#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:22:58 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185228 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/52/7225237.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_7225237 loop_ _publ_author_name 'Guo, Hai-Yang' 'Zhang, Xiao' 'Cui, Xiao-Bing' 'Huo, Qi-Sheng' 'Xu, Ji-Qing' _publ_section_title ; Vanadoantimonates: from discrete clusters to high dimensional aggregates ; _journal_issue 27 _journal_name_full CrystEngComm _journal_page_first 5130 _journal_paper_doi 10.1039/C6CE00616G _journal_volume 18 _journal_year 2016 _chemical_formula_sum 'C12 H62 Co2 N12 O48 Sb6 V15' _chemical_formula_weight 2755.19 _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 ; 2016-05-11 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 12.4543(18) _cell_length_b 12.4543(18) _cell_length_c 39.916(8) _cell_measurement_reflns_used 15141 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 3.06 _cell_volume 5361.9(15) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'SHELXL-2014/7 (Sheldrick, 2014)' _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 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker P4' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_Laue_measured_fraction_full 0.998 _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 -13 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_number 17328 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.477 _diffrn_reflns_theta_min 3.062 _exptl_absorpt_coefficient_mu 4.628 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5005 _exptl_absorpt_correction_type empirical _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.560 _exptl_crystal_description polyhedron _exptl_crystal_F_000 3921 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.120 _refine_diff_density_max 1.780 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.194 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.44(7) _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 287 _refine_ls_number_reflns 5447 _refine_ls_number_restraints 26 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0501 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1324 _refine_ls_wR_factor_ref 0.1415 _reflns_Friedel_coverage 1.000 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 4591 _reflns_number_total 5447 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00616g2.cif _cod_data_source_block shelx_3 _cod_depositor_comments 'Adding full bibliography for 7225235--7225239.cif.' _cod_original_cell_volume 5361.9(19) _cod_database_code 7225237 _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 0.416 _shelx_estimated_absorpt_t_max 0.607 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL K in R3 CELL 0.71073 12.4543 12.4543 39.9164 90.000 90.000 120.000 ZERR 3.00 0.0018 0.0018 0.0080 0.000 0.000 0.000 LATT -3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O V CO SB UNIT 36 186 36 144 45 6 18 L.S. 14 BOND FMAP 2 PLAN 20 ACTA TWIN SIZE 0.23*0.13*0.12 ISOR 0.001 o2w o4w simu 0.01 0.02 2.3 c1 n1 c2 dfix 1.42 c1 c2 WGHT 0.087000 BASF 0.44437 FVAR 0.03296 SB1 7 0.601206 0.626104 0.250829 11.00000 0.03084 0.03525 = 0.02646 -0.00127 0.00290 0.01113 SB2 7 0.788519 0.553542 0.302533 11.00000 0.04571 0.02989 = 0.02681 0.00488 0.00729 0.01721 V5 5 0.804835 0.867597 0.202496 11.00000 0.02624 0.02793 = 0.02057 -0.00175 0.00006 0.01155 V4 5 0.855272 1.045541 0.353302 11.00000 0.03236 0.03627 = 0.02190 -0.00108 0.00082 0.02022 V3 5 0.792779 1.085608 0.222119 11.00000 0.03158 0.03495 = 0.02466 -0.00246 -0.00401 0.01817 V2 5 0.646816 0.907723 0.277881 11.00000 0.02600 0.04004 = 0.02394 -0.00218 -0.00058 0.01739 V1 5 0.708636 0.785365 0.332734 11.00000 0.03501 0.03726 = 0.02255 0.00346 0.00505 0.01679 CO2 6 1.000000 1.000000 0.093153 10.33333 0.03645 0.03645 = 0.02565 0.00000 0.00000 0.01823 CO1 6 0.333333 0.666667 0.133076 10.33333 0.03125 0.03125 = 0.03243 0.00000 0.00000 0.01562 O14 4 0.953623 0.854991 0.197919 11.00000 0.02679 0.03284 = 0.03095 0.00801 0.00862 0.01593 O13 4 0.805305 0.700769 0.325684 11.00000 0.03769 0.03826 = 0.03350 -0.00480 -0.00473 0.01812 O12 4 0.706812 0.909459 0.233486 11.00000 0.03437 0.04241 = 0.02239 0.00066 0.00444 0.02638 O11 4 0.910882 0.647727 0.268709 11.00000 0.03431 0.02627 = 0.02328 0.00635 -0.00244 0.00793 O10 4 0.720401 0.945233 0.322246 11.00000 0.03753 0.03452 = 0.02120 0.00540 0.00306 0.01776 O9 4 0.955715 1.231568 0.230560 11.00000 0.04167 0.04012 = 0.03805 -0.01448 -0.00561 0.02077 O8 4 0.796635 1.063148 0.387372 11.00000 0.04132 0.04667 = 0.02788 -0.00231 0.00768 0.02355 O7 4 0.858288 0.891927 0.357565 11.00000 0.04149 0.03743 = 0.03096 -0.00814 -0.00442 0.02062 O6 4 0.645030 0.516911 0.275718 11.00000 0.04172 0.02748 = 0.03907 -0.00209 0.00902 0.00701 O5 4 0.724749 0.815361 0.168540 11.00000 0.03530 0.03906 = 0.02652 -0.00370 -0.00391 0.01576 O4 4 0.640459 0.748479 0.286912 11.00000 0.04313 0.03551 = 0.02709 -0.00084 -0.00585 0.01736 O1W 4 0.333333 0.666667 0.326939 10.33333 0.02885 0.02885 = 0.04919 0.00000 0.00000 0.01442 O3 4 0.502524 0.869875 0.279300 11.00000 0.03829 0.06794 = 0.03920 0.00086 0.01045 0.03044 O2 4 0.715501 1.123696 0.196471 11.00000 0.05031 0.06810 = 0.03930 -0.00227 -0.01686 0.03125 N3 3 0.876167 1.034199 0.121897 11.00000 0.04397 0.03216 = 0.02789 0.00610 -0.00061 0.01513 AFIX 23 H3C 2 0.805978 0.963123 0.125275 11.00000 -1.20000 H3D 2 0.909907 1.064776 0.141790 11.00000 -1.20000 AFIX 0 N1 3 0.476130 0.812595 0.163561 11.00000 0.05602 0.04852 = 0.06577 -0.00968 -0.03364 0.02037 AFIX 23 H1C 2 0.457778 0.797489 0.185220 11.00000 -1.20000 H1D 2 0.549249 0.818187 0.159895 11.00000 -1.20000 AFIX 0 O1 4 0.593335 0.709721 0.357957 11.00000 0.05572 0.05050 = 0.04570 0.01098 0.02440 0.01873 C3 1 0.848699 1.121694 0.104868 11.00000 0.04553 0.05162 = 0.04964 0.00325 0.00476 0.02300 AFIX 23 H3A 2 0.822333 1.162231 0.120956 11.00000 -1.20000 H3B 2 0.782825 1.078579 0.088632 11.00000 -1.20000 AFIX 0 C1 1 0.479213 0.925615 0.153644 11.00000 0.09309 0.05895 = 0.08842 -0.00507 -0.04435 0.00871 AFIX 23 H1A 2 0.418700 0.934518 0.166831 11.00000 -1.20000 H1B 2 0.560357 0.995188 0.158928 11.00000 -1.20000 AFIX 0 N2 3 0.364048 0.824875 0.103446 11.00000 0.03666 0.03399 = 0.03657 0.00245 -0.00836 0.01310 AFIX 23 H2C 2 0.388951 0.819410 0.082937 11.00000 -1.20000 H2D 2 0.294026 0.827261 0.101712 11.00000 -1.20000 AFIX 0 C2 1 0.454706 0.931685 0.119278 11.00000 0.10066 0.04243 = 0.07793 0.00357 -0.03274 0.01753 AFIX 23 H2A 2 0.431770 0.995097 0.116772 11.00000 -1.20000 H2B 2 0.531738 0.959979 0.107150 11.00000 -1.20000 AFIX 0 N4 3 1.012017 1.153881 0.064422 11.00000 0.05341 0.06162 = 0.02910 0.00207 -0.00181 0.02922 C4 1 0.969191 1.218598 0.087061 11.00000 0.07710 0.04597 = 0.03864 0.01854 0.00283 0.02865 AFIX 23 H4A 2 0.953477 1.275659 0.074324 11.00000 -1.20000 H4B 2 1.032715 1.265867 0.103568 11.00000 -1.20000 AFIX 0 O3W 4 1.000000 1.000000 0.276161 10.33333 0.03017 0.03017 = 0.01716 0.00000 0.00000 0.01509 O2W 4 0.333333 0.666667 0.231691 10.33333 0.09456 0.09456 = 0.09378 0.00000 0.00000 0.04728 O4W 4 0.471700 0.442447 0.354199 11.00000 0.13253 0.13163 = 0.13232 0.00079 -0.00148 0.06607 HKLF 4 REM K in R3 REM R1 = 0.0501 for 4591 Fo > 4sig(Fo) and 0.0608 for all 5447 data REM 287 parameters refined using 26 restraints END WGHT 0.0836 0.0000 REM Highest difference peak 1.780, deepest hole -1.278, 1-sigma level 0.194 Q1 1 0.6667 1.3333 0.1535 10.33333 0.05 1.78 Q2 1 0.6667 1.3333 0.1885 10.33333 0.05 1.75 Q3 1 0.5445 0.9264 0.1370 11.00000 0.05 1.67 Q4 1 0.6667 1.3333 0.2143 10.33333 0.05 1.51 Q5 1 0.5614 0.7750 0.2616 11.00000 0.05 1.44 Q6 1 0.4056 0.3720 0.3109 11.00000 0.05 1.15 Q7 1 0.8561 0.5760 0.3139 11.00000 0.05 1.05 Q8 1 0.9505 1.2761 0.2416 11.00000 0.05 0.88 Q9 1 0.4097 0.7691 0.3919 11.00000 0.05 0.80 Q10 1 0.3333 0.6667 0.3887 10.33333 0.05 0.78 Q11 1 0.2869 0.6753 0.3859 11.00000 0.05 0.75 Q12 1 0.7605 0.6436 0.2977 11.00000 0.05 0.74 Q13 1 0.8687 0.6730 0.3104 11.00000 0.05 0.72 Q14 1 0.4809 0.5813 0.2589 11.00000 0.05 0.69 Q15 1 0.8054 0.4638 0.3090 11.00000 0.05 0.69 Q16 1 0.6712 0.5155 0.3098 11.00000 0.05 0.69 Q17 1 0.5009 0.6602 0.2735 11.00000 0.05 0.68 Q18 1 0.5655 0.7063 0.2447 11.00000 0.05 0.67 Q19 1 0.7067 0.4332 0.2974 11.00000 0.05 0.66 Q20 1 0.5090 0.5138 0.2415 11.00000 0.05 0.64 ; _shelx_res_checksum 59610 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 0.60121(9) 0.62610(9) 0.25083(2) 0.0332(3) Uani 1 1 d . . . Sb2 Sb 0.78852(10) 0.55354(9) 0.30253(2) 0.0349(3) Uani 1 1 d . . . V5 V 0.8048(2) 0.8676(2) 0.20250(6) 0.0258(5) Uani 1 1 d . . . V4 V 0.8553(2) 1.0455(2) 0.35330(6) 0.0288(5) Uani 1 1 d . . . V3 V 0.7928(2) 1.0856(2) 0.22212(6) 0.0297(5) Uani 1 1 d . . . V2 V 0.6468(2) 0.9077(2) 0.27788(6) 0.0296(5) Uani 1 1 d . . . V1 V 0.7086(2) 0.7854(3) 0.33273(6) 0.0322(6) Uani 1 1 d . . . Co2 Co 1.0000 1.0000 0.09315(9) 0.0328(7) Uani 1 3 d S T P Co1 Co 0.3333 0.6667 0.13308(9) 0.0316(7) Uani 1 3 d S T P O14 O 0.9536(9) 0.8550(10) 0.1979(2) 0.030(2) Uani 1 1 d . . . O13 O 0.8053(11) 0.7008(11) 0.3257(3) 0.037(2) Uani 1 1 d . . . O12 O 0.7068(10) 0.9095(10) 0.2335(2) 0.030(2) Uani 1 1 d . . . O11 O 0.9109(9) 0.6477(9) 0.2687(2) 0.031(2) Uani 1 1 d . . . O10 O 0.7204(10) 0.9452(10) 0.3222(2) 0.031(2) Uani 1 1 d . . . O9 O 0.9557(11) 1.2316(11) 0.2306(3) 0.040(3) Uani 1 1 d . . . O8 O 0.7966(11) 1.0631(11) 0.3874(3) 0.038(2) Uani 1 1 d . . . O7 O 0.8583(11) 0.8919(10) 0.3576(3) 0.036(2) Uani 1 1 d . . . O6 O 0.6450(11) 0.5169(10) 0.2757(3) 0.041(3) Uani 1 1 d . . . O5 O 0.7247(10) 0.8154(10) 0.1685(3) 0.035(2) Uani 1 1 d . . . O4 O 0.6405(11) 0.7485(10) 0.2869(3) 0.036(2) Uani 1 1 d . . . O1W O 0.3333 0.6667 0.3269(5) 0.036(4) Uani 1 3 d S T P O3 O 0.5025(11) 0.8699(13) 0.2793(3) 0.047(3) Uani 1 1 d . . . O2 O 0.7155(12) 1.1237(14) 0.1965(3) 0.052(3) Uani 1 1 d . . . N3 N 0.8762(13) 1.0342(12) 0.1219(3) 0.036(3) Uani 1 1 d . . . H3C H 0.8060 0.9631 0.1253 0.044 Uiso 1 1 calc R U . H3D H 0.9099 1.0648 0.1418 0.044 Uiso 1 1 calc R U . N1 N 0.4761(16) 0.8126(16) 0.1636(5) 0.059(4) Uani 1 1 d . U . H1C H 0.4578 0.7975 0.1852 0.071 Uiso 1 1 calc R U . H1D H 0.5492 0.8182 0.1599 0.071 Uiso 1 1 calc R U . O1 O 0.5933(13) 0.7097(12) 0.3580(3) 0.054(3) Uani 1 1 d . . . C3 C 0.8487(18) 1.1217(18) 0.1049(5) 0.049(4) Uani 1 1 d . . . H3A H 0.8223 1.1622 0.1210 0.059 Uiso 1 1 calc R U . H3B H 0.7828 1.0786 0.0886 0.059 Uiso 1 1 calc R U . C1 C 0.479(3) 0.926(3) 0.1536(7) 0.093(7) Uani 1 1 d D U . H1A H 0.4187 0.9345 0.1668 0.112 Uiso 1 1 calc R U . H1B H 0.5604 0.9952 0.1589 0.112 Uiso 1 1 calc R U . N2 N 0.3640(12) 0.8249(12) 0.1034(3) 0.038(3) Uani 1 1 d . . . H2C H 0.3890 0.8194 0.0829 0.045 Uiso 1 1 calc R U . H2D H 0.2940 0.8273 0.1017 0.045 Uiso 1 1 calc R U . C2 C 0.455(3) 0.932(2) 0.1193(6) 0.082(7) Uani 1 1 d D U . H2A H 0.4318 0.9951 0.1168 0.098 Uiso 1 1 calc R U . H2B H 0.5317 0.9600 0.1071 0.098 Uiso 1 1 calc R U . N4 N 1.0120(15) 1.1539(16) 0.0644(4) 0.048(3) Uani 1 1 d . . . C4 C 0.969(2) 1.2186(18) 0.0871(5) 0.055(5) Uani 1 1 d . . . H4A H 0.9535 1.2757 0.0743 0.066 Uiso 1 1 calc R U . H4B H 1.0327 1.2659 0.1036 0.066 Uiso 1 1 calc R U . O3W O 1.0000 1.0000 0.2762(4) 0.026(3) Uani 1 3 d S T P O2W O 0.3333 0.6667 0.2317(10) 0.094(4) Uani 1 3 d S TU P O4W O 0.472(3) 0.442(3) 0.3542(8) 0.132(9) Uani 1 1 d . U . 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 0.0308(5) 0.0353(5) 0.0265(5) -0.0013(4) 0.0029(4) 0.0111(4) Sb2 0.0457(6) 0.0299(5) 0.0268(4) 0.0049(4) 0.0073(4) 0.0172(4) V5 0.0262(11) 0.0279(11) 0.0206(11) -0.0017(9) 0.0001(8) 0.0116(9) V4 0.0324(12) 0.0363(13) 0.0219(11) -0.0011(10) 0.0008(9) 0.0202(11) V3 0.0316(12) 0.0349(13) 0.0247(11) -0.0025(10) -0.0040(10) 0.0182(11) V2 0.0260(12) 0.0400(13) 0.0239(11) -0.0022(10) -0.0006(9) 0.0174(11) V1 0.0350(13) 0.0373(14) 0.0225(12) 0.0035(10) 0.0050(10) 0.0168(11) Co2 0.0365(11) 0.0365(11) 0.0256(16) 0.000 0.000 0.0182(5) Co1 0.0312(10) 0.0312(10) 0.0324(18) 0.000 0.000 0.0156(5) O14 0.027(5) 0.033(5) 0.031(5) 0.008(4) 0.009(4) 0.016(4) O13 0.038(6) 0.038(6) 0.033(6) -0.005(5) -0.005(5) 0.018(5) O12 0.034(5) 0.042(6) 0.022(5) 0.001(4) 0.004(4) 0.026(5) O11 0.034(5) 0.026(5) 0.023(5) 0.006(4) -0.002(4) 0.008(4) O10 0.038(5) 0.035(5) 0.021(5) 0.005(4) 0.003(4) 0.018(4) O9 0.042(6) 0.040(6) 0.038(6) -0.014(5) -0.006(5) 0.021(5) O8 0.041(6) 0.047(6) 0.028(5) -0.002(5) 0.008(5) 0.024(5) O7 0.041(6) 0.037(6) 0.031(5) -0.008(5) -0.004(5) 0.021(5) O6 0.042(6) 0.027(5) 0.039(6) -0.002(5) 0.009(5) 0.007(5) O5 0.035(6) 0.039(6) 0.027(5) -0.004(4) -0.004(4) 0.016(5) O4 0.043(6) 0.036(6) 0.027(6) -0.001(4) -0.006(5) 0.017(5) O1W 0.029(5) 0.029(5) 0.049(11) 0.000 0.000 0.014(3) O3 0.038(6) 0.068(8) 0.039(6) 0.001(6) 0.010(5) 0.030(6) O2 0.050(7) 0.068(9) 0.039(7) -0.002(6) -0.017(6) 0.031(7) N3 0.044(7) 0.032(7) 0.028(6) 0.006(5) -0.001(5) 0.015(6) N1 0.056(9) 0.049(8) 0.066(10) -0.010(7) -0.034(8) 0.020(7) O1 0.056(8) 0.051(7) 0.046(7) 0.011(6) 0.024(6) 0.019(6) C3 0.046(10) 0.052(10) 0.050(11) 0.003(8) 0.005(8) 0.023(9) C1 0.093(11) 0.059(9) 0.088(11) -0.005(9) -0.044(10) 0.009(9) N2 0.037(7) 0.034(7) 0.037(7) 0.002(6) -0.008(6) 0.013(6) C2 0.101(14) 0.042(9) 0.078(13) 0.004(10) -0.033(11) 0.018(10) N4 0.053(9) 0.062(10) 0.029(7) 0.002(7) -0.002(6) 0.029(8) C4 0.077(14) 0.046(10) 0.039(10) 0.019(8) 0.003(9) 0.029(10) O3W 0.030(5) 0.030(5) 0.017(7) 0.000 0.000 0.015(2) O2W 0.095(3) 0.095(3) 0.094(5) 0.000 0.000 0.0473(17) O4W 0.133(10) 0.132(10) 0.132(10) 0.001(3) -0.001(3) 0.066(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' 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' 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 O6 Sb1 O4 96.8(5) . . O6 Sb1 O9 93.6(5) . 2_765 O4 Sb1 O9 92.5(5) . 2_765 O11 Sb2 O6 96.4(4) . . O11 Sb2 O13 94.5(5) . . O6 Sb2 O13 97.8(5) . . O5 V5 O14 106.7(5) . 3_675 O5 V5 O14 108.1(5) . . O14 V5 O14 90.9(6) 3_675 . O5 V5 O9 107.3(6) . 2_765 O14 V5 O9 146.0(5) 3_675 2_765 O14 V5 O9 77.0(4) . 2_765 O5 V5 O12 107.0(5) . . O14 V5 O12 82.3(4) 3_675 . O14 V5 O12 144.8(4) . . O9 V5 O12 89.5(5) 2_765 . O5 V5 V3 107.0(4) . . O14 V5 V3 40.8(3) 3_675 . O14 V5 V3 126.7(3) . . O9 V5 V3 127.0(4) 2_765 . O12 V5 V3 42.1(3) . . O5 V5 V3 110.0(4) . 2_765 O14 V5 V3 123.8(3) 3_675 2_765 O14 V5 V3 37.8(3) . 2_765 O9 V5 V3 39.4(3) 2_765 2_765 O12 V5 V3 123.5(3) . 2_765 V3 V5 V3 142.93(12) . 2_765 O8 V4 O7 107.5(6) . 3_675 O8 V4 O7 107.1(5) . . O7 V4 O7 91.2(7) 3_675 . O8 V4 O10 108.6(5) . . O7 V4 O10 143.7(5) 3_675 . O7 V4 O10 81.9(5) . . O8 V4 O13 105.0(6) . 3_675 O7 V4 O13 78.2(5) 3_675 3_675 O7 V4 O13 147.8(5) . 3_675 O10 V4 O13 88.9(4) . 3_675 O8 V4 V1 108.2(4) . . O7 V4 V1 126.7(4) 3_675 . O7 V4 V1 40.8(3) . . O10 V4 V1 41.8(3) . . O13 V4 V1 127.0(4) 3_675 . O8 V4 V1 109.7(4) . 3_675 O7 V4 V1 38.3(3) 3_675 3_675 O7 V4 V1 124.2(4) . 3_675 O10 V4 V1 122.0(3) . 3_675 O13 V4 V1 40.0(3) 3_675 3_675 V1 V4 V1 142.10(12) . 3_675 O2 V3 O14 110.7(6) . 3_675 O2 V3 O12 113.6(6) . . O14 V3 O12 83.7(4) 3_675 . O2 V3 O9 109.0(7) . . O14 V3 O9 77.7(4) 3_675 . O12 V3 O9 137.1(5) . . O2 V3 O11 108.4(6) . 3_675 O14 V3 O11 140.9(5) 3_675 3_675 O12 V3 O11 78.9(4) . 3_675 O9 V3 O11 91.7(5) . 3_675 O2 V3 V5 114.7(5) . . O14 V3 V5 41.5(3) 3_675 . O12 V3 V5 42.9(3) . . O9 V3 V5 113.6(4) . . O11 V3 V5 117.0(3) 3_675 . O2 V3 V2 116.7(5) . . O14 V3 V2 115.3(3) 3_675 . O12 V3 V2 38.3(3) . . O9 V3 V2 121.1(4) . . O11 V3 V2 40.6(3) 3_675 . V5 V3 V2 78.84(9) . . O2 V3 V5 113.0(5) . 3_675 O14 V3 V5 38.6(3) 3_675 3_675 O12 V3 V5 115.3(3) . 3_675 O9 V3 V5 39.3(3) . 3_675 O11 V3 V5 123.5(3) 3_675 3_675 V5 V3 V5 77.69(11) . 3_675 V2 V3 V5 130.18(10) . 3_675 O3 V2 O12 113.9(6) . . O3 V2 O10 111.2(6) . . O12 V2 O10 134.9(4) . . O3 V2 O4 102.7(6) . . O12 V2 O4 90.0(5) . . O10 V2 O4 81.5(4) . . O3 V2 O11 104.5(6) . 3_675 O12 V2 O11 79.8(4) . 3_675 O10 V2 O11 88.0(4) . 3_675 O4 V2 O11 152.7(5) . 3_675 O3 V2 V1 111.1(5) . . O12 V2 V1 119.0(3) . . O10 V2 V1 40.6(3) . . O4 V2 V1 40.9(3) . . O11 V2 V1 124.9(3) 3_675 . O3 V2 V3 114.4(5) . . O12 V2 V3 39.1(3) . . O10 V2 V3 117.2(3) . . O4 V2 V3 125.2(4) . . O11 V2 V3 40.7(3) 3_675 . V1 V2 V3 134.52(10) . . O1 V1 O7 110.6(6) . . O1 V1 O10 108.5(6) . . O7 V1 O10 81.7(5) . . O1 V1 O4 106.8(7) . . O7 V1 O4 142.2(5) . . O10 V1 O4 81.0(5) . . O1 V1 O13 112.2(7) . . O7 V1 O13 78.7(5) . . O10 V1 O13 138.8(5) . . O4 V1 O13 92.9(5) . . O1 V1 V4 110.5(5) . . O7 V1 V4 40.9(3) . . O10 V1 V4 41.5(3) . . O4 V1 V4 118.4(3) . . O13 V1 V4 114.9(4) . . O1 V1 V2 112.0(6) . . O7 V1 V2 115.6(4) . . O10 V1 V2 40.0(3) . . O4 V1 V2 41.1(3) . . O13 V1 V2 123.4(4) . . V4 V1 V2 79.51(9) . . O1 V1 V4 116.6(6) . 2_765 O7 V1 V4 38.3(3) . 2_765 O10 V1 V4 113.3(3) . 2_765 O4 V1 V4 124.7(4) . 2_765 O13 V1 V4 40.4(3) . 2_765 V4 V1 V4 76.93(11) . 2_765 V2 V1 V4 130.79(11) . 2_765 N3 Co2 N3 93.7(5) 3_675 2_765 N3 Co2 N3 93.7(5) 3_675 . N3 Co2 N3 93.7(5) 2_765 . N3 Co2 N4 90.8(6) 3_675 . N3 Co2 N4 173.3(6) 2_765 . N3 Co2 N4 81.1(5) . . N3 Co2 N4 173.3(6) 3_675 2_765 N3 Co2 N4 81.1(5) 2_765 2_765 N3 Co2 N4 90.8(6) . 2_765 N4 Co2 N4 94.7(5) . 2_765 N3 Co2 N4 81.1(5) 3_675 3_675 N3 Co2 N4 90.8(6) 2_765 3_675 N3 Co2 N4 173.3(6) . 3_675 N4 Co2 N4 94.7(5) . 3_675 N4 Co2 N4 94.7(5) 2_765 3_675 N2 Co1 N2 92.9(5) 2_665 . N2 Co1 N2 92.9(5) 2_665 3_565 N2 Co1 N2 92.9(5) . 3_565 N2 Co1 N1 81.1(6) 2_665 2_665 N2 Co1 N1 95.1(7) . 2_665 N2 Co1 N1 170.3(6) 3_565 2_665 N2 Co1 N1 170.3(6) 2_665 . N2 Co1 N1 81.1(6) . . N2 Co1 N1 95.0(7) 3_565 . N1 Co1 N1 91.7(7) 2_665 . N2 Co1 N1 95.0(7) 2_665 3_565 N2 Co1 N1 170.3(6) . 3_565 N2 Co1 N1 81.1(6) 3_565 3_565 N1 Co1 N1 91.7(7) 2_665 3_565 N1 Co1 N1 91.7(7) . 3_565 V3 O14 V5 97.7(5) 2_765 2_765 V3 O14 V5 103.6(4) 2_765 . V5 O14 V5 146.9(6) 2_765 . Sb2 O13 V1 138.9(6) . . Sb2 O13 V4 121.4(6) . 2_765 V1 O13 V4 99.6(5) . 2_765 V2 O12 V3 102.6(5) . . V2 O12 V5 149.4(6) . . V3 O12 V5 95.0(4) . . Sb2 O11 V2 122.9(5) . 2_765 Sb2 O11 V3 137.8(6) . 2_765 V2 O11 V3 98.7(4) 2_765 2_765 V2 O10 V4 152.1(6) . . V2 O10 V1 99.4(5) . . V4 O10 V1 96.7(5) . . V5 O9 V3 101.3(5) 3_675 . V5 O9 Sb1 119.1(6) 3_675 3_675 V3 O9 Sb1 138.4(6) . 3_675 V4 O7 V1 103.4(5) 2_765 . V4 O7 V4 146.8(7) 2_765 . V1 O7 V4 98.3(5) . . Sb2 O6 Sb1 131.3(6) . . V1 O4 Sb1 140.3(6) . . V1 O4 V2 98.0(5) . . Sb1 O4 V2 120.8(5) . . C3 N3 Co2 111.2(10) . . C1 N1 Co1 105.9(13) . . N3 C3 C4 107.3(15) . . C2 C1 N1 115(2) . . C2 N2 Co1 108.2(12) . . N2 C2 C1 119(2) . . C4 N4 Co2 105.9(10) . . N4 C4 C3 109.2(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb1 O6 1.969(13) . Sb1 O4 1.973(11) . Sb1 O9 1.985(11) 2_765 Sb2 O11 1.932(10) . Sb2 O6 1.932(13) . Sb2 O13 1.969(11) . V5 O5 1.614(10) . V5 O14 1.939(10) 3_675 V5 O14 1.945(10) . V5 O9 1.960(12) 2_765 V5 O12 1.982(10) . V5 V3 2.901(3) . V5 V3 3.032(4) 2_765 V4 O8 1.610(10) . V4 O7 1.933(11) 3_675 V4 O7 1.940(11) . V4 O10 1.955(11) . V4 O13 1.997(12) 3_675 V4 V1 2.931(4) . V4 V1 3.035(4) 3_675 V3 O2 1.630(12) . V3 O14 1.914(10) 3_675 V3 O12 1.953(11) . V3 O9 1.961(12) . V3 O11 1.994(10) 3_675 V3 V2 3.023(4) . V3 V5 3.032(4) 3_675 V2 O3 1.615(11) . V2 O12 1.919(10) . V2 O10 1.941(11) . V2 O4 1.978(11) . V2 O11 1.990(11) 3_675 V2 V1 2.980(4) . V1 O1 1.616(12) . V1 O7 1.935(12) . V1 O10 1.967(11) . V1 O4 1.972(11) . V1 O13 1.977(11) . V1 V4 3.035(4) 2_765 Co2 N3 2.129(14) 3_675 Co2 N3 2.129(14) 2_765 Co2 N3 2.129(14) . Co2 N4 2.173(16) . Co2 N4 2.173(16) 2_765 Co2 N4 2.173(16) 3_675 Co1 N2 2.162(14) 2_665 Co1 N2 2.162(14) . Co1 N2 2.162(14) 3_565 Co1 N1 2.171(15) 2_665 Co1 N1 2.171(15) . Co1 N1 2.171(15) 3_565 O14 V3 1.914(10) 2_765 O14 V5 1.939(10) 2_765 O13 V4 1.997(12) 2_765 O11 V2 1.990(11) 2_765 O11 V3 1.994(10) 2_765 O9 V5 1.960(12) 3_675 O9 Sb1 1.985(11) 3_675 O7 V4 1.933(11) 2_765 N3 C3 1.46(2) . N1 C1 1.44(3) . C3 C4 1.55(3) . C1 C2 1.42(2) . N2 C2 1.39(3) . N4 C4 1.48(3) .