Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_compound1 _database_code_CSD 188658 _journal_coden_Cambridge 0186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Li-Juan Zhang' 'Xiao-Li Zhao' 'Ji-Qing Xu' 'Tie-Gang Wang' __publ_contact_author_name 'Dr Li-Juan Zhang' _publ_contact_author_address ; Jiefang Road 119 Changchun CHINA ; _publ_contact_author_email 'zengzh@mail.jl.cn' _publ_requested_journal 'Journal of the Chemical Society, Dalton Transactions' _publ_section_title ; A novel two-dimensional structure containing first antimony-substituted polyoxovandium clusters: [{Co(en)2}2Sb¢ó8V¢ô14O42(H2O)].6H2O' ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H23 Co N4 O24.50 Sb4 V7' _chemical_formula_weight 1421.77 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' 'Co' 'Co' 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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' _cell_length_a 14.602(3) _cell_length_b 12.855(3) _cell_length_c 17.631(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.80(3) _cell_angle_gamma 90.00 _cell_volume 3184.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.48 _exptl_crystal_description rhombus _exptl_crystal_colour black _exptl_crystal_size_max 0.167 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.140 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2652 _exptl_absorpt_coefficient_mu 5.882 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8466 _exptl_absorpt_correction_T_max 1.1284 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Rugaku _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13804 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7297 _reflns_number_gt 5414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00128(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7297 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Sb1 Sb 0.28178(4) 0.70740(4) 0.08838(3) 0.01134(12) Uani 1 1 d . . . Sb2 Sb 0.14174(4) 0.71250(4) 0.22639(3) 0.01052(12) Uani 1 1 d . . . Sb3 Sb -0.08662(4) 0.77218(4) -0.18965(3) 0.01173(12) Uani 1 1 d . . . Sb4 Sb 0.22685(4) 0.22082(4) 0.05383(3) 0.01285(12) Uani 1 1 d . . . V1 V 0.26991(9) 0.46602(9) 0.00931(7) 0.0097(3) Uani 1 1 d . . . V2 V 0.22788(9) 0.45937(9) 0.17167(7) 0.0080(2) Uani 1 1 d . . . V3 V -0.08950(9) 0.71218(9) 0.12457(7) 0.0087(2) Uani 1 1 d . . . V4 V 0.15929(9) 0.49338(10) -0.15388(7) 0.0104(3) Uani 1 1 d . . . V5 V 0.13318(9) 0.69675(9) -0.09315(7) 0.0079(2) Uani 1 1 d . . . V6 V -0.04511(9) 0.52238(9) -0.22533(7) 0.0096(3) Uani 1 1 d . . . V7 V 0.03534(9) 0.79566(9) 0.02182(7) 0.0081(2) Uani 1 1 d . . . Co1 Co 0.23048(7) 0.88967(8) -0.20764(6) 0.0124(2) Uani 1 1 d . . . O1 O -0.0687(4) 0.5351(4) -0.3198(3) 0.0200(12) Uani 1 1 d . . . O2 O 0.0095(4) 0.7527(4) -0.0875(3) 0.0113(10) Uani 1 1 d . . . O3 O 0.2215(4) 0.4930(4) -0.2187(3) 0.0181(12) Uani 1 1 d . . . O4 O 0.2516(4) 0.7437(4) 0.1859(3) 0.0117(11) Uani 1 1 d . . . O5 O 0.3202(4) 0.4364(4) 0.2439(3) 0.0162(12) Uani 1 1 d . . . O6 O 0.2360(4) 0.3683(4) 0.0830(3) 0.0121(11) Uani 1 1 d . . . O7 O 0.2201(3) 0.5797(4) -0.0632(3) 0.0095(10) Uani 1 1 d . . . O8 O 0.0670(4) 0.6055(4) -0.1756(3) 0.0103(10) Uani 1 1 d . . . O9 O 0.3804(4) 0.4523(4) 0.0138(3) 0.0190(12) Uani 1 1 d . . . O10 O 0.1891(4) 0.1775(4) 0.1464(3) 0.0117(11) Uani 1 1 d . . . O11 O -0.1458(4) 0.4359(4) -0.2023(3) 0.0141(11) Uani 1 1 d . . . O12 O 0.0997(3) 0.2288(4) -0.0182(3) 0.0116(11) Uani 1 1 d . . . O13 O 0.1961(4) 0.3809(4) -0.0779(3) 0.0118(11) Uani 1 1 d . . . O14 O 0.0608(4) 0.9173(4) 0.0281(3) 0.0152(11) Uani 1 1 d . . . O15 O -0.1270(4) 0.7983(4) 0.1745(3) 0.0156(11) Uani 1 1 d . . . O16 O 0.0446(4) 0.7429(4) 0.1276(3) 0.0120(11) Uani 1 1 d . . . O17 O 0.1543(3) 0.7257(4) 0.0207(3) 0.0106(10) Uani 1 1 d . . . O18 O -0.1226(4) 0.6239(4) -0.1863(3) 0.0126(11) Uani 1 1 d . . . O19 O 0.0454(4) 0.4083(4) -0.1926(3) 0.0104(10) Uani 1 1 d . . . O20 O 0.1842(4) 0.7867(4) -0.1316(3) 0.0158(11) Uani 1 1 d . . . O21 O 0.2629(4) 0.5574(4) 0.0985(3) 0.0125(11) Uani 1 1 d . . . OW1 O 0.0000 0.5000 0.0000 0.173(10) Uani 1 2 d S . . OW2 O 0.4276(6) 0.6391(7) -0.0824(6) 0.074(3) Uani 1 1 d . . . OW3 O -0.2361(5) 0.5587(8) -0.4392(4) 0.064(3) Uani 1 1 d . . . OW4 O -0.0253(4) 0.9661(4) -0.1522(3) 0.0212(13) Uani 1 1 d . . . N1 N 0.3760(5) 0.8457(6) -0.1570(4) 0.0224(16) Uani 1 1 d . . . H1A H 0.3800 0.7768 -0.1474 0.080 Uiso 1 1 calc . . . H1B H 0.4110 0.8608 -0.1904 0.080 Uiso 1 1 calc . . . N2 N 0.2630(5) 1.0019(5) -0.1146(4) 0.0236(16) Uani 1 1 d . . . H2A H 0.2357 1.0634 -0.1317 0.080 Uiso 1 1 calc . . . H2B H 0.2418 0.9803 -0.0739 0.080 Uiso 1 1 calc . . . N3 N 0.0938(5) 0.9501(6) -0.2651(4) 0.0238(16) Uani 1 1 d . . . H3A H 0.0543 0.9414 -0.2343 0.080 Uiso 1 1 calc . . . H3B H 0.0981 1.0186 -0.2740 0.080 Uiso 1 1 calc . . . N4 N 0.1874(5) 0.7744(6) -0.2985(4) 0.0259(17) Uani 1 1 d . . . H4A H 0.2187 0.7839 -0.3354 0.080 Uiso 1 1 calc . . . H4B H 0.2011 0.7103 -0.2779 0.080 Uiso 1 1 calc . . . C1 C 0.4116(7) 0.9035(9) -0.0832(6) 0.041(3) Uani 1 1 d . . . H1C H 0.4803 0.9094 -0.0708 0.080 Uiso 1 1 calc . . . H1D H 0.3960 0.8661 -0.0406 0.080 Uiso 1 1 calc . . . C2 C 0.3676(8) 1.0118(8) -0.0905(6) 0.040(3) Uani 1 1 d . . . H2C H 0.3879 1.0477 -0.0403 0.080 Uiso 1 1 calc . . . H2D H 0.3883 1.0520 -0.1293 0.080 Uiso 1 1 calc . . . C3 C 0.0557(7) 0.8947(9) -0.3408(6) 0.040(3) Uani 1 1 d . . . H3C H -0.0131 0.8996 -0.3566 0.080 Uiso 1 1 calc . . . H3D H 0.0793 0.9277 -0.3813 0.080 Uiso 1 1 calc . . . C4 C 0.0840(7) 0.7845(8) -0.3341(6) 0.036(2) Uani 1 1 d . . . H4C H 0.0670 0.7529 -0.3860 0.080 Uiso 1 1 calc . . . H4D H 0.0500 0.7481 -0.3019 0.080 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0105(3) 0.0112(2) 0.0117(2) 0.00035(19) 0.00196(19) -0.00080(19) Sb2 0.0118(3) 0.0101(2) 0.0090(2) -0.00082(18) 0.00165(19) -0.00007(19) Sb3 0.0125(3) 0.0113(2) 0.0109(2) 0.00123(18) 0.0023(2) 0.00044(19) Sb4 0.0129(3) 0.0126(3) 0.0128(3) -0.00035(18) 0.0031(2) 0.0011(2) V1 0.0101(6) 0.0090(6) 0.0101(6) -0.0003(5) 0.0029(5) -0.0001(5) V2 0.0080(6) 0.0087(6) 0.0064(6) 0.0005(4) 0.0005(5) 0.0006(5) V3 0.0090(6) 0.0091(6) 0.0074(6) -0.0008(5) 0.0013(5) 0.0008(5) V4 0.0107(7) 0.0133(6) 0.0090(6) -0.0015(5) 0.0056(5) 0.0009(5) V5 0.0096(6) 0.0071(5) 0.0069(6) 0.0014(4) 0.0022(5) -0.0006(5) V6 0.0101(6) 0.0103(6) 0.0079(6) 0.0001(5) 0.0018(5) 0.0005(5) V7 0.0089(6) 0.0072(5) 0.0076(6) -0.0001(4) 0.0016(5) 0.0007(5) Co1 0.0124(6) 0.0142(5) 0.0113(5) 0.0012(4) 0.0047(4) -0.0009(4) O1 0.020(3) 0.027(3) 0.012(3) 0.003(2) 0.003(2) 0.001(3) O2 0.009(3) 0.014(2) 0.009(2) 0.000(2) 0.000(2) 0.004(2) O3 0.016(3) 0.025(3) 0.016(3) -0.005(2) 0.010(2) 0.000(2) O4 0.013(3) 0.013(2) 0.010(3) -0.002(2) 0.006(2) -0.003(2) O5 0.015(3) 0.017(3) 0.013(3) 0.002(2) -0.002(2) 0.002(2) O6 0.017(3) 0.010(2) 0.010(3) -0.001(2) 0.005(2) -0.002(2) O7 0.010(3) 0.010(2) 0.008(2) 0.0012(19) 0.001(2) 0.003(2) O8 0.013(3) 0.010(2) 0.009(2) 0.0009(19) 0.005(2) 0.000(2) O9 0.011(3) 0.027(3) 0.019(3) -0.001(2) 0.004(2) 0.001(2) O10 0.011(3) 0.013(3) 0.011(2) 0.003(2) 0.003(2) 0.000(2) O11 0.015(3) 0.009(2) 0.020(3) 0.000(2) 0.007(2) -0.001(2) O12 0.008(3) 0.017(3) 0.008(2) 0.002(2) 0.000(2) -0.002(2) O13 0.012(3) 0.011(2) 0.012(3) -0.001(2) 0.001(2) -0.002(2) O14 0.019(3) 0.008(2) 0.019(3) -0.001(2) 0.005(2) 0.001(2) O15 0.020(3) 0.012(3) 0.018(3) -0.004(2) 0.010(2) 0.000(2) O16 0.009(3) 0.018(3) 0.008(2) 0.000(2) 0.000(2) -0.001(2) O17 0.008(3) 0.012(2) 0.010(2) -0.0016(19) 0.000(2) 0.001(2) O18 0.009(3) 0.011(2) 0.019(3) 0.001(2) 0.007(2) -0.003(2) O19 0.010(3) 0.010(2) 0.011(2) -0.0001(19) 0.003(2) 0.001(2) O20 0.018(3) 0.013(3) 0.018(3) 0.004(2) 0.008(2) -0.004(2) O21 0.019(3) 0.008(2) 0.010(2) 0.0006(19) 0.002(2) -0.001(2) OW1 0.19(2) 0.21(2) 0.119(17) 0.018(17) 0.053(16) -0.06(2) OW2 0.044(5) 0.055(5) 0.129(8) 0.053(6) 0.031(5) 0.012(4) OW3 0.037(5) 0.124(8) 0.032(4) 0.020(5) 0.009(4) 0.031(5) OW4 0.023(3) 0.018(3) 0.021(3) 0.000(2) 0.005(3) 0.004(2) N1 0.019(4) 0.027(4) 0.022(4) 0.005(3) 0.008(3) -0.001(3) N2 0.034(5) 0.019(4) 0.016(4) -0.001(3) 0.005(3) -0.005(3) N3 0.019(4) 0.029(4) 0.025(4) 0.009(3) 0.008(3) -0.001(3) N4 0.023(4) 0.030(4) 0.026(4) -0.012(3) 0.010(3) -0.005(3) C1 0.029(6) 0.053(7) 0.029(5) 0.000(5) -0.009(4) -0.010(5) C2 0.041(6) 0.035(6) 0.036(6) -0.014(5) -0.005(5) -0.016(5) C3 0.021(5) 0.060(7) 0.034(6) 0.004(5) -0.002(4) 0.002(5) C4 0.031(6) 0.045(6) 0.028(5) -0.008(4) 0.003(4) -0.011(5) _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. ; 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 Sb1 O17 1.933(5) . ? Sb1 O4 1.944(5) . ? Sb1 O21 1.963(5) . ? Sb2 O11 1.958(5) 3_565 ? Sb2 O16 1.962(5) . ? Sb2 O4 1.966(5) . ? Sb3 O10 1.965(5) 3_565 ? Sb3 O2 1.974(5) . ? Sb3 O18 1.982(5) . ? Sb4 O10 1.941(5) . ? Sb4 O12 1.947(5) . ? Sb4 O6 1.960(5) . ? V1 O9 1.603(5) . ? V1 O7 1.947(5) . ? V1 O13 1.954(5) . ? V1 O6 1.965(5) . ? V1 O21 1.987(5) . ? V1 V4 2.912(2) . ? V1 V2 3.0878(17) . ? V2 O5 1.610(5) . ? V2 O18 1.947(5) 3_565 ? V2 O21 1.968(5) . ? V2 O11 1.974(5) 3_565 ? V2 O6 1.982(5) . ? V2 V6 3.0738(18) 3_565 ? V3 O15 1.601(5) . ? V3 O19 1.957(5) 3_565 ? V3 O13 1.959(5) 3_565 ? V3 O16 1.984(5) . ? V3 O12 1.990(5) 3_565 ? V3 V4 2.9283(18) 3_565 ? V3 V7 3.0910(18) . ? V4 O3 1.642(5) . ? V4 O8 1.938(5) . ? V4 O13 1.946(5) . ? V4 O7 1.949(5) . ? V4 O19 1.952(5) . ? V4 V5 2.8894(17) . ? V4 V3 2.9283(18) 3_565 ? V4 V6 2.930(2) . ? V5 O20 1.621(5) . ? V5 O8 1.913(5) . ? V5 O7 1.947(5) . ? V5 O2 1.972(5) . ? V5 O17 1.981(5) . ? V5 V7 3.0566(17) . ? V6 O1 1.614(5) . ? V6 O8 1.952(5) . ? V6 O19 1.954(5) . ? V6 O18 1.971(5) . ? V6 O11 1.971(5) . ? V6 V2 3.0738(18) 3_565 ? V7 O14 1.605(5) . ? V7 O2 1.941(5) . ? V7 O16 1.955(5) . ? V7 O17 1.961(5) . ? V7 O12 1.980(5) 3_565 ? Co1 O3 2.106(5) 2_554 ? Co1 O20 2.121(5) . ? Co1 N3 2.125(7) . ? Co1 N2 2.138(7) . ? Co1 N1 2.145(7) . ? Co1 N4 2.147(7) . ? O3 Co1 2.106(5) 2_544 ? O10 Sb3 1.965(5) 3_565 ? O11 Sb2 1.958(5) 3_565 ? O11 V2 1.974(5) 3_565 ? O12 V7 1.980(5) 3_565 ? O12 V3 1.990(5) 3_565 ? O13 V3 1.959(5) 3_565 ? O18 V2 1.947(5) 3_565 ? O19 V3 1.957(5) 3_565 ? N1 C1 1.465(12) . ? N2 C2 1.475(12) . ? N3 C3 1.481(12) . ? N4 C4 1.476(12) . ? C1 C2 1.524(15) . ? C3 C4 1.471(15) . ? 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 O17 Sb1 O4 96.0(2) . . ? O17 Sb1 O21 92.3(2) . . ? O4 Sb1 O21 94.8(2) . . ? O11 Sb2 O16 93.4(2) 3_565 . ? O11 Sb2 O4 92.5(2) 3_565 . ? O16 Sb2 O4 95.8(2) . . ? O10 Sb3 O2 96.6(2) 3_565 . ? O10 Sb3 O18 93.9(2) 3_565 . ? O2 Sb3 O18 88.8(2) . . ? O10 Sb4 O12 97.2(2) . . ? O10 Sb4 O6 94.1(2) . . ? O12 Sb4 O6 96.0(2) . . ? O9 V1 O7 107.8(2) . . ? O9 V1 O13 108.0(2) . . ? O7 V1 O13 82.9(2) . . ? O9 V1 O6 109.2(3) . . ? O7 V1 O6 142.9(2) . . ? O13 V1 O6 88.7(2) . . ? O9 V1 O21 107.1(3) . . ? O7 V1 O21 89.2(2) . . ? O13 V1 O21 144.8(2) . . ? O6 V1 O21 77.2(2) . . ? O9 V1 V4 110.0(2) . . ? O7 V1 V4 41.67(14) . . ? O13 V1 V4 41.58(15) . . ? O6 V1 V4 123.96(16) . . ? O21 V1 V4 125.17(15) . . ? O9 V1 V2 113.7(2) . . ? O7 V1 V2 119.77(15) . . ? O13 V1 V2 120.49(15) . . ? O6 V1 V2 38.72(14) . . ? O21 V1 V2 38.45(14) . . ? V4 V1 V2 136.26(6) . . ? O5 V2 O18 108.4(2) . 3_565 ? O5 V2 O21 108.9(2) . . ? O18 V2 O21 142.6(2) 3_565 . ? O5 V2 O11 110.4(2) . 3_565 ? O18 V2 O11 77.2(2) 3_565 3_565 ? O21 V2 O11 91.6(2) . 3_565 ? O5 V2 O6 107.4(2) . . ? O18 V2 O6 89.9(2) 3_565 . ? O21 V2 O6 77.2(2) . . ? O11 V2 O6 142.2(2) 3_565 . ? O5 V2 V6 112.4(2) . 3_565 ? O18 V2 V6 38.59(15) 3_565 3_565 ? O21 V2 V6 123.73(16) . 3_565 ? O11 V2 V6 38.79(15) 3_565 3_565 ? O6 V2 V6 122.08(16) . 3_565 ? O5 V2 V1 113.8(2) . . ? O18 V2 V1 120.07(16) 3_565 . ? O21 V2 V1 38.90(14) . . ? O11 V2 V1 121.60(16) 3_565 . ? O6 V2 V1 38.33(14) . . ? V6 V2 V1 133.76(6) 3_565 . ? O15 V3 O19 108.3(2) . 3_565 ? O15 V3 O13 107.5(3) . 3_565 ? O19 V3 O13 82.3(2) 3_565 3_565 ? O15 V3 O16 109.3(2) . . ? O19 V3 O16 89.0(2) 3_565 . ? O13 V3 O16 143.0(2) 3_565 . ? O15 V3 O12 107.8(2) . 3_565 ? O19 V3 O12 143.8(2) 3_565 3_565 ? O13 V3 O12 89.4(2) 3_565 3_565 ? O16 V3 O12 76.7(2) . 3_565 ? O15 V3 V4 109.82(19) . 3_565 ? O19 V3 V4 41.42(15) 3_565 3_565 ? O13 V3 V4 41.24(15) 3_565 3_565 ? O16 V3 V4 124.28(16) . 3_565 ? O12 V3 V4 124.75(15) 3_565 3_565 ? O15 V3 V7 115.28(19) . . ? O19 V3 V7 119.08(15) 3_565 . ? O13 V3 V7 119.60(15) 3_565 . ? O16 V3 V7 37.97(14) . . ? O12 V3 V7 38.76(15) 3_565 . ? V4 V3 V7 134.90(5) 3_565 . ? O3 V4 O8 110.5(2) . . ? O3 V4 O13 112.1(3) . . ? O8 V4 O13 137.4(2) . . ? O3 V4 O7 111.0(2) . . ? O8 V4 O7 82.9(2) . . ? O13 V4 O7 83.1(2) . . ? O3 V4 O19 109.5(2) . . ? O8 V4 O19 82.4(2) . . ? O13 V4 O19 82.8(2) . . ? O7 V4 O19 139.5(2) . . ? O3 V4 V5 114.5(2) . . ? O8 V4 V5 41.06(15) . . ? O13 V4 V5 117.19(15) . . ? O7 V4 V5 42.09(14) . . ? O19 V4 V5 116.81(15) . . ? O3 V4 V1 115.1(2) . . ? O8 V4 V1 117.01(15) . . ? O13 V4 V1 41.80(14) . . ? O7 V4 V1 41.62(14) . . ? O19 V4 V1 117.95(15) . . ? V5 V4 V1 80.61(5) . . ? O3 V4 V3 113.9(2) . 3_565 ? O8 V4 V3 116.70(15) . 3_565 ? O13 V4 V3 41.57(15) . 3_565 ? O7 V4 V3 118.13(15) . 3_565 ? O19 V4 V3 41.56(14) . 3_565 ? V5 V4 V3 131.58(5) . 3_565 ? V1 V4 V3 80.95(5) . 3_565 ? O3 V4 V6 113.1(2) . . ? O8 V4 V6 41.29(15) . . ? O13 V4 V6 116.68(16) . . ? O7 V4 V6 117.60(15) . . ? O19 V4 V6 41.40(15) . . ? V5 V4 V6 79.78(5) . . ? V1 V4 V6 131.77(6) . . ? V3 V4 V6 80.09(5) 3_565 . ? O20 V5 O8 108.3(2) . . ? O20 V5 O7 109.0(2) . . ? O8 V5 O7 83.6(2) . . ? O20 V5 O2 107.0(2) . . ? O8 V5 O2 89.0(2) . . ? O7 V5 O2 143.8(2) . . ? O20 V5 O17 109.1(2) . . ? O8 V5 O17 142.4(2) . . ? O7 V5 O17 87.7(2) . . ? O2 V5 O17 76.9(2) . . ? O20 V5 V4 111.60(19) . . ? O8 V5 V4 41.71(15) . . ? O7 V5 V4 42.16(15) . . ? O2 V5 V4 124.31(16) . . ? O17 V5 V4 123.06(15) . . ? O20 V5 V7 109.39(19) . . ? O8 V5 V7 121.94(16) . . ? O7 V5 V7 122.00(15) . . ? O2 V5 V7 38.28(14) . . ? O17 V5 V7 38.91(14) . . ? V4 V5 V7 139.01(5) . . ? O1 V6 O8 109.0(2) . . ? O1 V6 O19 108.5(3) . . ? O8 V6 O19 82.0(2) . . ? O1 V6 O18 108.2(3) . . ? O8 V6 O18 88.4(2) . . ? O19 V6 O18 143.2(2) . . ? O1 V6 O11 107.9(3) . . ? O8 V6 O11 142.9(2) . . ? O19 V6 O11 89.9(2) . . ? O18 V6 O11 76.7(2) . . ? O1 V6 V4 111.2(2) . . ? O8 V6 V4 40.94(14) . . ? O19 V6 V4 41.36(15) . . ? O18 V6 V4 123.27(16) . . ? O11 V6 V4 124.70(16) . . ? O1 V6 V2 110.5(2) . 3_565 ? O8 V6 V2 120.86(15) . 3_565 ? O19 V6 V2 122.75(15) . 3_565 ? O18 V6 V2 38.04(14) . 3_565 ? O11 V6 V2 38.84(15) . 3_565 ? V4 V6 V2 138.20(5) . 3_565 ? O14 V7 O2 109.0(2) . . ? O14 V7 O16 108.5(2) . . ? O2 V7 O16 142.5(2) . . ? O14 V7 O17 105.0(2) . . ? O2 V7 O17 78.0(2) . . ? O16 V7 O17 91.1(2) . . ? O14 V7 O12 111.5(2) . 3_565 ? O2 V7 O12 90.0(2) . 3_565 ? O16 V7 O12 77.6(2) . 3_565 ? O17 V7 O12 143.5(2) . 3_565 ? O14 V7 V5 108.04(19) . . ? O2 V7 V5 38.99(15) . . ? O16 V7 V5 124.42(16) . . ? O17 V7 V5 39.39(14) . . ? O12 V7 V5 123.62(15) 3_565 . ? O14 V7 V3 117.44(19) . . ? O2 V7 V3 119.79(16) . . ? O16 V7 V3 38.63(15) . . ? O17 V7 V3 120.80(15) . . ? O12 V7 V3 39.00(14) 3_565 . ? V5 V7 V3 134.50(5) . . ? O3 Co1 O20 178.9(2) 2_554 . ? O3 Co1 N3 84.4(2) 2_554 . ? O20 Co1 N3 96.3(2) . . ? O3 Co1 N2 90.3(2) 2_554 . ? O20 Co1 N2 88.8(2) . . ? N3 Co1 N2 95.9(3) . . ? O3 Co1 N1 88.0(2) 2_554 . ? O20 Co1 N1 91.3(2) . . ? N3 Co1 N1 172.2(3) . . ? N2 Co1 N1 82.6(3) . . ? O3 Co1 N4 93.1(2) 2_554 . ? O20 Co1 N4 87.8(2) . . ? N3 Co1 N4 81.4(3) . . ? N2 Co1 N4 175.4(3) . . ? N1 Co1 N4 100.6(3) . . ? V7 O2 V5 102.7(2) . . ? V7 O2 Sb3 140.1(3) . . ? V5 O2 Sb3 115.7(2) . . ? V4 O3 Co1 140.5(3) . 2_544 ? Sb1 O4 Sb2 132.6(3) . . ? Sb4 O6 V1 117.1(2) . . ? Sb4 O6 V2 139.8(3) . . ? V1 O6 V2 102.9(2) . . ? V5 O7 V1 149.0(3) . . ? V5 O7 V4 95.7(2) . . ? V1 O7 V4 96.7(2) . . ? V5 O8 V4 97.2(2) . . ? V5 O8 V6 149.9(3) . . ? V4 O8 V6 97.8(2) . . ? Sb4 O10 Sb3 130.7(3) . 3_565 ? Sb2 O11 V6 115.9(3) 3_565 . ? Sb2 O11 V2 141.3(3) 3_565 3_565 ? V6 O11 V2 102.4(2) . 3_565 ? Sb4 O12 V7 141.0(3) . 3_565 ? Sb4 O12 V3 116.6(2) . 3_565 ? V7 O12 V3 102.2(2) 3_565 3_565 ? V4 O13 V1 96.6(2) . . ? V4 O13 V3 97.2(2) . 3_565 ? V1 O13 V3 151.4(3) . 3_565 ? V7 O16 Sb2 139.6(3) . . ? V7 O16 V3 103.4(2) . . ? Sb2 O16 V3 117.0(2) . . ? Sb1 O17 V7 139.1(3) . . ? Sb1 O17 V5 117.4(2) . . ? V7 O17 V5 101.7(2) . . ? V2 O18 V6 103.4(2) 3_565 . ? V2 O18 Sb3 139.3(3) 3_565 . ? V6 O18 Sb3 116.4(2) . . ? V4 O19 V6 97.2(2) . . ? V4 O19 V3 97.0(2) . 3_565 ? V6 O19 V3 149.1(3) . 3_565 ? V5 O20 Co1 166.3(3) . . ? Sb1 O21 V2 139.2(3) . . ? Sb1 O21 V1 118.0(2) . . ? V2 O21 V1 102.6(2) . . ? C1 N1 Co1 107.9(6) . . ? C2 N2 Co1 106.0(5) . . ? C3 N3 Co1 109.1(6) . . ? C4 N4 Co1 108.3(5) . . ? N1 C1 C2 110.5(8) . . ? N2 C2 C1 109.0(8) . . ? C4 C3 N3 111.3(8) . . ? C3 C4 N4 110.6(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.743 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.434