# Copyright The Royal Society of Chemistry, 1998 # Paper No: 8/02816H entitled `Synthesis and characterisation of new # vanadates of antimony, ASbV2O8 (A = K, Rb, Tl and Cs). data_ksbv _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'K O8 Sb V2' _chemical_formula_weight 390.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'K' 'K' 0.2009 0.2494 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.6248(10) _cell_length_b 5.5633(10) _cell_length_c 8.5168(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 692.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'rectangular block shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.745 _exptl_crystal_density_method ? _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 7.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 2 _diffrn_reflns_number 676 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0107 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 24.97 _reflns_number_total 676 _reflns_number_observed 649 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD4 programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+7.1089P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 676 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_obs 0.0241 _refine_ls_wR_factor_all 0.0744 _refine_ls_wR_factor_obs 0.0738 _refine_ls_goodness_of_fit_all 1.411 _refine_ls_goodness_of_fit_obs 1.430 _refine_ls_restrained_S_all 1.411 _refine_ls_restrained_S_obs 1.430 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K K 0.38118(14) 0.2500 0.5490(3) 0.0217(5) Uani 1 d S . Sb Sb 0.11784(4) 0.2500 0.68743(6) 0.0053(2) Uani 1 d S . V(1) V 0.28398(9) 0.2500 0.9920(2) 0.0074(3) Uani 1 d S . V(2) V 0.02718(10) 0.2500 0.2933(2) 0.0060(3) Uani 1 d S . O(1) O 0.1796(4) 0.2500 0.8917(7) 0.0121(13) Uani 1 d S . O(2) O 0.2046(3) 0.0089(8) 0.6083(5) 0.0147(9) Uani 1 d . . O(3) O 0.3643(4) 0.2500 0.8660(8) 0.0172(14) Uani 1 d S . O(4) O 0.0457(4) 0.2500 0.4916(7) 0.0108(13) Uani 1 d S . O(5) O 0.0357(3) 0.0029(8) 0.7745(5) 0.0115(9) Uani 1 d . . O(6) O 0.3787(4) -0.2500 0.6993(8) 0.0158(15) Uani 1 d S . 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 K 0.0226(11) 0.0224(11) 0.0200(11) 0.000 0.0036(9) 0.000 Sb 0.0074(3) 0.0012(3) 0.0072(3) 0.000 -0.0007(2) 0.000 V(1) 0.0091(7) 0.0025(7) 0.0106(7) 0.000 -0.0025(6) 0.000 V(2) 0.0089(7) 0.0019(7) 0.0070(7) 0.000 -0.0012(5) 0.000 O(1) 0.010(3) 0.010(3) 0.016(3) 0.000 -0.003(3) 0.000 O(2) 0.014(2) 0.013(2) 0.017(2) -0.005(2) 0.001(2) 0.004(2) O(3) 0.013(3) 0.018(4) 0.020(3) 0.000 0.003(3) 0.000 O(4) 0.014(3) 0.004(3) 0.014(3) 0.000 -0.003(2) 0.000 O(5) 0.015(2) 0.007(2) 0.012(2) 0.002(2) -0.003(2) -0.003(2) O(6) 0.014(3) 0.010(3) 0.024(4) 0.000 -0.004(3) 0.000 _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 K O(3) 2.712(7) . ? K O(2) 2.953(5) . ? K O(2) 2.953(5) 7_565 ? K O(5) 2.987(5) 2_554 ? K O(5) 2.987(5) 8_665 ? K O(5) 3.042(5) 4_556 ? K O(5) 3.042(5) 6_657 ? K O(6) 3.062(3) 1_565 ? K O(6) 3.062(3) . ? K O(1) 3.213(3) 2_554 ? K O(1) 3.213(3) 2_564 ? K V(2) 3.613(3) 6_656 ? Sb O(1) 1.960(6) . ? Sb O(2) 1.966(4) 7_565 ? Sb O(2) 1.966(4) . ? Sb O(5) 1.971(4) . ? Sb O(5) 1.971(4) 7_565 ? Sb O(4) 1.974(6) . ? Sb K 4.126(2) 6_557 ? Sb K 4.149(2) 2_565 ? Sb K 4.149(2) 2 ? V(1) O(3) 1.591(7) . ? V(1) O(1) 1.750(6) . ? V(1) O(2) 1.756(4) 8_666 ? V(1) O(2) 1.756(4) 2 ? V(1) O(6) 2.963(6) 2 ? V(1) K 3.716(2) 2 ? V(1) K 3.716(2) 2_565 ? V(2) O(6) 1.592(6) 2_554 ? V(2) O(4) 1.711(6) . ? V(2) O(5) 1.777(4) 5_556 ? V(2) O(5) 1.777(4) 3_556 ? V(2) O(3) 3.262(3) 2_564 ? V(2) O(3) 3.262(3) 2_554 ? V(2) K 3.613(3) 6_556 ? V(2) K 3.723(2) 2_554 ? V(2) K 3.723(2) 2_564 ? O(1) O(5) 2.705(6) . ? O(1) O(5) 2.705(6) 7_565 ? O(1) O(3) 2.711(9) . ? O(1) O(6) 2.755(9) 2 ? O(1) O(2) 2.786(7) . ? O(1) O(2) 2.786(7) 7_565 ? O(1) O(2) 2.889(7) 8_666 ? O(1) O(2) 2.889(7) 2 ? O(1) K 3.213(3) 2_565 ? O(1) K 3.213(3) 2 ? O(2) V(1) 1.756(4) 2_554 ? O(2) O(2) 2.683(9) 7_565 ? O(2) O(3) 2.711(7) 2_554 ? O(2) O(5) 2.848(6) . ? O(2) O(4) 2.863(7) . ? O(2) O(2) 2.880(9) 7 ? O(2) O(1) 2.889(7) 2_554 ? O(2) O(6) 3.026(7) . ? O(2) O(3) 3.475(7) . ? O(3) O(2) 2.711(7) 8_666 ? O(3) O(2) 2.711(7) 2 ? O(3) O(4) 2.916(9) 6_657 ? O(3) O(5) 3.098(7) 4_556 ? O(3) O(5) 3.098(7) 6_657 ? O(3) O(6) 3.130(4) . ? O(3) O(6) 3.130(4) 1_565 ? O(3) O(4) 3.258(5) 2_565 ? O(3) O(4) 3.258(5) 2 ? O(4) O(6) 2.724(9) 2_554 ? O(4) O(5) 2.778(7) 7_565 ? O(4) O(5) 2.778(7) . ? O(4) O(2) 2.863(7) 7_565 ? O(4) O(3) 2.916(9) 6_557 ? O(4) O(5) 2.920(7) 5_556 ? O(4) O(5) 2.920(7) 3_556 ? O(4) O(4) 3.089(5) 5_556 ? O(4) O(4) 3.089(5) 5_566 ? O(5) V(2) 1.777(4) 5_556 ? O(5) O(6) 2.701(6) 6_557 ? O(5) O(5) 2.749(9) 7_565 ? O(5) O(5) 2.814(9) 7 ? O(5) O(4) 2.920(7) 5_556 ? O(5) K 2.987(5) 2 ? O(5) K 3.042(5) 6_557 ? O(5) O(3) 3.098(7) 6_557 ? O(6) V(2) 1.592(6) 2 ? O(6) O(5) 2.701(6) 6_657 ? O(6) O(5) 2.701(6) 4_546 ? O(6) O(4) 2.724(9) 2 ? O(6) O(1) 2.755(9) 2_554 ? O(6) V(1) 2.963(6) 2_554 ? O(6) O(2) 3.026(7) 7 ? O(6) K 3.062(3) 1_545 ? O(6) O(3) 3.130(4) 1_545 ? 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 O(3) K O(2) 75.5(2) . . ? O(3) K O(2) 75.5(2) . 7_565 ? O(2) K O(2) 54.0(2) . 7_565 ? O(3) K O(5) 144.71(13) . 2_554 ? O(2) K O(5) 106.01(12) . 2_554 ? O(2) K O(5) 134.73(14) 7_565 2_554 ? O(3) K O(5) 144.71(13) . 8_665 ? O(2) K O(5) 134.73(14) . 8_665 ? O(2) K O(5) 106.01(12) 7_565 8_665 ? O(5) K O(5) 56.2(2) 2_554 8_665 ? O(3) K O(5) 64.86(15) . 4_556 ? O(2) K O(5) 140.35(13) . 4_556 ? O(2) K O(5) 111.07(12) 7_565 4_556 ? O(5) K O(5) 107.29(10) 2_554 4_556 ? O(5) K O(5) 82.62(12) 8_665 4_556 ? O(3) K O(5) 64.86(15) . 6_657 ? O(2) K O(5) 111.07(12) . 6_657 ? O(2) K O(5) 140.35(13) 7_565 6_657 ? O(5) K O(5) 82.62(12) 2_554 6_657 ? O(5) K O(5) 107.29(10) 8_665 6_657 ? O(5) K O(5) 53.7(2) 4_556 6_657 ? O(3) K O(6) 65.33(12) . 1_565 ? O(2) K O(6) 109.3(2) . 1_565 ? O(2) K O(6) 60.37(15) 7_565 1_565 ? O(5) K O(6) 139.4(2) 2_554 1_565 ? O(5) K O(6) 84.49(14) 8_665 1_565 ? O(5) K O(6) 52.52(14) 4_556 1_565 ? O(5) K O(6) 102.26(15) 6_657 1_565 ? O(3) K O(6) 65.33(12) . . ? O(2) K O(6) 60.37(15) . . ? O(2) K O(6) 109.3(2) 7_565 . ? O(5) K O(6) 84.49(14) 2_554 . ? O(5) K O(6) 139.4(2) 8_665 . ? O(5) K O(6) 102.26(15) 4_556 . ? O(5) K O(6) 52.52(14) 6_657 . ? O(6) K O(6) 130.6(2) 1_565 . ? O(3) K O(1) 112.96(12) . 2_554 ? O(2) K O(1) 55.68(14) . 2_554 ? O(2) K O(1) 102.88(14) 7_565 2_554 ? O(5) K O(1) 51.57(13) 2_554 2_554 ? O(5) K O(1) 101.20(15) 8_665 2_554 ? O(5) K O(1) 143.38(13) 4_556 2_554 ? O(5) K O(1) 91.16(13) 6_657 2_554 ? O(6) K O(1) 163.3(2) 1_565 2_554 ? O(6) K O(1) 52.02(15) . 2_554 ? O(3) K O(1) 112.96(12) . 2_564 ? O(2) K O(1) 102.88(14) . 2_564 ? O(2) K O(1) 55.68(14) 7_565 2_564 ? O(5) K O(1) 101.20(15) 2_554 2_564 ? O(5) K O(1) 51.57(13) 8_665 2_564 ? O(5) K O(1) 91.16(13) 4_556 2_564 ? O(5) K O(1) 143.38(13) 6_657 2_564 ? O(6) K O(1) 52.02(15) 1_565 2_564 ? O(6) K O(1) 163.3(2) . 2_564 ? O(1) K O(1) 120.0(2) 2_554 2_564 ? O(3) K V(2) 149.0(2) . 6_656 ? O(2) K V(2) 130.89(10) . 6_656 ? O(2) K V(2) 130.89(10) 7_565 6_656 ? O(5) K V(2) 29.32(8) 2_554 6_656 ? O(5) K V(2) 29.32(8) 8_665 6_656 ? O(5) K V(2) 87.70(9) 4_556 6_656 ? O(5) K V(2) 87.70(9) 6_657 6_656 ? O(6) K V(2) 110.13(12) 1_565 6_656 ? O(6) K V(2) 110.13(12) . 6_656 ? O(1) K V(2) 80.04(12) 2_554 6_656 ? O(1) K V(2) 80.04(12) 2_564 6_656 ? O(1) Sb O(2) 90.4(2) . 7_565 ? O(1) Sb O(2) 90.4(2) . . ? O(2) Sb O(2) 86.0(3) 7_565 . ? O(1) Sb O(5) 87.0(2) . . ? O(2) Sb O(5) 177.1(2) 7_565 . ? O(2) Sb O(5) 92.7(2) . . ? O(1) Sb O(5) 87.0(2) . 7_565 ? O(2) Sb O(5) 92.7(2) 7_565 7_565 ? O(2) Sb O(5) 177.1(2) . 7_565 ? O(5) Sb O(5) 88.4(2) . 7_565 ? O(1) Sb O(4) 175.1(2) . . ? O(2) Sb O(4) 93.2(2) 7_565 . ? O(2) Sb O(4) 93.2(2) . . ? O(5) Sb O(4) 89.5(2) . . ? O(5) Sb O(4) 89.5(2) 7_565 . ? O(1) Sb K 79.6(2) . . ? O(2) Sb K 44.13(13) 7_565 . ? O(2) Sb K 44.13(13) . . ? O(5) Sb K 133.90(12) . . ? O(5) Sb K 133.90(12) 7_565 . ? O(4) Sb K 105.3(2) . . ? O(1) Sb K 84.5(2) . 6_557 ? O(2) Sb K 136.75(13) 7_565 6_557 ? O(2) Sb K 136.75(13) . 6_557 ? O(5) Sb K 44.24(12) . 6_557 ? O(5) Sb K 44.24(12) 7_565 6_557 ? O(4) Sb K 90.6(2) . 6_557 ? K Sb K 164.06(3) . 6_557 ? O(1) Sb K 48.68(8) . 2_565 ? O(2) Sb K 78.16(13) 7_565 2_565 ? O(2) Sb K 135.20(13) . 2_565 ? O(5) Sb K 100.98(13) . 2_565 ? O(5) Sb K 41.88(12) 7_565 2_565 ? O(4) Sb K 128.96(9) . 2_565 ? K Sb K 102.35(3) . 2_565 ? K Sb K 66.37(4) 6_557 2_565 ? O(1) Sb K 48.68(8) . 2 ? O(2) Sb K 135.20(13) 7_565 2 ? O(2) Sb K 78.16(13) . 2 ? O(5) Sb K 41.88(12) . 2 ? O(5) Sb K 100.98(13) 7_565 2 ? O(4) Sb K 128.96(9) . 2 ? K Sb K 102.35(3) . 2 ? K Sb K 66.37(4) 6_557 2 ? K Sb K 84.19(4) 2_565 2 ? O(3) V(1) O(1) 108.4(3) . . ? O(3) V(1) O(2) 108.1(2) . 8_666 ? O(1) V(1) O(2) 111.0(2) . 8_666 ? O(3) V(1) O(2) 108.1(2) . 2 ? O(1) V(1) O(2) 111.0(2) . 2 ? O(2) V(1) O(2) 110.2(3) 8_666 2 ? O(3) V(1) O(6) 174.2(3) . 2 ? O(1) V(1) O(6) 65.8(2) . 2 ? O(2) V(1) O(6) 74.9(2) 8_666 2 ? O(2) V(1) O(6) 74.9(2) 2 2 ? O(3) V(1) K 124.62(11) . 2 ? O(1) V(1) K 59.77(11) . 2 ? O(2) V(1) K 127.0(2) 8_666 2 ? O(2) V(1) K 51.23(14) 2 2 ? O(6) V(1) K 53.14(6) 2 2 ? O(3) V(1) K 124.62(11) . 2_565 ? O(1) V(1) K 59.77(11) . 2_565 ? O(2) V(1) K 51.23(14) 8_666 2_565 ? O(2) V(1) K 127.0(2) 2 2_565 ? O(6) V(1) K 53.14(6) 2 2_565 ? K V(1) K 96.94(6) 2 2_565 ? O(3) V(1) K 27.0(2) . . ? O(1) V(1) K 81.4(2) . . ? O(2) V(1) K 119.63(15) 8_666 . ? O(2) V(1) K 119.63(15) 2 . ? O(6) V(1) K 147.21(14) 2 . ? K V(1) K 110.57(5) 2 . ? K V(1) K 110.57(5) 2_565 . ? O(6) V(2) O(4) 111.1(3) 2_554 . ? O(6) V(2) O(5) 106.5(2) 2_554 5_556 ? O(4) V(2) O(5) 113.7(2) . 5_556 ? O(6) V(2) O(5) 106.5(2) 2_554 3_556 ? O(4) V(2) O(5) 113.7(2) . 3_556 ? O(5) V(2) O(5) 104.7(3) 5_556 3_556 ? O(6) V(2) O(3) 71.0(2) 2_554 2_564 ? O(4) V(2) O(3) 74.7(2) . 2_564 ? O(5) V(2) O(3) 171.3(2) 5_556 2_564 ? O(5) V(2) O(3) 68.8(2) 3_556 2_564 ? O(6) V(2) O(3) 71.0(2) 2_554 2_554 ? O(4) V(2) O(3) 74.7(2) . 2_554 ? O(5) V(2) O(3) 68.8(2) 5_556 2_554 ? O(5) V(2) O(3) 171.3(2) 3_556 2_554 ? O(3) V(2) O(3) 117.0(2) 2_564 2_554 ? O(6) V(2) K 96.0(2) 2_554 6_556 ? O(4) V(2) K 152.9(2) . 6_556 ? O(5) V(2) K 55.42(14) 5_556 6_556 ? O(5) V(2) K 55.42(14) 3_556 6_556 ? O(3) V(2) K 116.15(11) 2_564 6_556 ? O(3) V(2) K 116.15(11) 2_554 6_556 ? O(6) V(2) K 53.69(10) 2_554 2_554 ? O(4) V(2) K 119.67(11) . 2_554 ? O(5) V(2) K 54.06(14) 5_556 2_554 ? O(5) V(2) K 126.61(15) 3_556 2_554 ? O(3) V(2) K 124.63(12) 2_564 2_554 ? O(3) V(2) K 45.09(12) 2_554 2_554 ? K V(2) K 76.23(5) 6_556 2_554 ? O(6) V(2) K 53.69(10) 2_554 2_564 ? O(4) V(2) K 119.67(11) . 2_564 ? O(5) V(2) K 126.61(15) 5_556 2_564 ? O(5) V(2) K 54.06(14) 3_556 2_564 ? O(3) V(2) K 45.09(12) 2_564 2_564 ? O(3) V(2) K 124.63(12) 2_554 2_564 ? K V(2) K 76.23(5) 6_556 2_564 ? K V(2) K 96.68(6) 2_554 2_564 ? V(1) O(1) Sb 146.6(4) . . ? V(1) O(1) O(5) 149.24(12) . . ? Sb O(1) O(5) 46.69(14) . . ? V(1) O(1) O(5) 149.24(12) . 7_565 ? Sb O(1) O(5) 46.69(14) . 7_565 ? O(5) O(1) O(5) 61.1(2) . 7_565 ? V(1) O(1) O(3) 33.8(2) . . ? Sb O(1) O(3) 112.8(3) . . ? O(5) O(1) O(3) 138.2(2) . . ? O(5) O(1) O(3) 138.2(2) 7_565 . ? V(1) O(1) O(6) 78.8(3) . 2 ? Sb O(1) O(6) 134.6(3) . 2 ? O(5) O(1) O(6) 96.3(2) . 2 ? O(5) O(1) O(6) 96.3(2) 7_565 2 ? O(3) O(1) O(6) 112.6(3) . 2 ? V(1) O(1) O(2) 107.9(3) . . ? Sb O(1) O(2) 44.89(14) . . ? O(5) O(1) O(2) 62.5(2) . . ? O(5) O(1) O(2) 91.6(2) 7_565 . ? O(3) O(1) O(2) 78.4(2) . . ? O(6) O(1) O(2) 149.85(14) 2 . ? V(1) O(1) O(2) 107.9(3) . 7_565 ? Sb O(1) O(2) 44.89(14) . 7_565 ? O(5) O(1) O(2) 91.6(2) . 7_565 ? O(5) O(1) O(2) 62.5(2) 7_565 7_565 ? O(3) O(1) O(2) 78.4(2) . 7_565 ? O(6) O(1) O(2) 149.85(14) 2 7_565 ? O(2) O(1) O(2) 57.6(2) . 7_565 ? V(1) O(1) O(2) 34.57(12) . 8_666 ? Sb O(1) O(2) 146.8(2) . 8_666 ? O(5) O(1) O(2) 160.9(3) . 8_666 ? O(5) O(1) O(2) 116.01(14) 7_565 8_666 ? O(3) O(1) O(2) 57.8(2) . 8_666 ? O(6) O(1) O(2) 64.8(2) 2 8_666 ? O(2) O(1) O(2) 135.7(2) . 8_666 ? O(2) O(1) O(2) 103.65(12) 7_565 8_666 ? V(1) O(1) O(2) 34.57(12) . 2 ? Sb O(1) O(2) 146.8(2) . 2 ? O(5) O(1) O(2) 116.01(14) . 2 ? O(5) O(1) O(2) 160.9(3) 7_565 2 ? O(3) O(1) O(2) 57.8(2) . 2 ? O(6) O(1) O(2) 64.8(2) 2 2 ? O(2) O(1) O(2) 103.65(12) . 2 ? O(2) O(1) O(2) 135.7(2) 7_565 2 ? O(2) O(1) O(2) 59.8(2) 8_666 2 ? V(1) O(1) K 92.2(2) . 2_565 ? Sb O(1) K 104.05(14) . 2_565 ? O(5) O(1) K 112.3(2) . 2_565 ? O(5) O(1) K 59.91(12) 7_565 2_565 ? O(3) O(1) K 108.01(14) . 2_565 ? O(6) O(1) K 61.18(11) 2 2_565 ? O(2) O(1) K 144.6(2) . 2_565 ? O(2) O(1) K 88.90(11) 7_565 2_565 ? O(2) O(1) K 57.60(12) 8_666 2_565 ? O(2) O(1) K 109.1(2) 2 2_565 ? V(1) O(1) K 92.2(2) . 2 ? Sb O(1) K 104.05(14) . 2 ? O(5) O(1) K 59.91(12) . 2 ? O(5) O(1) K 112.3(2) 7_565 2 ? O(3) O(1) K 108.01(14) . 2 ? O(6) O(1) K 61.18(11) 2 2 ? O(2) O(1) K 88.90(11) . 2 ? O(2) O(1) K 144.6(2) 7_565 2 ? O(2) O(1) K 109.1(2) 8_666 2 ? O(2) O(1) K 57.60(12) 2 2 ? K O(1) K 120.0(2) 2_565 2 ? V(1) O(2) Sb 144.5(3) 2_554 . ? V(1) O(2) O(2) 145.11(15) 2_554 7_565 ? Sb O(2) O(2) 46.98(13) . 7_565 ? V(1) O(2) O(3) 33.92(13) 2_554 2_554 ? Sb O(2) O(3) 112.5(2) . 2_554 ? O(2) O(2) O(3) 122.09(12) 7_565 2_554 ? V(1) O(2) O(1) 153.7(2) 2_554 . ? Sb O(2) O(1) 44.70(14) . . ? O(2) O(2) O(1) 61.21(11) 7_565 . ? O(3) O(2) O(1) 150.0(2) 2_554 . ? V(1) O(2) O(5) 110.7(2) 2_554 . ? Sb O(2) O(5) 43.72(12) . . ? O(2) O(2) O(5) 90.66(12) 7_565 . ? O(3) O(2) O(5) 92.8(2) 2_554 . ? O(1) O(2) O(5) 57.4(2) . . ? V(1) O(2) O(4) 105.4(2) 2_554 . ? Sb O(2) O(4) 43.52(14) . . ? O(2) O(2) O(4) 62.05(11) 7_565 . ? O(3) O(2) O(4) 71.5(2) 2_554 . ? O(1) O(2) O(4) 88.2(2) . . ? O(5) O(2) O(4) 58.2(2) . . ? V(1) O(2) O(2) 34.89(15) 2_554 7 ? Sb O(2) O(2) 133.02(13) . 7 ? O(2) O(2) O(2) 180.0(5) 7_565 7 ? O(3) O(2) O(2) 57.91(12) 2_554 7 ? O(1) O(2) O(2) 118.79(11) . 7 ? O(5) O(2) O(2) 89.34(12) . 7 ? O(4) O(2) O(2) 117.95(11) . 7 ? V(1) O(2) O(1) 34.44(12) 2_554 2_554 ? Sb O(2) O(1) 159.7(2) . 2_554 ? O(2) O(2) O(1) 119.90(11) 7_565 2_554 ? O(3) O(2) O(1) 57.8(2) 2_554 2_554 ? O(1) O(2) O(1) 150.5(2) . 2_554 ? O(5) O(2) O(1) 145.1(2) . 2_554 ? O(4) O(2) O(1) 119.2(2) . 2_554 ? O(2) O(2) O(1) 60.10(11) 7 2_554 ? V(1) O(2) K 101.1(2) 2_554 . ? Sb O(2) K 108.3(2) . . ? O(2) O(2) K 62.98(9) 7_565 . ? O(3) O(2) K 115.9(2) 2_554 . ? O(1) O(2) K 92.6(2) . . ? O(5) O(2) K 148.1(2) . . ? O(4) O(2) K 116.0(2) . . ? O(2) O(2) K 117.02(9) 7 . ? O(1) O(2) K 66.72(12) 2_554 . ? V(1) O(2) O(6) 71.0(2) 2_554 . ? Sb O(2) O(6) 141.3(2) . . ? O(2) O(2) O(6) 118.42(10) 7_565 . ? O(3) O(2) O(6) 104.8(2) 2_554 . ? O(1) O(2) O(6) 96.8(2) . . ? O(5) O(2) O(6) 126.7(2) . . ? O(4) O(2) O(6) 174.5(2) . . ? O(2) O(2) O(6) 61.58(10) 7 . ? O(1) O(2) O(6) 55.5(2) 2_554 . ? K O(2) O(6) 61.60(12) . . ? V(1) O(2) O(3) 127.5(2) 2_554 . ? Sb O(2) O(3) 87.4(2) . . ? O(2) O(2) O(3) 67.29(9) 7_565 . ? O(3) O(2) O(3) 159.4(2) 2_554 . ? O(1) O(2) O(3) 49.8(2) . . ? O(5) O(2) O(3) 105.9(2) . . ? O(4) O(2) O(3) 125.8(2) . . ? O(2) O(2) O(3) 112.71(9) 7 . ? O(1) O(2) O(3) 101.6(2) 2_554 . ? K O(2) O(3) 49.08(13) . . ? O(6) O(2) O(3) 57.07(12) . . ? V(1) O(3) O(2) 38.01(14) . 8_666 ? V(1) O(3) O(2) 38.01(14) . 2 ? O(2) O(3) O(2) 64.2(2) 8_666 2 ? V(1) O(3) O(1) 37.8(2) . . ? O(2) O(3) O(1) 64.4(2) 8_666 . ? O(2) O(3) O(1) 64.4(2) 2 . ? V(1) O(3) K 137.6(4) . . ? O(2) O(3) K 142.3(2) 8_666 . ? O(2) O(3) K 142.3(2) 2 . ? O(1) O(3) K 99.8(3) . . ? V(1) O(3) O(4) 113.0(3) . 6_657 ? O(2) O(3) O(4) 91.3(2) 8_666 6_657 ? O(2) O(3) O(4) 91.3(2) 2 6_657 ? O(1) O(3) O(4) 150.8(3) . 6_657 ? K O(3) O(4) 109.4(2) . 6_657 ? V(1) O(3) O(5) 149.1(2) . 4_556 ? O(2) O(3) O(5) 111.1(2) 8_666 4_556 ? O(2) O(3) O(5) 146.2(3) 2 4_556 ? O(1) O(3) O(5) 146.8(2) . 4_556 ? K O(3) O(5) 62.7(2) . 4_556 ? O(4) O(3) O(5) 54.9(2) 6_657 4_556 ? V(1) O(3) O(5) 149.1(2) . 6_657 ? O(2) O(3) O(5) 146.2(3) 8_666 6_657 ? O(2) O(3) O(5) 111.1(2) 2 6_657 ? O(1) O(3) O(5) 146.8(2) . 6_657 ? K O(3) O(5) 62.7(2) . 6_657 ? O(4) O(3) O(5) 54.9(2) 6_657 6_657 ? O(5) O(3) O(5) 52.7(2) 4_556 6_657 ? V(1) O(3) O(6) 110.8(2) . . ? O(2) O(3) O(6) 147.4(2) 8_666 . ? O(2) O(3) O(6) 84.2(2) 2 . ? O(1) O(3) O(6) 95.9(2) . . ? K O(3) O(6) 62.7(2) . . ? O(4) O(3) O(6) 97.3(2) 6_657 . ? O(5) O(3) O(6) 99.5(2) 4_556 . ? O(5) O(3) O(6) 51.40(15) 6_657 . ? V(1) O(3) O(6) 110.8(2) . 1_565 ? O(2) O(3) O(6) 84.2(2) 8_666 1_565 ? O(2) O(3) O(6) 147.4(2) 2 1_565 ? O(1) O(3) O(6) 95.9(2) . 1_565 ? K O(3) O(6) 62.7(2) . 1_565 ? O(4) O(3) O(6) 97.3(2) 6_657 1_565 ? O(5) O(3) O(6) 51.40(15) 4_556 1_565 ? O(5) O(3) O(6) 99.5(2) 6_657 1_565 ? O(6) O(3) O(6) 125.4(3) . 1_565 ? V(1) O(3) O(4) 94.4(2) . 2_565 ? O(2) O(3) O(4) 56.4(2) 8_666 2_565 ? O(2) O(3) O(4) 110.7(3) 2 2_565 ? O(1) O(3) O(4) 112.1(2) . 2_565 ? K O(3) O(4) 106.9(2) . 2_565 ? O(4) O(3) O(4) 59.74(14) 6_657 2_565 ? O(5) O(3) O(4) 54.64(15) 4_556 2_565 ? O(5) O(3) O(4) 100.3(2) 6_657 2_565 ? O(6) O(3) O(4) 151.7(3) . 2_565 ? O(6) O(3) O(4) 50.43(15) 1_565 2_565 ? V(1) O(3) O(4) 94.4(2) . 2 ? O(2) O(3) O(4) 110.7(2) 8_666 2 ? O(2) O(3) O(4) 56.4(2) 2 2 ? O(1) O(3) O(4) 112.1(2) . 2 ? K O(3) O(4) 106.9(2) . 2 ? O(4) O(3) O(4) 59.74(14) 6_657 2 ? O(5) O(3) O(4) 100.3(2) 4_556 2 ? O(5) O(3) O(4) 54.64(15) 6_657 2 ? O(6) O(3) O(4) 50.43(15) . 2 ? O(6) O(3) O(4) 151.7(3) 1_565 2 ? O(4) O(3) O(4) 117.3(3) 2_565 2 ? V(2) O(4) Sb 156.8(4) . . ? V(2) O(4) O(6) 33.0(2) . 2_554 ? Sb O(4) O(6) 123.7(3) . 2_554 ? V(2) O(4) O(5) 148.0(2) . 7_565 ? Sb O(4) O(5) 45.19(14) . 7_565 ? O(6) O(4) O(5) 144.5(2) 2_554 7_565 ? V(2) O(4) O(5) 148.0(2) . . ? Sb O(4) O(5) 45.19(14) . . ? O(6) O(4) O(5) 144.5(2) 2_554 . ? O(5) O(4) O(5) 59.3(2) 7_565 . ? V(2) O(4) O(2) 118.1(3) . 7_565 ? Sb O(4) O(2) 43.30(13) . 7_565 ? O(6) O(4) O(2) 89.3(2) 2_554 7_565 ? O(5) O(4) O(2) 60.6(2) 7_565 7_565 ? O(5) O(4) O(2) 88.5(2) . 7_565 ? V(2) O(4) O(2) 118.1(3) . . ? Sb O(4) O(2) 43.30(13) . . ? O(6) O(4) O(2) 89.3(2) 2_554 . ? O(5) O(4) O(2) 88.5(2) 7_565 . ? O(5) O(4) O(2) 60.6(2) . . ? O(2) O(4) O(2) 55.9(2) 7_565 . ? V(2) O(4) O(3) 105.5(3) . 6_557 ? Sb O(4) O(3) 97.8(3) . 6_557 ? O(6) O(4) O(3) 138.5(3) 2_554 6_557 ? O(5) O(4) O(3) 65.9(2) 7_565 6_557 ? O(5) O(4) O(3) 65.9(2) . 6_557 ? O(2) O(4) O(3) 126.5(2) 7_565 6_557 ? O(2) O(4) O(3) 126.5(2) . 6_557 ? V(2) O(4) O(5) 33.85(12) . 5_556 ? Sb O(4) O(5) 150.85(11) . 5_556 ? O(6) O(4) O(5) 57.1(2) 2_554 5_556 ? O(5) O(4) O(5) 152.9(2) 7_565 5_556 ? O(5) O(4) O(5) 114.41(13) . 5_556 ? O(2) O(4) O(5) 145.7(3) 7_565 5_556 ? O(2) O(4) O(5) 112.0(2) . 5_556 ? O(3) O(4) O(5) 87.3(2) 6_557 5_556 ? V(2) O(4) O(5) 33.85(12) . 3_556 ? Sb O(4) O(5) 150.85(11) . 3_556 ? O(6) O(4) O(5) 57.1(2) 2_554 3_556 ? O(5) O(4) O(5) 114.41(13) 7_565 3_556 ? O(5) O(4) O(5) 152.9(2) . 3_556 ? O(2) O(4) O(5) 112.0(2) 7_565 3_556 ? O(2) O(4) O(5) 145.7(3) . 3_556 ? O(3) O(4) O(5) 87.3(2) 6_557 3_556 ? O(5) O(4) O(5) 57.6(2) 5_556 3_556 ? V(2) O(4) O(4) 88.7(2) . 5_556 ? Sb O(4) O(4) 101.1(2) . 5_556 ? O(6) O(4) O(4) 102.6(2) 2_554 5_556 ? O(5) O(4) O(4) 112.5(3) 7_565 5_556 ? O(5) O(4) O(4) 59.4(2) . 5_556 ? O(2) O(4) O(4) 139.2(3) 7_565 5_556 ? O(2) O(4) O(4) 85.0(2) . 5_556 ? O(3) O(4) O(4) 65.6(2) 6_557 5_556 ? O(5) O(4) O(4) 55.0(2) 5_556 5_556 ? O(5) O(4) O(4) 107.1(3) 3_556 5_556 ? V(2) O(4) O(4) 88.7(2) . 5_566 ? Sb O(4) O(4) 101.1(2) . 5_566 ? O(6) O(4) O(4) 102.6(2) 2_554 5_566 ? O(5) O(4) O(4) 59.4(2) 7_565 5_566 ? O(5) O(4) O(4) 112.5(3) . 5_566 ? O(2) O(4) O(4) 85.0(2) 7_565 5_566 ? O(2) O(4) O(4) 139.2(3) . 5_566 ? O(3) O(4) O(4) 65.6(2) 6_557 5_566 ? O(5) O(4) O(4) 107.1(3) 5_556 5_566 ? O(5) O(4) O(4) 55.0(2) 3_556 5_566 ? O(4) O(4) O(4) 128.5(4) 5_556 5_566 ? V(2) O(5) Sb 138.2(2) 5_556 . ? V(2) O(5) O(6) 34.41(13) 5_556 6_557 ? Sb O(5) O(6) 155.9(2) . 6_557 ? V(2) O(5) O(1) 157.6(2) 5_556 . ? Sb O(5) O(1) 46.35(15) . . ? O(6) O(5) O(1) 153.5(3) 6_557 . ? V(2) O(5) O(5) 142.37(14) 5_556 7_565 ? Sb O(5) O(5) 45.78(12) . 7_565 ? O(6) O(5) O(5) 121.40(11) 6_557 7_565 ? O(1) O(5) O(5) 59.45(11) . 7_565 ? V(2) O(5) O(4) 97.9(2) 5_556 . ? Sb O(5) O(4) 45.29(14) . . ? O(6) O(5) O(4) 112.0(2) 6_557 . ? O(1) O(5) O(4) 91.6(2) . . ? O(5) O(5) O(4) 60.34(11) 7_565 . ? V(2) O(5) O(5) 37.63(14) 5_556 7 ? Sb O(5) O(5) 134.22(12) . 7 ? O(6) O(5) O(5) 58.60(11) 6_557 7 ? O(1) O(5) O(5) 120.55(11) . 7 ? O(5) O(5) O(5) 180.0(5) 7_565 7 ? O(4) O(5) O(5) 119.66(11) . 7 ? V(2) O(5) O(2) 107.2(2) 5_556 . ? Sb O(5) O(2) 43.59(12) . . ? O(6) O(5) O(2) 141.7(2) 6_557 . ? O(1) O(5) O(2) 60.2(2) . . ? O(5) O(5) O(2) 89.34(12) 7_565 . ? O(4) O(5) O(2) 61.1(2) . . ? O(5) O(5) O(2) 90.66(12) 7 . ? V(2) O(5) O(4) 32.43(12) 5_556 5_556 ? Sb O(5) O(4) 107.0(2) . 5_556 ? O(6) O(5) O(4) 57.8(2) 6_557 5_556 ? O(1) O(5) O(4) 148.0(2) . 5_556 ? O(5) O(5) O(4) 118.81(10) 7_565 5_556 ? O(4) O(5) O(4) 65.59(13) . 5_556 ? O(5) O(5) O(4) 61.19(10) 7 5_556 ? O(2) O(5) O(4) 88.5(2) . 5_556 ? V(2) O(5) K 95.3(2) 5_556 2 ? Sb O(5) K 112.0(2) . 2 ? O(6) O(5) K 92.1(2) 6_557 2 ? O(1) O(5) K 68.52(13) . 2 ? O(5) O(5) K 118.10(8) 7_565 2 ? O(4) O(5) K 152.9(2) . 2 ? O(5) O(5) K 61.90(8) 7 2 ? O(2) O(5) K 92.36(15) . 2 ? O(4) O(5) K 123.1(2) 5_556 2 ? V(2) O(5) K 97.7(2) 5_556 6_557 ? Sb O(5) K 108.9(2) . 6_557 ? O(6) O(5) K 64.12(12) 6_557 6_557 ? O(1) O(5) K 99.5(2) . 6_557 ? O(5) O(5) K 63.14(8) 7_565 6_557 ? O(4) O(5) K 104.1(2) . 6_557 ? O(5) O(5) K 116.86(8) 7 6_557 ? O(2) O(5) K 152.2(2) . 6_557 ? O(4) O(5) K 107.4(2) 5_556 6_557 ? K O(5) K 97.38(12) 2 6_557 ? V(2) O(5) O(3) 78.91(15) 5_556 6_557 ? Sb O(5) O(3) 92.2(2) . 6_557 ? O(6) O(5) O(3) 64.92(14) 6_557 6_557 ? O(1) O(5) O(3) 123.1(2) . 6_557 ? O(5) O(5) O(3) 63.66(9) 7_565 6_557 ? O(4) O(5) O(3) 59.2(2) . 6_557 ? O(5) O(5) O(3) 116.34(9) 7 6_557 ? O(2) O(5) O(3) 120.3(2) . 6_557 ? O(4) O(5) O(3) 65.47(15) 5_556 6_557 ? K O(5) O(3) 147.2(2) 2 6_557 ? K O(5) O(3) 52.41(14) 6_557 6_557 ? V(2) O(6) O(5) 39.11(14) 2 6_657 ? V(2) O(6) O(5) 39.11(14) 2 4_546 ? O(5) O(6) O(5) 62.8(2) 6_657 4_546 ? V(2) O(6) O(4) 35.9(2) 2 2 ? O(5) O(6) O(4) 65.1(2) 6_657 2 ? O(5) O(6) O(4) 65.1(2) 4_546 2 ? V(2) O(6) O(1) 138.2(4) 2 2_554 ? O(5) O(6) O(1) 110.0(2) 6_657 2_554 ? O(5) O(6) O(1) 110.0(2) 4_546 2_554 ? O(4) O(6) O(1) 174.1(3) 2 2_554 ? V(2) O(6) V(1) 173.6(4) 2 2_554 ? O(5) O(6) V(1) 137.0(2) 6_657 2_554 ? O(5) O(6) V(1) 137.0(2) 4_546 2_554 ? O(4) O(6) V(1) 150.5(3) 2 2_554 ? O(1) O(6) V(1) 35.40(14) 2_554 2_554 ? V(2) O(6) O(2) 148.9(2) 2 7 ? O(5) O(6) O(2) 169.7(3) 6_657 7 ? O(5) O(6) O(2) 119.21(13) 4_546 7 ? O(4) O(6) O(2) 125.1(2) 2 7 ? O(1) O(6) O(2) 59.7(2) 2_554 7 ? V(1) O(6) O(2) 34.07(10) 2_554 7 ? V(2) O(6) O(2) 148.9(2) 2 . ? O(5) O(6) O(2) 119.21(13) 6_657 . ? O(5) O(6) O(2) 169.7(3) 4_546 . ? O(4) O(6) O(2) 125.1(2) 2 . ? O(1) O(6) O(2) 59.7(2) 2_554 . ? V(1) O(6) O(2) 34.07(10) 2_554 . ? O(2) O(6) O(2) 56.8(2) 7 . ? V(2) O(6) K 101.5(2) 2 1_545 ? O(5) O(6) K 119.9(2) 6_657 1_545 ? O(5) O(6) K 63.35(12) 4_546 1_545 ? O(4) O(6) K 112.17(12) 2 1_545 ? O(1) O(6) K 66.80(12) 2_554 1_545 ? V(1) O(6) K 76.13(13) 2_554 1_545 ? O(2) O(6) K 58.02(12) 7 1_545 ? O(2) O(6) K 109.6(2) . 1_545 ? V(2) O(6) K 101.5(2) 2 . ? O(5) O(6) K 63.35(12) 6_657 . ? O(5) O(6) K 119.9(2) 4_546 . ? O(4) O(6) K 112.17(12) 2 . ? O(1) O(6) K 66.80(12) 2_554 . ? V(1) O(6) K 76.13(13) 2_554 . ? O(2) O(6) K 109.6(2) 7 . ? O(2) O(6) K 58.02(12) . . ? K O(6) K 130.6(2) 1_545 . ? V(2) O(6) O(3) 80.2(2) 2 . ? O(5) O(6) O(3) 63.7(2) 6_657 . ? O(5) O(6) O(3) 118.8(2) 4_546 . ? O(4) O(6) O(3) 67.2(2) 2 . ? O(1) O(6) O(3) 114.2(2) 2_554 . ? V(1) O(6) O(3) 102.5(2) 2_554 . ? O(2) O(6) O(3) 118.9(2) 7 . ? O(2) O(6) O(3) 68.7(2) . . ? K O(6) O(3) 176.0(3) 1_545 . ? K O(6) O(3) 51.93(12) . . ? V(2) O(6) O(3) 80.2(2) 2 1_545 ? O(5) O(6) O(3) 118.8(2) 6_657 1_545 ? O(5) O(6) O(3) 63.7(2) 4_546 1_545 ? O(4) O(6) O(3) 67.2(2) 2 1_545 ? O(1) O(6) O(3) 114.2(2) 2_554 1_545 ? V(1) O(6) O(3) 102.5(2) 2_554 1_545 ? O(2) O(6) O(3) 68.7(2) 7 1_545 ? O(2) O(6) O(3) 118.9(2) . 1_545 ? K O(6) O(3) 51.93(12) 1_545 1_545 ? K O(6) O(3) 176.0(3) . 1_545 ? O(3) O(6) O(3) 125.4(3) . 1_545 ? _refine_diff_density_max 1.042 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.208 #=END data_rbsbv _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'O8 Rb Sb V2' _chemical_formula_weight 437.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rb' 'Rb' -1.0440 2.9730 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.2670 0.5300 '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' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.722(2) _cell_length_b 5.5679(8) _cell_length_c 8.6697(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 710.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'rectangular block shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.085 _exptl_crystal_density_method ? _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 12.918 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5 _exptl_absorpt_correction_T_max 0.82 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 2 _diffrn_reflns_number 700 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 24.96 _reflns_number_total 700 _reflns_number_observed 637 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD4 programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.6484P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0106(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 700 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_obs 0.0272 _refine_ls_wR_factor_all 0.0779 _refine_ls_wR_factor_obs 0.0750 _refine_ls_goodness_of_fit_all 1.163 _refine_ls_goodness_of_fit_obs 1.181 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.181 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rb Rb 0.38578(5) 0.2500 0.54738(11) 0.0175(3) Uani 1 d S . Sb Sb 0.12178(3) 0.2500 0.68170(6) 0.0055(2) Uani 1 d S . V(1) V 0.28317(8) 0.2500 0.9904(2) 0.0070(3) Uani 1 d S . V(2) V 0.02460(8) 0.2500 0.2970(2) 0.0059(3) Uani 1 d S . O(1) O 0.1813(4) 0.2500 0.8834(6) 0.0110(12) Uani 1 d S . O(2) O 0.2078(2) 0.0097(7) 0.6057(4) 0.0122(8) Uani 1 d . . O(3) O 0.3663(4) 0.2500 0.8743(8) 0.0180(14) Uani 1 d S . O(4) O 0.0519(4) 0.2500 0.4887(7) 0.0104(12) Uani 1 d S . O(5) O 0.0396(2) 0.0030(7) 0.7634(5) 0.0101(8) Uani 1 d . . O(6) O 0.3862(4) -0.2500 0.6924(8) 0.0160(14) Uani 1 d S . 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 Rb 0.0145(5) 0.0186(5) 0.0195(5) 0.000 0.0023(3) 0.000 Sb 0.0033(3) 0.0044(3) 0.0089(4) 0.000 -0.0005(2) 0.000 V(1) 0.0042(6) 0.0056(6) 0.0113(7) 0.000 -0.0027(5) 0.000 V(2) 0.0030(6) 0.0053(6) 0.0095(7) 0.000 -0.0013(5) 0.000 O(1) 0.010(3) 0.016(3) 0.007(3) 0.000 -0.001(2) 0.000 O(2) 0.009(2) 0.010(2) 0.018(2) -0.002(2) 0.003(2) 0.001(2) O(3) 0.011(3) 0.024(3) 0.018(3) 0.000 0.002(2) 0.000 O(4) 0.012(3) 0.011(3) 0.008(3) 0.000 -0.006(2) 0.000 O(5) 0.011(2) 0.008(2) 0.011(2) 0.002(2) -0.0016(14) -0.002(2) O(6) 0.011(3) 0.016(3) 0.021(4) 0.000 -0.004(2) 0.000 _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 Rb O(3) 2.849(7) . ? Rb O(2) 2.985(4) . ? Rb O(2) 2.985(4) 7_565 ? Rb O(5) 3.042(4) 8_665 ? Rb O(5) 3.042(4) 2_554 ? Rb O(6) 3.055(3) 1_565 ? Rb O(6) 3.055(3) . ? Rb O(5) 3.116(4) 4_556 ? Rb O(5) 3.116(4) 6_657 ? Rb O(1) 3.278(3) 2_554 ? Rb O(1) 3.278(3) 2_564 ? Rb V(2) 3.618(2) 6_656 ? Sb O(2) 1.957(4) . ? Sb O(2) 1.957(4) 7_565 ? Sb O(1) 1.956(5) . ? Sb O(4) 1.964(6) . ? Sb O(5) 1.964(4) 7_565 ? Sb O(5) 1.964(4) . ? V(1) O(3) 1.585(6) . ? V(1) O(1) 1.764(5) . ? V(1) O(2) 1.763(4) 8_666 ? V(1) O(2) 1.763(4) 2 ? V(1) O(6) 3.047(6) 2 ? V(1) Rb 3.7657(11) 2 ? V(1) Rb 3.7657(11) 2_565 ? V(2) O(6) 1.596(6) 2_554 ? V(2) O(4) 1.710(6) . ? V(2) O(5) 1.775(4) 5_556 ? V(2) O(5) 1.775(4) 3_556 ? V(2) Rb 3.618(2) 6_556 ? V(2) Rb 3.7649(11) 2_554 ? V(2) Rb 3.7649(11) 2_564 ? O(1) O(5) 2.706(6) . ? O(1) O(5) 2.706(6) 7_565 ? O(1) O(3) 2.726(8) . ? O(1) O(2) 2.782(6) . ? O(1) O(2) 2.782(6) 7_565 ? O(1) O(6) 2.857(8) 2 ? O(1) O(2) 2.910(6) 8_666 ? O(1) O(2) 2.910(6) 2 ? O(1) Rb 3.278(3) 2_565 ? O(1) Rb 3.278(3) 2 ? O(2) V(1) 1.763(4) 2_554 ? O(2) O(2) 2.676(7) 7_565 ? O(2) O(3) 2.703(6) 2_554 ? O(2) O(5) 2.829(6) . ? O(2) O(4) 2.844(6) . ? O(2) O(2) 2.891(7) 7 ? O(2) O(1) 2.910(6) 2_554 ? O(2) O(6) 3.090(6) . ? O(3) O(2) 2.703(6) 8_666 ? O(3) O(2) 2.703(6) 2 ? O(3) O(4) 2.979(8) 6_657 ? O(3) O(5) 3.134(7) 4_556 ? O(3) O(5) 3.134(7) 6_657 ? O(3) O(4) 3.191(4) 2_565 ? O(3) O(4) 3.191(4) 2 ? O(3) O(6) 3.213(5) . ? O(3) O(6) 3.213(5) 1_565 ? O(4) O(6) 2.725(9) 2_554 ? O(4) O(5) 2.756(7) 7_565 ? O(4) O(5) 2.756(6) . ? O(4) O(2) 2.844(6) 7_565 ? O(4) O(5) 2.928(6) 5_556 ? O(4) O(5) 2.928(6) 3_556 ? O(4) O(3) 2.979(8) 6_557 ? O(4) O(4) 3.182(5) 5_556 ? O(4) O(4) 3.182(5) 5_566 ? O(5) V(2) 1.775(4) 5_556 ? O(5) O(6) 2.690(6) 6_557 ? O(5) O(5) 2.750(8) 7_565 ? O(5) O(5) 2.818(8) 7 ? O(5) O(4) 2.928(6) 5_556 ? O(5) Rb 3.042(4) 2 ? O(5) Rb 3.116(4) 6_557 ? O(5) O(3) 3.134(7) 6_557 ? O(6) V(2) 1.596(6) 2 ? O(6) O(5) 2.690(6) 6_657 ? O(6) O(5) 2.690(6) 4_546 ? O(6) O(4) 2.725(9) 2 ? O(6) O(1) 2.857(8) 2_554 ? O(6) V(1) 3.047(6) 2_554 ? O(6) Rb 3.055(3) 1_545 ? O(6) O(2) 3.090(6) 7 ? O(6) O(3) 3.213(5) 1_545 ? 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 O(3) Rb O(2) 75.13(13) . . ? O(3) Rb O(2) 75.13(13) . 7_565 ? O(2) Rb O(2) 53.27(14) . 7_565 ? O(3) Rb O(5) 147.30(10) . 8_665 ? O(2) Rb O(5) 131.43(11) . 8_665 ? O(2) Rb O(5) 104.27(10) 7_565 8_665 ? O(3) Rb O(5) 147.30(10) . 2_554 ? O(2) Rb O(5) 104.27(10) . 2_554 ? O(2) Rb O(5) 131.43(11) 7_565 2_554 ? O(5) Rb O(5) 55.18(15) 8_665 2_554 ? O(3) Rb O(6) 65.83(12) . 1_565 ? O(2) Rb O(6) 109.90(13) . 1_565 ? O(2) Rb O(6) 61.53(13) 7_565 1_565 ? O(5) Rb O(6) 84.86(14) 8_665 1_565 ? O(5) Rb O(6) 138.99(14) 2_554 1_565 ? O(3) Rb O(6) 65.83(12) . . ? O(2) Rb O(6) 61.53(13) . . ? O(2) Rb O(6) 109.90(13) 7_565 . ? O(5) Rb O(6) 138.99(14) 8_665 . ? O(5) Rb O(6) 84.86(14) 2_554 . ? O(6) Rb O(6) 131.4(2) 1_565 . ? O(3) Rb O(5) 63.20(12) . 4_556 ? O(2) Rb O(5) 138.28(11) . 4_556 ? O(2) Rb O(5) 110.54(10) 7_565 4_556 ? O(5) Rb O(5) 87.67(11) 8_665 4_556 ? O(5) Rb O(5) 111.60(7) 2_554 4_556 ? O(6) Rb O(5) 51.67(12) 1_565 4_556 ? O(6) Rb O(5) 100.61(13) . 4_556 ? O(3) Rb O(5) 63.20(12) . 6_657 ? O(2) Rb O(5) 110.54(10) . 6_657 ? O(2) Rb O(5) 138.28(11) 7_565 6_657 ? O(5) Rb O(5) 111.60(7) 8_665 6_657 ? O(5) Rb O(5) 87.67(11) 2_554 6_657 ? O(6) Rb O(5) 100.61(13) 1_565 6_657 ? O(6) Rb O(5) 51.67(12) . 6_657 ? O(5) Rb O(5) 52.37(14) 4_556 6_657 ? O(3) Rb O(1) 113.65(10) . 2_554 ? O(2) Rb O(1) 55.14(12) . 2_554 ? O(2) Rb O(1) 100.95(12) 7_565 2_554 ? O(5) Rb O(1) 98.69(12) 8_665 2_554 ? O(5) Rb O(1) 50.54(12) 2_554 2_554 ? O(6) Rb O(1) 162.37(13) 1_565 2_554 ? O(6) Rb O(1) 53.49(14) . 2_554 ? O(5) Rb O(1) 145.27(11) 4_556 2_554 ? O(5) Rb O(1) 94.15(11) 6_657 2_554 ? O(3) Rb O(1) 113.65(10) . 2_564 ? O(2) Rb O(1) 100.95(12) . 2_564 ? O(2) Rb O(1) 55.14(12) 7_565 2_564 ? O(5) Rb O(1) 50.54(12) 8_665 2_564 ? O(5) Rb O(1) 98.69(12) 2_554 2_564 ? O(6) Rb O(1) 53.49(14) 1_565 2_564 ? O(6) Rb O(1) 162.37(13) . 2_564 ? O(5) Rb O(1) 94.15(11) 4_556 2_564 ? O(5) Rb O(1) 145.27(11) 6_657 2_564 ? O(1) Rb O(1) 116.3(2) 2_554 2_564 ? O(3) Rb V(2) 151.37(12) . 6_656 ? O(2) Rb V(2) 129.46(8) . 6_656 ? O(2) Rb V(2) 129.46(8) 7_565 6_656 ? O(5) Rb V(2) 29.32(7) 8_665 6_656 ? O(5) Rb V(2) 29.32(7) 2_554 6_656 ? O(6) Rb V(2) 109.80(12) 1_565 6_656 ? O(6) Rb V(2) 109.80(12) . 6_656 ? O(5) Rb V(2) 91.38(7) 4_556 6_656 ? O(5) Rb V(2) 91.38(7) 6_657 6_656 ? O(1) Rb V(2) 79.18(9) 2_554 6_656 ? O(1) Rb V(2) 79.18(9) 2_564 6_656 ? O(2) Sb O(2) 86.3(2) . 7_565 ? O(2) Sb O(1) 90.7(2) . . ? O(2) Sb O(1) 90.7(2) 7_565 . ? O(2) Sb O(4) 93.0(2) . . ? O(2) Sb O(4) 93.0(2) 7_565 . ? O(1) Sb O(4) 175.0(2) . . ? O(2) Sb O(5) 177.57(15) . 7_565 ? O(2) Sb O(5) 92.4(2) 7_565 7_565 ? O(1) Sb O(5) 87.3(2) . 7_565 ? O(4) Sb O(5) 89.1(2) . 7_565 ? O(2) Sb O(5) 92.4(2) . . ? O(2) Sb O(5) 177.57(15) 7_565 . ? O(1) Sb O(5) 87.3(2) . . ? O(4) Sb O(5) 89.1(2) . . ? O(5) Sb O(5) 88.9(2) 7_565 . ? O(2) Sb Rb 44.22(11) . . ? O(2) Sb Rb 44.22(11) 7_565 . ? O(1) Sb Rb 80.1(2) . . ? O(4) Sb Rb 104.9(2) . . ? O(5) Sb Rb 133.93(11) 7_565 . ? O(5) Sb Rb 133.93(11) . . ? O(3) V(1) O(1) 108.9(3) . . ? O(3) V(1) O(2) 107.6(2) . 8_666 ? O(1) V(1) O(2) 111.2(2) . 8_666 ? O(3) V(1) O(2) 107.6(2) . 2 ? O(1) V(1) O(2) 111.2(2) . 2 ? O(2) V(1) O(2) 110.2(3) 8_666 2 ? O(3) V(1) O(6) 175.7(3) . 2 ? O(1) V(1) O(6) 66.8(2) . 2 ? O(2) V(1) O(6) 74.67(14) 8_666 2 ? O(2) V(1) O(6) 74.67(14) 2 2 ? O(3) V(1) Rb 126.42(10) . 2 ? O(1) V(1) Rb 60.47(10) . 2 ? O(2) V(1) Rb 125.57(14) 8_666 2 ? O(2) V(1) Rb 50.88(12) 2 2 ? O(6) V(1) Rb 51.99(5) 2 2 ? O(3) V(1) Rb 126.42(10) . 2_565 ? O(1) V(1) Rb 60.47(10) . 2_565 ? O(2) V(1) Rb 50.88(12) 8_666 2_565 ? O(2) V(1) Rb 125.57(14) 2 2_565 ? O(6) V(1) Rb 51.99(5) 2 2_565 ? Rb V(1) Rb 95.34(4) 2 2_565 ? O(6) V(2) O(4) 111.0(3) 2_554 . ? O(6) V(2) O(5) 105.7(2) 2_554 5_556 ? O(4) V(2) O(5) 114.3(2) . 5_556 ? O(6) V(2) O(5) 105.7(2) 2_554 3_556 ? O(4) V(2) O(5) 114.3(2) . 3_556 ? O(5) V(2) O(5) 105.0(2) 5_556 3_556 ? O(6) V(2) Rb 89.8(2) 2_554 6_556 ? O(4) V(2) Rb 159.2(2) . 6_556 ? O(5) V(2) Rb 57.05(13) 5_556 6_556 ? O(5) V(2) Rb 57.05(13) 3_556 6_556 ? O(6) V(2) Rb 52.06(8) 2_554 2_554 ? O(4) V(2) Rb 118.44(10) . 2_554 ? O(5) V(2) Rb 55.27(12) 5_556 2_554 ? O(5) V(2) Rb 127.15(14) 3_556 2_554 ? Rb V(2) Rb 73.96(3) 6_556 2_554 ? O(6) V(2) Rb 52.06(8) 2_554 2_564 ? O(4) V(2) Rb 118.44(10) . 2_564 ? O(5) V(2) Rb 127.15(14) 5_556 2_564 ? O(5) V(2) Rb 55.27(13) 3_556 2_564 ? Rb V(2) Rb 73.96(3) 6_556 2_564 ? Rb V(2) Rb 95.37(4) 2_554 2_564 ? V(1) O(1) Sb 148.3(3) . . ? V(1) O(1) O(5) 149.07(11) . . ? Sb O(1) O(5) 46.45(13) . . ? V(1) O(1) O(5) 149.07(11) . 7_565 ? Sb O(1) O(5) 46.45(13) . 7_565 ? O(5) O(1) O(5) 61.1(2) . 7_565 ? V(1) O(1) O(3) 33.4(2) . . ? Sb O(1) O(3) 114.9(3) . . ? O(5) O(1) O(3) 139.4(2) . . ? O(5) O(1) O(3) 139.4(2) 7_565 . ? V(1) O(1) O(2) 109.6(2) . . ? Sb O(1) O(2) 44.69(13) . . ? O(5) O(1) O(2) 62.0(2) . . ? O(5) O(1) O(2) 91.1(2) 7_565 . ? O(3) O(1) O(2) 80.5(2) . . ? V(1) O(1) O(2) 109.6(2) . 7_565 ? Sb O(1) O(2) 44.69(13) . 7_565 ? O(5) O(1) O(2) 91.1(2) . 7_565 ? O(5) O(1) O(2) 62.0(2) 7_565 7_565 ? O(3) O(1) O(2) 80.5(2) . 7_565 ? O(2) O(1) O(2) 57.5(2) . 7_565 ? V(1) O(1) O(6) 78.6(2) . 2 ? Sb O(1) O(6) 133.1(3) . 2 ? O(5) O(1) O(6) 95.3(2) . 2 ? O(5) O(1) O(6) 95.3(2) 7_565 2 ? O(3) O(1) O(6) 112.0(3) . 2 ? O(2) O(1) O(6) 149.35(13) . 2 ? O(2) O(1) O(6) 149.35(13) 7_565 2 ? V(1) O(1) O(2) 34.37(10) . 8_666 ? Sb O(1) O(2) 147.49(14) . 8_666 ? O(5) O(1) O(2) 160.0(2) . 8_666 ? O(5) O(1) O(2) 115.77(13) 7_565 8_666 ? O(3) O(1) O(2) 57.2(2) . 8_666 ? O(2) O(1) O(2) 137.1(2) . 8_666 ? O(2) O(1) O(2) 104.79(11) 7_565 8_666 ? O(6) O(1) O(2) 64.8(2) 2 8_666 ? V(1) O(1) O(2) 34.37(10) . 2 ? Sb O(1) O(2) 147.49(14) . 2 ? O(5) O(1) O(2) 115.77(13) . 2 ? O(5) O(1) O(2) 160.0(2) 7_565 2 ? O(3) O(1) O(2) 57.2(2) . 2 ? O(2) O(1) O(2) 104.79(11) . 2 ? O(2) O(1) O(2) 137.1(2) 7_565 2 ? O(6) O(1) O(2) 64.8(2) 2 2 ? O(2) O(1) O(2) 59.6(2) 8_666 2 ? V(1) O(1) Rb 91.61(14) . 2_565 ? Sb O(1) Rb 104.65(12) . 2_565 ? O(5) O(1) Rb 111.5(2) . 2_565 ? O(5) O(1) Rb 60.21(10) 7_565 2_565 ? O(3) O(1) Rb 108.27(13) . 2_565 ? O(2) O(1) Rb 145.7(2) . 2_565 ? O(2) O(1) Rb 90.52(9) 7_565 2_565 ? O(6) O(1) Rb 59.26(9) 2 2_565 ? O(2) O(1) Rb 57.32(9) 8_666 2_565 ? O(2) O(1) Rb 107.7(2) 2 2_565 ? V(1) O(1) Rb 91.61(14) . 2 ? Sb O(1) Rb 104.65(12) . 2 ? O(5) O(1) Rb 60.21(10) . 2 ? O(5) O(1) Rb 111.5(2) 7_565 2 ? O(3) O(1) Rb 108.27(13) . 2 ? O(2) O(1) Rb 90.52(9) . 2 ? O(2) O(1) Rb 145.7(2) 7_565 2 ? O(6) O(1) Rb 59.26(9) 2 2 ? O(2) O(1) Rb 107.7(2) 8_666 2 ? O(2) O(1) Rb 57.32(10) 2 2 ? Rb O(1) Rb 116.3(2) 2_565 2 ? V(1) O(2) Sb 143.2(2) 2_554 . ? V(1) O(2) O(2) 145.10(13) 2_554 7_565 ? Sb O(2) O(2) 46.85(11) . 7_565 ? V(1) O(2) O(3) 33.99(12) 2_554 2_554 ? Sb O(2) O(3) 110.8(2) . 2_554 ? O(2) O(2) O(3) 122.34(11) 7_565 2_554 ? V(1) O(2) O(1) 153.6(2) 2_554 . ? Sb O(2) O(1) 44.66(12) . . ? O(2) O(2) O(1) 61.25(9) 7_565 . ? O(3) O(2) O(1) 147.4(2) 2_554 . ? V(1) O(2) O(5) 109.2(2) 2_554 . ? Sb O(2) O(5) 43.92(11) . . ? O(2) O(2) O(5) 90.75(11) 7_565 . ? O(3) O(2) O(5) 89.9(2) 2_554 . ? O(1) O(2) O(5) 57.67(15) . . ? V(1) O(2) O(4) 104.1(2) 2_554 . ? Sb O(2) O(4) 43.62(13) . . ? O(2) O(2) O(4) 61.93(9) 7_565 . ? O(3) O(2) O(4) 70.18(14) 2_554 . ? O(1) O(2) O(4) 88.2(2) . . ? O(5) O(2) O(4) 58.1(2) . . ? V(1) O(2) O(2) 34.90(13) 2_554 7 ? Sb O(2) O(2) 133.15(11) . 7 ? O(2) O(2) O(2) 180.0(4) 7_565 7 ? O(3) O(2) O(2) 57.66(11) 2_554 7 ? O(1) O(2) O(2) 118.75(10) . 7 ? O(5) O(2) O(2) 89.25(11) . 7 ? O(4) O(2) O(2) 118.07(9) . 7 ? V(1) O(2) O(1) 34.39(11) 2_554 2_554 ? Sb O(2) O(1) 157.8(2) . 2_554 ? O(2) O(2) O(1) 119.78(9) 7_565 2_554 ? O(3) O(2) O(1) 58.0(2) 2_554 2_554 ? O(1) O(2) O(1) 153.0(2) . 2_554 ? O(5) O(2) O(1) 143.6(2) . 2_554 ? O(4) O(2) O(1) 116.8(2) . 2_554 ? O(2) O(2) O(1) 60.22(9) 7 2_554 ? V(1) O(2) Rb 101.9(2) 2_554 . ? Sb O(2) Rb 108.57(15) . . ? O(2) O(2) Rb 63.37(7) 7_565 . ? O(3) O(2) Rb 117.9(2) 2_554 . ? O(1) O(2) Rb 93.11(15) . . ? O(5) O(2) Rb 148.9(2) . . ? O(4) O(2) Rb 115.91(14) . . ? O(2) O(2) Rb 116.63(7) 7 . ? O(1) O(2) Rb 67.54(11) 2_554 . ? V(1) O(2) O(6) 71.96(15) 2_554 . ? Sb O(2) O(6) 142.0(2) . . ? O(2) O(2) O(6) 117.89(8) 7_565 . ? O(3) O(2) O(6) 105.9(2) 2_554 . ? O(1) O(2) O(6) 97.7(2) . . ? O(5) O(2) O(6) 128.3(2) . . ? O(4) O(2) O(6) 173.0(2) . . ? O(2) O(2) O(6) 62.11(8) 7 . ? O(1) O(2) O(6) 56.8(2) 2_554 . ? Rb O(2) O(6) 60.34(10) . . ? V(1) O(3) O(2) 38.45(14) . 8_666 ? V(1) O(3) O(2) 38.45(14) . 2 ? O(2) O(3) O(2) 64.7(2) 8_666 2 ? V(1) O(3) O(1) 37.7(2) . . ? O(2) O(3) O(1) 64.8(2) 8_666 . ? O(2) O(3) O(1) 64.8(2) 2 . ? V(1) O(3) Rb 135.2(3) . . ? O(2) O(3) Rb 141.2(2) 8_666 . ? O(2) O(3) Rb 141.2(2) 2 . ? O(1) O(3) Rb 97.4(2) . . ? V(1) O(3) O(4) 117.1(3) . 6_657 ? O(2) O(3) O(4) 94.3(2) 8_666 6_657 ? O(2) O(3) O(4) 94.3(2) 2 6_657 ? O(1) O(3) O(4) 154.8(3) . 6_657 ? Rb O(3) O(4) 107.7(2) . 6_657 ? V(1) O(3) O(5) 150.5(2) . 4_556 ? O(2) O(3) O(5) 112.13(15) 8_666 4_556 ? O(2) O(3) O(5) 147.8(3) 2 4_556 ? O(1) O(3) O(5) 145.5(2) . 4_556 ? Rb O(3) O(5) 62.56(14) . 4_556 ? O(4) O(3) O(5) 53.53(15) 6_657 4_556 ? V(1) O(3) O(5) 150.5(2) . 6_657 ? O(2) O(3) O(5) 147.8(3) 8_666 6_657 ? O(2) O(3) O(5) 112.13(15) 2 6_657 ? O(1) O(3) O(5) 145.5(2) . 6_657 ? Rb O(3) O(5) 62.56(14) . 6_657 ? O(4) O(3) O(5) 53.53(15) 6_657 6_657 ? O(5) O(3) O(5) 52.1(2) 4_556 6_657 ? V(1) O(3) O(4) 95.4(2) . 2_565 ? O(2) O(3) O(4) 56.98(14) 8_666 2_565 ? O(2) O(3) O(4) 112.9(2) 2 2_565 ? O(1) O(3) O(4) 111.59(15) . 2_565 ? Rb O(3) O(4) 105.7(2) . 2_565 ? O(4) O(3) O(4) 61.98(12) 6_657 2_565 ? O(5) O(3) O(4) 55.15(13) 4_556 2_565 ? O(5) O(3) O(4) 101.2(2) 6_657 2_565 ? V(1) O(3) O(4) 95.4(2) . 2 ? O(2) O(3) O(4) 112.9(2) 8_666 2 ? O(2) O(3) O(4) 56.98(14) 2 2 ? O(1) O(3) O(4) 111.59(15) . 2 ? Rb O(3) O(4) 105.7(2) . 2 ? O(4) O(3) O(4) 61.98(12) 6_657 2 ? O(5) O(3) O(4) 101.2(2) 4_556 2 ? O(5) O(3) O(4) 55.15(13) 6_657 2 ? O(4) O(3) O(4) 121.5(3) 2_565 2 ? V(1) O(3) O(6) 112.4(2) . . ? O(2) O(3) O(6) 149.8(2) 8_666 . ? O(2) O(3) O(6) 86.41(14) 2 . ? O(1) O(3) O(6) 96.0(2) . . ? Rb O(3) O(6) 60.17(15) . . ? O(4) O(3) O(6) 96.5(2) 6_657 . ? O(5) O(3) O(6) 96.9(2) 4_556 . ? O(5) O(3) O(6) 50.13(13) 6_657 . ? O(4) O(3) O(6) 151.0(2) 2_565 . ? O(4) O(3) O(6) 50.37(15) 2 . ? V(1) O(3) O(6) 112.4(2) . 1_565 ? O(2) O(3) O(6) 86.41(14) 8_666 1_565 ? O(2) O(3) O(6) 149.8(2) 2 1_565 ? O(1) O(3) O(6) 96.0(2) . 1_565 ? Rb O(3) O(6) 60.17(15) . 1_565 ? O(4) O(3) O(6) 96.5(2) 6_657 1_565 ? O(5) O(3) O(6) 50.13(13) 4_556 1_565 ? O(5) O(3) O(6) 96.9(2) 6_657 1_565 ? O(4) O(3) O(6) 50.37(15) 2_565 1_565 ? O(4) O(3) O(6) 151.0(2) 2 1_565 ? O(6) O(3) O(6) 120.1(3) . 1_565 ? V(2) O(4) Sb 162.0(3) . . ? V(2) O(4) O(6) 33.1(2) . 2_554 ? Sb O(4) O(6) 128.9(3) . 2_554 ? V(2) O(4) O(5) 145.5(2) . 7_565 ? Sb O(4) O(5) 45.44(13) . 7_565 ? O(6) O(4) O(5) 146.76(14) 2_554 7_565 ? V(2) O(4) O(5) 145.5(2) . . ? Sb O(4) O(5) 45.44(13) . . ? O(6) O(4) O(5) 146.76(14) 2_554 . ? O(5) O(4) O(5) 59.9(2) 7_565 . ? V(2) O(4) O(2) 122.5(2) . 7_565 ? Sb O(4) O(2) 43.40(12) . 7_565 ? O(6) O(4) O(2) 93.8(2) 2_554 7_565 ? O(5) O(4) O(2) 60.66(15) 7_565 7_565 ? O(5) O(4) O(2) 88.8(2) . 7_565 ? V(2) O(4) O(2) 122.5(2) . . ? Sb O(4) O(2) 43.40(12) . . ? O(6) O(4) O(2) 93.8(2) 2_554 . ? O(5) O(4) O(2) 88.8(2) 7_565 . ? O(5) O(4) O(2) 60.66(15) . . ? O(2) O(4) O(2) 56.1(2) 7_565 . ? V(2) O(4) O(5) 33.54(11) . 5_556 ? Sb O(4) O(5) 151.24(9) . 5_556 ? O(6) O(4) O(5) 56.7(2) 2_554 5_556 ? O(5) O(4) O(5) 148.7(2) 7_565 5_556 ? O(5) O(4) O(5) 111.99(12) . 5_556 ? O(2) O(4) O(5) 149.8(2) 7_565 5_556 ? O(2) O(4) O(5) 114.27(14) . 5_556 ? V(2) O(4) O(5) 33.54(11) . 3_556 ? Sb O(4) O(5) 151.24(9) . 3_556 ? O(6) O(4) O(5) 56.7(2) 2_554 3_556 ? O(5) O(4) O(5) 111.99(12) 7_565 3_556 ? O(5) O(4) O(5) 148.7(2) . 3_556 ? O(2) O(4) O(5) 114.27(14) 7_565 3_556 ? O(2) O(4) O(5) 149.8(2) . 3_556 ? O(5) O(4) O(5) 57.5(2) 5_556 3_556 ? V(2) O(4) O(3) 99.9(3) . 6_557 ? Sb O(4) O(3) 98.1(2) . 6_557 ? O(6) O(4) O(3) 133.0(3) 2_554 6_557 ? O(5) O(4) O(3) 66.1(2) 7_565 6_557 ? O(5) O(4) O(3) 66.1(2) . 6_557 ? O(2) O(4) O(3) 126.7(2) 7_565 6_557 ? O(2) O(4) O(3) 126.7(2) . 6_557 ? O(5) O(4) O(3) 82.9(2) 5_556 6_557 ? O(5) O(4) O(3) 82.9(2) 3_556 6_557 ? V(2) O(4) O(4) 87.0(2) . 5_556 ? Sb O(4) O(4) 101.5(2) . 5_556 ? O(6) O(4) O(4) 102.6(2) 2_554 5_556 ? O(5) O(4) O(4) 110.6(3) 7_565 5_556 ? O(5) O(4) O(4) 58.6(2) . 5_556 ? O(2) O(4) O(4) 141.0(3) 7_565 5_556 ? O(2) O(4) O(4) 87.36(15) . 5_556 ? O(5) O(4) O(4) 53.4(2) 5_556 5_556 ? O(5) O(4) O(4) 104.2(3) 3_556 5_556 ? O(3) O(4) O(4) 62.3(2) 6_557 5_556 ? V(2) O(4) O(4) 87.0(2) . 5_566 ? Sb O(4) O(4) 101.5(2) . 5_566 ? O(6) O(4) O(4) 102.6(2) 2_554 5_566 ? O(5) O(4) O(4) 58.6(2) 7_565 5_566 ? O(5) O(4) O(4) 110.6(3) . 5_566 ? O(2) O(4) O(4) 87.36(15) 7_565 5_566 ? O(2) O(4) O(4) 141.0(3) . 5_566 ? O(5) O(4) O(4) 104.2(3) 5_556 5_566 ? O(5) O(4) O(4) 53.4(2) 3_556 5_566 ? O(3) O(4) O(4) 62.3(2) 6_557 5_566 ? O(4) O(4) O(4) 122.1(3) 5_556 5_566 ? V(2) O(5) Sb 141.0(2) 5_556 . ? V(2) O(5) O(6) 34.84(13) 5_556 6_557 ? Sb O(5) O(6) 159.3(2) . 6_557 ? V(2) O(5) O(1) 157.9(2) 5_556 . ? Sb O(5) O(1) 46.21(13) . . ? O(6) O(5) O(1) 149.2(2) 6_557 . ? V(2) O(5) O(5) 142.52(12) 5_556 7_565 ? Sb O(5) O(5) 45.56(11) . 7_565 ? O(6) O(5) O(5) 121.59(10) 6_557 7_565 ? O(1) O(5) O(5) 59.46(10) . 7_565 ? V(2) O(5) O(4) 100.2(2) 5_556 . ? Sb O(5) O(4) 45.45(13) . . ? O(6) O(5) O(4) 116.1(2) 6_557 . ? O(1) O(5) O(4) 91.6(2) . . ? O(5) O(5) O(4) 60.07(10) 7_565 . ? V(2) O(5) O(5) 37.48(12) 5_556 7 ? Sb O(5) O(5) 134.44(11) . 7 ? O(6) O(5) O(5) 58.41(10) 6_557 7 ? O(1) O(5) O(5) 120.54(10) . 7 ? O(5) O(5) O(5) 180.0(4) 7_565 7 ? O(4) O(5) O(5) 119.93(10) . 7 ? V(2) O(5) O(2) 109.5(2) 5_556 . ? Sb O(5) O(2) 43.72(11) . . ? O(6) O(5) O(2) 144.2(2) 6_557 . ? O(1) O(5) O(2) 60.3(2) . . ? O(5) O(5) O(2) 89.25(11) 7_565 . ? O(4) O(5) O(2) 61.2(2) . . ? O(5) O(5) O(2) 90.75(11) 7 . ? V(2) O(5) O(4) 32.15(11) 5_556 5_556 ? Sb O(5) O(4) 110.6(2) . 5_556 ? O(6) O(5) O(4) 57.9(2) 6_557 5_556 ? O(1) O(5) O(4) 152.4(2) . 5_556 ? O(5) O(5) O(4) 118.76(9) 7_565 5_556 ? O(4) O(5) O(4) 68.01(12) . 5_556 ? O(5) O(5) O(4) 61.24(9) 7 5_556 ? O(2) O(5) O(4) 92.8(2) . 5_556 ? V(2) O(5) Rb 93.6(2) 5_556 2 ? Sb O(5) Rb 113.18(14) . 2 ? O(6) O(5) Rb 86.9(2) 6_557 2 ? O(1) O(5) Rb 69.25(12) . 2 ? O(5) O(5) Rb 117.59(7) 7_565 2 ? O(4) O(5) Rb 155.1(2) . 2 ? O(5) O(5) Rb 62.41(7) 7 2 ? O(2) O(5) Rb 94.64(13) . 2 ? O(4) O(5) Rb 123.18(14) 5_556 2 ? V(2) O(5) Rb 96.81(14) 5_556 6_557 ? Sb O(5) Rb 109.2(2) . 6_557 ? O(6) O(5) Rb 62.99(12) 6_557 6_557 ? O(1) O(5) Rb 97.7(2) . 6_557 ? O(5) O(5) Rb 63.81(7) 7_565 6_557 ? O(4) O(5) Rb 106.42(15) . 6_557 ? O(5) O(5) Rb 116.19(7) 7 6_557 ? O(2) O(5) Rb 152.2(2) . 6_557 ? O(4) O(5) Rb 105.72(15) 5_556 6_557 ? Rb O(5) Rb 92.33(11) 2 6_557 ? V(2) O(5) O(3) 78.62(13) 5_556 6_557 ? Sb O(5) O(3) 93.3(2) . 6_557 ? O(6) O(5) O(3) 66.46(13) 6_557 6_557 ? O(1) O(5) O(3) 123.4(2) . 6_557 ? O(5) O(5) O(3) 63.97(9) 7_565 6_557 ? O(4) O(5) O(3) 60.4(2) . 6_557 ? O(5) O(5) O(3) 116.03(9) 7 6_557 ? O(2) O(5) O(3) 121.5(2) . 6_557 ? O(4) O(5) O(3) 63.41(13) 5_556 6_557 ? Rb O(5) O(3) 143.7(2) 2 6_557 ? Rb O(5) O(3) 54.24(13) 6_557 6_557 ? V(2) O(6) O(5) 39.45(13) 2 6_657 ? V(2) O(6) O(5) 39.45(13) 2 4_546 ? O(5) O(6) O(5) 63.2(2) 6_657 4_546 ? V(2) O(6) O(4) 35.9(2) 2 2 ? O(5) O(6) O(4) 65.5(2) 6_657 2 ? O(5) O(6) O(4) 65.5(2) 4_546 2 ? V(2) O(6) O(1) 144.9(4) 2 2_554 ? O(5) O(6) O(1) 115.2(2) 6_657 2_554 ? O(5) O(6) O(1) 115.2(2) 4_546 2_554 ? O(4) O(6) O(1) 179.2(3) 2 2_554 ? V(2) O(6) V(1) 179.5(4) 2 2_554 ? O(5) O(6) V(1) 140.3(2) 6_657 2_554 ? O(5) O(6) V(1) 140.3(2) 4_546 2_554 ? O(4) O(6) V(1) 144.6(3) 2 2_554 ? O(1) O(6) V(1) 34.57(13) 2_554 2_554 ? V(2) O(6) Rb 103.61(13) 2 1_545 ? O(5) O(6) Rb 122.5(2) 6_657 1_545 ? O(5) O(6) Rb 65.34(11) 4_546 1_545 ? O(4) O(6) Rb 112.87(12) 2 1_545 ? O(1) O(6) Rb 67.25(12) 2_554 1_545 ? V(1) O(6) Rb 76.22(12) 2_554 1_545 ? V(2) O(6) Rb 103.61(13) 2 . ? O(5) O(6) Rb 65.34(11) 6_657 . ? O(5) O(6) Rb 122.5(2) 4_546 . ? O(4) O(6) Rb 112.87(12) 2 . ? O(1) O(6) Rb 67.25(12) 2_554 . ? V(1) O(6) Rb 76.22(12) 2_554 . ? Rb O(6) Rb 131.4(2) 1_545 . ? V(2) O(6) O(2) 146.9(2) 2 7 ? O(5) O(6) O(2) 173.4(3) 6_657 7 ? O(5) O(6) O(2) 120.21(11) 4_546 7 ? O(4) O(6) O(2) 120.9(2) 2 7 ? O(1) O(6) O(2) 58.4(2) 2_554 7 ? V(1) O(6) O(2) 33.38(9) 2_554 7 ? Rb O(6) O(2) 58.13(10) 1_545 7 ? Rb O(6) O(2) 108.9(2) . 7 ? V(2) O(6) O(2) 146.9(2) 2 . ? O(5) O(6) O(2) 120.21(11) 6_657 . ? O(5) O(6) O(2) 173.4(3) 4_546 . ? O(4) O(6) O(2) 120.9(2) 2 . ? O(1) O(6) O(2) 58.4(2) 2_554 . ? V(1) O(6) O(2) 33.38(9) 2_554 . ? Rb O(6) O(2) 108.9(2) 1_545 . ? Rb O(6) O(2) 58.13(10) . . ? O(2) O(6) O(2) 55.8(2) 7 . ? V(2) O(6) O(3) 78.2(2) 2 . ? O(5) O(6) O(3) 63.41(15) 6_657 . ? O(5) O(6) O(3) 117.4(2) 4_546 . ? O(4) O(6) O(3) 64.4(2) 2 . ? O(1) O(6) O(3) 115.4(2) 2_554 . ? V(1) O(6) O(3) 102.0(2) 2_554 . ? Rb O(6) O(3) 172.6(2) 1_545 . ? Rb O(6) O(3) 54.00(10) . . ? O(2) O(6) O(3) 116.6(2) 7 . ? O(2) O(6) O(3) 68.71(15) . . ? V(2) O(6) O(3) 78.2(2) 2 1_545 ? O(5) O(6) O(3) 117.4(2) 6_657 1_545 ? O(5) O(6) O(3) 63.41(15) 4_546 1_545 ? O(4) O(6) O(3) 64.4(2) 2 1_545 ? O(1) O(6) O(3) 115.4(2) 2_554 1_545 ? V(1) O(6) O(3) 102.0(2) 2_554 1_545 ? Rb O(6) O(3) 54.00(10) 1_545 1_545 ? Rb O(6) O(3) 172.6(2) . 1_545 ? O(2) O(6) O(3) 68.71(15) 7 1_545 ? O(2) O(6) O(3) 116.6(2) . 1_545 ? O(3) O(6) O(3) 120.1(3) . 1_545 ? _refine_diff_density_max 1.053 _refine_diff_density_min -1.974 _refine_diff_density_rms 0.230 #=END data_tlsbv _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'O8 Sb Tl V2' _chemical_formula_weight 555.96 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Tl' 'Tl' -3.5560 9.6590 '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' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.569(5) _cell_length_b 8.670(4) _cell_length_c 14.630(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.14(4) _cell_angle_gamma 90.00 _cell_volume 706.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'rectangular blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.228 _exptl_crystal_density_method ? _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 28.215 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.82 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 3 _diffrn_reflns_number 1250 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1250 _reflns_number_observed 1143 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD4 programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.2367P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1250 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_obs 0.0222 _refine_ls_wR_factor_all 0.0580 _refine_ls_wR_factor_obs 0.0560 _refine_ls_goodness_of_fit_all 1.155 _refine_ls_goodness_of_fit_obs 1.172 _refine_ls_restrained_S_all 1.155 _refine_ls_restrained_S_obs 1.172 _refine_ls_shift/esd_max -4.896 _refine_ls_shift/esd_mean 0.049 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tl Tl 0.75001(4) 0.05657(3) 0.38587(2) 0.01599(13) Uani 1 d . . Sb Sb 0.74996(6) 0.18183(4) 0.12170(2) 0.00211(14) Uani 1 d . . V(1) V 0.7498(2) 0.00804(11) 0.78226(6) 0.0039(2) Uani 1 d . . V(2) V 0.2499(2) 0.20344(10) 0.97448(6) 0.0024(2) Uiso 1 d . . O(1) O 0.7503(7) 0.1145(5) 0.6813(2) 0.0080(8) Uani 1 d . . O(2) O 0.5089(7) 0.1067(5) 0.2089(3) 0.0083(8) Uani 1 d . . O(3) O 0.9904(7) 0.1067(5) 0.2094(3) 0.0091(8) Uani 1 d . . O(4) O 0.7507(8) 0.1254(5) 0.8665(3) 0.0142(9) Uani 1 d . . O(5) O 0.2497(7) 0.0122(5) 0.9482(3) 0.0069(8) Uani 1 d . . O(6) O 0.5036(7) 0.2388(5) 0.5386(3) 0.0077(8) Uani 1 d . . O(7) O 0.9954(7) 0.2383(5) 0.5383(3) 0.0078(8) Uani 1 d . . O(8) O 0.2494(7) 0.1925(6) 0.3840(3) 0.0132(10) Uani 1 d . . 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 Tl 0.0162(2) 0.0156(2) 0.0161(2) 0.00156(9) -0.00024(11) 0.00002(10) Sb 0.0006(2) 0.0033(2) 0.0024(2) -0.00062(12) -0.00022(15) 0.00009(12) V(1) 0.0018(4) 0.0060(5) 0.0039(4) 0.0017(3) -0.0004(3) 0.0001(4) O(1) 0.010(2) 0.008(2) 0.006(2) 0.003(2) -0.0012(15) -0.001(2) O(2) 0.005(2) 0.012(2) 0.007(2) 0.001(2) 0.0027(14) -0.003(2) O(3) 0.006(2) 0.012(2) 0.009(2) -0.001(2) -0.0024(15) 0.003(2) O(4) 0.016(2) 0.014(2) 0.012(2) -0.005(2) -0.002(2) 0.001(2) O(5) 0.004(2) 0.006(2) 0.010(2) -0.002(2) 0.000(2) -0.001(2) O(6) 0.003(2) 0.010(2) 0.010(2) 0.0004(15) -0.0048(15) 0.000(2) O(7) 0.006(2) 0.011(2) 0.006(2) 0.0021(15) 0.0025(15) 0.005(2) O(8) 0.013(2) 0.012(2) 0.014(2) 0.001(2) 0.001(2) 0.001(2) _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 Tl O(4) 2.772(5) 4_565 ? Tl O(3) 2.944(4) . ? Tl O(2) 2.946(4) . ? Tl O(8) 3.021(5) 1_655 ? Tl O(8) 3.027(4) . ? Tl O(7) 3.051(4) . ? Tl O(6) 3.064(4) . ? Tl O(7) 3.126(4) 3_756 ? Tl O(6) 3.127(4) 3_656 ? Tl O(1) 3.304(4) 3_656 ? Tl O(1) 3.305(4) 3_756 ? Tl V(2) 3.681(2) 2_646 ? Sb O(6) 1.956(4) 4_565 ? Sb O(7) 1.961(4) 4_565 ? Sb O(3) 1.963(4) . ? Sb O(2) 1.966(4) . ? Sb O(5) 1.969(4) 3_656 ? Sb O(1) 1.969(4) 4_565 ? Sb O(4) 3.765(4) 1_554 ? Sb O(4) 3.854(5) 3_756 ? Sb O(4) 3.860(5) 3_656 ? Sb O(4) 3.952(4) 4_565 ? Sb O(5) 4.042(4) 1_554 ? V(1) O(4) 1.598(4) . ? V(1) O(1) 1.741(4) . ? V(1) O(2) 1.756(4) 3_656 ? V(1) O(3) 1.760(4) 3_756 ? V(1) O(8) 2.990(4) 3_656 ? V(1) O(5) 3.689(5) 1_655 ? V(1) O(5) 3.699(5) . ? V(1) Tl 3.752(2) 3_656 ? V(1) O(3) 3.754(4) 4_566 ? V(1) O(2) 3.755(4) 4_566 ? V(1) Tl 3.763(2) 3_756 ? V(1) O(6) 3.785(4) 2_646 ? V(2) O(8) 1.602(4) 4_566 ? V(2) O(5) 1.702(4) . ? V(2) O(6) 1.767(4) 4_566 ? V(2) O(7) 1.773(4) 4_466 ? V(2) O(4) 3.265(5) 1_455 ? V(2) O(4) 3.279(5) . ? V(2) O(5) 3.539(4) 3_657 ? V(2) O(5) 3.540(4) 3_557 ? V(2) O(4) 3.680(5) 3_657 ? V(2) Tl 3.681(2) 2_656 ? V(2) Tl 3.707(2) 4_466 ? V(2) Tl 3.713(2) 4_566 ? O(1) Sb 1.969(4) 4_566 ? O(1) O(4) 2.711(5) . ? O(1) O(6) 2.719(5) . ? O(1) O(7) 2.722(5) . ? O(1) O(3) 2.792(6) 4_566 ? O(1) O(2) 2.795(6) 4_566 ? O(1) O(8) 2.829(7) 3_656 ? O(1) O(3) 2.883(6) 3_756 ? O(1) O(2) 2.890(5) 3_656 ? O(1) Tl 3.304(4) 3_656 ? O(1) Tl 3.305(4) 3_756 ? O(2) V(1) 1.756(4) 3_656 ? O(2) O(3) 2.682(5) . ? O(2) O(4) 2.711(6) 3_656 ? O(2) O(1) 2.795(6) 4_565 ? O(2) O(6) 2.829(5) 4_565 ? O(2) O(5) 2.858(6) 3_656 ? O(2) O(3) 2.887(6) 1_455 ? O(2) O(1) 2.890(5) 3_656 ? O(2) O(8) 3.036(5) . ? O(2) O(4) 3.537(6) 4_565 ? O(3) V(1) 1.760(4) 3_756 ? O(3) O(4) 2.715(6) 3_756 ? O(3) O(1) 2.792(6) 4_565 ? O(3) O(7) 2.841(5) 4_565 ? O(3) O(5) 2.855(6) 3_656 ? O(3) O(1) 2.883(6) 3_756 ? O(3) O(2) 2.887(6) 1_655 ? O(3) O(8) 3.024(5) 1_655 ? O(3) O(4) 3.532(6) 4_565 ? O(4) O(2) 2.711(6) 3_656 ? O(4) O(3) 2.715(6) 3_756 ? O(4) Tl 2.772(5) 4_566 ? O(4) O(5) 2.962(6) 3_657 ? O(4) O(7) 3.091(6) 4_566 ? O(4) O(6) 3.104(6) 4_566 ? O(4) O(5) 3.178(6) 1_655 ? O(4) O(5) 3.192(6) . ? O(4) O(8) 3.205(6) 4_666 ? O(4) O(8) 3.218(6) 4_566 ? O(5) Sb 1.969(4) 3_656 ? O(5) O(8) 2.727(6) 4_566 ? O(5) O(7) 2.746(5) 2_646 ? O(5) O(6) 2.746(6) 2_646 ? O(5) O(3) 2.855(6) 3_656 ? O(5) O(2) 2.858(6) 3_656 ? O(5) O(6) 2.899(6) 4_566 ? O(5) O(7) 2.904(6) 4_466 ? O(5) O(4) 2.962(6) 3_657 ? O(5) O(5) 3.177(8) 3_657 ? O(5) O(4) 3.178(6) 1_455 ? O(6) V(2) 1.767(4) 4_565 ? O(6) Sb 1.956(4) 4_566 ? O(6) O(8) 2.696(5) . ? O(6) O(7) 2.739(6) . ? O(6) O(5) 2.746(6) 2_656 ? O(6) O(2) 2.829(5) 4_566 ? O(6) O(7) 2.830(6) 1_455 ? O(6) O(5) 2.899(6) 4_565 ? O(6) O(4) 3.104(6) 4_565 ? O(6) Tl 3.127(4) 3_656 ? O(7) V(2) 1.773(4) 4_665 ? O(7) Sb 1.961(4) 4_566 ? O(7) O(8) 2.696(5) 1_655 ? O(7) O(5) 2.746(5) 2_656 ? O(7) O(6) 2.830(6) 1_655 ? O(7) O(3) 2.841(5) 4_566 ? O(7) O(5) 2.904(6) 4_665 ? O(7) O(4) 3.091(6) 4_565 ? O(7) Tl 3.126(4) 3_756 ? O(8) V(2) 1.602(4) 4_565 ? O(8) O(7) 2.696(5) 1_455 ? O(8) O(5) 2.727(6) 4_565 ? O(8) O(1) 2.829(7) 3_656 ? O(8) V(1) 2.990(4) 3_656 ? O(8) Tl 3.021(5) 1_455 ? O(8) O(3) 3.024(5) 1_455 ? O(8) O(4) 3.205(6) 4_465 ? O(8) O(4) 3.218(6) 4_565 ? 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 O(4) Tl O(3) 76.27(12) 4_565 . ? O(4) Tl O(2) 76.35(12) 4_565 . ? O(3) Tl O(2) 54.17(11) . . ? O(4) Tl O(8) 67.02(13) 4_565 1_655 ? O(3) Tl O(8) 60.91(11) . 1_655 ? O(2) Tl O(8) 110.62(11) . 1_655 ? O(4) Tl O(8) 67.24(13) 4_565 . ? O(3) Tl O(8) 110.82(11) . . ? O(2) Tl O(8) 61.09(10) . . ? O(8) Tl O(8) 134.1(2) 1_655 . ? O(4) Tl O(7) 63.91(11) 4_565 . ? O(3) Tl O(7) 111.16(11) . . ? O(2) Tl O(7) 140.22(11) . . ? O(8) Tl O(7) 52.72(10) 1_655 . ? O(8) Tl O(7) 102.50(11) . . ? O(4) Tl O(6) 64.05(11) 4_565 . ? O(3) Tl O(6) 140.27(11) . . ? O(2) Tl O(6) 111.16(11) . . ? O(8) Tl O(6) 102.67(11) 1_655 . ? O(8) Tl O(6) 52.54(10) . . ? O(7) Tl O(6) 53.21(10) . . ? O(4) Tl O(7) 148.13(12) 4_565 3_756 ? O(3) Tl O(7) 103.03(11) . 3_756 ? O(2) Tl O(7) 129.66(11) . 3_756 ? O(8) Tl O(7) 84.58(12) 1_655 3_756 ? O(8) Tl O(7) 137.62(11) . 3_756 ? O(7) Tl O(7) 87.76(11) . 3_756 ? O(6) Tl O(7) 111.48(10) . 3_756 ? O(4) Tl O(6) 148.36(12) 4_565 3_656 ? O(3) Tl O(6) 129.61(11) . 3_656 ? O(2) Tl O(6) 103.06(11) . 3_656 ? O(8) Tl O(6) 137.67(11) 1_655 3_656 ? O(8) Tl O(6) 84.56(12) . 3_656 ? O(7) Tl O(6) 111.51(10) . 3_656 ? O(6) Tl O(6) 87.77(11) . 3_656 ? O(7) Tl O(6) 53.83(11) 3_756 3_656 ? O(4) Tl O(1) 114.68(11) 4_565 3_656 ? O(3) Tl O(1) 100.97(11) . 3_656 ? O(2) Tl O(1) 54.72(10) . 3_656 ? O(8) Tl O(1) 161.48(9) 1_655 3_656 ? O(8) Tl O(1) 52.86(12) . 3_656 ? O(7) Tl O(1) 145.62(10) . 3_656 ? O(6) Tl O(1) 94.00(11) . 3_656 ? O(7) Tl O(1) 96.88(11) 3_756 3_656 ? O(6) Tl O(1) 49.92(9) 3_656 3_656 ? O(4) Tl O(1) 114.51(11) 4_565 3_756 ? O(3) Tl O(1) 54.58(10) . 3_756 ? O(2) Tl O(1) 100.79(10) . 3_756 ? O(8) Tl O(1) 52.88(12) 1_655 3_756 ? O(8) Tl O(1) 161.48(9) . 3_756 ? O(7) Tl O(1) 94.20(11) . 3_756 ? O(6) Tl O(1) 145.81(10) . 3_756 ? O(7) Tl O(1) 49.98(9) 3_756 3_756 ? O(6) Tl O(1) 96.83(11) 3_656 3_756 ? O(1) Tl O(1) 114.83(12) 3_656 3_756 ? O(4) Tl V(2) 152.15(9) 4_565 2_646 ? O(3) Tl V(2) 127.61(8) . 2_646 ? O(2) Tl V(2) 127.59(8) . 2_646 ? O(8) Tl V(2) 109.31(9) 1_655 2_646 ? O(8) Tl V(2) 109.13(9) . 2_646 ? O(7) Tl V(2) 91.40(8) . 2_646 ? O(6) Tl V(2) 91.34(8) . 2_646 ? O(7) Tl V(2) 28.74(7) 3_756 2_646 ? O(6) Tl V(2) 28.63(7) 3_656 2_646 ? O(1) Tl V(2) 77.91(7) 3_656 2_646 ? O(1) Tl V(2) 78.04(7) 3_756 2_646 ? O(6) Sb O(7) 88.7(2) 4_565 4_565 ? O(6) Sb O(3) 177.6(2) 4_565 . ? O(7) Sb O(3) 92.8(2) 4_565 . ? O(6) Sb O(2) 92.3(2) 4_565 . ? O(7) Sb O(2) 177.9(2) 4_565 . ? O(3) Sb O(2) 86.1(2) . . ? O(6) Sb O(5) 88.8(2) 4_565 3_656 ? O(7) Sb O(5) 88.7(2) 4_565 3_656 ? O(3) Sb O(5) 93.1(2) . 3_656 ? O(2) Sb O(5) 93.2(2) . 3_656 ? O(6) Sb O(1) 87.7(2) 4_565 4_565 ? O(7) Sb O(1) 87.7(2) 4_565 4_565 ? O(3) Sb O(1) 90.5(2) . 4_565 ? O(2) Sb O(1) 90.5(2) . 4_565 ? O(5) Sb O(1) 175.0(2) 3_656 4_565 ? O(6) Sb O(4) 55.39(13) 4_565 1_554 ? O(7) Sb O(4) 55.00(13) 4_565 1_554 ? O(3) Sb O(4) 127.04(13) . 1_554 ? O(2) Sb O(4) 127.09(13) . 1_554 ? O(5) Sb O(4) 51.24(14) 3_656 1_554 ? O(1) Sb O(4) 123.76(13) 4_565 1_554 ? O(6) Sb O(4) 140.90(13) 4_565 3_756 ? O(7) Sb O(4) 76.58(14) 4_565 3_756 ? O(3) Sb O(4) 41.46(13) . 3_756 ? O(2) Sb O(4) 103.65(14) . 3_756 ? O(5) Sb O(4) 55.33(13) 3_656 3_756 ? O(1) Sb O(4) 126.86(13) 4_565 3_756 ? O(4) Sb O(4) 87.25(10) 1_554 3_756 ? O(6) Sb O(4) 76.41(14) 4_565 3_656 ? O(7) Sb O(4) 140.91(13) 4_565 3_656 ? O(3) Sb O(4) 103.51(14) . 3_656 ? O(2) Sb O(4) 41.23(13) . 3_656 ? O(5) Sb O(4) 55.60(13) 3_656 3_656 ? O(1) Sb O(4) 126.78(13) 4_565 3_656 ? O(4) Sb O(4) 87.54(10) 1_554 3_656 ? O(4) Sb O(4) 92.42(11) 3_756 3_656 ? O(6) Sb O(4) 114.41(13) 4_565 4_565 ? O(7) Sb O(4) 114.55(13) 4_565 4_565 ? O(3) Sb O(4) 63.20(13) . 4_565 ? O(2) Sb O(4) 63.31(13) . 4_565 ? O(5) Sb O(4) 146.31(13) 3_656 4_565 ? O(1) Sb O(4) 38.69(13) 4_565 4_565 ? O(4) Sb O(4) 162.45(4) 1_554 4_565 ? O(4) Sb O(4) 104.63(7) 3_756 4_565 ? O(4) Sb O(4) 104.51(7) 3_656 4_565 ? O(6) Sb Tl 133.78(12) 4_565 . ? O(7) Sb Tl 134.12(12) 4_565 . ? O(3) Sb Tl 44.18(12) . . ? O(2) Sb Tl 44.26(12) . . ? O(5) Sb Tl 105.60(12) 3_656 . ? O(1) Sb Tl 79.40(11) 4_565 . ? O(4) Sb Tl 156.84(7) 1_554 . ? O(4) Sb Tl 76.80(7) 3_756 . ? O(4) Sb Tl 76.63(7) 3_656 . ? O(4) Sb Tl 40.71(7) 4_565 . ? O(6) Sb O(5) 41.96(13) 4_565 1_554 ? O(7) Sb O(5) 102.60(13) 4_565 1_554 ? O(3) Sb O(5) 139.26(13) . 1_554 ? O(2) Sb O(5) 79.42(13) . 1_554 ? O(5) Sb O(5) 50.5(2) 3_656 1_554 ? O(1) Sb O(5) 127.18(13) 4_565 1_554 ? O(4) Sb O(5) 48.11(9) 1_554 1_554 ? O(4) Sb O(5) 105.83(9) 3_756 1_554 ? O(4) Sb O(5) 43.95(9) 3_656 1_554 ? O(4) Sb O(5) 136.24(9) 4_565 1_554 ? Tl Sb O(5) 120.31(6) . 1_554 ? O(4) V(1) O(1) 108.4(2) . . ? O(4) V(1) O(2) 107.8(2) . 3_656 ? O(1) V(1) O(2) 111.4(2) . 3_656 ? O(4) V(1) O(3) 107.8(2) . 3_756 ? O(1) V(1) O(3) 110.8(2) . 3_756 ? O(2) V(1) O(3) 110.4(2) 3_656 3_756 ? O(4) V(1) O(8) 176.0(2) . 3_656 ? O(1) V(1) O(8) 67.6(2) . 3_656 ? O(2) V(1) O(8) 74.5(2) 3_656 3_656 ? O(3) V(1) O(8) 74.0(2) 3_756 3_656 ? O(4) V(1) O(5) 59.0(2) . 1_655 ? O(1) V(1) O(5) 123.4(2) . 1_655 ? O(2) V(1) O(5) 125.11(15) 3_656 1_655 ? O(3) V(1) O(5) 48.76(15) 3_756 1_655 ? O(8) V(1) O(5) 122.57(11) 3_656 1_655 ? O(4) V(1) O(5) 59.2(2) . . ? O(1) V(1) O(5) 123.6(2) . . ? O(2) V(1) O(5) 48.57(14) 3_656 . ? O(3) V(1) O(5) 125.44(15) 3_756 . ? O(8) V(1) O(5) 122.82(11) 3_656 . ? O(5) V(1) O(5) 97.83(11) 1_655 . ? O(4) V(1) Tl 127.0(2) . 3_656 ? O(1) V(1) Tl 61.70(14) . 3_656 ? O(2) V(1) Tl 49.91(13) 3_656 3_656 ? O(3) V(1) Tl 124.72(14) 3_756 3_656 ? O(8) V(1) Tl 51.86(8) 3_656 3_656 ? O(5) V(1) Tl 171.96(7) 1_655 3_656 ? O(5) V(1) Tl 82.71(8) . 3_656 ? O(4) V(1) O(3) 69.7(2) . 4_566 ? O(1) V(1) O(3) 44.45(14) . 4_566 ? O(2) V(1) O(3) 144.94(14) 3_656 4_566 ? O(3) V(1) O(3) 103.23(11) 3_756 4_566 ? O(8) V(1) O(3) 106.56(11) 3_656 4_566 ? O(5) V(1) O(3) 84.78(9) 1_655 4_566 ? O(5) V(1) O(3) 116.59(9) . 4_566 ? Tl V(1) O(3) 102.20(6) 3_656 4_566 ? O(4) V(1) O(2) 69.8(2) . 4_566 ? O(1) V(1) O(2) 44.56(15) . 4_566 ? O(2) V(1) O(2) 103.44(10) 3_656 4_566 ? O(3) V(1) O(2) 144.68(15) 3_756 4_566 ? O(8) V(1) O(2) 106.62(11) 3_656 4_566 ? O(5) V(1) O(2) 116.61(9) 1_655 4_566 ? O(5) V(1) O(2) 84.83(9) . 4_566 ? Tl V(1) O(2) 71.43(7) 3_656 4_566 ? O(3) V(1) O(2) 41.84(9) 4_566 4_566 ? O(4) V(1) Tl 126.7(2) . 3_756 ? O(1) V(1) Tl 61.45(14) . 3_756 ? O(2) V(1) Tl 124.92(14) 3_656 3_756 ? O(3) V(1) Tl 49.58(13) 3_756 3_756 ? O(8) V(1) Tl 51.62(8) 3_656 3_756 ? O(5) V(1) Tl 82.70(8) 1_655 3_756 ? O(5) V(1) Tl 171.98(7) . 3_756 ? Tl V(1) Tl 95.65(5) 3_656 3_756 ? O(3) V(1) Tl 71.42(7) 4_566 3_756 ? O(2) V(1) Tl 102.14(6) 4_566 3_756 ? O(4) V(1) O(6) 81.9(2) . 2_646 ? O(1) V(1) O(6) 156.2(2) . 2_646 ? O(2) V(1) O(6) 44.95(14) 3_656 2_646 ? O(3) V(1) O(6) 84.88(15) 3_756 2_646 ? O(8) V(1) O(6) 101.87(11) 3_656 2_646 ? O(5) V(1) O(6) 80.36(9) 1_655 2_646 ? O(5) V(1) O(6) 43.04(9) . 2_646 ? Tl V(1) O(6) 94.84(7) 3_656 2_646 ? O(3) V(1) O(6) 151.57(8) 4_566 2_646 ? O(2) V(1) O(6) 127.80(9) 4_566 2_646 ? Tl V(1) O(6) 129.69(7) 3_756 2_646 ? O(8) V(2) O(5) 111.2(2) 4_566 . ? O(8) V(2) O(6) 106.2(2) 4_566 4_566 ? O(5) V(2) O(6) 113.4(2) . 4_566 ? O(8) V(2) O(7) 106.0(2) 4_566 4_466 ? O(5) V(2) O(7) 113.4(2) . 4_466 ? O(6) V(2) O(7) 106.2(2) 4_566 4_466 ? O(8) V(2) O(4) 73.6(2) 4_566 1_455 ? O(5) V(2) O(4) 71.9(2) . 1_455 ? O(6) V(2) O(4) 174.0(2) 4_566 1_455 ? O(7) V(2) O(4) 68.5(2) 4_466 1_455 ? O(8) V(2) O(4) 73.6(2) 4_566 . ? O(5) V(2) O(4) 72.0(2) . . ? O(6) V(2) O(4) 68.6(2) 4_566 . ? O(7) V(2) O(4) 174.1(2) 4_466 . ? O(4) V(2) O(4) 116.64(14) 1_455 . ? O(8) V(2) O(5) 124.2(2) 4_566 3_657 ? O(5) V(2) O(5) 63.8(2) . 3_657 ? O(6) V(2) O(5) 49.61(14) 4_566 3_657 ? O(7) V(2) O(5) 127.74(15) 4_466 3_657 ? O(4) V(2) O(5) 135.56(11) 1_455 3_657 ? O(4) V(2) O(5) 51.32(11) . 3_657 ? O(8) V(2) O(5) 124.2(2) 4_566 3_557 ? O(5) V(2) O(5) 63.7(2) . 3_557 ? O(6) V(2) O(5) 127.45(15) 4_566 3_557 ? O(7) V(2) O(5) 49.61(14) 4_466 3_557 ? O(4) V(2) O(5) 51.40(11) 1_455 3_557 ? O(4) V(2) O(5) 135.64(11) . 3_557 ? O(5) V(2) O(5) 103.75(12) 3_657 3_557 ? O(8) V(2) O(4) 163.5(2) 4_566 3_657 ? O(5) V(2) O(4) 52.3(2) . 3_657 ? O(6) V(2) O(4) 83.44(15) 4_566 3_657 ? O(7) V(2) O(4) 83.45(15) 4_466 3_657 ? O(4) V(2) O(4) 98.23(10) 1_455 3_657 ? O(4) V(2) O(4) 98.44(10) . 3_657 ? O(5) V(2) O(4) 52.45(10) 3_657 3_657 ? O(5) V(2) O(4) 52.18(10) 3_557 3_657 ? O(8) V(2) Tl 89.4(2) 4_566 2_656 ? O(5) V(2) Tl 159.34(14) . 2_656 ? O(6) V(2) Tl 58.01(13) 4_566 2_656 ? O(7) V(2) Tl 57.97(13) 4_466 2_656 ? O(4) V(2) Tl 116.09(8) 1_455 2_656 ? O(4) V(2) Tl 116.11(8) . 2_656 ? O(5) V(2) Tl 105.24(7) 3_657 2_656 ? O(5) V(2) Tl 105.12(7) 3_557 2_656 ? O(4) V(2) Tl 107.07(7) 3_657 2_656 ? O(8) V(2) Tl 52.78(14) 4_566 4_466 ? O(5) V(2) Tl 117.88(14) . 4_466 ? O(6) V(2) Tl 128.72(14) 4_566 4_466 ? O(7) V(2) Tl 54.79(13) 4_466 4_466 ? O(4) V(2) Tl 46.31(9) 1_455 4_466 ? O(4) V(2) Tl 125.89(9) . 4_466 ? O(5) V(2) Tl 176.70(7) 3_657 4_466 ? O(5) V(2) Tl 79.51(8) 3_557 4_466 ? O(4) V(2) Tl 130.85(8) 3_657 4_466 ? Tl V(2) Tl 74.12(3) 2_656 4_466 ? O(8) V(2) Tl 52.81(14) 4_566 4_566 ? O(5) V(2) Tl 117.86(14) . 4_566 ? O(6) V(2) Tl 55.04(13) 4_566 4_566 ? O(7) V(2) Tl 128.73(14) 4_466 4_566 ? O(4) V(2) Tl 125.86(9) 1_455 4_566 ? O(4) V(2) Tl 46.20(9) . 4_566 ? O(5) V(2) Tl 79.46(8) 3_657 4_566 ? O(5) V(2) Tl 176.76(7) 3_557 4_566 ? O(4) V(2) Tl 131.06(8) 3_657 4_566 ? Tl V(2) Tl 74.25(3) 2_656 4_566 ? Tl V(2) Tl 97.28(6) 4_466 4_566 ? V(1) O(1) Sb 148.3(2) . 4_566 ? V(1) O(1) O(4) 34.01(12) . . ? Sb O(1) O(4) 114.3(2) 4_566 . ? V(1) O(1) O(6) 149.2(2) . . ? Sb O(1) O(6) 45.95(11) 4_566 . ? O(4) O(1) O(6) 138.8(2) . . ? V(1) O(1) O(7) 149.6(2) . . ? Sb O(1) O(7) 46.04(11) 4_566 . ? O(4) O(1) O(7) 139.1(2) . . ? O(6) O(1) O(7) 60.45(14) . . ? V(1) O(1) O(3) 109.6(2) . 4_566 ? Sb O(1) O(3) 44.68(11) 4_566 4_566 ? O(4) O(1) O(3) 79.9(2) . 4_566 ? O(6) O(1) O(3) 90.6(2) . 4_566 ? O(7) O(1) O(3) 62.01(14) . 4_566 ? V(1) O(1) O(2) 109.5(2) . 4_566 ? Sb O(1) O(2) 44.68(11) 4_566 4_566 ? O(4) O(1) O(2) 79.9(2) . 4_566 ? O(6) O(1) O(2) 61.71(14) . 4_566 ? O(7) O(1) O(2) 90.7(2) . 4_566 ? O(3) O(1) O(2) 57.37(14) 4_566 4_566 ? V(1) O(1) O(8) 77.7(2) . 3_656 ? Sb O(1) O(8) 134.0(2) 4_566 3_656 ? O(4) O(1) O(8) 111.7(2) . 3_656 ? O(6) O(1) O(8) 96.6(2) . 3_656 ? O(7) O(1) O(8) 96.3(2) . 3_656 ? O(3) O(1) O(8) 149.7(2) 4_566 3_656 ? O(2) O(1) O(8) 149.7(2) 4_566 3_656 ? V(1) O(1) O(3) 34.79(12) . 3_756 ? Sb O(1) O(3) 147.4(2) 4_566 3_756 ? O(4) O(1) O(3) 57.97(14) . 3_756 ? O(6) O(1) O(3) 160.2(2) . 3_756 ? O(7) O(1) O(3) 115.9(2) . 3_756 ? O(3) O(1) O(3) 104.80(13) 4_566 3_756 ? O(2) O(1) O(3) 137.4(2) 4_566 3_756 ? O(8) O(1) O(3) 63.93(14) 3_656 3_756 ? V(1) O(1) O(2) 34.44(11) . 3_656 ? Sb O(1) O(2) 147.3(2) 4_566 3_656 ? O(4) O(1) O(2) 57.80(15) . 3_656 ? O(6) O(1) O(2) 115.9(2) . 3_656 ? O(7) O(1) O(2) 160.2(2) . 3_656 ? O(3) O(1) O(2) 137.1(2) 4_566 3_656 ? O(2) O(1) O(2) 104.64(13) 4_566 3_656 ? O(8) O(1) O(2) 64.13(14) 3_656 3_656 ? O(3) O(1) O(2) 60.02(14) 3_756 3_656 ? V(1) O(1) Tl 90.6(2) . 3_656 ? Sb O(1) Tl 105.72(15) 4_566 3_656 ? O(4) O(1) Tl 108.2(2) . 3_656 ? O(6) O(1) Tl 61.66(12) . 3_656 ? O(7) O(1) Tl 111.86(15) . 3_656 ? O(3) O(1) Tl 146.7(2) 4_566 3_656 ? O(2) O(1) Tl 91.47(14) 4_566 3_656 ? O(8) O(1) Tl 58.53(11) 3_656 3_656 ? O(3) O(1) Tl 106.69(14) 3_756 3_656 ? O(2) O(1) Tl 56.31(11) 3_656 3_656 ? V(1) O(1) Tl 91.0(2) . 3_756 ? Sb O(1) Tl 105.69(15) 4_566 3_756 ? O(4) O(1) Tl 108.3(2) . 3_756 ? O(6) O(1) Tl 111.94(15) . 3_756 ? O(7) O(1) Tl 61.58(12) . 3_756 ? O(3) O(1) Tl 91.65(14) 4_566 3_756 ? O(2) O(1) Tl 146.8(2) 4_566 3_756 ? O(8) O(1) Tl 58.39(11) 3_656 3_756 ? O(3) O(1) Tl 56.31(11) 3_756 3_756 ? O(2) O(1) Tl 106.81(14) 3_656 3_756 ? Tl O(1) Tl 114.83(12) 3_656 3_756 ? V(1) O(2) Sb 142.9(2) 3_656 . ? V(1) O(2) O(3) 145.1(2) 3_656 . ? Sb O(2) O(3) 46.91(12) . . ? V(1) O(2) O(4) 34.15(12) 3_656 3_656 ? Sb O(2) O(4) 110.2(2) . 3_656 ? O(3) O(2) O(4) 122.2(2) . 3_656 ? V(1) O(2) O(1) 153.6(2) 3_656 4_565 ? Sb O(2) O(1) 44.79(11) . 4_565 ? O(3) O(2) O(1) 61.25(14) . 4_565 ? O(4) O(2) O(1) 147.0(2) 3_656 4_565 ? V(1) O(2) O(6) 109.0(2) 3_656 4_565 ? Sb O(2) O(6) 43.69(11) . 4_565 ? O(3) O(2) O(6) 90.6(2) . 4_565 ? O(4) O(2) O(6) 89.3(2) 3_656 4_565 ? O(1) O(2) O(6) 57.81(13) 4_565 4_565 ? V(1) O(2) O(5) 104.0(2) 3_656 3_656 ? Sb O(2) O(5) 43.45(11) . 3_656 ? O(3) O(2) O(5) 61.94(14) . 3_656 ? O(4) O(2) O(5) 69.9(2) 3_656 3_656 ? O(1) O(2) O(5) 88.19(15) 4_565 3_656 ? O(6) O(2) O(5) 57.75(13) 4_565 3_656 ? V(1) O(2) O(3) 34.84(12) 3_656 1_455 ? Sb O(2) O(3) 133.3(2) . 1_455 ? O(3) O(2) O(3) 179.7(2) . 1_455 ? O(4) O(2) O(3) 57.91(14) 3_656 1_455 ? O(1) O(2) O(3) 118.8(2) 4_565 1_455 ? O(6) O(2) O(3) 89.64(15) 4_565 1_455 ? O(5) O(2) O(3) 118.3(2) 3_656 1_455 ? V(1) O(2) O(1) 34.12(11) 3_656 3_656 ? Sb O(2) O(1) 157.4(2) . 3_656 ? O(3) O(2) O(1) 120.0(2) . 3_656 ? O(4) O(2) O(1) 57.78(14) 3_656 3_656 ? O(1) O(2) O(1) 153.5(2) 4_565 3_656 ? O(6) O(2) O(1) 143.1(2) 4_565 3_656 ? O(5) O(2) O(1) 116.3(2) 3_656 3_656 ? O(3) O(2) O(1) 59.87(14) 1_455 3_656 ? V(1) O(2) Tl 103.0(2) 3_656 . ? Sb O(2) Tl 108.0(2) . . ? O(3) O(2) Tl 62.88(12) . . ? O(4) O(2) Tl 119.3(2) 3_656 . ? O(1) O(2) Tl 92.08(14) 4_565 . ? O(6) O(2) Tl 148.0(2) 4_565 . ? O(5) O(2) Tl 116.0(2) 3_656 . ? O(3) O(2) Tl 116.86(14) 1_455 . ? O(1) O(2) Tl 68.96(12) 3_656 . ? V(1) O(2) O(8) 71.63(15) 3_656 . ? Sb O(2) O(8) 142.5(2) . . ? O(3) O(2) O(8) 118.4(2) . . ? O(4) O(2) O(8) 105.7(2) 3_656 . ? O(1) O(2) O(8) 98.1(2) 4_565 . ? O(6) O(2) O(8) 128.5(2) 4_565 . ? O(5) O(2) O(8) 173.0(2) 3_656 . ? O(3) O(2) O(8) 61.33(13) 1_455 . ? O(1) O(2) O(8) 56.95(14) 3_656 . ? Tl O(2) O(8) 60.77(11) . . ? V(1) O(2) O(4) 129.5(2) 3_656 4_565 ? Sb O(2) O(4) 86.91(15) . 4_565 ? O(3) O(2) O(4) 67.63(14) . 4_565 ? O(4) O(2) O(4) 162.68(14) 3_656 4_565 ? O(1) O(2) O(4) 48.99(12) 4_565 4_565 ? O(6) O(2) O(4) 105.4(2) 4_565 4_565 ? O(5) O(2) O(4) 125.6(2) 3_656 4_565 ? O(3) O(2) O(4) 112.2(2) 1_455 4_565 ? O(1) O(2) O(4) 105.29(15) 3_656 4_565 ? Tl O(2) O(4) 49.61(9) . 4_565 ? O(8) O(2) O(4) 58.02(13) . 4_565 ? V(1) O(3) Sb 142.4(2) 3_756 . ? V(1) O(3) O(2) 145.3(2) 3_756 . ? Sb O(3) O(2) 46.99(12) . . ? V(1) O(3) O(4) 34.10(12) 3_756 3_756 ? Sb O(3) O(4) 109.9(2) . 3_756 ? O(2) O(3) O(4) 122.1(2) . 3_756 ? V(1) O(3) O(1) 153.3(2) 3_756 4_565 ? Sb O(3) O(1) 44.86(11) . 4_565 ? O(2) O(3) O(1) 61.38(15) . 4_565 ? O(4) O(3) O(1) 146.8(2) 3_756 4_565 ? V(1) O(3) O(7) 108.6(2) 3_756 4_565 ? Sb O(3) O(7) 43.59(11) . 4_565 ? O(2) O(3) O(7) 90.6(2) . 4_565 ? O(4) O(3) O(7) 89.1(2) 3_756 4_565 ? O(1) O(3) O(7) 57.79(13) 4_565 4_565 ? V(1) O(3) O(5) 103.6(2) 3_756 3_656 ? Sb O(3) O(5) 43.52(11) . 3_656 ? O(2) O(3) O(5) 62.07(14) . 3_656 ? O(4) O(3) O(5) 69.5(2) 3_756 3_656 ? O(1) O(3) O(5) 88.3(2) 4_565 3_656 ? O(7) O(3) O(5) 57.66(13) 4_565 3_656 ? V(1) O(3) O(1) 34.37(11) 3_756 3_756 ? Sb O(3) O(1) 157.4(2) . 3_756 ? O(2) O(3) O(1) 120.1(2) . 3_756 ? O(4) O(3) O(1) 57.83(14) 3_756 3_756 ? O(1) O(3) O(1) 153.7(2) 4_565 3_756 ? O(7) O(3) O(1) 142.9(2) 4_565 3_756 ? O(5) O(3) O(1) 116.1(2) 3_656 3_756 ? V(1) O(3) O(2) 34.74(12) 3_756 1_655 ? Sb O(3) O(2) 132.8(2) . 1_655 ? O(2) O(3) O(2) 179.7(2) . 1_655 ? O(4) O(3) O(2) 57.79(14) 3_756 1_655 ? O(1) O(3) O(2) 118.6(2) 4_565 1_655 ? O(7) O(3) O(2) 89.21(15) 4_565 1_655 ? O(5) O(3) O(2) 117.7(2) 3_656 1_655 ? O(1) O(3) O(2) 60.11(14) 3_756 1_655 ? V(1) O(3) Tl 103.3(2) 3_756 . ? Sb O(3) Tl 108.1(2) . . ? O(2) O(3) Tl 62.95(11) . . ? O(4) O(3) Tl 119.5(2) 3_756 . ? O(1) O(3) Tl 92.18(14) 4_565 . ? O(7) O(3) Tl 148.0(2) 4_565 . ? O(5) O(3) Tl 116.2(2) 3_656 . ? O(1) O(3) Tl 69.11(12) 3_756 . ? O(2) O(3) Tl 117.31(14) 1_655 . ? V(1) O(3) O(8) 71.93(15) 3_756 1_655 ? Sb O(3) O(8) 142.5(2) . 1_655 ? O(2) O(3) O(8) 118.5(2) . 1_655 ? O(4) O(3) O(8) 106.0(2) 3_756 1_655 ? O(1) O(3) O(8) 98.0(2) 4_565 1_655 ? O(7) O(3) O(8) 128.5(2) 4_565 1_655 ? O(5) O(3) O(8) 173.0(2) 3_656 1_655 ? O(1) O(3) O(8) 57.16(14) 3_756 1_655 ? O(2) O(3) O(8) 61.76(13) 1_655 1_655 ? Tl O(3) O(8) 60.80(11) . 1_655 ? V(1) O(3) O(4) 129.7(2) 3_756 4_565 ? Sb O(3) O(4) 87.07(15) . 4_565 ? O(2) O(3) O(4) 67.79(14) . 4_565 ? O(4) O(3) O(4) 162.85(15) 3_756 4_565 ? O(1) O(3) O(4) 49.06(12) 4_565 4_565 ? O(7) O(3) O(4) 105.5(2) 4_565 4_565 ? O(5) O(3) O(4) 125.9(2) 3_656 4_565 ? O(1) O(3) O(4) 105.43(15) 3_756 4_565 ? O(2) O(3) O(4) 112.4(2) 1_655 4_565 ? Tl O(3) O(4) 49.67(9) . 4_565 ? O(8) O(3) O(4) 57.90(13) 1_655 4_565 ? V(1) O(4) O(1) 37.55(13) . . ? V(1) O(4) O(2) 38.08(13) . 3_656 ? O(1) O(4) O(2) 64.4(2) . 3_656 ? V(1) O(4) O(3) 38.13(13) . 3_756 ? O(1) O(4) O(3) 64.2(2) . 3_756 ? O(2) O(4) O(3) 64.3(2) 3_656 3_756 ? V(1) O(4) Tl 135.4(2) . 4_566 ? O(1) O(4) Tl 97.9(2) . 4_566 ? O(2) O(4) Tl 141.2(2) 3_656 4_566 ? O(3) O(4) Tl 141.3(2) 3_756 4_566 ? V(1) O(4) O(5) 116.7(2) . 3_657 ? O(1) O(4) O(5) 154.3(2) . 3_657 ? O(2) O(4) O(5) 94.1(2) 3_656 3_657 ? O(3) O(4) O(5) 94.4(2) 3_756 3_657 ? Tl O(4) O(5) 107.9(2) 4_566 3_657 ? V(1) O(4) O(7) 150.6(2) . 4_566 ? O(1) O(4) O(7) 145.6(2) . 4_566 ? O(2) O(4) O(7) 148.0(2) 3_656 4_566 ? O(3) O(4) O(7) 112.5(2) 3_756 4_566 ? Tl O(4) O(7) 62.44(12) 4_566 4_566 ? O(5) O(4) O(7) 53.92(13) 3_657 4_566 ? V(1) O(4) O(6) 150.1(2) . 4_566 ? O(1) O(4) O(6) 145.5(2) . 4_566 ? O(2) O(4) O(6) 112.0(2) 3_656 4_566 ? O(3) O(4) O(6) 148.2(2) 3_756 4_566 ? Tl O(4) O(6) 62.55(12) 4_566 4_566 ? O(5) O(4) O(6) 53.78(13) 3_657 4_566 ? O(7) O(4) O(6) 52.47(12) 4_566 4_566 ? V(1) O(4) O(5) 95.4(2) . 1_655 ? O(1) O(4) O(5) 111.3(2) . 1_655 ? O(2) O(4) O(5) 112.9(2) 3_656 1_655 ? O(3) O(4) O(5) 57.31(14) 3_756 1_655 ? Tl O(4) O(5) 105.68(15) 4_566 1_655 ? O(5) O(4) O(5) 62.22(15) 3_657 1_655 ? O(7) O(4) O(5) 55.17(13) 4_566 1_655 ? O(6) O(4) O(5) 101.6(2) 4_566 1_655 ? V(1) O(4) O(5) 95.3(2) . . ? O(1) O(4) O(5) 111.4(2) . . ? O(2) O(4) O(5) 57.22(14) 3_656 . ? O(3) O(4) O(5) 113.0(2) 3_756 . ? Tl O(4) O(5) 105.44(15) 4_566 . ? O(5) O(4) O(5) 62.0(2) 3_657 . ? O(7) O(4) O(5) 101.4(2) 4_566 . ? O(6) O(4) O(5) 54.81(13) 4_566 . ? O(5) O(4) O(5) 121.9(2) 1_655 . ? V(1) O(4) O(8) 112.1(2) . 4_666 ? O(1) O(4) O(8) 95.5(2) . 4_666 ? O(2) O(4) O(8) 149.2(2) 3_656 4_666 ? O(3) O(4) O(8) 86.4(2) 3_756 4_666 ? Tl O(4) O(8) 60.20(12) 4_566 4_666 ? O(5) O(4) O(8) 97.3(2) 3_657 4_666 ? O(7) O(4) O(8) 50.68(12) 4_566 4_666 ? O(6) O(4) O(8) 97.7(2) 4_566 4_666 ? O(5) O(4) O(8) 50.59(13) 1_655 4_666 ? O(5) O(4) O(8) 151.6(2) . 4_666 ? V(1) O(4) O(8) 111.9(2) . 4_566 ? O(1) O(4) O(8) 95.6(2) . 4_566 ? O(2) O(4) O(8) 86.3(2) 3_656 4_566 ? O(3) O(4) O(8) 149.1(2) 3_756 4_566 ? Tl O(4) O(8) 60.16(12) 4_566 4_566 ? O(5) O(4) O(8) 97.0(2) 3_657 4_566 ? O(7) O(4) O(8) 97.4(2) 4_566 4_566 ? O(6) O(4) O(8) 50.44(12) 4_566 4_566 ? O(5) O(4) O(8) 151.6(2) 1_655 4_566 ? O(5) O(4) O(8) 50.36(13) . 4_566 ? O(8) O(4) O(8) 120.2(2) 4_666 4_566 ? V(2) O(5) Sb 161.8(2) . 3_656 ? V(2) O(5) O(8) 33.20(12) . 4_566 ? Sb O(5) O(8) 128.6(2) 3_656 4_566 ? V(2) O(5) O(7) 145.7(2) . 2_646 ? Sb O(5) O(7) 45.54(11) 3_656 2_646 ? O(8) O(5) O(7) 146.8(2) 4_566 2_646 ? V(2) O(5) O(6) 145.6(2) . 2_646 ? Sb O(5) O(6) 45.39(11) 3_656 2_646 ? O(8) O(5) O(6) 146.6(2) 4_566 2_646 ? O(7) O(5) O(6) 59.81(14) 2_646 2_646 ? V(2) O(5) O(3) 122.3(2) . 3_656 ? Sb O(5) O(3) 43.36(11) 3_656 3_656 ? O(8) O(5) O(3) 93.5(2) 4_566 3_656 ? O(7) O(5) O(3) 60.92(14) 2_646 3_656 ? O(6) O(5) O(3) 88.7(2) 2_646 3_656 ? V(2) O(5) O(2) 122.2(2) . 3_656 ? Sb O(5) O(2) 43.36(11) 3_656 3_656 ? O(8) O(5) O(2) 93.5(2) 4_566 3_656 ? O(7) O(5) O(2) 88.9(2) 2_646 3_656 ? O(6) O(5) O(2) 60.58(14) 2_646 3_656 ? O(3) O(5) O(2) 55.99(14) 3_656 3_656 ? V(2) O(5) O(6) 34.03(12) . 4_566 ? Sb O(5) O(6) 150.8(2) 3_656 4_566 ? O(8) O(5) O(6) 57.16(14) 4_566 4_566 ? O(7) O(5) O(6) 148.5(2) 2_646 4_566 ? O(6) O(5) O(6) 111.6(2) 2_646 4_566 ? O(3) O(5) O(6) 149.8(2) 3_656 4_566 ? O(2) O(5) O(6) 114.0(2) 3_656 4_566 ? V(2) O(5) O(7) 34.09(12) . 4_466 ? Sb O(5) O(7) 150.9(2) 3_656 4_466 ? O(8) O(5) O(7) 57.11(14) 4_566 4_466 ? O(7) O(5) O(7) 111.6(2) 2_646 4_466 ? O(6) O(5) O(7) 148.8(2) 2_646 4_466 ? O(3) O(5) O(7) 114.1(2) 3_656 4_466 ? O(2) O(5) O(7) 149.8(2) 3_656 4_466 ? O(6) O(5) O(7) 58.39(14) 4_566 4_466 ? V(2) O(5) O(4) 100.7(2) . 3_657 ? Sb O(5) O(4) 97.5(2) 3_656 3_657 ? O(8) O(5) O(4) 133.9(2) 4_566 3_657 ? O(7) O(5) O(4) 65.44(15) 2_646 3_657 ? O(6) O(5) O(4) 65.77(15) 2_646 3_657 ? O(3) O(5) O(4) 126.3(2) 3_656 3_657 ? O(2) O(5) O(4) 126.3(2) 3_656 3_657 ? O(6) O(5) O(4) 83.3(2) 4_566 3_657 ? O(7) O(5) O(4) 83.3(2) 4_466 3_657 ? V(2) O(5) O(5) 87.5(2) . 3_657 ? Sb O(5) O(5) 100.9(2) 3_656 3_657 ? O(8) O(5) O(5) 103.1(2) 4_566 3_657 ? O(7) O(5) O(5) 110.1(2) 2_646 3_657 ? O(6) O(5) O(5) 58.06(15) 2_646 3_657 ? O(3) O(5) O(5) 140.4(2) 3_656 3_657 ? O(2) O(5) O(5) 86.9(2) 3_656 3_657 ? O(6) O(5) O(5) 53.50(14) 4_566 3_657 ? O(7) O(5) O(5) 105.1(2) 4_466 3_657 ? O(4) O(5) O(5) 62.5(2) 3_657 3_657 ? V(2) O(5) O(4) 77.5(2) . 1_455 ? Sb O(5) O(4) 94.0(2) 3_656 1_455 ? O(8) O(5) O(4) 65.22(14) 4_566 1_455 ? O(7) O(5) O(4) 81.9(2) 2_646 1_455 ? O(6) O(5) O(4) 136.9(2) 2_646 1_455 ? O(3) O(5) O(4) 53.16(13) 3_656 1_455 ? O(2) O(5) O(4) 102.8(2) 3_656 1_455 ? O(6) O(5) O(4) 111.5(2) 4_566 1_455 ? O(7) O(5) O(4) 60.89(13) 4_466 1_455 ? O(4) O(5) O(4) 117.78(15) 3_657 1_455 ? O(5) O(5) O(4) 164.9(2) 3_657 1_455 ? V(2) O(6) Sb 142.1(2) 4_565 4_566 ? V(2) O(6) O(8) 34.79(12) 4_565 . ? Sb O(6) O(8) 160.0(2) 4_566 . ? V(2) O(6) O(1) 157.2(2) 4_565 . ? Sb O(6) O(1) 46.37(12) 4_566 . ? O(8) O(6) O(1) 148.1(2) . . ? V(2) O(6) O(7) 142.9(2) 4_565 . ? Sb O(6) O(7) 45.71(11) 4_566 . ? O(8) O(6) O(7) 121.4(2) . . ? O(1) O(6) O(7) 59.84(14) . . ? V(2) O(6) O(5) 101.0(2) 4_565 2_656 ? Sb O(6) O(5) 45.78(12) 4_566 2_656 ? O(8) O(6) O(5) 116.7(2) . 2_656 ? O(1) O(6) O(5) 92.1(2) . 2_656 ? O(7) O(6) O(5) 60.09(14) . 2_656 ? V(2) O(6) O(2) 109.9(2) 4_565 4_566 ? Sb O(6) O(2) 43.97(11) 4_566 4_566 ? O(8) O(6) O(2) 144.5(2) . 4_566 ? O(1) O(6) O(2) 60.48(14) . 4_566 ? O(7) O(6) O(2) 89.7(2) . 4_566 ? O(5) O(6) O(2) 61.66(14) 2_656 4_566 ? V(2) O(6) O(7) 36.97(11) 4_565 1_455 ? Sb O(6) O(7) 134.6(2) 4_566 1_455 ? O(8) O(6) O(7) 58.34(14) . 1_455 ? O(1) O(6) O(7) 120.3(2) . 1_455 ? O(7) O(6) O(7) 179.7(2) . 1_455 ? O(5) O(6) O(7) 120.1(2) 2_656 1_455 ? O(2) O(6) O(7) 90.6(2) 4_566 1_455 ? V(2) O(6) O(5) 32.62(11) 4_565 4_565 ? Sb O(6) O(5) 111.2(2) 4_566 4_565 ? O(8) O(6) O(5) 58.21(15) . 4_565 ? O(1) O(6) O(5) 153.0(2) . 4_565 ? O(7) O(6) O(5) 119.1(2) . 4_565 ? O(5) O(6) O(5) 68.4(2) 2_656 4_565 ? O(2) O(6) O(5) 93.1(2) 4_566 4_565 ? O(7) O(6) O(5) 60.89(13) 1_455 4_565 ? V(2) O(6) Tl 96.7(2) 4_565 . ? Sb O(6) Tl 108.7(2) 4_566 . ? O(8) O(6) Tl 63.02(12) . . ? O(1) O(6) Tl 97.45(14) . . ? O(7) O(6) Tl 63.15(12) . . ? O(5) O(6) Tl 105.75(15) 2_656 . ? O(2) O(6) Tl 152.0(2) 4_566 . ? O(7) O(6) Tl 116.58(15) 1_455 . ? O(5) O(6) Tl 105.65(14) 4_565 . ? V(2) O(6) O(4) 79.4(2) 4_565 4_565 ? Sb O(6) O(4) 93.4(2) 4_566 4_565 ? O(8) O(6) O(4) 66.95(15) . 4_565 ? O(1) O(6) O(4) 123.3(2) . 4_565 ? O(7) O(6) O(4) 63.51(14) . 4_565 ? O(5) O(6) O(4) 60.46(14) 2_656 4_565 ? O(2) O(6) O(4) 122.1(2) 4_566 4_565 ? O(7) O(6) O(4) 116.4(2) 1_455 4_565 ? O(5) O(6) O(4) 64.13(14) 4_565 4_565 ? Tl O(6) O(4) 53.40(11) . 4_565 ? V(2) O(6) Tl 93.4(2) 4_565 3_656 ? Sb O(6) Tl 112.7(2) 4_566 3_656 ? O(8) O(6) Tl 86.43(15) . 3_656 ? O(1) O(6) Tl 68.42(12) . 3_656 ? O(7) O(6) Tl 116.88(15) . 3_656 ? O(5) O(6) Tl 155.3(2) 2_656 3_656 ? O(2) O(6) Tl 94.61(14) 4_566 3_656 ? O(7) O(6) Tl 63.06(11) 1_455 3_656 ? O(5) O(6) Tl 123.42(15) 4_565 3_656 ? Tl O(6) Tl 92.23(11) . 3_656 ? O(4) O(6) Tl 143.0(2) 4_565 3_656 ? V(2) O(7) Sb 141.9(2) 4_665 4_566 ? V(2) O(7) O(8) 34.84(12) 4_665 1_655 ? Sb O(7) O(8) 160.2(2) 4_566 1_655 ? V(2) O(7) O(1) 157.0(2) 4_665 . ? Sb O(7) O(1) 46.30(12) 4_566 . ? O(8) O(7) O(1) 148.3(2) 1_655 . ? V(2) O(7) O(6) 143.3(2) 4_665 . ? Sb O(7) O(6) 45.55(11) 4_566 . ? O(8) O(7) O(6) 121.9(2) 1_655 . ? O(1) O(7) O(6) 59.72(14) . . ? V(2) O(7) O(5) 100.9(2) 4_665 2_656 ? Sb O(7) O(5) 45.77(12) 4_566 2_656 ? O(8) O(7) O(5) 116.7(2) 1_655 2_656 ? O(1) O(7) O(5) 92.0(2) . 2_656 ? O(6) O(7) O(5) 60.09(14) . 2_656 ? V(2) O(7) O(6) 36.84(11) 4_665 1_655 ? Sb O(7) O(6) 134.2(2) 4_566 1_655 ? O(8) O(7) O(6) 58.33(14) 1_655 1_655 ? O(1) O(7) O(6) 120.2(2) . 1_655 ? O(6) O(7) O(6) 179.7(2) . 1_655 ? O(5) O(7) O(6) 119.7(2) 2_656 1_655 ? V(2) O(7) O(3) 109.8(2) 4_665 4_566 ? Sb O(7) O(3) 43.65(11) 4_566 4_566 ? O(8) O(7) O(3) 144.4(2) 1_655 4_566 ? O(1) O(7) O(3) 60.20(14) . 4_566 ? O(6) O(7) O(3) 89.2(2) . 4_566 ? O(5) O(7) O(3) 61.42(14) 2_656 4_566 ? O(6) O(7) O(3) 90.6(2) 1_655 4_566 ? V(2) O(7) O(5) 32.56(11) 4_665 4_665 ? Sb O(7) O(5) 111.2(2) 4_566 4_665 ? O(8) O(7) O(5) 58.15(15) 1_655 4_665 ? O(1) O(7) O(5) 152.7(2) . 4_665 ? O(6) O(7) O(5) 119.2(2) . 4_665 ? O(5) O(7) O(5) 68.4(2) 2_656 4_665 ? O(6) O(7) O(5) 60.73(13) 1_655 4_665 ? O(3) O(7) O(5) 93.1(2) 4_566 4_665 ? V(2) O(7) Tl 96.9(2) 4_665 . ? Sb O(7) Tl 109.0(2) 4_566 . ? O(8) O(7) Tl 63.07(12) 1_655 . ? O(1) O(7) Tl 97.68(15) . . ? O(6) O(7) Tl 63.64(12) . . ? O(5) O(7) Tl 106.10(15) 2_656 . ? O(6) O(7) Tl 116.63(15) 1_655 . ? O(3) O(7) Tl 152.0(2) 4_566 . ? O(5) O(7) Tl 105.73(14) 4_665 . ? V(2) O(7) O(4) 79.3(2) 4_665 4_565 ? Sb O(7) O(4) 93.7(2) 4_566 4_565 ? O(8) O(7) O(4) 66.85(15) 1_655 4_565 ? O(1) O(7) O(4) 123.7(2) . 4_565 ? O(6) O(7) O(4) 64.02(14) . 4_565 ? O(5) O(7) O(4) 60.64(14) 2_656 4_565 ? O(6) O(7) O(4) 116.1(2) 1_655 4_565 ? O(3) O(7) O(4) 122.0(2) 4_566 4_565 ? O(5) O(7) O(4) 63.94(14) 4_665 4_565 ? Tl O(7) O(4) 53.65(11) . 4_565 ? V(2) O(7) Tl 93.29(15) 4_665 3_756 ? Sb O(7) Tl 112.59(15) 4_566 3_756 ? O(8) O(7) Tl 86.46(14) 1_655 3_756 ? O(1) O(7) Tl 68.44(12) . 3_756 ? O(6) O(7) Tl 116.95(15) . 3_756 ? O(5) O(7) Tl 155.1(2) 2_656 3_756 ? O(6) O(7) Tl 63.11(11) 1_655 3_756 ? O(3) O(7) Tl 94.56(14) 4_566 3_756 ? O(5) O(7) Tl 123.31(15) 4_665 3_756 ? Tl O(7) Tl 92.24(11) . 3_756 ? O(4) O(7) Tl 143.1(2) 4_565 3_756 ? V(2) O(8) O(6) 39.01(12) 4_565 . ? V(2) O(8) O(7) 39.21(12) 4_565 1_455 ? O(6) O(8) O(7) 63.32(15) . 1_455 ? V(2) O(8) O(5) 35.58(14) 4_565 4_565 ? O(6) O(8) O(5) 64.6(2) . 4_565 ? O(7) O(8) O(5) 64.74(15) 1_455 4_565 ? V(2) O(8) O(1) 144.0(3) 4_565 3_656 ? O(6) O(8) O(1) 115.0(2) . 3_656 ? O(7) O(8) O(1) 115.0(2) 1_455 3_656 ? O(5) O(8) O(1) 179.6(2) 4_565 3_656 ? V(2) O(8) V(1) 178.7(3) 4_565 3_656 ? O(6) O(8) V(1) 140.1(2) . 3_656 ? O(7) O(8) V(1) 140.2(2) 1_455 3_656 ? O(5) O(8) V(1) 145.7(2) 4_565 3_656 ? O(1) O(8) V(1) 34.69(9) 3_656 3_656 ? V(2) O(8) Tl 102.2(2) 4_565 1_455 ? O(6) O(8) Tl 122.1(2) . 1_455 ? O(7) O(8) Tl 64.21(12) 1_455 1_455 ? O(5) O(8) Tl 111.3(2) 4_565 1_455 ? O(1) O(8) Tl 68.73(13) 3_656 1_455 ? V(1) O(8) Tl 77.50(11) 3_656 1_455 ? V(2) O(8) O(3) 146.8(2) 4_565 1_455 ? O(6) O(8) O(3) 173.8(2) . 1_455 ? O(7) O(8) O(3) 119.6(2) 1_455 1_455 ? O(5) O(8) O(3) 121.4(2) 4_565 1_455 ? O(1) O(8) O(3) 58.92(14) 3_656 1_455 ? V(1) O(8) O(3) 34.03(9) 3_656 1_455 ? Tl O(8) O(3) 58.29(11) 1_455 1_455 ? V(2) O(8) Tl 102.2(2) 4_565 . ? O(6) O(8) Tl 64.44(12) . . ? O(7) O(8) Tl 122.3(2) 1_455 . ? O(5) O(8) Tl 111.3(2) 4_565 . ? O(1) O(8) Tl 68.61(13) 3_656 . ? V(1) O(8) Tl 77.16(10) 3_656 . ? Tl O(8) Tl 134.1(2) 1_455 . ? O(3) O(8) Tl 110.45(15) 1_455 . ? V(2) O(8) O(2) 146.6(2) 4_565 . ? O(6) O(8) O(2) 119.6(2) . . ? O(7) O(8) O(2) 173.7(2) 1_455 . ? O(5) O(8) O(2) 121.4(2) 4_565 . ? O(1) O(8) O(2) 58.92(14) 3_656 . ? V(1) O(8) O(2) 33.87(9) 3_656 . ? Tl O(8) O(2) 110.61(15) 1_455 . ? O(3) O(8) O(2) 56.91(13) 1_455 . ? Tl O(8) O(2) 58.13(11) . . ? V(2) O(8) O(4) 77.8(2) 4_565 4_465 ? O(6) O(8) O(4) 116.5(2) . 4_465 ? O(7) O(8) O(4) 62.47(14) 1_455 4_465 ? O(5) O(8) O(4) 64.19(15) 4_565 4_465 ? O(1) O(8) O(4) 116.0(2) 3_656 4_465 ? V(1) O(8) O(4) 102.97(14) 3_656 4_465 ? Tl O(8) O(4) 52.78(11) 1_455 4_465 ? O(3) O(8) O(4) 69.03(14) 1_455 4_465 ? Tl O(8) O(4) 172.2(2) . 4_465 ? O(2) O(8) O(4) 117.9(2) . 4_465 ? V(2) O(8) O(4) 77.8(2) 4_565 4_565 ? O(6) O(8) O(4) 62.60(14) . 4_565 ? O(7) O(8) O(4) 116.8(2) 1_455 4_565 ? O(5) O(8) O(4) 64.34(15) 4_565 4_565 ? O(1) O(8) O(4) 115.7(2) 3_656 4_565 ? V(1) O(8) O(4) 102.58(14) 3_656 4_565 ? Tl O(8) O(4) 172.3(2) 1_455 4_565 ? O(3) O(8) O(4) 117.8(2) 1_455 4_565 ? Tl O(8) O(4) 52.60(11) . 4_565 ? O(2) O(8) O(4) 68.80(14) . 4_565 ? O(4) O(8) O(4) 120.2(2) 4_465 4_565 ? _refine_diff_density_max 1.425 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.407 #=END data_cs _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Cs O8 Sb V2' _chemical_formula_weight 484.49 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cs' 'Cs' -0.3680 2.1192 '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' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 5.627(2) _cell_length_b 16.178(4) _cell_length_c 8.400(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.30(5) _cell_angle_gamma 90.00 _cell_volume 764.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'rectangular blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.209 _exptl_crystal_density_method ? _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 10.563 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.85 _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 'Enraf Nonius CAD4' _diffrn_measurement_method '2theta-omega' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 3 _diffrn_reflns_number 1345 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1345 _reflns_number_observed 1308 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 programs' _computing_cell_refinement 'CAD4 programs' _computing_data_reduction MOLEN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP92 _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+37.0107P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1345 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_obs 0.0481 _refine_ls_wR_factor_all 0.1262 _refine_ls_wR_factor_obs 0.1254 _refine_ls_goodness_of_fit_all 1.186 _refine_ls_goodness_of_fit_obs 1.196 _refine_ls_restrained_S_all 1.186 _refine_ls_restrained_S_obs 1.196 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cs Cs 0.73861(15) 0.21421(5) 0.00531(11) 0.0210(3) Uani 1 d . . Sb Sb 0.25778(13) 0.05058(5) 0.74138(9) 0.0074(3) Uani 1 d . . V(1) V 0.7443(3) 0.11001(12) 0.5416(2) 0.0083(4) Uani 1 d . . V(2) V 0.2302(4) 0.07623(12) 1.1388(2) 0.0091(5) Uani 1 d . . O(1) O 0.7450(15) 0.0116(5) 0.4592(10) 0.012(2) Uani 1 d . . O(2) O 0.9962(15) 0.1201(6) 0.6645(11) 0.018(2) Uani 1 d . . O(3) O 0.4769(15) 0.1291(6) 0.6501(11) 0.016(2) Uani 1 d . . O(4) O 0.7594(17) 0.1814(6) 0.4089(11) 0.020(2) Uani 1 d . . O(6) O 0.4530(17) 0.0091(7) 1.1813(12) 0.027(2) Uani 1 d . . O(7) O 0.9448(16) 0.0344(7) 0.1671(13) 0.024(2) Uani 1 d . . O(5) O 0.2574(15) 0.1124(5) 0.9404(9) 0.010(2) Uani 1 d . . O(8) O 0.2557(18) 0.1582(6) 1.2437(11) 0.024(2) Uani 1 d . . 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 Cs 0.0209(5) 0.0161(5) 0.0259(5) 0.0033(3) -0.0014(4) -0.0006(3) Sb 0.0073(4) 0.0100(4) 0.0049(4) 0.0005(3) 0.0010(3) -0.0001(3) V(1) 0.0086(10) 0.0108(10) 0.0054(10) 0.0007(7) -0.0010(7) -0.0002(7) V(2) 0.0099(10) 0.0111(10) 0.0063(10) 0.0003(8) 0.0001(8) 0.0007(8) O(1) 0.010(4) 0.015(4) 0.011(4) -0.002(3) 0.000(3) 0.001(3) O(2) 0.012(4) 0.020(5) 0.021(5) -0.008(4) -0.006(4) 0.004(4) O(3) 0.012(4) 0.020(5) 0.016(5) 0.002(4) -0.004(4) -0.001(4) O(4) 0.027(5) 0.021(5) 0.011(4) 0.006(4) 0.001(4) -0.003(4) O(6) 0.013(5) 0.039(6) 0.029(6) 0.006(5) -0.004(4) 0.016(4) O(7) 0.009(4) 0.030(5) 0.033(6) -0.001(4) -0.001(4) -0.006(4) O(5) 0.014(4) 0.014(4) 0.004(4) -0.001(3) 0.001(3) -0.001(3) O(8) 0.028(5) 0.024(5) 0.019(5) -0.010(4) 0.003(4) -0.006(4) _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 Cs O(8) 3.017(10) 4_664 ? Cs O(3) 3.112(9) 4_665 ? Cs O(5) 3.214(8) 1_554 ? Cs O(4) 3.279(10) 4_565 ? Cs O(2) 3.295(10) 4_565 ? Cs O(5) 3.399(8) 1_654 ? Cs O(7) 3.412(11) . ? Cs O(4) 3.433(9) . ? Cs O(4) 3.481(10) 4_665 ? Cs O(8) 3.503(10) 1_554 ? Cs O(2) 3.558(9) 1_554 ? Cs O(3) 3.594(9) 1_554 ? Sb O(3) 1.932(9) . ? Sb O(7) 1.946(10) 3_656 ? Sb O(5) 1.948(8) . ? Sb O(2) 1.959(9) 1_455 ? Sb O(1) 1.962(8) 3_656 ? Sb O(6) 1.997(9) 3_657 ? Sb Cs 4.292(2) 4_566 ? Sb Cs 4.379(2) 1_556 ? Sb Cs 4.530(2) 1_456 ? V(1) O(4) 1.608(9) . ? V(1) O(1) 1.736(9) . ? V(1) O(2) 1.757(9) . ? V(1) O(3) 1.790(9) . ? V(1) O(6) 3.223(11) 3_657 ? V(1) Cs 3.991(2) 4_666 ? V(1) Cs 4.033(2) 4_566 ? V(1) Cs 4.245(3) 1_556 ? V(2) O(8) 1.598(10) . ? V(2) O(6) 1.696(9) . ? V(2) O(7) 1.760(9) 1_456 ? V(2) O(5) 1.773(8) . ? V(2) O(7) 3.278(11) 3_656 ? V(2) Cs 3.723(2) 1_456 ? V(2) Cs 3.802(2) 1_556 ? O(1) Sb 1.962(8) 3_656 ? O(1) O(7) 2.729(14) . ? O(1) O(3) 2.752(12) 3_656 ? O(1) O(4) 2.781(13) . ? O(1) O(2) 2.785(12) 3_756 ? O(1) O(2) 2.833(12) . ? O(1) O(6) 2.847(13) 1_554 ? O(1) O(1) 2.87(2) 3_656 ? O(1) O(3) 2.914(13) . ? O(1) O(1) 2.97(2) 3_756 ? O(1) O(6) 3.241(13) 3_657 ? O(2) Sb 1.959(9) 1_655 ? O(2) O(4) 2.709(13) . ? O(2) O(3) 2.712(12) 1_655 ? O(2) O(5) 2.740(12) 1_655 ? O(2) O(1) 2.785(12) 3_756 ? O(2) O(7) 2.889(15) 3_756 ? O(2) O(3) 2.927(12) . ? O(2) Cs 3.295(10) 4_666 ? O(2) Cs 3.558(9) 1_556 ? O(3) O(6) 2.674(14) 3_657 ? O(3) O(2) 2.712(12) 1_455 ? O(3) O(4) 2.717(13) . ? O(3) O(1) 2.752(12) 3_656 ? O(3) O(5) 2.752(12) . ? O(3) Cs 3.112(9) 4_566 ? O(3) Cs 3.594(9) 1_556 ? O(4) O(8) 3.148(14) 1_654 ? O(4) O(8) 3.171(14) 1_554 ? O(4) Cs 3.279(10) 4_666 ? O(4) O(7) 3.301(14) . ? O(4) O(5) 3.346(13) 4_665 ? O(4) Cs 3.481(10) 4_566 ? O(6) Sb 1.997(9) 3_657 ? O(6) O(3) 2.674(14) 3_657 ? O(6) O(8) 2.708(15) . ? O(6) O(5) 2.752(13) 3_657 ? O(6) O(7) 2.801(13) 1_556 ? O(6) O(5) 2.842(13) . ? O(6) O(1) 2.847(13) 1_556 ? O(6) O(7) 2.891(13) 1_456 ? O(6) O(6) 3.11(2) 3_657 ? O(6) V(1) 3.223(11) 3_657 ? O(6) O(1) 3.241(13) 3_657 ? O(7) V(2) 1.760(9) 1_654 ? O(7) Sb 1.946(10) 3_656 ? O(7) O(8) 2.734(14) 1_654 ? O(7) O(5) 2.781(13) 3_656 ? O(7) O(6) 2.801(13) 1_554 ? O(7) O(5) 2.889(13) 1_654 ? O(7) O(2) 2.889(15) 3_756 ? O(7) O(6) 2.891(13) 1_654 ? O(7) O(7) 3.09(2) 3_755 ? O(7) V(2) 3.278(11) 3_656 ? O(5) O(8) 2.654(12) . ? O(5) O(2) 2.740(12) 1_455 ? O(5) O(6) 2.752(13) 3_657 ? O(5) O(7) 2.781(13) 3_656 ? O(5) O(7) 2.889(13) 1_456 ? O(5) Cs 3.214(8) 1_556 ? O(5) O(4) 3.346(13) 4_566 ? O(5) Cs 3.399(8) 1_456 ? O(8) O(7) 2.734(14) 1_456 ? O(8) Cs 3.017(10) 4_567 ? O(8) O(4) 3.148(14) 1_456 ? O(8) O(4) 3.171(14) 1_556 ? O(8) Cs 3.503(10) 1_556 ? O(8) Cs 3.638(11) 1_456 ? 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 O(8) Cs O(3) 73.3(3) 4_664 4_665 ? O(8) Cs O(5) 104.9(3) 4_664 1_554 ? O(3) Cs O(5) 147.7(2) 4_665 1_554 ? O(8) Cs O(4) 59.8(3) 4_664 4_565 ? O(3) Cs O(4) 91.7(2) 4_665 4_565 ? O(5) Cs O(4) 62.0(2) 1_554 4_565 ? O(8) Cs O(2) 75.8(3) 4_664 4_565 ? O(3) Cs O(2) 50.0(2) 4_665 4_565 ? O(5) Cs O(2) 97.8(2) 1_554 4_565 ? O(4) Cs O(2) 48.7(2) 4_565 4_565 ? O(8) Cs O(5) 100.6(2) 4_664 1_654 ? O(3) Cs O(5) 95.1(2) 4_665 1_654 ? O(5) Cs O(5) 116.6(2) 1_554 1_654 ? O(4) Cs O(5) 156.3(2) 4_565 1_654 ? O(2) Cs O(5) 144.8(2) 4_565 1_654 ? O(8) Cs O(7) 149.5(3) 4_664 . ? O(3) Cs O(7) 113.2(2) 4_665 . ? O(5) Cs O(7) 85.1(2) 1_554 . ? O(4) Cs O(7) 144.6(2) 4_565 . ? O(2) Cs O(7) 132.3(2) 4_565 . ? O(5) Cs O(7) 50.2(2) 1_654 . ? O(8) Cs O(4) 145.5(3) 4_664 . ? O(3) Cs O(4) 74.2(2) 4_665 . ? O(5) Cs O(4) 96.5(2) 1_554 . ? O(4) Cs O(4) 110.3(3) 4_565 . ? O(2) Cs O(4) 74.7(2) 4_565 . ? O(5) Cs O(4) 93.4(2) 1_654 . ? O(7) Cs O(4) 57.7(2) . . ? O(8) Cs O(4) 57.9(3) 4_664 4_665 ? O(3) Cs O(4) 48.3(2) 4_665 4_665 ? O(5) Cs O(4) 156.7(2) 1_554 4_665 ? O(4) Cs O(4) 112.7(3) 4_565 4_665 ? O(2) Cs O(4) 92.9(2) 4_565 4_665 ? O(5) Cs O(4) 58.2(2) 1_654 4_665 ? O(7) Cs O(4) 102.8(2) . 4_665 ? O(4) Cs O(4) 106.3(3) . 4_665 ? O(8) Cs O(8) 128.4(3) 4_664 1_554 ? O(3) Cs O(8) 108.7(2) 4_665 1_554 ? O(5) Cs O(8) 46.3(2) 1_554 1_554 ? O(4) Cs O(8) 68.6(2) 4_565 1_554 ? O(2) Cs O(8) 69.8(2) 4_565 1_554 ? O(5) Cs O(8) 129.5(2) 1_654 1_554 ? O(7) Cs O(8) 79.3(2) . 1_554 ? O(4) Cs O(8) 54.4(2) . 1_554 ? O(4) Cs O(8) 156.2(2) 4_665 1_554 ? O(8) Cs O(2) 72.1(3) 4_664 1_554 ? O(3) Cs O(2) 119.1(2) 4_665 1_554 ? O(5) Cs O(2) 89.5(2) 1_554 1_554 ? O(4) Cs O(2) 111.1(2) 4_565 1_554 ? O(2) Cs O(2) 147.8(2) 4_565 1_554 ? O(5) Cs O(2) 46.3(2) 1_654 1_554 ? O(7) Cs O(2) 79.4(2) . 1_554 ? O(4) Cs O(2) 135.8(2) . 1_554 ? O(4) Cs O(2) 70.9(2) 4_665 1_554 ? O(8) Cs O(2) 132.0(2) 1_554 1_554 ? O(8) Cs O(3) 70.8(3) 4_664 1_554 ? O(3) Cs O(3) 144.1(2) 4_665 1_554 ? O(5) Cs O(3) 47.3(2) 1_554 1_554 ? O(4) Cs O(3) 70.1(2) 4_565 1_554 ? O(2) Cs O(3) 118.7(2) 4_565 1_554 ? O(5) Cs O(3) 91.7(2) 1_654 1_554 ? O(7) Cs O(3) 98.1(2) . 1_554 ? O(4) Cs O(3) 140.6(2) . 1_554 ? O(4) Cs O(3) 109.5(2) 4_665 1_554 ? O(8) Cs O(3) 93.4(2) 1_554 1_554 ? O(2) Cs O(3) 48.3(2) 1_554 1_554 ? O(3) Sb O(7) 175.9(4) . 3_656 ? O(3) Sb O(5) 90.4(4) . . ? O(7) Sb O(5) 91.1(4) 3_656 . ? O(3) Sb O(2) 88.4(4) . 1_455 ? O(7) Sb O(2) 95.4(4) 3_656 1_455 ? O(5) Sb O(2) 89.1(4) . 1_455 ? O(3) Sb O(1) 89.9(4) . 3_656 ? O(7) Sb O(1) 88.6(4) 3_656 3_656 ? O(5) Sb O(1) 179.5(3) . 3_656 ? O(2) Sb O(1) 90.5(4) 1_455 3_656 ? O(3) Sb O(6) 85.8(4) . 3_657 ? O(7) Sb O(6) 90.5(4) 3_656 3_657 ? O(5) Sb O(6) 88.5(4) . 3_657 ? O(2) Sb O(6) 173.6(4) 1_455 3_657 ? O(1) Sb O(6) 92.0(4) 3_656 3_657 ? O(3) Sb Cs 41.2(3) . 4_566 ? O(7) Sb Cs 142.7(3) 3_656 4_566 ? O(5) Sb Cs 86.6(2) . 4_566 ? O(2) Sb Cs 47.3(3) 1_455 4_566 ? O(1) Sb Cs 93.3(3) 3_656 4_566 ? O(6) Sb Cs 126.6(3) 3_657 4_566 ? O(3) Sb Cs 53.8(3) . 1_556 ? O(7) Sb Cs 126.0(3) 3_656 1_556 ? O(5) Sb Cs 42.2(2) . 1_556 ? O(2) Sb Cs 106.3(3) 1_455 1_556 ? O(1) Sb Cs 138.3(2) 3_656 1_556 ? O(6) Sb Cs 68.1(3) 3_657 1_556 ? Cs Sb Cs 73.26(3) 4_566 1_556 ? O(3) Sb Cs 103.0(3) . 1_456 ? O(7) Sb Cs 80.7(3) 3_656 1_456 ? O(5) Sb Cs 43.7(2) . 1_456 ? O(2) Sb Cs 48.7(3) 1_455 1_456 ? O(1) Sb Cs 135.8(2) 3_656 1_456 ? O(6) Sb Cs 130.5(3) 3_657 1_456 ? Cs Sb Cs 72.14(3) 4_566 1_456 ? Cs Sb Cs 78.31(3) 1_556 1_456 ? O(4) V(1) O(1) 112.5(5) . . ? O(4) V(1) O(2) 107.2(5) . . ? O(1) V(1) O(2) 108.4(4) . . ? O(4) V(1) O(3) 106.0(5) . . ? O(1) V(1) O(3) 111.4(4) . . ? O(2) V(1) O(3) 111.2(4) . . ? O(4) V(1) O(6) 161.7(4) . 3_657 ? O(1) V(1) O(6) 75.0(3) . 3_657 ? O(2) V(1) O(6) 84.9(4) . 3_657 ? O(3) V(1) O(6) 56.1(3) . 3_657 ? O(4) V(1) Cs 52.8(3) . 4_666 ? O(1) V(1) Cs 128.3(3) . 4_666 ? O(2) V(1) Cs 54.4(3) . 4_666 ? O(3) V(1) Cs 120.2(3) . 4_666 ? O(6) V(1) Cs 136.4(2) 3_657 4_666 ? O(4) V(1) Cs 58.7(4) . 4_566 ? O(1) V(1) Cs 128.3(3) . 4_566 ? O(2) V(1) Cs 123.1(3) . 4_566 ? O(3) V(1) Cs 47.3(3) . 4_566 ? O(6) V(1) Cs 103.3(2) 3_657 4_566 ? Cs V(1) Cs 89.06(5) 4_666 4_566 ? O(4) V(1) Cs 110.6(4) . 1_556 ? O(1) V(1) Cs 136.9(3) . 1_556 ? O(2) V(1) Cs 55.5(3) . 1_556 ? O(3) V(1) Cs 56.9(3) . 1_556 ? O(6) V(1) Cs 64.5(2) 3_657 1_556 ? Cs V(1) Cs 78.21(5) 4_666 1_556 ? Cs V(1) Cs 77.32(5) 4_566 1_556 ? O(8) V(2) O(6) 110.6(6) . . ? O(8) V(2) O(7) 108.9(5) . 1_456 ? O(6) V(2) O(7) 113.5(5) . 1_456 ? O(8) V(2) O(5) 103.7(5) . . ? O(6) V(2) O(5) 110.0(5) . . ? O(7) V(2) O(5) 109.7(5) 1_456 . ? O(8) V(2) O(7) 155.6(4) . 3_656 ? O(6) V(2) O(7) 92.0(4) . 3_656 ? O(7) V(2) O(7) 68.0(5) 1_456 3_656 ? O(5) V(2) O(7) 58.0(3) . 3_656 ? O(8) V(2) Cs 74.5(4) . 1_456 ? O(6) V(2) Cs 174.3(4) . 1_456 ? O(7) V(2) Cs 66.1(4) 1_456 1_456 ? O(5) V(2) Cs 65.6(3) . 1_456 ? O(7) V(2) Cs 82.6(2) 3_656 1_456 ? O(8) V(2) Cs 67.0(4) . 1_556 ? O(6) V(2) Cs 83.2(4) . 1_556 ? O(7) V(2) Cs 162.6(4) 1_456 1_556 ? O(5) V(2) Cs 57.4(3) . 1_556 ? O(7) V(2) Cs 108.2(2) 3_656 1_556 ? Cs V(2) Cs 96.79(6) 1_456 1_556 ? V(1) O(1) Sb 144.3(5) . 3_656 ? V(1) O(1) O(7) 103.7(4) . . ? Sb O(1) O(7) 45.5(3) 3_656 . ? V(1) O(1) O(3) 152.8(5) . 3_656 ? Sb O(1) O(3) 44.6(3) 3_656 3_656 ? O(7) O(1) O(3) 90.0(4) . 3_656 ? V(1) O(1) O(4) 32.3(3) . . ? Sb O(1) O(4) 112.1(4) 3_656 . ? O(7) O(1) O(4) 73.6(4) . . ? O(3) O(1) O(4) 141.3(4) 3_656 . ? V(1) O(1) O(2) 148.5(5) . 3_756 ? Sb O(1) O(2) 44.7(3) 3_656 3_756 ? O(7) O(1) O(2) 63.2(4) . 3_756 ? O(3) O(1) O(2) 58.7(3) 3_656 3_756 ? O(4) O(1) O(2) 133.1(4) . 3_756 ? V(1) O(1) O(2) 36.0(3) . . ? Sb O(1) O(2) 147.3(4) 3_656 . ? O(7) O(1) O(2) 104.9(4) . . ? O(3) O(1) O(2) 160.0(4) 3_656 . ? O(4) O(1) O(2) 57.7(3) . . ? O(2) O(1) O(2) 116.2(3) 3_756 . ? V(1) O(1) O(6) 109.7(4) . 1_554 ? Sb O(1) O(6) 44.5(3) 3_656 1_554 ? O(7) O(1) O(6) 60.3(3) . 1_554 ? O(3) O(1) O(6) 57.0(3) 3_656 1_554 ? O(4) O(1) O(6) 84.7(4) . 1_554 ? O(2) O(1) O(6) 89.1(4) 3_756 1_554 ? O(2) O(1) O(6) 142.4(4) . 1_554 ? V(1) O(1) O(1) 91.2(4) . 3_656 ? Sb O(1) O(1) 97.8(4) 3_656 3_656 ? O(7) O(1) O(1) 129.3(5) . 3_656 ? O(3) O(1) O(1) 62.4(4) 3_656 3_656 ? O(4) O(1) O(1) 101.2(5) . 3_656 ? O(2) O(1) O(1) 119.6(5) 3_756 3_656 ? O(2) O(1) O(1) 114.4(5) . 3_656 ? O(6) O(1) O(1) 69.1(4) 1_554 3_656 ? V(1) O(1) O(3) 34.9(2) . . ? Sb O(1) O(3) 143.7(4) 3_656 . ? O(7) O(1) O(3) 128.6(4) . . ? O(3) O(1) O(3) 119.2(3) 3_656 . ? O(4) O(1) O(3) 56.9(3) . . ? O(2) O(1) O(3) 167.9(4) 3_756 . ? O(2) O(1) O(3) 61.2(3) . . ? O(6) O(1) O(3) 99.4(4) 1_554 . ? O(1) O(1) O(3) 56.8(3) 3_656 . ? V(1) O(1) O(1) 91.6(4) . 3_756 ? Sb O(1) O(1) 97.9(4) 3_656 3_756 ? O(7) O(1) O(1) 79.8(4) . 3_756 ? O(3) O(1) O(1) 114.1(5) 3_656 3_756 ? O(4) O(1) O(1) 97.5(4) . 3_756 ? O(2) O(1) O(1) 58.9(3) 3_756 3_756 ? O(2) O(1) O(1) 57.3(3) . 3_756 ? O(6) O(1) O(1) 137.7(5) 1_554 3_756 ? O(1) O(1) O(1) 148.9(6) 3_656 3_756 ? O(3) O(1) O(1) 117.2(5) . 3_756 ? V(1) O(1) O(6) 73.8(3) . 3_657 ? Sb O(1) O(6) 138.2(4) 3_656 3_657 ? O(7) O(1) O(6) 175.3(4) . 3_657 ? O(3) O(1) O(6) 93.9(4) 3_656 3_657 ? O(4) O(1) O(6) 104.7(4) . 3_657 ? O(2) O(1) O(6) 116.9(4) 3_756 3_657 ? O(2) O(1) O(6) 70.7(3) . 3_657 ? O(6) O(1) O(6) 124.2(3) 1_554 3_657 ? O(1) O(1) O(6) 55.1(3) 3_656 3_657 ? O(3) O(1) O(6) 51.2(3) . 3_657 ? O(1) O(1) O(6) 96.2(4) 3_756 3_657 ? V(1) O(2) Sb 138.0(5) . 1_655 ? V(1) O(2) O(4) 34.5(3) . . ? Sb O(2) O(4) 146.8(5) 1_655 . ? V(1) O(2) O(3) 141.3(5) . 1_655 ? Sb O(2) O(3) 45.4(3) 1_655 1_655 ? O(4) O(2) O(3) 115.6(5) . 1_655 ? V(1) O(2) O(5) 157.0(5) . 1_655 ? Sb O(2) O(5) 45.3(3) 1_655 1_655 ? O(4) O(2) O(5) 161.1(5) . 1_655 ? O(3) O(2) O(5) 60.6(3) 1_655 1_655 ? V(1) O(2) O(1) 97.6(4) . 3_756 ? Sb O(2) O(1) 44.8(3) 1_655 3_756 ? O(4) O(2) O(1) 103.9(4) . 3_756 ? O(3) O(2) O(1) 60.1(3) 1_655 3_756 ? O(5) O(2) O(1) 90.1(4) 1_655 3_756 ? V(1) O(2) O(1) 35.5(3) . . ? Sb O(2) O(1) 102.5(4) 1_655 . ? O(4) O(2) O(1) 60.2(3) . . ? O(3) O(2) O(1) 120.1(4) 1_655 . ? O(5) O(2) O(1) 138.6(4) 1_655 . ? O(1) O(2) O(1) 63.8(3) 3_756 . ? V(1) O(2) O(7) 107.3(5) . 3_756 ? Sb O(2) O(7) 42.1(3) 1_655 3_756 ? O(4) O(2) O(7) 139.4(4) . 3_756 ? O(3) O(2) O(7) 87.5(4) 1_655 3_756 ? O(5) O(2) O(7) 59.1(3) 1_655 3_756 ? O(1) O(2) O(7) 57.5(3) 3_756 3_756 ? O(1) O(2) O(7) 79.5(4) . 3_756 ? V(1) O(2) O(3) 34.8(3) . . ? Sb O(2) O(3) 142.2(5) 1_655 . ? O(4) O(2) O(3) 57.5(3) . . ? O(3) O(2) O(3) 172.3(5) 1_655 . ? O(5) O(2) O(3) 124.6(4) 1_655 . ? O(1) O(2) O(3) 123.1(4) 3_756 . ? O(1) O(2) O(3) 60.7(3) . . ? O(7) O(2) O(3) 100.1(4) 3_756 . ? V(1) O(2) Cs 99.9(4) . 4_666 ? Sb O(2) Cs 106.8(3) 1_655 4_666 ? O(4) O(2) Cs 65.4(3) . 4_666 ? O(3) O(2) Cs 61.5(3) 1_655 4_666 ? O(5) O(2) Cs 99.1(3) 1_655 4_666 ? O(1) O(2) Cs 104.6(3) 3_756 4_666 ? O(1) O(2) Cs 117.6(4) . 4_666 ? O(7) O(2) Cs 148.8(4) 3_756 4_666 ? O(3) O(2) Cs 111.0(3) . 4_666 ? V(1) O(2) Cs 100.5(4) . 1_556 ? Sb O(2) Cs 106.8(4) 1_655 1_556 ? O(4) O(2) Cs 106.3(3) . 1_556 ? O(3) O(2) Cs 115.0(3) 1_655 1_556 ? O(5) O(2) Cs 63.8(3) 1_655 1_556 ? O(1) O(2) Cs 147.5(4) 3_756 1_556 ? O(1) O(2) Cs 123.4(3) . 1_556 ? O(7) O(2) Cs 91.3(3) 3_756 1_556 ? O(3) O(2) Cs 66.5(3) . 1_556 ? Cs O(2) Cs 98.6(2) 4_666 1_556 ? V(1) O(3) Sb 128.9(5) . . ? V(1) O(3) O(6) 90.2(4) . 3_657 ? Sb O(3) O(6) 48.1(3) . 3_657 ? V(1) O(3) O(2) 148.7(5) . 1_455 ? Sb O(3) O(2) 46.2(3) . 1_455 ? O(6) O(3) O(2) 94.3(4) 3_657 1_455 ? V(1) O(3) O(4) 34.7(3) . . ? Sb O(3) O(4) 151.4(5) . . ? O(6) O(3) O(4) 124.7(4) 3_657 . ? O(2) O(3) O(4) 129.6(4) 1_455 . ? V(1) O(3) O(1) 93.9(4) . 3_656 ? Sb O(3) O(1) 45.5(3) . 3_656 ? O(6) O(3) O(1) 63.3(4) 3_657 3_656 ? O(2) O(3) O(1) 61.3(3) 1_455 3_656 ? O(4) O(3) O(1) 106.0(4) . 3_656 ? V(1) O(3) O(5) 144.7(5) . . ? Sb O(3) O(5) 45.0(3) . . ? O(6) O(3) O(5) 60.9(3) 3_657 . ? O(2) O(3) O(5) 60.2(3) 1_455 . ? O(4) O(3) O(5) 163.4(5) . . ? O(1) O(3) O(5) 90.5(4) 3_656 . ? V(1) O(3) O(1) 33.7(2) . . ? Sb O(3) O(1) 97.0(4) . . ? O(6) O(3) O(1) 70.8(4) 3_657 . ? O(2) O(3) O(1) 120.6(4) 1_455 . ? O(4) O(3) O(1) 59.1(3) . . ? O(1) O(3) O(1) 60.8(3) 3_656 . ? O(5) O(3) O(1) 131.2(4) . . ? V(1) O(3) O(2) 34.0(3) . . ? Sb O(3) O(2) 126.1(4) . . ? O(6) O(3) O(2) 78.0(4) 3_657 . ? O(2) O(3) O(2) 172.3(5) 1_455 . ? O(4) O(3) O(2) 57.2(3) . . ? O(1) O(3) O(2) 115.0(4) 3_656 . ? O(5) O(3) O(2) 114.3(4) . . ? O(1) O(3) O(2) 58.0(3) . . ? V(1) O(3) Cs 107.6(4) . 4_566 ? Sb O(3) Cs 114.6(4) . 4_566 ? O(6) O(3) Cs 161.8(4) 3_657 4_566 ? O(2) O(3) Cs 68.5(3) 1_455 4_566 ? O(4) O(3) Cs 73.0(3) . 4_566 ? O(1) O(3) Cs 110.5(3) 3_656 4_566 ? O(5) O(3) Cs 103.4(3) . 4_566 ? O(1) O(3) Cs 122.7(3) . 4_566 ? O(2) O(3) Cs 119.0(3) . 4_566 ? V(1) O(3) Cs 98.5(3) . 1_556 ? Sb O(3) Cs 100.5(3) . 1_556 ? O(6) O(3) Cs 79.8(3) 3_657 1_556 ? O(2) O(3) Cs 112.8(3) 1_455 1_556 ? O(4) O(3) Cs 105.1(3) . 1_556 ? O(1) O(3) Cs 141.0(4) 3_656 1_556 ? O(5) O(3) Cs 59.1(2) . 1_556 ? O(1) O(3) Cs 119.7(3) . 1_556 ? O(2) O(3) Cs 65.2(2) . 1_556 ? Cs O(3) Cs 100.7(2) 4_566 1_556 ? V(1) O(4) O(2) 38.3(3) . . ? V(1) O(4) O(3) 39.3(3) . . ? O(2) O(4) O(3) 65.3(3) . . ? V(1) O(4) O(1) 35.2(3) . . ? O(2) O(4) O(1) 62.1(3) . . ? O(3) O(4) O(1) 64.0(3) . . ? V(1) O(4) O(8) 105.7(5) . 1_654 ? O(2) O(4) O(8) 82.6(4) . 1_654 ? O(3) O(4) O(8) 144.6(4) . 1_654 ? O(1) O(4) O(8) 88.6(4) . 1_654 ? V(1) O(4) O(8) 99.6(5) . 1_554 ? O(2) O(4) O(8) 137.6(4) . 1_554 ? O(3) O(4) O(8) 76.4(3) . 1_554 ? O(1) O(4) O(8) 85.6(4) . 1_554 ? O(8) O(4) O(8) 125.9(4) 1_654 1_554 ? V(1) O(4) Cs 104.2(4) . 4_666 ? O(2) O(4) Cs 66.0(3) . 4_666 ? O(3) O(4) Cs 117.4(4) . 4_666 ? O(1) O(4) Cs 119.7(4) . 4_666 ? O(8) O(4) Cs 55.9(2) 1_654 4_666 ? O(8) O(4) Cs 154.3(4) 1_554 4_666 ? V(1) O(4) O(7) 85.8(4) . . ? O(2) O(4) O(7) 93.9(4) . . ? O(3) O(4) O(7) 115.0(4) . . ? O(1) O(4) O(7) 52.5(3) . . ? O(8) O(4) O(7) 50.1(3) 1_654 . ? O(8) O(4) O(7) 86.0(3) 1_554 . ? Cs O(4) O(7) 105.1(3) 4_666 . ? V(1) O(4) O(5) 131.4(5) . 4_665 ? O(2) O(4) O(5) 107.7(4) . 4_665 ? O(3) O(4) O(5) 104.4(4) . 4_665 ? O(1) O(4) O(5) 166.6(4) . 4_665 ? O(8) O(4) O(5) 99.0(3) 1_654 4_665 ? O(8) O(4) O(5) 98.6(3) 1_554 4_665 ? Cs O(4) O(5) 58.0(2) 4_666 4_665 ? O(7) O(4) O(5) 140.2(4) . 4_665 ? V(1) O(4) Cs 142.5(5) . . ? O(2) O(4) Cs 148.6(4) . . ? O(3) O(4) Cs 140.1(4) . . ? O(1) O(4) Cs 107.5(3) . . ? O(8) O(4) Cs 67.0(3) 1_654 . ? O(8) O(4) Cs 63.9(2) 1_554 . ? Cs O(4) Cs 100.8(2) 4_666 . ? O(7) O(4) Cs 60.8(2) . . ? O(5) O(4) Cs 85.6(2) 4_665 . ? V(1) O(4) Cs 98.0(4) . 4_566 ? O(2) O(4) Cs 113.9(4) . 4_566 ? O(3) O(4) Cs 58.7(3) . 4_566 ? O(1) O(4) Cs 114.7(3) . 4_566 ? O(8) O(4) Cs 155.6(4) 1_654 4_566 ? O(8) O(4) Cs 53.7(2) 1_554 4_566 ? Cs O(4) Cs 112.7(3) 4_666 4_566 ? O(7) O(4) Cs 139.6(3) . 4_566 ? O(5) O(4) Cs 59.7(2) 4_665 4_566 ? Cs O(4) Cs 97.5(2) . 4_566 ? V(2) O(6) Sb 168.0(7) . 3_657 ? V(2) O(6) O(3) 139.0(6) . 3_657 ? Sb O(6) O(3) 46.1(3) 3_657 3_657 ? V(2) O(6) O(8) 33.5(3) . . ? Sb O(6) O(8) 134.6(5) 3_657 . ? O(3) O(6) O(8) 134.6(5) 3_657 . ? V(2) O(6) O(5) 144.8(6) . 3_657 ? Sb O(6) O(5) 45.0(3) 3_657 3_657 ? O(3) O(6) O(5) 60.9(3) 3_657 3_657 ? O(8) O(6) O(5) 162.1(5) . 3_657 ? V(2) O(6) O(7) 128.8(6) . 1_556 ? Sb O(6) O(7) 44.0(3) 3_657 1_556 ? O(3) O(6) O(7) 90.1(4) 3_657 1_556 ? O(8) O(6) O(7) 106.5(5) . 1_556 ? O(5) O(6) O(7) 60.1(3) 3_657 1_556 ? V(2) O(6) O(5) 35.9(3) . . ? Sb O(6) O(5) 145.8(5) 3_657 . ? O(3) O(6) O(5) 157.5(5) 3_657 . ? O(8) O(6) O(5) 57.1(3) . . ? O(5) O(6) O(5) 112.5(4) 3_657 . ? O(7) O(6) O(5) 105.2(4) 1_556 . ? V(2) O(6) O(1) 125.9(6) . 1_556 ? Sb O(6) O(1) 43.5(3) 3_657 1_556 ? O(3) O(6) O(1) 59.7(3) 3_657 1_556 ? O(8) O(6) O(1) 93.7(4) . 1_556 ? O(5) O(6) O(1) 88.5(4) 3_657 1_556 ? O(7) O(6) O(1) 57.8(3) 1_556 1_556 ? O(5) O(6) O(1) 142.6(5) . 1_556 ? V(2) O(6) O(7) 33.9(3) . 1_456 ? Sb O(6) O(7) 152.4(6) 3_657 1_456 ? O(3) O(6) O(7) 106.5(5) 3_657 1_456 ? O(8) O(6) O(7) 58.4(3) . 1_456 ? O(5) O(6) O(7) 132.3(5) 3_657 1_456 ? O(7) O(6) O(7) 162.8(6) 1_556 1_456 ? O(5) O(6) O(7) 60.5(3) . 1_456 ? O(1) O(6) O(7) 126.7(5) 1_556 1_456 ? V(2) O(6) O(6) 89.0(5) . 3_657 ? Sb O(6) O(6) 97.5(5) 3_657 3_657 ? O(3) O(6) O(6) 114.5(6) 3_657 3_657 ? O(8) O(6) O(6) 110.2(5) . 3_657 ? O(5) O(6) O(6) 57.6(4) 3_657 3_657 ? O(7) O(6) O(6) 78.4(4) 1_556 3_657 ? O(5) O(6) O(6) 54.9(3) . 3_657 ? O(1) O(6) O(6) 134.8(5) 1_556 3_657 ? O(7) O(6) O(6) 98.4(5) 1_456 3_657 ? V(2) O(6) V(1) 106.2(4) . 3_657 ? Sb O(6) V(1) 76.1(3) 3_657 3_657 ? O(3) O(6) V(1) 33.7(2) 3_657 3_657 ? O(8) O(6) V(1) 104.5(4) . 3_657 ? O(5) O(6) V(1) 92.8(3) 3_657 3_657 ? O(7) O(6) V(1) 117.5(4) 1_556 3_657 ? O(5) O(6) V(1) 137.1(4) . 3_657 ? O(1) O(6) V(1) 67.4(3) 1_556 3_657 ? O(7) O(6) V(1) 76.7(3) 1_456 3_657 ? O(6) O(6) V(1) 135.4(6) 3_657 3_657 ? V(2) O(6) O(1) 90.3(4) . 3_657 ? Sb O(6) O(1) 86.0(4) 3_657 3_657 ? O(3) O(6) O(1) 58.1(3) 3_657 3_657 ? O(8) O(6) O(1) 76.6(4) . 3_657 ? O(5) O(6) O(1) 118.7(4) 3_657 3_657 ? O(7) O(6) O(1) 113.5(4) 1_556 3_657 ? O(5) O(6) O(1) 126.2(4) . 3_657 ? O(1) O(6) O(1) 55.8(3) 1_556 3_657 ? O(7) O(6) O(1) 73.0(3) 1_456 3_657 ? O(6) O(6) O(1) 164.7(6) 3_657 3_657 ? V(1) O(6) O(1) 31.2(2) 3_657 3_657 ? V(2) O(7) Sb 149.5(6) 1_654 3_656 ? V(2) O(7) O(1) 123.6(5) 1_654 . ? Sb O(7) O(1) 46.0(3) 3_656 . ? V(2) O(7) O(8) 33.6(3) 1_654 1_654 ? Sb O(7) O(8) 143.1(5) 3_656 1_654 ? O(1) O(7) O(8) 98.8(4) . 1_654 ? V(2) O(7) O(5) 131.0(5) 1_654 3_656 ? Sb O(7) O(5) 44.4(3) 3_656 3_656 ? O(1) O(7) O(5) 90.4(4) . 3_656 ? O(8) O(7) O(5) 164.2(5) 1_654 3_656 ? V(2) O(7) O(6) 164.7(6) 1_654 1_554 ? Sb O(7) O(6) 45.5(3) 3_656 1_554 ? O(1) O(7) O(6) 62.0(3) . 1_554 ? O(8) O(7) O(6) 136.7(5) 1_654 1_554 ? O(5) O(7) O(6) 59.1(3) 3_656 1_554 ? V(2) O(7) O(5) 35.3(3) 1_654 1_654 ? Sb O(7) O(5) 158.2(5) 3_656 1_654 ? O(1) O(7) O(5) 155.0(5) . 1_654 ? O(8) O(7) O(5) 56.2(3) 1_654 1_654 ? O(5) O(7) O(5) 114.1(4) 3_656 1_654 ? O(6) O(7) O(5) 134.2(5) 1_554 1_654 ? V(2) O(7) O(2) 107.2(5) 1_654 3_756 ? Sb O(7) O(2) 42.5(3) 3_656 3_756 ? O(1) O(7) O(2) 59.3(3) . 3_756 ? O(8) O(7) O(2) 116.5(4) 1_654 3_756 ? O(5) O(7) O(2) 57.8(3) 3_656 3_756 ? O(6) O(7) O(2) 87.9(4) 1_554 3_756 ? O(5) O(7) O(2) 129.2(4) 1_654 3_756 ? V(2) O(7) O(6) 32.5(3) 1_654 1_654 ? Sb O(7) O(6) 117.7(5) 3_656 1_654 ? O(1) O(7) O(6) 110.9(4) . 1_654 ? O(8) O(7) O(6) 57.5(4) 1_654 1_654 ? O(5) O(7) O(6) 107.2(4) 3_656 1_654 ? O(6) O(7) O(6) 162.8(6) 1_554 1_654 ? O(5) O(7) O(6) 58.9(3) 1_654 1_654 ? O(2) O(7) O(6) 75.3(4) 3_756 1_654 ? V(2) O(7) O(7) 80.1(4) 1_654 3_755 ? Sb O(7) O(7) 103.1(5) 3_656 3_755 ? O(1) O(7) O(7) 148.8(6) . 3_755 ? O(8) O(7) O(7) 110.3(5) 1_654 3_755 ? O(5) O(7) O(7) 58.7(4) 3_656 3_755 ? O(6) O(7) O(7) 100.9(5) 1_554 3_755 ? O(5) O(7) O(7) 55.4(3) 1_654 3_755 ? O(2) O(7) O(7) 96.3(5) 3_756 3_755 ? O(6) O(7) O(7) 77.5(4) 1_654 3_755 ? V(2) O(7) V(2) 112.0(5) 1_654 3_656 ? Sb O(7) V(2) 75.5(3) 3_656 3_656 ? O(1) O(7) V(2) 120.5(4) . 3_656 ? O(8) O(7) V(2) 140.7(4) 1_654 3_656 ? O(5) O(7) V(2) 32.7(2) 3_656 3_656 ? O(6) O(7) V(2) 70.2(3) 1_554 3_656 ? O(5) O(7) V(2) 84.4(3) 1_654 3_656 ? O(2) O(7) V(2) 86.8(3) 3_756 3_656 ? O(6) O(7) V(2) 104.4(4) 1_654 3_656 ? O(7) O(7) V(2) 31.9(2) 3_755 3_656 ? V(2) O(7) O(4) 95.6(4) 1_654 . ? Sb O(7) O(4) 94.5(4) 3_656 . ? O(1) O(7) O(4) 53.9(3) . . ? O(8) O(7) O(4) 62.0(3) 1_654 . ? O(5) O(7) O(4) 133.2(4) 3_656 . ? O(6) O(7) O(4) 76.3(4) 1_554 . ? O(5) O(7) O(4) 106.6(4) 1_654 . ? O(2) O(7) O(4) 111.0(4) 3_756 . ? O(6) O(7) O(4) 113.1(4) 1_654 . ? O(7) O(7) O(4) 152.3(6) 3_755 . ? V(2) O(7) O(4) 141.4(4) 3_656 . ? V(2) O(5) Sb 129.6(5) . . ? V(2) O(5) O(8) 35.8(3) . . ? Sb O(5) O(8) 165.4(5) . . ? V(2) O(5) O(2) 139.6(5) . 1_455 ? Sb O(5) O(2) 45.6(3) . 1_455 ? O(8) O(5) O(2) 142.6(4) . 1_455 ? V(2) O(5) O(3) 155.0(5) . . ? Sb O(5) O(3) 44.6(3) . . ? O(8) O(5) O(3) 145.8(4) . . ? O(2) O(5) O(3) 59.2(3) 1_455 . ? V(2) O(5) O(6) 99.7(4) . 3_657 ? Sb O(5) O(6) 46.5(3) . 3_657 ? O(8) O(5) O(6) 124.1(4) . 3_657 ? O(2) O(5) O(6) 92.0(4) 1_455 3_657 ? O(3) O(5) O(6) 58.1(3) . 3_657 ? V(2) O(5) O(7) 89.2(4) . 3_656 ? Sb O(5) O(7) 44.4(3) . 3_656 ? O(8) O(5) O(7) 123.1(4) . 3_656 ? O(2) O(5) O(7) 63.1(3) 1_455 3_656 ? O(3) O(5) O(7) 88.9(4) . 3_656 ? O(6) O(5) O(7) 60.8(3) 3_657 3_656 ? V(2) O(5) O(6) 34.1(3) . . ? Sb O(5) O(6) 107.9(4) . . ? O(8) O(5) O(6) 58.9(4) . . ? O(2) O(5) O(6) 146.4(4) 1_455 . ? O(3) O(5) O(6) 121.0(4) . . ? O(6) O(5) O(6) 67.5(4) 3_657 . ? O(7) O(5) O(6) 83.4(4) 3_656 . ? V(2) O(5) O(7) 35.0(3) . 1_456 ? Sb O(5) O(7) 110.2(4) . 1_456 ? O(8) O(5) O(7) 58.9(3) . 1_456 ? O(2) O(5) O(7) 104.6(4) 1_455 1_456 ? O(3) O(5) O(7) 154.8(4) . 1_456 ? O(6) O(5) O(7) 107.3(4) 3_657 1_456 ? O(7) O(5) O(7) 65.9(4) 3_656 1_456 ? O(6) O(5) O(7) 60.6(3) . 1_456 ? V(2) O(5) Cs 94.9(3) . 1_556 ? Sb O(5) Cs 113.8(3) . 1_556 ? O(8) O(5) Cs 72.6(3) . 1_556 ? O(2) O(5) Cs 124.6(3) 1_455 1_556 ? O(3) O(5) Cs 73.6(3) . 1_556 ? O(6) O(5) Cs 85.9(3) 3_657 1_556 ? O(7) O(5) Cs 146.7(4) 3_656 1_556 ? O(6) O(5) Cs 81.8(3) . 1_556 ? O(7) O(5) Cs 128.8(3) 1_456 1_556 ? V(2) O(5) O(4) 113.8(4) . 4_566 ? Sb O(5) O(4) 116.3(4) . 4_566 ? O(8) O(5) O(4) 78.3(3) . 4_566 ? O(2) O(5) O(4) 83.7(3) 1_455 4_566 ? O(3) O(5) O(4) 80.2(3) . 4_566 ? O(6) O(5) O(4) 132.8(4) 3_657 4_566 ? O(7) O(5) O(4) 145.8(4) 3_656 4_566 ? O(6) O(5) O(4) 129.9(4) . 4_566 ? O(7) O(5) O(4) 119.3(4) 1_456 4_566 ? Cs O(5) O(4) 59.9(2) 1_556 4_566 ? V(2) O(5) Cs 86.0(3) . 1_456 ? Sb O(5) Cs 113.0(3) . 1_456 ? O(8) O(5) Cs 72.7(3) . 1_456 ? O(2) O(5) Cs 69.9(3) 1_455 1_456 ? O(3) O(5) Cs 119.0(3) . 1_456 ? O(6) O(5) Cs 156.4(4) 3_657 1_456 ? O(7) O(5) Cs 96.6(3) 3_656 1_456 ? O(6) O(5) Cs 120.0(3) . 1_456 ? O(7) O(5) Cs 65.1(3) 1_456 1_456 ? Cs O(5) Cs 116.6(2) 1_556 1_456 ? O(4) O(5) Cs 62.1(2) 4_566 1_456 ? V(2) O(8) O(5) 40.5(3) . . ? V(2) O(8) O(6) 35.9(3) . . ? O(5) O(8) O(6) 64.0(4) . . ? V(2) O(8) O(7) 37.5(3) . 1_456 ? O(5) O(8) O(7) 64.8(4) . 1_456 ? O(6) O(8) O(7) 64.2(4) . 1_456 ? V(2) O(8) Cs 165.1(6) . 4_567 ? O(5) O(8) Cs 153.0(5) . 4_567 ? O(6) O(8) Cs 139.9(4) . 4_567 ? O(7) O(8) Cs 130.5(4) 1_456 4_567 ? V(2) O(8) O(4) 105.4(5) . 1_456 ? O(5) O(8) O(4) 117.7(4) . 1_456 ? O(6) O(8) O(4) 123.9(5) . 1_456 ? O(7) O(8) O(4) 67.9(4) 1_456 1_456 ? Cs O(8) O(4) 64.2(3) 4_567 1_456 ? V(2) O(8) O(4) 114.7(5) . 1_556 ? O(5) O(8) O(4) 116.5(4) . 1_556 ? O(6) O(8) O(4) 79.9(4) . 1_556 ? O(7) O(8) O(4) 139.4(5) 1_456 1_556 ? Cs O(8) O(4) 68.4(3) 4_567 1_556 ? O(4) O(8) O(4) 125.9(4) 1_456 1_556 ? V(2) O(8) Cs 88.1(4) . 1_556 ? O(5) O(8) Cs 61.1(3) . 1_556 ? O(6) O(8) Cs 78.5(3) . 1_556 ? O(7) O(8) Cs 123.5(4) 1_456 1_556 ? Cs O(8) Cs 105.5(3) 4_567 1_556 ? O(4) O(8) Cs 156.0(4) 1_456 1_556 ? O(4) O(8) Cs 61.7(2) 1_556 1_556 ? V(2) O(8) Cs 80.4(4) . 1_456 ? O(5) O(8) Cs 63.1(3) . 1_456 ? O(6) O(8) Cs 116.3(4) . 1_456 ? O(7) O(8) Cs 62.9(3) 1_456 1_456 ? Cs O(8) Cs 101.7(3) 4_567 1_456 ? O(4) O(8) Cs 60.3(2) 1_456 1_456 ? O(4) O(8) Cs 157.2(4) 1_556 1_456 ? Cs O(8) Cs 104.0(3) 1_556 1_456 ? _refine_diff_density_max 2.755 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.371 #=END