# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jingui Qin' _publ_contact_author_address ; Wuhan 430072 ; _publ_contact_author_email jgqin@whu.edu.cn loop_ _publ_author_name J.Qin T.Zhu P.Halasyamani # Attachment '- K4V6Te3O24-cif.cif' data_K4Te3V6O24 _database_code_depnum_ccdc_archive 'CCDC 819244' #TrackingRef '- K4V6Te3O24-cif.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'K4 O24 Te3 V6' _chemical_formula_weight 1228.84 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _cell_length_a 9.7075(6) _cell_length_b 9.7075(6) _cell_length_c 42.701(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3484.9(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 3.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3372 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.828 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7718 _exptl_absorpt_correction_T_max 0.8214 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0137 _diffrn_reflns_number 6577 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.6 _diffrn_reflns_theta_max 28.76 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _reflns_number_total 982 _reflns_number_gt 953 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+20.2751P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00030(3) _refine_ls_number_reflns 982 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0435 _refine_ls_wR_factor_gt 0.0432 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.53 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.116 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.3333 0.6667 0.018283(6) 0.01178(10) Uani 1 3 d S . . Te2 Te 0.6667 0.3333 0.0833 0.01067(10) Uani 1 6 d S . . K1 K 0 0 0 0.0698(8) Uani 1 6 d S . . K2 K 0.06414(9) 0.3333 0.0833 0.0284(2) Uani 1 2 d S . . V1 V 0.38612(5) 0.35432(5) 0.037388(10) 0.01332(11) Uani 1 1 d . . . O1 O 0.3334(2) 0.5077(2) 0.04385(4) 0.0161(3) Uani 1 1 d . . . O2 O 0.5770(2) 0.4271(2) 0.05706(4) 0.0168(4) Uani 1 1 d . . . O3 O 0.2441(2) 0.1919(2) 0.05259(5) 0.0245(4) Uani 1 1 d . . . O4 O 0.4012(3) 0.3196(3) 0.00022(5) 0.0272(4) Uani 1 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 Te1 0.01157(11) 0.01157(11) 0.01220(14) 0 0 0.00579(5) Te2 0.00898(12) 0.00898(12) 0.01404(19) 0 0 0.00449(6) K1 0.0801(12) 0.0801(12) 0.0493(14) 0 0 0.0400(6) K2 0.0193(3) 0.0317(5) 0.0382(5) 0.0060(4) 0.00299(19) 0.0159(2) V1 0.0129(2) 0.0126(2) 0.0157(2) -0.00031(14) -0.00020(14) 0.00734(16) O1 0.0187(9) 0.0160(8) 0.0175(8) 0.0028(7) 0.0007(7) 0.0116(7) O2 0.0160(8) 0.0166(8) 0.0200(9) 0.0020(7) -0.0029(7) 0.0097(7) O3 0.0219(10) 0.0171(9) 0.0317(11) 0.0056(8) 0.0043(8) 0.0078(8) O4 0.0332(11) 0.0317(11) 0.0190(9) -0.0054(8) -0.0010(8) 0.0179(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Te1 O1 1.8901(17) 3_565 ? Te1 O1 1.8901(17) 2_665 ? Te1 O1 1.8901(17) . ? Te1 K2 4.0693(3) 3_565 ? Te1 K2 4.0693(3) 2_665 ? Te1 K2 4.0693(3) . ? Te2 O2 1.9070(17) 18_654 ? Te2 O2 1.9070(17) 17_554 ? Te2 O2 1.9070(17) 16_544 ? Te2 O2 1.9071(17) 2_655 ? Te2 O2 1.9071(17) 3_665 ? Te2 O2 1.9071(17) . ? Te2 K2 3.8585(9) 1_655 ? Te2 K2 3.8585(9) 3 ? Te2 K2 3.8585(9) 2_665 ? K1 O3 3.117(2) 19 ? K1 O3 3.117(2) . ? K1 O3 3.117(2) 21 ? K1 O3 3.117(2) 20 ? K1 O3 3.117(2) 2 ? K1 O3 3.117(2) 3 ? K1 V1 3.9417(5) . ? K1 V1 3.9417(5) 19 ? K1 V1 3.9417(5) 2 ? K1 V1 3.9417(5) 3 ? K1 V1 3.9417(5) 20 ? K1 V1 3.9417(5) 21 ? K2 O1 2.8486(18) 17_554 ? K2 O1 2.8486(18) . ? K2 O2 2.854(2) 16_444 ? K2 O2 2.854(2) 3_565 ? K2 O3 2.927(2) 18_554 ? K2 O3 2.927(2) 2 ? K2 O3 3.010(2) 17_554 ? K2 O3 3.010(2) . ? K2 O1 3.3156(18) 16_444 ? K2 O1 3.3157(18) 3_565 ? K2 V1 3.6088(8) 17_554 ? K2 V1 3.6088(8) . ? V1 O3 1.623(2) . ? V1 O4 1.644(2) . ? V1 O1 1.8219(18) . ? V1 O2 1.8243(18) . ? V1 K2 3.8301(7) 2_665 ? O1 K2 3.3157(18) 2_665 ? O2 K2 2.854(2) 2_665 ? O3 K2 2.927(2) 3 ? 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 O1 Te1 O1 89.97(7) 3_565 2_665 ? O1 Te1 O1 89.97(7) 3_565 . ? O1 Te1 O1 89.97(7) 2_665 . ? O1 Te1 K2 38.63(6) 3_565 3_565 ? O1 Te1 K2 53.55(6) 2_665 3_565 ? O1 Te1 K2 101.09(5) . 3_565 ? O1 Te1 K2 101.09(5) 3_565 2_665 ? O1 Te1 K2 38.63(5) 2_665 2_665 ? O1 Te1 K2 53.55(6) . 2_665 ? K2 Te1 K2 78.525(7) 3_565 2_665 ? O1 Te1 K2 53.55(6) 3_565 . ? O1 Te1 K2 101.09(5) 2_665 . ? O1 Te1 K2 38.63(6) . . ? K2 Te1 K2 78.525(7) 3_565 . ? K2 Te1 K2 78.525(7) 2_665 . ? O2 Te2 O2 88.92(8) 18_654 17_554 ? O2 Te2 O2 88.92(8) 18_654 16_544 ? O2 Te2 O2 88.92(8) 17_554 16_544 ? O2 Te2 O2 178.83(11) 18_654 2_655 ? O2 Te2 O2 90.27(11) 17_554 2_655 ? O2 Te2 O2 91.91(11) 16_544 2_655 ? O2 Te2 O2 91.91(11) 18_654 3_665 ? O2 Te2 O2 178.83(11) 17_554 3_665 ? O2 Te2 O2 90.27(11) 16_544 3_665 ? O2 Te2 O2 88.91(8) 2_655 3_665 ? O2 Te2 O2 90.27(11) 18_654 . ? O2 Te2 O2 91.91(11) 17_554 . ? O2 Te2 O2 178.83(11) 16_544 . ? O2 Te2 O2 88.91(8) 2_655 . ? O2 Te2 O2 88.91(8) 3_665 . ? O2 Te2 K2 90.58(5) 18_654 1_655 ? O2 Te2 K2 134.04(5) 17_554 1_655 ? O2 Te2 K2 45.13(5) 16_544 1_655 ? O2 Te2 K2 90.59(5) 2_655 1_655 ? O2 Te2 K2 45.14(5) 3_665 1_655 ? O2 Te2 K2 134.04(5) . 1_655 ? O2 Te2 K2 134.05(5) 18_654 3 ? O2 Te2 K2 45.13(5) 17_554 3 ? O2 Te2 K2 90.59(5) 16_544 3 ? O2 Te2 K2 45.14(5) 2_655 3 ? O2 Te2 K2 134.04(5) 3_665 3 ? O2 Te2 K2 90.59(5) . 3 ? K2 Te2 K2 120 1_655 3 ? O2 Te2 K2 45.14(5) 18_654 2_665 ? O2 Te2 K2 90.59(5) 17_554 2_665 ? O2 Te2 K2 134.05(5) 16_544 2_665 ? O2 Te2 K2 134.04(5) 2_655 2_665 ? O2 Te2 K2 90.59(5) 3_665 2_665 ? O2 Te2 K2 45.14(5) . 2_665 ? K2 Te2 K2 120 1_655 2_665 ? K2 Te2 K2 120 3 2_665 ? O3 K1 O3 180.00(5) 19 . ? O3 K1 O3 73.82(6) 19 21 ? O3 K1 O3 106.18(6) . 21 ? O3 K1 O3 73.82(6) 19 20 ? O3 K1 O3 106.18(6) . 20 ? O3 K1 O3 73.82(6) 21 20 ? O3 K1 O3 106.18(6) 19 2 ? O3 K1 O3 73.82(6) . 2 ? O3 K1 O3 106.18(6) 21 2 ? O3 K1 O3 180.00(5) 20 2 ? O3 K1 O3 106.18(6) 19 3 ? O3 K1 O3 73.82(6) . 3 ? O3 K1 O3 180.00(5) 21 3 ? O3 K1 O3 106.18(6) 20 3 ? O3 K1 O3 73.82(6) 2 3 ? O3 K1 V1 157.00(4) 19 . ? O3 K1 V1 23.00(4) . . ? O3 K1 V1 84.62(4) 21 . ? O3 K1 V1 92.79(4) 20 . ? O3 K1 V1 87.21(4) 2 . ? O3 K1 V1 95.38(4) 3 . ? O3 K1 V1 23.00(4) 19 19 ? O3 K1 V1 157.00(4) . 19 ? O3 K1 V1 95.38(4) 21 19 ? O3 K1 V1 87.21(4) 20 19 ? O3 K1 V1 92.79(4) 2 19 ? O3 K1 V1 84.62(4) 3 19 ? V1 K1 V1 180.000(11) . 19 ? O3 K1 V1 84.62(4) 19 2 ? O3 K1 V1 95.38(4) . 2 ? O3 K1 V1 92.79(4) 21 2 ? O3 K1 V1 157.00(4) 20 2 ? O3 K1 V1 23.00(4) 2 2 ? O3 K1 V1 87.21(4) 3 2 ? V1 K1 V1 104.709(7) . 2 ? V1 K1 V1 75.291(7) 19 2 ? O3 K1 V1 92.79(4) 19 3 ? O3 K1 V1 87.21(4) . 3 ? O3 K1 V1 157.00(4) 21 3 ? O3 K1 V1 84.62(4) 20 3 ? O3 K1 V1 95.38(4) 2 3 ? O3 K1 V1 23.00(4) 3 3 ? V1 K1 V1 104.709(7) . 3 ? V1 K1 V1 75.291(7) 19 3 ? V1 K1 V1 104.710(7) 2 3 ? O3 K1 V1 95.38(4) 19 20 ? O3 K1 V1 84.62(4) . 20 ? O3 K1 V1 87.21(4) 21 20 ? O3 K1 V1 23.00(4) 20 20 ? O3 K1 V1 157.00(4) 2 20 ? O3 K1 V1 92.79(4) 3 20 ? V1 K1 V1 75.291(7) . 20 ? V1 K1 V1 104.709(7) 19 20 ? V1 K1 V1 180.000(11) 2 20 ? V1 K1 V1 75.291(7) 3 20 ? O3 K1 V1 87.21(4) 19 21 ? O3 K1 V1 92.79(4) . 21 ? O3 K1 V1 23.00(4) 21 21 ? O3 K1 V1 95.38(4) 20 21 ? O3 K1 V1 84.62(4) 2 21 ? O3 K1 V1 157.00(4) 3 21 ? V1 K1 V1 75.291(7) . 21 ? V1 K1 V1 104.709(7) 19 21 ? V1 K1 V1 75.291(7) 2 21 ? V1 K1 V1 180.000(11) 3 21 ? V1 K1 V1 104.709(7) 20 21 ? O1 K2 O1 103.33(7) 17_554 . ? O1 K2 O2 100.23(5) 17_554 16_444 ? O1 K2 O2 156.20(5) . 16_444 ? O1 K2 O2 156.20(5) 17_554 3_565 ? O1 K2 O2 100.23(5) . 3_565 ? O2 K2 O2 56.54(7) 16_444 3_565 ? O1 K2 O3 112.82(5) 17_554 18_554 ? O1 K2 O3 95.02(5) . 18_554 ? O2 K2 O3 72.53(5) 16_444 18_554 ? O2 K2 O3 68.00(6) 3_565 18_554 ? O1 K2 O3 95.02(5) 17_554 2 ? O1 K2 O3 112.82(5) . 2 ? O2 K2 O3 68.00(6) 16_444 2 ? O2 K2 O3 72.52(5) 3_565 2 ? O3 K2 O3 134.95(8) 18_554 2 ? O1 K2 O3 56.19(5) 17_554 17_554 ? O1 K2 O3 63.47(5) . 17_554 ? O2 K2 O3 130.17(5) 16_444 17_554 ? O2 K2 O3 141.19(5) 3_565 17_554 ? O3 K2 O3 78.18(8) 18_554 17_554 ? O3 K2 O3 145.52(3) 2 17_554 ? O1 K2 O3 63.47(5) 17_554 . ? O1 K2 O3 56.19(5) . . ? O2 K2 O3 141.18(5) 16_444 . ? O2 K2 O3 130.17(5) 3_565 . ? O3 K2 O3 145.52(3) 18_554 . ? O3 K2 O3 78.18(8) 2 . ? O3 K2 O3 72.09(8) 17_554 . ? O1 K2 O1 50.69(6) 17_554 16_444 ? O1 K2 O1 146.97(3) . 16_444 ? O2 K2 O1 55.34(5) 16_444 16_444 ? O2 K2 O1 106.13(5) 3_565 16_444 ? O3 K2 O1 113.02(5) 18_554 16_444 ? O3 K2 O1 58.83(5) 2 16_444 ? O3 K2 O1 104.21(5) 17_554 16_444 ? O3 K2 O1 91.24(5) . 16_444 ? O1 K2 O1 146.97(3) 17_554 3_565 ? O1 K2 O1 50.69(6) . 3_565 ? O2 K2 O1 106.13(5) 16_444 3_565 ? O2 K2 O1 55.34(5) 3_565 3_565 ? O3 K2 O1 58.83(5) 18_554 3_565 ? O3 K2 O1 113.02(5) 2 3_565 ? O3 K2 O1 91.24(5) 17_554 3_565 ? O3 K2 O1 104.21(5) . 3_565 ? O1 K2 O1 160.99(7) 16_444 3_565 ? O1 K2 V1 29.93(4) 17_554 17_554 ? O1 K2 V1 80.05(4) . 17_554 ? O2 K2 V1 120.75(4) 16_444 17_554 ? O2 K2 V1 164.70(4) 3_565 17_554 ? O3 K2 V1 96.70(4) 18_554 17_554 ? O3 K2 V1 121.69(4) 2 17_554 ? O3 K2 V1 26.45(4) 17_554 17_554 ? O3 K2 V1 62.63(4) . 17_554 ? O1 K2 V1 79.67(3) 16_444 17_554 ? O1 K2 V1 117.14(3) 3_565 17_554 ? O1 K2 V1 80.05(4) 17_554 . ? O1 K2 V1 29.93(4) . . ? O2 K2 V1 164.70(4) 16_444 . ? O2 K2 V1 120.75(4) 3_565 . ? O3 K2 V1 121.69(4) 18_554 . ? O3 K2 V1 96.70(4) 2 . ? O3 K2 V1 62.63(4) 17_554 . ? O3 K2 V1 26.45(4) . . ? O1 K2 V1 117.14(3) 16_444 . ? O1 K2 V1 79.67(3) 3_565 . ? V1 K2 V1 66.16(2) 17_554 . ? O3 V1 O4 107.84(11) . . ? O3 V1 O1 106.51(9) . . ? O4 V1 O1 113.84(10) . . ? O3 V1 O2 113.37(9) . . ? O4 V1 O2 110.28(10) . . ? O1 V1 O2 105.06(8) . . ? O3 V1 K2 55.71(7) . . ? O4 V1 K2 132.58(8) . . ? O1 V1 K2 51.27(6) . . ? O2 V1 K2 117.04(6) . . ? O3 V1 K2 125.13(8) . 2_665 ? O4 V1 K2 126.62(8) . 2_665 ? O1 V1 K2 59.92(6) . 2_665 ? O2 V1 K2 45.16(6) . 2_665 ? K2 V1 K2 87.589(12) . 2_665 ? O3 V1 K1 48.63(7) . . ? O4 V1 K1 64.75(8) . . ? O1 V1 K1 103.97(6) . . ? O2 V1 K1 149.64(6) . . ? K2 V1 K1 75.644(9) . . ? K2 V1 K1 162.243(14) 2_665 . ? V1 O1 Te1 133.99(10) . . ? V1 O1 K2 98.81(7) . . ? Te1 O1 K2 116.90(8) . . ? V1 O1 K2 91.69(7) . 2_665 ? Te1 O1 K2 99.15(7) . 2_665 ? K2 O1 K2 113.14(5) . 2_665 ? V1 O2 Te2 134.73(10) . . ? V1 O2 K2 107.89(8) . 2_665 ? Te2 O2 K2 106.59(7) . 2_665 ? V1 O3 K2 127.85(10) . 3 ? V1 O3 K2 97.83(9) . . ? K2 O3 K2 120.36(7) 3 . ? V1 O3 K1 108.37(9) . . ? K2 O3 K1 100.18(6) 3 . ? K2 O3 K1 98.37(6) . . ? # Attachment '- Rb4V6Te3O24_cif.cif' data_Rb4Te3V6O24 _database_code_depnum_ccdc_archive 'CCDC 819245' #TrackingRef '- Rb4V6Te3O24_cif.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'O24 Rb4 Te3 V6' _chemical_formula_weight 1414.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _cell_length_a 9.8399(9) _cell_length_b 9.8399(9) _cell_length_c 43.012(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3606.6(6) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 3.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3804 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 0.6796 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5558 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.06 _reflns_number_total 718 _reflns_number_gt 594 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+1.0851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_coef 0.000029(13) _refine_ls_number_reflns 718 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.3333 0.6667 0.017735(13) 0.01201(17) Uani 1 3 d S . . Te2 Te 0.6667 0.3333 0.0833 0.0129(2) Uani 1 6 d S . . Rb1 Rb 0.0000 0.0000 0.0000 0.0559(5) Uani 1 6 d S . . Rb2 Rb 0.06539(7) 0.3333 0.0833 0.0239(2) Uani 1 2 d S . . V1 V 0.39010(10) 0.35828(10) 0.03731(2) 0.0153(2) Uani 1 1 d . . . O1 O 0.3420(4) 0.5134(4) 0.04287(7) 0.0150(8) Uani 1 1 d . . . O2 O 0.5767(4) 0.4245(4) 0.05709(8) 0.0187(8) Uani 1 1 d . . . O3 O 0.2481(4) 0.2002(4) 0.05255(9) 0.0243(9) Uani 1 1 d . . . O4 O 0.4040(5) 0.3196(4) 0.00084(9) 0.0287(9) Uani 1 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 Te1 0.0112(2) 0.0112(2) 0.0136(3) 0.000 0.000 0.00562(10) Te2 0.0103(3) 0.0103(3) 0.0180(5) 0.000 0.000 0.00515(13) Rb1 0.0648(8) 0.0648(8) 0.0380(11) 0.000 0.000 0.0324(4) Rb2 0.0165(3) 0.0255(4) 0.0327(5) 0.0059(4) 0.00294(18) 0.0127(2) V1 0.0139(5) 0.0134(5) 0.0198(5) 0.0003(4) 0.0008(4) 0.0078(4) O1 0.0139(19) 0.0128(18) 0.020(2) 0.0018(16) 0.0006(17) 0.0080(16) O2 0.0171(19) 0.0167(19) 0.025(2) 0.0027(17) -0.0024(17) 0.0109(16) O3 0.021(2) 0.019(2) 0.033(2) 0.0043(19) 0.0039(19) 0.0098(18) O4 0.036(2) 0.029(2) 0.020(2) -0.0027(18) -0.0001(19) 0.0151(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Te1 O1 1.891(3) 3_565 ? Te1 O1 1.891(3) 2_665 ? Te1 O1 1.891(3) . ? Te1 Rb2 4.1259(5) 3_565 ? Te1 Rb2 4.1259(5) 2_665 ? Te1 Rb2 4.1259(5) . ? Te2 O2 1.912(3) 18_654 ? Te2 O2 1.912(3) 17_554 ? Te2 O2 1.912(3) 16_544 ? Te2 O2 1.912(3) 2_655 ? Te2 O2 1.912(3) 3_665 ? Te2 O2 1.912(3) . ? Te2 Rb2 3.9234(8) 1_655 ? Te2 Rb2 3.9234(8) 3 ? Te2 Rb2 3.9234(8) 2_665 ? Rb1 O3 3.184(4) 19 ? Rb1 O3 3.184(4) . ? Rb1 O3 3.184(4) 21 ? Rb1 O3 3.184(4) 20 ? Rb1 O3 3.184(4) 2 ? Rb1 O3 3.184(4) 3 ? Rb1 O4 3.632(4) . ? Rb1 O4 3.632(4) 19 ? Rb1 O4 3.632(4) 21 ? Rb1 O4 3.632(4) 3 ? Rb1 O4 3.632(4) 2 ? Rb1 O4 3.632(4) 20 ? Rb2 O2 2.922(3) 16_444 ? Rb2 O2 2.922(3) 3_565 ? Rb2 O1 2.959(3) 17_554 ? Rb2 O1 2.959(3) . ? Rb2 O3 3.010(4) 17_554 ? Rb2 O3 3.010(4) . ? Rb2 O3 3.021(3) 18_554 ? Rb2 O3 3.021(3) 2 ? Rb2 O1 3.315(3) 16_444 ? Rb2 O1 3.315(3) 3_565 ? Rb2 V1 3.6610(11) 17_554 ? Rb2 V1 3.6610(11) . ? V1 O3 1.621(4) . ? V1 O4 1.636(4) . ? V1 O2 1.823(3) . ? V1 O1 1.826(3) . ? V1 Rb2 3.8525(10) 2_665 ? V1 Rb2 4.2108(10) 3 ? O1 Rb2 3.315(3) 2_665 ? O2 Rb2 2.922(3) 2_665 ? O3 Rb2 3.021(3) 3 ? 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 O1 Te1 O1 90.57(14) 3_565 2_665 ? O1 Te1 O1 90.57(14) 3_565 . ? O1 Te1 O1 90.57(14) 2_665 . ? O1 Te1 Rb2 40.62(10) 3_565 3_565 ? O1 Te1 Rb2 52.00(10) 2_665 3_565 ? O1 Te1 Rb2 101.66(10) . 3_565 ? O1 Te1 Rb2 101.66(10) 3_565 2_665 ? O1 Te1 Rb2 40.62(10) 2_665 2_665 ? O1 Te1 Rb2 52.00(10) . 2_665 ? Rb2 Te1 Rb2 78.375(11) 3_565 2_665 ? O1 Te1 Rb2 52.00(10) 3_565 . ? O1 Te1 Rb2 101.66(10) 2_665 . ? O1 Te1 Rb2 40.62(10) . . ? Rb2 Te1 Rb2 78.375(11) 3_565 . ? Rb2 Te1 Rb2 78.375(11) 2_665 . ? O2 Te2 O2 88.70(15) 18_654 17_554 ? O2 Te2 O2 88.70(15) 18_654 16_544 ? O2 Te2 O2 88.70(15) 17_554 16_544 ? O2 Te2 O2 179.6(2) 18_654 2_655 ? O2 Te2 O2 91.0(2) 17_554 2_655 ? O2 Te2 O2 91.6(2) 16_544 2_655 ? O2 Te2 O2 91.6(2) 18_654 3_665 ? O2 Te2 O2 179.6(2) 17_554 3_665 ? O2 Te2 O2 91.0(2) 16_544 3_665 ? O2 Te2 O2 88.70(15) 2_655 3_665 ? O2 Te2 O2 91.0(2) 18_654 . ? O2 Te2 O2 91.6(2) 17_554 . ? O2 Te2 O2 179.6(2) 16_544 . ? O2 Te2 O2 88.70(15) 2_655 . ? O2 Te2 O2 88.70(15) 3_665 . ? O2 Te2 Rb2 90.18(10) 18_654 1_655 ? O2 Te2 Rb2 134.22(10) 17_554 1_655 ? O2 Te2 Rb2 45.52(10) 16_544 1_655 ? O2 Te2 Rb2 90.18(10) 2_655 1_655 ? O2 Te2 Rb2 45.52(10) 3_665 1_655 ? O2 Te2 Rb2 134.22(10) . 1_655 ? O2 Te2 Rb2 134.22(10) 18_654 3 ? O2 Te2 Rb2 45.52(10) 17_554 3 ? O2 Te2 Rb2 90.18(10) 16_544 3 ? O2 Te2 Rb2 45.52(10) 2_655 3 ? O2 Te2 Rb2 134.22(10) 3_665 3 ? O2 Te2 Rb2 90.18(10) . 3 ? Rb2 Te2 Rb2 120.0 1_655 3 ? O2 Te2 Rb2 45.52(10) 18_654 2_665 ? O2 Te2 Rb2 90.19(10) 17_554 2_665 ? O2 Te2 Rb2 134.22(10) 16_544 2_665 ? O2 Te2 Rb2 134.22(10) 2_655 2_665 ? O2 Te2 Rb2 90.18(10) 3_665 2_665 ? O2 Te2 Rb2 45.52(10) . 2_665 ? Rb2 Te2 Rb2 120.0 1_655 2_665 ? Rb2 Te2 Rb2 120.0 3 2_665 ? O3 Rb1 O3 180.00(16) 19 . ? O3 Rb1 O3 75.19(10) 19 21 ? O3 Rb1 O3 104.81(10) . 21 ? O3 Rb1 O3 75.19(10) 19 20 ? O3 Rb1 O3 104.81(10) . 20 ? O3 Rb1 O3 75.19(10) 21 20 ? O3 Rb1 O3 104.81(10) 19 2 ? O3 Rb1 O3 75.19(10) . 2 ? O3 Rb1 O3 104.81(10) 21 2 ? O3 Rb1 O3 180.00(14) 20 2 ? O3 Rb1 O3 104.81(10) 19 3 ? O3 Rb1 O3 75.19(10) . 3 ? O3 Rb1 O3 180.00(14) 21 3 ? O3 Rb1 O3 104.81(10) 20 3 ? O3 Rb1 O3 75.19(10) 2 3 ? O3 Rb1 O4 135.34(9) 19 . ? O3 Rb1 O4 44.66(9) . . ? O3 Rb1 O4 70.41(9) 21 . ? O3 Rb1 O4 69.21(9) 20 . ? O3 Rb1 O4 110.79(9) 2 . ? O3 Rb1 O4 109.59(9) 3 . ? O3 Rb1 O4 44.66(9) 19 19 ? O3 Rb1 O4 135.34(9) . 19 ? O3 Rb1 O4 109.59(9) 21 19 ? O3 Rb1 O4 110.79(9) 20 19 ? O3 Rb1 O4 69.21(9) 2 19 ? O3 Rb1 O4 70.41(9) 3 19 ? O4 Rb1 O4 180.0(2) . 19 ? O3 Rb1 O4 110.79(9) 19 21 ? O3 Rb1 O4 69.21(9) . 21 ? O3 Rb1 O4 44.66(9) 21 21 ? O3 Rb1 O4 109.59(9) 20 21 ? O3 Rb1 O4 70.41(9) 2 21 ? O3 Rb1 O4 135.34(9) 3 21 ? O4 Rb1 O4 60.010(2) . 21 ? O4 Rb1 O4 119.990(2) 19 21 ? O3 Rb1 O4 69.21(9) 19 3 ? O3 Rb1 O4 110.79(9) . 3 ? O3 Rb1 O4 135.34(9) 21 3 ? O3 Rb1 O4 70.41(9) 20 3 ? O3 Rb1 O4 109.59(9) 2 3 ? O3 Rb1 O4 44.66(9) 3 3 ? O4 Rb1 O4 119.990(2) . 3 ? O4 Rb1 O4 60.010(2) 19 3 ? O4 Rb1 O4 180.00(17) 21 3 ? O3 Rb1 O4 70.41(9) 19 2 ? O3 Rb1 O4 109.59(9) . 2 ? O3 Rb1 O4 69.21(9) 21 2 ? O3 Rb1 O4 135.34(9) 20 2 ? O3 Rb1 O4 44.66(9) 2 2 ? O3 Rb1 O4 110.79(9) 3 2 ? O4 Rb1 O4 119.990(2) . 2 ? O4 Rb1 O4 60.010(2) 19 2 ? O4 Rb1 O4 60.010(2) 21 2 ? O4 Rb1 O4 119.990(2) 3 2 ? O3 Rb1 O4 109.59(9) 19 20 ? O3 Rb1 O4 70.41(9) . 20 ? O3 Rb1 O4 110.79(9) 21 20 ? O3 Rb1 O4 44.66(9) 20 20 ? O3 Rb1 O4 135.34(9) 2 20 ? O3 Rb1 O4 69.21(9) 3 20 ? O4 Rb1 O4 60.010(2) . 20 ? O4 Rb1 O4 119.990(2) 19 20 ? O4 Rb1 O4 119.990(2) 21 20 ? O4 Rb1 O4 60.010(2) 3 20 ? O4 Rb1 O4 180.00(12) 2 20 ? O2 Rb2 O2 55.67(13) 16_444 3_565 ? O2 Rb2 O1 100.68(9) 16_444 17_554 ? O2 Rb2 O1 155.77(9) 3_565 17_554 ? O2 Rb2 O1 155.77(9) 16_444 . ? O2 Rb2 O1 100.68(9) 3_565 . ? O1 Rb2 O1 103.31(12) 17_554 . ? O2 Rb2 O3 130.52(10) 16_444 17_554 ? O2 Rb2 O3 142.36(9) 3_565 17_554 ? O1 Rb2 O3 55.33(9) 17_554 17_554 ? O1 Rb2 O3 63.74(9) . 17_554 ? O2 Rb2 O3 142.36(9) 16_444 . ? O2 Rb2 O3 130.52(10) 3_565 . ? O1 Rb2 O3 63.74(9) 17_554 . ? O1 Rb2 O3 55.33(9) . . ? O3 Rb2 O3 70.81(14) 17_554 . ? O2 Rb2 O3 71.82(10) 16_444 18_554 ? O2 Rb2 O3 66.69(10) 3_565 18_554 ? O1 Rb2 O3 114.08(9) 17_554 18_554 ? O1 Rb2 O3 95.08(9) . 18_554 ? O3 Rb2 O3 80.21(14) 17_554 18_554 ? O3 Rb2 O3 145.33(4) . 18_554 ? O2 Rb2 O3 66.69(10) 16_444 2 ? O2 Rb2 O3 71.81(10) 3_565 2 ? O1 Rb2 O3 95.08(9) 17_554 2 ? O1 Rb2 O3 114.08(9) . 2 ? O3 Rb2 O3 145.33(4) 17_554 2 ? O3 Rb2 O3 80.21(14) . 2 ? O3 Rb2 O3 132.82(14) 18_554 2 ? O2 Rb2 O1 55.29(9) 16_444 16_444 ? O2 Rb2 O1 105.90(8) 3_565 16_444 ? O1 Rb2 O1 50.35(11) 17_554 16_444 ? O1 Rb2 O1 147.71(3) . 16_444 ? O3 Rb2 O1 102.70(9) 17_554 16_444 ? O3 Rb2 O1 93.00(9) . 16_444 ? O3 Rb2 O1 112.01(9) 18_554 16_444 ? O3 Rb2 O1 59.44(9) 2 16_444 ? O2 Rb2 O1 105.90(8) 16_444 3_565 ? O2 Rb2 O1 55.29(9) 3_565 3_565 ? O1 Rb2 O1 147.71(3) 17_554 3_565 ? O1 Rb2 O1 50.35(11) . 3_565 ? O3 Rb2 O1 93.01(9) 17_554 3_565 ? O3 Rb2 O1 102.70(9) . 3_565 ? O3 Rb2 O1 59.44(9) 18_554 3_565 ? O3 Rb2 O1 112.01(9) 2 3_565 ? O1 Rb2 O1 160.77(11) 16_444 3_565 ? O2 Rb2 V1 121.20(7) 16_444 17_554 ? O2 Rb2 V1 165.07(7) 3_565 17_554 ? O1 Rb2 V1 29.68(6) 17_554 17_554 ? O1 Rb2 V1 80.07(6) . 17_554 ? O3 Rb2 V1 25.84(7) 17_554 17_554 ? O3 Rb2 V1 62.09(7) . 17_554 ? O3 Rb2 V1 98.38(7) 18_554 17_554 ? O3 Rb2 V1 121.74(7) 2 17_554 ? O1 Rb2 V1 78.92(6) 16_444 17_554 ? O1 Rb2 V1 118.19(6) 3_565 17_554 ? O2 Rb2 V1 165.06(7) 16_444 . ? O2 Rb2 V1 121.20(7) 3_565 . ? O1 Rb2 V1 80.07(6) 17_554 . ? O1 Rb2 V1 29.68(6) . . ? O3 Rb2 V1 62.09(7) 17_554 . ? O3 Rb2 V1 25.84(7) . . ? O3 Rb2 V1 121.74(7) 18_554 . ? O3 Rb2 V1 98.37(7) 2 . ? O1 Rb2 V1 118.19(6) 16_444 . ? O1 Rb2 V1 78.92(6) 3_565 . ? V1 Rb2 V1 65.88(3) 17_554 . ? O3 V1 O4 107.2(2) . . ? O3 V1 O2 112.65(17) . . ? O4 V1 O2 110.13(18) . . ? O3 V1 O1 106.87(16) . . ? O4 V1 O1 114.01(18) . . ? O2 V1 O1 106.02(15) . . ? O3 V1 Rb2 54.04(12) . . ? O4 V1 Rb2 132.41(15) . . ? O2 V1 Rb2 117.45(11) . . ? O1 V1 Rb2 53.34(10) . . ? O3 V1 Rb2 124.54(14) . 2_665 ? O4 V1 Rb2 127.85(14) . 2_665 ? O2 V1 Rb2 46.73(11) . 2_665 ? O1 V1 Rb2 59.29(10) . 2_665 ? Rb2 V1 Rb2 87.85(2) . 2_665 ? O3 V1 Rb1 48.23(13) . . ? O4 V1 Rb1 64.40(14) . . ? O2 V1 Rb1 148.00(11) . . ? O1 V1 Rb1 104.60(11) . . ? Rb2 V1 Rb1 74.857(16) . . ? Rb2 V1 Rb1 161.80(3) 2_665 . ? O3 V1 Rb2 34.65(12) . 3 ? O4 V1 Rb2 103.65(14) . 3 ? O2 V1 Rb2 82.67(11) . 3 ? O1 V1 Rb2 134.52(11) . 3 ? Rb2 V1 Rb2 82.641(19) . 3 ? Rb2 V1 Rb2 114.79(3) 2_665 3 ? Rb1 V1 Rb2 69.220(16) . 3 ? V1 O1 Te1 136.50(19) . . ? V1 O1 Rb2 96.98(13) . . ? Te1 O1 Rb2 114.78(13) . . ? V1 O1 Rb2 92.44(12) . 2_665 ? Te1 O1 Rb2 101.28(12) . 2_665 ? Rb2 O1 Rb2 112.29(10) . 2_665 ? V1 O2 Te2 136.67(19) . . ? V1 O2 Rb2 106.25(13) . 2_665 ? Te2 O2 Rb2 106.64(14) . 2_665 ? V1 O3 Rb2 100.12(15) . . ? V1 O3 Rb2 127.58(17) . 3 ? Rb2 O3 Rb2 119.64(12) . 3 ? V1 O3 Rb1 109.45(17) . . ? Rb2 O3 Rb1 98.12(10) . . ? Rb2 O3 Rb1 97.89(10) 3 . ? V1 O4 Rb1 91.63(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.602 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.135