -0.290(6) 1.304(6) -0.185(5) 0.10(2) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01905(14) 0.02074(14) 0.02113(14) -0.00684(11) -0.00229(10) -0.00507(11)
Ru2 0.02005(14) 0.02209(14) 0.02017(14) -0.00866(11) -0.00236(10) -0.00346(11)
O1 0.0323(16) 0.0387(16) 0.0424(17) -0.0066(13) -0.0003(13) -0.0184(13)
O2 0.0284(14) 0.0269(14) 0.0423(16) -0.0137(12) -0.0060(12) -0.0005(11)
O3 0.0448(18) 0.0438(17) 0.0263(15) -0.0123(13) 0.0046(13) -0.0092(14)
O4 0.0265(15) 0.0533(19) 0.0426(17) -0.0242(15) -0.0049(12) -0.0080(13)
O5 0.0318(15) 0.0362(15) 0.0304(14) -0.0134(12) -0.0051(11) -0.0090(12)
O6 0.0210(12) 0.0239(12) 0.0206(12) -0.0047(10) -0.0031(9) -0.0068(10)
O7 0.0237(12) 0.0225(12) 0.0203(12) -0.0071(9) -0.0031(9) -0.0055(10)
C1 0.0248(18) 0.0243(17) 0.0277(18) -0.0084(14) -0.0076(14) -0.0059(14)
C2 0.0204(17) 0.0265(18) 0.0252(17) -0.0075(14) -0.0015(13) -0.0073(14)
C3 0.0241(18) 0.0321(19) 0.0275(19) -0.0146(16) -0.0040(15) -0.0007(15)
C4 0.0251(19) 0.034(2) 0.0253(18) -0.0137(15) -0.0013(15) -0.0055(16)
C5 0.033(2) 0.0295(19) 0.035(2) -0.0135(16) -0.0072(17) -0.0056(16)
C6 0.037(3) 0.065(3) 0.033(2) -0.022(2) -0.0047(19) -0.012(2)
C7 0.030(2) 0.081(4) 0.057(3) -0.039(3) -0.005(2) 0.005(3)
C8 0.0213(17) 0.0251(17) 0.0249(17) -0.0097(14) 0.0004(14) -0.0073(14)
C9 0.0200(17) 0.0273(18) 0.0255(18) -0.0108(14) -0.0008(14) -0.0048(14)
C10 0.0223(17) 0.0188(15) 0.0211(16) -0.0078(13) -0.0015(13) -0.0023(13)
C11 0.0173(16) 0.0220(16) 0.0201(16) -0.0077(13) -0.0020(12) -0.0058(13)
C12 0.0200(16) 0.0202(15) 0.0191(15) -0.0061(13) -0.0006(12) -0.0064(13)
C13 0.0219(17) 0.0245(17) 0.0302(19) -0.0086(15) -0.0002(14) -0.0097(14)
C14 0.036(2) 0.035(2) 0.032(2) -0.0089(17) -0.0001(17) -0.0134(18)
C15 0.050(3) 0.048(3) 0.034(2) -0.006(2) 0.009(2) -0.028(2)
C16 0.033(2) 0.040(2) 0.053(3) -0.009(2) 0.006(2) -0.022(2)
C17 0.031(2) 0.035(2) 0.048(3) -0.0152(19) -0.0053(19) -0.0136(18)
C18 0.027(2) 0.032(2) 0.030(2) -0.0102(16) 0.0012(15) -0.0109(16)
C19 0.0213(17) 0.0217(16) 0.0190(15) -0.0068(13) -0.0036(13) -0.0039(13)
C20 0.0239(18) 0.0241(17) 0.0232(17) -0.0078(14) 0.0014(14) -0.0078(14)
C21 0.0283(19) 0.0228(17) 0.034(2) -0.0120(15) -0.0014(15) -0.0070(15)
C22 0.032(2) 0.0273(19) 0.032(2) -0.0149(16) 0.0014(16) -0.0047(16)
C23 0.0260(19) 0.032(2) 0.0263(19) -0.0107(16) 0.0084(15) -0.0074(16)
C24 0.0281(19) 0.0238(17) 0.0278(18) -0.0093(15) 0.0017(15) -0.0087(15)
C25 0.0270(18) 0.0216(16) 0.0217(17) -0.0067(13) -0.0077(14) -0.0029(14)
C26 0.0304(19) 0.0208(17) 0.0233(17) -0.0061(14) -0.0043(14) -0.0082(14)
C27 0.0244(17) 0.0209(16) 0.0202(16) -0.0045(13) -0.0055(13) -0.0096(14)
C28 0.0190(16) 0.0210(16) 0.0220(16) -0.0087(13) -0.0028(13) -0.0052(13)
C29 0.0230(18) 0.0224(17) 0.0231(17) -0.0085(14) -0.0008(14) -0.0051(14)
C30 0.0291(19) 0.0229(17) 0.0269(18) -0.0111(14) -0.0038(15) -0.0027(15)
C31 0.040(2) 0.034(2) 0.028(2) -0.0136(17) -0.0059(17) -0.0006(18)
C32 0.042(2) 0.032(2) 0.038(2) -0.0124(18) -0.0108(19) 0.0021(18)
C33 0.030(2) 0.032(2) 0.048(3) -0.0193(19) -0.0038(18) 0.0007(17)
C34 0.038(2) 0.032(2) 0.036(2) -0.0205(18) 0.0020(18) -0.0074(17)
C35 0.035(2) 0.0306(19) 0.0268(19) -0.0142(16) -0.0032(16) -0.0074(17)
C36 0.0303(19) 0.0245(17) 0.0154(15) -0.0079(13) -0.0006(13) -0.0057(15)
C37 0.026(2) 0.030(2) 0.0284(19) -0.0100(16) 0.0020(15) -0.0036(16)
C38 0.040(2) 0.037(2) 0.033(2) -0.0118(18) 0.0096(18) -0.017(2)
C39 0.052(3) 0.026(2) 0.0238(19) -0.0041(15) 0.0034(17) -0.0127(19)
C40 0.039(2) 0.0268(19) 0.0256(19) -0.0051(15) -0.0062(17) 0.0010(17)
C41 0.031(2) 0.0285(19) 0.0237(18) -0.0061(15) -0.0044(15) -0.0066(16)
O1S 0.070(3) 0.066(2) 0.093(3) -0.049(2) 0.020(2) -0.041(2)
C1S 0.047(3) 0.049(3) 0.060(3) -0.037(2) 0.019(2) -0.022(2)
C2S 0.079(5) 0.048(3) 0.054(3) -0.018(3) -0.006(3) -0.024(3)
C3S 0.044(3) 0.054(3) 0.080(4) -0.023(3) -0.013(3) -0.012(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100882.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-27 05:05:50 +0300 (Sun, 27 Mar 2016) $
#$Revision: 180535 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100882.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100882
loop_
_publ_author_name
'Panda, Tarun K.'
'Zulys, Agustino'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
Bis(phosphinimino)methanides: Synthesis, Structure, and
Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2197
_journal_page_last 2202
_journal_paper_doi 10.1021/om0491138
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C41.5 H52 N2 P2 Si2 Y'
_chemical_formula_weight 785.88
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 93.146(4)
_cell_angle_beta 92.938(4)
_cell_angle_gamma 98.530(4)
_cell_formula_units_Z 2
_cell_length_a 9.4016(17)
_cell_length_b 9.5304(16)
_cell_length_c 22.771(4)
_cell_measurement_temperature 173(2)
_cell_volume 2011.1(6)
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_collection 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL''
_computing_molecular_graphics 'Diamond 2.1a '
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type 'Bruker Smart 1000 CCD'
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0183
_diffrn_reflns_av_sigmaI/netI 0.0309
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 25111
_diffrn_reflns_theta_full 30.52
_diffrn_reflns_theta_max 30.52
_diffrn_reflns_theta_min 0.90
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.620
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.795879
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.298
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 824
_exptl_crystal_size_max .58
_exptl_crystal_size_mid .36
_exptl_crystal_size_min .1
_refine_diff_density_max 1.005
_refine_diff_density_min -0.334
_refine_diff_density_rms 0.070
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 12116
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0465
_refine_ls_R_factor_gt 0.0341
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.4061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0875
_refine_ls_wR_factor_ref 0.0949
_reflns_number_gt 10132
_reflns_number_total 12116
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060417
_cod_data_source_file om0491138si20041116_113831.cif
_cod_data_source_block 1a
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C41.50 H52 N2 P2 Si2 Y'
_cod_database_code 1100882
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.536698(16) 0.781580(17) 0.743874(7) 0.02018(5) Uani 1 1 d . . .
P1 P 0.77196(4) 0.88677(4) 0.659539(18) 0.01845(8) Uani 1 1 d . . .
P2 P 0.83060(4) 0.95561(4) 0.794163(18) 0.01820(8) Uani 1 1 d . . .
Si1 Si 0.51121(6) 1.04750(6) 0.63883(2) 0.02661(11) Uani 1 1 d . . .
Si2 Si 0.61705(5) 1.03727(6) 0.87687(2) 0.02512(10) Uani 1 1 d . . .
N1 N 0.61263(15) 0.92362(15) 0.66319(6) 0.0218(3) Uani 1 1 d . . .
N2 N 0.66760(14) 0.96187(15) 0.81126(6) 0.0191(3) Uani 1 1 d . . .
C1 C 0.5242(2) 0.5109(2) 0.72394(12) 0.0438(6) Uani 1 1 d . . .
H1 H 0.5931 0.4543 0.7110 0.053 Uiso 1 1 calc R . .
C2 C 0.4397(3) 0.5511(2) 0.67709(10) 0.0428(5) Uani 1 1 d . . .
H2 H 0.4598 0.5093 0.6402 0.051 Uiso 1 1 calc R . .
C3 C 0.3327(3) 0.6380(2) 0.67174(11) 0.0456(6) Uani 1 1 d . . .
H3 H 0.2959 0.6397 0.6322 0.055 Uiso 1 1 calc R . .
C4 C 0.2672(2) 0.7230(2) 0.71083(13) 0.0481(6) Uani 1 1 d . . .
H4 H 0.2038 0.7767 0.6913 0.058 Uiso 1 1 calc R . .
C5 C 0.2739(2) 0.7474(2) 0.77314(14) 0.0501(7) Uani 1 1 d . . .
H5 H 0.2129 0.8127 0.7859 0.060 Uiso 1 1 calc R . .
C6 C 0.3500(3) 0.6971(3) 0.81973(11) 0.0489(6) Uani 1 1 d . . .
H6 H 0.3232 0.7307 0.8570 0.059 Uiso 1 1 calc R . .
C7 C 0.4560(3) 0.6091(3) 0.82492(11) 0.0500(6) Uani 1 1 d . . .
H7 H 0.4838 0.5971 0.8648 0.060 Uiso 1 1 calc R . .
C8 C 0.5311(3) 0.5344(2) 0.78514(12) 0.0459(6) Uani 1 1 d . . .
H8 H 0.6029 0.4897 0.8042 0.055 Uiso 1 1 calc R . .
C9 C 0.82895(17) 0.84649(17) 0.72960(7) 0.0188(3) Uani 1 1 d . . .
H9 H 0.8859 0.7660 0.7317 0.023 Uiso 1 1 calc R . .
C10 C 0.78065(18) 0.72718(18) 0.61287(8) 0.0231(3) Uani 1 1 d . . .
C11 C 0.8976(2) 0.6535(2) 0.61861(9) 0.0351(4) Uani 1 1 d . . .
H11 H 0.9712 0.6841 0.6487 0.042 Uiso 1 1 calc R . .
C12 C 0.9083(3) 0.5364(2) 0.58113(11) 0.0480(6) Uani 1 1 d . . .
H12 H 0.9877 0.4861 0.5860 0.058 Uiso 1 1 calc R . .
C13 C 0.8035(3) 0.4932(2) 0.53680(11) 0.0472(6) Uani 1 1 d . . .
H13 H 0.8108 0.4132 0.5110 0.057 Uiso 1 1 calc R . .
C14 C 0.6884(3) 0.5653(3) 0.52967(10) 0.0467(6) Uani 1 1 d . . .
H14 H 0.6173 0.5359 0.4985 0.056 Uiso 1 1 calc R . .
C15 C 0.6753(2) 0.6815(2) 0.56798(9) 0.0352(4) Uani 1 1 d . . .
H15 H 0.5942 0.7295 0.5634 0.042 Uiso 1 1 calc R . .
C16 C 0.88893(18) 1.01652(18) 0.62080(8) 0.0223(3) Uani 1 1 d . . .
C17 C 0.8511(2) 1.0343(2) 0.56191(8) 0.0316(4) Uani 1 1 d . . .
H17 H 0.7671 0.9788 0.5432 0.038 Uiso 1 1 calc R . .
C18 C 0.9352(2) 1.1326(2) 0.53048(9) 0.0372(5) Uani 1 1 d . . .
H18 H 0.9089 1.1438 0.4904 0.045 Uiso 1 1 calc R . .
C19 C 1.0566(2) 1.2136(2) 0.55738(10) 0.0368(5) Uani 1 1 d . . .
H19 H 1.1132 1.2817 0.5359 0.044 Uiso 1 1 calc R . .
C20 C 1.0963(2) 1.1966(2) 0.61517(11) 0.0393(5) Uani 1 1 d . . .
H20 H 1.1802 1.2529 0.6336 0.047 Uiso 1 1 calc R . .
C21 C 1.01322(19) 1.0962(2) 0.64683(9) 0.0308(4) Uani 1 1 d . . .
H21 H 1.0424 1.0828 0.6864 0.037 Uiso 1 1 calc R . .
C22 C 0.93096(18) 0.87253(19) 0.84966(8) 0.0236(3) Uani 1 1 d . . .
C23 C 0.9143(2) 0.7245(2) 0.84842(9) 0.0313(4) Uani 1 1 d . . .
H23 H 0.8600 0.6697 0.8165 0.038 Uiso 1 1 calc R . .
C24 C 0.9760(3) 0.6566(3) 0.89315(10) 0.0432(5) Uani 1 1 d . . .
H24 H 0.9652 0.5557 0.8915 0.052 Uiso 1 1 calc R . .
C25 C 1.0536(3) 0.7353(3) 0.94027(10) 0.0464(6) Uani 1 1 d . . .
H25 H 1.0949 0.6886 0.9712 0.056 Uiso 1 1 calc R . .
C26 C 1.0707(2) 0.8824(3) 0.94233(10) 0.0443(6) Uani 1 1 d . . .
H26 H 1.1244 0.9365 0.9746 0.053 Uiso 1 1 calc R . .
C27 C 1.0097(2) 0.9510(2) 0.89750(9) 0.0337(4) Uani 1 1 d . . .
H27 H 1.0214 1.0519 0.8993 0.040 Uiso 1 1 calc R . .
C28 C 0.92503(18) 1.13421(18) 0.78744(8) 0.0241(3) Uani 1 1 d . . .
C29 C 1.0753(2) 1.1695(2) 0.79577(9) 0.0322(4) Uani 1 1 d . . .
H29 H 1.1313 1.1016 0.8096 0.039 Uiso 1 1 calc R . .
C30 C 1.1423(2) 1.3049(2) 0.78361(11) 0.0430(5) Uani 1 1 d . . .
H30 H 1.2438 1.3293 0.7900 0.052 Uiso 1 1 calc R . .
C31 C 1.0625(3) 1.4030(2) 0.76241(12) 0.0482(6) Uani 1 1 d . . .
H31 H 1.1088 1.4945 0.7539 0.058 Uiso 1 1 calc R . .
C32 C 0.9139(3) 1.3679(2) 0.75346(12) 0.0424(5) Uani 1 1 d . . .
H32 H 0.8588 1.4354 0.7385 0.051 Uiso 1 1 calc R . .
C33 C 0.8453(2) 1.2341(2) 0.76626(9) 0.0314(4) Uani 1 1 d . . .
H33 H 0.7435 1.2112 0.7605 0.038 Uiso 1 1 calc R . .
C34 C 0.3794(3) 0.9672(3) 0.57754(10) 0.0485(6) Uani 1 1 d . . .
H34A H 0.4315 0.9330 0.5448 0.073 Uiso 1 1 calc R . .
H34B H 0.3229 1.0390 0.5641 0.073 Uiso 1 1 calc R . .
H34C H 0.3148 0.8874 0.5916 0.073 Uiso 1 1 calc R . .
C35 C 0.6127(3) 1.2138(2) 0.61272(11) 0.0463(6) Uani 1 1 d . . .
H35A H 0.6967 1.2471 0.6398 0.070 Uiso 1 1 calc R . .
H35B H 0.5499 1.2871 0.6114 0.070 Uiso 1 1 calc R . .
H35C H 0.6447 1.1944 0.5732 0.070 Uiso 1 1 calc R . .
C36 C 0.4122(2) 1.1035(2) 0.70309(9) 0.0320(4) Uani 1 1 d . . .
H36A H 0.3405 1.0239 0.7128 0.048 Uiso 1 1 calc R . .
H36B H 0.3637 1.1840 0.6931 0.048 Uiso 1 1 calc R . .
H36C H 0.4806 1.1320 0.7371 0.048 Uiso 1 1 calc R . .
C37 C 0.6200(3) 0.9108(3) 0.93664(9) 0.0410(5) Uani 1 1 d . . .
H37A H 0.5463 0.8275 0.9270 0.062 Uiso 1 1 calc R . .
H37B H 0.6001 0.9580 0.9740 0.062 Uiso 1 1 calc R . .
H37C H 0.7150 0.8805 0.9403 0.062 Uiso 1 1 calc R . .
C38 C 0.4320(2) 1.0826(2) 0.86641(9) 0.0365(5) Uani 1 1 d . . .
H38A H 0.4334 1.1617 0.8406 0.055 Uiso 1 1 calc R . .
H38B H 0.3980 1.1102 0.9047 0.055 Uiso 1 1 calc R . .
H38C H 0.3672 0.9996 0.8484 0.055 Uiso 1 1 calc R . .
C39 C 0.7355(2) 1.2066(2) 0.90452(10) 0.0393(5) Uani 1 1 d . . .
H39A H 0.8356 1.1897 0.9090 0.059 Uiso 1 1 calc R . .
H39B H 0.7044 1.2391 0.9427 0.059 Uiso 1 1 calc R . .
H39C H 0.7281 1.2795 0.8763 0.059 Uiso 1 1 calc R . .
C100 C 0.2426(6) 0.3789(6) 0.9495(3) 0.0864(14) Uiso 0.75 1 d P . .
C101 C 0.3100(7) 0.4677(7) 0.9807(3) 0.0960(16) Uiso 0.75 1 d P . .
C102 C 0.4323(7) 0.4148(7) 0.9684(3) 0.0592(14) Uiso 0.50 1 d P . .
C103 C 0.5214(6) 0.5332(6) 1.0069(3) 0.0514(13) Uiso 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01623(7) 0.01943(8) 0.02295(8) 0.00151(6) 0.00188(5) -0.00387(5)
P1 0.01750(18) 0.01855(19) 0.01920(19) 0.00177(15) 0.00337(14) 0.00137(14)
P2 0.01381(17) 0.01897(19) 0.02080(19) -0.00069(15) 0.00014(14) 0.00019(14)
Si1 0.0302(2) 0.0308(3) 0.0220(2) 0.00552(19) 0.00319(19) 0.0128(2)
Si2 0.0216(2) 0.0321(3) 0.0216(2) -0.00350(19) 0.00223(17) 0.00542(19)
N1 0.0190(6) 0.0241(7) 0.0232(7) 0.0051(5) 0.0032(5) 0.0045(5)
N2 0.0146(6) 0.0208(7) 0.0208(6) -0.0005(5) 0.0014(5) -0.0003(5)
C1 0.0350(11) 0.0222(10) 0.0725(17) -0.0023(10) 0.0105(11) -0.0022(8)
C2 0.0501(13) 0.0288(10) 0.0425(12) -0.0101(9) 0.0093(10) -0.0147(9)
C3 0.0451(13) 0.0383(12) 0.0437(12) 0.0037(10) -0.0162(10) -0.0196(10)
C4 0.0219(9) 0.0318(11) 0.0859(19) 0.0102(12) -0.0120(10) -0.0081(8)
C5 0.0227(9) 0.0291(11) 0.095(2) -0.0084(12) 0.0244(11) -0.0092(8)
C6 0.0487(13) 0.0419(13) 0.0494(13) -0.0060(11) 0.0275(11) -0.0198(11)
C7 0.0662(16) 0.0395(13) 0.0370(12) 0.0161(10) 0.0037(11) -0.0212(12)
C8 0.0431(12) 0.0261(10) 0.0656(16) 0.0155(10) -0.0095(11) -0.0049(9)
C9 0.0177(7) 0.0176(7) 0.0210(7) 0.0014(6) 0.0017(6) 0.0023(6)
C10 0.0242(8) 0.0210(8) 0.0234(8) -0.0001(6) 0.0075(6) -0.0008(6)
C11 0.0420(11) 0.0324(10) 0.0329(10) -0.0020(8) 0.0028(8) 0.0134(9)
C12 0.0733(17) 0.0336(12) 0.0432(13) 0.0015(10) 0.0162(12) 0.0242(11)
C13 0.0688(16) 0.0255(10) 0.0446(13) -0.0082(9) 0.0283(12) -0.0060(10)
C14 0.0423(12) 0.0513(14) 0.0374(11) -0.0176(10) 0.0128(9) -0.0195(10)
C15 0.0265(9) 0.0445(12) 0.0315(10) -0.0082(8) 0.0066(7) -0.0026(8)
C16 0.0227(8) 0.0209(8) 0.0245(8) 0.0040(6) 0.0081(6) 0.0040(6)
C17 0.0371(10) 0.0335(10) 0.0246(9) 0.0051(7) 0.0063(7) 0.0034(8)
C18 0.0463(12) 0.0390(11) 0.0310(10) 0.0137(8) 0.0151(9) 0.0130(9)
C19 0.0372(10) 0.0298(10) 0.0486(12) 0.0177(9) 0.0234(9) 0.0090(8)
C20 0.0269(9) 0.0374(11) 0.0527(13) 0.0122(10) 0.0107(9) -0.0040(8)
C21 0.0220(8) 0.0354(10) 0.0344(10) 0.0088(8) 0.0043(7) -0.0004(7)
C22 0.0170(7) 0.0302(9) 0.0235(8) -0.0001(7) -0.0004(6) 0.0045(6)
C23 0.0356(10) 0.0317(10) 0.0271(9) 0.0034(7) -0.0029(7) 0.0079(8)
C24 0.0548(14) 0.0420(12) 0.0361(11) 0.0082(9) -0.0051(10) 0.0183(11)
C25 0.0506(13) 0.0649(16) 0.0289(10) 0.0071(10) -0.0067(9) 0.0273(12)
C26 0.0388(11) 0.0652(16) 0.0288(10) -0.0067(10) -0.0128(9) 0.0166(11)
C27 0.0290(9) 0.0403(11) 0.0307(10) -0.0075(8) -0.0061(7) 0.0082(8)
C28 0.0194(7) 0.0197(8) 0.0307(9) -0.0038(7) 0.0030(6) -0.0036(6)
C29 0.0195(8) 0.0304(10) 0.0438(11) -0.0041(8) 0.0013(7) -0.0033(7)
C30 0.0242(9) 0.0364(11) 0.0624(15) -0.0084(10) 0.0071(9) -0.0126(8)
C31 0.0420(12) 0.0238(10) 0.0741(17) -0.0018(10) 0.0133(11) -0.0117(9)
C32 0.0405(11) 0.0209(9) 0.0659(15) 0.0049(9) 0.0093(11) 0.0015(8)
C33 0.0235(8) 0.0231(9) 0.0462(11) 0.0005(8) 0.0053(8) -0.0014(7)
C34 0.0542(14) 0.0636(16) 0.0312(11) -0.0010(10) -0.0125(10) 0.0270(12)
C35 0.0660(16) 0.0331(11) 0.0480(13) 0.0164(10) 0.0250(12) 0.0215(11)
C36 0.0292(9) 0.0385(11) 0.0315(9) 0.0038(8) 0.0058(7) 0.0134(8)
C37 0.0453(12) 0.0555(14) 0.0237(9) 0.0057(9) 0.0059(8) 0.0099(10)
C38 0.0268(9) 0.0473(12) 0.0366(11) -0.0065(9) 0.0034(8) 0.0121(8)
C39 0.0347(10) 0.0418(12) 0.0387(11) -0.0172(9) -0.0014(8) 0.0056(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Y1 N1 89.25(5) . . ?
N2 Y1 C5 106.76(7) . . ?
N1 Y1 C5 121.41(8) . . ?
N2 Y1 C4 132.01(7) . . ?
N1 Y1 C4 97.62(7) . . ?
C5 Y1 C4 32.07(9) . . ?
N2 Y1 C8 110.65(7) . . ?
N1 Y1 C8 144.01(7) . . ?
C5 Y1 C8 82.35(8) . . ?
C4 Y1 C8 90.83(8) . . ?
N2 Y1 C1 136.55(7) . . ?
N1 Y1 C1 115.33(7) . . ?
C5 Y1 C1 90.79(7) . . ?
C4 Y1 C1 82.07(8) . . ?
C8 Y1 C1 31.42(8) . . ?
N2 Y1 C6 93.37(6) . . ?
N1 Y1 C6 151.45(8) . . ?
C5 Y1 C6 31.31(9) . . ?
C4 Y1 C6 60.22(9) . . ?
C8 Y1 C6 60.02(9) . . ?
C1 Y1 C6 81.35(8) . . ?
N2 Y1 C7 94.83(6) . . ?
N1 Y1 C7 175.07(7) . . ?
C5 Y1 C7 59.96(10) . . ?
C4 Y1 C7 81.69(9) . . ?
C8 Y1 C7 31.41(9) . . ?
C1 Y1 C7 59.74(9) . . ?
C6 Y1 C7 31.17(9) . . ?
N2 Y1 C2 166.96(7) . . ?
N1 Y1 C2 95.02(6) . . ?
C5 Y1 C2 81.48(8) . . ?
C4 Y1 C2 59.65(8) . . ?
C8 Y1 C2 59.64(8) . . ?
C1 Y1 C2 31.27(8) . . ?
C6 Y1 C2 88.75(7) . . ?
C7 Y1 C2 80.40(8) . . ?
N2 Y1 C3 161.94(7) . . ?
N1 Y1 C3 88.28(6) . . ?
C5 Y1 C3 60.03(9) . . ?
C4 Y1 C3 31.13(9) . . ?
C8 Y1 C3 81.12(8) . . ?
C1 Y1 C3 59.67(8) . . ?
C6 Y1 C3 80.51(8) . . ?
C7 Y1 C3 88.67(8) . . ?
C2 Y1 C3 30.94(8) . . ?
N2 Y1 C9 63.82(5) . . ?
N1 Y1 C9 62.01(5) . . ?
C5 Y1 C9 170.46(7) . . ?
C4 Y1 C9 156.30(8) . . ?
C8 Y1 C9 99.29(7) . . ?
C1 Y1 C9 95.45(6) . . ?
C6 Y1 C9 142.97(8) . . ?
C7 Y1 C9 117.49(7) . . ?
C2 Y1 C9 107.51(6) . . ?
C3 Y1 C9 129.47(7) . . ?
N2 Y1 P1 83.83(3) . . ?
N1 Y1 P1 30.58(3) . . ?
C5 Y1 P1 151.44(7) . . ?
C4 Y1 P1 122.99(7) . . ?
C8 Y1 P1 119.39(6) . . ?
C1 Y1 P1 99.50(5) . . ?
C6 Y1 P1 176.72(6) . . ?
C7 Y1 P1 147.20(7) . . ?
C2 Y1 P1 93.60(5) . . ?
C3 Y1 P1 102.66(6) . . ?
C9 Y1 P1 33.92(3) . . ?
N1 P1 C9 107.37(8) . . ?
N1 P1 C10 113.16(8) . . ?
C9 P1 C10 104.81(8) . . ?
N1 P1 C16 112.86(8) . . ?
C9 P1 C16 118.65(8) . . ?
C10 P1 C16 99.66(8) . . ?
N1 P1 Y1 50.48(5) . . ?
C9 P1 Y1 62.61(5) . . ?
C10 P1 Y1 102.40(5) . . ?
C16 P1 Y1 156.60(5) . . ?
N2 P2 C9 109.38(7) . . ?
N2 P2 C28 110.10(8) . . ?
C9 P2 C28 112.58(8) . . ?
N2 P2 C22 111.94(8) . . ?
C9 P2 C22 104.98(8) . . ?
C28 P2 C22 107.79(8) . . ?
N2 P2 Y1 48.46(5) . . ?
C9 P2 Y1 61.55(5) . . ?
C28 P2 Y1 135.53(6) . . ?
C22 P2 Y1 116.35(6) . . ?
N1 Si1 C35 116.47(10) . . ?
N1 Si1 C34 110.45(10) . . ?
C35 Si1 C34 107.31(13) . . ?
N1 Si1 C36 106.45(8) . . ?
C35 Si1 C36 106.29(10) . . ?
C34 Si1 C36 109.68(11) . . ?
N2 Si2 C38 109.83(8) . . ?
N2 Si2 C37 110.56(9) . . ?
C38 Si2 C37 108.99(11) . . ?
N2 Si2 C39 114.20(9) . . ?
C38 Si2 C39 106.11(10) . . ?
C37 Si2 C39 106.96(11) . . ?
P1 N1 Si1 139.18(9) . . ?
P1 N1 Y1 98.93(7) . . ?
Si1 N1 Y1 120.23(7) . . ?
P2 N2 Si2 125.51(8) . . ?
P2 N2 Y1 101.28(6) . . ?
Si2 N2 Y1 130.00(7) . . ?
C8 C1 C2 135.1(2) . . ?
C8 C1 Y1 74.24(13) . . ?
C2 C1 Y1 76.01(12) . . ?
C3 C2 C1 135.2(2) . . ?
C3 C2 Y1 74.78(12) . . ?
C1 C2 Y1 72.73(12) . . ?
C4 C3 C2 135.1(2) . . ?
C4 C3 Y1 72.42(12) . . ?
C2 C3 Y1 74.28(12) . . ?
C3 C4 C5 134.6(2) . . ?
C3 C4 Y1 76.45(13) . . ?
C5 C4 Y1 73.75(12) . . ?
C6 C5 C4 134.3(2) . . ?
C6 C5 Y1 75.48(12) . . ?
C4 C5 Y1 74.17(12) . . ?
C5 C6 C7 135.6(2) . . ?
C5 C6 Y1 73.20(12) . . ?
C7 C6 Y1 74.65(13) . . ?
C6 C7 C8 135.1(2) . . ?
C6 C7 Y1 74.18(13) . . ?
C8 C7 Y1 73.20(13) . . ?
C1 C8 C7 134.6(2) . . ?
C1 C8 Y1 74.35(13) . . ?
C7 C8 Y1 75.39(13) . . ?
P1 C9 P2 125.58(10) . . ?
P1 C9 Y1 83.47(6) . . ?
P2 C9 Y1 84.60(6) . . ?
C15 C10 C11 118.38(17) . . ?
C15 C10 P1 120.57(15) . . ?
C11 C10 P1 120.91(14) . . ?
C12 C11 C10 121.1(2) . . ?
C13 C12 C11 119.7(2) . . ?
C14 C13 C12 120.3(2) . . ?
C13 C14 C15 120.3(2) . . ?
C10 C15 C14 120.2(2) . . ?
C21 C16 C17 118.80(17) . . ?
C21 C16 P1 123.13(14) . . ?
C17 C16 P1 118.06(14) . . ?
C18 C17 C16 120.5(2) . . ?
C19 C18 C17 120.0(2) . . ?
C20 C19 C18 120.30(18) . . ?
C19 C20 C21 120.0(2) . . ?
C16 C21 C20 120.34(19) . . ?
C23 C22 C27 118.62(18) . . ?
C23 C22 P2 118.69(14) . . ?
C27 C22 P2 122.20(15) . . ?
C24 C23 C22 120.73(19) . . ?
C25 C24 C23 120.1(2) . . ?
C24 C25 C26 119.9(2) . . ?
C25 C26 C27 120.2(2) . . ?
C26 C27 C22 120.4(2) . . ?
C33 C28 C29 119.24(17) . . ?
C33 C28 P2 117.43(13) . . ?
C29 C28 P2 122.86(15) . . ?
C30 C29 C28 119.8(2) . . ?
C31 C30 C29 120.5(2) . . ?
C30 C31 C32 119.8(2) . . ?
C31 C32 C33 120.3(2) . . ?
C28 C33 C32 120.29(18) . . ?
C101 C100 C102 49.3(4) . . ?
C100 C101 C102 90.3(6) . . ?
C100 C101 C103 119.7(6) . 2_667 ?
C102 C101 C103 29.8(3) . 2_667 ?
C103 C102 C101 92.0(8) 2_667 . ?
C103 C102 C103 10.4(8) 2_667 . ?
C101 C102 C103 90.7(5) . . ?
C103 C102 C100 132.0(8) 2_667 . ?
C101 C102 C100 40.5(3) . . ?
C103 C102 C100 131.1(5) . . ?
C103 C103 C102 158.4(16) 2_667 2_667 ?
C103 C103 C102 11.2(8) 2_667 . ?
C102 C103 C102 169.6(8) 2_667 . ?
C103 C103 C101 116.7(11) 2_667 2_667 ?
C102 C103 C101 58.2(7) 2_667 2_667 ?
C102 C103 C101 119.9(5) . 2_667 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 N2 2.3899(14) . ?
Y1 N1 2.4163(14) . ?
Y1 C5 2.571(2) . ?
Y1 C4 2.576(2) . ?
Y1 C8 2.578(2) . ?
Y1 C1 2.579(2) . ?
Y1 C6 2.600(2) . ?
Y1 C7 2.606(2) . ?
Y1 C2 2.621(2) . ?
Y1 C3 2.627(2) . ?
Y1 C9 2.7654(16) . ?
Y1 P1 3.0942(6) . ?
P1 N1 1.5936(15) . ?
P1 C9 1.7378(17) . ?
P1 C10 1.8215(17) . ?
P1 C16 1.8255(17) . ?
P2 N2 1.6091(14) . ?
P2 C9 1.7517(16) . ?
P2 C28 1.8174(18) . ?
P2 C22 1.8231(18) . ?
Si1 N1 1.7211(15) . ?
Si1 C35 1.868(2) . ?
Si1 C34 1.869(2) . ?
Si1 C36 1.8692(19) . ?
Si2 N2 1.7409(14) . ?
Si2 C38 1.860(2) . ?
Si2 C37 1.869(2) . ?
Si2 C39 1.877(2) . ?
C1 C8 1.396(4) . ?
C1 C2 1.402(4) . ?
C2 C3 1.400(4) . ?
C3 C4 1.397(4) . ?
C4 C5 1.422(4) . ?
C5 C6 1.396(4) . ?
C6 C7 1.399(4) . ?
C7 C8 1.403(4) . ?
C10 C15 1.391(3) . ?
C10 C11 1.394(3) . ?
C11 C12 1.387(3) . ?
C12 C13 1.375(4) . ?
C13 C14 1.372(4) . ?
C14 C15 1.396(3) . ?
C16 C21 1.382(3) . ?
C16 C17 1.396(3) . ?
C17 C18 1.387(3) . ?
C18 C19 1.374(3) . ?
C19 C20 1.374(3) . ?
C20 C21 1.399(3) . ?
C22 C23 1.395(3) . ?
C22 C27 1.399(3) . ?
C23 C24 1.384(3) . ?
C24 C25 1.384(3) . ?
C25 C26 1.385(4) . ?
C26 C27 1.387(3) . ?
C28 C33 1.388(3) . ?
C28 C29 1.403(2) . ?
C29 C30 1.398(3) . ?
C30 C31 1.375(4) . ?
C31 C32 1.389(3) . ?
C32 C33 1.394(3) . ?
C100 C101 1.163(7) . ?
C100 C102 1.791(9) . ?
C101 C102 1.357(8) . ?
C101 C103 1.597(9) 2_667 ?
C102 C103 0.794(7) 2_667 ?
C102 C103 1.509(9) . ?
C103 C103 0.742(10) 2_667 ?
C103 C102 0.794(7) 2_667 ?
C103 C101 1.597(9) 2_667 ?
|
1100883.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-27 05:05:50 +0300 (Sun, 27 Mar 2016) $
#$Revision: 180535 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100883.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100883
loop_
_publ_author_name
'Panda, Tarun K.'
'Zulys, Agustino'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
Bis(phosphinimino)methanides: Synthesis, Structure, and
Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2197
_journal_page_last 2202
_journal_paper_doi 10.1021/om0491138
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C39 H47 N2 P2 Si2 Sm'
_chemical_formula_weight 812.26
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 99.364(8)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.3050(8)
_cell_length_b 19.6230(13)
_cell_length_c 15.6500(10)
_cell_measurement_temperature 203(2)
_cell_volume 3728.5(4)
_computing_molecular_graphics 'Diamond 2.1e'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 203(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type Stoe-IPDS
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type AgK\a
_diffrn_radiation_wavelength 0.56087
_diffrn_reflns_av_R_equivalents 0.1285
_diffrn_reflns_av_sigmaI/netI 0.0876
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 24303
_diffrn_reflns_theta_full 20.81
_diffrn_reflns_theta_max 20.81
_diffrn_reflns_theta_min 1.54
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.938
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.447
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plates
_exptl_crystal_F_000 1660
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.24
_refine_diff_density_max 2.180
_refine_diff_density_min -2.106
_refine_diff_density_rms 0.243
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 421
_refine_ls_number_reflns 7714
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.120
_refine_ls_R_factor_all 0.0721
_refine_ls_R_factor_gt 0.0585
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1619
_refine_ls_wR_factor_ref 0.1742
_reflns_number_gt 5976
_reflns_number_total 7714
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060418
_cod_data_source_file om0491138si20041116_113831.cif
_cod_data_source_block 1b
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100883
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1097(5) 0.1802(3) 0.4317(4) 0.0440(14) Uani 1 1 d . . .
H1 H -0.1167 0.1451 0.3902 0.053 Uiso 1 1 calc R . .
C2 C -0.0991(5) 0.1551(3) 0.5176(5) 0.0438(15) Uani 1 1 d . . .
H2A H -0.1012 0.1073 0.5204 0.053 Uiso 1 1 calc R . .
C3 C -0.0859(4) 0.1865(3) 0.6003(4) 0.0372(13) Uani 1 1 d . . .
H3A H -0.0763 0.1546 0.6458 0.045 Uiso 1 1 calc R . .
C4 C -0.0839(5) 0.2534(2) 0.6298(4) 0.0347(14) Uani 1 1 d . . .
H4A H -0.0762 0.2562 0.6904 0.042 Uiso 1 1 calc R . .
C5 C -0.0907(4) 0.3176(3) 0.5904(4) 0.0347(12) Uani 1 1 d . . .
H5A H -0.0863 0.3531 0.6311 0.042 Uiso 1 1 calc R . .
C6 C -0.1025(5) 0.3420(3) 0.5052(4) 0.0369(12) Uani 1 1 d . . .
H6A H -0.1054 0.3898 0.5020 0.044 Uiso 1 1 calc R . .
C7 C -0.1111(5) 0.3109(3) 0.4232(4) 0.0381(12) Uani 1 1 d . . .
H7A H -0.1174 0.3425 0.3776 0.046 Uiso 1 1 calc R . .
C8 C -0.1122(5) 0.2440(3) 0.3951(4) 0.0425(15) Uani 1 1 d . . .
H8A H -0.1155 0.2415 0.3347 0.051 Uiso 1 1 calc R . .
C9 C 0.1872(5) 0.25479(18) 0.3926(3) 0.0206(10) Uani 1 1 d . . .
H9A H 0.1484 0.2568 0.3321 0.025 Uiso 1 1 calc R . .
C10 C 0.1588(4) 0.3960(2) 0.3716(3) 0.0246(9) Uani 1 1 d . . .
C11 C 0.1576(4) 0.3979(3) 0.2836(3) 0.0353(11) Uani 1 1 d . . .
H11A H 0.1976 0.3656 0.2570 0.042 Uiso 1 1 calc R . .
C12 C 0.0980(5) 0.4470(3) 0.2349(4) 0.0484(14) Uani 1 1 d . . .
H12A H 0.0981 0.4484 0.1749 0.058 Uiso 1 1 calc R . .
C13 C 0.0379(5) 0.4945(3) 0.2717(4) 0.0495(15) Uani 1 1 d . . .
H13A H -0.0046 0.5271 0.2371 0.059 Uiso 1 1 calc R . .
C14 C 0.0409(4) 0.4937(3) 0.3589(4) 0.0425(13) Uani 1 1 d . . .
H14A H 0.0018 0.5269 0.3849 0.051 Uiso 1 1 calc R . .
C15 C 0.1009(4) 0.4443(2) 0.4103(4) 0.0342(11) Uani 1 1 d . . .
H15A H 0.1021 0.4439 0.4706 0.041 Uiso 1 1 calc R . .
C16 C 0.3770(4) 0.3497(2) 0.4236(3) 0.0219(9) Uani 1 1 d . . .
C17 C 0.4401(3) 0.3980(2) 0.4737(3) 0.0236(9) Uani 1 1 d . . .
H17A H 0.4099 0.4224 0.5160 0.028 Uiso 1 1 calc R . .
C18 C 0.5476(4) 0.4107(2) 0.4618(3) 0.0310(10) Uani 1 1 d . . .
H18A H 0.5904 0.4431 0.4966 0.037 Uiso 1 1 calc R . .
C19 C 0.5914(4) 0.3762(3) 0.3995(3) 0.0333(11) Uani 1 1 d . . .
H19A H 0.6646 0.3842 0.3921 0.040 Uiso 1 1 calc R . .
C20 C 0.5285(4) 0.3298(3) 0.3478(3) 0.0374(12) Uani 1 1 d . . .
H20A H 0.5584 0.3068 0.3043 0.045 Uiso 1 1 calc R . .
C21 C 0.4211(4) 0.3167(2) 0.3594(3) 0.0308(10) Uani 1 1 d . . .
H21A H 0.3783 0.2851 0.3233 0.037 Uiso 1 1 calc R . .
C22 C 0.1997(4) 0.1194(2) 0.3375(3) 0.0238(9) Uani 1 1 d . . .
C23 C 0.1438(4) 0.0594(2) 0.3476(3) 0.0331(11) Uani 1 1 d . . .
H23A H 0.1242 0.0485 0.4015 0.040 Uiso 1 1 calc R . .
C24 C 0.1170(5) 0.0159(3) 0.2782(4) 0.0428(13) Uani 1 1 d . . .
H24A H 0.0807 -0.0253 0.2857 0.051 Uiso 1 1 calc R . .
C25 C 0.1425(4) 0.0317(3) 0.1986(3) 0.0395(12) Uani 1 1 d . . .
H25A H 0.1240 0.0016 0.1517 0.047 Uiso 1 1 calc R . .
C26 C 0.1955(4) 0.0919(3) 0.1878(3) 0.0337(11) Uani 1 1 d . . .
H26A H 0.2124 0.1035 0.1331 0.040 Uiso 1 1 calc R . .
C27 C 0.2241(4) 0.1357(2) 0.2570(3) 0.0287(10) Uani 1 1 d . . .
H27A H 0.2603 0.1768 0.2492 0.034 Uiso 1 1 calc R . .
C28 C 0.3869(4) 0.1745(2) 0.4527(3) 0.0253(9) Uani 1 1 d . . .
C29 C 0.4556(4) 0.1447(2) 0.4010(3) 0.0361(11) Uani 1 1 d . . .
H29A H 0.4251 0.1209 0.3507 0.043 Uiso 1 1 calc R . .
C30 C 0.5683(5) 0.1499(3) 0.4237(4) 0.0461(14) Uani 1 1 d . . .
H30A H 0.6143 0.1299 0.3882 0.055 Uiso 1 1 calc R . .
C31 C 0.6140(5) 0.1838(3) 0.4971(5) 0.0556(17) Uani 1 1 d . . .
H31A H 0.6910 0.1873 0.5117 0.067 Uiso 1 1 calc R . .
C32 C 0.5473(4) 0.2130(3) 0.5498(4) 0.0479(14) Uani 1 1 d . . .
H32A H 0.5784 0.2361 0.6006 0.057 Uiso 1 1 calc R . .
C33 C 0.4345(4) 0.2079(2) 0.5274(3) 0.0343(11) Uani 1 1 d . . .
H33A H 0.3891 0.2275 0.5636 0.041 Uiso 1 1 calc R . .
C34 C 0.2675(5) 0.4626(3) 0.6351(4) 0.0470(14) Uani 1 1 d . . .
H34C H 0.2939 0.4797 0.5841 0.056 Uiso 1 1 calc R . .
H34B H 0.3150 0.4789 0.6866 0.056 Uiso 1 1 calc R . .
H34A H 0.1930 0.4786 0.6353 0.056 Uiso 1 1 calc R . .
C35 C 0.4106(4) 0.3376(3) 0.6764(3) 0.0340(11) Uani 1 1 d . . .
H35C H 0.4092 0.2897 0.6914 0.041 Uiso 1 1 calc R . .
H35B H 0.4398 0.3639 0.7275 0.041 Uiso 1 1 calc R . .
H35A H 0.4570 0.3441 0.6325 0.041 Uiso 1 1 calc R . .
C36 C 0.1815(4) 0.3373(3) 0.7118(3) 0.0439(14) Uani 1 1 d . . .
H36C H 0.1733 0.2882 0.7077 0.053 Uiso 1 1 calc R . .
H36B H 0.1096 0.3586 0.6985 0.053 Uiso 1 1 calc R . .
H36A H 0.2156 0.3496 0.7700 0.053 Uiso 1 1 calc R . .
C37 C 0.1156(5) 0.0355(3) 0.6034(4) 0.0526(16) Uani 1 1 d . . .
H37C H 0.0843 0.0148 0.5486 0.063 Uiso 1 1 calc R . .
H37B H 0.0597 0.0624 0.6249 0.063 Uiso 1 1 calc R . .
H37A H 0.1417 0.0001 0.6449 0.063 Uiso 1 1 calc R . .
C38 C 0.2860(6) 0.1302(3) 0.6938(4) 0.0542(16) Uani 1 1 d . . .
H38C H 0.3548 0.1534 0.6907 0.065 Uiso 1 1 calc R . .
H38B H 0.2984 0.0949 0.7376 0.065 Uiso 1 1 calc R . .
H38A H 0.2328 0.1627 0.7089 0.065 Uiso 1 1 calc R . .
C39 C 0.3392(5) 0.0341(3) 0.5560(4) 0.0513(15) Uani 1 1 d . . .
H39C H 0.3166 0.0191 0.4968 0.062 Uiso 1 1 calc R . .
H39B H 0.3483 -0.0051 0.5942 0.062 Uiso 1 1 calc R . .
H39A H 0.4085 0.0585 0.5606 0.062 Uiso 1 1 calc R . .
N1 N 0.2155(3) 0.33235(19) 0.5364(2) 0.0225(8) Uani 1 1 d . . .
N2 N 0.1887(3) 0.15457(18) 0.5132(3) 0.0226(8) Uani 1 1 d . . .
Si1 Si 0.26894(11) 0.36673(6) 0.63387(8) 0.0267(3) Uani 1 1 d . . .
Si2 Si 0.23247(11) 0.09143(6) 0.58749(8) 0.0274(3) Uani 1 1 d . . .
P1 P 0.23608(10) 0.33103(5) 0.43812(7) 0.0191(2) Uani 1 1 d . . .
P2 P 0.23821(9) 0.17538(5) 0.42901(7) 0.0189(2) Uani 1 1 d . . .
Sm1 Sm 0.057188(18) 0.248290(9) 0.517652(14) 0.02030(13) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.038(3) 0.048(3) 0.047(3) -0.023(3) 0.009(3) -0.015(2)
C2 0.030(3) 0.027(3) 0.076(4) -0.004(3) 0.015(3) -0.007(2)
C3 0.028(3) 0.035(3) 0.051(3) 0.004(2) 0.016(3) -0.003(2)
C4 0.028(3) 0.049(4) 0.031(3) 0.006(2) 0.017(3) 0.0064(19)
C5 0.033(3) 0.037(3) 0.038(3) -0.004(2) 0.017(2) 0.008(2)
C6 0.033(3) 0.033(3) 0.046(3) 0.006(2) 0.012(3) 0.012(2)
C7 0.037(3) 0.045(3) 0.031(3) 0.007(2) 0.002(2) 0.014(2)
C8 0.035(3) 0.059(4) 0.032(3) -0.006(2) 0.001(3) 0.006(2)
C9 0.024(3) 0.017(2) 0.024(2) -0.0031(14) 0.012(2) -0.0012(14)
C10 0.025(2) 0.019(2) 0.030(2) 0.0055(17) 0.0065(19) -0.0014(17)
C11 0.041(3) 0.033(3) 0.032(3) 0.004(2) 0.006(2) 0.006(2)
C12 0.056(4) 0.052(3) 0.036(3) 0.018(3) 0.002(3) -0.005(3)
C13 0.044(3) 0.030(3) 0.071(4) 0.018(3) -0.002(3) 0.003(2)
C14 0.040(3) 0.027(2) 0.058(4) 0.001(2) 0.000(3) 0.007(2)
C15 0.036(3) 0.024(2) 0.043(3) 0.002(2) 0.008(2) 0.0038(19)
C16 0.025(2) 0.021(2) 0.021(2) 0.0046(16) 0.0102(18) -0.0034(16)
C17 0.031(2) 0.022(2) 0.017(2) 0.0026(15) 0.0035(18) -0.0037(16)
C18 0.030(2) 0.028(2) 0.036(3) 0.0010(19) 0.008(2) -0.0113(18)
C19 0.022(2) 0.039(3) 0.040(3) 0.002(2) 0.008(2) -0.006(2)
C20 0.030(3) 0.045(3) 0.042(3) -0.011(2) 0.022(2) -0.006(2)
C21 0.031(2) 0.030(2) 0.035(3) -0.0068(19) 0.015(2) -0.0103(19)
C22 0.024(2) 0.022(2) 0.027(2) -0.0058(17) 0.0068(19) -0.0022(16)
C23 0.044(3) 0.023(2) 0.034(3) -0.0034(19) 0.011(2) -0.006(2)
C24 0.052(3) 0.025(2) 0.051(3) -0.007(2) 0.007(3) -0.011(2)
C25 0.045(3) 0.033(3) 0.039(3) -0.020(2) 0.006(2) -0.007(2)
C26 0.029(2) 0.043(3) 0.031(3) -0.013(2) 0.009(2) -0.001(2)
C27 0.031(2) 0.030(2) 0.028(2) -0.0070(19) 0.012(2) -0.0062(19)
C28 0.023(2) 0.018(2) 0.036(2) -0.0008(18) 0.011(2) 0.0030(16)
C29 0.036(3) 0.033(3) 0.042(3) -0.001(2) 0.017(2) 0.010(2)
C30 0.033(3) 0.051(3) 0.057(4) 0.001(3) 0.018(3) 0.012(2)
C31 0.023(3) 0.062(4) 0.084(5) 0.010(4) 0.016(3) 0.011(3)
C32 0.030(3) 0.057(4) 0.056(4) -0.012(3) 0.004(3) -0.002(2)
C33 0.031(3) 0.032(2) 0.042(3) -0.001(2) 0.013(2) 0.003(2)
C34 0.053(3) 0.033(3) 0.057(4) -0.021(2) 0.016(3) -0.004(2)
C35 0.032(3) 0.044(3) 0.026(2) -0.001(2) 0.005(2) -0.008(2)
C36 0.034(3) 0.075(4) 0.023(2) -0.006(3) 0.006(2) -0.013(3)
C37 0.055(4) 0.043(3) 0.059(4) 0.027(3) 0.007(3) -0.008(3)
C38 0.092(5) 0.036(3) 0.032(3) 0.001(2) 0.001(3) -0.013(3)
C39 0.063(4) 0.037(3) 0.055(4) 0.014(3) 0.013(3) 0.027(3)
N1 0.028(2) 0.0194(17) 0.0222(18) -0.0025(14) 0.0107(16) -0.0020(15)
N2 0.0242(19) 0.0179(17) 0.028(2) 0.0005(14) 0.0115(16) 0.0006(14)
Si1 0.0306(7) 0.0288(6) 0.0230(6) -0.0070(5) 0.0113(5) -0.0061(5)
Si2 0.0351(7) 0.0197(6) 0.0272(6) 0.0029(5) 0.0049(6) 0.0010(5)
P1 0.0233(6) 0.0156(5) 0.0208(5) -0.0007(4) 0.0107(5) -0.0024(4)
P2 0.0200(6) 0.0158(5) 0.0229(6) -0.0032(4) 0.0093(5) 0.0003(4)
Sm1 0.0189(2) 0.02117(18) 0.02323(19) -0.00092(7) 0.01054(13) 0.00054(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.4287 2.2815 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C1 C2 134.7(5) . . ?
C8 C1 Sm1 73.3(4) . . ?
C2 C1 Sm1 75.3(3) . . ?
C1 C2 C3 134.0(5) . . ?
C1 C2 Sm1 73.5(3) . . ?
C3 C2 Sm1 74.1(3) . . ?
C4 C3 C2 134.8(6) . . ?
C4 C3 Sm1 75.6(3) . . ?
C2 C3 Sm1 74.9(3) . . ?
C3 C4 C5 135.0(6) . . ?
C3 C4 Sm1 74.0(3) . . ?
C5 C4 Sm1 75.1(3) . . ?
C4 C5 C6 135.8(5) . . ?
C4 C5 Sm1 74.5(3) . . ?
C6 C5 Sm1 75.0(3) . . ?
C5 C6 C7 134.3(5) . . ?
C5 C6 Sm1 74.6(3) . . ?
C7 C6 Sm1 73.4(3) . . ?
C8 C7 C6 134.1(5) . . ?
C8 C7 Sm1 72.7(3) . . ?
C6 C7 Sm1 75.9(3) . . ?
C1 C8 C7 137.2(6) . . ?
C1 C8 Sm1 76.2(4) . . ?
C7 C8 Sm1 76.6(4) . . ?
P1 C9 P2 124.0(3) . . ?
P1 C9 Sm1 87.15(18) . . ?
P2 C9 Sm1 86.90(18) . . ?
C11 C10 C15 119.9(4) . . ?
C11 C10 P1 120.9(4) . . ?
C15 C10 P1 119.3(4) . . ?
C12 C11 C10 119.6(5) . . ?
C11 C12 C13 121.5(5) . . ?
C14 C13 C12 118.9(5) . . ?
C13 C14 C15 120.9(5) . . ?
C10 C15 C14 119.1(5) . . ?
C21 C16 C17 118.9(4) . . ?
C21 C16 P1 119.4(3) . . ?
C17 C16 P1 121.6(3) . . ?
C16 C17 C18 120.4(4) . . ?
C19 C18 C17 120.0(4) . . ?
C20 C19 C18 120.0(4) . . ?
C19 C20 C21 120.4(4) . . ?
C16 C21 C20 120.2(4) . . ?
C27 C22 C23 119.1(4) . . ?
C27 C22 P2 121.1(3) . . ?
C23 C22 P2 119.9(3) . . ?
C24 C23 C22 119.8(5) . . ?
C25 C24 C23 121.0(5) . . ?
C24 C25 C26 119.4(4) . . ?
C25 C26 C27 120.2(5) . . ?
C22 C27 C26 120.5(4) . . ?
C33 C28 C29 118.5(4) . . ?
C33 C28 P2 116.4(3) . . ?
C29 C28 P2 125.1(4) . . ?
C30 C29 C28 120.0(5) . . ?
C31 C30 C29 120.7(5) . . ?
C30 C31 C32 120.1(5) . . ?
C33 C32 C31 119.4(6) . . ?
C32 C33 C28 121.3(5) . . ?
P1 N1 Si1 140.5(3) . . ?
P1 N1 Sm1 96.72(18) . . ?
Si1 N1 Sm1 122.71(18) . . ?
P2 N2 Si2 128.5(2) . . ?
P2 N2 Sm1 100.02(18) . . ?
Si2 N2 Sm1 130.80(19) . . ?
N1 Si1 C36 106.7(2) . . ?
N1 Si1 C35 113.8(2) . . ?
C36 Si1 C35 106.4(2) . . ?
N1 Si1 C34 113.8(2) . . ?
C36 Si1 C34 107.4(3) . . ?
C35 Si1 C34 108.3(3) . . ?
N2 Si2 C38 109.7(2) . . ?
N2 Si2 C39 114.4(2) . . ?
C38 Si2 C39 108.9(3) . . ?
N2 Si2 C37 110.5(2) . . ?
C38 Si2 C37 107.0(3) . . ?
C39 Si2 C37 105.9(3) . . ?
N1 P1 C9 108.2(2) . . ?
N1 P1 C10 113.0(2) . . ?
C9 P1 C10 104.9(2) . . ?
N1 P1 C16 114.8(2) . . ?
C9 P1 C16 113.5(2) . . ?
C10 P1 C16 101.98(19) . . ?
N1 P1 Sm1 53.01(14) . . ?
C9 P1 Sm1 59.74(17) . . ?
C10 P1 Sm1 104.72(14) . . ?
C16 P1 Sm1 153.29(14) . . ?
N2 P2 C9 109.5(2) . . ?
N2 P2 C22 114.4(2) . . ?
C9 P2 C22 104.5(2) . . ?
N2 P2 C28 109.8(2) . . ?
C9 P2 C28 112.0(2) . . ?
C22 P2 C28 106.5(2) . . ?
N2 P2 Sm1 50.15(13) . . ?
C9 P2 Sm1 59.64(16) . . ?
C22 P2 Sm1 120.81(14) . . ?
C28 P2 Sm1 132.70(15) . . ?
N2 Sm1 N1 89.60(13) . . ?
N2 Sm1 C8 114.09(15) . . ?
N1 Sm1 C8 128.09(16) . . ?
N2 Sm1 C1 93.90(16) . . ?
N1 Sm1 C1 155.81(16) . . ?
C8 Sm1 C1 30.54(19) . . ?
N2 Sm1 C7 142.30(15) . . ?
N1 Sm1 C7 106.26(16) . . ?
C8 Sm1 C7 30.61(17) . . ?
C1 Sm1 C7 58.3(2) . . ?
N2 Sm1 C3 99.46(15) . . ?
N1 Sm1 C3 143.43(15) . . ?
C8 Sm1 C3 80.1(2) . . ?
C1 Sm1 C3 59.35(19) . . ?
C7 Sm1 C3 87.91(18) . . ?
N2 Sm1 C2 87.98(16) . . ?
N1 Sm1 C2 172.95(17) . . ?
C8 Sm1 C2 58.8(2) . . ?
C1 Sm1 C2 31.1(2) . . ?
C7 Sm1 C2 79.54(19) . . ?
C3 Sm1 C2 31.07(19) . . ?
N2 Sm1 C4 123.34(14) . . ?
N1 Sm1 C4 118.07(15) . . ?
C8 Sm1 C4 87.5(2) . . ?
C1 Sm1 C4 79.50(19) . . ?
C7 Sm1 C4 79.37(18) . . ?
C3 Sm1 C4 30.40(15) . . ?
C2 Sm1 C4 58.42(19) . . ?
N2 Sm1 C5 152.94(15) . . ?
N1 Sm1 C5 100.59(15) . . ?
C8 Sm1 C5 79.07(18) . . ?
C1 Sm1 C5 86.98(18) . . ?
C7 Sm1 C5 58.36(17) . . ?
C3 Sm1 C5 58.0(2) . . ?
C2 Sm1 C5 78.87(18) . . ?
C4 Sm1 C5 30.40(15) . . ?
N2 Sm1 C6 172.46(16) . . ?
N1 Sm1 C6 95.92(17) . . ?
C8 Sm1 C6 58.40(18) . . ?
C1 Sm1 C6 78.98(19) . . ?
C7 Sm1 C6 30.73(18) . . ?
C3 Sm1 C6 79.11(17) . . ?
C2 Sm1 C6 87.1(2) . . ?
C4 Sm1 C6 58.13(17) . . ?
C5 Sm1 C6 30.40(17) . . ?
N2 Sm1 C9 63.16(13) . . ?
N1 Sm1 C9 61.47(13) . . ?
C8 Sm1 C9 88.01(19) . . ?
C1 Sm1 C9 99.04(16) . . ?
C7 Sm1 C9 94.28(16) . . ?
C3 Sm1 C9 152.71(15) . . ?
C2 Sm1 C9 122.83(17) . . ?
C4 Sm1 C9 173.30(15) . . ?
C5 Sm1 C9 143.40(15) . . ?
C6 Sm1 C9 115.20(16) . . ?
N2 Sm1 P1 82.47(9) . . ?
N1 Sm1 P1 30.28(8) . . ?
C8 Sm1 P1 104.68(15) . . ?
C1 Sm1 P1 126.70(13) . . ?
C7 Sm1 P1 94.22(13) . . ?
C3 Sm1 P1 173.68(13) . . ?
C2 Sm1 P1 155.24(15) . . ?
C4 Sm1 P1 144.40(11) . . ?
C5 Sm1 P1 118.32(12) . . ?
C6 Sm1 P1 99.75(12) . . ?
C9 Sm1 P1 33.11(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C8 1.376(8) . ?
C1 C2 1.418(9) . ?
C1 Sm1 2.630(5) . ?
C2 C3 1.419(9) . ?
C2 Sm1 2.654(5) . ?
C3 C4 1.392(7) . ?
C3 Sm1 2.644(5) . ?
C4 C5 1.398(7) . ?
C4 Sm1 2.664(6) . ?
C5 C6 1.401(8) . ?
C5 Sm1 2.670(5) . ?
C6 C7 1.409(8) . ?
C6 Sm1 2.675(5) . ?
C7 C8 1.383(8) . ?
C7 Sm1 2.643(5) . ?
C8 Sm1 2.594(7) . ?
C9 P1 1.723(4) . ?
C9 P2 1.741(4) . ?
C9 Sm1 2.724(5) . ?
C10 C11 1.376(7) . ?
C10 C15 1.384(6) . ?
C10 P1 1.815(5) . ?
C11 C12 1.365(8) . ?
C12 C13 1.372(9) . ?
C13 C14 1.360(8) . ?
C14 C15 1.391(7) . ?
C16 C21 1.380(6) . ?
C16 C17 1.385(6) . ?
C16 P1 1.822(4) . ?
C17 C18 1.389(6) . ?
C18 C19 1.369(7) . ?
C19 C20 1.369(7) . ?
C20 C21 1.387(6) . ?
C22 C27 1.379(6) . ?
C22 C23 1.385(6) . ?
C22 P2 1.805(4) . ?
C23 C24 1.379(7) . ?
C24 C25 1.370(8) . ?
C25 C26 1.374(7) . ?
C26 C27 1.382(6) . ?
C28 C33 1.385(7) . ?
C28 C29 1.391(6) . ?
C28 P2 1.807(5) . ?
C29 C30 1.378(7) . ?
C30 C31 1.368(9) . ?
C31 C32 1.380(8) . ?
C32 C33 1.378(7) . ?
C34 Si1 1.882(5) . ?
C35 Si1 1.852(5) . ?
C36 Si1 1.845(5) . ?
C37 Si2 1.858(5) . ?
C38 Si2 1.851(6) . ?
C39 Si2 1.855(5) . ?
N1 P1 1.599(4) . ?
N1 Si1 1.699(4) . ?
N1 Sm1 2.533(4) . ?
N2 P2 1.592(4) . ?
N2 Si2 1.724(4) . ?
N2 Sm1 2.458(4) . ?
P1 Sm1 3.1500(11) . ?
P2 Sm1 3.1525(11) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C1 C2 C3 -0.5(12) . . . . ?
Sm1 C1 C2 C3 46.9(7) . . . . ?
C8 C1 C2 Sm1 -47.4(7) . . . . ?
C1 C2 C3 C4 4.0(12) . . . . ?
Sm1 C2 C3 C4 50.8(7) . . . . ?
C1 C2 C3 Sm1 -46.8(7) . . . . ?
C2 C3 C4 C5 -2.4(13) . . . . ?
Sm1 C3 C4 C5 48.2(8) . . . . ?
C2 C3 C4 Sm1 -50.5(7) . . . . ?
C3 C4 C5 C6 0.1(14) . . . . ?
Sm1 C4 C5 C6 48.0(7) . . . . ?
C3 C4 C5 Sm1 -47.9(8) . . . . ?
C4 C5 C6 C7 -1.0(12) . . . . ?
Sm1 C5 C6 C7 46.8(7) . . . . ?
C4 C5 C6 Sm1 -47.9(7) . . . . ?
C5 C6 C7 C8 0.8(12) . . . . ?
Sm1 C6 C7 C8 48.0(7) . . . . ?
C5 C6 C7 Sm1 -47.2(7) . . . . ?
C2 C1 C8 C7 -4.0(15) . . . . ?
Sm1 C1 C8 C7 -52.1(9) . . . . ?
C2 C1 C8 Sm1 48.1(7) . . . . ?
C6 C7 C8 C1 2.9(14) . . . . ?
Sm1 C7 C8 C1 51.9(9) . . . . ?
C6 C7 C8 Sm1 -49.0(7) . . . . ?
C15 C10 C11 C12 -0.9(8) . . . . ?
P1 C10 C11 C12 179.5(4) . . . . ?
C10 C11 C12 C13 -0.6(9) . . . . ?
C11 C12 C13 C14 2.1(9) . . . . ?
C12 C13 C14 C15 -2.0(8) . . . . ?
C11 C10 C15 C14 1.0(7) . . . . ?
P1 C10 C15 C14 -179.4(4) . . . . ?
C13 C14 C15 C10 0.5(8) . . . . ?
C21 C16 C17 C18 -2.8(6) . . . . ?
P1 C16 C17 C18 179.3(3) . . . . ?
C16 C17 C18 C19 1.0(7) . . . . ?
C17 C18 C19 C20 1.1(8) . . . . ?
C18 C19 C20 C21 -1.2(8) . . . . ?
C17 C16 C21 C20 2.6(7) . . . . ?
P1 C16 C21 C20 -179.4(4) . . . . ?
C19 C20 C21 C16 -0.6(8) . . . . ?
C27 C22 C23 C24 2.4(7) . . . . ?
P2 C22 C23 C24 -178.3(4) . . . . ?
C22 C23 C24 C25 -1.6(8) . . . . ?
C23 C24 C25 C26 -0.1(9) . . . . ?
C24 C25 C26 C27 0.9(8) . . . . ?
C23 C22 C27 C26 -1.6(7) . . . . ?
P2 C22 C27 C26 179.1(4) . . . . ?
C25 C26 C27 C22 0.0(7) . . . . ?
C33 C28 C29 C30 -1.3(7) . . . . ?
P2 C28 C29 C30 177.0(4) . . . . ?
C28 C29 C30 C31 0.5(9) . . . . ?
C29 C30 C31 C32 0.4(10) . . . . ?
C30 C31 C32 C33 -0.4(10) . . . . ?
C31 C32 C33 C28 -0.5(9) . . . . ?
C29 C28 C33 C32 1.3(8) . . . . ?
P2 C28 C33 C32 -177.1(4) . . . . ?
P1 N1 Si1 C36 179.3(4) . . . . ?
Sm1 N1 Si1 C36 -5.4(3) . . . . ?
P1 N1 Si1 C35 -63.7(4) . . . . ?
Sm1 N1 Si1 C35 111.6(2) . . . . ?
P1 N1 Si1 C34 61.1(5) . . . . ?
Sm1 N1 Si1 C34 -123.6(3) . . . . ?
P2 N2 Si2 C38 114.1(4) . . . . ?
Sm1 N2 Si2 C38 -54.5(4) . . . . ?
P2 N2 Si2 C39 -8.7(4) . . . . ?
Sm1 N2 Si2 C39 -177.2(3) . . . . ?
P2 N2 Si2 C37 -128.2(3) . . . . ?
Sm1 N2 Si2 C37 63.3(4) . . . . ?
Si1 N1 P1 C9 151.8(4) . . . . ?
Sm1 N1 P1 C9 -24.2(2) . . . . ?
Si1 N1 P1 C10 -92.5(4) . . . . ?
Sm1 N1 P1 C10 91.5(2) . . . . ?
Si1 N1 P1 C16 23.9(5) . . . . ?
Sm1 N1 P1 C16 -152.15(16) . . . . ?
Si1 N1 P1 Sm1 176.1(5) . . . . ?
P2 C9 P1 N1 -62.0(4) . . . . ?
Sm1 C9 P1 N1 22.3(2) . . . . ?
P2 C9 P1 C10 177.1(3) . . . . ?
Sm1 C9 P1 C10 -98.56(18) . . . . ?
P2 C9 P1 C16 66.6(4) . . . . ?
Sm1 C9 P1 C16 150.93(16) . . . . ?
P2 C9 P1 Sm1 -84.3(3) . . . . ?
C11 C10 P1 N1 -173.3(4) . . . . ?
C15 C10 P1 N1 7.1(4) . . . . ?
C11 C10 P1 C9 -55.6(4) . . . . ?
C15 C10 P1 C9 124.7(4) . . . . ?
C11 C10 P1 C16 63.0(4) . . . . ?
C15 C10 P1 C16 -116.7(4) . . . . ?
C11 C10 P1 Sm1 -117.7(4) . . . . ?
C15 C10 P1 Sm1 62.7(4) . . . . ?
C21 C16 P1 N1 144.7(4) . . . . ?
C17 C16 P1 N1 -37.4(4) . . . . ?
C21 C16 P1 C9 19.5(5) . . . . ?
C17 C16 P1 C9 -162.6(4) . . . . ?
C21 C16 P1 C10 -92.8(4) . . . . ?
C17 C16 P1 C10 85.1(4) . . . . ?
C21 C16 P1 Sm1 88.5(5) . . . . ?
C17 C16 P1 Sm1 -93.6(4) . . . . ?
Si2 N2 P2 C9 -164.9(3) . . . . ?
Sm1 N2 P2 C9 6.3(3) . . . . ?
Si2 N2 P2 C22 78.1(3) . . . . ?
Sm1 N2 P2 C22 -110.69(19) . . . . ?
Si2 N2 P2 C28 -41.6(4) . . . . ?
Sm1 N2 P2 C28 129.68(18) . . . . ?
Si2 N2 P2 Sm1 -171.2(4) . . . . ?
P1 C9 P2 N2 78.9(4) . . . . ?
Sm1 C9 P2 N2 -5.6(2) . . . . ?
P1 C9 P2 C22 -158.1(3) . . . . ?
Sm1 C9 P2 C22 117.47(17) . . . . ?
P1 C9 P2 C28 -43.2(4) . . . . ?
Sm1 C9 P2 C28 -127.65(18) . . . . ?
P1 C9 P2 Sm1 84.5(3) . . . . ?
C27 C22 P2 N2 171.4(4) . . . . ?
C23 C22 P2 N2 -7.9(5) . . . . ?
C27 C22 P2 C9 51.6(4) . . . . ?
C23 C22 P2 C9 -127.7(4) . . . . ?
C27 C22 P2 C28 -67.1(4) . . . . ?
C23 C22 P2 C28 113.6(4) . . . . ?
C27 C22 P2 Sm1 114.6(4) . . . . ?
C23 C22 P2 Sm1 -64.7(4) . . . . ?
C33 C28 P2 N2 -48.2(4) . . . . ?
C29 C28 P2 N2 133.4(4) . . . . ?
C33 C28 P2 C9 73.7(4) . . . . ?
C29 C28 P2 C9 -104.7(4) . . . . ?
C33 C28 P2 C22 -172.6(4) . . . . ?
C29 C28 P2 C22 9.0(5) . . . . ?
C33 C28 P2 Sm1 5.3(5) . . . . ?
C29 C28 P2 Sm1 -173.0(3) . . . . ?
P2 N2 Sm1 N1 -62.11(18) . . . . ?
Si2 N2 Sm1 N1 108.8(3) . . . . ?
P2 N2 Sm1 C8 70.2(2) . . . . ?
Si2 N2 Sm1 C8 -118.9(3) . . . . ?
P2 N2 Sm1 C1 93.9(2) . . . . ?
Si2 N2 Sm1 C1 -95.1(3) . . . . ?
P2 N2 Sm1 C7 54.6(3) . . . . ?
Si2 N2 Sm1 C7 -134.5(3) . . . . ?
P2 N2 Sm1 C3 153.5(2) . . . . ?
Si2 N2 Sm1 C3 -35.6(3) . . . . ?
P2 N2 Sm1 C2 124.5(2) . . . . ?
Si2 N2 Sm1 C2 -64.6(3) . . . . ?
P2 N2 Sm1 C4 173.9(2) . . . . ?
Si2 N2 Sm1 C4 -15.1(4) . . . . ?
P2 N2 Sm1 C5 -175.1(3) . . . . ?
Si2 N2 Sm1 C5 -4.2(5) . . . . ?
P2 N2 Sm1 C6 75.0(10) . . . . ?
Si2 N2 Sm1 C6 -114.0(10) . . . . ?
P2 N2 Sm1 C9 -4.24(17) . . . . ?
Si2 N2 Sm1 C9 166.7(3) . . . . ?
P2 N2 Sm1 P1 -32.59(15) . . . . ?
Si2 N2 Sm1 P1 138.3(3) . . . . ?
P1 N1 Sm1 N2 75.64(17) . . . . ?
Si1 N1 Sm1 N2 -101.4(2) . . . . ?
P1 N1 Sm1 C8 -45.2(3) . . . . ?
Si1 N1 Sm1 C8 137.7(2) . . . . ?
P1 N1 Sm1 C1 -23.0(5) . . . . ?
Si1 N1 Sm1 C1 160.0(3) . . . . ?
P1 N1 Sm1 C7 -69.7(2) . . . . ?
Si1 N1 Sm1 C7 113.3(2) . . . . ?
P1 N1 Sm1 C3 -178.9(2) . . . . ?
Si1 N1 Sm1 C3 4.1(4) . . . . ?
P1 N1 Sm1 C2 145.5(10) . . . . ?
Si1 N1 Sm1 C2 -31.5(12) . . . . ?
P1 N1 Sm1 C4 -156.11(18) . . . . ?
Si1 N1 Sm1 C4 26.9(3) . . . . ?
P1 N1 Sm1 C5 -129.58(19) . . . . ?
Si1 N1 Sm1 C5 53.4(3) . . . . ?
P1 N1 Sm1 C6 -99.2(2) . . . . ?
Si1 N1 Sm1 C6 83.8(2) . . . . ?
P1 N1 Sm1 C9 16.31(16) . . . . ?
Si1 N1 Sm1 C9 -160.7(3) . . . . ?
Si1 N1 Sm1 P1 -177.0(4) . . . . ?
C1 C8 Sm1 N2 52.3(4) . . . . ?
C7 C8 Sm1 N2 -161.2(3) . . . . ?
C1 C8 Sm1 N1 162.2(3) . . . . ?
C7 C8 Sm1 N1 -51.2(4) . . . . ?
C7 C8 Sm1 C1 146.5(6) . . . . ?
C1 C8 Sm1 C7 -146.5(6) . . . . ?
C1 C8 Sm1 C3 -43.7(4) . . . . ?
C7 C8 Sm1 C3 102.8(4) . . . . ?
C1 C8 Sm1 C2 -19.3(3) . . . . ?
C7 C8 Sm1 C2 127.2(4) . . . . ?
C1 C8 Sm1 C4 -73.4(4) . . . . ?
C7 C8 Sm1 C4 73.2(4) . . . . ?
C1 C8 Sm1 C5 -102.8(4) . . . . ?
C7 C8 Sm1 C5 43.7(4) . . . . ?
C1 C8 Sm1 C6 -126.9(4) . . . . ?
C7 C8 Sm1 C6 19.6(3) . . . . ?
C1 C8 Sm1 C9 111.6(4) . . . . ?
C7 C8 Sm1 C9 -101.8(4) . . . . ?
C1 C8 Sm1 P1 140.5(3) . . . . ?
C7 C8 Sm1 P1 -72.9(4) . . . . ?
C8 C1 Sm1 N2 -133.6(4) . . . . ?
C2 C1 Sm1 N2 79.6(3) . . . . ?
C8 C1 Sm1 N1 -35.9(6) . . . . ?
C2 C1 Sm1 N1 177.3(3) . . . . ?
C2 C1 Sm1 C8 -146.8(5) . . . . ?
C8 C1 Sm1 C7 19.3(4) . . . . ?
C2 C1 Sm1 C7 -127.6(4) . . . . ?
C8 C1 Sm1 C3 127.7(4) . . . . ?
C2 C1 Sm1 C3 -19.1(3) . . . . ?
C8 C1 Sm1 C2 146.8(5) . . . . ?
C8 C1 Sm1 C4 103.2(4) . . . . ?
C2 C1 Sm1 C4 -43.7(3) . . . . ?
C8 C1 Sm1 C5 73.5(4) . . . . ?
C2 C1 Sm1 C5 -73.4(3) . . . . ?
C8 C1 Sm1 C6 43.9(4) . . . . ?
C2 C1 Sm1 C6 -102.9(4) . . . . ?
C8 C1 Sm1 C9 -70.2(4) . . . . ?
C2 C1 Sm1 C9 143.0(3) . . . . ?
C8 C1 Sm1 P1 -50.1(4) . . . . ?
C2 C1 Sm1 P1 163.1(3) . . . . ?
C8 C7 Sm1 N2 28.8(5) . . . . ?
C6 C7 Sm1 N2 174.8(3) . . . . ?
C8 C7 Sm1 N1 140.3(4) . . . . ?
C6 C7 Sm1 N1 -73.7(4) . . . . ?
C6 C7 Sm1 C8 146.0(6) . . . . ?
C8 C7 Sm1 C1 -19.2(4) . . . . ?
C6 C7 Sm1 C1 126.8(4) . . . . ?
C8 C7 Sm1 C3 -74.0(4) . . . . ?
C6 C7 Sm1 C3 72.0(3) . . . . ?
C8 C7 Sm1 C2 -43.8(4) . . . . ?
C6 C7 Sm1 C2 102.2(4) . . . . ?
C8 C7 Sm1 C4 -103.4(4) . . . . ?
C6 C7 Sm1 C4 42.6(3) . . . . ?
C8 C7 Sm1 C5 -127.1(4) . . . . ?
C6 C7 Sm1 C5 18.9(3) . . . . ?
C8 C7 Sm1 C6 -146.0(6) . . . . ?
C8 C7 Sm1 C9 78.8(4) . . . . ?
C6 C7 Sm1 C9 -135.2(3) . . . . ?
C8 C7 Sm1 P1 112.0(4) . . . . ?
C6 C7 Sm1 P1 -102.0(3) . . . . ?
C4 C3 Sm1 N2 144.8(4) . . . . ?
C2 C3 Sm1 N2 -69.8(4) . . . . ?
C4 C3 Sm1 N1 42.5(5) . . . . ?
C2 C3 Sm1 N1 -172.0(3) . . . . ?
C4 C3 Sm1 C8 -102.2(4) . . . . ?
C2 C3 Sm1 C8 43.3(3) . . . . ?
C4 C3 Sm1 C1 -126.3(4) . . . . ?
C2 C3 Sm1 C1 19.2(3) . . . . ?
C4 C3 Sm1 C7 -72.4(4) . . . . ?
C2 C3 Sm1 C7 73.1(4) . . . . ?
C4 C3 Sm1 C2 -145.4(6) . . . . ?
C2 C3 Sm1 C4 145.4(6) . . . . ?
C4 C3 Sm1 C5 -19.0(4) . . . . ?
C2 C3 Sm1 C5 126.5(4) . . . . ?
C4 C3 Sm1 C6 -42.7(4) . . . . ?
C2 C3 Sm1 C6 102.7(4) . . . . ?
C4 C3 Sm1 C9 -167.7(3) . . . . ?
C2 C3 Sm1 C9 -22.2(6) . . . . ?
C4 C3 Sm1 P1 37.5(13) . . . . ?
C2 C3 Sm1 P1 -177.1(9) . . . . ?
C1 C2 Sm1 N2 -101.0(3) . . . . ?
C3 C2 Sm1 N2 112.2(3) . . . . ?
C1 C2 Sm1 N1 -170.9(10) . . . . ?
C3 C2 Sm1 N1 42.2(12) . . . . ?
C1 C2 Sm1 C8 19.0(3) . . . . ?
C3 C2 Sm1 C8 -127.9(4) . . . . ?
C3 C2 Sm1 C1 -146.9(5) . . . . ?
C1 C2 Sm1 C7 43.3(3) . . . . ?
C3 C2 Sm1 C7 -103.6(4) . . . . ?
C1 C2 Sm1 C3 146.9(5) . . . . ?
C1 C2 Sm1 C4 127.2(4) . . . . ?
C3 C2 Sm1 C4 -19.7(3) . . . . ?
C1 C2 Sm1 C5 102.8(4) . . . . ?
C3 C2 Sm1 C5 -44.1(3) . . . . ?
C1 C2 Sm1 C6 73.3(4) . . . . ?
C3 C2 Sm1 C6 -73.6(4) . . . . ?
C1 C2 Sm1 C9 -45.0(4) . . . . ?
C3 C2 Sm1 C9 168.1(3) . . . . ?
C1 C2 Sm1 P1 -33.9(5) . . . . ?
C3 C2 Sm1 P1 179.2(2) . . . . ?
C3 C4 Sm1 N2 -42.9(4) . . . . ?
C5 C4 Sm1 N2 170.1(3) . . . . ?
C3 C4 Sm1 N1 -152.9(3) . . . . ?
C5 C4 Sm1 N1 60.2(4) . . . . ?
C3 C4 Sm1 C8 74.5(4) . . . . ?
C5 C4 Sm1 C8 -72.4(4) . . . . ?
C3 C4 Sm1 C1 44.9(4) . . . . ?
C5 C4 Sm1 C1 -102.1(4) . . . . ?
C3 C4 Sm1 C7 104.3(4) . . . . ?
C5 C4 Sm1 C7 -42.7(4) . . . . ?
C5 C4 Sm1 C3 -147.0(7) . . . . ?
C3 C4 Sm1 C2 20.1(4) . . . . ?
C5 C4 Sm1 C2 -126.9(5) . . . . ?
C3 C4 Sm1 C5 147.0(7) . . . . ?
C3 C4 Sm1 C6 128.3(5) . . . . ?
C5 C4 Sm1 C6 -18.6(4) . . . . ?
C3 C4 Sm1 C9 122.9(12) . . . . ?
C5 C4 Sm1 C9 -24.1(15) . . . . ?
C3 C4 Sm1 P1 -173.4(3) . . . . ?
C5 C4 Sm1 P1 39.6(5) . . . . ?
C4 C5 Sm1 N2 -18.3(6) . . . . ?
C6 C5 Sm1 N2 -165.9(3) . . . . ?
C4 C5 Sm1 N1 -128.9(4) . . . . ?
C6 C5 Sm1 N1 83.6(4) . . . . ?
C4 C5 Sm1 C8 104.0(4) . . . . ?
C6 C5 Sm1 C8 -43.5(4) . . . . ?
C4 C5 Sm1 C1 74.3(4) . . . . ?
C6 C5 Sm1 C1 -73.2(4) . . . . ?
C4 C5 Sm1 C7 128.5(4) . . . . ?
C6 C5 Sm1 C7 -19.1(3) . . . . ?
C4 C5 Sm1 C3 19.0(4) . . . . ?
C6 C5 Sm1 C3 -128.6(4) . . . . ?
C4 C5 Sm1 C2 44.0(4) . . . . ?
C6 C5 Sm1 C2 -103.6(4) . . . . ?
C6 C5 Sm1 C4 -147.5(6) . . . . ?
C4 C5 Sm1 C6 147.5(6) . . . . ?
C4 C5 Sm1 C9 175.4(3) . . . . ?
C6 C5 Sm1 C9 27.9(5) . . . . ?
C4 C5 Sm1 P1 -155.1(3) . . . . ?
C6 C5 Sm1 P1 57.4(4) . . . . ?
C5 C6 Sm1 N2 122.3(10) . . . . ?
C7 C6 Sm1 N2 -24.7(12) . . . . ?
C5 C6 Sm1 N1 -100.9(3) . . . . ?
C7 C6 Sm1 N1 112.1(3) . . . . ?
C5 C6 Sm1 C8 127.5(4) . . . . ?
C7 C6 Sm1 C8 -19.5(3) . . . . ?
C5 C6 Sm1 C1 103.1(4) . . . . ?
C7 C6 Sm1 C1 -44.0(3) . . . . ?
C5 C6 Sm1 C7 147.0(5) . . . . ?
C5 C6 Sm1 C3 42.5(3) . . . . ?
C7 C6 Sm1 C3 -104.5(4) . . . . ?
C5 C6 Sm1 C2 72.8(4) . . . . ?
C7 C6 Sm1 C2 -74.3(4) . . . . ?
C5 C6 Sm1 C4 18.6(3) . . . . ?
C7 C6 Sm1 C4 -128.4(4) . . . . ?
C7 C6 Sm1 C5 -147.0(5) . . . . ?
C5 C6 Sm1 C9 -162.0(3) . . . . ?
C7 C6 Sm1 C9 50.9(4) . . . . ?
C5 C6 Sm1 P1 -131.2(3) . . . . ?
C7 C6 Sm1 P1 81.8(3) . . . . ?
P1 C9 Sm1 N2 -120.5(2) . . . . ?
P2 C9 Sm1 N2 3.82(16) . . . . ?
P1 C9 Sm1 N1 -15.02(16) . . . . ?
P2 C9 Sm1 N1 109.3(2) . . . . ?
P1 C9 Sm1 C8 121.2(2) . . . . ?
P2 C9 Sm1 C8 -114.6(2) . . . . ?
P1 C9 Sm1 C1 149.7(2) . . . . ?
P2 C9 Sm1 C1 -86.0(2) . . . . ?
P1 C9 Sm1 C7 91.2(2) . . . . ?
P2 C9 Sm1 C7 -144.5(2) . . . . ?
P1 C9 Sm1 C3 -175.1(3) . . . . ?
P2 C9 Sm1 C3 -50.8(5) . . . . ?
P1 C9 Sm1 C2 171.5(2) . . . . ?
P2 C9 Sm1 C2 -64.2(3) . . . . ?
P1 C9 Sm1 C4 72.8(13) . . . . ?
P2 C9 Sm1 C4 -162.9(12) . . . . ?
P1 C9 Sm1 C5 52.6(4) . . . . ?
P2 C9 Sm1 C5 176.8(2) . . . . ?
P1 C9 Sm1 C6 67.7(3) . . . . ?
P2 C9 Sm1 C6 -167.99(19) . . . . ?
P2 C9 Sm1 P1 124.3(3) . . . . ?
N1 P1 Sm1 N2 -102.27(19) . . . . ?
C9 P1 Sm1 N2 50.9(2) . . . . ?
C10 P1 Sm1 N2 149.82(18) . . . . ?
C16 P1 Sm1 N2 -31.6(3) . . . . ?
C9 P1 Sm1 N1 153.2(3) . . . . ?
C10 P1 Sm1 N1 -107.9(2) . . . . ?
C16 P1 Sm1 N1 70.7(4) . . . . ?
N1 P1 Sm1 C8 144.7(2) . . . . ?
C9 P1 Sm1 C8 -62.1(2) . . . . ?
C10 P1 Sm1 C8 36.8(2) . . . . ?
C16 P1 Sm1 C8 -144.6(3) . . . . ?
N1 P1 Sm1 C1 168.5(2) . . . . ?
C9 P1 Sm1 C1 -38.4(3) . . . . ?
C10 P1 Sm1 C1 60.6(2) . . . . ?
C16 P1 Sm1 C1 -120.8(4) . . . . ?
N1 P1 Sm1 C7 115.5(2) . . . . ?
C9 P1 Sm1 C7 -91.4(2) . . . . ?
C10 P1 Sm1 C7 7.6(2) . . . . ?
C16 P1 Sm1 C7 -173.8(3) . . . . ?
N1 P1 Sm1 C3 5.9(11) . . . . ?
C9 P1 Sm1 C3 159.1(11) . . . . ?
C10 P1 Sm1 C3 -102.0(11) . . . . ?
C16 P1 Sm1 C3 76.7(12) . . . . ?
N1 P1 Sm1 C2 -170.4(3) . . . . ?
C9 P1 Sm1 C2 -17.3(4) . . . . ?
C10 P1 Sm1 C2 81.6(4) . . . . ?
C16 P1 Sm1 C2 -99.7(5) . . . . ?
N1 P1 Sm1 C4 37.9(3) . . . . ?
C9 P1 Sm1 C4 -169.0(3) . . . . ?
C10 P1 Sm1 C4 -70.0(3) . . . . ?
C16 P1 Sm1 C4 108.6(4) . . . . ?
N1 P1 Sm1 C5 59.4(2) . . . . ?
C9 P1 Sm1 C5 -147.5(3) . . . . ?
C10 P1 Sm1 C5 -48.5(2) . . . . ?
C16 P1 Sm1 C5 130.1(3) . . . . ?
N1 P1 Sm1 C6 85.0(2) . . . . ?
C9 P1 Sm1 C6 -121.8(3) . . . . ?
C10 P1 Sm1 C6 -22.9(2) . . . . ?
C16 P1 Sm1 C6 155.7(3) . . . . ?
N1 P1 Sm1 C9 -153.2(3) . . . . ?
C10 P1 Sm1 C9 98.9(3) . . . . ?
C16 P1 Sm1 C9 -82.4(4) . . . . ?
|
1100884.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-27 05:05:50 +0300 (Sun, 27 Mar 2016) $
#$Revision: 180535 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100884.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100884
loop_
_publ_author_name
'Panda, Tarun K.'
'Zulys, Agustino'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
Bis(phosphinimino)methanides: Synthesis, Structure, and
Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2197
_journal_page_last 2202
_journal_paper_doi 10.1021/om0491138
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C41.5 H52 Er N2 P2 Si2'
_chemical_formula_weight 864.23
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 93.345(4)
_cell_angle_beta 92.875(4)
_cell_angle_gamma 98.921(4)
_cell_formula_units_Z 2
_cell_length_a 9.3791(17)
_cell_length_b 9.4895(17)
_cell_length_c 22.693(4)
_cell_measurement_temperature 173(2)
_cell_volume 1988.3(6)
_computing_molecular_graphics 'Diamond 2.1'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type 'Bruker Smart 1000 CCD'
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0189
_diffrn_reflns_av_sigmaI/netI 0.0301
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 24365
_diffrn_reflns_theta_full 30.52
_diffrn_reflns_theta_max 30.52
_diffrn_reflns_theta_min 0.90
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.282
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.746431
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.444
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 882
_exptl_crystal_size_max .4
_exptl_crystal_size_mid .36
_exptl_crystal_size_min 0.09
_refine_diff_density_max 1.252
_refine_diff_density_min -0.901
_refine_diff_density_rms 0.098
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 11911
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.065
_refine_ls_R_factor_all 0.0330
_refine_ls_R_factor_gt 0.0262
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+1.4800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0607
_refine_ls_wR_factor_ref 0.0653
_reflns_number_gt 10569
_reflns_number_total 11911
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060419
_cod_data_source_file om0491138si20041116_113831.cif
_cod_data_source_block 1c
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C41.50 H52 Er N2 P2 Si2'
_cod_database_code 1100884
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er Er 0.537141(11) 0.779060(11) 0.743660(4) 0.01756(3) Uani 1 1 d . . .
P1 P 0.77123(6) 0.88363(6) 0.65945(2) 0.01652(10) Uani 1 1 d . . .
P2 P 0.82992(6) 0.95321(6) 0.79434(2) 0.01636(10) Uani 1 1 d . . .
Si1 Si 0.51069(8) 1.04487(8) 0.63908(3) 0.02373(13) Uani 1 1 d . . .
Si2 Si 0.61555(7) 1.03524(8) 0.87702(3) 0.02207(13) Uani 1 1 d . . .
N1 N 0.6118(2) 0.9205(2) 0.66341(8) 0.0192(4) Uani 1 1 d . . .
N2 N 0.6659(2) 0.9586(2) 0.81129(8) 0.0175(3) Uani 1 1 d . . .
C1 C 0.5262(3) 0.5092(3) 0.72361(14) 0.0349(6) Uani 1 1 d . . .
H1 H 0.5958 0.4531 0.7107 0.042 Uiso 1 1 calc R . .
C2 C 0.4413(3) 0.5483(3) 0.67633(13) 0.0367(6) Uani 1 1 d . . .
H2 H 0.4610 0.5056 0.6393 0.044 Uiso 1 1 calc R . .
C3 C 0.3345(3) 0.6356(3) 0.67104(13) 0.0376(7) Uani 1 1 d . . .
H3 H 0.2978 0.6367 0.6313 0.045 Uiso 1 1 calc R . .
C4 C 0.2684(3) 0.7218(3) 0.71021(16) 0.0394(7) Uani 1 1 d . . .
H4 H 0.2056 0.7755 0.6904 0.047 Uiso 1 1 calc R . .
C5 C 0.2739(3) 0.7471(3) 0.77201(16) 0.0409(7) Uani 1 1 d . . .
H5 H 0.2127 0.8126 0.7846 0.049 Uiso 1 1 calc R . .
C6 C 0.3497(3) 0.6968(3) 0.81928(14) 0.0405(7) Uani 1 1 d . . .
H6 H 0.3222 0.7310 0.8565 0.049 Uiso 1 1 calc R . .
C7 C 0.4558(4) 0.6089(3) 0.82524(13) 0.0415(7) Uani 1 1 d . . .
H7 H 0.4824 0.5972 0.8654 0.050 Uiso 1 1 calc R . .
C8 C 0.5325(3) 0.5334(3) 0.78535(14) 0.0382(7) Uani 1 1 d . . .
H8 H 0.6044 0.4892 0.8047 0.046 Uiso 1 1 calc R . .
C9 C 0.8277(2) 0.8429(2) 0.72967(9) 0.0176(4) Uani 1 1 d . . .
H9 H 0.8842 0.7620 0.7318 0.021 Uiso 1 1 calc R . .
C10 C 0.7803(3) 0.7237(2) 0.61244(10) 0.0209(4) Uani 1 1 d . . .
C11 C 0.8972(3) 0.6503(3) 0.61839(12) 0.0318(6) Uani 1 1 d . . .
H11 H 0.9704 0.6808 0.6489 0.038 Uiso 1 1 calc R . .
C12 C 0.9082(4) 0.5332(3) 0.58029(14) 0.0420(7) Uani 1 1 d . . .
H12 H 0.9878 0.4832 0.5851 0.050 Uiso 1 1 calc R . .
C13 C 0.8043(4) 0.4899(3) 0.53575(14) 0.0413(7) Uani 1 1 d . . .
H13 H 0.8120 0.4098 0.5096 0.050 Uiso 1 1 calc R . .
C14 C 0.6889(3) 0.5614(4) 0.52855(13) 0.0417(7) Uani 1 1 d . . .
H14 H 0.6180 0.5314 0.4971 0.050 Uiso 1 1 calc R . .
C15 C 0.6751(3) 0.6777(3) 0.56700(11) 0.0313(6) Uani 1 1 d . . .
H15 H 0.5939 0.7257 0.5622 0.038 Uiso 1 1 calc R . .
C16 C 0.8889(2) 1.0140(2) 0.62113(10) 0.0201(4) Uani 1 1 d . . .
C17 C 0.8509(3) 1.0322(3) 0.56177(11) 0.0286(5) Uani 1 1 d . . .
H17 H 0.7666 0.9760 0.5428 0.034 Uiso 1 1 calc R . .
C18 C 0.9354(3) 1.1315(3) 0.53062(12) 0.0337(6) Uani 1 1 d . . .
H18 H 0.9087 1.1435 0.4905 0.040 Uiso 1 1 calc R . .
C19 C 1.0577(3) 1.2126(3) 0.55774(13) 0.0338(6) Uani 1 1 d . . .
H19 H 1.1150 1.2814 0.5364 0.041 Uiso 1 1 calc R . .
C20 C 1.0978(3) 1.1948(3) 0.61568(14) 0.0357(6) Uani 1 1 d . . .
H20 H 1.1824 1.2513 0.6342 0.043 Uiso 1 1 calc R . .
C21 C 1.0144(3) 1.0941(3) 0.64724(11) 0.0278(5) Uani 1 1 d . . .
H21 H 1.0439 1.0803 0.6869 0.033 Uiso 1 1 calc R . .
C22 C 0.9301(2) 0.8706(3) 0.85001(10) 0.0208(4) Uani 1 1 d . . .
C23 C 0.9138(3) 0.7223(3) 0.84862(11) 0.0277(5) Uani 1 1 d . . .
H23 H 0.8597 0.6669 0.8165 0.033 Uiso 1 1 calc R . .
C24 C 0.9754(3) 0.6541(3) 0.89354(13) 0.0373(6) Uani 1 1 d . . .
H24 H 0.9642 0.5527 0.8917 0.045 Uiso 1 1 calc R . .
C25 C 1.0532(3) 0.7337(4) 0.94099(12) 0.0407(7) Uani 1 1 d . . .
H25 H 1.0948 0.6870 0.9719 0.049 Uiso 1 1 calc R . .
C26 C 1.0702(3) 0.8808(4) 0.94330(12) 0.0392(7) Uani 1 1 d . . .
H26 H 1.1236 0.9355 0.9758 0.047 Uiso 1 1 calc R . .
C27 C 1.0090(3) 0.9496(3) 0.89796(11) 0.0295(5) Uani 1 1 d . . .
H27 H 1.0213 1.0511 0.8998 0.035 Uiso 1 1 calc R . .
C28 C 0.9247(2) 1.1321(2) 0.78746(11) 0.0221(4) Uani 1 1 d . . .
C29 C 1.0758(3) 1.1691(3) 0.79592(12) 0.0291(5) Uani 1 1 d . . .
H29 H 1.1319 1.1015 0.8100 0.035 Uiso 1 1 calc R . .
C30 C 1.1427(3) 1.3040(3) 0.78369(14) 0.0376(6) Uani 1 1 d . . .
H30 H 1.2446 1.3289 0.7902 0.045 Uiso 1 1 calc R . .
C31 C 1.0634(3) 1.4021(3) 0.76227(16) 0.0426(7) Uani 1 1 d . . .
H31 H 1.1104 1.4940 0.7537 0.051 Uiso 1 1 calc R . .
C32 C 0.9136(3) 1.3662(3) 0.75318(15) 0.0371(6) Uani 1 1 d . . .
H32 H 0.8585 1.4335 0.7381 0.045 Uiso 1 1 calc R . .
C33 C 0.8451(3) 1.2322(3) 0.76609(12) 0.0273(5) Uani 1 1 d . . .
H33 H 0.7430 1.2086 0.7603 0.033 Uiso 1 1 calc R . .
C34 C 0.3778(4) 0.9632(4) 0.57772(12) 0.0423(7) Uani 1 1 d . . .
H34A H 0.4298 0.9338 0.5439 0.064 Uiso 1 1 calc R . .
H34B H 0.3175 1.0335 0.5658 0.064 Uiso 1 1 calc R . .
H34C H 0.3164 0.8796 0.5913 0.064 Uiso 1 1 calc R . .
C35 C 0.6129(4) 1.2115(3) 0.61291(14) 0.0401(7) Uani 1 1 d . . .
H35A H 0.6966 1.2461 0.6404 0.060 Uiso 1 1 calc R . .
H35B H 0.5499 1.2846 0.6111 0.060 Uiso 1 1 calc R . .
H35C H 0.6460 1.1914 0.5735 0.060 Uiso 1 1 calc R . .
C36 C 0.4120(3) 1.1021(3) 0.70374(11) 0.0289(5) Uani 1 1 d . . .
H36A H 0.3379 1.0230 0.7129 0.043 Uiso 1 1 calc R . .
H36B H 0.3660 1.1844 0.6941 0.043 Uiso 1 1 calc R . .
H36C H 0.4805 1.1287 0.7381 0.043 Uiso 1 1 calc R . .
C37 C 0.6183(3) 0.9087(3) 0.93701(11) 0.0356(6) Uani 1 1 d . . .
H37A H 0.5407 0.8271 0.9284 0.053 Uiso 1 1 calc R . .
H37B H 0.6039 0.9579 0.9749 0.053 Uiso 1 1 calc R . .
H37C H 0.7118 0.8747 0.9392 0.053 Uiso 1 1 calc R . .
C38 C 0.4305(3) 1.0814(3) 0.86673(12) 0.0324(6) Uani 1 1 d . . .
H38A H 0.4328 1.1613 0.8411 0.049 Uiso 1 1 calc R . .
H38B H 0.3965 1.1089 0.9052 0.049 Uiso 1 1 calc R . .
H38C H 0.3648 0.9982 0.8484 0.049 Uiso 1 1 calc R . .
C39 C 0.7349(3) 1.2055(3) 0.90469(12) 0.0344(6) Uani 1 1 d . . .
H39A H 0.8351 1.1885 0.9094 0.052 Uiso 1 1 calc R . .
H39B H 0.7036 1.2387 0.9429 0.052 Uiso 1 1 calc R . .
H39C H 0.7284 1.2783 0.8762 0.052 Uiso 1 1 calc R . .
C100 C 0.2434(7) 0.3799(7) 0.9493(3) 0.0735(16) Uiso 0.75 1 d P . .
C101 C 0.3083(9) 0.4693(9) 0.9802(4) 0.090(2) Uiso 0.75 1 d P . .
C102 C 0.4291(8) 0.4136(8) 0.9676(3) 0.0490(16) Uiso 0.50 1 d P . .
C103 C 0.5199(8) 0.5322(7) 1.0067(3) 0.0415(14) Uiso 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Er 0.01494(5) 0.01770(5) 0.01834(5) 0.00095(3) 0.00134(3) -0.00276(3)
P1 0.0167(3) 0.0168(3) 0.0161(2) 0.00099(19) 0.00299(19) 0.0021(2)
P2 0.0131(2) 0.0171(3) 0.0180(2) -0.00085(19) 0.00010(18) 0.00039(19)
Si1 0.0278(3) 0.0278(3) 0.0185(3) 0.0045(2) 0.0032(2) 0.0118(3)
Si2 0.0198(3) 0.0284(3) 0.0179(3) -0.0035(2) 0.0017(2) 0.0051(3)
N1 0.0172(9) 0.0212(9) 0.0199(8) 0.0030(7) 0.0034(7) 0.0046(7)
N2 0.0148(8) 0.0198(9) 0.0173(8) -0.0014(7) 0.0010(6) 0.0012(7)
C1 0.0305(14) 0.0200(12) 0.0529(17) -0.0024(11) 0.0078(12) -0.0008(10)
C2 0.0446(17) 0.0248(13) 0.0347(14) -0.0086(11) 0.0071(12) -0.0113(12)
C3 0.0368(15) 0.0328(15) 0.0357(14) 0.0024(11) -0.0130(12) -0.0134(12)
C4 0.0187(12) 0.0306(14) 0.065(2) 0.0063(13) -0.0100(12) -0.0062(10)
C5 0.0199(12) 0.0262(14) 0.074(2) -0.0048(14) 0.0175(13) -0.0052(10)
C6 0.0404(16) 0.0358(16) 0.0396(15) -0.0043(12) 0.0209(13) -0.0156(13)
C7 0.0534(19) 0.0353(16) 0.0291(13) 0.0133(11) 0.0019(12) -0.0177(14)
C8 0.0376(15) 0.0229(13) 0.0517(17) 0.0134(12) -0.0056(13) -0.0038(11)
C9 0.0183(10) 0.0161(10) 0.0185(9) 0.0012(7) 0.0015(7) 0.0026(8)
C10 0.0223(11) 0.0201(11) 0.0190(10) -0.0001(8) 0.0057(8) -0.0009(8)
C11 0.0376(15) 0.0284(13) 0.0312(13) -0.0028(10) 0.0023(11) 0.0124(11)
C12 0.061(2) 0.0306(15) 0.0390(16) 0.0007(12) 0.0142(14) 0.0197(14)
C13 0.060(2) 0.0231(13) 0.0388(15) -0.0067(11) 0.0241(14) -0.0025(13)
C14 0.0401(16) 0.0462(18) 0.0302(13) -0.0149(12) 0.0110(12) -0.0161(14)
C15 0.0245(12) 0.0399(15) 0.0268(12) -0.0070(11) 0.0050(10) -0.0006(11)
C16 0.0224(11) 0.0179(10) 0.0214(10) 0.0027(8) 0.0090(8) 0.0050(8)
C17 0.0334(14) 0.0301(13) 0.0225(11) 0.0046(9) 0.0057(10) 0.0035(11)
C18 0.0436(16) 0.0356(15) 0.0269(12) 0.0123(11) 0.0140(11) 0.0140(12)
C19 0.0340(14) 0.0276(13) 0.0447(15) 0.0156(11) 0.0228(12) 0.0087(11)
C20 0.0245(13) 0.0348(15) 0.0476(16) 0.0112(12) 0.0101(11) -0.0018(11)
C21 0.0213(11) 0.0329(13) 0.0295(12) 0.0071(10) 0.0050(9) 0.0023(10)
C22 0.0165(10) 0.0272(12) 0.0187(10) -0.0014(8) -0.0009(8) 0.0053(9)
C23 0.0325(13) 0.0291(13) 0.0218(11) 0.0026(9) -0.0034(9) 0.0068(10)
C24 0.0472(17) 0.0361(15) 0.0310(13) 0.0077(11) -0.0036(12) 0.0141(13)
C25 0.0432(17) 0.058(2) 0.0255(13) 0.0052(12) -0.0069(11) 0.0234(15)
C26 0.0335(15) 0.059(2) 0.0250(12) -0.0065(12) -0.0107(11) 0.0158(14)
C27 0.0255(12) 0.0354(14) 0.0268(12) -0.0074(10) -0.0051(9) 0.0080(11)
C28 0.0184(10) 0.0172(10) 0.0285(11) -0.0051(8) 0.0037(8) -0.0026(8)
C29 0.0163(11) 0.0285(13) 0.0397(14) -0.0045(10) 0.0016(9) -0.0025(9)
C30 0.0226(13) 0.0316(15) 0.0530(17) -0.0081(12) 0.0065(11) -0.0109(11)
C31 0.0392(16) 0.0232(14) 0.061(2) -0.0013(13) 0.0125(14) -0.0105(12)
C32 0.0342(15) 0.0215(13) 0.0551(18) 0.0038(12) 0.0075(13) 0.0007(11)
C33 0.0216(11) 0.0205(11) 0.0387(13) 0.0003(10) 0.0043(10) -0.0004(9)
C34 0.0495(18) 0.0550(19) 0.0260(13) -0.0009(12) -0.0115(12) 0.0251(15)
C35 0.060(2) 0.0290(14) 0.0379(15) 0.0126(12) 0.0218(14) 0.0177(14)
C36 0.0279(13) 0.0352(14) 0.0266(11) 0.0035(10) 0.0050(9) 0.0126(11)
C37 0.0423(16) 0.0453(17) 0.0204(11) 0.0036(11) 0.0049(10) 0.0093(13)
C38 0.0236(12) 0.0443(16) 0.0300(12) -0.0064(11) 0.0028(10) 0.0109(11)
C39 0.0323(14) 0.0369(15) 0.0319(13) -0.0157(11) -0.0016(11) 0.0068(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Er N1 89.82(7) . . ?
N2 Er C5 106.20(9) . . ?
N1 Er C5 120.30(9) . . ?
N2 Er C1 136.22(8) . . ?
N1 Er C1 115.21(8) . . ?
C5 Er C1 91.86(9) . . ?
N2 Er C4 131.39(9) . . ?
N1 Er C4 96.83(9) . . ?
C5 Er C4 31.87(11) . . ?
C1 Er C4 83.03(10) . . ?
N2 Er C8 109.93(8) . . ?
N1 Er C8 144.29(9) . . ?
C5 Er C8 83.42(10) . . ?
C1 Er C8 31.80(10) . . ?
C4 Er C8 91.86(10) . . ?
N2 Er C6 92.61(8) . . ?
N1 Er C6 150.63(10) . . ?
C5 Er C6 31.68(11) . . ?
C1 Er C6 82.26(10) . . ?
C4 Er C6 60.40(11) . . ?
C8 Er C6 60.68(11) . . ?
N2 Er C7 93.94(8) . . ?
N1 Er C7 175.68(9) . . ?
C5 Er C7 60.61(12) . . ?
C1 Er C7 60.51(10) . . ?
C4 Er C7 82.28(10) . . ?
C8 Er C7 31.84(11) . . ?
C6 Er C7 31.39(11) . . ?
N2 Er C2 166.94(9) . . ?
N1 Er C2 94.61(8) . . ?
C5 Er C2 82.12(10) . . ?
C1 Er C2 31.55(10) . . ?
C4 Er C2 60.28(11) . . ?
C8 Er C2 60.29(10) . . ?
C6 Er C2 89.55(9) . . ?
C7 Er C2 81.27(10) . . ?
N2 Er C3 161.75(9) . . ?
N1 Er C3 87.65(8) . . ?
C5 Er C3 60.24(11) . . ?
C1 Er C3 60.18(10) . . ?
C4 Er C3 31.51(11) . . ?
C8 Er C3 81.92(10) . . ?
C6 Er C3 81.00(10) . . ?
C7 Er C3 89.44(10) . . ?
C2 Er C3 31.14(10) . . ?
N2 Er C9 64.46(6) . . ?
N1 Er C9 62.60(6) . . ?
C5 Er C9 170.61(9) . . ?
C1 Er C9 94.62(8) . . ?
C4 Er C9 156.12(9) . . ?
C8 Er C9 98.59(8) . . ?
C6 Er C9 143.04(9) . . ?
C7 Er C9 117.26(9) . . ?
C2 Er C9 106.88(8) . . ?
C3 Er C9 129.06(9) . . ?
N2 Er P1 84.53(5) . . ?
N1 Er P1 30.87(5) . . ?
C5 Er P1 150.62(8) . . ?
C1 Er P1 98.99(7) . . ?
C4 Er P1 122.50(8) . . ?
C8 Er P1 119.22(8) . . ?
C6 Er P1 176.90(7) . . ?
C7 Er P1 147.47(8) . . ?
C2 Er P1 92.98(7) . . ?
C3 Er P1 102.08(7) . . ?
C9 Er P1 34.22(4) . . ?
N1 P1 C9 107.14(10) . . ?
N1 P1 C16 112.92(10) . . ?
C9 P1 C16 118.65(11) . . ?
N1 P1 C10 113.60(11) . . ?
C9 P1 C10 104.67(11) . . ?
C16 P1 C10 99.58(10) . . ?
N1 P1 Er 50.41(7) . . ?
C9 P1 Er 62.36(7) . . ?
C16 P1 Er 156.37(7) . . ?
C10 P1 Er 102.84(7) . . ?
N2 P2 C9 109.07(10) . . ?
N2 P2 C28 110.24(11) . . ?
C9 P2 C28 112.58(11) . . ?
N2 P2 C22 112.02(10) . . ?
C9 P2 C22 104.95(11) . . ?
C28 P2 C22 107.91(11) . . ?
N2 P2 Er 48.33(7) . . ?
C9 P2 Er 61.33(7) . . ?
C28 P2 Er 135.20(8) . . ?
C22 P2 Er 116.60(8) . . ?
N1 Si1 C35 116.53(13) . . ?
N1 Si1 C34 110.37(13) . . ?
C35 Si1 C34 107.40(16) . . ?
N1 Si1 C36 106.53(11) . . ?
C35 Si1 C36 106.13(13) . . ?
C34 Si1 C36 109.69(14) . . ?
N2 Si2 C38 110.11(11) . . ?
N2 Si2 C37 110.36(12) . . ?
C38 Si2 C37 109.23(14) . . ?
N2 Si2 C39 114.25(11) . . ?
C38 Si2 C39 105.81(14) . . ?
C37 Si2 C39 106.86(14) . . ?
P1 N1 Si1 139.07(12) . . ?
P1 N1 Er 98.71(9) . . ?
Si1 N1 Er 120.57(9) . . ?
P2 N2 Si2 125.25(11) . . ?
P2 N2 Er 101.05(9) . . ?
Si2 N2 Er 130.64(10) . . ?
C8 C1 C2 135.1(3) . . ?
C8 C1 Er 74.17(16) . . ?
C2 C1 Er 76.08(16) . . ?
C3 C2 C1 134.9(3) . . ?
C3 C2 Er 74.48(16) . . ?
C1 C2 Er 72.37(16) . . ?
C2 C3 C4 135.5(3) . . ?
C2 C3 Er 74.38(16) . . ?
C4 C3 Er 72.38(16) . . ?
C3 C4 C5 134.7(3) . . ?
C3 C4 Er 76.11(16) . . ?
C5 C4 Er 74.03(16) . . ?
C6 C5 C4 134.1(3) . . ?
C6 C5 Er 75.11(16) . . ?
C4 C5 Er 74.10(16) . . ?
C7 C6 C5 135.9(3) . . ?
C7 C6 Er 74.66(16) . . ?
C5 C6 Er 73.21(16) . . ?
C6 C7 C8 134.9(3) . . ?
C6 C7 Er 73.94(16) . . ?
C8 C7 Er 72.85(15) . . ?
C1 C8 C7 134.3(3) . . ?
C1 C8 Er 74.03(16) . . ?
C7 C8 Er 75.31(16) . . ?
P1 C9 P2 125.25(13) . . ?
P1 C9 Er 83.42(8) . . ?
P2 C9 Er 84.57(8) . . ?
C15 C10 C11 118.5(2) . . ?
C15 C10 P1 120.5(2) . . ?
C11 C10 P1 120.88(19) . . ?
C12 C11 C10 120.8(3) . . ?
C13 C12 C11 119.9(3) . . ?
C12 C13 C14 120.4(3) . . ?
C13 C14 C15 120.5(3) . . ?
C10 C15 C14 119.9(3) . . ?
C21 C16 C17 118.7(2) . . ?
C21 C16 P1 123.35(18) . . ?
C17 C16 P1 117.95(19) . . ?
C18 C17 C16 120.5(3) . . ?
C19 C18 C17 120.0(3) . . ?
C18 C19 C20 120.3(2) . . ?
C19 C20 C21 120.1(3) . . ?
C16 C21 C20 120.3(2) . . ?
C23 C22 C27 118.4(2) . . ?
C23 C22 P2 118.79(18) . . ?
C27 C22 P2 122.34(19) . . ?
C24 C23 C22 121.0(2) . . ?
C25 C24 C23 120.1(3) . . ?
C26 C25 C24 119.9(3) . . ?
C25 C26 C27 120.2(3) . . ?
C22 C27 C26 120.5(3) . . ?
C33 C28 C29 118.9(2) . . ?
C33 C28 P2 117.53(18) . . ?
C29 C28 P2 123.1(2) . . ?
C30 C29 C28 120.0(3) . . ?
C31 C30 C29 120.7(3) . . ?
C30 C31 C32 119.8(3) . . ?
C33 C32 C31 120.0(3) . . ?
C32 C33 C28 120.5(2) . . ?
C101 C100 C102 51.0(5) . . ?
C100 C101 C102 88.1(7) . . ?
C100 C101 C103 118.5(8) . 2_667 ?
C102 C101 C103 30.8(4) . 2_667 ?
C100 C101 C103 136.2(7) . . ?
C102 C101 C103 48.1(5) . . ?
C103 C101 C103 18.4(4) 2_667 . ?
C103 C102 C101 92.7(9) 2_667 . ?
C103 C102 C103 10.1(8) 2_667 . ?
C101 C102 C103 89.9(6) . . ?
C103 C102 C100 133.0(10) 2_667 . ?
C101 C102 C100 40.9(4) . . ?
C103 C102 C100 130.8(6) . . ?
C103 C103 C102 158.0(18) 2_667 2_667 ?
C103 C103 C102 11.9(10) 2_667 . ?
C102 C103 C102 169.9(8) 2_667 . ?
C103 C103 C101 115.3(14) 2_667 2_667 ?
C102 C103 C101 56.6(8) 2_667 2_667 ?
C102 C103 C101 120.2(6) . 2_667 ?
C103 C103 C101 46.4(11) 2_667 . ?
C102 C103 C101 139.8(9) 2_667 . ?
C102 C103 C101 42.0(4) . . ?
C101 C103 C101 161.6(4) 2_667 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er N2 2.3641(19) . ?
Er N1 2.3933(19) . ?
Er C5 2.560(3) . ?
Er C1 2.560(3) . ?
Er C4 2.561(3) . ?
Er C8 2.562(3) . ?
Er C6 2.584(3) . ?
Er C7 2.593(3) . ?
Er C2 2.607(3) . ?
Er C3 2.608(3) . ?
Er C9 2.737(2) . ?
Er P1 3.0697(7) . ?
P1 N1 1.594(2) . ?
P1 C9 1.738(2) . ?
P1 C16 1.817(2) . ?
P1 C10 1.819(2) . ?
P2 N2 1.6119(19) . ?
P2 C9 1.750(2) . ?
P2 C28 1.810(2) . ?
P2 C22 1.822(2) . ?
Si1 N1 1.723(2) . ?
Si1 C35 1.862(3) . ?
Si1 C34 1.869(3) . ?
Si1 C36 1.872(3) . ?
Si2 N2 1.7398(19) . ?
Si2 C38 1.862(3) . ?
Si2 C37 1.869(3) . ?
Si2 C39 1.872(3) . ?
C1 C8 1.403(4) . ?
C1 C2 1.406(4) . ?
C2 C3 1.400(5) . ?
C3 C4 1.404(5) . ?
C4 C5 1.406(5) . ?
C5 C6 1.404(5) . ?
C6 C7 1.401(5) . ?
C7 C8 1.414(5) . ?
C10 C15 1.393(3) . ?
C10 C11 1.393(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.367(5) . ?
C13 C14 1.371(5) . ?
C14 C15 1.393(4) . ?
C16 C21 1.383(4) . ?
C16 C17 1.404(3) . ?
C17 C18 1.385(4) . ?
C18 C19 1.374(4) . ?
C19 C20 1.377(4) . ?
C20 C21 1.394(4) . ?
C22 C23 1.390(4) . ?
C22 C27 1.395(3) . ?
C23 C24 1.388(3) . ?
C24 C25 1.385(4) . ?
C25 C26 1.377(5) . ?
C26 C27 1.396(4) . ?
C28 C33 1.389(3) . ?
C28 C29 1.406(3) . ?
C29 C30 1.386(4) . ?
C30 C31 1.373(5) . ?
C31 C32 1.395(4) . ?
C32 C33 1.387(4) . ?
C100 C101 1.144(10) . ?
C100 C102 1.746(10) . ?
C101 C102 1.358(10) . ?
C101 C103 1.626(11) 2_667 ?
C101 C103 2.031(11) . ?
C102 C103 0.833(8) 2_667 ?
C102 C103 1.512(11) . ?
C103 C103 0.707(12) 2_667 ?
C103 C102 0.833(8) 2_667 ?
C103 C101 1.626(11) 2_667 ?
|
1100885.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-27 05:05:50 +0300 (Sun, 27 Mar 2016) $
#$Revision: 180535 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100885.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100885
loop_
_publ_author_name
'Panda, Tarun K.'
'Zulys, Agustino'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
Bis(phosphinimino)methanides: Synthesis, Structure, and
Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2197
_journal_page_last 2202
_journal_paper_doi 10.1021/om0491138
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C41.5 H52 N2 P2 Si2 Yb'
_chemical_formula_weight 870.01
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 93.493(4)
_cell_angle_beta 92.759(4)
_cell_angle_gamma 99.268(4)
_cell_formula_units_Z 2
_cell_length_a 9.377(2)
_cell_length_b 9.508(2)
_cell_length_c 22.703(5)
_cell_measurement_temperature 173(2)
_cell_volume 1990.6(7)
_computing_molecular_graphics 'Diamond 2.1a '
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type 'Bruker Smart 1000 CCD'
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0195
_diffrn_reflns_av_sigmaI/netI 0.0303
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 24561
_diffrn_reflns_theta_full 30.57
_diffrn_reflns_theta_max 30.57
_diffrn_reflns_theta_min 0.90
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.521
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.640115
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.451
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 886
_exptl_crystal_size_max .6
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min .05
_refine_diff_density_max 1.616
_refine_diff_density_min -1.219
_refine_diff_density_rms 0.100
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 11939
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all 0.0326
_refine_ls_R_factor_gt 0.0265
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+1.1567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0621
_refine_ls_wR_factor_ref 0.0670
_reflns_number_gt 10682
_reflns_number_total 11939
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060420
_cod_data_source_file om0491138si20041116_113831.cif
_cod_data_source_block 1d
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C41.50 H52 N2 P2 Si2 Yb'
_cod_database_code 1100885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb Yb 0.538462(10) 0.778087(10) 0.743355(4) 0.01859(3) Uani 1 1 d . . .
P1 P 0.77058(6) 0.88181(6) 0.65951(2) 0.01737(10) Uani 1 1 d . . .
P2 P 0.82934(6) 0.95171(6) 0.79424(2) 0.01722(10) Uani 1 1 d . . .
Si1 Si 0.51058(8) 1.04211(8) 0.63937(3) 0.02478(14) Uani 1 1 d . . .
Si2 Si 0.61479(7) 1.03354(8) 0.87653(3) 0.02403(13) Uani 1 1 d . . .
N1 N 0.6111(2) 0.9179(2) 0.66369(8) 0.0195(4) Uani 1 1 d . . .
N2 N 0.6655(2) 0.9563(2) 0.81090(8) 0.0186(4) Uani 1 1 d . . .
C1 C 0.5296(3) 0.5098(3) 0.72393(15) 0.0375(6) Uani 1 1 d . . .
H1 H 0.5991 0.4536 0.7114 0.045 Uiso 1 1 calc R . .
C2 C 0.4456(4) 0.5478(3) 0.67644(14) 0.0390(7) Uani 1 1 d . . .
H2 H 0.4663 0.5051 0.6396 0.047 Uiso 1 1 calc R . .
C3 C 0.3381(3) 0.6341(3) 0.67048(14) 0.0394(7) Uani 1 1 d . . .
H3 H 0.3019 0.6345 0.6307 0.047 Uiso 1 1 calc R . .
C4 C 0.2719(3) 0.7195(3) 0.70945(16) 0.0406(7) Uani 1 1 d . . .
H4 H 0.2087 0.7722 0.6896 0.049 Uiso 1 1 calc R . .
C5 C 0.2769(3) 0.7456(3) 0.77120(17) 0.0423(8) Uani 1 1 d . . .
H5 H 0.2157 0.8109 0.7836 0.051 Uiso 1 1 calc R . .
C6 C 0.3521(4) 0.6969(3) 0.81849(15) 0.0423(7) Uani 1 1 d . . .
H6 H 0.3241 0.7312 0.8556 0.051 Uiso 1 1 calc R . .
C7 C 0.4583(4) 0.6101(3) 0.82469(14) 0.0420(7) Uani 1 1 d . . .
H7 H 0.4847 0.5994 0.8649 0.050 Uiso 1 1 calc R . .
C8 C 0.5349(3) 0.5354(3) 0.78554(15) 0.0398(7) Uani 1 1 d . . .
H8 H 0.6067 0.4922 0.8052 0.048 Uiso 1 1 calc R . .
C9 C 0.8268(2) 0.8411(2) 0.72964(10) 0.0188(4) Uani 1 1 d . . .
H9 H 0.8829 0.7604 0.7317 0.023 Uiso 1 1 calc R . .
C10 C 0.7792(3) 0.7220(3) 0.61218(10) 0.0225(4) Uani 1 1 d . . .
C11 C 0.8968(3) 0.6495(3) 0.61826(12) 0.0333(6) Uani 1 1 d . . .
H11 H 0.9700 0.6808 0.6488 0.040 Uiso 1 1 calc R . .
C12 C 0.9077(4) 0.5325(3) 0.58028(15) 0.0445(8) Uani 1 1 d . . .
H12 H 0.9868 0.4825 0.5855 0.053 Uiso 1 1 calc R . .
C13 C 0.8050(4) 0.4886(3) 0.53526(14) 0.0441(8) Uani 1 1 d . . .
H13 H 0.8134 0.4091 0.5090 0.053 Uiso 1 1 calc R . .
C14 C 0.6893(4) 0.5601(4) 0.52809(14) 0.0432(8) Uani 1 1 d . . .
H14 H 0.6187 0.5301 0.4965 0.052 Uiso 1 1 calc R . .
C15 C 0.6747(3) 0.6757(3) 0.56672(12) 0.0330(6) Uani 1 1 d . . .
H15 H 0.5934 0.7229 0.5620 0.040 Uiso 1 1 calc R . .
C16 C 0.8888(3) 1.0131(2) 0.62145(10) 0.0211(4) Uani 1 1 d . . .
C17 C 0.8507(3) 1.0314(3) 0.56237(11) 0.0301(5) Uani 1 1 d . . .
H17 H 0.7659 0.9755 0.5434 0.036 Uiso 1 1 calc R . .
C18 C 0.9359(3) 1.1306(3) 0.53141(13) 0.0356(6) Uani 1 1 d . . .
H18 H 0.9094 1.1424 0.4913 0.043 Uiso 1 1 calc R . .
C19 C 1.0591(3) 1.2124(3) 0.55845(14) 0.0357(6) Uani 1 1 d . . .
H19 H 1.1165 1.2813 0.5372 0.043 Uiso 1 1 calc R . .
C20 C 1.0991(3) 1.1943(3) 0.61643(14) 0.0370(6) Uani 1 1 d . . .
H20 H 1.1839 1.2507 0.6351 0.044 Uiso 1 1 calc R . .
C21 C 1.0148(3) 1.0930(3) 0.64765(12) 0.0294(5) Uani 1 1 d . . .
H21 H 1.0441 1.0788 0.6872 0.035 Uiso 1 1 calc R . .
C22 C 0.9298(2) 0.8700(3) 0.84982(10) 0.0230(4) Uani 1 1 d . . .
C23 C 0.9147(3) 0.7215(3) 0.84808(11) 0.0301(5) Uani 1 1 d . . .
H23 H 0.8609 0.6657 0.8158 0.036 Uiso 1 1 calc R . .
C24 C 0.9771(4) 0.6540(4) 0.89277(13) 0.0407(7) Uani 1 1 d . . .
H24 H 0.9668 0.5527 0.8908 0.049 Uiso 1 1 calc R . .
C25 C 1.0546(4) 0.7348(4) 0.94034(13) 0.0446(8) Uani 1 1 d . . .
H25 H 1.0966 0.6888 0.9712 0.054 Uiso 1 1 calc R . .
C26 C 1.0706(3) 0.8820(4) 0.94288(13) 0.0410(7) Uani 1 1 d . . .
H26 H 1.1245 0.9370 0.9753 0.049 Uiso 1 1 calc R . .
C27 C 1.0079(3) 0.9504(3) 0.89798(12) 0.0317(6) Uani 1 1 d . . .
H27 H 1.0183 1.0517 0.9002 0.038 Uiso 1 1 calc R . .
C28 C 0.9249(3) 1.1314(3) 0.78761(11) 0.0236(5) Uani 1 1 d . . .
C29 C 1.0757(3) 1.1684(3) 0.79619(13) 0.0307(5) Uani 1 1 d . . .
H29 H 1.1314 1.1011 0.8104 0.037 Uiso 1 1 calc R . .
C30 C 1.1438(3) 1.3039(3) 0.78387(15) 0.0404(7) Uani 1 1 d . . .
H30 H 1.2458 1.3292 0.7904 0.049 Uiso 1 1 calc R . .
C31 C 1.0643(4) 1.4011(3) 0.76230(16) 0.0452(8) Uani 1 1 d . . .
H31 H 1.1114 1.4931 0.7537 0.054 Uiso 1 1 calc R . .
C32 C 0.9149(4) 1.3647(3) 0.75311(16) 0.0407(7) Uani 1 1 d . . .
H32 H 0.8602 1.4318 0.7380 0.049 Uiso 1 1 calc R . .
C33 C 0.8454(3) 1.2307(3) 0.76588(12) 0.0289(5) Uani 1 1 d . . .
H33 H 0.7432 1.2066 0.7597 0.035 Uiso 1 1 calc R . .
C34 C 0.3774(4) 0.9599(4) 0.57801(13) 0.0451(8) Uani 1 1 d . . .
H34A H 0.4294 0.9269 0.5448 0.068 Uiso 1 1 calc R . .
H34B H 0.3200 1.0310 0.5651 0.068 Uiso 1 1 calc R . .
H34C H 0.3131 0.8786 0.5920 0.068 Uiso 1 1 calc R . .
C35 C 0.6135(4) 1.2085(3) 0.61334(14) 0.0422(7) Uani 1 1 d . . .
H35A H 0.6985 1.2422 0.6403 0.063 Uiso 1 1 calc R . .
H35B H 0.5514 1.2821 0.6124 0.063 Uiso 1 1 calc R . .
H35C H 0.6448 1.1889 0.5735 0.063 Uiso 1 1 calc R . .
C36 C 0.4119(3) 1.1001(3) 0.70373(12) 0.0304(5) Uani 1 1 d . . .
H36A H 0.3341 1.0229 0.7117 0.046 Uiso 1 1 calc R . .
H36B H 0.3705 1.1851 0.6946 0.046 Uiso 1 1 calc R . .
H36C H 0.4794 1.1227 0.7386 0.046 Uiso 1 1 calc R . .
C37 C 0.6169(4) 0.9081(4) 0.93680(12) 0.0388(7) Uani 1 1 d . . .
H37A H 0.5359 0.8290 0.9294 0.058 Uiso 1 1 calc R . .
H37B H 0.6077 0.9592 0.9749 0.058 Uiso 1 1 calc R . .
H37C H 0.7083 0.8705 0.9377 0.058 Uiso 1 1 calc R . .
C38 C 0.4301(3) 1.0797(3) 0.86628(13) 0.0348(6) Uani 1 1 d . . .
H38A H 0.4331 1.1597 0.8409 0.052 Uiso 1 1 calc R . .
H38B H 0.3961 1.1070 0.9048 0.052 Uiso 1 1 calc R . .
H38C H 0.3640 0.9968 0.8478 0.052 Uiso 1 1 calc R . .
C39 C 0.7351(3) 1.2042(3) 0.90418(13) 0.0365(6) Uani 1 1 d . . .
H39A H 0.8348 1.1867 0.9100 0.055 Uiso 1 1 calc R . .
H39B H 0.7021 1.2391 0.9418 0.055 Uiso 1 1 calc R . .
H39C H 0.7312 1.2758 0.8752 0.055 Uiso 1 1 calc R . .
C100 C 0.2424(8) 0.3817(8) 0.9497(3) 0.0835(19) Uiso 0.75 1 d P . .
C101 C 0.3113(10) 0.4710(10) 0.9815(4) 0.099(2) Uiso 0.75 1 d P . .
C102 C 0.4281(9) 0.4123(9) 0.9668(4) 0.0576(19) Uiso 0.50 1 d P . .
C103 C 0.5195(8) 0.5322(7) 1.0067(3) 0.0461(16) Uiso 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Yb 0.01575(5) 0.01877(5) 0.01998(5) 0.00202(3) 0.00159(3) -0.00140(3)
P1 0.0173(3) 0.0182(3) 0.0172(2) 0.00233(19) 0.00319(19) 0.0039(2)
P2 0.0138(2) 0.0182(3) 0.0193(2) 0.00001(19) 0.00049(19) 0.00205(19)
Si1 0.0290(3) 0.0285(3) 0.0204(3) 0.0053(2) 0.0034(2) 0.0138(3)
Si2 0.0215(3) 0.0312(4) 0.0197(3) -0.0026(2) 0.0023(2) 0.0067(3)
N1 0.0167(8) 0.0219(9) 0.0213(9) 0.0038(7) 0.0036(7) 0.0055(7)
N2 0.0158(8) 0.0198(9) 0.0194(8) -0.0014(7) 0.0007(7) 0.0017(7)
C1 0.0327(14) 0.0193(12) 0.0598(19) 0.0007(12) 0.0079(13) 0.0009(10)
C2 0.0458(17) 0.0277(14) 0.0372(15) -0.0076(11) 0.0074(13) -0.0106(12)
C3 0.0388(16) 0.0350(15) 0.0370(15) 0.0036(12) -0.0114(12) -0.0125(12)
C4 0.0198(12) 0.0301(14) 0.068(2) 0.0075(14) -0.0108(13) -0.0051(10)
C5 0.0213(13) 0.0287(14) 0.075(2) -0.0027(14) 0.0182(14) -0.0042(11)
C6 0.0394(16) 0.0376(16) 0.0441(16) -0.0025(13) 0.0197(13) -0.0139(13)
C7 0.0494(18) 0.0386(16) 0.0324(14) 0.0138(12) 0.0030(13) -0.0139(14)
C8 0.0372(15) 0.0235(13) 0.0570(19) 0.0160(13) -0.0068(13) -0.0024(11)
C9 0.0197(10) 0.0167(10) 0.0204(10) 0.0024(8) 0.0025(8) 0.0037(8)
C10 0.0234(11) 0.0219(11) 0.0223(10) 0.0009(8) 0.0071(8) 0.0021(9)
C11 0.0398(15) 0.0313(14) 0.0319(13) -0.0007(11) 0.0040(11) 0.0157(12)
C12 0.065(2) 0.0323(15) 0.0430(17) 0.0000(13) 0.0157(15) 0.0241(15)
C13 0.067(2) 0.0250(14) 0.0393(16) -0.0044(11) 0.0287(15) -0.0005(14)
C14 0.0412(17) 0.0469(18) 0.0336(15) -0.0146(13) 0.0116(12) -0.0130(14)
C15 0.0264(13) 0.0420(16) 0.0280(12) -0.0071(11) 0.0050(10) 0.0007(11)
C16 0.0236(11) 0.0197(10) 0.0220(10) 0.0040(8) 0.0099(8) 0.0061(8)
C17 0.0350(14) 0.0328(14) 0.0236(11) 0.0063(10) 0.0066(10) 0.0055(11)
C18 0.0448(16) 0.0386(15) 0.0292(13) 0.0145(11) 0.0166(12) 0.0153(13)
C19 0.0361(15) 0.0298(14) 0.0473(16) 0.0181(12) 0.0237(12) 0.0121(11)
C20 0.0261(13) 0.0369(15) 0.0485(17) 0.0124(13) 0.0114(12) 0.0000(11)
C21 0.0220(11) 0.0347(14) 0.0323(13) 0.0093(11) 0.0062(10) 0.0032(10)
C22 0.0177(10) 0.0317(12) 0.0205(10) -0.0004(9) 0.0000(8) 0.0080(9)
C23 0.0351(14) 0.0305(13) 0.0249(11) 0.0022(10) -0.0050(10) 0.0083(11)
C24 0.0528(19) 0.0403(16) 0.0331(14) 0.0082(12) -0.0051(13) 0.0200(14)
C25 0.0469(18) 0.063(2) 0.0291(14) 0.0072(13) -0.0073(12) 0.0268(16)
C26 0.0352(15) 0.061(2) 0.0271(13) -0.0055(13) -0.0123(11) 0.0167(14)
C27 0.0271(13) 0.0403(15) 0.0275(12) -0.0054(11) -0.0056(10) 0.0100(11)
C28 0.0185(11) 0.0202(11) 0.0300(12) -0.0027(9) 0.0038(9) -0.0021(8)
C29 0.0189(11) 0.0292(13) 0.0417(14) -0.0037(11) 0.0021(10) -0.0007(10)
C30 0.0263(13) 0.0340(15) 0.0554(19) -0.0079(13) 0.0076(12) -0.0093(11)
C31 0.0436(18) 0.0238(14) 0.063(2) -0.0024(13) 0.0113(15) -0.0107(12)
C32 0.0389(16) 0.0213(13) 0.062(2) 0.0046(13) 0.0098(14) 0.0018(11)
C33 0.0231(12) 0.0221(12) 0.0406(14) 0.0017(10) 0.0045(10) 0.0006(9)
C34 0.0524(19) 0.057(2) 0.0297(14) -0.0006(13) -0.0132(13) 0.0266(16)
C35 0.061(2) 0.0323(15) 0.0412(16) 0.0136(12) 0.0232(14) 0.0217(14)
C36 0.0307(13) 0.0361(14) 0.0288(12) 0.0045(10) 0.0061(10) 0.0163(11)
C37 0.0440(17) 0.0517(18) 0.0219(12) 0.0049(12) 0.0047(11) 0.0101(14)
C38 0.0260(13) 0.0459(17) 0.0335(14) -0.0072(12) 0.0050(10) 0.0118(12)
C39 0.0325(14) 0.0416(16) 0.0337(14) -0.0151(12) -0.0002(11) 0.0075(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Yb N1 90.35(7) . . ?
N2 Yb C5 105.98(9) . . ?
N1 Yb C5 119.74(10) . . ?
N2 Yb C4 131.53(9) . . ?
N1 Yb C4 96.16(9) . . ?
C5 Yb C4 32.13(12) . . ?
N2 Yb C8 109.21(9) . . ?
N1 Yb C8 144.67(10) . . ?
C5 Yb C8 83.71(11) . . ?
C4 Yb C8 92.31(10) . . ?
N2 Yb C1 135.59(9) . . ?
N1 Yb C1 115.38(9) . . ?
C5 Yb C1 92.29(10) . . ?
C4 Yb C1 83.41(10) . . ?
C8 Yb C1 31.93(11) . . ?
N2 Yb C6 92.12(9) . . ?
N1 Yb C6 150.20(10) . . ?
C5 Yb C6 31.84(11) . . ?
C4 Yb C6 60.80(12) . . ?
C8 Yb C6 60.77(12) . . ?
C1 Yb C6 82.53(11) . . ?
N2 Yb C7 93.33(9) . . ?
N1 Yb C7 175.86(9) . . ?
C5 Yb C7 60.97(12) . . ?
C4 Yb C7 82.82(11) . . ?
C8 Yb C7 31.70(11) . . ?
C1 Yb C7 60.55(11) . . ?
C6 Yb C7 31.60(11) . . ?
N2 Yb C2 166.44(9) . . ?
N1 Yb C2 94.42(9) . . ?
C5 Yb C2 82.60(11) . . ?
C4 Yb C2 60.56(11) . . ?
C8 Yb C2 60.58(11) . . ?
C1 Yb C2 31.69(10) . . ?
C6 Yb C2 90.03(10) . . ?
C7 Yb C2 81.57(10) . . ?
N2 Yb C3 161.94(9) . . ?
N1 Yb C3 87.04(8) . . ?
C5 Yb C3 60.59(11) . . ?
C4 Yb C3 31.55(11) . . ?
C8 Yb C3 82.50(10) . . ?
C1 Yb C3 60.62(10) . . ?
C6 Yb C3 81.54(11) . . ?
C7 Yb C3 90.05(10) . . ?
C2 Yb C3 31.44(11) . . ?
N2 Yb C9 64.86(7) . . ?
N1 Yb C9 63.24(6) . . ?
C5 Yb C9 170.78(9) . . ?
C4 Yb C9 155.84(10) . . ?
C8 Yb C9 98.05(9) . . ?
C1 Yb C9 93.93(8) . . ?
C6 Yb C9 142.84(9) . . ?
C7 Yb C9 116.77(9) . . ?
C2 Yb C9 106.19(9) . . ?
C3 Yb C9 128.57(9) . . ?
N2 Yb P1 85.06(5) . . ?
N1 Yb P1 31.17(5) . . ?
C5 Yb P1 150.33(9) . . ?
C4 Yb P1 121.98(8) . . ?
C8 Yb P1 119.22(8) . . ?
C1 Yb P1 98.75(7) . . ?
C6 Yb P1 176.99(8) . . ?
C7 Yb P1 147.39(9) . . ?
C2 Yb P1 92.48(7) . . ?
C3 Yb P1 101.46(8) . . ?
C9 Yb P1 34.55(5) . . ?
N1 P1 C9 107.03(11) . . ?
N1 P1 C16 112.91(11) . . ?
C9 P1 C16 118.62(11) . . ?
N1 P1 C10 113.59(11) . . ?
C9 P1 C10 104.68(11) . . ?
C16 P1 C10 99.74(11) . . ?
N1 P1 Yb 50.38(7) . . ?
C9 P1 Yb 62.16(8) . . ?
C16 P1 Yb 156.06(8) . . ?
C10 P1 Yb 103.03(8) . . ?
N2 P2 C9 108.78(10) . . ?
N2 P2 C28 110.23(11) . . ?
C9 P2 C28 112.86(11) . . ?
N2 P2 C22 112.33(11) . . ?
C9 P2 C22 104.89(11) . . ?
C28 P2 C22 107.70(12) . . ?
N2 P2 Yb 48.28(7) . . ?
C9 P2 Yb 61.05(8) . . ?
C28 P2 Yb 135.10(8) . . ?
C22 P2 Yb 116.92(8) . . ?
N1 Si1 C35 116.58(13) . . ?
N1 Si1 C36 106.79(11) . . ?
C35 Si1 C36 105.85(14) . . ?
N1 Si1 C34 110.31(13) . . ?
C35 Si1 C34 107.46(16) . . ?
C36 Si1 C34 109.65(15) . . ?
N1 Si1 Yb 34.57(7) . . ?
C35 Si1 Yb 141.48(12) . . ?
C36 Si1 Yb 75.65(8) . . ?
C34 Si1 Yb 107.97(12) . . ?
N2 Si2 C38 110.35(11) . . ?
N2 Si2 C37 110.43(12) . . ?
C38 Si2 C37 109.29(15) . . ?
N2 Si2 C39 114.20(12) . . ?
C38 Si2 C39 105.68(14) . . ?
C37 Si2 C39 106.67(15) . . ?
P1 N1 Si1 138.82(13) . . ?
P1 N1 Yb 98.45(9) . . ?
Si1 N1 Yb 121.04(10) . . ?
P2 N2 Si2 125.12(11) . . ?
P2 N2 Yb 100.97(9) . . ?
Si2 N2 Yb 130.99(10) . . ?
C8 C1 C2 134.9(3) . . ?
C8 C1 Yb 73.97(16) . . ?
C2 C1 Yb 75.78(17) . . ?
C1 C2 C3 135.2(3) . . ?
C1 C2 Yb 72.53(16) . . ?
C3 C2 Yb 74.48(16) . . ?
C4 C3 C2 134.9(3) . . ?
C4 C3 Yb 72.13(16) . . ?
C2 C3 Yb 74.08(16) . . ?
C3 C4 C5 134.9(3) . . ?
C3 C4 Yb 76.32(16) . . ?
C5 C4 Yb 73.73(16) . . ?
C6 C5 C4 134.2(3) . . ?
C6 C5 Yb 75.10(17) . . ?
C4 C5 Yb 74.14(17) . . ?
C5 C6 C7 135.9(3) . . ?
C5 C6 Yb 73.06(17) . . ?
C7 C6 Yb 74.66(17) . . ?
C8 C7 C6 135.0(3) . . ?
C8 C7 Yb 73.07(16) . . ?
C6 C7 Yb 73.73(17) . . ?
C7 C8 C1 134.5(3) . . ?
C7 C8 Yb 75.23(16) . . ?
C1 C8 Yb 74.10(16) . . ?
P1 C9 P2 125.05(13) . . ?
P1 C9 Yb 83.28(8) . . ?
P2 C9 Yb 84.59(9) . . ?
C15 C10 C11 118.6(2) . . ?
C15 C10 P1 120.7(2) . . ?
C11 C10 P1 120.48(19) . . ?
C12 C11 C10 120.7(3) . . ?
C13 C12 C11 120.2(3) . . ?
C12 C13 C14 119.9(3) . . ?
C13 C14 C15 120.7(3) . . ?
C10 C15 C14 119.9(3) . . ?
C21 C16 C17 118.8(2) . . ?
C21 C16 P1 123.32(18) . . ?
C17 C16 P1 117.84(19) . . ?
C18 C17 C16 120.3(3) . . ?
C19 C18 C17 120.3(3) . . ?
C18 C19 C20 120.0(3) . . ?
C19 C20 C21 119.9(3) . . ?
C16 C21 C20 120.5(3) . . ?
C23 C22 C27 118.8(2) . . ?
C23 C22 P2 118.87(18) . . ?
C27 C22 P2 121.9(2) . . ?
C24 C23 C22 121.0(3) . . ?
C23 C24 C25 119.9(3) . . ?
C26 C25 C24 120.0(3) . . ?
C25 C26 C27 120.3(3) . . ?
C26 C27 C22 120.1(3) . . ?
C33 C28 C29 119.2(2) . . ?
C33 C28 P2 117.41(18) . . ?
C29 C28 P2 122.9(2) . . ?
C30 C29 C28 119.9(3) . . ?
C31 C30 C29 120.4(3) . . ?
C30 C31 C32 120.0(3) . . ?
C33 C32 C31 120.2(3) . . ?
C32 C33 C28 120.2(3) . . ?
C101 C100 C102 51.0(6) . . ?
C100 C101 C102 87.0(8) . . ?
C100 C101 C103 118.9(8) . 2_667 ?
C102 C101 C103 32.3(5) . 2_667 ?
C100 C101 C103 137.0(8) . . ?
C102 C101 C103 50.1(6) . . ?
C103 C101 C103 18.9(5) 2_667 . ?
C103 C102 C101 90.1(10) 2_667 . ?
C103 C102 C103 10.2(9) 2_667 . ?
C101 C102 C103 87.2(7) . . ?
C103 C102 C100 131.6(11) 2_667 . ?
C101 C102 C100 42.0(5) . . ?
C103 C102 C100 129.2(7) . . ?
C103 C103 C102 157(2) 2_667 2_667 ?
C103 C103 C102 12.5(11) 2_667 . ?
C102 C103 C102 169.8(9) 2_667 . ?
C103 C103 C101 113.6(15) 2_667 2_667 ?
C102 C103 C101 57.6(8) 2_667 2_667 ?
C102 C103 C101 118.9(6) . 2_667 ?
C103 C103 C101 47.5(12) 2_667 . ?
C102 C103 C101 139.2(10) 2_667 . ?
C102 C103 C101 42.8(4) . . ?
C101 C103 C101 161.1(5) 2_667 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb N2 2.3451(19) . ?
Yb N1 2.3712(19) . ?
Yb C5 2.538(3) . ?
Yb C4 2.543(3) . ?
Yb C8 2.548(3) . ?
Yb C1 2.550(3) . ?
Yb C6 2.564(3) . ?
Yb C7 2.575(3) . ?
Yb C2 2.591(3) . ?
Yb C3 2.596(3) . ?
Yb C9 2.711(2) . ?
Yb P1 3.0447(7) . ?
P1 N1 1.593(2) . ?
P1 C9 1.739(2) . ?
P1 C16 1.819(2) . ?
P1 C10 1.822(2) . ?
P2 N2 1.607(2) . ?
P2 C9 1.749(2) . ?
P2 C28 1.816(2) . ?
P2 C22 1.823(2) . ?
Si1 N1 1.725(2) . ?
Si1 C35 1.860(3) . ?
Si1 C36 1.868(3) . ?
Si1 C34 1.870(3) . ?
Si2 N2 1.741(2) . ?
Si2 C38 1.861(3) . ?
Si2 C37 1.870(3) . ?
Si2 C39 1.875(3) . ?
C1 C8 1.402(5) . ?
C1 C2 1.404(5) . ?
C2 C3 1.405(5) . ?
C3 C4 1.398(5) . ?
C4 C5 1.406(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.399(5) . ?
C7 C8 1.399(5) . ?
C10 C15 1.388(3) . ?
C10 C11 1.396(4) . ?
C11 C12 1.386(4) . ?
C12 C13 1.368(5) . ?
C13 C14 1.378(5) . ?
C14 C15 1.393(4) . ?
C16 C21 1.384(4) . ?
C16 C17 1.400(3) . ?
C17 C18 1.384(4) . ?
C18 C19 1.379(5) . ?
C19 C20 1.380(4) . ?
C20 C21 1.395(4) . ?
C22 C23 1.394(4) . ?
C22 C27 1.399(3) . ?
C23 C24 1.388(3) . ?
C24 C25 1.389(5) . ?
C25 C26 1.381(5) . ?
C26 C27 1.399(4) . ?
C28 C33 1.392(4) . ?
C28 C29 1.402(3) . ?
C29 C30 1.393(4) . ?
C30 C31 1.376(5) . ?
C31 C32 1.390(5) . ?
C32 C33 1.389(4) . ?
C100 C101 1.166(11) . ?
C100 C102 1.739(11) . ?
C101 C102 1.354(12) . ?
C101 C103 1.603(12) 2_667 ?
C101 C103 1.991(12) . ?
C102 C103 0.856(9) 2_667 ?
C102 C103 1.529(12) . ?
C103 C103 0.704(13) 2_667 ?
C103 C102 0.856(9) 2_667 ?
C103 C101 1.603(12) 2_667 ?
|
1100886.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-27 05:05:50 +0300 (Sun, 27 Mar 2016) $
#$Revision: 180535 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100886.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100886
loop_
_publ_author_name
'Panda, Tarun K.'
'Zulys, Agustino'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
Bis(phosphinimino)methanides: Synthesis, Structure, and
Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2197
_journal_page_last 2202
_journal_paper_doi 10.1021/om0491138
_journal_volume 24
_journal_year 2005
_chemical_formula_sum 'C41.5 H52 Lu N2 P2 Si2'
_chemical_formula_weight 871.94
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 93.619(5)
_cell_angle_beta 92.852(5)
_cell_angle_gamma 99.437(5)
_cell_formula_units_Z 2
_cell_length_a 9.351(2)
_cell_length_b 9.500(2)
_cell_length_c 22.700(5)
_cell_measurement_temperature 173(2)
_cell_volume 1981.7(7)
_computing_molecular_graphics 'Diamond 2.1 '
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type 'Bruker Smart 1000 CCD'
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0189
_diffrn_reflns_av_sigmaI/netI 0.0294
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 23438
_diffrn_reflns_theta_full 30.55
_diffrn_reflns_theta_max 30.55
_diffrn_reflns_theta_min 0.90
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.663
_exptl_absorpt_correction_T_max 0.345
_exptl_absorpt_correction_T_min 0.19044
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details ?
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.461
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 888
_exptl_crystal_size_max .7
_exptl_crystal_size_mid .5
_exptl_crystal_size_min .4
_refine_diff_density_max 1.297
_refine_diff_density_min -1.661
_refine_diff_density_rms 0.101
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 11918
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0275
_refine_ls_R_factor_gt 0.0237
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0565
_refine_ls_wR_factor_ref 0.0605
_reflns_number_gt 10971
_reflns_number_total 11918
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 4060421
_cod_data_source_file om0491138si20041116_113831.cif
_cod_data_source_block 1e
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C41.50 H52 Lu N2 P2 Si2'
_cod_database_code 1100886
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu Lu 0.539565(9) 0.775943(9) 0.743258(4) 0.01579(3) Uani 1 1 d . . .
P1 P 0.77048(6) 0.88096(6) 0.65951(2) 0.01521(9) Uani 1 1 d . . .
P2 P 0.82938(6) 0.95091(6) 0.79426(2) 0.01481(9) Uani 1 1 d . . .
Si1 Si 0.51030(7) 1.04075(7) 0.63956(3) 0.02240(12) Uani 1 1 d . . .
Si2 Si 0.61410(7) 1.03252(7) 0.87633(3) 0.02122(12) Uani 1 1 d . . .
N1 N 0.61096(19) 0.91688(19) 0.66426(8) 0.0179(3) Uani 1 1 d . . .
N2 N 0.66470(18) 0.95494(19) 0.81074(7) 0.0158(3) Uani 1 1 d . . .
C1 C 0.5310(3) 0.5086(3) 0.72354(14) 0.0348(6) Uani 1 1 d . . .
H1 H 0.6014 0.4533 0.7110 0.042 Uiso 1 1 calc R . .
C2 C 0.4465(3) 0.5457(3) 0.67630(12) 0.0348(6) Uani 1 1 d . . .
H2 H 0.4668 0.5021 0.6395 0.042 Uiso 1 1 calc R . .
C3 C 0.3391(3) 0.6316(3) 0.66992(12) 0.0348(6) Uani 1 1 d . . .
H3 H 0.3025 0.6303 0.6301 0.042 Uiso 1 1 calc R . .
C4 C 0.2732(3) 0.7188(3) 0.70836(14) 0.0359(6) Uani 1 1 d . . .
H4 H 0.2108 0.7718 0.6882 0.043 Uiso 1 1 calc R . .
C5 C 0.2785(3) 0.7459(3) 0.77072(14) 0.0367(6) Uani 1 1 d . . .
H5 H 0.2179 0.8120 0.7830 0.044 Uiso 1 1 calc R . .
C6 C 0.3531(3) 0.6969(3) 0.81819(12) 0.0363(6) Uani 1 1 d . . .
H6 H 0.3256 0.7323 0.8553 0.044 Uiso 1 1 calc R . .
C7 C 0.4584(3) 0.6088(3) 0.82456(12) 0.0384(7) Uani 1 1 d . . .
H7 H 0.4832 0.5966 0.8648 0.046 Uiso 1 1 calc R . .
C8 C 0.5358(3) 0.5341(3) 0.78524(14) 0.0369(6) Uani 1 1 d . . .
H8 H 0.6078 0.4912 0.8049 0.044 Uiso 1 1 calc R . .
C9 C 0.8267(2) 0.8400(2) 0.72944(9) 0.0167(4) Uani 1 1 d . . .
H9 H 0.8833 0.7596 0.7314 0.020 Uiso 1 1 calc R . .
C10 C 0.7795(2) 0.7209(2) 0.61202(9) 0.0200(4) Uani 1 1 d . . .
C11 C 0.8966(3) 0.6494(3) 0.61812(11) 0.0305(5) Uani 1 1 d . . .
H11 H 0.9698 0.6809 0.6488 0.037 Uiso 1 1 calc R . .
C12 C 0.9085(4) 0.5319(3) 0.57987(13) 0.0413(7) Uani 1 1 d . . .
H12 H 0.9883 0.4826 0.5850 0.050 Uiso 1 1 calc R . .
C13 C 0.8048(4) 0.4875(3) 0.53480(13) 0.0412(7) Uani 1 1 d . . .
H13 H 0.8129 0.4076 0.5086 0.049 Uiso 1 1 calc R . .
C14 C 0.6892(3) 0.5584(3) 0.52745(12) 0.0403(7) Uani 1 1 d . . .
H14 H 0.6185 0.5283 0.4957 0.048 Uiso 1 1 calc R . .
C15 C 0.6746(3) 0.6747(3) 0.56643(11) 0.0309(5) Uani 1 1 d . . .
H15 H 0.5932 0.7218 0.5617 0.037 Uiso 1 1 calc R . .
C16 C 0.8892(2) 1.0125(2) 0.62145(9) 0.0193(4) Uani 1 1 d . . .
C17 C 0.8512(3) 1.0309(3) 0.56240(10) 0.0286(5) Uani 1 1 d . . .
H17 H 0.7662 0.9745 0.5434 0.034 Uiso 1 1 calc R . .
C18 C 0.9364(3) 1.1305(3) 0.53138(11) 0.0343(6) Uani 1 1 d . . .
H18 H 0.9098 1.1423 0.4913 0.041 Uiso 1 1 calc R . .
C19 C 1.0598(3) 1.2123(3) 0.55884(13) 0.0345(6) Uani 1 1 d . . .
H19 H 1.1177 1.2813 0.5377 0.041 Uiso 1 1 calc R . .
C20 C 1.0994(3) 1.1947(3) 0.61644(13) 0.0350(6) Uani 1 1 d . . .
H20 H 1.1844 1.2518 0.6352 0.042 Uiso 1 1 calc R . .
C21 C 1.0152(3) 1.0930(3) 0.64780(11) 0.0271(5) Uani 1 1 d . . .
H21 H 1.0448 1.0791 0.6874 0.033 Uiso 1 1 calc R . .
C22 C 0.9298(2) 0.8699(2) 0.84985(9) 0.0202(4) Uani 1 1 d . . .
C23 C 0.9153(3) 0.7216(3) 0.84814(10) 0.0273(5) Uani 1 1 d . . .
H23 H 0.8612 0.6654 0.8159 0.033 Uiso 1 1 calc R . .
C24 C 0.9784(3) 0.6541(3) 0.89276(12) 0.0385(6) Uani 1 1 d . . .
H24 H 0.9687 0.5528 0.8906 0.046 Uiso 1 1 calc R . .
C25 C 1.0556(3) 0.7351(4) 0.94037(12) 0.0417(7) Uani 1 1 d . . .
H25 H 1.0982 0.6895 0.9712 0.050 Uiso 1 1 calc R . .
C26 C 1.0705(3) 0.8823(4) 0.94297(11) 0.0382(6) Uani 1 1 d . . .
H26 H 1.1240 0.9377 0.9756 0.046 Uiso 1 1 calc R . .
C27 C 1.0078(3) 0.9506(3) 0.89813(10) 0.0293(5) Uani 1 1 d . . .
H27 H 1.0182 1.0520 0.9005 0.035 Uiso 1 1 calc R . .
C28 C 0.9253(2) 1.1308(2) 0.78767(10) 0.0205(4) Uani 1 1 d . . .
C29 C 1.0761(3) 1.1686(3) 0.79635(11) 0.0276(5) Uani 1 1 d . . .
H29 H 1.1322 1.1018 0.8107 0.033 Uiso 1 1 calc R . .
C30 C 1.1441(3) 1.3042(3) 0.78389(14) 0.0386(7) Uani 1 1 d . . .
H30 H 1.2465 1.3299 0.7904 0.046 Uiso 1 1 calc R . .
C31 C 1.0652(3) 1.4012(3) 0.76230(15) 0.0426(7) Uani 1 1 d . . .
H31 H 1.1127 1.4933 0.7539 0.051 Uiso 1 1 calc R . .
C32 C 0.9152(3) 1.3643(3) 0.75279(14) 0.0378(6) Uani 1 1 d . . .
H32 H 0.8604 1.4309 0.7374 0.045 Uiso 1 1 calc R . .
C33 C 0.8457(3) 1.2302(3) 0.76584(11) 0.0269(5) Uani 1 1 d . . .
H33 H 0.7431 1.2059 0.7598 0.032 Uiso 1 1 calc R . .
C34 C 0.3775(4) 0.9577(4) 0.57802(12) 0.0425(7) Uani 1 1 d . . .
H34A H 0.4301 0.9275 0.5445 0.064 Uiso 1 1 calc R . .
H34B H 0.3178 1.0277 0.5658 0.064 Uiso 1 1 calc R . .
H34C H 0.3149 0.8744 0.5915 0.064 Uiso 1 1 calc R . .
C35 C 0.6142(4) 1.2075(3) 0.61317(13) 0.0388(7) Uani 1 1 d . . .
H35A H 0.7000 1.2414 0.6400 0.058 Uiso 1 1 calc R . .
H35B H 0.5523 1.2813 0.6124 0.058 Uiso 1 1 calc R . .
H35C H 0.6448 1.1874 0.5733 0.058 Uiso 1 1 calc R . .
C36 C 0.4114(3) 1.1000(3) 0.70374(11) 0.0281(5) Uani 1 1 d . . .
H36A H 0.3368 1.0210 0.7133 0.042 Uiso 1 1 calc R . .
H36B H 0.3654 1.1815 0.6935 0.042 Uiso 1 1 calc R . .
H36C H 0.4802 1.1285 0.7381 0.042 Uiso 1 1 calc R . .
C37 C 0.6152(3) 0.9073(3) 0.93656(11) 0.0360(6) Uani 1 1 d . . .
H37A H 0.5330 0.8285 0.9292 0.054 Uiso 1 1 calc R . .
H37B H 0.6068 0.9588 0.9747 0.054 Uiso 1 1 calc R . .
H37C H 0.7062 0.8687 0.9374 0.054 Uiso 1 1 calc R . .
C38 C 0.4296(3) 1.0794(3) 0.86620(12) 0.0321(5) Uani 1 1 d . . .
H38A H 0.4321 1.1566 0.8394 0.048 Uiso 1 1 calc R . .
H38B H 0.3976 1.1110 0.9046 0.048 Uiso 1 1 calc R . .
H38C H 0.3617 0.9953 0.8493 0.048 Uiso 1 1 calc R . .
C39 C 0.7347(3) 1.2039(3) 0.90382(12) 0.0335(6) Uani 1 1 d . . .
H39A H 0.8350 1.1871 0.9093 0.050 Uiso 1 1 calc R . .
H39B H 0.7025 1.2386 0.9417 0.050 Uiso 1 1 calc R . .
H39C H 0.7298 1.2756 0.8749 0.050 Uiso 1 1 calc R . .
C100 C 0.2415(8) 0.3805(8) 0.9498(3) 0.0807(18) Uiso 0.75 1 d P . .
C101 C 0.3106(9) 0.4714(9) 0.9817(4) 0.098(2) Uiso 0.75 1 d P . .
C102 C 0.4273(8) 0.4117(8) 0.9665(3) 0.0523(16) Uiso 0.50 1 d P . .
C103 C 0.5183(8) 0.5321(6) 1.0071(3) 0.0429(14) Uiso 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Lu 0.01209(4) 0.01680(4) 0.01714(4) 0.00100(3) 0.00208(3) -0.00182(3)
P1 0.0143(2) 0.0169(2) 0.0147(2) 0.00074(17) 0.00400(18) 0.00253(18)
P2 0.0103(2) 0.0171(2) 0.0163(2) -0.00124(17) 0.00118(17) 0.00124(18)
Si1 0.0257(3) 0.0274(3) 0.0174(3) 0.0042(2) 0.0037(2) 0.0125(3)
Si2 0.0168(3) 0.0296(3) 0.0173(3) -0.0038(2) 0.0028(2) 0.0055(2)
N1 0.0158(8) 0.0220(8) 0.0171(7) 0.0033(6) 0.0040(6) 0.0051(7)
N2 0.0109(7) 0.0198(8) 0.0159(7) -0.0022(6) 0.0012(6) 0.0010(6)
C1 0.0288(13) 0.0197(11) 0.0545(16) -0.0020(10) 0.0079(12) -0.0003(10)
C2 0.0379(15) 0.0235(11) 0.0372(13) -0.0095(10) 0.0085(11) -0.0096(10)
C3 0.0324(14) 0.0315(13) 0.0332(13) 0.0013(10) -0.0090(11) -0.0122(11)
C4 0.0179(11) 0.0294(13) 0.0567(17) 0.0076(11) -0.0094(11) -0.0053(10)
C5 0.0157(11) 0.0277(12) 0.0648(19) -0.0035(12) 0.0141(12) -0.0028(9)
C6 0.0331(14) 0.0344(13) 0.0364(13) -0.0019(11) 0.0177(11) -0.0123(11)
C7 0.0493(17) 0.0322(13) 0.0278(12) 0.0128(10) 0.0024(11) -0.0143(12)
C8 0.0336(14) 0.0224(12) 0.0530(17) 0.0142(11) -0.0054(12) -0.0028(10)
C9 0.0161(9) 0.0179(9) 0.0166(8) 0.0011(7) 0.0033(7) 0.0039(7)
C10 0.0217(10) 0.0196(9) 0.0185(9) -0.0004(7) 0.0076(8) 0.0014(8)
C11 0.0349(14) 0.0300(12) 0.0293(12) -0.0023(9) 0.0059(10) 0.0143(10)
C12 0.060(2) 0.0313(13) 0.0393(14) 0.0004(11) 0.0188(14) 0.0236(13)
C13 0.0603(19) 0.0235(12) 0.0381(14) -0.0063(10) 0.0276(14) -0.0022(12)
C14 0.0362(15) 0.0469(16) 0.0295(12) -0.0160(11) 0.0122(11) -0.0128(12)
C15 0.0241(12) 0.0406(14) 0.0253(11) -0.0079(10) 0.0058(9) 0.0003(10)
C16 0.0199(10) 0.0199(9) 0.0197(9) 0.0024(7) 0.0095(8) 0.0047(8)
C17 0.0329(13) 0.0330(12) 0.0210(10) 0.0062(9) 0.0076(9) 0.0052(10)
C18 0.0433(16) 0.0387(14) 0.0266(11) 0.0138(10) 0.0169(11) 0.0150(12)
C19 0.0357(14) 0.0287(12) 0.0451(15) 0.0170(11) 0.0238(12) 0.0118(11)
C20 0.0240(12) 0.0342(13) 0.0471(15) 0.0104(11) 0.0126(11) -0.0005(10)
C21 0.0195(11) 0.0329(12) 0.0297(11) 0.0087(9) 0.0079(9) 0.0025(9)
C22 0.0143(9) 0.0288(11) 0.0182(9) -0.0017(8) -0.0001(7) 0.0072(8)
C23 0.0297(12) 0.0297(12) 0.0229(10) 0.0028(9) -0.0034(9) 0.0075(10)
C24 0.0476(17) 0.0402(15) 0.0312(13) 0.0066(11) -0.0039(12) 0.0184(13)
C25 0.0427(17) 0.062(2) 0.0261(12) 0.0061(12) -0.0067(11) 0.0267(15)
C26 0.0305(14) 0.0606(19) 0.0241(11) -0.0064(11) -0.0098(10) 0.0164(13)
C27 0.0242(12) 0.0387(13) 0.0244(11) -0.0066(9) -0.0048(9) 0.0091(10)
C28 0.0150(10) 0.0184(9) 0.0267(10) -0.0041(8) 0.0032(8) -0.0001(8)
C29 0.0149(10) 0.0273(11) 0.0387(13) -0.0047(9) 0.0026(9) -0.0003(9)
C30 0.0202(12) 0.0327(13) 0.0567(17) -0.0083(12) 0.0061(11) -0.0103(10)
C31 0.0354(15) 0.0229(12) 0.0646(19) -0.0023(12) 0.0126(14) -0.0104(11)
C32 0.0343(14) 0.0194(11) 0.0595(18) 0.0043(11) 0.0088(13) 0.0014(10)
C33 0.0192(11) 0.0220(10) 0.0387(13) 0.0011(9) 0.0048(9) 0.0010(8)
C34 0.0478(18) 0.0564(18) 0.0271(12) -0.0002(12) -0.0119(12) 0.0257(15)
C35 0.0555(18) 0.0300(13) 0.0391(14) 0.0147(11) 0.0212(13) 0.0214(13)
C36 0.0260(12) 0.0349(13) 0.0267(11) 0.0028(9) 0.0070(9) 0.0134(10)
C37 0.0398(15) 0.0498(16) 0.0198(10) 0.0056(10) 0.0056(10) 0.0095(13)
C38 0.0212(12) 0.0442(15) 0.0321(12) -0.0074(11) 0.0047(9) 0.0123(10)
C39 0.0279(13) 0.0390(14) 0.0314(12) -0.0165(10) 0.0002(10) 0.0064(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Lu N1 90.16(6) . . ?
N2 Lu C5 105.16(8) . . ?
N1 Lu C5 118.93(9) . . ?
N2 Lu C4 130.93(8) . . ?
N1 Lu C4 95.30(8) . . ?
C5 Lu C4 32.58(10) . . ?
N2 Lu C8 109.43(8) . . ?
N1 Lu C8 145.20(8) . . ?
C5 Lu C8 84.28(10) . . ?
C4 Lu C8 92.92(9) . . ?
N2 Lu C1 136.01(8) . . ?
N1 Lu C1 115.66(8) . . ?
C5 Lu C1 93.03(9) . . ?
C4 Lu C1 83.88(9) . . ?
C8 Lu C1 32.10(10) . . ?
N2 Lu C6 91.51(7) . . ?
N1 Lu C6 149.41(9) . . ?
C5 Lu C6 31.99(10) . . ?
C4 Lu C6 61.37(10) . . ?
C8 Lu C6 61.20(10) . . ?
C1 Lu C6 83.20(9) . . ?
N2 Lu C7 93.24(8) . . ?
N1 Lu C7 176.41(7) . . ?
C5 Lu C7 61.19(11) . . ?
C4 Lu C7 83.33(10) . . ?
C8 Lu C7 31.93(10) . . ?
C1 Lu C7 60.93(10) . . ?
C6 Lu C7 31.71(10) . . ?
N2 Lu C2 166.93(8) . . ?
N1 Lu C2 94.70(8) . . ?
C5 Lu C2 83.07(9) . . ?
C4 Lu C2 60.73(10) . . ?
C8 Lu C2 60.63(10) . . ?
C1 Lu C2 31.66(10) . . ?
C6 Lu C2 90.47(9) . . ?
C7 Lu C2 81.74(9) . . ?
N2 Lu C3 161.48(8) . . ?
N1 Lu C3 86.88(8) . . ?
C5 Lu C3 61.02(10) . . ?
C4 Lu C3 31.64(10) . . ?
C8 Lu C3 82.64(9) . . ?
C1 Lu C3 60.66(10) . . ?
C6 Lu C3 81.97(9) . . ?
C7 Lu C3 90.24(9) . . ?
C2 Lu C3 31.40(10) . . ?
N2 Lu C9 65.37(6) . . ?
N1 Lu C9 63.30(6) . . ?
C5 Lu C9 170.52(8) . . ?
C4 Lu C9 155.13(8) . . ?
C8 Lu C9 98.30(8) . . ?
C1 Lu C9 93.93(8) . . ?
C6 Lu C9 143.13(8) . . ?
C7 Lu C9 117.23(9) . . ?
C2 Lu C9 106.17(8) . . ?
C3 Lu C9 128.27(8) . . ?
N2 Lu P1 85.38(4) . . ?
N1 Lu P1 31.23(5) . . ?
C5 Lu P1 149.63(8) . . ?
C4 Lu P1 121.13(7) . . ?
C8 Lu P1 119.57(7) . . ?
C1 Lu P1 98.81(7) . . ?
C6 Lu P1 176.87(6) . . ?
C7 Lu P1 148.01(8) . . ?
C2 Lu P1 92.49(6) . . ?
C3 Lu P1 101.11(7) . . ?
C9 Lu P1 34.61(4) . . ?
N1 P1 C9 106.57(10) . . ?
N1 P1 C16 113.14(10) . . ?
C9 P1 C16 118.79(11) . . ?
N1 P1 C10 114.10(10) . . ?
C9 P1 C10 104.49(10) . . ?
C16 P1 C10 99.54(9) . . ?
N1 P1 Lu 50.36(7) . . ?
C9 P1 Lu 61.84(7) . . ?
C16 P1 Lu 156.35(7) . . ?
C10 P1 Lu 103.04(7) . . ?
N2 P2 C9 108.68(9) . . ?
N2 P2 C28 110.34(10) . . ?
C9 P2 C28 112.71(10) . . ?
N2 P2 C22 112.27(10) . . ?
C9 P2 C22 105.06(10) . . ?
C28 P2 C22 107.72(11) . . ?
N2 P2 Lu 48.39(6) . . ?
C9 P2 Lu 60.88(7) . . ?
C28 P2 Lu 135.26(8) . . ?
C22 P2 Lu 116.75(8) . . ?
N1 Si1 C34 110.30(12) . . ?
N1 Si1 C35 116.59(12) . . ?
C34 Si1 C35 107.20(15) . . ?
N1 Si1 C36 106.86(10) . . ?
C34 Si1 C36 109.90(14) . . ?
C35 Si1 C36 105.81(12) . . ?
N2 Si2 C38 110.57(10) . . ?
N2 Si2 C37 110.51(11) . . ?
C38 Si2 C37 109.10(13) . . ?
N2 Si2 C39 114.15(10) . . ?
C38 Si2 C39 105.22(13) . . ?
C37 Si2 C39 107.03(14) . . ?
P1 N1 Si1 138.38(12) . . ?
P1 N1 Lu 98.41(9) . . ?
Si1 N1 Lu 121.74(9) . . ?
P2 N2 Si2 124.97(10) . . ?
P2 N2 Lu 100.59(8) . . ?
Si2 N2 Lu 131.45(9) . . ?
C2 C1 C8 134.7(3) . . ?
C2 C1 Lu 75.95(15) . . ?
C8 C1 Lu 73.92(15) . . ?
C1 C2 C3 135.6(2) . . ?
C1 C2 Lu 72.39(14) . . ?
C3 C2 Lu 74.65(14) . . ?
C4 C3 C2 135.1(3) . . ?
C4 C3 Lu 71.96(14) . . ?
C2 C3 Lu 73.94(14) . . ?
C3 C4 C5 134.4(3) . . ?
C3 C4 Lu 76.40(15) . . ?
C5 C4 Lu 73.26(14) . . ?
C6 C5 C4 134.3(3) . . ?
C6 C5 Lu 75.15(15) . . ?
C4 C5 Lu 74.16(15) . . ?
C5 C6 C7 135.8(3) . . ?
C5 C6 Lu 72.86(15) . . ?
C7 C6 Lu 74.88(15) . . ?
C6 C7 C8 134.9(3) . . ?
C6 C7 Lu 73.41(15) . . ?
C8 C7 Lu 72.67(15) . . ?
C1 C8 C7 134.6(3) . . ?
C1 C8 Lu 73.98(15) . . ?
C7 C8 Lu 75.39(15) . . ?
P1 C9 P2 124.92(12) . . ?
P1 C9 Lu 83.55(8) . . ?
P2 C9 Lu 84.50(8) . . ?
C11 C10 C15 118.8(2) . . ?
C11 C10 P1 120.53(18) . . ?
C15 C10 P1 120.51(19) . . ?
C10 C11 C12 120.9(3) . . ?
C13 C12 C11 119.9(3) . . ?
C12 C13 C14 120.1(2) . . ?
C13 C14 C15 120.5(3) . . ?
C10 C15 C14 119.9(3) . . ?
C21 C16 C17 118.8(2) . . ?
C21 C16 P1 123.22(17) . . ?
C17 C16 P1 118.01(18) . . ?
C18 C17 C16 120.6(2) . . ?
C19 C18 C17 119.8(2) . . ?
C20 C19 C18 120.3(2) . . ?
C19 C20 C21 120.2(3) . . ?
C16 C21 C20 120.2(2) . . ?
C23 C22 C27 118.5(2) . . ?
C23 C22 P2 119.04(16) . . ?
C27 C22 P2 122.02(19) . . ?
C24 C23 C22 121.2(2) . . ?
C25 C24 C23 119.7(3) . . ?
C26 C25 C24 119.8(3) . . ?
C25 C26 C27 120.6(2) . . ?
C22 C27 C26 120.0(3) . . ?
C33 C28 C29 118.9(2) . . ?
C33 C28 P2 117.51(17) . . ?
C29 C28 P2 123.10(18) . . ?
C30 C29 C28 119.9(2) . . ?
C31 C30 C29 120.8(2) . . ?
C30 C31 C32 119.8(3) . . ?
C33 C32 C31 120.0(3) . . ?
C32 C33 C28 120.5(2) . . ?
C101 C100 C102 51.5(6) . . ?
C100 C101 C102 86.0(7) . . ?
C100 C101 C103 117.9(7) . 2_667 ?
C102 C101 C103 32.3(4) . 2_667 ?
C100 C101 C103 136.6(8) . . ?
C102 C101 C103 50.7(5) . . ?
C103 C101 C103 19.2(4) 2_667 . ?
C103 C102 C101 90.4(9) 2_667 . ?
C103 C102 C103 9.7(8) 2_667 . ?
C101 C102 C103 86.1(6) . . ?
C103 C102 C100 132.4(9) 2_667 . ?
C101 C102 C100 42.5(5) . . ?
C103 C102 C100 128.6(6) . . ?
C103 C103 C102 158.2(18) 2_667 2_667 ?
C103 C103 C102 12.0(10) 2_667 . ?
C102 C103 C102 170.3(8) 2_667 . ?
C103 C103 C101 111.3(14) 2_667 2_667 ?
C102 C103 C101 57.3(7) 2_667 2_667 ?
C102 C103 C101 118.0(6) . 2_667 ?
C103 C103 C101 49.5(11) 2_667 . ?
C102 C103 C101 140.2(9) 2_667 . ?
C102 C103 C101 43.2(4) . . ?
C101 C103 C101 160.8(4) 2_667 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu N2 2.3340(17) . ?
Lu N1 2.3628(18) . ?
Lu C5 2.525(3) . ?
Lu C4 2.537(3) . ?
Lu C8 2.538(3) . ?
Lu C1 2.539(3) . ?
Lu C6 2.554(2) . ?
Lu C7 2.573(3) . ?
Lu C2 2.584(2) . ?
Lu C3 2.593(2) . ?
Lu C9 2.693(2) . ?
Lu P1 3.0355(7) . ?
P1 N1 1.5912(19) . ?
P1 C9 1.735(2) . ?
P1 C16 1.822(2) . ?
P1 C10 1.823(2) . ?
P2 N2 1.6087(18) . ?
P2 C9 1.751(2) . ?
P2 C28 1.814(2) . ?
P2 C22 1.819(2) . ?
Si1 N1 1.726(2) . ?
Si1 C34 1.866(3) . ?
Si1 C35 1.867(3) . ?
Si1 C36 1.870(2) . ?
Si2 N2 1.7407(17) . ?
Si2 C38 1.859(3) . ?
Si2 C37 1.869(3) . ?
Si2 C39 1.874(3) . ?
C1 C2 1.398(4) . ?
C1 C8 1.404(4) . ?
C2 C3 1.401(4) . ?
C3 C4 1.400(4) . ?
C4 C5 1.420(4) . ?
C5 C6 1.400(4) . ?
C6 C7 1.401(5) . ?
C7 C8 1.406(4) . ?
C10 C11 1.386(3) . ?
C10 C15 1.388(3) . ?
C11 C12 1.393(3) . ?
C12 C13 1.370(5) . ?
C13 C14 1.373(5) . ?
C14 C15 1.400(3) . ?
C16 C21 1.381(3) . ?
C16 C17 1.398(3) . ?
C17 C18 1.385(4) . ?
C18 C19 1.377(4) . ?
C19 C20 1.369(4) . ?
C20 C21 1.397(3) . ?
C22 C23 1.392(3) . ?
C22 C27 1.397(3) . ?
C23 C24 1.390(4) . ?
C24 C25 1.384(4) . ?
C25 C26 1.379(5) . ?
C26 C27 1.396(4) . ?
C28 C33 1.394(3) . ?
C28 C29 1.398(3) . ?
C29 C30 1.393(4) . ?
C30 C31 1.370(5) . ?
C31 C32 1.391(4) . ?
C32 C33 1.390(3) . ?
C100 C101 1.173(10) . ?
C100 C102 1.732(10) . ?
C101 C102 1.359(11) . ?
C101 C103 1.614(11) 2_667 ?
C101 C103 1.979(11) . ?
C102 C103 0.862(8) 2_667 ?
C102 C103 1.535(10) . ?
C103 C103 0.700(11) 2_667 ?
C103 C102 0.862(8) 2_667 ?
C103 C101 1.614(11) 2_667 ?
|
1100887.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-17 01:36:00 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100887.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100887
loop_
_publ_author_name
'Cuffe, Laurence'
'Hudson, Richard D. A.'
'Gallagher, John F.'
'Jennings, Sarah'
'McAdam, C. John'
'Connelly, Rosamond B. T.'
'Manning, Anthony R.'
'Robinson, Brian. H.'
'Simpson, Jim'
_publ_section_title
;
Synthesis, Structure, and Redox Chemistry of Ethenyl and Ethynyl
Ferrocene Polyaromatic Dyads
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2051
_journal_page_last 2060
_journal_paper_doi 10.1021/om0492653
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C26 H18 Fe'
_chemical_formula_sum 'C26 H18 Fe'
_chemical_formula_weight 386.25
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 91.824(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 7.265(3)
_cell_length_b 11.059(4)
_cell_length_c 22.303(8)
_cell_measurement_reflns_used 4049
_cell_measurement_temperature 168(2)
_cell_measurement_theta_max 52.67
_cell_measurement_theta_min 5.19
_cell_volume 1791.2(10)
_exptl_absorpt_coefficient_mu 0.849
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82274
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Bruker 1997)'
_exptl_crystal_colour gold
_exptl_crystal_density_diffrn 1.432
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 800
_exptl_crystal_size_max 0.64
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.10
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.919
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 2421
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.919
_refine_ls_R_factor_all 0.0608
_refine_ls_R_factor_gt 0.0423
_refine_ls_shift/su_max '< 0.001'
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1010
_refine_ls_wR_factor_ref 0.1075
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100887
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2723(6) 0.2970(3) 0.4328(2) 0.0407(11) Uani 1 1 d . . .
H1 H 0.3347 0.3142 0.3970 0.049 Uiso 1 1 calc R . .
C2 C 0.1966(5) 0.3828(3) 0.47256(19) 0.0396(12) Uani 1 1 d . . .
H2 H 0.2004 0.4682 0.4681 0.048 Uiso 1 1 calc R . .
C3 C 0.1150(6) 0.3195(4) 0.51956(19) 0.0420(12) Uani 1 1 d . . .
H3 H 0.0533 0.3551 0.5521 0.050 Uiso 1 1 calc R . .
C4 C 0.1399(6) 0.1949(3) 0.5104(2) 0.0454(12) Uani 1 1 d . . .
H4 H 0.0990 0.1316 0.5355 0.054 Uiso 1 1 calc R . .
C5 C 0.2372(6) 0.1814(3) 0.4568(2) 0.0416(12) Uani 1 1 d . . .
H5 H 0.2731 0.1067 0.4398 0.050 Uiso 1 1 calc R . .
Fe1 Fe -0.00455(8) 0.26907(4) 0.43972(2) 0.0273(2) Uani 1 1 d . . .
C6 C -0.1156(5) 0.2745(3) 0.35494(19) 0.0341(11) Uani 1 1 d . . .
H6 H -0.0487 0.2825 0.3193 0.041 Uiso 1 1 calc R . .
C7 C -0.1871(5) 0.3703(3) 0.38925(18) 0.0363(11) Uani 1 1 d . . .
H7 H -0.1776 0.4540 0.3802 0.044 Uiso 1 1 calc R . .
C8 C -0.2760(5) 0.3202(3) 0.43983(19) 0.0377(11) Uani 1 1 d . . .
H8 H -0.3346 0.3643 0.4704 0.045 Uiso 1 1 calc R . .
C9 C -0.2608(5) 0.1918(3) 0.43610(18) 0.0319(10) Uani 1 1 d . . .
H9 H -0.3080 0.1352 0.4637 0.038 Uiso 1 1 calc R . .
C10 C -0.1624(5) 0.1633(3) 0.38368(16) 0.0269(9) Uani 1 1 d . . .
C11 C -0.1180(5) 0.0438(3) 0.36367(16) 0.0255(9) Uani 1 1 d . . .
C12 C -0.0861(5) -0.0563(3) 0.34715(15) 0.0265(9) Uani 1 1 d . . .
C13 C -0.0448(5) -0.1770(3) 0.32758(16) 0.0253(9) Uani 1 1 d . . .
C14 C -0.1726(6) -0.2395(2) 0.29009(17) 0.0273(10) Uani 1 1 d . . .
C15 C -0.3380(5) -0.1848(3) 0.26719(17) 0.0319(10) Uani 1 1 d . . .
H15 H -0.3653 -0.1038 0.2780 0.038 Uiso 1 1 calc R . .
C16 C -0.4571(6) -0.2459(3) 0.23038(19) 0.0396(12) Uani 1 1 d . . .
H16 H -0.5661 -0.2073 0.2155 0.048 Uiso 1 1 calc R . .
C17 C -0.4202(6) -0.3670(3) 0.21382(18) 0.0407(11) Uani 1 1 d . . .
H17 H -0.5043 -0.4091 0.1879 0.049 Uiso 1 1 calc R . .
C18 C -0.2643(6) -0.4231(3) 0.23506(17) 0.0364(11) Uani 1 1 d . . .
H18 H -0.2420 -0.5047 0.2242 0.044 Uiso 1 1 calc R . .
C19 C -0.1339(5) -0.3617(3) 0.27334(16) 0.0304(10) Uani 1 1 d . . .
C20 C 0.0302(5) -0.4155(3) 0.29370(16) 0.0309(10) Uani 1 1 d . . .
H20 H 0.0544 -0.4967 0.2826 0.037 Uiso 1 1 calc R . .
C21 C 0.1601(5) -0.3544(3) 0.32979(16) 0.0283(10) Uani 1 1 d . . .
C22 C 0.3287(6) -0.4091(3) 0.35039(17) 0.0365(11) Uani 1 1 d . . .
H22 H 0.3552 -0.4899 0.3390 0.044 Uiso 1 1 calc R . .
C23 C 0.4505(6) -0.3482(3) 0.38564(18) 0.0423(11) Uani 1 1 d . . .
H23 H 0.5612 -0.3867 0.3991 0.051 Uiso 1 1 calc R . .
C24 C 0.4152(6) -0.2277(3) 0.4028(2) 0.0444(12) Uani 1 1 d . . .
H24 H 0.5028 -0.1853 0.4274 0.053 Uiso 1 1 calc R . .
C25 C 0.2569(6) -0.1723(3) 0.38452(17) 0.0359(11) Uani 1 1 d . . .
H25 H 0.2349 -0.0915 0.3968 0.043 Uiso 1 1 calc R . .
C26 C 0.1232(5) -0.2318(3) 0.34743(16) 0.0266(10) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.015(3) 0.058(2) 0.048(3) 0.0003(18) -0.005(2) -0.0053(17)
C2 0.024(3) 0.042(2) 0.052(3) -0.0106(18) -0.010(2) -0.0064(16)
C3 0.029(3) 0.062(2) 0.034(3) -0.0122(19) -0.005(2) -0.0011(19)
C4 0.038(3) 0.053(2) 0.044(3) 0.0118(18) -0.017(3) -0.0071(18)
C5 0.024(3) 0.045(2) 0.054(3) -0.0096(18) -0.013(3) 0.0079(17)
Fe1 0.0199(4) 0.0279(2) 0.0338(4) -0.0050(2) -0.0039(3) 0.0000(2)
C6 0.028(3) 0.0322(17) 0.041(3) -0.0028(15) -0.012(2) 0.0038(15)
C7 0.031(3) 0.0289(17) 0.048(3) -0.0056(16) -0.013(2) 0.0043(15)
C8 0.017(3) 0.0389(19) 0.057(3) -0.0213(18) -0.005(2) 0.0039(15)
C9 0.020(3) 0.0380(18) 0.038(3) -0.0070(15) -0.001(2) -0.0029(15)
C10 0.020(3) 0.0280(17) 0.033(3) -0.0027(14) -0.010(2) 0.0017(13)
C11 0.017(2) 0.0294(17) 0.030(2) -0.0006(13) -0.0053(19) -0.0019(13)
C12 0.023(3) 0.0285(17) 0.028(2) 0.0024(13) -0.0049(19) -0.0009(13)
C13 0.025(3) 0.0240(15) 0.027(2) -0.0020(13) 0.0031(19) -0.0008(14)
C14 0.029(3) 0.0220(16) 0.031(3) 0.0038(13) 0.007(2) -0.0046(13)
C15 0.029(3) 0.0307(16) 0.036(3) 0.0025(15) -0.006(2) 0.0023(15)
C16 0.030(3) 0.046(2) 0.042(3) 0.0075(16) -0.011(2) -0.0052(16)
C17 0.038(3) 0.045(2) 0.038(3) -0.0020(16) -0.007(2) -0.0165(18)
C18 0.042(3) 0.0302(17) 0.037(3) -0.0048(15) 0.002(2) -0.0087(16)
C19 0.035(3) 0.0263(16) 0.030(3) -0.0001(13) 0.006(2) -0.0055(15)
C20 0.039(3) 0.0207(15) 0.034(3) 0.0019(13) 0.003(2) 0.0033(15)
C21 0.035(3) 0.0272(16) 0.023(2) 0.0047(13) 0.004(2) 0.0029(15)
C22 0.039(3) 0.0322(18) 0.038(3) 0.0033(15) 0.004(2) 0.0087(16)
C23 0.031(3) 0.056(2) 0.039(3) 0.0049(18) 0.000(2) 0.0151(19)
C24 0.033(3) 0.055(2) 0.044(3) -0.0053(18) -0.010(2) 0.0011(19)
C25 0.035(3) 0.0374(19) 0.035(3) -0.0026(16) -0.005(2) 0.0025(16)
C26 0.030(3) 0.0268(15) 0.024(2) 0.0041(13) 0.002(2) -0.0011(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100888.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-17 01:36:00 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100888.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100888
loop_
_publ_author_name
'Cuffe, Laurence'
'Hudson, Richard D. A.'
'Gallagher, John F.'
'Jennings, Sarah'
'McAdam, C. John'
'Connelly, Rosamond B. T.'
'Manning, Anthony R.'
'Robinson, Brian. H.'
'Simpson, Jim'
_publ_section_title
;
Synthesis, Structure, and Redox Chemistry of Ethenyl and Ethynyl
Ferrocene Polyaromatic Dyads
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2051
_journal_page_last 2060
_journal_paper_doi 10.1021/om0492653
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C28 H18 Fe'
_chemical_formula_sum 'C28 H18 Fe'
_chemical_formula_weight 410.27
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 107.540(6)
_cell_angle_beta 101.733(7)
_cell_angle_gamma 100.521(6)
_cell_formula_units_Z 2
_cell_length_a 7.810(5)
_cell_length_b 9.956(6)
_cell_length_c 13.205(8)
_cell_measurement_reflns_used 4181
_cell_measurement_temperature 163(2)
_cell_measurement_theta_max 26.128
_cell_measurement_theta_min 2.759
_cell_volume 925.4(10)
_diffrn_ambient_temperature 163(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0463
_diffrn_reflns_av_sigmaI/netI 0.0541
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 11682
_diffrn_reflns_theta_max 26.41
_diffrn_reflns_theta_min 2.22
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.826
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.747516
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS Bruker 1999'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.472
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 424
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.11
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.966
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 262
_refine_ls_number_reflns 3719
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.966
_refine_ls_R_factor_all 0.0515
_refine_ls_R_factor_gt 0.0374
_refine_ls_shift/su_max '< 0.001'
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0894
_refine_ls_wR_factor_ref 0.0930
_reflns_number_gt 2932
_reflns_number_total 3719
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100888
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1980(3) 0.0861(3) 0.3521(2) 0.0340(6) Uani 1 1 d . . .
H1 H 0.1635 0.0377 0.3997 0.041 Uiso 1 1 calc R . .
C2 C 0.1999(3) 0.2331(3) 0.3627(2) 0.0328(6) Uani 1 1 d . . .
H2 H 0.1670 0.3003 0.4187 0.039 Uiso 1 1 calc R . .
C3 C 0.2595(3) 0.2613(3) 0.2749(2) 0.0298(6) Uani 1 1 d . . .
H3 H 0.2736 0.3510 0.2620 0.036 Uiso 1 1 calc R . .
C4 C 0.2943(3) 0.1333(3) 0.2099(2) 0.0275(6) Uani 1 1 d . . .
H4 H 0.3355 0.1220 0.1456 0.033 Uiso 1 1 calc R . .
C5 C 0.2571(3) 0.0247(3) 0.2575(2) 0.0282(6) Uani 1 1 d . . .
H5 H 0.2694 -0.0719 0.2308 0.034 Uiso 1 1 calc R . .
Fe1 Fe 0.45496(4) 0.20244(3) 0.36941(3) 0.02010(12) Uani 1 1 d . . .
C6 C 0.6214(3) 0.1998(3) 0.51043(19) 0.0234(5) Uani 1 1 d . . .
H6 H 0.5857 0.1541 0.5592 0.028 Uiso 1 1 calc R . .
C7 C 0.6244(3) 0.3460(3) 0.5174(2) 0.0267(6) Uani 1 1 d . . .
H7 H 0.5901 0.4146 0.5717 0.032 Uiso 1 1 calc R . .
C8 C 0.6871(3) 0.3719(3) 0.4296(2) 0.0285(6) Uani 1 1 d . . .
H8 H 0.7032 0.4610 0.4158 0.034 Uiso 1 1 calc R . .
C9 C 0.7216(3) 0.2420(2) 0.3660(2) 0.0248(5) Uani 1 1 d . . .
H9 H 0.7632 0.2286 0.3018 0.030 Uiso 1 1 calc R . .
C10 C 0.6823(3) 0.1340(2) 0.41594(18) 0.0205(5) Uani 1 1 d . . .
C11 C 0.6986(3) -0.0135(3) 0.37773(18) 0.0214(5) Uani 1 1 d . . .
C12 C 0.7138(3) -0.1352(3) 0.34459(19) 0.0228(5) Uani 1 1 d . . .
C13 C 0.7384(3) -0.2790(2) 0.29776(19) 0.0222(5) Uani 1 1 d . . .
C14 C 0.9100(3) -0.3035(3) 0.3270(2) 0.0262(5) Uani 1 1 d . . .
H14 H 1.0042 -0.2291 0.3847 0.031 Uiso 1 1 calc R . .
C15 C 0.9443(3) -0.4337(3) 0.2736(2) 0.0255(5) Uani 1 1 d . . .
H15 H 1.0612 -0.4480 0.2957 0.031 Uiso 1 1 calc R . .
C16 C 0.8086(3) -0.5458(2) 0.18692(19) 0.0212(5) Uani 1 1 d . . .
C17 C 0.8432(3) -0.6796(2) 0.1249(2) 0.0243(5) Uani 1 1 d . . .
H17 H 0.9607 -0.6942 0.1432 0.029 Uiso 1 1 calc R . .
C18 C 0.7113(3) -0.7840(2) 0.04151(19) 0.0246(5) Uani 1 1 d . . .
H18 H 0.7394 -0.8695 0.0008 0.029 Uiso 1 1 calc R . .
C19 C 0.5286(3) -0.7703(2) 0.01194(19) 0.0210(5) Uani 1 1 d . . .
C20 C 0.3895(3) -0.8791(3) -0.0730(2) 0.0261(5) Uani 1 1 d . . .
H20 H 0.4150 -0.9654 -0.1147 0.031 Uiso 1 1 calc R . .
C21 C 0.2134(3) -0.8627(3) -0.0976(2) 0.0287(6) Uani 1 1 d . . .
H21 H 0.1199 -0.9393 -0.1541 0.034 Uiso 1 1 calc R . .
C22 C 0.1739(3) -0.7369(3) -0.0410(2) 0.0262(5) Uani 1 1 d . . .
H22 H 0.0538 -0.7270 -0.0591 0.031 Uiso 1 1 calc R . .
C23 C 0.3108(3) -0.6221(2) 0.04419(18) 0.0212(5) Uani 1 1 d . . .
C24 C 0.2769(3) -0.4877(3) 0.10440(19) 0.0235(5) Uani 1 1 d . . .
H24 H 0.1581 -0.4750 0.0876 0.028 Uiso 1 1 calc R . .
C25 C 0.4114(3) -0.3786(3) 0.18487(19) 0.0227(5) Uani 1 1 d . . .
H25 H 0.3847 -0.2905 0.2221 0.027 Uiso 1 1 calc R . .
C26 C 0.5935(3) -0.3928(2) 0.21538(18) 0.0193(5) Uani 1 1 d . . .
C27 C 0.6308(3) -0.5261(2) 0.15896(18) 0.0191(5) Uani 1 1 d . . .
C28 C 0.4892(3) -0.6400(2) 0.07191(18) 0.0198(5) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0192(13) 0.0449(16) 0.0314(14) 0.0163(13) -0.0005(11) -0.0038(11)
C2 0.0224(13) 0.0393(16) 0.0285(14) 0.0015(12) 0.0030(11) 0.0108(11)
C3 0.0275(14) 0.0275(13) 0.0313(14) 0.0098(11) -0.0017(11) 0.0118(11)
C4 0.0285(14) 0.0285(13) 0.0198(12) 0.0044(10) 0.0020(10) 0.0060(11)
C5 0.0215(13) 0.0232(13) 0.0307(14) 0.0053(11) -0.0035(11) 0.0029(10)
Fe1 0.01817(19) 0.01909(19) 0.02013(18) 0.00495(13) 0.00273(13) 0.00404(13)
C6 0.0175(12) 0.0282(13) 0.0208(12) 0.0069(10) 0.0011(9) 0.0044(10)
C7 0.0218(13) 0.0232(13) 0.0252(12) -0.0038(10) 0.0037(10) 0.0061(10)
C8 0.0234(13) 0.0183(12) 0.0374(15) 0.0073(11) 0.0022(11) 0.0010(10)
C9 0.0193(12) 0.0241(13) 0.0297(13) 0.0097(11) 0.0070(10) 0.0017(10)
C10 0.0165(11) 0.0205(12) 0.0194(11) 0.0035(9) 0.0012(9) 0.0028(9)
C11 0.0180(12) 0.0262(13) 0.0183(11) 0.0083(10) 0.0023(9) 0.0037(10)
C12 0.0214(12) 0.0241(13) 0.0220(12) 0.0093(10) 0.0049(10) 0.0027(10)
C13 0.0261(13) 0.0202(12) 0.0210(12) 0.0078(10) 0.0074(10) 0.0060(10)
C14 0.0227(13) 0.0252(13) 0.0255(12) 0.0076(10) 0.0009(10) 0.0026(10)
C15 0.0183(12) 0.0279(13) 0.0297(13) 0.0106(11) 0.0037(10) 0.0073(10)
C16 0.0206(12) 0.0225(12) 0.0240(12) 0.0122(10) 0.0066(10) 0.0064(10)
C17 0.0230(13) 0.0278(13) 0.0309(13) 0.0152(11) 0.0122(11) 0.0137(10)
C18 0.0316(14) 0.0197(12) 0.0283(13) 0.0101(10) 0.0146(11) 0.0108(10)
C19 0.0226(12) 0.0216(12) 0.0215(12) 0.0104(10) 0.0086(10) 0.0047(10)
C20 0.0331(14) 0.0205(12) 0.0245(12) 0.0076(10) 0.0109(11) 0.0038(10)
C21 0.0292(14) 0.0263(13) 0.0227(12) 0.0069(10) 0.0024(11) -0.0032(11)
C22 0.0183(12) 0.0329(14) 0.0278(13) 0.0154(11) 0.0039(10) 0.0023(10)
C23 0.0215(12) 0.0257(12) 0.0201(11) 0.0130(10) 0.0079(10) 0.0043(10)
C24 0.0190(12) 0.0285(13) 0.0286(13) 0.0154(11) 0.0075(10) 0.0094(10)
C25 0.0246(13) 0.0238(12) 0.0251(12) 0.0118(10) 0.0102(10) 0.0102(10)
C26 0.0193(12) 0.0221(12) 0.0204(11) 0.0114(10) 0.0072(9) 0.0062(9)
C27 0.0197(12) 0.0209(12) 0.0198(11) 0.0105(9) 0.0067(9) 0.0053(9)
C28 0.0186(12) 0.0229(12) 0.0202(11) 0.0119(10) 0.0057(9) 0.0032(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100889.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-17 01:36:00 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100889.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100889
loop_
_publ_author_name
'Cuffe, Laurence'
'Hudson, Richard D. A.'
'Gallagher, John F.'
'Jennings, Sarah'
'McAdam, C. John'
'Connelly, Rosamond B. T.'
'Manning, Anthony R.'
'Robinson, Brian. H.'
'Simpson, Jim'
_publ_section_title
;
Synthesis, Structure, and Redox Chemistry of Ethenyl and Ethynyl
Ferrocene Polyaromatic Dyads
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2051
_journal_page_last 2060
_journal_paper_doi 10.1021/om0492653
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C32 H20 Fe'
_chemical_formula_sum 'C32 H20 Fe'
_chemical_formula_weight 460.33
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 99.609(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.421(1)
_cell_length_b 10.868(1)
_cell_length_c 17.2066(16)
_cell_measurement_reflns_used 7089
_cell_measurement_temperature 158(2)
_cell_measurement_theta_max 26.41
_cell_measurement_theta_min 2.75
_cell_volume 2105.8(3)
_diffrn_ambient_temperature 158(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0233
_diffrn_reflns_av_sigmaI/netI 0.0257
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 14350
_diffrn_reflns_theta_max 26.41
_diffrn_reflns_theta_min 2.75
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.735
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.722976
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS Bruker 1997'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.452
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 952
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.38
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 298
_refine_ls_number_reflns 4127
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0891
_refine_ls_R_factor_gt 0.0754
_refine_ls_shift/su_max '< 0.001'
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+4.4913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2192
_refine_ls_wR_factor_ref 0.2279
_reflns_number_gt 3284
_reflns_number_total 4127
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1100889
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6204(8) 0.4384(7) 0.2668(4) 0.085(2) Uani 1 1 d . . .
H1 H 0.6942 0.4159 0.2978 0.102 Uiso 1 1 calc R . .
C2 C 0.5460(7) 0.5297(7) 0.2847(4) 0.079(2) Uani 1 1 d . . .
H2 H 0.5594 0.5805 0.3302 0.095 Uiso 1 1 calc R . .
C3 C 0.4486(6) 0.5353(8) 0.2255(5) 0.092(2) Uani 1 1 d . . .
H3 H 0.3840 0.5909 0.2233 0.110 Uiso 1 1 calc R . .
C4 C 0.4609(7) 0.4453(8) 0.1691(5) 0.096(3) Uani 1 1 d . . .
H4 H 0.4061 0.4291 0.1223 0.115 Uiso 1 1 calc R . .
C5 C 0.5682(8) 0.3832(7) 0.1940(4) 0.091(2) Uani 1 1 d . . .
H5 H 0.5999 0.3174 0.1677 0.109 Uiso 1 1 calc R . .
Fe1 Fe 0.59609(6) 0.56551(7) 0.17901(4) 0.0498(3) Uani 1 1 d . . .
C6 C 0.7579(5) 0.6351(6) 0.1678(3) 0.0640(15) Uani 1 1 d . . .
H6 H 0.8324 0.6116 0.1973 0.077 Uiso 1 1 calc R . .
C7 C 0.6832(7) 0.7297(6) 0.1870(4) 0.078(2) Uani 1 1 d . . .
H7 H 0.6988 0.7814 0.2321 0.094 Uiso 1 1 calc R . .
C8 C 0.5833(7) 0.7345(6) 0.1290(4) 0.0751(18) Uani 1 1 d . . .
H8 H 0.5190 0.7903 0.1276 0.090 Uiso 1 1 calc R . .
C9 C 0.5927(5) 0.6437(5) 0.0728(3) 0.0628(14) Uani 1 1 d . . .
H9 H 0.5359 0.6271 0.0270 0.075 Uiso 1 1 calc R . .
C10 C 0.7007(5) 0.5810(5) 0.0956(3) 0.0550(12) Uani 1 1 d . . .
C11 C 0.7468(5) 0.4812(5) 0.0549(3) 0.0625(13) Uani 1 1 d . . .
C12 C 0.7882(5) 0.3976(6) 0.0207(3) 0.0658(14) Uani 1 1 d . . .
C13 C 0.8345(4) 0.2956(5) -0.0165(3) 0.0525(11) Uani 1 1 d . . .
C14 C 0.9304(5) 0.3119(5) -0.0544(3) 0.0543(12) Uani 1 1 d . . .
H14 H 0.9639 0.3917 -0.0560 0.065 Uiso 1 1 calc R . .
C15 C 0.9791(5) 0.2155(5) -0.0900(3) 0.0558(12) Uani 1 1 d . . .
H15 H 1.0449 0.2309 -0.1158 0.067 Uiso 1 1 calc R . .
C16 C 0.9346(4) 0.0954(4) -0.0895(3) 0.0439(10) Uani 1 1 d . . .
C17 C 0.9877(4) -0.0081(5) -0.1270(3) 0.0459(10) Uani 1 1 d . . .
C18 C 1.0831(5) 0.0064(6) -0.1661(3) 0.0605(13) Uani 1 1 d . . .
H18 H 1.1173 0.0856 -0.1688 0.073 Uiso 1 1 calc R . .
C19 C 1.1298(5) -0.0929(7) -0.2015(4) 0.0731(17) Uani 1 1 d . . .
H19 H 1.1939 -0.0790 -0.2292 0.088 Uiso 1 1 calc R . .
C20 C 1.0875(5) -0.2085(6) -0.1982(3) 0.0636(14) Uani 1 1 d . . .
H20 H 1.1226 -0.2748 -0.2221 0.076 Uiso 1 1 calc R . .
C21 C 0.9894(4) -0.2299(5) -0.1584(3) 0.0521(12) Uani 1 1 d . . .
C22 C 0.9423(5) -0.3491(5) -0.1527(3) 0.0615(14) Uani 1 1 d . . .
H22 H 0.9771 -0.4173 -0.1749 0.074 Uiso 1 1 calc R . .
C23 C 0.8476(5) -0.3666(5) -0.1157(4) 0.0651(15) Uani 1 1 d . . .
H23 H 0.8153 -0.4468 -0.1134 0.078 Uiso 1 1 calc R . .
C24 C 0.7968(4) -0.2675(5) -0.0809(3) 0.0564(12) Uani 1 1 d . . .
H24 H 0.7309 -0.2823 -0.0550 0.068 Uiso 1 1 calc R . .
C25 C 0.8403(4) -0.1484(4) -0.0833(3) 0.0432(10) Uani 1 1 d . . .
C26 C 0.7888(4) -0.0452(4) -0.0455(3) 0.0444(10) Uani 1 1 d . . .
C27 C 0.6958(5) -0.0626(5) -0.0046(3) 0.0594(13) Uani 1 1 d . . .
H27 H 0.6644 -0.1430 -0.0012 0.071 Uiso 1 1 calc R . .
C28 C 0.6470(5) 0.0348(6) 0.0320(4) 0.0664(15) Uani 1 1 d . . .
H28 H 0.5844 0.0196 0.0609 0.080 Uiso 1 1 calc R . .
C29 C 0.6888(4) 0.1531(5) 0.0267(3) 0.0576(13) Uani 1 1 d . . .
H29 H 0.6531 0.2196 0.0499 0.069 Uiso 1 1 calc R . .
C30 C 0.7853(4) 0.1746(5) -0.0138(3) 0.0473(10) Uani 1 1 d . . .
C31 C 0.8366(4) 0.0753(4) -0.0502(3) 0.0428(10) Uani 1 1 d . . .
C32 C 0.9389(4) -0.1281(4) -0.1233(2) 0.0427(10) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.113(6) 0.085(5) 0.057(4) 0.010(3) 0.015(4) -0.029(4)
C2 0.091(5) 0.105(5) 0.048(3) -0.014(3) 0.031(3) -0.039(4)
C3 0.065(4) 0.131(6) 0.091(5) -0.024(5) 0.047(4) -0.034(4)
C4 0.081(5) 0.133(7) 0.078(4) -0.034(4) 0.031(4) -0.072(5)
C5 0.128(7) 0.073(4) 0.083(5) -0.013(4) 0.048(5) -0.050(4)
Fe1 0.0527(4) 0.0598(5) 0.0397(4) -0.0109(3) 0.0159(3) -0.0186(3)
C6 0.063(3) 0.074(4) 0.060(3) -0.011(3) 0.025(3) -0.028(3)
C7 0.106(5) 0.068(4) 0.072(4) -0.022(3) 0.047(4) -0.042(4)
C8 0.097(5) 0.059(3) 0.079(4) 0.000(3) 0.045(4) 0.007(3)
C9 0.075(4) 0.069(3) 0.049(3) 0.005(3) 0.026(3) 0.008(3)
C10 0.066(3) 0.054(3) 0.050(3) 0.001(2) 0.026(2) -0.008(2)
C11 0.074(4) 0.060(3) 0.056(3) -0.001(3) 0.016(3) -0.002(3)
C12 0.071(4) 0.069(3) 0.056(3) -0.002(3) 0.009(3) 0.003(3)
C13 0.056(3) 0.053(3) 0.045(3) -0.002(2) 0.000(2) 0.007(2)
C14 0.061(3) 0.044(3) 0.057(3) 0.007(2) 0.009(2) -0.005(2)
C15 0.055(3) 0.058(3) 0.056(3) 0.005(2) 0.012(2) -0.004(2)
C16 0.046(2) 0.046(2) 0.036(2) 0.0046(18) -0.0034(18) -0.0035(19)
C17 0.040(2) 0.060(3) 0.036(2) 0.008(2) 0.0011(17) 0.003(2)
C18 0.057(3) 0.071(4) 0.056(3) 0.015(3) 0.016(2) 0.002(3)
C19 0.058(3) 0.103(5) 0.064(4) 0.014(3) 0.025(3) 0.021(3)
C20 0.062(3) 0.075(4) 0.053(3) 0.001(3) 0.011(2) 0.021(3)
C21 0.046(2) 0.067(3) 0.039(2) -0.005(2) -0.0017(19) 0.012(2)
C22 0.059(3) 0.059(3) 0.060(3) -0.018(3) -0.006(2) 0.014(2)
C23 0.064(3) 0.049(3) 0.076(4) -0.010(3) -0.006(3) -0.005(2)
C24 0.048(3) 0.057(3) 0.063(3) -0.004(2) 0.005(2) -0.012(2)
C25 0.038(2) 0.051(3) 0.039(2) -0.0050(19) 0.0006(17) -0.0006(18)
C26 0.040(2) 0.052(3) 0.038(2) -0.0051(19) -0.0012(18) -0.0054(18)
C27 0.053(3) 0.065(3) 0.063(3) -0.015(3) 0.018(2) -0.014(2)
C28 0.049(3) 0.085(4) 0.070(4) -0.017(3) 0.023(3) -0.014(3)
C29 0.046(3) 0.070(3) 0.057(3) -0.014(3) 0.009(2) 0.004(2)
C30 0.044(2) 0.055(3) 0.039(2) -0.003(2) -0.0028(18) -0.002(2)
C31 0.037(2) 0.053(3) 0.035(2) -0.0020(19) -0.0034(17) 0.0025(19)
C32 0.039(2) 0.055(3) 0.031(2) 0.0001(18) -0.0032(16) 0.0019(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100890.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-17 01:36:00 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100890.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100890
loop_
_publ_author_name
'Cuffe, Laurence'
'Hudson, Richard D. A.'
'Gallagher, John F.'
'Jennings, Sarah'
'McAdam, C. John'
'Connelly, Rosamond B. T.'
'Manning, Anthony R.'
'Robinson, Brian. H.'
'Simpson, Jim'
_publ_section_title
;
Synthesis, Structure, and Redox Chemistry of Ethenyl and Ethynyl
Ferrocene Polyaromatic Dyads
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2051
_journal_page_last 2060
_journal_paper_doi 10.1021/om0492653
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C26 H20 Fe'
_chemical_formula_sum 'C26 H20 Fe'
_chemical_formula_weight 388.27
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 101.449(5)
_cell_angle_beta 100.901(4)
_cell_angle_gamma 95.453(5)
_cell_formula_units_Z 2
_cell_length_a 7.7278(4)
_cell_length_b 10.5188(9)
_cell_length_c 12.0885(8)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 294(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 936.69(11)
_diffrn_ambient_temperature 294(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0142
_diffrn_reflns_av_sigmaI/netI 0.0219
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 5507
_diffrn_reflns_theta_max 28.10
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.812
_exptl_absorpt_correction_T_max 0.8879
_exptl_absorpt_correction_T_min 0.7372
_exptl_absorpt_correction_type ?
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 404
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.15
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.613
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 295
_refine_ls_number_reflns 4528
_refine_ls_number_restraints 80
_refine_ls_restrained_S_all 0.607
_refine_ls_R_factor_all 0.0436
_refine_ls_R_factor_gt 0.0345
_refine_ls_shift/su_max 0.045
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+1.1862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0905
_refine_ls_wR_factor_ref 0.1033
_reflns_number_gt 3841
_reflns_number_total 4528
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.0587(3) 0.16573(18) 0.94447(16) 0.0459(4) Uani 1 1 d . . .
H11 H 0.035(3) 0.136(2) 0.994(2) 0.060(6) Uiso 1 1 d . . .
C12 C -0.1588(3) 0.24284(19) 0.99632(17) 0.0471(4) Uani 1 1 d . . .
H12 H -0.252(3) 0.273(2) 0.950(2) 0.064(7) Uiso 1 1 d . . .
C13 C -0.1327(2) 0.28406(17) 1.12377(16) 0.0425(4) Uani 1 1 d . . .
C14 C -0.2690(2) 0.24532(16) 1.17799(16) 0.0417(4) Uani 1 1 d . . .
C15 C -0.4334(3) 0.1689(2) 1.11467(19) 0.0516(4) Uani 1 1 d . . .
H15 H -0.4533 0.1444 1.0346 0.062 Uiso 1 1 calc R . .
C16 C -0.5612(3) 0.1314(2) 1.1692(2) 0.0607(5) Uani 1 1 d . . .
H16 H -0.6677 0.0826 1.1260 0.073 Uiso 1 1 calc R . .
C17 C -0.5347(3) 0.1655(2) 1.2905(2) 0.0624(5) Uani 1 1 d . . .
H17 H -0.6238 0.1396 1.3267 0.075 Uiso 1 1 calc R . .
C18 C -0.3801(3) 0.2357(2) 1.35433(19) 0.0553(5) Uani 1 1 d . . .
H18 H -0.3641 0.2575 1.4343 0.066 Uiso 1 1 calc R . .
C19 C -0.2409(2) 0.27716(17) 1.30154(16) 0.0444(4) Uani 1 1 d . . .
C20 C -0.0781(3) 0.34467(18) 1.36639(17) 0.0478(4) Uani 1 1 d . . .
H20 H -0.0592 0.3630 1.4466 0.057 Uiso 1 1 calc R . .
C21 C 0.0568(2) 0.38539(18) 1.31481(17) 0.0464(4) Uani 1 1 d . . .
C22 C 0.2229(3) 0.4566(2) 1.3815(2) 0.0574(5) Uani 1 1 d . . .
H22 H 0.2435 0.4730 1.4617 0.069 Uiso 1 1 calc R . .
C23 C 0.3500(3) 0.5002(2) 1.3306(2) 0.0653(6) Uani 1 1 d . . .
H23 H 0.4575 0.5456 1.3756 0.078 Uiso 1 1 calc R . .
C24 C 0.3206(3) 0.4774(2) 1.2091(2) 0.0657(6) Uani 1 1 d . . .
H24 H 0.4081 0.5098 1.1747 0.079 Uiso 1 1 calc R . .
C25 C 0.1657(3) 0.4085(2) 1.1415(2) 0.0559(5) Uani 1 1 d . . .
H25 H 0.1492 0.3945 1.0615 0.067 Uiso 1 1 calc R . .
C26 C 0.0283(2) 0.35755(17) 1.19104(16) 0.0437(4) Uani 1 1 d . . .
C6 C -0.0089(3) 0.00774(18) 0.76653(18) 0.0489(4) Uani 1 1 d . A .
H6 H 0.0528 -0.0483 0.8047 0.059 Uiso 1 1 calc R . .
C7 C -0.0512(3) -0.0042(2) 0.64574(19) 0.0568(5) Uani 1 1 d . A .
H7 H -0.0228 -0.0694 0.5907 0.068 Uiso 1 1 calc R . .
C8 C -0.1439(3) 0.1001(2) 0.62337(18) 0.0570(5) Uani 1 1 d . A .
H8 H -0.1872 0.1155 0.5508 0.068 Uiso 1 1 calc R . .
C9 C -0.1599(2) 0.1774(2) 0.73017(17) 0.0497(4) Uani 1 1 d . A .
H9 H -0.2151 0.2525 0.7397 0.060 Uiso 1 1 calc R . .
C10 C -0.0769(2) 0.12044(17) 0.82038(16) 0.0429(4) Uani 1 1 d . A .
Fe1 Fe 0.10239(3) 0.17043(3) 0.72621(2) 0.04557(10) Uani 1 1 d . . .
C1 C 0.376(2) 0.1843(17) 0.7812(13) 0.057(2) Uani 0.568(17) 1 d PU A -1
H1 H 0.4399 0.1328 0.8235 0.069 Uiso 0.568(17) 1 calc PR A -1
C2 C 0.3317(11) 0.1620(10) 0.6569(8) 0.0599(17) Uani 0.568(17) 1 d PU A -1
H2 H 0.3565 0.0928 0.6039 0.072 Uiso 0.568(17) 1 calc PR A -1
C3 C 0.2438(10) 0.2666(15) 0.6333(12) 0.070(3) Uani 0.568(17) 1 d PU A -1
H3 H 0.2004 0.2806 0.5602 0.084 Uiso 0.568(17) 1 calc PR A -1
C4 C 0.2317(11) 0.3471(9) 0.7380(15) 0.077(4) Uani 0.568(17) 1 d PU A -1
H4 H 0.1809 0.4242 0.7482 0.093 Uiso 0.568(17) 1 calc PR A -1
C5 C 0.3120(14) 0.2871(14) 0.8241(9) 0.080(3) Uani 0.568(17) 1 d PU A -1
H5 H 0.3186 0.3178 0.9027 0.096 Uiso 0.568(17) 1 calc PR A -1
C1A C 0.364(3) 0.176(2) 0.7555(19) 0.077(6) Uani 0.432(17) 1 d PU A -2
H1A H 0.4148 0.1004 0.7613 0.092 Uiso 0.432(17) 1 calc PR A -2
C2A C 0.3063(19) 0.2228(19) 0.6577(12) 0.076(5) Uani 0.432(17) 1 d PU A -2
H2A H 0.3245 0.1867 0.5848 0.092 Uiso 0.432(17) 1 calc PR A -2
C3A C 0.218(2) 0.3311(19) 0.6823(13) 0.070(4) Uani 0.432(17) 1 d PU A -2
H3A H 0.1595 0.3730 0.6282 0.084 Uiso 0.432(17) 1 calc PR A -2
C4A C 0.2309(11) 0.3656(9) 0.7999(10) 0.059(2) Uani 0.432(17) 1 d PU A -2
H4A H 0.1848 0.4363 0.8377 0.071 Uiso 0.432(17) 1 calc PR A -2
C5A C 0.3216(11) 0.2807(9) 0.8533(10) 0.047(2) Uani 0.432(17) 1 d PRU A -2
H5A H 0.3518 0.2850 0.9323 0.056 Uiso 0.432(17) 1 calc PR A -2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C11 0.0480(10) 0.0440(9) 0.0474(9) 0.0136(7) 0.0123(8) 0.0039(7)
C12 0.0439(9) 0.0486(10) 0.0474(10) 0.0100(8) 0.0074(8) 0.0051(8)
C13 0.0427(9) 0.0380(8) 0.0470(9) 0.0077(7) 0.0108(7) 0.0070(7)
C14 0.0393(8) 0.0368(8) 0.0491(9) 0.0088(7) 0.0091(7) 0.0067(7)
C15 0.0431(9) 0.0513(10) 0.0565(11) 0.0101(8) 0.0057(8) 0.0012(8)
C16 0.0409(10) 0.0592(12) 0.0789(15) 0.0167(11) 0.0084(10) -0.0028(9)
C17 0.0502(11) 0.0625(13) 0.0806(15) 0.0224(11) 0.0258(11) 0.0013(9)
C18 0.0567(11) 0.0561(11) 0.0592(12) 0.0172(9) 0.0221(9) 0.0090(9)
C19 0.0450(9) 0.0405(8) 0.0496(10) 0.0112(7) 0.0125(7) 0.0083(7)
C20 0.0510(10) 0.0455(9) 0.0447(9) 0.0067(7) 0.0088(8) 0.0060(8)
C21 0.0429(9) 0.0399(9) 0.0536(10) 0.0065(7) 0.0071(8) 0.0065(7)
C22 0.0488(11) 0.0519(11) 0.0632(12) 0.0056(9) 0.0009(9) 0.0027(9)
C23 0.0450(11) 0.0560(12) 0.0838(16) 0.0050(11) 0.0035(10) -0.0061(9)
C24 0.0498(11) 0.0525(12) 0.0943(18) 0.0120(11) 0.0251(11) -0.0063(9)
C25 0.0542(11) 0.0487(10) 0.0655(12) 0.0103(9) 0.0208(10) -0.0005(9)
C26 0.0415(9) 0.0373(8) 0.0523(10) 0.0073(7) 0.0124(7) 0.0054(7)
C6 0.0530(10) 0.0428(9) 0.0572(11) 0.0158(8) 0.0233(9) 0.0045(8)
C7 0.0588(12) 0.0551(11) 0.0562(11) 0.0039(9) 0.0260(9) -0.0032(9)
C8 0.0439(10) 0.0792(14) 0.0473(10) 0.0163(10) 0.0101(8) 0.0004(9)
C9 0.0383(9) 0.0572(11) 0.0555(11) 0.0169(9) 0.0102(8) 0.0069(8)
C10 0.0396(8) 0.0427(9) 0.0482(9) 0.0126(7) 0.0136(7) 0.0012(7)
Fe1 0.03639(15) 0.05029(17) 0.05472(17) 0.02321(12) 0.01095(11) 0.00229(10)
C1 0.033(3) 0.082(6) 0.052(3) 0.020(3) -0.002(2) -0.002(3)
C2 0.041(2) 0.077(4) 0.061(4) 0.011(4) 0.019(2) -0.002(3)
C3 0.046(3) 0.089(7) 0.082(6) 0.050(5) 0.008(3) -0.009(4)
C4 0.055(4) 0.045(3) 0.131(13) 0.015(8) 0.027(8) -0.002(3)
C5 0.066(5) 0.110(7) 0.050(4) -0.003(4) 0.019(3) -0.029(5)
C1A 0.038(5) 0.064(6) 0.119(17) 0.000(8) 0.012(8) 0.012(4)
C2A 0.059(7) 0.094(11) 0.071(7) -0.002(8) 0.034(5) -0.019(8)
C3A 0.070(5) 0.069(8) 0.071(8) 0.038(8) 0.003(6) -0.018(5)
C4A 0.043(3) 0.046(3) 0.085(7) 0.014(4) 0.010(4) 0.000(2)
C5A 0.035(3) 0.055(4) 0.049(5) 0.015(3) 0.005(3) 0.000(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100891.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-17 01:36:00 +0300 (Fri, 17 Aug 2018) $
#$Revision: 209832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100891.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100891
loop_
_publ_author_name
'Cuffe, Laurence'
'Hudson, Richard D. A.'
'Gallagher, John F.'
'Jennings, Sarah'
'McAdam, C. John'
'Connelly, Rosamond B. T.'
'Manning, Anthony R.'
'Robinson, Brian. H.'
'Simpson, Jim'
_publ_section_title
;
Synthesis, Structure, and Redox Chemistry of Ethenyl and Ethynyl
Ferrocene Polyaromatic Dyads
;
_journal_coden_ASTM ORGND7
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2051
_journal_page_last 2060
_journal_paper_doi 10.1021/om0492653
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety 'C28 H20 Fe'
_chemical_formula_sum 'C28 H20 Fe'
_chemical_formula_weight 412.29
_chemical_name_systematic
;
(E)-1-ferrocenyl-2-(1-pyrenyl) ethene
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 110.62(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.12(3)
_cell_length_b 7.379(9)
_cell_length_c 14.89(3)
_cell_measurement_reflns_used 3254
_cell_measurement_temperature 168(2)
_cell_measurement_theta_max 25.65
_cell_measurement_theta_min 2.72
_cell_volume 1966(5)
_diffrn_ambient_temperature 168(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0841
_diffrn_reflns_av_sigmaI/netI 0.1049
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 23370
_diffrn_reflns_theta_max 26.47
_diffrn_reflns_theta_min 2.28
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.778
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.845189
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS Bruker 1997'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.393
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 856
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.829
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 262
_refine_ls_number_reflns 4001
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.829
_refine_ls_R_factor_all 0.1020
_refine_ls_R_factor_gt 0.0363
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean '< 0.001'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0594
_refine_ls_wR_factor_ref 0.0696
_reflns_number_gt 2081
_reflns_number_total 4001
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1100891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.47603(17) 0.8951(4) 0.7826(2) 0.0460(8) Uani 1 1 d . . .
H1 H 0.5126 0.8191 0.7722 0.055 Uiso 1 1 calc R . .
C2 C 0.48342(17) 0.9905(4) 0.8678(2) 0.0482(8) Uani 1 1 d . . .
H2 H 0.5264 0.9914 0.9247 0.058 Uiso 1 1 calc R . .
C3 C 0.41642(19) 1.0836(4) 0.8538(2) 0.0538(9) Uani 1 1 d . . .
H3 H 0.4060 1.1573 0.8998 0.065 Uiso 1 1 calc R . .
C4 C 0.36763(18) 1.0493(4) 0.7603(2) 0.0548(9) Uani 1 1 d . . .
H4 H 0.3184 1.0958 0.7319 0.066 Uiso 1 1 calc R . .
C5 C 0.40428(19) 0.9337(4) 0.7156(2) 0.0514(9) Uani 1 1 d . . .
H5 H 0.3842 0.8895 0.6517 0.062 Uiso 1 1 calc R . .
Fe1 Fe 0.39580(2) 0.81332(5) 0.83414(3) 0.03032(12) Uani 1 1 d . . .
C6 C 0.41067(14) 0.5420(3) 0.85998(19) 0.0345(7) Uani 1 1 d . . .
H6 H 0.4493 0.4697 0.8524 0.041 Uiso 1 1 calc R . .
C7 C 0.41370(14) 0.6338(3) 0.94409(19) 0.0334(7) Uani 1 1 d . . .
H7 H 0.4549 0.6340 1.0030 0.040 Uiso 1 1 calc R . .
C8 C 0.34496(14) 0.7260(3) 0.92630(19) 0.0354(7) Uani 1 1 d . . .
H8 H 0.3321 0.7981 0.9710 0.043 Uiso 1 1 calc R . .
C9 C 0.29906(13) 0.6917(3) 0.83035(19) 0.0342(6) Uani 1 1 d . . .
H9 H 0.2499 0.7373 0.7994 0.041 Uiso 1 1 calc R . .
C10 C 0.33874(13) 0.5770(3) 0.78740(19) 0.0288(6) Uani 1 1 d . . .
C11 C 0.31499(14) 0.5140(3) 0.68919(19) 0.0310(7) Uani 1 1 d . . .
H11 H 0.3498 0.4434 0.6718 0.037 Uiso 1 1 calc R . .
C12 C 0.24877(14) 0.5454(3) 0.62043(19) 0.0335(7) Uani 1 1 d . . .
H12 H 0.2135 0.6132 0.6383 0.040 Uiso 1 1 calc R . .
C13 C 0.22527(14) 0.4855(3) 0.52025(19) 0.0317(7) Uani 1 1 d . . .
C14 C 0.24930(14) 0.3173(4) 0.4973(2) 0.0396(7) Uani 1 1 d . . .
H14 H 0.2797 0.2416 0.5476 0.047 Uiso 1 1 calc R . .
C15 C 0.22978(15) 0.2597(4) 0.4036(2) 0.0448(8) Uani 1 1 d . . .
H15 H 0.2482 0.1468 0.3907 0.054 Uiso 1 1 calc R . .
C16 C 0.18381(14) 0.3629(4) 0.3275(2) 0.0370(7) Uani 1 1 d . . .
C17 C 0.16191(15) 0.3073(4) 0.2295(2) 0.0482(8) Uani 1 1 d . . .
H17 H 0.1791 0.1938 0.2153 0.058 Uiso 1 1 calc R . .
C18 C 0.11794(16) 0.4093(5) 0.1566(2) 0.0528(9) Uani 1 1 d . . .
H18 H 0.1045 0.3663 0.0926 0.063 Uiso 1 1 calc R . .
C19 C 0.09101(14) 0.5832(4) 0.1745(2) 0.0421(8) Uani 1 1 d . . .
C20 C 0.04480(15) 0.6926(5) 0.1008(2) 0.0534(9) Uani 1 1 d . . .
H20 H 0.0299 0.6521 0.0362 0.064 Uiso 1 1 calc R . .
C21 C 0.02045(16) 0.8602(5) 0.1209(2) 0.0572(10) Uani 1 1 d . . .
H21 H -0.0116 0.9320 0.0701 0.069 Uiso 1 1 calc R . .
C22 C 0.04236(15) 0.9227(4) 0.2137(2) 0.0506(8) Uani 1 1 d . . .
H22 H 0.0263 1.0389 0.2261 0.061 Uiso 1 1 calc R . .
C23 C 0.08794(13) 0.8178(4) 0.29012(19) 0.0365(7) Uani 1 1 d . . .
C24 C 0.11216(14) 0.8773(4) 0.3870(2) 0.0413(8) Uani 1 1 d . . .
H24 H 0.0975 0.9941 0.4006 0.050 Uiso 1 1 calc R . .
C25 C 0.15535(14) 0.7735(4) 0.4606(2) 0.0373(7) Uani 1 1 d . . .
H25 H 0.1704 0.8195 0.5242 0.045 Uiso 1 1 calc R . .
C26 C 0.17904(13) 0.5946(4) 0.44466(19) 0.0292(6) Uani 1 1 d . . .
C27 C 0.15775(13) 0.5336(4) 0.34842(19) 0.0313(7) Uani 1 1 d . . .
C28 C 0.11207(13) 0.6432(3) 0.2708(2) 0.0332(7) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.050(2) 0.0432(19) 0.055(2) 0.0017(17) 0.0305(19) -0.0091(16)
C2 0.053(2) 0.045(2) 0.046(2) 0.0003(16) 0.0162(18) -0.0220(17)
C3 0.089(3) 0.0251(18) 0.055(3) -0.0032(16) 0.035(2) -0.0116(18)
C4 0.058(2) 0.038(2) 0.066(3) 0.0237(18) 0.020(2) 0.0053(17)
C5 0.072(2) 0.050(2) 0.034(2) 0.0032(17) 0.020(2) -0.0208(19)
Fe1 0.0332(2) 0.0253(2) 0.0340(2) 0.0028(2) 0.01381(18) 0.0005(2)
C6 0.0370(19) 0.0274(16) 0.043(2) 0.0037(14) 0.0193(16) 0.0030(13)
C7 0.0320(16) 0.0318(17) 0.0341(18) 0.0085(13) 0.0090(14) 0.0041(12)
C8 0.0390(17) 0.0371(18) 0.0354(18) 0.0001(14) 0.0195(15) 0.0012(14)
C9 0.0266(14) 0.0347(15) 0.0450(18) 0.0057(16) 0.0172(14) 0.0060(14)
C10 0.0249(16) 0.0276(16) 0.0332(17) 0.0040(13) 0.0092(14) -0.0002(12)
C11 0.0330(17) 0.0223(15) 0.0407(19) 0.0019(13) 0.0170(15) -0.0008(12)
C12 0.0338(17) 0.0302(16) 0.0393(19) 0.0030(14) 0.0165(15) 0.0022(13)
C13 0.0283(16) 0.0312(17) 0.0359(18) -0.0009(14) 0.0119(14) -0.0033(13)
C14 0.0400(17) 0.0311(16) 0.0440(19) 0.0003(16) 0.0102(14) 0.0001(15)
C15 0.0457(19) 0.0321(18) 0.059(2) -0.0073(16) 0.0222(18) 0.0014(14)
C16 0.0317(17) 0.0383(18) 0.041(2) -0.0071(15) 0.0135(15) -0.0064(13)
C17 0.0435(18) 0.0472(19) 0.057(2) -0.014(2) 0.0220(17) -0.0067(17)
C18 0.042(2) 0.073(2) 0.043(2) -0.0140(19) 0.0141(17) -0.0129(18)
C19 0.0250(17) 0.065(2) 0.038(2) 0.0013(18) 0.0130(15) -0.0064(16)
C20 0.0287(17) 0.099(3) 0.0331(19) 0.001(2) 0.0112(15) -0.009(2)
C21 0.0328(19) 0.094(3) 0.046(2) 0.025(2) 0.0155(17) 0.0081(18)
C22 0.0330(18) 0.068(2) 0.056(2) 0.021(2) 0.0221(17) 0.0140(16)
C23 0.0228(15) 0.0519(18) 0.0385(18) 0.0077(18) 0.0153(14) 0.0025(15)
C24 0.0345(18) 0.0397(18) 0.054(2) 0.0021(16) 0.0211(16) 0.0105(14)
C25 0.0325(16) 0.0419(18) 0.0398(19) -0.0016(15) 0.0154(15) 0.0034(14)
C26 0.0217(15) 0.0338(16) 0.0319(18) 0.0008(14) 0.0093(13) -0.0012(13)
C27 0.0230(16) 0.0353(17) 0.0389(19) -0.0024(14) 0.0151(14) -0.0062(13)
C28 0.0219(15) 0.0423(19) 0.0384(19) -0.0002(14) 0.0144(14) -0.0046(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100892.cif | #------------------------------------------------------------------------------
#$Date: 2018-09-01 22:50:30 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100892.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100892
loop_
_publ_author_name
'Chase, Preston A.'
'Gagliardo, Marcella'
'Lutz, Martin'
'Spek, Anthony L.'
'van Klink, Gerard P. M.'
'van Koten, Gerard'
_publ_section_title
;
Electron-Poor Pentafluorophenyl-Substituted PCP--Palladium Pincer Complexes
;
_journal_coden_ASTM INOCAJ
_journal_issue 9
_journal_name_full Organometallics
_journal_page_first 2016
_journal_page_last 2019
_journal_paper_doi 10.1021/om0500063
_journal_volume 24
_journal_year 2005
_chemical_formula_moiety '0.82(C32 H8 F20 P2), 0.18(C32 H8 F20 O P2)'
_chemical_formula_sum 'C32 H8 F20 O0.18 P2'
_chemical_formula_weight 837.20
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.0616(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 6.0387(1)
_cell_length_b 32.3369(5)
_cell_length_c 15.9373(2)
_cell_measurement_reflns_used 58833
_cell_measurement_temperature 125(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 1.02
_cell_volume 3031.60(8)
_diffrn_ambient_temperature 125(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method ?
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0584
_diffrn_reflns_av_sigmaI/netI 0.0410
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_k_min -40
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 45613
_diffrn_reflns_theta_max 27.51
_diffrn_reflns_theta_min 1.26
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.294
_exptl_absorpt_correction_T_max 0.98
_exptl_absorpt_correction_T_min 0.86
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.834
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1646
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.06
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 496
_refine_ls_number_reflns 6955
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0615
_refine_ls_R_factor_gt 0.0381
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0929
_refine_ls_wR_factor_ref 0.1046
_reflns_number_gt 5018
_reflns_number_total 6955
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100892
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5154(14) 0.5820(3) 0.2872(6) 0.042(2) Uani 0.18 1 d P . .
P1 P 0.28669(8) 0.579831(14) 0.25268(3) 0.02404(12) Uani 1 1 d . . .
P2 P 0.60722(8) 0.678176(15) 0.61867(3) 0.02590(13) Uani 1 1 d . . .
F1 F -0.19382(18) 0.58511(3) 0.13245(8) 0.0327(3) Uani 1 1 d . . .
F2 F -0.34269(19) 0.63553(4) -0.00089(8) 0.0417(3) Uani 1 1 d . . .
F3 F -0.0618(2) 0.69353(4) -0.04351(8) 0.0417(3) Uani 1 1 d . . .
F4 F 0.3746(2) 0.69906(4) 0.04733(8) 0.0384(3) Uani 1 1 d . . .
F5 F 0.52837(18) 0.64856(3) 0.17973(7) 0.0308(3) Uani 1 1 d . . .
F6 F 0.4430(3) 0.53832(4) 0.11493(11) 0.0587(4) Uani 1 1 d . . .
F7 F 0.3078(3) 0.46866(5) 0.02719(12) 0.0762(6) Uani 1 1 d . . .
F8 F -0.0332(3) 0.42288(4) 0.06455(10) 0.0611(4) Uani 1 1 d . . .
F9 F -0.2324(3) 0.44724(4) 0.19233(11) 0.0668(5) Uani 1 1 d . . .
F10 F -0.1002(3) 0.51572(4) 0.28008(10) 0.0574(4) Uani 1 1 d . . .
F11 F 0.9596(2) 0.74955(4) 0.60462(9) 0.0516(4) Uani 1 1 d . . .
F12 F 1.3597(2) 0.76446(4) 0.71106(9) 0.0544(4) Uani 1 1 d . . .
F13 F 1.5216(2) 0.71442(4) 0.84627(8) 0.0450(3) Uani 1 1 d . . .
F14 F 1.2672(2) 0.64901(4) 0.87765(8) 0.0481(4) Uani 1 1 d . . .
F15 F 0.8582(2) 0.63495(4) 0.77652(8) 0.0468(4) Uani 1 1 d . . .
F16 F 0.9653(2) 0.63155(4) 0.53874(8) 0.0388(3) Uani 1 1 d . . .
F17 F 1.0006(2) 0.55067(4) 0.51315(9) 0.0489(4) Uani 1 1 d . . .
F18 F 0.7125(2) 0.49674(4) 0.56553(9) 0.0487(4) Uani 1 1 d . . .
F19 F 0.3938(2) 0.52510(4) 0.64487(10) 0.0499(4) Uani 1 1 d . . .
F20 F 0.3487(2) 0.60655(4) 0.66909(8) 0.0395(3) Uani 1 1 d . . .
C1 C 0.3458(3) 0.64739(6) 0.41158(12) 0.0247(4) Uani 1 1 d . . .
H1 H 0.4651 0.6276 0.4239 0.030 Uiso 1 1 calc R . .
C2 C 0.1389(3) 0.63649(6) 0.35750(12) 0.0251(4) Uani 1 1 d . . .
C3 C -0.0302(3) 0.66610(6) 0.33702(13) 0.0302(4) Uani 1 1 d . . .
H3 H -0.1707 0.6593 0.2990 0.036 Uiso 1 1 calc R . .
C4 C 0.0033(4) 0.70545(6) 0.37128(14) 0.0335(5) Uani 1 1 d . . .
H4 H -0.1132 0.7256 0.3563 0.040 Uiso 1 1 calc R . .
C5 C 0.2067(3) 0.71548(6) 0.42740(13) 0.0303(4) Uani 1 1 d . . .
H5 H 0.2269 0.7423 0.4521 0.036 Uiso 1 1 calc R . .
C6 C 0.3814(3) 0.68676(6) 0.44801(12) 0.0257(4) Uani 1 1 d . . .
C7 C 0.0948(3) 0.59285(6) 0.32400(13) 0.0276(4) Uani 1 1 d . . .
H7A H -0.0651 0.5903 0.2917 0.033 Uiso 1 1 calc R . .
H7B H 0.1196 0.5733 0.3730 0.033 Uiso 1 1 calc R . .
C8 C 0.1739(3) 0.61450(5) 0.16148(12) 0.0227(4) Uani 1 1 d . . .
C9 C -0.0489(3) 0.61297(6) 0.11353(13) 0.0249(4) Uani 1 1 d . . .
C10 C -0.1286(3) 0.63901(6) 0.04492(13) 0.0287(4) Uani 1 1 d . . .
C11 C 0.0137(3) 0.66801(6) 0.02285(12) 0.0291(4) Uani 1 1 d . . .
C12 C 0.2352(3) 0.67068(6) 0.06866(13) 0.0272(4) Uani 1 1 d . . .
C13 C 0.3114(3) 0.64415(6) 0.13670(12) 0.0236(4) Uani 1 1 d . . .
C14 C 0.1781(3) 0.53040(6) 0.20122(13) 0.0260(4) Uani 1 1 d . . .
C15 C 0.2769(4) 0.51608(6) 0.13634(15) 0.0357(5) Uani 1 1 d . . .
C16 C 0.2104(4) 0.48043(7) 0.09063(16) 0.0452(6) Uani 1 1 d . . .
C17 C 0.0377(4) 0.45714(6) 0.10966(15) 0.0421(6) Uani 1 1 d . . .
C18 C -0.0631(4) 0.46959(6) 0.17386(15) 0.0398(5) Uani 1 1 d . . .
C19 C 0.0075(4) 0.50552(6) 0.21868(13) 0.0330(5) Uani 1 1 d . . .
C20 C 0.6027(3) 0.69851(6) 0.50931(13) 0.0298(5) Uani 1 1 d . . .
H20A H 0.6185 0.7290 0.5116 0.036 Uiso 1 1 calc R . .
H20B H 0.7322 0.6869 0.4884 0.036 Uiso 1 1 calc R . .
C21 C 0.8941(3) 0.69037(6) 0.68346(12) 0.0265(4) Uani 1 1 d . . .
C22 C 1.0286(3) 0.72358(6) 0.67183(13) 0.0314(5) Uani 1 1 d . . .
C23 C 1.2357(4) 0.73203(6) 0.72599(14) 0.0333(5) Uani 1 1 d . . .
C24 C 1.3182(3) 0.70701(6) 0.79450(13) 0.0328(5) Uani 1 1 d . . .
C25 C 1.1909(4) 0.67386(6) 0.81004(13) 0.0324(5) Uani 1 1 d . . .
C26 C 0.9828(3) 0.66660(6) 0.75618(13) 0.0305(5) Uani 1 1 d . . .
C27 C 0.6505(3) 0.62246(6) 0.60241(12) 0.0238(4) Uani 1 1 d . . .
C28 C 0.8182(3) 0.60635(6) 0.56493(13) 0.0279(4) Uani 1 1 d . . .
C29 C 0.8396(4) 0.56457(6) 0.55160(14) 0.0327(5) Uani 1 1 d . . .
C30 C 0.6948(4) 0.53755(6) 0.57830(14) 0.0342(5) Uani 1 1 d . . .
C31 C 0.5306(4) 0.55187(6) 0.61759(14) 0.0329(5) Uani 1 1 d . . .
C32 C 0.5104(3) 0.59384(6) 0.62940(13) 0.0282(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.038(5) 0.038(5) 0.044(5) -0.002(4) 0.000(4) 0.005(4)
P1 0.0281(3) 0.0206(2) 0.0219(3) -0.00096(19) 0.00230(19) -0.00207(19)
P2 0.0269(3) 0.0250(3) 0.0235(3) -0.0022(2) 0.0009(2) -0.0006(2)
F1 0.0248(6) 0.0338(6) 0.0376(7) -0.0013(5) 0.0031(5) -0.0076(5)
F2 0.0259(6) 0.0525(8) 0.0385(7) -0.0013(6) -0.0099(5) 0.0020(6)
F3 0.0469(7) 0.0392(7) 0.0336(7) 0.0131(6) -0.0019(6) 0.0089(6)
F4 0.0416(7) 0.0302(6) 0.0423(8) 0.0114(5) 0.0073(6) -0.0056(5)
F5 0.0233(6) 0.0320(6) 0.0335(7) 0.0036(5) -0.0013(5) -0.0052(5)
F6 0.0631(9) 0.0498(8) 0.0790(11) -0.0290(8) 0.0493(8) -0.0270(7)
F7 0.1076(14) 0.0583(10) 0.0861(13) -0.0423(9) 0.0709(11) -0.0308(9)
F8 0.0995(12) 0.0373(7) 0.0555(9) -0.0267(7) 0.0366(9) -0.0319(8)
F9 0.0947(12) 0.0487(9) 0.0728(11) -0.0275(8) 0.0521(9) -0.0460(8)
F10 0.0834(11) 0.0454(8) 0.0590(9) -0.0242(7) 0.0488(8) -0.0339(7)
F11 0.0554(8) 0.0380(7) 0.0474(8) 0.0173(6) -0.0180(7) -0.0184(6)
F12 0.0499(8) 0.0505(8) 0.0529(9) 0.0122(7) -0.0091(7) -0.0263(7)
F13 0.0306(6) 0.0536(8) 0.0423(8) -0.0001(6) -0.0099(6) -0.0075(6)
F14 0.0510(8) 0.0493(8) 0.0330(7) 0.0111(6) -0.0137(6) -0.0068(6)
F15 0.0539(8) 0.0488(8) 0.0304(7) 0.0117(6) -0.0054(6) -0.0221(6)
F16 0.0335(7) 0.0408(7) 0.0465(8) 0.0079(6) 0.0183(6) 0.0004(5)
F17 0.0523(8) 0.0472(8) 0.0529(9) 0.0005(7) 0.0241(7) 0.0196(7)
F18 0.0624(9) 0.0251(6) 0.0550(9) -0.0034(6) 0.0059(7) 0.0074(6)
F19 0.0524(8) 0.0347(7) 0.0655(10) 0.0095(7) 0.0193(7) -0.0120(6)
F20 0.0358(7) 0.0418(7) 0.0466(8) -0.0002(6) 0.0212(6) -0.0028(5)
C1 0.0289(10) 0.0242(9) 0.0204(10) -0.0001(8) 0.0039(8) 0.0014(8)
C2 0.0314(10) 0.0244(9) 0.0194(10) -0.0008(8) 0.0054(8) -0.0022(8)
C3 0.0277(10) 0.0367(11) 0.0231(10) -0.0020(9) -0.0009(8) 0.0004(8)
C4 0.0337(11) 0.0328(11) 0.0319(12) -0.0017(9) 0.0029(9) 0.0109(9)
C5 0.0401(11) 0.0246(10) 0.0247(11) -0.0044(8) 0.0042(9) 0.0004(8)
C6 0.0309(10) 0.0268(10) 0.0178(9) -0.0001(8) 0.0026(8) -0.0009(8)
C7 0.0333(10) 0.0263(10) 0.0227(10) -0.0022(8) 0.0051(8) -0.0054(8)
C8 0.0251(9) 0.0213(9) 0.0209(10) -0.0033(7) 0.0033(7) 0.0011(7)
C9 0.0244(9) 0.0237(9) 0.0266(10) -0.0039(8) 0.0058(8) -0.0024(8)
C10 0.0229(9) 0.0327(11) 0.0272(11) -0.0052(9) -0.0017(8) 0.0043(8)
C11 0.0349(11) 0.0283(10) 0.0223(10) 0.0020(8) 0.0023(8) 0.0065(8)
C12 0.0321(11) 0.0225(9) 0.0271(11) 0.0016(8) 0.0068(8) -0.0012(8)
C13 0.0219(9) 0.0242(9) 0.0229(10) -0.0035(8) 0.0010(7) 0.0008(7)
C14 0.0299(10) 0.0218(9) 0.0254(10) -0.0001(8) 0.0045(8) -0.0005(8)
C15 0.0408(12) 0.0276(11) 0.0436(13) -0.0077(9) 0.0202(10) -0.0077(9)
C16 0.0628(16) 0.0347(12) 0.0463(15) -0.0156(11) 0.0292(12) -0.0087(11)
C17 0.0635(16) 0.0255(11) 0.0391(13) -0.0109(10) 0.0155(11) -0.0135(10)
C18 0.0566(14) 0.0303(11) 0.0380(13) -0.0062(10) 0.0222(11) -0.0195(10)
C19 0.0491(13) 0.0264(10) 0.0273(11) -0.0047(9) 0.0171(9) -0.0075(9)
C20 0.0366(11) 0.0252(10) 0.0246(11) -0.0018(8) 0.0009(8) -0.0048(8)
C21 0.0286(10) 0.0267(10) 0.0230(10) -0.0042(8) 0.0033(8) 0.0001(8)
C22 0.0360(11) 0.0275(10) 0.0269(11) 0.0032(8) -0.0008(9) -0.0035(8)
C23 0.0341(11) 0.0307(11) 0.0333(12) -0.0017(9) 0.0036(9) -0.0103(9)
C24 0.0261(10) 0.0387(12) 0.0292(11) -0.0058(9) -0.0029(8) -0.0024(9)
C25 0.0369(11) 0.0334(11) 0.0229(11) 0.0024(9) -0.0015(9) 0.0000(9)
C26 0.0346(11) 0.0306(10) 0.0248(10) -0.0002(9) 0.0034(8) -0.0079(9)
C27 0.0224(9) 0.0266(10) 0.0200(10) 0.0002(8) 0.0001(7) 0.0006(7)
C28 0.0252(10) 0.0309(10) 0.0264(11) 0.0046(8) 0.0030(8) -0.0007(8)
C29 0.0348(11) 0.0334(11) 0.0302(11) -0.0001(9) 0.0080(9) 0.0092(9)
C30 0.0429(12) 0.0236(10) 0.0323(12) -0.0008(9) 0.0006(9) 0.0052(9)
C31 0.0350(11) 0.0274(10) 0.0346(12) 0.0048(9) 0.0042(9) -0.0065(9)
C32 0.0261(10) 0.0326(10) 0.0253(10) -0.0012(8) 0.0049(8) -0.0002(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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