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1500046.cif | #------------------------------------------------------------------------------
#$Date: 2023-12-01 10:31:03 +0200 (Fri, 01 Dec 2023) $
#$Revision: 287927 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500046.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_1500046
loop_
_publ_author_name
'Yoon, Il'
'Lee, Yoon Hee'
'Lee, Shim Sung'
'Lee, Sang Cheol'
'Park, Sung Bae'
_publ_contact_author_address
;
Prof Shim Sung Lee
Dept of Chemistry & Research Inst of Natural Sciences
Gyeongsang National University
Chinju 660-701
KOREA
;
_publ_contact_author_email sslee@nongae.gsnu.ac.kr
_publ_contact_author_name 'Prof Shim Sung Lee'
_publ_section_references
;
Siemens, SMART and SAINT. Area detector Control and Intergration Software.
Version 4.0, Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin,
USA. 1996.
G. M. Sheldrick, SHELXTL. Structure Determination Programs. Version 5.03,
Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 1996.
;
_publ_section_title
;
S2O2 donor cyclic and acyclic ionophores: Potentiometric sensing for
Ag(i) and a new nitrate-bridged dimeric Ag(i) complex of the acyclic
ionophore with an unusual structure
;
_journal_issue 10
_journal_name_full 'The Analyst'
_journal_page_first 1773
_journal_paper_doi 10.1039/b105136a
_journal_volume 126
_journal_year 2001
_chemical_formula_sum 'C40 H52 Ag2 F6 N O7 P S4'
_chemical_formula_weight 1147.78
_space_group_IT_number 5
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C 2y'
_symmetry_space_group_name_H-M 'C 1 2 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXLTL
_cell_angle_alpha 90.00
_cell_angle_beta 106.009(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 23.8522(15)
_cell_length_b 7.5310(4)
_cell_length_c 14.0178(8)
_cell_measurement_reflns_used 7809
_cell_measurement_temperature 571(2)
_cell_measurement_theta_max 28.29
_cell_measurement_theta_min 1.78
_cell_volume 2420.4(2)
_computing_cell_refinement 'SAINT (Siemens, 1996)'
_computing_data_collection 'SMART (Siemens, 1996)'
_computing_data_reduction 'SHELXTL (Sheldrick, 1996)'
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_computing_structure_refinement SHELXTL
_computing_structure_solution SHELXTL
_diffrn_ambient_temperature 571(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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 0.0338
_diffrn_reflns_av_sigmaI/netI 0.0244
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 7809
_diffrn_reflns_theta_full 28.29
_diffrn_reflns_theta_max 28.29
_diffrn_reflns_theta_min 1.78
_exptl_absorpt_coefficient_mu 1.083
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.624
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Siemens, 1996)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.575
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1164
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.480
_refine_diff_density_min -0.722
_refine_diff_density_rms 0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.01(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_hydrogen_treatment 'H atoms riding'
_refine_ls_matrix_type full
_refine_ls_number_parameters 277
_refine_ls_number_reflns 4790
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0383
_refine_ls_R_factor_gt 0.0340
_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^)+(0.0657P)^2^+0.7979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0950
_refine_ls_wR_factor_ref 0.0989
_reflns_number_gt 4355
_reflns_number_total 4790
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file crystallography_data.txt
_cod_data_source_block '[Ag2(I)2(NO3)](PF6)'
_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 '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 C2
_cod_database_code 1500046
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'
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
Ag Ag -0.474998(10) -0.31201(4) -0.871806(18) 0.06213(10) Uani 1 1 d . . .
S1 S -0.37487(4) -0.44195(16) -0.80448(7) 0.0617(2) Uani 1 1 d . . .
S2 S -0.57150(4) -0.46300(13) -0.93093(7) 0.0571(2) Uani 1 1 d . . .
O1 O -0.43001(14) -0.1707(5) -0.6905(2) 0.0797(9) Uani 1 1 d . . .
O2 O -0.54661(14) -0.1184(5) -0.7982(3) 0.0761(8) Uani 1 1 d . . .
C1 C -0.2882(3) -0.7837(9) -0.7407(5) 0.0915(16) Uani 1 1 d . . .
H1 H -0.2900 -0.7435 -0.8065 0.110 Uiso 1 1 calc R . .
C2 C -0.2390(3) -0.8718(9) -0.6852(6) 0.109(2) Uani 1 1 d . . .
H2 H -0.2071 -0.8910 -0.7133 0.131 Uiso 1 1 calc R . .
C3 C -0.2348(4) -0.9316(10) -0.5921(6) 0.115(3) Uani 1 1 d . . .
H3 H -0.2001 -0.9914 -0.5548 0.138 Uiso 1 1 calc R . .
C4 C -0.2802(4) -0.9060(10) -0.5522(5) 0.112(2) Uani 1 1 d . . .
H4 H -0.2780 -0.9502 -0.4870 0.134 Uiso 1 1 calc R . .
C5 C -0.3303(2) -0.8148(11) -0.6066(3) 0.0873(13) Uani 1 1 d . . .
H5 H -0.3619 -0.7946 -0.5777 0.105 Uiso 1 1 calc R . .
C6 C -0.3345(2) -0.7534(6) -0.7022(3) 0.0698(11) Uani 1 1 d . . .
C7 C -0.38929(19) -0.6625(7) -0.7613(4) 0.0691(10) Uani 1 1 d . . .
H7A H -0.4157 -0.6512 -0.7209 0.083 Uiso 1 1 calc R . .
H7B H -0.4078 -0.7347 -0.8176 0.083 Uiso 1 1 calc R . .
C8 C -0.34504(16) -0.3238(8) -0.6898(3) 0.0676(9) Uani 1 1 d . . .
H8A H -0.3140 -0.3934 -0.6485 0.081 Uiso 1 1 calc R . .
H8B H -0.3284 -0.2145 -0.7044 0.081 Uiso 1 1 calc R . .
C9 C -0.3875(2) -0.2823(7) -0.6330(3) 0.0719(12) Uani 1 1 d . . .
H9A H -0.4051 -0.3897 -0.6181 0.086 Uiso 1 1 calc R . .
H9B H -0.3681 -0.2250 -0.5716 0.086 Uiso 1 1 calc R . .
C10 C -0.4742(3) -0.1338(9) -0.6411(4) 0.0944(17) Uani 1 1 d . . .
H10A H -0.4576 -0.0705 -0.5805 0.113 Uiso 1 1 calc R . .
H10B H -0.4906 -0.2427 -0.6255 0.113 Uiso 1 1 calc R . .
C11 C -0.5187(3) -0.0277(10) -0.7073(4) 0.0998(19) Uani 1 1 d . . .
H11A H -0.5476 0.0037 -0.6743 0.120 Uiso 1 1 calc R . .
H11B H -0.5015 0.0801 -0.7225 0.120 Uiso 1 1 calc R . .
C12 C -0.5963(2) -0.2213(7) -0.7973(4) 0.0810(13) Uani 1 1 d . . .
H12A H -0.6255 -0.1466 -0.7829 0.097 Uiso 1 1 calc R . .
H12B H -0.5857 -0.3106 -0.7467 0.097 Uiso 1 1 calc R . .
C13 C -0.61976(16) -0.3068(8) -0.8960(3) 0.0749(11) Uani 1 1 d . . .
H13A H -0.6295 -0.2154 -0.9456 0.090 Uiso 1 1 calc R . .
H13B H -0.6552 -0.3673 -0.8964 0.090 Uiso 1 1 calc R . .
C14 C -0.57173(16) -0.6511(6) -0.8488(3) 0.0554(8) Uani 1 1 d . . .
H14A H -0.5437 -0.7373 -0.8569 0.066 Uiso 1 1 calc R . .
H14B H -0.5600 -0.6110 -0.7812 0.066 Uiso 1 1 calc R . .
C15 C -0.63049(16) -0.7376(5) -0.8693(3) 0.0579(9) Uani 1 1 d . . .
C16 C -0.65435(16) -0.8225(8) -0.9587(3) 0.0663(9) Uani 1 1 d . . .
H16 H -0.6337 -0.8213 -1.0085 0.080 Uiso 1 1 calc R . .
C17 C -0.7076(2) -0.9096(8) -0.9779(5) 0.0842(14) Uani 1 1 d . . .
H17 H -0.7231 -0.9721 -1.0392 0.101 Uiso 1 1 calc R . .
C18 C -0.7379(2) -0.9041(9) -0.9068(5) 0.0944(18) Uani 1 1 d . . .
H18 H -0.7754 -0.9602 -0.9197 0.113 Uiso 1 1 calc R . .
C19 C -0.7151(2) -0.8202(12) -0.8189(5) 0.0970(15) Uani 1 1 d . . .
H19 H -0.7364 -0.8186 -0.7700 0.116 Uiso 1 1 calc R . .
C20 C -0.6617(2) -0.7376(7) -0.7990(4) 0.0775(12) Uani 1 1 d . . .
H20 H -0.6460 -0.6797 -0.7363 0.093 Uiso 1 1 calc R . .
O3 O -0.45762(17) -0.0388(7) -0.9484(3) 0.0965(12) Uani 1 1 d . . .
O4 O -0.5000 0.2060(8) -1.0000 0.126(2) Uani 1 2 d S . .
N N -0.5000 0.0421(6) -1.0000 0.0638(12) Uani 1 2 d S . .
P P -0.5000 -0.6220(2) -0.5000 0.0738(5) Uani 1 2 d S . .
F1 F -0.5137(2) -0.6217(5) -0.3951(2) 0.1080(12) Uani 1 1 d . . .
F2 F -0.5469(2) -0.7727(7) -0.5362(3) 0.159(2) Uani 1 1 d . . .
F3 F -0.5470(2) -0.4732(6) -0.5360(3) 0.1237(15) 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
Ag 0.05032(14) 0.07359(19) 0.05996(15) 0.00528(16) 0.01097(10) -0.00286(18)
S1 0.0484(5) 0.0804(7) 0.0557(5) -0.0005(4) 0.0133(4) 0.0005(5)
S2 0.0534(5) 0.0588(5) 0.0547(4) 0.0097(4) 0.0073(4) -0.0060(4)
O1 0.0683(17) 0.093(2) 0.0717(18) -0.0128(17) 0.0084(14) 0.0135(18)
O2 0.0615(17) 0.073(2) 0.090(2) -0.0110(16) 0.0140(15) 0.0022(15)
C1 0.090(3) 0.082(4) 0.102(3) -0.001(3) 0.026(3) 0.020(3)
C2 0.086(4) 0.096(5) 0.144(6) 0.000(4) 0.029(4) 0.028(3)
C3 0.105(5) 0.078(4) 0.134(6) 0.000(4) -0.012(5) 0.000(4)
C4 0.125(6) 0.098(4) 0.085(4) 0.004(3) -0.019(4) -0.024(4)
C5 0.089(3) 0.088(3) 0.076(2) -0.010(3) 0.009(2) -0.019(4)
C6 0.074(3) 0.060(2) 0.071(2) -0.0119(17) 0.013(2) -0.0048(19)
C7 0.059(2) 0.067(2) 0.079(3) -0.012(2) 0.0143(19) -0.007(2)
C8 0.0551(17) 0.071(2) 0.0679(19) -0.002(2) 0.0014(15) -0.004(2)
C9 0.076(2) 0.077(3) 0.0571(18) -0.0091(19) 0.0092(17) -0.009(2)
C10 0.103(4) 0.102(4) 0.077(3) -0.018(3) 0.022(3) 0.022(3)
C11 0.103(4) 0.101(4) 0.086(3) -0.029(3) 0.011(3) 0.026(3)
C12 0.069(3) 0.074(3) 0.105(4) 0.005(3) 0.032(3) 0.012(2)
C13 0.0502(16) 0.060(2) 0.105(3) 0.013(3) 0.0053(18) 0.006(3)
C14 0.0524(18) 0.055(2) 0.0588(18) 0.0099(15) 0.0150(15) 0.0023(16)
C15 0.0513(19) 0.0512(18) 0.075(2) 0.0143(17) 0.0244(17) 0.0057(15)
C16 0.0552(17) 0.067(2) 0.076(2) 0.006(3) 0.0180(16) 0.003(3)
C17 0.074(3) 0.067(3) 0.104(4) 0.008(3) 0.011(3) -0.009(2)
C18 0.059(3) 0.092(4) 0.134(5) 0.029(4) 0.029(3) 0.001(3)
C19 0.075(3) 0.111(4) 0.123(4) 0.013(5) 0.056(3) -0.002(4)
C20 0.080(3) 0.075(3) 0.089(3) 0.002(2) 0.043(3) 0.005(2)
O3 0.081(2) 0.110(3) 0.096(2) 0.039(2) 0.0189(19) -0.021(2)
O4 0.185(6) 0.049(3) 0.188(6) 0.000 0.123(6) 0.000
N 0.092(4) 0.047(3) 0.064(3) 0.000 0.041(3) 0.000
P 0.1175(14) 0.0581(9) 0.0554(7) 0.000 0.0400(8) 0.000
F1 0.171(4) 0.101(2) 0.0711(16) 0.0131(16) 0.066(2) 0.025(2)
F2 0.227(5) 0.138(4) 0.142(4) -0.047(3) 0.102(4) -0.095(4)
F3 0.151(4) 0.128(3) 0.099(3) 0.034(2) 0.045(3) 0.051(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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
O3 Ag S2 119.83(9) . . yes
O3 Ag S1 103.75(10) . . yes
S2 Ag S1 129.92(4) . . yes
C8 S1 C7 102.5(2) . . ?
C8 S1 Ag 104.08(16) . . ?
C7 S1 Ag 103.39(14) . . ?
C13 S2 C14 102.8(2) . . ?
C13 S2 Ag 102.23(17) . . ?
C14 S2 Ag 107.88(12) . . ?
C9 O1 C10 110.6(4) . . ?
C12 O2 C11 115.8(5) . . ?
C6 C1 C2 120.5(6) . . ?
C3 C2 C1 121.7(7) . . ?
C2 C3 C4 119.4(7) . . ?
C3 C4 C5 119.9(7) . . ?
C6 C5 C4 120.5(6) . . ?
C1 C6 C5 118.0(5) . . ?
C1 C6 C7 121.9(5) . . ?
C5 C6 C7 120.0(5) . . ?
C6 C7 S1 112.4(3) . . ?
C9 C8 S1 115.0(3) . . ?
O1 C9 C8 108.2(4) . . ?
O1 C10 C11 107.8(5) . . ?
O2 C11 C10 112.7(5) . . ?
O2 C12 C13 109.2(4) . . ?
C12 C13 S2 115.4(3) . . ?
C15 C14 S2 112.4(3) . . ?
C16 C15 C20 118.4(4) . . ?
C16 C15 C14 120.3(4) . . ?
C20 C15 C14 121.3(4) . . ?
C15 C16 C17 121.4(4) . . ?
C18 C17 C16 118.5(5) . . ?
C19 C18 C17 120.6(5) . . ?
C18 C19 C20 120.8(5) . . ?
C19 C20 C15 120.3(5) . . ?
N O3 Ag 118.1(3) . . ?
O3 N O3 120.6(6) 2_453 . ?
O3 N O4 119.7(3) 2_453 . ?
O3 N O4 119.7(3) . . ?
F3 P F3 88.7(4) 2_454 . ?
F3 P F2 91.7(3) 2_454 2_454 ?
F3 P F2 179.5(3) . 2_454 ?
F3 P F2 179.5(3) 2_454 . ?
F3 P F2 91.7(3) . . ?
F2 P F2 87.8(5) 2_454 . ?
F3 P F1 90.7(2) 2_454 . ?
F3 P F1 89.2(2) . . ?
F2 P F1 90.7(2) 2_454 . ?
F2 P F1 89.4(2) . . ?
F3 P F1 89.2(2) 2_454 2_454 ?
F3 P F1 90.7(2) . 2_454 ?
F2 P F1 89.4(2) 2_454 2_454 ?
F2 P F1 90.7(2) . 2_454 ?
F1 P F1 179.9(4) . 2_454 ?
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
Ag O3 2.409(4) . yes
Ag S2 2.4952(10) . yes
Ag S1 2.5117(10) . yes
S1 C8 1.803(4) . ?
S1 C7 1.832(5) . ?
S2 C13 1.805(5) . ?
S2 C14 1.826(4) . ?
O1 C9 1.390(6) . ?
O1 C10 1.437(7) . ?
O2 C12 1.418(6) . ?
O2 C11 1.437(6) . ?
C1 C6 1.375(8) . ?
C1 C2 1.386(9) . ?
C2 C3 1.358(11) . ?
C3 C4 1.364(12) . ?
C4 C5 1.407(10) . ?
C5 C6 1.395(7) . ?
C6 C7 1.506(6) . ?
C8 C9 1.485(6) . ?
C10 C11 1.444(9) . ?
C12 C13 1.489(8) . ?
C14 C15 1.500(5) . ?
C15 C16 1.381(7) . ?
C15 C20 1.390(6) . ?
C16 C17 1.389(7) . ?
C17 C18 1.384(8) . ?
C18 C19 1.358(10) . ?
C19 C20 1.374(8) . ?
O3 N 1.230(5) . ?
O4 N 1.235(8) . ?
N O3 1.230(5) 2_453 ?
P F3 1.567(4) 2_454 ?
P F3 1.567(4) . ?
P F2 1.575(4) 2_454 ?
P F2 1.575(4) . ?
P F1 1.592(3) . ?
P F1 1.592(3) 2_454 ?
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
O1 C10 C11 O2 61.8(8) . . . . yes
O1 C9 C8 S1 -62.6(5) . . . . yes
O2 C12 C13 S2 63.2(5) . . . . yes
N O3 Ag S1 170.1(3) . . . . yes
N O3 Ag S2 15.7(4) . . . . yes
|
1501458.cif | #------------------------------------------------------------------------------
#$Date: 2023-12-04 14:50:57 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501458.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_1501458
loop_
_publ_author_name
'Theivanayagam C. Deivaraj'
'Wei Hoon Lye'
'Jagadese J. Vittal'
_publ_contact_author_address
; Department of Chemistry
National University of Singapore
Kent Ridge
Singapore 117543
;
_publ_contact_author_email chmjjv@nus.edu.sg
_publ_contact_author_fax '(65) 874 2975'
_publ_contact_author_name 'Jagadese J. Vittal'
_publ_contact_author_phone '(65) 779 1691'
_publ_section_title
;
New Metalloligands [M(SC{O}Ph)4]-: Synthesis and Characterization of
Polymeric [A(MeCN)x{M(SC{O}Ph)4}] Compounds (A = Li, Na and K; M = Ga and
In; x= 0-2)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3755
_journal_page_last 3760
_journal_paper_doi 10.1021/ic025533i
_journal_volume 41
_journal_year 2002
_chemical_formula_sum 'C32 H26 K N2 O4 S4'
_chemical_formula_weight 784.71
_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 geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 92.356(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.307(3)
_cell_length_b 13.672(3)
_cell_length_c 20.575(4)
_cell_measurement_reflns_used 8192
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 25.0
_cell_measurement_theta_min 2.06
_cell_volume 3459.0(13)
_computing_cell_refinement 'Bruker AXS, SAINT'
_computing_data_collection 'Bruker AXS, SMART'
_computing_data_reduction 'Bruker AXS, SAINT'
_computing_molecular_graphics 'Bruker AXS, SHELXTL'
_computing_publication_material 'Bruker AXS, SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 223(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_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 0.0345
_diffrn_reflns_av_sigmaI/netI 0.0503
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 21042
_diffrn_reflns_theta_full 28.40
_diffrn_reflns_theta_max 28.40
_diffrn_reflns_theta_min 1.79
_exptl_absorpt_coefficient_mu 1.083
_exptl_absorpt_correction_T_max 0.9805
_exptl_absorpt_correction_T_min 0.7079
_exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.507
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'plates, cut'
_exptl_crystal_F_000 1584
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.791
_refine_diff_density_min -0.330
_refine_diff_density_rms 0.071
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.885
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 399
_refine_ls_number_reflns 7870
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.885
_refine_ls_R_factor_all 0.0479
_refine_ls_R_factor_gt 0.0349
_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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.0677
_reflns_number_gt 5896
_reflns_number_total 7870
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic025533i_s1_1.cif
_cod_data_source_block compound6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume 3458.8(12)
_cod_original_formula_sum 'C32 H26 K N2 O4 S4'
_cod_database_code 1501458
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
In1 In 0.554999(14) 0.228321(13) 0.220503(9) 0.03393(6) Uani 1 1 d . . .
K1 K 0.75709(4) 0.47198(4) 0.30440(3) 0.03944(14) Uani 1 1 d . . .
S1 S 0.68113(5) 0.22993(5) 0.13123(3) 0.04275(17) Uani 1 1 d . . .
S2 S 0.39488(5) 0.33901(5) 0.19808(3) 0.04127(17) Uani 1 1 d . . .
S3 S 0.46139(5) 0.06536(5) 0.21631(3) 0.04133(17) Uani 1 1 d . . .
S4 S 0.59837(6) 0.25250(5) 0.33851(3) 0.04109(17) Uani 1 1 d . . .
O1 O 0.79291(13) 0.32028(13) 0.22456(9) 0.0433(4) Uani 1 1 d . . .
O2 O 0.57948(12) 0.42502(12) 0.22223(8) 0.0409(4) Uani 1 1 d . . .
O3 O 0.45247(15) 0.14298(14) 0.09998(9) 0.0539(5) Uani 1 1 d . . .
O4 O 0.70482(13) 0.10651(13) 0.29055(8) 0.0411(4) Uani 1 1 d . . .
C1 C 0.78835(19) 0.29932(18) 0.16709(13) 0.0347(6) Uani 1 1 d . . .
C2 C 0.48168(19) 0.43835(18) 0.20965(11) 0.0327(6) Uani 1 1 d . . .
C3 C 0.4163(2) 0.07934(19) 0.13443(13) 0.0376(6) Uani 1 1 d . . .
C4 C 0.68960(19) 0.15381(18) 0.34000(12) 0.0344(6) Uani 1 1 d . . .
N1 N 0.9055(2) 0.38477(19) 0.39508(13) 0.0578(7) Uani 1 1 d . . .
C5 C 0.9664(2) 0.3353(2) 0.42105(14) 0.0485(7) Uani 1 1 d . . .
C6 C 1.0443(3) 0.2711(2) 0.45536(16) 0.0656(9) Uani 1 1 d . . .
H6A H 1.1176 0.2885 0.4440 0.098 Uiso 1 1 calc R . .
H6B H 1.0298 0.2037 0.4430 0.098 Uiso 1 1 calc R . .
H6C H 1.0374 0.2783 0.5019 0.098 Uiso 1 1 calc R . .
C7 C 0.5040(3) 0.5975(2) 0.37778(15) 0.0537(8) Uani 1 1 d . . .
N2 N 0.5790(2) 0.5524(2) 0.36986(13) 0.0626(7) Uani 1 1 d . . .
C8 C 0.4084(2) 0.6569(2) 0.38706(19) 0.0750(11) Uani 1 1 d . . .
H8A H 0.3588 0.6507 0.3494 0.112 Uiso 1 1 calc R . .
H8B H 0.4298 0.7248 0.3924 0.112 Uiso 1 1 calc R . .
H8C H 0.3725 0.6350 0.4256 0.112 Uiso 1 1 calc R . .
C1A C 0.87272(19) 0.33515(17) 0.12229(13) 0.0356(6) Uani 1 1 d . . .
C2A C 0.9550(2) 0.39439(19) 0.14820(15) 0.0479(7) Uani 1 1 d . . .
H2A H 0.9567 0.4105 0.1926 0.058 Uiso 1 1 calc R . .
C3A C 1.0345(2) 0.4299(2) 0.10896(19) 0.0609(9) Uani 1 1 d . . .
H3A H 1.0897 0.4703 0.1269 0.073 Uiso 1 1 calc R . .
C4A C 1.0336(2) 0.4068(2) 0.04426(19) 0.0605(9) Uani 1 1 d . . .
H4A H 1.0885 0.4306 0.0181 0.073 Uiso 1 1 calc R . .
C5A C 0.9526(3) 0.3488(2) 0.01766(16) 0.0582(8) Uani 1 1 d . . .
H5A H 0.9516 0.3334 -0.0269 0.070 Uiso 1 1 calc R . .
C6A C 0.8716(2) 0.3126(2) 0.05655(14) 0.0463(7) Uani 1 1 d . . .
H6A1 H 0.8162 0.2728 0.0382 0.056 Uiso 1 1 calc R . .
C1B C 0.43702(19) 0.53978(18) 0.20492(12) 0.0334(6) Uani 1 1 d . . .
C2B C 0.5080(2) 0.61799(19) 0.21433(12) 0.0414(6) Uani 1 1 d . . .
H2B H 0.5830 0.6064 0.2201 0.050 Uiso 1 1 calc R . .
C3B C 0.4693(3) 0.7122(2) 0.21520(14) 0.0522(8) Uani 1 1 d . . .
H3B H 0.5178 0.7648 0.2216 0.063 Uiso 1 1 calc R . .
C4B C 0.3600(3) 0.7295(2) 0.20670(16) 0.0630(9) Uani 1 1 d . . .
H4B H 0.3336 0.7939 0.2084 0.076 Uiso 1 1 calc R . .
C5B C 0.2887(2) 0.6532(2) 0.19563(16) 0.0598(9) Uani 1 1 d . . .
H5B H 0.2140 0.6657 0.1886 0.072 Uiso 1 1 calc R . .
C6B C 0.3270(2) 0.5580(2) 0.19479(14) 0.0458(7) Uani 1 1 d . . .
H6B1 H 0.2784 0.5057 0.1874 0.055 Uiso 1 1 calc R . .
C1C C 0.32943(19) 0.01217(18) 0.10830(12) 0.0355(6) Uani 1 1 d . . .
C2C C 0.2618(2) -0.03948(18) 0.14786(13) 0.0390(6) Uani 1 1 d . . .
H2C H 0.2739 -0.0374 0.1933 0.047 Uiso 1 1 calc R . .
C3C C 0.1768(2) -0.09400(19) 0.12138(15) 0.0471(7) Uani 1 1 d . . .
H3C H 0.1307 -0.1283 0.1487 0.057 Uiso 1 1 calc R . .
C4C C 0.1596(2) -0.0981(2) 0.05504(16) 0.0581(8) Uani 1 1 d . . .
H4C H 0.1006 -0.1340 0.0370 0.070 Uiso 1 1 calc R . .
C5C C 0.2285(3) -0.0496(2) 0.01493(16) 0.0658(9) Uani 1 1 d . . .
H5C H 0.2182 -0.0545 -0.0305 0.079 Uiso 1 1 calc R . .
C6C C 0.3124(2) 0.0061(2) 0.04147(14) 0.0541(8) Uani 1 1 d . . .
H6C1 H 0.3584 0.0402 0.0140 0.065 Uiso 1 1 calc R . .
C1D C 0.74630(18) 0.12916(18) 0.40320(12) 0.0334(6) Uani 1 1 d . . .
C2D C 0.7977(2) 0.03900(19) 0.40867(13) 0.0436(7) Uani 1 1 d . . .
H2D H 0.7973 -0.0035 0.3728 0.052 Uiso 1 1 calc R . .
C3D C 0.8497(2) 0.0114(2) 0.46677(15) 0.0539(8) Uani 1 1 d . . .
H3D H 0.8827 -0.0504 0.4707 0.065 Uiso 1 1 calc R . .
C4D C 0.8526(2) 0.0749(3) 0.51864(14) 0.0582(9) Uani 1 1 d . . .
H4D H 0.8881 0.0562 0.5580 0.070 Uiso 1 1 calc R . .
C5D C 0.8044(2) 0.1651(2) 0.51355(14) 0.0540(8) Uani 1 1 d . . .
H5D H 0.8083 0.2085 0.5490 0.065 Uiso 1 1 calc R . .
C6D C 0.7499(2) 0.1924(2) 0.45612(12) 0.0410(6) Uani 1 1 d . . .
H6D H 0.7154 0.2536 0.4530 0.049 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
In1 0.03436(10) 0.03701(11) 0.03027(11) -0.00125(8) -0.00037(7) 0.00273(8)
K1 0.0425(3) 0.0398(3) 0.0358(3) -0.0002(3) -0.0019(3) 0.0009(3)
S1 0.0385(4) 0.0549(4) 0.0351(4) -0.0106(3) 0.0041(3) -0.0074(3)
S2 0.0370(4) 0.0372(4) 0.0488(4) 0.0009(3) -0.0070(3) 0.0002(3)
S3 0.0480(4) 0.0374(4) 0.0377(4) 0.0024(3) -0.0090(3) -0.0017(3)
S4 0.0463(4) 0.0449(4) 0.0318(4) -0.0026(3) -0.0017(3) 0.0106(3)
O1 0.0403(10) 0.0537(12) 0.0356(11) -0.0097(9) -0.0005(9) 0.0009(9)
O2 0.0323(10) 0.0416(11) 0.0484(12) 0.0016(9) -0.0043(9) 0.0058(8)
O3 0.0633(13) 0.0530(13) 0.0446(12) 0.0111(10) -0.0070(10) -0.0190(10)
O4 0.0443(10) 0.0469(11) 0.0318(10) -0.0068(9) -0.0022(8) 0.0061(9)
C1 0.0329(13) 0.0344(14) 0.0367(16) -0.0029(12) 0.0007(12) 0.0081(11)
C2 0.0339(14) 0.0388(15) 0.0255(14) 0.0019(11) 0.0014(11) 0.0025(11)
C3 0.0399(14) 0.0367(15) 0.0357(16) 0.0006(12) -0.0040(12) 0.0038(12)
C4 0.0325(13) 0.0367(15) 0.0340(15) 0.0021(12) 0.0021(11) -0.0063(11)
N1 0.0547(15) 0.0633(18) 0.0550(17) 0.0070(14) -0.0006(13) 0.0031(14)
C5 0.0490(17) 0.058(2) 0.0389(18) 0.0027(15) 0.0067(14) -0.0024(15)
C6 0.059(2) 0.082(2) 0.057(2) 0.0160(18) 0.0025(17) 0.0130(18)
C7 0.0506(19) 0.057(2) 0.053(2) -0.0050(16) 0.0024(16) -0.0157(16)
N2 0.0534(16) 0.080(2) 0.0547(18) -0.0060(15) 0.0024(14) 0.0014(15)
C8 0.054(2) 0.053(2) 0.119(3) -0.015(2) 0.017(2) -0.0110(17)
C1A 0.0317(13) 0.0309(14) 0.0444(17) -0.0010(12) 0.0030(12) 0.0083(11)
C2A 0.0423(16) 0.0430(17) 0.058(2) -0.0032(14) -0.0001(15) -0.0026(13)
C3A 0.0434(18) 0.0465(19) 0.093(3) 0.0060(18) 0.0066(18) -0.0073(14)
C4A 0.0503(19) 0.0451(19) 0.088(3) 0.0185(18) 0.0262(19) 0.0052(15)
C5A 0.067(2) 0.058(2) 0.051(2) 0.0064(16) 0.0217(17) 0.0068(17)
C6A 0.0488(17) 0.0457(17) 0.0452(18) -0.0037(14) 0.0091(14) -0.0003(14)
C1B 0.0352(14) 0.0377(15) 0.0276(14) 0.0054(11) 0.0024(11) 0.0043(11)
C2B 0.0434(15) 0.0429(16) 0.0376(16) 0.0070(13) -0.0013(12) 0.0012(13)
C3B 0.063(2) 0.0383(18) 0.055(2) 0.0082(14) -0.0003(16) -0.0020(15)
C4B 0.075(2) 0.0391(18) 0.075(2) 0.0136(16) 0.0049(19) 0.0184(18)
C5B 0.0398(16) 0.060(2) 0.080(2) 0.0188(18) 0.0077(16) 0.0188(16)
C6B 0.0386(15) 0.0439(17) 0.0550(19) 0.0123(14) 0.0023(14) 0.0044(13)
C1C 0.0387(14) 0.0329(14) 0.0344(15) -0.0022(11) -0.0023(12) 0.0047(11)
C2C 0.0477(15) 0.0341(15) 0.0348(16) -0.0004(12) -0.0034(13) 0.0021(12)
C3C 0.0442(16) 0.0397(17) 0.058(2) 0.0014(14) 0.0034(15) -0.0057(13)
C4C 0.0507(18) 0.057(2) 0.065(2) -0.0163(17) -0.0101(17) -0.0095(15)
C5C 0.069(2) 0.088(3) 0.0403(19) -0.0136(18) -0.0059(17) -0.017(2)
C6C 0.0578(18) 0.068(2) 0.0362(18) -0.0039(15) 0.0029(15) -0.0154(16)
C1D 0.0317(13) 0.0394(15) 0.0290(14) 0.0033(11) -0.0007(11) -0.0073(11)
C2D 0.0472(16) 0.0409(16) 0.0420(17) 0.0019(13) -0.0062(13) -0.0023(13)
C3D 0.0538(18) 0.0536(19) 0.053(2) 0.0149(16) -0.0107(15) 0.0046(15)
C4D 0.0512(18) 0.086(3) 0.0367(18) 0.0159(17) -0.0104(15) -0.0027(17)
C5D 0.0512(17) 0.078(2) 0.0322(17) -0.0050(15) -0.0046(14) -0.0070(17)
C6D 0.0392(15) 0.0510(17) 0.0328(16) -0.0001(13) 0.0006(12) -0.0018(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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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
S1 In1 S4 127.80(3) . . ?
S1 In1 S3 106.62(2) . . ?
S4 In1 S3 103.39(2) . . ?
S1 In1 S2 111.88(3) . . ?
S4 In1 S2 103.56(2) . . ?
S3 In1 S2 99.97(3) . . ?
O1 K1 O4 92.58(6) . 2_655 ?
O1 K1 O2 66.17(5) . . ?
O4 K1 O2 82.80(5) 2_655 . ?
O1 K1 N1 87.72(7) . . ?
O4 K1 N1 129.11(6) 2_655 . ?
O2 K1 N1 140.83(7) . . ?
O1 K1 N2 137.39(7) . . ?
O4 K1 N2 103.68(7) 2_655 . ?
O2 K1 N2 77.01(7) . . ?
N1 K1 N2 109.95(8) . . ?
O1 K1 S4 65.67(4) . . ?
O4 K1 S4 142.67(4) 2_655 . ?
O2 K1 S4 61.04(4) . . ?
N1 K1 S4 82.12(5) . . ?
N2 K1 S4 78.36(6) . . ?
O1 K1 S3 91.02(4) . 2_655 ?
O4 K1 S3 60.12(4) 2_655 2_655 ?
O2 K1 S3 135.97(4) . 2_655 ?
N1 K1 S3 68.99(5) . 2_655 ?
N2 K1 S3 131.27(6) . 2_655 ?
S4 K1 S3 143.76(2) . 2_655 ?
C1 S1 In1 100.21(9) . . ?
C2 S2 In1 88.43(8) . . ?
C3 S3 In1 93.59(9) . . ?
C3 S3 K1 100.68(9) . 2_645 ?
In1 S3 K1 83.14(2) . 2_645 ?
C4 S4 In1 91.51(9) . . ?
C4 S4 K1 106.69(8) . . ?
In1 S4 K1 90.95(2) . . ?
C1 O1 K1 140.59(17) . . ?
C2 O2 K1 145.92(16) . . ?
C4 O4 K1 169.34(17) . 2_645 ?
O1 C1 C1A 121.0(2) . . ?
O1 C1 S1 122.5(2) . . ?
C1A C1 S1 116.37(19) . . ?
O2 C2 C1B 120.3(2) . . ?
O2 C2 S2 120.12(19) . . ?
C1B C2 S2 119.62(18) . . ?
O3 C3 C1C 120.2(2) . . ?
O3 C3 S3 121.7(2) . . ?
C1C C3 S3 118.05(19) . . ?
O4 C4 C1D 121.5(2) . . ?
O4 C4 S4 120.69(19) . . ?
C1D C4 S4 117.76(19) . . ?
C5 N1 K1 165.1(2) . . ?
N1 C5 C6 179.3(3) . . ?
N2 C7 C8 178.9(4) . . ?
C7 N2 K1 158.8(3) . . ?
C2A C1A C6A 118.9(3) . . ?
C2A C1A C1 117.9(2) . . ?
C6A C1A C1 123.2(2) . . ?
C3A C2A C1A 120.3(3) . . ?
C4A C3A C2A 120.7(3) . . ?
C3A C4A C5A 119.9(3) . . ?
C4A C5A C6A 120.1(3) . . ?
C1A C6A C5A 120.1(3) . . ?
C6B C1B C2B 119.2(2) . . ?
C6B C1B C2 122.1(2) . . ?
C2B C1B C2 118.6(2) . . ?
C3B C2B C1B 120.5(3) . . ?
C4B C3B C2B 119.9(3) . . ?
C3B C4B C5B 120.5(3) . . ?
C4B C5B C6B 119.9(3) . . ?
C1B C6B C5B 119.9(3) . . ?
C2C C1C C6C 118.9(2) . . ?
C2C C1C C3 122.8(2) . . ?
C6C C1C C3 118.1(2) . . ?
C3C C2C C1C 120.6(3) . . ?
C4C C3C C2C 119.9(3) . . ?
C3C C4C C5C 120.2(3) . . ?
C4C C5C C6C 119.9(3) . . ?
C5C C6C C1C 120.5(3) . . ?
C2D C1D C6D 119.3(2) . . ?
C2D C1D C4 117.9(2) . . ?
C6D C1D C4 122.9(2) . . ?
C3D C2D C1D 120.3(3) . . ?
C4D C3D C2D 119.6(3) . . ?
C5D C4D C3D 120.8(3) . . ?
C4D C5D C6D 120.0(3) . . ?
C5D C6D C1D 120.0(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
In1 S1 2.4532(8) . ?
In1 S4 2.4865(8) . ?
In1 S3 2.5080(8) . ?
In1 S2 2.5122(8) . ?
K1 O1 2.6932(19) . ?
K1 O4 2.7376(19) 2_655 ?
K1 O2 2.7829(18) . ?
K1 N1 2.821(3) . ?
K1 N2 2.841(3) . ?
K1 S4 3.6640(11) . ?
K1 S3 3.7331(11) 2_655 ?
S1 C1 1.762(3) . ?
S2 C2 1.738(2) . ?
S3 C3 1.762(3) . ?
S3 K1 3.7331(11) 2_645 ?
S4 C4 1.755(3) . ?
O1 C1 1.216(3) . ?
O2 C2 1.234(3) . ?
O3 C3 1.218(3) . ?
O4 C4 1.226(3) . ?
O4 K1 2.7376(19) 2_645 ?
C1 C1A 1.499(3) . ?
C2 C1B 1.493(3) . ?
C3 C1C 1.493(3) . ?
C4 C1D 1.489(3) . ?
N1 C5 1.127(3) . ?
C5 C6 1.462(4) . ?
C7 N2 1.128(4) . ?
C7 C8 1.449(4) . ?
C1A C2A 1.386(3) . ?
C1A C6A 1.387(4) . ?
C2A C3A 1.382(4) . ?
C3A C4A 1.368(4) . ?
C4A C5A 1.370(4) . ?
C5A C6A 1.394(4) . ?
C1B C6B 1.383(3) . ?
C1B C2B 1.389(3) . ?
C2B C3B 1.373(4) . ?
C3B C4B 1.370(4) . ?
C4B C5B 1.376(4) . ?
C5B C6B 1.386(4) . ?
C1C C2C 1.382(3) . ?
C1C C6C 1.385(4) . ?
C2C C3C 1.379(3) . ?
C3C C4C 1.374(4) . ?
C4C C5C 1.377(4) . ?
C5C C6C 1.378(4) . ?
C1D C2D 1.388(3) . ?
C1D C6D 1.389(3) . ?
C2D C3D 1.385(4) . ?
C3D C4D 1.375(4) . ?
C4D C5D 1.371(4) . ?
C5D C6D 1.385(4) . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2023-12-04T14:50:13+02:00
;
Changed the atom site label from '1' to 'In1' in multiple data loops for
consistency and readability.
;
|
1501459.cif | #------------------------------------------------------------------------------
#$Date: 2023-12-04 14:50:57 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501459.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_1501459
loop_
_publ_author_name
'Theivanayagam C. Deivaraj'
'Wei Hoon Lye'
'Jagadese J. Vittal'
_publ_contact_author_address
; Department of Chemistry
National University of Singapore
Kent Ridge
Singapore 117543
;
_publ_contact_author_email chmjjv@nus.edu.sg
_publ_contact_author_fax '(65) 874 2975'
_publ_contact_author_name 'Jagadese J. Vittal'
_publ_contact_author_phone '(65) 779 1691'
_publ_section_title
;
New Metalloligands [M(SC{O}Ph)4]-: Synthesis and Characterization of
Polymeric [A(MeCN)x{M(SC{O}Ph)4}] Compounds (A = Li, Na and K; M = Ga and
In; x= 0-2)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3755
_journal_page_last 3760
_journal_paper_doi 10.1021/ic025533i
_journal_volume 41
_journal_year 2002
_chemical_formula_sum 'C28.75 H22 Li N0.5 O4.25 S4'
_chemical_formula_weight 692.47
_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 108.4260(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 24.5766(8)
_cell_length_b 13.2758(5)
_cell_length_c 19.9983(8)
_cell_measurement_reflns_used 3975
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 22.85
_cell_measurement_theta_min 2.20
_cell_volume 6190.4(4)
_computing_cell_refinement 'Bruker AXS, SAINT'
_computing_data_collection 'Bruker AXS, SMART'
_computing_data_reduction 'Bruker AXS, SAINT'
_computing_molecular_graphics 'Bruker AXS, SHELXTL'
_computing_publication_material 'Bruker AXS, SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 0.0557
_diffrn_reflns_av_sigmaI/netI 0.0557
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 17859
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.75
_exptl_absorpt_coefficient_mu 1.066
_exptl_absorpt_correction_T_max 0.8880
_exptl_absorpt_correction_T_min 0.6500
_exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.486
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'rectangular shape, cut'
_exptl_crystal_F_000 2784
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.940
_refine_diff_density_min -0.349
_refine_diff_density_rms 0.096
_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 346
_refine_ls_number_reflns 5451
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.099
_refine_ls_R_factor_all 0.0722
_refine_ls_R_factor_gt 0.0514
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1089
_refine_ls_wR_factor_ref 0.1166
_reflns_number_gt 4022
_reflns_number_total 5451
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic025533i_s1_2.cif
_cod_data_source_block compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'not measured' 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_formula_sum 'C28.75 H22 Li N0.50 O4.25 S4'
_cod_database_code 1501459
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
In1 In 0.675105(15) 0.69979(2) 0.696687(19) 0.05182(15) Uani 1 1 d . . .
S1 S 0.69230(7) 0.72104(9) 0.82442(7) 0.0643(4) Uani 1 1 d . . .
S2 S 0.60248(6) 0.56506(9) 0.64662(8) 0.0639(4) Uani 1 1 d . . .
S3 S 0.60154(6) 0.82996(9) 0.63901(8) 0.0670(4) Uani 1 1 d . . .
S4 S 0.74250(6) 0.68473(9) 0.62776(7) 0.0619(4) Uani 1 1 d . . .
O1 O 0.74223(15) 0.5714(2) 0.78714(17) 0.0596(9) Uani 1 1 d . . .
O2 O 0.69476(14) 0.4604(2) 0.65159(16) 0.0511(8) Uani 1 1 d . . .
O3 O 0.66608(15) 0.9398(2) 0.7460(2) 0.0635(9) Uani 1 1 d . . .
O4 O 0.76120(16) 0.8349(2) 0.71327(18) 0.0630(9) Uani 1 1 d . . .
C1 C 0.7335(2) 0.6138(3) 0.8384(3) 0.0516(12) Uani 1 1 d . . .
C2 C 0.6425(2) 0.4663(3) 0.6274(2) 0.0477(12) Uani 1 1 d . . .
C3 C 0.6213(2) 0.9351(3) 0.6955(3) 0.0629(14) Uani 1 1 d . . .
C4 C 0.7756(2) 0.7947(3) 0.6657(3) 0.0549(13) Uani 1 1 d . . .
Li1 Li 0.7545(3) 0.4522(5) 0.7374(4) 0.052(2) Uani 1 1 d . . .
C11 C 0.7594(2) 0.5748(3) 0.9107(2) 0.0499(12) Uani 1 1 d . . .
C12 C 0.8005(2) 0.5003(4) 0.9235(3) 0.0679(15) Uani 1 1 d . . .
H12 H 0.8110 0.4743 0.8857 0.082 Uiso 1 1 calc R . .
C13 C 0.8262(3) 0.4633(4) 0.9896(3) 0.0772(17) Uani 1 1 d . . .
H13 H 0.8546 0.4133 0.9974 0.093 Uiso 1 1 calc R . .
C14 C 0.8101(3) 0.5001(5) 1.0446(3) 0.086(2) Uani 1 1 d . . .
H14 H 0.8277 0.4751 1.0904 0.103 Uiso 1 1 calc R . .
C15 C 0.7691(3) 0.5717(5) 1.0339(3) 0.0846(19) Uani 1 1 d . . .
H15 H 0.7582 0.5959 1.0720 0.102 Uiso 1 1 calc R . .
C16 C 0.7429(2) 0.6097(4) 0.9665(3) 0.0664(15) Uani 1 1 d . . .
H16 H 0.7141 0.6589 0.9590 0.080 Uiso 1 1 calc R . .
C21 C 0.6095(2) 0.3872(3) 0.5782(3) 0.0567(13) Uani 1 1 d . . .
C22 C 0.5522(2) 0.3950(4) 0.5425(3) 0.0821(19) Uani 1 1 d . . .
H22 H 0.5320 0.4522 0.5492 0.098 Uiso 1 1 calc R . .
C23 C 0.5238(3) 0.3217(5) 0.4973(4) 0.116(3) Uani 1 1 d . . .
H23 H 0.4843 0.3277 0.4736 0.139 Uiso 1 1 calc R . .
C24 C 0.5531(3) 0.2396(5) 0.4868(5) 0.150(4) Uani 1 1 d . . .
H24 H 0.5341 0.1898 0.4545 0.180 Uiso 1 1 calc R . .
C25 C 0.6101(3) 0.2291(5) 0.5229(5) 0.139(4) Uani 1 1 d . . .
H25 H 0.6296 0.1709 0.5165 0.167 Uiso 1 1 calc R . .
C26 C 0.6390(3) 0.3021(4) 0.5682(4) 0.093(2) Uani 1 1 d . . .
H26 H 0.6783 0.2950 0.5925 0.112 Uiso 1 1 calc R . .
C31 C 0.5816(2) 1.0235(4) 0.6790(3) 0.0736(17) Uani 1 1 d . . .
C32 C 0.5977(3) 1.1085(4) 0.7168(4) 0.095(2) Uani 1 1 d . . .
H32 H 0.6334 1.1105 0.7524 0.115 Uiso 1 1 calc R . .
C33 C 0.5632(4) 1.1923(5) 0.7048(6) 0.143(4) Uani 1 1 d . . .
H33 H 0.5755 1.2506 0.7321 0.171 Uiso 1 1 calc R . .
C34 C 0.5124(4) 1.1913(6) 0.6546(6) 0.154(4) Uani 1 1 d . . .
H34 H 0.4886 1.2483 0.6466 0.185 Uiso 1 1 calc R . .
C35 C 0.4955(4) 1.1070(7) 0.6152(7) 0.207(6) Uani 1 1 d . . .
H35 H 0.4599 1.1058 0.5792 0.249 Uiso 1 1 calc R . .
C36 C 0.5303(3) 1.0230(5) 0.6279(5) 0.161(5) Uani 1 1 d . . .
H36 H 0.5182 0.9647 0.6006 0.194 Uiso 1 1 calc R . .
C41 C 0.8211(2) 0.8389(4) 0.6405(3) 0.0579(13) Uani 1 1 d . . .
C42 C 0.8575(3) 0.9105(4) 0.6814(3) 0.0794(17) Uani 1 1 d . . .
H42 H 0.8538 0.9287 0.7252 0.095 Uiso 1 1 calc R . .
C43 C 0.8989(3) 0.9551(5) 0.6591(5) 0.097(2) Uani 1 1 d . . .
H43 H 0.9235 1.0032 0.6878 0.117 Uiso 1 1 calc R . .
C44 C 0.9047(3) 0.9307(6) 0.5961(5) 0.105(2) Uani 1 1 d . . .
H44 H 0.9328 0.9622 0.5806 0.125 Uiso 1 1 calc R . .
C45 C 0.8693(3) 0.8595(7) 0.5550(4) 0.107(2) Uani 1 1 d . . .
H45 H 0.8732 0.8421 0.5112 0.128 Uiso 1 1 calc R . .
C46 C 0.8280(2) 0.8133(4) 0.5771(3) 0.0757(17) Uani 1 1 d . . .
H46 H 0.8044 0.7638 0.5487 0.091 Uiso 1 1 calc R . .
N1S N 1.0461(2) 1.3536(4) 0.8055(3) 0.162(5) Uiso 0.50 1 d PRD A -1
C1S C 1.0026(2) 1.3267(4) 0.7565(3) 0.162(5) Uiso 0.25 1 d PRD A -1
C2S C 0.9683(2) 1.2455(4) 0.7015(3) 0.162(5) Uiso 0.50 1 d PRD A -1
H2SA H 0.9468 1.2787 0.6580 0.243 Uiso 0.50 1 calc PR B -1
H2SB H 0.9420 1.2100 0.7206 0.243 Uiso 0.50 1 calc PR C -1
H2SC H 0.9950 1.1979 0.6922 0.243 Uiso 0.50 1 calc PR D -1
O1S O 1.0000 1.1882(13) 0.7500 0.173(7) Uiso 0.50 2 d SP E -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
In1 0.0586(3) 0.0427(2) 0.0505(2) -0.00257(16) 0.01208(18) 0.00517(16)
S1 0.0836(10) 0.0510(7) 0.0559(9) -0.0052(6) 0.0187(8) 0.0111(7)
S2 0.0559(8) 0.0526(7) 0.0794(10) -0.0105(7) 0.0158(7) 0.0016(6)
S3 0.0635(9) 0.0481(7) 0.0723(10) -0.0027(7) -0.0029(8) 0.0051(6)
S4 0.0750(10) 0.0522(7) 0.0600(9) -0.0133(6) 0.0236(8) -0.0030(7)
O1 0.078(2) 0.058(2) 0.044(2) -0.0073(16) 0.0202(18) 0.0074(18)
O2 0.045(2) 0.0496(18) 0.052(2) -0.0058(15) 0.0055(16) -0.0024(15)
O3 0.052(2) 0.057(2) 0.074(3) 0.0058(18) 0.009(2) 0.0005(17)
O4 0.079(3) 0.056(2) 0.061(2) -0.0137(17) 0.033(2) 0.0037(18)
C1 0.061(3) 0.043(3) 0.053(3) -0.005(2) 0.020(3) -0.009(2)
C2 0.055(3) 0.038(2) 0.045(3) 0.006(2) 0.009(2) -0.002(2)
C3 0.066(4) 0.044(3) 0.076(4) 0.010(3) 0.019(3) 0.002(3)
C4 0.060(3) 0.051(3) 0.050(3) 0.008(2) 0.012(3) 0.014(3)
Li1 0.064(5) 0.042(4) 0.048(5) 0.000(4) 0.014(4) 0.002(4)
C11 0.069(3) 0.040(3) 0.039(3) -0.005(2) 0.015(3) -0.008(2)
C12 0.096(4) 0.058(3) 0.045(3) -0.005(3) 0.016(3) 0.004(3)
C13 0.104(5) 0.058(3) 0.058(4) 0.006(3) 0.009(4) 0.001(3)
C14 0.123(6) 0.073(4) 0.056(4) 0.014(3) 0.019(4) -0.024(4)
C15 0.127(6) 0.083(4) 0.053(4) -0.001(3) 0.042(4) -0.007(4)
C16 0.090(4) 0.056(3) 0.058(4) 0.004(3) 0.030(3) -0.003(3)
C21 0.058(3) 0.038(3) 0.061(3) 0.000(2) 0.000(3) -0.002(2)
C22 0.063(4) 0.050(3) 0.104(5) -0.008(3) -0.016(3) 0.005(3)
C23 0.066(4) 0.072(4) 0.158(8) -0.033(4) -0.040(5) 0.003(3)
C24 0.110(6) 0.077(5) 0.191(10) -0.062(6) -0.054(6) 0.011(5)
C25 0.095(6) 0.079(5) 0.193(9) -0.073(5) -0.026(6) 0.013(4)
C26 0.059(4) 0.061(4) 0.131(6) -0.031(4) -0.011(4) 0.004(3)
C31 0.065(4) 0.045(3) 0.099(5) -0.002(3) 0.009(3) 0.002(3)
C32 0.087(5) 0.061(4) 0.116(6) -0.015(4) 0.001(4) 0.015(3)
C33 0.133(7) 0.072(5) 0.174(9) -0.031(5) -0.021(7) 0.038(5)
C34 0.137(8) 0.078(5) 0.211(12) -0.008(6) 0.001(8) 0.046(6)
C35 0.138(8) 0.096(6) 0.283(14) -0.018(8) -0.083(8) 0.058(6)
C36 0.093(6) 0.078(5) 0.237(11) -0.036(6) -0.057(6) 0.035(4)
C41 0.068(4) 0.045(3) 0.061(4) 0.001(2) 0.020(3) 0.010(3)
C42 0.089(4) 0.062(3) 0.094(5) -0.013(3) 0.038(4) -0.002(3)
C43 0.084(5) 0.078(4) 0.139(7) -0.006(4) 0.049(5) -0.016(4)
C44 0.089(5) 0.118(6) 0.122(7) 0.022(5) 0.054(5) -0.012(5)
C45 0.094(6) 0.153(7) 0.083(5) 0.010(5) 0.042(5) 0.005(5)
C46 0.073(4) 0.100(5) 0.057(4) 0.000(3) 0.024(3) -0.007(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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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
S1 In1 S4 131.25(5) . . ?
S1 In1 S2 111.27(5) . . ?
S4 In1 S2 103.75(5) . . ?
S1 In1 S3 105.08(5) . . ?
S4 In1 S3 108.19(5) . . ?
S2 In1 S3 89.38(5) . . ?
C1 S1 In1 88.46(17) . . ?
C2 S2 In1 104.10(16) . . ?
C3 S3 In1 103.77(19) . . ?
C4 S4 In1 89.58(19) . . ?
C1 O1 Li1 152.1(4) . . ?
C2 O2 Li1 141.8(4) . . ?
C3 O3 Li1 138.9(5) . 4_656 ?
C4 O4 Li1 152.4(4) . 4_656 ?
O1 C1 C11 120.9(4) . . ?
O1 C1 S1 119.1(4) . . ?
C11 C1 S1 119.9(4) . . ?
O2 C2 C21 120.1(4) . . ?
O2 C2 S2 123.5(4) . . ?
C21 C2 S2 116.4(4) . . ?
O3 C3 C31 119.4(5) . . ?
O3 C3 S3 123.8(4) . . ?
C31 C3 S3 116.7(4) . . ?
O4 C4 C41 121.4(5) . . ?
O4 C4 S4 119.5(4) . . ?
C41 C4 S4 119.1(4) . . ?
O2 Li1 O3 129.4(5) . 4_646 ?
O2 Li1 O1 102.6(4) . . ?
O3 Li1 O1 107.6(4) 4_646 . ?
O2 Li1 O4 106.6(4) . 4_646 ?
O3 Li1 O4 101.6(4) 4_646 4_646 ?
O1 Li1 O4 107.7(4) . 4_646 ?
C12 C11 C16 118.4(5) . . ?
C12 C11 C1 119.8(4) . . ?
C16 C11 C1 121.8(5) . . ?
C13 C12 C11 121.8(5) . . ?
C12 C13 C14 119.1(6) . . ?
C15 C14 C13 120.9(6) . . ?
C14 C15 C16 120.1(6) . . ?
C11 C16 C15 119.8(5) . . ?
C22 C21 C26 119.0(5) . . ?
C22 C21 C2 123.2(5) . . ?
C26 C21 C2 117.8(4) . . ?
C23 C22 C21 121.3(5) . . ?
C24 C23 C22 119.4(6) . . ?
C23 C24 C25 120.4(6) . . ?
C26 C25 C24 120.7(6) . . ?
C25 C26 C21 119.2(6) . . ?
C32 C31 C36 117.9(6) . . ?
C32 C31 C3 118.5(5) . . ?
C36 C31 C3 123.6(5) . . ?
C31 C32 C33 121.7(7) . . ?
C34 C33 C32 120.2(7) . . ?
C33 C34 C35 119.3(7) . . ?
C34 C35 C36 120.0(8) . . ?
C31 C36 C35 120.9(7) . . ?
C46 C41 C42 118.0(5) . . ?
C46 C41 C4 122.8(5) . . ?
C42 C41 C4 119.2(5) . . ?
C43 C42 C41 121.0(6) . . ?
C44 C43 C42 120.5(7) . . ?
C43 C44 C45 119.4(7) . . ?
C44 C45 C46 120.7(7) . . ?
C45 C46 C41 120.5(6) . . ?
N1S C1S C2S 151.0 . . ?
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
In1 S1 2.4700(14) . ?
In1 S4 2.4751(14) . ?
In1 S2 2.5015(13) . ?
In1 S3 2.5034(13) . ?
S1 C1 1.718(5) . ?
S2 C2 1.754(5) . ?
S3 C3 1.765(5) . ?
S4 C4 1.726(5) . ?
O1 C1 1.247(5) . ?
O1 Li1 1.943(8) . ?
O2 C2 1.223(5) . ?
O2 Li1 1.876(8) . ?
O3 C3 1.237(6) . ?
O3 Li1 1.880(9) 4_656 ?
O4 C4 1.237(6) . ?
O4 Li1 1.947(8) 4_656 ?
C1 C11 1.478(6) . ?
C2 C21 1.492(6) . ?
C3 C31 1.496(7) . ?
C4 C41 1.484(7) . ?
Li1 O3 1.880(9) 4_646 ?
Li1 O4 1.947(8) 4_646 ?
C11 C12 1.378(7) . ?
C11 C16 1.381(7) . ?
C12 C13 1.364(7) . ?
C13 C14 1.371(8) . ?
C14 C15 1.353(8) . ?
C15 C16 1.391(7) . ?
C21 C22 1.365(6) . ?
C21 C26 1.390(7) . ?
C22 C23 1.362(7) . ?
C23 C24 1.358(9) . ?
C24 C25 1.364(9) . ?
C25 C26 1.364(8) . ?
C31 C32 1.347(7) . ?
C31 C36 1.348(8) . ?
C32 C33 1.373(8) . ?
C33 C34 1.331(11) . ?
C34 C35 1.356(11) . ?
C35 C36 1.380(9) . ?
C41 C46 1.373(7) . ?
C41 C42 1.383(7) . ?
C42 C43 1.368(8) . ?
C43 C44 1.351(9) . ?
C44 C45 1.369(9) . ?
C45 C46 1.371(8) . ?
N1S C1S 1.2531 . ?
C1S C2S 1.5798 . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2023-12-04T14:50:13+02:00
;
Changed the atom site label from '1' to 'In1' in multiple data loops for
consistency and readability.
;
|
1501460.cif | #------------------------------------------------------------------------------
#$Date: 2023-12-04 14:50:57 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501460.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_1501460
loop_
_publ_author_name
'Theivanayagam C. Deivaraj'
'Wei Hoon Lye'
'Jagadese J. Vittal'
_publ_contact_author_address
; Department of Chemistry
National University of Singapore
Kent Ridge
Singapore 117543
;
_publ_contact_author_email chmjjv@nus.edu.sg
_publ_contact_author_fax '(65) 874 2975'
_publ_contact_author_name 'Jagadese J. Vittal'
_publ_contact_author_phone '(65) 779 1691'
_publ_section_title
;
New Metalloligands [M(SC{O}Ph)4]-: Synthesis and Characterization of
Polymeric [A(MeCN)x{M(SC{O}Ph)4}] Compounds (A = Li, Na and K; M = Ga and
In; x= 0-2)
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3755
_journal_page_last 3760
_journal_paper_doi 10.1021/ic025533i
_journal_volume 41
_journal_year 2002
_chemical_formula_sum 'C30 H23 N Na O4 S4'
_chemical_formula_weight 727.54
_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 110.121(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.5774(7)
_cell_length_b 21.9723(15)
_cell_length_c 14.4196(10)
_cell_measurement_reflns_used 5980
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 25.0
_cell_measurement_theta_min 2.06
_cell_volume 3146.7(4)
_computing_cell_refinement 'Bruker AXS, SAINT'
_computing_data_collection 'Bruker AXS, SMART'
_computing_data_reduction 'Bruker AXS, SAINT'
_computing_molecular_graphics 'Bruker AXS, SHELXTL'
_computing_publication_material 'Bruker AXS, SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 223(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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 0.0177
_diffrn_reflns_av_sigmaI/netI 0.0186
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 20502
_diffrn_reflns_theta_full 28.99
_diffrn_reflns_theta_max 28.99
_diffrn_reflns_theta_min 2.05
_exptl_absorpt_coefficient_mu 1.066
_exptl_absorpt_correction_T_max 0.8068
_exptl_absorpt_correction_T_min 0.6948
_exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.536
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'prism, cut'
_exptl_crystal_F_000 1464
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.22
_refine_diff_density_max 0.311
_refine_diff_density_min -0.316
_refine_diff_density_rms 0.045
_refine_ls_extinction_coef 0.00016(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 1.027
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 372
_refine_ls_number_reflns 7782
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.027
_refine_ls_R_factor_all 0.0364
_refine_ls_R_factor_gt 0.0250
_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^)+(0.0201P)^2^+1.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0514
_refine_ls_wR_factor_ref 0.0557
_reflns_number_gt 6342
_reflns_number_total 7782
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic025533i_s1_3.cif
_cod_data_source_block compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'not measured' 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_formula_sum 'C30 H23 N Na O4 S4'
_cod_database_code 1501460
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
In1 In 0.204943(13) 0.310613(6) -0.044119(9) 0.04027(5) Uani 1 1 d . . .
S1 S 0.15335(6) 0.22189(2) -0.15805(4) 0.05586(14) Uani 1 1 d . . .
S2 S 0.01712(5) 0.38346(3) -0.08219(4) 0.05221(13) Uani 1 1 d . . .
S3 S 0.33478(5) 0.26649(2) 0.11977(4) 0.04699(11) Uani 1 1 d . . .
S4 S 0.39075(5) 0.36106(2) -0.08348(4) 0.04872(12) Uani 1 1 d . . .
O1 O 0.06217(16) 0.18533(7) -0.02062(11) 0.0562(4) Uani 1 1 d . . .
O2 O 0.00962(16) 0.31163(7) 0.05865(12) 0.0604(4) Uani 1 1 d . . .
O3 O 0.31154(17) 0.38423(7) 0.12021(11) 0.0630(4) Uani 1 1 d . . .
O4 O 0.19804(13) 0.34962(6) -0.25453(10) 0.0467(3) Uani 1 1 d . . .
Na1 Na 0.06694(8) 0.21913(3) 0.13083(5) 0.04408(17) Uani 1 1 d . . .
N1 N -0.1310(2) 0.19694(12) 0.16724(17) 0.0756(6) Uani 1 1 d . . .
C5 C -0.1934(3) 0.20815(13) 0.2134(2) 0.0714(7) Uani 1 1 d . . .
C6 C -0.2728(4) 0.2243(2) 0.2749(3) 0.1306(15) Uani 1 1 d . . .
H6A H -0.2264 0.2557 0.3214 0.196 Uiso 1 1 calc R . .
H6B H -0.2844 0.1886 0.3108 0.196 Uiso 1 1 calc R . .
H6C H -0.3602 0.2393 0.2334 0.196 Uiso 1 1 calc R . .
C1 C 0.08487(18) 0.17121(8) -0.09520(13) 0.0401(4) Uani 1 1 d . . .
C2 C -0.03614(19) 0.35800(8) 0.01285(13) 0.0422(4) Uani 1 1 d . . .
C3 C 0.3640(2) 0.34007(9) 0.16983(14) 0.0450(4) Uani 1 1 d . . .
C4 C 0.31350(19) 0.36701(8) -0.21097(14) 0.0396(4) Uani 1 1 d . . .
C11 C 0.0555(2) 0.10852(8) -0.13676(13) 0.0425(4) Uani 1 1 d . . .
C12 C 0.1005(2) 0.08686(10) -0.21004(15) 0.0518(5) Uani 1 1 d . . .
H12 H 0.1521 0.1120 -0.2359 0.062 Uiso 1 1 calc R . .
C13 C 0.0692(3) 0.02788(11) -0.24536(18) 0.0655(6) Uani 1 1 d . . .
H13 H 0.1000 0.0133 -0.2951 0.079 Uiso 1 1 calc R . .
C14 C -0.0050(3) -0.00875(12) -0.2088(2) 0.0851(9) Uani 1 1 d . . .
H14 H -0.0253 -0.0486 -0.2329 0.102 Uiso 1 1 calc R . .
C15 C -0.0504(4) 0.01221(13) -0.1368(2) 0.1033(12) Uani 1 1 d . . .
H15 H -0.1021 -0.0133 -0.1116 0.124 Uiso 1 1 calc R . .
C16 C -0.0207(3) 0.07086(12) -0.1007(2) 0.0784(8) Uani 1 1 d . . .
H16 H -0.0528 0.0850 -0.0513 0.094 Uiso 1 1 calc R . .
C21 C -0.14081(18) 0.39421(8) 0.03557(13) 0.0396(4) Uani 1 1 d . . .
C22 C -0.2011(2) 0.36879(10) 0.09805(17) 0.0572(5) Uani 1 1 d . . .
H22 H -0.1771 0.3294 0.1234 0.069 Uiso 1 1 calc R . .
C23 C -0.2961(3) 0.40127(12) 0.1230(2) 0.0696(7) Uani 1 1 d . . .
H23 H -0.3371 0.3839 0.1650 0.084 Uiso 1 1 calc R . .
C24 C -0.3311(2) 0.45915(12) 0.08650(19) 0.0664(6) Uani 1 1 d . . .
H24 H -0.3960 0.4811 0.1039 0.080 Uiso 1 1 calc R . .
C25 C -0.2722(2) 0.48491(10) 0.02513(17) 0.0572(5) Uani 1 1 d . . .
H25 H -0.2965 0.5244 0.0003 0.069 Uiso 1 1 calc R . .
C26 C -0.1767(2) 0.45265(9) -0.00031(14) 0.0464(4) Uani 1 1 d . . .
H26 H -0.1358 0.4704 -0.0422 0.056 Uiso 1 1 calc R . .
C31 C 0.4605(2) 0.34686(9) 0.27232(14) 0.0453(4) Uani 1 1 d . . .
C32 C 0.4940(2) 0.29926(11) 0.33908(15) 0.0572(5) Uani 1 1 d . . .
H32 H 0.4512 0.2613 0.3217 0.069 Uiso 1 1 calc R . .
C33 C 0.5911(3) 0.30758(14) 0.43201(18) 0.0795(8) Uani 1 1 d . . .
H33 H 0.6136 0.2755 0.4779 0.095 Uiso 1 1 calc R . .
C34 C 0.6540(3) 0.36294(16) 0.4563(2) 0.0911(9) Uani 1 1 d . . .
H34 H 0.7218 0.3682 0.5182 0.109 Uiso 1 1 calc R . .
C35 C 0.6193(3) 0.41017(14) 0.3920(2) 0.0831(8) Uani 1 1 d . . .
H35 H 0.6621 0.4480 0.4099 0.100 Uiso 1 1 calc R . .
C36 C 0.5214(2) 0.40293(11) 0.30018(17) 0.0605(6) Uani 1 1 d . . .
H36 H 0.4962 0.4361 0.2565 0.073 Uiso 1 1 calc R . .
C41 C 0.3957(2) 0.39449(8) -0.26642(15) 0.0454(4) Uani 1 1 d . . .
C42 C 0.3417(2) 0.39760(10) -0.36817(16) 0.0557(5) Uani 1 1 d . . .
H42 H 0.2535 0.3838 -0.4011 0.067 Uiso 1 1 calc R . .
C43 C 0.4168(3) 0.42097(12) -0.4220(2) 0.0771(8) Uani 1 1 d . . .
H43 H 0.3798 0.4229 -0.4913 0.093 Uiso 1 1 calc R . .
C44 C 0.5459(3) 0.44140(14) -0.3736(2) 0.0863(9) Uani 1 1 d . . .
H44 H 0.5972 0.4571 -0.4100 0.104 Uiso 1 1 calc R . .
C45 C 0.5995(3) 0.43888(15) -0.2732(2) 0.0917(10) Uani 1 1 d . . .
H45 H 0.6873 0.4533 -0.2406 0.110 Uiso 1 1 calc R . .
C46 C 0.5254(2) 0.41515(12) -0.21864(19) 0.0678(7) Uani 1 1 d . . .
H46 H 0.5633 0.4131 -0.1494 0.081 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
In1 0.04394(8) 0.04024(7) 0.03691(7) 0.00104(5) 0.01428(5) 0.00087(6)
S1 0.0839(4) 0.0454(3) 0.0390(2) -0.0030(2) 0.0220(3) -0.0153(3)
S2 0.0518(3) 0.0620(3) 0.0456(3) 0.0117(2) 0.0203(2) 0.0139(2)
S3 0.0491(3) 0.0469(3) 0.0411(2) 0.0024(2) 0.0107(2) -0.0008(2)
S4 0.0464(3) 0.0547(3) 0.0459(3) -0.0088(2) 0.0168(2) -0.0108(2)
O1 0.0670(9) 0.0580(9) 0.0527(8) -0.0175(7) 0.0321(7) -0.0094(7)
O2 0.0680(10) 0.0477(8) 0.0714(10) 0.0181(7) 0.0316(8) 0.0210(7)
O3 0.0818(11) 0.0540(9) 0.0472(8) 0.0087(7) 0.0146(8) 0.0113(8)
O4 0.0436(7) 0.0471(7) 0.0502(7) -0.0071(6) 0.0172(6) -0.0093(6)
Na1 0.0520(4) 0.0428(4) 0.0403(4) 0.0068(3) 0.0196(3) 0.0092(3)
N1 0.0536(12) 0.1077(18) 0.0661(13) 0.0060(12) 0.0215(11) -0.0090(12)
C5 0.0539(14) 0.0805(18) 0.0764(17) 0.0166(14) 0.0182(13) 0.0010(12)
C6 0.115(3) 0.155(4) 0.153(4) 0.033(3) 0.086(3) 0.049(3)
C1 0.0400(10) 0.0427(9) 0.0356(9) -0.0035(7) 0.0105(8) 0.0011(7)
C2 0.0440(10) 0.0391(9) 0.0402(9) 0.0004(8) 0.0105(8) 0.0031(8)
C3 0.0465(11) 0.0511(11) 0.0408(10) 0.0014(8) 0.0195(8) 0.0016(9)
C4 0.0439(10) 0.0313(8) 0.0479(10) -0.0088(7) 0.0211(8) -0.0024(7)
C11 0.0479(11) 0.0392(10) 0.0393(9) -0.0036(7) 0.0138(8) -0.0017(8)
C12 0.0617(13) 0.0487(11) 0.0470(11) -0.0035(9) 0.0213(10) 0.0053(10)
C13 0.0830(17) 0.0539(13) 0.0567(13) -0.0144(11) 0.0203(12) 0.0103(12)
C14 0.124(3) 0.0460(13) 0.0789(18) -0.0156(13) 0.0272(18) -0.0147(15)
C15 0.158(3) 0.0670(18) 0.105(2) -0.0234(17) 0.070(2) -0.054(2)
C16 0.113(2) 0.0657(16) 0.0764(17) -0.0205(13) 0.0576(17) -0.0338(15)
C21 0.0391(10) 0.0391(9) 0.0381(9) -0.0020(7) 0.0102(8) 0.0014(7)
C22 0.0613(13) 0.0478(12) 0.0705(14) 0.0090(10) 0.0331(12) 0.0054(10)
C23 0.0684(16) 0.0728(16) 0.0839(17) 0.0019(13) 0.0471(14) 0.0023(12)
C24 0.0554(14) 0.0679(15) 0.0803(17) -0.0139(13) 0.0290(13) 0.0114(11)
C25 0.0559(13) 0.0437(11) 0.0663(14) -0.0059(10) 0.0136(11) 0.0102(10)
C26 0.0501(11) 0.0414(10) 0.0454(10) -0.0001(8) 0.0136(9) 0.0036(8)
C31 0.0469(11) 0.0544(12) 0.0383(9) 0.0009(8) 0.0194(8) 0.0003(9)
C32 0.0634(14) 0.0631(14) 0.0433(11) 0.0056(10) 0.0161(10) 0.0000(11)
C33 0.093(2) 0.089(2) 0.0459(13) 0.0092(13) 0.0101(13) 0.0129(16)
C34 0.091(2) 0.103(2) 0.0563(15) -0.0185(16) -0.0045(14) -0.0004(18)
C35 0.090(2) 0.0806(19) 0.0694(17) -0.0227(15) 0.0152(15) -0.0196(16)
C36 0.0721(15) 0.0595(13) 0.0515(12) -0.0065(10) 0.0233(11) -0.0082(11)
C41 0.0506(11) 0.0385(10) 0.0549(11) -0.0085(8) 0.0279(10) -0.0077(8)
C42 0.0658(14) 0.0495(12) 0.0564(12) -0.0033(10) 0.0269(11) -0.0140(10)
C43 0.107(2) 0.0724(17) 0.0652(15) -0.0012(13) 0.0466(16) -0.0240(15)
C44 0.098(2) 0.090(2) 0.096(2) -0.0052(17) 0.0654(19) -0.0316(17)
C45 0.0728(18) 0.117(3) 0.098(2) -0.0106(19) 0.0458(17) -0.0419(17)
C46 0.0568(14) 0.0854(17) 0.0669(15) -0.0092(13) 0.0287(12) -0.0242(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
In In -0.7276 1.3100 '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
S2 In1 S3 127.245(18) . . ?
S2 In1 S1 112.68(2) . . ?
S3 In1 S1 104.262(19) . . ?
S2 In1 S4 107.45(2) . . ?
S3 In1 S4 99.750(18) . . ?
S1 In1 S4 102.115(18) . . ?
C1 S1 In1 101.16(6) . . ?
C1 S1 Na1 137.14(7) . 4_565 ?
In1 S1 Na1 103.98(2) . 4_565 ?
C2 S2 In1 94.03(6) . . ?
C3 S3 In1 89.62(7) . . ?
C3 S3 Na1 109.03(7) . . ?
In1 S3 Na1 87.92(2) . . ?
C4 S4 In1 98.85(6) . . ?
C1 O1 Na1 167.54(14) . . ?
C2 O2 Na1 171.91(16) . . ?
C4 O4 Na1 144.61(12) . 4_565 ?
O2 Na1 O1 86.46(6) . . ?
O2 Na1 O4 155.77(7) . 4_566 ?
O1 Na1 O4 106.29(6) . 4_566 ?
O2 Na1 N1 99.69(8) . . ?
O1 Na1 N1 114.31(8) . . ?
O4 Na1 N1 93.74(7) 4_566 . ?
O2 Na1 S3 77.20(5) . . ?
O1 Na1 S3 77.21(4) . . ?
O4 Na1 S3 85.50(4) 4_566 . ?
N1 Na1 S3 168.06(7) . . ?
O2 Na1 S1 91.02(5) . 4_566 ?
O1 Na1 S1 164.00(5) . 4_566 ?
O4 Na1 S1 70.98(4) 4_566 4_566 ?
N1 Na1 S1 81.68(6) . 4_566 ?
S3 Na1 S1 86.82(3) . 4_566 ?
C5 N1 Na1 146.5(2) . . ?
N1 C5 C6 178.4(4) . . ?
O1 C1 C11 120.80(17) . . ?
O1 C1 S1 122.61(15) . . ?
C11 C1 S1 116.59(13) . . ?
O2 C2 C21 120.92(17) . . ?
O2 C2 S2 121.21(15) . . ?
C21 C2 S2 117.86(13) . . ?
O3 C3 C31 121.43(19) . . ?
O3 C3 S3 120.76(16) . . ?
C31 C3 S3 117.72(15) . . ?
O4 C4 C41 120.76(17) . . ?
O4 C4 S4 122.71(14) . . ?
C41 C4 S4 116.53(14) . . ?
C16 C11 C12 118.81(19) . . ?
C16 C11 C1 118.13(18) . . ?
C12 C11 C1 123.07(18) . . ?
C11 C12 C13 120.0(2) . . ?
C14 C13 C12 120.6(2) . . ?
C13 C14 C15 120.0(2) . . ?
C14 C15 C16 120.4(3) . . ?
C11 C16 C15 120.2(2) . . ?
C26 C21 C22 119.11(18) . . ?
C26 C21 C2 122.78(17) . . ?
C22 C21 C2 118.07(17) . . ?
C23 C22 C21 120.0(2) . . ?
C22 C23 C24 120.2(2) . . ?
C25 C24 C23 120.4(2) . . ?
C24 C25 C26 119.8(2) . . ?
C25 C26 C21 120.44(19) . . ?
C32 C31 C36 119.3(2) . . ?
C32 C31 C3 122.70(19) . . ?
C36 C31 C3 118.01(19) . . ?
C31 C32 C33 119.9(2) . . ?
C34 C33 C32 119.7(3) . . ?
C35 C34 C33 120.6(3) . . ?
C34 C35 C36 120.4(3) . . ?
C35 C36 C31 120.1(2) . . ?
C42 C41 C46 119.34(19) . . ?
C42 C41 C4 118.94(18) . . ?
C46 C41 C4 121.70(19) . . ?
C41 C42 C43 120.4(2) . . ?
C44 C43 C42 119.8(3) . . ?
C45 C44 C43 120.2(2) . . ?
C44 C45 C46 120.5(3) . . ?
C41 C46 C45 119.8(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
In1 S2 2.4617(5) . ?
In1 S3 2.4856(5) . ?
In1 S1 2.4859(5) . ?
In1 S4 2.4861(5) . ?
S1 C1 1.7429(19) . ?
S1 Na1 3.1413(9) 4_565 ?
S2 C2 1.7434(19) . ?
S3 C3 1.754(2) . ?
S3 Na1 3.0733(9) . ?
S4 C4 1.7409(19) . ?
O1 C1 1.220(2) . ?
O1 Na1 2.2908(15) . ?
O2 C2 1.220(2) . ?
O2 Na1 2.2688(15) . ?
O3 C3 1.220(2) . ?
O4 C4 1.226(2) . ?
O4 Na1 2.3152(14) 4_565 ?
Na1 O4 2.3152(14) 4_566 ?
Na1 N1 2.377(2) . ?
Na1 S1 3.1413(9) 4_566 ?
N1 C5 1.114(3) . ?
C5 C6 1.459(4) . ?
C1 C11 1.492(3) . ?
C2 C21 1.488(3) . ?
C3 C31 1.487(3) . ?
C4 C41 1.496(3) . ?
C11 C16 1.376(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.352(4) . ?
C14 C15 1.365(4) . ?
C15 C16 1.385(4) . ?
C21 C26 1.388(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.377(3) . ?
C23 C24 1.377(3) . ?
C24 C25 1.368(3) . ?
C25 C26 1.383(3) . ?
C31 C32 1.383(3) . ?
C31 C36 1.384(3) . ?
C32 C33 1.392(3) . ?
C33 C34 1.373(4) . ?
C34 C35 1.356(4) . ?
C35 C36 1.380(3) . ?
C41 C42 1.381(3) . ?
C41 C46 1.383(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.377(4) . ?
C44 C45 1.363(4) . ?
C45 C46 1.389(3) . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2023-12-04T14:50:13+02:00
;
Changed the atom site label from '1' to 'In1' in multiple data loops for
consistency and readability.
;
|
1501461.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-15 03:23:08 +0300 (Sun, 15 Oct 2017) $
#$Revision: 202022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501461.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_1501461
loop_
_publ_author_name
'Krzton-Maziopa, A.'
'Shermadini, Z.'
'Pomjakushina, E.'
'Pomjakushina, V.'
'Bendele, M.'
'Amato, A.'
'Khasanov, R.'
'Luetkens, H.'
'Conder, K.'
_publ_section_title
;
Synthesis and crystal growth of Cs0.8(FeSe0.98)2: a new iron-based
superconductor with Tc=27K
;
_journal_name_full
;
Journal of Physics: Condensed Matter
;
_journal_page_first 1
_journal_page_last 4
_journal_volume 23
_journal_year 2011
_chemical_formula_structural 'K0.8 (FeSe0.98)2'
_chemical_formula_sum 'Fe2 K0.8 Se1.96'
_space_group_IT_number 139
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4 2'
_symmetry_space_group_name_H-M 'I 4/m m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 3.9092
_cell_length_b 3.9092
_cell_length_c 14.1353
_cell_volume 216.013
_refine_ls_R_factor_all 0.051
_cod_data_source_file K0.8FeSe0.982.cif
_cod_data_source_block chateigner1
_cod_original_formula_sum 'K0.8 Fe2 Se1.96'
_cod_database_code 1501461
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
-x,y,z
x,-y,z
-y,x,z
y,-x,z
y,x,z
-y,-x,z
-x,-y,-z
x,y,-z
x,-y,-z
-x,y,-z
y,-x,-z
-y,x,-z
-y,-x,-z
y,x,-z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+z
1/2-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+y,1/2+x,1/2+z
1/2-y,1/2-x,1/2+z
1/2-x,1/2-y,1/2-z
1/2+x,1/2+y,1/2-z
1/2+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-y,1/2-x,1/2-z
1/2+y,1/2+x,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Fe1 Fe2+ 4 d 0. 0.5 0.25 1. 0 d
Se1 Se2- 4 e 0. 0. 0.3503 1. 0 d
K1 K+ 2 a 0. 0. 0. 0.792 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe2+ 2.000
Se2- -2.000
K+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 MPOD 1000195
|
1501462.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-15 03:23:08 +0300 (Sun, 15 Oct 2017) $
#$Revision: 202022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501462.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_1501462
loop_
_publ_author_name
'Krzton-Maziopa, A.'
'Shermadini, Z.'
'Pomjakushina, E.'
'Pomjakushina, V.'
'Bendele, M.'
'Amato, A.'
'Khasanov, R.'
'Luetkens, H.'
'Conder, K.'
_publ_section_title
;
Synthesis and crystal growth of Cs0.8(FeSe0.98)2: a new iron-based
superconductor with Tc=27K
;
_journal_name_full
;
Journal of Physics: Condensed Matter
;
_journal_page_first 1
_journal_page_last 4
_journal_volume 23
_journal_year 2011
_chemical_formula_structural 'Cs0.8 (FeSe0.98)2'
_chemical_formula_sum 'Cs0.8 Fe2 Se1.96'
_space_group_IT_number 139
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4 2'
_symmetry_space_group_name_H-M 'I 4/m m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 3.9601
_cell_length_b 3.9601
_cell_length_c 15.2846
_cell_volume 239.699
_cod_data_source_file Cs0_8FeSe0_982.cif
_cod_data_source_block chateigner2
_cod_database_code 1501462
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
-x,y,z
x,-y,z
-y,x,z
y,-x,z
y,x,z
-y,-x,z
-x,-y,-z
x,y,-z
x,-y,-z
-x,y,-z
y,-x,-z
-y,x,-z
-y,-x,-z
y,x,-z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+z
1/2-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+y,1/2+x,1/2+z
1/2-y,1/2-x,1/2+z
1/2-x,1/2-y,1/2-z
1/2+x,1/2+y,1/2-z
1/2+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-y,1/2-x,1/2-z
1/2+y,1/2+x,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Fe1 Fe2+ 4 d 0. 0.5 0.25 1. 0 d
Se1 Se2- 4 e 0. 0. 0.3439 1. 0 d
Cs1 Cs+ 2 a 0. 0. 0. 0.771 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe2+ 2.000
Se2- -2.000
Cs+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 MPOD 1000194
|
1501463.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501463.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_1501463
loop_
_publ_author_name
'Lejaeghere, Kurt'
'Cottenier, Stefaan'
'Claessens, Serge'
'Waroquier, Michel'
'Van Speybroeck, Veronique'
_publ_section_title
;
Assessment of a low-cost protocol for an ab initio based prediction of
the mixing enthalpy at elevated temperatures: The Fe-Mo system
;
_journal_issue 18
_journal_name_full 'Physical Review B'
_journal_page_first 184201
_journal_paper_doi 10.1103/PhysRevB.83.184201
_journal_volume 83
_journal_year 2011
_chemical_formula_sum 'Fe7 Mo6'
_space_group_IT_number 166
_symmetry_Int_Tables_number 166
_symmetry_space_group_name_Hall '-R 3 2"'
_symmetry_space_group_name_H-M 'R -3 m :H'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_formula_units_Z 3
_cell_length_a 4.7402
_cell_length_b 4.7402
_cell_length_c 26.0028
_cell_volume 505.992
_cod_data_source_file mu_COD.cif
_cod_data_source_block mu-phase_Fe7Mo6\par
_cod_depositor_comments
;
This is a density functional theory prediction for the ground state
structure of Fe7Mo6 (mu-phase of the Fe-Mo system).
Stefaan Cottenier
2011-05-06 14:48
;
_cod_database_code 1501463
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 y,x,-z
5 x-y,-y,-z
6 -x,-x+y,-z
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 -y,-x,z
11 -x+y,y,z
12 x,x-y,z
13 x+2/3,y+1/3,z+1/3
14 -y+2/3,x-y+1/3,z+1/3
15 -x+y+2/3,-x+1/3,z+1/3
16 y+2/3,x+1/3,-z+1/3
17 x-y+2/3,-y+1/3,-z+1/3
18 -x+2/3,-x+y+1/3,-z+1/3
19 -x+2/3,-y+1/3,-z+1/3
20 y+2/3,-x+y+1/3,-z+1/3
21 x-y+2/3,x+1/3,-z+1/3
22 -y+2/3,-x+1/3,z+1/3
23 -x+y+2/3,y+1/3,z+1/3
24 x+2/3,x-y+1/3,z+1/3
25 x+1/3,y+2/3,z+2/3
26 -y+1/3,x-y+2/3,z+2/3
27 -x+y+1/3,-x+2/3,z+2/3
28 y+1/3,x+2/3,-z+2/3
29 x-y+1/3,-y+2/3,-z+2/3
30 -x+1/3,-x+y+2/3,-z+2/3
31 -x+1/3,-y+2/3,-z+2/3
32 y+1/3,-x+y+2/3,-z+2/3
33 x-y+1/3,x+2/3,-z+2/3
34 -y+1/3,-x+2/3,z+2/3
35 -x+y+1/3,y+2/3,z+2/3
36 x+1/3,x-y+2/3,z+2/3
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Fe1 Fe 3a 0.0000000 0.0000000 0.0000000 1
Fe2 Fe 18h 0.3322470 0.1661235 0.2567500 1
Mo3 Mo 6c 0.0000000 0.0000000 0.1664500 1
Mo4 Mo 6c 0.0000000 0.0000000 0.3483700 1
Mo5 Mo 6c 0.0000000 0.0000000 0.4512800 1
|
1501464.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501464.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_1501464
loop_
_publ_author_name
'Lejaeghere, Kurt'
'Cottenier, Stefaan'
'Claessens, Serge'
'Waroquier, Michel'
'Van Speybroeck, Veronique'
_publ_section_title
;
Assessment of a low-cost protocol for an ab initio based prediction of
the mixing enthalpy at elevated temperatures: The Fe-Mo system
;
_journal_issue 18
_journal_name_full 'Physical Review B'
_journal_page_first 184201
_journal_paper_doi 10.1103/PhysRevB.83.184201
_journal_volume 83
_journal_year 2011
_chemical_formula_sum 'Fe2 Mo'
_space_group_IT_number 194
_symmetry_Int_Tables_number 194
_symmetry_space_group_name_Hall '-P 6c 2c'
_symmetry_space_group_name_H-M 'P 63/m m c'
_cell_angle_alpha 90.000000
_cell_angle_beta 90.000000
_cell_angle_gamma 120.000000
_cell_formula_units_Z 4
_cell_length_a 4.6594
_cell_length_b 4.6594
_cell_length_c 7.7433
_cell_volume 145.585
_cod_data_source_file femo2.cif
_cod_data_source_block Fe2Mo
_cod_depositor_comments
;
This is a density functional theory prediction for the ground state
structure of FeMo2 (lambda-phase of the Fe-Mo system).
;
_cod_database_code 1501464
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-y,+x-y,+z
-x+y,-x,+z
-x,-y,+z+1/2
+y,-x+y,+z+1/2
+x-y,+x,+z+1/2
+y,+x,-z
+x-y,-y,-z
-x,-x+y,-z
-y,-x,-z+1/2
-x+y,+y,-z+1/2
+x,+x-y,-z+1/2
-x,-y,-z
+y,-x+y,-z
+x-y,+x,-z
+x,+y,-z+1/2
-y,+x-y,-z+1/2
-x+y,-x,-z+1/2
-y,-x,+z
-x+y,+y,+z
+x,+x-y,+z
+y,+x,+z+1/2
+x-y,-y,+z+1/2
-x,-x+y,+z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Mo001 Mo 4f 0.33333 0.66667 0.56934
Fe002 Fe 2a 0.00000 0.00000 0.50000
Fe003 Fe 6h 0.17084 0.34169 0.25000
|
1501465.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501465.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_1501465
loop_
_publ_author_name
'Errico, Leonardo'
'Darriba, German'
'Renteria, Mario'
'Zhengning, Tang'
'Emmerich, Heike'
'Cottenier, Stefaan'
_publ_section_title
;
Nuclear quadrupole moment of the 99Tc ground state
;
_journal_name_full 'Physical Review B'
_journal_page_first 195118
_journal_paper_doi 10.1103/PhysRevB.77.195118
_journal_volume 77
_journal_year 2008
_chemical_formula_sum 'Tc2 Y'
_space_group_IT_number 194
_symmetry_space_group_name_Hall '-P 6c 2c'
_symmetry_space_group_name_H-M 'P 63/m m c'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 4
_cell_length_a 5.373
_cell_length_b 5.373
_cell_length_c 8.847
_cell_volume 221.187
_cod_data_source_file YTc2-COD.cif
_cod_data_source_block YTc2
_cod_depositor_comments
;
This is a density functional theory prediction for the atomic positions
in the YTc2 crystal, using the experimental lattice constants.
The entry has been updated according to the author's e-mail:
From: Stefaan Cottenier <Stefaan.Cottenier@xxxx.be>
To: Saulius Grazulis <grazulis@xxxx.lt>
Date: 2011-06-22 17:26
/.../
The last blocks should read:
/.../
for YTc2:
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Y1 Y 4 f 0.33333333 0.66666667 0.06358 1
Tc1 Tc 2 a 0 0 0 1
Tc2 Tc 6 h 0.82920 0.65840 0.25 1
Saulius Gra\<zulis
2011.06.23
;
_cod_database_code 1501465
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
'x-y, x, z+1/2'
'-x+y, -x, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'-x, -y, z+1/2'
'x, y, -z+1/2'
'-x+y, -x, z'
'x-y, x, -z'
'y, -x+y, z+1/2'
'-y, x-y, -z+1/2'
'x-y, -y, -z'
'-x+y, y, z'
'-x, -x+y, -z'
'x, x-y, z'
'y, x, -z'
'-y, -x, z'
'-y, -x, -z+1/2'
'y, x, z+1/2'
'-x+y, y, -z+1/2'
'x-y, -y, z+1/2'
'x, x-y, -z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Y1 Y 4 f 0.33333333 0.66666667 0.06358 1
Tc1 Tc 2 a 0 0 0 1
Tc2 Tc 6 h 0.82920 0.65840 0.25 1
|
1501466.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501466.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_1501466
loop_
_publ_author_name
'Errico, Leonardo'
'Darriba, German'
'Renteria, Mario'
'Zhengning, Tang'
'Emmerich, Heike'
'Cottenier, Stefaan'
_publ_section_title
;
Nuclear quadrupole moment of the 99Tc ground state
;
_journal_name_full 'Physical Review B'
_journal_page_first 195118
_journal_paper_doi 10.1103/PhysRevB.77.195118
_journal_volume 77
_journal_year 2008
_chemical_formula_sum 'Tc2 Zr'
_space_group_IT_number 194
_symmetry_space_group_name_Hall '-P 6c 2c'
_symmetry_space_group_name_H-M 'P 63/m m c'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 4
_cell_length_a 5.2185
_cell_length_b 5.2185
_cell_length_c 8.6527
_cell_volume 204.067
_cod_data_source_file ZrTc2-COD.cif
_cod_data_source_block ZrTc2
_cod_depositor_comments
;
This is a density functional theory prediction for the atomic positions
in the ZrTc2 crystal, using the experimental lattice constants.
The entry has been updated according to the author's e-mail:
From: Stefaan Cottenier <Stefaan.Cottenier@xxxx.be>
To: Saulius Grazulis <grazulis@xxxx.lt>
Date: 2011-06-22 17:26
/.../
The last blocks should read:
/.../
for ZrTc2:
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Zr1 Zr 4 f 0.33333333 0.66666667 0.06243 1
Tc1 Tc 2 a 0 0 0 1
Tc2 Tc 6 h 0.82895 0.65790 0.25 1
Saulius Gra\<zulis
2011.06.23
;
_cod_database_code 1501466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
'x-y, x, z+1/2'
'-x+y, -x, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'-x, -y, z+1/2'
'x, y, -z+1/2'
'-x+y, -x, z'
'x-y, x, -z'
'y, -x+y, z+1/2'
'-y, x-y, -z+1/2'
'x-y, -y, -z'
'-x+y, y, z'
'-x, -x+y, -z'
'x, x-y, z'
'y, x, -z'
'-y, -x, z'
'-y, -x, -z+1/2'
'y, x, z+1/2'
'-x+y, y, -z+1/2'
'x-y, -y, z+1/2'
'x, x-y, -z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Zr1 Zr 4 f 0.33333333 0.66666667 0.06243 1
Tc1 Tc 2 a 0 0 0 1
Tc2 Tc 6 h 0.82895 0.65790 0.25 1
|
1501467.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501467.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_1501467
loop_
_publ_author_name
'Errico, Leonardo'
'Darriba, German'
'Renteria, Mario'
'Zhengning, Tang'
'Emmerich, Heike'
'Cottenier, Stefaan'
_publ_section_title
;
Nuclear quadrupole moment of the 99Tc ground state
;
_journal_name_full 'Physical Review B'
_journal_page_first 195118
_journal_paper_doi 10.1103/PhysRevB.77.195118
_journal_volume 77
_journal_year 2008
_chemical_formula_sum 'K O4 Tc'
_space_group_IT_number 88
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.630
_cell_length_b 5.630
_cell_length_c 12.867
_cell_volume 407.844
_cod_data_source_file KTcO4-COD.cif
_cod_data_source_block KTcO4
_cod_depositor_comments
;
This is a density functional theory prediction for the atomic positions
in the KTcO4 crystal, using the experimental lattice constants.
;
_cod_database_code 1501467
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'
'-y-1/4, x+1/4, z+1/4'
'-y+1/4, x-1/4, z-1/4'
'y+1/4, -x-1/4, -z-1/4'
'y-1/4, -x+1/4, -z+1/4'
'-x, -y+1/2, z'
'-x+1/2, -y, z+1/2'
'x, y+1/2, -z'
'x+1/2, y, -z+1/2'
'y+1/4, -x+1/4, z+1/4'
'y-1/4, -x-1/4, z-1/4'
'-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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Tc1 Tc 4 a 0 0.25 0.125 1
K1 K 4 b 0 0.25 0.625 1
O1 O 16 f 0.1170 0.0273 0.2015 1
|
1501468.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501468.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_1501468
loop_
_publ_author_name
'Errico, Leonardo'
'Darriba, German'
'Renteria, Mario'
'Zhengning, Tang'
'Emmerich, Heike'
'Cottenier, Stefaan'
_publ_section_title
;
Nuclear quadrupole moment of the 99Tc ground state
;
_journal_name_full 'Physical Review B'
_journal_page_first 195118
_journal_paper_doi 10.1103/PhysRevB.77.195118
_journal_volume 77
_journal_year 2008
_chemical_formula_sum 'O4 Rb Tc'
_space_group_IT_number 88
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.758
_cell_length_b 5.758
_cell_length_c 13.540
_cell_volume 448.913
_cod_data_source_file RbTcO4-COD.cif
_cod_data_source_block RbTcO4
_cod_depositor_comments
;
This is a density functional theory prediction for the atomic positions
in the RbTcO4 crystal, using the experimental lattice constants.
;
_cod_database_code 1501468
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'
'-y-1/4, x+1/4, z+1/4'
'-y+1/4, x-1/4, z-1/4'
'y+1/4, -x-1/4, -z-1/4'
'y-1/4, -x+1/4, -z+1/4'
'-x, -y+1/2, z'
'-x+1/2, -y, z+1/2'
'x, y+1/2, -z'
'x+1/2, y, -z+1/2'
'y+1/4, -x+1/4, z+1/4'
'y-1/4, -x-1/4, z-1/4'
'-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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
Tc1 Tc 4 a 0 0.25 0.125 1
Rb1 Rb 4 b 0 0.25 0.625 1
O1 O 16 f 0.1100 0.0308 0.1980 1
|
1501469.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501469.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_1501469
loop_
_publ_author_name
'Carmen Enrique'
'Miguel Quir\'os'
'Juan M. Salas'
'Antonio Garc\'ia'
'Jos\'e Daniel Mart\'in'
_publ_contact_author_address
;
Departamento de Qu\'imica Inorg\'anica
Facultad de Ciencias
Universidad de Granada
18071 Granada
SPAIN
;
_publ_contact_author_email mquiros@ugr.es
_publ_contact_author_fax 34-58-248526
_publ_contact_author_name 'Miguel Quir\'os'
_publ_contact_author_phone 34-58-240441
_publ_section_title
;
5(2'Carboxy)phenylazo barbiturate diaqua copper(II) trihydrate:
Characterization and crystal structure
;
_journal_name_full
'Journal of Crystallographic and Spectroscopic Research'
_journal_page_first 407
_journal_page_last 410
_journal_paper_doi 10.1007/BF01159143
_journal_volume 23
_journal_year 1993
_chemical_formula_sum 'C11 H16 Cu N4 O10'
_chemical_formula_weight 427.82
_chemical_name_systematic
;
?
;
_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 106.54(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.432(3)
_cell_length_b 6.927(2)
_cell_length_c 21.289(8)
_cell_measurement_temperature 293(2)
_cell_volume 1616.1(9)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0428
_diffrn_reflns_av_sigmaI/netI 0.0257
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 4444
_diffrn_reflns_theta_full 45.13
_diffrn_reflns_theta_max 45.13
_diffrn_reflns_theta_min 4.03
_exptl_absorpt_coefficient_mu 2.525
_exptl_crystal_density_diffrn 1.758
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 876
_refine_diff_density_max 0.399
_refine_diff_density_min -0.621
_refine_diff_density_rms 0.142
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 285
_refine_ls_number_reflns 1318
_refine_ls_number_restraints 21
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0418
_refine_ls_R_factor_gt 0.0416
_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^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1177
_refine_ls_wR_factor_ref 0.1181
_reflns_number_gt 1297
_reflns_number_total 1318
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file cubn2c.cif
_cod_data_source_block cubn2c
_cod_database_code 1501469
_cod_database_fobs_code 1501469
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
Cu Cu 0.04566(5) 0.18305(8) 0.14577(3) 0.0315(5) Uani 1 1 d . . .
N1 N 0.3636(3) 0.3572(5) 0.11464(17) 0.0266(10) Uani 1 1 d D . .
H1 H 0.404(3) 0.355(6) 0.1568(8) 0.034(5) Uiso 1 1 d D . .
C2 C 0.4189(4) 0.4133(6) 0.0692(2) 0.0266(11) Uani 1 1 d . . .
O2 O 0.5279(3) 0.4581(4) 0.08412(13) 0.0348(8) Uani 1 1 d . . .
N3 N 0.3467(3) 0.4148(5) 0.00608(17) 0.0277(10) Uani 1 1 d D . .
H3 H 0.381(3) 0.461(5) -0.0238(15) 0.034(5) Uiso 1 1 d D . .
C4 C 0.2244(4) 0.3688(6) -0.0157(2) 0.0237(11) Uani 1 1 d . . .
O4 O 0.1719(3) 0.3756(4) -0.07400(16) 0.0373(8) Uani 1 1 d . . .
C5 C 0.1696(4) 0.3131(5) 0.0362(2) 0.0221(11) Uani 1 1 d . . .
C6 C 0.2439(4) 0.3054(5) 0.1022(2) 0.0237(12) Uani 1 1 d . . .
O6 O 0.2082(2) 0.2537(5) 0.14980(14) 0.0312(8) Uani 1 1 d . . .
N7 N 0.0512(3) 0.2691(5) 0.01385(16) 0.0260(10) Uani 1 1 d . . .
N8 N -0.0145(3) 0.2135(5) 0.05110(17) 0.0239(10) Uani 1 1 d . . .
C1' C -0.1386(4) 0.1755(5) 0.0136(2) 0.0246(12) Uani 1 1 d . . .
C2' C -0.2270(4) 0.1169(6) 0.04382(19) 0.0233(11) Uani 1 1 d . . .
C3' C -0.3457(4) 0.0843(6) 0.0039(2) 0.0315(12) Uani 1 1 d D . .
H3' H -0.396(3) 0.037(5) 0.0294(16) 0.034(5) Uiso 1 1 d D . .
C4' C -0.3787(4) 0.1029(6) -0.0627(2) 0.0339(12) Uani 1 1 d D . .
H4' H -0.4562(19) 0.066(5) -0.0917(16) 0.034(5) Uiso 1 1 d D . .
C5' C -0.2916(4) 0.1590(6) -0.0929(2) 0.0332(13) Uani 1 1 d D . .
H5' H -0.319(4) 0.176(5) -0.1393(6) 0.034(5) Uiso 1 1 d D . .
C6' C -0.1728(4) 0.1955(5) -0.0545(2) 0.0281(12) Uani 1 1 d D . .
H6' H -0.115(3) 0.250(5) -0.0744(18) 0.034(5) Uiso 1 1 d D . .
C7' C -0.2089(5) 0.0824(6) 0.1152(2) 0.0327(12) Uani 1 1 d . . .
O1' O -0.1027(3) 0.0982(6) 0.15588(14) 0.0517(10) Uani 1 1 d . . .
O2' O -0.2973(3) 0.0377(5) 0.13471(14) 0.0419(9) Uani 1 1 d . . .
OW1 O 0.1211(3) 0.0661(5) 0.23419(14) 0.0425(9) Uani 1 1 d D . .
HW11 H 0.074(4) 0.065(10) 0.258(2) 0.100(8) Uiso 1 1 d D . .
HW12 H 0.192(2) 0.099(9) 0.257(2) 0.100(8) Uiso 1 1 d D . .
OW2 O 0.0159(3) 0.5049(5) 0.17890(14) 0.0422(9) Uani 1 1 d D . .
HW21 H 0.086(2) 0.555(8) 0.190(3) 0.100(8) Uiso 1 1 d D . .
HW22 H -0.025(4) 0.569(8) 0.146(2) 0.100(8) Uiso 1 1 d D . .
OW3 O -0.2433(4) 0.1893(5) 0.26304(18) 0.0607(11) Uani 1 1 d D . .
HW31 H -0.218(6) 0.165(8) 0.230(2) 0.100(8) Uiso 1 1 d D . .
HW32 H -0.300(4) 0.106(7) 0.258(3) 0.100(8) Uiso 1 1 d D . .
OW4 O 0.6635(3) 0.6940(4) 0.18931(15) 0.0454(10) Uani 1 1 d D . .
HW41 H 0.690(6) 0.784(6) 0.170(2) 0.100(8) Uiso 1 1 d D . .
HW42 H 0.626(5) 0.615(7) 0.160(2) 0.100(8) Uiso 1 1 d D . .
OW5 O 0.5029(4) 0.3231(6) 0.24320(18) 0.0637(12) Uani 1 1 d D . .
HW51 H 0.502(6) 0.360(8) 0.2054(14) 0.100(8) Uiso 1 1 d D . .
HW52 H 0.493(7) 0.202(2) 0.241(3) 0.100(8) Uiso 1 1 d 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
Cu 0.0188(7) 0.0555(6) 0.0194(7) 0.0026(3) 0.0043(4) -0.0063(3)
N1 0.018(3) 0.050(2) 0.010(2) 0.0036(17) 0.000(2) -0.0027(18)
C2 0.022(3) 0.035(3) 0.023(3) 0.002(2) 0.006(3) 0.004(2)
O2 0.015(2) 0.060(2) 0.0297(19) 0.0013(14) 0.0066(16) -0.0072(15)
N3 0.020(3) 0.050(2) 0.015(3) 0.0043(18) 0.008(2) -0.0048(19)
C4 0.015(3) 0.036(2) 0.020(3) -0.002(2) 0.003(3) -0.002(2)
O4 0.0254(19) 0.068(2) 0.017(2) 0.0026(16) 0.0036(17) -0.0088(16)
C5 0.006(3) 0.033(2) 0.026(3) -0.0001(18) 0.003(3) -0.0046(18)
C6 0.013(3) 0.032(3) 0.023(4) -0.005(2) 0.001(3) 0.0000(19)
O6 0.024(2) 0.0597(18) 0.0120(18) 0.0070(16) 0.0087(14) -0.0037(16)
N7 0.022(3) 0.032(2) 0.024(2) 0.0024(17) 0.005(2) -0.0002(18)
N8 0.012(2) 0.036(2) 0.023(2) 0.0004(16) 0.004(2) -0.0031(16)
C1' 0.020(3) 0.028(2) 0.026(3) -0.0011(18) 0.005(3) 0.0003(19)
C2' 0.016(3) 0.032(2) 0.019(3) 0.001(2) 0.000(3) 0.001(2)
C3' 0.019(3) 0.046(3) 0.030(4) 0.001(2) 0.009(3) -0.003(2)
C4' 0.015(3) 0.048(3) 0.034(4) -0.002(2) -0.001(3) -0.008(2)
C5' 0.027(3) 0.047(3) 0.021(3) 0.000(2) -0.001(3) 0.000(2)
C6' 0.018(3) 0.040(3) 0.026(4) 0.0023(19) 0.004(3) -0.006(2)
C7' 0.022(3) 0.041(3) 0.035(3) -0.003(2) 0.008(3) -0.009(2)
O1' 0.026(2) 0.106(3) 0.0220(19) 0.0104(17) 0.0038(18) -0.0222(19)
O2' 0.022(2) 0.075(2) 0.0304(19) 0.0054(16) 0.0105(15) -0.0111(16)
OW1 0.025(2) 0.074(2) 0.0266(19) 0.0122(16) 0.0037(15) -0.0061(18)
OW2 0.031(2) 0.063(2) 0.030(2) -0.0039(16) 0.0038(15) 0.0058(16)
OW3 0.057(3) 0.092(3) 0.036(2) -0.0020(18) 0.018(2) 0.0025(19)
OW4 0.042(2) 0.063(2) 0.028(2) -0.0032(15) 0.0032(16) -0.0085(16)
OW5 0.048(2) 0.106(3) 0.031(2) 0.0101(19) 0.0016(18) -0.005(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
O1' Cu O6 170.49(13) . . ?
O1' Cu N8 95.10(15) . . ?
O6 Cu N8 94.10(15) . . ?
O1' Cu OW1 85.80(13) . . ?
O6 Cu OW1 84.71(13) . . ?
N8 Cu OW1 161.17(14) . . ?
O1' Cu OW2 92.81(14) . . ?
O6 Cu OW2 88.05(12) . . ?
N8 Cu OW2 99.58(12) . . ?
OW1 Cu OW2 99.16(12) . . ?
C2 N1 C6 125.6(4) . . ?
O2 C2 N1 122.0(4) . . ?
O2 C2 N3 122.3(4) . . ?
N1 C2 N3 115.6(4) . . ?
C2 N3 C4 127.0(4) . . ?
O4 C4 N3 119.6(4) . . ?
O4 C4 C5 125.9(4) . . ?
N3 C4 C5 114.6(4) . . ?
N7 C5 C6 127.1(4) . . ?
N7 C5 C4 113.5(4) . . ?
C6 C5 C4 119.4(4) . . ?
O6 C6 N1 117.3(4) . . ?
O6 C6 C5 124.9(4) . . ?
N1 C6 C5 117.8(4) . . ?
C6 O6 Cu 125.4(3) . . ?
N8 N7 C5 123.7(3) . . ?
N7 N8 C1' 111.4(3) . . ?
N7 N8 Cu 124.8(3) . . ?
C1' N8 Cu 123.8(3) . . ?
C6' C1' C2' 118.6(4) . . ?
C6' C1' N8 119.8(4) . . ?
C2' C1' N8 121.5(4) . . ?
C3' C2' C1' 117.9(4) . . ?
C3' C2' C7' 115.0(4) . . ?
C1' C2' C7' 127.1(4) . . ?
C4' C3' C2' 123.4(4) . . ?
C3' C4' C5' 119.0(4) . . ?
C4' C5' C6' 119.2(5) . . ?
C5' C6' C1' 121.9(4) . . ?
O2' C7' O1' 120.2(4) . . ?
O2' C7' C2' 119.5(4) . . ?
O1' C7' C2' 120.3(4) . . ?
C7' O1' Cu 131.9(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
Cu O1' 1.865(3) . ?
Cu O6 1.900(3) . ?
Cu N8 1.947(4) . ?
Cu OW1 2.005(3) . ?
Cu OW2 2.392(3) . ?
N1 C2 1.354(6) . ?
N1 C6 1.366(5) . ?
C2 O2 1.235(5) . ?
C2 N3 1.362(6) . ?
N3 C4 1.379(5) . ?
C4 O4 1.215(5) . ?
C4 C5 1.469(6) . ?
C5 N7 1.337(5) . ?
C5 C6 1.420(7) . ?
C6 O6 1.248(5) . ?
N7 N8 1.296(5) . ?
N8 C1' 1.441(6) . ?
C1' C6' 1.397(6) . ?
C1' C2' 1.404(6) . ?
C2' C3' 1.399(6) . ?
C2' C7' 1.494(6) . ?
C3' C4' 1.364(6) . ?
C4' C5' 1.386(6) . ?
C5' C6' 1.395(7) . ?
C7' O2' 1.236(5) . ?
C7' O1' 1.279(5) . ?
|
1501470.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501470.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_1501470
loop_
_publ_author_name
'Kr\"uger, Hannes'
'Kahlenberg, Volker'
'Kaindl, R.'
_publ_section_title
;
Li2Si3O7: Crystal structure and Raman Spectroscopy
;
_journal_name_full 'Journal of Solid State Chemistry'
_journal_page_first 936
_journal_page_last 942
_journal_volume 180
_journal_year 2007
_chemical_formula_sum 'Li2 O7 Si3'
_chemical_formula_weight 210.13
_chemical_name_systematic ' ?'
_space_group_IT_number 57
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 57
_symmetry_space_group_name_Hall '-P 2ac 2a'
_symmetry_space_group_name_H-M 'P m c a'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.648(3)
_cell_length_b 5.9969(8)
_cell_length_c 4.8691(6)
_cell_measurement_reflns_used 3544
_cell_measurement_temperature 298
_cell_measurement_theta_max 29.48
_cell_measurement_theta_min 2.07
_cell_volume 573.71(14)
_computing_cell_refinement 'STOE X-AREA'
_computing_data_collection 'STOE X-AREA'
_computing_data_reduction 'STOE X-RED'
_computing_molecular_graphics 'DRAWxtl5.1 (Finger, Kroeker and Toby, 2005)'
_computing_publication_material '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_solution SIR-97
_diffrn_ambient_temperature 298
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type STOE
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_details ' 120 frames, detector distance = 100 mm'
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS 2'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_polarisn_norm 0
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0451
_diffrn_reflns_av_sigmaI/netI 0.0123
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 4610
_diffrn_reflns_theta_full 29.23
_diffrn_reflns_theta_max 29.23
_diffrn_reflns_theta_min 2.07
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current 40
_diffrn_source_power 2.00
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.81
_exptl_absorpt_correction_T_max 0.9833
_exptl_absorpt_correction_T_min 0.8754
_exptl_absorpt_correction_type integration
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.435
_exptl_crystal_description plate
_exptl_crystal_F_000 416
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.53
_refine_diff_density_min -0.50
_refine_ls_extinction_coef 0.04(2)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt 2.46
_refine_ls_goodness_of_fit_ref 2.34
_refine_ls_number_parameters 59
_refine_ls_number_reflns 803
_refine_ls_R_factor_all 0.0505
_refine_ls_R_factor_gt 0.0350
_refine_ls_shift/su_max 0.0002
_refine_ls_shift/su_mean 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_gt 0.0374
_refine_ls_wR_factor_ref 0.0399
_reflns_number_gt 649
_reflns_number_total 803
_reflns_threshold_expression I>3\s(I)
_cod_data_source_file Li2Si3O7.cif
_cod_data_source_block li2si3o7
_cod_original_cell_volume 573.70(14)
_cod_database_code 1501470
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,y,z
3 x,-y,1/2+z
4 1/2-x,-y,1/2+z
5 -x,-y,-z
6 1/2+x,-y,-z
7 -x,y,1/2-z
8 1/2+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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.25 0.34929(15) 0.57981(18) Uani 0.0123(2) 4 1 d . . .
Si2 Si 0.10440(3) 0.14615(10) 0.55364(12) Uani 0.01098(16) 8 1 d . . .
O1 O 0.05547(8) 0.3389(3) 0.4566(3) Uani 0.0156(4) 8 1 d . . .
O2 O 0.18419(9) 0.2016(3) 0.5144(4) Uani 0.0194(5) 8 1 d . . .
O3 O 0.25 0.4260(4) 0.8970(5) Uani 0.0206(7) 4 1 d . . .
O4 O 0.09068(8) 0.0865(3) 0.8801(3) Uani 0.0141(4) 8 1 d . . .
Li1 Li 0.0440(2) 0.3535(7) 0.0567(9) Uani 0.0190(11) 8 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Si1 Si 0.0135(4) 0.0119(4) 0.0115(4) 0 0 -0.0001(3)
Si2 Si 0.0124(3) 0.0101(3) 0.0104(3) -0.0006(2) -0.0002(2) 0.0000(2)
O1 O 0.0190(7) 0.0128(7) 0.0151(7) 0.0020(6) -0.0014(6) 0.0013(7)
O2 O 0.0155(7) 0.0226(9) 0.0201(9) -0.0053(7) 0.0006(6) -0.0024(7)
O3 O 0.0334(13) 0.0161(12) 0.0123(11) 0 0 -0.0001(10)
O4 O 0.0195(7) 0.0119(7) 0.0108(7) 0.0024(6) 0.0011(5) -0.0001(6)
Li1 Li 0.0246(19) 0.0156(18) 0.0169(18) 0.0018(15) -0.0007(15) 0.0011(17)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
Si 0.082 0.070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0150
1 0 0 0.0050
5 6 0 0.0330
3 0 -5 0.1120
2 5 3 0.1020
-3 -4 0 0.0540
-3 0 5 0.1440
-5 -4 3 0.1230
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Si1 O2 . . 2_555 107.88(10) yes
O2 Si1 O3 . . . 110.43(9) yes
O2 Si1 O3 . . 3_564 110.63(9) yes
O2 Si1 O2 2_555 . . 107.88(10) yes
O2 Si1 O3 2_555 . . 110.43(9) yes
O2 Si1 O3 2_555 . 3_564 110.63(9) yes
O3 Si1 O3 . . 3_564 106.86(14) yes
O3 Si1 O3 3_564 . . 106.86(14) yes
O1 Si2 O2 . . . 113.96(10) yes
O1 Si2 O4 . . . 110.36(9) yes
O1 Si2 O4 . . 3_554 111.47(9) yes
O2 Si2 O4 . . . 108.50(9) yes
O2 Si2 O4 . . 3_554 105.77(9) yes
O4 Si2 O4 . . 3_554 106.41(9) yes
O4 Si2 O4 3_554 . . 106.41(9) yes
O1 Li1 O1 1_554 . . 168.2(2) yes
O1 Li1 O1 1_554 . 3_564 76.52(15) yes
O1 Li1 O1 1_554 . 7_555 92.43(16) yes
O1 Li1 O4 1_554 . 1_554 61.38(12) yes
O1 Li1 O1 . . 1_554 168.2(2) yes
O1 Li1 O1 . . 3_564 106.3(2) yes
O1 Li1 O1 . . 7_555 98.4(2) yes
O1 Li1 O4 . . 1_554 109.4(2) yes
O1 Li1 O1 3_564 . 1_554 76.52(15) yes
O1 Li1 O1 3_564 . . 106.3(2) yes
O1 Li1 O1 3_564 . 7_555 98.7(2) yes
O1 Li1 O4 3_564 . 1_554 126.5(2) yes
O1 Li1 O1 7_555 . 1_554 92.43(16) yes
O1 Li1 O1 7_555 . . 98.4(2) yes
O1 Li1 O1 7_555 . 3_564 98.7(2) yes
O1 Li1 O4 7_555 . 1_554 113.6(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O2 . . 1.5993(19) yes
Si1 O2 . 2_555 1.5993(19) yes
Si1 O3 . . 1.612(3) yes
Si1 O3 . 3_564 1.615(3) yes
Si2 O1 . . 1.5759(18) yes
Si2 O2 . . 1.6139(19) yes
Si2 O4 . . 1.6515(17) yes
Si2 O4 . 3_554 1.6531(18) yes
Li1 O1 . 1_554 2.932(5) yes
Li1 O1 . . 1.962(5) yes
Li1 O1 . 3_564 1.921(5) yes
Li1 O1 . 7_555 1.957(4) yes
Li1 O4 . 1_554 2.036(5) yes
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_intensity_meas
_refln_intensity_calc
_refln_intensity_sigma
_refln_observed_status
4 0 0 3291.0 3515.1 120.6 o
6 0 0 84512.8 84806.3 1696.9 o
8 0 0 5.8 0.9 57.9 <
10 0 0 1425.4 1388.4 59.0 o
12 0 0 9082.5 8264.2 189.6 o
14 0 0 47870.1 47125.0 960.7 o
16 0 0 1569.6 1577.8 51.2 o
18 0 0 94.8 72.1 36.6 <
20 0 0 18182.4 16969.4 367.5 o
22 0 0 47.7 33.8 34.6 <
24 0 0 1255.8 1202.1 43.7 o
26 0 0 2831.4 2807.7 68.6 o
0 1 0 3171.1 3422.1 128.4 o
2 1 0 7042.6 7363.5 160.3 o
4 1 0 64337.8 62161.1 1292.8 o
6 1 0 112.9 86.0 47.7 <
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3 5 3 1579.4 1610.7 45.5 o
4 5 3 819.5 763.4 37.7 o
5 5 3 67.2 14.8 24.4 <
6 5 3 2652.5 2614.8 58.6 o
7 5 3 719.7 734.5 25.0 o
8 5 3 5618.5 5515.4 114.8 o
9 5 3 134.9 97.2 20.2 o
10 5 3 1855.5 1802.1 42.3 o
11 5 3 435.1 410.1 21.2 o
12 5 3 849.8 816.3 28.9 o
13 5 3 39.7 48.1 21.7 <
14 5 3 4128.9 4184.7 85.7 o
15 5 3 407.0 447.1 23.0 o
16 5 3 107.3 6.4 21.3 o
17 5 3 558.9 631.3 23.8 o
0 6 3 825.9 852.0 47.4 o
1 6 3 60.5 0.3 30.0 <
2 6 3 1100.2 1076.8 36.2 o
3 6 3 650.0 703.9 28.3 o
4 6 3 1897.8 1938.8 45.3 o
5 6 3 16.0 11.9 22.5 <
6 6 3 357.4 333.1 23.9 o
7 6 3 1371.6 1343.7 34.9 o
8 6 3 35.4 13.5 19.6 <
9 6 3 47.1 19.0 22.7 <
10 6 3 1353.1 1373.6 34.7 o
11 6 3 356.2 285.7 22.9 o
12 6 3 218.1 265.0 25.2 o
13 6 3 82.7 84.6 23.3 o
0 7 3 15.2 6.3 27.6 <
1 7 3 11.2 50.3 24.1 <
2 7 3 267.3 351.2 25.1 o
3 7 3 2.5 0.4 20.1 <
4 7 3 92.8 30.5 25.7 o
5 7 3 24.2 7.8 25.5 <
6 7 3 -1.4 4.9 28.4 <
7 7 3 85.4 131.9 31.2 <
0 0 4 168.8 4.9 49.3 o
1 0 4 7745.4 8030.4 160.3 o
2 0 4 475.6 330.5 32.8 o
3 0 4 723.0 713.3 34.8 o
4 0 4 689.9 723.7 34.2 o
5 0 4 51.7 6.6 31.8 <
6 0 4 4247.5 4451.8 92.0 o
7 0 4 11031.6 11393.0 225.7 o
8 0 4 2809.7 3107.7 65.2 o
9 0 4 63.9 4.2 30.5 <
10 0 4 405.8 415.8 31.8 o
11 0 4 2591.9 2489.5 60.7 o
12 0 4 2380.8 2480.7 57.1 o
13 0 4 9583.4 9709.2 195.4 o
14 0 4 -8.7 48.3 28.2 <
15 0 4 2469.8 2471.6 58.2 o
16 0 4 324.9 262.7 28.8 o
17 0 4 872.7 933.8 33.8 o
18 0 4 1698.0 1676.0 45.2 o
19 0 4 1103.1 1114.8 36.5 o
20 0 4 121.9 129.6 28.6 o
21 0 4 1784.8 1996.8 47.2 o
0 1 4 22.3 24.4 33.6 <
1 1 4 527.2 497.7 25.5 o
2 1 4 2227.5 2355.5 50.7 o
3 1 4 4398.5 4602.7 92.0 o
4 1 4 895.2 918.0 31.2 o
5 1 4 391.1 332.8 25.9 o
6 1 4 53.9 45.8 30.6 <
7 1 4 770.9 742.3 30.6 o
8 1 4 961.0 961.5 30.4 o
9 1 4 1248.6 1350.8 34.8 o
10 1 4 372.4 311.1 23.3 o
11 1 4 1770.7 1782.4 43.9 o
12 1 4 31.2 14.0 23.0 <
13 1 4 91.1 99.6 22.2 o
14 1 4 794.5 735.3 27.1 o
15 1 4 108.7 118.3 21.0 o
16 1 4 812.8 768.9 26.9 o
17 1 4 1711.8 1725.1 40.4 o
18 1 4 43.6 7.2 20.3 <
19 1 4 219.2 216.1 21.3 o
20 1 4 57.8 36.6 19.8 <
21 1 4 446.6 532.0 22.9 o
0 2 4 2715.9 2830.7 65.5 o
1 2 4 1392.4 1339.6 39.1 o
2 2 4 95.1 19.9 25.2 o
3 2 4 78.2 30.4 23.3 o
4 2 4 247.2 151.1 23.8 o
5 2 4 0.0 4.9 22.9 <
6 2 4 78.0 26.7 25.7 o
7 2 4 1264.4 1250.0 36.4 o
8 2 4 533.0 517.6 27.7 o
9 2 4 57.1 3.3 23.9 <
10 2 4 290.9 300.6 21.6 o
11 2 4 100.5 72.0 21.6 o
12 2 4 200.4 141.9 21.6 o
13 2 4 1479.5 1476.6 36.5 o
14 2 4 383.7 337.1 22.0 o
15 2 4 239.5 268.7 21.0 o
16 2 4 34.2 25.5 20.1 <
17 2 4 -36.9 0.2 20.2 <
18 2 4 52.1 20.1 20.3 <
19 2 4 248.1 213.3 22.1 o
20 2 4 56.2 4.0 20.6 <
0 3 4 1076.1 1061.5 48.4 o
1 3 4 546.4 463.5 27.3 o
2 3 4 1205.4 1163.4 37.3 o
3 3 4 12515.1 12658.8 252.8 o
4 3 4 152.1 13.1 32.5 o
5 3 4 1081.2 1156.1 33.1 o
6 3 4 20.1 12.7 21.5 <
7 3 4 577.1 509.6 24.8 o
8 3 4 280.0 238.4 22.4 o
9 3 4 4280.3 4381.8 89.4 o
10 3 4 379.9 400.5 25.1 o
11 3 4 4352.2 4303.7 90.8 o
12 3 4 389.6 370.7 23.9 o
13 3 4 76.1 34.9 21.1 o
14 3 4 1041.1 1060.6 31.5 o
15 3 4 86.5 89.4 22.4 o
16 3 4 152.3 130.8 22.5 o
17 3 4 4113.3 4132.2 86.2 o
18 3 4 210.7 173.2 21.1 o
19 3 4 452.5 540.2 23.0 o
0 4 4 321.6 202.0 50.4 o
1 4 4 3154.0 3173.4 73.5 o
2 4 4 593.8 548.7 29.7 o
3 4 4 678.7 670.4 27.1 o
4 4 4 208.4 193.1 24.9 o
5 4 4 187.9 121.7 24.7 o
6 4 4 84.8 71.8 22.0 o
7 4 4 6078.3 6172.5 124.7 o
8 4 4 29.9 32.7 22.2 <
9 4 4 69.0 65.7 20.1 o
10 4 4 49.0 19.3 20.7 <
11 4 4 831.8 815.7 27.9 o
12 4 4 746.6 738.9 26.9 o
13 4 4 3415.0 3534.2 71.7 o
14 4 4 -19.2 60.9 22.1 <
15 4 4 894.7 962.6 28.4 o
16 4 4 28.0 28.1 23.4 <
17 4 4 587.7 650.3 27.3 o
1 5 4 42.0 0.3 33.5 <
2 5 4 45.4 0.3 24.9 <
3 5 4 25.4 18.2 23.9 <
4 5 4 396.0 350.0 24.7 o
5 5 4 70.2 4.7 24.1 <
6 5 4 21.0 0.7 23.9 <
7 5 4 394.0 365.3 23.6 o
8 5 4 499.2 405.4 22.7 o
9 5 4 113.2 51.4 22.1 o
10 5 4 720.0 730.2 27.5 o
11 5 4 66.5 16.4 23.1 <
12 5 4 160.8 199.4 23.4 o
13 5 4 13.9 58.2 25.1 <
14 5 4 6.5 59.4 58.9 <
0 6 4 1490.6 1338.2 60.2 o
1 6 4 1916.2 2057.8 52.4 o
2 6 4 257.9 278.5 31.1 o
3 6 4 37.0 8.6 28.5 <
4 6 4 335.5 362.3 27.5 o
5 6 4 73.1 50.5 26.2 <
6 6 4 430.6 497.3 29.7 o
7 6 4 3590.4 3742.7 76.7 o
8 6 4 115.9 113.7 26.5 o
9 6 4 34.5 42.1 39.2 <
0 1 5 2393.6 2281.8 58.7 o
1 1 5 68.3 11.3 21.5 o
2 1 5 1114.0 1143.3 31.6 o
3 1 5 462.6 448.3 24.1 o
4 1 5 1307.2 1272.7 37.8 o
5 1 5 344.0 283.2 25.0 o
6 1 5 936.2 942.4 33.2 o
7 1 5 1385.8 1306.7 35.6 o
8 1 5 3283.8 3172.3 70.2 o
9 1 5 1248.9 1193.0 35.0 o
10 1 5 2899.9 2920.5 62.9 o
11 1 5 157.8 143.4 22.3 o
12 1 5 542.4 494.4 24.1 o
13 1 5 88.6 30.3 21.9 o
14 1 5 3452.2 3381.1 73.3 o
15 1 5 10.9 16.4 21.3 <
16 1 5 55.3 33.1 23.2 <
17 1 5 51.8 13.3 22.5 <
0 2 5 5071.8 5072.9 109.8 o
1 2 5 1005.8 847.7 32.5 o
2 2 5 2524.9 2440.9 56.8 o
3 2 5 309.6 206.2 24.0 o
4 2 5 3807.7 3637.5 80.3 o
5 2 5 179.3 128.5 25.1 o
6 2 5 525.7 478.5 28.1 o
7 2 5 285.1 279.1 22.2 o
8 2 5 134.5 97.6 22.1 o
9 2 5 69.2 28.1 20.2 o
10 2 5 1872.5 1866.9 45.6 o
11 2 5 334.3 257.9 23.6 o
12 2 5 1446.5 1418.2 36.0 o
13 2 5 822.8 848.5 26.8 o
14 2 5 1542.6 1537.2 38.2 o
15 2 5 40.8 27.0 21.5 <
16 2 5 262.1 200.2 23.2 o
0 3 5 -28.9 37.9 35.3 <
1 3 5 37.1 8.5 24.7 <
2 3 5 56.5 29.6 24.1 <
3 3 5 313.4 293.0 24.5 o
4 3 5 140.4 79.0 28.2 o
5 3 5 342.0 228.0 27.7 o
6 3 5 134.3 99.2 24.4 o
7 3 5 497.1 442.7 22.8 o
8 3 5 688.0 635.0 25.7 o
9 3 5 44.3 15.4 21.1 <
10 3 5 90.2 78.1 21.4 o
11 3 5 -1.3 23.9 23.3 <
12 3 5 -17.2 21.2 22.6 <
13 3 5 26.1 35.3 21.4 <
14 3 5 291.9 290.5 22.5 o
0 4 5 3142.8 2912.5 73.9 o
1 4 5 585.8 599.4 31.6 o
2 4 5 1088.1 1060.5 42.6 o
3 4 5 2157.6 2144.3 57.4 o
4 4 5 1487.1 1448.5 41.0 o
5 4 5 181.1 90.2 24.0 o
6 4 5 506.5 430.1 24.6 o
7 4 5 55.0 1.0 22.0 <
8 4 5 326.1 337.6 20.9 o
9 4 5 511.2 467.0 23.2 o
10 4 5 836.6 876.6 27.2 o
11 4 5 306.0 301.3 22.5 o
12 4 5 124.8 87.1 22.7 o
0 5 5 2894.9 2481.1 67.7 o
1 5 5 1105.7 1035.4 34.6 o
2 5 5 354.2 300.6 28.0 o
3 5 5 368.4 322.7 30.5 o
4 5 5 1193.1 1288.6 36.4 o
5 5 5 405.6 429.2 27.8 o
6 5 5 1817.1 1944.4 44.7 o
7 5 5 1428.2 1268.4 60.7 o
0 0 6 3539.1 3149.8 84.9 o
1 0 6 3231.4 3156.6 72.8 o
2 0 6 287.6 190.6 31.8 o
3 0 6 1882.1 1884.7 50.1 o
4 0 6 145.0 167.9 32.4 o
5 0 6 139.4 44.9 33.4 o
6 0 6 4155.2 4204.9 93.2 o
7 0 6 4853.3 4944.0 104.8 o
8 0 6 2564.8 2710.0 63.5 o
9 0 6 700.9 779.7 38.1 o
10 0 6 246.4 238.1 37.2 o
11 0 6 1255.2 1436.3 51.5 o
0 1 6 164.5 112.0 29.7 o
1 1 6 669.0 624.3 27.5 o
2 1 6 808.9 777.7 28.9 o
3 1 6 3374.2 3353.7 73.3 o
4 1 6 1458.2 1423.3 38.2 o
5 1 6 61.6 5.8 23.8 <
6 1 6 71.4 33.1 23.6 o
7 1 6 785.2 805.3 28.1 o
8 1 6 109.5 66.7 25.0 o
9 1 6 1189.1 1202.6 33.5 o
10 1 6 1125.2 1161.6 33.8 o
11 1 6 445.3 491.6 25.3 o
0 2 6 18.4 0.0 35.1 <
1 2 6 29.9 12.8 27.4 <
2 2 6 59.2 25.1 26.2 <
3 2 6 65.9 2.4 23.6 <
4 2 6 17.4 2.2 24.6 <
5 2 6 238.9 234.8 23.0 o
6 2 6 258.0 230.1 23.9 o
7 2 6 104.5 2.1 23.2 o
8 2 6 192.4 227.8 24.7 o
9 2 6 12.1 9.3 22.6 <
10 2 6 28.1 35.1 63.6 <
0 3 6 192.8 198.5 51.8 o
1 3 6 1134.7 1152.2 39.9 o
2 3 6 965.8 895.9 36.2 o
3 3 6 2267.8 2496.4 58.7 o
4 3 6 1487.5 1575.8 43.0 o
5 3 6 -3.9 0.7 24.1 <
6 3 6 9.8 2.2 32.1 <
|
1501471.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501471.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_1501471
loop_
_publ_author_name
'Katarzyna Grubel'
'Brynna J. Laughlin'
'Thora R. Maltais'
'Rhett C. Smith'
'Atta M. Arif'
'Lisa M. Berreau'
_publ_section_title
;
Photochemically-induced dioxygenase-type CO-release reactivity of Group
12 metal flavonolate complexes
;
_journal_issue 37
_journal_name_full 'Chemical Communications'
_journal_page_first 10431
_journal_page_last 10433
_journal_paper_doi 10.1039/c1cc13961d
_journal_volume 47
_journal_year 2011
_chemical_formula_moiety 'C45 H35 Cd N4 O3, Cl O4'
_chemical_formula_sum 'C45 H35 Cd Cl N4 O7'
_chemical_formula_weight 891.62
_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 95.0205(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.4616(2)
_cell_length_b 16.3861(3)
_cell_length_c 20.8770(4)
_cell_measurement_reflns_used 8311
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 1.018
_cell_volume 3905.89(12)
_computing_cell_refinement DENZO-SMN
_computing_data_collection 'Nonius COLLECT'
_computing_data_reduction ENZO-SMN
_computing_molecular_graphics 'WinGX, Ortep3'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution SIR97
_diffrn_ambient_temperature 150(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method 'Phi and Omega 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 0.0303
_diffrn_reflns_av_sigmaI/netI 0.0543
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 15965
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 1.96
_exptl_absorpt_coefficient_mu 0.686
_exptl_absorpt_correction_T_max 0.9161
_exptl_absorpt_correction_T_min 0.8310
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.516
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1816
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.840
_refine_diff_density_min -0.573
_refine_diff_density_rms 0.074
_refine_ls_extinction_coef 0.00153(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 1.019
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 552
_refine_ls_number_reflns 8943
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.0631
_refine_ls_R_factor_gt 0.0364
_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^)+(0.0375P)^2^+1.0726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0765
_refine_ls_wR_factor_ref 0.0859
_reflns_number_gt 6629
_reflns_number_total 8943
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1cc13961d.txt
_cod_data_source_block usu204
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1501471
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
Cl1 Cl 1.12025(7) 0.36783(5) 0.72052(4) 0.0512(2) Uani 1 1 d . . .
Cd1 Cd 0.738195(15) 0.142631(10) 0.605534(8) 0.02421(7) Uani 1 1 d . . .
O1 O 0.62056(14) 0.21043(10) 0.53454(8) 0.0256(4) Uani 1 1 d . . .
O2 O 0.85203(14) 0.24183(10) 0.56650(8) 0.0295(4) Uani 1 1 d . . .
O3 O 0.68054(15) 0.36691(10) 0.41862(8) 0.0312(4) Uani 1 1 d . . .
N1 N 0.91533(18) 0.10483(14) 0.66159(10) 0.0320(5) Uani 1 1 d . . .
N2 N 0.70580(18) 0.02244(13) 0.66982(10) 0.0290(5) Uani 1 1 d . . .
N3 N 0.61547(18) 0.18499(13) 0.69083(10) 0.0272(5) Uani 1 1 d . . .
N4 N 0.70721(17) 0.02093(12) 0.54057(10) 0.0262(5) Uani 1 1 d . . .
C1 C 1.0114(2) 0.15210(18) 0.66458(15) 0.0404(7) Uani 1 1 d . . .
H1 H 1.0054 0.2054 0.6467 0.048 Uiso 1 1 calc R . .
C2 C 1.1183(3) 0.1261(2) 0.69254(17) 0.0528(9) Uani 1 1 d . . .
H2 H 1.1853 0.1602 0.6928 0.063 Uiso 1 1 calc R . .
C3 C 1.1262(3) 0.0500(2) 0.72004(18) 0.0590(9) Uani 1 1 d . . .
H3 H 1.1987 0.0309 0.7401 0.071 Uiso 1 1 calc R . .
C4 C 1.0272(3) 0.0015(2) 0.71819(15) 0.0482(8) Uani 1 1 d . . .
H4 H 1.0306 -0.0509 0.7377 0.058 Uiso 1 1 calc R . .
C5 C 0.9229(2) 0.03012(17) 0.68762(13) 0.0355(6) Uani 1 1 d . . .
C6 C 0.8166(2) -0.02411(17) 0.67823(14) 0.0377(7) Uani 1 1 d . . .
H6A H 0.8232 -0.0588 0.6399 0.045 Uiso 1 1 calc R . .
H6B H 0.8147 -0.0605 0.7160 0.045 Uiso 1 1 calc R . .
C7 C 0.6710(2) 0.05009(17) 0.73241(13) 0.0347(6) Uani 1 1 d . . .
H7A H 0.7415 0.0676 0.7597 0.042 Uiso 1 1 calc R . .
H7B H 0.6351 0.0040 0.7542 0.042 Uiso 1 1 calc R . .
C8 C 0.5851(2) 0.11988(16) 0.72536(12) 0.0299(6) Uani 1 1 d . . .
C9 C 0.4830(2) 0.11719(18) 0.75601(13) 0.0377(7) Uani 1 1 d . . .
H9 H 0.4636 0.0702 0.7795 0.045 Uiso 1 1 calc R . .
C10 C 0.4097(2) 0.18428(18) 0.75175(13) 0.0374(7) Uani 1 1 d . . .
H10 H 0.3385 0.1837 0.7718 0.045 Uiso 1 1 calc R . .
C11 C 0.4409(2) 0.25170(17) 0.71825(13) 0.0351(6) Uani 1 1 d . . .
H11 H 0.3916 0.2984 0.7155 0.042 Uiso 1 1 calc R . .
C12 C 0.5452(2) 0.25182(16) 0.68810(12) 0.0286(6) Uani 1 1 d . . .
C13 C 0.5838(2) 0.32660(16) 0.65589(13) 0.0329(6) Uani 1 1 d . . .
C14 C 0.5014(3) 0.38070(18) 0.62655(15) 0.0447(7) Uani 1 1 d . . .
H14 H 0.4203 0.3681 0.6252 0.054 Uiso 1 1 calc R . .
C15 C 0.5372(3) 0.4527(2) 0.59940(17) 0.0587(9) Uani 1 1 d . . .
H15 H 0.4804 0.4893 0.5799 0.070 Uiso 1 1 calc R . .
C16 C 0.6546(4) 0.4714(2) 0.60056(17) 0.0595(10) Uani 1 1 d . . .
H16 H 0.6788 0.5206 0.5816 0.071 Uiso 1 1 calc R . .
C17 C 0.7366(3) 0.41857(19) 0.62930(15) 0.0478(8) Uani 1 1 d . . .
H17 H 0.8175 0.4314 0.6301 0.057 Uiso 1 1 calc R . .
C18 C 0.7017(3) 0.34642(17) 0.65729(13) 0.0355(6) Uani 1 1 d . . .
H18 H 0.7588 0.3106 0.6774 0.043 Uiso 1 1 calc R . .
C19 C 0.6137(2) -0.02555(16) 0.63460(13) 0.0331(6) Uani 1 1 d . . .
H19A H 0.5370 0.0008 0.6387 0.040 Uiso 1 1 calc R . .
H19B H 0.6115 -0.0807 0.6539 0.040 Uiso 1 1 calc R . .
C20 C 0.6334(2) -0.03330(15) 0.56419(13) 0.0297(6) Uani 1 1 d . . .
C21 C 0.5767(2) -0.09268(16) 0.52635(14) 0.0353(6) Uani 1 1 d . . .
H21 H 0.5242 -0.1296 0.5441 0.042 Uiso 1 1 calc R . .
C22 C 0.5974(2) -0.09763(17) 0.46245(15) 0.0396(7) Uani 1 1 d . . .
H22 H 0.5589 -0.1379 0.4355 0.048 Uiso 1 1 calc R . .
C23 C 0.6743(2) -0.04376(17) 0.43805(14) 0.0352(6) Uani 1 1 d . . .
H23 H 0.6904 -0.0471 0.3943 0.042 Uiso 1 1 calc R . .
C24 C 0.7279(2) 0.01539(15) 0.47801(12) 0.0283(6) Uani 1 1 d . . .
C25 C 0.8145(2) 0.07303(16) 0.45461(13) 0.0323(6) Uani 1 1 d . . .
C26 C 0.9214(2) 0.08614(17) 0.48988(15) 0.0381(7) Uani 1 1 d . . .
H26 H 0.9381 0.0599 0.5302 0.046 Uiso 1 1 calc R . .
C27 C 1.0039(3) 0.1376(2) 0.46617(18) 0.0552(9) Uani 1 1 d . . .
H27 H 1.0774 0.1461 0.4900 0.066 Uiso 1 1 calc R . .
C28 C 0.9785(4) 0.1763(2) 0.4078(2) 0.0649(12) Uani 1 1 d . . .
H28 H 1.0349 0.2112 0.3913 0.078 Uiso 1 1 calc R . .
C29 C 0.8716(4) 0.1646(2) 0.37367(17) 0.0649(11) Uani 1 1 d . . .
H29 H 0.8540 0.1925 0.3341 0.078 Uiso 1 1 calc R . .
C30 C 0.7900(3) 0.11278(19) 0.39613(14) 0.0460(8) Uani 1 1 d . . .
H30 H 0.7171 0.1042 0.3718 0.055 Uiso 1 1 calc R . .
C31 C 0.6748(2) 0.26641(14) 0.50308(11) 0.0230(5) Uani 1 1 d . . .
C32 C 0.7987(2) 0.28128(15) 0.52143(12) 0.0249(5) Uani 1 1 d . . .
C33 C 0.8579(2) 0.34145(15) 0.48495(12) 0.0268(6) Uani 1 1 d . . .
C34 C 0.9782(2) 0.35928(15) 0.49855(14) 0.0326(6) Uani 1 1 d . . .
H34 H 1.0229 0.3321 0.5326 0.039 Uiso 1 1 calc R . .
C35 C 1.0301(2) 0.41662(18) 0.46176(14) 0.0401(7) Uani 1 1 d . . .
H35 H 1.1113 0.4280 0.4699 0.048 Uiso 1 1 calc R . .
C36 C 0.9643(3) 0.45781(18) 0.41299(14) 0.0422(7) Uani 1 1 d . . .
H36 H 1.0011 0.4980 0.3888 0.051 Uiso 1 1 calc R . .
C37 C 0.8478(3) 0.44195(17) 0.39887(14) 0.0387(7) Uani 1 1 d . . .
H37 H 0.8033 0.4707 0.3656 0.046 Uiso 1 1 calc R . .
C38 C 0.7959(2) 0.38197(16) 0.43506(12) 0.0288(6) Uani 1 1 d . . .
C39 C 0.6215(2) 0.30990(15) 0.45219(12) 0.0261(5) Uani 1 1 d . . .
C40 C 0.5006(2) 0.30148(15) 0.42368(13) 0.0296(6) Uani 1 1 d . . .
C41 C 0.4070(2) 0.29474(17) 0.46163(15) 0.0370(7) Uani 1 1 d . . .
H41 H 0.4212 0.2952 0.5071 0.044 Uiso 1 1 calc R . .
C42 C 0.2939(3) 0.2874(2) 0.43372(17) 0.0485(8) Uani 1 1 d . . .
H42 H 0.2307 0.2834 0.4601 0.058 Uiso 1 1 calc R . .
C43 C 0.2718(3) 0.2858(2) 0.36713(18) 0.0563(9) Uani 1 1 d . . .
H43 H 0.1938 0.2806 0.3480 0.068 Uiso 1 1 calc R . .
C44 C 0.3640(3) 0.2916(2) 0.32913(17) 0.0528(9) Uani 1 1 d . . .
H44 H 0.3499 0.2896 0.2836 0.063 Uiso 1 1 calc R . .
C45 C 0.4771(2) 0.30053(18) 0.35737(14) 0.0398(7) Uani 1 1 d . . .
H45 H 0.5398 0.3061 0.3308 0.048 Uiso 1 1 calc R . .
O4 O 1.0290(11) 0.3577(6) 0.6757(6) 0.129(6) Uani 0.555(11) 1 d PD A 1
O5 O 1.0985(8) 0.4339(5) 0.7648(5) 0.102(4) Uani 0.555(11) 1 d PD A 1
O6 O 1.2276(5) 0.3989(4) 0.6959(4) 0.079(3) Uani 0.555(11) 1 d PD A 1
O4' O 0.9974(9) 0.3639(9) 0.7094(7) 0.113(5) Uani 0.445(11) 1 d PD A 2
O5' O 1.1490(15) 0.4409(6) 0.7423(8) 0.165(9) Uani 0.445(11) 1 d PD A 2
O6' O 1.1611(9) 0.3454(7) 0.6587(5) 0.108(5) Uani 0.445(11) 1 d PD A 2
O8 O 1.1544(2) 0.29961(14) 0.75972(13) 0.0651(7) Uani 1 1 d . A .
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
Cl1 0.0484(4) 0.0356(4) 0.0680(5) 0.0113(4) -0.0038(4) 0.0030(3)
Cd1 0.02705(10) 0.02005(10) 0.02547(11) 0.00286(8) 0.00191(7) -0.00149(8)
O1 0.0271(9) 0.0223(9) 0.0274(9) 0.0056(7) 0.0026(7) -0.0032(7)
O2 0.0265(9) 0.0257(10) 0.0358(10) 0.0038(8) 0.0000(8) -0.0028(7)
O3 0.0347(10) 0.0276(10) 0.0313(10) 0.0085(8) 0.0023(8) -0.0069(8)
N1 0.0317(11) 0.0287(12) 0.0346(13) 0.0011(10) -0.0032(10) 0.0036(10)
N2 0.0361(12) 0.0236(11) 0.0278(12) 0.0056(9) 0.0048(9) 0.0015(9)
N3 0.0306(11) 0.0285(12) 0.0227(11) 0.0004(9) 0.0026(9) -0.0017(9)
N4 0.0301(11) 0.0172(10) 0.0312(12) -0.0010(9) 0.0027(9) -0.0021(9)
C1 0.0348(14) 0.0368(17) 0.0478(18) -0.0032(14) -0.0066(13) -0.0003(13)
C2 0.0359(16) 0.056(2) 0.063(2) -0.0084(17) -0.0107(15) 0.0060(15)
C3 0.0441(19) 0.064(2) 0.065(2) -0.0014(19) -0.0192(16) 0.0143(17)
C4 0.0539(19) 0.0436(18) 0.0455(19) 0.0055(15) -0.0057(15) 0.0173(16)
C5 0.0419(15) 0.0366(16) 0.0278(14) 0.0021(12) 0.0010(12) 0.0103(13)
C6 0.0483(17) 0.0270(15) 0.0379(16) 0.0087(12) 0.0047(13) 0.0076(13)
C7 0.0418(15) 0.0364(16) 0.0265(14) 0.0111(12) 0.0062(12) 0.0019(13)
C8 0.0358(14) 0.0326(14) 0.0209(13) -0.0027(11) 0.0006(11) -0.0017(12)
C9 0.0413(15) 0.0428(17) 0.0301(15) 0.0006(13) 0.0096(12) -0.0090(13)
C10 0.0314(14) 0.0432(17) 0.0385(16) -0.0086(13) 0.0089(12) -0.0072(13)
C11 0.0340(14) 0.0356(16) 0.0365(15) -0.0096(13) 0.0075(12) 0.0013(12)
C12 0.0332(13) 0.0297(14) 0.0228(13) -0.0069(11) 0.0016(10) 0.0015(11)
C13 0.0442(16) 0.0263(14) 0.0287(14) -0.0070(11) 0.0066(12) 0.0006(12)
C14 0.0505(18) 0.0360(17) 0.0485(19) -0.0024(14) 0.0084(15) 0.0095(14)
C15 0.081(3) 0.0345(18) 0.062(2) 0.0021(16) 0.0142(19) 0.0138(18)
C16 0.096(3) 0.0272(17) 0.058(2) -0.0031(15) 0.021(2) -0.0063(18)
C17 0.066(2) 0.0354(17) 0.0442(18) -0.0121(15) 0.0156(16) -0.0203(16)
C18 0.0453(16) 0.0321(15) 0.0298(14) -0.0093(12) 0.0065(12) -0.0043(13)
C19 0.0402(15) 0.0224(14) 0.0381(16) 0.0062(11) 0.0102(12) -0.0044(12)
C20 0.0306(13) 0.0194(13) 0.0394(15) 0.0019(11) 0.0049(11) -0.0008(11)
C21 0.0345(14) 0.0220(14) 0.0507(18) -0.0034(12) 0.0103(13) -0.0050(11)
C22 0.0355(15) 0.0302(15) 0.0530(19) -0.0124(14) 0.0029(13) -0.0056(12)
C23 0.0375(14) 0.0334(15) 0.0350(15) -0.0086(12) 0.0043(12) 0.0001(12)
C24 0.0307(13) 0.0233(13) 0.0314(14) -0.0010(11) 0.0047(11) -0.0009(11)
C25 0.0426(15) 0.0257(14) 0.0305(14) -0.0057(11) 0.0129(12) -0.0014(12)
C26 0.0391(15) 0.0306(15) 0.0467(17) -0.0066(13) 0.0151(13) -0.0061(13)
C27 0.0497(19) 0.046(2) 0.074(3) -0.0187(18) 0.0269(18) -0.0151(16)
C28 0.089(3) 0.0411(19) 0.073(3) -0.0128(19) 0.054(2) -0.027(2)
C29 0.112(3) 0.043(2) 0.045(2) 0.0029(16) 0.036(2) -0.015(2)
C30 0.071(2) 0.0345(16) 0.0336(17) -0.0012(13) 0.0107(15) -0.0068(15)
C31 0.0263(12) 0.0172(12) 0.0261(13) -0.0016(10) 0.0059(10) -0.0015(10)
C32 0.0293(12) 0.0194(12) 0.0263(13) -0.0029(10) 0.0036(10) 0.0017(10)
C33 0.0285(12) 0.0218(13) 0.0313(14) -0.0039(10) 0.0086(11) -0.0016(10)
C34 0.0294(13) 0.0271(14) 0.0418(16) -0.0033(12) 0.0066(11) -0.0046(12)
C35 0.0357(15) 0.0366(16) 0.0498(18) -0.0111(14) 0.0133(13) -0.0113(13)
C36 0.0529(18) 0.0405(17) 0.0351(16) -0.0015(13) 0.0146(14) -0.0205(15)
C37 0.0525(17) 0.0334(16) 0.0309(15) 0.0024(12) 0.0072(13) -0.0115(14)
C38 0.0340(13) 0.0263(13) 0.0269(14) -0.0007(11) 0.0062(11) -0.0067(11)
C39 0.0298(13) 0.0230(13) 0.0258(13) 0.0019(10) 0.0044(10) -0.0035(10)
C40 0.0306(13) 0.0206(13) 0.0375(15) 0.0051(11) 0.0020(11) 0.0011(11)
C41 0.0334(14) 0.0362(16) 0.0417(17) 0.0093(13) 0.0036(12) 0.0024(12)
C42 0.0306(15) 0.0487(19) 0.067(2) 0.0185(17) 0.0079(15) 0.0017(14)
C43 0.0369(16) 0.062(2) 0.067(2) 0.0255(19) -0.0126(16) -0.0104(16)
C44 0.0491(18) 0.061(2) 0.0449(19) 0.0101(16) -0.0142(15) -0.0083(16)
C45 0.0369(15) 0.0439(18) 0.0374(17) 0.0067(13) -0.0026(12) -0.0057(13)
O4 0.157(11) 0.070(5) 0.137(9) 0.027(5) -0.116(8) -0.039(6)
O5 0.113(6) 0.055(5) 0.142(6) -0.010(4) 0.038(5) 0.056(5)
O6 0.068(4) 0.063(4) 0.112(6) 0.030(4) 0.035(4) 0.009(3)
O4' 0.055(4) 0.143(9) 0.137(12) -0.036(8) -0.024(6) 0.031(5)
O5' 0.228(17) 0.042(6) 0.193(15) 0.026(7) -0.155(13) -0.061(9)
O6' 0.099(7) 0.134(10) 0.097(7) 0.050(6) 0.040(6) 0.031(7)
O8 0.0800(17) 0.0377(13) 0.0768(18) 0.0190(12) 0.0024(14) 0.0012(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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O5' Cl1 O4 120.5(6) . . ?
O5' Cl1 O4' 108.4(9) . . ?
O4 Cl1 O4' 34.7(6) . . ?
O5' Cl1 O8 118.0(5) . . ?
O4 Cl1 O8 117.4(4) . . ?
O4' Cl1 O8 106.3(7) . . ?
O5' Cl1 O5 32.3(9) . . ?
O4 Cl1 O5 111.4(7) . . ?
O4' Cl1 O5 85.1(6) . . ?
O8 Cl1 O5 105.8(4) . . ?
O5' Cl1 O6' 116.5(8) . . ?
O4 Cl1 O6' 69.2(6) . . ?
O4' Cl1 O6' 103.7(6) . . ?
O8 Cl1 O6' 102.6(3) . . ?
O5 Cl1 O6' 146.5(5) . . ?
O5' Cl1 O6 67.2(9) . . ?
O4 Cl1 O6 115.0(6) . . ?
O4' Cl1 O6 144.7(6) . . ?
O8 Cl1 O6 106.1(2) . . ?
O5 Cl1 O6 99.2(4) . . ?
O6' Cl1 O6 55.4(4) . . ?
O1 Cd1 O2 74.74(6) . . ?
O1 Cd1 N1 156.95(7) . . ?
O2 Cd1 N1 82.45(7) . . ?
O1 Cd1 N4 89.28(7) . . ?
O2 Cd1 N4 116.60(6) . . ?
N1 Cd1 N4 98.09(7) . . ?
O1 Cd1 N2 131.54(7) . . ?
O2 Cd1 N2 153.56(7) . . ?
N1 Cd1 N2 71.13(7) . . ?
N4 Cd1 N2 67.65(7) . . ?
O1 Cd1 N3 89.41(6) . . ?
O2 Cd1 N3 116.00(7) . . ?
N1 Cd1 N3 103.81(7) . . ?
N4 Cd1 N3 124.90(7) . . ?
N2 Cd1 N3 72.82(7) . . ?
C31 O1 Cd1 113.41(14) . . ?
C32 O2 Cd1 112.26(15) . . ?
C38 O3 C39 120.3(2) . . ?
C5 N1 C1 119.0(2) . . ?
C5 N1 Cd1 117.93(18) . . ?
C1 N1 Cd1 122.90(19) . . ?
C19 N2 C7 111.9(2) . . ?
C19 N2 C6 110.9(2) . . ?
C7 N2 C6 110.5(2) . . ?
C19 N2 Cd1 107.26(15) . . ?
C7 N2 Cd1 107.90(15) . . ?
C6 N2 Cd1 108.20(15) . . ?
C8 N3 C12 118.7(2) . . ?
C8 N3 Cd1 110.69(16) . . ?
C12 N3 Cd1 124.82(16) . . ?
C20 N4 C24 118.5(2) . . ?
C20 N4 Cd1 113.81(16) . . ?
C24 N4 Cd1 124.58(16) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.2(3) . . ?
N1 C5 C6 117.6(2) . . ?
C4 C5 C6 121.0(3) . . ?
N2 C6 C5 112.8(2) . . ?
N2 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N2 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N2 C7 C8 111.9(2) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N3 C8 C9 122.7(2) . . ?
N3 C8 C7 117.1(2) . . ?
C9 C8 C7 120.2(2) . . ?
C10 C9 C8 118.6(3) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C11 C10 C9 119.3(2) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N3 C12 C11 120.5(2) . . ?
N3 C12 C13 119.1(2) . . ?
C11 C12 C13 120.4(2) . . ?
C18 C13 C14 118.7(3) . . ?
C18 C13 C12 120.8(3) . . ?
C14 C13 C12 120.4(3) . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 120.3(3) . . ?
C13 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
N2 C19 C20 111.8(2) . . ?
N2 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N2 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
N4 C20 C21 122.3(2) . . ?
N4 C20 C19 116.8(2) . . ?
C21 C20 C19 120.9(2) . . ?
C22 C21 C20 118.9(3) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 119.4(3) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
N4 C24 C23 121.5(2) . . ?
N4 C24 C25 117.1(2) . . ?
C23 C24 C25 121.4(2) . . ?
C26 C25 C30 119.6(3) . . ?
C26 C25 C24 120.5(2) . . ?
C30 C25 C24 119.9(3) . . ?
C25 C26 C27 120.1(3) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 119.7(3) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C29 C28 C27 120.1(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C30 C29 C28 120.7(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C25 119.8(3) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
O1 C31 C39 123.3(2) . . ?
O1 C31 C32 118.5(2) . . ?
C39 C31 C32 118.2(2) . . ?
O2 C32 C33 121.6(2) . . ?
O2 C32 C31 120.6(2) . . ?
C33 C32 C31 117.7(2) . . ?
C38 C33 C34 118.8(2) . . ?
C38 C33 C32 119.4(2) . . ?
C34 C33 C32 121.9(2) . . ?
C35 C34 C33 119.3(3) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 120.4(3) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C37 C36 C35 121.6(3) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C38 118.0(3) . . ?
C36 C37 H37 121.0 . . ?
C38 C37 H37 121.0 . . ?
O3 C38 C33 121.9(2) . . ?
O3 C38 C37 116.1(2) . . ?
C33 C38 C37 122.0(2) . . ?
C31 C39 O3 122.5(2) . . ?
C31 C39 C40 127.2(2) . . ?
O3 C39 C40 110.2(2) . . ?
C45 C40 C41 118.4(3) . . ?
C45 C40 C39 120.0(2) . . ?
C41 C40 C39 121.6(2) . . ?
C42 C41 C40 120.6(3) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 120.4(3) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C44 C43 C42 119.5(3) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C45 119.9(3) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C40 121.3(3) . . ?
C44 C45 H45 119.4 . . ?
C40 C45 H45 119.4 . . ?
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
Cl1 O5' 1.312(9) . ?
Cl1 O4 1.350(8) . ?
Cl1 O4' 1.409(11) . ?
Cl1 O8 1.420(2) . ?
Cl1 O5 1.458(7) . ?
Cl1 O6' 1.459(9) . ?
Cl1 O6 1.466(5) . ?
Cd1 O1 2.2134(17) . ?
Cd1 O2 2.2792(16) . ?
Cd1 N1 2.337(2) . ?
Cd1 N4 2.420(2) . ?
Cd1 N2 2.430(2) . ?
Cd1 N3 2.4636(19) . ?
O1 C31 1.316(3) . ?
O2 C32 1.256(3) . ?
O3 C38 1.359(3) . ?
O3 C39 1.380(3) . ?
N1 C5 1.339(3) . ?
N1 C1 1.343(4) . ?
N2 C19 1.462(3) . ?
N2 C7 1.471(3) . ?
N2 C6 1.479(3) . ?
N3 C8 1.350(3) . ?
N3 C12 1.357(3) . ?
N4 C20 1.350(3) . ?
N4 C24 1.351(3) . ?
C1 C2 1.378(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.372(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.507(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.508(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.383(4) . ?
C9 C10 1.381(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.484(4) . ?
C13 C18 1.387(4) . ?
C13 C14 1.398(4) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.512(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.379(4) . ?
C21 C22 1.378(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.376(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.483(4) . ?
C25 C26 1.390(4) . ?
C25 C30 1.391(4) . ?
C26 C27 1.390(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.376(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C39 1.377(3) . ?
C31 C32 1.458(3) . ?
C32 C33 1.450(3) . ?
C33 C38 1.379(4) . ?
C33 C34 1.414(3) . ?
C34 C35 1.380(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.367(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.403(4) . ?
C37 H37 0.9500 . ?
C39 C40 1.466(3) . ?
C40 C45 1.387(4) . ?
C40 C41 1.392(4) . ?
C41 C42 1.380(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.391(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.379(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
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
O2 Cd1 O1 C31 5.31(15) . . . . ?
N1 Cd1 O1 C31 -3.3(3) . . . . ?
N4 Cd1 O1 C31 -112.57(15) . . . . ?
N2 Cd1 O1 C31 -171.29(14) . . . . ?
N3 Cd1 O1 C31 122.52(15) . . . . ?
O1 Cd1 O2 C32 -5.53(15) . . . . ?
N1 Cd1 O2 C32 171.07(17) . . . . ?
N4 Cd1 O2 C32 75.78(17) . . . . ?
N2 Cd1 O2 C32 168.75(16) . . . . ?
N3 Cd1 O2 C32 -87.20(17) . . . . ?
O1 Cd1 N1 C5 -155.08(18) . . . . ?
O2 Cd1 N1 C5 -163.5(2) . . . . ?
N4 Cd1 N1 C5 -47.5(2) . . . . ?
N2 Cd1 N1 C5 15.43(18) . . . . ?
N3 Cd1 N1 C5 81.5(2) . . . . ?
O1 Cd1 N1 C1 19.8(3) . . . . ?
O2 Cd1 N1 C1 11.4(2) . . . . ?
N4 Cd1 N1 C1 127.3(2) . . . . ?
N2 Cd1 N1 C1 -169.7(2) . . . . ?
N3 Cd1 N1 C1 -103.6(2) . . . . ?
O1 Cd1 N2 C19 27.50(19) . . . . ?
O2 Cd1 N2 C19 -145.12(16) . . . . ?
N1 Cd1 N2 C19 -147.55(17) . . . . ?
N4 Cd1 N2 C19 -40.02(15) . . . . ?
N3 Cd1 N2 C19 100.75(16) . . . . ?
O1 Cd1 N2 C7 -93.21(18) . . . . ?
O2 Cd1 N2 C7 94.2(2) . . . . ?
N1 Cd1 N2 C7 91.74(17) . . . . ?
N4 Cd1 N2 C7 -160.73(18) . . . . ?
N3 Cd1 N2 C7 -19.96(16) . . . . ?
O1 Cd1 N2 C6 147.21(16) . . . . ?
O2 Cd1 N2 C6 -25.4(3) . . . . ?
N1 Cd1 N2 C6 -27.84(16) . . . . ?
N4 Cd1 N2 C6 79.69(17) . . . . ?
N3 Cd1 N2 C6 -139.54(18) . . . . ?
O1 Cd1 N3 C8 128.91(17) . . . . ?
O2 Cd1 N3 C8 -158.42(15) . . . . ?
N1 Cd1 N3 C8 -70.17(17) . . . . ?
N4 Cd1 N3 C8 40.20(19) . . . . ?
N2 Cd1 N3 C8 -5.30(16) . . . . ?
O1 Cd1 N3 C12 -23.7(2) . . . . ?
O2 Cd1 N3 C12 48.9(2) . . . . ?
N1 Cd1 N3 C12 137.18(19) . . . . ?
N4 Cd1 N3 C12 -112.5(2) . . . . ?
N2 Cd1 N3 C12 -158.0(2) . . . . ?
O1 Cd1 N4 C20 -103.61(17) . . . . ?
O2 Cd1 N4 C20 -176.12(16) . . . . ?
N1 Cd1 N4 C20 98.31(18) . . . . ?
N2 Cd1 N4 C20 32.62(17) . . . . ?
N3 Cd1 N4 C20 -14.8(2) . . . . ?
O1 Cd1 N4 C24 56.2(2) . . . . ?
O2 Cd1 N4 C24 -16.3(2) . . . . ?
N1 Cd1 N4 C24 -101.9(2) . . . . ?
N2 Cd1 N4 C24 -167.6(2) . . . . ?
N3 Cd1 N4 C24 144.96(18) . . . . ?
C5 N1 C1 C2 1.1(4) . . . . ?
Cd1 N1 C1 C2 -173.7(2) . . . . ?
N1 C1 C2 C3 -2.0(5) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C1 N1 C5 C4 1.0(4) . . . . ?
Cd1 N1 C5 C4 176.0(2) . . . . ?
C1 N1 C5 C6 -174.6(2) . . . . ?
Cd1 N1 C5 C6 0.5(3) . . . . ?
C3 C4 C5 N1 -2.1(5) . . . . ?
C3 C4 C5 C6 173.3(3) . . . . ?
C19 N2 C6 C5 155.6(2) . . . . ?
C7 N2 C6 C5 -79.7(3) . . . . ?
Cd1 N2 C6 C5 38.2(3) . . . . ?
N1 C5 C6 N2 -27.6(3) . . . . ?
C4 C5 C6 N2 156.8(3) . . . . ?
C19 N2 C7 C8 -75.5(3) . . . . ?
C6 N2 C7 C8 160.4(2) . . . . ?
Cd1 N2 C7 C8 42.3(2) . . . . ?
C12 N3 C8 C9 2.6(4) . . . . ?
Cd1 N3 C8 C9 -151.9(2) . . . . ?
C12 N3 C8 C7 -174.3(2) . . . . ?
Cd1 N3 C8 C7 31.1(3) . . . . ?
N2 C7 C8 N3 -52.5(3) . . . . ?
N2 C7 C8 C9 130.4(3) . . . . ?
N3 C8 C9 C10 -0.8(4) . . . . ?
C7 C8 C9 C10 176.1(3) . . . . ?
C8 C9 C10 C11 -0.9(4) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C8 N3 C12 C11 -2.7(4) . . . . ?
Cd1 N3 C12 C11 147.9(2) . . . . ?
C8 N3 C12 C13 173.9(2) . . . . ?
Cd1 N3 C12 C13 -35.5(3) . . . . ?
C10 C11 C12 N3 1.0(4) . . . . ?
C10 C11 C12 C13 -175.5(3) . . . . ?
N3 C12 C13 C18 -32.4(4) . . . . ?
C11 C12 C13 C18 144.2(3) . . . . ?
N3 C12 C13 C14 151.1(3) . . . . ?
C11 C12 C13 C14 -32.3(4) . . . . ?
C18 C13 C14 C15 0.0(4) . . . . ?
C12 C13 C14 C15 176.6(3) . . . . ?
C13 C14 C15 C16 0.6(5) . . . . ?
C14 C15 C16 C17 -0.5(5) . . . . ?
C15 C16 C17 C18 -0.1(5) . . . . ?
C14 C13 C18 C17 -0.7(4) . . . . ?
C12 C13 C18 C17 -177.2(2) . . . . ?
C16 C17 C18 C13 0.7(4) . . . . ?
C7 N2 C19 C20 163.6(2) . . . . ?
C6 N2 C19 C20 -72.6(3) . . . . ?
Cd1 N2 C19 C20 45.4(2) . . . . ?
C24 N4 C20 C21 -1.5(4) . . . . ?
Cd1 N4 C20 C21 159.6(2) . . . . ?
C24 N4 C20 C19 179.3(2) . . . . ?
Cd1 N4 C20 C19 -19.6(3) . . . . ?
N2 C19 C20 N4 -18.3(3) . . . . ?
N2 C19 C20 C21 162.5(2) . . . . ?
N4 C20 C21 C22 0.9(4) . . . . ?
C19 C20 C21 C22 -179.9(3) . . . . ?
C20 C21 C22 C23 0.4(4) . . . . ?
C21 C22 C23 C24 -1.1(4) . . . . ?
C20 N4 C24 C23 0.7(4) . . . . ?
Cd1 N4 C24 C23 -158.21(19) . . . . ?
C20 N4 C24 C25 -176.7(2) . . . . ?
Cd1 N4 C24 C25 24.4(3) . . . . ?
C22 C23 C24 N4 0.6(4) . . . . ?
C22 C23 C24 C25 177.9(3) . . . . ?
N4 C24 C25 C26 46.1(4) . . . . ?
C23 C24 C25 C26 -131.4(3) . . . . ?
N4 C24 C25 C30 -135.6(3) . . . . ?
C23 C24 C25 C30 47.0(4) . . . . ?
C30 C25 C26 C27 -1.1(4) . . . . ?
C24 C25 C26 C27 177.2(3) . . . . ?
C25 C26 C27 C28 0.8(4) . . . . ?
C26 C27 C28 C29 0.6(5) . . . . ?
C27 C28 C29 C30 -1.6(5) . . . . ?
C28 C29 C30 C25 1.3(5) . . . . ?
C26 C25 C30 C29 0.0(4) . . . . ?
C24 C25 C30 C29 -178.3(3) . . . . ?
Cd1 O1 C31 C39 173.04(19) . . . . ?
Cd1 O1 C31 C32 -4.8(3) . . . . ?
Cd1 O2 C32 C33 -173.40(17) . . . . ?
Cd1 O2 C32 C31 5.1(3) . . . . ?
O1 C31 C32 O2 -0.4(3) . . . . ?
C39 C31 C32 O2 -178.3(2) . . . . ?
O1 C31 C32 C33 178.2(2) . . . . ?
C39 C31 C32 C33 0.3(3) . . . . ?
O2 C32 C33 C38 178.7(2) . . . . ?
C31 C32 C33 C38 0.1(3) . . . . ?
O2 C32 C33 C34 -0.5(4) . . . . ?
C31 C32 C33 C34 -179.1(2) . . . . ?
C38 C33 C34 C35 0.1(4) . . . . ?
C32 C33 C34 C35 179.4(2) . . . . ?
C33 C34 C35 C36 1.6(4) . . . . ?
C34 C35 C36 C37 -1.5(4) . . . . ?
C35 C36 C37 C38 -0.4(4) . . . . ?
C39 O3 C38 C33 0.2(4) . . . . ?
C39 O3 C38 C37 -178.9(2) . . . . ?
C34 C33 C38 O3 178.9(2) . . . . ?
C32 C33 C38 O3 -0.4(4) . . . . ?
C34 C33 C38 C37 -2.0(4) . . . . ?
C32 C33 C38 C37 178.7(2) . . . . ?
C36 C37 C38 O3 -178.7(2) . . . . ?
C36 C37 C38 C33 2.2(4) . . . . ?
O1 C31 C39 O3 -178.3(2) . . . . ?
C32 C31 C39 O3 -0.5(4) . . . . ?
O1 C31 C39 C40 -1.4(4) . . . . ?
C32 C31 C39 C40 176.4(2) . . . . ?
C38 O3 C39 C31 0.2(4) . . . . ?
C38 O3 C39 C40 -177.1(2) . . . . ?
C31 C39 C40 C45 -136.0(3) . . . . ?
O3 C39 C40 C45 41.2(3) . . . . ?
C31 C39 C40 C41 44.4(4) . . . . ?
O3 C39 C40 C41 -138.4(2) . . . . ?
C45 C40 C41 C42 -0.1(4) . . . . ?
C39 C40 C41 C42 179.6(3) . . . . ?
C40 C41 C42 C43 0.7(5) . . . . ?
C41 C42 C43 C44 -0.1(5) . . . . ?
C42 C43 C44 C45 -1.2(5) . . . . ?
C43 C44 C45 C40 1.8(5) . . . . ?
C41 C40 C45 C44 -1.2(4) . . . . ?
C39 C40 C45 C44 179.2(3) . . . . ?
|
1501472.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501472.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_1501472
loop_
_publ_author_name
'Katarzyna Grubel'
'Brynna J. Laughlin'
'Thora R. Maltais'
'Rhett C. Smith'
'Atta M. Arif'
'Lisa M. Berreau'
_publ_section_title
;
Photochemically-induced dioxygenase-type CO-release reactivity of Group
12 metal flavonolate complexes
;
_journal_issue 37
_journal_name_full 'Chemical Communications'
_journal_page_first 10431
_journal_page_last 10433
_journal_paper_doi 10.1039/c1cc13961d
_journal_volume 47
_journal_year 2011
_chemical_formula_moiety 'C45 H35 Hg N4 O3, Cl O4'
_chemical_formula_sum 'C45 H35 Cl Hg N4 O7'
_chemical_formula_weight 979.81
_chemical_name_systematic
;
?
;
_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 95.0070(9)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.4117(2)
_cell_length_b 16.3761(2)
_cell_length_c 20.9794(3)
_cell_measurement_reflns_used 8852
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 1.018
_cell_volume 3905.65(10)
_computing_cell_refinement DENZO-SMN
_computing_data_collection 'Nonius COLLECT'
_computing_data_reduction DENZO-SMN
_computing_molecular_graphics 'WinGX, Ortep3'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution SIR97
_diffrn_ambient_temperature 150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method 'Phi and Omega sacn'
_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 0.0366
_diffrn_reflns_av_sigmaI/netI 0.0553
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 16904
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 2.31
_exptl_absorpt_coefficient_mu 4.068
_exptl_absorpt_correction_T_max 0.6865
_exptl_absorpt_correction_T_min 0.4967
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.666
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1944
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.10
_refine_diff_density_max 1.486
_refine_diff_density_min -0.784
_refine_diff_density_rms 0.107
_refine_ls_extinction_coef 0.00090(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 1.039
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 552
_refine_ls_number_reflns 8946
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0565
_refine_ls_R_factor_gt 0.0324
_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^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0608
_refine_ls_wR_factor_ref 0.0674
_reflns_number_gt 6666
_reflns_number_total 8946
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1cc13961d.txt
_cod_data_source_block usu212
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1501472
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
Hg1 Hg 0.240696(12) 0.143923(8) 0.603733(6) 0.02729(6) Uani 1 1 d . . .
Cl1 Cl -0.38444(10) 0.36323(6) 0.71950(6) 0.0530(3) Uani 1 1 d . . .
O1 O 0.1278(2) 0.21553(14) 0.53453(11) 0.0298(6) Uani 1 1 d . . .
O2 O 0.3626(2) 0.24959(15) 0.56466(11) 0.0339(6) Uani 1 1 d . . .
O3 O 0.1832(2) 0.37183(15) 0.41872(11) 0.0339(6) Uani 1 1 d . . .
O4 O -0.3534(3) 0.29642(19) 0.76034(17) 0.0708(10) Uani 1 1 d . A .
O5 O -0.5058(7) 0.3677(8) 0.7097(5) 0.101(4) Uani 0.545(11) 1 d PD A 1
O6 O -0.3443(8) 0.3405(5) 0.6581(4) 0.084(4) Uani 0.545(11) 1 d PD A 1
O7 O -0.3411(14) 0.4358(6) 0.7400(6) 0.136(8) Uani 0.545(11) 1 d PD A 1
O5A O -0.4684(19) 0.3546(8) 0.6722(9) 0.186(14) Uani 0.455(11) 1 d PD A 2
O6A O -0.2746(9) 0.3979(7) 0.7025(6) 0.091(5) Uani 0.455(11) 1 d PD A 2
O7A O -0.4116(15) 0.4293(8) 0.7641(7) 0.128(7) Uani 0.455(11) 1 d PD A 2
N1 N 0.4177(3) 0.10528(18) 0.65864(14) 0.0345(7) Uani 1 1 d . . .
N2 N 0.2071(3) 0.02172(17) 0.66869(13) 0.0310(7) Uani 1 1 d . . .
N3 N 0.1143(3) 0.18569(18) 0.69352(13) 0.0305(7) Uani 1 1 d . . .
N4 N 0.2056(3) 0.01668(17) 0.53960(13) 0.0297(7) Uani 1 1 d . . .
C1 C 0.5138(4) 0.1528(3) 0.6609(2) 0.0432(10) Uani 1 1 d . . .
H1 H 0.5077 0.2059 0.6427 0.052 Uiso 1 1 calc R . .
C2 C 0.6207(4) 0.1271(3) 0.6889(2) 0.0541(12) Uani 1 1 d . . .
H2 H 0.6879 0.1614 0.6890 0.065 Uiso 1 1 calc R . .
C3 C 0.6295(4) 0.0508(3) 0.7170(2) 0.0581(13) Uani 1 1 d . . .
H3 H 0.7024 0.0318 0.7368 0.070 Uiso 1 1 calc R . .
C4 C 0.5297(4) 0.0026(3) 0.7155(2) 0.0493(11) Uani 1 1 d . . .
H4 H 0.5331 -0.0495 0.7354 0.059 Uiso 1 1 calc R . .
C5 C 0.4253(4) 0.0303(2) 0.68503(17) 0.0361(9) Uani 1 1 d . . .
C6 C 0.3181(4) -0.0240(2) 0.67632(19) 0.0384(9) Uani 1 1 d . . .
H6A H 0.3241 -0.0587 0.6381 0.046 Uiso 1 1 calc R . .
H6B H 0.3171 -0.0604 0.7139 0.046 Uiso 1 1 calc R . .
C7 C 0.1729(4) 0.0501(2) 0.73172(16) 0.0378(9) Uani 1 1 d . . .
H7A H 0.2442 0.0687 0.7580 0.045 Uiso 1 1 calc R . .
H7B H 0.1393 0.0036 0.7542 0.045 Uiso 1 1 calc R . .
C8 C 0.0847(3) 0.1186(2) 0.72607(16) 0.0318(8) Uani 1 1 d . . .
C9 C -0.0170(4) 0.1127(2) 0.75596(17) 0.0375(9) Uani 1 1 d . . .
H9 H -0.0356 0.0640 0.7775 0.045 Uiso 1 1 calc R . .
C10 C -0.0920(4) 0.1794(3) 0.75397(18) 0.0399(10) Uani 1 1 d . . .
H10 H -0.1627 0.1773 0.7747 0.048 Uiso 1 1 calc R . .
C11 C -0.0629(3) 0.2491(2) 0.72153(16) 0.0366(9) Uani 1 1 d . . .
H11 H -0.1136 0.2951 0.7196 0.044 Uiso 1 1 calc R . .
C12 C 0.0420(3) 0.2512(2) 0.69154(16) 0.0305(8) Uani 1 1 d . . .
C13 C 0.0776(4) 0.3264(2) 0.65956(17) 0.0335(9) Uani 1 1 d . . .
C14 C -0.0063(4) 0.3809(2) 0.6323(2) 0.0456(10) Uani 1 1 d . . .
H14 H -0.0876 0.3687 0.6330 0.055 Uiso 1 1 calc R . .
C15 C 0.0278(5) 0.4525(3) 0.6045(2) 0.0583(13) Uani 1 1 d . . .
H15 H -0.0301 0.4889 0.5857 0.070 Uiso 1 1 calc R . .
C16 C 0.1452(5) 0.4714(3) 0.6037(2) 0.0583(13) Uani 1 1 d . . .
H16 H 0.1681 0.5209 0.5847 0.070 Uiso 1 1 calc R . .
C17 C 0.2295(4) 0.4184(2) 0.63050(19) 0.0472(11) Uani 1 1 d . . .
H17 H 0.3105 0.4314 0.6297 0.057 Uiso 1 1 calc R . .
C18 C 0.1965(4) 0.3460(2) 0.65879(17) 0.0371(9) Uani 1 1 d . . .
H18 H 0.2549 0.3100 0.6776 0.044 Uiso 1 1 calc R . .
C19 C 0.1137(4) -0.0267(2) 0.63441(17) 0.0358(9) Uani 1 1 d . . .
H19A H 0.0369 0.0000 0.6385 0.043 Uiso 1 1 calc R . .
H19B H 0.1114 -0.0815 0.6543 0.043 Uiso 1 1 calc R . .
C20 C 0.1322(3) -0.0361(2) 0.56390(17) 0.0322(8) Uani 1 1 d . . .
C21 C 0.0726(4) -0.0955(2) 0.52780(19) 0.0386(9) Uani 1 1 d . . .
H21 H 0.0200 -0.1314 0.5465 0.046 Uiso 1 1 calc R . .
C22 C 0.0910(4) -0.1017(2) 0.4636(2) 0.0397(9) Uani 1 1 d . . .
H22 H 0.0512 -0.1423 0.4375 0.048 Uiso 1 1 calc R . .
C23 C 0.1678(3) -0.0483(2) 0.43805(18) 0.0370(9) Uani 1 1 d . . .
H23 H 0.1820 -0.0522 0.3942 0.044 Uiso 1 1 calc R . .
C24 C 0.2244(3) 0.0111(2) 0.47660(17) 0.0312(8) Uani 1 1 d . . .
C25 C 0.3092(4) 0.0691(2) 0.45225(17) 0.0352(9) Uani 1 1 d . . .
C26 C 0.4154(4) 0.0845(2) 0.4868(2) 0.0414(10) Uani 1 1 d . . .
H26 H 0.4335 0.0586 0.5270 0.050 Uiso 1 1 calc R . .
C27 C 0.4961(4) 0.1379(3) 0.4633(3) 0.0605(14) Uani 1 1 d . . .
H27 H 0.5702 0.1471 0.4864 0.073 Uiso 1 1 calc R . .
C28 C 0.4671(5) 0.1777(3) 0.4053(3) 0.0678(16) Uani 1 1 d . . .
H28 H 0.5216 0.2142 0.3887 0.081 Uiso 1 1 calc R . .
C29 C 0.3598(5) 0.1640(3) 0.3723(2) 0.0638(15) Uani 1 1 d . . .
H29 H 0.3395 0.1925 0.3334 0.077 Uiso 1 1 calc R . .
C30 C 0.2812(4) 0.1096(3) 0.39470(18) 0.0475(11) Uani 1 1 d . . .
H30 H 0.2079 0.0997 0.3709 0.057 Uiso 1 1 calc R . .
C31 C 0.1826(3) 0.2715(2) 0.50319(15) 0.0258(7) Uani 1 1 d . . .
C32 C 0.3064(3) 0.2872(2) 0.52015(16) 0.0276(8) Uani 1 1 d . . .
C33 C 0.3639(3) 0.3475(2) 0.48286(16) 0.0280(8) Uani 1 1 d . . .
C34 C 0.4842(3) 0.3658(2) 0.49412(19) 0.0368(9) Uani 1 1 d . . .
H34 H 0.5308 0.3386 0.5274 0.044 Uiso 1 1 calc R . .
C35 C 0.5346(4) 0.4227(2) 0.45734(19) 0.0421(10) Uani 1 1 d . . .
H35 H 0.6164 0.4337 0.4644 0.051 Uiso 1 1 calc R . .
C36 C 0.4662(4) 0.4646(2) 0.40953(18) 0.0450(11) Uani 1 1 d . . .
H36 H 0.5018 0.5052 0.3853 0.054 Uiso 1 1 calc R . .
C37 C 0.3488(4) 0.4482(2) 0.39692(18) 0.0414(10) Uani 1 1 d . . .
H37 H 0.3027 0.4768 0.3643 0.050 Uiso 1 1 calc R . .
C38 C 0.2987(3) 0.3881(2) 0.43349(17) 0.0314(8) Uani 1 1 d . . .
C39 C 0.1264(3) 0.3141(2) 0.45247(16) 0.0288(8) Uani 1 1 d . . .
C40 C 0.0050(3) 0.3044(2) 0.42547(17) 0.0314(8) Uani 1 1 d . . .
C41 C -0.0887(4) 0.2988(2) 0.4648(2) 0.0418(10) Uani 1 1 d . . .
H41 H -0.0736 0.3013 0.5100 0.050 Uiso 1 1 calc R . .
C42 C -0.2028(4) 0.2896(3) 0.4373(2) 0.0553(13) Uani 1 1 d . . .
H42 H -0.2658 0.2853 0.4639 0.066 Uiso 1 1 calc R . .
C43 C -0.2257(4) 0.2864(3) 0.3710(2) 0.0599(13) Uani 1 1 d . . .
H43 H -0.3043 0.2809 0.3524 0.072 Uiso 1 1 calc R . .
C44 C -0.1349(4) 0.2914(3) 0.3326(2) 0.0565(13) Uani 1 1 d . . .
H44 H -0.1503 0.2877 0.2874 0.068 Uiso 1 1 calc R . .
C45 C -0.0210(4) 0.3018(3) 0.35941(18) 0.0425(10) Uani 1 1 d . . .
H45 H 0.0410 0.3073 0.3322 0.051 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
Hg1 0.03265(9) 0.02100(8) 0.02826(8) 0.00423(6) 0.00286(5) -0.00119(6)
Cl1 0.0502(7) 0.0334(6) 0.0738(8) 0.0114(5) -0.0033(6) 0.0000(5)
O1 0.0330(15) 0.0231(13) 0.0333(13) 0.0085(10) 0.0036(11) -0.0028(11)
O2 0.0303(15) 0.0302(14) 0.0408(14) 0.0073(12) 0.0000(11) -0.0033(11)
O3 0.0367(16) 0.0304(14) 0.0349(14) 0.0083(11) 0.0038(11) -0.0050(11)
O4 0.086(3) 0.0416(19) 0.084(2) 0.0229(18) 0.005(2) 0.0000(18)
O5 0.043(5) 0.160(10) 0.096(8) -0.035(7) -0.016(5) 0.038(5)
O6 0.076(6) 0.093(7) 0.085(6) 0.042(5) 0.028(5) 0.024(5)
O7 0.201(17) 0.050(6) 0.135(12) 0.038(7) -0.111(11) -0.071(9)
O5A 0.28(3) 0.080(9) 0.163(16) 0.043(10) -0.189(18) -0.080(13)
O6A 0.074(7) 0.080(9) 0.124(11) 0.037(7) 0.031(7) 0.000(6)
O7A 0.182(15) 0.074(10) 0.135(11) 0.002(8) 0.051(10) 0.080(10)
N1 0.039(2) 0.0282(16) 0.0355(17) 0.0038(14) -0.0010(14) 0.0031(14)
N2 0.0380(19) 0.0264(16) 0.0290(15) 0.0056(13) 0.0058(13) 0.0014(14)
N3 0.0338(18) 0.0339(17) 0.0238(15) -0.0040(13) 0.0032(13) -0.0002(14)
N4 0.0375(19) 0.0186(15) 0.0336(16) 0.0026(13) 0.0068(14) -0.0025(13)
C1 0.036(2) 0.041(2) 0.050(2) -0.002(2) -0.0070(19) 0.0011(19)
C2 0.040(3) 0.056(3) 0.063(3) -0.008(2) -0.009(2) 0.003(2)
C3 0.047(3) 0.061(3) 0.063(3) 0.003(2) -0.012(2) 0.015(2)
C4 0.055(3) 0.045(3) 0.047(2) 0.007(2) -0.002(2) 0.019(2)
C5 0.045(3) 0.032(2) 0.0309(19) 0.0020(16) 0.0054(17) 0.0102(18)
C6 0.047(3) 0.028(2) 0.041(2) 0.0111(17) 0.0059(18) 0.0086(18)
C7 0.052(3) 0.037(2) 0.0256(18) 0.0080(16) 0.0088(17) 0.0065(19)
C8 0.039(2) 0.035(2) 0.0223(17) -0.0022(15) 0.0047(15) -0.0016(17)
C9 0.045(3) 0.037(2) 0.032(2) 0.0026(17) 0.0119(18) -0.0062(19)
C10 0.031(2) 0.053(3) 0.038(2) -0.0085(19) 0.0139(17) -0.008(2)
C11 0.039(2) 0.040(2) 0.0318(19) -0.0048(17) 0.0092(17) 0.0031(18)
C12 0.033(2) 0.0297(19) 0.0286(18) -0.0075(16) 0.0023(15) -0.0024(16)
C13 0.042(2) 0.0245(18) 0.035(2) -0.0084(16) 0.0053(17) -0.0014(17)
C14 0.045(3) 0.035(2) 0.058(3) 0.001(2) 0.011(2) 0.0117(19)
C15 0.075(4) 0.034(3) 0.067(3) 0.006(2) 0.016(3) 0.015(2)
C16 0.088(4) 0.029(2) 0.060(3) -0.002(2) 0.018(3) -0.006(2)
C17 0.062(3) 0.035(2) 0.046(2) -0.015(2) 0.016(2) -0.018(2)
C18 0.045(2) 0.033(2) 0.034(2) -0.0088(17) 0.0064(17) -0.0078(18)
C19 0.046(3) 0.0221(19) 0.041(2) 0.0066(16) 0.0103(18) -0.0049(17)
C20 0.037(2) 0.0194(18) 0.040(2) 0.0033(15) 0.0042(17) 0.0032(16)
C21 0.039(2) 0.023(2) 0.055(2) -0.0026(17) 0.0109(19) -0.0065(17)
C22 0.038(2) 0.028(2) 0.053(2) -0.0110(19) 0.0053(19) -0.0048(17)
C23 0.042(2) 0.033(2) 0.037(2) -0.0075(17) 0.0083(17) -0.0001(18)
C24 0.035(2) 0.0241(19) 0.0350(19) 0.0012(16) 0.0048(16) 0.0042(16)
C25 0.048(2) 0.0262(19) 0.0340(19) -0.0056(16) 0.0178(17) -0.0026(18)
C26 0.043(3) 0.038(2) 0.046(2) -0.0060(19) 0.0166(19) -0.0039(19)
C27 0.051(3) 0.060(3) 0.075(3) -0.024(3) 0.030(3) -0.017(2)
C28 0.098(5) 0.043(3) 0.070(3) -0.014(3) 0.053(3) -0.026(3)
C29 0.105(5) 0.046(3) 0.047(3) 0.002(2) 0.040(3) -0.013(3)
C30 0.070(3) 0.039(2) 0.035(2) 0.0008(19) 0.013(2) -0.008(2)
C31 0.031(2) 0.0184(17) 0.0291(18) -0.0017(14) 0.0085(15) 0.0014(14)
C32 0.030(2) 0.0217(18) 0.0314(18) -0.0018(15) 0.0053(15) 0.0015(15)
C33 0.031(2) 0.0225(18) 0.0314(18) -0.0016(15) 0.0104(15) -0.0032(15)
C34 0.034(2) 0.029(2) 0.048(2) -0.0033(17) 0.0066(18) -0.0037(17)
C35 0.034(2) 0.039(2) 0.055(2) -0.009(2) 0.0144(19) -0.0124(19)
C36 0.059(3) 0.040(2) 0.039(2) -0.0014(19) 0.019(2) -0.021(2)
C37 0.052(3) 0.039(2) 0.034(2) 0.0053(17) 0.0074(18) -0.015(2)
C38 0.034(2) 0.0283(19) 0.0328(19) -0.0021(16) 0.0068(16) -0.0046(16)
C39 0.033(2) 0.0230(18) 0.0307(18) 0.0007(15) 0.0067(16) -0.0003(15)
C40 0.031(2) 0.0221(18) 0.042(2) 0.0060(16) 0.0039(17) 0.0015(15)
C41 0.039(3) 0.032(2) 0.054(3) 0.0108(19) 0.006(2) 0.0020(18)
C42 0.033(3) 0.049(3) 0.085(4) 0.024(3) 0.012(2) 0.003(2)
C43 0.046(3) 0.054(3) 0.077(3) 0.025(3) -0.009(3) -0.004(2)
C44 0.048(3) 0.061(3) 0.057(3) 0.011(2) -0.017(2) -0.009(2)
C45 0.039(3) 0.046(3) 0.042(2) 0.0045(19) 0.0008(19) -0.0040(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'
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'
Hg Hg -2.3894 9.2266 '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
O1 Hg1 N1 155.23(10) . . ?
O1 Hg1 O2 73.37(8) . . ?
N1 Hg1 O2 82.05(10) . . ?
O1 Hg1 N2 133.43(9) . . ?
N1 Hg1 N2 71.10(11) . . ?
O2 Hg1 N2 153.15(9) . . ?
O1 Hg1 N4 91.84(9) . . ?
N1 Hg1 N4 97.57(10) . . ?
O2 Hg1 N4 119.16(9) . . ?
N2 Hg1 N4 66.12(9) . . ?
O1 Hg1 N3 90.47(9) . . ?
N1 Hg1 N3 103.23(10) . . ?
O2 Hg1 N3 115.92(9) . . ?
N2 Hg1 N3 71.72(10) . . ?
N4 Hg1 N3 123.03(10) . . ?
O5A Cl1 O7 123.7(7) . . ?
O5A Cl1 O5 41.0(11) . . ?
O7 Cl1 O5 109.6(9) . . ?
O5A Cl1 O4 119.8(5) . . ?
O7 Cl1 O4 115.1(4) . . ?
O5 Cl1 O4 109.0(6) . . ?
O5A Cl1 O6A 116.2(10) . . ?
O7 Cl1 O6A 55.3(7) . . ?
O5 Cl1 O6A 144.9(7) . . ?
O4 Cl1 O6A 106.0(5) . . ?
O5A Cl1 O6 64.7(11) . . ?
O7 Cl1 O6 112.0(8) . . ?
O5 Cl1 O6 105.7(5) . . ?
O4 Cl1 O6 104.9(3) . . ?
O6A Cl1 O6 62.3(6) . . ?
O5A Cl1 O7A 111.9(11) . . ?
O7 Cl1 O7A 40.8(8) . . ?
O5 Cl1 O7A 78.1(8) . . ?
O4 Cl1 O7A 103.7(6) . . ?
O6A Cl1 O7A 95.9(7) . . ?
O6 Cl1 O7A 147.9(7) . . ?
C31 O1 Hg1 115.2(2) . . ?
C32 O2 Hg1 109.6(2) . . ?
C38 O3 C39 120.7(3) . . ?
C1 N1 C5 119.4(3) . . ?
C1 N1 Hg1 122.1(3) . . ?
C5 N1 Hg1 118.3(3) . . ?
C19 N2 C6 111.2(3) . . ?
C19 N2 C7 111.7(3) . . ?
C6 N2 C7 110.7(3) . . ?
C19 N2 Hg1 108.0(2) . . ?
C6 N2 Hg1 107.4(2) . . ?
C7 N2 Hg1 107.7(2) . . ?
C12 N3 C8 118.8(3) . . ?
C12 N3 Hg1 124.8(2) . . ?
C8 N3 Hg1 109.6(2) . . ?
C20 N4 C24 119.0(3) . . ?
C20 N4 Hg1 114.3(2) . . ?
C24 N4 Hg1 123.3(2) . . ?
N1 C1 C2 122.0(4) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 119.2(5) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C6 117.7(3) . . ?
C4 C5 C6 121.4(4) . . ?
N2 C6 C5 113.3(3) . . ?
N2 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
N2 C7 C8 112.9(3) . . ?
N2 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N3 C8 C9 123.2(4) . . ?
N3 C8 C7 116.8(3) . . ?
C9 C8 C7 119.9(3) . . ?
C8 C9 C10 118.4(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N3 C12 C11 120.7(3) . . ?
N3 C12 C13 119.0(3) . . ?
C11 C12 C13 120.3(3) . . ?
C14 C13 C18 118.7(4) . . ?
C14 C13 C12 120.9(4) . . ?
C18 C13 C12 120.3(3) . . ?
C15 C14 C13 120.5(4) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.0(4) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 120.1(4) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
N2 C19 C20 112.0(3) . . ?
N2 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N2 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
N4 C20 C21 122.9(3) . . ?
N4 C20 C19 116.8(3) . . ?
C21 C20 C19 120.2(3) . . ?
C20 C21 C22 118.6(4) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C23 C22 C21 119.1(4) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 119.8(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
N4 C24 C23 120.5(3) . . ?
N4 C24 C25 117.2(3) . . ?
C23 C24 C25 122.3(3) . . ?
C26 C25 C30 119.6(4) . . ?
C26 C25 C24 120.5(3) . . ?
C30 C25 C24 119.9(4) . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C28 119.3(5) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 119.8(5) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.9(5) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C25 119.9(4) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
O1 C31 C39 121.8(3) . . ?
O1 C31 C32 119.8(3) . . ?
C39 C31 C32 118.4(3) . . ?
O2 C32 C31 121.5(3) . . ?
O2 C32 C33 120.8(3) . . ?
C31 C32 C33 117.8(3) . . ?
C38 C33 C34 118.3(3) . . ?
C38 C33 C32 119.3(3) . . ?
C34 C33 C32 122.4(3) . . ?
C35 C34 C33 120.2(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.3(4) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C37 C36 C35 121.2(4) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 118.1(4) . . ?
C36 C37 H37 120.9 . . ?
C38 C37 H37 120.9 . . ?
O3 C38 C33 121.5(3) . . ?
O3 C38 C37 116.7(3) . . ?
C33 C38 C37 121.8(4) . . ?
O3 C39 C31 122.3(3) . . ?
O3 C39 C40 110.4(3) . . ?
C31 C39 C40 127.2(3) . . ?
C45 C40 C41 118.3(4) . . ?
C45 C40 C39 120.1(3) . . ?
C41 C40 C39 121.6(3) . . ?
C42 C41 C40 119.8(4) . . ?
C42 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C41 C42 C43 120.4(5) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C44 C43 C42 120.0(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.1(4) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C40 121.3(4) . . ?
C44 C45 H45 119.3 . . ?
C40 C45 H45 119.3 . . ?
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
Hg1 O1 2.194(2) . ?
Hg1 N1 2.324(3) . ?
Hg1 O2 2.408(2) . ?
Hg1 N2 2.470(3) . ?
Hg1 N4 2.494(3) . ?
Hg1 N3 2.563(3) . ?
Cl1 O5A 1.325(10) . ?
Cl1 O7 1.343(8) . ?
Cl1 O5 1.384(8) . ?
Cl1 O4 1.416(3) . ?
Cl1 O6A 1.449(10) . ?
Cl1 O6 1.453(8) . ?
Cl1 O7A 1.481(11) . ?
O1 C31 1.317(4) . ?
O2 C32 1.248(4) . ?
O3 C38 1.354(4) . ?
O3 C39 1.377(4) . ?
N1 C1 1.343(5) . ?
N1 C5 1.346(5) . ?
N2 C19 1.466(5) . ?
N2 C6 1.469(5) . ?
N2 C7 1.485(4) . ?
N3 C12 1.351(5) . ?
N3 C8 1.352(5) . ?
N4 C20 1.335(5) . ?
N4 C24 1.361(4) . ?
C1 C2 1.373(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.382(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.510(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.506(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.369(5) . ?
C9 C10 1.387(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.400(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.476(5) . ?
C13 C14 1.395(5) . ?
C13 C18 1.395(5) . ?
C14 C15 1.381(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.520(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.375(5) . ?
C21 C22 1.384(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.478(5) . ?
C25 C26 1.381(5) . ?
C25 C30 1.390(5) . ?
C26 C27 1.391(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C39 1.383(5) . ?
C31 C32 1.449(5) . ?
C32 C33 1.451(5) . ?
C33 C38 1.391(5) . ?
C33 C34 1.405(5) . ?
C34 C35 1.368(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.396(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.369(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.400(5) . ?
C37 H37 0.9500 . ?
C39 C40 1.459(5) . ?
C40 C45 1.392(5) . ?
C40 C41 1.409(5) . ?
C41 C42 1.385(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.395(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.369(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
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
N1 Hg1 O1 C31 -0.8(4) . . . . ?
O2 Hg1 O1 C31 6.6(2) . . . . ?
N2 Hg1 O1 C31 -171.6(2) . . . . ?
N4 Hg1 O1 C31 -113.4(2) . . . . ?
N3 Hg1 O1 C31 123.5(2) . . . . ?
O1 Hg1 O2 C32 -6.9(2) . . . . ?
N1 Hg1 O2 C32 170.0(2) . . . . ?
N2 Hg1 O2 C32 170.1(2) . . . . ?
N4 Hg1 O2 C32 75.8(2) . . . . ?
N3 Hg1 O2 C32 -89.1(2) . . . . ?
O1 Hg1 N1 C1 17.4(5) . . . . ?
O2 Hg1 N1 C1 10.3(3) . . . . ?
N2 Hg1 N1 C1 -169.7(3) . . . . ?
N4 Hg1 N1 C1 128.8(3) . . . . ?
N3 Hg1 N1 C1 -104.6(3) . . . . ?
O1 Hg1 N1 C5 -157.9(2) . . . . ?
O2 Hg1 N1 C5 -165.0(3) . . . . ?
N2 Hg1 N1 C5 15.0(3) . . . . ?
N4 Hg1 N1 C5 -46.5(3) . . . . ?
N3 Hg1 N1 C5 80.1(3) . . . . ?
O1 Hg1 N2 C19 28.4(3) . . . . ?
N1 Hg1 N2 C19 -147.5(2) . . . . ?
O2 Hg1 N2 C19 -147.6(2) . . . . ?
N4 Hg1 N2 C19 -39.9(2) . . . . ?
N3 Hg1 N2 C19 100.9(2) . . . . ?
O1 Hg1 N2 C6 148.4(2) . . . . ?
N1 Hg1 N2 C6 -27.5(2) . . . . ?
O2 Hg1 N2 C6 -27.6(3) . . . . ?
N4 Hg1 N2 C6 80.1(2) . . . . ?
N3 Hg1 N2 C6 -139.1(2) . . . . ?
O1 Hg1 N2 C7 -92.4(2) . . . . ?
N1 Hg1 N2 C7 91.7(2) . . . . ?
O2 Hg1 N2 C7 91.6(3) . . . . ?
N4 Hg1 N2 C7 -160.6(3) . . . . ?
N3 Hg1 N2 C7 -19.9(2) . . . . ?
O1 Hg1 N3 C12 -20.3(3) . . . . ?
N1 Hg1 N3 C12 138.9(3) . . . . ?
O2 Hg1 N3 C12 51.4(3) . . . . ?
N2 Hg1 N3 C12 -156.5(3) . . . . ?
N4 Hg1 N3 C12 -112.8(3) . . . . ?
O1 Hg1 N3 C8 130.2(2) . . . . ?
N1 Hg1 N3 C8 -70.7(2) . . . . ?
O2 Hg1 N3 C8 -158.2(2) . . . . ?
N2 Hg1 N3 C8 -6.0(2) . . . . ?
N4 Hg1 N3 C8 37.7(3) . . . . ?
O1 Hg1 N4 C20 -104.9(2) . . . . ?
N1 Hg1 N4 C20 98.1(3) . . . . ?
O2 Hg1 N4 C20 -176.8(2) . . . . ?
N2 Hg1 N4 C20 32.7(2) . . . . ?
N3 Hg1 N4 C20 -13.1(3) . . . . ?
O1 Hg1 N4 C24 54.0(3) . . . . ?
N1 Hg1 N4 C24 -103.0(3) . . . . ?
O2 Hg1 N4 C24 -17.9(3) . . . . ?
N2 Hg1 N4 C24 -168.4(3) . . . . ?
N3 Hg1 N4 C24 145.8(3) . . . . ?
C5 N1 C1 C2 0.7(6) . . . . ?
Hg1 N1 C1 C2 -174.6(3) . . . . ?
N1 C1 C2 C3 -1.6(7) . . . . ?
C1 C2 C3 C4 0.4(7) . . . . ?
C2 C3 C4 C5 1.6(7) . . . . ?
C1 N1 C5 C4 1.4(6) . . . . ?
Hg1 N1 C5 C4 176.8(3) . . . . ?
C1 N1 C5 C6 -174.7(3) . . . . ?
Hg1 N1 C5 C6 0.7(4) . . . . ?
C3 C4 C5 N1 -2.5(6) . . . . ?
C3 C4 C5 C6 173.4(4) . . . . ?
C19 N2 C6 C5 155.9(3) . . . . ?
C7 N2 C6 C5 -79.3(4) . . . . ?
Hg1 N2 C6 C5 37.9(4) . . . . ?
N1 C5 C6 N2 -28.2(5) . . . . ?
C4 C5 C6 N2 155.8(4) . . . . ?
C19 N2 C7 C8 -74.3(4) . . . . ?
C6 N2 C7 C8 161.2(3) . . . . ?
Hg1 N2 C7 C8 44.1(4) . . . . ?
C12 N3 C8 C9 1.8(5) . . . . ?
Hg1 N3 C8 C9 -150.7(3) . . . . ?
C12 N3 C8 C7 -174.9(3) . . . . ?
Hg1 N3 C8 C7 32.7(3) . . . . ?
N2 C7 C8 N3 -55.4(4) . . . . ?
N2 C7 C8 C9 127.9(4) . . . . ?
N3 C8 C9 C10 -1.5(6) . . . . ?
C7 C8 C9 C10 175.0(3) . . . . ?
C8 C9 C10 C11 0.7(6) . . . . ?
C9 C10 C11 C12 -0.3(5) . . . . ?
C8 N3 C12 C11 -1.3(5) . . . . ?
Hg1 N3 C12 C11 146.7(3) . . . . ?
C8 N3 C12 C13 176.2(3) . . . . ?
Hg1 N3 C12 C13 -35.8(4) . . . . ?
C10 C11 C12 N3 0.6(5) . . . . ?
C10 C11 C12 C13 -176.8(3) . . . . ?
N3 C12 C13 C14 152.8(4) . . . . ?
C11 C12 C13 C14 -29.8(5) . . . . ?
N3 C12 C13 C18 -30.4(5) . . . . ?
C11 C12 C13 C18 147.1(4) . . . . ?
C18 C13 C14 C15 0.8(6) . . . . ?
C12 C13 C14 C15 177.7(4) . . . . ?
C13 C14 C15 C16 -0.6(7) . . . . ?
C14 C15 C16 C17 0.4(7) . . . . ?
C15 C16 C17 C18 -0.5(6) . . . . ?
C16 C17 C18 C13 0.7(6) . . . . ?
C14 C13 C18 C17 -0.8(5) . . . . ?
C12 C13 C18 C17 -177.8(3) . . . . ?
C6 N2 C19 C20 -71.6(4) . . . . ?
C7 N2 C19 C20 164.2(3) . . . . ?
Hg1 N2 C19 C20 46.0(3) . . . . ?
C24 N4 C20 C21 -1.1(5) . . . . ?
Hg1 N4 C20 C21 158.7(3) . . . . ?
C24 N4 C20 C19 -179.6(3) . . . . ?
Hg1 N4 C20 C19 -19.7(4) . . . . ?
N2 C19 C20 N4 -18.2(5) . . . . ?
N2 C19 C20 C21 163.3(3) . . . . ?
N4 C20 C21 C22 1.1(6) . . . . ?
C19 C20 C21 C22 179.5(4) . . . . ?
C20 C21 C22 C23 -0.2(6) . . . . ?
C21 C22 C23 C24 -0.7(6) . . . . ?
C20 N4 C24 C23 0.2(5) . . . . ?
Hg1 N4 C24 C23 -157.7(3) . . . . ?
C20 N4 C24 C25 -178.1(3) . . . . ?
Hg1 N4 C24 C25 24.0(4) . . . . ?
C22 C23 C24 N4 0.6(6) . . . . ?
C22 C23 C24 C25 178.9(4) . . . . ?
N4 C24 C25 C26 44.3(5) . . . . ?
C23 C24 C25 C26 -134.0(4) . . . . ?
N4 C24 C25 C30 -134.5(4) . . . . ?
C23 C24 C25 C30 47.2(5) . . . . ?
C30 C25 C26 C27 -2.5(6) . . . . ?
C24 C25 C26 C27 178.7(4) . . . . ?
C25 C26 C27 C28 2.1(6) . . . . ?
C26 C27 C28 C29 0.1(7) . . . . ?
C27 C28 C29 C30 -1.9(7) . . . . ?
C28 C29 C30 C25 1.5(7) . . . . ?
C26 C25 C30 C29 0.7(6) . . . . ?
C24 C25 C30 C29 179.5(4) . . . . ?
Hg1 O1 C31 C39 171.6(3) . . . . ?
Hg1 O1 C31 C32 -6.0(4) . . . . ?
Hg1 O2 C32 C31 6.5(4) . . . . ?
Hg1 O2 C32 C33 -172.4(2) . . . . ?
O1 C31 C32 O2 -1.0(5) . . . . ?
C39 C31 C32 O2 -178.6(3) . . . . ?
O1 C31 C32 C33 178.0(3) . . . . ?
C39 C31 C32 C33 0.3(5) . . . . ?
O2 C32 C33 C38 179.9(3) . . . . ?
C31 C32 C33 C38 0.9(5) . . . . ?
O2 C32 C33 C34 0.7(5) . . . . ?
C31 C32 C33 C34 -178.2(3) . . . . ?
C38 C33 C34 C35 0.4(5) . . . . ?
C32 C33 C34 C35 179.5(3) . . . . ?
C33 C34 C35 C36 1.8(6) . . . . ?
C34 C35 C36 C37 -2.1(6) . . . . ?
C35 C36 C37 C38 0.2(6) . . . . ?
C39 O3 C38 C33 0.1(5) . . . . ?
C39 O3 C38 C37 -179.5(3) . . . . ?
C34 C33 C38 O3 178.0(3) . . . . ?
C32 C33 C38 O3 -1.1(5) . . . . ?
C34 C33 C38 C37 -2.4(5) . . . . ?
C32 C33 C38 C37 178.5(3) . . . . ?
C36 C37 C38 O3 -178.3(3) . . . . ?
C36 C37 C38 C33 2.1(6) . . . . ?
C38 O3 C39 C31 1.2(5) . . . . ?
C38 O3 C39 C40 -176.9(3) . . . . ?
O1 C31 C39 O3 -179.0(3) . . . . ?
C32 C31 C39 O3 -1.4(5) . . . . ?
O1 C31 C39 C40 -1.2(6) . . . . ?
C32 C31 C39 C40 176.4(3) . . . . ?
O3 C39 C40 C45 42.5(5) . . . . ?
C31 C39 C40 C45 -135.5(4) . . . . ?
O3 C39 C40 C41 -136.5(3) . . . . ?
C31 C39 C40 C41 45.6(5) . . . . ?
C45 C40 C41 C42 1.0(6) . . . . ?
C39 C40 C41 C42 -180.0(4) . . . . ?
C40 C41 C42 C43 -0.5(6) . . . . ?
C41 C42 C43 C44 0.9(7) . . . . ?
C42 C43 C44 C45 -1.9(7) . . . . ?
C43 C44 C45 C40 2.4(7) . . . . ?
C41 C40 C45 C44 -2.0(6) . . . . ?
C39 C40 C45 C44 179.0(4) . . . . ?
|
1501473.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501473.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_1501473
loop_
_publ_author_name
'Katarzyna Grubel'
'Brynna J. Laughlin'
'Thora R. Maltais'
'Rhett C. Smith'
'Atta M. Arif'
'Lisa M. Berreau'
_publ_section_title
;
Photochemically-induced dioxygenase-type CO-release reactivity of Group
12 metal flavonolate complexes
;
_journal_issue 37
_journal_name_full 'Chemical Communications'
_journal_page_first 10431
_journal_page_last 10433
_journal_paper_doi 10.1039/c1cc13961d
_journal_volume 47
_journal_year 2011
_chemical_formula_moiety 'C44 H35 N4 O4 Zn, C F3 S O3'
_chemical_formula_sum 'C45 H35 F3 N4 O7 S Zn'
_chemical_formula_weight 898.20
_chemical_name_systematic
;
?
;
_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 91.0370(14)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.1785(2)
_cell_length_b 16.3337(5)
_cell_length_c 24.1620(5)
_cell_measurement_reflns_used 8374
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 1.018
_cell_volume 4016.34(17)
_computing_cell_refinement DENZO-SMN
_computing_data_collection 'Nonius COLLECT'
_computing_data_reduction DENZO-SMN
_computing_molecular_graphics 'WinGX, Ortep3'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution SIR97
_diffrn_ambient_temperature 150(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method 'Phi and Omega 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 0.0342
_diffrn_reflns_av_sigmaI/netI 0.0668
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 15119
_diffrn_reflns_theta_full 27.46
_diffrn_reflns_theta_max 27.46
_diffrn_reflns_theta_min 2.00
_exptl_absorpt_coefficient_mu 0.736
_exptl_absorpt_correction_T_max 0.9104
_exptl_absorpt_correction_T_min 0.8374
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.485
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1848
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.332
_refine_diff_density_min -0.482
_refine_diff_density_rms 0.065
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 690
_refine_ls_number_reflns 9139
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.016
_refine_ls_R_factor_all 0.0829
_refine_ls_R_factor_gt 0.0432
_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^+0.9142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0883
_refine_ls_wR_factor_ref 0.1034
_reflns_number_gt 6218
_reflns_number_total 9139
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1cc13961d.txt
_cod_data_source_block usu197
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501473
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
Zn1 Zn 0.30765(2) 0.152538(18) 0.306785(10) 0.02407(9) Uani 1 1 d . . .
F1 F 0.5992(3) 0.44648(14) 0.46946(8) 0.0988(9) Uani 1 1 d . . .
F2 F 0.7971(3) 0.44170(18) 0.50042(11) 0.1168(10) Uani 1 1 d . . .
F3 F 0.6373(2) 0.44078(12) 0.55734(7) 0.0695(6) Uani 1 1 d . . .
S1 S 0.67409(7) 0.30275(5) 0.50450(3) 0.04009(18) Uani 1 1 d . . .
O1 O 0.15704(15) 0.11021(11) 0.26570(7) 0.0302(4) Uani 1 1 d . . .
O2 O 0.10100(16) 0.03002(12) 0.33625(7) 0.0365(4) Uani 1 1 d . . .
O3 O -0.15889(17) -0.02471(11) 0.33141(7) 0.0348(4) Uani 1 1 d . . .
O4 O -0.15856(17) 0.10830(12) 0.35585(8) 0.0391(5) Uani 1 1 d . . .
O5 O 0.71438(18) 0.28612(13) 0.44895(7) 0.0404(5) Uani 1 1 d . . .
O6 O 0.7614(3) 0.27882(18) 0.54763(9) 0.0799(9) Uani 1 1 d . . .
O7 O 0.5378(2) 0.28456(17) 0.51441(9) 0.0662(7) Uani 1 1 d . . .
N1 N 0.21097(19) 0.23490(13) 0.35997(8) 0.0301(5) Uani 1 1 d . . .
N2 N 0.47025(18) 0.20329(12) 0.35658(8) 0.0255(4) Uani 1 1 d . . .
N3 N 0.41182(18) 0.04690(13) 0.33810(8) 0.0264(5) Uani 1 1 d . . .
N4 N 0.42926(19) 0.20261(12) 0.24432(8) 0.0258(4) Uani 1 1 d . . .
C1 C 0.0822(3) 0.23349(18) 0.37114(11) 0.0350(6) Uani 1 1 d . . .
C2 C 0.0276(3) 0.2842(2) 0.41047(12) 0.0424(7) Uani 1 1 d . . .
C3 C 0.1079(3) 0.3376(2) 0.43932(12) 0.0468(8) Uani 1 1 d . . .
C4 C 0.2409(3) 0.33907(18) 0.42805(11) 0.0401(7) Uani 1 1 d . . .
C5 C 0.2890(2) 0.28748(16) 0.38803(10) 0.0307(6) Uani 1 1 d . . .
C6 C 0.4312(3) 0.28733(17) 0.37184(11) 0.0318(6) Uani 1 1 d . . .
C7 C 0.4847(3) 0.14959(17) 0.40494(10) 0.0292(6) Uani 1 1 d . . .
C8 C 0.4698(2) 0.06127(16) 0.38799(10) 0.0272(5) Uani 1 1 d . . .
C9 C 0.5110(2) -0.00171(18) 0.42256(11) 0.0344(6) Uani 1 1 d . . .
C10 C 0.4885(3) -0.0812(2) 0.40671(13) 0.0429(7) Uani 1 1 d . . .
C11 C 0.4308(3) -0.09652(18) 0.35565(13) 0.0409(7) Uani 1 1 d . . .
C12 C 0.3957(2) -0.03151(16) 0.32152(10) 0.0300(6) Uani 1 1 d . . .
C13 C 0.3448(2) -0.04670(16) 0.26443(10) 0.0306(6) Uani 1 1 d . . .
C14 C 0.3960(3) -0.00507(17) 0.21965(11) 0.0348(6) Uani 1 1 d . . .
C15 C 0.3495(3) -0.02127(19) 0.16632(12) 0.0406(7) Uani 1 1 d . . .
C16 C 0.2517(3) -0.07846(19) 0.15757(13) 0.0432(7) Uani 1 1 d . . .
C17 C 0.2009(3) -0.1198(2) 0.20162(13) 0.0421(7) Uani 1 1 d . . .
C18 C 0.2474(3) -0.10510(18) 0.25500(12) 0.0362(6) Uani 1 1 d . . .
C19 C 0.5877(2) 0.20150(19) 0.32195(11) 0.0316(6) Uani 1 1 d . . .
C20 C 0.5566(2) 0.19781(15) 0.26091(10) 0.0276(5) Uani 1 1 d . . .
C21 C 0.6573(3) 0.18864(17) 0.22371(11) 0.0335(6) Uani 1 1 d . . .
C22 C 0.6272(3) 0.18449(17) 0.16803(12) 0.0370(6) Uani 1 1 d . . .
C23 C 0.4975(3) 0.19364(16) 0.15039(11) 0.0334(6) Uani 1 1 d . . .
C24 C 0.3995(2) 0.20350(15) 0.18884(9) 0.0273(5) Uani 1 1 d . . .
C25 C 0.2620(2) 0.22010(15) 0.17196(10) 0.0286(6) Uani 1 1 d . . .
C26 C 0.1836(3) 0.27105(17) 0.20366(10) 0.0328(6) Uani 1 1 d . . .
C27 C 0.0562(3) 0.2900(2) 0.18690(12) 0.0402(7) Uani 1 1 d . . .
C28 C 0.0051(3) 0.2582(2) 0.13828(12) 0.0452(8) Uani 1 1 d . . .
C29 C 0.0802(3) 0.2079(2) 0.10635(12) 0.0477(8) Uani 1 1 d . . .
C30 C 0.2087(3) 0.18902(19) 0.12251(11) 0.0400(7) Uani 1 1 d . . .
C31 C 0.0824(2) 0.05822(16) 0.28961(9) 0.0282(6) Uani 1 1 d . . .
C32 C -0.0356(2) 0.03211(15) 0.25437(10) 0.0269(5) Uani 1 1 d . . .
C33 C -0.0332(3) 0.04529(17) 0.19746(11) 0.0321(6) Uani 1 1 d . . .
C34 C -0.1362(3) 0.02087(18) 0.16301(11) 0.0361(6) Uani 1 1 d . . .
C35 C -0.2453(3) -0.01525(17) 0.18520(11) 0.0364(6) Uani 1 1 d . . .
C36 C -0.2511(3) -0.02836(17) 0.24129(12) 0.0350(6) Uani 1 1 d . . .
C37 C -0.1465(2) -0.00490(16) 0.27539(10) 0.0292(6) Uani 1 1 d . . .
C38 C -0.1577(2) 0.03710(18) 0.36909(11) 0.0332(6) Uani 1 1 d . . .
C39 C -0.1636(2) 0.00591(19) 0.42652(11) 0.0364(6) Uani 1 1 d . . .
C40 C -0.1702(3) -0.0778(2) 0.43802(12) 0.0413(7) Uani 1 1 d . . .
C41 C -0.1779(3) -0.1036(3) 0.49284(13) 0.0506(8) Uani 1 1 d . . .
C42 C -0.1770(3) -0.0472(3) 0.53490(13) 0.0564(10) Uani 1 1 d . . .
C43 C -0.1708(3) 0.0353(3) 0.52403(13) 0.0546(9) Uani 1 1 d . . .
C44 C -0.1638(3) 0.0628(2) 0.46943(12) 0.0453(8) Uani 1 1 d . . .
C45 C 0.6751(4) 0.4126(2) 0.50795(12) 0.0569(9) Uani 1 1 d . . .
H1 H 0.028(3) 0.1926(17) 0.3516(10) 0.034(7) Uiso 1 1 d . . .
H2 H -0.055(3) 0.2810(19) 0.4154(12) 0.049(9) Uiso 1 1 d . . .
H3 H 0.068(3) 0.3710(19) 0.4665(12) 0.050(9) Uiso 1 1 d . . .
H4 H 0.298(3) 0.3743(17) 0.4464(11) 0.036(7) Uiso 1 1 d . . .
H6A H 0.443(3) 0.3216(17) 0.3365(11) 0.035(7) Uiso 1 1 d . . .
H6B H 0.487(3) 0.3088(17) 0.3999(11) 0.037(7) Uiso 1 1 d . . .
H7A H 0.422(3) 0.1629(16) 0.4308(10) 0.029(7) Uiso 1 1 d . . .
H7B H 0.565(3) 0.1558(16) 0.4247(11) 0.036(7) Uiso 1 1 d . . .
H9 H 0.550(3) 0.0110(17) 0.4538(11) 0.036(8) Uiso 1 1 d . . .
H10 H 0.507(3) -0.1205(18) 0.4291(11) 0.034(8) Uiso 1 1 d . . .
H11 H 0.419(3) -0.153(2) 0.3417(12) 0.051(9) Uiso 1 1 d . . .
H14 H 0.463(3) 0.0323(17) 0.2255(10) 0.032(7) Uiso 1 1 d . . .
H15 H 0.386(3) 0.0051(17) 0.1375(11) 0.032(7) Uiso 1 1 d . . .
H16 H 0.223(3) -0.0908(18) 0.1227(11) 0.041(8) Uiso 1 1 d . . .
H17 H 0.140(3) -0.1603(19) 0.1968(12) 0.053(9) Uiso 1 1 d . . .
H18 H 0.213(3) -0.1332(16) 0.2832(10) 0.028(7) Uiso 1 1 d . . .
H19A H 0.647(3) 0.2501(19) 0.3300(11) 0.046(8) Uiso 1 1 d . . .
H19B H 0.636(2) 0.1562(16) 0.3309(10) 0.026(7) Uiso 1 1 d . . .
H21 H 0.743(3) 0.1845(16) 0.2376(10) 0.033(7) Uiso 1 1 d . . .
H22 H 0.695(3) 0.1765(17) 0.1392(11) 0.038(7) Uiso 1 1 d . . .
H23 H 0.474(3) 0.1978(18) 0.1120(12) 0.045(8) Uiso 1 1 d . . .
H26 H 0.216(2) 0.2935(15) 0.2365(10) 0.025(6) Uiso 1 1 d . . .
H27 H 0.010(3) 0.3261(18) 0.2085(12) 0.041(8) Uiso 1 1 d . . .
H28 H -0.080(3) 0.274(2) 0.1252(12) 0.057(9) Uiso 1 1 d . . .
H29 H 0.054(3) 0.1808(18) 0.0723(12) 0.048(8) Uiso 1 1 d . . .
H30 H 0.259(3) 0.1519(17) 0.1031(11) 0.035(8) Uiso 1 1 d . . .
H33 H 0.040(3) 0.0689(17) 0.1825(11) 0.037(8) Uiso 1 1 d . . .
H34 H -0.130(2) 0.0299(16) 0.1254(11) 0.031(7) Uiso 1 1 d . . .
H35 H -0.320(3) -0.0303(18) 0.1631(12) 0.050(8) Uiso 1 1 d . . .
H36 H -0.324(3) -0.0496(18) 0.2571(11) 0.046(8) Uiso 1 1 d . . .
H40 H -0.177(3) -0.121(2) 0.4062(13) 0.059(9) Uiso 1 1 d . . .
H41 H -0.182(3) -0.159(2) 0.4995(13) 0.054(10) Uiso 1 1 d . . .
H42 H -0.178(3) -0.0679(19) 0.5748(13) 0.058(9) Uiso 1 1 d . . .
H43 H -0.172(3) 0.0777(17) 0.5528(11) 0.037(7) Uiso 1 1 d . . .
H44 H -0.161(3) 0.120(2) 0.4578(11) 0.043(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
Zn1 0.01950(13) 0.02859(17) 0.02407(14) -0.00114(12) -0.00114(10) -0.00114(12)
F1 0.180(3) 0.0737(16) 0.0426(11) 0.0030(10) 0.0025(14) 0.0607(17)
F2 0.134(2) 0.104(2) 0.113(2) -0.0383(16) 0.0362(18) -0.0684(19)
F3 0.1076(17) 0.0611(13) 0.0397(10) -0.0189(9) -0.0024(10) 0.0149(12)
S1 0.0421(4) 0.0518(5) 0.0263(3) -0.0062(3) -0.0025(3) 0.0066(3)
O1 0.0241(9) 0.0340(10) 0.0322(9) 0.0014(8) -0.0035(7) -0.0051(8)
O2 0.0269(9) 0.0536(13) 0.0289(9) 0.0050(9) -0.0022(7) 0.0030(9)
O3 0.0357(10) 0.0362(11) 0.0326(9) 0.0005(8) 0.0020(8) -0.0041(8)
O4 0.0312(10) 0.0363(12) 0.0499(11) -0.0018(9) 0.0012(8) 0.0055(9)
O5 0.0338(10) 0.0562(13) 0.0313(9) -0.0097(9) 0.0048(8) 0.0013(9)
O6 0.0958(19) 0.097(2) 0.0460(13) -0.0126(13) -0.0289(13) 0.0511(17)
O7 0.0552(14) 0.100(2) 0.0441(12) -0.0182(13) 0.0209(10) -0.0244(14)
N1 0.0279(11) 0.0326(13) 0.0296(10) -0.0002(9) -0.0005(9) 0.0032(9)
N2 0.0223(10) 0.0270(12) 0.0271(10) -0.0004(9) -0.0039(8) -0.0022(9)
N3 0.0188(9) 0.0281(12) 0.0323(10) 0.0008(9) -0.0022(8) -0.0006(8)
N4 0.0239(10) 0.0244(12) 0.0293(10) -0.0016(9) 0.0019(8) -0.0032(9)
C1 0.0275(13) 0.0378(17) 0.0399(14) 0.0024(13) 0.0021(12) 0.0051(12)
C2 0.0369(16) 0.0467(19) 0.0438(16) 0.0075(14) 0.0109(13) 0.0108(15)
C3 0.059(2) 0.045(2) 0.0369(15) 0.0005(14) 0.0153(14) 0.0169(16)
C4 0.0535(18) 0.0321(16) 0.0347(14) -0.0076(13) -0.0034(13) 0.0057(14)
C5 0.0340(13) 0.0305(15) 0.0274(12) 0.0023(11) -0.0043(11) 0.0036(11)
C6 0.0307(13) 0.0307(15) 0.0337(14) -0.0043(12) -0.0046(11) -0.0026(11)
C7 0.0264(12) 0.0317(15) 0.0293(12) 0.0004(12) -0.0061(11) -0.0007(12)
C8 0.0168(11) 0.0333(15) 0.0315(12) 0.0007(11) 0.0020(10) -0.0009(10)
C9 0.0264(13) 0.0412(17) 0.0353(14) 0.0071(13) -0.0033(11) -0.0006(12)
C10 0.0376(15) 0.0382(18) 0.0526(18) 0.0171(15) -0.0082(14) 0.0019(14)
C11 0.0380(15) 0.0254(16) 0.0589(18) 0.0024(14) -0.0091(14) 0.0004(12)
C12 0.0206(12) 0.0270(14) 0.0424(14) -0.0005(12) -0.0028(10) 0.0005(10)
C13 0.0252(12) 0.0269(14) 0.0395(14) -0.0066(11) -0.0024(11) 0.0045(11)
C14 0.0293(14) 0.0301(15) 0.0451(16) -0.0094(13) 0.0017(12) 0.0003(12)
C15 0.0444(17) 0.0380(18) 0.0397(16) -0.0071(14) 0.0095(13) 0.0028(14)
C16 0.0429(16) 0.0450(19) 0.0416(16) -0.0160(14) -0.0034(13) 0.0036(14)
C17 0.0342(15) 0.0379(17) 0.0539(18) -0.0162(15) -0.0057(13) -0.0023(14)
C18 0.0293(14) 0.0317(17) 0.0476(16) -0.0060(13) -0.0002(13) 0.0001(12)
C19 0.0206(12) 0.0356(17) 0.0385(14) 0.0007(13) -0.0015(11) -0.0028(12)
C20 0.0249(12) 0.0208(13) 0.0372(13) -0.0005(11) 0.0039(10) -0.0022(10)
C21 0.0269(13) 0.0272(15) 0.0466(16) -0.0005(12) 0.0067(12) 0.0006(11)
C22 0.0403(15) 0.0289(15) 0.0424(15) -0.0013(12) 0.0168(13) 0.0009(13)
C23 0.0413(15) 0.0253(15) 0.0337(14) 0.0006(11) 0.0075(12) -0.0013(12)
C24 0.0339(13) 0.0220(13) 0.0263(12) -0.0006(10) 0.0043(10) -0.0042(11)
C25 0.0334(13) 0.0259(14) 0.0266(12) 0.0023(10) 0.0005(10) -0.0045(11)
C26 0.0345(14) 0.0346(16) 0.0291(13) 0.0019(11) -0.0043(11) -0.0019(12)
C27 0.0345(15) 0.0441(19) 0.0419(16) 0.0044(14) -0.0022(13) 0.0033(14)
C28 0.0384(16) 0.052(2) 0.0451(16) 0.0145(15) -0.0133(14) -0.0076(15)
C29 0.0560(19) 0.053(2) 0.0335(15) 0.0043(14) -0.0166(14) -0.0122(16)
C30 0.0525(18) 0.0395(17) 0.0278(13) -0.0019(12) -0.0011(13) -0.0005(15)
C31 0.0224(12) 0.0365(16) 0.0258(12) -0.0034(11) 0.0006(10) 0.0051(11)
C32 0.0233(12) 0.0249(14) 0.0323(12) 0.0007(11) -0.0025(10) 0.0011(10)
C33 0.0296(14) 0.0348(16) 0.0319(13) -0.0014(12) -0.0001(11) -0.0006(12)
C34 0.0362(15) 0.0420(17) 0.0299(14) -0.0061(12) -0.0070(12) -0.0018(13)
C35 0.0314(14) 0.0364(17) 0.0412(15) -0.0065(13) -0.0080(12) -0.0011(12)
C36 0.0265(13) 0.0299(16) 0.0484(16) 0.0005(13) -0.0016(12) -0.0064(12)
C37 0.0295(13) 0.0292(14) 0.0289(12) 0.0028(11) 0.0013(10) -0.0004(11)
C38 0.0181(12) 0.0383(17) 0.0431(15) -0.0033(13) 0.0007(11) 0.0019(11)
C39 0.0206(12) 0.0537(19) 0.0352(14) -0.0029(13) 0.0038(10) -0.0015(12)
C40 0.0316(14) 0.054(2) 0.0386(15) 0.0057(14) 0.0026(12) 0.0033(14)
C41 0.0416(17) 0.068(3) 0.0423(17) 0.0165(17) 0.0029(13) 0.0018(17)
C42 0.0363(17) 0.100(3) 0.0325(16) 0.0066(18) 0.0027(13) -0.0059(18)
C43 0.0340(16) 0.091(3) 0.0389(17) -0.0156(19) 0.0051(13) -0.0091(17)
C44 0.0286(14) 0.063(2) 0.0441(17) -0.0071(16) 0.0046(12) -0.0037(14)
C45 0.077(2) 0.058(2) 0.0363(16) -0.0103(15) 0.0057(16) -0.0013(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'
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'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 N1 99.53(7) . . ?
O1 Zn1 N4 103.78(7) . . ?
N1 Zn1 N4 117.93(8) . . ?
O1 Zn1 N3 105.88(7) . . ?
N1 Zn1 N3 121.81(8) . . ?
N4 Zn1 N3 105.51(8) . . ?
O1 Zn1 N2 176.79(8) . . ?
N1 Zn1 N2 77.34(7) . . ?
N4 Zn1 N2 78.53(7) . . ?
N3 Zn1 N2 75.42(7) . . ?
O6 S1 O5 116.77(14) . . ?
O6 S1 O7 114.51(17) . . ?
O5 S1 O7 114.05(12) . . ?
O6 S1 C45 103.83(16) . . ?
O5 S1 C45 103.35(14) . . ?
O7 S1 C45 101.71(17) . . ?
C31 O1 Zn1 118.34(14) . . ?
C38 O3 C37 118.4(2) . . ?
C1 N1 C5 118.6(2) . . ?
C1 N1 Zn1 125.27(19) . . ?
C5 N1 Zn1 115.81(17) . . ?
C7 N2 C19 111.8(2) . . ?
C7 N2 C6 112.4(2) . . ?
C19 N2 C6 112.6(2) . . ?
C7 N2 Zn1 105.95(14) . . ?
C19 N2 Zn1 107.06(14) . . ?
C6 N2 Zn1 106.54(14) . . ?
C12 N3 C8 118.5(2) . . ?
C12 N3 Zn1 126.75(15) . . ?
C8 N3 Zn1 112.20(16) . . ?
C20 N4 C24 119.0(2) . . ?
C20 N4 Zn1 109.49(15) . . ?
C24 N4 Zn1 125.18(15) . . ?
N1 C1 C2 122.2(3) . . ?
N1 C1 H1 117.3(16) . . ?
C2 C1 H1 120.5(16) . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2 123(2) . . ?
C1 C2 H2 118(2) . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 117.4(18) . . ?
C4 C3 H3 123.7(19) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 119.4(17) . . ?
C3 C4 H4 121.4(17) . . ?
N1 C5 C4 122.0(3) . . ?
N1 C5 C6 115.4(2) . . ?
C4 C5 C6 122.6(2) . . ?
N2 C6 C5 109.3(2) . . ?
N2 C6 H6A 105.3(15) . . ?
C5 C6 H6A 109.7(15) . . ?
N2 C6 H6B 111.4(17) . . ?
C5 C6 H6B 112.2(17) . . ?
H6A C6 H6B 109(2) . . ?
N2 C7 C8 110.38(19) . . ?
N2 C7 H7A 109.7(16) . . ?
C8 C7 H7A 110.0(16) . . ?
N2 C7 H7B 114.2(16) . . ?
C8 C7 H7B 108.8(16) . . ?
H7A C7 H7B 104(2) . . ?
N3 C8 C9 122.1(2) . . ?
N3 C8 C7 116.6(2) . . ?
C9 C8 C7 121.3(2) . . ?
C10 C9 C8 119.2(2) . . ?
C10 C9 H9 122.5(19) . . ?
C8 C9 H9 118.3(19) . . ?
C9 C10 C11 119.2(3) . . ?
C9 C10 H10 119.9(18) . . ?
C11 C10 H10 120.9(18) . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 121.4(17) . . ?
C12 C11 H11 118.9(17) . . ?
N3 C12 C11 121.4(2) . . ?
N3 C12 C13 118.2(2) . . ?
C11 C12 C13 120.4(2) . . ?
C14 C13 C18 119.0(2) . . ?
C14 C13 C12 120.8(2) . . ?
C18 C13 C12 120.1(2) . . ?
C13 C14 C15 120.2(3) . . ?
C13 C14 H14 119.4(16) . . ?
C15 C14 H14 120.3(16) . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 120.6(17) . . ?
C14 C15 H15 119.1(17) . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16 119.5(18) . . ?
C15 C16 H16 120.7(18) . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 H17 121.5(19) . . ?
C18 C17 H17 117.6(19) . . ?
C17 C18 C13 120.1(3) . . ?
C17 C18 H18 119.0(16) . . ?
C13 C18 H18 121.0(16) . . ?
N2 C19 C20 113.58(19) . . ?
N2 C19 H19A 111.1(17) . . ?
C20 C19 H19A 109.5(16) . . ?
N2 C19 H19B 108.8(16) . . ?
C20 C19 H19B 107.7(15) . . ?
H19A C19 H19B 106(2) . . ?
N4 C20 C21 122.1(2) . . ?
N4 C20 C19 118.1(2) . . ?
C21 C20 C19 119.8(2) . . ?
C22 C21 C20 119.1(2) . . ?
C22 C21 H21 122.5(16) . . ?
C20 C21 H21 118.4(16) . . ?
C21 C22 C23 119.2(3) . . ?
C21 C22 H22 123.2(15) . . ?
C23 C22 H22 117.6(15) . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 118.1(17) . . ?
C22 C23 H23 121.7(17) . . ?
N4 C24 C23 120.4(2) . . ?
N4 C24 C25 117.7(2) . . ?
C23 C24 C25 121.8(2) . . ?
C26 C25 C30 118.0(2) . . ?
C26 C25 C24 120.5(2) . . ?
C30 C25 C24 121.4(2) . . ?
C27 C26 C25 121.0(2) . . ?
C27 C26 H26 118.5(15) . . ?
C25 C26 H26 120.5(15) . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27 122.4(17) . . ?
C26 C27 H27 117.5(17) . . ?
C29 C28 C27 120.0(3) . . ?
C29 C28 H28 119.4(19) . . ?
C27 C28 H28 120.4(19) . . ?
C28 C29 C30 120.4(3) . . ?
C28 C29 H29 127.0(18) . . ?
C30 C29 H29 112.6(18) . . ?
C29 C30 C25 120.4(3) . . ?
C29 C30 H30 121.8(16) . . ?
C25 C30 H30 117.5(16) . . ?
O2 C31 O1 125.3(2) . . ?
O2 C31 C32 121.0(2) . . ?
O1 C31 C32 113.7(2) . . ?
C37 C32 C33 117.3(2) . . ?
C37 C32 C31 123.9(2) . . ?
C33 C32 C31 118.8(2) . . ?
C34 C33 C32 121.5(3) . . ?
C34 C33 H33 119.7(16) . . ?
C32 C33 H33 118.8(16) . . ?
C35 C34 C33 119.8(3) . . ?
C35 C34 H34 121.5(16) . . ?
C33 C34 H34 118.7(16) . . ?
C34 C35 C36 120.1(2) . . ?
C34 C35 H35 122.1(18) . . ?
C36 C35 H35 117.8(18) . . ?
C35 C36 C37 119.7(3) . . ?
C35 C36 H36 121.6(17) . . ?
C37 C36 H36 118.6(18) . . ?
C32 C37 C36 121.6(2) . . ?
C32 C37 O3 122.9(2) . . ?
C36 C37 O3 115.4(2) . . ?
O4 C38 O3 122.6(2) . . ?
O4 C38 C39 125.5(3) . . ?
O3 C38 C39 111.8(2) . . ?
C44 C39 C40 120.3(3) . . ?
C44 C39 C38 118.0(3) . . ?
C40 C39 C38 121.7(3) . . ?
C41 C40 C39 119.3(3) . . ?
C41 C40 H40 119.6(18) . . ?
C39 C40 H40 121.0(18) . . ?
C42 C41 C40 120.1(4) . . ?
C42 C41 H41 122(2) . . ?
C40 C41 H41 118(2) . . ?
C41 C42 C43 121.1(3) . . ?
C41 C42 H42 118.5(18) . . ?
C43 C42 H42 120.4(18) . . ?
C42 C43 C44 119.9(3) . . ?
C42 C43 H43 123.6(16) . . ?
C44 C43 H43 116.5(17) . . ?
C39 C44 C43 119.4(4) . . ?
C39 C44 H44 115.2(17) . . ?
C43 C44 H44 125.4(17) . . ?
F1 C45 F3 108.0(3) . . ?
F1 C45 F2 106.7(3) . . ?
F3 C45 F2 106.2(3) . . ?
F1 C45 S1 112.5(2) . . ?
F3 C45 S1 112.5(2) . . ?
F2 C45 S1 110.6(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
Zn1 O1 1.9387(15) . ?
Zn1 N1 2.115(2) . ?
Zn1 N4 2.132(2) . ?
Zn1 N3 2.155(2) . ?
Zn1 N2 2.1913(18) . ?
F1 C45 1.320(4) . ?
F2 C45 1.345(4) . ?
F3 C45 1.342(3) . ?
S1 O6 1.413(2) . ?
S1 O5 1.4366(18) . ?
S1 O7 1.442(2) . ?
S1 C45 1.797(4) . ?
O1 C31 1.284(3) . ?
O2 C31 1.229(3) . ?
O3 C38 1.359(3) . ?
O3 C37 1.400(3) . ?
O4 C38 1.206(3) . ?
N1 C1 1.343(3) . ?
N1 C5 1.345(3) . ?
N2 C7 1.466(3) . ?
N2 C19 1.472(3) . ?
N2 C6 1.478(3) . ?
N3 C12 1.351(3) . ?
N3 C8 1.353(3) . ?
N4 C20 1.352(3) . ?
N4 C24 1.369(3) . ?
C1 C2 1.384(4) . ?
C1 H1 0.98(3) . ?
C2 C3 1.376(5) . ?
C2 H2 0.86(3) . ?
C3 C4 1.386(4) . ?
C3 H3 0.95(3) . ?
C4 C5 1.379(4) . ?
C4 H4 0.92(3) . ?
C5 C6 1.506(4) . ?
C6 H6A 1.03(3) . ?
C6 H6B 0.94(3) . ?
C7 C8 1.506(4) . ?
C7 H7A 0.93(3) . ?
C7 H7B 0.95(3) . ?
C8 C9 1.385(4) . ?
C9 C10 1.371(4) . ?
C9 H9 0.87(3) . ?
C10 C11 1.380(4) . ?
C10 H10 0.86(3) . ?
C11 C12 1.387(4) . ?
C11 H11 0.99(3) . ?
C12 C13 1.485(3) . ?
C13 C14 1.387(4) . ?
C13 C18 1.392(4) . ?
C14 C15 1.390(4) . ?
C14 H14 0.93(3) . ?
C15 C16 1.379(4) . ?
C15 H15 0.90(3) . ?
C16 C17 1.369(4) . ?
C16 H16 0.91(3) . ?
C17 C18 1.387(4) . ?
C17 H17 0.91(3) . ?
C18 H18 0.90(3) . ?
C19 C20 1.504(3) . ?
C19 H19A 1.01(3) . ?
C19 H19B 0.91(3) . ?
C20 C21 1.383(4) . ?
C21 C22 1.376(4) . ?
C21 H21 0.94(3) . ?
C22 C23 1.388(4) . ?
C22 H22 0.99(3) . ?
C23 C24 1.385(4) . ?
C23 H23 0.96(3) . ?
C24 C25 1.476(3) . ?
C25 C26 1.392(4) . ?
C25 C30 1.399(3) . ?
C26 C27 1.387(4) . ?
C26 H26 0.93(2) . ?
C27 C28 1.377(4) . ?
C27 H27 0.92(3) . ?
C28 C29 1.369(5) . ?
C28 H28 0.95(3) . ?
C29 C30 1.393(4) . ?
C29 H29 0.97(3) . ?
C30 H30 0.93(3) . ?
C31 C32 1.520(3) . ?
C32 C37 1.385(3) . ?
C32 C33 1.393(3) . ?
C33 C34 1.385(3) . ?
C33 H33 0.92(3) . ?
C34 C35 1.375(4) . ?
C34 H34 0.92(2) . ?
C35 C36 1.375(4) . ?
C35 H35 0.95(3) . ?
C36 C37 1.388(3) . ?
C36 H36 0.91(3) . ?
C38 C39 1.480(4) . ?
C39 C44 1.392(4) . ?
C39 C40 1.397(4) . ?
C40 C41 1.393(4) . ?
C40 H40 1.04(3) . ?
C41 C42 1.371(5) . ?
C41 H41 0.93(3) . ?
C42 C43 1.375(5) . ?
C42 H42 1.02(3) . ?
C43 C44 1.396(5) . ?
C43 H43 0.98(3) . ?
C44 H44 0.98(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
N1 Zn1 O1 C31 -75.53(18) . . . . ?
N4 Zn1 O1 C31 162.46(17) . . . . ?
N3 Zn1 O1 C31 51.60(19) . . . . ?
N2 Zn1 O1 C31 -61.8(14) . . . . ?
O1 Zn1 N1 C1 18.3(2) . . . . ?
N4 Zn1 N1 C1 129.6(2) . . . . ?
N3 Zn1 N1 C1 -97.2(2) . . . . ?
N2 Zn1 N1 C1 -160.9(2) . . . . ?
O1 Zn1 N1 C5 -167.91(17) . . . . ?
N4 Zn1 N1 C5 -56.66(19) . . . . ?
N3 Zn1 N1 C5 76.57(19) . . . . ?
N2 Zn1 N1 C5 12.87(17) . . . . ?
O1 Zn1 N2 C7 76.0(14) . . . . ?
N1 Zn1 N2 C7 89.85(16) . . . . ?
N4 Zn1 N2 C7 -147.78(17) . . . . ?
N3 Zn1 N2 C7 -38.22(15) . . . . ?
O1 Zn1 N2 C19 -164.6(13) . . . . ?
N1 Zn1 N2 C19 -150.74(17) . . . . ?
N4 Zn1 N2 C19 -28.37(16) . . . . ?
N3 Zn1 N2 C19 81.18(17) . . . . ?
O1 Zn1 N2 C6 -43.8(14) . . . . ?
N1 Zn1 N2 C6 -30.00(16) . . . . ?
N4 Zn1 N2 C6 92.37(16) . . . . ?
N3 Zn1 N2 C6 -158.07(17) . . . . ?
O1 Zn1 N3 C12 15.0(2) . . . . ?
N1 Zn1 N3 C12 127.3(2) . . . . ?
N4 Zn1 N3 C12 -94.7(2) . . . . ?
N2 Zn1 N3 C12 -168.1(2) . . . . ?
O1 Zn1 N3 C8 -146.52(16) . . . . ?
N1 Zn1 N3 C8 -34.24(19) . . . . ?
N4 Zn1 N3 C8 103.85(16) . . . . ?
N2 Zn1 N3 C8 30.43(16) . . . . ?
O1 Zn1 N4 C20 -150.46(16) . . . . ?
N1 Zn1 N4 C20 100.69(17) . . . . ?
N3 Zn1 N4 C20 -39.33(17) . . . . ?
N2 Zn1 N4 C20 31.83(16) . . . . ?
O1 Zn1 N4 C24 1.0(2) . . . . ?
N1 Zn1 N4 C24 -107.8(2) . . . . ?
N3 Zn1 N4 C24 112.15(19) . . . . ?
N2 Zn1 N4 C24 -176.7(2) . . . . ?
C5 N1 C1 C2 -0.1(4) . . . . ?
Zn1 N1 C1 C2 173.6(2) . . . . ?
N1 C1 C2 C3 -0.3(4) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C1 N1 C5 C4 0.6(4) . . . . ?
Zn1 N1 C5 C4 -173.6(2) . . . . ?
C1 N1 C5 C6 -178.1(2) . . . . ?
Zn1 N1 C5 C6 7.7(3) . . . . ?
C3 C4 C5 N1 -0.8(4) . . . . ?
C3 C4 C5 C6 177.8(3) . . . . ?
C7 N2 C6 C5 -73.4(2) . . . . ?
C19 N2 C6 C5 159.27(19) . . . . ?
Zn1 N2 C6 C5 42.2(2) . . . . ?
N1 C5 C6 N2 -34.6(3) . . . . ?
C4 C5 C6 N2 146.8(2) . . . . ?
C19 N2 C7 C8 -75.1(2) . . . . ?
C6 N2 C7 C8 157.2(2) . . . . ?
Zn1 N2 C7 C8 41.2(2) . . . . ?
C12 N3 C8 C9 -0.9(3) . . . . ?
Zn1 N3 C8 C9 162.2(2) . . . . ?
C12 N3 C8 C7 -179.5(2) . . . . ?
Zn1 N3 C8 C7 -16.3(3) . . . . ?
N2 C7 C8 N3 -17.8(3) . . . . ?
N2 C7 C8 C9 163.7(2) . . . . ?
N3 C8 C9 C10 -2.2(4) . . . . ?
C7 C8 C9 C10 176.2(3) . . . . ?
C8 C9 C10 C11 2.9(4) . . . . ?
C9 C10 C11 C12 -0.5(5) . . . . ?
C8 N3 C12 C11 3.4(4) . . . . ?
Zn1 N3 C12 C11 -157.0(2) . . . . ?
C8 N3 C12 C13 -173.7(2) . . . . ?
Zn1 N3 C12 C13 25.8(3) . . . . ?
C10 C11 C12 N3 -2.8(4) . . . . ?
C10 C11 C12 C13 174.4(3) . . . . ?
N3 C12 C13 C14 46.5(3) . . . . ?
C11 C12 C13 C14 -130.7(3) . . . . ?
N3 C12 C13 C18 -135.5(3) . . . . ?
C11 C12 C13 C18 47.3(4) . . . . ?
C18 C13 C14 C15 0.5(4) . . . . ?
C12 C13 C14 C15 178.5(2) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
C14 C15 C16 C17 -0.5(4) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C16 C17 C18 C13 1.3(4) . . . . ?
C14 C13 C18 C17 -1.3(4) . . . . ?
C12 C13 C18 C17 -179.4(2) . . . . ?
C7 N2 C19 C20 137.3(2) . . . . ?
C6 N2 C19 C20 -95.1(3) . . . . ?
Zn1 N2 C19 C20 21.7(3) . . . . ?
C24 N4 C20 C21 -4.1(4) . . . . ?
Zn1 N4 C20 C21 149.4(2) . . . . ?
C24 N4 C20 C19 176.8(2) . . . . ?
Zn1 N4 C20 C19 -29.7(3) . . . . ?
N2 C19 C20 N4 4.8(3) . . . . ?
N2 C19 C20 C21 -174.4(2) . . . . ?
N4 C20 C21 C22 0.2(4) . . . . ?
C19 C20 C21 C22 179.3(3) . . . . ?
C20 C21 C22 C23 3.1(4) . . . . ?
C21 C22 C23 C24 -2.6(4) . . . . ?
C20 N4 C24 C23 4.6(4) . . . . ?
Zn1 N4 C24 C23 -144.4(2) . . . . ?
C20 N4 C24 C25 -171.8(2) . . . . ?
Zn1 N4 C24 C25 39.2(3) . . . . ?
C22 C23 C24 N4 -1.3(4) . . . . ?
C22 C23 C24 C25 175.0(2) . . . . ?
N4 C24 C25 C26 31.6(3) . . . . ?
C23 C24 C25 C26 -144.8(3) . . . . ?
N4 C24 C25 C30 -151.8(2) . . . . ?
C23 C24 C25 C30 31.8(4) . . . . ?
C30 C25 C26 C27 0.4(4) . . . . ?
C24 C25 C26 C27 177.1(3) . . . . ?
C25 C26 C27 C28 0.1(4) . . . . ?
C26 C27 C28 C29 -0.1(5) . . . . ?
C27 C28 C29 C30 -0.4(5) . . . . ?
C28 C29 C30 C25 1.0(5) . . . . ?
C26 C25 C30 C29 -0.9(4) . . . . ?
C24 C25 C30 C29 -177.6(3) . . . . ?
Zn1 O1 C31 O2 -3.0(3) . . . . ?
Zn1 O1 C31 C32 177.53(15) . . . . ?
O2 C31 C32 C37 18.6(4) . . . . ?
O1 C31 C32 C37 -162.0(2) . . . . ?
O2 C31 C32 C33 -161.0(2) . . . . ?
O1 C31 C32 C33 18.5(3) . . . . ?
C37 C32 C33 C34 -1.3(4) . . . . ?
C31 C32 C33 C34 178.3(2) . . . . ?
C32 C33 C34 C35 1.8(4) . . . . ?
C33 C34 C35 C36 -1.1(4) . . . . ?
C34 C35 C36 C37 0.1(4) . . . . ?
C33 C32 C37 C36 0.3(4) . . . . ?
C31 C32 C37 C36 -179.3(2) . . . . ?
C33 C32 C37 O3 177.2(2) . . . . ?
C31 C32 C37 O3 -2.4(4) . . . . ?
C35 C36 C37 C32 0.4(4) . . . . ?
C35 C36 C37 O3 -176.8(2) . . . . ?
C38 O3 C37 C32 63.0(3) . . . . ?
C38 O3 C37 C36 -119.9(3) . . . . ?
C37 O3 C38 O4 6.9(3) . . . . ?
C37 O3 C38 C39 -176.6(2) . . . . ?
O4 C38 C39 C44 -3.3(4) . . . . ?
O3 C38 C39 C44 -179.7(2) . . . . ?
O4 C38 C39 C40 176.1(3) . . . . ?
O3 C38 C39 C40 -0.3(3) . . . . ?
C44 C39 C40 C41 0.5(4) . . . . ?
C38 C39 C40 C41 -178.9(2) . . . . ?
C39 C40 C41 C42 -1.0(4) . . . . ?
C40 C41 C42 C43 1.1(5) . . . . ?
C41 C42 C43 C44 -0.7(5) . . . . ?
C40 C39 C44 C43 -0.1(4) . . . . ?
C38 C39 C44 C43 179.3(2) . . . . ?
C42 C43 C44 C39 0.2(4) . . . . ?
O6 S1 C45 F1 179.0(3) . . . . ?
O5 S1 C45 F1 56.6(3) . . . . ?
O7 S1 C45 F1 -61.8(3) . . . . ?
O6 S1 C45 F3 -58.7(3) . . . . ?
O5 S1 C45 F3 178.9(2) . . . . ?
O7 S1 C45 F3 60.5(3) . . . . ?
O6 S1 C45 F2 59.8(3) . . . . ?
O5 S1 C45 F2 -62.5(3) . . . . ?
O7 S1 C45 F2 179.0(2) . . . . ?
|
1501474.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501474.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_1501474
loop_
_publ_author_name
'Katarzyna Grubel'
'Brynna J. Laughlin'
'Thora R. Maltais'
'Rhett C. Smith'
'Atta M. Arif'
'Lisa M. Berreau'
_publ_section_title
;
Photochemically-induced dioxygenase-type CO-release reactivity of Group
12 metal flavonolate complexes
;
_journal_issue 37
_journal_name_full 'Chemical Communications'
_journal_page_first 10431
_journal_page_last 10433
_journal_paper_doi 10.1039/c1cc13961d
_journal_volume 47
_journal_year 2011
_chemical_formula_moiety 'C44 H35 Cd N4 O4, Cl O4, C2 H3 N'
_chemical_formula_sum 'C46 H38 Cd Cl N5 O8'
_chemical_formula_weight 936.66
_chemical_name_systematic
;
?
;
_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 102.5400(9)
_cell_angle_beta 116.8087(6)
_cell_angle_gamma 99.7178(9)
_cell_formula_units_Z 2
_cell_length_a 13.2066(2)
_cell_length_b 13.24300(10)
_cell_length_c 14.3060(2)
_cell_measurement_reflns_used 9137
_cell_measurement_temperature 150(1)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 1.018
_cell_volume 2075.18(5)
_computing_cell_refinement DENZO-SMN
_computing_data_collection 'Nonius COLLECT'
_computing_data_reduction DENZO-SMN
_computing_molecular_graphics 'WinGX, Ortep3'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution SIR97
_diffrn_ambient_temperature 150(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method 'Phi and Omega 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 0.0202
_diffrn_reflns_av_sigmaI/netI 0.0355
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 17877
_diffrn_reflns_theta_full 27.47
_diffrn_reflns_theta_max 27.47
_diffrn_reflns_theta_min 2.41
_exptl_absorpt_coefficient_mu 0.652
_exptl_absorpt_correction_T_max 0.9200
_exptl_absorpt_correction_T_min 0.8644
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.499
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 956
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.907
_refine_diff_density_min -1.184
_refine_diff_density_rms 0.066
_refine_ls_extinction_coef 0.0045(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 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 571
_refine_ls_number_reflns 9483
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.0469
_refine_ls_R_factor_gt 0.0348
_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^)+(0.0314P)^2^+1.6605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0749
_refine_ls_wR_factor_ref 0.0803
_reflns_number_gt 8015
_reflns_number_total 9483
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file c1cc13961d.txt
_cod_data_source_block usu205
_cod_database_code 1501474
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
Cd1 Cd 0.250333(14) 0.219526(13) 0.824474(13) 0.02710(7) Uani 1 1 d . . .
Cl1 Cl 0.08992(6) 0.39491(7) 0.24998(6) 0.0528(2) Uani 1 1 d . . .
O1 O 0.36304(14) 0.15922(12) 0.74267(13) 0.0314(4) Uani 1 1 d . . .
O2 O 0.34803(14) 0.09859(13) 0.86903(13) 0.0328(4) Uani 1 1 d . . .
O3 O 0.47979(15) 0.07149(14) 0.64887(14) 0.0354(4) Uani 1 1 d . . .
O4 O 0.67534(16) 0.16674(15) 0.74501(15) 0.0448(4) Uani 1 1 d . . .
N1 N 0.21487(17) 0.32723(15) 0.71084(15) 0.0298(4) Uani 1 1 d . . .
N2 N 0.12092(16) 0.31304(15) 0.84909(15) 0.0288(4) Uani 1 1 d . . .
N3 N 0.05195(16) 0.08401(15) 0.72429(15) 0.0301(4) Uani 1 1 d . . .
N4 N 0.35278(16) 0.34620(14) 1.01191(14) 0.0254(4) Uani 1 1 d . . .
N5 N 0.8483(5) 0.8937(3) -0.0077(4) 0.193(3) Uani 1 1 d . . .
C1 C 0.2325(2) 0.31226(19) 0.62402(19) 0.0345(5) Uani 1 1 d . . .
H1 H 0.2727 0.2616 0.6134 0.041 Uiso 1 1 calc R . .
C2 C 0.1943(2) 0.3679(2) 0.5496(2) 0.0392(6) Uani 1 1 d . . .
H2 H 0.2079 0.3559 0.4889 0.047 Uiso 1 1 calc R . .
C3 C 0.1360(2) 0.4412(2) 0.5653(2) 0.0408(6) Uani 1 1 d . . .
H3 H 0.1088 0.4804 0.5153 0.049 Uiso 1 1 calc R . .
C4 C 0.1175(2) 0.4571(2) 0.65430(19) 0.0372(6) Uani 1 1 d . . .
H4 H 0.0773 0.5072 0.6662 0.045 Uiso 1 1 calc R . .
C5 C 0.1584(2) 0.39887(18) 0.72628(18) 0.0297(5) Uani 1 1 d . . .
C6 C 0.1468(2) 0.41588(18) 0.82799(18) 0.0306(5) Uani 1 1 d . . .
H6A H 0.2219 0.4675 0.8931 0.037 Uiso 1 1 calc R . .
H6B H 0.0820 0.4484 0.8182 0.037 Uiso 1 1 calc R . .
C7 C -0.0037(2) 0.24507(19) 0.7692(2) 0.0351(5) Uani 1 1 d . . .
H7A H -0.0285 0.2558 0.6965 0.042 Uiso 1 1 calc R . .
H7B H -0.0560 0.2687 0.7959 0.042 Uiso 1 1 calc R . .
C8 C -0.0195(2) 0.1261(2) 0.75399(19) 0.0335(5) Uani 1 1 d . . .
C9 C -0.1068(2) 0.0635(2) 0.7644(2) 0.0428(6) Uani 1 1 d . . .
H9 H -0.1558 0.0953 0.7856 0.051 Uiso 1 1 calc R . .
C10 C -0.1206(2) -0.0465(2) 0.7432(2) 0.0474(7) Uani 1 1 d . . .
H10 H -0.1767 -0.0906 0.7537 0.057 Uiso 1 1 calc R . .
C11 C -0.0527(2) -0.0916(2) 0.7069(2) 0.0416(6) Uani 1 1 d . . .
H11 H -0.0640 -0.1676 0.6889 0.050 Uiso 1 1 calc R . .
C12 C 0.0328(2) -0.02470(18) 0.69680(19) 0.0322(5) Uani 1 1 d . . .
C13 C 0.0993(2) -0.07208(18) 0.64755(19) 0.0320(5) Uani 1 1 d . . .
C14 C 0.1240(2) -0.1689(2) 0.6592(2) 0.0429(6) Uani 1 1 d . . .
H14 H 0.1029 -0.2022 0.7031 0.051 Uiso 1 1 calc R . .
C15 C 0.1790(3) -0.2162(2) 0.6071(3) 0.0509(7) Uani 1 1 d . . .
H15 H 0.1954 -0.2818 0.6154 0.061 Uiso 1 1 calc R . .
C16 C 0.2102(2) -0.1687(2) 0.5432(2) 0.0502(7) Uani 1 1 d . . .
H16 H 0.2479 -0.2016 0.5076 0.060 Uiso 1 1 calc R . .
C17 C 0.1866(2) -0.0732(2) 0.5313(2) 0.0424(6) Uani 1 1 d . . .
H17 H 0.2080 -0.0403 0.4874 0.051 Uiso 1 1 calc R . .
C18 C 0.1315(2) -0.0252(2) 0.58332(18) 0.0335(5) Uani 1 1 d . . .
H18 H 0.1158 0.0406 0.5748 0.040 Uiso 1 1 calc R . .
C19 C 0.1474(2) 0.33438(19) 0.96442(19) 0.0324(5) Uani 1 1 d . . .
H19A H 0.1104 0.2669 0.9713 0.039 Uiso 1 1 calc R . .
H19B H 0.1115 0.3900 0.9823 0.039 Uiso 1 1 calc R . .
C20 C 0.2791(2) 0.37312(18) 1.04684(18) 0.0285(5) Uani 1 1 d . . .
C21 C 0.3197(2) 0.4327(2) 1.15700(19) 0.0370(6) Uani 1 1 d . . .
H21 H 0.2656 0.4514 1.1792 0.044 Uiso 1 1 calc R . .
C22 C 0.4401(2) 0.4637(2) 1.23292(19) 0.0394(6) Uani 1 1 d . . .
H22 H 0.4701 0.5037 1.3086 0.047 Uiso 1 1 calc R . .
C23 C 0.5165(2) 0.43627(19) 1.19788(18) 0.0342(5) Uani 1 1 d . . .
H23 H 0.5995 0.4568 1.2494 0.041 Uiso 1 1 calc R . .
C24 C 0.4712(2) 0.37819(17) 1.08643(18) 0.0268(5) Uani 1 1 d . . .
C25 C 0.5527(2) 0.35343(17) 1.04667(18) 0.0280(5) Uani 1 1 d . . .
C26 C 0.5366(2) 0.36312(17) 0.94630(18) 0.0285(5) Uani 1 1 d . . .
H26 H 0.4716 0.3853 0.9017 0.034 Uiso 1 1 calc R . .
C27 C 0.6152(2) 0.34059(18) 0.9110(2) 0.0357(5) Uani 1 1 d . . .
H27 H 0.6028 0.3460 0.8418 0.043 Uiso 1 1 calc R . .
C28 C 0.7109(2) 0.3104(2) 0.9764(2) 0.0424(6) Uani 1 1 d . . .
H28 H 0.7646 0.2954 0.9522 0.051 Uiso 1 1 calc R . .
C29 C 0.7288(2) 0.3020(2) 1.0768(2) 0.0440(6) Uani 1 1 d . . .
H29 H 0.7954 0.2820 1.1221 0.053 Uiso 1 1 calc R . .
C30 C 0.6503(2) 0.32245(19) 1.1116(2) 0.0372(6) Uani 1 1 d . . .
H30 H 0.6625 0.3155 1.1803 0.045 Uiso 1 1 calc R . .
C31 C 0.38427(18) 0.09934(17) 0.80141(18) 0.0265(5) Uani 1 1 d . . .
C32 C 0.45328(19) 0.02111(17) 0.79138(17) 0.0270(5) Uani 1 1 d . . .
C33 C 0.4696(2) -0.04710(18) 0.85523(19) 0.0314(5) Uani 1 1 d . . .
H33 H 0.4393 -0.0416 0.9045 0.038 Uiso 1 1 calc R . .
C34 C 0.5291(2) -0.1229(2) 0.8484(2) 0.0378(6) Uani 1 1 d . . .
H34 H 0.5419 -0.1667 0.8947 0.045 Uiso 1 1 calc R . .
C35 C 0.5696(2) -0.1345(2) 0.7745(2) 0.0419(6) Uani 1 1 d . . .
H35 H 0.6080 -0.1879 0.7680 0.050 Uiso 1 1 calc R . .
C36 C 0.5542(2) -0.0685(2) 0.7098(2) 0.0396(6) Uani 1 1 d . . .
H36 H 0.5822 -0.0763 0.6588 0.048 Uiso 1 1 calc R . .
C37 C 0.4978(2) 0.00910(19) 0.71944(18) 0.0312(5) Uani 1 1 d . . .
C38 C 0.5747(2) 0.15188(19) 0.67300(19) 0.0325(5) Uani 1 1 d . . .
C39 C 0.5386(2) 0.21914(18) 0.59974(19) 0.0313(5) Uani 1 1 d . . .
C40 C 0.4197(2) 0.2042(2) 0.52692(19) 0.0342(5) Uani 1 1 d . . .
H40 H 0.3590 0.1494 0.5219 0.041 Uiso 1 1 calc R . .
C41 C 0.3899(2) 0.2698(2) 0.4613(2) 0.0394(6) Uani 1 1 d . . .
H41 H 0.3085 0.2597 0.4109 0.047 Uiso 1 1 calc R . .
C42 C 0.4778(3) 0.3493(2) 0.4689(2) 0.0444(6) Uani 1 1 d . . .
H42 H 0.4567 0.3942 0.4240 0.053 Uiso 1 1 calc R . .
C43 C 0.5962(3) 0.3646(2) 0.5410(2) 0.0479(7) Uani 1 1 d . . .
H43 H 0.6564 0.4191 0.5451 0.058 Uiso 1 1 calc R . .
C44 C 0.6273(2) 0.2999(2) 0.6078(2) 0.0400(6) Uani 1 1 d . . .
H44 H 0.7087 0.3110 0.6587 0.048 Uiso 1 1 calc R . .
C45 C 0.8347(3) 0.9735(3) 0.0054(3) 0.0709(10) Uani 1 1 d . . .
C46 C 0.8182(5) 1.0748(3) 0.0165(4) 0.122(2) Uani 1 1 d . . .
H46A H 0.8934 1.1296 0.0423 0.183 Uiso 1 1 calc R . .
H46B H 0.7919 1.0916 0.0705 0.183 Uiso 1 1 calc R . .
H46C H 0.7575 1.0749 -0.0555 0.183 Uiso 1 1 calc R . .
O5 O 0.01056(18) 0.35544(18) 0.28295(18) 0.0564(5) Uani 1 1 d . A .
O6 O 0.19907(17) 0.3717(2) 0.30509(18) 0.0579(6) Uani 1 1 d . A .
O7 O 0.1101(4) 0.4928(5) 0.2460(9) 0.077(3) Uani 0.573(16) 1 d P A 1
O8 O 0.0269(5) 0.3159(8) 0.1298(4) 0.079(3) Uani 0.573(16) 1 d P A 1
O7' O 0.1213(6) 0.5228(6) 0.3300(13) 0.078(4) Uani 0.427(16) 1 d P A 2
O8' O 0.0556(10) 0.4115(17) 0.1546(9) 0.110(8) Uani 0.427(16) 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
Cd1 0.02484(9) 0.02627(9) 0.02655(10) 0.00531(6) 0.01063(7) 0.01090(6)
Cl1 0.0285(3) 0.0900(6) 0.0599(4) 0.0539(4) 0.0232(3) 0.0247(3)
O1 0.0328(9) 0.0268(8) 0.0324(9) 0.0102(7) 0.0127(7) 0.0144(7)
O2 0.0338(9) 0.0333(9) 0.0317(9) 0.0095(7) 0.0158(7) 0.0149(7)
O3 0.0348(9) 0.0435(10) 0.0331(9) 0.0205(7) 0.0157(8) 0.0187(8)
O4 0.0355(10) 0.0474(11) 0.0409(10) 0.0138(8) 0.0097(9) 0.0176(8)
N1 0.0315(10) 0.0308(10) 0.0236(9) 0.0069(8) 0.0108(8) 0.0136(8)
N2 0.0274(10) 0.0292(10) 0.0257(9) 0.0051(8) 0.0112(8) 0.0113(8)
N3 0.0243(10) 0.0316(10) 0.0277(10) 0.0048(8) 0.0104(8) 0.0077(8)
N4 0.0297(10) 0.0228(9) 0.0226(9) 0.0087(7) 0.0114(8) 0.0095(7)
N5 0.150(4) 0.053(2) 0.161(4) 0.003(2) -0.080(3) 0.039(3)
C1 0.0388(14) 0.0347(13) 0.0275(12) 0.0065(10) 0.0151(11) 0.0158(10)
C2 0.0447(15) 0.0469(15) 0.0244(12) 0.0104(10) 0.0159(11) 0.0172(12)
C3 0.0452(15) 0.0467(15) 0.0234(12) 0.0139(11) 0.0088(11) 0.0201(12)
C4 0.0386(14) 0.0400(13) 0.0268(12) 0.0093(10) 0.0089(11) 0.0223(11)
C5 0.0296(12) 0.0294(11) 0.0237(11) 0.0052(9) 0.0088(9) 0.0126(9)
C6 0.0363(13) 0.0285(11) 0.0256(11) 0.0068(9) 0.0127(10) 0.0181(10)
C7 0.0245(12) 0.0389(13) 0.0341(13) 0.0041(10) 0.0109(10) 0.0137(10)
C8 0.0211(11) 0.0393(13) 0.0287(12) 0.0022(10) 0.0080(10) 0.0080(9)
C9 0.0267(13) 0.0508(16) 0.0397(14) 0.0005(12) 0.0161(11) 0.0067(11)
C10 0.0357(14) 0.0466(16) 0.0473(16) 0.0025(12) 0.0225(13) -0.0043(12)
C11 0.0366(14) 0.0340(13) 0.0427(15) 0.0033(11) 0.0185(12) 0.0012(11)
C12 0.0262(12) 0.0310(12) 0.0277(12) 0.0025(9) 0.0093(10) 0.0038(9)
C13 0.0244(11) 0.0280(11) 0.0288(12) -0.0005(9) 0.0077(10) 0.0037(9)
C14 0.0418(15) 0.0312(13) 0.0434(15) 0.0045(11) 0.0166(12) 0.0074(11)
C15 0.0452(16) 0.0335(14) 0.0538(18) -0.0022(12) 0.0155(14) 0.0147(12)
C16 0.0350(14) 0.0522(17) 0.0396(15) -0.0104(13) 0.0113(12) 0.0139(12)
C17 0.0285(13) 0.0553(16) 0.0257(12) -0.0011(11) 0.0086(10) 0.0060(11)
C18 0.0240(11) 0.0365(13) 0.0238(11) 0.0002(9) 0.0050(9) 0.0050(9)
C19 0.0333(13) 0.0345(12) 0.0308(12) 0.0067(10) 0.0189(11) 0.0116(10)
C20 0.0361(12) 0.0274(11) 0.0246(11) 0.0113(9) 0.0160(10) 0.0105(9)
C21 0.0477(15) 0.0399(13) 0.0285(12) 0.0116(10) 0.0243(12) 0.0105(11)
C22 0.0518(16) 0.0393(14) 0.0207(11) 0.0087(10) 0.0161(11) 0.0078(12)
C23 0.0373(13) 0.0340(12) 0.0220(11) 0.0116(9) 0.0079(10) 0.0070(10)
C24 0.0306(12) 0.0221(10) 0.0240(11) 0.0119(8) 0.0092(9) 0.0076(9)
C25 0.0272(11) 0.0199(10) 0.0277(11) 0.0073(8) 0.0076(9) 0.0053(8)
C26 0.0285(12) 0.0223(10) 0.0272(11) 0.0067(9) 0.0093(9) 0.0066(9)
C27 0.0372(13) 0.0281(12) 0.0370(13) 0.0045(10) 0.0193(11) 0.0057(10)
C28 0.0352(14) 0.0335(13) 0.0506(16) 0.0017(11) 0.0208(12) 0.0110(11)
C29 0.0324(14) 0.0363(14) 0.0478(16) 0.0079(11) 0.0090(12) 0.0157(11)
C30 0.0335(13) 0.0340(13) 0.0339(13) 0.0123(10) 0.0082(11) 0.0113(10)
C31 0.0189(10) 0.0218(10) 0.0250(11) 0.0008(8) 0.0038(9) 0.0044(8)
C32 0.0253(11) 0.0237(10) 0.0227(11) 0.0039(8) 0.0061(9) 0.0087(8)
C33 0.0339(12) 0.0295(12) 0.0277(12) 0.0095(9) 0.0125(10) 0.0120(10)
C34 0.0427(14) 0.0326(13) 0.0370(13) 0.0170(10) 0.0142(12) 0.0197(11)
C35 0.0492(16) 0.0371(14) 0.0395(14) 0.0117(11) 0.0181(12) 0.0278(12)
C36 0.0465(15) 0.0479(15) 0.0317(13) 0.0141(11) 0.0205(12) 0.0284(12)
C37 0.0323(12) 0.0343(12) 0.0244(11) 0.0117(9) 0.0098(10) 0.0154(10)
C38 0.0345(13) 0.0355(12) 0.0290(12) 0.0076(10) 0.0164(11) 0.0174(10)
C39 0.0369(13) 0.0329(12) 0.0292(12) 0.0088(9) 0.0192(10) 0.0172(10)
C40 0.0383(13) 0.0371(13) 0.0311(12) 0.0128(10) 0.0183(11) 0.0170(11)
C41 0.0468(15) 0.0401(14) 0.0310(13) 0.0123(11) 0.0170(12) 0.0204(12)
C42 0.0676(19) 0.0361(14) 0.0365(14) 0.0155(11) 0.0280(14) 0.0230(13)
C43 0.0603(19) 0.0408(15) 0.0512(17) 0.0167(13) 0.0350(15) 0.0137(13)
C44 0.0396(14) 0.0413(14) 0.0399(14) 0.0098(11) 0.0217(12) 0.0142(11)
C45 0.065(2) 0.0474(19) 0.063(2) 0.0116(16) 0.0036(17) 0.0215(16)
C46 0.162(5) 0.051(2) 0.077(3) 0.003(2) 0.003(3) 0.047(3)
O5 0.0430(11) 0.0741(14) 0.0696(14) 0.0358(12) 0.0361(11) 0.0214(10)
O6 0.0362(11) 0.0953(16) 0.0654(14) 0.0510(13) 0.0281(10) 0.0362(11)
O7 0.042(2) 0.054(3) 0.131(9) 0.050(4) 0.031(4) 0.015(2)
O8 0.059(3) 0.124(6) 0.035(2) 0.005(3) 0.022(2) 0.015(3)
O7' 0.042(3) 0.051(4) 0.129(10) 0.028(5) 0.036(4) 0.012(3)
O8' 0.091(8) 0.25(2) 0.065(7) 0.106(12) 0.056(7) 0.117(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'
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'
Cd Cd -0.8075 1.2024 '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
O2 Cd1 N1 140.59(6) . . ?
O2 Cd1 N2 146.73(6) . . ?
N1 Cd1 N2 72.65(7) . . ?
O2 Cd1 O1 56.42(6) . . ?
N1 Cd1 O1 84.18(6) . . ?
N2 Cd1 O1 156.65(6) . . ?
O2 Cd1 N4 95.08(6) . . ?
N1 Cd1 N4 105.14(6) . . ?
N2 Cd1 N4 70.54(6) . . ?
O1 Cd1 N4 119.88(6) . . ?
O2 Cd1 N3 94.16(6) . . ?
N1 Cd1 N3 99.30(7) . . ?
N2 Cd1 N3 73.96(6) . . ?
O1 Cd1 N3 107.88(6) . . ?
N4 Cd1 N3 127.72(6) . . ?
O2 Cd1 C31 28.29(6) . . ?
N1 Cd1 C31 112.31(7) . . ?
N2 Cd1 C31 174.24(7) . . ?
O1 Cd1 C31 28.13(6) . . ?
N4 Cd1 C31 110.00(6) . . ?
N3 Cd1 C31 101.90(6) . . ?
O7 Cl1 O8' 59.3(6) . . ?
O7 Cl1 O5 121.6(4) . . ?
O8' Cl1 O5 123.3(5) . . ?
O7 Cl1 O6 110.5(2) . . ?
O8' Cl1 O6 120.8(3) . . ?
O5 Cl1 O6 111.12(13) . . ?
O7 Cl1 O8 107.3(4) . . ?
O8' Cl1 O8 48.0(6) . . ?
O5 Cl1 O8 100.0(3) . . ?
O6 Cl1 O8 104.4(4) . . ?
O7 Cl1 O7' 41.2(3) . . ?
O8' Cl1 O7' 98.5(7) . . ?
O5 Cl1 O7' 90.8(4) . . ?
O6 Cl1 O7' 102.5(3) . . ?
O8 Cl1 O7' 145.0(4) . . ?
C31 O1 Cd1 86.80(13) . . ?
C31 O2 Cd1 94.05(13) . . ?
C38 O3 C37 117.64(18) . . ?
C5 N1 C1 119.0(2) . . ?
C5 N1 Cd1 115.83(15) . . ?
C1 N1 Cd1 124.56(15) . . ?
C19 N2 C6 110.66(17) . . ?
C19 N2 C7 111.21(18) . . ?
C6 N2 C7 111.03(18) . . ?
C19 N2 Cd1 108.18(13) . . ?
C6 N2 Cd1 106.69(13) . . ?
C7 N2 Cd1 108.91(13) . . ?
C8 N3 C12 118.6(2) . . ?
C8 N3 Cd1 108.56(14) . . ?
C12 N3 Cd1 124.13(15) . . ?
C20 N4 C24 118.77(19) . . ?
C20 N4 Cd1 113.58(14) . . ?
C24 N4 Cd1 126.91(14) . . ?
N1 C1 C2 122.4(2) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 119.2(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 116.35(19) . . ?
C4 C5 C6 122.2(2) . . ?
N2 C6 C5 111.78(17) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 C8 112.10(19) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N3 C8 C9 122.6(2) . . ?
N3 C8 C7 115.8(2) . . ?
C9 C8 C7 121.5(2) . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 119.4(2) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
N3 C12 C11 121.2(2) . . ?
N3 C12 C13 118.0(2) . . ?
C11 C12 C13 120.6(2) . . ?
C18 C13 C14 118.6(2) . . ?
C18 C13 C12 120.7(2) . . ?
C14 C13 C12 120.6(2) . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 119.7(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 120.8(2) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
N2 C19 C20 112.55(18) . . ?
N2 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N2 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C21 122.5(2) . . ?
N4 C20 C19 118.44(19) . . ?
C21 C20 C19 119.0(2) . . ?
C22 C21 C20 118.5(2) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 119.7(2) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
N4 C24 C23 121.1(2) . . ?
N4 C24 C25 118.65(19) . . ?
C23 C24 C25 120.2(2) . . ?
C26 C25 C30 118.6(2) . . ?
C26 C25 C24 121.3(2) . . ?
C30 C25 C24 120.1(2) . . ?
C27 C26 C25 120.4(2) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 120.1(2) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.2(2) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 120.1(2) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.7(2) . . ?
C29 C30 H30 119.7 . . ?
C25 C30 H30 119.7 . . ?
O1 C31 O2 122.7(2) . . ?
O1 C31 C32 120.6(2) . . ?
O2 C31 C32 116.7(2) . . ?
O1 C31 Cd1 65.06(11) . . ?
O2 C31 Cd1 57.65(11) . . ?
C32 C31 Cd1 173.43(16) . . ?
C37 C32 C33 117.2(2) . . ?
C37 C32 C31 124.7(2) . . ?
C33 C32 C31 118.0(2) . . ?
C34 C33 C32 121.4(2) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C35 C34 C33 119.9(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0(2) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 119.8(2) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C36 C37 C32 121.7(2) . . ?
C36 C37 O3 117.9(2) . . ?
C32 C37 O3 120.3(2) . . ?
O4 C38 O3 123.9(2) . . ?
O4 C38 C39 124.9(2) . . ?
O3 C38 C39 111.2(2) . . ?
C40 C39 C44 120.2(2) . . ?
C40 C39 C38 121.4(2) . . ?
C44 C39 C38 118.4(2) . . ?
C39 C40 C41 119.5(2) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 H40 120.2 . . ?
C42 C41 C40 120.2(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 120.6(2) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C42 C43 C44 119.8(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C39 C44 C43 119.7(3) . . ?
C39 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
N5 C45 C46 176.4(7) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 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
Cd1 O2 2.2439(16) . ?
Cd1 N1 2.3328(19) . ?
Cd1 N2 2.3762(18) . ?
Cd1 O1 2.4062(16) . ?
Cd1 N4 2.4172(17) . ?
Cd1 N3 2.4592(18) . ?
Cd1 C31 2.649(2) . ?
Cl1 O7 1.298(4) . ?
Cl1 O8' 1.312(6) . ?
Cl1 O5 1.401(2) . ?
Cl1 O6 1.4228(19) . ?
Cl1 O8 1.542(5) . ?
Cl1 O7' 1.687(11) . ?
O1 C31 1.251(3) . ?
O2 C31 1.259(3) . ?
O3 C38 1.351(3) . ?
O3 C37 1.404(3) . ?
O4 C38 1.206(3) . ?
N1 C5 1.342(3) . ?
N1 C1 1.344(3) . ?
N2 C19 1.472(3) . ?
N2 C6 1.476(3) . ?
N2 C7 1.477(3) . ?
N3 C8 1.349(3) . ?
N3 C12 1.354(3) . ?
N4 C20 1.342(3) . ?
N4 C24 1.356(3) . ?
N5 C45 1.092(5) . ?
C1 C2 1.383(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.378(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.503(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.508(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.387(4) . ?
C9 C10 1.384(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.488(3) . ?
C13 C18 1.386(3) . ?
C13 C14 1.400(4) . ?
C14 C15 1.385(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.505(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.396(3) . ?
C21 C22 1.380(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.394(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.476(3) . ?
C25 C26 1.392(3) . ?
C25 C30 1.398(3) . ?
C26 C27 1.389(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.378(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.515(3) . ?
C32 C37 1.392(3) . ?
C32 C33 1.394(3) . ?
C33 C34 1.389(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(3) . ?
C36 H36 0.9500 . ?
C38 C39 1.489(3) . ?
C39 C40 1.386(3) . ?
C39 C44 1.390(4) . ?
C40 C41 1.389(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.376(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.377(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.381(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 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
O2 Cd1 O1 C31 1.22(11) . . . . ?
N1 Cd1 O1 C31 -179.65(13) . . . . ?
N2 Cd1 O1 C31 -172.58(15) . . . . ?
N4 Cd1 O1 C31 76.22(13) . . . . ?
N3 Cd1 O1 C31 -81.73(13) . . . . ?
N1 Cd1 O2 C31 -2.57(17) . . . . ?
N2 Cd1 O2 C31 174.31(12) . . . . ?
O1 Cd1 O2 C31 -1.21(11) . . . . ?
N4 Cd1 O2 C31 -123.99(13) . . . . ?
N3 Cd1 O2 C31 107.52(13) . . . . ?
O2 Cd1 N1 C5 -171.89(14) . . . . ?
N2 Cd1 N1 C5 9.90(15) . . . . ?
O1 Cd1 N1 C5 -173.03(16) . . . . ?
N4 Cd1 N1 C5 -53.60(17) . . . . ?
N3 Cd1 N1 C5 79.76(16) . . . . ?
C31 Cd1 N1 C5 -173.21(15) . . . . ?
O2 Cd1 N1 C1 17.3(2) . . . . ?
N2 Cd1 N1 C1 -161.0(2) . . . . ?
O1 Cd1 N1 C1 16.12(18) . . . . ?
N4 Cd1 N1 C1 135.54(18) . . . . ?
N3 Cd1 N1 C1 -91.10(19) . . . . ?
C31 Cd1 N1 C1 15.9(2) . . . . ?
O2 Cd1 N2 C19 34.4(2) . . . . ?
N1 Cd1 N2 C19 -147.63(15) . . . . ?
O1 Cd1 N2 C19 -155.00(14) . . . . ?
N4 Cd1 N2 C19 -34.01(13) . . . . ?
N3 Cd1 N2 C19 106.95(15) . . . . ?
C31 Cd1 N2 C19 62.4(7) . . . . ?
O2 Cd1 N2 C6 153.53(13) . . . . ?
N1 Cd1 N2 C6 -28.54(13) . . . . ?
O1 Cd1 N2 C6 -35.9(2) . . . . ?
N4 Cd1 N2 C6 85.07(13) . . . . ?
N3 Cd1 N2 C6 -133.97(14) . . . . ?
C31 Cd1 N2 C6 -178.5(6) . . . . ?
O2 Cd1 N2 C7 -86.56(18) . . . . ?
N1 Cd1 N2 C7 91.37(15) . . . . ?
O1 Cd1 N2 C7 84.0(2) . . . . ?
N4 Cd1 N2 C7 -155.02(16) . . . . ?
N3 Cd1 N2 C7 -14.05(15) . . . . ?
C31 Cd1 N2 C7 -58.6(7) . . . . ?
O2 Cd1 N3 C8 135.80(16) . . . . ?
N1 Cd1 N3 C8 -81.37(16) . . . . ?
N2 Cd1 N3 C8 -12.56(15) . . . . ?
O1 Cd1 N3 C8 -168.20(15) . . . . ?
N4 Cd1 N3 C8 36.10(18) . . . . ?
C31 Cd1 N3 C8 163.31(16) . . . . ?
O2 Cd1 N3 C12 -11.10(18) . . . . ?
N1 Cd1 N3 C12 131.73(18) . . . . ?
N2 Cd1 N3 C12 -159.46(19) . . . . ?
O1 Cd1 N3 C12 44.89(19) . . . . ?
N4 Cd1 N3 C12 -110.80(18) . . . . ?
C31 Cd1 N3 C12 16.41(19) . . . . ?
O2 Cd1 N4 C20 -126.31(14) . . . . ?
N1 Cd1 N4 C20 87.84(15) . . . . ?
N2 Cd1 N4 C20 22.88(14) . . . . ?
O1 Cd1 N4 C20 179.80(13) . . . . ?
N3 Cd1 N4 C20 -27.06(17) . . . . ?
C31 Cd1 N4 C20 -151.03(14) . . . . ?
O2 Cd1 N4 C24 43.63(17) . . . . ?
N1 Cd1 N4 C24 -102.22(17) . . . . ?
N2 Cd1 N4 C24 -167.18(18) . . . . ?
O1 Cd1 N4 C24 -10.26(19) . . . . ?
N3 Cd1 N4 C24 142.89(16) . . . . ?
C31 Cd1 N4 C24 18.91(18) . . . . ?
C5 N1 C1 C2 -0.2(4) . . . . ?
Cd1 N1 C1 C2 170.43(19) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C1 N1 C5 C4 0.3(3) . . . . ?
Cd1 N1 C5 C4 -171.06(18) . . . . ?
C1 N1 C5 C6 -177.1(2) . . . . ?
Cd1 N1 C5 C6 11.5(3) . . . . ?
C3 C4 C5 N1 -0.3(4) . . . . ?
C3 C4 C5 C6 176.9(2) . . . . ?
C19 N2 C6 C5 161.96(19) . . . . ?
C7 N2 C6 C5 -74.0(2) . . . . ?
Cd1 N2 C6 C5 44.5(2) . . . . ?
N1 C5 C6 N2 -39.4(3) . . . . ?
C4 C5 C6 N2 143.3(2) . . . . ?
C19 N2 C7 C8 -81.1(2) . . . . ?
C6 N2 C7 C8 155.19(19) . . . . ?
Cd1 N2 C7 C8 38.0(2) . . . . ?
C12 N3 C8 C9 4.3(3) . . . . ?
Cd1 N3 C8 C9 -144.7(2) . . . . ?
C12 N3 C8 C7 -172.4(2) . . . . ?
Cd1 N3 C8 C7 38.6(2) . . . . ?
N2 C7 C8 N3 -54.9(3) . . . . ?
N2 C7 C8 C9 128.4(2) . . . . ?
N3 C8 C9 C10 -0.1(4) . . . . ?
C7 C8 C9 C10 176.4(2) . . . . ?
C8 C9 C10 C11 -3.5(4) . . . . ?
C9 C10 C11 C12 2.8(4) . . . . ?
C8 N3 C12 C11 -4.9(3) . . . . ?
Cd1 N3 C12 C11 138.9(2) . . . . ?
C8 N3 C12 C13 170.7(2) . . . . ?
Cd1 N3 C12 C13 -45.5(3) . . . . ?
C10 C11 C12 N3 1.4(4) . . . . ?
C10 C11 C12 C13 -174.1(2) . . . . ?
N3 C12 C13 C18 -30.8(3) . . . . ?
C11 C12 C13 C18 144.9(2) . . . . ?
N3 C12 C13 C14 153.3(2) . . . . ?
C11 C12 C13 C14 -31.0(3) . . . . ?
C18 C13 C14 C15 -0.2(4) . . . . ?
C12 C13 C14 C15 175.8(2) . . . . ?
C13 C14 C15 C16 0.0(4) . . . . ?
C14 C15 C16 C17 0.1(4) . . . . ?
C15 C16 C17 C18 0.0(4) . . . . ?
C14 C13 C18 C17 0.3(3) . . . . ?
C12 C13 C18 C17 -175.7(2) . . . . ?
C16 C17 C18 C13 -0.1(4) . . . . ?
C6 N2 C19 C20 -73.4(2) . . . . ?
C7 N2 C19 C20 162.71(19) . . . . ?
Cd1 N2 C19 C20 43.2(2) . . . . ?
C24 N4 C20 C21 -0.1(3) . . . . ?
Cd1 N4 C20 C21 170.74(18) . . . . ?
C24 N4 C20 C19 -178.14(19) . . . . ?
Cd1 N4 C20 C19 -7.3(2) . . . . ?
N2 C19 C20 N4 -24.7(3) . . . . ?
N2 C19 C20 C21 157.1(2) . . . . ?
N4 C20 C21 C22 -0.8(4) . . . . ?
C19 C20 C21 C22 177.2(2) . . . . ?
C20 C21 C22 C23 0.7(4) . . . . ?
C21 C22 C23 C24 0.4(4) . . . . ?
C20 N4 C24 C23 1.2(3) . . . . ?
Cd1 N4 C24 C23 -168.32(16) . . . . ?
C20 N4 C24 C25 -176.87(19) . . . . ?
Cd1 N4 C24 C25 13.7(3) . . . . ?
C22 C23 C24 N4 -1.3(3) . . . . ?
C22 C23 C24 C25 176.7(2) . . . . ?
N4 C24 C25 C26 40.3(3) . . . . ?
C23 C24 C25 C26 -137.7(2) . . . . ?
N4 C24 C25 C30 -141.5(2) . . . . ?
C23 C24 C25 C30 40.4(3) . . . . ?
C30 C25 C26 C27 1.1(3) . . . . ?
C24 C25 C26 C27 179.3(2) . . . . ?
C25 C26 C27 C28 -1.2(3) . . . . ?
C26 C27 C28 C29 0.3(4) . . . . ?
C27 C28 C29 C30 0.8(4) . . . . ?
C28 C29 C30 C25 -0.9(4) . . . . ?
C26 C25 C30 C29 0.0(3) . . . . ?
C24 C25 C30 C29 -178.2(2) . . . . ?
Cd1 O1 C31 O2 -2.2(2) . . . . ?
Cd1 O1 C31 C32 176.18(17) . . . . ?
Cd1 O2 C31 O1 2.3(2) . . . . ?
Cd1 O2 C31 C32 -176.08(15) . . . . ?
O2 Cd1 C31 O1 -177.9(2) . . . . ?
N1 Cd1 C31 O1 0.38(14) . . . . ?
N2 Cd1 C31 O1 149.3(6) . . . . ?
N4 Cd1 C31 O1 -116.35(12) . . . . ?
N3 Cd1 C31 O1 105.74(12) . . . . ?
N1 Cd1 C31 O2 178.23(12) . . . . ?
N2 Cd1 C31 O2 -32.8(7) . . . . ?
O1 Cd1 C31 O2 177.9(2) . . . . ?
N4 Cd1 C31 O2 61.51(13) . . . . ?
N3 Cd1 C31 O2 -76.40(13) . . . . ?
O2 Cd1 C31 C32 32.2(13) . . . . ?
N1 Cd1 C31 C32 -149.5(13) . . . . ?
N2 Cd1 C31 C32 -0.6(17) . . . . ?
O1 Cd1 C31 C32 -149.9(14) . . . . ?
N4 Cd1 C31 C32 93.8(13) . . . . ?
N3 Cd1 C31 C32 -44.2(13) . . . . ?
O1 C31 C32 C37 0.2(3) . . . . ?
O2 C31 C32 C37 178.6(2) . . . . ?
Cd1 C31 C32 C37 148.3(12) . . . . ?
O1 C31 C32 C33 -177.1(2) . . . . ?
O2 C31 C32 C33 1.3(3) . . . . ?
Cd1 C31 C32 C33 -29.0(14) . . . . ?
C37 C32 C33 C34 0.8(3) . . . . ?
C31 C32 C33 C34 178.3(2) . . . . ?
C32 C33 C34 C35 -2.4(4) . . . . ?
C33 C34 C35 C36 2.0(4) . . . . ?
C34 C35 C36 C37 -0.1(4) . . . . ?
C35 C36 C37 C32 -1.5(4) . . . . ?
C35 C36 C37 O3 -177.5(2) . . . . ?
C33 C32 C37 C36 1.1(3) . . . . ?
C31 C32 C37 C36 -176.2(2) . . . . ?
C33 C32 C37 O3 177.0(2) . . . . ?
C31 C32 C37 O3 -0.3(3) . . . . ?
C38 O3 C37 C36 -76.1(3) . . . . ?
C38 O3 C37 C32 107.9(2) . . . . ?
C37 O3 C38 O4 6.9(3) . . . . ?
C37 O3 C38 C39 -172.83(18) . . . . ?
O4 C38 C39 C40 -173.0(2) . . . . ?
O3 C38 C39 C40 6.8(3) . . . . ?
O4 C38 C39 C44 5.4(3) . . . . ?
O3 C38 C39 C44 -174.8(2) . . . . ?
C44 C39 C40 C41 0.6(3) . . . . ?
C38 C39 C40 C41 179.0(2) . . . . ?
C39 C40 C41 C42 -0.3(4) . . . . ?
C40 C41 C42 C43 0.3(4) . . . . ?
C41 C42 C43 C44 -0.8(4) . . . . ?
C40 C39 C44 C43 -1.1(4) . . . . ?
C38 C39 C44 C43 -179.5(2) . . . . ?
C42 C43 C44 C39 1.2(4) . . . . ?
|
1501475.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501475.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_1501475
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.19(2)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0055(9)
_cell_length_b 3.9897(8)
_cell_length_c 4.0426(8)
_cell_volume 64.60(2)
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm_DC4.cif
_cod_data_source_block chateigner4_
_cod_original_sg_symbol_H-M 'P m'
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501475
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.7(2)
Ti1 Ti4+ 1 b 0.471(7) 0.5 0.531(6) 0.36 0 0.2(2)
Nb1 Nb5+ 1 b 0.471(7) 0.5 0.531(6) 0.427 0 0.2(2)
Mg1 Mg2+ 1 b 0.471(7) 0.5 0.531(6) 0.213 0 0.2(2)
O1 O2- 1 a 0.505(5) 0. 0.509(5) 1. 0 0.7(2)
O2 O2- 1 b 0.515(6) 0.5 0.001(3) 1. 0 1.7(2)
O3 O2- 1 b -0.029(5) 0.5 0.569(5) 1. 0 0.5(2)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501476.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501476.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_1501476
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.9960(1)
_cell_length_b 3.9960(1)
_cell_length_c 4.0492(2)
_cell_volume 64.658(4)
_diffrn_ambient_temperature 300
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_P4mm_DC5.cif
_cod_data_source_block chateigner5_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501476
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.3(1)
Ti1 Ti4+ 1 b 0.5 0.5 0.542(1) 0.36 0 0.48(9)
Nb1 Nb5+ 1 b 0.5 0.5 0.542(1) 0.427 0 0.48(9)
Mg1 Mg2+ 1 b 0.5 0.5 0.542(1) 0.213 0 0.48(9)
O1 O2- 1 b 0.5 0.5 0.063(1) 1. 0 1.10(7)
O2 O2- 2 c 0.5 0. 0.578 1. 0 1.16(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501477.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501477.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_1501477
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.9948(1)
_cell_length_b 3.9948(1)
_cell_length_c 4.0513(2)
_cell_volume 64.652(4)
_diffrn_ambient_temperature 275
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC6.cif
_cod_data_source_block chateigner6_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501477
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.19(8)
Ti1 Ti4+ 1 b 0.5 0.5 0.545(1) 0.36 0 0.42(9)
Nb1 Nb5+ 1 b 0.5 0.5 0.545(1) 0.427 0 0.42(9)
Mg1 Mg2+ 1 b 0.5 0.5 0.545(1) 0.213 0 0.42(9)
O1 O2- 1 b 0.5 0.5 0.069(1) 1. 0 0.99(7)
O2 O2- 2 c 0.5 0. 0.584(1) 1. 0 1.05(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501478.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501478.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_1501478
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.9938(1)
_cell_length_b 3.9938(1)
_cell_length_c 4.0532(2)
_cell_volume 64.650(4)
_diffrn_ambient_temperature 245
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC7.cif
_cod_data_source_block chateigner7_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501478
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.14(6)
Ti1 Ti4+ 1 b 0.5 0.5 0.546(1) 0.36 0 0.35(6)
Nb1 Nb5+ 1 b 0.5 0.5 0.546(1) 0.427 0 0.35(6)
Mg1 Mg2+ 1 b 0.5 0.5 0.546(1) 0.213 0 0.35(6)
O1 O2- 1 b 0.5 0.5 0.072(1) 1. 0 1.11(5)
O2 O2- 2 c 0.5 0. 0.5867(1) 1. 0 1.02(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501479.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501479.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_1501479
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0010(1)
_cell_length_b 4.0010(1)
_cell_length_c 4.0411(2)
_cell_volume 64.690(4)
_diffrn_ambient_temperature 350
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC8.cif
_cod_data_source_block chateigner8_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501479
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.90(5)
Ti1 Ti4+ 1 b 0.5 0.5 0.5373(9) 0.36 0 0.22(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.5373(9) 0.427 0 0.22(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.5373(9) 0.213 0 0.22(3)
O1 O2- 1 b 0.5 0.5 0.059(1) 1. 0 1.23(5)
O2 O2- 2 c 0.5 0. 0.5711(7) 1. 0 1.19(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501480.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501480.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_1501480
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0024(1)
_cell_length_b 4.0024(1)
_cell_length_c 4.0393(1)
_cell_volume 64.706(3)
_diffrn_ambient_temperature 375
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC9.cif
_cod_data_source_block chateigner9_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501480
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.96(5)
Ti1 Ti4+ 1 b 0.5 0.5 0.536(1) 0.36 0 0.30(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.536(1) 0.427 0 0.30(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.536(1) 0.213 0 0.30(3)
O1 O2- 1 b 0.5 0.5 0.057(1) 1. 0 1.27(5)
O2 O2- 2 c 0.5 0. 0.5679(7) 1. 0 1.26(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501481.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501481.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_1501481
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0083(2)
_cell_length_b 4.0083(2)
_cell_length_c 4.0290(2)
_cell_volume 64.732(6)
_diffrn_ambient_temperature 430
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC10.cif
_cod_data_source_block chateigner10_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501481
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.46(6)
Ti1 Ti4+ 1 b 0.5 0.5 0.526(1) 0.36 0 0.50(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.526(1) 0.427 0 0.50(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.526(1) 0.213 0 0.50(3)
O1 O2- 1 b 0.5 0.5 0.043(1) 1. 0 1.45(8)
O2 O2- 2 c 0.5 0. 0.5533(8) 1. 0 1.37(4)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501482.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501482.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_1501482
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0108(1)
_cell_length_b 4.0108(1)
_cell_length_c 4.0237(2)
_cell_volume 64.727(4)
_diffrn_ambient_temperature 445
_journal_article_reference 024101
_cod_data_source_file PMN0_36PT_P4mm_DC11.cif
_cod_data_source_block chateigner11_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501482
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.67(7)
Ti1 Ti4+ 1 b 0.5 0.5 0.515(1) 0.36 0 0.44(4)
Nb1 Nb5+ 1 b 0.5 0.5 0.515(1) 0.427 0 0.44(4)
Mg1 Mg2+ 1 b 0.5 0.5 0.515(1) 0.213 0 0.44(4)
O1 O2- 1 b 0.5 0.5 0.036(1) 1. 0 1.6(1)
O2 O2- 2 c 0.5 0. 0.543(1) 1. 0 1.32(4)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501483.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501483.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_1501483
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.23(1)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0054(6)
_cell_length_b 3.9896(5)
_cell_length_c 4.0452(6)
_cell_volume 64.642(16)
_diffrn_ambient_temperature 200
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm_DC12.cif
_cod_data_source_block chateigner4_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501483
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.4(1)
Ti1 Ti4+ 1 b 0.461(3) 0.5 0.525(4) 0.36 0 0.0(1)
Nb1 Nb5+ 1 b 0.461(3) 0.5 0.525(4) 0.427 0 0.0(1)
Mg1 Mg2+ 1 b 0.461(3) 0.5 0.525(4) 0.213 0 0.0(1)
O1 O2- 1 a 0.497(2) 0. 0.506(3) 1. 0 0.6(1)
O2 O2- 1 b 0.515(3) 0.5 -0.004(6) 1. 0 1.2(1)
O3 O2- 1 b -0.042(2) 0.5 0.571(3) 1. 0 0.4(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501484.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501484.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_1501484
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.241(4)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0050(2)
_cell_length_b 3.9851(2)
_cell_length_c 4.0475(2)
_cell_volume 64.599(6)
_diffrn_ambient_temperature 150
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm_DC13.cif
_cod_data_source_block chateigner4_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501484
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.92(9)
Ti1 Ti4+ 1 b 0.469(3) 0.5 0.532(3) 0.36 0 0.27(9)
Nb1 Nb5+ 1 b 0.469(3) 0.5 0.532(3) 0.427 0 0.27(9)
Mg1 Mg2+ 1 b 0.469(3) 0.5 0.532(3) 0.213 0 0.27(9)
O1 O2- 1 a 0.499(2) 0. 0.519(3) 1. 0 0.90(9)
O2 O2- 1 b 0.496(3) 0.5 0.003(4) 1. 0 1.4(1)
O3 O2- 1 b -0.039(2) 0.5 0.578(2) 1. 0 0.20(6)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501485.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501485.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_1501485
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.252(4)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0022(2)
_cell_length_b 3.9838(2)
_cell_length_c 4.0503(2)
_cell_volume 64.577(6)
_diffrn_ambient_temperature 80
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm_DC14.cif
_cod_data_source_block chateigner4_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501485
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.75(8)
Ti1 Ti4+ 1 b 0.462(2) 0.5 0.537(2) 0.36 0 0.13(8)
Nb1 Nb5+ 1 b 0.462(2) 0.5 0.537(2) 0.427 0 0.13(8)
Mg1 Mg2+ 1 b 0.462(2) 0.5 0.537(2) 0.213 0 0.13(8)
O1 O2- 1 a 0.492(2) 0. 0.516(2) 1. 0 0.86(7)
O2 O2- 1 b 0.482(2) 0.5 0.001(3) 1. 0 0.89(7)
O3 O2- 1 b -0.043(1) 0.5 0.581(2) 1. 0 0.43(7)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501486.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501486.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_1501486
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0152(1)
_cell_length_b 4.0152(1)
_cell_length_c 4.0152(1)
_cell_volume 64.732(3)
_diffrn_ambient_temperature 480
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm-3m_DC15.cif
_cod_data_source_block chateigner4_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501486
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.71(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.36 0 0.44(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.427 0 0.44(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.213 0 0.44(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.64(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501487.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501487.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_1501487
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.64-[PbTiO3]0.36'
_chemical_formula_sum 'Mg0.213 Nb0.427 O3 Pb Ti0.36'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0157(1)
_cell_length_b 4.0157(1)
_cell_length_c 4.0157(1)
_cell_volume 64.757(3)
_diffrn_ambient_temperature 530
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm-3m_DC16.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.213 Nb0.427 Ti0.36 O3'
_cod_database_code 1501487
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.74(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.36 0 0.53(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.427 0 0.53(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.213 0 0.53(3)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.64(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501488.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501488.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_1501488
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0191(1)
_cell_length_b 4.0191(1)
_cell_length_c 4.0191(1)
_cell_volume 64.921(3)
_diffrn_ambient_temperature 480
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm-3m_DC17.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501488
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.8(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.32 0 0.6(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.453 0 0.6(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.227 0 0.6(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.67(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501489.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501489.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_1501489
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0189(1)
_cell_length_b 4.0189(1)
_cell_length_c 4.0189(1)
_cell_volume 64.911(3)
_diffrn_ambient_temperature 455
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_36PT_Pm-3m_DC18.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501489
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.83(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.32 0 0.45(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.453 0 0.45(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.227 0 0.45(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.64(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501490.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501490.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_1501490
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0159(1)
_cell_length_b 4.0159(1)
_cell_length_c 4.0249(2)
_cell_volume 64.911(4)
_diffrn_ambient_temperature 430
_journal_article_reference 024101
_cod_data_source_file PMN0_32PT_P4mm_DC19.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501490
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.74(6)
Ti1 Ti4+ 1 b 0.5 0.5 0.517(1) 0.32 0 0.54(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.517(1) 0.453 0 0.54(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.517(1) 0.227 0 0.54(3)
O1 O2- 1 b 0.5 0.5 0.031(2) 1. 0 1.7(1)
O2 O2- 2 c 0.5 0. 0.543(1) 1. 0 1.37(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501491.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501491.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_1501491
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0134(1)
_cell_length_b 4.0134(1)
_cell_length_c 4.0301(2)
_cell_volume 64.914(4)
_diffrn_ambient_temperature 400
_journal_article_reference 024101
_cod_data_source_file PMN0_32PT_P4mm_DC20.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501491
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.53(5)
Ti1 Ti4+ 1 b 0.5 0.5 0.525(1) 0.32 0 0.33(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.525(1) 0.453 0 0.33(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.525(1) 0.227 0 0.33(3)
O1 O2- 1 b 0.5 0.5 0.044(1) 1. 0 1.84(9)
O2 O2- 2 c 0.5 0. 0.5541(8) 1. 0 1.23(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501492.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501492.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_1501492
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0121(1)
_cell_length_b 4.0121(1)
_cell_length_c 4.0322(2)
_cell_volume 64.906(4)
_diffrn_ambient_temperature 390
_journal_article_reference 024101
_cod_data_source_file PMN0_32PT_P4mm_DC21.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501492
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.35(5)
Ti1 Ti4+ 1 b 0.5 0.5 0.529(1) 0.32 0 0.33(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.529(1) 0.453 0 0.33(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.529(1) 0.227 0 0.33(3)
O1 O2- 1 b 0.5 0.5 0.049(1) 1. 0 1.72(8)
O2 O2- 2 c 0.5 0. 0.5597(8) 1. 0 1.22(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501493.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501493.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_1501493
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.128(6)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0190(2)
_cell_length_b 4.0078(2)
_cell_length_c 4.0276(2)
_cell_volume 64.874(6)
_diffrn_ambient_temperature 340
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_32PT_Pm_DC22.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501493
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.01(6)
Ti1 Ti4+ 1 b 0.460(3) 0.5 0.525(2) 0.32 0 0.24(6)
Nb1 Nb5+ 1 b 0.460(3) 0.5 0.525(2) 0.453 0 0.24(6)
Mg1 Mg2+ 1 b 0.460(3) 0.5 0.525(2) 0.227 0 0.24(6)
O1 O2- 1 a 0.493(2) 0. 0.517(2) 1. 0 1.0(7)
O2 O2- 1 b 0.491(3) 0.5 0.003(3) 1. 0 1.4(1)
O3 O2- 1 b -0.034(2) 0.5 0.566(2) 1. 0 1.2(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501494.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501494.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_1501494
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.178(5)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0200(3)
_cell_length_b 4.0046(2)
_cell_length_c 4.0281(3)
_cell_volume 64.846(8)
_diffrn_ambient_temperature 300
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_32PT_Pm_DC23.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501494
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.91(1)
Ti1 Ti4+ 1 b 0.472(3) 0.5 0.533(2) 0.32 0 0.40(5)
Nb1 Nb5+ 1 b 0.472(3) 0.5 0.533(2) 0.453 0 0.40(5)
Mg1 Mg2+ 1 b 0.472(3) 0.5 0.533(2) 0.227 0 0.40(5)
O1 O2- 1 a 0.496(2) 0. 0.519(2) 1. 0 0.84(5)
O2 O2- 1 b 0.504(4) 0.5 0.007(4) 1. 0 1.39(9)
O3 O2- 1 b -0.036(2) 0.5 0.572(2) 1. 0 1.08(8)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501495.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501495.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_1501495
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.241(4)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0204(4)
_cell_length_b 3.9997(2)
_cell_length_c 4.0289(4)
_cell_volume 64.786(10)
_diffrn_ambient_temperature 200
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_32PT_Pm_DC24.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501495
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.51(6)
Ti1 Ti4+ 1 b 0.465(3) 0.5 0.545(2) 0.32 0 0.19(5)
Nb1 Nb5+ 1 b 0.465(3) 0.5 0.545(2) 0.453 0 0.19(5)
Mg1 Mg2+ 1 b 0.465(3) 0.5 0.545(2) 0.227 0 0.19(5)
O1 O2- 1 a 0.497(2) 0. 0.524(2) 1. 0 0.60(5)
O2 O2- 1 b 0.507(4) 0.5 0.009(4) 1. 0 1.27(8)
O3 O2- 1 b -0.046(2) 0.5 0.579(2) 1. 0 0.71(6)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501496.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501496.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_1501496
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.314(5)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0220(4)
_cell_length_b 3.9946(2)
_cell_length_c 4.0314(4)
_cell_volume 64.769(10)
_diffrn_ambient_temperature 80
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_32PT_Pm_DC25.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501496
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.52(6)
Ti1 Ti4+ 1 b 0.474(3) 0.5 0.550(2) 0.32 0 0.18(5)
Nb1 Nb5+ 1 b 0.474(3) 0.5 0.550(2) 0.453 0 0.18(5)
Mg1 Mg2+ 1 b 0.474(3) 0.5 0.550(2) 0.227 0 0.18(5)
O1 O2- 1 a 0.503(2) 0. 0.530(2) 1. 0 0.68(6)
O2 O2- 1 b 0.510(3) 0.5 0.019(3) 1. 0 1.02(8)
O3 O2- 1 b -0.047(2) 0.5 0.584(2) 1. 0 0.53(6)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501497.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501497.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_1501497
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0215(1)
_cell_length_b 4.0215(1)
_cell_length_c 4.0215(1)
_cell_volume 65.038(3)
_diffrn_ambient_temperature 550
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_29PT_Pm-3m_DC26.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501497
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.86(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.29 0 0.65(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.473 0 0.65(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.237 0 0.65(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.67(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501498.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501498.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_1501498
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0211(1)
_cell_length_b 4.0211(1)
_cell_length_c 4.0211(1)
_cell_volume 65.018(3)
_diffrn_ambient_temperature 500
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_29PT_Pm-3m_DC27.cif
_cod_data_source_block chateigner_
_cod_original_cell_volume 65.031(3)
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501498
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.89(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.29 0 0.61(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.473 0 0.61(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.237 0 0.61(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.64(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501499.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/14/1501499.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_1501499
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0206(1)
_cell_length_b 4.0206(1)
_cell_length_c 4.0206(1)
_cell_volume 64.994(3)
_diffrn_ambient_temperature 450
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_29PT_Pm-3m_DC28.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501499
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.86(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.29 0 0.46(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.473 0 0.46(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.237 0 0.46(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.65(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501500.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501500.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_1501500
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0166(1)
_cell_length_b 4.0166(1)
_cell_length_c 4.0287(2)
_cell_volume 64.995(4)
_diffrn_ambient_temperature 415
_journal_article_reference 024101
_cod_data_source_file PMN0_29PT_P4mm_DC29.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501500
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 18
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.75(5)
Ti1 Ti4+ 1 b 0.5 0.5 0.521(1) 0.29 0 0.45(3)
Nb1 Nb5+ 1 b 0.5 0.5 0.521(1) 0.473 0 0.45(3)
Mg1 Mg2+ 1 b 0.5 0.5 0.521(1) 0.237 0 0.45(3)
O1 O2- 1 b 0.5 0.5 0.038(1) 1. 0 1.8(1)
O2 O2- 2 c 0.5 0. 0.5495(9) 1. 0 1.25(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501501.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501501.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_1501501
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.125(8)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6968(3)
_cell_length_b 5.6820(4)
_cell_length_c 4.0132(3)
_cell_volume 129.904(15)
_diffrn_ambient_temperature 300
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_29PT_Cm_DC30.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501501
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.0070(8) 0.030(2) 0.051(3) 0. 0. 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.530(1) 0. 0.500(6) 0.29 0 0.63(6)
Nb1 Nb5+ 2 a 0.530(1) 0. 0.500(6) 0.473 0 0.63(6)
Mg1 Mg2+ 2 a 0.530(1) 0. 0.500(6) 0.237 0 0.63(6)
O1 O2- 2 a 0.536(1) 0. -0.009(5) 1. 0 1.0(1)
O2 O2- 4 b 0.295(1) 0.258(1) 0.481(4) 1. 0 1.42(7)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501502.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501502.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_1501502
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.240(6)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.7025(3)
_cell_length_b 5.6778(3)
_cell_length_c 4.0087(2)
_cell_volume 129.791(12)
_diffrn_ambient_temperature 80
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_29PT_Cm_DC31.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501502
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.0089(9) 0.027(1) 0.034(2) 0. 0. 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.5351(9) 0. 0.484(2) 0.29 0 0.35(3)
Nb1 Nb5+ 2 a 0.5351(9) 0. 0.484(2) 0.473 0 0.35(3)
Mg1 Mg2+ 2 a 0.5351(9) 0. 0.484(2) 0.237 0 0.35(3)
O1 O2- 2 a 0.5727(8) 0. -0.030(2) 1. 0 0.55(4)
O2 O2- 4 b 0.270(1) 0.2524(6) 0.498(2) 1. 0 0.87(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501503.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501503.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_1501503
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.248(5)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.7022(3)
_cell_length_b 5.6815(4)
_cell_length_c 4.0167(3)
_cell_volume 130.128(15)
_diffrn_ambient_temperature 80
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Cm_DC32.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501503
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.007(1) 0.027(1) 0.038(2) 0. 0.009(1) 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.532(1) 0. 0.474(2) 0.25 0 0.37(3)
Nb1 Nb5+ 2 a 0.532(1) 0. 0.474(2) 0.5 0 0.37(3)
Mg1 Mg2+ 2 a 0.532(1) 0. 0.474(2) 0.25 0 0.37(3)
O1 O2- 2 a 0.5714(9) 0. -0.037(2) 1. 0 0.73(4)
O2 O2- 4 b 0.272(1) 0.2530(6) 0.495(2) 1. 0 0.85(2)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501504.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501504.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_1501504
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.135(8)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6987(5)
_cell_length_b 5.687(6)
_cell_length_c 4.0211(4)
_cell_volume 130.32(14)
_diffrn_ambient_temperature 300
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Cm_DC33.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501504
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.014(1) 0.032(2) 0.036(4) 0. 0.011(1) 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.522(1) 0. 0.465(4) 0.25 0 0.41(4)
Nb1 Nb5+ 2 a 0.522(1) 0. 0.465(4) 0.5 0 0.41(4)
Mg1 Mg2+ 2 a 0.522(1) 0. 0.465(4) 0.25 0 0.41(4)
O1 O2- 2 a 0.552(1) 0. -0.030(4) 1. 0 1.16(9)
O2 O2- 4 b 0.265(2) 0.252(1) 0.492(4) 1. 0 1.28(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501505.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501505.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_1501505
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.109(1)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6969(6)
_cell_length_b 5.6889(5)
_cell_length_c 4.0215(1)
_cell_volume 130.333(18)
_diffrn_ambient_temperature 350
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Cm_DC34.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501505
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.019(2) 0.032(3) 0.037(5) 0. 0.011(2) 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.519(2) 0. 0.464(4) 0.25 0 0.43(4)
Nb1 Nb5+ 2 a 0.519(2) 0. 0.464(4) 0.5 0 0.43(4)
Mg1 Mg2+ 2 a 0.519(2) 0. 0.464(4) 0.25 0 0.43(4)
O1 O2- 2 a 0.546(2) 0. -0.029(4) 1. 0 1.4(1)
O2 O2- 4 b 0.266(3) 0.252(1) 0.490(4) 1. 0 1.40(7)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501506.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501506.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_1501506
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.083(1)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6952(6)
_cell_length_b 5.6903(8)
_cell_length_c 4.0220(1)
_cell_volume 130.34(2)
_diffrn_ambient_temperature 375
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Cm_DC35.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501506
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_B_11
_atom_site_aniso_B_22
_atom_site_aniso_B_33
_atom_site_aniso_B_12
_atom_site_aniso_B_13
_atom_site_aniso_B_23
Pb1 Pb2+ 0.024(4) 0.031(4) 0.035(4) 0. 0.010(3) 0.
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 0
Ti1 Ti4+ 2 a 0.515(2) 0. 0.460(4) 0.25 0 0.39(6)
Nb1 Nb5+ 2 a 0.515(2) 0. 0.460(4) 0.5 0 0.39(6)
Mg1 Mg2+ 2 a 0.515(2) 0. 0.460(4) 0.25 0 0.39(6)
O1 O2- 2 a 0.537(2) 0. -0.029(5) 1. 0 1.4(2)
O2 O2- 4 b 0.264(5) 0.252(2) 0.490(5) 1. 0 1.5(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501507.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501507.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_1501507
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0242(1)
_cell_length_b 4.0242(1)
_cell_length_c 4.0242(1)
_cell_volume 65.169(3)
_diffrn_ambient_temperature 400
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Pm-3m_DC36.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501507
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.994(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.25 0 0.38(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.5 0 0.38(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.25 0 0.38(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.67(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501508.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501508.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_1501508
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0244(1)
_cell_length_b 4.0244(1)
_cell_length_c 4.0244(1)
_cell_volume 65.178(3)
_diffrn_ambient_temperature 450
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Pm-3m_DC37.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501508
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.98(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.25 0 0.49(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.5 0 0.49(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.25 0 0.49(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.63(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501509.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501509.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_1501509
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
'Zaharko, Oksana'
_publ_section_title
;
Powder neutron diffraction study of phase transitions in and a phase
diagram of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3
;
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.74.1
_journal_volume 74
_journal_year 2006
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.75-[PbTiO3]0.25'
_chemical_formula_sum 'Mg0.25 Nb0.5 O3 Pb Ti0.25'
_space_group_IT_number 221
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall '-P 4 2 3'
_symmetry_space_group_name_H-M 'P m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.02545(1)
_cell_length_b 4.02545(1)
_cell_length_c 4.02545(1)
_cell_volume 65.2294(3)
_diffrn_ambient_temperature 500
_journal_article_reference 024101
_journal_pages_number 18
_cod_data_source_file PMN0_25PT_Pm-3m_DC38.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.25 Nb0.5 Ti0.25 O3'
_cod_database_code 1501509
loop_
_symmetry_equiv_pos_as_xyz
'z, y, -x'
'y, x, -z'
'x, z, -y'
'z, x, -y'
'y, z, -x'
'x, y, -z'
'z, -y, x'
'y, -x, z'
'x, -z, y'
'z, -x, y'
'y, -z, x'
'x, -y, z'
'-z, y, x'
'-y, x, z'
'-x, z, y'
'-z, x, y'
'-y, z, x'
'-x, y, z'
'-z, -y, -x'
'-y, -x, -z'
'-x, -z, -y'
'-z, -x, -y'
'-y, -z, -x'
'-x, -y, -z'
'-z, -y, x'
'-y, -x, z'
'-x, -z, y'
'-z, -x, y'
'-y, -z, x'
'-x, -y, z'
'-z, y, -x'
'-y, x, -z'
'-x, z, -y'
'-z, x, -y'
'-y, z, -x'
'-x, y, -z'
'z, -y, -x'
'y, -x, -z'
'x, -z, -y'
'z, -x, -y'
'y, -z, -x'
'x, -y, -z'
'z, y, x'
'y, x, z'
'x, z, y'
'z, x, y'
'y, z, x'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.92(4)
Ti1 Ti4+ 1 b 0.5 0.5 0.5 0.25 0 0.62(2)
Nb1 Nb5+ 1 b 0.5 0.5 0.5 0.5 0 0.62(2)
Mg1 Mg2+ 1 b 0.5 0.5 0.5 0.25 0 0.62(2)
O1 O2- 3 c 0.5 0.5 0. 1. 0 1.64(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501510.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501510.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_1501510
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
_publ_section_title
;
Evidence for MB and MC phases in the morphotropic phase boundary region
of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3: a Rietveld study
;
_journal_issue 6
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 18
_journal_paper_doi 10.1103/PhysRev.67.1
_journal_volume 67
_journal_year 2003
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.61-[PbTiO3]0.39'
_chemical_formula_sum 'Mg0.203 Nb0.407 O3 Pb Ti0.39'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.9920(0)
_cell_length_b 3.9920(0)
_cell_length_c 4.0516(1)
_cell_volume 64.5666(16)
_journal_article_reference 064102
_cod_data_source_file PMN0_39PT_P4mm_DC39.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.203 Nb0.407 Ti0.39 O3'
_cod_database_code 1501510
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 12
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 2.92(1)
Ti1 Ti4+ 1 b 0.5 0.5 0.532(1) 0.39 0 0.76(4)
Nb1 Nb5+ 1 b 0.5 0.5 0.532(1) 0.407 0 0.76(4)
Mg1 Mg2+ 1 b 0.5 0.5 0.532(1) 0.203 0 0.76(4)
O1 O2- 1 b 0.5 0.5 0.054(4) 1. 0 0.8(3)
O2 O2- 2 c 0.5 0. 0.601(2) 1. 0 0.4(2)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501511.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501511.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_1501511
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
_publ_section_title
;
Evidence for MB and MC phases in the morphotropic phase boundary region
of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3: a Rietveld study
;
_journal_issue 6
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 12
_journal_paper_doi 10.1103/PhysRev.67.1
_journal_volume 67
_journal_year 2003
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.68-[PbTiO3]0.32'
_chemical_formula_sum 'Mg0.227 Nb0.453 O3 Pb Ti0.32'
_space_group_IT_number 6
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2y'
_symmetry_space_group_name_H-M 'P 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.146(3)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 4.0183(2)
_cell_length_b 4.0046(1)
_cell_length_c 4.0276(2)
_cell_volume 64.811(5)
_diffrn_ambient_temperature 80
_journal_article_reference 064102
_cod_data_source_file PMN0_32PT_Pm_DC40.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.227 Nb0.453 Ti0.32 O3'
_cod_database_code 1501511
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 12
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, -y, z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 1 a 0. 0. 0. 1. 0 3.28
Ti1 Ti4+ 1 b 0.509(2) 0.5 0.5479(7) 0.32 0 0.20(3)
Nb1 Nb5+ 1 b 0.509(2) 0.5 0.5479(7) 0.453 0 0.20(3)
Mg1 Mg2+ 1 b 0.509(2) 0.5 0.5479(7) 0.227 0 0.20(3)
O1 O2- 1 a 0.47(1) 0. 0.57(1) 1. 0 0.2(2)
O2 O2- 1 b 0.417(8) 0.5 0.059(6) 1. 0 0.2(2)
O3 O2- 1 b -0.02(1) 0.5 0.57(1) 1. 0 0.0(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501512.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501512.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_1501512
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
_publ_section_title
;
Evidence for MB and MC phases in the morphotropic phase boundary region
of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3: a Rietveld study
;
_journal_issue 6
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 12
_journal_paper_doi 10.1103/PhysRev.67.1
_journal_volume 67
_journal_year 2003
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.71-[PbTiO3]0.29'
_chemical_formula_sum 'Mg0.237 Nb0.473 O3 Pb Ti0.29'
_space_group_IT_number 8
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'C -2y'
_symmetry_space_group_name_H-M 'C 1 m 1'
_cell_angle_alpha 90
_cell_angle_beta 90.136(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6951(2)
_cell_length_b 5.6813(2)
_cell_length_c 4.0138(1)
_cell_volume 129.868(7)
_journal_article_reference 064102
_cod_data_source_file PMN0_29PT_Cm_DC41.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb1 Mg0.237 Nb0.473 Ti0.29 O3'
_cod_database_code 1501512
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 12
#END Tags that were not found in dictionaries
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 2 a 0. 0. 0. 1. 0 3.08(2)
Ti1 Ti4+ 2 a 0.5250(8) 0. 0.498(2) 0.29 0 0.73(4)
Nb1 Nb5+ 2 a 0.5250(8) 0. 0.498(2) 0.473 0 0.73(4)
Mg1 Mg2+ 2 a 0.5250(8) 0. 0.498(2) 0.237 0 0.73(4)
O1 O2- 2 a 0.54(1) 0. -0.01(2) 1. 0 0.2(3)
O2 O2- 4 b 0.317(2) 0.267(4) 0.48(1) 1. 0 0.3(2)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501513.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501513.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_1501513
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
_publ_section_title
;
Evidence for MB and MC phases in the morphotropic phase boundary region
of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3: a Rietveld study
;
_journal_issue 6
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 12
_journal_paper_doi 10.1103/PhysRev.67.1
_journal_volume 67
_journal_year 2003
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.74-[PbTiO3]0.26'
_chemical_formula_sum 'Mg0.247 Nb0.493 O3 Pb Ti0.26'
_space_group_IT_number 160
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'R 3 -2"'
_symmetry_space_group_name_H-M 'R 3 m :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 5.6841(1)
_cell_length_b 5.6841(1)
_cell_length_c 6.9800(1)
_cell_volume 195.303(6)
_journal_article_reference 064102
_cod_data_source_file PMN0_26PT_R3mH_DC42.cif
_cod_data_source_block chateigner_
_cod_original_sg_symbol_H-M 'R 3 m H'
_cod_original_formula_sum 'Pb1 Mg0.247 Nb0.493 Ti0.26 O3'
_cod_database_code 1501513
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 12
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z
y-x,-x,z
-y,-x,z
y-x,y,z
x,x-y,z
2/3+x,1/3+y,1/3+z
2/3-y,1/3+x-y,1/3+z
2/3+y-x,1/3-x,1/3+z
2/3-y,1/3-x,1/3+z
2/3+y-x,1/3+y,1/3+z
2/3+x,1/3+x-y,1/3+z
1/3+x,2/3+y,2/3+z
1/3-y,2/3+x-y,2/3+z
1/3+y-x,2/3-x,2/3+z
1/3-y,2/3-x,2/3+z
1/3+y-x,2/3+y,2/3+z
1/3+x,2/3+x-y,2/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 0. 0. 0.546(1) 1. 2.91(2)
Ti1 Ti4+ 0. 0. 0.019(1) 0.26 0.14(4)
Nb1 Nb5+ 0. 0. 0.019(1) 0.493 0.14(4)
Mg1 Mg2+ 0. 0. 0.019(1) 0.247 0.14(4)
O1 O2- 0.325(3) 0.162(3) 0.1667 1. 0.3(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501514.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501514.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_1501514
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Pandey, Dhananjai'
_publ_section_title
;
Evidence for MB and MC phases in the morphotropic phase boundary region
of (1-x)[Pb(Mg1/3Nb2/3)O3]-xPbTiO3: a Rietveld study
;
_journal_issue 6
_journal_name_full
;
Physical Review B
;
_journal_page_first 1
_journal_page_last 12
_journal_paper_doi 10.1103/PhysRev.67.1
_journal_volume 67
_journal_year 2003
_chemical_formula_structural '[Pb(Mg1/3Nb2/3)O3]0.8-[PbTiO3]0.20'
_chemical_formula_sum 'Mg0.267 Nb0.533 O3 Pb Ti0.2'
_space_group_IT_number 160
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'R 3 -2"'
_symmetry_space_group_name_H-M 'R 3 m :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 5.6921(1)
_cell_length_b 5.6921(1)
_cell_length_c 6.9882(2)
_cell_volume 196.083(7)
_journal_article_reference 064102
_cod_data_source_file PMN0_20PT_R3mH_DC43.cif
_cod_data_source_block chateigner_
_cod_original_sg_symbol_H-M 'R 3 m H'
_cod_original_formula_sum 'Pb1 Mg0.267 Nb0.533 Ti0.2 O3'
_cod_database_code 1501514
#BEGIN Tags that were not found in dictionaries:
_journal_article_numberofpages 12
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z
y-x,-x,z
-y,-x,z
y-x,y,z
x,x-y,z
2/3+x,1/3+y,1/3+z
2/3-y,1/3+x-y,1/3+z
2/3+y-x,1/3-x,1/3+z
2/3-y,1/3-x,1/3+z
2/3+y-x,1/3+y,1/3+z
2/3+x,1/3+x-y,1/3+z
1/3+x,2/3+y,2/3+z
1/3-y,2/3+x-y,2/3+z
1/3+y-x,2/3-x,2/3+z
1/3-y,2/3-x,2/3+z
1/3+y-x,2/3+y,2/3+z
1/3+x,2/3+x-y,2/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Pb1 Pb2+ 0. 0. 0.542(1) 1. 3.02(1)
Ti1 Ti4+ 0. 0. 0.02(2) 0.2 0.61(7)
Nb1 Nb5+ 0. 0. 0.02(2) 0.533 0.61(7)
Mg1 Mg2+ 0. 0. 0.02(2) 0.267 0.61(7)
O1 O2- 0.353(3) 0.176(3) 0.1667 1. 0.0(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2
Nb5+ 5
O2- -2
Pb2+ 2
Ti4+ 4
|
1501515.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501515.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_1501515
loop_
_publ_author_name
'Frantti, J.'
'Lappalainen, J.'
'Eriksson, S.'
'Lantto, V.'
'Nishio, S.'
'Kakihana, M.'
'Ivanov, S.'
'Rundlof, H.'
_publ_section_title
;
Neutron diffraction studies of Pb (Zrx Ti1-x) O3 ceramics
;
_journal_name_full
;
Japanese Journal of Applied Physics, Part 1
;
_journal_page_first 5697
_journal_page_last 5703
_journal_paper_doi 10.1143/JJAP.39.5697
_journal_volume 39
_journal_year 2000
_chemical_formula_structural PbMg0.8Ti0.2O3
_chemical_formula_sum 'Mg0.8 O3 Pb Ti0.2'
_space_group_IT_number 99
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4 -2'
_symmetry_space_group_name_H-M 'P 4 m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.952510(25)
_cell_length_b 3.952510(25)
_cell_length_c 4.14840(6)
_cell_volume 64.8077(11)
_cod_data_source_file PZ08T02_P4mm_DC44.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'Pb Mg0.8 Ti0.2 O3'
_cod_database_code 1501515
loop_
_symmetry_equiv_pos_as_xyz
'y, -x, z'
'-y, x, z'
'-y, -x, z'
'y, x, z'
'x, -y, z'
'-x, y, z'
'-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_occupancy
_atom_site_U_iso_or_equiv
Pb1 Pb2+ 0.0085(12) 0.0085(12) 0.0000(19) 0.25 0.01041(24)
Zr1 Zr4+ 0.5 0.5 0.5632(21) 0.2 0.0045(8)
Ti1 Ti5+ 0.5 0.5 0.5452(20) 0.8 0.0045(8)
O1 O2- 0.5 0.5 0.1035(19) 1 0.00919(20)
O2 O2- 0.5 0. 0.6162(19) 1. 0.00899(13)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Pb2+ 2
Zr4+ 4
Ti4+ 4
O2- -2
|
1501516.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501516.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_1501516
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.90590(6)
_cell_length_b 2.90590(6)
_cell_length_c 2.83767(8)
_cell_volume 20.7517(8)
_diffrn_ambient_pressure 1.01E2
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC45.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501516
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501517.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501517.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_1501517
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.90583(9)
_cell_length_b 2.90583(9)
_cell_length_c 2.83765(13)
_cell_volume 20.7506(13)
_diffrn_ambient_pressure 107500
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC46.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501517
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501518.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501518.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_1501518
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.90512(9)
_cell_length_b 2.90512(9)
_cell_length_c 2.83689(13)
_cell_volume 20.7349(13)
_diffrn_ambient_pressure 317500
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC47.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501518
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501519.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501519.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_1501519
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.90070(9)
_cell_length_b 2.90070(9)
_cell_length_c 2.83459(13)
_cell_volume 20.6551(13)
_diffrn_ambient_pressure 1715000
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC48.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501519
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501520.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501520.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_1501520
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.89385(9)
_cell_length_b 2.89385(9)
_cell_length_c 2.82990(12)
_cell_volume 20.5236(13)
_diffrn_ambient_pressure 4245000
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC49.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501520
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501521.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501521.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_1501521
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.87453(9)
_cell_length_b 2.87453(9)
_cell_length_c 2.81659(12)
_cell_volume 20.1552(12)
_diffrn_ambient_pressure 11940000
_diffrn_ambient_temperature 300
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC50.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501521
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
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|
1501522.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501522.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_1501522
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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|
1501523.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501523.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_1501523
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_publ_author_name
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;
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;
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|
1501524.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501524.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_1501524
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_publ_author_name
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'Fei, Yingwei'
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'Funakoshi, Kenichi'
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;
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;
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|
1501525.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501525.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_1501525
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_publ_author_name
'Litasov, Konstantin D.'
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501526.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501526.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_1501526
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501527.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501527.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_1501527
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_publ_author_name
'Litasov, Konstantin D.'
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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W W 0. 0. 0. 1.0 0.0
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|
1501528.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501528.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_1501528
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;
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W W 0. 0. 0. 1.0 0.0
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|
1501529.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501529.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_1501529
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;
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|
1501530.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501530.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_1501530
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Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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W W 0. 0. 0. 1.0 0.0
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|
1501531.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501531.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.
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data_1501531
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
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|
1501532.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501532.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
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# All data on this site have been placed in the public domain by the
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data_1501532
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;
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|
1501533.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501533.cif $
#------------------------------------------------------------------------------
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# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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|
1501534.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501534.cif $
#------------------------------------------------------------------------------
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# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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|
1501535.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501535.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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|
1501536.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501536.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
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# All data on this site have been placed in the public domain by the
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data_1501536
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|
1501537.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501537.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
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# All data on this site have been placed in the public domain by the
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|
1501538.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501538.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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|
1501539.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501539.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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data_1501539
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|
1501540.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501540.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
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# All data on this site have been placed in the public domain by the
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data_1501540
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;
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|
1501541.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501541.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
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# All data on this site have been placed in the public domain by the
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data_1501541
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;
Pressure-volume-temperature equation of state of tungsten carbide to 32
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;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.84648(9)
_cell_length_b 2.84648(9)
_cell_length_c 2.79542(12)
_cell_volume 19.6153(12)
_diffrn_ambient_pressure 26680000
_diffrn_ambient_temperature 673
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC70.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501541
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501542.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501542.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_1501542
loop_
_publ_author_name
'Litasov, Konstantin D.'
'Shatskiy, Anton'
'Fei, Yingwei'
'Suzuki, Akio'
'Ohtani, Eiji'
'Funakoshi, Kenichi'
_publ_section_title
;
Pressure-volume-temperature equation of state of tungsten carbide to 32
GPa and 1673 K
;
_journal_issue 5
_journal_name_full 'Journal of Applied Physics'
_journal_paper_doi 10.1063/1.3481667
_journal_volume 108
_journal_year 2010
_chemical_formula_structural WC
_chemical_formula_sum 'C W'
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 2.83895(9)
_cell_length_b 2.83895(9)
_cell_length_c 2.78842(18)
_cell_volume 19.4628(15)
_diffrn_ambient_pressure 30832500
_diffrn_ambient_temperature 673
_journal_article_reference 053513
_cod_data_source_file WC_P-6m2_DC71.cif
_cod_data_source_block chateigner_
_cod_original_formula_sum 'W C'
_cod_database_code 1501542
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
y-x,-x,-z
-y,x-y,+z
+x,+y,-z
y-x,-x,+z
-y,x-y,-z
y-x,+y,+z
+x,x-y,-z
-y,-x,+z
y-x,+y,-z
+x,x-y,+z
-y,-x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
W W 0. 0. 0. 1.0 0.0
C C 0.66667 0.3333 0.5 1.0 0.0
|
1501543.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501543.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_1501543
loop_
_publ_author_name
'Gagnon, Eric'
'Maris, Thierry'
'Wuest,James D'
_publ_section_title
;
Triarylamines Designed to Form Molecular Glasses. Derivatives of
Tris(p-terphenyl-4-yl)amine with Multiple Contiguous Phenyl Substituents
;
_journal_name_full 'Organic Letters'
_journal_page_first 404
_journal_page_last 407
_journal_paper_doi 10.1021/ol902841c
_journal_volume 12
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C126 H87 N, 13(C4 H8 O)'
_chemical_formula_sum 'C178 H191 N O13'
_chemical_formula_weight 2552.32
_chemical_name_systematic
;
?
;
_space_group_IT_number 7
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P -2yac'
_symmetry_space_group_name_H-M 'P 1 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
_cell_angle_beta 95.523(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 16.8098(13)
_cell_length_b 10.8804(9)
_cell_length_c 40.022(3)
_cell_measurement_reflns_used 24997
_cell_measurement_temperature 150
_cell_measurement_theta_max 49.49
_cell_measurement_theta_min 2.96
_cell_volume 7285.9(10)
_computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating A?de'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.071
_diffrn_reflns_av_sigmaI/netI 0.0351
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 111175
_diffrn_reflns_theta_full 55.74
_diffrn_reflns_theta_max 55.74
_diffrn_reflns_theta_min 2.76
_exptl_absorpt_coefficient_mu 0.556
_exptl_absorpt_correction_T_max 0.9618
_exptl_absorpt_correction_T_min 0.7951
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.163
_exptl_crystal_density_method '?t measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2740
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.550
_refine_diff_density_min -0.344
_refine_diff_density_rms 0.058
_refine_ls_abs_structure_details 'Friedel Pairs merged'
_refine_ls_extinction_method ?ne
_refine_ls_goodness_of_fit_ref 1.090
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1627
_refine_ls_number_reflns 9307
_refine_ls_number_restraints 1106
_refine_ls_restrained_S_all 1.071
_refine_ls_R_factor_all 0.0904
_refine_ls_R_factor_gt 0.0798
_refine_ls_shift/su_max 0.077
_refine_ls_shift/su_mean 0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1381P)^2^+5.4434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2068
_refine_ls_wR_factor_ref 0.2188
_reflns_number_gt 8139
_reflns_number_total 9307
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block gage42
_cod_original_cell_volume 7286.0(10)
_cod_original_sg_symbol_H-M Pn
_cod_database_code 1501543
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+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
C1 C 0.4023(5) 0.5553(6) 0.7542(2) 0.0458(15) Uani 1 1 d U . .
C2 C 0.4070(5) 0.6777(6) 0.7639(2) 0.0474(16) Uani 1 1 d U . .
H2 H 0.4571 0.7124 0.7718 0.057 Uiso 1 1 calc R . .
C3 C 0.3387(6) 0.7495(6) 0.7620(2) 0.0475(15) Uani 1 1 d U . .
H3 H 0.3425 0.8334 0.7685 0.057 Uiso 1 1 calc R . .
C4 C 0.2647(5) 0.7005(6) 0.7508(2) 0.0411(14) Uani 1 1 d U . .
C5 C 0.2616(5) 0.5802(7) 0.7387(2) 0.0473(16) Uani 1 1 d U . .
H5 H 0.2121 0.5468 0.7294 0.057 Uiso 1 1 calc R . .
C6 C 0.3299(6) 0.5094(6) 0.7401(2) 0.0458(15) Uani 1 1 d U . .
H6 H 0.3272 0.4282 0.7314 0.055 Uiso 1 1 calc R . .
C7 C 0.1894(5) 0.7700(6) 0.7562(2) 0.0419(14) Uani 1 1 d U . .
C8 C 0.1739(5) 0.7905(6) 0.7897(2) 0.0455(15) Uani 1 1 d U . .
C9 C 0.1042(5) 0.8519(6) 0.7968(2) 0.0449(15) Uani 1 1 d U . .
C10 C 0.0512(5) 0.8970(6) 0.7701(2) 0.0446(15) Uani 1 1 d U . .
C11 C 0.0674(5) 0.8795(6) 0.7369(2) 0.0435(15) Uani 1 1 d U . .
C12 C 0.1353(5) 0.8125(6) 0.7300(2) 0.0437(15) Uani 1 1 d U . .
C13 C 0.2302(5) 0.7438(6) 0.8183(2) 0.0444(15) Uani 1 1 d U . .
C14 C 0.2800(7) 0.8229(8) 0.8374(3) 0.073(2) Uani 1 1 d U . .
H14 H 0.2806 0.9078 0.8319 0.087 Uiso 1 1 calc R . .
C15 C 0.3297(7) 0.7782(10) 0.8649(3) 0.081(3) Uani 1 1 d U . .
H15 H 0.3623 0.8338 0.8784 0.097 Uiso 1 1 calc R . .
C16 C 0.3318(6) 0.6579(9) 0.8723(2) 0.070(2) Uani 1 1 d U . .
H16 H 0.3666 0.6287 0.8907 0.084 Uiso 1 1 calc R . .
C17 C 0.2845(6) 0.5783(9) 0.8536(3) 0.072(2) Uani 1 1 d U . .
H17 H 0.2861 0.4933 0.8591 0.086 Uiso 1 1 calc R . .
C18 C 0.2329(6) 0.6198(7) 0.8262(2) 0.0571(18) Uani 1 1 d U . .
H18 H 0.2000 0.5631 0.8132 0.069 Uiso 1 1 calc R . .
C19 C 0.0828(5) 0.8588(7) 0.8320(2) 0.0473(15) Uani 1 1 d U . .
C20 C 0.1137(7) 0.9486(8) 0.8548(2) 0.066(2) Uani 1 1 d U . .
H20 H 0.1478 1.0113 0.8478 0.079 Uiso 1 1 calc R . .
C21 C 0.0941(7) 0.9451(9) 0.8876(3) 0.076(2) Uani 1 1 d U . .
H21 H 0.1174 1.0032 0.9033 0.092 Uiso 1 1 calc R . .
C22 C 0.0419(6) 0.8598(10) 0.8977(3) 0.077(2) Uani 1 1 d U . .
H22 H 0.0281 0.8607 0.9202 0.093 Uiso 1 1 calc R . .
C23 C 0.0096(7) 0.7740(10) 0.8759(3) 0.082(3) Uani 1 1 d U . .
H23 H -0.0270 0.7150 0.8829 0.098 Uiso 1 1 calc R . .
C24 C 0.0309(6) 0.7735(9) 0.8430(2) 0.067(2) Uani 1 1 d U . .
H24 H 0.0089 0.7125 0.8278 0.080 Uiso 1 1 calc R . .
C25 C -0.0235(5) 0.9635(7) 0.7781(2) 0.0475(15) Uani 1 1 d U . .
C26 C -0.0190(6) 1.0803(7) 0.7923(3) 0.0625(19) Uani 1 1 d U . .
H26 H 0.0312 1.1201 0.7966 0.075 Uiso 1 1 calc R . .
C27 C -0.0878(7) 1.1379(9) 0.8002(3) 0.077(2) Uani 1 1 d U . .
H27 H -0.0848 1.2179 0.8097 0.092 Uiso 1 1 calc R . .
C28 C -0.1617(7) 1.0803(10) 0.7943(3) 0.077(2) Uani 1 1 d U . .
H28 H -0.2090 1.1206 0.7997 0.092 Uiso 1 1 calc R . .
C29 C -0.1654(6) 0.9670(10) 0.7810(3) 0.071(2) Uani 1 1 d U . .
H29 H -0.2156 0.9267 0.7773 0.086 Uiso 1 1 calc R . .
C30 C -0.0973(6) 0.9079(8) 0.7724(2) 0.0587(18) Uani 1 1 d U . .
H30 H -0.1015 0.8285 0.7625 0.070 Uiso 1 1 calc R . .
C31 C 0.0133(5) 0.9351(7) 0.7090(2) 0.0489(16) Uani 1 1 d U . .
C32 C 0.0162(6) 1.0576(7) 0.7029(2) 0.0580(18) Uani 1 1 d U . .
H32 H 0.0517 1.1078 0.7168 0.070 Uiso 1 1 calc R . .
C33 C -0.0320(7) 1.1107(9) 0.6766(3) 0.079(2) Uani 1 1 d U . .
H33 H -0.0282 1.1963 0.6723 0.095 Uiso 1 1 calc R . .
C34 C -0.0854(7) 1.0392(10) 0.6566(3) 0.083(3) Uani 1 1 d U . .
H34 H -0.1199 1.0755 0.6391 0.099 Uiso 1 1 calc R . .
C35 C -0.0877(7) 0.9156(10) 0.6623(3) 0.083(3) Uani 1 1 d U . .
H35 H -0.1231 0.8660 0.6482 0.099 Uiso 1 1 calc R . .
C36 C -0.0399(6) 0.8606(8) 0.6883(2) 0.0598(19) Uani 1 1 d U . .
H36 H -0.0428 0.7747 0.6922 0.072 Uiso 1 1 calc R . .
C37 C 0.1488(5) 0.7945(7) 0.6934(2) 0.0455(15) Uani 1 1 d U . .
C38 C 0.1741(6) 0.8912(8) 0.6752(2) 0.0587(18) Uani 1 1 d U . .
H38 H 0.1892 0.9660 0.6863 0.070 Uiso 1 1 calc R . .
C39 C 0.1779(6) 0.8816(9) 0.6409(3) 0.069(2) Uani 1 1 d U . .
H39 H 0.1955 0.9494 0.6286 0.083 Uiso 1 1 calc R . .
C40 C 0.1559(6) 0.7735(10) 0.6246(2) 0.074(2) Uani 1 1 d U . .
H40 H 0.1568 0.7671 0.6009 0.089 Uiso 1 1 calc R . .
C41 C 0.1332(6) 0.6770(9) 0.6425(2) 0.067(2) Uani 1 1 d U . .
H41 H 0.1207 0.6014 0.6314 0.081 Uiso 1 1 calc R . .
C42 C 0.1276(6) 0.6847(7) 0.6772(2) 0.0566(18) Uani 1 1 d U . .
H42 H 0.1096 0.6165 0.6893 0.068 Uiso 1 1 calc R . .
C43 C 0.5090(5) 0.4577(6) 0.7911(2) 0.0444(15) Uani 1 1 d U . .
C44 C 0.4744(5) 0.4976(6) 0.8196(2) 0.0448(15) Uani 1 1 d U . .
H44 H 0.4239 0.5377 0.8171 0.054 Uiso 1 1 calc R . .
C45 C 0.5129(5) 0.4794(6) 0.8515(2) 0.0451(15) Uani 1 1 d U . .
H45 H 0.4884 0.5084 0.8704 0.054 Uiso 1 1 calc R . .
C46 C 0.5857(5) 0.4204(6) 0.8565(2) 0.0417(14) Uani 1 1 d U . .
C47 C 0.6194(5) 0.3782(6) 0.8282(2) 0.0432(15) Uani 1 1 d U . .
H47 H 0.6689 0.3355 0.8310 0.052 Uiso 1 1 calc R . .
C48 C 0.5826(5) 0.3971(7) 0.7963(2) 0.0489(16) Uani 1 1 d U . .
H48 H 0.6077 0.3683 0.7775 0.059 Uiso 1 1 calc R . .
C49 C 0.6260(5) 0.4077(6) 0.8915(2) 0.0401(14) Uani 1 1 d U . .
C50 C 0.7032(5) 0.4591(6) 0.8989(2) 0.0415(14) Uani 1 1 d U . .
C51 C 0.7386(5) 0.4576(6) 0.9325(2) 0.0417(14) Uani 1 1 d U . .
C52 C 0.6972(5) 0.4045(6) 0.9579(2) 0.0413(14) Uani 1 1 d U . .
C53 C 0.6220(5) 0.3547(6) 0.9505(2) 0.0423(14) Uani 1 1 d U . .
C54 C 0.5856(5) 0.3544(6) 0.9169(2) 0.0415(14) Uani 1 1 d U . .
C55 C 0.7467(5) 0.5178(6) 0.8727(2) 0.0454(15) Uani 1 1 d U . .
C56 C 0.7215(6) 0.6278(7) 0.8579(2) 0.0613(19) Uani 1 1 d U . .
H56 H 0.6751 0.6669 0.8646 0.074 Uiso 1 1 calc R . .
C57 C 0.7625(7) 0.6817(9) 0.8336(3) 0.077(2) Uani 1 1 d U . .
H57 H 0.7451 0.7583 0.8241 0.092 Uiso 1 1 calc R . .
C58 C 0.8277(7) 0.6254(10) 0.8231(3) 0.079(2) Uani 1 1 d U . .
H58 H 0.8547 0.6608 0.8057 0.095 Uiso 1 1 calc R . .
C59 C 0.8545(7) 0.5185(10) 0.8376(3) 0.079(2) Uani 1 1 d U . .
H59 H 0.9017 0.4813 0.8309 0.095 Uiso 1 1 calc R . .
C60 C 0.8140(6) 0.4637(8) 0.8618(2) 0.0579(18) Uani 1 1 d U . .
H60 H 0.8325 0.3874 0.8712 0.069 Uiso 1 1 calc R . .
C61 C 0.8192(6) 0.5131(7) 0.9412(2) 0.0465(15) Uani 1 1 d U . .
C62 C 0.8304(6) 0.6389(7) 0.9400(2) 0.0539(17) Uani 1 1 d U . .
H62 H 0.7869 0.6897 0.9317 0.065 Uiso 1 1 calc R . .
C63 C 0.9041(6) 0.6934(9) 0.9505(2) 0.069(2) Uani 1 1 d U . .
H63 H 0.9105 0.7801 0.9500 0.083 Uiso 1 1 calc R . .
C64 C 0.9674(6) 0.6175(10) 0.9618(3) 0.074(2) Uani 1 1 d U . .
H64 H 1.0178 0.6528 0.9691 0.088 Uiso 1 1 calc R . .
C65 C 0.9582(6) 0.4927(10) 0.9624(3) 0.074(2) Uani 1 1 d U . .
H65 H 1.0024 0.4417 0.9696 0.089 Uiso 1 1 calc R . .
C66 C 0.8847(6) 0.4406(8) 0.9525(2) 0.0574(18) Uani 1 1 d U . .
H66 H 0.8786 0.3539 0.9535 0.069 Uiso 1 1 calc R . .
C67 C 0.7349(5) 0.4056(6) 0.9936(2) 0.0426(14) Uani 1 1 d U . .
C68 C 0.7467(6) 0.5166(7) 1.0109(2) 0.0523(17) Uani 1 1 d U . .
H68 H 0.7320 0.5914 0.9998 0.063 Uiso 1 1 calc R . .
C69 C 0.7791(6) 0.5198(7) 1.0437(2) 0.0595(19) Uani 1 1 d U . .
H69 H 0.7857 0.5959 1.0553 0.071 Uiso 1 1 calc R . .
C70 C 0.8019(6) 0.4119(7) 1.0596(2) 0.0570(19) Uani 1 1 d U . .
H70 H 0.8251 0.4136 1.0822 0.068 Uiso 1 1 calc R . .
C71 C 0.7916(6) 0.3018(7) 1.0433(2) 0.0528(17) Uani 1 1 d U . .
H71 H 0.8076 0.2277 1.0545 0.063 Uiso 1 1 calc R . .
C72 C 0.7576(5) 0.2985(7) 1.0101(2) 0.0470(15) Uani 1 1 d U . .
H72 H 0.7501 0.2219 0.9988 0.056 Uiso 1 1 calc R . .
C73 C 0.5788(5) 0.3035(6) 0.9784(2) 0.0465(15) Uani 1 1 d U . .
C74 C 0.5546(6) 0.3805(8) 1.0026(2) 0.0625(19) Uani 1 1 d U . .
H74 H 0.5612 0.4667 1.0003 0.075 Uiso 1 1 calc R . .
C75 C 0.5203(6) 0.3346(9) 1.0305(3) 0.071(2) Uani 1 1 d U . .
H75 H 0.5034 0.3889 1.0471 0.085 Uiso 1 1 calc R . .
C76 C 0.5116(6) 0.2105(9) 1.0336(3) 0.070(2) Uani 1 1 d U . .
H76 H 0.4895 0.1786 1.0528 0.084 Uiso 1 1 calc R . .
C77 C 0.5343(6) 0.1304(8) 1.0096(3) 0.0630(19) Uani 1 1 d U . .
H77 H 0.5276 0.0442 1.0120 0.076 Uiso 1 1 calc R . .
C78 C 0.5671(5) 0.1782(7) 0.9818(2) 0.0532(17) Uani 1 1 d U . .
H78 H 0.5817 0.1240 0.9648 0.064 Uiso 1 1 calc R . .
C79 C 0.5064(5) 0.2971(7) 0.9088(2) 0.0478(15) Uani 1 1 d U . .
C80 C 0.4370(6) 0.3455(8) 0.9204(2) 0.0587(18) Uani 1 1 d U . .
H80 H 0.4408 0.4168 0.9342 0.070 Uiso 1 1 calc R . .
C81 C 0.3637(6) 0.2923(10) 0.9125(3) 0.073(2) Uani 1 1 d U . .
H81 H 0.3173 0.3275 0.9204 0.087 Uiso 1 1 calc R . .
C82 C 0.3574(7) 0.1869(11) 0.8929(3) 0.087(3) Uani 1 1 d U . .
H82 H 0.3066 0.1501 0.8872 0.104 Uiso 1 1 calc R . .
C83 C 0.4232(7) 0.1370(10) 0.8818(3) 0.085(3) Uani 1 1 d U . .
H83 H 0.4183 0.0641 0.8687 0.102 Uiso 1 1 calc R . .
C84 C 0.4988(6) 0.1904(8) 0.8893(3) 0.0641(19) Uani 1 1 d U . .
H84 H 0.5446 0.1542 0.8811 0.077 Uiso 1 1 calc R . .
C85 C 0.4860(5) 0.4028(6) 0.7309(2) 0.0425(15) Uani 1 1 d U . .
C86 C 0.4923(6) 0.4590(6) 0.7004(2) 0.0495(16) Uani 1 1 d U . .
H86 H 0.4913 0.5461 0.6989 0.059 Uiso 1 1 calc R . .
C87 C 0.5000(5) 0.3896(6) 0.6720(2) 0.0469(16) Uani 1 1 d U . .
H87 H 0.5042 0.4297 0.6512 0.056 Uiso 1 1 calc R . .
C88 C 0.5017(5) 0.2646(6) 0.6734(2) 0.0385(14) Uani 1 1 d U . .
C89 C 0.4992(6) 0.2073(6) 0.7041(2) 0.0495(16) Uani 1 1 d U . .
H89 H 0.5031 0.1203 0.7057 0.059 Uiso 1 1 calc R . .
C90 C 0.4907(6) 0.2776(7) 0.7328(2) 0.0489(16) Uani 1 1 d U . .
H90 H 0.4882 0.2379 0.7538 0.059 Uiso 1 1 calc R . .
C91 C 0.4329(5) 0.1783(6) 0.6204(2) 0.0385(13) Uani 1 1 d U . .
C92 C 0.4352(5) 0.1206(6) 0.5890(2) 0.0407(14) Uani 1 1 d U . .
C93 C 0.5079(5) 0.0768(6) 0.5797(2) 0.0393(14) Uani 1 1 d U . .
C94 C 0.5781(5) 0.0882(6) 0.6010(2) 0.0420(14) Uani 1 1 d U . .
C95 C 0.5767(5) 0.1443(6) 0.6325(2) 0.0439(15) Uani 1 1 d U . .
C96 C 0.5041(5) 0.1923(6) 0.6415(2) 0.0419(14) Uani 1 1 d U . .
C97 C 0.3582(5) 0.2310(6) 0.6317(2) 0.0410(14) Uani 1 1 d U . .
C98 C 0.3332(5) 0.3488(7) 0.6224(2) 0.0522(17) Uani 1 1 d U . .
H98 H 0.3610 0.3931 0.6067 0.063 Uiso 1 1 calc R . .
C99 C 0.2697(6) 0.4018(7) 0.6352(3) 0.0605(19) Uani 1 1 d U . .
H99 H 0.2536 0.4821 0.6281 0.073 Uiso 1 1 calc R . .
C100 C 0.2287(6) 0.3427(7) 0.6580(2) 0.0572(18) Uani 1 1 d U . .
H100 H 0.1853 0.3819 0.6672 0.069 Uiso 1 1 calc R . .
C101 C 0.2507(6) 0.2254(7) 0.6675(2) 0.0586(18) Uani 1 1 d U . .
H101 H 0.2215 0.1819 0.6829 0.070 Uiso 1 1 calc R . .
C102 C 0.3158(6) 0.1703(7) 0.6547(2) 0.0557(18) Uani 1 1 d U . .
H102 H 0.3314 0.0897 0.6618 0.067 Uiso 1 1 calc R . .
C103 C 0.3610(5) 0.1060(6) 0.5659(2) 0.0411(14) Uani 1 1 d U . .
C104 C 0.3521(6) 0.1642(6) 0.5347(2) 0.0463(16) Uani 1 1 d U . .
H104 H 0.3930 0.2175 0.5285 0.056 Uiso 1 1 calc R . .
C105 C 0.2840(6) 0.1457(6) 0.5124(2) 0.0486(16) Uani 1 1 d U . .
H105 H 0.2788 0.1868 0.4914 0.058 Uiso 1 1 calc R . .
C106 C 0.2239(5) 0.0672(7) 0.5209(2) 0.0519(17) Uani 1 1 d U . .
H106 H 0.1779 0.0531 0.5056 0.062 Uiso 1 1 calc R . .
C107 C 0.2321(6) 0.0099(7) 0.5520(2) 0.0544(17) Uani 1 1 d U . .
H107 H 0.1913 -0.0439 0.5580 0.065 Uiso 1 1 calc R . .
C108 C 0.2987(5) 0.0301(7) 0.5743(2) 0.0480(16) Uani 1 1 d U . .
H108 H 0.3023 -0.0082 0.5958 0.058 Uiso 1 1 calc R . .
C109 C 0.5112(5) 0.0162(7) 0.5454(2) 0.0453(15) Uani 1 1 d U . .
C110 C 0.5525(6) 0.0723(8) 0.5214(2) 0.0575(18) Uani 1 1 d U . .
H110 H 0.5799 0.1475 0.5263 0.069 Uiso 1 1 calc R . .
C111 C 0.5539(6) 0.0186(11) 0.4903(2) 0.076(2) Uani 1 1 d U . .
H111 H 0.5840 0.0552 0.4740 0.092 Uiso 1 1 calc R . .
C112 C 0.5120(7) -0.0873(12) 0.4827(3) 0.086(3) Uani 1 1 d U . .
H112 H 0.5112 -0.1213 0.4609 0.104 Uiso 1 1 calc R . .
C113 C 0.4727(7) -0.1428(9) 0.5055(3) 0.078(2) Uani 1 1 d U . .
H113 H 0.4450 -0.2173 0.4999 0.093 Uiso 1 1 calc R . .
C114 C 0.4713(6) -0.0925(7) 0.5380(2) 0.0554(17) Uani 1 1 d U . .
H114 H 0.4434 -0.1328 0.5544 0.066 Uiso 1 1 calc R . .
C115 C 0.6568(5) 0.0385(6) 0.5913(2) 0.0461(15) Uani 1 1 d U . .
C116 C 0.7157(6) 0.1180(8) 0.5836(3) 0.0587(18) Uani 1 1 d U . .
H116 H 0.7069 0.2041 0.5843 0.070 Uiso 1 1 calc R . .
C117 C 0.7887(6) 0.0731(10) 0.5747(3) 0.071(2) Uani 1 1 d U . .
H117 H 0.8283 0.1287 0.5685 0.086 Uiso 1 1 calc R . .
C118 C 0.8031(6) -0.0497(10) 0.5747(3) 0.074(2) Uani 1 1 d U . .
H118 H 0.8532 -0.0798 0.5692 0.088 Uiso 1 1 calc R . .
C119 C 0.7456(6) -0.1294(9) 0.5827(3) 0.075(2) Uani 1 1 d U . .
H119 H 0.7555 -0.2154 0.5824 0.090 Uiso 1 1 calc R . .
C120 C 0.6716(6) -0.0862(7) 0.5914(3) 0.0614(19) Uani 1 1 d U . .
H120 H 0.6320 -0.1424 0.5973 0.074 Uiso 1 1 calc R . .
C121 C 0.6494(5) 0.1534(7) 0.6568(2) 0.0465(15) Uani 1 1 d U . .
C122 C 0.6886(6) 0.2615(8) 0.6639(3) 0.067(2) Uani 1 1 d U . .
H122 H 0.6719 0.3335 0.6518 0.081 Uiso 1 1 calc R . .
C123 C 0.7524(6) 0.2681(10) 0.6886(3) 0.080(2) Uani 1 1 d U . .
H123 H 0.7787 0.3444 0.6931 0.096 Uiso 1 1 calc R . .
C124 C 0.7777(6) 0.1658(11) 0.7064(3) 0.082(2) Uani 1 1 d U . .
H124 H 0.8206 0.1713 0.7236 0.098 Uiso 1 1 calc R . .
C125 C 0.7411(7) 0.0567(10) 0.6994(3) 0.082(3) Uani 1 1 d U . .
H125 H 0.7592 -0.0158 0.7110 0.098 Uiso 1 1 calc R . .
C126 C 0.6759(4) 0.0525(4) 0.67465(18) 0.070(2) Uani 1 1 d U . .
H126 H 0.6493 -0.0236 0.6702 0.084 Uiso 1 1 calc R . .
N1 N 0.4723(4) 0.4766(4) 0.75875(18) 0.0485(14) Uani 1 1 d RU . .
O1 O 0.4227(4) 0.6578(4) 0.63848(18) 0.080(4) Uiso 0.61(2) 1 d PRDU B 1
C127 C 0.4706(4) 0.7591(4) 0.63020(18) 0.114(7) Uiso 0.61(2) 1 d PRDU B 1
H12A H 0.4519 0.7897 0.6075 0.136 Uiso 0.61(2) 1 calc PR B 1
H12B H 0.5269 0.7323 0.6300 0.136 Uiso 0.61(2) 1 calc PR B 1
C128 C 0.4654(11) 0.8621(10) 0.6559(4) 0.100(6) Uiso 0.61(2) 1 d PDU B 1
H12C H 0.4442 0.9387 0.6451 0.120 Uiso 0.61(2) 1 calc PR B 1
H12D H 0.5182 0.8791 0.6682 0.120 Uiso 0.61(2) 1 calc PR B 1
C129 C 0.4069(12) 0.8081(13) 0.6794(4) 0.089(6) Uiso 0.61(2) 1 d PDU B 1
H12E H 0.4355 0.7835 0.7011 0.107 Uiso 0.61(2) 1 calc PR B 1
H12F H 0.3652 0.8690 0.6837 0.107 Uiso 0.61(2) 1 calc PR B 1
C130 C 0.3717(8) 0.7025(11) 0.6619(4) 0.077(5) Uiso 0.61(2) 1 d PDU B 1
H13A H 0.3625 0.6370 0.6782 0.092 Uiso 0.61(2) 1 calc PR B 1
H13B H 0.3195 0.7255 0.6500 0.092 Uiso 0.61(2) 1 calc PR B 1
O1A O 0.3708(15) 0.711(3) 0.6436(8) 0.172(13) Uiso 0.39(2) 1 d PDU B 2
C227 C 0.4469(19) 0.698(3) 0.6316(9) 0.175(17) Uiso 0.39(2) 1 d PDU B 2
H22A H 0.4420 0.7045 0.6068 0.210 Uiso 0.39(2) 1 calc PR B 2
H22B H 0.4698 0.6166 0.6380 0.210 Uiso 0.39(2) 1 calc PR B 2
C228 C 0.5016(15) 0.800(3) 0.6471(8) 0.137(14) Uiso 0.39(2) 1 d PDU B 2
H22C H 0.5020 0.8725 0.6320 0.164 Uiso 0.39(2) 1 calc PR B 2
H22D H 0.5570 0.7708 0.6526 0.164 Uiso 0.39(2) 1 calc PR B 2
C229 C 0.4610(17) 0.831(3) 0.6790(7) 0.139(15) Uiso 0.39(2) 1 d PDU B 2
H22E H 0.4900 0.7918 0.6989 0.167 Uiso 0.39(2) 1 calc PR B 2
H22F H 0.4595 0.9207 0.6827 0.167 Uiso 0.39(2) 1 calc PR B 2
C230 C 0.3812(14) 0.782(3) 0.6731(7) 0.094(10) Uiso 0.39(2) 1 d PDU B 2
H23A H 0.3698 0.7305 0.6925 0.112 Uiso 0.39(2) 1 calc PR B 2
H23B H 0.3425 0.8509 0.6714 0.112 Uiso 0.39(2) 1 calc PR B 2
O2 O 0.651(2) 0.662(2) 0.7390(7) 0.206(8) Uiso 0.643(15) 1 d PDU C 1
C131 C 0.6413(14) 0.729(2) 0.7078(6) 0.126(6) Uiso 0.643(15) 1 d PDU C 1
H13C H 0.6468 0.8182 0.7121 0.152 Uiso 0.643(15) 1 calc PR C 1
H13D H 0.5878 0.7133 0.6959 0.152 Uiso 0.643(15) 1 calc PR C 1
C132 C 0.7037(16) 0.687(3) 0.6873(7) 0.156(9) Uiso 0.643(15) 1 d PDU C 1
H13E H 0.7296 0.7578 0.6774 0.187 Uiso 0.643(15) 1 calc PR C 1
H13F H 0.6804 0.6331 0.6690 0.187 Uiso 0.643(15) 1 calc PR C 1
C133 C 0.7647(14) 0.615(2) 0.7106(6) 0.136(7) Uiso 0.643(15) 1 d PDU C 1
H13G H 0.7890 0.5480 0.6985 0.163 Uiso 0.643(15) 1 calc PR C 1
H13H H 0.8075 0.6702 0.7207 0.163 Uiso 0.643(15) 1 calc PR C 1
C134 C 0.7162(17) 0.567(2) 0.7363(7) 0.138(8) Uiso 0.643(15) 1 d PDU C 1
H13I H 0.7489 0.5578 0.7581 0.166 Uiso 0.643(15) 1 calc PR C 1
H13J H 0.6931 0.4863 0.7294 0.166 Uiso 0.643(15) 1 calc PR C 1
O2A O 0.668(3) 0.650(4) 0.7460(12) 0.206(8) Uiso 0.357(15) 1 d PDU C 2
C231 C 0.689(2) 0.758(3) 0.7277(10) 0.126(6) Uiso 0.357(15) 1 d PDU C 2
H23C H 0.7135 0.8204 0.7432 0.152 Uiso 0.357(15) 1 calc PR C 2
H23D H 0.6403 0.7932 0.7153 0.152 Uiso 0.357(15) 1 calc PR C 2
C232 C 0.745(3) 0.717(3) 0.7043(11) 0.156(9) Uiso 0.357(15) 1 d PDU C 2
H23E H 0.8009 0.7268 0.7145 0.187 Uiso 0.357(15) 1 calc PR C 2
H23F H 0.7384 0.7655 0.6833 0.187 Uiso 0.357(15) 1 calc PR C 2
C233 C 0.727(3) 0.581(3) 0.6971(9) 0.136(7) Uiso 0.357(15) 1 d PDU C 2
H23G H 0.6861 0.5722 0.6776 0.163 Uiso 0.357(15) 1 calc PR C 2
H23H H 0.7756 0.5360 0.6925 0.163 Uiso 0.357(15) 1 calc PR C 2
C234 C 0.696(3) 0.538(3) 0.7280(11) 0.138(8) Uiso 0.357(15) 1 d PDU C 2
H23I H 0.7387 0.4944 0.7423 0.166 Uiso 0.357(15) 1 calc PR C 2
H23J H 0.6512 0.4798 0.7227 0.166 Uiso 0.357(15) 1 calc PR C 2
O3 O 0.4806(9) 0.6799(13) 0.9486(4) 0.134(4) Uiso 0.579(9) 1 d PDU D 1
C135 C 0.4595(12) 0.8044(15) 0.9529(6) 0.129(6) Uiso 0.579(9) 1 d PDU D 1
H13K H 0.4574 0.8220 0.9771 0.155 Uiso 0.579(9) 1 calc PR D 1
H13L H 0.4059 0.8204 0.9412 0.155 Uiso 0.579(9) 1 calc PR D 1
C136 C 0.521(2) 0.8883(13) 0.9387(12) 0.27(2) Uiso 0.579(9) 1 d PDU D 1
H13M H 0.5534 0.9337 0.9567 0.328 Uiso 0.579(9) 1 calc PR D 1
H13N H 0.4957 0.9477 0.9223 0.328 Uiso 0.579(9) 1 calc PR D 1
C137 C 0.5731(15) 0.7947(19) 0.9215(7) 0.162(9) Uiso 0.579(9) 1 d PDU D 1
H13O H 0.5574 0.7913 0.8970 0.195 Uiso 0.579(9) 1 calc PR D 1
H13P H 0.6305 0.8163 0.9253 0.195 Uiso 0.579(9) 1 calc PR D 1
C138 C 0.5574(9) 0.6790(13) 0.9372(4) 0.078(4) Uiso 0.579(9) 1 d PDU D 1
H13Q H 0.5612 0.6113 0.9209 0.094 Uiso 0.579(9) 1 calc PR D 1
H13R H 0.5981 0.6647 0.9564 0.094 Uiso 0.579(9) 1 calc PR D 1
O3A O 0.5373(13) 0.8540(19) 0.9686(4) 0.134(4) Uiso 0.421(9) 1 d PDU D 2
C235 C 0.5785(18) 0.740(2) 0.9678(6) 0.129(6) Uiso 0.421(9) 1 d PDU D 2
H23K H 0.5445 0.6725 0.9748 0.155 Uiso 0.421(9) 1 calc PR D 2
H23L H 0.6281 0.7426 0.9833 0.155 Uiso 0.421(9) 1 calc PR D 2
C236 C 0.599(2) 0.720(4) 0.9315(8) 0.27(2) Uiso 0.421(9) 1 d PDU D 2
H23M H 0.5938 0.6319 0.9251 0.328 Uiso 0.421(9) 1 calc PR D 2
H23N H 0.6532 0.7489 0.9283 0.328 Uiso 0.421(9) 1 calc PR D 2
C237 C 0.534(2) 0.799(3) 0.9116(5) 0.162(9) Uiso 0.421(9) 1 d PDU D 2
H23O H 0.5588 0.8528 0.8956 0.195 Uiso 0.421(9) 1 calc PR D 2
H23P H 0.4940 0.7457 0.8990 0.195 Uiso 0.421(9) 1 calc PR D 2
C238 C 0.4979(13) 0.871(2) 0.9363(5) 0.078(4) Uiso 0.421(9) 1 d PDU D 2
H23Q H 0.4996 0.9587 0.9301 0.094 Uiso 0.421(9) 1 calc PR D 2
H23R H 0.4411 0.8465 0.9363 0.094 Uiso 0.421(9) 1 calc PR D 2
O4 O 0.2015(9) 0.1708(17) 0.7961(5) 0.171(7) Uani 0.763(19) 1 d PU E 1
C139 C 0.2215(9) 0.1338(16) 0.7655(4) 0.133(5) Uani 1 1 d U E 1
H13S H 0.1985 0.1921 0.7482 0.159 Uiso 1 1 calc R E 1
H13T H 0.1977 0.0520 0.7603 0.159 Uiso 1 1 calc R E 1
C140 C 0.3020(10) 0.1271(15) 0.7639(4) 0.137(5) Uani 1 1 d DU E 1
H14A H 0.3173 0.1623 0.7427 0.164 Uiso 1 1 calc R E 1
H14B H 0.3210 0.0411 0.7660 0.164 Uiso 1 1 calc R E 1
C141 C 0.3355(10) 0.2051(17) 0.7945(3) 0.161(6) Uani 1 1 d DU E 1
H14C H 0.3626 0.1534 0.8125 0.193 Uiso 1 1 calc R E 1
H14D H 0.3730 0.2691 0.7880 0.193 Uiso 1 1 calc R E 1
C142 C 0.2597(13) 0.2599(15) 0.8047(5) 0.158(5) Uani 1 1 d U E 1
H14E H 0.2642 0.2765 0.8292 0.189 Uiso 1 1 calc R E 1
H14F H 0.2469 0.3376 0.7925 0.189 Uiso 1 1 calc R E 1
O4A O 0.3518(18) 0.091(2) 0.7808(7) 0.074(10) Uiso 0.237(19) 1 d P E 2
O5 O 0.0270(9) 0.3477(12) 0.8508(3) 0.136(4) Uiso 0.676(11) 1 d PDU F 1
C143 C 0.0106(10) 0.2696(15) 0.8777(4) 0.156(8) Uiso 0.676(11) 1 d PDU F 1
H14G H 0.0109 0.1826 0.8705 0.187 Uiso 0.676(11) 1 calc PR F 1
H14H H -0.0425 0.2888 0.8851 0.187 Uiso 0.676(11) 1 calc PR F 1
C144 C 0.0769(12) 0.2925(16) 0.9066(4) 0.138(7) Uiso 0.676(11) 1 d PDU F 1
H14I H 0.1218 0.2339 0.9058 0.166 Uiso 0.676(11) 1 calc PR F 1
H14J H 0.0559 0.2870 0.9288 0.166 Uiso 0.676(11) 1 calc PR F 1
C145 C 0.1024(19) 0.4254(19) 0.8988(5) 0.247(14) Uiso 0.676(11) 1 d PDU F 1
H14K H 0.0845 0.4835 0.9156 0.297 Uiso 0.676(11) 1 calc PR F 1
H14L H 0.1612 0.4311 0.8991 0.297 Uiso 0.676(11) 1 calc PR F 1
C146 C 0.0644(11) 0.4528(9) 0.8658(2) 0.306(19) Uiso 0.676(11) 1 d PDU F 1
H14M H 0.0241 0.5182 0.8676 0.367 Uiso 0.676(11) 1 calc PR F 1
H14N H 0.1049 0.4837 0.8515 0.367 Uiso 0.676(11) 1 calc PR F 1
O5A O 0.0855(11) 0.3982(9) 0.8464(2) 0.136(4) Uiso 0.324(11) 1 d PRDU F 2
C243 C 0.0903(11) 0.2760(9) 0.8586(2) 0.156(8) Uiso 0.324(11) 1 d PRDU F 2
H24G H 0.1140 0.2216 0.8424 0.187 Uiso 0.324(11) 1 calc PR F 2
H24H H 0.0364 0.2447 0.8620 0.187 Uiso 0.324(11) 1 calc PR F 2
C244 C 0.1437(15) 0.2789(14) 0.8923(5) 0.138(7) Uiso 0.324(11) 1 d PDU F 2
H24I H 0.2005 0.2631 0.8891 0.166 Uiso 0.324(11) 1 calc PR F 2
H24J H 0.1255 0.2187 0.9085 0.166 Uiso 0.324(11) 1 calc PR F 2
C245 C 0.1306(18) 0.4129(16) 0.9037(5) 0.247(14) Uiso 0.324(11) 1 d PDU F 2
H24K H 0.1816 0.4592 0.9060 0.297 Uiso 0.324(11) 1 calc PR F 2
H24L H 0.1068 0.4149 0.9254 0.297 Uiso 0.324(11) 1 calc PR F 2
C246 C 0.0721(7) 0.4660(9) 0.8750(2) 0.306(19) Uiso 0.324(11) 1 d PDU F 2
H24M H 0.0161 0.4566 0.8803 0.367 Uiso 0.324(11) 1 calc PR F 2
H24N H 0.0830 0.5543 0.8716 0.367 Uiso 0.324(11) 1 calc PR F 2
O6 O 0.5280(7) 0.9543(9) 0.7765(2) 0.171(6) Uiso 0.577(11) 1 d PRDU G 1
C147 C 0.6024(7) 1.0149(9) 0.7773(2) 0.101(5) Uiso 0.577(11) 1 d PRDU G 1
H14O H 0.5937 1.1041 0.7737 0.122 Uiso 0.577(11) 1 calc PR G 1
H14P H 0.6325 0.9832 0.7590 0.122 Uiso 0.577(11) 1 calc PR G 1
C148 C 0.6507(8) 0.993(2) 0.8113(3) 0.116(6) Uiso 0.577(11) 1 d PDU G 1
H14Q H 0.6732 1.0713 0.8209 0.139 Uiso 0.577(11) 1 calc PR G 1
H14R H 0.6945 0.9339 0.8093 0.139 Uiso 0.577(11) 1 calc PR G 1
C149 C 0.5866(10) 0.941(3) 0.8324(3) 0.153(8) Uiso 0.577(11) 1 d PDU G 1
H14S H 0.6084 0.8720 0.8465 0.184 Uiso 0.577(11) 1 calc PR G 1
H14T H 0.5669 1.0053 0.8471 0.184 Uiso 0.577(11) 1 calc PR G 1
C150 C 0.5234(14) 0.899(3) 0.8082(4) 0.26(2) Uiso 0.577(11) 1 d PDU G 1
H15A H 0.5268 0.8089 0.8059 0.307 Uiso 0.577(11) 1 calc PR G 1
H15B H 0.4711 0.9191 0.8163 0.307 Uiso 0.577(11) 1 calc PR G 1
O6A O 0.5114(11) 0.918(2) 0.8202(8) 0.171(6) Uiso 0.423(11) 1 d PDU G 2
C247 C 0.5813(13) 0.8477(18) 0.8177(7) 0.101(5) Uiso 0.423(11) 1 d PDU G 2
H24A H 0.5673 0.7692 0.8061 0.122 Uiso 0.423(11) 1 calc PR G 2
H24B H 0.6067 0.8286 0.8404 0.122 Uiso 0.423(11) 1 calc PR G 2
C248 C 0.6398(13) 0.920(2) 0.7981(8) 0.116(6) Uiso 0.423(11) 1 d PDU G 2
H24C H 0.6411 0.8871 0.7751 0.139 Uiso 0.423(11) 1 calc PR G 2
H24D H 0.6945 0.9186 0.8097 0.139 Uiso 0.423(11) 1 calc PR G 2
C249 C 0.6036(19) 1.0501(19) 0.7977(10) 0.153(8) Uiso 0.423(11) 1 d PDU G 2
H24E H 0.6328 1.1026 0.8149 0.184 Uiso 0.423(11) 1 calc PR G 2
H24F H 0.6057 1.0891 0.7754 0.184 Uiso 0.423(11) 1 calc PR G 2
C250 C 0.5221(18) 1.032(3) 0.8049(13) 0.26(2) Uiso 0.423(11) 1 d PDU G 2
H25A H 0.5069 1.0988 0.8200 0.307 Uiso 0.423(11) 1 calc PR G 2
H25B H 0.4865 1.0377 0.7838 0.307 Uiso 0.423(11) 1 calc PR G 2
O7 O 0.2100(6) 0.1230(8) 0.9519(3) 0.109(2) Uani 1 1 d U H 1
C151 C 0.2184(8) 0.2089(15) 0.9787(4) 0.121(3) Uani 1 1 d U H 1
H15C H 0.1828 0.1868 0.9961 0.145 Uiso 1 1 calc R H 1
H15D H 0.2045 0.2927 0.9705 0.145 Uiso 1 1 calc R H 1
C152 C 0.3060(8) 0.2038(16) 0.9933(3) 0.120(3) Uani 1 1 d U H 1
H15E H 0.3385 0.2672 0.9832 0.144 Uiso 1 1 calc R H 1
H15F H 0.3112 0.2137 1.0180 0.144 Uiso 1 1 calc R H 1
C153 C 0.3285(10) 0.0791(19) 0.9835(4) 0.152(5) Uani 1 1 d U H 1
H15G H 0.3404 0.0274 1.0037 0.182 Uiso 1 1 calc R H 1
H15H H 0.3769 0.0826 0.9712 0.182 Uiso 1 1 calc R H 1
C154 C 0.2613(9) 0.0260(14) 0.9617(5) 0.137(4) Uani 1 1 d U H 1
H15I H 0.2811 -0.0136 0.9418 0.164 Uiso 1 1 calc R H 1
H15J H 0.2331 -0.0365 0.9741 0.164 Uiso 1 1 calc R H 1
O8 O -0.0095(8) 0.1804(13) 0.5509(3) 0.179(5) Uani 1 1 d U I 1
C155 C 0.0273(9) 0.1201(13) 0.5794(3) 0.111(3) Uani 1 1 d U I 1
H15K H 0.0565 0.0461 0.5729 0.133 Uiso 1 1 calc R I 1
H15L H -0.0127 0.0953 0.5947 0.133 Uiso 1 1 calc R I 1
C156 C 0.0847(9) 0.2147(12) 0.5960(4) 0.113(4) Uani 1 1 d U I 1
H15M H 0.0630 0.2502 0.6160 0.135 Uiso 1 1 calc R I 1
H15N H 0.1371 0.1765 0.6030 0.135 Uiso 1 1 calc R I 1
C157 C 0.0930(11) 0.3072(17) 0.5716(4) 0.142(5) Uani 1 1 d U I 1
H15O H 0.0901 0.3893 0.5821 0.170 Uiso 1 1 calc R I 1
H15P H 0.1459 0.2994 0.5628 0.170 Uiso 1 1 calc R I 1
C158 C 0.0349(12) 0.297(2) 0.5462(4) 0.176(8) Uani 1 1 d U I 1
H15Q H 0.0584 0.2949 0.5244 0.211 Uiso 1 1 calc R I 1
H15R H -0.0019 0.3677 0.5461 0.211 Uiso 1 1 calc R I 1
O9 O 0.0439(9) 0.4134(16) 0.7189(4) 0.145(7) Uiso 0.664(19) 1 d PDU J 1
C159 C -0.0364(10) 0.456(2) 0.7165(4) 0.156(10) Uiso 0.664(19) 1 d PDU J 1
H15S H -0.0737 0.3854 0.7157 0.187 Uiso 0.664(19) 1 calc PR J 1
H15T H -0.0481 0.5052 0.6958 0.187 Uiso 0.664(19) 1 calc PR J 1
C160 C -0.0463(12) 0.535(2) 0.7476(5) 0.131(8) Uiso 0.664(19) 1 d PDU J 1
H16A H -0.0994 0.5229 0.7559 0.158 Uiso 0.664(19) 1 calc PR J 1
H16B H -0.0388 0.6236 0.7429 0.158 Uiso 0.664(19) 1 calc PR J 1
C161 C 0.0212(16) 0.486(3) 0.7728(4) 0.193(14) Uiso 0.664(19) 1 d PDU J 1
H16C H 0.0528 0.5541 0.7835 0.232 Uiso 0.664(19) 1 calc PR J 1
H16D H -0.0010 0.4363 0.7904 0.232 Uiso 0.664(19) 1 calc PR J 1
C162 C 0.0703(13) 0.410(3) 0.7535(5) 0.156(10) Uiso 0.664(19) 1 d PDU J 1
H16E H 0.1262 0.4398 0.7568 0.188 Uiso 0.664(19) 1 calc PR J 1
H16F H 0.0692 0.3246 0.7616 0.188 Uiso 0.664(19) 1 calc PR J 1
O9A O 0.0747(13) 0.494(2) 0.7373(7) 0.109(9) Uiso 0.336(19) 1 d PDU J 2
C259 C 0.0483(13) 0.3704(18) 0.7341(14) 0.107(12) Uiso 0.336(19) 1 d PDU J 2
H25C H 0.0703 0.3218 0.7538 0.128 Uiso 0.336(19) 1 calc PR J 2
H25D H 0.0668 0.3331 0.7136 0.128 Uiso 0.336(19) 1 calc PR J 2
C260 C -0.0434(12) 0.371(2) 0.7318(8) 0.081(9) Uiso 0.336(19) 1 d PDU J 2
H26A H -0.0681 0.3899 0.7089 0.097 Uiso 0.336(19) 1 calc PR J 2
H26B H -0.0656 0.2934 0.7399 0.097 Uiso 0.336(19) 1 calc PR J 2
C261 C -0.050(2) 0.469(4) 0.7542(11) 0.108(12) Uiso 0.336(19) 1 d PU J 2
H26C H -0.0654 0.4345 0.7755 0.130 Uiso 0.336(19) 1 calc PR J 2
H26D H -0.0938 0.5227 0.7449 0.130 Uiso 0.336(19) 1 calc PR J 2
C262 C 0.0213(16) 0.545(3) 0.7620(7) 0.069(8) Uiso 0.336(19) 1 d PU J 2
H26E H 0.0446 0.5337 0.7855 0.083 Uiso 0.336(19) 1 calc PR J 2
H26F H 0.0096 0.6334 0.7579 0.083 Uiso 0.336(19) 1 calc PR J 2
O10 O 0.5876(12) 0.6045(16) 0.5490(5) 0.153(8) Uiso 0.534(17) 1 d PDU K 1
C163 C 0.5176(10) 0.5353(19) 0.5530(6) 0.125(9) Uiso 0.534(17) 1 d PDU K 1
H16G H 0.4910 0.5119 0.5307 0.150 Uiso 0.534(17) 1 calc PR K 1
H16H H 0.4797 0.5851 0.5648 0.150 Uiso 0.534(17) 1 calc PR K 1
C164 C 0.5415(13) 0.4196(17) 0.5735(8) 0.125(10) Uiso 0.534(17) 1 d PDU K 1
H16I H 0.5456 0.3472 0.5588 0.150 Uiso 0.534(17) 1 calc PR K 1
H16J H 0.5031 0.4018 0.5901 0.150 Uiso 0.534(17) 1 calc PR K 1
C165 C 0.6238(13) 0.457(2) 0.5908(6) 0.135(10) Uiso 0.534(17) 1 d PDU K 1
H16K H 0.6208 0.4686 0.6152 0.162 Uiso 0.534(17) 1 calc PR K 1
H16L H 0.6639 0.3922 0.5876 0.162 Uiso 0.534(17) 1 calc PR K 1
C166 C 0.6449(12) 0.570(2) 0.5753(6) 0.128(9) Uiso 0.534(17) 1 d PDU K 1
H16M H 0.6499 0.6356 0.5924 0.154 Uiso 0.534(17) 1 calc PR K 1
H16N H 0.6975 0.5599 0.5664 0.154 Uiso 0.534(17) 1 calc PR K 1
O10A O 0.6076(18) 0.417(3) 0.5458(7) 0.191(13) Uiso 0.466(17) 1 d PDU K 2
C263 C 0.629(2) 0.544(3) 0.5467(10) 0.191(19) Uiso 0.466(17) 1 d PDU K 2
H26G H 0.6102 0.5837 0.5251 0.229 Uiso 0.466(17) 1 calc PR K 2
H26H H 0.6878 0.5525 0.5504 0.229 Uiso 0.466(17) 1 calc PR K 2
C264 C 0.590(3) 0.604(3) 0.5756(12) 0.23(3) Uiso 0.466(17) 1 d PDU K 2
H26I H 0.5665 0.6855 0.5689 0.279 Uiso 0.466(17) 1 calc PR K 2
H26J H 0.6281 0.6146 0.5957 0.279 Uiso 0.466(17) 1 calc PR K 2
C265 C 0.524(2) 0.511(4) 0.5820(10) 0.187(18) Uiso 0.466(17) 1 d PDU K 2
H26K H 0.5304 0.4816 0.6055 0.224 Uiso 0.466(17) 1 calc PR K 2
H26L H 0.4702 0.5487 0.5775 0.224 Uiso 0.466(17) 1 calc PR K 2
C266 C 0.5330(19) 0.411(3) 0.5591(10) 0.164(17) Uiso 0.466(17) 1 d PDU K 2
H26M H 0.5288 0.3318 0.5710 0.196 Uiso 0.466(17) 1 calc PR K 2
H26N H 0.4895 0.4141 0.5405 0.196 Uiso 0.466(17) 1 calc PR K 2
O11 O 0.7528(8) -0.0767(10) 0.9082(4) 0.143(4) Uiso 0.750(11) 1 d PDU L 1
C167 C 0.8132(9) -0.0498(12) 0.8869(4) 0.113(5) Uiso 0.750(11) 1 d PDU L 1
H16O H 0.7908 -0.0539 0.8631 0.136 Uiso 0.750(11) 1 calc PR L 1
H16P H 0.8568 -0.1109 0.8904 0.136 Uiso 0.750(11) 1 calc PR L 1
C168 C 0.8461(13) 0.0796(16) 0.8950(7) 0.221(14) Uiso 0.750(11) 1 d PDU L 1
H16Q H 0.8444 0.1311 0.8745 0.265 Uiso 0.750(11) 1 calc PR L 1
H16R H 0.9016 0.0763 0.9056 0.265 Uiso 0.750(11) 1 calc PR L 1
C169 C 0.7885(13) 0.1287(15) 0.9195(7) 0.191(10) Uiso 0.750(11) 1 d PDU L 1
H16S H 0.8167 0.1396 0.9422 0.229 Uiso 0.750(11) 1 calc PR L 1
H16T H 0.7656 0.2086 0.9117 0.229 Uiso 0.750(11) 1 calc PR L 1
C170 C 0.7267(11) 0.0371(15) 0.9200(5) 0.161(8) Uiso 0.750(11) 1 d PDU L 1
H17A H 0.7120 0.0272 0.9432 0.193 Uiso 0.750(11) 1 calc PR L 1
H17B H 0.6786 0.0644 0.9057 0.193 Uiso 0.750(11) 1 calc PR L 1
O11A O 0.828(2) 0.037(4) 0.9346(7) 0.143(4) Uiso 0.250(11) 1 d PDU L 2
C267 C 0.8604(18) 0.025(5) 0.9033(9) 0.113(5) Uiso 0.250(11) 1 d PDU L 2
H26O H 0.8828 -0.0582 0.9011 0.136 Uiso 0.250(11) 1 calc PR L 2
H26P H 0.9040 0.0856 0.9019 0.136 Uiso 0.250(11) 1 calc PR L 2
C270 C 0.794(3) 0.048(6) 0.8749(7) 0.161(8) Uiso 0.250(11) 1 d PDU L 2
H27A H 0.7799 -0.0280 0.8622 0.193 Uiso 0.250(11) 1 calc PR L 2
H27B H 0.8098 0.1121 0.8592 0.193 Uiso 0.250(11) 1 calc PR L 2
C268 C 0.724(2) 0.093(7) 0.8941(13) 0.221(14) Uiso 0.250(11) 1 d PDU L 2
H26Q H 0.7034 0.1725 0.8851 0.265 Uiso 0.250(11) 1 calc PR L 2
H26R H 0.6802 0.0320 0.8922 0.265 Uiso 0.250(11) 1 calc PR L 2
C269 C 0.757(3) 0.105(6) 0.9285(11) 0.191(10) Uiso 0.250(11) 1 d PDU L 2
H26S H 0.7683 0.1932 0.9335 0.229 Uiso 0.250(11) 1 calc PR L 2
H26T H 0.7175 0.0765 0.9436 0.229 Uiso 0.250(11) 1 calc PR L 2
O12 O 0.9085(11) 0.6130(15) 0.6103(5) 0.183(8) Uiso 0.67(2) 1 d PDU M 1
C171 C 0.8530(15) 0.5603(19) 0.5855(6) 0.188(13) Uiso 0.67(2) 1 d PDU M 1
H17C H 0.8761 0.5585 0.5636 0.226 Uiso 0.67(2) 1 calc PR M 1
H17D H 0.8036 0.6104 0.5829 0.226 Uiso 0.67(2) 1 calc PR M 1
C172 C 0.8333(15) 0.4292(19) 0.5961(8) 0.195(13) Uiso 0.67(2) 1 d PDU M 1
H17E H 0.8420 0.3691 0.5782 0.234 Uiso 0.67(2) 1 calc PR M 1
H17F H 0.7773 0.4228 0.6017 0.234 Uiso 0.67(2) 1 calc PR M 1
C173 C 0.893(2) 0.409(2) 0.6273(8) 0.28(2) Uiso 0.67(2) 1 d PDU M 1
H17G H 0.8648 0.4069 0.6479 0.332 Uiso 0.67(2) 1 calc PR M 1
H17H H 0.9226 0.3314 0.6255 0.332 Uiso 0.67(2) 1 calc PR M 1
C174 C 0.9465(16) 0.513(3) 0.6279(9) 0.34(3) Uiso 0.67(2) 1 d PDU M 1
H17I H 0.9624 0.5375 0.6514 0.406 Uiso 0.67(2) 1 calc PR M 1
H17J H 0.9954 0.4901 0.6174 0.406 Uiso 0.67(2) 1 calc PR M 1
O12A O 0.842(3) 0.607(2) 0.6281(10) 0.188(19) Uiso 0.33(2) 1 d PDU M 2
C271 C 0.916(3) 0.577(3) 0.6470(14) 0.19(3) Uiso 0.33(2) 1 d PDU M 2
H27C H 0.9104 0.5876 0.6712 0.232 Uiso 0.33(2) 1 calc PR M 2
H27D H 0.9583 0.6330 0.6407 0.232 Uiso 0.33(2) 1 calc PR M 2
C272 C 0.938(2) 0.444(4) 0.6397(17) 0.32(6) Uiso 0.33(2) 1 d PDU M 2
H27E H 0.9481 0.3959 0.6608 0.384 Uiso 0.33(2) 1 calc PR M 2
H27F H 0.9853 0.4394 0.6270 0.384 Uiso 0.33(2) 1 calc PR M 2
C273 C 0.8623(17) 0.397(2) 0.6186(7) 0.065(8) Uiso 0.33(2) 1 d PDU M 2
H27G H 0.8733 0.3837 0.5950 0.079 Uiso 0.33(2) 1 calc PR M 2
H27H H 0.8434 0.3191 0.6277 0.079 Uiso 0.33(2) 1 calc PR M 2
C274 C 0.8038(16) 0.493(3) 0.6207(13) 0.20(3) Uiso 0.33(2) 1 d PDU M 2
H27I H 0.7700 0.4996 0.5991 0.242 Uiso 0.33(2) 1 calc PR M 2
H27J H 0.7687 0.4728 0.6384 0.242 Uiso 0.33(2) 1 calc PR M 2
O13 O 0.1935(11) 0.6993(17) 0.9829(6) 0.276(9) Uiso 1 1 d DU N 1
C175 C 0.2608(15) 0.682(2) 1.0066(5) 0.257(13) Uiso 1 1 d DU N 1
H17K H 0.2430 0.6630 1.0289 0.308 Uiso 1 1 calc R N 1
H17L H 0.2929 0.7589 1.0087 0.308 Uiso 1 1 calc R N 1
C176 C 0.3116(13) 0.577(2) 0.9948(5) 0.247(12) Uiso 1 1 d DU N 1
H17M H 0.3039 0.5005 1.0077 0.296 Uiso 1 1 calc R N 1
H17N H 0.3691 0.5981 0.9969 0.296 Uiso 1 1 calc R N 1
C177 C 0.2785(12) 0.5626(17) 0.9578(5) 0.176(7) Uiso 1 1 d DU N 1
H17O H 0.3210 0.5776 0.9428 0.211 Uiso 1 1 calc R N 1
H17P H 0.2569 0.4788 0.9535 0.211 Uiso 1 1 calc R N 1
C178 C 0.2159(15) 0.653(2) 0.9521(5) 0.256(13) Uiso 1 1 d DU N 1
H17Q H 0.2347 0.7213 0.9386 0.307 Uiso 1 1 calc R N 1
H17R H 0.1689 0.6150 0.9393 0.307 Uiso 1 1 calc R N 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
C1 0.052(4) 0.054(4) 0.029(3) -0.005(3) -0.009(3) 0.013(3)
C2 0.049(4) 0.051(4) 0.041(4) -0.003(3) -0.008(3) 0.005(3)
C3 0.051(4) 0.048(4) 0.043(4) -0.004(3) -0.003(3) 0.005(3)
C4 0.044(3) 0.055(4) 0.024(3) 0.005(3) 0.002(3) 0.006(3)
C5 0.040(3) 0.062(4) 0.039(4) -0.007(3) -0.002(3) 0.005(3)
C6 0.055(4) 0.047(4) 0.034(3) -0.005(3) -0.004(3) 0.008(3)
C7 0.043(3) 0.053(4) 0.029(3) -0.001(3) 0.001(3) 0.007(3)
C8 0.049(4) 0.053(4) 0.034(3) 0.002(3) 0.000(3) 0.006(3)
C9 0.046(4) 0.053(4) 0.034(3) -0.006(3) 0.001(3) 0.007(3)
C10 0.045(3) 0.054(4) 0.035(3) 0.005(3) 0.003(3) 0.005(3)
C11 0.049(4) 0.051(4) 0.031(3) 0.002(3) 0.005(3) 0.011(3)
C12 0.045(4) 0.051(4) 0.034(3) 0.004(3) 0.000(3) 0.004(3)
C13 0.046(4) 0.058(4) 0.029(3) 0.003(3) 0.002(3) 0.011(3)
C14 0.091(6) 0.068(5) 0.054(5) -0.005(4) -0.023(4) 0.008(4)
C15 0.080(6) 0.099(6) 0.057(5) -0.008(5) -0.029(4) 0.013(5)
C16 0.064(5) 0.108(6) 0.036(4) 0.007(4) -0.011(3) 0.024(5)
C17 0.080(6) 0.077(5) 0.057(5) 0.023(4) 0.004(4) 0.018(4)
C18 0.056(4) 0.067(4) 0.046(4) 0.009(3) -0.005(3) 0.007(4)
C19 0.048(4) 0.060(4) 0.033(3) -0.001(3) -0.001(3) 0.013(3)
C20 0.087(6) 0.067(5) 0.044(4) -0.010(3) 0.009(4) -0.002(4)
C21 0.103(7) 0.087(6) 0.039(4) -0.016(4) 0.004(4) 0.000(5)
C22 0.078(6) 0.119(7) 0.035(4) -0.008(4) 0.007(4) -0.005(5)
C23 0.087(6) 0.122(8) 0.039(4) -0.006(4) 0.015(4) -0.023(5)
C24 0.063(5) 0.099(6) 0.040(4) -0.009(4) 0.014(3) -0.014(4)
C25 0.052(4) 0.061(4) 0.029(3) 0.007(3) 0.001(3) 0.017(3)
C26 0.063(4) 0.065(4) 0.059(5) -0.007(4) 0.007(4) 0.013(4)
C27 0.083(5) 0.090(6) 0.058(5) -0.018(4) 0.007(4) 0.032(4)
C28 0.067(5) 0.102(6) 0.062(5) 0.009(5) 0.006(4) 0.032(5)
C29 0.052(4) 0.111(6) 0.050(5) 0.004(4) 0.003(4) 0.017(4)
C30 0.051(4) 0.080(5) 0.044(4) 0.009(4) 0.001(3) 0.008(3)
C31 0.049(4) 0.067(4) 0.030(3) -0.001(3) 0.003(3) 0.017(3)
C32 0.066(5) 0.061(4) 0.046(4) 0.006(3) 0.003(3) 0.023(4)
C33 0.100(7) 0.080(5) 0.055(5) 0.011(4) -0.001(4) 0.040(5)
C34 0.087(6) 0.112(6) 0.044(5) 0.001(4) -0.013(4) 0.052(5)
C35 0.078(6) 0.109(6) 0.057(5) -0.017(5) -0.021(4) 0.032(5)
C36 0.057(4) 0.081(5) 0.039(4) -0.008(3) -0.006(3) 0.013(4)
C37 0.045(4) 0.064(4) 0.028(3) -0.002(3) 0.004(3) 0.016(3)
C38 0.057(4) 0.076(5) 0.044(4) 0.007(3) 0.010(3) 0.010(4)
C39 0.064(5) 0.104(6) 0.041(4) 0.016(4) 0.013(4) 0.014(4)
C40 0.070(5) 0.124(7) 0.028(4) 0.003(4) 0.004(3) 0.027(5)
C41 0.067(5) 0.097(5) 0.035(4) -0.018(4) -0.004(4) 0.026(4)
C42 0.063(5) 0.069(4) 0.036(3) 0.000(3) -0.007(3) 0.014(4)
C43 0.050(4) 0.049(4) 0.031(3) -0.004(3) -0.006(3) 0.007(3)
C44 0.048(4) 0.050(4) 0.035(3) -0.003(3) -0.005(3) 0.012(3)
C45 0.044(4) 0.060(4) 0.031(3) -0.006(3) 0.001(3) 0.006(3)
C46 0.049(4) 0.045(4) 0.031(3) -0.001(3) -0.001(3) 0.001(3)
C47 0.047(4) 0.051(4) 0.031(3) -0.003(3) -0.002(3) 0.012(3)
C48 0.050(4) 0.061(4) 0.034(3) -0.009(3) -0.004(3) 0.013(3)
C49 0.045(3) 0.045(4) 0.029(3) -0.006(3) -0.002(2) 0.002(3)
C50 0.045(3) 0.052(4) 0.027(3) -0.003(3) 0.002(2) 0.005(3)
C51 0.048(3) 0.044(3) 0.031(3) 0.001(3) -0.004(3) 0.000(3)
C52 0.048(4) 0.043(4) 0.032(3) 0.002(3) -0.003(3) 0.002(3)
C53 0.046(4) 0.044(4) 0.036(3) -0.004(3) -0.001(3) 0.001(3)
C54 0.048(3) 0.047(4) 0.028(3) -0.002(3) -0.004(3) 0.001(3)
C55 0.051(4) 0.052(4) 0.032(3) 0.001(3) -0.006(3) -0.008(3)
C56 0.078(5) 0.065(4) 0.041(4) 0.008(3) 0.006(3) 0.002(4)
C57 0.107(7) 0.076(5) 0.045(5) 0.014(4) 0.000(4) -0.014(5)
C58 0.085(6) 0.109(7) 0.046(5) 0.016(4) 0.012(4) -0.028(5)
C59 0.072(6) 0.115(7) 0.053(5) 0.005(5) 0.016(4) -0.011(5)
C60 0.052(4) 0.082(5) 0.040(4) 0.004(3) 0.004(3) 0.003(4)
C61 0.051(4) 0.058(4) 0.030(3) 0.001(3) 0.001(3) -0.005(3)
C62 0.060(4) 0.064(4) 0.037(4) -0.005(3) 0.000(3) -0.007(3)
C63 0.076(5) 0.084(5) 0.047(4) -0.005(4) 0.007(4) -0.026(4)
C64 0.057(5) 0.110(6) 0.052(5) -0.004(5) -0.002(4) -0.028(4)
C65 0.052(4) 0.110(6) 0.057(5) 0.013(5) -0.009(4) -0.006(4)
C66 0.058(4) 0.076(5) 0.036(4) 0.008(3) -0.007(3) -0.004(3)
C67 0.048(4) 0.049(4) 0.032(3) 0.001(3) 0.003(3) -0.004(3)
C68 0.071(5) 0.052(4) 0.031(3) 0.002(3) -0.009(3) -0.006(3)
C69 0.077(5) 0.060(4) 0.039(4) -0.011(3) -0.009(4) -0.008(4)
C70 0.078(5) 0.059(4) 0.032(4) 0.000(3) -0.007(3) -0.001(4)
C71 0.064(5) 0.060(4) 0.032(4) 0.004(3) -0.007(3) -0.001(4)
C72 0.053(4) 0.054(4) 0.034(3) 0.002(3) -0.002(3) -0.004(3)
C73 0.050(4) 0.055(4) 0.032(3) 0.008(3) -0.006(3) 0.000(3)
C74 0.079(5) 0.067(4) 0.043(4) 0.003(3) 0.013(4) 0.003(4)
C75 0.078(6) 0.082(5) 0.056(5) 0.002(4) 0.030(4) 0.003(5)
C76 0.066(5) 0.097(5) 0.047(4) 0.015(4) 0.009(4) -0.013(5)
C77 0.057(5) 0.072(5) 0.059(5) 0.021(3) -0.002(4) -0.008(4)
C78 0.049(4) 0.060(4) 0.050(4) 0.007(3) -0.004(3) -0.005(3)
C79 0.046(3) 0.060(4) 0.036(4) 0.006(3) -0.005(3) 0.001(3)
C80 0.060(4) 0.075(5) 0.041(4) 0.010(3) 0.003(3) 0.000(4)
C81 0.044(4) 0.110(6) 0.063(5) 0.026(4) 0.004(4) -0.008(4)
C82 0.062(5) 0.125(8) 0.070(6) 0.015(5) -0.010(4) -0.038(5)
C83 0.082(6) 0.088(6) 0.077(6) -0.004(5) -0.024(5) -0.021(5)
C84 0.061(4) 0.066(5) 0.061(5) -0.008(4) -0.014(4) -0.009(4)
C85 0.044(4) 0.051(4) 0.030(3) -0.008(3) -0.007(3) 0.010(3)
C86 0.065(4) 0.045(4) 0.037(3) -0.004(3) -0.004(3) 0.011(3)
C87 0.058(4) 0.053(4) 0.029(3) -0.003(3) -0.001(3) 0.005(3)
C88 0.035(3) 0.049(3) 0.029(3) -0.007(3) -0.003(2) 0.005(3)
C89 0.065(4) 0.048(4) 0.034(3) -0.005(3) -0.006(3) -0.002(3)
C90 0.059(4) 0.058(4) 0.029(3) 0.000(3) 0.001(3) 0.002(3)
C91 0.049(3) 0.043(3) 0.023(3) -0.002(2) 0.000(2) 0.005(3)
C92 0.053(3) 0.041(3) 0.028(3) -0.001(2) 0.002(3) 0.002(3)
C93 0.045(3) 0.046(4) 0.027(3) -0.004(2) 0.003(3) -0.001(3)
C94 0.043(3) 0.047(4) 0.036(3) -0.004(3) 0.004(3) 0.001(3)
C95 0.046(3) 0.051(4) 0.033(3) -0.004(3) 0.000(3) 0.003(3)
C96 0.049(3) 0.044(3) 0.032(3) -0.005(3) 0.001(3) 0.007(3)
C97 0.044(3) 0.055(4) 0.023(3) -0.004(3) -0.003(2) 0.003(3)
C98 0.049(4) 0.068(4) 0.040(4) 0.012(3) 0.007(3) 0.011(3)
C99 0.063(5) 0.056(4) 0.062(5) 0.002(3) 0.002(4) 0.020(3)
C100 0.049(4) 0.073(5) 0.050(4) -0.008(4) 0.008(3) 0.012(3)
C101 0.058(4) 0.067(4) 0.053(4) 0.001(3) 0.021(3) 0.003(4)
C102 0.066(5) 0.050(4) 0.053(4) 0.002(3) 0.017(3) 0.007(3)
C103 0.046(3) 0.044(4) 0.033(3) -0.009(3) 0.001(3) 0.007(3)
C104 0.055(4) 0.055(4) 0.028(3) 0.000(3) 0.002(3) -0.005(3)
C105 0.055(4) 0.058(4) 0.031(3) 0.001(3) -0.004(3) 0.007(3)
C106 0.043(4) 0.070(5) 0.041(4) -0.005(3) -0.009(3) 0.004(3)
C107 0.045(4) 0.068(5) 0.050(4) 0.001(3) 0.001(3) -0.003(3)
C108 0.048(4) 0.064(4) 0.033(3) -0.001(3) 0.004(3) -0.002(3)
C109 0.048(4) 0.063(4) 0.025(3) -0.004(3) 0.001(3) 0.010(3)
C110 0.051(4) 0.080(5) 0.042(4) 0.000(3) 0.009(3) 0.010(4)
C111 0.057(5) 0.142(8) 0.030(4) -0.010(4) 0.001(3) 0.019(5)
C112 0.071(6) 0.145(8) 0.042(4) -0.031(5) 0.000(4) 0.022(5)
C113 0.077(6) 0.090(6) 0.062(5) -0.035(4) -0.012(4) 0.016(4)
C114 0.056(4) 0.063(4) 0.046(4) -0.020(3) 0.000(3) 0.007(3)
C115 0.048(3) 0.059(4) 0.031(3) -0.004(3) 0.003(3) 0.009(3)
C116 0.050(4) 0.067(4) 0.060(5) -0.006(4) 0.008(3) 0.001(3)
C117 0.049(4) 0.107(6) 0.058(5) -0.015(5) 0.005(4) 0.001(4)
C118 0.046(4) 0.115(6) 0.058(5) -0.024(5) -0.003(4) 0.017(4)
C119 0.067(5) 0.081(5) 0.077(6) -0.011(5) 0.002(4) 0.031(4)
C120 0.056(4) 0.062(4) 0.066(5) -0.007(4) 0.008(4) 0.010(3)
C121 0.040(3) 0.062(4) 0.037(4) -0.011(3) 0.000(3) 0.010(3)
C122 0.054(4) 0.078(5) 0.067(5) -0.006(4) -0.007(4) -0.006(4)
C123 0.064(5) 0.095(6) 0.078(6) -0.020(5) -0.007(4) -0.007(5)
C124 0.056(5) 0.132(7) 0.054(5) -0.010(5) -0.016(4) 0.005(5)
C125 0.080(6) 0.110(6) 0.049(5) 0.008(5) -0.021(4) 0.006(5)
C126 0.069(5) 0.080(5) 0.056(5) 0.007(4) -0.019(4) -0.004(4)
N1 0.050(3) 0.063(3) 0.029(3) -0.010(2) -0.011(2) 0.016(3)
O4 0.137(8) 0.211(15) 0.171(11) -0.084(12) 0.047(9) -0.027(9)
C139 0.108(6) 0.156(12) 0.138(9) -0.043(8) 0.024(7) -0.026(8)
C140 0.114(7) 0.130(11) 0.172(12) -0.004(8) 0.042(8) -0.005(9)
C141 0.123(7) 0.27(2) 0.086(8) 0.053(8) -0.032(7) -0.030(9)
C142 0.211(13) 0.116(11) 0.142(12) -0.028(8) -0.001(11) -0.016(9)
O7 0.091(5) 0.124(6) 0.110(5) 0.008(4) -0.006(4) 0.002(4)
C151 0.092(6) 0.151(9) 0.119(9) -0.008(6) -0.001(6) -0.023(5)
C152 0.097(6) 0.183(9) 0.077(6) 0.038(6) -0.003(5) -0.029(7)
C153 0.130(8) 0.231(14) 0.087(9) 0.010(9) -0.025(6) 0.033(8)
C154 0.092(8) 0.126(7) 0.189(15) 0.034(6) -0.002(7) 0.000(5)
O8 0.175(10) 0.213(12) 0.135(8) 0.012(7) -0.063(7) -0.055(8)
C155 0.112(9) 0.138(8) 0.082(7) -0.024(5) 0.006(5) -0.012(6)
C156 0.125(9) 0.112(8) 0.094(7) -0.029(5) -0.023(6) 0.018(6)
C157 0.135(11) 0.167(12) 0.122(10) -0.009(7) 0.005(7) -0.040(9)
C158 0.180(16) 0.245(17) 0.099(10) 0.054(11) -0.014(8) -0.060(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0000 '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 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0000 '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_publ_flag
C127 O1 C130 106.3(6) y
C227 O1A C230 107(2) y
C131 O2 C134 108(2) y
C231 O2A C234 108(4) y
C135 O3 C138 107.1(14) y
C235 O3A C238 106.3(18) y
C143 O5 C146 105.9(11) y
C243 O5A C246 102.8(8) y
C43 N1 C85 123.94 y
C1 N1 C85 115.37 y
C1 N1 C43 118.94 y
C147 O6 C150 107.7(12) y
C247 O6A C250 108(2) y
C159 O9 C162 106.3(15) y
C259 O9A C262 102(2) y
C163 O10 C166 106.8(18) y
C263 O10A C266 106(3) y
C167 O11 C170 106.5(12) y
C267 O11A C269 107(3) y
C171 O12 C174 105.8(19) y
C271 O12A C274 105(3) y
N1 C1 C6 120.54 y
C2 C1 C6 119.0(7) ?
N1 C1 C2 120.48 y
C1 C2 C3 120.1(8) ?
C2 C3 C4 120.9(6) ?
C3 C4 C5 118.4(7) ?
C139 O4 C142 101.5(15) y
C3 C4 C7 120.0(6) ?
C5 C4 C7 121.1(7) ?
C140 O4A C141 75.9(18) y
C4 C5 C6 120.5(8) ?
C1 C6 C5 120.7(7) ?
C8 C7 C12 119.7(7) ?
C4 C7 C12 123.5(7) ?
C4 C7 C8 116.8(7) ?
C7 C8 C13 120.8(7) ?
C9 C8 C13 119.0(7) ?
C7 C8 C9 120.2(7) ?
C8 C9 C19 119.9(7) ?
C10 C9 C19 120.4(7) ?
C8 C9 C10 119.4(7) ?
C9 C10 C25 118.9(7) ?
C9 C10 C11 120.5(7) ?
C11 C10 C25 120.7(7) ?
C12 C11 C31 120.7(7) ?
C10 C11 C31 119.7(7) ?
C10 C11 C12 119.7(7) ?
C7 C12 C37 122.3(7) ?
C7 C12 C11 120.4(7) ?
C11 C12 C37 117.2(7) ?
C14 C13 C18 118.5(8) ?
C8 C13 C18 120.5(7) ?
C8 C13 C14 121.0(7) ?
C13 C14 C15 120.2(8) ?
C14 C15 C16 120.8(10) ?
C15 C16 C17 120.1(9) ?
C16 C17 C18 120.8(9) ?
C13 C18 C17 119.7(8) ?
C20 C19 C24 118.0(8) ?
C9 C19 C24 119.2(7) ?
C9 C19 C20 122.9(7) ?
C19 C20 C21 119.4(9) ?
C20 C21 C22 121.2(10) ?
C21 C22 C23 120.5(11) ?
C22 C23 C24 119.1(10) ?
C19 C24 C23 121.8(9) ?
C26 C25 C30 118.7(8) ?
C10 C25 C26 120.7(8) ?
C10 C25 C30 120.5(7) ?
C25 C26 C27 119.7(9) ?
C26 C27 C28 120.8(9) ?
C27 C28 C29 119.2(10) ?
C28 C29 C30 121.2(10) ?
C25 C30 C29 120.5(8) ?
C32 C31 C36 119.3(8) ?
C11 C31 C32 120.1(7) ?
C11 C31 C36 120.6(7) ?
C31 C32 C33 121.1(8) ?
C32 C33 C34 120.2(9) ?
C33 C34 C35 119.0(11) ?
C34 C35 C36 121.8(10) ?
C31 C36 C35 118.7(8) ?
C38 C37 C42 119.4(7) ?
C12 C37 C42 120.4(7) ?
C12 C37 C38 119.8(7) ?
C37 C38 C39 121.0(8) ?
C38 C39 C40 119.9(9) ?
C39 C40 C41 119.4(8) ?
C40 C41 C42 122.0(8) ?
C37 C42 C41 118.3(8) ?
N1 C43 C48 120.87 y
N1 C43 C44 122.00 y
C44 C43 C48 117.1(7) ?
C43 C44 C45 120.8(7) ?
C44 C45 C46 121.9(7) ?
C45 C46 C47 117.4(7) ?
C45 C46 C49 119.5(7) ?
C47 C46 C49 123.1(7) ?
C46 C47 C48 121.5(7) ?
C43 C48 C47 121.3(7) ?
C50 C49 C54 120.6(7) ?
C46 C49 C54 120.5(7) ?
C46 C49 C50 118.7(7) ?
C49 C50 C51 119.1(7) ?
C49 C50 C55 121.8(7) ?
C51 C50 C55 119.1(7) ?
C50 C51 C61 120.3(7) ?
C52 C51 C61 119.8(7) ?
C50 C51 C52 119.8(7) ?
C51 C52 C53 120.8(7) ?
C53 C52 C67 120.0(7) ?
C51 C52 C67 119.3(7) ?
C54 C53 C73 120.6(7) ?
C52 C53 C73 119.1(7) ?
C52 C53 C54 120.3(7) ?
C53 C54 C79 120.3(7) ?
C49 C54 C79 120.3(7) ?
C49 C54 C53 119.4(7) ?
C56 C55 C60 117.3(8) ?
C50 C55 C56 121.7(7) ?
C50 C55 C60 121.0(7) ?
C55 C56 C57 121.2(9) ?
C56 C57 C58 120.1(10) ?
C57 C58 C59 119.9(11) ?
C58 C59 C60 120.5(11) ?
C55 C60 C59 120.9(8) ?
C51 C61 C66 121.2(7) ?
C62 C61 C66 117.7(9) ?
C51 C61 C62 121.0(8) ?
C61 C62 C63 121.9(9) ?
C62 C63 C64 118.3(9) ?
C63 C64 C65 120.8(10) ?
C64 C65 C66 120.1(10) ?
C61 C66 C65 121.2(8) ?
C52 C67 C68 120.3(6) ?
C52 C67 C72 121.4(6) ?
C68 C67 C72 118.4(7) ?
C67 C68 C69 121.4(7) ?
C68 C69 C70 119.3(7) ?
C69 C70 C71 120.8(8) ?
C70 C71 C72 119.9(7) ?
C67 C72 C71 120.3(7) ?
C74 C73 C78 118.5(8) ?
C53 C73 C74 119.8(6) ?
C53 C73 C78 121.5(7) ?
C73 C74 C75 121.3(8) ?
C74 C75 C76 118.8(10) ?
C75 C76 C77 121.5(10) ?
C76 C77 C78 118.6(8) ?
C73 C78 C77 121.2(8) ?
C54 C79 C80 122.1(7) ?
C54 C79 C84 120.3(8) ?
C80 C79 C84 117.6(8) ?
C79 C80 C81 121.6(8) ?
C80 C81 C82 119.8(10) ?
C81 C82 C83 120.0(11) ?
C82 C83 C84 121.2(10) ?
C79 C84 C83 119.7(9) ?
C86 C85 C90 118.9(7) ?
N1 C85 C90 122.45 y
N1 C85 C86 118.66 y
C85 C86 C87 120.5(6) ?
C86 C87 C88 121.0(7) ?
C89 C88 C96 121.6(6) ?
C87 C88 C89 119.0(7) ?
C87 C88 C96 119.3(7) ?
C88 C89 C90 119.8(6) ?
C85 C90 C89 120.6(7) ?
C92 C91 C96 119.3(7) ?
C96 C91 C97 118.0(7) ?
C92 C91 C97 122.6(7) ?
C91 C92 C103 120.6(7) ?
C93 C92 C103 120.1(7) ?
C91 C92 C93 119.4(7) ?
C94 C93 C109 119.1(7) ?
C92 C93 C94 121.2(7) ?
C92 C93 C109 119.7(7) ?
C93 C94 C95 120.1(7) ?
C95 C94 C115 118.5(7) ?
C93 C94 C115 121.4(7) ?
C94 C95 C121 122.1(7) ?
C96 C95 C121 119.1(7) ?
C94 C95 C96 118.8(7) ?
C88 C96 C91 118.4(7) ?
C91 C96 C95 121.1(7) ?
C88 C96 C95 120.5(7) ?
C98 C97 C102 117.2(8) ?
C91 C97 C98 121.1(7) ?
C91 C97 C102 121.4(7) ?
C97 C98 C99 121.3(8) ?
C98 C99 C100 121.4(8) ?
C99 C100 C101 119.1(9) ?
C100 C101 C102 120.0(8) ?
C97 C102 C101 120.9(7) ?
C1 C2 H2 120.00 ?
C3 C2 H2 120.00 ?
C92 C103 C108 121.0(7) ?
C92 C103 C104 121.3(7) ?
C2 C3 H3 120.00 ?
C4 C3 H3 119.00 ?
C104 C103 C108 117.7(8) ?
C103 C104 C105 121.1(8) ?
C140 O4A H14B 58.00 ?
C141 O4A H14B 131.00 ?
C104 C105 C106 120.2(7) ?
C4 C5 H5 120.00 ?
C6 C5 H5 120.00 ?
C1 C6 H6 120.00 ?
C5 C6 H6 120.00 ?
C105 C106 C107 119.0(8) ?
C106 C107 C108 120.9(8) ?
C103 C108 C107 121.2(7) ?
C110 C109 C114 119.8(8) ?
C93 C109 C110 119.9(7) ?
C93 C109 C114 120.3(7) ?
C109 C110 C111 119.7(9) ?
C110 C111 C112 120.3(9) ?
C111 C112 C113 120.8(11) ?
C112 C113 C114 120.8(10) ?
C109 C114 C113 118.6(8) ?
C15 C14 H14 120.00 ?
C13 C14 H14 120.00 ?
C116 C115 C120 119.1(8) ?
C14 C15 H15 120.00 ?
C94 C115 C120 120.8(7) ?
C16 C15 H15 120.00 ?
C94 C115 C116 120.0(7) ?
C15 C16 H16 120.00 ?
C17 C16 H16 120.00 ?
C115 C116 C117 120.5(8) ?
C18 C17 H17 120.00 ?
C16 C17 H17 120.00 ?
C116 C117 C118 120.3(10) ?
C13 C18 H18 120.00 ?
C17 C18 H18 120.00 ?
C117 C118 C119 119.8(10) ?
C118 C119 C120 120.8(9) ?
C19 C20 H20 120.00 ?
C115 C120 C119 119.5(9) ?
C21 C20 H20 120.00 ?
C95 C121 C122 122.9(8) ?
C95 C121 C126 119.7(7) ?
C22 C21 H21 120.00 ?
C20 C21 H21 119.00 ?
C122 C121 C126 117.3(8) ?
C23 C22 H22 120.00 ?
C121 C122 C123 121.1(9) ?
C21 C22 H22 120.00 ?
C122 C123 C124 120.6(10) ?
C22 C23 H23 120.00 ?
C24 C23 H23 120.00 ?
C19 C24 H24 119.00 ?
C123 C124 C125 119.6(11) ?
C23 C24 H24 119.00 ?
C124 C125 C126 118.8(10) ?
C27 C26 H26 120.00 ?
C121 C126 C125 122.5(7) ?
C25 C26 H26 120.00 ?
C28 C27 H27 120.00 ?
C26 C27 H27 120.00 ?
C29 C28 H28 120.00 ?
C27 C28 H28 120.00 ?
C28 C29 H29 120.00 ?
C30 C29 H29 119.00 ?
C29 C30 H30 120.00 ?
C25 C30 H30 120.00 ?
C33 C32 H32 119.00 ?
C31 C32 H32 119.00 ?
C32 C33 H33 120.00 ?
C34 C33 H33 120.00 ?
C33 C34 H34 121.00 ?
C35 C34 H34 120.00 ?
C36 C35 H35 119.00 ?
C34 C35 H35 119.00 ?
C35 C36 H36 121.00 ?
C31 C36 H36 120.00 ?
C37 C38 H38 119.00 ?
C39 C38 H38 120.00 ?
C38 C39 H39 120.00 ?
C40 C39 H39 120.00 ?
C39 C40 H40 120.00 ?
C41 C40 H40 120.00 ?
C40 C41 H41 119.00 ?
C42 C41 H41 119.00 ?
C41 C42 H42 121.00 ?
C37 C42 H42 121.00 ?
C45 C44 H44 120.00 ?
C43 C44 H44 120.00 ?
C46 C45 H45 119.00 ?
C44 C45 H45 119.00 ?
C46 C47 H47 119.00 ?
C48 C47 H47 119.00 ?
C47 C48 H48 119.00 ?
C43 C48 H48 119.00 ?
C55 C56 H56 120.00 ?
C57 C56 H56 119.00 ?
C56 C57 H57 120.00 ?
C58 C57 H57 120.00 ?
C57 C58 H58 120.00 ?
C59 C58 H58 120.00 ?
C60 C59 H59 120.00 ?
C58 C59 H59 120.00 ?
C59 C60 H60 120.00 ?
C55 C60 H60 120.00 ?
C61 C62 H62 119.00 ?
C63 C62 H62 119.00 ?
C62 C63 H63 121.00 ?
C64 C63 H63 121.00 ?
C65 C64 H64 120.00 ?
C63 C64 H64 120.00 ?
C66 C65 H65 120.00 ?
C64 C65 H65 120.00 ?
C61 C66 H66 119.00 ?
C65 C66 H66 119.00 ?
C67 C68 H68 119.00 ?
C69 C68 H68 119.00 ?
C70 C69 H69 120.00 ?
C68 C69 H69 120.00 ?
C69 C70 H70 120.00 ?
C71 C70 H70 120.00 ?
C72 C71 H71 120.00 ?
C70 C71 H71 120.00 ?
C67 C72 H72 120.00 ?
C71 C72 H72 120.00 ?
C73 C74 H74 119.00 ?
C75 C74 H74 119.00 ?
C76 C75 H75 121.00 ?
C74 C75 H75 121.00 ?
C77 C76 H76 119.00 ?
C75 C76 H76 119.00 ?
C76 C77 H77 121.00 ?
C78 C77 H77 121.00 ?
C73 C78 H78 119.00 ?
C77 C78 H78 119.00 ?
C79 C80 H80 119.00 ?
C81 C80 H80 119.00 ?
C80 C81 H81 120.00 ?
C82 C81 H81 120.00 ?
C81 C82 H82 120.00 ?
C83 C82 H82 120.00 ?
C82 C83 H83 119.00 ?
C84 C83 H83 119.00 ?
C79 C84 H84 120.00 ?
C83 C84 H84 120.00 ?
C85 C86 H86 120.00 ?
C87 C86 H86 120.00 ?
C86 C87 H87 119.00 ?
C88 C87 H87 120.00 ?
C90 C89 H89 120.00 ?
C88 C89 H89 120.00 ?
C89 C90 H90 120.00 ?
C85 C90 H90 120.00 ?
C99 C98 H98 119.00 ?
C97 C98 H98 119.00 ?
C98 C99 H99 119.00 ?
C100 C99 H99 119.00 ?
C101 C100 H100 120.00 ?
C99 C100 H100 120.00 ?
C100 C101 H101 120.00 ?
C102 C101 H101 120.00 ?
C97 C102 H102 120.00 ?
C101 C102 H102 120.00 ?
C103 C104 H104 120.00 ?
C105 C104 H104 119.00 ?
C104 C105 H105 120.00 ?
C106 C105 H105 120.00 ?
C107 C106 H106 121.00 ?
C105 C106 H106 120.00 ?
C151 O7 C154 105.8(12) y
C106 C107 H107 119.00 ?
C108 C107 H107 120.00 ?
C103 C108 H108 119.00 ?
C107 C108 H108 119.00 ?
C111 C110 H110 120.00 ?
C109 C110 H110 120.00 ?
C110 C111 H111 120.00 ?
C112 C111 H111 120.00 ?
C113 C112 H112 120.00 ?
C111 C112 H112 120.00 ?
C112 C113 H113 119.00 ?
C114 C113 H113 120.00 ?
C109 C114 H114 121.00 ?
C113 C114 H114 121.00 ?
C115 C116 H116 120.00 ?
C117 C116 H116 120.00 ?
C116 C117 H117 120.00 ?
C118 C117 H117 120.00 ?
C117 C118 H118 120.00 ?
C119 C118 H118 120.00 ?
C120 C119 H119 120.00 ?
C118 C119 H119 120.00 ?
C119 C120 H120 120.00 ?
C115 C120 H120 120.00 ?
C123 C122 H122 119.00 ?
C121 C122 H122 119.00 ?
C124 C123 H123 120.00 ?
C122 C123 H123 120.00 ?
C125 C124 H124 120.00 ?
C123 C124 H124 120.00 ?
C124 C125 H125 121.00 ?
C126 C125 H125 121.00 ?
C125 C126 H126 119.00 ?
C121 C126 H126 119.00 ?
O1 C127 C128 109.9(8) y
C127 C128 C129 102.3(10) ?
C128 C129 C130 105.3(13) ?
O1 C130 C129 110.4(12) y
C155 O8 C158 108.2(12) y
C128 C127 H12B 110.00 ?
C128 C127 H12A 110.00 ?
H12A C127 H12B 108.00 ?
O1A C227 C228 109(3) y
O1 C127 H12A 110.00 ?
O1 C127 H12B 110.00 ?
C129 C128 H12C 111.00 ?
C129 C128 H12D 111.00 ?
C127 C128 H12C 111.00 ?
H12C C128 H12D 109.00 ?
C127 C128 H12D 111.00 ?
C227 C228 C229 101(2) ?
C130 C129 H12E 111.00 ?
C130 C129 H12F 111.00 ?
C128 C129 H12E 111.00 ?
H12E C129 H12F 109.00 ?
C128 C129 H12F 111.00 ?
C228 C229 C230 105(2) ?
C129 C130 H13A 110.00 ?
H13A C130 H13B 108.00 ?
O1A C230 C229 112(2) y
O1 C130 H13B 109.00 ?
O1 C130 H13A 109.00 ?
C129 C130 H13B 110.00 ?
H22A C227 H22B 108.00 ?
C228 C227 H22B 110.00 ?
O1A C227 H22A 110.00 ?
C228 C227 H22A 110.00 ?
O1A C227 H22B 110.00 ?
C229 C228 H22C 111.00 ?
H22C C228 H22D 109.00 ?
C227 C228 H22C 112.00 ?
C227 C228 H22D 112.00 ?
C229 C228 H22D 112.00 ?
H22E C229 H22F 109.00 ?
C230 C229 H22F 111.00 ?
C228 C229 H22F 111.00 ?
C230 C229 H22E 111.00 ?
C228 C229 H22E 110.00 ?
O1A C230 H23B 109.00 ?
C229 C230 H23B 109.00 ?
H23A C230 H23B 108.00 ?
C229 C230 H23A 109.00 ?
O1A C230 H23A 109.00 ?
O2 C131 C132 108(2) y
C131 C132 C133 107(2) ?
C132 C133 C134 103(2) ?
O2 C134 C133 105(2) y
C175 O13 C178 105.9(18) y
C132 C131 H13D 110.00 ?
C132 C131 H13C 110.00 ?
H13C C131 H13D 109.00 ?
O2A C231 C232 106(3) y
O2 C131 H13D 111.00 ?
O2 C131 H13C 110.00 ?
C133 C132 H13E 110.00 ?
C231 C232 C233 107(3) ?
C131 C132 H13F 110.00 ?
C131 C132 H13E 110.00 ?
H13E C132 H13F 109.00 ?
C133 C132 H13F 110.00 ?
C134 C133 H13H 111.00 ?
C132 C133 H13H 111.00 ?
H13G C133 H13H 109.00 ?
C134 C133 H13G 111.00 ?
C232 C233 C234 103(3) ?
C132 C133 H13G 111.00 ?
O2 C134 H13J 111.00 ?
C133 C134 H13I 111.00 ?
O2A C234 C233 107(3) y
H13I C134 H13J 109.00 ?
O2 C134 H13I 110.00 ?
C133 C134 H13J 110.00 ?
H23C C231 H23D 109.00 ?
C232 C231 H23D 110.00 ?
C232 C231 H23C 111.00 ?
O2A C231 H23C 110.00 ?
O2A C231 H23D 110.00 ?
C231 C232 H23F 111.00 ?
C231 C232 H23E 110.00 ?
C233 C232 H23F 111.00 ?
C233 C232 H23E 110.00 ?
H23E C232 H23F 108.00 ?
C232 C233 H23G 110.00 ?
C234 C233 H23G 111.00 ?
H23G C233 H23H 109.00 ?
C234 C233 H23H 112.00 ?
C232 C233 H23H 111.00 ?
H23I C234 H23J 108.00 ?
O2A C234 H23I 111.00 ?
C233 C234 H23I 110.00 ?
O2A C234 H23J 111.00 ?
C233 C234 H23J 110.00 ?
O3 C135 C136 109.9(17) y
C135 C136 C137 101.8(14) ?
C136 C137 C138 104(2) ?
O3 C138 C137 110.3(15) y
O3A C235 C236 107(2) y
C136 C135 H13K 110.00 ?
H13K C135 H13L 108.00 ?
O3 C135 H13K 110.00 ?
O3 C135 H13L 110.00 ?
C136 C135 H13L 110.00 ?
C137 C136 H13N 111.00 ?
C135 C136 H13N 112.00 ?
C135 C136 H13M 112.00 ?
C137 C136 H13M 111.00 ?
C235 C236 C237 101(2) ?
H13M C136 H13N 109.00 ?
C138 C137 H13P 111.00 ?
C236 C237 C238 106(2) ?
C138 C137 H13O 111.00 ?
C136 C137 H13O 111.00 ?
H13O C137 H13P 109.00 ?
C136 C137 H13P 111.00 ?
O3A C238 C237 112(2) y
C137 C138 H13Q 110.00 ?
C137 C138 H13R 109.00 ?
H13Q C138 H13R 108.00 ?
O3 C138 H13R 110.00 ?
O3 C138 H13Q 110.00 ?
O3A C235 H23K 110.00 ?
C236 C235 H23L 110.00 ?
H23K C235 H23L 109.00 ?
O3A C235 H23L 110.00 ?
C236 C235 H23K 111.00 ?
C235 C236 H23N 112.00 ?
H23M C236 H23N 110.00 ?
C237 C236 H23M 111.00 ?
C237 C236 H23N 112.00 ?
C235 C236 H23M 111.00 ?
H23O C237 H23P 109.00 ?
C238 C237 H23O 111.00 ?
C236 C237 H23P 110.00 ?
C236 C237 H23O 110.00 ?
C238 C237 H23P 111.00 ?
H23Q C238 H23R 108.00 ?
O3A C238 H23R 109.00 ?
C237 C238 H23Q 109.00 ?
C237 C238 H23R 109.00 ?
O3A C238 H23Q 110.00 ?
O5 C143 C144 107.0(13) y
C143 C144 C145 101.1(15) ?
C144 C145 C146 105.7(17) ?
O5 C146 C145 111.2(12) y
O5A C243 C244 106.9(10) y
C144 C143 H14H 110.00 ?
O5 C143 H14G 110.00 ?
C144 C143 H14G 110.00 ?
O5 C143 H14H 110.00 ?
H14G C143 H14H 109.00 ?
C143 C144 H14I 112.00 ?
C143 C144 H14J 112.00 ?
C145 C144 H14J 112.00 ?
C145 C144 H14I 112.00 ?
C243 C244 C245 100.9(15) ?
H14I C144 H14J 109.00 ?
C146 C145 H14L 111.00 ?
H14K C145 H14L 109.00 ?
C244 C245 C246 103.3(15) ?
C146 C145 H14K 111.00 ?
C144 C145 H14K 111.00 ?
C144 C145 H14L 111.00 ?
C145 C146 H14N 109.00 ?
O5A C246 C245 105.6(12) y
O5 C146 H14N 109.00 ?
O5 C146 H14M 109.00 ?
H14M C146 H14N 108.00 ?
C145 C146 H14M 109.00 ?
O5A C243 H24H 110.00 ?
C244 C243 H24G 110.00 ?
C244 C243 H24H 110.00 ?
H24G C243 H24H 108.00 ?
O5A C243 H24G 110.00 ?
C243 C244 H24J 112.00 ?
C245 C244 H24I 112.00 ?
H24I C244 H24J 109.00 ?
C243 C244 H24I 112.00 ?
C245 C244 H24J 112.00 ?
C244 C245 H24L 111.00 ?
C246 C245 H24K 111.00 ?
C244 C245 H24K 111.00 ?
C246 C245 H24L 111.00 ?
H24K C245 H24L 109.00 ?
C245 C246 H24N 111.00 ?
C245 C246 H24M 111.00 ?
O5A C246 H24M 111.00 ?
H24M C246 H24N 109.00 ?
O5A C246 H24N 111.00 ?
O6 C147 C148 109.9(9) y
C147 C148 C149 101.8(10) ?
C148 C149 C150 104.9(12) ?
O6 C150 C149 112(2) y
C148 C147 H14P 110.00 ?
C148 C147 H14O 110.00 ?
O6 C147 H14P 110.00 ?
O6 C147 H14O 110.00 ?
O6A C247 C248 109.7(19) y
H14O C147 H14P 108.00 ?
C149 C148 H14Q 111.00 ?
C149 C148 H14R 112.00 ?
C147 C148 H14Q 111.00 ?
H14Q C148 H14R 109.00 ?
C147 C148 H14R 111.00 ?
C247 C248 C249 102(2) ?
C150 C149 H14T 111.00 ?
C150 C149 H14S 111.00 ?
C148 C149 H14S 111.00 ?
H14S C149 H14T 109.00 ?
C148 C149 H14T 111.00 ?
C248 C249 C250 105(2) ?
C149 C150 H15B 109.00 ?
O6 C150 H15B 109.00 ?
O6 C150 H15A 109.00 ?
C149 C150 H15A 109.00 ?
H15A C150 H15B 108.00 ?
O6A C250 C249 112(3) y
H24A C247 H24B 108.00 ?
O6A C247 H24A 110.00 ?
C248 C247 H24B 110.00 ?
C248 C247 H24A 110.00 ?
O6A C247 H24B 110.00 ?
H24C C248 H24D 109.00 ?
C247 C248 H24D 111.00 ?
C249 C248 H24C 112.00 ?
C247 C248 H24C 111.00 ?
C249 C248 H24D 112.00 ?
C248 C249 H24F 111.00 ?
C250 C249 H24E 111.00 ?
C250 C249 H24F 111.00 ?
H24E C249 H24F 109.00 ?
C248 C249 H24E 111.00 ?
O6A C250 H25A 109.00 ?
O6A C250 H25B 110.00 ?
C249 C250 H25A 109.00 ?
H25A C250 H25B 108.00 ?
C249 C250 H25B 109.00 ?
O9 C159 C160 107.7(14) y
C159 C160 C161 101.9(17) ?
C160 C161 C162 105.7(15) ?
O9 C162 C161 112(2) y
C160 C159 H15S 110.00 ?
H15S C159 H15T 109.00 ?
O9 C159 H15T 110.00 ?
O9A C259 C260 107.8(18) y
C160 C159 H15T 110.00 ?
O9 C159 H15S 110.00 ?
C159 C160 H16A 112.00 ?
C161 C160 H16A 111.00 ?
C161 C160 H16B 111.00 ?
H16A C160 H16B 109.00 ?
C159 C160 H16B 111.00 ?
C259 C260 C261 96(2) ?
H16C C161 H16D 109.00 ?
C260 C261 C262 117(3) ?
C162 C161 H16D 110.00 ?
C162 C161 H16C 111.00 ?
C160 C161 H16D 111.00 ?
C160 C161 H16C 111.00 ?
O9 C162 H16F 109.00 ?
C161 C162 H16F 110.00 ?
C161 C162 H16E 109.00 ?
O9 C162 H16E 109.00 ?
O9A C262 C261 100(3) y
H16E C162 H16F 108.00 ?
C260 C259 H25C 110.00 ?
C260 C259 H25D 110.00 ?
H25C C259 H25D 108.00 ?
O9A C259 H25C 110.00 ?
O9A C259 H25D 110.00 ?
H26A C260 H26B 110.00 ?
C261 C260 H26B 113.00 ?
C259 C260 H26A 113.00 ?
C259 C260 H26B 113.00 ?
C261 C260 H26A 112.00 ?
C260 C261 H26D 108.00 ?
C262 C261 H26D 108.00 ?
C262 C261 H26C 108.00 ?
C260 C261 H26C 108.00 ?
H26C C261 H26D 108.00 ?
H26E C262 H26F 109.00 ?
C261 C262 H26F 112.00 ?
O9A C262 H26F 112.00 ?
C261 C262 H26E 112.00 ?
O9A C262 H26E 112.00 ?
O10 C163 C164 108.6(16) y
C163 C164 C165 101.6(16) ?
C164 C165 C166 106.3(19) ?
O10 C166 C165 111.8(18) y
O10A C263 C264 108(3) y
H16G C163 H16H 108.00 ?
C164 C163 H16H 110.00 ?
O10 C163 H16G 110.00 ?
C164 C163 H16G 110.00 ?
O10 C163 H16H 110.00 ?
C165 C164 H16J 111.00 ?
C163 C164 H16J 111.00 ?
C163 C164 H16I 111.00 ?
C263 C264 C265 102(3) ?
H16I C164 H16J 109.00 ?
C165 C164 H16I 111.00 ?
C264 C265 C266 106(3) ?
C166 C165 H16K 111.00 ?
C164 C165 H16L 110.00 ?
C166 C165 H16L 111.00 ?
H16K C165 H16L 109.00 ?
C164 C165 H16K 110.00 ?
O10 C166 H16M 109.00 ?
H16M C166 H16N 108.00 ?
C165 C166 H16N 109.00 ?
O10A C266 C265 111(3) y
C165 C166 H16M 109.00 ?
O10 C166 H16N 109.00 ?
H26G C263 H26H 109.00 ?
O10A C263 H26H 110.00 ?
C264 C263 H26H 110.00 ?
O10A C263 H26G 110.00 ?
C264 C263 H26G 110.00 ?
C263 C264 H26I 111.00 ?
H26I C264 H26J 109.00 ?
C263 C264 H26J 112.00 ?
C265 C264 H26I 111.00 ?
C265 C264 H26J 111.00 ?
C264 C265 H26L 111.00 ?
H26K C265 H26L 109.00 ?
C266 C265 H26L 110.00 ?
C264 C265 H26K 111.00 ?
C266 C265 H26K 111.00 ?
O10A C266 H26M 109.00 ?
H26M C266 H26N 108.00 ?
C265 C266 H26N 110.00 ?
C265 C266 H26M 110.00 ?
O10A C266 H26N 109.00 ?
O11 C167 C168 109.1(14) y
C167 C168 C169 102.5(15) ?
C168 C169 C170 105.5(16) ?
O11 C170 C169 110.8(16) y
O11 C167 H16P 110.00 ?
C168 C167 H16O 110.00 ?
H16O C167 H16P 108.00 ?
C168 C167 H16P 110.00 ?
O11A C267 C270 109(3) y
O11 C167 H16O 110.00 ?
C169 C168 H16R 111.00 ?
C167 C168 H16R 111.00 ?
C169 C168 H16Q 111.00 ?
C269 C268 C270 105(3) ?
H16Q C168 H16R 109.00 ?
C167 C168 H16Q 111.00 ?
C170 C169 H16T 111.00 ?
O11A C269 C268 111(4) y
C168 C169 H16S 111.00 ?
C170 C169 H16S 111.00 ?
C168 C169 H16T 111.00 ?
H16S C169 H16T 109.00 ?
H17A C170 H17B 108.00 ?
C169 C170 H17A 109.00 ?
O11 C170 H17B 109.00 ?
C267 C270 C268 103(3) ?
C169 C170 H17B 110.00 ?
O11 C170 H17A 109.00 ?
C270 C267 H26O 110.00 ?
C270 C267 H26P 110.00 ?
O11A C267 H26O 110.00 ?
H26O C267 H26P 108.00 ?
O11A C267 H26P 110.00 ?
C269 C268 H26R 110.00 ?
C270 C268 H26R 110.00 ?
H26Q C268 H26R 109.00 ?
C270 C268 H26Q 111.00 ?
C269 C268 H26Q 111.00 ?
O11A C269 H26S 109.00 ?
C268 C269 H26T 110.00 ?
C268 C269 H26S 109.00 ?
H26S C269 H26T 108.00 ?
O11A C269 H26T 110.00 ?
H27A C270 H27B 109.00 ?
C268 C270 H27B 111.00 ?
C267 C270 H27A 111.00 ?
C268 C270 H27A 111.00 ?
C267 C270 H27B 111.00 ?
O12 C171 C172 109(2) y
C171 C172 C173 102.5(19) ?
C172 C173 C174 105(2) ?
O12 C174 C173 110(2) y
O12 C171 H17D 110.00 ?
H17C C171 H17D 108.00 ?
O12A C271 C272 109(4) y
C172 C171 H17C 110.00 ?
O12 C171 H17C 110.00 ?
C172 C171 H17D 110.00 ?
C171 C172 H17E 111.00 ?
H17E C172 H17F 109.00 ?
C173 C172 H17F 111.00 ?
C171 C172 H17F 111.00 ?
C173 C172 H17E 111.00 ?
C271 C272 C273 103(3) ?
H17G C173 H17H 109.00 ?
C272 C273 C274 105(3) ?
C174 C173 H17H 111.00 ?
C174 C173 H17G 111.00 ?
C172 C173 H17H 111.00 ?
C172 C173 H17G 111.00 ?
C173 C174 H17I 110.00 ?
C173 C174 H17J 110.00 ?
O12 C174 H17J 110.00 ?
O12 C174 H17I 110.00 ?
H17I C174 H17J 108.00 ?
O12A C274 C273 110(3) y
O4 C139 C140 113.0(15) y
O4A C140 C141 60.8(16) y
O4A C140 C139 134(2) y
C139 C140 C141 102.7(14) ?
O4A C141 C142 131.7(19) y
C140 C141 C142 100.3(13) ?
O4 C142 C141 104.5(15) y
C272 C271 H27C 110.00 ?
H27C C271 H27D 108.00 ?
O12A C271 H27D 110.00 ?
C272 C271 H27D 110.00 ?
O12A C271 H27C 109.00 ?
C273 C272 H27E 111.00 ?
C271 C272 H27F 112.00 ?
C273 C272 H27F 111.00 ?
H27E C272 H27F 109.00 ?
C271 C272 H27E 111.00 ?
H27G C273 H27H 109.00 ?
C272 C273 H27G 110.00 ?
C274 C273 H27H 111.00 ?
C274 C273 H27G 111.00 ?
C272 C273 H27H 111.00 ?
C273 C274 H27I 110.00 ?
H27I C274 H27J 108.00 ?
O12A C274 H27J 110.00 ?
O12A C274 H27I 109.00 ?
C273 C274 H27J 110.00 ?
O4 C139 H13T 109.00 ?
O4 C139 H13S 109.00 ?
C140 C139 H13T 109.00 ?
H13S C139 H13T 108.00 ?
C140 C139 H13S 109.00 ?
C141 C140 H14A 111.00 ?
C141 C140 H14B 111.00 ?
O4A C140 H14B 52.00 ?
C139 C140 H14B 111.00 ?
H14A C140 H14B 109.00 ?
O4A C140 H14A 115.00 ?
C139 C140 H14A 111.00 ?
H14C C141 H14D 109.00 ?
C142 C141 H14D 112.00 ?
C140 C141 H14C 112.00 ?
C142 C141 H14C 112.00 ?
O4A C141 H14C 72.00 ?
O4A C141 H14D 112.00 ?
C140 C141 H14D 112.00 ?
C141 C142 H14E 111.00 ?
C141 C142 H14F 111.00 ?
O4 C142 H14E 111.00 ?
H14E C142 H14F 109.00 ?
O4 C142 H14F 111.00 ?
O7 C151 C152 106.6(12) y
C151 C152 C153 101.2(13) ?
C152 C153 C154 108.5(14) ?
O7 C154 C153 106.7(13) y
O7 C151 H15D 111.00 ?
C152 C151 H15D 110.00 ?
H15C C151 H15D 109.00 ?
C152 C151 H15C 110.00 ?
O7 C151 H15C 110.00 ?
C151 C152 H15F 111.00 ?
C153 C152 H15F 111.00 ?
H15E C152 H15F 109.00 ?
C151 C152 H15E 112.00 ?
C153 C152 H15E 112.00 ?
C154 C153 H15G 110.00 ?
C152 C153 H15G 110.00 ?
C152 C153 H15H 110.00 ?
H15G C153 H15H 108.00 ?
C154 C153 H15H 110.00 ?
O7 C154 H15J 110.00 ?
C153 C154 H15J 110.00 ?
H15I C154 H15J 109.00 ?
C153 C154 H15I 110.00 ?
O7 C154 H15I 110.00 ?
O8 C155 C156 104.5(12) y
C155 C156 C157 106.3(13) ?
C156 C157 C158 110.5(17) ?
O8 C158 C157 108.1(15) y
O8 C155 H15K 111.00 ?
O8 C155 H15L 111.00 ?
C156 C155 H15L 111.00 ?
H15K C155 H15L 109.00 ?
C156 C155 H15K 111.00 ?
C155 C156 H15N 110.00 ?
C157 C156 H15M 110.00 ?
C157 C156 H15N 110.00 ?
H15M C156 H15N 109.00 ?
C155 C156 H15M 110.00 ?
C156 C157 H15P 110.00 ?
C158 C157 H15O 109.00 ?
C156 C157 H15O 110.00 ?
H15O C157 H15P 108.00 ?
C158 C157 H15P 110.00 ?
O8 C158 H15Q 110.00 ?
O8 C158 H15R 110.00 ?
C157 C158 H15R 110.00 ?
H15Q C158 H15R 108.00 ?
C157 C158 H15Q 110.00 ?
O13 C175 C176 109.0(17) y
C175 C176 C177 102.3(16) ?
C176 C177 C178 105.9(16) ?
O13 C178 C177 110.9(18) y
O13 C175 H17K 110.00 ?
O13 C175 H17L 110.00 ?
C176 C175 H17K 110.00 ?
C176 C175 H17L 110.00 ?
H17K C175 H17L 108.00 ?
C175 C176 H17M 111.00 ?
C175 C176 H17N 112.00 ?
C177 C176 H17M 111.00 ?
C177 C176 H17N 111.00 ?
H17M C176 H17N 109.00 ?
C176 C177 H17O 111.00 ?
C176 C177 H17P 111.00 ?
C178 C177 H17O 110.00 ?
C178 C177 H17P 111.00 ?
H17O C177 H17P 109.00 ?
O13 C178 H17Q 110.00 ?
O13 C178 H17R 109.00 ?
C177 C178 H17Q 109.00 ?
C177 C178 H17R 109.00 ?
H17Q C178 H17R 108.00 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C130 1.416(16) y
O1 C127 1.423(8) y
O1A C230 1.41(4) y
O1A C227 1.42(4) y
O2 C131 1.44(4) y
O2 C134 1.52(4) y
O2A C234 1.51(6) y
O2A C231 1.45(6) y
O3 C138 1.41(2) y
O3 C135 1.42(2) y
O3A C238 1.41(3) y
O3A C235 1.42(3) y
O5 C146 1.411(17) y
O5 C143 1.42(2) y
O5A C243 1.416(14) y
O5A C246 1.398(13) y
N1 C85 1.4105 y
N1 C1 1.4525 y
N1 C43 1.3948 y
O6 C150 1.41(2) y
O6 C147 1.411(16) y
O6A C250 1.40(4) y
O6A C247 1.41(3) y
O9 C159 1.42(2) y
O9 C162 1.41(3) y
O9A C259 1.42(3) y
O9A C262 1.50(4) y
O10 C166 1.41(3) y
O10 C163 1.42(3) y
O10A C266 1.41(4) y
O10A C263 1.43(5) y
O11 C170 1.41(2) y
O11 C167 1.42(2) y
O11A C267 1.42(5) y
O11A C269 1.41(7) y
O12 C171 1.42(3) y
O12 C174 1.42(4) y
O12A C271 1.43(7) y
O12A C274 1.42(4) y
C1 C2 1.387(9) ?
C1 C6 1.385(12) ?
C2 C3 1.385(12) ?
C3 C4 1.388(12) ?
O4 C142 1.40(3) y
C4 C5 1.395(10) ?
C4 C7 1.508(11) ?
O4 C139 1.36(3) y
O4A C141 1.40(3) y
O4A C140 1.10(3) y
C5 C6 1.379(12) ?
C7 C8 1.408(11) ?
C7 C12 1.399(11) ?
C8 C13 1.502(11) ?
C8 C9 1.401(11) ?
C9 C19 1.489(11) ?
C9 C10 1.412(11) ?
C10 C25 1.510(11) ?
C10 C11 1.395(11) ?
C11 C12 1.404(11) ?
C11 C31 1.498(11) ?
C12 C37 1.516(11) ?
C13 C14 1.379(13) ?
C13 C18 1.386(10) ?
C14 C15 1.403(17) ?
C15 C16 1.342(15) ?
C16 C17 1.352(14) ?
C17 C18 1.406(14) ?
C19 C20 1.402(12) ?
C19 C24 1.375(13) ?
C20 C21 1.384(15) ?
C21 C22 1.365(15) ?
C22 C23 1.355(16) ?
C23 C24 1.397(15) ?
C25 C26 1.391(11) ?
C25 C30 1.379(13) ?
C26 C27 1.379(15) ?
C27 C28 1.391(16) ?
C28 C29 1.342(16) ?
C29 C30 1.385(14) ?
C31 C32 1.357(11) ?
C31 C36 1.414(12) ?
C32 C33 1.391(14) ?
C33 C34 1.383(16) ?
C34 C35 1.365(15) ?
C35 C36 1.388(15) ?
C37 C42 1.389(11) ?
C37 C38 1.370(12) ?
C38 C39 1.384(14) ?
C39 C40 1.378(15) ?
C40 C41 1.347(14) ?
C41 C42 1.404(11) ?
C43 C44 1.398(11) ?
C43 C48 1.400(12) ?
C44 C45 1.389(11) ?
C45 C46 1.379(11) ?
C46 C49 1.503(11) ?
C46 C47 1.392(11) ?
C47 C48 1.380(11) ?
C49 C54 1.401(11) ?
C49 C50 1.418(12) ?
C50 C51 1.417(11) ?
C50 C55 1.480(11) ?
C51 C52 1.410(11) ?
C51 C61 1.494(13) ?
C52 C53 1.381(12) ?
C52 C67 1.506(11) ?
C53 C73 1.497(11) ?
C53 C54 1.423(11) ?
C54 C79 1.478(12) ?
C55 C60 1.383(13) ?
C55 C56 1.384(11) ?
C56 C57 1.376(14) ?
C57 C58 1.357(16) ?
C58 C59 1.357(16) ?
C59 C60 1.373(15) ?
C61 C66 1.394(13) ?
C61 C62 1.383(11) ?
C62 C63 1.401(14) ?
C63 C64 1.388(14) ?
C64 C65 1.367(15) ?
C65 C66 1.382(14) ?
C67 C68 1.397(10) ?
C67 C72 1.375(10) ?
C68 C69 1.372(12) ?
C69 C70 1.372(11) ?
C70 C71 1.367(11) ?
C71 C72 1.395(11) ?
C73 C78 1.386(10) ?
C73 C74 1.372(11) ?
C74 C75 1.397(14) ?
C75 C76 1.365(14) ?
C76 C77 1.378(15) ?
C77 C78 1.389(14) ?
C79 C84 1.398(12) ?
C79 C80 1.399(13) ?
C80 C81 1.371(14) ?
C81 C82 1.388(16) ?
C82 C83 1.345(17) ?
C83 C84 1.403(15) ?
C85 C86 1.378(11) ?
C85 C90 1.366(10) ?
C86 C87 1.381(11) ?
C87 C88 1.361(9) ?
C88 C96 1.503(11) ?
C88 C89 1.382(11) ?
C89 C90 1.399(11) ?
C91 C92 1.409(11) ?
C91 C97 1.490(12) ?
C91 C96 1.405(12) ?
C92 C93 1.395(12) ?
C92 C103 1.488(12) ?
C93 C94 1.393(12) ?
C93 C109 1.529(11) ?
C94 C115 1.514(12) ?
C94 C95 1.403(11) ?
C95 C96 1.406(12) ?
C95 C121 1.490(12) ?
C97 C98 1.389(10) ?
C97 C102 1.385(12) ?
C98 C99 1.356(13) ?
C99 C100 1.357(14) ?
C100 C101 1.372(11) ?
C101 C102 1.388(13) ?
C2 H2 0.9500 ?
C3 H3 0.9500 ?
C103 C108 1.400(11) ?
C103 C104 1.395(11) ?
C104 C105 1.397(13) ?
O4A H14B 0.9200 ?
C5 H5 0.9500 ?
C105 C106 1.390(12) ?
C6 H6 0.9500 ?
C106 C107 1.387(11) ?
C107 C108 1.381(12) ?
C109 C110 1.380(12) ?
C109 C114 1.378(11) ?
C110 C111 1.377(12) ?
C111 C112 1.369(17) ?
C112 C113 1.323(17) ?
C113 C114 1.413(14) ?
C14 H14 0.9500 ?
C115 C116 1.372(12) ?
C15 H15 0.9500 ?
C115 C120 1.379(10) ?
C16 H16 0.9500 ?
C116 C117 1.398(14) ?
C117 C118 1.358(15) ?
C17 H17 0.9500 ?
C18 H18 0.9500 ?
C118 C119 1.360(15) ?
C119 C120 1.405(14) ?
C20 H20 0.9500 ?
C121 C126 1.361(10) ?
C121 C122 1.365(12) ?
C21 H21 0.9500 ?
C22 H22 0.9500 ?
C122 C123 1.389(16) ?
C123 C124 1.367(16) ?
C23 H23 0.9500 ?
C124 C125 1.354(16) ?
C24 H24 0.9500 ?
C125 C126 1.406(14) ?
C26 H26 0.9500 ?
C27 H27 0.9500 ?
C28 H28 0.9500 ?
C29 H29 0.9500 ?
C30 H30 0.9500 ?
C32 H32 0.9500 ?
C33 H33 0.9500 ?
C34 H34 0.9500 ?
C35 H35 0.9500 ?
C36 H36 0.9500 ?
C38 H38 0.9500 ?
C39 H39 0.9500 ?
C40 H40 0.9500 ?
C41 H41 0.9500 ?
C42 H42 0.9500 ?
C44 H44 0.9500 ?
C45 H45 0.9500 ?
C47 H47 0.9500 ?
C48 H48 0.9500 ?
C56 H56 0.9500 ?
C57 H57 0.9500 ?
C58 H58 0.9500 ?
C59 H59 0.9500 ?
C60 H60 0.9500 ?
C62 H62 0.9500 ?
C63 H63 0.9500 ?
C64 H64 0.9500 ?
C65 H65 0.9500 ?
C66 H66 0.9500 ?
C68 H68 0.9500 ?
C69 H69 0.9500 ?
C70 H70 0.9500 ?
C71 H71 0.9500 ?
C72 H72 0.9500 ?
C74 H74 0.9500 ?
C75 H75 0.9500 ?
C76 H76 0.9500 ?
C77 H77 0.9500 ?
C78 H78 0.9500 ?
C80 H80 0.9500 ?
C81 H81 0.9500 ?
C82 H82 0.9500 ?
C83 H83 0.9500 ?
C84 H84 0.9500 ?
C86 H86 0.9500 ?
C87 H87 0.9500 ?
C89 H89 0.9500 ?
C90 H90 0.9500 ?
C98 H98 0.9500 ?
C99 H99 0.9500 ?
C100 H100 0.9500 ?
C101 H101 0.9500 ?
C102 H102 0.9500 ?
C104 H104 0.9500 ?
C105 H105 0.9500 ?
C106 H106 0.9500 ?
O7 C151 1.419(19) y
O7 C154 1.395(18) y
C107 H107 0.9500 ?
C108 H108 0.9500 ?
C110 H110 0.9500 ?
C111 H111 0.9500 ?
C112 H112 0.9500 ?
C113 H113 0.9500 ?
C114 H114 0.9500 ?
C116 H116 0.9500 ?
C117 H117 0.9500 ?
C118 H118 0.9500 ?
C119 H119 0.9500 ?
C120 H120 0.9500 ?
C122 H122 0.9500 ?
C123 H123 0.9500 ?
C124 H124 0.9500 ?
C125 H125 0.9500 ?
C126 H126 0.9500 ?
C127 C128 1.529(15) ?
C128 C129 1.54(2) ?
C129 C130 1.44(2) ?
O8 C158 1.49(3) y
O8 C155 1.407(18) y
C227 C228 1.53(4) ?
C127 H12A 0.9900 ?
C127 H12B 0.9900 ?
C228 C229 1.54(4) ?
C128 H12C 0.9900 ?
C128 H12D 0.9900 ?
C129 H12E 0.9900 ?
C129 H12F 0.9900 ?
C229 C230 1.44(4) ?
C130 H13B 0.9900 ?
C130 H13A 0.9900 ?
C227 H22A 0.9900 ?
C227 H22B 0.9900 ?
C228 H22D 0.9900 ?
C228 H22C 0.9900 ?
C229 H22E 0.9900 ?
C229 H22F 0.9900 ?
C230 H23B 0.9900 ?
C230 H23A 0.9900 ?
C131 C132 1.47(4) ?
C132 C133 1.53(4) ?
C133 C134 1.47(4) ?
O13 C175 1.42(3) y
O13 C178 1.42(3) y
C231 C232 1.46(6) ?
C131 H13D 0.9900 ?
C131 H13C 0.9900 ?
C132 H13F 0.9900 ?
C132 H13E 0.9900 ?
C232 C233 1.53(5) ?
C133 H13G 0.9900 ?
C133 H13H 0.9900 ?
C233 C234 1.46(6) ?
C134 H13I 0.9900 ?
C134 H13J 0.9900 ?
C231 H23D 0.9900 ?
C231 H23C 0.9800 ?
C232 H23E 0.9900 ?
C232 H23F 0.9900 ?
C233 H23H 0.9800 ?
C233 H23G 0.9900 ?
C234 H23J 0.9900 ?
C234 H23I 0.9900 ?
C135 C136 1.53(4) ?
C136 C137 1.55(4) ?
C137 C138 1.44(3) ?
C135 H13L 0.9900 ?
C135 H13K 0.9900 ?
C235 C236 1.54(4) ?
C136 H13N 0.9900 ?
C136 H13M 0.9900 ?
C236 C237 1.55(5) ?
C137 H13O 0.9900 ?
C137 H13P 0.9900 ?
C237 C238 1.44(3) ?
C138 H13Q 0.9900 ?
C138 H13R 0.9900 ?
C235 H23L 0.9900 ?
C235 H23K 0.9900 ?
C236 H23N 0.9800 ?
C236 H23M 0.9900 ?
C237 H23P 0.9900 ?
C237 H23O 0.9900 ?
C238 H23Q 0.9900 ?
C238 H23R 0.9900 ?
C143 C144 1.55(2) ?
C144 C145 1.55(3) ?
C145 C146 1.44(2) ?
C243 C244 1.55(2) ?
C143 H14H 0.9900 ?
C143 H14G 0.9900 ?
C144 H14J 0.9900 ?
C144 H14I 0.9900 ?
C244 C245 1.55(2) ?
C145 H14K 0.9900 ?
C245 C246 1.55(3) ?
C145 H14L 0.9900 ?
C146 H14N 0.9900 ?
C146 H14M 0.9900 ?
C243 H24H 0.9900 ?
C243 H24G 0.9900 ?
C244 H24I 0.9900 ?
C244 H24J 0.9900 ?
C245 H24L 0.9900 ?
C245 H24K 0.9900 ?
C246 H24M 0.9900 ?
C246 H24N 0.9900 ?
C147 C148 1.535(15) ?
C148 C149 1.54(2) ?
C149 C150 1.44(3) ?
C147 H14P 0.9900 ?
C247 C248 1.53(3) ?
C147 H14O 0.9900 ?
C248 C249 1.54(3) ?
C148 H14R 0.9900 ?
C148 H14Q 0.9900 ?
C249 C250 1.44(5) ?
C149 H14S 0.9900 ?
C149 H14T 0.9900 ?
C150 H15B 0.9900 ?
C150 H15A 0.9900 ?
C247 H24B 0.9900 ?
C247 H24A 0.9900 ?
C248 H24C 0.9900 ?
C248 H24D 0.9900 ?
C249 H24F 0.9900 ?
C249 H24E 0.9900 ?
C250 H25B 0.9900 ?
C250 H25A 0.9900 ?
C159 C160 1.54(3) ?
C160 C161 1.54(3) ?
C161 C162 1.44(4) ?
C259 C260 1.54(3) ?
C159 H15S 0.9900 ?
C159 H15T 0.9900 ?
C160 H16A 0.9900 ?
C260 C261 1.40(5) ?
C160 H16B 0.9900 ?
C261 C262 1.47(5) ?
C161 H16C 0.9900 ?
C161 H16D 0.9900 ?
C162 H16F 0.9800 ?
C162 H16E 0.9900 ?
C259 H25D 0.9900 ?
C259 H25C 0.9900 ?
C260 H26B 0.9900 ?
C260 H26A 0.9900 ?
C261 H26C 0.9900 ?
C261 H26D 0.9800 ?
C262 H26E 0.9900 ?
C262 H26F 0.9900 ?
C163 C164 1.54(3) ?
C164 C165 1.54(3) ?
C165 C166 1.44(3) ?
C263 C264 1.53(6) ?
C163 H16G 0.9900 ?
C163 H16H 0.9900 ?
C164 H16J 0.9900 ?
C164 H16I 0.9900 ?
C264 C265 1.54(6) ?
C165 H16L 0.9900 ?
C165 H16K 0.9900 ?
C265 C266 1.44(6) ?
C166 H16N 0.9900 ?
C166 H16M 0.9900 ?
C263 H26G 0.9900 ?
C263 H26H 0.9900 ?
C264 H26I 1.0000 ?
C264 H26J 0.9900 ?
C265 H26L 0.9900 ?
C265 H26K 0.9900 ?
C266 H26M 0.9900 ?
C266 H26N 0.9900 ?
C167 C168 1.54(2) ?
C168 C169 1.54(3) ?
C169 C170 1.44(3) ?
C267 C270 1.54(5) ?
C167 H16O 0.9900 ?
C167 H16P 0.9900 ?
C168 H16Q 0.9900 ?
C268 C270 1.55(7) ?
C168 H16R 0.9900 ?
C268 C269 1.44(7) ?
C169 H16T 0.9900 ?
C169 H16S 0.9900 ?
C170 H17B 0.9900 ?
C170 H17A 0.9900 ?
C267 H26P 0.9900 ?
C267 H26O 0.9900 ?
C268 H26R 0.9900 ?
C268 H26Q 0.9900 ?
C269 H26S 0.9900 ?
C269 H26T 0.9900 ?
C270 H27B 0.9900 ?
C270 H27A 0.9900 ?
C171 C172 1.53(3) ?
C172 C173 1.54(4) ?
C173 C174 1.44(4) ?
C171 H17D 0.9900 ?
C271 C272 1.53(6) ?
C171 H17C 0.9900 ?
C172 H17E 0.9900 ?
C272 C273 1.55(6) ?
C172 H17F 0.9900 ?
C173 H17H 0.9900 ?
C173 H17G 0.9900 ?
C273 C274 1.44(4) ?
C174 H17J 0.9900 ?
C174 H17I 0.9900 ?
C139 C140 1.36(2) ?
C140 C141 1.55(2) ?
C141 C142 1.50(3) ?
C271 H27D 0.9900 ?
C271 H27C 0.9900 ?
C272 H27E 0.9900 ?
C272 H27F 0.9900 ?
C273 H27G 0.9900 ?
C273 H27H 0.9900 ?
C274 H27I 0.9900 ?
C274 H27J 0.9900 ?
C139 H13S 0.9900 ?
C139 H13T 0.9900 ?
C140 H14B 0.9900 ?
C140 H14A 0.9900 ?
C141 H14D 0.9900 ?
C141 H14C 0.9900 ?
C142 H14E 0.9900 ?
C142 H14F 0.9900 ?
C151 C152 1.532(19) ?
C152 C153 1.47(3) ?
C153 C154 1.48(2) ?
C151 H15C 0.9900 ?
C151 H15D 0.9900 ?
C152 H15F 0.9900 ?
C152 H15E 0.9900 ?
C153 H15G 0.9900 ?
C153 H15H 0.9900 ?
C154 H15I 0.9900 ?
C154 H15J 0.9900 ?
C155 C156 1.52(2) ?
C156 C157 1.42(2) ?
C157 C158 1.35(2) ?
C155 H15K 0.9900 ?
C155 H15L 0.9900 ?
C156 H15N 0.9900 ?
C156 H15M 0.9900 ?
C157 H15O 0.9900 ?
C157 H15P 0.9900 ?
C158 H15R 0.9900 ?
C158 H15Q 0.9900 ?
C175 C176 1.53(3) ?
C176 C177 1.54(3) ?
C177 C178 1.44(3) ?
C175 H17K 0.9900 ?
C175 H17L 0.9900 ?
C176 H17M 0.9900 ?
C176 H17N 0.9900 ?
C177 H17O 0.9900 ?
C177 H17P 0.9900 ?
C178 H17Q 0.9900 ?
C178 H17R 0.9900 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O1 C87 3.416(9) .
O1 C86 3.410(10) .
O5A C161 3.19(2) .
O7 C244 3.05(2) .
O7 C144 3.30(2) .
O9A C42 3.36(3) .
O9A C5 3.27(2) .
O1 H86 2.8500 .
O1 H87 2.8600 .
O1 H70 2.7700 2_464
O1A H70 2.8500 2_464
O3 H16 2.9200 .
O3 H17O 2.8900 .
O3A H106 2.8500 2_565
O4 H26 2.9200 1_545
O4 H20 2.9100 1_545
O4A H3 2.8500 1_545
O5 H27 2.7600 1_545
O5A H16D 2.5800 .
O6 H2 2.8900 .
O7 H14I 2.5600 .
O7 H21 2.7100 1_545
O7 H24J 2.3800 .
O9 H27E 2.7000 1_455
O9 H42 2.7900 .
O9A H5 2.4300 .
O9A H42 2.4600 .
O11 H62 2.7500 1_545
C2 C150 3.48(3) .
C2 C44 3.100(11) .
C3 C18 3.555(12) .
C3 C13 3.033(12) .
C3 C14 3.360(14) .
C4 C18 3.236(11) .
C4 C42 3.565(12) .
C5 C42 3.370(12) .
C5 C37 3.414(11) .
C5 O9A 3.27(2) .
C6 C86 3.334(14) .
C13 C24 3.598(13) .
C13 C20 3.389(12) .
C13 C3 3.033(12) .
C14 C19 3.324(14) .
C14 C20 3.247(16) .
C14 C3 3.360(14) .
C18 C3 3.555(12) .
C18 C4 3.236(11) .
C19 C14 3.324(14) .
C19 C26 3.277(12) .
C20 C13 3.389(12) .
C20 C243 3.589(13) 1_565
C20 C26 3.495(14) .
C20 C14 3.247(16) .
C22 C267 3.57(4) 1_465
C23 C246 3.513(15) .
C24 C25 3.376(12) .
C24 C13 3.598(13) .
C25 C32 3.307(11) .
C25 C24 3.376(12) .
C26 C20 3.495(14) .
C26 C19 3.277(12) .
C28 C148 3.424(18) 1_455
C28 C270 3.40(3) 1_465
C29 C148 3.439(17) 1_455
C29 C248 3.45(2) 1_455
C30 C31 3.300(12) .
C31 C38 3.173(13) .
C31 C30 3.300(12) .
C32 C25 3.307(11) .
C32 C38 3.481(13) .
C33 C124 3.571(16) 1_465
C34 C125 3.527(17) 1_465
C34 C124 3.471(16) 1_465
C36 C271 3.55(4) 1_455
C36 C37 3.240(13) .
C36 C42 3.468(13) .
C37 C36 3.240(13) .
C37 C5 3.414(11) .
C38 C31 3.173(13) .
C38 C32 3.481(13) .
C42 C5 3.370(12) .
C42 C4 3.565(12) .
C42 C36 3.468(13) .
C42 O9A 3.36(3) .
C44 C2 3.100(11) .
C45 C80 3.469(12) .
C45 C79 3.042(11) .
C45 C84 3.507(12) .
C46 C84 3.239(12) .
C46 C56 3.207(12) .
C47 C60 3.539(13) .
C47 C55 3.054(11) .
C47 C56 3.368(11) .
C48 C90 3.127(12) .
C55 C62 3.200(11) .
C55 C47 3.054(11) .
C56 C46 3.207(12) .
C56 C47 3.368(11) .
C57 C247 3.55(2) .
C57 C248 3.53(3) .
C60 C61 3.216(11) .
C60 C47 3.539(13) .
C61 C68 3.150(12) .
C61 C60 3.216(11) .
C62 C68 3.546(12) .
C62 C55 3.200(11) .
C66 C67 3.161(13) .
C66 C68 3.546(13) .
C67 C74 3.098(13) .
C67 C66 3.161(13) .
C68 C74 3.539(14) .
C68 C61 3.150(12) .
C68 C66 3.546(13) .
C68 C62 3.546(12) .
C69 C98 3.499(11) 2_565
C71 C107 3.562(11) 2_555
C72 C73 3.148(12) .
C72 C74 3.512(13) .
C72 C78 3.543(12) .
C73 C80 3.196(12) .
C73 C72 3.148(12) .
C74 C72 3.512(13) .
C74 C67 3.098(13) .
C74 C68 3.539(14) .
C77 C153 3.56(2) .
C78 C79 3.268(11) .
C78 C72 3.543(12) .
C79 C78 3.268(11) .
C79 C45 3.042(11) .
C80 C45 3.469(12) .
C80 C73 3.196(12) .
C81 C152 3.596(17) .
C84 C46 3.239(12) .
C84 C45 3.507(12) .
C86 C130 3.592(15) .
C86 C6 3.334(14) .
C86 C234 3.60(5) .
C86 O1 3.410(10) .
C87 C122 3.507(13) .
C87 C97 3.244(11) .
C87 C98 3.306(12) .
C87 O1 3.416(9) .
C88 C122 3.201(13) .
C88 C102 3.306(13) .
C88 C98 3.452(12) .
C89 C102 3.522(13) .
C89 C121 3.350(13) .
C89 C97 3.572(12) .
C90 C48 3.127(12) .
C97 C87 3.244(11) .
C97 C89 3.572(12) .
C97 C108 3.258(11) .
C98 C87 3.306(12) .
C98 C103 3.538(11) .
C98 C88 3.452(12) .
C98 C69 3.499(11) 2_464
C100 C156 3.578(18) .
C1 H86 2.7900 .
C1 H44 2.5200 .
C2 H23A 2.9200 .
C102 C108 3.548(11) .
C102 C88 3.306(13) .
C102 C89 3.522(13) .
C2 H44 2.6100 .
C2 H15A 2.8800 .
C2 H12E 2.8500 .
C3 H23A 2.8900 .
C103 C98 3.538(11) .
C3 H12E 3.0800 .
C103 C114 3.122(12) .
C104 C114 3.433(12) .
C4 H23A 3.0800 .
C104 C109 3.116(12) .
C5 H16E 2.8900 .
C6 H13A 2.9400 .
C7 H13T 3.0800 1_565
C107 C71 3.562(11) 2_454
C108 C97 3.258(11) .
C108 C102 3.548(11) .
C8 H3 3.0700 .
C109 C104 3.116(12) .
C109 C120 3.308(13) .
C110 C116 3.558(14) .
C10 H13T 3.0400 1_565
C110 C115 3.177(12) .
C10 H26F 2.9800 .
C11 H13T 2.9700 1_565
C11 H26F 3.0000 .
C12 H13T 3.0200 1_565
C13 H3 3.0300 .
C114 C103 3.122(12) .
C114 C104 3.433(12) .
C14 H3 3.0500 .
C14 H20 3.0800 .
C15 H23P 2.9800 .
C115 C110 3.177(12) .
C115 C126 3.324(11) .
C16 H23P 2.9900 .
C16 H17O 2.9800 .
C116 C121 3.256(14) .
C116 C110 3.558(14) .
C17 H44 2.9100 .
C18 H14N 2.8800 .
C120 C109 3.308(13) .
C20 H14 3.0700 .
C20 H24G 3.0100 1_565
C121 C116 3.256(14) .
C121 C89 3.350(13) .
C21 H14G 2.9900 1_565
C122 C87 3.507(13) .
C122 C88 3.201(13) .
C22 H26O 2.8300 1_465
C23 H16P 2.9600 1_465
C123 C234 3.51(4) .
C123 C233 3.45(3) .
C23 H26O 3.0500 1_465
C23 H24N 2.7000 .
C23 H14M 2.8200 .
C24 H24N 2.7500 .
C24 H14M 2.9500 .
C126 C115 3.324(11) .
C27 H26B 3.0000 1_565
C27 H27B 3.0700 1_465
C28 H14R 3.0000 1_455
C28 H27B 2.7100 1_465
C28 H24D 3.1000 1_455
C28 H14Q 3.0700 1_455
C28 H124 2.9900 1_465
C29 H24D 2.7700 1_455
C29 H14R 2.7300 1_455
C29 H125 2.9700 1_465
C29 H23C 2.9000 1_455
C130 C86 3.592(15) .
C34 H15L 2.9300 1_565
C38 H23B 2.8800 .
C39 H23B 2.9300 .
C39 H13B 2.9200 .
C40 H13B 2.8900 .
C41 H27D 2.9700 1_455
C41 H99 3.0200 .
C42 H5 2.8400 .
C43 H90 2.8200 .
C43 H2 2.9800 .
C43 H14D 3.0700 .
C144 O7 3.30(2) .
C44 H2 3.0200 .
C46 H56 3.0800 .
C47 H24E 3.0600 1_545
C148 C28 3.424(18) 1_655
C48 H90 2.8100 .
C148 C29 3.439(17) 1_655
C49 H84 3.0900 .
C49 H26Q 2.8900 .
C49 H23M 2.8600 .
C49 H13Q 2.7800 .
C50 H23M 2.9000 .
C50 H47 3.0400 .
C50 H16T 2.9500 .
C150 C2 3.48(3) .
C51 H26S 2.9200 .
C51 H23M 3.0800 .
C51 H16T 2.8800 .
C51 H68 3.0700 .
C52 H74 3.0500 .
C52 H26S 2.8100 .
C152 C81 3.596(17) .
C153 C77 3.56(2) .
C54 H23M 3.0400 .
C54 H45 2.8900 .
C54 H13Q 2.8300 .
C55 H47 2.8300 .
C55 H62 3.0400 .
C156 C100 3.578(18) .
C56 H24B 2.9500 .
C57 H24D 2.9400 .
C57 H14R 3.0900 .
C58 H13I 2.9000 .
C158 C235 3.32(3) 2_464
C159 C272 3.07(7) 1_455
C59 H26C 3.0800 1_655
C59 H14M 2.9900 1_655
C159 C271 3.11(5) 1_455
C60 H47 2.9700 .
C161 O5A 3.19(2) .
C61 H68 3.0100 .
C62 H68 3.0800 .
C62 H105 2.9900 2_565
C63 H23 3.0500 1_655
C63 H105 3.0800 2_565
C64 H16G 3.0900 2_565
C65 H14K 2.9600 1_655
C65 H16G 2.7400 2_565
C165 C274 3.17(4) .
C166 C274 3.19(4) .
C67 H74 3.0300 .
C67 H66 3.0800 .
C69 H98 2.9100 2_565
C70 H26L 2.8800 2_565
C70 H16H 2.9800 2_565
C70 H98 2.9500 2_565
C73 H72 3.0500 .
C73 H80 3.0400 .
C75 H17C 3.1000 2_465
C77 H15H 2.9700 .
C177 C245 3.53(3) .
C77 H13M 3.0500 1_545
C78 H13M 2.8500 1_545
C178 C245 3.48(3) .
C79 H45 2.7700 .
C80 H45 2.8700 .
C81 H24I 2.8300 .
C81 H15E 2.9100 .
C82 H14E 3.0200 .
C82 H24I 2.7500 .
C83 H14C 2.8700 .
C83 H25A 2.9900 1_545
C83 H23Q 2.9400 1_545
C83 H13N 2.8200 1_545
C84 H25A 2.9600 1_545
C84 H13N 2.9600 1_545
C84 H14T 2.9300 1_545
C84 H23Q 3.0000 1_545
C85 H6 2.6900 .
C85 H48 2.6600 .
C85 H23J 2.9500 .
C86 H22B 3.0200 .
C86 H13A 2.9900 .
C86 H23J 2.7400 .
C87 H26K 2.9300 .
C87 H22B 2.8400 .
C90 H14O 2.9500 1_545
C90 H48 2.7100 .
C91 H16J 3.0100 .
C91 H108 3.0800 .
C91 H12C 2.7900 1_545
C92 H114 3.0900 .
C92 H12C 2.9900 1_545
C92 H26M 2.9100 .
C93 H26M 2.8200 .
C93 H104 3.0800 .
C93 H22C 3.0600 1_545
C94 H26M 2.9900 .
C94 H22C 3.0000 1_545
C94 H110 3.0600 .
C96 H16J 3.0700 .
C96 H12C 2.9500 1_545
C97 H108 3.0800 .
C98 H69 2.7900 2_464
C98 H70 3.0400 2_464
C102 H108 3.0500 .
C103 H114 3.0000 .
C104 H69 2.9900 2_464
C105 H68 3.0200 2_464
C105 H23L 3.0200 2_464
C106 H23L 2.9500 2_464
C107 H71 2.8800 2_454
C108 H71 2.9200 2_454
C108 H39 3.0400 1_545
C109 H104 2.9900 .
C111 H22 3.0900 2_564
C112 H15C 3.0700 2_554
C114 H26I 3.0900 1_545
C115 H110 3.0300 .
C116 H110 3.0900 .
C118 H15F 2.9000 2_554
C118 H15G 2.9800 2_554
C119 H15F 3.0500 2_554
C119 H16M 3.0700 1_545
C120 H16M 3.0500 1_545
C122 H27J 2.9000 .
C123 H27H 3.0500 .
C123 H13J 3.1000 .
C123 H23H 2.9400 .
C123 H17G 3.0200 .
C123 H27J 3.0300 .
C130 H86 2.9300 .
C233 C123 3.45(3) .
C133 H27C 3.0500 .
C133 H26D 2.8100 1_655
C133 H123 3.0400 .
C234 C86 3.60(5) .
C234 C123 3.51(4) .
C142 H24G 3.0300 .
C243 C20 3.589(13) 1_545
C143 H27 3.0700 1_545
C244 O7 3.05(2) .
C145 H17R 2.7900 .
C245 C177 3.53(3) .
C245 C178 3.48(3) .
C246 C23 3.513(15) .
C247 C57 3.55(2) .
C248 C29 3.45(2) 1_655
C148 H28 2.8100 1_655
C248 C57 3.53(3) .
C148 H57 3.0200 .
C148 H29 2.8300 1_655
C149 H23O 2.7900 .
C150 H2 2.6800 .
C151 H24J 3.0800 .
C158 H23K 2.9000 2_464
C159 H27C 2.4100 1_455
C159 H27E 2.3100 1_455
C162 H5 3.0400 .
C165 H122 2.8400 .
C165 H27I 2.4900 .
C165 H27J 2.9500 .
C166 H27I 2.3500 .
C268 C148 3.59(6) 1_545
C270 C148 3.39(4) 1_545
C271 C36 3.55(4) 1_655
C271 C159 3.11(5) 1_655
C272 C159 3.07(7) 1_655
C274 C165 3.17(4) .
C274 C166 3.19(4) .
C174 H41 3.0700 1_655
C177 H81 3.0700 .
C177 H24K 2.7500 .
C178 H24K 2.8200 .
C227 H70 2.9700 2_464
C227 H16H 3.0400 .
C231 H14P 2.9500 .
C231 H29 3.0400 1_655
C233 H123 2.7300 .
C234 H123 2.9500 .
C237 H15 3.0800 .
C243 H26 3.0900 1_545
C243 H20 3.0800 1_545
C244 H81 3.0700 .
C244 H21 3.0700 1_545
C245 H17R 2.6700 .
C245 H17P 2.8600 .
C247 H2 3.0300 .
C247 H57 2.9100 .
C247 H56 3.0500 .
C248 H29 2.6500 1_655
C248 H57 2.6400 .
C250 H14C 3.0300 1_565
C259 H32 2.9400 1_545
C260 H33 3.0800 1_545
C265 H87 2.9600 .
C268 H14Q 2.9800 1_545
C268 H84 3.0800 .
C270 H14Q 2.8300 1_545
C271 H36 2.8500 1_655
C271 H15T 2.1400 1_655
C272 H15T 2.3300 1_655
C274 H16K 3.0700 .
C274 H16N 2.7700 .
C274 H16L 2.8100 .
H2 O6 2.8900 .
H2 C150 2.6800 .
H2 C44 3.0200 .
H2 H24A 2.2800 .
H2 H15A 2.0100 .
H2 C247 3.0300 .
H2 C43 2.9800 .
H3 H14B 2.2900 1_565
H3 C8 3.0700 .
H3 C14 3.0500 .
H3 O4A 2.8500 1_565
H3 C13 3.0300 .
H5 H16E 2.2200 .
H5 O9A 2.4300 .
H5 C42 2.8400 .
H5 H42 2.3600 .
H5 C162 3.0400 .
H6 C85 2.6900 .
H12E C2 2.8500 .
H12E C3 3.0800 .
H13A C6 2.9400 .
H13A C86 2.9900 .
H13A H86 2.4500 .
H13B C39 2.9200 .
H13B C40 2.8900 .
H13D H86 2.4500 .
H13G H123 2.2300 .
H13G H26D 2.5900 1_655
H13G H27J 2.5300 .
H13G H27C 2.4400 .
H13H H26D 2.4400 1_655
H13I C58 2.9000 .
H13J C123 3.1000 .
H13L H15 2.5500 .
H13Q C54 2.8300 .
H13Q C49 2.7800 .
H13Q H45 2.5200 .
H13S H14F 2.4600 .
H13T C7 3.0800 1_545
H13T C12 3.0200 1_545
H13T C11 2.9700 1_545
H13T C10 3.0400 1_545
H14 C20 3.0700 .
H14B H3 2.2900 1_545
H14C C250 3.0300 1_545
H14C H25A 2.4900 1_545
H14C C83 2.8700 .
H14C H83 2.5400 .
H14D C43 3.0700 .
H14D H90 2.5000 .
H14E C82 3.0200 .
H14F H13S 2.4600 .
H14G C21 2.9900 1_545
H14I H21 2.5100 1_545
H14I O7 2.5600 .
H14K H17R 2.1700 .
H14L H17R 2.5600 .
H14M C24 2.9500 .
H14M H23 2.4100 .
H14M C23 2.8200 .
H14N H18 2.4700 .
H14N C18 2.8800 .
H14P H23C 2.3600 .
H14P C231 2.9500 .
H14Q H28 2.2900 1_655
H14Q C28 3.0700 1_655
H14R H29 2.0700 1_655
H14R C57 3.0900 .
H14R H57 2.1500 .
H14R C29 2.7300 1_655
H14R C28 3.0000 1_655
H14S H23O 2.2200 .
H14S H56 2.5700 .
H14T H23O 2.5700 .
H15 H23R 2.5600 .
H15 H13L 2.5500 .
H15 C237 3.0800 .
H15 H23P 2.4800 .
H15A C2 2.8800 .
H15A H2 2.0100 .
H15D H17P 2.3400 .
H15E H81 2.5900 .
H15E C81 2.9100 .
H15H C77 2.9700 .
H15K H107 2.5900 .
H15L C34 2.9300 1_545
H15M H27F 2.5000 1_455
H15M H17H 2.5800 1_455
H15O H17J 2.4800 1_455
H15Q O3A 2.7500 2_464
H15Q H23L 2.1500 2_464
H15Q H23K 2.0100 2_464
H15Q C235 2.3500 2_464
H15S H27E 2.2600 1_455
H15T C272 2.3300 1_455
H15T C271 2.1400 1_455
H15T H27E 1.8300 1_455
H15T H27C 1.4600 1_455
H16 H23P 2.4900 .
H16 O3 2.9200 .
H16 H17O 2.3600 .
H16D O5A 2.5800 .
H16E C5 2.8900 .
H16E H5 2.2200 .
H16G C64 3.0900 2_464
H16G H65 2.5200 2_464
H16G C65 2.7400 2_464
H16H H22A 2.2600 .
H16H C70 2.9800 2_464
H16H C227 3.0400 .
H16J H98 2.5400 .
H16J H87 2.4600 .
H16J C91 3.0100 .
H16J C96 3.0700 .
H16K C274 3.0700 .
H16K H87 2.5800 .
H16K H27J 2.5700 .
H16K H122 2.1900 .
H16L H116 2.1800 .
H16L H27I 2.1400 .
H16L C274 2.8100 .
H16M H27I 2.5000 .
H16N C274 2.7700 .
H16N H27I 1.8200 .
H16S H66 2.5800 .
H16T C50 2.9500 .
H16T C51 2.8800 .
H17B H84 2.5600 .
H17C C75 3.1000 2_564
H17C H75 2.3700 2_564
H17G H123 2.5200 .
H17G C123 3.0200 .
H17J H41 2.4500 1_655
H17K H17E 2.4800 2_465
H17M H17C 2.5200 2_465
H17O O3 2.8900 .
H17O H16 2.3600 .
H17O C16 2.9800 .
H17P H81 2.4000 .
H17P C245 2.8600 .
H17P H24K 2.1900 .
H17P H15D 2.3400 .
H17R H14L 2.5600 .
H17R C145 2.7900 .
H17R C245 2.6700 .
H17R H24L 2.4600 .
H17R H24K 2.1800 .
H17R H14K 2.1700 .
H18 H14N 2.4700 .
H20 C243 3.0800 1_565
H20 C14 3.0800 .
H20 O4 2.9100 1_565
H20 H24G 2.3600 1_565
H21 H24J 2.3600 1_565
H21 C244 3.0700 1_565
H21 H14I 2.5100 1_565
H22A H70 2.4700 2_464
H22A H16H 2.2600 .
H22B H86 2.5500 .
H22B H87 2.1700 .
H22B C86 3.0200 .
H22B C87 2.8400 .
H23 H14M 2.4100 .
H23A C4 3.0800 .
H23A C2 2.9200 .
H23A C3 2.8900 .
H23B C39 2.9300 .
H23B C38 2.8800 .
H23C H29 2.0800 1_655
H23C C29 2.9000 1_655
H23C H14P 2.3600 .
H23H C123 2.9400 .
H23H H123 2.0900 .
H23J C85 2.9500 .
H23J C86 2.7400 .
H23K H74 2.4700 .
H23L C106 2.9500 2_565
H23L H106 2.5100 2_565
H23L C105 3.0200 2_565
H23L H68 2.4400 .
H23M C50 2.9000 .
H23M C54 3.0400 .
H23M C51 3.0800 .
H23M C49 2.8600 .
H23N H62 2.3300 .
H23O C149 2.7900 .
H23O H14T 2.5700 .
H23O H14S 2.2200 .
H23P C16 2.9900 .
H23P C15 2.9800 .
H23P H15 2.4800 .
H23P H16 2.4900 .
H23R H15 2.5600 .
H24A H2 2.2800 .
H24B H57 2.5900 .
H24B H56 2.2700 .
H24B C56 2.9500 .
H24C H29 2.4400 1_655
H24D H57 2.0000 .
H24D H29 2.0900 1_655
H24D C29 2.7700 1_655
H24D C57 2.9400 .
H24D C28 3.1000 1_655
H24G C20 3.0100 1_545
H24G H26 2.4500 1_545
H24G C142 3.0300 .
H24G H20 2.3600 1_545
H24H H24M 2.4500 .
H24I C81 2.8300 .
H24I H81 2.3300 .
H24I C82 2.7500 .
H24I H82 2.1700 .
H24J H21 2.3600 1_545
H24J C151 3.0800 .
H24J O7 2.3800 .
H24K H17R 2.1800 .
H24K H17P 2.1900 .
H24K C177 2.7500 .
H24K C178 2.8200 .
H24L H17R 2.4600 .
H24M H24H 2.4500 .
H24N C24 2.7500 .
H24N C23 2.7000 .
H25A H14C 2.4900 1_565
H25D H32 2.4700 1_545
H26 O4 2.9200 1_565
H26 C243 3.0900 1_565
H26 H24G 2.4500 1_565
H26B C27 3.0000 1_545
H26D H13H 2.4400 1_455
H26D C133 2.8100 1_455
H26D H13G 2.5900 1_455
H26F C10 2.9800 .
H26F C11 3.0000 .
H26K C87 2.9300 .
H26K H87 2.0000 .
H26L C70 2.8800 2_464
H26L H70 2.5000 2_464
H26M C94 2.9900 .
H26M C92 2.9100 .
H26M C93 2.8200 .
H26P C143 2.9100 1_655
H26P H14G 2.5200 1_655
H26P H14H 2.5000 1_655
H26Q C49 2.8900 .
H26R H14T 2.5100 1_545
H26R C149 2.9100 1_545
H26S C52 2.8100 .
H26S C51 2.9200 .
H26T H78 2.5600 .
H27 C143 3.0700 1_565
H27 O5 2.7600 1_565
H27A C148 2.8400 1_545
H27A H14Q 2.5600 1_545
H27A H14R 2.4800 1_545
H27C H13G 2.4400 .
H27C C159 2.4100 1_655
H27C H15T 1.4600 1_655
H27C C133 3.0500 .
H27C H36 2.3100 1_655
H27D C41 2.9700 1_655
H27D H36 2.5800 1_655
H27E O9 2.7000 1_655
H27E H15S 2.2600 1_655
H27E C159 2.3100 1_655
H27E H15T 1.8300 1_655
H27H C123 3.0500 .
H27I C166 2.3500 .
H27I H16L 2.1400 .
H27I C165 2.4900 .
H27I H16N 1.8200 .
H27I H16M 2.5000 .
H27J H123 2.5900 .
H27J H122 2.3200 .
H27J H16K 2.5700 .
H27J C165 2.9500 .
H27J H13G 2.5300 .
H27J C122 2.9000 .
H27J C123 3.0300 .
H28 H14Q 2.2900 1_455
H28 H27B 2.3700 1_465
H28 C148 2.8100 1_455
H29 C148 2.8300 1_455
H29 H24C 2.4400 1_455
H29 H24D 2.0900 1_455
H29 C248 2.6500 1_455
H29 H14R 2.0700 1_455
H29 C231 3.0400 1_455
H29 H23C 2.0800 1_455
H32 C259 2.9400 1_565
H32 H25D 2.4700 1_565
H33 C260 3.0800 1_565
H34 C117 2.8700 1_465
H34 C118 3.0900 1_465
H36 H27C 2.3100 1_455
H36 C271 2.8500 1_455
H36 H27D 2.5800 1_455
H41 H17J 2.4500 1_455
H41 H99 2.6000 .
H41 C174 3.0700 1_455
H42 O9A 2.4600 .
H42 H5 2.3600 .
H42 O9 2.7900 .
H44 C2 2.6100 .
H44 C17 2.9100 .
H44 C1 2.5200 .
H45 C54 2.8900 .
H45 C80 2.8700 .
H45 H13Q 2.5200 .
H45 C79 2.7700 .
H47 C50 3.0400 .
H47 C55 2.8300 .
H47 C60 2.9700 .
H48 C85 2.6600 .
H48 C90 2.7100 .
H48 H90 2.5700 .
H56 C46 3.0800 .
H56 C247 3.0500 .
H56 H24B 2.2700 .
H56 H14S 2.5700 .
H57 C148 3.0200 .
H57 H14R 2.1500 .
H57 C248 2.6400 .
H57 H24B 2.5900 .
H57 C247 2.9100 .
H57 H24D 2.0000 .
H59 O5 2.6200 1_655
H59 C146 2.9700 1_655
H59 H26C 2.3900 1_655
H59 H16D 2.4600 1_655
H59 H14M 2.4400 1_655
H60 H14H 2.3800 1_655
H62 H23N 2.3300 .
H62 C55 3.0400 .
H63 H22 2.5600 1_655
H65 H16G 2.5200 2_565
H65 H14J 2.5700 1_655
H66 H113 2.5500 2_555
H66 C67 3.0800 .
H66 H16S 2.5800 .
H68 C51 3.0700 .
H68 C62 3.0800 .
H68 H23L 2.4400 .
H68 C61 3.0100 .
H68 H105 2.5700 2_565
H68 C105 3.0200 2_565
H69 H98 2.3100 2_565
H69 C104 2.9900 2_565
H69 C98 2.7900 2_565
H70 H99 2.5600 2_565
H70 C98 3.0400 2_565
H70 H98 2.3700 2_565
H70 H26L 2.5000 2_565
H71 H114 2.5100 2_555
H71 C107 2.8800 2_555
H71 C108 2.9200 2_555
H72 C73 3.0500 .
H74 C52 3.0500 .
H74 C67 3.0300 .
H74 H23K 2.4700 .
H75 H17C 2.3700 2_465
H77 H13M 2.5900 1_545
H77 O3A 2.7200 1_545
H78 H23Q 2.5900 1_545
H78 H13M 2.1400 1_545
H78 C136 2.9200 1_545
H78 H26T 2.5600 .
H80 C73 3.0400 .
H81 C177 3.0700 .
H81 H15E 2.5900 .
H81 H17P 2.4000 .
H81 C244 3.0700 .
H81 H24I 2.3300 .
H82 H24I 2.1700 .
H83 H25A 2.5900 1_545
H83 H14C 2.5400 .
H84 H25A 2.5400 1_545
H84 C49 3.0900 .
H84 H14T 2.1700 1_545
H84 H17B 2.5600 .
H84 C268 3.0800 .
H86 O1 2.8500 .
H86 C1 2.7900 .
H86 C130 2.9300 .
H86 H13A 2.4500 .
H86 H13D 2.4500 .
H86 H22B 2.5500 .
H87 O1 2.8600 .
H87 H26K 2.0000 .
H87 H16K 2.5800 .
H87 C265 2.9600 .
H87 H16J 2.4600 .
H87 H22B 2.1700 .
H89 H22F 2.4400 1_545
H90 H14D 2.5000 .
H90 C48 2.8100 .
H90 C43 2.8200 .
H90 C250 3.0500 1_545
H90 H14O 2.3700 1_545
H90 H48 2.5700 .
H90 H25B 2.4900 1_545
H98 C70 2.9500 2_464
H98 H16J 2.5400 .
H98 C69 2.9100 2_464
H98 H70 2.3700 2_464
H98 H69 2.3100 2_464
H99 C41 3.0200 .
H99 H70 2.5600 2_464
H99 H41 2.6000 .
H101 H38 2.4200 1_545
H104 C109 2.9900 .
H104 C93 3.0800 .
H105 H68 2.5700 2_464
H105 C62 2.9900 2_464
H105 C63 3.0800 2_464
H106 O3A 2.8500 2_464
H106 H23L 2.5100 2_464
H107 H15K 2.5900 .
H108 C91 3.0800 .
H108 C97 3.0800 .
H108 C102 3.0500 .
H108 H39 2.3700 1_545
H110 C116 3.0900 .
H110 C115 3.0300 .
H110 C94 3.0600 .
H111 H22 2.4400 2_564
H111 H15J 2.5100 2_554
H113 H66 2.5500 2_454
H114 C103 3.0000 .
H114 H12A 2.2800 1_545
H114 H71 2.5100 2_454
H114 C92 3.0900 .
H116 H16L 2.1800 .
H118 H15F 2.5600 2_554
H119 H16M 2.4600 1_545
H119 C166 2.9800 1_545
H120 H16M 2.4400 1_545
H120 C264 2.9600 1_545
H120 H26I 2.4000 1_545
H122 C165 2.8400 .
H122 H16K 2.1900 .
H122 H27J 2.3200 .
H123 C133 3.0400 .
H123 H13G 2.2300 .
H123 H17G 2.5200 .
H123 C233 2.7300 .
H123 C234 2.9500 .
H123 H23H 2.0900 .
H123 H27J 2.5900 .
H123 H15S 2.6000 1_655
H124 H26B 2.3700 1_655
H126 H12D 2.4400 1_545
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_publ_flag
C144 H14I O7 0.9900 2.5600 3.30(2) 132.00 y
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
C127 O1 C130 C129 -24.8(13)
C130 O1 C127 C128 15.4(11)
C131 O2 C134 C133 24(3)
C134 O2 C131 C132 -6(3)
C138 O3 C135 C136 9(3)
C135 O3 C138 C137 -23(2)
C146 O5 C143 C144 -31.1(17)
C143 O5 C146 C145 24(2)
C85 N1 C1 C2 -134.01
C43 N1 C1 C6 -119.59
C85 N1 C1 C6 45.94
C1 N1 C43 C44 9.18
C43 N1 C1 C2 60.46
C1 N1 C85 C90 -122.24
C85 N1 C43 C48 24.81
C1 N1 C43 C48 -170.99
C1 N1 C85 C86 55.63
C43 N1 C85 C90 42.48
C85 N1 C43 C44 -155.03
C43 N1 C85 C86 -139.66
C147 O6 C150 C149 11(3)
C150 O6 C147 C148 2.5(18)
C162 O9 C159 C160 27(2)
C159 O9 C162 C161 -19(3)
C166 O10 C163 C164 -23(2)
C163 O10 C166 C165 17(2)
C170 O11 C167 C168 20.1(19)
C167 O11 C170 C169 -25(2)
C174 O12 C171 C172 22(3)
C171 O12 C174 C173 -29(3)
N1 C1 C2 C3 -174.78
C6 C1 C2 C3 5.3(12)
C2 C1 C6 C5 -6.4(12)
N1 C1 C6 C5 173.68
C1 C2 C3 C4 0.7(12)
C2 C3 C4 C7 166.1(7)
C2 C3 C4 C5 -5.6(12)
C3 C4 C7 C12 117.8(9)
C139 O4 C142 C141 -42.2(18)
C3 C4 C5 C6 4.5(12)
C142 O4 C139 C140 39(2)
C3 C4 C7 C8 -63.0(9)
C5 C4 C7 C12 -70.8(10)
C7 C4 C5 C6 -167.1(7)
C5 C4 C7 C8 108.5(9)
C4 C5 C6 C1 1.5(12)
C12 C7 C8 C9 0.7(10)
C4 C7 C8 C13 -0.4(10)
C4 C7 C8 C9 -178.5(6)
C12 C7 C8 C13 178.9(6)
C4 C7 C12 C37 -1.4(11)
C4 C7 C12 C11 -178.3(7)
C8 C7 C12 C37 179.4(7)
C8 C7 C12 C11 2.5(11)
C7 C8 C13 C18 -74.2(10)
C7 C8 C9 C19 171.9(7)
C13 C8 C9 C19 -6.2(10)
C9 C8 C13 C18 103.9(9)
C7 C8 C9 C10 -2.4(10)
C13 C8 C9 C10 179.5(6)
C9 C8 C13 C14 -75.7(11)
C7 C8 C13 C14 106.2(10)
C8 C9 C19 C20 84.4(10)
C8 C9 C10 C11 0.8(11)
C10 C9 C19 C24 79.0(10)
C19 C9 C10 C11 -173.5(7)
C8 C9 C10 C25 -179.7(6)
C10 C9 C19 C20 -101.4(10)
C19 C9 C10 C25 6.0(10)
C8 C9 C19 C24 -95.2(10)
C9 C10 C11 C12 2.4(11)
C9 C10 C25 C30 -106.9(9)
C25 C10 C11 C12 -177.1(7)
C11 C10 C25 C30 72.6(10)
C25 C10 C11 C31 4.5(10)
C9 C10 C25 C26 71.1(10)
C11 C10 C25 C26 -109.4(10)
C9 C10 C11 C31 -176.0(7)
C10 C11 C31 C36 -106.6(9)
C10 C11 C31 C32 74.8(11)
C31 C11 C12 C37 -2.7(10)
C31 C11 C12 C7 174.4(7)
C10 C11 C12 C7 -4.1(11)
C12 C11 C31 C32 -103.6(9)
C12 C11 C31 C36 75.0(10)
C10 C11 C12 C37 178.8(7)
C7 C12 C37 C42 83.2(10)
C11 C12 C37 C42 -99.8(9)
C11 C12 C37 C38 73.3(10)
C7 C12 C37 C38 -103.7(9)
C8 C13 C14 C15 177.3(9)
C8 C13 C18 C17 -178.4(8)
C14 C13 C18 C17 1.3(14)
C18 C13 C14 C15 -2.4(15)
C13 C14 C15 C16 2.5(17)
C14 C15 C16 C17 -1.4(17)
C15 C16 C17 C18 0.3(16)
C16 C17 C18 C13 -0.2(15)
C20 C19 C24 C23 -0.7(14)
C9 C19 C20 C21 -176.7(9)
C24 C19 C20 C21 2.9(14)
C9 C19 C24 C23 178.9(9)
C19 C20 C21 C22 -3.5(16)
C20 C21 C22 C23 1.8(17)
C21 C22 C23 C24 0.5(17)
C22 C23 C24 C19 -1.0(16)
C10 C25 C30 C29 177.4(8)
C30 C25 C26 C27 -0.3(15)
C10 C25 C26 C27 -178.3(9)
C26 C25 C30 C29 -0.7(13)
C25 C26 C27 C28 0.3(17)
C26 C27 C28 C29 0.5(18)
C27 C28 C29 C30 -1.5(18)
C28 C29 C30 C25 1.6(16)
C32 C31 C36 C35 -0.1(14)
C11 C31 C32 C33 178.3(9)
C11 C31 C36 C35 -178.6(9)
C36 C31 C32 C33 -0.2(14)
C31 C32 C33 C34 1.5(16)
C32 C33 C34 C35 -2.5(17)
C33 C34 C35 C36 2.2(18)
C34 C35 C36 C31 -1.0(16)
C42 C37 C38 C39 0.8(14)
C38 C37 C42 C41 0.2(14)
C12 C37 C38 C39 -172.3(9)
C12 C37 C42 C41 173.3(8)
C37 C38 C39 C40 0.1(15)
C38 C39 C40 C41 -2.0(15)
C39 C40 C41 C42 3.1(16)
C40 C41 C42 C37 -2.1(15)
N1 C43 C48 C47 179.88
N1 C43 C44 C45 -178.91
C48 C43 C44 C45 1.3(10)
C44 C43 C48 C47 -0.3(11)
C43 C44 C45 C46 -0.9(11)
C44 C45 C46 C49 177.6(7)
C44 C45 C46 C47 -0.6(11)
C47 C46 C49 C50 57.2(9)
C47 C46 C49 C54 -127.6(8)
C45 C46 C47 C48 1.6(11)
C45 C46 C49 C54 54.3(9)
C49 C46 C47 C48 -176.6(7)
C45 C46 C49 C50 -120.9(8)
C46 C47 C48 C43 -1.2(11)
C54 C49 C50 C51 -1.0(10)
C46 C49 C54 C53 -173.7(6)
C50 C49 C54 C79 -177.8(7)
C54 C49 C50 C55 -179.0(6)
C46 C49 C50 C51 174.2(6)
C46 C49 C50 C55 -3.8(10)
C50 C49 C54 C53 1.4(10)
C46 C49 C54 C79 7.1(10)
C49 C50 C51 C61 -178.9(7)
C55 C50 C51 C61 -0.8(10)
C49 C50 C55 C56 68.8(10)
C49 C50 C55 C60 -110.5(9)
C51 C50 C55 C60 71.5(10)
C55 C50 C51 C52 178.6(6)
C49 C50 C51 C52 0.5(10)
C51 C50 C55 C56 -109.2(9)
C61 C51 C52 C53 178.8(7)
C50 C51 C52 C53 -0.6(10)
C61 C51 C52 C67 0.5(10)
C50 C51 C61 C66 -113.9(9)
C50 C51 C52 C67 -178.9(6)
C52 C51 C61 C62 -109.9(9)
C50 C51 C61 C62 69.5(10)
C52 C51 C61 C66 66.7(10)
C51 C52 C67 C68 66.6(11)
C51 C52 C67 C72 -114.2(9)
C51 C52 C53 C73 -177.7(6)
C67 C52 C53 C54 179.4(6)
C67 C52 C53 C73 0.6(10)
C53 C52 C67 C72 67.5(11)
C51 C52 C53 C54 1.1(11)
C53 C52 C67 C68 -111.8(9)
C73 C53 C54 C79 -3.5(10)
C54 C53 C73 C78 71.9(10)
C52 C53 C73 C78 -109.3(9)
C73 C53 C54 C49 177.3(6)
C52 C53 C54 C79 177.8(7)
C52 C53 C54 C49 -1.5(10)
C54 C53 C73 C74 -112.5(9)
C52 C53 C73 C74 66.3(10)
C53 C54 C79 C84 -112.3(9)
C49 C54 C79 C84 67.0(11)
C49 C54 C79 C80 -113.8(9)
C53 C54 C79 C80 67.0(10)
C50 C55 C56 C57 179.9(9)
C56 C55 C60 C59 0.9(13)
C50 C55 C60 C59 -179.7(9)
C60 C55 C56 C57 -0.8(13)
C55 C56 C57 C58 1.7(16)
C56 C57 C58 C59 -2.8(17)
C57 C58 C59 C60 3.0(18)
C58 C59 C60 C55 -2.1(16)
C51 C61 C62 C63 175.1(8)
C62 C61 C66 C65 0.5(13)
C51 C61 C66 C65 -176.2(9)
C66 C61 C62 C63 -1.6(12)
C61 C62 C63 C64 1.2(13)
C62 C63 C64 C65 0.5(15)
C63 C64 C65 C66 -1.7(17)
C64 C65 C66 C61 1.2(16)
C72 C67 C68 C69 -0.9(14)
C68 C67 C72 C71 -0.1(13)
C52 C67 C72 C71 -179.3(8)
C52 C67 C68 C69 178.4(9)
C67 C68 C69 C70 1.4(15)
C68 C69 C70 C71 -1.0(15)
C69 C70 C71 C72 0.1(15)
C70 C71 C72 C67 0.5(14)
C74 C73 C78 C77 -2.3(13)
C53 C73 C78 C77 173.3(8)
C53 C73 C74 C75 -174.5(9)
C78 C73 C74 C75 1.3(14)
C73 C74 C75 C76 0.5(15)
C74 C75 C76 C77 -1.3(16)
C75 C76 C77 C78 0.3(16)
C76 C77 C78 C73 1.5(14)
C54 C79 C80 C81 179.4(9)
C80 C79 C84 C83 0.7(14)
C84 C79 C80 C81 -1.3(13)
C54 C79 C84 C83 -180.0(9)
C79 C80 C81 C82 0.9(15)
C80 C81 C82 C83 0.2(17)
C81 C82 C83 C84 -0.8(18)
C82 C83 C84 C79 0.3(17)
C86 C85 C90 C89 -2.0(14)
C90 C85 C86 C87 2.6(14)
N1 C85 C86 C87 -175.37
N1 C85 C90 C89 175.84
C85 C86 C87 C88 -0.1(14)
C86 C87 C88 C96 175.6(8)
C86 C87 C88 C89 -2.9(13)
C89 C88 C96 C95 -81.8(10)
C87 C88 C96 C91 -77.7(10)
C87 C88 C96 C95 99.8(9)
C89 C88 C96 C91 100.7(10)
C96 C88 C89 C90 -175.0(9)
C87 C88 C89 C90 3.4(14)
C88 C89 C90 C85 -1.0(15)
C97 C91 C92 C103 -2.1(10)
C97 C91 C96 C95 179.7(6)
C92 C91 C97 C98 -84.3(9)
C96 C91 C92 C103 -179.1(6)
C96 C91 C92 C93 1.0(10)
C97 C91 C96 C88 -2.9(10)
C92 C91 C97 C102 102.9(9)
C96 C91 C97 C102 -80.1(9)
C92 C91 C96 C88 174.3(6)
C92 C91 C96 C95 -3.2(10)
C97 C91 C92 C93 178.0(6)
C96 C91 C97 C98 92.8(9)
C91 C92 C103 C104 116.0(8)
C91 C92 C93 C94 0.5(10)
C91 C92 C93 C109 -178.9(6)
C103 C92 C93 C109 1.3(10)
C93 C92 C103 C104 -64.2(9)
C91 C92 C103 C108 -66.1(9)
C103 C92 C93 C94 -179.4(6)
C93 C92 C103 C108 113.8(9)
C109 C93 C94 C95 179.5(6)
C92 C93 C109 C110 113.5(9)
C94 C93 C109 C110 -65.9(10)
C109 C93 C94 C115 -1.9(10)
C94 C93 C109 C114 115.9(9)
C92 C93 C94 C115 178.7(6)
C92 C93 C109 C114 -64.8(10)
C92 C93 C94 C95 0.1(10)
C95 C94 C115 C116 -72.0(11)
C95 C94 C115 C120 105.4(10)
C115 C94 C95 C121 -1.6(10)
C93 C94 C115 C120 -73.3(11)
C93 C94 C115 C116 109.4(10)
C115 C94 C95 C96 179.1(6)
C93 C94 C95 C96 -2.3(10)
C93 C94 C95 C121 177.1(7)
C121 C95 C96 C88 7.0(10)
C96 C95 C121 C126 103.2(8)
C94 C95 C121 C126 -76.2(10)
C96 C95 C121 C122 -72.3(11)
C94 C95 C96 C91 3.8(10)
C94 C95 C121 C122 108.4(10)
C121 C95 C96 C91 -175.5(7)
C94 C95 C96 C88 -173.6(6)
C102 C97 C98 C99 -0.3(13)
C91 C97 C98 C99 -173.5(8)
C91 C97 C102 C101 173.8(8)
C98 C97 C102 C101 0.6(12)
C97 C98 C99 C100 1.0(15)
C98 C99 C100 C101 -1.9(15)
C99 C100 C101 C102 2.2(13)
C151 O7 C154 C153 -30.2(16)
C154 O7 C151 C152 34.7(15)
C155 O8 C158 C157 -2.5(19)
C158 O8 C155 C156 11.1(16)
C175 O13 C178 C177 25(2)
C178 O13 C175 C176 -25(2)
|
1501544.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:23:32 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501544.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_1501544
loop_
_publ_author_name
'Daniel J. St-Cyr'
'Thierry Maris'
'William D. Lubel'
_publ_section_title
;
Crystal-State Structural Analysis of Beta-Hydroxy-gamma-Lactam
Constrained SER/THR Peptidomimetics
;
_journal_name_full Heterocycles
_journal_page_first 729
_journal_page_last 737
_journal_paper_doi 10.3987/COM-10-S(E)52
_journal_volume 82
_journal_year 2010
_chemical_absolute_configuration rmad
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C27 H24 N2 O6, C6 H6'
_chemical_formula_sum 'C33 H30 N2 O6'
_chemical_formula_weight 550.59
_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
_audit_creation_method SHELXL-97
_cell_angle_alpha 90
_cell_angle_beta 95.949(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 4.9653(3)
_cell_length_b 13.6703(8)
_cell_length_c 20.3533(11)
_cell_measurement_reflns_used 3091
_cell_measurement_temperature 150
_cell_measurement_theta_max 71.55
_cell_measurement_theta_min 2.18
_cell_volume 1374.08(14)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.060
_diffrn_reflns_av_sigmaI/netI 0.0600
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 17967
_diffrn_reflns_theta_full 72.41
_diffrn_reflns_theta_max 72.41
_diffrn_reflns_theta_min 2.18
_exptl_absorpt_coefficient_mu 0.751
_exptl_absorpt_correction_T_max 0.9631
_exptl_absorpt_correction_T_min 0.6806
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.331
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_F_000 580
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.158
_refine_diff_density_min -0.195
_refine_diff_density_rms 0.042
_refine_ls_abs_structure_details 'Flack H D (1983), 2327 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.2(2)
_refine_ls_extinction_coef 0.0044(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 1.067
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 374
_refine_ls_number_reflns 5162
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.067
_refine_ls_R_factor_all 0.0663
_refine_ls_R_factor_gt 0.0486
_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^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1071
_refine_ls_wR_factor_ref 0.1143
_reflns_number_gt 4048
_reflns_number_total 5162
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block lube46
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
;
_cod_original_sg_symbol_H-M P21
_cod_database_code 1501544
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
N1 N 0.3189(5) 0.65754(17) 0.00044(11) 0.0338(5) Uani 1 1 d .
N2 N 0.1108(5) 0.78052(18) 0.13845(11) 0.0340(5) Uani 1 1 d .
H2 H 0.2798 0.7941 0.1529 0.041 Uiso 1 1 calc R
C3 C 0.0571(6) 0.7178(2) 0.08128(14) 0.0344(7) Uani 1 1 d .
H3 H -0.1360 0.7264 0.0628 0.041 Uiso 1 1 calc R
C4 C 0.1090(6) 0.6104(2) 0.09441(14) 0.0377(7) Uani 1 1 d .
H4 H 0.2581 0.6028 0.1310 0.045 Uiso 1 1 calc R
C5 C 0.2024(6) 0.5707(2) 0.03020(14) 0.0389(7) Uani 1 1 d .
H5A H 0.3403 0.5188 0.0393 0.047 Uiso 1 1 calc R
H5B H 0.0480 0.5441 0.0009 0.047 Uiso 1 1 calc R
C2 C 0.2407(6) 0.7440(2) 0.02762(13) 0.0340(6) Uani 1 1 d .
C6 C 0.4843(6) 0.6469(2) -0.05185(13) 0.0331(6) Uani 1 1 d .
C7 C 0.5148(6) 0.5546(2) -0.07941(14) 0.0395(7) Uani 1 1 d .
H7 H 0.4196 0.5002 -0.0643 0.047 Uiso 1 1 calc R
C8 C 0.6842(6) 0.5421(2) -0.12895(14) 0.0407(7) Uani 1 1 d .
H8 H 0.7052 0.4789 -0.1471 0.049 Uiso 1 1 calc R
C9 C 0.8212(6) 0.6196(2) -0.15199(14) 0.0403(7) Uani 1 1 d .
H9 H 0.9369 0.6100 -0.1858 0.048 Uiso 1 1 calc R
C10 C 0.7910(6) 0.7127(2) -0.12586(14) 0.0348(6) Uani 1 1 d .
C11 C 0.6213(6) 0.7263(2) -0.07600(13) 0.0342(6) Uani 1 1 d .
H11 H 0.5990 0.7898 -0.0584 0.041 Uiso 1 1 calc R
C12 C 0.9318(6) 0.7998(2) -0.14896(14) 0.0374(7) Uani 1 1 d .
C13 C 1.2514(7) 0.8593(3) -0.21730(18) 0.0536(9) Uani 1 1 d .
H13A H 1.3664 0.8872 -0.1799 0.080 Uiso 1 1 calc R
H13B H 1.1268 0.9096 -0.2367 0.080 Uiso 1 1 calc R
H13C H 1.3651 0.8360 -0.2507 0.080 Uiso 1 1 calc R
C14 C -0.0883(6) 0.8186(2) 0.17006(13) 0.0322(6) Uani 1 1 d .
C15 C -0.1836(6) 0.9271(2) 0.25444(14) 0.0359(7) Uani 1 1 d .
H15A H -0.3259 0.8828 0.2678 0.043 Uiso 1 1 calc R
H15B H -0.2702 0.9760 0.2232 0.043 Uiso 1 1 calc R
C16 C -0.0429(6) 0.9783(2) 0.31482(14) 0.0358(7) Uani 1 1 d .
H16 H 0.1181 1.0153 0.3025 0.043 Uiso 1 1 calc R
C17 C 0.0401(6) 0.9109(2) 0.37258(14) 0.0352(7) Uani 1 1 d .
C18 C 0.2215(6) 0.8337(2) 0.37695(15) 0.0406(7) Uani 1 1 d .
H18 H 0.3161 0.8169 0.3403 0.049 Uiso 1 1 calc R
C19 C 0.2636(6) 0.7809(3) 0.43560(15) 0.0456(8) Uani 1 1 d .
H19 H 0.3902 0.7286 0.4395 0.055 Uiso 1 1 calc R
C20 C 0.1186(6) 0.8050(3) 0.48905(16) 0.0482(8) Uani 1 1 d .
H20 H 0.1466 0.7681 0.5287 0.058 Uiso 1 1 calc R
C21 C -0.0631(6) 0.8812(3) 0.48497(15) 0.0465(8) Uani 1 1 d .
H21 H -0.1596 0.8970 0.5215 0.056 Uiso 1 1 calc R
C22 C -0.1042(6) 0.9351(2) 0.42635(14) 0.0371(7) Uani 1 1 d .
C23 C -0.2764(6) 1.0200(2) 0.40815(14) 0.0371(7) Uani 1 1 d .
C24 C -0.4568(6) 1.0713(3) 0.44321(15) 0.0453(8) Uani 1 1 d .
H24 H -0.4821 1.0532 0.4872 0.054 Uiso 1 1 calc R
C25 C -0.5982(7) 1.1487(2) 0.41325(17) 0.0507(9) Uani 1 1 d .
H25 H -0.7237 1.1835 0.4366 0.061 Uiso 1 1 calc R
C26 C -0.5592(7) 1.1769(2) 0.34856(18) 0.0497(8) Uani 1 1 d .
H26 H -0.6570 1.2308 0.3286 0.060 Uiso 1 1 calc R
C27 C -0.3779(6) 1.1261(2) 0.31375(16) 0.0435(7) Uani 1 1 d .
H27 H -0.3498 1.1453 0.2701 0.052 Uiso 1 1 calc R
C28 C -0.2390(6) 1.0477(2) 0.34314(14) 0.0364(7) Uani 1 1 d .
C30 C 0.5779(8) 0.4873(3) 0.37950(17) 0.0572(10) Uani 1 1 d .
H30 H 0.5950 0.4395 0.4136 0.069 Uiso 1 1 calc R
C31 C 0.7565(8) 0.5646(3) 0.3807(2) 0.0685(11) Uani 1 1 d .
H31 H 0.8959 0.5709 0.4161 0.082 Uiso 1 1 calc R
C32 C 0.7332(8) 0.6327(3) 0.3306(2) 0.0682(11) Uani 1 1 d .
H32 H 0.8556 0.6863 0.3320 0.082 Uiso 1 1 calc R
C33 C 0.5351(7) 0.6240(3) 0.27890(19) 0.0576(9) Uani 1 1 d .
H33 H 0.5244 0.6697 0.2436 0.069 Uiso 1 1 calc R
C34 C 0.3528(7) 0.5490(3) 0.27856(17) 0.0574(9) Uani 1 1 d .
H34 H 0.2100 0.5440 0.2439 0.069 Uiso 1 1 calc R
C35 C 0.3765(8) 0.4802(3) 0.32894(18) 0.0582(10) Uani 1 1 d .
H35 H 0.2511 0.4276 0.3281 0.070 Uiso 1 1 calc R
O1 O 0.3006(4) 0.82579(15) 0.01205(10) 0.0455(5) Uani 1 1 d .
O2 O -0.1294(4) 0.56573(17) 0.11274(12) 0.0522(6) Uani 1 1 d .
H2B H -0.1026 0.5055 0.1183 0.078 Uiso 1 1 calc R
O3 O 0.9001(5) 0.88204(17) -0.12983(11) 0.0508(6) Uani 1 1 d .
O4 O 1.0969(4) 0.77792(16) -0.19449(10) 0.0472(6) Uani 1 1 d .
O5 O -0.3286(4) 0.80875(17) 0.15454(10) 0.0450(5) Uani 1 1 d .
O6 O 0.0160(4) 0.87176(15) 0.22311(9) 0.0337(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
N1 0.0374(13) 0.0332(13) 0.0321(12) -0.0014(10) 0.0096(10) 0.0005(10)
N2 0.0230(12) 0.0429(14) 0.0361(12) -0.0064(11) 0.0029(10) 0.0001(10)
C3 0.0301(16) 0.0390(17) 0.0349(15) -0.0022(13) 0.0066(12) 0.0007(12)
C4 0.0382(17) 0.0403(17) 0.0362(14) 0.0019(13) 0.0111(13) 0.0007(13)
C5 0.0411(17) 0.0357(17) 0.0412(16) -0.0019(14) 0.0113(13) -0.0024(13)
C2 0.0343(16) 0.0367(16) 0.0312(14) -0.0017(13) 0.0038(12) 0.0021(12)
C6 0.0296(15) 0.0393(17) 0.0306(14) -0.0026(12) 0.0038(11) 0.0020(12)
C7 0.0393(17) 0.0390(18) 0.0410(16) -0.0030(14) 0.0084(13) 0.0012(13)
C8 0.0433(18) 0.0401(17) 0.0402(16) -0.0090(14) 0.0111(14) 0.0007(14)
C9 0.0406(18) 0.0477(19) 0.0338(14) -0.0077(14) 0.0090(13) 0.0048(14)
C10 0.0334(16) 0.0426(17) 0.0285(13) -0.0042(13) 0.0034(12) 0.0039(12)
C11 0.0367(16) 0.0359(17) 0.0301(13) -0.0039(12) 0.0034(12) 0.0028(12)
C12 0.0353(16) 0.0458(19) 0.0316(14) 0.0011(13) 0.0066(12) 0.0030(13)
C13 0.056(2) 0.050(2) 0.059(2) 0.0051(17) 0.0305(17) 0.0042(17)
C14 0.0284(16) 0.0362(16) 0.0330(14) 0.0022(13) 0.0078(11) -0.0004(12)
C15 0.0301(16) 0.0416(17) 0.0376(15) -0.0012(13) 0.0119(12) 0.0012(13)
C16 0.0348(16) 0.0362(16) 0.0381(15) -0.0033(13) 0.0113(13) -0.0035(12)
C17 0.0310(16) 0.0380(17) 0.0375(15) -0.0075(13) 0.0084(12) -0.0085(12)
C18 0.0374(17) 0.0432(18) 0.0416(16) -0.0033(14) 0.0052(13) -0.0029(13)
C19 0.0418(19) 0.0475(19) 0.0468(17) 0.0035(15) 0.0012(15) -0.0027(15)
C20 0.0440(19) 0.057(2) 0.0425(17) 0.0121(16) -0.0018(15) -0.0041(16)
C21 0.0422(19) 0.055(2) 0.0429(17) -0.0021(16) 0.0078(14) -0.0058(15)
C22 0.0333(17) 0.0436(18) 0.0347(15) -0.0065(13) 0.0048(12) -0.0074(13)
C23 0.0392(17) 0.0352(17) 0.0380(15) -0.0116(13) 0.0096(13) -0.0083(13)
C24 0.0444(19) 0.051(2) 0.0430(17) -0.0103(16) 0.0143(15) -0.0084(15)
C25 0.050(2) 0.048(2) 0.056(2) -0.0219(17) 0.0158(16) -0.0034(16)
C26 0.048(2) 0.0375(19) 0.064(2) -0.0085(16) 0.0093(17) 0.0016(14)
C27 0.047(2) 0.0387(18) 0.0460(17) -0.0032(15) 0.0108(15) -0.0015(14)
C28 0.0361(16) 0.0322(16) 0.0413(16) -0.0057(13) 0.0070(13) -0.0066(12)
C30 0.063(2) 0.067(3) 0.0429(19) 0.0032(18) 0.0136(18) 0.019(2)
C31 0.059(3) 0.081(3) 0.063(2) -0.008(2) -0.0107(19) 0.014(2)
C32 0.061(3) 0.059(3) 0.083(3) 0.000(2) 0.000(2) -0.011(2)
C33 0.061(2) 0.053(2) 0.058(2) 0.0032(18) 0.0044(19) -0.0013(18)
C34 0.063(2) 0.058(2) 0.048(2) 0.0034(18) -0.0028(17) -0.0089(19)
C35 0.064(3) 0.060(2) 0.053(2) -0.0001(19) 0.0144(18) -0.0064(19)
O1 0.0593(14) 0.0346(12) 0.0459(11) 0.0001(10) 0.0214(10) 0.0012(10)
O2 0.0544(14) 0.0382(13) 0.0697(15) 0.0027(12) 0.0335(12) -0.0025(10)
O3 0.0614(15) 0.0400(13) 0.0549(13) -0.0048(11) 0.0243(11) -0.0010(11)
O4 0.0511(13) 0.0447(13) 0.0501(12) -0.0001(11) 0.0258(11) 0.0014(10)
O5 0.0282(12) 0.0607(14) 0.0468(11) -0.0123(11) 0.0077(9) -0.0006(10)
O6 0.0281(10) 0.0426(12) 0.0316(9) -0.0062(9) 0.0082(8) 0.0007(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
C2 N1 C6 126.8(2) y
C2 N1 C5 112.7(2) y
C6 N1 C5 120.5(2) y
C14 N2 C3 122.2(2) y
C14 N2 H2 118.9 ?
C3 N2 H2 118.9 ?
N2 C3 C4 114.8(2) y
N2 C3 C2 111.1(2) y
C4 C3 C2 104.5(2) y
N2 C3 H3 108.8 ?
C4 C3 H3 108.8 ?
C2 C3 H3 108.8 ?
O2 C4 C3 109.5(2) y
O2 C4 C5 114.0(3) y
C3 C4 C5 104.8(2) y
O2 C4 H4 109.5 ?
C3 C4 H4 109.5 ?
C5 C4 H4 109.5 ?
N1 C5 C4 103.4(2) y
N1 C5 H5A 111.1 ?
C4 C5 H5A 111.1 ?
N1 C5 H5B 111.1 ?
C4 C5 H5B 111.1 ?
H5A C5 H5B 109.1 ?
O1 C2 N1 127.0(3) y
O1 C2 C3 125.7(3) y
N1 C2 C3 107.3(2) y
C7 C6 C11 118.9(3) y
C7 C6 N1 119.3(3) y
C11 C6 N1 121.7(3) y
C8 C7 C6 120.1(3) y
C8 C7 H7 119.9 ?
C6 C7 H7 119.9 ?
C9 C8 C7 120.9(3) y
C9 C8 H8 119.5 ?
C7 C8 H8 119.5 ?
C8 C9 C10 120.0(3) y
C8 C9 H9 120.0 ?
C10 C9 H9 120.0 ?
C9 C10 C11 119.7(3) y
C9 C10 C12 122.7(3) y
C11 C10 C12 117.7(3) y
C6 C11 C10 120.4(3) y
C6 C11 H11 119.8 ?
C10 C11 H11 119.8 ?
O3 C12 O4 122.9(3) y
O3 C12 C10 124.4(3) y
O4 C12 C10 112.6(3) y
O4 C13 H13A 109.5 ?
O4 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
O4 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
O5 C14 N2 126.0(3) y
O5 C14 O6 123.4(2) y
N2 C14 O6 110.5(2) y
O6 C15 C16 108.6(2) y
O6 C15 H15A 110.0 ?
C16 C15 H15A 110.0 ?
O6 C15 H15B 110.0 ?
C16 C15 H15B 110.0 ?
H15A C15 H15B 108.4 ?
C28 C16 C17 102.6(2) y
C28 C16 C15 109.6(2) y
C17 C16 C15 114.4(2) y
C28 C16 H16 110.0 ?
C17 C16 H16 110.0 ?
C15 C16 H16 110.0 ?
C18 C17 C22 120.6(3) y
C18 C17 C16 129.5(3) y
C22 C17 C16 109.9(3) y
C17 C18 C19 119.3(3) y
C17 C18 H18 120.4 ?
C19 C18 H18 120.4 ?
C18 C19 C20 119.9(3) y
C18 C19 H19 120.0 ?
C20 C19 H19 120.0 ?
C21 C20 C19 121.1(3) y
C21 C20 H20 119.4 ?
C19 C20 H20 119.4 ?
C20 C21 C22 119.1(3) y
C20 C21 H21 120.4 ?
C22 C21 H21 120.4 ?
C21 C22 C17 119.9(3) y
C21 C22 C23 131.4(3) y
C17 C22 C23 108.6(3) y
C24 C23 C28 120.1(3) y
C24 C23 C22 131.2(3) y
C28 C23 C22 108.7(2) y
C25 C24 C23 119.1(3) y
C25 C24 H24 120.5 ?
C23 C24 H24 120.5 ?
C24 C25 C26 120.9(3) y
C24 C25 H25 119.6 ?
C26 C25 H25 119.6 ?
C27 C26 C25 120.0(3) y
C27 C26 H26 120.0 ?
C25 C26 H26 120.0 ?
C28 C27 C26 119.3(3) y
C28 C27 H27 120.3 ?
C26 C27 H27 120.3 ?
C27 C28 C23 120.6(3) y
C27 C28 C16 129.4(3) y
C23 C28 C16 110.0(3) y
C35 C30 C31 119.2(4) y
C35 C30 H30 120.4 ?
C31 C30 H30 120.4 ?
C32 C31 C30 120.1(4) y
C32 C31 H31 119.9 ?
C30 C31 H31 119.9 ?
C33 C32 C31 120.5(4) y
C33 C32 H32 119.7 ?
C31 C32 H32 119.7 ?
C34 C33 C32 119.5(4) y
C34 C33 H33 120.3 ?
C32 C33 H33 120.3 ?
C33 C34 C35 119.9(3) y
C33 C34 H34 120.0 ?
C35 C34 H34 120.0 ?
C30 C35 C34 120.6(4) y
C30 C35 H35 119.7 ?
C34 C35 H35 119.7 ?
C4 O2 H2B 109.5 ?
C12 O4 C13 115.7(2) y
C14 O6 C15 114.1(2) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C2 1.378(4) y
N1 C6 1.418(3) y
N1 C5 1.477(4) y
N2 C14 1.339(3) y
N2 C3 1.448(3) y
N2 H2 0.8800 ?
C3 C4 1.509(4) y
C3 C2 1.536(4) y
C3 H3 1.0000 ?
C4 O2 1.416(3) y
C4 C5 1.531(4) y
C4 H4 1.0000 ?
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C2 O1 1.208(3) y
C6 C7 1.396(4) y
C6 C11 1.397(4) y
C7 C8 1.389(4) y
C7 H7 0.9500 ?
C8 C9 1.368(4) y
C8 H8 0.9500 ?
C9 C10 1.394(4) y
C9 H9 0.9500 ?
C10 C11 1.397(4) y
C10 C12 1.481(4) y
C11 H11 0.9500 ?
C12 O3 1.206(4) y
C12 O4 1.334(3) y
C13 O4 1.455(4) y
C13 H13A 0.9800 ?
C13 H13B 0.9800 ?
C13 H13C 0.9800 ?
C14 O5 1.210(3) y
C14 O6 1.359(3) y
C15 O6 1.446(3) y
C15 C16 1.520(4) y
C15 H15A 0.9900 ?
C15 H15B 0.9900 ?
C16 C28 1.515(4) y
C16 C17 1.517(4) y
C16 H16 1.0000 ?
C17 C18 1.385(4) y
C17 C22 1.408(4) y
C18 C19 1.392(4) y
C18 H18 0.9500 ?
C19 C20 1.405(4) y
C19 H19 0.9500 ?
C20 C21 1.374(5) y
C20 H20 0.9500 ?
C21 C22 1.399(4) y
C21 H21 0.9500 ?
C22 C23 1.466(4) y
C23 C24 1.392(4) y
C23 C28 1.407(4) y
C24 C25 1.376(5) y
C24 H24 0.9500 ?
C25 C26 1.405(5) y
C25 H25 0.9500 ?
C26 C27 1.388(4) y
C26 H26 0.9500 ?
C27 C28 1.377(4) y
C27 H27 0.9500 ?
C30 C35 1.362(5) y
C30 C31 1.378(6) y
C30 H30 0.9500 ?
C31 C32 1.376(6) y
C31 H31 0.9500 ?
C32 C33 1.369(5) y
C32 H32 0.9500 ?
C33 C34 1.367(5) y
C33 H33 0.9500 ?
C34 C35 1.387(5) y
C34 H34 0.9500 ?
C35 H35 0.9500 ?
O2 H2B 0.8400 ?
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
N2 H2 O5 0.88 1.95 2.796(3) 160.3 1_655
O2 H2B O3 0.84 1.97 2.764(3) 158.4 2_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_publ_flag
C14 N2 C3 C4 -104.3(3) y
C14 N2 C3 C2 137.4(3) y
N2 C3 C4 O2 89.5(3) y
C2 C3 C4 O2 -148.5(2) y
N2 C3 C4 C5 -147.8(3) y
C2 C3 C4 C5 -25.8(3) y
C2 N1 C5 C4 -16.8(3) y
C6 N1 C5 C4 165.1(2) y
O2 C4 C5 N1 145.7(2) y
C3 C4 C5 N1 25.9(3) y
C6 N1 C2 O1 -0.5(5) y
C5 N1 C2 O1 -178.5(3) y
C6 N1 C2 C3 178.5(3) y
C5 N1 C2 C3 0.6(3) y
N2 C3 C2 O1 -40.4(4) y
C4 C3 C2 O1 -164.7(3) y
N2 C3 C2 N1 140.5(2) y
C4 C3 C2 N1 16.2(3) y
C2 N1 C6 C7 -171.5(3) y
C5 N1 C6 C7 6.3(4) y
C2 N1 C6 C11 9.5(4) y
C5 N1 C6 C11 -172.8(3) y
C11 C6 C7 C8 1.5(4) y
N1 C6 C7 C8 -177.5(3) y
C6 C7 C8 C9 -0.7(4) y
C7 C8 C9 C10 -0.2(5) y
C8 C9 C10 C11 0.2(4) y
C8 C9 C10 C12 -179.5(3) y
C7 C6 C11 C10 -1.5(4) y
N1 C6 C11 C10 177.5(2) y
C9 C10 C11 C6 0.6(4) y
C12 C10 C11 C6 -179.6(3) y
C9 C10 C12 O3 176.2(3) y
C11 C10 C12 O3 -3.6(4) y
C9 C10 C12 O4 -2.9(4) y
C11 C10 C12 O4 177.3(2) y
C3 N2 C14 O5 -2.5(5) y
C3 N2 C14 O6 177.9(2) y
O6 C15 C16 C28 172.3(2) y
O6 C15 C16 C17 -73.1(3) y
C28 C16 C17 C18 -178.4(3) y
C15 C16 C17 C18 62.9(4) y
C28 C16 C17 C22 3.3(3) y
C15 C16 C17 C22 -115.4(3) y
C22 C17 C18 C19 -1.1(4) y
C16 C17 C18 C19 -179.3(3) y
C17 C18 C19 C20 1.3(5) y
C18 C19 C20 C21 -0.9(5) y
C19 C20 C21 C22 0.2(5) y
C20 C21 C22 C17 -0.1(5) y
C20 C21 C22 C23 -178.4(3) y
C18 C17 C22 C21 0.5(4) y
C16 C17 C22 C21 179.0(3) y
C18 C17 C22 C23 179.2(3) y
C16 C17 C22 C23 -2.3(3) y
C21 C22 C23 C24 -1.9(5) y
C17 C22 C23 C24 179.7(3) y
C21 C22 C23 C28 178.8(3) y
C17 C22 C23 C28 0.3(3) y
C28 C23 C24 C25 0.4(4) y
C22 C23 C24 C25 -178.9(3) y
C23 C24 C25 C26 -1.0(5) y
C24 C25 C26 C27 0.5(5) y
C25 C26 C27 C28 0.5(5) y
C26 C27 C28 C23 -1.0(5) y
C26 C27 C28 C16 176.8(3) y
C24 C23 C28 C27 0.6(4) y
C22 C23 C28 C27 -179.9(3) y
C24 C23 C28 C16 -177.6(3) y
C22 C23 C28 C16 1.8(3) y
C17 C16 C28 C27 178.9(3) y
C15 C16 C28 C27 -59.2(4) y
C17 C16 C28 C23 -3.1(3) y
C15 C16 C28 C23 118.9(3) y
C35 C30 C31 C32 -1.0(6) y
C30 C31 C32 C33 -0.7(6) y
C31 C32 C33 C34 2.6(6) y
C32 C33 C34 C35 -2.7(6) y
C31 C30 C35 C34 0.9(6) y
C33 C34 C35 C30 1.0(6) y
O3 C12 O4 C13 3.6(4) y
C10 C12 O4 C13 -177.3(3) y
O5 C14 O6 C15 -8.2(4) y
N2 C14 O6 C15 171.5(2) y
C16 C15 O6 C14 176.9(2) y
|
1501545.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:23:32 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501545.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_1501545
loop_
_publ_author_name
'Daniel J. St-Cyr'
'Thierry Maris'
'William D. Lubel'
_publ_section_title
;
Crystal-State Structural Analysis of Beta-Hydroxy-gamma-Lactam
Constrained SER/THR Peptidomimetics
;
_journal_name_full Heterocycles
_journal_page_first 729
_journal_page_last 737
_journal_paper_doi 10.3987/COM-10-S(E)52
_journal_volume 82
_journal_year 2010
_chemical_absolute_configuration rmad
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C26 H30 N2 O6'
_chemical_formula_sum 'C26 H30 N2 O6'
_chemical_formula_weight 466.52
_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
_audit_creation_method SHELXL-97
_cell_angle_alpha 90
_cell_angle_beta 105.559(1)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.1833(3)
_cell_length_b 6.0199(1)
_cell_length_c 14.6315(3)
_cell_measurement_reflns_used 4513
_cell_measurement_temperature 150
_cell_measurement_theta_max 71.31
_cell_measurement_theta_min 3.14
_cell_volume 1203.49(4)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.037
_diffrn_reflns_av_sigmaI/netI 0.0375
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 14307
_diffrn_reflns_theta_full 72.57
_diffrn_reflns_theta_max 72.57
_diffrn_reflns_theta_min 3.14
_exptl_absorpt_coefficient_mu 0.752
_exptl_absorpt_correction_T_max 0.9137
_exptl_absorpt_correction_T_min 0.7675
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.287
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.155
_refine_diff_density_min -0.140
_refine_diff_density_rms 0.034
_refine_ls_abs_structure_details 'Flack H D (1983), 1909 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.26(18)
_refine_ls_extinction_coef 0.0035(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 1.055
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 351
_refine_ls_number_reflns 4540
_refine_ls_number_restraints 118
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0477
_refine_ls_R_factor_gt 0.0408
_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^)+(0.0588P)^2^+0.0687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1027
_refine_ls_wR_factor_ref 0.1063
_reflns_number_gt 4006
_reflns_number_total 4540
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block lube47
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
;
_cod_original_sg_symbol_H-M P21
_cod_database_code 1501545
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
N2 N 0.05006(12) 1.0617(3) 0.63156(13) 0.0414(4) Uani 1 1 d . . .
H2A H 0.0858 1.0369 0.5919 0.050 Uiso 1 1 calc R . .
C2 C -0.12199(14) 1.1004(3) 0.63597(14) 0.0357(4) Uani 1 1 d . . .
O1 O -0.16202(10) 0.9189(2) 0.61466(10) 0.0395(3) Uani 1 1 d . . .
C3 C -0.03807(14) 1.1918(3) 0.59949(15) 0.0367(4) Uani 1 1 d . . .
H3 H -0.0589 1.1867 0.5286 0.044 Uiso 1 1 calc R . .
C4 C -0.03332(15) 1.4378(3) 0.63026(15) 0.0394(5) Uani 1 1 d . . .
H4A H 0.0355 1.4945 0.6486 0.047 Uiso 1 1 calc R . .
O2 O -0.09223(11) 1.5535(2) 0.55030(11) 0.0457(4) Uani 1 1 d . . .
H2 H -0.1135 1.6711 0.5685 0.069 Uiso 1 1 calc . . .
C5 C -0.07822(14) 1.4400(3) 0.71396(14) 0.0372(5) Uani 1 1 d . . .
H5A H -0.0277 1.4179 0.7747 0.045 Uiso 1 1 calc R . .
H5B H -0.1131 1.5812 0.7168 0.045 Uiso 1 1 calc R . .
N1 N -0.14653(11) 1.2515(3) 0.69288(11) 0.0339(4) Uani 1 1 d . . .
C6 C -0.21641(14) 1.1992(3) 0.74673(13) 0.0341(4) Uani 1 1 d . . .
H6 H -0.2569 1.0702 0.7156 0.041 Uiso 1 1 calc R . .
C7 C -0.28515(14) 1.3932(3) 0.74953(13) 0.0353(4) Uani 1 1 d . . .
H7A H -0.2467 1.5148 0.7875 0.042 Uiso 1 1 calc R . .
H7B H -0.3342 1.3441 0.7822 0.042 Uiso 1 1 calc R . .
C8 C -0.33898(15) 1.4846(3) 0.65152(14) 0.0384(4) Uani 1 1 d . . .
H8 H -0.2895 1.5546 0.6231 0.046 Uiso 1 1 calc R . .
C9 C -0.39166(17) 1.3042(4) 0.58441(15) 0.0506(6) Uani 1 1 d . . .
H9A H -0.4314 1.3724 0.5259 0.076 Uiso 1 1 calc R . .
H9B H -0.4342 1.2199 0.6147 0.076 Uiso 1 1 calc R . .
H9C H -0.3435 1.2040 0.5694 0.076 Uiso 1 1 calc R . .
C10 C -0.41107(18) 1.6635(4) 0.66235(17) 0.0530(6) Uani 1 1 d . . .
H10A H -0.3767 1.7762 0.7074 0.080 Uiso 1 1 calc R . .
H10B H -0.4629 1.5963 0.6860 0.080 Uiso 1 1 calc R . .
H10C H -0.4400 1.7330 0.6006 0.080 Uiso 1 1 calc R . .
C11 C -0.15823(15) 1.1276(3) 0.84600(15) 0.0376(5) Uani 1 1 d . . .
O3 O -0.12090(12) 1.2541(2) 0.90877(10) 0.0509(4) Uani 1 1 d . . .
O4 O -0.15208(12) 0.9078(2) 0.85261(11) 0.0493(4) Uani 1 1 d . . .
C12 C -0.0893(2) 0.8241(4) 0.94143(19) 0.0724(9) Uani 1 1 d . . .
H12A H -0.1053 0.8997 0.9947 0.109 Uiso 1 1 calc R . .
H12B H -0.0207 0.8522 0.9436 0.109 Uiso 1 1 calc R . .
H12C H -0.0997 0.6640 0.9459 0.109 Uiso 1 1 calc R . .
O5 O 0.03950(13) 1.0030(3) 0.78198(12) 0.0650(5) Uani 1 1 d . . .
C14 C 0.07993(16) 0.9764(4) 0.72009(17) 0.0461(5) Uani 1 1 d . A .
O6 O 0.16082(11) 0.8496(3) 0.72865(12) 0.0541(4) Uani 1 1 d . . .
C15 C 0.1886(2) 0.7237(6) 0.8195(2) 0.0484(7) Uani 0.762(2) 1 d PDU A 1
H15A H 0.1463 0.5913 0.8161 0.058 Uiso 0.762(2) 1 calc PR A 1
H15B H 0.1822 0.8184 0.8729 0.058 Uiso 0.762(2) 1 calc PR A 1
C16 C 0.29511(19) 0.6550(5) 0.83262(19) 0.0399(6) Uani 0.762(2) 1 d PDU A 1
H16 H 0.3356 0.7920 0.8353 0.048 Uiso 0.762(2) 1 calc PR A 1
C17 C 0.3146(2) 0.5001(5) 0.75755(19) 0.0386(6) Uani 0.762(2) 1 d PDU A 1
C18 C 0.2915(2) 0.5244(6) 0.6600(2) 0.0472(7) Uani 0.762(2) 1 d PDU A 1
H18 H 0.2589 0.6542 0.6305 0.057 Uiso 0.762(2) 1 calc PR A 1
C19 C 0.3164(7) 0.3570(12) 0.6060(5) 0.0539(16) Uani 0.762(2) 1 d PDU A 1
H19 H 0.2984 0.3689 0.5388 0.065 Uiso 0.762(2) 1 calc PR A 1
C20 C 0.3677(17) 0.171(3) 0.6494(6) 0.0504(9) Uani 0.762(2) 1 d PDU A 1
H20 H 0.3854 0.0589 0.6117 0.061 Uiso 0.762(2) 1 calc PR A 1
C21 C 0.393(2) 0.149(4) 0.7472(6) 0.0449(7) Uani 0.762(2) 1 d PDU A 1
H21 H 0.4304 0.0247 0.7768 0.054 Uiso 0.762(2) 1 calc PR A 1
C22 C 0.3640(3) 0.3101(6) 0.8014(3) 0.0368(10) Uani 0.762(2) 1 d PDU A 1
C23 C 0.3751(3) 0.3236(6) 0.9038(3) 0.0361(9) Uani 0.762(2) 1 d PDU A 1
C24 C 0.4144(14) 0.175(3) 0.9772(5) 0.0420(9) Uani 0.762(2) 1 d PDU A 1
H24 H 0.4413 0.0373 0.9644 0.050 Uiso 0.762(2) 1 calc PR A 1
C25 C 0.414(2) 0.230(4) 1.0693(5) 0.0454(17) Uani 0.762(2) 1 d PDU A 1
H25 H 0.4414 0.1311 1.1199 0.054 Uiso 0.762(2) 1 calc PR A 1
C26 C 0.3728(2) 0.4297(6) 1.0877(2) 0.0456(8) Uani 0.762(2) 1 d PDU A 1
H26 H 0.3720 0.4648 1.1508 0.055 Uiso 0.762(2) 1 calc PR A 1
C27 C 0.3333(2) 0.5776(5) 1.0152(2) 0.0445(7) Uani 0.762(2) 1 d PDU A 1
H27 H 0.3059 0.7139 1.0284 0.053 Uiso 0.762(2) 1 calc PR A 1
C28 C 0.33414(19) 0.5251(5) 0.92332(18) 0.0374(6) Uani 0.762(2) 1 d PDU A 1
C15B C 0.2292(9) 0.7927(16) 0.8108(8) 0.0484(7) Uani 0.238(2) 1 d PDU A 2
H15C H 0.2111 0.8526 0.8668 0.058 Uiso 0.238(2) 1 calc PR A 2
H15D H 0.2946 0.8502 0.8109 0.058 Uiso 0.238(2) 1 calc PR A 2
C16B C 0.2288(6) 0.5356(13) 0.8117(5) 0.0399(6) Uani 0.238(2) 1 d PDU A 2
H16B H 0.1600 0.4811 0.8001 0.048 Uiso 0.238(2) 1 calc PR A 2
C17B C 0.2770(7) 0.4235(16) 0.7421(6) 0.0386(6) Uani 0.238(2) 1 d PDU A 2
C18B C 0.2548(8) 0.4392(19) 0.6436(7) 0.0472(7) Uani 0.238(2) 1 d PDU A 2
H18B H 0.2036 0.5335 0.6097 0.057 Uiso 0.238(2) 1 calc PR A 2
C19B C 0.309(3) 0.315(5) 0.5960(18) 0.0539(16) Uani 0.238(2) 1 d PDU A 2
H19B H 0.3005 0.3380 0.5301 0.065 Uiso 0.238(2) 1 calc PR A 2
C20B C 0.375(6) 0.156(11) 0.644(2) 0.0504(9) Uani 0.238(2) 1 d PDU A 2
H20B H 0.4062 0.0605 0.6089 0.061 Uiso 0.238(2) 1 calc PR A 2
C21B C 0.396(8) 0.136(15) 0.741(2) 0.0449(7) Uani 0.238(2) 1 d PDU A 2
H21B H 0.4422 0.0296 0.7738 0.054 Uiso 0.238(2) 1 calc PR A 2
C22B C 0.3485(13) 0.273(3) 0.7906(10) 0.0368(10) Uani 0.238(2) 1 d PDU A 2
C23B C 0.3562(11) 0.288(3) 0.8924(10) 0.0361(9) Uani 0.238(2) 1 d PDU A 2
C24B C 0.417(5) 0.176(10) 0.9693(16) 0.0420(9) Uani 0.238(2) 1 d PDU A 2
H24B H 0.4641 0.0723 0.9599 0.050 Uiso 0.238(2) 1 calc PR A 2
C25B C 0.408(7) 0.220(14) 1.060(2) 0.0454(17) Uani 0.238(2) 1 d PDU A 2
H25B H 0.4468 0.1414 1.1130 0.054 Uiso 0.238(2) 1 calc PR A 2
C26B C 0.3421(9) 0.382(2) 1.0714(9) 0.0456(8) Uani 0.238(2) 1 d PDU A 2
H26B H 0.3370 0.4138 1.1334 0.055 Uiso 0.238(2) 1 calc PR A 2
C27B C 0.2836(7) 0.4962(17) 0.9951(6) 0.0445(7) Uani 0.238(2) 1 d PDU A 2
H27B H 0.2398 0.6074 1.0049 0.053 Uiso 0.238(2) 1 calc PR A 2
C28B C 0.2896(6) 0.4482(15) 0.9060(5) 0.0374(6) Uani 0.238(2) 1 d PDU 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
N2 0.0395(9) 0.0342(8) 0.0492(10) 0.0028(7) 0.0098(8) 0.0083(7)
C2 0.0381(10) 0.0236(8) 0.0409(10) -0.0004(7) 0.0029(8) 0.0060(7)
O1 0.0436(8) 0.0236(6) 0.0484(8) -0.0057(6) 0.0075(6) -0.0013(6)
C3 0.0371(10) 0.0268(9) 0.0437(11) -0.0016(8) 0.0065(8) 0.0054(8)
C4 0.0406(11) 0.0269(9) 0.0510(11) -0.0011(8) 0.0126(9) -0.0004(8)
O2 0.0604(9) 0.0268(6) 0.0529(9) 0.0040(6) 0.0202(7) 0.0109(6)
C5 0.0397(10) 0.0240(9) 0.0454(11) -0.0019(8) 0.0069(9) -0.0019(8)
N1 0.0349(8) 0.0237(7) 0.0394(8) -0.0033(6) 0.0036(7) 0.0011(6)
C6 0.0357(10) 0.0249(8) 0.0385(10) -0.0003(7) 0.0046(8) -0.0005(7)
C7 0.0362(10) 0.0309(9) 0.0365(10) 0.0006(8) 0.0057(8) -0.0003(8)
C8 0.0384(10) 0.0351(9) 0.0383(10) 0.0035(8) 0.0044(8) 0.0018(8)
C9 0.0498(12) 0.0514(12) 0.0419(11) -0.0031(10) -0.0030(10) 0.0028(11)
C10 0.0521(13) 0.0412(11) 0.0560(13) 0.0030(10) -0.0024(11) 0.0101(10)
C11 0.0391(10) 0.0273(9) 0.0429(11) 0.0010(8) 0.0051(9) -0.0002(8)
O3 0.0635(10) 0.0309(7) 0.0446(8) 0.0000(6) -0.0093(7) -0.0013(7)
O4 0.0607(9) 0.0260(6) 0.0475(8) 0.0032(6) -0.0091(7) 0.0021(7)
C12 0.100(2) 0.0303(10) 0.0601(15) 0.0074(11) -0.0246(15) 0.0033(13)
O5 0.0697(11) 0.0733(12) 0.0506(9) 0.0087(9) 0.0137(9) 0.0350(10)
C14 0.0428(12) 0.0381(10) 0.0529(12) -0.0025(9) 0.0051(10) 0.0096(9)
O6 0.0484(9) 0.0501(9) 0.0570(9) 0.0039(7) 0.0027(7) 0.0184(7)
C15 0.0423(19) 0.0515(18) 0.0492(14) 0.0080(14) 0.0085(15) 0.0107(14)
C16 0.0344(12) 0.0364(12) 0.0461(14) 0.0012(11) 0.0058(11) -0.0002(10)
C17 0.0333(15) 0.0387(15) 0.0413(13) 0.0035(12) 0.0059(12) -0.0024(11)
C18 0.0386(18) 0.0536(19) 0.0458(14) 0.0056(14) 0.0051(13) 0.0042(13)
C19 0.052(2) 0.065(4) 0.043(2) 0.0009(19) 0.0100(18) 0.001(3)
C20 0.055(4) 0.047(3) 0.0503(17) -0.0089(19) 0.0148(17) -0.0032(13)
C21 0.049(2) 0.034(4) 0.0497(17) -0.002(2) 0.010(2) 0.0008(15)
C22 0.035(2) 0.0330(19) 0.0404(15) -0.0025(12) 0.0071(13) -0.0044(16)
C23 0.033(2) 0.0319(17) 0.0402(15) 0.0002(12) 0.0045(14) -0.0057(14)
C24 0.0439(16) 0.0346(10) 0.0462(16) 0.0021(18) 0.0098(18) -0.0005(12)
C25 0.048(3) 0.042(3) 0.044(2) 0.006(3) 0.008(3) -0.002(3)
C26 0.045(2) 0.0471(19) 0.0434(17) -0.0064(13) 0.0099(15) -0.0054(14)
C27 0.0421(16) 0.0426(15) 0.0474(15) -0.0053(12) 0.0096(13) 0.0030(12)
C28 0.0317(14) 0.0386(14) 0.0398(13) -0.0025(11) 0.0058(11) -0.0030(11)
C15B 0.0423(19) 0.0515(18) 0.0492(14) 0.0080(14) 0.0085(15) 0.0107(14)
C16B 0.0344(12) 0.0364(12) 0.0461(14) 0.0012(11) 0.0058(11) -0.0002(10)
C17B 0.0333(15) 0.0387(15) 0.0413(13) 0.0035(12) 0.0059(12) -0.0024(11)
C18B 0.0386(18) 0.0536(19) 0.0458(14) 0.0056(14) 0.0051(13) 0.0042(13)
C19B 0.052(2) 0.065(4) 0.043(2) 0.0009(19) 0.0100(18) 0.001(3)
C20B 0.055(4) 0.047(3) 0.0503(17) -0.0089(19) 0.0148(17) -0.0032(13)
C21B 0.049(2) 0.034(4) 0.0497(17) -0.002(2) 0.010(2) 0.0008(15)
C22B 0.035(2) 0.0330(19) 0.0404(15) -0.0025(12) 0.0071(13) -0.0044(16)
C23B 0.033(2) 0.0319(17) 0.0402(15) 0.0002(12) 0.0045(14) -0.0057(14)
C24B 0.0439(16) 0.0346(10) 0.0462(16) 0.0021(18) 0.0098(18) -0.0005(12)
C25B 0.048(3) 0.042(3) 0.044(2) 0.006(3) 0.008(3) -0.002(3)
C26B 0.045(2) 0.0471(19) 0.0434(17) -0.0064(13) 0.0099(15) -0.0054(14)
C27B 0.0421(16) 0.0426(15) 0.0474(15) -0.0053(12) 0.0096(13) 0.0030(12)
C28B 0.0317(14) 0.0386(14) 0.0398(13) -0.0025(11) 0.0058(11) -0.0030(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
C14 N2 C3 122.65(19) y
C14 N2 H2A 118.7 ?
C3 N2 H2A 118.7 ?
O1 C2 N1 125.5(2) y
O1 C2 C3 125.36(19) y
N1 C2 C3 109.17(15) y
N2 C3 C2 112.23(16) y
N2 C3 C4 117.35(17) y
C2 C3 C4 102.71(16) y
N2 C3 H3 108.0 ?
C2 C3 H3 108.0 ?
C4 C3 H3 108.0 ?
O2 C4 C5 112.10(16) y
O2 C4 C3 105.05(16) y
C5 C4 C3 104.35(16) y
O2 C4 H4A 111.6 ?
C5 C4 H4A 111.6 ?
C3 C4 H4A 111.6 ?
C4 O2 H2 109.5 ?
N1 C5 C4 102.62(15) y
N1 C5 H5A 111.2 ?
C4 C5 H5A 111.2 ?
N1 C5 H5B 111.2 ?
C4 C5 H5B 111.2 ?
H5A C5 H5B 109.2 ?
C2 N1 C6 121.12(16) y
C2 N1 C5 112.81(17) y
C6 N1 C5 124.01(16) y
N1 C6 C11 107.64(15) y
N1 C6 C7 112.36(15) y
C11 C6 C7 112.07(16) y
N1 C6 H6 108.2 ?
C11 C6 H6 108.2 ?
C7 C6 H6 108.2 ?
C6 C7 C8 114.20(16) y
C6 C7 H7A 108.7 ?
C8 C7 H7A 108.7 ?
C6 C7 H7B 108.7 ?
C8 C7 H7B 108.7 ?
H7A C7 H7B 107.6 ?
C9 C8 C10 110.19(18) y
C9 C8 C7 112.52(16) y
C10 C8 C7 109.63(17) y
C9 C8 H8 108.1 ?
C10 C8 H8 108.1 ?
C7 C8 H8 108.1 ?
C8 C9 H9A 109.5 ?
C8 C9 H9B 109.5 ?
H9A C9 H9B 109.5 ?
C8 C9 H9C 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
C8 C10 H10A 109.5 ?
C8 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C8 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
O3 C11 O4 124.68(19) y
O3 C11 C6 124.29(16) y
O4 C11 C6 111.00(16) y
C11 O4 C12 115.02(17) y
O4 C12 H12A 109.5 ?
O4 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
O4 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
O5 C14 N2 125.4(2) y
O5 C14 O6 124.5(2) y
N2 C14 O6 110.0(2) y
C14 O6 C15B 127.2(5) y
C14 O6 C15 112.6(2) y
O6 C15 C16 105.4(3) y
O6 C15 H15A 110.7 ?
C16 C15 H15A 110.7 ?
O6 C15 H15B 110.7 ?
C16 C15 H15B 110.7 ?
H15A C15 H15B 108.8 ?
C28 C16 C17 102.8(2) y
C28 C16 C15 111.5(2) y
C17 C16 C15 116.2(2) y
C28 C16 H16 108.7 ?
C17 C16 H16 108.7 ?
C15 C16 H16 108.7 ?
C18 C17 C22 120.6(3) y
C18 C17 C16 129.9(3) y
C22 C17 C16 109.5(3) y
C19 C18 C17 119.0(4) y
C19 C18 H18 120.5 ?
C17 C18 H18 120.5 ?
C18 C19 C20 120.5(6) y
C18 C19 H19 119.8 ?
C20 C19 H19 119.8 ?
C21 C20 C19 120.7(8) y
C21 C20 H20 119.7 ?
C19 C20 H20 119.7 ?
C22 C21 C20 119.2(7) y
C22 C21 H21 120.4 ?
C20 C21 H21 120.4 ?
C21 C22 C17 119.9(5) y
C21 C22 C23 131.1(5) y
C17 C22 C23 109.0(3) y
C24 C23 C28 120.0(4) y
C24 C23 C22 131.5(5) y
C28 C23 C22 108.5(3) y
C25 C24 C23 119.1(9) y
C25 C24 H24 120.4 ?
C23 C24 H24 120.4 ?
C24 C25 C26 120.4(8) y
C24 C25 H25 119.8 ?
C26 C25 H25 119.8 ?
C27 C26 C25 120.7(4) y
C27 C26 H26 119.6 ?
C25 C26 H26 119.6 ?
C26 C27 C28 119.4(3) y
C26 C27 H27 120.3 ?
C28 C27 H27 120.3 ?
C27 C28 C23 120.3(3) y
C27 C28 C16 129.7(3) y
C23 C28 C16 110.0(3) y
O6 C15B C16B 104.7(8) y
O6 C15B H15C 110.8 ?
C16B C15B H15C 110.8 ?
O6 C15B H15D 110.8 ?
C16B C15B H15D 110.8 ?
H15C C15B H15D 108.9 ?
C28B C16B C17B 102.0(6) y
C28B C16B C15B 110.6(7) y
C17B C16B C15B 115.7(8) y
C28B C16B H16B 109.4 ?
C17B C16B H16B 109.4 ?
C15B C16B H16B 109.4 ?
C18B C17B C22B 119.9(9) y
C18B C17B C16B 130.0(8) y
C22B C17B C16B 109.9(8) y
C19B C18B C17B 118.7(13) y
C19B C18B H18B 120.6 ?
C17B C18B H18B 120.6 ?
C18B C19B C20B 120.8(19) y
C18B C19B H19B 119.6 ?
C20B C19B H19B 119.6 ?
C21B C20B C19B 120.4(19) y
C21B C20B H20B 119.8 ?
C19B C20B H20B 119.8 ?
C20B C21B C22B 119.2(19) y
C20B C21B H21B 120.4 ?
C22B C21B H21B 120.4 ?
C21B C22B C17B 120.5(15) y
C21B C22B C23B 130.9(15) y
C17B C22B C23B 108.6(11) y
C24B C23B C28B 121.0(13) y
C24B C23B C22B 130.4(14) y
C28B C23B C22B 108.6(11) y
C25B C24B C23B 118.7(19) y
C25B C24B H24B 120.7 ?
C23B C24B H24B 120.7 ?
C24B C25B C26B 119.1(18) y
C24B C25B H25B 120.5 ?
C26B C25B H25B 120.5 ?
C27B C26B C25B 121.8(13) y
C27B C26B H26B 119.1 ?
C25B C26B H26B 119.1 ?
C28B C27B C26B 119.3(9) y
C28B C27B H27B 120.4 ?
C26B C27B H27B 120.4 ?
C27B C28B C23B 120.0(9) y
C27B C28B C16B 129.4(7) y
C23B C28B C16B 110.6(8) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N2 C14 1.352(3) y
N2 C3 1.442(2) y
N2 H2A 0.8800 ?
C2 O1 1.232(2) y
C2 N1 1.341(3) y
C2 C3 1.531(3) y
C3 C4 1.544(3) y
C3 H3 1.0000 ?
C4 O2 1.424(2) y
C4 C5 1.524(3) y
C4 H4A 1.0000 ?
O2 H2 0.8400 ?
C5 N1 1.470(2) y
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
N1 C6 1.457(3) y
C6 C11 1.527(3) y
C6 C7 1.529(2) y
C6 H6 1.0000 ?
C7 C8 1.534(3) y
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 C9 1.519(3) y
C8 C10 1.522(3) y
C8 H8 1.0000 ?
C9 H9A 0.9800 ?
C9 H9B 0.9800 ?
C9 H9C 0.9800 ?
C10 H10A 0.9800 ?
C10 H10B 0.9800 ?
C10 H10C 0.9800 ?
C11 O3 1.201(2) y
C11 O4 1.328(2) y
O4 C12 1.454(3) y
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
O5 C14 1.205(3) y
C14 O6 1.356(2) y
O6 C15B 1.371(11) y
O6 C15 1.489(3) y
C15 C16 1.528(4) y
C15 H15A 0.9900 ?
C15 H15B 0.9900 ?
C16 C28 1.511(3) y
C16 C17 1.522(4) y
C16 H16 1.0000 ?
C17 C18 1.384(4) y
C17 C22 1.403(4) y
C18 C19 1.383(5) y
C18 H18 0.9500 ?
C19 C20 1.390(7) y
C19 H19 0.9500 ?
C20 C21 1.385(5) y
C20 H20 0.9500 ?
C21 C22 1.385(8) y
C21 H21 0.9500 ?
C22 C23 1.467(4) y
C23 C24 1.395(7) y
C23 C28 1.407(4) y
C24 C25 1.391(6) y
C24 H24 0.9500 ?
C25 C26 1.392(10) y
C25 H25 0.9500 ?
C26 C27 1.383(4) y
C26 H26 0.9500 ?
C27 C28 1.384(4) y
C27 H27 0.9500 ?
C15B C16B 1.548(11) y
C15B H15C 0.9900 ?
C15B H15D 0.9900 ?
C16B C28B 1.512(10) y
C16B C17B 1.527(11) y
C16B H16B 1.0000 ?
C17B C18B 1.393(11) y
C17B C22B 1.403(13) y
C18B C19B 1.387(15) y
C18B H18B 0.9500 ?
C19B C20B 1.388(16) y
C19B H19B 0.9500 ?
C20B C21B 1.383(15) y
C20B H20B 0.9500 ?
C21B C22B 1.384(15) y
C21B H21B 0.9500 ?
C22B C23B 1.468(13) y
C23B C24B 1.395(15) y
C23B C28B 1.399(13) y
C24B C25B 1.389(15) y
C24B H24B 0.9500 ?
C25B C26B 1.392(17) y
C25B H25B 0.9500 ?
C26B C27B 1.383(12) y
C26B H26B 0.9500 ?
C27B C28B 1.360(10) y
C27B H27B 0.9500 ?
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
N2 H2A O2 0.88 2.11 2.880(2) 145.9 2_546
O2 H2 O1 0.84 1.85 2.6843(19) 176.3 1_565
|
1501546.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501546.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_1501546
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C9 H18 O2, C8 H8 N6'
_chemical_formula_sum 'C17 H26 N6 O2'
_chemical_formula_weight 346.44
_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 67.342(2)
_cell_angle_beta 85.030(2)
_cell_angle_gamma 89.545(2)
_cell_formula_units_Z 2
_cell_length_a 8.0471(4)
_cell_length_b 10.3951(5)
_cell_length_c 11.6890(5)
_cell_measurement_reflns_used 9533
_cell_measurement_temperature 150
_cell_measurement_theta_max 67.79
_cell_measurement_theta_min 4.61
_cell_volume 898.59(7)
_computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.054
_diffrn_reflns_av_sigmaI/netI 0.0488
_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 9
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 13101
_diffrn_reflns_theta_full 68.02
_diffrn_reflns_theta_max 68.02
_diffrn_reflns_theta_min 4.61
_exptl_absorpt_coefficient_mu 0.710
_exptl_absorpt_correction_T_max 0.9315
_exptl_absorpt_correction_T_min 0.7824
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.280
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 372
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.227
_refine_diff_density_min -0.203
_refine_diff_density_rms 0.045
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 227
_refine_ls_number_reflns 3214
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.031
_refine_ls_R_factor_all 0.0433
_refine_ls_R_factor_gt 0.0422
_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^)+(0.0650P)^2^+0.2135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1164
_refine_ls_wR_factor_ref 0.1177
_reflns_number_gt 3069
_reflns_number_total 3214
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam13
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501546
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
C1 C -0.15084(18) 2.12160(14) 0.34433(12) 0.0352(3) Uani 1 1 d .
H1 H -0.1326 2.2191 0.3000 0.042 Uiso 1 1 calc R
C2 C -0.23113(19) 2.07577(14) 0.46345(12) 0.0373(3) Uani 1 1 d .
H2 H -0.2664 2.1402 0.4996 0.045 Uiso 1 1 calc R
C3 C -0.25860(18) 1.93447(14) 0.52813(12) 0.0354(3) Uani 1 1 d .
H3 H -0.3136 1.8995 0.6099 0.042 Uiso 1 1 calc R
C4 C -0.20461(15) 1.84426(13) 0.47186(11) 0.0290(3) Uani 1 1 d .
H4 H -0.2226 1.7464 0.5141 0.035 Uiso 1 1 calc R
C5 C -0.12370(14) 1.89953(12) 0.35246(10) 0.0242(3) Uani 1 1 d .
C6 C -0.06523(13) 1.80645(12) 0.28723(10) 0.0229(3) Uani 1 1 d .
C7 C -0.00215(14) 1.59043(12) 0.29561(10) 0.0236(3) Uani 1 1 d .
C8 C 0.01212(14) 1.77551(12) 0.10932(10) 0.0240(3) Uani 1 1 d .
N1 N -0.09762(13) 2.03686(11) 0.28821(9) 0.0299(3) Uani 1 1 d .
N2 N -0.04834(12) 1.67197(10) 0.35890(9) 0.0243(2) Uani 1 1 d .
N3 N 0.02707(12) 1.63748(10) 0.17083(9) 0.0258(2) Uani 1 1 d .
N4 N -0.03654(12) 1.86532(10) 0.16390(9) 0.0240(2) Uani 1 1 d .
N5 N 0.01513(13) 1.45463(10) 0.35985(9) 0.0273(2) Uani 1 1 d .
H5A H 0.0445 1.3996 0.3206 0.033 Uiso 1 1 calc .
H5B H -0.0029 1.4199 0.4415 0.033 Uiso 1 1 calc .
N6 N 0.04595(14) 1.82775(11) -0.01360(9) 0.0310(3) Uani 1 1 d .
H6A H 0.0770 1.7724 -0.0521 0.037 Uiso 1 1 calc .
H6B H 0.0373 1.9177 -0.0565 0.037 Uiso 1 1 calc .
C9 C 0.24855(16) 1.38669(13) 0.09987(11) 0.0298(3) Uani 1 1 d .
C10 C 0.36729(17) 1.33438(14) 0.02217(12) 0.0353(3) Uani 1 1 d .
H10A H 0.4459 1.4115 -0.0301 0.042 Uiso 1 1 calc R
H10B H 0.3029 1.3082 -0.0344 0.042 Uiso 1 1 calc R
C11 C 0.46771(16) 1.20974(14) 0.09625(13) 0.0361(3) Uani 1 1 d .
H11A H 0.5707 1.2073 0.0444 0.043 Uiso 1 1 calc R
H11B H 0.5015 1.2232 0.1704 0.043 Uiso 1 1 calc R
C12 C 0.37525(16) 1.06983(14) 0.13877(12) 0.0333(3) Uani 1 1 d .
H12A H 0.3391 1.0563 0.0652 0.040 Uiso 1 1 calc R
H12B H 0.2741 1.0701 0.1933 0.040 Uiso 1 1 calc R
C13 C 0.48335(16) 0.94873(14) 0.20933(12) 0.0335(3) Uani 1 1 d .
H13A H 0.5901 0.9555 0.1581 0.040 Uiso 1 1 calc R
H13B H 0.5094 0.9578 0.2872 0.040 Uiso 1 1 calc R
C14 C 0.40290(16) 0.80569(14) 0.24189(13) 0.0347(3) Uani 1 1 d .
H14A H 0.3583 0.8026 0.1666 0.042 Uiso 1 1 calc R
H14B H 0.3076 0.7921 0.3053 0.042 Uiso 1 1 calc R
C15 C 0.52227(15) 0.68628(14) 0.29141(12) 0.0321(3) Uani 1 1 d .
H15A H 0.6211 0.7032 0.2303 0.039 Uiso 1 1 calc R
H15B H 0.5611 0.6857 0.3697 0.039 Uiso 1 1 calc R
C16 C 0.44504(17) 0.54363(14) 0.31638(13) 0.0367(3) Uani 1 1 d .
H16A H 0.3592 0.5193 0.3879 0.044 Uiso 1 1 calc R
H16B H 0.3886 0.5488 0.2428 0.044 Uiso 1 1 calc R
C17 C 0.57172(19) 0.42869(15) 0.34425(15) 0.0428(3) Uani 1 1 d .
H17A H 0.6553 0.4504 0.2728 0.064 Uiso 1 1 calc R
H17B H 0.5147 0.3397 0.3601 0.064 Uiso 1 1 calc R
H17C H 0.6269 0.4218 0.4178 0.064 Uiso 1 1 calc R
O1 O 0.21262(14) 1.32547(10) 0.21044(8) 0.0410(3) Uani 1 1 d .
O2 O 0.18796(14) 1.50899(11) 0.03479(8) 0.0438(3) Uani 1 1 d .
H2A H 0.1358 1.5405 0.0834 0.066 Uiso 1 1 calc .
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 0.0477(8) 0.0249(6) 0.0334(7) -0.0122(5) -0.0008(6) 0.0021(5)
C2 0.0502(8) 0.0344(7) 0.0313(7) -0.0175(6) -0.0033(6) 0.0112(6)
C3 0.0442(7) 0.0363(7) 0.0233(6) -0.0100(5) 0.0013(5) 0.0111(6)
C4 0.0339(6) 0.0266(6) 0.0232(6) -0.0062(5) -0.0015(5) 0.0071(5)
C5 0.0253(6) 0.0242(6) 0.0220(6) -0.0072(5) -0.0038(4) 0.0034(4)
C6 0.0213(5) 0.0240(6) 0.0218(5) -0.0069(5) -0.0025(4) 0.0016(4)
C7 0.0226(5) 0.0246(6) 0.0221(5) -0.0074(4) -0.0015(4) 0.0013(4)
C8 0.0240(5) 0.0243(6) 0.0222(5) -0.0073(5) -0.0025(4) 0.0029(4)
N1 0.0373(6) 0.0244(5) 0.0267(5) -0.0090(4) 0.0000(4) 0.0005(4)
N2 0.0268(5) 0.0232(5) 0.0208(5) -0.0064(4) -0.0012(4) 0.0026(4)
N3 0.0309(5) 0.0235(5) 0.0211(5) -0.0065(4) -0.0019(4) 0.0034(4)
N4 0.0263(5) 0.0230(5) 0.0203(5) -0.0059(4) -0.0008(4) 0.0026(4)
N5 0.0365(6) 0.0214(5) 0.0212(5) -0.0059(4) 0.0002(4) 0.0041(4)
N6 0.0458(6) 0.0246(5) 0.0193(5) -0.0058(4) 0.0004(4) 0.0074(4)
C9 0.0340(6) 0.0283(6) 0.0278(6) -0.0121(5) -0.0003(5) -0.0010(5)
C10 0.0400(7) 0.0348(7) 0.0313(6) -0.0149(5) 0.0051(5) -0.0006(6)
C11 0.0317(6) 0.0396(7) 0.0406(7) -0.0207(6) 0.0025(5) 0.0029(5)
C12 0.0325(6) 0.0371(7) 0.0349(7) -0.0190(6) -0.0034(5) 0.0048(5)
C13 0.0299(6) 0.0381(7) 0.0375(7) -0.0199(6) -0.0037(5) 0.0050(5)
C14 0.0303(6) 0.0389(7) 0.0389(7) -0.0192(6) -0.0039(5) 0.0031(5)
C15 0.0290(6) 0.0361(7) 0.0342(7) -0.0171(6) -0.0023(5) 0.0018(5)
C16 0.0323(7) 0.0368(7) 0.0432(7) -0.0183(6) -0.0011(5) 0.0001(5)
C17 0.0410(8) 0.0351(7) 0.0505(8) -0.0147(6) -0.0025(6) 0.0030(6)
O1 0.0593(6) 0.0300(5) 0.0286(5) -0.0084(4) 0.0076(4) 0.0088(4)
O2 0.0613(6) 0.0394(6) 0.0267(5) -0.0097(4) 0.0008(4) 0.0186(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
N1 C1 C2 123.89(12) y
N1 C1 H1 118.1 ?
C2 C1 H1 118.1 ?
C3 C2 C1 118.39(12) y
C3 C2 H2 120.8 ?
C1 C2 H2 120.8 ?
C2 C3 C4 118.83(11) y
C2 C3 H3 120.6 ?
C4 C3 H3 120.6 ?
C3 C4 C5 118.81(11) y
C3 C4 H4 120.6 ?
C5 C4 H4 120.6 ?
N1 C5 C4 122.88(11) y
N1 C5 C6 116.35(10) y
C4 C5 C6 120.75(11) y
N4 C6 N2 126.55(10) y
N4 C6 C5 116.87(10) y
N2 C6 C5 116.57(10) y
N5 C7 N3 117.28(10) y
N5 C7 N2 118.47(10) y
N3 C7 N2 124.24(10) y
N6 C8 N3 117.88(10) y
N6 C8 N4 117.59(10) y
N3 C8 N4 124.53(10) y
C1 N1 C5 117.19(11) y
C6 N2 C7 114.59(9) y
C8 N3 C7 115.62(10) y
C6 N4 C8 114.38(10) y
C7 N5 H5A 120 ?
C7 N5 H5B 120 ?
H5A N5 H5B 120 ?
C8 N6 H6A 120 ?
C8 N6 H6B 120 ?
H6A N6 H6B 120 ?
O1 C9 O2 122.92(11) y
O1 C9 C10 124.38(12) y
O2 C9 C10 112.69(11) y
C9 C10 C11 114.72(11) y
C9 C10 H10A 108.6 ?
C11 C10 H10A 108.6 ?
C9 C10 H10B 108.6 ?
C11 C10 H10B 108.6 ?
H10A C10 H10B 107.6 ?
C12 C11 C10 114.41(11) y
C12 C11 H11A 108.7 ?
C10 C11 H11A 108.7 ?
C12 C11 H11B 108.7 ?
C10 C11 H11B 108.7 ?
H11A C11 H11B 107.6 ?
C11 C12 C13 112.08(11) y
C11 C12 H12A 109.2 ?
C13 C12 H12A 109.2 ?
C11 C12 H12B 109.2 ?
C13 C12 H12B 109.2 ?
H12A C12 H12B 107.9 ?
C14 C13 C12 114.01(11) y
C14 C13 H13A 108.7 ?
C12 C13 H13A 108.7 ?
C14 C13 H13B 108.7 ?
C12 C13 H13B 108.7 ?
H13A C13 H13B 107.6 ?
C13 C14 C15 113.53(11) y
C13 C14 H14A 108.9 ?
C15 C14 H14A 108.9 ?
C13 C14 H14B 108.9 ?
C15 C14 H14B 108.9 ?
H14A C14 H14B 107.7 ?
C16 C15 C14 113.63(11) y
C16 C15 H15A 108.8 ?
C14 C15 H15A 108.8 ?
C16 C15 H15B 108.8 ?
C14 C15 H15B 108.8 ?
H15A C15 H15B 107.7 ?
C17 C16 C15 113.27(11) y
C17 C16 H16A 108.9 ?
C15 C16 H16A 108.9 ?
C17 C16 H16B 108.9 ?
C15 C16 H16B 108.9 ?
H16A C16 H16B 107.7 ?
C16 C17 H17A 109.5 ?
C16 C17 H17B 109.5 ?
H17A C17 H17B 109.5 ?
C16 C17 H17C 109.5 ?
H17A C17 H17C 109.5 ?
H17B C17 H17C 109.5 ?
C9 O2 H2A 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.3343(17) y
C1 C2 1.3860(19) y
C1 H1 0.95 ?
C2 C3 1.378(2) y
C2 H2 0.95 ?
C3 C4 1.3856(18) y
C3 H3 0.95 ?
C4 C5 1.3901(17) y
C4 H4 0.95 ?
C5 N1 1.3407(16) y
C5 C6 1.4960(16) y
C6 N4 1.3308(15) y
C6 N2 1.3375(15) y
C7 N5 1.3321(15) y
C7 N3 1.3471(15) y
C7 N2 1.3543(15) y
C8 N6 1.3292(15) y
C8 N3 1.3445(15) y
C8 N4 1.3571(15) y
N5 H5A 0.88 ?
N5 H5B 0.88 ?
N6 H6A 0.88 ?
N6 H6B 0.88 ?
C9 O1 1.2097(15) y
C9 O2 1.3198(16) y
C9 C10 1.5018(18) y
C10 C11 1.5237(19) y
C10 H10A 0.99 ?
C10 H10B 0.99 ?
C11 C12 1.5206(19) y
C11 H11A 0.99 ?
C11 H11B 0.99 ?
C12 C13 1.5259(18) y
C12 H12A 0.99 ?
C12 H12B 0.99 ?
C13 C14 1.5204(19) y
C13 H13A 0.99 ?
C13 H13B 0.99 ?
C14 C15 1.5239(18) y
C14 H14A 0.99 ?
C14 H14B 0.99 ?
C15 C16 1.5232(18) y
C15 H15A 0.99 ?
C15 H15B 0.99 ?
C16 C17 1.520(2) y
C16 H16A 0.99 ?
C16 H16B 0.99 ?
C17 H17A 0.98 ?
C17 H17B 0.98 ?
C17 H17C 0.98 ?
O2 H2A 0.84 ?
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
N5 H5B N2 0.88 2.23 3.0700(14) 159.9 2_586
N5 H5A O1 0.88 2.13 2.9445(13) 154 .
N6 H6B N4 0.88 2.12 2.9954(15) 175.6 2_595
O2 H2A N3 0.84 1.86 2.6909(14) 171 .
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_publ_flag
N1 C1 C2 C3 -0.3(2) y
C1 C2 C3 C4 0.2(2) y
C2 C3 C4 C5 0.4(2) y
C3 C4 C5 N1 -1.05(18) y
C3 C4 C5 C6 -179.16(11) y
N1 C5 C6 N4 -18.16(15) y
C4 C5 C6 N4 160.07(11) y
N1 C5 C6 N2 162.35(10) y
C4 C5 C6 N2 -19.42(16) y
C2 C1 N1 C5 -0.3(2) y
C4 C5 N1 C1 0.99(18) y
C6 C5 N1 C1 179.18(10) y
N4 C6 N2 C7 -2.15(17) y
C5 C6 N2 C7 177.28(9) y
N5 C7 N2 C6 -179.03(10) y
N3 C7 N2 C6 0.63(16) y
N6 C8 N3 C7 177.48(10) y
N4 C8 N3 C7 -3.10(17) y
N5 C7 N3 C8 -178.55(10) y
N2 C7 N3 C8 1.78(17) y
N2 C6 N4 C8 1.02(16) y
C5 C6 N4 C8 -178.41(9) y
N6 C8 N4 C6 -178.77(10) y
N3 C8 N4 C6 1.80(16) y
O1 C9 C10 C11 -11.18(19) y
O2 C9 C10 C11 167.97(11) y
C9 C10 C11 C12 81.80(14) y
C10 C11 C12 C13 178.45(11) y
C11 C12 C13 C14 -173.89(11) y
C12 C13 C14 C15 169.79(11) y
C13 C14 C15 C16 -176.36(11) y
C14 C15 C16 C17 170.11(12) y
|
1501547.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501547.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_1501547
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C14 H12 N6, 2(C7 H14 O2)'
_chemical_formula_sum 'C28 H40 N6 O4'
_chemical_formula_weight 524.66
_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
_cell_angle_beta 95.126(4)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 50.606(4)
_cell_length_b 7.9595(7)
_cell_length_c 14.0826(12)
_cell_measurement_reflns_used 2925
_cell_measurement_temperature 150
_cell_measurement_theta_max 53.11
_cell_measurement_theta_min 5.63
_cell_volume 5649.8(8)
_computing_cell_refinement 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.108
_diffrn_reflns_av_sigmaI/netI 0.0769
_diffrn_reflns_limit_h_max 42
_diffrn_reflns_limit_h_min -60
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 37062
_diffrn_reflns_theta_full 67.65
_diffrn_reflns_theta_max 67.65
_diffrn_reflns_theta_min 5.63
_exptl_absorpt_coefficient_mu 0.679
_exptl_absorpt_correction_T_max 0.9601
_exptl_absorpt_correction_T_min 0.8925
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.234
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2256
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.223
_refine_diff_density_min -0.238
_refine_diff_density_rms 0.046
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 345
_refine_ls_number_reflns 5020
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.006
_refine_ls_R_factor_all 0.1332
_refine_ls_R_factor_gt 0.0597
_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^)+(0.0825P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1367
_refine_ls_wR_factor_ref 0.1703
_reflns_number_gt 2591
_reflns_number_total 5020
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam20
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501547
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
C1 C 0.08760(6) 0.6807(4) 0.2569(2) 0.0568(8) Uani 1 1 d .
H1 H 0.0880 0.6953 0.1901 0.068 Uiso 1 1 calc R
C2 C 0.06777(6) 0.5837(4) 0.2889(2) 0.0545(8) Uani 1 1 d .
H2 H 0.0550 0.5324 0.2444 0.065 Uiso 1 1 calc R
C3 C 0.06627(6) 0.5603(3) 0.38598(19) 0.0462(7) Uani 1 1 d .
C4 C 0.08578(6) 0.6393(4) 0.4456(2) 0.0544(8) Uani 1 1 d .
H4 H 0.0858 0.6281 0.5128 0.065 Uiso 1 1 calc R
C5 C 0.10506(6) 0.7336(4) 0.4080(2) 0.0571(8) Uani 1 1 d .
H5 H 0.1181 0.7859 0.4507 0.068 Uiso 1 1 calc R
C6 C 0.04504(6) 0.4570(3) 0.42351(19) 0.0451(7) Uani 1 1 d .
C7 C 0.02205(6) 0.4161(4) 0.3672(2) 0.0514(8) Uani 1 1 d .
H7 H 0.0199 0.4541 0.3031 0.062 Uiso 1 1 calc R
C8 C 0.00220(6) 0.3219(4) 0.4018(2) 0.0488(7) Uani 1 1 d .
H8 H -0.0132 0.2955 0.3611 0.059 Uiso 1 1 calc R
C9 C 0.00447(6) 0.2652(3) 0.49545(19) 0.0449(7) Uani 1 1 d .
C10 C 0.02714(6) 0.3071(4) 0.5526(2) 0.0499(8) Uani 1 1 d .
H10 H 0.0290 0.2709 0.6172 0.060 Uiso 1 1 calc R
C11 C 0.04707(6) 0.4005(4) 0.5175(2) 0.0506(8) Uani 1 1 d .
H11 H 0.0625 0.4269 0.5582 0.061 Uiso 1 1 calc R
C12 C -0.01715(6) 0.1637(3) 0.5322(2) 0.0430(7) Uani 1 1 d .
C13 C -0.05649(6) 0.0314(4) 0.5050(2) 0.0467(7) Uani 1 1 d .
C14 C -0.03475(6) 0.0298(3) 0.6535(2) 0.0452(7) Uani 1 1 d .
N1 N 0.10634(5) 0.7554(3) 0.31448(17) 0.0529(6) Uani 1 1 d .
N2 N -0.03760(5) 0.1263(3) 0.46955(16) 0.0476(6) Uani 1 1 d .
N3 N -0.05587(5) -0.0205(3) 0.59605(15) 0.0466(6) Uani 1 1 d .
N4 N -0.01435(4) 0.1200(3) 0.62441(15) 0.0449(6) Uani 1 1 d .
N5 N -0.07737(5) -0.0116(3) 0.44561(16) 0.0533(7) Uani 1 1 d .
H5A H -0.0902 -0.0722 0.4663 0.064 Uiso 1 1 calc .
H5B H -0.0783 0.0206 0.3856 0.064 Uiso 1 1 calc .
N6 N -0.03391(4) -0.0130(3) 0.74507(15) 0.0493(6) Uani 1 1 d .
H6A H -0.0469 -0.0721 0.7659 0.059 Uiso 1 1 calc .
H6B H -0.0204 0.0179 0.7848 0.059 Uiso 1 1 calc .
O1 O 0.14894(4) 0.8809(3) 0.24581(15) 0.0742(7) Uani 1 1 d .
H1A H 0.1340 0.8559 0.2629 0.111 Uiso 1 1 calc .
O2 O 0.12919(5) 0.8204(3) 0.10255(16) 0.0749(7) Uani 1 1 d .
C16 C 0.14863(7) 0.8657(4) 0.1521(2) 0.0581(8) Uani 1 1 d .
C17 C 0.17473(6) 0.9072(4) 0.1168(2) 0.0617(9) Uani 1 1 d .
H17A H 0.1882 0.8290 0.1470 0.074 Uiso 1 1 calc R
H17B H 0.1798 1.0220 0.1386 0.074 Uiso 1 1 calc R
C18 C 0.17607(6) 0.8997(4) 0.0101(2) 0.0593(8) Uani 1 1 d .
H18A H 0.1640 0.9851 -0.0209 0.071 Uiso 1 1 calc R
H18B H 0.1700 0.7878 -0.0136 0.071 Uiso 1 1 calc R
C19 C 0.20413(6) 0.9312(4) -0.0166(2) 0.0622(9) Uani 1 1 d .
H19A H 0.2099 1.0434 0.0075 0.075 Uiso 1 1 calc R
H19B H 0.2161 0.8472 0.0167 0.075 Uiso 1 1 calc R
C20 C 0.20784(6) 0.9236(4) -0.1225(2) 0.0637(9) Uani 1 1 d .
H20A H 0.2012 0.8142 -0.1483 0.076 Uiso 1 1 calc R
H20B H 0.1971 1.0133 -0.1560 0.076 Uiso 1 1 calc R
C21 C 0.23640(7) 0.9445(5) -0.1421(2) 0.0790(11) Uani 1 1 d .
H21A H 0.2471 0.8564 -0.1070 0.095 Uiso 1 1 calc R
H21B H 0.2428 1.0547 -0.1167 0.095 Uiso 1 1 calc R
C22 C 0.24140(7) 0.9349(6) -0.2466(2) 0.0923(13) Uani 1 1 d .
H22A H 0.2339 0.8303 -0.2740 0.138 Uiso 1 1 calc R
H22B H 0.2605 0.9371 -0.2525 0.138 Uiso 1 1 calc R
H22C H 0.2330 1.0310 -0.2807 0.138 Uiso 1 1 calc R
O3 O -0.08574(4) -0.1983(3) 0.77839(14) 0.0588(6) Uani 1 1 d .
O4 O -0.09886(4) -0.1876(3) 0.62360(14) 0.0646(6) Uani 1 1 d .
H4A H -0.0837 -0.1454 0.6209 0.097 Uiso 1 1 calc .
C23 C -0.10237(7) -0.2244(4) 0.7123(2) 0.0531(8) Uani 1 1 d .
C24 C -0.12914(6) -0.3009(4) 0.7231(2) 0.0569(8) Uani 1 1 d .
H24A H -0.1306 -0.4081 0.6874 0.068 Uiso 1 1 calc R
H24B H -0.1431 -0.2244 0.6942 0.068 Uiso 1 1 calc R
C25 C -0.13421(6) -0.3341(4) 0.8263(2) 0.0584(8) Uani 1 1 d .
H25A H -0.1305 -0.2303 0.8638 0.070 Uiso 1 1 calc R
H25B H -0.1218 -0.4219 0.8526 0.070 Uiso 1 1 calc R
C26 C -0.16249(6) -0.3904(4) 0.8378(2) 0.0610(9) Uani 1 1 d .
H26A H -0.1654 -0.5022 0.8078 0.073 Uiso 1 1 calc R
H26B H -0.1750 -0.3105 0.8038 0.073 Uiso 1 1 calc R
C27 C -0.16845(6) -0.4007(4) 0.9418(2) 0.0630(9) Uani 1 1 d .
H27A H -0.1571 -0.4885 0.9740 0.076 Uiso 1 1 calc R
H27B H -0.1637 -0.2922 0.9732 0.076 Uiso 1 1 calc R
C28 C -0.19702(6) -0.4397(4) 0.9558(2) 0.0691(10) Uani 1 1 d .
H28A H -0.2016 -0.5511 0.9278 0.083 Uiso 1 1 calc R
H28B H -0.2086 -0.3551 0.9212 0.083 Uiso 1 1 calc R
C29 C -0.20260(8) -0.4403(5) 1.0606(2) 0.0869(12) Uani 1 1 d .
H29A H -0.1915 -0.5252 1.0950 0.130 Uiso 1 1 calc R
H29B H -0.2213 -0.4666 1.0655 0.130 Uiso 1 1 calc R
H29C H -0.1986 -0.3294 1.0884 0.130 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
C1 0.065(2) 0.065(2) 0.0410(18) 0.0075(16) 0.0083(16) -0.0063(18)
C2 0.065(2) 0.0589(19) 0.0404(18) 0.0010(14) 0.0091(15) -0.0043(16)
C3 0.0555(18) 0.0431(17) 0.0409(17) 0.0014(13) 0.0089(15) 0.0029(14)
C4 0.062(2) 0.061(2) 0.0408(17) 0.0008(15) 0.0074(15) -0.0053(17)
C5 0.059(2) 0.062(2) 0.051(2) -0.0028(16) 0.0102(16) -0.0057(17)
C6 0.0555(18) 0.0433(17) 0.0377(16) 0.0012(13) 0.0103(14) 0.0015(14)
C7 0.062(2) 0.0516(19) 0.0417(17) 0.0044(14) 0.0094(16) -0.0008(16)
C8 0.0555(18) 0.0534(18) 0.0379(16) -0.0026(14) 0.0058(14) -0.0032(15)
C9 0.0569(19) 0.0416(17) 0.0372(16) -0.0009(13) 0.0104(14) 0.0006(14)
C10 0.0611(19) 0.0528(18) 0.0368(16) 0.0029(14) 0.0095(15) -0.0050(16)
C11 0.0590(19) 0.0512(18) 0.0417(17) -0.0043(14) 0.0050(15) -0.0052(15)
C12 0.0528(18) 0.0382(16) 0.0389(17) -0.0025(13) 0.0090(14) 0.0012(14)
C13 0.0526(18) 0.0462(18) 0.0421(18) -0.0035(14) 0.0084(15) -0.0007(15)
C14 0.0524(18) 0.0416(17) 0.0425(18) -0.0019(14) 0.0093(15) 0.0008(15)
N1 0.0628(17) 0.0549(16) 0.0423(15) 0.0018(12) 0.0112(13) -0.0002(13)
N2 0.0565(15) 0.0471(14) 0.0400(14) 0.0002(11) 0.0093(12) -0.0029(12)
N3 0.0593(15) 0.0492(15) 0.0326(13) 0.0016(11) 0.0112(12) -0.0012(12)
N4 0.0563(15) 0.0446(14) 0.0351(14) 0.0008(11) 0.0111(11) -0.0003(12)
N5 0.0599(16) 0.0617(17) 0.0389(14) 0.0030(12) 0.0069(13) -0.0087(13)
N6 0.0589(15) 0.0569(16) 0.0333(13) 0.0031(11) 0.0110(11) -0.0064(12)
O1 0.0789(15) 0.0950(18) 0.0512(15) -0.0050(12) 0.0203(11) -0.0214(13)
O2 0.0646(15) 0.102(2) 0.0587(15) 0.0057(13) 0.0079(12) -0.0001(14)
C16 0.065(2) 0.054(2) 0.056(2) 0.0028(17) 0.0097(18) -0.0008(17)
C17 0.065(2) 0.063(2) 0.059(2) -0.0031(17) 0.0145(17) -0.0039(17)
C18 0.066(2) 0.062(2) 0.051(2) 0.0019(16) 0.0115(16) -0.0006(17)
C19 0.071(2) 0.064(2) 0.052(2) 0.0030(16) 0.0121(17) -0.0034(17)
C20 0.069(2) 0.075(2) 0.048(2) 0.0047(16) 0.0109(16) -0.0005(18)
C21 0.073(2) 0.103(3) 0.062(2) 0.004(2) 0.0157(19) -0.003(2)
C22 0.083(3) 0.137(4) 0.060(2) 0.005(2) 0.022(2) 0.003(2)
O3 0.0674(14) 0.0673(15) 0.0422(13) -0.0037(11) 0.0075(11) -0.0064(11)
O4 0.0728(14) 0.0766(16) 0.0449(13) 0.0074(11) 0.0084(10) -0.0178(12)
C23 0.068(2) 0.0487(19) 0.0430(19) -0.0014(15) 0.0085(17) 0.0010(16)
C24 0.063(2) 0.063(2) 0.0455(18) -0.0053(15) 0.0088(15) -0.0057(16)
C25 0.065(2) 0.063(2) 0.0487(19) 0.0002(15) 0.0133(16) -0.0061(17)
C26 0.070(2) 0.062(2) 0.052(2) 0.0015(16) 0.0107(16) -0.0044(17)
C27 0.070(2) 0.065(2) 0.055(2) 0.0055(16) 0.0131(17) -0.0063(17)
C28 0.074(2) 0.067(2) 0.069(2) 0.0032(18) 0.0191(18) -0.0044(18)
C29 0.105(3) 0.089(3) 0.072(3) 0.008(2) 0.036(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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
N1 C1 C2 123.6(3) y
N1 C1 H1 118.2 ?
C2 C1 H1 118.2 ?
C1 C2 C3 120.2(3) y
C1 C2 H2 119.9 ?
C3 C2 H2 119.9 ?
C4 C3 C2 115.9(3) y
C4 C3 C6 122.2(3) y
C2 C3 C6 121.9(3) y
C5 C4 C3 120.4(3) y
C5 C4 H4 119.8 ?
C3 C4 H4 119.8 ?
N1 C5 C4 123.3(3) y
N1 C5 H5 118.3 ?
C4 C5 H5 118.3 ?
C7 C6 C11 117.0(3) y
C7 C6 C3 121.5(3) y
C11 C6 C3 121.5(3) y
C8 C7 C6 121.8(3) y
C8 C7 H7 119.1 ?
C6 C7 H7 119.1 ?
C7 C8 C9 120.8(3) y
C7 C8 H8 119.6 ?
C9 C8 H8 119.6 ?
C10 C9 C8 118.0(3) y
C10 C9 C12 121.7(3) y
C8 C9 C12 120.3(3) y
C11 C10 C9 121.1(3) y
C11 C10 H10 119.5 ?
C9 C10 H10 119.5 ?
C10 C11 C6 121.4(3) y
C10 C11 H11 119.3 ?
C6 C11 H11 119.3 ?
N2 C12 N4 126.4(2) y
N2 C12 C9 116.2(2) y
N4 C12 C9 117.4(3) y
N5 C13 N3 118.0(3) y
N5 C13 N2 117.3(3) y
N3 C13 N2 124.6(3) y
N6 C14 N3 117.5(2) y
N6 C14 N4 118.1(3) y
N3 C14 N4 124.4(3) y
C1 N1 C5 116.6(3) y
C12 N2 C13 114.4(2) y
C14 N3 C13 115.6(2) y
C12 N4 C14 114.5(2) y
C13 N5 H5A 120 ?
C13 N5 H5B 120 ?
H5A N5 H5B 120 ?
C14 N6 H6A 120 ?
C14 N6 H6B 120 ?
H6A N6 H6B 120 ?
C16 O1 H1A 109.5 ?
O2 C16 O1 122.6(3) y
O2 C16 C17 125.0(3) y
O1 C16 C17 112.4(3) y
C16 C17 C18 116.3(3) y
C16 C17 H17A 108.2 ?
C18 C17 H17A 108.2 ?
C16 C17 H17B 108.2 ?
C18 C17 H17B 108.2 ?
H17A C17 H17B 107.4 ?
C17 C18 C19 111.4(3) y
C17 C18 H18A 109.3 ?
C19 C18 H18A 109.3 ?
C17 C18 H18B 109.3 ?
C19 C18 H18B 109.3 ?
H18A C18 H18B 108 ?
C20 C19 C18 115.9(3) y
C20 C19 H19A 108.3 ?
C18 C19 H19A 108.3 ?
C20 C19 H19B 108.3 ?
C18 C19 H19B 108.3 ?
H19A C19 H19B 107.4 ?
C21 C20 C19 112.4(3) y
C21 C20 H20A 109.1 ?
C19 C20 H20A 109.1 ?
C21 C20 H20B 109.1 ?
C19 C20 H20B 109.1 ?
H20A C20 H20B 107.9 ?
C20 C21 C22 114.7(3) y
C20 C21 H21A 108.6 ?
C22 C21 H21A 108.6 ?
C20 C21 H21B 108.6 ?
C22 C21 H21B 108.6 ?
H21A C21 H21B 107.6 ?
C21 C22 H22A 109.5 ?
C21 C22 H22B 109.5 ?
H22A C22 H22B 109.5 ?
C21 C22 H22C 109.5 ?
H22A C22 H22C 109.5 ?
H22B C22 H22C 109.5 ?
C23 O4 H4A 109.5 ?
O3 C23 O4 123.3(3) y
O3 C23 C24 124.1(3) y
O4 C23 C24 112.7(3) y
C23 C24 C25 113.4(2) y
C23 C24 H24A 108.9 ?
C25 C24 H24A 108.9 ?
C23 C24 H24B 108.9 ?
C25 C24 H24B 108.9 ?
H24A C24 H24B 107.7 ?
C24 C25 C26 113.2(2) y
C24 C25 H25A 108.9 ?
C26 C25 H25A 108.9 ?
C24 C25 H25B 108.9 ?
C26 C25 H25B 108.9 ?
H25A C25 H25B 107.8 ?
C25 C26 C27 112.8(3) y
C25 C26 H26A 109 ?
C27 C26 H26A 109 ?
C25 C26 H26B 109 ?
C27 C26 H26B 109 ?
H26A C26 H26B 107.8 ?
C28 C27 C26 114.3(3) y
C28 C27 H27A 108.7 ?
C26 C27 H27A 108.7 ?
C28 C27 H27B 108.7 ?
C26 C27 H27B 108.7 ?
H27A C27 H27B 107.6 ?
C27 C28 C29 112.9(3) y
C27 C28 H28A 109 ?
C29 C28 H28A 109 ?
C27 C28 H28B 109 ?
C29 C28 H28B 109 ?
H28A C28 H28B 107.8 ?
C28 C29 H29A 109.5 ?
C28 C29 H29B 109.5 ?
H29A C29 H29B 109.5 ?
C28 C29 H29C 109.5 ?
H29A C29 H29C 109.5 ?
H29B C29 H29C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.331(4) y
C1 C2 1.374(4) y
C1 H1 0.95 ?
C2 C3 1.389(4) y
C2 H2 0.95 ?
C3 C4 1.388(4) y
C3 C6 1.487(4) y
C4 C5 1.374(4) y
C4 H4 0.95 ?
C5 N1 1.336(3) y
C5 H5 0.95 ?
C6 C7 1.386(4) y
C6 C11 1.393(4) y
C7 C8 1.377(4) y
C7 H7 0.95 ?
C8 C9 1.389(4) y
C8 H8 0.95 ?
C9 C10 1.382(4) y
C9 C12 1.490(4) y
C10 C11 1.380(4) y
C10 H10 0.95 ?
C11 H11 0.95 ?
C12 N2 1.333(3) y
C12 N4 1.339(3) y
C13 N5 1.332(3) y
C13 N3 1.344(3) y
C13 N2 1.349(3) y
C14 N6 1.331(3) y
C14 N3 1.342(3) y
C14 N4 1.350(3) y
N5 H5A 0.88 ?
N5 H5B 0.88 ?
N6 H6A 0.88 ?
N6 H6B 0.88 ?
O1 C16 1.324(4) y
O1 H1A 0.84 ?
O2 C16 1.209(4) y
C16 C17 1.489(4) y
C17 C18 1.511(4) y
C17 H17A 0.99 ?
C17 H17B 0.99 ?
C18 C19 1.522(4) y
C18 H18A 0.99 ?
C18 H18B 0.99 ?
C19 C20 1.521(4) y
C19 H19A 0.99 ?
C19 H19B 0.99 ?
C20 C21 1.505(4) y
C20 H20A 0.99 ?
C20 H20B 0.99 ?
C21 C22 1.516(4) y
C21 H21A 0.99 ?
C21 H21B 0.99 ?
C22 H22A 0.98 ?
C22 H22B 0.98 ?
C22 H22C 0.98 ?
O3 C23 1.215(3) y
O4 C23 1.311(3) y
O4 H4A 0.84 ?
C23 C24 1.505(4) y
C24 C25 1.522(4) y
C24 H24A 0.99 ?
C24 H24B 0.99 ?
C25 C26 1.522(4) y
C25 H25A 0.99 ?
C25 H25B 0.99 ?
C26 C27 1.524(4) y
C26 H26A 0.99 ?
C26 H26B 0.99 ?
C27 C28 1.509(4) y
C27 H27A 0.99 ?
C27 H27B 0.99 ?
C28 C29 1.526(4) y
C28 H28A 0.99 ?
C28 H28B 0.99 ?
C29 H29A 0.98 ?
C29 H29B 0.98 ?
C29 H29C 0.98 ?
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
N5 H5A O2 0.88 2.28 2.968(3) 134.4 2_545
N5 H5A O4 0.88 2.47 3.149(3) 134.1 .
N5 H5B O3 0.88 2.08 2.887(3) 152.4 6
N6 H6A O3 0.88 2.23 3.082(3) 163.3 .
N6 H6B N4 0.88 2.23 3.108(3) 173.9 2_556
O1 H1A N1 0.84 1.82 2.637(3) 164.9 .
O4 H4A N3 0.84 1.79 2.608(3) 166 .
|
1501548.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501548.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_1501548
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety '2(C8 H16 O2), C8 H8 N6'
_chemical_formula_sum 'C24 H40 N6 O4'
_chemical_formula_weight 476.62
_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 83.881(7)
_cell_angle_beta 84.671(7)
_cell_angle_gamma 79.308(7)
_cell_formula_units_Z 1
_cell_length_a 4.8615(6)
_cell_length_b 7.4585(9)
_cell_length_c 19.034(3)
_cell_measurement_reflns_used 1616
_cell_measurement_temperature 150
_cell_measurement_theta_max 63.55
_cell_measurement_theta_min 2.34
_cell_volume 672.43(16)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.065
_diffrn_reflns_av_sigmaI/netI 0.0659
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 9662
_diffrn_reflns_theta_full 69.16
_diffrn_reflns_theta_max 69.16
_diffrn_reflns_theta_min 2.34
_exptl_absorpt_coefficient_mu 0.660
_exptl_absorpt_correction_T_max 0.9804
_exptl_absorpt_correction_T_min 0.6536
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.177
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 258
_exptl_crystal_size_max 0.06
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.185
_refine_diff_density_min -0.340
_refine_diff_density_rms 0.047
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 200
_refine_ls_number_reflns 2369
_refine_ls_number_restraints 53
_refine_ls_restrained_S_all 1.006
_refine_ls_R_factor_all 0.1355
_refine_ls_R_factor_gt 0.0632
_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^)+(0.1058P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1587
_refine_ls_wR_factor_ref 0.1975
_reflns_number_gt 1208
_reflns_number_total 2369
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam53
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_cell_volume 672.44(15)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501548
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
O1 O -0.2678(6) -0.0724(4) 0.66146(14) 0.0814(9) Uani 1 1 d . . .
O2 O -0.3942(5) 0.2038(3) 0.70033(12) 0.0720(8) Uani 1 1 d . . .
H2 H -0.2674 0.2283 0.6697 0.050 Uiso 1 1 calc . . .
C1 C -0.4145(7) 0.0295(5) 0.70089(19) 0.0610(10) Uani 1 1 d . . .
C2 C -0.6297(7) -0.0256(4) 0.75631(18) 0.0619(10) Uani 1 1 d . . .
H2A H -0.8143 0.0503 0.7465 0.074 Uiso 1 1 calc R . .
H2B H -0.5819 0.0023 0.8029 0.074 Uiso 1 1 calc R . .
C3 C -0.6577(7) -0.2256(4) 0.76124(17) 0.0577(9) Uani 1 1 d . . .
H3A H -0.7229 -0.2516 0.7162 0.069 Uiso 1 1 calc R . .
H3B H -0.4706 -0.3024 0.7672 0.069 Uiso 1 1 calc R . .
C4 C -0.8599(7) -0.2787(4) 0.82197(17) 0.0567(9) Uani 1 1 d . . .
H4A H -1.0469 -0.2020 0.8158 0.068 Uiso 1 1 calc R . .
H4B H -0.7951 -0.2518 0.8669 0.068 Uiso 1 1 calc R . .
C5 C -0.8893(7) -0.4801(4) 0.82785(16) 0.0569(9) Uani 1 1 d . . .
H5A H -0.9632 -0.5054 0.7839 0.068 Uiso 1 1 calc R . .
H5B H -0.7008 -0.5567 0.8314 0.068 Uiso 1 1 calc R . .
C6 C -1.0798(7) -0.5364(4) 0.89049(16) 0.0573(9) Uani 1 1 d . . .
H6A H -1.2666 -0.4572 0.8877 0.069 Uiso 1 1 calc R . .
H6B H -1.0025 -0.5149 0.9346 0.069 Uiso 1 1 calc R . .
C7 C -1.1160(7) -0.7351(4) 0.89501(19) 0.0658(10) Uani 1 1 d . . .
H7A H -1.1967 -0.7561 0.8513 0.079 Uiso 1 1 calc R . .
H7B H -0.9289 -0.8143 0.8969 0.079 Uiso 1 1 calc R . .
C8 C -1.3029(9) -0.7920(6) 0.9586(2) 0.0876(13) Uani 1 1 d . . .
H8A H -1.2173 -0.7810 1.0022 0.131 Uiso 1 1 calc R . .
H8B H -1.3246 -0.9194 0.9568 0.131 Uiso 1 1 calc R . .
H8C H -1.4874 -0.7125 0.9579 0.131 Uiso 1 1 calc R . .
N1 N 0.8302(12) 0.9737(6) 0.4449(3) 0.0652(16) Uani 0.50 1 d P A -1
H1A H 0.9638 1.0259 0.4216 0.078 Uiso 0.50 1 calc P B -1
H1B H 0.7029 1.0365 0.4731 0.078 Uiso 0.50 1 calc P C -1
N2 N 1.1532(10) 0.4268(6) 0.3527(3) 0.0478(13) Uani 0.50 1 d P A -1
H2C H 1.2729 0.4833 0.3254 0.057 Uiso 0.50 1 calc P D -1
H2D H 1.1531 0.3100 0.3494 0.057 Uiso 0.50 1 calc P E -1
N3 N 1.008(3) 0.6892(16) 0.3952(8) 0.043(2) Uani 0.50 1 d PDU A -1
C17 C 0.820(3) 0.7870(13) 0.4370(7) 0.053(4) Uani 0.50 1 d PDU A -1
N4 N 0.613(3) 0.7305(15) 0.4794(8) 0.049(2) Uani 0.50 1 d PDU A -1
C18 C 0.608(4) 0.5529(16) 0.4769(10) 0.0404(9) Uani 0.50 1 d PDU A -1
N5 N 0.781(3) 0.4392(13) 0.4369(7) 0.044(2) Uani 0.50 1 d PDU A -1
C19 C 0.976(3) 0.5161(16) 0.3979(6) 0.036(3) Uani 0.50 1 d PDU A -1
C20 C 0.397(4) 0.4672(18) 0.5250(9) 0.0404(9) Uani 0.50 1 d PGU A -1
C21 C 0.237(3) 0.5605(15) 0.5785(8) 0.044(3) Uani 0.50 1 d PGU A -1
H21 H 0.2594 0.6814 0.5850 0.053 Uiso 0.50 1 calc PR A -1
C22 C 0.044(3) 0.4769(17) 0.6226(6) 0.045(3) Uani 0.50 1 d PGU A -1
H22 H -0.0657 0.5407 0.6592 0.054 Uiso 0.50 1 calc PR A -1
N6 N 0.011(3) 0.3001(17) 0.6131(7) 0.054(4) Uani 0.50 1 d PGU A -1
C23 C 0.171(2) 0.2068(14) 0.5596(8) 0.051(3) Uani 0.50 1 d PGU A -1
H23 H 0.1490 0.0859 0.5531 0.061 Uiso 0.50 1 calc PR A -1
C24 C 0.364(3) 0.2904(16) 0.5155(8) 0.048(3) Uani 0.50 1 d PGU A -1
H24 H 0.4740 0.2266 0.4789 0.058 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
O1 0.0770(18) 0.0713(18) 0.0895(19) 0.0128(14) 0.0250(15) -0.0236(14)
O2 0.0658(16) 0.0658(17) 0.0836(17) 0.0150(12) 0.0102(13) -0.0296(12)
C1 0.045(2) 0.068(2) 0.067(2) 0.0189(18) -0.0024(17) -0.0187(18)
C2 0.050(2) 0.062(2) 0.070(2) 0.0145(17) 0.0040(17) -0.0179(16)
C3 0.052(2) 0.061(2) 0.058(2) 0.0096(16) 0.0032(16) -0.0186(16)
C4 0.052(2) 0.054(2) 0.061(2) 0.0094(15) 0.0066(16) -0.0152(15)
C5 0.054(2) 0.058(2) 0.058(2) 0.0066(15) 0.0050(16) -0.0185(16)
C6 0.056(2) 0.057(2) 0.056(2) 0.0084(15) 0.0038(16) -0.0156(16)
C7 0.063(2) 0.057(2) 0.076(2) 0.0109(17) 0.0024(18) -0.0230(17)
C8 0.092(3) 0.082(3) 0.088(3) 0.020(2) 0.009(2) -0.039(2)
N1 0.065(4) 0.032(3) 0.094(4) 0.002(3) 0.026(3) -0.015(3)
N2 0.048(3) 0.038(3) 0.056(3) 0.001(2) 0.009(3) -0.014(2)
N3 0.037(5) 0.037(4) 0.054(5) 0.016(4) -0.014(3) -0.007(3)
C17 0.090(10) 0.035(4) 0.035(6) 0.011(5) 0.008(6) -0.023(5)
N4 0.053(6) 0.032(2) 0.058(6) 0.012(3) -0.002(4) -0.010(3)
C18 0.0373(17) 0.0343(19) 0.0488(19) 0.0079(17) -0.0049(13) -0.0098(16)
N5 0.047(4) 0.036(3) 0.045(5) 0.011(2) -0.001(3) -0.008(2)
C19 0.037(3) 0.038(4) 0.032(6) 0.012(3) -0.012(3) -0.006(3)
C20 0.0373(17) 0.0343(19) 0.0488(19) 0.0079(17) -0.0049(13) -0.0098(16)
C21 0.041(5) 0.037(3) 0.053(7) 0.007(3) 0.000(4) -0.013(3)
C22 0.046(4) 0.044(4) 0.041(7) 0.023(3) -0.006(5) -0.012(3)
N6 0.050(7) 0.048(5) 0.062(6) 0.022(4) -0.004(5) -0.022(5)
C23 0.027(6) 0.048(5) 0.083(9) 0.005(5) -0.013(4) -0.019(5)
C24 0.049(7) 0.035(4) 0.062(8) 0.006(4) -0.004(5) -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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
C1 O2 H2 109.5 ?
O1 C1 O2 122.6(3) y
O1 C1 C2 125.1(3) y
O2 C1 C2 112.3(3) y
C1 C2 C3 115.0(3) y
C1 C2 H2A 108.5 ?
C3 C2 H2A 108.5 ?
C1 C2 H2B 108.5 ?
C3 C2 H2B 108.5 ?
H2A C2 H2B 107.5 ?
C4 C3 C2 113.2(3) y
C4 C3 H3A 108.9 ?
C2 C3 H3A 108.9 ?
C4 C3 H3B 108.9 ?
C2 C3 H3B 108.9 ?
H3A C3 H3B 107.8 ?
C3 C4 C5 113.8(3) y
C3 C4 H4A 108.8 ?
C5 C4 H4A 108.8 ?
C3 C4 H4B 108.8 ?
C5 C4 H4B 108.8 ?
H4A C4 H4B 107.7 ?
C6 C5 C4 114.1(3) y
C6 C5 H5A 108.7 ?
C4 C5 H5A 108.7 ?
C6 C5 H5B 108.7 ?
C4 C5 H5B 108.7 ?
H5A C5 H5B 107.6 ?
C5 C6 C7 114.1(3) y
C5 C6 H6A 108.7 ?
C7 C6 H6A 108.7 ?
C5 C6 H6B 108.7 ?
C7 C6 H6B 108.7 ?
H6A C6 H6B 107.6 ?
C8 C7 C6 114.0(3) y
C8 C7 H7A 108.8 ?
C6 C7 H7A 108.8 ?
C8 C7 H7B 108.8 ?
C6 C7 H7B 108.8 ?
H7A C7 H7B 107.7 ?
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 ?
C17 N1 H1A 120.0 ?
C17 N1 H1B 120.0 ?
H1A N1 H1B 120.0 ?
C19 N2 H2C 120.0 ?
C19 N2 H2D 120.0 ?
H2C N2 H2D 120.0 ?
C17 N3 C19 113.0(5) y
N3 C17 N4 127.6(5) y
N3 C17 N1 121.4(7) y
N4 C17 N1 110.9(7) y
C17 N4 C18 112.6(5) y
N5 C18 N4 126.2(4) y
N5 C18 C20 115.1(4) y
N4 C18 C20 118.6(5) y
C18 N5 C19 113.9(5) y
N2 C19 N3 111.3(7) y
N2 C19 N5 121.9(8) y
N3 C19 N5 126.6(5) y
C21 C20 C24 120.0 y
C21 C20 C18 121.4(4) y
C24 C20 C18 118.6(4) y
C20 C21 C22 120.0 y
C20 C21 H21 120.0 ?
C22 C21 H21 120.0 ?
N6 C22 C21 120.0 y
N6 C22 H22 120.0 ?
C21 C22 H22 120.0 ?
C23 N6 C22 120.0 y
N6 C23 C24 120.0 y
N6 C23 H23 120.0 ?
C24 C23 H23 120.0 ?
C23 C24 C20 120.0 y
C23 C24 H24 120.0 ?
C20 C24 H24 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 1.213(4) y
O2 C1 1.321(4) y
O2 H2 0.8400 ?
C1 C2 1.496(4) y
C2 C3 1.515(4) y
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 C4 1.515(4) y
C3 H3A 0.9900 ?
C3 H3B 0.9900 ?
C4 C5 1.526(4) y
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C5 C6 1.513(4) y
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 C7 1.517(4) y
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
C7 C8 1.516(4) y
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 H8A 0.9800 ?
C8 H8B 0.9800 ?
C8 H8C 0.9800 ?
N1 C17 1.427(10) y
N1 H1A 0.8800 ?
N1 H1B 0.8800 ?
N2 C19 1.303(10) y
N2 H2C 0.8800 ?
N2 H2D 0.8800 ?
N3 C17 1.320(5) y
N3 C19 1.323(5) y
C17 N4 1.332(5) y
N4 C18 1.335(5) y
C18 N5 1.326(5) y
C18 C20 1.497(4) y
N5 C19 1.328(5) y
C20 C21 1.3900 y
C20 C24 1.3900 y
C21 C22 1.3900 y
C21 H21 0.9500 ?
C22 N6 1.3900 y
C22 H22 0.9500 ?
N6 C23 1.3900 y
C23 C24 1.3900 y
C23 H23 0.9500 ?
C24 H24 0.9500 ?
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 H2 N6 0.84 1.78 2.611(8) 172.2 .
O2 H2 N3 0.84 1.83 2.662(9) 173 2_666
N1 H1A O1 0.88 2.11 2.938(5) 156.9 2_666
N1 H1B N4 0.88 2.3 3.150(11) 162.9 2_676
N2 H2C O2 0.88 2.5 3.220(5) 139.5 2_666
N2 H2D O1 0.88 1.78 2.636(6) 162.1 2_656
|
1501549.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501549.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_1501549
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety '2(C9 H18 O2), C8 H8 N6'
_chemical_formula_sum 'C26 H44 N6 O4'
_chemical_formula_weight 504.67
_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 94.378(4)
_cell_angle_beta 92.854(4)
_cell_angle_gamma 101.374(3)
_cell_formula_units_Z 3
_cell_length_a 7.5805(6)
_cell_length_b 11.1838(9)
_cell_length_c 25.627(2)
_cell_measurement_reflns_used 3034
_cell_measurement_temperature 150
_cell_measurement_theta_max 56.75
_cell_measurement_theta_min 3.47
_cell_volume 2119.1(3)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.074
_diffrn_reflns_av_sigmaI/netI 0.0648
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 29039
_diffrn_reflns_theta_full 57.21
_diffrn_reflns_theta_max 57.21
_diffrn_reflns_theta_min 1.73
_exptl_absorpt_coefficient_mu 0.654
_exptl_absorpt_correction_T_max 0.9806
_exptl_absorpt_correction_T_min 0.7060
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.186
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 822
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.281
_refine_diff_density_min -0.313
_refine_diff_density_rms 0.048
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.008
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 616
_refine_ls_number_reflns 5617
_refine_ls_number_restraints 212
_refine_ls_restrained_S_all 0.996
_refine_ls_R_factor_all 0.1419
_refine_ls_R_factor_gt 0.0658
_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^)+(0.1046P)^2^+0.6469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1651
_refine_ls_wR_factor_ref 0.2141
_reflns_number_gt 2775
_reflns_number_total 5617
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam54
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_cell_volume 2119.0(3)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501549
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
O1 O 0.4825(4) 0.7197(3) 0.66103(11) 0.0615(8) Uani 1 1 d . . .
O2 O 0.7686(4) 0.7789(3) 0.69039(10) 0.0642(9) Uani 1 1 d . . .
H2 H 0.7844 0.7375 0.6629 0.096 Uiso 1 1 calc . . .
C1 C 0.5961(6) 0.7757(4) 0.69383(17) 0.0470(11) Uani 1 1 d . . .
C2 C 0.5535(5) 0.8467(4) 0.74176(14) 0.0462(11) Uani 1 1 d . . .
H2A H 0.6022 0.9347 0.7390 0.055 Uiso 1 1 calc R . .
H2B H 0.6170 0.8223 0.7727 0.055 Uiso 1 1 calc R . .
C3 C 0.3536(5) 0.8304(4) 0.75141(14) 0.0447(10) Uani 1 1 d . . .
H3A H 0.2906 0.8612 0.7221 0.054 Uiso 1 1 calc R . .
H3B H 0.3019 0.7421 0.7519 0.054 Uiso 1 1 calc R . .
C4 C 0.3204(5) 0.8973(3) 0.80269(14) 0.0428(10) Uani 1 1 d . . .
H4A H 0.3893 0.8697 0.8317 0.051 Uiso 1 1 calc R . .
H4B H 0.3670 0.9861 0.8013 0.051 Uiso 1 1 calc R . .
C5 C 0.1233(5) 0.8775(3) 0.81474(14) 0.0423(10) Uani 1 1 d . . .
H5A H 0.0768 0.7888 0.8166 0.051 Uiso 1 1 calc R . .
H5B H 0.0539 0.9042 0.7856 0.051 Uiso 1 1 calc R . .
C6 C 0.0914(5) 0.9462(3) 0.86590(14) 0.0432(10) Uani 1 1 d . . .
H6A H 0.1632 0.9206 0.8948 0.052 Uiso 1 1 calc R . .
H6B H 0.1365 1.0349 0.8637 0.052 Uiso 1 1 calc R . .
C7 C -0.1045(5) 0.9264(3) 0.87955(14) 0.0438(10) Uani 1 1 d . . .
H7A H -0.1763 0.9537 0.8511 0.053 Uiso 1 1 calc R . .
H7B H -0.1506 0.8376 0.8813 0.053 Uiso 1 1 calc R . .
C8 C -0.1321(5) 0.9935(4) 0.93086(15) 0.0559(12) Uani 1 1 d . . .
H8A H -0.0870 1.0822 0.9288 0.067 Uiso 1 1 calc R . .
H8B H -0.0583 0.9671 0.9591 0.067 Uiso 1 1 calc R . .
C9 C -0.3259(5) 0.9739(4) 0.94587(17) 0.0704(14) Uani 1 1 d . . .
H9A H -0.3994 1.0042 0.9193 0.106 Uiso 1 1 calc R . .
H9B H -0.3314 1.0184 0.9800 0.106 Uiso 1 1 calc R . .
H9C H -0.3724 0.8863 0.9480 0.106 Uiso 1 1 calc R . .
O3 O 0.6642(4) 0.4410(3) 0.70334(10) 0.0584(8) Uani 1 1 d . . .
O4 O 0.9514(3) 0.5116(3) 0.73105(11) 0.0599(8) Uani 1 1 d . . .
H4 H 0.9685 0.4729 0.7030 0.090 Uiso 1 1 calc . . .
C10 C 0.7768(6) 0.4989(4) 0.73635(17) 0.0458(10) Uani 1 1 d . . .
C11 C 0.7344(5) 0.5617(4) 0.78587(14) 0.0443(10) Uani 1 1 d . . .
H11A H 0.7792 0.6509 0.7852 0.053 Uiso 1 1 calc R . .
H11B H 0.8008 0.5344 0.8155 0.053 Uiso 1 1 calc R . .
C12 C 0.5355(5) 0.5393(3) 0.79608(14) 0.0426(10) Uani 1 1 d . . .
H12A H 0.4883 0.4499 0.7947 0.051 Uiso 1 1 calc R . .
H12B H 0.4696 0.5716 0.7678 0.051 Uiso 1 1 calc R . .
C13 C 0.4980(5) 0.5984(4) 0.84871(14) 0.0445(10) Uani 1 1 d . . .
H13A H 0.5663 0.5672 0.8768 0.053 Uiso 1 1 calc R . .
H13B H 0.5438 0.6879 0.8497 0.053 Uiso 1 1 calc R . .
C14 C 0.3007(5) 0.5756(3) 0.86031(14) 0.0420(10) Uani 1 1 d . . .
H14A H 0.2549 0.4863 0.8600 0.050 Uiso 1 1 calc R . .
H14B H 0.2317 0.6059 0.8321 0.050 Uiso 1 1 calc R . .
C15 C 0.2677(5) 0.6375(4) 0.91304(14) 0.0464(10) Uani 1 1 d . . .
H15A H 0.3368 0.6068 0.9411 0.056 Uiso 1 1 calc R . .
H15B H 0.3149 0.7267 0.9133 0.056 Uiso 1 1 calc R . .
C16 C 0.0708(5) 0.6170(4) 0.92573(14) 0.0461(10) Uani 1 1 d . . .
H16A H 0.0016 0.6482 0.8979 0.055 Uiso 1 1 calc R . .
H16B H 0.0232 0.5279 0.9254 0.055 Uiso 1 1 calc R . .
C17 C 0.0400(5) 0.6781(4) 0.97799(15) 0.0573(12) Uani 1 1 d . . .
H17A H 0.0878 0.7672 0.9783 0.069 Uiso 1 1 calc R . .
H17B H 0.1093 0.6469 1.0058 0.069 Uiso 1 1 calc R . .
C18 C -0.1570(6) 0.6580(4) 0.99095(17) 0.0701(13) Uani 1 1 d . . .
H18A H -0.2244 0.6972 0.9660 0.105 Uiso 1 1 calc R . .
H18B H -0.1653 0.6940 1.0266 0.105 Uiso 1 1 calc R . .
H18C H -0.2080 0.5700 0.9886 0.105 Uiso 1 1 calc R . .
O5 O 1.7076(4) 0.0015(3) 0.38383(11) 0.0594(8) Uani 1 1 d . . .
O6 O 1.4213(4) -0.0517(3) 0.35450(11) 0.0719(10) Uani 1 1 d . . .
H6 H 1.4084 -0.0067 0.3813 0.108 Uiso 1 1 calc . . .
C19 C 1.5932(6) -0.0547(4) 0.35141(16) 0.0502(11) Uani 1 1 d . . .
C20 C 1.6294(5) -0.1323(4) 0.30482(14) 0.0452(10) Uani 1 1 d . . .
H20A H 1.5678 -0.1093 0.2733 0.054 Uiso 1 1 calc R . .
H20B H 1.5765 -0.2189 0.3092 0.054 Uiso 1 1 calc R . .
C21 C 1.8291(5) -0.1211(3) 0.29581(14) 0.0425(10) Uani 1 1 d . . .
H21A H 1.8839 -0.0340 0.2932 0.051 Uiso 1 1 calc R . .
H21B H 1.8899 -0.1487 0.3264 0.051 Uiso 1 1 calc R . .
C22 C 1.8612(5) -0.1960(3) 0.24648(14) 0.0413(10) Uani 1 1 d . . .
H22A H 1.8119 -0.2835 0.2501 0.050 Uiso 1 1 calc R . .
H22B H 1.7937 -0.1718 0.2163 0.050 Uiso 1 1 calc R . .
C23 C 2.0578(5) -0.1814(3) 0.23463(14) 0.0428(10) Uani 1 1 d . . .
H23A H 2.1090 -0.0933 0.2331 0.051 Uiso 1 1 calc R . .
H23B H 2.1239 -0.2102 0.2639 0.051 Uiso 1 1 calc R . .
C24 C 2.0900(5) -0.2499(3) 0.18397(14) 0.0431(10) Uani 1 1 d . . .
H24A H 2.0183 -0.2245 0.1550 0.052 Uiso 1 1 calc R . .
H24B H 2.0445 -0.3385 0.1863 0.052 Uiso 1 1 calc R . .
C25 C 2.2849(5) -0.2309(4) 0.17022(14) 0.0440(10) Uani 1 1 d . . .
H25A H 2.3555 -0.2613 0.1980 0.053 Uiso 1 1 calc R . .
H25B H 2.3328 -0.1419 0.1699 0.053 Uiso 1 1 calc R . .
C26 C 2.3129(5) -0.2941(4) 0.11781(15) 0.0510(11) Uani 1 1 d . . .
H26A H 2.2695 -0.3833 0.1188 0.061 Uiso 1 1 calc R . .
H26B H 2.2375 -0.2665 0.0904 0.061 Uiso 1 1 calc R . .
C27 C 2.5052(4) -0.2718(3) 0.10221(12) 0.0633(13) Uani 1 1 d . . .
H27A H 2.5596 -0.3412 0.1104 0.095 Uiso 1 1 calc R . .
H27B H 2.5739 -0.1968 0.1216 0.095 Uiso 1 1 calc R . .
H27C H 2.5069 -0.2629 0.0645 0.095 Uiso 1 1 calc R . .
N7 N 1.0457(4) 0.3960(3) 0.65343(12) 0.038(2) Uani 0.50 1 d PRDU A 1
C36 C 1.2244(4) 0.4048(3) 0.64606(12) 0.0380(19) Uani 0.50 1 d PRDU A 1
H36 H 1.3087 0.4573 0.6705 0.046 Uiso 0.50 1 calc PR B 1
C37 C 1.2906(4) 0.3432(3) 0.60596(12) 0.0317(17) Uani 0.50 1 d PRDU A 1
H37 H 1.4164 0.3498 0.6028 0.038 Uiso 0.50 1 calc PR C 1
C38 C 1.1681(4) 0.2730(3) 0.57132(12) 0.0306(17) Uani 0.50 1 d PRDU A 1
C39 C 0.9844(4) 0.2609(3) 0.57330(12) 0.0317(17) Uani 0.50 1 d PRDU A 1
H39 H 0.9002 0.2131 0.5474 0.038 Uiso 0.50 1 calc PR D 1
C40 C 0.9335(4) 0.3250(3) 0.61648(12) 0.0380(19) Uani 0.50 1 d PRDU A 1
H40 H 0.8079 0.3179 0.6202 0.046 Uiso 0.50 1 calc PR E 1
C41 C 1.2349(4) 0.2066(3) 0.52628(12) 0.0306(17) Uani 0.50 1 d PRDU A 1
N8 N 1.1138(4) 0.1480(3) 0.48790(12) 0.0328(15) Uani 0.50 1 d PRDU A 1
C42 C 1.1833(4) 0.0892(3) 0.44626(12) 0.0363(18) Uani 0.50 1 d PRDU A 1
N9 N 1.3558(4) 0.0884(3) 0.44189(12) 0.035(2) Uani 0.50 1 d PRDU A 1
C43 C 1.4643(5) 0.1408(10) 0.4843(3) 0.0363(18) Uani 0.50 1 d PDU A 1
N10 N 1.4141(6) 0.2008(11) 0.5258(3) 0.0328(15) Uani 0.50 1 d PDU A 1
N11 N 1.0654(5) 0.0405(5) 0.40541(16) 0.0424(16) Uani 0.50 1 d PDU A 1
H11C H 1.1041 0.0091 0.3767 0.051 Uiso 0.50 1 calc P F 1
H11D H 0.9498 0.0401 0.4075 0.051 Uiso 0.50 1 calc P G 1
N12 N 1.6411(5) 0.1417(6) 0.47963(19) 0.0473(16) Uani 0.50 1 d PDU A 1
H12C H 1.7216 0.1819 0.5040 0.057 Uiso 0.50 1 calc P H 1
H12D H 1.6758 0.1022 0.4522 0.057 Uiso 0.50 1 calc P I 1
N7B N 1.3317(6) 0.0721(7) 0.4299(2) 0.042(2) Uani 0.50 1 d PDU J 2
C36B C 1.4446(6) 0.1403(11) 0.4690(3) 0.045(3) Uani 0.50 1 d PDU J 2
H36B H 1.5706 0.1461 0.4666 0.054 Uiso 0.50 1 calc PR J 2
C37B C 1.3888(5) 0.2007(14) 0.5114(4) 0.045(3) Uani 0.50 1 d PDU J 2
H37B H 1.4719 0.2472 0.5379 0.054 Uiso 0.50 1 calc PR J 2
C38B C 1.2105(5) 0.1907(7) 0.5136(2) 0.0314(19) Uani 0.50 1 d PDU J 2
C39B C 1.0840(5) 0.1284(7) 0.4756(2) 0.0333(19) Uani 0.50 1 d PDU J 2
H39B H 0.9582 0.1242 0.4776 0.040 Uiso 0.50 1 calc PR J 2
C40B C 1.1566(6) 0.0724(8) 0.4341(2) 0.040(2) Uani 0.50 1 d PDU J 2
H40B H 1.0750 0.0306 0.4063 0.049 Uiso 0.50 1 calc PR J 2
C41B C 1.1438(5) 0.2573(7) 0.5586(2) 0.0336(19) Uani 0.50 1 d PDU J 2
N8B N 1.2653(5) 0.3246(6) 0.5948(2) 0.0422(19) Uani 0.50 1 d PDU J 2
C42B C 1.1947(5) 0.3860(7) 0.6355(2) 0.040(2) Uani 0.50 1 d PDU J 2
N9B N 1.0214(5) 0.3791(7) 0.6417(2) 0.041(2) Uani 0.50 1 d PDU J 2
C43B C 0.9100(5) 0.3061(7) 0.6043(3) 0.045(2) Uani 0.50 1 d PDU J 2
N10B N 0.9616(6) 0.2472(7) 0.5627(2) 0.050(2) Uani 0.50 1 d PDU J 2
N11B N 1.3153(5) 0.4564(5) 0.67121(19) 0.0465(16) Uani 0.50 1 d PDU J 2
H11E H 1.2777 0.4965 0.6979 0.056 Uiso 0.50 1 calc P K 2
H11F H 1.4315 0.4623 0.6678 0.056 Uiso 0.50 1 calc P L 2
N12B N 0.7338(5) 0.3090(5) 0.60756(19) 0.0430(15) Uani 0.50 1 d PDU J 2
H12E H 0.6546 0.2720 0.5822 0.052 Uiso 0.50 1 calc P M 2
H12F H 0.6981 0.3478 0.6350 0.052 Uiso 0.50 1 calc P N 2
N1 N 0.8626(7) 0.6546(15) 0.6164(4) 0.038(2) Uani 0.50 1 d PDU O -1
C28 C 1.0404(7) 0.6691(19) 0.6068(5) 0.037(2) Uani 0.50 1 d PDU O -1
H28 H 1.1256 0.7206 0.6313 0.044 Uiso 0.50 1 calc PR O -1
C29 C 1.1040(7) 0.6147(14) 0.5642(4) 0.029(2) Uani 0.50 1 d PDU O -1
H29 H 1.2292 0.6274 0.5588 0.035 Uiso 0.50 1 calc PR O -1
C30 C 0.9806(7) 0.5424(15) 0.5304(4) 0.029(2) Uani 0.50 1 d PDU O -1
C31 C 0.7979(7) 0.5199(12) 0.5363(4) 0.035(3) Uani 0.50 1 d PDU O -1
H31 H 0.7131 0.4647 0.5129 0.042 Uiso 0.50 1 calc PR O -1
C32 C 0.7487(7) 0.5852(14) 0.5794(4) 0.043(3) Uani 0.50 1 d PDU O -1
H32 H 0.6234 0.5802 0.5830 0.051 Uiso 0.50 1 calc PR O -1
C33 C 1.0456(7) 0.4780(16) 0.4845(4) 0.029(2) Uani 0.50 1 d PDU O -1
N2 N 0.9228(6) 0.4144(14) 0.4476(4) 0.039(2) Uani 0.50 1 d PDU O -1
C34 C 0.9915(6) 0.3545(19) 0.4062(5) 0.034(2) Uani 0.50 1 d PDU O -1
N3 N 1.1641(6) 0.3560(13) 0.4007(3) 0.0298(19) Uani 0.50 1 d PDU O -1
C35 C 1.2763(6) 0.4211(13) 0.4399(3) 0.031(2) Uani 0.50 1 d PDU O -1
N4 N 1.2258(7) 0.4759(11) 0.4828(3) 0.036(3) Uani 0.50 1 d PDU O -1
N5 N 0.8707(6) 0.2957(6) 0.36769(18) 0.0427(17) Uani 0.50 1 d PDU O -1
H5C H 0.9076 0.2595 0.3398 0.051 Uiso 0.50 1 calc P P -1
H5D H 0.7549 0.2935 0.3705 0.051 Uiso 0.50 1 calc P Q -1
N6 N 1.4523(5) 0.4197(5) 0.43543(19) 0.0384(14) Uani 0.50 1 d PDU O -1
H6C H 1.5325 0.4549 0.4608 0.046 Uiso 0.50 1 calc P R -1
H6D H 1.4869 0.3836 0.4071 0.046 Uiso 0.50 1 calc P S -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
O1 0.0543(19) 0.077(2) 0.0563(19) -0.0068(16) 0.0071(16) 0.0236(17)
O2 0.0425(19) 0.084(2) 0.073(2) 0.0052(17) 0.0215(15) 0.0269(16)
C1 0.046(3) 0.049(3) 0.054(3) 0.016(2) 0.015(2) 0.022(2)
C2 0.040(3) 0.051(3) 0.048(3) 0.006(2) 0.004(2) 0.012(2)
C3 0.040(2) 0.051(3) 0.044(2) 0.000(2) 0.0032(19) 0.012(2)
C4 0.036(2) 0.047(3) 0.044(2) 0.000(2) 0.0023(18) 0.0068(19)
C5 0.036(2) 0.046(2) 0.045(2) 0.0008(19) 0.0058(18) 0.0075(19)
C6 0.036(2) 0.050(3) 0.043(2) -0.003(2) 0.0057(18) 0.0073(19)
C7 0.037(2) 0.045(2) 0.048(2) 0.000(2) 0.0060(18) 0.0057(18)
C8 0.045(3) 0.074(3) 0.045(3) -0.012(2) 0.009(2) 0.010(2)
C9 0.054(3) 0.082(4) 0.074(3) -0.009(3) 0.024(2) 0.012(3)
O3 0.0493(18) 0.073(2) 0.0518(18) -0.0129(16) 0.0026(15) 0.0168(16)
O4 0.0405(18) 0.070(2) 0.071(2) -0.0055(16) 0.0163(14) 0.0150(15)
C10 0.041(3) 0.048(3) 0.055(3) 0.007(2) 0.017(2) 0.019(2)
C11 0.032(2) 0.051(3) 0.049(3) 0.002(2) 0.0056(19) 0.0072(19)
C12 0.038(2) 0.045(2) 0.045(2) -0.002(2) 0.0046(18) 0.0121(19)
C13 0.036(2) 0.049(3) 0.047(2) -0.002(2) 0.0006(19) 0.0075(19)
C14 0.035(2) 0.048(2) 0.043(2) -0.0030(19) 0.0058(18) 0.0083(18)
C15 0.039(2) 0.052(3) 0.045(2) -0.004(2) 0.0055(19) 0.003(2)
C16 0.042(2) 0.054(3) 0.041(2) -0.001(2) 0.0048(18) 0.009(2)
C17 0.051(3) 0.077(3) 0.042(2) -0.009(2) 0.011(2) 0.010(2)
C18 0.056(3) 0.089(4) 0.069(3) 0.006(3) 0.023(2) 0.018(3)
O5 0.0500(18) 0.071(2) 0.0573(19) -0.0128(16) 0.0084(15) 0.0186(16)
O6 0.0440(19) 0.113(3) 0.067(2) -0.0024(18) 0.0113(15) 0.0383(18)
C19 0.048(3) 0.066(3) 0.043(3) 0.009(2) 0.009(2) 0.024(2)
C20 0.038(2) 0.056(3) 0.044(2) 0.001(2) 0.0023(19) 0.017(2)
C21 0.038(2) 0.047(2) 0.044(2) 0.0009(19) 0.0036(18) 0.0126(19)
C22 0.034(2) 0.047(2) 0.042(2) -0.0016(19) 0.0034(18) 0.0084(18)
C23 0.039(2) 0.048(3) 0.041(2) 0.002(2) 0.0044(19) 0.0087(19)
C24 0.039(2) 0.046(2) 0.042(2) -0.0025(19) 0.0006(18) 0.0076(19)
C25 0.038(2) 0.048(3) 0.044(2) -0.003(2) 0.0041(18) 0.0076(19)
C26 0.042(2) 0.058(3) 0.054(3) 0.000(2) 0.011(2) 0.013(2)
C27 0.050(3) 0.076(3) 0.063(3) -0.003(2) 0.014(2) 0.013(2)
N7 0.026(2) 0.033(6) 0.051(5) -0.005(3) 0.008(3) 0.001(4)
C36 0.025(2) 0.027(5) 0.061(5) -0.008(3) 0.003(3) 0.007(3)
C37 0.0208(17) 0.024(4) 0.048(4) 0.000(3) 0.004(2) 0.000(3)
C38 0.0218(17) 0.045(5) 0.026(3) 0.008(2) -0.0010(19) 0.009(3)
C39 0.0208(17) 0.024(4) 0.048(4) 0.000(3) 0.004(2) 0.000(3)
C40 0.025(2) 0.027(5) 0.061(5) -0.008(3) 0.003(3) 0.007(3)
C41 0.0218(17) 0.045(5) 0.026(3) 0.008(2) -0.0010(19) 0.009(3)
N8 0.0209(18) 0.041(4) 0.037(3) 0.001(3) -0.0026(17) 0.008(3)
C42 0.0265(17) 0.050(5) 0.033(3) 0.002(3) -0.0005(19) 0.011(3)
N9 0.028(2) 0.057(7) 0.023(4) 0.008(3) 0.002(2) 0.014(4)
C43 0.0265(17) 0.050(5) 0.033(3) 0.002(3) -0.0005(19) 0.011(3)
N10 0.0209(18) 0.041(4) 0.037(3) 0.001(3) -0.0026(17) 0.008(3)
N11 0.028(2) 0.053(4) 0.043(3) -0.009(3) -0.002(2) 0.008(3)
N12 0.0271(18) 0.066(4) 0.047(4) -0.014(3) 0.000(2) 0.013(3)
N7B 0.028(3) 0.055(6) 0.045(4) -0.001(4) -0.006(3) 0.017(4)
C36B 0.025(2) 0.082(8) 0.030(6) 0.004(4) -0.004(3) 0.017(4)
C37B 0.023(2) 0.068(7) 0.043(6) -0.004(5) -0.007(3) 0.015(4)
C38B 0.021(2) 0.021(5) 0.049(4) 0.000(3) 0.001(3) -0.001(3)
C39B 0.023(3) 0.044(5) 0.033(4) 0.007(3) -0.004(2) 0.007(3)
C40B 0.026(2) 0.063(7) 0.033(4) 0.003(3) -0.004(3) 0.011(4)
C41B 0.026(2) 0.029(5) 0.045(4) 0.002(3) 0.000(2) 0.005(3)
N8B 0.032(3) 0.064(6) 0.033(3) -0.001(3) -0.010(3) 0.019(3)
C42B 0.0328(18) 0.050(6) 0.036(4) 0.003(3) -0.001(3) 0.008(4)
N9B 0.0322(18) 0.037(6) 0.054(4) -0.001(3) -0.001(3) 0.010(4)
C43B 0.0298(18) 0.033(6) 0.065(5) -0.009(4) 0.010(3) -0.003(4)
N10B 0.0263(19) 0.043(5) 0.073(4) -0.017(3) 0.010(3) -0.002(3)
N11B 0.031(2) 0.050(4) 0.055(4) -0.012(3) 0.004(3) 0.005(3)
N12B 0.0329(18) 0.051(4) 0.043(4) -0.013(3) 0.002(2) 0.009(3)
N1 0.032(3) 0.055(6) 0.032(6) 0.007(5) -0.002(3) 0.023(4)
C28 0.030(3) 0.053(11) 0.029(7) -0.004(4) -0.007(4) 0.018(6)
C29 0.028(3) 0.023(8) 0.036(5) -0.002(3) -0.004(3) 0.011(5)
C30 0.027(2) 0.014(7) 0.042(7) -0.002(4) 0.010(3) -0.007(5)
C31 0.024(2) 0.033(5) 0.049(7) 0.002(5) 0.004(3) 0.008(3)
C32 0.026(3) 0.054(9) 0.049(8) -0.002(6) 0.006(3) 0.010(5)
C33 0.025(2) 0.024(7) 0.038(6) -0.003(4) -0.002(3) 0.006(4)
N2 0.027(3) 0.036(8) 0.048(6) -0.012(4) 0.002(3) -0.006(4)
C34 0.0262(19) 0.042(7) 0.031(7) -0.001(4) -0.007(3) 0.008(5)
N3 0.0251(18) 0.040(6) 0.026(6) 0.012(4) -0.005(3) 0.008(4)
C35 0.0225(17) 0.028(6) 0.041(6) -0.001(5) -0.001(2) 0.005(3)
N4 0.0248(19) 0.042(5) 0.040(5) 0.000(4) 0.003(2) 0.007(3)
N5 0.025(2) 0.053(4) 0.044(4) -0.014(3) -0.005(3) 0.002(3)
N6 0.0231(17) 0.053(4) 0.036(3) -0.013(3) -0.0017(19) 0.006(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
C1 O2 H2 109.5 ?
O1 C1 O2 122.7(4) y
O1 C1 C2 123.7(4) y
O2 C1 C2 113.6(4) y
C1 C2 C3 115.3(3) y
C1 C2 H2A 108.5 ?
C3 C2 H2A 108.5 ?
C1 C2 H2B 108.5 ?
C3 C2 H2B 108.5 ?
H2A C2 H2B 107.5 ?
C4 C3 C2 112.6(3) y
C4 C3 H3A 109.1 ?
C2 C3 H3A 109.1 ?
C4 C3 H3B 109.1 ?
C2 C3 H3B 109.1 ?
H3A C3 H3B 107.8 ?
C5 C4 C3 113.8(3) y
C5 C4 H4A 108.8 ?
C3 C4 H4A 108.8 ?
C5 C4 H4B 108.8 ?
C3 C4 H4B 108.8 ?
H4A C4 H4B 107.7 ?
C4 C5 C6 113.3(3) y
C4 C5 H5A 108.9 ?
C6 C5 H5A 108.9 ?
C4 C5 H5B 108.9 ?
C6 C5 H5B 108.9 ?
H5A C5 H5B 107.7 ?
C7 C6 C5 114.6(3) y
C7 C6 H6A 108.6 ?
C5 C6 H6A 108.6 ?
C7 C6 H6B 108.6 ?
C5 C6 H6B 108.6 ?
H6A C6 H6B 107.6 ?
C8 C7 C6 113.6(3) y
C8 C7 H7A 108.8 ?
C6 C7 H7A 108.8 ?
C8 C7 H7B 108.8 ?
C6 C7 H7B 108.8 ?
H7A C7 H7B 107.7 ?
C7 C8 C9 114.8(3) y
C7 C8 H8A 108.6 ?
C9 C8 H8A 108.6 ?
C7 C8 H8B 108.6 ?
C9 C8 H8B 108.6 ?
H8A C8 H8B 107.6 ?
C8 C9 H9A 109.5 ?
C8 C9 H9B 109.5 ?
H9A C9 H9B 109.5 ?
C8 C9 H9C 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
C10 O4 H4 109.5 ?
O3 C10 O4 122.3(4) y
O3 C10 C11 124.6(4) y
O4 C10 C11 113.0(4) y
C10 C11 C12 114.8(3) y
C10 C11 H11A 108.6 ?
C12 C11 H11A 108.6 ?
C10 C11 H11B 108.6 ?
C12 C11 H11B 108.6 ?
H11A C11 H11B 107.5 ?
C11 C12 C13 113.4(3) y
C11 C12 H12A 108.9 ?
C13 C12 H12A 108.9 ?
C11 C12 H12B 108.9 ?
C13 C12 H12B 108.9 ?
H12A C12 H12B 107.7 ?
C14 C13 C12 114.4(3) y
C14 C13 H13A 108.6 ?
C12 C13 H13A 108.6 ?
C14 C13 H13B 108.6 ?
C12 C13 H13B 108.6 ?
H13A C13 H13B 107.6 ?
C13 C14 C15 113.1(3) y
C13 C14 H14A 109.0 ?
C15 C14 H14A 109.0 ?
C13 C14 H14B 109.0 ?
C15 C14 H14B 109.0 ?
H14A C14 H14B 107.8 ?
C16 C15 C14 114.4(3) y
C16 C15 H15A 108.7 ?
C14 C15 H15A 108.7 ?
C16 C15 H15B 108.7 ?
C14 C15 H15B 108.7 ?
H15A C15 H15B 107.6 ?
C17 C16 C15 113.9(3) y
C17 C16 H16A 108.8 ?
C15 C16 H16A 108.8 ?
C17 C16 H16B 108.8 ?
C15 C16 H16B 108.8 ?
H16A C16 H16B 107.7 ?
C16 C17 C18 114.2(3) y
C16 C17 H17A 108.7 ?
C18 C17 H17A 108.7 ?
C16 C17 H17B 108.7 ?
C18 C17 H17B 108.7 ?
H17A C17 H17B 107.6 ?
C17 C18 H18A 109.5 ?
C17 C18 H18B 109.5 ?
H18A C18 H18B 109.5 ?
C17 C18 H18C 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
C19 O6 H6 109.5 ?
O5 C19 O6 121.9(4) y
O5 C19 C20 124.8(4) y
O6 C19 C20 113.3(4) y
C19 C20 C21 114.0(3) y
C19 C20 H20A 108.8 ?
C21 C20 H20A 108.8 ?
C19 C20 H20B 108.8 ?
C21 C20 H20B 108.8 ?
H20A C20 H20B 107.7 ?
C22 C21 C20 112.7(3) y
C22 C21 H21A 109.0 ?
C20 C21 H21A 109.0 ?
C22 C21 H21B 109.0 ?
C20 C21 H21B 109.0 ?
H21A C21 H21B 107.8 ?
C23 C22 C21 114.2(3) y
C23 C22 H22A 108.7 ?
C21 C22 H22A 108.7 ?
C23 C22 H22B 108.7 ?
C21 C22 H22B 108.7 ?
H22A C22 H22B 107.6 ?
C24 C23 C22 114.4(3) y
C24 C23 H23A 108.7 ?
C22 C23 H23A 108.7 ?
C24 C23 H23B 108.7 ?
C22 C23 H23B 108.7 ?
H23A C23 H23B 107.6 ?
C23 C24 C25 115.0(3) y
C23 C24 H24A 108.5 ?
C25 C24 H24A 108.5 ?
C23 C24 H24B 108.5 ?
C25 C24 H24B 108.5 ?
H24A C24 H24B 107.5 ?
C24 C25 C26 114.2(3) y
C24 C25 H25A 108.7 ?
C26 C25 H25A 108.7 ?
C24 C25 H25B 108.7 ?
C26 C25 H25B 108.7 ?
H25A C25 H25B 107.6 ?
C27 C26 C25 115.1(3) y
C27 C26 H26A 108.5 ?
C25 C26 H26A 108.5 ?
C27 C26 H26B 108.5 ?
C25 C26 H26B 108.5 ?
H26A C26 H26B 107.5 ?
C26 C27 H27A 109.5 ?
C26 C27 H27B 109.5 ?
H27A C27 H27B 109.5 ?
C26 C27 H27C 109.5 ?
H27A C27 H27C 109.5 ?
H27B C27 H27C 109.5 ?
C40 N7 C36 115.0 y
N7 C36 C37 124.5 y
N7 C36 H36 117.8 ?
C37 C36 H36 117.8 ?
C38 C37 C36 116.2 y
C38 C37 H37 121.9 ?
C36 C37 H37 121.9 ?
C37 C38 C39 124.7 y
C37 C38 C41 117.8 y
C39 C38 C41 117.5 y
C38 C39 C40 113.8 y
C38 C39 H39 123.1 ?
C40 C39 H39 123.1 ?
N7 C40 C39 125.7 y
N7 C40 H40 117.1 ?
C39 C40 H40 117.1 ?
N8 C41 N10 121.58(16) y
N8 C41 C38 118.2 y
N10 C41 C38 120.15(16) y
C41 N8 C42 116.0 y
N9 C42 N11 118.5(2) y
N9 C42 N8 124.9 y
N11 C42 N8 116.2(2) y
C42 N9 C43 114.47(16) y
N10 C43 N12 119.3(4) y
N10 C43 N9 125.7(3) y
N12 C43 N9 114.6(4) y
C43 N10 C41 116.9(3) y
C42 N11 H11C 120.0 ?
C42 N11 H11D 120.0 ?
H11C N11 H11D 120.0 ?
C43 N12 H12C 120.0 ?
C43 N12 H12D 120.0 ?
H12C N12 H12D 120.0 ?
C40B N7B C36B 115.03(13) y
N7B C36B C37B 124.41(14) y
N7B C36B H36B 117.8 ?
C37B C36B H36B 117.8 ?
C38B C37B C36B 116.28(13) y
C38B C37B H37B 121.9 ?
C36B C37B H37B 121.9 ?
C37B C38B C39B 124.52(12) y
C37B C38B C41B 118.10(12) y
C39B C38B C41B 117.28(12) y
C38B C39B C40B 113.98(12) y
C38B C39B H39B 123.0 ?
C40B C39B H39B 123.0 ?
N7B C40B C39B 125.63(14) y
N7B C40B H40B 117.2 ?
C39B C40B H40B 117.2 ?
N8B C41B N10B 121.76(18) y
N8B C41B C38B 118.52(12) y
N10B C41B C38B 119.71(19) y
C41B N8B C42B 115.77(12) y
N9B C42B N11B 118.5(2) y
N9B C42B N8B 125.17(12) y
N11B C42B N8B 116.3(2) y
C42B N9B C43B 114.64(19) y
N10B C43B N12B 119.2(4) y
N10B C43B N9B 125.6(3) y
N12B C43B N9B 114.7(4) y
C43B N10B C41B 117.0(3) y
C42B N11B H11E 120.0 ?
C42B N11B H11F 120.0 ?
H11E N11B H11F 120.0 ?
C43B N12B H12E 120.0 ?
C43B N12B H12F 120.0 ?
H12E N12B H12F 120.0 ?
C32 N1 C28 115.00(14) y
N1 C28 C29 124.36(14) y
N1 C28 H28 117.8 ?
C29 C28 H28 117.8 ?
C30 C29 C28 116.39(13) y
C30 C29 H29 121.8 ?
C28 C29 H29 121.8 ?
C29 C30 C31 124.45(12) y
C29 C30 C33 117.88(13) y
C31 C30 C33 117.63(13) y
C30 C31 C32 113.89(13) y
C30 C31 H31 123.1 ?
C32 C31 H31 123.1 ?
N1 C32 C31 125.58(16) y
N1 C32 H32 117.2 ?
C31 C32 H32 117.2 ?
N2 C33 N4 121.6(2) y
N2 C33 C30 118.50(13) y
N4 C33 C30 119.7(2) y
C33 N2 C34 115.84(12) y
N3 C34 N5 118.4(2) y
N3 C34 N2 125.16(12) y
N5 C34 N2 116.3(2) y
C34 N3 C35 114.54(19) y
N4 C35 N6 119.4(4) y
N4 C35 N3 125.6(3) y
N6 C35 N3 114.8(4) y
C35 N4 C33 116.8(3) y
C34 N5 H5C 120.0 ?
C34 N5 H5D 120.0 ?
H5C N5 H5D 120.0 ?
C35 N6 H6C 120.0 ?
C35 N6 H6D 120.0 ?
H6C N6 H6D 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 1.215(4) y
O2 C1 1.308(4) y
O2 H2 0.8400 ?
C1 C2 1.495(5) y
C2 C3 1.525(5) y
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 C4 1.519(5) y
C3 H3A 0.9900 ?
C3 H3B 0.9900 ?
C4 C5 1.517(5) y
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C5 C6 1.523(5) y
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 C7 1.520(5) y
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
C7 C8 1.508(5) y
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 C9 1.516(5) y
C8 H8A 0.9900 ?
C8 H8B 0.9900 ?
C9 H9A 0.9800 ?
C9 H9B 0.9800 ?
C9 H9C 0.9800 ?
O3 C10 1.221(4) y
O4 C10 1.318(4) y
O4 H4 0.8400 ?
C10 C11 1.483(5) y
C11 C12 1.518(5) y
C11 H11A 0.9900 ?
C11 H11B 0.9900 ?
C12 C13 1.521(5) y
C12 H12A 0.9900 ?
C12 H12B 0.9900 ?
C13 C14 1.515(5) y
C13 H13A 0.9900 ?
C13 H13B 0.9900 ?
C14 C15 1.526(5) y
C14 H14A 0.9900 ?
C14 H14B 0.9900 ?
C15 C16 1.520(5) y
C15 H15A 0.9900 ?
C15 H15B 0.9900 ?
C16 C17 1.507(5) y
C16 H16A 0.9900 ?
C16 H16B 0.9900 ?
C17 C18 1.523(6) y
C17 H17A 0.9900 ?
C17 H17B 0.9900 ?
C18 H18A 0.9800 ?
C18 H18B 0.9800 ?
C18 H18C 0.9800 ?
O5 C19 1.213(4) y
O6 C19 1.316(5) y
O6 H6 0.8400 ?
C19 C20 1.490(5) y
C20 C21 1.525(5) y
C20 H20A 0.9900 ?
C20 H20B 0.9900 ?
C21 C22 1.519(5) y
C21 H21A 0.9900 ?
C21 H21B 0.9900 ?
C22 C23 1.516(5) y
C22 H22A 0.9900 ?
C22 H22B 0.9900 ?
C23 C24 1.512(5) y
C23 H23A 0.9900 ?
C23 H23B 0.9900 ?
C24 C25 1.514(5) y
C24 H24A 0.9900 ?
C24 H24B 0.9900 ?
C25 C26 1.514(5) y
C25 H25A 0.9900 ?
C25 H25B 0.9900 ?
C26 C27 1.509(4) y
C26 H26A 0.9900 ?
C26 H26B 0.9900 ?
C27 H27A 0.9800 ?
C27 H27B 0.9800 ?
C27 H27C 0.9800 ?
N7 C40 1.3377 y
N7 C36 1.3628 y
C36 C37 1.3641 y
C36 H36 0.9500 ?
C37 C38 1.3384 y
C37 H37 0.9500 ?
C38 C39 1.3763 y
C38 C41 1.4882 y
C39 C40 1.3846 y
C39 H39 0.9500 ?
C40 H40 0.9500 ?
C41 N8 1.3468 y
C41 N10 1.373(4) y
N8 C42 1.3907 y
C42 N9 1.3201 y
C42 N11 1.3487(10) y
N9 C43 1.351(5) y
C43 N10 1.327(5) y
C43 N12 1.3489(10) y
N11 H11C 0.8800 ?
N11 H11D 0.8800 ?
N12 H12C 0.8800 ?
N12 H12D 0.8800 ?
N7B C40B 1.3377(10) y
N7B C36B 1.3627(10) y
C36B C37B 1.3646(10) y
C36B H36B 0.9500 ?
C37B C38B 1.3382(9) y
C37B H37B 0.9500 ?
C38B C39B 1.3764(9) y
C38B C41B 1.4885(9) y
C39B C40B 1.3839(10) y
C39B H39B 0.9500 ?
C40B H40B 0.9500 ?
C41B N8B 1.3463(9) y
C41B N10B 1.374(4) y
N8B C42B 1.3902(9) y
C42B N9B 1.3196(9) y
C42B N11B 1.3477(14) y
N9B C43B 1.350(5) y
C43B N10B 1.327(5) y
C43B N12B 1.3488(14) y
N11B H11E 0.8800 ?
N11B H11F 0.8800 ?
N12B H12E 0.8800 ?
N12B H12F 0.8800 ?
N1 C32 1.3378(10) y
N1 C28 1.3628(10) y
C28 C29 1.3641(10) y
C28 H28 0.9500 ?
C29 C30 1.3388(9) y
C29 H29 0.9500 ?
C30 C31 1.3761(9) y
C30 C33 1.4885(9) y
C31 C32 1.3846(10) y
C31 H31 0.9500 ?
C32 H32 0.9500 ?
C33 N2 1.3466(10) y
C33 N4 1.374(4) y
N2 C34 1.3902(9) y
C34 N3 1.3198(9) y
C34 N5 1.3479(14) y
N3 C35 1.350(5) y
C35 N4 1.327(5) y
C35 N6 1.3480(14) y
N5 H5C 0.8800 ?
N5 H5D 0.8800 ?
N6 H6C 0.8800 ?
N6 H6D 0.8800 ?
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 H2 N1 0.84 1.66 2.481(6) 166.1 .
O2 H2 N3 0.84 1.97 2.805(5) 176.8 2_766
O4 H4 N7 0.84 1.67 2.500(4) 167.7 .
O4 H4 N9B 0.84 1.92 2.763(5) 175.5 .
O6 H6 N7B 0.84 1.67 2.492(5) 166.5 .
O6 H6 N9 0.84 1.92 2.756(4) 174.7 .
N11 H11D O5 0.88 1.86 2.683(4) 154.9 1_455
N12 H12D O5 0.88 2.06 2.931(5) 169.5 .
N11B H11F O3 0.88 2.01 2.773(5) 144.5 1_655
N12B H12F O3 0.88 2.02 2.892(5) 169.3 .
N5 H5D O1 0.88 1.91 2.710(5) 150.5 2_666
N6 H6D O1 0.88 2.07 2.936(5) 168.9 2_766
N6 H6C N4 0.88 2.25 3.114(7) 168.6 2_866
|
1501550.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501550.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_1501550
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C8 H16 O2, C8 H8 N6'
_chemical_formula_sum 'C16 H24 N6 O2'
_chemical_formula_weight 332.41
_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
_audit_creation_method SHELXL-97
_cell_angle_alpha 104.685(2)
_cell_angle_beta 90.861(2)
_cell_angle_gamma 98.832(3)
_cell_formula_units_Z 2
_cell_length_a 8.8653(4)
_cell_length_b 9.4282(4)
_cell_length_c 10.7014(5)
_cell_measurement_reflns_used 8454
_cell_measurement_temperature 150
_cell_measurement_theta_max 69.07
_cell_measurement_theta_min 4.28
_cell_volume 853.62(7)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.036
_diffrn_reflns_av_sigmaI/netI 0.0411
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 14242
_diffrn_reflns_theta_full 69.30
_diffrn_reflns_theta_max 69.30
_diffrn_reflns_theta_min 4.28
_exptl_absorpt_coefficient_mu 0.726
_exptl_absorpt_correction_T_max 0.9785
_exptl_absorpt_correction_T_min 0.6001
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.293
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 356
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.555
_refine_diff_density_min -0.361
_refine_diff_density_rms 0.099
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 218
_refine_ls_number_reflns 3105
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.069
_refine_ls_R_factor_all 0.0744
_refine_ls_R_factor_gt 0.0701
_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^)+(0.1539P)^2^+0.1124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1849
_refine_ls_wR_factor_ref 0.1955
_reflns_number_gt 2749
_reflns_number_total 3105
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam55
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501550
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
O1 O 0.47582(15) 1.31235(14) 1.01988(13) 0.0426(4) Uani 1 1 d .
O2 O 0.42854(14) 1.13557(14) 0.83620(13) 0.0402(4) Uani 1 1 d .
H2 H 0.3508 1.1755 0.8322 0.060 Uiso 1 1 calc .
C1 C 0.51109(18) 1.20558(18) 0.94235(16) 0.0279(4) Uani 1 1 d .
C2 C 0.65414(18) 1.14146(18) 0.96042(16) 0.0291(4) Uani 1 1 d .
H2A H 0.6486 1.1093 1.0416 0.035 Uiso 1 1 calc R
H2B H 0.7436 1.2213 0.9709 0.035 Uiso 1 1 calc R
C3 C 0.68088(18) 1.01053(17) 0.85080(16) 0.0277(4) Uani 1 1 d .
H3A H 0.6833 1.0406 0.7686 0.033 Uiso 1 1 calc R
H3B H 0.5944 0.9281 0.8425 0.033 Uiso 1 1 calc R
C4 C 0.83007(18) 0.95527(18) 0.87244(16) 0.0296(4) Uani 1 1 d .
H4A H 0.9155 1.0399 0.8894 0.035 Uiso 1 1 calc R
H4B H 0.8236 0.9156 0.9498 0.035 Uiso 1 1 calc R
C5 C 0.86370(19) 0.83468(18) 0.75664(17) 0.0311(4) Uani 1 1 d .
H5A H 0.8678 0.8742 0.6792 0.037 Uiso 1 1 calc R
H5B H 0.7786 0.7498 0.7408 0.037 Uiso 1 1 calc R
C6 C 1.01377(19) 0.7785(2) 0.77407(17) 0.0324(4) Uani 1 1 d .
H6A H 1.0976 0.8646 0.7981 0.039 Uiso 1 1 calc R
H6B H 1.0060 0.7303 0.8464 0.039 Uiso 1 1 calc R
C7 C 1.0542(2) 0.6686(2) 0.65373(18) 0.0354(4) Uani 1 1 d .
H7A H 1.0548 0.7139 0.5798 0.042 Uiso 1 1 calc R
H7B H 0.9745 0.5789 0.6334 0.042 Uiso 1 1 calc R
C8 C 1.2093(2) 0.6227(2) 0.6697(2) 0.0456(5) Uani 1 1 d .
H8A H 1.2889 0.7108 0.6886 0.068 Uiso 1 1 calc R
H8B H 1.2302 0.5526 0.5897 0.068 Uiso 1 1 calc R
H8C H 1.2085 0.5751 0.7413 0.068 Uiso 1 1 calc R
C9 C -0.46436(18) 1.20357(18) 0.53206(16) 0.0291(4) Uani 1 1 d .
H9 H -0.5197 1.1266 0.4647 0.035 Uiso 1 1 calc R
C10 C -0.53069(19) 1.32911(18) 0.58261(18) 0.0306(4) Uani 1 1 d .
H10 H -0.6288 1.3371 0.5509 0.037 Uiso 1 1 calc R
C11 C -0.45003(19) 1.44185(18) 0.68024(17) 0.0313(4) Uani 1 1 d .
H11 H -0.4917 1.5292 0.7171 0.038 Uiso 1 1 calc R
C12 C -0.30684(18) 1.42488(17) 0.72335(16) 0.0270(4) Uani 1 1 d .
H12 H -0.2485 1.5009 0.7897 0.032 Uiso 1 1 calc R
C13 C -0.25027(17) 1.29500(16) 0.66789(15) 0.0223(4) Uani 1 1 d .
C14 C -0.09605(17) 1.27237(16) 0.71168(15) 0.0219(4) Uani 1 1 d .
C15 C 0.10723(17) 1.33944(16) 0.85722(15) 0.0235(4) Uani 1 1 d .
C16 C 0.10658(17) 1.15036(16) 0.67531(15) 0.0229(4) Uani 1 1 d .
N1 N -0.32752(15) 1.18515(14) 0.57283(13) 0.0257(4) Uani 1 1 d .
N2 N -0.03467(15) 1.36146(14) 0.82448(13) 0.0235(3) Uani 1 1 d .
N3 N 0.18020(14) 1.23497(14) 0.78552(13) 0.0256(4) Uani 1 1 d .
N4 N -0.03362(14) 1.16591(13) 0.63290(13) 0.0234(3) Uani 1 1 d .
N5 N 0.18004(15) 1.42551(15) 0.96535(13) 0.0303(4) Uani 1 1 d .
H5C H 0.2721 1.4128 0.9874 0.036 Uiso 1 1 calc .
H5D H 0.1363 1.4953 1.0152 0.036 Uiso 1 1 calc .
N6 N 0.17546(15) 1.04545(15) 0.60301(13) 0.0283(4) Uani 1 1 d .
H6C H 0.2665 1.0333 0.6281 0.034 Uiso 1 1 calc .
H6D H 0.1300 0.9880 0.5300 0.034 Uiso 1 1 calc .
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 0.0400(7) 0.0419(7) 0.0410(8) -0.0084(6) -0.0075(6) 0.0245(6)
O2 0.0345(7) 0.0444(7) 0.0373(7) -0.0073(6) -0.0089(5) 0.0245(6)
C1 0.0243(8) 0.0292(8) 0.0307(8) 0.0057(6) 0.0010(6) 0.0093(6)
C2 0.0233(8) 0.0332(8) 0.0317(8) 0.0059(7) -0.0007(6) 0.0120(7)
C3 0.0229(8) 0.0292(8) 0.0331(9) 0.0082(7) 0.0012(6) 0.0103(6)
C4 0.0248(8) 0.0333(8) 0.0332(9) 0.0080(7) 0.0027(6) 0.0135(7)
C5 0.0277(8) 0.0305(8) 0.0373(9) 0.0080(7) 0.0013(7) 0.0124(7)
C6 0.0288(9) 0.0372(9) 0.0360(9) 0.0114(7) 0.0064(7) 0.0168(7)
C7 0.0357(9) 0.0353(9) 0.0394(10) 0.0096(7) 0.0085(7) 0.0182(7)
C8 0.0427(11) 0.0544(11) 0.0520(12) 0.0214(9) 0.0188(9) 0.0312(9)
C9 0.0235(8) 0.0293(8) 0.0317(8) 0.0009(6) -0.0020(6) 0.0078(6)
C10 0.0224(8) 0.0327(8) 0.0375(9) 0.0061(7) -0.0008(7) 0.0123(7)
C11 0.0297(9) 0.0290(8) 0.0351(9) 0.0019(7) 0.0011(7) 0.0160(7)
C12 0.0270(8) 0.0256(8) 0.0271(8) 0.0004(6) 0.0004(6) 0.0113(6)
C13 0.0218(8) 0.0231(7) 0.0224(7) 0.0037(6) 0.0032(6) 0.0087(6)
C14 0.0216(8) 0.0198(7) 0.0239(7) 0.0025(6) 0.0024(6) 0.0071(6)
C15 0.0215(7) 0.0238(7) 0.0248(8) 0.0023(6) 0.0025(6) 0.0092(6)
C16 0.0206(7) 0.0236(7) 0.0238(8) 0.0019(6) 0.0019(6) 0.0083(6)
N1 0.0223(7) 0.0261(7) 0.0273(7) 0.0008(5) 0.0001(5) 0.0101(5)
N2 0.0210(7) 0.0234(6) 0.0248(7) 0.0009(5) -0.0003(5) 0.0092(5)
N3 0.0218(7) 0.0277(7) 0.0246(7) -0.0019(5) 0.0003(5) 0.0106(5)
N4 0.0223(7) 0.0226(6) 0.0237(7) -0.0006(5) 0.0004(5) 0.0103(5)
N5 0.0233(7) 0.0343(7) 0.0284(8) -0.0065(6) -0.0042(5) 0.0145(6)
N6 0.0217(6) 0.0296(7) 0.0291(7) -0.0060(5) -0.0017(5) 0.0139(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
C1 O2 H2 109.5 ?
O1 C1 O2 122.91(14) y
O1 C1 C2 123.08(15) y
O2 C1 C2 114.01(13) y
C1 C2 C3 115.24(14) y
C1 C2 H2A 108.5 ?
C3 C2 H2A 108.5 ?
C1 C2 H2B 108.5 ?
C3 C2 H2B 108.5 ?
H2A C2 H2B 107.5 ?
C2 C3 C4 112.59(14) y
C2 C3 H3A 109.1 ?
C4 C3 H3A 109.1 ?
C2 C3 H3B 109.1 ?
C4 C3 H3B 109.1 ?
H3A C3 H3B 107.8 ?
C5 C4 C3 112.24(14) y
C5 C4 H4A 109.2 ?
C3 C4 H4A 109.2 ?
C5 C4 H4B 109.2 ?
C3 C4 H4B 109.2 ?
H4A C4 H4B 107.9 ?
C4 C5 C6 113.66(14) y
C4 C5 H5A 108.8 ?
C6 C5 H5A 108.8 ?
C4 C5 H5B 108.8 ?
C6 C5 H5B 108.8 ?
H5A C5 H5B 107.7 ?
C7 C6 C5 113.48(15) y
C7 C6 H6A 108.9 ?
C5 C6 H6A 108.9 ?
C7 C6 H6B 108.9 ?
C5 C6 H6B 108.9 ?
H6A C6 H6B 107.7 ?
C6 C7 C8 112.67(16) y
C6 C7 H7A 109.1 ?
C8 C7 H7A 109.1 ?
C6 C7 H7B 109.1 ?
C8 C7 H7B 109.1 ?
H7A C7 H7B 107.8 ?
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 ?
N1 C9 C10 123.77(15) y
N1 C9 H9 118.1 ?
C10 C9 H9 118.1 ?
C11 C10 C9 118.30(15) y
C11 C10 H10 120.8 ?
C9 C10 H10 120.8 ?
C10 C11 C12 118.69(14) y
C10 C11 H11 120.7 ?
C12 C11 H11 120.7 ?
C11 C12 C13 119.00(14) y
C11 C12 H12 120.5 ?
C13 C12 H12 120.5 ?
N1 C13 C12 122.73(14) y
N1 C13 C14 116.61(13) y
C12 C13 C14 120.65(14) y
N4 C14 N2 126.64(14) y
N4 C14 C13 116.42(13) y
N2 C14 C13 116.93(13) y
N5 C15 N3 117.06(13) y
N5 C15 N2 119.08(13) y
N3 C15 N2 123.86(14) y
N6 C16 N3 117.82(13) y
N6 C16 N4 118.16(13) y
N3 C16 N4 124.02(13) y
C9 N1 C13 117.51(13) y
C14 N2 C15 114.41(13) y
C16 N3 C15 116.52(13) y
C14 N4 C16 114.54(13) y
C15 N5 H5C 120.0 ?
C15 N5 H5D 120.0 ?
H5C N5 H5D 120.0 ?
C16 N6 H6C 120.0 ?
C16 N6 H6D 120.0 ?
H6C N6 H6D 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 1.217(2) y
O2 C1 1.307(2) y
O2 H2 0.8400 ?
C1 C2 1.516(2) y
C2 C3 1.523(2) y
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 C4 1.529(2) y
C3 H3A 0.9900 ?
C3 H3B 0.9900 ?
C4 C5 1.522(2) y
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C5 C6 1.531(2) y
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 C7 1.521(2) y
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
C7 C8 1.523(2) y
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 H8A 0.9800 ?
C8 H8B 0.9800 ?
C8 H8C 0.9800 ?
C9 N1 1.334(2) y
C9 C10 1.392(2) y
C9 H9 0.9500 ?
C10 C11 1.383(2) y
C10 H10 0.9500 ?
C11 C12 1.390(2) y
C11 H11 0.9500 ?
C12 C13 1.390(2) y
C12 H12 0.9500 ?
C13 N1 1.343(2) y
C13 C14 1.502(2) y
C14 N4 1.3342(19) y
C14 N2 1.336(2) y
C15 N5 1.325(2) y
C15 N3 1.3434(19) y
C15 N2 1.361(2) y
C16 N6 1.3272(19) y
C16 N3 1.339(2) y
C16 N4 1.3583(19) y
N5 H5C 0.8800 ?
N5 H5D 0.8800 ?
N6 H6C 0.8800 ?
N6 H6D 0.8800 ?
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 H2 N3 0.84 1.8 2.6220(17) 166.7 .
N5 H5C O1 0.88 2.23 3.0795(18) 163.4 .
N5 H5D N2 0.88 2.2 3.0569(19) 165.6 2_587
N6 H6C O2 0.88 2.52 3.1866(18) 133.2 .
N6 H6D N4 0.88 2.04 2.9172(19) 173.1 2_576
|
1501551.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 17:43:13 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501551.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_1501551
loop_
_publ_author_name
'Adam Duong'
'Marc-Andr\'e Dubois'
'Thierry Maris'
'Val\'erie M\'etivaud'
'Ji-Hyun Yi'
'Antonio Nanci'
'Alain Rochefort'
'Wuest,James D'
_publ_section_title
;
Engineering Homologous Molecular Organization in 2D and 3D.
Cocrystallization of Pyridyl-Substituted Diaminotriazines with
Alkanecarboxylic Acids
;
_journal_name_full 'The Journal of Physical Chemistry C'
_journal_page_first 12908
_journal_page_last 12919
_journal_paper_doi 10.1021/jp201119g
_journal_volume 115
_journal_year 2011
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_moiety 'C14 H12 N6, 2(C9 H18 O2)'
_chemical_formula_sum 'C32 H48 N6 O4'
_chemical_formula_weight 580.76
_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
_cell_angle_beta 102.299(5)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 58.554(7)
_cell_length_b 7.9545(10)
_cell_length_c 14.0407(15)
_cell_measurement_reflns_used 3945
_cell_measurement_temperature 150
_cell_measurement_theta_max 54.27
_cell_measurement_theta_min 4.64
_cell_volume 6389.6(13)
_computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material 'UdMX (Maris, 2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature 150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type 'Bruker Microstar'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Helios optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.113
_diffrn_reflns_av_sigmaI/netI 0.0858
_diffrn_reflns_limit_h_max 54
_diffrn_reflns_limit_h_min -63
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 48619
_diffrn_reflns_theta_full 57.55
_diffrn_reflns_theta_max 57.55
_diffrn_reflns_theta_min 3.09
_exptl_absorpt_coefficient_mu 0.646
_exptl_absorpt_correction_T_max 0.9808
_exptl_absorpt_correction_T_min 0.7193
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.208
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 2512
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.423
_refine_diff_density_min -0.268
_refine_diff_density_rms 0.076
_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 381
_refine_ls_number_reflns 4231
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.1553
_refine_ls_R_factor_gt 0.0981
_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^)+(0.1639P)^2^+11.2748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2534
_refine_ls_wR_factor_ref 0.2954
_reflns_number_gt 2484
_reflns_number_total 4231
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block adam56
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_* data items to establish
relationships between loop packets from different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501551
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
C1 C 0.57735(10) 0.3166(9) 0.2960(4) 0.0639(18) Uani 1 1 d .
H1 H 0.5777 0.3027 0.2291 0.077 Uiso 1 1 calc R
C2 C 0.55999(9) 0.4130(8) 0.3186(4) 0.0581(16) Uani 1 1 d .
H2 H 0.5488 0.4634 0.2678 0.070 Uiso 1 1 calc R
C3 C 0.55851(9) 0.4383(8) 0.4156(3) 0.0539(16) Uani 1 1 d .
C4 C 0.57578(9) 0.3558(8) 0.4852(4) 0.0611(17) Uani 1 1 d .
H4 H 0.5758 0.3661 0.5527 0.073 Uiso 1 1 calc R
C5 C 0.59259(10) 0.2604(9) 0.4552(4) 0.0647(18) Uani 1 1 d .
H5 H 0.6039 0.2055 0.5037 0.078 Uiso 1 1 calc R
C6 C 0.53994(9) 0.5407(8) 0.4433(3) 0.0522(15) Uani 1 1 d .
C7 C 0.51981(9) 0.5809(8) 0.3761(4) 0.0573(16) Uani 1 1 d .
H7 H 0.5180 0.5423 0.3108 0.069 Uiso 1 1 calc R
C8 C 0.50217(9) 0.6761(8) 0.4015(3) 0.0582(16) Uani 1 1 d .
H8 H 0.4886 0.7029 0.3534 0.070 Uiso 1 1 calc R
C9 C 0.50405(8) 0.7331(7) 0.4967(3) 0.0493(15) Uani 1 1 d .
C10 C 0.52411(9) 0.6899(8) 0.5652(3) 0.0571(16) Uani 1 1 d .
H10 H 0.5257 0.7252 0.6309 0.069 Uiso 1 1 calc R
C11 C 0.54168(9) 0.5962(9) 0.5385(4) 0.0617(17) Uani 1 1 d .
H11 H 0.5552 0.5692 0.5863 0.074 Uiso 1 1 calc R
C12 C 0.48518(9) 0.8333(8) 0.5223(4) 0.0547(16) Uani 1 1 d .
C13 C 0.45049(9) 0.9674(8) 0.4764(3) 0.0550(16) Uani 1 1 d .
C14 C 0.46953(9) 0.9696(8) 0.6359(4) 0.0525(15) Uani 1 1 d .
N1 N 0.59387(7) 0.2405(7) 0.3623(3) 0.0601(14) Uani 1 1 d .
N2 N 0.46703(7) 0.8727(6) 0.4509(3) 0.0554(13) Uani 1 1 d .
N3 N 0.45096(7) 1.0203(6) 0.5687(3) 0.0532(13) Uani 1 1 d .
N4 N 0.48749(7) 0.8787(6) 0.6174(3) 0.0530(13) Uani 1 1 d .
N5 N 0.43202(7) 1.0115(7) 0.4081(3) 0.0600(14) Uani 1 1 d .
H5A H 0.4309 0.9781 0.3475 0.072 Uiso 1 1 calc .
H5B H 0.4209 1.0740 0.4235 0.072 Uiso 1 1 calc .
N6 N 0.47011(7) 1.0135(6) 0.7286(3) 0.0540(13) Uani 1 1 d .
H6A H 0.4586 1.0729 0.7431 0.065 Uiso 1 1 calc .
H6B H 0.4820 0.9828 0.7751 0.065 Uiso 1 1 calc .
O1 O 0.61450(7) 0.1720(7) 0.1605(3) 0.0838(15) Uani 1 1 d .
O2 O 0.63191(7) 0.1185(6) 0.3132(3) 0.0793(14) Uani 1 1 d .
H2A H 0.6182 0.1290 0.3218 0.119 Uiso 1 1 calc .
C15 C 0.63180(10) 0.1315(8) 0.2181(4) 0.0637(17) Uani 1 1 d .
C16 C 0.65495(10) 0.0943(9) 0.1969(4) 0.0694(18) Uani 1 1 d .
H16A H 0.6597 -0.0199 0.2213 0.083 Uiso 1 1 calc R
H16B H 0.6664 0.1743 0.2340 0.083 Uiso 1 1 calc R
C17 C 0.65631(10) 0.1036(9) 0.0897(4) 0.0681(18) Uani 1 1 d .
H17A H 0.6459 0.0177 0.0524 0.082 Uiso 1 1 calc R
H17B H 0.6509 0.2154 0.0633 0.082 Uiso 1 1 calc R
C18 C 0.68105(10) 0.0746(9) 0.0770(4) 0.0662(17) Uani 1 1 d .
H18A H 0.6862 -0.0378 0.1033 0.079 Uiso 1 1 calc R
H18B H 0.6914 0.1588 0.1164 0.079 Uiso 1 1 calc R
C19 C 0.68419(10) 0.0850(9) -0.0281(4) 0.0663(18) Uani 1 1 d .
H19A H 0.6747 -0.0042 -0.0669 0.080 Uiso 1 1 calc R
H19B H 0.6782 0.1947 -0.0560 0.080 Uiso 1 1 calc R
C20 C 0.70926(10) 0.0659(9) -0.0369(4) 0.0672(18) Uani 1 1 d .
H20A H 0.7151 -0.0435 -0.0082 0.081 Uiso 1 1 calc R
H20B H 0.7186 0.1549 0.0025 0.081 Uiso 1 1 calc R
C21 C 0.71359(10) 0.0746(10) -0.1398(4) 0.0735(19) Uani 1 1 d .
H21A H 0.7052 -0.0193 -0.1782 0.088 Uiso 1 1 calc R
H21B H 0.7069 0.1807 -0.1703 0.088 Uiso 1 1 calc R
C22 C 0.73862(11) 0.0663(12) -0.1457(4) 0.091(2) Uani 1 1 d .
H22A H 0.7452 -0.0409 -0.1162 0.110 Uiso 1 1 calc R
H22B H 0.7471 0.1587 -0.1060 0.110 Uiso 1 1 calc R
C23 C 0.74331(12) 0.0782(13) -0.2474(5) 0.106(3) Uani 1 1 d .
H23A H 0.7379 -0.0248 -0.2835 0.160 Uiso 1 1 calc R
H23B H 0.7601 0.0922 -0.2433 0.160 Uiso 1 1 calc R
H23C H 0.7349 0.1749 -0.2812 0.160 Uiso 1 1 calc R
O3 O 0.42476(6) 1.2001(6) 0.7367(2) 0.0657(12) Uani 1 1 d .
O4 O 0.41333(6) 1.1897(6) 0.5759(2) 0.0714(13) Uani 1 1 d .
H4A H 0.4277 1.1755 0.5791 0.107 Uiso 1 1 calc .
C24 C 0.40981(10) 1.2273(9) 0.6626(4) 0.0635(18) Uani 1 1 d .
C25 C 0.38666(9) 1.3021(9) 0.6613(4) 0.0647(18) Uani 1 1 d .
H25A H 0.3744 1.2252 0.6264 0.078 Uiso 1 1 calc R
H25B H 0.3853 1.4089 0.6244 0.078 Uiso 1 1 calc R
C26 C 0.38215(10) 1.3366(9) 0.7624(4) 0.0680(18) Uani 1 1 d .
H26A H 0.3858 1.2337 0.8024 0.082 Uiso 1 1 calc R
H26B H 0.3930 1.4259 0.7936 0.082 Uiso 1 1 calc R
C27 C 0.35732(10) 1.3900(9) 0.7632(4) 0.0677(18) Uani 1 1 d .
H27A H 0.3463 1.3096 0.7237 0.081 Uiso 1 1 calc R
H27B H 0.3544 1.5021 0.7324 0.081 Uiso 1 1 calc R
C28 C 0.35264(9) 1.3974(9) 0.8653(4) 0.0656(18) Uani 1 1 d .
H28A H 0.3578 1.2902 0.8988 0.079 Uiso 1 1 calc R
H28B H 0.3623 1.4881 0.9016 0.079 Uiso 1 1 calc R
C29 C 0.32752(10) 1.4274(9) 0.8708(4) 0.0687(18) Uani 1 1 d .
H29A H 0.3176 1.3417 0.8308 0.082 Uiso 1 1 calc R
H29B H 0.3226 1.5389 0.8425 0.082 Uiso 1 1 calc R
C30 C 0.32343(10) 1.4205(9) 0.9751(4) 0.0676(18) Uani 1 1 d .
H30A H 0.3291 1.3112 1.0045 0.081 Uiso 1 1 calc R
H30B H 0.3328 1.5101 1.0141 0.081 Uiso 1 1 calc R
C31 C 0.29811(10) 1.4418(10) 0.9805(4) 0.075(2) Uani 1 1 d .
H31A H 0.2887 1.3533 0.9406 0.090 Uiso 1 1 calc R
H31B H 0.2925 1.5518 0.9519 0.090 Uiso 1 1 calc R
C32 C 0.29395(12) 1.4325(11) 1.0840(5) 0.091(2) Uani 1 1 d .
H32A H 0.3022 1.5252 1.1228 0.136 Uiso 1 1 calc R
H32B H 0.2998 1.3252 1.1137 0.136 Uiso 1 1 calc R
H32C H 0.2772 1.4411 1.0822 0.136 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
C1 0.069(4) 0.086(5) 0.039(3) -0.005(3) 0.016(3) 0.006(4)
C2 0.065(3) 0.074(5) 0.035(3) 0.002(3) 0.012(2) 0.005(3)
C3 0.059(3) 0.068(5) 0.036(3) 0.000(3) 0.012(2) -0.003(3)
C4 0.071(4) 0.082(5) 0.032(3) -0.002(3) 0.014(3) 0.003(3)
C5 0.061(3) 0.086(5) 0.048(3) 0.005(3) 0.013(3) 0.006(3)
C6 0.055(3) 0.068(5) 0.035(3) 0.003(3) 0.012(2) -0.001(3)
C7 0.068(4) 0.071(5) 0.035(3) 0.000(3) 0.015(3) 0.000(3)
C8 0.064(3) 0.081(5) 0.030(3) 0.007(3) 0.010(2) 0.003(3)
C9 0.060(3) 0.054(4) 0.034(3) 0.005(3) 0.012(2) -0.002(3)
C10 0.064(3) 0.077(5) 0.031(3) -0.006(3) 0.012(2) 0.001(3)
C11 0.062(3) 0.086(5) 0.037(3) 0.004(3) 0.010(2) 0.004(3)
C12 0.061(3) 0.067(5) 0.036(3) 0.000(3) 0.011(2) -0.003(3)
C13 0.057(3) 0.074(5) 0.036(3) 0.002(3) 0.014(3) -0.001(3)
C14 0.058(3) 0.066(5) 0.036(3) 0.000(3) 0.015(2) -0.003(3)
N1 0.063(3) 0.079(4) 0.040(3) -0.003(2) 0.016(2) 0.003(3)
N2 0.061(3) 0.079(4) 0.027(2) 0.002(2) 0.013(2) -0.002(3)
N3 0.063(3) 0.069(4) 0.030(2) -0.004(2) 0.0135(19) 0.000(2)
N4 0.066(3) 0.070(4) 0.025(2) 0.005(2) 0.0140(19) -0.002(3)
N5 0.066(3) 0.083(4) 0.030(2) -0.001(2) 0.009(2) 0.009(3)
N6 0.072(3) 0.070(4) 0.023(2) -0.002(2) 0.0156(18) 0.006(2)
O1 0.066(3) 0.137(5) 0.049(2) -0.004(3) 0.012(2) -0.002(3)
O2 0.080(3) 0.120(4) 0.042(2) 0.006(2) 0.0214(18) 0.015(3)
C15 0.065(4) 0.072(5) 0.053(4) -0.009(3) 0.009(3) -0.005(3)
C16 0.063(4) 0.093(6) 0.054(3) 0.004(3) 0.015(3) -0.001(3)
C17 0.074(4) 0.085(6) 0.045(3) 0.002(3) 0.014(3) -0.001(3)
C18 0.073(4) 0.080(5) 0.047(3) 0.002(3) 0.016(3) 0.002(3)
C19 0.074(4) 0.079(5) 0.046(3) -0.001(3) 0.013(3) -0.002(3)
C20 0.071(4) 0.082(5) 0.050(3) 0.004(3) 0.015(3) 0.000(3)
C21 0.072(4) 0.098(6) 0.051(3) -0.005(3) 0.015(3) 0.001(4)
C22 0.072(4) 0.145(8) 0.059(4) -0.004(4) 0.018(3) -0.001(4)
C23 0.102(5) 0.164(9) 0.063(4) -0.002(5) 0.036(4) 0.003(5)
O3 0.075(2) 0.087(4) 0.036(2) 0.002(2) 0.0129(18) 0.007(2)
O4 0.077(3) 0.100(4) 0.039(2) -0.007(2) 0.0151(17) 0.015(2)
C24 0.071(4) 0.084(5) 0.037(3) 0.007(3) 0.015(3) -0.003(3)
C25 0.069(4) 0.083(5) 0.043(3) 0.003(3) 0.013(3) 0.005(3)
C26 0.075(4) 0.089(6) 0.042(3) -0.003(3) 0.016(3) 0.004(3)
C27 0.069(4) 0.080(5) 0.055(3) -0.005(3) 0.014(3) 0.002(3)
C28 0.073(4) 0.080(5) 0.045(3) -0.002(3) 0.016(3) 0.004(3)
C29 0.070(4) 0.087(6) 0.051(3) 0.006(3) 0.016(3) 0.001(3)
C30 0.082(4) 0.075(5) 0.047(3) -0.004(3) 0.016(3) 0.001(3)
C31 0.072(4) 0.092(6) 0.065(4) 0.002(4) 0.024(3) -0.003(4)
C32 0.102(5) 0.114(7) 0.065(4) -0.005(4) 0.037(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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_publ_flag
N1 C1 C2 123.9(5) y
N1 C1 H1 118.0 ?
C2 C1 H1 118.0 ?
C1 C2 C3 120.7(5) y
C1 C2 H2 119.6 ?
C3 C2 H2 119.6 ?
C2 C3 C4 115.1(5) y
C2 C3 C6 122.6(5) y
C4 C3 C6 122.3(4) y
C5 C4 C3 119.9(5) y
C5 C4 H4 120.0 ?
C3 C4 H4 120.0 ?
N1 C5 C4 123.8(5) y
N1 C5 H5 118.1 ?
C4 C5 H5 118.1 ?
C7 C6 C11 117.4(5) y
C7 C6 C3 121.1(5) y
C11 C6 C3 121.4(5) y
C6 C7 C8 121.6(5) y
C6 C7 H7 119.2 ?
C8 C7 H7 119.2 ?
C7 C8 C9 120.9(5) y
C7 C8 H8 119.6 ?
C9 C8 H8 119.6 ?
C8 C9 C10 117.7(5) y
C8 C9 C12 120.1(5) y
C10 C9 C12 122.2(5) y
C11 C10 C9 120.7(5) y
C11 C10 H10 119.6 ?
C9 C10 H10 119.6 ?
C10 C11 C6 121.6(5) y
C10 C11 H11 119.2 ?
C6 C11 H11 119.2 ?
N2 C12 N4 124.8(5) y
N2 C12 C9 117.7(5) y
N4 C12 C9 117.5(4) y
N5 C13 N2 118.7(5) y
N5 C13 N3 117.1(5) y
N2 C13 N3 124.2(5) y
N6 C14 N3 117.0(5) y
N6 C14 N4 117.9(5) y
N3 C14 N4 125.1(4) y
C5 N1 C1 116.5(5) y
C12 N2 C13 116.1(4) y
C14 N3 C13 115.3(5) y
C14 N4 C12 114.4(4) y
C13 N5 H5A 120.0 ?
C13 N5 H5B 120.0 ?
H5A N5 H5B 120.0 ?
C14 N6 H6A 120.0 ?
C14 N6 H6B 120.0 ?
H6A N6 H6B 120.0 ?
C15 O2 H2A 109.5 ?
O1 C15 O2 121.3(5) y
O1 C15 C16 126.7(5) y
O2 C15 C16 112.0(5) y
C15 C16 C17 115.5(5) y
C15 C16 H16A 108.4 ?
C17 C16 H16A 108.4 ?
C15 C16 H16B 108.4 ?
C17 C16 H16B 108.4 ?
H16A C16 H16B 107.5 ?
C18 C17 C16 111.1(4) y
C18 C17 H17A 109.4 ?
C16 C17 H17A 109.4 ?
C18 C17 H17B 109.4 ?
C16 C17 H17B 109.4 ?
H17A C17 H17B 108.0 ?
C17 C18 C19 114.8(4) y
C17 C18 H18A 108.6 ?
C19 C18 H18A 108.6 ?
C17 C18 H18B 108.6 ?
C19 C18 H18B 108.6 ?
H18A C18 H18B 107.6 ?
C20 C19 C18 113.1(4) y
C20 C19 H19A 109.0 ?
C18 C19 H19A 109.0 ?
C20 C19 H19B 109.0 ?
C18 C19 H19B 109.0 ?
H19A C19 H19B 107.8 ?
C19 C20 C21 115.8(5) y
C19 C20 H20A 108.3 ?
C21 C20 H20A 108.3 ?
C19 C20 H20B 108.3 ?
C21 C20 H20B 108.3 ?
H20A C20 H20B 107.4 ?
C22 C21 C20 114.6(5) y
C22 C21 H21A 108.6 ?
C20 C21 H21A 108.6 ?
C22 C21 H21B 108.6 ?
C20 C21 H21B 108.6 ?
H21A C21 H21B 107.6 ?
C21 C22 C23 115.4(5) y
C21 C22 H22A 108.4 ?
C23 C22 H22A 108.4 ?
C21 C22 H22B 108.4 ?
C23 C22 H22B 108.4 ?
H22A C22 H22B 107.5 ?
C22 C23 H23A 109.5 ?
C22 C23 H23B 109.5 ?
H23A C23 H23B 109.5 ?
C22 C23 H23C 109.5 ?
H23A C23 H23C 109.5 ?
H23B C23 H23C 109.5 ?
C24 O4 H4A 109.5 ?
O3 C24 O4 121.5(5) y
O3 C24 C25 124.7(5) y
O4 C24 C25 113.9(5) y
C24 C25 C26 113.6(4) y
C24 C25 H25A 108.8 ?
C26 C25 H25A 108.8 ?
C24 C25 H25B 108.8 ?
C26 C25 H25B 108.8 ?
H25A C25 H25B 107.7 ?
C27 C26 C25 114.3(4) y
C27 C26 H26A 108.7 ?
C25 C26 H26A 108.7 ?
C27 C26 H26B 108.7 ?
C25 C26 H26B 108.7 ?
H26A C26 H26B 107.6 ?
C26 C27 C28 112.5(4) y
C26 C27 H27A 109.1 ?
C28 C27 H27A 109.1 ?
C26 C27 H27B 109.1 ?
C28 C27 H27B 109.1 ?
H27A C27 H27B 107.8 ?
C29 C28 C27 115.3(4) y
C29 C28 H28A 108.4 ?
C27 C28 H28A 108.4 ?
C29 C28 H28B 108.4 ?
C27 C28 H28B 108.4 ?
H28A C28 H28B 107.5 ?
C28 C29 C30 113.2(5) y
C28 C29 H29A 108.9 ?
C30 C29 H29A 108.9 ?
C28 C29 H29B 108.9 ?
C30 C29 H29B 108.9 ?
H29A C29 H29B 107.7 ?
C31 C30 C29 113.4(5) y
C31 C30 H30A 108.9 ?
C29 C30 H30A 108.9 ?
C31 C30 H30B 108.9 ?
C29 C30 H30B 108.9 ?
H30A C30 H30B 107.7 ?
C30 C31 C32 113.5(5) y
C30 C31 H31A 108.9 ?
C32 C31 H31A 108.9 ?
C30 C31 H31B 108.9 ?
C32 C31 H31B 108.9 ?
H31A C31 H31B 107.7 ?
C31 C32 H32A 109.5 ?
C31 C32 H32B 109.5 ?
H32A C32 H32B 109.5 ?
C31 C32 H32C 109.5 ?
H32A C32 H32C 109.5 ?
H32B C32 H32C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.336(7) y
C1 C2 1.363(8) y
C1 H1 0.9500 ?
C2 C3 1.397(7) y
C2 H2 0.9500 ?
C3 C4 1.410(7) y
C3 C6 1.475(8) y
C4 C5 1.377(8) y
C4 H4 0.9500 ?
C5 N1 1.332(6) y
C5 H5 0.9500 ?
C6 C7 1.382(7) y
C6 C11 1.389(7) y
C7 C8 1.387(8) y
C7 H7 0.9500 ?
C8 C9 1.393(7) y
C8 H8 0.9500 ?
C9 C10 1.393(7) y
C9 C12 1.467(8) y
C10 C11 1.385(8) y
C10 H10 0.9500 ?
C11 H11 0.9500 ?
C12 N2 1.334(6) y
C12 N4 1.362(6) y
C13 N5 1.330(6) y
C13 N2 1.334(7) y
C13 N3 1.357(6) y
C14 N6 1.341(6) y
C14 N3 1.341(6) y
C14 N4 1.346(7) y
N5 H5A 0.8800 ?
N5 H5B 0.8800 ?
N6 H6A 0.8800 ?
N6 H6B 0.8800 ?
O1 C15 1.198(6) y
O2 C15 1.337(6) y
O2 H2A 0.8400 ?
C15 C16 1.477(8) y
C16 C17 1.525(7) y
C16 H16A 0.9900 ?
C16 H16B 0.9900 ?
C17 C18 1.513(7) y
C17 H17A 0.9900 ?
C17 H17B 0.9900 ?
C18 C19 1.527(7) y
C18 H18A 0.9900 ?
C18 H18B 0.9900 ?
C19 C20 1.506(7) y
C19 H19A 0.9900 ?
C19 H19B 0.9900 ?
C20 C21 1.519(7) y
C20 H20A 0.9900 ?
C20 H20B 0.9900 ?
C21 C22 1.486(8) y
C21 H21A 0.9900 ?
C21 H21B 0.9900 ?
C22 C23 1.512(8) y
C22 H22A 0.9900 ?
C22 H22B 0.9900 ?
C23 H23A 0.9800 ?
C23 H23B 0.9800 ?
C23 H23C 0.9800 ?
O3 C24 1.228(6) y
O4 C24 1.311(6) y
O4 H4A 0.8400 ?
C24 C25 1.477(8) y
C25 C26 1.522(7) y
C25 H25A 0.9900 ?
C25 H25B 0.9900 ?
C26 C27 1.516(7) y
C26 H26A 0.9900 ?
C26 H26B 0.9900 ?
C27 C28 1.517(7) y
C27 H27A 0.9900 ?
C27 H27B 0.9900 ?
C28 C29 1.507(7) y
C28 H28A 0.9900 ?
C28 H28B 0.9900 ?
C29 C30 1.533(7) y
C29 H29A 0.9900 ?
C29 H29B 0.9900 ?
C30 C31 1.509(8) y
C30 H30A 0.9900 ?
C30 H30B 0.9900 ?
C31 C32 1.526(8) y
C31 H31A 0.9900 ?
C31 H31B 0.9900 ?
C32 H32A 0.9800 ?
C32 H32B 0.9800 ?
C32 H32C 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
N5 H5A O3 0.88 2.08 2.893(6) 153.4 6_575
N5 H5B O1 0.88 2.29 2.976(6) 134.3 2_665
N5 H5B O4 0.88 2.45 3.138(6) 134.9 .
N6 H6A O3 0.88 2.21 3.064(6) 163.5 .
N6 H6B N4 0.88 2.24 3.115(6) 173.4 2_656
O2 H2A N1 0.84 1.87 2.650(6) 154.8 .
O4 H4A N3 0.84 1.87 2.602(6) 145.4 .
|
1501552.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/15/1501552.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_1501552
loop_
_publ_author_name
'Okba Saied'
'Thierry Maris'
'Michel Simard'
'Wuest,James D'
_publ_section_title
;
Tectonique Mol\'eculaire: Stabilisation d'un polymorphe d'inclusion
m\'etastable
;
_journal_name_full
'Journal de la Soci\'et\'e Chimique de Tunisie'
_journal_page_first 101
_journal_page_last 107
_journal_volume 11
_journal_year 2009
_chemical_formula_moiety 'C20 H16 N4 O4 Sn, 4(C3 H6 O2)'
_chemical_formula_sum 'C32 H40 N4 O12 Sn'
_chemical_formula_weight 791.37
_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 104.233(5)
_cell_angle_beta 98.682(5)
_cell_angle_gamma 92.148(5)
_cell_formula_units_Z 2
_cell_length_a 8.612(5)
_cell_length_b 13.909(5)
_cell_length_c 15.522(5)
_cell_measurement_reflns_used 14156
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 72.6915
_cell_measurement_theta_min 2.983
_cell_volume 1776.2(13)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 4.5
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type 'Bruker Smart 2K'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0576
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 5932
_diffrn_reflns_theta_full 72.48
_diffrn_reflns_theta_max 72.48
_diffrn_reflns_theta_min 2.98
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 6.288
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.4246
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.480
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 812
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_diff_density_max 1.803
_refine_diff_density_min -0.925
_refine_diff_density_rms 0.122
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 442
_refine_ls_number_reflns 5932
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.028
_refine_ls_R_factor_all 0.0693
_refine_ls_R_factor_gt 0.0543
_refine_ls_shift/su_max 0.063
_refine_ls_shift/su_mean 0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1436
_refine_ls_wR_factor_ref 0.1578
_reflns_number_gt 4938
_reflns_number_total 5932
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file deposit.cif
_cod_data_source_block jiw470
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1501552
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
Sn1 Sn -0.09291(4) 0.28672(2) 0.74435(2) 0.03882(16) Uani 1 1 d .
C1 C -0.2936(6) 0.3498(3) 0.6887(4) 0.0400(12) Uani 1 1 d .
C2 C -0.2736(7) 0.4042(4) 0.6288(4) 0.0455(13) Uani 1 1 d .
H2 H -0.1726 0.4169 0.6177 0.055 Uiso 1 1 calc .
N3 N -0.3981(6) 0.4407(3) 0.5845(3) 0.0487(11) Uani 1 1 d .
H3 H -0.3786 0.4759 0.5484 0.058 Uiso 1 1 calc .
C4 C -0.5513(7) 0.4248(4) 0.5940(4) 0.0455(13) Uani 1 1 d .
O4 O -0.6592(5) 0.4568(3) 0.5459(3) 0.0565(11) Uani 1 1 d .
C5 C -0.5753(7) 0.3709(4) 0.6589(4) 0.0490(14) Uani 1 1 d .
H5 H -0.6759 0.3607 0.6715 0.059 Uiso 1 1 calc .
C6 C -0.4507(7) 0.3343(4) 0.7021(4) 0.0451(13) Uani 1 1 d .
H6 H -0.4695 0.2974 0.7424 0.054 Uiso 1 1 calc .
C7 C 0.0614(6) 0.4020(3) 0.8393(4) 0.0396(12) Uani 1 1 d .
C8 C 0.2118(7) 0.3838(4) 0.8668(4) 0.0465(13) Uani 1 1 d .
H8 H 0.2462 0.3220 0.8419 0.056 Uiso 1 1 calc .
N9 N 0.3142(6) 0.4517(3) 0.9290(4) 0.0491(12) Uani 1 1 d .
H9A H 0.4086 0.4361 0.9432 0.059 Uiso 1 1 calc .
C10 C 0.2744(7) 0.5439(4) 0.9700(4) 0.0476(14) Uani 1 1 d .
O10 O 0.3760(5) 0.6011(3) 1.0295(3) 0.0642(12) Uani 1 1 d .
C11 C 0.1183(7) 0.5666(4) 0.9406(4) 0.0501(14) Uani 1 1 d .
H11 H 0.0861 0.6295 0.9639 0.060 Uiso 1 1 calc .
C12 C 0.0160(6) 0.4973(4) 0.8791(4) 0.0455(13) Uani 1 1 d .
H12 H -0.0864 0.5130 0.8627 0.055 Uiso 1 1 calc .
C13 C -0.1384(6) 0.1735(3) 0.8101(4) 0.0391(12) Uani 1 1 d .
C14 C -0.0464(6) 0.1726(3) 0.8893(4) 0.0413(12) Uani 1 1 d .
H14 H 0.0249 0.2267 0.9189 0.050 Uiso 1 1 calc .
N15 N -0.0578(5) 0.0927(3) 0.9261(3) 0.0417(10) Uani 1 1 d .
H15 H 0.0027 0.0948 0.9760 0.050 Uiso 1 1 calc .
C16 C -0.1593(6) 0.0102(4) 0.8880(4) 0.0405(12) Uani 1 1 d .
O16 O -0.1595(5) -0.0598(3) 0.9261(3) 0.0532(10) Uani 1 1 d .
C17 C -0.2577(7) 0.0111(4) 0.8060(4) 0.0475(14) Uani 1 1 d .
H17 H -0.3308 -0.0425 0.7778 0.057 Uiso 1 1 calc .
C18 C -0.2467(7) 0.0895(4) 0.7679(4) 0.0455(13) Uani 1 1 d .
H18 H -0.3111 0.0878 0.7137 0.055 Uiso 1 1 calc .
C19 C 0.0240(7) 0.2111(4) 0.6384(4) 0.0472(13) Uani 1 1 d .
C20 C 0.1330(8) 0.1485(4) 0.6560(4) 0.0522(14) Uani 1 1 d .
H20 H 0.1638 0.1454 0.7152 0.063 Uiso 1 1 calc .
N21 N 0.1999(6) 0.0895(4) 0.5896(3) 0.0594(13) Uani 1 1 d .
H21 H 0.2722 0.0529 0.6046 0.071 Uiso 1 1 calc .
C22 C 0.1573(10) 0.0860(5) 0.5010(5) 0.0706(19) Uani 1 1 d .
O22 O 0.2212(8) 0.0277(4) 0.4436(3) 0.0950(18) Uani 1 1 d .
C23 C 0.0448(11) 0.1535(7) 0.4810(5) 0.084(3) Uani 1 1 d .
H23 H 0.0140 0.1563 0.4217 0.101 Uiso 1 1 calc .
C24 C -0.0170(9) 0.2131(5) 0.5472(5) 0.0684(19) Uani 1 1 d .
H24 H -0.0890 0.2571 0.5325 0.082 Uiso 1 1 calc .
C25 C -0.4098(8) 0.3689(5) 1.1953(5) 0.0687(19) Uani 1 1 d .
H25A H -0.3512 0.4315 1.2244 0.103 Uiso 1 1 calc R
H25B H -0.3626 0.3354 1.1451 0.103 Uiso 1 1 calc R
H25C H -0.4088 0.3285 1.2374 0.103 Uiso 1 1 calc R
C26 C -0.5780(8) 0.3867(5) 1.1623(5) 0.0662(18) Uani 1 1 d .
H26A H -0.6221 0.4234 1.2134 0.079 Uiso 1 1 calc R
H26B H -0.5767 0.4285 1.1207 0.079 Uiso 1 1 calc R
C27 C -0.6860(8) 0.2944(4) 1.1159(4) 0.0523(15) Uani 1 1 d .
O28 O -0.7930(7) 0.2921(3) 1.0572(4) 0.0821(16) Uani 1 1 d .
O29 O -0.6491(5) 0.2174(3) 1.1476(3) 0.0644(12) Uani 1 1 d .
H29 H -0.7057 0.1681 1.1177 0.097 Uiso 1 1 calc .
C30 C -0.7019(9) -0.0078(5) 0.8337(5) 0.077(2) Uani 1 1 d .
H30A H -0.7305 -0.0689 0.8478 0.116 Uiso 1 1 calc R
H30B H -0.6530 -0.0222 0.7808 0.116 Uiso 1 1 calc R
H30C H -0.7947 0.0265 0.8229 0.116 Uiso 1 1 calc R
C31 C -0.5875(8) 0.0571(4) 0.9122(5) 0.0605(17) Uani 1 1 d .
H31A H -0.4944 0.0217 0.9226 0.073 Uiso 1 1 calc R
H31B H -0.6360 0.0684 0.9659 0.073 Uiso 1 1 calc R
C32 C -0.5375(8) 0.1568(4) 0.8979(4) 0.0519(15) Uani 1 1 d .
O33 O -0.5960(5) 0.1895(3) 0.8367(3) 0.0586(11) Uani 1 1 d .
O34 O -0.4216(6) 0.2051(3) 0.9637(3) 0.0649(12) Uani 1 1 d .
H34 H -0.4128 0.2638 0.9629 0.097 Uiso 1 1 calc .
C35 C -0.0110(12) 0.2529(7) 0.2592(6) 0.102(3) Uani 1 1 d .
H35A H 0.0712 0.2271 0.2268 0.153 Uiso 1 1 calc R
H35B H -0.1010 0.2606 0.2174 0.153 Uiso 1 1 calc R
H35C H -0.0401 0.2076 0.2928 0.153 Uiso 1 1 calc R
C36 C 0.0454(11) 0.3500(6) 0.3213(8) 0.106(3) Uani 1 1 d .
H36A H 0.0770 0.3945 0.2868 0.127 Uiso 1 1 calc R
H36B H 0.1381 0.3416 0.3621 0.127 Uiso 1 1 calc R
C37 C -0.0736(9) 0.3977(5) 0.3760(6) 0.072(2) Uani 1 1 d .
O38 O -0.1475(8) 0.3540(5) 0.4155(5) 0.106(2) Uani 1 1 d .
O39 O -0.0850(5) 0.4903(3) 0.3777(4) 0.0754(14) Uani 1 1 d .
H39 H -0.1500 0.5129 0.4093 0.113 Uiso 1 1 calc .
C40 C -0.5367(14) 0.2369(8) 0.3668(6) 0.120(4) Uani 1 1 d .
H40A H -0.5927 0.2960 0.3759 0.180 Uiso 1 1 calc R
H40B H -0.5942 0.1867 0.3171 0.180 Uiso 1 1 calc R
H40C H -0.4342 0.2517 0.3540 0.180 Uiso 1 1 calc R
C41 C -0.5221(17) 0.2046(7) 0.4394(7) 0.145(6) Uani 1 1 d .
H41A H -0.6279 0.1929 0.4508 0.174 Uiso 1 1 calc R
H41B H -0.4712 0.2593 0.4885 0.174 Uiso 1 1 calc R
C42 C -0.4383(11) 0.1154(5) 0.4480(5) 0.079(2) Uani 1 1 d .
O43 O -0.4120(6) 0.0533(3) 0.3837(3) 0.0751(14) Uani 1 1 d .
O44 O -0.3916(7) 0.1116(4) 0.5318(4) 0.0850(16) Uani 1 1 d .
H44 H -0.3016 0.0939 0.5371 0.128 Uiso 1 1 calc .
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
Sn1 0.0500(2) 0.0280(2) 0.0412(2) 0.01508(16) 0.00564(19) 0.00234(14)
C1 0.045(3) 0.029(2) 0.049(3) 0.019(2) 0.002(3) 0.007(2)
C2 0.051(3) 0.039(3) 0.050(3) 0.020(3) 0.006(3) 0.001(2)
N3 0.057(3) 0.039(2) 0.058(3) 0.027(2) 0.008(3) 0.007(2)
C4 0.050(3) 0.038(3) 0.048(3) 0.012(3) 0.005(3) 0.013(2)
O4 0.054(2) 0.061(3) 0.062(3) 0.027(2) 0.011(2) 0.015(2)
C5 0.053(3) 0.047(3) 0.056(4) 0.021(3) 0.023(3) 0.011(3)
C6 0.058(3) 0.037(3) 0.040(3) 0.012(2) 0.005(3) -0.004(2)
C7 0.049(3) 0.026(2) 0.042(3) 0.008(2) 0.002(3) -0.004(2)
C8 0.060(3) 0.028(2) 0.053(3) 0.013(2) 0.009(3) 0.001(2)
N9 0.053(3) 0.031(2) 0.060(3) 0.009(2) 0.004(3) -0.0003(19)
C10 0.057(3) 0.031(3) 0.053(4) 0.009(3) 0.006(3) -0.004(2)
O10 0.062(3) 0.038(2) 0.079(3) 0.001(2) -0.006(3) -0.0023(19)
C11 0.058(3) 0.034(3) 0.056(4) 0.008(3) 0.011(3) 0.004(2)
C12 0.050(3) 0.036(3) 0.053(3) 0.016(3) 0.011(3) 0.005(2)
C13 0.055(3) 0.024(2) 0.040(3) 0.014(2) 0.005(3) 0.001(2)
C14 0.050(3) 0.030(2) 0.045(3) 0.012(2) 0.008(3) 0.001(2)
N15 0.055(3) 0.034(2) 0.037(2) 0.0161(19) 0.002(2) 0.0002(19)
C16 0.049(3) 0.033(3) 0.040(3) 0.012(2) 0.006(3) -0.001(2)
O16 0.071(3) 0.0356(19) 0.056(3) 0.0227(18) 0.005(2) -0.0072(18)
C17 0.064(3) 0.032(3) 0.045(3) 0.011(2) 0.005(3) -0.008(2)
C18 0.063(3) 0.037(3) 0.036(3) 0.012(2) 0.005(3) 0.002(2)
C19 0.062(3) 0.039(3) 0.046(3) 0.018(3) 0.016(3) 0.007(2)
C20 0.073(4) 0.040(3) 0.043(3) 0.009(3) 0.011(3) 0.003(3)
N21 0.077(4) 0.057(3) 0.043(3) 0.007(2) 0.011(3) 0.024(3)
C22 0.098(6) 0.072(4) 0.041(4) 0.010(3) 0.013(4) 0.020(4)
O22 0.135(5) 0.101(4) 0.054(3) 0.013(3) 0.033(3) 0.045(4)
C23 0.112(7) 0.102(6) 0.046(4) 0.027(4) 0.013(5) 0.038(5)
C24 0.089(5) 0.076(5) 0.047(4) 0.024(3) 0.011(4) 0.024(4)
C25 0.073(4) 0.060(4) 0.068(5) 0.019(4) -0.004(4) -0.017(3)
C26 0.074(4) 0.048(3) 0.071(5) 0.010(3) 0.004(4) -0.011(3)
C27 0.070(4) 0.038(3) 0.049(4) 0.012(3) 0.008(4) 0.000(3)
O28 0.095(4) 0.054(3) 0.085(4) 0.024(3) -0.032(3) -0.007(3)
O29 0.082(3) 0.047(2) 0.061(3) 0.024(2) -0.012(2) -0.014(2)
C30 0.095(5) 0.049(4) 0.092(6) 0.017(4) 0.029(5) -0.001(4)
C31 0.082(4) 0.049(3) 0.059(4) 0.021(3) 0.027(4) 0.015(3)
C32 0.063(4) 0.042(3) 0.056(4) 0.014(3) 0.022(4) 0.013(3)
O33 0.077(3) 0.041(2) 0.062(3) 0.022(2) 0.009(3) 0.012(2)
O34 0.082(3) 0.049(2) 0.057(3) 0.011(2) -0.003(3) 0.003(2)
C35 0.116(7) 0.092(6) 0.100(7) 0.018(5) 0.036(6) 0.008(5)
C36 0.090(6) 0.072(5) 0.158(10) 0.009(6) 0.058(6) 0.012(4)
C37 0.071(4) 0.062(4) 0.086(6) 0.026(4) 0.004(4) 0.002(3)
O38 0.111(4) 0.113(5) 0.125(5) 0.068(4) 0.047(4) 0.026(4)
O39 0.069(3) 0.062(3) 0.098(4) 0.021(3) 0.020(3) 0.006(2)
C40 0.191(11) 0.128(8) 0.070(6) 0.050(6) 0.052(7) 0.097(8)
C41 0.287(16) 0.078(6) 0.123(8) 0.052(6) 0.137(10) 0.093(8)
C42 0.131(7) 0.048(4) 0.066(5) 0.012(4) 0.045(5) 0.019(4)
O43 0.114(4) 0.057(3) 0.058(3) 0.009(2) 0.028(3) 0.031(3)
O44 0.126(5) 0.062(3) 0.064(3) -0.003(3) 0.035(3) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 '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_publ_flag
C13 Sn1 C1 116.4(2) y
C13 Sn1 C19 102.64(19) y
C1 Sn1 C19 109.4(2) y
C13 Sn1 C7 107.7(2) y
C1 Sn1 C7 109.5(2) y
C19 Sn1 C7 111.1(2) y
C2 C1 C6 115.7(5) y
C2 C1 Sn1 117.8(4) y
C6 C1 Sn1 126.3(4) y
C1 C2 N3 121.7(5) y
C2 N3 C4 124.2(4) y
O4 C4 N3 119.4(5) y
O4 C4 C5 125.3(5) y
N3 C4 C5 115.3(5) y
C6 C5 C4 119.9(5) y
C5 C6 C1 123.2(5) y
C8 C7 C12 116.1(5) y
C8 C7 Sn1 119.4(4) y
C12 C7 Sn1 124.4(4) y
N9 C8 C7 122.7(5) y
C8 N9 C10 123.0(5) y
O10 C10 N9 118.6(5) y
O10 C10 C11 125.7(5) y
N9 C10 C11 115.7(5) y
C12 C11 C10 120.7(5) y
C11 C12 C7 121.7(5) y
C14 C13 C18 117.5(4) y
C14 C13 Sn1 119.8(4) y
C18 C13 Sn1 122.1(4) y
C13 C14 N15 120.8(5) y
C16 N15 C14 124.0(5) y
O16 C16 N15 119.3(5) y
O16 C16 C17 125.0(5) y
N15 C16 C17 115.7(4) y
C18 C17 C16 121.1(5) y
C17 C18 C13 121.0(5) y
C20 C19 C24 116.3(5) y
C20 C19 Sn1 119.0(4) y
C24 C19 Sn1 124.3(4) y
C19 C20 N21 122.2(6) y
C22 N21 C20 122.9(6) y
O22 C22 N21 119.2(7) y
O22 C22 C23 125.0(7) y
N21 C22 C23 115.8(6) y
C24 C23 C22 120.6(7) y
C23 C24 C19 122.1(6) y
C27 C26 C25 115.6(6) y
O28 C27 O29 123.8(6) y
O28 C27 C26 123.3(6) y
O29 C27 C26 112.9(6) y
C30 C31 C32 113.9(6) y
O33 C32 O34 124.3(5) y
O33 C32 C31 124.7(6) y
O34 C32 C31 111.0(6) y
C35 C36 C37 114.3(7) y
O38 C37 O39 123.7(8) y
O38 C37 C36 122.7(7) y
O39 C37 C36 113.6(7) y
C40 C41 C42 123.0(7) y
O43 C42 O44 123.2(7) y
O43 C42 C41 122.6(8) y
O44 C42 C41 114.2(7) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 C13 2.131(4) y
Sn1 C1 2.131(5) y
Sn1 C19 2.133(5) y
Sn1 C7 2.144(5) y
C1 C2 1.360(7) y
C1 C6 1.415(7) y
C2 N3 1.367(7) y
N3 C4 1.366(7) y
C4 O4 1.266(7) y
C4 C5 1.429(8) y
C5 C6 1.361(9) y
C7 C8 1.355(8) y
C7 C12 1.415(7) y
C8 N9 1.354(7) y
N9 C10 1.365(7) y
C10 O10 1.262(7) y
C10 C11 1.426(9) y
C11 C12 1.359(8) y
C13 C14 1.362(7) y
C13 C18 1.422(7) y
C14 N15 1.375(6) y
N15 C16 1.366(6) y
C16 O16 1.258(6) y
C16 C17 1.421(8) y
C17 C18 1.370(7) y
C19 C20 1.347(8) y
C19 C24 1.415(8) y
C20 N21 1.366(7) y
N21 C22 1.357(8) y
C22 O22 1.258(8) y
C22 C23 1.427(11) y
C23 C24 1.344(10) y
C25 C26 1.513(10) y
C26 C27 1.512(9) y
C27 O28 1.188(8) y
C27 O29 1.314(7) y
C30 C31 1.516(10) y
C31 C32 1.514(8) y
C32 O33 1.203(7) y
C32 O34 1.340(8) y
C35 C36 1.469(11) y
C36 C37 1.499(11) y
C37 O38 1.192(9) y
C37 O39 1.290(8) y
C40 C41 1.302(11) y
C41 C42 1.483(11) y
C42 O43 1.205(8) y
C42 O44 1.316(9) y
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 H3 O4 0.86 1.98 2.836(6) 173.6 2_466
N9 H9A O10 0.86 1.96 2.817(7) 177.7 2_667
N15 H15 O16 0.86 2.04 2.874(6) 163.2 2_557
N21 H21 O43 0.86 1.97 2.811(7) 167.4 2_556
O29 H29 O16 0.82 1.79 2.599(5) 168.4 2_457
O34 H34 O10 0.82 1.87 2.683(6) 174.3 2_567
O39 H39 O4 0.82 1.90 2.698(6) 163.7 2_466
O44 H44 O22 0.82 1.92 2.541(8) 131.3 2_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_publ_flag
C13 Sn1 C1 C2 -164.8(4) y
C19 Sn1 C1 C2 -49.2(5) y
C7 Sn1 C1 C2 72.8(5) y
C13 Sn1 C1 C6 9.7(5) y
C19 Sn1 C1 C6 125.4(5) y
C7 Sn1 C1 C6 -112.7(5) y
C6 C1 C2 N3 -0.3(8) y
Sn1 C1 C2 N3 174.8(4) y
C1 C2 N3 C4 -1.5(9) y
C2 N3 C4 O4 -175.7(5) y
C2 N3 C4 C5 3.5(8) y
O4 C4 C5 C6 175.4(6) y
N3 C4 C5 C6 -3.8(8) y
C4 C5 C6 C1 2.3(9) y
C2 C1 C6 C5 -0.1(8) y
Sn1 C1 C6 C5 -174.8(5) y
C13 Sn1 C7 C8 68.3(5) y
C1 Sn1 C7 C8 -164.3(4) y
C19 Sn1 C7 C8 -43.4(5) y
C13 Sn1 C7 C12 -109.5(4) y
C1 Sn1 C7 C12 17.9(5) y
C19 Sn1 C7 C12 138.9(4) y
C12 C7 C8 N9 0.4(8) y
Sn1 C7 C8 N9 -177.6(4) y
C7 C8 N9 C10 0.7(9) y
C8 N9 C10 O10 177.5(5) y
C8 N9 C10 C11 -2.5(8) y
O10 C10 C11 C12 -176.7(6) y
N9 C10 C11 C12 3.3(8) y
C10 C11 C12 C7 -2.4(9) y
C8 C7 C12 C11 0.5(8) y
Sn1 C7 C12 C11 178.4(4) y
C1 Sn1 C13 C14 -137.9(4) y
C19 Sn1 C13 C14 102.7(4) y
C7 Sn1 C13 C14 -14.6(5) y
C1 Sn1 C13 C18 51.7(5) y
C19 Sn1 C13 C18 -67.7(5) y
C7 Sn1 C13 C18 175.0(4) y
C18 C13 C14 N15 0.7(8) y
Sn1 C13 C14 N15 -170.2(4) y
C13 C14 N15 C16 -0.4(8) y
C14 N15 C16 O16 179.0(5) y
C14 N15 C16 C17 -0.7(8) y
O16 C16 C17 C18 -178.2(6) y
N15 C16 C17 C18 1.4(8) y
C16 C17 C18 C13 -1.2(9) y
C14 C13 C18 C17 0.1(8) y
Sn1 C13 C18 C17 170.7(4) y
C13 Sn1 C19 C20 -41.9(5) y
C1 Sn1 C19 C20 -166.0(4) y
C7 Sn1 C19 C20 73.0(5) y
C13 Sn1 C19 C24 130.8(5) y
C1 Sn1 C19 C24 6.6(6) y
C7 Sn1 C19 C24 -114.4(5) y
C24 C19 C20 N21 -0.6(9) y
Sn1 C19 C20 N21 172.7(4) y
C19 C20 N21 C22 -2.9(10) y
C20 N21 C22 O22 -178.0(7) y
C20 N21 C22 C23 4.2(11) y
O22 C22 C23 C24 -180.0(8) y
N21 C22 C23 C24 -2.3(13) y
C22 C23 C24 C19 -0.9(14) y
C20 C19 C24 C23 2.4(11) y
Sn1 C19 C24 C23 -170.4(7) y
C25 C26 C27 O28 -148.6(7) y
C25 C26 C27 O29 31.5(8) y
C30 C31 C32 O33 9.6(9) y
C30 C31 C32 O34 -171.9(5) y
C35 C36 C37 O38 48.3(14) y
C35 C36 C37 O39 -133.3(9) y
C40 C41 C42 O43 -19(2) y
C40 C41 C42 O44 159.5(13) y
|
1501553.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501553.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_1501553
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C10 H24 Ag Cl O4 S4'
_chemical_formula_weight 479.85
_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 93.6910(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.0656(2)
_cell_length_b 21.8175(4)
_cell_length_c 10.5558(2)
_cell_measurement_reflns_used 13930
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.43
_cell_measurement_theta_min 4.05
_cell_volume 1853.66(7)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.035
_diffrn_reflns_av_sigmaI/netI 0.0176
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 22802
_diffrn_reflns_theta_full 68.42
_diffrn_reflns_theta_max 68.42
_diffrn_reflns_theta_min 4.05
_diffrn_standards_decay_% 5.36
_diffrn_standards_number 136
_exptl_absorpt_coefficient_mu 14.339
_exptl_absorpt_correction_T_max 0.3210
_exptl_absorpt_correction_T_min 0.1160
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.719
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 976
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.08
_refine_diff_density_max 1.096
_refine_diff_density_min -0.597
_refine_diff_density_rms 0.090
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 181
_refine_ls_number_reflns 3339
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.098
_refine_ls_R_factor_all 0.0292
_refine_ls_R_factor_gt 0.0277
_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^)+(0.0522P)^2^+1.0279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0784
_refine_ls_wR_factor_ref 0.0796
_reflns_number_gt 3125
_reflns_number_total 3339
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande57
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501553
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
Ag1 Ag 0.39145(2) 0.630248(9) 0.60900(2) 0.02641(10) Uani 1 1 d .
Cl1 Cl 0.80847(9) 0.87259(3) 0.52380(7) 0.03235(17) Uani 1 1 d .
S1 S 0.68968(8) 0.63896(3) 0.54897(6) 0.02367(15) Uani 1 1 d .
S2 S 0.21621(8) 0.62006(3) 0.38630(6) 0.02247(15) Uani 1 1 d .
S3 S 0.29008(8) 0.54195(3) 0.73789(6) 0.02383(15) Uani 1 1 d .
S4 S 0.30662(7) 0.73538(3) 0.70191(6) 0.02082(14) Uani 1 1 d .
O1 O 0.9087(5) 0.9052(2) 0.6168(4) 0.1015(15) Uani 1 1 d .
O2 O 0.6683(4) 0.85218(17) 0.5835(4) 0.0952(14) Uani 1 1 d .
O3 O 0.9025(3) 0.82234(11) 0.4810(2) 0.0453(6) Uani 1 1 d .
O4 O 0.7745(6) 0.9133(2) 0.4236(4) 0.1055(15) Uani 1 1 d .
C11 C 0.6924(4) 0.68210(18) 0.4036(3) 0.0452(9) Uani 1 1 d .
H11A H 0.6416 0.7224 0.4153 0.068 Uiso 1 1 calc R
H11B H 0.6295 0.6600 0.3355 0.068 Uiso 1 1 calc R
H11C H 0.8074 0.6874 0.3810 0.068 Uiso 1 1 calc R
C12 C 0.8032(3) 0.69087(12) 0.6575(3) 0.0241(5) Uani 1 1 d .
H12A H 0.7591 0.7329 0.6452 0.029 Uiso 1 1 calc R
H12B H 0.7872 0.6784 0.7460 0.029 Uiso 1 1 calc R
C13 C 0.9870(3) 0.69037(12) 0.6351(2) 0.0225(5) Uani 1 1 d .
H13A H 1.0025 0.7035 0.5468 0.027 Uiso 1 1 calc R
H13B H 1.0300 0.6480 0.6453 0.027 Uiso 1 1 calc R
C21 C 0.0703(4) 0.55899(14) 0.4101(3) 0.0345(7) Uani 1 1 d .
H21A H 0.0078 0.5498 0.3297 0.052 Uiso 1 1 calc R
H21B H -0.0068 0.5717 0.4732 0.052 Uiso 1 1 calc R
H21C H 0.1307 0.5223 0.4404 0.052 Uiso 1 1 calc R
C22 C 0.3343(3) 0.58429(12) 0.2657(2) 0.0241(5) Uani 1 1 d .
H22A H 0.2556 0.5676 0.1985 0.029 Uiso 1 1 calc R
H22B H 0.4016 0.6162 0.2264 0.029 Uiso 1 1 calc R
C23 C 0.4496(3) 0.53289(12) 0.3138(2) 0.0251(6) Uani 1 1 d .
H23A H 0.5338 0.5493 0.3773 0.030 Uiso 1 1 calc R
H23B H 0.3848 0.5010 0.3555 0.030 Uiso 1 1 calc R
C31 C 0.2279(5) 0.57120(16) 0.8877(3) 0.0445(8) Uani 1 1 d .
H31A H 0.1944 0.5371 0.9406 0.067 Uiso 1 1 calc R
H31B H 0.1342 0.5994 0.8724 0.067 Uiso 1 1 calc R
H31C H 0.3213 0.5930 0.9312 0.067 Uiso 1 1 calc R
C32 C 0.4643(3) 0.49526(12) 0.7962(2) 0.0245(5) Uani 1 1 d .
H32A H 0.5444 0.5208 0.8479 0.029 Uiso 1 1 calc R
H32B H 0.4247 0.4623 0.8512 0.029 Uiso 1 1 calc R
C41 C 0.0859(3) 0.73255(12) 0.7264(2) 0.0232(5) Uani 1 1 d .
H41A H 0.0713 0.7187 0.8143 0.028 Uiso 1 1 calc R
H41B H 0.0398 0.7745 0.7176 0.028 Uiso 1 1 calc R
C42 C 0.3034(4) 0.77998(13) 0.5577(3) 0.0283(6) Uani 1 1 d .
H42A H 0.2577 0.7551 0.4864 0.042 Uiso 1 1 calc R
H42B H 0.4167 0.7926 0.5418 0.042 Uiso 1 1 calc R
H42C H 0.2339 0.8164 0.5666 0.042 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
Ag1 0.01753(15) 0.02378(14) 0.03848(15) 0.00350(7) 0.00616(9) 0.00009(6)
Cl1 0.0317(4) 0.0298(4) 0.0365(4) -0.0037(3) 0.0093(3) 0.0053(3)
S1 0.0141(3) 0.0295(3) 0.0277(3) -0.0019(3) 0.0034(2) -0.0035(2)
S2 0.0198(3) 0.0200(3) 0.0279(3) -0.0001(2) 0.0035(2) 0.0006(2)
S3 0.0210(3) 0.0219(3) 0.0291(3) 0.0014(2) 0.0057(2) -0.0005(2)
S4 0.0168(3) 0.0235(3) 0.0220(3) -0.0013(2) 0.0000(2) -0.0026(2)
O1 0.088(3) 0.114(3) 0.101(3) -0.059(3) -0.001(2) -0.031(2)
O2 0.063(2) 0.074(2) 0.157(4) -0.029(2) 0.071(2) -0.0181(17)
O3 0.0465(14) 0.0443(13) 0.0468(14) 0.0008(11) 0.0158(11) 0.0191(10)
O4 0.135(4) 0.092(3) 0.090(3) 0.033(2) 0.011(2) 0.067(3)
C11 0.0364(19) 0.071(2) 0.0277(16) 0.0111(15) -0.0044(13) -0.0208(16)
C12 0.0191(14) 0.0284(14) 0.0250(13) -0.0025(10) 0.0041(10) -0.0009(10)
C13 0.0163(13) 0.0249(13) 0.0261(13) -0.0029(10) 0.0007(10) 0.0010(10)
C21 0.0298(16) 0.0325(16) 0.0423(17) -0.0045(13) 0.0103(12) -0.0089(12)
C22 0.0248(14) 0.0242(13) 0.0236(13) 0.0020(10) 0.0045(10) 0.0005(10)
C23 0.0286(15) 0.0233(13) 0.0237(13) 0.0016(10) 0.0038(10) 0.0044(11)
C31 0.054(2) 0.0414(18) 0.0407(18) 0.0039(14) 0.0233(15) 0.0145(15)
C32 0.0240(14) 0.0252(13) 0.0245(13) 0.0009(10) 0.0032(10) 0.0021(10)
C41 0.0190(14) 0.0268(13) 0.0241(13) -0.0043(10) 0.0027(10) -0.0018(10)
C42 0.0293(15) 0.0265(14) 0.0292(14) 0.0041(11) 0.0032(11) -0.0052(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S3 Ag1 S1 . . 122.52(2) y
S3 Ag1 S4 . . 111.55(2) y
S1 Ag1 S4 . . 107.75(2) y
S3 Ag1 S2 . . 103.84(2) y
S1 Ag1 S2 . . 104.07(2) y
S4 Ag1 S2 . . 105.52(2) y
O4 Cl1 O2 . . 114.7(3) y
O4 Cl1 O1 . . 106.3(3) y
O2 Cl1 O1 . . 106.7(3) y
O4 Cl1 O3 . . 109.4(2) y
O2 Cl1 O3 . . 111.07(19) y
O1 Cl1 O3 . . 108.3(2) y
C11 S1 C12 . . 100.26(15) y
C11 S1 Ag1 . . 108.41(12) y
C12 S1 Ag1 . . 109.72(9) y
C21 S2 C22 . . 99.01(13) y
C21 S2 Ag1 . . 104.56(11) y
C22 S2 Ag1 . . 112.39(9) y
C31 S3 C32 . . 98.89(15) y
C31 S3 Ag1 . . 108.66(12) y
C32 S3 Ag1 . . 109.95(9) y
C42 S4 C41 . . 100.21(13) y
C42 S4 Ag1 . . 98.46(10) y
C41 S4 Ag1 . . 107.91(9) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 110.83(18) y
C13 C12 H12A . . 109.5 ?
S1 C12 H12A . . 109.5 ?
C13 C12 H12B . . 109.5 ?
S1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108.1 ?
C12 C13 C41 . 1_655 112.0(2) y
C12 C13 H13A . . 109.2 ?
C41 C13 H13A 1_655 . 109.2 ?
C12 C13 H13B . . 109.2 ?
C41 C13 H13B 1_655 . 109.2 ?
H13A C13 H13B . . 107.9 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C23 C22 S2 . . 114.81(18) y
C23 C22 H22A . . 108.6 ?
S2 C22 H22A . . 108.6 ?
C23 C22 H22B . . 108.6 ?
S2 C22 H22B . . 108.6 ?
H22A C22 H22B . . 107.5 ?
C32 C23 C22 3_666 . 110.0(2) y
C32 C23 H23A 3_666 . 109.7 ?
C22 C23 H23A . . 109.7 ?
C32 C23 H23B 3_666 . 109.7 ?
C22 C23 H23B . . 109.7 ?
H23A C23 H23B . . 108.2 ?
S3 C31 H31A . . 109.5 ?
S3 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
S3 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C23 C32 S3 3_666 . 110.50(18) y
C23 C32 H32A 3_666 . 109.6 ?
S3 C32 H32A . . 109.6 ?
C23 C32 H32B 3_666 . 109.6 ?
S3 C32 H32B . . 109.6 ?
H32A C32 H32B . . 108.1 ?
C13 C41 S4 1_455 . 114.16(18) y
C13 C41 H41A 1_455 . 108.7 ?
S4 C41 H41A . . 108.7 ?
C13 C41 H41B 1_455 . 108.7 ?
S4 C41 H41B . . 108.7 ?
H41A C41 H41B . . 107.6 ?
S4 C42 H42A . . 109.5 ?
S4 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
S4 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 S3 . 2.5247(6) y
Ag1 S1 . 2.5338(7) y
Ag1 S4 . 2.6034(6) y
Ag1 S2 . 2.6731(7) y
Cl1 O4 . 1.396(4) y
Cl1 O2 . 1.402(3) y
Cl1 O1 . 1.421(3) y
Cl1 O3 . 1.423(2) y
S1 C11 . 1.801(3) y
S1 C12 . 1.816(3) y
S2 C21 . 1.806(3) y
S2 C22 . 1.815(3) y
S3 C31 . 1.806(3) y
S3 C32 . 1.811(3) y
S4 C42 . 1.805(3) y
S4 C41 . 1.816(3) y
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.516(4) y
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 C41 1_655 1.522(3) y
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 C23 . 1.523(4) y
C22 H22A . 0.99 ?
C22 H22B . 0.99 ?
C23 C32 3_666 1.520(4) y
C23 H23A . 0.99 ?
C23 H23B . 0.99 ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 C23 3_666 1.520(4) y
C32 H32A . 0.99 ?
C32 H32B . 0.99 ?
C41 C13 1_455 1.522(3) y
C41 H41A . 0.99 ?
C41 H41B . 0.99 ?
C42 H42A . 0.98 ?
C42 H42B . 0.98 ?
C42 H42C . 0.98 ?
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_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S3 Ag1 S1 C11 . 152.56(14) y
S4 Ag1 S1 C11 . -76.04(14) y
S2 Ag1 S1 C11 . 35.67(14) y
S3 Ag1 S1 C12 . -98.86(10) y
S4 Ag1 S1 C12 . 32.54(10) y
S2 Ag1 S1 C12 . 144.25(10) y
S3 Ag1 S2 C21 . 6.01(11) y
S1 Ag1 S2 C21 . 135.24(11) y
S4 Ag1 S2 C21 . -111.44(11) y
S3 Ag1 S2 C22 . -100.37(10) y
S1 Ag1 S2 C22 . 28.86(10) y
S4 Ag1 S2 C22 . 142.18(9) y
S1 Ag1 S3 C31 . 115.37(14) y
S4 Ag1 S3 C31 . -14.46(14) y
S2 Ag1 S3 C31 . -127.64(14) y
S1 Ag1 S3 C32 . 8.14(10) y
S4 Ag1 S3 C32 . -121.68(9) y
S2 Ag1 S3 C32 . 125.14(9) y
S3 Ag1 S4 C42 . -153.59(10) y
S1 Ag1 S4 C42 . 69.26(10) y
S2 Ag1 S4 C42 . -41.46(10) y
S3 Ag1 S4 C41 . -49.91(9) y
S1 Ag1 S4 C41 . 172.93(9) y
S2 Ag1 S4 C41 . 62.22(9) y
C11 S1 C12 C13 . -73.7(2) y
Ag1 S1 C12 C13 . 172.35(16) y
S1 C12 C13 C41 1_655 -178.89(18) y
C21 S2 C22 C23 . -72.7(2) y
Ag1 S2 C22 C23 . 37.2(2) y
S2 C22 C23 C32 3_666 177.50(18) y
C31 S3 C32 C23 3_666 -176.5(2) y
Ag1 S3 C32 C23 3_666 -62.8(2) y
C42 S4 C41 C13 1_455 73.2(2) y
Ag1 S4 C41 C13 1_455 -29.2(2) y
|
1501554.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501554.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_1501554
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C10 H24 Ag B F4 S4'
_chemical_formula_weight 467.21
_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 92.324(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.0371(2)
_cell_length_b 21.6514(6)
_cell_length_c 10.4766(3)
_cell_measurement_reflns_used 2739
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 67.96
_cell_measurement_theta_min 4.08
_cell_volume 1821.58(9)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.075
_diffrn_reflns_av_sigmaI/netI 0.0708
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 24468
_diffrn_reflns_theta_full 68.60
_diffrn_reflns_theta_max 68.60
_diffrn_reflns_theta_min 4.08
_diffrn_standards_decay_% -3.81
_diffrn_standards_number 17
_exptl_absorpt_coefficient_mu 13.401
_exptl_absorpt_correction_T_max 0.1340
_exptl_absorpt_correction_T_min 0.1200
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.704
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle-like
_exptl_crystal_F_000 944
_exptl_crystal_size_max 0.13
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.973
_refine_diff_density_min -0.619
_refine_diff_density_rms 0.149
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.905
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 185
_refine_ls_number_reflns 3347
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.905
_refine_ls_R_factor_all 0.0550
_refine_ls_R_factor_gt 0.0401
_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^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0887
_refine_ls_wR_factor_ref 0.0930
_reflns_number_gt 2511
_reflns_number_total 3347
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande61
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1501554
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
Ag1 Ag 0.11351(4) 0.630262(16) 0.38656(4) 0.01314(12) Uani 1 1 d .
S1 S 0.28145(14) 0.62130(5) 0.61055(12) 0.0112(3) Uani 1 1 d .
S2 S -0.18856(14) 0.63790(5) 0.44474(12) 0.0117(3) Uani 1 1 d .
S3 S 0.21920(15) 0.54040(5) 0.26000(12) 0.0123(3) Uani 1 1 d .
S4 S 0.19759(14) 0.73665(5) 0.29505(12) 0.0105(3) Uani 1 1 d .
F1 F 0.8271(4) 0.65267(17) 0.9035(4) 0.0393(10) Uani 1 1 d .
F2 F 0.6019(4) 0.67946(14) 1.0144(3) 0.0266(8) Uani 1 1 d .
F3 F 0.5878(5) 0.59795(19) 0.8794(4) 0.0498(11) Uani 1 1 d .
F4 F 0.7397(5) 0.59095(17) 1.0631(4) 0.0463(11) Uani 1 1 d .
C11 C 0.1600(6) 0.5860(2) 0.7332(5) 0.0123(11) Uani 1 1 d .
H11A H 0.2374 0.5696 0.8008 0.015 Uiso 1 1 calc R
H11B H 0.0918 0.6185 0.7723 0.015 Uiso 1 1 calc R
C12 C 0.4287(7) 0.5591(2) 0.5880(5) 0.0188(12) Uani 1 1 d .
H12A H 0.4881 0.5500 0.6694 0.028 Uiso 1 1 calc R
H12B H 0.5088 0.5715 0.5248 0.028 Uiso 1 1 calc R
H12C H 0.3687 0.5222 0.5577 0.028 Uiso 1 1 calc R
C21 C -0.1957(7) 0.6823(3) 0.5910(5) 0.0246(14) Uani 1 1 d .
H21A H -0.1468 0.7231 0.5778 0.037 Uiso 1 1 calc R
H21B H -0.1324 0.6608 0.6594 0.037 Uiso 1 1 calc R
H21C H -0.3116 0.6869 0.6149 0.037 Uiso 1 1 calc R
C23 C -0.2993(6) 0.6895(2) 0.3345(5) 0.0121(11) Uani 1 1 d .
H23A H -0.2535 0.7318 0.3443 0.015 Uiso 1 1 calc R
H23B H -0.2825 0.6759 0.2457 0.015 Uiso 1 1 calc R
C24 C -0.4847(6) 0.6905(2) 0.3586(5) 0.0115(11) Uani 1 1 d .
H24A H -0.5300 0.6482 0.3489 0.014 Uiso 1 1 calc R
H24B H -0.5009 0.7039 0.4476 0.014 Uiso 1 1 calc R
C31 C 0.0432(6) 0.4943(2) 0.2013(5) 0.0117(10) Uani 1 1 d .
H31A H -0.0355 0.5206 0.1506 0.014 Uiso 1 1 calc R
H31B H 0.0827 0.4611 0.1450 0.014 Uiso 1 1 calc R
C32 C -0.0450(6) 0.4660(2) 0.3128(5) 0.0126(11) Uani 1 1 d .
H32A H -0.1107 0.4982 0.3551 0.015 Uiso 1 1 calc R
H32B H 0.0386 0.4497 0.3762 0.015 Uiso 1 1 calc R
C34 C 0.2933(8) 0.5673(3) 0.1089(6) 0.0296(15) Uani 1 1 d .
H34A H 0.3213 0.5317 0.0560 0.044 Uiso 1 1 calc R
H34B H 0.3927 0.5929 0.1243 0.044 Uiso 1 1 calc R
H34C H 0.2062 0.5918 0.0647 0.044 Uiso 1 1 calc R
C41 C 0.2003(6) 0.7814(2) 0.4413(5) 0.0151(11) Uani 1 1 d .
H41A H 0.2417 0.7556 0.5127 0.023 Uiso 1 1 calc R
H41B H 0.0873 0.7955 0.4575 0.023 Uiso 1 1 calc R
H41C H 0.2735 0.8172 0.4329 0.023 Uiso 1 1 calc R
C42 C 0.4201(6) 0.7332(2) 0.2684(5) 0.0121(11) Uani 1 1 d .
H42A H 0.4360 0.7193 0.1797 0.015 Uiso 1 1 calc R
H42B H 0.4672 0.7752 0.2773 0.015 Uiso 1 1 calc R
B1 B 0.6893(7) 0.6301(3) 0.9662(6) 0.0173(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
Ag1 0.00926(18) 0.00980(18) 0.0206(2) -0.00168(16) 0.00405(13) -0.00004(16)
S1 0.0122(5) 0.0076(5) 0.0139(7) -0.0003(5) 0.0025(5) -0.0006(5)
S2 0.0077(5) 0.0129(6) 0.0147(7) 0.0015(5) 0.0029(5) 0.0023(5)
S3 0.0130(6) 0.0087(5) 0.0155(7) -0.0010(5) 0.0050(5) 0.0007(5)
S4 0.0091(5) 0.0104(6) 0.0121(6) 0.0016(5) 0.0009(5) 0.0014(5)
F1 0.0245(18) 0.042(2) 0.053(3) -0.0012(19) 0.0238(18) -0.0023(17)
F2 0.0318(18) 0.0229(17) 0.026(2) -0.0029(14) 0.0106(15) 0.0105(15)
F3 0.051(3) 0.049(2) 0.049(3) -0.019(2) -0.005(2) -0.016(2)
F4 0.061(3) 0.039(2) 0.039(3) 0.0147(19) 0.005(2) 0.025(2)
C11 0.016(3) 0.013(2) 0.008(3) -0.003(2) 0.001(2) 0.005(2)
C12 0.022(3) 0.018(3) 0.017(3) 0.004(2) 0.005(2) 0.000(2)
C21 0.023(3) 0.039(3) 0.013(3) -0.003(3) 0.002(2) 0.016(3)
C23 0.013(2) 0.012(2) 0.012(3) 0.000(2) 0.004(2) 0.000(2)
C24 0.013(2) 0.010(2) 0.012(3) 0.001(2) 0.003(2) 0.000(2)
C31 0.015(2) 0.008(2) 0.013(3) 0.000(2) 0.004(2) 0.000(2)
C32 0.019(3) 0.010(2) 0.009(3) -0.0028(19) 0.004(2) 0.001(2)
C34 0.033(3) 0.021(3) 0.036(4) -0.002(3) 0.018(3) -0.011(3)
C41 0.017(3) 0.016(3) 0.012(3) -0.002(2) 0.000(2) 0.003(2)
C42 0.018(3) 0.010(2) 0.009(3) 0.003(2) 0.004(2) -0.001(2)
B1 0.018(3) 0.019(3) 0.016(3) 0.001(3) 0.005(2) 0.003(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S3 Ag1 S2 . . 121.58(4) y
S3 Ag1 S4 . . 113.10(4) y
S2 Ag1 S4 . . 107.31(4) y
S3 Ag1 S1 . . 103.73(4) y
S2 Ag1 S1 . . 104.42(4) y
S4 Ag1 S1 . . 105.05(4) y
C11 S1 C12 . . 98.8(2) y
C11 S1 Ag1 . . 112.73(17) y
C12 S1 Ag1 . . 104.43(19) y
C21 S2 C23 . . 100.4(2) y
C21 S2 Ag1 . . 107.55(19) y
C23 S2 Ag1 . . 109.71(16) y
C34 S3 C31 . . 99.2(3) y
C34 S3 Ag1 . . 110.0(2) y
C31 S3 Ag1 . . 109.13(16) y
C41 S4 C42 . . 100.0(2) y
C41 S4 Ag1 . . 98.98(17) y
C42 S4 Ag1 . . 106.95(16) y
C32 C11 S1 3_566 . 115.1(3) y
C32 C11 H11A 3_566 . 108.5 ?
S1 C11 H11A . . 108.5 ?
C32 C11 H11B 3_566 . 108.5 ?
S1 C11 H11B . . 108.5 ?
H11A C11 H11B . . 107.5 ?
S1 C12 H12A . . 109.5 ?
S1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
S1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C24 C23 S2 . . 111.2(3) y
C24 C23 H23A . . 109.4 ?
S2 C23 H23A . . 109.4 ?
C24 C23 H23B . . 109.4 ?
S2 C23 H23B . . 109.4 ?
H23A C23 H23B . . 108 ?
C42 C24 C23 1_455 . 112.4(4) y
C42 C24 H24A 1_455 . 109.1 ?
C23 C24 H24A . . 109.1 ?
C42 C24 H24B 1_455 . 109.1 ?
C23 C24 H24B . . 109.1 ?
H24A C24 H24B . . 107.9 ?
C32 C31 S3 . . 110.0(4) y
C32 C31 H31A . . 109.7 ?
S3 C31 H31A . . 109.7 ?
C32 C31 H31B . . 109.7 ?
S3 C31 H31B . . 109.7 ?
H31A C31 H31B . . 108.2 ?
C31 C32 C11 . 3_566 110.5(4) y
C31 C32 H32A . . 109.5 ?
C11 C32 H32A 3_566 . 109.5 ?
C31 C32 H32B . . 109.5 ?
C11 C32 H32B 3_566 . 109.5 ?
H32A C32 H32B . . 108.1 ?
S3 C34 H34A . . 109.5 ?
S3 C34 H34B . . 109.5 ?
H34A C34 H34B . . 109.5 ?
S3 C34 H34C . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 109.5 ?
S4 C41 H41A . . 109.5 ?
S4 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
S4 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C24 C42 S4 1_655 . 113.9(3) y
C24 C42 H42A 1_655 . 108.8 ?
S4 C42 H42A . . 108.8 ?
C24 C42 H42B 1_655 . 108.8 ?
S4 C42 H42B . . 108.8 ?
H42A C42 H42B . . 107.7 ?
F4 B1 F2 . . 110.3(5) y
F4 B1 F3 . . 108.9(5) y
F2 B1 F3 . . 109.5(5) y
F4 B1 F1 . . 110.3(5) y
F2 B1 F1 . . 108.9(5) y
F3 B1 F1 . . 108.9(5) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 S3 . 2.5212(12) y
Ag1 S2 . 2.5324(12) y
Ag1 S4 . 2.5951(12) y
Ag1 S1 . 2.6663(13) y
S1 C11 . 1.814(5) y
S1 C12 . 1.815(5) y
S2 C21 . 1.812(6) y
S2 C23 . 1.814(5) y
S3 C34 . 1.810(6) y
S3 C31 . 1.818(5) y
S4 C41 . 1.812(5) y
S4 C42 . 1.822(5) y
F1 B1 . 1.399(7) y
F2 B1 . 1.385(7) y
F3 B1 . 1.385(7) y
F4 B1 . 1.371(7) y
C11 C32 3_566 1.523(7) y
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C23 C24 . 1.522(6) y
C23 H23A . 0.99 ?
C23 H23B . 0.99 ?
C24 C42 1_455 1.507(7) y
C24 H24A . 0.99 ?
C24 H24B . 0.99 ?
C31 C32 . 1.520(6) y
C31 H31A . 0.99 ?
C31 H31B . 0.99 ?
C32 C11 3_566 1.523(7) y
C32 H32A . 0.99 ?
C32 H32B . 0.99 ?
C34 H34A . 0.98 ?
C34 H34B . 0.98 ?
C34 H34C . 0.98 ?
C41 H41A . 0.98 ?
C41 H41B . 0.98 ?
C41 H41C . 0.98 ?
C42 C24 1_655 1.507(7) y
C42 H42A . 0.99 ?
C42 H42B . 0.99 ?
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_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S3 Ag1 S1 C11 . -100.20(17) y
S2 Ag1 S1 C11 . 28.08(17) y
S4 Ag1 S1 C11 . 140.86(17) y
S3 Ag1 S1 C12 . 5.96(18) y
S2 Ag1 S1 C12 . 134.24(18) y
S4 Ag1 S1 C12 . -112.98(18) y
S3 Ag1 S2 C21 . 152.3(2) y
S4 Ag1 S2 C21 . -75.3(2) y
S1 Ag1 S2 C21 . 35.8(2) y
S3 Ag1 S2 C23 . -99.39(18) y
S4 Ag1 S2 C23 . 32.99(18) y
S1 Ag1 S2 C23 . 144.14(18) y
S2 Ag1 S3 C34 . 117.0(2) y
S4 Ag1 S3 C34 . -12.9(2) y
S1 Ag1 S3 C34 . -126.2(2) y
S2 Ag1 S3 C31 . 9.15(18) y
S4 Ag1 S3 C31 . -120.79(17) y
S1 Ag1 S3 C31 . 125.96(17) y
S3 Ag1 S4 C41 . -152.11(17) y
S2 Ag1 S4 C41 . 71.07(18) y
S1 Ag1 S4 C41 . -39.65(18) y
S3 Ag1 S4 C42 . -48.71(18) y
S2 Ag1 S4 C42 . 174.46(17) y
S1 Ag1 S4 C42 . 63.74(18) y
C12 S1 C11 C32 3_566 -72.8(4) y
Ag1 S1 C11 C32 3_566 36.9(4) y
C21 S2 C23 C24 . -72.3(4) y
Ag1 S2 C23 C24 . 174.6(3) y
S2 C23 C24 C42 1_455 179.9(3) y
C34 S3 C31 C32 . -179.4(4) y
Ag1 S3 C31 C32 . -64.4(3) y
S3 C31 C32 C11 3_566 -164.3(3) y
C41 S4 C42 C24 1_655 73.1(4) y
Ag1 S4 C42 C24 1_655 -29.6(4) y
|
1501555.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501555.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_1501555
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_absolute_configuration rmad
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C9 H18 Ag F3 O4 S3'
_chemical_formula_weight 451.28
_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 8.0541(2)
_cell_length_b 9.6501(2)
_cell_length_c 21.0990(5)
_cell_measurement_reflns_used 6496
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 68.30
_cell_measurement_theta_min 4.19
_cell_volume 1639.87(7)
_computing_cell_refinement 'SMART (Bruker, 2003)'
_computing_data_collection 'SMART (Bruker, 2003)'
_computing_data_reduction 'SAINT (Bruker, 2004)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker Smart 6000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator 'Montel 200 optics'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.045
_diffrn_reflns_av_sigmaI/netI 0.0363
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 21431
_diffrn_reflns_theta_full 68.40
_diffrn_reflns_theta_max 68.40
_diffrn_reflns_theta_min 4.19
_diffrn_standards_decay_% -1.94
_diffrn_standards_number 104
_exptl_absorpt_coefficient_mu 13.816
_exptl_absorpt_correction_T_max 0.4200
_exptl_absorpt_correction_T_min 0.1230
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.828
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle-like
_exptl_crystal_F_000 904
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.07
_refine_diff_density_max 1.234
_refine_diff_density_min -1.154
_refine_diff_density_rms 0.147
_refine_ls_abs_structure_details 'Flack H D (1983), XXXX Friedel Pairs'
_refine_ls_abs_structure_Flack -0.023(16)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 185
_refine_ls_number_reflns 2988
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0450
_refine_ls_R_factor_gt 0.0395
_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^)+(0.0819P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1165
_refine_ls_wR_factor_ref 0.1193
_reflns_number_gt 2670
_reflns_number_total 2988
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande45
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_cell_volume 1639.88(7)
_cod_original_sg_symbol_H-M P212121
_cod_database_code 1501555
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
Ag1 Ag 0.95873(5) 0.63810(4) 0.00249(3) 0.02884(16) Uani 1 1 d .
S1 S 1.15225(18) 0.83435(16) 0.03846(7) 0.0230(3) Uani 1 1 d .
S2 S 0.5471(2) 1.10485(17) 0.02269(8) 0.0304(4) Uani 1 1 d .
S3 S 0.6718(2) 0.7013(2) 0.14405(9) 0.0329(4) Uani 1 1 d .
F1 F 0.7169(7) 0.5666(7) 0.2501(2) 0.0613(15) Uani 1 1 d .
F2 F 0.4711(6) 0.6493(6) 0.2377(2) 0.0566(14) Uani 1 1 d .
F3 F 0.5454(8) 0.4686(6) 0.1866(3) 0.0632(14) Uani 1 1 d .
O1 O 0.7972(6) 0.6173(7) 0.1139(3) 0.0454(15) Uani 1 1 d .
O2 O 0.7318(8) 0.8215(7) 0.1762(3) 0.0547(16) Uani 1 1 d .
O3 O 0.5234(7) 0.7232(7) 0.1069(2) 0.0473(15) Uani 1 1 d .
O4 O 0.8684(9) 0.7328(7) 0.3778(3) 0.0571(17) Uani 1 1 d .
C1 C 0.5971(10) 0.5890(9) 0.2078(4) 0.0380(18) Uani 1 1 d .
C11 C 1.1509(9) 0.8464(9) 0.1240(3) 0.0344(16) Uani 1 1 d .
H11A H 1.1910 0.9381 0.1369 0.052 Uiso 1 1 calc R
H11B H 1.2234 0.7748 0.1418 0.052 Uiso 1 1 calc R
H11C H 1.0374 0.8331 0.1396 0.052 Uiso 1 1 calc R
C12 C 1.0445(8) 0.9930(7) 0.0156(3) 0.0291(15) Uani 1 1 d .
H12A H 1.0977 1.0732 0.0367 0.035 Uiso 1 1 calc R
H12B H 1.0544 1.0062 -0.0308 0.035 Uiso 1 1 calc R
C13 C 0.8623(8) 0.9876(8) 0.0337(4) 0.0346(16) Uani 1 1 d .
H13A H 0.8112 0.9041 0.0147 0.042 Uiso 1 1 calc R
H13B H 0.8528 0.9797 0.0803 0.042 Uiso 1 1 calc R
C14 C 0.7689(8) 1.1145(7) 0.0118(4) 0.0323(16) Uani 1 1 d .
H14A H 0.7923 1.1294 -0.0337 0.039 Uiso 1 1 calc R
H14B H 0.8114 1.1961 0.0352 0.039 Uiso 1 1 calc R
C21 C 0.5274(10) 1.1165(9) 0.1073(4) 0.0426(19) Uani 1 1 d .
H21A H 0.5761 1.0339 0.1269 0.064 Uiso 1 1 calc R
H21B H 0.4096 1.1227 0.1187 0.064 Uiso 1 1 calc R
H21C H 0.5856 1.1993 0.1225 0.064 Uiso 1 1 calc R
C31 C 1.0661(14) 0.7461(12) 0.2964(5) 0.066(3) Uani 1 1 d .
H31A H 1.0823 0.6475 0.3057 0.099 Uiso 1 1 calc R
H31B H 1.1688 0.7968 0.3054 0.099 Uiso 1 1 calc R
H31C H 1.0369 0.7576 0.2516 0.099 Uiso 1 1 calc R
C32 C 0.9298(10) 0.8014(8) 0.3367(3) 0.0373(18) Uani 1 1 d .
C33 C 0.8721(14) 0.9454(9) 0.3229(5) 0.060(3) Uani 1 1 d .
H33A H 0.7979 0.9442 0.2860 0.090 Uiso 1 1 calc R
H33B H 0.9682 1.0044 0.3138 0.090 Uiso 1 1 calc R
H33C H 0.8123 0.9819 0.3597 0.090 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
Ag1 0.0175(2) 0.0270(3) 0.0420(3) -0.0027(2) -0.0009(2) 0.00058(17)
S1 0.0135(7) 0.0257(9) 0.0297(8) -0.0013(6) 0.0006(6) -0.0009(6)
S2 0.0206(8) 0.0242(8) 0.0463(9) 0.0017(7) -0.0020(7) 0.0034(6)
S3 0.0250(9) 0.0437(10) 0.0300(9) 0.0065(8) 0.0022(7) 0.0038(8)
F1 0.053(3) 0.083(4) 0.048(3) 0.020(3) -0.010(2) 0.008(3)
F2 0.041(3) 0.078(4) 0.051(3) 0.007(3) 0.021(2) 0.009(3)
F3 0.059(3) 0.051(3) 0.080(4) -0.002(3) 0.002(3) -0.015(3)
O1 0.025(3) 0.069(4) 0.041(3) 0.000(3) 0.008(2) 0.016(3)
O2 0.061(4) 0.045(4) 0.059(4) 0.005(3) 0.004(3) -0.012(3)
O3 0.019(3) 0.083(5) 0.040(3) 0.012(3) 0.000(2) 0.016(3)
O4 0.065(5) 0.056(4) 0.051(4) 0.016(3) 0.009(3) 0.001(3)
C1 0.033(4) 0.044(5) 0.037(4) 0.001(3) 0.003(3) 0.002(3)
C11 0.027(4) 0.043(4) 0.033(4) 0.001(3) 0.004(3) 0.001(4)
C12 0.016(3) 0.028(3) 0.044(4) 0.002(3) 0.005(3) -0.003(3)
C13 0.021(3) 0.036(4) 0.047(4) 0.004(3) -0.004(3) -0.003(3)
C14 0.020(3) 0.030(4) 0.047(5) 0.003(3) -0.001(3) -0.005(3)
C21 0.028(4) 0.042(5) 0.058(5) -0.013(4) 0.008(4) 0.000(4)
C31 0.063(7) 0.072(7) 0.062(6) 0.004(5) 0.007(5) -0.002(6)
C32 0.039(5) 0.038(4) 0.035(4) 0.003(3) -0.009(3) -0.012(4)
C33 0.066(7) 0.038(5) 0.076(7) 0.016(5) -0.018(5) -0.008(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 Ag1 S1 4_565 . 125.47(5) y
S2 Ag1 S1 4_565 4_465 106.94(6) y
S1 Ag1 S1 . 4_465 126.34(3) y
C11 S1 C12 . . 101.9(3) y
C11 S1 Ag1 . . 109.8(3) y
C12 S1 Ag1 . . 104.6(2) y
C11 S1 Ag1 . 4_565 109.1(2) y
C12 S1 Ag1 . 4_565 105.9(2) y
Ag1 S1 Ag1 . 4_565 123.19(6) y
C21 S2 C14 . . 102.2(4) y
C21 S2 Ag1 . 4_465 104.1(3) y
C14 S2 Ag1 . 4_465 107.6(2) y
O2 S3 O1 . . 115.4(4) y
O2 S3 O3 . . 114.7(4) y
O1 S3 O3 . . 115.0(3) y
O2 S3 C1 . . 104.1(4) y
O1 S3 C1 . . 102.8(4) y
O3 S3 C1 . . 102.4(4) y
F3 C1 F2 . . 107.9(7) y
F3 C1 F1 . . 108.3(7) y
F2 C1 F1 . . 107.8(6) y
F3 C1 S3 . . 112.2(6) y
F2 C1 S3 . . 109.9(6) y
F1 C1 S3 . . 110.6(6) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 111.4(5) y
C13 C12 H12A . . 109.4 ?
S1 C12 H12A . . 109.4 ?
C13 C12 H12B . . 109.4 ?
S1 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108 ?
C14 C13 C12 . . 112.2(6) y
C14 C13 H13A . . 109.2 ?
C12 C13 H13A . . 109.2 ?
C14 C13 H13B . . 109.2 ?
C12 C13 H13B . . 109.2 ?
H13A C13 H13B . . 107.9 ?
C13 C14 S2 . . 114.4(5) y
C13 C14 H14A . . 108.7 ?
S2 C14 H14A . . 108.7 ?
C13 C14 H14B . . 108.7 ?
S2 C14 H14B . . 108.7 ?
H14A C14 H14B . . 107.6 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C32 C31 H31A . . 109.5 ?
C32 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C32 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
O4 C32 C31 . . 121.4(8) y
O4 C32 C33 . . 121.8(9) y
C31 C32 C33 . . 116.9(8) y
C32 C33 H33A . . 109.5 ?
C32 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C32 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 S2 4_565 2.5070(17) y
Ag1 S1 . 2.5675(15) y
Ag1 S1 4_465 2.6288(15) y
S1 C11 . 1.808(7) y
S1 C12 . 1.825(7) y
S1 Ag1 4_565 2.6288(15) y
S2 C21 . 1.796(8) y
S2 C14 . 1.804(7) y
S2 Ag1 4_465 2.5070(17) y
S3 O2 . 1.429(7) y
S3 O1 . 1.443(6) y
S3 O3 . 1.445(5) y
S3 C1 . 1.829(8) y
F1 C1 . 1.332(9) y
F2 C1 . 1.330(9) y
F3 C1 . 1.314(10) y
O4 C32 . 1.198(9) y
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.517(9) y
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 C14 . 1.51(1) y
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C31 C32 . 1.487(13) y
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 C33 . 1.494(12) y
C33 H33A . 0.98 ?
C33 H33B . 0.98 ?
C33 H33C . 0.98 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S2 Ag1 S1 C11 4_565 . -95.8(3) y
S1 Ag1 S1 C11 4_465 . 98.7(3) y
S2 Ag1 S1 C12 4_565 . 155.5(2) y
S1 Ag1 S1 C12 4_465 . -10.0(2) y
S2 Ag1 S1 Ag1 4_565 4_565 34.87(10) y
S1 Ag1 S1 Ag1 4_465 4_565 -130.64(9) y
O2 S3 C1 F3 . . -176.4(6) y
O1 S3 C1 F3 . . -55.7(7) y
O3 S3 C1 F3 . . 63.9(6) y
O2 S3 C1 F2 . . 63.6(6) y
O1 S3 C1 F2 . . -175.7(5) y
O3 S3 C1 F2 . . -56.2(6) y
O2 S3 C1 F1 . . -55.3(7) y
O1 S3 C1 F1 . . 65.3(6) y
O3 S3 C1 F1 . . -175.1(6) y
C11 S1 C12 C13 . . -68.7(6) y
Ag1 S1 C12 C13 . . 45.7(5) y
Ag1 S1 C12 C13 4_565 . 177.2(5) y
S1 C12 C13 C14 . . -176.7(5) y
C12 C13 C14 S2 . . 172.4(5) y
C21 S2 C14 C13 . . 70.5(6) y
Ag1 S2 C14 C13 4_465 . -38.8(6) y
|
1501556.cif | #------------------------------------------------------------------------------
#$Date: 2020-10-02 18:11:04 +0300 (Fri, 02 Oct 2020) $
#$Revision: 256942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/15/1501556.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_1501556
loop_
_publ_author_name
'Mohamed Osman Awaleh'
'Francois Brisse'
'Youssouf Djibril Soubaneh'
'Thierry Maris'
_publ_section_title
;
Influence of the counteranion on silver(I)-dithioether coordination
polymers
;
_journal_name_full Polyhedron
_journal_page_first 2966
_journal_page_last 2975
_journal_paper_doi 10.1016/j.poly.2010.08.013
_journal_volume 29
_journal_year 2010
_chemical_compound_source 'Synthesized by the authors. See text'
_chemical_formula_sum 'C5 H12 Ag F6 S2 Sb'
_chemical_formula_weight 479.89
_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 100.5040(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 18.1075(4)
_cell_length_b 7.9194(2)
_cell_length_c 18.0488(4)
_cell_measurement_reflns_used 4986
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 72.98
_cell_measurement_theta_min 4.98
_cell_volume 2544.83(10)
_computing_cell_refinement 'SMART (Bruker, 1999)'
_computing_data_collection 'SMART (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_molecular_graphics 'SHELXTL (Bruker, 1997)'
_computing_publication_material 'UdMX (local program)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 200(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker Smart 2000'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray Sealed Tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.052
_diffrn_reflns_av_sigmaI/netI 0.0463
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 15460
_diffrn_reflns_theta_full 73.04
_diffrn_reflns_theta_max 73.04
_diffrn_reflns_theta_min 4.97
_diffrn_standards_decay_% -0.26
_diffrn_standards_number 110
_exptl_absorpt_coefficient_mu 32.721
_exptl_absorpt_correction_T_max 0.1030
_exptl_absorpt_correction_T_min 0.0710
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.505
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle-like
_exptl_crystal_F_000 1808
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.07
_refine_diff_density_max 2.309
_refine_diff_density_min -1.624
_refine_diff_density_rms 0.232
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.115
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 130
_refine_ls_number_reflns 2529
_refine_ls_number_restraints 36
_refine_ls_restrained_S_all 1.181
_refine_ls_R_factor_all 0.0532
_refine_ls_R_factor_gt 0.0467
_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^)+(0.0867P)^2^+1.0005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1333
_refine_ls_wR_factor_ref 0.1369
_reflns_number_gt 2144
_reflns_number_total 2529
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file deposit.cif
_cod_data_source_block ande55
_cod_depositor_comments
;
Updated values of the _geom_bond_atom_site_label_*,
_geom_angle_atom_site_label_* and _geom_torsion_atom_site_label
data items to establish relationships between loop packets from
different data loops.
Antanas Vaitkus,
2020-10-02
;
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1501556
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
Ag1 Ag 0.30591(3) 0.90505(7) 0.28718(3) 0.0317(2) Uani 1 1 d .
Sb1 Sb 0.37739(3) 0.55910(7) 0.11037(3) 0.0293(2) Uani 1 1 d .
S1 S 0.22982(11) 1.0941(2) 0.18637(10) 0.0249(4) Uani 1 1 d .
S2 S 0.07128(11) 0.4918(3) 0.13347(12) 0.0335(5) Uani 1 1 d .
F1 F 0.3657(4) 0.7209(9) 0.1824(4) 0.0654(18) Uani 1 1 d U
F2 F 0.4027(5) 0.3982(10) 0.1849(4) 0.077(2) Uani 1 1 d U
F3 F 0.3846(4) 0.3934(8) 0.0389(4) 0.0584(16) Uani 1 1 d U
F4 F 0.3444(4) 0.7129(9) 0.0350(4) 0.0719(19) Uani 1 1 d U
F5 F 0.4761(4) 0.6195(11) 0.1147(5) 0.089(2) Uani 1 1 d U
F6 F 0.2777(4) 0.4951(10) 0.1069(5) 0.076(2) Uani 1 1 d U
C11 C 0.2768(7) 1.0809(14) 0.1064(7) 0.059(2) Uani 1 1 d .
H11A H 0.2753 0.9640 0.0883 0.088 Uiso 1 1 calc R
H11B H 0.3292 1.1168 0.1216 0.088 Uiso 1 1 calc R
H11C H 0.2514 1.1545 0.0661 0.088 Uiso 1 1 calc R
C12 C 0.1401(4) 0.9940(10) 0.1511(4) 0.0264(16) Uani 1 1 d .
H12A H 0.1037 1.0265 0.1833 0.032 Uiso 1 1 calc R
H12B H 0.1206 1.0350 0.0994 0.032 Uiso 1 1 calc R
C13 C 0.1466(4) 0.8033(10) 0.1499(5) 0.0305(17) Uani 1 1 d .
H13A H 0.1797 0.7704 0.1143 0.037 Uiso 1 1 calc R
H13B H 0.1701 0.7631 0.2007 0.037 Uiso 1 1 calc R
C14 C 0.0715(5) 0.7195(11) 0.1268(7) 0.049(3) Uani 1 1 d .
H14A H 0.0510 0.7515 0.0740 0.059 Uiso 1 1 calc R
H14B H 0.0369 0.7649 0.1585 0.059 Uiso 1 1 calc R
C21 C 0.0983(8) 0.4548(15) 0.0403(6) 0.059(2) Uani 1 1 d .
H21A H 0.0615 0.5084 0.0008 0.088 Uiso 1 1 calc R
H21B H 0.0997 0.3331 0.0307 0.088 Uiso 1 1 calc R
H21C H 0.1481 0.5035 0.0402 0.088 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
Ag1 0.0351(4) 0.0226(3) 0.0322(3) -0.0016(2) -0.0078(2) 0.0007(2)
Sb1 0.0290(3) 0.0307(3) 0.0290(3) -0.00017(19) 0.0069(2) 0.0054(2)
S1 0.0282(9) 0.0175(9) 0.0257(8) -0.0009(6) -0.0035(7) -0.0010(7)
S2 0.0253(9) 0.0253(10) 0.0445(11) -0.0024(8) -0.0074(8) -0.0044(8)
F1 0.077(3) 0.061(3) 0.059(3) -0.016(3) 0.013(3) 0.015(3)
F2 0.100(4) 0.070(3) 0.059(3) 0.009(3) 0.008(3) 0.019(3)
F3 0.070(3) 0.055(3) 0.051(3) -0.013(2) 0.013(2) 0.003(3)
F4 0.087(4) 0.064(3) 0.065(3) 0.018(3) 0.015(3) 0.012(3)
F5 0.066(3) 0.088(4) 0.114(4) -0.014(3) 0.017(3) -0.003(3)
F6 0.060(3) 0.078(4) 0.096(4) 0.000(3) 0.029(3) -0.006(3)
C11 0.077(6) 0.052(5) 0.046(4) 0.004(3) 0.008(4) 0.004(4)
C12 0.028(4) 0.024(4) 0.024(4) 0.001(3) -0.004(3) 0.002(3)
C13 0.023(4) 0.020(4) 0.044(5) -0.004(3) -0.006(3) 0.003(3)
C14 0.035(5) 0.026(5) 0.076(7) 0.011(4) -0.021(5) -0.005(4)
C21 0.077(6) 0.052(5) 0.046(4) 0.004(3) 0.008(4) 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 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 Ag1 S1 4 . 123.50(7) y
S2 Ag1 S1 4 4_545 112.13(7) y
S1 Ag1 S1 . 4_545 124.26(4) y
F5 Sb1 F4 . . 92.4(4) y
F5 Sb1 F2 . . 92.2(4) y
F4 Sb1 F2 . . 175.4(4) y
F5 Sb1 F3 . . 91.3(3) y
F4 Sb1 F3 . . 90.5(3) y
F2 Sb1 F3 . . 88.8(3) y
F5 Sb1 F1 . . 91.4(3) y
F4 Sb1 F1 . . 89.9(3) y
F2 Sb1 F1 . . 90.7(3) y
F3 Sb1 F1 . . 177.3(3) y
F5 Sb1 F6 . . 179.2(4) y
F4 Sb1 F6 . . 88.5(4) y
F2 Sb1 F6 . . 87.0(4) y
F3 Sb1 F6 . . 88.6(3) y
F1 Sb1 F6 . . 88.7(3) y
C11 S1 C12 . . 102.5(5) y
C11 S1 Ag1 . . 105.3(4) y
C12 S1 Ag1 . . 109.0(2) y
C11 S1 Ag1 . 4 111.7(4) y
C12 S1 Ag1 . 4 103.9(3) y
Ag1 S1 Ag1 . 4 122.78(7) y
C14 S2 C21 . . 95.3(5) y
C14 S2 Ag1 . 4_545 107.4(3) y
C21 S2 Ag1 . 4_545 96.9(4) y
S1 C11 H11A . . 109.5 ?
S1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
S1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 S1 . . 111.9(5) y
C13 C12 H12A . . 109.2 ?
S1 C12 H12A . . 109.2 ?
C13 C12 H12B . . 109.2 ?
S1 C12 H12B . . 109.2 ?
H12A C12 H12B . . 107.9 ?
C14 C13 C12 . . 112.0(7) y
C14 C13 H13A . . 109.2 ?
C12 C13 H13A . . 109.2 ?
C14 C13 H13B . . 109.2 ?
C12 C13 H13B . . 109.2 ?
H13A C13 H13B . . 107.9 ?
C13 C14 S2 . . 115.8(6) y
C13 C14 H14A . . 108.3 ?
S2 C14 H14A . . 108.3 ?
C13 C14 H14B . . 108.3 ?
S2 C14 H14B . . 108.3 ?
H14A C14 H14B . . 107.4 ?
S2 C21 H21A . . 109.5 ?
S2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
S2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 S2 4 2.511(2) y
Ag1 S1 . 2.5567(18) y
Ag1 S1 4_545 2.6120(19) y
Sb1 F5 . 1.838(8) y
Sb1 F4 . 1.843(7) y
Sb1 F2 . 1.848(7) y
Sb1 F3 . 1.861(6) y
Sb1 F1 . 1.864(6) y
Sb1 F6 . 1.865(7) y
S1 C11 . 1.806(12) y
S1 C12 . 1.816(8) y
S1 Ag1 4 2.6120(19) y
S2 C14 . 1.807(9) y
S2 C21 . 1.859(12) y
S2 Ag1 4_545 2.511(2) y
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.515(11) y
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
C13 C14 . 1.503(11) y
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S2 Ag1 S1 C11 4 . 77.7(4) y
S1 Ag1 S1 C11 4_545 . -98.0(4) y
S2 Ag1 S1 C12 4 . -173.0(3) y
S1 Ag1 S1 C12 4_545 . 11.3(3) y
S2 Ag1 S1 Ag1 4 4 -51.36(12) y
S1 Ag1 S1 Ag1 4_545 4 132.86(11) y
C11 S1 C12 C13 . . 77.3(7) y
Ag1 S1 C12 C13 . . -33.8(6) y
Ag1 S1 C12 C13 4 . -166.3(5) y
S1 C12 C13 C14 . . 175.3(7) y
C12 C13 C14 S2 . . -173.4(7) y
C21 S2 C14 C13 . . -84.0(9) y
Ag1 S2 C14 C13 4_545 . 15.0(9) y
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