#------------------------------------------------------------------------------ #$Date: 2016-05-14 06:25:04 +0300 (Sat, 14 May 2016) $ #$Revision: 182955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/52/7225236.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7225236 loop_ _publ_author_name 'Cui, Xiaobing' 'guo, haiyang' 'Zhang, Xiao' 'Huo, Qisheng' 'Xu, Ji-Qing' _publ_section_title ; Vanadoantimonates: from discrete clusters to high dimensional aggregates ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C6CE00616G _journal_year 2016 _chemical_formula_sum 'C12 H62 N12 Ni2 O48 Sb6 V15' _chemical_formula_weight 2754.75 _space_group_crystal_system trigonal _space_group_IT_number 146 _space_group_name_Hall 'R 3' _space_group_name_H-M_alt 'R 3 :H' _symmetry_space_group_name_Hall 'R 3' _symmetry_space_group_name_H-M 'R 3 :H' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-04-26 deposited with the CCDC. 2016-05-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 12.4887(7) _cell_length_b 12.4887(7) _cell_length_c 39.986(5) _cell_measurement_reflns_used 9937 _cell_measurement_temperature 292(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 2.77 _cell_volume 5401.0(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 292(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1301 _diffrn_reflns_av_unetI/netI 0.0875 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_number 17120 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.290 _diffrn_reflns_theta_min 2.141 _exptl_absorpt_coefficient_mu 4.656 _exptl_absorpt_correction_T_max 0.703 _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.541 _exptl_crystal_description polyhedron _exptl_crystal_F_000 3927 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.120 _refine_diff_density_max 3.827 _refine_diff_density_min -1.652 _refine_diff_density_rms 0.369 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.26(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 5859 _refine_ls_number_restraints 19 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0890 _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/[\s^2^(Fo^2^)+(0.1449P)^2^+364.4051P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2245 _refine_ls_wR_factor_ref 0.2432 _reflns_Friedel_coverage 1.000 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 5296 _reflns_number_total 5859 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00616g2.cif _cod_data_source_block shelx_2 _cod_original_cell_volume 5401.0(9) _cod_database_code 7225236 _shelx_shelxl_version_number 2014/7 _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 0.285 _shelx_estimated_absorpt_t_max 0.605 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL k in R3 CELL 0.71073 12.4887 12.4887 39.9863 90.000 90.000 120.000 ZERR 3.00 0.0007 0.0007 0.0046 0.000 0.000 0.000 LATT -3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O V NI SB UNIT 36 186 36 144 45 6 18 TEMP 19.180 L.S. 14 BOND FMAP 2 PLAN 10 TWIN acta size 0.36*0.12*0.12 acta ISOR 0.001 c3 c4 n4 WGHT 0.144900 364.405090 BASF 0.26040 FVAR 0.07589 SB1 7 0.397696 0.027014 0.295459 11.00000 0.01682 0.02905 = 0.01794 0.00298 0.00068 0.01269 SB2 7 0.212853 -0.232669 0.244074 11.00000 0.02703 0.02565 = 0.01809 0.00226 0.00447 0.01861 V5 5 0.144151 0.189693 0.193461 11.00000 0.01582 0.01491 = 0.01436 0.00075 -0.00071 0.00562 V4 5 0.193955 0.062981 0.343542 11.00000 0.01243 0.01626 = 0.01276 0.00180 -0.00072 0.00707 V3 5 0.205798 0.291542 0.324038 11.00000 0.01790 0.01494 = 0.01554 -0.00235 -0.00318 0.00623 V2 5 0.290026 0.076716 0.213765 11.00000 0.01624 0.02138 = 0.01540 -0.00013 0.00400 0.00908 V1 5 0.351686 0.261274 0.268604 11.00000 0.01429 0.01685 = 0.01446 0.00120 -0.00158 0.00398 NI2 6 0.000000 0.000000 0.080691 10.33333 0.02131 0.02131 = 0.02210 0.00000 0.00000 0.01065 NI1 6 0.333333 0.666667 0.119391 10.33333 0.02373 0.02373 = 0.01532 0.00000 0.00000 0.01187 O14 4 0.044800 -0.097519 0.348308 11.00000 0.01471 0.01338 = 0.01767 -0.00046 0.00295 0.00328 O13 4 0.193395 -0.103340 0.221089 11.00000 0.01566 0.02562 = 0.02770 0.00619 -0.00632 0.00510 O12 4 0.089313 -0.263763 0.277914 11.00000 0.02267 0.03518 = 0.01127 -0.00059 0.00609 0.01898 O11 4 0.290856 0.200266 0.312841 11.00000 0.02347 0.02041 = 0.00983 0.00775 0.00561 0.01189 O10 4 0.358301 -0.122034 0.270427 11.00000 0.01634 0.02231 = 0.03059 -0.00268 0.00268 0.01237 O9 4 0.140397 0.033279 0.189981 11.00000 0.02855 0.01195 = 0.02286 0.00002 -0.00256 0.01341 O8 4 0.280223 0.224459 0.224118 11.00000 0.02658 0.02206 = 0.01497 -0.00516 -0.00621 0.01168 O7 4 0.043958 0.276967 0.314850 11.00000 0.01384 0.02744 = 0.03349 0.01306 -0.00538 0.00948 O6 4 0.272814 0.089274 0.377655 11.00000 0.00997 0.03340 = 0.02545 0.00496 -0.00548 0.00866 O5 4 0.202428 0.264808 0.159283 11.00000 0.02240 0.01750 = 0.01868 0.00414 0.00337 -0.00341 O4 4 0.357627 0.107986 0.259481 11.00000 0.02286 0.02459 = 0.01801 0.00390 0.00289 0.01854 N2 3 0.197003 0.515728 0.148013 11.00000 0.04674 0.03760 = 0.02408 0.01693 0.00572 0.02180 AFIX 23 H2C 2 0.224872 0.465635 0.154233 11.00000 -1.20000 H2D 2 0.177387 0.543118 0.166241 11.00000 -1.20000 AFIX 0 O1W 4 0.000000 0.000000 0.268970 10.33333 0.08253 0.08253 = 0.04920 0.00000 0.00000 0.04126 O3 4 0.281181 0.403877 0.349856 11.00000 0.03097 0.03555 = 0.03090 -0.01696 -0.01311 0.01013 N4 3 -0.001087 -0.144413 0.050878 11.00000 0.04123 0.04120 = 0.04126 -0.00035 0.00046 0.02074 O2 4 0.494060 0.368232 0.267647 11.00000 0.02779 0.03460 = 0.02390 -0.00250 0.00435 0.00577 N3 3 -0.030887 0.124046 0.110378 11.00000 0.02456 0.02438 = 0.03466 -0.00427 0.00119 0.01108 AFIX 23 H3C 2 -0.057403 0.091911 0.130607 11.00000 -1.20000 H3D 2 0.039457 0.195417 0.112736 11.00000 -1.20000 AFIX 0 N1 3 0.175921 0.629809 0.090550 11.00000 0.02819 0.01750 = 0.03194 0.00662 0.00579 0.00850 AFIX 23 H1C 2 0.176222 0.700060 0.086545 11.00000 -1.20000 H1D 2 0.178202 0.596880 0.071010 11.00000 -1.20000 AFIX 0 O1 4 0.402890 0.107937 0.188575 11.00000 0.02588 0.05023 = 0.03436 0.00941 0.00731 0.02136 C1 1 0.063965 0.544809 0.108489 11.00000 0.03613 0.05056 = 0.02419 0.00236 0.00162 0.01913 AFIX 23 H1A 2 -0.005179 0.506228 0.093090 11.00000 -1.20000 H1B 2 0.045364 0.589215 0.125276 11.00000 -1.20000 AFIX 0 C2 1 0.084002 0.447506 0.124960 11.00000 0.03642 0.02946 = 0.04716 0.00801 0.01823 0.00928 AFIX 23 H2A 2 0.099059 0.400396 0.108207 11.00000 -1.20000 H2B 2 0.011682 0.391091 0.137837 11.00000 -1.20000 AFIX 0 C3 1 -0.121426 0.144772 0.094317 11.00000 0.05489 0.05502 = 0.05502 -0.00012 -0.00007 0.02769 AFIX 23 H3A 2 -0.167851 0.158763 0.111515 11.00000 -1.20000 H3B 2 -0.078364 0.220128 0.081271 11.00000 -1.20000 AFIX 0 C4 1 -0.051165 -0.256232 0.073437 11.00000 0.08632 0.08627 = 0.08634 -0.00011 0.00009 0.04313 AFIX 23 H4A 2 -0.082904 -0.330147 0.059795 11.00000 -1.20000 H4B 2 0.015683 -0.251039 0.086994 11.00000 -1.20000 AFIX 0 O4W 4 0.028233 0.552883 0.192660 11.00000 0.08464 0.16946 = 0.04595 0.00395 0.01813 0.06568 O3W 4 0.000000 0.000000 -0.016890 10.33333 0.08426 0.08426 = 0.04694 0.00000 0.00000 0.04213 O5W 4 0.666667 0.333333 0.209670 10.33333 0.18321 HKLF 4 REM k in R3 REM R1 = 0.0890 for 5296 Fo > 4sig(Fo) and 0.0995 for all 5859 data REM 286 parameters refined using 19 restraints END WGHT 0.1444 395.5990 REM Highest difference peak 3.827, deepest hole -1.652, 1-sigma level 0.369 Q1 1 0.4421 0.2193 0.2877 11.00000 0.05 3.83 Q2 1 0.0408 -0.3611 0.2363 11.00000 0.05 3.72 Q3 1 0.3333 0.6667 0.3326 10.33333 0.05 2.83 Q4 1 0.3333 0.6667 0.3901 10.33333 0.05 2.69 Q5 1 0.6667 0.3333 0.1545 10.33333 0.05 2.16 Q6 1 -0.1177 -0.2566 0.0581 11.00000 0.05 1.89 Q7 1 0.3661 0.6517 0.3567 11.00000 0.05 1.85 Q8 1 0.1375 -0.0419 0.1940 11.00000 0.05 1.75 Q9 1 0.1395 -0.3184 0.2385 11.00000 0.05 1.68 Q10 1 0.1607 -0.2659 0.2254 11.00000 0.05 1.65 ; _shelx_res_checksum 90743 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 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 Sb1 Sb 0.39770(13) 0.02701(14) 0.29546(3) 0.0207(3) Uani 1 1 d . . . Sb2 Sb 0.21285(14) -0.23267(14) 0.24407(3) 0.0212(3) Uani 1 1 d . . . V5 V 0.1442(3) 0.1897(3) 0.19346(8) 0.0159(7) Uani 1 1 d . . . V4 V 0.1940(3) 0.0630(3) 0.34354(8) 0.0139(6) Uani 1 1 d . . . V3 V 0.2058(3) 0.2915(3) 0.32404(9) 0.0170(7) Uani 1 1 d . . . V2 V 0.2900(3) 0.0767(4) 0.21377(9) 0.0178(7) Uani 1 1 d . . . V1 V 0.3517(3) 0.2613(3) 0.26860(8) 0.0169(7) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.08069(12) 0.0216(10) Uani 1 3 d S T P Ni1 Ni 0.3333 0.6667 0.11939(12) 0.0209(9) Uani 1 3 d S T P O14 O 0.0448(14) -0.0975(14) 0.3483(4) 0.017(3) Uani 1 1 d . . . O13 O 0.1934(15) -0.1033(16) 0.2211(4) 0.025(3) Uani 1 1 d . . . O12 O 0.0893(15) -0.2638(17) 0.2779(4) 0.021(3) Uani 1 1 d . . . O11 O 0.2909(15) 0.2003(15) 0.3128(3) 0.017(3) Uani 1 1 d . . . O10 O 0.3583(15) -0.1220(15) 0.2704(4) 0.022(3) Uani 1 1 d . . . O9 O 0.1404(16) 0.0333(13) 0.1900(4) 0.020(3) Uani 1 1 d . . . O8 O 0.2802(16) 0.2245(15) 0.2241(4) 0.021(3) Uani 1 1 d . . . O7 O 0.0440(15) 0.2770(16) 0.3149(4) 0.025(3) Uani 1 1 d . . . O6 O 0.2728(14) 0.0893(17) 0.3777(4) 0.024(3) Uani 1 1 d . . . O5 O 0.2024(16) 0.2648(15) 0.1593(4) 0.025(3) Uani 1 1 d . . . O4 O 0.3576(15) 0.1080(15) 0.2595(4) 0.019(3) Uani 1 1 d . . . N2 N 0.197(2) 0.516(2) 0.1480(5) 0.036(5) Uani 1 1 d . . . H2C H 0.2249 0.4656 0.1542 0.043 Uiso 1 1 calc R U . H2D H 0.1774 0.5431 0.1662 0.043 Uiso 1 1 calc R U . O1W O 0.0000 0.0000 0.2690(14) 0.071(14) Uani 1 3 d S T P O3 O 0.2812(18) 0.4039(19) 0.3499(5) 0.035(4) Uani 1 1 d . . . N4 N -0.001(3) -0.144(3) 0.0509(7) 0.041(6) Uani 1 1 d . U . O2 O 0.4941(17) 0.3682(19) 0.2676(5) 0.033(4) Uani 1 1 d . . . N3 N -0.031(2) 0.124(2) 0.1104(5) 0.028(4) Uani 1 1 d . . . H3C H -0.0574 0.0919 0.1306 0.034 Uiso 1 1 calc R U . H3D H 0.0395 0.1954 0.1127 0.034 Uiso 1 1 calc R U . N1 N 0.1759(19) 0.6298(18) 0.0906(5) 0.027(4) Uani 1 1 d . . . H1C H 0.1762 0.7001 0.0865 0.033 Uiso 1 1 calc R U . H1D H 0.1782 0.5969 0.0710 0.033 Uiso 1 1 calc R U . O1 O 0.4029(18) 0.108(2) 0.1886(5) 0.036(4) Uani 1 1 d . . . C1 C 0.064(3) 0.545(3) 0.1085(6) 0.038(6) Uani 1 1 d . . . H1A H -0.0052 0.5062 0.0931 0.046 Uiso 1 1 calc R U . H1B H 0.0454 0.5892 0.1253 0.046 Uiso 1 1 calc R U . C2 C 0.084(3) 0.448(3) 0.1250(8) 0.041(7) Uani 1 1 d . . . H2A H 0.0991 0.4004 0.1082 0.049 Uiso 1 1 calc R U . H2B H 0.0117 0.3911 0.1378 0.049 Uiso 1 1 calc R U . C3 C -0.121(4) 0.145(4) 0.0943(10) 0.055(8) Uani 1 1 d . U . H3A H -0.1679 0.1588 0.1115 0.066 Uiso 1 1 calc R U . H3B H -0.0784 0.2201 0.0813 0.066 Uiso 1 1 calc R U . C4 C -0.051(6) -0.256(6) 0.0734(15) 0.086(14) Uani 1 1 d . U . H4A H -0.0829 -0.3301 0.0598 0.104 Uiso 1 1 calc R U . H4B H 0.0157 -0.2510 0.0870 0.104 Uiso 1 1 calc R U . O4W O 0.028(4) 0.553(5) 0.1927(8) 0.099(14) Uani 1 1 d . . . O3W O 0.0000 0.0000 -0.0169(13) 0.072(15) Uani 1 3 d S T P O5W O 0.6667 0.3333 0.210(3) 0.18(5) Uiso 1 3 d S . 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 Sb1 0.0168(6) 0.0291(8) 0.0179(6) 0.0030(5) 0.0007(5) 0.0127(6) Sb2 0.0270(7) 0.0257(7) 0.0181(6) 0.0023(5) 0.0045(5) 0.0186(6) V5 0.0158(15) 0.0149(16) 0.0144(14) 0.0007(12) -0.0007(11) 0.0056(13) V4 0.0124(15) 0.0163(15) 0.0128(14) 0.0018(11) -0.0007(11) 0.0071(12) V3 0.0179(16) 0.0149(15) 0.0155(15) -0.0023(12) -0.0032(12) 0.0062(13) V2 0.0162(15) 0.0214(17) 0.0154(15) -0.0001(12) 0.0040(12) 0.0091(14) V1 0.0143(15) 0.0168(16) 0.0145(15) 0.0012(12) -0.0016(12) 0.0040(12) Ni2 0.0213(14) 0.0213(14) 0.022(2) 0.000 0.000 0.0107(7) Ni1 0.0237(14) 0.0237(14) 0.015(2) 0.000 0.000 0.0119(7) O14 0.015(7) 0.013(6) 0.018(6) 0.000(5) 0.003(5) 0.003(5) O13 0.016(7) 0.026(8) 0.028(8) 0.006(7) -0.006(6) 0.005(6) O12 0.023(7) 0.035(9) 0.011(6) -0.001(6) 0.006(5) 0.019(7) O11 0.023(7) 0.020(7) 0.010(6) 0.008(5) 0.006(5) 0.012(6) O10 0.016(7) 0.022(8) 0.031(8) -0.003(6) 0.003(6) 0.012(6) O9 0.029(8) 0.012(6) 0.023(7) 0.000(5) -0.003(6) 0.013(6) O8 0.027(8) 0.022(7) 0.015(6) -0.005(6) -0.006(6) 0.012(6) O7 0.014(7) 0.027(8) 0.033(9) 0.013(7) -0.005(6) 0.009(6) O6 0.010(6) 0.033(9) 0.025(8) 0.005(6) -0.005(6) 0.009(6) O5 0.022(8) 0.018(7) 0.019(7) 0.004(6) 0.003(6) -0.003(6) O4 0.023(7) 0.025(7) 0.018(7) 0.004(6) 0.003(5) 0.019(7) N2 0.047(14) 0.038(12) 0.024(10) 0.017(9) 0.006(9) 0.022(11) O1W 0.08(2) 0.08(2) 0.05(3) 0.000 0.000 0.041(11) O3 0.031(9) 0.036(10) 0.031(9) -0.017(8) -0.013(7) 0.010(8) N4 0.041(6) 0.041(6) 0.041(6) -0.0003(15) 0.0005(15) 0.021(3) O2 0.028(9) 0.035(10) 0.024(8) -0.002(7) 0.004(7) 0.006(8) N3 0.025(10) 0.024(10) 0.035(11) -0.004(8) 0.001(8) 0.011(8) N1 0.028(10) 0.017(9) 0.032(10) 0.007(8) 0.006(8) 0.009(8) O1 0.026(9) 0.050(12) 0.034(10) 0.009(9) 0.007(7) 0.021(9) C1 0.036(14) 0.051(17) 0.024(12) 0.002(11) 0.002(10) 0.019(13) C2 0.036(14) 0.029(13) 0.047(16) 0.008(12) 0.018(12) 0.009(12) C3 0.055(8) 0.055(8) 0.055(8) -0.0001(15) -0.0001(15) 0.028(4) C4 0.086(14) 0.086(14) 0.086(14) -0.0001(15) 0.0001(15) 0.043(7) O4W 0.08(3) 0.17(4) 0.046(16) 0.00(2) 0.018(16) 0.07(3) O3W 0.08(2) 0.08(2) 0.05(2) 0.000 0.000 0.042(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' Sb Sb -0.5866 1.5461 '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 O10 Sb1 O7 93.7(7) . 3 O10 Sb1 O4 96.2(7) . . O7 Sb1 O4 92.5(7) 3 . O12 Sb2 O10 97.5(7) . . O12 Sb2 O13 94.4(7) . . O10 Sb2 O13 97.1(7) . . O5 V5 O9 108.3(8) . 2 O5 V5 O9 107.6(8) . . O9 V5 O9 90.8(10) 2 . O5 V5 O8 108.2(8) . . O9 V5 O8 143.3(7) 2 . O9 V5 O8 81.3(7) . . O5 V5 O13 105.8(9) . 2 O9 V5 O13 77.7(7) 2 2 O9 V5 O13 146.5(8) . 2 O8 V5 O13 89.4(7) . 2 O5 V5 V2 107.9(7) . . O9 V5 V2 126.1(5) 2 . O9 V5 V2 40.4(5) . . O8 V5 V2 41.6(5) . . O13 V5 V2 127.0(5) 2 . O5 V5 V2 109.8(7) . 2 O9 V5 V2 37.9(5) 2 2 O9 V5 V2 123.6(5) . 2 O8 V5 V2 122.8(5) . 2 O13 V5 V2 39.9(5) 2 2 V2 V5 V2 142.26(17) . 2 O6 V4 O14 106.7(8) . 2 O6 V4 O14 107.4(8) . . O14 V4 O14 89.9(9) 2 . O6 V4 O11 107.7(8) . . O14 V4 O11 83.3(7) 2 . O14 V4 O11 144.8(7) . . O6 V4 O7 107.0(9) . 3 O14 V4 O7 146.2(8) 2 3 O14 V4 O7 78.2(6) . 3 O11 V4 O7 88.6(6) . 3 O6 V4 V3 107.6(7) . . O14 V4 V3 41.4(5) 2 . O14 V4 V3 126.4(5) . . O11 V4 V3 42.5(5) . . O7 V4 V3 126.6(5) 3 . O6 V4 V3 109.3(7) . 3 O14 V4 V3 123.5(5) 2 3 O14 V4 V3 38.4(5) . 3 O11 V4 V3 123.2(5) . 3 O7 V4 V3 40.0(4) 3 3 V3 V4 V3 143.08(17) . 3 O3 V3 O14 109.9(9) . 2 O3 V3 O11 113.7(9) . . O14 V3 O11 82.8(6) 2 . O3 V3 O7 109.0(10) . . O14 V3 O7 79.2(6) 2 . O11 V3 O7 137.1(8) . . O3 V3 O12 108.4(9) . 2 O14 V3 O12 141.5(7) 2 2 O11 V3 O12 79.3(6) . 2 O7 V3 O12 91.2(7) . 2 O3 V3 V4 113.9(8) . . O14 V3 V4 41.0(4) 2 . O11 V3 V4 42.4(4) . . O7 V3 V4 114.5(5) . . O12 V3 V4 117.4(5) 2 . O3 V3 V1 117.0(8) . . O14 V3 V1 115.1(5) 2 . O11 V3 V1 38.8(4) . . O7 V3 V1 120.5(6) . . O12 V3 V1 40.5(5) 2 . V4 V3 V1 79.05(13) . . O3 V3 V4 112.5(8) . 2 O14 V3 V4 38.9(4) 2 2 O11 V3 V4 114.7(5) . 2 O7 V3 V4 40.6(5) . 2 O12 V3 V4 124.3(5) 2 2 V4 V3 V4 77.53(15) . 2 V1 V3 V4 130.29(15) . 2 O1 V2 O9 111.6(9) . . O1 V2 O8 111.3(10) . . O9 V2 O8 81.9(7) . . O1 V2 O4 107.2(9) . . O9 V2 O4 141.0(7) . . O8 V2 O4 80.7(6) . . O1 V2 O13 109.3(10) . . O9 V2 O13 78.3(6) . . O8 V2 O13 139.0(8) . . O4 V2 O13 92.6(7) . . O1 V2 V5 113.0(7) . . O9 V2 V5 40.9(4) . . O8 V2 V5 41.8(5) . . O4 V2 V5 118.1(5) . . O13 V2 V5 114.7(5) . . O1 V2 V1 114.5(8) . . O9 V2 V1 114.9(5) . . O8 V2 V1 39.7(4) . . O4 V2 V1 41.1(4) . . O13 V2 V1 123.0(6) . . V5 V2 V1 79.28(13) . . O1 V2 V5 114.4(8) . 3 O9 V2 V5 38.1(4) . 3 O8 V2 V5 114.0(5) . 3 O4 V2 V5 124.5(5) . 3 O13 V2 V5 40.3(5) . 3 V5 V2 V5 77.13(16) . 3 V1 V2 V5 130.74(15) . 3 O2 V1 O11 113.9(8) . . O2 V1 O8 111.3(9) . . O11 V1 O8 134.8(7) . . O2 V1 O12 103.1(10) . 2 O11 V1 O12 80.4(6) . 2 O8 V1 O12 89.3(7) . 2 O2 V1 O4 103.8(9) . . O11 V1 O4 89.1(6) . . O8 V1 O4 80.7(7) . . O12 V1 O4 153.1(7) 2 . O2 V1 V2 112.1(7) . . O11 V1 V2 118.0(5) . . O8 V1 V2 40.0(5) . . O12 V1 V2 125.5(5) 2 . O4 V1 V2 40.7(4) . . O2 V1 V3 113.7(7) . . O11 V1 V3 39.6(5) . . O8 V1 V3 118.0(5) . . O12 V1 V3 40.8(4) 2 . O4 V1 V3 124.9(5) . . V2 V1 V3 134.27(15) . . N3 Ni2 N3 92.1(9) 3 2 N3 Ni2 N3 92.1(9) 3 . N3 Ni2 N3 92.1(9) 2 . N3 Ni2 N4 170.7(9) 3 3 N3 Ni2 N4 94.9(9) 2 3 N3 Ni2 N4 81.4(9) . 3 N3 Ni2 N4 81.4(9) 3 2 N3 Ni2 N4 170.7(9) 2 2 N3 Ni2 N4 94.9(9) . 2 N4 Ni2 N4 92.4(10) 3 2 N3 Ni2 N4 94.9(9) 3 . N3 Ni2 N4 81.4(9) 2 . N3 Ni2 N4 170.7(9) . . N4 Ni2 N4 92.4(10) 3 . N4 Ni2 N4 92.4(10) 2 . N1 Ni1 N1 93.3(8) . 3_565 N1 Ni1 N1 93.3(8) . 2_665 N1 Ni1 N1 93.3(8) 3_565 2_665 N1 Ni1 N2 91.4(9) . 3_565 N1 Ni1 N2 81.7(8) 3_565 3_565 N1 Ni1 N2 173.3(9) 2_665 3_565 N1 Ni1 N2 81.7(8) . . N1 Ni1 N2 173.3(9) 3_565 . N1 Ni1 N2 91.4(9) 2_665 . N2 Ni1 N2 93.9(9) 3_565 . N1 Ni1 N2 173.3(9) . 2_665 N1 Ni1 N2 91.4(9) 3_565 2_665 N1 Ni1 N2 81.7(8) 2_665 2_665 N2 Ni1 N2 93.9(9) 3_565 2_665 N2 Ni1 N2 93.9(9) . 2_665 V4 O14 V3 97.6(7) 3 3 V4 O14 V4 147.6(9) 3 . V3 O14 V4 102.7(7) 3 . V2 O13 Sb2 138.3(9) . . V2 O13 V5 99.8(8) . 3 Sb2 O13 V5 121.8(8) . 3 Sb2 O12 V1 123.2(8) . 3 Sb2 O12 V3 137.2(9) . 3 V1 O12 V3 98.7(6) 3 3 V1 O11 V3 101.6(7) . . V1 O11 V4 150.6(9) . . V3 O11 V4 95.1(6) . . Sb1 O10 Sb2 130.9(8) . . V2 O9 V5 104.0(7) . 3 V2 O9 V5 98.7(7) . . V5 O9 V5 147.9(10) 3 . V1 O8 V2 100.3(7) . . V1 O8 V5 150.6(10) . . V2 O8 V5 96.6(7) . . Sb1 O7 V3 140.6(9) 2 . Sb1 O7 V4 118.7(8) 2 2 V3 O7 V4 99.4(7) . 2 Sb1 O4 V2 140.6(9) . . Sb1 O4 V1 120.3(8) . . V2 O4 V1 98.2(6) . . C2 N2 Ni1 105.9(15) . . C4 N4 Ni2 106(3) . . C3 N3 Ni2 109(2) . . C1 N1 Ni1 109.8(16) . . N1 C1 C2 108(2) . . C1 C2 N2 107(2) . . C4 C3 N3 117(4) 3 . C3 C4 N4 112(4) 2 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb1 O10 1.948(16) . Sb1 O7 1.948(15) 3 Sb1 O4 1.962(14) . Sb2 O12 1.940(14) . Sb2 O10 1.952(17) . Sb2 O13 1.976(17) . V5 O5 1.611(16) . V5 O9 1.926(15) 2 V5 O9 1.935(15) . V5 O8 1.960(16) . V5 O13 1.987(16) 2 V5 V2 2.922(5) . V5 V2 3.028(5) 2 V4 O6 1.617(15) . V4 O14 1.914(15) 2 V4 O14 1.947(15) . V4 O11 1.959(15) . V4 O7 1.997(17) 3 V4 V3 2.891(5) . V4 V3 3.027(5) 3 V3 O3 1.612(18) . V3 O14 1.930(16) 2 V3 O11 1.959(16) . V3 O7 1.971(16) . V3 O12 1.990(15) 2 V3 V1 3.011(5) . V3 V4 3.027(5) 2 V2 O1 1.614(19) . V2 O9 1.918(17) . V2 O8 1.954(17) . V2 O4 1.969(15) . V2 O13 1.971(17) . V2 V1 2.990(5) . V2 V5 3.028(5) 3 V1 O2 1.604(19) . V1 O11 1.926(14) . V1 O8 1.940(15) . V1 O12 1.979(17) 2 V1 O4 1.986(16) . Ni2 N3 2.13(2) 3 Ni2 N3 2.13(2) 2 Ni2 N3 2.13(2) . Ni2 N4 2.16(3) 3 Ni2 N4 2.16(3) 2 Ni2 N4 2.16(3) . Ni1 N1 2.12(2) . Ni1 N1 2.12(2) 3_565 Ni1 N1 2.12(2) 2_665 Ni1 N2 2.13(2) 3_565 Ni1 N2 2.13(2) . Ni1 N2 2.13(2) 2_665 O14 V4 1.914(15) 3 O14 V3 1.930(16) 3 O13 V5 1.987(16) 3 O12 V1 1.979(17) 3 O12 V3 1.990(15) 3 O9 V5 1.926(15) 3 O7 Sb1 1.948(15) 2 O7 V4 1.997(17) 2 N2 C2 1.54(4) . N4 C4 1.51(7) . N3 C3 1.43(4) . N1 C1 1.45(3) . C1 C2 1.51(4) . C3 C4 1.39(7) 3 C4 C3 1.39(7) 2