file_name stringlengths 11 11 | content stringlengths 1.16k 56.6M |
|---|---|
1101193.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101193.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_1101193
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4 H11 N O7 P2 V'
_chemical_formula_weight 298.02
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.401(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.2895(15)
_cell_length_b 13.4657(16)
_cell_length_c 6.0846(7)
_cell_measurement_temperature 90(2)
_cell_volume 979.5(2)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.021
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101193
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
V1 V 0.28394(5) 0.36543(5) 1.10959(10) 0.00656(19) Uani 1 1 d . . .
P1 P 0.38941(8) 0.35477(7) 0.65957(16) 0.0072(2) Uani 1 1 d . . .
P2 P 0.25094(8) 0.61154(7) 1.02593(17) 0.0094(2) Uani 1 1 d . . .
O1 O 0.3955(2) 0.2580(2) 1.1687(5) 0.0093(5) Uani 1 1 d . . .
O2 O 0.3254(2) 0.3961(2) 1.4314(5) 0.0103(5) Uani 1 1 d . . .
O3 O 0.1677(2) 0.3080(2) 1.0457(5) 0.0120(6) Uani 1 1 d . . .
O4 O 0.3376(2) 0.4008(2) 0.8432(5) 0.0106(5) Uani 1 1 d . . .
O5 O 0.2244(2) 0.5060(2) 1.0871(5) 0.0085(5) Uani 1 1 d . . .
O6 O 0.2119(3) 0.6753(2) 1.2096(5) 0.0158(6) Uani 1 1 d . . .
H6 H 0.2107 0.7356 1.1737 0.024 Uiso 1 1 calc R . .
O7 O 0.1934(3) 0.6421(2) 0.7876(5) 0.0153(6) Uani 1 1 d . . .
N1 N 0.1057(3) 0.5156(3) 0.4417(6) 0.0115(6) Uani 1 1 d . . .
H1A H 0.1451 0.5482 0.5681 0.014 Uiso 1 1 calc R . .
H1B H 0.1515 0.5093 0.3424 0.014 Uiso 1 1 calc R . .
C1 C 0.5311(3) 0.3987(3) 0.7070(7) 0.0112(7) Uani 1 1 d . . .
H1C H 0.5657 0.3718 0.5879 0.013 Uiso 1 1 calc R . .
H1D H 0.5306 0.4720 0.6947 0.013 Uiso 1 1 calc R . .
C2 C 0.3975(3) 0.6315(3) 1.0608(7) 0.0119(7) Uani 1 1 d . . .
H2A H 0.4233 0.5935 0.9430 0.014 Uiso 1 1 calc R . .
H2B H 0.4103 0.7028 1.0361 0.014 Uiso 1 1 calc R . .
C3 C 0.0049(3) 0.5752(3) 0.3338(7) 0.0152(8) Uani 1 1 d . . .
H3A H -0.0351 0.5423 0.1926 0.018 Uiso 1 1 calc R . .
H3B H 0.0284 0.6419 0.2946 0.018 Uiso 1 1 calc R . .
C4 C 0.0731(3) 0.4147(3) 0.5070(7) 0.0128(8) Uani 1 1 d . . .
H4A H 0.1408 0.3772 0.5821 0.015 Uiso 1 1 calc R . .
H4B H 0.0352 0.3776 0.3702 0.015 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
V1 0.0057(3) 0.0046(3) 0.0090(3) 0.0000(2) 0.0009(2) 0.0000(2)
P1 0.0065(4) 0.0059(4) 0.0090(4) 0.0000(3) 0.0011(3) -0.0006(3)
P2 0.0095(5) 0.0064(4) 0.0120(5) 0.0001(3) 0.0019(3) -0.0005(3)
O1 0.0094(12) 0.0059(12) 0.0122(13) 0.0007(10) 0.0021(10) 0.0015(10)
O2 0.0121(13) 0.0093(13) 0.0092(12) -0.0002(10) 0.0017(10) 0.0014(10)
O3 0.0098(13) 0.0075(13) 0.0175(14) 0.0003(10) 0.0004(10) -0.0014(10)
O4 0.0140(13) 0.0078(12) 0.0109(12) 0.0005(10) 0.0048(10) 0.0025(10)
O5 0.0071(12) 0.0056(12) 0.0127(12) 0.0011(10) 0.0018(10) 0.0002(9)
O6 0.0210(15) 0.0084(13) 0.0194(15) -0.0022(11) 0.0074(12) 0.0022(12)
O7 0.0204(15) 0.0097(14) 0.0140(14) 0.0027(10) 0.0003(11) -0.0007(11)
N1 0.0084(15) 0.0116(15) 0.0151(15) -0.0005(12) 0.0040(12) -0.0015(12)
C1 0.0088(17) 0.0112(18) 0.0133(17) 0.0010(14) 0.0017(14) -0.0030(14)
C2 0.0039(16) 0.0155(19) 0.0150(18) 0.0023(14) -0.0006(13) -0.0007(14)
C3 0.0129(19) 0.016(2) 0.0167(19) 0.0039(15) 0.0045(15) 0.0006(15)
C4 0.0078(17) 0.0090(18) 0.022(2) 0.0022(14) 0.0042(14) 0.0018(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.592(3) . ?
V1 O4 1.945(3) . ?
V1 O2 1.950(3) . ?
V1 O1 1.968(3) . ?
V1 O5 2.022(3) . ?
P1 O1 1.521(3) 4_565 ?
P1 O2 1.533(3) 1_554 ?
P1 O4 1.539(3) . ?
P1 C1 1.798(4) . ?
P2 O7 1.515(3) . ?
P2 O5 1.523(3) . ?
P2 O6 1.570(3) . ?
P2 C2 1.784(4) . ?
O1 P1 1.521(3) 4_566 ?
O2 P1 1.533(3) 1_556 ?
O6 H6 0.8400 . ?
N1 C3 1.494(5) . ?
N1 C4 1.496(5) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C1 C2 1.535(5) 3_667 ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C1 1.535(5) 3_667 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.518(6) 3_566 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C3 1.518(6) 3_566 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
|
1101194.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101194.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_1101194
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C6 H15 N O7 P2 V'
_chemical_formula_weight 326.07
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 98.7300(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.6046(10)
_cell_length_b 13.4811(9)
_cell_length_c 6.0678(4)
_cell_measurement_temperature 90(2)
_cell_volume 1180.82(14)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.834
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101194
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
V1 V 0.23571(4) 0.86561(5) 1.06952(11) 0.00435(17) Uani 1 1 d . . .
P1 P 0.20769(7) 1.11209(7) 0.98854(17) 0.0068(2) Uani 1 1 d . . .
P2 P 0.32297(7) 0.85398(7) 0.60225(16) 0.0048(2) Uani 1 1 d . . .
O1 O 0.1527(2) 1.1444(2) 0.7701(5) 0.0104(6) Uani 1 1 d . . .
O2 O 0.1848(2) 1.1753(2) 1.1901(5) 0.0118(6) Uani 1 1 d . . .
H2 H 0.1870 1.1389 1.3031 0.018 Uiso 1 1 calc R . .
O3 O 0.1876(2) 1.0065(2) 1.0569(5) 0.0068(5) Uani 1 1 d . . .
O4 O 0.1392(2) 0.8090(2) 1.0207(5) 0.0109(6) Uani 1 1 d . . .
O5 O 0.2826(2) 0.9011(2) 0.7969(5) 0.0089(6) Uani 1 1 d . . .
O6 O 0.2676(2) 0.8953(2) 1.3871(5) 0.0084(6) Uani 1 1 d . . .
O7 O 0.32788(19) 0.7584(2) 1.1130(4) 0.0058(5) Uani 1 1 d . . .
N1 N 0.0889(2) 1.0156(3) 0.4311(6) 0.0091(7) Uani 1 1 d . . .
H1A H 0.1285 1.0083 0.3277 0.011 Uiso 1 1 calc R . .
H1B H 0.1198 1.0498 0.5510 0.011 Uiso 1 1 calc R . .
C1 C 0.4399(3) 0.8979(3) 0.6170(7) 0.0093(7) Uani 1 1 d . . .
H1C H 0.4643 0.8755 0.4818 0.011 Uiso 1 1 calc R . .
H1D H 0.4390 0.9713 0.6151 0.011 Uiso 1 1 calc R . .
C2 C 0.5063(3) 0.8638(3) 0.8210(7) 0.0131(8) Uani 1 1 d . . .
H2A H 0.5069 0.7904 0.8259 0.016 Uiso 1 1 calc R . .
H2B H 0.4837 0.8880 0.9572 0.016 Uiso 1 1 calc R . .
C3 C 0.6046(3) 0.9013(3) 0.8198(7) 0.0113(8) Uani 1 1 d . . .
H3A H 0.6272 0.8767 0.6841 0.014 Uiso 1 1 calc R . .
H3B H 0.6037 0.9747 0.8133 0.014 Uiso 1 1 calc R . .
C4 C 0.3285(3) 1.1315(3) 0.9759(7) 0.0113(8) Uani 1 1 d . . .
H4A H 0.3444 1.0957 0.8444 0.014 Uiso 1 1 calc R . .
H4B H 0.3384 1.2031 0.9517 0.014 Uiso 1 1 calc R . .
C5 C 0.0620(3) 0.9158(3) 0.5056(7) 0.0105(8) Uani 1 1 d . . .
H5A H 0.1179 0.8799 0.5767 0.013 Uiso 1 1 calc R . .
H5B H 0.0332 0.8768 0.3751 0.013 Uiso 1 1 calc R . .
C6 C -0.0055(3) 0.9263(3) 0.6700(7) 0.0113(8) Uani 1 1 d . . .
H6A H -0.0250 0.8598 0.7137 0.014 Uiso 1 1 calc R . .
H6B H 0.0252 0.9605 0.8058 0.014 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
V1 0.0051(3) 0.0035(3) 0.0044(3) -0.0001(2) 0.0005(2) 0.0002(2)
P1 0.0075(5) 0.0056(4) 0.0069(4) 0.0008(3) 0.0000(3) 0.0000(3)
P2 0.0052(4) 0.0047(4) 0.0045(4) -0.0001(3) 0.0011(3) -0.0005(3)
O1 0.0121(14) 0.0086(13) 0.0092(13) 0.0015(10) -0.0023(11) -0.0003(11)
O2 0.0177(15) 0.0078(13) 0.0102(14) -0.0010(11) 0.0035(12) 0.0015(11)
O3 0.0092(13) 0.0047(12) 0.0066(12) 0.0003(10) 0.0018(10) 0.0006(10)
O4 0.0093(14) 0.0085(13) 0.0146(14) 0.0004(11) 0.0012(11) -0.0001(11)
O5 0.0141(14) 0.0060(13) 0.0070(13) -0.0002(10) 0.0027(11) 0.0029(10)
O6 0.0113(14) 0.0082(13) 0.0064(12) 0.0006(10) 0.0035(10) 0.0056(11)
O7 0.0056(13) 0.0068(12) 0.0054(12) -0.0008(10) 0.0015(10) 0.0007(10)
N1 0.0084(16) 0.0097(16) 0.0092(15) 0.0005(12) 0.0017(13) 0.0002(12)
C1 0.0078(18) 0.0083(17) 0.0115(18) -0.0024(14) 0.0008(14) -0.0010(14)
C2 0.0075(19) 0.017(2) 0.015(2) 0.0043(15) 0.0012(15) -0.0026(15)
C3 0.0080(18) 0.0116(19) 0.0142(19) 0.0032(15) 0.0006(15) -0.0026(14)
C4 0.0104(18) 0.0105(18) 0.0132(19) 0.0011(15) 0.0024(15) -0.0021(15)
C5 0.0079(18) 0.0098(18) 0.0139(19) 0.0024(15) 0.0020(15) 0.0008(14)
C6 0.0107(19) 0.0132(19) 0.0103(18) 0.0056(15) 0.0022(15) 0.0005(15)
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
V1 O4 1.591(3) . ?
V1 O5 1.943(3) . ?
V1 O6 1.954(3) . ?
V1 O7 1.966(3) . ?
V1 O3 2.022(3) . ?
P1 O1 1.506(3) . ?
P1 O3 1.524(3) . ?
P1 O2 1.567(3) . ?
P1 C4 1.797(4) . ?
P2 O7 1.517(3) 4_575 ?
P2 O6 1.533(3) 1_554 ?
P2 O5 1.536(3) . ?
P2 C1 1.797(4) . ?
O2 H2 0.8400 . ?
O6 P2 1.533(3) 1_556 ?
O7 P2 1.517(3) 4_576 ?
N1 C5 1.490(5) . ?
N1 C6 1.498(5) 3_576 ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C1 C2 1.522(6) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C3 1.523(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(6) 3_677 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C3 1.523(6) 3_677 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.512(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.498(5) 3_576 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
|
1101195.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101195.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_1101195
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C8 H19 N O7 P2 V'
_chemical_formula_weight 354.12
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 95.026(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.941(3)
_cell_length_b 13.470(2)
_cell_length_c 6.0553(10)
_cell_measurement_temperature 90(2)
_cell_volume 1376.5(4)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.709
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101195
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
V1 V 0.20164(4) 0.36569(4) 1.03372(10) 0.00392(15) Uani 1 1 d . . .
P1 P 0.17725(6) 0.61240(7) 0.95695(16) 0.0074(2) Uani 1 1 d . . .
P2 P 0.27679(6) 0.35415(7) 0.55265(15) 0.00468(19) Uani 1 1 d . . .
O1 O 0.12848(16) 0.6454(2) 0.7508(5) 0.0108(6) Uani 1 1 d . . .
O2 O 0.16040(18) 0.6746(2) 1.1679(5) 0.0132(6) Uani 1 1 d . . .
H2 H 0.1461 0.7322 1.1292 0.020 Uiso 1 1 calc R . .
O3 O 0.16018(16) 0.50659(19) 1.0276(4) 0.0068(5) Uani 1 1 d . . .
O4 O 0.24193(16) 0.4012(2) 0.7542(4) 0.0080(5) Uani 1 1 d . . .
O5 O 0.11877(16) 0.3091(2) 1.0008(5) 0.0092(5) Uani 1 1 d . . .
O6 O 0.23017(16) 0.39648(19) 1.3450(4) 0.0075(5) Uani 1 1 d . . .
O7 O 0.28010(15) 0.25825(19) 1.0621(4) 0.0055(5) Uani 1 1 d . . .
N1 N 0.07616(19) 0.5159(2) 0.4191(5) 0.0086(6) Uani 1 1 d . . .
H1A H 0.1104 0.5089 0.3104 0.010 Uiso 1 1 calc R . .
H1B H 0.1021 0.5502 0.5352 0.010 Uiso 1 1 calc R . .
C1 C 0.2796(2) 0.6316(3) 0.9159(7) 0.0134(8) Uani 1 1 d . . .
H1C H 0.2914 0.5960 0.7795 0.016 Uiso 1 1 calc R . .
H1D H 0.2878 0.7033 0.8900 0.016 Uiso 1 1 calc R . .
C2 C 0.3395(2) 0.5982(3) 1.1048(7) 0.0135(8) Uani 1 1 d . . .
H2A H 0.3220 0.6222 1.2472 0.016 Uiso 1 1 calc R . .
H2B H 0.3405 0.5247 1.1098 0.016 Uiso 1 1 calc R . .
C3 C 0.4231(2) 0.6363(3) 1.0804(7) 0.0166(8) Uani 1 1 d . . .
H3A H 0.4401 0.6139 0.9362 0.020 Uiso 1 1 calc R . .
H3B H 0.4225 0.7098 1.0799 0.020 Uiso 1 1 calc R . .
C4 C 0.4827(2) 0.6005(3) 1.2651(7) 0.0136(8) Uani 1 1 d . . .
H4A H 0.4850 0.5271 1.2596 0.016 Uiso 1 1 calc R . .
H4B H 0.4634 0.6192 1.4091 0.016 Uiso 1 1 calc R . .
C5 C 0.3774(2) 0.3967(3) 0.5516(6) 0.0087(7) Uani 1 1 d . . .
H5A H 0.3980 0.3759 0.4107 0.010 Uiso 1 1 calc R . .
H5B H 0.3775 0.4702 0.5551 0.010 Uiso 1 1 calc R . .
C6 C 0.4338(2) 0.3587(3) 0.7442(7) 0.0141(8) Uani 1 1 d . . .
H6A H 0.4135 0.3785 0.8862 0.017 Uiso 1 1 calc R . .
H6B H 0.4355 0.2853 0.7395 0.017 Uiso 1 1 calc R . .
C7 C 0.0047(2) 0.5739(3) 0.3289(7) 0.0114(8) Uani 1 1 d . . .
H7A H -0.0212 0.5395 0.1975 0.014 Uiso 1 1 calc R . .
H7B H 0.0213 0.6406 0.2820 0.014 Uiso 1 1 calc R . .
C8 C 0.0531(2) 0.4158(3) 0.4972(7) 0.0097(7) Uani 1 1 d . . .
H8A H 0.1008 0.3798 0.5600 0.012 Uiso 1 1 calc R . .
H8B H 0.0285 0.3769 0.3705 0.012 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
V1 0.0052(3) 0.0020(3) 0.0044(3) -0.0003(2) 0.0001(2) 0.0002(2)
P1 0.0092(5) 0.0044(4) 0.0085(4) 0.0006(3) -0.0001(3) 0.0001(3)
P2 0.0061(4) 0.0036(4) 0.0044(4) -0.0001(3) 0.0005(3) -0.0011(3)
O1 0.0129(13) 0.0064(13) 0.0126(13) 0.0025(11) -0.0027(11) -0.0019(10)
O2 0.0202(16) 0.0062(13) 0.0134(14) -0.0023(11) 0.0019(12) 0.0000(11)
O3 0.0100(13) 0.0051(12) 0.0055(12) 0.0008(9) 0.0013(10) 0.0014(10)
O4 0.0117(13) 0.0061(12) 0.0062(12) 0.0000(10) 0.0012(10) 0.0014(10)
O5 0.0075(13) 0.0058(12) 0.0143(14) 0.0005(10) 0.0002(11) -0.0005(10)
O6 0.0111(13) 0.0046(12) 0.0069(12) -0.0006(10) 0.0012(10) 0.0017(10)
O7 0.0062(12) 0.0050(12) 0.0054(12) -0.0008(9) 0.0012(10) 0.0014(9)
N1 0.0073(15) 0.0103(15) 0.0083(15) -0.0007(12) 0.0021(12) 0.0001(12)
C1 0.0105(18) 0.0119(19) 0.018(2) 0.0039(16) 0.0008(15) -0.0025(15)
C2 0.0080(18) 0.0114(18) 0.021(2) 0.0031(16) -0.0013(15) -0.0027(14)
C3 0.0128(19) 0.017(2) 0.020(2) 0.0038(17) -0.0008(16) -0.0042(16)
C4 0.0082(18) 0.0139(19) 0.019(2) 0.0021(16) 0.0011(16) -0.0021(15)
C5 0.0068(17) 0.0070(17) 0.0121(18) 0.0004(14) 0.0001(14) -0.0007(13)
C6 0.0106(18) 0.014(2) 0.0166(19) 0.0058(16) -0.0027(15) -0.0026(15)
C7 0.0116(19) 0.0110(18) 0.0117(19) 0.0048(15) 0.0016(15) 0.0014(15)
C8 0.0057(17) 0.0095(18) 0.0145(19) 0.0038(14) 0.0040(14) 0.0017(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O5 1.594(3) . ?
V1 O4 1.940(3) . ?
V1 O6 1.949(3) . ?
V1 O7 1.962(3) . ?
V1 O3 2.023(3) . ?
P1 O1 1.503(3) . ?
P1 O3 1.523(3) . ?
P1 O2 1.575(3) . ?
P1 C1 1.792(4) . ?
P2 O7 1.516(3) 4_565 ?
P2 O6 1.535(3) 1_554 ?
P2 O4 1.538(3) . ?
P2 C5 1.798(4) . ?
O6 P2 1.535(3) 1_556 ?
O7 P2 1.516(3) 4_566 ?
N1 C8 1.493(5) . ?
N1 C7 1.503(5) . ?
C1 C2 1.529(6) . ?
C2 C3 1.526(6) . ?
C3 C4 1.518(6) . ?
C4 C6 1.523(6) 3_667 ?
C5 C6 1.531(5) . ?
C6 C4 1.523(5) 3_667 ?
C7 C8 1.505(5) 3_566 ?
C8 C7 1.505(5) 3_566 ?
|
1101196.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101196.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_1101196
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C9 H24 N2 O15 P4 V3'
_chemical_formula_weight 677.00
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 89.994(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.3248(15)
_cell_length_b 13.3361(12)
_cell_length_c 10.1019(9)
_cell_measurement_temperature 90(2)
_cell_volume 2199.3(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.045
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101196
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
V1 V 1.02370(2) 0.54667(3) 1.24768(3) 0.01093(8) Uani 1 1 d . . .
V2 V 0.74997(2) 0.74997(3) 0.96353(3) 0.01021(8) Uani 1 1 d . . .
V3 V 0.52366(2) 1.04669(3) 0.75232(3) 0.01125(8) Uani 1 1 d . . .
P1 P 1.08665(3) 0.39478(4) 1.49759(5) 0.01071(11) Uani 1 1 d . . .
P2 P 0.91431(3) 0.60619(4) 0.98508(5) 0.01092(11) Uani 1 1 d . . .
P3 P 0.58567(3) 0.89385(4) 0.98501(5) 0.01121(11) Uani 1 1 d . . .
P4 P 0.58665(3) 0.89483(4) 0.50240(5) 0.01105(11) Uani 1 1 d . . .
O1 O 1.07158(10) 0.47978(13) 1.40110(16) 0.0198(3) Uani 1 1 d . . .
O2 O 1.09529(10) 0.45740(13) 1.14037(15) 0.0196(3) Uani 1 1 d . . .
O3 O 1.06956(10) 0.65132(13) 1.24107(17) 0.0209(3) Uani 1 1 d . . .
O4 O 0.92483(9) 0.57169(13) 1.35831(14) 0.0157(3) Uani 1 1 d . . .
O5 O 0.94529(9) 0.54468(12) 1.10114(15) 0.0154(3) Uani 1 1 d . . .
O6 O 0.83150(9) 0.65138(12) 1.02107(15) 0.0158(3) Uani 1 1 d . . .
O7 O 0.67444(9) 0.64287(12) 1.01813(16) 0.0162(3) Uani 1 1 d . . .
O8 O 0.75006(14) 0.74992(13) 0.80634(17) 0.0244(4) Uani 1 1 d . . .
O9 O 0.82560(9) 0.85714(12) 1.01799(15) 0.0161(3) Uani 1 1 d . . .
O10 O 0.66854(9) 0.84857(12) 1.02097(15) 0.0158(3) Uani 1 1 d . . .
O11 O 0.59522(10) 0.95765(13) 0.85958(16) 0.0202(3) Uani 1 1 d . . .
O12 O 0.57168(11) 0.97994(13) 0.59880(16) 0.0208(3) Uani 1 1 d . . .
O13 O 0.56941(10) 1.15138(13) 0.75894(17) 0.0217(3) Uani 1 1 d . . .
O14 O 0.44518(9) 1.04469(12) 0.89876(15) 0.0155(3) Uani 1 1 d . . .
O15 O 0.42481(9) 1.07157(13) 0.64180(15) 0.0163(3) Uani 1 1 d . . .
N1 N 0.23761(13) 1.03252(15) 0.2640(2) 0.0210(4) Uani 1 1 d . . .
H1A H 0.2817 1.0373 0.2126 0.031 Uiso 1 1 calc R . .
H1B H 0.2381 1.0817 0.3235 0.031 Uiso 1 1 calc R . .
H1C H 0.1927 1.0374 0.2144 0.031 Uiso 1 1 calc R . .
N2 N 0.26240(13) 0.46740(15) 0.2641(2) 0.0211(4) Uani 1 1 d . . .
H2A H 0.2189 0.4631 0.2114 0.032 Uiso 1 1 calc R . .
H2B H 0.2608 0.4183 0.3237 0.032 Uiso 1 1 calc R . .
H2C H 0.3078 0.4619 0.2160 0.032 Uiso 1 1 calc R . .
C1 C 1.01441(14) 0.29675(18) 1.4607(2) 0.0195(4) Uani 1 1 d . . .
H1D H 0.9598 0.3255 1.4617 0.023 Uiso 1 1 calc R . .
H1E H 1.0248 0.2732 1.3715 0.023 Uiso 1 1 calc R . .
C2 C 0.98493(15) 0.70551(18) 0.9458(2) 0.0208(5) Uani 1 1 d . . .
H2D H 1.0397 0.6774 0.9440 0.025 Uiso 1 1 calc R . .
H2E H 0.9727 0.7291 0.8572 0.025 Uiso 1 1 calc R . .
C3 C 0.51512(15) 0.79457(19) 0.9457(2) 0.0218(5) Uani 1 1 d . . .
H3A H 0.4603 0.8227 0.9437 0.026 Uiso 1 1 calc R . .
H3B H 0.5274 0.7709 0.8571 0.026 Uiso 1 1 calc R . .
C4 C 0.51436(14) 0.79672(18) 0.5392(2) 0.0204(5) Uani 1 1 d . . .
H4A H 0.5248 0.7732 0.6285 0.025 Uiso 1 1 calc R . .
H4B H 0.4598 0.8254 0.5382 0.025 Uiso 1 1 calc R . .
C5 C 0.23804(16) 0.93439(18) 0.3330(3) 0.0235(5) Uani 1 1 d . . .
H5A H 0.1903 0.9305 0.3900 0.028 Uiso 1 1 calc R . .
H5B H 0.2863 0.9307 0.3889 0.028 Uiso 1 1 calc R . .
C6 C 0.23777(17) 0.84515(19) 0.2403(3) 0.0264(5) Uani 1 1 d . . .
H6A H 0.2814 0.8519 0.1758 0.032 Uiso 1 1 calc R . .
H6B H 0.1861 0.8419 0.1932 0.032 Uiso 1 1 calc R . .
C7 C 0.2500(2) 0.75001(19) 0.3211(3) 0.0306(6) Uani 1 1 d . . .
H7A H 0.2975 0.7591 0.3777 0.037 Uiso 1 1 calc R . .
H7B H 0.2028 0.7410 0.3781 0.037 Uiso 1 1 calc R . .
C8 C 0.26212(17) 0.65483(19) 0.2404(3) 0.0267(5) Uani 1 1 d . . .
H8A H 0.2184 0.6481 0.1761 0.032 Uiso 1 1 calc R . .
H8B H 0.3138 0.6580 0.1932 0.032 Uiso 1 1 calc R . .
C9 C 0.26189(16) 0.56578(18) 0.3330(3) 0.0234(5) Uani 1 1 d . . .
H9A H 0.3096 0.5698 0.3900 0.028 Uiso 1 1 calc R . .
H9B H 0.2137 0.5695 0.3889 0.028 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
V1 0.01176(17) 0.01129(17) 0.00975(16) 0.00044(12) -0.00053(12) 0.00239(13)
V2 0.00936(16) 0.00871(16) 0.01255(16) -0.00012(12) -0.00003(12) -0.00005(12)
V3 0.01194(17) 0.01176(17) 0.01004(16) -0.00051(12) 0.00051(12) 0.00256(13)
P1 0.0099(2) 0.0125(2) 0.0097(2) 0.00084(18) -0.00014(17) 0.00321(18)
P2 0.0101(2) 0.0124(2) 0.0103(2) -0.00028(18) 0.00017(17) 0.00350(19)
P3 0.0102(2) 0.0130(3) 0.0104(2) -0.00005(18) -0.00018(17) 0.00359(19)
P4 0.0099(2) 0.0134(3) 0.0099(2) -0.00045(18) 0.00015(17) 0.00348(19)
O1 0.0228(8) 0.0215(8) 0.0150(7) 0.0065(6) -0.0003(6) 0.0082(7)
O2 0.0196(8) 0.0257(9) 0.0135(7) -0.0069(6) -0.0043(6) 0.0102(7)
O3 0.0206(8) 0.0152(8) 0.0269(9) 0.0019(6) 0.0003(6) -0.0007(6)
O4 0.0140(7) 0.0224(8) 0.0107(7) -0.0009(6) 0.0004(5) 0.0024(6)
O5 0.0152(7) 0.0191(8) 0.0117(7) 0.0013(6) -0.0030(5) 0.0035(6)
O6 0.0121(7) 0.0141(7) 0.0212(8) 0.0025(6) 0.0029(6) 0.0048(6)
O7 0.0116(7) 0.0143(8) 0.0226(8) 0.0032(6) -0.0032(6) -0.0041(6)
O8 0.0356(10) 0.0217(8) 0.0158(8) -0.0001(6) -0.0004(7) -0.0017(7)
O9 0.0121(7) 0.0149(8) 0.0214(8) -0.0032(6) 0.0033(6) -0.0043(6)
O10 0.0119(7) 0.0144(7) 0.0210(8) -0.0022(6) -0.0031(6) 0.0045(6)
O11 0.0202(8) 0.0268(9) 0.0137(7) 0.0069(6) 0.0044(6) 0.0103(7)
O12 0.0227(8) 0.0245(9) 0.0152(7) -0.0069(6) 0.0000(6) 0.0093(7)
O13 0.0213(8) 0.0157(8) 0.0281(9) -0.0015(7) 0.0001(7) -0.0005(6)
O14 0.0150(7) 0.0198(8) 0.0118(7) -0.0013(6) 0.0026(5) 0.0037(6)
O15 0.0140(7) 0.0237(8) 0.0113(7) 0.0014(6) -0.0003(5) 0.0024(6)
N1 0.0251(10) 0.0148(9) 0.0231(10) -0.0007(7) -0.0005(8) 0.0014(8)
N2 0.0252(10) 0.0159(10) 0.0223(10) 0.0014(7) -0.0003(8) 0.0009(8)
C1 0.0165(10) 0.0184(11) 0.0234(11) -0.0021(9) -0.0046(8) 0.0002(9)
C2 0.0200(11) 0.0172(11) 0.0252(12) 0.0022(9) 0.0093(9) 0.0004(9)
C3 0.0205(11) 0.0204(11) 0.0247(12) -0.0033(9) -0.0091(9) 0.0010(9)
C4 0.0169(10) 0.0198(11) 0.0246(12) 0.0034(9) 0.0048(8) 0.0000(9)
C5 0.0253(12) 0.0176(11) 0.0276(12) 0.0020(9) 0.0015(9) 0.0012(9)
C6 0.0267(13) 0.0164(11) 0.0362(14) -0.0023(10) -0.0042(10) 0.0015(10)
C7 0.0354(14) 0.0157(11) 0.0408(15) -0.0006(10) 0.0010(12) -0.0005(10)
C8 0.0279(13) 0.0163(11) 0.0359(14) 0.0018(10) 0.0057(10) 0.0018(10)
C9 0.0258(12) 0.0168(11) 0.0277(12) -0.0013(9) -0.0002(9) 0.0005(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5851(17) . ?
V1 O1 1.9517(16) . ?
V1 O5 1.9573(15) . ?
V1 O2 1.9895(16) . ?
V1 O4 1.9912(15) . ?
V2 O8 1.5880(17) . ?
V2 O10 1.9577(16) . ?
V2 O6 1.9591(15) . ?
V2 O7 1.9659(16) . ?
V2 O9 1.9671(16) . ?
V3 O13 1.5848(17) . ?
V3 O12 1.9524(16) . ?
V3 O14 1.9570(15) . ?
V3 O11 1.9872(16) . ?
V3 O15 1.9901(16) . ?
P1 O1 1.5152(16) . ?
P1 O9 1.5259(16) 2_747 ?
P1 O4 1.5343(15) 3_768 ?
P1 C1 1.800(2) . ?
P2 O5 1.5178(15) . ?
P2 O6 1.5241(15) . ?
P2 O2 1.5330(16) 3_767 ?
P2 C2 1.800(2) . ?
P3 O14 1.5178(16) 3_677 ?
P3 O10 1.5254(15) . ?
P3 O11 1.5342(16) . ?
P3 C3 1.799(2) . ?
P4 O12 1.5154(17) . ?
P4 O7 1.5270(16) 4_575 ?
P4 O15 1.5355(15) 3_676 ?
P4 C4 1.801(2) . ?
O2 P2 1.5329(16) 3_767 ?
O4 P1 1.5343(15) 3_768 ?
O7 P4 1.5271(16) 4_576 ?
O9 P1 1.5259(16) 2_757 ?
O14 P3 1.5178(16) 3_677 ?
O15 P4 1.5355(15) 3_676 ?
N1 C5 1.483(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C9 1.485(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C1 C2 1.540(3) 2_747 ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 C1 1.540(3) 2_757 ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C3 C4 1.541(4) 4_576 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C3 1.541(4) 4_575 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.515(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.522(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.521(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.512(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
|
1101197.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101197.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_1101197
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C0.5 H2 O2.5 P0.5 V0.5'
_chemical_formula_weight 88.98
_space_group_IT_number 63
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-C 2c 2'
_symmetry_space_group_name_H-M 'C m c m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 7.4670(5)
_cell_length_b 13.8824(9)
_cell_length_c 9.3289(6)
_cell_measurement_temperature 90(2)
_cell_volume 967.03(11)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.445
_cod_duplicate_entry 1101175
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_formula_sum 'C0.50 H2 O2.50 P0.50 V0.50'
_cod_database_code 1101197
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-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'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'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'
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
V1 V 0.20578(5) 0.23916(3) 0.2500 0.00785(14) Uani 1 2 d S . .
P1 P 0.0000 0.34326(4) 0.51600(5) 0.00666(16) Uani 1 2 d S . .
O1 O 0.0000 0.26945(10) 0.38945(16) 0.0078(3) Uani 1 2 d S . .
O2 O 0.0000 0.10926(17) 0.2500 0.0111(4) Uani 1 4 d S . .
O3 O 0.32849(15) 0.16633(8) 0.39904(12) 0.0112(2) Uani 1 1 d . . .
O4 O 0.3029(2) 0.34148(12) 0.2500 0.0152(4) Uani 1 2 d S . .
O90 O 1.0000 0.0395(3) 0.5350(4) 0.0186(7) Uani 0.50 2 d SP . .
H90 H 0.8995 0.0475 0.5737 0.028 Uiso 0.50 1 calc PR . .
C1 C 0.0000 0.46123(15) 0.4415(2) 0.0117(4) Uani 1 2 d S . .
H1A H 0.1072 0.4694 0.3802 0.014 Uiso 0.50 1 calc PR . .
H1B H -0.1072 0.4694 0.3802 0.014 Uiso 0.50 1 calc PR . .
H2 H 0.0000 0.080(3) 0.308(4) 0.038(11) Uiso 1 2 d S . .
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
V1 0.0070(2) 0.0094(2) 0.0072(2) 0.000 0.000 0.00059(11)
P1 0.0063(3) 0.0085(3) 0.0052(3) 0.00031(16) 0.000 0.000
O1 0.0073(7) 0.0093(6) 0.0068(7) -0.0025(5) 0.000 0.000
O2 0.0143(11) 0.0110(10) 0.0080(10) 0.000 0.000 0.000
O3 0.0096(5) 0.0134(5) 0.0105(5) -0.0005(4) -0.0041(4) 0.0022(4)
O4 0.0121(8) 0.0124(8) 0.0211(8) 0.000 0.000 -0.0014(5)
O90 0.0193(16) 0.0177(16) 0.0189(17) -0.0001(13) 0.000 0.000
C1 0.0166(10) 0.0106(9) 0.0077(9) -0.0005(7) 0.000 0.000
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
V1 O4 1.5948(17) . ?
V1 O3 1.9480(11) 10_556 ?
V1 O3 1.9480(11) . ?
V1 O1 2.0567(10) . ?
V1 O1 2.0568(10) 10_556 ?
V1 O2 2.3692(18) . ?
V1 V1 3.0731(7) 3 ?
P1 O3 1.5120(11) 13_556 ?
P1 O3 1.5120(11) 8_456 ?
P1 O1 1.5632(15) . ?
P1 C1 1.779(2) . ?
O1 V1 2.0567(10) 3 ?
O2 V1 2.3692(18) 3 ?
O2 H2 0.67(4) . ?
O3 P1 1.5120(11) 13_556 ?
O90 H90 0.8400 . ?
C1 C1 1.534(4) 9_566 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
|
1101198.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101198.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_1101198
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C0.75 H3 O2.75 P0.5 V0.5'
_chemical_formula_weight 96.99
_space_group_IT_number 71
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-I 2 2'
_symmetry_space_group_name_H-M 'I m m m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 7.4265(13)
_cell_length_b 9.3477(16)
_cell_length_c 16.793(3)
_cell_measurement_temperature 90(2)
_cell_volume 1165.8(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.210
_cod_duplicate_entry 1101176
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_formula_sum 'C0.75 H3 O2.75 P0.50 V0.50'
_cod_database_code 1101198
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'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'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-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'
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
V1 V 0.20621(14) 0.5000 0.24238(5) 0.0199(3) Uani 1 2 d S . .
P1 P 0.0000 0.23139(13) 0.32989(7) 0.0171(3) Uani 1 2 d S . .
O1 O 0.3271(4) 0.3522(3) 0.17987(16) 0.0254(7) Uani 1 1 d . . .
O2 O 0.3071(6) 0.5000 0.3258(2) 0.0281(9) Uani 1 2 d S . .
O3 O 0.0000 0.3610(4) 0.2703(2) 0.0191(8) Uani 1 2 d S . .
O90 O 0.0000 0.5000 0.1407(3) 0.0235(12) Uani 1 4 d S . .
O91 O 0.0000 0.2346(5) 0.0810(3) 0.0578(17) Uani 1 2 d S . .
C1 C 0.0000 0.3084(5) 0.4260(3) 0.0156(9) Uani 1 2 d S . .
H1A H 0.1071 0.3711 0.4296 0.019 Uiso 0.50 1 calc PR . .
H1B H -0.1071 0.3711 0.4296 0.019 Uiso 0.50 1 calc PR . .
C2 C 0.0000 0.2122(7) 0.5000 0.0143(13) Uani 1 4 d S . .
H2A H 0.1081 0.1503 0.5000 0.017 Uiso 0.50 2 calc SPR . .
H2B H -0.1081 0.1503 0.5000 0.017 Uiso 0.50 2 calc SPR . .
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
V1 0.0413(6) 0.0066(4) 0.0119(4) 0.000 0.0083(4) 0.000
P1 0.0370(8) 0.0045(5) 0.0098(6) -0.0001(4) 0.000 0.000
O1 0.0464(17) 0.0104(11) 0.0193(13) 0.0019(10) 0.0128(12) 0.0074(11)
O2 0.039(2) 0.029(2) 0.0158(18) 0.000 0.0108(17) 0.000
O3 0.038(2) 0.0076(15) 0.0115(16) 0.0019(12) 0.000 0.000
O90 0.052(4) 0.007(2) 0.012(2) 0.000 0.000 0.000
O91 0.119(5) 0.024(2) 0.030(3) -0.011(2) 0.000 0.000
C1 0.026(2) 0.009(2) 0.012(2) 0.0009(17) 0.000 0.000
C2 0.014(3) 0.011(3) 0.018(3) 0.000 0.000 0.000
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
V1 O2 1.588(4) . ?
V1 O1 1.954(3) . ?
V1 O1 1.954(3) 11_565 ?
V1 O3 2.062(2) . ?
V1 O3 2.062(2) 2_565 ?
V1 O90 2.294(4) . ?
V1 V1 3.063(2) 2_565 ?
P1 O1 1.512(3) 8_455 ?
P1 O1 1.512(3) 13 ?
P1 O3 1.572(4) . ?
P1 C1 1.767(5) . ?
O1 P1 1.512(3) 13 ?
O3 V1 2.062(2) 2_565 ?
O90 V1 2.294(4) 2_565 ?
C1 C2 1.534(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C1 1.534(6) 10_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
|
1101199.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/11/1101199.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_1101199
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C H4 O3 P0.5 V0.5'
_chemical_formula_weight 105.00
_space_group_IT_number 63
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-C 2c 2'
_symmetry_space_group_name_H-M 'C m c m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 7.4362(5)
_cell_length_b 19.1491(12)
_cell_length_c 9.3446(6)
_cell_measurement_temperature 90(2)
_cell_volume 1330.64(15)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.096
_cod_duplicate_entry 1101177
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_formula_sum 'C H4 O3 P0.50 V0.50'
_cod_database_code 1101199
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-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'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'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'
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
V1 V 0.20583(8) 0.25889(3) 0.7500 0.00606(17) Uani 1 2 d S . .
P1 P 0.0000 0.18052(4) 0.48448(9) 0.0050(2) Uani 1 2 d S . .
O1 O 0.0000 0.23467(12) 0.6099(3) 0.0068(5) Uani 1 2 d S . .
O2 O 0.3276(2) 0.31228(9) 0.60042(18) 0.0098(4) Uani 1 1 d . . .
O3 O 0.0000 0.3486(2) 0.7500 0.0088(7) Uani 1 4 d S . .
O4 O 0.3053(3) 0.18516(14) 0.7500 0.0131(5) Uani 1 2 d S . .
O90A O 0.0000 0.3999(4) 0.4759(6) 0.0290(19) Uani 0.670(19) 2 d SP A 1
O90B O 0.0000 0.4456(11) 0.537(2) 0.060(8) Uani 0.330(19) 2 d SP A 2
O91 O 0.0000 0.528(3) 0.7500 0.57(5) Uani 1 4 d S . .
C1 C 0.0000 0.09621(17) 0.5641(4) 0.0084(6) Uani 1 2 d S . .
H1A H 0.1073 0.0923 0.6263 0.010 Uiso 0.50 1 calc PR . .
H1B H -0.1073 0.0923 0.6263 0.010 Uiso 0.50 1 calc PR . .
C2 C 0.0000 0.03485(17) 0.4601(4) 0.0109(7) Uani 1 2 d S . .
H2A H 0.1077 0.0376 0.3981 0.013 Uiso 0.50 1 calc PR . .
H2B H -0.1077 0.0376 0.3981 0.013 Uiso 0.50 1 calc PR . .
H3 H 0.0000 0.370(3) 0.693(6) 0.040(19) Uiso 1 2 d S . .
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
V1 0.0047(3) 0.0091(3) 0.0043(3) 0.000 0.000 -0.0005(2)
P1 0.0053(4) 0.0069(4) 0.0028(4) 0.0002(3) 0.000 0.000
O1 0.0063(11) 0.0102(11) 0.0040(10) -0.0013(9) 0.000 0.000
O2 0.0092(8) 0.0120(8) 0.0081(8) -0.0007(6) 0.0037(7) -0.0013(6)
O3 0.0090(16) 0.0106(17) 0.0068(17) 0.000 0.000 0.000
O4 0.0082(12) 0.0137(12) 0.0174(13) 0.000 0.000 0.0011(10)
O90A 0.034(3) 0.033(4) 0.020(3) 0.005(2) 0.000 0.000
O90B 0.041(7) 0.064(14) 0.073(14) 0.053(12) 0.000 0.000
O91 0.31(4) 1.22(15) 0.16(3) 0.000 0.000 0.000
C1 0.0113(15) 0.0075(14) 0.0065(14) 0.0006(12) 0.000 0.000
C2 0.0170(16) 0.0085(16) 0.0072(15) -0.0009(12) 0.000 0.000
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
V1 O4 1.594(3) . ?
V1 O2 1.9541(18) . ?
V1 O2 1.9541(18) 10_557 ?
V1 O1 2.0669(17) 10_557 ?
V1 O1 2.0669(17) . ?
V1 O3 2.300(3) . ?
V1 V1 3.0611(11) 3_556 ?
P1 O2 1.5142(18) 8_456 ?
P1 O2 1.5142(18) 13_556 ?
P1 O1 1.565(2) . ?
P1 C1 1.778(3) . ?
O1 V1 2.0669(17) 3_556 ?
O2 P1 1.5142(18) 13_556 ?
O3 V1 2.300(3) 3_556 ?
O3 H3 0.67(5) . ?
C1 C2 1.524(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.529(7) 9_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
|
1101200.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101200.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_1101200
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C1.25 H4.5 O3 P0.5 V0.5'
_chemical_formula_weight 108.50
_space_group_IT_number 71
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-I 2 2'
_symmetry_space_group_name_H-M 'I m m m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 7.4330(4)
_cell_length_b 9.3673(5)
_cell_length_c 21.8357(11)
_cell_measurement_temperature 90(2)
_cell_volume 1520.36(14)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.896
_cod_duplicate_entry 1101178
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_formula_sum 'C1.25 H4.50 O3 P0.50 V0.50'
_cod_database_code 1101200
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'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'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-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'
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
V1 V 0.20623(6) 0.5000 0.255827(18) 0.00709(11) Uani 1 2 d S . .
P1 P 0.0000 0.23216(6) 0.18855(3) 0.00584(13) Uani 1 2 d S . .
O1 O 0.0000 0.36095(19) 0.23435(8) 0.0083(3) Uani 1 2 d S . .
O2 O 0.3077(3) 0.5000 0.19139(9) 0.0162(4) Uani 1 2 d S . .
O3 O 0.32738(18) 0.35137(14) 0.30350(6) 0.0118(3) Uani 1 1 d . . .
O90 O 0.0000 0.5000 0.33395(12) 0.0101(5) Uani 1 4 d S . .
O91 O 0.0000 0.2371(2) 0.38060(12) 0.0265(5) Uani 1 2 d S . .
O92 O 0.4376(10) 0.3609(7) 0.0000 0.0521(19) Uani 0.50 2 d SP . .
C1 C 0.0000 0.3070(3) 0.11351(11) 0.0118(4) Uani 1 2 d S . .
H1A H -0.1072 0.3691 0.1097 0.014 Uiso 0.50 1 calc PR . .
H1B H 0.1072 0.3691 0.1097 0.014 Uiso 0.50 1 calc PR . .
C2 C 0.0000 0.2038(3) 0.05932(12) 0.0144(5) Uani 1 2 d S . .
H2A H 0.1080 0.1421 0.0610 0.017 Uiso 0.50 1 calc PR . .
H2B H -0.1080 0.1421 0.0610 0.017 Uiso 0.50 1 calc PR . .
C3 C 0.0000 0.2897(4) 0.0000 0.0222(9) Uani 1 4 d S . .
H3A H 0.1073 0.3523 0.0000 0.027 Uiso 0.50 2 calc SPR . .
H3B H -0.1073 0.3523 0.0000 0.027 Uiso 0.50 2 calc SPR . .
H90 H 0.0000 0.437(4) 0.3531(19) 0.030(12) Uiso 1 2 d S . .
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
V1 0.00636(18) 0.00626(18) 0.00863(18) 0.000 -0.00014(13) 0.000
P1 0.0068(3) 0.0042(2) 0.0064(2) -0.00001(18) 0.000 0.000
O1 0.0083(7) 0.0066(7) 0.0098(7) -0.0022(6) 0.000 0.000
O2 0.0109(9) 0.0260(10) 0.0116(8) 0.000 0.0016(7) 0.000
O3 0.0118(6) 0.0092(5) 0.0143(6) -0.0021(5) -0.0028(5) 0.0042(4)
O90 0.0137(12) 0.0081(11) 0.0083(11) 0.000 0.000 0.000
O91 0.0382(13) 0.0162(10) 0.0252(12) 0.0075(9) 0.000 0.000
O92 0.070(5) 0.052(4) 0.034(3) 0.000 0.000 0.009(3)
C1 0.0186(11) 0.0093(10) 0.0075(9) 0.0001(8) 0.000 0.000
C2 0.0244(13) 0.0094(10) 0.0094(10) -0.0001(8) 0.000 0.000
C3 0.046(3) 0.0118(16) 0.0090(15) 0.000 0.000 0.000
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
V1 O2 1.596(2) . ?
V1 O3 1.9578(13) . ?
V1 O3 1.9578(13) 11_565 ?
V1 O1 2.0655(12) . ?
V1 O1 2.0656(12) 2_565 ?
V1 O90 2.293(2) . ?
V1 V1 3.0658(8) 2_565 ?
P1 O3 1.5128(13) 8_455 ?
P1 O3 1.5128(13) 13 ?
P1 O1 1.5670(18) . ?
P1 C1 1.782(3) . ?
O1 V1 2.0656(12) 2_565 ?
O3 P1 1.5128(13) 13 ?
O90 V1 2.293(2) 2_565 ?
C1 C2 1.528(4) . ?
C2 C3 1.525(3) . ?
C3 C2 1.525(3) 10 ?
|
1101201.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101201.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_1101201
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C3 H10 O6 P V'
_chemical_formula_weight 224.02
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 94.606(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.0943(12)
_cell_length_b 5.2746(4)
_cell_length_c 10.1660(8)
_cell_measurement_temperature 90(2)
_cell_volume 753.32(10)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.975
_cod_duplicate_entry 1101179
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101201
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
V1 V 0.80978(4) 1.10864(9) 0.34935(5) 0.00629(17) Uani 1 1 d . . .
P1 P 0.78928(6) 0.89833(14) 0.64335(8) 0.0056(2) Uani 1 1 d . . .
O1 O 0.83060(16) 0.8711(4) 0.5071(2) 0.0066(4) Uani 1 1 d . . .
O2 O 0.69779(18) 1.1387(5) 0.3533(3) 0.0147(5) Uani 1 1 d . . .
O4 O 0.82384(17) 1.3433(4) 0.1979(2) 0.0096(5) Uani 1 1 d . . .
O5 O 0.82557(16) 0.8194(4) 0.2303(2) 0.0098(5) Uani 1 1 d . . .
O90 O 0.9749(2) 1.0732(5) 0.3368(3) 0.0144(5) Uani 1 1 d . . .
O91 O 0.86291(19) 1.3819(4) 0.4743(3) 0.0112(5) Uani 1 1 d . . .
C1 C 0.6621(2) 0.8820(6) 0.6241(3) 0.0094(6) Uani 1 1 d . . .
H1A H 0.6371 0.8844 0.7123 0.011 Uiso 1 1 calc R . .
H1B H 0.6373 1.0338 0.5754 0.011 Uiso 1 1 calc R . .
C2 C 0.6254(3) 0.6442(7) 0.5501(4) 0.0200(8) Uani 1 1 d . . .
H2A H 0.6473 0.6486 0.4600 0.024 Uiso 1 1 calc R . .
H2B H 0.6545 0.4937 0.5954 0.024 Uiso 1 1 calc R . .
C3 C 0.5194(3) 0.6129(8) 0.5394(5) 0.0264(9) Uani 1 1 d . . .
H3A H 0.4905 0.7683 0.4991 0.032 Uiso 1 1 calc R . .
H3B H 0.4982 0.5996 0.6297 0.032 Uiso 1 1 calc R . .
H90A H 1.017(5) 1.123(12) 0.397(7) 0.06(2) Uiso 1 1 d . . .
H90B H 0.989(5) 0.969(15) 0.309(7) 0.06(2) Uiso 1 1 d . . .
H91A H 0.857(4) 1.352(10) 0.547(6) 0.031(15) Uiso 1 1 d . . .
H91B H 0.856(6) 1.530(16) 0.465(8) 0.08(2) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0117(3) 0.0008(2) 0.0066(3) 0.00029(17) 0.00190(19) 0.00042(17)
P1 0.0093(4) 0.0012(3) 0.0064(4) 0.0000(2) 0.0016(3) 0.0002(3)
O1 0.0120(11) 0.0006(9) 0.0070(10) 0.0001(7) 0.0010(8) 0.0001(7)
O2 0.0151(12) 0.0135(12) 0.0159(12) 0.0051(9) 0.0033(9) 0.0034(9)
O4 0.0160(12) 0.0030(10) 0.0102(11) 0.0025(8) 0.0027(9) 0.0022(8)
O5 0.0129(11) 0.0064(10) 0.0102(11) -0.0045(8) 0.0013(8) 0.0004(8)
O90 0.0157(13) 0.0124(12) 0.0152(12) -0.0053(10) 0.0016(10) 0.0014(10)
O91 0.0250(13) 0.0002(10) 0.0086(11) -0.0006(8) 0.0024(9) -0.0004(9)
C1 0.0087(14) 0.0090(14) 0.0105(14) -0.0002(11) 0.0006(11) 0.0007(11)
C2 0.0107(16) 0.0141(16) 0.035(2) -0.0113(15) 0.0013(15) -0.0022(13)
C3 0.0102(17) 0.026(2) 0.043(3) -0.0149(18) 0.0019(16) -0.0036(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.590(3) . ?
V1 O5 1.971(2) . ?
V1 O4 1.998(2) . ?
V1 O91 2.025(2) . ?
V1 O1 2.038(2) . ?
V1 O90 2.348(3) . ?
P1 O5 1.513(2) 4_576 ?
P1 O4 1.536(2) 4_586 ?
P1 O1 1.552(2) . ?
P1 C1 1.790(3) . ?
O4 P1 1.536(2) 4_585 ?
O5 P1 1.513(2) 4_575 ?
O90 H90A 0.86(7) . ?
O90 H90B 0.66(8) . ?
O91 H91A 0.77(6) . ?
O91 H91B 0.79(8) . ?
C1 C2 1.530(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.499(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.513(7) 3_666 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
|
1101202.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101202.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_1101202
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4.5 H10 O3.5 P V0.5'
_chemical_formula_weight 176.57
_space_group_IT_number 87
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4'
_symmetry_space_group_name_H-M 'I 4/m'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 8.9297(3)
_cell_length_b 8.9297(3)
_cell_length_c 34.847(2)
_cell_measurement_temperature 90(2)
_cell_volume 2778.6(2)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.688
_cod_duplicate_entry 1101180
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_formula_sum 'C4.50 H10 O3.50 P V0.50'
_cod_database_code 1101202
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1A V 0.5000 0.5000 0.32005(2) 0.0050(2) Uani 0.893(3) 4 d SP . 1
V1B V 0.5000 0.5000 0.2928(2) 0.020(2) Uani 0.107(3) 4 d SP . 2
V2A V 0.5000 0.5000 0.20912(2) 0.0042(2) Uani 0.805(3) 4 d SP . 1
V2B V 0.5000 0.5000 0.18190(12) 0.0142(12) Uani 0.195(3) 4 d SP . 2
P1 P 0.71239(7) 0.21156(7) 0.310348(12) 0.00707(12) Uani 1 1 d . . .
O1 O 0.87683(18) 0.17397(16) 0.30592(4) 0.0095(4) Uani 1 1 d . . .
O2 O 0.62540(18) 0.13161(17) 0.27647(4) 0.0106(3) Uani 1 1 d . . .
H2 H 0.5384 0.1668 0.2749 0.016 Uiso 1 1 calc R . .
O3 O 0.68533(18) 0.37973(18) 0.30925(4) 0.0088(3) Uani 1 1 d . . .
O4 O 0.5000 0.5000 0.36583(9) 0.0079(6) Uani 0.84 4 d SP . .
O5 O 0.5000 0.5000 0.25372(9) 0.0149(6) Uani 1 4 d S . .
O6 O 0.5000 0.5000 0.1371(5) 0.015(4) Uani 0.16 4 d SP . .
C1 C 0.6460(2) 0.1383(2) 0.35499(5) 0.0104(3) Uani 1 1 d . . .
H1A H 0.5388 0.1643 0.3579 0.012 Uiso 1 1 calc R . .
H1B H 0.6539 0.0278 0.3545 0.012 Uiso 1 1 calc R . .
C2 C 0.7328(3) 0.1981(3) 0.38988(6) 0.0162(5) Uani 1 1 d . . .
H2A H 0.8372 0.1611 0.3889 0.019 Uiso 1 1 calc R . .
H2B H 0.7355 0.3089 0.3889 0.019 Uiso 1 1 calc R . .
C3 C 0.6600(3) 0.1480(3) 0.42719(5) 0.0149(4) Uani 1 1 d . . .
H3A H 0.6526 0.0373 0.4272 0.018 Uiso 1 1 calc R . .
H3B H 0.5568 0.1885 0.4282 0.018 Uiso 1 1 calc R . .
C4 C 0.7437(3) 0.1971(3) 0.46313(6) 0.0189(5) Uani 1 1 d . . .
H4A H 0.7553 0.3074 0.4627 0.023 Uiso 1 1 calc R . .
H4B H 0.8451 0.1523 0.4629 0.023 Uiso 1 1 calc R . .
C5 C 0.6637(4) 0.1515(4) 0.5000 0.0172(6) Uani 1 2 d S . .
H5A H 0.5625 0.1967 0.5000 0.021 Uiso 1 2 calc SR . .
H5B H 0.6512 0.0413 0.5000 0.021 Uiso 1 2 calc SR . .
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
V1A 0.0050(2) 0.0050(2) 0.0048(5) 0.000 0.000 0.000
V1B 0.020(3) 0.020(3) 0.019(5) 0.000 0.000 0.000
V2A 0.0046(2) 0.0046(2) 0.0036(5) 0.000 0.000 0.000
V2B 0.0130(12) 0.0130(12) 0.017(3) 0.000 0.000 0.000
P1 0.0068(3) 0.0067(3) 0.0078(2) -0.00030(18) -0.00027(18) 0.00004(14)
O1 0.0079(8) 0.0083(8) 0.0124(7) -0.0005(5) -0.0008(5) -0.0004(6)
O2 0.0096(7) 0.0105(7) 0.0115(6) -0.0026(6) -0.0030(6) 0.0008(5)
O3 0.0085(7) 0.0070(7) 0.0109(7) 0.0010(5) 0.0015(5) 0.0015(6)
O4 0.0089(9) 0.0089(9) 0.0059(15) 0.000 0.000 0.000
O5 0.0137(8) 0.0137(8) 0.0173(15) 0.000 0.000 0.000
O6 0.015(5) 0.015(5) 0.015(9) 0.000 0.000 0.000
C1 0.0093(9) 0.0126(10) 0.0092(7) 0.0003(8) 0.0009(7) -0.0017(7)
C2 0.0187(11) 0.0200(11) 0.0098(8) 0.0010(7) -0.0006(8) -0.0082(9)
C3 0.0171(11) 0.0194(12) 0.0080(7) 0.0007(8) 0.0011(8) -0.0023(8)
C4 0.0235(12) 0.0226(11) 0.0106(8) 0.0003(8) 0.0004(8) -0.0077(10)
C5 0.0204(17) 0.0229(17) 0.0083(11) 0.000 0.000 -0.0020(12)
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
V1A O4 1.595(3) . ?
V1A O3 2.0084(16) 4_565 ?
V1A O3 2.0084(16) 2_665 ?
V1A O3 2.0084(16) 3_655 ?
V1A O3 2.0084(16) . ?
V1B O5 1.563(9) . ?
V1B O3 2.054(3) 4_565 ?
V1B O3 2.054(3) . ?
V1B O3 2.054(3) 2_665 ?
V1B O3 2.054(3) 3_655 ?
V2A O5 1.554(3) . ?
V2A O1 1.9743(15) 13_655 ?
V2A O1 1.9743(15) 16_545 ?
V2A O1 1.9743(15) 15_565 ?
V2A O1 1.9743(15) 14_455 ?
V2B O6 1.560(2) . ?
V2B O1 1.9501(18) 13_655 ?
V2B O1 1.9501(18) 16_545 ?
V2B O1 1.9501(18) 15_565 ?
V2B O1 1.9501(18) 14_455 ?
P1 O1 1.5141(17) . ?
P1 O3 1.5215(17) . ?
P1 O2 1.5834(13) . ?
P1 C1 1.7886(18) . ?
O1 V2B 1.9501(18) 13_655 ?
O1 V2A 1.9743(15) 13_655 ?
O2 H2 0.8400 . ?
C1 C2 1.538(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.525(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C4 1.525(3) 10_556 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
|
1101203.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101203.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_1101203
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4 H17.5 N O11.75 P2 V2'
_chemical_formula_weight 431.51
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 98.8370(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 14.5794(11)
_cell_length_b 10.2424(8)
_cell_length_c 18.7815(14)
_cell_measurement_temperature 90(2)
_cell_volume 2771.3(4)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.068
_cod_duplicate_entry 1101181
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C4 H17.50 N O11.75 P2 V2'
_cod_database_code 1101203
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
V1 V 0.15469(3) 0.62181(4) 0.08849(2) 0.01450(13) Uani 1 1 d . . .
V2 V 0.22975(4) 0.56336(5) 0.28294(2) 0.02063(14) Uani 1 1 d . . .
P1 P 0.16015(5) 0.33944(6) 0.17148(3) 0.01293(15) Uani 1 1 d . . .
P2 P 0.21799(5) 0.38091(6) 0.42608(3) 0.01342(15) Uani 1 1 d . . .
O1 O 0.19108(13) 0.80720(18) 0.07557(10) 0.0165(4) Uani 1 1 d . . .
O2 O 0.20845(16) 0.57710(19) 0.00276(10) 0.0202(4) Uani 1 1 d . . .
O3 O 0.04484(16) 0.6341(2) 0.06918(14) 0.0306(5) Uani 1 1 d . . .
O4 O 0.1936(2) 0.6558(2) 0.19040(12) 0.0317(6) Uani 1 1 d . . .
O5 O 0.17126(14) 0.43479(18) 0.11024(10) 0.0169(4) Uani 1 1 d . . .
O6 O 0.15681(15) 0.41020(19) 0.24249(10) 0.0193(4) Uani 1 1 d . . .
O7 O 0.33253(17) 0.5100(2) 0.27584(13) 0.0331(5) Uani 1 1 d . . .
O8 O 0.26146(14) 0.73995(18) 0.32440(10) 0.0184(4) Uani 1 1 d . . .
O9 O 0.21471(14) 0.50492(17) 0.38075(10) 0.0177(4) Uani 1 1 d . . .
O90 O 0.0803(2) 0.6500(3) 0.30017(17) 0.0482(7) Uani 1 1 d . . .
O91 O 0.0083(2) 0.9200(3) 0.05864(19) 0.0518(8) Uani 1 1 d . . .
O92 O 0.0479(6) 0.9134(6) 0.3081(4) 0.108(3) Uani 0.75 1 d P . .
N1A N 0.1337(3) 0.6924(3) 0.46749(19) 0.0244(9) Uani 0.732(8) 1 d P A 1
H1A1 H 0.0793 0.7358 0.4546 0.037 Uiso 0.732(8) 1 calc PR A 1
H1A2 H 0.1273 0.6339 0.5029 0.037 Uiso 0.732(8) 1 calc PR A 1
H1A3 H 0.1490 0.6493 0.4286 0.037 Uiso 0.732(8) 1 calc PR A 1
N1B N 0.1616(7) 0.8431(9) 0.4308(5) 0.022(2) Uani 0.268(8) 1 d P A 2
H1B1 H 0.1581 0.7870 0.3930 0.033 Uiso 0.268(8) 1 calc PR A 2
H1B2 H 0.1955 0.9144 0.4221 0.033 Uiso 0.268(8) 1 calc PR A 2
H1B3 H 0.1034 0.8686 0.4366 0.033 Uiso 0.268(8) 1 calc PR A 2
C1 C 0.05125(18) 0.2560(2) 0.14771(14) 0.0154(5) Uani 1 1 d . . .
H1A H 0.0563 0.1947 0.1077 0.019 Uiso 1 1 calc R . .
H1B H 0.0386 0.2039 0.1895 0.019 Uiso 1 1 calc R . .
C2 C 0.12257(19) 0.2756(2) 0.39197(14) 0.0162(5) Uani 1 1 d . . .
H2A H 0.1360 0.2323 0.3476 0.019 Uiso 1 1 calc R . .
H2B H 0.1168 0.2067 0.4280 0.019 Uiso 1 1 calc R . .
C3 C 0.03043(19) 0.3485(3) 0.37515(14) 0.0172(5) Uani 1 1 d . . .
H3A H 0.0342 0.4121 0.3360 0.021 Uiso 1 1 calc R . .
H3B H 0.0194 0.3978 0.4184 0.021 Uiso 1 1 calc R . .
C4 C 0.2038(2) 0.7815(4) 0.49273(18) 0.0335(8) Uani 1 1 d . . .
H4A H 0.1897 0.8224 0.5376 0.040 Uiso 1 1 calc R A 1
H4B H 0.2051 0.8514 0.4565 0.040 Uiso 1 1 calc R A 1
H4 H 0.205(3) 0.706(5) 0.196(3) 0.036(15) 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
V1 0.0241(2) 0.0089(2) 0.0098(2) 0.00157(14) 0.00016(16) -0.00243(16)
V2 0.0388(3) 0.0122(2) 0.0094(2) 0.00016(15) -0.00087(18) -0.00773(19)
P1 0.0213(3) 0.0085(3) 0.0086(3) 0.0013(2) 0.0012(2) -0.0003(2)
P2 0.0243(3) 0.0071(3) 0.0084(3) -0.0009(2) 0.0009(2) 0.0021(2)
O1 0.0241(10) 0.0093(8) 0.0149(9) 0.0016(7) -0.0005(7) -0.0012(7)
O2 0.0384(12) 0.0115(9) 0.0112(9) 0.0015(7) 0.0050(8) -0.0013(8)
O3 0.0287(12) 0.0191(10) 0.0427(14) 0.0072(10) 0.0011(10) -0.0033(9)
O4 0.0710(19) 0.0112(10) 0.0105(9) 0.0017(8) -0.0018(10) -0.0096(11)
O5 0.0290(10) 0.0102(8) 0.0117(8) 0.0027(6) 0.0040(7) -0.0001(7)
O6 0.0348(11) 0.0124(8) 0.0108(8) -0.0010(7) 0.0038(8) -0.0062(8)
O7 0.0372(13) 0.0295(12) 0.0326(13) -0.0141(10) 0.0058(10) -0.0045(10)
O8 0.0249(10) 0.0141(9) 0.0159(9) -0.0044(7) 0.0024(7) -0.0032(7)
O9 0.0325(11) 0.0087(8) 0.0115(8) 0.0005(6) 0.0027(7) 0.0019(7)
O90 0.0595(18) 0.0314(14) 0.0508(17) 0.0054(12) -0.0004(14) -0.0036(13)
O91 0.0324(14) 0.0529(18) 0.071(2) 0.0033(16) 0.0109(14) 0.0128(13)
O92 0.170(7) 0.047(3) 0.136(6) 0.002(3) 0.117(5) -0.003(3)
N1A 0.0318(19) 0.0190(17) 0.0232(17) -0.0006(13) 0.0064(14) 0.0045(14)
N1B 0.033(5) 0.018(4) 0.015(4) 0.008(3) 0.006(4) 0.006(4)
C1 0.0213(12) 0.0108(11) 0.0138(11) -0.0013(9) 0.0015(9) -0.0001(9)
C2 0.0245(13) 0.0099(11) 0.0137(11) -0.0015(9) 0.0018(10) 0.0004(9)
C3 0.0238(13) 0.0108(11) 0.0159(12) -0.0012(9) -0.0006(10) 0.0002(10)
C4 0.043(2) 0.0339(18) 0.0238(15) -0.0004(13) 0.0067(14) 0.0178(16)
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
V1 O3 1.592(2) . ?
V1 O4 1.942(2) . ?
V1 O2 1.951(2) . ?
V1 O5 1.9657(18) . ?
V1 O1 1.9964(19) . ?
V2 O7 1.620(3) . ?
V2 O9 1.9760(19) . ?
V2 O4 1.978(2) . ?
V2 O6 1.980(2) . ?
V2 O8 1.9952(19) . ?
V2 O90 2.421(3) . ?
P1 O8 1.524(2) 4_545 ?
P1 O6 1.5251(19) . ?
P1 O5 1.5363(19) . ?
P1 C1 1.798(3) . ?
P2 O9 1.5258(19) . ?
P2 O2 1.5296(19) 6_566 ?
P2 O1 1.530(2) 4_545 ?
P2 C2 1.799(3) . ?
O1 P2 1.530(2) 4 ?
O2 P2 1.5296(19) 6_565 ?
O8 P1 1.524(2) 4 ?
N1A C4 1.397(5) . ?
N1B C4 1.382(9) . ?
C1 C3 1.530(4) 2 ?
C2 C3 1.527(4) . ?
C3 C1 1.530(4) 2 ?
C4 C4 1.481(6) 7_566 ?
|
1101204.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101204.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_1101204
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4.5 H16 N O10.5 P2 V2'
_chemical_formula_weight 416.00
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 104.4230(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.5527(7)
_cell_length_b 10.0841(5)
_cell_length_c 18.7813(8)
_cell_measurement_temperature 90(2)
_cell_volume 2852.7(2)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.937
_cod_duplicate_entry 1101182
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C4.50 H16 N O10.50 P2 V2'
_cod_database_code 1101204
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
V1 V 0.24928(2) -0.03062(3) 0.284885(17) 0.00895(8) Uani 1 1 d . . .
V2 V 0.16899(2) 0.10983(3) 0.585705(17) 0.00939(8) Uani 1 1 d . . .
P1 P 0.20151(3) 0.12821(5) 0.41982(3) 0.00907(10) Uani 1 1 d . . .
P2 P 0.16855(3) -0.18035(5) 0.65966(2) 0.00931(10) Uani 1 1 d . . .
O1 O 0.06449(10) 0.13500(15) 0.56742(9) 0.0178(3) Uani 1 1 d . . .
O2 O 0.18326(10) -0.08138(14) 0.60226(8) 0.0145(3) Uani 1 1 d . . .
O3 O 0.21634(9) 0.28922(14) 0.57836(7) 0.0127(3) Uani 1 1 d . . .
O4 O 0.20246(9) 0.06650(14) 0.49461(7) 0.0127(3) Uani 1 1 d . . .
O5 O 0.19472(9) 0.01211(13) 0.36587(7) 0.0119(3) Uani 1 1 d . . .
O6 O 0.17511(10) 0.11553(14) 0.23450(8) 0.0140(3) Uani 1 1 d . . .
O7 O 0.26455(9) -0.20658(14) 0.33479(8) 0.0137(3) Uani 1 1 d . . .
O8 O 0.34693(10) 0.02714(16) 0.29659(9) 0.0193(3) Uani 1 1 d . . .
O9 O 0.21641(12) -0.13252(16) 0.19255(8) 0.0195(3) Uani 1 1 d . . .
O90 O 0.3279(3) 0.8666(4) 0.50608(19) 0.1124(17) Uani 1 1 d . . .
O91 O 0.0402(6) 0.4526(8) 0.5262(5) 0.107(3) Uani 0.50 1 d P . .
N1 N 0.08492(14) 0.7910(2) 0.38176(13) 0.0294(5) Uani 1 1 d . . .
H1A H 0.1216 0.8541 0.3710 0.044 Uiso 1 1 calc R . .
H1B H 0.1164 0.7367 0.4176 0.044 Uiso 1 1 calc R . .
H1C H 0.0405 0.8306 0.3977 0.044 Uiso 1 1 calc R . .
C1 C 0.10549(13) 0.23119(19) 0.39149(11) 0.0137(4) Uani 1 1 d . . .
H1D H 0.1065 0.2987 0.4300 0.016 Uiso 1 1 calc R . .
H1E H 0.1084 0.2784 0.3460 0.016 Uiso 1 1 calc R . .
C2 C 0.01730(13) 0.1551(2) 0.37729(11) 0.0147(4) Uani 1 1 d . . .
H2A H 0.0096 0.1010 0.3321 0.018 Uiso 1 1 calc R . .
H2B H 0.0182 0.0945 0.4189 0.018 Uiso 1 1 calc R . .
C3 C 0.06012(13) -0.2520(2) 0.63152(12) 0.0160(4) Uani 1 1 d . . .
H3A H 0.0549 -0.2979 0.5840 0.019 Uiso 1 1 calc R . .
H3B H 0.0545 -0.3201 0.6681 0.019 Uiso 1 1 calc R . .
C4 C 0.04591(18) 0.7111(2) 0.31433(17) 0.0321(6) Uani 1 1 d . . .
H4A H 0.0025 0.6473 0.3252 0.039 Uiso 1 1 calc R . .
H4B H 0.0936 0.6598 0.3006 0.039 Uiso 1 1 calc R . .
C5 C 0.0000 0.7981(4) 0.2500 0.0319(8) Uani 1 2 d S . .
H5A H 0.0442 0.8556 0.2353 0.038 Uiso 0.50 1 calc PR . .
H5B H -0.0442 0.8556 0.2647 0.038 Uiso 0.50 1 calc PR . .
H2 H 0.227(2) -0.199(3) 0.2003(17) 0.027(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
V1 0.01076(15) 0.00869(15) 0.00807(14) 0.00096(10) 0.00361(11) 0.00036(10)
V2 0.01199(15) 0.00901(15) 0.00818(15) 0.00097(10) 0.00437(11) -0.00056(11)
P1 0.0125(2) 0.0080(2) 0.0073(2) 0.00043(15) 0.00358(16) -0.00059(16)
P2 0.0122(2) 0.0082(2) 0.0075(2) 0.00015(16) 0.00235(16) -0.00037(16)
O1 0.0147(7) 0.0163(7) 0.0247(8) 0.0019(6) 0.0092(6) 0.0000(5)
O2 0.0243(7) 0.0106(6) 0.0095(6) 0.0021(5) 0.0057(5) 0.0012(5)
O3 0.0145(6) 0.0106(6) 0.0134(6) 0.0009(5) 0.0040(5) -0.0029(5)
O4 0.0191(7) 0.0125(6) 0.0078(6) 0.0016(5) 0.0055(5) 0.0003(5)
O5 0.0178(7) 0.0099(6) 0.0097(6) -0.0011(5) 0.0064(5) -0.0023(5)
O6 0.0199(7) 0.0139(6) 0.0097(6) 0.0024(5) 0.0064(5) 0.0056(5)
O7 0.0145(6) 0.0110(6) 0.0171(7) 0.0040(5) 0.0068(5) 0.0019(5)
O8 0.0151(7) 0.0210(8) 0.0224(8) 0.0054(6) 0.0058(6) -0.0024(6)
O9 0.0387(9) 0.0101(7) 0.0091(6) 0.0002(5) 0.0046(6) 0.0061(6)
O90 0.178(4) 0.109(3) 0.075(2) 0.049(2) 0.078(2) 0.112(3)
O91 0.116(7) 0.071(5) 0.107(6) -0.028(4) -0.021(5) 0.026(4)
N1 0.0281(10) 0.0216(10) 0.0460(13) 0.0072(9) 0.0233(10) 0.0025(8)
C1 0.0136(8) 0.0113(8) 0.0160(9) 0.0010(7) 0.0031(7) 0.0006(7)
C2 0.0141(8) 0.0120(8) 0.0170(9) 0.0002(7) 0.0018(7) -0.0005(7)
C3 0.0144(9) 0.0121(9) 0.0195(9) -0.0025(7) 0.0009(7) 0.0004(7)
C4 0.0288(12) 0.0183(11) 0.0557(17) 0.0006(11) 0.0223(12) 0.0008(9)
C5 0.0289(17) 0.0223(16) 0.051(2) 0.000 0.0218(17) 0.000
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
V1 O8 1.5900(15) . ?
V1 O6 1.9632(14) . ?
V1 O5 1.9653(14) . ?
V1 O9 1.9705(15) . ?
V1 O7 1.9931(14) . ?
V2 O1 1.5956(15) . ?
V2 O2 1.9569(15) . ?
V2 O4 1.9576(14) . ?
V2 O3 1.9709(14) . ?
V2 O9 1.9713(15) 6_556 ?
P1 O3 1.5182(14) 7_556 ?
P1 O4 1.5331(14) . ?
P1 O5 1.5347(14) . ?
P1 C1 1.788(2) . ?
P2 O2 1.5276(14) . ?
P2 O7 1.5296(14) 7_546 ?
P2 O6 1.5304(14) 6_556 ?
P2 C3 1.789(2) . ?
O3 P1 1.5182(14) 7_556 ?
O6 P2 1.5304(14) 6 ?
O7 P2 1.5296(14) 7_546 ?
O9 V2 1.9712(15) 6 ?
O9 H2 0.69(3) . ?
O91 O91 1.683(15) 5_566 ?
N1 C4 1.496(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.536(3) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.528(3) 5_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.528(3) 5_556 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.519(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C4 1.519(4) 2 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
|
1101205.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101205.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_1101205
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C5 H16.5 N O10.25 P2 V2'
_chemical_formula_weight 418.51
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.5300(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.2003(11)
_cell_length_b 10.2122(7)
_cell_length_c 18.5903(13)
_cell_measurement_temperature 90(2)
_cell_volume 2805.7(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.982
_cod_duplicate_entry 1101183
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C5 H16.50 N O10.25 P2 V2'
_cod_database_code 1101205
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
V1 V 0.16025(4) 0.38417(6) 0.08394(3) 0.01194(16) Uani 1 1 d . . .
V2 V 0.25210(4) -0.04648(6) 0.21606(3) 0.01174(16) Uani 1 1 d . . .
P1 P 0.28636(6) 0.12163(9) 0.07779(5) 0.0111(2) Uani 1 1 d . . .
P2 P 0.33657(6) 0.16866(9) 0.33572(5) 0.0108(2) Uani 1 1 d . . .
O1 O 0.21142(19) 0.4257(3) -0.00013(14) 0.0158(5) Uani 1 1 d . . .
O2 O 0.17471(19) 0.5730(3) 0.10387(14) 0.0159(5) Uani 1 1 d . . .
O3 O 0.0539(2) 0.3647(3) 0.05904(18) 0.0242(6) Uani 1 1 d . . .
O4 O 0.2025(3) 0.3566(3) 0.19155(17) 0.0259(7) Uani 1 1 d . . .
O5 O 0.20186(18) 0.2008(3) 0.07841(15) 0.0163(5) Uani 1 1 d . . .
O6 O 0.29019(19) -0.0014(3) 0.12580(14) 0.0154(5) Uani 1 1 d . . .
O7 O 0.23296(18) -0.2219(3) 0.16968(15) 0.0164(5) Uani 1 1 d . . .
O8 O 0.1526(2) 0.0052(3) 0.2138(2) 0.0291(7) Uani 1 1 d . . .
O9 O 0.32841(18) 0.1006(3) 0.26113(14) 0.0149(5) Uani 1 1 d . . .
O90 O 0.0431(9) 0.0279(15) 0.0189(9) 0.038(4) Uani 0.25 1 d P . .
O91 O 0.8270(10) 0.2940(6) 0.0371(5) 0.188(6) Uani 1 1 d . . .
C1 C 0.3840(2) 0.2210(4) 0.1123(2) 0.0139(7) Uani 1 1 d . . .
H1D H 0.3860 0.2909 0.0758 0.017 Uiso 1 1 calc R . .
H1E H 0.3776 0.2637 0.1586 0.017 Uiso 1 1 calc R . .
C2 C 0.4468(3) 0.2411(4) 0.3599(2) 0.0162(7) Uani 1 1 d . . .
H2A H 0.4524 0.3028 0.3201 0.019 Uiso 1 1 calc R . .
H2B H 0.4517 0.2929 0.4056 0.019 Uiso 1 1 calc R . .
C3 C 0.5263(3) 0.1465(4) 0.3722(2) 0.0160(7) Uani 1 1 d . . .
H3A H 0.5213 0.0911 0.3277 0.019 Uiso 1 1 calc R . .
H3B H 0.5248 0.0885 0.4145 0.019 Uiso 1 1 calc R . .
N1 N 0.8937(18) 0.125(3) 0.0823(10) 0.352(14) Uani 1 1 d DU . .
H1A H 0.8360 0.1210 0.0882 0.527 Uiso 1 1 calc R . .
H1B H 0.9050 0.0535 0.0566 0.527 Uiso 1 1 calc R . .
H1C H 0.9009 0.1989 0.0570 0.527 Uiso 1 1 calc R . .
C4 C 0.9602(9) 0.1272(15) 0.1587(10) 0.198(10) Uani 1 1 d D . .
H4A1 H 0.9519 0.0431 0.1828 0.237 Uiso 1 1 calc R . .
H4A2 H 1.0216 0.1246 0.1493 0.237 Uiso 1 1 calc R . .
C5 C 0.9624(5) 0.2341(7) 0.2173(4) 0.0616(19) Uani 1 1 d D . .
H5A H 0.9620 0.3201 0.1926 0.074 Uiso 1 1 calc R . .
H5B H 0.9055 0.2278 0.2343 0.074 Uiso 1 1 calc R . .
H4 H 0.214(4) 0.294(6) 0.196(3) 0.019(14) 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
V1 0.0141(3) 0.0136(3) 0.0092(3) -0.0014(2) 0.0050(2) 0.0016(2)
V2 0.0131(3) 0.0134(3) 0.0098(3) -0.0028(2) 0.0048(2) -0.0022(2)
P1 0.0148(4) 0.0115(4) 0.0071(4) -0.0007(3) 0.0030(3) 0.0012(3)
P2 0.0133(4) 0.0115(4) 0.0074(4) 0.0006(3) 0.0022(3) -0.0005(3)
O1 0.0216(13) 0.0180(13) 0.0090(11) -0.0013(10) 0.0059(10) -0.0015(11)
O2 0.0266(14) 0.0132(12) 0.0090(11) -0.0014(10) 0.0067(10) -0.0005(11)
O3 0.0184(14) 0.0246(15) 0.0314(17) -0.0075(13) 0.0098(12) 0.0002(12)
O4 0.053(2) 0.0152(15) 0.0103(13) -0.0001(12) 0.0082(13) 0.0078(15)
O5 0.0168(13) 0.0172(13) 0.0156(13) 0.0000(10) 0.0054(10) 0.0034(10)
O6 0.0246(14) 0.0122(12) 0.0108(11) 0.0002(10) 0.0072(10) 0.0021(11)
O7 0.0180(13) 0.0147(13) 0.0180(13) -0.0047(10) 0.0075(10) -0.0031(10)
O8 0.0188(14) 0.0285(16) 0.0424(19) -0.0182(15) 0.0121(13) -0.0029(13)
O9 0.0201(13) 0.0169(13) 0.0083(11) -0.0020(10) 0.0045(10) -0.0067(10)
O90 0.023(7) 0.033(8) 0.055(10) 0.014(7) -0.001(6) 0.000(6)
O91 0.461(18) 0.034(3) 0.140(7) -0.007(4) 0.214(10) -0.012(6)
C1 0.0152(16) 0.0114(16) 0.0145(17) -0.0030(13) 0.0024(13) 0.0007(13)
C2 0.0168(17) 0.0120(16) 0.0179(17) -0.0019(14) 0.0002(14) -0.0015(14)
C3 0.0183(18) 0.0130(16) 0.0147(17) -0.0004(14) -0.0003(14) -0.0017(14)
N1 0.352(14) 0.352(14) 0.352(14) 0.0004(10) 0.083(3) 0.0000(10)
C4 0.084(9) 0.149(13) 0.32(2) -0.158(15) -0.041(12) 0.006(8)
C5 0.077(5) 0.042(3) 0.077(5) -0.001(3) 0.038(4) -0.004(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
V1 O3 1.586(3) . ?
V1 O1 1.948(3) . ?
V1 O2 1.966(3) . ?
V1 O4 1.973(3) . ?
V1 O5 1.987(3) . ?
V2 O8 1.593(3) . ?
V2 O6 1.954(3) . ?
V2 O9 1.962(3) . ?
V2 O4 1.963(3) 4_545 ?
V2 O7 1.980(3) . ?
P1 O5 1.520(3) . ?
P1 O1 1.530(3) 7 ?
P1 O6 1.534(3) . ?
P1 C1 1.788(4) . ?
P2 O7 1.525(3) 4 ?
P2 O2 1.528(3) 4_545 ?
P2 O9 1.530(3) . ?
P2 C2 1.790(4) . ?
O1 P1 1.530(3) 7 ?
O2 P2 1.528(3) 4 ?
O4 V2 1.963(3) 4 ?
O4 H4 0.66(6) . ?
O7 P2 1.525(3) 4_545 ?
O90 O90 1.45(3) 5 ?
C1 C3 1.528(5) 2_655 ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.521(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C1 1.528(5) 2_655 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N1 C4 1.537(10) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C4 C5 1.536(8) . ?
C4 H4A1 0.9900 . ?
C4 H4A2 0.9900 . ?
C5 C5 1.462(16) 2_755 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
|
1101206.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101206.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_1101206
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C5.5 H16 N O9.5 P2 V2'
_chemical_formula_weight 412.01
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.328(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.712(1)
_cell_length_b 10.030(1)
_cell_length_c 18.656(2)
_cell_measurement_temperature 90(2)
_cell_volume 2861.0(5)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.913
_cod_duplicate_entry 1101184
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C5.50 H16 N O9.50 P2 V2'
_cod_database_code 1101206
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
O91 O 0.0896(8) 0.5117(12) 0.0101(6) 0.093(4) Uani 0.50 1 d P . .
V1 V 0.16272(4) 0.11690(5) 0.08371(3) 0.01463(14) Uani 1 1 d . . .
V2 V 0.24588(4) 0.04224(5) 0.28392(3) 0.01517(14) Uani 1 1 d . . .
P1 P 0.15956(6) -0.17215(8) 0.16288(4) 0.01515(18) Uani 1 1 d . . .
P2 P 0.29416(6) 0.37877(8) 0.07898(4) 0.01508(18) Uani 1 1 d . . .
O1 O 0.20269(17) 0.0005(2) 0.37129(13) 0.0206(5) Uani 1 1 d . . .
O2 O 0.34031(19) -0.0210(3) 0.29084(18) 0.0351(7) Uani 1 1 d . . .
O3 O 0.27184(17) 0.2185(2) 0.33165(14) 0.0222(5) Uani 1 1 d . . .
O4 O 0.16691(18) -0.1013(3) 0.23618(14) 0.0241(5) Uani 1 1 d . . .
O5 O 0.2109(2) 0.1415(3) 0.19037(15) 0.0297(7) Uani 1 1 d . . .
O6 O 0.16827(18) -0.0766(2) 0.10163(13) 0.0222(5) Uani 1 1 d . . .
O7 O 0.05983(18) 0.1473(3) 0.06266(17) 0.0303(6) Uani 1 1 d . . .
O8 O 0.20081(18) 0.0677(2) -0.00404(13) 0.0222(5) Uani 1 1 d . . .
O9 O 0.21103(16) 0.2981(2) 0.07550(14) 0.0211(5) Uani 1 1 d . . .
N1A N 0.8388(7) 0.2197(5) 0.0419(4) 0.071(3) Uani 0.65 1 d P . .
H1A' H 0.8522 0.1471 0.0697 0.107 Uiso 0.50 1 calc PR . .
H1B' H 0.8598 0.2117 0.0017 0.107 Uiso 0.50 1 calc PR . .
H1C' H 0.7809 0.2288 0.0289 0.107 Uiso 0.50 1 calc PR . .
N1B N 0.9993(7) 0.3790(11) 0.1222(6) 0.027(2) Uani 0.35 1 d P . .
H1D' H 1.0498 0.4142 0.1462 0.040 Uiso 0.50 1 calc PR . .
H1E' H 0.9742 0.4329 0.0855 0.040 Uiso 0.50 1 calc PR . .
H1F' H 1.0091 0.2999 0.1040 0.040 Uiso 0.50 1 calc PR . .
C1 C 0.0528(2) -0.2480(4) 0.1397(2) 0.0233(7) Uani 1 1 d . . .
H1A H 0.0479 -0.2995 0.0949 0.028 Uiso 1 1 calc R . .
H1B H 0.0481 -0.3097 0.1786 0.028 Uiso 1 1 calc R . .
C2 C -0.0240(2) -0.1508(4) 0.1283(2) 0.0247(7) Uani 1 1 d . . .
H2A H -0.0226 -0.0929 0.0870 0.030 Uiso 1 1 calc R . .
H2B H -0.0184 -0.0956 0.1718 0.030 Uiso 1 1 calc R . .
C3 C 0.3878(2) 0.2749(3) 0.1135(2) 0.0225(7) Uani 1 1 d . . .
H3A H 0.3815 0.2335 0.1589 0.027 Uiso 1 1 calc R . .
H3B H 0.3888 0.2043 0.0782 0.027 Uiso 1 1 calc R . .
C4A C 0.9583(4) 0.2533(5) 0.2184(3) 0.0514(13) Uani 1 1 d . . .
H4A1 H 0.9574 0.1714 0.1906 0.062 Uiso 1 1 calc R . .
H4A2 H 0.9078 0.2516 0.2402 0.062 Uiso 1 1 calc R . .
C5 C 0.9480(7) 0.3645(11) 0.1670(7) 0.088(3) Uani 1 1 d . . .
C6 C 0.8797(7) 0.3442(10) 0.0863(6) 0.042(2) Uani 0.50 1 d P . .
H6A H 0.8294 0.3979 0.0899 0.051 Uiso 0.50 1 calc PR . .
H6B H 0.9073 0.3917 0.0525 0.051 Uiso 0.50 1 calc PR . .
H5A H 0.975(3) 0.360(5) 0.138(3) 0.000(12) Uiso 1 1 d . . .
H5B H 0.946(7) 0.454(12) 0.184(6) 0.13(4) Uiso 1 1 d . . .
H5' H 0.218(4) 0.198(6) 0.194(3) 0.030(17) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O91 0.091(8) 0.105(8) 0.066(6) -0.021(6) -0.017(5) 0.060(7)
V1 0.0187(3) 0.0138(3) 0.0124(3) 0.00116(18) 0.0057(2) -0.00002(19)
V2 0.0193(3) 0.0143(3) 0.0128(3) -0.00079(19) 0.0055(2) -0.0004(2)
P1 0.0199(4) 0.0131(4) 0.0123(4) 0.0002(3) 0.0034(3) -0.0007(3)
P2 0.0209(4) 0.0134(4) 0.0119(4) 0.0002(3) 0.0056(3) -0.0007(3)
O1 0.0323(13) 0.0176(11) 0.0144(11) 0.0025(9) 0.0102(10) 0.0031(10)
O2 0.0269(14) 0.0386(16) 0.0405(17) -0.0078(13) 0.0094(13) 0.0077(12)
O3 0.0226(12) 0.0196(12) 0.0254(13) -0.0054(10) 0.0077(10) -0.0028(10)
O4 0.0350(14) 0.0226(12) 0.0168(12) -0.0052(9) 0.0104(10) -0.0105(11)
O5 0.057(2) 0.0159(14) 0.0147(12) 0.0005(10) 0.0060(12) -0.0091(13)
O6 0.0382(14) 0.0150(11) 0.0144(11) 0.0020(9) 0.0085(10) 0.0020(10)
O7 0.0227(13) 0.0297(14) 0.0397(16) 0.0015(12) 0.0099(12) 0.0014(11)
O8 0.0375(14) 0.0181(11) 0.0138(11) 0.0012(9) 0.0119(10) 0.0007(10)
O9 0.0240(12) 0.0169(11) 0.0228(12) 0.0007(9) 0.0061(10) -0.0034(9)
N1A 0.176(9) 0.012(2) 0.055(4) -0.019(3) 0.087(5) -0.040(4)
N1B 0.024(5) 0.033(5) 0.030(5) 0.001(4) 0.020(4) -0.006(4)
C1 0.0211(16) 0.0190(16) 0.0285(18) -0.0030(13) 0.0028(14) -0.0017(13)
C2 0.0199(16) 0.0218(17) 0.0303(19) 0.0006(14) 0.0017(14) 0.0010(13)
C3 0.0236(17) 0.0171(15) 0.0259(18) 0.0027(13) 0.0037(14) 0.0011(13)
C4A 0.052(3) 0.040(3) 0.064(4) -0.005(2) 0.016(3) -0.007(2)
C5 0.070(6) 0.067(5) 0.111(8) 0.035(5) -0.013(5) -0.022(4)
C6 0.040(5) 0.033(5) 0.053(6) 0.001(4) 0.009(4) -0.001(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
V1 O7 1.603(3) . ?
V1 O8 1.932(3) . ?
V1 O6 1.968(3) . ?
V1 O5 1.975(3) . ?
V1 O9 1.989(3) . ?
V2 O2 1.591(3) . ?
V2 O1 1.950(3) . ?
V2 O4 1.974(3) . ?
V2 O5 1.974(3) . ?
V2 O3 1.979(3) . ?
P1 O6 1.521(3) . ?
P1 O4 1.522(3) . ?
P1 O3 1.524(3) 4_545 ?
P1 C1 1.801(4) . ?
P2 O8 1.516(3) 7 ?
P2 O9 1.525(3) . ?
P2 O1 1.527(3) 4 ?
P2 C3 1.797(4) . ?
O1 P2 1.527(3) 4_545 ?
O3 P1 1.524(3) 4 ?
O8 P2 1.516(3) 7 ?
N1A C6 1.554(11) . ?
N1B C5 1.297(15) . ?
C1 C2 1.527(5) . ?
C2 C3 1.541(5) 3_445 ?
C3 C2 1.541(5) 3 ?
C4A C5 1.455(10) . ?
C4A C4A 1.549(12) 2_755 ?
C5 C6 1.648(15) . ?
|
1101207.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101207.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_1101207
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C6 H16.5 N O9.25 P2 V2'
_chemical_formula_weight 414.52
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 105.4840(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.6403(11)
_cell_length_b 10.2112(7)
_cell_length_c 18.6795(14)
_cell_measurement_temperature 90(2)
_cell_volume 2875.0(4)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.915
_cod_duplicate_entry 1101185
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C6 H16.50 N O9.25 P2 V2'
_cod_database_code 1101207
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
V1 V 0.16504(4) 0.38063(6) 0.08450(3) 0.01129(16) Uani 1 1 d . . .
V2 V 0.24827(4) 0.45311(6) 0.28748(3) 0.01168(16) Uani 1 1 d . . .
P1 P 0.20739(7) 0.37992(9) -0.07875(5) 0.0116(2) Uani 1 1 d . . .
P2 P 0.16413(6) 0.66770(9) 0.16281(5) 0.0113(2) Uani 1 1 d . . .
O1 O 0.2074(2) 0.4273(3) -0.00107(15) 0.0162(6) Uani 1 1 d . . .
O2 O 0.21134(19) 0.2014(3) 0.07871(15) 0.0149(5) Uani 1 1 d . . .
O3 O 0.0607(2) 0.3543(3) 0.05918(18) 0.0210(6) Uani 1 1 d . . .
O4 O 0.1716(2) 0.5712(3) 0.10203(14) 0.0154(5) Uani 1 1 d . . .
O5 O 0.2117(2) 0.3571(3) 0.19244(16) 0.0208(6) Uani 1 1 d . . .
O6 O 0.1758(2) 0.6015(3) 0.23814(15) 0.0161(6) Uani 1 1 d . . .
O7 O 0.3460(2) 0.5075(3) 0.29949(19) 0.0254(7) Uani 1 1 d . . .
O8 O 0.26885(18) 0.2777(3) 0.33434(15) 0.0151(5) Uani 1 1 d . . .
O9 O 0.20363(19) 0.4966(3) 0.37359(14) 0.0143(5) Uani 1 1 d . . .
O90 O 0.5626(10) 0.5383(13) 0.0310(9) 0.033(3) Uani 0.25 1 d P . .
N1 N 0.3611(8) 0.8064(6) 0.0428(4) 0.113(4) Uani 1 1 d . A 1
H1A' H 0.3009 0.7994 0.0275 0.169 Uiso 1 1 calc R A 1
H1B' H 0.3814 0.8416 0.0057 0.169 Uiso 1 1 calc R A 1
H1C' H 0.3767 0.8590 0.0835 0.169 Uiso 1 1 calc R A 1
C4 C 0.410(2) 0.6444(17) 0.0662(13) 0.33(2) Uani 1 1 d . . .
H4A H 0.3658 0.5774 0.0417 0.393 Uiso 1 1 calc R A 1
H4B H 0.4619 0.6357 0.0462 0.393 Uiso 1 1 calc R A 1
C1 C 0.1100(3) 0.2824(4) -0.1147(2) 0.0149(7) Uani 1 1 d . . .
H1A H 0.1136 0.2427 -0.1622 0.018 Uiso 1 1 calc R . .
H1B H 0.1099 0.2101 -0.0795 0.018 Uiso 1 1 calc R . .
C2 C 0.0553(3) 0.7388(4) 0.1385(2) 0.0168(7) Uani 1 1 d . . .
H2A H 0.0518 0.8023 0.1776 0.020 Uiso 1 1 calc R . .
H2B H 0.0476 0.7885 0.0917 0.020 Uiso 1 1 calc R . .
C3 C -0.0218(3) 0.6431(4) 0.1284(2) 0.0168(7) Uani 1 1 d . . .
H3A H -0.0131 0.5880 0.1733 0.020 Uiso 1 1 calc R . .
H3B H -0.0234 0.5849 0.0856 0.020 Uiso 1 1 calc R . .
C5 C 0.4404(10) 0.6150(10) 0.1565(11) 0.151(8) Uani 1 1 d . A .
H5A H 0.3875 0.5880 0.1724 0.181 Uiso 1 1 calc R . .
H5B H 0.4824 0.5404 0.1659 0.181 Uiso 1 1 calc R . .
C6 C 0.4831(9) 0.7274(11) 0.2035(7) 0.110(5) Uani 1 1 d . . .
H6A H 0.4413 0.8017 0.1896 0.132 Uiso 1 1 calc R A .
H6B H 0.5358 0.7507 0.1863 0.132 Uiso 1 1 calc R . .
H5 H 0.217(4) 0.290(7) 0.196(4) 0.032(18) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0153(3) 0.0120(3) 0.0075(3) -0.0011(2) 0.0046(2) 0.0001(2)
V2 0.0153(3) 0.0123(3) 0.0084(3) 0.0006(2) 0.0048(2) 0.0005(2)
P1 0.0184(5) 0.0107(4) 0.0069(4) -0.0006(3) 0.0054(3) -0.0001(3)
P2 0.0166(4) 0.0107(4) 0.0067(4) -0.0002(3) 0.0034(3) 0.0008(3)
O1 0.0269(15) 0.0157(13) 0.0080(12) -0.0014(10) 0.0082(10) -0.0020(11)
O2 0.0197(13) 0.0128(12) 0.0128(12) -0.0011(10) 0.0052(10) 0.0011(10)
O3 0.0172(14) 0.0221(15) 0.0249(15) -0.0021(12) 0.0077(12) 0.0006(12)
O4 0.0264(15) 0.0126(12) 0.0071(11) -0.0013(9) 0.0044(10) 0.0010(11)
O5 0.0425(19) 0.0121(14) 0.0076(12) 0.0002(10) 0.0066(12) 0.0053(13)
O6 0.0258(15) 0.0152(13) 0.0087(12) 0.0020(10) 0.0069(10) 0.0061(11)
O7 0.0203(15) 0.0251(16) 0.0325(17) 0.0043(13) 0.0098(13) -0.0031(12)
O8 0.0181(13) 0.0146(13) 0.0136(12) 0.0023(10) 0.0063(10) 0.0014(10)
O9 0.0227(14) 0.0126(12) 0.0097(12) -0.0007(9) 0.0078(10) -0.0006(10)
O90 0.031(7) 0.021(7) 0.040(8) -0.001(6) -0.002(6) -0.005(6)
N1 0.275(13) 0.033(3) 0.056(4) 0.011(3) 0.090(6) 0.048(5)
C4 0.67(5) 0.162(16) 0.32(3) -0.183(18) 0.44(4) -0.25(3)
C1 0.0178(17) 0.0122(16) 0.0151(17) -0.0018(13) 0.0048(13) -0.0006(14)
C2 0.0167(17) 0.0149(17) 0.0176(18) 0.0006(14) 0.0027(14) 0.0011(14)
C3 0.0207(19) 0.0146(17) 0.0147(17) 0.0003(14) 0.0041(14) -0.0008(14)
C5 0.134(11) 0.049(6) 0.33(2) -0.011(9) 0.157(15) -0.006(6)
C6 0.138(10) 0.076(7) 0.153(12) -0.032(7) 0.105(10) -0.024(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.595(3) . ?
V1 O1 1.946(3) . ?
V1 O5 1.967(3) . ?
V1 O4 1.971(3) . ?
V1 O2 1.981(3) . ?
V2 O7 1.585(3) . ?
V2 O9 1.968(3) . ?
V2 O6 1.968(3) . ?
V2 O5 1.974(3) . ?
V2 O8 1.982(3) . ?
P1 O2 1.518(3) 7 ?
P1 O1 1.530(3) . ?
P1 O9 1.536(3) 6_565 ?
P1 C1 1.793(4) . ?
P2 O8 1.528(3) 4 ?
P2 O6 1.528(3) . ?
P2 O4 1.531(3) . ?
P2 C2 1.794(4) . ?
O2 P1 1.518(3) 7 ?
O8 P2 1.528(3) 4_545 ?
O9 P1 1.536(3) 6_566 ?
N1 C4 1.82(3) . ?
C4 C5 1.65(3) . ?
C1 C3 1.536(5) 5_565 ?
C2 C3 1.523(5) . ?
C3 C1 1.536(5) 5_565 ?
C5 C6 1.489(18) . ?
|
1101208.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101208.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_1101208
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C6.5 H17 N O9 P2 V2'
_chemical_formula_weight 417.03
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 104.292(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.8220(15)
_cell_length_b 10.0614(9)
_cell_length_c 18.6103(17)
_cell_measurement_temperature 90(2)
_cell_volume 2870.9(5)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.930
_cod_duplicate_entry 1101186
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C6.50 H17 N O9 P2 V2'
_cod_database_code 1101208
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
V1 V 0.16162(3) 0.12474(5) 1.08518(3) 0.01265(13) Uani 1 1 d . . .
V2A V 0.24245(5) -0.05144(6) 0.78521(3) 0.0148(2) Uani 0.927(3) 1 d P . 1
V2B V 0.1914(6) -0.0851(7) 0.7809(4) 0.011(2) Uani 0.073(3) 1 d PU . 2
P1 P 0.34231(5) -0.33367(8) 0.83475(4) 0.01223(17) Uani 1 1 d . . .
P2 P 0.20657(5) 0.11775(8) 0.92207(4) 0.01194(17) Uani 1 1 d . . .
O1 O 0.27403(15) -0.2261(2) 0.83275(13) 0.0187(5) Uani 1 1 d . . .
O2 O 0.33535(19) 0.0112(3) 0.78992(18) 0.0390(8) Uani 1 1 d . . .
O3 O 0.16690(17) 0.0958(2) 0.73934(12) 0.0213(5) Uani 1 1 d . . .
O4 O 0.20289(15) -0.0091(2) 0.87543(12) 0.0148(5) Uani 1 1 d . . .
O5 O 0.20314(15) 0.0706(2) 0.99957(12) 0.0152(5) Uani 1 1 d . . .
O6 O 0.16279(15) -0.0691(2) 1.10272(12) 0.0155(5) Uani 1 1 d . . .
O7 O 0.21258(15) 0.3015(2) 1.07786(12) 0.0161(5) Uani 1 1 d . . .
O8 O 0.05960(16) 0.1551(3) 1.05947(15) 0.0223(5) Uani 1 1 d . . .
O9 O 0.2040(2) 0.1481(3) 1.19204(15) 0.0305(7) Uani 1 1 d . . .
N1 N 0.87734(19) 0.1878(3) 0.04188(16) 0.0205(6) Uani 1 1 d . . .
H1A H 0.9346 0.1641 0.0519 0.031 Uiso 1 1 calc R . .
H1B H 0.8498 0.1602 -0.0046 0.031 Uiso 1 1 calc R . .
H1C H 0.8519 0.1491 0.0755 0.031 Uiso 1 1 calc R . .
C1 C 0.4485(2) -0.2575(3) 0.85697(18) 0.0161(6) Uani 1 1 d . . .
H1D H 0.4528 -0.1977 0.8157 0.019 Uiso 1 1 calc R . .
H1E H 0.4541 -0.2019 0.9018 0.019 Uiso 1 1 calc R . .
C2 C 0.1123(2) 0.2188(3) 0.88590(18) 0.0147(6) Uani 1 1 d . . .
H2A H 0.1112 0.2915 0.9215 0.018 Uiso 1 1 calc R . .
H2B H 0.1181 0.2600 0.8391 0.018 Uiso 1 1 calc R . .
C3 C 0.0249(2) 0.1449(3) 0.87076(18) 0.0153(6) Uani 1 1 d . . .
H3A H 0.0191 0.0869 0.8269 0.018 Uiso 1 1 calc R . .
H3B H 0.0234 0.0879 0.9138 0.018 Uiso 1 1 calc R . .
C4 C 0.8704(4) 0.3337(5) 0.0465(3) 0.0552(16) Uani 1 1 d . . .
H4A H 0.8952 0.3744 0.0078 0.066 Uiso 1 1 calc R . .
H4B H 0.8079 0.3582 0.0355 0.066 Uiso 1 1 calc R . .
C5 C 0.9135(4) 0.3884(5) 0.1167(3) 0.0541(15) Uani 1 1 d . . .
H5A H 0.8692 0.4440 0.1317 0.065 Uiso 1 1 calc R . .
H5B H 0.9573 0.4509 0.1062 0.065 Uiso 1 1 calc R . .
C6 C 0.9572(6) 0.3189(6) 0.1821(3) 0.096(3) Uani 1 1 d . . .
H6A H 1.0018 0.2623 0.1682 0.115 Uiso 1 1 calc R . .
H6B H 0.9138 0.2579 0.1945 0.115 Uiso 1 1 calc R . .
C7 C 1.0000 0.3851(7) 0.2500 0.0410(15) Uani 1 2 d S . .
H7A H 1.0444 0.4441 0.2375 0.049 Uiso 0.50 1 calc PR . .
H7B H 0.9556 0.4441 0.2625 0.049 Uiso 0.50 1 calc PR . .
H9 H 0.215(3) 0.205(5) 1.196(3) 0.020(14) 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
V1 0.0126(3) 0.0151(3) 0.0106(2) 0.00085(19) 0.00347(19) -0.0017(2)
V2A 0.0150(4) 0.0182(3) 0.0114(3) 0.0031(2) 0.0037(2) 0.0048(3)
V2B 0.011(3) 0.009(3) 0.012(3) 0.0013(18) -0.0003(19) -0.0041(19)
P1 0.0142(4) 0.0137(4) 0.0083(3) 0.0009(3) 0.0018(3) -0.0002(3)
P2 0.0132(4) 0.0126(4) 0.0099(3) 0.0007(3) 0.0027(3) -0.0011(3)
O1 0.0175(11) 0.0206(12) 0.0173(11) 0.0057(9) 0.0027(9) 0.0060(9)
O2 0.0273(15) 0.0438(19) 0.0450(18) 0.0166(15) 0.0070(13) -0.0005(14)
O3 0.0340(14) 0.0207(12) 0.0101(10) 0.0029(9) 0.0076(10) 0.0094(11)
O4 0.0185(11) 0.0143(11) 0.0119(10) 0.0014(8) 0.0043(8) -0.0009(9)
O5 0.0175(11) 0.0180(11) 0.0111(10) 0.0019(8) 0.0054(8) 0.0011(9)
O6 0.0212(12) 0.0151(11) 0.0098(10) 0.0020(8) 0.0031(9) -0.0010(9)
O7 0.0153(11) 0.0172(11) 0.0163(11) 0.0007(9) 0.0050(9) -0.0032(9)
O8 0.0158(12) 0.0216(13) 0.0315(14) -0.0017(10) 0.0093(10) -0.0018(10)
O9 0.056(2) 0.0187(15) 0.0133(12) -0.0004(11) 0.0020(12) -0.0139(14)
N1 0.0199(14) 0.0226(15) 0.0194(14) 0.0000(12) 0.0055(11) 0.0000(12)
C1 0.0172(15) 0.0132(14) 0.0160(15) 0.0016(12) 0.0005(12) -0.0003(12)
C2 0.0159(15) 0.0125(14) 0.0159(15) 0.0024(11) 0.0043(12) -0.0014(12)
C3 0.0169(15) 0.0124(15) 0.0152(14) 0.0019(11) 0.0014(12) 0.0002(12)
C4 0.101(5) 0.024(2) 0.031(2) 0.0017(19) 0.000(3) 0.026(3)
C5 0.072(4) 0.025(2) 0.049(3) 0.001(2) -0.015(3) 0.000(2)
C6 0.185(9) 0.042(3) 0.033(3) -0.010(3) -0.024(4) 0.013(4)
C7 0.033(3) 0.041(4) 0.046(4) 0.000 0.005(3) 0.000
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
V1 O8 1.596(3) . ?
V1 O5 1.945(2) . ?
V1 O9 1.950(3) . ?
V1 O7 1.971(2) . ?
V1 O6 1.977(2) . ?
V2A O2 1.582(3) . ?
V2A O9 1.950(3) 6 ?
V2A O3 1.962(2) . ?
V2A O1 1.975(2) . ?
V2A O4 1.978(2) . ?
V2B O9 1.827(8) 6 ?
V2B O4 1.886(8) . ?
V2B O3 1.979(8) . ?
V2B O1 2.008(8) . ?
P1 O1 1.523(2) . ?
P1 O3 1.525(2) 4_546 ?
P1 O6 1.538(2) 7_547 ?
P1 C1 1.800(3) . ?
P2 O7 1.515(2) 7_557 ?
P2 O5 1.532(2) . ?
P2 O4 1.537(2) . ?
P2 C2 1.794(3) . ?
O3 P1 1.525(2) 4_556 ?
O6 P1 1.538(2) 7_547 ?
O7 P2 1.515(2) 7_557 ?
O9 V2B 1.827(8) 6_556 ?
O9 V2A 1.950(3) 6_556 ?
O9 H9 0.59(5) . ?
N1 C4 1.476(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C3 1.529(4) 3_545 ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.533(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C1 1.529(4) 3_455 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.426(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.427(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.441(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C6 1.441(6) 2_755 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
|
1101209.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101209.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_1101209
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4.5 H12.75 N O9 P2 V2'
_chemical_formula_weight 388.73
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.5240(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.2345(10)
_cell_length_b 10.1817(6)
_cell_length_c 18.6968(12)
_cell_measurement_temperature 90(2)
_cell_volume 2819.7(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.831
_cod_duplicate_entry 1101187
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C4.50 H12.75 N O9 P2 V2'
_cod_database_code 1101209
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
V1A V 0.75200(8) -0.04720(8) 0.21718(4) 0.0152(3) Uani 0.898(5) 1 d P . 1
O2 O 0.6543(2) 0.0084(3) 0.2165(2) 0.0351(9) Uani 0.898(5) 1 d P . 1
V1B V 0.8047(10) -0.0750(7) 0.2187(3) 0.027(4) Uani 0.102(5) 1 d P . 2
O2B O 0.9094(17) -0.123(3) 0.2292(16) 0.028(7) Uani 0.102(5) 1 d P . 2
V2 V 0.66193(4) 0.38449(5) 0.08390(3) 0.01656(16) Uani 1 1 d . . .
P1 P 0.66171(6) -0.33276(8) 0.16590(5) 0.0162(2) Uani 1 1 d . . .
P2 P 0.78554(7) 0.11826(8) 0.07647(5) 0.0169(2) Uani 1 1 d . . .
O1 O 0.73127(18) -0.2227(2) 0.17113(14) 0.0231(6) Uani 1 1 d . . .
O3 O 0.8302(2) 0.0982(2) 0.26029(13) 0.0242(6) Uani 1 1 d . . .
O4 O 0.78635(19) -0.0033(2) 0.12477(13) 0.0213(5) Uani 1 1 d . . .
O5 O 0.70163(18) 0.2009(2) 0.07478(14) 0.0205(5) Uani 1 1 d . . .
O6 O 0.7048(3) 0.3551(3) 0.19028(15) 0.0333(8) Uani 1 1 d . . .
O7 O 0.55530(19) 0.3646(3) 0.05936(17) 0.0299(6) Uani 1 1 d . . .
O8 O 0.67459(19) 0.5735(2) 0.10537(13) 0.0207(5) Uani 1 1 d . . .
O9 O 0.71048(19) 0.4320(3) -0.00036(13) 0.0227(6) Uani 1 1 d . . .
C1 C 0.5521(3) -0.2609(4) 0.1419(2) 0.0231(7) Uani 1 1 d . . .
N1 N 0.2641(9) 0.2766(12) 0.0180(7) 0.074(4) Uani 0.50 1 d PD . .
H1A H 0.5458 -0.2008 0.1820 0.028 Uiso 1 1 calc R . .
H1B H 0.5477 -0.2071 0.0971 0.028 Uiso 1 1 calc R . .
C2 C 0.4727(3) -0.3569(3) 0.1277(2) 0.0216(7) Uani 1 1 d . . .
H2A H 0.4769 -0.4136 0.1714 0.026 Uiso 1 1 calc R . .
H2B H 0.4755 -0.4139 0.0854 0.026 Uiso 1 1 calc R . .
C3 C 0.8826(3) 0.2173(3) 0.1114(2) 0.0203(7) Uani 1 1 d . . .
H3A H 0.8849 0.2876 0.0753 0.024 Uiso 1 1 calc R . .
H3B H 0.8755 0.2601 0.1573 0.024 Uiso 1 1 calc R . .
N2 N 0.4051(12) 0.2896(10) 0.1091(14) 0.176(12) Uani 0.50 1 d PD . .
C4 C 0.3468(10) 0.2035(15) 0.0188(9) 0.084(5) Uani 0.50 1 d PD . .
C5 C 0.4038(12) 0.1502(10) 0.0907(8) 0.087(5) Uani 0.50 1 d PD . .
C6 C 0.4889(11) 0.0788(13) 0.0812(11) 0.22(2) Uani 0.50 1 d PD . .
H6' H 0.715(4) 0.292(5) 0.195(3) 0.038(16) 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
V1A 0.0215(6) 0.0133(3) 0.0109(3) -0.0017(2) 0.0036(3) -0.0022(3)
O2 0.0282(18) 0.0343(18) 0.044(2) -0.0172(15) 0.0107(15) -0.0012(14)
V1B 0.059(9) 0.011(3) 0.009(3) 0.002(2) 0.007(3) -0.011(4)
O2B 0.013(12) 0.035(15) 0.036(16) 0.023(12) 0.008(11) 0.013(11)
V2 0.0255(3) 0.0130(3) 0.0114(3) -0.0018(2) 0.0047(2) 0.0008(2)
P1 0.0240(5) 0.0123(4) 0.0113(4) -0.0012(3) 0.0020(3) 0.0006(3)
P2 0.0283(5) 0.0121(4) 0.0103(4) -0.0008(3) 0.0049(3) 0.0011(3)
O1 0.0305(14) 0.0158(11) 0.0225(13) -0.0053(10) 0.0050(11) -0.0047(10)
O3 0.0416(17) 0.0186(12) 0.0128(12) -0.0020(9) 0.0071(11) -0.0094(11)
O4 0.0384(15) 0.0131(11) 0.0138(11) 0.0009(9) 0.0091(11) 0.0011(10)
O5 0.0271(13) 0.0161(11) 0.0177(12) -0.0028(9) 0.0043(10) 0.0021(10)
O6 0.073(2) 0.0132(13) 0.0125(12) -0.0002(10) 0.0076(13) 0.0091(14)
O7 0.0288(15) 0.0253(14) 0.0366(16) -0.0071(12) 0.0099(12) -0.0005(12)
O8 0.0373(15) 0.0133(11) 0.0120(11) -0.0032(9) 0.0067(10) -0.0002(10)
O9 0.0371(15) 0.0183(12) 0.0140(12) -0.0022(9) 0.0084(11) -0.0030(11)
N1 0.106(10) 0.060(8) 0.074(10) -0.014(6) 0.060(9) 0.000(7)
C1 0.0244(18) 0.0187(16) 0.0245(18) -0.0007(14) 0.0022(14) 0.0022(14)
C2 0.0276(19) 0.0155(15) 0.0199(17) -0.0003(13) 0.0018(14) 0.0027(14)
C3 0.0275(18) 0.0180(16) 0.0164(16) -0.0020(13) 0.0073(13) 0.0006(14)
N2 0.164(15) 0.040(6) 0.41(3) -0.029(11) 0.25(2) -0.016(8)
C4 0.130(15) 0.059(9) 0.072(10) 0.008(7) 0.041(10) 0.000(9)
C5 0.104(13) 0.079(10) 0.067(9) 0.022(8) -0.002(9) -0.025(10)
C6 0.25(3) 0.021(6) 0.26(3) 0.041(11) -0.20(3) -0.022(11)
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
V1A O2 1.590(4) . ?
V1A O3 1.952(3) . ?
V1A O4 1.970(3) . ?
V1A O6 1.971(3) 4_645 ?
V1A O1 1.977(3) . ?
V1B O2B 1.630(3) . ?
V1B O4 1.862(6) . ?
V1B O6 1.881(7) 4_645 ?
V1B O3 1.930(7) . ?
V1B O1 1.959(8) . ?
V2 O7 1.594(3) . ?
V2 O9 1.951(3) . ?
V2 O6 1.966(3) . ?
V2 O8 1.966(2) . ?
V2 O5 1.984(3) . ?
P1 O8 1.528(2) 1_545 ?
P1 O3 1.528(3) 4_645 ?
P1 O1 1.529(3) . ?
P1 C1 1.782(4) . ?
P2 O5 1.525(3) . ?
P2 O9 1.526(3) 7_655 ?
P2 O4 1.530(3) . ?
P2 C3 1.783(4) . ?
O3 P1 1.528(3) 4_655 ?
O6 V1B 1.881(7) 4_655 ?
O6 V1A 1.971(3) 4_655 ?
O6 H6' 0.67(5) . ?
O8 P1 1.528(2) 1_565 ?
O9 P2 1.527(3) 7_655 ?
N1 C4 1.460(2) . ?
C1 C2 1.529(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.534(5) 3_445 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.534(5) 3 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N2 C5 1.460(2) . ?
C5 C6 1.531(2) . ?
|
1101210.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101210.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_1101210
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4 H16 N O10.5 P2 V2'
_chemical_formula_weight 410.00
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 101.00(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.003(3)
_cell_length_b 10.126(2)
_cell_length_c 18.604(4)
_cell_measurement_temperature 90(2)
_cell_volume 2774.3(10)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.963
_cod_duplicate_entry 1101188
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C4 H16 N O10.50 P2 V2'
_cod_database_code 1101210
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
V1 V 0.15898(6) 0.38593(9) 0.08585(5) 0.00815(19) Uani 1 1 d . . .
V2 V 0.25318(6) -0.04587(9) 0.21865(5) 0.00768(19) Uani 1 1 d . . .
P1 P 0.28574(9) 0.12254(13) 0.07702(7) 0.0075(3) Uani 1 1 d . . .
P2 P 0.16260(9) -0.33013(13) 0.16686(7) 0.0066(3) Uani 1 1 d . . .
O1 O 0.1760(3) 0.5759(4) 0.10549(19) 0.0096(7) Uani 1 1 d . . .
O2 O 0.2079(3) 0.4282(4) -0.0009(2) 0.0103(8) Uani 1 1 d . . .
O3 O 0.0517(3) 0.3675(4) 0.0652(2) 0.0170(9) Uani 1 1 d . . .
O4 O 0.1992(3) 0.3577(5) 0.1911(2) 0.0186(10) Uani 1 1 d . . .
O5 O 0.2000(3) 0.2018(4) 0.0770(2) 0.0116(8) Uani 1 1 d . . .
O6 O 0.2873(2) 0.0005(4) 0.12562(19) 0.0088(7) Uani 1 1 d . . .
O7 O 0.3334(3) 0.0988(4) 0.2599(2) 0.0106(7) Uani 1 1 d . . .
O8 O 0.1538(3) 0.0072(4) 0.2225(2) 0.0205(9) Uani 1 1 d . . .
O9 O 0.2342(3) -0.2218(4) 0.1724(2) 0.0106(7) Uani 1 1 d . . .
O90 O 0.0000 0.2411(15) 0.2500 0.105(5) Uani 1 2 d S . .
O92 O 0.0433(9) 0.1423(13) 0.3071(8) 0.057(4) Uani 0.50 1 d P . .
O91 O 0.0329(7) 0.0625(10) 0.0677(6) 0.032(2) Uani 0.50 1 d P . .
N1A N 0.8763(6) 0.2966(8) 0.0743(5) 0.021(2) Uani 0.599(13) 1 d P A 1
H1A1 H 0.8855 0.3801 0.0888 0.032 Uiso 0.599(13) 1 calc PR A 1
H1A2 H 0.9201 0.2714 0.0511 0.032 Uiso 0.599(13) 1 calc PR A 1
H1A3 H 0.8768 0.2452 0.1132 0.032 Uiso 0.599(13) 1 calc PR A 1
N1B N 0.8570(9) 0.1805(13) 0.0393(8) 0.023(4) Uani 0.401(13) 1 d P A 2
H1B1 H 0.9058 0.2131 0.0687 0.034 Uiso 0.401(13) 1 calc PR A 2
H1B2 H 0.8721 0.1537 -0.0024 0.034 Uiso 0.401(13) 1 calc PR A 2
H1B3 H 0.8357 0.1123 0.0610 0.034 Uiso 0.401(13) 1 calc PR A 2
C1 C 0.3826(3) 0.2243(5) 0.1102(3) 0.0109(10) Uani 1 1 d . . .
H1A H 0.3867 0.2918 0.0740 0.013 Uiso 1 1 calc R . .
H1B H 0.3734 0.2685 0.1545 0.013 Uiso 1 1 calc R . .
C2 C 0.4724(3) 0.1495(5) 0.1268(3) 0.0105(10) Uani 1 1 d . . .
H2A H 0.4786 0.0957 0.0849 0.013 Uiso 1 1 calc R . .
H2B H 0.4727 0.0912 0.1682 0.013 Uiso 1 1 calc R . .
C3 C 0.0527(3) -0.2550(5) 0.1443(3) 0.0100(10) Uani 1 1 d . . .
H3A H 0.0441 -0.1996 0.1849 0.012 Uiso 1 1 calc R . .
H3B H 0.0516 -0.1979 0.1022 0.012 Uiso 1 1 calc R . .
C4 C 0.7856(7) 0.2851(9) 0.0232(6) 0.055(3) Uani 1 1 d . . .
H4 H 0.208(5) 0.304(6) 0.198(4) 0.000(18) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0105(4) 0.0053(4) 0.0089(4) -0.0013(3) 0.0028(3) 0.0007(3)
V2 0.0089(4) 0.0058(4) 0.0087(4) -0.0012(3) 0.0025(3) -0.0011(3)
P1 0.0100(6) 0.0051(6) 0.0071(6) -0.0006(5) 0.0007(5) 0.0002(5)
P2 0.0090(6) 0.0042(6) 0.0067(6) -0.0003(5) 0.0020(5) 0.0008(5)
O1 0.0162(18) 0.0056(17) 0.0075(16) 0.0002(13) 0.0037(14) -0.0018(14)
O2 0.0174(19) 0.0083(18) 0.0074(17) -0.0018(14) 0.0078(15) -0.0008(14)
O3 0.0135(19) 0.0076(19) 0.029(2) -0.0022(17) 0.0031(17) 0.0003(15)
O4 0.038(3) 0.004(2) 0.012(2) -0.0011(17) 0.0008(18) 0.0053(19)
O5 0.0128(18) 0.0073(17) 0.0141(18) 0.0001(15) 0.0015(15) 0.0008(15)
O6 0.0134(17) 0.0065(17) 0.0069(16) -0.0002(14) 0.0033(14) -0.0008(14)
O7 0.0148(18) 0.0067(17) 0.0104(17) -0.0016(14) 0.0028(14) -0.0047(15)
O8 0.019(2) 0.021(2) 0.024(2) -0.0097(18) 0.0077(18) 0.0022(18)
O9 0.0129(18) 0.0080(18) 0.0115(17) -0.0044(15) 0.0041(14) -0.0018(14)
O90 0.088(10) 0.098(11) 0.124(12) 0.000 0.006(9) 0.000
O92 0.062(9) 0.038(7) 0.076(10) -0.017(7) 0.030(8) 0.001(6)
O91 0.027(5) 0.030(5) 0.039(6) -0.006(5) 0.006(4) -0.012(4)
N1A 0.025(5) 0.008(4) 0.035(5) 0.001(4) 0.019(4) 0.000(3)
N1B 0.026(7) 0.016(7) 0.029(7) -0.006(6) 0.014(6) -0.005(6)
C1 0.011(2) 0.007(2) 0.015(3) -0.003(2) 0.0027(19) 0.001(2)
C2 0.010(2) 0.007(2) 0.014(2) -0.003(2) 0.0017(19) -0.0008(19)
C3 0.010(2) 0.007(2) 0.013(2) 0.0017(19) 0.0016(19) -0.0008(19)
C4 0.070(7) 0.037(5) 0.057(6) -0.003(4) 0.015(5) -0.001(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
V1 O3 1.592(4) . ?
V1 O2 1.943(4) . ?
V1 O4 1.957(5) . ?
V1 O1 1.965(4) . ?
V1 O5 1.980(4) . ?
V2 O8 1.599(4) . ?
V2 O6 1.954(4) . ?
V2 O4 1.955(4) 4_545 ?
V2 O7 1.957(4) . ?
V2 O9 1.975(4) . ?
P1 O5 1.517(4) . ?
P1 O2 1.527(4) 7 ?
P1 O6 1.529(4) . ?
P1 C1 1.792(5) . ?
P2 O9 1.525(4) . ?
P2 O1 1.529(4) 1_545 ?
P2 O7 1.532(4) 4_545 ?
P2 C3 1.792(5) . ?
O1 P2 1.529(4) 1_565 ?
O2 P1 1.527(4) 7 ?
O4 V2 1.955(4) 4 ?
O7 P2 1.532(4) 4 ?
N1A C4 1.508(13) . ?
N1B C4 1.495(16) . ?
C1 C2 1.525(7) . ?
C2 C3 1.531(7) 3 ?
C3 C2 1.531(7) 3_445 ?
C4 C4 1.43(2) 7_655 ?
|
1101211.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101211.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_1101211
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C5 H15 N O9.5 P2 V2'
_chemical_formula_weight 405.00
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 102.5210(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.0877(9)
_cell_length_b 10.2027(6)
_cell_length_c 18.6376(11)
_cell_measurement_temperature 90(2)
_cell_volume 2800.7(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.921
_cod_duplicate_entry 1101189
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C5 H15 N O9.50 P2 V2'
_cod_database_code 1101211
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
V1 V 0.16060(3) 0.61538(5) 0.08485(3) 0.00838(13) Uani 1 1 d . . .
V2 V 0.24829(4) 0.54620(5) 0.28319(3) 0.00970(13) Uani 1 1 d . . .
P1 P 0.28632(5) 0.87848(7) 0.07721(4) 0.00890(17) Uani 1 1 d . . .
P2 P 0.16411(5) 0.33098(7) 0.16562(4) 0.00846(16) Uani 1 1 d . . .
O1 O 0.20149(15) 0.7978(2) 0.07685(12) 0.0128(4) Uani 1 1 d . . .
O2 O 0.20928(16) 0.5718(2) -0.00058(12) 0.0130(4) Uani 1 1 d . . .
O3 O 0.05325(16) 0.6327(2) 0.06134(14) 0.0178(5) Uani 1 1 d . . .
O4 O 0.17506(15) 0.4257(2) 0.10450(12) 0.0117(4) Uani 1 1 d . . .
O5 O 0.20282(18) 0.6442(2) 0.19135(12) 0.0185(5) Uani 1 1 d . . .
O6 O 0.26575(15) 0.7218(2) 0.32973(12) 0.0123(4) Uani 1 1 d . . .
O7 O 0.34801(17) 0.4941(3) 0.28395(14) 0.0216(5) Uani 1 1 d . . .
O8 O 0.21122(15) 0.5006(2) 0.37448(12) 0.0119(4) Uani 1 1 d . . .
O9 O 0.17100(16) 0.4001(2) 0.23946(12) 0.0129(4) Uani 1 1 d . . .
O90 O 0.9727(14) 0.8757(19) 0.2101(17) 0.153(19) Uani 0.303(13) 1 d P . 1
O90B O 0.9690(14) 0.752(3) 0.2071(16) 0.097(14) Uani 0.197(13) 1 d P . 2
N1A N 0.8623(6) 0.6975(6) 0.0469(5) 0.047(2) Uani 0.691(17) 1 d P A 1
H1A1 H 0.9046 0.6627 0.0243 0.071 Uiso 0.691(17) 1 calc PR A 1
H1A2 H 0.8060 0.6704 0.0234 0.071 Uiso 0.691(17) 1 calc PR A 1
H1A3 H 0.8735 0.6705 0.0945 0.071 Uiso 0.691(17) 1 calc PR A 1
N1B N 0.8981(12) 0.7267(13) 0.0988(13) 0.052(7) Uani 0.309(17) 1 d P A 2
H1B1 H 0.9409 0.6777 0.0835 0.078 Uiso 0.309(17) 1 calc PR A 2
H1B2 H 0.8501 0.6750 0.1023 0.078 Uiso 0.309(17) 1 calc PR A 2
H1B3 H 0.9225 0.7619 0.1437 0.078 Uiso 0.309(17) 1 calc PR A 2
C1 C 0.3840(2) 0.7783(3) 0.11120(17) 0.0121(6) Uani 1 1 d . . .
H1A H 0.3762 0.7344 0.1568 0.014 Uiso 1 1 calc R . .
H1B H 0.3871 0.7092 0.0745 0.014 Uiso 1 1 calc R . .
C2 C 0.0539(2) 0.2572(3) 0.14274(18) 0.0140(6) Uani 1 1 d . . .
H2A H 0.0505 0.2016 0.0987 0.017 Uiso 1 1 calc R . .
H2B H 0.0470 0.1990 0.1837 0.017 Uiso 1 1 calc R . .
C3 C -0.0261(2) 0.3533(3) 0.12749(18) 0.0140(6) Uani 1 1 d . . .
H3A H -0.0234 0.4107 0.1707 0.017 Uiso 1 1 calc R . .
H3B H -0.0221 0.4094 0.0850 0.017 Uiso 1 1 calc R . .
C4 C 0.8667(6) 0.8351(8) 0.0445(6) 0.090(3) Uani 1 1 d D . .
H4A H 0.8049 0.8732 0.0353 0.108 Uiso 1 1 calc R A 1
H4B H 0.8966 0.8636 0.0048 0.108 Uiso 1 1 calc R A 1
C5A C 0.9193(13) 0.877(2) 0.1158(10) 0.111(7) Uani 0.539(17) 1 d PDU A 1
H5A1 H 0.9811 0.8995 0.1114 0.166 Uiso 0.539(17) 1 calc PR A 1
H5A2 H 0.9219 0.8055 0.1514 0.166 Uiso 0.539(17) 1 calc PR A 1
H5A3 H 0.8905 0.9537 0.1326 0.166 Uiso 0.539(17) 1 calc PR A 1
C5B C 0.9400(10) 0.9208(12) 0.0456(10) 0.064(5) Uani 0.461(17) 1 d P A 2
H5B1 H 0.9501 0.9739 0.0905 0.096 Uiso 0.461(17) 1 calc PR A 2
H5B2 H 0.9261 0.9784 0.0026 0.096 Uiso 0.461(17) 1 calc PR A 2
H5B3 H 0.9948 0.8698 0.0446 0.096 Uiso 0.461(17) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0104(3) 0.0081(2) 0.0068(2) 0.00130(17) 0.00233(18) 0.00043(17)
V2 0.0126(3) 0.0084(2) 0.0082(2) -0.00104(18) 0.00258(18) -0.00084(18)
P1 0.0131(4) 0.0072(3) 0.0065(3) 0.0012(3) 0.0023(3) 0.0004(3)
P2 0.0112(4) 0.0071(3) 0.0066(3) -0.0001(3) 0.0009(3) -0.0005(3)
O1 0.0132(11) 0.0097(10) 0.0145(11) 0.0011(8) 0.0011(8) -0.0003(8)
O2 0.0200(11) 0.0116(10) 0.0081(10) 0.0018(8) 0.0046(8) 0.0021(9)
O3 0.0130(11) 0.0155(11) 0.0247(13) 0.0044(9) 0.0038(9) 0.0014(9)
O4 0.0191(11) 0.0083(9) 0.0078(10) 0.0020(8) 0.0033(8) 0.0019(8)
O5 0.0373(15) 0.0097(10) 0.0079(10) 0.0007(8) 0.0038(10) -0.0028(10)
O6 0.0133(11) 0.0099(10) 0.0140(11) -0.0038(8) 0.0037(8) -0.0027(8)
O7 0.0173(12) 0.0224(12) 0.0254(13) -0.0086(10) 0.0056(10) 0.0008(10)
O8 0.0181(11) 0.0099(10) 0.0084(10) 0.0002(8) 0.0044(8) 0.0007(8)
O9 0.0203(12) 0.0111(10) 0.0077(10) -0.0013(8) 0.0037(8) -0.0044(9)
O90 0.09(2) 0.091(14) 0.33(5) -0.104(19) 0.16(3) -0.046(11)
O90B 0.047(13) 0.13(3) 0.13(2) -0.11(2) 0.052(14) -0.056(14)
N1A 0.079(5) 0.025(3) 0.044(5) -0.005(3) 0.028(4) -0.018(3)
N1B 0.052(10) 0.022(6) 0.099(18) -0.013(8) 0.053(11) -0.006(6)
C1 0.0121(14) 0.0112(13) 0.0126(14) 0.0025(11) 0.0019(11) 0.0015(11)
C2 0.0134(14) 0.0106(13) 0.0166(15) -0.0011(11) 0.0002(11) -0.0006(11)
C3 0.0133(15) 0.0113(14) 0.0163(15) 0.0014(12) 0.0009(11) 0.0002(11)
C4 0.094(6) 0.063(4) 0.133(8) -0.003(5) 0.069(6) 0.006(4)
C5A 0.102(10) 0.120(10) 0.109(10) -0.012(8) 0.019(8) -0.003(8)
C5B 0.057(8) 0.025(5) 0.112(14) -0.013(7) 0.024(8) -0.005(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
V1 O3 1.593(2) . ?
V1 O2 1.944(2) . ?
V1 O5 1.971(2) . ?
V1 O4 1.972(2) . ?
V1 O1 1.977(2) . ?
V2 O7 1.593(3) . ?
V2 O9 1.958(2) . ?
V2 O8 1.959(2) . ?
V2 O5 1.972(2) . ?
V2 O6 1.983(2) . ?
P1 O1 1.520(2) . ?
P1 O2 1.531(2) 7_565 ?
P1 O8 1.533(2) 4 ?
P1 C1 1.792(3) . ?
P2 O6 1.526(2) 4_545 ?
P2 O9 1.530(2) . ?
P2 O4 1.530(2) . ?
P2 C2 1.791(3) . ?
O2 P1 1.531(2) 7_565 ?
O6 P2 1.526(2) 4 ?
O8 P1 1.533(2) 4_545 ?
O90 O90 1.54(6) 2_755 ?
O90B O90B 1.67(6) 2_755 ?
N1A C4 1.406(9) . ?
N1A H1A1 0.9100 . ?
N1A H1A2 0.9100 . ?
N1A H1A3 0.9100 . ?
N1B C4 1.50(2) . ?
N1B H1B1 0.9100 . ?
N1B H1B2 0.9100 . ?
N1B H1B3 0.9100 . ?
C1 C3 1.530(4) 3 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.533(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C1 1.530(4) 3_445 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5B 1.407(15) . ?
C4 C5A 1.456(13) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5A H5A1 0.9800 . ?
C5A H5A2 0.9800 . ?
C5A H5A3 0.9800 . ?
C5B H5B1 0.9800 . ?
C5B H5B2 0.9800 . ?
C5B H5B3 0.9800 . ?
|
1101212.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101212.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_1101212
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C6 H17 N O9 P2 V2'
_chemical_formula_weight 411.03
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.8350(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.4228(9)
_cell_length_b 10.2047(6)
_cell_length_c 18.7078(11)
_cell_measurement_temperature 90(2)
_cell_volume 2858.9(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.910
_cod_duplicate_entry 1101190
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1101212
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
V1 V 0.16434(2) 0.12191(3) 1.08617(2) 0.01086(11) Uani 1 1 d . . .
V2A V 0.24587(4) -0.05145(5) 0.78487(3) 0.01083(19) Uani 0.6719(19) 1 d P . 1
V2B V 0.18727(8) -0.08297(11) 0.78053(6) 0.0095(4) Uani 0.3281(19) 1 d P . 2
P1 P 0.20897(4) 0.11803(5) 0.92278(3) 0.01206(13) Uani 1 1 d . . .
P2 P 0.16486(4) 0.16431(5) 0.66595(3) 0.01312(13) Uani 1 1 d . . .
O1 O 0.20873(11) 0.29907(16) 1.07397(9) 0.0169(3) Uani 1 1 d . . .
O2 O 0.05895(12) 0.14660(18) 1.06552(12) 0.0248(4) Uani 1 1 d . . .
O3 O 0.21375(16) 0.1469(2) 1.19040(10) 0.0286(5) Uani 1 1 d . . .
O4 O 0.17016(11) -0.06951(15) 1.10343(9) 0.0144(3) Uani 1 1 d . . .
O5 O 0.20323(12) 0.06928(16) 0.99908(9) 0.0169(3) Uani 1 1 d . . .
O6 O 0.20899(12) -0.00534(15) 0.87631(9) 0.0156(3) Uani 1 1 d . . .
O7 O 0.26731(11) -0.22657(16) 0.83215(9) 0.0161(3) Uani 1 1 d . . .
O8A O 0.34256(18) 0.0063(3) 0.79112(16) 0.0178(8) Uani 0.583(6) 1 d P . 1
O8B O 0.0898(3) -0.1363(6) 0.7696(2) 0.0388(18) Uani 0.417(6) 1 d P . 2
O9 O 0.17724(16) 0.09530(18) 0.73993(10) 0.0275(4) Uani 1 1 d . . .
N1 N 0.12460(15) 0.8109(2) 0.95471(14) 0.0229(5) Uani 1 1 d . . .
H1A H 0.1475 0.8386 0.9168 0.034 Uiso 1 1 calc R . .
H1B H 0.1498 0.8573 0.9960 0.034 Uiso 1 1 calc R . .
H1C H 0.0644 0.8234 0.9431 0.034 Uiso 1 1 calc R . .
C1 C 0.11188(16) 0.2159(2) 0.88569(13) 0.0166(4) Uani 1 1 d . . .
H1D H 0.1099 0.2886 0.9203 0.020 Uiso 1 1 calc R . .
H1E H 0.1182 0.2551 0.8388 0.020 Uiso 1 1 calc R . .
C2 C 0.02267(16) 0.1416(2) 0.87133(14) 0.0179(5) Uani 1 1 d . . .
H2A H 0.0182 0.0812 0.8292 0.021 Uiso 1 1 calc R . .
H2B H 0.0202 0.0887 0.9151 0.021 Uiso 1 1 calc R . .
C3 C 0.05552(16) 0.2375(2) 0.64545(14) 0.0192(5) Uani 1 1 d . . .
H3A H 0.0503 0.2923 0.6879 0.023 Uiso 1 1 calc R . .
H3B H 0.0503 0.2964 0.6026 0.023 Uiso 1 1 calc R . .
C4 C 0.14445(19) 0.6685(3) 0.96835(17) 0.0268(6) Uani 1 1 d . . .
H4A H 0.1968 0.6447 0.9490 0.032 Uiso 1 1 calc R . .
H4B H 0.1601 0.6521 1.0221 0.032 Uiso 1 1 calc R . .
C5 C 0.0678(3) 0.5837(3) 0.9331(2) 0.0448(9) Uani 1 1 d . . .
H5A H 0.0136 0.6134 0.9481 0.054 Uiso 1 1 calc R . .
H5B H 0.0803 0.4923 0.9502 0.054 Uiso 1 1 calc R . .
C6 C 0.0509(5) 0.5879(6) 0.8508(3) 0.092(2) Uani 1 1 d . . .
H6A H 0.0457 0.6793 0.8342 0.139 Uiso 1 1 calc R . .
H6B H -0.0047 0.5413 0.8290 0.139 Uiso 1 1 calc R . .
H6C H 0.1006 0.5459 0.8354 0.139 Uiso 1 1 calc R . .
H3 H 0.220(3) 0.213(5) 1.195(2) 0.054(14) 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
V1 0.01451(19) 0.00810(18) 0.01080(19) 0.00083(12) 0.00470(14) 0.00025(13)
V2A 0.0136(4) 0.0091(3) 0.0104(3) 0.00103(19) 0.0041(2) 0.0013(2)
V2B 0.0129(8) 0.0067(5) 0.0090(5) -0.0005(4) 0.0030(4) 0.0003(4)
P1 0.0191(3) 0.0073(3) 0.0111(3) -0.00007(19) 0.0063(2) -0.0008(2)
P2 0.0221(3) 0.0072(3) 0.0109(3) -0.00090(19) 0.0057(2) -0.0003(2)
O1 0.0210(8) 0.0107(7) 0.0197(8) 0.0018(6) 0.0062(6) -0.0031(6)
O2 0.0170(8) 0.0176(8) 0.0416(11) 0.0053(8) 0.0108(8) 0.0030(7)
O3 0.0529(13) 0.0137(9) 0.0135(8) 0.0032(7) -0.0030(8) -0.0107(9)
O4 0.0223(8) 0.0091(7) 0.0126(7) 0.0020(6) 0.0056(6) 0.0008(6)
O5 0.0288(9) 0.0110(7) 0.0133(8) 0.0018(6) 0.0099(7) 0.0012(6)
O6 0.0260(9) 0.0091(7) 0.0132(7) -0.0012(6) 0.0076(6) -0.0007(6)
O7 0.0216(8) 0.0113(7) 0.0146(8) 0.0025(6) 0.0028(6) 0.0023(6)
O8A 0.0114(14) 0.0188(15) 0.0231(16) 0.0063(11) 0.0039(11) -0.0041(11)
O8B 0.022(2) 0.081(4) 0.012(2) -0.006(2) 0.0012(17) -0.038(3)
O9 0.0594(14) 0.0122(8) 0.0148(8) 0.0021(7) 0.0166(9) 0.0052(8)
N1 0.0207(10) 0.0143(10) 0.0344(12) 0.0011(9) 0.0077(9) -0.0004(8)
C1 0.0221(11) 0.0106(10) 0.0186(11) 0.0015(8) 0.0080(9) 0.0009(8)
C2 0.0213(12) 0.0113(10) 0.0219(12) 0.0015(9) 0.0068(9) 0.0014(9)
C3 0.0231(12) 0.0107(10) 0.0264(12) -0.0017(9) 0.0112(10) -0.0011(9)
C4 0.0329(14) 0.0157(12) 0.0336(14) 0.0023(10) 0.0115(12) 0.0062(10)
C5 0.047(2) 0.0164(13) 0.071(3) -0.0042(15) 0.0135(18) -0.0056(13)
C6 0.120(5) 0.069(3) 0.066(3) -0.027(3) -0.021(3) -0.024(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
V1 O2 1.5982(18) . ?
V1 O3 1.933(2) . ?
V1 O5 1.9417(17) . ?
V1 O1 1.9656(17) . ?
V1 O4 1.9785(16) . ?
V2A O8A 1.582(3) . ?
V2A O9 1.909(2) . ?
V2A O3 1.974(2) 6 ?
V2A O6 1.9842(17) . ?
V2A O7 1.9864(17) . ?
V2B O8B 1.566(4) . ?
V2B O6 1.9141(19) . ?
V2B O3 1.940(2) 6 ?
V2B O9 1.963(2) . ?
V2B O7 2.0084(19) . ?
P1 O1 1.5146(17) 7_557 ?
P1 O6 1.5299(16) . ?
P1 O5 1.5340(16) . ?
P1 C1 1.795(2) . ?
P2 O7 1.5225(17) 4_556 ?
P2 O9 1.5235(18) . ?
P2 O4 1.5350(16) 6 ?
P2 C3 1.800(3) . ?
O1 P1 1.5146(17) 7_557 ?
O3 V2B 1.940(2) 6_556 ?
O3 V2A 1.975(2) 6_556 ?
O3 H3 0.68(5) . ?
O4 P2 1.5351(16) 6_556 ?
O7 P2 1.5224(17) 4_546 ?
N1 C4 1.494(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.537(3) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.526(3) 2_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.526(3) 2_556 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.486(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.500(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
|
1101213.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101213.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_1101213
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C7 H19.5 N O9 P2 V2'
_chemical_formula_weight 425.56
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90.00
_cell_angle_beta 103.2520(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.2768(8)
_cell_length_b 10.2216(6)
_cell_length_c 18.6279(10)
_cell_measurement_temperature 90(2)
_cell_volume 2831.4(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.997
_cod_duplicate_entry 1101191
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C7 H19.50 N O9 P2 V2'
_cod_database_code 1101213
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
V1 V 0.74870(4) 0.04535(6) 0.21455(3) 0.00863(17) Uani 1 1 d . . .
V2 V 0.83739(4) 0.11735(6) 0.41440(3) 0.00862(16) Uani 1 1 d . . .
P1 P 0.83634(6) -0.16810(9) 0.33474(5) 0.0082(2) Uani 1 1 d . . .
P2 P 0.71187(6) 0.37985(9) 0.42286(5) 0.0085(2) Uani 1 1 d . . .
O1 O 0.73201(18) 0.2215(3) 0.16855(15) 0.0123(5) Uani 1 1 d . . .
O2 O 0.79047(19) 0.0028(3) 0.12522(14) 0.0111(5) Uani 1 1 d . . .
O3 O 0.8261(2) -0.1005(3) 0.26011(15) 0.0131(5) Uani 1 1 d . . .
O4 O 0.6499(2) -0.0089(3) 0.20979(17) 0.0193(6) Uani 1 1 d . . .
O5 O 0.7907(2) 0.1422(3) 0.30808(17) 0.0172(6) Uani 1 1 d . . .
O6 O 0.82654(19) -0.0730(3) 0.39591(14) 0.0114(5) Uani 1 1 d . . .
O7 O 0.79516(18) 0.2982(3) 0.42318(15) 0.0120(5) Uani 1 1 d . . .
O8 O 0.79221(19) 0.0713(3) 0.50033(15) 0.0127(5) Uani 1 1 d . . .
O9 O 0.94393(19) 0.1390(3) 0.43602(17) 0.0165(6) Uani 1 1 d . . .
N1 N 0.0000 0.1793(11) 0.2500 0.088(4) Uani 1 2 d S . .
H1A H 0.0402 0.1275 0.2330 0.106 Uiso 0.50 1 calc PR . .
H1B H -0.0402 0.1275 0.2670 0.106 Uiso 0.50 1 calc PR . .
N2A N 0.0672(10) 0.4250(13) 0.4637(8) 0.022(4) Uani 0.277(11) 1 d P A 1
H2A1 H 0.0178 0.3802 0.4696 0.032 Uiso 0.277(11) 1 calc PR A 1
H2A2 H 0.0524 0.4750 0.4222 0.032 Uiso 0.277(11) 1 calc PR A 1
H2A3 H 0.0873 0.4775 0.5035 0.032 Uiso 0.277(11) 1 calc PR A 1
N2B N 0.0867(11) 0.4069(15) 0.3918(9) 0.016(4) Uani 0.223(11) 1 d PU A 2
H2B1 H 0.1200 0.4139 0.3572 0.024 Uiso 0.223(11) 1 calc PR A 2
H2B2 H 0.0742 0.4882 0.4067 0.024 Uiso 0.223(11) 1 calc PR A 2
H2B3 H 0.0344 0.3644 0.3721 0.024 Uiso 0.223(11) 1 calc PR A 2
C1 C 0.9462(3) -0.2397(4) 0.3568(2) 0.0129(7) Uani 1 1 d . . .
H1C H 0.9507 -0.2962 0.4007 0.015 Uiso 1 1 calc R . .
H1D H 0.9523 -0.2969 0.3153 0.015 Uiso 1 1 calc R . .
C2 C 0.6144(3) 0.2809(4) 0.3883(2) 0.0114(7) Uani 1 1 d . . .
H2A H 0.6212 0.2378 0.3423 0.014 Uiso 1 1 calc R . .
H2B H 0.6119 0.2113 0.4247 0.014 Uiso 1 1 calc R . .
C3 C 0.5253(3) 0.3556(4) 0.3723(2) 0.0128(7) Uani 1 1 d . . .
H3A H 0.5222 0.4110 0.4153 0.015 Uiso 1 1 calc R . .
H3B H 0.5219 0.4134 0.3292 0.015 Uiso 1 1 calc R . .
C4 C 0.0520(9) 0.2859(14) 0.3140(7) 0.102(4) Uani 1 1 d U . .
H4A H 0.1008 0.3289 0.2957 0.123 Uiso 1 1 calc R . .
H4B H 0.0084 0.3545 0.3197 0.123 Uiso 1 1 calc R . .
C5 C 0.0927(7) 0.2273(11) 0.3905(5) 0.073(2) Uani 1 1 d . . .
H5A H 0.1204 0.2971 0.4242 0.109 Uiso 1 1 calc R . .
H5B H 0.1384 0.1623 0.3863 0.109 Uiso 1 1 calc R . .
H5C H 0.0451 0.1852 0.4097 0.109 Uiso 1 1 calc R . .
C6 C 0.1387(5) 0.3314(7) 0.4568(4) 0.0503(17) Uani 1 1 d . . .
H6A H 0.1528 0.3541 0.4090 0.060 Uiso 1 1 calc R A 1
H6B H 0.1916 0.3600 0.4949 0.060 Uiso 1 1 calc R A 1
C7 C 0.1434(8) 0.1945(9) 0.4593(5) 0.079(3) Uani 1 1 d . A .
H7A H 0.1692 0.1662 0.5100 0.118 Uiso 1 1 calc R . .
H7B H 0.1814 0.1637 0.4269 0.118 Uiso 1 1 calc R . .
H7C H 0.0828 0.1579 0.4427 0.118 Uiso 1 1 calc R . .
H5 H 0.788(4) 0.200(7) 0.303(4) 0.025(19) 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
V1 0.0111(3) 0.0086(3) 0.0067(3) 0.0010(2) 0.0032(2) 0.0008(2)
V2 0.0097(3) 0.0096(3) 0.0070(3) -0.0010(2) 0.0029(2) -0.0002(2)
P1 0.0099(4) 0.0086(4) 0.0060(4) 0.0001(3) 0.0016(3) 0.0003(3)
P2 0.0118(4) 0.0081(4) 0.0062(4) -0.0007(3) 0.0033(3) -0.0004(3)
O1 0.0137(13) 0.0103(13) 0.0138(13) 0.0023(10) 0.0046(10) 0.0013(10)
O2 0.0170(13) 0.0094(12) 0.0084(12) -0.0017(10) 0.0057(10) -0.0008(10)
O3 0.0199(14) 0.0115(12) 0.0088(12) 0.0007(10) 0.0051(10) 0.0050(11)
O4 0.0171(14) 0.0211(15) 0.0206(15) 0.0045(12) 0.0064(12) -0.0009(12)
O5 0.0325(18) 0.0094(14) 0.0091(13) -0.0003(11) 0.0037(12) 0.0036(13)
O6 0.0185(13) 0.0093(12) 0.0067(11) -0.0014(10) 0.0038(10) -0.0003(10)
O7 0.0129(12) 0.0110(13) 0.0121(12) -0.0014(10) 0.0026(10) 0.0009(10)
O8 0.0180(13) 0.0153(13) 0.0067(12) -0.0018(10) 0.0065(10) -0.0017(11)
O9 0.0131(13) 0.0151(14) 0.0222(15) -0.0031(11) 0.0058(11) -0.0003(11)
N1 0.123(10) 0.050(6) 0.123(10) 0.000 0.093(9) 0.000
N2A 0.028(7) 0.012(6) 0.027(7) 0.002(5) 0.011(6) -0.016(5)
N2B 0.020(5) 0.011(5) 0.014(5) 0.003(4) 0.001(4) -0.004(4)
C1 0.0133(17) 0.0111(17) 0.0132(17) -0.0008(14) 0.0008(14) -0.0008(14)
C2 0.0133(17) 0.0101(16) 0.0107(16) -0.0026(13) 0.0025(13) -0.0011(13)
C3 0.0111(17) 0.0117(17) 0.0141(17) 0.0003(14) -0.0001(13) 0.0000(14)
C4 0.098(7) 0.099(7) 0.115(8) 0.010(6) 0.032(6) 0.003(6)
C5 0.079(6) 0.076(6) 0.065(5) 0.008(5) 0.020(5) -0.006(5)
C6 0.052(4) 0.052(4) 0.051(4) -0.002(3) 0.020(3) -0.012(3)
C7 0.142(10) 0.051(5) 0.055(5) -0.001(4) 0.047(6) -0.001(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
V1 O4 1.591(3) . ?
V1 O2 1.963(3) . ?
V1 O3 1.970(3) . ?
V1 O5 1.979(3) . ?
V1 O1 1.985(3) . ?
V2 O9 1.600(3) . ?
V2 O8 1.941(3) . ?
V2 O5 1.962(3) . ?
V2 O6 1.977(3) . ?
V2 O7 1.977(3) . ?
P1 O3 1.528(3) . ?
P1 O1 1.529(3) 4_645 ?
P1 O6 1.531(3) . ?
P1 C1 1.790(4) . ?
P2 O7 1.521(3) . ?
P2 O8 1.530(3) 7_656 ?
P2 O2 1.539(3) 4_655 ?
P2 C2 1.793(4) . ?
O1 P1 1.529(3) 4_655 ?
O2 P2 1.539(3) 4_645 ?
O8 P2 1.530(3) 7_656 ?
N1 C4 1.675(15) 2 ?
N1 C4 1.675(15) . ?
N2A C6 1.481(17) . ?
N2B C6 1.500(17) . ?
C1 C3 1.528(5) 3_545 ?
C2 C3 1.529(5) . ?
C3 C1 1.528(5) 3_455 ?
C4 C5 1.538(15) . ?
C6 C7 1.401(12) . ?
|
1101214.cif | #------------------------------------------------------------------------------
#$Date: 2016-01-28 12:58:41 +0200 (Thu, 28 Jan 2016) $
#$Revision: 175229 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101214.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_1101214
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C12 H32.75 N2 O18.75 P4 V4'
_chemical_formula_weight 832.79
_space_group_IT_number 36
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'C 2c -2'
_symmetry_space_group_name_H-M 'C m c 21'
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 30.947(2)
_cell_length_b 10.6168(8)
_cell_length_c 18.6040(14)
_cell_measurement_temperature 90(2)
_cell_volume 6112.5(8)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.810
_cod_duplicate_entry 1101192
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1101214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-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'
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
V1 V 0.16985(4) 0.94918(10) 1.26464(8) 0.0393(3) Uani 1 1 d . . .
V2 V 0.16695(5) 0.90260(10) 1.06622(8) 0.0410(3) Uani 1 1 d . . .
V3 V 0.16085(3) 0.59298(9) 0.87097(8) 0.0253(2) Uani 1 1 d . . .
V4 V 0.12799(6) 0.56114(11) 0.68111(8) 0.0584(5) Uani 1 1 d . . .
P1 P 0.12172(6) 1.13660(15) 1.15108(10) 0.0299(3) Uani 1 1 d D . .
P2 P 0.13140(7) 0.62157(16) 1.04051(10) 0.0377(5) Uani 1 1 d . . .
P3 P 0.13341(5) 0.88512(14) 0.89867(9) 0.0258(3) Uani 1 1 d . . .
P4 P 0.13269(8) 0.32954(17) 0.79331(11) 0.0476(6) Uani 1 1 d . . .
O1 O 0.14389(16) 0.9954(4) 1.3578(2) 0.0342(10) Uani 1 1 d . . .
O2 O 0.1670(2) 0.7757(4) 1.3049(3) 0.0511(15) Uani 1 1 d . . .
O3 O 0.21949(19) 0.9886(7) 1.2706(4) 0.0669(17) Uani 1 1 d . . .
O4 O 0.1385(2) 1.0919(5) 1.2236(2) 0.0510(16) Uani 1 1 d . A .
O5 O 0.1613(3) 0.8666(6) 1.1701(3) 0.067(3) Uani 1 1 d . . .
O6 O 0.1374(2) 1.0590(5) 1.0875(3) 0.0616(19) Uani 1 1 d . A .
O7 O 0.2146(2) 0.9430(6) 1.0475(4) 0.0672(17) Uani 1 1 d . . .
O8 O 0.13163(19) 0.9128(4) 0.9791(2) 0.0395(12) Uani 1 1 d . . .
O9 O 0.16641(18) 0.7169(4) 1.0582(3) 0.0421(12) Uani 1 1 d . . .
O10 O 0.1373(2) 0.4985(5) 1.0817(2) 0.0494(14) Uani 1 1 d . . .
O11 O 0.12986(18) 0.5873(5) 0.9609(2) 0.0420(13) Uani 1 1 d . . .
O12 O 0.16617(14) 0.7814(3) 0.8809(2) 0.0271(9) Uani 1 1 d . . .
O13 O 0.20980(17) 0.5549(5) 0.8821(4) 0.0668(19) Uani 1 1 d . . .
O14 O 0.1347(2) 0.4235(5) 0.8550(3) 0.0510(15) Uani 1 1 d . . .
O15 O 0.1478(2) 0.6334(5) 0.7723(3) 0.0457(13) Uani 1 1 d . . .
O16 O 0.1388(2) 0.3891(4) 0.7202(3) 0.0513(16) Uani 1 1 d . . .
O17 O 0.1346(2) 0.7300(4) 0.6370(3) 0.0510(15) Uani 1 1 d . . .
O18 O 0.0755(2) 0.5613(6) 0.6903(3) 0.0709(18) Uani 1 1 d . . .
O90 O 0.2093(3) 0.5581(8) 0.6705(5) 0.068(2) Uani 0.75 1 d P . .
N1 N 0.1551(2) 0.2792(8) 0.9852(4) 0.065(2) Uani 1 1 d . . .
H1A H 0.1479 0.3308 0.9495 0.097 Uiso 1 1 calc R . .
H1B H 0.1396 0.2984 1.0241 0.097 Uiso 1 1 calc R . .
H1C H 0.1496 0.2000 0.9723 0.097 Uiso 1 1 calc R . .
N2 N 0.2412(2) 0.2994(6) 0.8872(5) 0.067(2) Uani 1 1 d . . .
H2A H 0.2314 0.3779 0.8910 0.100 Uiso 1 1 calc R . .
H2B H 0.2281 0.2611 0.8506 0.100 Uiso 1 1 calc R . .
H2C H 0.2696 0.3008 0.8795 0.100 Uiso 1 1 calc R . .
C1A C 0.0646(2) 1.159(3) 1.1505(17) 0.064(8) Uani 0.46(4) 1 d PD A 1
H1A1 H 0.0580 1.2184 1.1885 0.076 Uiso 0.46(4) 1 calc PR A 1
H1A2 H 0.0575 1.2001 1.1055 0.076 Uiso 0.46(4) 1 calc PR A 1
C1B C 0.0664(4) 1.091(4) 1.1583(14) 0.123(14) Uani 0.54(4) 1 d PD A 2
H1B1 H 0.0650 1.0002 1.1610 0.147 Uiso 0.54(4) 1 calc PR A 2
H1B2 H 0.0550 1.1245 1.2030 0.147 Uiso 0.54(4) 1 calc PR A 2
C2A C 0.0331(9) 1.049(3) 1.1589(17) 0.097(16) Uani 0.35(3) 1 d PD A 1
H2A1 H 0.0179 1.0572 1.2043 0.116 Uiso 0.35(3) 1 calc PR A 1
H2A2 H 0.0494 0.9707 1.1604 0.116 Uiso 0.35(3) 1 calc PR A 1
C2B C 0.0375(5) 1.136(2) 1.0968(14) 0.20(2) Uani 0.65(3) 1 d PD A 2
H2B1 H 0.0527 1.1326 1.0512 0.235 Uiso 0.65(3) 1 calc PR A 2
H2B2 H 0.0272 1.2207 1.1050 0.235 Uiso 0.65(3) 1 calc PR A 2
C3 C 0.0000 1.041(2) 1.0980(18) 0.22(2) Uani 1 2 d SD . .
H3A H 0.0000 1.1134 1.0658 0.267 Uiso 1 2 calc SR A 1
H3B H 0.0000 0.9625 1.0717 0.267 Uiso 1 2 calc SR A 1
C4 C 0.0803(3) 0.6846(7) 1.0650(4) 0.057(2) Uani 1 1 d . . .
H4A H 0.0800 0.6962 1.1168 0.068 Uiso 1 1 calc R . .
H4B H 0.0777 0.7674 1.0434 0.068 Uiso 1 1 calc R . .
C5 C 0.0409(3) 0.6093(8) 1.0448(5) 0.057(2) Uani 1 1 d . . .
H5A H 0.0406 0.5975 0.9931 0.068 Uiso 1 1 calc R . .
H5B H 0.0427 0.5268 1.0670 0.068 Uiso 1 1 calc R . .
C6 C 0.0000 0.6709(12) 1.0673(6) 0.057(3) Uani 1 2 d S . .
H6A H 0.0000 0.6768 1.1193 0.069 Uiso 1 2 calc SR . .
H6B H 0.0000 0.7562 1.0486 0.069 Uiso 1 2 calc SR . .
C7 C 0.08128(19) 0.8268(6) 0.8734(4) 0.0325(13) Uani 1 1 d . . .
H7A H 0.0816 0.8115 0.8220 0.039 Uiso 1 1 calc R . .
H7B H 0.0771 0.7462 0.8969 0.039 Uiso 1 1 calc R . .
C8 C 0.0416(2) 0.9106(7) 0.8907(5) 0.0452(18) Uani 1 1 d . . .
H8A H 0.0414 0.9309 0.9415 0.054 Uiso 1 1 calc R . .
H8B H 0.0436 0.9888 0.8639 0.054 Uiso 1 1 calc R . .
C9 C 0.0000 0.8418(10) 0.8706(6) 0.043(2) Uani 1 2 d S . .
H9A H 0.0000 0.8271 0.8192 0.051 Uiso 1 2 calc SR . .
H9B H 0.0000 0.7602 0.8941 0.051 Uiso 1 2 calc SR . .
C10 C 0.0822(3) 0.2539(7) 0.7979(5) 0.059(2) Uani 1 1 d . . .
H10A H 0.0805 0.1952 0.7580 0.071 Uiso 1 1 calc R . .
H10B H 0.0817 0.2045 0.8417 0.071 Uiso 1 1 calc R . .
C11 C 0.0409(4) 0.3363(8) 0.7965(6) 0.073(3) Uani 1 1 d . . .
H11A H 0.0421 0.3964 0.8357 0.088 Uiso 1 1 calc R . .
H11B H 0.0401 0.3834 0.7518 0.088 Uiso 1 1 calc R . .
C12 C 0.0000 0.2602(13) 0.8030(9) 0.076(4) Uani 1 2 d S . .
H12A H 0.0000 0.2179 0.8492 0.091 Uiso 1 2 calc SR . .
H12B H 0.0000 0.1958 0.7660 0.091 Uiso 1 2 calc SR . .
C13 C 0.2020(3) 0.2931(10) 1.0016(8) 0.090(4) Uani 1 1 d . . .
H13A H 0.2089 0.3822 1.0012 0.108 Uiso 1 1 calc R . .
H13B H 0.2069 0.2629 1.0502 0.108 Uiso 1 1 calc R . .
C14 C 0.2320(3) 0.2298(9) 0.9548(5) 0.065(3) Uani 1 1 d . . .
H14A H 0.2204 0.1476 0.9428 0.077 Uiso 1 1 calc R . .
H14B H 0.2589 0.2169 0.9805 0.077 Uiso 1 1 calc R . .
H15' H 0.161(3) 0.705(9) 0.766(6) 0.08(3) Uiso 1 1 d . . .
H5' H 0.172(2) 0.831(6) 1.169(4) 0.000(17) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0764(9) 0.0282(5) 0.0132(4) 0.0006(4) -0.0048(5) 0.0148(5)
V2 0.0795(10) 0.0288(5) 0.0147(5) -0.0020(4) -0.0097(5) 0.0043(6)
V3 0.0319(5) 0.0258(5) 0.0184(5) 0.0021(4) 0.0027(4) 0.0016(4)
V4 0.1391(16) 0.0252(6) 0.0109(5) -0.0011(4) 0.0001(7) -0.0069(7)
P1 0.0448(9) 0.0282(8) 0.0168(7) 0.0019(6) -0.0067(6) -0.0024(7)
P2 0.0756(14) 0.0285(8) 0.0090(7) 0.0012(6) 0.0032(8) 0.0056(8)
P3 0.0439(10) 0.0224(7) 0.0112(7) 0.0005(5) -0.0053(6) 0.0020(6)
P4 0.1022(17) 0.0276(8) 0.0128(7) -0.0007(6) -0.0013(9) -0.0194(9)
O1 0.065(3) 0.022(2) 0.0153(19) -0.0029(17) -0.0001(19) -0.003(2)
O2 0.106(5) 0.028(2) 0.018(2) -0.0002(19) -0.003(2) 0.013(3)
O3 0.052(4) 0.095(5) 0.053(3) 0.008(4) -0.004(3) 0.017(3)
O4 0.106(5) 0.037(3) 0.011(2) 0.0034(19) -0.005(2) 0.025(3)
O5 0.154(8) 0.031(3) 0.015(3) 0.002(2) -0.006(3) 0.042(4)
O6 0.141(6) 0.031(3) 0.013(2) -0.003(2) -0.009(3) 0.025(3)
O7 0.066(4) 0.066(4) 0.070(4) 0.007(3) -0.012(3) -0.019(3)
O8 0.074(4) 0.036(2) 0.009(2) 0.0008(18) -0.008(2) 0.011(2)
O9 0.073(4) 0.033(2) 0.021(2) -0.001(2) -0.007(2) 0.008(2)
O10 0.102(5) 0.029(2) 0.017(2) 0.0019(19) 0.005(2) 0.007(3)
O11 0.070(4) 0.044(3) 0.012(2) -0.004(2) 0.008(2) -0.004(2)
O12 0.041(3) 0.0179(18) 0.022(2) -0.0006(17) -0.0062(18) -0.0057(16)
O13 0.036(3) 0.053(3) 0.111(6) 0.027(4) 0.000(3) 0.012(2)
O14 0.100(5) 0.031(3) 0.022(2) -0.007(2) 0.009(3) -0.022(3)
O15 0.085(4) 0.033(3) 0.019(2) -0.002(2) -0.001(2) -0.012(3)
O16 0.118(5) 0.021(2) 0.015(2) -0.0005(18) 0.006(3) -0.006(2)
O17 0.109(5) 0.027(2) 0.017(2) 0.0003(18) 0.011(3) 0.002(3)
O18 0.090(5) 0.069(4) 0.054(4) 0.002(3) 0.000(3) -0.020(4)
O90 0.082(6) 0.075(6) 0.046(4) 0.019(4) 0.003(4) -0.006(5)
N1 0.064(5) 0.095(6) 0.035(4) 0.016(4) 0.012(3) 0.014(4)
N2 0.046(4) 0.056(4) 0.098(6) 0.019(4) 0.014(4) 0.012(3)
C1A 0.059(14) 0.053(14) 0.078(16) -0.017(12) 0.019(12) -0.031(10)
C1B 0.11(2) 0.15(3) 0.11(2) -0.01(2) -0.023(17) -0.11(2)
C2A 0.10(3) 0.11(3) 0.08(3) -0.01(2) -0.01(2) 0.04(2)
C2B 0.035(10) 0.41(6) 0.14(3) -0.11(4) -0.020(12) 0.032(19)
C3 0.047(10) 0.19(3) 0.43(6) -0.20(3) 0.000 0.000
C4 0.098(7) 0.048(4) 0.024(3) 0.006(3) 0.019(4) 0.000(4)
C5 0.077(6) 0.054(5) 0.039(4) 0.007(4) -0.004(4) 0.012(4)
C6 0.075(9) 0.065(7) 0.031(5) 0.003(6) 0.000 0.000
C7 0.033(3) 0.039(3) 0.026(3) -0.003(3) 0.000(3) -0.004(3)
C8 0.048(4) 0.042(4) 0.046(5) 0.002(3) 0.000(3) 0.001(3)
C9 0.029(5) 0.051(6) 0.048(6) 0.002(5) 0.000 0.000
C10 0.095(7) 0.035(4) 0.047(4) 0.002(4) -0.001(5) -0.014(4)
C11 0.122(9) 0.045(5) 0.052(5) 0.003(4) -0.002(6) -0.012(5)
C12 0.102(12) 0.055(7) 0.070(9) -0.003(7) 0.000 0.000
C13 0.059(7) 0.075(7) 0.137(11) 0.024(7) -0.007(7) 0.014(5)
C14 0.050(5) 0.068(6) 0.076(7) 0.009(5) 0.005(4) 0.019(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
V1 O3 1.596(6) . ?
V1 O4 1.954(5) . ?
V1 O1 1.972(5) . ?
V1 O5 1.982(6) . ?
V1 O2 1.990(5) . ?
V2 O7 1.575(7) . ?
V2 O6 1.936(5) . ?
V2 O8 1.958(5) . ?
V2 O9 1.977(5) . ?
V2 O5 1.978(6) . ?
V2 H5' 2.07(7) . ?
V3 O13 1.581(5) . ?
V3 O15 1.929(5) . ?
V3 O11 1.930(5) . ?
V3 O14 1.995(5) . ?
V3 O12 2.015(4) . ?
V4 O18 1.633(8) . ?
V4 O15 1.959(5) . ?
V4 O10 1.975(5) 3_564 ?
V4 O17 1.982(5) . ?
V4 O16 1.995(5) . ?
P1 O17 1.495(5) 3_575 ?
P1 O6 1.521(5) . ?
P1 O4 1.522(5) . ?
P1 C1B 1.783(5) . ?
P1 C1A 1.785(5) . ?
P2 O9 1.519(6) . ?
P2 O11 1.526(4) . ?
P2 O10 1.526(5) . ?
P2 C4 1.777(9) . ?
P3 O1 1.514(5) 3_574 ?
P3 O8 1.525(4) . ?
P3 O12 1.533(4) . ?
P3 C7 1.790(6) . ?
P4 O16 1.512(5) . ?
P4 O14 1.522(5) . ?
P4 O2 1.556(6) 3_564 ?
P4 C10 1.758(9) . ?
O1 P3 1.514(5) 3_575 ?
O2 P4 1.557(6) 3_565 ?
O5 H5' 0.51(6) . ?
O10 V4 1.975(5) 3_565 ?
O17 P1 1.495(5) 3_574 ?
N1 C13 1.493(13) . ?
N2 C14 1.486(12) . ?
C1A C2A 1.530(2) . ?
C1B C2B 1.528(5) . ?
C2A C3 1.530(2) . ?
C3 C2A 1.530(2) 4 ?
C3 C2B 1.531(5) 4 ?
C4 C5 1.505(12) . ?
C5 C6 1.486(11) . ?
C6 C5 1.486(11) 4 ?
C7 C8 1.549(9) . ?
C8 C9 1.528(9) . ?
C9 C8 1.528(9) 4 ?
C10 C11 1.551(14) . ?
C11 C12 1.506(12) . ?
C12 C11 1.506(12) 4 ?
C13 C14 1.439(14) . ?
|
1101215.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101215.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_1101215
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C4 H11 N O7 P2 V'
_chemical_formula_weight 298.02
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 103.401(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.2895(15)
_cell_length_b 13.4657(16)
_cell_length_c 6.0846(7)
_cell_measurement_temperature 90(2)
_cell_volume 979.5(2)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.021
_cod_duplicate_entry 1101193
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101215
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
V1 V 0.28394(5) 0.36543(5) 1.10959(10) 0.00656(19) Uani 1 1 d . . .
P1 P 0.38941(8) 0.35477(7) 0.65957(16) 0.0072(2) Uani 1 1 d . . .
P2 P 0.25094(8) 0.61154(7) 1.02593(17) 0.0094(2) Uani 1 1 d . . .
O1 O 0.3955(2) 0.2580(2) 1.1687(5) 0.0093(5) Uani 1 1 d . . .
O2 O 0.3254(2) 0.3961(2) 1.4314(5) 0.0103(5) Uani 1 1 d . . .
O3 O 0.1677(2) 0.3080(2) 1.0457(5) 0.0120(6) Uani 1 1 d . . .
O4 O 0.3376(2) 0.4008(2) 0.8432(5) 0.0106(5) Uani 1 1 d . . .
O5 O 0.2244(2) 0.5060(2) 1.0871(5) 0.0085(5) Uani 1 1 d . . .
O6 O 0.2119(3) 0.6753(2) 1.2096(5) 0.0158(6) Uani 1 1 d . . .
H6 H 0.2107 0.7356 1.1737 0.024 Uiso 1 1 calc R . .
O7 O 0.1934(3) 0.6421(2) 0.7876(5) 0.0153(6) Uani 1 1 d . . .
N1 N 0.1057(3) 0.5156(3) 0.4417(6) 0.0115(6) Uani 1 1 d . . .
H1A H 0.1451 0.5482 0.5681 0.014 Uiso 1 1 calc R . .
H1B H 0.1515 0.5093 0.3424 0.014 Uiso 1 1 calc R . .
C1 C 0.5311(3) 0.3987(3) 0.7070(7) 0.0112(7) Uani 1 1 d . . .
H1C H 0.5657 0.3718 0.5879 0.013 Uiso 1 1 calc R . .
H1D H 0.5306 0.4720 0.6947 0.013 Uiso 1 1 calc R . .
C2 C 0.3975(3) 0.6315(3) 1.0608(7) 0.0119(7) Uani 1 1 d . . .
H2A H 0.4233 0.5935 0.9430 0.014 Uiso 1 1 calc R . .
H2B H 0.4103 0.7028 1.0361 0.014 Uiso 1 1 calc R . .
C3 C 0.0049(3) 0.5752(3) 0.3338(7) 0.0152(8) Uani 1 1 d . . .
H3A H -0.0351 0.5423 0.1926 0.018 Uiso 1 1 calc R . .
H3B H 0.0284 0.6419 0.2946 0.018 Uiso 1 1 calc R . .
C4 C 0.0731(3) 0.4147(3) 0.5070(7) 0.0128(8) Uani 1 1 d . . .
H4A H 0.1408 0.3772 0.5821 0.015 Uiso 1 1 calc R . .
H4B H 0.0352 0.3776 0.3702 0.015 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
V1 0.0057(3) 0.0046(3) 0.0090(3) 0.0000(2) 0.0009(2) 0.0000(2)
P1 0.0065(4) 0.0059(4) 0.0090(4) 0.0000(3) 0.0011(3) -0.0006(3)
P2 0.0095(5) 0.0064(4) 0.0120(5) 0.0001(3) 0.0019(3) -0.0005(3)
O1 0.0094(12) 0.0059(12) 0.0122(13) 0.0007(10) 0.0021(10) 0.0015(10)
O2 0.0121(13) 0.0093(13) 0.0092(12) -0.0002(10) 0.0017(10) 0.0014(10)
O3 0.0098(13) 0.0075(13) 0.0175(14) 0.0003(10) 0.0004(10) -0.0014(10)
O4 0.0140(13) 0.0078(12) 0.0109(12) 0.0005(10) 0.0048(10) 0.0025(10)
O5 0.0071(12) 0.0056(12) 0.0127(12) 0.0011(10) 0.0018(10) 0.0002(9)
O6 0.0210(15) 0.0084(13) 0.0194(15) -0.0022(11) 0.0074(12) 0.0022(12)
O7 0.0204(15) 0.0097(14) 0.0140(14) 0.0027(10) 0.0003(11) -0.0007(11)
N1 0.0084(15) 0.0116(15) 0.0151(15) -0.0005(12) 0.0040(12) -0.0015(12)
C1 0.0088(17) 0.0112(18) 0.0133(17) 0.0010(14) 0.0017(14) -0.0030(14)
C2 0.0039(16) 0.0155(19) 0.0150(18) 0.0023(14) -0.0006(13) -0.0007(14)
C3 0.0129(19) 0.016(2) 0.0167(19) 0.0039(15) 0.0045(15) 0.0006(15)
C4 0.0078(17) 0.0090(18) 0.022(2) 0.0022(14) 0.0042(14) 0.0018(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.592(3) . ?
V1 O4 1.945(3) . ?
V1 O2 1.950(3) . ?
V1 O1 1.968(3) . ?
V1 O5 2.022(3) . ?
P1 O1 1.521(3) 4_565 ?
P1 O2 1.533(3) 1_554 ?
P1 O4 1.539(3) . ?
P1 C1 1.798(4) . ?
P2 O7 1.515(3) . ?
P2 O5 1.523(3) . ?
P2 O6 1.570(3) . ?
P2 C2 1.784(4) . ?
O1 P1 1.521(3) 4_566 ?
O2 P1 1.533(3) 1_556 ?
O6 H6 0.8400 . ?
N1 C3 1.494(5) . ?
N1 C4 1.496(5) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C1 C2 1.535(5) 3_667 ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C1 1.535(5) 3_667 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.518(6) 3_566 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C3 1.518(6) 3_566 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
|
1101216.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101216.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_1101216
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C6 H15 N O7 P2 V'
_chemical_formula_weight 326.07
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 98.7300(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.6046(10)
_cell_length_b 13.4811(9)
_cell_length_c 6.0678(4)
_cell_measurement_temperature 90(2)
_cell_volume 1180.82(14)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.834
_cod_duplicate_entry 1101194
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101216
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
V1 V 0.23571(4) 0.86561(5) 1.06952(11) 0.00435(17) Uani 1 1 d . . .
P1 P 0.20769(7) 1.11209(7) 0.98854(17) 0.0068(2) Uani 1 1 d . . .
P2 P 0.32297(7) 0.85398(7) 0.60225(16) 0.0048(2) Uani 1 1 d . . .
O1 O 0.1527(2) 1.1444(2) 0.7701(5) 0.0104(6) Uani 1 1 d . . .
O2 O 0.1848(2) 1.1753(2) 1.1901(5) 0.0118(6) Uani 1 1 d . . .
H2 H 0.1870 1.1389 1.3031 0.018 Uiso 1 1 calc R . .
O3 O 0.1876(2) 1.0065(2) 1.0569(5) 0.0068(5) Uani 1 1 d . . .
O4 O 0.1392(2) 0.8090(2) 1.0207(5) 0.0109(6) Uani 1 1 d . . .
O5 O 0.2826(2) 0.9011(2) 0.7969(5) 0.0089(6) Uani 1 1 d . . .
O6 O 0.2676(2) 0.8953(2) 1.3871(5) 0.0084(6) Uani 1 1 d . . .
O7 O 0.32788(19) 0.7584(2) 1.1130(4) 0.0058(5) Uani 1 1 d . . .
N1 N 0.0889(2) 1.0156(3) 0.4311(6) 0.0091(7) Uani 1 1 d . . .
H1A H 0.1285 1.0083 0.3277 0.011 Uiso 1 1 calc R . .
H1B H 0.1198 1.0498 0.5510 0.011 Uiso 1 1 calc R . .
C1 C 0.4399(3) 0.8979(3) 0.6170(7) 0.0093(7) Uani 1 1 d . . .
H1C H 0.4643 0.8755 0.4818 0.011 Uiso 1 1 calc R . .
H1D H 0.4390 0.9713 0.6151 0.011 Uiso 1 1 calc R . .
C2 C 0.5063(3) 0.8638(3) 0.8210(7) 0.0131(8) Uani 1 1 d . . .
H2A H 0.5069 0.7904 0.8259 0.016 Uiso 1 1 calc R . .
H2B H 0.4837 0.8880 0.9572 0.016 Uiso 1 1 calc R . .
C3 C 0.6046(3) 0.9013(3) 0.8198(7) 0.0113(8) Uani 1 1 d . . .
H3A H 0.6272 0.8767 0.6841 0.014 Uiso 1 1 calc R . .
H3B H 0.6037 0.9747 0.8133 0.014 Uiso 1 1 calc R . .
C4 C 0.3285(3) 1.1315(3) 0.9759(7) 0.0113(8) Uani 1 1 d . . .
H4A H 0.3444 1.0957 0.8444 0.014 Uiso 1 1 calc R . .
H4B H 0.3384 1.2031 0.9517 0.014 Uiso 1 1 calc R . .
C5 C 0.0620(3) 0.9158(3) 0.5056(7) 0.0105(8) Uani 1 1 d . . .
H5A H 0.1179 0.8799 0.5767 0.013 Uiso 1 1 calc R . .
H5B H 0.0332 0.8768 0.3751 0.013 Uiso 1 1 calc R . .
C6 C -0.0055(3) 0.9263(3) 0.6700(7) 0.0113(8) Uani 1 1 d . . .
H6A H -0.0250 0.8598 0.7137 0.014 Uiso 1 1 calc R . .
H6B H 0.0252 0.9605 0.8058 0.014 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
V1 0.0051(3) 0.0035(3) 0.0044(3) -0.0001(2) 0.0005(2) 0.0002(2)
P1 0.0075(5) 0.0056(4) 0.0069(4) 0.0008(3) 0.0000(3) 0.0000(3)
P2 0.0052(4) 0.0047(4) 0.0045(4) -0.0001(3) 0.0011(3) -0.0005(3)
O1 0.0121(14) 0.0086(13) 0.0092(13) 0.0015(10) -0.0023(11) -0.0003(11)
O2 0.0177(15) 0.0078(13) 0.0102(14) -0.0010(11) 0.0035(12) 0.0015(11)
O3 0.0092(13) 0.0047(12) 0.0066(12) 0.0003(10) 0.0018(10) 0.0006(10)
O4 0.0093(14) 0.0085(13) 0.0146(14) 0.0004(11) 0.0012(11) -0.0001(11)
O5 0.0141(14) 0.0060(13) 0.0070(13) -0.0002(10) 0.0027(11) 0.0029(10)
O6 0.0113(14) 0.0082(13) 0.0064(12) 0.0006(10) 0.0035(10) 0.0056(11)
O7 0.0056(13) 0.0068(12) 0.0054(12) -0.0008(10) 0.0015(10) 0.0007(10)
N1 0.0084(16) 0.0097(16) 0.0092(15) 0.0005(12) 0.0017(13) 0.0002(12)
C1 0.0078(18) 0.0083(17) 0.0115(18) -0.0024(14) 0.0008(14) -0.0010(14)
C2 0.0075(19) 0.017(2) 0.015(2) 0.0043(15) 0.0012(15) -0.0026(15)
C3 0.0080(18) 0.0116(19) 0.0142(19) 0.0032(15) 0.0006(15) -0.0026(14)
C4 0.0104(18) 0.0105(18) 0.0132(19) 0.0011(15) 0.0024(15) -0.0021(15)
C5 0.0079(18) 0.0098(18) 0.0139(19) 0.0024(15) 0.0020(15) 0.0008(14)
C6 0.0107(19) 0.0132(19) 0.0103(18) 0.0056(15) 0.0022(15) 0.0005(15)
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
V1 O4 1.591(3) . ?
V1 O5 1.943(3) . ?
V1 O6 1.954(3) . ?
V1 O7 1.966(3) . ?
V1 O3 2.022(3) . ?
P1 O1 1.506(3) . ?
P1 O3 1.524(3) . ?
P1 O2 1.567(3) . ?
P1 C4 1.797(4) . ?
P2 O7 1.517(3) 4_575 ?
P2 O6 1.533(3) 1_554 ?
P2 O5 1.536(3) . ?
P2 C1 1.797(4) . ?
O2 H2 0.8400 . ?
O6 P2 1.533(3) 1_556 ?
O7 P2 1.517(3) 4_576 ?
N1 C5 1.490(5) . ?
N1 C6 1.498(5) 3_576 ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
C1 C2 1.522(6) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C3 1.523(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.523(6) 3_677 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C3 1.523(6) 3_677 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.512(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.498(5) 3_576 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
|
1101217.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101217.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_1101217
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C8 H19 N O7 P2 V'
_chemical_formula_weight 354.12
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 95.026(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.941(3)
_cell_length_b 13.470(2)
_cell_length_c 6.0553(10)
_cell_measurement_temperature 90(2)
_cell_volume 1376.5(4)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 1.709
_cod_duplicate_entry 1101195
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101217
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
V1 V 0.20164(4) 0.36569(4) 1.03372(10) 0.00392(15) Uani 1 1 d . . .
P1 P 0.17725(6) 0.61240(7) 0.95695(16) 0.0074(2) Uani 1 1 d . . .
P2 P 0.27679(6) 0.35415(7) 0.55265(15) 0.00468(19) Uani 1 1 d . . .
O1 O 0.12848(16) 0.6454(2) 0.7508(5) 0.0108(6) Uani 1 1 d . . .
O2 O 0.16040(18) 0.6746(2) 1.1679(5) 0.0132(6) Uani 1 1 d . . .
H2 H 0.1461 0.7322 1.1292 0.020 Uiso 1 1 calc R . .
O3 O 0.16018(16) 0.50659(19) 1.0276(4) 0.0068(5) Uani 1 1 d . . .
O4 O 0.24193(16) 0.4012(2) 0.7542(4) 0.0080(5) Uani 1 1 d . . .
O5 O 0.11877(16) 0.3091(2) 1.0008(5) 0.0092(5) Uani 1 1 d . . .
O6 O 0.23017(16) 0.39648(19) 1.3450(4) 0.0075(5) Uani 1 1 d . . .
O7 O 0.28010(15) 0.25825(19) 1.0621(4) 0.0055(5) Uani 1 1 d . . .
N1 N 0.07616(19) 0.5159(2) 0.4191(5) 0.0086(6) Uani 1 1 d . . .
H1A H 0.1104 0.5089 0.3104 0.010 Uiso 1 1 calc R . .
H1B H 0.1021 0.5502 0.5352 0.010 Uiso 1 1 calc R . .
C1 C 0.2796(2) 0.6316(3) 0.9159(7) 0.0134(8) Uani 1 1 d . . .
H1C H 0.2914 0.5960 0.7795 0.016 Uiso 1 1 calc R . .
H1D H 0.2878 0.7033 0.8900 0.016 Uiso 1 1 calc R . .
C2 C 0.3395(2) 0.5982(3) 1.1048(7) 0.0135(8) Uani 1 1 d . . .
H2A H 0.3220 0.6222 1.2472 0.016 Uiso 1 1 calc R . .
H2B H 0.3405 0.5247 1.1098 0.016 Uiso 1 1 calc R . .
C3 C 0.4231(2) 0.6363(3) 1.0804(7) 0.0166(8) Uani 1 1 d . . .
H3A H 0.4401 0.6139 0.9362 0.020 Uiso 1 1 calc R . .
H3B H 0.4225 0.7098 1.0799 0.020 Uiso 1 1 calc R . .
C4 C 0.4827(2) 0.6005(3) 1.2651(7) 0.0136(8) Uani 1 1 d . . .
H4A H 0.4850 0.5271 1.2596 0.016 Uiso 1 1 calc R . .
H4B H 0.4634 0.6192 1.4091 0.016 Uiso 1 1 calc R . .
C5 C 0.3774(2) 0.3967(3) 0.5516(6) 0.0087(7) Uani 1 1 d . . .
H5A H 0.3980 0.3759 0.4107 0.010 Uiso 1 1 calc R . .
H5B H 0.3775 0.4702 0.5551 0.010 Uiso 1 1 calc R . .
C6 C 0.4338(2) 0.3587(3) 0.7442(7) 0.0141(8) Uani 1 1 d . . .
H6A H 0.4135 0.3785 0.8862 0.017 Uiso 1 1 calc R . .
H6B H 0.4355 0.2853 0.7395 0.017 Uiso 1 1 calc R . .
C7 C 0.0047(2) 0.5739(3) 0.3289(7) 0.0114(8) Uani 1 1 d . . .
H7A H -0.0212 0.5395 0.1975 0.014 Uiso 1 1 calc R . .
H7B H 0.0213 0.6406 0.2820 0.014 Uiso 1 1 calc R . .
C8 C 0.0531(2) 0.4158(3) 0.4972(7) 0.0097(7) Uani 1 1 d . . .
H8A H 0.1008 0.3798 0.5600 0.012 Uiso 1 1 calc R . .
H8B H 0.0285 0.3769 0.3705 0.012 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
V1 0.0052(3) 0.0020(3) 0.0044(3) -0.0003(2) 0.0001(2) 0.0002(2)
P1 0.0092(5) 0.0044(4) 0.0085(4) 0.0006(3) -0.0001(3) 0.0001(3)
P2 0.0061(4) 0.0036(4) 0.0044(4) -0.0001(3) 0.0005(3) -0.0011(3)
O1 0.0129(13) 0.0064(13) 0.0126(13) 0.0025(11) -0.0027(11) -0.0019(10)
O2 0.0202(16) 0.0062(13) 0.0134(14) -0.0023(11) 0.0019(12) 0.0000(11)
O3 0.0100(13) 0.0051(12) 0.0055(12) 0.0008(9) 0.0013(10) 0.0014(10)
O4 0.0117(13) 0.0061(12) 0.0062(12) 0.0000(10) 0.0012(10) 0.0014(10)
O5 0.0075(13) 0.0058(12) 0.0143(14) 0.0005(10) 0.0002(11) -0.0005(10)
O6 0.0111(13) 0.0046(12) 0.0069(12) -0.0006(10) 0.0012(10) 0.0017(10)
O7 0.0062(12) 0.0050(12) 0.0054(12) -0.0008(9) 0.0012(10) 0.0014(9)
N1 0.0073(15) 0.0103(15) 0.0083(15) -0.0007(12) 0.0021(12) 0.0001(12)
C1 0.0105(18) 0.0119(19) 0.018(2) 0.0039(16) 0.0008(15) -0.0025(15)
C2 0.0080(18) 0.0114(18) 0.021(2) 0.0031(16) -0.0013(15) -0.0027(14)
C3 0.0128(19) 0.017(2) 0.020(2) 0.0038(17) -0.0008(16) -0.0042(16)
C4 0.0082(18) 0.0139(19) 0.019(2) 0.0021(16) 0.0011(16) -0.0021(15)
C5 0.0068(17) 0.0070(17) 0.0121(18) 0.0004(14) 0.0001(14) -0.0007(13)
C6 0.0106(18) 0.014(2) 0.0166(19) 0.0058(16) -0.0027(15) -0.0026(15)
C7 0.0116(19) 0.0110(18) 0.0117(19) 0.0048(15) 0.0016(15) 0.0014(15)
C8 0.0057(17) 0.0095(18) 0.0145(19) 0.0038(14) 0.0040(14) 0.0017(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O5 1.594(3) . ?
V1 O4 1.940(3) . ?
V1 O6 1.949(3) . ?
V1 O7 1.962(3) . ?
V1 O3 2.023(3) . ?
P1 O1 1.503(3) . ?
P1 O3 1.523(3) . ?
P1 O2 1.575(3) . ?
P1 C1 1.792(4) . ?
P2 O7 1.516(3) 4_565 ?
P2 O6 1.535(3) 1_554 ?
P2 O4 1.538(3) . ?
P2 C5 1.798(4) . ?
O6 P2 1.535(3) 1_556 ?
O7 P2 1.516(3) 4_566 ?
N1 C8 1.493(5) . ?
N1 C7 1.503(5) . ?
C1 C2 1.529(6) . ?
C2 C3 1.526(6) . ?
C3 C4 1.518(6) . ?
C4 C6 1.523(6) 3_667 ?
C5 C6 1.531(5) . ?
C6 C4 1.523(5) 3_667 ?
C7 C8 1.505(5) 3_566 ?
C8 C7 1.505(5) 3_566 ?
|
1101218.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101218.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_1101218
loop_
_publ_author_name
'Ouellette, Wayne'
'Yu, Ming Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
Structural Diversity of the Oxovanadium Organodiphosphonate System:
A Platform for the Design of Void Channels
;
_journal_issue 8
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3224
_journal_page_last 3239
_journal_paper_doi 10.1021/ic0517422
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C9 H24 N2 O15 P4 V3'
_chemical_formula_weight 677.00
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 89.994(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.3248(15)
_cell_length_b 13.3361(12)
_cell_length_c 10.1019(9)
_cell_measurement_temperature 90(2)
_cell_volume 2199.3(3)
_diffrn_ambient_temperature 90(2)
_exptl_crystal_density_diffrn 2.045
_cod_duplicate_entry 1101196
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1101218
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
V1 V 1.02370(2) 0.54667(3) 1.24768(3) 0.01093(8) Uani 1 1 d . . .
V2 V 0.74997(2) 0.74997(3) 0.96353(3) 0.01021(8) Uani 1 1 d . . .
V3 V 0.52366(2) 1.04669(3) 0.75232(3) 0.01125(8) Uani 1 1 d . . .
P1 P 1.08665(3) 0.39478(4) 1.49759(5) 0.01071(11) Uani 1 1 d . . .
P2 P 0.91431(3) 0.60619(4) 0.98508(5) 0.01092(11) Uani 1 1 d . . .
P3 P 0.58567(3) 0.89385(4) 0.98501(5) 0.01121(11) Uani 1 1 d . . .
P4 P 0.58665(3) 0.89483(4) 0.50240(5) 0.01105(11) Uani 1 1 d . . .
O1 O 1.07158(10) 0.47978(13) 1.40110(16) 0.0198(3) Uani 1 1 d . . .
O2 O 1.09529(10) 0.45740(13) 1.14037(15) 0.0196(3) Uani 1 1 d . . .
O3 O 1.06956(10) 0.65132(13) 1.24107(17) 0.0209(3) Uani 1 1 d . . .
O4 O 0.92483(9) 0.57169(13) 1.35831(14) 0.0157(3) Uani 1 1 d . . .
O5 O 0.94529(9) 0.54468(12) 1.10114(15) 0.0154(3) Uani 1 1 d . . .
O6 O 0.83150(9) 0.65138(12) 1.02107(15) 0.0158(3) Uani 1 1 d . . .
O7 O 0.67444(9) 0.64287(12) 1.01813(16) 0.0162(3) Uani 1 1 d . . .
O8 O 0.75006(14) 0.74992(13) 0.80634(17) 0.0244(4) Uani 1 1 d . . .
O9 O 0.82560(9) 0.85714(12) 1.01799(15) 0.0161(3) Uani 1 1 d . . .
O10 O 0.66854(9) 0.84857(12) 1.02097(15) 0.0158(3) Uani 1 1 d . . .
O11 O 0.59522(10) 0.95765(13) 0.85958(16) 0.0202(3) Uani 1 1 d . . .
O12 O 0.57168(11) 0.97994(13) 0.59880(16) 0.0208(3) Uani 1 1 d . . .
O13 O 0.56941(10) 1.15138(13) 0.75894(17) 0.0217(3) Uani 1 1 d . . .
O14 O 0.44518(9) 1.04469(12) 0.89876(15) 0.0155(3) Uani 1 1 d . . .
O15 O 0.42481(9) 1.07157(13) 0.64180(15) 0.0163(3) Uani 1 1 d . . .
N1 N 0.23761(13) 1.03252(15) 0.2640(2) 0.0210(4) Uani 1 1 d . . .
H1A H 0.2817 1.0373 0.2126 0.031 Uiso 1 1 calc R . .
H1B H 0.2381 1.0817 0.3235 0.031 Uiso 1 1 calc R . .
H1C H 0.1927 1.0374 0.2144 0.031 Uiso 1 1 calc R . .
N2 N 0.26240(13) 0.46740(15) 0.2641(2) 0.0211(4) Uani 1 1 d . . .
H2A H 0.2189 0.4631 0.2114 0.032 Uiso 1 1 calc R . .
H2B H 0.2608 0.4183 0.3237 0.032 Uiso 1 1 calc R . .
H2C H 0.3078 0.4619 0.2160 0.032 Uiso 1 1 calc R . .
C1 C 1.01441(14) 0.29675(18) 1.4607(2) 0.0195(4) Uani 1 1 d . . .
H1D H 0.9598 0.3255 1.4617 0.023 Uiso 1 1 calc R . .
H1E H 1.0248 0.2732 1.3715 0.023 Uiso 1 1 calc R . .
C2 C 0.98493(15) 0.70551(18) 0.9458(2) 0.0208(5) Uani 1 1 d . . .
H2D H 1.0397 0.6774 0.9440 0.025 Uiso 1 1 calc R . .
H2E H 0.9727 0.7291 0.8572 0.025 Uiso 1 1 calc R . .
C3 C 0.51512(15) 0.79457(19) 0.9457(2) 0.0218(5) Uani 1 1 d . . .
H3A H 0.4603 0.8227 0.9437 0.026 Uiso 1 1 calc R . .
H3B H 0.5274 0.7709 0.8571 0.026 Uiso 1 1 calc R . .
C4 C 0.51436(14) 0.79672(18) 0.5392(2) 0.0204(5) Uani 1 1 d . . .
H4A H 0.5248 0.7732 0.6285 0.025 Uiso 1 1 calc R . .
H4B H 0.4598 0.8254 0.5382 0.025 Uiso 1 1 calc R . .
C5 C 0.23804(16) 0.93439(18) 0.3330(3) 0.0235(5) Uani 1 1 d . . .
H5A H 0.1903 0.9305 0.3900 0.028 Uiso 1 1 calc R . .
H5B H 0.2863 0.9307 0.3889 0.028 Uiso 1 1 calc R . .
C6 C 0.23777(17) 0.84515(19) 0.2403(3) 0.0264(5) Uani 1 1 d . . .
H6A H 0.2814 0.8519 0.1758 0.032 Uiso 1 1 calc R . .
H6B H 0.1861 0.8419 0.1932 0.032 Uiso 1 1 calc R . .
C7 C 0.2500(2) 0.75001(19) 0.3211(3) 0.0306(6) Uani 1 1 d . . .
H7A H 0.2975 0.7591 0.3777 0.037 Uiso 1 1 calc R . .
H7B H 0.2028 0.7410 0.3781 0.037 Uiso 1 1 calc R . .
C8 C 0.26212(17) 0.65483(19) 0.2404(3) 0.0267(5) Uani 1 1 d . . .
H8A H 0.2184 0.6481 0.1761 0.032 Uiso 1 1 calc R . .
H8B H 0.3138 0.6580 0.1932 0.032 Uiso 1 1 calc R . .
C9 C 0.26189(16) 0.56578(18) 0.3330(3) 0.0234(5) Uani 1 1 d . . .
H9A H 0.3096 0.5698 0.3900 0.028 Uiso 1 1 calc R . .
H9B H 0.2137 0.5695 0.3889 0.028 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
V1 0.01176(17) 0.01129(17) 0.00975(16) 0.00044(12) -0.00053(12) 0.00239(13)
V2 0.00936(16) 0.00871(16) 0.01255(16) -0.00012(12) -0.00003(12) -0.00005(12)
V3 0.01194(17) 0.01176(17) 0.01004(16) -0.00051(12) 0.00051(12) 0.00256(13)
P1 0.0099(2) 0.0125(2) 0.0097(2) 0.00084(18) -0.00014(17) 0.00321(18)
P2 0.0101(2) 0.0124(2) 0.0103(2) -0.00028(18) 0.00017(17) 0.00350(19)
P3 0.0102(2) 0.0130(3) 0.0104(2) -0.00005(18) -0.00018(17) 0.00359(19)
P4 0.0099(2) 0.0134(3) 0.0099(2) -0.00045(18) 0.00015(17) 0.00348(19)
O1 0.0228(8) 0.0215(8) 0.0150(7) 0.0065(6) -0.0003(6) 0.0082(7)
O2 0.0196(8) 0.0257(9) 0.0135(7) -0.0069(6) -0.0043(6) 0.0102(7)
O3 0.0206(8) 0.0152(8) 0.0269(9) 0.0019(6) 0.0003(6) -0.0007(6)
O4 0.0140(7) 0.0224(8) 0.0107(7) -0.0009(6) 0.0004(5) 0.0024(6)
O5 0.0152(7) 0.0191(8) 0.0117(7) 0.0013(6) -0.0030(5) 0.0035(6)
O6 0.0121(7) 0.0141(7) 0.0212(8) 0.0025(6) 0.0029(6) 0.0048(6)
O7 0.0116(7) 0.0143(8) 0.0226(8) 0.0032(6) -0.0032(6) -0.0041(6)
O8 0.0356(10) 0.0217(8) 0.0158(8) -0.0001(6) -0.0004(7) -0.0017(7)
O9 0.0121(7) 0.0149(8) 0.0214(8) -0.0032(6) 0.0033(6) -0.0043(6)
O10 0.0119(7) 0.0144(7) 0.0210(8) -0.0022(6) -0.0031(6) 0.0045(6)
O11 0.0202(8) 0.0268(9) 0.0137(7) 0.0069(6) 0.0044(6) 0.0103(7)
O12 0.0227(8) 0.0245(9) 0.0152(7) -0.0069(6) 0.0000(6) 0.0093(7)
O13 0.0213(8) 0.0157(8) 0.0281(9) -0.0015(7) 0.0001(7) -0.0005(6)
O14 0.0150(7) 0.0198(8) 0.0118(7) -0.0013(6) 0.0026(5) 0.0037(6)
O15 0.0140(7) 0.0237(8) 0.0113(7) 0.0014(6) -0.0003(5) 0.0024(6)
N1 0.0251(10) 0.0148(9) 0.0231(10) -0.0007(7) -0.0005(8) 0.0014(8)
N2 0.0252(10) 0.0159(10) 0.0223(10) 0.0014(7) -0.0003(8) 0.0009(8)
C1 0.0165(10) 0.0184(11) 0.0234(11) -0.0021(9) -0.0046(8) 0.0002(9)
C2 0.0200(11) 0.0172(11) 0.0252(12) 0.0022(9) 0.0093(9) 0.0004(9)
C3 0.0205(11) 0.0204(11) 0.0247(12) -0.0033(9) -0.0091(9) 0.0010(9)
C4 0.0169(10) 0.0198(11) 0.0246(12) 0.0034(9) 0.0048(8) 0.0000(9)
C5 0.0253(12) 0.0176(11) 0.0276(12) 0.0020(9) 0.0015(9) 0.0012(9)
C6 0.0267(13) 0.0164(11) 0.0362(14) -0.0023(10) -0.0042(10) 0.0015(10)
C7 0.0354(14) 0.0157(11) 0.0408(15) -0.0006(10) 0.0010(12) -0.0005(10)
C8 0.0279(13) 0.0163(11) 0.0359(14) 0.0018(10) 0.0057(10) 0.0018(10)
C9 0.0258(12) 0.0168(11) 0.0277(12) -0.0013(9) -0.0002(9) 0.0005(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5851(17) . ?
V1 O1 1.9517(16) . ?
V1 O5 1.9573(15) . ?
V1 O2 1.9895(16) . ?
V1 O4 1.9912(15) . ?
V2 O8 1.5880(17) . ?
V2 O10 1.9577(16) . ?
V2 O6 1.9591(15) . ?
V2 O7 1.9659(16) . ?
V2 O9 1.9671(16) . ?
V3 O13 1.5848(17) . ?
V3 O12 1.9524(16) . ?
V3 O14 1.9570(15) . ?
V3 O11 1.9872(16) . ?
V3 O15 1.9901(16) . ?
P1 O1 1.5152(16) . ?
P1 O9 1.5259(16) 2_747 ?
P1 O4 1.5343(15) 3_768 ?
P1 C1 1.800(2) . ?
P2 O5 1.5178(15) . ?
P2 O6 1.5241(15) . ?
P2 O2 1.5330(16) 3_767 ?
P2 C2 1.800(2) . ?
P3 O14 1.5178(16) 3_677 ?
P3 O10 1.5254(15) . ?
P3 O11 1.5342(16) . ?
P3 C3 1.799(2) . ?
P4 O12 1.5154(17) . ?
P4 O7 1.5270(16) 4_575 ?
P4 O15 1.5355(15) 3_676 ?
P4 C4 1.801(2) . ?
O2 P2 1.5329(16) 3_767 ?
O4 P1 1.5343(15) 3_768 ?
O7 P4 1.5271(16) 4_576 ?
O9 P1 1.5259(16) 2_757 ?
O14 P3 1.5178(16) 3_677 ?
O15 P4 1.5355(15) 3_676 ?
N1 C5 1.483(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C9 1.485(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C1 C2 1.540(3) 2_747 ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 C1 1.540(3) 2_757 ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C3 C4 1.541(4) 4_576 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C3 1.541(4) 4_575 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.515(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.522(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.521(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.512(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
|
1101219.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-16 14:49:56 +0200 (Wed, 16 Mar 2016) $
#$Revision: 178223 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101219.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_1101219
loop_
_publ_author_name
'Goto, Yuya'
'Kamata, Keigo'
'Yamaguchi, Kazuya'
'Uehara, Kazuhiro'
'Hikichi, Shiro'
'Mizuno, Noritaka'
_publ_section_title
;
Synthesis, Structural Characterization, and Catalytic Performance of
Dititanium-Substituted \g-Keggin Silicotungstate
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 2347
_journal_page_last 2356
_journal_paper_doi 10.1021/ic052179q
_journal_volume 45
_journal_year 2006
_chemical_formula_sum 'C258 H579 N17 O156 Si4 Ti8 W40'
_chemical_formula_weight 14265.94
_space_group_IT_number 33
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_audit_creation_date 2005-10-26T15:24:59-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 29.166
_cell_length_b 38.497
_cell_length_c 37.405
_cell_measurement_temperature 293(2)
_cell_volume 41998.1
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 42
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -41
_diffrn_reflns_number 30698
_diffrn_reflns_theta_full 23.27
_diffrn_reflns_theta_max 23.27
_diffrn_reflns_theta_min 2.05
_exptl_absorpt_coefficient_mu 11.132
_exptl_absorpt_correction_type none
_exptl_crystal_density_diffrn 2.256
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 26744
_refine_diff_density_max 1.835
_refine_diff_density_min -2.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.093(9)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1166
_refine_ls_number_reflns 30698
_refine_ls_number_restraints 36
_refine_ls_restrained_S_all 1.005
_refine_ls_R_factor_gt 0.0444
_refine_ls_shift/su_max 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1266
_reflns_number_gt 25900
_reflns_number_total 30698
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P ? ? ?'
_cod_database_code 1101219
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
N901 N 0.1967(10) 0.2672(7) 0.7157(8) 0.083(9) Uiso 1 d . . .
C901 C 0.1724(13) 0.2460(9) 0.6519(10) 0.081(10) Uiso 1 d . . .
C902 C 0.1855(12) 0.2603(9) 0.6874(10) 0.075(10) Uiso 1 d . . .
N2B N 0.2075 0.5163 1.2685 0.071 Uiso 0.46 d P . .
N20B N 0.2463 0.4798 1.313 0.071 Uiso 0.54 d P . .
C251 C 0.2489 0.4389 1.2755 0.121 Uiso 0.33 d P . .
C271 C 0.2788 0.4687 1.2978 0.121 Uiso 0.67 d P . .
C252 C 0.2753 0.4489 1.2738 0.117 Uiso 0.57 d P . .
C272 C 0.3193 0.4354 1.2458 0.117 Uiso 0.43 d P . .
C253 C 0.328 0.4211 1.268 0.233 Uiso 1 d . . .
C275 C 0.1928 0.5094 1.2295 0.119 Uiso 0.35 d P . .
C255 C 0.2393 0.4979 1.2687 0.119 Uiso 0.65 d P . .
C256 C 0.2252 0.5457 1.2614 0.204 Uiso 0.53 d P . .
C276 C 0.2645 0.5002 1.2354 0.204 Uiso 0.47 d P . .
C257 C 0.1892 0.5603 1.2253 0.148 Uiso 1 d . . .
C259 C 0.1989 0.4646 1.3204 0.163 Uiso 1 d . . .
C260 C 0.1875 0.4297 1.3448 0.334 Uiso 1 d . . .
C261 C 0.1254 0.4278 1.3587 0.338 Uiso 1 d . . .
C283 C 0.2729 0.4759 1.3584 0.074 Uiso 0.27 d P . .
C263 C 0.2369 0.5063 1.3067 0.074 Uiso 0.73 d P . .
C284 C 0.2495 0.4853 1.3587 0.153 Uiso 0.41 d P . .
C264 C 0.2672 0.5329 1.3259 0.153 Uiso 0.59 d P . .
C265 C 0.2679 0.5677 1.3428 0.285 Uiso 1 d . . .
N3B N 0.3449 0.0756 0.0619 0.082 Uiso 0.36 d P . .
N30B N 0.3566 0.1075 0.0821 0.082 Uiso 0.64 d P . .
C351 C 0.3677 0.0571 0.0534 0.079 Uiso 1 d . . .
C372 C 0.4025 0.0133 0.0446 0.058 Uiso 0.27 d P . .
C352 C 0.4066 0.0504 0.0586 0.058 Uiso 0.73 d P . .
C353 C 0.4881 0.0165 0.0569 0.088 Uiso 0.49 d P . .
C373 C 0.4403 0.0269 0.0416 0.088 Uiso 0.51 d P . .
C354 C 0.5305 0.0161 0.0381 0.119 Uiso 0.35 d P . .
C374 C 0.4571 0.0114 0.0315 0.119 Uiso 0.65 d P . .
C355 C 0.3256 0.0364 0.0776 0.156 Uiso 1 d . . .
C375 C 0.3314 0.0443 0.1109 0.18 Uiso 1 d . . .
C356 C 0.3032 0.0043 0.1288 0.152 Uiso 1 d . . .
C357 C 0.3148 -0.0308 0.1096 0.138 Uiso 1 d . . .
C363 C 0.319 0.1169 0.081 0.091 Uiso 0.55 d P . .
C383 C 0.3196 0.1267 0.1209 0.091 Uiso 0.45 d P . .
C364 C 0.3196 0.145 0.0926 0.077 Uiso 0.56 d P . .
C384 C 0.3379 0.1562 0.1332 0.077 Uiso 0.44 d P . .
C365 C 0.3255 0.1666 0.1103 0.147 Uiso 1 d . . .
C359 C 0.3527 0.0769 0.0104 0.229 Uiso 1 d . . .
W8C W 0.43926(4) 0.77424(3) 1.09026(7) 0.0392(3) Uani 1 d . . .
W4D W 0.61014(4) 0.55288(2) 1.22678(7) 0.0326(2) Uani 1 d . . .
W5B W 0.55065(4) 0.13034(3) 0.28185(7) 0.0407(3) Uani 1 d . . .
W8A W 0.48464(4) 0.27447(3) 0.04980(7) 0.0363(3) Uani 1 d . . .
W11D W 0.52278(4) 0.52884(3) 1.34092(7) 0.0374(3) Uani 1 d . . .
W12A W 0.57881(4) 0.28878(3) 0.00241(7) 0.0383(3) Uani 1 d . . .
W5A W 0.43082(4) 0.19137(3) 0.02556(7) 0.0340(2) Uani 1 d . . .
W12C W 0.52016(4) 0.79346(3) 1.03097(7) 0.0408(3) Uani 1 d . . .
W6B W 0.38619(4) 0.06982(3) 0.21259(7) 0.0374(3) Uani 1 d . . .
W3C W 0.60784(4) 0.68532(3) 1.06733(7) 0.0395(3) Uani 1 d . . .
W5D W 0.55572(4) 0.60281(2) 1.28579(7) 0.0333(2) Uani 1 d . . .
W4C W 0.42560(4) 0.63303(3) 1.01875(7) 0.0376(3) Uani 1 d . . .
W6C W 0.55675(4) 0.74899(3) 1.11229(7) 0.0372(3) Uani 1 d . . .
W10D W 0.58195(4) 0.47217(2) 1.27395(7) 0.0358(3) Uani 1 d . . .
W3D W 0.43153(4) 0.49504(3) 1.17678(7) 0.0419(3) Uani 1 d . . .
W9D W 0.48201(4) 0.43972(3) 1.24558(7) 0.0403(3) Uani 1 d . . .
W7D W 0.55427(4) 0.47626(3) 1.18832(7) 0.0388(3) Uani 1 d . . .
W10A W 0.55731(4) 0.17775(3) -0.06700(7) 0.0402(3) Uani 1 d . . .
W9C W 0.57783(4) 0.72207(3) 0.98013(7) 0.0452(3) Uani 1 d . . .
W4A W 0.49419(4) 0.12499(3) -0.00227(7) 0.0382(3) Uani 1 d . . .
W5C W 0.37467(4) 0.69630(3) 1.06441(7) 0.0347(2) Uani 1 d . . .
W3B W 0.45008(4) 0.00968(3) 0.17256(7) 0.0435(3) Uani 1 d . . .
W3A W 0.65740(4) 0.18804(3) 0.06621(7) 0.0363(2) Uani 1 d . . .
W6A W 0.59506(4) 0.25539(2) 0.09311(7) 0.0319(2) Uani 1 d . . .
W12B W 0.40482(4) 0.03047(3) 0.30039(7) 0.0401(3) Uani 1 d . . .
W12D W 0.42304(4) 0.49472(3) 1.31388(7) 0.0434(3) Uani 1 d . . .
W11A W 0.48611(4) 0.25255(3) -0.03578(7) 0.0368(3) Uani 1 d . . .
W8B W 0.42697(4) 0.11462(3) 0.29297(7) 0.0406(3) Uani 1 d . . .
W10B W 0.57167(4) -0.00016(3) 0.29409(7) 0.0463(3) Uani 1 d . . .
W6D W 0.37679(4) 0.54314(3) 1.23722(7) 0.0437(3) Uani 1 d . . .
W11C W 0.41760(4) 0.76421(3) 1.00426(7) 0.0420(3) Uani 1 d . . .
W9B W 0.47918(4) -0.03565(3) 0.25561(7) 0.0462(3) Uani 1 d . . .
W7A W 0.61891(4) 0.13312(3) -0.00828(7) 0.0449(3) Uani 1 d . . .
W7C W 0.54751(4) 0.64027(3) 0.99448(7) 0.0442(3) Uani 1 d . . .
W8D W 0.43831(4) 0.57997(3) 1.31378(7) 0.0438(3) Uani 1 d . . .
W11B W 0.49745(4) 0.06528(3) 0.33991(7) 0.0420(3) Uani 1 d . . .
W4B W 0.61607(4) 0.07210(3) 0.24047(7) 0.0437(3) Uani 1 d . . .
W9A W 0.64943(4) 0.21345(3) -0.02788(7) 0.0413(3) Uani 1 d . . .
W10C W 0.47528(4) 0.69298(3) 0.95318(7) 0.0455(3) Uani 1 d . . .
W7B W 0.56622(4) -0.00860(3) 0.20616(7) 0.0503(3) Uani 1 d . . .
Ti2B Ti 0.55317(17) 0.12543(11) 0.19458(13) 0.0376(11) Uani 1 d . . .
Ti2C Ti 0.43861(16) 0.63971(11) 1.10437(14) 0.0362(11) Uani 1 d . . .
Ti1D Ti 0.43847(17) 0.57935(11) 1.17517(14) 0.0405(12) Uani 1 d . . .
Ti1C Ti 0.53441(16) 0.66817(11) 1.12893(13) 0.0346(11) Uani 1 d . . .
Ti2D Ti 0.53415(16) 0.60851(10) 1.20039(13) 0.0340(11) Uani 1 d . . .
Ti1B Ti 0.46751(17) 0.09161(12) 0.15752(14) 0.0408(12) Uani 1 d . . .
Ti1A Ti 0.57060(16) 0.17726(12) 0.11832(13) 0.0369(11) Uani 1 d . . .
Ti2A Ti 0.48484(16) 0.14305(11) 0.08148(13) 0.0360(11) Uani 1 d . . .
N4A N 0.3903 0.2735 0.7407 0.047 Uiso 1 d . . .
C401 C 0.3941 0.2416 0.7641 0.063 Uiso 1 d . . .
C402 C 0.4215 0.2484 0.8011 0.071 Uiso 1 d . . .
C403 C 0.4287 0.2105 0.819 0.07 Uiso 1 d . . .
C404 C 0.4534 0.2153 0.8544 0.094 Uiso 1 d . . .
C405 C 0.3593 0.3005 0.7611 0.057 Uiso 1 d . . .
C406 C 0.3498 0.3295 0.7393 0.085 Uiso 1 d . . .
C407 C 0.3096 0.3526 0.7619 0.061 Uiso 1 d . . .
C408 C 0.2688 0.334 0.7668 0.074 Uiso 1 d . . .
C409 C 0.4378 0.2903 0.7347 0.049 Uiso 1 d . . .
C410 C 0.4754 0.2647 0.7222 0.063 Uiso 1 d . . .
C411 C 0.5199 0.2866 0.7173 0.052 Uiso 1 d . . .
C412 C 0.5583 0.2628 0.7039 0.07 Uiso 1 d . . .
C413 C 0.3749 0.2629 0.705 0.05 Uiso 1 d . . .
C414 C 0.3233 0.2451 0.7047 0.084 Uiso 1 d . . .
C415 C 0.3087 0.2401 0.6672 0.054 Uiso 1 d . . .
C416 C 0.2989 0.2734 0.6469 0.061 Uiso 1 d . . .
N1A N 0.7479 0.4804 0.2594 0.044 Uiso 1 d . . .
C101 C 0.7216 0.5036 0.2867 0.048 Uiso 1 d . . .
C102 C 0.753 0.5155 0.3181 0.068 Uiso 1 d . . .
C103 C 0.7213 0.5452 0.3389 0.064 Uiso 1 d . . .
C104 C 0.7124 0.5778 0.3173 0.047 Uiso 1 d . . .
C105 C 0.7885 0.4993 0.2434 0.064 Uiso 1 d . . .
C106 C 0.7759 0.5338 0.2232 0.048 Uiso 1 d . . .
C107 C 0.8214 0.5468 0.207 0.09 Uiso 1 d . . .
C128 C 0.8259 0.5534 0.2187 0.082 Uiso 0.46 d P . .
C108 C 0.8474 0.5678 0.2427 0.082 Uiso 0.54 d P . .
C109 C 0.7682 0.45 0.2779 0.037 Uiso 1 d . . .
C110 C 0.7281 0.4254 0.2973 0.062 Uiso 1 d . . .
C111 C 0.7585 0.3935 0.3134 0.108 Uiso 1 d . . .
C112 C 0.777 0.4072 0.3468 0.175 Uiso 1 d . . .
C113 C 0.7096 0.4716 0.2318 0.048 Uiso 1 d . . .
C114 C 0.729 0.4466 0.203 0.059 Uiso 1 d . . .
C115 C 0.6918 0.4454 0.1736 0.079 Uiso 1 d . . .
C116 C 0.7046 0.4186 0.1414 0.115 Uiso 1 d . . .
N5A N 0.6586 0.2402 0.8342 0.057 Uiso 1 d . . .
C501 C 0.6127 0.2254 0.8282 0.047 Uiso 1 d . . .
C502 C 0.6052 0.2022 0.7934 0.069 Uiso 1 d . . .
C503 C 0.5529 0.1927 0.7934 0.053 Uiso 1 d . . .
C504 C 0.5419 0.1699 0.762 0.116 Uiso 1 d . . .
C505 C 0.6526 0.2625 0.8686 0.056 Uiso 1 d . . .
C506 C 0.6995 0.2809 0.8819 0.07 Uiso 1 d . . .
C507 C 0.6514 0.2774 0.9251 0.08 Uiso 0.35 d P . .
C527 C 0.6856 0.3055 0.911 0.08 Uiso 0.65 d P . .
C508 C 0.7319 0.3203 0.9256 0.106 Uiso 1 d . . .
C509 C 0.695 0.2131 0.8378 0.068 Uiso 1 d . . .
C510 C 0.6903 0.187 0.8674 0.058 Uiso 1 d . . .
C511 C 0.7247 0.1587 0.8659 0.078 Uiso 1 d . . .
C512 C 0.7224 0.1366 0.9017 0.088 Uiso 1 d . . .
C513 C 0.6737 0.2622 0.8028 0.071 Uiso 1 d . . .
C514 C 0.6381 0.2919 0.7926 0.092 Uiso 1 d . . .
C515 C 0.665 0.3167 0.7612 0.078 Uiso 1 d . . .
C516 C 0.633 0.345 0.7553 0.093 Uiso 1 d . . .
N3A N 0.4896 0.3774 0.9338 0.042 Uiso 1 d . . .
C301 C 0.4802 0.3678 0.9708 0.055 Uiso 1 d . . .
C302 C 0.4674 0.4009 0.9962 0.059 Uiso 1 d . . .
C303 C 0.4521 0.385 1.0334 0.075 Uiso 1 d . . .
C304 C 0.4456 0.4166 1.063 0.094 Uiso 1 d . . .
C305 C 0.502 0.3443 0.915 0.049 Uiso 1 d . . .
C306 C 0.5069 0.3457 0.8735 0.046 Uiso 1 d . . .
C307 C 0.5185 0.3103 0.8611 0.056 Uiso 1 d . . .
C308 C 0.5249 0.3085 0.8181 0.058 Uiso 1 d . . .
C309 C 0.4469 0.396 0.9174 0.051 Uiso 1 d . . .
C310 C 0.4003 0.3714 0.9179 0.082 Uiso 1 d . . .
C311 C 0.3646 0.3855 0.8946 0.147 Uiso 1 d . . .
C312 C 0.35 0.4225 0.9142 0.128 Uiso 1 d . . .
C313 C 0.5247 0.4048 0.9304 0.063 Uiso 1 d . . .
C314 C 0.575 0.3889 0.9373 0.087 Uiso 1 d . . .
C315 C 0.6074 0.4232 0.9261 0.129 Uiso 1 d . . .
C316 C 0.655 0.409 0.9449 0.194 Uiso 1 d . . .
N6A N 0.4953 0.6589 0.6613 0.047 Uiso 1 d . . .
C601 C 0.5048 0.6982 0.6579 0.064 Uiso 1 d . . .
C602 C 0.5262 0.7175 0.6898 0.056 Uiso 1 d . . .
C603 C 0.5296 0.7559 0.6787 0.052 Uiso 1 d . . .
C604 C 0.5542 0.7767 0.706 0.078 Uiso 1 d . . .
C605 C 0.474 0.6489 0.6278 0.051 Uiso 1 d . . .
C606 C 0.4564 0.6104 0.6243 0.07 Uiso 1 d . . .
C607 C 0.4386 0.6023 0.5868 0.061 Uiso 1 d . . .
C608 C 0.3934 0.6256 0.5744 0.118 Uiso 1 d . . .
C609 C 0.5395 0.639 0.6691 0.062 Uiso 1 d . . .
C610 C 0.5796 0.6454 0.6401 0.099 Uiso 1 d . . .
C611 C 0.6167 0.6181 0.6482 0.082 Uiso 1 d . . .
C612 C 0.6394 0.6253 0.6861 0.094 Uiso 0.57 d P . .
C632 C 0.6528 0.6121 0.6208 0.094 Uiso 0.43 d P . .
C613 C 0.4654 0.6506 0.6964 0.061 Uiso 1 d . . .
C614 C 0.4204 0.6679 0.6936 0.075 Uiso 1 d . . .
C615 C 0.3951 0.6572 0.7271 0.126 Uiso 1 d . . .
C616 C 0.3823 0.6271 0.7284 0.231 Uiso 1 d . . .
N7A N 0.4367 0.5855 0.8863 0.084 Uiso 1 d . . .
C701 C 0.4613 0.5791 0.9242 0.096 Uiso 1 d . . .
C702 C 0.477 0.5405 0.929 0.085 Uiso 1 d . . .
C703 C 0.4956 0.5375 0.9639 0.07 Uiso 1 d . . .
C704 C 0.5109 0.499 0.9707 0.095 Uiso 1 d . . .
C705 C 0.4803 0.5841 0.8582 0.08 Uiso 1 d . . .
C706 C 0.5238 0.6075 0.8709 0.137 Uiso 1 d . . .
C707 C 0.5278 0.6204 0.8321 0.167 Uiso 1 d . . .
C708 C 0.5025 0.6508 0.8123 0.118 Uiso 0.69 d P . .
C728 C 0.5271 0.6749 0.8228 0.118 Uiso 0.31 d P . .
C709 C 0.397 0.5588 0.8777 0.083 Uiso 1 d . . .
C710 C 0.3627 0.5563 0.9015 0.112 Uiso 1 d . . .
C711 C 0.3311 0.5266 0.8889 0.11 Uiso 1 d . . .
C712 C 0.2842 0.5204 0.9108 0.086 Uiso 0.76 d P . .
C732 C 0.3378 0.4923 0.8841 0.086 Uiso 0.24 d P . .
C713 C 0.4193 0.6216 0.8845 0.089 Uiso 1 d . . .
C714 C 0.4157 0.6292 0.8493 0.056 Uiso 0.47 d P . .
C734 C 0.3793 0.629 0.8511 0.056 Uiso 0.53 d P . .
C715 C 0.3782 0.6681 0.8484 0.119 Uiso 1 d . . .
C716 C 0.3364 0.6727 0.824 0.176 Uiso 1 d . . .
N8A N 0.2434 0.7599 0.0021 0.098 Uiso 1 d . . .
C801 C 0.2301 0.7836 -0.0272 0.089 Uiso 1 d . . .
C802 C 0.2689 0.8043 -0.0459 0.144 Uiso 1 d . . .
C804 C 0.235 0.8264 -0.0939 0.293 Uiso 1 d . . .
C803 C 0.213 0.7981 -0.1179 0.153 Uiso 0.47 d P . .
C823 C 0.2783 0.8217 -0.0846 0.153 Uiso 0.53 d P . .
C805 C 0.2791 0.7761 0.0262 0.131 Uiso 1 d . . .
C806 C 0.2567 0.8011 0.0446 0.16 Uiso 1 d . . .
C807 C 0.3022 0.8205 0.0699 0.114 Uiso 1 d . . .
C808 C 0.3232 0.8488 0.074 0.212 Uiso 1 d . . .
C809 C 0.201 0.7383 0.0152 0.108 Uiso 1 d . . .
C810 C 0.2124 0.715 0.0439 0.069 Uiso 1 d . . .
C811 C 0.1651 0.6981 0.0506 0.101 Uiso 1 d . . .
C812 C 0.1665 0.6721 0.0813 0.107 Uiso 1 d . . .
C813 C 0.2789 0.7314 -0.0125 0.096 Uiso 1 d . . .
C814 C 0.2159 0.7065 -0.0308 0.099 Uiso 0.31 d P . .
C834 C 0.2567 0.7085 -0.0422 0.099 Uiso 0.69 d P . .
C815 C 0.3025 0.6878 -0.051 0.18 Uiso 1 d . . .
C816 C 0.2937 0.6624 -0.076 0.194 Uiso 1 d . . .
N2A N 0.8068 0.2228 0.018 0.072 Uiso 1 d . . .
C201 C 0.7651 0.2404 0.0216 0.059 Uiso 1 d . . .
C202 C 0.7688 0.2798 0.0251 0.068 Uiso 1 d . . .
C203 C 0.7185 0.2969 0.0263 0.074 Uiso 1 d . . .
C204 C 0.716 0.3336 0.0344 0.085 Uiso 1 d . . .
C205 C 0.8414 0.228 0.0491 0.057 Uiso 1 d . . .
C206 C 0.8204 0.2202 0.0849 0.086 Uiso 1 d . . .
C207 C 0.8543 0.2312 0.1142 0.073 Uiso 1 d . . .
C208 C 0.8393 0.2259 0.1541 0.108 Uiso 1 d . . .
C209 C 0.837 0.2328 -0.0155 0.063 Uiso 1 d . . .
C210 C 0.8173 0.2199 -0.051 0.085 Uiso 1 d . . .
C211 C 0.8387 0.2449 -0.0807 0.086 Uiso 1 d . . .
C212 C 0.8229 0.2247 -0.1181 0.134 Uiso 1 d . . .
C213 C 0.7906 0.185 0.0145 0.072 Uiso 1 d . . .
C214 C 0.8365 0.1549 0.0179 0.092 Uiso 1 d . . .
C215 C 0.8194 0.1242 0.0068 0.119 Uiso 1 d . . .
C216 C 0.7817 0.1085 0.029 0.255 Uiso 1 d . . .
C236 C 0.8452 0.1554 -0.0146 0.05 Uiso 1 d . . .
N1B N 0.3023 0.5613 1.0948 0.109 Uiso 1 d . . .
C151 C 0.2687 0.575 1.0627 0.077 Uiso 1 d . . .
C152 C 0.295 0.6056 1.042 0.095 Uiso 1 d . . .
C153 C 0.2513 0.6184 1.0151 0.114 Uiso 1 d . . .
C154 C 0.2734 0.5927 0.9866 0.275 Uiso 1 d . . .
C155 C 0.2732 0.5332 1.1097 0.132 Uiso 1 d . . .
C156 C 0.2961 0.5145 1.1438 0.145 Uiso 1 d . . .
C157 C 0.2698 0.4782 1.1487 0.12 Uiso 0.61 d P . .
C177 C 0.2126 0.4888 1.1646 0.12 Uiso 0.39 d P . .
C158 C 0.2907 0.4635 1.1854 0.105 Uiso 0.48 d P . .
C178 C 0.2504 0.4938 1.1686 0.105 Uiso 0.52 d P . .
C159 C 0.3477 0.5527 1.0756 0.118 Uiso 1 d . . .
C160 C 0.3493 0.5194 1.0431 0.144 Uiso 1 d . . .
C161 C 0.3854 0.5048 1.0271 0.149 Uiso 1 d . . .
C162 C 0.39 0.4934 0.9918 0.163 Uiso 1 d . . .
C163 C 0.3179 0.5904 1.1167 0.111 Uiso 1 d . . .
C164 C 0.2848 0.6019 1.1356 0.11 Uiso 1 d . . .
C165 C 0.2937 0.6301 1.16 0.103 Uiso 0.65 d P . .
C166 C 0.2721 0.6354 1.1846 0.103 Uiso 0.69 d P . .
C186 C 0.2728 0.656 1.1652 0.103 Uiso 0.66 d P . .
N7B N 0.3138 0.7968 0.7081 0.072 Uiso 1 d . . .
C751 C 0.3654 0.7884 0.7188 0.081 Uiso 1 d . . .
C752 C 0.388 0.7633 0.7443 0.138 Uiso 1 d . . .
C753 C 0.4283 0.7563 0.7469 0.077 Uiso 1 d . . .
C754 C 0.4429 0.7331 0.7785 0.129 Uiso 1 d . . .
C755 C 0.3133 0.8333 0.6879 0.097 Uiso 1 d . . .
C756 C 0.2642 0.8462 0.6772 0.089 Uiso 1 d . . .
C757 C 0.2678 0.862 0.6535 0.056 Uiso 0.46 d P . .
C777 C 0.2672 0.8878 0.6702 0.056 Uiso 0.54 d P . .
C758 C 0.2497 0.8958 0.6234 0.1 Uiso 1 d . . .
C778 C 0.2824 0.8848 0.6455 0.1 Uiso 1 d . . .
C759 C 0.2856 0.8011 0.7335 0.107 Uiso 1 d . . .
C760 C 0.2868 0.8324 0.7674 0.177 Uiso 1 d . . .
C763 C 0.2993 0.7728 0.6668 0.191 Uiso 1 d . . .
C764 C 0.3054 0.7406 0.6768 0.172 Uiso 1 d . . .
C765 C 0.2775 0.7154 0.6503 0.104 Uiso 1 d . . .
C766 C 0.2875 0.6771 0.6563 0.209 Uiso 1 d . . .
N6B N 0.6391 0.554 1.084 0.065 Uiso 1 d . . .
C651 C 0.6714 0.561 1.0547 0.088 Uiso 1 d . . .
C652 C 0.6714 0.5924 1.0394 0.086 Uiso 1 d . . .
C653 C 0.7023 0.5981 0.9981 0.101 Uiso 1 d . . .
C655 C 0.5908 0.5543 1.0698 0.072 Uiso 1 d . . .
C656 C 0.5525 0.5482 1.0955 0.082 Uiso 1 d . . .
C657 C 0.5077 0.5412 1.0767 0.058 Uiso 1 d . . .
C658 C 0.5085 0.496 1.0747 0.108 Uiso 1 d . . .
C659 C 0.644 0.5813 1.1134 0.068 Uiso 1 d . . .
C660 C 0.6905 0.5898 1.1278 0.083 Uiso 1 d . . .
C661 C 0.6901 0.6197 1.1519 0.058 Uiso 1 d . . .
C662 C 0.7327 0.6228 1.1695 0.123 Uiso 1 d . . .
C663 C 0.653 0.5165 1.1006 0.069 Uiso 1 d . . .
C664 C 0.6463 0.487 1.0758 0.081 Uiso 1 d . . .
C665 C 0.6945 0.474 1.0651 0.123 Uiso 1 d . . .
C666 C 0.6905 0.4426 1.0358 0.132 Uiso 1 d . . .
N5B N 0.5313 1.0531 0.8932 0.119 Uiso 1 d . . .
C551 C 0.4992 1.0215 0.8862 0.076 Uiso 1 d . . .
C552 C 0.459 1.0219 0.9218 0.154 Uiso 1 d . . .
C553 C 0.4302 0.9894 0.9106 0.096 Uiso 1 d . . .
C554 C 0.3828 0.9745 0.9361 0.226 Uiso 1 d . . .
C555 C 0.5466 1.0476 0.9296 0.105 Uiso 1 d . . .
C556 C 0.5852 1.0108 0.928 0.188 Uiso 1 d . . .
C557 C 0.6062 1.0279 0.9628 0.457 Uiso 1 d . . .
C558 C 0.5825 1.005 0.9853 0.362 Uiso 1 d . . .
C559 C 0.5114 1.0902 0.892 0.074 Uiso 1 d . . .
C560 C 0.4939 1.0963 0.8599 0.109 Uiso 0.76 d P . .
C580 C 0.443 1.1092 0.873 0.109 Uiso 0.24 d P . .
C561 C 0.4775 1.107 0.886 0.267 Uiso 0.66 d P . .
C581 C 0.404 1.1048 0.8951 0.267 Uiso 0.34 d P . .
C562 C 0.478 1.134 0.8429 0.156 Uiso 1 d . . .
C563 C 0.5816 1.0439 0.8651 0.121 Uiso 0.78 d P . .
C564 C 0.6138 1.0656 0.878 0.121 Uiso 0.79 d P . .
C568 C 0.5953 1.0842 0.85 0.121 Uiso 0.44 d P . .
C565 C 0.6457 1.0751 0.8449 0.077 Uiso 0.58 d P . .
C585 C 0.6296 1.104 0.8269 0.077 Uiso 0.42 d P . .
C566 C 0.6387 1.1015 0.8015 0.086 Uiso 0.45 d P . .
C586 C 0.6409 1.0791 0.8104 0.086 Uiso 0.55 d P . .
N8B N 0.501 0.8896 1.1352 0.077 Uiso 1 d . . .
C851 C 0.5342 0.8617 1.1459 0.084 Uiso 1 d . . .
C852 C 0.5524 0.8707 1.1865 0.098 Uiso 1 d . . .
C853 C 0.5926 0.8452 1.1976 0.098 Uiso 1 d . . .
C854 C 0.6294 0.8527 1.1793 0.05 Uiso 1 d . . .
C855 C 0.4624 0.9016 1.1589 0.089 Uiso 1 d . . .
C856 C 0.4386 0.8748 1.1726 0.087 Uiso 1 d . . .
C857 C 0.3883 0.8807 1.1744 0.136 Uiso 1 d . . .
C858 C 0.3599 0.8528 1.1889 0.091 Uiso 1 d . . .
C859 C 0.5357 0.9233 1.1231 0.091 Uiso 1 d . . .
C860 C 0.5716 0.9147 1.101 0.117 Uiso 1 d . . .
C861 C 0.5915 0.9498 1.0857 0.166 Uiso 1 d . . .
C863 C 0.4815 0.8752 1.0977 0.13 Uiso 1 d . . .
C864 C 0.4528 0.9006 1.0795 0.097 Uiso 1 d . . .
C865 C 0.4558 0.8989 1.0359 0.129 Uiso 0.38 d P . .
C885 C 0.4135 0.8794 1.0531 0.129 Uiso 0.62 d P . .
C866 C 0.3824 0.905 1.0299 0.108 Uiso 1 d . . .
N4B N 0.5053 0.8116 0.8952 0.082 Uiso 1 d . . .
C451 C 0.5208 0.8058 0.8543 0.083 Uiso 1 d . . .
C452 C 0.5428 0.7711 0.8499 0.1 Uiso 1 d . . .
C453 C 0.561 0.7677 0.8107 0.104 Uiso 1 d . . .
C454 C 0.577 0.7318 0.8019 0.115 Uiso 1 d . . .
C455 C 0.5384 0.8063 0.9226 0.065 Uiso 1 d . . .
C456 C 0.6151 0.8257 0.9484 0.121 Uiso 1 d . . .
C476 C 0.5866 0.8363 0.9183 0.121 Uiso 1 d . . .
C457 C 0.6717 0.8287 0.9164 0.145 Uiso 0.64 d P . .
C477 C 0.6583 0.8518 0.9466 0.145 Uiso 0.36 d P . .
C459 C 0.4781 0.8456 0.8964 0.122 Uiso 1 d . . .
C460 C 0.4431 0.8567 0.9289 0.142 Uiso 1 d . . .
C461 C 0.4433 0.8864 0.9221 0.123 Uiso 0.59 d P . .
C481 C 0.4828 0.8577 0.9374 0.123 Uiso 0.41 d P . .
C463 C 0.4641 0.7856 0.9041 0.062 Uiso 1 d . . .
C464 C 0.4229 0.7867 0.8792 0.102 Uiso 1 d . . .
C465 C 0.3878 0.7597 0.8867 0.101 Uiso 1 d . . .
C466 C 0.3528 0.7652 0.8674 0.119 Uiso 1 d . . .
Si1A Si 0.5503(2) 0.20122(16) 0.02480(19) 0.0293(15) Uiso 1 d . . .
Si2D Si 0.4951(2) 0.53164(16) 1.24658(18) 0.0293(15) Uiso 1 d . . .
Si2C Si 0.4927(2) 0.70460(16) 1.04541(18) 0.0289(15) Uiso 1 d . . .
Si1B Si 0.4986(2) 0.05612(17) 0.24435(19) 0.0336(16) Uiso 1 d . . .
O24A O 0.6178(6) 0.2551(4) -0.0226(4) 0.040(4) Uiso 1 d . . .
O6A O 0.5788(5) 0.2238(4) 0.1288(4) 0.030(4) Uiso 1 d . . .
O9C O 0.3726(5) 0.6578(4) 1.0309(4) 0.034(4) Uiso 1 d . . .
O5D O 0.5478(6) 0.6297(4) 1.2444(4) 0.040(4) Uiso 1 d . . .
O12C O 0.6111(6) 0.7262(4) 1.0946(4) 0.039(4) Uiso 1 d . . .
O3B O 0.4597(6) 0.0473(4) 0.1398(4) 0.042(4) Uiso 1 d . . .
O305 O 0.3193(6) 0.7057(4) 1.0689(5) 0.048(5) Uiso 1 d . . .
O9A O 0.4382(5) 0.1486(4) -0.0031(4) 0.032(4) Uiso 1 d . . .
O204 O 0.6747(6) 0.0669(4) 0.2389(5) 0.053(5) Uiso 1 d . . .
O12B O 0.3905(6) 0.0291(4) 0.1811(4) 0.040(4) Uiso 1 d . . .
O4C O 0.4274(5) 0.6128(4) 1.0636(4) 0.037(4) Uiso 1 d . . .
O25B O 0.4627(5) 0.0570(4) 0.2095(4) 0.034(4) Uiso 1 d . . .
O209 O 0.4569(7) -0.0767(5) 0.2595(5) 0.053(5) Uiso 1 d . . .
O13C O 0.6039(6) 0.7146(4) 1.0247(4) 0.038(4) Uiso 1 d . . .
O25A O 0.5829(5) 0.2038(4) 0.0605(4) 0.030(4) Uiso 1 d . . .
O13B O 0.4466(6) -0.0175(4) 0.2155(4) 0.037(4) Uiso 1 d . . .
O2C O 0.4676(6) 0.6782(4) 1.1317(4) 0.038(4) Uiso 1 d . . .
O2B O 0.4848(5) 0.1287(4) 0.1924(4) 0.035(4) Uiso 1 d . . .
O5B O 0.5547(5) 0.1515(4) 0.2362(4) 0.036(4) Uiso 1 d . . .
O9D O 0.6129(5) 0.5852(4) 1.2641(4) 0.032(4) Uiso 1 d . . .
O24D O 0.4531(6) 0.4595(4) 1.2834(5) 0.043(4) Uiso 1 d . . .
O26B O 0.5373(6) 0.0842(4) 0.2402(4) 0.040(4) Uiso 1 d . . .
O15C O 0.3859(6) 0.7246(4) 1.0226(5) 0.046(4) Uiso 1 d . . .
O7D O 0.4977(6) 0.4936(4) 1.1696(4) 0.041(4) Uiso 1 d . . .
O7C O 0.5781(5) 0.6490(4) 1.0372(4) 0.035(4) Uiso 1 d . . .
O101 O 0.5687(6) 0.1570(4) 0.1614(4) 0.038(4) Uiso 1 d . . .
O3C O 0.5910(5) 0.6607(4) 1.1070(4) 0.034(4) Uiso 1 d . . .
O10C O 0.4060(6) 0.7319(4) 1.0916(4) 0.038(4) Uiso 1 d . . .
O1B O 0.5345(6) 0.0864(4) 0.1609(5) 0.045(4) Uiso 1 d . . .
O212 O 0.3602(6) 0.0101(4) 0.3175(4) 0.043(4) Uiso 1 d . . .
O2D O 0.4673(5) 0.6124(4) 1.2102(4) 0.032(4) Uiso 1 d . . .
O10B O 0.4844(5) 0.1344(4) 0.2772(4) 0.034(4) Uiso 1 d . . .
O24 O 0.4891(5) 0.6036(4) 1.2928(4) 0.036(4) Uiso 1 d . . .
O19D O 0.4831(6) 0.5650(4) 1.3507(4) 0.037(4) Uiso 1 d . . .
O5A O 0.4335(5) 0.1666(4) 0.0674(4) 0.037(4) Uiso 1 d . . .
O11C O 0.4912(5) 0.7570(4) 1.1138(4) 0.035(4) Uiso 1 d . . .
O16A O 0.6031(5) 0.2748(4) 0.0457(4) 0.032(4) Uiso 1 d . . .
O8B O 0.5969(6) 0.0350(4) 0.2077(5) 0.047(5) Uiso 1 d . . .
O301 O 0.5381(6) 0.6444(4) 1.1702(4) 0.043(4) Uiso 1 d . . .
O306 O 0.5774(6) 0.7811(5) 1.1385(5) 0.051(5) Uiso 1 d . . .
O2A O 0.5039(6) 0.1873(4) 0.1092(5) 0.043(4) Uiso 1 d . . .
O1C O 0.5067(5) 0.6312(4) 1.0978(4) 0.032(4) Uiso 1 d . . .
O19B O 0.4556(6) 0.1041(4) 0.3366(5) 0.045(4) Uiso 1 d . . .
O18B O 0.5955(6) -0.0196(4) 0.2511(4) 0.043(4) Uiso 1 d . . .
O25C O 0.5315(5) 0.7016(4) 1.0762(4) 0.031(4) Uiso 1 d . . .
O12A O 0.6548(5) 0.2326(4) 0.0875(4) 0.033(4) Uiso 1 d . . .
O22C O 0.4470(5) 0.7340(4) 0.9710(4) 0.035(4) Uiso 1 d . . .
O210 O 0.6072(6) -0.0174(5) 0.3239(5) 0.052(5) Uiso 1 d . . .
O311 O 0.3795(6) 0.7843(4) 0.9763(5) 0.048(5) Uiso 1 d . . .
O6D O 0.3853(6) 0.5781(4) 1.2005(4) 0.038(4) Uiso 1 d . . .
O23B O 0.4450(6) 0.0360(4) 0.3412(4) 0.038(4) Uiso 1 d . . .
O3D O 0.4277(5) 0.5366(4) 1.1499(4) 0.036(4) Uiso 1 d . . .
O411 O 0.5497(7) 0.5260(5) 1.3798(5) 0.054(5) Uiso 1 d . . .
O108 O 0.4500(6) 0.3016(4) 0.0729(5) 0.044(4) Uiso 1 d . . .
O109 O 0.6974(7) 0.2283(5) -0.0497(5) 0.061(5) Uiso 1 d . . .
O14C O 0.4332(5) 0.6649(4) 0.9794(4) 0.034(4) Uiso 1 d . . .
O6C O 0.5491(5) 0.7131(4) 1.1447(4) 0.034(4) Uiso 1 d . . .
O16C O 0.5558(6) 0.7738(4) 1.0660(4) 0.039(4) Uiso 1 d . . .
O103 O 0.7130(6) 0.1792(4) 0.0734(5) 0.048(5) Uiso 1 d . . .
O4A O 0.4849(5) 0.1102(4) 0.0436(4) 0.035(4) Uiso 1 d . . .
O312 O 0.5459(7) 0.8323(5) 1.0206(5) 0.054(5) Uiso 1 d . . .
O27D O 0.5200(5) 0.4935(4) 1.2409(4) 0.032(4) Uiso 1 d . . .
O8A O 0.5603(6) 0.1191(4) 0.0030(4) 0.041(4) Uiso 1 d . . .
O1A O 0.5511(6) 0.1374(4) 0.0893(5) 0.043(4) Uiso 1 d . . .
O24C O 0.5503(7) 0.7645(5) 0.9967(5) 0.056(5) Uiso 1 d . . .
O11A O 0.5294(5) 0.2623(4) 0.0835(4) 0.034(4) Uiso 1 d . . .
O1D O 0.5073(6) 0.5742(4) 1.1665(5) 0.046(5) Uiso 1 d . . .
O105 O 0.3729(6) 0.1974(4) 0.0209(5) 0.045(4) Uiso 1 d . . .
O10A O 0.4505(5) 0.2323(4) 0.0509(4) 0.034(4) Uiso 1 d . . .
O4B O 0.6081(6) 0.1037(4) 0.2017(5) 0.047(5) Uiso 1 d . . .
O20C O 0.4812(5) 0.8076(4) 1.0689(4) 0.035(4) Uiso 1 d . . .
O16B O 0.3848(6) 0.0382(4) 0.2510(4) 0.040(4) Uiso 1 d . . .
O28A O 0.5326(5) 0.2408(4) 0.0131(4) 0.028(4) Uiso 1 d . . .
O12D O 0.3771(6) 0.5077(4) 1.2006(5) 0.050(5) Uiso 1 d . . .
O201 O 0.4657(7) 0.1167(5) 0.1176(5) 0.055(5) Uiso 1 d . . .
O5C O 0.3849(5) 0.6645(4) 1.1010(4) 0.035(4) Uiso 1 d . . .
O106 O 0.6077(6) 0.2914(4) 0.1185(4) 0.040(4) Uiso 1 d . . .
O401 O 0.4266(6) 0.6100(4) 1.1393(5) 0.048(5) Uiso 1 d . . .
O22D O 0.5540(6) 0.4929(4) 1.3123(4) 0.037(4) Uiso 1 d . . .
O24B O 0.4405(6) -0.0079(4) 0.2850(5) 0.046(5) Uiso 1 d . . .
O412 O 0.3840(6) 0.4697(4) 1.3367(5) 0.049(5) Uiso 1 d . . .
O8D O 0.5808(6) 0.5203(4) 1.1917(4) 0.040(4) Uiso 1 d . . .
O3A O 0.6330(5) 0.1693(4) 0.1058(4) 0.033(4) Uiso 1 d . . .
O21B O 0.5258(6) -0.0345(4) 0.2916(5) 0.045(4) Uiso 1 d . . .
O25D O 0.4524(5) 0.5368(4) 1.2194(4) 0.033(4) Uiso 1 d . . .
O23C O 0.4696(6) 0.7960(4) 0.9984(4) 0.039(4) Uiso 1 d . . .
O28B O 0.4681(6) 0.0627(4) 0.2811(4) 0.038(4) Uiso 1 d . . .
O112 O 0.6077(6) 0.3260(5) -0.0087(5) 0.052(5) Uiso 1 d . . .
O404 O 0.6657(6) 0.5494(5) 1.2147(5) 0.053(5) Uiso 1 d . . .
O304 O 0.4021(6) 0.5987(5) 0.9941(5) 0.050(5) Uiso 1 d . . .
O27A O 0.5828(5) 0.1875(4) -0.0089(4) 0.034(4) Uiso 1 d . . .
O11B O 0.4093(6) 0.1067(4) 0.2434(4) 0.042(4) Uiso 1 d . . .
O6B O 0.4057(6) 0.0965(4) 0.1734(4) 0.037(4) Uiso 1 d . . .
O26C O 0.4496(6) 0.6783(4) 1.0542(4) 0.037(4) Uiso 1 d . . .
O206 O 0.3290(6) 0.0791(4) 0.2085(5) 0.047(5) Uiso 1 d . . .
O26D O 0.5350(5) 0.5627(4) 1.2404(4) 0.032(4) Uiso 1 d . . .
O13A O 0.6636(6) 0.2124(4) 0.0196(5) 0.044(4) Uiso 1 d . . .
O20A O 0.5310(6) 0.3059(4) 0.0299(4) 0.038(4) Uiso 1 d . . .
O405 O 0.5759(6) 0.6347(4) 1.3132(5) 0.046(5) Uiso 1 d . . .
O4D O 0.5926(6) 0.5888(4) 1.1945(5) 0.044(4) Uiso 1 d . . .
O17C O 0.5888(6) 0.6740(4) 0.9720(4) 0.043(4) Uiso 1 d . . .
O407 O 0.5811(6) 0.4610(5) 1.1496(5) 0.049(5) Uiso 1 d . . .
O28D O 0.4782(5) 0.5332(4) 1.2886(4) 0.031(4) Uiso 1 d . . .
O7A O 0.6363(6) 0.1486(4) 0.0372(4) 0.045(4) Uiso 1 d . . .
O14B O 0.6028(6) 0.0418(5) 0.2793(5) 0.050(5) Uiso 1 d . . .
O203 O 0.4349(6) -0.0216(5) 0.1399(5) 0.056(5) Uiso 1 d . . .
O7B O 0.5181(5) 0.0052(4) 0.1746(4) 0.034(4) Uiso 1 d . . .
O22A O 0.5237(6) 0.2194(4) -0.0604(4) 0.036(4) Uiso 1 d . . .
O26A O 0.5084(5) 0.1765(4) 0.0309(4) 0.036(4) Uiso 1 d . . .
O11D O 0.4057(6) 0.5762(4) 1.2704(4) 0.040(4) Uiso 1 d . . .
O406 O 0.3219(7) 0.5499(5) 1.2440(6) 0.064(5) Uiso 1 d . . .
O19C O 0.4045(6) 0.7860(4) 1.0485(5) 0.048(5) Uiso 1 d . . .
O211 O 0.5117(6) 0.0670(4) 0.3825(5) 0.050(5) Uiso 1 d . . .
O14A O 0.5096(6) 0.1521(4) -0.0442(4) 0.038(4) Uiso 1 d . . .
O15B O 0.5397(6) 0.0961(4) 0.3175(4) 0.036(4) Uiso 1 d . . .
O104 O 0.4791(6) 0.0876(5) -0.0249(5) 0.051(5) Uiso 1 d . . .
O308 O 0.4150(7) 0.7998(5) 1.1219(5) 0.060(5) Uiso 1 d . . .
O21A O 0.6131(6) 0.2046(4) -0.0709(5) 0.046(5) Uiso 1 d . . .
O8C O 0.4917(5) 0.6247(4) 1.0138(4) 0.032(4) Uiso 1 d . . .
O16D O 0.3913(6) 0.5073(4) 1.2711(5) 0.046(5) Uiso 1 d . . .
O309 O 0.6216(7) 0.7380(5) 0.9557(5) 0.054(5) Uiso 1 d . . .
O27B O 0.5213(5) 0.0175(4) 0.2479(4) 0.034(4) Uiso 1 d . . .
O303 O 0.6659(6) 0.6748(4) 1.0636(5) 0.053(5) Uiso 1 d . . .
O13D O 0.4404(6) 0.4611(4) 1.2136(4) 0.039(4) Uiso 1 d . . .
O15D O 0.5579(6) 0.5636(4) 1.3156(4) 0.039(4) Uiso 1 d . . .
O205 O 0.5635(6) 0.1649(5) 0.3073(5) 0.051(5) Uiso 1 d . . .
O23A O 0.5374(6) 0.2849(4) -0.0381(4) 0.042(4) Uiso 1 d . . .
O20B O 0.3852(6) 0.0780(4) 0.3064(5) 0.049(5) Uiso 1 d . . .
O409 O 0.4611(7) 0.3975(5) 1.2466(5) 0.054(5) Uiso 1 d . . .
O110 O 0.5492(7) 0.1704(5) -0.1111(5) 0.062(5) Uiso 1 d . . .
O111 O 0.4524(6) 0.2662(5) -0.0705(5) 0.051(5) Uiso 1 d . . .
O14D O 0.6092(6) 0.5173(4) 1.2596(4) 0.043(4) Uiso 1 d . . .
O408 O 0.4112(6) 0.6133(5) 1.3346(5) 0.054(5) Uiso 1 d . . .
O20D O 0.4036(6) 0.5405(4) 1.3292(5) 0.043(4) Uiso 1 d . . .
O21D O 0.5384(6) 0.4349(4) 1.2719(5) 0.047(5) Uiso 1 d . . .
O17A O 0.6621(6) 0.1647(4) -0.0285(5) 0.050(5) Uiso 1 d . . .
O107 O 0.6494(7) 0.0945(5) -0.0120(5) 0.063(6) Uiso 1 d . . .
O410 O 0.6280(6) 0.4515(4) 1.2925(4) 0.039(4) Uiso 1 d . . .
O23D O 0.4727(6) 0.4974(4) 1.3462(5) 0.048(5) Uiso 1 d . . .
O22B O 0.5333(6) 0.0270(4) 0.3239(4) 0.036(4) Uiso 1 d . . .
O310 O 0.4537(7) 0.6914(5) 0.9088(5) 0.061(5) Uiso 1 d . . .
O18A O 0.5939(6) 0.1366(4) -0.0567(4) 0.041(4) Uiso 1 d . . .
O307 O 0.5732(7) 0.6014(5) 0.9815(5) 0.061(5) Uiso 1 d . . .
O15A O 0.4491(6) 0.2165(4) -0.0179(4) 0.036(4) Uiso 1 d . . .
O18C O 0.5126(6) 0.6515(4) 0.9507(5) 0.047(5) Uiso 1 d . . .
O208 O 0.3923(7) 0.1498(5) 0.3041(5) 0.057(5) Uiso 1 d . . .
O27C O 0.5133(6) 0.6946(4) 1.0058(4) 0.037(4) Uiso 1 d . . .
O21C O 0.5306(6) 0.7193(5) 0.9423(5) 0.049(5) Uiso 1 d . . .
O9B O 0.6083(6) 0.1098(4) 0.2723(4) 0.044(4) Uiso 1 d . . .
O17D O 0.5200(5) 0.4360(4) 1.2029(4) 0.037(4) Uiso 1 d . . .
O28C O 0.4746(5) 0.7447(4) 1.0419(4) 0.033(4) Uiso 1 d . . .
O207 O 0.6007(8) -0.0317(5) 0.1770(6) 0.072(6) Uiso 1 d . . .
O17B O 0.5256(7) -0.0451(5) 0.2209(5) 0.055(5) Uiso 1 d . . .
O18D O 0.5952(7) 0.4617(5) 1.2238(5) 0.054(5) Uiso 1 d . . .
O403 O 0.4131(7) 0.4678(5) 1.1425(5) 0.060(5) Uiso 1 d . . .
O19A O 0.4589(6) 0.2797(4) 0.0016(5) 0.045(4) Uiso 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
W8C 0.0507(7) 0.0277(5) 0.0393(6) -0.0041(5) 0.0019(5) 0.0038(5)
W4D 0.0326(6) 0.0313(5) 0.0340(6) 0.0011(4) -0.0011(5) 0.0013(4)
W5B 0.0512(7) 0.0345(6) 0.0365(6) -0.0006(5) -0.0013(5) -0.0150(5)
W8A 0.0360(6) 0.0299(5) 0.0429(6) -0.0056(5) -0.0053(5) 0.0060(5)
W11D 0.0493(7) 0.0329(6) 0.0299(6) 0.0004(4) -0.0006(5) -0.0023(5)
W12A 0.0435(7) 0.0320(5) 0.0395(6) 0.0082(5) -0.0086(5) -0.0074(5)
W5A 0.0281(6) 0.0358(6) 0.0382(6) 0.0015(5) -0.0031(5) -0.0012(4)
W12C 0.0533(8) 0.0304(6) 0.0388(6) 0.0043(5) -0.0020(5) -0.0025(5)
W6B 0.0343(6) 0.0311(6) 0.0467(6) 0.0070(5) -0.0015(5) -0.0042(5)
W3C 0.0349(6) 0.0362(6) 0.0474(6) -0.0012(5) -0.0045(5) -0.0023(5)
W5D 0.0434(7) 0.0252(5) 0.0313(5) -0.0017(4) -0.0038(5) -0.0011(4)
W4C 0.0412(7) 0.0335(6) 0.0383(6) -0.0075(5) -0.0099(5) 0.0006(5)
W6C 0.0509(7) 0.0280(5) 0.0326(6) -0.0008(4) -0.0088(5) -0.0066(5)
W10D 0.0421(7) 0.0255(5) 0.0397(6) 0.0011(4) -0.0044(5) 0.0037(5)
W3D 0.0499(7) 0.0329(6) 0.0429(6) -0.0003(5) -0.0125(5) -0.0080(5)
W9D 0.0483(7) 0.0257(5) 0.0471(7) 0.0000(5) -0.0050(6) -0.0036(5)
W7D 0.0482(7) 0.0309(6) 0.0373(6) -0.0082(5) 0.0001(5) 0.0034(5)
W10A 0.0425(7) 0.0469(6) 0.0311(6) -0.0058(5) 0.0030(5) -0.0052(5)
W9C 0.0474(7) 0.0505(7) 0.0377(6) -0.0037(5) 0.0058(5) -0.0041(6)
W4A 0.0450(7) 0.0303(5) 0.0394(6) -0.0046(5) -0.0010(5) -0.0047(5)
W5C 0.0364(6) 0.0335(5) 0.0342(6) 0.0007(4) -0.0047(5) 0.0045(5)
W3B 0.0511(8) 0.0295(6) 0.0499(7) -0.0052(5) -0.0087(6) -0.0050(5)
W3A 0.0297(6) 0.0424(6) 0.0368(6) 0.0047(5) 0.0008(5) 0.0040(5)
W6A 0.0330(6) 0.0298(5) 0.0331(5) -0.0001(4) -0.0038(5) -0.0031(4)
W12B 0.0388(7) 0.0354(6) 0.0460(6) 0.0104(5) 0.0009(5) -0.0065(5)
W12D 0.0449(7) 0.0426(6) 0.0426(6) 0.0052(5) 0.0072(6) -0.0063(5)
W11A 0.0409(7) 0.0314(6) 0.0380(6) 0.0062(4) -0.0093(5) -0.0022(5)
W8B 0.0468(7) 0.0311(6) 0.0438(6) 0.0001(5) 0.0065(5) -0.0001(5)
W10B 0.0429(7) 0.0379(6) 0.0582(7) 0.0081(5) -0.0085(6) -0.0002(5)
W6D 0.0325(6) 0.0417(6) 0.0569(7) 0.0055(5) -0.0023(5) -0.0027(5)
W11C 0.0483(7) 0.0384(6) 0.0393(6) 0.0083(5) -0.0060(5) 0.0061(5)
W9B 0.0503(8) 0.0264(6) 0.0619(8) 0.0033(5) -0.0088(6) -0.0034(5)
W7A 0.0434(7) 0.0406(6) 0.0507(7) -0.0097(5) 0.0032(6) 0.0110(5)
W7C 0.0429(7) 0.0412(6) 0.0485(7) -0.0175(5) 0.0002(6) 0.0056(5)
W8D 0.0469(7) 0.0400(6) 0.0446(7) -0.0057(5) 0.0080(6) 0.0054(5)
W11B 0.0478(7) 0.0382(6) 0.0399(6) 0.0047(5) -0.0008(5) -0.0086(5)
W4B 0.0335(6) 0.0482(7) 0.0495(7) 0.0056(5) -0.0030(5) -0.0055(5)
W9A 0.0350(7) 0.0556(7) 0.0334(6) -0.0004(5) 0.0050(5) -0.0052(5)
W10C 0.0532(8) 0.0531(7) 0.0303(6) -0.0046(5) -0.0045(5) -0.0014(6)
W7B 0.0474(8) 0.0420(7) 0.0615(8) -0.0083(6) -0.0005(6) 0.0069(5)
Ti2B 0.046(3) 0.036(3) 0.031(2) 0.005(2) 0.001(2) -0.012(2)
Ti2C 0.040(3) 0.030(2) 0.039(3) 0.003(2) -0.012(2) -0.001(2)
Ti1D 0.043(3) 0.034(3) 0.045(3) 0.009(2) -0.013(2) -0.006(2)
Ti1C 0.039(3) 0.030(2) 0.035(3) 0.0037(19) -0.012(2) -0.001(2)
Ti2D 0.041(3) 0.026(2) 0.035(3) 0.0050(19) -0.005(2) -0.006(2)
Ti1B 0.042(3) 0.041(3) 0.040(3) 0.007(2) -0.001(2) -0.009(2)
Ti1A 0.035(3) 0.038(3) 0.037(3) 0.005(2) 0.002(2) -0.004(2)
Ti2A 0.039(3) 0.036(3) 0.033(2) 0.003(2) -0.003(2) -0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N901 C902 C901 172(4) . . ?
C255 N2B C256 102.8 . . ?
C255 N2B C275 97.1 . . ?
C256 N2B C275 94.1 . . ?
C255 N2B C263 57.3 . . ?
C256 N2B C263 99.8 . . ?
C275 N2B C263 153 . . ?
C263 N20B C271 115.9 . . ?
C263 N20B C259 99.9 . . ?
C271 N20B C259 132.3 . . ?
C263 N20B C284 96.5 . . ?
C271 N20B C284 118.5 . . ?
C259 N20B C284 85.2 . . ?
C263 N20B C255 53.8 . . ?
C271 N20B C255 77.8 . . ?
C259 N20B C255 102.3 . . ?
C284 N20B C255 150 . . ?
C263 N20B C283 112.2 . . ?
C271 N20B C283 94.3 . . ?
C259 N20B C283 100.4 . . ?
C284 N20B C283 24.4 . . ?
C255 N20B C283 155.2 . . ?
C252 C251 C271 42.6 . . ?
C252 C271 N20B 122 . . ?
C252 C271 C251 29.6 . . ?
N20B C271 C251 94.1 . . ?
C252 C271 C263 124.3 . . ?
N20B C271 C263 30.4 . . ?
C251 C271 C263 105.9 . . ?
C252 C271 C255 84.1 . . ?
N20B C271 C255 65.6 . . ?
C251 C271 C255 79 . . ?
C263 C271 C255 44.4 . . ?
C251 C252 C271 107.8 . . ?
C251 C252 C272 125 . . ?
C271 C252 C272 126 . . ?
C251 C252 C253 119 . . ?
C271 C252 C253 112.5 . . ?
C272 C252 C253 32.8 . . ?
C253 C272 C252 81.8 . . ?
C272 C253 C252 65.5 . . ?
N2B C275 C257 85.2 . . ?
N2B C255 C276 111.1 . . ?
N2B C255 C263 80.5 . . ?
C276 C255 C263 147.9 . . ?
N2B C255 N20B 109.3 . . ?
C276 C255 N20B 138.9 . . ?
C263 C255 N20B 36.8 . . ?
N2B C255 C256 40.6 . . ?
C276 C255 C256 85.8 . . ?
C263 C255 C256 85 . . ?
N20B C255 C256 121.8 . . ?
N2B C255 C271 145.8 . . ?
C276 C255 C271 102.5 . . ?
C263 C255 C271 67.2 . . ?
N20B C255 C271 36.7 . . ?
C256 C255 C271 140.1 . . ?
N2B C256 C257 101.4 . . ?
N2B C256 C255 36.7 . . ?
C257 C256 C255 122.3 . . ?
C256 C257 C275 66.4 . . ?
N20B C259 C260 126.3 . . ?
N20B C259 C263 32 . . ?
C260 C259 C263 153.6 . . ?
C259 C260 C261 112 . . ?
C284 C283 N20B 67 . . ?
N20B C263 C255 89.4 . . ?
N20B C263 C264 112.5 . . ?
C255 C263 C264 125.2 . . ?
N20B C263 N2B 121.3 . . ?
C255 C263 N2B 42.2 . . ?
C264 C263 N2B 122 . . ?
N20B C263 C271 33.7 . . ?
C255 C263 C271 68.4 . . ?
C264 C263 C271 102.7 . . ?
N2B C263 C271 109.9 . . ?
N20B C263 C259 48.2 . . ?
C255 C263 C259 95.6 . . ?
C264 C263 C259 136.9 . . ?
N2B C263 C259 96.7 . . ?
C271 C263 C259 78.1 . . ?
C283 C284 N20B 88.6 . . ?
C265 C264 C263 144.4 . . ?
C351 N3B N30B 125.8 . . ?
C351 N3B C355 73 . . ?
N30B N3B C355 129 . . ?
C351 N3B C363 163 . . ?
N30B N3B C363 37.5 . . ?
C355 N3B C363 118.4 . . ?
C351 N3B C359 68.6 . . ?
N30B N3B C359 117.3 . . ?
C355 N3B C359 113.7 . . ?
C363 N3B C359 113.5 . . ?
C363 N30B N3B 91.3 . . ?
C363 N30B C364 37.6 . . ?
N3B N30B C364 128.5 . . ?
C363 N30B C383 51.9 . . ?
N3B N30B C383 124.4 . . ?
C364 N30B C383 39 . . ?
N3B C351 C352 136.5 . . ?
N3B C351 C355 72.3 . . ?
C352 C351 C355 120 . . ?
N3B C351 C359 80 . . ?
C352 C351 C359 117.6 . . ?
C355 C351 C359 118.9 . . ?
N3B C351 C372 165.6 . . ?
C352 C351 C372 49.7 . . ?
C355 C351 C372 93.3 . . ?
C359 C351 C372 109.2 . . ?
C373 C372 C352 63.8 . . ?
C373 C372 C374 29.9 . . ?
C352 C372 C374 93.7 . . ?
C373 C372 C351 96.3 . . ?
C352 C372 C351 36.1 . . ?
C374 C372 C351 124.7 . . ?
C351 C352 C373 134.7 . . ?
C351 C352 C372 94.2 . . ?
C373 C352 C372 48.2 . . ?
C374 C353 C354 103.7 . . ?
C374 C353 C373 33.4 . . ?
C354 C353 C373 126.8 . . ?
C374 C373 C372 104.8 . . ?
C374 C373 C352 172.8 . . ?
C372 C373 C352 68 . . ?
C374 C373 C353 58.2 . . ?
C372 C373 C353 131.3 . . ?
C352 C373 C353 126.5 . . ?
C373 C374 C353 88.4 . . ?
C373 C374 C372 45.3 . . ?
C353 C374 C372 115.7 . . ?
C375 C355 N3B 94.5 . . ?
C375 C355 C351 107.6 . . ?
N3B C355 C351 34.7 . . ?
C355 C375 C356 95.2 . . ?
C357 C356 C375 116.9 . . ?
N30B C363 C364 105.3 . . ?
N30B C363 C383 91.9 . . ?
C364 C363 C383 54.1 . . ?
N30B C363 N3B 51.2 . . ?
C364 C363 N3B 155.6 . . ?
C383 C363 N3B 124.5 . . ?
C364 C383 C384 79.3 . . ?
C364 C383 C363 47.9 . . ?
C384 C383 C363 123.1 . . ?
C364 C383 C365 42.2 . . ?
C384 C383 C365 39.1 . . ?
C363 C383 C365 89.8 . . ?
C364 C383 N30B 66 . . ?
C384 C383 N30B 110.8 . . ?
C363 C383 N30B 36.3 . . ?
C365 C383 N30B 96.9 . . ?
C365 C364 C363 161.4 . . ?
C365 C364 C383 85.3 . . ?
C363 C364 C383 78 . . ?
C365 C364 C384 35.9 . . ?
C363 C364 C384 125.6 . . ?
C383 C364 C384 52.1 . . ?
C365 C364 N30B 130 . . ?
C363 C364 N30B 37.1 . . ?
C383 C364 N30B 75 . . ?
C384 C364 N30B 102 . . ?
C365 C384 C383 84.4 . . ?
C365 C384 C364 38.5 . . ?
C383 C384 C364 48.6 . . ?
C384 C365 C364 105.7 . . ?
C384 C365 C383 56.4 . . ?
C364 C365 C383 52.5 . . ?
C351 C359 N3B 31.4 . . ?
O308 W8C O11C 102.5(8) . . ?
O308 W8C O10C 105.5(8) . . ?
O11C W8C O10C 95.5(7) . . ?
O308 W8C O19C 102.2(8) . . ?
O11C W8C O19C 153.4(7) . . ?
O10C W8C O19C 87.4(7) . . ?
O308 W8C O20C 99.6(8) . . ?
O11C W8C O20C 85.4(7) . . ?
O10C W8C O20C 154.0(7) . . ?
O19C W8C O20C 80.8(7) . . ?
O308 W8C O28C 173.1(8) . . ?
O11C W8C O28C 80.5(6) . . ?
O10C W8C O28C 80.2(6) . . ?
O19C W8C O28C 73.9(6) . . ?
O20C W8C O28C 74.3(6) . . ?
O404 W4D O14D 97.7(8) . . ?
O404 W4D O9D 102.2(8) . . ?
O14D W4D O9D 89.9(7) . . ?
O404 W4D O4D 98.4(8) . . ?
O14D W4D O4D 163.6(8) . . ?
O9D W4D O4D 90.1(7) . . ?
O404 W4D O8D 100.6(8) . . ?
O14D W4D O8D 88.0(7) . . ?
O9D W4D O8D 157.2(7) . . ?
O4D W4D O8D 85.7(7) . . ?
O404 W4D O26D 174.5(7) . . ?
O14D W4D O26D 87.6(7) . . ?
O9D W4D O26D 76.5(6) . . ?
O4D W4D O26D 76.4(6) . . ?
O8D W4D O26D 80.8(6) . . ?
O404 W4D Ti2D 129.0(6) . . ?
O14D W4D Ti2D 133.3(5) . . ?
O9D W4D Ti2D 79.5(5) . . ?
O4D W4D Ti2D 31.0(5) . . ?
O8D W4D Ti2D 85.5(5) . . ?
O26D W4D Ti2D 45.7(4) . . ?
O205 W5B O9B 103.8(8) . . ?
O205 W5B O5B 99.0(8) . . ?
O9B W5B O5B 87.3(7) . . ?
O205 W5B O15B 100.9(8) . . ?
O9B W5B O15B 89.6(7) . . ?
O5B W5B O15B 160.0(7) . . ?
O205 W5B O10B 102.0(8) . . ?
O9B W5B O10B 154.1(7) . . ?
O5B W5B O10B 87.0(7) . . ?
O15B W5B O10B 87.2(7) . . ?
O205 W5B O26B 173.4(7) . . ?
O9B W5B O26B 73.3(6) . . ?
O5B W5B O26B 75.1(6) . . ?
O15B W5B O26B 85.1(6) . . ?
O10B W5B O26B 80.8(6) . . ?
O205 W5B Ti2B 127.4(6) . . ?
O9B W5B Ti2B 76.6(5) . . ?
O5B W5B Ti2B 28.9(5) . . ?
O15B W5B Ti2B 131.6(5) . . ?
O10B W5B Ti2B 86.5(5) . . ?
O26B W5B Ti2B 46.5(4) . . ?
O108 W8A O11A 103.2(7) . . ?
O108 W8A O10A 101.7(7) . . ?
O11A W8A O10A 97.8(7) . . ?
O108 W8A O20A 103.0(7) . . ?
O11A W8A O20A 85.9(7) . . ?
O10A W8A O20A 153.4(7) . . ?
O108 W8A O19A 100.2(8) . . ?
O11A W8A O19A 155.4(7) . . ?
O10A W8A O19A 84.7(7) . . ?
O20A W8A O19A 81.5(7) . . ?
O108 W8A O28A 174.4(7) . . ?
O11A W8A O28A 80.8(6) . . ?
O10A W8A O28A 81.6(6) . . ?
O20A W8A O28A 73.0(6) . . ?
O19A W8A O28A 75.3(6) . . ?
O411 W11D O19D 100.0(8) . . ?
O411 W11D O23D 103.4(9) . . ?
O19D W11D O23D 88.8(7) . . ?
O411 W11D O15D 103.0(8) . . ?
O19D W11D O15D 84.6(7) . . ?
O23D W11D O15D 153.5(7) . . ?
O411 W11D O22D 102.2(8) . . ?
O19D W11D O22D 157.8(7) . . ?
O23D W11D O22D 88.0(7) . . ?
O15D W11D O22D 88.5(7) . . ?
O411 W11D O28D 174.8(8) . . ?
O19D W11D O28D 76.5(6) . . ?
O23D W11D O28D 73.0(6) . . ?
O15D W11D O28D 80.5(6) . . ?
O22D W11D O28D 81.6(6) . . ?
O112 W12A O16A 105.4(8) . . ?
O112 W12A O20A 102.0(8) . . ?
O16A W12A O20A 84.6(7) . . ?
O112 W12A O23A 100.5(8) . . ?
O16A W12A O23A 154.1(7) . . ?
O20A W12A O23A 89.6(7) . . ?
O112 W12A O24A 98.7(8) . . ?
O16A W12A O24A 90.2(7) . . ?
O20A W12A O24A 159.3(7) . . ?
O23A W12A O24A 86.4(7) . . ?
O112 W12A O28A 173.1(7) . . ?
O16A W12A O28A 80.9(6) . . ?
O20A W12A O28A 75.5(6) . . ?
O23A W12A O28A 73.2(6) . . ?
O24A W12A O28A 83.8(6) . . ?
O105 W5A O5A 101.5(8) . . ?
O105 W5A O10A 103.5(7) . . ?
O5A W5A O10A 89.6(7) . . ?
O105 W5A O15A 96.7(7) . . ?
O5A W5A O15A 161.8(7) . . ?
O10A W5A O15A 85.6(6) . . ?
O105 W5A O9A 99.5(7) . . ?
O5A W5A O9A 91.4(7) . . ?
O10A W5A O9A 156.3(6) . . ?
O15A W5A O9A 86.1(6) . . ?
O105 W5A O26A 173.5(7) . . ?
O5A W5A O26A 76.0(6) . . ?
O10A W5A O26A 82.6(6) . . ?
O15A W5A O26A 85.9(6) . . ?
O9A W5A O26A 74.7(6) . . ?
O105 W5A Ti2A 128.8(6) . . ?
O5A W5A Ti2A 28.6(5) . . ?
O10A W5A Ti2A 90.4(5) . . ?
O15A W5A Ti2A 133.7(5) . . ?
O9A W5A Ti2A 79.4(4) . . ?
O26A W5A Ti2A 47.9(4) . . ?
O312 W12C O16C 105.7(8) . . ?
O312 W12C O20C 100.4(8) . . ?
O16C W12C O20C 85.7(7) . . ?
O312 W12C O24C 98.9(8) . . ?
O16C W12C O24C 88.7(8) . . ?
O20C W12C O24C 160.6(7) . . ?
O312 W12C O23C 98.6(8) . . ?
O16C W12C O23C 155.7(7) . . ?
O20C W12C O23C 89.9(7) . . ?
O24C W12C O23C 87.6(8) . . ?
O312 W12C O28C 171.1(7) . . ?
O16C W12C O28C 82.3(6) . . ?
O20C W12C O28C 76.0(6) . . ?
O24C W12C O28C 84.9(7) . . ?
O23C W12C O28C 73.5(6) . . ?
O206 W6B O6B 96.4(8) . . ?
O206 W6B O16B 100.5(8) . . ?
O6B W6B O16B 162.7(7) . . ?
O206 W6B O11B 103.7(7) . . ?
O6B W6B O11B 87.6(7) . . ?
O16B W6B O11B 91.6(7) . . ?
O206 W6B O12B 100.1(7) . . ?
O6B W6B O12B 87.1(7) . . ?
O16B W6B O12B 86.7(7) . . ?
O11B W6B O12B 156.0(7) . . ?
O206 W6B O25B 172.0(7) . . ?
O6B W6B O25B 77.4(6) . . ?
O16B W6B O25B 85.4(6) . . ?
O11B W6B O25B 81.3(6) . . ?
O12B W6B O25B 74.7(6) . . ?
O206 W6B Ti1B 126.9(6) . . ?
O6B W6B Ti1B 31.0(5) . . ?
O16B W6B Ti1B 131.7(5) . . ?
O11B W6B Ti1B 86.2(5) . . ?
O12B W6B Ti1B 77.3(5) . . ?
O25B W6B Ti1B 46.6(4) . . ?
O303 W3C O3C 101.8(8) . . ?
O303 W3C O12C 100.9(8) . . ?
O3C W3C O12C 90.4(7) . . ?
O303 W3C O13C 97.2(8) . . ?
O3C W3C O13C 160.9(7) . . ?
O12C W3C O13C 87.8(7) . . ?
O303 W3C O7C 102.4(7) . . ?
O3C W3C O7C 88.8(7) . . ?
O12C W3C O7C 156.4(7) . . ?
O13C W3C O7C 85.3(6) . . ?
O303 W3C O25C 175.8(7) . . ?
O3C W3C O25C 76.5(6) . . ?
O12C W3C O25C 75.3(6) . . ?
O13C W3C O25C 84.6(6) . . ?
O7C W3C O25C 81.6(6) . . ?
O303 W3C Ti1C 130.9(6) . . ?
O3C W3C Ti1C 29.8(5) . . ?
O12C W3C Ti1C 79.4(5) . . ?
O13C W3C Ti1C 131.6(5) . . ?
O7C W3C Ti1C 88.4(5) . . ?
O25C W3C Ti1C 47.0(4) . . ?
O405 W5D O5D 98.1(8) . . ?
O405 W5D O15D 102.1(8) . . ?
O5D W5D O15D 159.6(7) . . ?
O405 W5D O24 104.5(7) . . ?
O5D W5D O24 88.8(7) . . ?
O15D W5D O24 88.1(7) . . ?
O405 W5D O9D 101.6(7) . . ?
O5D W5D O9D 87.4(7) . . ?
O15D W5D O9D 86.5(7) . . ?
O24 W5D O9D 153.9(6) . . ?
O405 W5D O26D 170.8(7) . . ?
O5D W5D O26D 74.8(6) . . ?
O15D W5D O26D 84.8(6) . . ?
O24 W5D O26D 81.6(6) . . ?
O9D W5D O26D 72.5(6) . . ?
O405 W5D Ti2D 127.4(6) . . ?
O5D W5D Ti2D 29.8(5) . . ?
O15D W5D Ti2D 129.9(5) . . ?
O24 W5D Ti2D 86.5(5) . . ?
O9D W5D Ti2D 77.5(4) . . ?
O26D W5D Ti2D 45.1(4) . . ?
O304 W4C O4C 99.9(8) . . ?
O304 W4C O9C 100.9(8) . . ?
O4C W4C O9C 91.0(7) . . ?
O304 W4C O14C 97.0(7) . . ?
O4C W4C O14C 162.9(7) . . ?
O9C W4C O14C 87.4(7) . . ?
O304 W4C O8C 102.1(7) . . ?
O4C W4C O8C 89.4(7) . . ?
O9C W4C O8C 156.6(6) . . ?
O14C W4C O8C 85.4(6) . . ?
O304 W4C O26C 174.3(7) . . ?
O4C W4C O26C 77.7(6) . . ?
O9C W4C O26C 74.0(6) . . ?
O14C W4C O26C 85.5(6) . . ?
O8C W4C O26C 83.2(6) . . ?
O304 W4C Ti2C 128.9(6) . . ?
O4C W4C Ti2C 29.8(5) . . ?
O9C W4C Ti2C 79.4(5) . . ?
O14C W4C Ti2C 133.7(5) . . ?
O8C W4C Ti2C 89.5(4) . . ?
O26C W4C Ti2C 48.2(4) . . ?
O306 W6C O6C 102.0(8) . . ?
O306 W6C O12C 103.9(8) . . ?
O6C W6C O12C 89.1(7) . . ?
O306 W6C O11C 102.6(8) . . ?
O6C W6C O11C 88.9(7) . . ?
O12C W6C O11C 153.2(7) . . ?
O306 W6C O16C 99.2(8) . . ?
O6C W6C O16C 158.8(7) . . ?
O12C W6C O16C 86.0(7) . . ?
O11C W6C O16C 86.3(7) . . ?
O306 W6C O25C 176.6(7) . . ?
O6C W6C O25C 76.3(6) . . ?
O12C W6C O25C 73.2(6) . . ?
O11C W6C O25C 80.4(6) . . ?
O16C W6C O25C 82.6(6) . . ?
O306 W6C Ti1C 131.5(6) . . ?
O6C W6C Ti1C 29.9(5) . . ?
O12C W6C Ti1C 78.1(5) . . ?
O11C W6C Ti1C 87.0(5) . . ?
O16C W6C Ti1C 129.0(5) . . ?
O25C W6C Ti1C 46.5(4) . . ?
O410 W10D O22D 103.6(7) . . ?
O410 W10D O21D 100.8(8) . . ?
O22D W10D O21D 93.6(7) . . ?
O410 W10D O18D 97.9(8) . . ?
O22D W10D O18D 158.0(7) . . ?
O21D W10D O18D 86.5(8) . . ?
O410 W10D O14D 101.7(7) . . ?
O22D W10D O14D 90.4(7) . . ?
O21D W10D O14D 155.5(7) . . ?
O18D W10D O14D 80.9(7) . . ?
O410 W10D O27D 170.3(6) . . ?
O22D W10D O27D 85.2(6) . . ?
O21D W10D O27D 74.4(6) . . ?
O18D W10D O27D 73.6(7) . . ?
O14D W10D O27D 81.9(6) . . ?
O403 W3D O12D 104.1(9) . . ?
O403 W3D O3D 95.7(8) . . ?
O12D W3D O3D 89.1(7) . . ?
O403 W3D O13D 99.2(8) . . ?
O12D W3D O13D 87.1(7) . . ?
O3D W3D O13D 165.1(7) . . ?
O403 W3D O7D 100.8(8) . . ?
O12D W3D O7D 155.0(7) . . ?
O3D W3D O7D 90.5(7) . . ?
O13D W3D O7D 86.9(7) . . ?
O403 W3D O25D 173.6(7) . . ?
O12D W3D O25D 73.8(7) . . ?
O3D W3D O25D 78.3(6) . . ?
O13D W3D O25D 86.8(6) . . ?
O7D W3D O25D 81.7(6) . . ?
O403 W3D Ti1D 127.3(6) . . ?
O12D W3D Ti1D 78.7(5) . . ?
O3D W3D Ti1D 31.8(5) . . ?
O13D W3D Ti1D 133.3(5) . . ?
O7D W3D Ti1D 87.9(5) . . ?
O25D W3D Ti1D 46.5(4) . . ?
O409 W9D O24D 102.3(8) . . ?
O409 W9D O13D 101.3(8) . . ?
O24D W9D O13D 90.7(7) . . ?
O409 W9D O21D 101.4(8) . . ?
O24D W9D O21D 92.2(8) . . ?
O13D W9D O21D 155.9(7) . . ?
O409 W9D O17D 98.5(8) . . ?
O24D W9D O17D 159.0(7) . . ?
O13D W9D O17D 83.0(7) . . ?
O21D W9D O17D 85.8(7) . . ?
O409 W9D O27D 171.8(7) . . ?
O24D W9D O27D 84.7(6) . . ?
O13D W9D O27D 82.6(6) . . ?
O21D W9D O27D 73.8(6) . . ?
O17D W9D O27D 74.7(6) . . ?
O407 W7D O8D 100.2(8) . . ?
O407 W7D O18D 101.7(8) . . ?
O8D W7D O18D 87.7(8) . . ?
O407 W7D O7D 101.5(8) . . ?
O8D W7D O7D 93.7(7) . . ?
O18D W7D O7D 156.1(8) . . ?
O407 W7D O17D 101.3(7) . . ?
O8D W7D O17D 158.1(7) . . ?
O18D W7D O17D 83.7(7) . . ?
O7D W7D O17D 86.4(7) . . ?
O407 W7D O27D 176.8(7) . . ?
O8D W7D O27D 82.0(6) . . ?
O18D W7D O27D 75.9(7) . . ?
O7D W7D O27D 80.7(6) . . ?
O17D W7D O27D 76.4(6) . . ?
O110 W10A O22A 101.3(8) . . ?
O110 W10A O14A 104.3(8) . . ?
O22A W10A O14A 90.1(7) . . ?
O110 W10A O21A 97.7(9) . . ?
O22A W10A O21A 89.5(7) . . ?
O14A W10A O21A 157.7(7) . . ?
O110 W10A O18A 97.7(8) . . ?
O22A W10A O18A 160.9(7) . . ?
O14A W10A O18A 83.7(7) . . ?
O21A W10A O18A 89.4(7) . . ?
O110 W10A O27A 169.5(8) . . ?
O22A W10A O27A 84.6(6) . . ?
O14A W10A O27A 84.3(6) . . ?
O21A W10A O27A 73.5(6) . . ?
O18A W10A O27A 76.8(6) . . ?
O309 W9C O13C 103.4(8) . . ?
O309 W9C O17C 98.0(8) . . ?
O13C W9C O17C 85.7(7) . . ?
O309 W9C O24C 100.4(8) . . ?
O13C W9C O24C 90.7(8) . . ?
O17C W9C O24C 161.5(8) . . ?
O309 W9C O21C 99.2(8) . . ?
O13C W9C O21C 157.1(7) . . ?
O17C W9C O21C 87.2(7) . . ?
O24C W9C O21C 89.2(8) . . ?
O309 W9C O27C 170.6(7) . . ?
O13C W9C O27C 83.8(6) . . ?
O17C W9C O27C 76.4(6) . . ?
O24C W9C O27C 85.3(7) . . ?
O21C W9C O27C 73.3(7) . . ?
O104 W4A O4A 99.4(8) . . ?
O104 W4A O9A 100.1(8) . . ?
O4A W4A O9A 92.1(7) . . ?
O104 W4A O14A 96.4(8) . . ?
O4A W4A O14A 164.3(7) . . ?
O9A W4A O14A 85.8(7) . . ?
O104 W4A O8A 101.7(8) . . ?
O4A W4A O8A 90.9(7) . . ?
O9A W4A O8A 157.1(7) . . ?
O14A W4A O8A 85.2(7) . . ?
O104 W4A O26A 175.1(7) . . ?
O4A W4A O26A 78.2(6) . . ?
O9A W4A O26A 75.8(6) . . ?
O14A W4A O26A 86.1(6) . . ?
O8A W4A O26A 82.6(6) . . ?
O104 W4A Ti2A 129.5(6) . . ?
O4A W4A Ti2A 30.9(5) . . ?
O9A W4A Ti2A 80.6(5) . . ?
O14A W4A Ti2A 133.7(5) . . ?
O8A W4A Ti2A 90.6(5) . . ?
O26A W4A Ti2A 47.7(4) . . ?
O305 W5C O5C 103.0(8) . . ?
O305 W5C O10C 104.6(7) . . ?
O5C W5C O10C 90.1(7) . . ?
O305 W5C O15C 97.1(8) . . ?
O5C W5C O15C 159.8(7) . . ?
O10C W5C O15C 86.9(7) . . ?
O305 W5C O9C 101.6(7) . . ?
O5C W5C O9C 88.8(6) . . ?
O10C W5C O9C 153.4(7) . . ?
O15C W5C O9C 85.0(7) . . ?
O305 W5C O26C 173.9(7) . . ?
O5C W5C O26C 77.0(6) . . ?
O10C W5C O26C 81.5(6) . . ?
O15C W5C O26C 82.8(6) . . ?
O9C W5C O26C 72.3(6) . . ?
O305 W5C Ti2C 131.2(6) . . ?
O5C W5C Ti2C 28.8(5) . . ?
O10C W5C Ti2C 87.8(5) . . ?
O15C W5C Ti2C 131.0(5) . . ?
O9C W5C Ti2C 78.6(5) . . ?
O26C W5C Ti2C 48.2(4) . . ?
O203 W3B O3B 96.3(8) . . ?
O203 W3B O12B 98.8(8) . . ?
O3B W3B O12B 86.9(7) . . ?
O203 W3B O13B 101.1(8) . . ?
O3B W3B O13B 162.6(7) . . ?
O12B W3B O13B 91.5(7) . . ?
O203 W3B O7B 102.5(8) . . ?
O3B W3B O7B 86.8(7) . . ?
O12B W3B O7B 158.3(6) . . ?
O13B W3B O7B 88.5(7) . . ?
O203 W3B O25B 170.4(7) . . ?
O3B W3B O25B 76.4(6) . . ?
O12B W3B O25B 74.9(6) . . ?
O13B W3B O25B 86.4(6) . . ?
O7B W3B O25B 83.5(6) . . ?
O203 W3B Ti1B 125.5(6) . . ?
O3B W3B Ti1B 29.8(5) . . ?
O12B W3B Ti1B 78.0(5) . . ?
O13B W3B Ti1B 133.1(5) . . ?
O7B W3B Ti1B 86.2(4) . . ?
O25B W3B Ti1B 46.7(4) . . ?
O103 W3A O3A 99.8(8) . . ?
O103 W3A O12A 99.0(7) . . ?
O3A W3A O12A 90.1(6) . . ?
O103 W3A O7A 103.4(8) . . ?
O3A W3A O7A 91.2(7) . . ?
O12A W3A O7A 157.0(7) . . ?
O103 W3A O13A 98.5(8) . . ?
O3A W3A O13A 161.7(7) . . ?
O12A W3A O13A 86.9(7) . . ?
O7A W3A O13A 84.7(7) . . ?
O103 W3A O25A 174.7(7) . . ?
O3A W3A O25A 78.8(6) . . ?
O12A W3A O25A 76.0(6) . . ?
O7A W3A O25A 81.7(6) . . ?
O13A W3A O25A 83.0(6) . . ?
O103 W3A Ti1A 129.5(6) . . ?
O3A W3A Ti1A 30.4(5) . . ?
O12A W3A Ti1A 80.3(5) . . ?
O7A W3A Ti1A 89.4(5) . . ?
O13A W3A Ti1A 131.5(5) . . ?
O25A W3A Ti1A 48.6(4) . . ?
O106 W6A O6A 100.6(7) . . ?
O106 W6A O16A 99.7(7) . . ?
O6A W6A O16A 159.5(6) . . ?
O106 W6A O12A 103.2(7) . . ?
O6A W6A O12A 90.7(6) . . ?
O16A W6A O12A 88.1(6) . . ?
O106 W6A O11A 101.6(7) . . ?
O6A W6A O11A 88.3(6) . . ?
O16A W6A O11A 84.2(6) . . ?
O12A W6A O11A 154.9(6) . . ?
O106 W6A O25A 175.4(7) . . ?
O6A W6A O25A 77.6(6) . . ?
O16A W6A O25A 82.5(6) . . ?
O12A W6A O25A 72.7(6) . . ?
O11A W6A O25A 82.6(6) . . ?
O106 W6A Ti1A 129.5(5) . . ?
O6A W6A Ti1A 29.5(5) . . ?
O16A W6A Ti1A 130.8(4) . . ?
O12A W6A Ti1A 79.1(4) . . ?
O11A W6A Ti1A 87.9(4) . . ?
O25A W6A Ti1A 48.3(4) . . ?
O212 W12B O24B 100.4(8) . . ?
O212 W12B O20B 99.9(8) . . ?
O24B W12B O20B 159.4(7) . . ?
O212 W12B O23B 102.9(7) . . ?
O24B W12B O23B 89.6(7) . . ?
O20B W12B O23B 89.0(7) . . ?
O212 W12B O16B 101.7(8) . . ?
O24B W12B O16B 89.7(7) . . ?
O20B W12B O16B 83.0(7) . . ?
O23B W12B O16B 155.1(7) . . ?
O212 W12B O28B 174.4(7) . . ?
O24B W12B O28B 83.5(6) . . ?
O20B W12B O28B 76.5(7) . . ?
O23B W12B O28B 73.0(6) . . ?
O16B W12B O28B 82.2(6) . . ?
O412 W12D O23D 102.7(8) . . ?
O412 W12D O16D 103.7(8) . . ?
O23D W12D O16D 153.3(7) . . ?
O412 W12D O20D 99.8(8) . . ?
O23D W12D O20D 89.2(7) . . ?
O16D W12D O20D 82.8(7) . . ?
O412 W12D O24D 101.3(8) . . ?
O23D W12D O24D 93.8(7) . . ?
O16D W12D O24D 84.6(7) . . ?
O20D W12D O24D 157.5(7) . . ?
O412 W12D O28D 173.2(7) . . ?
O23D W12D O28D 72.7(7) . . ?
O16D W12D O28D 80.7(6) . . ?
O20D W12D O28D 75.5(6) . . ?
O24D W12D O28D 84.1(6) . . ?
O111 W11A O15A 99.5(8) . . ?
O111 W11A O19A 98.5(8) . . ?
O15A W11A O19A 84.6(7) . . ?
O111 W11A O22A 99.7(8) . . ?
O15A W11A O22A 90.5(7) . . ?
O19A W11A O22A 161.7(7) . . ?
O111 W11A O23A 102.3(8) . . ?
O15A W11A O23A 158.1(7) . . ?
O19A W11A O23A 90.1(7) . . ?
O22A W11A O23A 88.0(7) . . ?
O111 W11A O28A 173.3(7) . . ?
O15A W11A O28A 85.0(6) . . ?
O19A W11A O28A 77.0(6) . . ?
O22A W11A O28A 85.1(6) . . ?
O23A W11A O28A 73.2(6) . . ?
O208 W8B O19B 102.6(8) . . ?
O208 W8B O20B 98.0(8) . . ?
O19B W8B O20B 84.1(7) . . ?
O208 W8B O10B 105.6(8) . . ?
O19B W8B O10B 88.0(7) . . ?
O20B W8B O10B 156.2(7) . . ?
O208 W8B O11B 101.2(8) . . ?
O19B W8B O11B 155.7(7) . . ?
O20B W8B O11B 88.1(7) . . ?
O10B W8B O11B 90.1(7) . . ?
O208 W8B O28B 173.6(7) . . ?
O19B W8B O28B 75.9(6) . . ?
O20B W8B O28B 75.7(7) . . ?
O10B W8B O28B 80.6(6) . . ?
O11B W8B O28B 79.9(6) . . ?
O210 W10B O21B 101.2(8) . . ?
O210 W10B O22B 101.2(8) . . ?
O21B W10B O22B 89.8(7) . . ?
O210 W10B O18B 100.5(8) . . ?
O21B W10B O18B 86.7(7) . . ?
O22B W10B O18B 158.3(7) . . ?
O210 W10B O14B 103.5(8) . . ?
O21B W10B O14B 155.0(7) . . ?
O22B W10B O14B 89.1(7) . . ?
O18B W10B O14B 85.2(7) . . ?
O210 W10B O27B 172.7(7) . . ?
O21B W10B O27B 74.0(6) . . ?
O22B W10B O27B 84.5(6) . . ?
O18B W10B O27B 73.9(6) . . ?
O14B W10B O27B 80.9(7) . . ?
O406 W6D O16D 103.1(9) . . ?
O406 W6D O12D 103.1(9) . . ?
O16D W6D O12D 87.6(7) . . ?
O406 W6D O6D 97.1(8) . . ?
O16D W6D O6D 159.7(7) . . ?
O12D W6D O6D 89.3(7) . . ?
O406 W6D O11D 102.6(9) . . ?
O16D W6D O11D 87.4(7) . . ?
O12D W6D O11D 154.3(7) . . ?
O6D W6D O11D 86.7(7) . . ?
O406 W6D O25D 171.6(8) . . ?
O16D W6D O25D 84.6(6) . . ?
O12D W6D O25D 73.6(7) . . ?
O6D W6D O25D 75.3(6) . . ?
O11D W6D O25D 80.9(6) . . ?
O406 W6D Ti1D 125.6(7) . . ?
O16D W6D Ti1D 131.1(5) . . ?
O12D W6D Ti1D 78.2(5) . . ?
O6D W6D Ti1D 29.0(5) . . ?
O11D W6D Ti1D 86.3(5) . . ?
O25D W6D Ti1D 46.6(4) . . ?
O311 W11C O19C 101.7(8) . . ?
O311 W11C O22C 99.7(7) . . ?
O19C W11C O22C 158.6(7) . . ?
O311 W11C O15C 105.4(8) . . ?
O19C W11C O15C 86.7(7) . . ?
O22C W11C O15C 88.0(7) . . ?
O311 W11C O23C 98.8(8) . . ?
O19C W11C O23C 88.7(7) . . ?
O22C W11C O23C 87.7(7) . . ?
O15C W11C O23C 155.9(7) . . ?
O311 W11C O28C 171.7(7) . . ?
O19C W11C O28C 75.9(7) . . ?
O22C W11C O28C 82.9(6) . . ?
O15C W11C O28C 82.5(6) . . ?
O23C W11C O28C 73.4(6) . . ?
O209 W9B O24B 104.1(8) . . ?
O209 W9B O13B 102.4(8) . . ?
O24B W9B O13B 87.4(7) . . ?
O209 W9B O17B 98.6(8) . . ?
O24B W9B O17B 156.9(7) . . ?
O13B W9B O17B 83.6(7) . . ?
O209 W9B O21B 103.4(8) . . ?
O24B W9B O21B 90.1(7) . . ?
O13B W9B O21B 153.9(7) . . ?
O17B W9B O21B 88.8(8) . . ?
O209 W9B O27B 171.2(7) . . ?
O24B W9B O27B 84.0(6) . . ?
O13B W9B O27B 81.3(6) . . ?
O17B W9B O27B 73.7(7) . . ?
O21B W9B O27B 72.7(6) . . ?
O107 W7A O8A 104.0(8) . . ?
O107 W7A O7A 101.9(8) . . ?
O8A W7A O7A 97.9(8) . . ?
O107 W7A O17A 100.1(8) . . ?
O8A W7A O17A 153.0(7) . . ?
O7A W7A O17A 88.8(8) . . ?
O107 W7A O18A 100.0(8) . . ?
O8A W7A O18A 83.4(7) . . ?
O7A W7A O18A 157.0(7) . . ?
O17A W7A O18A 80.5(7) . . ?
O107 W7A O27A 173.4(8) . . ?
O8A W7A O27A 81.2(6) . . ?
O7A W7A O27A 81.2(6) . . ?
O17A W7A O27A 74.0(7) . . ?
O18A W7A O27A 76.3(6) . . ?
O307 W7C O7C 100.8(8) . . ?
O307 W7C O8C 101.9(8) . . ?
O7C W7C O8C 98.3(7) . . ?
O307 W7C O17C 100.6(8) . . ?
O7C W7C O17C 87.4(7) . . ?
O8C W7C O17C 155.3(7) . . ?
O307 W7C O18C 100.3(8) . . ?
O7C W7C O18C 156.8(7) . . ?
O8C W7C O18C 86.6(7) . . ?
O17C W7C O18C 79.4(7) . . ?
O307 W7C O27C 174.0(8) . . ?
O7C W7C O27C 83.6(6) . . ?
O8C W7C O27C 81.2(6) . . ?
O17C W7C O27C 75.5(6) . . ?
O18C W7C O27C 74.7(6) . . ?
O408 W8D O11D 102.6(8) . . ?
O408 W8D O24 100.8(8) . . ?
O11D W8D O24 94.2(7) . . ?
O408 W8D O20D 102.6(8) . . ?
O11D W8D O20D 86.1(7) . . ?
O24 W8D O20D 156.0(7) . . ?
O408 W8D O19D 101.9(8) . . ?
O11D W8D O19D 155.2(7) . . ?
O24 W8D O19D 85.1(7) . . ?
O20D W8D O19D 84.8(7) . . ?
O408 W8D O28D 176.2(7) . . ?
O11D W8D O28D 81.1(6) . . ?
O24 W8D O28D 79.4(6) . . ?
O20D W8D O28D 76.9(6) . . ?
O19D W8D O28D 74.3(6) . . ?
O211 W11B O23B 101.6(8) . . ?
O211 W11B O22B 101.4(8) . . ?
O23B W11B O22B 89.4(7) . . ?
O211 W11B O15B 103.8(8) . . ?
O23B W11B O15B 154.4(7) . . ?
O22B W11B O15B 89.3(7) . . ?
O211 W11B O19B 101.0(8) . . ?
O23B W11B O19B 87.3(7) . . ?
O22B W11B O19B 157.6(7) . . ?
O15B W11B O19B 84.2(7) . . ?
O211 W11B O28B 173.3(8) . . ?
O23B W11B O28B 73.0(6) . . ?
O22B W11B O28B 82.7(6) . . ?
O15B W11B O28B 81.4(6) . . ?
O19B W11B O28B 75.2(6) . . ?
O204 W4B O9B 103.2(8) . . ?
O204 W4B O14B 99.0(8) . . ?
O9B W4B O14B 88.0(7) . . ?
O204 W4B O4B 99.8(8) . . ?
O9B W4B O4B 88.6(7) . . ?
O14B W4B O4B 161.2(8) . . ?
O204 W4B O8B 100.2(8) . . ?
O9B W4B O8B 156.6(7) . . ?
O14B W4B O8B 88.4(7) . . ?
O4B W4B O8B 87.4(7) . . ?
O204 W4B O26B 174.9(7) . . ?
O9B W4B O26B 74.5(6) . . ?
O14B W4B O26B 85.6(7) . . ?
O4B W4B O26B 75.6(7) . . ?
O8B W4B O26B 82.1(7) . . ?
O204 W4B Ti2B 128.2(6) . . ?
O9B W4B Ti2B 77.3(5) . . ?
O14B W4B Ti2B 132.5(6) . . ?
O4B W4B Ti2B 29.0(5) . . ?
O8B W4B Ti2B 88.3(5) . . ?
O26B W4B Ti2B 47.0(4) . . ?
O109 W9A O13A 106.7(8) . . ?
O109 W9A O24A 99.7(8) . . ?
O13A W9A O24A 91.7(7) . . ?
O109 W9A O17A 99.3(8) . . ?
O13A W9A O17A 86.9(7) . . ?
O24A W9A O17A 160.6(8) . . ?
O109 W9A O21A 96.1(8) . . ?
O13A W9A O21A 156.9(7) . . ?
O24A W9A O21A 88.1(7) . . ?
O17A W9A O21A 85.6(7) . . ?
O109 W9A O27A 168.6(8) . . ?
O13A W9A O27A 83.2(7) . . ?
O24A W9A O27A 85.6(6) . . ?
O17A W9A O27A 75.0(7) . . ?
O21A W9A O27A 73.8(6) . . ?
O310 W10C O22C 101.6(8) . . ?
O310 W10C O14C 103.5(8) . . ?
O22C W10C O14C 90.7(7) . . ?
O310 W10C O18C 97.3(8) . . ?
O22C W10C O18C 161.0(7) . . ?
O14C W10C O18C 85.3(7) . . ?
O310 W10C O21C 96.6(8) . . ?
O22C W10C O21C 90.0(7) . . ?
O14C W10C O21C 159.3(7) . . ?
O18C W10C O21C 87.4(7) . . ?
O310 W10C O27C 171.4(8) . . ?
O22C W10C O27C 83.4(6) . . ?
O14C W10C O27C 83.3(6) . . ?
O18C W10C O27C 77.7(7) . . ?
O21C W10C O27C 76.2(7) . . ?
O207 W7B O8B 101.5(9) . . ?
O207 W7B O7B 100.4(9) . . ?
O8B W7B O7B 96.8(7) . . ?
O207 W7B O17B 99.4(9) . . ?
O8B W7B O17B 158.1(8) . . ?
O7B W7B O17B 85.9(7) . . ?
O207 W7B O18B 100.3(9) . . ?
O8B W7B O18B 87.6(7) . . ?
O7B W7B O18B 157.5(7) . . ?
O17B W7B O18B 82.1(8) . . ?
O207 W7B O27B 174.7(8) . . ?
O8B W7B O27B 82.0(7) . . ?
O7B W7B O27B 83.0(6) . . ?
O17B W7B O27B 76.7(7) . . ?
O18B W7B O27B 75.8(6) . . ?
O101 Ti2B O4B 100.8(8) . . ?
O101 Ti2B O5B 102.0(7) . . ?
O4B Ti2B O5B 96.0(8) . . ?
O101 Ti2B O2B 100.4(7) . . ?
O4B Ti2B O2B 155.5(7) . . ?
O5B Ti2B O2B 91.4(7) . . ?
O101 Ti2B O1B 98.0(7) . . ?
O4B Ti2B O1B 89.2(8) . . ?
O5B Ti2B O1B 157.9(7) . . ?
O2B Ti2B O1B 75.8(7) . . ?
O101 Ti2B O26B 176.3(7) . . ?
O4B Ti2B O26B 76.1(7) . . ?
O5B Ti2B O26B 76.3(6) . . ?
O2B Ti2B O26B 83.0(6) . . ?
O1B Ti2B O26B 84.2(6) . . ?
O101 Ti2B Ti1B 100.2(5) . . ?
O4B Ti2B Ti1B 124.9(6) . . ?
O5B Ti2B Ti1B 128.0(5) . . ?
O2B Ti2B Ti1B 38.2(4) . . ?
O1B Ti2B Ti1B 37.6(5) . . ?
O26B Ti2B Ti1B 83.4(4) . . ?
O101 Ti2B W4B 130.6(6) . . ?
O4B Ti2B W4B 30.4(5) . . ?
O5B Ti2B W4B 83.3(5) . . ?
O2B Ti2B W4B 128.7(5) . . ?
O1B Ti2B W4B 90.7(5) . . ?
O26B Ti2B W4B 46.1(4) . . ?
Ti1B Ti2B W4B 114.92(15) . . ?
O101 Ti2B W5B 131.0(5) . . ?
O4B Ti2B W5B 84.3(6) . . ?
O5B Ti2B W5B 29.6(5) . . ?
O2B Ti2B W5B 90.9(5) . . ?
O1B Ti2B W5B 130.9(5) . . ?
O26B Ti2B W5B 47.0(4) . . ?
Ti1B Ti2B W5B 116.54(16) . . ?
W4B Ti2B W5B 61.40(9) . . ?
O401 Ti2C O5C 102.6(8) . . ?
O401 Ti2C O4C 102.1(8) . . ?
O5C Ti2C O4C 94.7(7) . . ?
O401 Ti2C O2C 100.7(7) . . ?
O5C Ti2C O2C 90.5(7) . . ?
O4C Ti2C O2C 154.8(7) . . ?
O401 Ti2C O1C 100.3(7) . . ?
O5C Ti2C O1C 155.5(7) . . ?
O4C Ti2C O1C 89.0(7) . . ?
O2C Ti2C O1C 76.5(7) . . ?
O401 Ti2C O26C 175.3(7) . . ?
O5C Ti2C O26C 74.9(6) . . ?
O4C Ti2C O26C 74.4(6) . . ?
O2C Ti2C O26C 83.4(6) . . ?
O1C Ti2C O26C 82.9(6) . . ?
O401 Ti2C Ti1C 100.7(6) . . ?
O5C Ti2C Ti1C 126.6(5) . . ?
O4C Ti2C Ti1C 125.9(5) . . ?
O2C Ti2C Ti1C 37.9(5) . . ?
O1C Ti2C Ti1C 38.8(4) . . ?
O26C Ti2C Ti1C 84.0(4) . . ?
O401 Ti2C W5C 131.4(6) . . ?
O5C Ti2C W5C 29.2(5) . . ?
O4C Ti2C W5C 84.0(5) . . ?
O2C Ti2C W5C 88.9(5) . . ?
O1C Ti2C W5C 128.2(5) . . ?
O26C Ti2C W5C 45.8(4) . . ?
Ti1C Ti2C W5C 114.43(15) . . ?
O401 Ti2C W4C 131.0(6) . . ?
O5C Ti2C W4C 82.7(5) . . ?
O4C Ti2C W4C 29.4(5) . . ?
O2C Ti2C W4C 128.2(5) . . ?
O1C Ti2C W4C 89.0(5) . . ?
O26C Ti2C W4C 45.2(4) . . ?
Ti1C Ti2C W4C 114.96(17) . . ?
W5C Ti2C W4C 61.87(8) . . ?
O6D Ti1D O401 103.8(8) . . ?
O6D Ti1D O3D 95.4(7) . . ?
O401 Ti1D O3D 99.3(8) . . ?
O6D Ti1D O2D 91.9(7) . . ?
O401 Ti1D O2D 98.6(7) . . ?
O3D Ti1D O2D 158.5(7) . . ?
O6D Ti1D O1D 156.7(8) . . ?
O401 Ti1D O1D 97.6(8) . . ?
O3D Ti1D O1D 90.0(7) . . ?
O2D Ti1D O1D 75.8(7) . . ?
O6D Ti1D O25D 76.4(6) . . ?
O401 Ti1D O25D 176.5(7) . . ?
O3D Ti1D O25D 77.3(6) . . ?
O2D Ti1D O25D 84.8(6) . . ?
O1D Ti1D O25D 82.8(6) . . ?
O6D Ti1D Ti2D 127.5(6) . . ?
O401 Ti1D Ti2D 99.1(6) . . ?
O3D Ti1D Ti2D 126.6(5) . . ?
O2D Ti1D Ti2D 37.8(5) . . ?
O1D Ti1D Ti2D 38.0(5) . . ?
O25D Ti1D Ti2D 83.4(4) . . ?
O6D Ti1D W6D 31.2(5) . . ?
O401 Ti1D W6D 134.3(6) . . ?
O3D Ti1D W6D 83.9(5) . . ?
O2D Ti1D W6D 92.1(5) . . ?
O1D Ti1D W6D 128.0(5) . . ?
O25D Ti1D W6D 45.4(4) . . ?
Ti2D Ti1D W6D 115.40(16) . . ?
O6D Ti1D W3D 84.9(5) . . ?
O401 Ti1D W3D 130.5(6) . . ?
O3D Ti1D W3D 31.3(5) . . ?
O2D Ti1D W3D 130.2(5) . . ?
O1D Ti1D W3D 88.2(5) . . ?
O25D Ti1D W3D 46.1(4) . . ?
Ti2D Ti1D W3D 113.88(16) . . ?
W6D Ti1D W3D 61.60(8) . . ?
O301 Ti1C O3C 104.2(8) . . ?
O301 Ti1C O6C 100.8(7) . . ?
O3C Ti1C O6C 94.4(7) . . ?
O301 Ti1C O2C 96.5(8) . . ?
O3C Ti1C O2C 156.9(7) . . ?
O6C Ti1C O2C 91.6(7) . . ?
O301 Ti1C O1C 99.2(7) . . ?
O3C Ti1C O1C 89.5(7) . . ?
O6C Ti1C O1C 158.0(7) . . ?
O2C Ti1C O1C 76.9(7) . . ?
O301 Ti1C O25C 177.3(7) . . ?
O3C Ti1C O25C 75.4(6) . . ?
O6C Ti1C O25C 76.6(6) . . ?
O2C Ti1C O25C 84.4(6) . . ?
O1C Ti1C O25C 83.5(6) . . ?
O301 Ti1C Ti2C 97.2(6) . . ?
O3C Ti1C Ti2C 127.3(5) . . ?
O6C Ti1C Ti2C 128.1(5) . . ?
O2C Ti1C Ti2C 37.9(5) . . ?
O1C Ti1C Ti2C 39.2(5) . . ?
O25C Ti1C Ti2C 85.0(4) . . ?
O301 Ti1C W3C 132.9(6) . . ?
O3C Ti1C W3C 29.2(5) . . ?
O6C Ti1C W3C 83.3(5) . . ?
O2C Ti1C W3C 130.5(5) . . ?
O1C Ti1C W3C 89.9(5) . . ?
O25C Ti1C W3C 46.5(4) . . ?
Ti2C Ti1C W3C 117.07(16) . . ?
O301 Ti1C W6C 130.0(6) . . ?
O3C Ti1C W6C 83.4(5) . . ?
O6C Ti1C W6C 29.5(5) . . ?
O2C Ti1C W6C 91.2(5) . . ?
O1C Ti1C W6C 130.6(5) . . ?
O25C Ti1C W6C 47.3(4) . . ?
Ti2C Ti1C W6C 117.27(15) . . ?
W3C Ti1C W6C 62.03(8) . . ?
O301 Ti2D O4D 100.3(8) . . ?
O301 Ti2D O5D 101.8(7) . . ?
O4D Ti2D O5D 94.9(7) . . ?
O301 Ti2D O1D 97.7(7) . . ?
O4D Ti2D O1D 90.9(7) . . ?
O5D Ti2D O1D 158.3(7) . . ?
O301 Ti2D O2D 97.0(7) . . ?
O4D Ti2D O2D 160.3(7) . . ?
O5D Ti2D O2D 90.7(7) . . ?
O1D Ti2D O2D 77.5(7) . . ?
O301 Ti2D O26D 175.6(7) . . ?
O4D Ti2D O26D 76.0(6) . . ?
O5D Ti2D O26D 76.3(6) . . ?
O1D Ti2D O26D 84.9(6) . . ?
O2D Ti2D O26D 87.0(6) . . ?
O301 Ti2D Ti1D 98.2(6) . . ?
O4D Ti2D Ti1D 128.7(6) . . ?
O5D Ti2D Ti1D 127.1(5) . . ?
O1D Ti2D Ti1D 39.2(5) . . ?
O2D Ti2D Ti1D 38.3(4) . . ?
O26D Ti2D Ti1D 86.1(4) . . ?
O301 Ti2D W4D 131.3(6) . . ?
O4D Ti2D W4D 31.5(5) . . ?
O5D Ti2D W4D 82.8(5) . . ?
O1D Ti2D W4D 91.4(5) . . ?
O2D Ti2D W4D 131.7(5) . . ?
O26D Ti2D W4D 44.8(4) . . ?
Ti1D Ti2D W4D 117.52(15) . . ?
O301 Ti2D W5D 131.2(6) . . ?
O4D Ti2D W5D 85.0(5) . . ?
O5D Ti2D W5D 29.7(5) . . ?
O1D Ti2D W5D 130.9(5) . . ?
O2D Ti2D W5D 90.7(5) . . ?
O26D Ti2D W5D 46.7(4) . . ?
Ti1D Ti2D W5D 116.09(16) . . ?
W4D Ti2D W5D 61.63(8) . . ?
O201 Ti1B O3B 101.4(8) . . ?
O201 Ti1B O6B 100.4(8) . . ?
O3B Ti1B O6B 95.0(7) . . ?
O201 Ti1B O1B 98.0(8) . . ?
O3B Ti1B O1B 92.9(7) . . ?
O6B Ti1B O1B 158.1(7) . . ?
O201 Ti1B O2B 99.6(8) . . ?
O3B Ti1B O2B 157.9(7) . . ?
O6B Ti1B O2B 88.0(7) . . ?
O1B Ti1B O2B 77.3(7) . . ?
O201 Ti1B O25B 174.7(8) . . ?
O3B Ti1B O25B 76.5(6) . . ?
O6B Ti1B O25B 75.1(6) . . ?
O1B Ti1B O25B 87.0(6) . . ?
O2B Ti1B O25B 83.1(6) . . ?
O201 Ti1B Ti2B 99.7(6) . . ?
O3B Ti1B Ti2B 129.8(6) . . ?
O6B Ti1B Ti2B 125.0(5) . . ?
O1B Ti1B Ti2B 39.1(5) . . ?
O2B Ti1B Ti2B 38.3(5) . . ?
O25B Ti1B Ti2B 85.2(4) . . ?
O201 Ti1B W3B 132.0(6) . . ?
O3B Ti1B W3B 31.0(5) . . ?
O6B Ti1B W3B 83.9(5) . . ?
O1B Ti1B W3B 92.6(5) . . ?
O2B Ti1B W3B 128.4(5) . . ?
O25B Ti1B W3B 45.5(4) . . ?
Ti2B Ti1B W3B 116.82(17) . . ?
O201 Ti1B W6B 130.5(7) . . ?
O3B Ti1B W6B 84.2(5) . . ?
O6B Ti1B W6B 30.5(5) . . ?
O1B Ti1B W6B 131.1(5) . . ?
O2B Ti1B W6B 87.5(5) . . ?
O25B Ti1B W6B 44.7(4) . . ?
Ti2B Ti1B W6B 114.06(16) . . ?
W3B Ti1B W6B 61.64(9) . . ?
O101 Ti1A O6A 103.6(7) . . ?
O101 Ti1A O3A 100.4(7) . . ?
O6A Ti1A O3A 94.9(7) . . ?
O101 Ti1A O1A 98.6(7) . . ?
O6A Ti1A O1A 155.7(7) . . ?
O3A Ti1A O1A 90.9(7) . . ?
O101 Ti1A O2A 102.0(7) . . ?
O6A Ti1A O2A 88.5(7) . . ?
O3A Ti1A O2A 155.9(7) . . ?
O1A Ti1A O2A 77.1(7) . . ?
O101 Ti1A O25A 173.2(7) . . ?
O6A Ti1A O25A 76.2(6) . . ?
O3A Ti1A O25A 72.9(6) . . ?
O1A Ti1A O25A 83.0(6) . . ?
O2A Ti1A O25A 84.8(6) . . ?
O101 Ti1A Ti2A 100.8(6) . . ?
O6A Ti1A Ti2A 126.9(5) . . ?
O3A Ti1A Ti2A 125.8(5) . . ?
O1A Ti1A Ti2A 36.9(5) . . ?
O2A Ti1A Ti2A 40.3(5) . . ?
O25A Ti1A Ti2A 84.4(4) . . ?
O101 Ti1A W3A 128.6(6) . . ?
O6A Ti1A W3A 84.4(5) . . ?
O3A Ti1A W3A 28.5(5) . . ?
O1A Ti1A W3A 89.7(5) . . ?
O2A Ti1A W3A 129.2(5) . . ?
O25A Ti1A W3A 44.6(4) . . ?
Ti2A Ti1A W3A 114.44(16) . . ?
O101 Ti1A W6A 132.4(5) . . ?
O6A Ti1A W6A 29.8(5) . . ?
O3A Ti1A W6A 82.3(5) . . ?
O1A Ti1A W6A 129.0(5) . . ?
O2A Ti1A W6A 89.1(5) . . ?
O25A Ti1A W6A 46.6(3) . . ?
Ti2A Ti1A W6A 115.94(16) . . ?
W3A Ti1A W6A 61.97(8) . . ?
O201 Ti2A O5A 104.1(8) . . ?
O201 Ti2A O4A 100.8(8) . . ?
O5A Ti2A O4A 96.6(7) . . ?
O201 Ti2A O1A 97.6(8) . . ?
O5A Ti2A O1A 154.5(7) . . ?
O4A Ti2A O1A 92.1(7) . . ?
O201 Ti2A O2A 99.9(8) . . ?
O5A Ti2A O2A 87.5(7) . . ?
O4A Ti2A O2A 157.1(7) . . ?
O1A Ti2A O2A 75.7(7) . . ?
O201 Ti2A O26A 177.0(8) . . ?
O5A Ti2A O26A 74.9(6) . . ?
O4A Ti2A O26A 76.6(6) . . ?
O1A Ti2A O26A 84.0(6) . . ?
O2A Ti2A O26A 82.9(6) . . ?
O201 Ti2A Ti1A 99.0(6) . . ?
O5A Ti2A Ti1A 124.8(5) . . ?
O4A Ti2A Ti1A 127.3(5) . . ?
O1A Ti2A Ti1A 36.9(5) . . ?
O2A Ti2A Ti1A 38.9(5) . . ?
O26A Ti2A Ti1A 83.9(4) . . ?
O201 Ti2A W5A 132.1(7) . . ?
O5A Ti2A W5A 28.7(5) . . ?
O4A Ti2A W5A 84.3(5) . . ?
O1A Ti2A W5A 130.0(5) . . ?
O2A Ti2A W5A 89.0(5) . . ?
O26A Ti2A W5A 46.6(4) . . ?
Ti1A Ti2A W5A 115.66(16) . . ?
O201 Ti2A W4A 130.0(6) . . ?
O5A Ti2A W4A 84.0(5) . . ?
O4A Ti2A W4A 29.6(5) . . ?
O1A Ti2A W4A 92.1(5) . . ?
O2A Ti2A W4A 129.9(5) . . ?
O26A Ti2A W4A 47.3(4) . . ?
Ti1A Ti2A W4A 116.71(16) . . ?
W5A Ti2A W4A 62.17(8) . . ?
C413 N4A C401 108.9 . . ?
C413 N4A C409 104.9 . . ?
C401 N4A C409 111.1 . . ?
C413 N4A C405 116.5 . . ?
C401 N4A C405 107.4 . . ?
C409 N4A C405 108 . . ?
N4A C401 C402 113.4 . . ?
C401 C402 C403 105.8 . . ?
C404 C403 C402 108.3 . . ?
C406 C405 N4A 110.9 . . ?
C405 C406 C407 105.3 . . ?
C408 C407 C406 112.5 . . ?
N4A C409 C410 114.3 . . ?
C409 C410 C411 106.2 . . ?
C412 C411 C410 108.7 . . ?
N4A C413 C414 113.6 . . ?
C415 C414 C413 108.8 . . ?
C414 C415 C416 114.9 . . ?
C109 N1A C105 104.6 . . ?
C109 N1A C101 110.1 . . ?
C105 N1A C101 111.8 . . ?
C109 N1A C113 115 . . ?
C105 N1A C113 113.7 . . ?
C101 N1A C113 101.8 . . ?
C102 C101 N1A 111.8 . . ?
C101 C102 C103 103.2 . . ?
C104 C103 C102 114.5 . . ?
N1A C105 C106 114.5 . . ?
C107 C106 C105 105.1 . . ?
C107 C106 C128 18.4 . . ?
C105 C106 C128 103.2 . . ?
C128 C107 C106 92.8 . . ?
C128 C107 C108 11.3 . . ?
C106 C107 C108 103.1 . . ?
C107 C128 C108 163.9 . . ?
C107 C128 C106 68.8 . . ?
C108 C128 C106 125.7 . . ?
C128 C108 C107 4.8 . . ?
N1A C109 C110 111.8 . . ?
C111 C110 C109 101.9 . . ?
C112 C111 C110 104.1 . . ?
C114 C113 N1A 109.4 . . ?
C115 C114 C113 105 . . ?
C114 C115 C116 112.7 . . ?
C501 N5A C509 113 . . ?
C501 N5A C513 111.4 . . ?
C509 N5A C513 104.7 . . ?
C501 N5A C505 103.7 . . ?
C509 N5A C505 112.9 . . ?
C513 N5A C505 111.3 . . ?
N5A C501 C502 117.7 . . ?
C503 C502 C501 105.3 . . ?
C504 C503 C502 110.2 . . ?
N5A C505 C506 113.6 . . ?
C527 C506 C505 105.7 . . ?
C506 C527 C508 104.4 . . ?
C506 C527 C507 88.8 . . ?
C508 C527 C507 133.2 . . ?
N5A C509 C510 118 . . ?
C511 C510 C509 113.8 . . ?
C510 C511 C512 109.6 . . ?
N5A C513 C514 113.5 . . ?
C513 C514 C515 105.5 . . ?
C516 C515 C514 103.2 . . ?
C301 N3A C313 113 . . ?
C301 N3A C305 106 . . ?
C313 N3A C305 113.6 . . ?
C301 N3A C309 109.9 . . ?
C313 N3A C309 101.1 . . ?
C305 N3A C309 113.5 . . ?
N3A C301 C302 113.4 . . ?
C303 C302 C301 105.8 . . ?
C302 C303 C304 109.6 . . ?
N3A C305 C306 117.3 . . ?
C307 C306 C305 107.6 . . ?
C306 C307 C308 112.2 . . ?
N3A C309 C310 112.8 . . ?
C311 C310 C309 111.3 . . ?
C310 C311 C312 103.7 . . ?
N3A C313 C314 110.2 . . ?
C313 C314 C315 99.9 . . ?
C316 C315 C314 96.1 . . ?
C605 N6A C609 113.1 . . ?
C605 N6A C601 105.4 . . ?
C609 N6A C601 111 . . ?
C605 N6A C613 114.7 . . ?
C609 N6A C613 101.7 . . ?
C601 N6A C613 111 . . ?
N6A C601 C602 118.8 . . ?
C603 C602 C601 106.3 . . ?
C604 C603 C602 111.3 . . ?
N6A C605 C606 117.6 . . ?
C607 C606 C605 112.4 . . ?
C606 C607 C608 114.6 . . ?
N6A C609 C610 114 . . ?
C611 C610 C609 105.8 . . ?
C632 C611 C610 117.8 . . ?
C632 C611 C612 110.4 . . ?
C610 C611 C612 110.4 . . ?
C614 C613 N6A 109.7 . . ?
C613 C614 C615 104.8 . . ?
C616 C615 C614 116.1 . . ?
C713 N7A C709 110.6 . . ?
C713 N7A C701 109.5 . . ?
C709 N7A C701 113.9 . . ?
C713 N7A C705 105.4 . . ?
C709 N7A C705 114.5 . . ?
C701 N7A C705 102.3 . . ?
C702 C701 N7A 112.1 . . ?
C703 C702 C701 107.1 . . ?
C702 C703 C704 109.6 . . ?
C706 C705 N7A 113.4 . . ?
C707 C706 C705 87.8 . . ?
C706 C707 C708 130.6 . . ?
C728 C708 C707 97.8 . . ?
C710 C709 N7A 117.2 . . ?
C709 C710 C711 107.2 . . ?
C732 C711 C710 132.9 . . ?
C732 C711 C712 92.7 . . ?
C710 C711 C712 117.3 . . ?
C714 C713 N7A 105.8 . . ?
C714 C713 C734 37.8 . . ?
N7A C713 C734 114.6 . . ?
C734 C714 C713 90.8 . . ?
C734 C714 C715 54.3 . . ?
C713 C714 C715 103.7 . . ?
C714 C734 C715 90.7 . . ?
C714 C734 C713 51.3 . . ?
C715 C734 C713 103.2 . . ?
C734 C715 C716 100 . . ?
C734 C715 C714 34.9 . . ?
C716 C715 C714 125 . . ?
C801 N8A C805 111.6 . . ?
C801 N8A C809 110.6 . . ?
C805 N8A C809 125.1 . . ?
C801 N8A C813 109.9 . . ?
C805 N8A C813 92.3 . . ?
C809 N8A C813 104.7 . . ?
N8A C801 C802 117.4 . . ?
C801 C802 C823 137.8 . . ?
C823 C804 C803 116.9 . . ?
C804 C823 C802 97.4 . . ?
C806 C805 N8A 105.4 . . ?
C805 C806 C807 101.9 . . ?
C808 C807 C806 141.7 . . ?
C810 C809 N8A 112.5 . . ?
C809 C810 C811 100.3 . . ?
C812 C811 C810 112 . . ?
C834 C813 N8A 111 . . ?
C814 C834 C813 100.7 . . ?
C814 C834 C815 145.8 . . ?
C813 C834 C815 94.7 . . ?
C816 C815 C834 109.9 . . ?
C201 N2A C213 101.5 . . ?
C201 N2A C205 115.5 . . ?
C213 N2A C205 112.8 . . ?
C201 N2A C209 116.3 . . ?
C213 N2A C209 109.6 . . ?
C205 N2A C209 101.6 . . ?
N2A C201 C202 115.4 . . ?
C201 C202 C203 110.2 . . ?
C204 C203 C202 116.8 . . ?
C206 C205 N2A 112.2 . . ?
C205 C206 C207 108.6 . . ?
C206 C207 C208 117.6 . . ?
C210 C209 N2A 113.5 . . ?
C209 C210 C211 105.1 . . ?
C210 C211 C212 101.2 . . ?
N2A C213 C214 112.3 . . ?
C236 C214 C215 77.8 . . ?
C236 C214 C213 94.3 . . ?
C215 C214 C213 105.8 . . ?
C214 C215 C216 117 . . ?
C214 C215 C236 48.1 . . ?
C216 C215 C236 154.8 . . ?
C214 C236 C215 54.1 . . ?
C163 N1B C155 121.7 . . ?
C163 N1B C159 99.1 . . ?
C155 N1B C159 120.7 . . ?
C163 N1B C151 110.4 . . ?
C155 N1B C151 99.7 . . ?
C159 N1B C151 104.1 . . ?
C152 C151 N1B 107.7 . . ?
C151 C152 C153 98.1 . . ?
C154 C153 C152 85 . . ?
N1B C155 C156 112.8 . . ?
C157 C156 C155 106.4 . . ?
C157 C156 C178 37.4 . . ?
C155 C156 C178 107.4 . . ?
C178 C157 C156 81.3 . . ?
C178 C157 C158 79.2 . . ?
C156 C157 C158 102.9 . . ?
C178 C157 C177 36.2 . . ?
C156 C157 C177 106.3 . . ?
C158 C157 C177 98.6 . . ?
C178 C177 C157 35.6 . . ?
C157 C158 C178 38 . . ?
C157 C178 C177 108.2 . . ?
C157 C178 C158 62.8 . . ?
C177 C178 C158 125.5 . . ?
C157 C178 C156 61.3 . . ?
C177 C178 C156 136.5 . . ?
C158 C178 C156 89.1 . . ?
N1B C159 C160 119.8 . . ?
C161 C160 C159 129.4 . . ?
C160 C161 C162 129.2 . . ?
C164 C163 N1B 110 . . ?
C163 C164 C165 118.4 . . ?
C166 C165 C186 55.2 . . ?
C166 C165 C164 123.4 . . ?
C186 C165 C164 130.1 . . ?
C186 C166 C165 65 . . ?
C166 C186 C165 59.8 . . ?
C759 N7B C751 116.9 . . ?
C759 N7B C755 103.5 . . ?
C751 N7B C755 107.9 . . ?
C759 N7B C763 122.8 . . ?
C751 N7B C763 109 . . ?
C755 N7B C763 92.5 . . ?
C752 C751 N7B 134.7 . . ?
C753 C752 C751 128.1 . . ?
C752 C753 C754 117.3 . . ?
C756 C755 N7B 114.1 . . ?
C757 C756 C755 107.4 . . ?
C757 C756 C777 46.2 . . ?
C755 C756 C777 107.6 . . ?
C757 C756 C778 19.4 . . ?
C755 C756 C778 98.3 . . ?
C777 C756 C778 31.4 . . ?
C778 C757 C756 140 . . ?
C778 C757 C777 55.5 . . ?
C756 C757 C777 92.2 . . ?
C778 C757 C758 46.8 . . ?
C756 C757 C758 153.2 . . ?
C777 C757 C758 73.6 . . ?
C778 C777 C757 54.9 . . ?
C778 C777 C756 93.5 . . ?
C757 C777 C756 41.6 . . ?
C778 C777 C758 44.6 . . ?
C757 C777 C758 69 . . ?
C756 C777 C758 107.6 . . ?
C778 C758 C757 34.2 . . ?
C778 C758 C777 33 . . ?
C757 C758 C777 37.5 . . ?
C757 C778 C777 69.5 . . ?
C757 C778 C758 98.9 . . ?
C777 C778 C758 102.4 . . ?
C757 C778 C756 20.5 . . ?
C777 C778 C756 55.1 . . ?
C758 C778 C756 114.7 . . ?
N7B C759 C760 128.2 . . ?
C764 C763 N7B 101.8 . . ?
C763 C764 C765 109.2 . . ?
C766 C765 C764 113.5 . . ?
C651 N6B C655 109.6 . . ?
C651 N6B C659 110.5 . . ?
C655 N6B C659 109.6 . . ?
C651 N6B C663 106.8 . . ?
C655 N6B C663 112.1 . . ?
C659 N6B C663 108.2 . . ?
C652 C651 N6B 119.1 . . ?
C651 C652 C653 118.5 . . ?
C656 C655 N6B 118.1 . . ?
C655 C656 C657 112.1 . . ?
C656 C657 C658 100.9 . . ?
C660 C659 N6B 119.5 . . ?
C661 C660 C659 112.7 . . ?
C662 C661 C660 110.4 . . ?
C664 C663 N6B 114.1 . . ?
C663 C664 C665 106.9 . . ?
C664 C665 C666 110.3 . . ?
C555 N5B C559 106.2 . . ?
C555 N5B C551 103.4 . . ?
C559 N5B C551 119.5 . . ?
C555 N5B C563 105.2 . . ?
C559 N5B C563 117.4 . . ?
C551 N5B C563 103.5 . . ?
N5B C551 C552 105.4 . . ?
C553 C552 C551 98.6 . . ?
C552 C553 C554 122.2 . . ?
N5B C555 C556 106 . . ?
C557 C556 C555 83.7 . . ?
C558 C557 C556 92.4 . . ?
C561 C559 C560 54.6 . . ?
C561 C559 N5B 144.3 . . ?
C560 C559 N5B 109.5 . . ?
C561 C560 C559 57.4 . . ?
C561 C560 C580 43 . . ?
C559 C560 C580 97.5 . . ?
C561 C560 C562 83.9 . . ?
C559 C560 C562 127.6 . . ?
C580 C560 C562 66 . . ?
C561 C580 C581 117.2 . . ?
C561 C580 C560 45.2 . . ?
C581 C580 C560 149.9 . . ?
C561 C580 C562 78.6 . . ?
C581 C580 C562 152.4 . . ?
C560 C580 C562 57.3 . . ?
C580 C561 C560 91.8 . . ?
C580 C561 C559 149.3 . . ?
C560 C561 C559 68 . . ?
C580 C561 C562 66.5 . . ?
C560 C561 C562 59 . . ?
C559 C561 C562 116.1 . . ?
C560 C562 C580 56.6 . . ?
C560 C562 C561 37.1 . . ?
C580 C562 C561 34.9 . . ?
C564 C563 C568 52.3 . . ?
C564 C563 N5B 103.5 . . ?
C568 C563 N5B 101.7 . . ?
C563 C564 C568 77.1 . . ?
C563 C564 C565 105.8 . . ?
C568 C564 C565 61.1 . . ?
C564 C568 C565 66.4 . . ?
C564 C568 C585 115.6 . . ?
C565 C568 C585 53.8 . . ?
C564 C568 C563 50.5 . . ?
C565 C568 C563 93.4 . . ?
C585 C568 C563 143 . . ?
C564 C568 C586 104.5 . . ?
C565 C568 C586 40.7 . . ?
C585 C568 C586 36.2 . . ?
C563 C568 C586 108.3 . . ?
C586 C565 C585 52.3 . . ?
C586 C565 C568 89.7 . . ?
C585 C565 C568 63.2 . . ?
C586 C565 C564 137.2 . . ?
C585 C565 C564 111.5 . . ?
C568 C565 C564 52.5 . . ?
C586 C565 C566 25.1 . . ?
C585 C565 C566 29.5 . . ?
C568 C565 C566 83.3 . . ?
C564 C565 C566 135.7 . . ?
C566 C585 C586 49.4 . . ?
C566 C585 C565 107.4 . . ?
C586 C585 C565 60.6 . . ?
C566 C585 C568 132 . . ?
C586 C585 C568 94.3 . . ?
C565 C585 C568 63 . . ?
C586 C566 C585 76.2 . . ?
C586 C566 C565 36.7 . . ?
C585 C566 C565 43.1 . . ?
C566 C586 C585 54.4 . . ?
C566 C586 C565 118.3 . . ?
C585 C586 C565 67 . . ?
C566 C586 C568 97.4 . . ?
C585 C586 C568 49.5 . . ?
C565 C586 C568 49.6 . . ?
C851 N8B C855 123.1 . . ?
C851 N8B C863 102.4 . . ?
C855 N8B C863 110.7 . . ?
C851 N8B C859 103.4 . . ?
C855 N8B C859 111.6 . . ?
C863 N8B C859 103.8 . . ?
N8B C851 C852 107.6 . . ?
C853 C852 C851 110.3 . . ?
C854 C853 C852 109.5 . . ?
C856 C855 N8B 112 . . ?
C855 C856 C857 114.1 . . ?
C858 C857 C856 117.7 . . ?
C860 C859 N8B 115.5 . . ?
C859 C860 C861 107.1 . . ?
C864 C863 N8B 112.3 . . ?
C863 C864 C865 114.1 . . ?
C863 C864 C885 109.4 . . ?
C865 C864 C885 56.1 . . ?
C885 C865 C864 64.7 . . ?
C865 C885 C866 86 . . ?
C865 C885 C864 59.2 . . ?
C866 C885 C864 113.5 . . ?
C455 N4B C459 117.1 . . ?
C455 N4B C463 105.6 . . ?
C459 N4B C463 98 . . ?
C455 N4B C451 118.3 . . ?
C459 N4B C451 107 . . ?
C463 N4B C451 108.7 . . ?
C452 C451 N4B 110.5 . . ?
C451 C452 C453 108.9 . . ?
C454 C453 C452 112.8 . . ?
N4B C455 C476 111.6 . . ?
C476 C456 C477 103.8 . . ?
C456 C476 C455 101.3 . . ?
C457 C477 C456 82.3 . . ?
N4B C459 C481 103.5 . . ?
N4B C459 C460 124.6 . . ?
C481 C459 C460 43.3 . . ?
C461 C460 C481 91.3 . . ?
C461 C460 C459 95.2 . . ?
C481 C460 C459 66.7 . . ?
C460 C461 C481 45.1 . . ?
C460 C481 C459 70 . . ?
C460 C481 C461 43.6 . . ?
C459 C481 C461 79.1 . . ?
C464 C463 N4B 116.6 . . ?
C465 C464 C463 114.1 . . ?
C466 C465 C464 109.4 . . ?
O26A Si1A O25A 111.8(9) . . ?
O26A Si1A O27A 111.2(9) . . ?
O25A Si1A O27A 107.8(8) . . ?
O26A Si1A O28A 110.6(9) . . ?
O25A Si1A O28A 109.7(8) . . ?
O27A Si1A O28A 105.5(8) . . ?
O25D Si2D O28D 111.4(9) . . ?
O25D Si2D O27D 111.5(8) . . ?
O28D Si2D O27D 106.6(8) . . ?
O25D Si2D O26D 110.9(8) . . ?
O28D Si2D O26D 108.1(8) . . ?
O27D Si2D O26D 108.1(8) . . ?
O25C Si2C O28C 110.4(8) . . ?
O25C Si2C O27C 111.5(9) . . ?
O28C Si2C O27C 105.5(8) . . ?
O25C Si2C O26C 110.4(9) . . ?
O28C Si2C O26C 110.5(9) . . ?
O27C Si2C O26C 108.4(9) . . ?
O26B Si1B O27B 110.0(9) . . ?
O26B Si1B O28B 111.2(9) . . ?
O27B Si1B O28B 106.8(9) . . ?
O26B Si1B O25B 111.1(9) . . ?
O27B Si1B O25B 109.6(8) . . ?
O28B Si1B O25B 108.0(9) . . ?
W9A O24A W12A 155.1(9) . . ?
Ti1A O6A W6A 120.7(8) . . ?
W4C O9C W5C 121.3(8) . . ?
W5D O5D Ti2D 120.6(8) . . ?
W3C O12C W6C 121.8(9) . . ?
Ti1B O3B W3B 119.2(9) . . ?
W4A O9A W5A 119.5(8) . . ?
W3B O12B W6B 117.9(8) . . ?
W4C O4C Ti2C 120.8(8) . . ?
Si1B O25B W6B 125.1(8) . . ?
Si1B O25B W3B 123.3(8) . . ?
W6B O25B W3B 92.5(6) . . ?
Si1B O25B Ti1B 128.1(9) . . ?
W6B O25B Ti1B 88.7(5) . . ?
W3B O25B Ti1B 87.8(5) . . ?
W9C O13C W3C 147.7(9) . . ?
Si1A O25A W3A 128.0(8) . . ?
Si1A O25A W6A 124.0(8) . . ?
W3A O25A W6A 91.9(5) . . ?
Si1A O25A Ti1A 128.0(8) . . ?
W3A O25A Ti1A 86.8(5) . . ?
W6A O25A Ti1A 85.1(5) . . ?
W9B O13B W3B 146.3(9) . . ?
Ti2C O2C Ti1C 104.2(7) . . ?
Ti1B O2B Ti2B 103.5(7) . . ?
Ti2B O5B W5B 121.5(8) . . ?
W4D O9D W5D 119.8(8) . . ?
W9D O24D W12D 160.7(10) . . ?
Si1B O26B W4B 124.7(9) . . ?
Si1B O26B Ti2B 132.0(10) . . ?
W4B O26B Ti2B 86.8(6) . . ?
Si1B O26B W5B 124.3(9) . . ?
W4B O26B W5B 89.2(6) . . ?
Ti2B O26B W5B 86.5(5) . . ?
W11C O15C W5C 145.2(10) . . ?
W7D O7D W3D 144.4(9) . . ?
W7C O7C W3C 145.2(9) . . ?
Ti1A O101 Ti2B 157.5(10) . . ?
W3C O3C Ti1C 121.0(8) . . ?
W8C O10C W5C 146.6(9) . . ?
Ti1B O1B Ti2B 103.3(8) . . ?
Ti2D O2D Ti1D 103.9(7) . . ?
W8B O10B W5B 143.3(8) . . ?
W8D O24 W5D 144.7(9) . . ?
W11D O19D W8D 119.5(8) . . ?
Ti2A O5A W5A 122.7(9) . . ?
W8C O11C W6C 147.2(9) . . ?
W12A O16A W6A 150.1(9) . . ?
W7B O8B W4B 142.6(10) . . ?
Ti2D O301 Ti1C 158.8(10) . . ?
Ti1A O2A Ti2A 100.8(7) . . ?
Ti1C O1C Ti2C 102.0(7) . . ?
W8B O19B W11B 120.2(9) . . ?
W10B O18B W7B 119.1(9) . . ?
Si2C O25C W3C 125.8(8) . . ?
Si2C O25C Ti1C 131.3(9) . . ?
W3C O25C Ti1C 86.5(5) . . ?
Si2C O25C W6C 124.3(8) . . ?
W3C O25C W6C 89.5(5) . . ?
Ti1C O25C W6C 86.2(5) . . ?
W3A O12A W6A 119.0(8) . . ?
W10C O22C W11C 158.4(9) . . ?
Ti1D O6D W6D 119.8(8) . . ?
W11B O23B W12B 122.1(8) . . ?
W3D O3D Ti1D 116.9(8) . . ?
W10C O14C W4C 145.8(9) . . ?
W6C O6C Ti1C 120.6(8) . . ?
W12C O16C W6C 146.2(9) . . ?
W4A O4A Ti2A 119.5(8) . . ?
Si2D O27D W7D 123.8(8) . . ?
Si2D O27D W10D 125.7(8) . . ?
W7D O27D W10D 90.8(5) . . ?
Si2D O27D W9D 124.4(8) . . ?
W7D O27D W9D 90.8(5) . . ?
W10D O27D W9D 90.9(5) . . ?
W7A O8A W4A 149.3(10) . . ?
Ti2A O1A Ti1A 106.3(8) . . ?
W12C O24C W9C 154.6(11) . . ?
W8A O11A W6A 146.7(9) . . ?
Ti2D O1D Ti1D 102.8(8) . . ?
W8A O10A W5A 147.3(9) . . ?
Ti2B O4B W4B 120.6(9) . . ?
W12C O20C W8C 119.7(8) . . ?
W6B O16B W12B 144.1(9) . . ?
Si1A O28A W11A 124.5(8) . . ?
Si1A O28A W12A 126.3(8) . . ?
W11A O28A W12A 92.8(5) . . ?
Si1A O28A W8A 122.3(8) . . ?
W11A O28A W8A 90.3(5) . . ?
W12A O28A W8A 90.4(5) . . ?
W3D O12D W6D 121.4(9) . . ?
Ti2A O201 Ti1B 159.6(13) . . ?
Ti2C O5C W5C 122.0(8) . . ?
Ti2C O401 Ti1D 157.6(11) . . ?
W10D O22D W11D 159.4(9) . . ?
W12B O24B W9B 159.7(10) . . ?
W7D O8D W4D 142.0(9) . . ?
W3A O3A Ti1A 121.2(8) . . ?
W10B O21B W9B 123.7(9) . . ?
Si2D O25D W6D 124.3(8) . . ?
Si2D O25D W3D 122.8(8) . . ?
W6D O25D W3D 91.1(5) . . ?
Si2D O25D Ti1D 131.1(9) . . ?
W6D O25D Ti1D 88.0(5) . . ?
W3D O25D Ti1D 87.4(5) . . ?
W12C O23C W11C 119.5(8) . . ?
Si1B O28B W12B 126.7(9) . . ?
Si1B O28B W11B 125.8(9) . . ?
W12B O28B W11B 91.2(6) . . ?
Si1B O28B W8B 123.7(8) . . ?
W12B O28B W8B 89.4(6) . . ?
W11B O28B W8B 88.5(5) . . ?
Si1A O27A W9A 125.3(8) . . ?
Si1A O27A W10A 125.2(9) . . ?
W9A O27A W10A 93.0(6) . . ?
Si1A O27A W7A 122.1(8) . . ?
W9A O27A W7A 90.6(6) . . ?
W10A O27A W7A 90.5(5) . . ?
W8B O11B W6B 140.2(9) . . ?
W6B O6B Ti1B 118.5(8) . . ?
Si2C O26C W4C 125.7(9) . . ?
Si2C O26C W5C 124.6(9) . . ?
W4C O26C W5C 92.0(6) . . ?
Si2C O26C Ti2C 129.3(9) . . ?
W4C O26C Ti2C 86.6(5) . . ?
W5C O26C Ti2C 86.0(5) . . ?
Si2D O26D W4D 125.3(8) . . ?
Si2D O26D Ti2D 128.5(8) . . ?
W4D O26D Ti2D 89.5(5) . . ?
Si2D O26D W5D 122.7(8) . . ?
W4D O26D W5D 91.3(5) . . ?
Ti2D O26D W5D 88.2(5) . . ?
W9A O13A W3A 147.6(10) . . ?
W12A O20A W8A 120.7(8) . . ?
Ti2D O4D W4D 117.5(9) . . ?
W9C O17C W7C 118.1(9) . . ?
Si2D O28D W8D 124.0(8) . . ?
Si2D O28D W11D 128.7(8) . . ?
W8D O28D W11D 89.7(5) . . ?
Si2D O28D W12D 123.9(8) . . ?
W8D O28D W12D 89.0(5) . . ?
W11D O28D W12D 90.0(5) . . ?
W7A O7A W3A 146.3(9) . . ?
W4B O14B W10B 145.7(10) . . ?
W7B O7B W3B 141.2(8) . . ?
W10A O22A W11A 157.1(9) . . ?
Si1A O26A W5A 126.3(9) . . ?
Si1A O26A W4A 124.7(9) . . ?
W5A O26A W4A 89.5(5) . . ?
Si1A O26A Ti2A 131.8(9) . . ?
W5A O26A Ti2A 85.5(5) . . ?
W4A O26A Ti2A 85.1(5) . . ?
W8D O11D W6D 143.9(9) . . ?
W11C O19C W8C 120.0(9) . . ?
W10A O14A W4A 144.0(9) . . ?
W5B O15B W11B 148.1(9) . . ?
W10A O21A W9A 119.1(9) . . ?
W7C O8C W4C 146.6(8) . . ?
W12D O16D W6D 147.3(10) . . ?
Si1B O27B W7B 125.5(9) . . ?
Si1B O27B W10B 124.9(8) . . ?
W7B O27B W10B 91.0(5) . . ?
Si1B O27B W9B 125.2(8) . . ?
W7B O27B W9B 90.1(5) . . ?
W10B O27B W9B 89.2(5) . . ?
W9D O13D W3D 146.9(9) . . ?
W5D O15D W11D 146.1(9) . . ?
W12A O23A W11A 119.5(8) . . ?
W8B O20B W12B 118.4(9) . . ?
W4D O14D W10D 147.0(10) . . ?
W8D O20D W12D 118.6(9) . . ?
W10D O21D W9D 120.8(9) . . ?
W7A O17A W9A 119.4(9) . . ?
W12D O23D W11D 123.7(9) . . ?
W10B O22B W11B 159.6(9) . . ?
W10A O18A W7A 116.3(8) . . ?
W11A O15A W5A 144.3(9) . . ?
W10C O18C W7C 115.6(9) . . ?
Si2C O27C W10C 127.6(9) . . ?
Si2C O27C W7C 121.7(8) . . ?
W10C O27C W7C 91.6(6) . . ?
Si2C O27C W9C 123.6(8) . . ?
W10C O27C W9C 92.8(6) . . ?
W7C O27C W9C 89.3(5) . . ?
W10C O21C W9C 117.0(9) . . ?
W4B O9B W5B 123.0(9) . . ?
W7D O17D W9D 117.9(8) . . ?
Si2C O28C W11C 126.0(8) . . ?
Si2C O28C W12C 126.1(9) . . ?
W11C O28C W12C 92.3(5) . . ?
Si2C O28C W8C 122.2(8) . . ?
W11C O28C W8C 89.7(5) . . ?
W12C O28C W8C 89.7(5) . . ?
W9B O17B W7B 119.5(9) . . ?
W7D O18D W10D 119.5(10) . . ?
W11A O19A W8A 117.1(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N901 C902 1.14(4) . ?
C901 C902 1.49(5) . ?
N2B C255 1.1665 . ?
N2B C256 1.2702 . ?
N2B C275 1.5439 . ?
N2B C263 1.7119 . ?
N20B C263 1.0832 . ?
N20B C271 1.1869 . ?
N20B C259 1.5244 . ?
N20B C284 1.7238 . ?
N20B C255 1.8102 . ?
N20B C283 1.8726 . ?
C251 C252 0.8634 . ?
C251 C271 1.663 . ?
C271 C252 1.1815 . ?
C271 C263 1.9253 . ?
C271 C255 1.9429 . ?
C252 C272 1.7343 . ?
C252 C253 1.8867 . ?
C272 C253 1.0318 . ?
C275 C257 1.9697 . ?
C255 C276 1.4475 . ?
C255 C263 1.4612 . ?
C255 C256 1.9049 . ?
C256 C257 1.8001 . ?
C259 C260 1.6605 . ?
C259 C263 2.016 . ?
C260 C261 1.8848 . ?
C283 C284 0.7745 . ?
C263 C264 1.5288 . ?
C264 C265 1.4837 . ?
N3B C351 1.0259 . ?
N3B N30B 1.4812 . ?
N3B C355 1.717 . ?
N3B C363 1.9 . ?
N3B C359 1.9405 . ?
N30B C363 1.156 . ?
N30B C364 1.8467 . ?
N30B C383 1.9533 . ?
C351 C352 1.1778 . ?
C351 C355 1.7232 . ?
C351 C359 1.8346 . ?
C351 C372 1.9932 . ?
C372 C373 1.2266 . ?
C372 C352 1.5245 . ?
C372 C374 1.6686 . ?
C352 C373 1.4761 . ?
C353 C374 1.3271 . ?
C353 C354 1.4217 . ?
C353 C373 1.5605 . ?
C373 C374 0.86 . ?
C355 C375 1.2936 . ?
C375 C356 1.8712 . ?
C356 C357 1.564 . ?
C363 C364 1.167 . ?
C363 C383 1.5372 . ?
C383 C364 1.2727 . ?
C383 C384 1.3382 . ?
C383 C365 1.5984 . ?
C364 C365 1.0766 . ?
C364 C384 1.666 . ?
C384 C365 1.0135 . ?
W8C O308 1.693(19) . ?
W8C O11C 1.873(16) . ?
W8C O10C 1.899(16) . ?
W8C O19C 1.917(18) . ?
W8C O20C 1.945(16) . ?
W8C O28C 2.372(15) . ?
W4D O404 1.689(19) . ?
W4D O14D 1.842(17) . ?
W4D O9D 1.873(15) . ?
W4D O4D 1.905(17) . ?
W4D O8D 2.008(16) . ?
W4D O26D 2.282(16) . ?
W4D Ti2D 3.236(4) . ?
W5B O205 1.677(18) . ?
W5B O9B 1.893(17) . ?
W5B O5B 1.896(15) . ?
W5B O15B 1.902(15) . ?
W5B O10B 1.946(15) . ?
W5B O26B 2.395(16) . ?
W5B Ti2B 3.271(5) . ?
W8A O108 1.691(17) . ?
W8A O11A 1.874(15) . ?
W8A O10A 1.907(15) . ?
W8A O20A 1.960(16) . ?
W8A O19A 1.964(17) . ?
W8A O28A 2.350(14) . ?
W11D O411 1.656(19) . ?
W11D O19D 1.847(16) . ?
W11D O23D 1.909(18) . ?
W11D O15D 1.933(16) . ?
W11D O22D 1.971(16) . ?
W11D O28D 2.354(15) . ?
W12A O112 1.714(18) . ?
W12A O16A 1.847(15) . ?
W12A O20A 1.854(16) . ?
W12A O23A 1.942(17) . ?
W12A O24A 1.963(16) . ?
W12A O28A 2.322(14) . ?
W5A O105 1.713(18) . ?
W5A O5A 1.835(16) . ?
W5A O10A 1.925(15) . ?
W5A O15A 1.967(16) . ?
W5A O9A 1.976(15) . ?
W5A O26A 2.343(16) . ?
W5A Ti2A 3.212(5) . ?
W12C O312 1.719(19) . ?
W12C O16C 1.836(16) . ?
W12C O20C 1.897(16) . ?
W12C O24C 1.913(19) . ?
W12C O23C 1.914(17) . ?
W12C O28C 2.337(15) . ?
W6B O206 1.713(18) . ?
W6B O6B 1.877(16) . ?
W6B O16B 1.883(16) . ?
W6B O11B 1.950(16) . ?
W6B O12B 1.967(16) . ?
W6B O25B 2.289(16) . ?
W6B Ti1B 3.252(5) . ?
W3C O303 1.746(19) . ?
W3C O3C 1.828(15) . ?
W3C O12C 1.878(16) . ?
W3C O13C 1.957(16) . ?
W3C O7C 1.995(15) . ?
W3C O25C 2.336(16) . ?
W3C Ti1C 3.214(5) . ?
W5D O405 1.705(17) . ?
W5D O5D 1.877(16) . ?
W5D O15D 1.877(16) . ?
W5D O24 1.962(16) . ?
W5D O9D 1.975(15) . ?
W5D O26D 2.374(15) . ?
W5D Ti2D 3.263(4) . ?
W4C O304 1.753(18) . ?
W4C O4C 1.850(16) . ?
W4C O9C 1.872(16) . ?
W4C O14C 1.927(15) . ?
W4C O8C 1.962(15) . ?
W4C O26C 2.299(16) . ?
W4C Ti2C 3.235(5) . ?
W6C O306 1.690(18) . ?
W6C O6C 1.852(15) . ?
W6C O12C 1.927(16) . ?
W6C O11C 1.938(16) . ?
W6C O16C 1.978(16) . ?
W6C O25C 2.387(15) . ?
W6C Ti1C 3.239(4) . ?
W10D O410 1.707(16) . ?
W10D O22D 1.834(16) . ?
W10D O21D 1.919(18) . ?
W10D O18D 1.956(19) . ?
W10D O14D 1.982(17) . ?
W10D O27D 2.339(15) . ?
W3D O403 1.74(2) . ?
W3D O12D 1.884(18) . ?
W3D O3D 1.893(16) . ?
W3D O13D 1.915(16) . ?
W3D O7D 1.949(17) . ?
W3D O25D 2.345(15) . ?
W3D Ti1D 3.253(5) . ?
W9D O409 1.737(18) . ?
W9D O24D 1.814(17) . ?
W9D O13D 1.893(16) . ?
W9D O21D 1.927(18) . ?
W9D O17D 1.949(16) . ?
W9D O27D 2.354(15) . ?
W7D O407 1.748(18) . ?
W7D O8D 1.867(16) . ?
W7D O18D 1.872(19) . ?
W7D O7D 1.913(17) . ?
W7D O17D 1.923(15) . ?
W7D O27D 2.304(15) . ?
W10A O110 1.69(2) . ?
W10A O22A 1.896(16) . ?
W10A O14A 1.907(16) . ?
W10A O21A 1.934(17) . ?
W10A O18A 1.950(16) . ?
W10A O27A 2.327(15) . ?
W9C O309 1.686(19) . ?
W9C O13C 1.855(16) . ?
W9C O17C 1.902(16) . ?
W9C O24C 1.922(19) . ?
W9C O21C 1.979(18) . ?
W9C O27C 2.363(16) . ?
W4A O104 1.727(18) . ?
W4A O4A 1.829(15) . ?
W4A O9A 1.868(15) . ?
W4A O14A 1.938(16) . ?
W4A O8A 1.950(17) . ?
W4A O26A 2.374(15) . ?
W4A Ti2A 3.220(5) . ?
W5C O305 1.664(18) . ?
W5C O5C 1.859(15) . ?
W5C O10C 1.935(16) . ?
W5C O15C 1.936(17) . ?
W5C O9C 1.943(15) . ?
W5C O26C 2.323(16) . ?
W5C Ti2C 3.234(4) . ?
W3B O203 1.770(19) . ?
W3B O3B 1.916(16) . ?
W3B O12B 1.919(17) . ?
W3B O13B 1.919(16) . ?
W3B O7B 1.993(16) . ?
W3B O25B 2.318(15) . ?
W3B Ti1B 3.244(5) . ?
W3A O103 1.679(18) . ?
W3A O3A 1.795(15) . ?
W3A O12A 1.893(15) . ?
W3A O7A 1.966(17) . ?
W3A O13A 1.987(17) . ?
W3A O25A 2.267(15) . ?
W3A Ti1A 3.222(5) . ?
W6A O106 1.718(16) . ?
W6A O6A 1.867(15) . ?
W6A O16A 1.940(15) . ?
W6A O12A 1.963(15) . ?
W6A O11A 1.966(16) . ?
W6A O25A 2.357(14) . ?
W6A Ti1A 3.232(4) . ?
W12B O212 1.647(17) . ?
W12B O24B 1.896(17) . ?
W12B O20B 1.931(17) . ?
W12B O23B 1.938(16) . ?
W12B O16B 1.961(16) . ?
W12B O28B 2.338(16) . ?
W12D O412 1.720(18) . ?
W12D O23D 1.888(18) . ?
W12D O16D 1.913(17) . ?
W12D O20D 1.936(17) . ?
W12D O24D 1.976(17) . ?
W12D O28D 2.383(15) . ?
W11A O111 1.711(18) . ?
W11A O15A 1.880(16) . ?
W11A O19A 1.917(17) . ?
W11A O22A 1.917(16) . ?
W11A O23A 1.948(17) . ?
W11A O28A 2.319(14) . ?
W8B O208 1.740(19) . ?
W8B O19B 1.877(17) . ?
W8B O20B 1.928(18) . ?
W8B O10B 1.932(15) . ?
W8B O11B 1.947(17) . ?
W8B O28B 2.373(16) . ?
W10B O210 1.663(18) . ?
W10B O21B 1.883(17) . ?
W10B O22B 1.894(16) . ?
W10B O18B 1.905(17) . ?
W10B O14B 1.933(18) . ?
W10B O27B 2.367(15) . ?
W6D O406 1.64(2) . ?
W6D O16D 1.918(17) . ?
W6D O12D 1.934(17) . ?
W6D O6D 1.940(16) . ?
W6D O11D 1.967(16) . ?
W6D O25D 2.318(16) . ?
W6D Ti1D 3.251(5) . ?
W11C O311 1.712(18) . ?
W11C O19C 1.894(18) . ?
W11C O22C 1.909(15) . ?
W11C O15C 1.910(17) . ?
W11C O23C 1.961(16) . ?
W11C O28C 2.306(16) . ?
W9B O209 1.713(18) . ?
W9B O24B 1.904(17) . ?
W9B O13B 1.908(16) . ?
W9B O17B 1.910(19) . ?
W9B O21B 1.915(17) . ?
W9B O27B 2.403(15) . ?
W7A O107 1.74(2) . ?
W7A O8A 1.843(17) . ?
W7A O7A 1.872(17) . ?
W7A O17A 1.907(18) . ?
W7A O18A 1.956(16) . ?
W7A O27A 2.344(15) . ?
W7C O307 1.74(2) . ?
W7C O7C 1.859(15) . ?
W7C O8C 1.880(15) . ?
W7C O17C 1.962(17) . ?
W7C O18C 1.975(17) . ?
W7C O27C 2.355(15) . ?
W8D O408 1.697(18) . ?
W8D O11D 1.887(17) . ?
W8D O24 1.907(16) . ?
W8D O20D 1.915(17) . ?
W8D O19D 1.987(16) . ?
W8D O28D 2.343(15) . ?
W11B O211 1.648(18) . ?
W11B O23B 1.901(16) . ?
W11B O22B 1.904(15) . ?
W11B O15B 1.905(16) . ?
W11B O19B 1.935(17) . ?
W11B O28B 2.362(16) . ?
W4B O204 1.722(19) . ?
W4B O9B 1.892(16) . ?
W4B O14B 1.903(18) . ?
W4B O4B 1.909(17) . ?
W4B O8B 1.965(17) . ?
W4B O26B 2.343(17) . ?
W4B Ti2B 3.244(5) . ?
W9A O109 1.72(2) . ?
W9A O13A 1.824(17) . ?
W9A O24A 1.860(16) . ?
W9A O17A 1.915(17) . ?
W9A O21A 1.957(17) . ?
W9A O27A 2.297(16) . ?
W10C O310 1.78(2) . ?
W10C O22C 1.900(15) . ?
W10C O14C 1.909(16) . ?
W10C O18C 1.935(17) . ?
W10C O21C 1.949(18) . ?
W10C O27C 2.261(16) . ?
W7B O207 1.73(2) . ?
W7B O8B 1.902(17) . ?
W7B O7B 1.909(15) . ?
W7B O17B 1.920(19) . ?
W7B O18B 1.932(17) . ?
W7B O27B 2.272(15) . ?
Ti2B O101 1.797(16) . ?
Ti2B O4B 1.826(18) . ?
Ti2B O5B 1.852(16) . ?
Ti2B O2B 1.999(16) . ?
Ti2B O1B 2.035(17) . ?
Ti2B O26B 2.378(17) . ?
Ti2B Ti1B 3.140(7) . ?
Ti2C O401 1.772(18) . ?
Ti2C O5C 1.839(16) . ?
Ti2C O4C 1.871(16) . ?
Ti2C O2C 1.988(17) . ?
Ti2C O1C 2.028(16) . ?
Ti2C O26C 2.417(16) . ?
Ti2C Ti1C 3.138(6) . ?
Ti1D O6D 1.816(17) . ?
Ti1D O401 1.819(18) . ?
Ti1D O3D 1.924(16) . ?
Ti1D O2D 2.012(15) . ?
Ti1D O1D 2.044(18) . ?
Ti1D O25D 2.362(16) . ?
Ti1D Ti2D 3.152(6) . ?
Ti1C O301 1.798(17) . ?
Ti1C O3C 1.865(16) . ?
Ti1C O6C 1.877(16) . ?
Ti1C O2C 1.990(17) . ?
Ti1C O1C 2.009(15) . ?
Ti1C O25C 2.356(15) . ?
Ti2D O301 1.788(17) . ?
Ti2D O4D 1.879(18) . ?
Ti2D O5D 1.881(17) . ?
Ti2D O1D 1.990(18) . ?
Ti2D O2D 1.991(16) . ?
Ti2D O26D 2.314(15) . ?
Ti1B O201 1.780(19) . ?
Ti1B O3B 1.846(17) . ?
Ti1B O6B 1.907(17) . ?
Ti1B O1B 1.968(18) . ?
Ti1B O2B 1.999(16) . ?
Ti1B O25B 2.362(16) . ?
Ti1A O101 1.790(16) . ?
Ti1A O6A 1.851(15) . ?
Ti1A O3A 1.904(16) . ?
Ti1A O1A 1.965(17) . ?
Ti1A O2A 2.011(18) . ?
Ti1A O25A 2.420(15) . ?
Ti1A Ti2A 3.145(6) . ?
Ti2A O201 1.779(19) . ?
Ti2A O5A 1.826(16) . ?
Ti2A O4A 1.899(16) . ?
Ti2A O1A 1.965(18) . ?
Ti2A O2A 2.070(17) . ?
Ti2A O26A 2.390(16) . ?
N4A C413 1.4671 . ?
N4A C401 1.5107 . ?
N4A C409 1.5456 . ?
N4A C405 1.5747 . ?
C401 C402 1.6183 . ?
C402 C403 1.62 . ?
C403 C404 1.5165 . ?
C405 C406 1.4098 . ?
C406 C407 1.6981 . ?
C407 C408 1.4009 . ?
C409 C410 1.5466 . ?
C410 C411 1.56 . ?
C411 C412 1.5339 . ?
C413 C414 1.6524 . ?
C414 C415 1.4804 . ?
C415 C416 1.5152 . ?
N1A C109 1.4847 . ?
N1A C105 1.5113 . ?
N1A C101 1.5584 . ?
N1A C113 1.5611 . ?
C101 C102 1.558 . ?
C102 C103 1.6616 . ?
C103 C104 1.5174 . ?
C105 C106 1.5743 . ?
C106 C107 1.5405 . ?
C106 C128 1.6498 . ?
C107 C128 0.5211 . ?
C107 C108 1.7369 . ?
C128 C108 1.2303 . ?
C109 C110 1.6697 . ?
C110 C111 1.6281 . ?
C111 C112 1.4599 . ?
C113 C114 1.5508 . ?
C114 C115 1.5451 . ?
C115 C116 1.628 . ?
N5A C501 1.471 . ?
N5A C509 1.4958 . ?
N5A C513 1.5142 . ?
N5A C505 1.5576 . ?
C501 C502 1.5928 . ?
C502 C503 1.5682 . ?
C503 C504 1.502 . ?
C505 C506 1.62 . ?
C506 C527 1.5008 . ?
C507 C527 1.5629 . ?
C527 C508 1.5626 . ?
C509 C510 1.499 . ?
C510 C511 1.4785 . ?
C511 C512 1.5889 . ?
C513 C514 1.5919 . ?
C514 C515 1.7069 . ?
C515 C516 1.45 . ?
N3A C301 1.4612 . ?
N3A C313 1.4767 . ?
N3A C305 1.4969 . ?
N3A C309 1.5616 . ?
C301 C302 1.6321 . ?
C302 C303 1.5859 . ?
C303 C304 1.6539 . ?
C305 C306 1.5597 . ?
C306 C307 1.4805 . ?
C307 C308 1.6178 . ?
C309 C310 1.6575 . ?
C310 C311 1.4615 . ?
C311 C312 1.6587 . ?
C313 C314 1.6103 . ?
C314 C315 1.6791 . ?
C315 C316 1.6479 . ?
N6A C605 1.4501 . ?
N6A C609 1.5271 . ?
N6A C601 1.5415 . ?
N6A C613 1.6089 . ?
C601 C602 1.5419 . ?
C602 C603 1.5393 . ?
C603 C604 1.4824 . ?
C605 C606 1.5718 . ?
C606 C607 1.5279 . ?
C607 C608 1.6577 . ?
C609 C610 1.6147 . ?
C610 C611 1.5399 . ?
C611 C632 1.4889 . ?
C611 C612 1.5874 . ?
C613 C614 1.474 . ?
C614 C615 1.51 . ?
C615 C616 1.2199 . ?
N7A C713 1.4789 . ?
N7A C709 1.5815 . ?
N7A C701 1.61 . ?
N7A C705 1.6524 . ?
C701 C702 1.5671 . ?
C702 C703 1.4164 . ?
C703 C704 1.571 . ?
C705 C706 1.6253 . ?
C706 C707 1.5385 . ?
C707 C708 1.57 . ?
C708 C728 1.2377 . ?
C709 C710 1.3405 . ?
C710 C711 1.5433 . ?
C711 C732 1.3451 . ?
C711 C712 1.6134 . ?
C713 C714 1.3539 . ?
C713 C734 1.7336 . ?
C714 C734 1.0633 . ?
C714 C715 1.8569 . ?
C734 C715 1.5088 . ?
C715 C716 1.532 . ?
N8A C801 1.4767 . ?
N8A C805 1.5136 . ?
N8A C809 1.5674 . ?
N8A C813 1.6027 . ?
C801 C802 1.5508 . ?
C802 C823 1.6181 . ?
C804 C823 1.3245 . ?
C804 C803 1.5489 . ?
C805 C806 1.35 . ?
C806 C807 1.7935 . ?
C807 C808 1.2601 . ?
C809 C810 1.4401 . ?
C810 C811 1.5434 . ?
C811 C812 1.5213 . ?
C813 C834 1.561 . ?
C814 C834 1.2664 . ?
C834 C815 1.5916 . ?
C815 C816 1.3758 . ?
N2A C201 1.3982 . ?
N2A C213 1.5342 . ?
N2A C205 1.5529 . ?
N2A C209 1.5775 . ?
C201 C202 1.5271 . ?
C202 C203 1.6083 . ?
C203 C204 1.4451 . ?
C205 C206 1.5029 . ?
C206 C207 1.5345 . ?
C207 C208 1.5702 . ?
C209 C210 1.5298 . ?
C210 C211 1.5993 . ?
C211 C212 1.6644 . ?
C213 C214 1.7761 . ?
C214 C236 1.241 . ?
C214 C215 1.3502 . ?
C215 C216 1.5031 . ?
C215 C236 1.6295 . ?
N1B C163 1.4601 . ?
N1B C155 1.4821 . ?
N1B C159 1.5418 . ?
N1B C151 1.6371 . ?
C151 C152 1.6042 . ?
C152 C153 1.6967 . ?
C153 C154 1.5917 . ?
C155 C156 1.6082 . ?
C156 C157 1.6052 . ?
C156 C178 1.8083 . ?
C157 C178 1.1116 . ?
C157 C158 1.6059 . ?
C157 C177 1.8156 . ?
C177 C178 1.1294 . ?
C158 C178 1.7729 . ?
C159 C160 1.765 . ?
C160 C161 1.3377 . ?
C161 C162 1.3972 . ?
C163 C164 1.2768 . ?
C164 C165 1.4403 . ?
C165 C166 1.1324 . ?
C165 C186 1.1876 . ?
C166 C186 1.0754 . ?
N7B C759 1.2685 . ?
N7B C751 1.5879 . ?
N7B C755 1.5932 . ?
N7B C763 1.8489 . ?
C751 C752 1.5109 . ?
C752 C753 1.2091 . ?
C753 C754 1.5434 . ?
C755 C756 1.5691 . ?
C756 C757 1.0799 . ?
C756 C777 1.6252 . ?
C756 C778 1.9779 . ?
C757 C778 1.0245 . ?
C757 C777 1.1731 . ?
C757 C758 1.8001 . ?
C777 C778 1.0325 . ?
C777 C758 1.8495 . ?
C758 C778 1.3294 . ?
C759 C760 1.7487 . ?
C763 C764 1.3045 . ?
C764 C765 1.6089 . ?
C765 C766 1.5188 . ?
N6B C651 1.4689 . ?
N6B C655 1.5052 . ?
N6B C659 1.5277 . ?
N6B C663 1.6246 . ?
C651 C652 1.3351 . ?
C652 C653 1.8023 . ?
C655 C656 1.495 . ?
C656 C657 1.5069 . ?
C657 C658 1.7395 . ?
C659 C660 1.4957 . ?
C660 C661 1.4642 . ?
C661 C662 1.4107 . ?
C663 C664 1.4796 . ?
C664 C665 1.5456 . ?
C665 C666 1.6373 . ?
N5B C555 1.4462 . ?
N5B C559 1.5443 . ?
N5B C551 1.5536 . ?
N5B C563 1.8397 . ?
C551 C552 1.7741 . ?
C552 C553 1.565 . ?
C553 C554 1.7729 . ?
C555 C556 1.809 . ?
C556 C557 1.5827 . ?
C557 C558 1.399 . ?
C559 C561 1.2027 . ?
C559 C560 1.3237 . ?
C560 C561 1.1646 . ?
C560 C580 1.6403 . ?
C560 C562 1.6531 . ?
C580 C561 1.1186 . ?
C580 C581 1.4201 . ?
C580 C562 1.7945 . ?
C561 C562 1.9187 . ?
C563 C564 1.3457 . ?
C563 C568 1.6992 . ?
C564 C568 1.38 . ?
C564 C565 1.5932 . ?
C568 C565 1.5229 . ?
C568 C585 1.5259 . ?
C568 C586 2.001 . ?
C565 C586 1.3053 . ?
C565 C585 1.3793 . ?
C565 C566 1.9253 . ?
C585 C566 0.9923 . ?
C585 C586 1.1855 . ?
C566 C586 0.9263 . ?
N8B C851 1.501 . ?
N8B C855 1.5042 . ?
N8B C863 1.6126 . ?
N8B C859 1.7084 . ?
C851 C852 1.6467 . ?
C852 C853 1.5853 . ?
C853 C854 1.3043 . ?
C855 C856 1.3425 . ?
C856 C857 1.4881 . ?
C857 C858 1.4593 . ?
C859 C860 1.372 . ?
C860 C861 1.5761 . ?
C863 C864 1.457 . ?
C864 C865 1.6326 . ?
C864 C885 1.7183 . ?
C865 C885 1.578 . ?
C885 C866 1.595 . ?
N4B C455 1.4204 . ?
N4B C459 1.5284 . ?
N4B C463 1.6012 . ?
N4B C451 1.6122 . ?
C451 C452 1.4913 . ?
C452 C453 1.5633 . ?
C453 C454 1.497 . ?
C455 C476 1.827 . ?
C456 C476 1.4556 . ?
C456 C477 1.6121 . ?
C457 C477 1.4881 . ?
C459 C481 1.6078 . ?
C459 C460 1.6447 . ?
C460 C461 1.1692 . ?
C460 C481 1.1998 . ?
C461 C481 1.6944 . ?
C463 C464 1.5197 . ?
C464 C465 1.487 . ?
C465 C466 1.2673 . ?
Si1A O26A 1.566(17) . ?
Si1A O25A 1.642(16) . ?
Si1A O27A 1.664(17) . ?
Si1A O28A 1.667(15) . ?
Si2D O25D 1.620(17) . ?
Si2D O28D 1.648(16) . ?
Si2D O27D 1.651(16) . ?
Si2D O26D 1.683(16) . ?
Si2C O25C 1.620(17) . ?
Si2C O28C 1.634(16) . ?
Si2C O27C 1.645(17) . ?
Si2C O26C 1.646(17) . ?
Si1B O26B 1.571(17) . ?
Si1B O27B 1.635(16) . ?
Si1B O28B 1.657(17) . ?
Si1B O25B 1.670(17) . ?
|
1101220.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-16 14:49:56 +0200 (Wed, 16 Mar 2016) $
#$Revision: 178223 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101220.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_1101220
loop_
_publ_author_name
'Goto, Yuya'
'Kamata, Keigo'
'Yamaguchi, Kazuya'
'Uehara, Kazuhiro'
'Hikichi, Shiro'
'Mizuno, Noritaka'
_publ_section_title
;
Synthesis, Structural Characterization, and Catalytic Performance of
Dititanium-Substituted \g-Keggin Silicotungstate
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 2347
_journal_page_last 2356
_journal_paper_doi 10.1021/ic052179q
_journal_volume 45
_journal_year 2006
_chemical_formula_moiety 'C100 H212 K8 O128 S2 Si2 Ti4 W20 '
_chemical_formula_sum 'C100 H212 K8 O128 S2 Si2 Ti4 W20'
_chemical_formula_weight 7764.38
_space_group_IT_number 70
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-F 2uv 2vw'
_symmetry_space_group_name_H-M 'F d d d :2'
_cell_angle_alpha 90.0000
_cell_angle_beta 90.0000
_cell_angle_gamma 90.0000
_cell_formula_units_Z 16
_cell_length_a 33.2107(3)
_cell_length_b 35.4445(4)
_cell_length_c 85.0187(8)
_cell_measurement_temperature 296.1
_cell_volume 100078.6(17)
_computing_cell_refinement CrystalClear
_computing_data_collection CrystalClear
_computing_data_reduction CrystalStructure
_computing_publication_material 'CrystalStructure 3.7.0'
_computing_structure_refinement CRYSTALS
_computing_structure_solution SAPI91
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type 'Rigaku Saturn'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_limit_h_max 42
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 47
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 113
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 29407
_diffrn_reflns_theta_full 28.29
_diffrn_reflns_theta_max 28.29
_exptl_absorpt_coefficient_mu 9.523
_exptl_absorpt_correction_type none
_exptl_crystal_colour NONE
_exptl_crystal_density_diffrn 2.061
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description NONE
_exptl_crystal_F_000 57856.00
_exptl_crystal_size_max 0.00
_exptl_crystal_size_mid 0.00
_exptl_crystal_size_min 0.00
_refine_diff_density_max 3.50
_refine_diff_density_min -2.46
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 8.293
_refine_ls_number_parameters 696
_refine_ls_number_reflns 18443
_refine_ls_R_factor_gt 0.0546
_refine_ls_shift/su_max 1.0102
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1.0'
_refine_ls_weighting_scheme unit
_refine_ls_wR_factor_ref 0.0538
_reflns_number_gt 18331
_reflns_number_total 29407
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'F d d d'
_cod_original_formula_sum 'C100 H212 K8 O128 S2 Si2 Ti4 W20 '
_cod_database_code 1101220
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,1/4+Y,1/4+Z
3 1/4+X,-Y,1/4+Z
4 1/4-X,3/4-Y,1/2+Z
5 -X,-Y,-Z
6 +X,1/4-Y,1/4-Z
7 1/4-X,+Y,1/4-Z
8 1/4+X,3/4+Y,1/2-Z
9 +X,1/2+Y,1/2+Z
10 -X,3/4+Y,3/4+Z
11 1/4+X,1/2-Y,3/4+Z
12 1/4-X,1/4-Y,+Z
13 -X,1/2-Y,1/2-Z
14 +X,3/4-Y,3/4-Z
15 1/4-X,1/2+Y,3/4-Z
16 1/4+X,1/4+Y,-Z
17 1/2+X,+Y,1/2+Z
18 1/2-X,1/4+Y,3/4+Z
19 3/4+X,-Y,3/4+Z
20 3/4-X,3/4-Y,+Z
21 1/2-X,-Y,1/2-Z
22 1/2+X,1/4-Y,3/4-Z
23 3/4-X,+Y,3/4-Z
24 3/4+X,3/4+Y,-Z
25 1/2+X,1/2+Y,+Z
26 1/2-X,3/4+Y,1/4+Z
27 3/4+X,1/2-Y,1/4+Z
28 3/4-X,1/4-Y,1/2+Z
29 1/2-X,1/2-Y,-Z
30 1/2+X,3/4-Y,1/4-Z
31 3/4-X,1/2+Y,1/4-Z
32 3/4+X,1/4+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
W(3) W 0.40443(2) 0.21135(2) 0.078530(10) 0.04873(15) Uani 1.00 1 d . . .
W(4) W 0.40446(2) 0.04324(2) 0.077170(10) 0.04463(14) Uani 1.00 1 d . . .
W(5) W 0.30505(2) 0.04385(2) 0.073050(10) 0.04409(14) Uani 1.00 1 d . . .
W(6) W 0.30503(2) 0.21120(2) 0.074440(10) 0.04717(15) Uani 1.00 1 d . . .
W(7) W 0.46363(2) 0.12776(2) 0.067730(10) 0.04897(14) Uani 1.00 1 d . . .
W(8) W 0.25312(2) 0.12821(2) 0.058430(10) 0.04683(14) Uani 1.00 1 d . . .
W(9) W 0.42258(2) 0.17633(2) 0.038600(10) 0.05178(16) Uani 1.00 1 d . . .
W(10) W 0.42247(2) 0.08201(2) 0.037800(10) 0.04822(15) Uani 1.00 1 d . . .
W(11) W 0.31061(2) 0.08213(2) 0.033100(10) 0.04613(15) Uani 1.00 1 d . . .
W(12) W 0.31064(2) 0.17672(2) 0.033860(10) 0.04921(15) Uani 1.00 1 d . . .
Ti(1) Ti 0.34744(8) 0.17046(6) 0.10461(3) 0.0448(6) Uani 1.00 1 d . . .
Ti(2) Ti 0.34745(8) 0.08139(6) 0.10395(3) 0.0437(6) Uani 1.00 1 d . . .
K(1) K 0.6257(2) 0.2580(2) 0.20237(9) 0.0803(19) Uiso 0.54 1 d P . .
K(2) K 0.12541(19) 0.30662(16) 0.21142(6) 0.1085(15) Uiso 1.00 1 d . . .
K(3) K 0.3750 0.3750 0.22099(9) 0.1019(19) Uiso 1.00 2 d S . .
K(4) K 0.3750 0.3750 0.12755(10) 0.121(2) Uiso 1.00 2 d S . .
K(5) K 0.1250 0.0374(2) 0.1250 0.082(2) Uiso 0.63 2 d SP . .
K(6) K 0.3750 0.3750 0.02146(10) 0.112(2) Uiso 1.00 2 d S . .
K(11) K 0.6267(3) 0.2323(2) 0.20372(11) 0.079(2) Uiso 0.46 1 d P . .
K(55) K 0.1250 0.0770(6) 0.1250 0.111(5) Uiso 0.37 2 d SP . .
S(1) S 0.4643 0.0730 0.1250 0.102 Uiso 0.50 1 d R . .
S(11) S 0.5249 0.0756 0.1247 0.096 Uiso 0.50 1 d R . .
Si(1) Si 0.35821(11) 0.12802(11) 0.06546(4) 0.0425(9) Uani 1.00 1 d . . .
O(1) O 0.3830(2) 0.1257(2) 0.10587(9) 0.045(2) Uani 1.00 1 d . . .
O(2) O 0.3107(2) 0.1263(2) 0.10138(9) 0.045(2) Uani 1.00 1 d . . .
O(3) O 0.3903(2) 0.2020(2) 0.09982(10) 0.050(2) Uani 1.00 1 d . . .
O(4) O 0.3906(2) 0.0503(2) 0.09842(10) 0.043(2) Uani 1.00 1 d . . .
O(5) O 0.3079(2) 0.0504(2) 0.09504(10) 0.045(2) Uani 1.00 1 d . . .
O(6) O 0.3081(2) 0.2025(2) 0.09617(10) 0.048(2) Uani 1.00 1 d . . .
O(7) O 0.4397(2) 0.1677(2) 0.07918(10) 0.050(2) Uani 1.00 1 d . . .
O(8) O 0.4399(2) 0.0869(2) 0.07859(10) 0.047(2) Uani 1.00 1 d . . .
O(9) O 0.3549(2) 0.0164(2) 0.07401(10) 0.048(2) Uani 1.00 1 d . . .
O(10) O 0.2708(2) 0.0877(2) 0.07188(10) 0.045(2) Uani 1.00 1 d . . .
O(11) O 0.2710(2) 0.1674(2) 0.07236(10) 0.050(2) Uani 1.00 1 d . . .
O(12) O 0.3550(3) 0.2386(2) 0.07583(10) 0.053(2) Uani 1.00 1 d . . .
O(13) O 0.4073(2) 0.2073(2) 0.05606(11) 0.053(2) Uani 1.00 1 d . . .
O(14) O 0.4074(2) 0.0503(2) 0.05463(10) 0.049(2) Uani 1.00 1 d . . .
O(15) O 0.3153(2) 0.0500(2) 0.05088(10) 0.047(2) Uani 1.00 1 d . . .
O(16) O 0.3150(2) 0.2069(2) 0.05216(11) 0.053(2) Uani 1.00 1 d . . .
O(17) O 0.4688(3) 0.1638(2) 0.05069(11) 0.056(2) Uani 1.00 1 d . . .
O(18) O 0.4686(2) 0.0934(2) 0.05002(10) 0.051(2) Uani 1.00 1 d . . .
O(19) O 0.2577(2) 0.0932(2) 0.04113(10) 0.048(2) Uani 1.00 1 d . . .
O(20) O 0.2578(2) 0.1646(2) 0.04186(11) 0.053(2) Uani 1.00 1 d . . .
O(21) O 0.4303(2) 0.1298(2) 0.02744(10) 0.055(2) Uani 1.00 1 d . . .
O(22) O 0.3670(2) 0.0817(2) 0.03101(9) 0.046(2) Uani 1.00 1 d . . .
O(23) O 0.3080(2) 0.1297(2) 0.02264(10) 0.052(2) Uani 1.00 1 d . . .
O(24) O 0.3669(2) 0.1774(2) 0.03196(10) 0.051(2) Uani 1.00 1 d . . .
O(25) O 0.3551(2) 0.0894(2) 0.07608(9) 0.044(2) Uani 1.00 1 d . . .
O(26) O 0.3545(2) 0.1655(2) 0.07666(10) 0.045(2) Uani 1.00 1 d . . .
O(27) O 0.4005(2) 0.1281(2) 0.05577(9) 0.043(2) Uani 1.00 1 d . . .
O(28) O 0.3222(2) 0.1284(2) 0.05245(9) 0.044(2) Uani 1.00 1 d . . .
O(101) O 0.3413(2) 0.0709(2) 0.12462(10) 0.048(2) Uani 1.00 1 d . . .
O(103) O 0.4376(3) 0.2476(2) 0.08126(11) 0.059(3) Uani 1.00 1 d . . .
O(104) O 0.4375(3) 0.0064(2) 0.07931(11) 0.055(2) Uani 1.00 1 d . . .
O(105) O 0.2714(3) 0.0077(2) 0.07234(11) 0.056(2) Uani 1.00 1 d . . .
O(106) O 0.2717(3) 0.2476(2) 0.07426(12) 0.061(3) Uani 1.00 1 d . . .
O(107) O 0.5119(2) 0.1273(3) 0.07515(11) 0.062(3) Uani 1.00 1 d . . .
O(108) O 0.2020(2) 0.1279(2) 0.06136(11) 0.056(2) Uani 1.00 1 d . . .
O(109) O 0.4433(3) 0.2080(3) 0.02576(11) 0.064(3) Uani 1.00 1 d . . .
O(110) O 0.4436(3) 0.0516(3) 0.02436(11) 0.059(3) Uani 1.00 1 d . . .
O(111) O 0.2967(3) 0.0517(2) 0.01828(11) 0.056(2) Uani 1.00 1 d . . .
O(112) O 0.2976(3) 0.2083(3) 0.01953(11) 0.063(3) Uani 1.00 1 d . . .
O(201) O 0.7025 0.2385 0.2131 0.073 Uiso 0.50 1 d R . .
O(202) O 0.6848(5) 0.2460(5) 0.1801(2) 0.121(5) Uiso 1.00 1 d . . .
O(203) O 0.6051(6) 0.2295(5) 0.1714(2) 0.131(5) Uiso 1.00 1 d . . .
O(204) O 0.5476(4) 0.2442(4) 0.19407(19) 0.105(4) Uiso 1.00 1 d . . .
O(205) O 0.5686(5) 0.2449(4) 0.2259(2) 0.114(4) Uiso 1.00 1 d . . .
O(206) O 0.6488(6) 0.2622(5) 0.2333(2) 0.134(6) Uiso 1.00 1 d . . .
O(211) O 0.7141 0.2463 0.2076 0.095 Uiso 0.50 1 d R . .
O(301) O 0.1428(9) 0.2354(8) 0.1976(3) 0.190(9) Uiso 1.00 1 d . . .
O(302) O 0.0682(8) 0.2500(7) 0.2120(3) 0.176(8) Uiso 1.00 1 d . . .
O(303) O 0.0439(9) 0.3210(9) 0.2193(3) 0.204(10) Uiso 1.00 1 d . . .
O(304) O 0.1057(9) 0.3749(7) 0.2281(2) 0.175(8) Uiso 1.00 1 d . . .
O(305) O 0.1709(9) 0.3329(9) 0.2378(3) 0.191(9) Uiso 1.00 1 d . . .
O(306) O 0.1995(9) 0.2745(9) 0.2200(3) 0.196(10) Uiso 1.00 1 d . . .
O(401) O 0.4269(15) 0.3205(13) 0.2049(4) 0.260(15) Uiso 1.00 1 d . . .
O(402) O 0.3649(11) 0.2999(11) 0.2207(4) 0.240(13) Uiso 1.00 1 d . . .
O(403) O 0.2897(14) 0.3567(15) 0.2046(5) 0.302(18) Uiso 1.00 1 d . . .
O(501) O 0.3300(9) 0.3283(8) 0.1055(3) 0.223(8) Uiso 0.50 1 d P . .
O(502) O 0.3782(9) 0.3907(8) 0.0964(2) 0.223(8) Uiso 0.50 1 d P . .
O(503) O 0.3948(10) 0.4467(6) 0.1185(3) 0.223(8) Uiso 0.50 1 d P . .
O(504) O 0.3956(6) 0.4261(3) 0.1508(3) 0.223(8) Uiso 0.50 1 d P . .
O(505) O 0.3492(2) 0.3612(2) 0.1596(2) 0.223(8) Uiso 0.50 1 d P . .
O(506) O 0.3320(8) 0.3059(5) 0.1367(3) 0.223(8) Uiso 0.50 1 d P . .
O(601) O 0.1524(5) 0.0925(4) 0.1522(7) 0.43(2) Uiso 0.50 1 d P . .
O(602) O 0.2113(11) 0.0724(16) 0.1287(8) 0.43(2) Uiso 0.50 1 d P . .
O(603) O 0.191(2) 0.0157(19) 0.1061(7) 0.43(2) Uiso 0.50 1 d P . .
O(604) O 0.107(2) 0.006(2) 0.0982(6) 0.43(2) Uiso 0.50 1 d P . .
O(605) O 0.0464(17) 0.0281(18) 0.1211(8) 0.43(2) Uiso 0.50 1 d P . .
O(606) O 0.0695(6) 0.0846(10) 0.1447(7) 0.43(2) Uiso 0.50 1 d P . .
O(701) O 0.375000(10) 0.375000(10) -0.0191(8) 0.52(3) Uiso 1.00 2 d S . .
O(702) O 0.4135(19) 0.4267(15) -0.0011(11) 0.52(3) Uiso 0.50 1 d P . .
O(703) O 0.376(3) 0.454(2) 0.0267(11) 0.52(3) Uiso 0.50 1 d P . .
O(704) O 0.327(3) 0.402(3) 0.0435(8) 0.52(3) Uiso 0.50 1 d P . .
O(705) O 0.288(2) 0.343(3) 0.0259(11) 0.52(3) Uiso 0.50 1 d P . .
O(706) O 0.323(2) 0.3149(15) -0.0031(11) 0.52(3) Uiso 0.50 1 d P . .
O(901) O 0.4485 0.1250 0.1250 0.061 Uiso 1.00 2 d R . .
O(911) O 0.5578 0.0451 0.1247 0.094 Uiso 0.50 1 d R . .
C(201) C 0.7354(9) 0.2502(8) 0.1973(3) 0.129(8) Uiso 1.00 1 d . . .
C(202) C 0.7221(10) 0.2313(9) 0.1838(3) 0.138(10) Uiso 1.00 1 d . . .
C(203) C 0.6741(13) 0.2330(11) 0.1640(4) 0.179(13) Uiso 1.00 1 d . . .
C(204) C 0.6311(12) 0.2517(11) 0.1588(4) 0.169(12) Uiso 1.00 1 d . . .
C(205) C 0.5645(10) 0.2449(9) 0.1672(3) 0.143(10) Uiso 1.00 1 d . . .
C(206) C 0.5377(9) 0.2240(8) 0.1793(3) 0.131(9) Uiso 1.00 1 d . . .
C(207) C 0.5204(9) 0.2323(8) 0.2062(3) 0.130(9) Uiso 1.00 1 d . . .
C(208) C 0.5296(8) 0.2553(7) 0.2210(3) 0.109(7) Uiso 1.00 1 d . . .
C(209) C 0.5783(9) 0.2674(8) 0.2394(3) 0.128(9) Uiso 1.00 1 d . . .
C(210) C 0.6198(11) 0.2540(9) 0.2446(4) 0.150(10) Uiso 1.00 1 d . . .
C(211) C 0.6887(10) 0.2460(9) 0.2377(4) 0.143(10) Uiso 1.00 1 d . . .
C(212) C 0.7156(11) 0.2578(10) 0.2249(4) 0.152(11) Uiso 1.00 1 d . . .
C(301) C 0.1181(12) 0.2072(11) 0.2013(4) 0.160(11) Uiso 1.00 1 d . . .
C(302) C 0.0739(13) 0.2245(11) 0.1990(5) 0.177(13) Uiso 1.00 1 d . . .
C(303) C 0.0270(10) 0.2618(9) 0.2113(3) 0.137(9) Uiso 1.00 1 d . . .
C(304) C 0.0225(13) 0.2916(13) 0.2254(5) 0.180(14) Uiso 1.00 1 d . . .
C(305) C 0.043(2) 0.346(2) 0.2361(8) 0.29(2) Uiso 1.00 1 d . . .
C(306) C 0.069(2) 0.3808(19) 0.2299(7) 0.26(2) Uiso 1.00 1 d . . .
C(307) C 0.1267(8) 0.3795(7) 0.2432(2) 0.113(7) Uiso 1.00 1 d . . .
C(308) C 0.1654(14) 0.3723(15) 0.2370(5) 0.194(15) Uiso 1.00 1 d . . .
C(309) C 0.2105(17) 0.3196(16) 0.2372(5) 0.216(18) Uiso 1.00 1 d . . .
C(310) C 0.2106(13) 0.2809(14) 0.2356(5) 0.187(14) Uiso 1.00 1 d . . .
C(311) C 0.2062(19) 0.238(2) 0.2165(7) 0.24(2) Uiso 1.00 1 d . . .
C(312) C 0.1851(16) 0.2246(13) 0.2009(5) 0.204(16) Uiso 1.00 1 d . . .
C(401) C 0.4182(12) 0.2850(12) 0.2107(4) 0.164(12) Uiso 1.00 1 d . . .
C(402) C 0.3734(11) 0.2742(10) 0.2115(4) 0.146(10) Uiso 1.00 1 d . . .
C(403) C 0.3152(15) 0.2925(13) 0.2177(5) 0.195(15) Uiso 1.00 1 d . . .
C(404) C 0.3009(17) 0.3155(18) 0.2050(6) 0.225(19) Uiso 1.00 1 d . . .
C(405) C 0.3(9) 0(38) 0(30) 0.1(19) Uani 1.00 1 d . . .
C(406) C 0.465(2) 0.3359(17) 0.2037(6) 0.24(2) Uiso 1.00 1 d . . .
C(501) C 0.3495(11) 0.3299(8) 0.0905(3) 0.223(8) Uiso 0.50 1 d P . .
C(502) C 0.3525(10) 0.3699(9) 0.0858(2) 0.223(8) Uiso 0.50 1 d P . .
C(503) C 0.3827(11) 0.4298(8) 0.0917(3) 0.223(8) Uiso 0.50 1 d P . .
C(504) C 0.4110(11) 0.4477(8) 0.1027(3) 0.223(8) Uiso 0.50 1 d P . .
C(505) C 0.4187(11) 0.4660(6) 0.1299(3) 0.223(8) Uiso 0.50 1 d P . .
C(506) C 0.3971(10) 0.4647(3) 0.1450(3) 0.223(8) Uiso 0.50 1 d P . .
C(507) C 0.3755(5) 0.42361(6) 0.1653(3) 0.223(8) Uiso 0.50 1 d P . .
C(508) C 0.375000(10) 0.375000(10) 0.1704(2) 0.223(8) Uiso 1.00 2 d S . .
C(509) C 0.3474(5) 0.3222(2) 0.1635(3) 0.223(8) Uiso 0.50 1 d P . .
C(510) C 0.3191(8) 0.3026(5) 0.1526(3) 0.223(8) Uiso 0.50 1 d P . .
C(511) C 0.3047(10) 0.2896(8) 0.1260(3) 0.223(8) Uiso 0.50 1 d P . .
C(512) C 0.3235(12) 0.2894(7) 0.1102(3) 0.223(8) Uiso 0.50 1 d P . .
C(601) C 0.1924(3) 0.1101(10) 0.1512(8) 0.43(2) Uiso 0.50 1 d P . .
C(602) C 0.2227(7) 0.0827(15) 0.1447(9) 0.43(2) Uiso 0.50 1 d P . .
C(603) C 0.2417(15) 0.048(2) 0.1213(9) 0.43(2) Uiso 0.50 1 d P . .
C(604) C 0.227(2) 0.037(2) 0.1050(8) 0.43(2) Uiso 0.50 1 d P . .
C(605) C 0.177(2) -0.001(2) 0.0912(7) 0.43(2) Uiso 0.50 1 d P . .
C(606) C 0.137(2) -0.021(2) 0.0927(6) 0.43(2) Uiso 0.50 1 d P . .
C(607) C 0.067(2) -0.011(2) 0.0992(7) 0.43(2) Uiso 0.50 1 d P . .
C(608) C 0.037(2) 0.018(2) 0.1052(8) 0.43(2) Uiso 0.50 1 d P . .
C(609) C 0.0191(13) 0.057(2) 0.1279(9) 0.43(2) Uiso 0.50 1 d P . .
C(610) C 0.0303(9) 0.0662(16) 0.1445(9) 0.43(2) Uiso 0.50 1 d P . .
C(611) C 0.0835(5) 0.0974(6) 0.1603(7) 0.43(2) Uiso 0.50 1 d P . .
C(612) C 0.125000(10) 0.125000(10) 0.1592(8) 0.43(2) Uiso 1.00 2 d S . .
C(701) C 0.4151(2) 0.3786(11) -0.0227(10) 0.52(3) Uiso 0.50 1 d P . .
C(702) C 0.4197(14) 0.4206(12) -0.0180(11) 0.52(3) Uiso 0.50 1 d P . .
C(703) C 0.415(3) 0.4663(18) 0.0036(13) 0.52(3) Uiso 0.50 1 d P . .
C(704) C 0.415(3) 0.469(2) 0.0216(13) 0.52(3) Uiso 0.50 1 d P . .
C(705) C 0.375(4) 0.455(3) 0.0440(11) 0.52(3) Uiso 0.50 1 d P . .
C(706) C 0.334(4) 0.442(3) 0.0485(9) 0.52(3) Uiso 0.50 1 d P . .
C(707) C 0.288(3) 0.389(4) 0.0482(9) 0.52(3) Uiso 0.50 1 d P . .
C(708) C 0.285(3) 0.347(3) 0.0434(11) 0.52(3) Uiso 0.50 1 d P . .
C(709) C 0.282(3) 0.304(3) 0.0199(13) 0.52(3) Uiso 0.50 1 d P . .
C(710) C 0.283(2) 0.305(2) 0.0021(13) 0.52(3) Uiso 0.50 1 d P . .
C(711) C 0.3256(18) 0.3159(13) -0.0201(11) 0.52(3) Uiso 0.50 1 d P . .
C(712) C 0.3676(15) 0.3267(3) -0.0242(10) 0.52(3) Uiso 0.50 1 d P . .
C(901) C 0.4967(7) 0.0682(6) 0.1087(2) 0.099(6) Uiso 1.00 1 d . . .
C(911) C 0.4970(7) 0.0673(7) 0.1412(2) 0.109(7) Uiso 1.00 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W(3) 0.0520(3) 0.0516(3) 0.0426(2) -0.0078(2) 0.0016(2) -0.0041(2)
W(4) 0.0442(3) 0.0517(3) 0.0379(2) 0.0054(2) -0.0026(2) -0.0055(2)
W(5) 0.0449(3) 0.0476(2) 0.0398(2) -0.0029(2) -0.0040(2) -0.0033(2)
W(6) 0.0518(3) 0.0479(3) 0.0418(2) 0.0044(2) -0.0012(2) -0.0019(2)
W(7) 0.0410(2) 0.0636(3) 0.0423(2) -0.0034(2) -0.0004(2) -0.0064(2)
W(8) 0.0422(2) 0.0548(3) 0.0435(2) 0.0027(2) -0.0039(2) -0.0023(2)
W(9) 0.0530(3) 0.0623(3) 0.0400(2) -0.0071(2) 0.0048(2) -0.0005(2)
W(10) 0.0452(3) 0.0625(3) 0.0369(2) 0.0011(2) 0.0017(2) -0.0075(2)
W(11) 0.0465(3) 0.0544(3) 0.0374(2) 0.0011(2) -0.0058(2) -0.0050(2)
W(12) 0.0548(3) 0.0544(3) 0.0385(2) 0.0032(2) -0.0044(2) 0.0012(2)
Ti(1) 0.0483(15) 0.0484(13) 0.0378(11) -0.0008(10) 0.0010(10) -0.0039(9)
Ti(2) 0.0456(14) 0.0496(13) 0.0358(11) 0.0005(10) -0.0013(9) -0.0049(9)
Si(1) 0.0432(19) 0.0481(19) 0.0364(16) -0.0017(16) -0.0005(13) -0.0041(15)
O(1) 0.047(5) 0.056(5) 0.033(3) 0.003(4) -0.001(3) -0.005(3)
O(2) 0.049(5) 0.054(5) 0.033(3) -0.000(4) 0.003(3) -0.004(3)
O(3) 0.051(5) 0.057(5) 0.042(4) -0.001(4) -0.004(4) -0.009(4)
O(4) 0.045(5) 0.046(4) 0.040(4) 0.002(3) -0.003(3) -0.005(3)
O(5) 0.047(5) 0.049(5) 0.038(4) -0.002(4) -0.004(3) -0.001(3)
O(6) 0.055(5) 0.049(5) 0.038(4) 0.000(4) 0.001(4) -0.002(3)
O(7) 0.046(5) 0.065(5) 0.038(4) -0.009(4) -0.000(3) -0.003(4)
O(8) 0.036(5) 0.070(6) 0.036(4) 0.001(4) -0.004(3) -0.003(4)
O(9) 0.058(5) 0.048(5) 0.038(4) 0.001(4) -0.003(4) -0.005(3)
O(10) 0.043(5) 0.053(5) 0.041(4) 0.002(4) -0.001(3) -0.007(3)
O(11) 0.057(6) 0.049(5) 0.045(4) 0.006(4) -0.004(4) 0.001(4)
O(12) 0.073(6) 0.044(4) 0.041(4) 0.009(4) 0.004(4) -0.004(3)
O(13) 0.055(6) 0.055(5) 0.048(5) -0.001(4) 0.002(4) -0.004(4)
O(14) 0.054(5) 0.054(5) 0.038(4) 0.006(4) -0.001(4) -0.015(3)
O(15) 0.046(5) 0.050(5) 0.046(4) 0.003(4) -0.007(4) -0.005(3)
O(16) 0.057(6) 0.058(5) 0.045(5) 0.002(4) -0.002(4) 0.002(4)
O(17) 0.058(6) 0.063(6) 0.045(5) -0.006(4) 0.008(4) -0.003(4)
O(18) 0.048(5) 0.067(6) 0.039(4) 0.007(4) 0.004(4) -0.007(4)
O(19) 0.050(5) 0.048(5) 0.048(5) 0.004(4) -0.000(4) -0.004(4)
O(20) 0.060(6) 0.053(5) 0.046(5) 0.007(4) -0.007(4) -0.001(4)
O(21) 0.061(6) 0.066(6) 0.038(4) -0.008(4) 0.007(4) -0.005(4)
O(22) 0.043(5) 0.059(5) 0.035(4) 0.001(4) 0.001(3) -0.003(3)
O(23) 0.055(5) 0.063(5) 0.038(4) 0.006(4) -0.003(3) -0.002(4)
O(24) 0.051(6) 0.066(6) 0.036(4) -0.006(4) -0.001(3) 0.002(4)
O(25) 0.047(5) 0.049(4) 0.035(4) -0.002(4) -0.004(3) -0.003(3)
O(26) 0.049(5) 0.046(4) 0.041(4) 0.001(4) 0.000(3) -0.003(3)
O(27) 0.040(4) 0.051(4) 0.040(4) -0.002(3) 0.002(3) 0.000(3)
O(28) 0.044(4) 0.052(5) 0.035(4) 0.005(4) -0.006(3) -0.002(3)
O(101) 0.048(5) 0.063(5) 0.032(3) 0.006(4) -0.001(4) -0.004(4)
O(103) 0.063(6) 0.058(5) 0.055(5) -0.021(4) 0.004(4) 0.000(4)
O(104) 0.059(6) 0.064(6) 0.043(4) 0.006(4) -0.002(4) -0.009(4)
O(105) 0.063(6) 0.058(5) 0.047(5) -0.005(4) -0.003(4) -0.003(4)
O(106) 0.074(7) 0.055(5) 0.055(5) 0.005(5) -0.005(5) -0.001(4)
O(107) 0.050(5) 0.078(6) 0.059(5) -0.005(5) -0.007(4) -0.005(5)
O(108) 0.044(5) 0.066(6) 0.057(5) 0.005(4) -0.010(4) -0.008(4)
O(109) 0.067(7) 0.080(7) 0.046(5) -0.018(5) 0.007(4) 0.005(4)
O(110) 0.055(6) 0.081(7) 0.041(4) 0.005(5) 0.003(4) -0.013(4)
O(111) 0.058(6) 0.066(6) 0.044(5) 0.002(4) -0.015(4) -0.007(4)
O(112) 0.069(7) 0.073(6) 0.047(5) 0.013(5) -0.008(4) 0.005(4)
C(405) 0(11) 0.073(6) 0.046(5) 0.013(5) -0.009(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 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
K K 0.200 0.250
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.278 0.446
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O(3) W(3) O(7) 89.0(4) ? . . .
O(3) W(3) O(12) 89.5(4) ? . . .
O(3) W(3) O(13) 161.4(4) ? . . .
O(3) W(3) O(26) 76.7(3) ? . . .
O(3) W(3) O(103) 99.2(4) ? . . .
O(7) W(3) O(12) 157.0(4) ? . . .
O(7) W(3) O(13) 86.5(4) ? . . .
O(7) W(3) O(26) 82.6(3) ? . . .
O(7) W(3) O(103) 102.1(4) ? . . .
O(12) W(3) O(13) 87.7(4) ? . . .
O(12) W(3) O(26) 74.7(3) ? . . .
O(12) W(3) O(103) 100.9(4) ? . . .
O(13) W(3) O(26) 84.8(3) ? . . .
O(13) W(3) O(103) 99.4(4) ? . . .
O(26) W(3) O(103) 173.8(4) ? . . .
O(4) W(4) O(8) 88.9(3) ? . . .
O(4) W(4) O(9) 89.5(4) ? . . .
O(4) W(4) O(14) 161.3(4) ? . . .
O(4) W(4) O(25) 76.8(3) ? . . .
O(4) W(4) O(104) 99.0(4) ? . . .
O(8) W(4) O(9) 157.0(4) ? . . .
O(8) W(4) O(14) 86.0(3) ? . . .
O(8) W(4) O(25) 82.5(3) ? . . .
O(8) W(4) O(104) 102.0(4) ? . . .
O(9) W(4) O(14) 88.2(4) ? . . .
O(9) W(4) O(25) 74.8(3) ? . . .
O(9) W(4) O(104) 100.9(4) ? . . .
O(14) W(4) O(25) 84.7(3) ? . . .
O(14) W(4) O(104) 99.8(4) ? . . .
O(25) W(4) O(104) 173.8(4) ? . . .
O(5) W(5) O(9) 88.6(4) ? . . .
O(5) W(5) O(10) 89.1(3) ? . . .
O(5) W(5) O(15) 161.3(4) ? . . .
O(5) W(5) O(25) 76.8(3) ? . . .
O(5) W(5) O(105) 99.2(4) ? . . .
O(9) W(5) O(10) 156.7(4) ? . . .
O(9) W(5) O(15) 86.8(4) ? . . .
O(9) W(5) O(25) 74.5(3) ? . . .
O(9) W(5) O(105) 100.6(4) ? . . .
O(10) W(5) O(15) 87.9(3) ? . . .
O(10) W(5) O(25) 82.4(3) ? . . .
O(10) W(5) O(105) 102.7(4) ? . . .
O(15) W(5) O(25) 84.6(3) ? . . .
O(15) W(5) O(105) 99.4(4) ? . . .
O(25) W(5) O(105) 173.6(4) ? . . .
O(6) W(6) O(11) 89.1(4) ? . . .
O(6) W(6) O(12) 88.6(4) ? . . .
O(6) W(6) O(16) 161.0(4) ? . . .
O(6) W(6) O(26) 76.5(3) ? . . .
O(6) W(6) O(106) 99.7(4) ? . . .
O(11) W(6) O(12) 156.3(4) ? . . .
O(11) W(6) O(16) 87.2(4) ? . . .
O(11) W(6) O(26) 81.9(3) ? . . .
O(11) W(6) O(106) 103.2(4) ? . . .
O(12) W(6) O(16) 87.3(4) ? . . .
O(12) W(6) O(26) 74.6(3) ? . . .
O(12) W(6) O(106) 100.5(4) ? . . .
O(16) W(6) O(26) 84.6(3) ? . . .
O(16) W(6) O(106) 99.3(4) ? . . .
O(26) W(6) O(106) 173.7(4) ? . . .
O(7) W(7) O(8) 98.3(4) ? . . .
O(7) W(7) O(17) 86.0(4) ? . . .
O(7) W(7) O(18) 154.5(4) ? . . .
O(7) W(7) O(27) 80.8(3) ? . . .
O(7) W(7) O(107) 102.2(4) ? . . .
O(8) W(7) O(17) 155.0(4) ? . . .
O(8) W(7) O(18) 86.1(4) ? . . .
O(8) W(7) O(27) 80.9(3) ? . . .
O(8) W(7) O(107) 101.7(4) ? . . .
O(17) W(7) O(18) 80.1(4) ? . . .
O(17) W(7) O(27) 75.5(3) ? . . .
O(17) W(7) O(107) 101.4(4) ? . . .
O(18) W(7) O(27) 75.1(3) ? . . .
O(18) W(7) O(107) 101.4(4) ? . . .
O(27) W(7) O(107) 175.6(3) ? . . .
O(10) W(8) O(11) 94.4(3) ? . . .
O(10) W(8) O(19) 87.2(3) ? . . .
O(10) W(8) O(20) 155.9(4) ? . . .
O(10) W(8) O(28) 80.3(3) ? . . .
O(10) W(8) O(108) 102.3(4) ? . . .
O(11) W(8) O(19) 155.6(4) ? . . .
O(11) W(8) O(20) 86.8(4) ? . . .
O(11) W(8) O(28) 80.2(3) ? . . .
O(11) W(8) O(108) 102.8(4) ? . . .
O(19) W(8) O(20) 82.1(4) ? . . .
O(19) W(8) O(28) 76.1(3) ? . . .
O(19) W(8) O(108) 100.6(4) ? . . .
O(20) W(8) O(28) 76.3(3) ? . . .
O(20) W(8) O(108) 100.8(4) ? . . .
O(28) W(8) O(108) 175.8(3) ? . . .
O(13) W(9) O(17) 86.1(4) ? . . .
O(13) W(9) O(21) 155.4(4) ? . . .
O(13) W(9) O(24) 87.7(4) ? . . .
O(13) W(9) O(27) 81.3(3) ? . . .
O(13) W(9) O(109) 103.3(4) ? . . .
O(17) W(9) O(21) 87.6(4) ? . . .
O(17) W(9) O(24) 159.5(4) ? . . .
O(17) W(9) O(27) 75.6(3) ? . . .
O(17) W(9) O(109) 99.8(5) ? . . .
O(21) W(9) O(24) 90.0(4) ? . . .
O(21) W(9) O(27) 74.1(3) ? . . .
O(21) W(9) O(109) 101.2(4) ? . . .
O(24) W(9) O(27) 84.2(3) ? . . .
O(24) W(9) O(109) 100.6(4) ? . . .
O(27) W(9) O(109) 173.4(4) ? . . .
O(14) W(10) O(18) 85.6(4) ? . . .
O(14) W(10) O(21) 155.2(4) ? . . .
O(14) W(10) O(22) 88.5(4) ? . . .
O(14) W(10) O(27) 80.9(3) ? . . .
O(14) W(10) O(110) 103.9(4) ? . . .
O(18) W(10) O(21) 87.5(4) ? . . .
O(18) W(10) O(22) 159.4(4) ? . . .
O(18) W(10) O(27) 75.4(3) ? . . .
O(18) W(10) O(110) 99.6(4) ? . . .
O(21) W(10) O(22) 89.7(4) ? . . .
O(21) W(10) O(27) 74.2(3) ? . . .
O(21) W(10) O(110) 100.7(4) ? . . .
O(22) W(10) O(27) 84.2(3) ? . . .
O(22) W(10) O(110) 101.0(4) ? . . .
O(27) W(10) O(110) 172.9(4) ? . . .
O(15) W(11) O(19) 85.2(4) ? . . .
O(15) W(11) O(22) 89.4(4) ? . . .
O(15) W(11) O(23) 154.9(3) ? . . .
O(15) W(11) O(28) 81.3(3) ? . . .
O(15) W(11) O(111) 102.9(4) ? . . .
O(19) W(11) O(22) 160.5(4) ? . . .
O(19) W(11) O(23) 86.5(4) ? . . .
O(19) W(11) O(28) 76.1(3) ? . . .
O(19) W(11) O(111) 98.3(4) ? . . .
O(22) W(11) O(23) 90.4(4) ? . . .
O(22) W(11) O(28) 84.6(3) ? . . .
O(22) W(11) O(111) 101.2(4) ? . . .
O(23) W(11) O(28) 73.7(3) ? . . .
O(23) W(11) O(111) 101.7(4) ? . . .
O(28) W(11) O(111) 172.7(4) ? . . .
O(16) W(12) O(20) 84.6(4) ? . . .
O(16) W(12) O(23) 154.4(4) ? . . .
O(16) W(12) O(24) 89.4(4) ? . . .
O(16) W(12) O(28) 81.4(3) ? . . .
O(16) W(12) O(112) 103.6(4) ? . . .
O(20) W(12) O(23) 86.4(4) ? . . .
O(20) W(12) O(24) 160.0(4) ? . . .
O(20) W(12) O(28) 75.5(3) ? . . .
O(20) W(12) O(112) 99.5(5) ? . . .
O(23) W(12) O(24) 90.9(4) ? . . .
O(23) W(12) O(28) 73.2(3) ? . . .
O(23) W(12) O(112) 101.5(4) ? . . .
O(24) W(12) O(28) 84.7(3) ? . . .
O(24) W(12) O(112) 100.5(4) ? . . .
O(28) W(12) O(112) 172.7(4) ? . . .
Ti(2) Ti(1) O(1) 36.9(2) ? . . .
Ti(2) Ti(1) O(2) 38.3(2) ? . . .
Ti(2) Ti(1) O(3) 126.7(3) ? . . .
Ti(2) Ti(1) O(6) 126.7(3) ? . . .
Ti(2) Ti(1) O(26) 84.7(2) ? . . .
Ti(2) Ti(1) O(101) 100.8(3) ? . . 55506
O(1) Ti(1) O(2) 75.1(3) ? . . .
O(1) Ti(1) O(3) 92.1(4) ? . . .
O(1) Ti(1) O(6) 157.0(3) ? . . .
O(1) Ti(1) O(26) 86.1(3) ? . . .
O(1) Ti(1) O(101) 98.8(3) ? . . 55506
O(2) Ti(1) O(3) 155.2(4) ? . . .
O(2) Ti(1) O(6) 89.8(4) ? . . .
O(2) Ti(1) O(26) 82.4(3) ? . . .
O(2) Ti(1) O(101) 101.3(3) ? . . 55506
O(3) Ti(1) O(6) 94.9(4) ? . . .
O(3) Ti(1) O(26) 75.5(3) ? . . .
O(3) Ti(1) O(101) 101.6(4) ? . . 55506
O(6) Ti(1) O(26) 74.5(3) ? . . .
O(6) Ti(1) O(101) 101.2(4) ? . . 55506
O(26) Ti(1) O(101) 174.4(3) ? . . 55506
Ti(1) Ti(2) O(1) 36.9(2) ? . . .
Ti(1) Ti(2) O(2) 38.2(2) ? . . .
Ti(1) Ti(2) O(4) 126.4(3) ? . . .
Ti(1) Ti(2) O(5) 126.6(3) ? . . .
Ti(1) Ti(2) O(25) 84.2(2) ? . . .
Ti(1) Ti(2) O(101) 100.7(3) ? . . .
O(1) Ti(2) O(2) 75.0(3) ? . . .
O(1) Ti(2) O(4) 91.9(4) ? . . .
O(1) Ti(2) O(5) 157.0(3) ? . . .
O(1) Ti(2) O(25) 85.6(3) ? . . .
O(1) Ti(2) O(101) 98.8(3) ? . . .
O(2) Ti(2) O(4) 154.5(3) ? . . .
O(2) Ti(2) O(5) 89.7(4) ? . . .
O(2) Ti(2) O(25) 82.2(3) ? . . .
O(2) Ti(2) O(101) 101.3(3) ? . . .
O(4) Ti(2) O(5) 95.1(4) ? . . .
O(4) Ti(2) O(25) 74.9(3) ? . . .
O(4) Ti(2) O(101) 102.3(4) ? . . .
O(5) Ti(2) O(25) 75.1(3) ? . . .
O(5) Ti(2) O(101) 101.1(4) ? . . .
O(25) Ti(2) O(101) 175.0(3) ? . . .
K(11) K(1) O(201) 71.7 ? . . .
K(11) K(1) O(202) 85.1(9) ? . . .
K(11) K(1) O(203) 77.0(8) ? . . .
K(11) K(1) O(204) 82.8(9) ? . . .
K(11) K(1) O(205) 75.8(9) ? . . .
K(11) K(1) O(206) 85.3(9) ? . . .
K(11) K(1) O(211) 79.4 ? . . .
O(201) K(1) O(202) 62.5 ? . . .
O(201) K(1) O(203) 115.0 ? . . .
O(201) K(1) O(204) 154.5 ? . . .
O(201) K(1) O(205) 110.0 ? . . .
O(201) K(1) O(206) 56.2 ? . . .
O(201) K(1) O(211) 12.6 ? . . .
O(202) K(1) O(203) 59.4(6) ? . . .
O(202) K(1) O(204) 117.7(6) ? . . .
O(202) K(1) O(205) 160.9(6) ? . . .
O(202) K(1) O(206) 117.9(7) ? . . .
O(202) K(1) O(211) 52.1 ? . . .
O(203) K(1) O(204) 58.3(5) ? . . .
O(203) K(1) O(205) 115.2(6) ? . . .
O(203) K(1) O(206) 162.2(6) ? . . .
O(203) K(1) O(211) 108.5 ? . . .
O(204) K(1) O(205) 60.7(5) ? . . .
O(204) K(1) O(206) 121.6(6) ? . . .
O(204) K(1) O(211) 160.1 ? . . .
O(205) K(1) O(206) 60.9(6) ? . . .
O(205) K(1) O(211) 122.2 ? . . .
O(206) K(1) O(211) 65.8 ? . . .
O(301) K(2) O(302) 60.0(8) ? . . .
O(301) K(2) O(303) 117.4(10) ? . . .
O(301) K(2) O(304) 175.0(8) ? . . .
O(301) K(2) O(305) 120.2(9) ? . . .
O(301) K(2) O(306) 64.3(9) ? . . .
O(302) K(2) O(303) 58.7(9) ? . . .
O(302) K(2) O(304) 116.9(8) ? . . .
O(302) K(2) O(305) 125.9(8) ? . . .
O(302) K(2) O(306) 107.2(9) ? . . .
O(303) K(2) O(304) 60.7(9) ? . . .
O(303) K(2) O(305) 105.1(9) ? . . .
O(303) K(2) O(306) 148.2(10) ? . . .
O(304) K(2) O(305) 57.7(8) ? . . .
O(304) K(2) O(306) 114.6(9) ? . . .
O(305) K(2) O(306) 57.7(9) ? . . .
O(401) K(3) O(401) 124.8(13) ? . . 55520
O(401) K(3) O(402) 55.0(13) ? . . .
O(401) K(3) O(402) 124.2(13) ? . . 55520
O(401) K(3) O(403) 100.3(13) ? . . .
O(401) K(3) O(403) 54.4(14) ? . . 55520
O(401) K(3) C(404) 76.1(19) ? . . .
O(401) K(3) C(404) 82.2(17) ? . . 55520
O(401) K(3) O(402) 124.2(13) ? 55520 . .
O(401) K(3) O(402) 55.0(13) ? 55520 . 55520
O(401) K(3) O(403) 54.4(14) ? 55520 . .
O(401) K(3) O(403) 100.3(13) ? 55520 . 55520
O(401) K(3) C(404) 82.2(18) ? 55520 . .
O(401) K(3) C(404) 76.1(18) ? 55520 . 55520
O(402) K(3) O(402) 178.7(12) ? . . 55520
O(402) K(3) O(403) 70.3(12) ? . . .
O(402) K(3) O(403) 109.1(12) ? . . 55520
O(402) K(3) C(404) 42.0(17) ? . . .
O(402) K(3) C(404) 137.2(16) ? . . 55520
O(402) K(3) O(403) 109.1(12) ? 55520 . .
O(402) K(3) O(403) 70.3(12) ? 55520 . 55520
O(402) K(3) C(404) 137.2(16) ? 55520 . .
O(402) K(3) C(404) 42.0(16) ? 55520 . 55520
O(403) K(3) O(403) 128.3(11) ? . . 55520
O(403) K(3) C(404) 29.2(18) ? . . .
O(403) K(3) C(404) 121.3(17) ? . . 55520
O(403) K(3) C(404) 121.3(17) ? 55520 . .
O(403) K(3) C(404) 29.2(17) ? 55520 . 55520
C(404) K(3) C(404) 132(2) ? . . 55520
O(501) K(4) O(501) 99.8(8) ? . . 55520
O(501) K(4) O(502) 60.4(8) ? . . .
O(501) K(4) O(502) 40.0(8) ? . . 55520
O(501) K(4) O(503) 117.8(8) ? . . .
O(501) K(4) O(503) 33.9(8) ? . . 55520
O(501) K(4) O(504) 163.2(7) ? . . .
O(501) K(4) O(504) 87.9(7) ? . . 55520
O(501) K(4) O(505) 110.9(6) ? . . .
O(501) K(4) O(505) 148.6(6) ? . . 55520
O(501) K(4) O(506) 56.5(7) ? . . .
O(501) K(4) O(506) 153.1(8) ? . . 55520
O(501) K(4) O(502) 40.0(8) ? 55520 . .
O(501) K(4) O(502) 60.4(8) ? 55520 . 55520
O(501) K(4) O(503) 33.9(8) ? 55520 . .
O(501) K(4) O(503) 117.8(8) ? 55520 . 55520
O(501) K(4) O(504) 87.9(7) ? 55520 . .
O(501) K(4) O(504) 163.2(7) ? 55520 . 55520
O(501) K(4) O(505) 148.6(6) ? 55520 . .
O(501) K(4) O(505) 110.9(6) ? 55520 . 55520
O(501) K(4) O(506) 153.1(8) ? 55520 . .
O(501) K(4) O(506) 56.5(7) ? 55520 . 55520
O(502) K(4) O(502) 24.3(9) ? . . 55520
O(502) K(4) O(503) 61.5(8) ? . . .
O(502) K(4) O(503) 85.7(9) ? . . 55520
O(502) K(4) O(504) 123.6(7) ? . . .
O(502) K(4) O(504) 147.4(8) ? . . 55520
O(502) K(4) O(505) 164.7(7) ? . . .
O(502) K(4) O(505) 150.8(6) ? . . 55520
O(502) K(4) O(506) 116.6(8) ? . . .
O(502) K(4) O(506) 93.9(8) ? . . 55520
O(502) K(4) O(503) 85.7(9) ? 55520 . .
O(502) K(4) O(503) 61.5(8) ? 55520 . 55520
O(502) K(4) O(504) 147.4(8) ? 55520 . .
O(502) K(4) O(504) 123.6(7) ? 55520 . 55520
O(502) K(4) O(505) 150.8(6) ? 55520 . .
O(502) K(4) O(505) 164.7(7) ? 55520 . 55520
O(502) K(4) O(506) 93.9(8) ? 55520 . .
O(502) K(4) O(506) 116.6(8) ? 55520 . 55520
O(503) K(4) O(503) 147.2(9) ? . . 55520
O(503) K(4) O(504) 62.2(7) ? . . .
O(503) K(4) O(504) 150.4(8) ? . . 55520
O(503) K(4) O(505) 119.5(6) ? . . .
O(503) K(4) O(505) 92.2(6) ? . . 55520
O(503) K(4) O(506) 164.6(9) ? . . .
O(503) K(4) O(506) 35.4(8) ? . . 55520
O(503) K(4) O(504) 150.4(8) ? 55520 . .
O(503) K(4) O(504) 62.2(7) ? 55520 . 55520
O(503) K(4) O(505) 92.2(6) ? 55520 . .
O(503) K(4) O(505) 119.5(6) ? 55520 . 55520
O(503) K(4) O(506) 35.4(8) ? 55520 . .
O(503) K(4) O(506) 164.6(9) ? 55520 . 55520
O(504) K(4) O(504) 88.9(6) ? . . 55520
O(504) K(4) O(505) 60.8(5) ? . . .
O(504) K(4) O(505) 31.3(4) ? . . 55520
O(504) K(4) O(506) 118.5(7) ? . . .
O(504) K(4) O(506) 31.4(7) ? . . 55520
O(504) K(4) O(505) 31.3(4) ? 55520 . .
O(504) K(4) O(505) 60.8(5) ? 55520 . 55520
O(504) K(4) O(506) 31.4(7) ? 55520 . .
O(504) K(4) O(506) 118.5(7) ? 55520 . 55520
O(505) K(4) O(505) 39.9(3) ? . . 55520
O(505) K(4) O(506) 57.8(6) ? . . .
O(505) K(4) O(506) 92.1(6) ? . . 55520
O(505) K(4) O(506) 92.1(6) ? 55520 . .
O(505) K(4) O(506) 57.8(6) ? 55520 . 55520
O(506) K(4) O(506) 149.5(8) ? . . 55520
K(55) K(5) O(601) 51.9(7) ? . . .
K(55) K(5) O(601) 51.9(7) ? . . 55507
K(55) K(5) O(602) 66.9(10) ? . . .
K(55) K(5) O(602) 66.9(10) ? . . 55507
K(55) K(5) O(603) 106.2(15) ? . . .
K(55) K(5) O(603) 106.2(15) ? . . 55507
K(55) K(5) O(604) 115.5(16) ? . . .
K(55) K(5) O(604) 115.5(16) ? . . 55507
K(55) K(5) O(605) 97.0(15) ? . . .
K(55) K(5) O(605) 97.0(15) ? . . 55507
K(55) K(5) O(606) 56.1(8) ? . . .
K(55) K(5) O(606) 56.1(8) ? . . 55507
O(601) K(5) O(601) 103.7(11) ? . . 55507
O(601) K(5) O(602) 54.7(14) ? . . .
O(601) K(5) O(602) 95.4(13) ? . . 55507
O(601) K(5) O(603) 111.7(15) ? . . .
O(601) K(5) O(603) 88.6(16) ? . . 55507
O(601) K(5) O(604) 166.2(19) ? . . .
O(601) K(5) O(604) 63.9(18) ? . . 55507
O(601) K(5) O(605) 116.6(16) ? . . .
O(601) K(5) O(605) 72.7(16) ? . . 55507
O(601) K(5) O(606) 54.8(9) ? . . .
O(601) K(5) O(606) 83.5(14) ? . . 55507
O(601) K(5) O(602) 95.4(13) ? 55507 . .
O(601) K(5) O(602) 54.7(14) ? 55507 . 55507
O(601) K(5) O(603) 88.6(16) ? 55507 . .
O(601) K(5) O(603) 111.7(16) ? 55507 . 55507
O(601) K(5) O(604) 63.9(18) ? 55507 . .
O(601) K(5) O(604) 166.2(18) ? 55507 . 55507
O(601) K(5) O(605) 72.7(16) ? 55507 . .
O(601) K(5) O(605) 116.6(16) ? 55507 . 55507
O(601) K(5) O(606) 83.5(14) ? 55507 . .
O(601) K(5) O(606) 54.8(9) ? 55507 . 55507
O(602) K(5) O(602) 133.9(15) ? . . 55507
O(602) K(5) O(603) 57.4(19) ? . . .
O(602) K(5) O(603) 139(2) ? . . 55507
O(602) K(5) O(604) 118(2) ? . . .
O(602) K(5) O(604) 82(2) ? . . 55507
O(602) K(5) O(605) 163.9(18) ? . . .
O(602) K(5) O(605) 30.0(18) ? . . 55507
O(602) K(5) O(606) 106.7(14) ? . . .
O(602) K(5) O(606) 43.6(17) ? . . 55507
O(602) K(5) O(603) 139(2) ? 55507 . .
O(602) K(5) O(603) 57.4(19) ? 55507 . 55507
O(602) K(5) O(604) 82(2) ? 55507 . .
O(602) K(5) O(604) 118(2) ? 55507 . 55507
O(602) K(5) O(605) 30.0(18) ? 55507 . .
O(602) K(5) O(605) 163.9(19) ? 55507 . 55507
O(602) K(5) O(606) 43.6(17) ? 55507 . .
O(602) K(5) O(606) 106.7(14) ? 55507 . 55507
O(603) K(5) O(603) 148(2) ? . . 55507
O(603) K(5) O(604) 64(2) ? . . .
O(603) K(5) O(604) 101(2) ? . . 55507
O(603) K(5) O(605) 131(2) ? . . .
O(603) K(5) O(605) 44(2) ? . . 55507
O(603) K(5) O(606) 161.5(17) ? . . .
O(603) K(5) O(606) 50.4(17) ? . . 55507
O(603) K(5) O(604) 101(2) ? 55507 . .
O(603) K(5) O(604) 64(2) ? 55507 . 55507
O(603) K(5) O(605) 44(2) ? 55507 . .
O(603) K(5) O(605) 131(2) ? 55507 . 55507
O(603) K(5) O(606) 50.4(17) ? 55507 . .
O(603) K(5) O(606) 161.5(17) ? 55507 . 55507
O(604) K(5) O(604) 129(2) ? . . 55507
O(604) K(5) O(605) 67(2) ? . . .
O(604) K(5) O(605) 107(2) ? . . 55507
O(604) K(5) O(606) 126(2) ? . . .
O(604) K(5) O(606) 84(2) ? . . 55507
O(604) K(5) O(605) 107(2) ? 55507 . .
O(604) K(5) O(605) 67(2) ? 55507 . 55507
O(604) K(5) O(606) 84(2) ? 55507 . .
O(604) K(5) O(606) 126(2) ? 55507 . 55507
O(605) K(5) O(605) 166(2) ? . . 55507
O(605) K(5) O(606) 62.0(17) ? . . .
O(605) K(5) O(606) 127.2(18) ? . . 55507
O(605) K(5) O(606) 127.2(18) ? 55507 . .
O(605) K(5) O(606) 62.0(17) ? 55507 . 55507
O(606) K(5) O(606) 112.1(12) ? . . 55507
O(702) K(6) O(702) 100(2) ? . . 55520
O(702) K(6) O(703) 58(2) ? . . .
O(702) K(6) O(703) 136(2) ? . . 55520
O(702) K(6) O(704) 117(2) ? . . .
O(702) K(6) O(704) 115(2) ? . . 55520
O(702) K(6) O(705) 133(2) ? . . .
O(702) K(6) O(705) 58(2) ? . . 55520
O(702) K(6) O(703) 136(2) ? 55520 . .
O(702) K(6) O(703) 58(2) ? 55520 . 55520
O(702) K(6) O(704) 115(2) ? 55520 . .
O(702) K(6) O(704) 117(2) ? 55520 . 55520
O(702) K(6) O(705) 58(2) ? 55520 . .
O(702) K(6) O(705) 133(2) ? 55520 . 55520
O(703) K(6) O(703) 162(2) ? . . 55520
O(703) K(6) O(704) 60(3) ? . . .
O(703) K(6) O(704) 106(3) ? . . 55520
O(703) K(6) O(705) 107(3) ? . . .
O(703) K(6) O(705) 71(3) ? . . 55520
O(703) K(6) O(704) 106(3) ? 55520 . .
O(703) K(6) O(704) 60(3) ? 55520 . 55520
O(703) K(6) O(705) 71(3) ? 55520 . .
O(703) K(6) O(705) 107(3) ? 55520 . 55520
O(704) K(6) O(704) 94(2) ? . . 55520
O(704) K(6) O(705) 58(3) ? . . .
O(704) K(6) O(705) 112(3) ? . . 55520
O(704) K(6) O(705) 112(3) ? 55520 . .
O(704) K(6) O(705) 58(3) ? 55520 . 55520
O(705) K(6) O(705) 167(2) ? . . 55520
K(1) K(11) O(201) 89.1 ? . . .
K(1) K(11) O(202) 76.0(9) ? . . .
K(1) K(11) O(203) 84.5(9) ? . . .
K(1) K(11) O(204) 77.9(9) ? . . .
K(1) K(11) O(205) 85.1(9) ? . . .
K(1) K(11) O(206) 75.7(9) ? . . .
K(1) K(11) O(211) 82.9 ? . . .
O(201) K(11) O(202) 63.2 ? . . .
O(201) K(11) O(203) 122.0 ? . . .
O(201) K(11) O(204) 166.9 ? . . .
O(201) K(11) O(205) 116.9 ? . . .
O(201) K(11) O(206) 56.9 ? . . .
O(201) K(11) O(211) 12.0 ? . . .
O(202) K(11) O(203) 59.3(6) ? . . .
O(202) K(11) O(204) 113.9(6) ? . . .
O(202) K(11) O(205) 161.0(6) ? . . .
O(202) K(11) O(206) 112.9(7) ? . . .
O(202) K(11) O(211) 51.7 ? . . .
O(203) K(11) O(204) 58.6(5) ? . . .
O(203) K(11) O(205) 119.8(7) ? . . .
O(203) K(11) O(206) 160.1(7) ? . . .
O(203) K(11) O(211) 110.9 ? . . .
O(204) K(11) O(205) 61.2(5) ? . . .
O(204) K(11) O(206) 117.4(6) ? . . .
O(204) K(11) O(211) 158.8 ? . . .
O(205) K(11) O(206) 60.9(6) ? . . .
O(205) K(11) O(211) 126.1 ? . . .
O(206) K(11) O(211) 65.3 ? . . .
K(5) K(55) K(55) 180.0000 ? . . 55506
K(5) K(55) O(601) 102.5(7) ? . . .
K(5) K(55) O(601) 102.5(7) ? . . 55507
K(5) K(55) O(602) 86.6(13) ? . . .
K(5) K(55) O(602) 86.6(13) ? . . 55507
K(5) K(55) O(605) 57.0(12) ? . . .
K(5) K(55) O(605) 57.0(12) ? . . 55507
K(5) K(55) O(606) 96.4(10) ? . . .
K(5) K(55) O(606) 96.4(10) ? . . 55507
K(55) K(55) O(601) 77.5(7) ? 55506 . .
K(55) K(55) O(601) 77.5(7) ? 55506 . 55507
K(55) K(55) O(602) 93.4(13) ? 55506 . .
K(55) K(55) O(602) 93.4(13) ? 55506 . 55507
K(55) K(55) O(605) 123.0(12) ? 55506 . .
K(55) K(55) O(605) 123.0(12) ? 55506 . 55507
K(55) K(55) O(606) 83.6(10) ? 55506 . .
K(55) K(55) O(606) 83.6(10) ? 55506 . 55507
O(601) K(55) O(601) 154.9(12) ? . . 55507
O(601) K(55) O(602) 63.9(16) ? . . .
O(601) K(55) O(602) 117.7(16) ? . . 55507
O(601) K(55) O(605) 120.6(15) ? . . .
O(601) K(55) O(605) 74.2(14) ? . . 55507
O(601) K(55) O(606) 68.3(14) ? . . .
O(601) K(55) O(606) 108.7(15) ? . . 55507
O(601) K(55) O(602) 117.7(16) ? 55507 . .
O(601) K(55) O(602) 63.9(16) ? 55507 . 55507
O(601) K(55) O(605) 74.2(14) ? 55507 . .
O(601) K(55) O(605) 120.6(15) ? 55507 . 55507
O(601) K(55) O(606) 108.7(14) ? 55507 . .
O(601) K(55) O(606) 68.3(14) ? 55507 . 55507
O(602) K(55) O(602) 173.2(19) ? . . 55507
O(602) K(55) O(605) 143.6(19) ? . . .
O(602) K(55) O(605) 29.6(17) ? . . 55507
O(602) K(55) O(606) 132(2) ? . . .
O(602) K(55) O(606) 49(2) ? . . 55507
O(602) K(55) O(605) 29.6(17) ? 55507 . .
O(602) K(55) O(605) 143.6(19) ? 55507 . 55507
O(602) K(55) O(606) 49.4(19) ? 55507 . .
O(602) K(55) O(606) 132(2) ? 55507 . 55507
O(605) K(55) O(605) 113.9(18) ? . . 55507
O(605) K(55) O(606) 61.2(17) ? . . .
O(605) K(55) O(606) 127.2(18) ? . . 55507
O(605) K(55) O(606) 127.2(18) ? 55507 . .
O(605) K(55) O(606) 61.2(17) ? 55507 . 55507
O(606) K(55) O(606) 167.1(16) ? . . 55507
S(11) S(1) O(901) 103.3 ? . . .
S(11) S(1) C(901) 51.9 ? . . .
S(11) S(1) C(911) 53.4 ? . . .
O(901) S(1) C(901) 105.0 ? . . .
O(901) S(1) C(911) 106.2 ? . . .
C(901) S(1) C(911) 103.2 ? . . .
S(1) S(11) O(911) 132.7 ? . . .
S(1) S(11) C(901) 56.7 ? . . .
S(1) S(11) C(911) 56.1 ? . . .
O(911) S(11) C(901) 106.5 ? . . .
O(911) S(11) C(911) 105.2 ? . . .
C(901) S(11) C(911) 110.5 ? . . .
O(25) Si(1) O(26) 110.6(4) ? . . .
O(25) Si(1) O(27) 109.7(5) ? . . .
O(25) Si(1) O(28) 109.4(5) ? . . .
O(26) Si(1) O(27) 110.6(5) ? . . .
O(26) Si(1) O(28) 109.7(5) ? . . .
O(27) Si(1) O(28) 106.8(4) ? . . .
Ti(1) O(1) Ti(2) 106.2(4) ? . . .
Ti(1) O(2) Ti(2) 103.5(4) ? . . .
W(3) O(3) Ti(1) 120.2(5) ? . . .
W(4) O(4) Ti(2) 120.6(5) ? . . .
W(5) O(5) Ti(2) 120.6(4) ? . . .
W(6) O(6) Ti(1) 121.1(5) ? . . .
W(3) O(7) W(7) 146.6(5) ? . . .
W(4) O(8) W(7) 146.1(4) ? . . .
W(4) O(9) W(5) 119.5(4) ? . . .
W(5) O(10) W(8) 144.3(4) ? . . .
W(6) O(11) W(8) 144.9(5) ? . . .
W(3) O(12) W(6) 119.4(4) ? . . .
W(3) O(13) W(9) 146.0(5) ? . . .
W(4) O(14) W(10) 147.1(5) ? . . .
W(5) O(15) W(11) 146.0(5) ? . . .
W(6) O(16) W(12) 146.8(5) ? . . .
W(7) O(17) W(9) 119.0(5) ? . . .
W(7) O(18) W(10) 119.3(5) ? . . .
W(8) O(19) W(11) 118.3(5) ? . . .
W(8) O(20) W(12) 118.8(5) ? . . .
W(9) O(21) W(10) 120.8(4) ? . . .
W(10) O(22) W(11) 157.3(5) ? . . .
W(11) O(23) W(12) 122.2(4) ? . . .
W(9) O(24) W(12) 157.8(5) ? . . .
W(4) O(25) W(5) 91.1(3) ? . . .
W(4) O(25) Ti(2) 87.2(3) ? . . .
W(4) O(25) Si(1) 124.4(5) ? . . .
W(5) O(25) Ti(2) 87.2(3) ? . . .
W(5) O(25) Si(1) 124.2(4) ? . . .
Ti(2) O(25) Si(1) 130.4(5) ? . . .
W(3) O(26) W(6) 91.3(3) ? . . .
W(3) O(26) Ti(1) 87.2(3) ? . . .
W(3) O(26) Si(1) 123.9(5) ? . . .
W(6) O(26) Ti(1) 87.6(3) ? . . .
W(6) O(26) Si(1) 124.8(5) ? . . .
Ti(1) O(26) Si(1) 130.0(5) ? . . .
W(7) O(27) W(9) 89.7(3) ? . . .
W(7) O(27) W(10) 89.9(3) ? . . .
W(7) O(27) Si(1) 123.7(4) ? . . .
W(9) O(27) W(10) 90.3(2) ? . . .
W(9) O(27) Si(1) 125.8(5) ? . . .
W(10) O(27) Si(1) 126.4(5) ? . . .
W(8) O(28) W(11) 89.4(3) ? . . .
W(8) O(28) W(12) 89.2(3) ? . . .
W(8) O(28) Si(1) 124.7(4) ? . . .
W(11) O(28) W(12) 90.6(2) ? . . .
W(11) O(28) Si(1) 126.2(5) ? . . .
W(12) O(28) Si(1) 125.3(5) ? . . .
Ti(1) O(101) Ti(2) 154.7(5) ? 55506 . .
K(1) O(201) K(11) 19.2 ? . . .
K(1) O(201) O(211) 101.0 ? . . .
K(1) O(201) C(201) 104.3 ? . . .
K(1) O(201) C(212) 115.3 ? . . .
K(11) O(201) O(211) 111.8 ? . . .
K(11) O(201) C(201) 111.6 ? . . .
K(11) O(201) C(212) 126.6 ? . . .
O(211) O(201) C(201) 11.4 ? . . .
O(211) O(201) C(212) 97.4 ? . . .
C(201) O(201) C(212) 105.3 ? . . .
K(1) O(202) K(11) 18.9(3) ? . . .
K(1) O(202) C(202) 123.1(17) ? . . .
K(1) O(202) C(203) 121(2) ? . . .
K(11) O(202) C(202) 113.3(17) ? . . .
K(11) O(202) C(203) 116(2) ? . . .
C(202) O(202) C(203) 108(2) ? . . .
K(1) O(203) K(11) 18.5(3) ? . . .
K(1) O(203) C(204) 109.2(17) ? . . .
K(1) O(203) C(205) 107.4(16) ? . . .
K(11) O(203) C(204) 121.1(18) ? . . .
K(11) O(203) C(205) 116.3(16) ? . . .
C(204) O(203) C(205) 98(2) ? . . .
K(1) O(204) K(11) 19.3(3) ? . . .
K(1) O(204) C(206) 121.3(16) ? . . .
K(1) O(204) C(207) 117.8(15) ? . . .
K(11) O(204) C(206) 112.9(15) ? . . .
K(11) O(204) C(207) 109.8(15) ? . . .
C(206) O(204) C(207) 109(2) ? . . .
K(1) O(205) K(11) 19.2(3) ? . . .
K(1) O(205) C(208) 111.7(15) ? . . .
K(1) O(205) C(209) 108.8(15) ? . . .
K(11) O(205) C(208) 119.6(15) ? . . .
K(11) O(205) C(209) 118.8(16) ? . . .
C(208) O(205) C(209) 106(2) ? . . .
K(1) O(206) K(11) 19.0(3) ? . . .
K(1) O(206) C(210) 118(2) ? . . .
K(1) O(206) C(211) 117.6(17) ? . . .
K(11) O(206) C(210) 111(2) ? . . .
K(11) O(206) C(211) 107.9(17) ? . . .
C(210) O(206) C(211) 110(2) ? . . .
K(1) O(211) K(11) 17.8 ? . . .
K(1) O(211) O(201) 66.4 ? . . .
K(1) O(211) C(201) 117.9 ? . . .
K(1) O(211) C(212) 97.9 ? . . .
K(11) O(211) O(201) 56.2 ? . . .
K(11) O(211) C(201) 122.3 ? . . .
K(11) O(211) C(212) 100.5 ? . . .
O(201) O(211) C(201) 161.9 ? . . .
O(201) O(211) C(212) 56.9 ? . . .
C(201) O(211) C(212) 134.6 ? . . .
K(2) O(301) C(301) 116(2) ? . . .
K(2) O(301) C(312) 111(2) ? . . .
C(301) O(301) C(312) 109(3) ? . . .
K(2) O(302) C(302) 111(2) ? . . .
K(2) O(302) C(303) 115(2) ? . . .
C(302) O(302) C(303) 104(2) ? . . .
K(2) O(303) C(304) 116(2) ? . . .
K(2) O(303) C(305) 108(3) ? . . .
C(304) O(303) C(305) 94(3) ? . . .
K(2) O(304) C(306) 117(3) ? . . .
K(2) O(304) C(307) 114.9(18) ? . . .
C(306) O(304) C(307) 108(3) ? . . .
K(2) O(305) C(308) 101(2) ? . . .
K(2) O(305) C(309) 110(2) ? . . .
C(308) O(305) C(309) 118(4) ? . . .
K(2) O(306) C(310) 116(2) ? . . .
K(2) O(306) C(311) 121(3) ? . . .
C(310) O(306) C(311) 106(4) ? . . .
K(3) O(401) C(401) 108(3) ? . . .
K(3) O(401) C(406) 108(3) ? . . .
C(401) O(401) C(406) 127(5) ? . . .
K(3) O(402) C(402) 135(2) ? . . .
K(3) O(402) C(403) 108(2) ? . . .
C(402) O(402) C(403) 93(3) ? . . .
K(3) O(403) C(404) 75(3) ? . . .
K(3) O(403) C(405) 114(5) ? . . .
C(404) O(403) C(405) 40(6) ? . . .
K(4) O(501) O(503) 67.0(13) ? . . 55520
K(4) O(501) C(501) 109(2) ? . . .
K(4) O(501) C(503) 99.1(17) ? . . 55520
K(4) O(501) C(504) 121(2) ? . . 55520
K(4) O(501) C(512) 115.7(19) ? . . .
O(503) O(501) C(501) 113(2) ? 55520 . .
O(503) O(501) C(503) 89(2) ? 55520 . 55520
O(503) O(501) C(504) 60(2) ? 55520 . 55520
O(503) O(501) C(512) 51.6(19) ? 55520 . .
C(501) O(501) C(503) 23.4(18) ? . . 55520
C(501) O(501) C(504) 72(2) ? . . 55520
C(501) O(501) C(512) 111(2) ? . . .
C(503) O(501) C(504) 58(2) ? 55520 . 55520
C(503) O(501) C(512) 98(2) ? 55520 . .
C(504) O(501) C(512) 40(2) ? 55520 . .
K(4) O(502) O(502) 77.9(18) ? . . 55520
K(4) O(502) C(501) 122.5(19) ? . . 55520
K(4) O(502) C(502) 119.0(19) ? . . .
K(4) O(502) C(502) 135(2) ? . . 55520
K(4) O(502) C(503) 118.2(18) ? . . .
O(502) O(502) C(501) 147(3) ? 55520 . 55520
O(502) O(502) C(502) 53(2) ? 55520 . .
O(502) O(502) C(502) 77(2) ? 55520 . 55520
O(502) O(502) C(503) 163(3) ? 55520 . .
C(501) O(502) C(502) 118(2) ? 55520 . .
C(501) O(502) C(502) 70(2) ? 55520 . 55520
C(501) O(502) C(503) 29(2) ? 55520 . .
C(502) O(502) C(502) 72(2) ? . . 55520
C(502) O(502) C(503) 112(2) ? . . .
C(502) O(502) C(503) 92(2) ? 55520 . .
K(4) O(503) O(501) 79.1(13) ? . . 55520
K(4) O(503) O(506) 78.7(11) ? . . 55520
K(4) O(503) C(504) 112.1(17) ? . . .
K(4) O(503) C(505) 112.7(17) ? . . .
K(4) O(503) C(512) 131(2) ? . . 55520
O(501) O(503) O(506) 110(2) ? 55520 . 55520
O(501) O(503) C(504) 37.2(17) ? 55520 . .
O(501) O(503) C(505) 115(2) ? 55520 . .
O(501) O(503) C(512) 56(2) ? 55520 . 55520
O(506) O(503) C(504) 131(3) ? 55520 . .
O(506) O(503) C(505) 34.0(14) ? 55520 . .
O(506) O(503) C(512) 97(2) ? 55520 . 55520
C(504) O(503) C(505) 114(3) ? . . .
C(504) O(503) C(512) 39(2) ? . . 55520
C(505) O(503) C(512) 75(2) ? . . 55520
K(4) O(504) O(505) 79.1(10) ? . . 55520
K(4) O(504) O(506) 80.6(13) ? . . 55520
K(4) O(504) C(506) 112.5(18) ? . . .
K(4) O(504) C(507) 117.9(10) ? . . .
K(4) O(504) C(509) 141.7(10) ? . . 55520
K(4) O(504) C(510) 129.5(18) ? . . 55520
O(505) O(504) O(506) 132.5(17) ? 55520 . 55520
O(505) O(504) C(506) 167(2) ? 55520 . .
O(505) O(504) C(507) 64.6(12) ? 55520 . .
O(505) O(504) C(509) 62.9(14) ? 55520 . 55520
O(505) O(504) C(510) 108.2(18) ? 55520 . 55520
O(506) O(504) C(506) 48.4(16) ? 55520 . .
O(506) O(504) C(507) 159.1(13) ? 55520 . .
O(506) O(504) C(509) 129(2) ? 55520 . 55520
O(506) O(504) C(510) 57.3(17) ? 55520 . 55520
C(506) O(504) C(507) 112.0(17) ? . . .
C(506) O(504) C(509) 105.8(17) ? . . 55520
C(506) O(504) C(510) 60.2(18) ? . . 55520
C(507) O(504) C(509) 41.3(16) ? . . 55520
C(507) O(504) C(510) 110(2) ? . . 55520
C(509) O(504) C(510) 71.6(19) ? 55520 . 55520
K(4) O(505) O(504) 69.6(12) ? . . 55520
K(4) O(505) C(507) 105.1(12) ? . . 55520
K(4) O(505) C(508) 112.9(11) ? . . .
K(4) O(505) C(509) 113.0(15) ? . . .
O(504) O(505) C(507) 53.7(12) ? 55520 . 55520
O(504) O(505) C(508) 124.8(10) ? 55520 . .
O(504) O(505) C(509) 43.6(14) ? 55520 . .
C(507) O(505) C(508) 74.6(10) ? 55520 . .
C(507) O(505) C(509) 35.6(10) ? 55520 . .
C(508) O(505) C(509) 102.8(16) ? . . .
K(4) O(506) O(503) 65.9(11) ? . . 55520
K(4) O(506) O(504) 68.0(10) ? . . 55520
K(4) O(506) C(505) 121(2) ? . . 55520
K(4) O(506) C(506) 112(2) ? . . 55520
K(4) O(506) C(510) 117.7(15) ? . . .
K(4) O(506) C(511) 119.1(18) ? . . .
O(503) O(506) O(504) 120(2) ? 55520 . 55520
O(503) O(506) C(505) 55(2) ? 55520 . 55520
O(503) O(506) C(506) 103(2) ? 55520 . 55520
O(503) O(506) C(510) 168(2) ? 55520 . .
O(503) O(506) C(511) 72(2) ? 55520 . .
O(504) O(506) C(505) 143(3) ? 55520 . 55520
O(504) O(506) C(506) 61.7(17) ? 55520 . 55520
O(504) O(506) C(510) 56.2(17) ? 55520 . .
O(504) O(506) C(511) 168(2) ? 55520 . .
C(505) O(506) C(506) 83(2) ? 55520 . 55520
C(505) O(506) C(510) 120(2) ? 55520 . .
C(505) O(506) C(511) 44(2) ? 55520 . .
C(506) O(506) C(510) 65(2) ? 55520 . .
C(506) O(506) C(511) 119(2) ? 55520 . .
C(510) O(506) C(511) 113(2) ? . . .
K(5) O(601) K(55) 25.6(6) ? . . .
K(5) O(601) C(601) 118(4) ? . . .
K(5) O(601) C(612) 124(2) ? . . .
K(55) O(601) C(601) 111(4) ? . . .
K(55) O(601) C(612) 107(3) ? . . .
C(601) O(601) C(612) 103(2) ? . . .
K(5) O(602) K(55) 26.5(6) ? . . .
K(5) O(602) O(605) 58(2) ? . . 55507
K(5) O(602) C(602) 115(3) ? . . .
K(5) O(602) C(603) 110(4) ? . . .
K(5) O(602) C(609) 110(5) ? . . 55507
K(55) O(602) O(605) 85(2) ? . . 55507
K(55) O(602) C(602) 110(3) ? . . .
K(55) O(602) C(603) 131(4) ? . . .
K(55) O(602) C(609) 128(6) ? . . 55507
O(605) O(602) C(602) 106(5) ? 55507 . .
O(605) O(602) C(603) 61(4) ? 55507 . .
O(605) O(602) C(609) 66(5) ? 55507 . 55507
C(602) O(602) C(603) 112(4) ? . . .
C(602) O(602) C(609) 118(6) ? . . 55507
C(603) O(602) C(609) 9(6) ? . . 55507
K(5) O(603) C(604) 124(5) ? . . .
K(5) O(603) C(605) 112(5) ? . . .
C(604) O(603) C(605) 114(6) ? . . .
K(5) O(604) C(606) 114(5) ? . . .
K(5) O(604) C(607) 109(4) ? . . .
C(606) O(604) C(607) 113(7) ? . . .
K(5) O(605) K(55) 26.1(7) ? . . .
K(5) O(605) O(602) 92(3) ? . . 55507
K(5) O(605) C(603) 133(4) ? . . 55507
K(5) O(605) C(608) 112(4) ? . . .
K(5) O(605) C(609) 118(4) ? . . .
K(55) O(605) O(602) 65(2) ? . . 55507
K(55) O(605) C(603) 113(4) ? . . 55507
K(55) O(605) C(608) 115(4) ? . . .
K(55) O(605) C(609) 95(3) ? . . .
O(602) O(605) C(603) 57(4) ? 55507 . 55507
O(602) O(605) C(608) 102(6) ? 55507 . .
O(602) O(605) C(609) 39(3) ? 55507 . .
C(603) O(605) C(608) 108(5) ? 55507 . .
C(603) O(605) C(609) 19(3) ? 55507 . .
C(608) O(605) C(609) 113(6) ? . . .
K(5) O(606) K(55) 27.5(7) ? . . .
K(5) O(606) C(610) 107(3) ? . . .
K(5) O(606) C(611) 118.6(17) ? . . .
K(55) O(606) C(610) 127(4) ? . . .
K(55) O(606) C(611) 113.7(17) ? . . .
C(610) O(606) C(611) 115(5) ? . . .
C(701) O(701) C(701) 157(7) ? . . 55520
C(701) O(701) C(712) 100(3) ? . . .
C(701) O(701) C(712) 75(2) ? . . 55520
C(701) O(701) C(712) 75(2) ? 55520 . .
C(701) O(701) C(712) 100(3) ? 55520 . 55520
C(712) O(701) C(712) 153(5) ? . . 55520
K(6) O(702) O(706) 146(12) ? . . 55520
K(6) O(702) C(702) 126(3) ? . . .
K(6) O(702) C(703) 118(6) ? . . .
K(6) O(702) C(711) 144(4) ? . . 55520
O(706) O(702) C(702) 68(12) ? 55520 . .
O(706) O(702) C(703) 69(9) ? 55520 . .
O(706) O(702) C(711) 56(12) ? 55520 . 55520
C(702) O(702) C(703) 114(6) ? . . .
C(702) O(702) C(711) 18(2) ? . . 55520
C(703) O(702) C(711) 96(6) ? . . 55520
K(6) O(703) C(704) 107(6) ? . . .
K(6) O(703) C(705) 100(6) ? . . .
C(704) O(703) C(705) 110(10) ? . . .
K(6) O(704) C(706) 118(7) ? . . .
K(6) O(704) C(707) 128(7) ? . . .
C(706) O(704) C(707) 111(10) ? . . .
K(6) O(705) C(708) 99(6) ? . . .
K(6) O(705) C(709) 112(6) ? . . .
C(708) O(705) C(709) 115(9) ? . . .
O(702) O(706) C(702) 88(12) ? 55520 . 55520
O(702) O(706) C(703) 87(10) ? 55520 . 55520
O(702) O(706) C(710) 143(15) ? 55520 . .
O(702) O(706) C(711) 104(13) ? 55520 . .
C(702) O(706) C(703) 128(7) ? 55520 . 55520
C(702) O(706) C(710) 121(7) ? 55520 . .
C(702) O(706) C(711) 22(3) ? 55520 . .
C(703) O(706) C(710) 90(7) ? 55520 . .
C(703) O(706) C(711) 113(7) ? 55520 . .
C(710) O(706) C(711) 111(7) ? . . .
S(1) O(901) S(1) 148.2 ? . . 55506
O(201) C(201) O(211) 6.7 ? . . .
O(201) C(201) C(202) 109.5 ? . . .
O(211) C(201) C(202) 113.7 ? . . .
O(202) C(202) C(201) 107(2) ? . . .
O(202) C(203) C(204) 110(3) ? . . .
O(203) C(204) C(203) 96(2) ? . . .
O(203) C(205) C(206) 100(2) ? . . .
O(204) C(206) C(205) 101(2) ? . . .
O(204) C(207) C(208) 108(2) ? . . .
O(205) C(208) C(207) 106(2) ? . . .
O(205) C(209) C(210) 105(2) ? . . .
O(206) C(210) C(209) 110(2) ? . . .
O(206) C(211) C(212) 104(2) ? . . .
O(201) C(212) O(211) 25.8 ? . . .
O(201) C(212) C(211) 102.5 ? . . .
O(211) C(212) C(211) 128.2 ? . . .
O(301) C(301) C(302) 105(3) ? . . .
O(302) C(302) C(301) 102(3) ? . . .
O(302) C(303) C(304) 105(3) ? . . .
O(303) C(304) C(303) 101(3) ? . . .
O(303) C(305) C(306) 95(4) ? . . .
O(304) C(306) C(305) 115(5) ? . . .
O(304) C(307) C(308) 94(2) ? . . .
O(305) C(308) C(307) 107(3) ? . . .
O(305) C(309) C(310) 111(4) ? . . .
O(306) C(310) C(309) 103(4) ? . . .
O(306) C(311) C(312) 112(4) ? . . .
O(301) C(312) C(311) 122(4) ? . . .
O(401) C(401) C(402) 117(4) ? . . .
O(402) C(402) C(401) 96(3) ? . . .
O(402) C(403) C(404) 89(4) ? . . .
K(3) C(404) O(403) 76(3) ? . . .
K(3) C(404) C(403) 96(4) ? . . .
K(3) C(404) C(405) 139(7) ? . . .
O(403) C(404) C(403) 126(6) ? . . .
O(403) C(404) C(405) 64(7) ? . . .
C(403) C(404) C(405) 101(8) ? . . .
O(403) C(405) C(404) 76(7) ? . . .
O(501) C(501) O(502) 87(2) ? . . 55520
O(501) C(501) C(502) 108(2) ? . . .
O(501) C(501) C(503) 103(3) ? . . 55520
O(501) C(501) C(504) 40.5(19) ? . . 55520
O(502) C(501) C(502) 49(2) ? 55520 . .
O(502) C(501) C(503) 81(4) ? 55520 . 55520
O(502) C(501) C(504) 111(2) ? 55520 . 55520
C(502) C(501) C(503) 117(4) ? . . 55520
C(502) C(501) C(504) 148(2) ? . . 55520
C(503) C(501) C(504) 76(3) ? 55520 . 55520
O(502) C(502) O(502) 50(2) ? . . 55520
O(502) C(502) C(501) 111(2) ? . . .
O(502) C(502) C(502) 46.3(18) ? . . 55520
O(502) C(502) C(501) 61(2) ? 55520 . .
O(502) C(502) C(502) 62(2) ? 55520 . 55520
C(501) C(502) C(502) 106(2) ? . . 55520
O(501) C(503) O(502) 74(2) ? 55520 . .
O(501) C(503) C(501) 53(3) ? 55520 . 55520
O(501) C(503) C(504) 35.3(17) ? 55520 . .
O(502) C(503) C(501) 70(3) ? . . 55520
O(502) C(503) C(504) 107(2) ? . . .
C(501) C(503) C(504) 76(4) ? 55520 . .
O(501) C(504) O(503) 83(2) ? 55520 . .
O(501) C(504) C(501) 67(2) ? 55520 . 55520
O(501) C(504) C(503) 87(3) ? 55520 . .
O(501) C(504) C(512) 96(3) ? 55520 . 55520
O(503) C(504) C(501) 124(2) ? . . 55520
O(503) C(504) C(503) 110(3) ? . . .
O(503) C(504) C(512) 66(3) ? . . 55520
C(501) C(504) C(503) 28(2) ? 55520 . .
C(501) C(504) C(512) 158(4) ? 55520 . 55520
C(503) C(504) C(512) 174(4) ? . . 55520
O(503) C(505) O(506) 91(2) ? . . 55520
O(503) C(505) C(506) 108(2) ? . . .
O(503) C(505) C(511) 100(3) ? . . 55520
O(503) C(505) C(512) 51(2) ? . . 55520
O(506) C(505) C(506) 56(2) ? 55520 . .
O(506) C(505) C(511) 93(3) ? 55520 . 55520
O(506) C(505) C(512) 119(2) ? 55520 . 55520
C(506) C(505) C(511) 137(3) ? . . 55520
C(506) C(505) C(512) 158(3) ? . . 55520
C(511) C(505) C(512) 60(2) ? 55520 . 55520
O(504) C(506) O(506) 69.9(16) ? . . 55520
O(504) C(506) C(505) 110(2) ? . . .
O(504) C(506) C(510) 58.2(15) ? . . 55520
O(506) C(506) C(505) 41.0(18) ? 55520 . .
O(506) C(506) C(510) 64(2) ? 55520 . 55520
C(505) C(506) C(510) 92(2) ? . . 55520
O(504) C(507) O(505) 61.7(12) ? . . 55520
O(504) C(507) C(508) 106.3(12) ? . . .
O(504) C(507) C(509) 52(2) ? . . 55520
O(505) C(507) C(508) 47.0(8) ? 55520 . .
O(505) C(507) C(509) 63.3(11) ? 55520 . 55520
C(508) C(507) C(509) 101.8(11) ? . . 55520
O(505) C(508) O(505) 94(2) ? . . 55520
O(505) C(508) C(507) 100.9(14) ? . . .
O(505) C(508) C(507) 58.4(9) ? . . 55520
O(505) C(508) C(507) 58.4(9) ? 55520 . .
O(505) C(508) C(507) 100.9(14) ? 55520 . 55520
C(507) C(508) C(507) 152(2) ? . . 55520
O(504) C(509) O(505) 73.5(15) ? 55520 . .
O(504) C(509) C(507) 87(2) ? 55520 . 55520
O(504) C(509) C(510) 63.7(19) ? 55520 . .
O(505) C(509) C(507) 81.0(11) ? . . 55520
O(505) C(509) C(510) 109.7(19) ? . . .
C(507) C(509) C(510) 142(2) ? 55520 . .
O(504) C(510) O(506) 67(2) ? 55520 . .
O(504) C(510) C(506) 61.6(16) ? 55520 . 55520
O(504) C(510) C(509) 44.6(16) ? 55520 . .
O(506) C(510) C(506) 51.2(18) ? . . 55520
O(506) C(510) C(509) 111(2) ? . . .
C(506) C(510) C(509) 89(2) ? 55520 . .
O(506) C(511) C(505) 44(2) ? . . 55520
O(506) C(511) C(512) 108(3) ? . . .
C(505) C(511) C(512) 85(3) ? 55520 . .
O(501) C(512) O(503) 72(2) ? . . 55520
O(501) C(512) C(504) 44(2) ? . . 55520
O(501) C(512) C(505) 111(2) ? . . 55520
O(501) C(512) C(511) 108(2) ? . . .
O(503) C(512) C(504) 75(3) ? 55520 . 55520
O(503) C(512) C(505) 54(2) ? 55520 . 55520
O(503) C(512) C(511) 82(2) ? 55520 . .
C(504) C(512) C(505) 129(4) ? 55520 . 55520
C(504) C(512) C(511) 148(3) ? 55520 . .
C(505) C(512) C(511) 35(2) ? 55520 . .
O(601) C(601) C(602) 111(3) ? . . .
O(602) C(602) C(601) 109(4) ? . . .
O(602) C(603) O(605) 62(4) ? . . 55507
O(602) C(603) C(604) 109(5) ? . . .
O(602) C(603) C(609) 18(11) ? . . 55507
O(602) C(603) C(610) 79(4) ? . . 55507
O(605) C(603) C(604) 91(5) ? 55507 . .
O(605) C(603) C(609) 74(10) ? 55507 . 55507
O(605) C(603) C(610) 100(4) ? 55507 . 55507
C(604) C(603) C(609) 96(13) ? . . 55507
C(604) C(603) C(610) 40(4) ? . . 55507
C(609) C(603) C(610) 61(13) ? 55507 . 55507
O(603) C(604) C(603) 110(6) ? . . .
O(603) C(604) C(609) 104(5) ? . . 55507
O(603) C(604) C(610) 109(6) ? . . 55507
C(603) C(604) C(609) 18(3) ? . . 55507
C(603) C(604) C(610) 78(7) ? . . 55507
C(609) C(604) C(610) 63(6) ? 55507 . 55507
O(603) C(605) C(606) 112(6) ? . . .
O(604) C(606) C(605) 109(7) ? . . .
O(604) C(607) C(608) 110(6) ? . . .
O(605) C(608) C(607) 109(6) ? . . .
O(602) C(609) O(605) 75(5) ? 55507 . .
O(602) C(609) C(603) 153(17) ? 55507 . 55507
O(602) C(609) C(604) 132(6) ? 55507 . 55507
O(602) C(609) C(610) 104(6) ? 55507 . .
O(605) C(609) C(603) 87(12) ? . . 55507
O(605) C(609) C(604) 88(5) ? . . 55507
O(605) C(609) C(610) 111(5) ? . . .
C(603) C(609) C(604) 67(13) ? 55507 . 55507
C(603) C(609) C(610) 101(15) ? 55507 . .
C(604) C(609) C(610) 41(4) ? 55507 . .
O(606) C(610) C(603) 125(6) ? . . 55507
O(606) C(610) C(604) 129(5) ? . . 55507
O(606) C(610) C(609) 109(5) ? . . .
C(603) C(610) C(604) 62(6) ? 55507 . 55507
C(603) C(610) C(609) 17(3) ? 55507 . .
C(604) C(610) C(609) 77(6) ? 55507 . .
O(606) C(611) C(612) 113(4) ? . . .
O(601) C(612) O(601) 136(5) ? . . 55512
O(601) C(612) C(611) 93.9(16) ? . . .
O(601) C(612) C(611) 88.5(16) ? . . 55512
O(601) C(612) C(611) 88.5(16) ? 55512 . .
O(601) C(612) C(611) 93.9(16) ? 55512 . 55512
C(611) C(612) C(611) 174(6) ? . . 55512
O(701) C(701) C(702) 97(3) ? . . .
O(702) C(702) O(706) 24(4) ? . . 55520
O(702) C(702) C(701) 112(6) ? . . .
O(702) C(702) C(711) 105(13) ? . . 55520
O(702) C(702) C(712) 102(5) ? . . 55520
O(706) C(702) C(701) 126(6) ? 55520 . .
O(706) C(702) C(711) 88(13) ? 55520 . 55520
O(706) C(702) C(712) 120(6) ? 55520 . 55520
C(701) C(702) C(711) 142(15) ? . . 55520
C(701) C(702) C(712) 84(3) ? . . 55520
C(711) C(702) C(712) 93(10) ? 55520 . 55520
O(702) C(703) O(706) 24(4) ? . . 55520
O(702) C(703) C(704) 109(7) ? . . .
O(706) C(703) C(704) 119(8) ? 55520 . .
O(703) C(704) C(703) 107(9) ? . . .
O(703) C(705) C(706) 107(9) ? . . .
O(704) C(706) C(705) 110(10) ? . . .
O(704) C(707) C(708) 107(10) ? . . .
O(705) C(708) C(707) 111(9) ? . . .
O(705) C(709) C(710) 109(8) ? . . .
O(706) C(710) C(709) 109(8) ? . . .
O(702) C(711) O(706) 20(3) ? 55520 . .
O(702) C(711) C(702) 57(13) ? 55520 . 55520
O(702) C(711) C(712) 87(5) ? 55520 . .
O(706) C(711) C(702) 70(13) ? . . 55520
O(706) C(711) C(712) 107(6) ? . . .
C(702) C(711) C(712) 66(9) ? 55520 . .
O(701) C(712) C(702) 87(3) ? . . 55520
O(701) C(712) C(711) 108(3) ? . . .
C(702) C(712) C(711) 21(3) ? 55520 . .
S(1) C(901) S(11) 71.4 ? . . .
S(1) C(911) S(11) 70.5 ? . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
W(3) O(3) 1.898(9) ? . .
W(3) O(7) 1.944(10) ? . .
W(3) O(12) 1.918(11) ? . .
W(3) O(13) 1.918(10) ? . .
W(3) O(26) 2.324(9) ? . .
W(3) O(103) 1.710(11) ? . .
W(4) O(4) 1.880(9) ? . .
W(4) O(8) 1.943(10) ? . .
W(4) O(9) 1.919(10) ? . .
W(4) O(14) 1.934(9) ? . .
W(4) O(25) 2.320(9) ? . .
W(4) O(104) 1.716(10) ? . .
W(5) O(5) 1.883(8) ? . .
W(5) O(9) 1.924(10) ? . .
W(5) O(10) 1.926(9) ? . .
W(5) O(15) 1.928(9) ? . .
W(5) O(25) 2.330(9) ? . .
W(5) O(105) 1.697(10) ? . .
W(6) O(6) 1.876(8) ? . .
W(6) O(11) 1.928(10) ? . .
W(6) O(12) 1.926(11) ? . .
W(6) O(16) 1.926(9) ? . .
W(6) O(26) 2.319(9) ? . .
W(6) O(106) 1.708(11) ? . .
W(7) O(7) 1.890(10) ? . .
W(7) O(8) 1.895(9) ? . .
W(7) O(17) 1.948(10) ? . .
W(7) O(18) 1.944(9) ? . .
W(7) O(27) 2.333(8) ? . .
W(7) O(107) 1.725(10) ? . .
W(8) O(10) 1.929(9) ? . .
W(8) O(11) 1.922(9) ? . .
W(8) O(19) 1.929(9) ? . .
W(8) O(20) 1.914(9) ? . .
W(8) O(28) 2.351(8) ? . .
W(8) O(108) 1.722(9) ? . .
W(9) O(13) 1.914(10) ? . .
W(9) O(17) 1.895(10) ? . .
W(9) O(21) 1.924(10) ? . .
W(9) O(24) 1.935(9) ? . .
W(9) O(27) 2.363(9) ? . .
W(9) O(109) 1.716(11) ? . .
W(10) O(14) 1.890(9) ? . .
W(10) O(18) 1.895(9) ? . .
W(10) O(21) 1.924(10) ? . .
W(10) O(22) 1.931(9) ? . .
W(10) O(27) 2.357(8) ? . .
W(10) O(110) 1.713(10) ? . .
W(11) O(15) 1.902(9) ? . .
W(11) O(19) 1.927(10) ? . .
W(11) O(22) 1.881(9) ? . .
W(11) O(23) 1.908(10) ? . .
W(11) O(28) 2.354(8) ? . .
W(11) O(111) 1.724(10) ? . .
W(12) O(16) 1.897(9) ? . .
W(12) O(20) 1.934(10) ? . .
W(12) O(23) 1.922(10) ? . .
W(12) O(24) 1.875(9) ? . .
W(12) O(28) 2.365(8) ? . .
W(12) O(112) 1.713(11) ? . .
Ti(1) Ti(2) 3.158(3) ? . .
Ti(1) O(1) 1.974(9) ? . .
Ti(1) O(2) 2.008(9) ? . .
Ti(1) O(3) 1.858(10) ? . .
Ti(1) O(6) 1.873(10) ? . .
Ti(1) O(26) 2.397(8) ? . .
Ti(1) O(101) 1.804(9) ? . 55506
Ti(2) O(1) 1.974(9) ? . .
Ti(2) O(2) 2.014(10) ? . .
Ti(2) O(4) 1.866(9) ? . .
Ti(2) O(5) 1.873(9) ? . .
Ti(2) O(25) 2.401(8) ? . .
Ti(2) O(101) 1.807(9) ? . .
K(1) K(11) 0.922(14) ? . .
K(1) O(201) 2.800 ? . .
K(1) O(202) 2.76(2) ? . .
K(1) O(203) 2.90(2) ? . .
K(1) O(204) 2.729(19) ? . .
K(1) O(205) 2.79(2) ? . .
K(1) O(206) 2.75(2) ? . .
K(1) O(211) 2.999 ? . .
K(2) O(301) 2.84(3) ? . .
K(2) O(302) 2.77(2) ? . .
K(2) O(303) 2.84(3) ? . .
K(2) O(304) 2.88(2) ? . .
K(2) O(305) 2.85(3) ? . .
K(2) O(306) 2.81(3) ? . .
K(3) O(401) 2.93(5) ? . .
K(3) O(401) 2.93(5) ? . 55520
K(3) O(402) 2.67(3) ? . .
K(3) O(402) 2.67(3) ? . 55520
K(3) O(403) 3.19(4) ? . .
K(3) O(403) 3.19(4) ? . 55520
K(3) C(404) 3.18(8) ? . .
K(3) C(404) 3.18(8) ? . 55520
K(5) K(55) 1.40(2) ? . .
K(6) O(702) 2.92(7) ? . .
K(6) O(702) 2.92(7) ? . 55520
K(6) O(703) 2.92(9) ? . .
K(6) O(703) 2.92(9) ? . 55520
K(6) O(704) 2.74(10) ? . .
K(6) O(704) 2.74(10) ? . 55520
K(6) O(705) 3.18(9) ? . .
K(6) O(705) 3.18(9) ? . 55520
K(11) O(201) 2.658 ? . .
K(11) O(202) 2.84(2) ? . .
K(11) O(203) 2.84(2) ? . .
K(11) O(204) 2.77(2) ? . .
K(11) O(205) 2.72(2) ? . .
K(11) O(206) 2.83(2) ? . .
K(11) O(211) 2.971 ? . .
K(55) K(55) 3.41(3) ? . 55506
S(1) S(11) 2.016 ? . .
S(1) O(901) 1.917 ? . .
S(1) C(901) 1.780 ? . .
S(1) C(911) 1.776 ? . .
S(11) O(911) 1.535 ? . .
S(11) C(901) 1.674 ? . .
S(11) C(911) 1.717 ? . .
Si(1) O(25) 1.641(9) ? . .
Si(1) O(26) 1.638(9) ? . .
Si(1) O(27) 1.627(9) ? . .
Si(1) O(28) 1.626(8) ? . .
O(201) O(211) 0.667 ? . .
O(201) C(201) 1.783 ? . .
O(201) C(212) 1.285 ? . .
O(202) C(202) 1.38(3) ? . .
O(202) C(203) 1.49(4) ? . .
O(203) C(204) 1.59(4) ? . .
O(203) C(205) 1.50(4) ? . .
O(204) C(206) 1.48(3) ? . .
O(204) C(207) 1.44(3) ? . .
O(205) C(208) 1.41(3) ? . .
O(205) C(209) 1.44(3) ? . .
O(206) C(210) 1.38(4) ? . .
O(206) C(211) 1.50(4) ? . .
O(211) C(201) 1.137 ? . .
O(211) C(212) 1.521 ? . .
O(301) C(301) 1.33(5) ? . .
O(301) C(312) 1.47(6) ? . .
O(302) C(302) 1.43(5) ? . .
O(302) C(303) 1.45(4) ? . .
O(303) C(304) 1.38(6) ? . .
O(303) C(305) 1.71(8) ? . .
O(304) C(306) 1.24(8) ? . .
O(304) C(307) 1.48(3) ? . .
O(305) C(308) 1.42(6) ? . .
O(305) C(309) 1.40(7) ? . .
O(306) C(310) 1.37(6) ? . .
O(306) C(311) 1.33(7) ? . .
O(401) C(401) 1.37(6) ? . .
O(401) C(406) 1.38(9) ? . .
O(402) C(402) 1.24(5) ? . .
O(402) C(403) 1.70(6) ? . .
O(403) C(404) 1.61(9) ? . .
O(403) C(405) 1.49(11) ? . .
O(501) O(503) 1.66(4) ? . 55520
O(501) C(501) 1.43(4) ? . .
O(501) C(503) 1.74(4) ? . 55520
O(501) C(504) 1.01(4) ? . 55520
O(501) C(512) 1.45(4) ? . .
O(502) O(502) 1.14(4) ? . 55520
O(502) C(501) 1.38(4) ? . 55520
O(502) C(502) 1.45(4) ? . .
O(502) C(502) 1.18(4) ? . 55520
O(502) C(503) 1.45(4) ? . .
O(503) O(506) 1.74(4) ? . 55520
O(503) C(504) 1.44(4) ? . .
O(503) C(505) 1.43(4) ? . .
O(503) C(512) 1.37(4) ? . 55520
O(504) O(505) 1.53(2) ? . 55520
O(504) O(506) 1.55(3) ? . 55520
O(504) C(506) 1.46(2) ? . .
O(504) C(507) 1.40(3) ? . .
O(504) C(509) 1.10(3) ? . 55520
O(504) C(510) 1.41(3) ? . 55520
O(505) C(507) 1.572(17) ? . 55520
O(505) C(508) 1.35(2) ? . .
O(505) C(509) 1.422(16) ? . .
O(506) C(505) 0.97(3) ? . 55520
O(506) C(506) 1.24(3) ? . 55520
O(506) C(510) 1.42(4) ? . .
O(506) C(511) 1.41(4) ? . .
O(601) C(601) 1.47(2) ? . .
O(601) C(612) 1.58(4) ? . .
O(602) O(605) 1.57(9) ? . 55507
O(602) C(602) 1.46(11) ? . .
O(602) C(603) 1.48(9) ? . .
O(602) C(609) 1.01(9) ? . 55507
O(603) C(604) 1.43(11) ? . .
O(603) C(605) 1.46(9) ? . .
O(604) C(606) 1.45(12) ? . .
O(604) C(607) 1.47(12) ? . .
O(605) C(603) 1.55(9) ? . 55507
O(605) C(608) 1.43(10) ? . .
O(605) C(609) 1.49(9) ? . .
O(606) C(610) 1.46(4) ? . .
O(606) C(611) 1.48(9) ? . .
O(701) C(701) 1.37(2) ? . .
O(701) C(701) 1.37(2) ? . 55520
O(701) C(712) 1.79(3) ? . .
O(701) C(712) 1.79(3) ? . 55520
O(702) O(706) 0.59(10) ? . 55520
O(702) C(702) 1.47(13) ? . .
O(702) C(703) 1.47(9) ? . .
O(702) C(711) 1.69(13) ? . 55520
O(703) C(704) 1.44(16) ? . .
O(703) C(705) 1.48(13) ? . .
O(704) C(706) 1.50(18) ? . .
O(704) C(707) 1.44(17) ? . .
O(705) C(708) 1.49(14) ? . .
O(705) C(709) 1.49(15) ? . .
O(706) C(702) 1.36(13) ? . 55520
O(706) C(703) 1.37(10) ? . 55520
O(706) C(710) 1.44(11) ? . .
O(706) C(711) 1.45(13) ? . .
C(201) C(202) 1.39(4) ? . .
C(203) C(204) 1.63(6) ? . .
C(205) C(206) 1.55(4) ? . .
C(207) C(208) 1.55(4) ? . .
C(209) C(210) 1.56(5) ? . .
C(211) C(212) 1.47(5) ? . .
C(301) C(302) 1.65(6) ? . .
C(303) C(304) 1.58(6) ? . .
C(305) C(306) 1.64(10) ? . .
C(307) C(308) 1.42(5) ? . .
C(309) C(310) 1.40(8) ? . .
C(311) C(312) 1.61(8) ? . .
C(401) C(402) 1.56(5) ? . .
C(403) C(404) 1.35(9) ? . .
C(404) C(405) 1.07(16) ? . .
C(501) C(502) 1.47(4) ? . .
C(501) C(503) 0.71(5) ? . 55520
C(501) C(504) 1.48(4) ? . 55520
C(502) C(502) 1.55(5) ? . 55520
C(503) C(504) 1.48(4) ? . .
C(504) C(512) 0.94(4) ? . 55520
C(505) C(506) 1.47(4) ? . .
C(505) C(511) 0.97(5) ? . 55520
C(505) C(512) 1.71(4) ? . 55520
C(506) C(510) 1.44(4) ? . 55520
C(507) C(508) 1.778(9) ? . .
C(507) C(509) 0.93(2) ? . 55520
C(509) C(510) 1.49(3) ? . .
C(511) C(512) 1.48(4) ? . .
C(601) C(602) 1.50(6) ? . .
C(603) C(604) 1.51(11) ? . .
C(603) C(609) 0.51(9) ? . 55507
C(603) C(610) 1.67(11) ? . 55507
C(604) C(609) 1.64(11) ? . 55507
C(604) C(610) 1.10(10) ? . 55507
C(605) C(606) 1.51(13) ? . .
C(607) C(608) 1.53(12) ? . .
C(609) C(610) 1.50(11) ? . .
C(611) C(612) 1.69(2) ? . .
C(701) C(702) 1.55(6) ? . .
C(702) C(711) 0.54(8) ? . 55520
C(702) C(712) 1.36(8) ? . 55520
C(703) C(704) 1.54(16) ? . .
C(705) C(706) 1.5(2) ? . .
C(707) C(708) 1.54(19) ? . .
C(709) C(710) 1.52(16) ? . .
C(711) C(712) 1.49(8) ? . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
K(3) C(403) 3.58(4) ? . .
K(3) C(403) 3.58(4) ? . 55520
K(4) O(501) 2.92(2) ? . .
K(4) O(501) 2.92(3) ? . 55520
K(4) O(502) 2.71(2) ? . .
K(4) O(502) 2.71(2) ? . 55520
K(4) O(503) 2.74(2) ? . .
K(4) O(503) 2.74(2) ? . 55520
K(4) O(504) 2.76(2) ? . .
K(4) O(504) 2.76(2) ? . 55520
K(4) O(505) 2.90(2) ? . .
K(4) O(505) 2.90(2) ? . 55520
K(4) O(506) 2.94(2) ? . .
K(4) O(506) 2.94(2) ? . 55520
K(4) C(504) 3.54(3) ? . .
K(4) C(504) 3.54(3) ? . 55520
K(4) C(505) 3.54(2) ? . .
K(4) C(505) 3.54(2) ? . 55520
K(4) C(506) 3.584(19) ? . .
K(4) C(506) 3.584(19) ? . 55520
K(5) O(601) 3.16(5) ? . .
K(5) O(601) 3.16(5) ? . 55507
K(5) O(602) 3.13(4) ? . .
K(5) O(602) 3.13(4) ? . 55507
K(5) O(603) 2.81(7) ? . .
K(5) O(603) 2.81(7) ? . 55507
K(5) O(604) 2.61(6) ? . .
K(5) O(604) 2.61(6) ? . 55507
K(5) O(605) 2.66(6) ? . .
K(5) O(605) 2.66(6) ? . 55507
K(5) O(606) 3.01(4) ? . .
K(5) O(606) 3.01(4) ? . 55507
K(5) C(606) 3.45(7) ? . .
K(5) C(606) 3.45(7) ? . 55507
K(5) C(607) 3.40(8) ? . .
K(5) C(607) 3.40(8) ? . 55507
K(5) C(608) 3.46(7) ? . .
K(5) C(608) 3.46(7) ? . 55507
K(6) O(701) 3.41(7) ? . .
K(6) O(706) 3.42(7) ? . .
K(6) O(706) 3.42(7) ? . 55520
K(6) C(705) 3.50(11) ? . .
K(6) C(705) 3.50(11) ? . 55520
K(55) O(601) 2.54(6) ? . .
K(55) O(601) 2.54(6) ? . 55507
K(55) O(602) 2.88(4) ? . .
K(55) O(602) 2.88(4) ? . 55507
K(55) O(603) 3.47(7) ? . .
K(55) O(603) 3.47(7) ? . 55507
K(55) O(604) 3.45(7) ? . .
K(55) O(604) 3.45(7) ? . 55507
K(55) O(605) 3.15(6) ? . .
K(55) O(605) 3.15(6) ? . 55507
K(55) O(606) 2.51(5) ? . .
K(55) O(606) 2.51(5) ? . 55507
K(55) C(601) 3.36(5) ? . .
K(55) C(601) 3.36(5) ? . 55507
K(55) C(610) 3.58(5) ? . .
K(55) C(610) 3.58(4) ? . 55507
K(55) C(611) 3.38(6) ? . .
K(55) C(611) 3.38(6) ? . 55507
K(55) C(612) 3.37(6) ? . .
K(55) C(612) 3.37(6) ? . 55506
S(1) O(3) 3.374 ? . 55506
S(1) O(4) 3.429 ? . .
O(1) O(901) 2.720 ? . .
O(2) C(602) 3.29(3) ? . 55506
O(3) S(1) 3.374 ? . 55506
O(4) S(1) 3.429 ? . .
O(4) C(506) 3.33(2) ? . 54531
O(5) C(506) 3.49(2) ? . 54531
O(5) C(603) 3.15(7) ? . .
O(5) C(604) 2.86(7) ? . .
O(5) C(609) 3.45(7) ? . 55507
O(5) C(610) 3.11(4) ? . 55507
O(6) C(512) 3.34(3) ? . .
O(6) C(602) 3.19(4) ? . 55506
O(6) C(603) 3.54(7) ? . 55506
O(6) C(608) 3.38(8) ? . 55512
O(7) C(911) 3.20(2) ? . 55506
O(8) C(901) 3.24(2) ? . .
O(9) C(402) 3.40(3) ? . 55506
O(9) C(506) 3.21(2) ? . 54531
O(9) C(507) 3.476(12) ? . 54531
O(9) C(509) 3.325(16) ? . 55506
O(9) C(510) 3.37(2) ? . 55506
O(10) C(610) 3.40(7) ? . 55507
O(11) C(601) 3.58(5) ? . 55506
O(11) C(602) 3.22(7) ? . 55506
O(12) C(501) 3.47(3) ? . .
O(12) C(503) 3.21(3) ? . 55520
O(12) C(504) 3.24(3) ? . 55520
O(12) C(512) 3.58(3) ? . .
O(12) C(705) 3.40(11) ? . 55520
O(13) C(705) 3.33(12) ? . 55520
O(13) C(706) 3.55(13) ? . 55520
O(14) C(401) 3.30(4) ? . 55506
O(14) C(402) 3.19(3) ? . 55506
O(15) C(402) 3.42(3) ? . 55506
O(17) C(201) 3.42(3) ? . 65507
O(17) C(202) 3.37(3) ? . 65507
O(18) C(207) 3.23(3) ? . 55506
O(19) C(311) 3.41(6) ? . 55506
O(19) C(312) 3.47(5) ? . 55506
O(20) C(302) 3.52(4) ? . 55507
O(20) C(702) 3.59(6) ? . 44524
O(20) C(711) 3.42(7) ? . 55529
O(21) C(307) 3.43(2) ? . 55411
O(21) C(308) 3.50(4) ? . 55411
O(22) C(307) 3.50(2) ? . 55411
O(23) C(305) 3.21(7) ? . 55411
O(23) C(307) 3.40(2) ? . 55411
O(101) C(603) 3.43(5) ? . .
O(103) C(201) 3.52(3) ? . 65507
O(103) C(202) 3.30(3) ? . 65507
O(103) C(503) 3.57(3) ? . 55520
O(103) C(706) 3.51(10) ? . 55520
O(104) C(206) 3.48(3) ? . 55506
O(105) C(312) 3.59(5) ? . 55506
O(105) C(405) 3.35(10) ? . 55506
O(105) C(510) 3.41(2) ? . 55506
O(105) C(604) 3.30(8) ? . .
O(105) C(605) 3.54(9) ? . .
O(106) C(303) 3.45(3) ? . 55507
O(106) C(608) 3.30(8) ? . 55512
O(107) C(901) 3.56(2) ? . .
O(107) C(911) 3.49(2) ? . 55506
O(108) C(601) 3.23(8) ? . 55506
O(108) C(611) 2.89(6) ? . 55507
O(108) C(612) 3.58(5) ? . 55506
O(108) C(701) 3.57(8) ? . 44524
O(109) C(212) 3.50(3) ? . 65507
O(109) C(309) 3.50(5) ? . 55411
O(109) C(310) 3.52(5) ? . 55411
O(110) C(207) 3.27(3) ? . 55506
O(110) C(208) 3.54(3) ? . 55506
O(110) C(209) 3.30(3) ? . 64410
O(110) C(401) 3.44(4) ? . 55506
O(111) C(211) 3.31(3) ? . 64410
O(111) C(311) 3.52(6) ? . 55506
O(111) C(403) 3.57(5) ? . 55506
O(112) C(303) 3.53(3) ? . 55507
O(112) C(305) 3.37(7) ? . 55411
O(112) C(703) 3.21(8) ? . 55520
O(112) C(704) 2.86(10) ? . 55520
O(112) C(709) 3.52(11) ? . .
O(112) C(710) 3.25(9) ? . 55529
O(301) C(605) 3.53(7) ? . 55506
O(301) C(712) 3.40(7) ? . 45527
O(302) C(702) 3.33(7) ? . 54526
O(302) C(711) 2.80(7) ? . 45527
O(302) C(712) 3.38(5) ? . 45527
O(303) O(705) 2.79(10) ? . 55507
O(303) C(708) 2.91(13) ? . 55507
O(303) C(709) 2.67(11) ? . 55507
O(303) C(710) 3.54(10) ? . 55507
O(306) C(405) 3.48(12) ? . .
O(401) O(402) 2.60(6) ? . .
O(401) O(403) 2.81(7) ? . 55520
O(401) C(402) 2.50(6) ? . .
O(402) O(401) 2.60(6) ? . .
O(402) O(403) 3.41(6) ? . .
O(402) C(210) 3.56(5) ? . 65513
O(402) C(401) 2.09(5) ? . .
O(402) C(404) 2.15(9) ? . .
O(402) C(405) 3.14(12) ? . .
O(403) O(401) 2.81(7) ? . 55520
O(403) O(402) 3.41(6) ? . .
O(403) C(403) 2.64(7) ? . .
O(403) C(406) 2.06(8) ? . 55520
O(501) K(4) 2.92(2) ? . .
O(501) O(502) 2.84(4) ? . .
O(501) O(502) 1.94(4) ? . 55520
O(501) O(506) 2.77(3) ? . .
O(501) C(502) 2.35(4) ? . .
O(501) C(502) 3.35(4) ? . 55520
O(501) C(505) 2.61(4) ? . 55520
O(501) C(511) 2.38(4) ? . .
O(502) K(4) 2.71(2) ? . .
O(502) O(501) 2.84(4) ? . .
O(502) O(501) 1.94(4) ? . 55520
O(502) O(503) 2.79(3) ? . .
O(502) C(501) 2.41(4) ? . .
O(502) C(503) 2.56(4) ? . 55520
O(502) C(504) 2.36(4) ? . .
O(502) C(504) 3.44(4) ? . 55520
O(502) C(512) 3.18(4) ? . 55520
O(503) K(4) 2.74(2) ? . .
O(503) O(502) 2.79(3) ? . .
O(503) O(504) 2.84(3) ? . .
O(503) C(501) 2.58(3) ? . 55520
O(503) C(503) 2.39(4) ? . .
O(503) C(506) 2.34(4) ? . .
O(503) C(510) 3.14(4) ? . 55520
O(503) C(511) 1.87(5) ? . 55520
O(504) K(4) 2.76(2) ? . .
O(504) O(503) 2.84(3) ? . .
O(504) O(505) 2.868(19) ? . .
O(504) C(505) 2.40(3) ? . .
O(504) C(508) 2.55(2) ? . .
O(504) C(511) 2.94(4) ? . 55520
O(505) K(4) 2.90(2) ? . .
O(505) O(504) 2.868(19) ? . .
O(505) O(505) 1.978(11) ? . 55520
O(505) O(506) 2.82(3) ? . .
O(505) C(506) 2.97(2) ? . 55520
O(505) C(507) 2.426(13) ? . .
O(505) C(509) 2.971(17) ? . 55520
O(505) C(510) 2.38(2) ? . .
O(506) K(4) 2.94(2) ? . .
O(506) O(501) 2.77(3) ? . .
O(506) O(505) 2.82(3) ? . .
O(506) C(504) 2.90(4) ? . 55520
O(506) C(507) 2.90(3) ? . 55520
O(506) C(509) 2.40(3) ? . .
O(506) C(512) 2.34(4) ? . .
O(601) K(5) 3.16(5) ? . .
O(601) K(55) 2.54(6) ? . .
O(601) O(601) 2.93(2) ? . 55512
O(601) O(602) 2.89(7) ? . .
O(601) O(604) 3.09(8) ? . 55507
O(601) O(605) 3.47(8) ? . 55507
O(601) O(606) 2.84(3) ? . .
O(601) O(606) 2.82(4) ? . 55512
O(601) C(601) 3.57(2) ? . 55512
O(601) C(602) 2.45(4) ? . .
O(601) C(608) 3.38(8) ? . 55507
O(601) C(611) 2.40(3) ? . .
O(601) C(611) 2.29(4) ? . 55512
O(602) K(5) 3.13(4) ? . .
O(602) K(55) 2.88(4) ? . .
O(602) O(601) 2.89(7) ? . .
O(602) O(603) 2.86(9) ? . .
O(602) O(606) 2.28(9) ? . 55507
O(602) C(601) 2.41(9) ? . .
O(602) C(601) 3.56(9) ? . 55506
O(602) C(604) 2.44(11) ? . .
O(602) C(607) 3.60(10) ? . 55507
O(602) C(608) 2.33(11) ? . 55507
O(602) C(610) 2.01(11) ? . 55507
O(603) K(5) 2.81(7) ? . .
O(603) K(55) 3.47(7) ? . .
O(603) O(602) 2.86(9) ? . .
O(603) O(604) 2.88(11) ? . .
O(603) O(605) 2.04(10) ? . 55507
O(603) O(606) 2.48(8) ? . 55507
O(603) C(603) 2.41(10) ? . .
O(603) C(606) 2.47(11) ? . .
O(603) C(608) 3.38(10) ? . 55507
O(603) C(609) 2.43(10) ? . 55507
O(603) C(610) 2.06(9) ? . 55507
O(603) C(611) 3.33(8) ? . 55507
O(604) K(5) 2.61(6) ? . .
O(604) K(55) 3.45(7) ? . .
O(604) O(601) 3.09(8) ? . 55507
O(604) O(603) 2.88(11) ? . .
O(604) O(605) 2.92(10) ? . .
O(604) C(605) 2.42(12) ? . .
O(604) C(608) 2.46(11) ? . .
O(605) K(5) 2.66(6) ? . .
O(605) K(55) 3.15(6) ? . .
O(605) O(601) 3.47(8) ? . 55507
O(605) O(603) 2.04(10) ? . 55507
O(605) O(604) 2.92(10) ? . .
O(605) O(606) 2.94(9) ? . .
O(605) C(601) 3.48(9) ? . 55507
O(605) C(602) 2.42(9) ? . 55507
O(605) C(604) 2.18(10) ? . 55507
O(605) C(605) 3.48(10) ? . 55507
O(605) C(607) 2.42(10) ? . .
O(605) C(610) 2.46(10) ? . .
O(606) K(5) 3.01(4) ? . .
O(606) K(55) 2.51(5) ? . .
O(606) O(601) 2.84(3) ? . .
O(606) O(601) 2.82(4) ? . 55512
O(606) O(602) 2.28(9) ? . 55507
O(606) O(603) 2.48(8) ? . 55507
O(606) O(605) 2.94(9) ? . .
O(606) C(601) 2.08(6) ? . 55512
O(606) C(602) 3.25(6) ? . 55512
O(606) C(603) 2.78(8) ? . 55507
O(606) C(604) 2.31(8) ? . 55507
O(606) C(605) 3.27(9) ? . 55507
O(606) C(609) 2.41(8) ? . .
O(606) C(612) 2.64(5) ? . .
O(701) K(6) 3.41(7) ? . .
O(701) O(702) 2.72(8) ? . .
O(701) O(702) 2.72(8) ? . 55520
O(701) O(706) 3.05(8) ? . .
O(701) O(706) 3.05(8) ? . 55520
O(701) C(702) 2.20(4) ? . .
O(701) C(702) 2.20(4) ? . 55520
O(701) C(711) 2.66(5) ? . .
O(701) C(711) 2.66(5) ? . 55520
O(702) O(701) 2.72(8) ? . .
O(702) O(703) 2.85(13) ? . .
O(702) O(705) 2.95(12) ? . 55520
O(702) C(701) 2.51(10) ? . .
O(702) C(704) 2.45(13) ? . .
O(702) C(709) 2.65(14) ? . 55520
O(702) C(710) 1.94(11) ? . 55520
O(702) C(712) 2.20(12) ? . 55520
O(703) O(702) 2.85(13) ? . .
O(703) O(704) 2.85(15) ? . .
O(703) O(705) 3.53(15) ? . 55520
O(703) O(706) 3.18(13) ? . 55520
O(703) C(703) 2.39(15) ? . .
O(703) C(706) 2.36(15) ? . .
O(703) C(709) 3.27(16) ? . 55520
O(704) O(703) 2.85(15) ? . .
O(704) O(705) 2.88(15) ? . .
O(704) C(705) 2.44(18) ? . .
O(704) C(708) 2.39(18) ? . .
O(705) O(303) 2.79(10) ? . 55507
O(705) O(702) 2.95(13) ? . 55520
O(705) O(703) 3.53(15) ? . 55520
O(705) O(704) 2.88(15) ? . .
O(705) O(706) 2.92(13) ? . .
O(705) C(304) 2.72(11) ? . 55507
O(705) C(305) 2.82(12) ? . 55507
O(705) C(703) 3.35(14) ? . 55520
O(705) C(704) 2.93(15) ? . 55520
O(705) C(707) 2.50(15) ? . .
O(705) C(710) 2.45(15) ? . .
O(706) K(6) 3.42(7) ? . .
O(706) O(701) 3.05(8) ? . .
O(706) O(703) 3.18(13) ? . 55520
O(706) O(705) 2.92(13) ? . .
O(706) C(701) 2.60(9) ? . 55520
O(706) C(704) 2.51(14) ? . 55520
O(706) C(709) 2.41(14) ? . .
O(706) C(712) 2.36(11) ? . .
O(901) O(1) 2.720 ? . .
O(901) O(1) 2.720 ? . 55506
O(911) C(203) 3.526 ? . 65512
C(201) O(17) 3.42(3) ? . 65507
C(201) O(103) 3.52(3) ? . 65507
C(202) O(17) 3.37(3) ? . 65507
C(202) O(103) 3.30(3) ? . 65507
C(203) O(911) 3.526 ? . 65512
C(206) O(104) 3.48(3) ? . 55506
C(207) O(18) 3.23(3) ? . 55506
C(207) O(110) 3.27(3) ? . 55506
C(208) O(110) 3.54(3) ? . 55506
C(209) O(110) 3.30(3) ? . 65502
C(210) O(402) 3.56(5) ? . 65513
C(211) O(111) 3.31(3) ? . 65502
C(212) O(109) 3.50(3) ? . 65507
C(301) C(702) 3.23(9) ? . 54526
C(301) C(711) 2.97(9) ? . 45527
C(301) C(712) 2.47(8) ? . 45527
C(302) O(20) 3.52(4) ? . 55507
C(302) C(702) 3.49(9) ? . 54526
C(302) C(711) 3.06(9) ? . 45527
C(302) C(712) 3.35(7) ? . 45527
C(303) O(106) 3.45(3) ? . 55507
C(303) O(112) 3.53(3) ? . 55507
C(303) C(709) 2.93(12) ? . 55507
C(303) C(711) 3.59(7) ? . 45527
C(304) O(705) 2.72(11) ? . 55507
C(304) C(708) 3.16(13) ? . 55507
C(304) C(709) 1.86(12) ? . 55507
C(304) C(710) 2.70(11) ? . 55507
C(305) O(23) 3.21(7) ? . 45527
C(305) O(112) 3.37(8) ? . 45527
C(305) O(705) 2.82(12) ? . 55507
C(305) C(708) 3.56(13) ? . 55507
C(305) C(709) 2.86(13) ? . 55507
C(305) C(710) 3.00(12) ? . 55507
C(307) O(21) 3.43(2) ? . 45527
C(307) O(22) 3.50(2) ? . 45527
C(307) O(23) 3.40(2) ? . 45527
C(308) O(21) 3.50(4) ? . 45527
C(309) O(109) 3.50(5) ? . 45527
C(310) O(109) 3.52(5) ? . 45527
C(311) O(19) 3.41(6) ? . 55506
C(311) O(111) 3.52(6) ? . 55506
C(312) O(19) 3.47(5) ? . 55506
C(312) O(105) 3.59(5) ? . 55506
C(312) C(712) 3.55(8) ? . 45527
C(401) O(14) 3.30(4) ? . 55506
C(401) O(110) 3.44(4) ? . 55506
C(401) O(402) 2.09(5) ? . .
C(401) C(403) 3.56(6) ? . .
C(401) C(406) 2.46(8) ? . .
C(402) O(9) 3.40(3) ? . 55506
C(402) O(14) 3.19(3) ? . 55506
C(402) O(15) 3.42(3) ? . 55506
C(402) O(401) 2.50(6) ? . .
C(402) C(403) 2.16(6) ? . .
C(402) C(404) 2.51(9) ? . .
C(402) C(405) 3.41(13) ? . .
C(403) K(3) 3.58(4) ? . .
C(403) O(111) 3.57(5) ? . 55506
C(403) O(403) 2.64(7) ? . .
C(403) C(401) 3.56(6) ? . .
C(403) C(402) 2.16(6) ? . .
C(403) C(405) 1.87(11) ? . .
C(404) O(402) 2.15(9) ? . .
C(404) C(402) 2.51(9) ? . .
C(404) C(406) 3.59(10) ? . 55520
C(405) O(105) 3.35(10) ? . 55506
C(405) O(306) 3.48(12) ? . .
C(405) O(402) 3.14(12) ? . .
C(405) C(402) 3.41(13) ? . .
C(405) C(403) 1.87(11) ? . .
C(405) C(406) 3.50(12) ? . 55520
C(406) O(403) 2.06(8) ? . 55520
C(406) C(401) 2.46(8) ? . .
C(406) C(404) 3.59(10) ? . 55520
C(406) C(405) 3.50(12) ? . 55520
C(501) O(12) 3.47(3) ? . .
C(501) O(502) 2.41(4) ? . .
C(501) O(503) 2.58(3) ? . 55520
C(501) C(502) 2.42(4) ? . 55520
C(501) C(512) 2.37(4) ? . .
C(502) O(501) 2.35(4) ? . .
C(502) O(501) 3.35(4) ? . 55520
C(502) C(501) 2.42(4) ? . 55520
C(502) C(503) 2.40(4) ? . .
C(502) C(503) 1.91(4) ? . 55520
C(502) C(504) 2.84(4) ? . 55520
C(503) O(12) 3.21(3) ? . 55520
C(503) O(103) 3.57(3) ? . 55520
C(503) O(502) 2.56(4) ? . 55520
C(503) O(503) 2.39(4) ? . .
C(503) C(502) 2.40(4) ? . .
C(503) C(502) 1.91(4) ? . 55520
C(503) C(512) 2.41(4) ? . 55520
C(504) K(4) 3.54(3) ? . .
C(504) O(12) 3.24(3) ? . 55520
C(504) O(502) 2.36(4) ? . .
C(504) O(502) 3.44(4) ? . 55520
C(504) O(506) 2.90(4) ? . 55520
C(504) C(502) 2.84(4) ? . 55520
C(504) C(505) 2.41(4) ? . .
C(504) C(511) 2.33(4) ? . 55520
C(505) K(4) 3.54(2) ? . .
C(505) O(501) 2.61(4) ? . 55520
C(505) O(504) 2.40(3) ? . .
C(505) C(504) 2.41(4) ? . .
C(505) C(509) 3.20(3) ? . 55520
C(505) C(510) 2.08(4) ? . 55520
C(506) K(4) 3.584(19) ? . .
C(506) O(4) 3.33(2) ? . 55531
C(506) O(5) 3.49(2) ? . 55531
C(506) O(9) 3.21(2) ? . 55531
C(506) O(503) 2.34(4) ? . .
C(506) O(505) 2.97(2) ? . 55520
C(506) C(507) 2.37(3) ? . .
C(506) C(509) 2.05(3) ? . 55520
C(506) C(511) 2.28(4) ? . 55520
C(506) C(512) 3.12(4) ? . 55520
C(507) O(9) 3.476(12) ? . 55531
C(507) O(505) 2.426(13) ? . .
C(507) O(506) 2.90(3) ? . 55520
C(507) C(506) 2.37(3) ? . .
C(507) C(507) 3.447(3) ? . 55520
C(507) C(510) 2.29(3) ? . 55520
C(508) O(504) 2.55(2) ? . .
C(508) O(504) 2.55(2) ? . 55520
C(508) C(509) 2.166(16) ? . .
C(508) C(509) 2.166(16) ? . 55520
C(508) C(510) 3.51(2) ? . .
C(508) C(510) 3.51(2) ? . 55520
C(509) O(9) 3.325(16) ? . 55506
C(509) O(505) 2.971(17) ? . 55520
C(509) O(506) 2.40(3) ? . .
C(509) C(505) 3.20(3) ? . 55520
C(509) C(506) 2.05(3) ? . 55520
C(509) C(508) 2.166(16) ? . .
C(510) O(9) 3.37(2) ? . 55506
C(510) O(105) 3.41(2) ? . 55506
C(510) O(503) 3.14(4) ? . 55520
C(510) O(505) 2.38(2) ? . .
C(510) C(505) 2.08(4) ? . 55520
C(510) C(507) 2.29(3) ? . 55520
C(510) C(508) 3.51(2) ? . .
C(510) C(511) 2.36(4) ? . .
C(511) O(501) 2.38(4) ? . .
C(511) O(503) 1.87(5) ? . 55520
C(511) O(504) 2.94(4) ? . 55520
C(511) C(504) 2.33(4) ? . 55520
C(511) C(506) 2.28(4) ? . 55520
C(511) C(510) 2.36(4) ? . .
C(512) O(6) 3.34(3) ? . .
C(512) O(12) 3.58(3) ? . .
C(512) O(502) 3.18(4) ? . 55520
C(512) O(506) 2.34(4) ? . .
C(512) C(501) 2.37(4) ? . .
C(512) C(503) 2.41(4) ? . 55520
C(512) C(506) 3.12(4) ? . 55520
C(601) K(55) 3.36(5) ? . .
C(601) O(11) 3.58(5) ? . 55506
C(601) O(108) 3.23(8) ? . 55506
C(601) O(601) 3.57(2) ? . 55512
C(601) O(602) 2.41(9) ? . .
C(601) O(602) 3.56(9) ? . 55506
C(601) O(605) 3.48(9) ? . 55507
C(601) O(606) 2.08(6) ? . 55512
C(601) C(608) 3.35(9) ? . 55507
C(601) C(609) 3.35(10) ? . 55507
C(601) C(610) 2.83(7) ? . 55512
C(601) C(611) 1.90(5) ? . 55512
C(601) C(612) 2.40(3) ? . .
C(602) O(2) 3.29(3) ? . 55506
C(602) O(6) 3.19(3) ? . 55506
C(602) O(11) 3.22(7) ? . 55506
C(602) O(601) 2.45(4) ? . .
C(602) O(605) 2.42(9) ? . 55507
C(602) O(606) 3.25(6) ? . 55512
C(602) C(603) 2.44(11) ? . .
C(602) C(607) 3.57(10) ? . 55507
C(602) C(608) 2.27(10) ? . 55507
C(602) C(609) 2.14(11) ? . 55507
C(602) C(610) 3.39(11) ? . 55507
C(602) C(610) 3.59(8) ? . 55512
C(602) C(611) 3.37(6) ? . 55512
C(603) O(5) 3.15(7) ? . .
C(603) O(6) 3.54(7) ? . 55506
C(603) O(101) 3.43(5) ? . .
C(603) O(603) 2.41(10) ? . .
C(603) O(606) 2.78(8) ? . 55507
C(603) C(602) 2.44(11) ? . .
C(603) C(608) 2.41(11) ? . 55507
C(604) O(5) 2.86(7) ? . .
C(604) O(105) 3.30(8) ? . .
C(604) O(602) 2.44(11) ? . .
C(604) O(605) 2.18(10) ? . 55507
C(604) O(606) 2.31(8) ? . 55507
C(604) C(605) 2.42(11) ? . .
C(604) C(608) 3.46(11) ? . 55507
C(604) C(611) 3.23(8) ? . 55507
C(605) O(105) 3.54(9) ? . .
C(605) O(301) 3.53(7) ? . 55506
C(605) O(604) 2.42(12) ? . .
C(605) O(605) 3.48(10) ? . 55507
C(605) O(606) 3.27(9) ? . 55507
C(605) C(604) 2.42(11) ? . .
C(605) C(610) 3.04(10) ? . 55507
C(605) C(611) 3.51(9) ? . 55507
C(606) K(5) 3.45(7) ? . .
C(606) O(603) 2.47(11) ? . .
C(606) C(607) 2.44(13) ? . .
C(607) K(5) 3.40(8) ? . .
C(607) O(602) 3.60(10) ? . 55507
C(607) O(605) 2.42(10) ? . .
C(607) C(602) 3.57(10) ? . 55507
C(607) C(606) 2.44(13) ? . .
C(608) K(5) 3.46(7) ? . .
C(608) O(6) 3.38(8) ? . 55512
C(608) O(106) 3.30(8) ? . 55512
C(608) O(601) 3.38(8) ? . 55507
C(608) O(602) 2.33(11) ? . 55507
C(608) O(603) 3.38(10) ? . 55507
C(608) O(604) 2.46(11) ? . .
C(608) C(601) 3.35(9) ? . 55507
C(608) C(602) 2.27(10) ? . 55507
C(608) C(603) 2.41(11) ? . 55507
C(608) C(604) 3.46(11) ? . 55507
C(608) C(609) 2.44(11) ? . .
C(609) O(5) 3.45(6) ? . 55507
C(609) O(603) 2.43(10) ? . 55507
C(609) O(606) 2.41(8) ? . .
C(609) C(601) 3.35(10) ? . 55507
C(609) C(602) 2.14(11) ? . 55507
C(609) C(608) 2.44(11) ? . .
C(610) K(55) 3.58(5) ? . .
C(610) O(5) 3.11(4) ? . 55507
C(610) O(10) 3.40(7) ? . 55507
C(610) O(602) 2.01(11) ? . 55507
C(610) O(603) 2.06(9) ? . 55507
C(610) O(605) 2.46(10) ? . .
C(610) C(601) 2.83(7) ? . 55512
C(610) C(602) 3.39(11) ? . 55507
C(610) C(602) 3.59(8) ? . 55512
C(610) C(605) 3.04(10) ? . 55507
C(610) C(611) 2.48(7) ? . .
C(611) K(55) 3.38(6) ? . .
C(611) O(108) 2.89(6) ? . 55507
C(611) O(601) 2.40(3) ? . .
C(611) O(601) 2.29(4) ? . 55512
C(611) O(603) 3.33(8) ? . 55507
C(611) C(601) 1.90(5) ? . 55512
C(611) C(602) 3.37(6) ? . 55512
C(611) C(604) 3.23(8) ? . 55507
C(611) C(605) 3.51(9) ? . 55507
C(611) C(610) 2.48(7) ? . .
C(611) C(611) 3.38(2) ? . 55512
C(612) K(55) 3.37(6) ? . .
C(612) K(55) 3.37(6) ? . 55506
C(612) O(108) 3.58(5) ? . 55506
C(612) O(108) 3.58(5) ? . 55507
C(612) O(606) 2.64(5) ? . .
C(612) O(606) 2.64(5) ? . 55512
C(612) C(601) 2.40(3) ? . .
C(612) C(601) 2.40(3) ? . 55512
C(701) O(108) 3.57(8) ? . 55516
C(701) O(702) 2.51(10) ? . .
C(701) O(706) 2.60(9) ? . 55520
C(701) C(701) 2.684(12) ? . 55520
C(701) C(702) 3.33(5) ? . 55520
C(701) C(710) 3.55(11) ? . 55520
C(701) C(711) 2.01(6) ? . 55520
C(701) C(712) 2.43(4) ? . .
C(701) C(712) 1.95(4) ? . 55520
C(702) O(20) 3.59(7) ? . 55516
C(702) O(302) 3.33(7) ? . 55418
C(702) O(701) 2.20(4) ? . .
C(702) C(301) 3.23(9) ? . 55418
C(702) C(302) 3.49(9) ? . 55418
C(702) C(701) 3.33(5) ? . 55520
C(702) C(703) 2.46(12) ? . .
C(702) C(710) 2.45(13) ? . 55520
C(703) O(112) 3.21(8) ? . 55520
C(703) O(703) 2.39(15) ? . .
C(703) O(705) 3.35(14) ? . 55520
C(703) C(702) 2.46(12) ? . .
C(703) C(709) 2.45(15) ? . 55520
C(703) C(710) 1.98(13) ? . 55520
C(703) C(711) 2.36(13) ? . 55520
C(703) C(712) 3.00(12) ? . 55520
C(704) O(112) 2.86(10) ? . 55520
C(704) O(702) 2.45(13) ? . .
C(704) O(705) 2.93(15) ? . 55520
C(704) O(706) 2.51(14) ? . 55520
C(704) C(705) 2.38(16) ? . .
C(704) C(709) 2.14(16) ? . 55520
C(704) C(710) 2.68(15) ? . 55520
C(705) K(6) 3.50(11) ? . .
C(705) O(12) 3.40(10) ? . 55520
C(705) O(13) 3.33(12) ? . 55520
C(705) O(704) 2.44(18) ? . .
C(705) C(704) 2.38(16) ? . .
C(706) O(13) 3.55(13) ? . 55520
C(706) O(103) 3.51(10) ? . 55520
C(706) O(703) 2.36(15) ? . .
C(706) C(707) 2.43(19) ? . .
C(707) O(705) 2.50(15) ? . .
C(707) C(706) 2.43(19) ? . .
C(708) O(303) 2.91(13) ? . 55507
C(708) O(704) 2.39(18) ? . .
C(708) C(304) 3.16(13) ? . 55507
C(708) C(305) 3.56(14) ? . 55507
C(708) C(709) 2.52(16) ? . .
C(709) O(112) 3.52(11) ? . .
C(709) O(303) 2.67(11) ? . 55507
C(709) O(702) 2.65(13) ? . 55520
C(709) O(703) 3.27(16) ? . 55520
C(709) O(706) 2.41(14) ? . .
C(709) C(303) 2.93(12) ? . 55507
C(709) C(304) 1.86(12) ? . 55507
C(709) C(305) 2.86(13) ? . 55507
C(709) C(703) 2.45(15) ? . 55520
C(709) C(704) 2.14(16) ? . 55520
C(709) C(708) 2.52(16) ? . .
C(710) O(112) 3.25(10) ? . 55529
C(710) O(303) 3.54(10) ? . 55507
C(710) O(702) 1.94(11) ? . 55520
C(710) O(705) 2.45(15) ? . .
C(710) C(304) 2.70(11) ? . 55507
C(710) C(305) 3.00(12) ? . 55507
C(710) C(701) 3.55(11) ? . 55520
C(710) C(702) 2.45(12) ? . 55520
C(710) C(703) 1.98(13) ? . 55520
C(710) C(704) 2.68(15) ? . 55520
C(710) C(711) 2.38(13) ? . .
C(711) O(20) 3.42(7) ? . 55529
C(711) O(302) 2.80(7) ? . 55411
C(711) O(701) 2.66(5) ? . .
C(711) C(301) 2.97(9) ? . 55411
C(711) C(302) 3.06(9) ? . 55411
C(711) C(303) 3.59(7) ? . 55411
C(711) C(701) 2.01(6) ? . 55520
C(711) C(703) 2.36(13) ? . 55520
C(711) C(710) 2.38(13) ? . .
C(712) O(301) 3.40(7) ? . 55411
C(712) O(302) 3.38(5) ? . 55411
C(712) O(702) 2.20(12) ? . 55520
C(712) O(706) 2.36(11) ? . .
C(712) C(301) 2.47(8) ? . 55411
C(712) C(302) 3.35(7) ? . 55411
C(712) C(312) 3.55(8) ? . 55411
C(712) C(701) 2.43(4) ? . .
C(712) C(701) 1.95(4) ? . 55520
C(712) C(703) 3.00(12) ? . 55520
C(712) C(712) 3.48(2) ? . 55520
C(901) O(8) 3.24(2) ? . .
C(901) O(107) 3.56(2) ? . .
C(911) O(7) 3.20(2) ? . 55506
C(911) O(107) 3.49(2) ? . 55506
|
1101221.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-16 14:49:56 +0200 (Wed, 16 Mar 2016) $
#$Revision: 178223 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101221.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_1101221
loop_
_publ_author_name
'Goto, Yuya'
'Kamata, Keigo'
'Yamaguchi, Kazuya'
'Uehara, Kazuhiro'
'Hikichi, Shiro'
'Mizuno, Noritaka'
_publ_section_title
;
Synthesis, Structural Characterization, and Catalytic Performance of
Dititanium-Substituted \g-Keggin Silicotungstate
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 2347
_journal_page_last 2356
_journal_paper_doi 10.1021/ic052179q
_journal_volume 45
_journal_year 2006
_chemical_formula_moiety 'C98 H200 K8 O126 Si2 Ti4 W20 '
_chemical_formula_sum 'C98 H200 K8 O126 Si2 Ti4 W20'
_chemical_formula_weight 7632.14
_space_group_IT_number 12
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2y'
_symmetry_space_group_name_H-M 'C 1 2/m 1'
_cell_angle_alpha 90.0000
_cell_angle_beta 96.3280(8)
_cell_angle_gamma 90.0000
_cell_formula_units_Z 2
_cell_length_a 45.4319(7)
_cell_length_b 17.8884(4)
_cell_length_c 15.8179(3)
_cell_measurement_temperature 296.1
_cell_volume 12776.9(4)
_computing_cell_refinement CrystalClear
_computing_data_collection CrystalClear
_computing_data_reduction CrystalStructure
_computing_publication_material 'CrystalStructure 3.7.0'
_computing_structure_refinement CRYSTALS
_computing_structure_solution 'DIRDIF99 (PATTY)'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type 'Rigaku Saturn'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_limit_h_max 59
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 15078
_diffrn_reflns_theta_full 27.71
_diffrn_reflns_theta_max 27.71
_exptl_absorpt_coefficient_mu 9.306
_exptl_absorpt_correction_type none
_exptl_crystal_colour NONE
_exptl_crystal_density_diffrn 1.984
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description NONE
_exptl_crystal_F_000 7088.00
_exptl_crystal_size_max 0.00
_exptl_crystal_size_mid 0.00
_exptl_crystal_size_min 0.00
_refine_diff_density_max 2.27
_refine_diff_density_min -2.04
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 11.430
_refine_ls_number_parameters 301
_refine_ls_number_reflns 9127
_refine_ls_R_factor_gt 0.0602
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1.0'
_refine_ls_weighting_scheme unit
_refine_ls_wR_factor_ref 0.0783
_reflns_number_gt 9072
_reflns_number_total 15078
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'C 2/m'
_cod_original_formula_sum 'C98 H200 K8 O126 Si2 Ti4 W20 '
_cod_database_code 1101221
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,-Z
3 -X,-Y,-Z
4 +X,-Y,+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,-Z
7 1/2-X,1/2-Y,-Z
8 1/2+X,1/2-Y,+Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W(1) W 0.40682(2) 0.33421(5) 0.36778(6) 0.0591(2) Uani 1.00 1 d . . .
W(2) W 0.40685(2) 0.33410(5) 0.57717(6) 0.0594(2) Uani 1.00 1 d . . .
W(3) W 0.38232(3) 0.5000 0.24307(10) 0.0611(3) Uani 1.00 2 d S . .
W(4) W 0.38282(3) 0.5000 0.68746(10) 0.0612(3) Uani 1.00 2 d S . .
W(5) W 0.33104(2) 0.40641(5) 0.33194(6) 0.0539(2) Uani 1.00 1 d . . .
W(6) W 0.33116(2) 0.40637(5) 0.56773(6) 0.0542(2) Uani 1.00 1 d . . .
Ti(1) Ti 0.46076(6) 0.41131(19) 0.4892(3) 0.0620(11) Uani 1.00 1 d . . .
K(1) K 0.5000 0.0000 0.5000 0.115 Uani 1.00 4 d R . .
K(2) K 0.3153(2) 0.0000 0.4735(9) 0.138(4) Uani 1.00 2 d S . .
K(3) K 0.5000 0.2892(11) 0.0000 0.181(6) Uani 1.00 2 d S . .
K(4) K 0.6783 0.1737 0.0435 0.448 Uiso 0.75 1 d R . .
Si(1) Si 0.38713(13) 0.5000 0.4666(5) 0.046(2) Uani 1.00 2 d S . .
O(1) O 0.4602(3) 0.5000 0.5666(15) 0.064(6) Uani 1.00 2 d S . .
O(2) O 0.4593(3) 0.5000 0.4116(17) 0.074(7) Uani 1.00 2 d S . .
O(3) O 0.4477(2) 0.3505(6) 0.3966(10) 0.063(4) Uani 1.00 1 d . . .
O(4) O 0.4477(2) 0.3509(7) 0.5738(10) 0.062(4) Uani 1.00 1 d . . .
O(5) O 0.4061(2) 0.4210(7) 0.2944(9) 0.062(4) Uani 1.00 1 d . . .
O(6) O 0.4063(2) 0.4201(7) 0.6501(9) 0.062(4) Uani 1.00 1 d . . .
O(7) O 0.4052(2) 0.2815(7) 0.4708(10) 0.064(4) Uani 1.00 1 d . . .
O(8) O 0.3647(2) 0.3451(7) 0.3633(9) 0.058(4) Uani 1.00 1 d . . .
O(9) O 0.3643(2) 0.3447(7) 0.5565(9) 0.057(4) Uani 1.00 1 d . . .
O(10) O 0.3500(2) 0.4294(8) 0.2334(9) 0.066(4) Uani 1.00 1 d . . .
O(11) O 0.3503(2) 0.4282(8) 0.6773(9) 0.062(4) Uani 1.00 1 d . . .
O(12) O 0.3109(3) 0.5000 0.3145(12) 0.053(5) Uani 1.00 2 d S . .
O(13) O 0.3107(3) 0.5000 0.5717(13) 0.055(5) Uani 1.00 2 d S . .
O(14) O 0.3235(2) 0.4048(6) 0.4466(8) 0.049(3) Uani 1.00 1 d . . .
O(15) O 0.4076(2) 0.4249(6) 0.4722(9) 0.051(3) Uani 1.00 1 d . . .
O(16) O 0.3655(3) 0.5000 0.3770(12) 0.047(5) Uani 1.00 2 d S . .
O(17) O 0.3658(3) 0.5000 0.5423(12) 0.050(5) Uani 1.00 2 d S . .
O(101) O 0.5000 0.3929(9) 0.5000 0.073(6) Uani 1.00 2 d S . .
O(102) O 0.4082(2) 0.2626(8) 0.2987(11) 0.075(5) Uani 1.00 1 d . . .
O(103) O 0.4092(2) 0.2623(8) 0.6474(11) 0.079(5) Uani 1.00 1 d . . .
O(104) O 0.3918(5) 0.5000 0.1433(16) 0.084(8) Uani 1.00 2 d S . .
O(105) O 0.3927(5) 0.5000 0.7957(15) 0.081(8) Uani 1.00 2 d S . .
O(106) O 0.3051(2) 0.3448(8) 0.2895(10) 0.067(4) Uani 1.00 1 d . . .
O(107) O 0.3050(2) 0.3455(8) 0.5944(9) 0.065(4) Uani 1.00 1 d . . .
O(201) O 0.500000(10) 0.1576(3) 0.500000(10) 0.24(2) Uiso 0.50 2 d SP . .
O(202) O 0.4614(7) 0.06729(10) 0.614(2) 0.24(2) Uiso 0.25 1 d P . .
O(203) O 0.4705(9) -0.08895(18) 0.611(3) 0.24(2) Uiso 0.25 1 d P . .
O(204) O 0.5258(7) -0.1394(3) 0.555(3) 0.24(2) Uiso 0.25 1 d P . .
O(205) O 0.5553(5) -0.04823(11) 0.447(3) 0.24(2) Uiso 0.25 1 d P . .
O(206) O 0.5471(3) 0.10647(12) 0.457(2) 0.24(2) Uiso 0.25 1 d P . .
O(301) O 0.3255(7) 0.15670(6) 0.457(3) 0.229(9) Uiso 0.50 1 d P . .
O(302) O 0.2722(6) 0.10702(8) 0.517(2) 0.229(9) Uiso 0.50 1 d P . .
O(303) O 0.2672(5) -0.0463(5) 0.5631(16) 0.229(9) Uiso 0.50 1 d P . .
O(304) O 0.2992(7) -0.15127(12) 0.477(3) 0.229(9) Uiso 0.50 1 d P . .
O(305) O 0.3532(6) -0.10408(3) 0.414(2) 0.229(9) Uiso 0.50 1 d P . .
O(306) O 0.3601(5) 0.0512(5) 0.3716(17) 0.229(9) Uiso 0.50 1 d P . .
O(401) O 0.5455(10) 0.363(2) 0.104(3) 0.322(16) Uiso 0.50 1 d P . .
O(402) O 0.5482(10) 0.382(2) -0.073(4) 0.322(16) Uiso 0.50 1 d P . .
O(403) O 0.5031(13) 0.323(2) -0.186(3) 0.322(16) Uiso 0.50 1 d P . .
O(404) O 0.4460(11) 0.306(2) -0.130(4) 0.322(16) Uiso 0.50 1 d P . .
O(405) O 0.4434(10) 0.293(2) 0.049(4) 0.322(16) Uiso 0.50 1 d P . .
O(406) O 0.4900(13) 0.352(2) 0.162(3) 0.322(16) Uiso 0.50 1 d P . .
O(504) O 0.7044 0.2164 0.2268 0.253 Uiso 0.75 1 d R . .
O(503) O 0.6457 0.1795 0.1808 0.253 Uiso 0.75 1 d R . .
O(502) O 0.6326 0.0708 0.0565 0.253 Uiso 0.75 1 d R . .
O(501) O 0.6730 0.0482 -0.0640 0.253 Uiso 0.75 1 d R . .
O(506) O 0.7325 0.0911 -0.0165 0.253 Uiso 0.75 1 d R . .
O(505) O 0.7440 0.1994 0.1056 0.253 Uiso 0.75 1 d R . .
C(1) C 0.4705(15) 0.5000 0.659(4) 0.07(2) Uani 0.50 2 d SP . .
C(2) C 0.4708(14) 0.5000 0.334(5) 0.08(2) Uani 0.50 2 d SP . .
C(412) C 0.5398(13) 0.388(3) 0.188(3) 0.322(16) Uiso 0.50 1 d P . .
C(411) C 0.5162(15) 0.341(3) 0.217(3) 0.322(16) Uiso 0.50 1 d P . .
C(201) C 0.4720(4) 0.18638(18) 0.5610(15) 0.24(2) Uiso 0.25 1 d P . .
C(202) C 0.4480(5) 0.1317(3) 0.575(2) 0.24(2) Uiso 0.25 1 d P . .
C(203) C 0.4391(9) 0.000000(10) 0.633(3) 0.24(2) Uiso 0.50 2 d SP . .
C(204) C 0.4551(12) -0.0544(4) 0.673(3) 0.24(2) Uiso 0.25 1 d P . .
C(205) C 0.4869(11) -0.1538(6) 0.644(3) 0.24(2) Uiso 0.25 1 d P . .
C(206) C 0.5025(8) -0.1885(2) 0.576(3) 0.24(2) Uiso 0.25 1 d P . .
C(207) C 0.5444(7) -0.16838(11) 0.493(3) 0.24(2) Uiso 0.25 1 d P . .
C(208) C 0.5691(6) -0.1162(2) 0.480(4) 0.24(2) Uiso 0.25 1 d P . .
C(209) C 0.5777(6) 0.000000(10) 0.428(4) 0.24(2) Uiso 0.50 2 d SP . .
C(210) C 0.5633(7) 0.0734(4) 0.393(3) 0.24(2) Uiso 0.25 1 d P . .
C(211) C 0.5341(5) 0.1764(4) 0.4275(18) 0.24(2) Uiso 0.25 1 d P . .
C(212) C 0.51664(12) 0.20628(18) 0.4954(9) 0.24(2) Uiso 0.25 1 d P . .
C(301) C 0.3000(8) 0.2058(3) 0.462(4) 0.229(9) Uiso 0.50 1 d P . .
C(302) C 0.2834(8) 0.1824(4) 0.535(3) 0.229(9) Uiso 0.50 1 d P . .
C(303) C 0.2542(6) 0.0801(5) 0.582(2) 0.229(9) Uiso 0.50 1 d P . .
C(304) C 0.2424(5) 0.000000(10) 0.5609(16) 0.229(9) Uiso 1.00 2 d S . .
C(305) C 0.2568(6) -0.12287(9) 0.548(2) 0.229(9) Uiso 0.50 1 d P . .
C(306) C 0.2837(8) -0.1721(5) 0.548(3) 0.229(9) Uiso 0.50 1 d P . .
C(307) C 0.3230(8) -0.20176(12) 0.464(4) 0.229(9) Uiso 0.50 1 d P . .
C(308) C 0.3401(8) -0.1754(5) 0.392(3) 0.229(9) Uiso 0.50 1 d P . .
C(309) C 0.3716(6) -0.0757(6) 0.350(2) 0.229(9) Uiso 0.50 1 d P . .
C(310) C 0.3843(5) 0.000000(10) 0.3753(17) 0.229(9) Uiso 1.00 2 d S . .
C(311) C 0.3703(6) 0.12633(6) 0.398(2) 0.229(9) Uiso 0.50 1 d P . .
C(312) C 0.3444(8) 0.1781(5) 0.392(3) 0.229(9) Uiso 0.50 1 d P . .
C(401) C 0.5675(10) 0.409(2) 0.072(4) 0.322(16) Uiso 0.50 1 d P . .
C(402) C 0.5739(9) 0.378(2) -0.010(4) 0.322(16) Uiso 0.50 1 d P . .
C(403) C 0.5543(12) 0.354(3) -0.155(4) 0.322(16) Uiso 0.50 1 d P . .
C(404) C 0.5272(14) 0.365(3) -0.214(3) 0.322(16) Uiso 0.50 1 d P . .
C(405) C 0.4764(15) 0.325(3) -0.243(3) 0.322(16) Uiso 0.50 1 d P . .
C(406) C 0.4548(14) 0.275(3) -0.209(3) 0.322(16) Uiso 0.50 1 d P . .
C(407) C 0.4251(10) 0.261(2) -0.096(4) 0.322(16) Uiso 0.50 1 d P . .
C(408) C 0.4180(9) 0.296(2) -0.014(4) 0.322(16) Uiso 0.50 1 d P . .
C(409) C 0.4382(12) 0.326(3) 0.128(4) 0.322(16) Uiso 0.50 1 d P . .
C(410) C 0.4649(14) 0.317(3) 0.190(3) 0.322(16) Uiso 0.50 1 d P . .
C(506) C 0.6807 0.2521 0.2628 0.253 Uiso 0.75 1 d R . .
C(505) C 0.6562 0.1984 0.2640 0.253 Uiso 0.75 1 d R . .
C(504) C 0.6196 0.1361 0.1744 0.253 Uiso 0.75 1 d R . .
C(503) C 0.6102 0.1134 0.0861 0.253 Uiso 0.75 1 d R . .
C(502) C 0.6248 0.0432 -0.0279 0.253 Uiso 0.75 1 d R . .
C(501) C 0.6495 0.0000 -0.0556 0.253 Uiso 1.50 2 d R . .
C(512) C 0.6983 0.0000 -0.0897 0.253 Uiso 1.50 2 d R . .
C(511) C 0.7223 0.0630 -0.0979 0.253 Uiso 0.75 1 d R . .
C(510) C 0.7575 0.1404 -0.0145 0.253 Uiso 0.75 1 d R . .
C(509) C 0.7678 0.1613 0.0729 0.253 Uiso 0.75 1 d R . .
C(508) C 0.7524 0.2258 0.1900 0.253 Uiso 0.75 1 d R . .
C(507) C 0.7283 0.2665 0.2210 0.253 Uiso 0.75 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W(1) 0.0343(3) 0.0379(4) 0.1065(7) -0.0021(3) 0.0143(4) -0.0103(4)
W(2) 0.0343(3) 0.0386(4) 0.1040(7) -0.0009(3) 0.0018(4) 0.0114(4)
W(3) 0.0454(6) 0.0590(7) 0.0814(9) 0.0000 0.0177(6) 0.0000
W(4) 0.0445(6) 0.0586(7) 0.0785(9) 0.0000 -0.0019(6) 0.0000
W(5) 0.0327(3) 0.0492(4) 0.0797(6) -0.0042(3) 0.0054(3) -0.0073(4)
W(6) 0.0326(3) 0.0493(4) 0.0812(6) -0.0041(3) 0.0089(3) 0.0048(4)
Ti(1) 0.0283(15) 0.0301(17) 0.127(3) -0.0018(13) 0.0079(18) 0.000(2)
K(1) 0.064(6) 0.032(5) 0.247(18) 0.0000 0.005(8) 0.0000
K(2) 0.083(5) 0.039(4) 0.312(16) 0.0000 0.105(8) 0.0000
K(3) 0.117(8) 0.34(2) 0.083(7) 0.0000 0.005(6) 0.0000
Si(1) 0.027(3) 0.036(3) 0.077(5) 0.0000 0.007(3) 0.0000
O(1) 0.028(8) 0.039(10) 0.123(19) 0.0000 0.001(10) 0.0000
O(2) 0.033(9) 0.037(10) 0.15(2) 0.0000 0.018(12) 0.0000
O(3) 0.039(6) 0.032(6) 0.118(12) 0.007(5) 0.013(7) -0.003(7)
O(4) 0.039(6) 0.039(7) 0.108(12) 0.006(5) 0.001(7) 0.004(7)
O(5) 0.037(6) 0.060(8) 0.091(11) -0.006(6) 0.017(6) -0.018(8)
O(6) 0.039(6) 0.051(8) 0.093(11) -0.000(6) -0.003(6) 0.012(7)
O(7) 0.028(5) 0.039(7) 0.125(12) 0.001(5) 0.014(6) -0.006(8)
O(8) 0.039(6) 0.044(7) 0.092(10) -0.006(5) 0.012(6) -0.010(7)
O(9) 0.036(6) 0.039(7) 0.095(10) -0.006(5) 0.003(6) 0.010(7)
O(10) 0.053(7) 0.067(9) 0.080(10) 0.004(7) 0.018(7) -0.005(8)
O(11) 0.040(6) 0.066(9) 0.079(10) -0.000(6) 0.006(6) 0.010(7)
O(12) 0.034(8) 0.051(11) 0.074(13) 0.0000 0.005(8) 0.0000
O(13) 0.040(9) 0.054(11) 0.073(14) 0.0000 0.013(9) 0.0000
O(14) 0.035(5) 0.042(6) 0.070(8) -0.006(5) 0.008(5) -0.004(6)
O(15) 0.028(5) 0.040(6) 0.085(9) -0.001(5) 0.004(5) -0.003(6)
O(16) 0.029(8) 0.037(9) 0.075(13) 0.0000 0.007(8) 0.0000
O(17) 0.030(8) 0.035(9) 0.083(14) 0.0000 0.001(8) 0.0000
O(101) 0.019(7) 0.035(10) 0.16(2) 0.0000 -0.001(10) 0.0000
O(102) 0.048(8) 0.055(9) 0.122(14) -0.003(6) 0.016(8) -0.019(9)
O(103) 0.048(8) 0.055(9) 0.131(14) 0.000(6) 0.001(8) 0.018(9)
O(104) 0.077(15) 0.079(16) 0.099(19) 0.0000 0.028(13) 0.0000
O(105) 0.079(15) 0.086(17) 0.076(16) 0.0000 -0.000(12) 0.0000
O(106) 0.043(7) 0.063(9) 0.096(11) -0.007(6) 0.008(7) -0.014(8)
O(107) 0.037(6) 0.069(9) 0.091(11) -0.010(6) 0.010(6) 0.004(8)
C(1) 0.07(4) 0.10(5) 0.04(3) 0.0000 0.01(3) 0.0000
C(2) 0.06(3) 0.04(3) 0.14(6) 0.0000 0.04(4) 0.0000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
W W -0.849 6.872
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.278 0.446
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
K K 0.200 0.250
;
International Tables for Crystallography
(1992, 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O(3) W(1) O(5) 88.2(6) ? . . .
O(3) W(1) O(7) 90.3(6) ? . . .
O(3) W(1) O(8) 161.0(6) ? . . .
O(3) W(1) O(15) 77.4(5) ? . . .
O(3) W(1) O(102) 99.7(7) ? . . .
O(5) W(1) O(7) 156.6(6) ? . . .
O(5) W(1) O(8) 86.7(6) ? . . .
O(5) W(1) O(15) 82.0(6) ? . . .
O(5) W(1) O(102) 102.5(8) ? . . .
O(7) W(1) O(8) 87.2(6) ? . . .
O(7) W(1) O(15) 74.8(6) ? . . .
O(7) W(1) O(102) 100.8(7) ? . . .
O(8) W(1) O(15) 83.8(5) ? . . .
O(8) W(1) O(102) 99.2(6) ? . . .
O(15) W(1) O(102) 174.6(6) ? . . .
O(4) W(2) O(6) 88.0(6) ? . . .
O(4) W(2) O(7) 90.0(6) ? . . .
O(4) W(2) O(9) 161.5(6) ? . . .
O(4) W(2) O(15) 77.3(5) ? . . .
O(4) W(2) O(103) 98.4(7) ? . . .
O(6) W(2) O(7) 156.0(6) ? . . .
O(6) W(2) O(9) 86.9(6) ? . . .
O(6) W(2) O(15) 83.0(6) ? . . .
O(6) W(2) O(103) 102.5(8) ? . . .
O(7) W(2) O(9) 87.5(6) ? . . .
O(7) W(2) O(15) 73.2(5) ? . . .
O(7) W(2) O(103) 101.4(8) ? . . .
O(9) W(2) O(15) 84.4(5) ? . . .
O(9) W(2) O(103) 100.0(7) ? . . .
O(15) W(2) O(103) 173.0(7) ? . . .
O(5) W(3) O(5) 95.9(6) ? . . 56504
O(5) W(3) O(10) 86.4(6) ? . . .
O(5) W(3) O(10) 155.5(7) ? . . 56504
O(5) W(3) O(16) 80.8(5) ? . . .
O(5) W(3) O(104) 101.9(7) ? . . .
O(5) W(3) O(10) 155.5(7) ? 56504 . .
O(5) W(3) O(10) 86.4(6) ? 56504 . 56504
O(5) W(3) O(16) 80.8(5) ? 56504 . .
O(5) W(3) O(104) 101.9(7) ? 56504 . .
O(10) W(3) O(10) 81.9(6) ? . . 56504
O(10) W(3) O(16) 75.4(6) ? . . .
O(10) W(3) O(104) 101.5(8) ? . . .
O(10) W(3) O(16) 75.4(6) ? 56504 . .
O(10) W(3) O(104) 101.5(8) ? 56504 . .
O(16) W(3) O(104) 175.9(9) ? . . .
O(6) W(4) O(6) 96.6(6) ? . . 56504
O(6) W(4) O(11) 85.7(6) ? . . .
O(6) W(4) O(11) 155.2(6) ? . . 56504
O(6) W(4) O(17) 80.4(5) ? . . .
O(6) W(4) O(105) 102.4(7) ? . . .
O(6) W(4) O(11) 155.2(6) ? 56504 . .
O(6) W(4) O(11) 85.7(6) ? 56504 . 56504
O(6) W(4) O(17) 80.4(5) ? 56504 . .
O(6) W(4) O(105) 102.4(7) ? 56504 . .
O(11) W(4) O(11) 82.3(6) ? . . 56504
O(11) W(4) O(17) 75.6(5) ? . . .
O(11) W(4) O(105) 101.2(8) ? . . .
O(11) W(4) O(17) 75.6(5) ? 56504 . .
O(11) W(4) O(105) 101.2(8) ? 56504 . .
O(17) W(4) O(105) 175.7(9) ? . . .
O(8) W(5) O(10) 84.9(6) ? . . .
O(8) W(5) O(12) 154.2(6) ? . . .
O(8) W(5) O(14) 88.2(6) ? . . .
O(8) W(5) O(16) 80.9(5) ? . . .
O(8) W(5) O(106) 103.3(6) ? . . .
O(10) W(5) O(12) 86.9(8) ? . . .
O(10) W(5) O(14) 159.7(6) ? . . .
O(10) W(5) O(16) 75.6(7) ? . . .
O(10) W(5) O(106) 99.6(7) ? . . .
O(12) W(5) O(14) 91.1(8) ? . . .
O(12) W(5) O(16) 73.3(5) ? . . .
O(12) W(5) O(106) 102.2(7) ? . . .
O(14) W(5) O(16) 84.5(6) ? . . .
O(14) W(5) O(106) 100.6(7) ? . . .
O(16) W(5) O(106) 173.4(7) ? . . .
O(9) W(6) O(11) 85.1(6) ? . . .
O(9) W(6) O(13) 154.7(6) ? . . .
O(9) W(6) O(14) 87.4(6) ? . . .
O(9) W(6) O(17) 81.0(5) ? . . .
O(9) W(6) O(107) 103.6(6) ? . . .
O(11) W(6) O(13) 88.0(8) ? . . .
O(11) W(6) O(14) 159.2(6) ? . . .
O(11) W(6) O(17) 75.9(7) ? . . .
O(11) W(6) O(107) 99.8(7) ? . . .
O(13) W(6) O(14) 90.5(7) ? . . .
O(13) W(6) O(17) 73.7(6) ? . . .
O(13) W(6) O(107) 101.5(7) ? . . .
O(14) W(6) O(17) 83.8(6) ? . . .
O(14) W(6) O(107) 100.8(6) ? . . .
O(17) W(6) O(107) 173.6(7) ? . . .
O(1) Ti(1) O(2) 75.5(9) ? . . .
O(1) Ti(1) O(3) 156.2(7) ? . . .
O(1) Ti(1) O(4) 89.4(8) ? . . .
O(1) Ti(1) O(15) 85.0(6) ? . . .
O(1) Ti(1) O(101) 99.5(7) ? . . .
O(2) Ti(1) O(3) 89.3(8) ? . . .
O(2) Ti(1) O(4) 155.1(8) ? . . .
O(2) Ti(1) O(15) 83.4(7) ? . . .
O(2) Ti(1) O(101) 99.7(8) ? . . .
O(3) Ti(1) O(4) 97.7(7) ? . . .
O(3) Ti(1) O(15) 74.9(5) ? . . .
O(3) Ti(1) O(101) 101.1(6) ? . . .
O(4) Ti(1) O(15) 75.4(5) ? . . .
O(4) Ti(1) O(101) 102.4(6) ? . . .
O(15) Ti(1) O(101) 175.0(7) ? . . .
O(201) K(1) O(201) 0(440) ? . . 65603
O(201) K(1) O(202) 65.6(3) ? . . .
O(201) K(1) O(202) 65.6(3) ? . . 65602
O(201) K(1) O(202) 114.4(3) ? . . 65603
O(201) K(1) O(202) 114.4(3) ? . . 55504
O(201) K(1) O(203) 124.6(5) ? . . .
O(201) K(1) O(203) 124.6(6) ? . . 65602
O(201) K(1) O(203) 55.4(6) ? . . 65603
O(201) K(1) O(203) 55.4(5) ? . . 55504
O(201) K(1) O(204) 151.4(7) ? . . .
O(201) K(1) O(204) 151.4(6) ? . . 65602
O(201) K(1) O(204) 28.6(6) ? . . 65603
O(201) K(1) O(204) 28.6(7) ? . . 55504
O(201) K(1) O(205) 107.5(2) ? . . .
O(201) K(1) O(205) 107.5(2) ? . . 65602
O(201) K(1) O(205) 72.5(2) ? . . 65603
O(201) K(1) O(205) 72.5(2) ? . . 55504
O(201) K(1) O(206) 50.5(2) ? . . .
O(201) K(1) O(206) 50.5(2) ? . . 65602
O(201) K(1) O(206) 129.5(2) ? . . 65603
O(201) K(1) O(206) 129.5(2) ? . . 55504
O(201) K(1) O(202) 114.4(3) ? 65603 . .
O(201) K(1) O(202) 114.4(3) ? 65603 . 65602
O(201) K(1) O(202) 65.6(3) ? 65603 . 65603
O(201) K(1) O(202) 65.6(3) ? 65603 . 55504
O(201) K(1) O(203) 55.4(5) ? 65603 . .
O(201) K(1) O(203) 55.4(6) ? 65603 . 65602
O(201) K(1) O(203) 124.6(6) ? 65603 . 65603
O(201) K(1) O(203) 124.6(5) ? 65603 . 55504
O(201) K(1) O(204) 28.6(7) ? 65603 . .
O(201) K(1) O(204) 28.6(6) ? 65603 . 65602
O(201) K(1) O(204) 151.4(6) ? 65603 . 65603
O(201) K(1) O(204) 151.4(7) ? 65603 . 55504
O(201) K(1) O(205) 72.5(2) ? 65603 . .
O(201) K(1) O(205) 72.5(2) ? 65603 . 65602
O(201) K(1) O(205) 107.5(2) ? 65603 . 65603
O(201) K(1) O(205) 107.5(2) ? 65603 . 55504
O(201) K(1) O(206) 129.5(2) ? 65603 . .
O(201) K(1) O(206) 129.5(2) ? 65603 . 65602
O(201) K(1) O(206) 50.5(2) ? 65603 . 65603
O(201) K(1) O(206) 50.5(2) ? 65603 . 55504
O(202) K(1) O(202) 131.1(4) ? . . 65602
O(202) K(1) O(202) 180.0(11) ? . . 65603
O(202) K(1) O(202) 48.9(4) ? . . 55504
O(202) K(1) O(203) 59.3(6) ? . . .
O(202) K(1) O(203) 168.7(7) ? . . 65602
O(202) K(1) O(203) 120.7(6) ? . . 65603
O(202) K(1) O(203) 11.3(7) ? . . 55504
O(202) K(1) O(204) 115.7(11) ? . . .
O(202) K(1) O(204) 107.0(9) ? . . 65602
O(202) K(1) O(204) 64.3(11) ? . . 65603
O(202) K(1) O(204) 73.0(9) ? . . 55504
O(202) K(1) O(205) 156.2(11) ? . . .
O(202) K(1) O(205) 48.3(7) ? . . 65602
O(202) K(1) O(205) 23.8(11) ? . . 65603
O(202) K(1) O(205) 131.7(8) ? . . 55504
O(202) K(1) O(206) 111.9(6) ? . . .
O(202) K(1) O(206) 26.1(9) ? . . 65602
O(202) K(1) O(206) 68.1(6) ? . . 65603
O(202) K(1) O(206) 153.9(9) ? . . 55504
O(202) K(1) O(202) 48.9(4) ? 65602 . 65603
O(202) K(1) O(202) 180.0(11) ? 65602 . 55504
O(202) K(1) O(203) 168.7(7) ? 65602 . .
O(202) K(1) O(203) 59.3(6) ? 65602 . 65602
O(202) K(1) O(203) 11.3(7) ? 65602 . 65603
O(202) K(1) O(203) 120.7(6) ? 65602 . 55504
O(202) K(1) O(204) 107.0(9) ? 65602 . .
O(202) K(1) O(204) 115.7(11) ? 65602 . 65602
O(202) K(1) O(204) 73.0(9) ? 65602 . 65603
O(202) K(1) O(204) 64.3(11) ? 65602 . 55504
O(202) K(1) O(205) 48.3(8) ? 65602 . .
O(202) K(1) O(205) 156.2(11) ? 65602 . 65602
O(202) K(1) O(205) 131.7(7) ? 65602 . 65603
O(202) K(1) O(205) 23.8(11) ? 65602 . 55504
O(202) K(1) O(206) 26.1(9) ? 65602 . .
O(202) K(1) O(206) 111.9(6) ? 65602 . 65602
O(202) K(1) O(206) 153.9(9) ? 65602 . 65603
O(202) K(1) O(206) 68.1(6) ? 65602 . 55504
O(202) K(1) O(202) 131.1(4) ? 65603 . 55504
O(202) K(1) O(203) 120.7(6) ? 65603 . .
O(202) K(1) O(203) 11.3(7) ? 65603 . 65602
O(202) K(1) O(203) 59.3(6) ? 65603 . 65603
O(202) K(1) O(203) 168.7(7) ? 65603 . 55504
O(202) K(1) O(204) 64.3(11) ? 65603 . .
O(202) K(1) O(204) 73.0(9) ? 65603 . 65602
O(202) K(1) O(204) 115.7(11) ? 65603 . 65603
O(202) K(1) O(204) 107.0(9) ? 65603 . 55504
O(202) K(1) O(205) 23.8(11) ? 65603 . .
O(202) K(1) O(205) 131.7(7) ? 65603 . 65602
O(202) K(1) O(205) 156.2(11) ? 65603 . 65603
O(202) K(1) O(205) 48.3(8) ? 65603 . 55504
O(202) K(1) O(206) 68.1(6) ? 65603 . .
O(202) K(1) O(206) 153.9(9) ? 65603 . 65602
O(202) K(1) O(206) 111.9(6) ? 65603 . 65603
O(202) K(1) O(206) 26.1(9) ? 65603 . 55504
O(202) K(1) O(203) 11.3(7) ? 55504 . .
O(202) K(1) O(203) 120.7(6) ? 55504 . 65602
O(202) K(1) O(203) 168.7(7) ? 55504 . 65603
O(202) K(1) O(203) 59.3(6) ? 55504 . 55504
O(202) K(1) O(204) 73.0(9) ? 55504 . .
O(202) K(1) O(204) 64.3(11) ? 55504 . 65602
O(202) K(1) O(204) 107.0(9) ? 55504 . 65603
O(202) K(1) O(204) 115.7(11) ? 55504 . 55504
O(202) K(1) O(205) 131.7(8) ? 55504 . .
O(202) K(1) O(205) 23.8(11) ? 55504 . 65602
O(202) K(1) O(205) 48.3(7) ? 55504 . 65603
O(202) K(1) O(205) 156.2(11) ? 55504 . 55504
O(202) K(1) O(206) 153.9(9) ? 55504 . .
O(202) K(1) O(206) 68.1(6) ? 55504 . 65602
O(202) K(1) O(206) 26.1(9) ? 55504 . 65603
O(202) K(1) O(206) 111.9(6) ? 55504 . 55504
O(203) K(1) O(203) 110.9(8) ? . . 65602
O(203) K(1) O(203) 180.0(15) ? . . 65603
O(203) K(1) O(203) 69.1(8) ? . . 55504
O(203) K(1) O(204) 61.6(10) ? . . .
O(203) K(1) O(204) 58.6(13) ? . . 65602
O(203) K(1) O(204) 118.4(10) ? . . 65603
O(203) K(1) O(204) 121.4(12) ? . . 55504
O(203) K(1) O(205) 120.5(9) ? . . .
O(203) K(1) O(205) 32.0(11) ? . . 65602
O(203) K(1) O(205) 59.5(9) ? . . 65603
O(203) K(1) O(205) 148.0(11) ? . . 55504
O(203) K(1) O(206) 154.7(11) ? . . .
O(203) K(1) O(206) 79.5(7) ? . . 65602
O(203) K(1) O(206) 25.3(11) ? . . 65603
O(203) K(1) O(206) 100.5(7) ? . . 55504
O(203) K(1) O(203) 69.1(8) ? 65602 . 65603
O(203) K(1) O(203) 180.0(15) ? 65602 . 55504
O(203) K(1) O(204) 58.6(13) ? 65602 . .
O(203) K(1) O(204) 61.6(10) ? 65602 . 65602
O(203) K(1) O(204) 121.4(13) ? 65602 . 65603
O(203) K(1) O(204) 118.4(10) ? 65602 . 55504
O(203) K(1) O(205) 32.0(11) ? 65602 . .
O(203) K(1) O(205) 120.5(8) ? 65602 . 65602
O(203) K(1) O(205) 148.0(11) ? 65602 . 65603
O(203) K(1) O(205) 59.5(9) ? 65602 . 55504
O(203) K(1) O(206) 79.5(7) ? 65602 . .
O(203) K(1) O(206) 154.7(11) ? 65602 . 65602
O(203) K(1) O(206) 100.5(7) ? 65602 . 65603
O(203) K(1) O(206) 25.3(11) ? 65602 . 55504
O(203) K(1) O(203) 110.9(8) ? 65603 . 55504
O(203) K(1) O(204) 118.4(10) ? 65603 . .
O(203) K(1) O(204) 121.4(13) ? 65603 . 65602
O(203) K(1) O(204) 61.6(10) ? 65603 . 65603
O(203) K(1) O(204) 58.6(13) ? 65603 . 55504
O(203) K(1) O(205) 59.5(9) ? 65603 . .
O(203) K(1) O(205) 148.0(11) ? 65603 . 65602
O(203) K(1) O(205) 120.5(8) ? 65603 . 65603
O(203) K(1) O(205) 32.0(11) ? 65603 . 55504
O(203) K(1) O(206) 25.3(11) ? 65603 . .
O(203) K(1) O(206) 100.5(7) ? 65603 . 65602
O(203) K(1) O(206) 154.7(11) ? 65603 . 65603
O(203) K(1) O(206) 79.5(7) ? 65603 . 55504
O(203) K(1) O(204) 121.4(12) ? 55504 . .
O(203) K(1) O(204) 118.4(10) ? 55504 . 65602
O(203) K(1) O(204) 58.6(13) ? 55504 . 65603
O(203) K(1) O(204) 61.6(10) ? 55504 . 55504
O(203) K(1) O(205) 148.0(11) ? 55504 . .
O(203) K(1) O(205) 59.5(9) ? 55504 . 65602
O(203) K(1) O(205) 32.0(11) ? 55504 . 65603
O(203) K(1) O(205) 120.5(9) ? 55504 . 55504
O(203) K(1) O(206) 100.5(7) ? 55504 . .
O(203) K(1) O(206) 25.3(11) ? 55504 . 65602
O(203) K(1) O(206) 79.5(7) ? 55504 . 65603
O(203) K(1) O(206) 154.7(11) ? 55504 . 55504
O(204) K(1) O(204) 57.3(9) ? . . 65602
O(204) K(1) O(204) 180.0(17) ? . . 65603
O(204) K(1) O(204) 122.7(9) ? . . 55504
O(204) K(1) O(205) 58.8(10) ? . . .
O(204) K(1) O(205) 89.4(8) ? . . 65602
O(204) K(1) O(205) 121.2(10) ? . . 65603
O(204) K(1) O(205) 90.6(8) ? . . 55504
O(204) K(1) O(206) 110.4(7) ? . . .
O(204) K(1) O(206) 140.2(11) ? . . 65602
O(204) K(1) O(206) 69.6(7) ? . . 65603
O(204) K(1) O(206) 39.8(11) ? . . 55504
O(204) K(1) O(204) 122.7(9) ? 65602 . 65603
O(204) K(1) O(204) 180.0(17) ? 65602 . 55504
O(204) K(1) O(205) 89.4(8) ? 65602 . .
O(204) K(1) O(205) 58.8(10) ? 65602 . 65602
O(204) K(1) O(205) 90.6(8) ? 65602 . 65603
O(204) K(1) O(205) 121.2(10) ? 65602 . 55504
O(204) K(1) O(206) 140.2(11) ? 65602 . .
O(204) K(1) O(206) 110.4(7) ? 65602 . 65602
O(204) K(1) O(206) 39.8(11) ? 65602 . 65603
O(204) K(1) O(206) 69.6(7) ? 65602 . 55504
O(204) K(1) O(204) 57.3(9) ? 65603 . 55504
O(204) K(1) O(205) 121.2(10) ? 65603 . .
O(204) K(1) O(205) 90.6(8) ? 65603 . 65602
O(204) K(1) O(205) 58.8(10) ? 65603 . 65603
O(204) K(1) O(205) 89.4(8) ? 65603 . 55504
O(204) K(1) O(206) 69.6(7) ? 65603 . .
O(204) K(1) O(206) 39.8(11) ? 65603 . 65602
O(204) K(1) O(206) 110.4(7) ? 65603 . 65603
O(204) K(1) O(206) 140.2(11) ? 65603 . 55504
O(204) K(1) O(205) 90.6(8) ? 55504 . .
O(204) K(1) O(205) 121.2(10) ? 55504 . 65602
O(204) K(1) O(205) 89.4(8) ? 55504 . 65603
O(204) K(1) O(205) 58.8(10) ? 55504 . 55504
O(204) K(1) O(206) 39.8(11) ? 55504 . .
O(204) K(1) O(206) 69.6(7) ? 55504 . 65602
O(204) K(1) O(206) 140.2(11) ? 55504 . 65603
O(204) K(1) O(206) 110.4(7) ? 55504 . 55504
O(205) K(1) O(205) 145.0(3) ? . . 65602
O(205) K(1) O(205) 180.0(15) ? . . 65603
O(205) K(1) O(205) 35.0(3) ? . . 55504
O(205) K(1) O(206) 57.0(3) ? . . .
O(205) K(1) O(206) 158.0(3) ? . . 65602
O(205) K(1) O(206) 123.0(3) ? . . 65603
O(205) K(1) O(206) 22.0(3) ? . . 55504
O(205) K(1) O(205) 35.0(2) ? 65602 . 65603
O(205) K(1) O(205) 180.0(15) ? 65602 . 55504
O(205) K(1) O(206) 158.0(3) ? 65602 . .
O(205) K(1) O(206) 57.0(3) ? 65602 . 65602
O(205) K(1) O(206) 22.0(3) ? 65602 . 65603
O(205) K(1) O(206) 123.0(3) ? 65602 . 55504
O(205) K(1) O(205) 145.0(3) ? 65603 . 55504
O(205) K(1) O(206) 123.0(3) ? 65603 . .
O(205) K(1) O(206) 22.0(3) ? 65603 . 65602
O(205) K(1) O(206) 57.0(3) ? 65603 . 65603
O(205) K(1) O(206) 158.0(3) ? 65603 . 55504
O(205) K(1) O(206) 22.0(3) ? 55504 . .
O(205) K(1) O(206) 123.0(3) ? 55504 . 65602
O(205) K(1) O(206) 158.0(3) ? 55504 . 65603
O(205) K(1) O(206) 57.0(3) ? 55504 . 55504
O(206) K(1) O(206) 101.1(3) ? . . 65602
O(206) K(1) O(206) 180.0(10) ? . . 65603
O(206) K(1) O(206) 78.9(3) ? . . 55504
O(206) K(1) O(206) 78.9(3) ? 65602 . 65603
O(206) K(1) O(206) 180.0(10) ? 65602 . 55504
O(206) K(1) O(206) 101.1(3) ? 65603 . 55504
O(301) K(2) O(301) 157.7(13) ? . . 55504
O(301) K(2) O(302) 59.4(9) ? . . .
O(301) K(2) O(302) 142.7(10) ? . . 55504
O(301) K(2) O(303) 118.0(10) ? . . .
O(301) K(2) O(303) 84.2(9) ? . . 55504
O(301) K(2) O(304) 173.4(11) ? . . .
O(301) K(2) O(304) 26.2(11) ? . . 55504
O(301) K(2) O(305) 121.2(11) ? . . .
O(301) K(2) O(305) 36.5(10) ? . . 55504
O(301) K(2) O(306) 60.4(10) ? . . .
O(301) K(2) O(306) 97.6(10) ? . . 55504
O(301) K(2) O(302) 142.7(10) ? 55504 . .
O(301) K(2) O(302) 59.4(9) ? 55504 . 55504
O(301) K(2) O(303) 84.2(9) ? 55504 . .
O(301) K(2) O(303) 118.0(10) ? 55504 . 55504
O(301) K(2) O(304) 26.2(11) ? 55504 . .
O(301) K(2) O(304) 173.4(11) ? 55504 . 55504
O(301) K(2) O(305) 36.5(10) ? 55504 . .
O(301) K(2) O(305) 121.2(11) ? 55504 . 55504
O(301) K(2) O(306) 97.6(10) ? 55504 . .
O(301) K(2) O(306) 60.4(10) ? 55504 . 55504
O(302) K(2) O(302) 83.4(7) ? . . 55504
O(302) K(2) O(303) 59.7(6) ? . . .
O(302) K(2) O(303) 26.9(6) ? . . 55504
O(302) K(2) O(304) 116.6(10) ? . . .
O(302) K(2) O(304) 33.5(10) ? . . 55504
O(302) K(2) O(305) 173.7(12) ? . . .
O(302) K(2) O(305) 95.6(6) ? . . 55504
O(302) K(2) O(306) 117.7(6) ? . . .
O(302) K(2) O(306) 152.8(8) ? . . 55504
O(302) K(2) O(303) 26.9(6) ? 55504 . .
O(302) K(2) O(303) 59.7(6) ? 55504 . 55504
O(302) K(2) O(304) 33.5(10) ? 55504 . .
O(302) K(2) O(304) 116.6(10) ? 55504 . 55504
O(302) K(2) O(305) 95.6(6) ? 55504 . .
O(302) K(2) O(305) 173.7(12) ? 55504 . 55504
O(302) K(2) O(306) 152.8(8) ? 55504 . .
O(302) K(2) O(306) 117.7(6) ? 55504 . 55504
O(303) K(2) O(303) 33.8(3) ? . . 55504
O(303) K(2) O(304) 59.5(10) ? . . .
O(303) K(2) O(304) 93.0(10) ? . . 55504
O(303) K(2) O(305) 120.7(6) ? . . .
O(303) K(2) O(305) 154.3(6) ? . . 55504
O(303) K(2) O(306) 175.2(8) ? . . .
O(303) K(2) O(306) 144.2(3) ? . . 55504
O(303) K(2) O(304) 93.0(10) ? 55504 . .
O(303) K(2) O(304) 59.5(10) ? 55504 . 55504
O(303) K(2) O(305) 154.3(6) ? 55504 . .
O(303) K(2) O(305) 120.7(6) ? 55504 . 55504
O(303) K(2) O(306) 144.2(3) ? 55504 . .
O(303) K(2) O(306) 175.2(8) ? 55504 . 55504
O(304) K(2) O(304) 149.0(11) ? . . 55504
O(304) K(2) O(305) 62.1(10) ? . . .
O(304) K(2) O(305) 146.2(12) ? . . 55504
O(304) K(2) O(306) 121.6(11) ? . . .
O(304) K(2) O(306) 84.7(10) ? . . 55504
O(304) K(2) O(305) 146.2(12) ? 55504 . .
O(304) K(2) O(305) 62.1(10) ? 55504 . 55504
O(304) K(2) O(306) 84.7(10) ? 55504 . .
O(304) K(2) O(306) 121.6(11) ? 55504 . 55504
O(305) K(2) O(305) 84.7(8) ? . . 55504
O(305) K(2) O(306) 61.5(6) ? . . .
O(305) K(2) O(306) 24.7(7) ? . . 55504
O(305) K(2) O(306) 24.7(7) ? 55504 . .
O(305) K(2) O(306) 61.5(6) ? 55504 . 55504
O(306) K(2) O(306) 37.3(4) ? . . 55504
O(401) K(3) O(401) 123.8(16) ? . . 65502
O(401) K(3) O(402) 57.1(18) ? . . .
O(401) K(3) O(402) 91.7(16) ? . . 65502
O(401) K(3) O(403) 111.2(18) ? . . .
O(401) K(3) O(403) 56.9(18) ? . . 65502
O(401) K(3) O(404) 146.7(16) ? . . .
O(401) K(3) O(404) 23.1(13) ? . . 65502
O(401) K(3) O(405) 118.2(19) ? . . .
O(401) K(3) O(405) 61.2(19) ? . . 65502
O(401) K(3) O(406) 58.4(18) ? . . .
O(401) K(3) O(406) 99.2(18) ? . . 65502
O(401) K(3) O(402) 91.7(16) ? 65502 . .
O(401) K(3) O(402) 57.1(18) ? 65502 . 65502
O(401) K(3) O(403) 56.9(18) ? 65502 . .
O(401) K(3) O(403) 111.2(18) ? 65502 . 65502
O(401) K(3) O(404) 23.1(13) ? 65502 . .
O(401) K(3) O(404) 146.7(16) ? 65502 . 65502
O(401) K(3) O(405) 61.2(19) ? 65502 . .
O(401) K(3) O(405) 118.2(19) ? 65502 . 65502
O(401) K(3) O(406) 99.2(18) ? 65502 . .
O(401) K(3) O(406) 58.4(18) ? 65502 . 65502
O(402) K(3) O(402) 113.9(15) ? . . 65502
O(402) K(3) O(403) 54.2(17) ? . . .
O(402) K(3) O(403) 111.8(18) ? . . 65502
O(402) K(3) O(404) 104.4(17) ? . . .
O(402) K(3) O(404) 69.8(17) ? . . 65502
O(402) K(3) O(405) 145.1(16) ? . . .
O(402) K(3) O(405) 33.8(14) ? . . 65502
O(402) K(3) O(406) 108.1(18) ? . . .
O(402) K(3) O(406) 43.0(17) ? . . 65502
O(402) K(3) O(403) 111.8(18) ? 65502 . .
O(402) K(3) O(403) 54.2(17) ? 65502 . 65502
O(402) K(3) O(404) 69.8(17) ? 65502 . .
O(402) K(3) O(404) 104.4(16) ? 65502 . 65502
O(402) K(3) O(405) 33.8(13) ? 65502 . .
O(402) K(3) O(405) 145.1(16) ? 65502 . 65502
O(402) K(3) O(406) 43.0(17) ? 65502 . .
O(402) K(3) O(406) 108.1(18) ? 65502 . 65502
O(403) K(3) O(403) 157.4(17) ? . . 65502
O(403) K(3) O(404) 56.1(18) ? . . .
O(403) K(3) O(404) 121.5(18) ? . . 65502
O(403) K(3) O(405) 115.0(19) ? . . .
O(403) K(3) O(405) 64.8(19) ? . . 65502
O(403) K(3) O(406) 145.4(17) ? . . .
O(403) K(3) O(406) 13.1(16) ? . . 65502
O(403) K(3) O(404) 121.5(18) ? 65502 . .
O(403) K(3) O(404) 56.1(18) ? 65502 . 65502
O(403) K(3) O(405) 64.8(19) ? 65502 . .
O(403) K(3) O(405) 115.0(19) ? 65502 . 65502
O(403) K(3) O(406) 13.1(16) ? 65502 . .
O(403) K(3) O(406) 145.4(18) ? 65502 . 65502
O(404) K(3) O(404) 169.8(15) ? . . 65502
O(404) K(3) O(405) 59.2(19) ? . . .
O(404) K(3) O(405) 121(2) ? . . 65502
O(404) K(3) O(406) 112.3(18) ? . . .
O(404) K(3) O(406) 63.4(18) ? . . 65502
O(404) K(3) O(405) 120.7(19) ? 65502 . .
O(404) K(3) O(405) 59.2(19) ? 65502 . 65502
O(404) K(3) O(406) 63.4(17) ? 65502 . .
O(404) K(3) O(406) 112.3(17) ? 65502 . 65502
O(405) K(3) O(405) 179(2) ? . . 65502
O(405) K(3) O(406) 60.2(19) ? . . .
O(405) K(3) O(406) 119.3(19) ? . . 65502
O(405) K(3) O(406) 119.3(19) ? 65502 . .
O(405) K(3) O(406) 60.2(19) ? 65502 . 65502
O(406) K(3) O(406) 134.6(18) ? . . 65502
O(504) K(4) O(503) 55.8 ? . . .
O(504) K(4) O(502) 107.7 ? . . .
O(504) K(4) O(501) 139.5 ? . . .
O(504) K(4) O(506) 99.7 ? . . .
O(504) K(4) O(505) 53.7 ? . . .
O(503) K(4) O(502) 60.1 ? . . .
O(503) K(4) O(501) 119.2 ? . . .
O(503) K(4) O(506) 140.3 ? . . .
O(503) K(4) O(505) 109.2 ? . . .
O(502) K(4) O(501) 60.3 ? . . .
O(502) K(4) O(506) 109.2 ? . . .
O(502) K(4) O(505) 141.1 ? . . .
O(501) K(4) O(506) 56.9 ? . . .
O(501) K(4) O(505) 109.2 ? . . .
O(506) K(4) O(505) 52.7 ? . . .
O(15) Si(1) O(15) 111.2(7) ? . . 56504
O(15) Si(1) O(16) 109.2(7) ? . . .
O(15) Si(1) O(17) 110.2(7) ? . . .
O(15) Si(1) O(16) 109.2(7) ? 56504 . .
O(15) Si(1) O(17) 110.2(7) ? 56504 . .
O(16) Si(1) O(17) 106.9(10) ? . . .
Ti(1) O(1) Ti(1) 104.4(12) ? . . 56504
Ti(1) O(1) C(1) 125.5(9) ? . . .
Ti(1) O(1) C(1) 125.5(9) ? 56504 . .
Ti(1) O(2) Ti(1) 104.5(14) ? . . 56504
Ti(1) O(2) C(2) 123.8(12) ? . . .
Ti(1) O(2) C(2) 123.8(12) ? 56504 . .
W(1) O(3) Ti(1) 119.9(8) ? . . .
W(2) O(4) Ti(1) 120.1(8) ? . . .
W(1) O(5) W(3) 145.2(8) ? . . .
W(2) O(6) W(4) 145.5(7) ? . . .
W(1) O(7) W(2) 120.7(7) ? . . .
W(1) O(8) W(5) 147.3(8) ? . . .
W(2) O(9) W(6) 146.4(8) ? . . .
W(3) O(10) W(5) 118.9(8) ? . . .
W(4) O(11) W(6) 119.0(8) ? . . .
W(5) O(12) W(5) 121.9(9) ? . . 56504
W(6) O(13) W(6) 121.8(10) ? . . 56504
W(5) O(14) W(6) 159.2(7) ? . . .
W(1) O(15) W(2) 91.2(4) ? . . .
W(1) O(15) Ti(1) 87.0(4) ? . . .
W(1) O(15) Si(1) 125.6(8) ? . . .
W(2) O(15) Ti(1) 86.5(4) ? . . .
W(2) O(15) Si(1) 123.8(8) ? . . .
Ti(1) O(15) Si(1) 130.2(7) ? . . .
W(3) O(16) W(5) 89.9(6) ? . . .
W(3) O(16) W(5) 89.9(6) ? . . 56504
W(3) O(16) Si(1) 124.0(10) ? . . .
W(5) O(16) W(5) 91.0(5) ? . . 56504
W(5) O(16) Si(1) 125.6(6) ? . . .
W(5) O(16) Si(1) 125.6(6) ? 56504 . .
W(4) O(17) W(6) 89.3(6) ? . . .
W(4) O(17) W(6) 89.3(6) ? . . 56504
W(4) O(17) Si(1) 124.7(9) ? . . .
W(6) O(17) W(6) 90.2(6) ? . . 56504
W(6) O(17) Si(1) 126.0(7) ? . . .
W(6) O(17) Si(1) 126.0(7) ? 56504 . .
Ti(1) O(101) Ti(1) 158.8(12) ? . . 65602
K(1) O(201) O(204) 76.5(5) ? . . 65603
K(1) O(201) O(204) 76.5(5) ? . . 55504
K(1) O(201) C(201) 107.0(3) ? . . .
K(1) O(201) C(201) 107.0(3) ? . . 65602
K(1) O(201) C(206) 115.1(12) ? . . 65603
K(1) O(201) C(206) 115.1(11) ? . . 55504
K(1) O(201) C(212) 138.5(3) ? . . .
K(1) O(201) C(212) 138.5(3) ? . . 65602
O(204) O(201) O(204) 153.1(8) ? 65603 . 55504
O(204) O(201) C(201) 79(2) ? 65603 . .
O(204) O(201) C(201) 110(2) ? 65603 . 65602
O(204) O(201) C(206) 64(2) ? 65603 . 65603
O(204) O(201) C(206) 129(2) ? 65603 . 55504
O(204) O(201) C(212) 129.8(15) ? 65603 . .
O(204) O(201) C(212) 73.0(10) ? 65603 . 65602
O(204) O(201) C(201) 110(2) ? 55504 . .
O(204) O(201) C(201) 78.5(19) ? 55504 . 65602
O(204) O(201) C(206) 129(2) ? 55504 . 65603
O(204) O(201) C(206) 64(2) ? 55504 . 55504
O(204) O(201) C(212) 73.0(10) ? 55504 . .
O(204) O(201) C(212) 129.8(15) ? 55504 . 65602
C(201) O(201) C(201) 146.0(5) ? . . 65602
C(201) O(201) C(206) 112.8(18) ? . . 65603
C(201) O(201) C(206) 50.5(19) ? . . 55504
C(201) O(201) C(212) 109.4(7) ? . . .
C(201) O(201) C(212) 39.7(8) ? . . 65602
C(201) O(201) C(206) 50.5(19) ? 65602 . 65603
C(201) O(201) C(206) 112.8(18) ? 65602 . 55504
C(201) O(201) C(212) 39.7(8) ? 65602 . .
C(201) O(201) C(212) 109.4(7) ? 65602 . 65602
C(206) O(201) C(206) 129.8(16) ? 65603 . 55504
C(206) O(201) C(212) 67.3(16) ? 65603 . .
C(206) O(201) C(212) 75.6(18) ? 65603 . 65602
C(206) O(201) C(212) 75.6(17) ? 55504 . .
C(206) O(201) C(212) 67.3(16) ? 55504 . 65602
C(212) O(201) C(212) 83.0(5) ? . . 65602
K(1) O(202) O(203) 74(5) ? . . 55504
K(1) O(202) O(205) 76(2) ? . . 65603
K(1) O(202) O(206) 81(2) ? . . 65602
K(1) O(202) C(202) 109(2) ? . . .
K(1) O(202) C(203) 103.8(18) ? . . .
K(1) O(202) C(204) 136(2) ? . . 55504
K(1) O(202) C(210) 131(3) ? . . 65602
O(203) O(202) O(205) 120(7) ? 55504 . 65603
O(203) O(202) O(206) 72(5) ? 55504 . 65602
O(203) O(202) C(202) 71(3) ? 55504 . .
O(203) O(202) C(203) 173(5) ? 55504 . .
O(203) O(202) C(204) 121(7) ? 55504 . 55504
O(203) O(202) C(210) 130(4) ? 55504 . 65602
O(205) O(202) O(206) 52(2) ? 65603 . 65602
O(205) O(202) C(202) 72(2) ? 65603 . .
O(205) O(202) C(203) 65(3) ? 65603 . .
O(205) O(202) C(204) 116(4) ? 65603 . 55504
O(205) O(202) C(210) 55(3) ? 65603 . 65602
O(206) O(202) C(202) 31(2) ? 65602 . .
O(206) O(202) C(203) 115(3) ? 65602 . .
O(206) O(202) C(204) 142(4) ? 65602 . 55504
O(206) O(202) C(210) 72(3) ? 65602 . 65602
C(202) O(202) C(203) 116(2) ? . . .
C(202) O(202) C(204) 115(3) ? . . 55504
C(202) O(202) C(210) 60(2) ? . . 65602
C(203) O(202) C(204) 55(3) ? . . 55504
C(203) O(202) C(210) 57(2) ? . . 65602
C(204) O(202) C(210) 74(4) ? 55504 . 65602
K(1) O(203) O(202) 94(4) ? . . 55504
K(1) O(203) O(205) 76(2) ? . . 65602
K(1) O(203) O(206) 86(2) ? . . 65603
K(1) O(203) C(202) 118(3) ? . . 55504
K(1) O(203) C(204) 119.7(11) ? . . .
K(1) O(203) C(205) 115(3) ? . . .
K(1) O(203) C(210) 115(2) ? . . 65603
K(1) O(203) C(211) 111(2) ? . . 65603
O(202) O(203) O(205) 41(5) ? 55504 . 65602
O(202) O(203) O(206) 82(5) ? 55504 . 65603
O(202) O(203) C(202) 85(5) ? 55504 . 55504
O(202) O(203) C(204) 39(5) ? 55504 . .
O(202) O(203) C(205) 148(8) ? 55504 . .
O(202) O(203) C(210) 33(3) ? 55504 . 65603
O(202) O(203) C(211) 128(5) ? 55504 . 65603
O(205) O(203) O(206) 45.2(18) ? 65602 . 65603
O(205) O(203) C(202) 63(2) ? 65602 . 55504
O(205) O(203) C(204) 79(3) ? 65602 . .
O(205) O(203) C(205) 154(2) ? 65602 . .
O(205) O(203) C(210) 40(2) ? 65602 . 65603
O(205) O(203) C(211) 100(2) ? 65602 . 65603
O(206) O(203) C(202) 32(2) ? 65603 . 55504
O(206) O(203) C(204) 112(3) ? 65603 . .
O(206) O(203) C(205) 110(2) ? 65603 . .
O(206) O(203) C(210) 61(2) ? 65603 . 65603
O(206) O(203) C(211) 56.2(14) ? 65603 . 65603
C(202) O(203) C(204) 97(3) ? 55504 . .
C(202) O(203) C(205) 91.6(19) ? 55504 . .
C(202) O(203) C(210) 53(2) ? 55504 . 65603
C(202) O(203) C(211) 42.8(12) ? 55504 . 65603
C(204) O(203) C(205) 112(4) ? . . .
C(204) O(203) C(210) 51(3) ? . . 65603
C(204) O(203) C(211) 127(3) ? . . 65603
C(205) O(203) C(210) 128(3) ? . . 65603
C(205) O(203) C(211) 54.3(19) ? . . 65603
C(210) O(203) C(211) 94(2) ? 65603 . 65603
K(1) O(204) O(201) 74.8(11) ? . . 65603
K(1) O(204) C(206) 108.5(18) ? . . .
K(1) O(204) C(207) 111(2) ? . . .
K(1) O(204) C(212) 116(2) ? . . 55504
O(201) O(204) C(206) 54(2) ? 65603 . .
O(201) O(204) C(207) 90(3) ? 65603 . .
O(201) O(204) C(212) 46.2(11) ? 65603 . 55504
C(206) O(204) C(207) 116(2) ? . . .
C(206) O(204) C(212) 61(2) ? . . 55504
C(207) O(204) C(212) 56.8(18) ? . . 55504
K(1) O(205) O(202) 80(2) ? . . 65603
K(1) O(205) O(203) 72.0(19) ? . . 65602
K(1) O(205) O(205) 72.5(14) ? . . 55504
K(1) O(205) O(206) 86(2) ? . . 55504
K(1) O(205) C(202) 107.2(17) ? . . 65603
K(1) O(205) C(203) 107.5(18) ? . . 65602
K(1) O(205) C(208) 120(3) ? . . .
K(1) O(205) C(209) 124.1(12) ? . . .
K(1) O(205) C(210) 139(3) ? . . 55504
O(202) O(205) O(203) 18(2) ? 65603 . 65602
O(202) O(205) O(205) 107(2) ? 65603 . 55504
O(202) O(205) O(206) 70(2) ? 65603 . 55504
O(202) O(205) C(202) 60.8(18) ? 65603 . 65603
O(202) O(205) C(203) 71(3) ? 65603 . 65602
O(202) O(205) C(208) 105(2) ? 65603 . .
O(202) O(205) C(209) 115(5) ? 65603 . .
O(202) O(205) C(210) 59(3) ? 65603 . 55504
O(203) O(205) O(205) 118(2) ? 65602 . 55504
O(203) O(205) O(206) 54(2) ? 65602 . 55504
O(203) O(205) C(202) 51.3(16) ? 65602 . 65603
O(203) O(205) C(203) 89(3) ? 65602 . 65602
O(203) O(205) C(208) 94.2(18) ? 65602 . .
O(203) O(205) C(209) 133(5) ? 65602 . .
O(203) O(205) C(210) 69(3) ? 65602 . 55504
O(205) O(205) O(206) 158(3) ? 55504 . 55504
O(205) O(205) C(202) 167(4) ? 55504 . 65603
O(205) O(205) C(203) 57(2) ? 55504 . 65602
O(205) O(205) C(208) 148(3) ? 55504 . .
O(205) O(205) C(209) 51.7(15) ? 55504 . .
O(205) O(205) C(210) 115(3) ? 55504 . 55504
O(206) O(205) C(202) 27(2) ? 55504 . 65603
O(206) O(205) C(203) 136(4) ? 55504 . 65602
O(206) O(205) C(208) 45.4(15) ? 55504 . .
O(206) O(205) C(209) 150(2) ? 55504 . .
O(206) O(205) C(210) 83(2) ? 55504 . 55504
C(202) O(205) C(203) 112(3) ? 65603 . 65602
C(202) O(205) C(208) 44(2) ? 65603 . .
C(202) O(205) C(209) 127(3) ? 65603 . .
C(202) O(205) C(210) 56(2) ? 65603 . 55504
C(203) O(205) C(208) 131(4) ? 65602 . .
C(203) O(205) C(209) 45(3) ? 65602 . .
C(203) O(205) C(210) 59(3) ? 65602 . 55504
C(208) O(205) C(209) 108(2) ? . . .
C(208) O(205) C(210) 76(3) ? . . 55504
C(209) O(205) C(210) 77(3) ? . . 55504
K(1) O(206) O(202) 73.2(16) ? . . 65602
K(1) O(206) O(203) 69.0(19) ? . . 65603
K(1) O(206) O(205) 72.4(18) ? . . 55504
K(1) O(206) C(201) 102.3(10) ? . . 65602
K(1) O(206) C(202) 147(3) ? . . 65602
K(1) O(206) C(207) 111(2) ? . . 55504
K(1) O(206) C(208) 135(3) ? . . 55504
K(1) O(206) C(210) 109.4(10) ? . . .
K(1) O(206) C(211) 110.6(12) ? . . .
O(202) O(206) O(203) 25(2) ? 65602 . 65603
O(202) O(206) O(205) 57(3) ? 65602 . 55504
O(202) O(206) C(201) 102(2) ? 65602 . 65602
O(202) O(206) C(202) 80(4) ? 65602 . 65602
O(202) O(206) C(207) 143(3) ? 65602 . 55504
O(202) O(206) C(208) 123(4) ? 65602 . 55504
O(202) O(206) C(210) 47(2) ? 65602 . .
O(202) O(206) C(211) 97(2) ? 65602 . .
O(203) O(206) O(205) 81(2) ? 65603 . 55504
O(203) O(206) C(201) 79.0(15) ? 65603 . 65602
O(203) O(206) C(202) 78(4) ? 65603 . 65602
O(203) O(206) C(207) 119(2) ? 65603 . 55504
O(203) O(206) C(208) 144(5) ? 65603 . 55504
O(203) O(206) C(210) 69(3) ? 65603 . .
O(203) O(206) C(211) 75.8(18) ? 65603 . .
O(205) O(206) C(201) 159(3) ? 55504 . 65602
O(205) O(206) C(202) 110(4) ? 55504 . 65602
O(205) O(206) C(207) 160(4) ? 55504 . 55504
O(205) O(206) C(208) 84(2) ? 55504 . 55504
O(205) O(206) C(210) 47(3) ? 55504 . .
O(205) O(206) C(211) 153(4) ? 55504 . .
C(201) O(206) C(202) 63(2) ? 65602 . 65602
C(201) O(206) C(207) 41(2) ? 65602 . 55504
C(201) O(206) C(208) 111.9(7) ? 65602 . 55504
C(201) O(206) C(210) 121(2) ? 65602 . .
C(201) O(206) C(211) 11.4(14) ? 65602 . .
C(202) O(206) C(207) 79(3) ? 65602 . 55504
C(202) O(206) C(208) 77(4) ? 65602 . 55504
C(202) O(206) C(210) 63(3) ? 65602 . .
C(202) O(206) C(211) 52(2) ? 65602 . .
C(207) O(206) C(208) 81(2) ? 55504 . 55504
C(207) O(206) C(210) 139(2) ? 55504 . .
C(207) O(206) C(211) 46(2) ? 55504 . .
C(208) O(206) C(210) 77(3) ? 55504 . .
C(208) O(206) C(211) 107.8(13) ? 55504 . .
C(210) O(206) C(211) 110(3) ? . . .
K(2) O(301) O(304) 74.8(7) ? . . 55504
K(2) O(301) C(301) 116(2) ? . . .
K(2) O(301) C(307) 157(5) ? . . 55504
K(2) O(301) C(308) 114.2(19) ? . . 55504
K(2) O(301) C(312) 115.8(18) ? . . .
O(304) O(301) C(301) 42.1(17) ? 55504 . .
O(304) O(301) C(307) 83(4) ? 55504 . 55504
O(304) O(301) C(308) 139(4) ? 55504 . 55504
O(304) O(301) C(312) 146(4) ? 55504 . .
C(301) O(301) C(307) 43(3) ? . . 55504
C(301) O(301) C(308) 111(3) ? . . 55504
C(301) O(301) C(312) 115(3) ? . . .
C(307) O(301) C(308) 86(5) ? 55504 . 55504
C(307) O(301) C(312) 86(5) ? 55504 . .
C(308) O(301) C(312) 7(2) ? 55504 . .
K(2) O(302) O(303) 75.8(13) ? . . 55504
K(2) O(302) O(304) 70.9(12) ? . . 55504
K(2) O(302) C(302) 116(2) ? . . .
K(2) O(302) C(303) 113.5(9) ? . . .
K(2) O(302) C(305) 153(2) ? . . 55504
K(2) O(302) C(306) 115(2) ? . . 55504
O(303) O(302) O(304) 142(2) ? 55504 . 55504
O(303) O(302) C(302) 136(4) ? 55504 . .
O(303) O(302) C(303) 37.8(15) ? 55504 . .
O(303) O(302) C(305) 77(2) ? 55504 . 55504
O(303) O(302) C(306) 127(4) ? 55504 . 55504
O(304) O(302) C(302) 52(2) ? 55504 . .
O(304) O(302) C(303) 158(3) ? 55504 . .
O(304) O(302) C(305) 133.4(11) ? 55504 . 55504
O(304) O(302) C(306) 57(2) ? 55504 . 55504
C(302) O(302) C(303) 111(3) ? . . .
C(302) O(302) C(305) 83(2) ? . . 55504
C(302) O(302) C(306) 9(3) ? . . 55504
C(303) O(302) C(305) 40(2) ? . . 55504
C(303) O(302) C(306) 105(3) ? . . 55504
C(305) O(302) C(306) 81(2) ? 55504 . 55504
K(2) O(303) O(302) 77.2(18) ? . . 55504
K(2) O(303) O(303) 73.1(13) ? . . 55504
K(2) O(303) C(303) 156(2) ? . . 55504
K(2) O(303) C(304) 118.5(13) ? . . .
K(2) O(303) C(305) 117(2) ? . . .
O(302) O(303) O(303) 144(2) ? 55504 . 55504
O(302) O(303) C(303) 79(2) ? 55504 . 55504
O(302) O(303) C(304) 131(2) ? 55504 . .
O(302) O(303) C(305) 39(2) ? 55504 . .
O(303) O(303) C(303) 131(2) ? 55504 . 55504
O(303) O(303) C(304) 53.6(12) ? 55504 . .
O(303) O(303) C(305) 159(2) ? 55504 . .
C(303) O(303) C(304) 81(2) ? 55504 . .
C(303) O(303) C(305) 40(2) ? 55504 . .
C(304) O(303) C(305) 108(2) ? . . .
K(2) O(304) O(301) 79.1(9) ? . . 55504
K(2) O(304) O(302) 75.6(6) ? . . 55504
K(2) O(304) C(301) 156(4) ? . . 55504
K(2) O(304) C(302) 124(2) ? . . 55504
K(2) O(304) C(306) 115(2) ? . . .
K(2) O(304) C(307) 113(2) ? . . .
O(301) O(304) O(302) 152.6(19) ? 55504 . 55504
O(301) O(304) C(301) 79(3) ? 55504 . 55504
O(301) O(304) C(302) 135(3) ? 55504 . 55504
O(301) O(304) C(306) 136(4) ? 55504 . .
O(301) O(304) C(307) 34.6(16) ? 55504 . .
O(302) O(304) C(301) 127(4) ? 55504 . 55504
O(302) O(304) C(302) 57(2) ? 55504 . 55504
O(302) O(304) C(306) 51(2) ? 55504 . .
O(302) O(304) C(307) 164(4) ? 55504 . .
C(301) O(304) C(302) 78(4) ? 55504 . 55504
C(301) O(304) C(306) 87(4) ? 55504 . .
C(301) O(304) C(307) 46(3) ? 55504 . .
C(302) O(304) C(306) 9.7(18) ? 55504 . .
C(302) O(304) C(307) 108(2) ? 55504 . .
C(306) O(304) C(307) 113(3) ? . . .
K(2) O(305) O(306) 82.8(14) ? . . 55504
K(2) O(305) C(308) 115(2) ? . . .
K(2) O(305) C(309) 114.9(8) ? . . .
K(2) O(305) C(311) 160(2) ? . . 55504
K(2) O(305) C(312) 123(2) ? . . 55504
O(306) O(305) C(308) 133(4) ? 55504 . .
O(306) O(305) C(309) 32.2(16) ? 55504 . .
O(306) O(305) C(311) 85(3) ? 55504 . 55504
O(306) O(305) C(312) 134(4) ? 55504 . 55504
C(308) O(305) C(309) 113(3) ? . . .
C(308) O(305) C(311) 84(2) ? . . 55504
C(308) O(305) C(312) 9(2) ? . . 55504
C(309) O(305) C(311) 54(3) ? . . 55504
C(309) O(305) C(312) 109(3) ? . . 55504
C(311) O(305) C(312) 76(2) ? 55504 . 55504
K(2) O(306) O(305) 72.5(19) ? . . 55504
K(2) O(306) C(309) 165(2) ? . . 55504
K(2) O(306) C(310) 111.2(14) ? . . .
K(2) O(306) C(311) 111(2) ? . . .
O(305) O(306) C(309) 93(2) ? 55504 . 55504
O(305) O(306) C(310) 137(2) ? 55504 . .
O(305) O(306) C(311) 40(2) ? 55504 . .
C(309) O(306) C(310) 81(2) ? 55504 . .
C(309) O(306) C(311) 55(2) ? 55504 . .
C(310) O(306) C(311) 111(2) ? . . .
K(3) O(401) O(404) 88(3) ? . . 65502
K(3) O(401) C(412) 119(3) ? . . .
K(3) O(401) C(401) 124(4) ? . . .
O(404) O(401) C(412) 92(6) ? 65502 . .
O(404) O(401) C(401) 117(5) ? 65502 . .
C(412) O(401) C(401) 111(5) ? . . .
K(3) O(402) O(405) 63(2) ? . . 65502
K(3) O(402) C(402) 106(4) ? . . .
K(3) O(402) C(403) 111(3) ? . . .
K(3) O(402) C(409) 100(3) ? . . 65502
O(405) O(402) C(402) 71(3) ? 65502 . .
O(405) O(402) C(403) 79(4) ? 65502 . .
O(405) O(402) C(409) 51(4) ? 65502 . 65502
C(402) O(402) C(403) 112(5) ? . . .
C(402) O(402) C(409) 90(4) ? . . 65502
C(403) O(402) C(409) 29(4) ? . . 65502
K(3) O(403) O(406) 70(7) ? . . 65502
K(3) O(403) C(411) 113(5) ? . . 65502
K(3) O(403) C(404) 122(4) ? . . .
K(3) O(403) C(405) 119(4) ? . . .
K(3) O(403) C(410) 101(3) ? . . 65502
O(406) O(403) C(411) 109(9) ? 65502 . 65502
O(406) O(403) C(404) 59(7) ? 65502 . .
O(406) O(403) C(405) 128(9) ? 65502 . .
O(406) O(403) C(410) 74(8) ? 65502 . 65502
C(411) O(403) C(404) 109(6) ? 65502 . .
C(411) O(403) C(405) 19(4) ? 65502 . .
C(411) O(403) C(410) 145(7) ? 65502 . 65502
C(404) O(403) C(405) 114(5) ? . . .
C(404) O(403) C(410) 41(4) ? . . 65502
C(405) O(403) C(410) 138(6) ? . . 65502
K(3) O(404) O(401) 69(3) ? . . 65502
K(3) O(404) C(406) 106(3) ? . . .
K(3) O(404) C(407) 102(4) ? . . .
O(401) O(404) C(406) 122(6) ? 65502 . .
O(401) O(404) C(407) 126(6) ? 65502 . .
C(406) O(404) C(407) 112(5) ? . . .
K(3) O(405) O(402) 84(2) ? . . 65502
K(3) O(405) C(408) 120(5) ? . . .
K(3) O(405) C(409) 120(3) ? . . .
O(402) O(405) C(408) 105(4) ? 65502 . .
O(402) O(405) C(409) 58(4) ? 65502 . .
C(408) O(405) C(409) 113(5) ? . . .
K(3) O(406) O(403) 97(7) ? . . 65502
K(3) O(406) C(411) 107(4) ? . . .
K(3) O(406) C(404) 149(5) ? . . 65502
K(3) O(406) C(410) 109(4) ? . . .
O(403) O(406) C(411) 43(6) ? 65502 . .
O(403) O(406) C(404) 92(8) ? 65502 . 65502
O(403) O(406) C(410) 78(8) ? 65502 . .
C(411) O(406) C(404) 100(5) ? . . 65502
C(411) O(406) C(410) 113(5) ? . . .
C(404) O(406) C(410) 44(4) ? 65502 . .
K(4) O(504) C(506) 104.9 ? . . .
K(4) O(504) C(507) 108.1 ? . . .
C(506) O(504) C(507) 111.2 ? . . .
K(4) O(503) C(505) 126.7 ? . . .
K(4) O(503) C(504) 116.3 ? . . .
C(505) O(503) C(504) 113.4 ? . . .
K(4) O(502) C(503) 103.9 ? . . .
K(4) O(502) C(502) 105.7 ? . . .
C(503) O(502) C(502) 112.8 ? . . .
K(4) O(501) O(501) 143.0 ? . . 55504
K(4) O(501) C(501) 117.0 ? . . .
K(4) O(501) C(512) 126.5 ? . . .
O(501) O(501) C(501) 51.7 ? 55504 . .
O(501) O(501) C(512) 55.6 ? 55504 . .
C(501) O(501) C(512) 106.5 ? . . .
K(4) O(506) C(511) 104.7 ? . . .
K(4) O(506) C(510) 110.6 ? . . .
C(511) O(506) C(510) 114.8 ? . . .
K(4) O(505) C(509) 124.2 ? . . .
K(4) O(505) C(508) 119.9 ? . . .
C(509) O(505) C(508) 111.2 ? . . .
O(401) C(412) C(411) 108(5) ? . . .
O(401) C(412) C(405) 114(4) ? . . 65502
C(411) C(412) C(405) 20(3) ? . . 65502
O(403) C(411) O(406) 27(4) ? 65502 . .
O(403) C(411) C(412) 131(6) ? 65502 . .
O(403) C(411) C(405) 125(12) ? 65502 . 65502
O(403) C(411) C(406) 111(6) ? 65502 . 65502
O(406) C(411) C(412) 108(5) ? . . .
O(406) C(411) C(405) 152(12) ? . . 65502
O(406) C(411) C(406) 128(5) ? . . 65502
C(412) C(411) C(405) 99(11) ? . . 65502
C(412) C(411) C(406) 79(4) ? . . 65502
C(405) C(411) C(406) 50(9) ? 65502 . 65502
O(201) C(201) O(206) 92.8(12) ? . . 65602
O(201) C(201) C(202) 118.2(13) ? . . .
O(201) C(201) C(205) 95(2) ? . . 55504
O(201) C(201) C(206) 47(2) ? . . 55504
O(201) C(201) C(207) 88(2) ? . . 65603
O(201) C(201) C(211) 136(2) ? . . 65602
O(201) C(201) C(212) 40.6(7) ? . . 65602
O(206) C(201) C(202) 25.8(17) ? 65602 . .
O(206) C(201) C(205) 89.4(17) ? 65602 . 55504
O(206) C(201) C(206) 122.8(8) ? 65602 . 55504
O(206) C(201) C(207) 48(2) ? 65602 . 65603
O(206) C(201) C(211) 46(3) ? 65602 . 65602
O(206) C(201) C(212) 114(2) ? 65602 . 65602
C(202) C(201) C(205) 83(2) ? . . 55504
C(202) C(201) C(206) 137.0(15) ? . . 55504
C(202) C(201) C(207) 59(3) ? . . 65603
C(202) C(201) C(211) 21(4) ? . . 65602
C(202) C(201) C(212) 136(2) ? . . 65602
C(205) C(201) C(206) 62(3) ? 55504 . 55504
C(205) C(201) C(207) 137(2) ? 55504 . 65603
C(205) C(201) C(211) 73(5) ? 55504 . 65602
C(205) C(201) C(212) 127(2) ? 55504 . 65602
C(206) C(201) C(207) 135(4) ? 55504 . 65603
C(206) C(201) C(211) 134(5) ? 55504 . 65602
C(206) C(201) C(212) 65(2) ? 55504 . 65602
C(207) C(201) C(211) 76(5) ? 65603 . 65602
C(207) C(201) C(212) 80(3) ? 65603 . 65602
C(211) C(201) C(212) 156(5) ? 65602 . 65602
O(202) C(202) O(203) 23.9(18) ? . . 55504
O(202) C(202) O(205) 48(2) ? . . 65603
O(202) C(202) O(206) 69(2) ? . . 65602
O(202) C(202) C(201) 108(2) ? . . .
O(202) C(202) C(207) 128(3) ? . . 65603
O(202) C(202) C(208) 110.8(17) ? . . 65603
O(202) C(202) C(210) 48(2) ? . . 65602
O(202) C(202) C(211) 108(2) ? . . 65602
O(203) C(202) O(205) 65.4(17) ? 55504 . 65603
O(203) C(202) O(206) 70(3) ? 55504 . 65602
O(203) C(202) C(201) 84(2) ? 55504 . .
O(203) C(202) C(207) 110(3) ? 55504 . 65603
O(203) C(202) C(208) 127(2) ? 55504 . 65603
O(203) C(202) C(210) 72(2) ? 55504 . 65602
O(203) C(202) C(211) 84(2) ? 55504 . 65602
O(205) C(202) O(206) 43(2) ? 65603 . 65602
O(205) C(202) C(201) 131(2) ? 65603 . .
O(205) C(202) C(207) 110(3) ? 65603 . 65603
O(205) C(202) C(208) 63.3(19) ? 65603 . 65603
O(205) C(202) C(210) 43(2) ? 65603 . 65602
O(205) C(202) C(211) 136(2) ? 65603 . 65602
O(206) C(202) C(201) 91(3) ? 65602 . .
O(206) C(202) C(207) 68(3) ? 65602 . 65603
O(206) C(202) C(208) 64(3) ? 65602 . 65603
O(206) C(202) C(210) 87(2) ? 65602 . 65602
O(206) C(202) C(211) 98(3) ? 65602 . 65602
C(201) C(202) C(207) 45(2) ? . . 65603
C(201) C(202) C(208) 120(4) ? . . 65603
C(201) C(202) C(210) 155(2) ? . . 65602
C(201) C(202) C(211) 7.1(18) ? . . 65602
C(207) C(202) C(208) 75(4) ? 65603 . 65603
C(207) C(202) C(210) 151(4) ? 65603 . 65602
C(207) C(202) C(211) 51(2) ? 65603 . 65602
C(208) C(202) C(210) 81(3) ? 65603 . 65602
C(208) C(202) C(211) 125(4) ? 65603 . 65602
C(210) C(202) C(211) 153(3) ? 65602 . 65602
O(202) C(203) O(202) 96(3) ? . . 55504
O(202) C(203) O(205) 96(3) ? . . 65602
O(202) C(203) O(205) 44(2) ? . . 65603
O(202) C(203) C(204) 108(3) ? . . .
O(202) C(203) C(204) 39(2) ? . . 55504
O(202) C(203) C(209) 102(3) ? . . 65602
O(202) C(203) C(210) 43(2) ? . . 65602
O(202) C(203) C(210) 133(4) ? . . 65603
O(202) C(203) O(205) 44(2) ? 55504 . 65602
O(202) C(203) O(205) 96(3) ? 55504 . 65603
O(202) C(203) C(204) 39(2) ? 55504 . .
O(202) C(203) C(204) 108(3) ? 55504 . 55504
O(202) C(203) C(209) 102(3) ? 55504 . 65602
O(202) C(203) C(210) 133(4) ? 55504 . 65602
O(202) C(203) C(210) 43(2) ? 55504 . 65603
O(205) C(203) O(205) 67(2) ? 65602 . 65603
O(205) C(203) C(204) 81(3) ? 65602 . .
O(205) C(203) C(204) 131(4) ? 65602 . 55504
O(205) C(203) C(209) 59(3) ? 65602 . 65602
O(205) C(203) C(210) 108(4) ? 65602 . 65602
O(205) C(203) C(210) 42(2) ? 65602 . 65603
O(205) C(203) C(204) 131(4) ? 65603 . .
O(205) C(203) C(204) 81(3) ? 65603 . 55504
O(205) C(203) C(209) 59(3) ? 65603 . 65602
O(205) C(203) C(210) 42(2) ? 65603 . 65602
O(205) C(203) C(210) 108(4) ? 65603 . 65603
C(204) C(203) C(204) 94(3) ? . . 55504
C(204) C(203) C(209) 132(2) ? . . 65602
C(204) C(203) C(210) 149(4) ? . . 65602
C(204) C(203) C(210) 57(2) ? . . 65603
C(204) C(203) C(209) 132(2) ? 55504 . 65602
C(204) C(203) C(210) 57(2) ? 55504 . 65602
C(204) C(203) C(210) 149(4) ? 55504 . 65603
C(209) C(203) C(210) 75(3) ? 65602 . 65602
C(209) C(203) C(210) 75(3) ? 65602 . 65603
C(210) C(203) C(210) 147(5) ? 65602 . 65603
O(202) C(204) O(203) 20(2) ? 55504 . .
O(202) C(204) C(203) 85(4) ? 55504 . .
O(202) C(204) C(210) 56(3) ? 55504 . 65603
O(203) C(204) C(203) 105(4) ? . . .
O(203) C(204) C(210) 69(3) ? . . 65603
C(203) C(204) C(210) 63(3) ? . . 65603
O(203) C(205) C(201) 81(3) ? . . 55504
O(203) C(205) C(206) 110(4) ? . . .
O(203) C(205) C(211) 71(2) ? . . 65603
C(201) C(205) C(206) 54(2) ? 55504 . .
C(201) C(205) C(211) 15.0(13) ? 55504 . 65603
C(206) C(205) C(211) 69(3) ? . . 65603
O(201) C(206) O(204) 61(2) ? 65603 . .
O(201) C(206) C(201) 82(2) ? 65603 . 55504
O(201) C(206) C(205) 119(2) ? 65603 . .
O(201) C(206) C(211) 87(2) ? 65603 . 65603
O(201) C(206) C(212) 51(2) ? 65603 . 65603
O(201) C(206) C(212) 48.0(19) ? 65603 . 55504
O(204) C(206) C(201) 134(2) ? . . 55504
O(204) C(206) C(205) 110(2) ? . . .
O(204) C(206) C(211) 132.0(19) ? . . 65603
O(204) C(206) C(212) 111(4) ? . . 65603
O(204) C(206) C(212) 63(2) ? . . 55504
C(201) C(206) C(205) 64(2) ? 55504 . .
C(201) C(206) C(211) 9.7(12) ? 55504 . 65603
C(201) C(206) C(212) 49.1(19) ? 55504 . 65603
C(201) C(206) C(212) 113(3) ? 55504 . 55504
C(205) C(206) C(211) 54(2) ? . . 65603
C(205) C(206) C(212) 112(3) ? . . 65603
C(205) C(206) C(212) 167(2) ? . . 55504
C(211) C(206) C(212) 58.4(19) ? 65603 . 65603
C(211) C(206) C(212) 122(3) ? 65603 . 55504
C(212) C(206) C(212) 64(2) ? 65603 . 55504
O(204) C(207) O(206) 94(2) ? . . 55504
O(204) C(207) C(201) 103(3) ? . . 65603
O(204) C(207) C(202) 126.1(16) ? . . 65603
O(204) C(207) C(208) 111(2) ? . . .
O(204) C(207) C(211) 118(3) ? . . 55504
O(204) C(207) C(212) 64(2) ? . . 55504
O(206) C(207) C(201) 91(4) ? 55504 . 65603
O(206) C(207) C(202) 33(2) ? 55504 . 65603
O(206) C(207) C(208) 43.2(18) ? 55504 . .
O(206) C(207) C(211) 76(3) ? 55504 . 55504
O(206) C(207) C(212) 125(2) ? 55504 . 55504
C(201) C(207) C(202) 76(4) ? 65603 . 65603
C(201) C(207) C(208) 123(5) ? 65603 . .
C(201) C(207) C(211) 21(2) ? 65603 . 55504
C(201) C(207) C(212) 51.6(18) ? 65603 . 55504
C(202) C(207) C(208) 47(3) ? 65603 . .
C(202) C(207) C(211) 56(3) ? 65603 . 55504
C(202) C(207) C(212) 126(4) ? 65603 . 55504
C(208) C(207) C(211) 102(4) ? . . 55504
C(208) C(207) C(212) 168(3) ? . . 55504
C(211) C(207) C(212) 72(2) ? 55504 . 55504
O(205) C(208) O(206) 51.0(16) ? . . 55504
O(205) C(208) C(202) 73(2) ? . . 65603
O(205) C(208) C(207) 106(2) ? . . .
O(205) C(208) C(210) 41(2) ? . . 55504
O(206) C(208) C(202) 39(2) ? 55504 . 65603
O(206) C(208) C(207) 56(2) ? 55504 . .
O(206) C(208) C(210) 64(3) ? 55504 . 55504
C(202) C(208) C(207) 59(3) ? 65603 . .
C(202) C(208) C(210) 54(3) ? 65603 . 55504
C(207) C(208) C(210) 111(3) ? . . 55504
O(205) C(209) O(205) 77(2) ? . . 55504
O(205) C(209) C(203) 76(3) ? . . 65602
O(205) C(209) C(210) 109(2) ? . . .
O(205) C(209) C(210) 42(2) ? . . 55504
O(205) C(209) C(203) 76(3) ? 55504 . 65602
O(205) C(209) C(210) 42(2) ? 55504 . .
O(205) C(209) C(210) 109(2) ? 55504 . 55504
C(203) C(209) C(210) 59(2) ? 65602 . .
C(203) C(209) C(210) 59(2) ? 65602 . 55504
C(210) C(209) C(210) 117(3) ? . . 55504
O(202) C(210) O(203) 16.5(8) ? 65602 . 65603
O(202) C(210) O(205) 66(3) ? 65602 . 55504
O(202) C(210) O(206) 61(2) ? 65602 . .
O(202) C(210) C(202) 71(2) ? 65602 . 65602
O(202) C(210) C(203) 81(2) ? 65602 . 65602
O(202) C(210) C(204) 50(3) ? 65602 . 65603
O(202) C(210) C(208) 101(3) ? 65602 . 55504
O(202) C(210) C(209) 109(2) ? 65602 . .
O(203) C(210) O(205) 71(3) ? 65603 . 55504
O(203) C(210) O(206) 51(2) ? 65603 . .
O(203) C(210) C(202) 55.5(19) ? 65603 . 65602
O(203) C(210) C(203) 97(2) ? 65603 . 65602
O(203) C(210) C(204) 59(3) ? 65603 . 65603
O(203) C(210) C(208) 90(3) ? 65603 . 55504
O(203) C(210) C(209) 122(2) ? 65603 . .
O(205) C(210) O(206) 50(2) ? 55504 . .
O(205) C(210) C(202) 81(3) ? 55504 . 65602
O(205) C(210) C(203) 79(3) ? 55504 . 65602
O(205) C(210) C(204) 106(3) ? 55504 . 65603
O(205) C(210) C(208) 63(3) ? 55504 . 55504
O(205) C(210) C(209) 61(2) ? 55504 . .
O(206) C(210) C(202) 30(2) ? . . 65602
O(206) C(210) C(203) 124(3) ? . . 65602
O(206) C(210) C(204) 110(3) ? . . 65603
O(206) C(210) C(208) 39.7(19) ? . . 55504
O(206) C(210) C(209) 109(4) ? . . .
C(202) C(210) C(203) 150(3) ? 65602 . 65602
C(202) C(210) C(204) 107(3) ? 65602 . 65603
C(202) C(210) C(208) 45(2) ? 65602 . 55504
C(202) C(210) C(209) 135(5) ? 65602 . .
C(203) C(210) C(204) 60(2) ? 65602 . 65603
C(203) C(210) C(208) 136(4) ? 65602 . 55504
C(203) C(210) C(209) 46(2) ? 65602 . .
C(204) C(210) C(208) 149(3) ? 65603 . 55504
C(204) C(210) C(209) 106(2) ? 65603 . .
C(208) C(210) C(209) 94(3) ? 55504 . .
O(203) C(211) O(206) 47.9(19) ? 65603 . .
O(203) C(211) C(201) 121(3) ? 65603 . 65602
O(203) C(211) C(202) 52.8(19) ? 65603 . 65602
O(203) C(211) C(205) 54.7(18) ? 65603 . 65603
O(203) C(211) C(206) 91.7(19) ? 65603 . 65603
O(203) C(211) C(207) 103.1(18) ? 65603 . 55504
O(203) C(211) C(212) 122(2) ? 65603 . .
O(206) C(211) C(201) 122(5) ? . . 65602
O(206) C(211) C(202) 30(2) ? . . 65602
O(206) C(211) C(205) 102.5(16) ? . . 65603
O(206) C(211) C(206) 119.3(16) ? . . 65603
O(206) C(211) C(207) 57.4(18) ? . . 55504
O(206) C(211) C(212) 108(2) ? . . .
C(201) C(211) C(202) 152(6) ? 65602 . 65602
C(201) C(211) C(205) 92(5) ? 65602 . 65603
C(201) C(211) C(206) 36(4) ? 65602 . 65603
C(201) C(211) C(207) 83(6) ? 65602 . 55504
C(201) C(211) C(212) 18(4) ? 65602 . .
C(202) C(211) C(205) 101(2) ? 65602 . 65603
C(202) C(211) C(206) 142.9(14) ? 65602 . 65603
C(202) C(211) C(207) 73(3) ? 65602 . 55504
C(202) C(211) C(212) 135(3) ? 65602 . .
C(205) C(211) C(206) 57(3) ? 65603 . 65603
C(205) C(211) C(207) 150(2) ? 65603 . 55504
C(205) C(211) C(212) 107(2) ? 65603 . .
C(206) C(211) C(207) 111(3) ? 65603 . 55504
C(206) C(211) C(212) 51(2) ? 65603 . .
C(207) C(211) C(212) 65(2) ? 55504 . .
O(201) C(212) O(204) 60.7(12) ? . . 55504
O(201) C(212) C(201) 99.7(9) ? . . 65602
O(201) C(212) C(206) 61.3(17) ? . . 65603
O(201) C(212) C(206) 56.4(13) ? . . 55504
O(201) C(212) C(207) 103.1(7) ? . . 55504
O(201) C(212) C(211) 100.3(8) ? . . .
O(201) C(212) C(212) 48.5(3) ? . . 65602
O(204) C(212) C(201) 96.8(18) ? 55504 . 65602
O(204) C(212) C(206) 114.1(15) ? 55504 . 65603
O(204) C(212) C(206) 56.5(19) ? 55504 . 55504
O(204) C(212) C(207) 59(2) ? 55504 . 55504
O(204) C(212) C(211) 91.7(18) ? 55504 . .
O(204) C(212) C(212) 98.1(15) ? 55504 . 65602
C(201) C(212) C(206) 65(2) ? 65602 . 65603
C(201) C(212) C(206) 149.6(7) ? 65602 . 55504
C(201) C(212) C(207) 49(2) ? 65602 . 55504
C(201) C(212) C(211) 6.2(13) ? 65602 . .
C(201) C(212) C(212) 127.4(14) ? 65602 . 65602
C(206) C(212) C(206) 110(2) ? 65603 . 55504
C(206) C(212) C(207) 109(2) ? 65603 . 55504
C(206) C(212) C(211) 71(2) ? 65603 . .
C(206) C(212) C(212) 62(2) ? 65603 . 65602
C(206) C(212) C(207) 114(2) ? 55504 . 55504
C(206) C(212) C(211) 146.2(8) ? 55504 . .
C(206) C(212) C(212) 53.3(17) ? 55504 . 65602
C(207) C(212) C(211) 43(2) ? 55504 . .
C(207) C(212) C(212) 151.6(8) ? 55504 . 65602
C(211) C(212) C(212) 132.0(13) ? . . 65602
O(301) C(301) O(304) 59(2) ? . . 55504
O(301) C(301) C(302) 110(3) ? . . .
O(301) C(301) C(306) 105(3) ? . . 55504
O(301) C(301) C(307) 33.0(14) ? . . 55504
O(304) C(301) C(302) 62(4) ? 55504 . .
O(304) C(301) C(306) 57(4) ? 55504 . 55504
O(304) C(301) C(307) 90(3) ? 55504 . 55504
C(302) C(301) C(306) 5.2(13) ? . . 55504
C(302) C(301) C(307) 125(6) ? . . 55504
C(306) C(301) C(307) 121(6) ? 55504 . 55504
O(302) C(302) O(304) 71(2) ? . . 55504
O(302) C(302) C(301) 107(4) ? . . .
O(302) C(302) C(305) 34.9(19) ? . . 55504
O(302) C(302) C(306) 56(13) ? . . 55504
O(304) C(302) C(301) 41(2) ? 55504 . .
O(304) C(302) C(305) 105(2) ? 55504 . 55504
O(304) C(302) C(306) 104(14) ? 55504 . 55504
C(301) C(302) C(305) 135(4) ? . . 55504
C(301) C(302) C(306) 141(15) ? . . 55504
C(305) C(302) C(306) 52(12) ? 55504 . 55504
O(302) C(303) O(303) 63(2) ? . . 55504
O(302) C(303) C(304) 111(2) ? . . .
O(302) C(303) C(305) 39(2) ? . . 55504
O(303) C(303) C(304) 62.8(17) ? 55504 . .
O(303) C(303) C(305) 102(4) ? 55504 . 55504
C(304) C(303) C(305) 132(4) ? . . 55504
O(303) C(304) O(303) 72.9(16) ? . . 55504
O(303) C(304) C(303) 106.3(19) ? . . .
O(303) C(304) C(303) 35.8(14) ? . . 55504
O(303) C(304) C(303) 35.8(14) ? 55504 . .
O(303) C(304) C(303) 106.3(19) ? 55504 . 55504
C(303) C(304) C(303) 134(2) ? . . 55504
O(302) C(305) O(303) 63.3(18) ? 55504 . .
O(302) C(305) C(302) 62(2) ? 55504 . 55504
O(302) C(305) C(303) 101(2) ? 55504 . 55504
O(302) C(305) C(306) 61(2) ? 55504 . .
O(303) C(305) C(302) 113(2) ? . . 55504
O(303) C(305) C(303) 38(2) ? . . 55504
O(303) C(305) C(306) 107(2) ? . . .
C(302) C(305) C(303) 135(3) ? 55504 . 55504
C(302) C(305) C(306) 7(2) ? 55504 . .
C(303) C(305) C(306) 128(4) ? 55504 . .
O(302) C(306) O(304) 72(3) ? 55504 . .
O(302) C(306) C(301) 102(4) ? 55504 . 55504
O(302) C(306) C(302) 115(17) ? 55504 . 55504
O(302) C(306) C(305) 38(2) ? 55504 . .
O(304) C(306) C(301) 35.9(16) ? . . 55504
O(304) C(306) C(302) 67(16) ? . . 55504
O(304) C(306) C(305) 109(3) ? . . .
C(301) C(306) C(302) 33(14) ? 55504 . 55504
C(301) C(306) C(305) 130(4) ? 55504 . .
C(302) C(306) C(305) 120(14) ? 55504 . .
O(301) C(307) O(304) 62(3) ? 55504 . .
O(301) C(307) C(301) 104(4) ? 55504 . 55504
O(301) C(307) C(308) 61(5) ? 55504 . .
O(301) C(307) C(312) 64(5) ? 55504 . 55504
O(304) C(307) C(301) 44.1(19) ? . . 55504
O(304) C(307) C(308) 112(3) ? . . .
O(304) C(307) C(312) 118(3) ? . . 55504
C(301) C(307) C(308) 128(6) ? 55504 . .
C(301) C(307) C(312) 135(6) ? 55504 . 55504
C(308) C(307) C(312) 7(2) ? . . 55504
O(301) C(308) O(305) 79(2) ? 55504 . .
O(301) C(308) C(307) 32.7(17) ? 55504 . .
O(301) C(308) C(311) 107(3) ? 55504 . 55504
O(301) C(308) C(312) 120(24) ? 55504 . 55504
O(305) C(308) C(307) 109(4) ? . . .
O(305) C(308) C(311) 34.8(17) ? . . 55504
O(305) C(308) C(312) 79(7) ? . . 55504
C(307) C(308) C(311) 128(4) ? . . 55504
C(307) C(308) C(312) 113(21) ? . . 55504
C(311) C(308) C(312) 47(6) ? 55504 . 55504
O(305) C(309) O(306) 55(2) ? . . 55504
O(305) C(309) C(310) 110(2) ? . . .
O(305) C(309) C(311) 39(2) ? . . 55504
O(306) C(309) C(310) 69(2) ? 55504 . .
O(306) C(309) C(311) 92(4) ? 55504 . 55504
C(310) C(309) C(311) 122(3) ? . . 55504
O(306) C(310) O(306) 80.3(17) ? . . 55504
O(306) C(310) C(309) 107(2) ? . . .
O(306) C(310) C(309) 31.0(16) ? . . 55504
O(306) C(310) C(309) 31.0(16) ? 55504 . .
O(306) C(310) C(309) 107(2) ? 55504 . 55504
C(309) C(310) C(309) 127(2) ? . . 55504
O(305) C(311) O(306) 55(2) ? 55504 . .
O(305) C(311) C(308) 61(2) ? 55504 . 55504
O(305) C(311) C(309) 86(2) ? 55504 . 55504
O(305) C(311) C(312) 66(2) ? 55504 . .
O(306) C(311) C(308) 103(2) ? . . 55504
O(306) C(311) C(309) 32.5(19) ? . . 55504
O(306) C(311) C(312) 109(2) ? . . .
C(308) C(311) C(309) 117(3) ? 55504 . 55504
C(308) C(311) C(312) 6.2(15) ? 55504 . .
C(309) C(311) C(312) 121(3) ? 55504 . .
O(301) C(312) O(305) 76(2) ? . . 55504
O(301) C(312) C(307) 30.5(14) ? . . 55504
O(301) C(312) C(308) 52(22) ? . . 55504
O(301) C(312) C(311) 108(3) ? . . .
O(305) C(312) C(307) 105(3) ? 55504 . 55504
O(305) C(312) C(308) 92(6) ? 55504 . 55504
O(305) C(312) C(311) 37.6(18) ? 55504 . .
C(307) C(312) C(308) 60(20) ? 55504 . 55504
C(307) C(312) C(311) 131(4) ? 55504 . .
C(308) C(312) C(311) 127(6) ? 55504 . .
O(401) C(401) C(402) 108(4) ? . . .
O(402) C(402) C(401) 111(4) ? . . .
O(402) C(402) C(408) 111(4) ? . . 65502
C(401) C(402) C(408) 102(6) ? . . 65502
O(402) C(403) C(404) 107(5) ? . . .
O(402) C(403) C(409) 82(8) ? . . 65502
O(402) C(403) C(410) 114(6) ? . . 65502
C(404) C(403) C(409) 137(8) ? . . 65502
C(404) C(403) C(410) 43(4) ? . . 65502
C(409) C(403) C(410) 94(8) ? 65502 . 65502
O(403) C(404) O(406) 29(3) ? . . 65502
O(403) C(404) C(403) 110(5) ? . . .
O(403) C(404) C(410) 69(6) ? . . 65502
O(406) C(404) C(403) 95(5) ? 65502 . .
O(406) C(404) C(410) 77(6) ? 65502 . 65502
C(403) C(404) C(410) 55(5) ? . . 65502
O(403) C(405) C(412) 95(4) ? . . 65502
O(403) C(405) C(411) 36(8) ? . . 65502
O(403) C(405) C(406) 108(5) ? . . .
C(412) C(405) C(411) 61(10) ? 65502 . 65502
C(412) C(405) C(406) 83(5) ? 65502 . .
C(411) C(405) C(406) 112(11) ? 65502 . .
O(404) C(406) C(411) 95(4) ? . . 65502
O(404) C(406) C(405) 110(5) ? . . .
C(411) C(406) C(405) 17(3) ? 65502 . .
O(404) C(407) C(408) 108(4) ? . . .
O(405) C(408) C(402) 74(3) ? . . 65502
O(405) C(408) C(407) 110(4) ? . . .
C(402) C(408) C(407) 123(5) ? 65502 . .
O(402) C(409) O(405) 71(4) ? 65502 . .
O(402) C(409) C(403) 69(7) ? 65502 . 65502
O(402) C(409) C(410) 96(4) ? 65502 . .
O(405) C(409) C(403) 134(9) ? . . 65502
O(405) C(409) C(410) 109(5) ? . . .
C(403) C(409) C(410) 55(6) ? 65502 . .
O(403) C(410) O(406) 28(3) ? 65502 . .
O(403) C(410) C(403) 127(6) ? 65502 . 65502
O(403) C(410) C(404) 69(6) ? 65502 . 65502
O(403) C(410) C(409) 134(6) ? 65502 . .
O(406) C(410) C(403) 99(6) ? . . 65502
O(406) C(410) C(404) 58(6) ? . . 65502
O(406) C(410) C(409) 111(5) ? . . .
C(403) C(410) C(404) 82(6) ? 65502 . 65502
C(403) C(410) C(409) 30(4) ? 65502 . .
C(404) C(410) C(409) 112(7) ? 65502 . .
O(504) C(506) C(505) 108.6 ? . . .
O(503) C(505) C(506) 109.0 ? . . .
O(503) C(504) C(503) 111.8 ? . . .
O(502) C(503) C(504) 109.0 ? . . .
O(502) C(502) C(502) 110.2 ? . . 55504
O(502) C(502) C(501) 109.9 ? . . .
C(502) C(502) C(501) 58.3 ? 55504 . .
O(501) C(501) O(501) 76.7 ? . . 55504
O(501) C(501) C(502) 108.8 ? . . .
O(501) C(501) C(502) 167.2 ? . . 55504
O(501) C(501) C(502) 167.2 ? 55504 . .
O(501) C(501) C(502) 108.8 ? 55504 . 55504
C(502) C(501) C(502) 63.4 ? . . 55504
O(501) C(512) O(501) 68.7 ? . . 55504
O(501) C(512) C(511) 99.5 ? . . .
O(501) C(512) C(511) 165.7 ? . . 55504
O(501) C(512) C(511) 165.7 ? 55504 . .
O(501) C(512) C(511) 99.5 ? 55504 . 55504
C(511) C(512) C(511) 90.8 ? . . 55504
O(506) C(511) C(512) 109.8 ? . . .
O(506) C(510) C(509) 110.5 ? . . .
O(505) C(509) C(510) 106.8 ? . . .
O(505) C(508) C(507) 110.5 ? . . .
O(504) C(507) C(508) 108.6 ? . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
W(1) O(3) 1.888(13) ? . .
W(1) O(5) 1.932(16) ? . .
W(1) O(7) 1.880(17) ? . .
W(1) O(8) 1.917(13) ? . .
W(1) O(15) 2.303(14) ? . .
W(1) O(102) 1.687(18) ? . .
W(2) O(4) 1.884(13) ? . .
W(2) O(6) 1.925(16) ? . .
W(2) O(7) 1.931(17) ? . .
W(2) O(9) 1.932(13) ? . .
W(2) O(15) 2.333(14) ? . .
W(2) O(103) 1.693(18) ? . .
W(3) O(5) 1.909(15) ? . .
W(3) O(5) 1.909(15) ? . 56504
W(3) O(10) 1.935(15) ? . .
W(3) O(10) 1.935(15) ? . 56504
W(3) O(16) 2.33(2) ? . .
W(3) O(104) 1.68(3) ? . .
W(4) O(6) 1.917(15) ? . .
W(4) O(6) 1.917(15) ? . 56504
W(4) O(11) 1.945(15) ? . .
W(4) O(11) 1.945(15) ? . 56504
W(4) O(17) 2.34(2) ? . .
W(4) O(105) 1.72(2) ? . .
W(5) O(8) 1.899(13) ? . .
W(5) O(10) 1.903(17) ? . .
W(5) O(12) 1.915(8) ? . .
W(5) O(14) 1.877(15) ? . .
W(5) O(16) 2.348(12) ? . .
W(5) O(106) 1.699(15) ? . .
W(6) O(9) 1.893(13) ? . .
W(6) O(11) 1.891(15) ? . .
W(6) O(13) 1.917(9) ? . .
W(6) O(14) 1.914(14) ? . .
W(6) O(17) 2.365(13) ? . .
W(6) O(107) 1.699(15) ? . .
Ti(1) O(1) 2.009(17) ? . .
Ti(1) O(2) 2.01(2) ? . .
Ti(1) O(3) 1.866(16) ? . .
Ti(1) O(4) 1.871(17) ? . .
Ti(1) O(15) 2.415(12) ? . .
Ti(1) O(101) 1.803(5) ? . .
K(1) O(201) 2.822(6) ? . .
K(1) O(201) 2.822(6) ? . 65603
K(1) O(202) 2.91(3) ? . .
K(1) O(202) 2.91(3) ? . 65602
K(1) O(202) 2.91(3) ? . 65603
K(1) O(202) 2.91(3) ? . 55504
K(1) O(203) 2.81(4) ? . .
K(1) O(203) 2.81(4) ? . 65602
K(1) O(203) 2.81(4) ? . 65603
K(1) O(203) 2.81(4) ? . 55504
K(1) O(204) 2.84(2) ? . .
K(1) O(204) 2.844(19) ? . 65602
K(1) O(204) 2.844(19) ? . 65603
K(1) O(204) 2.84(2) ? . 55504
K(1) O(205) 2.86(3) ? . .
K(1) O(205) 2.86(3) ? . 65602
K(1) O(205) 2.86(3) ? . 65603
K(1) O(205) 2.86(3) ? . 55504
K(1) O(206) 2.997(17) ? . .
K(1) O(206) 2.997(17) ? . 65602
K(1) O(206) 2.997(17) ? . 65603
K(1) O(206) 2.997(17) ? . 55504
K(2) O(301) 2.856(9) ? . .
K(2) O(301) 2.856(9) ? . 55504
K(2) O(302) 2.88(2) ? . .
K(2) O(302) 2.88(2) ? . 55504
K(2) O(303) 2.86(3) ? . .
K(2) O(303) 2.86(3) ? . 55504
K(2) O(304) 2.807(10) ? . .
K(2) O(304) 2.807(10) ? . 55504
K(2) O(305) 2.76(2) ? . .
K(2) O(305) 2.76(2) ? . 55504
K(2) O(306) 2.87(3) ? . .
K(2) O(306) 2.87(3) ? . 55504
K(3) O(401) 2.84(5) ? . .
K(3) O(401) 2.84(5) ? . 65502
K(3) O(402) 3.08(5) ? . .
K(3) O(402) 3.08(5) ? . 65502
K(3) O(403) 3.02(6) ? . .
K(3) O(403) 3.02(6) ? . 65502
K(3) O(404) 3.03(5) ? . .
K(3) O(404) 3.03(5) ? . 65502
K(3) O(405) 2.75(5) ? . .
K(3) O(405) 2.75(5) ? . 65502
K(3) O(406) 2.86(6) ? . .
K(3) O(406) 2.86(6) ? . 65502
K(4) O(504) 3.104 ? . .
K(4) O(503) 2.762 ? . .
K(4) O(502) 2.798 ? . .
K(4) O(501) 2.811 ? . .
K(4) O(506) 3.108 ? . .
K(4) O(505) 3.072 ? . .
Si(1) O(15) 1.631(13) ? . .
Si(1) O(15) 1.631(13) ? . 56504
Si(1) O(16) 1.63(2) ? . .
Si(1) O(17) 1.62(2) ? . .
O(1) C(1) 1.51(8) ? . .
O(2) C(2) 1.41(10) ? . .
O(201) O(204) 1.40(3) ? . 65603
O(201) O(204) 1.40(3) ? . 55504
O(201) C(201) 1.76(2) ? . .
O(201) C(201) 1.76(2) ? . 65602
O(201) C(206) 1.30(5) ? . 65603
O(201) C(206) 1.30(5) ? . 55504
O(201) C(212) 1.160(6) ? . .
O(201) C(212) 1.160(6) ? . 65602
O(202) O(203) 0.57(4) ? . 55504
O(202) O(205) 1.19(5) ? . 65603
O(202) O(206) 1.34(4) ? . 65602
O(202) C(202) 1.41(2) ? . .
O(202) C(203) 1.62(4) ? . .
O(202) C(204) 1.03(7) ? . 55504
O(202) C(210) 1.12(5) ? . 65602
O(203) O(205) 1.56(5) ? . 65602
O(203) O(206) 1.28(5) ? . 65603
O(203) C(202) 1.34(4) ? . 55504
O(203) C(204) 1.42(7) ? . .
O(203) C(205) 1.45(4) ? . .
O(203) C(210) 1.55(5) ? . 65603
O(203) C(211) 1.68(2) ? . 65603
O(204) C(206) 1.44(4) ? . .
O(204) C(207) 1.46(6) ? . .
O(204) C(212) 1.54(3) ? . 55504
O(205) O(205) 1.724(3) ? . 55504
O(205) O(206) 1.125(16) ? . 55504
O(205) C(202) 1.536(17) ? . 65603
O(205) C(203) 1.56(7) ? . 65602
O(205) C(208) 1.44(3) ? . .
O(205) C(209) 1.39(4) ? . .
O(205) C(210) 1.07(7) ? . 55504
O(206) C(201) 1.680(14) ? . 65602
O(206) C(202) 0.73(4) ? . 65602
O(206) C(207) 1.25(3) ? . 55504
O(206) C(208) 1.03(3) ? . 55504
O(206) C(210) 1.45(5) ? . .
O(206) C(211) 1.438(19) ? . .
O(301) O(304) 1.28(5) ? . 55504
O(301) C(301) 1.47(4) ? . .
O(301) C(307) 0.823(16) ? . 55504
O(301) C(308) 1.33(7) ? . 55504
O(301) C(312) 1.46(7) ? . .
O(302) O(303) 1.34(3) ? . 55504
O(302) O(304) 1.64(5) ? . 55504
O(302) C(302) 1.46(2) ? . .
O(302) C(303) 1.47(5) ? . .
O(302) C(305) 0.95(5) ? . 55504
O(302) C(306) 1.34(3) ? . 55504
O(303) O(303) 1.661(14) ? . 55504
O(303) C(303) 0.92(3) ? . 55504
O(303) C(304) 1.40(3) ? . .
O(303) C(305) 1.461(17) ? . .
O(304) C(301) 1.00(2) ? . 55504
O(304) C(302) 1.36(7) ? . 55504
O(304) C(306) 1.44(7) ? . .
O(304) C(307) 1.44(4) ? . .
O(305) O(306) 1.21(3) ? . 55504
O(305) C(308) 1.43(2) ? . .
O(305) C(309) 1.48(5) ? . .
O(305) C(311) 0.94(4) ? . 55504
O(305) C(312) 1.41(2) ? . 55504
O(306) C(309) 0.79(3) ? . 55504
O(306) C(310) 1.43(2) ? . .
O(306) C(311) 1.47(2) ? . .
O(401) O(404) 1.19(7) ? . 65502
O(401) C(412) 1.45(9) ? . .
O(401) C(401) 1.43(8) ? . .
O(402) O(405) 1.73(7) ? . 65502
O(402) C(402) 1.45(8) ? . .
O(402) C(403) 1.45(10) ? . .
O(402) C(409) 1.54(9) ? . 65502
O(403) O(406) 0.69(8) ? . 65502
O(403) C(411) 1.02(9) ? . 65502
O(403) C(404) 1.44(10) ? . .
O(403) C(405) 1.43(9) ? . .
O(403) C(410) 1.44(10) ? . 65502
O(404) C(406) 1.45(9) ? . .
O(404) C(407) 1.40(8) ? . .
O(405) C(408) 1.45(8) ? . .
O(405) C(409) 1.42(10) ? . .
O(406) C(411) 1.41(9) ? . .
O(406) C(404) 1.24(10) ? . 65502
O(406) C(410) 1.42(9) ? . .
O(504) C(506) 1.424 ? . .
O(504) C(507) 1.420 ? . .
O(503) C(505) 1.390 ? . .
O(503) C(504) 1.414 ? . .
O(502) C(503) 1.393 ? . .
O(502) C(502) 1.430 ? . .
O(501) O(501) 1.723 ? . 55504
O(501) C(501) 1.389 ? . .
O(501) C(512) 1.526 ? . .
O(506) C(511) 1.413 ? . .
O(506) C(510) 1.434 ? . .
O(505) C(509) 1.422 ? . .
O(505) C(508) 1.427 ? . .
C(412) C(411) 1.48(10) ? . .
C(412) C(405) 1.67(9) ? . 65502
C(411) C(405) 0.58(9) ? . 65502
C(411) C(406) 1.77(9) ? . 65502
C(201) C(202) 1.50(2) ? . .
C(201) C(205) 1.51(5) ? . 55504
C(201) C(206) 1.37(4) ? . 55504
C(201) C(207) 1.09(5) ? . 65603
C(201) C(211) 0.39(3) ? . 65602
C(201) C(212) 1.14(2) ? . 65602
C(202) C(207) 1.32(6) ? . 65603
C(202) C(208) 1.12(6) ? . 65603
C(202) C(210) 1.29(3) ? . 65602
C(202) C(211) 1.15(2) ? . 65602
C(203) C(204) 1.34(5) ? . .
C(203) C(204) 1.34(5) ? . 55504
C(203) C(209) 1.15(7) ? . 65602
C(203) C(210) 1.37(2) ? . 65602
C(203) C(210) 1.37(2) ? . 65603
C(204) C(210) 1.29(7) ? . 65603
C(205) C(206) 1.49(7) ? . .
C(205) C(211) 1.44(5) ? . 65603
C(206) C(211) 1.66(4) ? . 65603
C(206) C(212) 1.37(5) ? . 65603
C(206) C(212) 1.51(5) ? . 55504
C(207) C(208) 1.49(3) ? . .
C(207) C(211) 1.07(6) ? . 55504
C(207) C(212) 1.43(3) ? . 55504
C(208) C(210) 1.57(7) ? . 55504
C(209) C(210) 1.54(3) ? . .
C(209) C(210) 1.54(3) ? . 55504
C(211) C(212) 1.50(3) ? . .
C(212) C(212) 1.538(9) ? . 65602
C(301) C(302) 1.51(8) ? . .
C(301) C(306) 1.71(8) ? . 55504
C(301) C(307) 1.03(6) ? . 55504
C(302) C(305) 1.65(4) ? . 55504
C(302) C(306) 0.25(6) ? . 55504
C(303) C(304) 1.555(18) ? . .
C(303) C(305) 0.96(3) ? . 55504
C(305) C(306) 1.51(4) ? . .
C(307) C(308) 1.52(8) ? . .
C(307) C(312) 1.62(8) ? . 55504
C(308) C(311) 1.63(4) ? . 55504
C(308) C(312) 0.22(5) ? . 55504
C(309) C(310) 1.51(2) ? . .
C(309) C(311) 1.21(4) ? . 55504
C(311) C(312) 1.49(4) ? . .
C(401) C(402) 1.47(11) ? . .
C(402) C(408) 1.62(7) ? . 65502
C(403) C(404) 1.48(9) ? . .
C(403) C(409) 0.76(9) ? . 65502
C(403) C(410) 1.23(9) ? . 65502
C(404) C(410) 1.02(9) ? . 65502
C(405) C(406) 1.47(10) ? . .
C(407) C(408) 1.50(11) ? . .
C(409) C(410) 1.49(9) ? . .
C(506) C(505) 1.472 ? . .
C(504) C(503) 1.471 ? . .
C(502) C(502) 1.545 ? . 55504
C(502) C(501) 1.470 ? . .
C(512) C(511) 1.584 ? . .
C(512) C(511) 1.584 ? . 55504
C(510) C(509) 1.458 ? . .
C(508) C(507) 1.446 ? . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
O(1) O(101) 2.91(2) ? . 66603
O(2) O(101) 2.92(2) ? . 66603
O(3) C(212) 3.404(16) ? . 65602
O(3) C(404) 3.22(7) ? . 65502
O(3) C(410) 3.50(7) ? . .
O(4) C(411) 3.53(6) ? . 65602
O(4) C(201) 3.156(16) ? . .
O(4) C(207) 3.46(2) ? . 65603
O(4) C(211) 3.225(17) ? . 65602
O(4) C(212) 3.307(16) ? . 65602
O(4) C(405) 3.08(6) ? . 55601
O(5) C(403) 3.22(7) ? . 65502
O(5) C(404) 3.54(7) ? . 65502
O(6) C(412) 3.39(6) ? . 65602
O(7) C(202) 3.59(2) ? . .
O(7) C(207) 3.07(2) ? . 65603
O(7) C(208) 3.24(2) ? . 65603
O(7) C(211) 3.56(2) ? . 65602
O(7) C(311) 3.32(2) ? . .
O(7) C(312) 3.42(3) ? . .
O(8) C(308) 3.29(2) ? . 55504
O(8) C(312) 3.18(2) ? . .
O(9) C(307) 3.41(3) ? . 55504
O(12) C(304) 3.28(3) ? . 55606
O(13) C(304) 3.02(3) ? . 55606
O(14) C(303) 3.52(3) ? . 55607
O(14) C(304) 3.43(2) ? . 55606
O(101) C(212) 3.420(19) ? . .
O(101) C(212) 3.420(19) ? . 65602
O(102) C(311) 3.47(3) ? . .
O(102) C(403) 3.41(7) ? . 65502
O(102) C(409) 3.35(7) ? . .
O(102) C(410) 3.38(7) ? . .
O(103) C(201) 3.56(2) ? . .
O(103) C(202) 3.21(3) ? . .
O(103) C(208) 3.52(4) ? . 65603
O(103) C(211) 3.32(2) ? . 65602
O(103) C(405) 3.54(7) ? . 55601
O(103) C(406) 2.93(7) ? . 55601
O(104) C(402) 3.52(7) ? . 65502
O(104) C(402) 3.52(7) ? . 66503
O(104) C(403) 3.55(6) ? . 65502
O(104) C(403) 3.55(6) ? . 66503
O(105) C(401) 3.07(6) ? . 65602
O(105) C(401) 3.07(6) ? . 66603
O(106) C(508) 2.993 ? . 45508
O(107) C(301) 3.23(4) ? . .
O(107) C(302) 3.18(2) ? . .
O(107) C(305) 3.44(4) ? . 55606
O(107) C(306) 3.31(2) ? . 55504
O(107) C(307) 3.45(5) ? . 55504
O(107) C(506) 2.826 ? . 65602
O(505) C(510) 3.204 ? . 65507
C(1) O(101) 3.57(6) ? . 66603
C(1) C(412) 3.18(8) ? . 65602
C(1) C(412) 3.18(9) ? . 66603
C(1) C(411) 3.48(7) ? . 65602
C(1) C(411) 3.48(7) ? . 66603
C(1) C(405) 3.51(7) ? . 55601
C(1) C(405) 3.51(7) ? . 56604
C(2) O(101) 3.42(7) ? . 66603
C(2) C(404) 3.07(9) ? . 65502
C(2) C(404) 3.07(9) ? . 66503
C(412) O(6) 3.39(6) ? . 65602
C(412) C(1) 3.18(9) ? . 65602
C(411) O(4) 3.53(6) ? . 65602
C(411) C(1) 3.48(7) ? . 65602
C(201) O(4) 3.156(16) ? . .
C(201) O(103) 3.56(2) ? . .
C(202) O(7) 3.59(2) ? . .
C(202) O(103) 3.21(3) ? . .
C(205) C(405) 3.57(7) ? . 55604
C(205) C(406) 3.56(8) ? . 55604
C(207) O(4) 3.46(2) ? . 65603
C(207) O(7) 3.07(2) ? . 65603
C(208) O(7) 3.24(2) ? . 65603
C(208) O(103) 3.52(4) ? . 65603
C(208) C(310) 3.58(4) ? . 65602
C(208) C(311) 3.16(5) ? . 65603
C(209) C(310) 3.34(6) ? . 65602
C(211) O(4) 3.225(17) ? . 65602
C(211) O(7) 3.56(2) ? . 65602
C(211) O(103) 3.32(2) ? . 65602
C(212) O(3) 3.404(16) ? . 65602
C(212) O(4) 3.307(16) ? . 65602
C(212) O(101) 3.420(19) ? . .
C(301) O(107) 3.23(4) ? . .
C(302) O(107) 3.18(2) ? . .
C(303) O(14) 3.52(3) ? . 55607
C(304) O(12) 3.28(3) ? . 54606
C(304) O(13) 3.02(3) ? . 54606
C(304) O(14) 3.43(2) ? . 54606
C(304) O(14) 3.43(2) ? . 55607
C(305) O(107) 3.44(4) ? . 54606
C(306) O(107) 3.31(2) ? . 55504
C(306) C(506) 3.551 ? . 65603
C(307) O(9) 3.41(3) ? . 55504
C(307) O(107) 3.45(5) ? . 55504
C(308) O(8) 3.29(2) ? . 55504
C(310) C(208) 3.58(4) ? . 65602
C(310) C(208) 3.58(4) ? . 65603
C(310) C(209) 3.34(6) ? . 65602
C(311) O(7) 3.32(2) ? . .
C(311) O(102) 3.47(3) ? . .
C(311) C(208) 3.16(5) ? . 65603
C(312) O(7) 3.42(3) ? . .
C(312) O(8) 3.18(2) ? . .
C(401) O(105) 3.07(6) ? . 65602
C(401) C(401) 3.24(7) ? . 56504
C(402) O(104) 3.52(7) ? . 65502
C(403) O(5) 3.22(7) ? . 65502
C(403) O(102) 3.41(7) ? . 65502
C(403) O(104) 3.55(6) ? . 65502
C(404) O(3) 3.22(7) ? . 65502
C(404) O(5) 3.54(7) ? . 65502
C(404) C(2) 3.07(9) ? . 65502
C(405) O(4) 3.08(6) ? . 55401
C(405) O(103) 3.54(7) ? . 55401
C(405) C(1) 3.51(7) ? . 55401
C(405) C(205) 3.57(7) ? . 55404
C(406) O(103) 2.93(7) ? . 55401
C(406) C(205) 3.56(8) ? . 55404
C(407) C(504) 3.145 ? . 65502
C(407) C(503) 3.065 ? . 65502
C(408) C(503) 3.584 ? . 65502
C(409) O(102) 3.35(7) ? . .
C(410) O(3) 3.50(7) ? . .
C(410) O(102) 3.38(7) ? . .
C(506) O(107) 2.826 ? . 65602
C(506) C(306) 3.551 ? . 65603
C(504) C(407) 3.145 ? . 65502
C(503) C(407) 3.065 ? . 65502
C(503) C(408) 3.584 ? . 65502
C(510) O(505) 3.204 ? . 65507
C(508) O(106) 2.993 ? . 55508
|
1101222.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/12/1101222.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_1101222
loop_
_publ_author_name
'Lionel Beitone'
'Clarisse Huguenard'
'Axel Gansm\"uller'
'Marc Henry'
'Francis Taulelle'
'Thierry Loiseau'
'G\'erard F\'erey'
_publ_section_title
;
Order-Disorder in the Super-Sodalite Zn3Al6(PO4)12, 4tren, 17H2O
(MIL-74): A Combined XRD-NMR Assessment
;
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 9102
_journal_page_last 9110
_journal_paper_doi 10.1021/ja0294818
_journal_volume 125
_journal_year 2003
_chemical_formula_sum 'C24 H118 Al6 N16 O65 P12 Zn3'
_chemical_formula_weight 2400.97
_chemical_name_common MIL-74
_space_group_IT_number 218
_space_group_name_Hall 'P -4n 2 3'
_space_group_name_H-M_alt 'P -4 3 n'
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall 'P -4n 2 3'
_symmetry_space_group_name_H-M 'P -4 3 n'
_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 2
_cell_length_a 16.79420(10)
_cell_length_b 16.79420(10)
_cell_length_c 16.79420(10)
_cell_measurement_temperature 293(2)
_cell_volume 4736.72(5)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens SHELXTL'
_computing_molecular_graphics 'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'Siemens SHELXTL'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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 0.0334
_diffrn_reflns_av_sigmaI/netI 0.0160
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 29988
_diffrn_reflns_theta_full 29.75
_diffrn_reflns_theta_max 29.75
_diffrn_reflns_theta_min 1.71
_exptl_absorpt_coefficient_mu 1.125
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.683
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rhombododecahedron
_exptl_crystal_F_000 2484
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.24
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.614
_refine_diff_density_min -0.368
_refine_diff_density_rms 0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.01(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.176
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 105
_refine_ls_number_reflns 2198
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.176
_refine_ls_R_factor_all 0.0532
_refine_ls_R_factor_gt 0.0404
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+2.5681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1014
_refine_ls_wR_factor_ref 0.1091
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_reflns_number_gt 1686
_reflns_number_total 2198
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
Adding additional data items after consulting the original supplementary
material.
Antanas Vaitkus,
2018-11-16
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1101222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'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, 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'
'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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.0000 0.5000 0.0000 0.0143(3) Uani 1 4 d S . .
Al2 Al 0.2500 0.5000 0.0000 0.0188(3) Uiso 0.626(5) 4 d SP . .
Zn2 Zn 0.2500 0.5000 0.0000 0.0188(3) Uiso 0.374(5) 4 d SP . .
Al3 Al 0.0000 0.5000 0.2500 0.0118(2) Uiso 0.542(5) 4 d SP . .
Zn3 Zn 0.0000 0.5000 0.2500 0.0118(2) Uiso 0.458(5) 4 d SP . .
P P 0.12289(4) 0.43554(4) 0.12217(4) 0.01811(16) Uani 1 1 d . . .
O1 O 0.14597(14) 0.35132(13) 0.14297(15) 0.0355(5) Uani 1 1 d . . .
O2 O 0.19471(11) 0.48395(13) 0.09007(13) 0.0312(5) Uani 1 1 d . . .
O2A O 0.09342(13) 0.48318(13) 0.19447(11) 0.0323(6) Uani 1 1 d . . .
O3 O 0.05757(12) 0.56458(13) -0.05792(12) 0.0296(4) Uani 1 1 d . . .
N1 N 0.30224(15) 0.30224(15) 0.30224(15) 0.0257(8) Uani 1 3 d S . .
C1 C 0.3237(6) 0.2583(5) 0.3749(5) 0.0529(19) Uani 0.50 1 d P . .
C1A C 0.3743(3) 0.2570(3) 0.3242(3) 0.0220(10) Uani 0.50 1 d P . .
C2 C 0.1408(2) 0.6752(2) 0.1422(2) 0.0375(7) Uani 1 1 d . . .
N2 N 0.12761(16) 0.30645(16) 0.30453(16) 0.0339(5) Uani 1 1 d . . .
O1W O 0.5000 0.5000 0.5000 0.111(6) Uani 1 12 d S . .
O2W O 0.5936(4) 0.5936(4) 0.5936(4) 0.105(3) Uani 1 3 d S . .
O3W O 0.5484(5) 0.5578(5) 0.7415(4) 0.237(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0118(5) 0.0179(6) 0.0133(6) 0.000 0.000 0.000
P 0.0181(4) 0.0191(3) 0.0171(4) 0.0013(2) -0.0008(2) 0.0020(2)
O1 0.0380(13) 0.0229(9) 0.0456(14) 0.0071(9) -0.0104(10) 0.0066(9)
O2 0.0257(10) 0.0297(13) 0.0382(12) -0.0017(8) 0.0057(8) -0.0044(8)
O2A 0.0372(11) 0.0357(14) 0.0241(10) -0.0035(8) 0.0079(8) -0.0040(9)
O3 0.0289(10) 0.0308(10) 0.0291(10) 0.0022(9) 0.0117(8) -0.0014(9)
N1 0.0257(8) 0.0257(8) 0.0257(8) 0.0011(9) 0.0011(9) 0.0011(9)
C1 0.059(5) 0.052(5) 0.048(4) 0.005(4) -0.009(4) -0.001(4)
C1A 0.014(2) 0.026(3) 0.026(3) 0.006(2) -0.004(2) 0.002(2)
C2 0.0390(19) 0.0373(16) 0.0362(18) -0.0131(15) -0.0044(12) -0.0050(15)
N2 0.0260(11) 0.0375(15) 0.0383(15) 0.0030(10) 0.0073(12) 0.0053(12)
O1W 0.111(6) 0.111(6) 0.111(6) 0.000 0.000 0.000
O2W 0.105(3) 0.105(3) 0.105(3) -0.001(3) -0.001(3) -0.001(3)
O3W 0.306(11) 0.339(11) 0.065(3) -0.046(5) -0.033(4) -0.152(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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'
H H 0.0000 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Al1 O3 103.32(14) 3 . ?
O3 Al1 O3 112.86(14) 3 2_565 ?
O3 Al1 O3 112.40(14) . 2_565 ?
O3 Al1 O3 112.39(14) 3 4_565 ?
O3 Al1 O3 112.86(14) . 4_565 ?
O3 Al1 O3 103.32(14) 2_565 4_565 ?
O2 Al2 O2 105.52(6) 18 4_565 ?
O2 Al2 O2 105.52(6) 18 . ?
O2 Al2 O2 117.71(13) 4_565 . ?
O2 Al2 O2 117.71(13) 18 19_554 ?
O2 Al2 O2 105.52(6) 4_565 19_554 ?
O2 Al2 O2 105.52(6) . 19_554 ?
O2 Zn2 O2 105.52(6) 18 4_565 ?
O2 Zn2 O2 105.52(6) 18 . ?
O2 Zn2 O2 117.71(13) 4_565 . ?
O2 Zn2 O2 117.71(13) 18 19_554 ?
O2 Zn2 O2 105.52(6) 4_565 19_554 ?
O2 Zn2 O2 105.52(6) . 19_554 ?
O2A Al3 O2A 104.77(6) 16 2_565 ?
O2A Al3 O2A 104.77(6) 16 . ?
O2A Al3 O2A 119.34(13) 2_565 . ?
O2A Al3 O2A 119.34(13) 16 15_455 ?
O2A Al3 O2A 104.77(6) 2_565 15_455 ?
O2A Al3 O2A 104.77(6) . 15_455 ?
O2A Zn3 O2A 104.77(6) 16 2_565 ?
O2A Zn3 O2A 104.77(6) 16 . ?
O2A Zn3 O2A 119.34(13) 2_565 . ?
O2A Zn3 O2A 119.34(13) 16 15_455 ?
O2A Zn3 O2A 104.77(6) 2_565 15_455 ?
O2A Zn3 O2A 104.77(6) . 15_455 ?
O1 P O2A 112.85(13) . . ?
O1 P O3 110.15(13) . 4_565 ?
O2A P O3 108.98(13) . 4_565 ?
O1 P O2 111.85(12) . . ?
O2A P O2 104.61(12) . . ?
O3 P O2 108.14(13) 4_565 . ?
P O2 Al2 140.68(14) . . ?
P O2 Zn2 140.68(14) . . ?
Al2 O2 Zn2 0.0 . . ?
P O2A Al3 138.82(14) . . ?
P O2A Zn3 138.82(14) . . ?
Al3 O2A Zn3 0.0 . . ?
P O3 Al1 141.58(15) 4_565 . ?
C1 N1 C1 109.6(4) 9 5 ?
C1 N1 C1 109.6(4) 9 . ?
C1 N1 C1 109.6(4) 5 . ?
C1 N1 C1A 64.7(4) 9 5 ?
C1 N1 C1A 48.1(4) 5 5 ?
C1 N1 C1A 141.0(5) . 5 ?
C1 N1 C1A 48.1(4) 9 9 ?
C1 N1 C1A 141.0(5) 5 9 ?
C1 N1 C1A 64.7(4) . 9 ?
C1A N1 C1A 110.2(3) 5 9 ?
C1 N1 C1A 141.0(5) 9 . ?
C1 N1 C1A 64.7(4) 5 . ?
C1 N1 C1A 48.1(4) . . ?
C1A N1 C1A 110.2(3) 5 . ?
C1A N1 C1A 110.2(3) 9 . ?
C1A C1 N1 66.2(5) . . ?
C1A C1 C2 66.3(6) . 23_545 ?
N1 C1 C2 114.0(6) . 23_545 ?
C1A C1 C1A 120.8(8) . 9 ?
N1 C1 C1A 57.8(4) . 9 ?
C2 C1 C1A 154.9(7) 23_545 9 ?
C1 C1A N1 65.7(5) . . ?
C1 C1A C2 67.3(5) . 23_545 ?
N1 C1A C2 114.3(4) . 23_545 ?
C1 C1A C1 119.2(8) . 5 ?
N1 C1A C1 57.5(4) . 5 ?
C2 C1A C1 156.3(5) 23_545 5 ?
N2 C2 C1A 111.4(3) 16 23 ?
N2 C2 C1 111.5(4) 16 23 ?
C1A C2 C1 46.4(4) 23 23 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 O3 1.749(2) 3 ?
Al1 O3 1.749(2) . ?
Al1 O3 1.749(2) 2_565 ?
Al1 O3 1.749(2) 4_565 ?
Al2 O2 1.795(2) 18 ?
Al2 O2 1.795(2) 4_565 ?
Al2 O2 1.795(2) . ?
Al2 O2 1.795(2) 19_554 ?
Zn2 O2 1.795(2) 18 ?
Zn2 O2 1.795(2) 4_565 ?
Zn2 O2 1.795(2) . ?
Zn2 O2 1.795(2) 19_554 ?
Al3 O2A 1.847(2) 16 ?
Al3 O2A 1.847(2) 2_565 ?
Al3 O2A 1.847(2) . ?
Al3 O2A 1.847(2) 15_455 ?
Zn3 O2A 1.847(2) 16 ?
Zn3 O2A 1.847(2) 2_565 ?
Zn3 O2A 1.847(2) . ?
Zn3 O2A 1.847(2) 15_455 ?
P O1 1.508(2) . ?
P O2A 1.536(2) . ?
P O3 1.539(2) 4_565 ?
P O2 1.551(2) . ?
O3 P 1.539(2) 4_565 ?
N1 C1 1.471(9) 9 ?
N1 C1 1.471(9) 5 ?
N1 C1 1.471(9) . ?
N1 C1A 1.477(5) 5 ?
N1 C1A 1.477(5) 9 ?
N1 C1A 1.477(5) . ?
C1 C1A 1.202(11) . ?
C1 C2 1.530(10) 23_545 ?
C1 C1A 1.576(10) 9 ?
C1A C2 1.519(6) 23_545 ?
C1A C1 1.576(10) 5 ?
C2 N2 1.491(5) 16 ?
C2 C1A 1.519(6) 23 ?
C2 C1 1.530(10) 23 ?
N2 C2 1.491(5) 15_455 ?
|
1101223.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-16 15:05:45 +0200 (Wed, 16 Mar 2016) $
#$Revision: 178224 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101223.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_1101223
loop_
_publ_author_name
'Botar, Bogdan'
'K\"ogerler, Paul'
'Hill, Craig L.'
_publ_contact_author_address
;
Emory University
Department of Chemistry
Atlanta GA 30322-2210
USA
;
_publ_contact_author_email bbotar@emory.edu
_publ_contact_author_fax 404-727-6276
_publ_contact_author_name 'Bogdan Botar'
_publ_contact_author_phone 404-727-4419
_publ_section_title
;
A Nanoring--Nanosphere Molecule, {Mo~214~V~30~}: Pushing the
Boundaries of Controllable Inorganic Structural Organization
at the Molecular Level
;
_journal_coden_ASTM JACSAT
_journal_issue 16
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 5336
_journal_page_last 5337
_journal_paper_doi 10.1021/ja060886s
_journal_volume 128
_journal_year 2006
_chemical_formula_sum 'H1262 K43 Mo214 Na11 O1404 S12 V34'
_chemical_formula_weight 48318.13
_space_group_IT_number 12
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2y'
_symmetry_space_group_name_H-M 'C 1 2/m 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 112.549(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 46.324(5)
_cell_length_b 42.268(4)
_cell_length_c 41.896(4)
_cell_measurement_reflns_used 9224
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 20.69
_cell_measurement_theta_min 2.25
_cell_volume 75763(13)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0886
_diffrn_reflns_av_sigmaI/netI 0.0691
_diffrn_reflns_limit_h_max 48
_diffrn_reflns_limit_h_min -48
_diffrn_reflns_limit_k_max 44
_diffrn_reflns_limit_k_min -44
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_limit_l_min -44
_diffrn_reflns_number 233867
_diffrn_reflns_theta_full 21.97
_diffrn_reflns_theta_max 21.97
_diffrn_reflns_theta_min 1.47
_exptl_absorpt_coefficient_mu 2.154
_exptl_absorpt_correction_T_max 0.9188
_exptl_absorpt_correction_T_min 0.4577
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS V2.10, Sheldrick 2003'
_exptl_crystal_colour blue-black
_exptl_crystal_density_diffrn 2.118
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 46788
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.04
_refine_diff_density_max 2.007
_refine_diff_density_min -1.734
_refine_diff_density_rms 0.251
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 2981
_refine_ls_number_reflns 47009
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.1577
_refine_ls_R_factor_gt 0.0998
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1815P)^2^+2890.0208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2731
_refine_ls_wR_factor_ref 0.3412
_reflns_number_gt 28070
_reflns_number_total 47009
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/m'
_cod_database_code 1101223
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -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
Mo1 Mo 0.37181(6) 0.0000 0.23201(6) 0.0583(7) Uani 1 2 d S . .
Mo2 Mo 0.2697(2) 0.0000 0.50181(10) 0.069(2) Uani 0.79(3) 2 d SP . .
Mo3 Mo 0.32269(5) 0.04584(4) 0.25162(5) 0.0617(5) Uani 1 1 d . . .
Mo4 Mo 0.33697(10) 0.19231(12) 0.43075(7) 0.0635(14) Uani 0.863(17) 1 d P . .
Mo5 Mo 0.38467(5) 0.21240(4) 0.39124(4) 0.0633(5) Uani 1 1 d . . .
Mo6 Mo 0.59426(5) 0.13064(5) 0.35034(4) 0.0682(6) Uani 1 1 d . . .
Mo7 Mo 0.39653(5) 0.07409(4) 0.23667(5) 0.0605(5) Uani 1 1 d . . .
Mo8 Mo 0.41573(9) 0.23804(17) 0.47247(7) 0.0655(15) Uani 0.85(2) 1 d P . .
Mo9 Mo 0.51994(5) 0.14670(5) 0.30300(4) 0.0645(5) Uani 1 1 d . . .
Mo10 Mo 0.57270(12) 0.19263(14) 0.38472(11) 0.0646(16) Uani 0.83(3) 1 d P . .
Mo11 Mo 0.64618(5) 0.07235(6) 0.36966(5) 0.0791(6) Uani 1 1 d . . .
Mo12 Mo 0.33021(13) 0.16332(17) 0.34061(10) 0.0641(16) Uani 0.83(2) 1 d P . .
Mo13 Mo 0.40398(5) 0.19210(4) 0.32521(4) 0.0621(5) Uani 1 1 d . . .
Mo14 Mo 0.65106(12) 0.14689(13) 0.42601(9) 0.0696(16) Uani 0.82(2) 1 d P . .
Mo15 Mo 0.56588(17) 0.07299(17) 0.29341(14) 0.0625(18) Uani 0.74(3) 1 d P . .
Mo16 Mo 0.4412(2) 0.0000 0.2263(4) 0.048(3) Uani 0.50(3) 2 d SP . .
Mo17 Mo 0.26542(16) 0.07433(6) 0.44571(7) 0.0723(17) Uani 0.856(16) 1 d P . .
Mo18 Mo 0.45679(11) 0.2376(2) 0.40715(10) 0.0681(18) Uani 0.74(2) 1 d P . .
Mo19 Mo 0.25463(16) 0.0000 0.41758(9) 0.0667(18) Uani 0.912(18) 2 d SP . .
Mo20 Mo 0.25808(13) 0.04608(6) 0.35462(7) 0.0662(15) Uani 0.864(14) 1 d P . .
Mo21 Mo 0.48180(5) 0.20686(6) 0.15827(5) 0.0842(7) Uani 1 1 d . . .
Mo22 Mo 0.25481(5) 0.37010(5) 0.18549(7) 0.0887(7) Uani 1 1 d . . .
Mo23 Mo 0.45878(6) 0.13065(6) 0.11423(5) 0.0811(7) Uani 1 1 d . . .
Mo24 Mo 0.25969(6) 0.34917(6) 0.11243(6) 0.0984(9) Uani 1 1 d . . .
Mo25 Mo 0.32017(6) 0.36992(5) 0.25636(6) 0.0822(6) Uani 1 1 d . . .
Mo26 Mo 0.44532(6) 0.10798(6) -0.00913(5) 0.0888(7) Uani 1 1 d . . .
Mo27 Mo 0.41812(5) 0.29425(5) 0.22920(5) 0.0755(6) Uani 1 1 d . . .
Mo28 Mo 0.36310(8) 0.5000 0.27707(10) 0.0904(10) Uani 1 2 d S . .
Mo29 Mo 0.30595(16) 0.5000 0.1932(5) 0.075(4) Uani 0.75(5) 2 d SP . .
Mo30 Mo 0.38150(5) 0.42676(5) 0.26221(7) 0.0893(7) Uani 1 1 d . . .
Mo31 Mo 0.37762(5) 0.23656(6) 0.12389(5) 0.0783(6) Uani 1 1 d . . .
Mo32 Mo 0.64477(6) 0.20921(7) -0.01122(6) 0.0971(8) Uani 1 1 d . . .
Mo33 Mo 0.50841(7) 0.11224(6) 0.06367(5) 0.0947(8) Uani 1 1 d . . .
Mo34 Mo 0.34711(6) 0.16809(6) 0.08466(5) 0.0820(7) Uani 1 1 d . . .
Mo35 Mo 0.30344(6) 0.45369(6) 0.26610(9) 0.0975(8) Uani 1 1 d . . .
Mo36 Mo 0.25762(9) 0.42698(7) 0.11348(8) 0.1285(13) Uani 1 1 d . . .
Mo37 Mo 0.60594(5) 0.16551(7) 0.02523(5) 0.0881(7) Uani 1 1 d . . .
Mo38 Mo 0.24404(7) 0.45588(7) 0.1866(2) 0.090(2) Uani 0.796(17) 1 d P . .
Mo39 Mo 0.49531(17) 0.2785(3) 0.2198(3) 0.088(3) Uani 0.85(4) 1 d P . .
Mo40 Mo 0.56286(6) 0.17713(8) 0.07196(6) 0.1043(9) Uani 1 1 d . . .
Mo41 Mo 0.43364(9) 0.5000 0.27476(15) 0.1283(17) Uani 1 2 d S . .
Mo42 Mo 0.29246(7) 0.29592(7) 0.07772(6) 0.1093(9) Uani 1 1 d . . .
Mo43 Mo 0.45984(5) 0.17367(5) 0.04813(5) 0.0755(6) Uani 1 1 d . . .
Mo44 Mo 0.39397(6) 0.12796(6) 0.04332(5) 0.0795(6) Uani 1 1 d . . .
Mo45 Mo 0.32882(5) 0.35283(5) 0.18261(5) 0.0817(7) Uani 1 1 d . . .
Mo46 Mo 0.30702(5) 0.22180(5) 0.12553(5) 0.0759(6) Uani 1 1 d . . .
Mo47 Mo 0.27617(5) 0.28671(5) 0.16191(5) 0.0720(6) Uani 1 1 d . . .
Mo48 Mo 0.34077(5) 0.28952(5) 0.23395(5) 0.0708(6) Uani 1 1 d . . .
Mo49 Mo 0.43738(5) 0.22670(5) 0.20139(4) 0.0653(5) Uani 1 1 d . . .
Mo50 Mo 0.40922(5) 0.16223(5) 0.15779(5) 0.0680(6) Uani 1 1 d . . .
Mo51 Mo 0.36716(5) 0.21913(5) 0.20087(4) 0.0624(5) Uani 1 1 d . . .
Mo52 Mo 0.62534(12) 0.23800(12) 0.06456(13) 0.0953(14) Uani 0.70 1 d P . .
Mo53 Mo 0.6304(3) 0.2189(3) 0.0744(3) 0.089(3) Uani 0.30 1 d P . .
Mo54 Mo 0.2554(3) 0.3813(2) 0.0418(2) 0.214(5) Uani 0.65 1 d P . .
Mo55 Mo 0.2677(2) 0.37271(19) 0.0370(2) 0.067(2) Uiso 0.35 1 d P . .
Mo61 Mo 0.2763(3) 0.4601(3) 0.0360(4) 0.080(5) Uiso 0.25 1 d P . .
Mo62 Mo 0.2611(3) 0.45837(17) 0.0279(2) 0.070(2) Uani 0.30 1 d P . .
Mo63 Mo 0.6820(3) 0.2837(3) 0.0490(3) 0.099(3) Uiso 0.25 1 d P . .
Mo64 Mo 0.2756(3) 0.3311(3) -0.0121(4) 0.121(4) Uiso 0.25 1 d P . .
Mo65 Mo 0.5589(2) 0.2460(3) 0.1958(2) 0.102(3) Uani 0.40 1 d P . .
Mo66 Mo 0.5528(3) 0.2666(2) 0.1826(3) 0.104(3) Uani 0.40 1 d P . .
Mo67 Mo 0.5998(3) 0.2359(5) 0.1417(4) 0.106(5) Uani 0.30 1 d P . .
Mo68 Mo 0.5922(3) 0.2549(3) 0.1258(3) 0.097(4) Uani 0.40 1 d P . .
Mo69 Mo 0.49116(12) 0.34055(14) 0.27915(18) 0.0898(16) Uani 0.45 1 d P . .
Mo70 Mo 0.4886(4) 0.3497(5) 0.2556(6) 0.121(6) Uiso 0.20 1 d P . .
Mo71 Mo 0.46982(14) 0.41938(15) 0.2954(3) 0.106(2) Uani 0.40 1 d P . .
Mo72 Mo 0.4666(4) 0.4246(4) 0.2676(5) 0.107(5) Uiso 0.20 1 d P . .
Mo73 Mo 0.6643(7) 0.2926(6) 0.0332(8) 0.083(6) Uiso 0.10 1 d P . .
Mo81 Mo 0.2871(11) 0.0000 0.5052(6) 0.091(8) Uiso 0.21(3) 2 d SP . .
Mo82 Mo 0.2777(9) 0.0441(4) 0.3629(6) 0.075(7) Uiso 0.136(14) 1 d P . .
Mo83 Mo 0.5599(4) 0.0663(4) 0.3015(7) 0.066(4) Uiso 0.26(3) 1 d P . .
Mo84 Mo 0.2843(9) 0.0732(4) 0.4520(5) 0.065(7) Uiso 0.144(16) 1 d P . .
Mo85 Mo 0.3397(6) 0.1506(7) 0.3489(6) 0.057(6) Uiso 0.17(2) 1 d P . .
Mo86 Mo 0.2746(17) 0.0000 0.4244(11) 0.061(15) Uiso 0.088(18) 2 d SP . .
Mo87 Mo 0.6426(5) 0.1378(5) 0.4331(5) 0.067(6) Uiso 0.18(2) 1 d P . .
Mo88 Mo 0.5669(5) 0.1832(7) 0.3926(8) 0.068(6) Uiso 0.17(3) 1 d P . .
Mo89 Mo 0.2433(3) 0.4552(3) 0.2066(5) 0.055(5) Uiso 0.204(17) 1 d P . .
Mo90 Mo 0.3474(7) 0.1785(9) 0.4361(6) 0.073(8) Uiso 0.137(17) 1 d P . .
Mo91 Mo 0.4477(3) 0.0000 0.2421(6) 0.074(3) Uiso 0.50(3) 2 d SP . .
Mo92 Mo 0.5021(7) 0.2680(8) 0.2330(14) 0.071(9) Uiso 0.15(4) 1 d P . .
Mo93 Mo 0.4627(3) 0.2227(5) 0.4139(3) 0.062(4) Uiso 0.26(2) 1 d P . .
Mo94 Mo 0.4216(5) 0.2230(9) 0.4771(5) 0.067(7) Uiso 0.15(2) 1 d P . .
Mo95 Mo 0.3047(4) 0.5000 0.2078(14) 0.068(7) Uiso 0.25(5) 2 d SP . .
V1 V 0.28392(16) 0.0000 0.29696(15) 0.0758(17) Uani 1 2 d S . .
V2 V 0.37745(11) 0.19992(12) 0.52404(9) 0.0883(14) Uani 1 1 d . . .
V3 V 0.60914(15) 0.0000 0.32629(17) 0.093(2) Uani 1 2 d S . .
V4 V 0.5000 0.24726(18) 0.5000 0.089(2) Uani 1 2 d S . .
V5 V 0.48779(10) 0.20264(11) 0.34677(10) 0.0843(13) Uani 1 1 d . . .
V6 V 0.29092(12) 0.12292(11) 0.38949(10) 0.0861(13) Uani 1 1 d . . .
V7 V 0.69755(12) 0.07622(11) 0.46037(10) 0.0913(14) Uani 1 1 d . . .
V8 V 0.48027(10) 0.07604(10) 0.25717(14) 0.0926(14) Uani 1 1 d . . .
V9 V 0.36244(9) 0.11947(8) 0.28703(8) 0.0567(9) Uani 1 1 d . . .
K1 K 0.43378(12) 0.15012(11) 0.26795(11) 0.0661(13) Uani 1 1 d . . .
K2 K 0.3329(4) 0.1323(4) 0.1767(4) 0.122(5) Uani 0.50 1 d P . .
K3 K 0.2841(2) 0.09314(19) 0.29748(19) 0.126(2) Uani 1 1 d . . .
K4 K 0.2976(3) 0.1523(3) 0.4816(2) 0.077(3) Uani 0.50 1 d P . .
K5 K 0.6933(4) 0.0000 0.4031(4) 0.086(5) Uani 0.50 2 d SP . .
K6 K 0.5271(3) 0.0000 0.2476(3) 0.132(4) Uani 1 2 d S . .
K7 K 0.4121(3) 0.3472(3) 0.2968(4) 0.124(5) Uani 0.50 1 d P . .
K8 K 0.5426(3) 0.2477(3) 0.4329(3) 0.105(4) Uani 0.50 1 d P . .
K9 K 0.5482(10) 0.1548(10) 0.1548(8) 0.113(13) Uani 0.20 1 d P . .
K10 K 0.5479(5) 0.1799(7) 0.1463(5) 0.094(6) Uani 0.30 1 d P . .
O1 O 0.3343(5) 0.0000 0.2445(5) 0.062(5) Uani 1 2 d S . .
O2 O 0.3523(5) 0.0000 0.1892(4) 0.061(5) Uani 1 2 d S . .
O3 O 0.3316(3) 0.2000(3) 0.1692(3) 0.068(4) Uani 1 1 d . . .
O4 O 0.3838(3) 0.3000(3) 0.2406(3) 0.065(4) Uani 1 1 d . . .
O5 O 0.6147(4) 0.0552(4) 0.3993(4) 0.081(4) Uani 1 1 d . . .
O6 O 0.3484(3) 0.2484(3) 0.2190(3) 0.066(4) Uani 1 1 d . . .
O7 O 0.5581(4) 0.1584(3) 0.3466(3) 0.071(4) Uani 1 1 d . . .
O8 O 0.2857(4) 0.0329(4) 0.5300(4) 0.086(5) Uani 1 1 d . . .
O9 O 0.5246(4) 0.0670(4) 0.2685(4) 0.074(4) Uani 1 1 d . . .
O10 O 0.2900(3) 0.2493(4) 0.1495(3) 0.073(4) Uani 1 1 d . . .
O11 O 0.4256(4) 0.1074(3) 0.0783(4) 0.079(4) Uani 1 1 d . . .
O12 O 0.3715(3) 0.1868(3) 0.3482(3) 0.067(4) Uani 1 1 d . . .
O13 O 0.6023(3) 0.0870(4) 0.3367(3) 0.069(4) Uani 1 1 d . . .
O14 O 0.3798(4) 0.1913(3) 0.2318(3) 0.068(4) Uani 1 1 d . . .
O15 O 0.3303(3) 0.1453(3) 0.2406(3) 0.070(4) Uani 1 1 d . . .
O16 O 0.4428(4) 0.1931(3) 0.3265(3) 0.069(4) Uani 1 1 d . . .
O17 O 0.3777(3) 0.0801(3) 0.1934(3) 0.060(4) Uani 1 1 d . . .
O18 O 0.2966(3) 0.2831(3) 0.2097(4) 0.071(4) Uani 1 1 d . . .
O19 O 0.3092(3) 0.1605(3) 0.4172(3) 0.071(4) Uani 1 1 d . . .
O20 O 0.3687(4) 0.1504(4) 0.1311(3) 0.074(4) Uani 1 1 d . . .
O21 O 0.6184(4) 0.1138(4) 0.4433(4) 0.086(5) Uani 1 1 d . . .
O22 O 0.3631(3) 0.0448(3) 0.2418(3) 0.061(4) Uani 1 1 d . . .
O23 O 0.3852(4) 0.1007(3) 0.3215(3) 0.066(4) Uani 1 1 d . . .
O24 O 0.4872(4) 0.2353(3) 0.3211(3) 0.079(5) Uani 1 1 d . . .
O25 O 0.4077(3) 0.0279(3) 0.2335(3) 0.061(4) Uani 1 1 d . . .
O26 O 0.4443(3) 0.1936(3) 0.1707(3) 0.067(4) Uani 1 1 d . . .
O27 O 0.5557(3) 0.1146(4) 0.3116(3) 0.071(4) Uani 1 1 d . . .
O28 O 0.3465(3) 0.1871(3) 0.3870(3) 0.069(4) Uani 1 1 d . . .
O29 O 0.2968(3) 0.0317(3) 0.2710(4) 0.066(4) Uani 1 1 d . . .
O30 O 0.4186(3) 0.2142(3) 0.3724(3) 0.063(4) Uani 1 1 d . . .
O31 O 0.2570(5) 0.0000 0.3704(5) 0.082(6) Uani 1 2 d S . .
O32 O 0.3334(3) 0.3362(3) 0.2314(3) 0.070(4) Uani 1 1 d . . .
O33 O 0.4827(4) 0.1684(4) 0.1392(3) 0.076(4) Uani 1 1 d . . .
O34 O 0.6073(3) 0.1592(4) 0.3917(3) 0.074(4) Uani 1 1 d . . .
O35 O 0.2687(4) 0.0324(4) 0.3201(4) 0.077(4) Uani 1 1 d . . .
O36 O 0.4142(3) 0.2524(3) 0.1522(3) 0.068(4) Uani 1 1 d . . .
O37 O 0.4808(4) 0.1361(4) 0.0816(3) 0.079(4) Uani 1 1 d . . .
O38 O 0.3301(3) 0.3068(3) 0.1782(3) 0.073(4) Uani 1 1 d . . .
O39 O 0.6850(4) 0.1804(6) 0.0265(4) 0.118(7) Uani 1 1 d . . .
O40 O 0.4039(3) 0.2477(3) 0.2129(3) 0.064(4) Uani 1 1 d . . .
O41 O 0.5352(4) 0.1974(4) 0.0388(4) 0.087(5) Uani 1 1 d . . .
O42 O 0.4323(3) 0.1672(3) 0.0727(3) 0.063(4) Uani 1 1 d . . .
O43 O 0.3923(4) 0.1978(4) 0.1097(4) 0.086(5) Uani 1 1 d . . .
O44 O 0.3982(4) 0.0000 0.2901(5) 0.062(5) Uani 1 2 d S . .
O45 O 0.4256(4) 0.1492(3) 0.3641(3) 0.073(4) Uani 1 1 d . . .
O46 O 0.3875(3) 0.2249(3) 0.3009(3) 0.065(4) Uani 1 1 d . . .
O47 O 0.5000 0.1985(5) 0.5000 0.073(6) Uani 1 2 d S . .
O48 O 0.4497(3) 0.2032(4) 0.2368(3) 0.073(4) Uani 1 1 d . . .
O49 O 0.3346(3) 0.1387(4) 0.3077(3) 0.073(4) Uani 1 1 d . . .
O50 O 0.2979(3) 0.0514(3) 0.2101(3) 0.070(4) Uani 1 1 d . . .
O51 O 0.5809(4) 0.0335(4) 0.2986(3) 0.076(4) Uani 1 1 d . . .
O52 O 0.4359(3) 0.0847(3) 0.2446(3) 0.067(4) Uani 1 1 d . . .
O53 O 0.3823(3) 0.1059(3) 0.2551(3) 0.061(4) Uani 1 1 d . . .
O54 O 0.3948(3) 0.2031(3) 0.1750(3) 0.067(4) Uani 1 1 d . . .
O55 O 0.3712(4) 0.1408(4) 0.0682(3) 0.082(5) Uani 1 1 d . . .
O56 O 0.2655(4) 0.0275(4) 0.4600(4) 0.086(5) Uani 1 1 d . . .
O57 O 0.4237(3) 0.2307(3) 0.4279(3) 0.067(4) Uani 1 1 d . . .
O58 O 0.4296(4) 0.1388(4) 0.1358(3) 0.076(4) Uani 1 1 d . . .
O59 O 0.5562(4) 0.1504(4) 0.4117(4) 0.082(5) Uani 1 1 d . . .
O60 O 0.2401(4) 0.2801(5) 0.0505(5) 0.116(7) Uani 1 1 d . . .
O61 O 0.3476(4) 0.4548(3) 0.2701(4) 0.084(5) Uani 1 1 d . . .
O62 O 0.3608(3) 0.0340(4) 0.3065(3) 0.073(4) Uani 1 1 d . . .
O63 O 0.5848(4) 0.2194(4) 0.3625(4) 0.092(5) Uani 1 1 d . . .
O64 O 0.6225(4) 0.1659(4) -0.0125(3) 0.088(5) Uani 1 1 d . . .
O65 O 0.6798(4) 0.1181(4) 0.4511(4) 0.081(4) Uani 1 1 d . . .
O67 O 0.4199(3) 0.0585(3) 0.2955(3) 0.069(4) Uani 1 1 d . . .
O68 O 0.6345(3) 0.1141(4) 0.3858(3) 0.078(4) Uani 1 1 d . . .
O69 O 0.4332(4) 0.2655(4) 0.2819(4) 0.093(5) Uani 1 1 d . . .
O70 O 0.2267(4) 0.0814(4) 0.4353(4) 0.090(5) Uani 1 1 d . . .
O71 O 0.4926(3) 0.1193(3) 0.2745(3) 0.065(4) Uani 1 1 d . . .
O72 O 0.5000 0.2919(5) 0.5000 0.088(7) Uani 1 2 d S . .
O73 O 0.3388(4) 0.2069(4) 0.1067(4) 0.077(4) Uani 1 1 d . . .
O74 O 0.6591(4) 0.1950(4) -0.0435(3) 0.084(5) Uani 1 1 d . . .
O75 O 0.3130(4) 0.1506(4) 0.0740(4) 0.084(5) Uani 1 1 d . . .
O76 O 0.3316(3) 0.0849(3) 0.2674(3) 0.064(4) Uani 1 1 d . . .
O77 O 0.5918(4) 0.2047(4) 0.4289(3) 0.075(4) Uani 1 1 d . . .
O78 O 0.4709(4) 0.0910(4) 0.0330(4) 0.087(5) Uani 1 1 d . . .
O79 O 0.6766(3) 0.0664(4) 0.4112(3) 0.073(4) Uani 1 1 d . . .
O80 O 0.4808(3) 0.1492(4) 0.0232(3) 0.072(4) Uani 1 1 d . . .
O81 O 0.5895(5) 0.0000 0.3584(5) 0.073(6) Uani 1 2 d S . .
O82 O 0.6290(4) 0.2061(5) 0.0281(4) 0.107(6) Uani 1 1 d . . .
O83 O 0.2163(6) 0.0000 0.4050(6) 0.088(7) Uani 1 2 d S . .
O84 O 0.4857(4) 0.2466(4) 0.4494(3) 0.076(4) Uani 1 1 d . . .
O85 O 0.3668(3) 0.2460(3) 0.3740(3) 0.070(4) Uani 1 1 d . . .
O86 O 0.2753(4) 0.3045(4) 0.1172(4) 0.083(5) Uani 1 1 d . . .
O87 O 0.6466(4) 0.1718(4) 0.4580(4) 0.081(5) Uani 1 1 d . . .
O88 O 0.5727(4) 0.1460(4) 0.0387(3) 0.080(5) Uani 1 1 d . . .
O89 O 0.3457(5) 0.5000 0.2201(6) 0.087(7) Uani 1 2 d S . .
O90 O 0.3477(4) 0.1934(4) 0.4769(3) 0.077(4) Uani 1 1 d . . .
O91 O 0.4097(4) 0.1653(3) 0.4148(3) 0.072(4) Uani 1 1 d . . .
O92 O 0.5390(4) 0.1471(4) 0.0812(3) 0.088(5) Uani 1 1 d . . .
O93 O 0.3142(4) 0.2256(4) 0.4172(4) 0.089(5) Uani 1 1 d . . .
O94 O 0.5772(4) 0.0890(4) 0.2635(4) 0.086(5) Uani 1 1 d . . .
O95 O 0.5320(4) 0.2666(5) 0.2193(4) 0.102(6) Uani 1 1 d . . .
O96 O 0.6082(4) 0.1525(4) 0.3262(4) 0.079(4) Uani 1 1 d . . .
O97 O 0.2771(4) 0.3572(4) 0.2309(4) 0.085(5) Uani 1 1 d . . .
O98 O 0.3042(3) 0.1401(4) 0.3535(3) 0.072(4) Uani 1 1 d . . .
O99 O 0.4204(3) 0.1333(4) 0.0135(3) 0.073(4) Uani 1 1 d . . .
O100 O 0.2508(4) 0.1455(4) 0.3684(4) 0.095(5) Uani 1 1 d . . .
O101 O 0.4678(3) 0.0334(3) 0.2383(3) 0.066(4) Uani 1 1 d . . .
O102 O 0.4566(5) 0.0000 0.2883(5) 0.070(6) Uani 1 2 d S . .
O103 O 0.3531(3) 0.2511(3) 0.1496(3) 0.069(4) Uani 1 1 d . . .
O104 O 0.3867(3) 0.1592(3) 0.2969(3) 0.063(4) Uani 1 1 d . . .
O105 O 0.4763(3) 0.0911(4) 0.2102(3) 0.074(4) Uani 1 1 d . . .
O106 O 0.5146(3) 0.1127(4) 0.3456(3) 0.075(4) Uani 1 1 d . . .
O107 O 0.5733(3) 0.1020(3) 0.3834(3) 0.069(4) Uani 1 1 d . . .
O108 O 0.4590(4) 0.2278(4) 0.1220(4) 0.084(5) Uani 1 1 d . . .
O109 O 0.4273(5) 0.0000 0.1839(5) 0.069(6) Uani 1 2 d S . .
O110 O 0.4843(4) 0.0625(4) 0.3019(3) 0.073(4) Uani 1 1 d . . .
O111 O 0.6384(4) 0.0332(4) 0.3526(4) 0.081(4) Uani 1 1 d . . .
O112 O 0.4851(3) 0.2016(4) 0.0692(4) 0.079(4) Uani 1 1 d . . .
O113 O 0.4798(3) 0.2253(3) 0.3833(3) 0.069(4) Uani 1 1 d . . .
O114 O 0.4676(4) 0.1860(3) 0.4275(4) 0.079(4) Uani 1 1 d . . .
O115 O 0.6710(4) 0.1700(4) 0.4085(4) 0.095(5) Uani 1 1 d . . .
O116 O 0.4021(4) 0.1620(4) 0.5189(4) 0.088(5) Uani 1 1 d . . .
O117 O 0.4958(3) 0.1714(3) 0.3161(3) 0.073(4) Uani 1 1 d . . .
O118 O 0.4349(4) 0.1851(3) 0.4794(4) 0.079(4) Uani 1 1 d . . .
O119 O 0.4906(4) 0.1610(4) 0.3796(4) 0.083(5) Uani 1 1 d . . .
O120 O 0.2319(5) 0.0000 0.4961(5) 0.092(7) Uani 1 2 d S . .
O121 O 0.4450(4) 0.2750(3) 0.3917(4) 0.081(5) Uani 1 1 d . . .
O122 O 0.4567(4) 0.2469(3) 0.4949(3) 0.072(4) Uani 1 1 d . . .
O123 O 0.3066(4) 0.1931(3) 0.3165(4) 0.080(5) Uani 1 1 d . . .
O124 O 0.3050(4) 0.4108(4) 0.2631(4) 0.083(4) Uani 1 1 d . . .
O125 O 0.5328(4) 0.2042(3) 0.3740(3) 0.068(4) Uani 1 1 d . . .
O126 O 0.3784(3) 0.2138(3) 0.4364(3) 0.070(4) Uani 1 1 d . . .
O127 O 0.4540(4) 0.2682(4) 0.2243(4) 0.076(4) Uani 1 1 d . . .
O128 O 0.3661(4) 0.3654(4) 0.1926(4) 0.087(5) Uani 1 1 d . . .
O129 O 0.2415(6) 0.0000 0.2581(6) 0.096(7) Uani 1 2 d S . .
O130 O 0.2733(4) 0.3354(4) 0.1646(4) 0.084(5) Uani 1 1 d . . .
O131 O 0.3675(4) 0.2604(4) 0.0892(4) 0.097(6) Uani 1 1 d . . .
O132 O 0.3435(4) 0.2831(4) 0.2740(4) 0.077(4) Uani 1 1 d . . .
O133 O 0.4336(4) 0.1939(4) 0.0115(3) 0.078(4) Uani 1 1 d . . .
O134 O 0.3723(4) 0.1493(4) 0.4451(4) 0.084(5) Uani 1 1 d . . .
O135 O 0.4162(4) 0.1424(4) 0.1952(3) 0.079(4) Uani 1 1 d . . .
O136 O 0.2605(4) 0.0446(3) 0.4050(3) 0.074(4) Uani 1 1 d . . .
O137 O 0.3728(4) 0.0986(4) 0.0196(4) 0.096(5) Uani 1 1 d . . .
O138 O 0.2717(4) 0.0860(4) 0.3604(3) 0.083(5) Uani 1 1 d . . .
O139 O 0.3992(4) 0.2755(4) 0.4614(4) 0.089(5) Uani 1 1 d . . .
O140 O 0.5499(4) 0.0555(4) 0.3386(4) 0.090(5) Uani 1 1 d . . .
O141 O 0.3092(5) 0.0000 0.4361(5) 0.078(6) Uani 1 2 d S . .
O142 O 0.3666(4) 0.1274(4) 0.3762(4) 0.082(5) Uani 1 1 d . . .
O143 O 0.4040(4) 0.3094(4) 0.1887(4) 0.096(5) Uani 1 1 d . . .
O144 O 0.3174(4) 0.0585(4) 0.4577(4) 0.090(5) Uani 1 1 d . . .
O145 O 0.2964(4) 0.2541(4) 0.0896(3) 0.079(4) Uani 1 1 d . . .
O146 O 0.6298(6) 0.0000 0.2919(5) 0.088(7) Uani 1 2 d S . .
O147 O 0.3277(4) 0.3505(4) 0.2937(4) 0.089(5) Uani 1 1 d . . .
O148 O 0.2454(4) 0.4456(5) 0.1379(6) 0.126(9) Uani 1 1 d . . .
O149 O 0.2799(4) 0.1942(4) 0.1080(4) 0.089(5) Uani 1 1 d . . .
O150 O 0.4030(3) 0.2257(3) 0.5062(3) 0.073(4) Uani 1 1 d . . .
O151 O 0.3223(5) 0.0000 0.5029(6) 0.096(8) Uani 1 2 d S . .
O152 O 0.5289(4) 0.1025(4) 0.0336(4) 0.095(5) Uani 1 1 d . . .
O153 O 0.2385(4) 0.2795(4) 0.1554(4) 0.086(5) Uani 1 1 d . . .
O154 O 0.2190(4) 0.0509(4) 0.3361(4) 0.092(5) Uani 1 1 d . . .
O155 O 0.3297(4) 0.1002(4) 0.4103(4) 0.089(5) Uani 1 1 d . . .
O156 O 0.4797(4) 0.1005(4) 0.1372(4) 0.099(6) Uani 1 1 d . . .
O157 O 0.2773(4) 0.1068(4) 0.4247(3) 0.079(4) Uani 1 1 d . . .
O158 O 0.6596(4) 0.0619(5) 0.4682(4) 0.103(6) Uani 1 1 d . . .
O159 O 0.5300(4) 0.1708(4) 0.2762(3) 0.082(5) Uani 1 1 d . . .
O160 O 0.6655(4) 0.0883(4) 0.3461(4) 0.088(5) Uani 1 1 d . . .
O161 O 0.3227(5) 0.0000 0.3339(6) 0.081(6) Uani 1 2 d S . .
O162 O 0.2829(4) 0.0854(4) 0.4907(4) 0.087(5) Uani 1 1 d . . .
O163 O 0.3547(4) 0.2360(4) 0.5285(4) 0.096(5) Uani 1 1 d . . .
O164 O 0.3091(4) 0.3856(4) 0.1996(4) 0.080(4) Uani 1 1 d . . .
O165 O 0.2223(5) 0.3392(4) 0.0989(5) 0.123(8) Uani 1 1 d . . .
O166 O 0.2609(4) 0.4595(4) 0.2394(6) 0.106(6) Uani 1 1 d . . .
O167 O 0.3098(4) 0.3611(4) 0.1381(4) 0.089(5) Uani 1 1 d . . .
O168 O 0.6085(3) 0.2261(4) -0.0407(4) 0.089(5) Uani 1 1 d . . .
O169 O 0.4769(4) 0.2357(4) 0.1950(4) 0.084(5) Uani 1 1 d . . .
O170 O 0.3118(4) 0.0364(4) 0.3854(4) 0.094(5) Uani 1 1 d . . .
O171 O 0.3283(5) 0.3098(5) 0.1018(4) 0.115(7) Uani 1 1 d . . .
O172 O 0.3603(4) 0.3909(4) 0.2650(4) 0.080(4) Uani 1 1 d . . .
O173 O 0.6335(4) 0.1416(6) 0.0493(4) 0.124(8) Uani 1 1 d . . .
O174 O 0.5126(4) 0.2412(4) 0.2658(4) 0.090(5) Uani 1 1 d . . .
O175 O 0.4455(4) 0.3214(4) 0.2536(5) 0.107(6) Uani 1 1 d . . .
O176 O 0.3717(7) 0.5000 0.3193(9) 0.122(10) Uani 1 2 d S . .
O177 O 0.2536(4) 0.3862(4) 0.1401(4) 0.096(5) Uani 1 1 d . . .
O178 O 0.7338(4) 0.0900(5) 0.4530(4) 0.098(5) Uani 1 1 d . . .
O179 O 0.2208(4) 0.3526(4) 0.1757(5) 0.108(6) Uani 1 1 d . . .
O180 O 0.2976(4) 0.4562(4) 0.2053(5) 0.092(5) Uani 1 1 d . . .
O181 O 0.3659(4) 0.4328(4) 0.2189(5) 0.093(5) Uani 1 1 d . . .
O182 O 0.4180(5) 0.0805(5) -0.0254(4) 0.121(7) Uani 1 1 d . . .
O183 O 0.2468(4) 0.4113(4) 0.1950(5) 0.106(6) Uani 1 1 d . . .
O184 O 0.2586(5) 0.5000 0.1864(9) 0.120(11) Uani 1 2 d S . .
O185 O 0.4184(4) 0.4140(4) 0.2699(6) 0.116(7) Uani 1 1 d . . .
O186 O 0.3972(4) 0.4724(4) 0.2755(5) 0.096(5) Uani 1 1 d . . .
O187 O 0.5046(5) 0.3054(4) 0.2549(5) 0.104(6) Uani 1 1 d . . .
O188 O 0.2959(5) 0.4305(4) 0.1351(4) 0.106(6) Uani 1 1 d . . .
O189 O 0.3060(4) 0.4588(4) 0.3042(8) 0.135(9) Uani 1 1 d . . .
O190 O 0.6672(4) 0.2413(5) 0.0067(5) 0.119(7) Uani 1 1 d . . .
O191 O 0.5219(5) 0.0860(5) 0.0956(4) 0.127(8) Uani 1 1 d . . .
O192 O 0.4806(5) 0.3010(6) 0.1852(6) 0.142(8) Uani 1 1 d . . .
O193 O 0.3143(6) 0.5000 0.2585(7) 0.092(7) Uani 1 2 d S . .
O194 O 0.3971(5) 0.4218(5) 0.3211(5) 0.126(7) Uani 1 1 d . . .
O195 O 0.3028(5) 0.5000 0.1544(7) 0.093(7) Uani 1 2 d S . .
O196 O 0.5735(4) 0.2034(6) 0.1062(5) 0.137(9) Uani 1 1 d . . .
O197 O 0.2586(4) 0.3875(5) 0.0844(5) 0.106(6) Uiso 1 1 d . . .
O198 O 0.2687(5) 0.3390(5) 0.0714(6) 0.128(7) Uiso 1 1 d . . .
O199 O 0.6002(5) 0.1451(5) 0.1102(6) 0.131(7) Uiso 1 1 d . . .
O200 O 0.5073(6) 0.1812(6) 0.2083(7) 0.154(9) Uiso 1 1 d . . .
O201 O 0.2049(6) 0.4138(6) 0.0861(7) 0.146(8) Uiso 1 1 d . . .
O202 O 0.2072(5) 0.4637(6) 0.1811(6) 0.137(8) Uiso 1 1 d . . .
O203 O 0.2920(5) 0.2962(5) 0.0356(6) 0.134(7) Uiso 1 1 d . . .
O204 O 0.4458(10) 0.5000 0.3315(12) 0.187(16) Uiso 1 2 d S . .
O205 O 0.4186(10) 0.5000 0.2298(12) 0.177(15) Uiso 1 2 d S . .
O206 O 0.6009(4) 0.1917(5) 0.0623(5) 0.107(6) Uiso 1 1 d . . .
O207 O 0.2512(6) 0.4511(6) 0.0769(7) 0.153(9) Uiso 1 1 d . . .
O208 O 0.5177(5) 0.2233(5) 0.1654(6) 0.127(7) Uiso 1 1 d . . .
O209 O 0.4570(6) 0.4670(7) 0.2802(7) 0.166(10) Uiso 1 1 d . . .
O210 O 0.2027(8) 0.3752(8) 0.0255(9) 0.205(13) Uiso 1 1 d . . .
O211 O 0.6644(10) 0.2193(11) 0.0940(11) 0.114(13) Uiso 0.50 1 d P . .
O212 O 0.6210(7) 0.2414(7) 0.1067(8) 0.186(11) Uiso 1 1 d . . .
O213 O 0.6655(11) 0.1691(11) 0.1262(12) 0.135(15) Uiso 0.50 1 d P . .
O214 O 0.6669(9) 0.1951(11) 0.0995(10) 0.108(12) Uiso 0.50 1 d P . .
O215 O 0.6580(10) 0.2500(11) 0.0730(11) 0.113(13) Uiso 0.50 1 d P . .
O216 O 0.2496(10) 0.4172(9) 0.0259(10) 0.126(12) Uiso 0.60 1 d P . .
O217 O 0.2487(10) 0.3573(10) 0.0030(11) 0.119(13) Uiso 0.50 1 d P . .
O218 O 0.2996(9) 0.3518(9) 0.0150(9) 0.064(10) Uiso 0.40 1 d P . .
O219 O 0.3196(16) 0.3881(17) 0.0820(18) 0.069(19) Uiso 0.20 1 d P . .
O220 O 0.2840(4) 0.3750(3) 0.0402(3) 0.019(3) Uiso 0.80 1 d P . .
O221 O 0.2734(16) 0.4195(14) 0.0300(16) 0.14(2) Uiso 0.40 1 d P . .
O231 O 0.2206(15) 0.4614(15) 0.0064(17) 0.21(2) Uiso 0.55 1 d P . .
O232 O 0.3047(12) 0.4585(11) 0.0586(13) 0.156(16) Uiso 0.55 1 d P . .
O233 O 0.2781(10) 0.4660(10) -0.0033(11) 0.135(14) Uiso 0.55 1 d P . .
O234 O 0.2579(11) 0.5000 0.0423(13) 0.227(19) Uiso 1.10 2 d SP . .
O235 O 0.6788(12) 0.3203(12) 0.0678(14) 0.101(16) Uiso 0.35 1 d P . .
O236 O 0.6491(17) 0.3008(17) 0.010(2) 0.14(2) Uiso 0.35 1 d P . .
O237 O 0.7164(7) 0.2630(7) 0.0771(8) 0.041(8) Uiso 0.35 1 d P . .
O238 O 0.2602(11) 0.3151(11) -0.0360(13) 0.050(12) Uiso 0.25 1 d P . .
O239 O 0.3094(6) 0.3392(6) 0.0080(6) 0.041(6) Uiso 0.50 1 d P . .
O240 O 0.2534(14) 0.3570(15) -0.0605(16) 0.080(17) Uiso 0.25 1 d P . .
O241 O 0.5755(9) 0.2263(10) 0.1672(11) 0.068(11) Uiso 0.35 1 d P . .
O242 O 0.5667(9) 0.2470(10) 0.1511(10) 0.077(11) Uiso 0.40 1 d P . .
O243 O 0.6095(9) 0.2187(8) 0.1524(10) 0.053(11) Uiso 0.50 1 d P . .
O244 O 0.5758(11) 0.2648(11) 0.1120(13) 0.074(17) Uiso 0.45 1 d P . .
O245 O 0.4945(10) 0.3168(11) 0.3160(12) 0.174(16) Uiso 0.65 1 d P . .
O246 O 0.4820(7) 0.3629(8) 0.2298(9) 0.118(10) Uiso 0.65 1 d P . .
O247 O 0.5263(13) 0.3603(14) 0.2849(15) 0.22(2) Uiso 0.65 1 d P . .
O248 O 0.4687(8) 0.3758(8) 0.2826(9) 0.124(11) Uiso 0.63 1 d P . .
O249 O 0.5779(13) 0.2298(12) 0.2154(14) 0.094(14) Uiso 0.40 1 d P . .
O250 O 0.5325(9) 0.2856(9) 0.1545(10) 0.168(13) Uiso 0.80 1 d P . .
O251 O 0.5835(10) 0.2901(11) 0.2051(12) 0.094(13) Uiso 0.40 1 d P . .
O252 O 0.5886(8) 0.2518(8) 0.0362(9) 0.194(12) Uiso 1 1 d . . .
O253 O 0.4728(12) 0.4176(12) 0.3346(15) 0.186(19) Uiso 0.60 1 d P . .
O254 O 0.4585(9) 0.4250(9) 0.2384(11) 0.125(12) Uiso 0.60 1 d P . .
O255 O 0.5569(16) 0.2715(15) 0.0879(19) 0.101(18) Uiso 0.30 1 d P . .
O256 O 0.6497(9) 0.2684(10) 0.0579(11) 0.104(12) Uiso 0.50 1 d P . .
O257 O 0.3232(8) 0.3210(8) 0.0104(8) 0.030(8) Uiso 0.30 1 d P . .
O258 O 0.5917(11) 0.2694(12) 0.2198(12) 0.098(13) Uiso 0.40 1 d P . .
O259 O 0.6286(16) 0.2089(15) 0.1712(18) 0.053(16) Uiso 0.20 1 d P . .
O260 O 0.6136(14) 0.2818(14) 0.1518(15) 0.137(19) Uiso 0.40 1 d P . .
O261 O 0.6274(16) 0.2396(17) 0.1721(18) 0.12(2) Uiso 0.30 1 d P . .
O262 O 0.5039(16) 0.4236(16) 0.3046(17) 0.20(2) Uiso 0.50 1 d P . .
O263 O 0.5713(10) 0.2116(11) 0.2275(11) 0.091(12) Uiso 0.40 1 d P . .
O301 O 0.6491(5) 0.1152(5) 0.5129(5) 0.111(6) Uiso 1 1 d . . .
O302 O 0.3425(6) 0.3055(5) 0.3447(6) 0.066(6) Uiso 0.65 1 d P . .
O303 O 0.3206(4) 0.2070(4) 0.2571(4) 0.084(5) Uiso 1 1 d . . .
O304 O 0.4519(5) 0.1119(5) 0.3279(6) 0.122(7) Uiso 1 1 d . . .
O305 O 0.6440(8) 0.0000 0.4270(9) 0.141(11) Uiso 1 2 d S . .
O306 O 0.5194(7) 0.0000 0.3141(8) 0.127(10) Uiso 1 2 d S . .
O307 O 0.4196(6) 0.0706(6) 0.1558(7) 0.043(7) Uiso 0.40 1 d P . .
O308 O 0.5307(6) 0.1841(6) 0.4498(7) 0.152(9) Uiso 1 1 d . . .
O309 O 0.4928(6) 0.2682(6) 0.0886(7) 0.161(9) Uiso 1 1 d . . .
O310 O 0.4390(7) 0.2944(7) 0.1149(8) 0.174(10) Uiso 1 1 d . . .
O311 O 0.2696(6) 0.1244(7) 0.2347(7) 0.166(10) Uiso 1 1 d . . .
O312 O 0.5309(6) 0.1226(7) 0.2082(7) 0.166(10) Uiso 1 1 d . . .
O313 O 0.2837(7) 0.2403(8) 0.0184(8) 0.080(9) Uiso 0.50 1 d P . .
O314 O 0.3994(8) 0.2947(8) 0.3328(9) 0.199(12) Uiso 1 1 d . . .
O315 O 0.2288(6) 0.2044(7) 0.1392(7) 0.164(10) Uiso 1 1 d . . .
O316 O 0.1922(19) 0.5000 0.105(2) 0.17(3) Uiso 0.50 2 d SP . .
O317 O 0.5937(13) 0.0807(13) 0.1064(14) 0.163(19) Uiso 0.50 1 d P . .
O318 O 0.1867(8) 0.2871(8) 0.1715(9) 0.196(12) Uiso 1 1 d . . .
O319 O 0.3103(8) 0.0902(8) 0.0362(9) 0.208(13) Uiso 1 1 d . . .
O320 O 0.1710(10) 0.3955(10) 0.1925(11) 0.252(17) Uiso 1 1 d . . .
O321 O 0.5188(10) 0.2490(10) -0.0065(11) 0.126(14) Uiso 0.50 1 d P . .
O322 O 0.3573(9) 0.4073(10) 0.3538(11) 0.116(12) Uiso 0.50 1 d P . .
O323 O 0.3651(10) 0.4714(11) 0.1623(12) 0.132(15) Uiso 0.50 1 d P . .
O324 O 0.2615(10) 0.2134(10) 0.2097(11) 0.125(14) Uiso 0.50 1 d P . .
O325 O 0.2960(11) 0.3902(12) 0.3397(13) 0.146(16) Uiso 0.50 1 d P . .
O326 O 0.2845(17) 0.0000 0.151(2) 0.16(3) Uiso 0.50 2 d SP . .
O327 O 0.5000 0.0339(19) 0.0000 0.16(3) Uiso 0.50 2 d SP . .
O328 O 0.5793(11) 0.2195(11) 0.2900(13) 0.143(16) Uiso 0.50 1 d P . .
O329 O 0.2200(16) 0.5000 0.2597(18) 0.14(2) Uiso 0.50 2 d SP . .
O330 O 0.3915(12) 0.3331(13) 0.1209(14) 0.159(18) Uiso 0.50 1 d P . .
O331 O 0.2618(12) 0.2885(12) 0.2574(13) 0.147(17) Uiso 0.50 1 d P . .
O332 O 0.2349(13) 0.3954(13) 0.2627(14) 0.163(19) Uiso 0.50 1 d P . .
O333 O 0.240(2) 0.0000 0.191(2) 0.20(3) Uiso 0.50 2 d SP . .
O334 O 0.5549(10) 0.1178(11) 0.1643(12) 0.131(14) Uiso 0.50 1 d P . .
O335 O 0.3642(18) 0.0000 0.122(2) 0.17(3) Uiso 0.50 2 d SP . .
O336 O 0.1697(12) 0.3955(12) 0.1257(13) 0.153(17) Uiso 0.50 1 d P . .
O337 O 0.3402(4) 0.0698(4) 0.3495(5) 0.093(5) Uiso 1 1 d . . .
O338 O 0.4234(13) 0.3694(14) 0.1713(15) 0.17(2) Uiso 0.50 1 d P . .
O339 O 0.3166(13) 0.0520(13) 0.1382(15) 0.167(19) Uiso 0.50 1 d P . .
O340 O 0.5111(13) -0.0429(13) 0.1911(15) 0.17(2) Uiso 0.50 1 d P . .
O341 O 0.2767(8) 0.2157(9) 0.0211(9) 0.092(10) Uiso 0.50 1 d P . .
O342 O 0.2212(8) 0.5000 0.0854(9) 0.146(12) Uiso 1 2 d S . .
O343 O 0.3250(8) 0.2947(7) 0.3326(8) 0.072(8) Uiso 0.50 1 d P . .
O344 O 0.2338(14) 0.1705(14) 0.2359(16) 0.18(2) Uiso 0.50 1 d P . .
O345 O 0.4462(13) 0.3195(13) 0.4446(15) 0.166(19) Uiso 0.50 1 d P . .
O346 O 0.5977(12) 0.2899(13) -0.0460(14) 0.159(18) Uiso 0.50 1 d P . .
O347 O 0.3603(14) 0.0774(14) 0.0997(16) 0.18(2) Uiso 0.50 1 d P . .
O348 O 0.1554(14) 0.4464(14) 0.0404(16) 0.18(2) Uiso 0.50 1 d P . .
O349 O 0.6385(14) 0.1171(15) 0.2734(16) 0.19(2) Uiso 0.50 1 d P . .
O404 O 0.5290(11) 0.0682(11) 0.3871(12) 0.030(12) Uiso 0.20 1 d P . .
O405 O 0.5635(18) 0.0956(19) 0.439(2) 0.08(2) Uiso 0.20 1 d P . .
O406 O 0.4080(13) 0.1087(13) 0.4314(14) 0.043(14) Uiso 0.20 1 d P . .
O407 O 0.4259(17) 0.1115(17) 0.4116(18) 0.069(19) Uiso 0.20 1 d P . .
O408 O 0.4555(18) 0.1262(18) 0.423(2) 0.08(2) Uiso 0.20 1 d P . .
O411 O 0.3572(19) 0.027(2) 0.443(2) 0.09(2) Uiso 0.20 1 d P . .
O412 O 0.361(2) 0.018(2) 0.481(3) 0.11(3) Uiso 0.20 1 d P . .
O414 O 0.4009(13) 0.0000 0.3507(14) 0.079(15) Uiso 0.40 2 d SP . .
S1 S 0.5998(7) 0.0827(7) 0.4171(8) 0.070(8) Uiso 0.20 1 d P . .
S2 S 0.5764(9) 0.0632(9) 0.3795(10) 0.098(11) Uiso 0.20 1 d P . .
S3 S 0.5431(11) 0.1177(11) 0.3860(12) 0.118(13) Uiso 0.20 1 d P . .
S4 S 0.5409(5) 0.0852(5) 0.3616(6) 0.042(5) Uiso 0.20 1 d P . .
S5 S 0.5777(6) 0.1172(6) 0.4203(7) 0.061(7) Uiso 0.20 1 d P . .
S6 S 0.3865(5) 0.1369(5) 0.4165(5) 0.034(5) Uiso 0.20 1 d P . .
S7 S 0.4065(7) 0.1378(7) 0.3889(8) 0.072(8) Uiso 0.20 1 d P . .
S8 S 0.4403(8) 0.1572(8) 0.4051(8) 0.078(8) Uiso 0.20 1 d P . .
S9 S 0.4433(8) 0.1702(8) 0.4472(9) 0.087(9) Uiso 0.20 1 d P . .
S10 S 0.4115(11) 0.1580(11) 0.4546(12) 0.121(14) Uiso 0.20 1 d P . .
S11 S 0.3245(8) 0.0343(8) 0.4308(9) 0.088(9) Uiso 0.20 1 d P . .
S12 S 0.3267(8) 0.0204(8) 0.4716(9) 0.086(9) Uiso 0.20 1 d P . .
S13 S 0.3225(9) 0.0000 0.4038(10) 0.059(9) Uiso 0.20 2 d SP . .
S14 S 0.3782(4) 0.0000 0.3144(5) 0.053(4) Uiso 0.40 2 d SP . .
S15 S 0.3978(8) 0.0335(9) 0.3075(9) 0.061(9) Uiso 0.15 1 d P . .
S16 S 0.4323(11) 0.0209(11) 0.3015(12) 0.089(13) Uiso 0.15 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0758(18) 0.0568(16) 0.0407(14) 0.000 0.0205(13) 0.000
Mo2 0.068(6) 0.098(3) 0.042(2) 0.000 0.021(2) 0.000
Mo3 0.0736(13) 0.0608(12) 0.0488(11) -0.0002(9) 0.0214(9) 0.0020(10)
Mo4 0.077(2) 0.070(3) 0.0369(15) -0.0029(12) 0.0142(13) 0.0154(19)
Mo5 0.0828(14) 0.0599(12) 0.0380(10) -0.0014(8) 0.0127(9) 0.0065(10)
Mo6 0.0780(14) 0.0867(14) 0.0359(10) 0.0015(9) 0.0175(9) -0.0100(11)
Mo7 0.0771(13) 0.0600(12) 0.0449(10) 0.0024(8) 0.0240(9) -0.0011(10)
Mo8 0.089(2) 0.060(3) 0.0363(15) -0.0032(13) 0.0108(13) 0.0055(18)
Mo9 0.0801(13) 0.0733(13) 0.0324(9) 0.0029(8) 0.0131(9) -0.0046(10)
Mo10 0.078(2) 0.071(2) 0.0352(19) 0.0025(14) 0.0111(13) -0.0138(19)
Mo11 0.0758(14) 0.1051(17) 0.0499(12) -0.0074(11) 0.0168(10) -0.0036(12)
Mo12 0.078(2) 0.068(3) 0.0389(18) -0.0047(16) 0.0142(16) 0.007(2)
Mo13 0.0811(14) 0.0596(12) 0.0370(10) -0.0001(8) 0.0130(9) 0.0000(10)
Mo14 0.071(2) 0.091(2) 0.0411(18) 0.0009(14) 0.0156(13) -0.019(2)
Mo15 0.071(2) 0.083(2) 0.033(2) 0.0008(15) 0.0207(15) -0.011(2)
Mo16 0.064(4) 0.056(4) 0.022(6) 0.000 0.014(4) 0.000
Mo17 0.081(4) 0.0900(19) 0.0458(16) 0.0001(12) 0.0237(18) 0.0068(15)
Mo18 0.088(2) 0.065(4) 0.0385(19) -0.0080(18) 0.0101(16) -0.003(2)
Mo19 0.064(5) 0.088(2) 0.046(2) 0.000 0.019(2) 0.000
Mo20 0.074(4) 0.0790(18) 0.0418(15) -0.0010(11) 0.0185(16) 0.0040(14)
Mo21 0.0850(15) 0.1172(19) 0.0495(12) -0.0163(12) 0.0248(11) -0.0161(13)
Mo22 0.0734(15) 0.0653(14) 0.1047(18) 0.0123(12) 0.0091(13) -0.0047(11)
Mo23 0.1116(18) 0.0937(16) 0.0405(11) 0.0119(10) 0.0322(11) 0.0102(13)
Mo24 0.1050(18) 0.0722(15) 0.0732(15) 0.0244(12) -0.0155(13) -0.0122(13)
Mo25 0.0890(16) 0.0710(14) 0.0800(15) 0.0084(11) 0.0251(12) 0.0026(12)
Mo26 0.128(2) 0.1011(18) 0.0459(12) -0.0024(11) 0.0429(13) -0.0209(15)
Mo27 0.0798(14) 0.0749(14) 0.0678(13) 0.0039(10) 0.0238(11) -0.0065(11)
Mo28 0.077(2) 0.067(2) 0.109(3) 0.000 0.0166(19) 0.000
Mo29 0.068(3) 0.083(3) 0.063(8) 0.000 0.013(3) 0.000
Mo30 0.0744(15) 0.0682(14) 0.1111(19) 0.0035(13) 0.0198(13) 0.0031(11)
Mo31 0.0836(15) 0.0977(16) 0.0407(11) 0.0131(10) 0.0094(10) -0.0206(12)
Mo32 0.116(2) 0.124(2) 0.0479(13) -0.0248(13) 0.0278(13) -0.0086(16)
Mo33 0.131(2) 0.1144(19) 0.0446(12) 0.0160(12) 0.0407(13) 0.0299(16)
Mo34 0.0916(16) 0.1064(18) 0.0456(12) -0.0030(11) 0.0235(11) -0.0222(13)
Mo35 0.0922(18) 0.0724(16) 0.129(2) 0.0013(15) 0.0434(17) 0.0029(13)
Mo36 0.161(3) 0.0776(19) 0.090(2) 0.0258(15) -0.014(2) -0.0237(18)
Mo37 0.0785(15) 0.146(2) 0.0345(11) -0.0135(12) 0.0156(10) 0.0170(14)
Mo38 0.076(2) 0.073(2) 0.105(5) 0.0093(18) 0.018(2) -0.0015(15)
Mo39 0.083(3) 0.110(4) 0.069(4) -0.004(4) 0.027(3) -0.016(3)
Mo40 0.0879(17) 0.167(3) 0.0586(14) -0.0422(15) 0.0290(13) -0.0028(17)
Mo41 0.079(3) 0.080(3) 0.213(5) 0.000 0.041(3) 0.000
Mo42 0.132(2) 0.117(2) 0.0562(14) 0.0325(13) 0.0103(14) -0.0198(17)
Mo43 0.0820(14) 0.0914(15) 0.0416(11) 0.0149(10) 0.0109(10) -0.0016(12)
Mo44 0.1034(17) 0.0968(16) 0.0420(11) 0.0024(10) 0.0321(11) -0.0171(13)
Mo45 0.0880(16) 0.0868(16) 0.0539(12) 0.0195(11) 0.0089(11) -0.0191(12)
Mo46 0.0777(14) 0.0857(15) 0.0536(12) 0.0050(10) 0.0133(10) -0.0097(11)
Mo47 0.0750(14) 0.0656(13) 0.0610(12) 0.0149(10) 0.0102(10) -0.0064(10)
Mo48 0.0836(14) 0.0716(13) 0.0518(12) 0.0132(9) 0.0201(10) 0.0017(11)
Mo49 0.0719(13) 0.0814(14) 0.0372(10) 0.0026(9) 0.0147(9) -0.0039(10)
Mo50 0.0916(15) 0.0760(13) 0.0370(10) 0.0055(9) 0.0253(10) -0.0074(11)
Mo51 0.0762(13) 0.0669(12) 0.0408(10) 0.0100(8) 0.0188(9) -0.0059(10)
Mo52 0.104(3) 0.099(3) 0.079(3) -0.049(3) 0.030(3) -0.012(3)
Mo53 0.123(9) 0.091(8) 0.061(6) -0.013(5) 0.042(5) -0.016(7)
Mo54 0.337(14) 0.182(8) 0.121(5) 0.091(5) 0.087(7) 0.037(8)
Mo62 0.107(8) 0.046(4) 0.054(5) -0.005(3) 0.027(5) -0.002(5)
Mo65 0.074(5) 0.166(9) 0.077(6) -0.065(6) 0.040(5) -0.037(7)
Mo66 0.106(7) 0.116(7) 0.112(8) -0.060(6) 0.067(6) -0.041(6)
Mo67 0.097(9) 0.152(16) 0.086(10) -0.050(10) 0.053(9) -0.035(12)
Mo68 0.122(10) 0.104(8) 0.093(8) -0.043(6) 0.071(8) -0.037(8)
Mo69 0.067(3) 0.085(4) 0.101(5) -0.025(3) 0.014(3) 0.001(3)
Mo71 0.063(4) 0.070(4) 0.165(8) -0.023(4) 0.023(4) -0.005(3)
V1 0.118(5) 0.054(3) 0.083(4) 0.000 0.069(4) 0.000
V2 0.096(3) 0.124(4) 0.029(2) 0.004(2) 0.006(2) -0.021(3)
V3 0.081(4) 0.085(4) 0.077(4) 0.000 -0.010(3) 0.000
V4 0.084(4) 0.140(6) 0.028(3) 0.000 0.004(3) 0.000
V5 0.079(3) 0.103(3) 0.056(2) -0.025(2) 0.009(2) -0.006(2)
V6 0.131(4) 0.088(3) 0.050(2) -0.020(2) 0.045(2) -0.030(3)
V7 0.118(4) 0.093(3) 0.041(2) -0.004(2) 0.005(2) 0.014(3)
V8 0.071(3) 0.072(3) 0.123(4) -0.035(3) 0.025(3) -0.006(2)
V9 0.076(2) 0.053(2) 0.0431(19) -0.0073(15) 0.0253(18) -0.0056(18)
K1 0.085(3) 0.062(3) 0.043(3) 0.002(2) 0.016(2) -0.001(2)
K2 0.158(13) 0.118(11) 0.091(9) 0.014(8) 0.049(9) -0.012(10)
K3 0.152(7) 0.129(6) 0.095(5) -0.008(4) 0.047(5) -0.008(5)
K4 0.089(7) 0.095(8) 0.040(5) -0.004(5) 0.018(5) 0.002(6)
K5 0.085(11) 0.117(13) 0.042(8) 0.000 0.008(7) 0.000
K6 0.132(9) 0.144(10) 0.118(8) 0.000 0.046(7) 0.000
K7 0.113(11) 0.101(10) 0.118(11) 0.009(8) 0.001(9) 0.019(8)
K8 0.119(10) 0.128(11) 0.055(7) -0.010(7) 0.019(7) 0.008(8)
K9 0.18(4) 0.12(3) 0.058(19) 0.010(19) 0.07(2) 0.00(3)
K10 0.109(16) 0.13(2) 0.045(11) -0.005(12) 0.038(10) 0.013(14)
O1 0.078(14) 0.040(11) 0.062(12) 0.000 0.021(10) 0.000
O2 0.098(15) 0.050(11) 0.033(10) 0.000 0.023(10) 0.000
O3 0.079(10) 0.066(9) 0.054(9) 0.007(7) 0.021(7) -0.009(7)
O4 0.081(10) 0.056(8) 0.051(8) 0.013(6) 0.018(7) 0.002(7)
O5 0.083(11) 0.106(12) 0.058(9) 0.015(8) 0.032(8) 0.009(9)
O6 0.076(10) 0.064(9) 0.049(8) 0.003(7) 0.014(7) -0.007(7)
O7 0.105(12) 0.074(10) 0.028(7) 0.000(6) 0.018(7) -0.009(8)
O8 0.104(13) 0.099(12) 0.052(9) 0.008(8) 0.026(9) -0.007(10)
O9 0.092(11) 0.085(11) 0.050(9) -0.005(7) 0.033(8) -0.002(9)
O10 0.062(9) 0.090(11) 0.053(9) 0.011(8) 0.008(7) -0.006(8)
O11 0.122(13) 0.068(10) 0.059(9) 0.003(7) 0.048(9) -0.010(9)
O12 0.084(10) 0.072(9) 0.030(7) -0.001(6) 0.005(7) -0.005(8)
O13 0.070(9) 0.095(11) 0.033(7) 0.001(7) 0.009(7) -0.017(8)
O14 0.100(11) 0.059(9) 0.046(8) 0.017(6) 0.027(8) 0.006(8)
O15 0.087(10) 0.062(9) 0.055(9) 0.001(7) 0.021(8) 0.003(8)
O16 0.107(12) 0.056(9) 0.029(7) -0.002(6) 0.011(7) 0.005(8)
O17 0.077(9) 0.065(9) 0.032(7) -0.002(6) 0.014(7) -0.002(7)
O18 0.084(10) 0.054(9) 0.071(10) 0.012(7) 0.027(8) -0.001(7)
O19 0.085(10) 0.083(10) 0.042(8) 0.005(7) 0.020(7) 0.012(8)
O20 0.088(11) 0.102(12) 0.039(8) -0.003(7) 0.033(7) -0.017(9)
O21 0.101(12) 0.112(13) 0.053(9) -0.010(8) 0.039(9) -0.034(10)
O22 0.086(10) 0.049(8) 0.043(8) 0.002(6) 0.021(7) 0.001(7)
O23 0.108(11) 0.053(8) 0.042(8) 0.008(6) 0.035(8) 0.003(8)
O24 0.112(12) 0.069(10) 0.033(8) 0.021(7) 0.003(8) -0.003(8)
O25 0.095(10) 0.053(8) 0.040(7) 0.005(6) 0.030(7) 0.008(7)
O26 0.074(10) 0.082(10) 0.044(8) 0.006(7) 0.023(7) -0.001(8)
O27 0.077(10) 0.091(11) 0.044(8) 0.003(7) 0.020(7) -0.015(8)
O28 0.071(9) 0.085(10) 0.042(8) -0.006(7) 0.011(7) 0.021(8)
O29 0.069(9) 0.064(9) 0.065(9) -0.002(7) 0.025(8) 0.004(7)
O30 0.070(9) 0.070(9) 0.034(7) -0.011(6) 0.002(6) -0.011(7)
O31 0.091(16) 0.090(16) 0.064(14) 0.000 0.028(12) 0.000
O32 0.077(10) 0.077(10) 0.055(9) 0.014(7) 0.025(8) -0.001(8)
O33 0.088(11) 0.098(12) 0.045(8) 0.013(8) 0.030(8) 0.009(9)
O34 0.078(10) 0.088(11) 0.047(8) 0.006(7) 0.016(7) -0.004(8)
O35 0.099(12) 0.073(10) 0.059(9) 0.009(7) 0.031(8) 0.018(9)
O36 0.090(10) 0.072(9) 0.037(7) 0.008(6) 0.019(7) -0.015(8)
O37 0.094(11) 0.099(12) 0.045(8) 0.016(8) 0.029(8) 0.018(9)
O38 0.087(11) 0.075(10) 0.045(8) 0.022(7) 0.014(7) -0.014(8)
O39 0.071(11) 0.21(2) 0.051(10) 0.007(12) 0.003(8) 0.021(12)
O40 0.073(9) 0.077(10) 0.040(8) 0.011(7) 0.020(7) -0.002(7)
O41 0.078(11) 0.099(13) 0.091(12) -0.014(9) 0.040(10) -0.005(9)
O42 0.067(9) 0.084(10) 0.033(7) 0.007(6) 0.013(6) -0.008(7)
O43 0.107(13) 0.100(12) 0.044(9) 0.009(8) 0.020(8) -0.012(10)
O44 0.070(13) 0.059(12) 0.052(12) 0.000 0.020(10) 0.000
O45 0.090(11) 0.079(10) 0.042(8) 0.010(7) 0.017(7) 0.015(8)
O46 0.085(10) 0.050(8) 0.049(8) 0.010(6) 0.011(7) -0.005(7)
O47 0.074(14) 0.076(14) 0.064(13) 0.000 0.020(11) 0.000
O48 0.085(10) 0.089(11) 0.036(8) -0.007(7) 0.015(7) -0.010(8)
O49 0.078(10) 0.084(11) 0.046(8) -0.003(7) 0.012(7) 0.002(8)
O50 0.084(10) 0.083(10) 0.042(8) 0.004(7) 0.021(7) 0.011(8)
O51 0.083(11) 0.094(11) 0.046(8) -0.007(8) 0.019(8) -0.004(9)
O52 0.099(11) 0.068(9) 0.032(7) 0.010(6) 0.021(7) -0.001(8)
O53 0.083(10) 0.058(8) 0.037(7) -0.008(6) 0.018(7) -0.006(7)
O54 0.094(11) 0.072(10) 0.046(8) 0.001(7) 0.037(8) -0.013(8)
O55 0.098(12) 0.107(12) 0.041(8) 0.003(8) 0.027(8) -0.023(10)
O56 0.112(13) 0.098(12) 0.049(9) 0.002(8) 0.032(9) 0.010(10)
O57 0.074(10) 0.078(10) 0.045(8) -0.013(7) 0.019(7) -0.001(8)
O58 0.099(12) 0.083(11) 0.044(8) -0.002(7) 0.025(8) -0.003(9)
O59 0.113(13) 0.068(10) 0.064(10) 0.000(8) 0.032(9) -0.003(9)
O60 0.100(14) 0.128(16) 0.079(12) 0.013(11) -0.010(10) -0.002(12)
O61 0.094(12) 0.065(10) 0.089(12) -0.007(8) 0.031(9) -0.006(8)
O62 0.082(10) 0.084(11) 0.042(8) 0.004(7) 0.012(7) 0.020(8)
O63 0.133(15) 0.082(11) 0.061(10) 0.008(8) 0.037(10) -0.014(10)
O64 0.082(11) 0.154(16) 0.025(7) -0.012(8) 0.017(7) 0.026(10)
O65 0.086(11) 0.094(12) 0.052(9) -0.004(8) 0.015(8) -0.021(9)
O67 0.085(10) 0.069(9) 0.047(8) 0.009(7) 0.020(7) -0.003(8)
O68 0.079(10) 0.096(12) 0.047(9) -0.005(8) 0.011(8) -0.019(9)
O69 0.093(12) 0.107(13) 0.054(10) 0.001(9) -0.001(9) 0.012(10)
O70 0.089(12) 0.098(13) 0.086(12) -0.004(9) 0.039(10) 0.003(10)
O71 0.082(10) 0.064(9) 0.046(8) 0.001(7) 0.022(7) 0.002(7)
O72 0.13(2) 0.044(12) 0.083(16) 0.000 0.031(14) 0.000
O73 0.082(11) 0.098(12) 0.061(9) -0.006(8) 0.039(8) -0.018(9)
O74 0.090(11) 0.112(13) 0.038(8) 0.002(8) 0.011(8) 0.002(9)
O75 0.096(12) 0.098(12) 0.058(10) -0.006(8) 0.030(9) -0.018(9)
O76 0.078(10) 0.060(9) 0.051(8) 0.000(7) 0.023(7) -0.005(7)
O77 0.092(11) 0.083(11) 0.037(8) 0.001(7) 0.011(7) 0.005(8)
O78 0.138(15) 0.077(11) 0.056(9) 0.004(8) 0.048(10) -0.006(10)
O79 0.078(10) 0.101(12) 0.043(8) -0.001(7) 0.025(7) 0.008(8)
O80 0.077(10) 0.092(11) 0.040(8) -0.001(7) 0.014(7) -0.002(8)
O81 0.090(16) 0.087(15) 0.047(12) 0.000 0.034(11) 0.000
O82 0.084(12) 0.177(19) 0.054(10) -0.053(11) 0.019(9) -0.029(12)
O83 0.11(2) 0.096(17) 0.062(14) 0.000 0.032(13) 0.000
O84 0.105(12) 0.080(10) 0.032(8) 0.000(7) 0.015(8) -0.011(9)
O85 0.085(10) 0.064(9) 0.044(8) -0.001(7) 0.008(7) 0.011(8)
O86 0.081(11) 0.082(11) 0.056(9) 0.018(8) -0.006(8) -0.020(8)
O87 0.088(11) 0.099(12) 0.044(8) -0.003(8) 0.012(8) -0.021(9)
O88 0.083(11) 0.122(13) 0.041(8) 0.005(8) 0.031(8) 0.034(9)
O89 0.077(15) 0.070(15) 0.101(18) 0.000 0.019(13) 0.000
O90 0.086(11) 0.095(11) 0.032(8) -0.003(7) 0.003(7) 0.008(9)
O91 0.098(11) 0.061(9) 0.044(8) 0.004(7) 0.012(8) 0.020(8)
O92 0.091(12) 0.126(14) 0.033(8) -0.008(8) 0.008(8) 0.021(10)
O93 0.110(13) 0.087(12) 0.063(10) -0.005(8) 0.025(9) 0.026(10)
O94 0.093(12) 0.123(14) 0.044(9) 0.010(8) 0.028(8) 0.004(10)
O95 0.088(12) 0.135(16) 0.091(12) -0.065(11) 0.044(10) -0.040(11)
O96 0.094(11) 0.094(11) 0.051(9) -0.004(8) 0.032(8) -0.017(9)
O97 0.088(11) 0.062(10) 0.106(13) 0.005(9) 0.038(10) 0.003(8)
O98 0.080(10) 0.086(11) 0.038(8) 0.000(7) 0.011(7) 0.002(8)
O99 0.084(10) 0.100(12) 0.040(8) 0.007(7) 0.030(7) -0.011(9)
O100 0.090(12) 0.117(14) 0.063(10) -0.010(9) 0.012(9) 0.033(10)
O101 0.082(10) 0.068(9) 0.052(8) -0.006(7) 0.031(8) 0.005(8)
O102 0.082(14) 0.089(15) 0.037(11) 0.000 0.021(10) 0.000
O103 0.071(9) 0.081(10) 0.043(8) 0.011(7) 0.008(7) -0.018(8)
O104 0.090(10) 0.057(8) 0.038(7) 0.004(6) 0.020(7) 0.002(7)
O105 0.078(10) 0.105(12) 0.032(7) 0.015(7) 0.014(7) -0.002(9)
O106 0.080(10) 0.095(11) 0.045(8) 0.018(8) 0.018(7) 0.002(8)
O107 0.080(10) 0.079(10) 0.046(8) -0.002(7) 0.021(7) -0.002(8)
O108 0.117(13) 0.085(11) 0.058(9) 0.010(8) 0.043(9) -0.008(10)
O109 0.100(16) 0.062(13) 0.038(11) 0.000 0.018(11) 0.000
O110 0.090(11) 0.093(11) 0.043(8) 0.004(7) 0.032(8) -0.007(9)
O111 0.076(10) 0.107(12) 0.054(9) 0.007(8) 0.018(8) -0.009(9)
O112 0.059(9) 0.117(13) 0.049(9) 0.002(8) 0.007(7) -0.013(9)
O113 0.090(11) 0.071(9) 0.039(8) -0.004(7) 0.017(7) -0.007(8)
O114 0.081(10) 0.069(10) 0.061(10) 0.018(8) -0.002(8) 0.003(8)
O115 0.113(13) 0.119(14) 0.058(10) 0.003(9) 0.040(10) -0.035(11)
O116 0.123(14) 0.087(11) 0.052(9) 0.003(8) 0.032(9) 0.021(10)
O117 0.088(11) 0.079(10) 0.033(7) 0.011(7) 0.003(7) -0.005(8)
O118 0.117(13) 0.060(9) 0.048(9) -0.002(7) 0.019(8) 0.007(9)
O119 0.096(12) 0.081(11) 0.072(10) 0.024(8) 0.032(9) 0.008(9)
O120 0.074(16) 0.14(2) 0.054(14) 0.000 0.013(11) 0.000
O121 0.114(13) 0.055(9) 0.064(10) 0.001(7) 0.024(9) 0.002(8)
O122 0.091(11) 0.070(10) 0.046(8) -0.011(7) 0.017(8) 0.005(8)
O123 0.098(12) 0.066(10) 0.061(9) 0.009(7) 0.014(8) 0.029(8)
O124 0.098(12) 0.073(10) 0.080(11) 0.002(8) 0.036(9) 0.002(9)
O125 0.101(11) 0.058(9) 0.040(8) 0.000(6) 0.022(7) -0.004(8)
O126 0.090(11) 0.074(10) 0.035(8) -0.004(7) 0.012(7) 0.011(8)
O127 0.084(11) 0.085(11) 0.057(9) -0.010(8) 0.024(8) -0.004(8)
O128 0.100(12) 0.097(12) 0.056(9) 0.006(8) 0.020(9) -0.033(10)
O129 0.12(2) 0.088(17) 0.068(15) 0.000 0.017(14) 0.000
O130 0.089(11) 0.066(10) 0.080(11) 0.020(8) 0.012(9) -0.010(8)
O131 0.129(15) 0.111(13) 0.036(8) 0.023(8) 0.014(9) -0.022(11)
O132 0.092(11) 0.084(11) 0.051(9) 0.012(8) 0.024(8) 0.008(9)
O133 0.082(11) 0.098(12) 0.045(8) 0.021(8) 0.012(8) -0.003(9)
O134 0.103(12) 0.074(11) 0.084(11) 0.013(8) 0.044(10) 0.016(9)
O135 0.123(13) 0.079(10) 0.040(8) 0.010(7) 0.036(8) 0.000(9)
O136 0.096(11) 0.078(10) 0.050(9) -0.001(7) 0.032(8) 0.001(8)
O137 0.119(14) 0.118(14) 0.063(10) -0.003(9) 0.049(10) -0.023(11)
O138 0.131(14) 0.073(10) 0.040(8) -0.002(7) 0.028(9) 0.002(9)
O139 0.126(14) 0.063(10) 0.074(11) -0.009(8) 0.034(10) 0.020(9)
O140 0.119(14) 0.106(13) 0.047(9) -0.011(8) 0.034(9) -0.014(10)
O141 0.086(16) 0.089(16) 0.055(13) 0.000 0.022(11) 0.000
O142 0.096(12) 0.083(11) 0.049(9) 0.002(8) 0.009(8) 0.007(9)
O143 0.133(15) 0.081(11) 0.084(12) 0.016(9) 0.054(11) 0.016(10)
O144 0.113(14) 0.091(12) 0.065(10) -0.011(9) 0.032(9) 0.008(10)
O145 0.085(11) 0.100(12) 0.040(8) 0.007(8) 0.011(7) -0.015(9)
O146 0.103(18) 0.116(19) 0.058(14) 0.000 0.044(13) 0.000
O147 0.104(13) 0.081(11) 0.079(11) -0.001(9) 0.034(10) 0.009(9)
O148 0.087(13) 0.126(17) 0.108(16) 0.097(15) -0.028(11) -0.021(12)
O149 0.076(11) 0.102(13) 0.074(11) -0.001(9) 0.014(9) -0.015(9)
O150 0.080(10) 0.078(10) 0.049(8) -0.010(7) 0.013(7) 0.006(8)
O151 0.083(17) 0.15(2) 0.060(14) 0.000 0.031(13) 0.000
O152 0.134(15) 0.099(13) 0.056(10) 0.006(8) 0.040(10) 0.022(11)
O153 0.082(11) 0.082(11) 0.085(12) 0.011(9) 0.023(9) -0.005(9)
O154 0.095(13) 0.110(13) 0.068(11) -0.012(9) 0.027(9) 0.000(10)
O155 0.082(11) 0.109(13) 0.078(11) 0.020(9) 0.030(9) 0.013(10)
O156 0.137(15) 0.124(14) 0.035(8) 0.020(9) 0.032(9) 0.025(12)
O157 0.105(12) 0.082(11) 0.047(9) -0.013(7) 0.028(8) 0.007(9)
O158 0.097(13) 0.144(17) 0.064(11) -0.001(10) 0.027(10) 0.000(11)
O159 0.100(12) 0.096(12) 0.044(8) 0.013(8) 0.022(8) -0.016(9)
O160 0.107(13) 0.110(13) 0.062(10) 0.012(9) 0.050(9) -0.012(10)
O161 0.078(15) 0.094(17) 0.071(15) 0.000 0.029(12) 0.000
O162 0.111(13) 0.096(12) 0.050(9) 0.006(8) 0.026(9) 0.004(10)
O163 0.095(12) 0.110(14) 0.071(11) -0.019(9) 0.019(9) 0.033(10)
O164 0.080(11) 0.072(10) 0.076(11) 0.010(8) 0.018(8) -0.006(8)
O165 0.132(16) 0.074(12) 0.091(13) 0.024(10) -0.039(11) -0.014(11)
O166 0.081(12) 0.061(11) 0.17(2) -0.002(11) 0.038(13) -0.006(9)
O167 0.109(13) 0.089(12) 0.058(10) 0.018(8) 0.019(9) -0.018(10)
O168 0.054(9) 0.130(15) 0.084(12) -0.021(10) 0.027(8) -0.002(9)
O169 0.085(11) 0.115(13) 0.046(9) -0.026(8) 0.018(8) -0.016(9)
O170 0.105(14) 0.091(12) 0.090(12) 0.001(10) 0.042(11) -0.006(10)
O171 0.125(16) 0.143(17) 0.070(12) 0.018(11) 0.029(11) -0.037(13)
O172 0.092(11) 0.075(10) 0.064(10) 0.004(8) 0.022(8) 0.017(8)
O173 0.102(14) 0.22(2) 0.046(10) -0.001(12) 0.019(9) 0.039(14)
O174 0.101(13) 0.101(13) 0.059(10) 0.005(9) 0.022(9) -0.007(10)
O175 0.089(13) 0.100(14) 0.125(16) -0.002(11) 0.035(11) -0.015(10)
O176 0.13(2) 0.051(15) 0.15(3) 0.000 0.02(2) 0.000
O177 0.093(12) 0.074(11) 0.089(12) 0.017(9) -0.001(10) -0.019(9)
O178 0.089(12) 0.122(15) 0.083(12) 0.000(10) 0.033(10) -0.013(11)
O179 0.069(11) 0.085(12) 0.151(18) 0.022(12) 0.021(11) -0.011(9)
O180 0.063(10) 0.083(12) 0.108(13) -0.004(10) 0.008(9) 0.008(8)
O181 0.098(13) 0.081(12) 0.105(14) 0.023(10) 0.045(11) 0.008(9)
O182 0.17(2) 0.150(18) 0.067(12) -0.008(11) 0.077(13) -0.028(15)
O183 0.086(12) 0.069(11) 0.131(16) 0.008(10) 0.005(11) -0.001(9)
O184 0.068(16) 0.064(16) 0.19(3) 0.000 0.008(17) 0.000
O185 0.095(13) 0.075(12) 0.142(18) 0.010(11) 0.005(12) -0.001(10)
O186 0.065(10) 0.074(11) 0.122(15) 0.000(10) 0.006(10) -0.001(8)
O187 0.126(15) 0.095(13) 0.101(14) -0.038(11) 0.057(12) -0.038(11)
O188 0.130(16) 0.097(13) 0.067(11) 0.004(9) 0.010(11) -0.042(11)
O189 0.084(13) 0.076(13) 0.22(3) 0.037(15) 0.035(16) -0.001(10)
O190 0.100(14) 0.135(17) 0.114(15) -0.056(13) 0.033(12) -0.034(12)
O191 0.17(2) 0.17(2) 0.054(11) 0.027(11) 0.053(12) 0.047(16)
O192 0.136(18) 0.18(2) 0.109(17) 0.029(16) 0.045(14) -0.036(16)
O193 0.095(17) 0.056(14) 0.11(2) 0.000 0.025(15) 0.000
O194 0.123(16) 0.096(14) 0.117(16) -0.003(12) 0.000(13) 0.002(12)
O195 0.081(16) 0.089(17) 0.09(2) 0.000 0.014(14) 0.000
O196 0.079(12) 0.24(3) 0.107(15) -0.101(16) 0.050(11) -0.037(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
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 Mo1 O1 96.6(9) . . ?
O2 Mo1 O22 98.7(4) . . ?
O1 Mo1 O22 71.5(4) . . ?
O2 Mo1 O22 98.7(4) . 6 ?
O1 Mo1 O22 71.5(4) . 6 ?
O22 Mo1 O22 140.6(8) . 6 ?
O2 Mo1 O25 97.6(7) . . ?
O1 Mo1 O25 141.3(4) . . ?
O22 Mo1 O25 70.8(5) . . ?
O22 Mo1 O25 140.5(6) 6 . ?
O2 Mo1 O25 97.6(7) . 6 ?
O1 Mo1 O25 141.3(4) . 6 ?
O22 Mo1 O25 140.5(6) . 6 ?
O22 Mo1 O25 70.8(5) 6 6 ?
O25 Mo1 O25 71.5(7) . 6 ?
O2 Mo1 O44 180.0(9) . . ?
O1 Mo1 O44 83.3(7) . . ?
O22 Mo1 O44 81.3(4) . . ?
O22 Mo1 O44 81.3(4) 6 . ?
O25 Mo1 O44 82.4(5) . . ?
O25 Mo1 O44 82.4(5) 6 . ?
Mo81 Mo2 O120 177.6(19) . . ?
Mo81 Mo2 O8 74.8(12) . . ?
O120 Mo2 O8 103.8(8) . . ?
Mo81 Mo2 O8 74.8(12) . 6 ?
O120 Mo2 O8 103.8(8) . 6 ?
O8 Mo2 O8 101.8(10) . 6 ?
Mo81 Mo2 O56 84.7(15) . . ?
O120 Mo2 O56 97.2(8) . . ?
O8 Mo2 O56 90.3(7) . . ?
O8 Mo2 O56 152.3(8) 6 . ?
Mo81 Mo2 O56 84.7(15) . 6 ?
O120 Mo2 O56 97.3(8) . 6 ?
O8 Mo2 O56 152.3(8) . 6 ?
O8 Mo2 O56 90.3(7) 6 6 ?
O56 Mo2 O56 69.1(9) . 6 ?
Mo81 Mo2 O151 9.0(18) . . ?
O120 Mo2 O151 173.4(9) . . ?
O8 Mo2 O151 80.2(7) . . ?
O8 Mo2 O151 80.2(7) 6 . ?
O56 Mo2 O151 77.3(7) . . ?
O56 Mo2 O151 77.3(7) 6 . ?
Mo81 Mo2 K5 77.2(18) . 5_656 ?
O120 Mo2 K5 100.5(8) . 5_656 ?
O8 Mo2 K5 51.9(5) . 5_656 ?
O8 Mo2 K5 51.9(5) 6 5_656 ?
O56 Mo2 K5 141.0(5) . 5_656 ?
O56 Mo2 K5 141.0(5) 6 5_656 ?
O151 Mo2 K5 86.2(6) . 5_656 ?
O50 Mo3 O76 102.8(7) . . ?
O50 Mo3 O29 101.8(7) . . ?
O76 Mo3 O29 104.1(6) . . ?
O50 Mo3 O1 95.4(7) . . ?
O76 Mo3 O1 153.6(7) . . ?
O29 Mo3 O1 90.5(7) . . ?
O50 Mo3 O22 96.2(6) . . ?
O76 Mo3 O22 89.7(6) . . ?
O29 Mo3 O22 154.1(6) . . ?
O1 Mo3 O22 69.2(6) . . ?
O50 Mo3 O62 172.8(6) . . ?
O76 Mo3 O62 81.6(6) . . ?
O29 Mo3 O62 82.4(6) . . ?
O1 Mo3 O62 78.6(6) . . ?
O22 Mo3 O62 78.0(5) . . ?
O50 Mo3 K3 100.7(5) . . ?
O76 Mo3 K3 52.2(5) . . ?
O29 Mo3 K3 53.1(5) . . ?
O1 Mo3 K3 142.3(5) . . ?
O22 Mo3 K3 140.8(4) . . ?
O62 Mo3 K3 86.4(4) . . ?
Mo90 Mo4 O93 176.2(18) . . ?
Mo90 Mo4 O19 79.2(17) . . ?
O93 Mo4 O19 103.5(8) . . ?
Mo90 Mo4 O90 79.4(16) . . ?
O93 Mo4 O90 102.4(7) . . ?
O19 Mo4 O90 103.1(7) . . ?
Mo90 Mo4 O126 80.5(16) . . ?
O93 Mo4 O126 96.1(8) . . ?
O19 Mo4 O126 153.1(7) . . ?
O90 Mo4 O126 90.2(6) . . ?
Mo90 Mo4 O28 81.0(16) . . ?
O93 Mo4 O28 96.2(7) . . ?
O19 Mo4 O28 90.6(6) . . ?
O90 Mo4 O28 153.4(7) . . ?
O126 Mo4 O28 68.9(5) . . ?
Mo90 Mo4 O134 4.1(16) . . ?
O93 Mo4 O134 172.2(7) . . ?
O19 Mo4 O134 81.1(7) . . ?
O90 Mo4 O134 82.4(7) . . ?
O126 Mo4 O134 77.6(6) . . ?
O28 Mo4 O134 77.3(6) . . ?
Mo90 Mo4 K4 82.9(16) . . ?
O93 Mo4 K4 100.8(6) . . ?
O19 Mo4 K4 52.3(4) . . ?
O90 Mo4 K4 52.3(5) . . ?
O126 Mo4 K4 141.3(4) . . ?
O28 Mo4 K4 141.8(5) . . ?
O134 Mo4 K4 87.0(4) . . ?
O85 Mo5 O12 98.2(6) . . ?
O85 Mo5 O30 97.6(7) . . ?
O12 Mo5 O30 71.4(5) . . ?
O85 Mo5 O28 98.0(7) . . ?
O12 Mo5 O28 71.1(6) . . ?
O30 Mo5 O28 141.0(5) . . ?
O85 Mo5 O57 98.8(6) . . ?
O12 Mo5 O57 140.4(6) . . ?
O30 Mo5 O57 71.2(5) . . ?
O28 Mo5 O57 140.2(5) . . ?
O85 Mo5 O126 99.0(6) . . ?
O12 Mo5 O126 139.5(6) . . ?
O30 Mo5 O126 141.1(5) . . ?
O28 Mo5 O126 70.3(6) . . ?
O57 Mo5 O126 71.7(6) . . ?
O85 Mo5 O91 179.4(6) . . ?
O12 Mo5 O91 81.3(5) . . ?
O30 Mo5 O91 82.1(6) . . ?
O28 Mo5 O91 82.0(6) . . ?
O57 Mo5 O91 81.5(6) . . ?
O126 Mo5 O91 81.6(5) . . ?
O96 Mo6 O7 97.9(7) . . ?
O96 Mo6 O34 97.5(7) . . ?
O7 Mo6 O34 71.4(6) . . ?
O96 Mo6 O13 100.2(7) . . ?
O7 Mo6 O13 139.2(6) . . ?
O34 Mo6 O13 140.5(6) . . ?
O96 Mo6 O68 100.0(7) . . ?
O7 Mo6 O68 140.5(6) . . ?
O34 Mo6 O68 71.5(6) . . ?
O13 Mo6 O68 70.8(6) . . ?
O96 Mo6 O27 97.3(6) . . ?
O7 Mo6 O27 71.2(6) . . ?
O34 Mo6 O27 141.2(6) . . ?
O13 Mo6 O27 70.5(6) . . ?
O68 Mo6 O27 139.7(6) . . ?
O96 Mo6 O107 177.6(7) . . ?
O7 Mo6 O107 79.7(5) . . ?
O34 Mo6 O107 81.7(5) . . ?
O13 Mo6 O107 81.8(5) . . ?
O68 Mo6 O107 81.9(6) . . ?
O27 Mo6 O107 82.0(5) . . ?
O17 Mo7 O52 103.4(6) . . ?
O17 Mo7 O53 102.9(6) . . ?
O52 Mo7 O53 104.3(6) . . ?
O17 Mo7 O25 96.5(6) . . ?
O52 Mo7 O25 89.3(6) . . ?
O53 Mo7 O25 152.9(5) . . ?
O17 Mo7 O22 95.9(6) . . ?
O52 Mo7 O22 152.9(6) . . ?
O53 Mo7 O22 89.5(6) . . ?
O25 Mo7 O22 69.6(5) . . ?
O17 Mo7 O67 172.0(6) . . ?
O52 Mo7 O67 81.4(5) . . ?
O53 Mo7 O67 81.9(5) . . ?
O25 Mo7 O67 77.0(5) . . ?
O22 Mo7 O67 77.6(5) . . ?
O17 Mo7 K1 103.3(5) . . ?
O52 Mo7 K1 53.2(5) . . ?
O53 Mo7 K1 52.1(4) . . ?
O25 Mo7 K1 140.5(4) . . ?
O22 Mo7 K1 139.8(4) . . ?
O67 Mo7 K1 84.7(4) . . ?
O17 Mo7 K2 43.3(5) . . ?
O52 Mo7 K2 115.2(5) . . ?
O53 Mo7 K2 59.7(5) . . ?
O25 Mo7 K2 134.9(4) . . ?
O22 Mo7 K2 91.9(4) . . ?
O67 Mo7 K2 140.4(4) . . ?
K1 Mo7 K2 79.2(2) . . ?
Mo94 Mo8 O139 176.8(17) . . ?
Mo94 Mo8 O122 79.9(16) . . ?
O139 Mo8 O122 102.4(8) . . ?
Mo94 Mo8 O150 74.0(16) . . ?
O139 Mo8 O150 103.2(8) . . ?
O122 Mo8 O150 104.3(7) . . ?
Mo94 Mo8 O57 86.0(16) . . ?
O139 Mo8 O57 96.2(7) . . ?
O122 Mo8 O57 89.2(6) . . ?
O150 Mo8 O57 153.2(7) . . ?
Mo94 Mo8 O126 82.9(16) . . ?
O139 Mo8 O126 95.7(7) . . ?
O122 Mo8 O126 153.7(7) . . ?
O150 Mo8 O126 89.7(6) . . ?
O57 Mo8 O126 69.8(6) . . ?
Mo94 Mo8 O118 8.9(15) . . ?
O139 Mo8 O118 172.2(6) . . ?
O122 Mo8 O118 82.2(7) . . ?
O150 Mo8 O118 81.5(6) . . ?
O57 Mo8 O118 77.4(6) . . ?
O126 Mo8 O118 78.0(6) . . ?
Mo94 Mo8 K8 79.2(15) . 2_656 ?
O139 Mo8 K8 100.4(6) . 2_656 ?
O122 Mo8 K8 53.7(5) . 2_656 ?
O150 Mo8 K8 52.2(5) . 2_656 ?
O57 Mo8 K8 141.8(5) . 2_656 ?
O126 Mo8 K8 141.1(5) . 2_656 ?
O118 Mo8 K8 87.5(4) . 2_656 ?
O159 Mo9 O117 102.6(7) . . ?
O159 Mo9 O71 104.4(7) . . ?
O117 Mo9 O71 102.6(6) . . ?
O159 Mo9 O7 94.8(6) . . ?
O117 Mo9 O7 90.8(6) . . ?
O71 Mo9 O7 153.4(6) . . ?
O159 Mo9 O27 95.9(7) . . ?
O117 Mo9 O27 153.9(5) . . ?
O71 Mo9 O27 90.3(6) . . ?
O7 Mo9 O27 69.2(6) . . ?
O159 Mo9 O106 170.9(7) . . ?
O117 Mo9 O106 82.1(6) . . ?
O71 Mo9 O106 81.9(6) . . ?
O7 Mo9 O106 77.2(5) . . ?
O27 Mo9 O106 77.3(5) . . ?
O159 Mo9 K1 103.9(6) . . ?
O117 Mo9 K1 51.8(5) . . ?
O71 Mo9 K1 51.7(5) . . ?
O7 Mo9 K1 140.7(4) . . ?
O27 Mo9 K1 140.2(4) . . ?
O106 Mo9 K1 85.1(4) . . ?
Mo88 Mo10 O63 175(2) . . ?
Mo88 Mo10 O125 72.9(19) . . ?
O63 Mo10 O125 101.9(8) . . ?
Mo88 Mo10 O77 77.5(17) . . ?
O63 Mo10 O77 104.0(8) . . ?
O125 Mo10 O77 103.5(7) . . ?
Mo88 Mo10 O7 83.2(18) . . ?
O63 Mo10 O7 97.1(7) . . ?
O125 Mo10 O7 89.7(6) . . ?
O77 Mo10 O7 152.0(7) . . ?
Mo88 Mo10 O34 87.4(17) . . ?
O63 Mo10 O34 97.6(8) . . ?
O125 Mo10 O34 152.6(7) . . ?
O77 Mo10 O34 90.1(6) . . ?
O7 Mo10 O34 68.8(6) . . ?
Mo88 Mo10 O59 9.9(16) . . ?
O63 Mo10 O59 173.5(7) . . ?
O125 Mo10 O59 80.7(7) . . ?
O77 Mo10 O59 81.1(7) . . ?
O7 Mo10 O59 76.8(6) . . ?
O34 Mo10 O59 78.1(6) . . ?
Mo88 Mo10 K8 78.0(16) . . ?
O63 Mo10 K8 98.8(7) . . ?
O125 Mo10 K8 52.9(5) . . ?
O77 Mo10 K8 52.7(5) . . ?
O7 Mo10 K8 141.6(5) . . ?
O34 Mo10 K8 142.0(4) . . ?
O59 Mo10 K8 87.5(5) . . ?
O160 Mo11 O111 101.9(8) . . ?
O160 Mo11 O79 103.1(7) . . ?
O111 Mo11 O79 102.9(7) . . ?
O160 Mo11 O68 96.6(7) . . ?
O111 Mo11 O68 154.0(7) . . ?
O79 Mo11 O68 90.4(6) . . ?
O160 Mo11 O13 95.4(7) . . ?
O111 Mo11 O13 90.9(6) . . ?
O79 Mo11 O13 154.0(6) . . ?
O68 Mo11 O13 69.1(6) . . ?
O160 Mo11 O5 172.9(7) . . ?
O111 Mo11 O5 81.7(6) . . ?
O79 Mo11 O5 82.0(6) . . ?
O68 Mo11 O5 78.2(6) . . ?
O13 Mo11 O5 78.3(5) . . ?
O160 Mo11 K5 100.4(7) . . ?
O111 Mo11 K5 52.1(5) . . ?
O79 Mo11 K5 52.2(5) . . ?
O68 Mo11 K5 141.5(4) . . ?
O13 Mo11 K5 141.9(5) . . ?
O5 Mo11 K5 86.7(5) . . ?
Mo85 Mo12 O123 174.6(14) . . ?
Mo85 Mo12 O98 78.1(13) . . ?
O123 Mo12 O98 103.3(8) . . ?
Mo85 Mo12 O49 72.6(14) . . ?
O123 Mo12 O49 102.0(7) . . ?
O98 Mo12 O49 101.6(7) . . ?
Mo85 Mo12 O28 88.5(13) . . ?
O123 Mo12 O28 96.7(7) . . ?
O98 Mo12 O28 91.6(6) . . ?
O49 Mo12 O28 153.8(7) . . ?
Mo85 Mo12 O12 85.7(13) . . ?
O123 Mo12 O12 94.7(7) . . ?
O98 Mo12 O12 154.9(6) . . ?
O49 Mo12 O12 91.4(6) . . ?
O28 Mo12 O12 68.7(6) . . ?
Mo85 Mo12 O142 10.4(13) . . ?
O123 Mo12 O142 173.4(7) . . ?
O98 Mo12 O142 81.6(7) . . ?
O49 Mo12 O142 81.1(7) . . ?
O28 Mo12 O142 78.6(6) . . ?
O12 Mo12 O142 79.3(6) . . ?
Mo85 Mo12 K3 76.1(13) . . ?
O123 Mo12 K3 100.5(6) . . ?
O98 Mo12 K3 51.6(5) . . ?
O49 Mo12 K3 51.4(5) . . ?
O28 Mo12 K3 142.0(5) . . ?
O12 Mo12 K3 141.9(5) . . ?
O142 Mo12 K3 86.0(4) . . ?
O46 Mo13 O16 102.3(6) . . ?
O46 Mo13 O104 104.4(6) . . ?
O16 Mo13 O104 103.1(6) . . ?
O46 Mo13 O30 96.3(6) . . ?
O16 Mo13 O30 90.2(6) . . ?
O104 Mo13 O30 152.1(6) . . ?
O46 Mo13 O12 97.1(6) . . ?
O16 Mo13 O12 152.6(5) . . ?
O104 Mo13 O12 90.3(6) . . ?
O30 Mo13 O12 68.6(5) . . ?
O46 Mo13 O45 173.5(6) . . ?
O16 Mo13 O45 80.9(6) . . ?
O104 Mo13 O45 80.1(5) . . ?
O30 Mo13 O45 77.9(5) . . ?
O12 Mo13 O45 78.0(5) . . ?
O46 Mo13 K1 101.4(5) . . ?
O16 Mo13 K1 53.1(4) . . ?
O104 Mo13 K1 51.5(5) . . ?
O30 Mo13 K1 141.8(4) . . ?
O12 Mo13 K1 140.5(4) . . ?
O45 Mo13 K1 85.1(4) . . ?
Mo87 Mo14 O115 178.2(15) . . ?
Mo87 Mo14 O87 75.7(13) . . ?
O115 Mo14 O87 103.1(8) . . ?
Mo87 Mo14 O65 77.8(14) . . ?
O115 Mo14 O65 103.8(9) . . ?
O87 Mo14 O65 103.4(7) . . ?
Mo87 Mo14 O34 82.7(14) . . ?
O115 Mo14 O34 96.0(8) . . ?
O87 Mo14 O34 90.5(7) . . ?
O65 Mo14 O34 152.3(7) . . ?
Mo87 Mo14 O68 83.6(14) . . ?
O115 Mo14 O68 97.2(7) . . ?
O87 Mo14 O68 152.7(8) . . ?
O65 Mo14 O68 89.1(7) . . ?
O34 Mo14 O68 69.2(6) . . ?
Mo87 Mo14 O21 7.1(13) . . ?
O115 Mo14 O21 172.7(7) . . ?
O87 Mo14 O21 81.1(7) . . ?
O65 Mo14 O21 80.7(7) . . ?
O34 Mo14 O21 77.9(6) . . ?
O68 Mo14 O21 77.0(6) . . ?
Mo87 Mo14 K4 79.9(13) . 2_656 ?
O115 Mo14 K4 100.4(6) . 2_656 ?
O87 Mo14 K4 52.3(5) . 2_656 ?
O65 Mo14 K4 53.0(5) . 2_656 ?
O34 Mo14 K4 141.7(5) . 2_656 ?
O68 Mo14 K4 141.0(5) . 2_656 ?
O21 Mo14 K4 86.9(4) . 2_656 ?
Mo83 Mo15 O94 168.4(18) . . ?
Mo83 Mo15 O51 74.0(15) . . ?
O94 Mo15 O51 104.4(8) . . ?
Mo83 Mo15 O9 68.6(17) . . ?
O94 Mo15 O9 101.0(7) . . ?
O51 Mo15 O9 102.3(8) . . ?
Mo83 Mo15 O13 92.5(15) . . ?
O94 Mo15 O13 99.0(8) . . ?
O51 Mo15 O13 90.8(6) . . ?
O9 Mo15 O13 152.4(7) . . ?
Mo83 Mo15 O27 88.6(14) . . ?
O94 Mo15 O27 96.6(8) . . ?
O51 Mo15 O27 153.2(7) . . ?
O9 Mo15 O27 89.6(6) . . ?
O13 Mo15 O27 69.4(6) . . ?
Mo83 Mo15 O140 16.0(15) . . ?
O94 Mo15 O140 174.0(8) . . ?
O51 Mo15 O140 80.8(7) . . ?
O9 Mo15 O140 80.5(7) . . ?
O13 Mo15 O140 77.8(6) . . ?
O27 Mo15 O140 77.6(6) . . ?
Mo83 Mo15 K6 69.7(16) . . ?
O94 Mo15 K6 100.2(6) . . ?
O51 Mo15 K6 51.3(5) . . ?
O9 Mo15 K6 52.5(5) . . ?
O13 Mo15 K6 140.8(5) . . ?
O27 Mo15 K6 140.6(6) . . ?
O140 Mo15 K6 85.3(5) . . ?
Mo91 Mo16 O109 174.4(15) . . ?
Mo91 Mo16 O101 72.5(10) . . ?
O109 Mo16 O101 104.2(7) . . ?
Mo91 Mo16 O101 72.6(10) . 6 ?
O109 Mo16 O101 104.2(7) . 6 ?
O101 Mo16 O101 102.2(10) . 6 ?
Mo91 Mo16 O25 85.7(10) . 6 ?
O109 Mo16 O25 98.8(9) . 6 ?
O101 Mo16 O25 150.9(8) . 6 ?
O101 Mo16 O25 89.1(6) 6 6 ?
Mo91 Mo16 O25 85.7(10) . . ?
O109 Mo16 O25 98.8(9) . . ?
O101 Mo16 O25 89.1(6) . . ?
O101 Mo16 O25 150.9(8) 6 . ?
O25 Mo16 O25 69.8(8) 6 . ?
Mo91 Mo16 O102 11.1(11) . . ?
O109 Mo16 O102 174.5(10) . . ?
O101 Mo16 O102 79.1(7) . . ?
O101 Mo16 O102 79.2(7) 6 . ?
O25 Mo16 O102 76.7(6) 6 . ?
O25 Mo16 O102 76.7(6) . . ?
Mo91 Mo16 K6 72.9(12) . . ?
O109 Mo16 K6 101.5(8) . . ?
O101 Mo16 K6 52.0(5) . . ?
O101 Mo16 K6 52.0(5) 6 . ?
O25 Mo16 K6 139.4(5) 6 . ?
O25 Mo16 K6 139.4(5) . . ?
O102 Mo16 K6 84.0(6) . . ?
Mo84 Mo17 O70 172.4(14) . . ?
Mo84 Mo17 O162 71.5(13) . . ?
O70 Mo17 O162 103.2(8) . . ?
Mo84 Mo17 O157 73.3(13) . . ?
O70 Mo17 O157 103.2(8) . . ?
O162 Mo17 O157 102.1(7) . . ?
Mo84 Mo17 O136 89.6(13) . . ?
O70 Mo17 O136 97.2(7) . . ?
O162 Mo17 O136 152.4(7) . . ?
O157 Mo17 O136 91.0(6) . . ?
Mo84 Mo17 O56 88.2(13) . . ?
O70 Mo17 O56 97.3(8) . . ?
O162 Mo17 O56 89.8(7) . . ?
O157 Mo17 O56 153.1(7) . . ?
O136 Mo17 O56 69.1(6) . . ?
Mo84 Mo17 O144 14.2(12) . . ?
O70 Mo17 O144 173.4(7) . . ?
O162 Mo17 O144 80.7(7) . . ?
O157 Mo17 O144 81.0(7) . . ?
O136 Mo17 O144 77.5(6) . . ?
O56 Mo17 O144 77.2(7) . . ?
Mo84 Mo17 K4 72.8(12) . . ?
O70 Mo17 K4 99.7(6) . . ?
O162 Mo17 K4 52.6(5) . . ?
O157 Mo17 K4 51.3(5) . . ?
O136 Mo17 K4 141.3(5) . . ?
O56 Mo17 K4 141.4(5) . . ?
O144 Mo17 K4 86.9(5) . . ?
Mo93 Mo18 O121 176.0(11) . . ?
Mo93 Mo18 O113 74.8(11) . . ?
O121 Mo18 O113 103.4(8) . . ?
Mo93 Mo18 O84 76.4(10) . . ?
O121 Mo18 O84 100.8(8) . . ?
O113 Mo18 O84 103.4(7) . . ?
Mo93 Mo18 O57 86.7(10) . . ?
O121 Mo18 O57 96.2(8) . . ?
O113 Mo18 O57 153.3(7) . . ?
O84 Mo18 O57 90.4(6) . . ?
Mo93 Mo18 O30 87.1(10) . . ?
O121 Mo18 O30 96.5(7) . . ?
O113 Mo18 O30 90.0(6) . . ?
O84 Mo18 O30 154.9(7) . . ?
O57 Mo18 O30 69.6(5) . . ?
Mo93 Mo18 O114 9.8(9) . . ?
O121 Mo18 O114 174.1(7) . . ?
O113 Mo18 O114 80.8(7) . . ?
O84 Mo18 O114 82.0(7) . . ?
O57 Mo18 O114 78.6(6) . . ?
O30 Mo18 O114 79.3(6) . . ?
Mo93 Mo18 K8 77.0(9) . . ?
O121 Mo18 K8 99.0(6) . . ?
O113 Mo18 K8 53.0(5) . . ?
O84 Mo18 K8 52.0(5) . . ?
O57 Mo18 K8 141.5(5) . . ?
O30 Mo18 K8 142.3(5) . . ?
O114 Mo18 K8 86.8(5) . . ?
Mo86 Mo19 O83 179(2) . . ?
Mo86 Mo19 O136 81.3(9) . . ?
O83 Mo19 O136 98.9(5) . . ?
Mo86 Mo19 O136 81.3(9) . 6 ?
O83 Mo19 O136 98.9(5) . 6 ?
O136 Mo19 O136 140.3(8) . 6 ?
Mo86 Mo19 O56 80.4(19) . 6 ?
O83 Mo19 O56 98.9(8) . 6 ?
O136 Mo19 O56 139.5(6) . 6 ?
O136 Mo19 O56 71.1(6) 6 6 ?
Mo86 Mo19 O56 80.5(19) . . ?
O83 Mo19 O56 98.9(8) . . ?
O136 Mo19 O56 71.1(6) . . ?
O136 Mo19 O56 139.5(6) 6 . ?
O56 Mo19 O56 70.3(9) 6 . ?
Mo86 Mo19 O31 82(2) . . ?
O83 Mo19 O31 98.3(10) . . ?
O136 Mo19 O31 71.3(4) . . ?
O136 Mo19 O31 71.3(4) 6 . ?
O56 Mo19 O31 140.5(6) 6 . ?
O56 Mo19 O31 140.5(6) . . ?
Mo86 Mo19 O141 0(2) . . ?
O83 Mo19 O141 179.3(9) . . ?
O136 Mo19 O141 81.3(5) . . ?
O136 Mo19 O141 81.3(5) 6 . ?
O56 Mo19 O141 80.5(7) 6 . ?
O56 Mo19 O141 80.5(7) . . ?
O31 Mo19 O141 82.4(8) . . ?
Mo82 Mo20 O154 176.8(16) . . ?
Mo82 Mo20 O138 76.6(14) . . ?
O154 Mo20 O138 102.1(8) . . ?
Mo82 Mo20 O35 73.4(14) . . ?
O154 Mo20 O35 104.2(8) . . ?
O138 Mo20 O35 102.9(7) . . ?
Mo82 Mo20 O31 86.0(14) . . ?
O154 Mo20 O31 96.2(9) . . ?
O138 Mo20 O31 154.1(8) . . ?
O35 Mo20 O31 90.1(7) . . ?
Mo82 Mo20 O136 87.1(14) . . ?
O154 Mo20 O136 95.9(7) . . ?
O138 Mo20 O136 90.6(6) . . ?
O35 Mo20 O136 152.7(7) . . ?
O31 Mo20 O136 69.2(7) . . ?
Mo82 Mo20 O170 9.5(14) . . ?
O154 Mo20 O170 173.8(7) . . ?
O138 Mo20 O170 81.1(7) . . ?
O35 Mo20 O170 80.1(7) . . ?
O31 Mo20 O170 79.1(8) . . ?
O136 Mo20 O170 78.6(6) . . ?
Mo82 Mo20 K3 75.4(13) . . ?
O154 Mo20 K3 101.4(6) . . ?
O138 Mo20 K3 52.2(5) . . ?
O35 Mo20 K3 52.1(5) . . ?
O31 Mo20 K3 141.0(6) . . ?
O136 Mo20 K3 141.3(5) . . ?
O170 Mo20 K3 84.8(4) . . ?
O208 Mo21 O108 99.8(9) . . ?
O208 Mo21 O33 104.7(9) . . ?
O108 Mo21 O33 100.5(7) . . ?
O208 Mo21 O169 90.4(9) . . ?
O108 Mo21 O169 98.6(7) . . ?
O33 Mo21 O169 153.1(7) . . ?
O208 Mo21 O26 156.0(8) . . ?
O108 Mo21 O26 94.1(7) . . ?
O33 Mo21 O26 91.7(6) . . ?
O169 Mo21 O26 68.1(6) . . ?
O208 Mo21 O200 84.6(10) . . ?
O108 Mo21 O200 173.0(9) . . ?
O33 Mo21 O200 83.4(8) . . ?
O169 Mo21 O200 75.9(8) . . ?
O26 Mo21 O200 80.0(8) . . ?
O208 Mo21 K10 46.5(9) . . ?
O108 Mo21 K10 108.5(6) . . ?
O33 Mo21 K10 58.2(7) . . ?
O169 Mo21 K10 131.5(6) . . ?
O26 Mo21 K10 144.6(6) . . ?
O200 Mo21 K10 78.5(8) . . ?
O208 Mo21 K9 60.1(10) . . ?
O108 Mo21 K9 119.4(7) . . ?
O33 Mo21 K9 46.8(8) . . ?
O169 Mo21 K9 134.0(7) . . ?
O26 Mo21 K9 128.0(7) . . ?
O200 Mo21 K9 67.5(8) . . ?
K10 Mo21 K9 16.7(6) . . ?
O179 Mo22 O183 102.9(9) . . ?
O179 Mo22 O97 103.1(9) . . ?
O183 Mo22 O97 97.7(8) . . ?
O179 Mo22 O177 104.0(9) . . ?
O183 Mo22 O177 87.1(8) . . ?
O97 Mo22 O177 150.7(7) . . ?
O179 Mo22 O130 95.2(8) . . ?
O183 Mo22 O130 155.7(8) . . ?
O97 Mo22 O130 93.8(6) . . ?
O177 Mo22 O130 72.7(7) . . ?
O179 Mo22 O164 168.8(8) . . ?
O183 Mo22 O164 88.1(7) . . ?
O97 Mo22 O164 73.5(6) . . ?
O177 Mo22 O164 77.9(6) . . ?
O130 Mo22 O164 74.7(6) . . ?
O156 Mo23 O58 102.9(7) . . ?
O156 Mo23 O11 99.8(8) . . ?
O58 Mo23 O11 88.0(6) . . ?
O156 Mo23 O33 103.0(8) . . ?
O58 Mo23 O33 87.7(6) . . ?
O11 Mo23 O33 157.1(6) . . ?
O156 Mo23 O37 98.4(7) . . ?
O58 Mo23 O37 158.7(6) . . ?
O11 Mo23 O37 89.3(6) . . ?
O33 Mo23 O37 86.6(6) . . ?
O156 Mo23 O42 167.2(6) . . ?
O58 Mo23 O42 88.3(6) . . ?
O11 Mo23 O42 73.9(5) . . ?
O33 Mo23 O42 83.5(5) . . ?
O37 Mo23 O42 70.7(5) . . ?
O156 Mo23 K9 70.6(9) . . ?
O58 Mo23 K9 124.1(6) . . ?
O11 Mo23 K9 147.6(7) . . ?
O33 Mo23 K9 44.7(7) . . ?
O37 Mo23 K9 62.7(6) . . ?
O42 Mo23 K9 108.5(7) . . ?
O165 Mo24 O198 101.1(10) . . ?
O165 Mo24 O197 102.6(8) . . ?
O198 Mo24 O197 68.1(9) . . ?
O165 Mo24 O86 94.9(8) . . ?
O198 Mo24 O86 72.1(8) . . ?
O197 Mo24 O86 138.8(7) . . ?
O165 Mo24 O177 92.0(9) . . ?
O198 Mo24 O177 142.2(8) . . ?
O197 Mo24 O177 74.4(7) . . ?
O86 Mo24 O177 142.4(6) . . ?
O165 Mo24 O130 98.1(8) . . ?
O198 Mo24 O130 140.1(8) . . ?
O197 Mo24 O130 139.9(7) . . ?
O86 Mo24 O130 71.6(6) . . ?
O177 Mo24 O130 70.9(6) . . ?
O165 Mo24 O167 171.6(8) . . ?
O198 Mo24 O167 86.5(8) . . ?
O197 Mo24 O167 83.4(7) . . ?
O86 Mo24 O167 83.9(6) . . ?
O177 Mo24 O167 84.1(7) . . ?
O130 Mo24 O167 73.6(6) . . ?
O165 Mo24 Mo54 96.1(7) . . ?
O198 Mo24 Mo54 40.6(7) . . ?
O197 Mo24 Mo54 29.4(6) . . ?
O86 Mo24 Mo54 112.7(5) . . ?
O177 Mo24 Mo54 103.2(5) . . ?
O130 Mo24 Mo54 164.8(5) . . ?
O167 Mo24 Mo54 92.0(4) . . ?
O147 Mo25 O124 105.0(7) . . ?
O147 Mo25 O97 100.3(8) . . ?
O124 Mo25 O97 88.5(7) . . ?
O147 Mo25 O172 101.8(7) . . ?
O124 Mo25 O172 86.7(7) . . ?
O97 Mo25 O172 157.8(7) . . ?
O147 Mo25 O32 98.3(7) . . ?
O124 Mo25 O32 156.7(6) . . ?
O97 Mo25 O32 88.3(6) . . ?
O172 Mo25 O32 87.6(6) . . ?
O147 Mo25 O164 167.3(7) . . ?
O124 Mo25 O164 86.8(6) . . ?
O97 Mo25 O164 75.0(6) . . ?
O172 Mo25 O164 83.2(6) . . ?
O32 Mo25 O164 70.1(6) . . ?
O147 Mo25 K7 71.6(6) . . ?
O124 Mo25 K7 122.4(5) . . ?
O97 Mo25 K7 149.0(5) . . ?
O172 Mo25 K7 42.3(5) . . ?
O32 Mo25 K7 64.3(5) . . ?
O164 Mo25 K7 106.2(5) . . ?
O182 Mo26 O78 103.3(9) . . ?
O182 Mo26 O152 103.6(8) . 2_655 ?
O78 Mo26 O152 99.4(8) . 2_655 ?
O182 Mo26 O88 103.6(9) . 2_655 ?
O78 Mo26 O88 149.5(6) . 2_655 ?
O152 Mo26 O88 87.8(7) 2_655 2_655 ?
O182 Mo26 O99 94.6(8) . . ?
O78 Mo26 O99 91.7(6) . . ?
O152 Mo26 O99 155.8(7) 2_655 . ?
O88 Mo26 O99 72.2(6) 2_655 . ?
O182 Mo26 O80 168.7(7) . . ?
O78 Mo26 O80 72.3(6) . . ?
O152 Mo26 O80 87.5(6) 2_655 . ?
O88 Mo26 O80 78.6(5) 2_655 . ?
O99 Mo26 O80 75.4(5) . . ?
O143 Mo27 O175 104.8(9) . . ?
O143 Mo27 O4 99.8(7) . . ?
O175 Mo27 O4 105.6(8) . . ?
O143 Mo27 O127 96.8(7) . . ?
O175 Mo27 O127 88.6(8) . . ?
O4 Mo27 O127 154.4(6) . . ?
O143 Mo27 O40 94.3(7) . . ?
O175 Mo27 O40 151.9(8) . . ?
O4 Mo27 O40 90.8(6) . . ?
O127 Mo27 O40 68.5(6) . . ?
O143 Mo27 O69 170.8(8) . . ?
O175 Mo27 O69 84.4(8) . . ?
O4 Mo27 O69 78.7(6) . . ?
O127 Mo27 O69 81.9(6) . . ?
O40 Mo27 O69 76.6(5) . . ?
O143 Mo27 K7 115.1(6) . . ?
O175 Mo27 K7 53.0(7) . . ?
O4 Mo27 K7 52.9(5) . . ?
O127 Mo27 K7 134.1(5) . . ?
O40 Mo27 K7 135.1(4) . . ?
O69 Mo27 K7 71.4(5) . . ?
O176 Mo28 O186 99.7(10) . . ?
O176 Mo28 O186 99.7(10) . 6_565 ?
O186 Mo28 O186 71.9(10) . 6_565 ?
O176 Mo28 O61 94.7(6) . 6_565 ?
O186 Mo28 O61 142.4(7) . 6_565 ?
O186 Mo28 O61 71.6(7) 6_565 6_565 ?
O176 Mo28 O61 94.7(6) . . ?
O186 Mo28 O61 71.5(7) . . ?
O186 Mo28 O61 142.4(7) 6_565 . ?
O61 Mo28 O61 141.7(9) 6_565 . ?
O176 Mo28 O193 100.4(13) . . ?
O186 Mo28 O193 138.5(6) . . ?
O186 Mo28 O193 138.5(6) 6_565 . ?
O61 Mo28 O193 70.9(5) 6_565 . ?
O61 Mo28 O193 70.9(5) . . ?
O176 Mo28 O89 173.1(12) . . ?
O186 Mo28 O89 85.9(7) . . ?
O186 Mo28 O89 85.9(7) 6_565 . ?
O61 Mo28 O89 83.2(5) 6_565 . ?
O61 Mo28 O89 83.2(5) . . ?
O193 Mo28 O89 72.7(9) . . ?
O176 Mo28 Mo95 139.5(13) . . ?
O186 Mo28 Mo95 112.7(8) . . ?
O186 Mo28 Mo95 112.7(8) 6_565 . ?
O61 Mo28 Mo95 74.4(5) 6_565 . ?
O61 Mo28 Mo95 74.4(5) . . ?
O193 Mo28 Mo95 39.1(11) . . ?
O89 Mo28 Mo95 33.6(10) . . ?
Mo95 Mo29 O195 170(3) . . ?
Mo95 Mo29 O89 81(2) . . ?
O195 Mo29 O89 108.8(16) . . ?
Mo95 Mo29 O180 70.0(10) . . ?
O195 Mo29 O180 108.1(8) . . ?
O89 Mo29 O180 95.5(6) . . ?
Mo95 Mo29 O180 70.0(10) . 6_565 ?
O195 Mo29 O180 108.1(8) . 6_565 ?
O89 Mo29 O180 95.5(6) . 6_565 ?
O180 Mo29 O180 136.1(16) . 6_565 ?
Mo95 Mo29 O184 70(3) . . ?
O195 Mo29 O184 100.4(13) . . ?
O89 Mo29 O184 150.8(19) . . ?
O180 Mo29 O184 74.9(7) . . ?
O180 Mo29 O184 74.9(7) 6_565 . ?
O181 Mo30 O185 103.6(10) . . ?
O181 Mo30 O172 100.0(7) . . ?
O185 Mo30 O172 104.5(8) . . ?
O181 Mo30 O186 96.2(8) . . ?
O185 Mo30 O186 91.2(8) . . ?
O172 Mo30 O186 154.0(7) . . ?
O181 Mo30 O61 92.6(7) . . ?
O185 Mo30 O61 155.6(8) . . ?
O172 Mo30 O61 90.3(6) . . ?
O186 Mo30 O61 68.7(6) . . ?
O181 Mo30 O194 172.7(8) . . ?
O185 Mo30 O194 83.6(9) . . ?
O172 Mo30 O194 79.2(7) . . ?
O186 Mo30 O194 82.1(7) . . ?
O61 Mo30 O194 80.1(7) . . ?
O181 Mo30 K7 119.7(6) . . ?
O185 Mo30 K7 55.6(7) . . ?
O172 Mo30 K7 50.3(5) . . ?
O186 Mo30 K7 134.3(5) . . ?
O61 Mo30 K7 130.3(5) . . ?
O194 Mo30 K7 65.4(6) . . ?
O131 Mo31 O36 103.1(7) . . ?
O131 Mo31 O103 105.2(8) . . ?
O36 Mo31 O103 97.0(6) . . ?
O131 Mo31 O43 104.7(8) . . ?
O36 Mo31 O43 99.5(7) . . ?
O103 Mo31 O43 141.3(6) . . ?
O131 Mo31 O73 98.4(7) . . ?
O36 Mo31 O73 158.4(6) . . ?
O103 Mo31 O73 76.7(6) . . ?
O43 Mo31 O73 75.2(7) . . ?
O131 Mo31 O54 177.2(7) . . ?
O36 Mo31 O54 74.1(5) . . ?
O103 Mo31 O54 76.0(5) . . ?
O43 Mo31 O54 75.3(5) . . ?
O73 Mo31 O54 84.3(5) . . ?
O190 Mo32 O168 103.8(9) . . ?
O190 Mo32 O74 104.8(9) . . ?
O168 Mo32 O74 97.6(7) . . ?
O190 Mo32 O82 92.4(9) . . ?
O168 Mo32 O82 92.8(7) . . ?
O74 Mo32 O82 157.0(8) . . ?
O190 Mo32 O64 157.3(8) . . ?
O168 Mo32 O64 90.4(7) . . ?
O74 Mo32 O64 90.5(7) . . ?
O82 Mo32 O64 68.9(6) . . ?
O190 Mo32 O39 85.6(10) . . ?
O168 Mo32 O39 169.4(8) . . ?
O74 Mo32 O39 84.5(7) . . ?
O82 Mo32 O39 81.7(7) . . ?
O64 Mo32 O39 79.2(7) . . ?
O191 Mo33 O152 105.1(8) . . ?
O191 Mo33 O78 100.9(10) . . ?
O152 Mo33 O78 90.4(7) . . ?
O191 Mo33 O92 101.8(10) . . ?
O152 Mo33 O92 86.5(7) . . ?
O78 Mo33 O92 157.1(6) . . ?
O191 Mo33 O37 97.6(8) . . ?
O152 Mo33 O37 157.3(7) . . ?
O78 Mo33 O37 86.8(7) . . ?
O92 Mo33 O37 87.4(7) . . ?
O191 Mo33 O80 167.7(8) . . ?
O152 Mo33 O80 86.3(6) . . ?
O78 Mo33 O80 73.9(6) . . ?
O92 Mo33 O80 83.3(6) . . ?
O37 Mo33 O80 71.2(5) . . ?
O191 Mo33 K9 68.8(10) . . ?
O152 Mo33 K9 124.9(8) . . ?
O78 Mo33 K9 144.5(7) . . ?
O92 Mo33 K9 46.0(7) . . ?
O37 Mo33 K9 62.4(8) . . ?
O80 Mo33 K9 108.8(7) . . ?
O75 Mo34 O55 105.2(7) . . ?
O75 Mo34 O20 99.8(7) . . ?
O55 Mo34 O20 88.9(6) . . ?
O75 Mo34 O74 102.4(7) . 2_655 ?
O55 Mo34 O74 86.8(6) . 2_655 ?
O20 Mo34 O74 157.7(6) . 2_655 ?
O75 Mo34 O73 99.2(7) . . ?
O55 Mo34 O73 155.6(6) . . ?
O20 Mo34 O73 88.2(6) . . ?
O74 Mo34 O73 86.7(6) 2_655 . ?
O75 Mo34 O43 166.9(7) . . ?
O55 Mo34 O43 86.6(6) . . ?
O20 Mo34 O43 74.3(6) . . ?
O74 Mo34 O43 83.6(6) 2_655 . ?
O73 Mo34 O43 69.3(6) . . ?
O189 Mo35 O124 102.5(8) . . ?
O189 Mo35 O166 103.8(10) . . ?
O124 Mo35 O166 98.6(7) . . ?
O189 Mo35 O61 103.8(9) . . ?
O124 Mo35 O61 87.9(7) . . ?
O166 Mo35 O61 149.4(8) . . ?
O189 Mo35 O193 95.7(10) . . ?
O124 Mo35 O193 155.6(9) . . ?
O166 Mo35 O193 92.6(8) . . ?
O61 Mo35 O193 71.9(8) . . ?
O189 Mo35 O180 169.5(8) . . ?
O124 Mo35 O180 87.9(6) . . ?
O166 Mo35 O180 72.7(8) . . ?
O61 Mo35 O180 77.7(6) . . ?
O193 Mo35 O180 74.7(8) . . ?
O189 Mo35 Mo89 122.4(8) . . ?
O124 Mo35 Mo89 90.7(6) . . ?
O166 Mo35 Mo89 18.8(8) . . ?
O61 Mo35 Mo89 132.8(6) . . ?
O193 Mo35 Mo89 93.2(7) . . ?
O180 Mo35 Mo89 55.1(5) . . ?
O189 Mo35 Mo95 133.4(9) . . ?
O124 Mo35 Mo95 123.6(8) . . ?
O166 Mo35 Mo95 77.5(7) . . ?
O61 Mo35 Mo95 74.1(6) . . ?
O193 Mo35 Mo95 38.4(10) . . ?
O180 Mo35 Mo95 36.6(8) . . ?
Mo89 Mo35 Mo95 67.8(5) . . ?
O148 Mo36 O188 100.2(10) . . ?
O148 Mo36 O207 107.1(10) . . ?
O188 Mo36 O207 102.3(10) . . ?
O148 Mo36 O197 152.4(9) . . ?
O188 Mo36 O197 97.6(9) . . ?
O207 Mo36 O197 89.4(10) . . ?
O148 Mo36 O177 86.4(8) . . ?
O188 Mo36 O177 94.4(7) . . ?
O207 Mo36 O177 156.0(10) . . ?
O197 Mo36 O177 71.2(8) . . ?
O148 Mo36 O201 82.4(9) . . ?
O188 Mo36 O201 170.9(9) . . ?
O207 Mo36 O201 85.1(10) . . ?
O197 Mo36 O201 76.9(8) . . ?
O177 Mo36 O201 77.0(8) . . ?
O173 Mo37 O206 99.2(8) . . ?
O173 Mo37 O82 102.7(10) . . ?
O206 Mo37 O82 72.3(7) . . ?
O173 Mo37 O64 92.7(8) . . ?
O206 Mo37 O64 143.6(8) . . ?
O82 Mo37 O64 71.5(7) . . ?
O173 Mo37 O88 94.2(9) . . ?
O206 Mo37 O88 71.1(7) . . ?
O82 Mo37 O88 141.7(7) . . ?
O64 Mo37 O88 142.3(7) . . ?
O173 Mo37 O99 99.2(9) . 2_655 ?
O206 Mo37 O99 138.7(7) . 2_655 ?
O82 Mo37 O99 137.5(6) . 2_655 ?
O64 Mo37 O99 71.4(6) . 2_655 ?
O88 Mo37 O99 70.9(6) . 2_655 ?
O173 Mo37 O133 174.0(9) . 2_655 ?
O206 Mo37 O133 85.9(7) . 2_655 ?
O82 Mo37 O133 81.9(7) . 2_655 ?
O64 Mo37 O133 85.1(6) . 2_655 ?
O88 Mo37 O133 84.2(6) . 2_655 ?
O99 Mo37 O133 74.8(6) 2_655 2_655 ?
O173 Mo37 Mo53 92.4(8) . . ?
O206 Mo37 Mo53 33.4(6) . . ?
O82 Mo37 Mo53 41.7(5) . . ?
O64 Mo37 Mo53 112.4(6) . . ?
O88 Mo37 Mo53 104.2(5) . . ?
O99 Mo37 Mo53 167.7(5) 2_655 . ?
O133 Mo37 Mo53 93.6(4) 2_655 . ?
Mo89 Mo38 O202 73.5(13) . . ?
Mo89 Mo38 O183 79.1(10) . . ?
O202 Mo38 O183 102.3(10) . . ?
Mo89 Mo38 O184 100.1(14) . . ?
O202 Mo38 O184 98.4(11) . . ?
O183 Mo38 O184 158.1(8) . . ?
Mo89 Mo38 O166 23.6(9) . . ?
O202 Mo38 O166 94.5(10) . . ?
O183 Mo38 O166 84.5(8) . . ?
O184 Mo38 O166 86.7(11) . . ?
Mo89 Mo38 O148 166.3(10) . . ?
O202 Mo38 O148 108.5(10) . . ?
O183 Mo38 O148 87.2(9) . . ?
O184 Mo38 O148 93.1(12) . . ?
O166 Mo38 O148 156.8(7) . . ?
Mo89 Mo38 O180 96.3(10) . . ?
O202 Mo38 O180 164.0(10) . . ?
O183 Mo38 O180 87.4(7) . . ?
O184 Mo38 O180 70.8(8) . . ?
O166 Mo38 O180 73.6(7) . . ?
O148 Mo38 O180 84.4(7) . . ?
Mo89 Mo38 Mo95 96.2(13) . . ?
O202 Mo38 Mo95 131.9(9) . . ?
O183 Mo38 Mo95 122.2(6) . . ?
O184 Mo38 Mo95 35.9(7) . . ?
O166 Mo38 Mo95 74.1(11) . . ?
O148 Mo38 Mo95 92.3(11) . . ?
O180 Mo38 Mo95 35.3(4) . . ?
Mo92 Mo39 O192 173(3) . . ?
Mo92 Mo39 O187 82(2) . . ?
O192 Mo39 O187 104.2(13) . . ?
Mo92 Mo39 O95 72(2) . . ?
O192 Mo39 O95 103.0(11) . . ?
O187 Mo39 O95 105.1(8) . . ?
Mo92 Mo39 O127 86.7(18) . . ?
O192 Mo39 O127 96.7(10) . . ?
O187 Mo39 O127 89.9(7) . . ?
O95 Mo39 O127 151.2(11) . . ?
Mo92 Mo39 O169 79(2) . . ?
O192 Mo39 O169 96.2(10) . . ?
O187 Mo39 O169 152.5(9) . . ?
O95 Mo39 O169 87.7(8) . . ?
O127 Mo39 O169 69.2(6) . . ?
Mo92 Mo39 O174 6.9(18) . . ?
O192 Mo39 O174 173.2(10) . . ?
O187 Mo39 O174 81.7(9) . . ?
O95 Mo39 O174 78.3(10) . . ?
O127 Mo39 O174 79.8(7) . . ?
O169 Mo39 O174 77.2(7) . . ?
O41 Mo40 O196 103.8(10) . . ?
O41 Mo40 O92 101.2(7) . . ?
O196 Mo40 O92 106.0(9) . . ?
O41 Mo40 O206 97.1(8) . . ?
O196 Mo40 O206 88.7(8) . . ?
O92 Mo40 O206 152.9(8) . . ?
O41 Mo40 O88 93.5(7) . . ?
O196 Mo40 O88 153.0(7) . . ?
O92 Mo40 O88 90.4(7) . . ?
O206 Mo40 O88 68.5(7) . . ?
O41 Mo40 O199 171.6(8) . . ?
O196 Mo40 O199 84.3(10) . . ?
O92 Mo40 O199 78.3(7) . . ?
O206 Mo40 O199 80.8(8) . . ?
O88 Mo40 O199 78.1(7) . . ?
O41 Mo40 K10 111.6(7) . . ?
O196 Mo40 K10 47.2(9) . . ?
O92 Mo40 K10 58.8(6) . . ?
O206 Mo40 K10 131.0(7) . . ?
O88 Mo40 K10 142.6(7) . . ?
O199 Mo40 K10 75.4(7) . . ?
O41 Mo40 K9 120.7(8) . . ?
O196 Mo40 K9 60.7(10) . . ?
O92 Mo40 K9 46.7(7) . . ?
O206 Mo40 K9 134.8(8) . . ?
O88 Mo40 K9 126.6(8) . . ?
O199 Mo40 K9 65.0(9) . . ?
K10 Mo40 K9 16.0(6) . . ?
O209 Mo41 O209 107.8(19) 6_565 . ?
O209 Mo41 O205 96.5(13) 6_565 . ?
O209 Mo41 O205 96.5(13) . . ?
O209 Mo41 O186 91.0(10) 6_565 6_565 ?
O209 Mo41 O186 158.5(11) . 6_565 ?
O205 Mo41 O186 91.5(13) . 6_565 ?
O209 Mo41 O186 158.5(11) 6_565 . ?
O209 Mo41 O186 91.0(10) . . ?
O205 Mo41 O186 91.5(13) . . ?
O186 Mo41 O186 68.8(9) 6_565 . ?
O209 Mo41 O204 88.2(12) 6_565 . ?
O209 Mo41 O204 88.2(12) . . ?
O205 Mo41 O204 171.9(18) . . ?
O186 Mo41 O204 81.8(11) 6_565 . ?
O186 Mo41 O204 81.8(11) . . ?
O171 Mo42 O203 103.2(10) . . ?
O171 Mo42 O145 101.6(9) . . ?
O203 Mo42 O145 104.0(9) . . ?
O171 Mo42 O198 97.0(10) . . ?
O203 Mo42 O198 93.6(10) . . ?
O145 Mo42 O198 150.5(8) . . ?
O171 Mo42 O86 92.9(8) . . ?
O203 Mo42 O86 156.6(9) . . ?
O145 Mo42 O86 88.9(6) . . ?
O198 Mo42 O86 67.4(7) . . ?
O171 Mo42 O60 171.2(9) . . ?
O203 Mo42 O60 84.4(9) . . ?
O145 Mo42 O60 80.4(7) . . ?
O198 Mo42 O60 77.9(8) . . ?
O86 Mo42 O60 78.5(7) . . ?
O112 Mo43 O133 103.1(7) . . ?
O112 Mo43 O42 106.9(7) . . ?
O133 Mo43 O42 99.0(6) . . ?
O112 Mo43 O80 105.3(7) . . ?
O133 Mo43 O80 96.2(7) . . ?
O42 Mo43 O80 139.9(6) . . ?
O112 Mo43 O37 97.5(7) . . ?
O133 Mo43 O37 159.2(7) . . ?
O42 Mo43 O37 76.7(6) . . ?
O80 Mo43 O37 76.1(6) . . ?
O112 Mo43 O99 177.0(6) . . ?
O133 Mo43 O99 73.9(6) . . ?
O42 Mo43 O99 74.3(5) . . ?
O80 Mo43 O99 74.7(5) . . ?
O37 Mo43 O99 85.4(6) . . ?
O137 Mo44 O55 103.1(8) . . ?
O137 Mo44 O11 103.3(8) . . ?
O55 Mo44 O11 98.2(7) . . ?
O137 Mo44 O64 102.8(8) . 2_655 ?
O55 Mo44 O64 88.3(7) . 2_655 ?
O11 Mo44 O64 150.9(6) . 2_655 ?
O137 Mo44 O99 94.0(7) . . ?
O55 Mo44 O99 156.5(7) . . ?
O11 Mo44 O99 93.3(6) . . ?
O64 Mo44 O99 72.1(6) 2_655 . ?
O137 Mo44 O42 168.0(7) . . ?
O55 Mo44 O42 88.8(6) . . ?
O11 Mo44 O42 73.3(6) . . ?
O64 Mo44 O42 78.6(5) 2_655 . ?
O99 Mo44 O42 74.9(5) . . ?
O128 Mo45 O167 104.3(7) . . ?
O128 Mo45 O164 105.2(8) . . ?
O167 Mo45 O164 97.6(8) . . ?
O128 Mo45 O38 105.6(8) . . ?
O167 Mo45 O38 96.8(7) . . ?
O164 Mo45 O38 141.3(6) . . ?
O128 Mo45 O32 98.7(6) . . ?
O167 Mo45 O32 157.0(7) . . ?
O164 Mo45 O32 76.6(6) . . ?
O38 Mo45 O32 76.3(6) . . ?
O128 Mo45 O130 176.9(6) . . ?
O167 Mo45 O130 72.6(6) . . ?
O164 Mo45 O130 75.3(6) . . ?
O38 Mo45 O130 75.2(6) . . ?
O32 Mo45 O130 84.4(5) . . ?
O149 Mo46 O10 105.5(8) . . ?
O149 Mo46 O145 103.1(7) . . ?
O10 Mo46 O145 86.9(6) . . ?
O149 Mo46 O3 98.7(7) . . ?
O10 Mo46 O3 90.3(6) . . ?
O145 Mo46 O3 158.0(6) . . ?
O149 Mo46 O73 98.5(7) . . ?
O10 Mo46 O73 155.9(6) . . ?
O145 Mo46 O73 85.6(7) . . ?
O3 Mo46 O73 88.1(6) . . ?
O149 Mo46 O103 166.4(7) . . ?
O10 Mo46 O103 86.7(6) . . ?
O145 Mo46 O103 83.2(5) . . ?
O3 Mo46 O103 74.9(5) . . ?
O73 Mo46 O103 69.7(6) . . ?
O153 Mo47 O10 104.3(7) . . ?
O153 Mo47 O18 103.2(7) . . ?
O10 Mo47 O18 98.3(6) . . ?
O153 Mo47 O86 105.5(7) . . ?
O10 Mo47 O86 86.7(7) . . ?
O18 Mo47 O86 148.6(6) . . ?
O153 Mo47 O130 95.9(7) . . ?
O10 Mo47 O130 154.3(7) . . ?
O18 Mo47 O130 92.2(6) . . ?
O86 Mo47 O130 72.5(7) . . ?
O153 Mo47 O38 168.2(7) . . ?
O10 Mo47 O38 87.1(6) . . ?
O18 Mo47 O38 71.8(5) . . ?
O86 Mo47 O38 77.6(5) . . ?
O130 Mo47 O38 73.9(6) . . ?
O132 Mo48 O18 99.6(7) . . ?
O132 Mo48 O6 103.2(7) . . ?
O18 Mo48 O6 89.5(6) . . ?
O132 Mo48 O4 102.4(7) . . ?
O18 Mo48 O4 158.0(6) . . ?
O6 Mo48 O4 87.0(6) . . ?
O132 Mo48 O32 99.4(7) . . ?
O18 Mo48 O32 89.1(6) . . ?
O6 Mo48 O32 157.3(6) . . ?
O4 Mo48 O32 85.8(6) . . ?
O132 Mo48 O38 168.3(7) . . ?
O18 Mo48 O38 74.9(6) . . ?
O6 Mo48 O38 87.3(6) . . ?
O4 Mo48 O38 83.3(5) . . ?
O32 Mo48 O38 70.5(5) . . ?
O48 Mo49 O169 102.3(7) . . ?
O48 Mo49 O40 94.7(6) . . ?
O169 Mo49 O40 141.9(6) . . ?
O48 Mo49 O127 99.0(6) . . ?
O169 Mo49 O127 72.1(6) . . ?
O40 Mo49 O127 71.7(6) . . ?
O48 Mo49 O26 93.9(6) . . ?
O169 Mo49 O26 70.4(6) . . ?
O40 Mo49 O26 142.5(6) . . ?
O127 Mo49 O26 142.1(6) . . ?
O48 Mo49 O54 96.6(6) . . ?
O169 Mo49 O54 138.3(5) . . ?
O40 Mo49 O54 71.3(6) . . ?
O127 Mo49 O54 140.8(6) . . ?
O26 Mo49 O54 71.5(6) . . ?
O48 Mo49 O36 170.4(6) . . ?
O169 Mo49 O36 85.5(6) . . ?
O40 Mo49 O36 82.1(5) . . ?
O127 Mo49 O36 88.7(6) . . ?
O26 Mo49 O36 83.4(5) . . ?
O54 Mo49 O36 73.8(5) . . ?
O135 Mo50 O58 104.2(7) . . ?
O135 Mo50 O20 102.4(7) . . ?
O58 Mo50 O20 98.6(7) . . ?
O135 Mo50 O26 103.3(7) . . ?
O58 Mo50 O26 88.4(6) . . ?
O20 Mo50 O26 150.8(6) . . ?
O135 Mo50 O54 93.5(6) . . ?
O58 Mo50 O54 156.4(6) . . ?
O20 Mo50 O54 92.7(6) . . ?
O26 Mo50 O54 72.2(6) . . ?
O135 Mo50 O43 166.8(7) . . ?
O58 Mo50 O43 89.0(6) . . ?
O20 Mo50 O43 74.4(6) . . ?
O26 Mo50 O43 77.4(5) . . ?
O54 Mo50 O43 74.1(5) . . ?
O135 Mo50 K2 62.8(6) . . ?
O58 Mo50 K2 125.1(5) . . ?
O20 Mo50 K2 44.2(4) . . ?
O26 Mo50 K2 145.2(4) . . ?
O54 Mo50 K2 76.9(4) . . ?
O43 Mo50 K2 109.1(5) . . ?
O14 Mo51 O6 103.4(6) . . ?
O14 Mo51 O3 101.5(7) . . ?
O6 Mo51 O3 99.1(6) . . ?
O14 Mo51 O40 102.6(6) . . ?
O6 Mo51 O40 88.9(6) . . ?
O3 Mo51 O40 152.0(5) . . ?
O14 Mo51 O54 94.1(6) . . ?
O6 Mo51 O54 156.6(6) . . ?
O3 Mo51 O54 92.3(6) . . ?
O40 Mo51 O54 72.0(6) . . ?
O14 Mo51 O103 167.6(6) . . ?
O6 Mo51 O103 88.9(6) . . ?
O3 Mo51 O103 75.1(5) . . ?
O40 Mo51 O103 78.3(5) . . ?
O54 Mo51 O103 74.3(5) . . ?
O14 Mo51 K2 62.5(5) . . ?
O6 Mo51 K2 121.5(5) . . ?
O3 Mo51 K2 42.1(5) . . ?
O40 Mo51 K2 147.7(5) . . ?
O54 Mo51 K2 80.3(4) . . ?
O103 Mo51 K2 110.2(4) . . ?
Mo53 Mo52 O215 98(2) . . ?
Mo53 Mo52 O252 128.5(15) . . ?
O215 Mo52 O252 132(2) . . ?
Mo53 Mo52 O256 130.3(18) . . ?
O215 Mo52 O256 33.0(18) . . ?
O252 Mo52 O256 99.2(17) . . ?
Mo53 Mo52 O212 74.7(13) . . ?
O215 Mo52 O212 102.4(19) . . ?
O252 Mo52 O212 100.8(14) . . ?
O256 Mo52 O212 113.1(16) . . ?
Mo53 Mo52 O211 47.2(17) . . ?
O215 Mo52 O211 51(2) . . ?
O252 Mo52 O211 175.0(18) . . ?
O256 Mo52 O211 84.4(18) . . ?
O212 Mo52 O211 80.8(16) . . ?
Mo53 Mo52 O82 71.1(10) . . ?
O215 Mo52 O82 92.0(17) . . ?
O252 Mo52 O82 92.8(12) . . ?
O256 Mo52 O82 96.7(14) . . ?
O212 Mo52 O82 144.3(12) . . ?
O211 Mo52 O82 83.3(14) . . ?
Mo53 Mo52 O206 43.2(10) . . ?
O215 Mo52 O206 138.7(19) . . ?
O252 Mo52 O206 85.3(12) . . ?
O256 Mo52 O206 162.1(14) . . ?
O212 Mo52 O206 82.6(11) . . ?
O211 Mo52 O206 90.2(15) . . ?
O82 Mo52 O206 65.7(7) . . ?
Mo52 Mo53 O211 106(2) . . ?
Mo52 Mo53 O206 115.7(14) . . ?
O211 Mo53 O206 137(2) . . ?
Mo52 Mo53 O212 77.2(13) . . ?
O211 Mo53 O212 95(2) . . ?
O206 Mo53 O212 100.4(13) . . ?
Mo52 Mo53 O215 53.5(17) . . ?
O211 Mo53 O215 53(2) . . ?
O206 Mo53 O215 162.4(17) . . ?
O212 Mo53 O215 90.8(17) . . ?
Mo52 Mo53 O214 138.6(18) . . ?
O211 Mo53 O214 33.1(18) . . ?
O206 Mo53 O214 104.4(16) . . ?
O212 Mo53 O214 106.1(16) . . ?
O215 Mo53 O214 85.2(19) . . ?
Mo52 Mo53 O82 83.7(10) . . ?
O211 Mo53 O82 99.9(18) . . ?
O206 Mo53 O82 78.8(9) . . ?
O212 Mo53 O82 158.4(14) . . ?
O215 Mo53 O82 85.8(15) . . ?
O214 Mo53 O82 94.9(14) . . ?
Mo52 Mo53 O252 34.7(11) . . ?
O211 Mo53 O252 141(2) . . ?
O206 Mo53 O252 81.1(11) . . ?
O212 Mo53 O252 80.5(13) . . ?
O215 Mo53 O252 87.5(17) . . ?
O214 Mo53 O252 170.2(16) . . ?
O82 Mo53 O252 78.0(10) . . ?
Mo52 Mo53 O256 33.7(12) . . ?
O211 Mo53 O256 74(2) . . ?
O206 Mo53 O256 145.1(13) . . ?
O212 Mo53 O256 88.8(14) . . ?
O215 Mo53 O256 20.3(16) . . ?
O214 Mo53 O256 105.2(17) . . ?
O82 Mo53 O256 80.7(11) . . ?
O252 Mo53 O256 67.2(13) . . ?
Mo52 Mo53 Mo37 113.8(9) . . ?
O211 Mo53 Mo37 115.9(19) . . ?
O206 Mo53 Mo37 40.0(7) . . ?
O212 Mo53 Mo37 140.3(11) . . ?
O215 Mo53 Mo37 127.0(14) . . ?
O214 Mo53 Mo37 90.2(13) . . ?
O82 Mo53 Mo37 42.0(6) . . ?
O252 Mo53 Mo37 89.0(8) . . ?
O256 Mo53 Mo37 122.1(10) . . ?
Mo55 Mo54 O220 21.2(10) . . ?
Mo55 Mo54 O216 110.9(19) . . ?
O220 Mo54 O216 99.8(16) . . ?
Mo55 Mo54 O197 123.8(14) . . ?
O220 Mo54 O197 111.8(10) . . ?
O216 Mo54 O197 102.1(16) . . ?
Mo55 Mo54 O217 52.9(17) . . ?
O220 Mo54 O217 71.9(15) . . ?
O216 Mo54 O217 101.9(19) . . ?
O197 Mo54 O217 154.5(16) . . ?
Mo55 Mo54 O221 84(2) . . ?
O220 Mo54 O221 69(2) . . ?
O216 Mo54 O221 32.5(19) . . ?
O197 Mo54 O221 105(2) . . ?
O217 Mo54 O221 100(2) . . ?
Mo55 Mo54 O198 71.0(12) . . ?
O220 Mo54 O198 78.3(9) . . ?
O216 Mo54 O198 168.9(16) . . ?
O197 Mo54 O198 69.0(9) . . ?
O217 Mo54 O198 88.0(15) . . ?
O221 Mo54 O198 141(2) . . ?
Mo55 Mo54 O210 133.5(17) . . ?
O220 Mo54 O210 154.3(13) . . ?
O216 Mo54 O210 89.5(18) . . ?
O197 Mo54 O210 89.2(11) . . ?
O217 Mo54 O210 82.8(16) . . ?
O221 Mo54 O210 122(2) . . ?
O198 Mo54 O210 96.8(11) . . ?
Mo55 Mo54 Mo24 104.7(10) . . ?
O220 Mo54 Mo24 104.2(6) . . ?
O216 Mo54 Mo24 135.4(14) . . ?
O197 Mo54 Mo24 33.8(6) . . ?
O217 Mo54 Mo24 121.0(14) . . ?
O221 Mo54 Mo24 134.5(19) . . ?
O198 Mo54 Mo24 37.0(6) . . ?
O210 Mo54 Mo24 84.8(9) . . ?
O220 Mo55 Mo54 136.2(19) . . ?
O220 Mo55 O217 115(2) . . ?
Mo54 Mo55 O217 103(2) . . ?
O220 Mo55 O198 103.3(14) . . ?
Mo54 Mo55 O198 87.9(12) . . ?
O217 Mo55 O198 102.5(18) . . ?
O220 Mo55 O221 73(2) . . ?
Mo54 Mo55 O221 74(2) . . ?
O217 Mo55 O221 110(2) . . ?
O198 Mo55 O221 145.5(19) . . ?
O220 Mo55 O216 103.1(17) . . ?
Mo54 Mo55 O216 48.6(15) . . ?
O217 Mo55 O216 98(2) . . ?
O198 Mo55 O216 135.2(13) . . ?
O221 Mo55 O216 30.1(17) . . ?
O220 Mo55 O218 46.2(15) . . ?
Mo54 Mo55 O218 170.6(15) . . ?
O217 Mo55 O218 70.9(19) . . ?
O198 Mo55 O218 100.4(12) . . ?
O221 Mo55 O218 101(2) . . ?
O216 Mo55 O218 123.9(15) . . ?
O220 Mo55 O197 109.6(13) . . ?
Mo54 Mo55 O197 39.9(10) . . ?
O217 Mo55 O197 135.2(18) . . ?
O198 Mo55 O197 62.0(8) . . ?
O221 Mo55 O197 86.3(18) . . ?
O216 Mo55 O197 75.3(12) . . ?
O218 Mo55 O197 148.8(11) . . ?
O220 Mo55 O219 36.2(19) . . ?
Mo54 Mo55 O219 106(2) . . ?
O217 Mo55 O219 150(2) . . ?
O198 Mo55 O219 83.9(18) . . ?
O221 Mo55 O219 73(2) . . ?
O216 Mo55 O219 97(2) . . ?
O218 Mo55 O219 79.4(19) . . ?
O197 Mo55 O219 73.6(17) . . ?
O220 Mo55 Mo64 78.4(12) . . ?
Mo54 Mo55 Mo64 143.2(14) . . ?
O217 Mo55 Mo64 40.2(16) . . ?
O198 Mo55 Mo64 96.1(7) . . ?
O221 Mo55 Mo64 116.0(18) . . ?
O216 Mo55 Mo64 124.2(11) . . ?
O218 Mo55 Mo64 32.2(9) . . ?
O197 Mo55 Mo64 157.7(7) . . ?
O219 Mo55 Mo64 110.7(17) . . ?
Mo62 Mo61 O232 163(3) . . ?
Mo62 Mo61 O233 87(2) . . ?
O232 Mo61 O233 108(3) . . ?
Mo62 Mo61 O221 79(3) . . ?
O232 Mo61 O221 93(3) . . ?
O233 Mo61 O221 92(3) . . ?
Mo62 Mo61 O234 75(2) . . ?
O232 Mo61 O234 109(3) . . ?
O233 Mo61 O234 101(2) . . ?
O221 Mo61 O234 150(3) . . ?
Mo62 Mo61 O216 51.6(18) . . ?
O232 Mo61 O216 117(3) . . ?
O233 Mo61 O216 99.8(19) . . ?
O221 Mo61 O216 29(2) . . ?
O234 Mo61 O216 120.5(18) . . ?
Mo62 Mo61 O231 8(2) . . ?
O232 Mo61 O231 166(3) . . ?
O233 Mo61 O231 86(2) . . ?
O221 Mo61 O231 86(3) . . ?
O234 Mo61 O231 67(2) . . ?
O216 Mo61 O231 59.4(19) . . ?
Mo62 Mo61 O207 69.2(18) . . ?
O232 Mo61 O207 96(2) . . ?
O233 Mo61 O207 156.4(17) . . ?
O221 Mo61 O207 85(2) . . ?
O234 Mo61 O207 72.0(15) . . ?
O216 Mo61 O207 67.1(13) . . ?
O231 Mo61 O207 70.0(17) . . ?
Mo61 Mo62 O221 79(3) . . ?
Mo61 Mo62 O231 169(3) . . ?
O221 Mo62 O231 111(3) . . ?
Mo61 Mo62 O233 71(2) . . ?
O221 Mo62 O233 89(3) . . ?
O231 Mo62 O233 107(3) . . ?
Mo61 Mo62 O216 112(2) . . ?
O221 Mo62 O216 35(2) . . ?
O231 Mo62 O216 79(2) . . ?
O233 Mo62 O216 110.1(19) . . ?
Mo61 Mo62 O234 86(2) . . ?
O221 Mo62 O234 159(3) . . ?
O231 Mo62 O234 84(3) . . ?
O233 Mo62 O234 100(2) . . ?
O216 Mo62 O234 148(2) . . ?
Mo61 Mo62 O232 11(2) . . ?
O221 Mo62 O232 74(3) . . ?
O231 Mo62 O232 170(3) . . ?
O233 Mo62 O232 81(2) . . ?
O216 Mo62 O232 104.3(19) . . ?
O234 Mo62 O232 89(2) . . ?
Mo61 Mo62 O207 95.2(19) . . ?
O221 Mo62 O207 90(2) . . ?
O231 Mo62 O207 86(2) . . ?
O233 Mo62 O207 166.3(16) . . ?
O216 Mo62 O207 75.8(14) . . ?
O234 Mo62 O207 76.7(15) . . ?
O232 Mo62 O207 85.4(16) . . ?
Mo73 Mo63 O235 76(2) . . ?
Mo73 Mo63 O256 73(2) . . ?
O235 Mo63 O256 90(2) . . ?
Mo73 Mo63 O237 174(2) . . ?
O235 Mo63 O237 110(2) . . ?
O256 Mo63 O237 106.7(18) . . ?
Mo73 Mo63 O236 11(3) . . ?
O235 Mo63 O236 83(3) . . ?
O256 Mo63 O236 82(3) . . ?
O237 Mo63 O236 165(2) . . ?
Mo73 Mo63 O215 97(2) . . ?
O235 Mo63 O215 102(2) . . ?
O256 Mo63 O215 24.6(15) . . ?
O237 Mo63 O215 82.4(16) . . ?
O236 Mo63 O215 104(2) . . ?
Mo73 Mo63 O190 81.5(19) . . ?
O235 Mo63 O190 157.3(19) . . ?
O256 Mo63 O190 82.1(14) . . ?
O237 Mo63 O190 92.9(12) . . ?
O236 Mo63 O190 75(2) . . ?
O215 Mo63 O190 79.1(12) . . ?
O238 Mo64 O239 139(3) . . ?
O238 Mo64 O218 169(3) . . ?
O239 Mo64 O218 31.4(14) . . ?
O238 Mo64 O217 110(3) . . ?
O239 Mo64 O217 110.3(19) . . ?
O218 Mo64 O217 79(2) . . ?
O238 Mo64 O257 117(3) . . ?
O239 Mo64 O257 26.0(12) . . ?
O218 Mo64 O257 55.8(17) . . ?
O217 Mo64 O257 132.0(17) . . ?
O238 Mo64 O240 66(3) . . ?
O239 Mo64 O240 115(2) . . ?
O218 Mo64 O240 111(2) . . ?
O217 Mo64 O240 83(2) . . ?
O257 Mo64 O240 124.4(19) . . ?
O238 Mo64 O203 104(3) . . ?
O239 Mo64 O203 75.0(12) . . ?
O218 Mo64 O203 79.7(16) . . ?
O217 Mo64 O203 96.8(15) . . ?
O257 Mo64 O203 63.0(11) . . ?
O240 Mo64 O203 169.2(19) . . ?
O238 Mo64 Mo55 139(2) . . ?
O239 Mo64 Mo55 81.2(13) . . ?
O218 Mo64 Mo55 50.5(16) . . ?
O217 Mo64 Mo55 30.0(13) . . ?
O257 Mo64 Mo55 102.0(11) . . ?
O240 Mo64 Mo55 102.6(17) . . ?
O203 Mo64 Mo55 82.1(7) . . ?
Mo66 Mo65 O249 150(3) . . ?
Mo66 Mo65 O258 80.1(19) . . ?
O249 Mo65 O258 71(3) . . ?
Mo66 Mo65 O241 97.6(16) . . ?
O249 Mo65 O241 78(3) . . ?
O258 Mo65 O241 98(2) . . ?
Mo66 Mo65 O263 170.1(17) . . ?
O249 Mo65 O263 28(3) . . ?
O258 Mo65 O263 94(2) . . ?
O241 Mo65 O263 91(2) . . ?
Mo66 Mo65 O242 65.9(14) . . ?
O249 Mo65 O242 108(3) . . ?
O258 Mo65 O242 95.4(19) . . ?
O241 Mo65 O242 32.0(14) . . ?
O263 Mo65 O242 122.9(18) . . ?
Mo66 Mo65 O95 78.7(11) . . ?
O249 Mo65 O95 110(3) . . ?
O258 Mo65 O95 92.2(16) . . ?
O241 Mo65 O95 168.4(14) . . ?
O263 Mo65 O95 93.9(15) . . ?
O242 Mo65 O95 141.7(15) . . ?
Mo66 Mo65 O208 93.7(12) . . ?
O249 Mo65 O208 115(3) . . ?
O258 Mo65 O208 173.5(19) . . ?
O241 Mo65 O208 84.7(14) . . ?
O263 Mo65 O208 92.0(15) . . ?
O242 Mo65 O208 83.8(13) . . ?
O95 Mo65 O208 84.6(8) . . ?
Mo66 Mo65 O251 50.8(16) . . ?
O249 Mo65 O251 100(3) . . ?
O258 Mo65 O251 29.3(17) . . ?
O241 Mo65 O251 100.8(18) . . ?
O263 Mo65 O251 122.7(19) . . ?
O242 Mo65 O251 83.1(17) . . ?
O95 Mo65 O251 85.5(13) . . ?
O208 Mo65 O251 144.5(16) . . ?
Mo66 Mo65 O250 16.3(12) . . ?
O249 Mo65 O250 164(3) . . ?
O258 Mo65 O250 96.4(19) . . ?
O241 Mo65 O250 94.2(17) . . ?
O263 Mo65 O250 167.8(17) . . ?
O242 Mo65 O250 62.7(15) . . ?
O95 Mo65 O250 79.2(12) . . ?
O208 Mo65 O250 77.5(11) . . ?
O251 Mo65 O250 67.1(16) . . ?
Mo66 Mo65 K10 115.4(10) . . ?
O249 Mo65 K10 81(3) . . ?
O258 Mo65 K10 134.5(16) . . ?
O241 Mo65 K10 40.3(13) . . ?
O263 Mo65 K10 74.3(14) . . ?
O242 Mo65 K10 59.7(12) . . ?
O95 Mo65 K10 131.6(7) . . ?
O208 Mo65 K10 50.2(7) . . ?
O251 Mo65 K10 140.5(13) . . ?
O250 Mo65 K10 102.8(10) . . ?
Mo65 Mo66 O250 152.4(19) . . ?
Mo65 Mo66 O251 102(2) . . ?
O250 Mo66 O251 106(2) . . ?
Mo65 Mo66 O242 84.6(15) . . ?
O250 Mo66 O242 88(2) . . ?
O251 Mo66 O242 102(2) . . ?
Mo65 Mo66 O258 68.0(18) . . ?
O250 Mo66 O258 140(2) . . ?
O251 Mo66 O258 33.7(17) . . ?
O242 Mo66 O258 97.7(19) . . ?
Mo65 Mo66 O95 73.2(10) . . ?
O250 Mo66 O95 104.8(17) . . ?
O251 Mo66 O95 96.6(16) . . ?
O242 Mo66 O95 153.4(14) . . ?
O258 Mo66 O95 87.6(15) . . ?
Mo65 Mo66 O249 16.2(17) . . ?
O250 Mo66 O249 166(2) . . ?
O251 Mo66 O249 86(2) . . ?
O242 Mo66 O249 83.1(19) . . ?
O258 Mo66 O249 53(2) . . ?
O95 Mo66 O249 79.5(15) . . ?
Mo65 Mo66 O241 55.6(13) . . ?
O250 Mo66 O241 115.2(19) . . ?
O251 Mo66 O241 102.9(19) . . ?
O242 Mo66 O241 29.1(14) . . ?
O258 Mo66 O241 83.1(18) . . ?
O95 Mo66 O241 127.8(13) . . ?
O249 Mo66 O241 54.5(18) . . ?
Mo65 Mo66 O208 61.1(10) . . ?
O250 Mo66 O208 91.4(16) . . ?
O251 Mo66 O208 162.6(19) . . ?
O242 Mo66 O208 80.0(13) . . ?
O258 Mo66 O208 129.0(17) . . ?
O95 Mo66 O208 76.6(7) . . ?
O249 Mo66 O208 76.8(16) . . ?
O241 Mo66 O208 70.5(12) . . ?
Mo65 Mo66 K10 51.2(8) . . ?
O250 Mo66 K10 106.4(15) . . ?
O251 Mo66 K10 132.3(17) . . ?
O242 Mo66 K10 45.6(13) . . ?
O258 Mo66 K10 105.9(16) . . ?
O95 Mo66 K10 107.9(7) . . ?
O249 Mo66 K10 60.0(14) . . ?
O241 Mo66 K10 30.6(11) . . ?
O208 Mo66 K10 39.9(6) . . ?
O243 Mo67 Mo68 165(3) . . ?
O243 Mo67 O261 62(4) . . ?
Mo68 Mo67 O261 118(3) . . ?
O243 Mo67 O242 115(3) . . ?
Mo68 Mo67 O242 79.9(18) . . ?
O261 Mo67 O242 109(3) . . ?
O243 Mo67 O244 167(3) . . ?
Mo68 Mo67 O244 16.3(17) . . ?
O261 Mo67 O244 131(4) . . ?
O242 Mo67 O244 68(2) . . ?
O243 Mo67 O259 17(3) . . ?
Mo68 Mo67 O259 156(2) . . ?
O261 Mo67 O259 45(3) . . ?
O242 Mo67 O259 119(3) . . ?
O244 Mo67 O259 173(3) . . ?
O243 Mo67 O241 80(3) . . ?
Mo68 Mo67 O241 114.4(19) . . ?
O261 Mo67 O241 92(3) . . ?
O242 Mo67 O241 34.5(15) . . ?
O244 Mo67 O241 101(2) . . ?
O259 Mo67 O241 85(3) . . ?
O243 Mo67 O260 128(3) . . ?
Mo68 Mo67 O260 52(2) . . ?
O261 Mo67 O260 67(3) . . ?
O242 Mo67 O260 86(2) . . ?
O244 Mo67 O260 64(2) . . ?
O259 Mo67 O260 111(3) . . ?
O241 Mo67 O260 107(2) . . ?
O243 Mo67 O196 82(3) . . ?
Mo68 Mo67 O196 95.5(14) . . ?
O261 Mo67 O196 143(3) . . ?
O242 Mo67 O196 91.0(14) . . ?
O244 Mo67 O196 85.1(18) . . ?
O259 Mo67 O196 99(2) . . ?
O241 Mo67 O196 87.1(15) . . ?
O260 Mo67 O196 147(2) . . ?
O243 Mo67 O212 100(3) . . ?
Mo68 Mo67 O212 65.7(14) . . ?
O261 Mo67 O212 97(3) . . ?
O242 Mo67 O212 144(2) . . ?
O244 Mo67 O212 76.7(19) . . ?
O259 Mo67 O212 97(2) . . ?
O241 Mo67 O212 169.6(17) . . ?
O260 Mo67 O212 81(2) . . ?
O196 Mo67 O212 82.6(11) . . ?
O243 Mo67 K10 68(3) . . ?
Mo68 Mo67 K10 120.6(13) . . ?
O261 Mo67 K10 116(3) . . ?
O242 Mo67 K10 59.4(14) . . ?
O244 Mo67 K10 104.3(16) . . ?
O259 Mo67 K10 83(2) . . ?
O241 Mo67 K10 39.6(13) . . ?
O260 Mo67 K10 144.8(18) . . ?
O196 Mo67 K10 49.1(7) . . ?
O212 Mo67 K10 130.6(10) . . ?
O244 Mo68 Mo67 144(4) . . ?
O244 Mo68 O260 106(4) . . ?
Mo67 Mo68 O260 98(2) . . ?
O244 Mo68 O243 148(4) . . ?
Mo67 Mo68 O243 6.8(13) . . ?
O260 Mo68 O243 99(3) . . ?
O244 Mo68 O242 83(4) . . ?
Mo67 Mo68 O242 68.2(16) . . ?
O260 Mo68 O242 96(2) . . ?
O243 Mo68 O242 74.9(17) . . ?
O244 Mo68 O212 116(3) . . ?
Mo67 Mo68 O212 85.0(15) . . ?
O260 Mo68 O212 98(2) . . ?
O243 Mo68 O212 78.2(16) . . ?
O242 Mo68 O212 151.3(18) . . ?
O244 Mo68 O255 12(4) . . ?
Mo67 Mo68 O255 143(2) . . ?
O260 Mo68 O255 114(3) . . ?
O243 Mo68 O255 145(2) . . ?
O242 Mo68 O255 91(2) . . ?
O212 Mo68 O255 106(2) . . ?
O244 Mo68 O261 160(4) . . ?
Mo67 Mo68 O261 37(2) . . ?
O260 Mo68 O261 62(3) . . ?
O243 Mo68 O261 37(2) . . ?
O242 Mo68 O261 82(2) . . ?
O212 Mo68 O261 83(2) . . ?
O255 Mo68 O261 171(3) . . ?
O244 Mo68 O196 96(3) . . ?
Mo67 Mo68 O196 59.2(11) . . ?
O260 Mo68 O196 157(2) . . ?
O243 Mo68 O196 58.3(14) . . ?
O242 Mo68 O196 79.1(13) . . ?
O212 Mo68 O196 78.3(11) . . ?
O255 Mo68 O196 88(2) . . ?
O261 Mo68 O196 95(2) . . ?
O244 Mo68 O241 106(3) . . ?
Mo67 Mo68 O241 43.6(13) . . ?
O260 Mo68 O241 99(2) . . ?
O243 Mo68 O241 50.3(15) . . ?
O242 Mo68 O241 24.6(14) . . ?
O212 Mo68 O241 127.7(16) . . ?
O255 Mo68 O241 111(2) . . ?
O261 Mo68 O241 63(2) . . ?
O196 Mo68 O241 67.8(11) . . ?
O244 Mo68 K10 98(3) . . ?
Mo67 Mo68 K10 46.9(10) . . ?
O260 Mo68 K10 130(2) . . ?
O243 Mo68 K10 51.1(13) . . ?
O242 Mo68 K10 42.9(13) . . ?
O212 Mo68 K10 110.5(11) . . ?
O255 Mo68 K10 97.0(19) . . ?
O261 Mo68 K10 81(2) . . ?
O196 Mo68 K10 37.5(6) . . ?
O241 Mo68 K10 31.3(10) . . ?
Mo70 Mo69 O247 73(2) . . ?
Mo70 Mo69 O245 168.2(19) . . ?
O247 Mo69 O245 112(2) . . ?
Mo70 Mo69 O248 84.9(16) . . ?
O247 Mo69 O248 97(2) . . ?
O245 Mo69 O248 104.3(18) . . ?
Mo70 Mo69 O187 74.8(13) . . ?
O247 Mo69 O187 88.4(19) . . ?
O245 Mo69 O187 94.5(16) . . ?
O248 Mo69 O187 156.5(13) . . ?
Mo70 Mo69 O175 86.1(12) . . ?
O247 Mo69 O175 159(2) . . ?
O245 Mo69 O175 87.8(16) . . ?
O248 Mo69 O175 82.3(12) . . ?
O187 Mo69 O175 84.6(8) . . ?
Mo70 Mo69 O246 5.8(15) . . ?
O247 Mo69 O246 76(2) . . ?
O245 Mo69 O246 170.4(17) . . ?
O248 Mo69 O246 79.3(14) . . ?
O187 Mo69 O246 80.0(11) . . ?
O175 Mo69 O246 83.9(10) . . ?
Mo70 Mo69 K7 112.0(11) . . ?
O247 Mo69 K7 143.2(19) . . ?
O245 Mo69 K7 70.5(14) . . ?
O248 Mo69 K7 49.5(11) . . ?
O187 Mo69 K7 128.4(6) . . ?
O175 Mo69 K7 47.1(6) . . ?
O246 Mo69 K7 106.7(9) . . ?
Mo69 Mo70 O246 169(3) . . ?
Mo69 Mo70 O247 73(2) . . ?
O246 Mo70 O247 111(3) . . ?
Mo69 Mo70 O187 75.9(13) . . ?
O246 Mo70 O187 114(2) . . ?
O247 Mo70 O187 89(2) . . ?
Mo69 Mo70 O248 65.1(15) . . ?
O246 Mo70 O248 104(2) . . ?
O247 Mo70 O248 91(2) . . ?
O187 Mo70 O248 139.3(16) . . ?
Mo69 Mo70 O175 67.6(12) . . ?
O246 Mo70 O175 108(2) . . ?
O247 Mo70 O175 141(2) . . ?
O187 Mo70 O175 80.6(10) . . ?
O248 Mo70 O175 74.4(12) . . ?
Mo72 Mo71 O262 87(3) . . ?
Mo72 Mo71 O253 171(2) . . ?
O262 Mo71 O253 94(3) . . ?
Mo72 Mo71 O248 85.3(14) . . ?
O262 Mo71 O248 96(3) . . ?
O253 Mo71 O248 103(2) . . ?
Mo72 Mo71 O209 66.4(12) . . ?
O262 Mo71 O209 96(3) . . ?
O253 Mo71 O209 105(2) . . ?
O248 Mo71 O209 148.5(14) . . ?
Mo72 Mo71 O185 80.2(11) . . ?
O262 Mo71 O185 167(3) . . ?
O253 Mo71 O185 98(2) . . ?
O248 Mo71 O185 81.8(12) . . ?
O209 Mo71 O185 80.1(9) . . ?
Mo72 Mo71 O254 7.3(13) . . ?
O262 Mo71 O254 93(3) . . ?
O253 Mo71 O254 172(2) . . ?
O248 Mo71 O254 80.4(14) . . ?
O209 Mo71 O254 70.0(12) . . ?
O185 Mo71 O254 74.3(11) . . ?
Mo72 Mo71 K7 109.2(9) . . ?
O262 Mo71 K7 136(3) . . ?
O253 Mo71 K7 75.5(19) . . ?
O248 Mo71 K7 48.4(11) . . ?
O209 Mo71 K7 127.2(8) . . ?
O185 Mo71 K7 48.7(5) . . ?
O254 Mo71 K7 101.9(10) . . ?
O254 Mo72 Mo71 165(3) . . ?
O254 Mo72 O262 137(3) . . ?
Mo71 Mo72 O262 54(2) . . ?
O254 Mo72 O209 105(2) . . ?
Mo71 Mo72 O209 81.6(13) . . ?
O262 Mo72 O209 92(2) . . ?
O254 Mo72 O248 107(2) . . ?
Mo71 Mo72 O248 62.7(13) . . ?
O262 Mo72 O248 79(2) . . ?
O209 Mo72 O248 141.8(16) . . ?
O254 Mo72 O185 97(2) . . ?
Mo71 Mo72 O185 70.7(10) . . ?
O262 Mo72 O185 125(2) . . ?
O209 Mo72 O185 81.0(11) . . ?
O248 Mo72 O185 74.9(11) . . ?
Mo63 Mo73 O236 159(5) . . ?
Mo63 Mo73 O256 77(2) . . ?
O236 Mo73 O256 118(5) . . ?
Mo63 Mo73 O235 74(3) . . ?
O236 Mo73 O235 117(5) . . ?
O256 Mo73 O235 91(2) . . ?
Mo63 Mo73 O257 110(2) . 2_655 ?
O236 Mo73 O257 53(4) . 2_655 ?
O256 Mo73 O257 169(2) . 2_655 ?
O235 Mo73 O257 99(2) . 2_655 ?
Mo63 Mo73 O190 76.9(19) . . ?
O236 Mo73 O190 91(5) . . ?
O256 Mo73 O190 81.6(17) . . ?
O235 Mo73 O190 151(3) . . ?
O257 Mo73 O190 91.4(13) 2_655 . ?
Mo2 Mo81 O151 167(3) . . ?
Mo2 Mo81 O8 80.4(19) . 6 ?
O151 Mo81 O8 107.2(19) . 6 ?
Mo2 Mo81 O8 80.4(19) . . ?
O151 Mo81 O8 107.2(19) . . ?
O8 Mo81 O8 105.0(16) 6 . ?
Mo2 Mo81 O56 74.3(18) . . ?
O151 Mo81 O56 94.9(15) . . ?
O8 Mo81 O56 149(2) 6 . ?
O8 Mo81 O56 89.0(9) . . ?
Mo2 Mo81 O56 74.3(18) . 6 ?
O151 Mo81 O56 94.8(15) . 6 ?
O8 Mo81 O56 89.0(9) 6 6 ?
O8 Mo81 O56 149(2) . 6 ?
O56 Mo81 O56 66.5(12) . 6 ?
Mo2 Mo81 O120 1.6(13) . . ?
O151 Mo81 O120 168.6(16) . . ?
O8 Mo81 O120 79.4(17) 6 . ?
O8 Mo81 O120 79.4(17) . . ?
O56 Mo81 O120 75.6(14) . . ?
O56 Mo81 O120 75.7(14) 6 . ?
Mo2 Mo81 S12 138(2) . . ?
O151 Mo81 S12 30.8(10) . . ?
O8 Mo81 S12 136(2) 6 . ?
O8 Mo81 S12 103.4(15) . . ?
O56 Mo81 S12 64.1(11) . . ?
O56 Mo81 S12 84.1(12) 6 . ?
O120 Mo81 S12 139.5(13) . . ?
Mo2 Mo81 S12 138(2) . 6 ?
O151 Mo81 S12 30.8(10) . 6 ?
O8 Mo81 S12 103.4(15) 6 6 ?
O8 Mo81 S12 136(2) . 6 ?
O56 Mo81 S12 84.1(12) . 6 ?
O56 Mo81 S12 64.1(11) 6 6 ?
O120 Mo81 S12 139.5(13) . 6 ?
S12 Mo81 S12 35.4(15) . 6 ?
Mo2 Mo81 Mo86 93(2) . . ?
O151 Mo81 Mo86 73.9(18) . . ?
O8 Mo81 Mo86 126.4(8) 6 . ?
O8 Mo81 Mo86 126.4(8) . . ?
O56 Mo81 Mo86 39.1(9) . . ?
O56 Mo81 Mo86 39.1(9) 6 . ?
O120 Mo81 Mo86 94.6(18) . . ?
S12 Mo81 Mo86 50.7(15) . . ?
S12 Mo81 Mo86 50.7(15) 6 . ?
Mo2 Mo81 K5 90.9(19) . 5_656 ?
O151 Mo81 K5 102.2(16) . 5_656 ?
O8 Mo81 K5 54.3(8) 6 5_656 ?
O8 Mo81 K5 54.3(8) . 5_656 ?
O56 Mo81 K5 142.7(10) . 5_656 ?
O56 Mo81 K5 142.7(10) 6 5_656 ?
O120 Mo81 K5 89.3(11) . 5_656 ?
S12 Mo81 K5 125.7(15) . 5_656 ?
S12 Mo81 K5 125.7(15) 6 5_656 ?
Mo86 Mo81 K5 176(2) . 5_656 ?
Mo20 Mo82 O170 165(2) . . ?
Mo20 Mo82 O35 79(2) . . ?
O170 Mo82 O35 110.9(18) . . ?
Mo20 Mo82 O138 76.1(18) . . ?
O170 Mo82 O138 110.3(18) . . ?
O35 Mo82 O138 104.5(14) . . ?
Mo20 Mo82 O31 71.2(15) . . ?
O170 Mo82 O31 97.8(14) . . ?
O35 Mo82 O31 87.7(12) . . ?
O138 Mo82 O31 142(2) . . ?
Mo20 Mo82 O136 70.3(14) . . ?
O170 Mo82 O136 96.5(14) . . ?
O35 Mo82 O136 144(2) . . ?
O138 Mo82 O136 86.6(11) . . ?
O31 Mo82 O136 65.0(9) . . ?
Mo20 Mo82 S13 137.6(17) . . ?
O170 Mo82 S13 31.0(10) . . ?
O35 Mo82 S13 105.4(14) . . ?
O138 Mo82 S13 138.6(18) . . ?
O31 Mo82 S13 66.9(10) . . ?
O136 Mo82 S13 85.8(12) . . ?
Mo20 Mo82 S11 135.0(18) . . ?
O170 Mo82 S11 31.7(11) . . ?
O35 Mo82 S11 140.1(19) . . ?
O138 Mo82 S11 104.1(14) . . ?
O31 Mo82 S11 86.6(12) . . ?
O136 Mo82 S11 64.9(10) . . ?
S13 Mo82 S11 37.2(10) . . ?
Mo20 Mo82 K3 91.2(16) . . ?
O170 Mo82 K3 103.3(13) . . ?
O35 Mo82 K3 55.2(7) . . ?
O138 Mo82 K3 55.5(7) . . ?
O31 Mo82 K3 141.9(12) . . ?
O136 Mo82 K3 141.3(11) . . ?
S13 Mo82 K3 126.6(13) . . ?
S11 Mo82 K3 126.6(13) . . ?
Mo15 Mo83 O9 92(2) . . ?
Mo15 Mo83 O51 86.9(19) . . ?
O9 Mo83 O51 110.6(10) . . ?
Mo15 Mo83 O140 159.0(19) . . ?
O9 Mo83 O140 102.7(16) . . ?
O51 Mo83 O140 101.1(15) . . ?
Mo15 Mo83 O27 75.3(14) . . ?
O9 Mo83 O27 90.7(9) . . ?
O51 Mo83 O27 152.9(14) . . ?
O140 Mo83 O27 89.8(11) . . ?
Mo15 Mo83 O13 71.6(13) . . ?
O9 Mo83 O13 154.3(15) . . ?
O51 Mo83 O13 89.1(8) . . ?
O140 Mo83 O13 88.9(11) . . ?
O27 Mo83 O13 66.2(7) . . ?
Mo15 Mo83 O94 8.6(14) . . ?
O9 Mo83 O94 84.8(14) . . ?
O51 Mo83 O94 86.0(14) . . ?
O140 Mo83 O94 166.9(9) . . ?
O27 Mo83 O94 79.2(11) . . ?
O13 Mo83 O94 80.2(11) . . ?
Mo15 Mo83 K6 101.4(19) . . ?
O9 Mo83 K6 56.6(6) . . ?
O51 Mo83 K6 55.7(6) . . ?
O140 Mo83 K6 99.1(10) . . ?
O27 Mo83 K6 147.3(7) . . ?
O13 Mo83 K6 144.7(7) . . ?
O94 Mo83 K6 94.0(8) . . ?
Mo17 Mo84 O144 158.6(19) . . ?
Mo17 Mo84 O162 82.0(17) . . ?
O144 Mo84 O162 111.0(18) . . ?
Mo17 Mo84 O157 80.6(18) . . ?
O144 Mo84 O157 109.9(16) . . ?
O162 Mo84 O157 107.5(12) . . ?
Mo17 Mo84 O56 70.1(14) . . ?
O144 Mo84 O56 92.9(12) . . ?
O162 Mo84 O56 87.6(10) . . ?
O157 Mo84 O56 144.8(19) . . ?
Mo17 Mo84 O136 68.7(14) . . ?
O144 Mo84 O136 92.6(11) . . ?
O162 Mo84 O136 144.4(19) . . ?
O157 Mo84 O136 87.7(11) . . ?
O56 Mo84 O136 64.1(8) . . ?
Mo17 Mo84 O70 5.1(9) . . ?
O144 Mo84 O70 163.7(13) . . ?
O162 Mo84 O70 78.4(14) . . ?
O157 Mo84 O70 78.3(14) . . ?
O56 Mo84 O70 73.8(11) . . ?
O136 Mo84 O70 73.4(11) . . ?
Mo17 Mo84 S11 132.9(17) . . ?
O144 Mo84 S11 28.0(10) . . ?
O162 Mo84 S11 136.5(18) . . ?
O157 Mo84 S11 104.0(13) . . ?
O56 Mo84 S11 83.5(10) . . ?
O136 Mo84 S11 64.7(10) . . ?
O70 Mo84 S11 137.8(12) . . ?
Mo17 Mo84 S12 132.0(16) . . ?
O144 Mo84 S12 30.5(10) . . ?
O162 Mo84 S12 103.3(14) . . ?
O157 Mo84 S12 138.1(16) . . ?
O56 Mo84 S12 62.7(10) . . ?
O136 Mo84 S12 83.3(10) . . ?
O70 Mo84 S12 136.2(11) . . ?
S11 Mo84 S12 36.0(10) . . ?
Mo17 Mo84 K4 94.5(14) . . ?
O144 Mo84 K4 106.8(13) . . ?
O162 Mo84 K4 56.8(7) . . ?
O157 Mo84 K4 55.4(6) . . ?
O56 Mo84 K4 143.4(9) . . ?
O136 Mo84 K4 142.1(10) . . ?
O70 Mo84 K4 89.5(8) . . ?
S11 Mo84 K4 127.2(12) . . ?
S12 Mo84 K4 128.7(13) . . ?
Mo12 Mo85 O142 165.2(18) . . ?
Mo12 Mo85 O49 84.8(19) . . ?
O142 Mo85 O49 107.2(16) . . ?
Mo12 Mo85 O98 79.4(16) . . ?
O142 Mo85 O98 105.0(15) . . ?
O49 Mo85 O98 105.0(11) . . ?
Mo12 Mo85 O12 75.3(15) . . ?
O142 Mo85 O12 95.3(11) . . ?
O49 Mo85 O12 91.4(10) . . ?
O98 Mo85 O12 148.4(17) . . ?
Mo12 Mo85 O28 72.6(14) . . ?
O142 Mo85 O28 93.2(11) . . ?
O49 Mo85 O28 151.1(18) . . ?
O98 Mo85 O28 88.7(9) . . ?
O12 Mo85 O28 65.8(7) . . ?
Mo12 Mo85 O123 3.9(10) . . ?
O142 Mo85 O123 168.2(11) . . ?
O49 Mo85 O123 80.9(14) . . ?
O98 Mo85 O123 80.5(13) . . ?
O12 Mo85 O123 75.6(11) . . ?
O28 Mo85 O123 76.4(11) . . ?
Mo12 Mo85 S6 137.4(15) . . ?
O142 Mo85 S6 28.3(7) . . ?
O49 Mo85 S6 133.2(16) . . ?
O98 Mo85 S6 102.7(12) . . ?
O12 Mo85 S6 84.0(8) . . ?
O28 Mo85 S6 64.9(8) . . ?
O123 Mo85 S6 140.9(9) . . ?
Mo12 Mo85 K3 93.0(14) . . ?
O142 Mo85 K3 101.0(11) . . ?
O49 Mo85 K3 54.0(6) . . ?
O98 Mo85 K3 54.4(6) . . ?
O12 Mo85 K3 144.8(9) . . ?
O28 Mo85 K3 142.8(8) . . ?
O123 Mo85 K3 90.7(8) . . ?
S6 Mo85 K3 123.2(10) . . ?
Mo19 Mo86 O141 180(4) . . ?
Mo19 Mo86 O56 75(3) . 6 ?
O141 Mo86 O56 105(3) . 6 ?
Mo19 Mo86 O56 75(3) . . ?
O141 Mo86 O56 105(3) . . ?
O56 Mo86 O56 68.8(15) 6 . ?
Mo19 Mo86 O136 74(2) . . ?
O141 Mo86 O136 106(2) . . ?
O56 Mo86 O136 133(3) 6 . ?
O56 Mo86 O136 69.3(10) . . ?
Mo19 Mo86 O136 74(2) . 6 ?
O141 Mo86 O136 106(2) . 6 ?
O56 Mo86 O136 69.3(10) 6 6 ?
O56 Mo86 O136 133(3) . 6 ?
O136 Mo86 O136 133(3) . 6 ?
Mo19 Mo86 O31 74(3) . . ?
O141 Mo86 O31 106(3) . . ?
O56 Mo86 O31 133(3) 6 . ?
O56 Mo86 O31 133(3) . . ?
O136 Mo86 O31 68.9(12) . . ?
O136 Mo86 O31 68.9(12) 6 . ?
Mo19 Mo86 O83 0.5(16) . . ?
O141 Mo86 O83 180(2) . . ?
O56 Mo86 O83 75(2) 6 . ?
O56 Mo86 O83 75(2) . . ?
O136 Mo86 O83 75(2) . . ?
O136 Mo86 O83 75(2) 6 . ?
O31 Mo86 O83 74(2) . . ?
Mo19 Mo86 S12 145(3) . . ?
O141 Mo86 S12 35.2(15) . . ?
O56 Mo86 S12 91(2) 6 . ?
O56 Mo86 S12 69.5(16) . . ?
O136 Mo86 S12 93.3(16) . . ?
O136 Mo86 S12 132(3) 6 . ?
O31 Mo86 S12 133(3) . . ?
O83 Mo86 S12 144.4(17) . . ?
Mo19 Mo86 S12 145(3) . 6 ?
O141 Mo86 S12 35.2(15) . 6 ?
O56 Mo86 S12 69.5(16) 6 6 ?
O56 Mo86 S12 91(2) . 6 ?
O136 Mo86 S12 132(3) . 6 ?
O136 Mo86 S12 93.3(16) 6 6 ?
O31 Mo86 S12 133(3) . 6 ?
O83 Mo86 S12 144.4(17) . 6 ?
S12 Mo86 S12 38.6(18) . 6 ?
Mo19 Mo86 S11 145.2(16) . . ?
O141 Mo86 S11 34.8(12) . . ?
O56 Mo86 S11 130(3) 6 . ?
O56 Mo86 S11 91.8(17) . . ?
O136 Mo86 S11 70.8(14) . . ?
O136 Mo86 S11 132(3) 6 . ?
O31 Mo86 S11 94.1(18) . . ?
O83 Mo86 S11 145.3(13) . . ?
S12 Mo86 S11 39.4(14) . . ?
S12 Mo86 S11 66(2) 6 . ?
Mo19 Mo86 S11 145.2(16) . 6 ?
O141 Mo86 S11 34.8(12) . 6 ?
O56 Mo86 S11 91.8(17) 6 6 ?
O56 Mo86 S11 130(3) . 6 ?
O136 Mo86 S11 132(3) . 6 ?
O136 Mo86 S11 70.8(14) 6 6 ?
O31 Mo86 S11 94.1(18) . 6 ?
O83 Mo86 S11 145.3(13) . 6 ?
S12 Mo86 S11 66(2) . 6 ?
S12 Mo86 S11 39.4(14) 6 6 ?
S11 Mo86 S11 66(2) . 6 ?
Mo14 Mo87 O21 169.9(19) . . ?
Mo14 Mo87 O87 81.7(16) . . ?
O21 Mo87 O87 105.9(17) . . ?
Mo14 Mo87 O65 80.0(17) . . ?
O21 Mo87 O65 103.7(16) . . ?
O87 Mo87 O65 105.5(11) . . ?
Mo14 Mo87 O34 78.0(17) . . ?
O21 Mo87 O34 95.0(12) . . ?
O87 Mo87 O34 90.6(10) . . ?
O65 Mo87 O34 150.5(18) . . ?
Mo14 Mo87 O68 77.5(17) . . ?
O21 Mo87 O68 93.2(11) . . ?
O87 Mo87 O68 152.6(19) . . ?
O65 Mo87 O68 88.3(9) . . ?
O34 Mo87 O68 67.9(8) . . ?
Mo14 Mo87 O115 1.3(11) . . ?
O21 Mo87 O115 169.9(11) . . ?
O87 Mo87 O115 80.8(13) . . ?
O65 Mo87 O115 81.2(13) . . ?
O34 Mo87 O115 77.1(12) . . ?
O68 Mo87 O115 78.1(12) . . ?
Mo14 Mo87 K4 89.3(13) . 2_656 ?
O21 Mo87 K4 100.5(11) . 2_656 ?
O87 Mo87 K4 53.7(7) . 2_656 ?
O65 Mo87 K4 54.5(6) . 2_656 ?
O34 Mo87 K4 143.7(8) . 2_656 ?
O68 Mo87 K4 142.4(9) . 2_656 ?
O115 Mo87 K4 89.5(7) . 2_656 ?
Mo10 Mo88 O125 86(3) . . ?
Mo10 Mo88 O59 167(2) . . ?
O125 Mo88 O59 104.1(18) . . ?
Mo10 Mo88 O77 81.9(19) . . ?
O125 Mo88 O77 107.8(12) . . ?
O59 Mo88 O77 103(2) . . ?
Mo10 Mo88 O7 79(2) . . ?
O125 Mo88 O7 91.1(11) . . ?
O59 Mo88 O7 91.9(12) . . ?
O77 Mo88 O7 152.2(19) . . ?
Mo10 Mo88 O34 75.3(18) . . ?
O125 Mo88 O34 153(2) . . ?
O59 Mo88 O34 92.1(13) . . ?
O77 Mo88 O34 88.6(10) . . ?
O7 Mo88 O34 67.1(8) . . ?
Mo10 Mo88 O63 3.8(15) . . ?
O125 Mo88 O63 82.5(17) . . ?
O59 Mo88 O63 169.3(12) . . ?
O77 Mo88 O63 83.0(15) . . ?
O7 Mo88 O63 79.4(14) . . ?
O34 Mo88 O63 78.9(13) . . ?
Mo10 Mo88 K8 92.0(18) . . ?
O125 Mo88 K8 54.8(7) . . ?
O59 Mo88 K8 100.9(13) . . ?
O77 Mo88 K8 54.8(7) . . ?
O7 Mo88 K8 145.4(11) . . ?
O34 Mo88 K8 142.9(9) . . ?
O63 Mo88 K8 89.7(9) . . ?
Mo38 Mo89 O166 141.4(16) . . ?
Mo38 Mo89 O202 76.7(14) . . ?
O166 Mo89 O202 135.9(16) . . ?
Mo38 Mo89 O183 75.3(11) . . ?
O166 Mo89 O183 108.4(13) . . ?
O202 Mo89 O183 102.0(12) . . ?
Mo38 Mo89 O184 58.4(12) . . ?
O166 Mo89 O184 96.6(12) . . ?
O202 Mo89 O184 87.9(12) . . ?
O183 Mo89 O184 129.0(14) . . ?
Mo38 Mo89 Mo35 116.8(10) . . ?
O166 Mo89 Mo35 27.3(9) . . ?
O202 Mo89 Mo35 162.4(12) . . ?
O183 Mo89 Mo35 92.7(7) . . ?
O184 Mo89 Mo35 90.2(7) . . ?
Mo4 Mo90 O134 174(2) . . ?
Mo4 Mo90 O19 77(2) . . ?
O134 Mo90 O19 105.4(18) . . ?
Mo4 Mo90 O90 77(2) . . ?
O134 Mo90 O90 107.1(19) . . ?
O19 Mo90 O90 102.0(13) . . ?
Mo4 Mo90 O126 79(2) . . ?
O134 Mo90 O126 96.8(15) . . ?
O19 Mo90 O126 150(2) . . ?
O90 Mo90 O126 89.5(11) . . ?
Mo4 Mo90 O28 79(2) . . ?
O134 Mo90 O28 96.1(14) . . ?
O19 Mo90 O28 89.8(11) . . ?
O90 Mo90 O28 150(2) . . ?
O126 Mo90 O28 68.3(9) . . ?
Mo4 Mo90 O93 2.6(13) . . ?
O134 Mo90 O93 171.5(13) . . ?
O19 Mo90 O93 79.2(16) . . ?
O90 Mo90 O93 78.4(15) . . ?
O126 Mo90 O93 76.6(14) . . ?
O28 Mo90 O93 76.6(13) . . ?
Mo4 Mo90 S6 145(2) . . ?
O134 Mo90 S6 29.9(8) . . ?
O19 Mo90 S6 103.6(14) . . ?
O90 Mo90 S6 135(2) . . ?
O126 Mo90 S6 86.1(11) . . ?
O28 Mo90 S6 66.3(10) . . ?
O93 Mo90 S6 142.7(11) . . ?
Mo4 Mo90 K4 85.7(17) . . ?
O134 Mo90 K4 100.2(13) . . ?
O19 Mo90 K4 52.9(7) . . ?
O90 Mo90 K4 52.8(7) . . ?
O126 Mo90 K4 141.8(11) . . ?
O28 Mo90 K4 142.0(11) . . ?
O93 Mo90 K4 88.3(10) . . ?
S6 Mo90 K4 123.6(12) . . ?
Mo16 Mo91 O101 87.7(12) . . ?
Mo16 Mo91 O101 87.7(12) . 6 ?
O101 Mo91 O101 109.2(10) . 6 ?
Mo16 Mo91 O102 165.2(15) . . ?
O101 Mo91 O102 100.8(10) . . ?
O101 Mo91 O102 100.8(10) 6 . ?
Mo16 Mo91 O25 77.4(10) . 6 ?
O101 Mo91 O25 155.4(10) . 6 ?
O101 Mo91 O25 89.8(6) 6 6 ?
O102 Mo91 O25 90.4(9) . 6 ?
Mo16 Mo91 O25 77.4(10) . . ?
O101 Mo91 O25 89.8(6) . . ?
O101 Mo91 O25 155.4(10) 6 . ?
O102 Mo91 O25 90.4(9) . . ?
O25 Mo91 O25 68.1(8) 6 . ?
Mo16 Mo91 O109 4.1(11) . . ?
O101 Mo91 O109 85.3(10) . . ?
O101 Mo91 O109 85.3(10) 6 . ?
O102 Mo91 O109 169.3(10) . . ?
O25 Mo91 O109 80.7(9) 6 . ?
O25 Mo91 O109 80.7(9) . . ?
Mo16 Mo91 K6 97.7(13) . . ?
O101 Mo91 K6 55.4(5) . . ?
O101 Mo91 K6 55.4(5) 6 . ?
O102 Mo91 K6 97.1(9) . . ?
O25 Mo91 K6 145.2(4) 6 . ?
O25 Mo91 K6 145.2(4) . . ?
O109 Mo91 K6 93.7(7) . . ?
Mo39 Mo92 O95 86(3) . . ?
Mo39 Mo92 O174 170(3) . . ?
O95 Mo92 O174 103(2) . . ?
Mo39 Mo92 O187 76.4(19) . . ?
O95 Mo92 O187 107.4(14) . . ?
O174 Mo92 O187 103(3) . . ?
Mo39 Mo92 O169 82(3) . . ?
O95 Mo92 O169 90.5(14) . . ?
O174 Mo92 O169 94.9(15) . . ?
O187 Mo92 O169 150(3) . . ?
Mo39 Mo92 O127 74(2) . . ?
O95 Mo92 O127 152(3) . . ?
O174 Mo92 O127 95.8(17) . . ?
O187 Mo92 O127 86.8(11) . . ?
O169 Mo92 O127 68.1(10) . . ?
Mo39 Mo92 O192 4.9(18) . . ?
O95 Mo92 O192 82(2) . . ?
O174 Mo92 O192 171.7(15) . . ?
O187 Mo92 O192 81(2) . . ?
O169 Mo92 O192 79(2) . . ?
O127 Mo92 O192 77.0(17) . . ?
Mo18 Mo93 O114 166.0(13) . . ?
Mo18 Mo93 O113 82.4(13) . . ?
O114 Mo93 O113 105.9(12) . . ?
Mo18 Mo93 O84 81.0(12) . . ?
O114 Mo93 O84 106.7(12) . . ?
O113 Mo93 O84 106.6(9) . . ?
Mo18 Mo93 O57 74.0(10) . . ?
O114 Mo93 O57 94.2(9) . . ?
O113 Mo93 O57 149.5(13) . . ?
O84 Mo93 O57 88.7(8) . . ?
Mo18 Mo93 O30 73.7(11) . . ?
O114 Mo93 O30 94.9(9) . . ?
O113 Mo93 O30 88.6(8) . . ?
O84 Mo93 O30 148.4(13) . . ?
O57 Mo93 O30 66.6(6) . . ?
Mo18 Mo93 O121 2.9(8) . . ?
O114 Mo93 O121 168.8(9) . . ?
O113 Mo93 O121 81.1(10) . . ?
O84 Mo93 O121 79.0(10) . . ?
O57 Mo93 O121 76.1(8) . . ?
O30 Mo93 O121 76.3(8) . . ?
Mo18 Mo93 K8 92.1(10) . . ?
O114 Mo93 K8 101.9(9) . . ?
O113 Mo93 K8 55.4(5) . . ?
O84 Mo93 K8 54.5(6) . . ?
O57 Mo93 K8 142.6(6) . . ?
O30 Mo93 K8 143.2(7) . . ?
O121 Mo93 K8 89.2(6) . . ?
Mo8 Mo94 O118 168(2) . . ?
Mo8 Mo94 O150 84(2) . . ?
O118 Mo94 O150 107(2) . . ?
Mo8 Mo94 O122 78(2) . . ?
O118 Mo94 O122 104.6(17) . . ?
O150 Mo94 O122 106.4(12) . . ?
Mo8 Mo94 O126 78.2(19) . . ?
O118 Mo94 O126 94.7(13) . . ?
O150 Mo94 O126 90.4(10) . . ?
O122 Mo94 O126 149(2) . . ?
Mo8 Mo94 O57 75.1(19) . . ?
O118 Mo94 O57 92.8(12) . . ?
O150 Mo94 O57 152(2) . . ?
O122 Mo94 O57 86.9(11) . . ?
O126 Mo94 O57 68.1(8) . . ?
Mo8 Mo94 O139 2.3(12) . . ?
O118 Mo94 O139 168.5(12) . . ?
O150 Mo94 O139 81.7(15) . . ?
O122 Mo94 O139 79.9(15) . . ?
O126 Mo94 O139 77.1(13) . . ?
O57 Mo94 O139 76.7(13) . . ?
Mo8 Mo94 S10 142(2) . . ?
O118 Mo94 S10 29.9(12) . . ?
O150 Mo94 S10 103.3(17) . . ?
O122 Mo94 S10 132.2(19) . . ?
O126 Mo94 S10 64.8(13) . . ?
O57 Mo94 S10 83.7(13) . . ?
O139 Mo94 S10 141.5(13) . . ?
Mo8 Mo94 K8 90.1(17) . 2_656 ?
O118 Mo94 K8 101.5(13) . 2_656 ?
O150 Mo94 K8 53.8(7) . 2_656 ?
O122 Mo94 K8 55.6(7) . 2_656 ?
O126 Mo94 K8 143.6(9) . 2_656 ?
O57 Mo94 K8 142.0(10) . 2_656 ?
O139 Mo94 K8 89.8(9) . 2_656 ?
S10 Mo94 K8 124.3(15) . 2_656 ?
Mo29 Mo95 O89 78(2) . . ?
Mo29 Mo95 O180 91(2) . . ?
O89 Mo95 O180 99.4(7) . . ?
Mo29 Mo95 O180 91(2) . 6_565 ?
O89 Mo95 O180 99.4(7) . 6_565 ?
O180 Mo95 O180 161.1(14) . 6_565 ?
Mo29 Mo95 O184 92(3) . . ?
O89 Mo95 O184 171(4) . . ?
O180 Mo95 O184 80.6(7) . . ?
O180 Mo95 O184 80.6(7) 6_565 . ?
Mo29 Mo95 O193 163(3) . . ?
O89 Mo95 O193 85(2) . . ?
O180 Mo95 O193 91.3(19) . . ?
O180 Mo95 O193 91.3(19) 6_565 . ?
O184 Mo95 O193 104(2) . . ?
Mo29 Mo95 O195 6.9(18) . . ?
O89 Mo95 O195 85(2) . . ?
O180 Mo95 O195 90.3(18) . . ?
O180 Mo95 O195 90.3(18) 6_565 . ?
O184 Mo95 O195 86(2) . . ?
O193 Mo95 O195 170.3(13) . . ?
Mo29 Mo95 Mo28 122(2) . . ?
O89 Mo95 Mo28 43.8(14) . . ?
O180 Mo95 Mo28 97.2(14) . . ?
O180 Mo95 Mo28 97.1(14) 6_565 . ?
O184 Mo95 Mo28 146(3) . . ?
O193 Mo95 Mo28 41.4(10) . . ?
O195 Mo95 Mo28 128.9(12) . . ?
Mo29 Mo95 Mo35 141.4(6) . 6_565 ?
O89 Mo95 Mo35 96.5(17) . 6_565 ?
O180 Mo95 Mo35 127(2) . 6_565 ?
O180 Mo95 Mo35 51.3(12) 6_565 6_565 ?
O184 Mo95 Mo35 90.7(15) . 6_565 ?
O193 Mo95 Mo35 40.3(7) . 6_565 ?
O195 Mo95 Mo35 141.4(7) . 6_565 ?
Mo28 Mo95 Mo35 63.0(9) . 6_565 ?
Mo29 Mo95 Mo35 141.4(6) . . ?
O89 Mo95 Mo35 96.5(17) . . ?
O180 Mo95 Mo35 51.3(12) . . ?
O180 Mo95 Mo35 127(2) 6_565 . ?
O184 Mo95 Mo35 90.7(15) . . ?
O193 Mo95 Mo35 40.3(7) . . ?
O195 Mo95 Mo35 141.4(7) . . ?
Mo28 Mo95 Mo35 63.0(9) . . ?
Mo35 Mo95 Mo35 76.9(13) 6_565 . ?
Mo29 Mo95 Mo38 97(2) . 6_565 ?
O89 Mo95 Mo38 144.3(3) . 6_565 ?
O180 Mo95 Mo38 116.2(9) . 6_565 ?
O180 Mo95 Mo38 45.0(6) 6_565 6_565 ?
O184 Mo95 Mo38 36.1(3) . 6_565 ?
O193 Mo95 Mo38 96.3(14) . 6_565 ?
O195 Mo95 Mo38 91.6(13) . 6_565 ?
Mo28 Mo95 Mo38 127.9(14) . 6_565 ?
Mo35 Mo95 Mo38 65.0(5) 6_565 6_565 ?
Mo35 Mo95 Mo38 107.6(12) . 6_565 ?
Mo29 Mo95 Mo38 97(2) . . ?
O89 Mo95 Mo38 144.3(3) . . ?
O180 Mo95 Mo38 44.9(6) . . ?
O180 Mo95 Mo38 116.2(9) 6_565 . ?
O184 Mo95 Mo38 36.1(3) . . ?
O193 Mo95 Mo38 96.3(14) . . ?
O195 Mo95 Mo38 91.6(13) . . ?
Mo28 Mo95 Mo38 127.9(14) . . ?
Mo35 Mo95 Mo38 107.6(12) 6_565 . ?
Mo35 Mo95 Mo38 65.0(5) . . ?
Mo38 Mo95 Mo38 71.2(4) 6_565 . ?
O161 V1 O35 90.2(7) . 6 ?
O161 V1 O35 90.2(7) . . ?
O35 V1 O35 88.7(9) 6 . ?
O161 V1 O29 93.4(7) . . ?
O35 V1 O29 176.2(7) 6 . ?
O35 V1 O29 92.3(6) . . ?
O161 V1 O29 93.4(7) . 6 ?
O35 V1 O29 92.3(6) 6 6 ?
O35 V1 O29 176.2(7) . 6 ?
O29 V1 O29 86.4(8) . 6 ?
O161 V1 O129 178.3(10) . . ?
O35 V1 O129 88.6(7) 6 . ?
O35 V1 O129 88.6(7) . . ?
O29 V1 O129 87.8(7) . . ?
O29 V1 O129 87.8(7) 6 . ?
O161 V1 K3 89.78(16) . 6 ?
O35 V1 K3 45.4(5) 6 6 ?
O35 V1 K3 134.2(5) . 6 ?
O29 V1 K3 133.4(4) . 6 ?
O29 V1 K3 47.0(4) 6 6 ?
O129 V1 K3 90.21(16) . 6 ?
O161 V1 K3 89.78(16) . . ?
O35 V1 K3 134.2(5) 6 . ?
O35 V1 K3 45.4(5) . . ?
O29 V1 K3 47.0(4) . . ?
O29 V1 K3 133.4(4) 6 . ?
O129 V1 K3 90.21(16) . . ?
K3 V1 K3 179.4(3) 6 . ?
O163 V2 O90 90.6(7) . . ?
O163 V2 O77 92.0(7) . 2_656 ?
O90 V2 O77 177.4(7) . 2_656 ?
O163 V2 O150 91.7(8) . . ?
O90 V2 O150 89.3(6) . . ?
O77 V2 O150 90.8(6) 2_656 . ?
O163 V2 O87 91.7(8) . 2_656 ?
O90 V2 O87 91.0(7) . 2_656 ?
O77 V2 O87 88.8(6) 2_656 2_656 ?
O150 V2 O87 176.5(7) . 2_656 ?
O163 V2 O116 179.0(8) . . ?
O90 V2 O116 89.3(7) . . ?
O77 V2 O116 88.1(7) 2_656 . ?
O150 V2 O116 87.3(7) . . ?
O87 V2 O116 89.3(7) 2_656 . ?
O163 V2 K4 89.7(6) . . ?
O90 V2 K4 45.6(5) . . ?
O77 V2 K4 134.3(5) 2_656 . ?
O150 V2 K4 134.9(4) . . ?
O87 V2 K4 45.5(4) 2_656 . ?
O116 V2 K4 91.0(6) . . ?
O163 V2 K8 90.2(6) . 2_656 ?
O90 V2 K8 134.7(5) . 2_656 ?
O77 V2 K8 45.4(5) 2_656 2_656 ?
O150 V2 K8 45.5(4) . 2_656 ?
O87 V2 K8 134.2(5) 2_656 2_656 ?
O116 V2 K8 89.1(6) . 2_656 ?
K4 V2 K8 179.6(3) . 2_656 ?
O81 V3 O111 91.0(7) . . ?
O81 V3 O111 91.0(7) . 6 ?
O111 V3 O111 90.9(10) . 6 ?
O81 V3 O51 91.5(7) . 6 ?
O111 V3 O51 177.5(8) . 6 ?
O111 V3 O51 88.7(6) 6 6 ?
O81 V3 O51 91.5(7) . . ?
O111 V3 O51 88.7(6) . . ?
O111 V3 O51 177.5(8) 6 . ?
O51 V3 O51 91.5(9) 6 . ?
O81 V3 O146 179.7(10) . . ?
O111 V3 O146 89.3(7) . . ?
O111 V3 O146 89.2(7) 6 . ?
O51 V3 O146 88.3(7) 6 . ?
O51 V3 O146 88.3(7) . . ?
O81 V3 K6 91.3(7) . . ?
O111 V3 K6 134.5(5) . . ?
O111 V3 K6 134.5(5) 6 . ?
O51 V3 K6 45.8(4) 6 . ?
O51 V3 K6 45.8(4) . . ?
O146 V3 K6 88.4(7) . . ?
O81 V3 K5 90.8(7) . . ?
O111 V3 K5 45.5(5) . . ?
O111 V3 K5 45.4(5) 6 . ?
O51 V3 K5 134.2(4) 6 . ?
O51 V3 K5 134.2(4) . . ?
O146 V3 K5 89.5(7) . . ?
K6 V3 K5 177.9(4) . . ?
O72 V4 O122 90.4(5) . . ?
O72 V4 O122 90.4(5) . 2_656 ?
O122 V4 O122 179.1(10) . 2_656 ?
O72 V4 O84 90.9(5) . . ?
O122 V4 O84 88.4(6) . . ?
O122 V4 O84 91.6(6) 2_656 . ?
O72 V4 O84 90.9(5) . 2_656 ?
O122 V4 O84 91.6(6) . 2_656 ?
O122 V4 O84 88.4(6) 2_656 2_656 ?
O84 V4 O84 178.3(10) . 2_656 ?
O72 V4 O47 180.000(4) . . ?
O122 V4 O47 89.6(5) . . ?
O122 V4 O47 89.6(5) 2_656 . ?
O84 V4 O47 89.1(5) . . ?
O84 V4 O47 89.1(5) 2_656 . ?
O72 V4 K8 89.8(2) . 2_656 ?
O122 V4 K8 46.3(4) . 2_656 ?
O122 V4 K8 133.7(4) 2_656 2_656 ?
O84 V4 K8 134.7(5) . 2_656 ?
O84 V4 K8 45.3(5) 2_656 2_656 ?
O47 V4 K8 90.2(2) . 2_656 ?
O72 V4 K8 89.8(2) . . ?
O122 V4 K8 133.7(4) . . ?
O122 V4 K8 46.3(4) 2_656 . ?
O84 V4 K8 45.3(5) . . ?
O84 V4 K8 134.7(5) 2_656 . ?
O47 V4 K8 90.2(2) . . ?
K8 V4 K8 179.5(5) 2_656 . ?
O24 V5 O113 97.6(7) . . ?
O24 V5 O125 95.4(7) . . ?
O113 V5 O125 90.4(6) . . ?
O24 V5 O16 97.5(7) . . ?
O113 V5 O16 87.2(6) . . ?
O125 V5 O16 167.0(6) . . ?
O24 V5 O117 95.3(7) . . ?
O113 V5 O117 167.2(6) . . ?
O125 V5 O117 88.7(6) . . ?
O16 V5 O117 90.8(6) . . ?
O24 V5 O119 177.7(7) . . ?
O113 V5 O119 83.4(6) . . ?
O125 V5 O119 82.5(6) . . ?
O16 V5 O119 84.5(6) . . ?
O117 V5 O119 83.8(6) . . ?
O24 V5 K1 94.2(5) . . ?
O113 V5 K1 132.6(5) . . ?
O125 V5 K1 133.9(4) . . ?
O16 V5 K1 45.7(4) . . ?
O117 V5 K1 45.6(4) . . ?
O119 V5 K1 86.6(5) . . ?
O24 V5 K8 91.9(5) . . ?
O113 V5 K8 46.2(5) . . ?
O125 V5 K8 45.1(4) . . ?
O16 V5 K8 133.4(5) . . ?
O117 V5 K8 133.8(5) . . ?
O119 V5 K8 87.3(5) . . ?
K1 V5 K8 173.8(3) . . ?
O155 V6 O157 90.0(7) . . ?
O155 V6 O19 91.1(7) . . ?
O157 V6 O19 91.5(6) . . ?
O155 V6 O138 90.4(8) . . ?
O157 V6 O138 89.5(6) . . ?
O19 V6 O138 178.2(7) . . ?
O155 V6 O98 91.1(7) . . ?
O157 V6 O98 178.8(7) . . ?
O19 V6 O98 87.9(6) . . ?
O138 V6 O98 91.1(6) . . ?
O155 V6 O100 178.9(8) . . ?
O157 V6 O100 89.1(7) . . ?
O19 V6 O100 89.5(7) . . ?
O138 V6 O100 89.0(7) . . ?
O98 V6 O100 89.9(7) . . ?
O155 V6 K3 89.7(5) . . ?
O157 V6 K3 134.7(5) . . ?
O19 V6 K3 133.8(4) . . ?
O138 V6 K3 45.3(5) . . ?
O98 V6 K3 45.8(4) . . ?
O100 V6 K3 90.5(5) . . ?
O155 V6 K4 90.2(5) . . ?
O157 V6 K4 45.0(5) . . ?
O19 V6 K4 46.5(4) . . ?
O138 V6 K4 134.4(5) . . ?
O98 V6 K4 134.5(5) . . ?
O100 V6 K4 89.6(5) . . ?
K3 V6 K4 179.7(3) . . ?
O178 V7 O65 91.2(8) . . ?
O178 V7 O162 91.5(8) . 2_656 ?
O65 V7 O162 91.1(7) . 2_656 ?
O178 V7 O79 90.4(7) . . ?
O65 V7 O79 88.9(6) . . ?
O162 V7 O79 178.1(8) 2_656 . ?
O178 V7 O8 90.8(8) . 2_656 ?
O65 V7 O8 178.0(8) . 2_656 ?
O162 V7 O8 89.0(7) 2_656 2_656 ?
O79 V7 O8 90.9(6) . 2_656 ?
O178 V7 O158 179.8(10) . . ?
O65 V7 O158 88.6(8) . . ?
O162 V7 O158 88.3(7) 2_656 . ?
O79 V7 O158 89.8(7) . . ?
O8 V7 O158 89.4(8) 2_656 . ?
O178 V7 K5 89.6(6) . . ?
O65 V7 K5 134.8(5) . . ?
O162 V7 K5 134.1(6) 2_656 . ?
O79 V7 K5 45.8(5) . . ?
O8 V7 K5 45.1(5) 2_656 . ?
O158 V7 K5 90.7(6) . . ?
O178 V7 K4 90.3(6) . 2_656 ?
O65 V7 K4 45.7(4) . 2_656 ?
O162 V7 K4 45.4(5) 2_656 2_656 ?
O79 V7 K4 134.6(5) . 2_656 ?
O8 V7 K4 134.4(5) 2_656 2_656 ?
O158 V7 K4 89.5(6) . 2_656 ?
K5 V7 K4 179.5(3) . 2_656 ?
O110 V8 O52 90.9(6) . . ?
O110 V8 O9 90.4(6) . . ?
O52 V8 O9 178.5(6) . . ?
O110 V8 O101 91.3(6) . . ?
O52 V8 O101 87.0(6) . . ?
O9 V8 O101 92.1(6) . . ?
O110 V8 O71 90.7(6) . . ?
O52 V8 O71 92.9(6) . . ?
O9 V8 O71 88.0(6) . . ?
O101 V8 O71 178.1(6) . . ?
O110 V8 O105 179.0(7) . . ?
O52 V8 O105 89.2(6) . . ?
O9 V8 O105 89.6(6) . . ?
O101 V8 O105 89.7(6) . . ?
O71 V8 O105 88.3(6) . . ?
O110 V8 K1 88.7(5) . . ?
O52 V8 K1 46.6(4) . . ?
O9 V8 K1 134.3(5) . . ?
O101 V8 K1 133.6(4) . . ?
O71 V8 K1 46.4(4) . . ?
O105 V8 K1 90.7(5) . . ?
O110 V8 K6 90.3(5) . . ?
O52 V8 K6 133.1(5) . . ?
O9 V8 K6 46.0(5) . . ?
O101 V8 K6 46.1(4) . . ?
O71 V8 K6 134.0(5) . . ?
O105 V8 K6 90.3(5) . . ?
K1 V8 K6 178.9(2) . . ?
O23 V9 O104 96.1(6) . . ?
O23 V9 O53 98.5(6) . . ?
O104 V9 O53 90.7(6) . . ?
O23 V9 O49 96.9(6) . . ?
O104 V9 O49 88.5(6) . . ?
O53 V9 O49 164.6(6) . . ?
O23 V9 O76 97.3(6) . . ?
O104 V9 O76 166.6(6) . . ?
O53 V9 O76 87.4(6) . . ?
O49 V9 O76 89.8(6) . . ?
O23 V9 O15 178.3(7) . . ?
O104 V9 O15 84.4(5) . . ?
O53 V9 O15 83.1(5) . . ?
O49 V9 O15 81.5(6) . . ?
O76 V9 O15 82.2(5) . . ?
O23 V9 K1 91.9(5) . . ?
O104 V9 K1 45.7(4) . . ?
O53 V9 K1 46.2(4) . . ?
O49 V9 K1 134.1(5) . . ?
O76 V9 K1 133.6(4) . . ?
O15 V9 K1 89.6(4) . . ?
O23 V9 K3 94.2(5) . . ?
O104 V9 K3 133.3(4) . . ?
O53 V9 K3 132.4(4) . . ?
O49 V9 K3 45.0(5) . . ?
O76 V9 K3 45.4(4) . . ?
O15 V9 K3 84.3(4) . . ?
K1 V9 K3 173.92(17) . . ?
O304 K1 O48 145.1(5) . . ?
O304 K1 O135 138.5(6) . . ?
O48 K1 O135 67.4(4) . . ?
O304 K1 O104 73.7(5) . . ?
O48 K1 O104 117.3(4) . . ?
O135 K1 O104 120.6(5) . . ?
O304 K1 O53 75.0(5) . . ?
O48 K1 O53 139.7(4) . . ?
O135 K1 O53 81.4(4) . . ?
O104 K1 O53 57.9(4) . . ?
O304 K1 O71 73.4(5) . . ?
O48 K1 O71 89.9(4) . . ?
O135 K1 O71 85.6(4) . . ?
O104 K1 O71 147.1(4) . . ?
O53 K1 O71 113.3(4) . . ?
O304 K1 O14 134.3(5) . . ?
O48 K1 O14 67.3(4) . . ?
O135 K1 O14 71.3(4) . . ?
O104 K1 O14 60.7(4) . . ?
O53 K1 O14 79.1(4) . . ?
O71 K1 O14 152.2(4) . . ?
O304 K1 O52 73.9(5) . . ?
O48 K1 O52 122.8(4) . . ?
O135 K1 O52 64.6(4) . . ?
O104 K1 O52 112.9(4) . . ?
O53 K1 O52 57.7(4) . . ?
O71 K1 O52 57.7(4) . . ?
O14 K1 O52 120.9(4) . . ?
O304 K1 O117 71.8(5) . . ?
O48 K1 O117 73.5(4) . . ?
O135 K1 O117 124.7(5) . . ?
O104 K1 O117 111.4(4) . . ?
O53 K1 O117 146.8(4) . . ?
O71 K1 O117 56.4(4) . . ?
O14 K1 O117 125.8(4) . . ?
O52 K1 O117 111.4(4) . . ?
O304 K1 O16 73.4(5) . . ?
O48 K1 O16 85.2(4) . . ?
O135 K1 O16 148.1(4) . . ?
O104 K1 O16 57.3(4) . . ?
O53 K1 O16 113.3(4) . . ?
O71 K1 O16 111.4(4) . . ?
O14 K1 O16 83.4(4) . . ?
O52 K1 O16 147.3(4) . . ?
O117 K1 O16 56.8(4) . . ?
O304 K1 Mo7 75.8(4) . . ?
O48 K1 Mo7 134.7(3) . . ?
O135 K1 Mo7 67.3(3) . . ?
O104 K1 Mo7 86.5(3) . . ?
O53 K1 Mo7 29.1(3) . . ?
O71 K1 Mo7 86.3(3) . . ?
O14 K1 Mo7 98.3(3) . . ?
O52 K1 Mo7 29.0(3) . . ?
O117 K1 Mo7 135.9(3) . . ?
O16 K1 Mo7 137.6(3) . . ?
O304 K1 Mo13 75.7(4) . . ?
O48 K1 Mo13 98.6(3) . . ?
O135 K1 Mo13 137.0(4) . . ?
O104 K1 Mo13 29.2(3) . . ?
O53 K1 Mo13 86.9(3) . . ?
O71 K1 Mo13 136.5(3) . . ?
O14 K1 Mo13 65.8(3) . . ?
O52 K1 Mo13 137.9(3) . . ?
O117 K1 Mo13 85.3(3) . . ?
O16 K1 Mo13 28.8(3) . . ?
Mo7 K1 Mo13 114.73(14) . . ?
O15 K2 O3 84.4(6) . . ?
O15 K2 O17 101.9(6) . . ?
O3 K2 O17 139.4(7) . . ?
O15 K2 O20 141.5(7) . . ?
O3 K2 O20 71.2(5) . . ?
O17 K2 O20 80.4(6) . . ?
O15 K2 O53 52.7(4) . . ?
O3 K2 O53 114.3(6) . . ?
O17 K2 O53 50.6(4) . . ?
O20 K2 O53 111.0(6) . . ?
O15 K2 Mo7 78.8(4) . . ?
O3 K2 Mo7 132.3(6) . . ?
O17 K2 Mo7 23.5(3) . . ?
O20 K2 Mo7 95.8(5) . . ?
O53 K2 Mo7 27.2(2) . . ?
O15 K2 Mo51 74.5(4) . . ?
O3 K2 Mo51 25.6(3) . . ?
O17 K2 Mo51 117.3(5) . . ?
O20 K2 Mo51 70.7(4) . . ?
O53 K2 Mo51 90.1(4) . . ?
Mo7 K2 Mo51 106.7(4) . . ?
O15 K2 Mo50 118.9(6) . . ?
O3 K2 Mo50 69.9(4) . . ?
O17 K2 Mo50 72.2(4) . . ?
O20 K2 Mo50 24.8(3) . . ?
O53 K2 Mo50 88.6(4) . . ?
Mo7 K2 Mo50 79.9(3) . . ?
Mo51 K2 Mo50 58.4(2) . . ?
O15 K2 K1 65.9(4) . . ?
O3 K2 K1 84.5(4) . . ?
O17 K2 K1 63.0(4) . . ?
O20 K2 K1 82.1(4) . . ?
O53 K2 K1 36.4(3) . . ?
Mo7 K2 K1 47.84(19) . . ?
Mo51 K2 K1 58.9(2) . . ?
Mo50 K2 K1 57.4(2) . . ?
O311 K3 O337 134.8(7) . . ?
O311 K3 O35 136.3(7) . . ?
O337 K3 O35 73.3(5) . . ?
O311 K3 O138 147.3(7) . . ?
O337 K3 O138 73.2(5) . . ?
O35 K3 O138 57.3(4) . . ?
O311 K3 O49 73.6(7) . . ?
O337 K3 O49 70.9(5) . . ?
O35 K3 O49 144.2(5) . . ?
O138 K3 O49 110.9(5) . . ?
O311 K3 O98 108.8(7) . . ?
O337 K3 O98 72.9(5) . . ?
O35 K3 O98 112.1(5) . . ?
O138 K3 O98 57.3(4) . . ?
O49 K3 O98 56.5(4) . . ?
O311 K3 O76 66.5(6) . . ?
O337 K3 O76 71.1(5) . . ?
O35 K3 O76 110.6(5) . . ?
O138 K3 O76 144.3(5) . . ?
O49 K3 O76 57.0(4) . . ?
O98 K3 O76 111.2(5) . . ?
O311 K3 O29 94.1(7) . . ?
O337 K3 O29 74.4(5) . . ?
O35 K3 O29 57.3(4) . . ?
O138 K3 O29 112.5(5) . . ?
O49 K3 O29 111.5(5) . . ?
O98 K3 O29 147.2(5) . . ?
O76 K3 O29 56.6(4) . . ?
O311 K3 Mo82 161.4(9) . . ?
O337 K3 Mo82 61.8(7) . . ?
O35 K3 Mo82 29.5(4) . . ?
O138 K3 Mo82 30.3(5) . . ?
O49 K3 Mo82 124.7(7) . . ?
O98 K3 Mo82 82.6(5) . . ?
O76 K3 Mo82 124.1(7) . . ?
O29 K3 Mo82 82.2(5) . . ?
O311 K3 Mo85 95.9(8) . . ?
O337 K3 Mo85 62.7(7) . . ?
O35 K3 Mo85 127.5(6) . . ?
O138 K3 Mo85 82.7(4) . . ?
O49 K3 Mo85 28.4(4) . . ?
O98 K3 Mo85 29.6(4) . . ?
O76 K3 Mo85 81.7(4) . . ?
O29 K3 Mo85 128.0(6) . . ?
Mo82 K3 Mo85 100.7(6) . . ?
O311 K3 Mo20 148.9(6) . . ?
O337 K3 Mo20 75.1(4) . . ?
O35 K3 Mo20 29.0(3) . . ?
O138 K3 Mo20 28.9(3) . . ?
O49 K3 Mo20 135.0(4) . . ?
O98 K3 Mo20 85.8(3) . . ?
O76 K3 Mo20 134.8(4) . . ?
O29 K3 Mo20 86.1(3) . . ?
Mo82 K3 Mo20 13.4(6) . . ?
Mo85 K3 Mo20 108.4(4) . . ?
O311 K3 Mo3 75.7(6) . . ?
O337 K3 Mo3 74.3(4) . . ?
O35 K3 Mo3 85.4(3) . . ?
O138 K3 Mo3 136.0(4) . . ?
O49 K3 Mo3 85.0(3) . . ?
O98 K3 Mo3 135.7(4) . . ?
O76 K3 Mo3 28.3(3) . . ?
O29 K3 Mo3 28.8(3) . . ?
Mo82 K3 Mo3 106.8(5) . . ?
Mo85 K3 Mo3 107.5(4) . . ?
Mo20 K3 Mo3 113.3(2) . . ?
O301 K4 O157 72.7(6) 2_656 . ?
O301 K4 O87 68.9(6) 2_656 2_656 ?
O157 K4 O87 141.6(6) . 2_656 ?
O301 K4 O90 69.7(6) 2_656 . ?
O157 K4 O90 110.3(5) . . ?
O87 K4 O90 56.2(4) 2_656 . ?
O301 K4 O162 72.6(6) 2_656 . ?
O157 K4 O162 57.3(5) . . ?
O87 K4 O162 109.0(5) 2_656 . ?
O90 K4 O162 142.3(6) . . ?
O301 K4 O19 71.7(5) 2_656 . ?
O157 K4 O19 56.6(5) . . ?
O87 K4 O19 110.0(5) 2_656 . ?
O90 K4 O19 56.7(4) . . ?
O162 K4 O19 111.1(5) . . ?
O301 K4 O65 71.2(5) 2_656 2_656 ?
O157 K4 O65 109.9(6) . 2_656 ?
O87 K4 O65 56.7(5) 2_656 2_656 ?
O90 K4 O65 110.4(5) . 2_656 ?
O162 K4 O65 55.3(5) . 2_656 ?
O19 K4 O65 142.9(6) . 2_656 ?
O301 K4 Mo84 62.5(7) 2_656 . ?
O157 K4 Mo84 30.0(4) . . ?
O87 K4 Mo84 122.8(7) 2_656 . ?
O90 K4 Mo84 124.5(7) . . ?
O162 K4 Mo84 29.2(4) . . ?
O19 K4 Mo84 81.9(5) . . ?
O65 K4 Mo84 79.9(5) 2_656 . ?
O301 K4 Mo87 61.3(7) 2_656 2_656 ?
O157 K4 Mo87 125.3(7) . 2_656 ?
O87 K4 Mo87 28.3(4) 2_656 2_656 ?
O90 K4 Mo87 81.0(4) . 2_656 ?
O162 K4 Mo87 80.8(5) . 2_656 ?
O19 K4 Mo87 125.3(7) . 2_656 ?
O65 K4 Mo87 29.5(4) 2_656 2_656 ?
Mo84 K4 Mo87 98.7(7) . 2_656 ?
O301 K4 Mo90 60.9(8) 2_656 . ?
O157 K4 Mo90 81.1(5) . . ?
O87 K4 Mo90 81.0(5) 2_656 . ?
O90 K4 Mo90 29.2(4) . . ?
O162 K4 Mo90 125.1(7) . . ?
O19 K4 Mo90 29.1(5) . . ?
O65 K4 Mo90 125.0(8) 2_656 . ?
Mo84 K4 Mo90 99.3(7) . . ?
Mo87 K4 Mo90 99.6(7) 2_656 . ?
O301 K4 Mo17 75.2(5) 2_656 . ?
O157 K4 Mo17 29.2(3) . . ?
O87 K4 Mo17 133.0(5) 2_656 . ?
O90 K4 Mo17 134.5(4) . . ?
O162 K4 Mo17 28.9(3) . . ?
O19 K4 Mo17 85.4(4) . . ?
O65 K4 Mo17 83.9(4) 2_656 . ?
Mo84 K4 Mo17 12.7(5) . . ?
Mo87 K4 Mo17 106.7(4) 2_656 . ?
Mo90 K4 Mo17 107.1(5) . . ?
O301 K4 Mo14 72.1(5) 2_656 2_656 ?
O157 K4 Mo14 133.8(5) . 2_656 ?
O87 K4 Mo14 28.4(3) 2_656 2_656 ?
O90 K4 Mo14 84.3(3) . 2_656 ?
O162 K4 Mo14 83.9(4) . 2_656 ?
O19 K4 Mo14 133.8(5) . 2_656 ?
O65 K4 Mo14 29.1(3) 2_656 2_656 ?
Mo84 K4 Mo14 105.4(5) . 2_656 ?
Mo87 K4 Mo14 10.8(5) 2_656 2_656 ?
Mo90 K4 Mo14 106.4(5) . 2_656 ?
Mo17 K4 Mo14 111.7(3) . 2_656 ?
O305 K5 O8 71.3(8) . 2_656 ?
O305 K5 O8 71.3(8) . 5_656 ?
O8 K5 O8 56.4(7) 2_656 5_656 ?
O305 K5 O111 70.3(8) . 6 ?
O8 K5 O111 141.6(8) 2_656 6 ?
O8 K5 O111 109.7(5) 5_656 6 ?
O305 K5 O111 70.3(8) . . ?
O8 K5 O111 109.7(5) 2_656 . ?
O8 K5 O111 141.6(8) 5_656 . ?
O111 K5 O111 56.4(7) 6 . ?
O305 K5 O79 71.1(4) . 6 ?
O8 K5 O79 110.1(6) 2_656 6 ?
O8 K5 O79 56.5(4) 5_656 6 ?
O111 K5 O79 56.2(4) 6 6 ?
O111 K5 O79 109.8(6) . 6 ?
O305 K5 O79 71.1(4) . . ?
O8 K5 O79 56.5(4) 2_656 . ?
O8 K5 O79 110.1(6) 5_656 . ?
O111 K5 O79 109.8(6) 6 . ?
O111 K5 O79 56.2(4) . . ?
O79 K5 O79 142.3(8) 6 . ?
O305 K5 Mo81 61.8(11) . 5_656 ?
O8 K5 Mo81 29.0(4) 2_656 5_656 ?
O8 K5 Mo81 29.0(4) 5_656 5_656 ?
O111 K5 Mo81 123.9(8) 6 5_656 ?
O111 K5 Mo81 123.9(8) . 5_656 ?
O79 K5 Mo81 81.2(4) 6 5_656 ?
O79 K5 Mo81 81.2(4) . 5_656 ?
O305 K5 Mo2 73.7(8) . 5_656 ?
O8 K5 Mo2 28.6(4) 2_656 5_656 ?
O8 K5 Mo2 28.6(4) 5_656 5_656 ?
O111 K5 Mo2 133.4(5) 6 5_656 ?
O111 K5 Mo2 133.4(5) . 5_656 ?
O79 K5 Mo2 84.8(4) 6 5_656 ?
O79 K5 Mo2 84.8(4) . 5_656 ?
Mo81 K5 Mo2 11.9(6) 5_656 5_656 ?
O305 K5 Mo11 72.2(4) . . ?
O8 K5 Mo11 84.4(4) 2_656 . ?
O8 K5 Mo11 133.0(6) 5_656 . ?
O111 K5 Mo11 84.3(5) 6 . ?
O111 K5 Mo11 28.4(3) . . ?
O79 K5 Mo11 133.0(6) 6 . ?
O79 K5 Mo11 28.4(3) . . ?
Mo81 K5 Mo11 105.9(5) 5_656 . ?
Mo2 K5 Mo11 111.8(3) 5_656 . ?
O305 K5 Mo11 72.2(4) . 6 ?
O8 K5 Mo11 133.0(6) 2_656 6 ?
O8 K5 Mo11 84.4(4) 5_656 6 ?
O111 K5 Mo11 28.4(3) 6 6 ?
O111 K5 Mo11 84.3(5) . 6 ?
O79 K5 Mo11 28.4(3) 6 6 ?
O79 K5 Mo11 133.0(6) . 6 ?
Mo81 K5 Mo11 105.9(5) 5_656 6 ?
Mo2 K5 Mo11 111.7(3) 5_656 6 ?
Mo11 K5 Mo11 111.2(4) . 6 ?
O305 K5 V7 69.2(4) . 6 ?
O8 K5 V7 83.4(4) 2_656 6 ?
O8 K5 V7 28.4(3) 5_656 6 ?
O111 K5 V7 83.0(4) 6 6 ?
O111 K5 V7 130.1(5) . 6 ?
O79 K5 V7 28.2(3) 6 6 ?
O79 K5 V7 130.6(5) . 6 ?
Mo81 K5 V7 54.6(2) 5_656 6 ?
Mo2 K5 V7 56.79(18) 5_656 6 ?
Mo11 K5 V7 141.4(5) . 6 ?
Mo11 K5 V7 56.30(11) 6 6 ?
O340 K6 O340 79(2) 6 . ?
O340 K6 O306 134.5(12) 6 . ?
O340 K6 O306 134.5(12) . . ?
O340 K6 O51 100.1(12) 6 . ?
O340 K6 O51 141.9(12) . . ?
O306 K6 O51 71.9(6) . . ?
O340 K6 O51 141.9(12) 6 6 ?
O340 K6 O51 100.1(12) . 6 ?
O306 K6 O51 71.9(6) . 6 ?
O51 K6 O51 57.4(7) . 6 ?
O340 K6 O9 67.1(12) 6 . ?
O340 K6 O9 145.4(12) . . ?
O306 K6 O9 71.9(3) . . ?
O51 K6 O9 56.5(4) . . ?
O51 K6 O9 111.2(5) 6 . ?
O340 K6 O9 145.4(12) 6 6 ?
O340 K6 O9 67.1(12) . 6 ?
O306 K6 O9 71.9(3) . 6 ?
O51 K6 O9 111.2(5) . 6 ?
O51 K6 O9 56.5(4) 6 6 ?
O9 K6 O9 143.8(7) . 6 ?
O340 K6 O101 105.1(12) 6 6 ?
O340 K6 O101 69.9(12) . 6 ?
O306 K6 O101 71.5(6) . 6 ?
O51 K6 O101 143.4(6) . 6 ?
O51 K6 O101 110.4(4) 6 6 ?
O9 K6 O101 110.5(5) . 6 ?
O9 K6 O101 56.6(4) 6 6 ?
O340 K6 O101 69.9(12) 6 . ?
O340 K6 O101 105.1(12) . . ?
O306 K6 O101 71.5(6) . . ?
O51 K6 O101 110.4(4) . . ?
O51 K6 O101 143.4(6) 6 . ?
O9 K6 O101 56.6(4) . . ?
O9 K6 O101 110.5(5) 6 . ?
O101 K6 O101 56.6(6) 6 . ?
O340 K6 Mo83 160.5(13) 6 6 ?
O340 K6 Mo83 86.4(12) . 6 ?
O306 K6 Mo83 64.9(7) . 6 ?
O51 K6 Mo83 83.2(5) . 6 ?
O51 K6 Mo83 28.9(4) 6 6 ?
O9 K6 Mo83 128.2(7) . 6 ?
O9 K6 Mo83 28.3(4) 6 6 ?
O101 K6 Mo83 81.8(4) 6 6 ?
O101 K6 Mo83 127.2(6) . 6 ?
O340 K6 Mo83 86.4(12) 6 . ?
O340 K6 Mo83 160.5(13) . . ?
O306 K6 Mo83 64.9(7) . . ?
O51 K6 Mo83 28.9(4) . . ?
O51 K6 Mo83 83.2(5) 6 . ?
O9 K6 Mo83 28.3(4) . . ?
O9 K6 Mo83 128.2(7) 6 . ?
O101 K6 Mo83 127.2(6) 6 . ?
O101 K6 Mo83 81.8(4) . . ?
Mo83 K6 Mo83 104.1(8) 6 . ?
O340 K6 Mo91 90.7(12) 6 . ?
O340 K6 Mo91 90.7(12) . . ?
O306 K6 Mo91 64.5(7) . . ?
O51 K6 Mo91 127.3(5) . . ?
O51 K6 Mo91 127.3(5) 6 . ?
O9 K6 Mo91 82.2(4) . . ?
O9 K6 Mo91 82.2(4) 6 . ?
O101 K6 Mo91 28.6(3) 6 . ?
O101 K6 Mo91 28.6(3) . . ?
Mo83 K6 Mo91 102.6(5) 6 . ?
Mo83 K6 Mo91 102.6(5) . . ?
O314 K7 O172 115.6(9) . . ?
O314 K7 O4 77.3(8) . . ?
O172 K7 O4 91.5(5) . . ?
O314 K7 O175 107.0(9) . . ?
O172 K7 O175 118.6(7) . . ?
O4 K7 O175 56.8(5) . . ?
O314 K7 O185 164.7(10) . . ?
O172 K7 O185 55.4(5) . . ?
O4 K7 O185 113.4(7) . . ?
O175 K7 O185 88.3(7) . . ?
O314 K7 O248 138.7(10) . . ?
O172 K7 O248 105.7(9) . . ?
O4 K7 O248 104.7(9) . . ?
O175 K7 O248 50.6(8) . . ?
O185 K7 O248 51.6(8) . . ?
O314 K7 Mo27 91.4(8) . . ?
O172 K7 Mo27 108.8(5) . . ?
O4 K7 Mo27 29.6(3) . . ?
O175 K7 Mo27 27.3(4) . . ?
O185 K7 Mo27 103.1(6) . . ?
O248 K7 Mo27 77.0(7) . . ?
O314 K7 Mo30 141.2(9) . . ?
O172 K7 Mo30 29.0(4) . . ?
O4 K7 Mo30 108.1(5) . . ?
O175 K7 Mo30 107.5(6) . . ?
O185 K7 Mo30 27.0(4) . . ?
O248 K7 Mo30 78.5(7) . . ?
Mo27 K7 Mo30 112.2(4) . . ?
O314 K7 Mo69 115.4(8) . . ?
O172 K7 Mo69 127.5(6) . . ?
O4 K7 Mo69 87.9(5) . . ?
O175 K7 Mo69 31.4(4) . . ?
O185 K7 Mo69 77.1(5) . . ?
O248 K7 Mo69 26.6(7) . . ?
Mo27 K7 Mo69 58.3(3) . . ?
Mo30 K7 Mo69 103.3(4) . . ?
O314 K7 Mo25 90.5(8) . . ?
O172 K7 Mo25 27.0(4) . . ?
O4 K7 Mo25 75.7(4) . . ?
O175 K7 Mo25 122.4(6) . . ?
O185 K7 Mo25 82.1(4) . . ?
O248 K7 Mo25 130.5(8) . . ?
Mo27 K7 Mo25 101.5(3) . . ?
Mo30 K7 Mo25 55.95(19) . . ?
Mo69 K7 Mo25 145.8(4) . . ?
O314 K7 Mo71 148.9(8) . . ?
O172 K7 Mo71 87.1(5) . . ?
O4 K7 Mo71 125.7(6) . . ?
O175 K7 Mo71 76.8(5) . . ?
O185 K7 Mo71 32.5(4) . . ?
O248 K7 Mo71 27.1(7) . . ?
Mo27 K7 Mo71 101.5(4) . . ?
Mo30 K7 Mo71 58.1(2) . . ?
Mo69 K7 Mo71 53.1(2) . . ?
Mo25 K7 Mo71 114.0(3) . . ?
O308 K8 O77 70.6(7) . . ?
O308 K8 O150 71.2(7) . 2_656 ?
O77 K8 O150 55.9(5) . 2_656 ?
O308 K8 O125 69.3(6) . . ?
O77 K8 O125 56.7(5) . . ?
O150 K8 O125 109.3(6) 2_656 . ?
O308 K8 O84 70.0(7) . . ?
O77 K8 O84 140.6(7) . . ?
O150 K8 O84 109.4(5) 2_656 . ?
O125 K8 O84 108.5(6) . . ?
O308 K8 O113 69.6(7) . . ?
O77 K8 O113 109.2(6) . . ?
O150 K8 O113 140.7(7) 2_656 . ?
O125 K8 O113 55.4(5) . . ?
O84 K8 O113 56.4(4) . . ?
O308 K8 O122 70.9(7) . 2_656 ?
O77 K8 O122 109.7(6) . 2_656 ?
O150 K8 O122 56.9(5) 2_656 2_656 ?
O125 K8 O122 140.1(7) . 2_656 ?
O84 K8 O122 55.6(4) . 2_656 ?
O113 K8 O122 109.0(6) . 2_656 ?
O308 K8 Mo88 62.3(9) . . ?
O77 K8 Mo88 29.2(4) . . ?
O150 K8 Mo88 81.5(6) 2_656 . ?
O125 K8 Mo88 28.2(4) . . ?
O84 K8 Mo88 124.2(8) . . ?
O113 K8 Mo88 80.3(5) . . ?
O122 K8 Mo88 125.2(8) 2_656 . ?
O308 K8 Mo93 60.5(7) . . ?
O77 K8 Mo93 123.4(6) . . ?
O150 K8 Mo93 123.8(6) 2_656 . ?
O125 K8 Mo93 79.6(5) . . ?
O84 K8 Mo93 29.1(3) . . ?
O113 K8 Mo93 28.6(3) . . ?
O122 K8 Mo93 80.5(5) 2_656 . ?
Mo88 K8 Mo93 98.8(6) . . ?
O308 K8 Mo94 62.2(9) . 2_656 ?
O77 K8 Mo94 80.1(5) . 2_656 ?
O150 K8 Mo94 28.3(4) 2_656 2_656 ?
O125 K8 Mo94 123.2(8) . 2_656 ?
O84 K8 Mo94 81.2(5) . 2_656 ?
O113 K8 Mo94 124.1(8) . 2_656 ?
O122 K8 Mo94 29.8(4) 2_656 2_656 ?
Mo88 K8 Mo94 99.7(8) . 2_656 ?
Mo93 K8 Mo94 99.5(6) . 2_656 ?
O308 K8 Mo10 72.3(6) . . ?
O77 K8 Mo10 28.8(3) . . ?
O150 K8 Mo10 84.2(4) 2_656 . ?
O125 K8 Mo10 28.8(3) . . ?
O84 K8 Mo10 132.3(5) . . ?
O113 K8 Mo10 83.8(4) . . ?
O122 K8 Mo10 133.0(5) 2_656 . ?
Mo88 K8 Mo10 10.0(6) . . ?
Mo93 K8 Mo10 105.3(4) . . ?
Mo94 K8 Mo10 105.6(6) 2_656 . ?
O308 K8 Mo8 72.8(6) . 2_656 ?
O77 K8 Mo8 84.1(4) . 2_656 ?
O150 K8 Mo8 28.7(3) 2_656 2_656 ?
O125 K8 Mo8 132.2(5) . 2_656 ?
O84 K8 Mo8 83.9(4) . 2_656 ?
O113 K8 Mo8 132.3(5) . 2_656 ?
O122 K8 Mo8 28.8(3) 2_656 2_656 ?
Mo88 K8 Mo8 106.8(6) . 2_656 ?
Mo93 K8 Mo8 105.7(4) . 2_656 ?
Mo94 K8 Mo8 10.7(6) 2_656 2_656 ?
Mo10 K8 Mo8 111.4(4) . 2_656 ?
K10 K9 O334 167(4) . . ?
K10 K9 O33 82(3) . . ?
O334 K9 O33 109(2) . . ?
K10 K9 O92 78.1(19) . . ?
O334 K9 O92 95(2) . . ?
O33 K9 O92 93.8(12) . . ?
K10 K9 O312 134(3) . . ?
O334 K9 O312 56.9(19) . . ?
O33 K9 O312 72.5(10) . . ?
O92 K9 O312 139.4(17) . . ?
K10 K9 O241 29(2) . . ?
O334 K9 O241 147(3) . . ?
O33 K9 O241 99.3(15) . . ?
O92 K9 O241 99.2(13) . . ?
O312 K9 O241 120.4(14) . . ?
K10 K9 O208 42(2) . . ?
O334 K9 O208 150(2) . . ?
O33 K9 O208 52.9(9) . . ?
O92 K9 O208 109.6(13) . . ?
O312 K9 O208 92.6(11) . . ?
O241 K9 O208 47.6(10) . . ?
K10 K9 O196 37.0(17) . . ?
O334 K9 O196 131(2) . . ?
O33 K9 O196 108.4(13) . . ?
O92 K9 O196 52.3(7) . . ?
O312 K9 O196 168.2(15) . . ?
O241 K9 O196 47.9(10) . . ?
O208 K9 O196 79.4(11) . . ?
K10 K9 Mo21 64(2) . . ?
O334 K9 Mo21 129(2) . . ?
O33 K9 Mo21 27.1(5) . . ?
O92 K9 Mo21 107.8(12) . . ?
O312 K9 Mo21 77.4(10) . . ?
O241 K9 Mo21 74.2(11) . . ?
O208 K9 Mo21 26.6(5) . . ?
O196 K9 Mo21 98.2(11) . . ?
K10 K9 Mo40 58.1(17) . . ?
O334 K9 Mo40 112(2) . . ?
O33 K9 Mo40 106.0(11) . . ?
O92 K9 Mo40 26.5(5) . . ?
O312 K9 Mo40 165.5(15) . . ?
O241 K9 Mo40 74.1(10) . . ?
O208 K9 Mo40 97.8(10) . . ?
O196 K9 Mo40 26.3(4) . . ?
Mo21 K9 Mo40 108.1(10) . . ?
K10 K9 Mo23 103(3) . . ?
O334 K9 Mo23 86(2) . . ?
O33 K9 Mo23 28.9(5) . . ?
O92 K9 Mo23 79.4(9) . . ?
O312 K9 Mo23 70.5(10) . . ?
O241 K9 Mo23 126.1(15) . . ?
O208 K9 Mo23 81.6(10) . . ?
O196 K9 Mo23 116.3(11) . . ?
Mo21 K9 Mo23 56.0(6) . . ?
Mo40 K9 Mo23 101.0(8) . . ?
K10 K9 Mo33 100(2) . . ?
O334 K9 Mo33 77(2) . . ?
O33 K9 Mo33 79.3(9) . . ?
O92 K9 Mo33 28.7(5) . . ?
O312 K9 Mo33 110.8(13) . . ?
O241 K9 Mo33 125.8(12) . . ?
O208 K9 Mo33 117.2(12) . . ?
O196 K9 Mo33 80.7(7) . . ?
Mo21 K9 Mo33 102.3(10) . . ?
Mo40 K9 Mo33 55.2(4) . . ?
Mo23 K9 Mo33 56.5(6) . . ?
K9 K10 O241 138(3) . . ?
K9 K10 O196 128(2) . . ?
O241 K10 O196 66.3(13) . . ?
K9 K10 O208 121(2) . . ?
O241 K10 O208 64.7(13) . . ?
O196 K10 O208 111.1(13) . . ?
K9 K10 O334 7(2) . . ?
O241 K10 O334 136.2(17) . . ?
O196 K10 O334 120.9(13) . . ?
O208 K10 O334 128.0(14) . . ?
K9 K10 O92 80(2) . . ?
O241 K10 O92 127.4(14) . . ?
O196 K10 O92 61.1(7) . . ?
O208 K10 O92 135.4(10) . . ?
O334 K10 O92 76.3(12) . . ?
K9 K10 O242 158(3) . . ?
O241 K10 O242 19.4(12) . . ?
O196 K10 O242 58.7(10) . . ?
O208 K10 O242 58.8(10) . . ?
O334 K10 O242 155.4(15) . . ?
O92 K10 O242 116.6(11) . . ?
K9 K10 O33 76(3) . . ?
O241 K10 O33 124.7(13) . . ?
O196 K10 O33 134.4(10) . . ?
O208 K10 O33 60.0(7) . . ?
O334 K10 O33 83.0(12) . . ?
O92 K10 O33 93.2(8) . . ?
O242 K10 O33 115.3(11) . . ?
K9 K10 O243 124(3) . . ?
O241 K10 O243 36.3(12) . . ?
O196 K10 O243 41.0(9) . . ?
O208 K10 O243 100.3(11) . . ?
O334 K10 O243 117.7(14) . . ?
O92 K10 O243 96.8(9) . . ?
O242 K10 O243 43.4(10) . . ?
O33 K10 O243 158.7(12) . . ?
K9 K10 Mo65 127(2) . . ?
O241 K10 Mo65 31.1(10) . . ?
O196 K10 Mo65 94.6(9) . . ?
O208 K10 Mo65 37.6(6) . . ?
O334 K10 Mo65 130.7(12) . . ?
O92 K10 Mo65 152.4(10) . . ?
O242 K10 Mo65 36.5(8) . . ?
O33 K10 Mo65 96.0(6) . . ?
O243 K10 Mo65 67.1(8) . . ?
K9 K10 O249 112(2) . . ?
O241 K10 O249 34.1(14) . . ?
O196 K10 O249 99.9(13) . . ?
O208 K10 O249 53.0(11) . . ?
O334 K10 O249 113.3(15) . . ?
O92 K10 O249 160.4(13) . . ?
O242 K10 O249 48.3(13) . . ?
O33 K10 O249 104.8(10) . . ?
O243 K10 O249 63.6(12) . . ?
Mo65 K10 O249 19.7(9) . . ?
K9 K10 O263 96(2) . . ?
O241 K10 O263 51.4(14) . . ?
O196 K10 O263 116.3(12) . . ?
O208 K10 O263 54.8(9) . . ?
O334 K10 O263 98.3(14) . . ?
O92 K10 O263 169.6(11) . . ?
O242 K10 O263 65.3(12) . . ?
O33 K10 O263 95.0(9) . . ?
O243 K10 O263 77.7(11) . . ?
Mo65 K10 O263 32.4(8) . . ?
O249 K10 O263 17.3(9) . . ?
Mo1 O1 Mo3 109.8(5) . . ?
Mo1 O1 Mo3 109.8(5) . 6 ?
Mo3 O1 Mo3 139.9(10) . 6 ?
Mo51 O3 Mo46 119.9(7) . . ?
Mo51 O3 K2 112.3(7) . . ?
Mo46 O3 K2 123.0(7) . . ?
Mo27 O4 Mo48 150.1(8) . . ?
Mo27 O4 K7 97.5(6) . . ?
Mo48 O4 K7 112.4(7) . . ?
S1 O5 S2 62.8(18) . . ?
S1 O5 Mo11 117.7(13) . . ?
S2 O5 Mo11 115.1(15) . . ?
Mo51 O6 Mo48 156.7(8) . . ?
Mo6 O7 Mo9 109.7(6) . . ?
Mo6 O7 Mo10 109.4(7) . . ?
Mo9 O7 Mo10 140.4(8) . . ?
Mo6 O7 Mo88 111.0(8) . . ?
Mo9 O7 Mo88 137.5(10) . . ?
Mo10 O7 Mo88 17.7(10) . . ?
Mo81 O8 Mo2 24.8(13) . . ?
Mo81 O8 V7 139.1(15) . 2_656 ?
Mo2 O8 V7 152.5(9) . 2_656 ?
Mo81 O8 K5 96.7(9) . 5_656 ?
Mo2 O8 K5 99.5(7) . 5_656 ?
V7 O8 K5 106.5(6) 2_656 5_656 ?
Mo83 O9 Mo15 18.9(9) . . ?
Mo83 O9 V8 142.8(12) . . ?
Mo15 O9 V8 152.6(8) . . ?
Mo83 O9 K6 95.1(8) . . ?
Mo15 O9 K6 98.7(7) . . ?
V8 O9 K6 105.7(6) . . ?
Mo47 O10 Mo46 158.6(9) . . ?
Mo44 O11 Mo23 121.6(8) . . ?
Mo5 O12 Mo12 110.2(7) . . ?
Mo5 O12 Mo13 109.5(6) . . ?
Mo12 O12 Mo13 140.3(7) . . ?
Mo5 O12 Mo85 110.6(7) . . ?
Mo12 O12 Mo85 19.0(7) . . ?
Mo13 O12 Mo85 135.1(8) . . ?
Mo6 O13 Mo15 109.9(7) . . ?
Mo6 O13 Mo11 109.2(6) . . ?
Mo15 O13 Mo11 140.8(8) . . ?
Mo6 O13 Mo83 110.5(7) . . ?
Mo15 O13 Mo83 15.9(6) . . ?
Mo11 O13 Mo83 138.1(9) . . ?
Mo51 O14 K1 141.8(8) . . ?
V9 O15 K2 118.9(7) . . ?
Mo13 O16 V5 155.5(7) . . ?
Mo13 O16 K1 98.0(5) . . ?
V5 O16 K1 105.9(6) . . ?
Mo7 O17 K2 113.2(6) . . ?
Mo47 O18 Mo48 123.8(8) . . ?
Mo4 O19 Mo90 23.5(12) . . ?
Mo4 O19 V6 152.8(8) . . ?
Mo90 O19 V6 136.9(14) . . ?
Mo4 O19 K4 99.1(6) . . ?
Mo90 O19 K4 98.1(8) . . ?
V6 O19 K4 104.9(6) . . ?
Mo50 O20 Mo34 120.7(7) . . ?
Mo50 O20 K2 111.0(6) . . ?
Mo34 O20 K2 121.3(7) . . ?
Mo87 O21 S1 121.3(14) . . ?
Mo87 O21 S5 119.1(14) . . ?
S1 O21 S5 63.0(14) . . ?
Mo87 O21 Mo14 2.9(6) . . ?
S1 O21 Mo14 118.6(12) . . ?
S5 O21 Mo14 117.2(12) . . ?
Mo1 O22 Mo7 109.0(6) . . ?
Mo1 O22 Mo3 109.2(6) . . ?
Mo7 O22 Mo3 141.7(7) . . ?
Mo1 O25 Mo7 109.6(6) . . ?
Mo1 O25 Mo16 108.6(6) . . ?
Mo7 O25 Mo16 141.4(7) . . ?
Mo1 O25 Mo91 109.7(6) . . ?
Mo7 O25 Mo91 138.9(8) . . ?
Mo16 O25 Mo91 16.9(3) . . ?
Mo50 O26 Mo49 108.7(6) . . ?
Mo50 O26 Mo21 141.6(7) . . ?
Mo49 O26 Mo21 109.1(7) . . ?
Mo6 O27 Mo15 109.2(7) . . ?
Mo6 O27 Mo9 108.9(7) . . ?
Mo15 O27 Mo9 141.9(7) . . ?
Mo6 O27 Mo83 111.5(8) . . ?
Mo15 O27 Mo83 16.1(7) . . ?
Mo9 O27 Mo83 137.0(8) . . ?
Mo5 O28 Mo4 110.2(6) . . ?
Mo5 O28 Mo12 109.6(6) . . ?
Mo4 O28 Mo12 140.1(8) . . ?
Mo5 O28 Mo90 108.8(8) . . ?
Mo4 O28 Mo90 20.5(11) . . ?
Mo12 O28 Mo90 135.4(11) . . ?
Mo5 O28 Mo85 108.7(7) . . ?
Mo4 O28 Mo85 135.7(9) . . ?
Mo12 O28 Mo85 18.8(7) . . ?
Mo90 O28 Mo85 123.4(14) . . ?
Mo3 O29 V1 151.7(8) . . ?
Mo3 O29 K3 98.2(6) . . ?
V1 O29 K3 104.2(6) . . ?
Mo5 O30 Mo13 110.0(6) . . ?
Mo5 O30 Mo18 109.3(6) . . ?
Mo13 O30 Mo18 140.8(8) . . ?
Mo5 O30 Mo93 109.6(6) . . ?
Mo13 O30 Mo93 135.7(8) . . ?
Mo18 O30 Mo93 19.1(4) . . ?
Mo19 O31 Mo20 109.2(6) . . ?
Mo19 O31 Mo20 109.3(6) . 6 ?
Mo20 O31 Mo20 141.5(11) . 6 ?
Mo19 O31 Mo86 24.0(18) . . ?
Mo20 O31 Mo86 107.4(7) . . ?
Mo20 O31 Mo86 107.4(6) 6 . ?
Mo19 O31 Mo82 109.5(8) . . ?
Mo20 O31 Mo82 22.8(9) . . ?
Mo20 O31 Mo82 134.3(13) 6 . ?
Mo86 O31 Mo82 98.4(14) . . ?
Mo19 O31 Mo82 109.5(8) . 6 ?
Mo20 O31 Mo82 134.3(13) . 6 ?
Mo20 O31 Mo82 22.8(9) 6 6 ?
Mo86 O31 Mo82 98.4(14) . 6 ?
Mo82 O31 Mo82 118.2(19) . 6 ?
Mo25 O32 Mo48 139.1(7) . . ?
Mo25 O32 Mo45 109.6(7) . . ?
Mo48 O32 Mo45 109.6(7) . . ?
Mo21 O33 Mo23 147.5(9) . . ?
Mo21 O33 K9 106.1(10) . . ?
Mo23 O33 K9 106.4(10) . . ?
Mo21 O33 K10 90.2(8) . . ?
Mo23 O33 K10 121.6(8) . . ?
K9 O33 K10 21.9(7) . . ?
Mo6 O34 Mo14 110.1(7) . . ?
Mo6 O34 Mo10 109.1(6) . . ?
Mo14 O34 Mo10 140.8(8) . . ?
Mo6 O34 Mo87 109.9(8) . . ?
Mo14 O34 Mo87 19.3(8) . . ?
Mo10 O34 Mo87 137.0(9) . . ?
Mo6 O34 Mo88 108.9(8) . . ?
Mo14 O34 Mo88 137.9(10) . . ?
Mo10 O34 Mo88 17.3(10) . . ?
Mo87 O34 Mo88 127.0(14) . . ?
Mo82 O35 Mo20 27.5(11) . . ?
Mo82 O35 V1 135.6(14) . . ?
Mo20 O35 V1 152.5(9) . . ?
Mo82 O35 K3 95.2(9) . . ?
Mo20 O35 K3 98.9(6) . . ?
V1 O35 K3 106.0(6) . . ?
Mo31 O36 Mo49 115.7(6) . . ?
Mo33 O37 Mo23 140.1(8) . . ?
Mo33 O37 Mo43 109.4(6) . . ?
Mo23 O37 Mo43 108.4(7) . . ?
Mo45 O38 Mo48 102.9(6) . . ?
Mo45 O38 Mo47 107.6(7) . . ?
Mo48 O38 Mo47 88.4(5) . . ?
Mo51 O40 Mo49 109.7(7) . . ?
Mo51 O40 Mo27 141.4(7) . . ?
Mo49 O40 Mo27 108.6(6) . . ?
Mo43 O42 Mo23 103.2(6) . . ?
Mo43 O42 Mo44 109.5(6) . . ?
Mo23 O42 Mo44 89.9(5) . . ?
Mo31 O43 Mo34 103.5(8) . . ?
Mo31 O43 Mo50 108.1(6) . . ?
Mo34 O43 Mo50 89.3(5) . . ?
S15 O44 S15 125(3) . 6 ?
S15 O44 S14 66.6(15) . . ?
S15 O44 S14 66.6(15) 6 . ?
S15 O44 S16 65(2) . . ?
S15 O44 S16 120(2) 6 . ?
S14 O44 S16 121.0(19) . . ?
S15 O44 S16 120(2) . 6 ?
S15 O44 S16 65(2) 6 6 ?
S14 O44 S16 121.0(19) . 6 ?
S16 O44 S16 62(3) . 6 ?
S15 O44 Mo1 113.2(15) . . ?
S15 O44 Mo1 113.2(15) 6 . ?
S14 O44 Mo1 118.1(12) . . ?
S16 O44 Mo1 111.1(18) . . ?
S16 O44 Mo1 111.1(18) 6 . ?
S8 O45 S7 60.7(16) . . ?
S8 O45 Mo13 117.5(14) . . ?
S7 O45 Mo13 117.3(13) . . ?
Mo49 O48 K1 144.1(7) . . ?
Mo85 O49 Mo12 22.7(10) . . ?
Mo85 O49 V9 134.1(12) . . ?
Mo12 O49 V9 148.8(9) . . ?
Mo85 O49 K3 97.7(8) . . ?
Mo12 O49 K3 100.0(6) . . ?
V9 O49 K3 106.4(6) . . ?
Mo83 O51 Mo15 19.1(8) . . ?
Mo83 O51 V3 143.1(12) . . ?
Mo15 O51 V3 151.5(8) . . ?
Mo83 O51 K6 95.4(7) . . ?
Mo15 O51 K6 100.4(6) . . ?
V3 O51 K6 105.5(6) . . ?
Mo7 O52 V8 154.2(8) . . ?
Mo7 O52 K1 97.9(6) . . ?
V8 O52 K1 104.7(6) . . ?
Mo7 O53 V9 148.2(8) . . ?
Mo7 O53 K1 98.7(6) . . ?
V9 O53 K1 104.4(5) . . ?
Mo7 O53 K2 93.1(5) . . ?
V9 O53 K2 104.0(6) . . ?
K1 O53 K2 99.7(5) . . ?
Mo51 O54 Mo50 142.6(7) . . ?
Mo51 O54 Mo49 102.3(6) . . ?
Mo50 O54 Mo49 102.3(6) . . ?
Mo51 O54 Mo31 102.2(6) . . ?
Mo50 O54 Mo31 102.5(5) . . ?
Mo49 O54 Mo31 96.4(5) . . ?
Mo44 O55 Mo34 158.5(9) . . ?
Mo19 O56 Mo2 109.6(8) . . ?
Mo19 O56 Mo86 24.3(19) . . ?
Mo2 O56 Mo86 108.7(10) . . ?
Mo19 O56 Mo17 108.9(7) . . ?
Mo2 O56 Mo17 141.2(8) . . ?
Mo86 O56 Mo17 108.0(9) . . ?
Mo19 O56 Mo81 110.1(8) . . ?
Mo2 O56 Mo81 21.0(10) . . ?
Mo86 O56 Mo81 100.4(15) . . ?
Mo17 O56 Mo81 137.0(10) . . ?
Mo19 O56 Mo84 110.6(8) . . ?
Mo2 O56 Mo84 135.7(10) . . ?
Mo86 O56 Mo84 100.5(13) . . ?
Mo17 O56 Mo84 21.7(8) . . ?
Mo81 O56 Mo84 122.6(14) . . ?
Mo5 O57 Mo18 109.2(6) . . ?
Mo5 O57 Mo8 109.1(7) . . ?
Mo18 O57 Mo8 141.6(7) . . ?
Mo5 O57 Mo94 108.5(8) . . ?
Mo18 O57 Mo94 138.7(9) . . ?
Mo8 O57 Mo94 18.8(9) . . ?
Mo5 O57 Mo93 109.6(6) . . ?
Mo18 O57 Mo93 19.3(4) . . ?
Mo8 O57 Mo93 137.5(8) . . ?
Mo94 O57 Mo93 126.9(12) . . ?
Mo50 O58 Mo23 156.8(9) . . ?
S5 O59 S3 59.9(19) . . ?
S5 O59 Mo88 120.5(15) . . ?
S3 O59 Mo88 116.3(19) . . ?
S5 O59 Mo10 117.1(12) . . ?
S3 O59 Mo10 114.0(17) . . ?
Mo88 O59 Mo10 3.6(6) . . ?
Mo35 O61 Mo28 109.3(7) . . ?
Mo35 O61 Mo30 141.7(8) . . ?
Mo28 O61 Mo30 108.1(7) . . ?
S14 O62 S15 64.2(14) . . ?
S14 O62 Mo3 121.1(9) . . ?
S15 O62 Mo3 113.6(14) . . ?
Mo10 O63 Mo88 1.4(5) . . ?
Mo37 O64 Mo44 109.4(9) . 2_655 ?
Mo37 O64 Mo32 108.8(7) . . ?
Mo44 O64 Mo32 140.8(7) 2_655 . ?
Mo87 O65 Mo14 22.1(9) . . ?
Mo87 O65 V7 140.9(12) . . ?
Mo14 O65 V7 153.5(9) . . ?
Mo87 O65 K4 96.0(8) . 2_656 ?
Mo14 O65 K4 97.9(7) . 2_656 ?
V7 O65 K4 106.7(6) . 2_656 ?
S16 O67 S15 65(2) . . ?
S16 O67 Mo7 114.4(18) . . ?
S15 O67 Mo7 113.6(14) . . ?
Mo6 O68 Mo11 110.1(6) . . ?
Mo6 O68 Mo14 108.4(8) . . ?
Mo11 O68 Mo14 141.4(8) . . ?
Mo6 O68 Mo87 107.9(8) . . ?
Mo11 O68 Mo87 138.2(9) . . ?
Mo14 O68 Mo87 18.9(8) . . ?
Mo17 O70 Mo84 2.4(4) . . ?
Mo9 O71 V8 151.2(8) . . ?
Mo9 O71 K1 99.7(6) . . ?
V8 O71 K1 104.6(6) . . ?
Mo34 O73 Mo46 137.7(8) . . ?
Mo34 O73 Mo31 111.1(7) . . ?
Mo46 O73 Mo31 109.8(7) . . ?
Mo32 O74 Mo34 149.1(10) . 2_655 ?
Mo3 O76 V9 150.3(8) . . ?
Mo3 O76 K3 99.4(6) . . ?
V9 O76 K3 105.8(5) . . ?
Mo88 O77 Mo10 20.6(12) . . ?
Mo88 O77 V2 142.9(15) . 2_656 ?
Mo10 O77 V2 153.3(9) . 2_656 ?
Mo88 O77 K8 96.0(8) . . ?
Mo10 O77 K8 98.5(6) . . ?
V2 O77 K8 106.7(6) 2_656 . ?
Mo26 O78 Mo33 122.5(8) . . ?
Mo11 O79 V7 152.1(9) . . ?
Mo11 O79 K5 99.4(6) . . ?
V7 O79 K5 106.0(6) . . ?
Mo43 O80 Mo33 102.3(6) . . ?
Mo43 O80 Mo26 107.8(6) . . ?
Mo33 O80 Mo26 89.4(5) . . ?
Mo53 O82 Mo37 96.2(9) . . ?
Mo53 O82 Mo32 151.6(10) . . ?
Mo37 O82 Mo32 110.7(7) . . ?
Mo53 O82 Mo52 25.2(3) . . ?
Mo37 O82 Mo52 113.9(8) . . ?
Mo32 O82 Mo52 134.5(11) . . ?
Mo19 O83 Mo86 0.3(8) . . ?
Mo93 O84 Mo18 22.7(5) . . ?
Mo93 O84 V4 139.5(10) . . ?
Mo18 O84 V4 151.7(9) . . ?
Mo93 O84 K8 96.4(7) . . ?
Mo18 O84 K8 99.4(6) . . ?
V4 O84 K8 106.7(6) . . ?
Mo47 O86 Mo24 108.9(8) . . ?
Mo47 O86 Mo42 141.7(9) . . ?
Mo24 O86 Mo42 108.1(6) . . ?
Mo87 O87 Mo14 22.7(10) . . ?
Mo87 O87 V2 141.5(13) . 2_656 ?
Mo14 O87 V2 153.4(9) . 2_656 ?
Mo87 O87 K4 97.9(9) . 2_656 ?
Mo14 O87 K4 99.3(7) . 2_656 ?
V2 O87 K4 106.2(6) 2_656 2_656 ?
Mo26 O88 Mo37 109.7(6) 2_655 . ?
Mo26 O88 Mo40 140.6(8) 2_655 . ?
Mo37 O88 Mo40 108.3(8) . . ?
Mo29 O89 Mo95 20.8(11) . . ?
Mo29 O89 Mo28 123.5(15) . . ?
Mo95 O89 Mo28 103(2) . . ?
Mo4 O90 Mo90 23.4(12) . . ?
Mo4 O90 V2 152.7(10) . . ?
Mo90 O90 V2 138.6(14) . . ?
Mo4 O90 K4 99.0(6) . . ?
Mo90 O90 K4 97.9(9) . . ?
V2 O90 K4 106.4(6) . . ?
S7 O91 S6 66.0(14) . . ?
S7 O91 S9 118.5(19) . . ?
S6 O91 S9 119.3(16) . . ?
S7 O91 S8 62.4(17) . . ?
S6 O91 S8 120.0(16) . . ?
S9 O91 S8 66.3(17) . . ?
S7 O91 S10 121(2) . . ?
S6 O91 S10 66.5(19) . . ?
S9 O91 S10 62(2) . . ?
S8 O91 S10 119(2) . . ?
S7 O91 Mo5 116.4(13) . . ?
S6 O91 Mo5 114.8(10) . . ?
S9 O91 Mo5 113.8(14) . . ?
S8 O91 Mo5 114.1(13) . . ?
S10 O91 Mo5 114.2(18) . . ?
Mo40 O92 Mo33 147.9(8) . . ?
Mo40 O92 K10 89.4(8) . . ?
Mo33 O92 K10 121.3(9) . . ?
Mo40 O92 K9 106.8(10) . . ?
Mo33 O92 K9 105.2(10) . . ?
K10 O92 K9 21.8(8) . . ?
Mo4 O93 Mo90 1.1(5) . . ?
Mo15 O94 Mo83 3.0(4) . . ?
Mo92 O95 Mo39 22.5(15) . . ?
Mo92 O95 Mo65 154.6(12) . . ?
Mo39 O95 Mo65 152.0(10) . . ?
Mo92 O95 Mo66 156(2) . . ?
Mo39 O95 Mo66 135.9(12) . . ?
Mo65 O95 Mo66 28.1(4) . . ?
Mo22 O97 Mo25 122.0(8) . . ?
Mo85 O98 Mo12 22.5(9) . . ?
Mo85 O98 V6 138.3(12) . . ?
Mo12 O98 V6 151.2(8) . . ?
Mo85 O98 K3 96.0(7) . . ?
Mo12 O98 K3 99.9(6) . . ?
V6 O98 K3 105.4(6) . . ?
Mo26 O99 Mo44 142.1(8) . . ?
Mo26 O99 Mo37 104.0(5) . 2_655 ?
Mo44 O99 Mo37 103.6(7) . 2_655 ?
Mo26 O99 Mo43 101.9(6) . . ?
Mo44 O99 Mo43 101.2(5) . . ?
Mo37 O99 Mo43 94.8(6) 2_655 . ?
Mo91 O101 Mo16 19.8(4) . . ?
Mo91 O101 V8 142.9(10) . . ?
Mo16 O101 V8 152.9(8) . . ?
Mo91 O101 K6 96.0(6) . . ?
Mo16 O101 K6 99.3(6) . . ?
V8 O101 K6 105.5(6) . . ?
S16 O102 S16 63(3) 6 . ?
S16 O102 Mo91 116.4(19) 6 . ?
S16 O102 Mo91 116.4(19) . . ?
S16 O102 Mo16 113.3(19) 6 . ?
S16 O102 Mo16 113.3(19) . . ?
Mo91 O102 Mo16 3.7(4) . . ?
Mo31 O103 Mo46 103.0(6) . . ?
Mo31 O103 Mo51 107.5(6) . . ?
Mo46 O103 Mo51 88.7(4) . . ?
Mo13 O104 V9 150.0(8) . . ?
Mo13 O104 K1 99.4(6) . . ?
V9 O104 K1 105.1(5) . . ?
S4 O106 S3 60.8(18) . . ?
S4 O106 Mo9 117.6(11) . . ?
S3 O106 Mo9 113.9(17) . . ?
S3 O107 S4 64.4(19) . . ?
S3 O107 S5 64(2) . . ?
S4 O107 S5 118.3(15) . . ?
S3 O107 S2 122(2) . . ?
S4 O107 S2 66.6(17) . . ?
S5 O107 S2 120.4(19) . . ?
S3 O107 S1 122(2) . . ?
S4 O107 S1 119.3(16) . . ?
S5 O107 S1 66.8(15) . . ?
S2 O107 S1 62.7(18) . . ?
S3 O107 Mo6 113.8(18) . . ?
S4 O107 Mo6 114.1(10) . . ?
S5 O107 Mo6 115.8(12) . . ?
S2 O107 Mo6 112.6(15) . . ?
S1 O107 Mo6 114.5(12) . . ?
Mo16 O109 Mo91 1.5(4) . . ?
Mo11 O111 V3 151.1(9) . . ?
Mo11 O111 K5 99.6(6) . . ?
V3 O111 K5 106.3(7) . . ?
Mo93 O113 Mo18 22.9(5) . . ?
Mo93 O113 V5 144.8(10) . . ?
Mo18 O113 V5 155.2(9) . . ?
Mo93 O113 K8 95.9(7) . . ?
Mo18 O113 K8 98.5(6) . . ?
V5 O113 K8 105.8(7) . . ?
Mo93 O114 S8 119.9(14) . . ?
Mo93 O114 S9 119.8(15) . . ?
S8 O114 S9 61.8(16) . . ?
Mo93 O114 Mo18 4.2(4) . . ?
S8 O114 Mo18 116.6(12) . . ?
S9 O114 Mo18 116.3(14) . . ?
Mo14 O115 Mo87 0.5(4) . . ?
Mo9 O117 V5 153.8(8) . . ?
Mo9 O117 K1 100.1(6) . . ?
V5 O117 K1 105.8(6) . . ?
S10 O118 S9 62(2) . . ?
S10 O118 Mo94 119(2) . . ?
S9 O118 Mo94 120.2(16) . . ?
S10 O118 Mo8 117.0(18) . . ?
S9 O118 Mo8 116.7(14) . . ?
Mo94 O118 Mo8 3.6(7) . . ?
Mo2 O120 Mo81 0.7(6) . . ?
Mo18 O121 Mo93 1.2(3) . . ?
Mo8 O122 Mo94 21.9(11) . . ?
Mo8 O122 V4 153.9(8) . . ?
Mo94 O122 V4 141.1(13) . . ?
Mo8 O122 K8 97.4(6) . 2_656 ?
Mo94 O122 K8 94.7(9) . 2_656 ?
V4 O122 K8 106.1(6) . 2_656 ?
Mo12 O123 Mo85 1.6(4) . . ?
Mo35 O124 Mo25 158.2(10) . . ?
Mo88 O125 Mo10 20.8(12) . . ?
Mo88 O125 V5 146.8(12) . . ?
Mo10 O125 V5 154.5(8) . . ?
Mo88 O125 K8 97.0(8) . . ?
Mo10 O125 K8 98.4(6) . . ?
V5 O125 K8 107.0(6) . . ?
Mo5 O126 Mo4 110.0(6) . . ?
Mo5 O126 Mo90 108.7(8) . . ?
Mo4 O126 Mo90 20.6(11) . . ?
Mo5 O126 Mo8 108.5(7) . . ?
Mo4 O126 Mo8 141.5(7) . . ?
Mo90 O126 Mo8 138.1(10) . . ?
Mo5 O126 Mo94 109.3(8) . . ?
Mo4 O126 Mo94 137.0(10) . . ?
Mo90 O126 Mo94 125.6(15) . . ?
Mo8 O126 Mo94 18.9(10) . . ?
Mo49 O127 Mo39 110.0(7) . . ?
Mo49 O127 Mo27 109.7(7) . . ?
Mo39 O127 Mo27 135.6(9) . . ?
Mo49 O127 Mo92 105.3(9) . . ?
Mo39 O127 Mo92 18.8(12) . . ?
Mo27 O127 Mo92 145.0(9) . . ?
Mo22 O130 Mo47 141.2(8) . . ?
Mo22 O130 Mo24 103.7(7) . . ?
Mo47 O130 Mo24 102.5(7) . . ?
Mo22 O130 Mo45 102.2(6) . . ?
Mo47 O130 Mo45 103.2(7) . . ?
Mo24 O130 Mo45 95.5(6) . . ?
Mo43 O133 Mo37 116.4(8) . 2_655 ?
Mo90 O134 S6 120.8(14) . . ?
Mo90 O134 S10 118.3(19) . . ?
S6 O134 S10 64.1(18) . . ?
Mo90 O134 Mo4 1.8(8) . . ?
S6 O134 Mo4 119.1(10) . . ?
S10 O134 Mo4 117.1(17) . . ?
Mo50 O135 K1 143.8(8) . . ?
Mo19 O136 Mo86 24.3(18) . . ?
Mo19 O136 Mo17 109.8(6) . . ?
Mo86 O136 Mo17 108.3(11) . . ?
Mo19 O136 Mo20 109.6(7) . . ?
Mo86 O136 Mo20 108.3(11) . . ?
Mo17 O136 Mo20 140.5(8) . . ?
Mo19 O136 Mo82 109.2(8) . . ?
Mo86 O136 Mo82 98.6(15) . . ?
Mo17 O136 Mo82 135.4(10) . . ?
Mo20 O136 Mo82 22.6(9) . . ?
Mo19 O136 Mo84 110.6(7) . . ?
Mo86 O136 Mo84 100.1(15) . . ?
Mo17 O136 Mo84 21.6(7) . . ?
Mo20 O136 Mo84 134.8(9) . . ?
Mo82 O136 Mo84 120.6(12) . . ?
Mo20 O138 Mo82 27.3(11) . . ?
Mo20 O138 V6 152.3(8) . . ?
Mo82 O138 V6 136.4(14) . . ?
Mo20 O138 K3 99.0(6) . . ?
Mo82 O138 K3 94.2(8) . . ?
V6 O138 K3 106.1(7) . . ?
Mo8 O139 Mo94 0.9(5) . . ?
S2 O140 S4 62.5(16) . . ?
S2 O140 Mo83 118.8(17) . . ?
S4 O140 Mo83 119.0(13) . . ?
S2 O140 Mo15 114.3(16) . . ?
S4 O140 Mo15 115.5(11) . . ?
Mo83 O140 Mo15 5.0(4) . . ?
Mo86 O141 S12 113(2) . 6 ?
Mo86 O141 S12 113(2) . . ?
S12 O141 S12 64(3) 6 . ?
Mo86 O141 S11 114.7(15) . . ?
S12 O141 S11 120(2) 6 . ?
S12 O141 S11 65.0(18) . . ?
Mo86 O141 S11 114.7(15) . 6 ?
S12 O141 S11 65.0(18) 6 6 ?
S12 O141 S11 120(2) . 6 ?
S11 O141 S11 121(3) . 6 ?
Mo86 O141 S13 114(2) . . ?
S12 O141 S13 121(2) 6 . ?
S12 O141 S13 121(2) . . ?
S11 O141 S13 65.5(15) . . ?
S11 O141 S13 65.5(15) 6 . ?
Mo86 O141 Mo19 0.0(14) . . ?
S12 O141 Mo19 113.3(16) 6 . ?
S12 O141 Mo19 113.3(16) . . ?
S11 O141 Mo19 114.6(14) . . ?
S11 O141 Mo19 114.6(14) 6 . ?
S13 O141 Mo19 114.4(16) . . ?
S6 O142 Mo85 123.1(13) . . ?
S6 O142 S7 61.2(13) . . ?
Mo85 O142 S7 119.0(14) . . ?
S6 O142 Mo12 118.9(11) . . ?
Mo85 O142 Mo12 4.4(6) . . ?
S7 O142 Mo12 116.5(12) . . ?
Mo84 O144 S11 125.1(18) . . ?
Mo84 O144 S12 121.5(17) . . ?
S11 O144 S12 63.8(18) . . ?
Mo84 O144 Mo17 7.2(7) . . ?
S11 O144 Mo17 119.1(15) . . ?
S12 O144 Mo17 116.2(15) . . ?
Mo42 O145 Mo46 148.9(8) . . ?
Mo36 O148 Mo38 153.0(10) . . ?
Mo94 O150 Mo8 22.3(12) . . ?
Mo94 O150 V2 139.7(14) . . ?
Mo8 O150 V2 152.6(8) . . ?
Mo94 O150 K8 97.9(9) . 2_656 ?
Mo8 O150 K8 99.1(7) . 2_656 ?
V2 O150 K8 106.5(6) . 2_656 ?
S12 O151 S12 63(3) . 6 ?
S12 O151 Mo81 117.9(18) . . ?
S12 O151 Mo81 117.9(18) 6 . ?
S12 O151 Mo2 114.5(16) . . ?
S12 O151 Mo2 114.6(16) 6 . ?
Mo81 O151 Mo2 4.1(9) . . ?
Mo26 O152 Mo33 158.5(11) 2_655 . ?
Mo84 O157 Mo17 26.1(10) . . ?
Mo84 O157 V6 137.6(13) . . ?
Mo17 O157 V6 151.3(8) . . ?
Mo84 O157 K4 94.6(8) . . ?
Mo17 O157 K4 99.5(6) . . ?
V6 O157 K4 107.1(7) . . ?
Mo84 O162 Mo17 26.5(10) . . ?
Mo84 O162 V7 139.7(14) . 2_656 ?
Mo17 O162 V7 153.4(10) . 2_656 ?
Mo84 O162 K4 94.0(8) . . ?
Mo17 O162 K4 98.4(6) . . ?
V7 O162 K4 106.9(7) 2_656 . ?
Mo45 O164 Mo25 102.7(6) . . ?
Mo45 O164 Mo22 107.8(7) . . ?
Mo25 O164 Mo22 88.5(5) . . ?
Mo89 O166 Mo35 133.9(15) . . ?
Mo89 O166 Mo38 15.0(8) . . ?
Mo35 O166 Mo38 120.8(10) . . ?
Mo45 O167 Mo24 118.3(8) . . ?
Mo49 O169 Mo21 111.3(7) . . ?
Mo49 O169 Mo92 107.3(9) . . ?
Mo21 O169 Mo92 140.8(10) . . ?
Mo49 O169 Mo39 108.6(7) . . ?
Mo21 O169 Mo39 138.3(8) . . ?
Mo92 O169 Mo39 18.8(12) . . ?
Mo82 O170 S13 121.6(18) . . ?
Mo82 O170 S11 121.1(17) . . ?
S13 O170 S11 63.1(17) . . ?
Mo82 O170 Mo20 5.2(8) . . ?
S13 O170 Mo20 117.8(15) . . ?
S11 O170 Mo20 116.6(14) . . ?
Mo30 O172 Mo25 148.6(8) . . ?
Mo30 O172 K7 100.7(7) . . ?
Mo25 O172 K7 110.7(7) . . ?
Mo92 O174 Mo39 2.8(7) . . ?
Mo27 O175 Mo69 156.0(12) . . ?
Mo27 O175 Mo70 143.0(12) . . ?
Mo69 O175 Mo70 26.3(5) . . ?
Mo27 O175 K7 99.7(8) . . ?
Mo69 O175 K7 101.5(8) . . ?
Mo70 O175 K7 115.3(9) . . ?
Mo22 O177 Mo24 108.7(7) . . ?
Mo22 O177 Mo36 143.9(9) . . ?
Mo24 O177 Mo36 105.6(8) . . ?
Mo95 O180 Mo29 18.6(11) . . ?
Mo95 O180 Mo38 99.8(8) . . ?
Mo29 O180 Mo38 102.0(7) . . ?
Mo95 O180 Mo35 92.1(19) . . ?
Mo29 O180 Mo35 110.3(10) . . ?
Mo38 O180 Mo35 91.7(7) . . ?
Mo22 O183 Mo38 152.9(13) . . ?
Mo22 O183 Mo89 173.8(11) . . ?
Mo38 O183 Mo89 25.5(5) . . ?
Mo95 O184 Mo38 108.0(7) . 6_565 ?
Mo95 O184 Mo38 108.0(7) . . ?
Mo38 O184 Mo38 140.1(15) 6_565 . ?
Mo95 O184 Mo29 17.6(11) . . ?
Mo38 O184 Mo29 109.8(7) 6_565 . ?
Mo38 O184 Mo29 109.8(7) . . ?
Mo95 O184 Mo89 105.5(12) . 6_565 ?
Mo38 O184 Mo89 21.5(4) 6_565 6_565 ?
Mo38 O184 Mo89 128.4(16) . 6_565 ?
Mo29 O184 Mo89 113.9(8) . 6_565 ?
Mo95 O184 Mo89 105.5(12) . . ?
Mo38 O184 Mo89 128.4(16) 6_565 . ?
Mo38 O184 Mo89 21.5(4) . . ?
Mo29 O184 Mo89 113.9(8) . . ?
Mo89 O184 Mo89 111.3(16) 6_565 . ?
Mo30 O185 Mo71 151.0(12) . . ?
Mo30 O185 Mo72 147.8(11) . . ?
Mo71 O185 Mo72 29.1(5) . . ?
Mo30 O185 K7 97.4(8) . . ?
Mo71 O185 K7 98.7(7) . . ?
Mo72 O185 K7 114.8(8) . . ?
Mo28 O186 Mo41 109.6(8) . . ?
Mo28 O186 Mo30 110.9(7) . . ?
Mo41 O186 Mo30 137.0(9) . . ?
Mo39 O187 Mo92 22.0(14) . . ?
Mo39 O187 Mo70 129.2(14) . . ?
Mo92 O187 Mo70 150(2) . . ?
Mo39 O187 Mo69 149.3(13) . . ?
Mo92 O187 Mo69 157.1(12) . . ?
Mo70 O187 Mo69 29.2(6) . . ?
Mo32 O190 Mo63 150.0(12) . . ?
Mo32 O190 Mo73 140.5(12) . . ?
Mo63 O190 Mo73 21.6(7) . . ?
Mo39 O192 Mo92 2.0(7) . . ?
Mo95 O193 Mo35 101.3(7) . 6_565 ?
Mo95 O193 Mo35 101.3(7) . . ?
Mo35 O193 Mo35 141.0(14) 6_565 . ?
Mo95 O193 Mo28 99.5(13) . . ?
Mo35 O193 Mo28 103.5(7) 6_565 . ?
Mo35 O193 Mo28 103.5(7) . . ?
Mo29 O195 Mo95 2.8(7) . . ?
Mo40 O196 Mo67 159.3(11) . . ?
Mo40 O196 Mo68 146.0(14) . . ?
Mo67 O196 Mo68 25.2(6) . . ?
Mo40 O196 K10 103.5(11) . . ?
Mo67 O196 K10 94.4(9) . . ?
Mo68 O196 K10 108.8(8) . . ?
Mo40 O196 K9 93.1(11) . . ?
Mo67 O196 K9 102.4(11) . . ?
Mo68 O196 K9 120.6(9) . . ?
K10 O196 K9 15.0(8) . . ?
Mo54 O197 Mo24 116.8(10) . . ?
Mo54 O197 Mo36 134.8(11) . . ?
Mo24 O197 Mo36 108.1(9) . . ?
Mo54 O197 Mo55 16.3(5) . . ?
Mo24 O197 Mo55 108.6(9) . . ?
Mo36 O197 Mo55 142.0(10) . . ?
Mo24 O198 Mo55 121.1(11) . . ?
Mo24 O198 Mo42 110.8(10) . . ?
Mo55 O198 Mo42 125.1(11) . . ?
Mo24 O198 Mo54 102.4(10) . . ?
Mo55 O198 Mo54 21.1(4) . . ?
Mo42 O198 Mo54 145.8(12) . . ?
Mo89 O202 Mo38 29.9(6) . . ?
Mo42 O203 Mo64 136.8(13) . . ?
Mo53 O206 Mo37 106.6(10) . . ?
Mo53 O206 Mo40 142.6(12) . . ?
Mo37 O206 Mo40 110.8(9) . . ?
Mo53 O206 Mo52 21.1(5) . . ?
Mo37 O206 Mo52 107.9(9) . . ?
Mo40 O206 Mo52 135.4(10) . . ?
Mo36 O207 Mo62 146.0(14) . . ?
Mo36 O207 Mo61 137.0(14) . . ?
Mo62 O207 Mo61 15.6(4) . . ?
Mo21 O208 Mo65 153.2(13) . . ?
Mo21 O208 Mo66 150.5(13) . . ?
Mo65 O208 Mo66 25.1(4) . . ?
Mo21 O208 K10 105.0(11) . . ?
Mo65 O208 K10 92.2(10) . . ?
Mo66 O208 K10 104.5(10) . . ?
Mo21 O208 K9 93.2(11) . . ?
Mo65 O208 K9 98.5(11) . . ?
Mo66 O208 K9 115.8(11) . . ?
K10 O208 K9 16.7(7) . . ?
Mo41 O209 Mo72 153.5(18) . . ?
Mo41 O209 Mo71 153.3(16) . . ?
Mo72 O209 Mo71 32.0(7) . . ?
O214 O211 Mo53 97(4) . . ?
O214 O211 O215 160(5) . . ?
Mo53 O211 O215 76(3) . . ?
O214 O211 Mo52 123(4) . . ?
Mo53 O211 Mo52 26.5(9) . . ?
O215 O211 Mo52 50(2) . . ?
Mo53 O212 Mo52 28.1(6) . . ?
Mo53 O212 Mo68 150.9(19) . . ?
Mo52 O212 Mo68 141.1(19) . . ?
Mo53 O212 Mo67 140.7(18) . . ?
Mo52 O212 Mo67 156.8(18) . . ?
Mo68 O212 Mo67 29.3(7) . . ?
O211 O214 O213 143(5) . . ?
O211 O214 Mo53 50(3) . . ?
O213 O214 Mo53 119(3) . . ?
O256 O215 Mo52 90(4) . . ?
O256 O215 O211 169(5) . . ?
Mo52 O215 O211 79(3) . . ?
O256 O215 Mo53 119(4) . . ?
Mo52 O215 Mo53 28.6(9) . . ?
O211 O215 Mo53 50(2) . . ?
O256 O215 Mo63 50(3) . . ?
Mo52 O215 Mo63 137(3) . . ?
O211 O215 Mo63 140(3) . . ?
Mo53 O215 Mo63 157(2) . . ?
O221 O216 Mo54 91(5) . . ?
O221 O216 Mo62 68(4) . . ?
Mo54 O216 Mo62 151(3) . . ?
O221 O216 Mo55 74(4) . . ?
Mo54 O216 Mo55 20.5(7) . . ?
Mo62 O216 Mo55 142(2) . . ?
O221 O216 Mo61 53(4) . . ?
Mo54 O216 Mo61 135(2) . . ?
Mo62 O216 Mo61 16.6(6) . . ?
Mo55 O216 Mo61 125(2) . . ?
Mo55 O217 Mo54 23.9(8) . . ?
Mo55 O217 Mo64 110(2) . . ?
Mo54 O217 Mo64 134(2) . . ?
O239 O218 Mo64 73(3) . . ?
O239 O218 O257 14(3) . . ?
Mo64 O218 O257 78(2) . . ?
O239 O218 O220 166(4) . . ?
Mo64 O218 O220 114(2) . . ?
O257 O218 O220 152(2) . . ?
O239 O218 Mo55 163(4) . . ?
Mo64 O218 Mo55 97.3(19) . . ?
O257 O218 Mo55 153(2) . . ?
O220 O218 Mo55 17.0(6) . . ?
Mo55 O220 Mo54 22.6(10) . . ?
Mo55 O220 O218 116.8(18) . . ?
Mo54 O220 O218 138.6(16) . . ?
O216 O221 Mo62 77(4) . . ?
O216 O221 Mo61 98(5) . . ?
Mo62 O221 Mo61 22.0(9) . . ?
O216 O221 Mo54 56(4) . . ?
Mo62 O221 Mo54 129(4) . . ?
Mo61 O221 Mo54 143(4) . . ?
O216 O221 Mo55 75(4) . . ?
Mo62 O221 Mo55 151(4) . . ?
Mo61 O221 Mo55 162(4) . . ?
Mo54 O221 Mo55 22.0(8) . . ?
Mo62 O231 Mo61 2.9(8) . . ?
Mo61 O232 Mo62 5.6(11) . . ?
Mo61 O233 Mo62 21.5(7) . . ?
Mo62 O234 Mo62 138(3) 6_565 . ?
Mo62 O234 Mo61 19.7(5) 6_565 6_565 ?
Mo62 O234 Mo61 132(3) . 6_565 ?
Mo62 O234 Mo61 132(3) 6_565 . ?
Mo62 O234 Mo61 19.7(5) . . ?
Mo61 O234 Mo61 119(3) 6_565 . ?
Mo63 O235 Mo73 29.9(12) . . ?
Mo73 O236 Mo63 10(3) . . ?
O218 O239 O257 154(5) . . ?
O218 O239 Mo64 76(3) . . ?
O257 O239 Mo64 112(3) . . ?
O242 O241 Mo65 83(3) . . ?
O242 O241 Mo67 69(3) . . ?
Mo65 O241 Mo67 140(3) . . ?
O242 O241 Mo66 57(3) . . ?
Mo65 O241 Mo66 26.7(7) . . ?
Mo67 O241 Mo66 117(2) . . ?
O242 O241 K10 115(4) . . ?
Mo65 O241 K10 108.6(19) . . ?
Mo67 O241 K10 109.5(19) . . ?
Mo66 O241 K10 120.2(18) . . ?
O242 O241 Mo68 47(3) . . ?
Mo65 O241 Mo68 123(2) . . ?
Mo67 O241 Mo68 22.0(8) . . ?
Mo66 O241 Mo68 97.9(17) . . ?
K10 O241 Mo68 115.2(17) . . ?
O242 O241 K9 129(4) . . ?
Mo65 O241 K9 106.9(18) . . ?
Mo67 O241 K9 113.3(18) . . ?
Mo66 O241 K9 124.2(17) . . ?
K10 O241 K9 13.3(9) . . ?
Mo68 O241 K9 123.6(16) . . ?
O241 O242 Mo67 77(3) . . ?
O241 O242 Mo66 94(3) . . ?
Mo67 O242 Mo66 146(2) . . ?
O241 O242 Mo68 109(4) . . ?
Mo67 O242 Mo68 31.9(8) . . ?
Mo66 O242 Mo68 141(2) . . ?
O241 O242 Mo65 65(3) . . ?
Mo67 O242 Mo65 132(2) . . ?
Mo66 O242 Mo65 29.5(7) . . ?
Mo68 O242 Mo65 152(2) . . ?
O241 O242 K10 45(3) . . ?
Mo67 O242 K10 89.3(17) . . ?
Mo66 O242 K10 107.5(17) . . ?
Mo68 O242 K10 111.2(17) . . ?
Mo65 O242 K10 83.8(14) . . ?
Mo67 O243 O259 148(6) . . ?
Mo67 O243 O261 81(4) . . ?
O259 O243 O261 68(5) . . ?
Mo67 O243 Mo68 7.9(15) . . ?
O259 O243 Mo68 147(5) . . ?
O261 O243 Mo68 81(4) . . ?
Mo67 O243 K10 97(3) . . ?
O259 O243 K10 110(4) . . ?
O261 O243 K10 138(4) . . ?
Mo68 O243 K10 101.9(16) . . ?
Mo68 O244 O255 159(7) . . ?
Mo68 O244 Mo67 19(2) . . ?
O255 O244 Mo67 152(5) . . ?
Mo70 O246 Mo69 5.2(13) . . ?
Mo69 O247 Mo70 33.7(13) . . ?
Mo69 O248 Mo71 147(2) . . ?
Mo69 O248 Mo70 30.0(8) . . ?
Mo71 O248 Mo70 135.1(19) . . ?
Mo69 O248 Mo72 135.4(19) . . ?
Mo71 O248 Mo72 31.9(7) . . ?
Mo70 O248 Mo72 109.7(17) . . ?
Mo69 O248 K7 103.9(14) . . ?
Mo71 O248 K7 104.6(14) . . ?
Mo70 O248 K7 119.0(15) . . ?
Mo72 O248 K7 118.5(14) . . ?
O263 O249 Mo65 120(6) . . ?
O263 O249 O258 145(5) . . ?
Mo65 O249 O258 70(3) . . ?
O263 O249 Mo66 133(5) . . ?
Mo65 O249 Mo66 13.9(14) . . ?
O258 O249 Mo66 57(2) . . ?
O263 O249 K10 82(4) . . ?
Mo65 O249 K10 79(3) . . ?
O258 O249 K10 133(3) . . ?
Mo66 O249 K10 87.7(18) . . ?
Mo66 O250 Mo65 11.3(8) . . ?
O258 O251 Mo66 83(4) . . ?
O258 O251 Mo65 55(3) . . ?
Mo66 O251 Mo65 27.5(8) . . ?
Mo52 O252 Mo53 16.8(5) . . ?
Mo72 O254 Mo71 7.3(14) . . ?
O244 O255 Mo68 9(3) . . ?
O215 O256 Mo73 134(5) . . ?
O215 O256 Mo63 106(4) . . ?
Mo73 O256 Mo63 29.8(11) . . ?
O215 O256 Mo52 57(3) . . ?
Mo73 O256 Mo52 155(3) . . ?
Mo63 O256 Mo52 155(3) . . ?
O215 O256 Mo53 41(3) . . ?
Mo73 O256 Mo53 156(2) . . ?
Mo63 O256 Mo53 141(2) . . ?
Mo52 O256 Mo53 16.0(6) . . ?
O239 O257 O218 12(2) . . ?
O239 O257 Mo64 42(2) . . ?
O218 O257 Mo64 45.8(15) . . ?
O239 O257 Mo73 130(3) . 2_655 ?
O218 O257 Mo73 142(2) . 2_655 ?
Mo64 O257 Mo73 106.1(15) . 2_655 ?
O251 O258 Mo65 95(4) . . ?
O251 O258 O249 133(5) . . ?
Mo65 O258 O249 38(2) . . ?
O251 O258 Mo66 63(4) . . ?
Mo65 O258 Mo66 31.9(9) . . ?
O249 O258 Mo66 70(2) . . ?
O243 O259 O261 65(5) . . ?
O243 O259 Mo67 15(3) . . ?
O261 O259 Mo67 51(4) . . ?
Mo68 O260 Mo67 29.6(12) . . ?
O243 O261 O259 47(4) . . ?
O243 O261 Mo67 38(3) . . ?
O259 O261 Mo67 84(5) . . ?
O243 O261 Mo68 62(3) . . ?
O259 O261 Mo68 108(5) . . ?
Mo67 O261 Mo68 25.4(16) . . ?
Mo71 O262 Mo72 38.5(17) . . ?
O249 O263 Mo65 32(4) . . ?
O249 O263 K10 81(4) . . ?
Mo65 O263 K10 73.2(14) . . ?
K9 O334 K10 5.1(16) . . ?
O407 O406 S6 98(4) . . ?
O407 O406 S7 45(3) . . ?
S6 O406 S7 53(2) . . ?
O406 O407 O408 125(7) . . ?
O406 O407 S7 95(5) . . ?
O408 O407 S7 99(5) . . ?
O406 O407 S8 117(5) . . ?
O408 O407 S8 47(4) . . ?
S7 O407 S8 52(3) . . ?
O407 O408 S8 90(5) . . ?
S11 O411 O412 97(6) . . ?
S11 O411 S13 57(3) . . ?
O412 O411 S13 114(6) . . ?
S12 O412 O412 94(4) . 6 ?
S12 O412 O411 90(6) . . ?
O412 O412 O411 104(4) 6 . ?
O5 S1 O107 104.8(18) . . ?
O5 S1 O21 129(2) . . ?
O107 S1 O21 101.0(17) . . ?
O5 S1 S2 59.0(17) . . ?
O107 S1 S2 57.8(17) . . ?
O21 S1 S2 158(2) . . ?
O5 S1 S5 159(2) . . ?
O107 S1 S5 54.6(13) . . ?
O21 S1 S5 59.8(14) . . ?
S2 S1 S5 106(2) . . ?
O107 S2 O5 106(2) . . ?
O107 S2 O140 103(2) . . ?
O5 S2 O140 132(3) . . ?
O107 S2 S1 59.5(17) . . ?
O5 S2 S1 58.3(17) . . ?
O140 S2 S1 163(3) . . ?
O107 S2 S4 55.0(15) . . ?
O5 S2 S4 160(3) . . ?
O140 S2 S4 59.1(16) . . ?
S1 S2 S4 107(2) . . ?
O107 S3 S5 58.8(19) . . ?
O107 S3 S4 57.9(18) . . ?
S5 S3 S4 109(3) . . ?
O107 S3 O59 106(3) . . ?
S5 S3 O59 59.0(19) . . ?
S4 S3 O59 164(3) . . ?
O107 S3 O106 104(3) . . ?
S5 S3 O106 163(3) . . ?
S4 S3 O106 57.2(18) . . ?
O59 S3 O106 132(3) . . ?
O404 S4 O107 108(2) . . ?
O404 S4 O106 102(2) . . ?
O107 S4 O106 107.9(15) . . ?
O404 S4 S3 85(3) . . ?
O107 S4 S3 57.7(18) . . ?
O106 S4 S3 62.1(18) . . ?
O404 S4 O140 106(2) . . ?
O107 S4 O140 105.6(14) . . ?
O106 S4 O140 126.3(15) . . ?
S3 S4 O140 163(2) . . ?
O404 S4 S2 89(2) . . ?
O107 S4 S2 58.5(15) . . ?
O106 S4 S2 165(2) . . ?
S3 S4 S2 110(2) . . ?
O140 S4 S2 58.4(15) . . ?
O405 S5 O107 110(4) . . ?
O405 S5 O59 106(3) . . ?
O107 S5 O59 106.4(17) . . ?
O405 S5 S3 90(4) . . ?
O107 S5 S3 57.4(19) . . ?
O59 S5 S3 61.1(19) . . ?
O405 S5 O21 104(3) . . ?
O107 S5 O21 102.0(16) . . ?
O59 S5 O21 127.5(18) . . ?
S3 S5 O21 159(2) . . ?
O405 S5 S1 86(3) . . ?
O107 S5 S1 58.5(14) . . ?
O59 S5 S1 164(2) . . ?
S3 S5 S1 109(2) . . ?
O21 S5 S1 57.3(14) . . ?
O406 S6 O91 105(2) . . ?
O406 S6 O142 105(2) . . ?
O91 S6 O142 104.8(13) . . ?
O406 S6 O134 109(2) . . ?
O91 S6 O134 104.5(13) . . ?
O142 S6 O134 127.1(15) . . ?
O406 S6 S7 82(2) . . ?
O91 S6 S7 55.0(13) . . ?
O142 S6 S7 63.3(14) . . ?
O134 S6 S7 159.2(18) . . ?
O406 S6 S10 86(3) . . ?
O91 S6 S10 57.6(17) . . ?
O142 S6 S10 162(2) . . ?
O134 S6 S10 60.3(17) . . ?
S7 S6 S10 104(2) . . ?
O406 S6 Mo90 138(2) . . ?
O91 S6 Mo90 93.4(11) . . ?
O142 S6 Mo90 106.3(12) . . ?
O134 S6 Mo90 29.4(9) . . ?
S7 S6 Mo90 137.3(15) . . ?
S10 S6 Mo90 72.9(17) . . ?
O406 S6 Mo85 133(2) . . ?
O91 S6 Mo85 94.0(10) . . ?
O142 S6 Mo85 28.6(8) . . ?
O134 S6 Mo85 106.8(11) . . ?
S7 S6 Mo85 74.6(12) . . ?
S10 S6 Mo85 138.9(19) . . ?
Mo90 S6 Mo85 80.7(9) . . ?
O407 S7 O91 104(3) . . ?
O407 S7 S8 82(3) . . ?
O91 S7 S8 61.7(17) . . ?
O407 S7 O45 106(3) . . ?
O91 S7 O45 106.6(19) . . ?
S8 S7 O45 58.1(16) . . ?
O407 S7 S6 85(3) . . ?
O91 S7 S6 59.1(14) . . ?
S8 S7 S6 114(2) . . ?
O45 S7 S6 164(2) . . ?
O407 S7 O142 108(3) . . ?
O91 S7 O142 101.8(18) . . ?
S8 S7 O142 163(2) . . ?
O45 S7 O142 128.6(19) . . ?
S6 S7 O142 55.5(12) . . ?
O407 S7 O406 40(3) . . ?
O91 S7 O406 83(2) . . ?
S8 S7 O406 103(2) . . ?
O45 S7 O406 146(2) . . ?
S6 S7 O406 44.8(18) . . ?
O142 S7 O406 78.8(19) . . ?
O408 S8 O45 105(4) . . ?
O408 S8 O91 110(3) . . ?
O45 S8 O91 104.6(19) . . ?
O408 S8 S7 88(3) . . ?
O45 S8 S7 61.2(17) . . ?
O91 S8 S7 55.9(15) . . ?
O408 S8 O114 104(3) . . ?
O45 S8 O114 130(2) . . ?
O91 S8 O114 103.5(19) . . ?
S7 S8 O114 159(2) . . ?
O408 S8 S9 87(3) . . ?
O45 S8 S9 161(2) . . ?
O91 S8 S9 56.5(16) . . ?
S7 S8 S9 105(2) . . ?
O114 S8 S9 59.5(16) . . ?
O408 S8 O407 42(3) . . ?
O45 S8 O407 85(2) . . ?
O91 S8 O407 79(2) . . ?
S7 S8 O407 46(2) . . ?
O114 S8 O407 141(3) . . ?
S9 S8 O407 94(3) . . ?
O91 S9 O118 106(2) . . ?
O91 S9 S10 60(2) . . ?
O118 S9 S10 59(2) . . ?
O91 S9 O114 103(2) . . ?
O118 S9 O114 129(2) . . ?
S10 S9 O114 163(3) . . ?
O91 S9 S8 57.2(16) . . ?
O118 S9 S8 163(3) . . ?
S10 S9 S8 110(3) . . ?
O114 S9 S8 58.7(16) . . ?
O118 S10 O91 106(3) . . ?
O118 S10 S9 60(2) . . ?
O91 S10 S9 58(2) . . ?
O118 S10 O134 132(3) . . ?
O91 S10 O134 99(3) . . ?
S9 S10 O134 158(3) . . ?
O118 S10 S6 161(3) . . ?
O91 S10 S6 55.9(17) . . ?
S9 S10 S6 107(3) . . ?
O134 S10 S6 55.6(16) . . ?
O118 S10 Mo94 31.1(13) . . ?
O91 S10 Mo94 95(2) . . ?
S9 S10 Mo94 74(2) . . ?
O134 S10 Mo94 107(2) . . ?
S6 S10 Mo94 137(2) . . ?
O411 S11 O144 110(4) . . ?
O411 S11 O141 103(4) . . ?
O144 S11 O141 104(2) . . ?
O411 S11 O170 106(4) . . ?
O144 S11 O170 129(2) . . ?
O141 S11 O170 102(2) . . ?
O411 S11 S12 86(4) . . ?
O144 S11 S12 59.7(17) . . ?
O141 S11 S12 56.7(17) . . ?
O170 S11 S12 158(3) . . ?
O411 S11 S13 82(4) . . ?
O144 S11 S13 161(3) . . ?
O141 S11 S13 57.8(17) . . ?
O170 S11 S13 57.0(16) . . ?
S12 S11 S13 108(2) . . ?
O411 S11 Mo86 133(4) . . ?
O144 S11 Mo86 90.7(17) . . ?
O141 S11 Mo86 30.6(13) . . ?
O170 S11 Mo86 90.0(17) . . ?
S12 S11 Mo86 68.9(18) . . ?
S13 S11 Mo86 70.5(17) . . ?
O411 S11 Mo82 133(4) . . ?
O144 S11 Mo82 108.3(18) . . ?
O141 S11 Mo82 93.5(17) . . ?
O170 S11 Mo82 27.2(10) . . ?
S12 S11 Mo82 138(2) . . ?
S13 S11 Mo82 70.2(16) . . ?
Mo86 S11 Mo82 71.4(14) . . ?
O411 S11 Mo84 137(4) . . ?
O144 S11 Mo84 26.8(11) . . ?
O141 S11 Mo84 95.5(17) . . ?
O170 S11 Mo84 108.3(17) . . ?
S12 S11 Mo84 72.1(17) . . ?
S13 S11 Mo84 140(2) . . ?
Mo86 S11 Mo84 72.5(12) . . ?
Mo82 S11 Mo84 83.7(12) . . ?
O412 S12 O141 108(4) . . ?
O412 S12 O151 102(4) . . ?
O141 S12 O151 106(2) . . ?
O412 S12 O144 105(4) . . ?
O141 S12 O144 102(2) . . ?
O151 S12 O144 132(2) . . ?
O412 S12 S12 86(4) . 6 ?
O141 S12 S12 58.2(13) . 6 ?
O151 S12 S12 58.3(13) . 6 ?
O144 S12 S12 160.3(13) . 6 ?
O412 S12 S11 86(4) . . ?
O141 S12 S11 58.2(17) . . ?
O151 S12 S11 164(3) . . ?
O144 S12 S11 56.4(17) . . ?
S12 S12 S11 109.3(16) 6 . ?
O412 S12 Mo86 139(4) . . ?
O141 S12 Mo86 31.5(14) . . ?
O151 S12 Mo86 94.1(18) . . ?
O144 S12 Mo86 90.9(16) . . ?
S12 S12 Mo86 70.7(9) 6 . ?
S11 S12 Mo86 71.6(18) . . ?
O412 S12 Mo81 133(4) . . ?
O141 S12 Mo81 95.9(17) . . ?
O151 S12 Mo81 31.4(12) . . ?
O144 S12 Mo81 109.3(17) . . ?
S12 S12 Mo81 72.3(7) 6 . ?
S11 S12 Mo81 140(2) . . ?
Mo86 S12 Mo81 72.0(14) . . ?
O412 S12 Mo84 132(4) . . ?
O141 S12 Mo84 95.9(16) . . ?
O151 S12 Mo84 111.0(18) . . ?
O144 S12 Mo84 28.0(10) . . ?
S12 S12 Mo84 140.9(9) 6 . ?
S11 S12 Mo84 71.8(16) . . ?
Mo86 S12 Mo84 73.1(12) . . ?
Mo81 S12 Mo84 83.1(12) . . ?
O141 S13 O170 103.3(15) . . ?
O141 S13 O170 103.3(15) . 6 ?
O170 S13 O170 129(3) . 6 ?
O141 S13 S11 56.7(15) . . ?
O170 S13 S11 59.9(13) . . ?
O170 S13 S11 159(3) 6 . ?
O141 S13 S11 56.7(15) . 6 ?
O170 S13 S11 159(3) . 6 ?
O170 S13 S11 59.9(13) 6 6 ?
S11 S13 S11 106(3) . 6 ?
O141 S13 O411 77(3) . . ?
O170 S13 O411 82(2) . . ?
O170 S13 O411 147(3) 6 . ?
S11 S13 O411 41(2) . . ?
S11 S13 O411 96(3) 6 . ?
O141 S13 O411 77(3) . 6 ?
O170 S13 O411 147(3) . 6 ?
O170 S13 O411 82(2) 6 6 ?
S11 S13 O411 96(3) . 6 ?
S11 S13 O411 41(2) 6 6 ?
O411 S13 O411 65(5) . 6 ?
O141 S13 Mo86 30.4(15) . . ?
O170 S13 Mo86 90.7(15) . . ?
O170 S13 Mo86 90.7(15) 6 . ?
S11 S13 Mo86 69.6(17) . . ?
S11 S13 Mo86 69.6(17) 6 . ?
O411 S13 Mo86 103(3) . . ?
O411 S13 Mo86 103(3) 6 . ?
O141 S13 Mo82 94.5(14) . . ?
O170 S13 Mo82 27.5(10) . . ?
O170 S13 Mo82 107.5(19) 6 . ?
S11 S13 Mo82 72.7(14) . . ?
S11 S13 Mo82 139(2) 6 . ?
O411 S13 Mo82 106(2) . . ?
O411 S13 Mo82 169(3) 6 . ?
Mo86 S13 Mo82 71.9(13) . . ?
O141 S13 Mo82 94.5(14) . 6 ?
O170 S13 Mo82 107.5(19) . 6 ?
O170 S13 Mo82 27.5(10) 6 6 ?
S11 S13 Mo82 139(2) . 6 ?
S11 S13 Mo82 72.7(14) 6 6 ?
O411 S13 Mo82 169(3) . 6 ?
O411 S13 Mo82 106(2) 6 6 ?
Mo86 S13 Mo82 71.9(13) . 6 ?
Mo82 S13 Mo82 82.5(15) . 6 ?
O414 S14 O62 108.2(11) . 6 ?
O414 S14 O62 108.2(11) . . ?
O62 S14 O62 125.3(16) 6 . ?
O414 S14 O44 107(2) . . ?
O62 S14 O44 103.3(9) 6 . ?
O62 S14 O44 103.3(9) . . ?
O414 S14 S15 87.7(19) . . ?
O62 S14 S15 157.7(17) 6 . ?
O62 S14 S15 60.1(13) . . ?
O44 S14 S15 56.0(13) . . ?
O414 S14 S15 87.7(19) . 6 ?
O62 S14 S15 60.1(13) 6 6 ?
O62 S14 S15 157.7(17) . 6 ?
O44 S14 S15 56.0(13) . 6 ?
S15 S14 S15 106(3) . 6 ?
O44 S15 O67 108(2) . . ?
O44 S15 O62 101(2) . . ?
O67 S15 O62 135(2) . . ?
O44 S15 S14 57.4(14) . . ?
O67 S15 S14 165(3) . . ?
O62 S15 S14 55.7(13) . . ?
O44 S15 S16 60(2) . . ?
O67 S15 S16 58(2) . . ?
O62 S15 S16 161(3) . . ?
S14 S15 S16 109(2) . . ?
O67 S16 O102 133(3) . . ?
O67 S16 O44 103(3) . . ?
O102 S16 O44 107(3) . . ?
O67 S16 S16 161.5(17) . 6 ?
O102 S16 S16 58.3(17) . 6 ?
O44 S16 S16 58.9(16) . 6 ?
O67 S16 S15 58(2) . . ?
O102 S16 S15 161(3) . . ?
O44 S16 S15 54.2(19) . . ?
S16 S16 S15 107.3(19) 6 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 1.672(17) . ?
Mo1 O1 2.00(2) . ?
Mo1 O22 2.012(13) . ?
Mo1 O22 2.012(13) 6 ?
Mo1 O25 2.019(14) . ?
Mo1 O25 2.020(14) 6 ?
Mo1 O44 2.268(18) . ?
Mo2 Mo81 0.76(4) . ?
Mo2 O120 1.67(3) . ?
Mo2 O8 1.790(17) . ?
Mo2 O8 1.790(17) 6 ?
Mo2 O56 2.049(15) . ?
Mo2 O56 2.049(15) 6 ?
Mo2 O151 2.42(2) . ?
Mo2 K5 3.685(14) 5_656 ?
Mo3 O50 1.693(13) . ?
Mo3 O76 1.769(13) . ?
Mo3 O29 1.788(14) . ?
Mo3 O1 2.062(7) . ?
Mo3 O22 2.064(14) . ?
Mo3 O62 2.352(13) . ?
Mo3 K3 3.677(8) . ?
Mo4 Mo90 0.73(4) . ?
Mo4 O93 1.719(17) . ?
Mo4 O19 1.796(16) . ?
Mo4 O90 1.801(13) . ?
Mo4 O126 2.054(16) . ?
Mo4 O28 2.056(13) . ?
Mo4 O134 2.364(16) . ?
Mo4 K4 3.702(11) . ?
Mo5 O85 1.665(13) . ?
Mo5 O12 1.989(12) . ?
Mo5 O30 2.011(14) . ?
Mo5 O28 2.014(15) . ?
Mo5 O57 2.023(14) . ?
Mo5 O126 2.023(13) . ?
Mo5 O91 2.325(13) . ?
Mo6 O96 1.671(14) . ?
Mo6 O7 2.002(16) . ?
Mo6 O34 2.005(15) . ?
Mo6 O13 2.007(16) . ?
Mo6 O68 2.012(15) . ?
Mo6 O27 2.016(14) . ?
Mo6 O107 2.316(14) . ?
Mo7 O17 1.703(12) . ?
Mo7 O52 1.781(15) . ?
Mo7 O53 1.794(13) . ?
Mo7 O25 2.037(13) . ?
Mo7 O22 2.059(13) . ?
Mo7 O67 2.374(13) . ?
Mo7 K1 3.645(5) . ?
Mo7 K2 3.923(16) . ?
Mo8 Mo94 0.69(4) . ?
Mo8 O139 1.743(17) . ?
Mo8 O122 1.803(15) . ?
Mo8 O150 1.805(15) . ?
Mo8 O57 2.062(13) . ?
Mo8 O126 2.077(14) . ?
Mo8 O118 2.382(16) . ?
Mo8 K8 3.707(12) 2_656 ?
Mo9 O159 1.706(14) . ?
Mo9 O117 1.764(16) . ?
Mo9 O71 1.795(14) . ?
Mo9 O7 2.056(14) . ?
Mo9 O27 2.063(16) . ?
Mo9 O106 2.375(14) . ?
Mo9 K1 3.690(5) . ?
Mo10 Mo88 0.64(4) . ?
Mo10 O63 1.693(18) . ?
Mo10 O125 1.792(16) . ?
Mo10 O77 1.793(13) . ?
Mo10 O7 2.068(13) . ?
Mo10 O34 2.073(16) . ?
Mo10 O59 2.390(18) . ?
Mo10 K8 3.685(13) . ?
Mo11 O160 1.703(14) . ?
Mo11 O111 1.785(17) . ?
Mo11 O79 1.788(14) . ?
Mo11 O68 2.037(16) . ?
Mo11 O13 2.066(14) . ?
Mo11 O5 2.365(15) . ?
Mo11 K5 3.706(9) . ?
Mo12 Mo85 0.70(3) . ?
Mo12 O123 1.717(16) . ?
Mo12 O98 1.791(15) . ?
Mo12 O49 1.799(15) . ?
Mo12 O28 2.057(13) . ?
Mo12 O12 2.067(15) . ?
Mo12 O142 2.331(17) . ?
Mo12 K3 3.697(9) . ?
Mo13 O46 1.718(13) . ?
Mo13 O16 1.780(16) . ?
Mo13 O104 1.804(13) . ?
Mo13 O30 2.055(12) . ?
Mo13 O12 2.087(15) . ?
Mo13 O45 2.386(14) . ?
Mo13 K1 3.654(5) . ?
Mo14 Mo87 0.69(3) . ?
Mo14 O115 1.692(17) . ?
Mo14 O87 1.779(16) . ?
Mo14 O65 1.812(17) . ?
Mo14 O34 2.050(15) . ?
Mo14 O68 2.085(15) . ?
Mo14 O21 2.370(17) . ?
Mo14 K4 3.691(10) 2_656 ?
Mo15 Mo83 0.59(2) . ?
Mo15 O94 1.675(18) . ?
Mo15 O51 1.790(17) . ?
Mo15 O9 1.811(17) . ?
Mo15 O13 2.036(13) . ?
Mo15 O27 2.042(16) . ?
Mo15 O140 2.399(19) . ?
Mo15 K6 3.712(9) . ?
Mo16 Mo91 0.614(11) . ?
Mo16 O109 1.64(2) . ?
Mo16 O101 1.813(16) . ?
Mo16 O101 1.813(16) 6 ?
Mo16 O25 2.062(14) 6 ?
Mo16 O25 2.063(14) . ?
Mo16 O102 2.42(2) . ?
Mo16 K6 3.730(14) . ?
Mo17 Mo84 0.81(3) . ?
Mo17 O70 1.700(19) . ?
Mo17 O162 1.805(15) . ?
Mo17 O157 1.826(16) . ?
Mo17 O136 2.059(14) . ?
Mo17 O56 2.068(17) . ?
Mo17 O144 2.361(18) . ?
Mo17 K4 3.690(11) . ?
Mo18 Mo93 0.704(15) . ?
Mo18 O121 1.714(17) . ?
Mo18 O113 1.797(15) . ?
Mo18 O84 1.804(14) . ?
Mo18 O57 2.052(14) . ?
Mo18 O30 2.062(12) . ?
Mo18 O114 2.326(17) . ?
Mo18 K8 3.723(15) . ?
Mo19 Mo86 0.86(7) . ?
Mo19 O83 1.65(3) . ?
Mo19 O136 2.006(15) . ?
Mo19 O136 2.006(15) 6 ?
Mo19 O56 2.018(15) 6 ?
Mo19 O56 2.018(15) . ?
Mo19 O31 2.02(2) . ?
Mo19 O141 2.34(2) . ?
Mo20 Mo82 0.84(3) . ?
Mo20 O154 1.686(18) . ?
Mo20 O138 1.786(16) . ?
Mo20 O35 1.794(15) . ?
Mo20 O31 2.063(7) . ?
Mo20 O136 2.070(13) . ?
Mo20 O170 2.357(19) . ?
Mo20 K3 3.654(8) . ?
Mo21 O208 1.72(2) . ?
Mo21 O108 1.728(16) . ?
Mo21 O33 1.819(16) . ?
Mo21 O169 2.043(15) . ?
Mo21 O26 2.071(14) . ?
Mo21 O200 2.25(3) . ?
Mo21 K10 3.48(2) . ?
Mo21 K9 3.83(4) . ?
Mo22 O179 1.644(16) . ?
Mo22 O183 1.854(18) . ?
Mo22 O97 1.865(17) . ?
Mo22 O177 2.000(17) . ?
Mo22 O130 2.054(18) . ?
Mo22 O164 2.442(15) . ?
Mo23 O156 1.667(17) . ?
Mo23 O58 1.922(15) . ?
Mo23 O11 1.954(16) . ?
Mo23 O33 1.995(16) . ?
Mo23 O37 2.009(14) . ?
Mo23 O42 2.300(13) . ?
Mo23 K9 3.96(4) . ?
Mo24 O165 1.66(2) . ?
Mo24 O198 1.97(2) . ?
Mo24 O197 1.990(19) . ?
Mo24 O86 2.005(16) . ?
Mo24 O177 2.031(19) . ?
Mo24 O130 2.111(16) . ?
Mo24 O167 2.212(17) . ?
Mo24 Mo54 3.191(7) . ?
Mo25 O147 1.680(16) . ?
Mo25 O124 1.929(16) . ?
Mo25 O97 1.942(16) . ?
Mo25 O172 1.963(17) . ?
Mo25 O32 1.999(15) . ?
Mo25 O164 2.330(15) . ?
Mo25 K7 4.049(14) . ?
Mo26 O182 1.66(2) . ?
Mo26 O78 1.851(16) . ?
Mo26 O152 1.864(17) 2_655 ?
Mo26 O88 2.004(17) 2_655 ?
Mo26 O99 2.056(15) . ?
Mo26 O80 2.423(15) . ?
Mo27 O143 1.692(16) . ?
Mo27 O175 1.722(18) . ?
Mo27 O4 1.845(15) . ?
Mo27 O127 2.068(15) . ?
Mo27 O40 2.103(14) . ?
Mo27 O69 2.376(16) . ?
Mo27 K7 3.704(17) . ?
Mo28 O176 1.66(3) . ?
Mo28 O186 1.984(17) . ?
Mo28 O186 1.984(17) 6_565 ?
Mo28 O61 2.024(15) 6_565 ?
Mo28 O61 2.024(15) . ?
Mo28 O193 2.09(2) . ?
Mo28 O89 2.21(2) . ?
Mo28 Mo95 3.12(4) . ?
Mo29 Mo95 0.64(3) . ?
Mo29 O195 1.58(4) . ?
Mo29 O89 1.75(2) . ?
Mo29 O180 1.997(19) . ?
Mo29 O180 1.997(19) 6_565 ?
Mo29 O184 2.10(3) . ?
Mo30 O181 1.697(18) . ?
Mo30 O185 1.702(19) . ?
Mo30 O172 1.835(16) . ?
Mo30 O186 2.063(16) . ?
Mo30 O61 2.092(16) . ?
Mo30 O194 2.30(2) . ?
Mo30 K7 3.721(14) . ?
Mo31 O131 1.681(14) . ?
Mo31 O36 1.785(14) . ?
Mo31 O103 1.942(15) . ?
Mo31 O43 1.952(18) . ?
Mo31 O73 2.083(15) . ?
Mo31 O54 2.432(13) . ?
Mo32 O190 1.698(18) . ?
Mo32 O168 1.807(16) . ?
Mo32 O74 1.824(16) . ?
Mo32 O82 2.047(17) . ?
Mo32 O64 2.091(19) . ?
Mo32 O39 2.279(18) . ?
Mo33 O191 1.664(18) . ?
Mo33 O152 1.891(16) . ?
Mo33 O78 1.939(17) . ?
Mo33 O92 1.981(18) . ?
Mo33 O37 1.987(15) . ?
Mo33 O80 2.299(14) . ?
Mo33 K9 3.98(4) . ?
Mo34 O75 1.642(16) . ?
Mo34 O55 1.908(17) . ?
Mo34 O20 1.963(14) . ?
Mo34 O74 1.991(15) 2_655 ?
Mo34 O73 1.991(16) . ?
Mo34 O43 2.317(16) . ?
Mo35 O189 1.57(3) . ?
Mo35 O124 1.819(16) . ?
Mo35 O166 1.873(18) . ?
Mo35 O61 1.988(17) . ?
Mo35 O193 2.076(9) . ?
Mo35 O180 2.458(19) . ?
Mo35 Mo89 2.943(16) . ?
Mo35 Mo95 3.15(4) . ?
Mo36 O148 1.56(3) . ?
Mo36 O188 1.660(19) . ?
Mo36 O207 1.77(3) . ?
Mo36 O197 2.076(19) . ?
Mo36 O177 2.100(16) . ?
Mo36 O201 2.34(2) . ?
Mo37 O173 1.635(19) . ?
Mo37 O206 1.992(19) . ?
Mo37 O82 2.00(2) . ?
Mo37 O64 2.005(14) . ?
Mo37 O88 2.012(16) . ?
Mo37 O99 2.110(15) 2_655 ?
Mo37 O133 2.238(15) 2_655 ?
Mo37 Mo53 2.971(11) . ?
Mo38 Mo89 0.853(14) . ?
Mo38 O202 1.67(2) . ?
Mo38 O183 1.914(17) . ?
Mo38 O184 1.984(10) . ?
Mo38 O166 2.05(2) . ?
Mo38 O148 2.11(3) . ?
Mo38 O180 2.296(16) . ?
Mo38 Mo95 3.203(15) . ?
Mo39 Mo92 0.68(4) . ?
Mo39 O192 1.65(3) . ?
Mo39 O187 1.776(16) . ?
Mo39 O95 1.781(18) . ?
Mo39 O127 2.039(16) . ?
Mo39 O169 2.097(16) . ?
Mo39 O174 2.38(2) . ?
Mo40 O41 1.716(17) . ?
Mo40 O196 1.729(17) . ?
Mo40 O92 1.818(19) . ?
Mo40 O206 2.047(19) . ?
Mo40 O88 2.089(14) . ?
Mo40 O199 2.30(2) . ?
Mo40 K10 3.443(18) . ?
Mo40 K9 3.90(3) . ?
Mo41 O209 1.73(3) 6_565 ?
Mo41 O209 1.73(3) . ?
Mo41 O205 1.74(4) . ?
Mo41 O186 2.061(17) 6_565 ?
Mo41 O186 2.061(17) . ?
Mo41 O204 2.22(4) . ?
Mo42 O171 1.686(19) . ?
Mo42 O203 1.76(2) . ?
Mo42 O145 1.826(16) . ?
Mo42 O198 2.09(2) . ?
Mo42 O86 2.124(18) . ?
Mo42 O60 2.348(19) . ?
Mo43 O112 1.659(15) . ?
Mo43 O133 1.771(14) . ?
Mo43 O42 1.939(13) . ?
Mo43 O80 1.971(15) . ?
Mo43 O37 2.095(14) . ?
Mo43 O99 2.513(15) . ?
Mo44 O137 1.657(17) . ?
Mo44 O55 1.828(16) . ?
Mo44 O11 1.847(16) . ?
Mo44 O64 2.017(17) 2_655 ?
Mo44 O99 2.067(13) . ?
Mo44 O42 2.398(14) . ?
Mo45 O128 1.699(16) . ?
Mo45 O167 1.764(15) . ?
Mo45 O164 1.939(16) . ?
Mo45 O38 1.956(15) . ?
Mo45 O32 2.092(13) . ?
Mo45 O130 2.498(16) . ?
Mo46 O149 1.665(16) . ?
Mo46 O10 1.894(16) . ?
Mo46 O145 1.952(14) . ?
Mo46 O3 1.972(14) . ?
Mo46 O73 2.018(15) . ?
Mo46 O103 2.335(13) . ?
Mo47 O153 1.685(16) . ?
Mo47 O10 1.854(16) . ?
Mo47 O18 1.862(14) . ?
Mo47 O86 2.004(15) . ?
Mo47 O130 2.070(15) . ?
Mo47 O38 2.476(15) . ?
Mo48 O132 1.654(14) . ?
Mo48 O18 1.923(15) . ?
Mo48 O6 1.923(14) . ?
Mo48 O4 1.953(14) . ?
Mo48 O32 1.999(15) . ?
Mo48 O38 2.311(13) . ?
Mo49 O48 1.691(14) . ?
Mo49 O169 1.985(16) . ?
Mo49 O40 1.999(14) . ?
Mo49 O127 2.007(15) . ?
Mo49 O26 2.010(14) . ?
Mo49 O54 2.107(14) . ?
Mo49 O36 2.210(13) . ?
Mo50 O135 1.696(13) . ?
Mo50 O58 1.842(15) . ?
Mo50 O20 1.846(15) . ?
Mo50 O26 2.005(14) . ?
Mo50 O54 2.081(14) . ?
Mo50 O43 2.393(15) . ?
Mo50 K2 4.108(16) . ?
Mo51 O14 1.682(12) . ?
Mo51 O6 1.838(14) . ?
Mo51 O3 1.857(14) . ?
Mo51 O40 1.989(14) . ?
Mo51 O54 2.079(14) . ?
Mo51 O103 2.406(13) . ?
Mo51 K2 3.972(15) . ?
Mo52 Mo53 0.896(9) . ?
Mo52 O215 1.50(4) . ?
Mo52 O252 1.76(3) . ?
Mo52 O256 1.80(4) . ?
Mo52 O212 1.86(3) . ?
Mo52 O211 1.92(5) . ?
Mo52 O82 2.091(17) . ?
Mo52 O206 2.25(2) . ?
Mo53 O211 1.47(4) . ?
Mo53 O206 1.71(2) . ?
Mo53 O212 1.84(3) . ?
Mo53 O215 1.85(5) . ?
Mo53 O214 1.90(4) . ?
Mo53 O82 1.990(18) . ?
Mo53 O252 2.42(3) . ?
Mo53 O256 2.48(4) . ?
Mo54 Mo55 0.766(12) . ?
Mo54 O220 1.379(17) . ?
Mo54 O216 1.64(4) . ?
Mo54 O197 1.75(2) . ?
Mo54 O217 1.84(4) . ?
Mo54 O221 1.97(6) . ?
Mo54 O198 2.13(2) . ?
Mo54 O210 2.28(4) . ?
Mo55 O220 0.721(12) . ?
Mo55 O217 1.51(4) . ?
Mo55 O198 2.01(2) . ?
Mo55 O221 2.03(6) . ?
Mo55 O216 2.04(4) . ?
Mo55 O218 2.21(4) . ?
Mo55 O197 2.27(2) . ?
Mo55 O219 2.50(7) . ?
Mo55 Mo64 2.835(16) . ?
Mo61 Mo62 0.660(14) . ?
Mo61 O232 1.29(5) . ?
Mo61 O233 1.70(4) . ?
Mo61 O221 1.73(6) . ?
Mo61 O234 1.95(3) . ?
Mo61 O216 2.15(4) . ?
Mo61 O231 2.40(6) . ?
Mo61 O207 2.44(3) . ?
Mo62 O221 1.73(6) . ?
Mo62 O231 1.75(6) . ?
Mo62 O233 1.80(4) . ?
Mo62 O216 1.81(4) . ?
Mo62 O234 1.885(19) . ?
Mo62 O232 1.93(5) . ?
Mo62 O207 2.29(3) . ?
Mo63 Mo73 0.92(3) . ?
Mo63 O235 1.77(5) . ?
Mo63 O256 1.80(4) . ?
Mo63 O237 1.80(3) . ?
Mo63 O236 1.89(8) . ?
Mo63 O215 2.27(5) . ?
Mo63 O190 2.43(2) . ?
Mo64 O238 1.19(5) . ?
Mo64 O239 1.50(3) . ?
Mo64 O218 1.52(4) . ?
Mo64 O217 1.94(4) . ?
Mo64 O257 2.08(4) . ?
Mo64 O240 2.18(6) . ?
Mo64 O203 2.36(3) . ?
Mo65 Mo66 1.009(11) . ?
Mo65 O249 1.17(5) . ?
Mo65 O258 1.77(5) . ?
Mo65 O241 1.85(4) . ?
Mo65 O263 1.90(5) . ?
Mo65 O242 2.04(4) . ?
Mo65 O95 2.053(18) . ?
Mo65 O208 2.08(2) . ?
Mo65 O251 2.14(5) . ?
Mo65 O250 2.38(4) . ?
Mo65 K10 3.40(3) . ?
Mo66 O250 1.44(4) . ?
Mo66 O251 1.69(5) . ?
Mo66 O242 1.87(4) . ?
Mo66 O258 1.88(5) . ?
Mo66 O95 2.102(19) . ?
Mo66 O249 2.10(6) . ?
Mo66 O241 2.22(4) . ?
Mo66 O208 2.37(2) . ?
Mo66 K10 3.94(3) . ?
Mo67 O243 0.88(3) . ?
Mo67 Mo68 1.016(17) . ?
Mo67 O261 1.43(7) . ?
Mo67 O242 1.79(4) . ?
Mo67 O244 1.79(5) . ?
Mo67 O259 1.83(7) . ?
Mo67 O241 1.87(4) . ?
Mo67 O260 2.03(6) . ?
Mo67 O196 2.05(2) . ?
Mo67 O212 2.07(3) . ?
Mo67 K10 3.43(3) . ?
Mo68 O244 0.86(4) . ?
Mo68 O260 1.62(6) . ?
Mo68 O243 1.88(3) . ?
Mo68 O242 1.89(4) . ?
Mo68 O212 1.89(3) . ?
Mo68 O255 1.92(7) . ?
Mo68 O261 2.10(7) . ?
Mo68 O196 2.37(2) . ?
Mo68 O241 2.47(4) . ?
Mo68 K10 4.04(3) . ?
Mo69 Mo70 1.02(2) . ?
Mo69 O247 1.76(6) . ?
Mo69 O245 1.80(5) . ?
Mo69 O248 1.85(3) . ?
Mo69 O187 2.030(18) . ?
Mo69 O175 2.133(18) . ?
Mo69 O246 2.16(4) . ?
Mo69 K7 4.015(18) . ?
Mo70 O246 1.15(3) . ?
Mo70 O247 1.76(6) . ?
Mo70 O187 2.02(3) . ?
Mo70 O248 2.04(4) . ?
Mo70 O175 2.30(3) . ?
Mo71 Mo72 1.140(17) . ?
Mo71 O262 1.49(7) . ?
Mo71 O253 1.59(5) . ?
Mo71 O248 1.92(4) . ?
Mo71 O209 2.13(3) . ?
Mo71 O185 2.216(19) . ?
Mo71 O254 2.26(4) . ?
Mo71 K7 4.071(17) . ?
Mo72 O254 1.13(4) . ?
Mo72 O262 1.83(7) . ?
Mo72 O209 1.97(3) . ?
Mo72 O248 2.15(4) . ?
Mo72 O185 2.31(3) . ?
Mo73 O236 1.01(7) . ?
Mo73 O256 1.77(5) . ?
Mo73 O235 1.78(6) . ?
Mo73 O257 2.43(4) 2_655 ?
Mo73 O190 2.47(3) . ?
Mo81 O151 1.67(5) . ?
Mo81 O8 1.75(2) 6 ?
Mo81 O8 1.75(2) . ?
Mo81 O56 2.12(3) . ?
Mo81 O56 2.12(3) 6 ?
Mo81 O120 2.44(6) . ?
Mo81 S12 2.84(5) . ?
Mo81 S12 2.84(5) 6 ?
Mo81 Mo86 3.21(4) . ?
Mo81 K5 3.59(3) 5_656 ?
Mo82 O170 1.53(4) . ?
Mo82 O35 1.75(3) . ?
Mo82 O138 1.79(3) . ?
Mo82 O31 2.17(2) . ?
Mo82 O136 2.20(2) . ?
Mo82 S13 2.83(4) . ?
Mo82 S11 2.87(5) . ?
Mo82 K3 3.54(2) . ?
Mo83 O9 1.688(19) . ?
Mo83 O51 1.72(2) . ?
Mo83 O140 1.84(4) . ?
Mo83 O27 2.11(2) . ?
Mo83 O13 2.143(18) . ?
Mo83 O94 2.25(4) . ?
Mo83 K6 3.551(13) . ?
Mo84 O144 1.58(4) . ?
Mo84 O162 1.73(2) . ?
Mo84 O157 1.77(2) . ?
Mo84 O56 2.20(3) . ?
Mo84 O136 2.21(2) . ?
Mo84 O70 2.51(4) . ?
Mo84 S11 2.87(5) . ?
Mo84 S12 2.87(5) . ?
Mo84 K4 3.536(19) . ?
Mo85 O142 1.65(4) . ?
Mo85 O49 1.72(2) . ?
Mo85 O98 1.78(2) . ?
Mo85 O12 2.13(2) . ?
Mo85 O28 2.15(2) . ?
Mo85 O123 2.41(4) . ?
Mo85 S6 2.89(4) . ?
Mo85 K3 3.594(16) . ?
Mo86 O141 1.48(8) . ?
Mo86 O56 2.06(3) 6 ?
Mo86 O56 2.06(3) . ?
Mo86 O136 2.06(3) . ?
Mo86 O136 2.06(3) 6 ?
Mo86 O31 2.09(5) . ?
Mo86 O83 2.50(8) . ?
Mo86 S12 2.61(7) . ?
Mo86 S12 2.61(7) 6 ?
Mo86 S11 2.66(7) . ?
Mo86 S11 2.66(7) 6 ?
Mo87 O21 1.68(4) . ?
Mo87 O87 1.74(2) . ?
Mo87 O65 1.80(2) . ?
Mo87 O34 2.08(2) . ?
Mo87 O68 2.12(2) . ?
Mo87 O115 2.38(4) . ?
Mo87 K4 3.634(17) 2_656 ?
Mo88 O125 1.72(2) . ?
Mo88 O59 1.76(5) . ?
Mo88 O77 1.77(2) . ?
Mo88 O7 2.09(2) . ?
Mo88 O34 2.14(2) . ?
Mo88 O63 2.33(5) . ?
Mo88 K8 3.61(2) . ?
Mo89 O166 1.32(3) . ?
Mo89 O202 1.64(3) . ?
Mo89 O183 1.94(2) . ?
Mo89 O184 2.29(2) . ?
Mo90 O134 1.63(5) . ?
Mo90 O19 1.81(3) . ?
Mo90 O90 1.82(2) . ?
Mo90 O126 2.06(3) . ?
Mo90 O28 2.07(3) . ?
Mo90 O93 2.45(5) . ?
Mo90 S6 2.86(4) . ?
Mo90 K4 3.68(2) . ?
Mo91 O101 1.731(15) . ?
Mo91 O101 1.731(15) 6 ?
Mo91 O102 1.82(3) . ?
Mo91 O25 2.108(15) 6 ?
Mo91 O25 2.108(15) . ?
Mo91 O109 2.25(3) . ?
Mo91 K6 3.597(14) . ?
Mo92 O95 1.70(3) . ?
Mo92 O174 1.70(6) . ?
Mo92 O187 1.81(3) . ?
Mo92 O169 2.08(3) . ?
Mo92 O127 2.11(3) . ?
Mo92 O192 2.33(7) . ?
Mo93 O114 1.64(3) . ?
Mo93 O113 1.749(17) . ?
Mo93 O84 1.775(17) . ?
Mo93 O57 2.131(17) . ?
Mo93 O30 2.146(17) . ?
Mo93 O121 2.42(3) . ?
Mo93 K8 3.631(17) . ?
Mo94 O118 1.71(4) . ?
Mo94 O150 1.75(2) . ?
Mo94 O122 1.81(2) . ?
Mo94 O126 2.11(2) . ?
Mo94 O57 2.13(2) . ?
Mo94 O139 2.43(5) . ?
Mo94 S10 2.89(6) . ?
Mo94 K8 3.64(2) 2_656 ?
Mo95 O89 1.77(3) . ?
Mo95 O180 1.877(17) . ?
Mo95 O180 1.877(17) 6_565 ?
Mo95 O184 1.97(3) . ?
Mo95 O193 1.99(6) . ?
Mo95 O195 2.21(7) . ?
Mo95 Mo35 3.15(4) 6_565 ?
Mo95 Mo38 3.202(15) 6_565 ?
V1 O161 1.87(2) . ?
V1 O35 1.958(15) 6 ?
V1 O35 1.958(15) . ?
V1 O29 1.959(14) . ?
V1 O29 1.959(14) 6 ?
V1 O129 2.02(2) . ?
V1 K3 3.937(8) 6 ?
V1 K3 3.937(8) . ?
V2 O163 1.906(16) . ?
V2 O90 1.948(13) . ?
V2 O77 1.950(14) 2_656 ?
V2 O150 1.956(16) . ?
V2 O87 1.963(17) 2_656 ?
V2 O116 2.030(16) . ?
V2 K4 3.981(12) . ?
V2 K8 3.989(14) 2_656 ?
V3 O81 1.89(2) . ?
V3 O111 1.967(16) . ?
V3 O111 1.967(16) 6 ?
V3 O51 1.974(16) 6 ?
V3 O51 1.975(16) . ?
V3 O146 2.01(2) . ?
V3 K6 3.962(13) . ?
V3 K5 3.992(16) . ?
V4 O72 1.89(2) . ?
V4 O122 1.936(15) . ?
V4 O122 1.936(15) 2_656 ?
V4 O84 1.962(12) . ?
V4 O84 1.962(12) 2_656 ?
V4 O47 2.06(2) . ?
V4 K8 4.008(13) 2_656 ?
V4 K8 4.008(13) . ?
V5 O24 1.742(14) . ?
V5 O113 1.956(14) . ?
V5 O125 1.958(15) . ?
V5 O16 1.966(16) . ?
V5 O117 1.976(16) . ?
V5 O119 2.209(15) . ?
V5 K1 3.970(6) . ?
V5 K8 4.007(13) . ?
V6 O155 1.928(17) . ?
V6 O157 1.938(15) . ?
V6 O19 1.958(15) . ?
V6 O138 1.969(15) . ?
V6 O98 1.971(15) . ?
V6 O100 1.972(16) . ?
V6 K3 3.951(8) . ?
V6 K4 3.951(10) . ?
V7 O178 1.910(18) . ?
V7 O65 1.929(17) . ?
V7 O162 1.937(15) 2_656 ?
V7 O79 1.954(14) . ?
V7 O8 1.971(17) 2_656 ?
V7 O158 2.004(19) . ?
V7 K5 3.978(9) . ?
V7 K4 3.984(12) 2_656 ?
V8 O110 1.901(14) . ?
V8 O52 1.951(16) . ?
V8 O9 1.960(16) . ?
V8 O101 1.964(14) . ?
V8 O71 1.967(14) . ?
V8 O105 2.010(13) . ?
V8 K1 3.923(6) . ?
V8 K6 3.983(8) . ?
V9 O23 1.633(13) . ?
V9 O104 1.975(14) . ?
V9 O53 1.980(13) . ?
V9 O49 1.983(15) . ?
V9 O76 1.987(14) . ?
V9 O15 2.228(14) . ?
V9 K1 3.907(6) . ?
V9 K3 3.978(9) . ?
K1 O304 2.83(2) . ?
K1 O48 2.832(15) . ?
K1 O135 2.854(14) . ?
K1 O104 2.896(15) . ?
K1 O53 2.912(14) . ?
K1 O71 2.936(15) . ?
K1 O14 2.944(15) . ?
K1 O52 2.945(15) . ?
K1 O117 2.946(15) . ?
K1 O16 2.952(13) . ?
K2 O15 2.78(2) . ?
K2 O3 2.88(2) . ?
K2 O17 2.93(2) . ?
K2 O20 3.068(19) . ?
K2 O53 3.394(19) . ?
K3 O311 2.78(3) . ?
K3 O337 2.851(19) . ?
K3 O35 2.918(17) . ?
K3 O138 2.922(16) . ?
K3 O49 2.933(17) . ?
K3 O98 2.940(16) . ?
K3 O76 2.946(16) . ?
K3 O29 2.969(16) . ?
K4 O301 2.86(2) 2_656 ?
K4 O157 2.921(17) . ?
K4 O87 2.958(18) 2_656 ?
K4 O90 2.96(2) . ?
K4 O162 2.97(2) . ?
K4 O19 2.966(16) . ?
K4 O65 2.975(17) 2_656 ?
K4 Mo87 3.634(17) 2_656 ?
K4 Mo14 3.691(10) 2_656 ?
K5 O305 2.82(4) . ?
K5 O8 2.940(19) 2_656 ?
K5 O8 2.940(19) 5_656 ?
K5 O111 2.96(2) 6 ?
K5 O111 2.96(2) . ?
K5 O79 2.968(16) 6 ?
K5 O79 2.968(16) . ?
K5 Mo81 3.59(3) 5_656 ?
K5 Mo2 3.685(14) 5_656 ?
K5 Mo11 3.706(9) 6 ?
K5 V7 3.978(9) 6 ?
K6 O340 2.84(6) 6 ?
K6 O340 2.84(6) . ?
K6 O306 2.94(3) . ?
K6 O51 2.946(18) . ?
K6 O51 2.946(18) 6 ?
K6 O9 2.978(15) . ?
K6 O9 2.978(15) 6 ?
K6 O101 2.978(17) 6 ?
K6 O101 2.979(17) . ?
K6 Mo83 3.551(13) 6 ?
K7 O314 2.87(4) . ?
K7 O172 2.91(2) . ?
K7 O4 2.98(2) . ?
K7 O175 3.00(3) . ?
K7 O185 3.10(2) . ?
K7 O248 3.14(4) . ?
K8 O308 2.88(3) . ?
K8 O77 2.96(2) . ?
K8 O150 2.966(18) 2_656 ?
K8 O125 2.969(18) . ?
K8 O84 2.98(2) . ?
K8 O113 3.006(19) . ?
K8 O122 3.014(18) 2_656 ?
K8 Mo94 3.64(2) 2_656 ?
K8 Mo8 3.707(12) 2_656 ?
K9 K10 1.12(4) . ?
K9 O334 1.61(6) . ?
K9 O33 2.90(5) . ?
K9 O92 2.97(3) . ?
K9 O312 2.98(4) . ?
K9 O241 3.24(6) . ?
K9 O208 3.33(5) . ?
K9 O196 3.40(4) . ?
K10 O241 2.32(5) . ?
K10 O196 2.60(3) . ?
K10 O208 2.61(3) . ?
K10 O334 2.71(6) . ?
K10 O92 2.94(2) . ?
K10 O242 2.95(5) . ?
K10 O33 2.96(3) . ?
K10 O243 3.21(4) . ?
K10 O249 3.42(5) . ?
K10 O263 3.42(5) . ?
O1 Mo3 2.063(7) 6 ?
O5 S1 1.67(3) . ?
O5 S2 1.68(4) . ?
O8 V7 1.971(17) 2_656 ?
O8 K5 2.940(19) 5_656 ?
O21 S1 1.72(3) . ?
O21 S5 1.76(3) . ?
O31 Mo20 2.063(7) 6 ?
O31 Mo82 2.17(2) 6 ?
O44 S15 1.59(4) . ?
O44 S15 1.59(4) 6 ?
O44 S14 1.62(3) . ?
O44 S16 1.71(5) . ?
O44 S16 1.71(5) 6 ?
O45 S8 1.62(3) . ?
O45 S7 1.67(3) . ?
O59 S5 1.67(3) . ?
O59 S3 1.71(5) . ?
O62 S14 1.620(16) . ?
O62 S15 1.70(4) . ?
O64 Mo44 2.017(17) 2_655 ?
O65 K4 2.975(17) 2_656 ?
O67 S16 1.67(5) . ?
O67 S15 1.67(4) . ?
O74 Mo34 1.991(15) 2_655 ?
O77 V2 1.951(14) 2_656 ?
O87 V2 1.963(17) 2_656 ?
O87 K4 2.958(18) 2_656 ?
O88 Mo26 2.004(17) 2_655 ?
O91 S7 1.56(3) . ?
O91 S6 1.63(3) . ?
O91 S9 1.64(4) . ?
O91 S8 1.66(4) . ?
O91 S10 1.66(5) . ?
O99 Mo37 2.110(15) 2_655 ?
O102 S16 1.68(5) 6 ?
O102 S16 1.68(5) . ?
O106 S4 1.63(3) . ?
O106 S3 1.72(5) . ?
O107 S3 1.59(5) . ?
O107 S4 1.59(3) . ?
O107 S5 1.61(3) . ?
O107 S2 1.66(4) . ?
O107 S1 1.69(3) . ?
O114 S8 1.75(4) . ?
O114 S9 1.76(4) . ?
O118 S10 1.65(5) . ?
O118 S9 1.67(4) . ?
O122 K8 3.014(18) 2_656 ?
O133 Mo37 2.238(15) 2_655 ?
O134 S6 1.66(3) . ?
O134 S10 1.75(5) . ?
O140 S2 1.71(4) . ?
O140 S4 1.73(3) . ?
O141 S12 1.64(4) 6 ?
O141 S12 1.64(4) . ?
O141 S11 1.67(4) . ?
O141 S11 1.67(4) 6 ?
O141 S13 1.69(4) . ?
O142 S6 1.63(2) . ?
O142 S7 1.77(3) . ?
O144 S11 1.65(4) . ?
O144 S12 1.71(4) . ?
O150 K8 2.966(18) 2_656 ?
O151 S12 1.64(4) . ?
O151 S12 1.64(4) 6 ?
O152 Mo26 1.864(17) 2_655 ?
O162 V7 1.936(15) 2_656 ?
O170 S13 1.71(2) . ?
O170 S11 1.76(4) . ?
O184 Mo38 1.984(10) 6_565 ?
O184 Mo89 2.29(2) 6_565 ?
O193 Mo35 2.076(9) 6_565 ?
O211 O214 1.05(5) . ?
O211 O215 1.53(6) . ?
O213 O214 1.59(6) . ?
O215 O256 0.98(5) . ?
O216 O221 1.06(6) . ?
O218 O239 0.82(4) . ?
O218 O257 1.76(5) . ?
O218 O220 1.78(4) . ?
O234 Mo62 1.885(19) 6_565 ?
O234 Mo61 1.95(3) 6_565 ?
O239 O257 0.98(3) . ?
O241 O242 1.09(5) . ?
O243 O259 1.02(6) . ?
O243 O261 1.27(8) . ?
O244 O255 1.09(6) . ?
O249 O263 1.03(5) . ?
O249 O258 1.78(7) . ?
O251 O258 1.05(5) . ?
O257 Mo73 2.43(4) 2_655 ?
O259 O261 1.30(9) . ?
O301 K4 2.86(2) 2_656 ?
O302 O343 0.90(3) . ?
O313 O341 1.11(4) . ?
O404 S4 1.55(5) . ?
O405 S5 1.52(8) . ?
O406 O407 1.39(9) . ?
O406 S6 1.53(6) . ?
O406 S7 2.14(6) . ?
O407 O408 1.41(10) . ?
O407 S7 1.51(8) . ?
O407 S8 2.09(8) . ?
O408 S8 1.54(8) . ?
O411 S11 1.43(8) . ?
O411 O412 1.58(12) . ?
O411 S13 2.14(9) . ?
O412 S12 1.51(10) . ?
O412 O412 1.52(18) 6 ?
O414 S14 1.48(6) . ?
S1 S2 1.74(5) . ?
S1 S5 1.82(4) . ?
S2 S4 1.78(4) . ?
S3 S5 1.69(5) . ?
S3 S4 1.69(5) . ?
S6 S7 1.74(4) . ?
S6 S10 1.81(5) . ?
S7 S8 1.67(4) . ?
S8 S9 1.80(5) . ?
S9 S10 1.70(6) . ?
S11 S12 1.78(5) . ?
S11 S13 1.82(4) . ?
S12 S12 1.73(7) 6 ?
S13 O170 1.71(2) 6 ?
S13 S11 1.82(4) 6 ?
S13 O411 2.14(9) 6 ?
S13 Mo82 2.83(4) 6 ?
S14 O62 1.620(16) 6 ?
S14 S15 1.77(4) . ?
S14 S15 1.77(4) 6 ?
S15 S16 1.79(6) . ?
S16 S16 1.77(10) 6 ?
|
1101224.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-17 16:41:39 +0200 (Thu, 17 Mar 2016) $
#$Revision: 178244 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101224.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_1101224
loop_
_publ_author_name
'Chi, Eun Ok'
'Ok, Kang Min'
'Porter, Yetta'
'Halasyamani, P. Shiv'
_publ_contact_author_address
;
Department of Chemistry
University of Houston
4800 Calhoun
TX 77204-5003 USA
;
_publ_contact_author_email psh@uh.edu
_publ_contact_author_fax 1(713)7432787
_publ_contact_author_name 'Halasyamani, P. Shiv'
_publ_contact_author_phone 1(713)7430796
_publ_section_title
;
Na~2~Te~3~Mo~3~O~16~: A New Molybdenum Tellurite with Second-Harmonic
Generating and Pyroelectric Properties
;
_journal_coden_ASTM CMATEX
_journal_issue 8
_journal_name_full 'Chemistry of Materials'
_journal_page_first 2070
_journal_page_last 2074
_journal_paper_doi 10.1021/cm052614e
_journal_volume 18
_journal_year 2006
_chemical_absolute_configuration unk
_chemical_formula_sum 'Mo3 Na2 O16 Te3'
_chemical_formula_weight 972.6
_chemical_name_systematic 'Sodium molybdenum tellurium oxide'
_space_group_IT_number 5
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'I 2y'
_symmetry_space_group_name_H-M 'I 1 2 1'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 97.387(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.3373(10)
_cell_length_b 11.2668(16)
_cell_length_c 8.2369(18)
_cell_measurement_temperature 293.0(2)
_cell_volume 675.3(2)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293.0(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0368
_diffrn_reflns_av_unetI/netI 0.0268
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 2082
_diffrn_reflns_theta_full 25
_diffrn_reflns_theta_max 27.97
_diffrn_reflns_theta_min 3.08
_exptl_absorpt_coefficient_mu 9.25
_exptl_absorpt_correction_T_max 0.637
_exptl_absorpt_correction_T_min 0.411
_exptl_absorpt_correction_type Psi-scan
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 4.783
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Block
_exptl_crystal_F_000 864
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_refine_diff_density_max 1.183
_refine_diff_density_min -1.597
_refine_diff_density_rms 0.288
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.47(4)
_refine_ls_extinction_coef 0.0022(3)
_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 1.081
_refine_ls_matrix_type full
_refine_ls_number_parameters 112
_refine_ls_number_reflns 1404
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.08
_refine_ls_R_factor_all 0.0337
_refine_ls_R_factor_gt 0.0331
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+8.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0886
_refine_ls_wR_factor_ref 0.0891
_reflns_number_gt 1380
_reflns_number_total 1404
_reflns_threshold_expression >2\(I)
_cod_data_source_file cm052614esi20060214_024006.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'I 2'
_cod_database_code 1101224
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_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
Na1 Na 0.5 1.0659(12) 0 0.056(4) Uani 1 2 d S . .
Na2 Na 0.5 0.9771(7) -0.5 0.0186(15) Uani 1 2 d S . .
Te1 Te 0 0.98861(7) 0 0.0102(2) Uani 1 2 d S . .
Te2 Te 0.27903(9) 0.82680(7) -0.21870(7) 0.0104(2) Uani 1 1 d . . .
Mo1 Mo 1 1.07971(11) -0.5 0.0095(3) Uani 1 2 d S . .
Mo2 Mo 0.25515(16) 0.74092(7) 0.22691(11) 0.0104(2) Uani 1 1 d . . .
O1 O 0.0950(9) 0.8773(7) 0.1636(8) 0.0152(14) Uani 1 1 d . . .
O2 O 0.2392(10) 0.9670(6) -0.0991(9) 0.0139(14) Uani 1 1 d . . .
O3 O 0.3096(9) 0.7327(6) -0.0281(8) 0.0136(13) Uani 1 1 d . . .
O4 O 0.5206(9) 0.8707(6) -0.2330(9) 0.0150(14) Uani 1 1 d . . .
O5 O -0.0417(9) 1.1283(6) -0.2816(8) 0.0137(14) Uani 1 1 d . . .
O6 O 1.1852(10) 0.9862(6) -0.4503(8) 0.0154(14) Uani 1 1 d . . .
O7 O 0.2742(11) 0.7487(8) 0.4358(9) 0.0241(18) Uani 1 1 d . . .
O8 O 0.0834(11) 0.6374(7) 0.1910(11) 0.0243(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.014(5) 0.041(6) 0.109(11) 0 -0.007(5) 0
Na2 0.015(3) 0.024(4) 0.017(3) 0 0.001(3) 0
Te1 0.0119(4) 0.0065(5) 0.0126(5) 0 0.0030(4) 0
Te2 0.0122(3) 0.0099(3) 0.0093(3) 0.0013(3) 0.0019(2) 0.0005(3)
Mo1 0.0121(9) 0.0082(6) 0.0083(7) 0 0.0020(5) 0
Mo2 0.0117(4) 0.0099(4) 0.0103(5) 0.0005(4) 0.0034(3) 0.0018(3)
O1 0.011(3) 0.019(4) 0.015(3) 0.002(3) 0.001(2) 0.002(3)
O2 0.014(3) 0.008(3) 0.018(3) -0.004(3) -0.003(3) -0.002(3)
O3 0.018(3) 0.012(3) 0.011(3) 0.004(3) 0.002(3) 0.006(3)
O4 0.009(3) 0.015(3) 0.022(4) 0.007(3) 0.005(3) 0.000(3)
O5 0.018(3) 0.011(3) 0.012(3) 0.004(3) 0.002(3) 0.004(3)
O6 0.022(4) 0.008(3) 0.018(3) -0.002(3) 0.010(3) 0.005(3)
O7 0.028(4) 0.034(5) 0.011(3) 0.000(3) 0.006(3) 0.012(4)
O8 0.024(4) 0.013(4) 0.036(4) 0.001(3) 0.005(3) -0.005(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.006 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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 Na1 O2 121.3(7) . 2_655 ?
O2 Na1 O8 101.2(3) . 4 ?
O2 Na1 O8 95.0(3) 2_655 4 ?
O2 Na1 O8 95.0(2) . 3_554 ?
O2 Na1 O8 101.2(3) 2_655 3_554 ?
O8 Na1 O8 146.7(7) 4 3_554 ?
O2 Na1 O4 60.7(3) . . ?
O2 Na1 O4 75.8(4) 2_655 . ?
O8 Na1 O4 147.4(5) 4 . ?
O8 Na1 O4 65.6(2) 3_554 . ?
O2 Na1 O4 75.8(4) . 2_655 ?
O2 Na1 O4 60.7(3) 2_655 2_655 ?
O8 Na1 O4 65.6(2) 4 2_655 ?
O8 Na1 O4 147.4(5) 3_554 2_655 ?
O4 Na1 O4 82.9(5) . 2_655 ?
O2 Na1 O7 146.4(3) . 3_554 ?
O2 Na1 O7 81.1(3) 2_655 3_554 ?
O8 Na1 O7 101.2(4) 4 3_554 ?
O8 Na1 O7 53.8(3) 3_554 3_554 ?
O4 Na1 O7 108.0(2) . 3_554 ?
O4 Na1 O7 136.7(2) 2_655 3_554 ?
O2 Na1 O7 81.1(3) . 4 ?
O2 Na1 O7 146.4(3) 2_655 4 ?
O8 Na1 O7 53.8(3) 4 4 ?
O8 Na1 O7 101.2(4) 3_554 4 ?
O4 Na1 O7 136.7(2) . 4 ?
O4 Na1 O7 108.0(2) 2_655 4 ?
O7 Na1 O7 92.4(5) 3_554 4 ?
O2 Na1 Te2 29.5(3) . . ?
O2 Na1 Te2 96.9(5) 2_655 . ?
O8 Na1 Te2 122.9(3) 4 . ?
O8 Na1 Te2 84.0(2) 3_554 . ?
O4 Na1 Te2 31.87(17) . . ?
O4 Na1 Te2 72.6(3) 2_655 . ?
O7 Na1 Te2 135.81(16) 3_554 . ?
O7 Na1 Te2 110.08(16) 4 . ?
O2 Na1 Te2 96.9(5) . 2_655 ?
O2 Na1 Te2 29.5(3) 2_655 2_655 ?
O8 Na1 Te2 84.0(2) 4 2_655 ?
O8 Na1 Te2 122.9(3) 3_554 2_655 ?
O4 Na1 Te2 72.6(3) . 2_655 ?
O4 Na1 Te2 31.87(17) 2_655 2_655 ?
O7 Na1 Te2 110.08(16) 3_554 2_655 ?
O7 Na1 Te2 135.81(16) 4 2_655 ?
Te2 Na1 Te2 80.1(3) . 2_655 ?
O2 Na1 Mo2 120.9(2) . 3_554 ?
O2 Na1 Mo2 90.6(2) 2_655 3_554 ?
O8 Na1 Mo2 126.0(4) 4 3_554 ?
O8 Na1 Mo2 26.58(18) 3_554 3_554 ?
O4 Na1 Mo2 85.92(13) . 3_554 ?
O4 Na1 Mo2 151.0(2) 2_655 3_554 ?
O7 Na1 Mo2 27.26(15) 3_554 3_554 ?
O7 Na1 Mo2 98.4(4) 4 3_554 ?
Te2 Na1 Mo2 109.54(7) . 3_554 ?
Te2 Na1 Mo2 119.09(9) 2_655 3_554 ?
O2 Na1 Mo2 90.6(2) . 4 ?
O2 Na1 Mo2 120.9(2) 2_655 4 ?
O8 Na1 Mo2 26.58(18) 4 4 ?
O8 Na1 Mo2 126.0(4) 3_554 4 ?
O4 Na1 Mo2 151.0(2) . 4 ?
O4 Na1 Mo2 85.92(13) 2_655 4 ?
O7 Na1 Mo2 98.4(4) 3_554 4 ?
O7 Na1 Mo2 27.25(15) 4 4 ?
Te2 Na1 Mo2 119.09(9) . 4 ?
Te2 Na1 Mo2 109.54(7) 2_655 4 ?
Mo2 Na1 Mo2 115.2(4) 3_554 4 ?
O6 Na2 O6 175.1(5) 2_754 1_455 ?
O6 Na2 O8 84.9(3) 2_754 3_554 ?
O6 Na2 O8 91.5(3) 1_455 3_554 ?
O6 Na2 O8 91.5(3) 2_754 4_554 ?
O6 Na2 O8 84.9(3) 1_455 4_554 ?
O8 Na2 O8 83.5(5) 3_554 4_554 ?
O6 Na2 O4 79.7(2) 2_754 2_654 ?
O6 Na2 O4 102.7(3) 1_455 2_654 ?
O8 Na2 O4 156.0(4) 3_554 2_654 ?
O8 Na2 O4 78.7(3) 4_554 2_654 ?
O6 Na2 O4 102.7(3) 2_754 . ?
O6 Na2 O4 79.7(2) 1_455 . ?
O8 Na2 O4 78.7(3) 3_554 . ?
O8 Na2 O4 156.0(4) 4_554 . ?
O4 Na2 O4 122.5(5) 2_654 . ?
O6 Na2 Te2 50.11(19) 2_754 2_654 ?
O6 Na2 Te2 133.1(3) 1_455 2_654 ?
O8 Na2 Te2 134.7(2) 3_554 2_654 ?
O8 Na2 Te2 91.8(2) 4_554 2_654 ?
O4 Na2 Te2 31.70(16) 2_654 2_654 ?
O4 Na2 Te2 112.2(3) . 2_654 ?
O6 Na2 Te2 133.1(3) 2_754 . ?
O6 Na2 Te2 50.11(19) 1_455 . ?
O8 Na2 Te2 91.8(2) 3_554 . ?
O8 Na2 Te2 134.7(2) 4_554 . ?
O4 Na2 Te2 112.2(3) 2_654 . ?
O4 Na2 Te2 31.70(16) . . ?
Te2 Na2 Te2 121.0(2) 2_654 . ?
O1 Te1 O1 97.7(4) 2 . ?
O1 Te1 O2 83.9(3) 2 . ?
O1 Te1 O2 87.1(3) . . ?
O1 Te1 O2 87.1(3) 2 2 ?
O1 Te1 O2 83.9(3) . 2 ?
O2 Te1 O2 166.3(4) . 2 ?
O4 Te2 O3 101.0(3) . . ?
O4 Te2 O2 91.3(3) . . ?
O3 Te2 O2 92.6(3) . . ?
O4 Te2 Na2 44.8(2) . . ?
O3 Te2 Na2 145.4(2) . . ?
O2 Te2 Na2 93.3(2) . . ?
O4 Te2 Na1 56.5(2) . . ?
O3 Te2 Na1 90.4(3) . . ?
O2 Te2 Na1 36.0(2) . . ?
Na2 Te2 Na1 75.04(14) . . ?
O6 Mo1 O6 104.8(5) 2_754 . ?
O6 Mo1 O5 100.3(3) 2_754 1_655 ?
O6 Mo1 O5 99.5(3) . 1_655 ?
O6 Mo1 O5 99.5(3) 2_754 2_654 ?
O6 Mo1 O5 100.3(3) . 2_654 ?
O5 Mo1 O5 147.2(4) 1_655 2_654 ?
O6 Mo1 O3 165.3(3) 2_754 4_654 ?
O6 Mo1 O3 89.0(3) . 4_654 ?
O5 Mo1 O3 81.7(3) 1_655 4_654 ?
O5 Mo1 O3 72.8(3) 2_654 4_654 ?
O6 Mo1 O3 89.0(3) 2_754 3_554 ?
O6 Mo1 O3 165.3(3) . 3_554 ?
O5 Mo1 O3 72.8(3) 1_655 3_554 ?
O5 Mo1 O3 81.7(3) 2_654 3_554 ?
O3 Mo1 O3 77.6(4) 4_654 3_554 ?
O7 Mo2 O8 99.9(4) . . ?
O7 Mo2 O1 101.3(3) . . ?
O8 Mo2 O1 94.9(3) . . ?
O7 Mo2 O5 96.0(3) . 3_545 ?
O8 Mo2 O5 95.7(4) . 3_545 ?
O1 Mo2 O5 157.9(3) . 3_545 ?
O7 Mo2 O3 164.9(3) . . ?
O8 Mo2 O3 91.5(4) . . ?
O1 Mo2 O3 87.4(3) . . ?
O5 Mo2 O3 72.9(3) 3_545 . ?
O7 Mo2 O4 88.8(4) . 2_655 ?
O8 Mo2 O4 171.2(4) . 2_655 ?
O1 Mo2 O4 84.6(3) . 2_655 ?
O5 Mo2 O4 82.0(3) 3_545 2_655 ?
O3 Mo2 O4 79.7(3) . 2_655 ?
O7 Mo2 Na1 52.7(3) . 3_445 ?
O8 Mo2 Na1 47.2(3) . 3_445 ?
O1 Mo2 Na1 104.3(3) . 3_445 ?
O5 Mo2 Na1 97.1(2) 3_545 3_445 ?
O3 Mo2 Na1 137.2(2) . 3_445 ?
O4 Mo2 Na1 141.4(2) 2_655 3_445 ?
Te1 O1 Mo2 148.7(4) . . ?
Te2 O2 Te1 120.1(3) . . ?
Te2 O2 Na1 114.5(4) . . ?
Te1 O2 Na1 121.7(4) . . ?
Te2 O3 Mo2 139.4(4) . . ?
Te2 O3 Mo1 122.1(3) . 3_445 ?
Mo2 O3 Mo1 97.1(3) . 3_445 ?
Te2 O4 Mo2 122.6(4) . 2_655 ?
Te2 O4 Na2 103.5(3) . . ?
Mo2 O4 Na2 107.5(3) 2_655 . ?
Te2 O4 Na1 91.6(3) . . ?
Mo2 O4 Na1 125.8(3) 2_655 . ?
Na2 O4 Na1 102.4(4) . . ?
Mo1 O5 Mo2 115.2(3) 1_455 3_454 ?
Mo1 O6 Na2 137.0(4) . 1_655 ?
Mo2 O7 Na1 100.0(4) . 3_445 ?
Mo2 O8 Na2 137.6(5) . 3_445 ?
Mo2 O8 Na1 106.2(4) . 3_445 ?
Na2 O8 Na1 107.9(4) 3_445 3_445 ?
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
Na1 O2 2.273(10) . ?
Na1 O2 2.273(10) 2_655 ?
Na1 O8 2.811(10) 4 ?
Na1 O8 2.811(10) 3_554 ?
Na1 O4 2.936(13) . ?
Na1 O4 2.936(13) 2_655 ?
Na1 O7 2.973(14) 3_554 ?
Na1 O7 2.973(14) 4 ?
Na1 Te2 3.519(11) . ?
Na1 Te2 3.519(11) 2_655 ?
Na1 Mo2 3.679(7) 3_554 ?
Na1 Mo2 3.679(7) 4 ?
Na2 O6 2.399(7) 2_754 ?
Na2 O6 2.399(7) 1_455 ?
Na2 O8 2.422(11) 3_554 ?
Na2 O8 2.422(11) 4_554 ?
Na2 O4 2.492(8) 2_654 ?
Na2 O4 2.492(8) . ?
Na2 Te2 3.439(4) 2_654 ?
Na2 Te2 3.439(4) . ?
Te1 O1 1.906(7) 2 ?
Te1 O1 1.906(7) . ?
Te1 O2 2.043(7) . ?
Te1 O2 2.043(7) 2 ?
Te2 O4 1.859(6) . ?
Te2 O3 1.884(7) . ?
Te2 O2 1.904(7) . ?
Mo1 O6 1.727(7) 2_754 ?
Mo1 O6 1.727(7) . ?
Mo1 O5 1.942(7) 1_655 ?
Mo1 O5 1.942(7) 2_654 ?
Mo1 O3 2.213(7) 4_654 ?
Mo1 O3 2.213(7) 3_554 ?
Mo2 O7 1.711(7) . ?
Mo2 O8 1.715(8) . ?
Mo2 O1 1.964(7) . ?
Mo2 O5 1.965(7) 3_545 ?
Mo2 O3 2.190(7) . ?
Mo2 O4 2.197(7) 2_655 ?
Mo2 Na1 3.679(7) 3_445 ?
O3 Mo1 2.213(7) 3_445 ?
O4 Mo2 2.197(7) 2_655 ?
O5 Mo1 1.942(7) 1_455 ?
O5 Mo2 1.965(7) 3_454 ?
O6 Na2 2.399(7) 1_655 ?
O7 Na1 2.973(14) 3_445 ?
O8 Na2 2.422(11) 3_445 ?
O8 Na1 2.811(10) 3_445 ?
|
1101225.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101225.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_1101225
loop_
_publ_author_name
'Botar, Bogdan'
'K\"ogerler, Paul'
'Hill, Craig L.'
_publ_section_title
;
[{(Mo)Mo5O21(H2O)3(SO4)}12(VO)30(H2O)20]36-: A molecular quantum spin
icosidodecahedron.
;
_journal_issue 25
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first 3138
_journal_page_last 3140
_journal_paper_doi 10.1039/b504491j
_journal_year 2005
_chemical_formula_sum 'H422 K26 Mo72 Na8 O542 S12 V31'
_chemical_formula_weight 19169.44
_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'
_cell_angle_alpha 90.00
_cell_angle_beta 90.134(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 47.177(3)
_cell_length_b 42.460(3)
_cell_length_c 26.4971(16)
_cell_measurement_temperature 173(2)
_cell_volume 53078(6)
_diffrn_ambient_temperature 173(2)
_exptl_crystal_density_diffrn 2.399
_cod_duplicate_entry 7100077
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1101225
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
Mo1 Mo 0.23114(2) 0.41051(4) 0.30851(8) 0.0157(5) Uani 0.937(8) 1 d P . .
Mo2 Mo 0.27619(2) 0.06950(2) 0.26948(4) 0.0152(2) Uani 1 1 d . . .
Mo3 Mo 0.31588(2) 0.46777(2) 0.15992(4) 0.0177(2) Uani 1 1 d . . .
Mo4 Mo 0.35608(2) 0.03201(2) -0.02643(4) 0.0153(2) Uani 1 1 d . . .
Mo5 Mo 0.44538(5) 0.33213(2) -0.14992(5) 0.0157(5) Uani 0.943(8) 1 d P . .
Mo6 Mo 0.21981(2) 0.34170(2) 0.36366(4) 0.0155(2) Uani 1 1 d . . .
Mo7 Mo 0.03104(2) 0.30206(2) 0.05996(4) 0.0173(2) Uani 1 1 d . . .
Mo8 Mo 0.11636(2) 0.43699(2) 0.13024(4) 0.0176(2) Uani 1 1 d . . .
Mo9 Mo 0.40009(2) 0.43757(2) -0.01627(4) 0.0171(2) Uani 1 1 d . . .
Mo10 Mo 0.47259(2) 0.28783(2) -0.03255(4) 0.0175(2) Uani 1 1 d . . .
Mo11 Mo 0.37471(2) 0.41257(2) 0.21158(4) 0.0191(2) Uani 1 1 d . . .
Mo12 Mo 0.35864(2) 0.03706(2) 0.09861(4) 0.0156(2) Uani 1 1 d . . .
Mo13 Mo 0.08663(7) 0.23116(3) 0.24009(7) 0.0176(7) Uani 0.910(11) 1 d P . .
Mo14 Mo 0.29603(2) 0.00351(2) 0.02065(4) 0.0157(2) Uani 1 1 d . . .
Mo15 Mo 0.20845(2) 0.08780(2) 0.28416(4) 0.0154(2) Uani 1 1 d . . .
Mo16 Mo 0.16666(2) 0.14303(2) 0.33163(4) 0.0194(2) Uani 1 1 d . . .
Mo17 Mo 0.25324(2) 0.27691(2) 0.40136(4) 0.0199(2) Uani 1 1 d . . .
Mo18 Mo 0.21439(2) 0.03627(2) 0.19122(4) 0.0163(2) Uani 1 1 d . . .
Mo19 Mo 0.06092(2) 0.31339(2) 0.19428(4) 0.0163(2) Uani 1 1 d . . .
Mo20 Mo 0.16243(4) 0.36096(4) 0.29694(12) 0.0156(7) Uani 0.791(10) 1 d P . .
Mo21 Mo 0.28930(2) 0.35535(2) 0.36008(4) 0.0165(2) Uani 1 1 d . . .
Mo22 Mo 0.41290(2) 0.07391(2) 0.00552(4) 0.0165(2) Uani 1 1 d . . .
Mo23 Mo 0.37692(3) 0.14016(3) 0.23630(6) 0.0301(5) Uani 0.949(5) 1 d P . .
Mo24 Mo 0.42671(2) 0.39419(2) 0.10224(4) 0.0175(2) Uani 1 1 d . . .
Mo25 Mo 0.24689(2) 0.13472(2) 0.35756(4) 0.0162(2) Uani 1 1 d . . .
Mo26 Mo 0.37344(2) 0.44563(2) 0.09822(4) 0.0163(2) Uani 1 1 d . . .
Mo27 Mo 0.17310(2) 0.28399(2) 0.37464(4) 0.0206(2) Uani 1 1 d . . .
Mo28 Mo 0.45648(2) 0.25513(2) -0.14261(4) 0.0155(2) Uani 1 1 d . . .
Mo29 Mo 0.39978(4) 0.21386(3) 0.23803(6) 0.0186(5) Uani 0.906(7) 1 d P . .
Mo30 Mo 0.19364(4) 0.46651(9) 0.11608(6) 0.0153(7) Uani 0.814(13) 1 d P . .
Mo31 Mo 0.34754(3) 0.20738(3) 0.32041(6) 0.0386(4) Uani 1 1 d . . .
Mo32 Mo 0.17504(7) 0.02904(11) -0.01449(8) 0.0165(9) Uani 0.717(15) 1 d P . .
Mo33 Mo 0.06963(3) 0.32302(3) -0.14298(6) 0.0316(6) Uani 0.939(6) 1 d P . .
Mo34 Mo 0.43456(3) 0.26610(3) 0.16971(6) 0.0284(6) Uani 0.922(6) 1 d P . .
Mo35 Mo 0.38256(4) 0.28487(3) 0.27823(6) 0.0363(7) Uani 0.930(6) 1 d P . .
Mo36 Mo 0.14983(6) 0.09065(9) 0.21416(16) 0.0168(10) Uani 0.590(12) 1 d P . .
Mo41 Mo 0.15814(13) 0.36593(16) 0.3190(4) 0.0142(19) Uiso 0.209(10) 1 d P . .
Mo42 Mo 0.16925(15) 0.0178(3) -0.0206(2) 0.0170(16) Uiso 0.283(15) 1 d P . .
Mo43 Mo 0.3623(4) 0.2017(4) 0.3452(9) 0.010(7) Uiso 0.061(8) 1 d P . .
Mo44 Mo 0.4109(4) 0.2099(3) 0.2592(8) 0.023(5) Uiso 0.094(7) 1 d P . .
Mo45 Mo 0.18884(19) 0.4791(4) 0.1203(3) 0.019(2) Uiso 0.186(13) 1 d P . .
Mo46 Mo 0.3967(4) 0.2798(4) 0.3031(8) 0.018(6) Uiso 0.070(6) 1 d P . .
Mo47 Mo 0.0744(6) 0.2301(3) 0.2503(6) 0.009(4) Uiso 0.090(11) 1 d P . .
Mo48 Mo 0.2310(3) 0.4015(6) 0.2872(11) 0.004(6) Uiso 0.063(8) 1 d P . .
Mo49 Mo 0.14559(8) 0.08122(14) 0.2299(2) 0.0162(11) Uiso 0.410(12) 1 d P . .
Mo50 Mo 0.4468(4) 0.2620(3) 0.1947(7) 0.017(5) Uiso 0.078(6) 1 d P . .
Mo51 Mo 0.4317(8) 0.3301(4) -0.1414(8) 0.011(7) Uiso 0.057(8) 1 d P . .
Mo52 Mo 0.0566(5) 0.3277(5) -0.1696(9) 0.020(7) Uiso 0.061(6) 1 d P . .
Mo53 Mo 0.3903(5) 0.1361(5) 0.2623(9) 0.008(7) Uiso 0.051(5) 1 d P . .
V1 V 0.42022(5) 0.34419(5) 0.21200(8) 0.0259(5) Uani 1 1 d . . .
V2 V 0.03142(5) 0.27033(5) -0.06641(8) 0.0254(5) Uani 1 1 d . . .
V3 V 0.32136(5) 0.12872(5) 0.32457(8) 0.0220(5) Uani 1 1 d . . .
V4 V 0.32739(5) 0.28180(5) 0.36825(9) 0.0254(5) Uani 1 1 d . . .
V5 V 0.40923(5) 0.09648(5) 0.13718(8) 0.0239(5) Uani 1 1 d . . .
V6 V 0.20879(5) 0.20738(5) 0.38604(9) 0.0253(5) Uani 1 1 d . . .
V7 V 0.06482(5) 0.37555(5) 0.09838(8) 0.0202(4) Uani 1 1 d . . .
V8 V 0.23984(4) 0.01454(5) -0.07056(8) 0.0208(4) Uani 1 1 d . . .
V9 V 0.15485(5) 0.04542(6) 0.10708(8) 0.0289(5) Uani 1 1 d . . .
V10 V 0.11483(5) 0.29953(5) 0.28969(8) 0.0251(5) Uani 1 1 d . . .
V11 V 0.28818(4) 0.02674(4) 0.15338(7) 0.0164(4) Uani 1 1 d . . .
V12 V 0.44575(5) 0.36804(5) -0.02410(8) 0.0209(4) Uani 1 1 d . . .
V13 V 0.30577(5) 0.41901(5) 0.27233(8) 0.0254(5) Uani 1 1 d . . .
V14 V 0.17244(4) 0.42599(5) 0.22222(8) 0.0194(4) Uani 1 1 d . . .
V15 V 0.10668(6) 0.15291(5) 0.24786(10) 0.0354(6) Uani 1 1 d . . .
K1 K 0.24377(6) 0.47617(6) 0.22186(11) 0.0274(6) Uani 1 1 d . . .
K2 K 0.31849(8) 0.10822(8) 0.16130(13) 0.0442(8) Uani 1 1 d . . .
K3 K 0.41217(11) 0.30899(9) 0.05848(15) 0.0601(11) Uani 1 1 d . . .
K4 K 0.23974(9) 0.15218(9) 0.50053(15) 0.0542(10) Uani 1 1 d . . .
K5 K 0.5000 0.31117(16) 0.2500 0.0679(17) Uani 1 2 d S . .
K6 K 0.32912(10) 0.33935(10) 0.23538(19) 0.0702(13) Uani 1 1 d . . .
K7 K 0.27208(9) 0.21386(9) 0.3048(2) 0.0748(15) Uani 1 1 d . . .
K8 K 0.09378(14) 0.33611(11) -0.01552(17) 0.0874(19) Uani 1 1 d . . .
K9 K 0.36592(19) 0.2296(2) 0.4811(3) 0.135(3) Uani 1 1 d . . .
K10 K 0.20987(17) -0.06138(19) 0.0004(3) 0.054(2) Uani 0.50 1 d P . .
K11 K 0.35375(18) 0.49282(16) 0.2752(3) 0.0492(18) Uani 0.50 1 d P . .
K12 K 0.12255(19) 0.21518(17) 0.3657(3) 0.133(3) Uani 1 1 d . . .
K13 K 0.0937(2) 0.3882(2) 0.2425(4) 0.145(3) Uani 1 1 d . . .
K14 K 0.03058(19) 0.2934(2) 0.3222(3) 0.133(3) Uani 1 1 d . . .
K15 K 0.0809(2) 0.0852(2) 0.1473(3) 0.066(3) Uani 0.50 1 d P . .
S1 S 0.40955(7) 0.24586(7) -0.04734(12) 0.0239(7) Uani 1 1 d . . .
S2 S 0.35674(7) 0.36829(7) 0.10670(12) 0.0249(7) Uani 1 1 d . . .
S3 S 0.25068(7) 0.14154(7) 0.22707(12) 0.0239(7) Uani 1 1 d . . .
S4 S 0.25832(7) 0.30207(7) 0.27699(12) 0.0272(7) Uani 1 1 d . . .
S5 S 0.34546(7) 0.10395(7) 0.02578(12) 0.0213(6) Uani 1 1 d . . .
S6 S 0.1412(2) 0.3082(3) -0.1422(4) 0.046(2) Uiso 0.40 1 d P . .
S7 S 0.3625(4) 0.2610(4) 0.1627(6) 0.058(4) Uiso 0.30 1 d P . .
S8 S 0.3350(3) 0.2008(4) 0.1935(6) 0.055(4) Uiso 0.30 1 d P . .
O1 O 0.34895(17) 0.04083(18) -0.0996(3) 0.0179(17) Uani 1 1 d . . .
O2 O 0.39586(17) 0.41679(18) 0.1438(3) 0.0175(17) Uani 1 1 d . . .
O3 O 0.25003(17) 0.37101(18) 0.3388(3) 0.0204(18) Uani 1 1 d . . .
O4 O 0.38673(16) 0.06074(17) -0.0529(3) 0.0163(17) Uani 1 1 d . . .
O5 O 0.13564(17) 0.43092(18) 0.1875(3) 0.0203(18) Uani 1 1 d . . .
O6 O 0.17003(17) 0.10745(17) 0.2793(3) 0.0173(17) Uani 1 1 d . . .
O7 O 0.06538(17) 0.34872(18) 0.1600(3) 0.0184(17) Uani 1 1 d . . .
O8 O 0.09529(18) 0.25875(18) 0.2880(3) 0.0207(18) Uani 1 1 d . . .
O9 O 0.18029(17) 0.32866(18) 0.3472(3) 0.0176(17) Uani 1 1 d . . .
O10 O 0.33232(17) 0.50076(19) 0.1810(3) 0.0219(18) Uani 1 1 d . . .
O11 O 0.13877(19) 0.06122(19) 0.1705(3) 0.0230(19) Uani 1 1 d . . .
O12 O 0.18759(17) 0.06739(17) 0.2273(3) 0.0158(16) Uani 1 1 d . . .
O13 O 0.43901(17) 0.28916(18) -0.1850(3) 0.0183(17) Uani 1 1 d . . .
O14 O 0.42326(17) 0.34993(18) -0.1965(3) 0.0196(18) Uani 1 1 d . . .
O15 O 0.33519(17) 0.46589(17) 0.0907(3) 0.0177(17) Uani 1 1 d . . .
O16 O 0.18762(17) 0.02919(18) 0.1453(3) 0.0196(18) Uani 1 1 d . . .
O17 O 0.35167(16) 0.43965(17) 0.1623(3) 0.0164(17) Uani 1 1 d . . .
O18 O 0.3900(3) 0.2677(3) 0.1273(6) 0.084(5) Uani 1 1 d . . .
O19 O 0.44323(17) 0.35778(17) -0.0967(3) 0.0167(17) Uani 1 1 d . . .
O20 O 0.3461(3) 0.1640(3) 0.1784(6) 0.082(5) Uani 1 1 d . . .
O21 O 0.13694(18) 0.29174(19) 0.2419(3) 0.0242(19) Uani 1 1 d . . .
O22 O 0.28462(17) 0.00964(18) 0.0842(3) 0.0187(17) Uani 1 1 d . . .
O23 O 0.40179(16) 0.42191(17) 0.0568(3) 0.0164(17) Uani 1 1 d . . .
O24 O 0.18754(17) 0.46164(17) 0.1821(3) 0.0177(17) Uani 1 1 d . . .
O25 O 0.39206(18) 0.47793(19) 0.1121(3) 0.0233(19) Uani 1 1 d . . .
O26 O 0.28354(18) 0.05916(19) 0.0141(3) 0.0213(18) Uani 1 1 d . . .
O27 O 0.3712(2) -0.00018(19) 0.1085(3) 0.026(2) Uani 1 1 d . . .
O28 O 0.38150(17) 0.44720(18) -0.0727(3) 0.0177(17) Uani 1 1 d . . .
O29 O 0.31645(17) 0.01820(18) -0.0441(3) 0.0191(17) Uani 1 1 d . . .
O30 O 0.42253(18) 0.46886(19) -0.0090(3) 0.0231(19) Uani 1 1 d . . .
O31 O 0.37995(17) 0.04651(17) 0.0320(3) 0.0156(16) Uani 1 1 d . . .
O32 O 0.28390(17) 0.48213(19) 0.1316(3) 0.0212(18) Uani 1 1 d . . .
O33 O 0.17598(18) 0.34267(18) 0.2449(3) 0.0204(18) Uani 1 1 d . . .
O34 O 0.26378(17) -0.00001(18) -0.0140(3) 0.0191(17) Uani 1 1 d . . .
O35 O 0.02841(18) 0.31750(19) 0.2211(3) 0.0234(19) Uani 1 1 d . . .
O36 O 0.15459(18) 0.39884(18) 0.2733(3) 0.0197(18) Uani 1 1 d . . .
O37 O 0.2044(2) 0.2002(2) 0.4465(3) 0.027(2) Uani 1 1 d . . .
O38 O 0.11793(18) 0.10962(18) 0.2343(3) 0.0207(18) Uani 1 1 d . . .
O39 O 0.15744(19) 0.11980(19) 0.3819(3) 0.0237(19) Uani 1 1 d . . .
O40 O 0.10555(18) 0.30069(19) 0.1528(3) 0.0240(19) Uani 1 1 d . . .
O41 O 0.23019(18) 0.31973(18) 0.2852(3) 0.0208(18) Uani 1 1 d . . .
O42 O 0.30473(17) 0.09039(18) 0.2990(3) 0.0212(18) Uani 1 1 d . . .
O43 O 0.21404(18) 0.35696(19) 0.4205(3) 0.0209(18) Uani 1 1 d . . .
O44 O 0.33485(17) 0.08168(18) -0.0149(3) 0.0204(18) Uani 1 1 d . . .
O45 O 0.43749(18) 0.3722(2) 0.0486(3) 0.0235(19) Uani 1 1 d . . .
O46 O 0.48901(17) 0.25642(18) -0.1676(3) 0.0195(18) Uani 1 1 d . . .
O47 O 0.47892(18) 0.3389(2) -0.1719(3) 0.0244(19) Uani 1 1 d . . .
O48 O 0.18222(18) 0.24339(18) 0.3812(3) 0.0194(17) Uani 1 1 d . . .
O49 O 0.20184(18) 0.06062(19) 0.3283(3) 0.0220(18) Uani 1 1 d . . .
O50 O 0.16741(18) 0.02050(19) 0.0489(3) 0.0220(18) Uani 1 1 d . . .
O51 O 0.4073(3) 0.2842(3) 0.3265(6) 0.062(4) Uani 1 1 d . . .
O52 O 0.45306(18) 0.20860(18) -0.1297(3) 0.0194(18) Uani 1 1 d . . .
O53 O 0.18311(18) 0.16963(19) 0.2574(3) 0.0244(19) Uani 1 1 d . . .
O54 O 0.32744(18) 0.03867(19) 0.1364(3) 0.0208(18) Uani 1 1 d . . .
O55 O 0.42473(19) 0.2712(2) -0.0198(3) 0.028(2) Uani 1 1 d . . .
O56 O 0.27244(19) 0.1172(2) 0.2213(3) 0.027(2) Uani 1 1 d . . .
O57 O 0.09670(19) 0.4697(2) 0.1426(3) 0.027(2) Uani 1 1 d . . .
O58 O 0.29093(17) 0.27181(18) 0.3982(3) 0.0204(18) Uani 1 1 d . . .
O59 O 0.24795(17) 0.09610(18) 0.3103(3) 0.0184(17) Uani 1 1 d . . .
O60 O 0.29825(18) 0.4186(2) 0.1227(3) 0.0249(19) Uani 1 1 d . . .
O61 O 0.08530(18) 0.3096(2) 0.3508(3) 0.0255(19) Uani 1 1 d . . .
O62 O 0.20364(18) 0.42992(18) 0.0982(3) 0.0207(18) Uani 1 1 d . . .
O63 O 0.22745(18) 0.43028(19) 0.3644(3) 0.0228(19) Uani 1 1 d . . .
O64 O 0.08456(17) 0.31714(18) 0.2464(3) 0.0189(17) Uani 1 1 d . . .
O65 O 0.30525(17) 0.38107(18) 0.3156(3) 0.0221(18) Uani 1 1 d . . .
O66 O -0.00194(19) 0.3105(2) 0.0807(3) 0.027(2) Uani 1 1 d . . .
O67 O 0.20619(17) 0.42921(17) 0.2673(3) 0.0180(17) Uani 1 1 d . . .
O68 O 0.1356(2) 0.0010(2) 0.1285(3) 0.029(2) Uani 1 1 d . . .
O69 O 0.4256(3) 0.2086(2) 0.2792(4) 0.043(3) Uani 1 1 d . . .
O70 O 0.16482(18) 0.11838(19) 0.1759(3) 0.0233(19) Uani 1 1 d . . .
O71 O 0.37201(17) -0.00297(18) -0.0323(3) 0.0199(18) Uani 1 1 d . . .
O72 O 0.24002(18) 0.11518(19) 0.4118(3) 0.0235(19) Uani 1 1 d . . .
O73 O 0.43624(16) 0.23508(17) -0.2002(3) 0.0159(16) Uani 1 1 d . . .
O74 O 0.2483(2) 0.2826(2) 0.4638(3) 0.028(2) Uani 1 1 d . . .
O75 O 0.34169(18) 0.08810(18) 0.0750(3) 0.0218(18) Uani 1 1 d . . .
O76 O 0.17015(19) 0.0798(2) 0.0896(3) 0.028(2) Uani 1 1 d . . .
O77 O 0.20778(16) 0.12707(18) 0.3264(3) 0.0188(17) Uani 1 1 d . . .
O78 O 0.25836(17) 0.32384(18) 0.3822(3) 0.0197(18) Uani 1 1 d . . .
O79 O 0.29121(17) 0.05614(19) 0.2111(3) 0.0205(18) Uani 1 1 d . . .
O80 O 0.23942(19) 0.23824(19) 0.3912(3) 0.027(2) Uani 1 1 d . . .
O81 O 0.04837(18) 0.33883(18) 0.0622(3) 0.0209(18) Uani 1 1 d . . .
O82 O 0.28486(17) 0.13561(18) 0.3571(3) 0.0204(18) Uani 1 1 d . . .
O83 O 0.38606(19) 0.3608(2) 0.0927(3) 0.027(2) Uani 1 1 d . . .
O84 O 0.04411(19) 0.2308(2) 0.2837(3) 0.027(2) Uani 1 1 d . . .
O85 O 0.39746(18) 0.38036(19) 0.2284(3) 0.0223(18) Uani 1 1 d . . .
O86 O 0.20520(17) 0.00612(18) -0.0311(3) 0.0203(18) Uani 1 1 d . . .
O87 O 0.4010(3) 0.1267(3) 0.2800(6) 0.063(4) Uani 1 1 d . . .
O88 O 0.23712(18) 0.17426(19) 0.3721(3) 0.0233(19) Uani 1 1 d . . .
O89 O 0.10560(18) 0.34975(19) 0.0841(3) 0.0243(19) Uani 1 1 d . . .
O90 O 0.22621(17) 0.48736(18) 0.1140(3) 0.0187(17) Uani 1 1 d . . .
O91 O 0.09059(17) 0.40612(18) 0.1306(3) 0.0188(17) Uani 1 1 d . . .
O92 O 0.27720(18) 0.07343(19) 0.1138(3) 0.0223(18) Uani 1 1 d . . .
O93 O 0.34374(18) 0.40656(19) 0.2481(3) 0.0216(18) Uani 1 1 d . . .
O94 O 0.17448(18) 0.51715(19) 0.1332(3) 0.0228(19) Uani 1 1 d . . .
O95 O 0.03552(19) 0.3942(2) 0.1100(3) 0.027(2) Uani 1 1 d . . .
O96 O 0.17898(17) 0.17766(18) 0.3613(3) 0.0202(18) Uani 1 1 d . . .
O97 O 0.24175(18) 0.0524(2) -0.0585(3) 0.0243(19) Uani 1 1 d . . .
O98 O 0.47027(17) 0.24624(18) -0.0720(3) 0.0172(17) Uani 1 1 d . . .
O99 O 0.41196(18) 0.25290(18) -0.1033(3) 0.0200(18) Uani 1 1 d . . .
O100 O 0.24666(17) 0.02721(18) 0.1601(3) 0.0189(17) Uani 1 1 d . . .
O101 O 0.21535(16) 0.29566(18) 0.3783(3) 0.0180(17) Uani 1 1 d . . .
O102 O 0.43333(18) 0.36816(19) 0.1541(3) 0.0227(19) Uani 1 1 d . . .
O103 O 0.34868(17) 0.39897(18) 0.0808(3) 0.0213(18) Uani 1 1 d . . .
O104 O 0.12842(17) 0.34223(18) 0.3035(3) 0.0197(18) Uani 1 1 d . . .
O105 O 0.30339(17) 0.44903(17) 0.2155(3) 0.0176(17) Uani 1 1 d . . .
O106 O 0.15522(18) 0.46313(19) 0.2717(3) 0.0223(18) Uani 1 1 d . . .
O107 O 0.50666(18) 0.2978(2) -0.0467(3) 0.027(2) Uani 1 1 d . . .
O108 O 0.18472(18) 0.39785(19) 0.1862(3) 0.0237(19) Uani 1 1 d . . .
O109 O 0.45317(19) 0.4207(2) 0.1085(4) 0.031(2) Uani 1 1 d . . .
O110 O 0.09142(19) 0.19367(18) 0.2689(3) 0.0239(19) Uani 1 1 d . . .
O111 O 0.42028(18) 0.08609(19) 0.0684(3) 0.0239(19) Uani 1 1 d . . .
O112 O 0.39050(19) 0.4435(2) 0.2413(3) 0.027(2) Uani 1 1 d . . .
O113 O 0.38408(19) 0.06047(19) 0.1322(3) 0.0238(19) Uani 1 1 d . . .
O114 O 0.13318(18) 0.15348(19) 0.3053(3) 0.0213(18) Uani 1 1 d . . .
O115 O 0.36589(18) 0.39449(19) -0.0167(3) 0.0226(18) Uani 1 1 d . . .
O116 O 0.18869(18) 0.27479(19) 0.2883(3) 0.0247(19) Uani 1 1 d . . .
O117 O 0.33417(17) 0.02550(18) 0.0369(3) 0.0199(18) Uani 1 1 d . . .
O118 O 0.26443(17) 0.42357(18) 0.2846(3) 0.0195(18) Uani 1 1 d . . .
O119 O 0.42337(17) 0.40673(18) -0.0347(3) 0.0198(18) Uani 1 1 d . . .
O120 O 0.21082(19) 0.00547(18) 0.2316(3) 0.0228(19) Uani 1 1 d . . .
O121 O 0.0035(2) 0.2759(2) -0.0981(4) 0.045(3) Uani 1 1 d . . .
O122 O 0.23699(19) -0.03719(19) -0.0872(3) 0.0244(19) Uani 1 1 d . . .
O123 O 0.45638(17) 0.29530(18) -0.1030(3) 0.0171(17) Uani 1 1 d . . .
O124 O 0.2531(2) 0.15777(19) 0.2764(3) 0.026(2) Uani 1 1 d . . .
O125 O 0.37560(19) 0.11093(19) 0.0159(3) 0.026(2) Uani 1 1 d . . .
O126 O 0.13130(19) 0.1691(2) 0.2052(4) 0.031(2) Uani 1 1 d . . .
O127 O 0.11562(18) 0.23360(19) 0.2016(3) 0.0239(19) Uani 1 1 d . . .
O128 O 0.23597(17) 0.06476(17) 0.2408(3) 0.0162(17) Uani 1 1 d . . .
O129 O 0.27437(18) 0.03575(18) 0.3036(3) 0.0235(19) Uani 1 1 d . . .
O130 O 0.07719(19) 0.1331(2) 0.2979(3) 0.027(2) Uani 1 1 d . . .
O131 O 0.35299(19) 0.37287(19) 0.1619(3) 0.027(2) Uani 1 1 d . . .
O132 O 0.13912(18) 0.28350(18) 0.3440(3) 0.0209(18) Uani 1 1 d . . .
O133 O 0.14732(18) 0.39347(19) 0.1045(3) 0.0228(19) Uani 1 1 d . . .
O134 O 0.31560(17) 0.32549(18) 0.3700(3) 0.0215(18) Uani 1 1 d . . .
O135 O 0.22140(18) 0.12586(19) 0.2252(3) 0.0212(18) Uani 1 1 d . . .
O136 O 0.39984(17) 0.31512(19) -0.1185(3) 0.0222(18) Uani 1 1 d . . .
O137 O 0.47733(19) 0.26615(19) 0.0249(3) 0.0238(19) Uani 1 1 d . . .
O138 O 0.42625(18) 0.10520(19) -0.0329(3) 0.0238(19) Uani 1 1 d . . .
O139 O 0.30905(19) -0.03416(19) 0.0223(3) 0.0249(19) Uani 1 1 d . . .
O140 O 0.21375(19) 0.2168(2) 0.3035(3) 0.027(2) Uani 1 1 d . . .
O141 O 0.29079(19) 0.3765(2) 0.4139(3) 0.030(2) Uani 1 1 d . . .
O142 O 0.1515(2) -0.0182(2) -0.0284(4) 0.030(2) Uani 1 1 d . . .
O143 O 0.20176(17) 0.37575(18) 0.3222(3) 0.0183(17) Uani 1 1 d . . .
O144 O 0.23448(18) 0.37557(18) 0.2349(3) 0.0217(18) Uani 1 1 d . . .
O145 O 0.1139(3) 0.3105(4) -0.1061(5) 0.088(5) Uani 1 1 d . . .
O146 O 0.13547(19) 0.05303(19) 0.2729(3) 0.0251(19) Uani 1 1 d . . .
O147 O 0.47710(18) 0.3840(2) -0.0245(3) 0.027(2) Uani 1 1 d . . .
O148 O 0.29349(18) -0.00487(19) 0.1847(3) 0.0238(19) Uani 1 1 d . . .
O149 O 0.2914(2) 0.3858(2) 0.2132(3) 0.029(2) Uani 1 1 d . . .
O150 O 0.36644(18) 0.45472(18) 0.0249(3) 0.0196(18) Uani 1 1 d . . .
O151 O 0.4282(3) 0.3072(2) 0.1726(5) 0.059(4) Uani 1 1 d . . .
O152 O 0.3521(3) 0.2811(3) 0.2119(6) 0.083(5) Uani 1 1 d . . .
O153 O 0.3251(3) 0.1739(2) 0.3253(5) 0.058(4) Uani 1 1 d . . .
O154 O 0.42242(19) 0.2146(2) -0.0378(3) 0.027(2) Uani 1 1 d . . .
O155 O 0.4655(3) 0.2635(3) 0.2044(5) 0.060(3) Uani 1 1 d . . .
O156 O 0.4066(2) 0.2598(2) 0.2278(4) 0.041(3) Uani 1 1 d . . .
O157 O 0.18892(19) 0.06632(19) -0.0105(3) 0.0248(19) Uani 1 1 d . . .
O158 O 0.0966(2) 0.3278(2) -0.2027(4) 0.036(2) Uani 1 1 d . . .
O159 O 0.3735(2) 0.2379(2) 0.2826(4) 0.041(3) Uani 1 1 d . . .
O160 O 0.16459(19) 0.2943(2) 0.4352(3) 0.026(2) Uani 1 1 d . . .
O161 O 0.4233(2) 0.2197(2) 0.1764(4) 0.037(2) Uani 1 1 d . . .
O162 O 0.43686(18) 0.0446(2) -0.0034(3) 0.0259(19) Uani 1 1 d . . .
O163 O 0.40260(18) 0.34521(19) -0.0248(3) 0.0251(19) Uani 1 1 d . . .
O164 O 0.3169(2) 0.4442(2) 0.3162(3) 0.029(2) Uani 1 1 d . . .
O165 O 0.02541(19) 0.29555(18) -0.0062(3) 0.0229(19) Uani 1 1 d . . .
O166 O 0.3449(2) 0.1288(2) 0.2637(5) 0.052(3) Uani 1 1 d . . .
O167 O 0.2589(2) 0.2749(2) 0.3131(3) 0.032(2) Uani 1 1 d . . .
O168 O 0.45775(18) 0.32405(19) -0.0121(3) 0.0231(19) Uani 1 1 d . . .
O169 O 0.22083(19) 0.08481(19) 0.1435(3) 0.026(2) Uani 1 1 d . . .
O170 O 0.15012(19) 0.3840(2) 0.3739(3) 0.027(2) Uani 1 1 d . . .
O171 O 0.4345(2) 0.0837(3) 0.1715(4) 0.047(3) Uani 1 1 d . . .
O172 O 0.3689(4) 0.2020(3) 0.3715(7) 0.078(5) Uani 1 1 d . . .
O173 O 0.28175(19) 0.3244(2) 0.2853(3) 0.029(2) Uani 1 1 d . . .
O174 O 0.3724(2) 0.1837(2) 0.2694(4) 0.039(3) Uani 1 1 d . . .
O175 O 0.4463(3) 0.2585(2) 0.1078(4) 0.049(3) Uani 1 1 d . . .
O176 O 0.3824(2) 0.1142(2) 0.1843(4) 0.048(3) Uani 1 1 d . . .
O177 O 0.3917(3) 0.3203(2) 0.2471(5) 0.060(4) Uani 1 1 d . . .
O178 O 0.3645(3) 0.2210(3) 0.1828(5) 0.055(3) Uani 1 1 d . . .
O179 O 0.0568(3) 0.3035(2) -0.0886(4) 0.049(3) Uani 1 1 d . . .
O180 O 0.0797(3) 0.3609(2) -0.1212(5) 0.060(4) Uani 1 1 d . . .
O181 O 0.0387(3) 0.3306(3) -0.1746(5) 0.062(4) Uani 1 1 d . . .
O182 O 0.3513(2) 0.2937(2) 0.3116(5) 0.049(3) Uani 1 1 d . . .
O183 O 0.3421(2) 0.1177(3) 0.3684(4) 0.050(3) Uani 1 1 d . . .
O184 O 0.3490(2) 0.2794(3) 0.4147(5) 0.054(3) Uani 1 1 d . . .
O185 O 0.4462(2) 0.3458(3) 0.2499(4) 0.047(3) Uani 1 1 d . . .
O186 O 0.3266(3) 0.2393(2) 0.3405(5) 0.058(4) Uani 1 1 d . . .
O187 O 0.3209(3) 0.2143(5) 0.2462(6) 0.096(6) Uani 1 1 d . . .
O188 O 0.3800(2) 0.2454(2) -0.0346(4) 0.037(2) Uani 1 1 d . . .
O189 O 0.3378(2) 0.3442(2) 0.0892(4) 0.038(2) Uani 1 1 d . . .
O190 O 0.2526(2) 0.1642(2) 0.1869(4) 0.036(2) Uani 1 1 d . . .
O191 O 0.2588(2) 0.2910(2) 0.2257(4) 0.041(3) Uani 1 1 d . . .
O192 O 0.3287(2) 0.1325(2) 0.0236(4) 0.035(2) Uani 1 1 d . . .
O193 O 0.1644(6) 0.2990(7) -0.1082(11) 0.050(7) Uiso 0.40 1 d P . .
O194 O 0.3400(10) 0.2642(12) 0.1281(18) 0.070(13) Uiso 0.30 1 d P . .
O195 O 0.3160(10) 0.2085(11) 0.1560(17) 0.067(12) Uiso 0.30 1 d P . .
O201 O 0.1459(3) -0.0506(3) -0.1179(5) 0.063(3) Uiso 1 1 d . . .
O202 O 0.2281(3) -0.0303(4) 0.0908(6) 0.082(4) Uiso 1 1 d . . .
O203 O 0.16862(18) 0.4482(2) 0.3724(3) 0.026(2) Uiso 1 1 d . . .
O204 O 0.2622(3) -0.0881(4) 0.0166(6) 0.080(4) Uiso 1 1 d . . .
O205 O 0.1877(3) 0.1237(4) 0.4788(6) 0.082(4) Uiso 1 1 d . . .
O206 O 0.1329(3) 0.5588(4) 0.1017(6) 0.086(5) Uiso 1 1 d . . .
O207 O 0.2950(4) 0.1621(5) 0.4605(7) 0.106(6) Uiso 1 1 d . . .
O208 O 0.3565(4) -0.0722(4) 0.0020(7) 0.098(5) Uiso 1 1 d . . .
O209 O -0.0314(4) 0.2278(5) -0.1784(7) 0.101(5) Uiso 1 1 d . . .
O210 O 0.3050(4) 0.2387(5) 0.4857(7) 0.107(6) Uiso 1 1 d . . .
O211 O 0.3647(4) 0.3604(4) 0.3248(7) 0.102(6) Uiso 1 1 d . . .
O212 O 0.1599(4) 0.3655(4) 0.4772(7) 0.102(5) Uiso 1 1 d . . .
O213 O 0.0823(5) 0.5336(5) 0.1182(8) 0.125(7) Uiso 1 1 d . . .
O214 O 0.3567(5) 0.2889(6) 0.5340(9) 0.146(8) Uiso 1 1 d . . .
O215 O 0.0734(5) 0.1836(6) 0.3659(9) 0.055(6) Uiso 0.50 1 d P . .
O216 O 0.0982(6) 0.4498(7) 0.2866(10) 0.159(9) Uiso 1 1 d . . .
O217 O 0.0312(7) 0.3633(8) -0.0464(12) 0.190(12) Uiso 1 1 d . . .
O218 O 0.4931(5) 0.3501(6) 0.1649(10) 0.151(9) Uiso 1 1 d . . .
O219 O 0.2921(6) 0.1568(7) 0.1054(11) 0.170(10) Uiso 1 1 d . . .
O220 O -0.0193(7) 0.2026(8) -0.0832(13) 0.203(13) Uiso 1 1 d . . .
O221 O 0.1061(6) 0.5433(7) 0.2526(11) 0.174(11) Uiso 1 1 d . . .
O222 O 0.0031(7) 0.4008(8) 0.0215(12) 0.199(13) Uiso 1 1 d . . .
O223 O 0.4705(5) 0.3226(6) 0.0970(10) 0.061(7) Uiso 0.50 1 d P . .
O224 O 0.0966(7) 0.2651(8) 0.4299(12) 0.195(12) Uiso 1 1 d . . .
O225 O 0.1810(3) -0.0249(3) 0.1112(5) 0.060(3) Uiso 1 1 d . . .
O226 O -0.0122(2) 0.2846(3) -0.2002(4) 0.047(3) Uiso 1 1 d . . .
O227 O 0.2901(2) -0.0641(2) -0.0860(4) 0.038(2) Uiso 1 1 d . . .
O228 O 0.5000 0.3043(3) -0.2500 0.025(3) Uiso 1 2 d S . .
O229 O 0.0403(8) 0.4093(9) 0.2233(14) 0.225(15) Uiso 1 1 d . . .
O230 O 0.4038(6) 0.1398(7) 0.3933(11) 0.179(11) Uiso 1 1 d . . .
O231 O 0.2904(7) 0.2026(9) 0.4063(13) 0.095(10) Uiso 0.50 1 d P . .
O232 O 0.1651(7) -0.0567(8) 0.0709(12) 0.196(12) Uiso 1 1 d . . .
O233 O 0.4113(8) 0.2497(8) 0.4201(13) 0.216(14) Uiso 1 1 d . . .
O234 O 0.4409(7) 0.0153(8) 0.1183(13) 0.207(13) Uiso 1 1 d . . .
O235 O 0.0478(8) 0.0880(10) 0.2359(14) 0.238(16) Uiso 1 1 d . . .
O236 O 0.0826(8) -0.0189(9) 0.0943(14) 0.228(15) Uiso 1 1 d . . .
O237 O 0.1164(7) 0.3344(8) 0.5138(12) 0.188(12) Uiso 1 1 d . . .
O238 O 0.1470(6) 0.1502(8) 0.5481(12) 0.185(11) Uiso 1 1 d . . .
O239 O -0.0338(9) 0.3518(10) -0.2121(16) 0.121(13) Uiso 0.50 1 d P . .
O240 O 0.0277(7) 0.4633(8) 0.1049(13) 0.209(13) Uiso 1 1 d . . .
O241 O 0.4415(8) 0.4754(9) 0.1889(14) 0.106(11) Uiso 0.50 1 d P . .
O242 O 0.0145(9) 0.3647(10) 0.3317(16) 0.118(13) Uiso 0.50 1 d P . .
O243 O -0.0065(10) 0.4603(11) -0.0157(18) 0.138(16) Uiso 0.50 1 d P . .
O244 O 0.0620(10) 0.5230(12) 0.0363(18) 0.144(16) Uiso 0.50 1 d P . .
O245 O 0.4257(9) 0.3566(11) 0.3560(16) 0.126(14) Uiso 0.50 1 d P . .
O246 O 0.0043(10) 0.3886(12) -0.1272(18) 0.136(15) Uiso 0.50 1 d P . .
O247 O 0.0422(9) 0.1780(10) 0.3569(15) 0.113(12) Uiso 0.50 1 d P . .
O248 O 0.0000 0.3660(11) 0.2500 0.194(17) Uiso 1 2 d S . .
O249 O 0.1596(2) 0.5237(2) 0.2366(4) 0.040(2) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0226(6) 0.0062(7) 0.0183(11) -0.0005(7) -0.0006(5) 0.0014(4)
Mo2 0.0230(5) 0.0056(4) 0.0171(5) -0.0003(4) 0.0003(4) -0.0004(4)
Mo3 0.0249(6) 0.0097(5) 0.0185(5) -0.0007(4) 0.0002(4) 0.0038(4)
Mo4 0.0222(5) 0.0063(5) 0.0176(5) -0.0015(4) -0.0001(4) 0.0003(4)
Mo5 0.0198(13) 0.0074(6) 0.0200(6) -0.0002(4) 0.0015(6) 0.0000(5)
Mo6 0.0222(5) 0.0072(5) 0.0172(5) -0.0005(4) 0.0008(4) 0.0012(4)
Mo7 0.0234(5) 0.0078(5) 0.0208(5) -0.0001(4) -0.0003(4) 0.0008(4)
Mo8 0.0230(5) 0.0114(5) 0.0185(5) -0.0009(4) -0.0002(4) -0.0004(4)
Mo9 0.0229(5) 0.0091(5) 0.0194(5) 0.0004(4) 0.0007(4) 0.0011(4)
Mo10 0.0226(5) 0.0086(5) 0.0214(5) -0.0004(4) 0.0000(4) 0.0001(4)
Mo11 0.0256(6) 0.0114(5) 0.0203(5) 0.0004(4) 0.0013(4) 0.0043(4)
Mo12 0.0227(5) 0.0071(5) 0.0170(5) 0.0001(4) -0.0007(4) -0.0006(4)
Mo13 0.0228(15) 0.0073(6) 0.0227(7) 0.0000(4) -0.0010(8) 0.0007(5)
Mo14 0.0229(5) 0.0065(5) 0.0176(5) -0.0012(4) -0.0008(4) -0.0005(4)
Mo15 0.0226(5) 0.0069(5) 0.0166(5) 0.0000(4) 0.0007(4) 0.0001(4)
Mo16 0.0239(6) 0.0106(5) 0.0239(5) -0.0032(4) -0.0004(4) 0.0013(4)
Mo17 0.0239(6) 0.0095(5) 0.0265(6) 0.0042(4) 0.0012(4) 0.0010(4)
Mo18 0.0226(5) 0.0073(5) 0.0189(5) 0.0000(4) -0.0005(4) -0.0006(4)
Mo19 0.0215(5) 0.0080(5) 0.0193(5) 0.0001(4) 0.0012(4) 0.0007(4)
Mo20 0.0221(8) 0.0067(7) 0.0181(15) 0.0011(7) -0.0002(7) -0.0007(5)
Mo21 0.0223(5) 0.0072(5) 0.0200(5) 0.0003(4) -0.0004(4) 0.0014(4)
Mo22 0.0223(5) 0.0076(5) 0.0195(5) -0.0001(4) -0.0003(4) -0.0005(4)
Mo23 0.0442(10) 0.0089(6) 0.0375(9) -0.0058(5) 0.0189(8) -0.0069(5)
Mo24 0.0222(5) 0.0095(5) 0.0210(5) -0.0001(4) 0.0002(4) 0.0020(4)
Mo25 0.0236(5) 0.0069(5) 0.0181(5) -0.0010(4) 0.0000(4) 0.0004(4)
Mo26 0.0224(5) 0.0071(5) 0.0193(5) -0.0013(4) 0.0001(4) 0.0021(4)
Mo27 0.0240(6) 0.0104(5) 0.0273(6) 0.0049(4) 0.0001(4) -0.0001(4)
Mo28 0.0187(5) 0.0079(5) 0.0199(5) 0.0000(4) 0.0017(4) 0.0003(4)
Mo29 0.0259(9) 0.0065(6) 0.0235(9) -0.0023(5) 0.0042(7) -0.0023(5)
Mo30 0.0222(8) 0.0070(14) 0.0167(7) -0.0016(6) -0.0002(5) 0.0027(8)
Mo31 0.0511(9) 0.0135(6) 0.0514(8) -0.0067(6) 0.0246(8) -0.0066(6)
Mo32 0.0217(11) 0.0097(16) 0.0180(9) -0.0012(8) -0.0018(7) -0.0005(10)
Mo33 0.0467(10) 0.0097(6) 0.0385(10) -0.0062(5) 0.0214(8) -0.0060(5)
Mo34 0.0411(10) 0.0076(6) 0.0367(10) -0.0048(5) 0.0185(8) -0.0045(5)
Mo35 0.0510(11) 0.0084(6) 0.0497(11) -0.0053(6) 0.0297(9) -0.0054(6)
Mo36 0.0241(11) 0.0096(14) 0.0168(16) -0.0011(12) 0.0007(9) 0.0008(9)
V1 0.0360(13) 0.0119(10) 0.0300(12) 0.0052(9) 0.0089(10) 0.0073(9)
V2 0.0416(14) 0.0101(10) 0.0245(11) -0.0014(8) 0.0039(10) -0.0024(9)
V3 0.0257(11) 0.0096(10) 0.0309(12) -0.0054(8) 0.0048(9) -0.0034(8)
V4 0.0255(12) 0.0100(10) 0.0405(13) 0.0030(9) 0.0082(10) 0.0023(8)
V5 0.0338(12) 0.0150(10) 0.0230(11) -0.0057(8) 0.0042(9) -0.0082(9)
V6 0.0266(12) 0.0097(10) 0.0398(13) -0.0017(9) -0.0003(10) 0.0002(9)
V7 0.0279(11) 0.0097(9) 0.0229(11) 0.0013(8) 0.0001(9) -0.0019(8)
V8 0.0237(11) 0.0190(11) 0.0195(10) -0.0007(8) 0.0000(8) 0.0021(9)
V9 0.0300(12) 0.0331(13) 0.0234(11) -0.0055(10) -0.0045(9) 0.0103(10)
V10 0.0319(12) 0.0118(10) 0.0315(12) 0.0035(9) -0.0095(10) -0.0033(9)
V11 0.0241(11) 0.0076(9) 0.0176(10) -0.0001(8) 0.0008(8) -0.0009(8)
V12 0.0290(12) 0.0125(10) 0.0211(11) -0.0011(8) 0.0018(9) 0.0043(9)
V13 0.0259(12) 0.0211(11) 0.0291(12) 0.0097(9) 0.0057(9) 0.0064(9)
V14 0.0241(11) 0.0121(10) 0.0219(11) 0.0015(8) -0.0012(8) 0.0000(8)
V15 0.0476(15) 0.0184(12) 0.0400(14) -0.0126(10) -0.0212(12) 0.0174(11)
K1 0.0333(16) 0.0137(13) 0.0351(16) 0.0023(11) -0.0077(13) -0.0033(11)
K2 0.050(2) 0.0373(19) 0.046(2) -0.0127(15) 0.0153(16) -0.0119(16)
K3 0.103(3) 0.0312(19) 0.046(2) 0.0004(16) 0.014(2) 0.019(2)
K4 0.071(3) 0.046(2) 0.046(2) -0.0085(17) 0.0008(19) 0.0022(19)
K5 0.054(4) 0.063(4) 0.087(5) 0.000 -0.007(3) 0.000
K6 0.070(3) 0.050(2) 0.090(3) 0.022(2) 0.031(2) 0.012(2)
K7 0.055(3) 0.028(2) 0.141(5) -0.017(2) 0.020(3) -0.0036(18)
K8 0.163(5) 0.052(3) 0.048(2) -0.005(2) 0.017(3) -0.059(3)
K9 0.150(7) 0.138(7) 0.117(6) 0.042(5) 0.001(5) -0.002(5)
K10 0.054(5) 0.054(5) 0.055(5) 0.025(4) 0.009(4) 0.004(4)
K11 0.081(6) 0.028(3) 0.038(4) -0.007(3) -0.006(4) 0.007(3)
K12 0.148(7) 0.082(5) 0.168(7) 0.000(5) -0.028(6) 0.004(4)
K13 0.157(7) 0.107(6) 0.171(8) 0.016(5) -0.028(6) -0.025(5)
K14 0.142(7) 0.123(6) 0.132(6) 0.001(5) 0.007(5) -0.021(5)
K15 0.086(6) 0.069(6) 0.043(4) -0.016(4) -0.014(4) 0.043(5)
S1 0.0240(16) 0.0187(15) 0.0289(17) -0.0003(13) 0.0014(13) -0.0005(12)
S2 0.0311(17) 0.0124(15) 0.0312(17) -0.0015(12) -0.0010(14) -0.0004(13)
S3 0.0344(18) 0.0109(14) 0.0265(16) 0.0041(12) 0.0026(13) -0.0004(13)
S4 0.0378(19) 0.0176(16) 0.0261(17) 0.0002(13) 0.0012(14) 0.0002(14)
S5 0.0295(17) 0.0098(14) 0.0246(16) -0.0003(12) 0.0001(13) 0.0025(12)
O1 0.021(4) 0.015(4) 0.018(4) 0.001(3) 0.002(3) 0.000(3)
O2 0.025(4) 0.010(4) 0.018(4) 0.000(3) 0.004(3) 0.005(3)
O3 0.024(4) 0.008(4) 0.030(5) 0.000(3) 0.003(4) 0.000(3)
O4 0.021(4) 0.009(4) 0.018(4) -0.004(3) -0.001(3) -0.003(3)
O5 0.023(4) 0.014(4) 0.024(4) 0.000(3) 0.001(3) 0.002(3)
O6 0.022(4) 0.007(4) 0.023(4) -0.005(3) 0.001(3) 0.003(3)
O7 0.023(4) 0.010(4) 0.023(4) 0.003(3) 0.003(3) 0.001(3)
O8 0.028(5) 0.010(4) 0.024(4) 0.000(3) -0.003(4) -0.003(3)
O9 0.025(4) 0.013(4) 0.015(4) 0.001(3) -0.004(3) 0.005(3)
O10 0.024(5) 0.017(4) 0.025(5) 0.001(3) -0.002(4) 0.001(3)
O11 0.036(5) 0.012(4) 0.022(4) 0.000(3) -0.002(4) 0.000(4)
O12 0.024(4) 0.008(4) 0.016(4) -0.003(3) 0.001(3) 0.004(3)
O13 0.024(4) 0.010(4) 0.021(4) 0.001(3) 0.001(3) 0.002(3)
O14 0.028(5) 0.010(4) 0.021(4) 0.002(3) 0.001(4) 0.003(3)
O15 0.027(5) 0.009(4) 0.017(4) 0.000(3) 0.002(3) 0.007(3)
O16 0.026(5) 0.009(4) 0.024(4) -0.002(3) -0.005(4) -0.002(3)
O17 0.021(4) 0.010(4) 0.018(4) 0.001(3) 0.001(3) 0.006(3)
O18 0.082(10) 0.061(9) 0.108(12) 0.037(9) 0.017(9) -0.021(8)
O19 0.026(4) 0.004(4) 0.020(4) -0.003(3) 0.001(3) -0.002(3)
O20 0.096(11) 0.038(7) 0.111(12) 0.002(8) -0.031(9) -0.021(7)
O21 0.030(5) 0.014(4) 0.028(5) 0.001(4) 0.000(4) -0.002(4)
O22 0.027(5) 0.009(4) 0.020(4) 0.002(3) -0.002(3) -0.002(3)
O23 0.021(4) 0.008(4) 0.020(4) -0.002(3) 0.001(3) 0.001(3)
O24 0.026(5) 0.007(4) 0.019(4) -0.002(3) 0.001(3) -0.001(3)
O25 0.026(5) 0.015(4) 0.029(5) -0.001(4) -0.001(4) 0.002(4)
O26 0.028(5) 0.015(4) 0.022(4) -0.002(3) -0.001(4) 0.003(3)
O27 0.041(5) 0.008(4) 0.030(5) 0.003(3) -0.001(4) 0.005(4)
O28 0.024(4) 0.009(4) 0.019(4) -0.003(3) -0.001(3) 0.002(3)
O29 0.025(4) 0.013(4) 0.019(4) 0.000(3) -0.004(3) -0.001(3)
O30 0.024(5) 0.015(4) 0.031(5) 0.002(4) -0.002(4) -0.006(3)
O31 0.024(4) 0.010(4) 0.013(4) -0.002(3) -0.001(3) -0.002(3)
O32 0.025(5) 0.020(4) 0.019(4) -0.002(3) -0.003(3) 0.006(4)
O33 0.029(5) 0.013(4) 0.019(4) -0.005(3) -0.002(4) -0.004(3)
O34 0.026(5) 0.012(4) 0.019(4) 0.000(3) 0.001(3) -0.002(3)
O35 0.026(5) 0.014(4) 0.030(5) -0.002(4) 0.009(4) -0.001(4)
O36 0.028(5) 0.011(4) 0.020(4) 0.000(3) -0.001(3) 0.000(3)
O37 0.038(5) 0.018(4) 0.027(5) 0.003(4) -0.003(4) 0.003(4)
O38 0.029(5) 0.012(4) 0.021(4) -0.003(3) -0.001(4) -0.001(3)
O39 0.033(5) 0.012(4) 0.026(5) -0.002(3) 0.001(4) -0.001(4)
O40 0.029(5) 0.015(4) 0.028(5) 0.006(4) 0.000(4) -0.001(4)
O41 0.034(5) 0.007(4) 0.021(4) -0.002(3) 0.004(4) 0.000(3)
O42 0.024(4) 0.008(4) 0.032(5) -0.006(3) -0.001(4) -0.003(3)
O43 0.029(5) 0.016(4) 0.017(4) -0.004(3) 0.002(3) -0.002(4)
O44 0.025(5) 0.012(4) 0.025(4) 0.000(3) -0.003(4) 0.000(3)
O45 0.030(5) 0.020(4) 0.020(4) 0.005(4) 0.004(4) 0.008(4)
O46 0.020(4) 0.013(4) 0.025(4) 0.001(3) 0.006(3) 0.004(3)
O47 0.026(5) 0.020(4) 0.027(5) 0.000(4) 0.005(4) -0.003(4)
O48 0.029(5) 0.011(4) 0.018(4) 0.001(3) 0.002(3) 0.002(3)
O49 0.027(5) 0.016(4) 0.023(4) -0.001(3) 0.002(4) -0.006(4)
O50 0.028(5) 0.017(4) 0.021(4) -0.002(3) 0.000(4) 0.008(4)
O51 0.089(10) 0.021(6) 0.075(9) -0.023(6) 0.008(9) -0.002(6)
O52 0.029(5) 0.009(4) 0.020(4) 0.004(3) -0.002(3) -0.004(3)
O53 0.029(5) 0.014(4) 0.031(5) 0.000(4) 0.002(4) -0.004(4)
O54 0.025(5) 0.017(4) 0.020(4) -0.003(3) 0.001(3) 0.000(3)
O55 0.028(5) 0.031(5) 0.026(5) -0.008(4) 0.002(4) 0.000(4)
O56 0.029(5) 0.020(5) 0.032(5) 0.011(4) 0.008(4) -0.002(4)
O57 0.031(5) 0.016(4) 0.033(5) -0.007(4) -0.003(4) 0.004(4)
O58 0.023(4) 0.009(4) 0.030(5) 0.007(3) 0.003(4) 0.002(3)
O59 0.027(5) 0.008(4) 0.020(4) -0.001(3) -0.002(3) 0.001(3)
O60 0.026(5) 0.017(4) 0.032(5) -0.001(4) -0.002(4) 0.002(4)
O61 0.030(5) 0.017(4) 0.029(5) 0.000(4) 0.005(4) 0.003(4)
O62 0.029(5) 0.010(4) 0.023(4) -0.002(3) 0.003(4) 0.002(3)
O63 0.031(5) 0.015(4) 0.023(4) 0.001(3) -0.006(4) 0.006(4)
O64 0.024(4) 0.008(4) 0.025(4) 0.003(3) 0.002(3) -0.002(3)
O65 0.020(4) 0.011(4) 0.035(5) 0.005(4) -0.001(4) -0.003(3)
O66 0.030(5) 0.023(5) 0.029(5) 0.005(4) 0.004(4) 0.007(4)
O67 0.026(5) 0.006(4) 0.022(4) -0.002(3) -0.002(3) 0.003(3)
O68 0.040(6) 0.015(4) 0.033(5) 0.001(4) -0.001(4) -0.003(4)
O69 0.062(8) 0.025(6) 0.042(6) -0.007(5) 0.018(6) -0.009(5)
O70 0.030(5) 0.014(4) 0.026(5) 0.002(4) -0.002(4) -0.001(4)
O71 0.026(5) 0.007(4) 0.026(4) -0.001(3) -0.001(4) 0.002(3)
O72 0.031(5) 0.018(4) 0.021(4) 0.002(3) -0.001(4) 0.002(4)
O73 0.023(4) 0.006(4) 0.019(4) 0.002(3) 0.002(3) 0.000(3)
O74 0.039(5) 0.020(5) 0.026(5) 0.003(4) -0.003(4) 0.006(4)
O75 0.034(5) 0.009(4) 0.022(4) -0.005(3) 0.001(4) 0.005(4)
O76 0.030(5) 0.023(5) 0.030(5) 0.000(4) -0.005(4) 0.002(4)
O77 0.017(4) 0.010(4) 0.029(5) -0.001(3) -0.002(3) 0.004(3)
O78 0.019(4) 0.010(4) 0.029(5) 0.004(3) 0.000(3) 0.003(3)
O79 0.026(5) 0.014(4) 0.022(4) -0.002(3) 0.001(4) -0.001(3)
O80 0.032(5) 0.014(4) 0.036(5) 0.003(4) -0.005(4) 0.002(4)
O81 0.034(5) 0.010(4) 0.019(4) -0.001(3) -0.005(4) 0.000(3)
O82 0.024(4) 0.013(4) 0.024(4) -0.006(3) -0.002(3) -0.004(3)
O83 0.031(5) 0.014(4) 0.036(5) -0.001(4) 0.001(4) 0.001(4)
O84 0.030(5) 0.015(4) 0.035(5) -0.003(4) 0.012(4) -0.002(4)
O85 0.026(5) 0.014(4) 0.027(5) 0.001(3) 0.002(4) 0.009(3)
O86 0.027(5) 0.011(4) 0.023(4) -0.002(3) 0.001(4) 0.004(3)
O87 0.076(9) 0.030(7) 0.082(10) 0.001(7) -0.012(8) -0.005(7)
O88 0.025(5) 0.011(4) 0.034(5) -0.007(4) -0.006(4) 0.001(3)
O89 0.031(5) 0.013(4) 0.029(5) -0.002(4) 0.008(4) -0.005(4)
O90 0.030(5) 0.009(4) 0.017(4) -0.002(3) -0.004(3) -0.001(3)
O91 0.022(4) 0.014(4) 0.021(4) -0.001(3) 0.001(3) -0.001(3)
O92 0.031(5) 0.013(4) 0.023(4) 0.002(3) 0.004(4) 0.001(4)
O93 0.025(5) 0.015(4) 0.024(4) 0.008(3) 0.003(4) 0.007(3)
O94 0.027(5) 0.013(4) 0.029(5) -0.004(3) -0.001(4) 0.005(3)
O95 0.029(5) 0.020(5) 0.031(5) 0.002(4) -0.001(4) 0.004(4)
O96 0.024(4) 0.011(4) 0.026(4) -0.003(3) 0.003(4) 0.000(3)
O97 0.026(5) 0.019(4) 0.027(5) -0.005(4) -0.004(4) 0.004(4)
O98 0.023(4) 0.011(4) 0.017(4) 0.002(3) -0.002(3) 0.000(3)
O99 0.029(5) 0.009(4) 0.022(4) -0.002(3) 0.003(4) 0.002(3)
O100 0.024(4) 0.014(4) 0.019(4) 0.000(3) 0.002(3) 0.001(3)
O101 0.017(4) 0.011(4) 0.026(4) 0.005(3) 0.000(3) 0.003(3)
O102 0.030(5) 0.017(4) 0.021(4) 0.000(3) 0.004(4) 0.009(4)
O103 0.024(5) 0.012(4) 0.027(5) -0.005(3) 0.003(4) -0.005(3)
O104 0.026(5) 0.012(4) 0.022(4) -0.001(3) 0.004(3) -0.002(3)
O105 0.027(4) 0.006(4) 0.020(4) 0.002(3) 0.004(3) 0.004(3)
O106 0.027(5) 0.013(4) 0.027(5) -0.004(3) 0.004(4) 0.006(3)
O107 0.023(5) 0.025(5) 0.031(5) -0.002(4) 0.003(4) 0.000(4)
O108 0.029(5) 0.015(4) 0.028(5) -0.002(4) -0.001(4) 0.005(4)
O109 0.033(5) 0.016(4) 0.043(6) 0.001(4) -0.002(4) -0.003(4)
O110 0.034(5) 0.004(4) 0.034(5) 0.002(3) -0.002(4) 0.001(3)
O111 0.025(5) 0.018(4) 0.028(5) -0.001(4) 0.000(4) -0.007(4)
O112 0.035(5) 0.019(5) 0.027(5) -0.002(4) -0.002(4) 0.001(4)
O113 0.034(5) 0.013(4) 0.024(5) 0.001(3) -0.003(4) -0.006(4)
O114 0.027(5) 0.020(4) 0.017(4) 0.000(3) -0.002(3) 0.001(4)
O115 0.029(5) 0.015(4) 0.024(4) -0.002(3) 0.000(4) 0.001(4)
O116 0.029(5) 0.015(4) 0.030(5) -0.003(4) -0.003(4) 0.002(4)
O117 0.021(4) 0.015(4) 0.024(4) 0.002(3) -0.001(3) 0.000(3)
O118 0.025(5) 0.011(4) 0.023(4) 0.003(3) 0.003(3) 0.002(3)
O119 0.023(4) 0.014(4) 0.023(4) 0.003(3) 0.001(3) 0.001(3)
O120 0.035(5) 0.011(4) 0.023(4) 0.004(3) 0.000(4) -0.004(4)
O121 0.064(7) 0.024(5) 0.047(6) -0.006(5) -0.018(5) 0.003(5)
O122 0.032(5) 0.013(4) 0.028(5) -0.004(4) -0.004(4) 0.000(4)
O123 0.024(4) 0.010(4) 0.017(4) 0.001(3) 0.000(3) 0.005(3)
O124 0.042(5) 0.013(4) 0.023(5) 0.005(3) 0.004(4) -0.010(4)
O125 0.034(5) 0.011(4) 0.033(5) -0.003(4) -0.002(4) -0.001(4)
O126 0.032(5) 0.016(4) 0.046(6) 0.009(4) -0.007(4) 0.003(4)
O127 0.025(5) 0.015(4) 0.032(5) -0.005(4) 0.005(4) 0.002(4)
O128 0.024(4) 0.009(4) 0.016(4) -0.003(3) 0.000(3) -0.001(3)
O129 0.031(5) 0.009(4) 0.030(5) 0.004(3) -0.002(4) -0.004(3)
O130 0.031(5) 0.021(5) 0.029(5) 0.002(4) 0.003(4) -0.005(4)
O131 0.034(5) 0.011(4) 0.035(5) 0.003(4) -0.005(4) -0.001(4)
O132 0.031(5) 0.008(4) 0.023(4) 0.006(3) 0.002(4) 0.002(3)
O133 0.034(5) 0.013(4) 0.020(4) 0.000(3) 0.001(4) -0.003(4)
O134 0.024(4) 0.009(4) 0.032(5) 0.004(3) 0.000(4) 0.003(3)
O135 0.036(5) 0.013(4) 0.014(4) 0.005(3) 0.001(4) 0.003(4)
O136 0.023(4) 0.015(4) 0.029(5) -0.001(4) 0.001(4) 0.005(3)
O137 0.035(5) 0.012(4) 0.024(5) 0.001(3) -0.006(4) -0.003(4)
O138 0.032(5) 0.016(4) 0.023(4) 0.002(3) 0.001(4) -0.008(4)
O139 0.035(5) 0.010(4) 0.031(5) -0.003(3) 0.000(4) 0.004(4)
O140 0.036(5) 0.017(4) 0.028(5) 0.001(4) 0.005(4) 0.008(4)
O141 0.031(5) 0.029(5) 0.031(5) -0.005(4) -0.006(4) 0.006(4)
O142 0.040(6) 0.013(4) 0.037(5) 0.003(4) -0.002(4) -0.002(4)
O143 0.025(4) 0.009(4) 0.021(4) 0.000(3) -0.004(3) 0.005(3)
O144 0.030(5) 0.010(4) 0.025(5) -0.005(3) 0.001(4) 0.000(3)
O145 0.098(12) 0.101(12) 0.064(9) -0.035(9) 0.003(8) 0.031(10)
O146 0.030(5) 0.014(4) 0.031(5) 0.004(4) 0.006(4) 0.002(4)
O147 0.028(5) 0.018(4) 0.034(5) -0.002(4) 0.000(4) -0.003(4)
O148 0.030(5) 0.014(4) 0.027(5) 0.008(4) -0.005(4) 0.003(4)
O149 0.038(5) 0.012(4) 0.037(5) 0.004(4) 0.009(4) 0.001(4)
O150 0.029(5) 0.010(4) 0.020(4) -0.001(3) 0.002(3) 0.003(3)
O151 0.089(9) 0.010(5) 0.079(8) -0.006(5) 0.060(7) -0.004(5)
O152 0.097(12) 0.045(8) 0.107(12) -0.030(8) 0.002(9) 0.026(8)
O153 0.078(9) 0.015(5) 0.081(9) -0.017(5) 0.057(7) -0.015(5)
O154 0.032(5) 0.027(5) 0.023(5) 0.005(4) 0.004(4) 0.001(4)
O155 0.059(9) 0.037(7) 0.084(10) 0.002(6) 0.013(7) -0.023(6)
O156 0.061(7) 0.016(5) 0.047(6) -0.005(4) 0.040(5) -0.008(5)
O157 0.031(5) 0.016(4) 0.028(5) -0.003(4) -0.004(4) -0.001(4)
O158 0.046(6) 0.013(4) 0.048(6) -0.006(4) 0.030(5) -0.009(4)
O159 0.056(7) 0.010(4) 0.058(7) -0.006(4) 0.037(5) -0.006(4)
O160 0.036(5) 0.019(4) 0.024(5) -0.002(4) -0.001(4) 0.001(4)
O161 0.047(6) 0.016(5) 0.048(6) -0.004(4) 0.019(5) -0.008(4)
O162 0.026(5) 0.018(4) 0.034(5) -0.002(4) -0.002(4) 0.003(4)
O163 0.029(5) 0.015(4) 0.032(5) -0.002(4) 0.008(4) -0.001(4)
O164 0.039(5) 0.019(5) 0.028(5) 0.003(4) -0.007(4) -0.006(4)
O165 0.040(5) 0.011(4) 0.019(4) 0.000(3) -0.002(4) 0.002(4)
O166 0.064(7) 0.019(5) 0.074(8) -0.021(5) 0.048(6) -0.018(5)
O167 0.050(6) 0.023(5) 0.024(5) -0.002(4) 0.001(4) 0.015(4)
O168 0.033(5) 0.013(4) 0.023(4) -0.005(3) -0.001(4) 0.005(4)
O169 0.036(5) 0.015(4) 0.028(5) 0.004(4) 0.004(4) 0.000(4)
O170 0.035(5) 0.018(4) 0.029(5) -0.006(4) 0.002(4) 0.003(4)
O171 0.041(6) 0.061(7) 0.038(6) 0.007(5) -0.008(5) -0.014(5)
O172 0.125(14) 0.072(11) 0.036(9) -0.009(7) 0.039(9) -0.018(9)
O173 0.032(5) 0.020(5) 0.035(5) -0.010(4) 0.002(4) -0.006(4)
O174 0.053(6) 0.012(4) 0.051(6) -0.012(4) 0.033(5) -0.007(4)
O175 0.085(9) 0.012(5) 0.049(7) -0.011(4) 0.039(6) -0.011(5)
O176 0.071(8) 0.016(5) 0.057(7) -0.020(5) 0.036(6) -0.022(5)
O177 0.087(9) 0.009(5) 0.085(9) -0.004(5) 0.061(7) 0.000(5)
O178 0.058(8) 0.045(7) 0.063(8) -0.002(6) 0.001(6) 0.003(6)
O179 0.082(8) 0.014(5) 0.052(7) -0.012(5) 0.038(6) -0.014(5)
O180 0.104(10) 0.011(5) 0.066(8) -0.017(5) 0.055(7) -0.021(6)
O181 0.068(10) 0.048(8) 0.071(9) -0.010(6) 0.021(7) 0.009(7)
O182 0.062(7) 0.014(5) 0.073(8) -0.006(5) 0.045(6) -0.004(5)
O183 0.043(6) 0.049(7) 0.056(7) -0.019(6) -0.018(5) 0.014(5)
O184 0.044(7) 0.033(6) 0.083(9) 0.018(6) -0.019(6) -0.002(5)
O185 0.031(6) 0.078(8) 0.033(6) 0.011(5) 0.004(4) 0.023(6)
O186 0.073(8) 0.016(5) 0.085(9) -0.014(5) 0.052(7) -0.015(5)
O187 0.058(9) 0.152(17) 0.079(11) 0.011(11) 0.036(8) 0.001(10)
O188 0.029(5) 0.041(6) 0.042(6) -0.002(5) 0.008(4) 0.002(4)
O189 0.043(6) 0.024(5) 0.049(6) -0.007(4) 0.000(5) -0.008(4)
O190 0.053(6) 0.023(5) 0.033(5) 0.010(4) 0.004(5) -0.004(4)
O191 0.056(7) 0.036(6) 0.029(5) -0.009(4) 0.003(5) 0.006(5)
O192 0.049(6) 0.012(4) 0.042(6) -0.003(4) -0.006(5) 0.012(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
Mo1 Mo48 0.68(3) . ?
Mo1 O63 1.712(8) . ?
Mo1 O118 1.783(8) . ?
Mo1 O67 1.789(8) . ?
Mo1 O143 2.058(8) . ?
Mo1 O3 2.061(8) . ?
Mo1 O144 2.456(8) . ?
Mo1 K1 3.661(3) . ?
Mo2 O129 1.697(8) . ?
Mo2 O42 1.791(8) . ?
Mo2 O79 1.796(8) . ?
Mo2 O128 2.052(8) . ?
Mo2 O59 2.057(8) . ?
Mo2 O56 2.403(8) . ?
Mo2 K2 3.864(4) . ?
Mo2 K1 4.079(3) 4_545 ?
Mo3 O10 1.695(8) . ?
Mo3 O105 1.776(8) . ?
Mo3 O32 1.791(8) . ?
Mo3 O15 2.050(8) . ?
Mo3 O17 2.069(7) . ?
Mo3 O60 2.454(8) . ?
Mo3 K11 3.692(7) . ?
Mo3 K1 3.798(3) . ?
Mo4 O71 1.672(8) . ?
Mo4 O117 1.992(8) . ?
Mo4 O1 2.001(8) . ?
Mo4 O31 2.010(7) . ?
Mo4 O29 2.013(8) . ?
Mo4 O4 2.019(8) . ?
Mo4 O44 2.355(8) . ?
Mo5 Mo51 0.69(4) . ?
Mo5 O47 1.711(9) . ?
Mo5 O14 1.783(8) . ?
Mo5 O19 1.785(7) . ?
Mo5 O123 2.063(7) . ?
Mo5 O13 2.069(8) . ?
Mo5 O136 2.417(9) . ?
Mo5 K15 3.725(8) 7 ?
Mo6 O43 1.663(8) . ?
Mo6 O9 1.992(8) . ?
Mo6 O143 2.004(8) . ?
Mo6 O101 2.004(8) . ?
Mo6 O3 2.005(8) . ?
Mo6 O78 2.030(8) . ?
Mo6 O41 2.333(8) . ?
Mo6 K4 4.078(4) 7_556 ?
Mo7 O66 1.690(9) . ?
Mo7 O81 1.764(8) . ?
Mo7 O165 1.793(8) . ?
Mo7 O52 2.043(8) 7 ?
Mo7 O98 2.076(8) 7 ?
Mo7 O154 2.382(9) 7 ?
Mo7 K8 3.857(5) . ?
Mo8 O57 1.704(8) . ?
Mo8 O5 1.785(8) . ?
Mo8 O91 1.788(8) . ?
Mo8 O4 2.056(8) 7 ?
Mo8 O1 2.057(8) 7 ?
Mo8 O133 2.453(8) . ?
Mo8 K13 3.782(9) . ?
Mo9 O30 1.709(8) . ?
Mo9 O119 1.778(8) . ?
Mo9 O28 1.778(8) . ?
Mo9 O23 2.048(8) . ?
Mo9 O150 2.061(8) . ?
Mo9 O115 2.439(8) . ?
Mo9 K15 3.714(8) 7 ?
Mo10 O107 1.705(9) . ?
Mo10 O168 1.774(8) . ?
Mo10 O137 1.792(8) . ?
Mo10 O123 2.041(8) . ?
Mo10 O98 2.054(8) . ?
Mo10 O55 2.391(9) . ?
Mo10 K3 3.845(4) . ?
Mo11 O112 1.702(9) . ?
Mo11 O93 1.773(8) . ?
Mo11 O85 1.794(8) . ?
Mo11 O17 2.050(7) . ?
Mo11 O2 2.065(8) . ?
Mo11 O131 2.370(9) . ?
Mo11 K6 3.833(5) . ?
Mo11 K11 3.929(7) . ?
Mo12 O27 1.708(8) . ?
Mo12 O54 1.784(8) . ?
Mo12 O113 1.793(8) . ?
Mo12 O117 2.059(8) . ?
Mo12 O31 2.072(8) . ?
Mo12 O75 2.393(8) . ?
Mo12 K2 3.936(4) . ?
Mo13 Mo47 0.64(3) . ?
Mo13 O127 1.711(9) . ?
Mo13 O8 1.774(8) . ?
Mo13 O110 1.780(8) . ?
Mo13 O13 2.081(8) 7 ?
Mo13 O73 2.081(8) 7 ?
Mo13 O84 2.318(9) . ?
Mo13 K12 3.792(9) . ?
Mo14 O139 1.714(8) . ?
Mo14 O34 1.782(8) . ?
Mo14 O22 1.788(8) . ?
Mo14 O29 2.066(8) . ?
Mo14 O117 2.072(8) . ?
Mo14 O26 2.441(8) . ?
Mo15 O49 1.673(8) . ?
Mo15 O128 1.992(8) . ?
Mo15 O12 1.995(8) . ?
Mo15 O6 1.999(8) . ?
Mo15 O77 2.008(8) . ?
Mo15 O59 2.018(8) . ?
Mo15 O135 2.331(8) . ?
Mo16 O39 1.714(8) . ?
Mo16 O96 1.765(8) . ?
Mo16 O114 1.781(8) . ?
Mo16 O6 2.057(7) . ?
Mo16 O77 2.060(8) . ?
Mo16 O53 2.399(9) . ?
Mo16 K12 3.813(8) . ?
Mo17 O74 1.688(9) . ?
Mo17 O80 1.787(8) . ?
Mo17 O58 1.793(8) . ?
Mo17 O101 2.049(8) . ?
Mo17 O78 2.071(8) . ?
Mo17 O167 2.358(9) . ?
Mo17 K7 3.811(5) . ?
Mo17 K4 3.991(4) 7_556 ?
Mo18 O120 1.699(8) . ?
Mo18 O100 1.775(8) . ?
Mo18 O16 1.777(8) . ?
Mo18 O128 2.055(7) . ?
Mo18 O12 2.065(7) . ?
Mo18 O169 2.437(8) . ?
Mo18 K11 3.813(8) 4_545 ?
Mo18 K1 3.961(3) 4_545 ?
Mo19 O35 1.701(8) . ?
Mo19 O7 1.766(8) . ?
Mo19 O64 1.780(8) . ?
Mo19 O52 2.057(8) 7 ?
Mo19 O73 2.068(7) 7 ?
Mo19 O40 2.438(9) . ?
Mo19 K13 3.755(8) . ?
Mo19 K14 3.778(8) . ?
Mo20 Mo41 0.655(10) . ?
Mo20 O33 1.708(8) . ?
Mo20 O36 1.765(8) . ?
Mo20 O104 1.799(8) . ?
Mo20 O143 2.069(8) . ?
Mo20 O9 2.088(8) . ?
Mo20 O170 2.336(9) . ?
Mo20 K13 3.731(9) . ?
Mo21 O141 1.686(9) . ?
Mo21 O65 1.775(8) . ?
Mo21 O134 1.793(8) . ?
Mo21 O3 2.046(8) . ?
Mo21 O78 2.066(8) . ?
Mo21 O173 2.404(9) . ?
Mo21 K6 3.865(5) . ?
Mo21 K4 3.955(4) 7_556 ?
Mo22 O162 1.698(8) . ?
Mo22 O111 1.779(8) . ?
Mo22 O138 1.790(8) . ?
Mo22 O4 2.056(8) . ?
Mo22 O31 2.066(8) . ?
Mo22 O125 2.376(9) . ?
Mo22 K8 3.843(5) 7 ?
Mo23 Mo53 0.95(3) . ?
Mo23 O87 1.717(17) . ?
Mo23 O166 1.747(10) . ?
Mo23 O176 1.785(9) . ?
Mo23 O158 2.051(9) 7 ?
Mo23 O174 2.058(9) . ?
Mo23 O20 2.341(15) . ?
Mo23 K2 3.655(4) . ?
Mo24 O109 1.690(9) . ?
Mo24 O45 1.776(8) . ?
Mo24 O102 1.790(8) . ?
Mo24 O23 2.053(8) . ?
Mo24 O2 2.063(8) . ?
Mo24 O83 2.397(9) . ?
Mo24 K3 3.860(4) . ?
Mo25 O72 1.692(8) . ?
Mo25 O88 1.784(8) . ?
Mo25 O82 1.792(8) . ?
Mo25 O77 2.046(8) . ?
Mo25 O59 2.064(8) . ?
Mo25 O124 2.381(8) . ?
Mo25 K7 3.830(5) . ?
Mo25 K4 3.875(4) . ?
Mo26 O25 1.669(8) . ?
Mo26 O17 2.002(8) . ?
Mo26 O23 2.004(8) . ?
Mo26 O150 2.008(8) . ?
Mo26 O15 2.008(8) . ?
Mo26 O2 2.017(8) . ?
Mo26 O103 2.345(8) . ?
Mo27 O160 1.713(9) . ?
Mo27 O48 1.785(8) . ?
Mo27 O132 1.796(8) . ?
Mo27 O101 2.056(8) . ?
Mo27 O9 2.059(8) . ?
Mo27 O116 2.435(9) . ?
Mo27 K12 3.779(8) . ?
Mo28 O46 1.674(8) . ?
Mo28 O73 1.989(8) . ?
Mo28 O123 2.003(8) . ?
Mo28 O13 2.006(8) . ?
Mo28 O52 2.011(8) . ?
Mo28 O98 2.016(8) . ?
Mo28 O99 2.348(8) . ?
Mo29 Mo44 0.78(3) . ?
Mo29 O69 1.647(15) . ?
Mo29 O161 1.994(10) . ?
Mo29 O156 1.996(9) . ?
Mo29 O159 1.997(9) . ?
Mo29 O174 2.001(9) . ?
Mo29 O158 2.010(9) 7 ?
Mo29 O178 2.235(13) . ?
Mo30 Mo45 0.591(16) . ?
Mo30 O62 1.692(8) . ?
Mo30 O90 1.775(8) . ?
Mo30 O24 1.785(8) . ?
Mo30 O29 2.069(8) 7 ?
Mo30 O1 2.079(8) 7 ?
Mo30 O94 2.376(9) . ?
Mo30 K1 3.686(3) . ?
Mo31 Mo43 0.99(2) . ?
Mo31 O172 1.70(2) . ?
Mo31 O186 1.758(11) . ?
Mo31 O153 1.776(10) . ?
Mo31 O159 2.045(9) . ?
Mo31 O174 2.054(9) . ?
Mo31 O187 2.351(17) . ?
Mo31 K7 3.594(5) . ?
Mo32 Mo42 0.572(8) . ?
Mo32 O157 1.716(10) . ?
Mo32 O50 1.756(8) . ?
Mo32 O86 1.780(8) . ?
Mo32 O15 2.087(8) 7 ?
Mo32 O150 2.092(8) 7 ?
Mo32 O142 2.320(10) . ?
Mo33 Mo52 0.96(3) . ?
Mo33 O181 1.712(17) . ?
Mo33 O179 1.770(10) . ?
Mo33 O180 1.772(10) . ?
Mo33 O158 2.043(9) . ?
Mo33 O161 2.046(9) 7 ?
Mo33 O145 2.366(16) . ?
Mo33 K8 3.605(5) . ?
Mo34 Mo50 0.89(2) . ?
Mo34 O155 1.726(16) . ?
Mo34 O175 1.762(10) . ?
Mo34 O151 1.774(10) . ?
Mo34 O161 2.047(9) . ?
Mo34 O156 2.047(9) . ?
Mo34 O18 2.383(16) . ?
Mo34 K3 3.620(4) . ?
Mo35 Mo46 0.96(2) . ?
Mo35 O51 1.728(18) . ?
Mo35 O182 1.761(10) . ?
Mo35 O177 1.767(10) . ?
Mo35 O159 2.043(9) . ?
Mo35 O156 2.052(9) . ?
Mo35 O152 2.275(17) . ?
Mo35 K6 3.603(5) . ?
Mo36 Mo49 0.612(3) . ?
Mo36 O70 1.709(10) . ?
Mo36 O11 1.780(8) . ?
Mo36 O38 1.789(9) . ?
Mo36 O12 2.066(8) . ?
Mo36 O6 2.095(8) . ?
Mo36 O146 2.333(10) . ?
Mo36 K15 3.707(9) . ?
Mo41 O170 1.687(15) . ?
Mo41 O104 1.774(10) . ?
Mo41 O36 1.858(10) . ?
Mo41 O9 2.037(9) . ?
Mo41 O143 2.101(10) . ?
Mo41 O33 2.356(15) . ?
Mo41 K13 3.772(11) . ?
Mo42 O142 1.754(16) . ?
Mo42 O86 1.790(9) . ?
Mo42 O50 1.845(10) . ?
Mo42 O15 1.995(9) 7 ?
Mo42 O150 2.051(9) 7 ?
Mo42 O157 2.275(15) . ?
Mo42 K10 3.909(11) . ?
Mo43 O172 0.76(2) . ?
Mo43 O153 2.18(2) . ?
Mo43 O174 2.20(2) . ?
Mo43 O186 2.32(2) . ?
Mo43 O159 2.32(2) . ?
Mo43 K9 3.79(2) . ?
Mo44 O69 0.87(2) . ?
Mo44 O174 2.147(19) . ?
Mo44 O159 2.22(2) . ?
Mo44 O158 2.22(2) 7 ?
Mo44 O156 2.28(2) . ?
Mo44 O161 2.31(2) . ?
Mo45 O94 1.79(2) . ?
Mo45 O24 1.797(11) . ?
Mo45 O90 1.806(11) . ?
Mo45 O29 2.038(10) 7 ?
Mo45 O1 2.047(11) 7 ?
Mo45 O62 2.28(2) . ?
Mo45 K1 3.733(8) . ?
Mo46 O51 0.81(2) . ?
Mo46 O159 2.16(2) . ?
Mo46 O156 2.22(2) . ?
Mo46 O182 2.23(2) . ?
Mo46 O177 2.28(2) . ?
Mo47 O84 1.68(3) . ?
Mo47 O110 1.810(15) . ?
Mo47 O8 1.856(16) . ?
Mo47 O13 2.014(14) 7 ?
Mo47 O73 2.049(14) 7 ?
Mo47 O127 2.34(3) . ?
Mo47 K12 3.857(15) . ?
Mo47 K14 3.89(2) . ?
Mo48 O67 1.740(17) . ?
Mo48 O144 1.78(3) . ?
Mo48 O118 1.837(19) . ?
Mo48 O143 1.991(17) . ?
Mo48 O3 2.085(17) . ?
Mo48 O63 2.39(3) . ?
Mo48 K1 3.663(16) . ?
Mo49 O146 1.722(11) . ?
Mo49 O38 1.781(9) . ?
Mo49 O11 1.817(9) . ?
Mo49 O12 2.068(8) . ?
Mo49 O6 2.068(8) . ?
Mo49 O70 2.317(11) . ?
Mo49 K15 3.755(9) . ?
Mo49 K11 3.756(9) 4_545 ?
Mo50 O155 0.92(2) . ?
Mo50 O156 2.095(19) . ?
Mo50 O161 2.165(19) . ?
Mo50 O151 2.19(2) . ?
Mo50 O175 2.31(2) . ?
Mo50 K5 3.575(19) . ?
Mo51 O14 1.73(2) . ?
Mo51 O136 1.74(4) . ?
Mo51 O19 1.76(2) . ?
Mo51 O13 2.11(2) . ?
Mo51 O123 2.14(2) . ?
Mo51 O47 2.40(4) . ?
Mo51 K15 3.65(2) 7 ?
Mo52 O181 0.86(2) . ?
Mo52 O158 2.08(2) . ?
Mo52 O180 2.19(2) . ?
Mo52 O161 2.23(2) 7 ?
Mo52 O179 2.38(3) . ?
Mo53 O87 0.79(2) . ?
Mo53 O166 2.17(2) . ?
Mo53 O174 2.20(2) . ?
Mo53 O158 2.29(2) 7 ?
Mo53 O176 2.30(3) . ?
V1 O185 1.584(11) . ?
V1 O151 1.922(10) . ?
V1 O85 1.924(8) . ?
V1 O177 1.928(10) . ?
V1 O102 1.944(9) . ?
V2 O121 1.578(11) . ?
V2 O179 1.939(10) . ?
V2 O165 1.944(8) . ?
V2 O137 1.945(8) 7 ?
V2 O175 1.952(10) 7 ?
V3 O183 1.585(11) . ?
V3 O153 1.927(10) . ?
V3 O42 1.929(8) . ?
V3 O82 1.950(8) . ?
V3 O166 1.958(10) . ?
V4 O184 1.600(12) . ?
V4 O134 1.937(8) . ?
V4 O58 1.944(8) . ?
V4 O182 1.946(10) . ?
V4 O186 1.951(10) . ?
V5 O171 1.594(11) . ?
V5 O176 1.932(10) . ?
V5 O180 1.932(10) 7 ?
V5 O113 1.940(8) . ?
V5 O111 1.947(9) . ?
V6 O37 1.644(9) . ?
V6 O80 1.955(9) . ?
V6 O88 1.975(8) . ?
V6 O48 1.981(8) . ?
V6 O96 1.999(8) . ?
V6 O140 2.236(9) . ?
V6 K7 3.696(5) . ?
V7 O95 1.623(9) . ?
V7 O138 1.963(8) 7 ?
V7 O91 1.971(8) . ?
V7 O81 1.987(8) . ?
V7 O7 1.992(8) . ?
V7 O89 2.247(9) . ?
V7 K8 3.715(5) . ?
V8 O97 1.641(8) . ?
V8 O32 1.969(8) 7 ?
V8 O34 1.974(8) . ?
V8 O86 1.974(9) . ?
V8 O90 1.976(8) 7 ?
V8 O122 2.244(8) . ?
V8 K10 3.993(8) . ?
V9 O76 1.693(9) . ?
V9 O50 1.963(8) . ?
V9 O11 1.964(9) . ?
V9 O28 1.966(8) 7 ?
V9 O16 1.970(8) . ?
V9 O68 2.171(9) . ?
V9 K11 3.858(7) 4_545 ?
V9 K15 4.021(9) . ?
V10 O21 1.676(9) . ?
V10 O104 1.957(8) . ?
V10 O132 1.959(8) . ?
V10 O8 1.962(8) . ?
V10 O64 1.976(8) . ?
V10 O61 2.180(9) . ?
V10 K14 4.077(9) . ?
V11 O148 1.597(8) . ?
V11 O100 1.968(8) . ?
V11 O54 1.973(9) . ?
V11 O22 1.978(8) . ?
V11 O79 1.978(8) . ?
V11 O92 2.301(8) . ?
V11 K2 3.749(4) . ?
V12 O147 1.627(9) . ?
V12 O119 1.973(8) . ?
V12 O45 1.975(8) . ?
V12 O19 1.976(8) . ?
V12 O168 1.977(8) . ?
V12 O163 2.255(9) . ?
V12 K3 3.688(5) . ?
V12 K15 4.020(8) 7 ?
V13 O164 1.664(9) . ?
V13 O93 1.976(8) . ?
V13 O105 1.976(8) . ?
V13 O65 1.977(8) . ?
V13 O118 1.988(8) . ?
V13 O149 2.212(10) . ?
V13 K6 3.690(5) . ?
V13 K11 3.867(8) . ?
V13 K1 4.027(3) . ?
V14 O108 1.636(8) . ?
V14 O36 1.968(8) . ?
V14 O5 1.974(8) . ?
V14 O24 1.984(8) . ?
V14 O67 1.993(8) . ?
V14 O106 2.208(8) . ?
V14 K1 3.983(3) . ?
V15 O126 1.762(10) . ?
V15 O38 1.947(8) . ?
V15 O110 1.956(8) . ?
V15 O14 1.963(8) 7 ?
V15 O114 1.968(8) . ?
V15 O130 2.100(9) . ?
K1 O129 2.755(8) 4 ?
K1 O120 2.765(9) 4 ?
K1 O24 2.918(9) . ?
K1 O67 2.929(8) . ?
K1 O118 2.949(8) . ?
K1 O90 3.012(8) . ?
K1 O105 3.045(8) . ?
K1 O32 3.065(9) . ?
K1 O148 3.144(9) 4 ?
K2 O75 2.677(9) . ?
K2 O56 2.721(9) . ?
K2 O20 2.742(13) . ?
K2 O92 2.748(9) . ?
K2 O219 2.82(3) . ?
K2 O79 2.880(9) . ?
K2 O54 3.055(9) . ?
K2 O176 3.085(13) . ?
K2 O166 3.109(13) . ?
K3 O83 2.682(9) . ?
K3 O55 2.690(9) . ?
K3 O163 2.727(10) . ?
K3 O18 2.741(13) . ?
K3 O168 2.925(10) . ?
K3 O45 2.948(10) . ?
K3 O175 2.983(13) . ?
K3 O223 2.99(3) . ?
K3 O151 3.115(14) . ?
K4 O205 2.795(16) . ?
K4 O72 2.827(9) . ?
K4 O207 2.85(2) . ?
K4 O204 2.950(16) 6_556 ?
K4 O141 2.952(10) 7_556 ?
K4 O74 2.979(10) 7_556 ?
K4 O37 2.997(9) . ?
K4 O43 3.043(9) 7_556 ?
K4 O78 3.272(9) 7_556 ?
K4 Mo21 3.955(4) 7_556 ?
K4 Mo17 3.991(4) 7_556 ?
K5 O218 2.81(3) . ?
K5 O218 2.81(3) 2_655 ?
K5 O155 2.863(14) . ?
K5 O155 2.863(14) 2_655 ?
K5 O209 2.924(19) 8_556 ?
K5 O209 2.925(19) 7 ?
K5 O185 2.934(10) 2_655 ?
K5 O185 2.934(10) . ?
K5 Mo50 3.575(19) 2_655 ?
K6 O131 2.664(10) . ?
K6 O173 2.677(10) . ?
K6 O149 2.719(10) . ?
K6 O152 2.770(13) . ?
K6 O93 2.955(9) . ?
K6 O182 2.989(13) . ?
K6 O65 2.989(10) . ?
K6 O211 3.034(19) . ?
K6 O177 3.076(14) . ?
K7 O124 2.652(9) . ?
K7 O167 2.672(10) . ?
K7 O140 2.755(10) . ?
K7 O187 2.778(14) . ?
K7 O231 2.87(4) . ?
K7 O186 2.945(14) . ?
K7 O80 2.950(10) . ?
K7 O88 2.958(10) . ?
K7 O153 3.071(14) . ?
K8 O125 2.673(9) 7 ?
K8 O154 2.688(10) 7 ?
K8 O89 2.759(10) . ?
K8 O145 2.802(14) . ?
K8 O179 2.951(13) . ?
K8 O138 2.959(10) 7 ?
K8 O81 2.977(10) . ?
K8 O180 3.063(14) . ?
K8 O217 3.27(3) . ?
K8 Mo22 3.843(5) 7 ?
K9 O233 2.82(4) . ?
K9 O160 2.834(12) 7_556 ?
K9 O237 2.85(3) 7_556 ?
K9 O184 2.862(13) . ?
K9 O210 2.90(2) . ?
K9 O214 2.91(3) . ?
K9 O224 2.95(3) 7_556 ?
K9 O172 3.135(19) . ?
K9 K12 4.718(13) 7_556 ?
K10 O204 2.750(17) . ?
K10 O232 2.83(3) . ?
K10 O122 2.846(11) . ?
K10 O202 2.864(18) . ?
K10 O205 2.900(18) 6 ?
K10 O86 2.994(11) . ?
K10 O142 3.395(12) . ?
K10 K4 4.105(9) 6 ?
K11 O68 2.623(11) 4 ?
K11 O10 2.713(11) . ?
K11 O112 2.865(11) . ?
K11 O146 2.903(11) 4 ?
K11 O164 2.911(12) . ?
K11 O120 3.098(12) 4 ?
K11 O11 3.260(10) 4 ?
K11 O16 3.264(11) 4 ?
K11 O105 3.404(11) . ?
K11 Mo49 3.756(9) 4 ?
K11 Mo18 3.813(8) 4 ?
K12 O215 2.68(3) . ?
K12 O214 2.83(3) 7_556 ?
K12 O224 2.98(3) . ?
K12 O8 3.050(11) . ?
K12 O132 3.059(11) . ?
K12 O48 3.086(12) . ?
K12 O110 3.091(12) . ?
K12 O96 3.105(12) . ?
K12 O114 3.111(11) . ?
K13 O229 2.72(4) . ?
K13 O216 2.87(3) . ?
K13 O104 3.016(12) . ?
K13 O36 3.020(12) . ?
K13 O64 3.050(11) . ?
K13 O5 3.058(12) . ?
K13 O7 3.059(12) . ?
K13 O91 3.066(12) . ?
K14 O61 2.775(12) . ?
K14 O35 2.868(12) . ?
K14 O46 2.899(11) 8_456 ?
K14 O84 2.921(12) . ?
K14 O66 2.997(12) 2 ?
K14 O242 3.13(4) . ?
K14 O35 3.176(13) 2 ?
K14 O64 3.399(11) . ?
K14 K14 4.786(17) 2 ?
K15 O235 2.83(4) . ?
K15 O11 2.976(12) . ?
K15 O28 2.992(11) 7 ?
K15 O19 2.992(11) 7 ?
K15 O119 3.008(11) 7 ?
K15 O14 3.056(11) 7 ?
K15 O38 3.070(12) . ?
K15 Mo51 3.65(2) 7 ?
K15 Mo9 3.714(8) 7 ?
K15 Mo5 3.725(8) 7 ?
S1 O188 1.434(10) . ?
S1 O154 1.480(9) . ?
S1 O55 1.483(9) . ?
S1 O99 1.518(9) . ?
S2 O189 1.434(10) . ?
S2 O83 1.467(9) . ?
S2 O131 1.486(10) . ?
S2 O103 1.521(9) . ?
S3 O190 1.437(9) . ?
S3 O56 1.464(9) . ?
S3 O124 1.482(9) . ?
S3 O135 1.534(9) . ?
S4 O191 1.439(10) . ?
S4 O173 1.471(9) . ?
S4 O167 1.499(10) . ?
S4 O41 1.540(9) . ?
S5 O192 1.450(9) . ?
S5 O125 1.477(9) . ?
S5 O75 1.478(9) . ?
S5 O44 1.517(8) . ?
S6 O193 1.47(3) . ?
S6 O145 1.610(19) . ?
S6 O20 1.634(18) 7 ?
S6 O178 1.660(16) 7 ?
S6 S8 1.804(19) 7 ?
S6 O195 2.17(5) 7 ?
S7 O194 1.41(5) . ?
S7 O18 1.62(2) . ?
S7 O152 1.64(2) . ?
S7 O178 1.78(2) . ?
S8 O195 1.38(5) . ?
S8 O187 1.65(2) . ?
S8 O178 1.66(2) . ?
S8 O20 1.69(2) . ?
S8 S6 1.804(19) 7 ?
O1 Mo45 2.047(11) 7 ?
O1 Mo8 2.057(8) 7 ?
O1 Mo30 2.079(8) 7 ?
O4 Mo8 2.056(8) 7 ?
O11 K11 3.259(10) 4_545 ?
O13 Mo47 2.014(14) 7 ?
O13 Mo13 2.081(8) 7 ?
O14 V15 1.963(8) 7 ?
O14 K15 3.056(11) 7 ?
O15 Mo42 1.995(9) 7 ?
O15 Mo32 2.087(8) 7 ?
O16 K11 3.263(11) 4_545 ?
O19 K15 2.992(11) 7 ?
O20 S6 1.634(18) 7 ?
O28 V9 1.966(8) 7 ?
O28 K15 2.993(11) 7 ?
O29 Mo45 2.038(10) 7 ?
O29 Mo30 2.069(8) 7 ?
O32 V8 1.969(8) 7 ?
O35 K14 3.176(13) 2 ?
O43 K4 3.043(9) 7_556 ?
O46 K14 2.899(11) 8 ?
O52 Mo7 2.044(8) 7 ?
O52 Mo19 2.057(8) 7 ?
O66 K14 2.997(12) 2 ?
O68 K11 2.623(11) 4_545 ?
O73 Mo47 2.049(14) 7 ?
O73 Mo19 2.068(7) 7 ?
O73 Mo13 2.081(8) 7 ?
O74 K4 2.979(10) 7_556 ?
O78 K4 3.271(9) 7_556 ?
O90 V8 1.976(8) 7 ?
O98 Mo7 2.076(8) 7 ?
O119 K15 3.008(11) 7 ?
O120 K1 2.765(9) 4_545 ?
O120 K11 3.098(12) 4_545 ?
O125 K8 2.673(9) 7 ?
O129 K1 2.754(8) 4_545 ?
O137 V2 1.945(8) 7 ?
O138 V7 1.963(8) 7 ?
O138 K8 2.959(10) 7 ?
O141 K4 2.952(10) 7_556 ?
O146 K11 2.902(11) 4_545 ?
O148 K1 3.144(9) 4_545 ?
O150 Mo42 2.051(9) 7 ?
O150 Mo32 2.092(8) 7 ?
O154 Mo7 2.382(9) 7 ?
O154 K8 2.688(10) 7 ?
O158 Mo29 2.010(9) 7 ?
O158 Mo23 2.051(9) 7 ?
O158 Mo44 2.22(2) 7 ?
O158 Mo53 2.29(2) 7 ?
O160 K9 2.834(12) 7_556 ?
O161 Mo33 2.047(9) 7 ?
O161 Mo52 2.23(2) 7 ?
O175 V2 1.952(10) 7 ?
O178 S6 1.660(16) 7 ?
O180 V5 1.932(10) 7 ?
O193 O195 1.60(5) 7 ?
O195 O193 1.60(5) 7 ?
O195 S6 2.17(5) 7 ?
O204 K4 2.950(16) 6 ?
O205 K10 2.900(18) 6_556 ?
O209 K5 2.925(19) 7 ?
O214 K12 2.83(3) 7_556 ?
O215 O247 1.51(4) . ?
O224 K9 2.95(3) 7_556 ?
O237 K9 2.85(3) 7_556 ?
|
1101226.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/12/1101226.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_1101226
loop_
_publ_author_name
'Qiong Ye'
'Yong-Hua Li'
'Yu-Mei Song'
'Xue-Feng Huang'
'Ren-Gen Xiong'
'Ziling Xue'
_publ_section_title
;
A Second-Order Nonlinear Optical Material Prepared through In Situ
Hydrothermal Ligand Synthesis
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3618
_journal_page_last 3625
_journal_paper_doi 10.1021/ic0500098
_journal_volume 44
_journal_year 2005
_chemical_formula_sum 'C48 H33 N12 O1.5 Zn'
_chemical_formula_weight 867.23
_chemical_name_systematic
;
?
;
_space_group_IT_number 43
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'F 2 -2d'
_symmetry_space_group_name_H-M 'F d d 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 16
_cell_length_a 61.594(9)
_cell_length_b 15.968(2)
_cell_length_c 16.590(2)
_cell_measurement_temperature 293(2)
_cell_volume 16317(4)
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 0.1014
_diffrn_reflns_av_sigmaI/netI 0.1242
_diffrn_reflns_limit_h_max 65
_diffrn_reflns_limit_h_min -73
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 22352
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 2.42
_exptl_absorpt_coefficient_mu 0.659
_exptl_crystal_density_diffrn 1.412
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 7152
_refine_diff_density_max 0.319
_refine_diff_density_min -0.209
_refine_diff_density_rms 0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.05(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.795
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 565
_refine_ls_number_reflns 7043
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.795
_refine_ls_R_factor_all 0.1360
_refine_ls_R_factor_gt 0.0636
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1402
_refine_ls_wR_factor_ref 0.1693
_reflns_number_gt 3768
_reflns_number_total 7043
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ic0500098si20050104_032035_3.cif
_cod_data_source_block 3
_cod_original_formula_sum 'C48 H33 N12 O1.50 Zn'
_cod_database_code 1101226
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.000840(18) 0.26952(5) 0.04953(7) 0.0536(3) Uani 1 1 d . . .
N12 N -0.01777(10) 0.2879(4) 0.1469(4) 0.0522(17) Uani 1 1 d . . .
N11 N 0.01922(10) 0.1703(4) 0.0764(4) 0.0533(16) Uani 1 1 d . . .
C47 C 0.08771(15) 0.0230(6) 0.3005(7) 0.080(3) Uani 1 1 d . . .
H47A H 0.0980 0.0388 0.2624 0.096 Uiso 1 1 calc R . .
C46 C -0.07296(12) 0.2986(4) 0.4689(4) 0.0463(18) Uani 1 1 d . . .
N10 N -0.05857(10) 0.2746(3) 0.4105(4) 0.0549(17) Uani 1 1 d . . .
H10A H -0.0519 0.2274 0.4089 0.066 Uiso 1 1 calc R . .
C45 C -0.04299(11) 0.3224(4) 0.2839(4) 0.0450(18) Uani 1 1 d . . .
C44 C 0.03364(14) 0.1693(5) 0.1387(5) 0.061(2) Uani 1 1 d . . .
H44A H 0.0356 0.2183 0.1680 0.073 Uiso 1 1 calc R . .
C43 C 0.04379(12) 0.0256(4) 0.1165(5) 0.051(2) Uani 1 1 d . . .
C42 C 0.05672(13) -0.0479(4) 0.1333(4) 0.0514(19) Uani 1 1 d . . .
C41 C -0.07969(11) 0.3796(4) 0.4531(4) 0.0422(17) Uani 1 1 d . . .
C40 C -0.05656(12) 0.3377(4) 0.3549(4) 0.0449(18) Uani 1 1 d . . .
C39 C -0.06917(11) 0.4033(4) 0.3771(4) 0.0428(18) Uani 1 1 d . . .
C38 C -0.08058(15) 0.2501(5) 0.5354(6) 0.062(3) Uani 1 1 d . . .
H38A H -0.0756 0.1961 0.5453 0.075 Uiso 1 1 calc R . .
C37 C -0.07042(13) 0.4893(5) 0.3414(4) 0.048(2) Uani 1 1 d . . .
C36 C 0.04548(13) 0.0995(5) 0.1607(4) 0.057(2) Uani 1 1 d . . .
H36A H 0.0546 0.1018 0.2053 0.068 Uiso 1 1 calc R . .
N9 N 0.05860(10) -0.1099(4) 0.0746(4) 0.0574(17) Uani 1 1 d . . .
H9A H 0.0519 -0.1100 0.0292 0.069 Uiso 1 1 calc R . .
C35 C 0.07950(12) -0.1492(4) 0.1777(4) 0.0473(19) Uani 1 1 d . . .
C34 C -0.03294(14) 0.3466(5) 0.1461(5) 0.060(2) Uani 1 1 d . . .
H34A H -0.0352 0.3761 0.0985 0.071 Uiso 1 1 calc R . .
C33 C 0.01788(13) 0.0979(5) 0.0344(5) 0.060(2) Uani 1 1 d . . .
H33A H 0.0089 0.0963 -0.0107 0.072 Uiso 1 1 calc R . .
C32 C -0.01593(14) 0.2443(5) 0.2163(5) 0.065(2) Uani 1 1 d . . .
H32A H -0.0061 0.2003 0.2181 0.078 Uiso 1 1 calc R . .
C31 C -0.08594(13) 0.5148(5) 0.2892(6) 0.061(2) Uani 1 1 d . . .
H31A H -0.0966 0.4773 0.2731 0.073 Uiso 1 1 calc R . .
C30 C 0.12363(15) -0.3191(5) 0.2872(7) 0.076(3) Uani 1 1 d . . .
H30A H 0.1337 -0.3556 0.3100 0.092 Uiso 1 1 calc R . .
C29 C -0.10162(12) 0.5022(4) 0.4989(4) 0.0526(19) Uani 1 1 d . . .
H29A H -0.0965 0.5348 0.4565 0.063 Uiso 1 1 calc R . .
C28 C 0.08039(17) -0.2408(5) 0.0581(7) 0.076(3) Uani 1 1 d . . .
H28A H 0.0750 -0.2539 0.0073 0.092 Uiso 1 1 calc R . .
C27 C 0.10252(15) -0.2734(5) 0.1720(6) 0.066(2) Uani 1 1 d . . .
C26 C -0.10278(12) 0.3700(5) 0.5710(4) 0.053(2) Uani 1 1 d . . .
C25 C 0.02900(12) 0.0275(4) 0.0548(5) 0.057(2) Uani 1 1 d . . .
H25A H 0.0265 -0.0213 0.0257 0.069 Uiso 1 1 calc R . .
C24 C 0.07246(14) -0.1696(5) 0.0994(5) 0.056(2) Uani 1 1 d . . .
C23 C 0.07119(12) -0.0300(4) 0.2789(4) 0.0391(17) Uani 1 1 d . . .
C22 C -0.09525(15) 0.2874(5) 0.5824(5) 0.065(2) Uani 1 1 d . . .
H22A H -0.1009 0.2569 0.6254 0.078 Uiso 1 1 calc R . .
C21 C -0.11580(14) 0.5373(5) 0.5534(5) 0.067(2) Uani 1 1 d . . .
H21A H -0.1197 0.5933 0.5486 0.080 Uiso 1 1 calc R . .
C20 C -0.09474(11) 0.4203(4) 0.5048(4) 0.0477(18) Uani 1 1 d . . .
C19 C 0.11518(14) -0.2554(5) 0.3323(6) 0.075(3) Uani 1 1 d . . .
H19A H 0.1187 -0.2514 0.3866 0.090 Uiso 1 1 calc R . .
C18 C -0.11814(13) 0.4087(6) 0.6232(5) 0.063(2) Uani 1 1 d . . .
H18A H -0.1243 0.3770 0.6643 0.076 Uiso 1 1 calc R . .
C17 C 0.06978(12) -0.0717(4) 0.1971(4) 0.0456(19) Uani 1 1 d . . .
C16 C 0.10157(13) -0.1974(4) 0.2989(5) 0.0577(19) Uani 1 1 d . . .
H16A H 0.0969 -0.1521 0.3294 0.069 Uiso 1 1 calc R . .
C15 C -0.04577(13) 0.3670(5) 0.2124(5) 0.057(2) Uani 1 1 d . . .
H15A H -0.0560 0.4096 0.2090 0.069 Uiso 1 1 calc R . .
C14 C -0.05475(13) 0.5482(4) 0.3638(4) 0.0505(19) Uani 1 1 d . . .
H14A H -0.0438 0.5315 0.3988 0.061 Uiso 1 1 calc R . .
C13 C 0.05615(13) -0.0516(4) 0.3351(5) 0.053(2) Uani 1 1 d . . .
H13A H 0.0446 -0.0859 0.3206 0.064 Uiso 1 1 calc R . .
C12 C -0.02762(13) 0.2613(5) 0.2832(5) 0.061(2) Uani 1 1 d . . .
H12A H -0.0251 0.2305 0.3298 0.073 Uiso 1 1 calc R . .
C11 C -0.12412(14) 0.4894(6) 0.6152(5) 0.071(2) Uani 1 1 d . . .
H11A H -0.1339 0.5129 0.6515 0.086 Uiso 1 1 calc R . .
C10 C 0.09452(12) -0.2060(4) 0.2171(5) 0.053(2) Uani 1 1 d . . .
C9 C -0.08614(14) 0.5968(5) 0.2591(5) 0.069(2) Uani 1 1 d . . .
H9B H -0.0966 0.6124 0.2215 0.083 Uiso 1 1 calc R . .
C8 C 0.11743(15) -0.3293(5) 0.2094(7) 0.080(3) Uani 1 1 d . . .
H8A H 0.1230 -0.3739 0.1799 0.096 Uiso 1 1 calc R . .
C7 C 0.08925(16) 0.0532(6) 0.3778(6) 0.086(3) Uani 1 1 d . . .
H7A H 0.1008 0.0877 0.3919 0.103 Uiso 1 1 calc R . .
C6 C 0.09537(17) -0.2888(5) 0.0912(5) 0.071(3) Uani 1 1 d . . .
H6A H 0.1013 -0.3329 0.0619 0.085 Uiso 1 1 calc R . .
C80 C -0.05469(12) 0.6297(4) 0.3366(4) 0.0451(18) Uani 1 1 d . . .
C5 C -0.03931(12) 0.6904(4) 0.3716(4) 0.0473(18) Uani 1 1 d . . .
C4 C -0.07106(14) 0.6542(4) 0.2844(5) 0.062(2) Uani 1 1 d . . .
H4A H -0.0718 0.7094 0.2666 0.074 Uiso 1 1 calc R . .
N8 N -0.03402(13) 0.7640(4) 0.3389(4) 0.074(2) Uani 1 1 d . . .
N7 N -0.02907(11) 0.6783(4) 0.4411(4) 0.0564(18) Uani 1 1 d . . .
N6 N -0.01978(12) 0.7986(4) 0.3910(5) 0.072(2) Uani 1 1 d . . .
N5 N -0.01757(11) 0.7475(4) 0.4515(4) 0.0558(16) Uani 1 1 d . . .
C3 C 0.05778(13) -0.0228(4) 0.4143(5) 0.055(2) Uani 1 1 d . . .
C2 C 0.04230(14) -0.0555(5) 0.4759(5) 0.058(2) Uani 1 1 d . . .
C1 C 0.07393(15) 0.0328(5) 0.4343(5) 0.079(3) Uani 1 1 d . . .
H1A H 0.0744 0.0563 0.4855 0.095 Uiso 1 1 calc R . .
N4 N 0.03129(11) -0.1256(4) 0.4659(4) 0.0573(18) Uani 1 1 d . . .
N3 N 0.03931(15) -0.0223(4) 0.5482(5) 0.099(3) Uani 1 1 d . . .
N2 N 0.02025(11) -0.1341(4) 0.5326(4) 0.0579(17) Uani 1 1 d . . .
N1 N 0.02440(15) -0.0730(5) 0.5816(5) 0.100(3) Uani 1 1 d . . .
O1W O 0.0000 0.0000 -0.1238(7) 0.157(6) Uani 1 2 d S . .
O2W O 0.0000 0.0000 0.7163(7) 0.138(4) Uani 1 2 d S . .
O4W O 0.0000 0.0000 0.303(2) 0.55(4) Uani 1 2 d S . .
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 0.0672(5) 0.0511(4) 0.0425(4) -0.0008(5) 0.0085(5) 0.0017(6)
N12 0.060(4) 0.057(4) 0.040(4) 0.005(3) 0.005(3) 0.007(3)
N11 0.063(4) 0.057(4) 0.040(4) -0.008(3) 0.001(3) 0.002(3)
C47 0.097(7) 0.089(6) 0.054(5) -0.014(5) 0.015(7) -0.041(6)
C46 0.051(5) 0.051(4) 0.037(4) 0.005(4) 0.007(4) -0.005(4)
N10 0.072(5) 0.041(3) 0.052(4) 0.006(3) 0.006(3) 0.011(3)
C45 0.050(4) 0.053(4) 0.033(4) 0.005(3) -0.002(3) 0.005(4)
C44 0.077(6) 0.046(5) 0.060(6) -0.008(4) -0.005(5) 0.008(4)
C43 0.058(5) 0.051(5) 0.043(5) -0.012(4) 0.012(4) -0.001(4)
C42 0.061(5) 0.053(5) 0.040(5) -0.005(3) 0.003(4) 0.000(4)
C41 0.048(4) 0.051(4) 0.028(4) 0.010(3) 0.002(3) -0.003(3)
C40 0.053(5) 0.035(4) 0.047(5) 0.009(3) -0.001(4) 0.005(3)
C39 0.045(4) 0.044(4) 0.039(4) 0.003(3) -0.002(3) 0.001(4)
C38 0.075(6) 0.054(6) 0.059(7) 0.025(5) 0.004(5) -0.003(4)
C37 0.049(5) 0.063(5) 0.031(4) 0.003(4) 0.007(4) 0.010(4)
C36 0.073(6) 0.063(5) 0.034(4) -0.003(4) -0.006(4) -0.004(4)
N9 0.066(4) 0.067(4) 0.039(4) -0.023(3) -0.005(3) 0.005(3)
C35 0.059(5) 0.049(4) 0.033(4) -0.006(3) 0.000(4) 0.000(4)
C34 0.079(6) 0.062(5) 0.037(5) 0.014(4) 0.005(4) 0.019(5)
C33 0.078(6) 0.057(5) 0.044(5) -0.013(4) -0.005(4) 0.008(4)
C32 0.077(6) 0.065(5) 0.053(5) 0.022(4) 0.013(5) 0.028(5)
C31 0.055(5) 0.066(5) 0.063(6) 0.012(5) -0.016(5) -0.004(4)
C30 0.078(6) 0.065(6) 0.086(8) 0.000(5) -0.011(6) 0.015(5)
C29 0.059(5) 0.063(5) 0.036(4) 0.014(4) 0.002(4) 0.011(4)
C28 0.106(8) 0.061(6) 0.063(7) -0.028(5) -0.002(7) 0.017(5)
C27 0.083(6) 0.044(4) 0.072(6) 0.008(4) 0.012(5) 0.015(4)
C26 0.052(5) 0.071(5) 0.035(5) 0.013(3) -0.010(4) -0.021(4)
C25 0.065(5) 0.053(5) 0.054(5) -0.016(4) -0.004(5) 0.008(4)
C24 0.072(6) 0.058(5) 0.038(5) 0.001(4) 0.003(4) -0.002(4)
C23 0.050(4) 0.039(4) 0.028(4) -0.006(3) 0.009(3) -0.008(3)
C22 0.093(7) 0.054(5) 0.047(5) 0.018(4) 0.023(5) -0.019(5)
C21 0.079(6) 0.073(5) 0.048(5) 0.010(5) 0.015(5) 0.014(4)
C20 0.047(4) 0.058(5) 0.038(4) 0.012(3) -0.003(3) 0.002(4)
C19 0.079(6) 0.064(5) 0.082(7) 0.001(5) -0.013(5) 0.008(5)
C18 0.063(5) 0.093(7) 0.034(4) -0.006(4) 0.018(4) -0.015(5)
C17 0.061(5) 0.044(4) 0.032(4) -0.006(3) 0.007(4) -0.003(4)
C16 0.077(5) 0.049(4) 0.047(5) -0.011(4) 0.005(5) 0.005(4)
C15 0.077(6) 0.058(5) 0.038(5) 0.005(4) 0.000(4) 0.020(4)
C14 0.062(5) 0.055(5) 0.034(4) 0.010(3) 0.000(4) 0.009(4)
C13 0.056(5) 0.050(4) 0.053(5) -0.019(4) -0.008(4) -0.005(4)
C12 0.071(5) 0.060(5) 0.053(6) 0.009(4) 0.006(5) 0.005(5)
C11 0.065(6) 0.096(7) 0.053(6) -0.006(5) 0.009(5) 0.005(5)
C10 0.055(5) 0.037(4) 0.068(6) -0.010(4) 0.013(4) -0.010(4)
C9 0.072(6) 0.067(6) 0.067(6) 0.024(5) -0.028(5) 0.006(5)
C8 0.085(7) 0.059(6) 0.097(8) -0.026(5) 0.022(6) 0.006(5)
C7 0.091(7) 0.105(7) 0.061(7) -0.028(6) 0.011(5) -0.035(6)
C6 0.103(7) 0.049(5) 0.062(6) -0.026(4) 0.018(6) 0.008(5)
C80 0.051(5) 0.043(4) 0.041(4) 0.017(3) 0.014(4) 0.003(3)
C5 0.061(5) 0.043(4) 0.038(4) 0.009(3) 0.008(4) 0.003(4)
C4 0.077(6) 0.043(4) 0.065(6) 0.015(4) -0.019(5) -0.002(4)
N8 0.091(6) 0.077(5) 0.055(5) 0.025(4) -0.013(4) -0.007(4)
N7 0.064(5) 0.069(5) 0.036(4) 0.004(3) -0.004(3) 0.002(4)
N6 0.085(6) 0.071(5) 0.061(5) 0.017(4) -0.012(4) -0.012(4)
N5 0.062(4) 0.058(4) 0.048(4) 0.004(3) 0.000(3) -0.007(4)
C3 0.069(6) 0.046(4) 0.051(5) -0.016(4) 0.010(4) -0.004(4)
C2 0.079(6) 0.045(4) 0.049(5) -0.015(4) 0.017(4) -0.006(4)
C1 0.112(8) 0.080(6) 0.046(5) -0.039(4) 0.002(5) -0.034(6)
N4 0.075(5) 0.055(4) 0.042(4) -0.009(3) 0.016(4) -0.003(4)
N3 0.160(8) 0.075(5) 0.062(5) -0.043(5) 0.051(6) -0.053(5)
N2 0.075(5) 0.058(4) 0.041(4) -0.005(3) 0.017(3) -0.001(3)
N1 0.152(8) 0.081(5) 0.067(5) -0.030(4) 0.044(5) -0.044(5)
O1W 0.099(9) 0.312(18) 0.059(7) 0.000 0.000 0.057(10)
O2W 0.132(10) 0.209(13) 0.073(8) 0.000 0.000 -0.018(9)
O4W 0.144(16) 1.26(12) 0.24(3) 0.000 0.000 0.16(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'
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
N2 Zn1 N12 110.4(3) 5_554 . ?
N2 Zn1 N11 107.9(3) 5_554 . ?
N12 Zn1 N11 105.1(2) . . ?
N2 Zn1 N5 111.3(3) 5_554 5_544 ?
N12 Zn1 N5 110.8(2) . 5_544 ?
N11 Zn1 N5 111.2(3) . 5_544 ?
C34 N12 C32 115.6(7) . . ?
C34 N12 Zn1 120.0(5) . . ?
C32 N12 Zn1 124.4(5) . . ?
C33 N11 C44 114.8(7) . . ?
C33 N11 Zn1 121.9(6) . . ?
C44 N11 Zn1 123.2(5) . . ?
C7 C47 C23 120.8(9) . . ?
N10 C46 C41 108.8(6) . . ?
N10 C46 C38 127.5(7) . . ?
C41 C46 C38 123.8(7) . . ?
C46 N10 C40 109.2(6) . . ?
C12 C45 C15 116.4(7) . . ?
C12 C45 C40 121.5(6) . . ?
C15 C45 C40 122.0(6) . . ?
C36 C44 N11 123.7(7) . . ?
C25 C43 C36 115.1(7) . . ?
C25 C43 C42 121.9(6) . . ?
C36 C43 C42 123.0(7) . . ?
C17 C42 N9 106.9(6) . . ?
C17 C42 C43 133.8(7) . . ?
N9 C42 C43 119.2(7) . . ?
C46 C41 C20 120.6(6) . . ?
C46 C41 C39 105.8(6) . . ?
C20 C41 C39 133.5(6) . . ?
C39 C40 N10 109.4(6) . . ?
C39 C40 C45 132.4(6) . . ?
N10 C40 C45 118.1(6) . . ?
C40 C39 C37 129.1(6) . . ?
C40 C39 C41 106.7(6) . . ?
C37 C39 C41 123.7(6) . . ?
C22 C38 C46 115.6(7) . . ?
C31 C37 C14 117.1(7) . . ?
C31 C37 C39 124.4(7) . . ?
C14 C37 C39 118.4(7) . . ?
C44 C36 C43 120.3(8) . . ?
C24 N9 C42 110.1(6) . . ?
C17 C35 C24 106.4(7) . . ?
C17 C35 C10 135.7(7) . . ?
C24 C35 C10 117.9(7) . . ?
N12 C34 C15 123.9(7) . . ?
C25 C33 N11 123.3(8) . . ?
N12 C32 C12 123.6(7) . . ?
C37 C31 C9 121.0(8) . . ?
C19 C30 C8 120.2(8) . . ?
C20 C29 C21 122.3(7) . . ?
C6 C28 C24 120.5(10) . . ?
C8 C27 C10 118.5(9) . . ?
C8 C27 C6 119.9(8) . . ?
C10 C27 C6 121.6(8) . . ?
C22 C26 C18 122.9(7) . . ?
C22 C26 C20 120.5(7) . . ?
C18 C26 C20 116.6(7) . . ?
C33 C25 C43 122.6(7) . . ?
N9 C24 C28 129.9(8) . . ?
N9 C24 C35 108.3(7) . . ?
C28 C24 C35 121.8(9) . . ?
C47 C23 C13 118.9(7) . . ?
C47 C23 C17 123.3(7) . . ?
C13 C23 C17 117.7(6) . . ?
C26 C22 C38 124.2(7) . . ?
C29 C21 C11 119.9(8) . . ?
C29 C20 C41 126.3(6) . . ?
C29 C20 C26 118.4(7) . . ?
C41 C20 C26 115.3(6) . . ?
C30 C19 C16 121.1(9) . . ?
C11 C18 C26 122.5(8) . . ?
C42 C17 C35 108.3(6) . . ?
C42 C17 C23 126.7(7) . . ?
C35 C17 C23 124.4(7) . . ?
C19 C16 C10 120.3(7) . . ?
C45 C15 C34 118.9(7) . . ?
C37 C14 C80 123.4(7) . . ?
C23 C13 C3 120.9(7) . . ?
C45 C12 C32 121.5(7) . . ?
C18 C11 C21 120.2(8) . . ?
C27 C10 C16 118.2(7) . . ?
C27 C10 C35 117.7(8) . . ?
C16 C10 C35 124.1(6) . . ?
C31 C9 C4 120.6(7) . . ?
C27 C8 C30 121.4(8) . . ?
C47 C7 C1 120.6(9) . . ?
C28 C6 C27 120.3(8) . . ?
C14 C80 C4 118.0(7) . . ?
C14 C80 C5 119.6(7) . . ?
C4 C80 C5 121.9(6) . . ?
N8 C5 N7 111.4(7) . . ?
N8 C5 C80 125.1(7) . . ?
N7 C5 C80 123.5(6) . . ?
C9 C4 C80 119.7(6) . . ?
C5 N8 N6 105.0(6) . . ?
N5 N7 C5 104.2(6) . . ?
N5 N6 N8 107.8(6) . . ?
N6 N5 N7 111.5(7) . . ?
N6 N5 Zn1 125.0(6) . 5 ?
N7 N5 Zn1 123.5(5) . 5 ?
C1 C3 C13 119.5(7) . . ?
C1 C3 C2 121.6(7) . . ?
C13 C3 C2 118.9(7) . . ?
N4 C2 N3 112.5(7) . . ?
N4 C2 C3 122.6(7) . . ?
N3 C2 C3 124.7(7) . . ?
C3 C1 C7 119.2(7) . . ?
N2 N4 C2 104.4(6) . . ?
N1 N3 C2 103.1(7) . . ?
N1 N2 N4 110.5(6) . . ?
N1 N2 Zn1 128.3(5) . 5_545 ?
N4 N2 Zn1 121.2(5) . 5_545 ?
N2 N1 N3 109.3(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 1.968(6) 5_554 ?
Zn1 N12 2.002(6) . ?
Zn1 N11 1.998(6) . ?
Zn1 N5 2.013(7) 5_544 ?
N12 C34 1.324(9) . ?
N12 C32 1.350(9) . ?
N11 C33 1.351(8) . ?
N11 C44 1.364(10) . ?
C47 C7 1.373(14) . ?
C47 C23 1.372(11) . ?
C46 N10 1.368(9) . ?
C46 C41 1.383(9) . ?
C46 C38 1.427(11) . ?
N10 C40 1.371(8) . ?
C45 C12 1.360(9) . ?
C45 C15 1.393(9) . ?
C45 C40 1.465(9) . ?
C44 C36 1.381(11) . ?
C43 C25 1.370(11) . ?
C43 C36 1.393(10) . ?
C43 C42 1.446(10) . ?
C42 C17 1.382(10) . ?
C42 N9 1.394(8) . ?
C41 C20 1.421(10) . ?
C41 C39 1.466(10) . ?
C40 C39 1.356(9) . ?
C39 C37 1.498(9) . ?
C38 C22 1.333(11) . ?
C37 C31 1.352(11) . ?
C37 C14 1.398(10) . ?
N9 C24 1.343(9) . ?
C35 C17 1.411(10) . ?
C35 C24 1.408(10) . ?
C35 C10 1.451(10) . ?
C34 C15 1.393(10) . ?
C33 C25 1.359(10) . ?
C32 C12 1.350(11) . ?
C31 C9 1.402(11) . ?
C30 C19 1.365(12) . ?
C30 C8 1.356(13) . ?
C29 C20 1.378(9) . ?
C29 C21 1.378(10) . ?
C28 C6 1.320(12) . ?
C28 C24 1.415(11) . ?
C27 C8 1.423(12) . ?
C27 C10 1.400(11) . ?
C27 C6 1.433(12) . ?
C26 C22 1.412(10) . ?
C26 C18 1.423(10) . ?
C26 C20 1.448(9) . ?
C23 C13 1.359(10) . ?
C23 C17 1.514(9) . ?
C21 C11 1.378(11) . ?
C19 C16 1.367(11) . ?
C18 C11 1.348(11) . ?
C16 C10 1.431(11) . ?
C14 C80 1.377(9) . ?
C13 C3 1.396(10) . ?
C9 C4 1.372(10) . ?
C7 C1 1.369(12) . ?
C80 C4 1.385(10) . ?
C80 C5 1.474(10) . ?
C5 N8 1.335(9) . ?
C5 N7 1.329(9) . ?
N8 N6 1.349(10) . ?
N7 N5 1.325(8) . ?
N6 N5 1.301(8) . ?
N5 Zn1 2.013(7) 5 ?
C3 C1 1.374(10) . ?
C3 C2 1.493(11) . ?
C2 N4 1.319(9) . ?
C2 N3 1.324(10) . ?
N4 N2 1.306(8) . ?
N3 N1 1.344(9) . ?
N2 N1 1.296(9) . ?
N2 Zn1 1.968(6) 5_545 ?
|
1200000.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-13 01:26:53 +0300 (Mon, 13 Aug 2018) $
#$Revision: 209639 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200000.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_1200000
loop_
_publ_author_name
'Otto, Stefanus'
'Muller, Alfred Johannes'
_publ_section_title
;
cis-Dichlorobis(triethylarsine)platinum(II) and
cis-dichlorobis(triethylphosphine)platinum(II)
;
_journal_coden_ASTM ACSCEE
_journal_issue 12
_journal_name_full
;
Acta Crystallographica, Section C: Crystal Structure Communications
;
_journal_page_first 1405
_journal_page_last 1407
_journal_paper_doi 10.1107/S0108270101016043
_journal_volume 57
_journal_year 2001
_chemical_formula_iupac '[Pt Cl2 (C6 H15 P1)2]'
_chemical_formula_moiety 'C12 H30 Cl2 P2 Pt'
_chemical_formula_sum 'C12 H30 Cl2 P2 Pt'
_chemical_formula_weight 502.29
_chemical_name_systematic cis-dichlorobis(triethylphosphine)platinum(II)
_space_group_crystal_system monoclinic
_space_group_IT_number 9
_space_group_name_Hall 'C -2yc'
_space_group_name_H-M_alt 'C 1 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 117.31(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.773(4)
_cell_length_b 7.5310(15)
_cell_length_c 13.726(3)
_cell_measurement_reflns_used 6951
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 31.66
_cell_measurement_theta_min 2.32
_cell_volume 1816.1(6)
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)'
_computing_publication_material SHELXL97
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full .901
_diffrn_measured_fraction_theta_max .901
_diffrn_measurement_device_type 'Siemens SMART CCD'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength .71073
_diffrn_reflns_av_R_equivalents .0530
_diffrn_reflns_av_sigmaI/netI .0425
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 9281
_diffrn_reflns_theta_full 32.03
_diffrn_reflns_theta_max 32.03
_diffrn_reflns_theta_min 2.94
_diffrn_standards_decay_% 0
_diffrn_standards_number
'First 50 frames repeated after data collection.'
_exptl_absorpt_coefficient_mu 8.178
_exptl_absorpt_correction_T_max .229
_exptl_absorpt_correction_T_min .092
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.837
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rectangular
_exptl_crystal_F_000 976
_exptl_crystal_size_max .35
_exptl_crystal_size_mid .30
_exptl_crystal_size_min .18
_exptl_special_details
;
For both complexes, the intensity data were collected on a Siemens SMART CCD
diffractometer using an exposure time of 15 s per frame for (I) and 20
s per frame for (II). A total of 1890 frames with a frame width of 0.25\%
were collected for (I) and 2250 frames with a frame width of 0.20\% were
collected for (II). A completeness of 98.9% was accomplished up to \q =
30.50\% for (I), while the completeness was 99.0% at \q = 30.51\% for (II).
The first 50 frames were recollected at the end of each data collection to
check for decay; no decay was found for either data collection.
;
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max .978
_refine_diff_density_min -2.063
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack '0.035(10), 1109 Friedel pairs'
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 162
_refine_ls_number_reflns 4284
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.020
_refine_ls_R_factor_all .0363
_refine_ls_R_factor_gt .0341
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0648P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt .0906
_refine_ls_wR_factor_ref .0921
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_reflns_number_gt 4059
_reflns_number_total 4284
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 2012395
_cod_depositor_comments
;
Adding additional information after consulting the original
supplementary material.
Antanas Vaitkus,
2018-08-13
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'C c'
_cod_database_code 1200000
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y,z+1/2
3 x+1/2,y+1/2,z
4 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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pt Pt .08960(2) .33029(2) .14145(2) .02873(7) Uani d . 1
P1 P -.03044(11) .3783(3) .00820(15) .0323(3) Uani d . 1
P2 P .15326(11) .4669(2) .06151(15) .0310(3) Uani d . 1
Cl1 Cl .20485(12) .2581(3) .29721(16) .0456(4) Uani d . 1
Cl2 Cl .02913(17) .1786(3) .2319(2) .0523(6) Uani d . 1
C111 C -.0511(5) .5107(13) -.1136(8) .049(2) Uani d . 1
H11A H -.0258 .6245 -.0897 .056(6) Uiso calc R 1
H11B H -.0285 .4517 -.1544 .056(6) Uiso calc R 1
C112 C -.1338(6) .5451(17) -.1910(10) .064(3) Uani d . 1
H11C H -.1584 .4353 -.2235 .113(11) Uiso calc R 1
H11D H -.1375 .6256 -.2475 .113(11) Uiso calc R 1
H11E H -.1582 .5966 -.1511 .113(11) Uiso calc R 1
C121 C -.0784(6) .1672(9) -.0468(9) .0429(19) Uani d . 1
H12A H -.0771 .0963 .0130 .056(6) Uiso calc R 1
H12B H -.1313 .1907 -.0971 .056(6) Uiso calc R 1
C122 C -.0438(7) .0607(13) -.1061(10) .064(3) Uani d . 1
H12C H -.0488 .1254 -.1694 .113(11) Uiso calc R 1
H12D H -.0697 -.0510 -.1288 .113(11) Uiso calc R 1
H12E H .0091 .0402 -.0579 .113(11) Uiso calc R 1
C131 C -.0886(6) .4812(12) .0646(8) .0488(19) Uani d . 1
H13A H -.1410 .4856 .0079 .056(6) Uiso calc R 1
H13B H -.0869 .4073 .1235 .056(6) Uiso calc R 1
C132 C -.0632(11) .6688(13) .1085(15) .073(4) Uani d . 1
H13C H -.0113 .6661 .1645 .113(11) Uiso calc R 1
H13D H -.0950 .7134 .1389 .113(11) Uiso calc R 1
H13E H -.0674 .7448 .0498 .113(11) Uiso calc R 1
C211 C .2563(5) .4640(12) .1434(7) .0455(17) Uani d . 1
H21A H .2693 .5226 .2127 .056(6) Uiso calc R 1
H21B H .2729 .3415 .1594 .056(6) Uiso calc R 1
C212 C .3006(6) .5532(15) .0900(9) .055(2) Uani d . 1
H21C H .2826 .5093 .0166 .113(11) Uiso calc R 1
H21D H .3538 .5269 .1318 .113(11) Uiso calc R 1
H21E H .2931 .6794 .0880 .113(11) Uiso calc R 1
C221 C .1378(6) .3677(13) -.0688(8) .0455(18) Uani d . 1
H22A H .0836 .3611 -.1175 .056(6) Uiso calc R 1
H22B H .1606 .4430 -.1032 .056(6) Uiso calc R 1
C222 C .1726(11) .1801(12) -.0526(13) .071(4) Uani d . 1
H22C H .2267 .1893 -.0251 .113(11) Uiso calc R 1
H22D H .1510 .1184 -.1214 .113(11) Uiso calc R 1
H22E H .1617 .1159 -.0010 .113(11) Uiso calc R 1
C231 C .1332(6) .7041(11) .0355(9) .047(2) Uani d . 1
H23A H .1643 .7531 .0042 .056(6) Uiso calc R 1
H23B H .0802 .7204 -.0172 .056(6) Uiso calc R 1
C232 C .1498(10) .8042(15) .1424(14) .074(4) Uani d . 1
H23C H .1326 .7344 .1852 .113(11) Uiso calc R 1
H23D H .1236 .9161 .1247 .113(11) Uiso calc R 1
H23E H .2036 .8244 .1836 .113(11) Uiso calc R 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pt .02999(12) .03011(10) .02696(10) .00048(11) .01382(8) .00179(11)
P1 .0290(9) .0342(7) .0346(8) .0027(7) .0154(7) .0041(7)
P2 .0317(8) .0308(7) .0311(8) -.0016(6) .0150(7) .0018(6)
Cl1 .0347(9) .0601(12) .0355(9) .0036(8) .0104(7) .0104(8)
Cl2 .0498(14) .0678(14) .0450(12) -.0028(9) .0265(11) .0167(8)
C111 .032(4) .065(5) .048(5) .007(4) .016(3) .022(4)
C112 .043(5) .083(6) .060(6) .015(5) .018(4) .033(5)
C121 .029(4) .044(4) .047(5) -.007(3) .010(4) -.003(3)
C122 .073(7) .040(4) .079(7) -.004(4) .034(6) -.015(4)
C131 .047(5) .059(5) .047(5) .012(4) .027(4) .003(3)
C132 .096(12) .057(7) .083(10) .015(5) .054(10) -.006(4)
C211 .037(4) .056(4) .042(4) -.001(3) .017(3) .009(3)
C212 .042(5) .071(6) .053(5) -.016(4) .023(4) .002(4)
C221 .048(5) .049(4) .044(4) .001(4) .025(4) -.005(3)
C222 .106(13) .053(6) .074(9) -.007(5) .057(9) -.022(4)
C231 .048(5) .034(3) .058(5) -.008(3) .025(4) .001(3)
C232 .096(11) .046(5) .091(10) -.010(5) .052(9) -.016(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Pt Cl2 . . 85.66(9) yes
P1 Pt P2 . . 98.39(7) yes
P1 Pt Cl1 . . 170.26(7) yes
P2 Pt Cl2 . . 176.82(8) yes
P1 Pt Cl2 . . 84.63(9) yes
P2 Pt Cl1 . . 91.33(7) yes
C111 P1 C131 . . 103.7(4) yes
C111 P1 C121 . . 104.0(5) yes
C131 P1 C121 . . 103.7(5) yes
C111 P1 Pt . . 122.6(3) ?
C131 P1 Pt . . 110.8(3) ?
C121 P1 Pt . . 110.4(3) ?
C211 P2 C231 . . 102.3(4) yes
C211 P2 C221 . . 103.6(5) yes
C231 P2 C221 . . 106.5(5) yes
C211 P2 Pt . . 114.2(3) ?
C231 P2 Pt . . 114.8(3) ?
C221 P2 Pt . . 114.1(3) ?
C112 C111 P1 . . 117.0(6) ?
C112 C111 H11A . . 108.1 ?
P1 C111 H11A . . 108.1 ?
C112 C111 H11B . . 108.1 ?
P1 C111 H11B . . 108.1 ?
H11A C111 H11B . . 107.3 ?
C111 C112 H11C . . 109.5 ?
C111 C112 H11D . . 109.5 ?
H11C C112 H11D . . 109.5 ?
C111 C112 H11E . . 109.5 ?
H11C C112 H11E . . 109.5 ?
H11D C112 H11E . . 109.5 ?
C122 C121 P1 . . 114.0(7) ?
C122 C121 H12A . . 108.7 ?
P1 C121 H12A . . 108.7 ?
C122 C121 H12B . . 108.7 ?
P1 C121 H12B . . 108.7 ?
H12A C121 H12B . . 107.6 ?
C121 C122 H12C . . 109.5 ?
C121 C122 H12D . . 109.5 ?
H12C C122 H12D . . 109.5 ?
C121 C122 H12E . . 109.5 ?
H12C C122 H12E . . 109.5 ?
H12D C122 H12E . . 109.5 ?
C132 C131 P1 . . 113.8(8) ?
C132 C131 H13A . . 108.8 ?
P1 C131 H13A . . 108.8 ?
C132 C131 H13B . . 108.8 ?
P1 C131 H13B . . 108.8 ?
H13A C131 H13B . . 107.7 ?
C131 C132 H13C . . 109.5 ?
C131 C132 H13D . . 109.5 ?
H13C C132 H13D . . 109.5 ?
C131 C132 H13E . . 109.5 ?
H13C C132 H13E . . 109.5 ?
H13D C132 H13E . . 109.5 ?
C212 C211 P2 . . 115.0(6) ?
C212 C211 H21A . . 108.5 ?
P2 C211 H21A . . 108.5 ?
C212 C211 H21B . . 108.5 ?
P2 C211 H21B . . 108.5 ?
H21A C211 H21B . . 107.5 ?
C211 C212 H21C . . 109.5 ?
C211 C212 H21D . . 109.5 ?
H21C C212 H21D . . 109.5 ?
C211 C212 H21E . . 109.5 ?
H21C C212 H21E . . 109.5 ?
H21D C212 H21E . . 109.5 ?
C222 C221 P2 . . 111.6(8) ?
C222 C221 H22A . . 109.3 ?
P2 C221 H22A . . 109.3 ?
C222 C221 H22B . . 109.3 ?
P2 C221 H22B . . 109.3 ?
H22A C221 H22B . . 108.0 ?
C221 C222 H22C . . 109.5 ?
C221 C222 H22D . . 109.5 ?
H22C C222 H22D . . 109.5 ?
C221 C222 H22E . . 109.5 ?
H22C C222 H22E . . 109.5 ?
H22D C222 H22E . . 109.5 ?
C232 C231 P2 . . 111.0(8) ?
C232 C231 H23A . . 109.4 ?
P2 C231 H23A . . 109.4 ?
C232 C231 H23B . . 109.4 ?
P2 C231 H23B . . 109.4 ?
H23A C231 H23B . . 108.0 ?
C231 C232 H23C . . 109.5 ?
C231 C232 H23D . . 109.5 ?
H23C C232 H23D . . 109.5 ?
C231 C232 H23E . . 109.5 ?
H23C C232 H23E . . 109.5 ?
H23D C232 H23E . . 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
Pt P1 . 2.264(2) yes
Pt P2 . 2.2616(18) yes
Pt Cl1 . 2.364(2) yes
Pt Cl2 . 2.374(2) yes
P1 C111 . 1.824(8) yes
P1 C131 . 1.827(9) yes
P1 C121 . 1.827(7) yes
P2 C211 . 1.821(9) yes
P2 C231 . 1.829(9) yes
P2 C221 . 1.831(9) yes
C111 C112 . 1.509(13) ?
C111 H11A . .9700 ?
C111 H11B . .9700 ?
C112 H11C . .9600 ?
C112 H11D . .9600 ?
C112 H11E . .9600 ?
C121 C122 . 1.511(15) ?
C121 H12A . .9700 ?
C121 H12B . .9700 ?
C122 H12C . .9600 ?
C122 H12D . .9600 ?
C122 H12E . .9600 ?
C131 C132 . 1.528(15) ?
C131 H13A . .9700 ?
C131 H13B . .9700 ?
C132 H13C . .9600 ?
C132 H13D . .9600 ?
C132 H13E . .9600 ?
C211 C212 . 1.531(12) ?
C211 H21A . .9700 ?
C211 H21B . .9700 ?
C212 H21C . .9600 ?
C212 H21D . .9600 ?
C212 H21E . .9600 ?
C221 C222 . 1.542(14) ?
C221 H22A . .9700 ?
C221 H22B . .9700 ?
C222 H22C . .9600 ?
C222 H22D . .9600 ?
C222 H22E . .9600 ?
C231 C232 . 1.545(17) ?
C231 H23A . .9700 ?
C231 H23B . .9700 ?
C232 H23C . .9600 ?
C232 H23D . .9600 ?
C232 H23E . .9600 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl2 Pt P1 C111 . . . . 176.7(4) yes
Cl2 Pt P1 C121 . . . . -60.5(4) yes
Cl2 Pt P1 C131 . . . . 53.8(3) yes
Cl1 Pt P2 C211 . . . . -.1(4) yes
Cl1 Pt P2 C221 . . . . 118.8(4) yes
Cl1 Pt P2 C231 . . . . -117.9(4) yes
P1 Pt P2 C211 . . . . 179.3(3) yes
P1 Pt P2 C221 . . . . -61.8(4) yes
P1 Pt P2 C231 . . . . 61.5(4) yes
P2 Pt P1 C111 . . . . -4.3(4) yes
P2 Pt P1 C121 . . . . 118.5(4) yes
P2 Pt P1 C131 . . . . -127.2(3) yes
|
1200001.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200001.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_1200001
loop_
_publ_author_name
'Gzella, Andrzej'
'Rozwadowska, Maria D.'
'Sulima, Agnieszka'
_publ_section_title
;
Two dihydro-5H-thiazolinono[2,3-a]isoquinoline S-oxides
;
_journal_issue 12
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1454
_journal_page_last 1456
_journal_paper_doi 10.1107/S0108270101016638
_journal_volume 57
_journal_year 2001
_chemical_formula_iupac 'C14 H17 N O4 S'
_chemical_formula_moiety 'C14 H17 N O4 S'
_chemical_formula_sum 'C14 H17 N O4 S'
_chemical_formula_weight 295.35
_chemical_name_systematic
;
8,9-Dimethoxy-10b-methyl-1-oxo-6,10b-dihydro-5H-
thiazolo[2,3-a]isoquinolin-3-one
;
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.9407(15)
_cell_length_b 9.1737(10)
_cell_length_c 19.015(2)
_cell_measurement_reflns_used 47
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 29.9
_cell_measurement_theta_min 15.0
_cell_volume 2780.7(5)
_computing_cell_refinement 'KM-4 Software'
_computing_data_collection 'KM-4 Software (Kuma, 1991)'
_computing_data_reduction 'KM-4 Software'
_computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material 'WINGX (Farrugia, 1999)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-7 (Sheldrick, 1997)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type 'Kuma KM-4'
_diffrn_measurement_method \w/2\q
_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 .0000
_diffrn_reflns_av_sigmaI/netI .0170
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 2643
_diffrn_reflns_theta_full 70.05
_diffrn_reflns_theta_max 70.05
_diffrn_reflns_theta_min 4.65
_diffrn_standards_decay_% 7.1
_diffrn_standards_interval_count 100
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 2.195
_exptl_absorpt_correction_T_max .645
_exptl_absorpt_correction_T_min .509
_exptl_absorpt_correction_type '\y scan'
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 1.411
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 1248
_exptl_crystal_size_max .33
_exptl_crystal_size_mid .31
_exptl_crystal_size_min .20
_refine_diff_density_max .201
_refine_diff_density_min -.226
_refine_ls_extinction_coef .00190(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL97
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 185
_refine_ls_number_reflns 2643
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all .0404
_refine_ls_R_factor_gt .0327
_refine_ls_shift/su_max .001
_refine_ls_shift/su_mean .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.9585P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt .0939
_refine_ls_wR_factor_ref .0980
_reflns_number_gt 2252
_reflns_number_total 2643
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1200001
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
S1 .25137(3) .12856(4) .44033(2) .04041(15) Uani d . 1 S
C2 .27792(12) .0366(2) .52145(9) .0490(4) Uani d . 1 C
H2A .2967 .1066 .5563 .059 Uiso calc . 1 H
H2B .2293 -.0141 .5399 .059 Uiso calc . 1 H
C3 .34702(11) -.07046(18) .50522(8) .0425(4) Uani d . 1 C
N4 .38423(9) -.03797(15) .44348(7) .0405(3) Uani d . 1 N
C5 .44589(12) -.1309(2) .40989(10) .0498(4) Uani d . 1 C
H5A .4518 -.2211 .4361 .060 Uiso calc . 1 H
H5B .4999 -.0824 .4088 .060 Uiso calc . 1 H
C6 .41712(12) -.16321(19) .33598(10) .0484(4) Uani d . 1 C
H6A .3684 -.2264 .3375 .058 Uiso calc . 1 H
H6B .4613 -.2139 .3108 .058 Uiso calc . 1 H
C6A .39521(10) -.02449(17) .29758(9) .0392(4) Uani d . 1 C
C7 .40452(11) -.01801(18) .22430(9) .0424(4) Uani d . 1 C
H7 .4229 -.1002 .2002 .051 Uiso calc . 1 H
C8 .38709(11) .10700(17) .18743(8) .0389(4) Uani d . 1 C
C9 .35971(10) .23192(17) .22336(8) .0383(4) Uani d . 1 C
C10 .35043(10) .22667(17) .29556(8) .0387(4) Uani d . 1 C
H10 .3320 .3089 .3197 .046 Uiso calc . 1 H
C10A .36851(10) .09837(17) .33281(8) .0366(4) Uani d . 1 C
C10B .36221(10) .10128(16) .41171(8) .0355(3) Uani d . 1 C
O1 .19727(8) .02683(15) .40025(7) .0543(3) Uani d . 1 O
O2 .36523(9) -.17314(15) .54328(7) .0576(4) Uani d . 1 O
O3 .39587(8) .12164(12) .11634(6) .0466(3) Uani d . 1 O
C11 .44023(15) .0080(2) .08183(10) .0596(5) Uani d . 1 C
H11A .4950 -.0018 .1024 .089 Uiso calc R 1 H
H11B .4457 .0309 .0328 .089 Uiso calc R 1 H
H11C .4100 -.0819 .0870 .089 Uiso calc R 1 H
O4 .34611(9) .35200(13) .18269(6) .0505(3) Uani d . 1 O
C12 .33515(15) .48769(19) .21733(10) .0584(5) Uani d . 1 C
H12A .2855 .4841 .2458 .088 Uiso calc R 1 H
H12B .3297 .5638 .1830 .088 Uiso calc R 1 H
H12C .3829 .5070 .2466 .088 Uiso calc R 1 H
C13 .41274(12) .2247(2) .44441(9) .0481(4) Uani d . 1 C
H13A .4057 .2232 .4945 .072 Uiso calc R 1 H
H13B .3934 .3163 .4262 .072 Uiso calc R 1 H
H13C .4710 .2124 .4331 .072 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_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
S1 .0427(2) .0409(3) .0376(2) .00452(17) .00164(16) .00195(16)
C2 .0569(10) .0526(11) .0375(8) .0017(8) .0029(8) .0041(8)
C3 .0529(9) .0384(8) .0362(8) -.0039(7) -.0076(7) .0024(7)
N4 .0484(8) .0352(7) .0379(7) .0050(6) -.0008(6) .0047(6)
C5 .0541(10) .0458(10) .0495(10) .0157(8) -.0005(8) .0081(8)
C6 .0615(11) .0364(9) .0474(10) .0130(8) .0063(8) .0048(7)
C6A .0426(8) .0335(8) .0415(8) .0037(7) .0024(7) .0050(7)
C7 .0520(9) .0347(8) .0405(8) .0054(7) .0078(7) -.0037(7)
C8 .0445(8) .0385(8) .0336(8) .0012(7) .0039(6) .0012(6)
C9 .0447(8) .0335(8) .0366(8) .0041(7) .0018(6) .0026(6)
C10 .0465(9) .0330(8) .0367(8) .0057(7) .0036(7) .0000(6)
C10A .0380(8) .0364(8) .0355(8) .0021(6) .0007(6) .0031(6)
C10B .0392(8) .0315(8) .0359(8) .0018(6) -.0016(6) .0023(6)
O1 .0487(7) .0589(8) .0554(7) -.0098(6) -.0085(6) .0051(6)
O2 .0729(9) .0512(7) .0488(7) .0016(7) -.0076(6) .0174(6)
O3 .0655(8) .0411(6) .0332(6) .0104(6) .0087(5) .0005(5)
C11 .0849(14) .0506(11) .0434(10) .0167(10) .0151(9) -.0049(9)
O4 .0808(9) .0349(6) .0360(6) .0125(6) .0041(6) .0061(5)
C12 .0902(15) .0355(9) .0495(10) .0145(10) .0054(10) .0024(8)
C13 .0559(10) .0418(10) .0465(9) -.0076(8) -.0104(8) .0025(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .3331 .5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1200002.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200002.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_1200002
_chemical_formula_sum 'Cu3 O8 P2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 72.3626
_cell_angle_beta 86.9965
_cell_angle_gamma 68.5473
_cell_length_a 4.85642
_cell_length_b 5.29074
_cell_length_c 6.18724
_cell_volume 140.7001
_pd_block_id
2002-07-08|PHASE_02|..creator_name..|..instr_name..
_pd_phase_name Cu3(PO4)2
_cod_original_formula_sum 'Cu3 P2 O8'
_cod_database_code 1200002
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_type_symbol
Cu1 1 1.0 0.0 0.0 0.0 Biso 1.0 Cu2+
Cu2 2 1.0 0.29117 0.24661 0.30896 Biso 1.0 Cu2+
P21 2 1.0 0.34286 0.35759 0.74501 Biso 1.0 P
O21 2 1.0 -0.1536 0.3443 0.3389 Biso 1.0 O-
O22 2 1.0 0.3324 0.6515 0.1695 Biso 1.0 O-
O23 2 1.0 0.2303 0.2274 0.0049 Biso 1.0 O-
O24 2 1.0 0.3786 0.1498 0.6334 Biso 1.0 O-
|
1200003.cif | #------------------------------------------------------------------------------
#$Date: 2017-07-04 18:48:19 +0300 (Tue, 04 Jul 2017) $
#$Revision: 198387 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200003.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_1200003
_chemical_formula_sum 'Cu2 O7 P2'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_cell_angle_alpha 90.0
_cell_angle_beta 109.3000
_cell_angle_gamma 90.0
_cell_length_a 6.85128
_cell_length_b 8.11775
_cell_length_c 9.15352
_cell_volume 480.4807
_pd_block_id
2002-07-08|PHASE_03|..creator_name..|..instr_name..
_pd_phase_name Cu2P2O7
_cod_depositor_comments
;
Changing the space group from 'P 1 2/c 1' to 'C 1 2/c 1' after consulting
the original publication. All related space group information was changed
accordingly.
Antanas Vaitkus,
2017-07-04
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'Cu2 P2 O7'
_cod_database_code 1200003
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z+1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_B_iso_or_equiv
_atom_site_type_symbol
Cu3 8 1.0 -0.02983 0.31894 0.51051 Biso 1.0 Cu2+
P31 8 1.0 0.19085 -0.00087 0.1965 Biso 1.0 P
O31 4 1.0 0.0 0.0466 0.25 Biso 1.0 O-
O32 8 1.0 0.3757 0.0002 0.3614 Biso 1.0 O-
O33 8 1.0 0.2208 0.1559 0.1128 Biso 1.0 O-
O34 8 1.0 0.1785 -0.1508 0.1179 Biso 1.0 O-
|
1200004.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-02 00:54:18 +0300 (Sat, 02 Sep 2017) $
#$Revision: 200088 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200004.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_1200004
loop_
_publ_author_name
'Coing-Boyat, J.'
_publ_section_title
;
Structure de la forme hautes temperatures du sulfate anhydre de
magnesium, \b-MgSO~4~
;
_journal_coden_ASTM COREAF
_journal_name_full
;
Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences
;
_journal_page_first 1962
_journal_page_last 1964
_journal_volume 255
_journal_year 1962
_chemical_formula_structural 'Mg S O4'
_chemical_formula_sum 'Mg O4 S'
_chemical_name_systematic 'Magnesium sulfate - \b'
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2c 2ab'
_symmetry_space_group_name_H-M 'P b n m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.742
_cell_length_b 8.575
_cell_length_c 6.699
_cell_volume 272.4
_refine_ls_R_factor_all 0.144
_cod_duplicate_entry 1100076
_cod_database_code 1200004
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
x,y,1/2-z
1/2-x,1/2+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_calc_flag
Mg1 Mg2+ 4 a 0. 0. 0. 1. 0 d
S1 S6+ 4 c 0.458 0.186 0.25 1. 0 d
O1 O2- 4 c 0.75 0.13 0.25 1. 0 d
O2 O2- 4 c 0.458 0.367 0.25 1. 0 d
O3 O2- 8 d 0.319 0.13 0.061 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
|
1200005.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200005.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_1200005
loop_
_publ_author_name
'Husson, E'
'Repelin, Y'
_publ_section_title
;
Structural studies of transition aluminas. Theta alumina
;
_journal_coden_ASTM EJSCE5
_journal_name_full
;
European Journal of Solid State Inorganic Chemistry
;
_journal_page_first 1223
_journal_page_last 1231
_journal_volume 33
_journal_year 1996
_chemical_formula_structural 'Al2 O3'
_chemical_formula_sum 'Al2 O3'
_chemical_name_systematic 'Aluminium oxide - $-theta'
_space_group_IT_number 12
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 12
_symmetry_space_group_name_Hall '-C 2y'
_symmetry_space_group_name_H-M 'C 1 2/m 1'
_cell_angle_alpha 90
_cell_angle_beta 103.79
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.795(5)
_cell_length_b 2.91(1)
_cell_length_c 5.621(7)
_cell_volume 187.4
_refine_ls_R_factor_all 0.06
_cod_database_code 1200005
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,z
-x,-y,-z
-x,y,-z
1/2+x,1/2+y,z
1/2+x,1/2-y,z
1/2-x,1/2-y,-z
1/2-x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
O1 O2- 4 i 0.16268 0. 0.12276 1. 0 d
O2 O2- 4 i 0.48945 0. 0.26127 1. 0 d
O3 O2- 4 i 0.82995 0. 0.43863 1. 0 d
Al1 Al3+ 4 i 0.10134 0. 0.7944 1. 0 d
Al2 Al3+ 4 i 0.35235 0. 0.68739 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
O2- -2.000
Al3+ 3.000
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 8164808 ChemSpider
|
1200006.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200006.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_1200006
loop_
_publ_author_name
'Peacor, D R'
_publ_section_title
;
Refinement of the Crystal Structure of a Pyroxene of Formula M1 M2
(Si1.5 Al.5) O6
;
_journal_coden_ASTM AMMIAY
_journal_name_full 'American Mineralogist'
_journal_page_first 31
_journal_page_last 41
_journal_volume 52
_journal_year 1967
_chemical_compound_source 'from Hessereau Hill, Oka, Quebec'
_chemical_formula_analytical
;
(Ca.975 Na.007 Mn.007 K.001) (Mg.57 Fe.222 Al.171 Ti.065) (Si1.506
Al.494) O6
;
_chemical_formula_structural '(Mg.6 Fe.2 Al.2) Ca (Si1.5 Al.5) O6'
_chemical_formula_sum 'Al0.7 Ca Fe0.2 Mg0.6 O6 Si1.5'
_chemical_name_mineral Augite
_chemical_name_systematic 'Magnesium iron calcium aluminium silicate *'
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 15
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 105.90(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.794(5)
_cell_length_b 8.906(5)
_cell_length_c 5.319(3)
_cell_volume 446.2
_exptl_crystal_density_meas 3.4
_refine_ls_R_factor_all 0.064
_cod_original_formula_sum 'Al.7 Ca Fe.2 Mg.6 O6 Si1.5'
_cod_database_code 1200006
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_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
Mg1 Mg2+ 4 e 0. 0.0932(2) 0.75 0.6 0 d
Fe1 Fe3+ 4 e 0. 0.0932(2) 0.75 0.2 0 d
Al1 Al3+ 4 e 0. 0.0932(2) 0.75 0.2 0 d
Ca1 Ca2+ 4 e 0. 0.6957(2) 0.75 1. 0 d
Si1 Si4+ 8 f 0.2129(2) 0.4072(2) 0.7728(3) 0.75 0 d
Al2 Al3+ 8 f 0.2129(2) 0.4072(2) 0.7728(3) 0.25 0 d
O1 O2- 8 f 0.3870(4) 0.4122(4) 0.8623(8) 1. 0 d
O2 O2- 8 f 0.1379(4) 0.2454(4) 0.6811(8) 1. 0 d
O3 O2- 8 f 0.1482(4) 0.4811(5) 0.0083(8) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
Fe3+ 3.000
Al3+ 3.000
Ca2+ 2.000
Si4+ 4.000
O2- -2.000
|
1200007.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200007.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_1200007
loop_
_publ_author_name
'Colville, A A'
'Geller, S'
_publ_section_title
;
Crystal structures of Ca~2~ Fe~1.43~ Al~0.57~ O~5~ and Ca~2~ Fe~1.28~
Al~0.72~ O~5~
;
_journal_coden_ASTM ACBCAR
_journal_name_full 'Acta Crystallographica B (24,1968-38,1982)'
_journal_page_first 3196
_journal_page_last 3200
_journal_paper_doi 10.1107/S0567740872007733
_journal_volume 28
_journal_year 1972
_chemical_formula_structural 'Ca2 Fe1.28 Al0.72 O5'
_chemical_formula_sum 'Al0.72 Ca2 Fe1.28 O5'
_chemical_name_systematic 'Calcium iron aluminium oxide (2/1.3/0.7/5)'
_space_group_IT_number 46
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 46
_symmetry_space_group_name_Hall 'I 2 -2b'
_symmetry_space_group_name_H-M 'I b m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.583(5)
_cell_length_b 14.58(2)
_cell_length_c 5.374(5)
_cell_volume 437.4
_refine_ls_R_factor_all 0.032
_cod_original_formula_sum 'Al.72 Ca2 Fe1.28 O5'
_cod_database_code 1200007
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
x,1/2-y,z
-x,1/2+y,z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+z
1/2+x,-y,1/2+z
1/2-x,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_calc_flag
Ca1 Ca2+ 8 c 0.0270(2) 0.1084(1) 0.4907(3) 1. 0 d
Fe1 Fe3+ 4 a 0. 0. 0. 0.83 0 d
Al1 Al3+ 4 a 0. 0. 0. 0.17 0 d
Fe2 Fe3+ 4 b 0.9291(2) 0.25 0.9520(4) 0.45 0 d
Al2 Al3+ 4 b 0.9291(2) 0.25 0.9520(4) 0.55 0 d
O1 O2- 8 c 0.2525(9) 0.9859(2) 0.2503(9) 1. 0 d
O2 O2- 8 c 0.0683(6) 0.1429(3) 0.256(9) 1. 0 d
O3 O2- 4 b 0.8653(9) 0.25 0.6133(9) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ca2+ 2.000
Fe3+ 3.000
Al3+ 3.000
O2- -2.000
|
1200008.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200008.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_1200008
loop_
_publ_author_name
'Bertaut, E F'
'Blum, P'
'Sagnieres, A'
_publ_section_title
;
Structure du Ferrite Bicalcique et de la Brownmillerite
;
_journal_coden_ASTM ACCRA9
_journal_name_full 'Acta Crystallographica (1,1948-23,1967)'
_journal_page_first 149
_journal_page_last 159
_journal_paper_doi 10.1107/S0365110X59000433
_journal_volume 12
_journal_year 1959
_chemical_formula_structural 'Fe2 O3 Al2 O3 (Ca O)4'
_chemical_formula_sum 'Al2 Ca4 Fe2 O10'
_chemical_name_systematic 'Diiron(III) dialuminium tetracalcium oxide'
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2n 2ac'
_symmetry_space_group_name_H-M 'P c m n'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.58
_cell_length_b 14.5
_cell_length_c 5.34
_cell_volume 432.1
_cod_duplicate_entry 1008124
_cod_database_code 1200008
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,1/2+z
-x,1/2+y,-z
1/2+x,-y,1/2-z
-x,-y,-z
1/2+x,1/2+y,1/2-z
x,1/2-y,z
1/2-x,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_calc_flag
Fe1 Fe3+ 4 a 0. 0. 0. 0.5 0 d
Al1 Al3+ 4 a 0. 0. 0. 0.5 0 d
Fe2 Fe3+ 4 c -0.072 0.25 -0.055 0.5 0 d
Al2 Al3+ 4 c -0.072 0.25 -0.055 0.5 0 d
Ca1 Ca2+ 8 d 0.028 0.112 0.48 1. 0 d
O1 O2- 8 d 0.25 -0.015 0.25 1. 0 d
O2 O2- 8 d 0.055 0.133 0. 1. 0 d
O3 O2- 4 c -0.137 0.25 0.607 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe3+ 3.000
Al3+ 3.000
Ca2+ 2.000
O2- -2.000
|
1200009.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200009.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_1200009
loop_
_publ_author_name
'Colville, A A'
'Geller, S'
_publ_section_title
;
The Crystal Structure of Brownmillerite, Ca2 Fe Al O5
;
_journal_coden_ASTM ACBCAR
_journal_name_full 'Acta Crystallographica B (24,1968-38,1982)'
_journal_page_first 2311
_journal_page_last 2315
_journal_paper_doi 10.1107/S056774087100579X
_journal_volume 27
_journal_year 1971
_chemical_formula_structural 'Ca2 Fe Al O5'
_chemical_formula_sum 'Al Ca2 Fe O5'
_chemical_name_mineral Brownmillerite
_chemical_name_systematic
;
Calcium iron(III) aluminium oxide (2/1.5/0.5/5)
;
_space_group_IT_number 46
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 46
_symmetry_space_group_name_Hall 'I 2 -2b'
_symmetry_space_group_name_H-M 'I b m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.584(5)
_cell_length_b 14.60(1)
_cell_length_c 5.374(5)
_cell_volume 438.1
_refine_ls_R_factor_all 0.027
_cod_database_code 1200009
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
x,1/2-y,z
-x,1/2+y,z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+z
1/2+x,-y,1/2+z
1/2-x,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_calc_flag
Ca1 Ca2+ 8 c 0.0273(2) 0.1087(1) 0.4920(3) 1. 0 d
Fe1 Fe3+ 4 a 0. 0. 0. 0.76 0 d
Fe2 Fe3+ 4 b 0.9283 0.25 0.9533 0.24 0 d
Al1 Al3+ 4 a 0. 0. 0. 0.24 0 d
Al2 Al3+ 4 b 0.9283 0.25 0.9533 0.76 0 d
O1 O2- 8 c 0.2523(10) 0.9861(2) 0.2491(10) 1. 0 d
O2 O2- 8 c 0.0680(7) 0.1493(3) 0.0246(9) 1. 0 d
O3 O2- 4 b 0.8607(10) 0.25 0.6193(11) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ca2+ 2.000
Fe3+ 3.000
Al3+ 3.000
O2- -2.000
|
1200010.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200010.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_1200010
loop_
_publ_author_name
'Bertaut, F'
'Blum, P'
'Sagnieres, A'
_publ_section_title
;
La structure du ferrite dicalcique et de la Brownmillerite.
;
_journal_coden_ASTM ACCRA9
_journal_name_full 'Acta Crystallographica (1,1948-23,1967)'
_journal_page_first 149
_journal_page_last 159
_journal_paper_doi 10.1107/S0365110X59000433
_journal_volume 12
_journal_year 1959
_chemical_formula_structural 'Fe Al O3 (Ca O)2'
_chemical_formula_sum 'Al Ca2 Fe O5'
_chemical_name_mineral Brownmillerite
_chemical_name_systematic
;
Iron(III) aluminium oxide bis(calcium oxide) *
;
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2n 2ac'
_symmetry_space_group_name_H-M 'P c m n'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.58
_cell_length_b 14.5
_cell_length_c 5.34
_cell_volume 432.1
_cod_duplicate_entry 1008724
_cod_database_code 1200010
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,1/2+z
-x,1/2+y,-z
1/2+x,-y,1/2-z
-x,-y,-z
1/2+x,1/2+y,1/2-z
x,1/2-y,z
1/2-x,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_calc_flag
Fe1 Fe3+ 4 a 0. 0. 0. 0.5 0 d
Al1 Al3+ 4 a 0. 0. 0. 0.5 0 d
Fe2 Fe3+ 4 c -0.072 0.25 -0.055 0.5 0 d
Al2 Al3+ 4 c -0.072 0.25 -0.055 0.5 0 d
Ca1 Ca2+ 8 d 0.028 0.112 0.48 1. 0 d
O1 O2- 8 d 0.25 -0.015 0.25 1. 0 d
O2 O2- 8 d 0.055 0.133 0. 1. 0 d
O3 O2- 4 c -0.137 0.25 0.607 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe3+ 3.000
Al3+ 3.000
Ca2+ 2.000
O2- -2.000
|
1200011.cif | #------------------------------------------------------------------------------
#$Date: 2017-09-03 03:17:11 +0300 (Sun, 03 Sep 2017) $
#$Revision: 200139 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200011.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_1200011
loop_
_publ_author_name
'Robinson, Mark T.'
_publ_section_title
;
The crystal structures of \b-K~2~SO~4~ and of \b-K~2~PO~3~F
;
_journal_coden_ASTM JPCHAX
_journal_issue 8
_journal_name_full 'Journal of Physical Chemistry'
_journal_page_first 925
_journal_page_last 928
_journal_paper_doi 10.1021/j150566a007
_journal_volume 62
_journal_year 1958
_chemical_formula_structural 'K2 S O4'
_chemical_formula_sum 'K2 O4 S'
_chemical_name_systematic 'Potassium sulfate - $-beta'
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2c 2n'
_symmetry_space_group_name_H-M 'P n a m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.456(6)
_cell_length_b 10.08(1)
_cell_length_c 5.776(5)
_cell_volume 434.1
_exptl_crystal_density_meas 2.62(0)
_refine_ls_R_factor_all 0.095
_cod_database_code 1200011
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,1/2-z
-x,-y,1/2+z
1/2-x,1/2+y,-z
-x,-y,-z
1/2-x,1/2+y,1/2+z
x,y,1/2-z
1/2+x,1/2-y,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
K1 K1+ 4 c 0.1768(25) 0.0818(128) 0.25 1. 0 d
K2 K1+ 4 c -0.0115(19) 0.7046(15) 0.25 1. 0 d
S1 S6+ 4 c 0.2358(36) 0.4155(161) 0.25 1. 0 d
O1 O2- 4 c 0.0315(74) 0.4032(87) 0.25 1. 0 d
O2 O2- 4 c 0.2970(89) 0.5579(44) 0.25 1. 0 d
O3 O2- 8 d 0.2997(46) 0.3484(28) 0.0410(41) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
K1+ 1.000
S6+ 6.000
O2- -2.000
|
1200012.cif | #------------------------------------------------------------------------------
#$Date: 2018-08-13 06:59:52 +0300 (Mon, 13 Aug 2018) $
#$Revision: 209648 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200012.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_1200012
loop_
_publ_author_name
'Ojima, K.'
'Nishihata, Y.'
'Sawada, A.'
_publ_section_title
;
Structure of potassium sulfate at temperatures from 296 K down to 15 K
;
_journal_coden_ASTM ASBSDK
_journal_issue 3
_journal_name_full
;
Acta Crystallographica, Section B: Structural Science
;
_journal_page_first 287
_journal_page_last 293
_journal_paper_doi 10.1107/S0108768194013327
_journal_volume 51
_journal_year 1995
_chemical_formula_moiety '(K 1+)2, O4 S 2- '
_chemical_formula_structural 'K2 (S O4)'
_chemical_formula_sum 'K2 O4 S'
_chemical_formula_weight 158
_chemical_name_systematic 'Dipotassium sulfate'
_space_group_crystal_system orthorhombic
_space_group_IT_number 62
_space_group_name_Hall '-P 2n 2a'
_space_group_name_H-M_alt 'P m c n'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.7704(3)
_cell_length_b 10.0712(9)
_cell_length_c 7.4776(4)
_cell_measurement_temperature 296
_cell_volume 434.6
_diffrn_ambient_temperature 296
_diffrn_radiation_type Mo
_diffrn_radiation_wavelength 0.70926
_exptl_absorpt_coefficient_mu 2.49
_exptl_crystal_density_diffrn 2.66
_refine_ls_number_parameters 41
_refine_ls_number_reflns 1429
_refine_ls_R_factor_all 0.036
_cod_duplicate_entry 2101318
_cod_depositor_comments
;
Adding the moiety chemical formula and updating the systematic chemical name.
Antanas Vaitkus,
2018-08-13
Updating space group information.
Antanas Vaitkus,
2018-08-13
;
_cod_database_code 1200012
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,-y+1/2,z+1/2
3 x+1/2,-y,-z
4 -x,y+1/2,-z+1/2
5 -x,-y,-z
6 x+1/2,y+1/2,-z+1/2
7 -x+1/2,y,z
8 x,-y+1/2,z+1/2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
K1 0.0169(2) 0.0197(2) 0.0164(2) 0 0 0.0006(2)
K2 0.0185(2) 0.0150(1) 0.0132(1) 0 0 -0.0005(1)
S1 0.0101(1) 0.0095(1) 0.0101(1) 0 0 -0.0005(1)
O1 0.0382(11) 0.0318(10) 0.0089(5) 0 0 -0.0019(7)
O2 0.0254(8) 0.0120(6) 0.0210(7) 0 0 -0.0044(5)
O3 0.0140(4) 0.0227(5) 0.0298(6) -0.0063(4) 0.0032(5) 0.0052(5)
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_calc_flag
K1 K1+ 4 c 0.25 0.08935(6) 0.17398(7) 1 d
K2 K1+ 4 c 0.25 0.79550(5) 0.48915(7) 1 d
S1 S6+ 4 c 0.25 0.41985(5) 0.23295(7) 1 d
O1 O2- 4 c 0.25 0.4162(3) 0.0368(3) 1 d
O2 O2- 4 c 0.25 0.5585(2) 0.2976(3) 1 d
O3 O2- 8 d 0.0412(3) 0.3522(2) 0.3017(2) 1 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
K1+ 1
S6+ 6
O2- -2
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0018288
|
1200013.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-27 16:31:08 +0200 (Tue, 27 Dec 2016) $
#$Revision: 189448 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200013.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_1200013
loop_
_publ_author_name
'Nimmo, J. K.'
'Lucas, B. W.'
_publ_section_title
;
The crystal structures of \g- and \b-KNO~3~ and the
\a \\leftarrow \g \\leftarrow \b phase transformations
;
_journal_coden_ASTM ACBCAR
_journal_issue 7
_journal_name_full 'Acta Crystallographica B (24,1968-38,1982)'
_journal_page_first 1968
_journal_page_last 1971
_journal_paper_doi 10.1107/S0567740876006894
_journal_volume 32
_journal_year 1976
_chemical_formula_structural 'K N O3'
_chemical_formula_sum 'K N O3'
_chemical_name_systematic 'Potasium nitrate - \b'
_space_group_IT_number 166
_symmetry_cell_setting trigonal
_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 5.425(1)
_cell_length_b 5.425(1)
_cell_length_c 9.836(4)
_cell_volume 250.7
_refine_ls_R_factor_all 0.13
_cod_original_sg_symbol_H-M 'R -3 m H'
_cod_database_code 1200013
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z
y-x,-x,z
-y,-x,z
x,x-y,z
y-x,y,z
-x,-y,-z
y,y-x,-z
x-y,x,-z
y,x,-z
-x,y-x,-z
x-y,-y,-z
1/3+x,2/3+y,2/3+z
2/3+x,1/3+y,1/3+z
1/3-y,2/3+x-y,2/3+z
2/3-y,1/3+x-y,1/3+z
1/3-x+y,2/3-x,2/3+z
2/3-x+y,1/3-x,1/3+z
1/3-y,2/3-x,2/3+z
2/3-y,1/3-x,1/3+z
1/3+x,2/3+x-y,2/3+z
2/3+x,1/3+x-y,1/3+z
1/3-x+y,2/3+y,2/3+z
2/3-x+y,1/3+y,1/3+z
1/3-x,2/3-y,2/3-z
2/3-x,1/3-y,1/3-z
1/3+y,2/3-x+y,2/3-z
2/3+y,1/3-x+y,1/3-z
1/3+x-y,2/3+x,2/3-z
2/3+x-y,1/3+x,1/3-z
1/3+y,2/3+x,2/3-z
2/3+y,1/3+x,1/3-z
1/3-x,2/3-x+y,2/3-z
2/3-x,1/3-x+y,1/3-z
1/3+x-y,2/3-y,2/3-z
2/3+x-y,1/3-y,1/3-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
K1 K1+ 3 a 0. 0. 0. 1. 0 d
N1 N5+ 3 b 0. 0. 0.5 1. 0 d
O1 O2- 18 h 0.130(2) -0.130(2) 0.475(5) 0.5 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
K1+ 1.000
N5+ 5.000
O2- -2.000
|
1200014.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-06 23:14:55 +0300 (Fri, 06 Jul 2018) $
#$Revision: 208883 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200014.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_1200014
loop_
_publ_author_name
'Beran, A.'
'Zemann, J.'
_publ_section_title
;
Refinement and comparison of the crystal structures of a dolomite and of
an Fe-rich ankerite
;
_journal_coden_ASTM TTMMDZ
_journal_issue 4
_journal_name_full
;
TMPM, Tschermaks Mineralogische und Petrographische Mitteilungen
;
_journal_page_first 279
_journal_page_last 286
_journal_paper_doi 10.1007/BF01081130
_journal_volume 24
_journal_year 1977
_chemical_compound_source 'from Oberdorf, Styria, Austria'
_chemical_formula_analytical 'Ca (Mg0.94 Fe0.05 Mn0.01) (C O3)2'
_chemical_formula_structural 'Ca Mg (C O3)2'
_chemical_formula_sum 'C2 Ca Mg O6'
_chemical_name_mineral Dolomite
_chemical_name_systematic 'Calcium magnesium carbonate'
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_Hall '-R 3'
_space_group_name_H-M_alt 'R -3 :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 4.812(1)
_cell_length_b 4.812(1)
_cell_length_c 16.020(3)
_cell_volume 321.3
_refine_ls_R_factor_all 0.029
_cod_depositor_comments
;
Merging entries 1200014, 5000116 and 9009592. Marking entries 5000116 and
9009592 as duplicates of entry 1200014. Marking entries 1200014, 5000116 and
9009592 as being related to AMCSD entry 0015666.
Antanas Vaitkus,
2018-07-06
;
_cod_original_sg_symbol_H-M 'R -3 H'
_cod_original_formula_sum 'Ca Mg O6'
_cod_database_code 1200014
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 y-x,-x,z
4 -x,-y,-z
5 y,y-x,-z
6 x-y,x,-z
7 1/3+x,2/3+y,2/3+z
8 2/3+x,1/3+y,1/3+z
9 1/3-y,2/3+x-y,2/3+z
10 2/3-y,1/3+x-y,1/3+z
11 1/3-x+y,2/3-x,2/3+z
12 2/3-x+y,1/3-x,1/3+z
13 1/3-x,2/3-y,2/3-z
14 2/3-x,1/3-y,1/3-z
15 1/3+y,2/3-x+y,2/3-z
16 2/3+y,1/3-x+y,1/3-z
17 1/3+x-y,2/3+x,2/3-z
18 2/3+x-y,1/3+x,1/3-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ca 0.00772 0.00772 0.00559 0.00386 0.00000 0.00000
Mg 0.00399 0.00399 0.00260 0.00199 0.00000 0.00000
C 0.00584 0.00584 0.00559 0.00292 0.00000 0.00000
O 0.00797 0.01141 0.01170 0.00635 -0.00220 -0.00298
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_calc_flag
Ca Ca2+ 3 a 0 0 0 1 d
Mg Mg2+ 3 b 0 0 0.5 1 d
C C4+ 6 c 0 0 0.2429(1) 1 d
O O2- 18 f 0.2485(2) -0.0343(2) 0.2439(1) 1 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ca2+ 2
Mg2+ 2
C4+ 4
O2- -2
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0015666
|
1200015.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200015.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_1200015
loop_
_publ_author_name
'Shirasuka, K.'
'Yanagida, H.'
'Yamaguchi, G.'
_publ_section_title
;
The Preparation of \h Alumina and its Structure
;
_journal_coden_ASTM YGKSA4
_journal_issue 976
_journal_name_full 'Journal of the Ceramic Association, Japan'
_journal_page_first 610
_journal_page_last 613
_journal_paper_doi 10.2109/jcersj1950.84.976_610
_journal_volume 84
_journal_year 1976
_chemical_formula_structural 'Al2.66 O4'
_chemical_formula_sum 'Al2.66 O4'
_chemical_name_systematic 'Aluminium oxide - \h'
_space_group_IT_number 227
_symmetry_cell_setting cubic
_symmetry_space_group_name_Hall 'F 4d 2 3 -1d'
_symmetry_space_group_name_H-M 'F d -3 m :1'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 7.906
_cell_length_b 7.906
_cell_length_c 7.906
_cell_volume 494.2
_exptl_crystal_density_meas 3.66
_refine_ls_R_factor_all 0.06
_cod_original_sg_symbol_H-M 'F d -3 m S'
_cod_database_code 1200015
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
y,z,x
z,x,y
x,z,y
y,x,z
z,y,x
x,-y,-z
y,-z,-x
z,-x,-y
x,-z,-y
y,-x,-z
z,-y,-x
-x,y,-z
-y,z,-x
-z,x,-y
-x,z,-y
-y,x,-z
-z,y,-x
-x,-y,z
-y,-z,x
-z,-x,y
-x,-z,y
-y,-x,z
-z,-y,x
1/4-x,1/4-y,1/4-z
1/4-y,1/4-z,1/4-x
1/4-z,1/4-x,1/4-y
1/4-x,1/4-z,1/4-y
1/4-y,1/4-x,1/4-z
1/4-z,1/4-y,1/4-x
1/4-x,1/4+y,1/4+z
1/4-y,1/4+z,1/4+x
1/4-z,1/4+x,1/4+y
1/4-x,1/4+z,1/4+y
1/4-y,1/4+x,1/4+z
1/4-z,1/4+y,1/4+x
1/4+x,1/4-y,1/4+z
1/4+y,1/4-z,1/4+x
1/4+z,1/4-x,1/4+y
1/4+x,1/4-z,1/4+y
1/4+y,1/4-x,1/4+z
1/4+z,1/4-y,1/4+x
1/4+x,1/4+y,1/4-z
1/4+y,1/4+z,1/4-x
1/4+z,1/4+x,1/4-y
1/4+x,1/4+z,1/4-y
1/4+y,1/4+x,1/4-z
1/4+z,1/4+y,1/4-x
x,1/2+y,1/2+z
1/2+x,y,1/2+z
1/2+x,1/2+y,z
y,1/2+z,1/2+x
1/2+y,z,1/2+x
1/2+y,1/2+z,x
z,1/2+x,1/2+y
1/2+z,x,1/2+y
1/2+z,1/2+x,y
x,1/2+z,1/2+y
1/2+x,z,1/2+y
1/2+x,1/2+z,y
y,1/2+x,1/2+z
1/2+y,x,1/2+z
1/2+y,1/2+x,z
z,1/2+y,1/2+x
1/2+z,y,1/2+x
1/2+z,1/2+y,x
x,1/2-y,1/2-z
1/2+x,-y,1/2-z
1/2+x,1/2-y,-z
y,1/2-z,1/2-x
1/2+y,-z,1/2-x
1/2+y,1/2-z,-x
z,1/2-x,1/2-y
1/2+z,-x,1/2-y
1/2+z,1/2-x,-y
x,1/2-z,1/2-y
1/2+x,-z,1/2-y
1/2+x,1/2-z,-y
y,1/2-x,1/2-z
1/2+y,-x,1/2-z
1/2+y,1/2-x,-z
z,1/2-y,1/2-x
1/2+z,-y,1/2-x
1/2+z,1/2-y,-x
-x,1/2+y,1/2-z
1/2-x,y,1/2-z
1/2-x,1/2+y,-z
-y,1/2+z,1/2-x
1/2-y,z,1/2-x
1/2-y,1/2+z,-x
-z,1/2+x,1/2-y
1/2-z,x,1/2-y
1/2-z,1/2+x,-y
-x,1/2+z,1/2-y
1/2-x,z,1/2-y
1/2-x,1/2+z,-y
-y,1/2+x,1/2-z
1/2-y,x,1/2-z
1/2-y,1/2+x,-z
-z,1/2+y,1/2-x
1/2-z,y,1/2-x
1/2-z,1/2+y,-x
-x,1/2-y,1/2+z
1/2-x,-y,1/2+z
1/2-x,1/2-y,z
-y,1/2-z,1/2+x
1/2-y,-z,1/2+x
1/2-y,1/2-z,x
-z,1/2-x,1/2+y
1/2-z,-x,1/2+y
1/2-z,1/2-x,y
-x,1/2-z,1/2+y
1/2-x,-z,1/2+y
1/2-x,1/2-z,y
-y,1/2-x,1/2+z
1/2-y,-x,1/2+z
1/2-y,1/2-x,z
-z,1/2-y,1/2+x
1/2-z,-y,1/2+x
1/2-z,1/2-y,x
1/4-x,3/4-y,3/4-z
3/4-x,1/4-y,3/4-z
3/4-x,3/4-y,1/4-z
1/4-y,3/4-z,3/4-x
3/4-y,1/4-z,3/4-x
3/4-y,3/4-z,1/4-x
1/4-z,3/4-x,3/4-y
3/4-z,1/4-x,3/4-y
3/4-z,3/4-x,1/4-y
1/4-x,3/4-z,3/4-y
3/4-x,1/4-z,3/4-y
3/4-x,3/4-z,1/4-y
1/4-y,3/4-x,3/4-z
3/4-y,1/4-x,3/4-z
3/4-y,3/4-x,1/4-z
1/4-z,3/4-y,3/4-x
3/4-z,1/4-y,3/4-x
3/4-z,3/4-y,1/4-x
1/4-x,3/4+y,3/4+z
3/4-x,1/4+y,3/4+z
3/4-x,3/4+y,1/4+z
1/4-y,3/4+z,3/4+x
3/4-y,1/4+z,3/4+x
3/4-y,3/4+z,1/4+x
1/4-z,3/4+x,3/4+y
3/4-z,1/4+x,3/4+y
3/4-z,3/4+x,1/4+y
1/4-x,3/4+z,3/4+y
3/4-x,1/4+z,3/4+y
3/4-x,3/4+z,1/4+y
1/4-y,3/4+x,3/4+z
3/4-y,1/4+x,3/4+z
3/4-y,3/4+x,1/4+z
1/4-z,3/4+y,3/4+x
3/4-z,1/4+y,3/4+x
3/4-z,3/4+y,1/4+x
1/4+x,3/4-y,3/4+z
3/4+x,1/4-y,3/4+z
3/4+x,3/4-y,1/4+z
1/4+y,3/4-z,3/4+x
3/4+y,1/4-z,3/4+x
3/4+y,3/4-z,1/4+x
1/4+z,3/4-x,3/4+y
3/4+z,1/4-x,3/4+y
3/4+z,3/4-x,1/4+y
1/4+x,3/4-z,3/4+y
3/4+x,1/4-z,3/4+y
3/4+x,3/4-z,1/4+y
1/4+y,3/4-x,3/4+z
3/4+y,1/4-x,3/4+z
3/4+y,3/4-x,1/4+z
1/4+z,3/4-y,3/4+x
3/4+z,1/4-y,3/4+x
3/4+z,3/4-y,1/4+x
1/4+x,3/4+y,3/4-z
3/4+x,1/4+y,3/4-z
3/4+x,3/4+y,1/4-z
1/4+y,3/4+z,3/4-x
3/4+y,1/4+z,3/4-x
3/4+y,3/4+z,1/4-x
1/4+z,3/4+x,3/4-y
3/4+z,1/4+x,3/4-y
3/4+z,3/4+x,1/4-y
1/4+x,3/4+z,3/4-y
3/4+x,1/4+z,3/4-y
3/4+x,3/4+z,1/4-y
1/4+y,3/4+x,3/4-z
3/4+y,1/4+x,3/4-z
3/4+y,3/4+x,1/4-z
1/4+z,3/4+y,3/4-x
3/4+z,1/4+y,3/4-x
3/4+z,3/4+y,1/4-x
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
O1 O2- 32 e 0.37 0.37 0.37 1. 0 d
Al1 Al3+ 8 a 0.25 0.25 0.25 0.503 0 d
Al2 Al3+ 48 f 0.25 0. 0. 0.083 0 d
Al3 Al3+ 16 d 0.625 0.625 0.625 0.564 0 d
Al4 Al3+ 16 c 0.125 0.125 0.125 0.27 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
O2- -2.000
Al3+ 3.000
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 8164808 ChemSpider
|
1200016.cif | #------------------------------------------------------------------------------
#$Date: 2023-03-26 11:09:57 +0300 (Sun, 26 Mar 2023) $
#$Revision: 282068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200016.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_1200016
loop_
_publ_author_name
'Saalfeld, H'
'Wedde, M'
_publ_section_title
;
Refinement of the crystal structure of gibbsite, Al (O H)3
;
_journal_coden_ASTM ZEKGAX
_journal_name_full
;
Zeitschrift fuer Kristallographie, Kristallgeometrie, Kristallphysik,
Kristallchemie (-144,1977)
;
_journal_page_first 129
_journal_page_last 135
_journal_volume 139
_journal_year 1974
_chemical_compound_source 'Langesundfjord, Norway'
_chemical_formula_structural 'Al (O H)3'
_chemical_formula_sum 'Al H3 O3'
_chemical_name_mineral Gibbsite
_chemical_name_systematic 'Aluminium hydroxide'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 94.54(1)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 8.684(1)
_cell_length_b 5.078(1)
_cell_length_c 9.736(2)
_cell_volume 428.0
_database_code_amcsd 0010761
_exptl_crystal_density_diffrn 2.421
_exptl_crystal_density_meas 2.4
_refine_ls_R_factor_all 0.032
_cod_original_formula_sum 'H3 Al O3'
_cod_database_code 1200016
loop_
_space_group_symop_operation_xyz
x,y,z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_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
Al1 Al3+ 4 e 0.1679(1) 0.5295(2) -0.0023(1) 1. 0 d
Al2 Al3+ 4 e 0.3344(1) 0.0236(2) -0.0024(1) 1. 0 d
O1 O2- 4 e 0.1779(2) 0.2183(4) -0.1115(2) 1. 0 d
O2 O2- 4 e 0.6692(2) 0.6558(4) -0.1023(2) 1. 0 d
O3 O2- 4 e 0.4984(2) 0.1315(4) -0.1044(2) 1. 0 d
O4 O2- 4 e -0.0205(2) 0.6293(4) -0.1068(2) 1. 0 d
O5 O2- 4 e 0.2971(2) 0.7178(4) -0.1052(2) 1. 0 d
O6 O2- 4 e 0.8194(2) 0.1491(4) -0.1015(2) 1. 0 d
H1 H1+ 4 e 0.101(6) 0.152(10) -0.124(5) 1. 0 d
H2 H1+ 4 e 0.595(6) 0.573(10) -0.098(5) 1. 0 d
H3 H1+ 4 e 0.503(5) 0.137(10) -0.190(5) 1. 0 d
H4 H1+ 4 e -0.029(5) 0.801(10) -0.107(4) 1. 0 d
H5 H1+ 4 e 0.293(6) 0.724(11) -0.196(6) 1. 0 d
H6 H1+ 4 e 0.815(5) 0.160(9) -0.190(5) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Al3+ 3.000
O2- -2.000
H1+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0010761
|
1200017.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-15 03:23:08 +0300 (Sun, 15 Oct 2017) $
#$Revision: 202022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200017.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_1200017
loop_
_publ_author_name
'Hassel, O'
_publ_section_title
;
Ueber die Kristallstruktur des Graphits
;
_journal_coden_ASTM ZEPYAA
_journal_name_full
;
Zeitschrift fuer Physik
;
_journal_page_first 317
_journal_page_last 337
_journal_paper_doi 10.1007/BF01327534
_journal_volume 25
_journal_year 1924
_chemical_compound_source 'from Kropfm}hl, Bavaria'
_chemical_formula_structural C
_chemical_formula_sum C
_chemical_name_mineral 'Graphite 2H'
_chemical_name_systematic Carbon
_space_group_IT_number 186
_symmetry_cell_setting hexagonal
_symmetry_Int_Tables_number 186
_symmetry_space_group_name_Hall 'P 6c -2c'
_symmetry_space_group_name_H-M 'P 63 m c'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 4
_cell_length_a 2.47
_cell_length_b 2.47
_cell_length_c 6.79
_cell_volume 35.9
_exptl_crystal_density_meas 2.16
_cod_database_code 1200017
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
-x,-y,1/2+z
y,y-x,1/2+z
x-y,x,1/2+z
y,x,1/2+z
x-y,-y,1/2+z
-x,y-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
C1 C0 2 a 0. 0. 0. 1. 0 d
C2 C0 2 b 0.3333 0.6667 0.005(5) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
C0 0.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 MPOD 1000021
2 MPOD 1000022
|
1200018.cif | #------------------------------------------------------------------------------
#$Date: 2023-03-26 11:09:57 +0300 (Sun, 26 Mar 2023) $
#$Revision: 282068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200018.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_1200018
loop_
_publ_author_name
'Lipson, H.'
'Stokes, A. R.'
_publ_section_title
;
The Structure of Graphite
;
_journal_coden_ASTM PRLAAZ
_journal_issue 984
_journal_name_full
;
Proceedings of the Royal Society A: Mathematical, Physical
and Engineering Sciences
;
_journal_page_first 101
_journal_page_last 105
_journal_paper_doi 10.1098/rspa.1942.0063
_journal_volume 181
_journal_year 1942
_chemical_compound_source 'Ceylon, Bavaria'
_chemical_formula_structural C
_chemical_formula_sum C
_chemical_name_mineral 'Graphite 3R'
_chemical_name_systematic Carbon
_space_group_IT_number 166
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall '-P 3* 2'
_symmetry_space_group_name_H-M 'R -3 m :R'
_audit_creation_date 100-06-21
_audit_creation_method 'generated by RETRIEVE 2.0'
_cell_angle_alpha 39.49
_cell_angle_beta 39.49
_cell_angle_gamma 39.49
_cell_formula_units_Z 2
_cell_length_a 3.635
_cell_length_b 3.635
_cell_length_c 3.635
_cell_volume 17.5
_database_code_amcsd 0015334
_exptl_crystal_density_diffrn 2.281
_cod_original_sg_symbol_H-M 'R -3 m R'
_cod_database_code 1200018
loop_
_space_group_symop_operation_xyz
x,y,z
y,x,z
y,z,x
x,z,y
z,x,y
z,y,x
-x,-y,-z
-y,-x,-z
-y,-z,-x
-x,-z,-y
-z,-x,-y
-z,-y,-x
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
C1 C0 2 c 0.164 0.164 0.164 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
C0 0.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0015334
|
1200019.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200019.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_1200019
loop_
_publ_author_name
'Yeh, C'
'Lu, Z W'
'Froyen, S'
'Zunger, A'
_publ_section_title
;
Zinc-blende-Wurtzite polytypism in semiconductors
;
_journal_coden_ASTM PRBMDO
_journal_issue 16
_journal_name_full
;
Physical Review, Serie 3. B - Condensed Matter (18,1978-)
;
_journal_page_first 10086
_journal_page_last 10097
_journal_paper_doi 10.1103/PhysRevB.46.10086
_journal_volume 46
_journal_year 1992
_chemical_formula_structural C
_chemical_formula_sum C
_chemical_name_mineral Lonsdaleite
_chemical_name_systematic Carbon
_space_group_IT_number 186
_symmetry_cell_setting hexagonal
_symmetry_Int_Tables_number 186
_symmetry_space_group_name_Hall 'P 6c -2c'
_symmetry_space_group_name_H-M 'P 63 m c'
_audit_creation_date 100-06-21
_audit_creation_method 'generated by RETRIEVE 2.0'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 4
_cell_length_a 2.49
_cell_length_b 2.49
_cell_length_c 4.144
_cell_volume 22.3
_exptl_crystal_density_meas 3.5
_cod_database_code 1200019
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
-x,-y,1/2+z
y,y-x,1/2+z
x-y,x,1/2+z
y,x,1/2+z
x-y,-y,1/2+z
-x,y-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
C1 C0 2 b 0.3333 0.6667 0. 1. 0 d
C2 C0 2 b 0.3333 0.6667 0.374 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
C0 0.000
|
1200020.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/20/00/1200020.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_1200020
loop_
_publ_author_name
'Thomas K. Reynolds'
'Joshua G. Bales'
'Francis J. DiSalvo'
_publ_section_title
;
Synthesis and Properties of a New Metal-Rich Nickel Antimonide
Telluride or Selenide: Ni7-SbX2 ( \d ≈ 1.3; X = Se or Te)
;
_journal_issue 11
_journal_name_full 'Chemistry of Materials'
_journal_page_first 4746
_journal_page_last 4751
_journal_paper_doi 10.1021/cm020585r
_journal_volume 14
_journal_year 2002
_chemical_formula_sum 'Ni5.72 Sb Se2'
_chemical_formula_weight 615.49
_chemical_name_common 'Nickel Antimonide Selenide'
_chemical_name_systematic
;
?
;
_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'
_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 2
_cell_length_a 3.7021(5)
_cell_length_b 3.7021(5)
_cell_length_c 18.593(4)
_cell_measurement_temperature 293(2)
_cell_volume 254.83(7)
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction SHELXTL
_computing_molecular_graphics SHELXTL
_computing_publication_material 'WingX (Farrugia, 1999)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_method 'omega and phi 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 0.1701
_diffrn_reflns_av_sigmaI/netI 0.0779
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 1433
_diffrn_reflns_theta_full 29.12
_diffrn_reflns_theta_max 29.12
_diffrn_reflns_theta_min 4.38
_diffrn_standards_decay_% 0
_exptl_absorpt_coefficient_mu 40.012
_exptl_absorpt_correction_type empirical
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 8.021
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 558
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.02
_refine_diff_density_max 1.995
_refine_diff_density_min -2.568
_refine_diff_density_rms 0.491
_refine_ls_extinction_coef 0.010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.279
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 17
_refine_ls_number_reflns 132
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.279
_refine_ls_R_factor_all 0.0534
_refine_ls_R_factor_gt 0.0534
_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^)+(0.0132P)^2^+15.7927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1199
_refine_ls_wR_factor_ref 0.1199
_reflns_number_gt 132
_reflns_number_total 132
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'I 4/mmm'
_cod_database_code 1200020
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+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, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-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'
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
Se1 Se 0.0000 0.0000 0.18100(15) 0.0159(8) Uani 1 8 d S
Sb1 Sb 0.0000 0.0000 0.5000 0.0150(8) Uani 1 16 d S
Ni1 Ni 0.0000 0.0000 0.0000 0.0158(10) Uani 1 16 d S
Ni2 Ni 0.0000 0.5000 0.10009(14) 0.0163(8) Uani 1 4 d S
Ni3 Ni 0.0000 0.0000 0.3020(6) 0.022(3) Uani 0.359(17) 8 d SP
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Se1 0.0108(9) 0.0108(9) 0.0261(15) 0.000 0.000 0.000
Sb1 0.0085(8) 0.0085(8) 0.0280(15) 0.000 0.000 0.000
Ni1 0.0109(13) 0.0109(13) 0.026(2) 0.000 0.000 0.000
Ni2 0.0125(12) 0.0097(11) 0.0266(15) 0.000 0.000 0.000
Ni3 0.021(4) 0.021(4) 0.024(6) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1200021.cif | #------------------------------------------------------------------------------
#$Date: 2022-04-22 19:48:29 +0300 (Fri, 22 Apr 2022) $
#$Revision: 274643 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/20/00/1200021.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_1200021
loop_
_publ_author_name
'Fujii, Isao'
'Hirayama, Noriaki'
_publ_section_title
;
Structure of Capillarisin
;
_journal_coden_ASTM XSAOAF
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first X63
_journal_page_last X64
_journal_paper_doi 10.2116/analscix.19.x63
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C16 H12 O7 '
_chemical_formula_sum 'C16 H12 O7'
_chemical_formula_weight 316.27
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yab'
_symmetry_space_group_name_H-M 'P 1 21/a 1'
_cell_angle_alpha 90
_cell_angle_beta 101.318(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.4556(4)
_cell_length_b 11.4100(7)
_cell_length_c 9.8681(7)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 297
_cell_measurement_theta_max 35.0
_cell_measurement_theta_min 30.0
_cell_volume 1375.2(1)
_diffrn_measured_fraction_theta_full 0.5175
_diffrn_measured_fraction_theta_max 0.5175
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_R_equivalents 0.030
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 3113
_diffrn_reflns_theta_full 74.76
_diffrn_reflns_theta_max 74.76
_exptl_absorpt_coefficient_mu 1.043
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.950
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.527
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description bipyramid
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.300
_refine_diff_density_max 0.23
_refine_diff_density_min -0.20
_refine_ls_extinction_coef 0.15(2)
_refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref 1.210
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 257
_refine_ls_number_reflns 2836
_refine_ls_R_factor_gt 0.0400
_refine_ls_shift/su_max 0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.10600(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1480
_reflns_number_gt 2427
_reflns_number_total 944
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file 1100680_b.cif
_cod_original_formula_sum 'C16 H12 O7 '
_cod_database_code 1200021
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,-z
-x,-y,-z
1/2+x,1/2-y,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
O(1) O 0.47247(8) 0.18961(8) 0.62838(9) 0.0449(2) Uani 1.00 d
O(1') O 0.34265(9) 0.23529(10) 0.7325(1) 0.0571(3) Uani 1.00 d
O(4) O 0.55351(9) -0.11093(9) 0.8475(1) 0.0550(3) Uani 1.00 d
O(4') O 0.0347(1) 0.1927(1) 1.0614(1) 0.0675(4) Uani 1.00 d
O(5) O 0.71310(9) -0.14218(8) 0.7200(1) 0.0501(3) Uani 1.00 d
O(6) O 0.83142(9) -0.05845(9) 0.5367(1) 0.0531(3) Uani 1.00 d
O(7) O 0.7707(1) 0.14115(9) 0.3976(1) 0.0592(3) Uani 1.00 d
C(1a) C 0.56050(10) 0.1243(1) 0.6055(1) 0.0387(3) Uani 1.00 d
C(1') C 0.2691(1) 0.2184(1) 0.8225(1) 0.0483(3) Uani 1.00 d
C(2) C 0.4195(1) 0.1552(1) 0.7272(1) 0.0424(3) Uani 1.00 d
C(2') C 0.2647(1) 0.3049(1) 0.9181(2) 0.0523(4) Uani 1.00 d
C(3) C 0.4429(1) 0.0575(1) 0.8050(1) 0.0441(3) Uani 1.00 d
C(3') C 0.1865(1) 0.2976(1) 1.0002(2) 0.0545(4) Uani 1.00 d
C(4) C 0.5284(1) -0.0171(1) 0.7814(1) 0.0411(3) Uani 1.00 d
C(4a) C 0.58855(10) 0.0203(1) 0.6785(1) 0.0380(3) Uani 1.00 d
C(4') C 0.1143(1) 0.2038(1) 0.9857(1) 0.0511(4) Uani 1.00 d
C(5) C 0.6801(1) -0.0414(1) 0.6515(1) 0.0404(3) Uani 1.00 d
C(5') C 0.1219(1) 0.1162(2) 0.8911(2) 0.0546(4) Uani 1.00 d
C(6) C 0.7401(1) 0.0009(1) 0.5585(1) 0.0424(3) Uani 1.00 d
C(6') C 0.1987(1) 0.1241(1) 0.8072(2) 0.0549(4) Uani 1.00 d
C(7) C 0.7081(1) 0.1053(1) 0.4870(1) 0.0448(3) Uani 1.00 d
C(8) C 0.6169(1) 0.1672(1) 0.5090(1) 0.0453(3) Uani 1.00 d
C(9) C 0.9275(1) -0.0250(2) 0.6351(2) 0.0669(5) Uani 1.00 d
H(2') H 0.311(2) 0.368(2) 0.932(2) 0.069(5) Uiso 1.00 calc
H(3) H 0.403(1) 0.038(2) 0.870(2) 0.056(4) Uiso 1.00 calc
H(3') H 0.181(2) 0.358(2) 1.071(2) 0.074(6) Uiso 1.00 calc
H(4') H 0.017(2) 0.258(3) 1.096(2) 0.102(8) Uiso 1.00 calc
H(5) H 0.662(2) -0.152(2) 0.776(3) 0.098(7) Uiso 1.00 calc
H(5') H 0.072(2) 0.057(2) 0.876(2) 0.059(5) Uiso 1.00 calc
H(6a) H 0.915(2) -0.050(2) 0.739(3) 0.109(8) Uiso 1.00 calc
H(6b) H 0.943(2) 0.065(2) 0.612(2) 0.103(7) Uiso 1.00 calc
H(6c) H 0.986(2) -0.069(2) 0.601(2) 0.101(8) Uiso 1.00 calc
H(6') H 0.205(2) 0.058(2) 0.741(2) 0.065(5) Uiso 1.00 calc
H(7) H 0.754(2) 0.212(2) 0.368(2) 0.072(6) Uiso 1.00 calc
H(8) H 0.598(1) 0.239(2) 0.464(2) 0.055(4) Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-04-22T19:45:00+03:00
'Updated bibliographic information.'
|
1500001.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500001.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_1500001
loop_
_publ_author_name
'David J. Steward'
'Osvald Knop'
'Conrad Ayasse'
'F. W. D. Woodhams'
_publ_section_title
'Pyrochlores. VII. The oxides of antimony: an X-ray and Moessbauer study'
_journal_name_full 'Canadian Journal of Chemistry'
_journal_page_first 690
_journal_page_last 700
_journal_paper_doi 10.1139/v72-106
_journal_volume 50
_journal_year 1972
_chemical_formula_sum 'O13 Sb6'
_chemical_name_common 'Antimony Oxide (6/13)'
_space_group_IT_number 227
_symmetry_space_group_name_Hall '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M 'F d -3 m :2'
_audit_creation_method 'Crystallographica 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.303
_cell_length_b 10.303
_cell_length_c 10.303
_cell_volume 1093.68
_cod_data_source_file 108994.cif
_cod_data_source_block AntimonyOxide
_cod_original_sg_symbol_H-M 'F d -3 m'
_cod_original_formula_sum 'Sb6 O13'
_cod_database_code 1500001
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, y+1/2, z+1/2'
'x+1/2, y, z+1/2'
'x+1/2, y+1/2, z'
'-x, -y, -z'
'-x, -y+1/2, -z+1/2'
'-x+1/2, -y, -z+1/2'
'-x+1/2, -y+1/2, -z'
'-y, x+1/4, z+1/4'
'-y, x-1/4, z-1/4'
'-y+1/2, x+1/4, z-1/4'
'-y+1/2, x-1/4, z+1/4'
'y, -x-1/4, -z-1/4'
'y, -x+1/4, -z+1/4'
'y+1/2, -x-1/4, -z+1/4'
'y+1/2, -x+1/4, -z-1/4'
'-x+1/4, -y+1/4, z'
'-x+1/4, -y-1/4, z+1/2'
'-x-1/4, -y+1/4, z+1/2'
'-x-1/4, -y-1/4, z'
'x-1/4, y-1/4, -z'
'x-1/4, y+1/4, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, y+1/4, -z'
'y+1/4, -x, z+1/4'
'y+1/4, -x+1/2, z-1/4'
'y-1/4, -x, z-1/4'
'y-1/4, -x+1/2, z+1/4'
'-y-1/4, x, -z-1/4'
'-y-1/4, x+1/2, -z+1/4'
'-y+1/4, x, -z+1/4'
'-y+1/4, x+1/2, -z-1/4'
'x+1/4, -z, y+1/4'
'x+1/4, -z+1/2, y-1/4'
'x-1/4, -z, y-1/4'
'x-1/4, -z+1/2, y+1/4'
'-x-1/4, z, -y-1/4'
'-x-1/4, z+1/2, -y+1/4'
'-x+1/4, z, -y+1/4'
'-x+1/4, z+1/2, -y-1/4'
'x, -y+1/4, -z+1/4'
'x, -y-1/4, -z-1/4'
'x+1/2, -y+1/4, -z-1/4'
'x+1/2, -y-1/4, -z+1/4'
'-x, y-1/4, z-1/4'
'-x, y+1/4, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, z+1/4, -y'
'x+1/4, z-1/4, -y+1/2'
'x-1/4, z+1/4, -y+1/2'
'x-1/4, z-1/4, -y'
'-x-1/4, -z-1/4, y'
'-x-1/4, -z+1/4, y+1/2'
'-x+1/4, -z-1/4, y+1/2'
'-x+1/4, -z+1/4, y'
'z+1/4, y+1/4, -x'
'z+1/4, y-1/4, -x+1/2'
'z-1/4, y+1/4, -x+1/2'
'z-1/4, y-1/4, -x'
'-z-1/4, -y-1/4, x'
'-z-1/4, -y+1/4, x+1/2'
'-z+1/4, -y-1/4, x+1/2'
'-z+1/4, -y+1/4, x'
'-x+1/4, y, -z+1/4'
'-x+1/4, y+1/2, -z-1/4'
'-x-1/4, y, -z-1/4'
'-x-1/4, y+1/2, -z+1/4'
'x-1/4, -y, z-1/4'
'x-1/4, -y+1/2, z+1/4'
'x+1/4, -y, z+1/4'
'x+1/4, -y+1/2, z-1/4'
'-z, y+1/4, x+1/4'
'-z, y-1/4, x-1/4'
'-z+1/2, y+1/4, x-1/4'
'-z+1/2, y-1/4, x+1/4'
'z, -y-1/4, -x-1/4'
'z, -y+1/4, -x+1/4'
'z+1/2, -y-1/4, -x+1/4'
'z+1/2, -y+1/4, -x-1/4'
'z, x, y'
'z, x+1/2, y+1/2'
'z+1/2, x, y+1/2'
'z+1/2, x+1/2, y'
'-z, -x, -y'
'-z, -x+1/2, -y+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, -x+1/2, -y'
'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, -x'
'-y+1/4, -z+1/4, x'
'-y+1/4, -z-1/4, x+1/2'
'-y-1/4, -z+1/4, x+1/2'
'-y-1/4, -z-1/4, x'
'y-1/4, z-1/4, -x'
'y-1/4, z+1/4, -x+1/2'
'y+1/4, z-1/4, -x+1/2'
'y+1/4, z+1/4, -x'
'z, -x+1/4, -y+1/4'
'z, -x-1/4, -y-1/4'
'z+1/2, -x+1/4, -y-1/4'
'z+1/2, -x-1/4, -y+1/4'
'-z, x-1/4, y-1/4'
'-z, x+1/4, y+1/4'
'-z+1/2, x-1/4, y+1/4'
'-z+1/2, x+1/4, y-1/4'
'-y+1/4, z, -x+1/4'
'-y+1/4, z+1/2, -x-1/4'
'-y-1/4, z, -x-1/4'
'-y-1/4, z+1/2, -x+1/4'
'y-1/4, -z, x-1/4'
'y-1/4, -z+1/2, x+1/4'
'y+1/4, -z, x+1/4'
'y+1/4, -z+1/2, x-1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, -x-1/4, y+1/2'
'-z-1/4, -x+1/4, y+1/2'
'-z-1/4, -x-1/4, y'
'z-1/4, x-1/4, -y'
'z-1/4, x+1/4, -y+1/2'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, x+1/4, -y'
'-z+1/4, x, -y+1/4'
'-z+1/4, x+1/2, -y-1/4'
'-z-1/4, x, -y-1/4'
'-z-1/4, x+1/2, -y+1/4'
'z-1/4, -x, y-1/4'
'z-1/4, -x+1/2, y+1/4'
'z+1/4, -x, y+1/4'
'z+1/4, -x+1/2, y-1/4'
'y, -z+1/4, -x+1/4'
'y, -z-1/4, -x-1/4'
'y+1/2, -z+1/4, -x-1/4'
'y+1/2, -z-1/4, -x+1/4'
'-y, z-1/4, x-1/4'
'-y, z+1/4, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, x+1/4, -z'
'y+1/4, x-1/4, -z+1/2'
'y-1/4, x+1/4, -z+1/2'
'y-1/4, x-1/4, -z'
'-y-1/4, -x-1/4, z'
'-y-1/4, -x+1/4, z+1/2'
'-y+1/4, -x-1/4, z+1/2'
'-y+1/4, -x+1/4, z'
'-y, -x, -z'
'-y, -x+1/2, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-y+1/2, -x+1/2, -z'
'y, x, z'
'y, x+1/2, z+1/2'
'y+1/2, x, z+1/2'
'y+1/2, x+1/2, z'
'-x, z+1/4, y+1/4'
'-x, z-1/4, y-1/4'
'-x+1/2, z+1/4, y-1/4'
'-x+1/2, z-1/4, y+1/4'
'x, -z-1/4, -y-1/4'
'x, -z+1/4, -y+1/4'
'x+1/2, -z-1/4, -y+1/4'
'x+1/2, -z+1/4, -y-1/4'
'-x, -z, -y'
'-x, -z+1/2, -y+1/2'
'-x+1/2, -z, -y+1/2'
'-x+1/2, -z+1/2, -y'
'x, z, y'
'x, z+1/2, y+1/2'
'x+1/2, z, y+1/2'
'x+1/2, z+1/2, y'
'z+1/4, -y, x+1/4'
'z+1/4, -y+1/2, x-1/4'
'z-1/4, -y, x-1/4'
'z-1/4, -y+1/2, x+1/4'
'-z-1/4, y, -x-1/4'
'-z-1/4, y+1/2, -x+1/4'
'-z+1/4, y, -x+1/4'
'-z+1/4, y+1/2, -x-1/4'
'-z, -y, -x'
'-z, -y+1/2, -x+1/2'
'-z+1/2, -y, -x+1/2'
'-z+1/2, -y+1/2, -x'
'z, y, x'
'z, y+1/2, x+1/2'
'z+1/2, y, x+1/2'
'z+1/2, y+1/2, x'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
Sb1 Sb5+ 0.5 0.5 0.5 0.0113986 Uiso 1
Sb2 Sb3+ 0 0 0 0.0785239 Uiso 0.5
O1 O2- 0.125 0.125 0.125 0.149449 Uiso 0.5
O2 O2- 0.4304 0.125 0.125 0.0215308 Uiso 1
|
1500002.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500002.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_1500002
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Chlorocadmate(II) salts of two
1,2,4-triazolo[1,5-a]pyrimidine derivatives
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 30
_journal_page_last 34
_journal_paper_doi 10.1016/j.molstruc.2007.09.004
_journal_volume 882
_journal_year 2008
_chemical_formula_moiety '2(C7 H9 N4 1+), Cd Cl4 2-, 2(H2 O)'
_chemical_formula_sum 'C14 H22 Cd Cl4 N8 O2'
_chemical_formula_weight 588.60
_chemical_name_systematic
;
?
;
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 98.6720(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.7860(7)
_cell_length_b 9.4013(5)
_cell_length_c 17.6679(9)
_cell_measurement_reflns_used 5409
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.23
_cell_measurement_theta_min 2.33
_cell_volume 2263.7(2)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0141
_diffrn_reflns_av_sigmaI/netI 0.0154
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 6876
_diffrn_reflns_theta_full 27.00
_diffrn_reflns_theta_max 28.23
_diffrn_reflns_theta_min 2.33
_diffrn_standards_decay_% 0
_diffrn_standards_number 372
_exptl_absorpt_coefficient_mu 1.465
_exptl_absorpt_correction_T_max 0.7020
_exptl_absorpt_correction_T_min 0.4942
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour white
_exptl_crystal_density_diffrn 1.727
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1176
_exptl_crystal_size_max 0.54
_exptl_crystal_size_mid 0.39
_exptl_crystal_size_min 0.26
_refine_diff_density_max 0.384
_refine_diff_density_min -0.401
_refine_diff_density_rms 0.087
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 140
_refine_ls_number_reflns 2585
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.060
_refine_ls_R_factor_all 0.0236
_refine_ls_R_factor_gt 0.0222
_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^)+(0.0350P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0580
_refine_ls_wR_factor_ref 0.0590
_reflns_number_gt 2458
_reflns_number_total 2585
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file cdcl4.cif
_cod_data_source_block cdcl4
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1500002
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
Cd Cd 0.5000 0.469121(18) 0.2500 0.03811(7) Uani 1 2 d S
Cl1 Cl 0.41039(4) 0.59926(5) 0.33803(3) 0.05197(12) Uani 1 1 d .
Cl2 Cl 0.61379(4) 0.31931(5) 0.33901(2) 0.05010(12) Uani 1 1 d .
N1 N 0.17711(12) 0.57490(18) 0.50818(9) 0.0442(3) Uani 1 1 d .
C2 C 0.24991(15) 0.5678(2) 0.46891(11) 0.0461(4) Uani 1 1 d .
H2 H 0.2560 0.6283 0.4282 0.055 Uiso 1 1 d R
N3 N 0.31551(12) 0.46450(15) 0.49324(9) 0.0432(3) Uani 1 1 d .
H3 H 0.3675 0.4436 0.4741 0.052 Uiso 1 1 d R
C3A C 0.28353(12) 0.40057(18) 0.55332(9) 0.0374(3) Uani 1 1 d .
N4 N 0.32303(11) 0.29319(16) 0.59543(9) 0.0424(3) Uani 1 1 d .
C5 C 0.27373(14) 0.25528(19) 0.65189(10) 0.0423(4) Uani 1 1 d .
C51 C 0.31528(17) 0.1361(2) 0.70221(12) 0.0576(5) Uani 1 1 d .
H51 H 0.3800 0.1140 0.6918 0.069 Uiso 1 1 d R
H52 H 0.2740 0.0538 0.6924 0.069 Uiso 1 1 d R
H53 H 0.3187 0.1635 0.7549 0.069 Uiso 1 1 d R
C6 C 0.18627(13) 0.3231(2) 0.66399(10) 0.0436(4) Uani 1 1 d .
H6 H 0.1552 0.2939 0.7046 0.052 Uiso 1 1 d R
C7 C 0.14607(12) 0.4299(2) 0.61776(10) 0.0388(3) Uani 1 1 d .
C71 C 0.05215(15) 0.5049(2) 0.62183(13) 0.0500(4) Uani 1 1 d .
H71 H 0.0644 0.6047 0.6299 0.060 Uiso 1 1 d R
H72 H 0.0228 0.4671 0.6635 0.060 Uiso 1 1 d R
H73 H 0.0084 0.4912 0.5747 0.060 Uiso 1 1 d R
N8 N 0.19914(11) 0.46799(14) 0.56167(8) 0.0364(3) Uani 1 1 d .
O1W O 0.47990(12) 0.31988(19) 0.47678(9) 0.0599(4) Uani 1 1 d D
H11W H 0.5209(15) 0.317(3) 0.4485(13) 0.072 Uiso 1 1 d D
H12W H 0.5057(18) 0.308(3) 0.5211(7) 0.072 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
Cd 0.04052(11) 0.04028(11) 0.03381(10) 0.000 0.00647(7) 0.000
Cl1 0.0594(3) 0.0525(3) 0.0468(2) -0.00343(19) 0.0171(2) 0.0086(2)
Cl2 0.0540(3) 0.0583(3) 0.0374(2) 0.00377(18) 0.00498(18) 0.0153(2)
N1 0.0504(9) 0.0440(8) 0.0379(7) 0.0037(6) 0.0051(6) -0.0013(7)
C2 0.0564(11) 0.0444(9) 0.0386(9) 0.0010(7) 0.0110(8) -0.0056(8)
N3 0.0459(8) 0.0450(9) 0.0410(8) -0.0032(6) 0.0139(6) -0.0060(6)
C3A 0.0377(8) 0.0394(8) 0.0352(8) -0.0059(6) 0.0052(6) -0.0066(7)
N4 0.0412(8) 0.0433(8) 0.0419(8) -0.0027(6) 0.0040(6) -0.0013(6)
C5 0.0488(9) 0.0396(9) 0.0364(8) -0.0024(7) -0.0001(7) -0.0064(7)
C51 0.0693(13) 0.0505(11) 0.0496(11) 0.0055(9) -0.0026(9) 0.0035(10)
C6 0.0472(9) 0.0478(10) 0.0364(8) -0.0001(7) 0.0083(7) -0.0085(8)
C7 0.0379(8) 0.0433(8) 0.0355(8) -0.0057(7) 0.0064(6) -0.0088(7)
C71 0.0426(10) 0.0560(11) 0.0531(11) -0.0050(9) 0.0128(8) -0.0003(8)
N8 0.0371(7) 0.0384(7) 0.0331(7) -0.0020(5) 0.0034(5) -0.0042(5)
O1W 0.0581(9) 0.0718(10) 0.0503(8) -0.0008(7) 0.0101(6) 0.0116(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Cl1 Cd Cl1 120.18(3) 2_655 .
Cl1 Cd Cl2 110.712(17) 2_655 .
Cl1 Cd Cl2 102.217(16) . .
Cl1 Cd Cl2 102.215(16) 2_655 2_655
Cl1 Cd Cl2 110.712(18) . 2_655
Cl2 Cd Cl2 110.94(3) . 2_655
C2 N1 N8 102.66(16) . .
N1 C2 N3 113.49(17) . .
N1 C2 H2 123.1 . .
N3 C2 H2 123.4 . .
C3A N3 C2 106.72(16) . .
C3A N3 H3 126.6 . .
C2 N3 H3 126.6 . .
N4 C3A N3 128.81(16) . .
N4 C3A N8 125.79(16) . .
N3 C3A N8 105.39(15) . .
C3A N4 C5 114.26(15) . .
N4 C5 C6 122.39(16) . .
N4 C5 C51 116.90(18) . .
C6 C5 C51 120.71(18) . .
C5 C51 H51 109.4 . .
C5 C51 H52 109.5 . .
H51 C51 H52 109.5 . .
C5 C51 H53 109.5 . .
H51 C51 H53 109.5 . .
H52 C51 H53 109.5 . .
C7 C6 C5 121.61(17) . .
C7 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
C6 C7 N8 114.55(16) . .
C6 C7 C71 126.97(17) . .
N8 C7 C71 118.47(17) . .
C7 C71 H71 109.6 . .
C7 C71 H72 109.4 . .
H71 C71 H72 109.5 . .
C7 C71 H73 109.4 . .
H71 C71 H73 109.5 . .
H72 C71 H73 109.5 . .
C3A N8 C7 121.34(15) . .
C3A N8 N1 111.74(14) . .
C7 N8 N1 126.91(15) . .
H11W O1W H12W 110(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd Cl1 2.4538(5) 2_655
Cd Cl1 2.4539(5) .
Cd Cl2 2.4846(4) .
Cd Cl2 2.4847(4) 2_655
N1 C2 1.305(2) .
N1 N8 1.382(2) .
C2 N3 1.352(3) .
C2 H2 0.9300 .
N3 C3A 1.350(2) .
N3 H3 0.8600 .
C3A N4 1.322(2) .
C3A N8 1.352(2) .
N4 C5 1.337(2) .
C5 C6 1.408(3) .
C5 C51 1.490(3) .
C51 H51 0.9600 .
C51 H52 0.9600 .
C51 H53 0.9601 .
C6 C7 1.359(3) .
C6 H6 0.9300 .
C7 N8 1.365(2) .
C7 C71 1.486(3) .
C71 H71 0.9600 .
C71 H72 0.9600 .
C71 H73 0.9600 .
O1W H11W 0.809(10) .
O1W H12W 0.817(10) .
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
O1W H11W Cl2 0.809(10) 2.476(12) 3.2692(17) 167(3)
N3 H3 O1W 0.86 1.93 2.696(2) 147.3
|
1500003.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500003.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_1500003
loop_
_publ_author_name
'Sonia B. Jim\'enez-Pulido'
'F\'atima M. Linares-Ordo\~nez'
'Miguel N. Moreno-Carretero'
'Miguel Quir\'os'
_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
;
Versatile Coordinative Abilities of a New Hybrid Pteridine-Thiosemicarbazone
Ligand: Crystal Structure, Spectroscopic Characterization, and
Luminescent Properties
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1096
_journal_page_last 1106
_journal_paper_doi 10.1021/ic701994s
_journal_volume 47
_journal_year 2008
_chemical_formula_sum 'C14 H21 Cd N9 O9 S'
_chemical_formula_weight 603.86
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 117.6730(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.8903(6)
_cell_length_b 13.1999(7)
_cell_length_c 14.7455(7)
_cell_measurement_reflns_used 5951
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.82
_cell_measurement_theta_min 2.19
_cell_volume 2221.96(19)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material '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 66.06
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0313
_diffrn_reflns_av_sigmaI/netI 0.0239
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 25308
_diffrn_reflns_theta_full 28.33
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 1.78
_exptl_absorpt_coefficient_mu 1.144
_exptl_absorpt_correction_T_max 0.8035
_exptl_absorpt_correction_T_min 0.6679
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.805
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular shape'
_exptl_crystal_F_000 1216
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_refine_diff_density_max 1.875
_refine_diff_density_min -0.806
_refine_diff_density_rms 0.114
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.997
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 315
_refine_ls_number_reflns 5214
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 0.997
_refine_ls_R_factor_all 0.0521
_refine_ls_R_factor_gt 0.0485
_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^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1437
_refine_ls_wR_factor_ref 0.1473
_reflns_number_gt 4795
_reflns_number_total 5214
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file cdiaz.cif
_cod_data_source_block cdiaz
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500003
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
Cd Cd 0.24353(2) 0.26256(2) 0.26394(2) 0.04047(13) Uani 1 1 d .
N1 N 0.2023(3) 0.6795(2) 0.3020(3) 0.0483(8) Uani 1 1 d .
C1 C 0.2072(5) 0.7879(4) 0.2829(5) 0.0709(14) Uani 1 1 d .
H11 H 0.1387 0.8210 0.2786 0.085 Uiso 1 1 d R
H12 H 0.2101 0.7965 0.2194 0.085 Uiso 1 1 d R
H13 H 0.2759 0.8172 0.3376 0.085 Uiso 1 1 d R
C1A C 0.2421(3) 0.6080(3) 0.2563(3) 0.0422(8) Uani 1 1 d .
C2 C 0.1629(3) 0.6514(3) 0.3695(3) 0.0490(9) Uani 1 1 d .
O2 O 0.1381(3) 0.7143(3) 0.4167(3) 0.0628(9) Uani 1 1 d .
N3 N 0.1511(3) 0.5491(3) 0.3835(3) 0.0492(8) Uani 1 1 d .
C3 C 0.0912(5) 0.5211(4) 0.4443(4) 0.0689(13) Uani 1 1 d .
H31 H 0.0110 0.5426 0.4089 0.083 Uiso 1 1 d R
H32 H 0.1292 0.5533 0.5101 0.083 Uiso 1 1 d R
H33 H 0.0944 0.4489 0.4530 0.083 Uiso 1 1 d R
C4 C 0.1874(3) 0.4718(3) 0.3426(3) 0.0465(8) Uani 1 1 d .
O4 O 0.1783(3) 0.3827(2) 0.3580(3) 0.0580(8) Uani 1 1 d .
C4A C 0.2402(3) 0.5072(3) 0.2787(3) 0.0397(7) Uani 1 1 d .
N5 N 0.2843(3) 0.4367(2) 0.2413(2) 0.0369(6) Uani 1 1 d .
C6 C 0.3267(3) 0.4650(3) 0.1790(3) 0.0378(7) Uani 1 1 d .
C7 C 0.3199(3) 0.5689(3) 0.1494(3) 0.0430(8) Uani 1 1 d .
C71 C 0.3493(5) 0.6067(3) 0.0685(4) 0.0590(11) Uani 1 1 d .
H71 H 0.3114 0.6707 0.0431 0.071 Uiso 1 1 d R
H72 H 0.3230 0.5589 0.0132 0.071 Uiso 1 1 d R
H73 H 0.4326 0.6152 0.0973 0.071 Uiso 1 1 d R
N8 N 0.2797(3) 0.6387(3) 0.1900(3) 0.0476(7) Uani 1 1 d .
C9 C 0.3755(3) 0.3820(3) 0.1419(3) 0.0384(7) Uani 1 1 d .
C91 C 0.4721(4) 0.3976(3) 0.1142(4) 0.0539(10) Uani 1 1 d .
H91 H 0.5281 0.3436 0.1421 0.065 Uiso 1 1 d R
H92 H 0.5101 0.4611 0.1417 0.065 Uiso 1 1 d R
H93 H 0.4402 0.3983 0.0411 0.065 Uiso 1 1 d R
N10 N 0.3337(3) 0.2946(2) 0.1452(2) 0.0390(6) Uani 1 1 d .
N11 N 0.3740(3) 0.2135(2) 0.1129(3) 0.0454(7) Uani 1 1 d .
H111 H 0.4092 0.2231 0.0764 0.055 Uiso 1 1 d R
C12 C 0.3586(4) 0.1185(3) 0.1383(3) 0.0453(8) Uani 1 1 d .
N12 N 0.3964(4) 0.0460(3) 0.0984(3) 0.0617(10) Uani 1 1 d .
H121 H 0.4280 0.0616 0.0601 0.074 Uiso 1 1 d R
H122 H 0.3898 -0.0165 0.1113 0.074 Uiso 1 1 d R
S12 S 0.29959(11) 0.08935(8) 0.21559(9) 0.0547(3) Uani 1 1 d .
N1N N 0.5039(3) 0.3322(2) 0.4398(2) 0.0447(7) Uani 1 1 d .
O1N O 0.4152(3) 0.2827(3) 0.4306(2) 0.0597(8) Uani 1 1 d .
O2N O 0.5300(3) 0.3341(2) 0.3708(2) 0.0571(7) Uani 1 1 d .
O3N O 0.5601(3) 0.3796(3) 0.5206(2) 0.0693(9) Uani 1 1 d .
N2N N 0.1392(4) 0.1039(4) 0.3430(4) 0.0750(13) Uani 1 1 d .
O4N O 0.0861(3) 0.1613(3) 0.2678(3) 0.0776(10) Uani 1 1 d .
O5N O 0.2407(4) 0.1296(5) 0.4011(3) 0.1099(18) Uani 1 1 d .
O6N O 0.0904(7) 0.0298(4) 0.3553(6) 0.147(3) Uani 1 1 d .
C1E C 0.0354(6) 0.3554(6) 0.0343(5) 0.090(2) Uani 1 1 d D
H11E H 0.0915 0.4056 0.0367 0.109 Uiso 1 1 d R
H12E H -0.0408 0.3874 0.0083 0.109 Uiso 1 1 d R
O1E O 0.0686(3) 0.3165(3) 0.1301(3) 0.0797(12) Uani 1 1 d D
H1E H 0.027(5) 0.263(3) 0.1237(16) 0.096 Uiso 1 1 d D
C2E C 0.0267(11) 0.2691(7) -0.0356(7) 0.128(4) Uani 1 1 d .
H21E H 0.0880 0.2217 0.0029 0.154 Uiso 1 1 d R
H22E H 0.0366 0.2942 -0.0922 0.154 Uiso 1 1 d R
H23E H -0.0479 0.2359 -0.0609 0.154 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd 0.04591(19) 0.03498(18) 0.04158(19) 0.00320(9) 0.02120(14) 0.00085(9)
N1 0.0456(17) 0.0356(16) 0.0565(19) -0.0068(14) 0.0176(15) 0.0058(13)
C1 0.075(3) 0.039(2) 0.099(4) -0.010(2) 0.040(3) 0.001(2)
C1A 0.0350(17) 0.037(2) 0.0457(19) -0.0038(14) 0.0117(15) 0.0032(13)
C2 0.0324(16) 0.054(2) 0.051(2) -0.0138(18) 0.0112(15) 0.0068(15)
O2 0.0477(16) 0.0640(19) 0.069(2) -0.0242(17) 0.0208(15) 0.0049(14)
N3 0.0459(17) 0.056(2) 0.0497(18) -0.0020(15) 0.0253(15) 0.0079(15)
C3 0.080(3) 0.073(3) 0.075(3) 0.006(3) 0.054(3) 0.016(3)
C4 0.048(2) 0.047(2) 0.0450(19) -0.0001(16) 0.0216(17) 0.0036(16)
O4 0.078(2) 0.0456(16) 0.067(2) 0.0061(14) 0.0481(18) 0.0055(14)
C4A 0.0398(17) 0.0356(18) 0.0407(17) -0.0035(13) 0.0163(15) 0.0015(13)
N5 0.0376(13) 0.0321(14) 0.0391(15) 0.0006(11) 0.0161(12) 0.0015(11)
C6 0.0374(16) 0.0368(17) 0.0345(16) -0.0011(13) 0.0128(13) -0.0010(13)
C7 0.0428(18) 0.0378(18) 0.0421(18) 0.0007(14) 0.0142(15) -0.0043(14)
C71 0.076(3) 0.045(2) 0.064(3) 0.0099(19) 0.040(2) 0.001(2)
N8 0.0468(17) 0.0367(16) 0.0547(19) 0.0008(14) 0.0197(15) 0.0007(13)
C9 0.0378(16) 0.0398(18) 0.0360(17) -0.0027(13) 0.0158(14) -0.0031(13)
C91 0.047(2) 0.058(2) 0.065(3) -0.012(2) 0.0324(19) -0.0089(18)
N10 0.0460(16) 0.0329(14) 0.0422(15) -0.0004(12) 0.0239(13) 0.0008(12)
N11 0.0593(19) 0.0357(15) 0.0518(18) -0.0049(14) 0.0347(16) 0.0013(14)
C12 0.050(2) 0.0378(19) 0.0427(19) -0.0055(15) 0.0173(16) 0.0035(15)
N12 0.084(3) 0.0399(18) 0.069(2) -0.0007(17) 0.042(2) 0.0133(18)
S12 0.0770(7) 0.0372(5) 0.0601(6) 0.0045(4) 0.0404(6) 0.0050(5)
N1N 0.0456(16) 0.0377(16) 0.0431(16) 0.0053(13) 0.0142(13) 0.0031(13)
O1N 0.0609(19) 0.0656(19) 0.0477(16) 0.0040(15) 0.0212(14) -0.0165(16)
O2N 0.0711(19) 0.0495(17) 0.0574(17) 0.0013(13) 0.0355(15) -0.0009(14)
O3N 0.0622(19) 0.087(3) 0.0491(17) -0.0116(16) 0.0177(15) -0.0158(17)
N2N 0.076(3) 0.080(3) 0.067(3) 0.025(2) 0.032(2) -0.010(2)
O4N 0.066(2) 0.090(3) 0.069(2) 0.026(2) 0.0248(17) 0.0050(19)
O5N 0.059(2) 0.192(6) 0.058(2) 0.005(3) 0.0090(18) -0.008(3)
O6N 0.224(7) 0.084(4) 0.193(6) 0.016(4) 0.148(6) -0.035(4)
C1E 0.076(4) 0.102(5) 0.077(4) 0.021(4) 0.021(3) -0.014(3)
O1E 0.0516(18) 0.088(3) 0.079(2) 0.029(2) 0.0124(17) -0.0148(18)
C2E 0.158(9) 0.148(8) 0.094(6) -0.024(5) 0.072(6) -0.045(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O1E Cd N5 77.14(12)
O1E Cd O1N 153.41(15)
N5 Cd O1N 83.22(10)
O1E Cd O4N 72.43(12)
N5 Cd O4N 139.21(12)
O1N Cd O4N 114.16(11)
O1E Cd O4 80.34(15)
N5 Cd O4 67.87(10)
O1N Cd O4 75.70(12)
O4N Cd O4 80.64(13)
O1E Cd N10 86.43(12)
N5 Cd N10 63.18(10)
O1N Cd N10 100.61(11)
O4N Cd N10 138.87(12)
O4 Cd N10 130.97(10)
O1E Cd S12 108.79(13)
N5 Cd S12 133.95(8)
O1N Cd S12 97.73(10)
O4N Cd S12 82.27(11)
O4 Cd S12 157.08(8)
N10 Cd S12 71.53(7)
O1E Cd O5N 119.59(12)
N5 Cd O5N 143.56(14)
O1N Cd O5N 68.70(12)
O4N Cd O5N 47.70(12)
O4 Cd O5N 82.59(15)
N10 Cd O5N 142.64(14)
S12 Cd O5N 74.61(13)
C2 N1 C1A 121.0(4)
C2 N1 C1 118.1(4)
C1A N1 C1 120.8(4)
N8 C1A C4A 121.4(4)
N8 C1A N1 119.3(4)
C4A C1A N1 119.4(4)
O2 C2 N1 121.2(4)
O2 C2 N3 120.2(4)
N1 C2 N3 118.6(3)
C4 N3 C2 125.1(4)
C4 N3 C3 117.5(4)
C2 N3 C3 117.3(4)
O4 C4 N3 123.7(4)
O4 C4 C4A 122.8(4)
N3 C4 C4A 113.5(4)
C4 O4 Cd 115.1(3)
N5 C4A C1A 121.2(4)
N5 C4A C4 117.0(3)
C1A C4A C4 121.8(3)
C6 N5 C4A 118.8(3)
C6 N5 Cd 123.5(2)
C4A N5 Cd 116.4(2)
N5 C6 C7 119.8(3)
N5 C6 C9 115.4(3)
C7 C6 C9 124.8(3)
N8 C7 C6 120.6(4)
N8 C7 C71 115.1(4)
C6 C7 C71 124.2(4)
C7 N8 C1A 117.9(4)
N10 C9 C6 113.1(3)
N10 C9 C91 123.4(4)
C6 C9 C91 123.2(3)
C9 N10 N11 117.2(3)
C9 N10 Cd 120.6(2)
N11 N10 Cd 118.5(2)
C12 N11 N10 120.2(3)
N12 C12 N11 114.5(4)
N12 C12 S12 120.7(3)
N11 C12 S12 124.8(3)
C12 S12 Cd 104.83(14)
O2N N1N O3N 122.1(4)
O2N N1N O1N 120.6(3)
O3N N1N O1N 117.3(4)
N1N O1N Cd 121.0(2)
O6N N2N O5N 124.8(6)
O6N N2N O4N 120.6(6)
O5N N2N O4N 114.6(5)
N2N O4N Cd 103.4(3)
N2N O5N Cd 92.2(3)
O1E C1E C2E 108.1(7)
C1E O1E Cd 135.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cd O1E 2.313(3)
Cd N5 2.415(3)
Cd O1N 2.440(3)
Cd O4N 2.453(4)
Cd O4 2.496(3)
Cd N10 2.547(3)
Cd S12 2.5955(11)
Cd O5N 2.690(5)
N1 C2 1.362(6)
N1 C1A 1.389(5)
N1 C1 1.465(6)
C1A N8 1.340(5)
C1A C4A 1.373(6)
C2 O2 1.218(5)
C2 N3 1.385(6)
N3 C4 1.373(5)
N3 C3 1.476(6)
C4 O4 1.214(5)
C4 C4A 1.471(5)
C4A N5 1.336(5)
N5 C6 1.322(5)
C6 C7 1.429(5)
C6 C9 1.488(5)
C7 N8 1.328(5)
C7 C71 1.496(6)
C9 N10 1.283(5)
C9 C91 1.494(5)
N10 N11 1.367(4)
N11 C12 1.350(5)
C12 N12 1.328(5)
C12 S12 1.682(5)
N1N O2N 1.211(4)
N1N O3N 1.239(4)
N1N O1N 1.268(5)
N2N O6N 1.221(6)
N2N O5N 1.233(6)
N2N O4N 1.252(6)
C1E O1E 1.371(7)
C1E C2E 1.505(11)
|
1500004.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500004.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_1500004
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Chlorocadmate(II) salts of two
1,2,4-triazolo[1,5-a]pyrimidine derivatives
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 30
_journal_page_last 34
_journal_paper_doi 10.1016/j.molstruc.2007.09.004
_journal_volume 882
_journal_year 2008
_chemical_formula_moiety 'C5 H5 N4 1+, Cd Cl3 1-'
_chemical_formula_sum 'C5 H5 Cd Cl3 N4'
_chemical_formula_weight 339.88
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 96.7100(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.7543(7)
_cell_length_b 12.6823(7)
_cell_length_c 6.6836(4)
_cell_measurement_reflns_used 4013
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.4
_cell_volume 989.51(10)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0230
_diffrn_reflns_av_sigmaI/netI 0.0251
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 6107
_diffrn_reflns_theta_full 27.00
_diffrn_reflns_theta_max 28.25
_diffrn_reflns_theta_min 1.74
_diffrn_standards_decay_% 0
_diffrn_standards_number 295
_exptl_absorpt_coefficient_mu 2.972
_exptl_absorpt_correction_T_max 0.7757
_exptl_absorpt_correction_T_min 0.5441
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.281
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description laminar
_exptl_crystal_F_000 648
_exptl_crystal_size_max 0.51
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.565
_refine_diff_density_min -0.525
_refine_diff_density_rms 0.088
_refine_ls_extinction_coef 0.0173(6)
_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 1.044
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 119
_refine_ls_number_reflns 2251
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0229
_refine_ls_R_factor_gt 0.0214
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0550
_refine_ls_wR_factor_ref 0.0559
_reflns_number_gt 2109
_reflns_number_total 2251
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file cdtpcl.cif
_cod_data_source_block cdtpcl
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500004
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
Cd Cd 0.175837(13) 0.254593(10) 0.45525(2) 0.03021(8) Uani 1 1 d .
Cl1 Cl 0.33711(4) 0.33187(4) 0.24983(7) 0.03332(12) Uani 1 1 d .
Cl2 Cl 0.03256(4) 0.33521(4) 0.17006(7) 0.03315(12) Uani 1 1 d .
Cl3 Cl 0.18814(4) 0.09312(4) 0.21503(6) 0.03436(13) Uani 1 1 d .
N1 N 0.59919(17) 0.42227(16) 0.9258(3) 0.0462(5) Uani 1 1 d .
C2 C 0.5051(2) 0.3951(2) 0.8155(4) 0.0502(6) Uani 1 1 d .
H2 H 0.4332 0.3991 0.8602 0.060 Uiso 1 1 d R
N3 N 0.52279(16) 0.36061(17) 0.6316(3) 0.0480(5) Uani 1 1 d .
H3 H 0.4711 0.3399 0.5383 0.058 Uiso 1 1 d R
C3A C 0.63641(18) 0.36456(16) 0.6204(3) 0.0350(4) Uani 1 1 d .
N4 N 0.69564(18) 0.33769(16) 0.4719(3) 0.0463(5) Uani 1 1 d .
C5 C 0.8074(2) 0.35551(19) 0.5115(4) 0.0480(6) Uani 1 1 d .
H5 H 0.8539 0.3385 0.4126 0.058 Uiso 1 1 d R
C6 C 0.8593(2) 0.39785(18) 0.6911(4) 0.0453(5) Uani 1 1 d .
H6 H 0.9380 0.4092 0.7092 0.054 Uiso 1 1 d R
C7 C 0.79562(19) 0.42261(18) 0.8374(4) 0.0420(5) Uani 1 1 d .
H7 H 0.8277 0.4513 0.9592 0.050 Uiso 1 1 d R
N8 N 0.68174(14) 0.40327(13) 0.7992(2) 0.0318(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
Cd 0.03316(12) 0.04006(12) 0.01789(11) -0.00171(5) 0.00506(7) -0.00194(5)
Cl1 0.0287(2) 0.0439(3) 0.0275(2) 0.00051(19) 0.00387(18) -0.00526(19)
Cl2 0.0290(2) 0.0445(3) 0.0261(2) 0.00100(18) 0.00411(18) 0.00629(19)
Cl3 0.0462(3) 0.0311(2) 0.0261(2) 0.00108(16) 0.0055(2) 0.00114(19)
N1 0.0423(11) 0.0512(11) 0.0470(11) -0.0147(9) 0.0135(9) -0.0047(9)
C2 0.0356(12) 0.0525(14) 0.0649(16) -0.0149(12) 0.0159(11) -0.0082(10)
N3 0.0312(10) 0.0612(12) 0.0504(12) -0.0140(10) 0.0004(8) -0.0125(9)
C3A 0.0351(11) 0.0350(10) 0.0342(11) -0.0012(8) 0.0007(8) -0.0053(8)
N4 0.0486(12) 0.0542(12) 0.0370(10) -0.0062(8) 0.0088(8) -0.0058(9)
C5 0.0479(14) 0.0428(12) 0.0571(14) 0.0009(11) 0.0229(11) 0.0018(10)
C6 0.0288(11) 0.0393(11) 0.0675(16) 0.0000(11) 0.0040(10) 0.0031(9)
C7 0.0318(11) 0.0408(12) 0.0503(13) -0.0073(10) -0.0079(10) 0.0003(9)
N8 0.0304(9) 0.0310(8) 0.0336(9) -0.0049(7) 0.0021(7) -0.0023(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Cl3 Cd Cl2 86.874(16) 4_566 4_566
Cl3 Cd Cl2 100.303(16) 4_566 .
Cl2 Cd Cl2 99.853(19) 4_566 .
Cl3 Cd Cl3 172.87(2) 4_566 .
Cl2 Cd Cl3 94.695(16) 4_566 .
Cl2 Cd Cl3 86.299(16) . .
Cl3 Cd Cl1 94.823(16) 4_566 .
Cl2 Cd Cl1 174.319(16) 4_566 .
Cl2 Cd Cl1 85.196(16) . .
Cl3 Cd Cl1 82.969(16) . .
Cl3 Cd Cl1 80.793(16) 4_566 4_566
Cl2 Cd Cl1 82.462(16) 4_566 4_566
Cl2 Cd Cl1 177.466(14) . 4_566
Cl3 Cd Cl1 92.502(16) . 4_566
Cl1 Cd Cl1 92.445(18) . 4_566
Cl3 Cd Cd 133.589(12) 4_566 4_565
Cl2 Cd Cd 127.754(11) 4_566 4_565
Cl2 Cd Cd 49.976(11) . 4_565
Cl3 Cd Cd 49.689(11) . 4_565
Cl1 Cd Cd 54.028(11) . 4_565
Cl1 Cd Cd 127.706(11) 4_566 4_565
Cl3 Cd Cd 50.392(11) 4_566 4_566
Cl2 Cd Cd 50.000(11) 4_566 4_566
Cl2 Cd Cd 132.105(11) . 4_566
Cl3 Cd Cd 126.329(12) . 4_566
Cl1 Cd Cd 127.814(11) . 4_566
Cl1 Cd Cd 50.285(10) 4_566 4_566
Cd Cd Cd 176.008(9) 4_565 4_566
Cd Cl1 Cd 75.685(13) . 4_565
Cd Cl2 Cd 80.023(14) 4_565 .
Cd Cl3 Cd 79.918(15) 4_565 .
C2 N1 N8 102.60(18) . .
N1 C2 N3 113.1(2) . .
N1 C2 H2 123.2 . .
N3 C2 H2 123.7 . .
C2 N3 C3A 107.40(19) . .
C2 N3 H3 126.3 . .
C3A N3 H3 126.3 . .
N4 C3A N8 125.0(2) . .
N4 C3A N3 130.1(2) . .
N8 C3A N3 104.88(18) . .
C3A N4 C5 113.7(2) . .
N4 C5 C6 124.1(2) . .
N4 C5 H5 117.9 . .
C6 C5 H5 118.0 . .
C7 C6 C5 119.8(2) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C6 C7 N8 116.4(2) . .
C6 C7 H7 121.9 . .
N8 C7 H7 121.7 . .
C3A N8 C7 120.94(19) . .
C3A N8 N1 112.01(17) . .
C7 N8 N1 127.02(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd Cl3 2.5898(5) 4_566
Cd Cl2 2.5999(5) 4_566
Cd Cl2 2.6009(5) .
Cd Cl3 2.6166(5) .
Cd Cl1 2.6547(5) .
Cd Cl1 2.7929(5) 4_566
Cd Cd 3.3438(2) 4_565
N1 C2 1.302(3) .
N1 N8 1.381(2) .
C2 N3 1.343(3) .
C2 H2 0.9300 .
N3 C3A 1.347(3) .
N3 H3 0.8600 .
C3A N4 1.322(3) .
C3A N8 1.343(3) .
N4 C5 1.329(3) .
C5 C6 1.389(4) .
C5 H5 0.9300 .
C6 C7 1.337(3) .
C6 H6 0.9300 .
C7 N8 1.356(3) .
C7 H7 0.9300 .
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
N3 H3 Cl1 0.86 2.34 3.1791(19) 163.7
|
1500005.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500005.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_1500005
loop_
_publ_author_name
'Ritu Bala'
'Raj Pal Sharma'
'Rajni Sharma'
'Juan M. Salas'
'Miguel Quir\'os'
'William T.A. Harrison'
_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
;
Cationic cobaltammines as anion receptors: Synthesis, characterization
an X-ray structure of bis-(hexaamminecobalt(III))
tris-(hydrogenarsenate) tetrahydrate
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 174
_journal_page_last 180
_journal_paper_doi 10.1016/j.molstruc.2006.05.047
_journal_volume 828
_journal_year 2007
_chemical_formula_moiety '2(Co H18 N6 3+), 3(As H O4 2-), 4(H2 O)'
_chemical_formula_sum 'As3 Co2 H47 N12 O16'
_chemical_formula_weight 814.12
_chemical_name_systematic
;
Hexaammine cobalt(III) hydrogenarseniate tetrahydrate
;
_space_group_IT_number 56
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ab 2ac'
_symmetry_space_group_name_H-M 'P c c n'
_atom_sites_solution_hydrogens mixed
_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 8
_cell_length_a 27.4534(16)
_cell_length_b 13.1997(8)
_cell_length_c 14.4680(8)
_cell_measurement_reflns_used 5510
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.3
_cell_measurement_theta_min 2.8
_cell_volume 5242.9(5)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0303
_diffrn_reflns_av_sigmaI/netI 0.0255
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 31491
_diffrn_reflns_theta_full 27.40
_diffrn_reflns_theta_max 28.35
_diffrn_reflns_theta_min 1.71
_diffrn_standards_decay_% -0.2
_diffrn_standards_number 790
_exptl_absorpt_coefficient_mu 5.106
_exptl_absorpt_correction_T_max 0.329
_exptl_absorpt_correction_T_min 0.199
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.063
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 3296
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.28
_refine_diff_density_max 0.394
_refine_diff_density_min -0.758
_refine_diff_density_rms 0.162
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 344
_refine_ls_number_reflns 6156
_refine_ls_number_restraints 11
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0335
_refine_ls_R_factor_gt 0.0264
_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^)+(0.0300P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0600
_refine_ls_wR_factor_ref 0.0622
_reflns_number_gt 5283
_reflns_number_total 6156
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file coars.cif
_cod_data_source_block coars
_cod_database_code 1500005
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
As1 As 0.130092(8) 0.479236(17) 0.520124(15) 0.01652(6) Uani 1 1 d .
O11 O 0.18316(6) 0.46595(14) 0.57271(14) 0.0363(5) Uani 1 1 d .
O12 O 0.13058(6) 0.57148(13) 0.44140(11) 0.0285(4) Uani 1 1 d .
O13 O 0.10883(6) 0.36985(13) 0.47834(11) 0.0270(4) Uani 1 1 d .
O14 O 0.08749(7) 0.52004(14) 0.60086(12) 0.0325(4) Uani 1 1 d D
H14 H 0.0936(11) 0.498(2) 0.6524(10) 0.039 Uiso 1 1 d D
As2 As 0.383002(8) 0.509787(16) 0.355549(15) 0.01521(6) Uani 1 1 d .
O21 O 0.32882(6) 0.45467(14) 0.36382(13) 0.0350(4) Uani 1 1 d .
O22 O 0.38011(6) 0.63576(12) 0.34866(12) 0.0277(4) Uani 1 1 d .
O23 O 0.41711(6) 0.46071(13) 0.27005(10) 0.0251(4) Uani 1 1 d .
O24 O 0.41773(7) 0.47863(15) 0.45093(12) 0.0339(5) Uani 1 1 d D
H24 H 0.4084(11) 0.508(2) 0.4975(13) 0.041 Uiso 1 1 d D
As3 As 0.126132(8) 0.504839(17) 0.191494(15) 0.01561(6) Uani 1 1 d .
O31 O 0.12092(6) 0.38040(13) 0.17634(13) 0.0328(4) Uani 1 1 d .
O32 O 0.10261(6) 0.57195(13) 0.10474(11) 0.0284(4) Uani 1 1 d .
O33 O 0.18305(5) 0.53646(14) 0.21959(12) 0.0274(4) Uani 1 1 d .
O34 O 0.08862(6) 0.53446(16) 0.28470(12) 0.0341(4) Uani 1 1 d D
H34 H 0.1048(9) 0.541(2) 0.3317(12) 0.041 Uiso 1 1 d D
Co1 Co 0.2500 0.2500 0.20528(3) 0.01370(9) Uani 1 2 d S
N11 N 0.18223(6) 0.20380(15) 0.20526(13) 0.0213(4) Uani 1 1 d .
H111 H 0.1626 0.2568 0.1977 0.026 Uiso 1 1 d R
H112 H 0.1756 0.1737 0.2588 0.026 Uiso 1 1 d R
H113 H 0.1777 0.1601 0.1592 0.026 Uiso 1 1 d R
N12 N 0.23381(7) 0.34957(14) 0.30192(13) 0.0213(4) Uani 1 1 d .
H121 H 0.2610 0.3792 0.3216 0.026 Uiso 1 1 d R
H122 H 0.2193 0.3184 0.3490 0.026 Uiso 1 1 d R
H123 H 0.2138 0.3962 0.2787 0.026 Uiso 1 1 d R
N13 N 0.23285(7) 0.34732(15) 0.10891(13) 0.0220(4) Uani 1 1 d .
H131 H 0.2597 0.3774 0.0882 0.026 Uiso 1 1 d R
H132 H 0.2127 0.3938 0.1319 0.026 Uiso 1 1 d R
H133 H 0.2183 0.3150 0.0626 0.026 Uiso 1 1 d R
Co2 Co 0.2500 0.7500 0.37388(3) 0.01467(9) Uani 1 2 d S
N21 N 0.20042(6) 0.75894(15) 0.27651(13) 0.0222(4) Uani 1 1 d .
H211 H 0.2128 0.7909 0.2277 0.027 Uiso 1 1 d R
H212 H 0.1748 0.7932 0.2976 0.027 Uiso 1 1 d R
H213 H 0.1912 0.6969 0.2601 0.027 Uiso 1 1 d R
N22 N 0.24489(7) 0.60134(14) 0.37708(14) 0.0230(4) Uani 1 1 d .
H221 H 0.2235 0.5809 0.3348 0.028 Uiso 1 1 d R
H222 H 0.2349 0.5818 0.4328 0.028 Uiso 1 1 d R
H223 H 0.2738 0.5740 0.3652 0.028 Uiso 1 1 d R
N23 N 0.19836(7) 0.75950(16) 0.46830(13) 0.0235(4) Uani 1 1 d .
H231 H 0.1779 0.8092 0.4534 0.028 Uiso 1 1 d R
H232 H 0.2117 0.7724 0.5231 0.028 Uiso 1 1 d R
H233 H 0.1822 0.7011 0.4709 0.028 Uiso 1 1 d R
Co3 Co 0.500335(9) 0.23345(2) 0.323171(18) 0.01361(7) Uani 1 1 d .
N31 N 0.49909(7) 0.12149(15) 0.23287(13) 0.0243(4) Uani 1 1 d .
H311 H 0.4958 0.1467 0.1762 0.029 Uiso 1 1 d R
H312 H 0.4741 0.0808 0.2453 0.029 Uiso 1 1 d R
H313 H 0.5267 0.0865 0.2363 0.029 Uiso 1 1 d R
N32 N 0.42913(6) 0.24057(15) 0.31918(13) 0.0191(4) Uani 1 1 d .
H321 H 0.4198 0.3042 0.3087 0.023 Uiso 1 1 d R
H322 H 0.4170 0.2197 0.3730 0.023 Uiso 1 1 d R
H323 H 0.4181 0.2009 0.2740 0.023 Uiso 1 1 d R
N33 N 0.49713(7) 0.13298(15) 0.42392(13) 0.0221(4) Uani 1 1 d .
H331 H 0.5075 0.1612 0.4762 0.027 Uiso 1 1 d R
H332 H 0.5160 0.0803 0.4100 0.027 Uiso 1 1 d R
H333 H 0.4665 0.1121 0.4310 0.027 Uiso 1 1 d R
N34 N 0.57191(6) 0.22872(14) 0.32525(13) 0.0193(4) Uani 1 1 d .
H341 H 0.5830 0.2159 0.2687 0.023 Uiso 1 1 d R
H342 H 0.5816 0.1801 0.3636 0.023 Uiso 1 1 d R
H343 H 0.5835 0.2881 0.3445 0.023 Uiso 1 1 d R
N35 N 0.50202(7) 0.34359(15) 0.41390(13) 0.0221(4) Uani 1 1 d .
H351 H 0.5304 0.3760 0.4097 0.027 Uiso 1 1 d R
H352 H 0.4987 0.3182 0.4705 0.027 Uiso 1 1 d R
H353 H 0.4778 0.3867 0.4026 0.027 Uiso 1 1 d R
N36 N 0.50184(7) 0.33439(15) 0.22481(13) 0.0229(4) Uani 1 1 d .
H361 H 0.4786 0.3802 0.2347 0.027 Uiso 1 1 d R
H362 H 0.4968 0.3043 0.1706 0.027 Uiso 1 1 d R
H363 H 0.5308 0.3649 0.2243 0.027 Uiso 1 1 d R
O1W O 0.44273(6) 0.23180(15) 0.07825(13) 0.0326(4) Uani 1 1 d D
H11W H 0.4225(8) 0.1912(18) 0.0976(19) 0.039 Uiso 1 1 d D
H12W H 0.4275(9) 0.2776(16) 0.0538(18) 0.039 Uiso 1 1 d D
O2W O 0.18274(7) 0.23201(14) 0.44574(14) 0.0324(4) Uani 1 1 d D
H21W H 0.1718(10) 0.1761(11) 0.4341(19) 0.039 Uiso 1 1 d D
H22W H 0.1604(7) 0.2694(18) 0.4606(19) 0.039 Uiso 1 1 d D
O3W O 0.25632(7) 0.62011(15) 0.11730(14) 0.0347(4) Uani 1 1 d D
H31W H 0.2767(8) 0.5777(17) 0.1027(19) 0.042 Uiso 1 1 d D
H32W H 0.2329(7) 0.593(2) 0.1420(18) 0.042 Uiso 1 1 d D
O4W O 0.56469(7) 0.22926(15) 0.55638(15) 0.0356(4) Uani 1 1 d D
H41W H 0.5828(9) 0.1801(15) 0.555(2) 0.043 Uiso 1 1 d D
H42W H 0.5812(9) 0.2732(17) 0.5810(19) 0.043 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
As1 0.01578(11) 0.01439(12) 0.01939(13) -0.00033(8) -0.00301(8) 0.00180(9)
O11 0.0223(9) 0.0293(10) 0.0574(13) -0.0021(9) -0.0188(8) 0.0040(8)
O12 0.0376(10) 0.0221(9) 0.0258(9) 0.0062(7) 0.0006(7) -0.0005(8)
O13 0.0280(9) 0.0203(9) 0.0327(10) -0.0054(7) -0.0029(7) -0.0041(7)
O14 0.0366(10) 0.0397(12) 0.0211(9) 0.0026(8) 0.0055(8) 0.0222(9)
As2 0.01432(11) 0.01365(11) 0.01765(12) -0.00077(8) 0.00021(8) 0.00294(8)
O21 0.0198(9) 0.0339(11) 0.0512(12) 0.0023(9) 0.0026(8) -0.0063(8)
O22 0.0318(9) 0.0138(8) 0.0375(10) -0.0024(7) -0.0088(7) 0.0046(7)
O23 0.0269(9) 0.0289(9) 0.0196(8) -0.0021(7) 0.0046(7) 0.0109(7)
O24 0.0400(11) 0.0426(12) 0.0192(9) -0.0032(8) -0.0061(8) 0.0238(9)
As3 0.01360(11) 0.01458(12) 0.01866(12) -0.00069(9) -0.00169(8) 0.00230(8)
O31 0.0407(10) 0.0163(9) 0.0414(11) -0.0001(8) -0.0071(8) -0.0022(8)
O32 0.0363(10) 0.0259(9) 0.0230(9) 0.0008(7) -0.0069(7) 0.0125(8)
O33 0.0161(8) 0.0333(10) 0.0328(10) -0.0003(8) -0.0027(7) -0.0050(7)
O34 0.0214(9) 0.0584(13) 0.0226(9) -0.0058(9) 0.0000(7) 0.0121(9)
Co1 0.01098(19) 0.0122(2) 0.0179(2) 0.000 0.000 -0.00039(15)
N11 0.0161(9) 0.0217(10) 0.0261(10) 0.0003(8) 0.0006(8) -0.0029(8)
N12 0.0220(10) 0.0160(10) 0.0258(10) -0.0029(8) 0.0003(8) 0.0026(8)
N13 0.0190(10) 0.0231(11) 0.0238(10) 0.0046(8) 0.0001(8) -0.0001(8)
Co2 0.01092(19) 0.0130(2) 0.0201(2) 0.000 0.000 0.00126(15)
N21 0.0164(9) 0.0233(11) 0.0268(11) -0.0016(8) -0.0009(8) 0.0025(8)
N22 0.0202(10) 0.0177(10) 0.0310(11) -0.0005(8) -0.0002(8) 0.0002(8)
N23 0.0185(9) 0.0266(11) 0.0253(11) 0.0007(8) 0.0007(8) 0.0027(8)
Co3 0.01063(14) 0.01224(15) 0.01798(15) 0.00023(11) 0.00103(11) 0.00057(10)
N31 0.0200(10) 0.0227(11) 0.0302(11) -0.0073(9) -0.0020(8) 0.0019(8)
N32 0.0136(9) 0.0201(10) 0.0234(10) 0.0027(8) 0.0004(7) 0.0020(7)
N33 0.0179(10) 0.0204(10) 0.0280(11) 0.0053(8) 0.0017(8) 0.0011(8)
N34 0.0154(9) 0.0189(10) 0.0237(10) 0.0002(8) 0.0011(7) 0.0006(7)
N35 0.0210(10) 0.0192(10) 0.0262(10) -0.0030(8) 0.0023(8) 0.0014(8)
N36 0.0214(10) 0.0230(11) 0.0244(10) 0.0044(8) 0.0009(8) -0.0010(8)
O1W 0.0253(10) 0.0359(12) 0.0367(11) 0.0084(9) -0.0023(8) -0.0036(8)
O2W 0.0278(10) 0.0282(11) 0.0410(11) -0.0033(9) 0.0006(8) 0.0012(8)
O3W 0.0329(11) 0.0251(10) 0.0462(12) 0.0055(9) 0.0123(9) 0.0027(8)
O4W 0.0294(10) 0.0287(11) 0.0488(12) -0.0021(9) -0.0124(9) 0.0009(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O11 As1 O12 112.63(9) . .
O11 As1 O13 112.51(9) . .
O12 As1 O13 112.76(8) . .
O11 As1 O14 108.46(9) . .
O12 As1 O14 103.77(8) . .
O13 As1 O14 106.01(9) . .
As1 O14 H14 111(2) . .
O21 As2 O22 113.50(9) . .
O21 As2 O23 112.53(9) . .
O22 As2 O23 111.51(9) . .
O21 As2 O24 109.44(10) . .
O22 As2 O24 108.14(9) . .
O23 As2 O24 100.88(8) . .
As2 O24 H24 112(2) . .
O31 As3 O32 113.10(9) . .
O31 As3 O33 111.09(9) . .
O32 As3 O33 114.44(9) . .
O31 As3 O34 105.84(10) . .
O32 As3 O34 103.57(8) . .
O33 As3 O34 108.01(8) . .
As3 O34 H34 110(2) . .
N13 Co1 N13 88.91(12) . 2
N13 Co1 N11 91.38(8) . 2
N13 Co1 N11 88.61(8) 2 2
N13 Co1 N11 88.61(8) . .
N13 Co1 N11 91.38(8) 2 .
N11 Co1 N11 179.98(11) 2 .
N13 Co1 N12 90.77(8) . .
N13 Co1 N12 178.94(8) 2 .
N11 Co1 N12 90.39(8) 2 .
N11 Co1 N12 89.63(8) . .
N13 Co1 N12 178.94(8) . 2
N13 Co1 N12 90.77(8) 2 2
N11 Co1 N12 89.63(8) 2 2
N11 Co1 N12 90.39(8) . 2
N12 Co1 N12 89.56(11) . 2
Co1 N11 H111 109.4 . .
Co1 N11 H112 109.5 . .
H111 N11 H112 109.5 . .
Co1 N11 H113 109.5 . .
H111 N11 H113 109.5 . .
H112 N11 H113 109.5 . .
Co1 N12 H121 109.3 . .
Co1 N12 H122 109.6 . .
H121 N12 H122 109.5 . .
Co1 N12 H123 109.5 . .
H121 N12 H123 109.5 . .
H122 N12 H123 109.5 . .
Co1 N13 H131 109.5 . .
Co1 N13 H132 109.6 . .
H131 N13 H132 109.5 . .
Co1 N13 H133 109.3 . .
H131 N13 H133 109.5 . .
H132 N13 H133 109.5 . .
N21 Co2 N21 88.25(11) . 2_565
N21 Co2 N22 90.37(8) . 2_565
N21 Co2 N22 91.57(8) 2_565 2_565
N21 Co2 N22 91.57(8) . .
N21 Co2 N22 90.37(8) 2_565 .
N22 Co2 N22 177.30(12) 2_565 .
N21 Co2 N23 177.95(8) . 2_565
N21 Co2 N23 89.71(8) 2_565 2_565
N22 Co2 N23 89.76(8) 2_565 2_565
N22 Co2 N23 88.37(8) . 2_565
N21 Co2 N23 89.70(8) . .
N21 Co2 N23 177.95(8) 2_565 .
N22 Co2 N23 88.37(8) 2_565 .
N22 Co2 N23 89.76(8) . .
N23 Co2 N23 92.35(11) 2_565 .
Co2 N21 H211 109.5 . .
Co2 N21 H212 109.5 . .
H211 N21 H212 109.5 . .
Co2 N21 H213 109.5 . .
H211 N21 H213 109.5 . .
H212 N21 H213 109.5 . .
Co2 N22 H221 109.4 . .
Co2 N22 H222 109.4 . .
H221 N22 H222 109.5 . .
Co2 N22 H223 109.6 . .
H221 N22 H223 109.5 . .
H222 N22 H223 109.5 . .
Co2 N23 H231 109.5 . .
Co2 N23 H232 109.5 . .
H231 N23 H232 109.5 . .
Co2 N23 H233 109.4 . .
H231 N23 H233 109.5 . .
H232 N23 H233 109.5 . .
N36 Co3 N32 88.10(8) . .
N36 Co3 N35 88.94(8) . .
N32 Co3 N35 90.44(8) . .
N36 Co3 N34 90.67(8) . .
N32 Co3 N34 178.76(8) . .
N35 Co3 N34 89.41(8) . .
N36 Co3 N33 178.43(8) . .
N32 Co3 N33 90.54(8) . .
N35 Co3 N33 90.28(8) . .
N34 Co3 N33 90.69(8) . .
N36 Co3 N31 91.66(8) . .
N32 Co3 N31 89.95(8) . .
N35 Co3 N31 179.30(9) . .
N34 Co3 N31 90.21(8) . .
N33 Co3 N31 89.14(9) . .
Co3 N31 H311 109.4 . .
Co3 N31 H312 109.4 . .
H311 N31 H312 109.5 . .
Co3 N31 H313 109.7 . .
H311 N31 H313 109.5 . .
H312 N31 H313 109.5 . .
Co3 N32 H321 109.7 . .
Co3 N32 H322 109.4 . .
H321 N32 H322 109.5 . .
Co3 N32 H323 109.4 . .
H321 N32 H323 109.5 . .
H322 N32 H323 109.5 . .
Co3 N33 H331 109.4 . .
Co3 N33 H332 109.3 . .
H331 N33 H332 109.5 . .
Co3 N33 H333 109.6 . .
H331 N33 H333 109.5 . .
H332 N33 H333 109.5 . .
Co3 N34 H341 109.6 . .
Co3 N34 H342 109.4 . .
H341 N34 H342 109.5 . .
Co3 N34 H343 109.5 . .
H341 N34 H343 109.5 . .
H342 N34 H343 109.5 . .
Co3 N35 H351 109.4 . .
Co3 N35 H352 109.6 . .
H351 N35 H352 109.5 . .
Co3 N35 H353 109.5 . .
H351 N35 H353 109.5 . .
H352 N35 H353 109.5 . .
Co3 N36 H361 109.4 . .
Co3 N36 H362 109.5 . .
H361 N36 H362 109.5 . .
Co3 N36 H363 109.5 . .
H361 N36 H363 109.5 . .
H362 N36 H363 109.5 . .
H11W O1W H12W 106(3) . .
H21W O2W H22W 109(3) . .
H31W O3W H32W 111(3) . .
H41W O4W H42W 104(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O11 1.6530(16) .
As1 O12 1.6673(16) .
As1 O13 1.6706(16) .
As1 O14 1.7386(17) .
O14 H14 0.816(10) .
As2 O21 1.6601(17) .
As2 O22 1.6676(16) .
As2 O23 1.6813(15) .
As2 O24 1.7271(17) .
O24 H24 0.817(10) .
As3 O31 1.6632(17) .
As3 O32 1.6665(16) .
As3 O33 1.6677(15) .
As3 O34 1.7413(17) .
O34 H34 0.817(10) .
Co1 N13 1.9535(18) .
Co1 N13 1.9535(18) 2
Co1 N11 1.9578(17) 2
Co1 N11 1.9578(17) .
Co1 N12 1.9697(18) .
Co1 N12 1.9698(18) 2
N11 H111 0.8901 .
N11 H112 0.8901 .
N11 H113 0.8900 .
N12 H121 0.8900 .
N12 H122 0.8900 .
N12 H123 0.8900 .
N13 H131 0.8900 .
N13 H132 0.8901 .
N13 H133 0.8901 .
Co2 N21 1.9623(18) .
Co2 N21 1.9623(18) 2_565
Co2 N22 1.9679(19) 2_565
Co2 N22 1.9679(19) .
Co2 N23 1.9727(19) 2_565
Co2 N23 1.9728(19) .
N21 H211 0.8902 .
N21 H212 0.8901 .
N21 H213 0.8901 .
N22 H221 0.8900 .
N22 H222 0.8901 .
N22 H223 0.8900 .
N23 H231 0.8900 .
N23 H232 0.8900 .
N23 H233 0.8900 .
Co3 N36 1.9500(19) .
Co3 N32 1.9580(17) .
Co3 N35 1.9592(19) .
Co3 N34 1.9663(17) .
Co3 N33 1.9726(18) .
Co3 N31 1.9729(19) .
N31 H311 0.8900 .
N31 H312 0.8900 .
N31 H313 0.8900 .
N32 H321 0.8901 .
N32 H322 0.8901 .
N32 H323 0.8900 .
N33 H331 0.8900 .
N33 H332 0.8900 .
N33 H333 0.8900 .
N34 H341 0.8901 .
N34 H342 0.8901 .
N34 H343 0.8901 .
N35 H351 0.8900 .
N35 H352 0.8901 .
N35 H353 0.8902 .
N36 H361 0.8901 .
N36 H362 0.8901 .
N36 H363 0.8901 .
O1W H11W 0.821(10) .
O1W H12W 0.816(10) .
O2W H21W 0.814(10) .
O2W H22W 0.816(10) .
O3W H31W 0.819(10) .
O3W H32W 0.815(10) .
O4W H41W 0.816(10) .
O4W H42W 0.818(10) .
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
O14 H14 O23 0.816(10) 1.798(15) 2.573(2) 158(3) 8_656
O24 H24 O32 0.817(10) 1.793(11) 2.604(2) 171(3) 8_656
O34 H34 O12 0.817(10) 1.783(11) 2.590(2) 169(3) .
N11 H111 O31 0.89 2.02 2.906(3) 176.8 .
N11 H112 O21 0.89 2.28 3.119(3) 157.4 2
N11 H113 O11 0.89 2.09 2.949(3) 162.9 7_565
N12 H121 O21 0.89 2.20 3.087(2) 177.4 .
N12 H122 O2W 0.89 2.07 2.950(3) 172.5 .
N12 H123 O33 0.89 2.21 3.073(3) 164.2 .
N13 H131 O11 0.89 1.97 2.836(3) 164.5 8_655
N13 H133 O2W 0.89 2.05 2.926(3) 168.9 7_565
N21 H211 O3W 0.89 2.16 3.044(3) 174.9 2_565
N21 H212 O22 0.89 1.92 2.813(2) 177.3 2_565
N21 H213 O33 0.89 2.21 3.087(3) 169.2 .
N22 H223 O21 0.89 2.18 3.016(3) 155.9 .
N22 H221 O33 0.89 2.09 2.968(2) 170.2 .
N23 H232 O3W 0.89 2.58 3.095(3) 117.4 8_656
N23 H231 O22 0.89 2.32 3.090(3) 145.4 2_565
N23 H233 O12 0.89 2.26 3.126(3) 163.6 .
N31 H311 O1W 0.89 2.32 3.085(3) 143.9 .
N31 H313 O23 0.89 2.27 3.130(3) 163.2 3_645
N32 H321 O23 0.89 2.14 3.010(3) 164.6 .
N32 H322 O13 0.89 2.06 2.918(2) 162.9 2
N32 H323 O31 0.89 2.07 2.951(3) 168.6 2
N33 H331 O4W 0.89 2.15 2.955(3) 150.2 .
N33 H333 O13 0.89 2.19 3.014(2) 153.2 2
N33 H332 O14 0.89 2.12 2.916(2) 147.9 6_656
N34 H341 O22 0.89 2.24 3.094(3) 160.3 3_645
N34 H342 O14 0.89 2.18 2.985(3) 150.3 6_656
N34 H343 O32 0.89 2.06 2.942(3) 173.6 4_565
N35 H351 O32 0.89 2.11 2.990(2) 170.1 4_565
N35 H352 O1W 0.89 2.29 3.049(3) 143.6 7_566
N35 H353 O24 0.89 2.16 2.970(3) 150.3 .
N36 H361 O23 0.89 2.06 2.936(2) 167.8 .
N36 H362 O1W 0.89 2.21 2.994(3) 146.0 .
N36 H363 O34 0.89 2.07 2.948(3) 166.6 4_565
O1W H11W O31 0.821(10) 1.900(13) 2.695(3) 162(3) 2
O1W H12W O13 0.816(10) 1.915(11) 2.723(3) 170(3) 8_655
O2W H21W O21 0.814(10) 2.003(16) 2.753(3) 153(3) 2
O2W H22W O13 0.816(10) 1.957(11) 2.766(3) 171(3) .
O3W H31W O11 0.819(10) 1.892(11) 2.705(3) 172(3) 8_655
O3W H32W O33 0.815(10) 1.923(11) 2.731(2) 170(3) .
O4W H41W O12 0.816(10) 1.945(11) 2.759(3) 174(3) 6_656
O4W H42W O22 0.818(10) 1.899(11) 2.713(3) 173(3) 5_666
|
1500006.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500006.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_1500006
loop_
_publ_author_name
'Rajni Sharma'
'Raj Pal Sharma'
'Paloth Venugopalan'
'Miguel Quir\'os'
'Juan M. Salas'
'J. Yu'
'Y. Du'
_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
;
Capture of aromatic carboxylate anion through second sphere
coordination: Topological complementarity of
[cis-Co(en)~2~(N~3~)~2~]^+^ and C~7~H~3~ClNO~4~^-^ ions
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 7
_journal_page_last 14
_journal_paper_doi 10.1016/j.molstruc.2007.10.010
_journal_volume 885
_journal_year 2008
_chemical_formula_moiety
'C4 H16 Co N10 1+, C7 H3 Cl N O4 1-, 1.25 (H2 O)'
_chemical_formula_sum 'C11 H21.5 Cl Co N11 O5.25'
_chemical_formula_weight 486.27
_chemical_name_systematic
;
?
;
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 116.426(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 21.9843(18)
_cell_length_b 8.7959(7)
_cell_length_c 23.0121(18)
_cell_measurement_reflns_used 4745
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.8
_cell_measurement_theta_min 2.5
_cell_volume 3984.9(6)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0229
_diffrn_reflns_av_sigmaI/netI 0.0290
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 12363
_diffrn_reflns_theta_full 26.20
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 1.98
_diffrn_standards_decay_% -0.4
_diffrn_standards_number 303
_exptl_absorpt_coefficient_mu 1.047
_exptl_absorpt_correction_T_max 0.842
_exptl_absorpt_correction_T_min 0.643
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.621
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 2004
_exptl_crystal_size_max 0.52
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.17
_refine_diff_density_max 0.390
_refine_diff_density_min -0.335
_refine_diff_density_rms 0.061
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 272
_refine_ls_number_reflns 4486
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.0433
_refine_ls_R_factor_gt 0.0369
_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^)+(0.0500P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0923
_refine_ls_wR_factor_ref 0.0954
_reflns_number_gt 3897
_reflns_number_total 4486
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file coaz2cln.cif
_cod_data_source_block coaz2cln
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C11 H21.50 Cl Co N11 O5.25'
_cod_database_code 1500006
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
Co Co 0.276990(13) 0.17445(3) 0.166986(12) 0.02780(9) Uani 1 1 d .
N1A N 0.28651(9) 0.2738(2) 0.24699(8) 0.0386(4) Uani 1 1 d .
N2A N 0.30508(10) 0.2020(2) 0.29597(9) 0.0391(4) Uani 1 1 d .
N3A N 0.32265(14) 0.1383(3) 0.34470(11) 0.0689(7) Uani 1 1 d .
N4A N 0.18493(9) 0.1023(2) 0.14462(9) 0.0405(4) Uani 1 1 d .
N5A N 0.15640(9) 0.1478(2) 0.17522(9) 0.0391(4) Uani 1 1 d .
N6A N 0.12599(12) 0.1871(3) 0.20236(12) 0.0617(6) Uani 1 1 d .
N1E N 0.36758(8) 0.2516(2) 0.18545(8) 0.0364(4) Uani 1 1 d .
H11E H 0.3969 0.2317 0.2269 0.044 Uiso 1 1 d R
H12E H 0.3827 0.2055 0.1595 0.044 Uiso 1 1 d R
C1E C 0.36305(12) 0.4177(3) 0.17367(12) 0.0476(6) Uani 1 1 d .
H13E H 0.4019 0.4532 0.1681 0.057 Uiso 1 1 d R
H14E H 0.3620 0.4712 0.2101 0.057 Uiso 1 1 d R
C2E C 0.29858(13) 0.4445(3) 0.11311(12) 0.0468(5) Uani 1 1 d .
H23E H 0.2891 0.5525 0.1068 0.056 Uiso 1 1 d R
H24E H 0.3025 0.4047 0.0756 0.056 Uiso 1 1 d R
N2E N 0.24337(9) 0.36496(19) 0.12146(8) 0.0358(4) Uani 1 1 d .
H21E H 0.2084 0.3469 0.0823 0.043 Uiso 1 1 d R
H22E H 0.2283 0.4242 0.1442 0.043 Uiso 1 1 d R
N3E N 0.31430(9) -0.01955(19) 0.20911(8) 0.0357(4) Uani 1 1 d .
H31E H 0.3527 -0.0036 0.2457 0.043 Uiso 1 1 d R
H32E H 0.2843 -0.0668 0.2197 0.043 Uiso 1 1 d R
C3E C 0.32872(13) -0.1153(3) 0.16360(11) 0.0473(6) Uani 1 1 d .
H33E H 0.3310 -0.2215 0.1757 0.057 Uiso 1 1 d R
H34E H 0.3719 -0.0865 0.1649 0.057 Uiso 1 1 d R
C4E C 0.27289(13) -0.0913(2) 0.09736(11) 0.0461(5) Uani 1 1 d .
H43E H 0.2841 -0.1390 0.0654 0.055 Uiso 1 1 d R
H44E H 0.2311 -0.1359 0.0940 0.055 Uiso 1 1 d R
N4E N 0.26433(8) 0.07520(18) 0.08588(8) 0.0321(4) Uani 1 1 d .
H41E H 0.2226 0.0954 0.0542 0.039 Uiso 1 1 d R
H42E H 0.2951 0.1103 0.0734 0.039 Uiso 1 1 d R
C1 C 0.45338(10) 0.2112(2) 0.02527(10) 0.0353(4) Uani 1 1 d .
C11 C 0.40268(11) 0.1703(2) 0.05078(10) 0.0363(5) Uani 1 1 d .
O11 O 0.34149(8) 0.1909(2) 0.01372(8) 0.0492(4) Uani 1 1 d .
O12 O 0.42529(8) 0.1176(2) 0.10672(8) 0.0513(4) Uani 1 1 d .
C2 C 0.50885(11) 0.3067(2) 0.05836(11) 0.0391(5) Uani 1 1 d .
Cl Cl 0.52321(3) 0.38999(8) 0.13175(3) 0.05904(18) Uani 1 1 d .
C3 C 0.55323(12) 0.3447(3) 0.03316(12) 0.0465(6) Uani 1 1 d .
H3 H 0.5895 0.4104 0.0551 0.056 Uiso 1 1 d R
C4 C 0.54224(11) 0.2824(3) -0.02536(12) 0.0455(5) Uani 1 1 d .
N4 N 0.58871(12) 0.3231(3) -0.05341(13) 0.0620(6) Uani 1 1 d .
O41 O 0.57792(14) 0.2700(3) -0.10576(13) 0.0896(8) Uani 1 1 d .
O42 O 0.63402(12) 0.4132(4) -0.02377(12) 0.1150(11) Uani 1 1 d .
C5 C 0.48904(13) 0.1852(3) -0.05979(12) 0.0468(6) Uani 1 1 d .
H5 H 0.4831 0.1437 -0.0991 0.056 Uiso 1 1 d R
C6 C 0.44466(12) 0.1515(3) -0.03387(11) 0.0422(5) Uani 1 1 d .
H6 H 0.4079 0.0878 -0.0567 0.051 Uiso 1 1 d R
O1W O 0.46144(12) 0.0235(4) 0.28964(11) 0.1001(9) Uani 1 1 d D
H11W H 0.4915(16) 0.059(4) 0.3254(11) 0.120 Uiso 1 1 d D
H12W H 0.480(2) -0.057(3) 0.284(2) 0.120 Uiso 1 1 d D
O2W O 0.0000 0.2161(16) 0.2500 0.182(5) Uiso 0.50 2 d SPD
H21W H 0.009(7) 0.1560 0.225(5) 0.218 Uiso 0.50 1 d PD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.02966(15) 0.02983(15) 0.02613(15) -0.00131(10) 0.01441(11) -0.00235(10)
N1A 0.0472(10) 0.0400(10) 0.0315(9) -0.0052(8) 0.0204(8) -0.0018(8)
N2A 0.0459(10) 0.0406(10) 0.0348(10) -0.0079(8) 0.0215(8) -0.0108(8)
N3A 0.100(2) 0.0644(15) 0.0395(12) 0.0041(11) 0.0289(13) -0.0166(13)
N4A 0.0351(9) 0.0518(11) 0.0407(10) -0.0080(8) 0.0223(8) -0.0079(8)
N5A 0.0386(10) 0.0427(10) 0.0376(9) -0.0035(8) 0.0186(9) -0.0086(8)
N6A 0.0567(13) 0.0807(16) 0.0634(14) -0.0257(12) 0.0408(12) -0.0153(11)
N1E 0.0335(9) 0.0419(10) 0.0346(9) -0.0032(8) 0.0157(7) -0.0057(7)
C1E 0.0514(14) 0.0408(12) 0.0570(14) -0.0099(11) 0.0299(12) -0.0163(10)
C2E 0.0652(15) 0.0336(12) 0.0512(13) 0.0033(10) 0.0346(12) -0.0049(10)
N2E 0.0409(10) 0.0360(9) 0.0316(8) 0.0012(7) 0.0172(8) 0.0044(7)
N3E 0.0412(9) 0.0347(9) 0.0331(8) 0.0016(7) 0.0183(8) -0.0005(7)
C3E 0.0631(15) 0.0370(12) 0.0444(12) 0.0003(10) 0.0261(12) 0.0078(10)
C4E 0.0594(15) 0.0366(12) 0.0419(12) -0.0083(9) 0.0220(11) -0.0011(10)
N4E 0.0327(8) 0.0368(9) 0.0287(8) -0.0024(7) 0.0154(7) -0.0034(7)
C1 0.0303(10) 0.0413(11) 0.0352(10) 0.0034(9) 0.0155(9) 0.0036(8)
C11 0.0343(11) 0.0422(11) 0.0352(11) -0.0050(9) 0.0181(9) -0.0025(8)
O11 0.0302(8) 0.0780(12) 0.0408(9) 0.0018(8) 0.0172(7) -0.0009(7)
O12 0.0422(9) 0.0750(12) 0.0413(9) 0.0125(8) 0.0226(8) 0.0034(8)
C2 0.0359(11) 0.0453(12) 0.0371(11) 0.0005(9) 0.0170(9) 0.0005(9)
Cl 0.0606(4) 0.0681(4) 0.0489(3) -0.0177(3) 0.0249(3) -0.0174(3)
C3 0.0350(11) 0.0539(14) 0.0516(14) 0.0060(11) 0.0201(11) -0.0027(10)
C4 0.0378(12) 0.0543(14) 0.0551(14) 0.0149(11) 0.0302(11) 0.0078(10)
N4 0.0525(13) 0.0795(16) 0.0701(16) 0.0187(13) 0.0417(13) 0.0050(11)
O41 0.121(2) 0.0849(16) 0.1154(19) -0.0099(15) 0.1002(18) -0.0064(14)
O42 0.0690(15) 0.206(3) 0.0793(16) 0.0006(19) 0.0413(14) -0.0600(19)
C5 0.0494(13) 0.0556(14) 0.0451(13) 0.0020(11) 0.0298(11) 0.0095(11)
C6 0.0396(12) 0.0496(13) 0.0410(12) -0.0048(10) 0.0211(10) -0.0024(9)
O1W 0.0546(14) 0.172(3) 0.0500(12) -0.0045(16) 0.0019(11) -0.0260(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2E Co N3E 175.93(7)
N2E Co N4A 92.14(8)
N3E Co N4A 90.22(8)
N2E Co N1A 88.74(8)
N3E Co N1A 94.44(7)
N4A Co N1A 93.28(8)
N2E Co N1E 85.65(7)
N3E Co N1E 91.90(7)
N4A Co N1E 177.32(7)
N1A Co N1E 88.20(7)
N2E Co N4E 90.69(7)
N3E Co N4E 86.21(7)
N4A Co N4E 85.03(7)
N1A Co N4E 178.19(7)
N1E Co N4E 93.46(7)
N2A N1A Co 119.92(15)
N3A N2A N1A 176.9(2)
N5A N4A Co 119.07(15)
N6A N5A N4A 176.3(2)
C1E N1E Co 108.80(13)
C1E N1E H11E 110.1
Co N1E H11E 110.0
C1E N1E H12E 109.8
Co N1E H12E 109.9
H11E N1E H12E 108.3
N1E C1E C2E 106.49(17)
N1E C1E H13E 110.5
C2E C1E H13E 110.5
N1E C1E H14E 110.2
C2E C1E H14E 110.5
H13E C1E H14E 108.6
N2E C2E C1E 107.14(18)
N2E C2E H23E 110.4
C1E C2E H23E 110.1
N2E C2E H24E 110.3
C1E C2E H24E 110.4
H23E C2E H24E 108.5
C2E N2E Co 109.86(14)
C2E N2E H21E 109.6
Co N2E H21E 109.7
C2E N2E H22E 109.7
Co N2E H22E 109.7
H21E N2E H22E 108.2
C3E N3E Co 108.65(13)
C3E N3E H31E 110.1
Co N3E H31E 109.9
C3E N3E H32E 109.9
Co N3E H32E 109.9
H31E N3E H32E 108.3
N3E C3E C4E 107.76(19)
N3E C3E H33E 110.1
C4E C3E H33E 110.2
N3E C3E H34E 110.1
C4E C3E H34E 110.2
H33E C3E H34E 108.5
N4E C4E C3E 107.69(18)
N4E C4E H43E 110.3
C3E C4E H43E 110.2
N4E C4E H44E 110.2
C3E C4E H44E 110.1
H43E C4E H44E 108.5
C4E N4E Co 108.42(13)
C4E N4E H41E 110.0
Co N4E H41E 110.1
C4E N4E H42E 110.0
Co N4E H42E 110.0
H41E N4E H42E 108.4
C6 C1 C2 117.9(2)
C6 C1 C11 118.98(19)
C2 C1 C11 123.10(19)
O11 C11 O12 125.1(2)
O11 C11 C1 117.18(19)
O12 C11 C1 117.69(19)
C3 C2 C1 121.8(2)
C3 C2 Cl 116.74(18)
C1 C2 Cl 121.43(17)
C4 C3 C2 117.9(2)
C4 C3 H3 121.0
C2 C3 H3 121.2
C3 C4 C5 123.0(2)
C3 C4 N4 118.6(2)
C5 C4 N4 118.3(2)
O41 N4 O42 123.8(2)
O41 N4 C4 118.3(2)
O42 N4 C4 117.8(3)
C4 C5 C6 117.8(2)
C4 C5 H5 121.2
C6 C5 H5 121.1
C5 C6 C1 121.7(2)
C5 C6 H6 119.1
C1 C6 H6 119.2
H11W O1W H12W 103(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co N2E 1.9397(17)
Co N3E 1.9536(17)
Co N4A 1.9588(17)
Co N1A 1.9632(17)
Co N1E 1.9633(16)
Co N4E 1.9648(16)
N1A N2A 1.194(2)
N2A N3A 1.156(3)
N4A N5A 1.201(3)
N5A N6A 1.152(3)
N1E C1E 1.481(3)
N1E H11E 0.9000
N1E H12E 0.9000
C1E C2E 1.499(3)
C1E H13E 0.9700
C1E H14E 0.9700
C2E N2E 1.485(3)
C2E H23E 0.9700
C2E H24E 0.9700
N2E H21E 0.9000
N2E H22E 0.9000
N3E C3E 1.484(3)
N3E H31E 0.9000
N3E H32E 0.9000
C3E C4E 1.486(3)
C3E H33E 0.9700
C3E H34E 0.9700
C4E N4E 1.485(3)
C4E H43E 0.9700
C4E H44E 0.9700
N4E H41E 0.9000
N4E H42E 0.9000
C1 C6 1.390(3)
C1 C2 1.395(3)
C1 C11 1.516(3)
C11 O11 1.244(3)
C11 O12 1.245(3)
C2 C3 1.380(3)
C2 Cl 1.736(2)
C3 C4 1.372(3)
C3 H3 0.9300
C4 C5 1.379(4)
C4 N4 1.475(3)
N4 O41 1.213(3)
N4 O42 1.217(3)
C5 C6 1.383(3)
C5 H5 0.9300
C6 H6 0.9300
O1W H11W 0.853(10)
O1W H12W 0.849(10)
O2W H21W 0.867(10)
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
N1E H11E O1W 0.90 2.37 3.103(3) 138.4 .
N1E H12E O12 0.90 1.99 2.886(2) 173.7 .
N2E H21E O11 0.90 2.01 2.869(2) 159.1 7
N2E H22E N3A 0.90 2.26 3.082(3) 151.2 4
N3E H31E O1W 0.90 2.15 2.951(3) 147.0 .
N4E H42E O11 0.90 2.16 3.030(2) 161.8 .
N4E H41E O11 0.90 2.45 3.186(2) 139.3 7
N4E H41E O42 0.90 2.54 3.189(3) 129.2 3_445
O1W H11W O12 0.853(10) 1.873(16) 2.700(3) 163(4) 2_655
O2W H21W O41 0.867(10) 2.63(12) 2.984(3) 105(9) 7
|
1500007.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500007.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_1500007
loop_
_publ_author_name
'Raj Pal Sharma'
'Rajni Sharma'
'Ritu Bala'
'Juan M. Salas'
'Miguel Quir\'os'
_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
;
Second sphere coordination complexes via hydrogen bonding:
Synthesis, spectroscopic characterisation of
[trans-Co(en)~2~Cl~2~]CdX~4~ (X = Br or I) and single crystal
X-ray structure determination of [trans-Co(en)~2~Cl~2~]CdBr~4~
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 341
_journal_page_last 347
_journal_paper_doi 10.1016/j.molstruc.2006.02.053
_journal_volume 794
_journal_year 2006
_chemical_formula_moiety '2(C4 H16 Cl2 Co N4 1+), Br4 Cd 2-'
_chemical_formula_sum 'C8 H32 Br4 Cd Cl4 Co2 N8'
_chemical_formula_weight 932.12
_chemical_name_systematic
;
?
;
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 18.6201(10)
_cell_length_b 12.0872(6)
_cell_length_c 24.0877(12)
_cell_measurement_reflns_used 6856
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 24.3
_cell_measurement_theta_min 2.2
_cell_volume 5421.3(5)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0426
_diffrn_reflns_av_sigmaI/netI 0.0387
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 32850
_diffrn_reflns_theta_full 27.40
_diffrn_reflns_theta_max 28.30
_diffrn_reflns_theta_min 2.01
_diffrn_standards_decay_% -0.2
_diffrn_standards_number 500
_exptl_absorpt_coefficient_mu 8.290
_exptl_absorpt_correction_T_max 0.317
_exptl_absorpt_correction_T_min 0.160
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 2.284
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular shape'
_exptl_crystal_F_000 3568
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.18
_refine_diff_density_max 2.699
_refine_diff_density_min -3.820
_refine_diff_density_rms 0.260
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 6320
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.055
_refine_ls_R_factor_all 0.0973
_refine_ls_R_factor_gt 0.0727
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2214
_refine_ls_wR_factor_ref 0.2409
_reflns_number_gt 4613
_reflns_number_total 6320
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cocdbr.cif
_cod_data_source_block cocdbr
_cod_database_code 1500007
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cd Cd 0.48239(4) 0.35833(7) 0.36652(3) 0.0409(2) Uani 1 1 d .
Br1 Br 0.46004(7) 0.33430(10) 0.26096(5) 0.0517(3) Uani 1 1 d .
Br2 Br 0.52225(8) 0.17361(12) 0.40933(6) 0.0651(4) Uani 1 1 d .
Br3 Br 0.56300(8) 0.53104(14) 0.37652(6) 0.0734(5) Uani 1 1 d .
Br4 Br 0.36998(10) 0.41441(16) 0.41834(8) 0.0871(5) Uani 1 1 d .
Co1 Co 0.24397(6) 0.57124(9) 0.27417(4) 0.0246(3) Uani 1 1 d .
Cl1 Cl 0.24939(14) 0.43471(18) 0.21078(9) 0.0394(5) Uani 1 1 d .
Cl2 Cl 0.23680(15) 0.70993(18) 0.33558(9) 0.0407(6) Uani 1 1 d .
N1 N 0.2848(6) 0.6724(6) 0.2200(3) 0.047(2) Uani 1 1 d .
H11 H 0.2655 0.6594 0.1864 0.056 Uiso 1 1 d R
H12 H 0.2745 0.7426 0.2297 0.056 Uiso 1 1 d R
C1 C 0.3631(8) 0.6575(13) 0.2180(6) 0.074(4) Uani 1 1 d .
H13 H 0.3859 0.7249 0.2050 0.088 Uiso 1 1 d R
H14 H 0.3749 0.5984 0.1923 0.088 Uiso 1 1 d R
C2 C 0.3902(8) 0.6301(12) 0.2766(7) 0.070(4) Uani 1 1 d .
H23 H 0.4393 0.6032 0.2754 0.084 Uiso 1 1 d R
H24 H 0.3880 0.6941 0.3009 0.084 Uiso 1 1 d R
N2 N 0.3421(5) 0.5437(7) 0.2954(4) 0.0415(19) Uani 1 1 d .
H21 H 0.3446 0.5386 0.3326 0.050 Uiso 1 1 d R
H22 H 0.3563 0.4784 0.2811 0.050 Uiso 1 1 d R
N3 N 0.2040(4) 0.4709(6) 0.3301(3) 0.0375(18) Uani 1 1 d .
H31 H 0.2277 0.4060 0.3290 0.045 Uiso 1 1 d R
H32 H 0.2102 0.5003 0.3640 0.045 Uiso 1 1 d R
C3 C 0.1280(8) 0.4518(16) 0.3208(9) 0.090(5) Uani 1 1 d .
H33 H 0.1039 0.4402 0.3561 0.108 Uiso 1 1 d R
H34 H 0.1216 0.3860 0.2983 0.108 Uiso 1 1 d R
C4 C 0.0983(8) 0.5511(18) 0.2927(12) 0.123(9) Uani 1 1 d .
H43 H 0.0547 0.5284 0.2739 0.148 Uiso 1 1 d R
H44 H 0.0851 0.6058 0.3204 0.148 Uiso 1 1 d R
N4 N 0.1452(5) 0.5994(8) 0.2524(4) 0.047(2) Uani 1 1 d .
H41 H 0.1372 0.6728 0.2511 0.057 Uiso 1 1 d R
H42 H 0.1369 0.5712 0.2184 0.057 Uiso 1 1 d R
Co2 Co 0.29877(7) 0.15447(10) 0.53301(5) 0.0341(3) Uani 1 1 d .
Cl3 Cl 0.32401(16) 0.0164(2) 0.47297(11) 0.0488(6) Uani 1 1 d .
Cl4 Cl 0.27262(18) 0.2961(2) 0.59096(10) 0.0511(7) Uani 1 1 d .
N5 N 0.2517(4) 0.2375(7) 0.4736(3) 0.0370(17) Uani 1 1 d .
H51 H 0.2760 0.2270 0.4417 0.044 Uiso 1 1 d R
H52 H 0.2535 0.3101 0.4818 0.044 Uiso 1 1 d R
C5 C 0.1771(8) 0.2040(15) 0.4647(8) 0.085(5) Uani 1 1 d .
H53 H 0.1731 0.1584 0.4317 0.102 Uiso 1 1 d R
H54 H 0.1477 0.2694 0.4593 0.102 Uiso 1 1 d R
C6 C 0.1509(8) 0.1442(19) 0.5137(7) 0.097(6) Uani 1 1 d .
H63 H 0.1238 0.1945 0.5371 0.116 Uiso 1 1 d R
H64 H 0.1179 0.0877 0.5008 0.116 Uiso 1 1 d R
N6 N 0.2059(6) 0.0899(8) 0.5475(5) 0.061(3) Uani 1 1 d .
H61 H 0.1949 0.0983 0.5836 0.074 Uiso 1 1 d R
H62 H 0.2071 0.0170 0.5400 0.074 Uiso 1 1 d R
N7 N 0.3469(6) 0.0733(8) 0.5926(4) 0.056(3) Uani 1 1 d .
H71 H 0.3530 0.0023 0.5823 0.067 Uiso 1 1 d R
H72 H 0.3195 0.0742 0.6233 0.067 Uiso 1 1 d R
C7 C 0.4143(8) 0.1229(12) 0.6051(5) 0.064(3) Uani 1 1 d .
H73 H 0.4084 0.1853 0.6300 0.077 Uiso 1 1 d R
H74 H 0.4449 0.0687 0.6231 0.077 Uiso 1 1 d R
C8 C 0.4463(7) 0.1556(12) 0.5533(5) 0.060(3) Uani 1 1 d .
H83 H 0.4871 0.2031 0.5612 0.072 Uiso 1 1 d R
H84 H 0.4635 0.0920 0.5326 0.072 Uiso 1 1 d R
N8 N 0.3932(4) 0.2174(7) 0.5203(3) 0.0402(18) Uani 1 1 d .
H81 H 0.3935 0.2893 0.5299 0.048 Uiso 1 1 d R
H82 H 0.4044 0.2126 0.4840 0.048 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd 0.0383(4) 0.0479(5) 0.0366(4) 0.0101(3) -0.0010(3) 0.0004(3)
Br1 0.0573(7) 0.0512(7) 0.0468(6) 0.0020(5) -0.0023(5) 0.0013(5)
Br2 0.0765(9) 0.0673(8) 0.0514(7) 0.0142(6) 0.0056(6) 0.0268(7)
Br3 0.0711(9) 0.0843(10) 0.0647(8) 0.0161(7) -0.0135(7) -0.0325(8)
Br4 0.0863(11) 0.0855(12) 0.0895(12) 0.0192(9) 0.0140(9) 0.0054(9)
Co1 0.0400(6) 0.0167(5) 0.0172(5) -0.0016(4) 0.0005(4) 0.0056(4)
Cl1 0.0669(15) 0.0223(10) 0.0291(10) -0.0082(8) 0.0088(10) 0.0034(10)
Cl2 0.0698(16) 0.0256(10) 0.0268(10) -0.0100(8) 0.0081(10) -0.0028(10)
N1 0.101(8) 0.018(3) 0.023(4) 0.001(3) 0.005(4) 0.003(4)
C1 0.089(10) 0.075(9) 0.057(8) -0.006(7) 0.039(8) -0.033(8)
C2 0.060(8) 0.058(8) 0.092(11) 0.004(7) -0.003(7) -0.014(6)
N2 0.047(5) 0.035(4) 0.042(5) 0.001(4) 0.004(4) 0.008(4)
N3 0.052(5) 0.024(4) 0.037(4) -0.001(3) 0.011(3) -0.001(3)
C3 0.063(9) 0.094(12) 0.113(14) -0.003(11) 0.027(9) -0.017(9)
C4 0.041(7) 0.105(15) 0.22(3) -0.044(16) -0.019(12) 0.010(9)
N4 0.049(5) 0.040(5) 0.054(5) -0.013(4) -0.016(4) 0.017(4)
Co2 0.0530(8) 0.0257(6) 0.0236(6) 0.0002(4) 0.0144(5) -0.0056(5)
Cl3 0.0654(16) 0.0390(13) 0.0419(13) -0.0142(10) 0.0102(12) 0.0010(12)
Cl4 0.0835(19) 0.0392(13) 0.0307(12) -0.0083(10) 0.0140(12) 0.0022(13)
N5 0.043(4) 0.039(4) 0.029(4) -0.004(3) 0.007(3) -0.004(3)
C5 0.053(7) 0.085(11) 0.116(14) 0.017(10) -0.009(8) -0.019(8)
C6 0.047(7) 0.166(19) 0.078(11) 0.016(11) 0.010(7) -0.033(10)
N6 0.077(7) 0.035(5) 0.073(7) 0.002(5) 0.037(6) -0.016(5)
N7 0.105(9) 0.036(5) 0.028(4) 0.014(4) 0.020(5) 0.009(5)
C7 0.087(10) 0.064(8) 0.041(6) 0.006(6) -0.007(6) 0.016(7)
C8 0.066(8) 0.074(8) 0.039(6) 0.009(5) -0.010(5) 0.009(6)
N8 0.045(4) 0.044(5) 0.032(4) 0.007(3) 0.003(3) -0.003(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Br4 Cd Br2 105.90(6)
Br4 Cd Br3 102.61(7)
Br2 Cd Br3 119.82(6)
Br4 Cd Br1 112.41(6)
Br2 Cd Br1 110.04(5)
Br3 Cd Br1 105.98(5)
N2 Co1 N1 85.2(4)
N2 Co1 N4 179.7(4)
N1 Co1 N4 94.5(4)
N2 Co1 N3 94.1(4)
N1 Co1 N3 178.8(4)
N4 Co1 N3 86.2(4)
N2 Co1 Cl2 90.6(3)
N1 Co1 Cl2 89.8(2)
N4 Co1 Cl2 89.5(3)
N3 Co1 Cl2 89.3(2)
N2 Co1 Cl1 90.6(3)
N1 Co1 Cl1 89.3(2)
N4 Co1 Cl1 89.3(3)
N3 Co1 Cl1 91.7(2)
Cl2 Co1 Cl1 178.41(11)
C1 N1 Co1 109.5(7)
C1 N1 H11 110.1
Co1 N1 H11 109.8
C1 N1 H12 109.5
Co1 N1 H12 109.7
H11 N1 H12 108.2
N1 C1 C2 108.8(10)
N1 C1 H13 110.0
C2 C1 H13 109.4
N1 C1 H14 109.7
C2 C1 H14 110.6
H13 C1 H14 108.4
N2 C2 C1 103.8(11)
N2 C2 H23 110.4
C1 C2 H23 110.8
N2 C2 H24 111.2
C1 C2 H24 111.6
H23 C2 H24 109.0
C2 N2 Co1 112.3(8)
C2 N2 H21 109.2
Co1 N2 H21 109.0
C2 N2 H22 109.4
Co1 N2 H22 109.2
H21 N2 H22 107.8
C3 N3 Co1 111.4(9)
C3 N3 H31 109.6
Co1 N3 H31 109.4
C3 N3 H32 109.1
Co1 N3 H32 109.3
H31 N3 H32 107.9
N3 C3 C4 107.7(13)
N3 C3 H33 109.9
C4 C3 H33 110.0
N3 C3 H34 109.7
C4 C3 H34 111.2
H33 C3 H34 108.3
N4 C4 C3 114.4(13)
N4 C4 H43 108.0
C3 C4 H43 107.2
N4 C4 H44 110.0
C3 C4 H44 109.5
H43 C4 H44 107.6
C4 N4 Co1 108.8(9)
C4 N4 H41 108.9
Co1 N4 H41 109.8
C4 N4 H42 111.1
Co1 N4 H42 109.9
H41 N4 H42 108.4
N6 Co2 N8 178.4(4)
N6 Co2 N5 86.5(4)
N8 Co2 N5 95.1(3)
N6 Co2 N7 94.3(5)
N8 Co2 N7 84.1(4)
N5 Co2 N7 179.1(4)
N6 Co2 Cl3 90.2(3)
N8 Co2 Cl3 90.0(3)
N5 Co2 Cl3 90.2(3)
N7 Co2 Cl3 90.2(3)
N6 Co2 Cl4 90.1(3)
N8 Co2 Cl4 89.8(3)
N5 Co2 Cl4 88.1(2)
N7 Co2 Cl4 91.5(3)
Cl3 Co2 Cl4 178.27(12)
C5 N5 Co2 113.0(8)
C5 N5 H51 108.2
Co2 N5 H51 109.1
C5 N5 H52 109.6
Co2 N5 H52 109.0
H51 N5 H52 107.9
N5 C5 C6 109.5(13)
N5 C5 H53 110.5
C6 C5 H53 110.7
N5 C5 H54 109.3
C6 C5 H54 108.7
H53 C5 H54 108.1
N6 C6 C5 115.9(12)
N6 C6 H63 108.8
C5 C6 H63 109.3
N6 C6 H64 107.8
C5 C6 H64 107.4
H63 C6 H64 107.3
C6 N6 Co2 110.2(8)
C6 N6 H61 109.2
Co2 N6 H61 109.4
C6 N6 H62 110.2
Co2 N6 H62 109.6
H61 N6 H62 108.2
C7 N7 Co2 110.4(7)
C7 N7 H71 110.5
Co2 N7 H71 109.6
C7 N7 H72 108.6
Co2 N7 H72 109.7
H71 N7 H72 108.0
N7 C7 C8 107.2(11)
N7 C7 H73 111.1
C8 C7 H73 111.7
N7 C7 H74 109.2
C8 C7 H74 109.3
H73 C7 H74 108.4
C7 C8 N8 109.3(11)
C7 C8 H83 108.5
N8 C8 H83 109.2
C7 C8 H84 111.4
N8 C8 H84 110.2
H83 C8 H84 108.2
C8 N8 Co2 108.9(7)
C8 N8 H81 110.3
Co2 N8 H81 110.0
C8 N8 H82 109.7
Co2 N8 H82 109.7
H81 N8 H82 108.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cd Br4 2.5295(19)
Cd Br2 2.5689(15)
Cd Br3 2.5824(16)
Cd Br1 2.5930(14)
Co1 N2 1.927(9)
Co1 N1 1.943(8)
Co1 N4 1.943(8)
Co1 N3 1.959(8)
Co1 Cl2 2.240(2)
Co1 Cl1 2.250(2)
N1 C1 1.469(18)
N1 H11 0.9000
N1 H12 0.9000
C1 C2 1.54(2)
C1 H13 0.9700
C1 H14 0.9700
C2 N2 1.448(15)
C2 H23 0.9700
C2 H24 0.9700
N2 H21 0.9000
N2 H22 0.9000
N3 C3 1.450(18)
N3 H31 0.9000
N3 H32 0.9000
C3 C4 1.49(3)
C3 H33 0.9700
C3 H34 0.9700
C4 N4 1.43(3)
C4 H43 0.9700
C4 H44 0.9700
N4 H41 0.9000
N4 H42 0.9000
Co2 N6 1.930(10)
Co2 N8 1.941(8)
Co2 N5 1.955(8)
Co2 N7 1.956(9)
Co2 Cl3 2.258(3)
Co2 Cl4 2.262(3)
N5 C5 1.464(16)
N5 H51 0.9000
N5 H52 0.9000
C5 C6 1.47(2)
C5 H53 0.9700
C5 H54 0.9700
C6 N6 1.46(2)
C6 H63 0.9700
C6 H64 0.9700
N6 H61 0.9000
N6 H62 0.9000
N7 C7 1.423(18)
N7 H71 0.9000
N7 H72 0.9000
C7 C8 1.439(18)
C7 H73 0.9700
C7 H74 0.9700
C8 N8 1.473(14)
C8 H83 0.9700
C8 H84 0.9700
N8 H81 0.9000
N8 H82 0.9000
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
N1 H11 Cl4 0.90 2.47 3.310(9) 156.4 2_564
N1 H12 Cl1 0.90 2.41 3.242(8) 154.1 8_665
N2 H22 Br1 0.90 2.65 3.452(8) 149.5 .
N2 H21 Br4 0.90 2.60 3.389(9) 147.3 .
N3 H31 Cl2 0.90 2.47 3.344(8) 165.2 8_655
N4 H41 Br1 0.90 2.67 3.456(8) 146.0 8_665
N4 H42 Br3 0.90 2.71 3.558(9) 157.1 6_556
N5 H51 Br4 0.90 2.92 3.345(8) 110.9 .
N5 H51 Cl2 0.90 2.58 3.348(8) 144.3 8_655
N6 H61 Br3 0.90 3.07 3.544(9) 115.3 4_456
N7 H72 Cl1 0.90 2.48 3.379(9) 175.8 7_566
N8 H82 Br4 0.90 2.98 3.447(8) 114.4 .
|
1500008.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500008.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_1500008
loop_
_publ_author_name
'Rajni Sharma'
'Raj Pal Sharma'
'Ritu Bala'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
A trinuclear cobalt(III) phosphate complex with a novel molecular structure:
Synthesis and crystal structure of
{[Co(en)~2~]~3~(PO~4~)(HPO~4~)}~2~(H~2~PO~4~)Cl~7~.6H~2~O
;
_journal_name_full 'Inorganic Chemistry Communications'
_journal_page_first 782
_journal_page_last 784
_journal_paper_doi 10.1016/j.inoche.2006.04.001
_journal_volume 9
_journal_year 2006
_chemical_absolute_configuration unk
_chemical_formula_moiety
'2 (C12 H49 Co3 N12 O8 P2 4+), H2 O4 P -1, 7 (Cl 1-), 6 (H2 O)'
_chemical_formula_sum 'C24 H112 Cl7 Co6 N24 O26 P5'
_chemical_formula_weight 1909.96
_chemical_name_systematic
;
?
;
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 109.230(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 12.8349(9)
_cell_length_b 18.7451(13)
_cell_length_c 16.0020(11)
_cell_measurement_reflns_used 5189
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.8
_cell_measurement_theta_min 2.6
_cell_volume 3635.1(4)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0188
_diffrn_reflns_av_sigmaI/netI 0.0421
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 22257
_diffrn_reflns_theta_full 26.90
_diffrn_reflns_theta_max 28.19
_diffrn_reflns_theta_min 1.68
_diffrn_standards_decay_% -0.1
_diffrn_standards_number 687
_exptl_absorpt_coefficient_mu 1.789
_exptl_absorpt_correction_T_max 0.788
_exptl_absorpt_correction_T_min 0.598
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.745
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1976
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.14
_refine_diff_density_max 0.703
_refine_diff_density_min -0.373
_refine_diff_density_rms 0.091
_refine_ls_abs_structure_details
;
The structure has been refined as a twin of the two enantiomers
in identical proportions
;
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 831
_refine_ls_number_reflns 14874
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0457
_refine_ls_R_factor_gt 0.0406
_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^)+(0.0500P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0950
_refine_ls_wR_factor_ref 0.0975
_reflns_number_gt 13711
_reflns_number_total 14874
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cohpo.cif
_cod_data_source_block cohpo
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 1500008
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
Co1 Co 0.93787(5) 0.71491(3) 0.31582(4) 0.02101(13) Uani 1 1 d .
N11 N 1.0416(3) 0.6452(2) 0.2995(2) 0.0228(8) Uani 1 1 d .
H111 H 1.0710 0.6204 0.3500 0.027 Uiso 1 1 d R
H112 H 1.0053 0.6142 0.2568 0.027 Uiso 1 1 d R
C11 C 1.1306(4) 0.6791(3) 0.2753(4) 0.0373(12) Uani 1 1 d .
H113 H 1.1583 0.6467 0.2403 0.045 Uiso 1 1 d R
H114 H 1.1911 0.6923 0.3279 0.045 Uiso 1 1 d R
C12 C 1.0815(4) 0.7442(3) 0.2218(4) 0.0356(12) Uani 1 1 d .
H123 H 1.1392 0.7739 0.2136 0.043 Uiso 1 1 d R
H124 H 1.0311 0.7307 0.1641 0.043 Uiso 1 1 d R
N12 N 1.0225(3) 0.7826(2) 0.2727(3) 0.0299(9) Uani 1 1 d .
H121 H 0.9770 0.8153 0.2379 0.036 Uiso 1 1 d R
H122 H 1.0711 0.8055 0.3185 0.036 Uiso 1 1 d R
N13 N 0.8416(3) 0.7894(2) 0.3354(3) 0.0287(9) Uani 1 1 d .
H131 H 0.8325 0.8238 0.2944 0.034 Uiso 1 1 d R
H132 H 0.7749 0.7707 0.3293 0.034 Uiso 1 1 d R
C13 C 0.8886(5) 0.8207(3) 0.4242(4) 0.0425(14) Uani 1 1 d .
H133 H 0.8302 0.8392 0.4442 0.051 Uiso 1 1 d R
H134 H 0.9381 0.8595 0.4232 0.051 Uiso 1 1 d R
C14 C 0.9508(5) 0.7623(3) 0.4851(4) 0.0436(14) Uani 1 1 d .
H143 H 0.9951 0.7819 0.5418 0.052 Uiso 1 1 d R
H144 H 0.9001 0.7274 0.4949 0.052 Uiso 1 1 d R
N14 N 1.0226(3) 0.7292(2) 0.4393(3) 0.0307(9) Uani 1 1 d .
H141 H 1.0483 0.6871 0.4647 0.037 Uiso 1 1 d R
H142 H 1.0806 0.7578 0.4441 0.037 Uiso 1 1 d R
Co2 Co 0.80597(5) 0.49271(3) 0.22232(4) 0.01842(12) Uani 1 1 d .
N21 N 0.8797(3) 0.4366(2) 0.1573(3) 0.0270(9) Uani 1 1 d .
H211 H 0.9465 0.4553 0.1642 0.032 Uiso 1 1 d R
H212 H 0.8893 0.3917 0.1785 0.032 Uiso 1 1 d R
C21 C 0.8134(5) 0.4360(3) 0.0639(4) 0.0402(13) Uani 1 1 d .
H213 H 0.8356 0.3965 0.0342 0.048 Uiso 1 1 d R
H214 H 0.8234 0.4801 0.0358 0.048 Uiso 1 1 d R
C22 C 0.6947(4) 0.4274(3) 0.0587(4) 0.0399(13) Uani 1 1 d .
H223 H 0.6461 0.4356 -0.0013 0.048 Uiso 1 1 d R
H224 H 0.6814 0.3797 0.0765 0.048 Uiso 1 1 d R
N22 N 0.6749(3) 0.4811(2) 0.1197(2) 0.0260(8) Uani 1 1 d .
H221 H 0.6182 0.4671 0.1370 0.031 Uiso 1 1 d R
H222 H 0.6568 0.5231 0.0914 0.031 Uiso 1 1 d R
N23 N 0.9396(3) 0.4987(2) 0.3265(2) 0.0243(8) Uani 1 1 d .
H231 H 0.9994 0.5003 0.3091 0.029 Uiso 1 1 d R
H232 H 0.9379 0.5392 0.3564 0.029 Uiso 1 1 d R
C23 C 0.9482(4) 0.4372(3) 0.3853(3) 0.0299(11) Uani 1 1 d .
H233 H 0.9889 0.4501 0.4461 0.036 Uiso 1 1 d R
H234 H 0.9866 0.3983 0.3680 0.036 Uiso 1 1 d R
C24 C 0.8337(4) 0.4154(3) 0.3776(3) 0.0342(11) Uani 1 1 d .
H243 H 0.8345 0.3699 0.4066 0.041 Uiso 1 1 d R
H244 H 0.7996 0.4506 0.4048 0.041 Uiso 1 1 d R
N24 N 0.7717(3) 0.4097(2) 0.2813(3) 0.0259(8) Uani 1 1 d .
H241 H 0.6987 0.4077 0.2722 0.031 Uiso 1 1 d R
H242 H 0.7915 0.3697 0.2593 0.031 Uiso 1 1 d R
Co3 Co 0.56979(5) 0.68795(3) 0.16017(4) 0.02321(13) Uani 1 1 d .
N31 N 0.6313(3) 0.7824(2) 0.1522(3) 0.0320(9) Uani 1 1 d .
H311 H 0.6283 0.8095 0.1978 0.038 Uiso 1 1 d R
H312 H 0.7026 0.7778 0.1563 0.038 Uiso 1 1 d R
C31 C 0.5701(6) 0.8180(3) 0.0679(4) 0.0505(16) Uani 1 1 d .
H313 H 0.6182 0.8503 0.0502 0.061 Uiso 1 1 d R
H314 H 0.5087 0.8451 0.0741 0.061 Uiso 1 1 d R
C32 C 0.5292(5) 0.7598(3) 0.0005(4) 0.0469(15) Uani 1 1 d .
H323 H 0.4756 0.7790 -0.0527 0.056 Uiso 1 1 d R
H324 H 0.5901 0.7399 -0.0150 0.056 Uiso 1 1 d R
N32 N 0.4776(3) 0.7041(3) 0.0385(3) 0.0343(10) Uani 1 1 d .
H321 H 0.4712 0.6635 0.0072 0.041 Uiso 1 1 d R
H322 H 0.4098 0.7179 0.0366 0.041 Uiso 1 1 d R
N33 N 0.4617(3) 0.7268(3) 0.2092(3) 0.0340(10) Uani 1 1 d .
H331 H 0.4934 0.7603 0.2499 0.041 Uiso 1 1 d R
H332 H 0.4062 0.7473 0.1659 0.041 Uiso 1 1 d R
C33 C 0.4191(5) 0.6699(4) 0.2490(4) 0.0517(16) Uani 1 1 d .
H333 H 0.3509 0.6846 0.2576 0.062 Uiso 1 1 d R
H334 H 0.4720 0.6577 0.3061 0.062 Uiso 1 1 d R
C34 C 0.3988(5) 0.6060(4) 0.1878(5) 0.0535(17) Uani 1 1 d .
H343 H 0.3846 0.5637 0.2172 0.064 Uiso 1 1 d R
H344 H 0.3355 0.6147 0.1354 0.064 Uiso 1 1 d R
N34 N 0.4996(3) 0.5966(2) 0.1627(3) 0.0319(9) Uani 1 1 d .
H341 H 0.4819 0.5758 0.1091 0.038 Uiso 1 1 d R
H342 H 0.5471 0.5678 0.2023 0.038 Uiso 1 1 d R
Co4 Co 0.46923(5) 0.62889(3) 0.64692(4) 0.02028(13) Uani 1 1 d .
N41 N 0.3657(3) 0.6526(2) 0.5330(2) 0.0277(9) Uani 1 1 d .
H411 H 0.2965 0.6424 0.5314 0.033 Uiso 1 1 d R
H412 H 0.3695 0.6995 0.5224 0.033 Uiso 1 1 d R
C41 C 0.3942(5) 0.6102(3) 0.4651(3) 0.0366(12) Uani 1 1 d .
H413 H 0.4596 0.6295 0.4557 0.044 Uiso 1 1 d R
H414 H 0.3339 0.6110 0.4093 0.044 Uiso 1 1 d R
C42 C 0.4154(4) 0.5358(3) 0.5001(3) 0.0396(13) Uani 1 1 d .
H423 H 0.3471 0.5139 0.5004 0.048 Uiso 1 1 d R
H424 H 0.4462 0.5073 0.4634 0.048 Uiso 1 1 d R
N42 N 0.4946(3) 0.5407(2) 0.5914(2) 0.0271(8) Uani 1 1 d .
H421 H 0.5641 0.5400 0.5901 0.033 Uiso 1 1 d R
H422 H 0.4857 0.5031 0.6233 0.033 Uiso 1 1 d R
N43 N 0.3563(3) 0.5840(2) 0.6863(3) 0.0308(9) Uani 1 1 d .
H431 H 0.3000 0.5691 0.6392 0.037 Uiso 1 1 d R
H432 H 0.3848 0.5459 0.7204 0.037 Uiso 1 1 d R
C43 C 0.3173(8) 0.6356(5) 0.7363(7) 0.102(4) Uani 1 1 d .
H433 H 0.2375 0.6367 0.7113 0.122 Uiso 1 1 d R
H434 H 0.3354 0.6175 0.7962 0.122 Uiso 1 1 d R
C44 C 0.3530(8) 0.7009(4) 0.7433(7) 0.094(3) Uani 1 1 d .
H443 H 0.3824 0.7138 0.8054 0.113 Uiso 1 1 d R
H444 H 0.2901 0.7315 0.7160 0.113 Uiso 1 1 d R
N44 N 0.4361(3) 0.7162(2) 0.7007(3) 0.0283(8) Uani 1 1 d .
H441 H 0.4977 0.7323 0.7420 0.034 Uiso 1 1 d R
H442 H 0.4117 0.7502 0.6591 0.034 Uiso 1 1 d R
Co5 Co 0.82977(5) 0.54767(3) 0.73755(4) 0.02124(13) Uani 1 1 d .
N51 N 0.7170(3) 0.4779(2) 0.7402(3) 0.0283(9) Uani 1 1 d .
H511 H 0.6532 0.5005 0.7347 0.034 Uiso 1 1 d R
H512 H 0.7050 0.4474 0.6945 0.034 Uiso 1 1 d R
C51 C 0.7542(5) 0.4379(3) 0.8241(4) 0.0497(16) Uani 1 1 d .
H513 H 0.7363 0.4642 0.8698 0.060 Uiso 1 1 d R
H514 H 0.7181 0.3918 0.8170 0.060 Uiso 1 1 d R
C52 C 0.8742(5) 0.4292(3) 0.8487(4) 0.0469(15) Uani 1 1 d .
H523 H 0.8907 0.3946 0.8096 0.056 Uiso 1 1 d R
H524 H 0.9038 0.4113 0.9088 0.056 Uiso 1 1 d R
N52 N 0.9260(3) 0.4983(2) 0.8411(3) 0.0306(9) Uani 1 1 d .
H521 H 0.9928 0.4912 0.8356 0.037 Uiso 1 1 d R
H522 H 0.9348 0.5246 0.8901 0.037 Uiso 1 1 d R
N53 N 0.9463(3) 0.6148(2) 0.7372(3) 0.0263(8) Uani 1 1 d .
H531 H 0.9159 0.6571 0.7160 0.032 Uiso 1 1 d R
H532 H 0.9912 0.6215 0.7932 0.032 Uiso 1 1 d R
C53 C 1.0115(5) 0.5891(3) 0.6827(4) 0.0449(15) Uani 1 1 d .
H533 H 1.0768 0.5644 0.7196 0.054 Uiso 1 1 d R
H534 H 1.0346 0.6288 0.6542 0.054 Uiso 1 1 d R
C54 C 0.9407(5) 0.5390(3) 0.6149(4) 0.0436(14) Uani 1 1 d .
H543 H 0.8876 0.5658 0.5682 0.052 Uiso 1 1 d R
H544 H 0.9856 0.5109 0.5888 0.052 Uiso 1 1 d R
N54 N 0.8829(4) 0.4920(2) 0.6582(3) 0.0328(9) Uani 1 1 d .
H541 H 0.9294 0.4581 0.6890 0.039 Uiso 1 1 d R
H542 H 0.8259 0.4704 0.6174 0.039 Uiso 1 1 d R
Co6 Co 0.75781(5) 0.78287(3) 0.76504(4) 0.01924(12) Uani 1 1 d .
N61 N 0.8960(3) 0.7486(2) 0.8527(3) 0.0253(8) Uani 1 1 d .
H611 H 0.8869 0.7035 0.8684 0.030 Uiso 1 1 d R
H612 H 0.9504 0.7488 0.8288 0.030 Uiso 1 1 d R
C61 C 0.9272(5) 0.7949(3) 0.9322(4) 0.0432(14) Uani 1 1 d .
H613 H 0.9722 0.8344 0.9246 0.052 Uiso 1 1 d R
H614 H 0.9694 0.7680 0.9840 0.052 Uiso 1 1 d R
C62 C 0.8227(5) 0.8223(3) 0.9434(3) 0.0421(14) Uani 1 1 d .
H623 H 0.7847 0.7842 0.9625 0.050 Uiso 1 1 d R
H624 H 0.8394 0.8599 0.9875 0.050 Uiso 1 1 d R
N62 N 0.7529(3) 0.8500(2) 0.8564(3) 0.0259(8) Uani 1 1 d .
H621 H 0.7782 0.8928 0.8464 0.031 Uiso 1 1 d R
H622 H 0.6830 0.8554 0.8557 0.031 Uiso 1 1 d R
N63 N 0.8363(3) 0.8477(2) 0.7124(3) 0.0273(9) Uani 1 1 d .
H631 H 0.8568 0.8869 0.7462 0.033 Uiso 1 1 d R
H632 H 0.8974 0.8263 0.7087 0.033 Uiso 1 1 d R
C63 C 0.7624(4) 0.8677(3) 0.6222(3) 0.0319(11) Uani 1 1 d .
H633 H 0.7586 0.8294 0.5806 0.038 Uiso 1 1 d R
H634 H 0.7896 0.9103 0.6018 0.038 Uiso 1 1 d R
C64 C 0.6499(4) 0.8818(3) 0.6300(4) 0.0345(12) Uani 1 1 d .
H643 H 0.6500 0.9265 0.6607 0.041 Uiso 1 1 d R
H644 H 0.5948 0.8848 0.5716 0.041 Uiso 1 1 d R
N64 N 0.6237(3) 0.82245(19) 0.6796(2) 0.0220(8) Uani 1 1 d .
H641 H 0.5885 0.7879 0.6417 0.026 Uiso 1 1 d R
H642 H 0.5784 0.8379 0.7083 0.026 Uiso 1 1 d R
P1 P 0.79623(9) 0.64537(6) 0.13219(7) 0.0180(2) Uani 1 1 d .
O11 O 0.8447(2) 0.70793(16) 0.19390(19) 0.0219(6) Uani 1 1 d .
O12 O 0.8531(2) 0.57532(16) 0.17234(19) 0.0204(6) Uani 1 1 d .
O13 O 0.6705(2) 0.64092(18) 0.11171(19) 0.0236(7) Uani 1 1 d .
O14 O 0.8193(3) 0.65775(18) 0.0448(2) 0.0256(7) Uani 1 1 d .
P2 P 0.74166(9) 0.61742(6) 0.33019(7) 0.0182(2) Uani 1 1 d .
O21 O 0.8623(2) 0.64050(17) 0.35800(19) 0.0230(6) Uani 1 1 d .
O22 O 0.7197(2) 0.54830(17) 0.27666(19) 0.0219(6) Uani 1 1 d .
O23 O 0.6659(2) 0.67756(17) 0.28169(19) 0.0238(7) Uani 1 1 d .
O24 O 0.7131(3) 0.59775(18) 0.4149(2) 0.0294(7) Uani 1 1 d .
P3 P 0.69338(9) 0.66786(6) 0.61092(7) 0.0186(2) Uani 1 1 d .
O31 O 0.5746(2) 0.68093(17) 0.60867(19) 0.0230(6) Uani 1 1 d .
O32 O 0.7264(3) 0.58960(17) 0.6321(2) 0.0234(7) Uani 1 1 d .
O33 O 0.7742(2) 0.71678(16) 0.6792(2) 0.0226(6) Uani 1 1 d .
O34 O 0.6998(3) 0.68754(18) 0.5193(2) 0.0313(7) Uani 1 1 d .
P4 P 0.67627(9) 0.63694(6) 0.82241(7) 0.0185(2) Uani 1 1 d .
O41 O 0.5778(2) 0.59865(16) 0.75616(19) 0.0213(6) Uani 1 1 d .
O42 O 0.7866(2) 0.60730(16) 0.8196(2) 0.0223(6) Uani 1 1 d .
O43 O 0.6712(2) 0.71824(17) 0.8109(2) 0.0225(6) Uani 1 1 d .
O44 O 0.6672(3) 0.61911(19) 0.9146(2) 0.0284(7) Uani 1 1 d .
P5 P 0.70243(11) 0.33928(7) 0.53936(9) 0.0328(3) Uani 1 1 d .
O51 O 0.6496(4) 0.3072(3) 0.4509(3) 0.0627(13) Uani 1 1 d .
O52 O 0.8249(3) 0.3411(2) 0.5729(3) 0.0513(11) Uani 1 1 d .
O53 O 0.6575(4) 0.4181(2) 0.5403(3) 0.0531(11) Uani 1 1 d .
O54 O 0.6662(4) 0.2998(3) 0.6122(3) 0.0645(14) Uani 1 1 d .
Cl1 Cl 1.08192(11) 0.77628(7) 0.75021(10) 0.0400(3) Uani 1 1 d .
Cl2 Cl 0.86908(12) 1.00097(7) 0.79796(11) 0.0468(3) Uani 1 1 d .
Cl3 Cl 0.4280(2) 0.39898(10) 0.70214(14) 0.0741(6) Uani 1 1 d .
Cl4 Cl 1.13611(11) 0.57154(8) 0.50144(9) 0.0434(3) Uani 1 1 d .
Cl5 Cl 0.49506(12) 0.89782(10) 0.80146(10) 0.0533(4) Uani 1 1 d .
Cl6 Cl 0.24180(12) 0.76611(9) 0.05009(11) 0.0541(4) Uani 1 1 d .
Cl7 Cl 0.86782(14) 0.91740(10) 0.19712(15) 0.0688(5) Uani 1 1 d .
O1W O 0.5727(3) 0.4834(2) 0.3860(3) 0.0514(11) Uani 1 1 d .
O2W O 0.9844(4) 0.5753(3) 0.0190(3) 0.0559(12) Uani 1 1 d .
O3W O 1.1061(4) 0.6348(3) 0.9221(3) 0.0720(14) Uani 1 1 d .
O4W O 0.5463(4) 0.7856(3) 0.4256(4) 0.0768(16) Uani 1 1 d .
O5W O 0.4963(6) 0.5656(4) 0.9673(5) 0.0622(18) Uiso 0.70 1 d P
O6W O 0.3637(8) 0.4817(6) 0.8379(7) 0.065(3) Uiso 0.50 1 d P
O7W O 0.5183(13) 0.4924(10) 0.8772(11) 0.058(4) Uiso 0.28 1 d P
O8W O 0.4188(17) 0.5457(12) 0.9854(13) 0.079(5) Uiso 0.28 1 d P
O9W O 0.227(2) 0.5041(14) 0.9757(16) 0.083(7) Uiso 0.24 1 d P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0198(3) 0.0242(3) 0.0175(3) -0.0028(2) 0.0042(2) -0.0034(2)
N11 0.0205(18) 0.025(2) 0.0222(19) 0.0008(15) 0.0054(15) -0.0019(15)
C11 0.027(3) 0.033(3) 0.058(3) -0.001(2) 0.023(2) -0.004(2)
C12 0.034(3) 0.033(3) 0.046(3) -0.001(2) 0.022(2) -0.006(2)
N12 0.031(2) 0.026(2) 0.032(2) -0.0017(18) 0.0108(18) -0.0064(18)
N13 0.030(2) 0.029(2) 0.026(2) -0.0037(17) 0.0073(17) -0.0050(17)
C13 0.047(3) 0.048(4) 0.032(3) -0.018(2) 0.013(3) -0.005(3)
C14 0.040(3) 0.063(4) 0.027(3) -0.018(3) 0.011(2) -0.011(3)
N14 0.027(2) 0.037(2) 0.022(2) -0.0039(17) 0.0010(17) -0.0075(17)
Co2 0.0192(3) 0.0196(3) 0.0172(3) -0.0008(2) 0.0070(2) -0.0005(2)
N21 0.023(2) 0.026(2) 0.035(2) -0.0021(17) 0.0151(18) 0.0002(16)
C21 0.044(3) 0.047(3) 0.032(3) -0.016(2) 0.017(3) -0.003(3)
C22 0.033(3) 0.054(4) 0.032(3) -0.017(2) 0.010(2) -0.006(2)
N22 0.025(2) 0.030(2) 0.023(2) -0.0028(16) 0.0077(16) -0.0057(16)
N23 0.0248(19) 0.025(2) 0.0240(19) 0.0012(16) 0.0095(16) 0.0008(16)
C23 0.036(3) 0.030(3) 0.017(2) 0.0020(19) 0.000(2) 0.003(2)
C24 0.043(3) 0.032(3) 0.030(3) 0.009(2) 0.015(2) 0.002(2)
N24 0.0226(19) 0.024(2) 0.034(2) 0.0008(16) 0.0128(17) 0.0004(15)
Co3 0.0190(3) 0.0311(3) 0.0188(3) 0.0006(2) 0.0053(2) 0.0043(2)
N31 0.033(2) 0.033(2) 0.030(2) 0.0017(18) 0.0095(18) 0.0048(18)
C31 0.059(4) 0.041(3) 0.045(4) 0.014(3) 0.010(3) 0.014(3)
C32 0.044(3) 0.058(4) 0.034(3) 0.019(3) 0.006(3) 0.015(3)
N32 0.030(2) 0.048(3) 0.022(2) 0.0018(18) 0.0044(17) 0.0107(19)
N33 0.028(2) 0.048(3) 0.027(2) -0.0039(19) 0.0117(18) 0.0091(19)
C33 0.047(3) 0.070(4) 0.052(4) 0.008(3) 0.034(3) 0.008(3)
C34 0.030(3) 0.060(4) 0.079(5) 0.005(4) 0.028(3) -0.004(3)
N34 0.029(2) 0.038(2) 0.030(2) -0.0022(18) 0.0113(18) 0.0001(18)
Co4 0.0185(3) 0.0238(3) 0.0165(3) -0.0001(2) 0.0031(2) -0.0017(2)
N41 0.027(2) 0.030(2) 0.022(2) 0.0023(16) 0.0018(16) -0.0028(16)
C41 0.038(3) 0.051(3) 0.018(2) -0.002(2) 0.005(2) 0.000(2)
C42 0.034(3) 0.053(4) 0.027(3) -0.017(2) 0.004(2) -0.004(3)
N42 0.028(2) 0.024(2) 0.027(2) -0.0058(16) 0.0071(17) -0.0035(16)
N43 0.029(2) 0.035(2) 0.025(2) 0.0046(17) 0.0040(17) -0.0067(18)
C43 0.126(8) 0.085(6) 0.151(9) -0.055(6) 0.122(8) -0.053(6)
C44 0.111(7) 0.062(5) 0.164(9) -0.022(5) 0.120(7) -0.019(5)
N44 0.025(2) 0.034(2) 0.027(2) -0.0026(18) 0.0094(17) 0.0008(17)
Co5 0.0221(3) 0.0201(3) 0.0227(3) -0.0004(2) 0.0089(2) 0.0020(2)
N51 0.032(2) 0.024(2) 0.030(2) 0.0018(16) 0.0113(18) -0.0011(17)
C51 0.046(3) 0.045(4) 0.058(4) 0.024(3) 0.017(3) -0.002(3)
C52 0.053(4) 0.042(3) 0.044(3) 0.019(3) 0.014(3) 0.008(3)
N52 0.029(2) 0.036(2) 0.028(2) 0.0051(18) 0.0114(17) 0.0088(18)
N53 0.025(2) 0.026(2) 0.027(2) -0.0021(16) 0.0081(16) 0.0024(16)
C53 0.040(3) 0.047(4) 0.061(4) -0.009(3) 0.035(3) -0.008(3)
C54 0.052(3) 0.041(3) 0.051(3) -0.008(3) 0.034(3) -0.003(3)
N54 0.039(2) 0.024(2) 0.040(2) -0.0061(18) 0.020(2) -0.0003(18)
Co6 0.0193(3) 0.0186(3) 0.0201(3) -0.0029(2) 0.0068(2) -0.0004(2)
N61 0.0228(19) 0.025(2) 0.026(2) -0.0029(16) 0.0053(16) 0.0003(15)
C61 0.035(3) 0.048(4) 0.036(3) -0.006(2) -0.002(2) 0.003(3)
C62 0.047(3) 0.050(4) 0.025(3) -0.013(2) 0.005(2) -0.001(3)
N62 0.025(2) 0.025(2) 0.029(2) -0.0056(16) 0.0101(17) 0.0006(16)
N63 0.030(2) 0.021(2) 0.034(2) -0.0020(16) 0.0152(18) -0.0039(16)
C63 0.034(3) 0.035(3) 0.030(3) 0.003(2) 0.015(2) -0.002(2)
C64 0.034(3) 0.026(3) 0.038(3) 0.008(2) 0.006(2) 0.001(2)
N64 0.0229(19) 0.0192(19) 0.0233(19) -0.0012(14) 0.0069(15) 0.0004(14)
P1 0.0181(5) 0.0226(6) 0.0131(5) 0.0000(4) 0.0047(4) -0.0001(4)
O11 0.0250(15) 0.0192(15) 0.0188(15) -0.0014(12) 0.0035(12) 0.0007(12)
O12 0.0181(15) 0.0235(16) 0.0196(15) 0.0029(12) 0.0061(12) -0.0018(12)
O13 0.0192(15) 0.0326(18) 0.0189(15) 0.0011(13) 0.0061(12) 0.0040(13)
O14 0.0239(16) 0.0375(19) 0.0150(15) 0.0025(13) 0.0057(12) 0.0001(13)
P2 0.0205(5) 0.0217(6) 0.0131(5) -0.0010(4) 0.0065(4) -0.0003(4)
O21 0.0228(16) 0.0256(16) 0.0182(15) 0.0009(12) 0.0034(12) -0.0027(13)
O22 0.0191(15) 0.0264(16) 0.0212(15) -0.0026(13) 0.0080(12) -0.0006(13)
O23 0.0229(15) 0.0270(17) 0.0197(15) -0.0019(13) 0.0047(12) 0.0020(13)
O24 0.041(2) 0.0311(18) 0.0206(16) -0.0008(13) 0.0157(15) -0.0038(15)
P3 0.0231(5) 0.0185(5) 0.0147(5) -0.0016(4) 0.0071(4) 0.0001(4)
O31 0.0245(16) 0.0227(16) 0.0207(15) -0.0019(13) 0.0061(13) 0.0004(13)
O32 0.0273(17) 0.0230(16) 0.0214(16) -0.0014(12) 0.0100(13) 0.0016(13)
O33 0.0207(15) 0.0204(15) 0.0275(17) -0.0033(13) 0.0090(13) -0.0037(12)
O34 0.047(2) 0.0288(18) 0.0241(17) -0.0018(14) 0.0199(16) -0.0007(16)
P4 0.0183(5) 0.0230(6) 0.0136(5) -0.0007(4) 0.0045(4) 0.0004(4)
O41 0.0210(15) 0.0228(16) 0.0159(15) -0.0009(12) 0.0005(12) -0.0036(12)
O42 0.0215(15) 0.0230(16) 0.0220(16) -0.0013(12) 0.0065(12) 0.0030(12)
O43 0.0190(15) 0.0235(16) 0.0263(16) -0.0010(13) 0.0091(13) -0.0011(13)
O44 0.0260(17) 0.042(2) 0.0166(15) 0.0025(14) 0.0067(13) -0.0029(14)
P5 0.0318(7) 0.0308(7) 0.0323(7) -0.0005(5) 0.0059(6) 0.0015(6)
O51 0.082(3) 0.054(3) 0.046(3) -0.017(2) 0.012(2) -0.015(2)
O52 0.032(2) 0.060(3) 0.055(3) 0.017(2) 0.0039(19) 0.0065(19)
O53 0.051(3) 0.041(2) 0.061(3) -0.010(2) 0.010(2) 0.0101(19)
O54 0.055(3) 0.079(4) 0.061(3) 0.033(3) 0.021(2) 0.009(2)
Cl1 0.0378(7) 0.0290(6) 0.0592(9) -0.0012(6) 0.0244(6) -0.0035(5)
Cl2 0.0395(7) 0.0296(7) 0.0727(10) -0.0101(6) 0.0200(7) -0.0055(6)
Cl3 0.1124(17) 0.0512(10) 0.0772(13) 0.0016(9) 0.0565(13) -0.0054(10)
Cl4 0.0281(6) 0.0591(9) 0.0346(7) 0.0091(6) -0.0013(5) -0.0111(6)
Cl5 0.0332(7) 0.0773(11) 0.0507(9) -0.0104(8) 0.0153(7) 0.0187(7)
Cl6 0.0336(7) 0.0543(9) 0.0640(10) 0.0060(8) 0.0021(7) 0.0095(6)
Cl7 0.0449(9) 0.0484(9) 0.1153(16) 0.0318(10) 0.0294(10) 0.0009(7)
O1W 0.047(2) 0.047(3) 0.068(3) 0.013(2) 0.029(2) -0.003(2)
O2W 0.048(3) 0.073(3) 0.047(3) 0.001(2) 0.017(2) 0.011(2)
O3W 0.068(3) 0.077(4) 0.059(3) -0.002(3) 0.006(3) -0.013(3)
O4W 0.053(3) 0.088(4) 0.091(4) 0.036(3) 0.026(3) 0.026(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O11 Co1 N14 174.58(16)
O11 Co1 N12 85.27(15)
N14 Co1 N12 94.63(17)
O11 Co1 O21 95.08(13)
N14 Co1 O21 85.50(15)
N12 Co1 O21 174.82(16)
O11 Co1 N11 92.43(14)
N14 Co1 N11 92.96(17)
N12 Co1 N11 84.47(17)
O21 Co1 N11 90.35(14)
O11 Co1 N13 89.81(15)
N14 Co1 N13 84.78(17)
N12 Co1 N13 92.72(18)
O21 Co1 N13 92.45(15)
N11 Co1 N13 176.25(17)
C11 N11 Co1 111.8(3)
C11 N11 H111 109.1
Co1 N11 H111 109.3
C11 N11 H112 109.5
Co1 N11 H112 109.2
H111 N11 H112 107.9
N11 C11 C12 106.6(4)
N11 C11 H113 110.2
C12 C11 H113 110.1
N11 C11 H114 110.6
C12 C11 H114 110.7
H113 C11 H114 108.6
N12 C12 C11 106.1(4)
N12 C12 H123 110.4
C11 C12 H123 110.3
N12 C12 H124 110.5
C11 C12 H124 110.8
H123 C12 H124 108.6
C12 N12 Co1 109.1(3)
C12 N12 H121 109.8
Co1 N12 H121 109.8
C12 N12 H122 109.9
Co1 N12 H122 109.9
H121 N12 H122 108.3
C13 N13 Co1 111.1(3)
C13 N13 H131 109.5
Co1 N13 H131 109.3
C13 N13 H132 109.4
Co1 N13 H132 109.4
H131 N13 H132 108.0
N13 C13 C14 107.3(4)
N13 C13 H133 110.2
C14 C13 H133 110.4
N13 C13 H134 110.2
C14 C13 H134 110.2
H133 C13 H134 108.5
N14 C14 C13 105.4(4)
N14 C14 H143 110.5
C13 C14 H143 110.7
N14 C14 H144 110.8
C13 C14 H144 110.6
H143 C14 H144 108.8
C14 N14 Co1 109.3(3)
C14 N14 H141 109.8
Co1 N14 H141 109.8
C14 N14 H142 109.9
Co1 N14 H142 109.9
H141 N14 H142 108.2
O22 Co2 O12 93.35(13)
O22 Co2 N21 174.28(15)
O12 Co2 N21 86.43(16)
O22 Co2 N22 88.60(15)
O12 Co2 N22 92.41(15)
N21 Co2 N22 85.70(17)
O22 Co2 N24 87.60(15)
O12 Co2 N24 174.70(15)
N21 Co2 N24 93.14(17)
N22 Co2 N24 92.83(17)
O22 Co2 N23 93.24(14)
O12 Co2 N23 90.02(14)
N21 Co2 N23 92.47(17)
N22 Co2 N23 176.87(17)
N24 Co2 N23 84.72(17)
C21 N21 Co2 109.5(3)
C21 N21 H211 109.8
Co2 N21 H211 109.7
C21 N21 H212 109.9
Co2 N21 H212 109.7
H211 N21 H212 108.2
N21 C21 C22 107.2(4)
N21 C21 H213 110.0
C22 C21 H213 110.2
N21 C21 H214 110.4
C22 C21 H214 110.6
H213 C21 H214 108.5
N22 C22 C21 106.3(4)
N22 C22 H223 110.5
C21 C22 H223 110.2
N22 C22 H224 110.5
C21 C22 H224 110.7
H223 C22 H224 108.7
C22 N22 Co2 110.2(3)
C22 N22 H221 109.6
Co2 N22 H221 109.7
C22 N22 H222 109.6
Co2 N22 H222 109.7
H221 N22 H222 108.1
C23 N23 Co2 111.1(3)
C23 N23 H231 109.4
Co2 N23 H231 109.5
C23 N23 H232 109.3
Co2 N23 H232 109.4
H231 N23 H232 108.0
N23 C23 C24 107.3(4)
N23 C23 H233 110.4
C24 C23 H233 110.0
N23 C23 H234 110.1
C24 C23 H234 110.5
H233 C23 H234 108.5
N24 C24 C23 106.4(4)
N24 C24 H243 110.5
C23 C24 H243 110.3
N24 C24 H244 110.4
C23 C24 H244 110.7
H243 C24 H244 108.6
C24 N24 Co2 108.4(3)
C24 N24 H241 110.1
Co2 N24 H241 110.1
C24 N24 H242 110.0
Co2 N24 H242 109.8
H241 N24 H242 108.4
O13 Co3 O23 93.92(13)
O13 Co3 N32 86.30(15)
O23 Co3 N32 176.48(18)
O13 Co3 N34 88.98(16)
O23 Co3 N34 92.11(16)
N32 Co3 N34 91.41(19)
O13 Co3 N33 174.66(18)
O23 Co3 N33 86.33(15)
N32 Co3 N33 93.79(18)
N34 Co3 N33 85.68(19)
O13 Co3 N31 92.83(16)
O23 Co3 N31 91.09(15)
N32 Co3 N31 85.39(19)
N34 Co3 N31 176.21(18)
N33 Co3 N31 92.50(19)
C31 N31 Co3 111.3(4)
C31 N31 H311 109.5
Co3 N31 H311 109.4
C31 N31 H312 109.3
Co3 N31 H312 109.3
H311 N31 H312 108.0
N31 C31 C32 106.4(5)
N31 C31 H313 110.5
C32 C31 H313 110.5
N31 C31 H314 110.3
C32 C31 H314 110.5
H313 C31 H314 108.6
N32 C32 C31 108.6(5)
N32 C32 H323 109.9
C31 C32 H323 109.9
N32 C32 H324 110.1
C31 C32 H324 110.0
H323 C32 H324 108.4
C32 N32 Co3 108.5(3)
C32 N32 H321 110.0
Co3 N32 H321 109.9
C32 N32 H322 110.1
Co3 N32 H322 110.0
H321 N32 H322 108.4
C33 N33 Co3 109.1(4)
C33 N33 H331 110.1
Co3 N33 H331 110.0
C33 N33 H332 109.7
Co3 N33 H332 109.8
H331 N33 H332 108.3
N33 C33 C34 108.0(5)
N33 C33 H333 110.2
C34 C33 H333 110.3
N33 C33 H334 110.0
C34 C33 H334 109.9
H333 C33 H334 108.5
N34 C34 C33 106.8(5)
N34 C34 H343 110.6
C33 C34 H343 110.8
N34 C34 H344 110.0
C33 C34 H344 110.1
H343 C34 H344 108.6
C34 N34 Co3 110.6(4)
C34 N34 H341 109.9
Co3 N34 H341 109.5
C34 N34 H342 109.2
Co3 N34 H342 109.4
H341 N34 H342 108.1
N41 Co4 O31 85.41(15)
N41 Co4 O41 175.03(16)
O31 Co4 O41 93.64(13)
N41 Co4 N43 92.92(17)
O31 Co4 N43 175.04(16)
O41 Co4 N43 88.42(15)
N41 Co4 N42 86.05(17)
O31 Co4 N42 92.56(15)
O41 Co4 N42 89.12(15)
N43 Co4 N42 91.99(18)
N41 Co4 N44 92.35(17)
O31 Co4 N44 89.63(15)
O41 Co4 N44 92.52(15)
N43 Co4 N44 85.77(18)
N42 Co4 N44 177.18(17)
C41 N41 Co4 108.1(3)
C41 N41 H411 110.1
Co4 N41 H411 110.2
C41 N41 H412 110.0
Co4 N41 H412 110.0
H411 N41 H412 108.4
N41 C41 C42 106.5(4)
N41 C41 H413 110.4
C42 C41 H413 110.2
N41 C41 H414 110.5
C42 C41 H414 110.6
H413 C41 H414 108.6
N42 C42 C41 107.0(4)
N42 C42 H423 110.4
C41 C42 H423 110.1
N42 C42 H424 110.3
C41 C42 H424 110.4
H423 C42 H424 108.6
C42 N42 Co4 109.7(3)
C42 N42 H421 109.8
Co4 N42 H421 109.8
C42 N42 H422 109.7
Co4 N42 H422 109.6
H421 N42 H422 108.2
C43 N43 Co4 108.7(4)
C43 N43 H431 110.0
Co4 N43 H431 109.9
C43 N43 H432 109.9
Co4 N43 H432 110.0
H431 N43 H432 108.3
C44 C43 N43 120.1(6)
C44 C43 H433 108.0
N43 C43 H433 107.3
C44 C43 H434 106.3
N43 C43 H434 107.4
H433 C43 H434 106.9
C43 C44 N44 115.6(6)
C43 C44 H443 109.3
N44 C44 H443 109.2
C43 C44 H444 107.6
N44 C44 H444 107.4
H443 C44 H444 107.4
C44 N44 Co4 109.7(4)
C44 N44 H441 108.8
Co4 N44 H441 109.7
C44 N44 H442 110.6
Co4 N44 H442 109.8
H441 N44 H442 108.2
N54 Co5 O32 86.31(17)
N54 Co5 O42 175.83(16)
O32 Co5 O42 95.12(13)
N54 Co5 N52 92.33(19)
O32 Co5 N52 175.18(17)
O42 Co5 N52 86.55(15)
N54 Co5 N53 84.85(17)
O32 Co5 N53 92.39(15)
O42 Co5 N53 91.18(15)
N52 Co5 N53 92.09(18)
N54 Co5 N51 94.38(17)
O32 Co5 N51 89.46(15)
O42 Co5 N51 89.55(15)
N52 Co5 N51 86.02(18)
N53 Co5 N51 177.94(17)
C51 N51 Co5 109.8(3)
C51 N51 H511 109.8
Co5 N51 H511 109.8
C51 N51 H512 109.5
Co5 N51 H512 109.7
H511 N51 H512 108.2
C52 C51 N51 107.3(5)
C52 C51 H513 110.0
N51 C51 H513 110.1
C52 C51 H514 110.5
N51 C51 H514 110.4
H513 C51 H514 108.5
C51 C52 N52 109.9(5)
C51 C52 H523 109.5
N52 C52 H523 109.5
C51 C52 H524 109.7
N52 C52 H524 110.1
H523 C52 H524 108.2
C52 N52 Co5 108.1(3)
C52 N52 H521 110.2
Co5 N52 H521 110.1
C52 N52 H522 109.8
Co5 N52 H522 110.1
H521 N52 H522 108.5
C53 N53 Co5 112.0(3)
C53 N53 H531 109.0
Co5 N53 H531 109.3
C53 N53 H532 109.4
Co5 N53 H532 109.1
H531 N53 H532 107.9
N53 C53 C54 107.9(4)
N53 C53 H533 109.9
C54 C53 H533 109.8
N53 C53 H534 110.4
C54 C53 H534 110.4
H533 C53 H534 108.5
N54 C54 C53 108.4(5)
N54 C54 H543 109.8
C53 C54 H543 109.7
N54 C54 H544 110.1
C53 C54 H544 110.4
H543 C54 H544 108.4
C54 N54 Co5 109.2(3)
C54 N54 H541 109.6
Co5 N54 H541 109.6
C54 N54 H542 110.2
Co5 N54 H542 109.9
H541 N54 H542 108.3
O33 Co6 N63 84.15(15)
O33 Co6 O43 94.53(13)
N63 Co6 O43 176.35(15)
O33 Co6 N62 175.79(15)
N63 Co6 N62 94.08(17)
O43 Co6 N62 87.46(15)
O33 Co6 N64 91.33(14)
N63 Co6 N64 85.55(16)
O43 Co6 N64 91.09(14)
N62 Co6 N64 92.34(16)
O33 Co6 N61 90.83(15)
N63 Co6 N61 92.23(17)
O43 Co6 N61 91.19(15)
N62 Co6 N61 85.41(16)
N64 Co6 N61 176.73(16)
C61 N61 Co6 110.2(3)
C61 N61 H611 109.6
Co6 N61 H611 109.6
C61 N61 H612 109.5
Co6 N61 H612 109.8
H611 N61 H612 108.2
N61 C61 C62 107.6(4)
N61 C61 H613 110.1
C62 C61 H613 110.1
N61 C61 H614 110.3
C62 C61 H614 110.2
H613 C61 H614 108.4
N62 C62 C61 107.2(4)
N62 C62 H623 110.0
C61 C62 H623 110.3
N62 C62 H624 110.5
C61 C62 H624 110.2
H623 C62 H624 108.6
C62 N62 Co6 108.7(3)
C62 N62 H621 109.7
Co6 N62 H621 109.9
C62 N62 H622 110.1
Co6 N62 H622 110.0
H621 N62 H622 108.3
C63 N63 Co6 108.8(3)
C63 N63 H631 110.0
Co6 N63 H631 110.0
C63 N63 H632 109.8
Co6 N63 H632 109.9
H631 N63 H632 108.3
N63 C63 C64 106.5(4)
N63 C63 H633 110.5
C64 C63 H633 110.7
N63 C63 H634 110.4
C64 C63 H634 110.1
H633 C63 H634 108.6
N64 C64 C63 107.9(4)
N64 C64 H643 110.1
C63 C64 H643 110.4
N64 C64 H644 109.9
C63 C64 H644 110.0
H643 C64 H644 108.4
C64 N64 Co6 111.1(3)
C64 N64 H641 109.5
Co6 N64 H641 109.2
C64 N64 H642 109.5
Co6 N64 H642 109.5
H641 N64 H642 108.0
O11 P1 O12 110.46(17)
O11 P1 O13 110.75(18)
O12 P1 O13 111.31(18)
O11 P1 O14 108.20(18)
O12 P1 O14 107.54(18)
O13 P1 O14 108.47(17)
P1 O11 Co1 133.72(19)
P1 O12 Co2 133.49(18)
P1 O13 Co3 133.2(2)
O23 P2 O21 110.80(18)
O23 P2 O22 111.91(17)
O21 P2 O22 112.69(17)
O23 P2 O24 108.89(18)
O21 P2 O24 108.67(18)
O22 P2 O24 103.54(18)
P2 O21 Co1 132.61(19)
P2 O22 Co2 133.31(18)
P2 O23 Co3 132.3(2)
O31 P3 O32 111.00(18)
O31 P3 O33 110.74(17)
O32 P3 O33 109.92(18)
O31 P3 O34 107.68(18)
O32 P3 O34 110.03(18)
O33 P3 O34 107.38(19)
P3 O31 Co4 135.2(2)
P3 O32 Co5 129.89(19)
P3 O33 Co6 133.56(18)
O41 P4 O43 112.88(18)
O41 P4 O42 111.58(18)
O43 P4 O42 111.05(18)
O41 P4 O44 104.67(18)
O43 P4 O44 108.33(18)
O42 P4 O44 107.97(18)
P4 O41 Co4 132.4(2)
P4 O42 Co5 134.46(19)
P4 O43 Co6 131.12(18)
O51 P5 O52 116.9(3)
O51 P5 O54 111.3(3)
O52 P5 O54 106.2(3)
O51 P5 O53 109.4(3)
O52 P5 O53 108.6(3)
O54 P5 O53 103.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 O11 1.928(3)
Co1 N14 1.935(4)
Co1 N12 1.940(4)
Co1 O21 1.942(3)
Co1 N11 1.944(4)
Co1 N13 1.957(4)
N11 C11 1.467(6)
N11 H111 0.9000
N11 H112 0.9000
C11 C12 1.504(8)
C11 H113 0.9700
C11 H114 0.9700
C12 N12 1.470(6)
C12 H123 0.9700
C12 H124 0.9700
N12 H121 0.9000
N12 H122 0.9000
N13 C13 1.470(6)
N13 H131 0.9000
N13 H132 0.9000
C13 C14 1.508(9)
C13 H133 0.9700
C13 H134 0.9700
C14 N14 1.488(7)
C14 H143 0.9700
C14 H144 0.9700
N14 H141 0.9000
N14 H142 0.9000
Co2 O22 1.924(3)
Co2 O12 1.929(3)
Co2 N21 1.932(4)
Co2 N22 1.937(4)
Co2 N24 1.944(4)
Co2 N23 1.962(4)
N21 C21 1.456(7)
N21 H211 0.9000
N21 H212 0.9000
C21 C22 1.508(7)
C21 H213 0.9700
C21 H214 0.9700
C22 N22 1.482(6)
C22 H223 0.9700
C22 H224 0.9700
N22 H221 0.9000
N22 H222 0.9000
N23 C23 1.469(6)
N23 H231 0.9000
N23 H232 0.9000
C23 C24 1.491(7)
C23 H233 0.9700
C23 H234 0.9700
C24 N24 1.488(6)
C24 H243 0.9700
C24 H244 0.9700
N24 H241 0.9000
N24 H242 0.9000
Co3 O13 1.926(3)
Co3 O23 1.939(3)
Co3 N32 1.940(4)
Co3 N34 1.942(4)
Co3 N33 1.946(4)
Co3 N31 1.959(4)
N31 C31 1.479(7)
N31 H311 0.9000
N31 H312 0.9000
C31 C32 1.501(9)
C31 H313 0.9700
C31 H314 0.9700
C32 N32 1.471(7)
C32 H323 0.9700
C32 H324 0.9700
N32 H321 0.9000
N32 H322 0.9000
N33 C33 1.440(8)
N33 H331 0.9000
N33 H332 0.9000
C33 C34 1.514(10)
C33 H333 0.9700
C33 H334 0.9700
C34 N34 1.486(7)
C34 H343 0.9700
C34 H344 0.9700
N34 H341 0.9000
N34 H342 0.9000
Co4 N41 1.921(4)
Co4 O31 1.924(3)
Co4 O41 1.927(3)
Co4 N43 1.951(4)
Co4 N42 1.953(4)
Co4 N44 1.960(4)
N41 C41 1.486(6)
N41 H411 0.9000
N41 H412 0.9000
C41 C42 1.494(8)
C41 H413 0.9700
C41 H414 0.9700
C42 N42 1.482(6)
C42 H423 0.9700
C42 H424 0.9700
N42 H421 0.9000
N42 H422 0.9000
N43 C43 1.446(8)
N43 H431 0.9000
N43 H432 0.9000
C43 C44 1.298(11)
C43 H433 0.9700
C43 H434 0.9700
C44 N44 1.471(7)
C44 H443 0.9700
C44 H444 0.9700
N44 H441 0.9000
N44 H442 0.9000
Co5 N54 1.933(4)
Co5 O32 1.936(3)
Co5 O42 1.939(3)
Co5 N52 1.944(4)
Co5 N53 1.956(4)
Co5 N51 1.961(4)
N51 C51 1.473(7)
N51 H511 0.9000
N51 H512 0.9000
C51 C52 1.468(8)
C51 H513 0.9700
C51 H514 0.9700
C52 N52 1.480(7)
C52 H523 0.9700
C52 H524 0.9700
N52 H521 0.9000
N52 H522 0.9000
N53 C53 1.474(6)
N53 H531 0.9000
N53 H532 0.9000
C53 C54 1.495(8)
C53 H533 0.9700
C53 H534 0.9700
C54 N54 1.465(7)
C54 H543 0.9700
C54 H544 0.9700
N54 H541 0.9000
N54 H542 0.9000
Co6 O33 1.912(3)
Co6 N63 1.939(4)
Co6 O43 1.944(3)
Co6 N62 1.945(4)
Co6 N64 1.957(4)
Co6 N61 1.972(4)
N61 C61 1.481(7)
N61 H611 0.9000
N61 H612 0.9000
C61 C62 1.501(8)
C61 H613 0.9700
C61 H614 0.9700
C62 N62 1.479(7)
C62 H623 0.9700
C62 H624 0.9700
N62 H621 0.9000
N62 H622 0.9000
N63 C63 1.491(6)
N63 H631 0.9000
N63 H632 0.9000
C63 C64 1.513(7)
C63 H633 0.9700
C63 H634 0.9700
C64 N64 1.468(6)
C64 H643 0.9700
C64 H644 0.9700
N64 H641 0.9000
N64 H642 0.9000
P1 O11 1.527(3)
P1 O12 1.537(3)
P1 O13 1.540(3)
P1 O14 1.540(3)
P2 O23 1.524(3)
P2 O21 1.526(3)
P2 O22 1.527(3)
P2 O24 1.561(3)
P3 O31 1.533(3)
P3 O32 1.534(3)
P3 O33 1.537(3)
P3 O34 1.540(3)
P4 O41 1.534(3)
P4 O43 1.534(3)
P4 O42 1.536(3)
P4 O44 1.554(3)
P5 O51 1.480(4)
P5 O52 1.485(4)
P5 O54 1.575(5)
P5 O53 1.589(4)
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
N11 H111 Cl4 0.90 2.47 3.352(4) 168.6 .
N11 H112 O12 0.90 2.11 2.909(5) 148.1 .
N12 H121 Cl7 0.90 2.34 3.194(5) 159.6 .
N12 H122 O52 0.90 1.93 2.821(6) 171.1 2_756
N13 H131 Cl7 0.90 2.48 3.356(5) 163.0 .
N13 H132 O23 0.90 2.21 2.991(5) 144.8 .
N14 H141 Cl4 0.90 2.42 3.301(5) 165.2 .
N14 H142 O52 0.90 2.05 2.919(6) 162.0 2_756
N21 H212 Cl1 0.90 2.42 3.314(4) 174.3 2_746
N21 H211 Cl2 0.90 2.40 3.294(4) 172.6 2_746
N22 H221 Cl5 0.90 2.39 3.256(4) 161.8 2_646
N22 H222 O13 0.90 2.23 2.997(5) 142.9 .
N23 H232 O21 0.90 2.14 2.937(5) 147.7 .
N24 H241 Cl5 0.90 2.38 3.246(4) 160.8 2_646
N24 H242 Cl1 0.90 2.43 3.265(4) 155.1 2_746
N31 H311 Cl3 0.90 2.58 3.458(5) 164.8 2_656
N31 H312 O11 0.90 2.16 2.948(5) 145.3 .
N32 H322 Cl6 0.90 2.41 3.304(4) 171.5 .
N32 H321 O5W 0.90 2.00 2.876(8) 163.2 1_554
N33 H332 Cl6 0.90 2.33 3.202(4) 163.0 .
N34 H342 O22 0.90 2.17 2.956(5) 144.9 .
N41 H411 Cl4 0.90 2.36 3.204(4) 155.6 1_455
N41 H412 O51 0.90 2.09 2.922(6) 152.4 2_656
N42 H422 Cl3 0.90 2.56 3.454(4) 171.0 .
N42 H421 O32 0.90 2.18 2.973(5) 147.4 .
N43 H431 Cl4 0.90 2.50 3.360(4) 160.8 1_455
N44 H441 O43 0.90 2.15 2.951(5) 147.9 .
N44 H442 O51 0.90 1.99 2.873(6) 167.5 2_656
N51 H511 O41 0.90 2.16 2.946(5) 145.8 .
N52 H521 Cl7 0.90 2.45 3.278(4) 153.0 2_746
N52 H522 O2W 0.90 2.17 3.056(6) 168.9 1_556
N53 H531 O33 0.90 2.05 2.837(5) 145.4 .
N53 H532 O3W 0.90 2.12 3.017(6) 176.1 .
N61 H612 Cl1 0.90 2.47 3.352(4) 166.9 .
N61 H611 O42 0.90 2.20 2.963(5) 141.6 .
N62 H621 Cl2 0.90 2.58 3.468(4) 168.2 .
N62 H622 Cl5 0.90 2.41 3.258(4) 156.4 .
N63 H632 Cl1 0.90 2.43 3.292(4) 161.2 .
N63 H631 Cl2 0.90 2.28 3.151(4) 163.2 .
N64 H642 Cl5 0.90 2.38 3.263(4) 166.0 .
N64 H641 O31 0.90 2.07 2.873(5) 148.4 .
O14 . O44 . . 2.449(4) . 1_554
O24 . O34 . . 2.417(4) . .
O53 . O1W . . 2.646(6) . .
O54 . O4W . . 2.606(7) . 2_646
O1W . O24 . . 2.740(5) . .
O2W . O14 . . 2.761(5) . .
O2W . O3W . . 2.771(7) . 1_554
O4W . O34 . . 2.750(6) . .
O4W . Cl3 . . 3.041(6) . 2_656
O5W . O44 . . 2.782(8) . .
O5W . O13 . . 2.988(8) . 1_556
|
1500009.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500009.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_1500009
loop_
_publ_author_name
'Raj Pal Sharma'
'Bal Krishan Vermani'
'Rajni Sharma'
'Ritu Bala'
'Dip Singh Gill'
'Juan M. Salas'
'Miguel Quir\'os'
_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
;
Synthesis, spectroscopic characterization and
X-ray structure determinations and packing of tetralkylammonium
trans-diamminetetranitrocobaltate(III) complex salts where
alkyl = methyl or ehtyl
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 222
_journal_page_last 227
_journal_paper_doi 10.1016/j.molstruc.2005.09.008
_journal_volume 784
_journal_year 2006
_chemical_formula_sum 'C8 H26 Co N7 O8'
_chemical_formula_weight 407.29
_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 104.493(12)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 10.2635(18)
_cell_length_b 9.0480(15)
_cell_length_c 9.752(2)
_cell_measurement_reflns_used 39
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.42
_cell_measurement_theta_min 4.86
_cell_volume 876.8(3)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0427
_diffrn_reflns_av_sigmaI/netI 0.0378
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 3303
_diffrn_reflns_theta_full 30.01
_diffrn_reflns_theta_max 30.01
_diffrn_reflns_theta_min 2.05
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.030
_exptl_absorpt_correction_T_max 0.6460
_exptl_absorpt_correction_T_min 0.5437
_exptl_absorpt_correction_type psi-scan
_exptl_crystal_density_diffrn 1.543
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 428
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_refine_diff_density_max 0.645
_refine_diff_density_min -0.414
_refine_diff_density_rms 0.070
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 111
_refine_ls_number_reflns 2560
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.050
_refine_ls_R_factor_all 0.0512
_refine_ls_R_factor_gt 0.0408
_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^)+(0.0600P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1184
_reflns_number_gt 2095
_reflns_number_total 2560
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file coinet.cif
_cod_data_source_block coinet
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M 'P 2(1)/c'
_cod_database_code 1500009
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
Co Co 0.5000 0.5000 0.5000 0.02632(12) Uani 1 2 d S
N1M N 0.47195(19) 0.5487(2) 0.29980(19) 0.0395(4) Uani 1 1 d .
H1M H 0.3946 0.5973 0.2700 0.047 Uiso 1 1 d R
H2M H 0.4690 0.4657 0.2501 0.047 Uiso 1 1 d R
H3M H 0.5394 0.6050 0.2879 0.047 Uiso 1 1 d R
N1N N 0.32854(17) 0.5887(2) 0.5016(2) 0.0396(4) Uani 1 1 d .
O1N O 0.23534(17) 0.5883(3) 0.3945(2) 0.0661(6) Uani 1 1 d .
O2N O 0.3133(2) 0.6491(3) 0.6099(2) 0.0709(6) Uani 1 1 d .
N2N N 0.58491(18) 0.6924(2) 0.5508(2) 0.0384(4) Uani 1 1 d .
O3N O 0.6560(2) 0.7153(2) 0.6705(2) 0.0613(5) Uani 1 1 d .
O4N O 0.5646(3) 0.7943(2) 0.4650(2) 0.0774(7) Uani 1 1 d .
N1C N 0.0000 0.5000 0.0000 0.0330(4) Uani 1 2 d S
C1C C -0.0925(5) 0.6053(5) -0.0877(5) 0.0449(9) Uiso 0.50 1 d P
H11C H -0.1843 0.5742 -0.0945 0.054 Uiso 0.50 1 d PR
H12C H -0.0786 0.6059 -0.1825 0.054 Uiso 0.50 1 d PR
C2C C -0.0242(5) 0.3470(5) -0.0673(5) 0.0431(9) Uiso 0.50 1 d P
H21C H -0.0093 0.3507 -0.1616 0.052 Uiso 0.50 1 d PR
H22C H -0.1170 0.3184 -0.0763 0.052 Uiso 0.50 1 d PR
C5C C -0.0704(3) 0.7708(3) -0.0219(4) 0.0674(8) Uani 1 1 d .
H51C H 0.0012 0.7697 0.0630 0.081 Uiso 0.50 1 d PR
H52C H -0.1518 0.8041 -0.0002 0.081 Uiso 0.50 1 d PR
H53C H -0.0474 0.8365 -0.0896 0.081 Uiso 0.50 1 d PR
H54C H -0.1611 0.7532 -0.0162 0.081 Uiso 0.50 1 d PR
H55C H -0.0659 0.7645 -0.1189 0.081 Uiso 0.50 1 d PR
H56C H -0.0426 0.8675 0.0143 0.081 Uiso 0.50 1 d PR
C3C C 0.1504(5) 0.5398(6) 0.0137(5) 0.0426(9) Uiso 0.50 1 d P
H31C H 0.2086 0.4638 0.0666 0.051 Uiso 0.50 1 d PR
H32C H 0.1729 0.6335 0.0621 0.051 Uiso 0.50 1 d PR
C4C C -0.0091(5) 0.4934(5) 0.1522(5) 0.0447(10) Uiso 0.50 1 d P
H41C H 0.0145 0.5883 0.1980 0.054 Uiso 0.50 1 d PR
H42C H 0.0515 0.4189 0.2042 0.054 Uiso 0.50 1 d PR
C6C C 0.1684(5) 0.5489(4) -0.1466(5) 0.0971(16) Uani 1 1 d .
H61C H 0.1040 0.4851 -0.2070 0.116 Uiso 0.50 1 d PR
H62C H 0.2577 0.5185 -0.1479 0.116 Uiso 0.50 1 d PR
H63C H 0.1538 0.6488 -0.1799 0.116 Uiso 0.50 1 d PR
H64C H 0.1709 0.6400 -0.1962 0.116 Uiso 0.50 1 d PR
H65C H 0.2076 0.4716 -0.1906 0.116 Uiso 0.50 1 d PR
H66C H 0.2183 0.5596 -0.0498 0.116 Uiso 0.50 1 d PR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.02216(17) 0.02658(18) 0.02904(18) 0.00093(13) 0.00420(11) 0.00146(11)
N1M 0.0400(9) 0.0414(9) 0.0345(8) 0.0047(7) 0.0042(7) 0.0003(8)
N1N 0.0304(8) 0.0398(9) 0.0492(10) 0.0043(8) 0.0112(7) 0.0072(7)
O1N 0.0326(8) 0.0774(14) 0.0765(13) -0.0106(11) -0.0086(8) 0.0174(9)
O2N 0.0632(12) 0.0953(17) 0.0605(11) 0.0009(11) 0.0273(10) 0.0363(12)
N2N 0.0382(8) 0.0329(8) 0.0436(9) -0.0033(7) 0.0093(7) -0.0044(7)
O3N 0.0737(12) 0.0509(10) 0.0502(10) -0.0126(8) -0.0017(9) -0.0188(9)
O4N 0.1131(19) 0.0389(10) 0.0678(12) 0.0132(9) -0.0007(13) -0.0218(11)
N1C 0.0322(10) 0.0333(11) 0.0312(10) -0.0020(9) 0.0036(8) -0.0066(8)
C5C 0.0642(17) 0.0403(13) 0.100(2) 0.0121(15) 0.0258(16) 0.0109(12)
C6C 0.134(4) 0.0568(17) 0.140(4) 0.011(2) 0.109(3) 0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1N Co N1M 90.44(8) . .
N1N Co N2N 88.69(8) . .
N1M Co N2N 89.83(8) . .
O1N N1N O2N 119.5(2) . .
O1N N1N Co 120.49(17) . .
O2N N1N Co 120.01(16) . .
O4N N2N O3N 118.7(2) . .
O4N N2N Co 120.50(16) . .
O3N N2N Co 120.74(15) . .
C1C N1C C4C 114.2(3) . .
C1C N1C C2C 109.2(2) . .
C4C N1C C2C 110.1(3) . .
C1C N1C C3C 112.6(3) . .
C4C N1C C3C 103.2(3) . .
C2C N1C C3C 107.3(3) . .
N1C C1C C5C 111.4(3) . .
N1C C2C C5C 111.7(3) . 3_565
C2C C5C C1C 66.1(3) 3_565 .
N1C C3C C6C 106.2(3) . .
N1C C4C C6C 106.2(3) . 3_565
C3C C6C C4C 70.9(3) . 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N1N 1.9379(17) .
Co N1M 1.9514(18) .
Co N2N 1.9546(18) .
N1N O1N 1.227(3) .
N1N O2N 1.233(3) .
N2N O4N 1.227(3) .
N2N O3N 1.230(3) .
N1C C1C 1.460(5) .
N1C C4C 1.511(5) .
N1C C2C 1.526(5) .
N1C C3C 1.558(5) .
C1C C5C 1.623(6) .
C2C C5C 1.553(5) 3_565
C5C C2C 1.553(5) 3_565
C3C C6C 1.622(6) .
C4C C6C 1.667(6) 3_565
C6C C4C 1.667(6) 3_565
|
1500010.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500010.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_1500010
loop_
_publ_author_name
'Raj Pal Sharma'
'Bal Krishan Vermani'
'Rajni Sharma'
'Ritu Bala'
'Dip Singh Gill'
'Juan M. Salas'
'Miguel Quir\'os'
_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
;
Synthesis, spectroscopic characterization and
X-ray structure determinations and packing of tetralkylammonium
trans-diamminetetranitrocobaltate(III) complex salts where
alkyl = methyl or ehtyl
;
_journal_name_full 'Journal of Molecular Structure'
_journal_page_first 222
_journal_page_last 227
_journal_paper_doi 10.1016/j.molstruc.2005.09.008
_journal_volume 784
_journal_year 2006
_chemical_formula_sum 'C4 H18 Co N7 O8'
_chemical_formula_weight 351.18
_chemical_name_systematic
;
?
;
_space_group_IT_number 11
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yb'
_symmetry_space_group_name_H-M 'P 1 21/m 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.078(7)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 6.1926(7)
_cell_length_b 18.248(3)
_cell_length_c 6.2335(6)
_cell_measurement_reflns_used 35
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.43
_cell_measurement_theta_min 4.64
_cell_volume 704.41(16)
_computing_cell_refinement 'Siemens XSCANS'
_computing_data_collection 'Siemens XSCANS'
_computing_data_reduction 'Siemens SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0213
_diffrn_reflns_av_sigmaI/netI 0.0350
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 3406
_diffrn_reflns_theta_full 32.50
_diffrn_reflns_theta_max 32.50
_diffrn_reflns_theta_min 2.23
_diffrn_standards_decay_% 7.92
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.268
_exptl_absorpt_correction_T_max 0.7786
_exptl_absorpt_correction_T_min 0.6546
_exptl_absorpt_correction_type psi-scan
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.656
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular shape'
_exptl_crystal_F_000 364
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.05
_refine_diff_density_max 1.425
_refine_diff_density_min -1.244
_refine_diff_density_rms 0.181
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.236
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 107
_refine_ls_number_reflns 2630
_refine_ls_number_restraints 10
_refine_ls_restrained_S_all 1.234
_refine_ls_R_factor_all 0.0999
_refine_ls_R_factor_gt 0.0868
_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^)+(0.1300P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2891
_refine_ls_wR_factor_ref 0.2981
_reflns_number_gt 2110
_reflns_number_total 2630
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file coinmet.cif
_cod_data_source_block coinmet
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_sg_symbol_H-M 'P 2(1)/m '
_cod_database_code 1500010
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-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
Co Co 0.5000 0.5000 0.5000 0.0239(3) Uani 1 2 d S
N1M N 0.3247(8) 0.5269(3) 0.2521(8) 0.0380(10) Uani 1 1 d .
H1M H 0.3252 0.4904 0.1573 0.046 Uiso 1 1 d R
H2M H 0.3791 0.5670 0.1916 0.046 Uiso 1 1 d R
H3M H 0.1897 0.5356 0.2940 0.046 Uiso 1 1 d R
N1N N 0.2443(8) 0.4565(3) 0.6309(8) 0.0378(10) Uani 1 1 d .
O1N O 0.1115(8) 0.4240(3) 0.5135(8) 0.0512(12) Uani 1 1 d .
O2N O 0.2155(10) 0.4596(4) 0.8232(8) 0.0667(17) Uani 1 1 d .
N2N N 0.5596(8) 0.4036(3) 0.3727(9) 0.0403(10) Uani 1 1 d .
O3N O 0.6049(11) 0.3518(3) 0.4923(9) 0.0582(14) Uani 1 1 d .
O4N O 0.5441(11) 0.3950(3) 0.1781(8) 0.0622(15) Uani 1 1 d .
N1C N 0.0680(13) 0.2500 -0.0032(12) 0.0399(14) Uani 1 2 d SD
C1C C 0.040(3) 0.3136(7) 0.128(3) 0.136(7) Uani 1 1 d .
H11C H 0.0693 0.3568 0.0438 0.163 Uiso 1 1 d R
H12C H 0.1395 0.3121 0.2476 0.163 Uiso 1 1 d R
H13C H -0.1052 0.3161 0.1822 0.163 Uiso 1 1 d R
C2C C 0.269(3) 0.2500 -0.128(4) 0.119(8) Uani 1 2 d SD
H21C H 0.354(3) 0.2927 -0.097(6) 0.143 Uiso 1 1 d D
H22C H 0.238(7) 0.2500 -0.279(3) 0.143 Uiso 1 2 d SD
C3C C -0.101(4) 0.2500 -0.165(4) 0.171(15) Uani 1 2 d SD
H31C H -0.192(4) 0.2927 -0.150(6) 0.205 Uiso 1 1 d D
H32C H -0.043(7) 0.2500 -0.308(3) 0.205 Uiso 1 2 d SD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0237(4) 0.0282(4) 0.0198(4) 0.0006(3) 0.0003(3) -0.0005(3)
N1M 0.036(2) 0.047(3) 0.031(2) 0.0040(19) -0.0019(17) 0.000(2)
N1N 0.032(2) 0.048(3) 0.033(2) 0.0009(19) 0.0013(16) -0.0042(19)
O1N 0.039(2) 0.063(3) 0.052(3) -0.007(2) 0.0024(19) -0.018(2)
O2N 0.057(3) 0.107(5) 0.036(2) 0.005(3) 0.009(2) -0.019(3)
N2N 0.037(2) 0.039(2) 0.044(3) -0.003(2) 0.0031(19) 0.0015(19)
O3N 0.083(4) 0.036(2) 0.055(3) 0.004(2) 0.001(3) 0.009(2)
O4N 0.087(4) 0.062(3) 0.038(2) -0.016(2) 0.004(2) 0.008(3)
N1C 0.038(3) 0.036(3) 0.046(4) 0.000 0.002(3) 0.000
C1C 0.192(19) 0.069(7) 0.146(14) -0.038(8) 0.074(13) -0.013(9)
C2C 0.075(11) 0.150(19) 0.133(17) 0.000 0.058(12) 0.000
C3C 0.098(17) 0.31(5) 0.105(17) 0.000 -0.027(14) 0.000
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1M Co N1M 180.0(2) . 3_666
N1M Co N1N 89.0(2) . .
N1M Co N1N 91.0(2) 3_666 .
N1M Co N1N 91.0(2) . 3_666
N1M Co N1N 89.0(2) 3_666 3_666
N1N Co N1N 179.999(2) . 3_666
N1M Co N2N 90.6(2) . .
N1M Co N2N 89.4(2) 3_666 .
N1N Co N2N 87.6(2) . .
N1N Co N2N 92.4(2) 3_666 .
N1M Co N2N 89.4(2) . 3_666
N1M Co N2N 90.6(2) 3_666 3_666
N1N Co N2N 92.4(2) . 3_666
N1N Co N2N 87.6(2) 3_666 3_666
N2N Co N2N 180.0(3) . 3_666
O2N N1N O1N 120.2(5) . .
O2N N1N Co 121.0(4) . .
O1N N1N Co 118.8(4) . .
O4N N2N O3N 121.0(6) . .
O4N N2N Co 120.0(5) . .
O3N N2N Co 118.9(4) . .
C1C N1C C1C 108.5(14) . 4_565
C1C N1C C3C 108.1(11) . .
C1C N1C C3C 108.1(11) 4_565 .
C1C N1C C2C 113.8(9) . .
C1C N1C C2C 113.8(9) 4_565 .
C3C N1C C2C 104.1(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N1M 1.950(5) .
Co N1M 1.950(5) 3_666
Co N1N 1.951(5) .
Co N1N 1.951(5) 3_666
Co N2N 1.965(5) .
Co N2N 1.965(5) 3_666
N1N O2N 1.214(7) .
N1N O1N 1.249(7) .
N2N O4N 1.227(7) .
N2N O3N 1.236(7) .
N1C C1C 1.430(13) .
N1C C1C 1.430(13) 4_565
N1C C3C 1.453(19) .
N1C C2C 1.470(15) .
|
1500011.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500011.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_1500011
loop_
_publ_author_name
'Sonia B. Jim\'enez-Pulido'
'F\'atima M. Linares-Ordo\~nez'
'Jos\'e M. Mart\'inez-Martos'
'Miguel N. Moreno-Carretero'
'Miguel Quir\'os'
'Mar\'ia J. Ram\'irez-Exp\'osito'
_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
;
Metal complexes with the ligand derived from
6-acetyl-1,3,7-trimethyllumazine and benzohydrazide.
Molecular structures of two new Co(II) and Rh(III) complexes
and analysis of in vitro antitumor activity
;
_journal_name_full 'Journal of Inorganic Biochemistry'
_journal_page_first 1677
_journal_page_last 1683
_journal_paper_doi 10.1016/j.jinorgbio.2008.04.004
_journal_volume 102
_journal_year 2008
_chemical_formula_sum 'C24 H29 Cl2 Co N9 O12'
_chemical_formula_weight 765.39
_chemical_name_systematic
;
?
;
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_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 8
_cell_length_a 14.9599(7)
_cell_length_b 19.0064(9)
_cell_length_c 23.4883(11)
_cell_measurement_reflns_used 5746
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 22.36
_cell_measurement_theta_min 2.20
_cell_volume 6678.5(5)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0538
_diffrn_reflns_av_sigmaI/netI 0.0489
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 40960
_diffrn_reflns_theta_full 28.42
_diffrn_reflns_theta_max 28.42
_diffrn_reflns_theta_min 1.73
_diffrn_standards_decay_% 0.25
_diffrn_standards_number 427
_exptl_absorpt_coefficient_mu 0.746
_exptl_absorpt_correction_T_max 0.8072
_exptl_absorpt_correction_T_min 0.6541
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.522
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 3144
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.31
_exptl_crystal_size_min 0.30
_refine_diff_density_max 0.925
_refine_diff_density_min -0.816
_refine_diff_density_rms 0.106
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 426
_refine_ls_number_reflns 7905
_refine_ls_number_restraints 20
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.1015
_refine_ls_R_factor_gt 0.0713
_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^)+(0.1300P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2027
_refine_ls_wR_factor_ref 0.2247
_reflns_number_gt 5368
_reflns_number_total 7905
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file cojdz.cif
_cod_data_source_block cojdz
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' tag value 'orthorrombic' was replaced with
'orthorhombic' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_database_code 1500011
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co Co 0.38654(3) 0.18435(2) 0.32809(2) 0.03548(18) Uani 1 1 d .
N1 N 0.3799(2) 0.45450(18) 0.26062(18) 0.0512(9) Uani 1 1 d .
C1 C 0.3735(4) 0.5311(3) 0.2659(3) 0.0816(17) Uani 1 1 d .
H01 H 0.4274 0.5534 0.2527 0.098 Uiso 1 1 d R
H02 H 0.3641 0.5425 0.3053 0.098 Uiso 1 1 d R
H03 H 0.3238 0.5478 0.2438 0.098 Uiso 1 1 d R
C1A C 0.3814(2) 0.4126(2) 0.30798(19) 0.0417(8) Uani 1 1 d .
C2 C 0.3809(3) 0.4273(2) 0.2064(2) 0.0536(11) Uani 1 1 d .
O2 O 0.3770(2) 0.4635(2) 0.16433(16) 0.0743(10) Uani 1 1 d .
N3 N 0.3862(2) 0.35269(19) 0.20036(14) 0.0451(8) Uani 1 1 d .
C3 C 0.3901(3) 0.3264(3) 0.1419(2) 0.0605(12) Uani 1 1 d .
H31 H 0.3971 0.2762 0.1424 0.073 Uiso 1 1 d R
H32 H 0.4400 0.3474 0.1227 0.073 Uiso 1 1 d R
H33 H 0.3359 0.3384 0.1223 0.073 Uiso 1 1 d R
C4 C 0.3861(2) 0.3073(2) 0.24432(17) 0.0390(8) Uani 1 1 d .
C4A C 0.3837(2) 0.33993(19) 0.30063(17) 0.0364(8) Uani 1 1 d .
O4 O 0.38779(17) 0.24328(14) 0.23944(11) 0.0442(6) Uani 1 1 d .
N5 N 0.38332(18) 0.29686(16) 0.34437(14) 0.0360(6) Uani 1 1 d .
C6 C 0.3808(2) 0.32336(18) 0.39757(17) 0.0373(8) Uani 1 1 d .
C7 C 0.3802(2) 0.3971(2) 0.40456(19) 0.0460(9) Uani 1 1 d .
C71 C 0.3789(4) 0.4345(3) 0.4600(2) 0.0723(15) Uani 1 1 d .
H71 H 0.3705 0.4842 0.4543 0.087 Uiso 1 1 d R
H72 H 0.4349 0.4266 0.4789 0.087 Uiso 1 1 d R
H73 H 0.3311 0.4164 0.4830 0.087 Uiso 1 1 d R
N8 N 0.3806(2) 0.44067(17) 0.35945(17) 0.0497(8) Uani 1 1 d .
C9 C 0.3784(2) 0.26774(19) 0.44181(16) 0.0393(8) Uani 1 1 d .
C91 C 0.3795(4) 0.2812(3) 0.50448(19) 0.0657(13) Uani 1 1 d .
H91 H 0.3237 0.3013 0.5164 0.079 Uiso 1 1 d R
H92 H 0.4273 0.3130 0.5134 0.079 Uiso 1 1 d R
H93 H 0.3888 0.2374 0.5240 0.079 Uiso 1 1 d R
N10 N 0.37684(19) 0.20577(16) 0.41991(13) 0.0381(7) Uani 1 1 d .
N11 N 0.3725(2) 0.14714(16) 0.45361(14) 0.0434(7) Uani 1 1 d .
H11 H 0.3652 0.1492 0.4899 0.052 Uiso 1 1 d R
C12 C 0.3805(2) 0.0853(2) 0.42484(17) 0.0412(8) Uani 1 1 d .
O12 O 0.3938(2) 0.08631(14) 0.37345(12) 0.0522(7) Uani 1 1 d .
C13 C 0.3767(2) 0.0193(2) 0.45799(17) 0.0433(9) Uani 1 1 d .
C14 C 0.3704(3) -0.0429(2) 0.4266(2) 0.0642(13) Uani 1 1 d .
H14 H 0.3652 -0.0416 0.3872 0.077 Uiso 1 1 d R
C15 C 0.3716(4) -0.1066(2) 0.4551(2) 0.0763(16) Uani 1 1 d .
H15 H 0.3677 -0.1482 0.4345 0.092 Uiso 1 1 d R
C16 C 0.3793(3) -0.1088(3) 0.5135(2) 0.0680(14) Uani 1 1 d .
H16 H 0.3813 -0.1517 0.5325 0.082 Uiso 1 1 d R
C17 C 0.3838(3) -0.0482(2) 0.5440(2) 0.0633(13) Uani 1 1 d .
H17 H 0.3872 -0.0503 0.5835 0.076 Uiso 1 1 d R
C18 C 0.3828(3) 0.0158(2) 0.51636(19) 0.0548(11) Uani 1 1 d .
H18 H 0.3856 0.0569 0.5378 0.066 Uiso 1 1 d R
O1W O 0.3938(2) 0.10618(16) 0.26258(13) 0.0682(9) Uani 1 1 d .
N1T N 0.5267(2) 0.19084(17) 0.32923(15) 0.0506(8) Uani 1 1 d .
C1T C 0.5999(3) 0.2030(3) 0.3334(2) 0.0548(11) Uani 1 1 d .
C2T C 0.6953(3) 0.2224(4) 0.3390(3) 0.098(2) Uani 1 1 d .
N2T N 0.2462(2) 0.18404(17) 0.32570(15) 0.0505(8) Uani 1 1 d .
C3T C 0.1713(3) 0.1910(2) 0.33225(19) 0.0532(10) Uani 1 1 d .
C4T C 0.0765(3) 0.2012(4) 0.3406(3) 0.0876(18) Uani 1 1 d .
N3T N 0.3743(4) 0.1082(4) 0.1356(3) 0.119(2) Uani 1 1 d .
C5T C 0.3673(4) 0.0524(4) 0.1208(2) 0.0813(16) Uani 1 1 d .
C6T C 0.3548(6) -0.0197(4) 0.1010(3) 0.118(3) Uani 1 1 d .
Cl1 Cl 0.14617(8) 0.17336(5) 0.50911(5) 0.0571(3) Uani 1 1 d .
O1P O 0.2272(2) 0.1532(2) 0.53757(16) 0.0820(11) Uani 1 1 d .
O2P O 0.1670(3) 0.2260(2) 0.46855(18) 0.0975(13) Uani 1 1 d .
O3P O 0.1079(4) 0.1159(3) 0.4819(2) 0.129(2) Uani 1 1 d .
O4P O 0.0866(3) 0.1996(3) 0.5503(2) 0.1207(18) Uani 1 1 d .
Cl2 Cl 0.13121(7) 0.39311(6) 0.25908(6) 0.0598(3) Uani 1 1 d D
O5P O 0.0711(6) 0.3419(4) 0.2417(4) 0.1266(13) Uiso 0.50 1 d PD
O6P O 0.0879(6) 0.4519(4) 0.2713(4) 0.1266(13) Uiso 0.50 1 d PD
O7P O 0.1958(5) 0.3959(5) 0.2184(3) 0.1266(13) Uiso 0.50 1 d PD
O8P O 0.1732(6) 0.3657(5) 0.3078(3) 0.1266(13) Uiso 0.50 1 d PD
O5P' O 0.0759(6) 0.3776(5) 0.2136(3) 0.1266(13) Uiso 0.50 1 d PD
O6P' O 0.1596(6) 0.4607(3) 0.2575(4) 0.1266(13) Uiso 0.50 1 d PD
O7P' O 0.2027(5) 0.3494(4) 0.2558(5) 0.1266(13) Uiso 0.50 1 d PD
O8P' O 0.0842(6) 0.3788(5) 0.3074(3) 0.1266(13) Uiso 0.50 1 d PD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0397(3) 0.0317(3) 0.0351(3) -0.00247(19) 0.0021(2) -0.00081(17)
N1 0.0524(19) 0.0340(17) 0.067(2) 0.0132(16) -0.0004(16) -0.0019(13)
C1 0.117(5) 0.037(2) 0.090(4) 0.018(3) -0.004(3) -0.001(2)
C1A 0.0335(17) 0.0336(18) 0.058(2) 0.0041(17) -0.0018(16) -0.0017(13)
C2 0.045(2) 0.051(2) 0.065(3) 0.019(2) -0.0016(19) -0.0007(17)
O2 0.088(2) 0.065(2) 0.070(2) 0.0329(19) -0.0044(18) -0.0023(17)
N3 0.0436(17) 0.050(2) 0.0414(18) 0.0121(15) -0.0002(14) 0.0026(13)
C3 0.068(3) 0.072(3) 0.042(2) 0.014(2) -0.002(2) -0.002(2)
C4 0.0327(17) 0.043(2) 0.041(2) 0.0052(16) 0.0001(15) -0.0010(13)
C4A 0.0305(16) 0.0333(17) 0.046(2) 0.0017(15) 0.0004(14) -0.0002(12)
O4 0.0555(15) 0.0392(15) 0.0378(14) -0.0004(11) 0.0005(11) 0.0009(11)
N5 0.0365(15) 0.0312(14) 0.0401(16) 0.0010(12) 0.0022(12) -0.0023(11)
C6 0.0357(18) 0.0346(18) 0.042(2) -0.0039(15) 0.0029(15) -0.0022(13)
C7 0.047(2) 0.0355(19) 0.056(2) -0.0054(18) -0.0024(17) -0.0005(15)
C71 0.104(4) 0.045(3) 0.068(3) -0.019(2) -0.003(3) 0.004(2)
N8 0.0516(19) 0.0329(16) 0.065(2) -0.0016(16) -0.0013(16) 0.0009(13)
C9 0.0464(19) 0.0356(18) 0.0360(18) -0.0044(15) 0.0045(15) -0.0054(14)
C91 0.105(4) 0.050(3) 0.042(2) -0.006(2) 0.007(2) -0.015(2)
N10 0.0440(16) 0.0345(15) 0.0358(16) 0.0021(13) 0.0032(13) -0.0016(12)
N11 0.062(2) 0.0333(16) 0.0346(16) 0.0013(13) 0.0043(14) -0.0004(13)
C12 0.045(2) 0.0381(19) 0.041(2) -0.0003(16) 0.0016(16) -0.0009(14)
O12 0.083(2) 0.0341(13) 0.0392(15) -0.0009(12) 0.0097(14) 0.0020(12)
C13 0.051(2) 0.0354(19) 0.043(2) -0.0002(16) 0.0045(16) 0.0007(15)
C14 0.109(4) 0.038(2) 0.046(2) -0.0009(19) 0.004(2) -0.006(2)
C15 0.133(5) 0.032(2) 0.064(3) -0.004(2) 0.009(3) -0.005(2)
C16 0.104(4) 0.042(2) 0.058(3) 0.013(2) 0.010(3) 0.003(2)
C17 0.099(4) 0.047(2) 0.045(2) 0.0076(19) 0.003(2) 0.008(2)
C18 0.084(3) 0.035(2) 0.045(2) -0.0036(18) 0.003(2) 0.0055(18)
O1W 0.122(3) 0.0396(16) 0.0434(17) -0.0092(13) 0.0014(17) 0.0002(16)
N1T 0.043(2) 0.053(2) 0.055(2) -0.0007(16) 0.0038(16) 0.0057(14)
C1T 0.043(2) 0.067(3) 0.054(3) 0.004(2) 0.0036(19) 0.0027(19)
C2T 0.039(3) 0.142(6) 0.113(5) 0.004(4) -0.007(3) -0.015(3)
N2T 0.0421(19) 0.051(2) 0.059(2) -0.0033(16) -0.0025(16) -0.0062(14)
C3T 0.055(3) 0.052(2) 0.053(3) -0.0038(19) -0.006(2) -0.0041(18)
C4T 0.037(2) 0.122(5) 0.104(5) -0.014(4) -0.003(3) 0.003(3)
N3T 0.165(6) 0.096(5) 0.094(4) -0.039(4) -0.009(4) -0.011(4)
C5T 0.108(5) 0.081(4) 0.055(3) -0.008(3) -0.007(3) 0.001(3)
C6T 0.216(9) 0.066(4) 0.073(4) -0.013(3) -0.018(5) -0.004(5)
Cl1 0.0659(7) 0.0453(6) 0.0601(7) 0.0043(5) 0.0032(5) 0.0038(4)
O1P 0.064(2) 0.108(3) 0.075(2) 0.020(2) 0.0066(18) 0.013(2)
O2P 0.132(4) 0.067(2) 0.093(3) 0.026(2) -0.008(3) -0.004(2)
O3P 0.193(6) 0.067(3) 0.127(4) -0.002(3) -0.054(4) -0.032(3)
O4P 0.086(3) 0.172(5) 0.104(4) -0.010(3) 0.025(3) 0.042(3)
Cl2 0.0484(6) 0.0585(7) 0.0725(8) -0.0099(5) 0.0020(5) -0.0015(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2T Co N1T 176.70(14)
N2T Co O1W 91.69(14)
N1T Co O1W 89.96(14)
N2T Co O12 93.51(12)
N1T Co O12 89.67(12)
O1W Co O12 75.65(12)
N2T Co N5 89.16(11)
N1T Co N5 87.83(12)
O1W Co N5 144.13(13)
O12 Co N5 140.09(11)
N2T Co N10 87.75(12)
N1T Co N10 92.43(12)
O1W Co N10 146.74(12)
O12 Co N10 71.20(11)
N5 Co N10 69.13(12)
N2T Co O4 89.18(11)
N1T Co O4 88.60(11)
O1W Co O4 72.27(11)
O12 Co O4 147.88(10)
N5 Co O4 71.88(11)
N10 Co O4 140.92(10)
C1A N1 C2 122.2(4)
C1A N1 C1 120.8(4)
C2 N1 C1 117.0(4)
N8 C1A N1 120.6(4)
N8 C1A C4A 120.9(4)
N1 C1A C4A 118.5(4)
O2 C2 N1 123.0(5)
O2 C2 N3 119.2(5)
N1 C2 N3 117.9(4)
C4 N3 C2 124.1(4)
C4 N3 C3 120.1(4)
C2 N3 C3 115.8(4)
O4 C4 N3 124.5(4)
O4 C4 C4A 120.6(3)
N3 C4 C4A 114.9(3)
N5 C4A C1A 121.4(4)
N5 C4A C4 116.3(3)
C1A C4A C4 122.3(4)
C4 O4 Co 112.9(2)
C4A N5 C6 119.5(3)
C4A N5 Co 118.4(3)
C6 N5 Co 122.1(2)
N5 C6 C7 118.6(4)
N5 C6 C9 112.6(3)
C7 C6 C9 128.8(4)
N8 C7 C6 121.3(4)
N8 C7 C71 113.3(4)
C6 C7 C71 125.4(4)
C1A N8 C7 118.2(3)
N10 C9 C6 111.9(3)
N10 C9 C91 123.5(4)
C6 C9 C91 124.6(3)
C9 N10 N11 121.0(3)
C9 N10 Co 124.1(3)
N11 N10 Co 114.8(2)
C12 N11 N10 114.3(3)
O12 C12 N11 119.4(4)
O12 C12 C13 122.7(4)
N11 C12 C13 117.9(3)
C12 O12 Co 119.7(3)
C18 C13 C14 119.4(4)
C18 C13 C12 124.2(4)
C14 C13 C12 116.3(4)
C15 C14 C13 119.0(4)
C16 C15 C14 120.7(4)
C17 C16 C15 120.2(4)
C16 C17 C18 119.9(4)
C13 C18 C17 120.8(4)
C1T N1T Co 170.5(4)
N1T C1T C2T 177.4(6)
C3T N2T Co 168.5(4)
N2T C3T C4T 178.9(5)
N3T C5T C6T 177.8(8)
O3P Cl1 O4P 109.4(4)
O3P Cl1 O2P 109.7(3)
O4P Cl1 O2P 110.6(3)
O3P Cl1 O1P 110.6(3)
O4P Cl1 O1P 108.0(3)
O2P Cl1 O1P 108.4(2)
O6P' Cl2 O7P' 109.4(5)
O6P Cl2 O7P 117.9(5)
O6P' Cl2 O8P' 112.0(5)
O7P' Cl2 O8P' 109.4(5)
O6P' Cl2 O5P' 111.6(5)
O7P' Cl2 O5P' 107.3(5)
O8P' Cl2 O5P' 107.0(5)
O6P Cl2 O5P 109.8(5)
O7P Cl2 O5P 106.3(5)
O6P Cl2 O8P 110.8(5)
O7P Cl2 O8P 105.6(5)
O5P Cl2 O8P 105.7(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co N2T 2.100(4)
Co N1T 2.100(4)
Co O1W 2.142(3)
Co O12 2.149(3)
Co N5 2.173(3)
Co N10 2.200(3)
Co O4 2.364(3)
N1 C1A 1.368(5)
N1 C2 1.374(6)
N1 C1 1.463(6)
C1A N8 1.321(6)
C1A C4A 1.393(5)
C2 O2 1.206(5)
C2 N3 1.427(6)
N3 C4 1.346(5)
N3 C3 1.462(6)
C4 O4 1.222(5)
C4 C4A 1.461(5)
C4A N5 1.314(5)
N5 C6 1.348(5)
C6 C7 1.411(5)
C6 C9 1.483(5)
C7 N8 1.345(6)
C7 C71 1.483(6)
C9 N10 1.285(5)
C9 C91 1.494(6)
N10 N11 1.369(4)
N11 C12 1.362(5)
C12 O12 1.223(5)
C12 C13 1.478(5)
C13 C18 1.375(6)
C13 C14 1.396(6)
C14 C15 1.383(7)
C15 C16 1.377(7)
C16 C17 1.358(7)
C17 C18 1.380(6)
N1T C1T 1.123(5)
C1T C2T 1.480(6)
N2T C3T 1.139(6)
C3T C4T 1.446(7)
N3T C5T 1.122(8)
C5T C6T 1.459(9)
Cl1 O3P 1.389(5)
Cl1 O4P 1.406(5)
Cl1 O2P 1.416(4)
Cl1 O1P 1.436(4)
Cl2 O6P 1.323(6)
Cl2 O6P' 1.354(6)
Cl2 O7P' 1.356(6)
Cl2 O7P 1.360(6)
Cl2 O8P' 1.363(6)
Cl2 O5P' 1.384(6)
Cl2 O5P 1.386(6)
Cl2 O8P 1.406(6)
|
1500012.cif | #------------------------------------------------------------------------------
#$Date: 2016-01-24 04:15:28 +0200 (Sun, 24 Jan 2016) $
#$Revision: 174896 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500012.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_1500012
loop_
_publ_author_name
'Raj Pal Sharma'
'Rajni Sharma'
'Ritu Bala'
'Juan M. Salas'
'Miguel Quir\'os'
_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
;
Synthesis, spectroscopic characterisation and
X-ray structure of [trans-Co(en)~2~(NO~2~)~2~]~2~(Cr~2~O~7~)
;
_journal_issue 10
_journal_name_full 'Journal of Chemical Crystallography'
_journal_page_first 769
_journal_page_last 775
_journal_paper_doi 10.1007/s10870-005-3886-9
_journal_volume 35
_journal_year 2005
_chemical_formula_sum 'C8 H32 Co2 Cr2 N12 O15'
_chemical_formula_weight 758.32
_space_group_IT_number 43
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'F 2 -2d'
_symmetry_space_group_name_H-M 'F d d 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_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 8
_cell_length_a 24.778(2)
_cell_length_b 30.457(2)
_cell_length_c 6.5364(5)
_cell_measurement_reflns_used 2692
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.36
_cell_measurement_theta_min 2.68
_cell_volume 4932.8(7)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0340
_diffrn_reflns_av_sigmaI/netI 0.0456
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 39
_diffrn_reflns_limit_k_min -33
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 7639
_diffrn_reflns_theta_full 28.25
_diffrn_reflns_theta_max 28.25
_diffrn_reflns_theta_min 2.12
_diffrn_standards_decay_% 0
_diffrn_standards_number 182
_exptl_absorpt_coefficient_mu 2.273
_exptl_absorpt_correction_T_max 0.8391
_exptl_absorpt_correction_T_min 0.6620
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour dark_red
_exptl_crystal_density_diffrn 2.042
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 3088
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.08
_refine_diff_density_max 1.059
_refine_diff_density_min -0.946
_refine_diff_density_rms 0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.04(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 173
_refine_ls_number_reflns 2779
_refine_ls_number_restraints 13
_refine_ls_restrained_S_all 1.128
_refine_ls_R_factor_all 0.0660
_refine_ls_R_factor_gt 0.0617
_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^)+(0.0800P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1518
_refine_ls_wR_factor_ref 0.1550
_reflns_number_gt 2556
_reflns_number_total 2779
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file conitdcr.cif
_cod_data_source_block conitdcr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' tag value 'orthorrombic' was replaced with
'orthorhombic' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_database_code 1500012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co Co 0.44299(3) 0.36255(3) 0.37586(13) 0.0228(2) Uani 1 1 d .
N1N N 0.4014(2) 0.3803(2) 0.6120(10) 0.0411(15) Uani 1 1 d .
O1N O 0.4223(2) 0.3816(2) 0.7777(10) 0.0570(16) Uani 1 1 d .
O2N O 0.3558(3) 0.3908(5) 0.5990(10) 0.137(5) Uani 1 1 d .
N2N N 0.4828(2) 0.3423(2) 0.1365(10) 0.0364(13) Uani 1 1 d .
O3N O 0.5169(2) 0.3649(3) 0.0559(11) 0.0654(19) Uani 1 1 d .
O4N O 0.4719(4) 0.3063(2) 0.0600(10) 0.077(2) Uani 1 1 d .
N1 N 0.5027(2) 0.34451(18) 0.5515(9) 0.0274(11) Uani 1 1 d .
H11 H 0.5341 0.3546 0.5007 0.033 Uiso 1 1 d R
H12 H 0.4982 0.3558 0.6777 0.033 Uiso 1 1 d R
C1 C 0.5040(3) 0.2960(2) 0.5623(11) 0.0334(14) Uani 1 1 d .
H13 H 0.5245 0.2865 0.6808 0.040 Uiso 1 1 d R
H14 H 0.5210 0.2841 0.4407 0.040 Uiso 1 1 d R
C2 C 0.4477(3) 0.2801(3) 0.5769(12) 0.0377(16) Uani 1 1 d .
H21 H 0.4463 0.2487 0.5536 0.045 Uiso 1 1 d R
H22 H 0.4333 0.2861 0.7120 0.045 Uiso 1 1 d R
N2 N 0.4154(2) 0.3036(2) 0.4184(9) 0.0383(14) Uani 1 1 d .
H23 H 0.3807 0.3050 0.4580 0.046 Uiso 1 1 d R
H24 H 0.4168 0.2886 0.2999 0.046 Uiso 1 1 d R
N3 N 0.3842(2) 0.3810(2) 0.1951(8) 0.0303(12) Uani 1 1 d .
H31 H 0.3877 0.3680 0.0721 0.036 Uiso 1 1 d R
H32 H 0.3523 0.3729 0.2490 0.036 Uiso 1 1 d R
C3 C 0.4417(4) 0.4436(3) 0.1712(19) 0.060(3) Uani 1 1 d .
H33 H 0.4433 0.4752 0.1891 0.072 Uiso 1 1 d R
H34 H 0.4584 0.4363 0.0414 0.072 Uiso 1 1 d R
C4 C 0.3859(3) 0.4290(3) 0.1724(14) 0.047(2) Uani 1 1 d .
H41 H 0.3686 0.4375 0.0452 0.056 Uiso 1 1 d R
H42 H 0.3666 0.4429 0.2843 0.056 Uiso 1 1 d R
N4 N 0.4708(2) 0.4213(2) 0.3417(11) 0.0416(15) Uani 1 1 d .
H43 H 0.4664 0.4366 0.4584 0.050 Uiso 1 1 d R
H44 H 0.5063 0.4202 0.3134 0.050 Uiso 1 1 d R
Cr Cr 0.56056(6) 0.47649(5) 0.6988(2) 0.0570(5) Uani 1 1 d D
O1D O 0.4845(5) 0.4789(4) 0.679(2) 0.058(3) Uiso 0.50 1 d P
O2D O 0.5750(4) 0.4367(3) 0.5491(15) 0.045(2) Uiso 0.50 1 d PD
O3D O 0.5655(4) 0.4571(3) 0.9359(11) 0.041(2) Uiso 0.50 1 d PD
O4D O 0.5915(6) 0.5204(3) 0.674(2) 0.084(5) Uiso 0.50 1 d PD
O2D' O 0.5752(6) 0.4697(5) 0.4491(13) 0.076(4) Uiso 0.50 1 d PD
O3D' O 0.5430(9) 0.4306(5) 0.786(3) 0.126(8) Uiso 0.50 1 d PD
O4D' O 0.6170(4) 0.4956(4) 0.792(2) 0.069(4) Uiso 0.50 1 d PD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0143(3) 0.0335(4) 0.0205(3) -0.0039(3) 0.0022(3) 0.0000(3)
N1N 0.026(3) 0.076(5) 0.022(3) -0.008(3) -0.001(3) 0.008(3)
O1N 0.045(3) 0.088(5) 0.039(3) -0.021(3) 0.001(3) 0.014(3)
O2N 0.045(4) 0.341(16) 0.026(4) -0.012(5) 0.011(3) 0.083(7)
N2N 0.027(3) 0.058(4) 0.024(3) 0.012(3) -0.003(3) 0.014(3)
O3N 0.032(3) 0.109(6) 0.056(4) 0.016(4) 0.016(3) 0.008(3)
O4N 0.143(7) 0.049(4) 0.040(3) -0.022(3) 0.009(4) 0.024(4)
N1 0.017(2) 0.036(3) 0.029(3) -0.006(2) 0.002(2) 0.002(2)
C1 0.035(4) 0.036(3) 0.029(3) -0.003(3) 0.001(3) 0.005(3)
C2 0.037(4) 0.040(4) 0.036(4) 0.001(3) -0.008(3) -0.009(3)
N2 0.033(3) 0.048(3) 0.034(3) 0.008(3) -0.007(2) -0.015(3)
N3 0.021(3) 0.050(3) 0.020(2) -0.003(2) 0.0021(19) 0.002(2)
C3 0.053(5) 0.042(4) 0.086(8) 0.017(5) -0.022(5) -0.001(3)
C4 0.037(4) 0.049(4) 0.055(5) 0.000(4) -0.011(4) 0.015(3)
N4 0.034(3) 0.036(3) 0.055(4) 0.000(3) -0.010(3) -0.003(2)
Cr 0.0529(9) 0.0485(8) 0.0698(10) -0.0171(7) -0.0245(7) 0.0165(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N4 Co N1N 91.4(3) . .
N4 Co N2 178.4(3) . .
N1N Co N2 87.5(3) . .
N4 Co N2N 91.1(3) . .
N1N Co N2N 177.4(3) . .
N2 Co N2N 90.1(3) . .
N4 Co N1 93.4(2) . .
N1N Co N1 90.8(2) . .
N2 Co N1 85.5(2) . .
N2N Co N1 90.0(2) . .
N4 Co N3 86.0(2) . .
N1N Co N3 90.3(2) . .
N2 Co N3 95.1(2) . .
N2N Co N3 89.0(2) . .
N1 Co N3 178.8(2) . .
O2N N1N O1N 118.1(7) . .
O2N N1N Co 122.0(6) . .
O1N N1N Co 119.9(5) . .
O3N N2N O4N 118.8(7) . .
O3N N2N Co 121.5(6) . .
O4N N2N Co 119.6(6) . .
C1 N1 Co 109.0(4) . .
C2 C1 N1 108.0(6) . .
C1 C2 N2 107.7(6) . .
C2 N2 Co 110.7(4) . .
C4 N3 Co 109.0(4) . .
C4 C3 N4 108.6(8) . .
C3 C4 N3 109.3(6) . .
C3 N4 Co 109.6(5) . .
O4D Cr O2D 118.6(7) . .
O3D' Cr O4D' 114.8(8) . .
O4D Cr O3D 111.5(6) . .
O2D Cr O3D 106.6(5) . .
O3D' Cr O2D' 107.6(8) . .
O4D' Cr O2D' 102.7(6) . .
O3D' Cr O1D 122.4(10) . 2_665
O4D' Cr O1D 107.2(7) . 2_665
O2D' Cr O1D 99.2(7) . 2_665
O4D Cr O1D 116.9(7) . .
O2D Cr O1D 102.2(6) . .
O3D Cr O1D 98.7(6) . .
Cr O1D Cr 131.0(7) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N4 1.930(6) .
Co N1N 1.933(6) .
Co N2 1.940(6) .
Co N2N 1.949(6) .
Co N1 1.952(5) .
Co N3 1.958(6) .
N1N O2N 1.175(8) .
N1N O1N 1.202(9) .
N2N O3N 1.210(9) .
N2N O4N 1.237(9) .
N1 C1 1.481(9) .
C1 C2 1.478(10) .
C2 N2 1.493(9) .
N3 C4 1.472(10) .
C3 C4 1.451(11) .
C3 N4 1.491(11) .
Cr O4D 1.549(8) .
Cr O3D' 1.571(9) .
Cr O2D 1.597(7) .
Cr O4D' 1.633(8) .
Cr O3D 1.663(7) .
Cr O2D' 1.684(8) .
Cr O1D 1.765(13) 2_665
Cr O1D 1.889(13) .
|
1500013.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500013.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_1500013
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_sum 'C22 H20 Cl2 Cu N10 O10'
_chemical_formula_weight 718.92
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 75.465(1)
_cell_angle_beta 71.674(1)
_cell_angle_gamma 78.059(1)
_cell_formula_units_Z 2
_cell_length_a 9.5677(5)
_cell_length_b 12.4114(6)
_cell_length_c 13.3517(6)
_cell_measurement_reflns_used 5826
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.3
_cell_volume 1442.71(12)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0172
_diffrn_reflns_av_sigmaI/netI 0.0208
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 16853
_diffrn_reflns_theta_full 26.90
_diffrn_reflns_theta_max 28.32
_diffrn_reflns_theta_min 1.64
_diffrn_standards_decay_% 0
_diffrn_standards_number 440
_exptl_absorpt_coefficient_mu 1.015
_exptl_absorpt_correction_T_max 0.8305
_exptl_absorpt_correction_T_min 0.7330
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.655
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 730
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.19
_refine_diff_density_max 1.890
_refine_diff_density_min -0.419
_refine_diff_density_rms 0.068
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 418
_refine_ls_number_reflns 6543
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.051
_refine_ls_R_factor_all 0.0321
_refine_ls_R_factor_gt 0.0306
_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^)+(0.0400P)^2^+1.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0817
_refine_ls_wR_factor_ref 0.0826
_reflns_number_gt 6186
_reflns_number_total 6543
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file CuDEA_compound1.cif
_cod_data_source_block cutpph
_cod_database_code 1500013
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
Cu Cu 0.37605(2) 0.316111(16) 0.283951(16) 0.01365(7) Uani 1 1 d .
N1A N 0.54811(17) 0.34146(13) 0.53032(12) 0.0192(3) Uani 1 1 d .
C2A C 0.4487(2) 0.36182(15) 0.47551(14) 0.0171(3) Uani 1 1 d .
H2A H 0.3549 0.4062 0.4967 0.020 Uiso 1 1 d R
N3A N 0.48899(16) 0.31493(12) 0.38728(12) 0.0151(3) Uani 1 1 d .
C3AA C 0.62682(19) 0.26071(14) 0.38511(14) 0.0151(3) Uani 1 1 d .
N4A N 0.71777(17) 0.20130(13) 0.31332(13) 0.0201(3) Uani 1 1 d .
C5A C 0.8481(2) 0.15784(17) 0.33177(16) 0.0241(4) Uani 1 1 d .
H5A H 0.9170 0.1149 0.2829 0.029 Uiso 1 1 d R
C6A C 0.8914(2) 0.17124(17) 0.41931(17) 0.0244(4) Uani 1 1 d .
H6A H 0.9866 0.1379 0.4283 0.029 Uiso 1 1 d R
C7A C 0.7954(2) 0.23218(16) 0.49044(15) 0.0212(4) Uani 1 1 d .
H7A H 0.8204 0.2432 0.5503 0.025 Uiso 1 1 d R
N8A N 0.66225(16) 0.27662(12) 0.47142(12) 0.0155(3) Uani 1 1 d .
N1B N 0.41942(17) -0.02958(13) 0.42031(12) 0.0180(3) Uani 1 1 d .
C2B C 0.3616(2) 0.07704(15) 0.41557(14) 0.0171(3) Uani 1 1 d .
H2B H 0.2936 0.1036 0.4763 0.021 Uiso 1 1 d R
N3B N 0.40527(17) 0.14655(12) 0.31825(12) 0.0158(3) Uani 1 1 d .
C3AB C 0.49958(19) 0.07794(14) 0.25569(14) 0.0156(3) Uani 1 1 d .
N4B N 0.57651(18) 0.10253(13) 0.15214(12) 0.0199(3) Uani 1 1 d .
C5B C 0.6647(2) 0.01680(17) 0.11249(16) 0.0243(4) Uani 1 1 d .
H5B H 0.7217 0.0308 0.0392 0.029 Uiso 1 1 d R
C6B C 0.6793(2) -0.09408(16) 0.17266(16) 0.0237(4) Uani 1 1 d .
H6B H 0.7455 -0.1522 0.1404 0.028 Uiso 1 1 d R
C7B C 0.5977(2) -0.11680(15) 0.27699(15) 0.0195(4) Uani 1 1 d .
H7B H 0.6029 -0.1906 0.3196 0.023 Uiso 1 1 d R
N8B N 0.50829(17) -0.02847(12) 0.31729(12) 0.0154(3) Uani 1 1 d .
N1F N 0.39608(16) 0.47892(12) 0.21217(12) 0.0150(3) Uani 1 1 d .
C1AF C 0.34600(18) 0.51089(14) 0.12303(13) 0.0145(3) Uani 1 1 d .
C2F C 0.4513(2) 0.55437(15) 0.23878(15) 0.0187(3) Uani 1 1 d .
H2F H 0.4859 0.5333 0.3013 0.022 Uiso 1 1 d R
C3F C 0.4602(2) 0.66348(15) 0.17797(15) 0.0207(4) Uani 1 1 d .
H3F H 0.5006 0.7150 0.1993 0.025 Uiso 1 1 d R
C4F C 0.4106(2) 0.69634(15) 0.08765(15) 0.0196(4) Uani 1 1 d .
H4F H 0.4172 0.7702 0.0457 0.024 Uiso 1 1 d R
C4AF C 0.34980(19) 0.61888(14) 0.05782(14) 0.0167(3) Uani 1 1 d .
C5F C 0.2908(2) 0.64436(16) -0.03339(15) 0.0202(4) Uani 1 1 d .
H5F H 0.2938 0.7169 -0.0785 0.024 Uiso 1 1 d R
C6F C 0.2308(2) 0.56662(16) -0.05623(14) 0.0202(4) Uani 1 1 d .
H6F H 0.1924 0.5856 -0.1169 0.024 Uiso 1 1 d R
C6AF C 0.22445(19) 0.45574(15) 0.01009(14) 0.0168(3) Uani 1 1 d .
C7F C 0.1590(2) 0.37222(16) -0.00611(14) 0.0196(4) Uani 1 1 d .
H7F H 0.1157 0.3868 -0.0640 0.024 Uiso 1 1 d R
C8F C 0.1582(2) 0.26929(16) 0.06305(15) 0.0208(4) Uani 1 1 d .
H8F H 0.1133 0.2124 0.0537 0.025 Uiso 1 1 d R
C9F C 0.2242(2) 0.24861(15) 0.14746(15) 0.0193(4) Uani 1 1 d .
H9F H 0.2242 0.1768 0.1940 0.023 Uiso 1 1 d R
N10F N 0.28655(16) 0.32609(12) 0.16435(12) 0.0153(3) Uani 1 1 d .
C0AF C 0.28526(18) 0.42844(14) 0.09778(13) 0.0144(3) Uani 1 1 d .
Cl1 Cl 0.18743(5) 0.93949(3) 0.21971(3) 0.01784(9) Uani 1 1 d .
O1P O 0.16174(16) 0.99545(12) 0.30794(11) 0.0257(3) Uani 1 1 d .
O2P O 0.33946(16) 0.93915(13) 0.15600(12) 0.0282(3) Uani 1 1 d .
O3P O 0.15743(16) 0.82463(12) 0.26319(12) 0.0259(3) Uani 1 1 d .
O4P O 0.09018(17) 0.99710(13) 0.15398(12) 0.0300(3) Uani 1 1 d .
Cl2 Cl 0.13764(5) 0.46846(3) 0.69814(3) 0.01719(9) Uani 1 1 d .
O5P O 0.10877(18) 0.49621(13) 0.59412(12) 0.0317(3) Uani 1 1 d .
O6P O 0.2013(2) 0.35206(13) 0.71947(14) 0.0360(4) Uani 1 1 d .
O7P O 0.2430(2) 0.53439(16) 0.69848(16) 0.0511(5) Uani 1 1 d .
O8P O 0.0045(2) 0.4890(2) 0.77924(14) 0.0584(6) Uani 1 1 d .
O1W O 0.16085(15) 0.33922(12) 0.40365(11) 0.0234(3) Uani 1 1 d D
H11W H 0.140(3) 0.3062(19) 0.4692(9) 0.028 Uiso 1 1 d D
H12W H 0.090(2) 0.3914(15) 0.400(2) 0.028 Uiso 1 1 d D
O2W O 0.12961(16) 0.21450(12) 0.60665(11) 0.0249(3) Uani 1 1 d D
H21W H 0.148(3) 0.2552(18) 0.6423(18) 0.030 Uiso 1 1 d D
H22W H 0.0485(17) 0.191(2) 0.6463(18) 0.030 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 0.01760(11) 0.01053(11) 0.01445(11) -0.00187(8) -0.00817(8) -0.00043(8)
N1A 0.0210(8) 0.0195(7) 0.0181(7) -0.0058(6) -0.0069(6) -0.0003(6)
C2A 0.0190(8) 0.0155(8) 0.0164(8) -0.0035(6) -0.0056(7) -0.0001(6)
N3A 0.0179(7) 0.0126(7) 0.0156(7) -0.0031(5) -0.0068(6) 0.0000(5)
C3AA 0.0172(8) 0.0138(8) 0.0154(8) -0.0011(6) -0.0069(6) -0.0029(6)
N4A 0.0190(7) 0.0210(8) 0.0204(8) -0.0072(6) -0.0056(6) 0.0005(6)
C5A 0.0188(9) 0.0262(10) 0.0273(10) -0.0098(8) -0.0059(7) 0.0016(7)
C6A 0.0172(9) 0.0266(10) 0.0305(10) -0.0054(8) -0.0107(8) 0.0007(7)
C7A 0.0218(9) 0.0216(9) 0.0228(9) -0.0008(7) -0.0122(7) -0.0036(7)
N8A 0.0182(7) 0.0143(7) 0.0147(7) -0.0015(5) -0.0069(6) -0.0018(5)
N1B 0.0228(8) 0.0167(7) 0.0150(7) -0.0013(6) -0.0071(6) -0.0035(6)
C2B 0.0201(8) 0.0170(8) 0.0163(8) -0.0031(7) -0.0076(7) -0.0031(6)
N3B 0.0191(7) 0.0135(7) 0.0156(7) -0.0018(5) -0.0074(6) -0.0018(5)
C3AB 0.0194(8) 0.0125(8) 0.0171(8) -0.0008(6) -0.0095(7) -0.0027(6)
N4B 0.0253(8) 0.0162(7) 0.0168(7) -0.0013(6) -0.0055(6) -0.0029(6)
C5B 0.0289(10) 0.0224(9) 0.0181(9) -0.0039(7) -0.0027(7) -0.0027(8)
C6B 0.0271(10) 0.0183(9) 0.0242(9) -0.0066(7) -0.0062(8) 0.0019(7)
C7B 0.0234(9) 0.0135(8) 0.0223(9) -0.0026(7) -0.0097(7) 0.0001(7)
N8B 0.0198(7) 0.0122(7) 0.0153(7) -0.0011(5) -0.0076(6) -0.0025(5)
N1F 0.0165(7) 0.0129(7) 0.0157(7) -0.0030(5) -0.0055(5) 0.0000(5)
C1AF 0.0133(7) 0.0148(8) 0.0135(7) -0.0037(6) -0.0024(6) 0.0011(6)
C2F 0.0217(9) 0.0172(8) 0.0190(8) -0.0048(7) -0.0084(7) -0.0006(7)
C3F 0.0242(9) 0.0154(8) 0.0240(9) -0.0061(7) -0.0065(7) -0.0039(7)
C4F 0.0224(9) 0.0133(8) 0.0194(9) -0.0015(7) -0.0023(7) -0.0019(7)
C4AF 0.0164(8) 0.0149(8) 0.0153(8) -0.0015(6) -0.0019(6) -0.0002(6)
C5F 0.0222(9) 0.0185(8) 0.0161(8) 0.0016(7) -0.0048(7) -0.0012(7)
C6F 0.0210(9) 0.0244(9) 0.0126(8) -0.0002(7) -0.0056(7) -0.0001(7)
C6AF 0.0149(8) 0.0200(8) 0.0137(8) -0.0039(6) -0.0035(6) 0.0011(6)
C7F 0.0194(9) 0.0249(9) 0.0159(8) -0.0050(7) -0.0075(7) -0.0009(7)
C8F 0.0240(9) 0.0213(9) 0.0213(9) -0.0059(7) -0.0100(7) -0.0046(7)
C9F 0.0240(9) 0.0155(8) 0.0208(9) -0.0032(7) -0.0098(7) -0.0029(7)
N10F 0.0171(7) 0.0137(7) 0.0160(7) -0.0030(5) -0.0069(6) -0.0004(5)
C0AF 0.0134(8) 0.0143(8) 0.0139(8) -0.0037(6) -0.0028(6) 0.0010(6)
Cl1 0.0185(2) 0.0167(2) 0.0188(2) -0.00473(15) -0.00561(16) -0.00145(15)
O1P 0.0324(8) 0.0243(7) 0.0238(7) -0.0109(6) -0.0108(6) 0.0005(6)
O2P 0.0210(7) 0.0290(8) 0.0325(8) -0.0085(6) -0.0006(6) -0.0066(6)
O3P 0.0272(7) 0.0186(7) 0.0303(7) -0.0050(6) -0.0040(6) -0.0057(5)
O4P 0.0327(8) 0.0330(8) 0.0276(7) -0.0066(6) -0.0179(6) 0.0039(6)
Cl2 0.0176(2) 0.0181(2) 0.01418(19) -0.00351(15) -0.00462(15) 0.00195(15)
O5P 0.0396(9) 0.0352(8) 0.0216(7) -0.0112(6) -0.0184(6) 0.0139(7)
O6P 0.0536(10) 0.0203(7) 0.0411(9) -0.0090(7) -0.0302(8) 0.0100(7)
O7P 0.0705(13) 0.0400(10) 0.0561(12) 0.0151(9) -0.0401(11) -0.0315(9)
O8P 0.0293(9) 0.0929(16) 0.0267(9) -0.0053(9) 0.0021(7) 0.0254(10)
O1W 0.0192(7) 0.0273(7) 0.0196(6) -0.0020(6) -0.0065(5) 0.0044(5)
O2W 0.0260(7) 0.0267(7) 0.0214(7) -0.0048(6) -0.0034(6) -0.0069(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu 0.3201 1.2651 '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
N3A Cu N10F 172.05(6)
N3A Cu N3B 89.43(6)
N10F Cu N3B 93.65(6)
N3A Cu N1F 93.29(6)
N10F Cu N1F 81.71(6)
N3B Cu N1F 163.53(6)
N3A Cu O1W 92.76(6)
N10F Cu O1W 94.17(6)
N3B Cu O1W 96.52(6)
N1F Cu O1W 99.57(6)
C2A N1A N8A 101.78(14)
N1A C2A N3A 115.72(16)
N1A C2A H2A 122.2
N3A C2A H2A 122.1
C3AA N3A C2A 103.70(14)
C3AA N3A Cu 125.72(12)
C2A N3A Cu 130.54(12)
N4A C3AA N3A 128.17(16)
N4A C3AA N8A 123.91(16)
N3A C3AA N8A 107.92(15)
C5A N4A C3AA 114.55(16)
N4A C5A C6A 124.28(18)
N4A C5A H5A 117.9
C6A C5A H5A 117.8
C7A C6A C5A 119.22(17)
C7A C6A H6A 120.4
C5A C6A H6A 120.4
N8A C7A C6A 116.42(17)
N8A C7A H7A 121.8
C6A C7A H7A 121.8
C7A N8A C3AA 121.62(16)
C7A N8A N1A 127.51(15)
C3AA N8A N1A 110.87(14)
C2B N1B N8B 101.78(14)
N1B C2B N3B 115.80(16)
N1B C2B H2B 122.1
N3B C2B H2B 122.1
C3AB N3B C2B 103.73(14)
C3AB N3B Cu 126.72(12)
C2B N3B Cu 128.11(12)
N4B C3AB N3B 129.12(16)
N4B C3AB N8B 123.03(16)
N3B C3AB N8B 107.84(15)
C5B N4B C3AB 115.37(16)
N4B C5B C6B 123.91(18)
N4B C5B H5B 118.0
C6B C5B H5B 118.0
C7B C6B C5B 119.34(18)
C7B C6B H6B 120.3
C5B C6B H6B 120.3
C6B C7B N8B 116.44(17)
C6B C7B H7B 121.8
N8B C7B H7B 121.7
C7B N8B N1B 127.25(15)
C7B N8B C3AB 121.89(15)
N1B N8B C3AB 110.84(14)
C2F N1F C1AF 118.01(15)
C2F N1F Cu 129.81(12)
C1AF N1F Cu 112.17(11)
N1F C1AF C4AF 123.45(16)
N1F C1AF C0AF 116.55(15)
C4AF C1AF C0AF 120.00(16)
N1F C2F C3F 122.29(17)
N1F C2F H2F 118.9
C3F C2F H2F 118.9
C4F C3F C2F 120.12(17)
C4F C3F H3F 119.9
C2F C3F H3F 120.0
C3F C4F C4AF 119.07(16)
C3F C4F H4F 120.5
C4AF C4F H4F 120.5
C1AF C4AF C4F 117.05(16)
C1AF C4AF C5F 118.77(16)
C4F C4AF C5F 124.17(16)
C6F C5F C4AF 121.19(17)
C6F C5F H5F 119.4
C4AF C5F H5F 119.4
C5F C6F C6AF 120.99(16)
C5F C6F H6F 119.5
C6AF C6F H6F 119.5
C0AF C6AF C7F 117.22(16)
C0AF C6AF C6F 118.57(16)
C7F C6AF C6F 124.21(16)
C8F C7F C6AF 119.18(16)
C8F C7F H7F 120.4
C6AF C7F H7F 120.4
C7F C8F C9F 119.73(17)
C7F C8F H8F 120.1
C9F C8F H8F 120.1
N10F C9F C8F 122.15(17)
N10F C9F H9F 118.9
C8F C9F H9F 118.9
C9F N10F C0AF 118.48(15)
C9F N10F Cu 128.21(12)
C0AF N10F Cu 113.21(11)
N10F C0AF C6AF 123.21(16)
N10F C0AF C1AF 116.32(15)
C6AF C0AF C1AF 120.43(16)
O2P Cl1 O4P 109.76(9)
O2P Cl1 O1P 109.67(9)
O4P Cl1 O1P 109.58(9)
O2P Cl1 O3P 109.32(9)
O4P Cl1 O3P 109.67(9)
O1P Cl1 O3P 108.83(9)
O8P Cl2 O7P 109.38(15)
O8P Cl2 O6P 110.24(12)
O7P Cl2 O6P 107.48(11)
O8P Cl2 O5P 110.14(10)
O7P Cl2 O5P 109.97(11)
O6P Cl2 O5P 109.59(9)
Cu O1W H11W 126.0(17)
Cu O1W H12W 127.9(17)
H11W O1W H12W 105(2)
H21W O2W H22W 104(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu N3A 1.9980(14)
Cu N10F 2.0039(14)
Cu N3B 2.0175(15)
Cu N1F 2.0276(15)
Cu O1W 2.1891(14)
N1A C2A 1.323(2)
N1A N8A 1.368(2)
C2A N3A 1.357(2)
C2A H2A 0.9500
N3A C3AA 1.346(2)
C3AA N4A 1.336(2)
C3AA N8A 1.367(2)
N4A C5A 1.324(2)
C5A C6A 1.413(3)
C5A H5A 0.9500
C6A C7A 1.357(3)
C6A H6A 0.9500
C7A N8A 1.355(2)
C7A H7A 0.9500
N1B C2B 1.318(2)
N1B N8B 1.369(2)
C2B N3B 1.361(2)
C2B H2B 0.9500
N3B C3AB 1.342(2)
C3AB N4B 1.337(2)
C3AB N8B 1.371(2)
N4B C5B 1.325(2)
C5B C6B 1.412(3)
C5B H5B 0.9500
C6B C7B 1.356(3)
C6B H6B 0.9500
C7B N8B 1.357(2)
C7B H7B 0.9500
N1F C2F 1.331(2)
N1F C1AF 1.359(2)
C1AF C4AF 1.404(2)
C1AF C0AF 1.429(2)
C2F C3F 1.397(3)
C2F H2F 0.9500
C3F C4F 1.371(3)
C3F H3F 0.9500
C4F C4AF 1.411(3)
C4F H4F 0.9500
C4AF C5F 1.438(2)
C5F C6F 1.357(3)
C5F H5F 0.9500
C6F C6AF 1.439(3)
C6F H6F 0.9500
C6AF C0AF 1.404(2)
C6AF C7F 1.407(3)
C7F C8F 1.376(3)
C7F H7F 0.9500
C8F C9F 1.404(2)
C8F H8F 0.9500
C9F N10F 1.327(2)
C9F H9F 0.9500
N10F C0AF 1.356(2)
Cl1 O2P 1.4355(14)
Cl1 O4P 1.4390(14)
Cl1 O1P 1.4452(14)
Cl1 O3P 1.4494(14)
Cl2 O8P 1.4131(17)
Cl2 O7P 1.4252(17)
Cl2 O6P 1.4415(15)
Cl2 O5P 1.4442(14)
O1W H11W 0.848(10)
O1W H12W 0.841(10)
O2W H21W 0.851(10)
O2W H22W 0.850(10)
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
O1W H11W O2W 0.848(10) 1.886(11) 2.722(2) 169(2) .
O1W H12W O5P 0.841(10) 2.103(11) 2.938(2) 171(2) 2_566
O2W H22W O3P 0.850(10) 1.981(11) 2.815(2) 166(2) 2_566
O2W H21W O6P 0.851(10) 1.992(10) 2.842(2) 177(3) .
|
1500014.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500014.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_1500014
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_sum 'C26 H26 Cl2 Cu N10 O9'
_chemical_formula_weight 757.01
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 102.712(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.1033(5)
_cell_length_b 18.1364(7)
_cell_length_c 14.2061(5)
_cell_measurement_reflns_used 9783
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.39
_cell_measurement_theta_min 2.25
_cell_volume 3041.9(2)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0220
_diffrn_reflns_av_sigmaI/netI 0.0179
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 34972
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.39
_diffrn_reflns_theta_min 1.72
_diffrn_standards_decay_% 0
_diffrn_standards_number 766
_exptl_absorpt_coefficient_mu 0.965
_exptl_absorpt_correction_T_max 0.7944
_exptl_absorpt_correction_T_min 0.7122
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.653
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregularly shaped block'
_exptl_crystal_F_000 1548
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.468
_refine_diff_density_min -0.385
_refine_diff_density_rms 0.063
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 443
_refine_ls_number_reflns 7160
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.012
_refine_ls_R_factor_all 0.0306
_refine_ls_R_factor_gt 0.0284
_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^)+(0.0450P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0767
_refine_ls_wR_factor_ref 0.0781
_reflns_number_gt 6646
_reflns_number_total 7160
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file CuDEA_compound2.cif
_cod_data_source_block cuphdmtp
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500014
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
Cu Cu 0.591893(14) 0.566133(9) 0.269184(12) 0.01250(6) Uani 1 1 d .
N1A N 0.64779(11) 0.43615(7) 0.04136(9) 0.0153(2) Uani 1 1 d .
C2A C 0.59005(13) 0.46540(8) 0.10045(11) 0.0153(3) Uani 1 1 d .
H2A H 0.5099 0.4617 0.0895 0.018 Uiso 1 1 d R
N3A N 0.65260(10) 0.50130(7) 0.17811(9) 0.0147(2) Uani 1 1 d .
C3AA C 0.76000(12) 0.49440(8) 0.16683(10) 0.0143(3) Uani 1 1 d .
N4A N 0.85547(11) 0.51995(7) 0.22343(9) 0.0160(2) Uani 1 1 d .
C5A C 0.94988(13) 0.50593(8) 0.19337(11) 0.0170(3) Uani 1 1 d .
C51A C 1.05789(14) 0.53719(10) 0.25270(12) 0.0230(3) Uani 1 1 d .
H51A H 1.0714 0.5860 0.2279 0.028 Uiso 1 1 d R
H52A H 1.1211 0.5044 0.2488 0.028 Uiso 1 1 d R
H53A H 1.0516 0.5415 0.3201 0.028 Uiso 1 1 d R
C6A C 0.95121(13) 0.46437(8) 0.10906(11) 0.0175(3) Uani 1 1 d .
H6A H 1.0211 0.4552 0.0912 0.021 Uiso 1 1 d R
C7A C 0.85299(13) 0.43734(8) 0.05312(11) 0.0162(3) Uani 1 1 d .
C71A C 0.84199(14) 0.39134(9) -0.03506(11) 0.0212(3) Uani 1 1 d .
H71A H 0.9175 0.3804 -0.0459 0.025 Uiso 1 1 d R
H72A H 0.7979 0.4181 -0.0907 0.025 Uiso 1 1 d R
H73A H 0.8034 0.3451 -0.0266 0.025 Uiso 1 1 d R
N8A N 0.75701(10) 0.45503(7) 0.08412(9) 0.0141(2) Uani 1 1 d .
N1B N 0.81040(12) 0.72520(7) 0.19861(10) 0.0194(3) Uani 1 1 d .
C2B C 0.71738(13) 0.68528(8) 0.18597(11) 0.0175(3) Uani 1 1 d .
H2B H 0.6611 0.6866 0.1277 0.021 Uiso 1 1 d R
N3B N 0.70721(11) 0.64212(7) 0.26199(9) 0.0151(2) Uani 1 1 d .
C3AB C 0.80302(13) 0.65476(8) 0.32781(11) 0.0157(3) Uani 1 1 d .
N4B N 0.83717(12) 0.62472(8) 0.41528(10) 0.0209(3) Uani 1 1 d .
C5B C 0.93812(15) 0.64669(10) 0.46488(12) 0.0256(4) Uani 1 1 d .
C51B C 0.9816(2) 0.61130(14) 0.56133(15) 0.0452(6) Uani 1 1 d .
H51B H 0.9273 0.6192 0.6024 0.054 Uiso 1 1 d R
H52B H 1.0546 0.6332 0.5920 0.054 Uiso 1 1 d R
H53B H 0.9912 0.5583 0.5526 0.054 Uiso 1 1 d R
C6B C 1.00474(14) 0.69972(10) 0.42906(12) 0.0241(3) Uani 1 1 d .
H6B H 1.0761 0.7141 0.4674 0.029 Uiso 1 1 d R
C7B C 0.96707(13) 0.73023(8) 0.34004(12) 0.0194(3) Uani 1 1 d .
C71B C 1.02394(16) 0.78730(10) 0.29288(14) 0.0281(4) Uani 1 1 d .
H71B H 1.0359 0.7684 0.2313 0.034 Uiso 1 1 d R
H72B H 1.0972 0.7997 0.3350 0.034 Uiso 1 1 d R
H73B H 0.9764 0.8315 0.2813 0.034 Uiso 1 1 d R
N8B N 0.86515(11) 0.70471(7) 0.28987(9) 0.0160(2) Uani 1 1 d .
N1F N 0.49477(10) 0.48688(7) 0.31087(9) 0.0145(2) Uani 1 1 d .
C1AF C 0.43000(12) 0.51410(8) 0.37032(10) 0.0142(3) Uani 1 1 d .
C2F C 0.48474(13) 0.41590(8) 0.28756(11) 0.0167(3) Uani 1 1 d .
H2F H 0.5307 0.3961 0.2474 0.020 Uiso 1 1 d R
C3F C 0.40848(13) 0.36908(8) 0.32031(11) 0.0186(3) Uani 1 1 d .
H3F H 0.4031 0.3186 0.3020 0.022 Uiso 1 1 d R
C4F C 0.34196(13) 0.39645(8) 0.37877(11) 0.0181(3) Uani 1 1 d .
H4F H 0.2894 0.3654 0.4004 0.022 Uiso 1 1 d R
C4AF C 0.35225(12) 0.47134(8) 0.40660(11) 0.0157(3) Uani 1 1 d .
C5F C 0.28970(13) 0.50510(9) 0.47008(11) 0.0189(3) Uani 1 1 d .
H5F H 0.2378 0.4763 0.4959 0.023 Uiso 1 1 d R
C6F C 0.30353(13) 0.57753(9) 0.49386(11) 0.0186(3) Uani 1 1 d .
H6F H 0.2599 0.5989 0.5348 0.022 Uiso 1 1 d R
C6AF C 0.38299(12) 0.62229(8) 0.45802(10) 0.0154(3) Uani 1 1 d .
C7F C 0.40320(13) 0.69750(9) 0.48123(11) 0.0179(3) Uani 1 1 d .
H7F H 0.3606 0.7222 0.5204 0.021 Uiso 1 1 d R
C8F C 0.48472(13) 0.73447(8) 0.44677(11) 0.0176(3) Uani 1 1 d .
H8F H 0.4995 0.7850 0.4623 0.021 Uiso 1 1 d R
C9F C 0.54620(13) 0.69726(8) 0.38835(11) 0.0160(3) Uani 1 1 d .
H9F H 0.6033 0.7233 0.3656 0.019 Uiso 1 1 d R
N10F N 0.52756(10) 0.62683(7) 0.36370(9) 0.0139(2) Uani 1 1 d .
C0AF C 0.44667(12) 0.59002(8) 0.39773(10) 0.0140(3) Uani 1 1 d .
Cl1 Cl 0.28456(3) 0.765442(19) 0.21812(2) 0.01584(8) Uani 1 1 d .
O1P O 0.39800(9) 0.75423(7) 0.20161(8) 0.0217(2) Uani 1 1 d .
O2P O 0.28745(11) 0.82669(7) 0.28280(9) 0.0273(3) Uani 1 1 d .
O3P O 0.24803(11) 0.69956(7) 0.25817(9) 0.0271(3) Uani 1 1 d .
O4P O 0.20919(10) 0.78174(7) 0.12680(8) 0.0250(3) Uani 1 1 d .
Cl2 Cl 0.24528(3) 0.382117(19) 0.06476(3) 0.01715(8) Uani 1 1 d .
O5P O 0.24045(12) 0.44431(7) 0.12682(10) 0.0320(3) Uani 1 1 d .
O6P O 0.24754(11) 0.31478(7) 0.11826(10) 0.0308(3) Uani 1 1 d .
O7P O 0.34702(11) 0.38720(7) 0.02751(10) 0.0300(3) Uani 1 1 d .
O8P O 0.14822(11) 0.38314(8) -0.01422(10) 0.0313(3) Uani 1 1 d .
O1W O 0.46604(10) 0.61663(7) 0.14680(8) 0.0222(2) Uani 1 1 d D
H11W H 0.4349(17) 0.6541(8) 0.1631(15) 0.027 Uiso 1 1 d D
H12W H 0.4300(16) 0.6013(11) 0.0942(9) 0.027 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 0.01223(9) 0.01259(10) 0.01304(10) -0.00158(6) 0.00356(7) -0.00195(6)
N1A 0.0149(6) 0.0151(6) 0.0146(6) 0.0001(5) 0.0006(5) -0.0002(4)
C2A 0.0166(7) 0.0134(7) 0.0155(7) 0.0005(5) 0.0024(5) -0.0005(5)
N3A 0.0143(6) 0.0146(6) 0.0150(6) -0.0002(5) 0.0028(5) -0.0005(4)
C3AA 0.0172(7) 0.0126(6) 0.0131(6) 0.0010(5) 0.0033(5) 0.0011(5)
N4A 0.0145(6) 0.0175(6) 0.0156(6) -0.0006(5) 0.0022(5) 0.0005(5)
C5A 0.0162(7) 0.0167(7) 0.0174(7) 0.0019(6) 0.0023(5) 0.0009(5)
C51A 0.0155(7) 0.0300(9) 0.0226(8) -0.0040(7) 0.0022(6) -0.0010(6)
C6A 0.0163(7) 0.0175(7) 0.0195(7) 0.0013(6) 0.0060(6) 0.0033(5)
C7A 0.0192(7) 0.0141(7) 0.0159(7) 0.0026(5) 0.0052(6) 0.0044(5)
C71A 0.0235(8) 0.0209(8) 0.0194(8) -0.0047(6) 0.0052(6) 0.0034(6)
N8A 0.0154(6) 0.0131(6) 0.0129(6) 0.0001(5) 0.0012(5) 0.0006(4)
N1B 0.0240(7) 0.0165(6) 0.0188(6) 0.0002(5) 0.0073(5) -0.0016(5)
C2B 0.0198(7) 0.0157(7) 0.0180(7) -0.0007(6) 0.0065(6) 0.0004(5)
N3B 0.0154(6) 0.0145(6) 0.0161(6) -0.0022(5) 0.0046(5) -0.0017(5)
C3AB 0.0163(7) 0.0141(7) 0.0183(7) -0.0037(5) 0.0069(6) -0.0035(5)
N4B 0.0214(7) 0.0243(7) 0.0167(6) -0.0009(5) 0.0033(5) -0.0092(5)
C5B 0.0257(8) 0.0301(9) 0.0198(8) -0.0016(7) 0.0021(6) -0.0106(7)
C51B 0.0422(12) 0.0595(14) 0.0257(10) 0.0106(9) -0.0100(8) -0.0272(11)
C6B 0.0189(8) 0.0266(8) 0.0262(8) -0.0056(7) 0.0034(6) -0.0096(6)
C7B 0.0192(7) 0.0168(7) 0.0248(8) -0.0072(6) 0.0102(6) -0.0061(6)
C71B 0.0279(9) 0.0259(8) 0.0340(9) -0.0044(7) 0.0148(7) -0.0129(7)
N8B 0.0181(6) 0.0137(6) 0.0181(6) -0.0024(5) 0.0078(5) -0.0024(5)
N1F 0.0132(6) 0.0150(6) 0.0145(6) 0.0004(5) 0.0016(4) -0.0009(4)
C1AF 0.0125(6) 0.0157(7) 0.0129(6) 0.0013(5) -0.0001(5) -0.0009(5)
C2F 0.0175(7) 0.0161(7) 0.0156(7) 0.0001(6) 0.0016(5) 0.0001(5)
C3F 0.0192(7) 0.0135(7) 0.0213(7) 0.0011(6) 0.0002(6) -0.0028(5)
C4F 0.0163(7) 0.0169(7) 0.0197(7) 0.0039(6) 0.0010(6) -0.0039(5)
C4AF 0.0132(6) 0.0181(7) 0.0144(7) 0.0027(5) -0.0002(5) -0.0012(5)
C5F 0.0150(7) 0.0242(8) 0.0181(7) 0.0045(6) 0.0046(6) -0.0022(6)
C6F 0.0158(7) 0.0252(8) 0.0157(7) 0.0015(6) 0.0054(6) 0.0012(6)
C6AF 0.0145(7) 0.0188(7) 0.0122(6) 0.0011(5) 0.0012(5) 0.0005(5)
C7F 0.0199(7) 0.0200(7) 0.0138(7) -0.0016(6) 0.0039(6) 0.0026(6)
C8F 0.0217(7) 0.0153(7) 0.0145(7) -0.0020(5) 0.0014(6) -0.0005(6)
C9F 0.0164(7) 0.0159(7) 0.0153(7) 0.0010(5) 0.0024(5) -0.0024(5)
N10F 0.0142(6) 0.0147(6) 0.0125(6) -0.0001(4) 0.0024(4) -0.0010(4)
C0AF 0.0131(6) 0.0163(7) 0.0114(6) 0.0017(5) -0.0002(5) -0.0009(5)
Cl1 0.01799(17) 0.01395(16) 0.01497(16) -0.00071(12) 0.00234(13) -0.00048(12)
O1P 0.0186(5) 0.0225(6) 0.0238(6) -0.0006(5) 0.0041(4) 0.0040(4)
O2P 0.0285(6) 0.0235(6) 0.0325(7) -0.0143(5) 0.0120(5) -0.0058(5)
O3P 0.0338(7) 0.0193(6) 0.0277(6) 0.0053(5) 0.0059(5) -0.0057(5)
O4P 0.0217(6) 0.0306(6) 0.0199(6) 0.0053(5) -0.0014(5) 0.0035(5)
Cl2 0.01604(17) 0.01538(17) 0.02032(17) 0.00203(13) 0.00460(13) 0.00282(12)
O5P 0.0395(8) 0.0253(6) 0.0309(7) -0.0066(5) 0.0069(6) 0.0103(5)
O6P 0.0337(7) 0.0222(6) 0.0366(7) 0.0121(5) 0.0081(6) 0.0008(5)
O7P 0.0244(6) 0.0306(7) 0.0393(7) -0.0051(6) 0.0163(6) -0.0057(5)
O8P 0.0243(6) 0.0355(7) 0.0293(7) -0.0002(5) -0.0045(5) 0.0079(5)
O1W 0.0223(6) 0.0229(6) 0.0178(5) -0.0070(5) -0.0033(4) 0.0067(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N3B Cu N3A 90.70(5)
N3B Cu N10F 91.96(5)
N3A Cu N10F 177.07(5)
N3B Cu N1F 165.88(5)
N3A Cu N1F 95.23(5)
N10F Cu N1F 81.90(5)
N3B Cu O1W 92.41(5)
N3A Cu O1W 91.27(5)
N10F Cu O1W 89.85(5)
N1F Cu O1W 100.24(5)
C2A N1A N8A 102.25(12)
N1A C2A N3A 115.58(13)
N1A C2A H2A 122.2
N3A C2A H2A 122.2
C3AA N3A C2A 103.77(12)
C3AA N3A Cu 129.09(10)
C2A N3A Cu 125.98(10)
N4A C3AA N3A 128.59(13)
N4A C3AA N8A 123.59(13)
N3A C3AA N8A 107.82(12)
C5A N4A C3AA 115.52(13)
N4A C5A C6A 122.90(14)
N4A C5A C51A 116.81(14)
C6A C5A C51A 120.28(14)
C5A C51A H51A 109.5
C5A C51A H52A 109.5
H51A C51A H52A 109.5
C5A C51A H53A 109.5
H51A C51A H53A 109.5
H52A C51A H53A 109.5
C7A C6A C5A 120.76(14)
C7A C6A H6A 119.6
C5A C6A H6A 119.7
C6A C7A N8A 114.84(13)
C6A C7A C71A 126.60(14)
N8A C7A C71A 118.56(14)
C7A C71A H71A 109.4
C7A C71A H72A 109.5
H71A C71A H72A 109.5
C7A C71A H73A 109.5
H71A C71A H73A 109.5
H72A C71A H73A 109.5
C7A N8A C3AA 122.34(13)
C7A N8A N1A 127.08(13)
C3AA N8A N1A 110.57(12)
C2B N1B N8B 101.59(12)
N1B C2B N3B 115.57(14)
N1B C2B H2B 122.2
N3B C2B H2B 122.2
C3AB N3B C2B 103.88(12)
C3AB N3B Cu 126.51(10)
C2B N3B Cu 128.98(10)
N4B C3AB N3B 128.49(14)
N4B C3AB N8B 123.67(14)
N3B C3AB N8B 107.83(13)
C5B N4B C3AB 115.51(14)
N4B C5B C6B 122.76(16)
N4B C5B C51B 116.89(15)
C6B C5B C51B 120.33(16)
C5B C51B H51B 109.6
C5B C51B H52B 109.4
H51B C51B H52B 109.5
C5B C51B H53B 109.4
H51B C51B H53B 109.5
H52B C51B H53B 109.5
C7B C6B C5B 120.47(15)
C7B C6B H6B 119.8
C5B C6B H6B 119.8
N8B C7B C6B 115.26(14)
N8B C7B C71B 117.24(15)
C6B C7B C71B 127.50(15)
C7B C71B H71B 109.5
C7B C71B H72B 109.4
H71B C71B H72B 109.5
C7B C71B H73B 109.5
H71B C71B H73B 109.5
H72B C71B H73B 109.5
C3AB N8B C7B 122.27(13)
C3AB N8B N1B 111.12(12)
C7B N8B N1B 126.59(13)
C2F N1F C1AF 118.13(13)
C2F N1F Cu 129.94(11)
C1AF N1F Cu 111.92(10)
N1F C1AF C4AF 123.41(13)
N1F C1AF C0AF 116.74(13)
C4AF C1AF C0AF 119.83(13)
N1F C2F C3F 122.23(14)
N1F C2F H2F 118.9
C3F C2F H2F 118.9
C4F C3F C2F 119.84(14)
C4F C3F H3F 120.1
C2F C3F H3F 120.1
C3F C4F C4AF 119.37(14)
C3F C4F H4F 120.4
C4AF C4F H4F 120.3
C1AF C4AF C4F 117.00(14)
C1AF C4AF C5F 118.96(14)
C4F C4AF C5F 124.03(14)
C6F C5F C4AF 121.05(14)
C6F C5F H5F 119.5
C4AF C5F H5F 119.5
C5F C6F C6AF 120.98(14)
C5F C6F H6F 119.5
C6AF C6F H6F 119.5
C0AF C6AF C7F 117.14(14)
C0AF C6AF C6F 118.86(14)
C7F C6AF C6F 123.99(14)
C8F C7F C6AF 119.41(14)
C8F C7F H7F 120.3
C6AF C7F H7F 120.3
C7F C8F C9F 119.56(14)
C7F C8F H8F 120.2
C9F C8F H8F 120.2
N10F C9F C8F 122.42(14)
N10F C9F H9F 118.8
C8F C9F H9F 118.8
C9F N10F C0AF 118.15(13)
C9F N10F Cu 129.07(10)
C0AF N10F Cu 112.46(10)
N10F C0AF C6AF 123.30(13)
N10F C0AF C1AF 116.41(13)
C6AF C0AF C1AF 120.28(13)
O3P Cl1 O2P 110.88(8)
O3P Cl1 O4P 109.77(8)
O2P Cl1 O4P 109.76(8)
O3P Cl1 O1P 109.34(7)
O2P Cl1 O1P 108.64(7)
O4P Cl1 O1P 108.40(7)
O8P Cl2 O6P 109.99(8)
O8P Cl2 O5P 109.38(8)
O6P Cl2 O5P 109.91(8)
O8P Cl2 O7P 109.25(8)
O6P Cl2 O7P 109.23(8)
O5P Cl2 O7P 109.06(8)
Cu O1W H11W 112.9(15)
Cu O1W H12W 134.3(15)
H11W O1W H12W 110(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu N3B 1.9800(13)
Cu N3A 2.0037(13)
Cu N10F 2.0202(12)
Cu N1F 2.0260(12)
Cu O1W 2.2397(11)
N1A C2A 1.316(2)
N1A N8A 1.3712(17)
C2A N3A 1.3589(19)
C2A H2A 0.9500
N3A C3AA 1.3501(19)
C3AA N4A 1.3371(19)
C3AA N8A 1.3685(19)
N4A C5A 1.329(2)
C5A C6A 1.418(2)
C5A C51A 1.502(2)
C51A H51A 0.9800
C51A H52A 0.9800
C51A H53A 0.9800
C6A C7A 1.367(2)
C6A H6A 0.9500
C7A N8A 1.3680(19)
C7A C71A 1.486(2)
C71A H71A 0.9800
C71A H72A 0.9800
C71A H73A 0.9800
N1B C2B 1.317(2)
N1B N8B 1.3710(19)
C2B N3B 1.361(2)
C2B H2B 0.9500
N3B C3AB 1.3395(19)
C3AB N4B 1.336(2)
C3AB N8B 1.3620(19)
N4B C5B 1.330(2)
C5B C6B 1.419(2)
C5B C51B 1.500(3)
C51B H51B 0.9800
C51B H52B 0.9800
C51B H53B 0.9800
C6B C7B 1.364(2)
C6B H6B 0.9500
C7B N8B 1.363(2)
C7B C71B 1.482(2)
C71B H71B 0.9800
C71B H72B 0.9800
C71B H73B 0.9800
N1F C2F 1.3281(19)
N1F C1AF 1.3650(19)
C1AF C4AF 1.402(2)
C1AF C0AF 1.433(2)
C2F C3F 1.407(2)
C2F H2F 0.9500
C3F C4F 1.371(2)
C3F H3F 0.9500
C4F C4AF 1.412(2)
C4F H4F 0.9500
C4AF C5F 1.436(2)
C5F C6F 1.358(2)
C5F H5F 0.9500
C6F C6AF 1.435(2)
C6F H6F 0.9500
C6AF C0AF 1.400(2)
C6AF C7F 1.412(2)
C7F C8F 1.369(2)
C7F H7F 0.9500
C8F C9F 1.403(2)
C8F H8F 0.9500
C9F N10F 1.3305(19)
C9F H9F 0.9500
N10F C0AF 1.3587(19)
Cl1 O3P 1.4345(12)
Cl1 O2P 1.4370(12)
Cl1 O4P 1.4429(12)
Cl1 O1P 1.4571(12)
Cl2 O8P 1.4350(13)
Cl2 O6P 1.4355(12)
Cl2 O5P 1.4407(13)
Cl2 O7P 1.4462(12)
O1W H11W 0.833(9)
O1W H12W 0.826(9)
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
O1W H11W O1P 0.833(9) 1.977(11) 2.7918(16) 166(2) .
O1W H12W N1A 0.826(9) 2.064(10) 2.8877(17) 175(2) 3_665
|
1500015.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500015.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_1500015
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_moiety 'C17 H14 Cu N7 O4 1+, N O3 1-'
_chemical_formula_sum 'C17 H14 Cu N8 O7'
_chemical_formula_weight 505.90
_chemical_name_systematic
;
?
;
_space_group_IT_number 13
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yac'
_symmetry_space_group_name_H-M 'P 1 2/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 95.563(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.8687(9)
_cell_length_b 7.3470(5)
_cell_length_c 18.2668(11)
_cell_measurement_reflns_used 6087
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.7
_cell_measurement_theta_min 2.7
_cell_volume 1986.1(2)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0175
_diffrn_reflns_av_sigmaI/netI 0.0225
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 12100
_diffrn_reflns_theta_full 27.00
_diffrn_reflns_theta_max 28.33
_diffrn_reflns_theta_min 1.69
_diffrn_standards_decay_% -0.2
_diffrn_standards_number 439
_exptl_absorpt_coefficient_mu 1.162
_exptl_absorpt_correction_T_max 0.673
_exptl_absorpt_correction_T_min 0.545
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.692
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1028
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.37
_exptl_crystal_size_min 0.37
_refine_diff_density_max 0.958
_refine_diff_density_min -0.662
_refine_diff_density_rms 0.081
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 304
_refine_ls_number_reflns 4523
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0507
_refine_ls_R_factor_gt 0.0451
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1332
_refine_ls_wR_factor_ref 0.1388
_reflns_number_gt 3909
_reflns_number_total 4523
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file CuDEA_compound3.cif
_cod_data_source_block cutphen
_cod_original_sg_symbol_H-M 'P 2/n'
_cod_database_code 1500015
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu Cu 0.245053(17) 0.28527(4) 0.485595(15) 0.03538(13) Uani 1 1 d .
N1 N 0.42137(16) 0.3380(4) 0.67758(14) 0.0573(6) Uani 1 1 d .
C2 C 0.35354(19) 0.3821(4) 0.62939(16) 0.0536(7) Uani 1 1 d .
H2 H 0.3215 0.4901 0.6325 0.064 Uiso 1 1 d R
N3 N 0.33444(15) 0.2608(3) 0.57364(13) 0.0431(5) Uani 1 1 d .
C3A C 0.39525(15) 0.1281(3) 0.58911(12) 0.0376(5) Uani 1 1 d .
N4 N 0.40601(15) -0.0267(3) 0.55263(12) 0.0477(5) Uani 1 1 d .
C5 C 0.4731(2) -0.1299(4) 0.58035(17) 0.0562(7) Uani 1 1 d .
H5 H 0.4828 -0.2402 0.5574 0.067 Uiso 1 1 d R
C6 C 0.5320(2) -0.0842(5) 0.64305(16) 0.0569(7) Uani 1 1 d .
H6 H 0.5791 -0.1614 0.6597 0.068 Uiso 1 1 d R
C7 C 0.51912(17) 0.0712(5) 0.67835(14) 0.0521(7) Uani 1 1 d .
H7 H 0.5573 0.1060 0.7193 0.063 Uiso 1 1 d R
N8 N 0.44804(14) 0.1761(3) 0.65115(11) 0.0429(5) Uani 1 1 d .
N1P N 0.14621(14) 0.3481(3) 0.40682(11) 0.0393(4) Uani 1 1 d .
C1AP C 0.06289(16) 0.3183(3) 0.42823(13) 0.0361(5) Uani 1 1 d .
C2P C 0.1526(2) 0.4035(4) 0.33813(15) 0.0516(6) Uani 1 1 d .
H2P H 0.2094 0.4246 0.3225 0.062 Uiso 1 1 d R
C3P C 0.0759(2) 0.4306(4) 0.28832(15) 0.0622(8) Uani 1 1 d .
H3P H 0.0817 0.4708 0.2407 0.075 Uiso 1 1 d R
C4P C -0.0076(2) 0.3982(4) 0.30954(16) 0.0570(7) Uani 1 1 d .
H4P H -0.0585 0.4135 0.2763 0.068 Uiso 1 1 d R
C4AP C -0.01705(18) 0.3423(3) 0.38191(15) 0.0471(6) Uani 1 1 d .
C5P C -0.1016(2) 0.3083(4) 0.4109(2) 0.0572(8) Uani 1 1 d .
H5P H -0.1551 0.3244 0.3807 0.069 Uiso 1 1 d R
C6P C -0.10547(19) 0.2529(4) 0.4805(2) 0.0545(7) Uani 1 1 d .
H6P H -0.1616 0.2326 0.4975 0.065 Uiso 1 1 d R
C6AP C -0.02522(19) 0.2237(3) 0.52839(17) 0.0450(6) Uani 1 1 d .
C7P C -0.0231(2) 0.1593(4) 0.60150(17) 0.0558(7) Uani 1 1 d .
H7P H -0.0770 0.1363 0.6218 0.067 Uiso 1 1 d R
C8P C 0.0572(2) 0.1311(4) 0.64140(16) 0.0547(7) Uani 1 1 d .
H8P H 0.0592 0.0856 0.6890 0.066 Uiso 1 1 d R
C9P C 0.13793(19) 0.1698(4) 0.61108(14) 0.0462(6) Uani 1 1 d .
H9P H 0.1927 0.1535 0.6395 0.055 Uiso 1 1 d R
N10P N 0.13868(14) 0.2320(3) 0.54272(11) 0.0366(4) Uani 1 1 d .
C0AP C 0.05873(16) 0.2573(3) 0.50156(14) 0.0353(5) Uani 1 1 d .
N1N N 0.35873(17) 0.5404(3) 0.44346(16) 0.0580(6) Uani 1 1 d .
O1N O 0.34054(13) 0.3758(3) 0.42523(11) 0.0521(5) Uani 1 1 d .
O2N O 0.31225(17) 0.6170(3) 0.48580(15) 0.0709(6) Uani 1 1 d .
O3N O 0.4235(2) 0.6132(5) 0.4183(2) 0.1257(14) Uani 1 1 d .
O1W O 0.25937(14) 0.0094(3) 0.43917(10) 0.0494(4) Uani 1 1 d D
H11W H 0.257(2) -0.006(5) 0.3930(6) 0.059 Uiso 1 1 d D
H12W H 0.3039(16) -0.050(4) 0.4609(16) 0.059 Uiso 1 1 d D
N2N N -0.2500 0.1589(7) 0.2500 0.0607(9) Uani 1 2 d S
O4N O -0.2500 0.3253(8) 0.2500 0.124(2) Uani 1 2 d S
O5N O -0.2993(3) 0.0804(9) 0.2826(3) 0.182(3) Uani 1 1 d .
N3N N 0.2500 -0.1107(6) 0.2500 0.0650(10) Uani 1 2 d SD
O6N O 0.2038(4) -0.1220(9) 0.3000(3) 0.0909(17) Uiso 0.50 1 d PD
O7N O 0.2787(6) 0.0351(10) 0.2285(5) 0.152(4) Uiso 0.50 1 d PD
O8N O 0.2446(8) -0.2276(12) 0.2013(5) 0.160(4) Uiso 0.50 1 d PD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.03257(19) 0.0373(2) 0.0360(2) 0.00080(10) 0.00185(12) 0.00027(10)
N1 0.0462(13) 0.0723(16) 0.0518(13) -0.0229(12) -0.0031(10) 0.0049(12)
C2 0.0478(14) 0.0552(16) 0.0563(16) -0.0202(13) -0.0030(12) 0.0058(12)
N3 0.0404(12) 0.0439(11) 0.0433(12) -0.0087(9) -0.0046(9) 0.0024(9)
C3A 0.0321(11) 0.0461(13) 0.0346(11) 0.0007(9) 0.0029(8) -0.0006(9)
N4 0.0522(12) 0.0431(11) 0.0467(11) -0.0019(9) 0.0000(9) 0.0050(10)
C5 0.0595(17) 0.0500(16) 0.0596(17) 0.0016(13) 0.0086(13) 0.0122(13)
C6 0.0467(15) 0.0717(19) 0.0523(15) 0.0149(14) 0.0051(12) 0.0172(14)
C7 0.0350(12) 0.084(2) 0.0367(12) 0.0057(12) 0.0016(10) 0.0068(13)
N8 0.0345(10) 0.0590(13) 0.0351(10) -0.0023(9) 0.0025(8) 0.0007(9)
N1P 0.0435(11) 0.0377(10) 0.0360(10) 0.0034(8) 0.0009(8) 0.0006(9)
C1AP 0.0394(12) 0.0257(9) 0.0423(12) -0.0038(8) -0.0012(9) 0.0006(8)
C2P 0.0588(16) 0.0525(15) 0.0433(14) 0.0083(11) 0.0042(12) -0.0002(13)
C3P 0.087(2) 0.0580(18) 0.0383(14) 0.0109(12) -0.0092(14) 0.0072(16)
C4P 0.0637(18) 0.0491(15) 0.0533(16) 0.0040(12) -0.0203(14) 0.0042(13)
C4AP 0.0472(14) 0.0325(12) 0.0586(16) -0.0035(11) -0.0106(12) 0.0042(10)
C5P 0.0383(14) 0.0455(15) 0.084(2) -0.0116(14) -0.0127(14) 0.0039(11)
C6P 0.0353(13) 0.0454(14) 0.083(2) -0.0133(14) 0.0085(14) -0.0035(11)
C6AP 0.0420(13) 0.0333(12) 0.0613(17) -0.0106(10) 0.0130(12) -0.0018(9)
C7P 0.0593(17) 0.0481(15) 0.0652(18) -0.0112(14) 0.0312(15) -0.0081(13)
C8P 0.0704(19) 0.0542(16) 0.0428(14) -0.0020(12) 0.0223(13) -0.0032(14)
C9P 0.0550(15) 0.0453(13) 0.0389(13) 0.0005(10) 0.0079(11) 0.0003(12)
N10P 0.0376(10) 0.0365(10) 0.0358(10) -0.0005(7) 0.0041(8) 0.0005(8)
C0AP 0.0364(12) 0.0262(10) 0.0433(12) -0.0061(8) 0.0045(9) -0.0009(8)
N1N 0.0530(13) 0.0458(13) 0.0776(17) 0.0063(12) 0.0182(12) -0.0097(11)
O1N 0.0486(10) 0.0449(10) 0.0650(12) -0.0035(9) 0.0167(9) -0.0011(8)
O2N 0.0741(15) 0.0412(11) 0.0989(18) -0.0108(11) 0.0157(13) 0.0039(10)
O3N 0.115(3) 0.111(3) 0.162(3) -0.004(2) 0.067(2) -0.063(2)
O1W 0.0598(12) 0.0417(10) 0.0455(10) -0.0069(8) -0.0010(9) 0.0047(8)
N2N 0.051(2) 0.077(3) 0.051(2) 0.000 -0.0131(16) 0.000
O4N 0.119(4) 0.094(4) 0.146(5) 0.000 -0.056(4) 0.000
O5N 0.131(4) 0.243(7) 0.165(4) 0.105(4) -0.012(3) -0.061(4)
N3N 0.058(2) 0.088(3) 0.050(2) 0.000 0.0109(17) 0.000
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'
Cu Cu 0.3201 1.2651 '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_3
N3 Cu O1N 91.23(9) .
N3 Cu N1P 169.56(9) .
O1N Cu N1P 92.17(9) .
N3 Cu N10P 93.44(9) .
O1N Cu N10P 170.85(8) .
N1P Cu N10P 81.91(8) .
N3 Cu O1W 98.35(8) .
O1N Cu O1W 89.63(8) .
N1P Cu O1W 91.54(8) .
N10P Cu O1W 97.46(8) .
N3 Cu O2N 81.89(9) .
O1N Cu O2N 53.27(8) .
N1P Cu O2N 92.26(9) .
N10P Cu O2N 119.70(8) .
O1W Cu O2N 142.81(8) .
C2 N1 N8 102.1(2) .
N1 C2 N3 115.5(3) .
N1 C2 H2 122.3 .
N3 C2 H2 122.2 .
C3A N3 C2 103.3(2) .
C3A N3 Cu 128.23(17) .
C2 N3 Cu 128.24(19) .
N4 C3A N3 128.7(2) .
N4 C3A N8 123.3(2) .
N3 C3A N8 108.0(2) .
C5 N4 C3A 115.0(2) .
N4 C5 C6 124.2(3) .
N4 C5 H5 118.2 .
C6 C5 H5 117.6 .
C7 C6 C5 119.3(3) .
C7 C6 H6 120.2 .
C5 C6 H6 120.6 .
C6 C7 N8 116.8(3) .
C6 C7 H7 121.3 .
N8 C7 H7 121.9 .
N1 N8 C3A 111.0(2) .
N1 N8 C7 127.5(2) .
C3A N8 C7 121.4(2) .
C2P N1P C1AP 118.2(2) .
C2P N1P Cu 129.18(19) .
C1AP N1P Cu 112.51(16) .
N1P C1AP C4AP 123.5(2) .
N1P C1AP C0AP 116.7(2) .
C4AP C1AP C0AP 119.8(2) .
N1P C2P C3P 121.8(3) .
N1P C2P H2P 119.3 .
C3P C2P H2P 118.9 .
C4P C3P C2P 119.9(3) .
C4P C3P H3P 119.6 .
C2P C3P H3P 120.5 .
C3P C4P C4AP 119.9(3) .
C3P C4P H4P 120.0 .
C4AP C4P H4P 120.1 .
C1AP C4AP C4P 116.7(3) .
C1AP C4AP C5P 118.6(3) .
C4P C4AP C5P 124.7(3) .
C6P C5P C4AP 121.5(3) .
C6P C5P H5P 119.1 .
C4AP C5P H5P 119.3 .
C5P C6P C6AP 121.1(3) .
C5P C6P H6P 119.2 .
C6AP C6P H6P 119.7 .
C0AP C6AP C7P 116.6(3) .
C0AP C6AP C6P 118.6(3) .
C7P C6AP C6P 124.7(3) .
C8P C7P C6AP 119.8(3) .
C8P C7P H7P 120.4 .
C6AP C7P H7P 119.7 .
C7P C8P C9P 120.1(3) .
C7P C8P H8P 120.3 .
C9P C8P H8P 119.6 .
N10P C9P C8P 121.8(3) .
N10P C9P H9P 118.8 .
C8P C9P H9P 119.4 .
C9P N10P C0AP 118.7(2) .
C9P N10P Cu 129.12(19) .
C0AP N10P Cu 112.07(16) .
N10P C0AP C6AP 122.9(2) .
N10P C0AP C1AP 116.8(2) .
C6AP C0AP C1AP 120.4(2) .
O2N N1N O3N 123.2(3) .
O2N N1N O1N 118.9(2) .
O3N N1N O1N 117.9(3) .
N1N O1N Cu 108.42(16) .
N1N O2N Cu 79.08(15) .
Cu O1W H11W 120(2) .
Cu O1W H12W 113(2) .
H11W O1W H12W 110(3) .
O5N N2N O5N 119.5(9) 2_455
O5N N2N O4N 120.2(4) .
O6N N3N O7N 123.0(6) .
O6N N3N O8N 120.0(6) .
O7N N3N O8N 112.1(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu N3 1.993(2)
Cu O1N 1.9944(19)
Cu N1P 2.008(2)
Cu N10P 2.016(2)
Cu O1W 2.2155(19)
Cu O2N 2.634(2)
N1 C2 1.313(4)
N1 N8 1.357(3)
C2 N3 1.362(3)
C2 H2 0.9300
N3 C3A 1.341(3)
C3A N4 1.336(3)
C3A N8 1.361(3)
N4 C5 1.315(4)
C5 C6 1.413(4)
C5 H5 0.9300
C6 C7 1.334(5)
C6 H6 0.9300
C7 N8 1.362(3)
C7 H7 0.9300
N1P C2P 1.331(3)
N1P C1AP 1.353(3)
C1AP C4AP 1.402(3)
C1AP C0AP 1.420(4)
C2P C3P 1.403(4)
C2P H2P 0.9300
C3P C4P 1.357(5)
C3P H3P 0.9300
C4P C4AP 1.404(4)
C4P H4P 0.9300
C4AP C5P 1.432(4)
C5P C6P 1.343(5)
C5P H5P 0.9300
C6P C6AP 1.425(4)
C6P H6P 0.9300
C6AP C0AP 1.406(4)
C6AP C7P 1.415(4)
C7P C8P 1.353(5)
C7P H7P 0.9300
C8P C9P 1.399(4)
C8P H8P 0.9300
C9P N10P 1.331(3)
C9P H9P 0.9300
N10P C0AP 1.356(3)
N1N O2N 1.223(3)
N1N O3N 1.229(3)
N1N O1N 1.276(3)
O1W H11W 0.848(10)
O1W H12W 0.856(10)
N2N O5N 1.145(4)
N2N O4N 1.223(7)
N3N O6N 1.198(5)
N3N O7N 1.231(6)
N3N O8N 1.233(7)
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
O1W H12W N4 0.856(10) 2.16(2) 2.871(3) 141(3)
O1W H11W O6N 0.848(10) 1.997(19) 2.769(6) 151(3)
|
1500016.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500016.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_1500016
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_moiety 'C12 H20 Cu N10 O2 2+, 2 (Cl O4 1-)'
_chemical_formula_sum 'C12 H20 Cl2 Cu N10 O10'
_chemical_formula_weight 598.82
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 114.735(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.3507(8)
_cell_length_b 14.2757(9)
_cell_length_c 13.0530(8)
_cell_measurement_reflns_used 4965
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 26.1
_cell_measurement_theta_min 2.2
_cell_volume 2259.5(2)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0243
_diffrn_reflns_av_sigmaI/netI 0.0291
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 14157
_diffrn_reflns_theta_full 26.80
_diffrn_reflns_theta_max 28.37
_diffrn_reflns_theta_min 1.68
_diffrn_standards_decay_% -0.2
_diffrn_standards_number 345
_exptl_absorpt_coefficient_mu 1.276
_exptl_absorpt_correction_T_max 0.822
_exptl_absorpt_correction_T_min 0.614
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.760
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1220
_exptl_crystal_size_max 0.65
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.16
_refine_diff_density_max 1.116
_refine_diff_density_min -0.410
_refine_diff_density_rms 0.083
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.080
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 328
_refine_ls_number_reflns 5104
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.0619
_refine_ls_R_factor_gt 0.0526
_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^)+(0.0800P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1446
_refine_ls_wR_factor_ref 0.1518
_reflns_number_gt 4257
_reflns_number_total 5104
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file CuDEA_compound4.cif
_cod_data_source_block cuentper
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500016
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
Cu Cu 0.24698(3) 0.47297(3) 0.20319(3) 0.03835(15) Uani 1 1 d .
N1A N 0.4182(3) 0.6275(2) 0.5011(3) 0.0504(7) Uani 1 1 d .
C2A C 0.3712(3) 0.5535(3) 0.4398(3) 0.0448(8) Uani 1 1 d .
H2A H 0.3694 0.4957 0.4719 0.054 Uiso 1 1 d R
N3A N 0.3253(2) 0.56692(19) 0.3272(2) 0.0390(6) Uani 1 1 d .
C3AA C 0.3435(3) 0.6582(2) 0.3162(3) 0.0379(7) Uani 1 1 d .
N4A N 0.3137(3) 0.7084(2) 0.2217(3) 0.0468(7) Uani 1 1 d .
C5A C 0.3417(3) 0.7977(3) 0.2359(3) 0.0518(9) Uani 1 1 d .
H5A H 0.3215 0.8350 0.1719 0.062 Uiso 1 1 d R
C6A C 0.3999(3) 0.8395(3) 0.3423(4) 0.0556(9) Uani 1 1 d .
H6A H 0.4186 0.9026 0.3478 0.067 Uiso 1 1 d R
C7A C 0.4287(3) 0.7866(3) 0.4366(4) 0.0537(9) Uani 1 1 d .
H7A H 0.4661 0.8118 0.5084 0.064 Uiso 1 1 d R
N8A N 0.3994(2) 0.6946(2) 0.4207(2) 0.0416(6) Uani 1 1 d .
N1B N 0.1628(3) 0.2951(2) 0.4135(3) 0.0643(9) Uani 1 1 d .
C2B C 0.2195(4) 0.3249(3) 0.3578(4) 0.0569(10) Uani 1 1 d .
H2B H 0.2791 0.2917 0.3569 0.068 Uiso 1 1 d R
N3B N 0.1858(2) 0.4061(2) 0.3017(2) 0.0437(6) Uani 1 1 d .
C3AB C 0.0979(3) 0.4300(2) 0.3206(3) 0.0427(7) Uani 1 1 d .
N4B N 0.0320(3) 0.5038(2) 0.2839(3) 0.0528(7) Uani 1 1 d .
C5B C -0.0489(4) 0.5076(3) 0.3165(4) 0.0632(11) Uani 1 1 d .
H5B H -0.0965 0.5586 0.2932 0.076 Uiso 1 1 d R
C6B C -0.0674(4) 0.4395(4) 0.3849(4) 0.0629(11) Uani 1 1 d .
H6B H -0.1263 0.4456 0.4049 0.076 Uiso 1 1 d R
C7B C 0.0011(4) 0.3656(3) 0.4211(4) 0.0619(11) Uani 1 1 d .
H7B H -0.0091 0.3185 0.4650 0.074 Uiso 1 1 d R
N8B N 0.0850(3) 0.3624(2) 0.3888(3) 0.0500(7) Uani 1 1 d .
N1E N 0.3161(3) 0.5257(2) 0.1046(3) 0.0458(7) Uani 1 1 d .
H11E H 0.2889 0.5831 0.0801 0.055 Uiso 1 1 d R
H12E H 0.3896 0.5306 0.1443 0.055 Uiso 1 1 d R
C1E C 0.2913(4) 0.4618(3) 0.0078(3) 0.0548(9) Uani 1 1 d .
H13E H 0.3414 0.4088 0.0296 0.066 Uiso 1 1 d R
H14E H 0.2992 0.4946 -0.0535 0.066 Uiso 1 1 d R
C2E C 0.1745(3) 0.4293(3) -0.0288(3) 0.0519(9) Uani 1 1 d .
H23E H 0.1241 0.4814 -0.0591 0.062 Uiso 1 1 d R
H24E H 0.1571 0.3820 -0.0871 0.062 Uiso 1 1 d R
N2E N 0.1633(3) 0.3896(2) 0.0705(2) 0.0450(7) Uani 1 1 d .
H21E H 0.1908 0.3311 0.0841 0.054 Uiso 1 1 d R
H22E H 0.0917 0.3874 0.0579 0.054 Uiso 1 1 d R
O1W O 0.0917(2) 0.5857(2) 0.1148(2) 0.0547(6) Uani 1 1 d D
H11W H 0.067(4) 0.596(3) 0.165(3) 0.066 Uiso 1 1 d D
H12W H 0.105(4) 0.6409(14) 0.099(4) 0.066 Uiso 1 1 d D
O2W O 0.4085(2) 0.3662(2) 0.2712(3) 0.0634(8) Uani 1 1 d D
H21W H 0.466(3) 0.369(4) 0.334(2) 0.076 Uiso 1 1 d D
H22W H 0.410(4) 0.3094(14) 0.250(4) 0.076 Uiso 1 1 d D
Cl1 Cl 0.11474(8) 0.75743(6) 0.38569(7) 0.0468(2) Uani 1 1 d .
O1P O 0.1669(3) 0.6826(3) 0.4610(3) 0.0968(13) Uani 1 1 d .
O2P O 0.1076(5) 0.7327(3) 0.2801(3) 0.1084(15) Uani 1 1 d .
O3P O 0.0109(4) 0.7731(4) 0.3816(5) 0.1275(19) Uani 1 1 d .
O4P O 0.1800(5) 0.8385(4) 0.4161(5) 0.147(2) Uani 1 1 d .
Cl2 Cl 0.63612(8) 0.61150(7) 0.29193(9) 0.0540(2) Uani 1 1 d .
O5P O 0.5891(5) 0.6738(5) 0.3394(5) 0.159(3) Uani 1 1 d .
O6P O 0.5674(5) 0.5903(5) 0.1788(4) 0.138(2) Uani 1 1 d .
O7P O 0.6804(9) 0.5356(4) 0.3550(6) 0.198(4) Uani 1 1 d .
O8P O 0.7272(6) 0.6590(6) 0.2934(7) 0.189(3) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.0413(2) 0.0376(2) 0.0389(2) -0.00181(15) 0.01952(19) -0.00715(15)
N1A 0.0516(18) 0.0534(17) 0.0397(15) 0.0001(13) 0.0127(13) 0.0035(14)
C2A 0.0462(19) 0.0438(17) 0.0439(18) 0.0030(14) 0.0182(15) 0.0047(14)
N3A 0.0390(14) 0.0386(14) 0.0373(14) 0.0003(11) 0.0138(12) -0.0008(11)
C3AA 0.0336(15) 0.0395(16) 0.0419(17) -0.0022(13) 0.0170(13) -0.0003(12)
N4A 0.0506(17) 0.0423(15) 0.0469(16) 0.0030(13) 0.0198(14) -0.0042(13)
C5A 0.055(2) 0.0435(19) 0.061(2) 0.0051(17) 0.0282(19) -0.0046(16)
C6A 0.059(2) 0.0362(17) 0.077(3) -0.0051(18) 0.033(2) -0.0069(16)
C7A 0.052(2) 0.047(2) 0.061(2) -0.0190(18) 0.0222(18) -0.0073(16)
N8A 0.0374(14) 0.0422(15) 0.0440(15) -0.0056(12) 0.0156(12) 0.0003(11)
N1B 0.086(3) 0.0478(18) 0.071(2) 0.0151(16) 0.044(2) 0.0022(17)
C2B 0.066(3) 0.046(2) 0.065(2) 0.0086(18) 0.034(2) 0.0014(18)
N3B 0.0495(16) 0.0405(14) 0.0451(16) 0.0010(12) 0.0236(13) -0.0087(12)
C3AB 0.054(2) 0.0403(17) 0.0363(16) -0.0027(13) 0.0218(15) -0.0091(15)
N4B 0.060(2) 0.0563(18) 0.0466(17) 0.0038(14) 0.0265(16) 0.0024(15)
C5B 0.070(3) 0.073(3) 0.054(2) -0.002(2) 0.033(2) 0.008(2)
C6B 0.065(3) 0.077(3) 0.061(3) -0.015(2) 0.041(2) -0.013(2)
C7B 0.083(3) 0.062(3) 0.058(2) -0.006(2) 0.047(2) -0.021(2)
N8B 0.0634(19) 0.0470(17) 0.0465(16) -0.0006(13) 0.0299(15) -0.0115(14)
N1E 0.0452(16) 0.0477(16) 0.0496(17) -0.0010(13) 0.0249(14) -0.0077(12)
C1E 0.066(2) 0.058(2) 0.052(2) -0.0044(17) 0.036(2) -0.0016(18)
C2E 0.065(2) 0.0442(19) 0.0431(19) -0.0037(15) 0.0195(17) -0.0033(17)
N2E 0.0485(16) 0.0400(15) 0.0464(16) -0.0059(12) 0.0197(13) -0.0078(12)
O1W 0.0546(16) 0.0569(16) 0.0562(16) -0.0005(13) 0.0269(13) -0.0025(13)
O2W 0.0537(17) 0.0590(17) 0.0621(18) -0.0028(14) 0.0090(13) 0.0102(14)
Cl1 0.0530(5) 0.0477(5) 0.0479(5) -0.0005(3) 0.0294(4) 0.0031(4)
O1P 0.079(2) 0.115(3) 0.086(3) 0.046(2) 0.025(2) 0.022(2)
O2P 0.182(5) 0.088(3) 0.070(2) -0.006(2) 0.067(3) 0.016(3)
O3P 0.095(3) 0.152(4) 0.178(5) 0.069(4) 0.100(3) 0.060(3)
O4P 0.182(6) 0.098(3) 0.167(5) -0.042(3) 0.080(4) -0.069(4)
Cl2 0.0502(5) 0.0510(5) 0.0630(6) 0.0095(4) 0.0257(4) 0.0072(4)
O5P 0.128(4) 0.211(7) 0.141(4) -0.027(4) 0.060(4) 0.072(4)
O6P 0.129(4) 0.185(6) 0.079(3) -0.006(3) 0.022(3) 0.022(4)
O7P 0.345(11) 0.106(4) 0.146(5) 0.053(4) 0.105(7) 0.087(6)
O8P 0.152(5) 0.208(7) 0.233(8) -0.013(6) 0.107(5) -0.072(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N2E Cu N1E 84.77(12)
N2E Cu N3A 174.78(11)
N1E Cu N3A 92.42(11)
N2E Cu N3B 92.37(12)
N1E Cu N3B 173.51(12)
N3A Cu N3B 90.86(11)
N2E Cu O2W 91.76(11)
N1E Cu O2W 84.05(12)
N3A Cu O2W 92.32(11)
N3B Cu O2W 90.23(12)
N2E Cu O1W 85.92(11)
N1E Cu O1W 88.72(11)
N3A Cu O1W 89.62(10)
N3B Cu O1W 96.90(11)
O2W Cu O1W 172.58(10)
C2A N1A N8A 102.0(3)
N1A C2A N3A 115.6(3)
N1A C2A H2A 122.3
N3A C2A H2A 122.1
C3AA N3A C2A 103.6(3)
C3AA N3A Cu 127.8(2)
C2A N3A Cu 128.7(2)
N4A C3AA N3A 128.4(3)
N4A C3AA N8A 123.4(3)
N3A C3AA N8A 108.1(3)
C5A N4A C3AA 115.6(3)
N4A C5A C6A 123.6(4)
N4A C5A H5A 118.0
C6A C5A H5A 118.4
C7A C6A C5A 119.3(3)
C7A C6A H6A 120.4
C5A C6A H6A 120.3
C6A C7A N8A 116.4(3)
C6A C7A H7A 121.9
N8A C7A H7A 121.6
C3AA N8A C7A 121.6(3)
C3AA N8A N1A 110.6(3)
C7A N8A N1A 127.7(3)
C2B N1B N8B 101.6(3)
N1B C2B N3B 116.1(4)
N1B C2B H2B 122.2
N3B C2B H2B 121.7
C3AB N3B C2B 103.8(3)
C3AB N3B Cu 127.8(2)
C2B N3B Cu 128.3(3)
N4B C3AB N3B 129.4(3)
N4B C3AB N8B 123.2(3)
N3B C3AB N8B 107.4(3)
C5B N4B C3AB 115.2(4)
N4B C5B C6B 124.1(4)
N4B C5B H5B 117.8
C6B C5B H5B 118.1
C7B C6B C5B 119.3(4)
C7B C6B H6B 120.4
C5B C6B H6B 120.3
C6B C7B N8B 116.6(4)
C6B C7B H7B 122.0
N8B C7B H7B 121.5
N1B N8B C7B 127.2(3)
N1B N8B C3AB 111.2(3)
C7B N8B C3AB 121.6(4)
C1E N1E Cu 108.4(2)
C1E N1E H11E 110.2
Cu N1E H11E 110.0
C1E N1E H12E 109.9
Cu N1E H12E 109.9
H11E N1E H12E 108.4
N1E C1E C2E 107.1(3)
N1E C1E H13E 110.5
C2E C1E H13E 110.4
N1E C1E H14E 110.1
C2E C1E H14E 110.2
H13E C1E H14E 108.5
N2E C2E C1E 108.2(3)
N2E C2E H23E 110.1
C1E C2E H23E 110.1
N2E C2E H24E 110.1
C1E C2E H24E 109.9
H23E C2E H24E 108.4
C2E N2E Cu 107.8(2)
C2E N2E H21E 110.3
Cu N2E H21E 110.2
C2E N2E H22E 110.0
Cu N2E H22E 110.0
H21E N2E H22E 108.5
Cu O1W H11W 105(3)
Cu O1W H12W 120(3)
H11W O1W H12W 102(5)
Cu O2W H21W 128(4)
Cu O2W H22W 126(3)
H21W O2W H22W 103(5)
O3P Cl1 O2P 110.6(3)
O3P Cl1 O4P 111.8(4)
O2P Cl1 O4P 105.6(3)
O3P Cl1 O1P 110.0(3)
O2P Cl1 O1P 107.8(3)
O4P Cl1 O1P 111.0(3)
O7P Cl2 O5P 114.4(4)
O7P Cl2 O8P 103.2(6)
O5P Cl2 O8P 103.9(5)
O7P Cl2 O6P 113.4(5)
O5P Cl2 O6P 113.0(4)
O8P Cl2 O6P 107.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu N2E 2.011(3)
Cu N1E 2.017(3)
Cu N3A 2.024(3)
Cu N3B 2.028(3)
Cu O2W 2.482(3)
Cu O1W 2.494(3)
N1A C2A 1.315(5)
N1A N8A 1.364(4)
C2A N3A 1.348(4)
C2A H2A 0.9300
N3A C3AA 1.345(4)
C3AA N4A 1.334(4)
C3AA N8A 1.355(4)
N4A C5A 1.320(5)
C5A C6A 1.410(6)
C5A H5A 0.9300
C6A C7A 1.355(6)
C6A H6A 0.9300
C7A N8A 1.362(5)
C7A H7A 0.9300
N1B C2B 1.320(5)
N1B N8B 1.351(5)
C2B N3B 1.344(5)
C2B H2B 0.9300
N3B C3AB 1.340(5)
C3AB N4B 1.328(5)
C3AB N8B 1.372(4)
N4B C5B 1.317(5)
C5B C6B 1.410(7)
C5B H5B 0.9300
C6B C7B 1.345(7)
C6B H6B 0.9300
C7B N8B 1.352(5)
C7B H7B 0.9300
N1E C1E 1.479(5)
N1E H11E 0.9000
N1E H12E 0.9000
C1E C2E 1.500(6)
C1E H13E 0.9700
C1E H14E 0.9700
C2E N2E 1.478(5)
C2E H23E 0.9700
C2E H24E 0.9700
N2E H21E 0.9000
N2E H22E 0.9000
O1W H11W 0.853(10)
O1W H12W 0.850(10)
O2W H21W 0.856(10)
O2W H22W 0.860(10)
Cl1 O3P 1.383(4)
Cl1 O2P 1.387(4)
Cl1 O4P 1.402(5)
Cl1 O1P 1.421(4)
Cl2 O7P 1.340(5)
Cl2 O5P 1.377(5)
Cl2 O8P 1.385(6)
Cl2 O6P 1.407(5)
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
N1E H11E O4P 0.90 2.31 3.062(6) 140.8 4_575
N1E H11E N4A 0.90 2.49 3.030(4) 118.8 .
O1W H11W N4B 0.853(10) 2.23(4) 2.889(4) 134(4) .
O1W H11W O2P 0.853(10) 2.39(4) 2.952(5) 124(4) .
|
1500017.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500017.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_1500017
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_sum 'C16 H28 Cl2 Cu N10 O10'
_chemical_formula_weight 654.92
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 117.222(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.2694(6)
_cell_length_b 8.7680(4)
_cell_length_c 23.9159(10)
_cell_measurement_reflns_used 8535
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.5
_cell_volume 2660.8(2)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0215
_diffrn_reflns_av_sigmaI/netI 0.0171
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 30021
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.31
_diffrn_reflns_theta_min 1.60
_diffrn_standards_decay_% 0.1
_diffrn_standards_number 650
_exptl_absorpt_coefficient_mu 1.091
_exptl_absorpt_correction_T_max 0.7013
_exptl_absorpt_correction_T_min 0.6392
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.635
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prisms
_exptl_crystal_F_000 1348
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.35
_refine_diff_density_max 2.593
_refine_diff_density_min -1.091
_refine_diff_density_rms 0.105
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 368
_refine_ls_number_reflns 6253
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.085
_refine_ls_R_factor_all 0.0511
_refine_ls_R_factor_gt 0.0484
_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^)+(0.0750P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1380
_refine_ls_wR_factor_ref 0.1403
_reflns_number_gt 5788
_reflns_number_total 6253
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file CuDEA_compound5.cif
_cod_data_source_block cuendmtp
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500017
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
Cu Cu 0.50464(2) 0.19694(3) 0.386622(14) 0.01394(11) Uani 1 1 d .
N1A N 0.35488(17) 0.5483(3) 0.25823(10) 0.0171(4) Uani 1 1 d .
C2A C 0.4339(2) 0.4807(3) 0.30558(12) 0.0161(5) Uani 1 1 d .
H2A H 0.5048 0.5134 0.3206 0.019 Uiso 1 1 d R
N3A N 0.40721(17) 0.3609(2) 0.33152(10) 0.0140(4) Uani 1 1 d .
C3AA C 0.3023(2) 0.3508(3) 0.29698(12) 0.0147(5) Uani 1 1 d .
N4A N 0.23727(17) 0.2480(3) 0.30188(11) 0.0172(4) Uani 1 1 d .
C5A C 0.1368(2) 0.2597(3) 0.25915(13) 0.0208(5) Uani 1 1 d .
C51A C 0.0624(2) 0.1420(4) 0.26109(17) 0.0315(7) Uani 1 1 d .
H51A H 0.0987 0.0794 0.2989 0.038 Uiso 1 1 d R
H52A H 0.0382 0.0770 0.2237 0.038 Uiso 1 1 d R
H53A H 0.0018 0.1926 0.2618 0.038 Uiso 1 1 d R
C6A C 0.1001(2) 0.3760(3) 0.21280(13) 0.0208(5) Uani 1 1 d .
H6A H 0.0274 0.3803 0.1836 0.025 Uiso 1 1 d R
C7A C 0.1672(2) 0.4813(3) 0.20928(12) 0.0181(5) Uani 1 1 d .
C71A C 0.1413(2) 0.6087(4) 0.16356(14) 0.0254(6) Uani 1 1 d .
H71A H 0.0656 0.6078 0.1348 0.030 Uiso 1 1 d R
H72A H 0.1809 0.5963 0.1395 0.030 Uiso 1 1 d R
H73A H 0.1604 0.7060 0.1863 0.030 Uiso 1 1 d R
N8A N 0.27048(16) 0.4637(2) 0.25293(10) 0.0148(4) Uani 1 1 d .
N1B N 0.64797(18) 0.5753(3) 0.50233(10) 0.0181(4) Uani 1 1 d .
C2B C 0.5693(2) 0.4897(3) 0.46263(12) 0.0161(5) Uani 1 1 d .
H2B H 0.4979 0.5212 0.4458 0.019 Uiso 1 1 d R
N3B N 0.59745(17) 0.3540(3) 0.44752(10) 0.0150(4) Uani 1 1 d .
C3AB C 0.7035(2) 0.3546(3) 0.48007(11) 0.0158(5) Uani 1 1 d .
N4B N 0.77101(18) 0.2482(3) 0.48068(11) 0.0192(5) Uani 1 1 d .
C5B C 0.8723(2) 0.2819(4) 0.51516(14) 0.0244(6) Uani 1 1 d .
C51B C 0.9499(3) 0.1640(5) 0.51743(17) 0.0376(8) Uani 1 1 d .
H51B H 0.9120 0.0736 0.4939 0.045 Uiso 1 1 d R
H52B H 0.9956 0.1358 0.5613 0.045 Uiso 1 1 d R
H53B H 0.9928 0.2056 0.4987 0.045 Uiso 1 1 d R
C6B C 0.9075(2) 0.4208(4) 0.54842(14) 0.0267(6) Uani 1 1 d .
H6B H 0.9810 0.4406 0.5712 0.032 Uiso 1 1 d R
C7B C 0.8373(2) 0.5262(4) 0.54794(13) 0.0223(6) Uani 1 1 d .
C71B C 0.8613(3) 0.6758(4) 0.58078(17) 0.0341(7) Uani 1 1 d .
H71B H 0.9379 0.6891 0.6041 0.041 Uiso 1 1 d R
H72B H 0.8309 0.6790 0.6101 0.041 Uiso 1 1 d R
H73B H 0.8311 0.7579 0.5498 0.041 Uiso 1 1 d R
N8B N 0.73348(17) 0.4881(3) 0.51281(10) 0.0169(4) Uani 1 1 d .
N1E N 0.59630(18) 0.0236(3) 0.43704(11) 0.0195(5) Uani 1 1 d .
H11E H 0.6635 0.0364 0.4418 0.023 Uiso 1 1 d R
H12E H 0.5997 0.0225 0.4764 0.023 Uiso 1 1 d R
C1E C 0.5528(2) -0.1222(3) 0.40488(15) 0.0247(6) Uani 1 1 d .
H13E H 0.5003 -0.1619 0.4175 0.030 Uiso 1 1 d R
H14E H 0.6098 -0.1986 0.4166 0.030 Uiso 1 1 d R
C2E C 0.5012(2) -0.0942(3) 0.33476(15) 0.0254(6) Uani 1 1 d .
H23E H 0.5552 -0.0697 0.3210 0.030 Uiso 1 1 d R
H24E H 0.4623 -0.1862 0.3119 0.030 Uiso 1 1 d R
N2E N 0.42779(18) 0.0359(3) 0.32172(11) 0.0194(4) Uani 1 1 d .
H21E H 0.3683 0.0052 0.3243 0.023 Uiso 1 1 d R
H22E H 0.4080 0.0735 0.2820 0.023 Uiso 1 1 d R
Cl1 Cl 0.24921(5) 0.14499(8) 0.13818(3) 0.02192(16) Uani 1 1 d .
O1P O 0.3327(2) 0.2018(3) 0.19611(11) 0.0392(6) Uani 1 1 d .
O2P O 0.2928(2) 0.0298(3) 0.11432(11) 0.0378(6) Uani 1 1 d .
O3P O 0.1681(2) 0.0814(4) 0.15010(15) 0.0533(8) Uani 1 1 d .
O4P O 0.2099(2) 0.2678(4) 0.09360(16) 0.0557(8) Uani 1 1 d .
Cl2 Cl 0.24322(5) 0.75594(8) 0.36084(3) 0.02180(16) Uani 1 1 d .
O5P O 0.2481(2) 0.8211(3) 0.30723(12) 0.0372(6) Uani 1 1 d .
O6P O 0.2003(3) 0.6011(4) 0.34317(16) 0.0615(9) Uani 1 1 d .
O7P O 0.1693(3) 0.8332(5) 0.37485(17) 0.0670(10) Uani 1 1 d .
O8P O 0.3422(3) 0.7382(6) 0.41314(18) 0.0796(13) Uani 1 1 d .
O1W O 0.39032(19) 0.1522(3) 0.43909(11) 0.0279(5) Uani 1 1 d D
H11W H 0.381(3) 0.223(4) 0.4601(17) 0.034 Uiso 1 1 d D
H12W H 0.331(2) 0.136(5) 0.4063(14) 0.034 Uiso 1 1 d D
O2W O 0.61215(17) 0.2430(3) 0.32908(10) 0.0249(4) Uani 1 1 d D
H21W H 0.628(3) 0.198(4) 0.3037(15) 0.030 Uiso 1 1 d D
H22W H 0.655(3) 0.313(3) 0.3431(18) 0.030 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 0.01344(17) 0.01146(17) 0.01462(17) 0.00083(10) 0.00443(13) 0.00135(10)
N1A 0.0161(10) 0.0167(10) 0.0189(10) 0.0017(8) 0.0083(9) 0.0007(8)
C2A 0.0158(11) 0.0142(11) 0.0180(11) 0.0007(9) 0.0073(10) 0.0000(9)
N3A 0.0132(10) 0.0127(10) 0.0150(10) 0.0005(8) 0.0055(8) 0.0004(8)
C3AA 0.0149(11) 0.0159(11) 0.0136(11) -0.0005(9) 0.0068(9) 0.0016(9)
N4A 0.0152(10) 0.0171(11) 0.0193(10) -0.0005(8) 0.0080(9) -0.0015(8)
C5A 0.0167(12) 0.0228(13) 0.0239(13) -0.0032(11) 0.0100(11) -0.0013(10)
C51A 0.0197(14) 0.0341(17) 0.0378(17) 0.0007(14) 0.0108(13) -0.0089(12)
C6A 0.0133(11) 0.0255(14) 0.0198(12) -0.0015(10) 0.0044(10) 0.0031(10)
C7A 0.0145(11) 0.0221(13) 0.0152(11) -0.0013(10) 0.0046(10) 0.0054(10)
C71A 0.0209(13) 0.0263(14) 0.0219(13) 0.0057(11) 0.0038(11) 0.0064(11)
N8A 0.0138(10) 0.0156(10) 0.0148(10) 0.0012(8) 0.0064(8) 0.0024(8)
N1B 0.0189(10) 0.0175(10) 0.0184(10) -0.0002(8) 0.0090(9) 0.0001(8)
C2B 0.0171(11) 0.0166(12) 0.0147(11) 0.0012(9) 0.0072(9) 0.0008(9)
N3B 0.0126(10) 0.0161(10) 0.0152(10) 0.0008(8) 0.0055(8) 0.0015(8)
C3AB 0.0157(12) 0.0193(12) 0.0123(11) 0.0009(9) 0.0063(9) -0.0004(9)
N4B 0.0153(10) 0.0240(12) 0.0170(10) 0.0026(9) 0.0062(9) 0.0050(9)
C5B 0.0170(13) 0.0364(16) 0.0195(13) 0.0025(12) 0.0079(11) 0.0044(12)
C51B 0.0186(14) 0.053(2) 0.0356(18) -0.0015(16) 0.0073(13) 0.0138(14)
C6B 0.0142(12) 0.0406(17) 0.0226(13) -0.0011(12) 0.0061(11) -0.0041(12)
C7B 0.0180(12) 0.0304(15) 0.0183(12) -0.0030(11) 0.0080(10) -0.0079(11)
C71B 0.0252(15) 0.0366(18) 0.0370(17) -0.0129(14) 0.0112(14) -0.0156(13)
N8B 0.0159(10) 0.0198(11) 0.0150(10) 0.0006(8) 0.0069(8) -0.0011(8)
N1E 0.0193(11) 0.0181(11) 0.0219(11) 0.0057(9) 0.0100(9) 0.0044(9)
C1E 0.0280(14) 0.0142(12) 0.0350(16) 0.0064(11) 0.0170(13) 0.0024(11)
C2E 0.0318(15) 0.0137(12) 0.0329(15) -0.0030(11) 0.0166(13) 0.0018(11)
N2E 0.0209(11) 0.0148(10) 0.0210(11) -0.0025(8) 0.0083(9) -0.0016(9)
Cl1 0.0182(3) 0.0273(3) 0.0203(3) -0.0005(2) 0.0088(2) 0.0060(2)
O1P 0.0512(16) 0.0369(14) 0.0241(11) -0.0083(10) 0.0125(11) -0.0168(11)
O2P 0.0538(15) 0.0341(13) 0.0324(12) -0.0046(10) 0.0258(12) 0.0120(11)
O3P 0.0281(13) 0.081(2) 0.0595(18) -0.0014(16) 0.0270(13) -0.0075(14)
O4P 0.0492(17) 0.0562(19) 0.0563(18) 0.0295(15) 0.0193(15) 0.0293(15)
Cl2 0.0203(3) 0.0260(3) 0.0197(3) 0.0028(2) 0.0097(3) 0.0011(2)
O5P 0.0494(15) 0.0378(13) 0.0360(13) 0.0130(10) 0.0295(12) 0.0059(11)
O6P 0.089(2) 0.0466(18) 0.060(2) -0.0049(15) 0.0445(19) -0.0130(17)
O7P 0.070(2) 0.090(3) 0.061(2) 0.0268(19) 0.0467(19) 0.037(2)
O8P 0.0342(16) 0.134(4) 0.059(2) 0.043(2) 0.0114(15) -0.006(2)
O1W 0.0368(12) 0.0246(11) 0.0288(11) -0.0003(9) 0.0205(10) 0.0028(9)
O2W 0.0257(10) 0.0264(11) 0.0281(11) -0.0089(9) 0.0168(9) -0.0046(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu 0.3201 1.2651 '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
N3B Cu N1E 92.95(9)
N3B Cu N2E 171.82(9)
N1E Cu N2E 84.70(10)
N3B Cu N3A 90.79(9)
N1E Cu N3A 176.22(9)
N2E Cu N3A 91.52(9)
N3B Cu O1W 96.26(8)
N1E Cu O1W 88.58(9)
N2E Cu O1W 91.52(9)
N3A Cu O1W 91.53(8)
N3B Cu O2W 85.50(8)
N1E Cu O2W 93.29(9)
N2E Cu O2W 86.81(8)
N3A Cu O2W 86.48(8)
O1W Cu O2W 177.37(7)
C2A N1A N8A 101.9(2)
N1A C2A N3A 115.5(2)
N1A C2A H2A 122.3
N3A C2A H2A 122.2
C3AA N3A C2A 103.7(2)
C3AA N3A Cu 126.68(18)
C2A N3A Cu 126.58(17)
N4A C3AA N3A 127.9(2)
N4A C3AA N8A 123.9(2)
N3A C3AA N8A 108.1(2)
C5A N4A C3AA 115.4(2)
N4A C5A C6A 122.6(3)
N4A C5A C51A 116.9(3)
C6A C5A C51A 120.5(3)
C5A C51A H51A 109.5
C5A C51A H52A 109.4
H51A C51A H52A 109.5
C5A C51A H53A 109.5
H51A C51A H53A 109.5
H52A C51A H53A 109.5
C7A C6A C5A 121.2(2)
C7A C6A H6A 119.4
C5A C6A H6A 119.4
C6A C7A N8A 114.7(2)
C6A C7A C71A 127.6(2)
N8A C7A C71A 117.6(2)
C7A C71A H71A 109.5
C7A C71A H72A 109.5
H71A C71A H72A 109.5
C7A C71A H73A 109.5
H71A C71A H73A 109.5
H72A C71A H73A 109.5
C3AA N8A N1A 110.7(2)
C3AA N8A C7A 122.2(2)
N1A N8A C7A 127.1(2)
C2B N1B N8B 102.0(2)
N1B C2B N3B 115.6(2)
N1B C2B H2B 122.2
N3B C2B H2B 122.2
C3AB N3B C2B 103.5(2)
C3AB N3B Cu 128.08(18)
C2B N3B Cu 128.28(17)
N4B C3AB N3B 128.1(2)
N4B C3AB N8B 123.8(2)
N3B C3AB N8B 108.0(2)
C5B N4B C3AB 115.2(3)
N4B C5B C6B 123.1(3)
N4B C5B C51B 116.5(3)
C6B C5B C51B 120.4(3)
C5B C51B H51B 109.5
C5B C51B H52B 109.4
H51B C51B H52B 109.5
C5B C51B H53B 109.5
H51B C51B H53B 109.5
H52B C51B H53B 109.5
C7B C6B C5B 120.6(3)
C7B C6B H6B 119.7
C5B C6B H6B 119.7
C6B C7B N8B 115.2(3)
C6B C7B C71B 127.2(3)
N8B C7B C71B 117.6(3)
C7B C71B H71B 109.5
C7B C71B H72B 109.5
H71B C71B H72B 109.5
C7B C71B H73B 109.5
H71B C71B H73B 109.5
H72B C71B H73B 109.5
N1B N8B C3AB 110.9(2)
N1B N8B C7B 127.0(2)
C3AB N8B C7B 122.0(2)
C1E N1E Cu 109.87(17)
C1E N1E H11E 109.7
Cu N1E H11E 109.7
C1E N1E H12E 109.7
Cu N1E H12E 109.7
H11E N1E H12E 108.2
N1E C1E C2E 108.2(2)
N1E C1E H13E 110.0
C2E C1E H13E 110.0
N1E C1E H14E 110.1
C2E C1E H14E 110.1
H13E C1E H14E 108.4
N2E C2E C1E 107.3(2)
N2E C2E H23E 110.2
C1E C2E H23E 110.2
N2E C2E H24E 110.3
C1E C2E H24E 110.3
H23E C2E H24E 108.5
C2E N2E Cu 107.14(17)
C2E N2E H21E 110.2
Cu N2E H21E 110.3
C2E N2E H22E 110.3
Cu N2E H22E 110.3
H21E N2E H22E 108.6
O3P Cl1 O2P 110.11(19)
O3P Cl1 O4P 111.4(2)
O2P Cl1 O4P 109.01(18)
O3P Cl1 O1P 109.41(17)
O2P Cl1 O1P 107.90(16)
O4P Cl1 O1P 108.99(19)
O8P Cl2 O7P 113.4(3)
O8P Cl2 O5P 113.59(19)
O7P Cl2 O5P 111.53(18)
O8P Cl2 O6P 105.7(3)
O7P Cl2 O6P 104.6(2)
O5P Cl2 O6P 107.18(18)
Cu O1W H11W 120(3)
Cu O1W H12W 100(3)
H11W O1W H12W 108(4)
Cu O2W H21W 139(3)
Cu O2W H22W 115(3)
H21W O2W H22W 105(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu N3B 2.002(2)
Cu N1E 2.008(2)
Cu N2E 2.012(2)
Cu N3A 2.015(2)
Cu O1W 2.502(2)
Cu O2W 2.518(2)
N1A C2A 1.318(3)
N1A N8A 1.370(3)
C2A N3A 1.360(3)
C2A H2A 0.9500
N3A C3AA 1.342(3)
C3AA N4A 1.337(3)
C3AA N8A 1.364(3)
N4A C5A 1.331(3)
C5A C6A 1.418(4)
C5A C51A 1.495(4)
C51A H51A 0.9800
C51A H52A 0.9800
C51A H53A 0.9800
C6A C7A 1.360(4)
C6A H6A 0.9500
C7A N8A 1.370(3)
C7A C71A 1.487(4)
C71A H71A 0.9800
C71A H72A 0.9800
C71A H73A 0.9800
N1B C2B 1.323(3)
N1B N8B 1.362(3)
C2B N3B 1.356(3)
C2B H2B 0.9500
N3B C3AB 1.348(3)
C3AB N4B 1.336(3)
C3AB N8B 1.364(3)
N4B C5B 1.329(4)
C5B C6B 1.415(5)
C5B C51B 1.497(4)
C51B H51B 0.9800
C51B H52B 0.9800
C51B H53B 0.9799
C6B C7B 1.360(4)
C6B H6B 0.9500
C7B N8B 1.369(3)
C7B C71B 1.486(4)
C71B H71B 0.9800
C71B H72B 0.9800
C71B H73B 0.9800
N1E C1E 1.475(4)
N1E H11E 0.9200
N1E H12E 0.9200
C1E C2E 1.512(4)
C1E H13E 0.9900
C1E H14E 0.9900
C2E N2E 1.482(4)
C2E H23E 0.9900
C2E H24E 0.9900
N2E H21E 0.9200
N2E H22E 0.9200
Cl1 O3P 1.426(3)
Cl1 O2P 1.434(2)
Cl1 O4P 1.436(3)
Cl1 O1P 1.441(2)
Cl2 O8P 1.403(3)
Cl2 O7P 1.417(3)
Cl2 O5P 1.435(2)
Cl2 O6P 1.470(3)
O1W H11W 0.844(19)
O1W H12W 0.865(19)
O2W H21W 0.838(19)
O2W H22W 0.818(19)
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
O1W H11W N1B 0.844(19) 2.11(2) 2.945(3) 169(4) 3_666
O2W H21W N1A 0.838(19) 2.07(2) 2.898(3) 167(4) 2_645
O2W H22W O2P 0.818(19) 2.12(2) 2.884(3) 154(4) 2_655
N1E H11E N4B 0.92 2.32 2.967(3) 127.5 .
N2E H22E O1P 0.92 2.15 3.042(3) 163.3 .
N2E H21E O5P 0.92 2.25 3.070(4) 147.9 1_545
|
1500018.cif | #------------------------------------------------------------------------------
#$Date: 2017-07-12 10:07:33 +0300 (Wed, 12 Jul 2017) $
#$Revision: 198667 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500018.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_1500018
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
Copper(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine
and its 5,7-dimethyl derivative
;
_journal_name_full Polyhedron
_journal_page_first 2779
_journal_page_last 2784
_journal_paper_doi 10.1016/j.poly.2008.06.001
_journal_volume 27
_journal_year 2008
_chemical_formula_moiety
;
C25 H25 Cu2 N20 O3 3+, 3(Cl O4 1-), 2(H2 O)
;
_chemical_formula_sum 'C25 H29 Cl3 Cu2 N20 O17'
_chemical_formula_weight 1115.11
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 102.797(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 13.2076(7)
_cell_length_b 22.2625(10)
_cell_length_c 14.1257(7)
_cell_measurement_reflns_used 6370
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.98
_cell_measurement_theta_min 2.35
_cell_volume 4050.3(3)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0374
_diffrn_reflns_av_sigmaI/netI 0.0319
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 47147
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.36
_diffrn_reflns_theta_min 1.58
_diffrn_standards_decay_% 0
_diffrn_standards_number 512
_exptl_absorpt_coefficient_mu 1.347
_exptl_absorpt_correction_T_max 0.8659
_exptl_absorpt_correction_T_min 0.7245
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.829
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular shape'
_exptl_crystal_F_000 2256
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.11
_refine_diff_density_max 2.662
_refine_diff_density_min -1.134
_refine_diff_density_rms 0.132
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 628
_refine_ls_number_reflns 9546
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.055
_refine_ls_R_factor_all 0.0693
_refine_ls_R_factor_gt 0.0604
_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^)+(0.0800P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1558
_refine_ls_wR_factor_ref 0.1626
_reflns_number_gt 8212
_reflns_number_total 9546
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file CuDEA_compound6.cif
_cod_data_source_block cutp3per
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2017-07-12
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500018
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_attached_hydrogens
Cu1 Cu 0.31183(3) 0.413643(19) 0.28825(3) 0.01560(12) Uani 1 1 d . 0
Cu2 Cu 0.11020(3) 0.50005(2) 0.24205(3) 0.01961(13) Uani 1 1 d . 0
O1 O 0.1891(2) 0.43911(12) 0.19569(18) 0.0197(5) Uani 1 1 d D 0
H1 H 0.211(3) 0.446(2) 0.145(2) 0.024 Uiso 1 1 d D 0
N1A N 0.1530(3) 0.29795(18) 0.4393(3) 0.0311(8) Uani 1 1 d . 0
C2A C 0.2347(3) 0.32469(17) 0.4182(3) 0.0216(7) Uani 1 1 d . 0
H2A H 0.3027 0.3086 0.4376 0.026 Uiso 1 1 d R 0
N3A N 0.2152(2) 0.37653(14) 0.3671(2) 0.0189(6) Uani 1 1 d . 0
C3AA C 0.1124(3) 0.38478(16) 0.3541(3) 0.0174(7) Uani 1 1 d . 0
N4A N 0.0526(2) 0.42981(14) 0.3096(2) 0.0200(6) Uani 1 1 d . 0
C5A C -0.0480(3) 0.42308(18) 0.3075(3) 0.0255(8) Uani 1 1 d . 0
H5A H -0.0947 0.4532 0.2765 0.031 Uiso 1 1 d R 0
C6A C -0.0883(4) 0.37473(19) 0.3476(3) 0.0308(9) Uani 1 1 d . 0
H6A H -0.1610 0.3726 0.3430 0.037 Uiso 1 1 d R 0
C7A C -0.0282(4) 0.3312(2) 0.3926(3) 0.0328(9) Uani 1 1 d . 0
H7A H -0.0549 0.2977 0.4209 0.039 Uiso 1 1 d R 0
N8A N 0.0715(3) 0.33791(16) 0.3953(2) 0.0277(7) Uani 1 1 d . 0
N1B N 0.4990(3) 0.47545(16) 0.1025(2) 0.0263(7) Uani 1 1 d . 0
C2B C 0.4487(3) 0.43668(18) 0.1456(3) 0.0232(8) Uani 1 1 d . 0
H2B H 0.4455 0.3952 0.1296 0.028 Uiso 1 1 d R 0
N3B N 0.4019(2) 0.45944(14) 0.2139(2) 0.0179(6) Uani 1 1 d . 0
C3AB C 0.4258(3) 0.51787(17) 0.2157(3) 0.0172(7) Uani 1 1 d . 0
N4B N 0.4009(2) 0.56150(15) 0.2718(2) 0.0211(6) Uani 1 1 d . 0
C5B C 0.4362(3) 0.61577(18) 0.2572(3) 0.0254(8) Uani 1 1 d . 0
H5B H 0.4217 0.6477 0.2968 0.030 Uiso 1 1 d R 0
C6B C 0.4940(3) 0.62903(19) 0.1869(3) 0.0286(9) Uani 1 1 d . 0
H6B H 0.5163 0.6689 0.1789 0.034 Uiso 1 1 d R 0
C7B C 0.5171(3) 0.58373(18) 0.1310(3) 0.0258(8) Uani 1 1 d . 0
H7B H 0.5551 0.5908 0.0822 0.031 Uiso 1 1 d R 0
N8B N 0.4836(2) 0.52795(15) 0.1477(2) 0.0209(6) Uani 1 1 d . 0
N1C N 0.5710(3) 0.39203(16) 0.5205(2) 0.0243(7) Uani 1 1 d . 0
C2C C 0.4769(3) 0.41045(17) 0.4777(3) 0.0210(7) Uani 1 1 d . 0
H2C H 0.4370 0.4359 0.5093 0.025 Uiso 1 1 d R 0
C3AC C 0.5190(3) 0.35718(16) 0.3682(3) 0.0169(7) Uani 1 1 d . 0
N3C N 0.4411(2) 0.39071(13) 0.3856(2) 0.0165(6) Uani 1 1 d . 0
N4C N 0.5256(2) 0.32701(14) 0.2873(2) 0.0195(6) Uani 1 1 d . 0
C5C C 0.6124(3) 0.29602(18) 0.2929(3) 0.0254(8) Uani 1 1 d . 0
H5C H 0.6213 0.2751 0.2367 0.031 Uiso 1 1 d R 0
C6C C 0.6928(3) 0.2924(2) 0.3776(3) 0.0307(9) Uani 1 1 d . 0
H6C H 0.7519 0.2678 0.3787 0.037 Uiso 1 1 d R 0
C7C C 0.6843(3) 0.3242(2) 0.4569(3) 0.0294(9) Uani 1 1 d . 0
H7C H 0.7370 0.3233 0.5149 0.035 Uiso 1 1 d R 0
N8C N 0.5969(2) 0.35736(15) 0.4499(2) 0.0204(6) Uani 1 1 d . 0
N1D N 0.1909(4) 0.65946(18) 0.1158(4) 0.0513(13) Uani 1 1 d . 0
C2D C 0.1575(4) 0.6251(2) 0.1796(4) 0.0397(12) Uani 1 1 d . 0
H2D H 0.1337 0.6417 0.2327 0.048 Uiso 1 1 d R 0
N3D N 0.1595(3) 0.56552(15) 0.1644(3) 0.0244(7) Uani 1 1 d . 0
C3AD C 0.1989(3) 0.56139(18) 0.0842(3) 0.0227(8) Uani 1 1 d . 0
N4D N 0.2208(3) 0.51252(16) 0.0381(2) 0.0252(7) Uani 1 1 d . 0
C5D C 0.2591(3) 0.5224(2) -0.0400(3) 0.0294(9) Uani 1 1 d . 0
H5D H 0.2749 0.4885 -0.0750 0.035 Uiso 1 1 d R 0
C6D C 0.2776(3) 0.5799(2) -0.0742(3) 0.0343(10) Uani 1 1 d . 0
H6D H 0.3048 0.5844 -0.1307 0.041 Uiso 1 1 d R 0
C7D C 0.2562(4) 0.6279(2) -0.0254(4) 0.0390(11) Uani 1 1 d . 0
H7D H 0.2674 0.6675 -0.0460 0.047 Uiso 1 1 d R 0
N8D N 0.2176(3) 0.61791(16) 0.0548(3) 0.0332(9) Uani 1 1 d . 0
N1E N -0.0507(3) 0.59812(17) 0.4157(3) 0.0274(7) Uani 1 1 d . 0
C2E C 0.0196(3) 0.56188(19) 0.3944(3) 0.0257(8) Uani 1 1 d . 0
H2E H 0.0675 0.5408 0.4432 0.031 Uiso 1 1 d R 0
N3E N 0.0196(2) 0.55635(14) 0.2986(2) 0.0211(6) Uani 1 1 d . 0
C3AE C -0.0584(3) 0.59253(16) 0.2551(3) 0.0201(7) Uani 1 1 d . 0
N4E N -0.0931(2) 0.60365(16) 0.1603(3) 0.0251(7) Uani 1 1 d . 0
C5E C -0.1720(3) 0.6421(2) 0.1396(3) 0.0315(9) Uani 1 1 d . 0
H5E H -0.1993 0.6514 0.0733 0.038 Uiso 1 1 d R 0
C6E C -0.2178(3) 0.6698(2) 0.2090(4) 0.0327(10) Uani 1 1 d . 0
H6E H -0.2737 0.6972 0.1894 0.039 Uiso 1 1 d R 0
C7E C -0.1808(3) 0.65719(18) 0.3041(4) 0.0302(9) Uani 1 1 d . 0
H7E H -0.2102 0.6746 0.3532 0.036 Uiso 1 1 d R 0
N8E N -0.1000(2) 0.61808(15) 0.3257(3) 0.0231(7) Uani 1 1 d . 0
O1W O 0.3056(2) 0.31973(14) 0.2193(2) 0.0268(6) Uani 1 1 d D 0
H11W H 0.257(3) 0.315(2) 0.170(2) 0.032 Uiso 1 1 d D 0
H12W H 0.3649(18) 0.315(2) 0.209(4) 0.032 Uiso 1 1 d D 0
O2W O 0.2577(2) 0.51243(13) 0.3760(2) 0.0255(6) Uani 1 1 d D 0
H21W H 0.257(4) 0.519(2) 0.4344(13) 0.031 Uiso 1 1 d D 0
H22W H 0.305(3) 0.5346(19) 0.365(4) 0.031 Uiso 1 1 d D 0
O3W O 0.1339(3) 0.30291(18) 0.0695(3) 0.0460(9) Uani 1 1 d . 0
H31W H 0.1320 0.2744 0.0302 0.055 Uiso 1 1 d R 0
H32W H 0.0805 0.2995 0.0922 0.055 Uiso 1 1 d R 0
O4W O -0.0201(5) 0.4708(5) 0.0984(7) 0.080(4) Uani 0.50 1 d P 2
O5W O 0.0153(5) 0.4210(5) 0.0175(5) 0.063(3) Uani 0.50 1 d P 2
Cl1 Cl 0.45664(7) 0.27724(4) 0.02704(6) 0.01958(18) Uani 1 1 d . 0
Cl2 Cl 0.70872(8) 0.50119(6) 0.34897(8) 0.0368(3) Uani 1 1 d . 0
Cl3 Cl 0.08958(8) 0.75173(5) 0.33728(9) 0.0336(2) Uani 1 1 d . 0
O1P O 0.4502(2) 0.25025(14) -0.0665(2) 0.0311(7) Uani 1 1 d . 0
O2P O 0.5525(3) 0.30842(19) 0.0589(3) 0.0470(9) Uani 1 1 d . 0
O3P O 0.3745(3) 0.32048(19) 0.0172(3) 0.0521(10) Uani 1 1 d . 0
O4P O 0.4403(4) 0.23363(17) 0.0963(3) 0.0537(11) Uani 1 1 d . 0
O5P O 0.7570(2) 0.51530(14) 0.2715(2) 0.0289(6) Uani 1 1 d . 0
O6P O 0.7829(2) 0.48039(17) 0.4326(2) 0.0359(7) Uani 1 1 d . 0
O7P O 0.6652(7) 0.5544(4) 0.3752(5) 0.183(5) Uani 1 1 d . 0
O8P O 0.6356(6) 0.4580(5) 0.3203(5) 0.198(6) Uani 1 1 d . 0
O9P O 0.1897(2) 0.76059(16) 0.3196(3) 0.0402(8) Uani 1 1 d . 0
O10P O 0.0205(3) 0.7323(2) 0.2483(3) 0.0638(12) Uani 1 1 d . 0
O11P O 0.0486(3) 0.8117(2) 0.3534(4) 0.0628(12) Uani 1 1 d . 0
O12P O 0.0867(4) 0.7089(3) 0.4052(5) 0.111(3) Uani 1 1 d . 0
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
Cu1 0.0154(2) 0.0165(2) 0.0155(2) 0.00140(15) 0.00458(16) 0.00150(15)
Cu2 0.0169(2) 0.0189(2) 0.0244(2) 0.00563(17) 0.00737(18) 0.00425(16)
O1 0.0194(13) 0.0228(13) 0.0168(12) -0.0002(10) 0.0036(10) 0.0027(10)
N1A 0.0259(18) 0.039(2) 0.0314(19) 0.0000(16) 0.0118(15) -0.0022(15)
C2A 0.0190(17) 0.0244(19) 0.0222(18) 0.0037(14) 0.0062(14) 0.0021(14)
N3A 0.0179(14) 0.0212(15) 0.0180(14) 0.0010(12) 0.0046(11) 0.0035(12)
C3AA 0.0184(17) 0.0171(16) 0.0179(16) -0.0032(13) 0.0063(13) 0.0001(13)
N4A 0.0162(14) 0.0210(15) 0.0233(16) 0.0022(12) 0.0055(12) 0.0004(11)
C5A 0.0167(18) 0.0231(19) 0.036(2) -0.0021(16) 0.0052(16) 0.0024(14)
C6A 0.033(2) 0.029(2) 0.038(2) -0.0019(18) 0.0237(19) -0.0031(17)
C7A 0.032(2) 0.036(2) 0.032(2) -0.0002(18) 0.0126(18) -0.0048(18)
N8A 0.0367(19) 0.0262(17) 0.0216(16) -0.0009(13) 0.0094(14) -0.0093(14)
N1B 0.0360(19) 0.0251(17) 0.0219(16) 0.0043(13) 0.0154(14) 0.0089(14)
C2B 0.030(2) 0.0220(18) 0.0199(18) 0.0027(14) 0.0097(15) 0.0068(15)
N3B 0.0185(14) 0.0198(15) 0.0157(14) 0.0020(11) 0.0041(11) 0.0020(11)
C3AB 0.0132(15) 0.0225(17) 0.0157(16) 0.0019(13) 0.0031(12) 0.0017(13)
N4B 0.0230(16) 0.0211(16) 0.0201(15) -0.0008(12) 0.0068(12) -0.0027(12)
C5B 0.032(2) 0.0220(19) 0.0229(19) -0.0019(15) 0.0075(16) -0.0034(15)
C6B 0.032(2) 0.025(2) 0.030(2) 0.0059(16) 0.0083(17) -0.0054(16)
C7B 0.026(2) 0.029(2) 0.0251(19) 0.0088(16) 0.0115(16) 0.0002(16)
N8B 0.0207(15) 0.0253(16) 0.0183(15) 0.0040(12) 0.0076(12) 0.0029(12)
N1C 0.0230(16) 0.0306(18) 0.0191(16) -0.0053(13) 0.0038(12) 0.0006(13)
C2C 0.0239(18) 0.0222(18) 0.0182(17) 0.0001(14) 0.0072(14) 0.0002(14)
C3AC 0.0161(16) 0.0184(16) 0.0161(16) 0.0031(13) 0.0032(13) 0.0000(13)
N3C 0.0167(14) 0.0180(14) 0.0157(14) -0.0004(11) 0.0054(11) 0.0000(11)
N4C 0.0201(15) 0.0219(15) 0.0170(14) -0.0010(12) 0.0053(11) 0.0025(12)
C5C 0.0255(19) 0.028(2) 0.0239(19) -0.0033(15) 0.0075(15) 0.0067(16)
C6C 0.0204(19) 0.036(2) 0.035(2) -0.0029(18) 0.0048(16) 0.0113(17)
C7C 0.0191(18) 0.038(2) 0.028(2) -0.0011(18) -0.0017(15) 0.0073(16)
N8C 0.0195(15) 0.0248(16) 0.0165(14) -0.0004(12) 0.0034(12) 0.0007(12)
N1D 0.061(3) 0.0220(19) 0.091(4) 0.006(2) 0.059(3) 0.0033(18)
C2D 0.039(3) 0.023(2) 0.068(3) 0.001(2) 0.037(2) 0.0006(18)
N3D 0.0215(16) 0.0213(16) 0.0332(18) 0.0036(14) 0.0118(14) 0.0030(12)
C3AD 0.0177(17) 0.0230(18) 0.0274(19) 0.0058(15) 0.0054(14) 0.0026(14)
N4D 0.0255(17) 0.0263(17) 0.0238(17) 0.0054(13) 0.0056(13) 0.0031(13)
C5D 0.027(2) 0.040(2) 0.0214(19) 0.0047(17) 0.0059(16) 0.0041(18)
C6D 0.028(2) 0.041(3) 0.038(2) 0.017(2) 0.0167(19) 0.0087(18)
C7D 0.031(2) 0.033(2) 0.060(3) 0.021(2) 0.026(2) 0.0075(18)
N8D 0.0305(19) 0.0227(17) 0.054(2) 0.0111(16) 0.0271(18) 0.0075(14)
N1E 0.0217(16) 0.0335(19) 0.0267(17) -0.0037(14) 0.0046(13) 0.0023(14)
C2E 0.0187(18) 0.030(2) 0.028(2) 0.0014(16) 0.0033(15) 0.0005(15)
N3E 0.0165(14) 0.0209(15) 0.0263(16) 0.0046(13) 0.0059(12) 0.0016(12)
C3AE 0.0137(16) 0.0191(17) 0.0286(19) 0.0035(14) 0.0074(14) -0.0014(13)
N4E 0.0175(15) 0.0279(17) 0.0300(18) 0.0093(14) 0.0059(13) 0.0006(13)
C5E 0.0203(19) 0.034(2) 0.039(2) 0.0152(19) 0.0056(17) 0.0028(16)
C6E 0.0197(19) 0.028(2) 0.050(3) 0.0094(19) 0.0077(18) 0.0042(16)
C7E 0.0196(19) 0.0216(19) 0.052(3) -0.0020(18) 0.0134(18) 0.0032(15)
N8E 0.0172(15) 0.0212(16) 0.0315(18) -0.0018(13) 0.0067(13) -0.0002(12)
O1W 0.0207(14) 0.0311(15) 0.0295(15) -0.0110(12) 0.0073(11) -0.0010(12)
O2W 0.0271(15) 0.0305(15) 0.0205(13) -0.0034(11) 0.0085(11) -0.0099(12)
O3W 0.0292(17) 0.063(2) 0.047(2) -0.0094(18) 0.0118(15) -0.0063(16)
O4W 0.023(3) 0.100(7) 0.097(7) 0.083(6) -0.035(4) -0.030(4)
O5W 0.014(3) 0.140(9) 0.038(4) 0.053(5) 0.010(3) 0.023(4)
Cl1 0.0199(4) 0.0207(4) 0.0189(4) -0.0019(3) 0.0060(3) -0.0030(3)
Cl2 0.0149(4) 0.0603(7) 0.0370(6) 0.0284(5) 0.0099(4) 0.0081(4)
Cl3 0.0283(5) 0.0307(5) 0.0461(6) -0.0113(4) 0.0172(4) -0.0097(4)
O1P 0.0378(17) 0.0306(16) 0.0285(16) -0.0105(12) 0.0156(13) -0.0044(13)
O2P 0.0308(17) 0.072(3) 0.0375(19) -0.0115(18) 0.0069(14) -0.0225(17)
O3P 0.045(2) 0.062(2) 0.045(2) -0.0213(19) -0.0006(16) 0.0259(18)
O4P 0.092(3) 0.0368(19) 0.0306(18) 0.0088(15) 0.0093(19) -0.021(2)
O5P 0.0279(15) 0.0363(16) 0.0247(15) -0.0007(12) 0.0106(12) -0.0042(12)
O6P 0.0221(15) 0.061(2) 0.0224(15) 0.0024(14) 0.0015(12) 0.0110(14)
O7P 0.250(9) 0.247(9) 0.102(5) 0.117(6) 0.141(6) 0.221(8)
O8P 0.135(6) 0.303(11) 0.107(5) 0.151(6) -0.081(4) -0.179(7)
O9P 0.0240(16) 0.049(2) 0.051(2) -0.0101(16) 0.0144(14) -0.0067(14)
O10P 0.043(2) 0.067(3) 0.069(3) 0.015(2) -0.012(2) -0.013(2)
O11P 0.059(3) 0.052(2) 0.087(3) -0.014(2) 0.036(2) -0.003(2)
O12P 0.060(3) 0.152(6) 0.105(4) 0.092(4) -0.019(3) -0.037(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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 N3C 177.64(12)
O1 Cu1 N3B 90.15(12)
N3C Cu1 N3B 88.56(12)
O1 Cu1 N3A 87.49(12)
N3C Cu1 N3A 93.59(12)
N3B Cu1 N3A 173.64(12)
O1 Cu1 O1W 91.97(11)
N3C Cu1 O1W 90.23(11)
N3B Cu1 O1W 102.02(12)
N3A Cu1 O1W 83.97(11)
O1 Cu2 N3E 173.21(12)
O1 Cu2 N3D 93.44(13)
N3E Cu2 N3D 93.31(13)
O1 Cu2 N4A 84.57(12)
N3E Cu2 N4A 88.64(13)
N3D Cu2 N4A 174.78(14)
O1 Cu2 O2W 86.72(11)
N3E Cu2 O2W 93.74(12)
N3D Cu2 O2W 92.40(12)
N4A Cu2 O2W 92.31(11)
O1 Cu2 O4W 82.2(3)
N3E Cu2 O4W 97.1(3)
N3D Cu2 O4W 89.65(19)
N4A Cu2 O4W 85.31(18)
O2W Cu2 O4W 168.8(3)
Cu2 O1 Cu1 114.61(13)
Cu2 O1 H1 119(3)
Cu1 O1 H1 103(3)
C2A N1A N8A 101.2(3)
N1A C2A N3A 115.8(3)
N1A C2A H2A 122.1
N3A C2A H2A 122.1
C3AA N3A C2A 104.9(3)
C3AA N3A Cu1 127.2(2)
C2A N3A Cu1 124.5(2)
N3A C3AA N4A 129.7(3)
N3A C3AA N8A 108.8(3)
N4A C3AA N8A 121.6(3)
C5A N4A C3AA 114.0(3)
C5A N4A Cu2 122.9(3)
C3AA N4A Cu2 122.9(2)
N4A C5A C6A 123.6(4)
N4A C5A H5A 118.3
C6A C5A H5A 118.2
C7A C6A C5A 121.7(4)
C7A C6A H6A 119.2
C5A C6A H6A 119.1
N8A C7A C6A 114.9(4)
N8A C7A H7A 122.6
C6A C7A H7A 122.5
C7A N8A C3AA 124.2(4)
C7A N8A N1A 126.4(4)
C3AA N8A N1A 109.3(3)
C2B N1B N8B 101.6(3)
N1B C2B N3B 116.1(3)
N1B C2B H2B 121.9
N3B C2B H2B 122.0
C3AB N3B C2B 103.6(3)
C3AB N3B Cu1 130.0(2)
C2B N3B Cu1 126.4(3)
N3B C3AB N4B 128.9(3)
N3B C3AB N8B 108.2(3)
N4B C3AB N8B 122.9(3)
C5B N4B C3AB 115.3(3)
N4B C5B C6B 124.2(4)
N4B C5B H5B 117.8
C6B C5B H5B 117.9
C7B C6B C5B 118.7(4)
C7B C6B H6B 120.6
C5B C6B H6B 120.6
N8B C7B C6B 117.1(4)
N8B C7B H7B 121.5
C6B C7B H7B 121.5
C7B N8B N1B 127.8(3)
C7B N8B C3AB 121.7(3)
N1B N8B C3AB 110.5(3)
C2C N1C N8C 101.8(3)
N1C C2C N3C 115.6(3)
N1C C2C H2C 122.2
N3C C2C H2C 122.2
N3C C3AC N4C 129.3(3)
N3C C3AC N8C 108.0(3)
N4C C3AC N8C 122.7(3)
C3AC N3C C2C 103.8(3)
C3AC N3C Cu1 126.0(2)
C2C N3C Cu1 129.7(3)
C5C N4C C3AC 115.3(3)
N4C C5C C6C 123.9(4)
N4C C5C H5C 118.1
C6C C5C H5C 118.0
C7C C6C C5C 119.1(4)
C7C C6C H6C 120.4
C5C C6C H6C 120.5
C6C C7C N8C 116.8(4)
C6C C7C H7C 121.7
N8C C7C H7C 121.5
C7C N8C N1C 127.1(3)
C7C N8C C3AC 122.0(3)
N1C N8C C3AC 110.8(3)
C2D N1D N8D 102.1(4)
N1D C2D N3D 115.9(4)
N1D C2D H2D 122.0
N3D C2D H2D 122.1
C2D N3D C3AD 103.1(3)
C2D N3D Cu2 127.3(3)
C3AD N3D Cu2 129.6(3)
N4D C3AD N3D 129.1(4)
N4D C3AD N8D 122.1(4)
N3D C3AD N8D 108.8(4)
C5D N4D C3AD 115.7(4)
N4D C5D C6D 124.2(4)
N4D C5D H5D 117.9
C6D C5D H5D 117.9
C7D C6D C5D 118.5(4)
C7D C6D H6D 120.8
C5D C6D H6D 120.7
C6D C7D N8D 117.5(4)
C6D C7D H7D 121.3
N8D C7D H7D 121.2
C7D N8D N1D 127.9(4)
C7D N8D C3AD 122.0(4)
N1D N8D C3AD 110.1(3)
C2E N1E N8E 101.6(3)
N1E C2E N3E 116.1(4)
N1E C2E H2E 121.9
N3E C2E H2E 122.0
C3AE N3E C2E 103.4(3)
C3AE N3E Cu2 130.8(3)
C2E N3E Cu2 125.6(3)
N4E C3AE N3E 128.7(4)
N4E C3AE N8E 123.3(3)
N3E C3AE N8E 107.9(3)
C5E N4E C3AE 114.6(4)
N4E C5E C6E 124.6(4)
N4E C5E H5E 117.7
C6E C5E H5E 117.7
C7E C6E C5E 119.0(4)
C7E C6E H6E 120.5
C5E C6E H6E 120.4
C6E C7E N8E 116.7(4)
C6E C7E H7E 121.7
N8E C7E H7E 121.7
C7E N8E C3AE 121.8(4)
C7E N8E N1E 127.3(4)
C3AE N8E N1E 111.0(3)
Cu1 O1W H11W 115(4)
Cu1 O1W H12W 104(4)
H11W O1W H12W 114(5)
Cu2 O2W H21W 128(3)
Cu2 O2W H22W 116(3)
H21W O2W H22W 104(5)
H31W O3W H32W 106.3
O2P Cl1 O4P 111.9(2)
O2P Cl1 O3P 107.7(3)
O4P Cl1 O3P 107.3(3)
O2P Cl1 O1P 111.1(2)
O4P Cl1 O1P 111.0(2)
O3P Cl1 O1P 107.6(2)
O8P Cl2 O7P 111.8(7)
O8P Cl2 O5P 109.8(4)
O7P Cl2 O5P 107.3(3)
O8P Cl2 O6P 109.1(3)
O7P Cl2 O6P 107.5(4)
O5P Cl2 O6P 111.44(19)
O12P Cl3 O9P 113.3(3)
O12P Cl3 O10P 107.1(3)
O9P Cl3 O10P 108.9(3)
O12P Cl3 O11P 117.2(4)
O9P Cl3 O11P 106.9(2)
O10P Cl3 O11P 102.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu1 O1 1.928(3)
Cu1 N3C 2.007(3)
Cu1 N3B 2.028(3)
Cu1 N3A 2.045(3)
Cu1 O1W 2.300(3)
Cu2 O1 1.913(3)
Cu2 N3E 2.016(3)
Cu2 N3D 2.017(3)
Cu2 N4A 2.063(3)
Cu2 O2W 2.412(3)
Cu2 O4W 2.441(9)
O1 H1 0.837(10)
N1A C2A 1.323(5)
N1A N8A 1.428(5)
C2A N3A 1.355(5)
C2A H2A 0.9500
N3A C3AA 1.342(5)
C3AA N4A 1.343(5)
C3AA N8A 1.363(5)
N4A C5A 1.332(5)
C5A C6A 1.377(6)
C5A H5A 0.9500
C6A C7A 1.322(7)
C6A H6A 0.9500
C7A N8A 1.318(6)
C7A H7A 0.9500
N1B C2B 1.318(5)
N1B N8B 1.369(5)
C2B N3B 1.354(5)
C2B H2B 0.9500
N3B C3AB 1.337(5)
C3AB N4B 1.340(5)
C3AB N8B 1.371(4)
N4B C5B 1.327(5)
C5B C6B 1.412(6)
C5B H5B 0.9500
C6B C7B 1.357(6)
C6B H6B 0.9500
C7B N8B 1.357(5)
C7B H7B 0.9500
N1C C2C 1.321(5)
N1C N8C 1.363(4)
C2C N3C 1.355(5)
C2C H2C 0.9500
C3AC N3C 1.337(4)
C3AC N4C 1.345(5)
C3AC N8C 1.367(5)
N4C C5C 1.325(5)
C5C C6C 1.415(6)
C5C H5C 0.9500
C6C C7C 1.351(6)
C6C H6C 0.9500
C7C N8C 1.355(5)
C7C H7C 0.9500
N1D C2D 1.329(6)
N1D N8D 1.363(6)
C2D N3D 1.346(5)
C2D H2D 0.9500
N3D C3AD 1.351(5)
C3AD N4D 1.332(5)
C3AD N8D 1.364(5)
N4D C5D 1.330(5)
C5D C6D 1.408(6)
C5D H5D 0.9500
C6D C7D 1.335(7)
C6D H6D 0.9500
C7D N8D 1.359(6)
C7D H7D 0.9500
N1E C2E 1.314(5)
N1E N8E 1.368(5)
C2E N3E 1.360(5)
C2E H2E 0.9500
N3E C3AE 1.344(5)
C3AE N4E 1.340(5)
C3AE N8E 1.365(5)
N4E C5E 1.329(5)
C5E C6E 1.403(7)
C5E H5E 0.9500
C6E C7E 1.353(7)
C6E H6E 0.9500
C7E N8E 1.359(5)
C7E H7E 0.9500
O1W H11W 0.838(10)
O1W H12W 0.836(10)
O2W H21W 0.839(10)
O2W H22W 0.837(10)
O3W H31W 0.8402
O3W H32W 0.8402
Cl1 O2P 1.426(3)
Cl1 O4P 1.428(3)
Cl1 O3P 1.434(3)
Cl1 O1P 1.437(3)
Cl2 O8P 1.359(6)
Cl2 O7P 1.402(7)
Cl2 O5P 1.419(3)
Cl2 O6P 1.434(3)
Cl3 O12P 1.358(5)
Cl3 O9P 1.413(3)
Cl3 O10P 1.447(4)
Cl3 O11P 1.477(4)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N4D 0.837(10) 2.15(3) 2.866(4) 144(4) .
O1W H12W N4C 0.836(10) 2.18(4) 2.856(4) 138(5) .
O1W H11W O3W 0.838(10) 1.930(13) 2.763(5) 172(5) .
O2W H22W N4B 0.837(10) 2.11(3) 2.858(4) 149(5) .
O2W H21W O6P 0.839(10) 2.063(19) 2.875(4) 163(5) 3_666
O3W H31W N1A 0.84 2.12 2.949(5) 171.0 4_565
O3W H32W O11P 0.84 2.04 2.863(5) 167.2 2_545
|
1500019.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500019.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_1500019
loop_
_publ_author_name
'Maria Lalia Kantouri'
'Christos D. Papadopoulos'
'Antonios G. Hatzdimitriou'
'Miguel Quir\'os'
_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
;
Synthesis and characterization of new Co(III) mixed-ligand complexes,
containing 2-hydroxy-aryloximes and \a-diimines. Crystal and molecular
strucutre of [Co(saox)(bipy)~2~]Br
;
_journal_name_full Polyhedron
_journal_page_first 1292
_journal_page_last 1302
_journal_paper_doi 10.1016/j.poly.2006.10.047
_journal_volume 26
_journal_year 2007
_chemical_formula_moiety 'C13 H11 N O2'
_chemical_formula_sum 'C13 H11 N O2'
_chemical_formula_weight 213.23
_chemical_name_systematic
;
?
;
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens mixed
_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 8
_cell_length_a 9.4668(7)
_cell_length_b 8.8177(6)
_cell_length_c 25.9413(18)
_cell_measurement_reflns_used 3731
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 26.9
_cell_measurement_theta_min 2.3
_cell_volume 2165.5(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0221
_diffrn_reflns_av_sigmaI/netI 0.0194
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 12832
_diffrn_reflns_theta_full 27.30
_diffrn_reflns_theta_max 28.29
_diffrn_reflns_theta_min 1.57
_diffrn_standards_decay_% -0.1
_diffrn_standards_number 267
_exptl_absorpt_coefficient_mu 0.089
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.308
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 896
_exptl_crystal_size_max 0.56
_exptl_crystal_size_mid 0.37
_exptl_crystal_size_min 0.34
_refine_diff_density_max 0.210
_refine_diff_density_min -0.210
_refine_diff_density_rms 0.039
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 151
_refine_ls_number_reflns 2532
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0584
_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^)+(0.0700P)^2^+0.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1264
_refine_ls_wR_factor_ref 0.1347
_reflns_number_gt 2005
_reflns_number_total 2532
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file hbpox.cif
_cod_data_source_block hbpox
_cod_database_code 1500019
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.21234(14) 0.38928(16) 0.44760(5) 0.0461(3) Uani 1 1 d .
O1 O 0.27498(11) 0.30186(13) 0.48430(4) 0.0605(3) Uani 1 1 d D
H1 H 0.3674(16) 0.313(2) 0.4807(7) 0.073 Uiso 1 1 d D
C2 C 0.29128(13) 0.46785(14) 0.41022(5) 0.0403(3) Uani 1 1 d .
C3 C 0.21648(14) 0.55779(16) 0.37534(5) 0.0486(3) Uani 1 1 d .
H3 H 0.2665 0.6131 0.3509 0.058 Uiso 1 1 d R
C4 C 0.07144(16) 0.56686(18) 0.37616(6) 0.0554(4) Uani 1 1 d .
H4 H 0.0244 0.6271 0.3523 0.066 Uiso 1 1 d R
C5 C -0.00362(16) 0.4865(2) 0.41231(7) 0.0612(4) Uani 1 1 d .
H5 H -0.1018 0.4911 0.4128 0.073 Uiso 1 1 d R
C6 C 0.06661(16) 0.3989(2) 0.44786(6) 0.0601(4) Uani 1 1 d .
H6 H 0.0154 0.3456 0.4725 0.072 Uiso 1 1 d R
C7 C 0.44659(14) 0.45530(14) 0.40709(5) 0.0408(3) Uani 1 1 d .
N2 N 0.50906(11) 0.38796(14) 0.44466(4) 0.0475(3) Uani 1 1 d .
O2 O 0.65421(10) 0.37195(15) 0.43796(4) 0.0617(3) Uani 1 1 d D
H2 H 0.6799(19) 0.318(2) 0.4643(6) 0.074 Uiso 1 1 d D
C1P C 0.52289(13) 0.51387(16) 0.36068(5) 0.0436(3) Uani 1 1 d .
C2P C 0.62540(15) 0.6245(2) 0.36590(6) 0.0579(4) Uani 1 1 d .
H2P H 0.6467 0.6630 0.3984 0.069 Uiso 1 1 d R
C3P C 0.69582(19) 0.6781(2) 0.32284(8) 0.0789(6) Uani 1 1 d .
H3P H 0.7632 0.7542 0.3262 0.095 Uiso 1 1 d R
C4P C 0.6664(2) 0.6191(3) 0.27523(8) 0.0879(7) Uani 1 1 d .
H4P H 0.7157 0.6530 0.2465 0.105 Uiso 1 1 d R
C5P C 0.5646(2) 0.5091(3) 0.26956(6) 0.0786(6) Uani 1 1 d .
H5P H 0.5444 0.4701 0.2371 0.094 Uiso 1 1 d R
C6P C 0.49203(18) 0.45695(19) 0.31214(5) 0.0573(4) Uani 1 1 d .
H6P H 0.4222 0.3837 0.3082 0.069 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0437(8) 0.0521(8) 0.0426(7) 0.0043(6) 0.0026(5) -0.0006(6)
O1 0.0451(6) 0.0827(8) 0.0536(6) 0.0280(5) 0.0066(4) 0.0001(5)
C2 0.0384(7) 0.0440(7) 0.0385(6) -0.0006(5) 0.0014(5) -0.0006(5)
C3 0.0469(8) 0.0527(8) 0.0462(7) 0.0064(6) 0.0007(5) 0.0014(6)
C4 0.0476(8) 0.0593(9) 0.0591(9) 0.0053(7) -0.0059(6) 0.0092(7)
C5 0.0366(7) 0.0696(10) 0.0773(11) 0.0047(8) 0.0017(7) 0.0023(7)
C6 0.0443(8) 0.0700(10) 0.0662(10) 0.0149(8) 0.0106(7) -0.0042(7)
C7 0.0398(6) 0.0471(7) 0.0354(6) 0.0021(5) 0.0012(5) -0.0013(5)
N2 0.0364(6) 0.0650(8) 0.0411(6) 0.0099(5) -0.0001(4) -0.0009(5)
O2 0.0372(6) 0.0911(8) 0.0567(6) 0.0278(6) -0.0007(4) 0.0044(5)
C1P 0.0372(7) 0.0525(8) 0.0409(7) 0.0101(5) 0.0032(5) 0.0060(5)
C2P 0.0461(8) 0.0660(10) 0.0616(9) 0.0151(7) 0.0013(6) -0.0042(7)
C3P 0.0522(9) 0.0944(14) 0.0901(14) 0.0414(11) 0.0093(9) -0.0085(9)
C4P 0.0691(12) 0.1253(18) 0.0692(12) 0.0493(12) 0.0270(9) 0.0179(12)
C5P 0.0888(13) 0.1055(15) 0.0416(8) 0.0155(9) 0.0107(8) 0.0249(12)
C6P 0.0621(9) 0.0676(10) 0.0423(8) 0.0078(7) -0.0016(6) 0.0058(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 C1 C6 117.80(12)
O1 C1 C2 121.99(12)
C6 C1 C2 120.21(12)
C1 O1 H1 107.0(12)
C3 C2 C1 117.21(12)
C3 C2 C7 120.79(11)
C1 C2 C7 122.00(11)
C4 C3 C2 121.95(13)
C4 C3 H3 119.2
C2 C3 H3 118.8
C5 C4 C3 119.80(14)
C5 C4 H4 120.1
C3 C4 H4 120.1
C4 C5 C6 119.85(14)
C4 C5 H5 120.2
C6 C5 H5 119.9
C5 C6 C1 120.95(14)
C5 C6 H6 119.5
C1 C6 H6 119.5
N2 C7 C2 116.81(11)
N2 C7 C1P 123.20(12)
C2 C7 C1P 119.94(11)
C7 N2 O2 113.97(10)
N2 O2 H2 103.5(12)
C2P C1P C6P 119.49(13)
C2P C1P C7 120.24(13)
C6P C1P C7 120.27(13)
C1P C2P C3P 120.00(17)
C1P C2P H2P 119.9
C3P C2P H2P 120.1
C4P C3P C2P 120.00(19)
C4P C3P H3P 119.9
C2P C3P H3P 120.1
C3P C4P C5P 120.50(16)
C3P C4P H4P 120.0
C5P C4P H4P 119.5
C4P C5P C6P 119.89(18)
C4P C5P H5P 120.1
C6P C5P H5P 120.0
C5P C6P C1P 120.10(17)
C5P C6P H6P 119.9
C1P C6P H6P 120.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.3610(16)
C1 C6 1.382(2)
C1 C2 1.4068(18)
O1 H1 0.886(14)
C2 C3 1.3960(18)
C2 C7 1.4767(18)
C3 C4 1.376(2)
C3 H3 0.9300
C4 C5 1.374(2)
C4 H4 0.9300
C5 C6 1.374(2)
C5 H5 0.9300
C6 H6 0.9300
C7 N2 1.2855(16)
C7 C1P 1.4959(17)
N2 O2 1.3922(14)
O2 H2 0.867(15)
C1P C2P 1.383(2)
C1P C6P 1.387(2)
C2P C3P 1.384(2)
C2P H2P 0.9300
C3P C4P 1.369(3)
C3P H3P 0.9300
C4P C5P 1.375(3)
C4P H4P 0.9300
C5P C6P 1.379(2)
C5P H5P 0.9300
C6P H6P 0.9300
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N2 0.886(14) 1.762(16) 2.5582(15) 148.3(17) .
O2 H2 O1 0.867(15) 1.925(15) 2.7789(14) 167.9(17) 4_556
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 21490405 ChemSpider
|
1500020.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500020.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_1500020
loop_
_publ_author_name
'Miguel A. Galindo'
'Miguel Quir\'os'
'M. Angustias Romero'
'Jorge A.R. Navarro'
_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
;
Cyclic tetranuclear half-sandwich ruthenium(II) complexes with
4,7-phenanthroline and hydroxo bridges: Crystal structure, solution
behaviour and binding to nucleosides
;
_journal_name_full 'Journal of Inorganic Biochemistry'
_journal_page_first 1025
_journal_page_last 1032
_journal_paper_doi 10.1016/j.jinorgbio.2007.11.009
_journal_volume 102
_journal_year 2008
_chemical_formula_sum 'C68 H76 F12 N4 O16 Ru4 S4'
_chemical_formula_weight 1965.85
_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 102.806(1)
_cell_angle_beta 102.335(1)
_cell_angle_gamma 107.799(1)
_cell_formula_units_Z 2
_cell_length_a 13.1234(6)
_cell_length_b 18.0169(9)
_cell_length_c 18.6161(9)
_cell_measurement_reflns_used 5619
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 24.82
_cell_measurement_theta_min 2.30
_cell_volume 3894.5(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0279
_diffrn_reflns_av_sigmaI/netI 0.0388
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 46093
_diffrn_reflns_theta_full 28.37
_diffrn_reflns_theta_max 28.37
_diffrn_reflns_theta_min 1.43
_diffrn_standards_decay_% 0
_diffrn_standards_number 411
_exptl_absorpt_coefficient_mu 0.962
_exptl_absorpt_correction_T_max 0.8535
_exptl_absorpt_correction_T_min 0.7142
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.676
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular shape'
_exptl_crystal_F_000 1976
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.17
_refine_diff_density_max 1.874
_refine_diff_density_min -1.208
_refine_diff_density_rms 0.168
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 852
_refine_ls_number_reflns 17722
_refine_ls_number_restraints 76
_refine_ls_restrained_S_all 1.080
_refine_ls_R_factor_all 0.1083
_refine_ls_R_factor_gt 0.0833
_refine_ls_shift/su_max 0.043
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2636
_refine_ls_wR_factor_ref 0.2882
_reflns_number_gt 12120
_reflns_number_total 17722
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ruter2.cif
_cod_data_source_block ruter2
_cod_database_code 1500020
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
Ru1 Ru 0.26641(4) 0.74598(3) 0.28257(3) 0.04938(17) Uani 1 1 d .
Ru2 Ru 0.52671(4) 0.74846(3) 0.34074(3) 0.04899(17) Uani 1 1 d .
O1 O 0.3669(4) 0.6791(3) 0.2622(3) 0.0503(10) Uani 1 1 d .
O2 O 0.4209(4) 0.8113(4) 0.3818(3) 0.0664(15) Uani 1 1 d .
C1P C 0.1134(7) 0.7765(5) 0.2725(6) 0.069(2) Uani 1 1 d .
C11P C 0.0294(8) 0.7667(7) 0.3178(6) 0.087(3) Uani 1 1 d .
H11P H 0.0175 0.7156 0.3309 0.104 Uiso 1 1 d R
C12P C -0.0805(10) 0.7618(10) 0.2654(9) 0.127(5) Uani 1 1 d .
H12P H -0.0648 0.7994 0.2362 0.152 Uiso 1 1 d R
H13P H -0.1258 0.7759 0.2963 0.152 Uiso 1 1 d R
H14P H -0.1202 0.7071 0.2307 0.152 Uiso 1 1 d R
C13P C 0.0690(14) 0.8387(11) 0.3924(10) 0.168(8) Uani 1 1 d .
H15P H 0.0892 0.8895 0.3805 0.201 Uiso 1 1 d R
H16P H 0.1331 0.8378 0.4280 0.201 Uiso 1 1 d R
H17P H 0.0094 0.8341 0.4154 0.201 Uiso 1 1 d R
C2P C 0.0981(7) 0.7105(5) 0.2095(5) 0.065(2) Uani 1 1 d .
H2P H 0.0378 0.6616 0.1976 0.078 Uiso 1 1 d R
C3P C 0.1694(7) 0.7154(5) 0.1642(5) 0.066(2) Uani 1 1 d .
H3P H 0.1557 0.6701 0.1228 0.079 Uiso 1 1 d R
C4P C 0.2621(7) 0.7874(6) 0.1798(6) 0.078(3) Uani 1 1 d .
C41P C 0.3401(10) 0.7919(8) 0.1308(7) 0.099(4) Uani 1 1 d .
H41P H 0.3413 0.7384 0.1104 0.119 Uiso 1 1 d R
H42P H 0.4144 0.8290 0.1618 0.119 Uiso 1 1 d R
H43P H 0.3143 0.8111 0.0889 0.119 Uiso 1 1 d R
C5P C 0.2803(7) 0.8545(5) 0.2460(6) 0.075(2) Uani 1 1 d .
H5P H 0.3419 0.9028 0.2588 0.090 Uiso 1 1 d R
C6P C 0.2115(7) 0.8493(5) 0.2895(6) 0.077(2) Uani 1 1 d .
H6P H 0.2270 0.8940 0.3320 0.092 Uiso 1 1 d R
C1Q C 0.6967(8) 0.8322(7) 0.4122(8) 0.096(3) Uani 1 1 d .
C11Q C 0.7446(11) 0.8728(9) 0.5046(8) 0.117(4) Uani 1 1 d .
H11Q H 0.7220 0.8292 0.5281 0.141 Uiso 1 1 d R
C12Q C 0.7120(16) 0.9312(9) 0.5344(10) 0.157(7) Uani 1 1 d .
H12Q H 0.7559 0.9579 0.5876 0.189 Uiso 1 1 d R
H13Q H 0.6341 0.9081 0.5308 0.189 Uiso 1 1 d R
H14Q H 0.7222 0.9704 0.5064 0.189 Uiso 1 1 d R
C13Q C 0.8681(13) 0.9065(18) 0.5256(16) 0.296(18) Uani 1 1 d .
H15Q H 0.8925 0.9514 0.5056 0.355 Uiso 1 1 d R
H16Q H 0.8932 0.8642 0.5041 0.355 Uiso 1 1 d R
H17Q H 0.8991 0.9252 0.5808 0.355 Uiso 1 1 d R
C2Q C 0.6957(7) 0.7545(6) 0.3880(6) 0.073(2) Uani 1 1 d .
H2Q H 0.7217 0.7310 0.4242 0.087 Uiso 1 1 d R
C3Q C 0.6558(7) 0.7099(6) 0.3094(7) 0.087(3) Uani 1 1 d .
H3Q H 0.6549 0.6570 0.2925 0.104 Uiso 1 1 d R
C4Q C 0.6151(8) 0.7495(9) 0.2537(6) 0.097(4) Uani 1 1 d .
C41Q C 0.5787(12) 0.7043(13) 0.1682(9) 0.173(8) Uani 1 1 d .
H41Q H 0.5090 0.7076 0.1433 0.207 Uiso 1 1 d R
H42Q H 0.5689 0.6478 0.1614 0.207 Uiso 1 1 d R
H43Q H 0.6350 0.7283 0.1459 0.207 Uiso 1 1 d R
C5Q C 0.6218(9) 0.8317(10) 0.2902(10) 0.106(4) Uani 1 1 d .
H5Q H 0.5988 0.8607 0.2586 0.127 Uiso 1 1 d R
C6Q C 0.6591(11) 0.8682(8) 0.3664(10) 0.109(4) Uani 1 1 d .
H6Q H 0.6577 0.9198 0.3865 0.131 Uiso 1 1 d R
Ru3 Ru 0.27235(5) 0.26202(3) 0.18593(3) 0.05162(18) Uani 1 1 d .
Ru4 Ru 0.01436(5) 0.26110(3) 0.12248(3) 0.05220(18) Uani 1 1 d .
O3 O 0.1847(4) 0.3341(3) 0.1528(3) 0.0497(10) Uani 1 1 d .
O4 O 0.1031(4) 0.2006(4) 0.1851(3) 0.0642(13) Uani 1 1 d .
C1R C 0.3092(8) 0.1501(5) 0.1640(5) 0.068(2) Uani 1 1 d .
C11R C 0.2471(11) 0.0669(6) 0.1718(7) 0.095(3) Uani 1 1 d .
H11R H 0.1680 0.0492 0.1421 0.114 Uiso 1 1 d R
C12R C 0.2512(15) 0.0631(8) 0.2496(9) 0.133(5) Uani 1 1 d .
H12R H 0.3251 0.0678 0.2765 0.159 Uiso 1 1 d R
H13R H 0.1974 0.0117 0.2468 0.159 Uiso 1 1 d R
H14R H 0.2339 0.1072 0.2767 0.159 Uiso 1 1 d R
C13R C 0.2955(13) 0.0058(6) 0.1311(9) 0.139(6) Uani 1 1 d .
H15R H 0.3664 0.0130 0.1650 0.167 Uiso 1 1 d R
H16R H 0.3058 0.0168 0.0845 0.167 Uiso 1 1 d R
H17R H 0.2442 -0.0495 0.1188 0.167 Uiso 1 1 d R
C2R C 0.3970(8) 0.2110(6) 0.2238(5) 0.073(2) Uani 1 1 d .
H2R H 0.4201 0.2017 0.2707 0.088 Uiso 1 1 d R
C3R C 0.4510(7) 0.2858(6) 0.2144(6) 0.075(2) Uani 1 1 d .
H3R H 0.5103 0.3252 0.2556 0.090 Uiso 1 1 d R
C4R C 0.4217(8) 0.3047(6) 0.1481(6) 0.077(2) Uani 1 1 d .
C41R C 0.4823(10) 0.3848(7) 0.1368(9) 0.110(4) Uani 1 1 d .
H41R H 0.5045 0.4284 0.1841 0.131 Uiso 1 1 d R
H42R H 0.4333 0.3943 0.0966 0.131 Uiso 1 1 d R
H43R H 0.5476 0.3827 0.1224 0.131 Uiso 1 1 d R
C5R C 0.3311(9) 0.2428(7) 0.0854(6) 0.078(3) Uani 1 1 d .
H5R H 0.3098 0.2531 0.0388 0.094 Uiso 1 1 d R
C6R C 0.2744(8) 0.1674(6) 0.0931(5) 0.077(2) Uani 1 1 d .
H6R H 0.2140 0.1283 0.0523 0.092 Uiso 1 1 d R
C1S C -0.1740(7) 0.2130(6) 0.0812(5) 0.076(2) Uani 1 1 d .
C11S C -0.2599(9) 0.1946(9) 0.1228(8) 0.108(4) Uani 1 1 d .
H11S H -0.2357 0.1682 0.1603 0.130 Uiso 1 1 d R
C12S C -0.2741(13) 0.2652(11) 0.1633(11) 0.149(6) Uani 1 1 d .
H12S H -0.2019 0.3070 0.1922 0.179 Uiso 1 1 d R
H13S H -0.3163 0.2517 0.1979 0.179 Uiso 1 1 d R
H14S H -0.3138 0.2848 0.1269 0.179 Uiso 1 1 d R
C13S C -0.3690(12) 0.1310(12) 0.0606(9) 0.179(9) Uani 1 1 d .
H15S H -0.4087 0.0926 0.0829 0.214 Uiso 1 1 d R
H16S H -0.3504 0.1023 0.0185 0.214 Uiso 1 1 d R
H17S H -0.4155 0.1589 0.0419 0.214 Uiso 1 1 d R
C2S C -0.1261(7) 0.2893(6) 0.0686(5) 0.069(2) Uani 1 1 d .
H2S H -0.1471 0.3326 0.0884 0.082 Uiso 1 1 d R
C3S C -0.0495(7) 0.3008(6) 0.0276(5) 0.067(2) Uani 1 1 d .
H3S H -0.0204 0.3515 0.0202 0.081 Uiso 1 1 d R
C4S C -0.0143(7) 0.2371(6) -0.0035(5) 0.072(2) Uani 1 1 d .
C41S C 0.0699(8) 0.2491(8) -0.0485(5) 0.092(3) Uani 1 1 d .
H41S H 0.0312 0.2381 -0.1019 0.111 Uiso 1 1 d R
H42S H 0.1087 0.2122 -0.0440 0.111 Uiso 1 1 d R
H43S H 0.1230 0.3046 -0.0280 0.111 Uiso 1 1 d R
C5S C -0.0565(8) 0.1627(5) 0.0131(6) 0.081(3) Uani 1 1 d .
H5S H -0.0325 0.1204 -0.0039 0.097 Uiso 1 1 d R
C6S C -0.1334(8) 0.1521(5) 0.0547(6) 0.077(2) Uani 1 1 d .
H6S H -0.1588 0.1028 0.0653 0.092 Uiso 1 1 d R
N1A N 0.2130(5) 0.6690(3) 0.3510(3) 0.0487(12) Uani 1 1 d .
C1AA C 0.1616(5) 0.5849(4) 0.3239(4) 0.0442(13) Uani 1 1 d .
C2A C 0.1439(5) 0.5419(4) 0.2457(4) 0.0436(13) Uani 1 1 d .
H2A H 0.1654 0.5717 0.2129 0.052 Uiso 1 1 d R
C3A C 0.0971(5) 0.4603(4) 0.2178(4) 0.0455(14) Uani 1 1 d .
H3A H 0.0863 0.4348 0.1660 0.055 Uiso 1 1 d R
C3AA C 0.0637(6) 0.4117(4) 0.2650(4) 0.0475(14) Uani 1 1 d .
N4A N 0.0242(5) 0.3282(3) 0.2355(3) 0.0495(13) Uani 1 1 d .
C5A C -0.0103(7) 0.2836(5) 0.2800(5) 0.065(2) Uani 1 1 d .
H5A H -0.0367 0.2268 0.2600 0.077 Uiso 1 1 d R
C6A C -0.0083(8) 0.3186(5) 0.3561(5) 0.067(2) Uani 1 1 d .
H6A H -0.0358 0.2854 0.3847 0.080 Uiso 1 1 d R
C7A C 0.0333(6) 0.4005(5) 0.3869(5) 0.0611(19) Uani 1 1 d .
H7A H 0.0362 0.4241 0.4374 0.073 Uiso 1 1 d R
C7AA C 0.0730(5) 0.4513(4) 0.3424(4) 0.0451(14) Uani 1 1 d .
C8A C 0.1361(6) 0.5827(5) 0.4478(4) 0.0563(17) Uani 1 1 d .
H8A H 0.1103 0.5546 0.4806 0.068 Uiso 1 1 d R
C8AA C 0.1238(5) 0.5395(4) 0.3719(4) 0.0451(14) Uani 1 1 d .
C9A C 0.1864(7) 0.6666(6) 0.4735(5) 0.071(2) Uani 1 1 d .
H9A H 0.1934 0.6960 0.5233 0.086 Uiso 1 1 d R
C10A C 0.2263(6) 0.7063(5) 0.4240(5) 0.0619(19) Uani 1 1 d .
H10A H 0.2649 0.7628 0.4432 0.074 Uiso 1 1 d R
N1B N 0.4747(5) 0.6734(4) 0.4113(3) 0.0503(13) Uani 1 1 d .
C1AB C 0.4338(5) 0.5885(4) 0.3878(4) 0.0461(14) Uani 1 1 d .
C2B C 0.4236(6) 0.5454(4) 0.3110(4) 0.0476(14) Uani 1 1 d .
H2B H 0.4487 0.5745 0.2787 0.057 Uiso 1 1 d R
C3B C 0.3781(6) 0.4633(4) 0.2847(4) 0.0501(15) Uani 1 1 d .
H3B H 0.3703 0.4368 0.2337 0.060 Uiso 1 1 d R
C3AB C 0.3417(6) 0.4154(4) 0.3322(4) 0.0476(14) Uani 1 1 d .
N4B N 0.2910(5) 0.3315(4) 0.3002(4) 0.0539(14) Uani 1 1 d .
C5B C 0.2530(8) 0.2896(5) 0.3473(5) 0.065(2) Uani 1 1 d .
H5B H 0.2180 0.2329 0.3271 0.078 Uiso 1 1 d R
C6B C 0.2629(8) 0.3257(6) 0.4230(5) 0.070(2) Uani 1 1 d .
H6B H 0.2342 0.2939 0.4524 0.085 Uiso 1 1 d R
C7B C 0.3153(6) 0.4090(5) 0.4547(4) 0.0564(17) Uani 1 1 d .
H7B H 0.3243 0.4338 0.5063 0.068 Uiso 1 1 d R
C7AB C 0.3543(5) 0.4558(4) 0.4107(4) 0.0485(15) Uani 1 1 d .
C8B C 0.4141(6) 0.5885(5) 0.5146(4) 0.0581(18) Uani 1 1 d .
H8B H 0.3954 0.5614 0.5498 0.070 Uiso 1 1 d R
C8AB C 0.4010(5) 0.5435(4) 0.4377(4) 0.0469(14) Uani 1 1 d .
C9B C 0.4544(7) 0.6721(5) 0.5355(4) 0.064(2) Uani 1 1 d .
H9B H 0.4637 0.7024 0.5855 0.077 Uiso 1 1 d R
C10B C 0.4813(7) 0.7114(5) 0.4831(4) 0.0621(19) Uani 1 1 d .
H10B H 0.5058 0.7683 0.4987 0.075 Uiso 1 1 d R
S1 S 0.2423(2) 0.51201(16) 0.05890(13) 0.0793(6) Uani 1 1 d D
O11T O 0.2597(8) 0.4417(5) 0.0711(5) 0.131(3) Uiso 1 1 d D
O12T O 0.3179(8) 0.5872(5) 0.1084(5) 0.145(3) Uiso 1 1 d D
O13T O 0.1289(7) 0.5040(7) 0.0478(7) 0.187(5) Uiso 1 1 d D
C1T C 0.2613(8) 0.5085(6) -0.0323(6) 0.112(4) Uiso 1 1 d D
F11T F 0.3579(7) 0.5066(6) -0.0325(5) 0.167(4) Uiso 1 1 d D
F12T F 0.1855(10) 0.4443(7) -0.0852(6) 0.225(5) Uiso 1 1 d D
F13T F 0.2542(9) 0.5709(6) -0.0533(6) 0.191(4) Uiso 1 1 d D
S2 S 0.7873(3) 0.5341(3) 0.37082(15) 0.1081(12) Uani 1 1 d D
O21T O 0.8613(6) 0.5057(5) 0.4106(4) 0.107(2) Uiso 1 1 d D
O22T O 0.6711(7) 0.4951(6) 0.3556(6) 0.156(4) Uiso 1 1 d D
O23T O 0.8215(11) 0.6215(6) 0.4036(7) 0.193(5) Uiso 1 1 d D
C2T C 0.8051(6) 0.5229(5) 0.2790(5) 0.075(2) Uiso 1 1 d D
F21T F 0.7438(6) 0.5504(4) 0.2357(4) 0.113(2) Uiso 1 1 d D
F22T F 0.9086(6) 0.5587(5) 0.2811(4) 0.131(2) Uiso 1 1 d D
F23T F 0.7750(9) 0.4465(6) 0.2440(6) 0.183(4) Uiso 1 1 d D
S3 S 0.4117(4) 0.9117(2) 0.6268(3) 0.1402(15) Uani 1 1 d D
O31T O 0.3488(10) 0.9025(8) 0.5517(6) 0.191(5) Uiso 1 1 d D
O32T O 0.4644(12) 0.8545(8) 0.6246(9) 0.234(7) Uiso 1 1 d D
O33T O 0.4837(13) 0.9937(7) 0.6660(10) 0.282(9) Uiso 1 1 d D
C3T C 0.3127(13) 0.8882(11) 0.6752(9) 0.55(4) Uiso 1 1 d D
F31T F 0.2611(17) 0.9383(14) 0.6729(14) 0.395(13) Uiso 1 1 d D
F32T F 0.2395(19) 0.8159(12) 0.6406(17) 0.51(2) Uiso 1 1 d D
F33T F 0.360(2) 0.893(2) 0.7446(11) 0.53(2) Uiso 1 1 d D
S4 S -0.0893(5) -0.0252(2) 0.1446(3) 0.159(2) Uani 1 1 d D
O41T O -0.0585(13) 0.0577(6) 0.1914(8) 0.240(7) Uiso 1 1 d D
O42T O -0.0846(12) -0.0335(9) 0.0715(6) 0.210(6) Uiso 1 1 d D
O43T O -0.0248(14) -0.0628(11) 0.1877(10) 0.296(10) Uiso 1 1 d D
C4T C -0.2231(11) -0.0736(8) 0.1489(8) 0.64(6) Uiso 1 1 d D
F41T F -0.2613(12) -0.1492(8) 0.1089(9) 0.275(7) Uiso 1 1 d D
F42T F -0.2102(14) -0.0673(11) 0.2218(8) 0.317(9) Uiso 1 1 d D
F43T F -0.2838(13) -0.0371(12) 0.1215(12) 0.365(12) 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
Ru1 0.0430(3) 0.0414(3) 0.0638(4) 0.0149(2) 0.0158(2) 0.0169(2)
Ru2 0.0411(3) 0.0470(3) 0.0589(3) 0.0159(2) 0.0164(2) 0.0158(2)
O1 0.044(2) 0.051(3) 0.056(3) 0.015(2) 0.014(2) 0.020(2)
O2 0.039(2) 0.112(5) 0.069(3) 0.041(3) 0.026(2) 0.041(3)
C1P 0.055(4) 0.064(5) 0.096(6) 0.027(5) 0.021(4) 0.032(4)
C11P 0.064(5) 0.101(7) 0.110(8) 0.033(6) 0.036(5) 0.045(5)
C12P 0.079(7) 0.177(13) 0.170(13) 0.071(11) 0.063(8) 0.080(9)
C13P 0.139(13) 0.174(15) 0.171(15) -0.036(12) 0.067(11) 0.082(12)
C2P 0.055(4) 0.049(4) 0.083(6) 0.023(4) 0.006(4) 0.018(3)
C3P 0.064(5) 0.062(5) 0.077(5) 0.030(4) 0.013(4) 0.033(4)
C4P 0.066(5) 0.092(7) 0.111(7) 0.070(6) 0.031(5) 0.047(5)
C41P 0.097(8) 0.140(10) 0.110(8) 0.084(8) 0.053(7) 0.062(7)
C5P 0.063(5) 0.046(4) 0.112(7) 0.032(5) 0.015(5) 0.017(4)
C6P 0.065(5) 0.046(4) 0.122(8) 0.022(5) 0.031(5) 0.027(4)
C1Q 0.054(5) 0.086(7) 0.116(9) 0.000(7) 0.014(5) 0.012(5)
C11Q 0.093(8) 0.099(9) 0.115(10) 0.003(8) 0.008(7) 0.012(7)
C12Q 0.189(17) 0.089(9) 0.131(12) 0.016(9) 0.030(12) -0.009(10)
C13Q 0.064(9) 0.33(3) 0.31(3) -0.10(3) -0.018(14) 0.021(15)
C2Q 0.055(5) 0.089(7) 0.087(6) 0.037(5) 0.026(4) 0.034(4)
C3Q 0.054(5) 0.059(5) 0.142(10) 0.007(6) 0.054(6) 0.016(4)
C4Q 0.053(5) 0.140(10) 0.060(5) 0.006(6) 0.024(4) -0.001(6)
C41Q 0.086(9) 0.29(2) 0.119(11) 0.021(13) 0.058(8) 0.043(12)
C5Q 0.071(6) 0.143(11) 0.155(12) 0.112(11) 0.059(8) 0.044(7)
C6Q 0.083(8) 0.089(8) 0.145(12) 0.045(9) 0.043(8) 0.005(6)
Ru3 0.0600(4) 0.0451(3) 0.0567(3) 0.0201(3) 0.0181(3) 0.0254(3)
Ru4 0.0536(3) 0.0416(3) 0.0603(4) 0.0156(3) 0.0178(3) 0.0159(2)
O3 0.047(2) 0.048(3) 0.060(3) 0.021(2) 0.017(2) 0.022(2)
O4 0.058(3) 0.078(4) 0.068(3) 0.031(3) 0.020(3) 0.033(3)
C1R 0.082(6) 0.056(4) 0.071(5) 0.018(4) 0.015(4) 0.040(4)
C11R 0.116(8) 0.052(5) 0.125(9) 0.034(5) 0.034(7) 0.036(5)
C12R 0.188(15) 0.074(7) 0.149(13) 0.046(8) 0.053(11) 0.055(9)
C13R 0.189(15) 0.053(6) 0.142(11) -0.011(6) 0.004(10) 0.061(8)
C2R 0.086(6) 0.070(5) 0.075(5) 0.023(4) 0.020(5) 0.048(5)
C3R 0.061(5) 0.072(6) 0.091(6) 0.015(5) 0.019(4) 0.034(4)
C4R 0.076(6) 0.075(6) 0.099(7) 0.028(5) 0.046(5) 0.041(5)
C41R 0.102(8) 0.110(9) 0.174(12) 0.085(9) 0.092(9) 0.053(7)
C5R 0.100(7) 0.102(7) 0.076(6) 0.048(5) 0.048(5) 0.067(6)
C6R 0.083(6) 0.079(6) 0.064(5) 0.001(4) 0.021(4) 0.041(5)
C1S 0.054(5) 0.086(6) 0.071(5) 0.014(5) 0.016(4) 0.013(4)
C11S 0.065(6) 0.126(10) 0.131(10) 0.033(8) 0.042(6) 0.027(6)
C12S 0.118(12) 0.161(15) 0.192(17) 0.058(13) 0.076(12) 0.061(11)
C13S 0.083(9) 0.230(19) 0.134(12) 0.002(12) 0.044(8) -0.030(10)
C2S 0.063(5) 0.074(5) 0.063(5) 0.016(4) 0.009(4) 0.027(4)
C3S 0.063(5) 0.069(5) 0.059(4) 0.020(4) 0.006(4) 0.019(4)
C4S 0.067(5) 0.085(6) 0.053(4) 0.015(4) 0.008(4) 0.026(5)
C41S 0.075(6) 0.144(10) 0.063(5) 0.028(6) 0.028(5) 0.046(6)
C5S 0.078(6) 0.054(5) 0.087(6) 0.006(4) 0.005(5) 0.018(4)
C6S 0.075(6) 0.055(5) 0.081(6) 0.009(4) 0.019(5) 0.008(4)
N1A 0.048(3) 0.046(3) 0.056(3) 0.012(2) 0.021(3) 0.021(2)
C1AA 0.041(3) 0.046(3) 0.048(3) 0.012(3) 0.016(3) 0.020(3)
C2A 0.050(3) 0.046(3) 0.043(3) 0.020(3) 0.020(3) 0.021(3)
C3A 0.044(3) 0.052(4) 0.043(3) 0.017(3) 0.015(3) 0.019(3)
C3AA 0.048(3) 0.050(4) 0.050(3) 0.017(3) 0.016(3) 0.025(3)
N4A 0.051(3) 0.045(3) 0.058(3) 0.022(3) 0.023(3) 0.016(2)
C5A 0.063(5) 0.055(4) 0.091(6) 0.036(4) 0.039(4) 0.022(4)
C6A 0.084(6) 0.070(5) 0.076(5) 0.044(4) 0.050(5) 0.035(4)
C7A 0.058(4) 0.085(6) 0.061(4) 0.038(4) 0.031(4) 0.034(4)
C7AA 0.042(3) 0.059(4) 0.045(3) 0.024(3) 0.020(3) 0.023(3)
C8A 0.051(4) 0.073(5) 0.044(4) 0.016(3) 0.016(3) 0.023(4)
C8AA 0.038(3) 0.059(4) 0.044(3) 0.017(3) 0.016(3) 0.024(3)
C9A 0.063(5) 0.090(6) 0.049(4) 0.002(4) 0.021(4) 0.024(4)
C10A 0.052(4) 0.057(4) 0.069(5) 0.004(4) 0.018(4) 0.019(3)
N1B 0.046(3) 0.052(3) 0.050(3) 0.011(3) 0.013(2) 0.017(3)
C1AB 0.042(3) 0.052(4) 0.050(3) 0.021(3) 0.015(3) 0.021(3)
C2B 0.050(4) 0.053(4) 0.045(3) 0.018(3) 0.017(3) 0.022(3)
C3B 0.056(4) 0.056(4) 0.046(3) 0.019(3) 0.020(3) 0.026(3)
C3AB 0.048(3) 0.056(4) 0.050(4) 0.025(3) 0.017(3) 0.026(3)
N4B 0.061(4) 0.047(3) 0.062(3) 0.026(3) 0.020(3) 0.024(3)
C5B 0.085(6) 0.056(4) 0.073(5) 0.036(4) 0.030(4) 0.034(4)
C6B 0.092(6) 0.078(6) 0.067(5) 0.047(5) 0.034(5) 0.043(5)
C7B 0.059(4) 0.073(5) 0.050(4) 0.029(4) 0.018(3) 0.035(4)
C7AB 0.040(3) 0.062(4) 0.050(4) 0.023(3) 0.012(3) 0.023(3)
C8B 0.059(4) 0.074(5) 0.041(3) 0.015(3) 0.016(3) 0.026(4)
C8AB 0.038(3) 0.065(4) 0.045(3) 0.019(3) 0.011(3) 0.027(3)
C9B 0.068(5) 0.076(5) 0.044(4) 0.010(4) 0.023(3) 0.024(4)
C10B 0.062(4) 0.059(4) 0.058(4) 0.007(3) 0.017(4) 0.020(4)
S1 0.0972(17) 0.0829(15) 0.0603(12) 0.0249(11) 0.0338(12) 0.0281(13)
S2 0.0937(18) 0.213(4) 0.0680(14) 0.074(2) 0.0408(14) 0.091(2)
S3 0.158(4) 0.098(2) 0.133(3) -0.002(2) 0.009(3) 0.057(2)
S4 0.248(6) 0.078(2) 0.131(3) 0.026(2) 0.081(4) 0.022(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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Ru1 C2P 122.5(3)
O1 Ru1 N1A 85.22(19)
C2P Ru1 N1A 92.6(3)
O1 Ru1 C3P 97.0(3)
C2P Ru1 C3P 37.6(3)
N1A Ru1 C3P 120.1(3)
O1 Ru1 C5P 121.8(3)
C2P Ru1 C5P 79.5(3)
N1A Ru1 C5P 151.9(3)
C3P Ru1 C5P 68.0(3)
O1 Ru1 C6P 156.7(3)
C2P Ru1 C6P 67.8(3)
N1A Ru1 C6P 116.5(3)
C3P Ru1 C6P 79.8(4)
C5P Ru1 C6P 35.6(4)
O1 Ru1 C4P 96.0(3)
C2P Ru1 C4P 67.9(3)
N1A Ru1 C4P 157.7(3)
C3P Ru1 C4P 37.6(3)
C5P Ru1 C4P 38.4(4)
C6P Ru1 C4P 67.2(4)
O1 Ru1 O2 76.63(19)
C2P Ru1 O2 160.7(3)
N1A Ru1 O2 85.5(2)
C3P Ru1 O2 153.3(3)
C5P Ru1 O2 93.1(3)
C6P Ru1 O2 95.9(3)
C4P Ru1 O2 116.5(3)
O1 Ru1 C1P 159.3(3)
C2P Ru1 C1P 37.4(3)
N1A Ru1 C1P 90.3(3)
C3P Ru1 C1P 67.9(3)
C5P Ru1 C1P 67.0(3)
C6P Ru1 C1P 38.3(3)
C4P Ru1 C1P 80.7(3)
O2 Ru1 C1P 123.3(3)
O1 Ru2 N1B 85.2(2)
O1 Ru2 C3Q 112.8(3)
N1B Ru2 C3Q 102.0(4)
O1 Ru2 C5Q 109.1(4)
N1B Ru2 C5Q 165.1(4)
C3Q Ru2 C5Q 69.2(5)
O1 Ru2 C2Q 146.9(3)
N1B Ru2 C2Q 87.9(3)
C3Q Ru2 C2Q 37.7(4)
C5Q Ru2 C2Q 77.8(4)
O1 Ru2 C4Q 95.5(3)
N1B Ru2 C4Q 138.4(5)
C3Q Ru2 C4Q 39.9(5)
C5Q Ru2 C4Q 39.1(5)
C2Q Ru2 C4Q 69.1(4)
O1 Ru2 C6Q 137.9(5)
N1B Ru2 C6Q 133.0(5)
C3Q Ru2 C6Q 80.1(5)
C5Q Ru2 C6Q 35.6(5)
C2Q Ru2 C6Q 65.0(5)
C4Q Ru2 C6Q 68.4(5)
O1 Ru2 C1Q 171.8(4)
N1B Ru2 C1Q 102.9(4)
C3Q Ru2 C1Q 67.1(4)
C5Q Ru2 C1Q 62.8(5)
C2Q Ru2 C1Q 36.6(4)
C4Q Ru2 C1Q 79.3(4)
C6Q Ru2 C1Q 34.1(5)
O1 Ru2 O2 76.6(2)
N1B Ru2 O2 84.2(2)
C3Q Ru2 O2 168.9(3)
C5Q Ru2 O2 102.7(4)
C2Q Ru2 O2 134.8(3)
C4Q Ru2 O2 136.6(5)
C6Q Ru2 O2 89.0(4)
C1Q Ru2 O2 102.7(3)
Ru1 O1 Ru2 106.4(2)
Ru2 O2 Ru1 98.5(2)
C2P C1P C6P 115.8(8)
C2P C1P C11P 119.0(8)
C6P C1P C11P 125.1(9)
C2P C1P Ru1 68.4(4)
C6P C1P Ru1 69.4(4)
C11P C1P Ru1 131.7(7)
C1P C11P C12P 107.2(9)
C1P C11P C13P 112.2(10)
C12P C11P C13P 109.7(10)
C3P C2P C1P 122.4(8)
C3P C2P Ru1 71.3(5)
C1P C2P Ru1 74.2(5)
C2P C3P C4P 121.2(9)
C2P C3P Ru1 71.1(5)
C4P C3P Ru1 73.2(5)
C3P C4P C5P 116.6(8)
C3P C4P C41P 120.8(10)
C5P C4P C41P 122.6(10)
C3P C4P Ru1 69.2(5)
C5P C4P Ru1 70.0(5)
C41P C4P Ru1 129.6(6)
C6P C5P C4P 122.0(8)
C6P C5P Ru1 72.3(5)
C4P C5P Ru1 71.5(4)
C5P C6P C1P 122.0(9)
C5P C6P Ru1 72.1(5)
C1P C6P Ru1 72.3(4)
C6Q C1Q C2Q 123.7(13)
C6Q C1Q C11Q 123.2(13)
C2Q C1Q C11Q 113.0(12)
C6Q C1Q Ru2 72.9(7)
C2Q C1Q Ru2 70.5(5)
C11Q C1Q Ru2 128.9(9)
C12Q C11Q C13Q 108.1(16)
C12Q C11Q C1Q 116.4(14)
C13Q C11Q C1Q 107.5(15)
C1Q C2Q C3Q 120.6(10)
C1Q C2Q Ru2 72.8(6)
C3Q C2Q Ru2 70.9(5)
C2Q C3Q C4Q 118.0(9)
C2Q C3Q Ru2 71.3(5)
C4Q C3Q Ru2 71.1(5)
C5Q C4Q C3Q 113.5(9)
C5Q C4Q C41Q 127.9(15)
C3Q C4Q C41Q 118.6(14)
C5Q C4Q Ru2 69.6(5)
C3Q C4Q Ru2 69.1(5)
C41Q C4Q Ru2 132.7(7)
C6Q C5Q C4Q 123.8(11)
C6Q C5Q Ru2 73.3(6)
C4Q C5Q Ru2 71.3(6)
C1Q C6Q C5Q 120.3(14)
C1Q C6Q Ru2 73.0(7)
C5Q C6Q Ru2 71.0(7)
O3 Ru3 N4B 83.7(2)
O3 Ru3 O4 74.81(19)
N4B Ru3 O4 83.7(2)
O3 Ru3 C6R 115.7(3)
N4B Ru3 C6R 160.1(3)
O4 Ru3 C6R 96.7(3)
O3 Ru3 C5R 96.0(3)
N4B Ru3 C5R 151.3(4)
O4 Ru3 C5R 124.1(3)
C6R Ru3 C5R 37.5(4)
O3 Ru3 C3R 129.8(3)
N4B Ru3 C3R 91.7(3)
O4 Ru3 C3R 154.4(3)
C6R Ru3 C3R 79.4(4)
C5R Ru3 C3R 66.4(4)
O3 Ru3 C2R 167.0(3)
N4B Ru3 C2R 94.3(3)
O4 Ru3 C2R 117.9(3)
C6R Ru3 C2R 67.8(4)
C5R Ru3 C2R 79.5(4)
C3R Ru3 C2R 37.2(3)
O3 Ru3 C1R 151.7(3)
N4B Ru3 C1R 121.5(3)
O4 Ru3 C1R 94.2(3)
C6R Ru3 C1R 38.6(3)
C5R Ru3 C1R 68.3(3)
C3R Ru3 C1R 66.9(3)
C2R Ru3 C1R 36.9(3)
O3 Ru3 C4R 101.8(3)
N4B Ru3 C4R 113.6(3)
O4 Ru3 C4R 162.2(3)
C6R Ru3 C4R 68.6(4)
C5R Ru3 C4R 38.1(4)
C3R Ru3 C4R 36.2(4)
C2R Ru3 C4R 67.2(4)
C1R Ru3 C4R 80.7(3)
O3 Ru4 N4A 84.8(2)
O3 Ru4 C3S 99.1(3)
N4A Ru4 C3S 117.4(3)
O3 Ru4 O4 74.53(19)
N4A Ru4 O4 83.3(2)
C3S Ru4 O4 158.2(3)
O3 Ru4 C2S 126.6(3)
N4A Ru4 C2S 92.3(3)
C3S Ru4 C2S 37.4(3)
O4 Ru4 C2S 158.1(3)
O3 Ru4 C5S 117.1(3)
N4A Ru4 C5S 157.2(3)
C3S Ru4 C5S 67.8(4)
O4 Ru4 C5S 96.1(3)
C2S Ru4 C5S 79.8(4)
O3 Ru4 C6S 153.0(3)
N4A Ru4 C6S 120.0(3)
C3S Ru4 C6S 79.6(4)
O4 Ru4 C6S 96.6(3)
C2S Ru4 C6S 67.1(4)
C5S Ru4 C6S 37.3(4)
O3 Ru4 C4S 94.8(3)
N4A Ru4 C4S 155.0(3)
C3S Ru4 C4S 37.9(3)
O4 Ru4 C4S 120.8(3)
C2S Ru4 C4S 67.9(3)
C5S Ru4 C4S 37.6(4)
C6S Ru4 C4S 67.5(4)
O3 Ru4 C1S 164.1(3)
N4A Ru4 C1S 93.5(3)
C3S Ru4 C1S 67.6(3)
O4 Ru4 C1S 121.1(3)
C2S Ru4 C1S 37.5(3)
C5S Ru4 C1S 67.2(4)
C6S Ru4 C1S 36.9(4)
C4S Ru4 C1S 80.1(3)
Ru3 O3 Ru4 105.8(2)
Ru3 O4 Ru4 101.3(2)
C2R C1R C6R 118.0(8)
C2R C1R C11R 122.3(9)
C6R C1R C11R 119.7(9)
C2R C1R Ru3 71.1(5)
C6R C1R Ru3 69.4(4)
C11R C1R Ru3 129.7(7)
C12R C11R C1R 117.1(10)
C12R C11R C13R 110.6(10)
C1R C11R C13R 106.3(10)
C1R C2R C3R 120.5(9)
C1R C2R Ru3 72.0(5)
C3R C2R Ru3 71.2(5)
C4R C3R C2R 123.6(9)
C4R C3R Ru3 73.0(5)
C2R C3R Ru3 71.6(5)
C3R C4R C5R 117.1(9)
C3R C4R C41R 123.8(11)
C5R C4R C41R 119.1(10)
C3R C4R Ru3 70.8(5)
C5R C4R Ru3 69.8(5)
C41R C4R Ru3 132.5(6)
C6R C5R C4R 120.9(9)
C6R C5R Ru3 70.5(5)
C4R C5R Ru3 72.0(5)
C5R C6R C1R 119.9(9)
C5R C6R Ru3 71.9(5)
C1R C6R Ru3 72.0(5)
C6S C1S C2S 116.5(8)
C6S C1S C11S 118.4(10)
C2S C1S C11S 125.1(10)
C6S C1S Ru4 68.9(5)
C2S C1S Ru4 68.1(5)
C11S C1S Ru4 132.0(8)
C12S C11S C1S 113.4(12)
C12S C11S C13S 113.4(13)
C1S C11S C13S 105.7(11)
C3S C2S C1S 121.6(9)
C3S C2S Ru4 70.9(5)
C1S C2S Ru4 74.4(5)
C2S C3S C4S 121.6(9)
C2S C3S Ru4 71.7(5)
C4S C3S Ru4 73.5(5)
C5S C4S C3S 116.8(9)
C5S C4S C41S 121.1(10)
C3S C4S C41S 122.0(9)
C5S C4S Ru4 69.7(5)
C3S C4S Ru4 68.7(5)
C41S C4S Ru4 129.7(6)
C6S C5S C4S 120.9(9)
C6S C5S Ru4 71.4(6)
C4S C5S Ru4 72.7(5)
C5S C6S C1S 122.4(9)
C5S C6S Ru4 71.4(5)
C1S C6S Ru4 74.2(5)
C10A N1A C1AA 118.0(6)
C10A N1A Ru1 116.7(5)
C1AA N1A Ru1 125.2(4)
N1A C1AA C8AA 121.4(6)
N1A C1AA C2A 120.2(6)
C8AA C1AA C2A 118.4(6)
C3A C2A C1AA 122.1(6)
C2A C3A C3AA 121.6(6)
N4A C3AA C3A 119.6(6)
N4A C3AA C7AA 121.6(6)
C3A C3AA C7AA 118.8(6)
C5A N4A C3AA 118.6(6)
C5A N4A Ru4 116.0(5)
C3AA N4A Ru4 125.4(4)
N4A C5A C6A 122.8(7)
C7A C6A C5A 119.4(7)
C6A C7A C7AA 120.2(7)
C3AA C7AA C7A 117.2(7)
C3AA C7AA C8AA 118.9(6)
C7A C7AA C8AA 123.9(6)
C9A C8A C8AA 119.8(7)
C8A C8AA C1AA 118.0(6)
C8A C8AA C7AA 122.0(6)
C1AA C8AA C7AA 120.0(6)
C8A C9A C10A 118.7(7)
N1A C10A C9A 124.0(8)
C10B N1B C1AB 117.4(6)
C10B N1B Ru2 117.4(5)
C1AB N1B Ru2 125.2(4)
N1B C1AB C8AB 121.9(6)
N1B C1AB C2B 119.1(6)
C8AB C1AB C2B 119.0(6)
C3B C2B C1AB 120.8(6)
C2B C3B C3AB 122.1(6)
N4B C3AB C3B 118.8(6)
N4B C3AB C7AB 122.0(6)
C3B C3AB C7AB 119.1(6)
C5B N4B C3AB 116.1(6)
C5B N4B Ru3 117.5(5)
C3AB N4B Ru3 126.4(4)
N4B C5B C6B 124.1(8)
C7B C6B C5B 119.4(7)
C7AB C7B C6B 120.1(7)
C7B C7AB C3AB 118.4(7)
C7B C7AB C8AB 123.3(7)
C3AB C7AB C8AB 118.2(6)
C9B C8B C8AB 118.7(7)
C1AB C8AB C8B 117.6(7)
C1AB C8AB C7AB 120.6(6)
C8B C8AB C7AB 121.7(6)
C8B C9B C10B 120.2(7)
N1B C10B C9B 124.1(8)
O12T S1 O11T 117.3(6)
O12T S1 O13T 113.4(6)
O11T S1 O13T 111.7(6)
O12T S1 C1T 105.6(5)
O11T S1 C1T 102.9(5)
O13T S1 C1T 104.3(6)
F11T C1T F13T 107.2(9)
F11T C1T F12T 108.4(9)
F13T C1T F12T 106.4(9)
F11T C1T S1 110.7(7)
F13T C1T S1 113.0(8)
F12T C1T S1 110.9(8)
O21T S2 O22T 120.2(6)
O21T S2 O23T 110.6(6)
O22T S2 O23T 110.6(7)
O21T S2 C2T 106.4(4)
O22T S2 C2T 104.0(5)
O23T S2 C2T 103.4(6)
F23T C2T F21T 106.6(8)
F23T C2T F22T 107.6(8)
F21T C2T F22T 107.3(7)
F23T C2T S2 108.5(7)
F21T C2T S2 113.4(6)
F22T C2T S2 113.1(6)
O32T S3 O33T 115.0(9)
O32T S3 O31T 110.4(8)
O33T S3 O31T 111.6(8)
O32T S3 C3T 108.2(7)
O33T S3 C3T 106.5(8)
O31T S3 C3T 104.6(7)
F32T C3T F33T 109.3(13)
F32T C3T F31T 107.3(12)
F33T C3T F31T 111.8(13)
F32T C3T S3 110.7(12)
F33T C3T S3 110.4(12)
F31T C3T S3 107.3(11)
O42T S4 O41T 114.6(8)
O42T S4 O43T 114.9(9)
O41T S4 O43T 107.7(8)
O42T S4 C4T 113.2(7)
O41T S4 C4T 103.3(7)
O43T S4 C4T 101.8(7)
F43T C4T F41T 110.7(12)
F43T C4T F42T 114.6(12)
F41T C4T F42T 109.7(11)
F43T C4T S4 106.7(11)
F41T C4T S4 109.9(10)
F42T C4T S4 105.0(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 O1 2.078(5)
Ru1 C2P 2.146(8)
Ru1 N1A 2.147(6)
Ru1 C3P 2.147(8)
Ru1 C5P 2.179(8)
Ru1 C6P 2.181(8)
Ru1 C4P 2.199(9)
Ru1 O2 2.210(5)
Ru1 C1P 2.220(8)
Ru2 O1 2.091(5)
Ru2 N1B 2.152(6)
Ru2 C3Q 2.158(8)
Ru2 C5Q 2.162(9)
Ru2 C2Q 2.163(8)
Ru2 C4Q 2.185(9)
Ru2 C6Q 2.190(11)
Ru2 C1Q 2.192(10)
Ru2 O2 2.197(5)
C1P C2P 1.402(12)
C1P C6P 1.445(12)
C1P C11P 1.518(13)
C11P C12P 1.524(15)
C11P C13P 1.537(17)
C2P C3P 1.382(12)
C3P C4P 1.402(12)
C4P C5P 1.441(14)
C4P C41P 1.505(14)
C5P C6P 1.331(13)
C1Q C6Q 1.285(17)
C1Q C2Q 1.368(15)
C1Q C11Q 1.609(18)
C11Q C12Q 1.31(2)
C11Q C13Q 1.47(2)
C2Q C3Q 1.398(14)
C3Q C4Q 1.481(17)
C4Q C5Q 1.454(18)
C4Q C41Q 1.512(17)
C5Q C6Q 1.333(19)
Ru3 O3 2.087(4)
Ru3 N4B 2.136(6)
Ru3 O4 2.152(5)
Ru3 C6R 2.153(8)
Ru3 C5R 2.171(9)
Ru3 C3R 2.171(9)
Ru3 C2R 2.176(8)
Ru3 C1R 2.187(8)
Ru3 C4R 2.199(9)
Ru4 O3 2.093(5)
Ru4 N4A 2.137(6)
Ru4 C3S 2.151(8)
Ru4 O4 2.159(5)
Ru4 C2S 2.162(8)
Ru4 C5S 2.176(9)
Ru4 C6S 2.176(9)
Ru4 C4S 2.214(8)
Ru4 C1S 2.244(9)
C1R C2R 1.382(12)
C1R C6R 1.435(13)
C1R C11R 1.528(13)
C11R C12R 1.454(18)
C11R C13R 1.565(16)
C2R C3R 1.387(13)
C3R C4R 1.360(14)
C4R C5R 1.428(14)
C4R C41R 1.504(13)
C5R C6R 1.391(14)
C1S C6S 1.400(14)
C1S C2S 1.420(13)
C1S C11S 1.497(14)
C11S C12S 1.414(18)
C11S C13S 1.550(18)
C2S C3S 1.381(13)
C3S C4S 1.417(13)
C4S C5S 1.415(13)
C4S C41S 1.516(13)
C5S C6S 1.391(14)
N1A C10A 1.324(9)
N1A C1AA 1.377(8)
C1AA C8AA 1.406(9)
C1AA C2A 1.421(9)
C2A C3A 1.335(9)
C3A C3AA 1.416(9)
C3AA N4A 1.367(9)
C3AA C7AA 1.420(9)
N4A C5A 1.330(9)
C5A C6A 1.410(12)
C6A C7A 1.342(12)
C7A C7AA 1.422(9)
C7AA C8AA 1.443(10)
C8A C9A 1.372(12)
C8A C8AA 1.402(9)
C9A C10A 1.381(12)
N1B C10B 1.331(9)
N1B C1AB 1.385(9)
C1AB C8AB 1.413(9)
C1AB C2B 1.423(9)
C2B C3B 1.342(10)
C3B C3AB 1.423(9)
C3AB N4B 1.378(9)
C3AB C7AB 1.429(9)
N4B C5B 1.356(9)
C5B C6B 1.375(12)
C6B C7B 1.370(12)
C7B C7AB 1.366(10)
C7AB C8AB 1.431(10)
C8B C9B 1.366(12)
C8B C8AB 1.426(9)
C9B C10B 1.371(12)
S1 O12T 1.379(7)
S1 O11T 1.411(7)
S1 O13T 1.415(8)
S1 C1T 1.759(10)
C1T F11T 1.280(9)
C1T F13T 1.290(9)
C1T F12T 1.293(9)
S2 O21T 1.385(7)
S2 O22T 1.405(8)
S2 O23T 1.442(8)
S2 C2T 1.751(9)
C2T F23T 1.279(8)
C2T F21T 1.298(8)
C2T F22T 1.301(8)
S3 O32T 1.404(9)
S3 O33T 1.408(9)
S3 O31T 1.409(8)
S3 C3T 1.736(13)
C3T F32T 1.278(11)
C3T F33T 1.278(11)
C3T F31T 1.286(11)
S4 O42T 1.353(8)
S4 O41T 1.434(9)
S4 O43T 1.456(9)
S4 C4T 1.734(13)
C4T F43T 1.274(10)
C4T F41T 1.279(10)
C4T F42T 1.305(10)
|
1500021.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500021.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_1500021
loop_
_publ_author_name
'Miguel A. Galindo'
'Miguel Quir\'os'
'M. Angustias Romero'
'Jorge A.R. Navarro'
_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
;
Cyclic tetranuclear half-sandwich ruthenium(II) complexes with
4,7-phenanthroline and hydroxo bridges: Crystal structure, solution
behaviour and binding to nucleosides
;
_journal_name_full 'Journal of Inorganic Biochemistry'
_journal_page_first 1025
_journal_page_last 1032
_journal_paper_doi 10.1016/j.jinorgbio.2007.11.009
_journal_volume 102
_journal_year 2008
_chemical_formula_sum 'C64 H84 N8 O20 Ru4'
_chemical_formula_weight 1689.67
_chemical_name_systematic
;
?
;
_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 105.708(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 32.9293(14)
_cell_length_b 20.2105(9)
_cell_length_c 22.4980(9)
_cell_measurement_reflns_used 7395
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.10
_cell_measurement_theta_min 2.37
_cell_volume 14413.6(11)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0352
_diffrn_reflns_av_sigmaI/netI 0.0277
_diffrn_reflns_limit_h_max 43
_diffrn_reflns_limit_h_min -42
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 83214
_diffrn_reflns_theta_full 28.35
_diffrn_reflns_theta_max 28.35
_diffrn_reflns_theta_min 1.41
_diffrn_standards_decay_% 0
_diffrn_standards_number 854
_exptl_absorpt_coefficient_mu 0.897
_exptl_absorpt_correction_T_max 0.8340
_exptl_absorpt_correction_T_min 0.7442
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.557
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 6880
_exptl_crystal_size_max 0.51
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.21
_refine_diff_density_max 1.375
_refine_diff_density_min -0.872
_refine_diff_density_rms 0.170
_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 781
_refine_ls_number_reflns 16838
_refine_ls_number_restraints 24
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0881
_refine_ls_R_factor_gt 0.0675
_refine_ls_shift/su_max 0.015
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2340
_refine_ls_wR_factor_ref 0.2589
_reflns_number_gt 12013
_reflns_number_total 16838
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file ruterf.cif
_cod_data_source_block ruterf
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1500021
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
Ru1 Ru 0.363726(14) 0.42826(2) 0.380221(19) 0.04715(15) Uani 1 1 d .
Ru2 Ru 0.381577(13) 0.55603(2) 0.29890(2) 0.04768(15) Uani 1 1 d .
O1 O 0.34117(11) 0.47552(17) 0.29536(15) 0.0493(8) Uani 1 1 d .
O2 O 0.39436(12) 0.51947(19) 0.38893(17) 0.0569(9) Uani 1 1 d .
C1P C 0.3588(2) 0.3514(3) 0.4480(3) 0.0623(15) Uani 1 1 d .
C11P C 0.3367(3) 0.3508(4) 0.4992(3) 0.086(2) Uani 1 1 d .
H11P H 0.3426 0.3932 0.5208 0.103 Uiso 1 1 d R
C12P C 0.2906(4) 0.3425(6) 0.4794(5) 0.125(4) Uani 1 1 d .
H12P H 0.2785 0.3760 0.4496 0.150 Uiso 1 1 d R
H13P H 0.2795 0.3467 0.5145 0.150 Uiso 1 1 d R
H14P H 0.2838 0.2996 0.4612 0.150 Uiso 1 1 d R
C13P C 0.3584(4) 0.2958(5) 0.5456(4) 0.112(3) Uani 1 1 d .
H15P H 0.3477 0.2974 0.5813 0.134 Uiso 1 1 d R
H16P H 0.3883 0.3029 0.5579 0.134 Uiso 1 1 d R
H17P H 0.3524 0.2532 0.5263 0.134 Uiso 1 1 d R
C2P C 0.4001(2) 0.3744(4) 0.4588(3) 0.078(2) Uani 1 1 d .
H2P H 0.4138 0.3910 0.4976 0.093 Uiso 1 1 d R
C3P C 0.4219(2) 0.3733(4) 0.4121(4) 0.082(2) Uani 1 1 d .
H3P H 0.4496 0.3881 0.4211 0.099 Uiso 1 1 d R
C4P C 0.4025(3) 0.3507(4) 0.3541(4) 0.081(2) Uani 1 1 d .
C41P C 0.4248(3) 0.3497(5) 0.3031(5) 0.114(3) Uani 1 1 d .
H41P H 0.4509 0.3735 0.3165 0.137 Uiso 1 1 d R
H42P H 0.4072 0.3703 0.2667 0.137 Uiso 1 1 d R
H43P H 0.4304 0.3048 0.2939 0.137 Uiso 1 1 d R
C5P C 0.3592(2) 0.3303(3) 0.3413(3) 0.0665(16) Uani 1 1 d .
H5P H 0.3448 0.3177 0.3014 0.080 Uiso 1 1 d R
C6P C 0.3382(2) 0.3292(3) 0.3877(3) 0.0598(14) Uani 1 1 d .
H6P H 0.3106 0.3138 0.3788 0.072 Uiso 1 1 d R
C1Q C 0.4435(2) 0.6014(4) 0.3077(4) 0.0723(18) Uani 1 1 d .
C11Q C 0.4780(3) 0.6203(6) 0.3648(5) 0.122(4) Uani 1 1 d .
H11Q H 0.4816 0.5828 0.3933 0.146 Uiso 1 1 d R
C12Q C 0.5186(3) 0.6260(8) 0.3453(6) 0.165(6) Uani 1 1 d .
H12Q H 0.5130 0.6491 0.3066 0.199 Uiso 1 1 d R
H13Q H 0.5291 0.5826 0.3407 0.199 Uiso 1 1 d R
H14Q H 0.5392 0.6499 0.3761 0.199 Uiso 1 1 d R
C13Q C 0.4715(4) 0.6771(11) 0.3977(11) 0.300(16) Uani 1 1 d .
H15Q H 0.4511 0.7055 0.3711 0.361 Uiso 1 1 d R
H16Q H 0.4977 0.7004 0.4127 0.361 Uiso 1 1 d R
H17Q H 0.4613 0.6637 0.4320 0.361 Uiso 1 1 d R
C2Q C 0.4120(3) 0.6450(4) 0.2773(5) 0.088(2) Uani 1 1 d .
H2Q H 0.4119 0.6880 0.2921 0.106 Uiso 1 1 d R
C3Q C 0.3800(2) 0.6254(4) 0.2242(4) 0.086(2) Uani 1 1 d .
H3Q H 0.3591 0.6555 0.2051 0.103 Uiso 1 1 d R
C4Q C 0.3793(2) 0.5614(4) 0.2002(3) 0.0714(18) Uani 1 1 d .
C41Q C 0.3445(3) 0.5402(6) 0.1450(3) 0.118(4) Uani 1 1 d .
H41Q H 0.3558 0.5332 0.1104 0.142 Uiso 1 1 d R
H42Q H 0.3233 0.5740 0.1350 0.142 Uiso 1 1 d R
H43Q H 0.3321 0.4998 0.1543 0.142 Uiso 1 1 d R
C5Q C 0.4105(2) 0.5174(3) 0.2305(3) 0.0680(16) Uani 1 1 d .
H5Q H 0.4105 0.4747 0.2150 0.082 Uiso 1 1 d R
C6Q C 0.4417(2) 0.5351(3) 0.2833(3) 0.0674(16) Uani 1 1 d .
H6Q H 0.4616 0.5039 0.3031 0.081 Uiso 1 1 d R
Ru3 Ru 0.135489(13) 0.56864(2) 0.123215(19) 0.04505(14) Uani 1 1 d .
Ru4 Ru 0.116841(14) 0.43893(2) 0.20190(2) 0.05117(15) Uani 1 1 d .
O3 O 0.16332(11) 0.48293(18) 0.16794(17) 0.0506(8) Uani 1 1 d .
O4 O 0.09400(11) 0.53372(19) 0.17240(18) 0.0552(9) Uani 1 1 d .
C1R C 0.08762(19) 0.6211(3) 0.0519(3) 0.0583(14) Uani 1 1 d .
C11R C 0.0432(2) 0.6444(3) 0.0484(4) 0.0755(19) Uani 1 1 d .
H11R H 0.0258 0.6048 0.0474 0.091 Uiso 1 1 d R
C12R C 0.0386(3) 0.6855(5) 0.1004(5) 0.111(3) Uani 1 1 d .
H12R H 0.0502 0.6624 0.1385 0.133 Uiso 1 1 d R
H13R H 0.0093 0.6945 0.0957 0.133 Uiso 1 1 d R
H14R H 0.0535 0.7264 0.1007 0.133 Uiso 1 1 d R
C13R C 0.0267(3) 0.6794(6) -0.0127(5) 0.138(4) Uani 1 1 d .
H15R H -0.0031 0.6862 -0.0206 0.165 Uiso 1 1 d R
H16R H 0.0322 0.6528 -0.0451 0.165 Uiso 1 1 d R
H17R H 0.0406 0.7214 -0.0114 0.165 Uiso 1 1 d R
C2R C 0.12243(19) 0.6615(3) 0.0737(3) 0.0610(14) Uani 1 1 d .
H2R H 0.1190 0.7037 0.0881 0.073 Uiso 1 1 d R
C3R C 0.1638(2) 0.6388(3) 0.0741(3) 0.0639(15) Uani 1 1 d .
H3R H 0.1869 0.6664 0.0892 0.077 Uiso 1 1 d R
C4R C 0.1698(2) 0.5764(3) 0.0525(3) 0.0655(15) Uani 1 1 d .
C41R C 0.2139(2) 0.5532(5) 0.0524(4) 0.090(2) Uani 1 1 d .
H41R H 0.2346 0.5778 0.0827 0.108 Uiso 1 1 d R
H42R H 0.2181 0.5603 0.0123 0.108 Uiso 1 1 d R
H43R H 0.2168 0.5069 0.0623 0.108 Uiso 1 1 d R
C5R C 0.1342(2) 0.5358(3) 0.0312(3) 0.0665(16) Uani 1 1 d .
H5R H 0.1376 0.4936 0.0168 0.080 Uiso 1 1 d R
C6R C 0.0943(2) 0.5568(3) 0.0309(3) 0.0620(15) Uani 1 1 d .
H6R H 0.0714 0.5284 0.0168 0.074 Uiso 1 1 d R
C1S C 0.0913(2) 0.3656(3) 0.2554(4) 0.0730(18) Uani 1 1 d .
C11S C 0.0869(3) 0.3645(4) 0.3211(4) 0.095(2) Uani 1 1 d .
H11S H 0.0703 0.4030 0.3266 0.114 Uiso 1 1 d R
C12S C 0.1258(4) 0.3637(5) 0.3708(4) 0.121(4) Uani 1 1 d .
H12S H 0.1430 0.3271 0.3653 0.146 Uiso 1 1 d R
H13S H 0.1192 0.3593 0.4097 0.146 Uiso 1 1 d R
H14S H 0.1409 0.4043 0.3704 0.146 Uiso 1 1 d R
C13S C 0.0613(4) 0.3020(6) 0.3247(5) 0.146(5) Uani 1 1 d .
H15S H 0.0670 0.2690 0.2973 0.175 Uiso 1 1 d R
H16S H 0.0318 0.3124 0.3130 0.175 Uiso 1 1 d R
H17S H 0.0693 0.2853 0.3662 0.175 Uiso 1 1 d R
C2S C 0.1272(2) 0.3395(3) 0.2401(4) 0.0728(18) Uani 1 1 d .
H2S H 0.1495 0.3228 0.2712 0.087 Uiso 1 1 d R
C3S C 0.1297(2) 0.3386(3) 0.1797(3) 0.0698(17) Uani 1 1 d .
H3S H 0.1538 0.3220 0.1709 0.084 Uiso 1 1 d R
C4S C 0.0955(3) 0.3627(4) 0.1304(4) 0.079(2) Uani 1 1 d .
C41S C 0.0983(3) 0.3606(5) 0.0640(4) 0.103(3) Uani 1 1 d .
H41S H 0.0883 0.3185 0.0461 0.124 Uiso 1 1 d R
H42S H 0.1271 0.3667 0.0633 0.124 Uiso 1 1 d R
H43S H 0.0812 0.3952 0.0407 0.124 Uiso 1 1 d R
C5S C 0.0614(2) 0.3905(3) 0.1462(4) 0.0742(19) Uani 1 1 d .
H5S H 0.0395 0.4085 0.1153 0.089 Uiso 1 1 d R
C6S C 0.0588(2) 0.3923(4) 0.2063(4) 0.0761(19) Uani 1 1 d .
H6S H 0.0354 0.4113 0.2150 0.091 Uiso 1 1 d R
N1A N 0.31716(15) 0.4848(2) 0.40849(19) 0.0507(10) Uani 1 1 d .
C1AA C 0.27421(16) 0.4852(2) 0.3809(2) 0.0448(10) Uani 1 1 d .
C2A C 0.25721(16) 0.4465(2) 0.3269(2) 0.0462(11) Uani 1 1 d .
H2A H 0.2752 0.4200 0.3117 0.055 Uiso 1 1 d R
C3A C 0.21679(18) 0.4475(3) 0.2981(2) 0.0493(12) Uani 1 1 d .
H3A H 0.2069 0.4213 0.2632 0.059 Uiso 1 1 d R
C3AA C 0.18727(16) 0.4880(2) 0.3191(2) 0.0469(11) Uani 1 1 d .
N4A N 0.14597(14) 0.4902(2) 0.2854(2) 0.0526(10) Uani 1 1 d .
C5A C 0.1192(2) 0.5261(3) 0.3083(3) 0.0641(15) Uani 1 1 d .
H5A H 0.0909 0.5281 0.2860 0.077 Uiso 1 1 d R
C6A C 0.1321(2) 0.5601(4) 0.3638(3) 0.0733(18) Uani 1 1 d .
H6A H 0.1124 0.5828 0.3789 0.088 Uiso 1 1 d R
C7A C 0.1732(2) 0.5601(3) 0.3959(3) 0.0671(16) Uani 1 1 d .
H7A H 0.1820 0.5844 0.4323 0.081 Uiso 1 1 d R
C7AA C 0.20249(18) 0.5235(3) 0.3744(2) 0.0509(12) Uani 1 1 d .
C8A C 0.2647(2) 0.5589(3) 0.4604(3) 0.0610(14) Uani 1 1 d .
H8A H 0.2474 0.5840 0.4781 0.073 Uiso 1 1 d R
C8AA C 0.24721(18) 0.5233(2) 0.4056(2) 0.0487(11) Uani 1 1 d .
C9A C 0.3062(2) 0.5566(3) 0.4870(3) 0.0676(17) Uani 1 1 d .
H9A H 0.3176 0.5795 0.5236 0.081 Uiso 1 1 d R
C10A C 0.3324(2) 0.5203(3) 0.4601(3) 0.0596(14) Uani 1 1 d .
H10A H 0.3614 0.5207 0.4784 0.072 Uiso 1 1 d R
N1B N 0.33568(14) 0.6139(2) 0.32838(19) 0.0492(10) Uani 1 1 d .
C1AB C 0.29371(16) 0.6198(2) 0.2983(2) 0.0440(10) Uani 1 1 d .
C2B C 0.27629(16) 0.5812(2) 0.2442(2) 0.0448(10) Uani 1 1 d .
H2B H 0.2939 0.5544 0.2286 0.054 Uiso 1 1 d R
C3B C 0.23480(16) 0.5830(2) 0.2155(2) 0.0461(11) Uani 1 1 d .
H3B H 0.2245 0.5578 0.1800 0.055 Uiso 1 1 d R
C3AB C 0.20604(16) 0.6224(2) 0.2377(2) 0.0434(10) Uani 1 1 d .
N4B N 0.16405(13) 0.6195(2) 0.20896(19) 0.0478(9) Uani 1 1 d .
C5B C 0.13826(19) 0.6567(3) 0.2316(3) 0.0574(13) Uani 1 1 d .
H5B H 0.1094 0.6539 0.2129 0.069 Uiso 1 1 d R
C6B C 0.1517(2) 0.6989(3) 0.2810(3) 0.0625(15) Uani 1 1 d .
H6B H 0.1324 0.7248 0.2942 0.075 Uiso 1 1 d R
C7B C 0.19355(19) 0.7024(3) 0.3104(3) 0.0584(14) Uani 1 1 d .
H7B H 0.2030 0.7305 0.3439 0.070 Uiso 1 1 d R
C7AB C 0.22227(18) 0.6638(2) 0.2901(2) 0.0479(11) Uani 1 1 d .
C8B C 0.2847(2) 0.7009(3) 0.3728(3) 0.0601(14) Uani 1 1 d .
H8B H 0.2681 0.7303 0.3879 0.072 Uiso 1 1 d R
C8AB C 0.26699(17) 0.6626(2) 0.3208(2) 0.0475(11) Uani 1 1 d .
C9B C 0.3274(2) 0.6945(3) 0.4017(3) 0.0682(16) Uani 1 1 d .
H9B H 0.3400 0.7201 0.4361 0.082 Uiso 1 1 d R
C10B C 0.35118(19) 0.6500(3) 0.3792(3) 0.0611(14) Uani 1 1 d .
H10B H 0.3794 0.6447 0.4005 0.073 Uiso 1 1 d R
N1N N 0.2734(3) 0.7305(4) 0.1633(4) 0.107(2) Uiso 1 1 d D
O1N O 0.2385(3) 0.7430(4) 0.1704(5) 0.157(4) Uiso 1 1 d D
O2N O 0.3082(3) 0.7363(5) 0.2017(4) 0.166(4) Uiso 1 1 d D
O3N O 0.2720(4) 0.6886(6) 0.1210(5) 0.212(5) Uiso 1 1 d D
N2N N -0.0212(3) 0.5221(5) 0.1046(4) 0.132(3) Uiso 1 1 d D
O4N O -0.0483(3) 0.5652(5) 0.0773(4) 0.165(3) Uiso 1 1 d D
O5N O 0.0031(4) 0.5335(6) 0.1552(5) 0.229(5) Uiso 1 1 d D
O6N O -0.0040(4) 0.4949(6) 0.0661(5) 0.229(5) Uiso 1 1 d D
N3N N 0.2225(4) 0.3732(8) 0.0875(6) 0.227(6) Uiso 1 1 d D
O7N O 0.2584(3) 0.3467(6) 0.0867(5) 0.198(4) Uiso 1 1 d D
O8N O 0.2195(4) 0.3954(7) 0.1366(5) 0.225(5) Uiso 1 1 d D
O9N O 0.1940(4) 0.3807(8) 0.0393(6) 0.256(6) Uiso 1 1 d D
N4N N 0.4528(5) 0.531(2) 0.5519(11) 0.47(2) Uiso 1 1 d D
O10N O 0.4608(5) 0.5104(9) 0.5032(7) 0.265(6) Uiso 1 1 d D
O11N O 0.4807(6) 0.5557(11) 0.5956(8) 0.344(10) Uiso 1 1 d D
O12N O 0.4162(6) 0.540(2) 0.5562(13) 0.53(2) Uiso 1 1 d D
O1W O 0.3262(3) 0.3848(5) 0.1953(5) 0.170(3) Uiso 1 1 d .
O2W O 0.2167(7) 0.2710(11) -0.0237(11) 0.331(10) Uiso 1 1 d .
O3W O 0.2548(6) 0.3258(10) 0.2284(9) 0.244(8) Uiso 0.75 1 d P
O4W O 0.3666(8) 0.3432(14) 0.1208(13) 0.319(11) Uiso 0.75 1 d P
O5W O -0.0208(7) 0.6070(12) 0.2382(12) 0.215(10) Uiso 0.50 1 d P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0532(3) 0.0426(2) 0.0419(2) 0.00129(16) 0.00634(19) 0.00307(17)
Ru2 0.0439(3) 0.0431(2) 0.0515(3) 0.00235(17) 0.00527(19) -0.00230(16)
O1 0.051(2) 0.0472(19) 0.0443(18) 0.0019(15) 0.0043(15) -0.0069(15)
O2 0.058(2) 0.052(2) 0.051(2) 0.0021(16) -0.0024(17) -0.0050(17)
C1P 0.084(4) 0.049(3) 0.050(3) 0.006(2) 0.012(3) 0.008(3)
C11P 0.148(8) 0.059(4) 0.063(4) 0.008(3) 0.049(5) 0.007(4)
C12P 0.140(9) 0.136(9) 0.126(8) 0.060(7) 0.083(7) 0.045(7)
C13P 0.170(9) 0.102(7) 0.068(5) 0.036(5) 0.040(5) 0.022(6)
C2P 0.093(5) 0.062(4) 0.060(4) 0.009(3) -0.010(4) 0.010(4)
C3P 0.059(4) 0.076(5) 0.107(6) 0.022(4) 0.014(4) 0.014(3)
C4P 0.102(6) 0.059(4) 0.095(5) 0.016(4) 0.050(5) 0.028(4)
C41P 0.142(8) 0.086(6) 0.144(8) 0.018(5) 0.091(7) 0.031(6)
C5P 0.101(5) 0.045(3) 0.058(3) 0.001(2) 0.028(3) 0.007(3)
C6P 0.081(4) 0.041(3) 0.057(3) 0.004(2) 0.019(3) 0.001(3)
C1Q 0.053(3) 0.074(4) 0.096(5) -0.014(4) 0.030(3) -0.015(3)
C11Q 0.066(5) 0.168(10) 0.127(7) -0.059(7) 0.019(5) -0.054(6)
C12Q 0.068(6) 0.274(17) 0.149(10) -0.046(11) 0.021(6) -0.074(8)
C13Q 0.094(8) 0.37(3) 0.42(3) -0.33(3) 0.038(12) -0.066(12)
C2Q 0.081(5) 0.052(4) 0.148(8) 0.007(4) 0.057(5) -0.006(3)
C3Q 0.075(5) 0.085(5) 0.103(6) 0.045(5) 0.035(4) 0.010(4)
C4Q 0.065(4) 0.092(5) 0.058(4) 0.024(3) 0.019(3) -0.002(3)
C41Q 0.107(7) 0.188(11) 0.047(4) 0.020(5) 0.000(4) -0.026(7)
C5Q 0.078(4) 0.065(4) 0.068(4) -0.007(3) 0.033(3) -0.009(3)
C6Q 0.058(3) 0.070(4) 0.076(4) 0.000(3) 0.023(3) 0.005(3)
Ru3 0.0440(2) 0.0442(2) 0.0438(2) 0.00159(16) 0.00640(18) -0.00055(16)
Ru4 0.0462(3) 0.0475(3) 0.0569(3) 0.00746(18) 0.0089(2) -0.00038(17)
O3 0.0464(19) 0.050(2) 0.052(2) 0.0020(16) 0.0080(15) 0.0028(15)
O4 0.050(2) 0.055(2) 0.059(2) 0.0104(17) 0.0131(17) 0.0048(16)
C1R 0.056(3) 0.057(3) 0.055(3) 0.014(3) 0.003(2) -0.003(3)
C11R 0.053(3) 0.061(4) 0.101(5) 0.012(4) 0.002(3) -0.003(3)
C12R 0.070(5) 0.125(8) 0.136(8) 0.001(6) 0.024(5) 0.023(5)
C13R 0.072(5) 0.178(11) 0.138(8) 0.075(8) -0.015(5) 0.009(6)
C2R 0.062(4) 0.054(3) 0.060(3) 0.009(3) 0.003(3) -0.003(3)
C3R 0.064(4) 0.069(4) 0.056(3) 0.008(3) 0.010(3) -0.012(3)
C4R 0.068(4) 0.079(4) 0.049(3) 0.007(3) 0.015(3) 0.000(3)
C41R 0.075(5) 0.128(7) 0.078(5) -0.005(5) 0.038(4) 0.005(4)
C5R 0.089(5) 0.064(4) 0.044(3) -0.001(3) 0.013(3) -0.004(3)
C6R 0.063(4) 0.060(3) 0.054(3) 0.006(3) 0.000(3) -0.010(3)
C1S 0.073(4) 0.060(4) 0.088(5) 0.015(3) 0.026(4) -0.004(3)
C11S 0.116(7) 0.084(5) 0.093(6) 0.027(4) 0.041(5) -0.006(5)
C12S 0.193(11) 0.090(6) 0.086(6) 0.024(5) 0.047(7) -0.014(7)
C13S 0.175(11) 0.144(10) 0.124(8) 0.039(7) 0.052(8) -0.056(9)
C2S 0.074(4) 0.049(3) 0.087(5) 0.015(3) 0.008(4) 0.004(3)
C3S 0.073(4) 0.048(3) 0.089(5) -0.004(3) 0.022(4) -0.005(3)
C4S 0.084(5) 0.064(4) 0.082(5) -0.005(3) 0.010(4) -0.024(4)
C41S 0.124(7) 0.105(6) 0.077(5) -0.023(5) 0.020(5) -0.038(6)
C5S 0.052(3) 0.068(4) 0.090(5) 0.012(3) -0.002(3) -0.014(3)
C6S 0.057(4) 0.068(4) 0.101(6) 0.016(4) 0.017(4) -0.005(3)
N1A 0.062(3) 0.046(2) 0.042(2) -0.0021(17) 0.0093(19) 0.003(2)
C1AA 0.055(3) 0.041(2) 0.039(2) 0.0035(19) 0.013(2) 0.001(2)
C2A 0.052(3) 0.042(2) 0.044(3) -0.001(2) 0.013(2) 0.007(2)
C3A 0.062(3) 0.044(3) 0.041(3) -0.006(2) 0.013(2) 0.001(2)
C3AA 0.052(3) 0.044(3) 0.047(3) 0.006(2) 0.017(2) 0.002(2)
N4A 0.053(3) 0.054(3) 0.053(2) 0.008(2) 0.019(2) 0.005(2)
C5A 0.060(3) 0.069(4) 0.069(4) 0.012(3) 0.027(3) 0.012(3)
C6A 0.077(4) 0.079(4) 0.071(4) -0.001(3) 0.032(4) 0.021(3)
C7A 0.085(5) 0.066(4) 0.059(3) -0.002(3) 0.035(3) 0.014(3)
C7AA 0.065(3) 0.047(3) 0.046(3) 0.008(2) 0.024(2) 0.008(2)
C8A 0.077(4) 0.060(3) 0.051(3) -0.010(2) 0.024(3) -0.004(3)
C8AA 0.065(3) 0.043(3) 0.041(2) 0.001(2) 0.019(2) -0.002(2)
C9A 0.090(5) 0.064(4) 0.047(3) -0.019(3) 0.016(3) -0.004(3)
C10A 0.067(4) 0.060(3) 0.046(3) -0.006(2) 0.005(3) -0.003(3)
N1B 0.051(2) 0.045(2) 0.046(2) -0.0044(18) 0.0038(18) -0.0042(19)
C1AB 0.050(3) 0.037(2) 0.042(2) 0.0000(19) 0.008(2) -0.002(2)
C2B 0.050(3) 0.040(2) 0.041(2) -0.0031(19) 0.008(2) 0.001(2)
C3B 0.050(3) 0.044(3) 0.042(2) -0.007(2) 0.009(2) 0.000(2)
C3AB 0.050(3) 0.038(2) 0.041(2) -0.0006(19) 0.012(2) 0.002(2)
N4B 0.051(2) 0.044(2) 0.049(2) 0.0018(18) 0.0143(19) 0.0046(18)
C5B 0.055(3) 0.059(3) 0.059(3) -0.001(3) 0.016(3) 0.008(3)
C6B 0.067(4) 0.053(3) 0.073(4) -0.006(3) 0.030(3) 0.012(3)
C7B 0.069(4) 0.051(3) 0.056(3) -0.012(2) 0.019(3) 0.006(3)
C7AB 0.062(3) 0.039(2) 0.042(3) 0.0019(19) 0.014(2) 0.004(2)
C8B 0.075(4) 0.050(3) 0.051(3) -0.013(2) 0.009(3) 0.002(3)
C8AB 0.062(3) 0.035(2) 0.042(2) -0.0014(19) 0.008(2) -0.002(2)
C9B 0.079(4) 0.060(4) 0.055(3) -0.015(3) 0.001(3) -0.010(3)
C10B 0.060(3) 0.057(3) 0.055(3) -0.012(3) -0.003(3) -0.005(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Ru1 O2 73.99(14)
O1 Ru1 N1A 85.49(15)
O2 Ru1 N1A 82.40(17)
O1 Ru1 C2P 165.7(3)
O2 Ru1 C2P 102.9(2)
N1A Ru1 C2P 108.1(3)
O1 Ru1 C5P 94.62(19)
O2 Ru1 C5P 146.1(2)
N1A Ru1 C5P 129.3(2)
C2P Ru1 C5P 80.3(3)
O1 Ru1 C3P 127.1(3)
O2 Ru1 C3P 93.5(2)
N1A Ru1 C3P 144.8(3)
C2P Ru1 C3P 38.6(3)
C5P Ru1 C3P 67.7(3)
O1 Ru1 C6P 116.07(19)
O2 Ru1 C6P 169.93(19)
N1A Ru1 C6P 98.3(2)
C2P Ru1 C6P 67.3(3)
C5P Ru1 C6P 37.5(2)
C3P Ru1 C6P 80.1(3)
O1 Ru1 C4P 99.8(2)
O2 Ru1 C4P 110.8(3)
N1A Ru1 C4P 166.7(2)
C2P Ru1 C4P 67.9(3)
C5P Ru1 C4P 38.5(3)
C3P Ru1 C4P 36.5(3)
C6P Ru1 C4P 68.4(3)
O1 Ru1 C1P 151.5(2)
O2 Ru1 C1P 132.82(19)
N1A Ru1 C1P 88.7(2)
C2P Ru1 C1P 37.3(3)
C5P Ru1 C1P 68.0(2)
C3P Ru1 C1P 68.6(3)
C6P Ru1 C1P 37.4(2)
C4P Ru1 C1P 80.8(2)
O2 Ru2 O1 73.78(14)
O2 Ru2 C6Q 97.8(2)
O1 Ru2 C6Q 116.5(2)
O2 Ru2 N1B 82.38(16)
O1 Ru2 N1B 86.67(15)
C6Q Ru2 N1B 156.0(2)
O2 Ru2 C5Q 123.4(2)
O1 Ru2 C5Q 95.2(2)
C6Q Ru2 C5Q 37.7(2)
N1B Ru2 C5Q 153.7(2)
O2 Ru2 C2Q 121.6(3)
O1 Ru2 C2Q 164.1(3)
C6Q Ru2 C2Q 68.0(3)
N1B Ru2 C2Q 91.4(2)
C5Q Ru2 C2Q 79.7(3)
O2 Ru2 C3Q 158.8(3)
O1 Ru2 C3Q 126.1(3)
C6Q Ru2 C3Q 80.3(3)
N1B Ru2 C3Q 90.9(2)
C5Q Ru2 C3Q 66.9(3)
C2Q Ru2 C3Q 38.0(3)
O2 Ru2 C1Q 97.0(2)
O1 Ru2 C1Q 153.5(2)
C6Q Ru2 C1Q 38.8(3)
N1B Ru2 C1Q 117.2(2)
C5Q Ru2 C1Q 68.8(3)
C2Q Ru2 C1Q 37.2(3)
C3Q Ru2 C1Q 68.2(3)
O2 Ru2 C4Q 159.6(2)
O1 Ru2 C4Q 98.7(2)
C6Q Ru2 C4Q 68.0(3)
N1B Ru2 C4Q 116.7(2)
C5Q Ru2 C4Q 37.1(3)
C2Q Ru2 C4Q 68.1(3)
C3Q Ru2 C4Q 37.3(3)
C1Q Ru2 C4Q 81.3(3)
Ru1 O1 Ru2 104.87(14)
Ru1 O2 Ru2 104.85(16)
C2P C1P C6P 117.5(6)
C2P C1P C11P 121.0(6)
C6P C1P C11P 121.5(7)
C2P C1P Ru1 68.6(4)
C6P C1P Ru1 70.5(3)
C11P C1P Ru1 131.9(4)
C12P C11P C1P 115.9(7)
C12P C11P C13P 111.7(7)
C1P C11P C13P 106.7(7)
C1P C2P C3P 121.9(7)
C1P C2P Ru1 74.1(4)
C3P C2P Ru1 71.3(4)
C4P C3P C2P 120.8(7)
C4P C3P Ru1 73.3(4)
C2P C3P Ru1 70.0(4)
C3P C4P C5P 118.0(6)
C3P C4P C41P 121.9(9)
C5P C4P C41P 120.1(8)
C3P C4P Ru1 70.2(4)
C5P C4P Ru1 69.0(4)
C41P C4P Ru1 130.1(5)
C6P C5P C4P 121.2(6)
C6P C5P Ru1 72.9(3)
C4P C5P Ru1 72.5(4)
C5P C6P C1P 120.5(6)
C5P C6P Ru1 69.7(3)
C1P C6P Ru1 72.1(3)
C2Q C1Q C6Q 116.9(7)
C2Q C1Q C11Q 123.0(8)
C6Q C1Q C11Q 120.2(8)
C2Q C1Q Ru2 70.7(4)
C6Q C1Q Ru2 68.7(3)
C11Q C1Q Ru2 130.3(6)
C13Q C11Q C1Q 117.7(11)
C13Q C11Q C12Q 111.1(11)
C1Q C11Q C12Q 106.8(8)
C1Q C2Q C3Q 121.4(7)
C1Q C2Q Ru2 72.2(4)
C3Q C2Q Ru2 71.0(4)
C4Q C3Q C2Q 120.9(7)
C4Q C3Q Ru2 72.4(4)
C2Q C3Q Ru2 70.9(4)
C5Q C4Q C3Q 118.0(7)
C5Q C4Q C41Q 121.3(8)
C3Q C4Q C41Q 120.6(8)
C5Q C4Q Ru2 69.9(4)
C3Q C4Q Ru2 70.4(4)
C41Q C4Q Ru2 128.9(5)
C4Q C5Q C6Q 122.1(7)
C4Q C5Q Ru2 73.1(4)
C6Q C5Q Ru2 70.4(4)
C5Q C6Q C1Q 120.6(6)
C5Q C6Q Ru2 71.9(4)
C1Q C6Q Ru2 72.5(4)
O3 Ru3 O4 74.35(14)
O3 Ru3 C3R 126.8(2)
O4 Ru3 C3R 157.4(2)
O3 Ru3 N4B 86.34(15)
O4 Ru3 N4B 82.96(16)
C3R Ru3 N4B 90.1(2)
O3 Ru3 C5R 95.7(2)
O4 Ru3 C5R 123.6(2)
C3R Ru3 C5R 67.1(2)
N4B Ru3 C5R 152.9(2)
O3 Ru3 C6R 116.74(19)
O4 Ru3 C6R 98.0(2)
C3R Ru3 C6R 80.0(2)
N4B Ru3 C6R 156.4(2)
C5R Ru3 C6R 37.1(2)
O3 Ru3 C2R 165.4(2)
O4 Ru3 C2R 119.7(2)
C3R Ru3 C2R 38.7(2)
N4B Ru3 C2R 91.4(2)
C5R Ru3 C2R 79.8(2)
C6R Ru3 C2R 67.5(2)
O3 Ru3 C4R 99.4(2)
O4 Ru3 C4R 160.6(2)
C3R Ru3 C4R 37.2(2)
N4B Ru3 C4R 115.4(2)
C5R Ru3 C4R 37.6(2)
C6R Ru3 C4R 67.9(2)
C2R Ru3 C4R 68.6(3)
O3 Ru3 C1R 152.67(19)
O4 Ru3 C1R 96.13(19)
C3R Ru3 C1R 68.4(2)
N4B Ru3 C1R 118.4(2)
C5R Ru3 C1R 67.9(3)
C6R Ru3 C1R 38.0(2)
C2R Ru3 C1R 37.0(2)
C4R Ru3 C1R 81.0(2)
O3 Ru4 O4 74.38(14)
O3 Ru4 N4A 85.19(16)
O4 Ru4 N4A 82.69(16)
O3 Ru4 C5S 124.9(2)
O4 Ru4 C5S 93.2(2)
N4A Ru4 C5S 147.4(3)
O3 Ru4 C6S 161.9(2)
O4 Ru4 C6S 99.7(2)
N4A Ru4 C6S 111.4(3)
C5S Ru4 C6S 37.3(3)
O3 Ru4 C3S 96.1(2)
O4 Ru4 C3S 149.4(2)
N4A Ru4 C3S 126.2(2)
C5S Ru4 C3S 68.1(3)
C6S Ru4 C3S 80.3(3)
O3 Ru4 C2S 119.1(2)
O4 Ru4 C2S 166.5(2)
N4A Ru4 C2S 96.6(2)
C5S Ru4 C2S 80.1(3)
C6S Ru4 C2S 67.9(3)
C3S Ru4 C2S 37.2(3)
O3 Ru4 C4S 98.7(2)
O4 Ru4 C4S 113.0(2)
N4A Ru4 C4S 164.3(2)
C5S Ru4 C4S 37.2(3)
C6S Ru4 C4S 67.5(3)
C3S Ru4 C4S 38.4(3)
C2S Ru4 C4S 68.1(3)
O3 Ru4 C1S 155.3(2)
O4 Ru4 C1S 128.8(2)
N4A Ru4 C1S 89.6(2)
C5S Ru4 C1S 67.9(3)
C6S Ru4 C1S 37.9(3)
C3S Ru4 C1S 67.9(3)
C2S Ru4 C1S 37.7(3)
C4S Ru4 C1S 80.5(3)
Ru4 O3 Ru3 105.11(15)
Ru4 O4 Ru3 104.17(16)
C2R C1R C6R 118.1(6)
C2R C1R C11R 121.9(6)
C6R C1R C11R 120.0(6)
C2R C1R Ru3 70.4(3)
C6R C1R Ru3 69.9(3)
C11R C1R Ru3 132.7(4)
C12R C11R C13R 111.7(8)
C12R C11R C1R 115.9(6)
C13R C11R C1R 107.1(7)
C1R C2R C3R 120.4(6)
C1R C2R Ru3 72.6(3)
C3R C2R Ru3 70.3(3)
C4R C3R C2R 121.0(6)
C4R C3R Ru3 72.8(4)
C2R C3R Ru3 70.9(3)
C3R C4R C5R 117.7(6)
C3R C4R C41R 120.5(6)
C5R C4R C41R 121.9(7)
C3R C4R Ru3 70.0(4)
C5R C4R Ru3 70.0(4)
C41R C4R Ru3 131.0(5)
C6R C5R C4R 122.0(6)
C6R C5R Ru3 71.5(4)
C4R C5R Ru3 72.3(4)
C5R C6R C1R 120.8(6)
C5R C6R Ru3 71.4(3)
C1R C6R Ru3 72.1(3)
C2S C1S C6S 117.1(7)
C2S C1S C11S 122.3(7)
C6S C1S C11S 120.6(7)
C2S C1S Ru4 69.7(4)
C6S C1S Ru4 68.9(4)
C11S C1S Ru4 133.3(5)
C12S C11S C1S 116.8(8)
C12S C11S C13S 109.4(8)
C1S C11S C13S 105.2(8)
C3S C2S C1S 121.2(6)
C3S C2S Ru4 70.7(4)
C1S C2S Ru4 72.6(4)
C2S C3S C4S 120.8(7)
C2S C3S Ru4 72.0(4)
C4S C3S Ru4 72.4(4)
C5S C4S C3S 117.4(7)
C5S C4S C41S 122.1(8)
C3S C4S C41S 120.4(8)
C5S C4S Ru4 69.4(4)
C3S C4S Ru4 69.2(4)
C41S C4S Ru4 130.3(5)
C6S C5S C4S 122.1(7)
C6S C5S Ru4 71.6(4)
C4S C5S Ru4 73.4(4)
C5S C6S C1S 121.3(7)
C5S C6S Ru4 71.1(4)
C1S C6S Ru4 73.2(4)
C10A N1A C1AA 118.9(5)
C10A N1A Ru1 114.3(4)
C1AA N1A Ru1 126.7(3)
N1A C1AA C8AA 120.5(5)
N1A C1AA C2A 119.8(4)
C8AA C1AA C2A 119.6(5)
C3A C2A C1AA 121.6(5)
C2A C3A C3AA 121.9(5)
N4A C3AA C7AA 122.5(5)
N4A C3AA C3A 119.6(5)
C7AA C3AA C3A 117.9(5)
C5A N4A C3AA 117.5(5)
C5A N4A Ru4 114.4(4)
C3AA N4A Ru4 128.0(4)
N4A C5A C6A 122.5(6)
C7A C6A C5A 120.0(6)
C6A C7A C7AA 119.9(6)
C7A C7AA C3AA 117.5(5)
C7A C7AA C8AA 122.5(5)
C3AA C7AA C8AA 120.0(5)
C9A C8A C8AA 120.0(6)
C1AA C8AA C8A 118.4(5)
C1AA C8AA C7AA 118.7(5)
C8A C8AA C7AA 122.9(5)
C8A C9A C10A 120.3(5)
N1A C10A C9A 121.9(6)
C10B N1B C1AB 118.4(5)
C10B N1B Ru2 115.0(4)
C1AB N1B Ru2 126.4(3)
N1B C1AB C8AB 121.1(4)
N1B C1AB C2B 119.5(4)
C8AB C1AB C2B 119.4(4)
C3B C2B C1AB 121.1(5)
C2B C3B C3AB 122.0(5)
N4B C3AB C7AB 121.6(4)
N4B C3AB C3B 119.6(4)
C7AB C3AB C3B 118.8(5)
C5B N4B C3AB 117.6(5)
C5B N4B Ru3 116.1(4)
C3AB N4B Ru3 125.9(3)
N4B C5B C6B 124.0(5)
C7B C6B C5B 119.1(5)
C6B C7B C7AB 120.1(5)
C7B C7AB C3AB 117.5(5)
C7B C7AB C8AB 123.1(5)
C3AB C7AB C8AB 119.3(4)
C9B C8B C8AB 118.9(5)
C8B C8AB C1AB 118.6(5)
C8B C8AB C7AB 122.1(5)
C1AB C8AB C7AB 119.2(4)
C10B C9B C8B 119.6(5)
N1B C10B C9B 123.3(5)
O1N N1N O2N 127.6(9)
O1N N1N O3N 113.0(9)
O2N N1N O3N 115.3(9)
O5N N2N O6N 114.5(10)
O5N N2N O4N 120.9(10)
O6N N2N O4N 110.3(9)
O8N N3N O9N 121.4(12)
O8N N3N O7N 117.3(11)
O9N N3N O7N 121.1(11)
O12N N4N O11N 114.0(13)
O12N N4N O10N 123.0(14)
O11N N4N O10N 122.0(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 O1 2.084(3)
Ru1 O2 2.085(4)
Ru1 N1A 2.142(4)
Ru1 C2P 2.144(6)
Ru1 C5P 2.153(6)
Ru1 C3P 2.161(7)
Ru1 C6P 2.194(6)
Ru1 C4P 2.199(6)
Ru1 C1P 2.215(6)
Ru2 O2 2.089(4)
Ru2 O1 2.090(3)
Ru2 C6Q 2.144(6)
Ru2 N1B 2.153(4)
Ru2 C5Q 2.163(6)
Ru2 C2Q 2.177(7)
Ru2 C3Q 2.178(7)
Ru2 C1Q 2.196(6)
Ru2 C4Q 2.204(6)
C1P C2P 1.396(10)
C1P C6P 1.416(8)
C1P C11P 1.517(9)
C11P C12P 1.471(13)
C11P C13P 1.559(10)
C2P C3P 1.425(11)
C3P C4P 1.365(11)
C4P C5P 1.437(11)
C4P C41P 1.521(11)
C5P C6P 1.397(9)
C1Q C2Q 1.393(11)
C1Q C6Q 1.443(10)
C1Q C11Q 1.514(11)
C11Q C13Q 1.413(15)
C11Q C12Q 1.520(13)
C2Q C3Q 1.419(12)
C3Q C4Q 1.400(11)
C4Q C5Q 1.389(10)
C4Q C41Q 1.508(10)
C5Q C6Q 1.391(9)
Ru3 O3 2.087(4)
Ru3 O4 2.100(4)
Ru3 C3R 2.158(6)
Ru3 N4B 2.163(4)
Ru3 C5R 2.163(6)
Ru3 C6R 2.165(6)
Ru3 C2R 2.166(6)
Ru3 C4R 2.193(6)
Ru3 C1R 2.194(6)
Ru4 O3 2.086(4)
Ru4 O4 2.099(4)
Ru4 N4A 2.132(5)
Ru4 C5S 2.150(6)
Ru4 C6S 2.157(7)
Ru4 C3S 2.159(6)
Ru4 C2S 2.175(6)
Ru4 C4S 2.200(7)
Ru4 C1S 2.213(6)
C1R C2R 1.385(8)
C1R C6R 1.420(9)
C1R C11R 1.520(9)
C11R C12R 1.474(12)
C11R C13R 1.512(11)
C2R C3R 1.434(9)
C3R C4R 1.386(9)
C4R C5R 1.405(9)
C4R C41R 1.525(9)
C5R C6R 1.378(9)
C1S C2S 1.418(10)
C1S C6S 1.419(10)
C1S C11S 1.524(11)
C11S C12S 1.455(13)
C11S C13S 1.534(12)
C2S C3S 1.384(10)
C3S C4S 1.435(10)
C4S C5S 1.388(11)
C4S C41S 1.520(11)
C5S C6S 1.378(11)
N1A C10A 1.342(7)
N1A C1AA 1.382(7)
C1AA C8AA 1.400(7)
C1AA C2A 1.425(7)
C2A C3A 1.313(7)
C3A C3AA 1.444(7)
C3AA N4A 1.366(7)
C3AA C7AA 1.406(7)
N4A C5A 1.348(7)
C5A C6A 1.387(10)
C6A C7A 1.351(10)
C7A C7AA 1.403(8)
C7AA C8AA 1.450(8)
C8A C9A 1.336(9)
C8A C8AA 1.409(7)
C9A C10A 1.389(9)
N1B C10B 1.337(7)
N1B C1AB 1.370(6)
C1AB C8AB 1.421(7)
C1AB C2B 1.428(7)
C2B C3B 1.344(7)
C3B C3AB 1.428(7)
C3AB N4B 1.360(6)
C3AB C7AB 1.426(7)
N4B C5B 1.334(7)
C5B C6B 1.377(8)
C6B C7B 1.358(9)
C7B C7AB 1.394(7)
C7AB C8AB 1.447(8)
C8B C9B 1.388(9)
C8B C8AB 1.392(7)
C9B C10B 1.374(9)
N1N O1N 1.231(7)
N1N O2N 1.238(7)
N1N O3N 1.265(8)
N2N O5N 1.223(8)
N2N O6N 1.279(8)
N2N O4N 1.279(8)
N3N O8N 1.222(8)
N3N O9N 1.236(8)
N3N O7N 1.302(8)
N4N O12N 1.247(9)
N4N O11N 1.251(9)
N4N O10N 1.267(9)
|
1500022.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500022.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_1500022
loop_
_publ_author_name
'Maria Lalia-Kantouri'
'Christos D. Papadopoulos'
'Antonios G. Hatzidimitriou'
'Miguel Quir\'os'
_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
;
Synthesis and characterization of new Co(III) mixed-ligand complexes,
containing 2-hydroxy-aryloximes and \a-diimines. Crystal and molecular
strucutre of [Co(saox)(bipy)~2~]Br
;
_journal_name_full Polyhedron
_journal_page_first 1292
_journal_page_last 1302
_journal_paper_doi 10.1016/j.poly.2006.10.047
_journal_volume 26
_journal_year 2007
_chemical_formula_sum 'C28.81 H26.43 Br Co N5.33 O3.9'
_chemical_formula_weight 648.87
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2ac 2n'
_symmetry_space_group_name_H-M 'P n m a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_date 06-07-06
_audit_creation_method CRYSTALS_ver_12.83
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 17.7483(10)
_cell_length_b 36.829(2)
_cell_length_c 17.3196(10)
_cell_measurement_reflns_used 6423
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.73
_cell_measurement_theta_min 2.33
_cell_volume 11320.9(11)
_computing_cell_refinement 'Bruker SMART (Bruker, 1999)'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0542
_diffrn_reflns_av_sigmaI/netI 0.0467
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 48
_diffrn_reflns_limit_k_min -49
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 69254
_diffrn_reflns_theta_full 26.919
_diffrn_reflns_theta_max 28.336
_diffrn_reflns_theta_min 1.106
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_decay_% 0.07
_diffrn_standards_number 767
_exptl_absorpt_coefficient_mu 2.062
_exptl_absorpt_correction_T_max 0.8522
_exptl_absorpt_correction_T_min 0.4232
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour black
_exptl_crystal_density_diffrn 1.522
_exptl_crystal_description laminae
_exptl_crystal_F_000 5277.647
_exptl_crystal_size_max 0.59
_exptl_crystal_size_mid 0.37
_exptl_crystal_size_min 0.08
_refine_diff_density_max 1.80
_refine_diff_density_min -1.59
_refine_ls_extinction_method None
_refine_ls_goodness_of_fit_ref 1.0498
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 745
_refine_ls_number_reflns 8040
_refine_ls_number_restraints 23
_refine_ls_R_factor_all 0.0406
_refine_ls_R_factor_gt 0.0306
_refine_ls_shift/su_max 0.000604
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
9.68 13.3 4.23
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.0870
_refine_ls_wR_factor_gt 0.0728
_refine_ls_wR_factor_ref 0.0728
_reflns_limit_h_max 23
_reflns_limit_h_min 0
_reflns_limit_k_max 49
_reflns_limit_k_min 0
_reflns_limit_l_max 23
_reflns_limit_l_min 0
_reflns_number_gt 8040
_reflns_number_total 13502
_reflns_threshold_expression I>2.0\s(I)
_cod_data_source_file teloxime4.cif
_cod_data_source_block CRYSTALS_cif
_cod_original_formula_sum 'C28.81 H26.43 Br Co N5.33 O3.90'
_cod_database_code 1500022
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Co1 Co 0.51571(2) 0.110773(10) 0.80532(2) 0.0136 1.0000 Uani . .
Co2 Co 0.50918(2) 0.109170(11) 0.30951(2) 0.0157 1.0000 Uani . .
Br3 Br 0.212885(19) 0.000897(10) 0.26884(2) 0.0284 1.0000 Uani . .
Br4 Br 0.23868(5) 0.2500 0.42250(5) 0.0390 0.7000 Uani S T
Br5 Br 0.17574(5) 0.2500 0.71807(6) 0.0384 0.6000 Uani S T
Br6 Br 0.26706(13) 0.10555(6) 0.50442(12) 0.0440(5) 0.2000 Uiso . .
Br7 Br 0.36505(11) 0.2500 0.29057(11) 0.0404(4) 0.3000 Uiso S .
O8 O 0.61576(15) 0.06826(7) 0.89848(13) 0.0379 1.0000 Uani . .
O9 O 0.56183(11) 0.14191(5) 0.73290(11) 0.0174 1.0000 Uani . .
O10 O 0.42586(12) 0.05683(6) 0.38628(12) 0.0214 1.0000 Uani . .
O11 O 0.46112(12) 0.14076(6) 0.24088(12) 0.0205 1.0000 Uani . .
O12 O 0.29328(13) 0.02992(7) 0.43770(13) 0.0301 1.0000 Uani . .
O13 O 0.36819(14) 0.00338(6) 0.16152(14) 0.0289 1.0000 Uani . .
O14 O 0.2969(2) 0.250000(6) 0.5843(2) 0.0478 1.0000 Uani S T
O15 O 0.5217(5) 0.250000(7) 0.2286(5) 0.060(2) 0.6000 Uiso S .
O16 O 0.02313(13) 0.28831(6) 0.75688(13) 0.0275 1.0000 Uani . .
N17 N 0.60612(13) 0.08486(7) 0.82779(13) 0.0163 1.0000 Uani . .
N18 N 0.45906(13) 0.08603(7) 0.88496(13) 0.0143 1.0000 Uani . .
N19 N 0.54351(14) 0.14274(7) 0.88919(14) 0.0182 1.0000 Uani . .
N20 N 0.48665(13) 0.07735(6) 0.72403(13) 0.0150 1.0000 Uani . .
N21 N 0.42283(13) 0.13615(7) 0.77381(14) 0.0174 1.0000 Uani . .
N22 N 0.42291(13) 0.07923(7) 0.32693(13) 0.0158 1.0000 Uani . .
N23 N 0.56752(13) 0.08370(7) 0.38702(14) 0.0168 1.0000 Uani . .
N24 N 0.47723(14) 0.13768(7) 0.39664(14) 0.0191 1.0000 Uani . .
N25 N 0.54299(14) 0.08092(7) 0.22242(14) 0.0186 1.0000 Uani . .
N26 N 0.59809(14) 0.13904(8) 0.28475(15) 0.0237 1.0000 Uani . .
N27 N 0.3347(5) 0.2500 0.9201(5) 0.053(2) 0.6660 Uiso S .
N28 N 0.1898(5) 0.2500 1.0720(5) 0.057(2) 0.6660 Uiso S .
C29 C 0.67289(16) 0.10625(8) 0.71371(15) 0.0147 1.0000 Uani . .
C30 C 0.66489(16) 0.08459(8) 0.78310(16) 0.0153 1.0000 Uani . .
C31 C 0.62457(16) 0.13526(8) 0.69511(16) 0.0161 1.0000 Uani . .
C32 C 0.64488(17) 0.15830(8) 0.63487(17) 0.0189 1.0000 Uani . .
C33 C 0.70826(18) 0.15177(8) 0.59010(17) 0.0202 1.0000 Uani . .
C34 C 0.75396(17) 0.12198(9) 0.60505(17) 0.0211 1.0000 Uani . .
C35 C 0.73724(16) 0.09954(8) 0.66723(17) 0.0172 1.0000 Uani . .
C36 C 0.41211(16) 0.05794(8) 0.87606(17) 0.0179 1.0000 Uani . .
C37 C 0.37263(17) 0.04282(8) 0.93705(17) 0.0194 1.0000 Uani . .
C38 C 0.38264(18) 0.05712(9) 1.01069(17) 0.0211 1.0000 Uani . .
C39 C 0.43024(17) 0.08651(8) 1.01980(17) 0.0193 1.0000 Uani . .
C40 C 0.46758(15) 0.10082(8) 0.95727(16) 0.0149 1.0000 Uani . .
C41 C 0.51770(16) 0.13186(8) 0.95980(16) 0.0174 1.0000 Uani . .
C42 C 0.53874(18) 0.15021(9) 1.02605(18) 0.0221 1.0000 Uani . .
C43 C 0.5882(2) 0.17891(10) 1.0212(2) 0.0301 1.0000 Uani . .
C44 C 0.6150(2) 0.18897(10) 0.9491(2) 0.0323 1.0000 Uani . .
C45 C 0.59166(18) 0.17030(9) 0.88402(19) 0.0243 1.0000 Uani . .
C46 C 0.51928(17) 0.04569(8) 0.70560(16) 0.0170 1.0000 Uani . .
C47 C 0.49798(18) 0.02512(9) 0.64244(17) 0.0208 1.0000 Uani . .
C48 C 0.44016(19) 0.03835(8) 0.59610(18) 0.0227 1.0000 Uani . .
C49 C 0.40361(17) 0.06972(8) 0.61642(17) 0.0191 1.0000 Uani . .
C50 C 0.42683(16) 0.08888(8) 0.68085(17) 0.0175 1.0000 Uani . .
C51 C 0.39057(16) 0.12201(8) 0.70941(17) 0.0169 1.0000 Uani . .
C52 C 0.32816(17) 0.13849(9) 0.67662(17) 0.0221 1.0000 Uani . .
C53 C 0.29847(18) 0.16884(9) 0.70824(19) 0.0241 1.0000 Uani . .
C54 C 0.33152(19) 0.18341(9) 0.7734(2) 0.0272 1.0000 Uani . .
C55 C 0.39342(17) 0.16610(9) 0.80550(19) 0.0216 1.0000 Uani . .
C56 C 0.35122(16) 0.10376(8) 0.21753(16) 0.0150 1.0000 Uani . .
C57 C 0.36305(16) 0.07950(8) 0.28246(16) 0.0162 1.0000 Uani . .
C58 C 0.39845(16) 0.13354(9) 0.20159(16) 0.0175 1.0000 Uani . .
C59 C 0.37784(18) 0.15726(8) 0.14139(16) 0.0187 1.0000 Uani . .
C60 C 0.31490(18) 0.15075(8) 0.09674(17) 0.0201 1.0000 Uani . .
C61 C 0.27022(18) 0.12050(8) 0.11029(17) 0.0211 1.0000 Uani . .
C62 C 0.28756(18) 0.09774(8) 0.17074(17) 0.0204 1.0000 Uani . .
C63 C 0.61467(17) 0.05607(8) 0.37431(17) 0.0191 1.0000 Uani . .
C64 C 0.65565(17) 0.03946(8) 0.43378(18) 0.0200 1.0000 Uani . .
C65 C 0.64675(18) 0.05246(9) 0.50783(18) 0.0234 1.0000 Uani . .
C66 C 0.59728(18) 0.08140(9) 0.52006(18) 0.0224 1.0000 Uani . .
C67 C 0.55891(17) 0.09648(8) 0.45915(17) 0.0176 1.0000 Uani . .
C68 C 0.50583(17) 0.12646(8) 0.46495(17) 0.0184 1.0000 Uani . .
C69 C 0.48686(18) 0.14476(8) 0.53286(18) 0.0221 1.0000 Uani . .
C70 C 0.4349(2) 0.17305(10) 0.5302(2) 0.0293 1.0000 Uani . .
C71 C 0.4057(2) 0.18313(10) 0.4602(2) 0.0322 1.0000 Uani . .
C72 C 0.42750(19) 0.16487(9) 0.3935(2) 0.0282 1.0000 Uani . .
C73 C 0.51180(17) 0.04994(9) 0.19586(17) 0.0210 1.0000 Uani . .
C74 C 0.5345(2) 0.03398(10) 0.12692(18) 0.0296 1.0000 Uani . .
C75 C 0.5925(2) 0.04974(11) 0.0854(2) 0.0336 1.0000 Uani . .
C76 C 0.6267(2) 0.08124(11) 0.1145(2) 0.0346 1.0000 Uani . .
C77 C 0.60156(17) 0.09631(10) 0.18275(19) 0.0258 1.0000 Uani . .
C78 C 0.63321(18) 0.12850(11) 0.2183(2) 0.0317 1.0000 Uani . .
C79 C 0.6938(2) 0.14839(12) 0.1883(2) 0.0426 1.0000 Uani . .
C80 C 0.7191(2) 0.17800(12) 0.2260(3) 0.0493 1.0000 Uani . .
C81 C 0.6841(2) 0.18837(12) 0.2939(3) 0.0482 1.0000 Uani . .
C82 C 0.6233(2) 0.16862(10) 0.3225(2) 0.0352 1.0000 Uani . .
C83 C 0.4097(6) 0.250000(7) 0.9145(6) 0.051(2) 0.6660 Uiso S .
C84 C 0.4567(7) 0.250000(7) 0.9776(6) 0.059(3) 0.6660 Uiso S .
C85 C 0.4247(6) 0.250000(7) 1.0496(6) 0.051(2) 0.6660 Uiso S .
C86 C 0.3488(6) 0.250000(7) 1.0565(6) 0.053(2) 0.6660 Uiso S .
C87 C 0.3031(6) 0.2500 0.9924(7) 0.059(3) 0.6660 Uiso S .
C88 C 0.2235(6) 0.2500 0.9993(7) 0.061(3) 0.6660 Uiso S .
C89 C 0.1764(6) 0.250000(7) 0.9368(7) 0.060(3) 0.6660 Uiso S .
C90 C 0.0990(6) 0.250000(7) 0.9440(6) 0.056(3) 0.6660 Uiso S .
C91 C 0.0679(6) 0.250000(7) 1.0159(6) 0.057(3) 0.6660 Uiso S .
C92 C 0.1141(7) 0.250000(7) 1.0790(7) 0.060(3) 0.6660 Uiso S .
C93 C 0.5880(6) 0.250000(7) 0.1988(6) 0.049(3) 0.6000 Uiso S .
H94 H 0.7050 0.0688 0.7967 0.0700 1.0000 Uiso R .
H95 H 0.6146 0.1789 0.6238 0.0700 1.0000 Uiso R .
H96 H 0.7208 0.1678 0.5491 0.0700 1.0000 Uiso R .
H97 H 0.7959 0.1168 0.5728 0.0700 1.0000 Uiso R .
H98 H 0.7695 0.0797 0.6786 0.0700 1.0000 Uiso R .
H99 H 0.4055 0.0481 0.8258 0.0700 1.0000 Uiso R .
H100 H 0.3391 0.0231 0.9288 0.0700 1.0000 Uiso R .
H101 H 0.3575 0.0467 1.0538 0.0700 1.0000 Uiso R .
H102 H 0.4373 0.0968 1.0696 0.0700 1.0000 Uiso R .
H103 H 0.5188 0.1431 1.0747 0.0700 1.0000 Uiso R .
H104 H 0.6042 0.1914 1.0662 0.0700 1.0000 Uiso R .
H105 H 0.6494 0.2086 0.9441 0.0700 1.0000 Uiso R .
H106 H 0.6091 0.1777 0.8346 0.0700 1.0000 Uiso R .
H107 H 0.5586 0.0368 0.7377 0.0700 1.0000 Uiso R .
H108 H 0.5223 0.0028 0.6309 0.0700 1.0000 Uiso R .
H109 H 0.4266 0.0256 0.5505 0.0700 1.0000 Uiso R .
H110 H 0.3623 0.0783 0.5866 0.0700 1.0000 Uiso R .
H111 H 0.3060 0.1281 0.6318 0.0700 1.0000 Uiso R .
H112 H 0.2558 0.1803 0.6857 0.0700 1.0000 Uiso R .
H113 H 0.3125 0.2050 0.7963 0.0700 1.0000 Uiso R .
H114 H 0.4157 0.1754 0.8513 0.0700 1.0000 Uiso R .
H115 H 0.3242 0.0626 0.2939 0.0700 1.0000 Uiso R .
H116 H 0.4074 0.1783 0.1316 0.0700 1.0000 Uiso R .
H117 H 0.3020 0.1670 0.0563 0.0700 1.0000 Uiso R .
H118 H 0.2278 0.1157 0.0785 0.0700 1.0000 Uiso R .
H119 H 0.2568 0.0771 0.1804 0.0700 1.0000 Uiso R .
H120 H 0.6213 0.0473 0.3232 0.0700 1.0000 Uiso R .
H121 H 0.6889 0.0198 0.4235 0.0700 1.0000 Uiso R .
H122 H 0.5906 0.0907 0.5708 0.0700 1.0000 Uiso R .
H123 H 0.5085 0.1376 0.5806 0.0700 1.0000 Uiso R .
H124 H 0.4208 0.1853 0.5763 0.0700 1.0000 Uiso R .
H125 H 0.3705 0.2025 0.4571 0.0700 1.0000 Uiso R .
H126 H 0.4069 0.1718 0.3451 0.0700 1.0000 Uiso R .
H127 H 0.4724 0.0388 0.2246 0.0700 1.0000 Uiso R .
H128 H 0.5109 0.0124 0.1088 0.0700 1.0000 Uiso R .
H129 H 0.6081 0.0396 0.0376 0.0700 1.0000 Uiso R .
H130 H 0.6673 0.0921 0.0873 0.0700 1.0000 Uiso R .
H131 H 0.7176 0.1407 0.1420 0.0700 1.0000 Uiso R .
H132 H 0.7605 0.1916 0.2065 0.0700 1.0000 Uiso R .
H133 H 0.7005 0.2095 0.3204 0.0700 1.0000 Uiso R .
H134 H 0.5996 0.1758 0.3693 0.0700 1.0000 Uiso R .
H135 H 0.2530 0.0168 0.4196 0.0700 1.0000 Uiso R .
H136 H 0.3233 0.0357 0.4042 0.0700 1.0000 Uiso R .
H137 H 0.3653 0.0043 0.2116 0.0700 1.0000 Uiso R .
H138 H 0.3214 0.0026 0.1437 0.0700 1.0000 Uiso R .
H139 H 0.2648 0.2500 0.6236 0.0700 1.0000 Uiso RS .
H140 H 0.2732 0.2500 0.5413 0.0700 1.0000 Uiso RS .
H141 H 0.4855 0.2500 0.1872 0.0700 0.6000 Uiso RS .
H142 H 0.0727 0.2817 0.7750 0.0700 1.0000 Uiso R .
H143 H 0.6719 0.0424 0.5476 0.0700 1.0000 Uiso R .
H144 H 0.0201 0.3151 0.7595 0.0700 1.0000 Uiso R .
H145 H 0.6293 0.2500 0.2398 0.0700 0.6000 Uiso RS .
H146 H 0.5972 0.2722 0.1650 0.0700 0.3000 Uiso R .
H147 H 0.5972 0.2278 0.1650 0.0700 0.3000 Uiso R .
H148 H 0.4338 0.2500 0.8584 0.0700 0.6660 Uiso RS .
H149 H 0.4582 0.2500 1.0967 0.0700 0.6660 Uiso RS .
H150 H 0.3248 0.2500 1.1106 0.0700 0.6660 Uiso RS .
H152 H 0.0664 0.2500 0.8969 0.0700 0.6660 Uiso RS .
H153 H 0.0097 0.2500 1.0221 0.0700 0.6660 Uiso RS .
H154 H 0.0901 0.2500 1.1348 0.0700 0.6660 Uiso RS .
H155 H 0.5127 0.2500 0.9712 0.0700 0.6660 Uiso RS .
H151 H 0.1989 0.2500 0.8839 0.0700 0.6660 Uiso RS .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01101(18) 0.01769(19) 0.01214(17) 0.00024(15) 0.00038(15) 0.00074(15)
Co2 0.01349(19) 0.0193(2) 0.01435(18) 0.00243(16) -0.00139(15) -0.00145(16)
Br3 0.02654(16) 0.02634(16) 0.03235(17) 0.00415(14) 0.00620(15) 0.00035(14)
Br4 0.0446(5) 0.0318(4) 0.0406(4) 0.0000 0.0010(4) 0.0000
Br5 0.0382(5) 0.0287(4) 0.0483(5) 0.0000 -0.0076(4) 0.0000
O8 0.0505(17) 0.0397(15) 0.0235(13) 0.0182(11) 0.0194(12) 0.0206(13)
O9 0.0145(10) 0.0200(10) 0.0177(10) 0.0058(8) 0.0050(8) 0.0028(8)
O10 0.0188(11) 0.0282(12) 0.0172(10) 0.0080(9) -0.0001(9) -0.0030(9)
O11 0.0179(10) 0.0248(11) 0.0189(10) 0.0046(9) -0.0064(9) -0.0025(9)
O12 0.0259(12) 0.0379(14) 0.0265(12) 0.0052(11) 0.0066(10) 0.0014(11)
O13 0.0341(13) 0.0229(12) 0.0296(12) 0.0023(10) 0.0079(10) -0.0034(10)
O14 0.060(3) 0.041(2) 0.042(2) 0.0000 0.029(2) 0.0000
O16 0.0279(13) 0.0254(12) 0.0294(12) -0.0009(10) 0.0001(10) 0.0007(10)
N17 0.0115(12) 0.0249(13) 0.0125(11) 0.0004(10) -0.0034(9) 0.0049(10)
N18 0.0093(11) 0.0222(13) 0.0115(11) 0.0000(10) -0.0017(9) 0.0035(10)
N19 0.0155(12) 0.0191(13) 0.0202(12) -0.0009(10) 0.0014(10) 0.0016(10)
N20 0.0131(11) 0.0187(12) 0.0133(11) 0.0041(9) 0.0022(10) -0.0002(10)
N21 0.0107(12) 0.0269(14) 0.0145(12) 0.0016(10) 0.0024(10) -0.0014(10)
N22 0.0135(12) 0.0204(13) 0.0134(11) 0.0032(10) -0.0014(9) 0.0007(10)
N23 0.0098(11) 0.0218(13) 0.0187(12) 0.0036(10) 0.0012(10) -0.0027(10)
N24 0.0193(14) 0.0229(13) 0.0152(12) 0.0018(10) -0.0031(10) -0.0005(10)
N25 0.0124(12) 0.0292(14) 0.0143(12) 0.0048(10) 0.0016(10) 0.0021(10)
N26 0.0168(13) 0.0333(16) 0.0209(13) 0.0114(12) -0.0097(11) -0.0059(11)
C29 0.0123(14) 0.0220(15) 0.0098(12) -0.0005(11) -0.0003(10) -0.0009(11)
C30 0.0123(13) 0.0201(15) 0.0134(13) -0.0017(11) 0.0001(11) 0.0012(11)
C31 0.0153(14) 0.0233(15) 0.0095(12) -0.0033(11) -0.0014(11) -0.0035(11)
C32 0.0193(15) 0.0193(15) 0.0180(14) -0.0022(12) -0.0019(12) -0.0014(12)
C33 0.0225(15) 0.0206(15) 0.0175(14) 0.0006(12) 0.0037(12) -0.0047(13)
C34 0.0168(15) 0.0290(17) 0.0174(14) -0.0015(13) 0.0029(12) -0.0010(12)
C35 0.0110(13) 0.0235(15) 0.0172(14) -0.0037(12) 0.0005(11) 0.0003(11)
C36 0.0127(14) 0.0270(16) 0.0141(14) 0.0008(12) -0.0012(11) 0.0036(12)
C37 0.0192(15) 0.0178(15) 0.0213(15) 0.0044(12) 0.0010(12) 0.0054(12)
C38 0.0212(16) 0.0271(17) 0.0148(14) 0.0010(12) 0.0047(12) 0.0022(13)
C39 0.0201(15) 0.0254(16) 0.0124(13) -0.0014(12) -0.0007(12) 0.0053(12)
C40 0.0100(13) 0.0241(15) 0.0107(13) -0.0005(11) -0.0033(10) 0.0057(11)
C41 0.0126(14) 0.0254(15) 0.0141(13) -0.0022(12) -0.0005(11) 0.0039(12)
C42 0.0232(16) 0.0245(16) 0.0187(15) -0.0037(13) 0.0014(13) 0.0014(13)
C43 0.0325(19) 0.0317(19) 0.0262(17) -0.0094(15) -0.0026(15) -0.0024(15)
C44 0.034(2) 0.0335(19) 0.0298(18) -0.0065(15) -0.0031(16) -0.0131(16)
C45 0.0204(16) 0.0285(17) 0.0239(16) -0.0024(14) 0.0044(13) -0.0053(13)
C46 0.0155(15) 0.0212(15) 0.0141(13) 0.0029(11) 0.0013(11) 0.0013(12)
C47 0.0210(16) 0.0249(16) 0.0165(14) 0.0008(12) 0.0021(12) -0.0025(12)
C48 0.0321(17) 0.0186(15) 0.0175(14) 0.0013(12) -0.0010(13) -0.0040(13)
C49 0.0191(15) 0.0230(16) 0.0153(13) 0.0039(12) -0.0025(12) -0.0048(12)
C50 0.0146(14) 0.0221(15) 0.0158(14) 0.0051(12) 0.0001(11) -0.0015(12)
C51 0.0116(14) 0.0195(15) 0.0195(14) 0.0029(11) 0.0012(11) -0.0009(11)
C52 0.0151(15) 0.0326(18) 0.0188(15) 0.0077(13) -0.0014(12) -0.0002(13)
C53 0.0159(15) 0.0245(16) 0.0318(17) 0.0115(13) 0.0046(13) 0.0034(12)
C54 0.0210(16) 0.0287(18) 0.0318(18) 0.0058(14) 0.0032(14) 0.0094(13)
C55 0.0147(15) 0.0244(16) 0.0256(15) -0.0009(13) 0.0035(13) 0.0025(12)
C56 0.0143(14) 0.0165(14) 0.0140(13) -0.0038(11) -0.0011(11) 0.0024(11)
C57 0.0125(13) 0.0195(15) 0.0168(14) 0.0002(11) -0.0001(11) -0.0010(11)
C58 0.0115(14) 0.0271(16) 0.0138(13) 0.0010(12) -0.0012(11) 0.0010(12)
C59 0.0223(16) 0.0182(15) 0.0156(14) 0.0003(11) 0.0015(12) -0.0001(12)
C60 0.0246(16) 0.0204(15) 0.0152(14) -0.0007(12) -0.0033(12) 0.0040(13)
C61 0.0244(16) 0.0209(15) 0.0180(14) -0.0019(12) -0.0063(13) 0.0016(12)
C62 0.0242(16) 0.0210(15) 0.0159(14) -0.0020(12) -0.0008(12) 0.0028(13)
C63 0.0192(15) 0.0212(15) 0.0170(14) 0.0016(12) -0.0034(12) -0.0044(12)
C64 0.0179(15) 0.0160(14) 0.0260(16) 0.0040(12) -0.0047(13) -0.0029(12)
C65 0.0203(17) 0.0256(17) 0.0244(16) 0.0074(13) -0.0095(13) -0.0053(13)
C66 0.0235(17) 0.0266(17) 0.0171(15) 0.0029(12) -0.0019(13) -0.0047(13)
C67 0.0152(14) 0.0193(15) 0.0182(14) 0.0005(11) 0.0004(12) -0.0059(12)
C68 0.0182(15) 0.0202(15) 0.0167(14) 0.0017(11) -0.0044(12) -0.0045(12)
C69 0.0220(16) 0.0218(15) 0.0224(15) -0.0001(12) 0.0036(13) -0.0010(13)
C70 0.0336(19) 0.0281(18) 0.0263(17) -0.0072(14) 0.0056(15) 0.0031(15)
C71 0.0330(19) 0.037(2) 0.0267(18) -0.0051(15) 0.0006(15) 0.0121(16)
C72 0.0248(18) 0.0299(18) 0.0299(18) -0.0029(14) -0.0018(14) 0.0060(14)
C73 0.0170(15) 0.0287(16) 0.0173(14) 0.0023(13) 0.0011(12) 0.0034(13)
C74 0.0315(19) 0.042(2) 0.0153(15) 0.0039(14) -0.0014(13) 0.0172(16)
C75 0.035(2) 0.048(2) 0.0181(15) 0.0072(15) 0.0066(15) 0.0183(17)
C76 0.0232(18) 0.055(2) 0.0261(17) 0.0182(17) 0.0112(14) 0.0193(17)
C77 0.0130(15) 0.042(2) 0.0221(16) 0.0152(15) 0.0045(13) 0.0076(14)
C78 0.0147(16) 0.049(2) 0.0319(18) 0.0244(17) -0.0056(14) -0.0045(15)
C79 0.0248(19) 0.059(3) 0.044(2) 0.033(2) 0.0002(17) -0.0103(18)
C80 0.027(2) 0.055(3) 0.066(3) 0.037(2) -0.012(2) -0.0210(19)
C81 0.039(2) 0.045(2) 0.060(3) 0.030(2) -0.027(2) -0.021(2)
C82 0.036(2) 0.0271(19) 0.042(2) 0.0168(16) -0.0222(17) -0.0160(16)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 . Co1 N17 . 94.29(10) yes
O9 . Co1 N18 . 170.33(9) yes
N17 . Co1 N18 . 93.21(10) yes
O9 . Co1 N19 . 91.06(10) yes
N17 . Co1 N19 . 86.38(10) yes
N18 . Co1 N19 . 83.33(10) yes
O9 . Co1 N20 . 91.06(9) yes
N17 . Co1 N20 . 93.10(10) yes
N18 . Co1 N20 . 94.61(10) yes
N19 . Co1 N20 . 177.84(10) yes
O9 . Co1 N21 . 83.72(9) yes
N17 . Co1 N21 . 175.55(10) yes
N18 . Co1 N21 . 89.21(10) yes
N19 . Co1 N21 . 97.62(11) yes
N20 . Co1 N21 . 82.97(10) yes
O11 . Co2 N22 . 95.39(10) yes
O11 . Co2 N23 . 170.32(10) yes
N22 . Co2 N23 . 92.26(10) yes
O11 . Co2 N24 . 91.41(10) yes
N22 . Co2 N24 . 87.42(11) yes
N23 . Co2 N24 . 83.00(10) yes
O11 . Co2 N25 . 88.88(10) yes
N22 . Co2 N25 . 93.53(11) yes
N23 . Co2 N25 . 96.57(10) yes
N24 . Co2 N25 . 178.98(11) yes
O11 . Co2 N26 . 83.09(10) yes
N22 . Co2 N26 . 176.41(11) yes
N23 . Co2 N26 . 89.60(10) yes
N24 . Co2 N26 . 95.86(11) yes
N25 . Co2 N26 . 83.21(12) yes
Co1 . O9 C31 . 125.82(19) yes
Co2 . O11 C58 . 125.61(19) yes
H135 . O12 H136 . 113.8 no
H137 . O13 H138 . 107.1 no
H139 . O14 H140 . 110.6 no
C93 . O15 H141 . 108.1 no
H142 . O16 H144 . 106.7 no
O8 . N17 Co1 . 120.49(18) yes
O8 . N17 C30 . 115.2(2) yes
Co1 . N17 C30 . 123.9(2) yes
Co1 . N18 C36 . 127.3(2) yes
Co1 . N18 C40 . 113.95(19) yes
C36 . N18 C40 . 118.7(2) yes
Co1 . N19 C41 . 114.1(2) yes
Co1 . N19 C45 . 125.3(2) yes
C41 . N19 C45 . 120.0(3) yes
Co1 . N20 C46 . 127.6(2) yes
Co1 . N20 C50 . 114.0(2) yes
C46 . N20 C50 . 118.4(3) yes
Co1 . N21 C51 . 113.5(2) yes
Co1 . N21 C55 . 127.1(2) yes
C51 . N21 C55 . 119.3(3) yes
O10 . N22 Co2 . 116.88(17) yes
O10 . N22 C57 . 119.6(2) yes
Co2 . N22 C57 . 123.5(2) yes
Co2 . N23 C63 . 126.1(2) yes
Co2 . N23 C67 . 114.4(2) yes
C63 . N23 C67 . 119.4(3) yes
Co2 . N24 C68 . 114.1(2) yes
Co2 . N24 C72 . 124.9(2) yes
C68 . N24 C72 . 120.8(3) yes
Co2 . N25 C73 . 126.5(2) yes
Co2 . N25 C77 . 113.9(2) yes
C73 . N25 C77 . 119.4(3) yes
Co2 . N26 C78 . 113.0(2) yes
Co2 . N26 C82 . 127.7(3) yes
C78 . N26 C82 . 119.2(3) yes
C83 . N27 C87 . 118.3(9) yes
C88 . N28 C92 . 120.5(10) yes
C30 . C29 C31 . 123.2(3) yes
C30 . C29 C35 . 117.0(3) yes
C31 . C29 C35 . 119.5(3) yes
C29 . C30 N17 . 124.7(3) yes
C29 . C30 H94 . 118.0 no
N17 . C30 H94 . 117.3 no
C29 . C31 O9 . 122.9(3) yes
C29 . C31 C32 . 118.5(3) yes
O9 . C31 C32 . 118.6(3) yes
C31 . C32 C33 . 121.5(3) yes
C31 . C32 H95 . 119.5 no
C33 . C32 H95 . 119.0 no
C32 . C33 C34 . 120.4(3) yes
C32 . C33 H96 . 120.0 no
C34 . C33 H96 . 119.5 no
C33 . C34 C35 . 119.3(3) yes
C33 . C34 H97 . 120.4 no
C35 . C34 H97 . 120.3 no
C29 . C35 C34 . 120.5(3) yes
C29 . C35 H98 . 120.1 no
C34 . C35 H98 . 119.3 no
N18 . C36 C37 . 122.6(3) yes
N18 . C36 H99 . 118.5 no
C37 . C36 H99 . 118.9 no
C36 . C37 C38 . 118.8(3) yes
C36 . C37 H100 . 120.6 no
C38 . C37 H100 . 120.5 no
C37 . C38 C39 . 118.6(3) yes
C37 . C38 H101 . 120.5 no
C39 . C38 H101 . 120.9 no
C38 . C39 C40 . 120.3(3) yes
C38 . C39 H102 . 119.7 no
C40 . C39 H102 . 119.9 no
C39 . C40 N18 . 120.9(3) yes
C39 . C40 C41 . 125.1(3) yes
N18 . C40 C41 . 114.1(2) yes
C40 . C41 N19 . 114.2(2) yes
C40 . C41 C42 . 125.2(3) yes
N19 . C41 C42 . 120.6(3) yes
C41 . C42 C43 . 119.8(3) yes
C41 . C42 H103 . 120.1 no
C43 . C42 H103 . 120.1 no
C42 . C43 C44 . 118.7(3) yes
C42 . C43 H104 . 120.9 no
C44 . C43 H104 . 120.4 no
C43 . C44 C45 . 119.8(3) yes
C43 . C44 H105 . 120.4 no
C45 . C44 H105 . 119.8 no
C44 . C45 N19 . 121.1(3) yes
C44 . C45 H106 . 119.6 no
N19 . C45 H106 . 119.2 no
N20 . C46 C47 . 123.1(3) yes
N20 . C46 H107 . 118.5 no
C47 . C46 H107 . 118.4 no
C46 . C47 C48 . 117.8(3) yes
C46 . C47 H108 . 121.1 no
C48 . C47 H108 . 121.1 no
C47 . C48 C49 . 119.7(3) yes
C47 . C48 H109 . 119.6 no
C49 . C48 H109 . 120.7 no
C48 . C49 C50 . 119.7(3) yes
C48 . C49 H110 . 120.4 no
C50 . C49 H110 . 119.8 no
C49 . C50 N20 . 121.0(3) yes
C49 . C50 C51 . 124.5(3) yes
N20 . C50 C51 . 114.5(3) yes
C50 . C51 N21 . 114.3(3) yes
C50 . C51 C52 . 125.3(3) yes
N21 . C51 C52 . 120.4(3) yes
C51 . C52 C53 . 120.5(3) yes
C51 . C52 H111 . 119.3 no
C53 . C52 H111 . 120.1 no
C52 . C53 C54 . 119.1(3) yes
C52 . C53 H112 . 120.8 no
C54 . C53 H112 . 120.1 no
C53 . C54 C55 . 119.1(3) yes
C53 . C54 H113 . 121.0 no
C55 . C54 H113 . 119.9 no
C54 . C55 N21 . 121.6(3) yes
C54 . C55 H114 . 119.9 no
N21 . C55 H114 . 118.6 no
C57 . C56 C58 . 123.0(3) yes
C57 . C56 C62 . 117.7(3) yes
C58 . C56 C62 . 119.2(3) yes
C56 . C57 N22 . 125.2(3) yes
C56 . C57 H115 . 117.4 no
N22 . C57 H115 . 117.4 no
C56 . C58 O11 . 123.6(3) yes
C56 . C58 C59 . 118.3(3) yes
O11 . C58 C59 . 118.1(3) yes
C58 . C59 C60 . 121.2(3) yes
C58 . C59 H116 . 119.6 no
C60 . C59 H116 . 119.3 no
C59 . C60 C61 . 120.5(3) yes
C59 . C60 H117 . 120.0 no
C61 . C60 H117 . 119.5 no
C60 . C61 C62 . 119.3(3) yes
C60 . C61 H118 . 120.4 no
C62 . C61 H118 . 120.3 no
C56 . C62 C61 . 121.4(3) yes
C56 . C62 H119 . 119.0 no
C61 . C62 H119 . 119.5 no
N23 . C63 C64 . 122.4(3) yes
N23 . C63 H120 . 119.4 no
C64 . C63 H120 . 118.2 no
C63 . C64 C65 . 118.2(3) yes
C63 . C64 H121 . 121.1 no
C65 . C64 H121 . 120.7 no
C64 . C65 C66 . 118.6(3) yes
C64 . C65 H143 . 120.8 no
C66 . C65 H143 . 120.6 no
C65 . C66 C67 . 120.3(3) yes
C65 . C66 H122 . 119.5 no
C67 . C66 H122 . 120.2 no
C66 . C67 N23 . 121.1(3) yes
C66 . C67 C68 . 125.1(3) yes
N23 . C67 C68 . 113.8(3) yes
C67 . C68 N24 . 114.5(3) yes
C67 . C68 C69 . 125.5(3) yes
N24 . C68 C69 . 119.9(3) yes
C68 . C69 C70 . 119.6(3) yes
C68 . C69 H123 . 120.1 no
C70 . C69 H123 . 120.3 no
C69 . C70 C71 . 118.8(3) yes
C69 . C70 H124 . 120.2 no
C71 . C70 H124 . 121.0 no
C70 . C71 C72 . 119.9(3) yes
C70 . C71 H125 . 120.1 no
C72 . C71 H125 . 119.9 no
C71 . C72 N24 . 120.8(3) yes
C71 . C72 H126 . 119.7 no
N24 . C72 H126 . 119.5 no
N25 . C73 C74 . 122.1(3) yes
N25 . C73 H127 . 119.2 no
C74 . C73 H127 . 118.7 no
C73 . C74 C75 . 119.0(4) yes
C73 . C74 H128 . 120.6 no
C75 . C74 H128 . 120.5 no
C74 . C75 C76 . 118.9(3) yes
C74 . C75 H129 . 120.4 no
C76 . C75 H129 . 120.7 no
C75 . C76 C77 . 120.0(3) yes
C75 . C76 H130 . 119.9 no
C77 . C76 H130 . 120.1 no
C76 . C77 N25 . 120.6(3) yes
C76 . C77 C78 . 124.6(3) yes
N25 . C77 C78 . 114.8(3) yes
C77 . C78 N26 . 114.4(3) yes
C77 . C78 C79 . 124.6(4) yes
N26 . C78 C79 . 120.9(4) yes
C78 . C79 C80 . 120.0(4) yes
C78 . C79 H131 . 120.0 no
C80 . C79 H131 . 120.0 no
C79 . C80 C81 . 119.0(4) yes
C79 . C80 H132 . 120.7 no
C81 . C80 H132 . 120.3 no
C80 . C81 C82 . 120.4(4) yes
C80 . C81 H133 . 120.0 no
C82 . C81 H133 . 119.6 no
C81 . C82 N26 . 120.5(4) yes
C81 . C82 H134 . 120.0 no
N26 . C82 H134 . 119.5 no
N27 . C83 C84 . 123.2(10) yes
N27 . C83 H148 . 117.9 no
C84 . C83 H148 . 118.9 no
C83 . C84 C85 . 118.1(10) yes
C83 . C84 H155 . 121.0 no
C85 . C84 H155 . 120.9 no
C84 . C85 C86 . 119.6(10) yes
C84 . C85 H149 . 119.4 no
C86 . C85 H149 . 121.0 no
C85 . C86 C87 . 121.0(11) yes
C85 . C86 H150 . 119.6 no
C87 . C86 H150 . 119.4 no
C86 . C87 N27 . 119.8(10) yes
C86 . C87 C88 . 121.3(11) yes
N27 . C87 C88 . 118.9(10) yes
C87 . C88 N28 . 120.2(10) yes
C87 . C88 C89 . 122.9(11) yes
N28 . C88 C89 . 116.9(10) yes
C88 . C89 C90 . 122.6(11) yes
C88 . C89 H151 . 118.8 no
C90 . C89 H151 . 118.6 no
C89 . C90 C91 . 119.0(11) yes
C89 . C90 H152 . 120.2 no
C91 . C90 H152 . 120.8 no
C90 . C91 C92 . 119.2(11) yes
C90 . C91 H153 . 119.8 no
C92 . C91 H153 . 120.9 no
C91 . C92 N28 . 121.7(11) yes
C91 . C92 H154 . 119.3 no
N28 . C92 H154 . 119.0 no
H146 5_555 C93 H147 5_555 106.7 no
H146 5_555 C93 O15 . 112.2 no
H147 5_555 C93 O15 . 112.2 no
H146 5_555 C93 H145 . 106.6 no
H147 5_555 C93 H145 . 106.6 no
O15 . C93 H145 . 112.2 no
H146 5_555 C93 H146 . 106.7 no
O15 . C93 H146 . 112.2 no
H145 . C93 H146 . 106.6 no
H147 5_555 C93 H147 . 106.7 no
O15 . C93 H147 . 112.2 no
H145 . C93 H147 . 106.6 no
H146 . C93 H147 . 106.7 no
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
Co1 O9 . 1.886(2) yes
Co1 N17 . 1.907(2) yes
Co1 N18 . 1.935(2) yes
Co1 N19 . 1.934(3) yes
Co1 N20 . 1.940(2) yes
Co1 N21 . 1.972(2) yes
Co2 O11 . 1.869(2) yes
Co2 N22 . 1.911(2) yes
Co2 N23 . 1.938(2) yes
Co2 N24 . 1.924(3) yes
Co2 N25 . 1.928(3) yes
Co2 N26 . 1.971(3) yes
O8 N17 . 1.379(3) yes
O9 C31 . 1.315(3) yes
O10 N22 . 1.319(3) yes
O11 C58 . 1.331(3) yes
O12 H135 . 0.918 no
O12 H136 . 0.816 no
O13 H137 . 0.870 no
O13 H138 . 0.886 no
O14 H139 . 0.888 no
O14 H140 . 0.856 no
O15 C93 . 1.285(12) yes
O15 H141 . 0.965 no
O16 H142 . 0.965 no
O16 H144 . 0.990 no
N17 C30 . 1.299(4) yes
N18 C36 . 1.337(4) yes
N18 C40 . 1.374(3) yes
N19 C41 . 1.366(4) yes
N19 C45 . 1.330(4) yes
N20 C46 . 1.340(4) yes
N20 C50 . 1.366(4) yes
N21 C51 . 1.358(4) yes
N21 C55 . 1.338(4) yes
N22 C57 . 1.312(4) yes
N23 C63 . 1.336(4) yes
N23 C67 . 1.344(4) yes
N24 C68 . 1.352(4) yes
N24 C72 . 1.336(4) yes
N25 C73 . 1.349(4) yes
N25 C77 . 1.369(4) yes
N26 C78 . 1.365(5) yes
N26 C82 . 1.347(4) yes
N27 C83 . 1.335(12) yes
N27 C87 . 1.371(13) yes
N28 C88 . 1.395(14) yes
N28 C92 . 1.349(13) yes
C29 C30 . 1.449(4) yes
C29 C31 . 1.407(4) yes
C29 C35 . 1.419(4) yes
C30 H94 . 0.950 no
C31 C32 . 1.392(4) yes
C32 C33 . 1.387(4) yes
C32 H95 . 0.950 no
C33 C34 . 1.389(4) yes
C33 H96 . 0.950 no
C34 C35 . 1.389(4) yes
C34 H97 . 0.950 no
C35 H98 . 0.950 no
C36 C37 . 1.385(4) yes
C36 H99 . 0.950 no
C37 C38 . 1.391(4) yes
C37 H100 . 0.950 no
C38 C39 . 1.382(4) yes
C38 H101 . 0.950 no
C39 C40 . 1.375(4) yes
C39 H102 . 0.950 no
C40 C41 . 1.449(4) yes
C41 C42 . 1.383(4) yes
C42 C43 . 1.377(5) yes
C42 H103 . 0.950 no
C43 C44 . 1.386(5) yes
C43 H104 . 0.950 no
C44 C45 . 1.384(4) yes
C44 H105 . 0.950 no
C45 H106 . 0.950 no
C46 C47 . 1.383(4) yes
C46 H107 . 0.950 no
C47 C48 . 1.391(4) yes
C47 H108 . 0.950 no
C48 C49 . 1.371(4) yes
C48 H109 . 0.950 no
C49 C50 . 1.383(4) yes
C49 H110 . 0.950 no
C50 C51 . 1.466(4) yes
C51 C52 . 1.385(4) yes
C52 C53 . 1.352(5) yes
C52 H111 . 0.950 no
C53 C54 . 1.380(5) yes
C53 H112 . 0.950 no
C54 C55 . 1.387(4) yes
C54 H113 . 0.950 no
C55 H114 . 0.950 no
C56 C57 . 1.451(4) yes
C56 C58 . 1.408(4) yes
C56 C62 . 1.408(4) yes
C57 H115 . 0.950 no
C58 C59 . 1.409(4) yes
C59 C60 . 1.380(4) yes
C59 H116 . 0.950 no
C60 C61 . 1.387(4) yes
C60 H117 . 0.950 no
C61 C62 . 1.376(4) yes
C61 H118 . 0.950 no
C62 H119 . 0.950 no
C63 C64 . 1.401(4) yes
C63 H120 . 0.950 no
C64 C65 . 1.378(4) yes
C64 H121 . 0.950 no
C65 C66 . 1.397(5) yes
C65 H143 . 0.900 no
C66 C67 . 1.373(4) yes
C66 H122 . 0.950 no
C67 C68 . 1.455(4) yes
C68 C69 . 1.397(4) yes
C69 C70 . 1.393(5) yes
C69 H123 . 0.950 no
C70 C71 . 1.370(5) yes
C70 H124 . 0.950 no
C71 C72 . 1.391(5) yes
C71 H125 . 0.950 no
C72 H126 . 0.950 no
C73 C74 . 1.390(4) yes
C73 H127 . 0.950 no
C74 C75 . 1.383(5) yes
C74 H128 . 0.950 no
C75 C76 . 1.403(6) yes
C75 H129 . 0.950 no
C76 C77 . 1.380(5) yes
C76 H130 . 0.950 no
C77 C78 . 1.449(5) yes
C78 C79 . 1.400(5) yes
C79 C80 . 1.348(6) yes
C79 H131 . 0.950 no
C80 C81 . 1.384(7) yes
C80 H132 . 0.950 no
C81 C82 . 1.393(5) yes
C81 H133 . 0.950 no
C82 H134 . 0.950 no
C83 C84 . 1.374(14) yes
C83 H148 . 1.061 no
C84 C85 . 1.370(14) yes
C84 H155 . 1.000 no
C85 C86 . 1.352(13) yes
C85 H149 . 1.011 no
C86 C87 . 1.376(14) yes
C86 H150 . 1.028 no
C87 C88 . 1.418(15) yes
C88 C89 . 1.366(15) yes
C89 C90 . 1.379(15) yes
C89 H151 . 1.000 no
C90 C91 . 1.362(14) yes
C90 H152 . 1.000 no
C91 C92 . 1.366(14) yes
C91 H153 . 1.039 no
C92 H154 . 1.057 no
C93 H146 5_555 1.017 no
C93 H147 5_555 1.017 no
C93 H145 . 1.020 no
C93 H146 . 1.017 no
C93 H147 . 1.017 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O12 H136 O10 . 144 0.82 2.00 2.704(2) yes
O16 H144 O9 4_456 152 0.99 1.75 2.666(2) yes
|
1500023.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500023.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_1500023
loop_
_publ_author_name
'Rajni Sharma'
'Raj Pal Sharma'
'Ritu Bala'
'Miguel Quir\'os'
'Juan M. Salas'
_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
;
First X-ray structure of a cis-isomer of cobalt(III) aromatic carboxylate:
Synthesis, and characterization of
[cis-Co(en)~2~(C~8~H~7~O~2~)~2~](C~8~H~7~O~2~).2H~2~O, where
C~8~H~7~O~2~ = p-methylbenzoate
;
_journal_name_full 'Inorganic Chemistry Communications'
_journal_page_first 1075
_journal_page_last 1078
_journal_paper_doi 10.1016/j.inoche.2006.07.002
_journal_volume 9
_journal_year 2006
_chemical_formula_moiety 'C20 H30 Co N4 O4 1+, C8 H7 O2 1-, 2 (H2 O)'
_chemical_formula_sum 'C28 H41 Co N4 O8'
_chemical_formula_weight 620.58
_chemical_name_systematic
;
?
;
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 103.487(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 36.332(2)
_cell_length_b 9.1289(5)
_cell_length_c 19.2431(11)
_cell_measurement_reflns_used 5652
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 25.4
_cell_measurement_theta_min 2.3
_cell_volume 6206.4(6)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0305
_diffrn_reflns_av_sigmaI/netI 0.0383
_diffrn_reflns_limit_h_max 47
_diffrn_reflns_limit_h_min -47
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 19078
_diffrn_reflns_theta_full 27.00
_diffrn_reflns_theta_max 28.35
_diffrn_reflns_theta_min 2.18
_diffrn_standards_decay_% -0.2
_diffrn_standards_number 408
_exptl_absorpt_coefficient_mu 0.605
_exptl_absorpt_correction_T_max 0.868
_exptl_absorpt_correction_T_min 0.710
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.328
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 2624
_exptl_crystal_size_max 0.54
_exptl_crystal_size_mid 0.46
_exptl_crystal_size_min 0.24
_refine_diff_density_max 1.088
_refine_diff_density_min -0.602
_refine_diff_density_rms 0.063
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 383
_refine_ls_number_reflns 7089
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0628
_refine_ls_R_factor_gt 0.0497
_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^)+(0.0800P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1321
_refine_ls_wR_factor_ref 0.1412
_reflns_number_gt 5598
_reflns_number_total 7089
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file tolito.cif
_cod_data_source_block tolito
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1500023
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
Co Co 0.415746(8) 0.60525(3) 0.310083(15) 0.03314(11) Uani 1 1 d .
C1A C 0.37116(6) 0.2457(3) 0.17923(12) 0.0382(5) Uani 1 1 d .
C11A C 0.39729(7) 0.3708(3) 0.20615(12) 0.0377(5) Uani 1 1 d .
O11A O 0.39253(5) 0.43091(19) 0.26401(8) 0.0413(4) Uani 1 1 d .
O12A O 0.42111(6) 0.4091(2) 0.17319(10) 0.0506(5) Uani 1 1 d .
C2A C 0.34360(8) 0.2032(3) 0.21355(15) 0.0517(6) Uani 1 1 d .
H2A H 0.3419 0.2497 0.2557 0.062 Uiso 1 1 d R
C3A C 0.31856(9) 0.0926(3) 0.18611(17) 0.0567(7) Uani 1 1 d .
H3A H 0.3000 0.0667 0.2098 0.068 Uiso 1 1 d R
C4A C 0.32055(8) 0.0201(3) 0.12393(14) 0.0497(6) Uani 1 1 d .
C41A C 0.29280(10) -0.0997(4) 0.09346(18) 0.0711(9) Uani 1 1 d .
H41A H 0.2982 -0.1856 0.1229 0.085 Uiso 1 1 d R
H42A H 0.2949 -0.1227 0.0459 0.085 Uiso 1 1 d R
H43A H 0.2676 -0.0667 0.0922 0.085 Uiso 1 1 d R
C5A C 0.34859(8) 0.0607(3) 0.09085(14) 0.0546(7) Uani 1 1 d .
H5A H 0.3508 0.0122 0.0495 0.066 Uiso 1 1 d R
C6A C 0.37359(7) 0.1715(3) 0.11728(13) 0.0489(6) Uani 1 1 d .
H6A H 0.3924 0.1962 0.0938 0.059 Uiso 1 1 d R
C1B C 0.30713(7) 0.7456(3) 0.32554(13) 0.0433(6) Uani 1 1 d .
C11B C 0.33722(7) 0.6851(3) 0.29138(13) 0.0449(6) Uani 1 1 d .
O11B O 0.36952(4) 0.6612(2) 0.33487(9) 0.0448(4) Uani 1 1 d .
O12B O 0.33022(5) 0.6675(3) 0.22616(9) 0.0658(6) Uani 1 1 d .
C2B C 0.27415(7) 0.8022(4) 0.28224(14) 0.0553(7) Uani 1 1 d .
H2B H 0.2703 0.7951 0.2328 0.066 Uiso 1 1 d R
C3B C 0.24726(8) 0.8684(4) 0.31107(16) 0.0599(8) Uani 1 1 d .
H3B H 0.2259 0.9082 0.2807 0.072 Uiso 1 1 d R
C4B C 0.25128(8) 0.8777(3) 0.38384(17) 0.0542(7) Uani 1 1 d .
C41B C 0.22111(9) 0.9493(5) 0.4146(2) 0.0764(10) Uani 1 1 d .
H41B H 0.2090 1.0257 0.3831 0.092 Uiso 1 1 d R
H42B H 0.2324 0.9902 0.4606 0.092 Uiso 1 1 d R
H43B H 0.2027 0.8771 0.4195 0.092 Uiso 1 1 d R
C5B C 0.28390(8) 0.8193(4) 0.42727(15) 0.0604(8) Uani 1 1 d .
H5B H 0.2873 0.8239 0.4766 0.072 Uiso 1 1 d R
C6B C 0.31167(8) 0.7560(3) 0.39876(14) 0.0544(7) Uani 1 1 d .
H6B H 0.3334 0.7190 0.4291 0.065 Uiso 1 1 d R
N1E N 0.46477(5) 0.5445(2) 0.29637(10) 0.0368(4) Uani 1 1 d .
H11E H 0.4629 0.5216 0.2502 0.044 Uiso 1 1 d R
H12E H 0.4816 0.6181 0.3083 0.044 Uiso 1 1 d R
C1E C 0.47755(8) 0.4156(3) 0.34215(14) 0.0484(6) Uani 1 1 d .
H13E H 0.5046 0.4016 0.3485 0.058 Uiso 1 1 d R
H14E H 0.4646 0.3279 0.3207 0.058 Uiso 1 1 d R
C2E C 0.46821(7) 0.4463(3) 0.41274(14) 0.0504(6) Uani 1 1 d .
H23E H 0.4721 0.3590 0.4423 0.060 Uiso 1 1 d R
H24E H 0.4844 0.5235 0.4378 0.060 Uiso 1 1 d R
N2E N 0.42792(5) 0.4917(2) 0.39814(10) 0.0408(4) Uani 1 1 d .
H21E H 0.4239 0.5463 0.4346 0.049 Uiso 1 1 d R
H22E H 0.4129 0.4122 0.3938 0.049 Uiso 1 1 d R
N3E N 0.40520(5) 0.7215(2) 0.22355(10) 0.0409(4) Uani 1 1 d .
H31E H 0.4209 0.6948 0.1958 0.049 Uiso 1 1 d R
H32E H 0.3813 0.7054 0.1989 0.049 Uiso 1 1 d R
C3E C 0.41022(12) 0.8764(4) 0.24023(18) 0.0809(11) Uani 1 1 d D
H33E H 0.3876 0.9179 0.2510 0.097 Uiso 0.50 1 d PR
H34E H 0.4156 0.9283 0.1997 0.097 Uiso 0.50 1 d PR
H33' H 0.3858 0.9247 0.2260 0.097 Uiso 0.50 1 d PR
H34' H 0.4263 0.9166 0.2112 0.097 Uiso 0.50 1 d PR
C4E C 0.44383(16) 0.8858(7) 0.3013(3) 0.0636(12) Uiso 0.50 1 d PD
H43E H 0.4457 0.9850 0.3198 0.076 Uiso 0.50 1 d PR
H44E H 0.4672 0.8617 0.2879 0.076 Uiso 0.50 1 d PR
C4E' C 0.43317(19) 0.9107(6) 0.3119(2) 0.0636(12) Uiso 0.50 1 d PD
H43' H 0.4561 0.9674 0.3149 0.076 Uiso 0.50 1 d PR
H44' H 0.4155 0.9707 0.3303 0.076 Uiso 0.50 1 d PR
N4E N 0.43626(6) 0.7844(2) 0.35900(11) 0.0446(5) Uani 1 1 d D
H41E H 0.4198 0.8230 0.3824 0.054 Uiso 0.50 1 d PR
H42E H 0.4581 0.7650 0.3909 0.054 Uiso 0.50 1 d PR
H41' H 0.4272 0.7950 0.3984 0.054 Uiso 0.50 1 d PR
H42' H 0.4616 0.7756 0.3731 0.054 Uiso 0.50 1 d PR
C1C C 0.57904(6) 0.7624(3) 0.46631(12) 0.0390(5) Uani 1 1 d .
C11C C 0.54040(6) 0.7609(3) 0.41652(12) 0.0382(5) Uani 1 1 d .
O11C O 0.51371(5) 0.8198(2) 0.43889(10) 0.0499(4) Uani 1 1 d .
O12C O 0.53591(5) 0.7018(2) 0.35694(9) 0.0528(5) Uani 1 1 d .
C2C C 0.58852(8) 0.8603(3) 0.52217(14) 0.0504(6) Uani 1 1 d .
H2C H 0.5708 0.9291 0.5289 0.060 Uiso 1 1 d R
C3C C 0.62434(8) 0.8576(4) 0.56845(15) 0.0623(8) Uani 1 1 d .
H3C H 0.6300 0.9245 0.6059 0.075 Uiso 1 1 d R
C4C C 0.65108(8) 0.7588(4) 0.56005(15) 0.0609(8) Uani 1 1 d .
C41C C 0.69044(9) 0.7567(6) 0.61005(19) 0.0970(15) Uani 1 1 d .
H41C H 0.6931 0.8383 0.6423 0.116 Uiso 1 1 d R
H42C H 0.7093 0.7633 0.5825 0.116 Uiso 1 1 d R
H43C H 0.6938 0.6671 0.6369 0.116 Uiso 1 1 d R
C5C C 0.64174(8) 0.6605(4) 0.50447(15) 0.0579(7) Uani 1 1 d .
H5C H 0.6596 0.5920 0.4980 0.070 Uiso 1 1 d R
C6C C 0.60608(7) 0.6613(3) 0.45749(13) 0.0469(6) Uani 1 1 d .
H6C H 0.6004 0.5939 0.4203 0.056 Uiso 1 1 d R
O1W O 0.49307(9) 0.8774(3) 0.56592(16) 0.0853(8) Uani 1 1 d D
H11W H 0.4883(12) 0.9703(15) 0.566(2) 0.102 Uiso 1 1 d D
H12W H 0.5048(11) 0.866(5) 0.5321(17) 0.102 Uiso 1 1 d D
O2W O 0.43696(7) 0.3342(3) 0.02964(13) 0.0744(6) Uani 1 1 d D
H21W H 0.4500(10) 0.254(3) 0.032(2) 0.089 Uiso 1 1 d D
H22W H 0.4332(11) 0.352(4) 0.0713(11) 0.089 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
Co 0.03084(17) 0.03809(19) 0.03016(17) -0.00049(12) 0.00648(11) 0.00096(12)
C1A 0.0396(12) 0.0382(12) 0.0366(12) 0.0022(9) 0.0086(9) -0.0012(10)
C11A 0.0420(12) 0.0382(12) 0.0333(11) 0.0034(9) 0.0099(9) 0.0017(10)
O11A 0.0425(9) 0.0448(9) 0.0384(9) -0.0058(7) 0.0131(7) -0.0089(7)
O12A 0.0592(11) 0.0528(11) 0.0450(10) -0.0068(8) 0.0229(8) -0.0178(9)
C2A 0.0570(16) 0.0513(15) 0.0520(15) -0.0099(13) 0.0234(12) -0.0089(13)
C3A 0.0544(16) 0.0583(18) 0.0626(17) -0.0035(14) 0.0240(13) -0.0163(13)
C4A 0.0519(15) 0.0478(15) 0.0447(13) 0.0021(12) 0.0018(11) -0.0080(12)
C41A 0.073(2) 0.071(2) 0.0615(19) -0.0019(16) 0.0003(15) -0.0294(17)
C5A 0.0649(17) 0.0588(17) 0.0405(13) -0.0116(12) 0.0129(12) -0.0127(14)
C6A 0.0508(14) 0.0560(16) 0.0432(13) -0.0036(12) 0.0179(11) -0.0105(12)
C1B 0.0340(12) 0.0529(15) 0.0425(13) -0.0011(11) 0.0077(9) -0.0025(10)
C11B 0.0332(12) 0.0582(16) 0.0415(13) -0.0037(12) 0.0052(9) -0.0035(11)
O11B 0.0323(8) 0.0631(11) 0.0379(8) -0.0028(8) 0.0060(6) 0.0059(8)
O12B 0.0407(10) 0.1158(19) 0.0384(10) -0.0097(11) 0.0044(7) 0.0024(11)
C2B 0.0338(12) 0.088(2) 0.0430(13) 0.0046(14) 0.0056(10) 0.0002(13)
C3B 0.0363(14) 0.083(2) 0.0573(17) 0.0098(15) 0.0049(11) 0.0084(14)
C4B 0.0411(14) 0.0592(17) 0.0628(17) -0.0027(13) 0.0135(12) 0.0019(12)
C41B 0.0544(18) 0.090(3) 0.085(2) -0.010(2) 0.0170(16) 0.0195(18)
C5B 0.0563(16) 0.078(2) 0.0451(15) -0.0042(14) 0.0078(12) 0.0144(15)
C6B 0.0447(14) 0.0696(19) 0.0450(14) -0.0018(13) 0.0024(11) 0.0129(13)
N1E 0.0336(9) 0.0418(11) 0.0354(10) 0.0007(8) 0.0087(7) 0.0017(8)
C1E 0.0444(14) 0.0475(15) 0.0540(15) 0.0066(12) 0.0130(11) 0.0114(11)
C2E 0.0497(14) 0.0564(16) 0.0430(13) 0.0111(12) 0.0067(11) 0.0119(13)
N2E 0.0422(10) 0.0464(12) 0.0349(10) 0.0034(9) 0.0110(8) 0.0020(9)
N3E 0.0378(10) 0.0467(11) 0.0370(10) 0.0067(9) 0.0067(8) 0.0032(9)
C3E 0.127(3) 0.0468(18) 0.063(2) 0.0087(15) 0.009(2) -0.0029(19)
N4E 0.0416(11) 0.0424(11) 0.0450(11) -0.0067(9) 0.0002(8) 0.0052(9)
C1C 0.0355(12) 0.0473(14) 0.0354(11) 0.0011(10) 0.0107(9) -0.0024(10)
C11C 0.0367(12) 0.0382(12) 0.0405(12) -0.0026(10) 0.0106(9) -0.0023(10)
O11C 0.0386(9) 0.0545(11) 0.0557(10) -0.0124(9) 0.0089(8) 0.0050(8)
O12C 0.0415(9) 0.0722(13) 0.0440(10) -0.0155(9) 0.0085(7) -0.0017(9)
C2C 0.0410(13) 0.0604(16) 0.0485(14) -0.0098(12) 0.0080(10) -0.0021(12)
C3C 0.0490(16) 0.089(2) 0.0458(15) -0.0127(15) 0.0040(12) -0.0127(15)
C4C 0.0401(14) 0.099(3) 0.0417(14) 0.0126(15) 0.0065(11) 0.0006(15)
C41C 0.0438(18) 0.176(5) 0.062(2) 0.009(2) -0.0048(14) 0.003(2)
C5C 0.0437(14) 0.079(2) 0.0520(16) 0.0134(15) 0.0140(12) 0.0157(14)
C6C 0.0472(14) 0.0532(15) 0.0413(13) 0.0044(11) 0.0123(10) 0.0062(12)
O1W 0.120(2) 0.0542(14) 0.096(2) 0.0023(13) 0.0535(17) 0.0103(14)
O2W 0.0795(16) 0.0912(18) 0.0604(13) 0.0146(13) 0.0321(12) 0.0072(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O11A Co O11B 91.13(7)
O11A Co N3E 94.58(8)
O11B Co N3E 93.36(8)
O11A Co N1E 91.08(8)
O11B Co N1E 173.56(7)
N3E Co N1E 92.49(8)
O11A Co N4E 176.22(8)
O11B Co N4E 85.12(8)
N3E Co N4E 86.10(9)
N1E Co N4E 92.61(9)
O11A Co N2E 86.95(8)
O11B Co N2E 87.69(8)
N3E Co N2E 178.12(9)
N1E Co N2E 86.38(8)
N4E Co N2E 92.45(9)
C2A C1A C6A 118.1(2)
C2A C1A C11A 121.4(2)
C6A C1A C11A 120.4(2)
O12A C11A O11A 125.0(2)
O12A C11A C1A 120.0(2)
O11A C11A C1A 114.9(2)
C11A O11A Co 128.27(15)
C1A C2A C3A 120.7(3)
C1A C2A H2A 119.5
C3A C2A H2A 119.7
C2A C3A C4A 121.2(3)
C2A C3A H3A 119.2
C4A C3A H3A 119.5
C5A C4A C3A 117.8(2)
C5A C4A C41A 121.1(3)
C3A C4A C41A 121.1(3)
C4A C41A H41A 109.7
C4A C41A H42A 109.5
H41A C41A H42A 109.5
C4A C41A H43A 109.2
H41A C41A H43A 109.5
H42A C41A H43A 109.5
C4A C5A C6A 121.7(3)
C4A C5A H5A 119.3
C6A C5A H5A 119.0
C5A C6A C1A 120.4(2)
C5A C6A H6A 119.7
C1A C6A H6A 119.9
C6B C1B C2B 117.8(2)
C6B C1B C11B 122.9(2)
C2B C1B C11B 119.1(2)
O12B C11B O11B 125.4(2)
O12B C11B C1B 119.6(2)
O11B C11B C1B 114.9(2)
C11B O11B Co 126.85(16)
C3B C2B C1B 121.1(3)
C3B C2B H2B 119.5
C1B C2B H2B 119.4
C2B C3B C4B 121.5(3)
C2B C3B H3B 119.2
C4B C3B H3B 119.3
C3B C4B C5B 117.5(3)
C3B C4B C41B 120.7(3)
C5B C4B C41B 121.8(3)
C4B C41B H41B 109.5
C4B C41B H42B 109.8
H41B C41B H42B 109.5
C4B C41B H43B 109.2
H41B C41B H43B 109.5
H42B C41B H43B 109.4
C6B C5B C4B 121.4(3)
C6B C5B H5B 119.3
C4B C5B H5B 119.3
C5B C6B C1B 120.5(2)
C5B C6B H6B 119.7
C1B C6B H6B 119.8
C1E N1E Co 108.47(15)
C1E N1E H11E 110.1
Co N1E H11E 110.0
C1E N1E H12E 110.0
Co N1E H12E 109.9
H11E N1E H12E 108.4
N1E C1E C2E 106.5(2)
N1E C1E H13E 110.3
C2E C1E H13E 110.3
N1E C1E H14E 110.5
C2E C1E H14E 110.5
H13E C1E H14E 108.6
N2E C2E C1E 107.6(2)
N2E C2E H23E 110.1
C1E C2E H23E 110.2
N2E C2E H24E 110.3
C1E C2E H24E 110.3
H23E C2E H24E 108.5
C2E N2E Co 109.11(15)
C2E N2E H21E 109.8
Co N2E H21E 109.8
C2E N2E H22E 109.9
Co N2E H22E 109.9
H21E N2E H22E 108.3
C3E N3E Co 110.76(17)
C3E N3E H31E 109.3
Co N3E H31E 109.6
C3E N3E H32E 109.4
Co N3E H32E 109.6
H31E N3E H32E 108.1
N3E C3E C4E' 115.4(3)
N3E C3E C4E 105.6(3)
N3E C3E H33E 111.0
C4E C3E H33E 112.9
N3E C3E H34E 109.6
C4E C3E H34E 109.0
H33E C3E H34E 108.6
N3E C3E H33' 108.7
C4E' C3E H33' 116.6
N3E C3E H34' 107.6
C4E' C3E H34' 100.0
H33' C3E H34' 107.5
C3E C4E N4E 106.7(3)
C3E C4E H43E 108.6
N4E C4E H43E 108.1
C3E C4E H44E 112.7
N4E C4E H44E 112.1
H43E C4E H44E 108.5
N4E C4E' C3E 111.1(4)
N4E C4E' H43' 116.5
C3E C4E' H43' 117.4
N4E C4E' H44' 100.5
C3E C4E' H44' 100.6
H43' C4E' H44' 107.9
C4E' N4E Co 113.6(2)
C4E N4E Co 105.8(3)
C4E N4E H41E 112.5
Co N4E H41E 110.3
C4E N4E H42E 109.7
Co N4E H42E 110.0
H41E N4E H42E 108.5
C4E' N4E H41' 116.7
Co N4E H41' 108.9
C4E' N4E H42' 100.6
Co N4E H42' 108.7
H41' N4E H42' 107.7
C2C C1C C6C 118.2(2)
C2C C1C C11C 121.9(2)
C6C C1C C11C 119.9(2)
O12C C11C O11C 123.4(2)
O12C C11C C1C 119.6(2)
O11C C11C C1C 117.0(2)
C1C C2C C3C 120.8(3)
C1C C2C H2C 119.4
C3C C2C H2C 119.8
C4C C3C C2C 121.4(3)
C4C C3C H3C 119.5
C2C C3C H3C 119.1
C3C C4C C5C 118.0(3)
C3C C4C C41C 121.5(3)
C5C C4C C41C 120.4(3)
C4C C41C H41C 109.6
C4C C41C H42C 109.5
H41C C41C H42C 109.5
C4C C41C H43C 109.4
H41C C41C H43C 109.5
H42C C41C H43C 109.5
C4C C5C C6C 121.5(3)
C4C C5C H5C 119.3
C6C C5C H5C 119.2
C1C C6C C5C 120.1(3)
C1C C6C H6C 119.9
C5C C6C H6C 120.0
H11W O1W H12W 105(4)
H21W O2W H22W 108(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co O11A 1.9187(17)
Co O11B 1.9189(16)
Co N3E 1.9363(19)
Co N1E 1.9414(18)
Co N4E 1.946(2)
Co N2E 1.9472(19)
C1A C2A 1.378(3)
C1A C6A 1.392(3)
C1A C11A 1.498(3)
C11A O12A 1.237(3)
C11A O11A 1.288(3)
C2A C3A 1.379(4)
C2A H2A 0.9300
C3A C4A 1.384(4)
C3A H3A 0.9300
C4A C5A 1.372(4)
C4A C41A 1.510(4)
C41A H41A 0.9600
C41A H42A 0.9601
C41A H43A 0.9600
C5A C6A 1.375(4)
C5A H5A 0.9300
C6A H6A 0.9301
C1B C6B 1.383(4)
C1B C2B 1.390(4)
C1B C11B 1.506(3)
C11B O12B 1.231(3)
C11B O11B 1.291(3)
C2B C3B 1.371(4)
C2B H2B 0.9300
C3B C4B 1.376(4)
C3B H3B 0.9300
C4B C5B 1.388(4)
C4B C41B 1.511(4)
C41B H41B 0.9601
C41B H42B 0.9601
C41B H43B 0.9601
C5B C6B 1.382(4)
C5B H5B 0.9300
C6B H6B 0.9300
N1E C1E 1.479(3)
N1E H11E 0.9000
N1E H12E 0.9000
C1E C2E 1.501(4)
C1E H13E 0.9699
C1E H14E 0.9700
C2E N2E 1.484(3)
C2E H23E 0.9700
C2E H24E 0.9700
N2E H21E 0.9000
N2E H22E 0.9000
N3E C3E 1.452(4)
N3E H31E 0.9000
N3E H32E 0.9000
C3E C4E' 1.470(4)
C3E C4E 1.486(4)
C3E H33E 0.9700
C3E H34E 0.9700
C3E H33' 0.9700
C3E H34' 0.9700
C4E N4E 1.519(4)
C4E H43E 0.9700
C4E H44E 0.9700
C4E' N4E 1.455(4)
C4E' H43' 0.9700
C4E' H44' 0.9700
N4E H41E 0.9000
N4E H42E 0.9000
N4E H41' 0.9000
N4E H42' 0.9000
C1C C2C 1.379(4)
C1C C6C 1.387(4)
C1C C11C 1.504(3)
C11C O12C 1.243(3)
C11C O11C 1.269(3)
C2C C3C 1.395(4)
C2C H2C 0.9300
C3C C4C 1.363(5)
C3C H3C 0.9300
C4C C5C 1.377(5)
C4C C41C 1.526(4)
C41C H41C 0.9601
C41C H42C 0.9601
C41C H43C 0.9601
C5C C6C 1.396(4)
C5C H5C 0.9300
C6C H6C 0.9300
O1W H11W 0.866(10)
O1W H12W 0.863(10)
O2W H21W 0.870(10)
O2W H22W 0.859(10)
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
N1E H11E O12A 0.90 2.12 2.812(3) 132.7 .
N1E H12E O12C 0.90 2.12 2.948(3) 152.5 .
N2E H21E O2W 0.90 2.09 2.941(3) 158.1 6_566
N3E H32E O12B 0.90 2.07 2.780(3) 135.0 .
N3E H31E O12C 0.90 2.06 2.925(3) 160.7 2_655
N4E H42' O11C 0.90 2.06 2.893(3) 153.9 .
O1W H12W O11C 0.863(10) 1.942(18) 2.769(3) 160(4) .
O1W H11W O11C 0.866(10) 1.919(13) 2.775(3) 170(4) 5_676
O2W H22W O12A 0.859(10) 2.171(11) 3.028(3) 176(4) .
O2W H21W O1W 0.870(10) 1.956(19) 2.777(4) 157(4) 6_565
|
1500024.cif | #------------------------------------------------------------------------------
#$Date: 2023-11-30 20:01:47 +0200 (Thu, 30 Nov 2023) $
#$Revision: 287905 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500024.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_1500024
loop_
_publ_author_name
'Armel Le Bail'
_publ_contact_author_address
;
Laboratoire des Oxydes et Fluorures, CNRS UMR 6010, Universit\'e du Maine,
72085 Le Mans, France
;
_publ_contact_author_email armel.le_bail@univ-lemans.fr
_publ_contact_author_fax '33 (0)2 43 83 35 06'
_publ_contact_author_name 'Armel Le Bail'
_publ_contact_author_phone '33 (0)2 43 83 33 47'
_publ_section_title
;
<i>Ab initio</i> structure determination of bethanechol chloride
;
_journal_name_full 'Powder Diffraction'
_journal_volume 25
_journal_year 2010
_chemical_compound_source www.serateclab.com
_chemical_formula_moiety 'C7 H17 N2 O2, Cl'
_chemical_formula_sum 'C7 H17 Cl N2 O2'
_chemical_formula_weight 196.68
_chemical_name_common 'bethanechol chloride'
_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'
_audit_update_record
;
2010-01-20 # Formatted by publCIF
;
_cell_angle_alpha 90.00000
_cell_angle_beta 93.8031(10)
_cell_angle_gamma 90.00000
_cell_formula_units_Z 4
_cell_length_a 8.8749(3)
_cell_length_b 16.4118(7)
_cell_length_c 7.1373(3)
_cell_measurement_temperature 293
_cell_volume 1037.28(7)
_computing_molecular_graphics DIAMOND
_computing_publication_material PUBLCIF
_computing_structure_refinement FULLPROF
_computing_structure_solution ESPOIR
_diffrn_ambient_temperature 293
_diffrn_detector 'linear detector'
_diffrn_detector_type X-celerator
_diffrn_measurement_device_type 'MPD-PRO Panalytical'
_diffrn_measurement_method Bragg-Brentano
_diffrn_radiation_monochromator none
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54056
_diffrn_source 'X-ray tube'
_exptl_absorpt_coefficient_mu 3.021
_exptl_crystal_density_diffrn 1.259
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 424
_pd_char_colour white
_pd_meas_2theta_range_inc 0.017000
_pd_meas_2theta_range_max 70.00000
_pd_meas_2theta_range_min 5.00000
_pd_meas_number_of_points 3825
_pd_proc_2theta_range_inc 0.017000
_pd_proc_2theta_range_max 69.8658
_pd_proc_2theta_range_min 4.8658
_pd_proc_ls_background_function 'interpolation between points'
_pd_proc_ls_pref_orient_corr none
_pd_proc_ls_profile_function pseudo-Voigt
_pd_proc_ls_prof_R_factor 2.4331
_pd_proc_ls_prof_wR_expected 1.8510
_pd_proc_ls_prof_wR_factor 3.1938
_pd_proc_wavelength 1.540560
_pd_spec_mount_mode reflection
_pd_spec_shape flat_sheet
_refine_ls_number_parameters 116
_refine_ls_number_reflns 1142
_refine_ls_number_restraints 31
_refine_ls_R_I_factor 3.5799
_cod_data_source_file bethanechol.cif
_cod_data_source_block bethanechol
_cod_depositor_comments
;
Changing the _atom_type_symbol and _atom_site_type_symbol data
item values to match each other.
Antanas Vaitkus,
2017-01-11
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1500024
_pd_proc_ls_prof_cr_factor 7.4877
_pd_proc_ls_prof_cwr_factor 7.0735
_pd_proc_ls_prof_cwr_expected 4.0994
_pd_proc_ls_prof_chi2 2.9773
_pd_proc_ls_prof_echi2 2.9773
_computing_data_indexing McMaille
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Cl 0.7108(3) 0.50368(16) 0.2406(3) 0.0866(13) 1.00000 Uiso Cl
C1 0.1624(13) 0.0998(4) 0.1895(11) 0.099(2) 1.00000 Uiso C
H1 0.104(5) 0.0886(13) 0.304(3) 0.099(2) 1.00000 Uiso H
H2 0.137(5) 0.0646(11) 0.084(2) 0.099(2) 1.00000 Uiso H
H3 0.147(5) 0.1601(6) 0.149(3) 0.099(2) 1.00000 Uiso H
C2 0.3793(8) 0.0152(7) 0.2538(10) 0.099(2) 1.00000 Uiso C
H4 0.4984(14) 0.015(2) 0.263(3) 0.099(2) 1.00000 Uiso H
H5 0.350(3) -0.024(2) 0.151(3) 0.099(2) 1.00000 Uiso H
H6 0.342(3) -0.005(2) 0.3787(19) 0.099(2) 1.00000 Uiso H
C3 0.3982(9) 0.1390(5) 0.0771(14) 0.099(2) 1.00000 Uiso C
H7 0.374(3) 0.0997(13) -0.030(5) 0.099(2) 1.00000 Uiso H
H8 0.372(3) 0.1946(8) 0.046(5) 0.099(2) 1.00000 Uiso H
H9 0.5236(16) 0.1355(14) 0.097(6) 0.099(2) 1.00000 Uiso H
C4 0.3615(10) 0.1507(9) 0.4209(20) 0.099(2) 1.00000 Uiso C
H10 0.322(3) 0.116(3) 0.523(7) 0.099(2) 1.00000 Uiso H
H11 0.475(2) 0.141(4) 0.415(8) 0.099(2) 1.00000 Uiso H
C5 0.3103(13) 0.2393(9) 0.4393(15) 0.099(2) 1.00000 Uiso C
H12 0.207(4) 0.255(5) 0.362(8) 0.099(2) 1.00000 Uiso H
C6 0.3185(8) 0.2549(5) 0.6500(15) 0.099(2) 1.00000 Uiso C
H13 0.294(3) 0.3148(9) 0.652(6) 0.099(2) 1.00000 Uiso H
H14 0.4301(16) 0.2453(15) 0.660(6) 0.099(2) 1.00000 Uiso H
H15 0.263(3) 0.2237(13) 0.741(5) 0.099(2) 1.00000 Uiso H
C7 0.3330(13) 0.3298(9) 0.1951(17) 0.099(2) 1.00000 Uiso C
N1 0.3358(9) 0.1040(5) 0.2419(11) 0.076(3) 1.00000 Uiso N
N2 0.4209(7) 0.3823(5) 0.1100(17) 0.076(3) 1.00000 Uiso N
H16 0.537(2) 0.374(2) 0.140(10) 0.076(3) 1.00000 Uiso H
H17 0.399(3) 0.4352(18) 0.058(8) 0.076(3) 1.00000 Uiso H
O1 0.3981(8) 0.2892(4) 0.3308(12) 0.101(3) 1.00000 Uiso O
O2 0.2033(7) 0.3187(4) 0.1301(10) 0.101(3) 1.00000 Uiso O
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl 11.46040 0.01040 7.19640 1.16620 6.25560 18.51940 1.64550 47.77840 -9.55740
0.34800 0.70200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 104.3(11) . . y
C1 N1 C4 108.6(12) . . y
C1 N1 C2 102.4(11) . . y
C3 N1 C4 116.4(14) . . y
C3 N1 C2 108.5(11) . . y
C4 N1 C2 115.0(14) . . y
C5 C4 N1 122.1(14) . . y
C4 C5 O1 109.2(14) . . y
C4 C5 C6 104.4(14) . . y
C6 C5 O1 117.2(12) . . y
C5 O1 C7 118.9(16) . . y
N2 C7 O1 115.6(14) . . y
N2 C7 O2 119.1(12) . . y
O1 C7 O2 125.0(12) . . y
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
Cl N2 3.337(8) . y
Cl N2 3.277(11) 3_665 y
Cl H7 2.71(3) 4_555 y
Cl H10 2.73(5) 4_554 y
Cl H4 2.589(13) 2_655 y
Cl H16 2.70(3) . y
Cl H17 2.49(5) 3_665 y
C1 N1 1.561(14) . y
C1 H1 1.01(3) . y
C1 H2 0.964(19) . y
C1 H3 1.037(14) . y
C5 C4 1.53(2) . y
C5 C6 1.522(15) . y
C5 O1 1.399(15) . y
C5 H12 1.07(5) . y
C3 N1 1.451(13) . y
C3 H9 1.114(16) . y
C3 H8 0.964(18) . y
C3 H7 1.01(3) . y
C4 C5 1.53(2) . y
C4 N1 1.494(16) . y
C4 H10 1.01(5) . y
C4 H11 1.02(2) . y
C2 N1 1.509(14) . y
C2 H4 1.055(14) . y
C2 H5 1.00(3) . y
C2 H6 1.03(2) . y
C6 C5 1.522(15) . y
C6 H13 1.007(18) . y
C6 H14 1.001(16) . y
C6 H15 0.98(3) . y
C7 N2 1.335(16) . y
C7 O1 1.281(15) . y
C7 O2 1.226(13) . y
N2 H16 1.05(2) . y
N2 H17 0.96(4) . y
O1 H12 1.81(4) . y
O2 H12 1.96(7) . y
H1 H2 1.66(3) . y
H1 H3 1.67(3) . y
H2 H3 1.64(2) . y
H9 H8 1.68(3) . y
H9 H7 1.66(4) . y
H8 H7 1.65(3) . y
H10 H11 1.66(5) . y
H4 H5 1.63(3) . y
H4 H6 1.69(3) . y
H5 H6 1.66(3) . y
H13 H14 1.66(3) . y
H13 H15 1.65(3) . y
H14 H15 1.67(4) . y
H16 H17 1.66(4) . y
|
1500026.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500026.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_1500026
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
'Antonio Rodr\'iguez-Di\'eguez'
_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
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 1553
_journal_page_last 1558
_journal_paper_doi 10.1016/j.ica.2008.07.029
_journal_volume 362
_journal_year 2009
_chemical_formula_moiety 'Cd H12 O6 2+, 2 (C5 H4 N5 O2 1-)'
_chemical_formula_sum 'C10 H20 Cd N10 O10'
_chemical_formula_weight 552.76
_chemical_name_systematic
;
Hexaacua cadmium(II) 4,5,6,7-tetrahydro-4-methyl-5,7-dioxo-
-1,2,3-triazolo-[4,5-d]-pyrimidinate
;
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 86.413(2)
_cell_angle_beta 67.813(2)
_cell_angle_gamma 87.315(2)
_cell_formula_units_Z 1
_cell_length_a 6.8110(8)
_cell_length_b 8.7316(10)
_cell_length_c 8.9234(10)
_cell_measurement_reflns_used 3487
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.6
_cell_measurement_theta_min 2.5
_cell_volume 490.27(10)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0236
_diffrn_reflns_av_sigmaI/netI 0.0257
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 5761
_diffrn_reflns_theta_full 26.70
_diffrn_reflns_theta_max 28.40
_diffrn_reflns_theta_min 2.34
_diffrn_standards_decay_% 0.1
_diffrn_standards_number 135
_exptl_absorpt_coefficient_mu 1.189
_exptl_absorpt_correction_T_max 0.954
_exptl_absorpt_correction_T_min 0.807
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.872
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 278
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.443
_refine_diff_density_min -0.304
_refine_diff_density_rms 0.070
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 161
_refine_ls_number_reflns 2223
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0250
_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^)+(0.0400P)^2^+0.0800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0638
_refine_ls_wR_factor_ref 0.0640
_reflns_number_gt 2177
_reflns_number_total 2223
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cd4max.cif
_cod_data_source_block cd4max
_cod_database_code 1500026
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
Cd Cd 0.5000 0.5000 0.5000 0.03147(9) Uani 1 2 d S . .
O1W O 0.5169(3) 0.49348(19) 0.2430(2) 0.0390(4) Uani 1 1 d D . .
H11W H 0.419(3) 0.533(3) 0.223(4) 0.047 Uiso 1 1 d D . .
H12W H 0.546(5) 0.4125(19) 0.199(3) 0.047 Uiso 1 1 d D . .
O2W O 0.1457(3) 0.5407(2) 0.5922(2) 0.0473(4) Uani 1 1 d D . .
H21W H 0.104(5) 0.6293(16) 0.605(4) 0.057 Uiso 1 1 d D . .
H22W H 0.057(4) 0.475(3) 0.624(4) 0.057 Uiso 1 1 d D . .
O3W O 0.4458(4) 0.2441(2) 0.5400(2) 0.0576(6) Uani 1 1 d D . .
H31W H 0.408(5) 0.191(3) 0.623(2) 0.069 Uiso 1 1 d D . .
H32W H 0.478(5) 0.179(3) 0.473(3) 0.069 Uiso 1 1 d D . .
N1 N 0.6416(3) 0.2053(2) 0.1255(2) 0.0321(4) Uani 1 1 d . . .
N2 N 0.5961(3) 0.0954(2) 0.2412(2) 0.0358(4) Uani 1 1 d . . .
N3 N 0.6582(3) -0.0454(2) 0.1794(2) 0.0317(4) Uani 1 1 d . . .
C3A C 0.7441(3) -0.0190(2) 0.0194(2) 0.0250(4) Uani 1 1 d . . .
N4 N 0.8296(3) -0.12565(19) -0.09825(19) 0.0268(3) Uani 1 1 d . . .
C4 C 0.8318(4) -0.2901(2) -0.0542(3) 0.0364(5) Uani 1 1 d . . .
H41 H 0.7500 -0.3433 -0.1006 0.044 Uiso 1 1 d R . .
H42 H 0.7718 -0.3053 0.0617 0.044 Uiso 1 1 d R . .
H43 H 0.9754 -0.3293 -0.0944 0.044 Uiso 1 1 d R . .
C5 C 0.9034(3) -0.0748(2) -0.2565(2) 0.0281(4) Uani 1 1 d . . .
O5 O 0.9745(3) -0.16261(18) -0.36857(18) 0.0386(4) Uani 1 1 d . . .
N6 N 0.8983(3) 0.0817(2) -0.2887(2) 0.0299(4) Uani 1 1 d . . .
H6 H 0.9505 0.1116 -0.3893 0.036 Uiso 1 1 d R . .
C7 C 0.8199(3) 0.1968(2) -0.1800(2) 0.0278(4) Uani 1 1 d . . .
O7 O 0.8286(3) 0.33242(17) -0.22786(19) 0.0395(4) Uani 1 1 d . . .
C7A C 0.7360(3) 0.1360(2) -0.0169(2) 0.0262(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
Cd 0.03890(14) 0.02466(13) 0.02553(13) -0.00238(8) -0.00607(9) 0.00079(8)
O1W 0.0528(10) 0.0319(8) 0.0324(8) -0.0046(7) -0.0166(7) 0.0076(7)
O2W 0.0391(9) 0.0303(9) 0.0606(11) 0.0027(8) -0.0063(8) 0.0014(7)
O3W 0.1114(17) 0.0241(8) 0.0229(8) -0.0011(6) -0.0085(10) -0.0057(9)
N1 0.0396(10) 0.0308(9) 0.0223(8) -0.0040(7) -0.0077(7) 0.0030(7)
N2 0.0477(11) 0.0330(10) 0.0214(8) -0.0035(7) -0.0069(8) 0.0018(8)
N3 0.0425(10) 0.0291(9) 0.0194(8) -0.0015(7) -0.0070(7) 0.0000(7)
C3A 0.0286(9) 0.0255(9) 0.0198(9) -0.0013(7) -0.0076(7) -0.0018(7)
N4 0.0368(9) 0.0206(8) 0.0193(8) -0.0011(6) -0.0064(7) -0.0001(7)
C4 0.0527(14) 0.0224(10) 0.0299(11) 0.0010(8) -0.0113(10) -0.0012(9)
C5 0.0354(11) 0.0265(10) 0.0207(9) -0.0021(7) -0.0089(8) 0.0022(8)
O5 0.0572(10) 0.0304(8) 0.0216(7) -0.0045(6) -0.0078(7) 0.0068(7)
N6 0.0404(10) 0.0261(9) 0.0177(8) 0.0029(6) -0.0058(7) 0.0024(7)
C7 0.0303(10) 0.0267(10) 0.0250(9) -0.0005(8) -0.0091(8) 0.0022(8)
O7 0.0520(10) 0.0237(8) 0.0347(8) 0.0056(6) -0.0087(7) 0.0031(7)
C7A 0.0313(10) 0.0251(10) 0.0210(9) -0.0016(7) -0.0083(8) 0.0003(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O2W Cd O2W 180.0 . 2_666 ?
O2W Cd O1W 91.18(7) . . ?
O2W Cd O1W 88.82(7) 2_666 . ?
O2W Cd O1W 88.82(7) . 2_666 ?
O2W Cd O1W 91.18(7) 2_666 2_666 ?
O1W Cd O1W 180.0 . 2_666 ?
O2W Cd O3W 91.02(8) . 2_666 ?
O2W Cd O3W 88.98(8) 2_666 2_666 ?
O1W Cd O3W 88.99(6) . 2_666 ?
O1W Cd O3W 91.01(6) 2_666 2_666 ?
O2W Cd O3W 88.98(8) . . ?
O2W Cd O3W 91.02(8) 2_666 . ?
O1W Cd O3W 91.01(6) . . ?
O1W Cd O3W 88.99(6) 2_666 . ?
O3W Cd O3W 180.0 2_666 . ?
Cd O1W H11W 117(2) . . ?
Cd O1W H12W 119(2) . . ?
H11W O1W H12W 107(3) . . ?
Cd O2W H21W 116(2) . . ?
Cd O2W H22W 126(2) . . ?
H21W O2W H22W 118(3) . . ?
Cd O3W H31W 130(2) . . ?
Cd O3W H32W 128(3) . . ?
H31W O3W H32W 101(3) . . ?
N2 N1 C7A 106.67(17) . . ?
N1 N2 N3 111.58(16) . . ?
C3A N3 N2 105.17(16) . . ?
N3 C3A C7A 109.51(17) . . ?
N3 C3A N4 127.71(18) . . ?
C7A C3A N4 122.79(17) . . ?
C5 N4 C3A 118.39(16) . . ?
C5 N4 C4 120.58(16) . . ?
C3A N4 C4 120.97(16) . . ?
N4 C4 H41 109.7 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.4 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 122.44(19) . . ?
O5 C5 N6 120.26(18) . . ?
N4 C5 N6 117.29(17) . . ?
C5 N6 C7 128.44(17) . . ?
C5 N6 H6 115.8 . . ?
C7 N6 H6 115.8 . . ?
O7 C7 N6 120.72(18) . . ?
O7 C7 C7A 127.68(19) . . ?
N6 C7 C7A 111.61(17) . . ?
N1 C7A C3A 107.08(17) . . ?
N1 C7A C7 131.54(19) . . ?
C3A C7A C7 121.38(17) . . ?
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
Cd O2W 2.2545(18) . ?
Cd O2W 2.2546(18) 2_666 ?
Cd O1W 2.2566(16) . ?
Cd O1W 2.2566(16) 2_666 ?
Cd O3W 2.2658(18) 2_666 ?
Cd O3W 2.2658(18) . ?
O1W H11W 0.812(10) . ?
O1W H12W 0.811(10) . ?
O2W H21W 0.811(10) . ?
O2W H22W 0.811(10) . ?
O3W H31W 0.811(10) . ?
O3W H32W 0.811(10) . ?
N1 N2 1.321(2) . ?
N1 C7A 1.355(2) . ?
N2 N3 1.362(2) . ?
N3 C3A 1.331(2) . ?
C3A C7A 1.376(3) . ?
C3A N4 1.385(2) . ?
N4 C5 1.361(2) . ?
N4 C4 1.466(3) . ?
C4 H41 0.9601 . ?
C4 H42 0.9601 . ?
C4 H43 0.9601 . ?
C5 O5 1.232(2) . ?
C5 N6 1.380(3) . ?
N6 C7 1.384(3) . ?
N6 H6 0.8600 . ?
C7 O7 1.230(3) . ?
C7 C7A 1.424(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H12W N1 0.811(10) 1.960(12) 2.758(2) 168(3) .
O1W H11W O7 0.812(10) 1.995(13) 2.783(2) 163(3) 2_665
O2W H21W O5 0.811(10) 1.971(11) 2.778(2) 173(3) 1_466
O2W H22W O7 0.811(10) 2.035(14) 2.817(2) 162(3) 1_456
O3W H32W N2 0.811(10) 2.084(17) 2.845(2) 156(3) .
O3W H31W N3 0.811(10) 2.024(11) 2.831(3) 174(3) 2_656
N6 H6 O5 0.86 2.05 2.896(2) 168.9 2_754
|
1500027.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500027.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_1500027
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
'Antonio Rodr\'iguez-Di\'eguez'
_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
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 1553
_journal_page_last 1558
_journal_paper_doi 10.1016/j.ica.2008.07.029
_journal_volume 362
_journal_year 2009
_chemical_formula_sum 'C12 H24 Cd N10 O10'
_chemical_formula_weight 580.81
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 75.722(1)
_cell_angle_beta 80.977(1)
_cell_angle_gamma 65.012(1)
_cell_formula_units_Z 1
_cell_length_a 7.7334(5)
_cell_length_b 7.8437(5)
_cell_length_c 9.9055(6)
_cell_measurement_reflns_used 5091
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.3
_cell_measurement_theta_min 2.9
_cell_volume 526.84(6)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0311
_diffrn_reflns_av_sigmaI/netI 0.0306
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 6126
_diffrn_reflns_theta_full 26.70
_diffrn_reflns_theta_max 28.26
_diffrn_reflns_theta_min 2.13
_diffrn_standards_decay_% 0.1
_diffrn_standards_number 202
_exptl_absorpt_coefficient_mu 1.111
_exptl_absorpt_correction_T_max 0.967
_exptl_absorpt_correction_T_min 0.814
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.831
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 294
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.754
_refine_diff_density_min -0.512
_refine_diff_density_rms 0.088
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.087
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 171
_refine_ls_number_reflns 2384
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.087
_refine_ls_R_factor_all 0.0243
_refine_ls_R_factor_gt 0.0242
_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^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0623
_refine_ls_wR_factor_ref 0.0624
_reflns_number_gt 2371
_reflns_number_total 2384
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cdax.cif
_cod_data_source_block cdax
_cod_database_code 1500027
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
Cd Cd 0.5000 0.5000 0.5000 0.01314(8) Uani 1 2 d S . .
O1W O 0.7203(2) 0.1978(2) 0.51160(16) 0.0185(3) Uani 1 1 d D . .
H11W H 0.816(3) 0.174(4) 0.453(2) 0.022 Uiso 1 1 d D . .
H12W H 0.765(4) 0.139(4) 0.5908(16) 0.022 Uiso 1 1 d D . .
O2W O 0.2685(2) 0.4117(2) 0.45818(16) 0.0190(3) Uani 1 1 d D . .
H21W H 0.217(4) 0.367(4) 0.5322(18) 0.023 Uiso 1 1 d D . .
H22W H 0.177(3) 0.503(3) 0.414(3) 0.023 Uiso 1 1 d D . .
O3W O 0.5736(2) 0.5841(2) 0.26680(16) 0.0189(3) Uani 1 1 d D . .
H31W H 0.669(3) 0.501(3) 0.229(3) 0.023 Uiso 1 1 d D . .
H32W H 0.508(3) 0.673(3) 0.203(2) 0.023 Uiso 1 1 d D . .
N1 N 1.1310(2) 0.0278(2) 0.23502(18) 0.0151(3) Uani 1 1 d . . .
N2 N 0.9733(2) 0.1643(2) 0.27556(19) 0.0167(4) Uani 1 1 d . . .
N3 N 0.8799(2) 0.2987(2) 0.16454(18) 0.0150(3) Uani 1 1 d . . .
C3A C 0.9868(3) 0.2402(3) 0.0522(2) 0.0122(4) Uani 1 1 d . . .
N4 N 0.9558(2) 0.3260(2) -0.08542(18) 0.0123(3) Uani 1 1 d . . .
C4 C 0.7871(3) 0.5040(3) -0.1258(2) 0.0161(4) Uani 1 1 d . . .
H41 H 0.8257 0.5932 -0.1988 0.019 Uiso 1 1 d R . .
H42 H 0.7298 0.5628 -0.0443 0.019 Uiso 1 1 d R . .
H43 H 0.6934 0.4748 -0.1613 0.019 Uiso 1 1 d R . .
C5 C 1.0816(3) 0.2410(3) -0.1869(2) 0.0130(4) Uani 1 1 d . . .
O5 O 1.0543(2) 0.3114(2) -0.31147(15) 0.0155(3) Uani 1 1 d . . .
N6 N 1.2414(2) 0.0726(2) -0.14511(18) 0.0126(3) Uani 1 1 d . . .
C6 C 1.3774(3) -0.0132(3) -0.2560(2) 0.0172(4) Uani 1 1 d . . .
H61 H 1.3088 0.0148 -0.3393 0.021 Uiso 1 1 d R . .
H62 H 1.4398 -0.1526 -0.2237 0.021 Uiso 1 1 d R . .
H63 H 1.4742 0.0410 -0.2787 0.021 Uiso 1 1 d R . .
C7 C 1.2841(3) -0.0221(3) -0.0063(2) 0.0130(4) Uani 1 1 d . . .
O7 O 1.4282(2) -0.1706(2) 0.01954(16) 0.0162(3) Uani 1 1 d . . .
C7A C 1.1435(3) 0.0722(3) 0.0929(2) 0.0127(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
Cd 0.01067(11) 0.01428(11) 0.01035(12) -0.00133(7) -0.00144(7) -0.00144(8)
O1W 0.0164(7) 0.0183(7) 0.0107(7) -0.0003(6) -0.0010(6) 0.0013(6)
O2W 0.0153(7) 0.0254(8) 0.0131(8) 0.0021(6) -0.0029(6) -0.0076(6)
O3W 0.0169(7) 0.0178(7) 0.0123(8) -0.0011(6) -0.0009(6) 0.0012(6)
N1 0.0148(8) 0.0160(8) 0.0112(8) -0.0016(6) -0.0010(6) -0.0033(7)
N2 0.0145(8) 0.0162(8) 0.0141(9) -0.0007(7) -0.0017(7) -0.0022(7)
N3 0.0140(8) 0.0167(8) 0.0106(8) -0.0021(6) -0.0017(6) -0.0028(7)
C3A 0.0112(8) 0.0119(8) 0.0127(10) -0.0010(7) -0.0015(7) -0.0044(7)
N4 0.0116(7) 0.0124(7) 0.0092(8) 0.0000(6) -0.0024(6) -0.0017(6)
C4 0.0117(9) 0.0126(9) 0.0176(10) 0.0002(7) -0.0039(7) 0.0005(7)
C5 0.0119(8) 0.0136(9) 0.0137(10) -0.0008(7) -0.0016(7) -0.0060(7)
O5 0.0149(7) 0.0182(7) 0.0105(7) -0.0004(5) -0.0020(5) -0.0048(6)
N6 0.0113(7) 0.0135(7) 0.0108(8) -0.0026(6) 0.0003(6) -0.0031(6)
C6 0.0145(9) 0.0183(9) 0.0149(10) -0.0054(8) 0.0018(8) -0.0028(8)
C7 0.0125(8) 0.0134(8) 0.0130(10) -0.0017(7) -0.0013(7) -0.0054(7)
O7 0.0143(7) 0.0131(6) 0.0147(7) -0.0004(5) -0.0020(6) -0.0001(5)
C7A 0.0122(8) 0.0121(8) 0.0114(9) 0.0000(7) -0.0018(7) -0.0036(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1W Cd O1W 180.00(8) . 2_666 ?
O1W Cd O3W 92.14(5) . . ?
O1W Cd O3W 87.86(5) 2_666 . ?
O1W Cd O3W 87.86(5) . 2_666 ?
O1W Cd O3W 92.14(5) 2_666 2_666 ?
O3W Cd O3W 180.0 . 2_666 ?
O1W Cd O2W 89.08(6) . 2_666 ?
O1W Cd O2W 90.92(6) 2_666 2_666 ?
O3W Cd O2W 87.32(6) . 2_666 ?
O3W Cd O2W 92.68(6) 2_666 2_666 ?
O1W Cd O2W 90.92(6) . . ?
O1W Cd O2W 89.08(6) 2_666 . ?
O3W Cd O2W 92.68(6) . . ?
O3W Cd O2W 87.32(6) 2_666 . ?
O2W Cd O2W 180.00(3) 2_666 . ?
Cd O1W H11W 119.8(19) . . ?
Cd O1W H12W 116.3(19) . . ?
H11W O1W H12W 106(3) . . ?
Cd O2W H21W 113.1(19) . . ?
Cd O2W H22W 113.9(19) . . ?
H21W O2W H22W 106(3) . . ?
Cd O3W H31W 117.7(19) . . ?
Cd O3W H32W 131(2) . . ?
H31W O3W H32W 109(3) . . ?
N2 N1 C7A 106.37(16) . . ?
N1 N2 N3 111.95(16) . . ?
C3A N3 N2 104.90(16) . . ?
N3 C3A N4 128.04(17) . . ?
N3 C3A C7A 109.66(18) . . ?
N4 C3A C7A 122.30(18) . . ?
C5 N4 C3A 119.33(16) . . ?
C5 N4 C4 119.49(16) . . ?
C3A N4 C4 121.15(17) . . ?
N4 C4 H41 109.4 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.6 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 120.81(17) . . ?
O5 C5 N6 121.08(18) . . ?
N4 C5 N6 118.11(17) . . ?
C5 N6 C7 125.76(17) . . ?
C5 N6 C6 117.16(17) . . ?
C7 N6 C6 117.08(16) . . ?
N6 C6 H61 109.5 . . ?
N6 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.4 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 120.74(18) . . ?
O7 C7 C7A 126.59(19) . . ?
N6 C7 C7A 112.67(16) . . ?
N1 C7A C3A 107.13(17) . . ?
N1 C7A C7 131.08(17) . . ?
C3A C7A C7 121.78(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd O1W 2.2472(14) . ?
Cd O1W 2.2473(14) 2_666 ?
Cd O3W 2.2910(16) . ?
Cd O3W 2.2910(16) 2_666 ?
Cd O2W 2.2974(15) 2_666 ?
Cd O2W 2.2974(15) . ?
O1W H11W 0.852(10) . ?
O1W H12W 0.849(10) . ?
O2W H21W 0.848(10) . ?
O2W H22W 0.851(10) . ?
O3W H31W 0.859(10) . ?
O3W H32W 0.850(10) . ?
N1 N2 1.323(2) . ?
N1 C7A 1.362(3) . ?
N2 N3 1.370(2) . ?
N3 C3A 1.333(3) . ?
C3A N4 1.372(3) . ?
C3A C7A 1.382(3) . ?
N4 C5 1.370(3) . ?
N4 C4 1.470(2) . ?
C4 H41 0.9801 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 O5 1.232(2) . ?
C5 N6 1.399(2) . ?
N6 C7 1.408(3) . ?
N6 C6 1.473(3) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 O7 1.229(2) . ?
C7 C7A 1.428(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W N2 0.852(10) 1.969(13) 2.792(2) 162(3) .
O1W H12W N1 0.849(10) 1.940(11) 2.783(2) 172(3) 2_756
O2W H21W O5 0.848(10) 1.921(11) 2.757(2) 168(3) 1_456
O2W H22W O5 0.851(10) 1.994(11) 2.839(2) 171(3) 2_665
O3W H31W N3 0.859(10) 1.889(11) 2.744(2) 174(3) .
O3W H32W O7 0.850(10) 1.953(13) 2.771(2) 161(3) 1_465
|
1500028.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500028.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_1500028
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 372
_journal_page_last 378
_journal_paper_doi 10.1016/j.poly.2009.06.002
_journal_volume 29
_journal_year 2010
_chemical_formula_moiety 'C18 H29 Cu N13 O4'
_chemical_formula_sum 'C18 H29 Cu N13 O4'
_chemical_formula_weight 555.08
_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 heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 113.298(1)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.4355(6)
_cell_length_b 40.985(3)
_cell_length_c 7.1685(5)
_cell_measurement_reflns_used 5063
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.8
_cell_measurement_theta_min 2.6
_cell_volume 2276.3(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0270
_diffrn_reflns_av_sigmaI/netI 0.0229
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 53
_diffrn_reflns_limit_k_min -54
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 26461
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 28.37
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% 0.0
_diffrn_standards_number 426
_exptl_absorpt_coefficient_mu 1.017
_exptl_absorpt_correction_T_max 0.914
_exptl_absorpt_correction_T_min 0.770
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.620
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1156
_exptl_crystal_size_max 0.47
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.335
_refine_diff_density_min -0.373
_refine_diff_density_rms 0.061
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.255
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 329
_refine_ls_number_reflns 5334
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.255
_refine_ls_R_factor_all 0.0530
_refine_ls_R_factor_gt 0.0476
_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^)+(0.0300P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1100
_refine_ls_wR_factor_ref 0.1121
_reflns_number_gt 4848
_reflns_number_total 5334
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cubapadmax.cif
_cod_data_source_block cutrenax
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500028
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 0.11762(4) 0.377801(7) 0.35923(5) 0.03240(11) Uani 1 1 d . . .
N1A N 0.3507(3) 0.42991(5) 0.6161(4) 0.0351(5) Uani 1 1 d . . .
N2A N 0.2028(3) 0.42300(5) 0.4636(4) 0.0359(5) Uani 1 1 d . . .
N3A N 0.1122(3) 0.44999(5) 0.3677(4) 0.0359(5) Uani 1 1 d . . .
C3AA C 0.2123(3) 0.47459(6) 0.4681(4) 0.0307(5) Uani 1 1 d . . .
N4A N 0.1788(3) 0.50744(5) 0.4306(4) 0.0328(5) Uani 1 1 d . . .
C4A C 0.0288(4) 0.51884(7) 0.2551(5) 0.0404(7) Uani 1 1 d . . .
H41A H -0.0247 0.5366 0.2956 0.049 Uiso 1 1 d R . .
H42A H -0.0525 0.5013 0.2038 0.049 Uiso 1 1 d R . .
H43A H 0.0652 0.5261 0.1510 0.049 Uiso 1 1 d R . .
C5A C 0.2974(4) 0.52970(6) 0.5479(4) 0.0335(6) Uani 1 1 d . . .
O5A O 0.2739(3) 0.55904(5) 0.5200(3) 0.0427(5) Uani 1 1 d . . .
N6A N 0.4471(3) 0.51757(5) 0.7013(3) 0.0330(5) Uani 1 1 d . . .
C6A C 0.5709(4) 0.54211(7) 0.8248(5) 0.0401(7) Uani 1 1 d . . .
H61A H 0.5942 0.5574 0.7374 0.048 Uiso 1 1 d R . .
H62A H 0.6762 0.5315 0.9099 0.048 Uiso 1 1 d R . .
H63A H 0.5234 0.5534 0.9080 0.048 Uiso 1 1 d R . .
C7A C 0.4922(4) 0.48453(6) 0.7503(4) 0.0324(6) Uani 1 1 d . . .
O7A O 0.6285(3) 0.47716(5) 0.8856(3) 0.0433(5) Uani 1 1 d . . .
C7AA C 0.3591(3) 0.46298(6) 0.6206(4) 0.0311(5) Uani 1 1 d . . .
N1B N -0.1231(3) 0.32465(5) 0.3884(4) 0.0360(5) Uani 1 1 d . . .
N2B N 0.0348(3) 0.33143(5) 0.4086(4) 0.0361(5) Uani 1 1 d . . .
N3B N 0.1340(3) 0.30422(5) 0.4263(4) 0.0362(5) Uani 1 1 d . . .
C3AB C 0.0268(3) 0.27979(6) 0.4145(4) 0.0311(5) Uani 1 1 d . . .
N4B N 0.0621(3) 0.24678(5) 0.4190(4) 0.0351(5) Uani 1 1 d . . .
C4B C 0.2317(4) 0.23491(7) 0.4405(5) 0.0446(7) Uani 1 1 d . . .
H41B H 0.2929 0.2268 0.5757 0.054 Uiso 1 1 d R . .
H42B H 0.2960 0.2525 0.4153 0.054 Uiso 1 1 d R . .
H43B H 0.2178 0.2177 0.3444 0.054 Uiso 1 1 d R . .
C5B C -0.0657(4) 0.22488(6) 0.4008(4) 0.0359(6) Uani 1 1 d . . .
O5B O -0.0424(3) 0.19558(5) 0.4015(4) 0.0498(6) Uani 1 1 d . . .
N6B N -0.2266(3) 0.23742(5) 0.3806(4) 0.0367(5) Uani 1 1 d . . .
C6B C -0.3619(4) 0.21315(8) 0.3548(5) 0.0505(8) Uani 1 1 d . . .
H61B H -0.3839 0.2008 0.2332 0.061 Uiso 1 1 d R . .
H62B H -0.4657 0.2241 0.3445 0.061 Uiso 1 1 d R . .
H63B H -0.3246 0.1987 0.4695 0.061 Uiso 1 1 d R . .
C7B C -0.2723(4) 0.27060(7) 0.3791(4) 0.0346(6) Uani 1 1 d . . .
O7B O -0.4148(3) 0.27836(5) 0.3661(4) 0.0491(6) Uani 1 1 d . . .
C7AB C -0.1316(3) 0.29149(6) 0.3931(4) 0.0320(6) Uani 1 1 d . . .
N1E N -0.1273(3) 0.39244(5) 0.2744(4) 0.0380(5) Uani 1 1 d . . .
H11E H -0.1882 0.3751 0.2859 0.046 Uiso 1 1 d R . .
H12E H -0.1291 0.4072 0.3663 0.046 Uiso 1 1 d R . .
C2E C -0.2226(4) 0.40665(8) 0.0716(5) 0.0507(8) Uani 1 1 d . . .
H21E H -0.1801 0.4286 0.0691 0.061 Uiso 1 1 d R . .
H22E H -0.3435 0.4083 0.0489 0.061 Uiso 1 1 d R . .
C3E C -0.2071(5) 0.38725(9) -0.0995(5) 0.0565(9) Uani 1 1 d . . .
H31E H -0.2355 0.3647 -0.0859 0.068 Uiso 1 1 d R . .
H32E H -0.2920 0.3953 -0.2271 0.068 Uiso 1 1 d R . .
C4E C -0.0329(5) 0.38820(9) -0.1096(5) 0.0568(9) Uani 1 1 d . . .
H41E H -0.0432 0.3800 -0.2408 0.068 Uiso 1 1 d R . .
H42E H 0.0047 0.4107 -0.0996 0.068 Uiso 1 1 d R . .
N5E N 0.1005(3) 0.36916(5) 0.0514(4) 0.0353(5) Uani 1 1 d . . .
H5E H 0.0638 0.3481 0.0247 0.042 Uiso 1 1 d R . .
C6E C 0.2629(4) 0.36988(8) 0.0205(5) 0.0505(8) Uani 1 1 d . . .
H61E H 0.3005 0.3923 0.0255 0.061 Uiso 1 1 d R . .
H62E H 0.2417 0.3614 -0.1137 0.061 Uiso 1 1 d R . .
C7E C 0.4055(4) 0.35027(9) 0.1759(6) 0.0531(9) Uani 1 1 d . . .
H71E H 0.4978 0.3478 0.1286 0.064 Uiso 1 1 d R . .
H72E H 0.3613 0.3286 0.1828 0.064 Uiso 1 1 d R . .
C8E C 0.4807(4) 0.36425(7) 0.3875(5) 0.0452(7) Uani 1 1 d . . .
H81E H 0.5878 0.3530 0.4658 0.054 Uiso 1 1 d R . .
H82E H 0.5071 0.3871 0.3806 0.054 Uiso 1 1 d R . .
N9E N 0.3618(3) 0.36099(6) 0.4913(4) 0.0408(6) Uani 1 1 d . . .
H91E H 0.4114 0.3710 0.6125 0.049 Uiso 1 1 d R . .
H92E H 0.3555 0.3396 0.5165 0.049 Uiso 1 1 d R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.02946(17) 0.02181(16) 0.0411(2) -0.00117(13) 0.00880(14) 0.00037(12)
N1A 0.0369(12) 0.0244(11) 0.0409(13) -0.0007(9) 0.0119(10) -0.0017(9)
N2A 0.0362(12) 0.0246(11) 0.0445(13) -0.0027(9) 0.0135(10) -0.0015(9)
N3A 0.0351(12) 0.0258(11) 0.0436(13) -0.0010(10) 0.0122(10) -0.0019(9)
C3AA 0.0345(13) 0.0233(12) 0.0370(14) -0.0009(10) 0.0172(11) -0.0009(10)
N4A 0.0358(12) 0.0237(11) 0.0374(12) 0.0020(9) 0.0129(10) 0.0014(9)
C4A 0.0439(16) 0.0318(14) 0.0418(16) 0.0045(12) 0.0129(13) 0.0051(12)
C5A 0.0445(15) 0.0245(13) 0.0383(15) -0.0026(10) 0.0235(13) -0.0015(11)
O5A 0.0552(13) 0.0231(9) 0.0524(13) -0.0001(8) 0.0239(10) 0.0009(9)
N6A 0.0402(12) 0.0233(10) 0.0355(12) -0.0039(9) 0.0149(10) -0.0060(9)
C6A 0.0455(16) 0.0285(14) 0.0460(17) -0.0087(12) 0.0178(13) -0.0099(12)
C7A 0.0386(14) 0.0272(12) 0.0345(14) -0.0016(11) 0.0180(12) -0.0031(11)
O7A 0.0390(11) 0.0371(11) 0.0447(12) 0.0019(9) 0.0067(9) -0.0012(9)
C7AA 0.0354(14) 0.0235(12) 0.0341(14) -0.0006(10) 0.0134(11) -0.0019(10)
N1B 0.0340(12) 0.0243(11) 0.0478(14) 0.0029(10) 0.0141(10) 0.0001(9)
N2B 0.0324(12) 0.0248(11) 0.0479(14) 0.0046(10) 0.0126(10) 0.0015(9)
N3B 0.0333(12) 0.0274(11) 0.0462(14) 0.0059(10) 0.0138(10) 0.0030(9)
C3AB 0.0326(13) 0.0247(12) 0.0329(13) 0.0037(10) 0.0097(11) 0.0007(10)
N4B 0.0367(12) 0.0220(10) 0.0436(13) 0.0044(9) 0.0128(10) 0.0060(9)
C4B 0.0389(16) 0.0352(15) 0.0558(19) 0.0040(13) 0.0147(14) 0.0095(12)
C5B 0.0466(16) 0.0235(12) 0.0324(14) 0.0036(10) 0.0103(12) 0.0015(11)
O5B 0.0613(14) 0.0234(10) 0.0591(14) 0.0042(9) 0.0178(11) 0.0039(9)
N6B 0.0367(12) 0.0267(11) 0.0427(13) 0.0042(10) 0.0112(10) -0.0029(9)
C6B 0.0481(18) 0.0366(16) 0.061(2) 0.0030(14) 0.0152(16) -0.0130(14)
C7B 0.0333(14) 0.0299(13) 0.0366(14) 0.0046(11) 0.0096(11) -0.0024(11)
O7B 0.0346(11) 0.0434(12) 0.0688(15) 0.0059(11) 0.0200(11) 0.0001(9)
C7AB 0.0329(13) 0.0237(12) 0.0361(14) 0.0036(10) 0.0101(11) 0.0015(10)
N1E 0.0331(12) 0.0230(11) 0.0551(15) -0.0014(10) 0.0143(11) 0.0026(9)
C2E 0.0400(16) 0.0343(16) 0.063(2) 0.0041(14) 0.0043(15) 0.0086(13)
C3E 0.0497(19) 0.0482(19) 0.049(2) 0.0000(15) -0.0040(15) 0.0069(15)
C4E 0.063(2) 0.057(2) 0.0435(19) 0.0129(16) 0.0138(16) 0.0089(17)
N5E 0.0398(13) 0.0239(11) 0.0395(13) -0.0019(9) 0.0128(10) -0.0028(9)
C6E 0.055(2) 0.0501(19) 0.0519(19) -0.0093(15) 0.0267(16) -0.0109(15)
C7E 0.0445(18) 0.0486(19) 0.069(2) -0.0163(17) 0.0256(17) 0.0004(15)
C8E 0.0307(14) 0.0341(15) 0.068(2) -0.0050(14) 0.0162(14) -0.0023(12)
N9E 0.0301(12) 0.0281(12) 0.0562(16) 0.0042(11) 0.0083(11) 0.0018(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N1E Cu N9E 169.95(11) . . ?
N1E Cu N2A 90.61(9) . . ?
N9E Cu N2A 89.55(10) . . ?
N1E Cu N2B 87.16(9) . . ?
N9E Cu N2B 87.57(9) . . ?
N2A Cu N2B 149.26(10) . . ?
N1E Cu N5E 95.37(10) . . ?
N9E Cu N5E 93.79(10) . . ?
N2A Cu N5E 113.26(9) . . ?
N2B Cu N5E 97.47(9) . . ?
N2A N1A C7AA 104.9(2) . . ?
N1A N2A N3A 113.6(2) . . ?
N1A N2A Cu 125.63(18) . . ?
N3A N2A Cu 120.67(17) . . ?
C3AA N3A N2A 103.5(2) . . ?
N3A C3AA C7AA 110.4(2) . . ?
N3A C3AA N4A 126.7(2) . . ?
C7AA C3AA N4A 123.0(2) . . ?
C5A N4A C3AA 119.1(2) . . ?
C5A N4A C4A 119.2(2) . . ?
C3AA N4A C4A 121.3(2) . . ?
N4A C4A H41A 109.4 . . ?
N4A C4A H42A 109.5 . . ?
H41A C4A H42A 109.5 . . ?
N4A C4A H43A 109.5 . . ?
H41A C4A H43A 109.5 . . ?
H42A C4A H43A 109.5 . . ?
O5A C5A N4A 121.6(3) . . ?
O5A C5A N6A 121.1(3) . . ?
N4A C5A N6A 117.4(2) . . ?
C5A N6A C7A 127.4(2) . . ?
C5A N6A C6A 115.9(2) . . ?
C7A N6A C6A 116.7(2) . . ?
N6A C6A H61A 109.5 . . ?
N6A C6A H62A 109.4 . . ?
H61A C6A H62A 109.5 . . ?
N6A C6A H63A 109.5 . . ?
H61A C6A H63A 109.5 . . ?
H62A C6A H63A 109.5 . . ?
O7A C7A N6A 121.0(2) . . ?
O7A C7A C7AA 127.8(3) . . ?
N6A C7A C7AA 111.2(2) . . ?
N1A C7AA C3AA 107.8(2) . . ?
N1A C7AA C7A 130.3(2) . . ?
C3AA C7AA C7A 121.9(2) . . ?
N2B N1B C7AB 105.6(2) . . ?
N1B N2B N3B 113.2(2) . . ?
N1B N2B Cu 124.28(17) . . ?
N3B N2B Cu 121.35(17) . . ?
C3AB N3B N2B 103.4(2) . . ?
N3B C3AB C7AB 110.6(2) . . ?
N3B C3AB N4B 126.9(2) . . ?
C7AB C3AB N4B 122.5(2) . . ?
C5B N4B C3AB 119.0(2) . . ?
C5B N4B C4B 119.6(2) . . ?
C3AB N4B C4B 121.4(2) . . ?
N4B C4B H41B 109.6 . . ?
N4B C4B H42B 109.4 . . ?
H41B C4B H42B 109.5 . . ?
N4B C4B H43B 109.4 . . ?
H41B C4B H43B 109.5 . . ?
H42B C4B H43B 109.5 . . ?
O5B C5B N4B 121.8(3) . . ?
O5B C5B N6B 120.6(3) . . ?
N4B C5B N6B 117.6(2) . . ?
C5B N6B C7B 127.1(2) . . ?
C5B N6B C6B 115.9(2) . . ?
C7B N6B C6B 117.1(2) . . ?
N6B C6B H61B 109.4 . . ?
N6B C6B H62B 109.4 . . ?
H61B C6B H62B 109.5 . . ?
N6B C6B H63B 109.5 . . ?
H61B C6B H63B 109.5 . . ?
H62B C6B H63B 109.5 . . ?
O7B C7B N6B 120.9(3) . . ?
O7B C7B C7AB 128.1(3) . . ?
N6B C7B C7AB 111.0(2) . . ?
N1B C7AB C3AB 107.1(2) . . ?
N1B C7AB C7B 130.1(3) . . ?
C3AB C7AB C7B 122.8(2) . . ?
C2E N1E Cu 120.9(2) . . ?
C2E N1E H11E 107.1 . . ?
Cu N1E H11E 107.1 . . ?
C2E N1E H12E 107.2 . . ?
Cu N1E H12E 107.1 . . ?
H11E N1E H12E 106.8 . . ?
N1E C2E C3E 113.8(3) . . ?
N1E C2E H21E 108.8 . . ?
C3E C2E H21E 108.8 . . ?
N1E C2E H22E 108.7 . . ?
C3E C2E H22E 108.9 . . ?
H21E C2E H22E 107.7 . . ?
C4E C3E C2E 115.2(3) . . ?
C4E C3E H31E 108.4 . . ?
C2E C3E H31E 108.4 . . ?
C4E C3E H32E 108.5 . . ?
C2E C3E H32E 108.5 . . ?
H31E C3E H32E 107.5 . . ?
N5E C4E C3E 114.0(3) . . ?
N5E C4E H41E 108.8 . . ?
C3E C4E H41E 108.9 . . ?
N5E C4E H42E 108.7 . . ?
C3E C4E H42E 108.6 . . ?
H41E C4E H42E 107.7 . . ?
C6E N5E C4E 109.8(3) . . ?
C6E N5E Cu 117.09(19) . . ?
C4E N5E Cu 115.5(2) . . ?
C6E N5E H5E 104.3 . . ?
C4E N5E H5E 104.2 . . ?
Cu N5E H5E 104.3 . . ?
N5E C6E C7E 113.4(3) . . ?
N5E C6E H61E 108.9 . . ?
C7E C6E H61E 109.0 . . ?
N5E C6E H62E 108.9 . . ?
C7E C6E H62E 108.8 . . ?
H61E C6E H62E 107.7 . . ?
C8E C7E C6E 115.9(3) . . ?
C8E C7E H71E 108.4 . . ?
C6E C7E H71E 108.3 . . ?
C8E C7E H72E 108.3 . . ?
C6E C7E H72E 108.3 . . ?
H71E C7E H72E 107.4 . . ?
N9E C8E C7E 112.0(3) . . ?
N9E C8E H81E 109.2 . . ?
C7E C8E H81E 109.1 . . ?
N9E C8E H82E 109.2 . . ?
C7E C8E H82E 109.3 . . ?
H81E C8E H82E 107.9 . . ?
C8E N9E Cu 120.3(2) . . ?
C8E N9E H91E 107.3 . . ?
Cu N9E H91E 107.2 . . ?
C8E N9E H92E 107.2 . . ?
Cu N9E H92E 107.2 . . ?
H91E N9E H92E 106.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu N1E 2.001(2) . ?
Cu N9E 2.017(2) . ?
Cu N2A 2.021(2) . ?
Cu N2B 2.102(2) . ?
Cu N5E 2.183(2) . ?
N1A N2A 1.324(3) . ?
N1A C7AA 1.357(3) . ?
N2A N3A 1.365(3) . ?
N3A C3AA 1.329(3) . ?
C3AA C7AA 1.373(4) . ?
C3AA N4A 1.380(3) . ?
N4A C5A 1.369(3) . ?
N4A C4A 1.464(4) . ?
C4A H41A 0.9599 . ?
C4A H42A 0.9601 . ?
C4A H43A 0.9600 . ?
C5A O5A 1.222(3) . ?
C5A N6A 1.398(4) . ?
N6A C7A 1.413(3) . ?
N6A C6A 1.468(3) . ?
C6A H61A 0.9600 . ?
C6A H62A 0.9600 . ?
C6A H63A 0.9600 . ?
C7A O7A 1.213(3) . ?
C7A C7AA 1.442(4) . ?
N1B N2B 1.312(3) . ?
N1B C7AB 1.362(3) . ?
N2B N3B 1.370(3) . ?
N3B C3AB 1.330(3) . ?
C3AB C7AB 1.370(4) . ?
C3AB N4B 1.383(3) . ?
N4B C5B 1.369(4) . ?
N4B C4B 1.460(4) . ?
C4B H41B 0.9600 . ?
C4B H42B 0.9600 . ?
C4B H43B 0.9600 . ?
C5B O5B 1.217(3) . ?
C5B N6B 1.404(4) . ?
N6B C7B 1.412(3) . ?
N6B C6B 1.469(4) . ?
C6B H61B 0.9600 . ?
C6B H62B 0.9600 . ?
C6B H63B 0.9600 . ?
C7B O7B 1.211(3) . ?
C7B C7AB 1.435(4) . ?
N1E C2E 1.474(4) . ?
N1E H11E 0.9000 . ?
N1E H12E 0.9000 . ?
C2E C3E 1.510(5) . ?
C2E H21E 0.9700 . ?
C2E H22E 0.9700 . ?
C3E C4E 1.501(5) . ?
C3E H31E 0.9700 . ?
C3E H32E 0.9700 . ?
C4E N5E 1.476(4) . ?
C4E H41E 0.9700 . ?
C4E H42E 0.9700 . ?
N5E C6E 1.472(4) . ?
N5E H5E 0.9100 . ?
C6E C7E 1.508(5) . ?
C6E H61E 0.9700 . ?
C6E H62E 0.9700 . ?
C7E C8E 1.507(5) . ?
C7E H71E 0.9700 . ?
C7E H72E 0.9700 . ?
C8E N9E 1.473(4) . ?
C8E H81E 0.9700 . ?
C8E H82E 0.9700 . ?
N9E H91E 0.9000 . ?
N9E H92E 0.9000 . ?
|
1500029.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500029.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_1500029
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 372
_journal_page_last 378
_journal_paper_doi 10.1016/j.poly.2009.06.002
_journal_volume 29
_journal_year 2010
_chemical_formula_moiety 'C16 H28 Cu N14 O4, 2 (H2 O)'
_chemical_formula_sum 'C16 H32 Cu N14 O6'
_chemical_formula_weight 580.10
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 108.819(1)
_cell_angle_beta 96.302(1)
_cell_angle_gamma 97.634(1)
_cell_formula_units_Z 1
_cell_length_a 7.5499(6)
_cell_length_b 8.1885(6)
_cell_length_c 10.9247(9)
_cell_measurement_reflns_used 2826
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.7
_cell_volume 625.18(9)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0126
_diffrn_reflns_av_sigmaI/netI 0.0243
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 3961
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 28.20
_diffrn_reflns_theta_min 2.00
_diffrn_standards_decay_% 1.1
_diffrn_standards_number 204
_exptl_absorpt_coefficient_mu 0.936
_exptl_absorpt_correction_T_max 0.850
_exptl_absorpt_correction_T_min 0.688
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.541
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 303
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.389
_refine_diff_density_min -0.319
_refine_diff_density_rms 0.061
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 177
_refine_ls_number_reflns 2679
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0311
_refine_ls_R_factor_gt 0.0303
_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^)+(0.0400P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0782
_refine_ls_wR_factor_ref 0.0787
_reflns_number_gt 2579
_reflns_number_total 2679
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cuendmax.cif
_cod_data_source_block cuendmax
_cod_database_code 1500029
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
Cu Cu 0.5000 0.5000 0.5000 0.01472(10) Uani 1 2 d S . .
N1 N 0.32670(19) 0.40219(18) 0.66906(14) 0.0168(3) Uani 1 1 d . . .
N2 N 0.2469(2) 0.23594(19) 0.63026(14) 0.0181(3) Uani 1 1 d . . .
N3 N 0.1819(2) 0.19187(19) 0.72961(14) 0.0182(3) Uani 1 1 d . . .
C3A C 0.2251(2) 0.3385(2) 0.83347(16) 0.0156(3) Uani 1 1 d . . .
N4 N 0.1918(2) 0.36377(19) 0.95955(14) 0.0180(3) Uani 1 1 d . . .
C4 C 0.1105(3) 0.2182(3) 0.99739(19) 0.0255(4) Uani 1 1 d . . .
H41 H 0.2031 0.1873 1.0520 0.031 Uiso 1 1 d R . .
H42 H 0.0610 0.1165 0.9184 0.031 Uiso 1 1 d R . .
H43 H 0.0129 0.2531 1.0469 0.031 Uiso 1 1 d R . .
C5 C 0.2407(2) 0.5283(2) 1.05237(17) 0.0178(3) Uani 1 1 d . . .
O5 O 0.20808(18) 0.55970(18) 1.16422(12) 0.0248(3) Uani 1 1 d . . .
N6 N 0.3298(2) 0.66135(19) 1.01504(14) 0.0170(3) Uani 1 1 d . . .
C6 C 0.3813(3) 0.8350(2) 1.11900(17) 0.0236(4) Uani 1 1 d . . .
H61 H 0.2764 0.8659 1.1610 0.028 Uiso 1 1 d R . .
H62 H 0.4230 0.9229 1.0804 0.028 Uiso 1 1 d R . .
H63 H 0.4791 0.8316 1.1845 0.028 Uiso 1 1 d R . .
C7 C 0.3744(2) 0.6451(2) 0.89029(16) 0.0170(3) Uani 1 1 d . . .
O7 O 0.45450(19) 0.77106(16) 0.86896(13) 0.0245(3) Uani 1 1 d . . .
C7A C 0.3146(2) 0.4709(2) 0.79883(16) 0.0153(3) Uani 1 1 d . . .
N1E N 0.48360(19) 0.75323(18) 0.59323(14) 0.0166(3) Uani 1 1 d . . .
H11E H 0.4599 0.7682 0.6766 0.020 Uiso 1 1 d R . .
H12E H 0.5911 0.8251 0.5992 0.020 Uiso 1 1 d R . .
C1E C 0.3348(2) 0.7974(2) 0.51656(19) 0.0210(4) Uani 1 1 d . . .
H13E H 0.3766 0.8210 0.4401 0.025 Uiso 1 1 d R . .
H14E H 0.2945 0.9034 0.5715 0.025 Uiso 1 1 d R . .
C2E C 0.1808(2) 0.6419(2) 0.47137(19) 0.0214(4) Uani 1 1 d . . .
H23E H 0.1299 0.6266 0.5475 0.026 Uiso 1 1 d R . .
H24E H 0.0832 0.6607 0.4117 0.026 Uiso 1 1 d R . .
N2E N 0.25428(19) 0.48495(18) 0.40204(14) 0.0162(3) Uani 1 1 d . . .
H21E H 0.2629 0.4803 0.3177 0.019 Uiso 1 1 d R . .
H22E H 0.1787 0.3851 0.3984 0.019 Uiso 1 1 d R . .
O1W O 0.11003(19) 0.10330(17) 0.35873(13) 0.0242(3) Uani 1 1 d D . .
H11W H 0.137(3) 0.122(3) 0.4388(11) 0.029 Uiso 1 1 d D . .
H12W H 0.020(2) 0.022(2) 0.333(2) 0.029 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 0.01360(15) 0.01031(15) 0.01794(16) 0.00238(11) 0.00035(10) 0.00229(10)
N1 0.0174(7) 0.0144(7) 0.0160(7) 0.0023(5) 0.0019(5) 0.0022(5)
N2 0.0182(7) 0.0151(7) 0.0191(7) 0.0044(6) 0.0019(5) 0.0013(5)
N3 0.0189(7) 0.0137(7) 0.0196(7) 0.0043(6) 0.0010(5) 0.0003(5)
C3A 0.0127(7) 0.0153(8) 0.0183(8) 0.0058(6) 0.0004(6) 0.0022(6)
N4 0.0187(7) 0.0169(7) 0.0184(7) 0.0076(6) 0.0028(5) -0.0002(6)
C4 0.0252(10) 0.0259(10) 0.0285(10) 0.0155(8) 0.0052(8) -0.0014(8)
C5 0.0160(8) 0.0210(9) 0.0179(8) 0.0082(7) 0.0022(6) 0.0055(6)
O5 0.0289(7) 0.0305(7) 0.0178(6) 0.0099(5) 0.0067(5) 0.0086(6)
N6 0.0201(7) 0.0151(7) 0.0138(7) 0.0024(5) 0.0020(5) 0.0031(6)
C6 0.0287(10) 0.0178(9) 0.0187(8) -0.0002(7) 0.0021(7) 0.0032(7)
C7 0.0174(8) 0.0163(8) 0.0169(8) 0.0051(6) 0.0026(6) 0.0028(6)
O7 0.0339(7) 0.0151(6) 0.0212(6) 0.0042(5) 0.0058(5) -0.0029(5)
C7A 0.0150(8) 0.0145(8) 0.0154(8) 0.0041(6) 0.0023(6) 0.0014(6)
N1E 0.0168(7) 0.0129(7) 0.0194(7) 0.0041(5) 0.0059(5) 0.0012(5)
C1E 0.0218(9) 0.0153(8) 0.0290(9) 0.0094(7) 0.0079(7) 0.0068(7)
C2E 0.0159(8) 0.0210(9) 0.0286(9) 0.0082(7) 0.0060(7) 0.0068(7)
N2E 0.0157(7) 0.0159(7) 0.0172(7) 0.0065(6) 0.0027(5) 0.0017(5)
O1W 0.0254(7) 0.0213(7) 0.0201(6) 0.0040(5) 0.0039(5) -0.0083(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N2E Cu N2E 180.0 . 2_666 ?
N2E Cu N1E 85.15(6) . . ?
N2E Cu N1E 94.85(6) 2_666 . ?
N2E Cu N1E 94.85(6) . 2_666 ?
N2E Cu N1E 85.15(6) 2_666 2_666 ?
N1E Cu N1E 180.000(2) . 2_666 ?
N2E Cu N1 93.79(5) . 2_666 ?
N2E Cu N1 86.21(5) 2_666 2_666 ?
N1E Cu N1 89.23(5) . 2_666 ?
N1E Cu N1 90.77(5) 2_666 2_666 ?
N2E Cu N1 86.21(5) . . ?
N2E Cu N1 93.79(5) 2_666 . ?
N1E Cu N1 90.77(5) . . ?
N1E Cu N1 89.23(5) 2_666 . ?
N1 Cu N1 180.0 2_666 . ?
N2 N1 C7A 105.90(14) . . ?
N2 N1 Cu 116.50(10) . . ?
C7A N1 Cu 136.84(11) . . ?
N1 N2 N3 112.26(13) . . ?
C3A N3 N2 104.82(14) . . ?
N3 C3A C7A 109.66(15) . . ?
N3 C3A N4 128.02(16) . . ?
C7A C3A N4 122.31(15) . . ?
C5 N4 C3A 119.14(15) . . ?
C5 N4 C4 119.25(15) . . ?
C3A N4 C4 121.59(15) . . ?
N4 C4 H41 109.5 . . ?
N4 C4 H42 109.3 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.6 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 121.94(17) . . ?
O5 C5 N6 120.41(16) . . ?
N4 C5 N6 117.65(15) . . ?
C5 N6 C7 126.68(14) . . ?
C5 N6 C6 115.40(14) . . ?
C7 N6 C6 117.92(14) . . ?
N6 C6 H61 109.6 . . ?
N6 C6 H62 109.3 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.04(15) . . ?
O7 C7 C7A 126.95(16) . . ?
N6 C7 C7A 112.01(15) . . ?
N1 C7A C3A 107.36(15) . . ?
N1 C7A C7 130.50(16) . . ?
C3A C7A C7 122.13(15) . . ?
C1E N1E Cu 107.65(10) . . ?
C1E N1E H11E 110.1 . . ?
Cu N1E H11E 110.1 . . ?
C1E N1E H12E 110.2 . . ?
Cu N1E H12E 110.3 . . ?
H11E N1E H12E 108.5 . . ?
N1E C1E C2E 107.42(14) . . ?
N1E C1E H13E 110.1 . . ?
C2E C1E H13E 110.2 . . ?
N1E C1E H14E 110.3 . . ?
C2E C1E H14E 110.3 . . ?
H13E C1E H14E 108.5 . . ?
N2E C2E C1E 107.61(14) . . ?
N2E C2E H23E 110.2 . . ?
C1E C2E H23E 110.2 . . ?
N2E C2E H24E 110.1 . . ?
C1E C2E H24E 110.1 . . ?
H23E C2E H24E 108.5 . . ?
C2E N2E Cu 108.30(11) . . ?
C2E N2E H21E 110.1 . . ?
Cu N2E H21E 110.0 . . ?
C2E N2E H22E 110.0 . . ?
Cu N2E H22E 110.0 . . ?
H21E N2E H22E 108.4 . . ?
H11W O1W H12W 105(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
Cu N2E 2.0051(14) . ?
Cu N2E 2.0052(14) 2_666 ?
Cu N1E 2.0213(14) . ?
Cu N1E 2.0214(14) 2_666 ?
Cu N1 2.6402(14) 2_666 ?
Cu N1 2.6402(14) . ?
N1 N2 1.323(2) . ?
N1 C7A 1.365(2) . ?
N2 N3 1.368(2) . ?
N3 C3A 1.331(2) . ?
C3A C7A 1.379(2) . ?
C3A N4 1.382(2) . ?
N4 C5 1.372(2) . ?
N4 C4 1.466(2) . ?
C4 H41 0.9801 . ?
C4 H42 0.9801 . ?
C4 H43 0.9801 . ?
C5 O5 1.225(2) . ?
C5 N6 1.400(2) . ?
N6 C7 1.408(2) . ?
N6 C6 1.475(2) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 O7 1.227(2) . ?
C7 C7A 1.431(2) . ?
N1E C1E 1.480(2) . ?
N1E H11E 0.9200 . ?
N1E H12E 0.9200 . ?
C1E C2E 1.514(3) . ?
C1E H13E 0.9900 . ?
C1E H14E 0.9900 . ?
C2E N2E 1.479(2) . ?
C2E H23E 0.9900 . ?
C2E H24E 0.9900 . ?
N2E H21E 0.9200 . ?
N2E H22E 0.9200 . ?
O1W H11W 0.834(10) . ?
O1W H12W 0.836(10) . ?
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
N1E H11E O7 0.92 2.10 3.0023(19) 167.0 .
N1E H12E O1W 0.92 2.21 3.0593(19) 152.8 2_666
N2E H21E O5 0.92 2.01 2.8514(19) 151.9 1_554
N2E H22E O1W 0.92 2.18 3.0340(19) 153.3 .
O1W H11W N2 0.834(10) 2.022(12) 2.828(2) 162(2) .
O1W H12W N3 0.836(10) 2.038(10) 2.871(2) 174(2) 2_556
|
1500030.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500030.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_1500030
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full 'Inorganic Chemistry Communications'
_journal_page_first 399
_journal_page_last 403
_journal_paper_doi 10.1016/j.inoche.2009.12.033
_journal_volume 13
_journal_year 2010
_chemical_formula_moiety
'C24 H22 Cu2 N4 O4 2+, 2(C6 H6 N5 O2 1-), 10(H2 O)'
_chemical_formula_sum 'C36 H54 Cu2 N14 O18'
_chemical_formula_weight 1098.01
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 71.035(2)
_cell_angle_beta 87.722(2)
_cell_angle_gamma 77.265(2)
_cell_formula_units_Z 1
_cell_length_a 9.2352(10)
_cell_length_b 11.4330(13)
_cell_length_c 11.7995(13)
_cell_measurement_reflns_used 5041
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.9
_cell_measurement_theta_min 2.2
_cell_volume 1148.6(2)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0340
_diffrn_reflns_av_sigmaI/netI 0.0402
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 13455
_diffrn_reflns_theta_full 26.80
_diffrn_reflns_theta_max 28.27
_diffrn_reflns_theta_min 1.83
_diffrn_standards_decay_% -0.1
_diffrn_standards_number 189
_exptl_absorpt_coefficient_mu 1.016
_exptl_absorpt_correction_T_max 0.970
_exptl_absorpt_correction_T_min 0.752
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.587
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description planar
_exptl_crystal_F_000 570
_exptl_crystal_size_max 0.58
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.379
_refine_diff_density_min -0.301
_refine_diff_density_rms 0.068
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 357
_refine_ls_number_reflns 5183
_refine_ls_number_restraints 13
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0479
_refine_ls_R_factor_gt 0.0419
_refine_ls_shift/su_max 0.075
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1056
_refine_ls_wR_factor_ref 0.1096
_reflns_number_gt 4627
_reflns_number_total 5183
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file cufohax.cif
_cod_data_source_block cufohax
_cod_database_code 1500030
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
Cu Cu 0.35129(3) 0.56166(3) 0.45030(3) 0.02896(10) Uani 1 1 d . . .
O1H O 0.51672(18) 0.43417(16) 0.42743(16) 0.0326(4) Uani 1 1 d D . .
H1H H 0.498(3) 0.3614(14) 0.445(2) 0.039 Uiso 1 1 d D . .
N1P N 0.1701(2) 0.67766(18) 0.48729(18) 0.0300(4) Uani 1 1 d . . .
C1AP C 0.0445(2) 0.6743(2) 0.4339(2) 0.0267(4) Uani 1 1 d . . .
C2P C 0.1581(3) 0.7531(2) 0.5540(2) 0.0359(5) Uani 1 1 d . . .
H2P H 0.2431 0.7548 0.5925 0.043 Uiso 1 1 d R . .
C3P C 0.0235(3) 0.8292(2) 0.5689(2) 0.0403(6) Uani 1 1 d . . .
H3P H 0.0200 0.8821 0.6149 0.048 Uiso 1 1 d R . .
C4P C -0.1030(3) 0.8260(2) 0.5158(2) 0.0397(6) Uani 1 1 d . . .
H4P H -0.1932 0.8767 0.5254 0.048 Uiso 1 1 d R . .
C4AP C -0.0962(3) 0.7454(2) 0.4462(2) 0.0324(5) Uani 1 1 d . . .
C5P C -0.2220(3) 0.7316(3) 0.3894(2) 0.0385(6) Uani 1 1 d . . .
H5P H -0.3159 0.7775 0.3981 0.046 Uiso 1 1 d R . .
C6P C -0.2084(3) 0.6520(3) 0.3242(2) 0.0379(6) Uani 1 1 d . . .
H6P H -0.2926 0.6431 0.2899 0.046 Uiso 1 1 d R . .
C6AP C -0.0656(3) 0.5807(2) 0.3079(2) 0.0310(5) Uani 1 1 d . . .
C7P C -0.0419(3) 0.4970(2) 0.2406(2) 0.0367(6) Uani 1 1 d . . .
H7P H -0.1216 0.4853 0.2029 0.044 Uiso 1 1 d R . .
C8P C 0.0987(3) 0.4331(3) 0.2315(2) 0.0401(6) Uani 1 1 d . . .
H8P H 0.1160 0.3789 0.1859 0.048 Uiso 1 1 d R . .
C9P C 0.2168(3) 0.4500(3) 0.2893(2) 0.0372(6) Uani 1 1 d . . .
H9P H 0.3117 0.4039 0.2836 0.045 Uiso 1 1 d R . .
N10P N 0.1997(2) 0.52765(18) 0.35418(17) 0.0293(4) Uani 1 1 d . . .
C0AP C 0.0602(2) 0.5923(2) 0.3630(2) 0.0269(5) Uani 1 1 d . . .
N1 N -0.0916(3) 0.0504(2) 0.7879(2) 0.0417(5) Uani 1 1 d . . .
N2 N 0.0343(3) -0.0135(2) 0.7616(2) 0.0445(5) Uani 1 1 d . . .
N3 N 0.1538(3) 0.0065(2) 0.8109(2) 0.0406(5) Uani 1 1 d . . .
C3A C 0.0966(3) 0.0867(2) 0.8701(2) 0.0330(5) Uani 1 1 d . . .
N4 N 0.1717(2) 0.1354(2) 0.93570(19) 0.0363(5) Uani 1 1 d . . .
C4 C 0.3328(3) 0.0949(3) 0.9532(3) 0.0532(8) Uani 1 1 d . . .
H41 H 0.3707 0.1558 0.9763 0.064 Uiso 1 1 d R . .
H42 H 0.3764 0.0878 0.8798 0.064 Uiso 1 1 d R . .
H43 H 0.3573 0.0140 1.0151 0.064 Uiso 1 1 d R . .
C5 C 0.0931(3) 0.2163(3) 0.9913(2) 0.0378(6) Uani 1 1 d . . .
O5 O 0.1551(2) 0.2639(2) 1.0489(2) 0.0543(5) Uani 1 1 d . . .
N6 N -0.0611(2) 0.2433(2) 0.97897(19) 0.0375(5) Uani 1 1 d . . .
C6 C -0.1415(4) 0.3244(3) 1.0456(3) 0.0533(8) Uani 1 1 d . . .
H61 H -0.1238 0.2808 1.1300 0.064 Uiso 1 1 d R . .
H62 H -0.2460 0.3435 1.0268 0.064 Uiso 1 1 d R . .
H63 H -0.1067 0.4017 1.0240 0.064 Uiso 1 1 d R . .
C7 C -0.1456(3) 0.1973(2) 0.9139(2) 0.0367(6) Uani 1 1 d . . .
O7 O -0.2815(2) 0.2276(2) 0.91137(18) 0.0520(5) Uani 1 1 d . . .
C7A C -0.0560(3) 0.1163(2) 0.8566(2) 0.0334(5) Uani 1 1 d . . .
O1W O 0.4292(2) 0.71952(19) 0.30232(17) 0.0423(4) Uani 1 1 d D . .
H11W H 0.402(3) 0.7893(17) 0.317(3) 0.051 Uiso 1 1 d D . .
H12W H 0.389(3) 0.726(3) 0.2366(16) 0.051 Uiso 1 1 d D . .
O2W O 0.3477(3) 0.9637(3) 0.3306(2) 0.0662(7) Uani 1 1 d D . .
H21W H 0.274(3) 0.979(4) 0.283(3) 0.079 Uiso 1 1 d D . .
H22W H 0.402(4) 1.011(3) 0.288(3) 0.079 Uiso 1 1 d D . .
O3W O 0.5032(3) 0.1773(2) 0.4461(2) 0.0548(5) Uani 1 1 d D . .
H31W H 0.520(4) 0.150(3) 0.387(2) 0.066 Uiso 1 1 d D . .
H32W H 0.552(3) 0.120(3) 0.506(2) 0.066 Uiso 1 1 d D . .
O4W O 0.5587(3) 0.1152(2) 0.2341(2) 0.0631(6) Uani 1 1 d D . .
H41W H 0.534(4) 0.1878(19) 0.180(3) 0.076 Uiso 1 1 d D . .
H42W H 0.646(2) 0.078(3) 0.223(3) 0.076 Uiso 1 1 d D . .
O5W O 0.4243(3) 0.3450(3) 0.0601(2) 0.0718(7) Uani 1 1 d D . .
H51W H 0.348(3) 0.320(4) 0.046(4) 0.086 Uiso 1 1 d D . .
H52W H 0.480(4) 0.355(4) 0.000(2) 0.086 Uiso 1 1 d D . .
O6W O 0.5868(3) 0.4804(3) 0.1806(2) 0.0731(7) Uani 1 1 d D . .
H61W H 0.561(5) 0.473(4) 0.2524(16) 0.088 Uiso 1 1 d D . .
H62W H 0.553(4) 0.431(3) 0.154(4) 0.088 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 0.02523(16) 0.03288(17) 0.03322(17) -0.01714(12) -0.00309(11) -0.00499(11)
O1H 0.0306(9) 0.0331(9) 0.0390(9) -0.0194(8) -0.0045(7) -0.0041(7)
N1P 0.0293(10) 0.0320(10) 0.0332(10) -0.0153(8) 0.0003(8) -0.0084(8)
C1AP 0.0269(11) 0.0270(11) 0.0275(11) -0.0092(9) 0.0016(8) -0.0078(9)
C2P 0.0374(13) 0.0397(13) 0.0381(13) -0.0198(11) -0.0006(10) -0.0125(11)
C3P 0.0489(15) 0.0363(13) 0.0424(15) -0.0228(11) 0.0049(12) -0.0086(11)
C4P 0.0392(14) 0.0383(14) 0.0433(14) -0.0193(11) 0.0067(11) -0.0036(11)
C4AP 0.0323(12) 0.0310(12) 0.0335(12) -0.0107(10) 0.0036(10) -0.0060(9)
C5P 0.0261(12) 0.0448(14) 0.0426(14) -0.0146(12) 0.0024(10) -0.0033(10)
C6P 0.0278(12) 0.0470(15) 0.0389(14) -0.0115(11) -0.0044(10) -0.0107(11)
C6AP 0.0318(12) 0.0342(12) 0.0288(11) -0.0094(10) -0.0022(9) -0.0120(10)
C7P 0.0375(13) 0.0446(14) 0.0350(13) -0.0168(11) -0.0039(10) -0.0165(11)
C8P 0.0444(15) 0.0459(15) 0.0424(14) -0.0273(12) 0.0009(11) -0.0150(12)
C9P 0.0321(13) 0.0444(14) 0.0416(14) -0.0234(12) 0.0001(10) -0.0067(11)
N10P 0.0284(10) 0.0327(10) 0.0313(10) -0.0155(8) 0.0000(8) -0.0080(8)
C0AP 0.0258(11) 0.0298(11) 0.0263(11) -0.0084(9) 0.0002(8) -0.0094(9)
N1 0.0512(14) 0.0436(13) 0.0356(12) -0.0158(10) -0.0051(10) -0.0154(11)
N2 0.0576(15) 0.0416(13) 0.0399(12) -0.0191(10) -0.0052(11) -0.0120(11)
N3 0.0486(13) 0.0393(12) 0.0372(12) -0.0185(10) -0.0001(10) -0.0068(10)
C3A 0.0404(13) 0.0334(12) 0.0267(11) -0.0107(9) -0.0009(10) -0.0097(10)
N4 0.0344(11) 0.0450(12) 0.0362(11) -0.0210(10) -0.0009(9) -0.0105(9)
C4 0.0358(15) 0.072(2) 0.061(2) -0.0366(17) -0.0064(13) -0.0075(14)
C5 0.0413(14) 0.0453(14) 0.0342(13) -0.0202(11) 0.0026(10) -0.0134(11)
O5 0.0506(12) 0.0740(15) 0.0601(13) -0.0458(12) 0.0037(10) -0.0220(11)
N6 0.0395(12) 0.0446(12) 0.0349(11) -0.0220(10) 0.0031(9) -0.0089(9)
C6 0.0527(18) 0.064(2) 0.0532(18) -0.0372(16) 0.0053(14) -0.0056(15)
C7 0.0387(14) 0.0425(14) 0.0285(12) -0.0103(10) -0.0032(10) -0.0088(11)
O7 0.0366(11) 0.0733(14) 0.0493(12) -0.0284(11) -0.0035(9) -0.0045(10)
C7A 0.0384(13) 0.0365(13) 0.0276(11) -0.0109(10) -0.0026(10) -0.0116(10)
O1W 0.0387(10) 0.0453(11) 0.0413(11) -0.0103(9) -0.0055(8) -0.0104(9)
O2W 0.0688(17) 0.0685(16) 0.0624(16) -0.0125(12) -0.0171(12) -0.0269(13)
O3W 0.0543(13) 0.0542(13) 0.0621(15) -0.0313(11) 0.0005(11) -0.0057(10)
O4W 0.0546(14) 0.0678(16) 0.0663(16) -0.0271(12) 0.0103(12) -0.0052(12)
O5W 0.081(2) 0.0826(18) 0.0635(16) -0.0281(14) 0.0077(13) -0.0360(15)
O6W 0.0849(19) 0.094(2) 0.0565(15) -0.0340(14) 0.0226(14) -0.0420(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu 0.3201 1.2651 '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
O1H Cu O1H 83.69(7) . 2_666 ?
O1H Cu N10P 96.31(7) . . ?
O1H Cu N10P 167.22(8) 2_666 . ?
O1H Cu N1P 173.40(8) . . ?
O1H Cu N1P 96.64(7) 2_666 . ?
N10P Cu N1P 81.91(8) . . ?
O1H Cu O1W 91.65(7) . . ?
O1H Cu O1W 93.71(7) 2_666 . ?
N10P Cu O1W 99.07(7) . . ?
N1P Cu O1W 94.90(8) . . ?
O1H Cu Cu 41.87(5) . 2_666 ?
O1H Cu Cu 41.82(5) 2_666 2_666 ?
N10P Cu Cu 136.77(6) . 2_666 ?
N1P Cu Cu 138.08(6) . 2_666 ?
O1W Cu Cu 93.60(5) . 2_666 ?
Cu O1H Cu 96.31(7) . 2_666 ?
Cu O1H H1H 114(2) . . ?
Cu O1H H1H 110(2) 2_666 . ?
C2P N1P C1AP 117.8(2) . . ?
C2P N1P Cu 130.05(17) . . ?
C1AP N1P Cu 112.19(15) . . ?
N1P C1AP C4AP 123.4(2) . . ?
N1P C1AP C0AP 116.7(2) . . ?
C4AP C1AP C0AP 119.9(2) . . ?
N1P C2P C3P 122.8(2) . . ?
N1P C2P H2P 118.6 . . ?
C3P C2P H2P 118.6 . . ?
C4P C3P C2P 119.7(2) . . ?
C4P C3P H3P 120.0 . . ?
C2P C3P H3P 120.2 . . ?
C3P C4P C4AP 119.5(2) . . ?
C3P C4P H4P 120.1 . . ?
C4AP C4P H4P 120.3 . . ?
C1AP C4AP C4P 116.8(2) . . ?
C1AP C4AP C5P 118.8(2) . . ?
C4P C4AP C5P 124.4(2) . . ?
C6P C5P C4AP 121.6(2) . . ?
C6P C5P H5P 119.1 . . ?
C4AP C5P H5P 119.3 . . ?
C5P C6P C6AP 120.6(2) . . ?
C5P C6P H6P 119.8 . . ?
C6AP C6P H6P 119.6 . . ?
C0AP C6AP C7P 116.9(2) . . ?
C0AP C6AP C6P 119.0(2) . . ?
C7P C6AP C6P 124.1(2) . . ?
C8P C7P C6AP 119.3(2) . . ?
C8P C7P H7P 120.3 . . ?
C6AP C7P H7P 120.4 . . ?
C7P C8P C9P 119.9(2) . . ?
C7P C8P H8P 120.1 . . ?
C9P C8P H8P 119.9 . . ?
N10P C9P C8P 122.8(2) . . ?
N10P C9P H9P 118.6 . . ?
C8P C9P H9P 118.6 . . ?
C9P N10P C0AP 117.6(2) . . ?
C9P N10P Cu 129.75(17) . . ?
C0AP N10P Cu 112.60(15) . . ?
N10P C0AP C6AP 123.4(2) . . ?
N10P C0AP C1AP 116.58(19) . . ?
C6AP C0AP C1AP 120.0(2) . . ?
N2 N1 C7A 106.7(2) . . ?
N1 N2 N3 111.9(2) . . ?
C3A N3 N2 105.1(2) . . ?
N3 C3A N4 127.7(2) . . ?
N3 C3A C7A 109.5(2) . . ?
N4 C3A C7A 122.8(2) . . ?
C5 N4 C3A 119.3(2) . . ?
C5 N4 C4 120.0(2) . . ?
C3A N4 C4 120.5(2) . . ?
N4 C4 H41 109.6 . . ?
N4 C4 H42 109.5 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.3 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 121.7(2) . . ?
O5 C5 N6 121.1(2) . . ?
N4 C5 N6 117.2(2) . . ?
C5 N6 C7 126.8(2) . . ?
C5 N6 C6 115.5(2) . . ?
C7 N6 C6 117.6(2) . . ?
N6 C6 H61 109.2 . . ?
N6 C6 H62 109.7 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.4 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 120.2(2) . . ?
O7 C7 C7A 127.2(3) . . ?
N6 C7 C7A 112.6(2) . . ?
N1 C7A C3A 106.9(2) . . ?
N1 C7A C7 131.9(2) . . ?
C3A C7A C7 121.2(2) . . ?
Cu O1W H11W 110(2) . . ?
Cu O1W H12W 108(2) . . ?
H11W O1W H12W 109(3) . . ?
H21W O2W H22W 102(4) . . ?
H31W O3W H32W 106(3) . . ?
H41W O4W H42W 110(4) . . ?
H51W O5W H52W 110(4) . . ?
H61W O6W H62W 112(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
Cu O1H 1.9423(17) . ?
Cu O1H 1.9442(17) 2_666 ?
Cu N10P 2.0125(19) . ?
Cu N1P 2.022(2) . ?
Cu O1W 2.291(2) . ?
Cu Cu 2.8952(6) 2_666 ?
O1H Cu 1.9442(16) 2_666 ?
O1H H1H 0.844(10) . ?
N1P C2P 1.329(3) . ?
N1P C1AP 1.356(3) . ?
C1AP C4AP 1.402(3) . ?
C1AP C0AP 1.429(3) . ?
C2P C3P 1.392(4) . ?
C2P H2P 0.9300 . ?
C3P C4P 1.361(4) . ?
C3P H3P 0.9300 . ?
C4P C4AP 1.411(3) . ?
C4P H4P 0.9300 . ?
C4AP C5P 1.426(4) . ?
C5P C6P 1.354(4) . ?
C5P H5P 0.9300 . ?
C6P C6AP 1.431(4) . ?
C6P H6P 0.9300 . ?
C6AP C0AP 1.405(3) . ?
C6AP C7P 1.409(3) . ?
C7P C8P 1.361(4) . ?
C7P H7P 0.9300 . ?
C8P C9P 1.390(3) . ?
C8P H8P 0.9300 . ?
C9P N10P 1.330(3) . ?
C9P H9P 0.9300 . ?
N10P C0AP 1.355(3) . ?
N1 N2 1.314(3) . ?
N1 C7A 1.364(3) . ?
N2 N3 1.363(3) . ?
N3 C3A 1.334(3) . ?
C3A N4 1.372(3) . ?
C3A C7A 1.378(3) . ?
N4 C5 1.369(3) . ?
N4 C4 1.459(3) . ?
C4 H41 0.9601 . ?
C4 H42 0.9601 . ?
C4 H43 0.9601 . ?
C5 O5 1.222(3) . ?
C5 N6 1.393(3) . ?
N6 C7 1.401(3) . ?
N6 C6 1.468(3) . ?
C6 H61 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C7 O7 1.225(3) . ?
C7 C7A 1.423(4) . ?
O1W H11W 0.852(10) . ?
O1W H12W 0.844(10) . ?
O2W H21W 0.852(10) . ?
O2W H22W 0.850(10) . ?
O3W H31W 0.850(10) . ?
O3W H32W 0.851(10) . ?
O4W H41W 0.854(10) . ?
O4W H42W 0.854(10) . ?
O5W H51W 0.860(10) . ?
O5W H52W 0.856(10) . ?
O6W H61W 0.855(10) . ?
O6W H62W 0.852(10) . ?
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
O1H H1H O3W 0.844(10) 2.091(13) 2.903(3) 161(3) .
O1W H11W O2W 0.852(10) 2.004(11) 2.851(3) 173(3) .
O1W H12W O7 0.844(10) 1.905(12) 2.739(3) 169(3) 2_566
O2W H21W N1 0.852(10) 2.048(18) 2.855(3) 158(4) 2_566
O2W H22W O4W 0.850(10) 2.025(16) 2.850(4) 163(4) 1_565
O3W H31W O4W 0.850(10) 1.971(12) 2.813(3) 171(3) .
O3W H32W O2W 0.851(10) 2.012(16) 2.826(3) 160(4) 2_666
O4W H41W O5W 0.854(10) 1.980(15) 2.814(4) 165(4) .
O4W H42W N3 0.854(10) 1.977(11) 2.830(3) 177(4) 2_656
O5W H51W O5 0.860(10) 2.014(14) 2.861(3) 168(4) 1_554
O5W H52W O6W 0.856(10) 2.33(4) 2.882(4) 123(3) 2_665
O6W H61W O1H 0.855(10) 2.011(12) 2.860(3) 172(4) .
O6W H62W O5W 0.852(10) 2.215(15) 3.049(4) 166(4) .
|
1500031.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500031.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_1500031
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C10 H18 Mn N2 O4 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum 'C22 H30 Mn N12 O8'
_chemical_formula_weight 645.52
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 89.138(1)
_cell_angle_beta 88.455(1)
_cell_angle_gamma 64.069(1)
_cell_formula_units_Z 1
_cell_length_a 8.4735(6)
_cell_length_b 9.1517(7)
_cell_length_c 10.2500(8)
_cell_measurement_reflns_used 4489
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.0
_cell_measurement_theta_min 2.5
_cell_volume 714.57(9)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0181
_diffrn_reflns_av_sigmaI/netI 0.0216
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 8332
_diffrn_reflns_theta_full 26.70
_diffrn_reflns_theta_max 28.27
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% -0.3
_diffrn_standards_number 195
_exptl_absorpt_coefficient_mu 0.530
_exptl_absorpt_correction_T_max 0.897
_exptl_absorpt_correction_T_min 0.789
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.500
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 335
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.21
_refine_diff_density_max 0.205
_refine_diff_density_min -0.234
_refine_diff_density_rms 0.067
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3227
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.010
_refine_ls_R_factor_all 0.0379
_refine_ls_R_factor_gt 0.0354
_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^)+(0.0600P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0985
_refine_ls_wR_factor_ref 0.1007
_reflns_number_gt 2992
_reflns_number_total 3227
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound1.cif
_cod_data_source_block mnaxpyr
_cod_database_code 1500031
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
Mn Mn 0.5000 0.5000 0.5000 0.03844(12) Uani 1 2 d S . .
O1W O 0.53474(16) 0.46962(17) 0.28773(11) 0.0508(3) Uani 1 1 d D . .
H11W H 0.489(3) 0.430(2) 0.2358(17) 0.061 Uiso 1 1 d D . .
H12W H 0.6323(17) 0.455(3) 0.2544(19) 0.061 Uiso 1 1 d D . .
O2W O 0.27399(16) 0.45179(18) 0.48530(11) 0.0518(3) Uani 1 1 d D . .
H21W H 0.203(2) 0.462(3) 0.5468(16) 0.062 Uiso 1 1 d D . .
H22W H 0.214(2) 0.473(3) 0.4181(14) 0.062 Uiso 1 1 d D . .
N1P N 0.33319(19) 0.77191(17) 0.46889(14) 0.0489(3) Uani 1 1 d . . .
C2P C 0.2180(3) 0.8268(2) 0.37300(18) 0.0554(4) Uani 1 1 d . . .
H2P H 0.2022 0.7512 0.3211 0.066 Uiso 1 1 d R . .
C3P C 0.1211(3) 0.9892(3) 0.3463(2) 0.0641(5) Uani 1 1 d . . .
H3P H 0.0420 1.0237 0.2778 0.077 Uiso 1 1 d R . .
C4P C 0.1420(3) 1.1010(2) 0.4225(2) 0.0662(5) Uani 1 1 d . . .
H4P H 0.0783 1.2131 0.4071 0.079 Uiso 1 1 d R . .
C5P C 0.2581(3) 1.0467(3) 0.5229(2) 0.0720(6) Uani 1 1 d . . .
H5P H 0.2750 1.1198 0.5770 0.086 Uiso 1 1 d R . .
C6P C 0.3503(3) 0.8828(2) 0.5427(2) 0.0630(5) Uani 1 1 d . . .
H6P H 0.4293 0.8458 0.6113 0.076 Uiso 1 1 d R . .
N1 N 0.09437(18) 0.46973(18) 0.25839(13) 0.0450(3) Uani 1 1 d . . .
N2 N -0.06811(18) 0.49837(19) 0.29063(13) 0.0475(3) Uani 1 1 d . . .
N3 N -0.13427(17) 0.42694(18) 0.20577(13) 0.0450(3) Uani 1 1 d . . .
C3A C -0.00586(19) 0.35201(19) 0.11911(14) 0.0384(3) Uani 1 1 d . . .
N4 N -0.00655(18) 0.26053(18) 0.01459(13) 0.0443(3) Uani 1 1 d . . .
C4 C -0.1630(2) 0.2379(3) -0.01247(19) 0.0583(5) Uani 1 1 d . . .
H41 H -0.2007 0.2007 0.0652 0.070 Uiso 1 1 d R . .
H42 H -0.1349 0.1573 -0.0797 0.070 Uiso 1 1 d R . .
H43 H -0.2563 0.3399 -0.0413 0.070 Uiso 1 1 d R . .
C5 C 0.1391(2) 0.1930(2) -0.06580(15) 0.0447(4) Uani 1 1 d . . .
O5 O 0.14681(19) 0.11009(18) -0.15883(13) 0.0632(4) Uani 1 1 d . . .
N6 N 0.28360(17) 0.22313(17) -0.03495(13) 0.0447(3) Uani 1 1 d . . .
C6 C 0.4334(3) 0.1579(3) -0.12698(19) 0.0603(5) Uani 1 1 d . . .
H61 H 0.4064 0.2273 -0.2032 0.072 Uiso 1 1 d R . .
H62 H 0.4559 0.0487 -0.1520 0.072 Uiso 1 1 d R . .
H63 H 0.5363 0.1550 -0.0864 0.072 Uiso 1 1 d R . .
C7 C 0.2949(2) 0.3118(2) 0.07121(16) 0.0443(3) Uani 1 1 d . . .
O7 O 0.42889(17) 0.32730(19) 0.08983(14) 0.0641(4) Uani 1 1 d . . .
C7A C 0.1377(2) 0.37698(19) 0.14934(14) 0.0396(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn 0.03403(18) 0.0474(2) 0.03647(19) -0.00574(13) -0.00270(12) -0.01995(14)
O1W 0.0453(6) 0.0758(8) 0.0397(6) -0.0131(6) 0.0028(5) -0.0339(6)
O2W 0.0436(6) 0.0844(9) 0.0380(6) -0.0094(6) -0.0011(5) -0.0376(6)
N1P 0.0483(8) 0.0481(8) 0.0488(8) -0.0055(6) -0.0069(6) -0.0193(6)
C2P 0.0607(11) 0.0542(10) 0.0485(9) -0.0059(8) -0.0104(8) -0.0219(8)
C3P 0.0707(13) 0.0620(11) 0.0527(10) 0.0068(9) -0.0146(9) -0.0222(10)
C4P 0.0754(13) 0.0471(10) 0.0695(13) 0.0053(9) -0.0029(10) -0.0210(9)
C5P 0.0888(16) 0.0546(11) 0.0784(14) -0.0079(10) -0.0143(12) -0.0359(11)
C6P 0.0677(12) 0.0583(11) 0.0660(12) -0.0044(9) -0.0213(10) -0.0291(9)
N1 0.0449(7) 0.0581(8) 0.0372(7) -0.0059(6) -0.0019(5) -0.0271(6)
N2 0.0443(7) 0.0635(9) 0.0376(7) -0.0061(6) -0.0010(5) -0.0260(7)
N3 0.0398(7) 0.0620(8) 0.0375(7) -0.0031(6) -0.0022(5) -0.0260(6)
C3A 0.0392(7) 0.0493(8) 0.0312(7) 0.0018(6) -0.0054(5) -0.0232(6)
N4 0.0437(7) 0.0585(8) 0.0392(7) -0.0061(6) -0.0039(5) -0.0298(6)
C4 0.0531(10) 0.0794(13) 0.0574(10) -0.0102(9) -0.0064(8) -0.0424(10)
C5 0.0504(9) 0.0501(9) 0.0389(8) -0.0031(6) -0.0022(6) -0.0268(7)
O5 0.0712(9) 0.0759(9) 0.0542(7) -0.0236(7) 0.0056(6) -0.0427(7)
N6 0.0421(7) 0.0548(8) 0.0401(7) -0.0065(6) 0.0031(5) -0.0240(6)
C6 0.0523(10) 0.0738(12) 0.0540(10) -0.0150(9) 0.0136(8) -0.0272(9)
C7 0.0409(8) 0.0545(9) 0.0424(8) -0.0032(7) -0.0024(6) -0.0251(7)
O7 0.0452(7) 0.0960(10) 0.0629(8) -0.0256(7) 0.0064(6) -0.0415(7)
C7A 0.0396(7) 0.0513(8) 0.0332(7) -0.0010(6) -0.0036(6) -0.0245(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
O2W Mn O2W 180.0 2_666 . ?
O2W Mn O1W 92.29(4) 2_666 . ?
O2W Mn O1W 87.71(4) . . ?
O2W Mn O1W 87.71(4) 2_666 2_666 ?
O2W Mn O1W 92.29(4) . 2_666 ?
O1W Mn O1W 180.00(8) . 2_666 ?
O2W Mn N1P 88.42(5) 2_666 . ?
O2W Mn N1P 91.58(5) . . ?
O1W Mn N1P 89.10(5) . . ?
O1W Mn N1P 90.90(5) 2_666 . ?
O2W Mn N1P 91.58(5) 2_666 2_666 ?
O2W Mn N1P 88.42(5) . 2_666 ?
O1W Mn N1P 90.90(5) . 2_666 ?
O1W Mn N1P 89.10(5) 2_666 2_666 ?
N1P Mn N1P 180.0 . 2_666 ?
Mn O1W H11W 129.9(15) . . ?
Mn O1W H12W 117.7(15) . . ?
H11W O1W H12W 107(2) . . ?
Mn O2W H21W 124.4(15) . . ?
Mn O2W H22W 122.3(15) . . ?
H21W O2W H22W 105(2) . . ?
C2P N1P C6P 117.05(16) . . ?
C2P N1P Mn 121.18(12) . . ?
C6P N1P Mn 121.73(12) . . ?
N1P C2P C3P 123.31(17) . . ?
N1P C2P H2P 118.5 . . ?
C3P C2P H2P 118.2 . . ?
C4P C3P C2P 118.69(19) . . ?
C4P C3P H3P 120.1 . . ?
C2P C3P H3P 121.2 . . ?
C3P C4P C5P 118.80(19) . . ?
C3P C4P H4P 121.2 . . ?
C5P C4P H4P 120.0 . . ?
C6P C5P C4P 118.94(19) . . ?
C6P C5P H5P 120.1 . . ?
C4P C5P H5P 121.0 . . ?
N1P C6P C5P 123.20(18) . . ?
N1P C6P H6P 117.8 . . ?
C5P C6P H6P 119.0 . . ?
N2 N1 C7A 106.53(12) . . ?
N1 N2 N3 111.64(13) . . ?
C3A N3 N2 105.18(12) . . ?
N3 C3A N4 127.79(14) . . ?
N3 C3A C7A 109.52(13) . . ?
N4 C3A C7A 122.68(14) . . ?
C5 N4 C3A 119.59(13) . . ?
C5 N4 C4 120.19(14) . . ?
C3A N4 C4 120.21(14) . . ?
N4 C4 H41 109.6 . . ?
N4 C4 H42 109.1 . . ?
H41 C4 H42 109.0 . . ?
N4 C4 H43 109.8 . . ?
H41 C4 H43 109.7 . . ?
H42 C4 H43 109.7 . . ?
O5 C5 N4 122.60(15) . . ?
O5 C5 N6 120.52(15) . . ?
N4 C5 N6 116.88(13) . . ?
C7 N6 C5 126.60(13) . . ?
C7 N6 C6 117.67(14) . . ?
C5 N6 C6 115.70(14) . . ?
N6 C6 H61 108.8 . . ?
N6 C6 H62 109.8 . . ?
H61 C6 H62 109.9 . . ?
N6 C6 H63 109.6 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.2 . . ?
O7 C7 N6 120.92(15) . . ?
O7 C7 C7A 126.57(15) . . ?
N6 C7 C7A 112.51(13) . . ?
N1 C7A C3A 107.13(13) . . ?
N1 C7A C7 131.17(14) . . ?
C3A C7A C7 121.70(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn O2W 2.1543(11) 2_666 ?
Mn O2W 2.1544(11) . ?
Mn O1W 2.1932(11) . ?
Mn O1W 2.1932(11) 2_666 ?
Mn N1P 2.2839(14) . ?
Mn N1P 2.2839(14) 2_666 ?
O1W H11W 0.837(9) . ?
O1W H12W 0.842(9) . ?
O2W H21W 0.836(9) . ?
O2W H22W 0.836(9) . ?
N1P C2P 1.334(2) . ?
N1P C6P 1.335(2) . ?
C2P C3P 1.375(3) . ?
C2P H2P 0.9352 . ?
C3P C4P 1.371(3) . ?
C3P H3P 0.9360 . ?
C4P C5P 1.373(3) . ?
C4P H4P 0.9403 . ?
C5P C6P 1.370(3) . ?
C5P H5P 0.9349 . ?
C6P H6P 0.9361 . ?
N1 N2 1.3175(19) . ?
N1 C7A 1.356(2) . ?
N2 N3 1.3646(18) . ?
N3 C3A 1.325(2) . ?
C3A N4 1.3713(19) . ?
C3A C7A 1.376(2) . ?
N4 C5 1.370(2) . ?
N4 C4 1.463(2) . ?
C4 H41 0.9617 . ?
C4 H42 0.9633 . ?
C4 H43 0.9704 . ?
C5 O5 1.210(2) . ?
C5 N6 1.412(2) . ?
N6 C7 1.397(2) . ?
N6 C6 1.465(2) . ?
C6 H61 0.9666 . ?
C6 H62 0.9687 . ?
C6 H63 0.9666 . ?
C7 O7 1.2243(19) . ?
C7 C7A 1.426(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O7 0.837(9) 1.973(11) 2.7955(17) 167(2) .
O1W H12W N3 0.842(9) 1.931(10) 2.7658(18) 171(2) 1_655
O2W H21W N2 0.836(9) 1.942(11) 2.7651(18) 168(2) 2_566
O2W H22W N1 0.836(9) 1.957(11) 2.7774(17) 167(2) .
|
1500032.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500032.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_1500032
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C10 H18 Co N2 O4 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum 'C22 H30 Co N12 O8'
_chemical_formula_weight 649.51
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 89.034(1)
_cell_angle_beta 88.769(1)
_cell_angle_gamma 63.924(1)
_cell_formula_units_Z 1
_cell_length_a 8.4326(5)
_cell_length_b 9.0674(5)
_cell_length_c 10.2434(6)
_cell_measurement_reflns_used 5738
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.8
_cell_measurement_theta_min 2.5
_cell_volume 703.32(7)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0134
_diffrn_reflns_av_sigmaI/netI 0.0164
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 8043
_diffrn_reflns_theta_full 26.70
_diffrn_reflns_theta_max 28.04
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% 0.1
_diffrn_standards_number 235
_exptl_absorpt_coefficient_mu 0.679
_exptl_absorpt_correction_T_max 0.854
_exptl_absorpt_correction_T_min 0.759
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.533
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 337
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.24
_refine_diff_density_max 0.300
_refine_diff_density_min -0.216
_refine_diff_density_rms 0.053
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.156
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3145
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.155
_refine_ls_R_factor_all 0.0330
_refine_ls_R_factor_gt 0.0316
_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^)+(0.0500P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0885
_refine_ls_wR_factor_ref 0.0895
_reflns_number_gt 2977
_reflns_number_total 3145
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound2.cif
_cod_data_source_block coaxpyr
_cod_database_code 1500032
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
Co Co 0.5000 0.5000 0.5000 0.03688(11) Uani 1 2 d S . .
O1W O 0.53182(15) 0.47440(16) 0.29338(11) 0.0478(3) Uani 1 1 d D . .
H11W H 0.486(2) 0.432(2) 0.2446(17) 0.057 Uiso 1 1 d D . .
H12W H 0.6293(17) 0.458(3) 0.2593(19) 0.057 Uiso 1 1 d D . .
O2W O 0.28134(15) 0.45295(17) 0.48566(11) 0.0499(3) Uani 1 1 d D . .
H21W H 0.208(2) 0.464(3) 0.5453(16) 0.060 Uiso 1 1 d D . .
H22W H 0.219(2) 0.473(2) 0.4195(14) 0.060 Uiso 1 1 d D . .
N1P N 0.34029(17) 0.76008(17) 0.47124(13) 0.0458(3) Uani 1 1 d . . .
C2P C 0.2232(2) 0.8172(2) 0.37471(17) 0.0521(4) Uani 1 1 d . . .
H2P H 0.2075 0.7416 0.3228 0.062 Uiso 1 1 d R . .
C3P C 0.1258(3) 0.9815(3) 0.34871(19) 0.0620(5) Uani 1 1 d . . .
H3P H 0.0467 1.0161 0.2802 0.074 Uiso 1 1 d R . .
C4P C 0.1473(3) 1.0937(2) 0.4257(2) 0.0643(5) Uani 1 1 d . . .
H4P H 0.0836 1.2058 0.4104 0.077 Uiso 1 1 d R . .
C5P C 0.2653(3) 1.0371(3) 0.5266(2) 0.0671(5) Uani 1 1 d . . .
H5P H 0.2822 1.1101 0.5807 0.081 Uiso 1 1 d R . .
C6P C 0.3578(3) 0.8717(2) 0.54583(19) 0.0579(4) Uani 1 1 d . . .
H6P H 0.4368 0.8346 0.6144 0.070 Uiso 1 1 d R . .
N1 N 0.09515(17) 0.46763(18) 0.26240(12) 0.0445(3) Uani 1 1 d . . .
N2 N -0.06761(18) 0.49571(19) 0.29453(13) 0.0474(3) Uani 1 1 d . . .
N3 N -0.13476(17) 0.42483(18) 0.20879(12) 0.0450(3) Uani 1 1 d . . .
C3A C -0.00651(19) 0.35074(19) 0.12148(13) 0.0382(3) Uani 1 1 d . . .
N4 N -0.00827(17) 0.26075(17) 0.01593(12) 0.0433(3) Uani 1 1 d . . .
C4 C -0.1654(2) 0.2381(3) -0.01186(19) 0.0568(4) Uani 1 1 d . . .
H41 H -0.1987 0.1943 0.0642 0.068 Uiso 1 1 d R . .
H42 H -0.1394 0.1627 -0.0829 0.068 Uiso 1 1 d R . .
H43 H -0.2608 0.3415 -0.0353 0.068 Uiso 1 1 d R . .
C5 C 0.1377(2) 0.1949(2) -0.06495(15) 0.0438(3) Uani 1 1 d . . .
O5 O 0.14401(19) 0.11320(18) -0.15917(13) 0.0618(3) Uani 1 1 d . . .
N6 N 0.28272(17) 0.22493(17) -0.03329(13) 0.0437(3) Uani 1 1 d . . .
C6 C 0.4331(2) 0.1601(3) -0.12557(18) 0.0585(4) Uani 1 1 d . . .
H61 H 0.4093 0.2334 -0.1991 0.070 Uiso 1 1 d R . .
H62 H 0.4506 0.0539 -0.1549 0.070 Uiso 1 1 d R . .
H63 H 0.5376 0.1506 -0.0831 0.070 Uiso 1 1 d R . .
C7 C 0.2955(2) 0.3111(2) 0.07425(15) 0.0434(3) Uani 1 1 d . . .
O7 O 0.43031(16) 0.32611(19) 0.09410(13) 0.0630(4) Uani 1 1 d . . .
C7A C 0.13765(19) 0.37599(19) 0.15241(14) 0.0393(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.03249(15) 0.04962(18) 0.03200(15) -0.00737(11) -0.00086(10) -0.02098(12)
O1W 0.0426(6) 0.0726(8) 0.0364(6) -0.0130(5) 0.0039(4) -0.0326(6)
O2W 0.0411(6) 0.0835(8) 0.0359(6) -0.0098(5) 0.0004(4) -0.0370(6)
N1P 0.0444(7) 0.0515(7) 0.0417(7) -0.0072(5) -0.0037(5) -0.0209(6)
C2P 0.0552(10) 0.0564(9) 0.0438(8) -0.0068(7) -0.0072(7) -0.0233(8)
C3P 0.0646(11) 0.0633(11) 0.0516(10) 0.0043(8) -0.0116(8) -0.0218(9)
C4P 0.0724(13) 0.0509(10) 0.0642(12) 0.0023(8) -0.0012(9) -0.0222(9)
C5P 0.0817(14) 0.0570(11) 0.0681(12) -0.0103(9) -0.0073(10) -0.0349(10)
C6P 0.0618(11) 0.0594(10) 0.0557(10) -0.0080(8) -0.0132(8) -0.0286(9)
N1 0.0431(7) 0.0600(8) 0.0356(6) -0.0069(5) 0.0004(5) -0.0273(6)
N2 0.0430(7) 0.0652(8) 0.0366(6) -0.0084(6) 0.0017(5) -0.0262(6)
N3 0.0380(6) 0.0644(8) 0.0366(6) -0.0047(6) 0.0004(5) -0.0260(6)
C3A 0.0375(7) 0.0512(8) 0.0304(6) 0.0004(6) -0.0034(5) -0.0235(6)
N4 0.0412(7) 0.0601(8) 0.0372(6) -0.0068(5) -0.0013(5) -0.0300(6)
C4 0.0502(9) 0.0793(12) 0.0557(10) -0.0101(9) -0.0052(8) -0.0416(9)
C5 0.0481(8) 0.0523(8) 0.0368(7) -0.0042(6) -0.0007(6) -0.0272(7)
O5 0.0678(8) 0.0777(9) 0.0512(7) -0.0246(6) 0.0074(6) -0.0418(7)
N6 0.0397(7) 0.0546(7) 0.0393(6) -0.0077(5) 0.0042(5) -0.0230(6)
C6 0.0497(10) 0.0739(12) 0.0522(10) -0.0154(8) 0.0142(8) -0.0277(9)
C7 0.0389(7) 0.0562(9) 0.0400(7) -0.0048(6) 0.0002(6) -0.0254(7)
O7 0.0431(6) 0.0969(10) 0.0616(8) -0.0265(7) 0.0083(5) -0.0417(7)
C7A 0.0379(7) 0.0522(8) 0.0330(7) -0.0027(6) -0.0019(5) -0.0244(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2W Co O2W 180.0 . 2_666 ?
O2W Co O1W 91.97(4) . 2_666 ?
O2W Co O1W 88.03(4) 2_666 2_666 ?
O2W Co O1W 88.03(4) . . ?
O2W Co O1W 91.97(4) 2_666 . ?
O1W Co O1W 179.999(1) 2_666 . ?
O2W Co N1P 88.39(5) . 2_666 ?
O2W Co N1P 91.61(5) 2_666 2_666 ?
O1W Co N1P 88.67(5) 2_666 2_666 ?
O1W Co N1P 91.33(5) . 2_666 ?
O2W Co N1P 91.61(5) . . ?
O2W Co N1P 88.39(5) 2_666 . ?
O1W Co N1P 91.33(5) 2_666 . ?
O1W Co N1P 88.67(5) . . ?
N1P Co N1P 179.999(1) 2_666 . ?
Co O1W H11W 127.0(15) . . ?
Co O1W H12W 118.7(14) . . ?
H11W O1W H12W 107(2) . . ?
Co O2W H21W 125.6(15) . . ?
Co O2W H22W 123.9(14) . . ?
H21W O2W H22W 102(2) . . ?
C6P N1P C2P 116.93(15) . . ?
C6P N1P Co 121.68(12) . . ?
C2P N1P Co 121.35(11) . . ?
N1P C2P C3P 123.23(16) . . ?
N1P C2P H2P 118.2 . . ?
C3P C2P H2P 118.5 . . ?
C2P C3P C4P 118.79(18) . . ?
C2P C3P H3P 120.5 . . ?
C4P C3P H3P 120.7 . . ?
C3P C4P C5P 118.72(18) . . ?
C3P C4P H4P 120.8 . . ?
C5P C4P H4P 120.4 . . ?
C6P C5P C4P 118.99(18) . . ?
C6P C5P H5P 120.3 . . ?
C4P C5P H5P 120.7 . . ?
N1P C6P C5P 123.32(17) . . ?
N1P C6P H6P 118.3 . . ?
C5P C6P H6P 118.4 . . ?
N2 N1 C7A 106.48(12) . . ?
N1 N2 N3 111.65(12) . . ?
C3A N3 N2 105.25(12) . . ?
N3 C3A N4 127.85(13) . . ?
N3 C3A C7A 109.32(13) . . ?
N4 C3A C7A 122.82(13) . . ?
C3A N4 C5 119.34(12) . . ?
C3A N4 C4 120.31(13) . . ?
C5 N4 C4 120.34(13) . . ?
N4 C4 H41 109.5 . . ?
N4 C4 H42 109.1 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.8 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 122.20(14) . . ?
O5 C5 N6 120.77(15) . . ?
N4 C5 N6 117.03(13) . . ?
C7 N6 C5 126.68(13) . . ?
C7 N6 C6 117.67(13) . . ?
C5 N6 C6 115.65(13) . . ?
N6 C6 H61 109.4 . . ?
N6 C6 H62 109.4 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.6 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.14(14) . . ?
O7 C7 C7A 126.41(15) . . ?
N6 C7 C7A 112.44(13) . . ?
N1 C7A C3A 107.30(13) . . ?
N1 C7A C7 131.06(13) . . ?
C3A C7A C7 121.64(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co O2W 2.0757(11) . ?
Co O2W 2.0758(11) 2_666 ?
Co O1W 2.1314(11) 2_666 ?
Co O1W 2.1314(11) . ?
Co N1P 2.1595(14) 2_666 ?
Co N1P 2.1595(14) . ?
O1W H11W 0.833(9) . ?
O1W H12W 0.839(9) . ?
O2W H21W 0.834(9) . ?
O2W H22W 0.831(9) . ?
N1P C6P 1.339(2) . ?
N1P C2P 1.340(2) . ?
C2P C3P 1.373(3) . ?
C2P H2P 0.9300 . ?
C3P C4P 1.373(3) . ?
C3P H3P 0.9300 . ?
C4P C5P 1.377(3) . ?
C4P H4P 0.9300 . ?
C5P C6P 1.366(3) . ?
C5P H5P 0.9300 . ?
C6P H6P 0.9300 . ?
N1 N2 1.3165(18) . ?
N1 C7A 1.3567(19) . ?
N2 N3 1.3657(18) . ?
N3 C3A 1.327(2) . ?
C3A N4 1.3697(19) . ?
C3A C7A 1.3763(19) . ?
N4 C5 1.373(2) . ?
N4 C4 1.4620(19) . ?
C4 H41 0.9601 . ?
C4 H42 0.9601 . ?
C4 H43 0.9601 . ?
C5 O5 1.2124(19) . ?
C5 N6 1.410(2) . ?
N6 C7 1.394(2) . ?
N6 C6 1.470(2) . ?
C6 H61 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C7 O7 1.2241(19) . ?
C7 C7A 1.429(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O7 0.833(9) 1.998(11) 2.8084(16) 164(2) .
O1W H12W N3 0.839(9) 1.936(10) 2.7669(17) 171(2) 1_655
O2W H21W N2 0.834(9) 1.946(11) 2.7674(17) 168(2) 2_566
O2W H22W N1 0.831(9) 1.954(11) 2.7701(17) 167(2) .
|
1500033.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500033.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_1500033
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C22 H26 N12 Ni O6, 2 (H2 O)'
_chemical_formula_sum 'C22 H30 N12 Ni O8'
_chemical_formula_weight 649.29
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 83.422(1)
_cell_angle_beta 69.440(1)
_cell_angle_gamma 61.375(1)
_cell_formula_units_Z 1
_cell_length_a 8.4471(4)
_cell_length_b 8.6061(4)
_cell_length_c 11.4137(6)
_cell_measurement_reflns_used 6266
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.1
_cell_measurement_theta_min 2.7
_cell_volume 680.47(6)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0190
_diffrn_reflns_av_sigmaI/netI 0.0195
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 7924
_diffrn_reflns_theta_full 26.80
_diffrn_reflns_theta_max 28.10
_diffrn_reflns_theta_min 1.91
_diffrn_standards_decay_% 0.0
_diffrn_standards_number 235
_exptl_absorpt_coefficient_mu 0.784
_exptl_absorpt_correction_T_max 0.859
_exptl_absorpt_correction_T_min 0.743
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.584
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 338
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.537
_refine_diff_density_min -0.384
_refine_diff_density_rms 0.066
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.147
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3077
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.147
_refine_ls_R_factor_all 0.0287
_refine_ls_R_factor_gt 0.0284
_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^)+(0.0400P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0772
_refine_ls_wR_factor_ref 0.0773
_reflns_number_gt 3020
_reflns_number_total 3077
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound3.cif
_cod_data_source_block niaxpyr
_cod_database_code 1500033
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.5000 0.5000 0.5000 0.01093(9) Uani 1 2 d S . .
N1 N 0.83659(17) 0.41187(16) 0.27434(11) 0.0153(2) Uani 1 1 d . . .
N2 N 0.66164(17) 0.42992(16) 0.31259(11) 0.0138(2) Uani 1 1 d . . .
N3 N 0.62022(17) 0.37901(16) 0.22333(11) 0.0151(2) Uani 1 1 d . . .
C3A C 0.7825(2) 0.32516(18) 0.12444(13) 0.0144(3) Uani 1 1 d . . .
N4 N 0.81997(18) 0.25761(17) 0.00842(11) 0.0167(2) Uani 1 1 d . . .
C4 C 0.6714(2) 0.2479(2) -0.02346(15) 0.0222(3) Uani 1 1 d . . .
H41 H 0.6344 0.3342 -0.0853 0.027 Uiso 1 1 d R . .
H42 H 0.5591 0.2744 0.0522 0.027 Uiso 1 1 d R . .
H43 H 0.7216 0.1281 -0.0588 0.027 Uiso 1 1 d R . .
C5 C 0.9973(2) 0.20715(19) -0.08081(13) 0.0176(3) Uani 1 1 d . . .
O5 O 1.03566(16) 0.14882(15) -0.18611(10) 0.0230(2) Uani 1 1 d . . .
N6 N 1.13390(18) 0.22448(18) -0.04868(12) 0.0188(3) Uani 1 1 d . . .
C6 C 1.3237(2) 0.1663(2) -0.14685(15) 0.0272(4) Uani 1 1 d . . .
H61 H 1.3755 0.0433 -0.1764 0.033 Uiso 1 1 d R . .
H62 H 1.4109 0.1744 -0.1124 0.033 Uiso 1 1 d R . .
H63 H 1.3106 0.2429 -0.2171 0.033 Uiso 1 1 d R . .
C7 C 1.1054(2) 0.2976(2) 0.06587(14) 0.0177(3) Uani 1 1 d . . .
O7 O 1.23137(16) 0.31511(17) 0.08280(11) 0.0253(3) Uani 1 1 d . . .
C7A C 0.9173(2) 0.34490(19) 0.15360(13) 0.0150(3) Uani 1 1 d . . .
N1P N 0.35328(16) 0.76517(15) 0.46105(11) 0.0130(2) Uani 1 1 d . . .
C2P C 0.2748(2) 0.81106(19) 0.37042(13) 0.0154(3) Uani 1 1 d . . .
H2P H 0.2860 0.7200 0.3233 0.018 Uiso 1 1 d R . .
C3P C 0.1784(2) 0.9855(2) 0.34263(14) 0.0182(3) Uani 1 1 d . . .
H3P H 0.1215 1.0137 0.2794 0.022 Uiso 1 1 d R . .
C4P C 0.1664(2) 1.1182(2) 0.40875(14) 0.0197(3) Uani 1 1 d . . .
H4P H 0.1036 1.2388 0.3905 0.024 Uiso 1 1 d R . .
C5P C 0.2475(2) 1.07200(19) 0.50233(14) 0.0185(3) Uani 1 1 d . . .
H5P H 0.2418 1.1603 0.5490 0.022 Uiso 1 1 d R . .
C6P C 0.3372(2) 0.89487(19) 0.52668(13) 0.0160(3) Uani 1 1 d . . .
H6P H 0.3892 0.8642 0.5925 0.019 Uiso 1 1 d R . .
O1W O 0.70872(14) 0.55642(13) 0.51311(9) 0.0145(2) Uani 1 1 d D . .
H11W H 0.756(2) 0.531(2) 0.5695(14) 0.017 Uiso 1 1 d D . .
H12W H 0.800(2) 0.521(2) 0.4467(12) 0.017 Uiso 1 1 d D . .
O2W O 0.88019(18) 0.47083(16) 0.69068(11) 0.0248(2) Uani 1 1 d D . .
H21W H 0.930(3) 0.3680(16) 0.7154(19) 0.030 Uiso 1 1 d D . .
H22W H 0.821(3) 0.540(2) 0.7554(14) 0.030 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
Ni 0.01153(13) 0.01068(13) 0.01020(13) -0.00027(8) -0.00363(9) -0.00479(10)
N1 0.0143(6) 0.0171(6) 0.0138(6) 0.0004(4) -0.0038(4) -0.0074(5)
N2 0.0140(5) 0.0149(5) 0.0126(5) 0.0005(4) -0.0050(4) -0.0065(5)
N3 0.0154(6) 0.0175(6) 0.0127(6) -0.0011(4) -0.0048(4) -0.0074(5)
C3A 0.0154(6) 0.0142(6) 0.0128(6) 0.0009(5) -0.0051(5) -0.0062(5)
N4 0.0161(6) 0.0216(6) 0.0123(6) -0.0018(5) -0.0045(5) -0.0083(5)
C4 0.0220(7) 0.0297(8) 0.0186(7) -0.0030(6) -0.0081(6) -0.0131(7)
C5 0.0190(7) 0.0174(7) 0.0137(7) 0.0011(5) -0.0053(5) -0.0066(6)
O5 0.0251(6) 0.0271(6) 0.0126(5) -0.0036(4) -0.0033(4) -0.0103(5)
N6 0.0149(6) 0.0241(6) 0.0127(6) -0.0007(5) -0.0014(5) -0.0075(5)
C6 0.0172(7) 0.0372(9) 0.0178(7) -0.0025(6) 0.0021(6) -0.0105(7)
C7 0.0155(7) 0.0206(7) 0.0154(7) 0.0013(5) -0.0046(5) -0.0077(6)
O7 0.0176(5) 0.0390(7) 0.0210(6) -0.0025(5) -0.0041(4) -0.0154(5)
C7A 0.0144(6) 0.0169(7) 0.0131(6) 0.0008(5) -0.0046(5) -0.0069(5)
N1P 0.0120(5) 0.0129(5) 0.0129(5) 0.0006(4) -0.0033(4) -0.0057(4)
C2P 0.0159(6) 0.0167(7) 0.0136(6) 0.0005(5) -0.0042(5) -0.0082(5)
C3P 0.0163(7) 0.0198(7) 0.0157(7) 0.0041(5) -0.0056(5) -0.0070(6)
C4P 0.0169(7) 0.0141(6) 0.0222(7) 0.0034(5) -0.0041(6) -0.0050(5)
C5P 0.0171(7) 0.0138(7) 0.0222(7) -0.0024(5) -0.0037(6) -0.0067(6)
C6P 0.0156(6) 0.0160(7) 0.0169(7) -0.0003(5) -0.0056(5) -0.0073(5)
O1W 0.0149(5) 0.0164(5) 0.0128(5) -0.0003(4) -0.0053(4) -0.0072(4)
O2W 0.0312(6) 0.0239(6) 0.0243(6) 0.0030(5) -0.0158(5) -0.0128(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni N2 179.999(1) 2_666 . ?
N2 Ni N1P 91.03(4) 2_666 2_666 ?
N2 Ni N1P 88.97(4) . 2_666 ?
N2 Ni N1P 88.97(4) 2_666 . ?
N2 Ni N1P 91.03(4) . . ?
N1P Ni N1P 180.00(7) 2_666 . ?
N2 Ni O1W 87.07(4) 2_666 2_666 ?
N2 Ni O1W 92.93(4) . 2_666 ?
N1P Ni O1W 87.78(4) 2_666 2_666 ?
N1P Ni O1W 92.22(4) . 2_666 ?
N2 Ni O1W 92.93(4) 2_666 . ?
N2 Ni O1W 87.08(4) . . ?
N1P Ni O1W 92.22(4) 2_666 . ?
N1P Ni O1W 87.78(4) . . ?
O1W Ni O1W 180.0 2_666 . ?
N2 N1 C7A 105.32(11) . . ?
N1 N2 N3 113.76(11) . . ?
N1 N2 Ni 117.69(9) . . ?
N3 N2 Ni 128.09(9) . . ?
C3A N3 N2 103.41(11) . . ?
N3 C3A N4 127.74(13) . . ?
N3 C3A C7A 110.10(12) . . ?
N4 C3A C7A 122.16(13) . . ?
C5 N4 C3A 119.06(13) . . ?
C5 N4 C4 119.47(12) . . ?
C3A N4 C4 121.39(12) . . ?
N4 C4 H41 109.6 . . ?
N4 C4 H42 109.6 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.3 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 121.12(14) . . ?
O5 C5 N6 120.85(14) . . ?
N4 C5 N6 118.03(13) . . ?
C5 N6 C7 126.48(12) . . ?
C5 N6 C6 116.27(13) . . ?
C7 N6 C6 117.20(13) . . ?
N6 C6 H61 109.6 . . ?
N6 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.3 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.61(13) . . ?
O7 C7 C7A 126.86(14) . . ?
N6 C7 C7A 111.53(13) . . ?
N1 C7A C3A 107.41(12) . . ?
N1 C7A C7 129.94(13) . . ?
C3A C7A C7 122.65(13) . . ?
C6P N1P C2P 118.07(12) . . ?
C6P N1P Ni 120.01(9) . . ?
C2P N1P Ni 121.92(9) . . ?
N1P C2P C3P 122.80(13) . . ?
N1P C2P H2P 118.6 . . ?
C3P C2P H2P 118.6 . . ?
C4P C3P C2P 118.77(13) . . ?
C4P C3P H3P 120.6 . . ?
C2P C3P H3P 120.7 . . ?
C3P C4P C5P 118.82(14) . . ?
C3P C4P H4P 120.7 . . ?
C5P C4P H4P 120.5 . . ?
C6P C5P C4P 118.92(14) . . ?
C6P C5P H5P 120.5 . . ?
C4P C5P H5P 120.6 . . ?
N1P C6P C5P 122.58(13) . . ?
N1P C6P H6P 118.8 . . ?
C5P C6P H6P 118.7 . . ?
Ni O1W H11W 127.5(13) . . ?
Ni O1W H12W 108.5(13) . . ?
H11W O1W H12W 105.7(18) . . ?
H21W O2W H22W 106(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
Ni N2 2.0637(12) 2_666 ?
Ni N2 2.0637(12) . ?
Ni N1P 2.0942(12) 2_666 ?
Ni N1P 2.0943(12) . ?
Ni O1W 2.0950(10) 2_666 ?
Ni O1W 2.0950(10) . ?
N1 N2 1.3195(17) . ?
N1 C7A 1.3571(18) . ?
N2 N3 1.3608(16) . ?
N3 C3A 1.3386(18) . ?
C3A N4 1.3774(18) . ?
C3A C7A 1.3785(19) . ?
N4 C5 1.3697(19) . ?
N4 C4 1.4638(19) . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 O5 1.2290(18) . ?
C5 N6 1.401(2) . ?
N6 C7 1.4092(19) . ?
N6 C6 1.4743(19) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 O7 1.2235(19) . ?
C7 C7A 1.4319(19) . ?
N1P C6P 1.3419(18) . ?
N1P C2P 1.3427(18) . ?
C2P C3P 1.385(2) . ?
C2P H2P 0.9500 . ?
C3P C4P 1.384(2) . ?
C3P H3P 0.9500 . ?
C4P C5P 1.387(2) . ?
C4P H4P 0.9500 . ?
C5P C6P 1.385(2) . ?
C5P H5P 0.9500 . ?
C6P H6P 0.9500 . ?
O1W H11W 0.831(9) . ?
O1W H12W 0.825(9) . ?
O2W H21W 0.842(9) . ?
O2W H22W 0.839(9) . ?
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
O1W H11W O2W 0.831(9) 1.899(9) 2.7286(15) 176.4(19) .
O1W H12W N1 0.825(9) 2.137(15) 2.7501(16) 131.0(16) .
O2W H21W O5 0.842(9) 2.056(11) 2.8809(17) 166(2) 1_556
O2W H22W O7 0.839(9) 2.143(12) 2.9467(16) 160(2) 2_766
|
1500034.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500034.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_1500034
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C22 H26 Cu N12 O6, 2 (H2 O)'
_chemical_formula_sum 'C22 H30 Cu N12 O8'
_chemical_formula_weight 654.12
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 110.327(1)
_cell_angle_beta 92.400(1)
_cell_angle_gamma 98.579(1)
_cell_formula_units_Z 2
_cell_length_a 8.6913(5)
_cell_length_b 11.2673(7)
_cell_length_c 14.9465(9)
_cell_measurement_reflns_used 5228
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.1
_cell_measurement_theta_min 2.4
_cell_volume 1350.22(14)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0186
_diffrn_reflns_av_sigmaI/netI 0.0221
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 15839
_diffrn_reflns_theta_full 26.80
_diffrn_reflns_theta_max 28.34
_diffrn_reflns_theta_min 1.46
_diffrn_standards_decay_% -0.1
_diffrn_standards_number 399
_exptl_absorpt_coefficient_mu 0.881
_exptl_absorpt_correction_T_max 0.810
_exptl_absorpt_correction_T_min 0.744
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.609
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 678
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.29
_exptl_crystal_size_min 0.25
_refine_diff_density_max 0.440
_refine_diff_density_min -0.396
_refine_diff_density_rms 0.088
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 416
_refine_ls_number_reflns 6150
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0302
_refine_ls_R_factor_gt 0.0290
_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^)+(0.0450P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0811
_refine_ls_wR_factor_ref 0.0820
_reflns_number_gt 5835
_reflns_number_total 6150
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound4.cif
_cod_data_source_block cupyrax
_cod_database_code 1500034
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
Cu Cu 0.227939(19) 0.496845(14) 0.244135(11) 0.01063(7) Uani 1 1 d . . .
N1A N 0.12388(14) 0.73090(11) 0.24120(9) 0.0132(2) Uani 1 1 d . . .
N2A N 0.20886(14) 0.68411(11) 0.29216(8) 0.0122(2) Uani 1 1 d . . .
N3A N 0.25954(14) 0.76830(11) 0.38287(9) 0.0131(2) Uani 1 1 d . . .
C3AA C 0.20060(16) 0.87253(13) 0.38703(10) 0.0122(3) Uani 1 1 d . . .
N4A N 0.21502(14) 0.98676(11) 0.46357(8) 0.0135(2) Uani 1 1 d . . .
C4A C 0.31389(18) 1.01125(15) 0.55254(10) 0.0176(3) Uani 1 1 d . . .
H41A H 0.4059 1.0763 0.5582 0.021 Uiso 1 1 d R . .
H42A H 0.3475 0.9315 0.5512 0.021 Uiso 1 1 d R . .
H43A H 0.2541 1.0424 0.6076 0.021 Uiso 1 1 d R . .
C5A C 0.14469(16) 1.08311(14) 0.45396(10) 0.0141(3) Uani 1 1 d . . .
O5A O 0.15757(13) 1.18775(10) 0.51996(8) 0.0180(2) Uani 1 1 d . . .
N6A N 0.05695(15) 1.05990(12) 0.36724(9) 0.0151(2) Uani 1 1 d . . .
C6A C -0.0166(2) 1.16708(15) 0.36124(12) 0.0217(3) Uani 1 1 d . . .
H61A H -0.0657 1.2041 0.4201 0.026 Uiso 1 1 d R . .
H62A H -0.0963 1.1352 0.3061 0.026 Uiso 1 1 d R . .
H63A H 0.0633 1.2332 0.3536 0.026 Uiso 1 1 d R . .
C7A C 0.03942(17) 0.94761(14) 0.28475(10) 0.0155(3) Uani 1 1 d . . .
O7A O -0.03494(15) 0.93855(11) 0.21081(8) 0.0241(3) Uani 1 1 d . . .
C7AA C 0.11718(16) 0.85188(13) 0.30075(10) 0.0129(3) Uani 1 1 d . . .
N1B N 0.31453(14) 0.26687(11) 0.25828(9) 0.0134(2) Uani 1 1 d . . .
N2B N 0.24374(14) 0.30838(11) 0.19819(8) 0.0120(2) Uani 1 1 d . . .
N3B N 0.21506(14) 0.22046(11) 0.10672(8) 0.0128(2) Uani 1 1 d . . .
C3AB C 0.27392(16) 0.12001(13) 0.11239(10) 0.0129(3) Uani 1 1 d . . .
N4B N 0.28103(15) 0.00651(12) 0.03956(9) 0.0156(2) Uani 1 1 d . . .
C4B C 0.2181(2) -0.01725(15) -0.05852(11) 0.0215(3) Uani 1 1 d . . .
H41B H 0.1125 -0.0682 -0.0712 0.026 Uiso 1 1 d R . .
H42B H 0.2858 -0.0645 -0.1036 0.026 Uiso 1 1 d R . .
H43B H 0.2139 0.0649 -0.0666 0.026 Uiso 1 1 d R . .
C5B C 0.35853(18) -0.08185(14) 0.05839(11) 0.0168(3) Uani 1 1 d . . .
O5B O 0.38175(14) -0.17810(11) -0.00507(8) 0.0231(2) Uani 1 1 d . . .
N6B N 0.41129(15) -0.05582(12) 0.15489(9) 0.0169(3) Uani 1 1 d . . .
C6B C 0.4829(2) -0.15581(16) 0.17455(12) 0.0245(3) Uani 1 1 d . . .
H61B H 0.5934 -0.1456 0.1630 0.029 Uiso 1 1 d R . .
H62B H 0.4284 -0.2408 0.1322 0.029 Uiso 1 1 d R . .
H63B H 0.4745 -0.1477 0.2415 0.029 Uiso 1 1 d R . .
C7B C 0.40663(17) 0.05659(14) 0.23328(10) 0.0150(3) Uani 1 1 d . . .
O7B O 0.45988(14) 0.07148(11) 0.31447(8) 0.0209(2) Uani 1 1 d . . .
C7AB C 0.33440(16) 0.14662(13) 0.20532(10) 0.0132(3) Uani 1 1 d . . .
N1P N 0.44799(14) 0.53622(11) 0.21006(8) 0.0115(2) Uani 1 1 d . . .
C2P C 0.55667(17) 0.62791(13) 0.27384(10) 0.0131(3) Uani 1 1 d . . .
H2P H 0.5293 0.6720 0.3361 0.016 Uiso 1 1 d R . .
C3P C 0.70678(17) 0.66008(14) 0.25190(11) 0.0151(3) Uani 1 1 d . . .
H3P H 0.7811 0.7245 0.2987 0.018 Uiso 1 1 d R . .
C4P C 0.74691(17) 0.59728(14) 0.16103(11) 0.0165(3) Uani 1 1 d . . .
H4P H 0.8484 0.6194 0.1439 0.020 Uiso 1 1 d R . .
C5P C 0.63644(18) 0.50111(15) 0.09511(10) 0.0161(3) Uani 1 1 d . . .
H5P H 0.6614 0.4556 0.0325 0.019 Uiso 1 1 d R . .
C6P C 0.48919(17) 0.47321(14) 0.12244(10) 0.0141(3) Uani 1 1 d . . .
H6P H 0.4142 0.4069 0.0776 0.017 Uiso 1 1 d R . .
N1Q N 0.00718(14) 0.45529(11) 0.27703(8) 0.0120(2) Uani 1 1 d . . .
C2Q C -0.02708(17) 0.51113(14) 0.36752(10) 0.0145(3) Uani 1 1 d . . .
H2Q H 0.0513 0.5732 0.4129 0.017 Uiso 1 1 d R . .
C3Q C -0.17215(18) 0.48186(15) 0.39710(11) 0.0172(3) Uani 1 1 d . . .
H3Q H -0.1921 0.5217 0.4618 0.021 Uiso 1 1 d R . .
C4Q C -0.28819(17) 0.39273(15) 0.33030(11) 0.0178(3) Uani 1 1 d . . .
H4Q H -0.3885 0.3705 0.3487 0.021 Uiso 1 1 d R . .
C5Q C -0.25478(17) 0.33731(14) 0.23664(11) 0.0163(3) Uani 1 1 d . . .
H5Q H -0.3327 0.2778 0.1894 0.020 Uiso 1 1 d R . .
C6Q C -0.10596(17) 0.36983(13) 0.21261(10) 0.0142(3) Uani 1 1 d . . .
H6Q H -0.0829 0.3305 0.1485 0.017 Uiso 1 1 d R . .
O1W O 0.32263(12) 0.51154(10) 0.39913(7) 0.0148(2) Uani 1 1 d D . .
H11W H 0.356(2) 0.4453(13) 0.3963(14) 0.018 Uiso 1 1 d D . .
H12W H 0.3949(17) 0.5654(15) 0.4355(12) 0.018 Uiso 1 1 d D . .
O2W O 0.14389(14) 0.50060(11) 0.08853(8) 0.0196(2) Uani 1 1 d D . .
H21W H 0.107(2) 0.5694(13) 0.0993(14) 0.023 Uiso 1 1 d D . .
H22W H 0.081(2) 0.4379(14) 0.0484(12) 0.023 Uiso 1 1 d D . .
O3W O 0.55721(14) 0.69360(11) 0.52840(8) 0.0223(2) Uani 1 1 d D . .
H31W H 0.6384(16) 0.7125(19) 0.5053(14) 0.027 Uiso 1 1 d D . .
H32W H 0.545(2) 0.7611(13) 0.5725(11) 0.027 Uiso 1 1 d D . .
O4W O 0.00204(14) 0.25923(12) -0.03037(8) 0.0241(3) Uani 1 1 d D . .
H41W H 0.003(3) 0.2108(17) -0.0872(8) 0.029 Uiso 1 1 d D . .
H42W H 0.067(2) 0.2413(19) 0.0047(13) 0.029 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 0.01086(10) 0.00875(10) 0.01179(10) 0.00259(7) 0.00269(6) 0.00245(6)
N1A 0.0136(6) 0.0117(5) 0.0138(6) 0.0036(5) 0.0008(4) 0.0033(4)
N2A 0.0133(6) 0.0112(5) 0.0113(5) 0.0032(4) 0.0007(4) 0.0017(4)
N3A 0.0145(6) 0.0114(5) 0.0115(5) 0.0016(5) 0.0003(4) 0.0027(4)
C3AA 0.0115(6) 0.0121(6) 0.0120(6) 0.0032(5) 0.0013(5) 0.0016(5)
N4A 0.0155(6) 0.0117(6) 0.0108(6) 0.0010(5) -0.0015(4) 0.0029(5)
C4A 0.0197(7) 0.0183(7) 0.0117(7) 0.0015(6) -0.0031(5) 0.0044(6)
C5A 0.0135(6) 0.0124(6) 0.0150(7) 0.0034(5) 0.0031(5) 0.0016(5)
O5A 0.0224(5) 0.0121(5) 0.0164(5) 0.0008(4) 0.0024(4) 0.0040(4)
N6A 0.0185(6) 0.0112(6) 0.0156(6) 0.0036(5) 0.0002(5) 0.0062(5)
C6A 0.0287(8) 0.0145(7) 0.0236(8) 0.0058(6) 0.0008(6) 0.0117(6)
C7A 0.0179(7) 0.0125(7) 0.0150(7) 0.0031(5) 0.0001(5) 0.0042(5)
O7A 0.0342(7) 0.0197(6) 0.0173(5) 0.0035(4) -0.0071(5) 0.0113(5)
C7AA 0.0144(6) 0.0113(6) 0.0117(6) 0.0026(5) 0.0003(5) 0.0024(5)
N1B 0.0152(6) 0.0127(6) 0.0129(6) 0.0050(5) 0.0009(4) 0.0035(5)
N2B 0.0134(6) 0.0113(5) 0.0105(5) 0.0029(4) 0.0009(4) 0.0021(4)
N3B 0.0149(6) 0.0108(5) 0.0112(5) 0.0021(4) 0.0003(4) 0.0022(4)
C3AB 0.0132(6) 0.0109(6) 0.0132(7) 0.0032(5) 0.0003(5) 0.0011(5)
N4B 0.0222(6) 0.0113(6) 0.0115(6) 0.0017(5) -0.0008(5) 0.0045(5)
C4B 0.0309(9) 0.0183(7) 0.0122(7) 0.0014(6) -0.0022(6) 0.0065(6)
C5B 0.0192(7) 0.0125(7) 0.0178(7) 0.0040(6) 0.0021(6) 0.0030(5)
O5B 0.0324(6) 0.0151(5) 0.0203(6) 0.0020(4) 0.0037(5) 0.0101(5)
N6B 0.0219(6) 0.0119(6) 0.0182(6) 0.0056(5) 0.0006(5) 0.0068(5)
C6B 0.0335(9) 0.0192(8) 0.0260(8) 0.0108(7) 0.0033(7) 0.0138(7)
C7B 0.0161(7) 0.0135(7) 0.0158(7) 0.0055(6) 0.0011(5) 0.0030(5)
O7B 0.0278(6) 0.0194(5) 0.0170(5) 0.0073(4) -0.0029(4) 0.0076(5)
C7AB 0.0144(6) 0.0120(6) 0.0127(7) 0.0039(5) 0.0008(5) 0.0027(5)
N1P 0.0123(5) 0.0112(5) 0.0115(5) 0.0044(4) 0.0017(4) 0.0031(4)
C2P 0.0158(7) 0.0115(6) 0.0121(6) 0.0037(5) 0.0012(5) 0.0035(5)
C3P 0.0144(7) 0.0133(6) 0.0169(7) 0.0048(5) -0.0008(5) 0.0022(5)
C4P 0.0126(7) 0.0190(7) 0.0205(7) 0.0096(6) 0.0039(5) 0.0040(5)
C5P 0.0178(7) 0.0188(7) 0.0125(6) 0.0053(6) 0.0039(5) 0.0058(6)
C6P 0.0155(7) 0.0142(6) 0.0117(6) 0.0037(5) 0.0005(5) 0.0031(5)
N1Q 0.0132(6) 0.0106(5) 0.0122(6) 0.0038(4) 0.0018(4) 0.0035(4)
C2Q 0.0155(7) 0.0149(7) 0.0123(6) 0.0035(5) 0.0013(5) 0.0039(5)
C3Q 0.0187(7) 0.0207(7) 0.0144(7) 0.0069(6) 0.0058(5) 0.0074(6)
C4Q 0.0144(7) 0.0188(7) 0.0235(8) 0.0107(6) 0.0065(6) 0.0046(6)
C5Q 0.0146(7) 0.0135(7) 0.0199(7) 0.0056(6) -0.0004(5) 0.0017(5)
C6Q 0.0170(7) 0.0121(6) 0.0130(6) 0.0036(5) 0.0019(5) 0.0035(5)
O1W 0.0167(5) 0.0133(5) 0.0127(5) 0.0027(4) 0.0000(4) 0.0031(4)
O2W 0.0225(6) 0.0190(5) 0.0161(5) 0.0037(4) 0.0009(4) 0.0067(4)
O3W 0.0221(6) 0.0227(6) 0.0168(5) 0.0033(5) 0.0003(4) -0.0027(5)
O4W 0.0274(6) 0.0256(6) 0.0168(5) 0.0034(5) -0.0031(5) 0.0089(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N2A Cu N2B 178.68(4) . . ?
N2A Cu N1P 91.91(5) . . ?
N2B Cu N1P 89.23(5) . . ?
N2A Cu N1Q 88.70(5) . . ?
N2B Cu N1Q 90.17(5) . . ?
N1P Cu N1Q 179.32(5) . . ?
N2A Cu O1W 91.53(4) . . ?
N2B Cu O1W 87.76(4) . . ?
N1P Cu O1W 91.55(4) . . ?
N1Q Cu O1W 88.75(4) . . ?
N2A Cu O2W 84.46(4) . . ?
N2B Cu O2W 96.31(4) . . ?
N1P Cu O2W 85.57(4) . . ?
N1Q Cu O2W 94.17(4) . . ?
O1W Cu O2W 174.97(4) . . ?
N2A N1A C7AA 104.91(11) . . ?
N1A N2A N3A 113.81(11) . . ?
N1A N2A Cu 121.11(9) . . ?
N3A N2A Cu 124.37(9) . . ?
C3AA N3A N2A 103.42(11) . . ?
N3A C3AA N4A 127.76(13) . . ?
N3A C3AA C7AA 110.11(12) . . ?
N4A C3AA C7AA 122.13(13) . . ?
C5A N4A C3AA 119.08(12) . . ?
C5A N4A C4A 119.14(12) . . ?
C3AA N4A C4A 121.61(12) . . ?
N4A C4A H41A 109.5 . . ?
N4A C4A H42A 109.5 . . ?
H41A C4A H42A 109.5 . . ?
N4A C4A H43A 109.4 . . ?
H41A C4A H43A 109.5 . . ?
H42A C4A H43A 109.5 . . ?
O5A C5A N4A 121.13(13) . . ?
O5A C5A N6A 120.57(13) . . ?
N4A C5A N6A 118.30(12) . . ?
C5A N6A C7A 126.30(12) . . ?
C5A N6A C6A 115.84(12) . . ?
C7A N6A C6A 117.77(12) . . ?
N6A C6A H61A 109.4 . . ?
N6A C6A H62A 109.5 . . ?
H61A C6A H62A 109.5 . . ?
N6A C6A H63A 109.5 . . ?
H61A C6A H63A 109.5 . . ?
H62A C6A H63A 109.5 . . ?
O7A C7A N6A 121.36(13) . . ?
O7A C7A C7AA 126.90(13) . . ?
N6A C7A C7AA 111.74(12) . . ?
N1A C7AA C3AA 107.75(12) . . ?
N1A C7AA C7A 129.87(13) . . ?
C3AA C7AA C7A 122.37(13) . . ?
N2B N1B C7AB 105.41(11) . . ?
N1B N2B N3B 113.32(11) . . ?
N1B N2B Cu 117.49(9) . . ?
N3B N2B Cu 128.13(9) . . ?
C3AB N3B N2B 103.72(11) . . ?
N3B C3AB N4B 127.91(13) . . ?
N3B C3AB C7AB 109.64(12) . . ?
N4B C3AB C7AB 122.43(13) . . ?
C3AB N4B C5B 119.21(12) . . ?
C3AB N4B C4B 120.83(12) . . ?
C5B N4B C4B 119.80(12) . . ?
N4B C4B H41B 109.5 . . ?
N4B C4B H42B 109.4 . . ?
H41B C4B H42B 109.5 . . ?
N4B C4B H43B 109.5 . . ?
H41B C4B H43B 109.5 . . ?
H42B C4B H43B 109.5 . . ?
O5B C5B N4B 121.99(14) . . ?
O5B C5B N6B 120.92(14) . . ?
N4B C5B N6B 117.09(13) . . ?
C7B N6B C5B 126.79(12) . . ?
C7B N6B C6B 116.87(13) . . ?
C5B N6B C6B 116.32(12) . . ?
N6B C6B H61B 109.5 . . ?
N6B C6B H62B 109.4 . . ?
H61B C6B H62B 109.5 . . ?
N6B C6B H63B 109.5 . . ?
H61B C6B H63B 109.5 . . ?
H62B C6B H63B 109.5 . . ?
O7B C7B N6B 121.80(13) . . ?
O7B C7B C7AB 126.43(14) . . ?
N6B C7B C7AB 111.76(12) . . ?
N1B C7AB C3AB 107.91(12) . . ?
N1B C7AB C7B 129.73(13) . . ?
C3AB C7AB C7B 122.35(13) . . ?
C6P N1P C2P 118.12(12) . . ?
C6P N1P Cu 120.98(10) . . ?
C2P N1P Cu 120.90(9) . . ?
N1P C2P C3P 122.40(13) . . ?
N1P C2P H2P 118.8 . . ?
C3P C2P H2P 118.8 . . ?
C4P C3P C2P 119.12(14) . . ?
C4P C3P H3P 120.5 . . ?
C2P C3P H3P 120.4 . . ?
C3P C4P C5P 118.96(14) . . ?
C3P C4P H4P 120.5 . . ?
C5P C4P H4P 120.5 . . ?
C6P C5P C4P 118.69(13) . . ?
C6P C5P H5P 120.6 . . ?
C4P C5P H5P 120.7 . . ?
N1P C6P C5P 122.68(13) . . ?
N1P C6P H6P 118.7 . . ?
C5P C6P H6P 118.6 . . ?
C2Q N1Q C6Q 118.28(12) . . ?
C2Q N1Q Cu 119.12(10) . . ?
C6Q N1Q Cu 122.56(10) . . ?
N1Q C2Q C3Q 122.62(14) . . ?
N1Q C2Q H2Q 118.7 . . ?
C3Q C2Q H2Q 118.6 . . ?
C2Q C3Q C4Q 118.79(14) . . ?
C2Q C3Q H3Q 120.6 . . ?
C4Q C3Q H3Q 120.6 . . ?
C5Q C4Q C3Q 118.84(14) . . ?
C5Q C4Q H4Q 120.6 . . ?
C3Q C4Q H4Q 120.5 . . ?
C4Q C5Q C6Q 119.13(14) . . ?
C4Q C5Q H5Q 120.4 . . ?
C6Q C5Q H5Q 120.4 . . ?
N1Q C6Q C5Q 122.32(13) . . ?
N1Q C6Q H6Q 118.8 . . ?
C5Q C6Q H6Q 118.9 . . ?
Cu O1W H11W 110.2(13) . . ?
Cu O1W H12W 127.3(13) . . ?
H11W O1W H12W 98.9(18) . . ?
Cu O2W H21W 106.2(14) . . ?
Cu O2W H22W 120.9(14) . . ?
H21W O2W H22W 110.0(19) . . ?
H31W O3W H32W 106(2) . . ?
H41W O4W H42W 108(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
Cu N2A 2.0142(12) . ?
Cu N2B 2.0203(12) . ?
Cu N1P 2.0248(12) . ?
Cu N1Q 2.0281(12) . ?
Cu O1W 2.3675(10) . ?
Cu O2W 2.4248(11) . ?
N1A N2A 1.3235(17) . ?
N1A C7AA 1.3560(18) . ?
N2A N3A 1.3652(16) . ?
N3A C3AA 1.3330(18) . ?
C3AA N4A 1.3777(18) . ?
C3AA C7AA 1.3804(19) . ?
N4A C5A 1.3681(18) . ?
N4A C4A 1.4701(18) . ?
C4A H41A 0.9800 . ?
C4A H42A 0.9800 . ?
C4A H43A 0.9800 . ?
C5A O5A 1.2325(18) . ?
C5A N6A 1.3971(19) . ?
N6A C7A 1.4097(18) . ?
N6A C6A 1.4753(18) . ?
C6A H61A 0.9800 . ?
C6A H62A 0.9800 . ?
C6A H63A 0.9800 . ?
C7A O7A 1.2214(18) . ?
C7A C7AA 1.4354(19) . ?
N1B N2B 1.3174(17) . ?
N1B C7AB 1.3522(18) . ?
N2B N3B 1.3672(16) . ?
N3B C3AB 1.3362(18) . ?
C3AB N4B 1.3735(18) . ?
C3AB C7AB 1.3777(19) . ?
N4B C5B 1.3794(19) . ?
N4B C4B 1.4616(19) . ?
C4B H41B 0.9800 . ?
C4B H42B 0.9800 . ?
C4B H43B 0.9800 . ?
C5B O5B 1.2178(19) . ?
C5B N6B 1.410(2) . ?
N6B C7B 1.4024(19) . ?
N6B C6B 1.4722(19) . ?
C6B H61B 0.9800 . ?
C6B H62B 0.9800 . ?
C6B H63B 0.9800 . ?
C7B O7B 1.2261(18) . ?
C7B C7AB 1.4353(19) . ?
N1P C6P 1.3477(18) . ?
N1P C2P 1.3481(18) . ?
C2P C3P 1.385(2) . ?
C2P H2P 0.9500 . ?
C3P C4P 1.383(2) . ?
C3P H3P 0.9500 . ?
C4P C5P 1.391(2) . ?
C4P H4P 0.9500 . ?
C5P C6P 1.384(2) . ?
C5P H5P 0.9500 . ?
C6P H6P 0.9500 . ?
N1Q C2Q 1.3462(18) . ?
N1Q C6Q 1.3474(18) . ?
C2Q C3Q 1.385(2) . ?
C2Q H2Q 0.9500 . ?
C3Q C4Q 1.393(2) . ?
C3Q H3Q 0.9500 . ?
C4Q C5Q 1.384(2) . ?
C4Q H4Q 0.9500 . ?
C5Q C6Q 1.388(2) . ?
C5Q H5Q 0.9500 . ?
C6Q H6Q 0.9500 . ?
O1W H11W 0.828(9) . ?
O1W H12W 0.829(9) . ?
O2W H21W 0.848(9) . ?
O2W H22W 0.847(9) . ?
O3W H31W 0.830(9) . ?
O3W H32W 0.840(9) . ?
O4W H41W 0.836(9) . ?
O4W H42W 0.849(9) . ?
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
O1W H11W N1B 0.828(9) 2.295(17) 2.8167(16) 121.5(16) .
O1W H12W O3W 0.829(9) 1.959(10) 2.7868(15) 176.3(19) .
O2W H21W N1A 0.848(9) 2.246(17) 2.8328(16) 126.5(17) .
O2W H22W O4W 0.847(9) 1.946(12) 2.7446(17) 156.7(19) .
O3W H32W O7B 0.840(9) 2.056(10) 2.8933(16) 174(2) 2_666
O3W H31W O5A 0.830(9) 2.075(11) 2.8788(16) 163(2) 2_676
O4W H42W N3B 0.849(9) 2.051(10) 2.8918(17) 171(2) .
O4W H41W O7A 0.836(9) 2.084(11) 2.8983(16) 164(2) 2_565
|
1500035.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500035.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_1500035
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C10 H18 N2 O4 Zn 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum 'C22 H30 N12 O8 Zn'
_chemical_formula_weight 655.95
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 86.016(2)
_cell_angle_beta 86.980(2)
_cell_angle_gamma 66.6810(10)
_cell_formula_units_Z 1
_cell_length_a 8.4090(9)
_cell_length_b 8.9126(9)
_cell_length_c 9.9452(10)
_cell_measurement_reflns_used 6128
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.5
_cell_volume 682.56(12)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0160
_diffrn_reflns_av_sigmaI/netI 0.0193
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 8018
_diffrn_reflns_theta_full 26.90
_diffrn_reflns_theta_max 28.24
_diffrn_reflns_theta_min 2.05
_diffrn_standards_decay_% 0.0
_diffrn_standards_number 234
_exptl_absorpt_coefficient_mu 0.971
_exptl_absorpt_correction_T_max 0.901
_exptl_absorpt_correction_T_min 0.781
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.596
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 340
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.353
_refine_diff_density_min -0.265
_refine_diff_density_rms 0.054
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.100
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3100
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.100
_refine_ls_R_factor_all 0.0245
_refine_ls_R_factor_gt 0.0240
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0634
_refine_ls_wR_factor_ref 0.0637
_reflns_number_gt 3035
_reflns_number_total 3100
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound5.cif
_cod_data_source_block znpyrax
_cod_database_code 1500035
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
Zn Zn 0.5000 0.5000 0.5000 0.01395(7) Uani 1 2 d S . .
N1P N 0.33922(14) 0.75519(14) 0.47032(11) 0.0163(2) Uani 1 1 d . . .
C2P C 0.36073(18) 0.86651(17) 0.54365(14) 0.0194(3) Uani 1 1 d . . .
H2P H 0.4426 0.8290 0.6134 0.023 Uiso 1 1 d R . .
C3P C 0.26912(19) 1.03315(17) 0.52258(14) 0.0211(3) Uani 1 1 d . . .
H3P H 0.2881 1.1080 0.5766 0.025 Uiso 1 1 d R . .
C4P C 0.14950(19) 1.08897(17) 0.42097(14) 0.0203(3) Uani 1 1 d . . .
H4P H 0.0854 1.2029 0.4039 0.024 Uiso 1 1 d R . .
C5P C 0.12477(18) 0.97564(17) 0.34504(14) 0.0200(3) Uani 1 1 d . . .
H5P H 0.0434 1.0104 0.2750 0.024 Uiso 1 1 d R . .
C6P C 0.22127(18) 0.81060(17) 0.37315(13) 0.0177(3) Uani 1 1 d . . .
H6P H 0.2032 0.7333 0.3215 0.021 Uiso 1 1 d R . .
N1 N 0.10472(15) 0.46536(14) 0.25822(11) 0.0161(2) Uani 1 1 d . . .
N2 N -0.05953(15) 0.49516(14) 0.29050(11) 0.0172(2) Uani 1 1 d . . .
N3 N -0.12883(14) 0.42388(14) 0.20585(11) 0.0163(2) Uani 1 1 d . . .
C3A C -0.00041(17) 0.34733(16) 0.11871(13) 0.0144(2) Uani 1 1 d . . .
N4 N -0.00465(14) 0.25630(14) 0.01425(11) 0.0156(2) Uani 1 1 d . . .
C4 C -0.16467(18) 0.23561(18) -0.01147(14) 0.0199(3) Uani 1 1 d . . .
H41 H -0.2101 0.2025 0.0730 0.024 Uiso 1 1 d R . .
H42 H -0.1401 0.1511 -0.0767 0.024 Uiso 1 1 d R . .
H43 H -0.2507 0.3393 -0.0480 0.024 Uiso 1 1 d R . .
C5 C 0.14028(17) 0.19054(16) -0.06818(13) 0.0158(3) Uani 1 1 d . . .
O5 O 0.14446(13) 0.11074(12) -0.16369(10) 0.0210(2) Uani 1 1 d . . .
N6 N 0.28849(14) 0.21754(14) -0.03625(11) 0.0159(2) Uani 1 1 d . . .
C6 C 0.43743(18) 0.15186(18) -0.13041(14) 0.0218(3) Uani 1 1 d . . .
H61 H 0.4165 0.2225 -0.2132 0.026 Uiso 1 1 d R . .
H62 H 0.4531 0.0413 -0.1523 0.026 Uiso 1 1 d R . .
H63 H 0.5420 0.1478 -0.0885 0.026 Uiso 1 1 d R . .
C7 C 0.30359(17) 0.30472(16) 0.07115(13) 0.0163(3) Uani 1 1 d . . .
O7 O 0.43992(13) 0.31864(13) 0.09108(10) 0.0223(2) Uani 1 1 d . . .
C7A C 0.14559(17) 0.37143(16) 0.14905(13) 0.0147(2) Uani 1 1 d . . .
O1W O 0.53138(12) 0.48345(12) 0.28531(10) 0.01728(19) Uani 1 1 d D . .
H11W H 0.487(2) 0.4391(19) 0.2370(15) 0.021 Uiso 1 1 d D . .
H12W H 0.6304(14) 0.467(2) 0.2531(17) 0.021 Uiso 1 1 d D . .
O2W O 0.28793(12) 0.43318(12) 0.49048(10) 0.01730(19) Uani 1 1 d D . .
H21W H 0.2110(18) 0.452(2) 0.5507(14) 0.021 Uiso 1 1 d D . .
H22W H 0.2277(19) 0.456(2) 0.4226(13) 0.021 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
Zn 0.01354(11) 0.01559(11) 0.01333(11) -0.00264(8) -0.00130(7) -0.00596(8)
N1P 0.0162(5) 0.0178(5) 0.0156(5) -0.0028(4) -0.0008(4) -0.0071(4)
C2P 0.0197(7) 0.0224(7) 0.0179(6) -0.0034(5) -0.0031(5) -0.0093(5)
C3P 0.0251(7) 0.0204(7) 0.0207(7) -0.0049(5) 0.0003(5) -0.0115(6)
C4P 0.0223(7) 0.0165(6) 0.0207(7) -0.0002(5) 0.0017(5) -0.0066(5)
C5P 0.0199(7) 0.0224(7) 0.0170(6) 0.0001(5) -0.0027(5) -0.0074(5)
C6P 0.0192(6) 0.0196(6) 0.0157(6) -0.0037(5) -0.0011(5) -0.0086(5)
N1 0.0167(5) 0.0183(5) 0.0136(5) -0.0020(4) -0.0003(4) -0.0072(4)
N2 0.0171(5) 0.0203(6) 0.0149(5) -0.0025(4) -0.0010(4) -0.0077(4)
N3 0.0155(5) 0.0195(5) 0.0141(5) -0.0018(4) -0.0013(4) -0.0070(4)
C3A 0.0155(6) 0.0157(6) 0.0122(6) 0.0000(4) -0.0025(5) -0.0062(5)
N4 0.0152(5) 0.0193(5) 0.0143(5) -0.0034(4) -0.0015(4) -0.0084(4)
C4 0.0173(6) 0.0258(7) 0.0209(7) -0.0043(5) -0.0030(5) -0.0124(5)
C5 0.0177(6) 0.0158(6) 0.0147(6) 0.0001(5) -0.0019(5) -0.0073(5)
O5 0.0243(5) 0.0239(5) 0.0177(5) -0.0074(4) 0.0001(4) -0.0116(4)
N6 0.0151(5) 0.0181(5) 0.0148(5) -0.0039(4) 0.0009(4) -0.0065(4)
C6 0.0187(7) 0.0261(7) 0.0209(7) -0.0079(5) 0.0052(5) -0.0089(6)
C7 0.0175(6) 0.0166(6) 0.0155(6) -0.0012(5) -0.0014(5) -0.0074(5)
O7 0.0158(5) 0.0303(5) 0.0238(5) -0.0097(4) 0.0013(4) -0.0113(4)
C7A 0.0151(6) 0.0163(6) 0.0132(6) -0.0011(5) -0.0019(5) -0.0067(5)
O1W 0.0158(5) 0.0237(5) 0.0149(5) -0.0050(4) -0.0001(4) -0.0099(4)
O2W 0.0158(5) 0.0247(5) 0.0135(4) -0.0044(4) -0.0002(4) -0.0097(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2W Zn O2W 180.0 . 2_666 ?
O2W Zn N1P 87.83(4) . 2_666 ?
O2W Zn N1P 92.17(4) 2_666 2_666 ?
O2W Zn N1P 92.17(4) . . ?
O2W Zn N1P 87.83(4) 2_666 . ?
N1P Zn N1P 180.0 2_666 . ?
O2W Zn O1W 88.09(4) . . ?
O2W Zn O1W 91.91(4) 2_666 . ?
N1P Zn O1W 90.85(4) 2_666 . ?
N1P Zn O1W 89.15(4) . . ?
O2W Zn O1W 91.91(4) . 2_666 ?
O2W Zn O1W 88.09(4) 2_666 2_666 ?
N1P Zn O1W 89.15(4) 2_666 2_666 ?
N1P Zn O1W 90.85(4) . 2_666 ?
O1W Zn O1W 180.0 . 2_666 ?
C2P N1P C6P 117.60(12) . . ?
C2P N1P Zn 120.63(9) . . ?
C6P N1P Zn 121.64(9) . . ?
N1P C2P C3P 123.10(13) . . ?
N1P C2P H2P 118.5 . . ?
C3P C2P H2P 118.4 . . ?
C2P C3P C4P 118.80(13) . . ?
C2P C3P H3P 120.6 . . ?
C4P C3P H3P 120.6 . . ?
C3P C4P C5P 118.83(13) . . ?
C3P C4P H4P 120.6 . . ?
C5P C4P H4P 120.6 . . ?
C6P C5P C4P 118.75(13) . . ?
C6P C5P H5P 120.6 . . ?
C4P C5P H5P 120.6 . . ?
N1P C6P C5P 122.91(12) . . ?
N1P C6P H6P 118.6 . . ?
C5P C6P H6P 118.5 . . ?
N2 N1 C7A 106.26(11) . . ?
N1 N2 N3 111.82(11) . . ?
C3A N3 N2 105.12(10) . . ?
N3 C3A N4 127.63(12) . . ?
N3 C3A C7A 109.41(11) . . ?
N4 C3A C7A 122.95(12) . . ?
C3A N4 C5 119.27(11) . . ?
C3A N4 C4 119.81(11) . . ?
C5 N4 C4 120.88(11) . . ?
N4 C4 H41 109.5 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 122.64(12) . . ?
O5 C5 N6 120.36(12) . . ?
N4 C5 N6 116.99(11) . . ?
C7 N6 C5 126.73(11) . . ?
C7 N6 C6 118.06(11) . . ?
C5 N6 C6 115.16(11) . . ?
N6 C6 H61 109.5 . . ?
N6 C6 H62 109.4 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.41(12) . . ?
O7 C7 C7A 126.40(12) . . ?
N6 C7 C7A 112.18(11) . . ?
N1 C7A C3A 107.39(11) . . ?
N1 C7A C7 130.78(12) . . ?
C3A C7A C7 121.82(12) . . ?
Zn O1W H11W 126.7(12) . . ?
Zn O1W H12W 116.0(12) . . ?
H11W O1W H12W 107.7(17) . . ?
Zn O2W H21W 123.1(12) . . ?
Zn O2W H22W 121.7(12) . . ?
H21W O2W H22W 100.0(17) . . ?
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
Zn O2W 2.1000(10) . ?
Zn O2W 2.1001(10) 2_666 ?
Zn N1P 2.1453(11) 2_666 ?
Zn N1P 2.1453(11) . ?
Zn O1W 2.1456(10) . ?
Zn O1W 2.1456(10) 2_666 ?
N1P C2P 1.3437(17) . ?
N1P C6P 1.3448(17) . ?
C2P C3P 1.382(2) . ?
C2P H2P 0.9500 . ?
C3P C4P 1.386(2) . ?
C3P H3P 0.9500 . ?
C4P C5P 1.387(2) . ?
C4P H4P 0.9500 . ?
C5P C6P 1.386(2) . ?
C5P H5P 0.9500 . ?
C6P H6P 0.9500 . ?
N1 N2 1.3251(16) . ?
N1 C7A 1.3628(17) . ?
N2 N3 1.3679(16) . ?
N3 C3A 1.3353(17) . ?
C3A N4 1.3721(17) . ?
C3A C7A 1.3789(18) . ?
N4 C5 1.3772(17) . ?
N4 C4 1.4661(17) . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 O5 1.2166(16) . ?
C5 N6 1.4149(17) . ?
N6 C7 1.4030(17) . ?
N6 C6 1.4698(17) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 O7 1.2283(17) . ?
C7 C7A 1.4314(18) . ?
O1W H11W 0.830(9) . ?
O1W H12W 0.837(9) . ?
O2W H21W 0.832(9) . ?
O2W H22W 0.830(9) . ?
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
O1W H11W O7 0.830(9) 2.007(10) 2.8153(14) 164.3(17) .
O1W H12W N3 0.837(9) 1.943(10) 2.7730(15) 171.5(17) 1_655
O2W H21W N2 0.832(9) 1.938(10) 2.7609(15) 169.9(17) 2_566
O2W H22W N1 0.830(9) 1.960(10) 2.7792(15) 169.3(17) .
|
1500036.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500036.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_1500036
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 911
_journal_page_last 916
_journal_paper_doi 10.1016/j.poly.2009.01.037
_journal_volume 28
_journal_year 2009
_chemical_formula_moiety 'C10 H18 Cd N2 O4 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum 'C22 H30 Cd N12 O8'
_chemical_formula_weight 702.98
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 87.250(1)
_cell_angle_beta 87.410(1)
_cell_angle_gamma 65.661(1)
_cell_formula_units_Z 1
_cell_length_a 8.5015(4)
_cell_length_b 9.1721(5)
_cell_length_c 10.1821(5)
_cell_measurement_reflns_used 7305
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.2
_cell_measurement_theta_min 2.4
_cell_volume 722.29(6)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0210
_diffrn_reflns_av_sigmaI/netI 0.0206
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 8365
_diffrn_reflns_theta_full 26.90
_diffrn_reflns_theta_max 28.24
_diffrn_reflns_theta_min 2.00
_diffrn_standards_decay_% 0.3
_diffrn_standards_number 272
_exptl_absorpt_coefficient_mu 0.823
_exptl_absorpt_correction_T_max 0.750
_exptl_absorpt_correction_T_min 0.644
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.616
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 358
_exptl_crystal_size_max 0.47
_exptl_crystal_size_mid 0.42
_exptl_crystal_size_min 0.37
_refine_diff_density_max 0.277
_refine_diff_density_min -0.286
_refine_diff_density_rms 0.066
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.095
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 3259
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.094
_refine_ls_R_factor_all 0.0230
_refine_ls_R_factor_gt 0.0229
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0605
_refine_ls_wR_factor_ref 0.0606
_reflns_number_gt 3243
_reflns_number_total 3259
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file dmaxpycompound6.cif
_cod_data_source_block cdaxpyr
_cod_database_code 1500036
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
Cd Cd 0.5000 0.5000 0.5000 0.03921(7) Uani 1 2 d S . .
O1W O 0.52928(18) 0.47827(19) 0.27267(13) 0.0513(3) Uani 1 1 d D . .
H11W H 0.488(3) 0.432(3) 0.227(2) 0.062 Uiso 1 1 d D . .
H12W H 0.6285(17) 0.462(3) 0.245(2) 0.062 Uiso 1 1 d D . .
O2W O 0.27075(18) 0.4323(2) 0.48888(13) 0.0523(3) Uani 1 1 d D . .
H21W H 0.198(3) 0.452(3) 0.5509(18) 0.063 Uiso 1 1 d D . .
H22W H 0.213(3) 0.457(3) 0.4211(16) 0.063 Uiso 1 1 d D . .
N1P N 0.3293(2) 0.77010(19) 0.46922(16) 0.0472(3) Uani 1 1 d . . .
C2P C 0.2162(3) 0.8234(2) 0.3725(2) 0.0534(5) Uani 1 1 d . . .
H2P H 0.2004 0.7478 0.3206 0.064 Uiso 1 1 d R . .
C3P C 0.1226(3) 0.9834(3) 0.3440(2) 0.0616(5) Uani 1 1 d . . .
H3P H 0.0435 1.0179 0.2755 0.074 Uiso 1 1 d R . .
C4P C 0.1452(3) 1.0938(3) 0.4187(2) 0.0629(5) Uani 1 1 d . . .
H4P H 0.0815 1.2060 0.4034 0.076 Uiso 1 1 d R . .
C5P C 0.2596(4) 1.0405(3) 0.5197(3) 0.0687(6) Uani 1 1 d . . .
H5P H 0.2766 1.1135 0.5738 0.082 Uiso 1 1 d R . .
C6P C 0.3488(3) 0.8789(3) 0.5411(2) 0.0608(5) Uani 1 1 d . . .
H6P H 0.4278 0.8418 0.6096 0.073 Uiso 1 1 d R . .
N1 N 0.0995(2) 0.4621(2) 0.25453(14) 0.0444(3) Uani 1 1 d . . .
N2 N -0.0624(2) 0.4914(2) 0.28682(15) 0.0466(3) Uani 1 1 d . . .
N3 N -0.13069(19) 0.4225(2) 0.20266(14) 0.0447(3) Uani 1 1 d . . .
C3A C -0.0041(2) 0.3485(2) 0.11657(15) 0.0383(3) Uani 1 1 d . . .
N4 N -0.00762(19) 0.25973(19) 0.01265(14) 0.0433(3) Uani 1 1 d . . .
C4 C -0.1646(3) 0.2389(3) -0.0131(2) 0.0580(5) Uani 1 1 d . . .
H41 H -0.2019 0.2012 0.0645 0.070 Uiso 1 1 d R . .
H42 H -0.1366 0.1587 -0.0806 0.070 Uiso 1 1 d R . .
H43 H -0.2580 0.3410 -0.0415 0.070 Uiso 1 1 d R . .
C5 C 0.1363(2) 0.1940(2) -0.06783(17) 0.0443(4) Uani 1 1 d . . .
O5 O 0.1408(2) 0.1140(2) -0.16068(15) 0.0619(4) Uani 1 1 d . . .
N6 N 0.28169(19) 0.22073(19) -0.03745(15) 0.0440(3) Uani 1 1 d . . .
C6 C 0.4303(3) 0.1567(3) -0.1301(2) 0.0609(5) Uani 1 1 d . . .
H61 H 0.4050 0.2282 -0.2049 0.073 Uiso 1 1 d R . .
H62 H 0.4502 0.0490 -0.1575 0.073 Uiso 1 1 d R . .
H63 H 0.5341 0.1503 -0.0885 0.073 Uiso 1 1 d R . .
C7 C 0.2962(2) 0.3063(2) 0.06797(17) 0.0435(4) Uani 1 1 d . . .
O7 O 0.43046(19) 0.3203(2) 0.08579(16) 0.0648(4) Uani 1 1 d . . .
C7A C 0.1401(2) 0.3714(2) 0.14604(16) 0.0391(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd 0.03526(10) 0.04566(11) 0.03884(10) -0.00700(7) -0.00426(6) -0.01785(7)
O1W 0.0454(7) 0.0741(9) 0.0416(7) -0.0152(6) 0.0019(5) -0.0309(7)
O2W 0.0431(7) 0.0821(10) 0.0420(7) -0.0146(7) -0.0006(5) -0.0347(7)
N1P 0.0464(8) 0.0470(8) 0.0478(8) -0.0075(6) -0.0078(6) -0.0175(7)
C2P 0.0589(11) 0.0535(10) 0.0467(10) -0.0082(8) -0.0118(8) -0.0204(9)
C3P 0.0664(13) 0.0605(12) 0.0519(11) 0.0044(9) -0.0148(10) -0.0193(10)
C4P 0.0736(14) 0.0459(10) 0.0656(13) 0.0039(9) -0.0058(11) -0.0210(10)
C5P 0.0845(17) 0.0516(11) 0.0763(15) -0.0098(11) -0.0157(13) -0.0320(12)
C6P 0.0646(13) 0.0544(11) 0.0654(13) -0.0077(10) -0.0223(10) -0.0237(10)
N1 0.0434(8) 0.0563(9) 0.0370(7) -0.0082(6) -0.0040(6) -0.0232(7)
N2 0.0431(8) 0.0598(9) 0.0380(7) -0.0085(6) -0.0019(6) -0.0215(7)
N3 0.0385(7) 0.0591(9) 0.0388(7) -0.0054(6) -0.0036(6) -0.0216(7)
C3A 0.0395(8) 0.0471(9) 0.0316(7) 0.0002(6) -0.0062(6) -0.0208(7)
N4 0.0429(8) 0.0562(9) 0.0387(7) -0.0076(6) -0.0049(6) -0.0274(7)
C4 0.0519(11) 0.0792(14) 0.0580(12) -0.0114(10) -0.0085(9) -0.0404(11)
C5 0.0503(10) 0.0485(9) 0.0390(9) -0.0049(7) -0.0040(7) -0.0245(8)
O5 0.0691(9) 0.0744(10) 0.0532(8) -0.0259(7) 0.0030(7) -0.0384(8)
N6 0.0415(8) 0.0526(8) 0.0406(7) -0.0091(6) 0.0021(6) -0.0216(7)
C6 0.0561(12) 0.0731(14) 0.0544(12) -0.0198(10) 0.0132(9) -0.0270(11)
C7 0.0408(9) 0.0524(10) 0.0416(9) -0.0067(7) -0.0025(7) -0.0229(8)
O7 0.0437(7) 0.0965(12) 0.0663(9) -0.0302(8) 0.0068(6) -0.0389(8)
C7A 0.0390(8) 0.0487(9) 0.0333(8) -0.0031(6) -0.0044(6) -0.0213(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2W Cd O2W 180.0 . 2_666 ?
O2W Cd N1P 87.16(6) . 2_666 ?
O2W Cd N1P 92.84(6) 2_666 2_666 ?
O2W Cd N1P 92.84(6) . . ?
O2W Cd N1P 87.16(6) 2_666 . ?
N1P Cd N1P 180.0 2_666 . ?
O2W Cd O1W 87.09(5) . . ?
O2W Cd O1W 92.91(5) 2_666 . ?
N1P Cd O1W 91.28(6) 2_666 . ?
N1P Cd O1W 88.72(6) . . ?
O2W Cd O1W 92.91(5) . 2_666 ?
O2W Cd O1W 87.09(5) 2_666 2_666 ?
N1P Cd O1W 88.72(6) 2_666 2_666 ?
N1P Cd O1W 91.28(6) . 2_666 ?
O1W Cd O1W 180.0 . 2_666 ?
Cd O1W H11W 126.7(18) . . ?
Cd O1W H12W 112.6(17) . . ?
H11W O1W H12W 109(2) . . ?
Cd O2W H21W 120.5(18) . . ?
Cd O2W H22W 119.2(18) . . ?
H21W O2W H22W 105(2) . . ?
C6P N1P C2P 117.56(17) . . ?
C6P N1P Cd 121.21(13) . . ?
C2P N1P Cd 121.06(13) . . ?
N1P C2P C3P 122.91(19) . . ?
N1P C2P H2P 118.7 . . ?
C3P C2P H2P 118.4 . . ?
C2P C3P C4P 118.7(2) . . ?
C2P C3P H3P 121.3 . . ?
C4P C3P H3P 120.0 . . ?
C3P C4P C5P 118.9(2) . . ?
C3P C4P H4P 121.5 . . ?
C5P C4P H4P 119.6 . . ?
C6P C5P C4P 118.7(2) . . ?
C6P C5P H5P 120.3 . . ?
C4P C5P H5P 120.9 . . ?
N1P C6P C5P 123.2(2) . . ?
N1P C6P H6P 117.8 . . ?
C5P C6P H6P 119.0 . . ?
N2 N1 C7A 106.37(14) . . ?
N1 N2 N3 111.65(14) . . ?
C3A N3 N2 105.13(14) . . ?
N3 C3A C7A 109.61(15) . . ?
N3 C3A N4 127.66(15) . . ?
C7A C3A N4 122.73(15) . . ?
C5 N4 C3A 119.34(14) . . ?
C5 N4 C4 120.53(15) . . ?
C3A N4 C4 120.12(16) . . ?
N4 C4 H41 109.2 . . ?
N4 C4 H42 108.0 . . ?
H41 C4 H42 109.0 . . ?
N4 C4 H43 111.2 . . ?
H41 C4 H43 108.4 . . ?
H42 C4 H43 110.9 . . ?
O5 C5 N4 122.21(17) . . ?
O5 C5 N6 120.62(17) . . ?
N4 C5 N6 117.16(15) . . ?
C7 N6 C5 126.72(15) . . ?
C7 N6 C6 117.47(16) . . ?
C5 N6 C6 115.77(16) . . ?
N6 C6 H61 107.1 . . ?
N6 C6 H62 111.6 . . ?
H61 C6 H62 109.6 . . ?
N6 C6 H63 109.6 . . ?
H61 C6 H63 110.6 . . ?
H62 C6 H63 108.3 . . ?
O7 C7 N6 121.04(17) . . ?
O7 C7 C7A 126.63(17) . . ?
N6 C7 C7A 112.33(15) . . ?
N1 C7A C3A 107.23(15) . . ?
N1 C7A C7 131.05(15) . . ?
C3A C7A C7 121.71(15) . . ?
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
Cd O2W 2.2848(13) . ?
Cd O2W 2.2848(13) 2_666 ?
Cd N1P 2.3119(16) 2_666 ?
Cd N1P 2.3119(16) . ?
Cd O1W 2.3261(13) . ?
Cd O1W 2.3261(13) 2_666 ?
O1W H11W 0.828(10) . ?
O1W H12W 0.832(10) . ?
O2W H21W 0.836(10) . ?
O2W H22W 0.834(10) . ?
N1P C6P 1.332(3) . ?
N1P C2P 1.336(2) . ?
C2P C3P 1.375(3) . ?
C2P H2P 0.9463 . ?
C3P C4P 1.375(3) . ?
C3P H3P 0.9408 . ?
C4P C5P 1.376(3) . ?
C4P H4P 0.9531 . ?
C5P C6P 1.370(3) . ?
C5P H5P 0.9460 . ?
C6P H6P 0.9407 . ?
N1 N2 1.318(2) . ?
N1 C7A 1.360(2) . ?
N2 N3 1.367(2) . ?
N3 C3A 1.326(2) . ?
C3A C7A 1.374(2) . ?
C3A N4 1.374(2) . ?
N4 C5 1.371(2) . ?
N4 C4 1.461(2) . ?
C4 H41 0.9410 . ?
C4 H42 0.9796 . ?
C4 H43 0.9864 . ?
C5 O5 1.214(2) . ?
C5 N6 1.406(2) . ?
N6 C7 1.399(2) . ?
N6 C6 1.471(2) . ?
C6 H61 0.9530 . ?
C6 H62 0.9827 . ?
C6 H63 0.9753 . ?
C7 O7 1.222(2) . ?
C7 C7A 1.431(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O7 0.828(10) 1.988(11) 2.800(2) 167(2) .
O1W H12W N3 0.832(10) 1.958(10) 2.785(2) 173(2) 1_655
O2W H21W N2 0.836(10) 1.935(11) 2.758(2) 168(3) 2_566
O2W H22W N1 0.834(10) 1.977(11) 2.795(2) 167(2) .
|
1500037.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500037.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_1500037
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
'Antonio Rodr\'iguez-Di\'eguez'
_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
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 1553
_journal_page_last 1558
_journal_paper_doi 10.1016/j.ica.2008.07.029
_journal_volume 362
_journal_year 2009
_chemical_formula_moiety 'H12 Mn O6 2+, 2 (C6 H6 N5 O2 1-)'
_chemical_formula_sum 'C12 H24 Mn N10 O10'
_chemical_formula_weight 523.35
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 74.563(3)
_cell_angle_beta 80.102(3)
_cell_angle_gamma 63.533(3)
_cell_formula_units_Z 1
_cell_length_a 7.7462(14)
_cell_length_b 8.0979(15)
_cell_length_c 9.9361(18)
_cell_measurement_reflns_used 4476
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.1
_cell_measurement_theta_min 2.9
_cell_volume 536.79(17)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0153
_diffrn_reflns_av_sigmaI/netI 0.0176
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 6253
_diffrn_reflns_theta_full 26.90
_diffrn_reflns_theta_max 28.27
_diffrn_reflns_theta_min 2.13
_diffrn_standards_decay_% 0.1
_diffrn_standards_number 181
_exptl_absorpt_coefficient_mu 0.688
_exptl_absorpt_correction_T_max 0.904
_exptl_absorpt_correction_T_min 0.780
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.619
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 271
_exptl_crystal_size_max 0.47
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.309
_refine_diff_density_min -0.326
_refine_diff_density_rms 0.078
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 171
_refine_ls_number_reflns 2425
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.031
_refine_ls_R_factor_all 0.0382
_refine_ls_R_factor_gt 0.0372
_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^)+(0.0700P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1113
_refine_ls_wR_factor_ref 0.1126
_reflns_number_gt 2326
_reflns_number_total 2425
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file mnax.cif
_cod_data_source_block mnax
_cod_database_code 1500037
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
Mn Mn 0.5000 0.5000 0.5000 0.03280(15) Uani 1 2 d S . .
O1W O 0.7103(2) 0.2140(2) 0.51298(15) 0.0462(4) Uani 1 1 d D . .
H11W H 0.755(4) 0.150(3) 0.5918(16) 0.055 Uiso 1 1 d D . .
H12W H 0.801(3) 0.184(4) 0.450(2) 0.055 Uiso 1 1 d D . .
O2W O 0.2725(2) 0.4267(3) 0.46492(16) 0.0482(4) Uani 1 1 d D . .
H21W H 0.227(4) 0.373(4) 0.5378(19) 0.058 Uiso 1 1 d D . .
H22W H 0.179(3) 0.517(3) 0.421(3) 0.058 Uiso 1 1 d D . .
O3W O 0.5650(2) 0.5744(2) 0.27584(14) 0.0413(3) Uani 1 1 d D . .
H31W H 0.659(3) 0.496(3) 0.235(3) 0.050 Uiso 1 1 d D . .
H32W H 0.501(3) 0.665(3) 0.212(2) 0.050 Uiso 1 1 d D . .
N1 N 1.1290(2) 0.0268(2) 0.23854(16) 0.0368(4) Uani 1 1 d . . .
N2 N 0.9711(2) 0.1630(3) 0.27832(17) 0.0415(4) Uani 1 1 d . . .
N3 N 0.8774(2) 0.2975(2) 0.16754(16) 0.0361(4) Uani 1 1 d . . .
C3A C 0.9849(2) 0.2388(2) 0.05519(17) 0.0278(3) Uani 1 1 d . . .
N4 N 0.9533(2) 0.3258(2) -0.08282(15) 0.0293(3) Uani 1 1 d . . .
C4 C 0.7841(3) 0.5045(3) -0.1221(2) 0.0384(4) Uani 1 1 d . . .
H41 H 0.6893 0.4809 -0.1549 0.046 Uiso 1 1 d R . .
H42 H 0.7299 0.5605 -0.0421 0.046 Uiso 1 1 d R . .
H43 H 0.8220 0.5890 -0.1950 0.046 Uiso 1 1 d R . .
C5 C 1.0804(2) 0.2425(2) -0.18382(17) 0.0272(3) Uani 1 1 d . . .
O5 O 1.05534(19) 0.3130(2) -0.30840(13) 0.0371(3) Uani 1 1 d . . .
N6 N 1.2415(2) 0.0733(2) -0.14074(15) 0.0285(3) Uani 1 1 d . . .
C6 C 1.3786(3) -0.0113(3) -0.2521(2) 0.0401(4) Uani 1 1 d . . .
H61 H 1.4463 -0.1449 -0.2180 0.048 Uiso 1 1 d R . .
H62 H 1.3092 0.0119 -0.3314 0.048 Uiso 1 1 d R . .
H63 H 1.4695 0.0440 -0.2794 0.048 Uiso 1 1 d R . .
C7 C 1.2839(2) -0.0225(2) -0.00254(17) 0.0283(3) Uani 1 1 d . . .
O7 O 1.4282(2) -0.17072(19) 0.02443(14) 0.0401(3) Uani 1 1 d . . .
C7A C 1.1420(2) 0.0717(2) 0.09633(17) 0.0282(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn 0.0263(2) 0.0352(2) 0.0236(2) -0.00130(15) -0.00229(14) -0.00380(16)
O1W 0.0401(8) 0.0418(8) 0.0258(7) 0.0006(6) 0.0004(6) 0.0046(6)
O2W 0.0365(8) 0.0663(10) 0.0317(7) 0.0105(7) -0.0090(6) -0.0221(7)
O3W 0.0383(7) 0.0380(7) 0.0232(6) -0.0011(5) -0.0005(5) 0.0019(6)
N1 0.0346(8) 0.0377(8) 0.0222(7) -0.0001(6) -0.0015(6) -0.0050(7)
N2 0.0370(9) 0.0436(9) 0.0246(8) -0.0029(7) 0.0008(6) -0.0035(7)
N3 0.0310(8) 0.0371(8) 0.0252(7) -0.0052(6) 0.0000(6) -0.0026(6)
C3A 0.0251(8) 0.0280(8) 0.0235(8) -0.0026(6) -0.0020(6) -0.0065(6)
N4 0.0257(7) 0.0262(7) 0.0240(7) -0.0004(5) -0.0050(5) -0.0020(6)
C4 0.0308(9) 0.0297(9) 0.0381(10) -0.0021(7) -0.0099(7) 0.0017(7)
C5 0.0244(7) 0.0288(8) 0.0240(8) -0.0007(6) -0.0036(6) -0.0093(6)
O5 0.0332(7) 0.0435(7) 0.0225(6) 0.0020(5) -0.0041(5) -0.0098(6)
N6 0.0249(7) 0.0290(7) 0.0224(7) -0.0032(5) -0.0002(5) -0.0050(6)
C6 0.0352(10) 0.0414(10) 0.0298(9) -0.0095(8) 0.0043(7) -0.0050(8)
C7 0.0256(8) 0.0264(8) 0.0256(8) -0.0013(6) -0.0028(6) -0.0064(6)
O7 0.0342(7) 0.0320(7) 0.0314(7) -0.0015(5) -0.0030(5) 0.0035(5)
C7A 0.0263(8) 0.0270(8) 0.0225(8) -0.0005(6) -0.0029(6) -0.0057(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Mn Mn 0.3368 0.7283 '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
O1W Mn O1W 180.0 2_666 . ?
O1W Mn O3W 87.99(5) 2_666 . ?
O1W Mn O3W 92.01(5) . . ?
O1W Mn O3W 92.01(5) 2_666 2_666 ?
O1W Mn O3W 87.99(5) . 2_666 ?
O3W Mn O3W 180.00(8) . 2_666 ?
O1W Mn O2W 91.16(7) 2_666 2_666 ?
O1W Mn O2W 88.84(7) . 2_666 ?
O3W Mn O2W 88.38(6) . 2_666 ?
O3W Mn O2W 91.62(6) 2_666 2_666 ?
O1W Mn O2W 88.84(7) 2_666 . ?
O1W Mn O2W 91.16(7) . . ?
O3W Mn O2W 91.62(6) . . ?
O3W Mn O2W 88.38(6) 2_666 . ?
O2W Mn O2W 179.999(2) 2_666 . ?
Mn O1W H11W 118.2(19) . . ?
Mn O1W H12W 121.4(19) . . ?
H11W O1W H12W 108(3) . . ?
Mn O2W H21W 115(2) . . ?
Mn O2W H22W 115(2) . . ?
H21W O2W H22W 108(3) . . ?
Mn O3W H31W 120.6(18) . . ?
Mn O3W H32W 131.9(19) . . ?
H31W O3W H32W 107(3) . . ?
N2 N1 C7A 106.28(14) . . ?
N1 N2 N3 112.17(15) . . ?
C3A N3 N2 104.77(14) . . ?
N3 C3A N4 127.78(15) . . ?
N3 C3A C7A 109.63(15) . . ?
N4 C3A C7A 122.58(15) . . ?
C5 N4 C3A 119.11(14) . . ?
C5 N4 C4 120.09(15) . . ?
C3A N4 C4 120.80(15) . . ?
N4 C4 H41 109.4 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.6 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 121.27(15) . . ?
O5 C5 N6 120.88(15) . . ?
N4 C5 N6 117.85(14) . . ?
C7 N6 C5 126.22(14) . . ?
C7 N6 C6 117.13(14) . . ?
C5 N6 C6 116.65(14) . . ?
N6 C6 H61 109.4 . . ?
N6 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.30(16) . . ?
O7 C7 C7A 126.32(16) . . ?
N6 C7 C7A 112.38(14) . . ?
N1 C7A C3A 107.15(15) . . ?
N1 C7A C7 131.01(16) . . ?
C3A C7A C7 121.84(15) . . ?
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
Mn O1W 2.1413(15) 2_666 ?
Mn O1W 2.1413(15) . ?
Mn O3W 2.1790(14) . ?
Mn O3W 2.1790(14) 2_666 ?
Mn O2W 2.1983(16) 2_666 ?
Mn O2W 2.1983(16) . ?
O1W H11W 0.847(10) . ?
O1W H12W 0.849(10) . ?
O2W H21W 0.848(10) . ?
O2W H22W 0.849(10) . ?
O3W H31W 0.853(10) . ?
O3W H32W 0.850(10) . ?
N1 N2 1.316(2) . ?
N1 C7A 1.360(2) . ?
N2 N3 1.362(2) . ?
N3 C3A 1.332(2) . ?
C3A N4 1.372(2) . ?
C3A C7A 1.374(2) . ?
N4 C5 1.364(2) . ?
N4 C4 1.466(2) . ?
C4 H41 0.9600 . ?
C4 H42 0.9600 . ?
C4 H43 0.9600 . ?
C5 O5 1.226(2) . ?
C5 N6 1.401(2) . ?
N6 C7 1.399(2) . ?
N6 C6 1.474(2) . ?
C6 H61 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C7 O7 1.224(2) . ?
C7 C7A 1.427(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H12W N2 0.849(10) 1.965(12) 2.799(2) 167(3) .
O1W H11W N1 0.847(10) 1.947(11) 2.789(2) 172(3) 2_756
O2W H21W O5 0.848(10) 1.955(13) 2.779(2) 164(3) 1_456
O2W H22W O5 0.849(10) 2.020(12) 2.855(2) 168(3) 2_665
O3W H31W N3 0.853(10) 1.908(11) 2.756(2) 172(3) .
O3W H32W O7 0.850(10) 1.983(13) 2.7998(19) 161(3) 1_465
|
1500038.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500038.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_1500038
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quir\'os'
'Juan M. Salas'
_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
_journal_name_full Polyhedron
_journal_page_first 372
_journal_page_last 378
_journal_paper_doi 10.1016/j.poly.2009.06.002
_journal_volume 29
_journal_year 2010
_chemical_formula_moiety 'C16 H28 N14 Ni O4, 3(H2 O)'
_chemical_formula_sum 'C16 H34 N14 Ni O7'
_chemical_formula_weight 593.28
_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 mixed
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 95.215(2)
_cell_angle_beta 95.770(3)
_cell_angle_gamma 117.933(2)
_cell_formula_units_Z 1
_cell_length_a 8.1905(19)
_cell_length_b 8.2396(13)
_cell_length_c 10.8651(17)
_cell_measurement_reflns_used 4966
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 27.9
_cell_measurement_theta_min 2.8
_cell_volume 636.5(2)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART (Bruker, 1999)'
_computing_data_reduction 'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 295(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_sigmaI/netI 0.0240
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 7343
_diffrn_reflns_theta_full 26.70
_diffrn_reflns_theta_max 28.24
_diffrn_reflns_theta_min 1.91
_diffrn_standards_decay_% 0.2
_diffrn_standards_number 179
_exptl_absorpt_coefficient_mu 0.829
_exptl_absorpt_correction_T_max 0.914
_exptl_absorpt_correction_T_min 0.698
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour pink
_exptl_crystal_density_diffrn 1.548
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 312
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.582
_refine_diff_density_min -0.456
_refine_diff_density_rms 0.073
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 187
_refine_ls_number_reflns 2851
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.068
_refine_ls_R_factor_all 0.0424
_refine_ls_R_factor_gt 0.0413
_refine_ls_shift/su_max 0.029
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1139
_refine_ls_wR_factor_ref 0.1147
_reflns_number_gt 2729
_reflns_number_total 2851
_reflns_threshold_expression I>2\s(I)
_cod_data_source_file niendmax.cif
_cod_data_source_block nienax
_cod_database_code 1500038
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.5000 0.5000 0.5000 0.02831(14) Uani 1 2 d S . .
N1 N 0.2052(2) 0.3169(2) 0.27040(16) 0.0352(4) Uani 1 1 d . . .
N2 N 0.3688(2) 0.4646(2) 0.31403(16) 0.0353(4) Uani 1 1 d . . .
N3 N 0.4351(2) 0.5807(2) 0.22773(16) 0.0337(4) Uani 1 1 d . . .
C3A C 0.3042(3) 0.4972(3) 0.12627(18) 0.0293(4) Uani 1 1 d . . .
N4 N 0.3024(2) 0.5552(2) 0.01151(16) 0.0344(4) Uani 1 1 d . . .
C4 C 0.4531(3) 0.7314(3) -0.0115(2) 0.0453(5) Uani 1 1 d . . .
H41 H 0.5410 0.7086 -0.0520 0.054 Uiso 1 1 d R . .
H42 H 0.5161 0.8130 0.0666 0.054 Uiso 1 1 d R . .
H43 H 0.4010 0.7884 -0.0645 0.054 Uiso 1 1 d R . .
C5 C 0.1556(3) 0.4463(3) -0.08334(19) 0.0334(4) Uani 1 1 d . . .
O5 O 0.1478(3) 0.4921(2) -0.18642(15) 0.0469(4) Uani 1 1 d . . .
N6 N 0.0124(2) 0.2800(2) -0.05720(16) 0.0339(4) Uani 1 1 d . . .
C6 C -0.1372(3) 0.1626(3) -0.1627(2) 0.0434(5) Uani 1 1 d . . .
H61 H -0.1992 0.0367 -0.1466 0.052 Uiso 1 1 d R . .
H62 H -0.0845 0.1667 -0.2382 0.052 Uiso 1 1 d R . .
H63 H -0.2262 0.2074 -0.1725 0.052 Uiso 1 1 d R . .
C7 C 0.0016(3) 0.2137(3) 0.05770(19) 0.0331(4) Uani 1 1 d . . .
O7 O -0.1334(2) 0.0686(2) 0.07098(16) 0.0469(4) Uani 1 1 d . . .
C7A C 0.1610(3) 0.3342(3) 0.15082(18) 0.0308(4) Uani 1 1 d . . .
N1E N 0.4280(4) 0.2184(3) 0.4678(2) 0.0637(7) Uani 1 1 d . . .
H11E H 0.4352 0.1771 0.5410 0.076 Uiso 1 1 d R . .
H12E H 0.3101 0.1503 0.4262 0.076 Uiso 1 1 d R . .
C1E C 0.5608(8) 0.2028(6) 0.3936(3) 0.0865(13) Uani 1 1 d . . .
H13E H 0.5261 0.2080 0.3066 0.104 Uiso 1 1 d R . .
H14E H 0.5585 0.0847 0.3981 0.104 Uiso 1 1 d R . .
C2E C 0.7543(7) 0.3613(7) 0.4448(3) 0.0924(15) Uani 1 1 d . . .
H23E H 0.7926 0.3514 0.5300 0.111 Uiso 1 1 d R . .
H24E H 0.8435 0.3570 0.3940 0.111 Uiso 1 1 d R . .
N2E N 0.7494(3) 0.5359(4) 0.4420(2) 0.0548(6) Uani 1 1 d . . .
H21E H 0.7531 0.5645 0.3640 0.066 Uiso 1 1 d R . .
H22E H 0.8486 0.6290 0.4937 0.066 Uiso 1 1 d R . .
O1W O 0.7897(3) 0.9175(3) 0.2983(2) 0.0696(6) Uani 1 1 d D . .
H11W H 0.811(6) 0.976(5) 0.235(2) 0.084 Uiso 1 1 d D . .
H12W H 0.685(3) 0.818(3) 0.276(3) 0.084 Uiso 1 1 d D . .
O2W O 0.0643(6) 0.9081(6) 0.4655(4) 0.0585(9) Uiso 0.50 1 d PD . .
H21W H 0.006(9) 0.954(9) 0.422(4) 0.070 Uiso 0.50 1 d PD . .
H22W H 0.071(9) 0.953(9) 0.5420(18) 0.070 Uiso 0.50 1 d PD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.02354(19) 0.02531(19) 0.0280(2) 0.00690(13) 0.00189(13) 0.00519(14)
N1 0.0278(8) 0.0330(8) 0.0310(8) 0.0085(7) 0.0010(7) 0.0035(7)
N2 0.0288(8) 0.0326(8) 0.0322(9) 0.0093(7) 0.0013(7) 0.0049(7)
N3 0.0275(8) 0.0302(8) 0.0318(8) 0.0091(7) 0.0028(7) 0.0041(7)
C3A 0.0256(9) 0.0270(9) 0.0297(9) 0.0062(7) 0.0042(7) 0.0078(7)
N4 0.0315(9) 0.0310(8) 0.0313(8) 0.0111(7) 0.0051(7) 0.0065(7)
C4 0.0393(12) 0.0369(11) 0.0467(12) 0.0175(10) 0.0111(10) 0.0052(10)
C5 0.0350(10) 0.0346(10) 0.0298(9) 0.0066(8) 0.0065(8) 0.0157(9)
O5 0.0534(10) 0.0499(10) 0.0307(8) 0.0129(7) 0.0045(7) 0.0188(8)
N6 0.0302(8) 0.0324(8) 0.0292(8) 0.0026(7) 0.0005(7) 0.0083(7)
C6 0.0393(11) 0.0440(12) 0.0331(11) -0.0019(9) -0.0047(9) 0.0123(10)
C7 0.0279(9) 0.0308(9) 0.0324(10) 0.0051(8) 0.0029(8) 0.0079(8)
O7 0.0337(8) 0.0378(8) 0.0434(9) 0.0096(7) 0.0002(7) -0.0032(7)
C7A 0.0258(9) 0.0282(9) 0.0301(9) 0.0076(7) 0.0043(7) 0.0057(8)
N1E 0.112(2) 0.0358(10) 0.0418(11) 0.0153(9) 0.0231(12) 0.0308(13)
C1E 0.171(4) 0.090(3) 0.0499(17) 0.0195(17) 0.026(2) 0.102(3)
C2E 0.133(4) 0.175(5) 0.0495(17) 0.036(2) 0.029(2) 0.133(4)
N2E 0.0409(11) 0.0934(18) 0.0383(10) 0.0250(11) 0.0132(9) 0.0353(12)
O1W 0.0528(11) 0.0628(13) 0.0483(11) 0.0198(9) -0.0015(9) -0.0088(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1E Ni N1E 180.0 2_666 . ?
N1E Ni N2E 82.91(11) 2_666 2_666 ?
N1E Ni N2E 97.09(11) . 2_666 ?
N1E Ni N2E 97.09(11) 2_666 . ?
N1E Ni N2E 82.91(11) . . ?
N2E Ni N2E 180.0 2_666 . ?
N1E Ni N2 92.29(9) 2_666 . ?
N1E Ni N2 87.72(9) . . ?
N2E Ni N2 87.47(8) 2_666 . ?
N2E Ni N2 92.53(8) . . ?
N1E Ni N2 87.71(9) 2_666 2_666 ?
N1E Ni N2 92.28(9) . 2_666 ?
N2E Ni N2 92.53(8) 2_666 2_666 ?
N2E Ni N2 87.47(8) . 2_666 ?
N2 Ni N2 180.00(11) . 2_666 ?
N2 N1 C7A 105.63(16) . . ?
N1 N2 N3 112.85(16) . . ?
N1 N2 Ni 120.02(13) . . ?
N3 N2 Ni 127.13(13) . . ?
C3A N3 N2 104.16(16) . . ?
N3 C3A N4 128.12(18) . . ?
N3 C3A C7A 109.60(18) . . ?
N4 C3A C7A 122.28(18) . . ?
C5 N4 C3A 119.42(17) . . ?
C5 N4 C4 119.14(18) . . ?
C3A N4 C4 121.43(18) . . ?
N4 C4 H41 109.6 . . ?
N4 C4 H42 109.6 . . ?
H41 C4 H42 109.4 . . ?
N4 C4 H43 109.3 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.4 . . ?
O5 C5 N4 121.7(2) . . ?
O5 C5 N6 120.7(2) . . ?
N4 C5 N6 117.53(17) . . ?
C5 N6 C7 126.51(17) . . ?
C5 N6 C6 115.95(18) . . ?
C7 N6 C6 117.52(18) . . ?
N6 C6 H61 109.5 . . ?
N6 C6 H62 109.6 . . ?
H61 C6 H62 109.4 . . ?
N6 C6 H63 109.5 . . ?
H61 C6 H63 109.4 . . ?
H62 C6 H63 109.4 . . ?
O7 C7 N6 120.93(19) . . ?
O7 C7 C7A 126.75(19) . . ?
N6 C7 C7A 112.32(17) . . ?
N1 C7A C3A 107.76(17) . . ?
N1 C7A C7 130.32(17) . . ?
C3A C7A C7 121.92(18) . . ?
C1E N1E Ni 107.1(2) . . ?
C1E N1E H11E 110.1 . . ?
Ni N1E H11E 110.3 . . ?
C1E N1E H12E 110.5 . . ?
Ni N1E H12E 110.2 . . ?
H11E N1E H12E 108.5 . . ?
N1E C1E C2E 108.7(3) . . ?
N1E C1E H13E 109.8 . . ?
C2E C1E H13E 110.0 . . ?
N1E C1E H14E 109.9 . . ?
C2E C1E H14E 110.1 . . ?
H13E C1E H14E 108.4 . . ?
N2E C2E C1E 108.3(3) . . ?
N2E C2E H23E 110.1 . . ?
C1E C2E H23E 110.1 . . ?
N2E C2E H24E 110.0 . . ?
C1E C2E H24E 109.9 . . ?
H23E C2E H24E 108.4 . . ?
C2E N2E Ni 107.5(2) . . ?
C2E N2E H21E 110.2 . . ?
Ni N2E H21E 110.2 . . ?
C2E N2E H22E 110.2 . . ?
Ni N2E H22E 110.2 . . ?
H21E N2E H22E 108.5 . . ?
H11W O1W H12W 107(4) . . ?
H21W O2W H22W 103.1(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N1E 2.093(2) 2_666 ?
Ni N1E 2.093(2) . ?
Ni N2E 2.093(2) 2_666 ?
Ni N2E 2.093(2) . ?
Ni N2 2.1179(17) . ?
Ni N2 2.1179(17) 2_666 ?
N1 N2 1.319(2) . ?
N1 C7A 1.352(3) . ?
N2 N3 1.367(2) . ?
N3 C3A 1.331(3) . ?
C3A N4 1.376(3) . ?
C3A C7A 1.379(2) . ?
N4 C5 1.373(3) . ?
N4 C4 1.464(3) . ?
C4 H41 0.9602 . ?
C4 H42 0.9603 . ?
C4 H43 0.9603 . ?
C5 O5 1.219(3) . ?
C5 N6 1.402(3) . ?
N6 C7 1.402(3) . ?
N6 C6 1.469(3) . ?
C6 H61 0.9605 . ?
C6 H62 0.9605 . ?
C6 H63 0.9605 . ?
C7 O7 1.224(3) . ?
C7 C7A 1.433(3) . ?
N1E C1E 1.463(5) . ?
N1E H11E 0.9000 . ?
N1E H12E 0.9000 . ?
C1E C2E 1.509(7) . ?
C1E H13E 0.9700 . ?
C1E H14E 0.9700 . ?
C2E N2E 1.461(5) . ?
C2E H23E 0.9700 . ?
C2E H24E 0.9700 . ?
N2E H21E 0.9000 . ?
N2E H22E 0.9000 . ?
O1W H11W 0.858(10) . ?
O1W H12W 0.854(10) . ?
O2W H21W 0.863(10) . ?
O2W H22W 0.866(10) . ?
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
O1W H12W N3 0.854(10) 2.034(11) 2.888(3) 178(4) .
O1W H11W O7 0.858(10) 2.016(13) 2.860(3) 168(4) 1_665
N1E H12E O2W 0.90 2.19 2.872(5) 132.5 1_545
N2E H22E O2W 0.90 2.22 2.905(5) 132.3 1_655
N2E H21E O5 0.90 2.26 3.002(3) 139.6 2_665
O2W H21W O1W 0.863(10) 2.00(3) 2.781(5) 150(6) 1_455
O2W H22W O1W 0.866(10) 1.89(3) 2.681(5) 151(6) 2_676
|
1500039.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500039.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_1500039
loop_
_publ_author_name
'Thun, J\"urgen'
'Seyfarth, Lena'
'Senker, J\"urgen'
'Dinnebier, Robert E.'
'Breu, Josef'
_publ_section_title
;
Polymorphism in benzamide: solving a 175-year-old riddle.
;
_journal_issue 35
_journal_name_full
'Angewandte Chemie (International ed. in English)'
_journal_page_first 6729
_journal_page_last 6731
_journal_paper_doi 10.1002/anie.200701383
_journal_volume 46
_journal_year 2007
_chemical_formula_sum 'C7 H7 N O'
_chemical_name_common Benzamide
_space_group_IT_number 14
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_audit_update_record
;
2008-06-03 # Formatted by publCIF
;
_cell_angle_alpha 90
_cell_angle_beta 101.2914(20)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.05506(12)
_cell_length_b 5.51404(14)
_cell_length_c 22.95644(91)
_cell_volume 627.50(3)
_exptl_crystal_colour colorless
_exptl_crystal_description needles
_exptl_crystal_preparation 'coolling crystallisation out of water'
_cod_data_source_file Benzamid_Phase3.CIF
_cod_data_source_block I
_cod_original_cell_volume 627.498(33)
_cod_database_code 1500039
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'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_B_iso_or_equiv
C6 C -0.8381848 -0.0277765 0.1127388 1 12.00(28)
C1 C -0.9156163 -0.05641078 0.1676438 1 12.00(28)
C5 C -0.6760289 0.1686831 0.1034122 1 12.00(28)
C7 C -0.9271704 -0.2040304 0.06486965 1 12.00(28)
C2 C -0.830921 0.1114492 0.2132364 1 12.00(28)
H10 H -1.031432 -0.1967648 0.1742954 1 12.00(28)
C4 C -0.5913647 0.3365869 0.1489963 1 12.00(28)
H14 H -0.6206821 0.1890765 0.06419718 1 12.00(28)
N8 N -0.7770325 -0.2439537 0.0242951 1 12.00(28)
O9 O -1.141541 -0.3150856 0.06233416 1 12.00(28)
C3 C -0.6688376 0.3079858 0.2039266 1 12.00(28)
H11 H -0.8862228 0.09095163 0.252454 1 12.00(28)
H13 H -0.475571 0.476939 0.14234 1 12.00(28)
H15 H -0.8532281 -0.3366809 -0.012614 1 12.00(28)
H16 H -0.5879374 -0.1812028 0.03069444 1 12.00(28)
H12 H -0.60839 0.4279133 0.236486 1 12.00(28)
|
1500040.cif | #------------------------------------------------------------------------------
#$Date: 2017-01-11 19:10:56 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500040.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_1500040
loop_
_publ_author_name
'Al-Ktaifani, M. M. '
'Rukiah, M. K. '
'Shaaban, A. K.'
_publ_contact_author_address
;Atomic Energy Commission of Syria (AECS),
Damascus,
P. O. Box 6091,
Syrian Arab Republic
;
_publ_contact_author_email malktaifani@aec.org.sy
_publ_contact_author_fax +963-11-6112289
_publ_contact_author_name 'M. M. Al-Ktaifani'
_publ_contact_author_phone +963-11-2132580
_publ_section_title
;
Synthesis and Solid State Characterization of Organometallic Polymer of
Ag(I) Using 2,2-Dimethyl-1,3-diisocyano Propane Ligand
;
_journal_coden_Cambridge 456
_journal_name_full Pol.J.Chem.
_journal_page_first 547
_journal_page_last 557
_journal_volume 82
_journal_year 2008
_chemical_formula_moiety 'C7 H10 Ag Cl N2'
_chemical_formula_sum 'C7 H10 Ag Cl N2'
_chemical_formula_weight 265.49
_chemical_name_systematic
' Silver(I) complex of 2,2-Dimethyl-1,3-Diisocyano Propane'
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90.00000
_cell_angle_beta 90.00000
_cell_angle_gamma 90.00000
_cell_formula_units_Z 8
_cell_length_a 16.33228(18)
_cell_length_b 16.2155(3)
_cell_length_c 7.24228(9)
_cell_measurement_temperature 295
_cell_volume 1918.02(5)
_computing_data_collection WinXPOW
_computing_molecular_graphics ORTEP
_computing_publication_material FULLPROF
_computing_structure_refinement FULLPROF
_computing_structure_solution FOX
_diffrn_ambient_temperature 295
_diffrn_detector 'linear PSD'
_diffrn_detector_type 'Stoe transmission STADI P'
_diffrn_measurement_device_type 'transmission geometry (horizontal set-up)'
_diffrn_radiation_monochromator 'Ge 111'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a~1~'
_diffrn_radiation_wavelength 1.54060
_diffrn_source 'sealed X-ray tube'
_diffrn_source_target Cu
_diffrn_source_type C-Tech
_exptl_absorpt_coefficient_mu 18.945
_exptl_absorpt_process_details
; FullProf Absorption/surface roughness correction
No correction is applied ?.
;
_exptl_crystal_density_diffrn 1.839
_exptl_crystal_F_000 1040
_pd_calc_method ' Rietveld Refinement'
_pd_char_colour white
_pd_meas_2theta_range_inc 0.010000
_pd_meas_2theta_range_max 99.99000
_pd_meas_2theta_range_min 5.00000
_pd_meas_number_of_points 9500
_pd_meas_scan_method cont
_pd_proc_ls_background_function ' FullProf Background function number'
_pd_proc_ls_peak_cutoff 0.00500
_pd_proc_ls_profile_function
;
;
_pd_proc_ls_prof_R_factor 3.0100
_pd_proc_ls_prof_wR_expected 2.0911
_pd_proc_ls_prof_wR_factor 3.8635
_pd_spec_mounting
;
drifted powder on two foils of Mylar
;
_pd_spec_mount_mode transmission
_pd_spec_shape flat_sheet
_pd_spec_size_axial 7.0
_pd_spec_size_equat 7.0
_pd_spec_size_thick 0.1
_refine_ls_goodness_of_fit_all 1.85
_refine_ls_number_parameters 106
_refine_ls_number_reflns 1026
_refine_ls_number_restraints 17
_refine_ls_R_I_factor 2.9758
_cod_data_source_file 665676.cif
_cod_data_source_block Ag(C7H10N2)Cl
_cod_depositor_comments
;
Changing the _atom_site_label data item values to match the ones in
the related data items (e. g. _geom_angle_atom_site_label_*).
Antanas Vaitkus,
2017-01-11
Changing the _atom_type_symbol and _atom_site_type_symbol data
item values to match each other.
Antanas Vaitkus,
2017-01-11
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_diffrn_radiation_probe' tag value 'x-rays' was replaced with
'x-ray' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_cell_volume 1918.01(4)
_cod_original_sg_symbol_H-M 'P B C A'
_cod_database_code 1500040
#BEGIN Tags that were not found in dictionaries:
_pd_proc_ls_prof_cr_factor 8.0553
_pd_proc_ls_prof_cwr_factor 7.8356
_pd_proc_ls_prof_cwr_expected 4.2409
_pd_proc_ls_prof_chi2 3.4137
_pd_proc_ls_prof_echi2 3.4738
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,y,1/2-z
1/2-x,1/2+y,z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Ag1 0.8823(4) 0.7061(8) 0.5940(11) 0.0500(4) 1.00000 Uiso Ag+1
Cl1 0.7976(13) 0.6736(3) 0.9004(4) 0.0632(11) 1.00000 Uiso Cl-1
C1 0.8312(4) 0.6057(8) 0.4270(13) 0.0409(15) 1.00000 Uiso C
C2 0.7101(2) 0.5435(6) 0.2437(12) 0.0409(15) 1.00000 Uiso C
C3 0.6311(3) 0.5871(3) 0.3129(5) 0.0409(15) 1.00000 Uiso C
C4 0.5650(4) 0.5457(7) 0.1923(11) 0.0409(15) 1.00000 Uiso C
C5 0.6157(6) 0.5752(7) 0.5219(6) 0.0409(15) 1.00000 Uiso C
C6 0.6300(4) 0.6758(3) 0.2334(9) 0.0409(15) 1.00000 Uiso C
C7 0.4949(3) 0.7486(8) 0.3393(13) 0.0409(15) 1.00000 Uiso C
N1 0.7785(3) 0.5783(6) 0.3405(8) 0.038(2) 1.00000 Uiso N
N2 0.5587(3) 0.7195(6) 0.3005(7) 0.038(2) 1.00000 Uiso N
H2A 0.70730 0.48520 0.27000 0.06333 1.00000 Uiso H
H2B 0.71740 0.55170 0.11360 0.06333 1.00000 Uiso H
H4A 0.57680 0.55390 0.06350 0.06333 1.00000 Uiso H
H4B 0.51230 0.56940 0.22000 0.06333 1.00000 Uiso H
H4C 0.56330 0.48750 0.21780 0.06333 1.00000 Uiso H
H5A 0.65870 0.60280 0.58710 0.06333 1.00000 Uiso H
H5B 0.61500 0.51830 0.54930 0.06333 1.00000 Uiso H
H5C 0.56400 0.60020 0.55150 0.06333 1.00000 Uiso H
H6A 0.67880 0.70500 0.28040 0.06333 1.00000 Uiso H
H6B 0.63160 0.67580 0.10310 0.06333 1.00000 Uiso H
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag+1 19.18120 0.64618 15.97190 7.19123 5.27475 21.73260 0.35753 66.11470
5.21572 -0.06000 4.28200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
Cl-1 18.29150 0.00660 7.20840 1.17170 6.53370 19.54240 2.33860 60.44860
-16.37800 0.34800 0.70200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
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
C1 Ag1 C7 . . 3_566 137.8(8) yes
C1 Ag1 Cl1 . . . 96.6(5) yes
C1 Ag1 Cl1 . . 8_564 93.1(6) yes
C7 Ag1 Cl1 3_566 . 8_564 108.4(7) yes
Cl1 Ag1 Cl1 . . 8_564 107.5(2) yes
Ag1 C1 N1 . . . 150.4(8) yes
C1 N1 C2 . . . 176.3(11) yes
N1 C2 C3 . . . 108.1(6) yes
C2 C3 C4 . . . 101.6(6) yes
C2 C3 C5 . . . 113.2(7) yes
C2 C3 C6 . . . 108.2(7) yes
C4 C3 C5 . . . 112.7(7) yes
C4 C3 C6 . . . 100.7(7) yes
C5 C3 C6 . . . 118.5(7) yes
C6 N2 C7 . . . 171.2(10) yes
N2 C7 Ag1 . . 3_466 177.5(7) 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
Ag1 Cl1 . . 2.668(14) yes
Ag1 C1 . . 2.193(16) yes
Ag1 C7 . 3_566 2.038(10) yes
Ag1 Cl1 . 8_564 2.772(15) yes
N1 C1 . . 1.154(11) yes
N1 C2 . . 1.435(9) yes
N2 C6 . . 1.447(9) yes
N2 C7 . . 1.178(9) yes
C2 C3 . . 1.554(8) yes
C3 C4 . . 1.542(9) yes
C3 C5 . . 1.547(6) yes
C3 C6 . . 1.549(7) yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 Ag1 Cl1 Ag1 . . . 8_565 174.5(5) yes
C7 Ag1 Cl1 Ag1 3_566 . . 8_565 27.7(7) yes
Cl1 Ag1 Cl1 Ag1 8_564 . . 8_565 -90.2(6) yes
Cl1 Ag1 C1 N1 . . . . 76.9(17) yes
C7 Ag1 C1 N1 3_566 . . . -153.2(14) yes
Cl1 Ag1 C1 N1 8_564 . . . -31.1(17) yes
Cl1 Ag1 Cl1 Ag1 . . 8_564 8_564 -163.7(5) yes
C1 Ag1 Cl1 Ag1 . . 8_564 8_564 -65.8(5) yes
N1 C2 C3 C4 . . . . 178.0(7) yes
N1 C2 C3 C5 . . . . -60.9(9) yes
N1 C2 C3 C6 . . . . 72.5(7) yes
C2 C3 C6 N2 . . . . -177.9(5) yes
C4 C3 C6 N2 . . . . 76.1(6) yes
C5 C3 C6 N2 . . . . -47.3(7) yes
|
1500041.cif | #------------------------------------------------------------------------------
#$Date: 2017-01-11 18:54:48 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190403 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500041.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_1500041
loop_
_publ_author_name
'Abbattista, F'
'Mazza, D'
'Vallino, M'
_publ_section_title
;
Preparatiion and characterization of BaLaFeO4
;
_journal_coden_ASTM MRBUA
_journal_name_full 'Materials Research Bulletin'
_journal_page_first 733
_journal_page_last 738
_journal_paper_doi 10.1016/0025-5408(86)90153-4
_journal_volume 21
_journal_year 1986
_chemical_formula_structural 'Ba La Fe O4'
_chemical_formula_sum 'Ba Fe La O4'
_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 3.921(2)
_cell_length_b 3.921(2)
_cell_length_c 13.175(5)
_cell_volume 202.56(17)
_refine_ls_R_factor_all 0.065
_cod_data_source_file BaLaFeO.cif
_cod_data_source_block 0000000
_cod_depositor_comments
;
Changing _atom_site_label data item values to unique ones after consulting
the original publication.
Antanas Vaitkus,
2017-01-11
Adding missing _atom_type_symbol and _atom_type_oxidation_number data
item values that correspond to the _atom_site_type_symbol data item
values ('Ba2+', 'La3+').
Antanas Vaitkus,
2017-01-11
;
_cod_original_cell_volume 202.6
_cod_original_formula_sum 'Ba La Fe O4'
_cod_database_code 1500041
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_U_iso_or_equiv
Ba Ba2+ 4 e 0 0 0.361 0.5 0.50
La La3+ 4 e 0 0 0.361 0.5 0.50
Fe Fe3+ 2 a 0 0 0 1.0 0.50
O1 O2- 4 c 0.5 0 0 1.0 0.50
O2 O2- 4 e 0 0 0.165 1.0 0.50
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe3+ 3.000
O2- -2.000
Ba2+ 2.000
La3+ 3.000
|
1500042.cif | #------------------------------------------------------------------------------
#$Date: 2017-01-11 18:54:48 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190403 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500042.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_1500042
loop_
_publ_author_name
'Abbattista, F'
'Mazza, D'
'Vallino, M'
_publ_section_title
;
New Phase with K2 Ni F4 Structure in the La-Li-Fe-O System
;
_journal_coden_ASTM MRBUA
_journal_name_full 'Materials Research Bulletin'
_journal_page_first 393
_journal_page_last 398
_journal_paper_doi 10.1016/0025-5408(85)90006-6
_journal_volume 20
_journal_year 1985
_chemical_formula_structural 'La1.75 Li0.75 Fe0.5 O3.92'
_chemical_formula_sum 'Fe0.5 La1.75 Li0.75 O3.92'
_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 3.765(1)
_cell_length_b 3.765(1)
_cell_length_c 12.918(10)
_cell_volume 183.12(16)
_refine_ls_R_factor_all 0.061
_cod_data_source_file La175Li075Fe05O.cif
_cod_data_source_block 0000000
_cod_depositor_comments
;
Changing _atom_site_label data item values to unique ones after consulting
the original publication.
Antanas Vaitkus,
2017-01-11
Adding missing _atom_type_symbol and _atom_type_oxidation_number data
item values that correspond to the _atom_site_type_symbol data item
values ('Ba3+', 'Li+').
Antanas Vaitkus,
2017-01-11
;
_cod_original_cell_volume 183.1
_cod_original_formula_sum 'La1.75 Li0.75 Fe0.5 O3.92'
_cod_database_code 1500042
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_U_iso_or_equiv
La La3+ 4 e 0 0 0.362 0.875 0.40
Li1 Li+ 4 e 0 0 0.362 0.125 2.50
Fe Fe3+ 2 a 0 0 0 0.5 3.30
Li2 Li+ 2 a 0 0 0 0.5 0.10
O2 O2- 4 c 0.5 0 0 1.0 0.10
O1 O2- 4 e 0 0 0.184 0.96 0.10
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe3+ 3.000
O2- -2.000
La3+ 3.000
Li+ 1.000
|
1500043.cif | #------------------------------------------------------------------------------
#$Date: 2017-01-11 18:54:48 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190403 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500043.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_1500043
loop_
_publ_author_name
'Abbattista, F'
'Mazza, D'
'Vallino, M'
_publ_section_title
;
Preparation and characterization of La2 Li.5 Al.5 O4 with K2 Ni F4
structure
;
_journal_coden_ASTM ICHAA
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 147
_journal_page_last 149
_journal_paper_doi 10.1016/S0020-1693(00)81072-5
_journal_volume 140
_journal_year 1987
_chemical_formula_structural 'La2 Li0.5 Al0.5 O4'
_chemical_formula_sum 'Al0.5 La2 Li0.5 O4'
_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 3.772(1)
_cell_length_b 3.772(1)
_cell_length_c 12.757(4)
_cell_volume 181.51(9)
_refine_ls_R_factor_all 0.070
_cod_data_source_file La2Li05Al05O.cif
_cod_data_source_block 0000000
_cod_depositor_comments
;
Changing _atom_site_label data item values to unique ones after consulting
the original publication.
Antanas Vaitkus,
2017-01-11
Adding missing _atom_type_symbol and _atom_type_oxidation_number data
item values that correspond to the _atom_site_type_symbol data item
values ('La3+', 'Li+').
Antanas Vaitkus,
2017-01-11
;
_cod_original_cell_volume 181.5
_cod_original_formula_sum 'La2 Li0.5 Al0.5 O4'
_cod_database_code 1500043
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_U_iso_or_equiv
La La3+ 4 e 0 0 0.3625 1.0 0.60
Li Li+ 2 a 0 0 0 0.5 0.90
Al Al3+ 2 a 0 0 0 0.5 1.2
O1 O2- 4 c 0.5 0 0 1.0 0.70
O2 O2- 4 e 0 0 0.17 1.0 0.70
loop_
_atom_type_symbol
_atom_type_oxidation_number
Al3+ 3.000
O2- -2.000
La3+ 3.000
Li+ 1.000
|
1500044.cif | #------------------------------------------------------------------------------
#$Date: 2017-01-11 18:54:48 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190403 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500044.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_1500044
loop_
_publ_author_name
'Abbattista, F'
'Mazza, D'
'Vallino, M'
'Gazzano, M'
_publ_section_title
;
A new structure in the La-Li-Fe-O system
;
_journal_coden_ASTM JCOMA
_journal_name_full 'Journal of the Less-Common Metals'
_journal_page_first 203
_journal_page_last 211
_journal_paper_doi 10.1016/0022-5088(88)90178-6
_journal_volume 142
_journal_year 1988
_chemical_formula_structural 'La24 Fe6 Li22 O56'
_chemical_formula_sum 'Fe6 La24 Li22 O56'
_space_group_IT_number 127
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-P 4 2ab'
_symmetry_space_group_name_H-M 'P 4/m b m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 13.240(3)
_cell_length_b 13.240(3)
_cell_length_c 7.497(3)
_cell_volume 1314.2(7)
_refine_ls_R_factor_all 0.024
_cod_data_source_file La24Fe6Li22O.cif
_cod_data_source_block 0000000
_cod_depositor_comments
;
Changing _atom_site_label data item values to unique ones after consulting
the original publication.
Antanas Vaitkus,
2017-01-11
Adding missing _atom_type_symbol and _atom_type_oxidation_number data
item values that correspond to the _atom_site_type_symbol data item
values ('Ba3+', 'Li+').
Antanas Vaitkus,
2017-01-11
;
_cod_original_cell_volume 1314.2
_cod_original_formula_sum 'La24 Fe6 Li22 O56'
_cod_database_code 1500044
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
1/2+x,1/2-y,z
1/2-x,1/2+y,z
-y,x,z
y,-x,z
1/2+y,1/2+x,z
1/2-y,1/2-x,z
-x,-y,-z
x,y,-z
1/2-x,1/2+y,-z
1/2+x,1/2-y,-z
y,-x,-z
-y,x,-z
1/2-y,1/2-x,-z
1/2+y,1/2+x,-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_U_iso_or_equiv
La1 La3+ 16 l 0.008(0) 0.1997(0) 0.2556(0) 1.0 0.0062
La2 La3+ 4 g 0.2605(0) 0.7605(0) 0 1.0 0.0034
La3 La3+ 4 h 0.2198(0) 0.7198(0) 0.5 1.0 0.0034
Fe1 Fe3+ 2 a 0 0 0 1.0 0.0094
Fe2 Fe3+ 4 g 0.0859(1) 0.5859(1) 0 1.0 0.0042
O1 O2- 4 f 0 0.5 0.1849(10) 1.0 0.0050
O2 O2- 8 j 0.3823(5) 0.3773(5) 0.5 1.0 0.0110
O3 O2- 8 k 0.3168(3) 0.8168(3) 0.7102(8) 1.0 0.0140
O4 O2- 8 j 0.3212(4) 0.0173(5) 0.5 1.0 0.0080
O5 O2- 4 e 0 0 0.2513(15) 1.0 0.0090
O6 O2- 8 i 0.1224(5) 0.1117(5) 0 1.0 0.0100
O7 O2- 8 i 0.0303(4) 0.3123(4) 0 1.0 0.0060
O8 O2- 8 k 0.1583(3) 0.6583(3) 0.8047(9) 1.0 0.0130
Li1 Li+ 2 b 0 0 0.5 1.0 0.0024
Li2 Li+ 4 h 0.6219(9) 0.1219(9) 0.5 1.0 0.0020
Li3 Li+ 8 k 0.0981(8) 0.4019(8) 0.1565(22) 1.0 0.0100
Li4 Li+ 8 k 0.0753(8) 0.5753(8) 0.6499(22) 1.0 0.0100
loop_
_atom_type_symbol
_atom_type_oxidation_number
Fe3+ 3.000
O2- -2.000
La3+ 3.000
Li+ 1.000
|
1500045.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500045.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_1500045
loop_
_publ_author_name
'Luukkanen, Saija'
'Haukka, Matti'
'Eskelinen, Esa'
'Pakkanen, Tapani A.'
'Lehtovuori, Viivi'
'Kallioinen, Jani'
'Myllyperki\"o, Pasi'
'Korppi-Tommola, Jouko'
_publ_section_title
;
Photochemical reactivity of halogen-containing ruthenium--dcbpy (dcbpy =
4,4'-dicarboxylic acid-2,2'-bipyridine) compounds,
trans(Br)-[Ru(dcbpy)(CO)2Br2] and trans(I)-[Ru(dcbpy)(CO)2I2]
;
_journal_issue 11
_journal_name_full 'Physical Chemistry Chemical Physics'
_journal_page_first 1992
_journal_paper_doi 10.1039/b100659m
_journal_volume 3
_journal_year 2001
_chemical_formula_sum 'C14 H10 Br2 N2 O7 Ru'
_chemical_formula_weight 579.13
_chemical_name_common Ru(dcbpy)(CO)2Br2.(H2O)
_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 90.0000(10)
_cell_angle_beta 92.7382(12)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 6.57440(10)
_cell_length_b 19.6040(4)
_cell_length_c 13.4362(2)
_cell_measurement_temperature 120(2)
_cell_volume 1729.74(5)
_computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection 'Collect (Nonius, 1999)'
_computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)'
_computing_publication_material SHELXL-97
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature 120(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method phi-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 0.0272
_diffrn_reflns_av_sigmaI/netI 0.0240
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 23446
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 3.27
_exptl_absorpt_coefficient_mu 5.567
_exptl_absorpt_correction_T_max 0.3068
_exptl_absorpt_correction_T_min 0.2101
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.224
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1112
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.657
_refine_diff_density_min -0.608
_refine_diff_density_rms 0.095
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 235
_refine_ls_number_reflns 3801
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0234
_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^)+(0.0268P)^2^+2.6533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0612
_refine_ls_wR_factor_ref 0.0626
_reflns_number_gt 3558
_reflns_number_total 3801
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file 156911_156912.txt
_cod_data_source_block structure_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1500045
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4666(4) 0.59133(12) 0.50370(18) 0.0189(5) Uani 1 1 d . . .
C2 C 0.8493(4) 0.58383(12) 0.59057(19) 0.0179(5) Uani 1 1 d . . .
C10 C 1.0302(3) 0.72855(12) 0.66179(18) 0.0154(4) Uani 1 1 d . . .
H10 H 1.0766 0.6836 0.6762 0.018 Uiso 1 1 calc R . .
C11 C 1.1485(3) 0.78288(12) 0.69480(17) 0.0148(4) Uani 1 1 d . . .
H11 H 1.2752 0.7754 0.7302 0.018 Uiso 1 1 calc R . .
C12 C 1.0798(4) 0.84836(11) 0.67555(18) 0.0137(5) Uani 1 1 d . . .
C13 C 0.8923(3) 0.85807(12) 0.62368(18) 0.0143(4) Uani 1 1 d . . .
H13 H 0.8412 0.9027 0.6107 0.017 Uiso 1 1 calc R . .
C14 C 0.7823(3) 0.80081(12) 0.59165(17) 0.0127(4) Uani 1 1 d . . .
C15 C 0.5828(3) 0.80494(12) 0.53614(17) 0.0128(4) Uani 1 1 d . . .
C16 C 0.4893(3) 0.86610(12) 0.50812(17) 0.0142(4) Uani 1 1 d . . .
H16 H 0.5529 0.9085 0.5242 0.017 Uiso 1 1 calc R . .
C17 C 0.3012(3) 0.86424(12) 0.45619(17) 0.0138(4) Uani 1 1 d . . .
C18 C 0.2118(3) 0.80147(12) 0.43312(18) 0.0153(4) Uani 1 1 d . . .
H18 H 0.0838 0.7991 0.3974 0.018 Uiso 1 1 calc R . .
C19 C 0.3133(3) 0.74271(12) 0.46329(18) 0.0142(4) Uani 1 1 d . . .
H19 H 0.2522 0.6998 0.4478 0.017 Uiso 1 1 calc R . .
C41 C 1.2046(4) 0.90890(12) 0.70882(18) 0.0168(5) Uani 1 1 d . . .
C42 C 0.1969(4) 0.92995(13) 0.4275(2) 0.0191(5) Uani 1 1 d . . .
N1 N 0.8519(3) 0.73672(10) 0.61002(15) 0.0133(4) Uani 1 1 d . . .
N2 N 0.4952(3) 0.74385(10) 0.51378(15) 0.0128(4) Uani 1 1 d . . .
O1 O 0.3495(3) 0.55755(10) 0.47558(16) 0.0273(4) Uani 1 1 d . . .
O2 O 0.9635(3) 0.54316(10) 0.60995(16) 0.0267(4) Uani 1 1 d . . .
O99 O 1.6310(3) 0.98867(11) 0.7887(2) 0.0457(7) Uani 1 1 d . . .
O411 O 1.1469(3) 0.96695(10) 0.70010(17) 0.0340(5) Uani 1 1 d . . .
O412 O 1.3832(3) 0.89099(9) 0.74724(15) 0.0265(4) Uani 1 1 d . . .
O421 O 0.2576(3) 0.98472(10) 0.45625(19) 0.0380(6) Uani 1 1 d . . .
O422 O 0.0317(3) 0.91976(9) 0.36976(17) 0.0307(5) Uani 1 1 d . . .
Br1 Br 0.51898(4) 0.651128(12) 0.725247(19) 0.01932(8) Uani 1 1 d . . .
Br2 Br 0.82727(4) 0.664891(13) 0.389539(18) 0.01985(8) Uani 1 1 d . . .
Ru1 Ru 0.66633(3) 0.655941(9) 0.555070(13) 0.01130(7) Uani 1 1 d . . .
H412 H 1.4660 0.9284 0.7666 0.050 Uiso 1 1 d . . .
H422 H -0.0277 0.9602 0.3520 0.050 Uiso 1 1 d . . .
H991 H 1.6131 1.0297 0.7852 0.050 Uiso 1 1 d . . .
H992 H 1.7515 0.9855 0.8093 0.050 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
C1 0.0301(14) 0.0132(11) 0.0137(12) 0.0024(9) 0.0035(10) 0.0133(10)
C2 0.0188(12) 0.0166(12) 0.0184(13) -0.0032(9) 0.0011(9) -0.0069(9)
C10 0.0152(11) 0.0147(11) 0.0159(12) -0.0004(8) -0.0013(8) 0.0028(8)
C11 0.0136(10) 0.0180(11) 0.0126(12) -0.0010(8) -0.0022(8) 0.0011(8)
C12 0.0155(11) 0.0150(11) 0.0106(12) -0.0016(8) -0.0005(9) -0.0011(8)
C13 0.0141(11) 0.0131(10) 0.0155(12) 0.0001(8) -0.0006(8) 0.0007(8)
C14 0.0120(10) 0.0144(11) 0.0117(11) 0.0000(8) 0.0008(8) -0.0003(8)
C15 0.0121(10) 0.0149(11) 0.0116(11) 0.0003(8) 0.0007(8) -0.0005(8)
C16 0.0139(10) 0.0130(11) 0.0157(12) 0.0001(8) 0.0000(8) -0.0006(8)
C17 0.0140(10) 0.0152(11) 0.0121(11) 0.0006(8) 0.0008(8) 0.0012(9)
C18 0.0126(10) 0.0174(11) 0.0157(12) 0.0016(9) -0.0019(8) -0.0002(9)
C19 0.0139(10) 0.0141(11) 0.0144(11) -0.0013(8) -0.0003(8) -0.0011(8)
C41 0.0175(11) 0.0175(11) 0.0149(12) -0.0005(9) -0.0044(9) -0.0011(9)
C42 0.0171(11) 0.0165(12) 0.0232(13) 0.0030(9) -0.0052(9) 0.0008(9)
N1 0.0134(9) 0.0129(9) 0.0135(10) -0.0012(7) -0.0004(7) -0.0001(7)
N2 0.0118(9) 0.0124(9) 0.0143(10) 0.0002(7) 0.0001(7) -0.0007(7)
O1 0.0208(9) 0.0216(10) 0.0394(12) 0.0028(8) -0.0018(8) -0.0006(8)
O2 0.0202(9) 0.0196(9) 0.0398(12) -0.0001(8) -0.0048(8) 0.0047(7)
O99 0.0283(11) 0.0209(11) 0.0853(19) -0.0014(11) -0.0238(11) -0.0050(9)
O411 0.0332(11) 0.0148(9) 0.0517(14) 0.0007(9) -0.0240(10) 0.0005(8)
O412 0.0187(9) 0.0176(9) 0.0419(12) -0.0059(8) -0.0135(8) 0.0000(7)
O421 0.0347(11) 0.0138(9) 0.0630(16) -0.0004(9) -0.0252(10) 0.0003(8)
O422 0.0269(10) 0.0159(9) 0.0471(13) 0.0015(8) -0.0210(9) 0.0030(8)
Br1 0.02165(14) 0.01869(13) 0.01798(15) 0.00228(8) 0.00471(10) 0.00357(9)
Br2 0.01855(13) 0.02479(14) 0.01644(14) -0.00292(9) 0.00324(9) -0.00516(9)
Ru1 0.01070(10) 0.01021(10) 0.01295(12) -0.00002(6) 0.00018(7) 0.00022(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Ru1 176.9(2) . . ?
O2 C2 Ru1 177.0(2) . . ?
N1 C10 C11 122.6(2) . . ?
N1 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C12 118.9(2) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 119.5(2) . . ?
C11 C12 C41 120.7(2) . . ?
C13 C12 C41 119.8(2) . . ?
C14 C13 C12 118.4(2) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
N1 C14 C13 121.7(2) . . ?
N1 C14 C15 115.20(19) . . ?
C13 C14 C15 123.1(2) . . ?
N2 C15 C16 121.6(2) . . ?
N2 C15 C14 114.82(19) . . ?
C16 C15 C14 123.6(2) . . ?
C17 C16 C15 118.9(2) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C18 119.4(2) . . ?
C16 C17 C42 119.4(2) . . ?
C18 C17 C42 121.2(2) . . ?
C19 C18 C17 118.6(2) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
N2 C19 C18 122.6(2) . . ?
N2 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
O411 C41 O412 124.4(2) . . ?
O411 C41 C12 123.7(2) . . ?
O412 C41 C12 111.9(2) . . ?
O421 C42 O422 125.1(2) . . ?
O421 C42 C17 122.9(2) . . ?
O422 C42 C17 112.0(2) . . ?
C10 N1 C14 118.9(2) . . ?
C10 N1 Ru1 124.54(16) . . ?
C14 N1 Ru1 116.56(15) . . ?
C19 N2 C15 118.9(2) . . ?
C19 N2 Ru1 124.51(16) . . ?
C15 N2 Ru1 116.50(15) . . ?
H991 O99 H992 103.1 . . ?
C41 O412 H412 113.3 . . ?
C42 O422 H422 110.7 . . ?
C2 Ru1 C1 90.76(10) . . ?
C2 Ru1 N1 97.00(9) . . ?
C1 Ru1 N1 172.03(8) . . ?
C2 Ru1 N2 172.87(9) . . ?
C1 Ru1 N2 95.54(8) . . ?
N1 Ru1 N2 76.82(8) . . ?
C2 Ru1 Br2 89.19(8) . . ?
C1 Ru1 Br2 92.14(7) . . ?
N1 Ru1 Br2 89.80(5) . . ?
N2 Ru1 Br2 87.26(5) . . ?
C2 Ru1 Br1 90.60(8) . . ?
C1 Ru1 Br1 90.88(7) . . ?
N1 Ru1 Br1 87.23(5) . . ?
N2 Ru1 Br1 92.62(5) . . ?
Br2 Ru1 Br1 176.972(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.070(3) . ?
C1 Ru1 1.928(3) . ?
C2 O2 1.117(3) . ?
C2 Ru1 1.902(3) . ?
C10 N1 1.344(3) . ?
C10 C11 1.380(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.400(3) . ?
C12 C41 1.499(3) . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
C14 N1 1.356(3) . ?
C14 C15 1.480(3) . ?
C15 N2 1.356(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.391(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(3) . ?
C17 C42 1.501(3) . ?
C18 C19 1.382(3) . ?
C18 H18 0.9500 . ?
C19 N2 1.347(3) . ?
C19 H19 0.9500 . ?
C41 O411 1.203(3) . ?
C41 O412 1.308(3) . ?
C42 O421 1.203(3) . ?
C42 O422 1.319(3) . ?
N1 Ru1 2.1107(19) . ?
N2 Ru1 2.1174(19) . ?
O99 H991 0.8140 . ?
O99 H992 0.8288 . ?
O412 H412 0.9425 . ?
O422 H422 0.9106 . ?
Br1 Ru1 2.5273(3) . ?
Br2 Ru1 2.5143(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O412 H412 O99 0.94 1.62 2.558(3) 171.9 .
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 C10 C11 C12 1.2(4) . . . . ?
C10 C11 C12 C13 0.3(4) . . . . ?
C10 C11 C12 C41 -179.2(2) . . . . ?
C11 C12 C13 C14 -1.1(3) . . . . ?
C41 C12 C13 C14 178.5(2) . . . . ?
C12 C13 C14 N1 0.4(3) . . . . ?
C12 C13 C14 C15 -179.9(2) . . . . ?
N1 C14 C15 N2 1.7(3) . . . . ?
C13 C14 C15 N2 -178.1(2) . . . . ?
N1 C14 C15 C16 -178.3(2) . . . . ?
C13 C14 C15 C16 2.0(4) . . . . ?
N2 C15 C16 C17 0.2(3) . . . . ?
C14 C15 C16 C17 -179.9(2) . . . . ?
C15 C16 C17 C18 -0.3(3) . . . . ?
C15 C16 C17 C42 178.7(2) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C42 C17 C18 C19 -178.7(2) . . . . ?
C17 C18 C19 N2 -0.2(4) . . . . ?
C11 C12 C41 O411 -174.9(3) . . . . ?
C13 C12 C41 O411 5.6(4) . . . . ?
C11 C12 C41 O412 5.8(3) . . . . ?
C13 C12 C41 O412 -173.7(2) . . . . ?
C16 C17 C42 O421 -8.1(4) . . . . ?
C18 C17 C42 O421 170.9(3) . . . . ?
C16 C17 C42 O422 173.2(2) . . . . ?
C18 C17 C42 O422 -7.8(3) . . . . ?
C11 C10 N1 C14 -1.9(3) . . . . ?
C11 C10 N1 Ru1 178.79(18) . . . . ?
C13 C14 N1 C10 1.0(3) . . . . ?
C15 C14 N1 C10 -178.7(2) . . . . ?
C13 C14 N1 Ru1 -179.57(17) . . . . ?
C15 C14 N1 Ru1 0.7(3) . . . . ?
C18 C19 N2 C15 0.1(3) . . . . ?
C18 C19 N2 Ru1 -176.39(18) . . . . ?
C16 C15 N2 C19 -0.1(3) . . . . ?
C14 C15 N2 C19 -180.0(2) . . . . ?
C16 C15 N2 Ru1 176.68(17) . . . . ?
C14 C15 N2 Ru1 -3.2(3) . . . . ?
O2 C2 Ru1 C1 139(4) . . . . ?
O2 C2 Ru1 N1 -43(4) . . . . ?
O2 C2 Ru1 N2 -14(5) . . . . ?
O2 C2 Ru1 Br2 47(4) . . . . ?
O2 C2 Ru1 Br1 -130(4) . . . . ?
O1 C1 Ru1 C2 160(4) . . . . ?
O1 C1 Ru1 N1 -7(5) . . . . ?
O1 C1 Ru1 N2 -24(4) . . . . ?
O1 C1 Ru1 Br2 -111(4) . . . . ?
O1 C1 Ru1 Br1 69(4) . . . . ?
C10 N1 Ru1 C2 -6.0(2) . . . . ?
C14 N1 Ru1 C2 174.58(17) . . . . ?
C10 N1 Ru1 C1 160.7(6) . . . . ?
C14 N1 Ru1 C1 -18.7(7) . . . . ?
C10 N1 Ru1 N2 177.6(2) . . . . ?
C14 N1 Ru1 N2 -1.81(16) . . . . ?
C10 N1 Ru1 Br2 -95.21(18) . . . . ?
C14 N1 Ru1 Br2 85.42(16) . . . . ?
C10 N1 Ru1 Br1 84.22(18) . . . . ?
C14 N1 Ru1 Br1 -95.15(16) . . . . ?
C19 N2 Ru1 C2 149.1(7) . . . . ?
C15 N2 Ru1 C2 -27.5(8) . . . . ?
C19 N2 Ru1 C1 -3.0(2) . . . . ?
C15 N2 Ru1 C1 -179.56(17) . . . . ?
C19 N2 Ru1 N1 179.3(2) . . . . ?
C15 N2 Ru1 N1 2.76(16) . . . . ?
C19 N2 Ru1 Br2 88.88(18) . . . . ?
C15 N2 Ru1 Br2 -87.67(16) . . . . ?
C19 N2 Ru1 Br1 -94.15(18) . . . . ?
C15 N2 Ru1 Br1 89.30(16) . . . . ?
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