#------------------------------------------------------------------------------
#$Date: 2019-12-03 02:02:11 +0200 (Tue, 03 Dec 2019) $
#$Revision: 244865 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/37/4133745.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4133745
loop_
_publ_author_name
'Cao, Jia-Peng'
'Xue, Yun-Shan'
'Li, Ning-Fang'
'Gong, Jun-Jie'
'Kang, Run-Kun'
'Xu, Yan'
_publ_section_title
;
 LA Dominant Windmill-Shaped V8 Clusters: A Bifunctional Heter-ogeneous
 Catalyst for CO2 Cycloaddition and Oxidation of Sulfides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11146
_journal_year                    2019
_chemical_formula_sum            'C16 H60 N8 O24 V8'
_chemical_formula_weight         1156.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                106.159(3)
_cell_angle_beta                 98.602(3)
_cell_angle_gamma                91.609(3)
_cell_formula_units_Z            2
_cell_length_a                   10.860(3)
_cell_length_b                   10.943(3)
_cell_length_c                   18.188(5)
_cell_measurement_reflns_used    8.5953
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.37
_cell_volume                     2047.2(10)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13786
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.182
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       spindle-shape
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7024
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0554P)²+15.8759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             7024
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b11146_si_002.cif
_cod_data_source_block           cjp-3
_cod_original_cell_volume        2047.1(10)
_cod_database_code               4133745
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.838
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 1.18568(10) 1.20000(11) 0.70351(7) 0.0240(3) Uani 1 1 d . . . . .
V2 V 1.45261(10) 1.20439(11) 0.83462(6) 0.0237(3) Uani 1 1 d . . . . .
V3 V 1.33782(10) 0.98300(11) 0.65986(6) 0.0234(3) Uani 1 1 d . . . . .
V4 V 1.56241(10) 0.93143(11) 0.77596(7) 0.0252(3) Uani 1 1 d . . . . .
V5 V 1.44945(11) 1.34006(11) 0.70221(7) 0.0260(3) Uani 1 1 d . . . . .
V6 V 1.08738(11) 0.84813(11) 0.68438(7) 0.0268(3) Uani 1 1 d . . . . .
V7 V 1.11915(11) 1.30022(12) 0.87396(7) 0.0289(3) Uani 1 1 d . . . . .
V8 V 1.24504(10) 1.03200(11) 0.83839(6) 0.0238(3) Uani 1 1 d . . . . .
O1 O 1.1794(4) 1.0287(4) 0.7031(3) 0.0245(10) Uani 1 1 d . . . . .
O2 O 1.3947(4) 1.0164(4) 0.7990(3) 0.0246(10) Uani 1 1 d . . . . .
O3 O 1.3634(4) 1.1615(4) 0.6983(3) 0.0258(10) Uani 1 1 d . . . . .
O4 O 1.2800(4) 1.2092(4) 0.8367(3) 0.0251(10) Uani 1 1 d . . . . .
O5 O 1.1649(4) 0.8827(4) 0.7934(3) 0.0286(10) Uani 1 1 d . . . . .
O6 O 1.4875(4) 0.9319(4) 0.6709(3) 0.0285(10) Uani 1 1 d . . . . .
O7 O 1.0735(4) 1.2630(5) 0.7599(3) 0.0283(10) Uani 1 1 d . . . . .
O8 O 1.4911(4) 1.3411(4) 0.8116(3) 0.0280(10) Uani 1 1 d . . . . .
O1T O 1.3012(5) 0.9674(5) 0.5682(3) 0.0345(11) Uani 1 1 d . . . . .
O2T O 1.5051(5) 1.2342(5) 0.9258(3) 0.0343(11) Uani 1 1 d . . . . .
O3T O 1.6976(5) 0.8779(5) 0.7666(3) 0.0393(13) Uani 1 1 d . . . . .
O4T O 1.0228(5) 0.7066(5) 0.6652(3) 0.0454(14) Uani 1 1 d . . . . .
O5T O 0.9958(5) 1.3585(6) 0.9029(3) 0.0482(14) Uani 1 1 d . . . . .
O6T O 1.2923(5) 1.0311(5) 0.9266(3) 0.0360(12) Uani 1 1 d . . . . .
O7T O 1.5023(5) 1.4800(5) 0.7034(3) 0.0409(13) Uani 1 1 d . . . . .
O8T O 1.1195(5) 1.1861(5) 0.6159(3) 0.0358(12) Uani 1 1 d . . . . .
O1A O 1.6043(4) 1.1193(4) 0.7989(3) 0.0281(10) Uani 1 1 d . . . . .
C1A C 1.7232(6) 1.1829(8) 0.8378(5) 0.0407(19) Uani 1 1 d . . . . .
H1AA H 1.721670 1.272309 0.842281 0.061 Uiso 1 1 calc R U . . .
H1AB H 1.740704 1.171143 0.888595 0.061 Uiso 1 1 calc R U . . .
H1AC H 1.786977 1.147712 0.808520 0.061 Uiso 1 1 calc R U . . .
O2A O 1.2558(4) 0.8121(4) 0.6545(3) 0.0277(10) Uani 1 1 d . . . . .
C2A C 1.2728(8) 0.7065(7) 0.5906(5) 0.0400(18) Uani 1 1 d . . . . .
H2AA H 1.359566 0.705372 0.585643 0.060 Uiso 1 1 calc R U . . .
H2AB H 1.245662 0.628434 0.599591 0.060 Uiso 1 1 calc R U . . .
H2AC H 1.224638 0.714964 0.543764 0.060 Uiso 1 1 calc R U . . .
O3A O 1.0854(4) 1.1144(5) 0.8617(3) 0.0301(11) Uani 1 1 d . . . . .
C3A C 1.0189(8) 1.0691(9) 0.9125(5) 0.046(2) Uani 1 1 d . . . . .
H3AA H 1.012623 0.977500 0.896837 0.069 Uiso 1 1 calc R U . . .
H3AB H 1.062778 1.100135 0.964726 0.069 Uiso 1 1 calc R U . . .
H3AC H 0.936625 1.099278 0.909872 0.069 Uiso 1 1 calc R U . . .
O4A O 1.2735(4) 1.3725(4) 0.7210(3) 0.0289(11) Uani 1 1 d . . . . .
C4A C 1.2058(7) 1.4679(8) 0.6951(5) 0.043(2) Uani 1 1 d . . . . .
H4AA H 1.259146 1.544694 0.707242 0.065 Uiso 1 1 calc R U . . .
H4AB H 1.178683 1.437528 0.640048 0.065 Uiso 1 1 calc R U . . .
H4AC H 1.134489 1.485157 0.720794 0.065 Uiso 1 1 calc R U . . .
N1 N 1.6029(6) 1.2322(6) 0.6697(4) 0.0340(14) Uani 1 1 d . . . . .
H1A H 1.671857 1.284367 0.681427 0.041 Uiso 1 1 calc R U . . .
H1B H 1.614332 1.175957 0.696796 0.041 Uiso 1 1 calc R U . . .
N2 N 1.3929(6) 1.2715(7) 0.5793(4) 0.0382(15) Uani 1 1 d . . . . .
H2A H 1.336367 1.205681 0.567760 0.046 Uiso 1 1 calc R U . . .
H2B H 1.358366 1.332799 0.561619 0.046 Uiso 1 1 calc R U . . .
C1 C 1.5831(9) 1.1649(10) 0.5872(5) 0.055(2) Uani 1 1 d . . . . .
H1C H 1.663161 1.156160 0.569435 0.066 Uiso 1 1 calc R U . . .
H1D H 1.545096 1.079916 0.579138 0.066 Uiso 1 1 calc R U . . .
C2 C 1.5036(9) 1.2312(10) 0.5419(5) 0.056(2) Uani 1 1 d . . . . .
H2C H 1.476527 1.175325 0.489850 0.067 Uiso 1 1 calc R U . . .
H2D H 1.550170 1.305510 0.538053 0.067 Uiso 1 1 calc R U . . .
N3 N 0.9324(5) 0.9521(6) 0.7139(4) 0.0323(14) Uani 1 1 d . . . . .
H3A H 0.880303 0.904234 0.729678 0.039 Uiso 1 1 calc R U . . .
H3B H 0.958658 1.021087 0.753408 0.039 Uiso 1 1 calc R U . . .
N4 N 1.0122(6) 0.8786(7) 0.5740(4) 0.0417(16) Uani 1 1 d . . . . .
H4A H 1.055004 0.943895 0.567072 0.050 Uiso 1 1 calc R U . . .
H4B H 1.018600 0.809372 0.535426 0.050 Uiso 1 1 calc R U . . .
C3 C 0.8644(8) 0.9918(10) 0.6493(5) 0.056(2) Uani 1 1 d . . . . .
H3C H 0.894222 1.078040 0.652928 0.067 Uiso 1 1 calc R U . . .
H3D H 0.776197 0.991756 0.652817 0.067 Uiso 1 1 calc R U . . .
C4 C 0.8820(9) 0.9052(10) 0.5738(5) 0.058(2) Uani 1 1 d . . . . .
H4C H 0.831350 0.825958 0.563402 0.069 Uiso 1 1 calc R U . . .
H4D H 0.854573 0.944076 0.532879 0.069 Uiso 1 1 calc R U . . .
N5 N 1.2283(6) 1.4691(6) 0.8831(4) 0.0374(15) Uani 1 1 d . . . . .
H5A H 1.266603 1.457155 0.841947 0.045 Uiso 1 1 calc R U . . .
H5B H 1.178458 1.532354 0.883213 0.045 Uiso 1 1 calc R U . . .
N6 N 1.2278(6) 1.3306(6) 0.9867(4) 0.0400(15) Uani 1 1 d . . . . .
H6A H 1.181108 1.310140 1.018395 0.048 Uiso 1 1 calc R U . . .
H6B H 1.291935 1.281629 0.983708 0.048 Uiso 1 1 calc R U . . .
C5 C 1.3238(9) 1.5061(9) 0.9554(5) 0.055(2) Uani 1 1 d . . . . .
H5C H 1.400099 1.465098 0.945493 0.065 Uiso 1 1 calc R U . . .
H5D H 1.343008 1.597754 0.971744 0.065 Uiso 1 1 calc R U . . .
C6 C 1.2737(9) 1.4661(9) 1.0170(5) 0.054(2) Uani 1 1 d . . . . .
H6C H 1.338702 1.477931 1.061743 0.065 Uiso 1 1 calc R U . . .
H6D H 1.206036 1.517758 1.033185 0.065 Uiso 1 1 calc R U . . .
N7 N 1.4607(6) 0.7579(6) 0.7660(3) 0.0320(13) Uani 1 1 d D . . . .
H7A H 1.386736 0.754997 0.736681 0.038 Uiso 0.78(3) 1 calc R U P A 1
H7B H 1.501464 0.693266 0.741830 0.038 Uiso 0.78(3) 1 calc R U P A 1
N8 N 1.5791(6) 0.9393(6) 0.8966(4) 0.0381(15) Uani 1 1 d D . . . .
H8A H 1.655826 0.968935 0.921229 0.046 Uiso 0.78(3) 1 calc R U P A 1
H8B H 1.524925 0.990843 0.919033 0.046 Uiso 0.78(3) 1 calc R U P A 1
C7 C 1.5523(13) 0.8070(10) 0.9003(7) 0.050(4) Uani 0.78(3) 1 d D . P A 1
H7C H 1.536085 0.809972 0.951813 0.060 Uiso 0.78(3) 1 calc R U P A 1
H7D H 1.624823 0.758729 0.891181 0.060 Uiso 0.78(3) 1 calc R U P A 1
C8 C 1.4410(13) 0.7407(13) 0.8409(5) 0.048(4) Uani 0.78(3) 1 d D . P A 1
H8C H 1.433887 0.650670 0.837451 0.058 Uiso 0.78(3) 1 calc R U P A 1
H8D H 1.364843 0.777694 0.855330 0.058 Uiso 0.78(3) 1 calc R U P A 1
C7A C 1.501(4) 0.839(2) 0.9113(18) 0.036(11) Uani 0.22(3) 1 d D U P A 2
H7AA H 1.417429 0.865438 0.916716 0.043 Uiso 0.22(3) 1 calc R U P A 2
H7AB H 1.537573 0.818108 0.957931 0.043 Uiso 0.22(3) 1 calc R U P A 2
C8A C 1.498(3) 0.727(3) 0.8402(10) 0.019(9) Uani 0.22(3) 1 d D U P A 2
H8AA H 1.580454 0.694171 0.840866 0.023 Uiso 0.22(3) 1 calc R U P A 2
H8AB H 1.440301 0.659136 0.842688 0.023 Uiso 0.22(3) 1 calc R U P A 2
O1B O 0.8885(10) 0.2870(8) 0.1293(5) 0.091(3) Uani 1 1 d D U . . .
H1BA H 0.895767 0.234055 0.153596 0.136 Uiso 1 1 calc R U . . .
C1B C 0.8439(16) 0.2260(12) 0.0516(6) 0.109(5) Uani 1 1 d D U . . .
H1BB H 0.888152 0.262100 0.019758 0.164 Uiso 1 1 calc R U . . .
H1BC H 0.756439 0.237165 0.040416 0.164 Uiso 1 1 calc R U . . .
H1BD H 0.856425 0.136698 0.040941 0.164 Uiso 1 1 calc R U . . .
C2B C 0.6560(13) 0.6206(12) 0.5972(6) 0.086(4) Uani 1 1 d D U . . .
H2BA H 0.586533 0.662220 0.617513 0.128 Uiso 0.20(4) 1 calc R U P B 1
H2BB H 0.716219 0.683348 0.593194 0.128 Uiso 0.20(4) 1 calc R U P B 1
H2BC H 0.693862 0.574250 0.631262 0.128 Uiso 0.20(4) 1 calc R U P B 1
H2BD H 0.590122 0.561273 0.598553 0.128 Uiso 0.80(4) 1 calc R U P B 2
H2BE H 0.623803 0.702396 0.600267 0.128 Uiso 0.80(4) 1 calc R U P B 2
H2BF H 0.721491 0.628354 0.640298 0.128 Uiso 0.80(4) 1 calc R U P B 2
O2B O 0.614(7) 0.536(4) 0.5236(18) 0.10(2) Uani 0.20(4) 1 d D U P B 1
O2C O 0.7030(18) 0.5767(13) 0.5281(6) 0.093(6) Uani 0.80(4) 1 d D U P B 2
O3B O 0.8596(7) 0.3542(10) 0.7003(6) 0.087(2) Uani 1 1 d D U . . .
H3BA H 0.923857 0.333358 0.722133 0.131 Uiso 0.51(2) 1 calc R U P C 1
H3BB H 0.917381 0.316390 0.715969 0.131 Uiso 0.49(2) 1 calc R U P C 2
C3B C 0.875(3) 0.355(3) 0.6250(10) 0.125(12) Uani 0.51(2) 1 d D U P C 1
H3BC H 0.845363 0.274288 0.588660 0.187 Uiso 0.51(2) 1 d R U P C 1
H3BD H 0.827553 0.420998 0.611380 0.187 Uiso 0.51(2) 1 d R U P C 1
H3BE H 0.961553 0.372688 0.623531 0.187 Uiso 0.51(2) 1 d R U P C 1
C3C C 0.854(2) 0.4728(16) 0.7567(11) 0.072(8) Uani 0.49(2) 1 d D U P C 2
H3CA H 0.812039 0.458518 0.796901 0.107 Uiso 0.49(2) 1 d R U P C 2
H3CB H 0.936359 0.510998 0.778761 0.107 Uiso 0.49(2) 1 d R U P C 2
H3CC H 0.807609 0.528838 0.732431 0.107 Uiso 0.49(2) 1 d R U P C 2
O4B O 0.8474(13) 0.7518(16) 0.8744(8) 0.079(4) Uani 0.556(12) 1 d D U P D 1
C4B C 0.847(4) 0.629(2) 0.823(2) 0.158(13) Uani 0.556(12) 1 d D U P D 1
H4BA H 0.804574 0.567337 0.841089 0.237 Uiso 0.556(12) 1 d R U P D 1
H4BB H 0.803455 0.628937 0.772829 0.237 Uiso 0.556(12) 1 d R U P D 1
H4BC H 0.930795 0.606877 0.818909 0.237 Uiso 0.556(12) 1 d R U P D 1
O5B O 0.9101(15) 0.4633(17) 0.5791(10) 0.075(5) Uani 0.444(12) 1 d D U P D 2
H5BA H 0.939034 0.517194 0.622297 0.112 Uiso 0.444(12) 1 d R U P D 2
C5B C 0.929(3) 0.531(3) 0.5258(17) 0.116(12) Uani 0.444(12) 1 d D U P D 2
H5BB H 0.900851 0.475393 0.474364 0.174 Uiso 0.444(12) 1 d R U P D 2
H5BC H 0.884751 0.606883 0.533134 0.174 Uiso 0.444(12) 1 d R U P D 2
H5BD H 1.016611 0.552213 0.532704 0.174 Uiso 0.444(12) 1 d R U P D 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'
V V 0.3005 0.5294 '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
O8T V1 O7 104.1(2) . .
O8T V1 O1 100.3(2) . .
O7 V1 O1 103.0(2) . .
O8T V1 O3 106.5(2) . .
O7 V1 O3 148.4(2) . .
O1 V1 O3 79.03(19) . .
O8T V1 O4A 95.7(2) . .
O7 V1 O4A 92.9(2) . .
O1 V1 O4A 153.8(2) . .
O3 V1 O4A 76.59(19) . .
O8T V1 O4 176.6(2) . .
O7 V1 O4 75.40(18) . .
O1 V1 O4 76.59(17) . .
O3 V1 O4 74.48(17) . .
O4A V1 O4 87.65(17) . .
O8T V1 V3 94.62(19) . .
O7 V1 V3 144.36(16) . .
O1 V1 V3 43.05(14) . .
O3 V1 V3 39.51(13) . .
O4A V1 V3 115.37(14) . .
O4 V1 V3 84.11(11) . .
O2T V2 O8 105.0(2) . .
O2T V2 O4 100.2(2) . .
O8 V2 O4 103.8(2) . .
O2T V2 O1A 95.4(2) . .
O8 V2 O1A 93.0(2) . .
O4 V2 O1A 153.0(2) . .
O2T V2 O2 105.0(2) . .
O8 V2 O2 149.0(2) . .
O4 V2 O2 78.04(19) . .
O1A V2 O2 76.75(18) . .
O2T V2 O3 177.3(2) . .
O8 V2 O3 75.48(19) . .
O4 V2 O3 77.06(18) . .
O1A V2 O3 87.20(17) . .
O2 V2 O3 74.88(17) . .
O2T V2 V8 93.89(19) . .
O8 V2 V8 144.21(16) . .
O4 V2 V8 42.02(14) . .
O1A V2 V8 115.46(14) . .
O2 V2 V8 39.35(13) . .
O3 V2 V8 84.34(11) . .
O1T V3 O6 104.8(2) . .
O1T V3 O3 100.2(2) . .
O6 V3 O3 103.5(2) . .
O1T V3 O1 104.7(2) . .
O6 V3 O1 149.5(2) . .
O3 V3 O1 78.40(19) . .
O1T V3 O2A 95.1(2) . .
O6 V3 O2A 93.5(2) . .
O3 V3 O2A 153.3(2) . .
O1 V3 O2A 76.56(19) . .
O1T V3 O2 177.5(2) . .
O6 V3 O2 75.77(19) . .
O3 V3 O2 77.34(18) . .
O1 V3 O2 75.05(16) . .
O2A V3 O2 87.25(17) . .
O1T V3 V1 93.37(18) . .
O6 V3 V1 144.64(17) . .
O3 V3 V1 42.54(14) . .
O1 V3 V1 39.35(13) . .
O2A V3 V1 115.17(14) . .
O2 V3 V1 84.92(11) . .
O3T V4 O6 104.6(2) . .
O3T V4 O1A 100.7(2) . .
O6 V4 O1A 87.57(19) . .
O3T V4 O2 173.9(3) . .
O6 V4 O2 79.84(19) . .
O1A V4 O2 75.11(18) . .
O3T V4 N7 98.9(3) . .
O6 V4 N7 92.2(2) . .
O1A V4 N7 159.8(2) . .
O2 V4 N7 85.0(2) . .
O3T V4 N8 94.6(3) . .
O6 V4 N8 160.3(2) . .
O1A V4 N8 93.5(2) . .
O2 V4 N8 81.4(2) . .
N7 V4 N8 80.1(2) . .
O7T V5 O8 103.1(2) . .
O7T V5 O4A 101.3(2) . .
O8 V5 O4A 87.7(2) . .
O7T V5 O3 174.8(2) . .
O8 V5 O3 78.88(18) . .
O4A V5 O3 73.81(18) . .
O7T V5 N1 100.3(3) . .
O8 V5 N1 93.0(2) . .
O4A V5 N1 157.6(2) . .
O3 V5 N1 84.4(2) . .
O7T V5 N2 96.0(3) . .
O8 V5 N2 160.5(2) . .
O4A V5 N2 92.7(2) . .
O3 V5 N2 82.5(2) . .
N1 V5 N2 79.3(2) . .
O4T V6 O5 102.4(3) . .
O4T V6 O2A 101.6(3) . .
O5 V6 O2A 88.5(2) . .
O4T V6 O1 175.9(3) . .
O5 V6 O1 79.68(18) . .
O2A V6 O1 74.92(18) . .
O4T V6 N3 98.6(3) . .
O5 V6 N3 92.5(2) . .
O2A V6 N3 159.1(2) . .
O1 V6 N3 84.7(2) . .
O4T V6 N4 95.9(3) . .
O5 V6 N4 160.8(2) . .
O2A V6 N4 93.3(2) . .
O1 V6 N4 82.3(2) . .
N3 V6 N4 79.1(3) . .
O5T V7 O7 101.7(3) . .
O5T V7 O3A 102.1(3) . .
O7 V7 O3A 88.4(2) . .
O5T V7 N5 100.8(3) . .
O7 V7 N5 92.5(2) . .
O3A V7 N5 156.4(2) . .
O5T V7 O4 175.7(3) . .
O7 V7 O4 79.25(18) . .
O3A V7 O4 73.70(18) . .
N5 V7 O4 83.3(2) . .
O5T V7 N6 96.6(3) . .
O7 V7 N6 161.1(2) . .
O3A V7 N6 92.2(2) . .
N5 V7 N6 79.6(3) . .
O4 V7 N6 82.8(2) . .
O6T V8 O5 104.8(2) . .
O6T V8 O2 101.0(2) . .
O5 V8 O2 103.1(2) . .
O6T V8 O4 105.6(2) . .
O5 V8 O4 148.3(2) . .
O2 V8 O4 79.79(19) . .
O6T V8 O3A 94.4(2) . .
O5 V8 O3A 92.1(2) . .
O2 V8 O3A 154.8(2) . .
O4 V8 O3A 76.84(19) . .
O6T V8 O1 178.0(2) . .
O5 V8 O1 74.80(18) . .
O2 V8 O1 77.25(17) . .
O4 V8 O1 75.17(17) . .
O3A V8 O1 87.63(17) . .
O6T V8 V2 94.59(19) . .
O5 V8 V2 144.82(17) . .
O2 V8 V2 43.57(14) . .
O4 V8 V2 39.66(13) . .
O3A V8 V2 115.77(15) . .
O1 V8 V2 84.80(11) . .
V1 O1 V3 97.60(19) . .
V1 O1 V6 153.7(2) . .
V3 O1 V6 102.1(2) . .
V1 O1 V8 105.4(2) . .
V3 O1 V8 100.73(18) . .
V6 O1 V8 88.00(16) . .
V8 O2 V2 97.1(2) . .
V8 O2 V4 154.7(2) . .
V2 O2 V4 101.53(19) . .
V8 O2 V3 105.87(19) . .
V2 O2 V3 100.80(18) . .
V4 O2 V3 87.43(16) . .
V3 O3 V1 98.0(2) . .
V3 O3 V5 152.6(3) . .
V1 O3 V5 102.7(2) . .
V3 O3 V2 105.49(19) . .
V1 O3 V2 102.19(19) . .
V5 O3 V2 87.58(16) . .
V2 O4 V8 98.3(2) . .
V2 O4 V7 153.0(3) . .
V8 O4 V7 102.7(2) . .
V2 O4 V1 104.78(19) . .
V8 O4 V1 101.71(19) . .
V7 O4 V1 87.48(16) . .
V8 O5 V6 117.3(2) . .
V3 O6 V4 116.7(3) . .
V1 O7 V7 117.5(2) . .
V2 O8 V5 117.6(2) . .
C1A O1A V4 124.2(4) . .
C1A O1A V2 116.3(4) . .
V4 O1A V2 105.7(2) . .
O1A C1A H1AA 109.5 . .
O1A C1A H1AB 109.5 . .
H1AA C1A H1AB 109.5 . .
O1A C1A H1AC 109.5 . .
H1AA C1A H1AC 109.5 . .
H1AB C1A H1AC 109.5 . .
C2A O2A V6 122.0(4) . .
C2A O2A V3 116.7(4) . .
V6 O2A V3 105.7(2) . .
O2A C2A H2AA 109.5 . .
O2A C2A H2AB 109.5 . .
H2AA C2A H2AB 109.5 . .
O2A C2A H2AC 109.5 . .
H2AA C2A H2AC 109.5 . .
H2AB C2A H2AC 109.5 . .
C3A O3A V7 122.5(5) . .
C3A O3A V8 116.7(4) . .
V7 O3A V8 106.1(2) . .
O3A C3A H3AA 109.5 . .
O3A C3A H3AB 109.5 . .
H3AA C3A H3AB 109.5 . .
O3A C3A H3AC 109.5 . .
H3AA C3A H3AC 109.5 . .
H3AB C3A H3AC 109.5 . .
C4A O4A V1 118.7(4) . .
C4A O4A V5 121.9(4) . .
V1 O4A V5 106.0(2) . .
O4A C4A H4AA 109.5 . .
O4A C4A H4AB 109.5 . .
H4AA C4A H4AB 109.5 . .
O4A C4A H4AC 109.5 . .
H4AA C4A H4AC 109.5 . .
H4AB C4A H4AC 109.5 . .
C1 N1 V5 112.1(5) . .
C1 N1 H1A 109.2 . .
V5 N1 H1A 109.2 . .
C1 N1 H1B 109.2 . .
V5 N1 H1B 109.2 . .
H1A N1 H1B 107.9 . .
C2 N2 V5 109.4(5) . .
C2 N2 H2A 109.8 . .
V5 N2 H2A 109.8 . .
C2 N2 H2B 109.8 . .
V5 N2 H2B 109.8 . .
H2A N2 H2B 108.2 . .
C2 C1 N1 111.9(8) . .
C2 C1 H1C 109.2 . .
N1 C1 H1C 109.2 . .
C2 C1 H1D 109.2 . .
N1 C1 H1D 109.2 . .
H1C C1 H1D 107.9 . .
C1 C2 N2 109.9(7) . .
C1 C2 H2C 109.7 . .
N2 C2 H2C 109.7 . .
C1 C2 H2D 109.7 . .
N2 C2 H2D 109.7 . .
H2C C2 H2D 108.2 . .
C3 N3 V6 113.2(5) . .
C3 N3 H3A 108.9 . .
V6 N3 H3A 108.9 . .
C3 N3 H3B 108.9 . .
V6 N3 H3B 108.9 . .
H3A N3 H3B 107.8 . .
C4 N4 V6 108.8(5) . .
C4 N4 H4A 109.9 . .
V6 N4 H4A 109.9 . .
C4 N4 H4B 109.9 . .
V6 N4 H4B 109.9 . .
H4A N4 H4B 108.3 . .
N3 C3 C4 111.0(8) . .
N3 C3 H3C 109.4 . .
C4 C3 H3C 109.4 . .
N3 C3 H3D 109.4 . .
C4 C3 H3D 109.4 . .
H3C C3 H3D 108.0 . .
N4 C4 C3 110.8(7) . .
N4 C4 H4C 109.5 . .
C3 C4 H4C 109.5 . .
N4 C4 H4D 109.5 . .
C3 C4 H4D 109.5 . .
H4C C4 H4D 108.1 . .
C5 N5 V7 111.7(5) . .
C5 N5 H5A 109.3 . .
V7 N5 H5A 109.3 . .
C5 N5 H5B 109.3 . .
V7 N5 H5B 109.3 . .
H5A N5 H5B 107.9 . .
C6 N6 V7 108.7(5) . .
C6 N6 H6A 109.9 . .
V7 N6 H6A 109.9 . .
C6 N6 H6B 109.9 . .
V7 N6 H6B 109.9 . .
H6A N6 H6B 108.3 . .
C6 C5 N5 108.9(8) . .
C6 C5 H5C 109.9 . .
N5 C5 H5C 109.9 . .
C6 C5 H5D 109.9 . .
N5 C5 H5D 109.9 . .
H5C C5 H5D 108.3 . .
N6 C6 C5 108.9(7) . .
N6 C6 H6C 109.9 . .
C5 C6 H6C 109.9 . .
N6 C6 H6D 109.9 . .
C5 C6 H6D 109.9 . .
H6C C6 H6D 108.3 . .
C8 N7 V4 113.8(6) . .
C8A N7 V4 106.6(14) . .
C8 N7 H7A 108.8 . .
V4 N7 H7A 108.8 . .
C8 N7 H7B 108.8 . .
V4 N7 H7B 108.8 . .
H7A N7 H7B 107.7 . .
C7A N8 V4 113.8(14) . .
C7 N8 V4 107.3(6) . .
C7 N8 H8A 110.3 . .
V4 N8 H8A 110.3 . .
C7 N8 H8B 110.3 . .
V4 N8 H8B 110.3 . .
H8A N8 H8B 108.5 . .
N8 C7 C8 111.3(8) . .
N8 C7 H7C 109.4 . .
C8 C7 H7C 109.4 . .
N8 C7 H7D 109.4 . .
C8 C7 H7D 109.4 . .
H7C C7 H7D 108.0 . .
N7 C8 C7 107.2(9) . .
N7 C8 H8C 110.3 . .
C7 C8 H8C 110.3 . .
N7 C8 H8D 110.3 . .
C7 C8 H8D 110.3 . .
H8C C8 H8D 108.5 . .
N8 C7A C8A 104(2) . .
N8 C7A H7AA 111.0 . .
C8A C7A H7AA 111.0 . .
N8 C7A H7AB 111.0 . .
C8A C7A H7AB 111.0 . .
H7AA C7A H7AB 109.0 . .
N7 C8A C7A 114(2) . .
N7 C8A H8AA 108.9 . .
C7A C8A H8AA 108.9 . .
N7 C8A H8AB 108.9 . .
C7A C8A H8AB 108.9 . .
H8AA C8A H8AB 107.7 . .
C1B O1B H1BA 109.5 . .
O1B C1B H1BB 109.5 . .
O1B C1B H1BC 109.5 . .
H1BB C1B H1BC 109.5 . .
O1B C1B H1BD 109.5 . .
H1BB C1B H1BD 109.5 . .
H1BC C1B H1BD 109.5 . .
O2B C2B H2BA 109.5 . .
O2B C2B H2BB 109.5 . .
H2BA C2B H2BB 109.5 . .
O2B C2B H2BC 109.5 . .
H2BA C2B H2BC 109.5 . .
H2BB C2B H2BC 109.5 . .
O2C C2B H2BD 109.5 . .
O2C C2B H2BE 109.5 . .
H2BD C2B H2BE 109.5 . .
O2C C2B H2BF 109.5 . .
H2BD C2B H2BF 109.5 . .
H2BE C2B H2BF 109.5 . .
C3B O3B H3BA 109.5 . .
C3C O3B H3BB 109.5 . .
O3B C3B H3BC 109.8 . .
O3B C3B H3BD 108.8 . .
H3BC C3B H3BD 109.5 . .
O3B C3B H3BE 109.8 . .
H3BC C3B H3BE 109.5 . .
H3BD C3B H3BE 109.5 . .
O3B C3C H3CA 109.2 . .
O3B C3C H3CB 109.9 . .
H3CA C3C H3CB 109.5 . .
O3B C3C H3CC 109.3 . .
H3CA C3C H3CC 109.5 . .
H3CB C3C H3CC 109.5 . .
O4B C4B H4BA 110.2 . .
O4B C4B H4BB 108.5 . .
H4BA C4B H4BB 109.5 . .
O4B C4B H4BC 109.6 . .
H4BA C4B H4BC 109.5 . .
H4BB C4B H4BC 109.5 . .
C5B O5B H5BA 102.3 . .
O5B C5B C5B 110(3) . 2_766
O5B C5B H5BB 108.4 . .
C5B C5B H5BB 69.0 2_766 .
O5B C5B H5BC 112.8 . .
C5B C5B H5BC 134.3 2_766 .
H5BB C5B H5BC 109.5 . .
O5B C5B H5BD 107.2 . .
C5B C5B H5BD 42.0 2_766 .
H5BB C5B H5BD 109.5 . .
H5BC C5B H5BD 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O8T 1.610(5) .
V1 O7 1.743(5) .
V1 O1 1.872(4) .
V1 O3 1.997(5) .
V1 O4A 2.012(5) .
V1 O4 2.459(5) .
V1 V3 2.9260(17) .
V2 O2T 1.608(5) .
V2 O8 1.718(5) .
V2 O4 1.883(5) .
V2 O1A 2.018(5) .
V2 O2 2.028(5) .
V2 O3 2.431(5) .
V2 V8 2.9196(17) .
V3 O1T 1.615(5) .
V3 O6 1.735(5) .
V3 O3 1.880(5) .
V3 O1 2.015(5) .
V3 O2A 2.020(5) .
V3 O2 2.434(5) .
V4 O3T 1.611(5) .
V4 O6 1.964(5) .
V4 O1A 2.005(5) .
V4 O2 2.113(5) .
V4 N7 2.119(6) .
V4 N8 2.152(6) .
V5 O7T 1.614(5) .
V5 O8 1.971(5) .
V5 O4A 2.015(5) .
V5 O3 2.121(5) .
V5 N1 2.130(6) .
V5 N2 2.137(6) .
V6 O4T 1.605(5) .
V6 O5 1.963(5) .
V6 O2A 2.003(5) .
V6 O1 2.105(5) .
V6 N3 2.110(6) .
V6 N4 2.169(6) .
V7 O5T 1.597(6) .
V7 O7 1.982(5) .
V7 O3A 2.000(5) .
V7 N5 2.120(6) .
V7 O4 2.139(5) .
V7 N6 2.140(6) .
V8 O6T 1.612(5) .
V8 O5 1.749(5) .
V8 O2 1.865(4) .
V8 O4 1.975(5) .
V8 O3A 2.023(5) .
V8 O1 2.447(5) .
O1A C1A 1.434(8) .
C1A H1AA 0.9600 .
C1A H1AB 0.9600 .
C1A H1AC 0.9600 .
O2A C2A 1.431(9) .
C2A H2AA 0.9600 .
C2A H2AB 0.9600 .
C2A H2AC 0.9600 .
O3A C3A 1.433(8) .
C3A H3AA 0.9600 .
C3A H3AB 0.9600 .
C3A H3AC 0.9600 .
O4A C4A 1.436(8) .
C4A H4AA 0.9600 .
C4A H4AB 0.9600 .
C4A H4AC 0.9600 .
N1 C1 1.455(10) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N2 C2 1.486(11) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
C1 C2 1.452(13) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 H2C 0.9700 .
C2 H2D 0.9700 .
N3 C3 1.469(10) .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N4 C4 1.451(12) .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
C3 C4 1.478(14) .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 H4C 0.9700 .
C4 H4D 0.9700 .
N5 C5 1.497(10) .
N5 H5A 0.8900 .
N5 H5B 0.8900 .
N6 C6 1.474(11) .
N6 H6A 0.8900 .
N6 H6B 0.8900 .
C5 C6 1.479(13) .
C5 H5C 0.9700 .
C5 H5D 0.9700 .
C6 H6C 0.9700 .
C6 H6D 0.9700 .
N7 C8 1.471(8) .
N7 C8A 1.486(10) .
N7 H7A 0.8900 .
N7 H7B 0.8900 .
N8 C7A 1.476(10) .
N8 C7 1.491(8) .
N8 H8A 0.8900 .
N8 H8B 0.8900 .
C7 C8 1.510(9) .
C7 H7C 0.9700 .
C7 H7D 0.9700 .
C8 H8C 0.9700 .
C8 H8D 0.9700 .
C7A C8A 1.512(10) .
C7A H7AA 0.9700 .
C7A H7AB 0.9700 .
C8A H8AA 0.9700 .
C8A H8AB 0.9700 .
O1B C1B 1.389(9) .
O1B H1BA 0.8200 .
C1B H1BB 0.9600 .
C1B H1BC 0.9600 .
C1B H1BD 0.9600 .
C2B O2C 1.393(9) .
C2B O2B 1.399(10) .
C2B H2BA 0.9600 .
C2B H2BB 0.9600 .
C2B H2BC 0.9600 .
C2B H2BD 0.9600 .
C2B H2BE 0.9600 .
C2B H2BF 0.9600 .
O3B C3B 1.409(10) .
O3B C3C 1.423(10) .
O3B H3BA 0.8200 .
O3B H3BB 0.8200 .
C3B H3BC 0.9600 .
C3B H3BD 0.9601 .
C3B H3BE 0.9602 .
C3C H3CA 0.9594 .
C3C H3CB 0.9599 .
C3C H3CC 0.9601 .
O4B C4B 1.409(10) .
C4B H4BA 0.9599 .
C4B H4BB 0.9599 .
C4B H4BC 0.9603 .
O5B C5B 1.403(10) .
O5B H5BA 0.8497 .
C5B C5B 1.97(7) 2_766
C5B H5BB 0.9600 .
C5B H5BC 0.9599 .
C5B H5BD 0.9600 .
