#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:22:58 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185228 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/52/7225238.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_7225238 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 'H16 O48 Sb8 V14' _chemical_formula_weight 2471.29 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 109.348(9) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.6766(10) _cell_length_b 11.9042(5) _cell_length_c 19.2758(15) _cell_measurement_reflns_used 4048 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.33 _cell_measurement_theta_min 3.42 _cell_volume 2961.0(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _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 0.854 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_unetI/netI 0.0503 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.854 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 16739 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.854 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.187 _diffrn_reflns_theta_min 3.157 _exptl_absorpt_coefficient_mu 5.764 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83285 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.772 _exptl_crystal_description polyhedron _exptl_crystal_F_000 2260 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _refine_diff_density_max 3.242 _refine_diff_density_min -2.367 _refine_diff_density_rms 0.301 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 6841 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0676 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+86.6103P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1731 _refine_ls_wR_factor_ref 0.2071 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4914 _reflns_number_total 6841 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00616g2.cif _cod_data_source_block shelx_4 _cod_depositor_comments 'Adding full bibliography for 7225235--7225239.cif.' _cod_database_code 7225238 _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 0.392 _shelx_estimated_absorpt_t_max 0.545 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL ghy2-2_a.res in P2(1)/n REM Old TITL GHy2-2 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.158, Rweak 0.008, Alpha 0.016, Orientation as input REM Formula found by SHELXT: O5 Si17 Cu7 W4 CELL 0.71073 13.676609 11.904212 19.275765 90 109.3479 90 ZERR 2 0.001005 0.000537 0.001509 0 0.0085 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC H O Sb V UNIT 32 96 16 28 L.S. 14 PLAN 30 BOND $H LIST 6 ACTA SIZE 0.20*0.14*0.12 ISOR 0.001 o1w o2w o3w o4w o5w WGHT 0.087900 86.610298 FVAR 0.13354 SB4 3 0.713035 0.044713 -0.222142 11.00000 0.03477 0.02139 = 0.03637 0.00134 0.00143 0.00058 SB3 3 1.101460 0.387863 0.039236 11.00000 0.03824 0.01934 = 0.04487 0.00174 0.00336 -0.00312 SB2 3 0.950320 0.099279 -0.252799 11.00000 0.04304 0.02515 = 0.04003 0.00334 0.01121 0.00055 SB1 3 0.859618 0.337913 0.067289 11.00000 0.04421 0.02844 = 0.04456 -0.00065 0.01011 0.00293 V7 4 0.884502 0.267545 -0.112524 11.00000 0.03584 0.01733 = 0.03661 0.00247 0.00237 0.00170 V6 4 1.085886 0.175912 0.176432 11.00000 0.03879 0.01754 = 0.03744 -0.00231 0.00325 0.00022 V5 4 0.732542 0.136538 -0.053944 11.00000 0.03452 0.02804 = 0.04225 -0.00120 0.00626 0.00096 V4 4 0.750235 -0.163441 -0.098747 11.00000 0.03445 0.02427 = 0.04562 0.00322 0.00686 0.00061 V3 4 0.887563 -0.225217 0.099510 11.00000 0.04080 0.02859 = 0.05370 0.00034 0.01295 -0.00335 V2 4 0.869062 0.075559 0.141828 11.00000 0.04252 0.03053 = 0.05523 0.00350 0.01273 0.00152 V1 4 0.730532 -0.065953 0.031262 11.00000 0.05335 0.05091 = 0.08184 0.00420 0.02186 -0.00331 O21 2 0.786773 0.140055 -0.136210 11.00000 0.03802 0.02148 = 0.03998 -0.00367 0.00688 -0.00243 O20 2 0.796611 -0.086275 -0.171490 11.00000 0.04060 0.02720 = 0.03874 0.00630 0.00908 0.00668 O19 2 0.939578 0.212709 0.123146 11.00000 0.04292 0.02554 = 0.04259 0.00423 -0.00047 -0.00094 O18 2 0.834505 0.259203 -0.026219 11.00000 0.05674 0.02627 = 0.03758 -0.00939 0.01369 -0.00997 O17 2 0.969659 0.193133 -0.163757 11.00000 0.03637 0.02414 = 0.04956 -0.00454 0.00766 -0.00133 O16 2 1.027077 0.300444 -0.049120 11.00000 0.03664 0.02389 = 0.04531 -0.01159 0.00297 0.00076 O15 2 1.015216 0.041074 0.193497 11.00000 0.03767 0.02533 = 0.04500 0.00184 0.00691 -0.00406 O14 2 1.130552 0.252665 0.102792 11.00000 0.03998 0.02865 = 0.04393 0.01046 0.00988 0.00761 O13 2 0.834755 0.378711 -0.156941 11.00000 0.04472 0.02483 = 0.04894 0.00933 0.00522 0.00807 O12 2 0.973373 0.427577 0.057662 11.00000 0.04320 0.02056 = 0.06625 0.00141 0.01415 0.00320 O11 2 0.707424 -0.022146 -0.071866 11.00000 0.03915 0.02279 = 0.05017 0.00028 0.01064 0.00375 O10 2 0.801461 0.084534 -0.278289 11.00000 0.04661 0.03475 = 0.03901 0.00788 0.00482 -0.00500 O9 2 0.785908 -0.202626 0.002973 11.00000 0.04723 0.03141 = 0.05551 0.00184 0.01418 0.00024 O8 2 0.843373 -0.082315 0.123741 11.00000 0.04360 0.02781 = 0.05342 -0.00276 0.01350 -0.00284 O7 2 0.646387 -0.228511 -0.141098 11.00000 0.05118 0.02574 = 0.06861 -0.00590 0.02208 -0.00497 O6 2 1.117708 0.250008 0.248842 11.00000 0.06029 0.02953 = 0.03675 -0.00694 0.00056 0.00016 O5 2 0.766400 0.093387 0.047499 11.00000 0.04239 0.03435 = 0.04578 0.00341 0.01011 0.00431 O4 2 0.621448 0.194042 -0.079362 11.00000 0.04268 0.04509 = 0.06805 0.00178 0.00477 0.01474 O3 2 0.842630 -0.321154 0.138038 11.00000 0.06062 0.04377 = 0.07165 0.01289 0.01714 -0.00733 O2 2 0.818455 0.106688 0.202696 11.00000 0.07820 0.05371 = 0.07527 -0.00771 0.04226 0.00652 O1 2 0.619242 -0.089157 0.041890 11.00000 0.06608 0.08654 = 0.12075 0.00392 0.04819 0.00022 O1W 2 0.866708 0.933336 0.623930 11.00000 0.08981 0.08883 = 0.09038 0.00004 0.03043 -0.00032 O2W 2 0.963432 0.547294 0.358956 10.50000 0.14729 0.14765 = 0.14797 0.00040 0.04919 -0.00038 O3W 2 0.618556 0.615144 0.126474 10.50000 0.25124 0.25146 = 0.25132 0.00009 0.08329 -0.00020 O4W 2 0.804585 0.327653 0.284975 10.50000 0.26666 0.26653 = 0.26643 -0.00010 0.08854 -0.00016 O5W 2 0.959263 -0.014412 0.014755 10.50000 0.15531 0.15499 = 0.15521 -0.00020 0.05100 0.00016 HKLF 4 REM ghy2-2_a.res in P2(1)/n REM R1 = 0.0676 for 4914 Fo > 4sig(Fo) and 0.1011 for all 6841 data REM 334 parameters refined using 30 restraints END WGHT 0.0757 78.9520 REM Highest difference peak 3.242, deepest hole -2.367, 1-sigma level 0.301 Q1 1 0.8930 0.0480 0.1063 11.00000 0.05 3.24 Q2 1 0.7337 0.2991 0.0923 11.00000 0.05 2.22 Q3 1 0.9021 -0.1649 0.0689 11.00000 0.05 2.19 Q4 1 0.7638 0.0488 -0.2393 11.00000 0.05 2.16 Q5 1 0.7633 0.4735 0.0146 11.00000 0.05 2.09 Q6 1 0.9002 0.4342 0.1645 11.00000 0.05 2.09 Q7 1 1.0432 0.3960 0.0547 11.00000 0.05 2.06 Q8 1 0.8986 0.0966 -0.2394 11.00000 0.05 1.98 Q9 1 0.9574 0.5135 0.3008 11.00000 0.05 1.95 Q10 1 0.9215 0.1005 -0.2933 11.00000 0.05 1.82 Q11 1 0.7258 0.3453 0.2362 11.00000 0.05 1.68 Q12 1 0.9371 0.6433 0.3888 11.00000 0.05 1.68 Q13 1 0.9428 0.6621 0.4020 11.00000 0.05 1.66 Q14 1 0.7399 0.0554 -0.1846 11.00000 0.05 1.63 Q15 1 0.9174 0.3433 0.0532 11.00000 0.05 1.62 Q16 1 0.8544 1.0749 0.5125 11.00000 0.05 1.59 Q17 1 0.6646 0.0530 -0.2037 11.00000 0.05 1.58 Q18 1 0.5991 0.6177 -0.0176 11.00000 0.05 1.48 Q19 1 1.1587 0.3804 0.0220 11.00000 0.05 1.39 Q20 1 0.9407 0.0979 -0.2747 11.00000 0.05 1.33 Q21 1 0.9944 0.1152 -0.2005 11.00000 0.05 1.30 Q22 1 0.9341 0.3761 0.2930 11.00000 0.05 1.29 Q23 1 1.0034 0.0848 -0.2711 11.00000 0.05 1.28 Q24 1 0.8969 -0.4221 0.1880 11.00000 0.05 1.25 Q25 1 0.9823 0.5518 0.3879 11.00000 0.05 1.24 Q26 1 0.9360 0.4275 0.3125 11.00000 0.05 1.23 Q27 1 1.1218 0.3583 0.0824 11.00000 0.05 1.20 Q28 1 0.8011 0.3400 0.0842 11.00000 0.05 1.14 Q29 1 0.6803 0.0411 -0.2675 11.00000 0.05 1.12 Q30 1 0.6378 0.6186 0.0320 11.00000 0.05 1.10 ; _shelx_res_checksum 63052 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_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_adp _atom_site_refinement_flags_occupancy Sb4 Sb 0.71304(6) 0.04471(7) -0.22214(5) 0.0334(2) Uani 1 1 d . . Sb3 Sb 1.10146(7) 0.38786(7) 0.03924(5) 0.0367(2) Uani 1 1 d . . Sb2 Sb 0.95032(7) 0.09928(7) -0.25280(5) 0.0367(2) Uani 1 1 d . . Sb1 Sb 0.85962(7) 0.33791(7) 0.06729(5) 0.0402(2) Uani 1 1 d . . V7 V 0.88450(17) 0.26755(16) -0.11252(12) 0.0323(5) Uani 1 1 d . . V6 V 1.08589(17) 0.17591(16) 0.17643(12) 0.0336(5) Uani 1 1 d . . V5 V 0.73254(17) 0.13654(19) -0.05394(13) 0.0365(5) Uani 1 1 d . . V4 V 0.75023(17) -0.16344(18) -0.09875(13) 0.0364(5) Uani 1 1 d . . V3 V 0.88756(19) -0.22522(19) 0.09951(14) 0.0417(6) Uani 1 1 d . . V2 V 0.86906(19) 0.0756(2) 0.14183(15) 0.0436(6) Uani 1 1 d . . V1 V 0.7305(2) -0.0660(3) 0.0313(2) 0.0622(8) Uani 1 1 d . . O21 O 0.7868(7) 0.1401(7) -0.1362(5) 0.0347(19) Uani 1 1 d . . O20 O 0.7966(7) -0.0863(7) -0.1715(5) 0.037(2) Uani 1 1 d . . O19 O 0.9396(7) 0.2127(7) 0.1231(5) 0.041(2) Uani 1 1 d . . O18 O 0.8345(8) 0.2592(7) -0.0262(5) 0.041(2) Uani 1 1 d . . O17 O 0.9697(7) 0.1931(7) -0.1638(5) 0.038(2) Uani 1 1 d . . O16 O 1.0271(7) 0.3004(7) -0.0491(5) 0.038(2) Uani 1 1 d . . O15 O 1.0152(7) 0.0411(7) 0.1935(5) 0.038(2) Uani 1 1 d . . O14 O 1.1306(7) 0.2527(7) 0.1028(5) 0.039(2) Uani 1 1 d . . O13 O 0.8348(7) 0.3787(7) -0.1569(5) 0.042(2) Uani 1 1 d . . O12 O 0.9734(7) 0.4276(7) 0.0577(6) 0.044(2) Uani 1 1 d . . O11 O 0.7074(7) -0.0221(7) -0.0719(5) 0.038(2) Uani 1 1 d . . O10 O 0.8015(8) 0.0845(8) -0.2783(5) 0.042(2) Uani 1 1 d . . O9 O 0.7859(8) -0.2026(8) 0.0030(6) 0.045(2) Uani 1 1 d . . O8 O 0.8434(7) -0.0823(8) 0.1237(6) 0.042(2) Uani 1 1 d . . O7 O 0.6464(8) -0.2285(8) -0.1411(6) 0.048(2) Uani 1 1 d . . O6 O 1.1177(8) 0.2500(8) 0.2488(5) 0.046(2) Uani 1 1 d . . O5 O 0.7664(7) 0.0934(8) 0.0475(5) 0.042(2) Uani 1 1 d . . O4 O 0.6214(8) 0.1940(9) -0.0794(6) 0.055(3) Uani 1 1 d . . O3 O 0.8426(9) -0.3212(9) 0.1380(7) 0.060(3) Uani 1 1 d . . O2 O 0.8185(10) 0.1067(10) 0.2027(7) 0.065(3) Uani 1 1 d . . O1 O 0.6192(11) -0.0892(14) 0.0419(9) 0.087(4) Uani 1 1 d . . O1W O 0.8667(12) 0.9333(14) 0.6239(9) 0.090(4) Uani 1 1 d U . O2W O 0.963(4) 0.547(4) 0.359(3) 0.148(16) Uani 0.5 1 d U P O3W O 0.619(6) 0.615(7) 0.126(5) 0.25(3) Uani 0.5 1 d U P O4W O 0.805(6) 0.328(7) 0.285(4) 0.27(3) Uani 0.5 1 d U P O5W O 0.959(4) -0.014(5) 0.015(3) 0.155(17) Uani 0.5 1 d U 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 Sb4 0.0348(4) 0.0214(4) 0.0364(5) 0.0013(3) 0.0014(3) 0.0006(3) Sb3 0.0382(5) 0.0193(4) 0.0449(5) 0.0017(3) 0.0034(4) -0.0031(3) Sb2 0.0430(5) 0.0252(4) 0.0400(5) 0.0033(3) 0.0112(4) 0.0005(3) Sb1 0.0442(5) 0.0284(4) 0.0446(5) -0.0007(4) 0.0101(4) 0.0029(4) V7 0.0358(11) 0.0173(9) 0.0366(11) 0.0025(8) 0.0024(9) 0.0017(8) V6 0.0388(11) 0.0175(9) 0.0374(11) -0.0023(8) 0.0032(9) 0.0002(8) V5 0.0345(11) 0.0280(10) 0.0423(12) -0.0012(9) 0.0063(9) 0.0010(9) V4 0.0345(11) 0.0243(10) 0.0456(13) 0.0032(9) 0.0069(10) 0.0006(8) V3 0.0408(12) 0.0286(11) 0.0537(15) 0.0003(10) 0.0130(11) -0.0033(9) V2 0.0425(13) 0.0305(11) 0.0552(15) 0.0035(11) 0.0127(11) 0.0015(10) V1 0.0533(16) 0.0509(17) 0.082(2) 0.0042(16) 0.0219(15) -0.0033(13) O21 0.038(5) 0.021(4) 0.040(5) -0.004(4) 0.007(4) -0.002(3) O20 0.041(5) 0.027(4) 0.039(5) 0.006(4) 0.009(4) 0.007(4) O19 0.043(5) 0.026(4) 0.043(5) 0.004(4) 0.000(4) -0.001(4) O18 0.057(6) 0.026(4) 0.038(5) -0.009(4) 0.014(4) -0.010(4) O17 0.036(5) 0.024(4) 0.050(5) -0.005(4) 0.008(4) -0.001(4) O16 0.037(5) 0.024(4) 0.045(5) -0.012(4) 0.003(4) 0.001(4) O15 0.038(5) 0.025(4) 0.045(5) 0.002(4) 0.007(4) -0.004(4) O14 0.040(5) 0.029(4) 0.044(5) 0.010(4) 0.010(4) 0.008(4) O13 0.045(5) 0.025(4) 0.049(6) 0.009(4) 0.005(4) 0.008(4) O12 0.043(5) 0.021(4) 0.066(7) 0.001(4) 0.014(5) 0.003(4) O11 0.039(5) 0.023(4) 0.050(5) 0.000(4) 0.011(4) 0.004(4) O10 0.047(5) 0.035(5) 0.039(5) 0.008(4) 0.005(4) -0.005(4) O9 0.047(5) 0.031(5) 0.056(6) 0.002(4) 0.014(5) 0.000(4) O8 0.044(5) 0.028(4) 0.053(6) -0.003(4) 0.013(5) -0.003(4) O7 0.051(6) 0.026(5) 0.069(7) -0.006(5) 0.022(5) -0.005(4) O6 0.060(6) 0.030(5) 0.037(5) -0.007(4) 0.001(4) 0.000(4) O5 0.042(5) 0.034(5) 0.046(5) 0.003(4) 0.010(4) 0.004(4) O4 0.043(6) 0.045(6) 0.068(7) 0.002(5) 0.005(5) 0.015(5) O3 0.061(7) 0.044(6) 0.072(8) 0.013(6) 0.017(6) -0.007(5) O2 0.078(8) 0.054(7) 0.075(8) -0.008(6) 0.042(7) 0.007(6) O1 0.066(8) 0.087(10) 0.121(13) 0.004(10) 0.048(9) 0.000(8) O1W 0.090(5) 0.089(5) 0.090(5) 0.000(2) 0.030(2) 0.000(2) O2W 0.147(16) 0.148(16) 0.148(16) 0.000(2) 0.049(6) 0.000(2) O3W 0.25(3) 0.25(3) 0.25(3) 0.000(2) 0.083(9) 0.000(2) O4W 0.27(3) 0.27(3) 0.27(3) 0.000(2) 0.089(10) 0.000(2) O5W 0.155(17) 0.155(17) 0.155(17) 0.000(2) 0.051(6) 0.000(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 O10 Sb4 O21 95.0(4) . . O10 Sb4 O20 95.9(4) . . O21 Sb4 O20 89.3(4) . . O12 Sb3 O16 92.7(4) . . O12 Sb3 O14 95.3(4) . . O16 Sb3 O14 92.6(4) . . O10 Sb2 O17 95.6(4) . . O10 Sb2 O15 95.7(4) . 3_755 O17 Sb2 O15 92.1(4) . 3_755 O12 Sb1 O19 98.8(4) . . O12 Sb1 O18 94.4(4) . . O19 Sb1 O18 92.2(4) . . O13 V7 O16 109.0(4) . . O13 V7 O17 108.7(5) . . O16 V7 O17 76.8(4) . . O13 V7 O21 112.1(4) . . O16 V7 O21 138.8(4) . . O17 V7 O21 90.3(4) . . O13 V7 O18 106.5(5) . . O16 V7 O18 92.0(4) . . O17 V7 O18 144.8(4) . . O21 V7 O18 76.2(4) . . O13 V7 V3 114.7(4) . 3_755 O16 V7 V3 38.3(3) . 3_755 O17 V7 V3 38.5(3) . 3_755 O21 V7 V3 118.8(3) . 3_755 O18 V7 V3 122.6(3) . 3_755 O13 V7 V5 113.2(4) . . O16 V7 V5 121.4(3) . . O17 V7 V5 122.4(3) . . O21 V7 V5 38.0(3) . . O18 V7 V5 38.3(3) . . V3 V7 V5 132.11(9) 3_755 . O6 V6 O14 108.6(5) . . O6 V6 O15 108.4(5) . . O14 V6 O15 143.0(4) . . O6 V6 O20 110.8(5) . 3_755 O14 V6 O20 76.1(4) . 3_755 O15 V6 O20 91.2(4) . 3_755 O6 V6 O19 105.7(5) . . O14 V6 O19 91.5(4) . . O15 V6 O19 78.3(4) . . O20 V6 O19 143.5(4) 3_755 . O6 V6 V2 111.9(4) . . O14 V6 V2 122.7(3) . . O15 V6 V2 38.7(3) . . O20 V6 V2 121.9(3) 3_755 . O19 V6 V2 39.6(3) . . O6 V6 V4 115.0(4) . 3_755 O14 V6 V4 38.3(3) . 3_755 O15 V6 V4 121.4(3) . 3_755 O20 V6 V4 37.8(3) 3_755 3_755 O19 V6 V4 122.2(3) . 3_755 V2 V6 V4 133.11(10) . 3_755 O4 V5 O5 108.2(5) . . O4 V5 O11 105.7(5) . . O5 V5 O11 83.6(4) . . O4 V5 O21 108.7(5) . . O5 V5 O21 143.1(4) . . O11 V5 O21 88.2(4) . . O4 V5 O18 106.5(5) . . O5 V5 O18 90.7(4) . . O11 V5 O18 147.5(4) . . O21 V5 O18 77.3(4) . . O4 V5 V1 110.0(5) . . O5 V5 V1 41.6(3) . . O11 V5 V1 42.2(3) . . O21 V5 V1 123.3(3) . . O18 V5 V1 126.7(3) . . O4 V5 V7 111.1(5) . . O5 V5 V7 122.7(3) . . O11 V5 V7 121.9(3) . . O21 V5 V7 38.3(2) . . O18 V5 V7 39.1(3) . . V1 V5 V7 138.86(11) . . O7 V4 O11 105.5(5) . . O7 V4 O9 106.8(5) . . O11 V4 O9 86.2(4) . . O7 V4 O20 108.0(5) . . O11 V4 O20 89.0(4) . . O9 V4 O20 144.9(4) . . O7 V4 O14 109.2(5) . 3_755 O11 V4 O14 145.0(4) . 3_755 O9 V4 O14 88.6(4) . 3_755 O20 V4 O14 75.8(4) . 3_755 O7 V4 V1 108.8(4) . . O11 V4 V1 43.7(3) . . O9 V4 V1 42.8(3) . . O20 V4 V1 126.0(3) . . O14 V4 V1 125.1(3) 3_755 . O7 V4 V6 113.4(4) . 3_755 O11 V4 V6 120.8(3) . 3_755 O9 V4 V6 120.4(3) . 3_755 O20 V4 V6 38.0(3) . 3_755 O14 V4 V6 37.8(3) 3_755 3_755 V1 V4 V6 137.82(11) . 3_755 O3 V3 O8 108.8(6) . . O3 V3 O9 106.4(5) . . O8 V3 O9 85.8(4) . . O3 V3 O16 106.7(5) . 3_755 O8 V3 O16 144.4(4) . 3_755 O9 V3 O16 86.7(4) . 3_755 O3 V3 O17 107.5(5) . 3_755 O8 V3 O17 90.1(4) . 3_755 O9 V3 O17 145.3(4) . 3_755 O16 V3 O17 76.8(4) 3_755 3_755 O3 V3 V1 110.2(5) . . O8 V3 V1 43.0(3) . . O9 V3 V1 43.2(3) . . O16 V3 V1 123.9(3) 3_755 . O17 V3 V1 126.9(3) 3_755 . O3 V3 V7 112.4(5) . 3_755 O8 V3 V7 121.2(3) . 3_755 O9 V3 V7 119.0(3) . 3_755 O16 V3 V7 38.3(3) 3_755 3_755 O17 V3 V7 38.5(3) 3_755 3_755 V1 V3 V7 137.34(12) . 3_755 O2 V2 O5 108.3(6) . . O2 V2 O8 105.3(6) . . O5 V2 O8 84.4(4) . . O2 V2 O15 107.1(6) . . O5 V2 O15 144.5(4) . . O8 V2 O15 89.0(4) . . O2 V2 O19 107.3(6) . . O5 V2 O19 89.1(4) . . O8 V2 O19 147.2(4) . . O15 V2 O19 77.9(4) . . O2 V2 V1 110.0(5) . . O5 V2 V1 42.5(3) . . O8 V2 V1 42.1(3) . . O15 V2 V1 124.3(3) . . O19 V2 V1 125.9(3) . . O2 V2 V6 112.1(5) . . O5 V2 V6 121.3(3) . . O8 V2 V6 121.8(3) . . O15 V2 V6 38.6(3) . . O19 V2 V6 39.2(3) . . V1 V2 V6 137.94(12) . . O1 V1 O8 111.1(7) . . O1 V1 O9 111.1(7) . . O8 V1 O9 84.8(4) . . O1 V1 O5 109.9(7) . . O8 V1 O5 82.5(4) . . O9 V1 O5 138.9(4) . . O1 V1 O11 109.1(7) . . O8 V1 O11 139.7(4) . . O9 V1 O11 83.5(4) . . O5 V1 O11 81.6(4) . . O1 V1 V3 115.1(6) . . O8 V1 V3 42.2(3) . . O9 V1 V3 42.9(3) . . O5 V1 V3 117.5(3) . . O11 V1 V3 119.1(3) . . O1 V1 V4 114.0(6) . . O8 V1 V4 119.2(3) . . O9 V1 V4 41.9(3) . . O5 V1 V4 116.3(3) . . O11 V1 V4 41.8(3) . . V3 V1 V4 81.86(11) . . O1 V1 V2 114.8(6) . . O8 V1 V2 41.6(3) . . O9 V1 V2 118.3(3) . . O5 V1 V2 41.1(3) . . O11 V1 V2 115.9(3) . . V3 V1 V2 80.59(11) . . V4 V1 V2 131.09(13) . . O1 V1 V5 113.2(6) . . O8 V1 V5 116.5(3) . . O9 V1 V5 117.1(3) . . O5 V1 V5 40.7(3) . . O11 V1 V5 41.0(3) . . V3 V1 V5 131.65(13) . . V4 V1 V5 79.67(11) . . V2 V1 V5 78.87(10) . . V5 O21 V7 103.8(4) . . V5 O21 Sb4 116.0(4) . . V7 O21 Sb4 138.6(5) . . V4 O20 V6 104.2(4) . 3_755 V4 O20 Sb4 116.9(5) . . V6 O20 Sb4 138.7(5) 3_755 . Sb1 O19 V6 138.1(5) . . Sb1 O19 V2 120.7(5) . . V6 O19 V2 101.1(4) . . Sb1 O18 V5 119.8(5) . . Sb1 O18 V7 137.6(5) . . V5 O18 V7 102.6(4) . . V7 O17 V3 103.0(4) . 3_755 V7 O17 Sb2 138.9(5) . . V3 O17 Sb2 118.1(5) 3_755 . V3 O16 V7 103.4(4) 3_755 . V3 O16 Sb3 116.6(4) 3_755 . V7 O16 Sb3 139.9(5) . . V6 O15 V2 102.7(4) . . V6 O15 Sb2 138.5(5) . 3_755 V2 O15 Sb2 118.4(4) . 3_755 V6 O14 V4 103.9(4) . 3_755 V6 O14 Sb3 141.6(5) . . V4 O14 Sb3 114.4(5) 3_755 . Sb1 O12 Sb3 132.6(5) . . V4 O11 V5 149.2(5) . . V4 O11 V1 94.5(4) . . V5 O11 V1 96.8(4) . . Sb4 O10 Sb2 132.9(5) . . V4 O9 V3 151.1(6) . . V4 O9 V1 95.3(4) . . V3 O9 V1 94.0(5) . . V3 O8 V2 149.3(6) . . V3 O8 V1 94.8(4) . . V2 O8 V1 96.3(4) . . V2 O5 V5 148.5(6) . . V2 O5 V1 96.4(4) . . V5 O5 V1 97.6(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb4 O10 1.930(10) . Sb4 O21 1.985(8) . Sb4 O20 1.988(8) . Sb3 O12 1.957(10) . Sb3 O16 1.967(8) . Sb3 O14 1.982(9) . Sb2 O10 1.938(10) . Sb2 O17 1.991(9) . Sb2 O15 1.991(9) 3_755 Sb1 O12 1.946(10) . Sb1 O19 1.948(9) . Sb1 O18 1.958(9) . V7 O13 1.600(9) . V7 O16 1.967(9) . V7 O17 1.969(10) . V7 O21 1.973(9) . V7 O18 2.000(10) . V7 V3 3.085(3) 3_755 V7 V5 3.095(3) . V6 O6 1.585(9) . V6 O14 1.949(9) . V6 O15 1.957(9) . V6 O20 1.958(9) 3_755 V6 O19 1.972(9) . V6 V2 3.059(3) . V6 V4 3.084(3) 3_755 V5 O4 1.589(10) . V5 O5 1.924(10) . V5 O11 1.931(9) . V5 O21 1.961(9) . V5 O18 1.967(9) . V5 V1 2.922(4) . V4 O7 1.586(10) . V4 O11 1.908(9) . V4 O9 1.915(11) . V4 O20 1.950(9) . V4 O14 1.969(9) 3_755 V4 V1 2.854(4) . V4 V6 3.084(3) 3_755 V3 O3 1.592(11) . V3 O8 1.914(10) . V3 O9 1.937(10) . V3 O16 1.965(9) 3_755 V3 O17 1.972(9) 3_755 V3 V1 2.840(4) . V3 V7 3.085(3) 3_755 V2 O2 1.591(12) . V2 O5 1.905(10) . V2 O8 1.922(9) . V2 O15 1.959(9) . V2 O19 1.989(9) . V2 V1 2.880(4) . V1 O1 1.625(14) . V1 O8 1.943(10) . V1 O9 1.947(10) . V1 O5 1.958(10) . V1 O11 1.977(10) . O20 V6 1.957(9) 3_755 O17 V3 1.972(9) 3_755 O16 V3 1.965(9) 3_755 O15 Sb2 1.991(9) 3_755 O14 V4 1.969(9) 3_755 O5W O5W 1.45(9) 3_755