# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/165 data_global _publ_contact_author ; J. Y. Pivan Laboratoire de Physicochimie ENS Chimie Rennes Campus de Beaulieu Avenue Du Gnral Leclerc 35700 Rennes France ; _publ_contact_author_email jean.yves-pivan@ensc-rennes.fr _publ_requested_journal 'Journal of Materials Chemistry ' data_pbvp3l _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'O56 P8 Pb4 V8' _chemical_formula_weight 2380.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 '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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.377(9) _cell_length_b 6.38420(10) _cell_length_c 25.357(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1032.4(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 18.433 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_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 6315 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 29.91 _reflns_number_total 2966 _reflns_number_gt 2556 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0636P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.003(8) _refine_ls_number_reflns 2966 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.87694(5) 0.11767(4) 0.124267(12) 0.01917(10) Uani 1 1 d . . . V1 V 1.2494(2) 0.34078(16) 0.22764(5) 0.0068(2) Uani 1 1 d . . . V3 V 1.15193(18) 0.00273(17) -0.02232(5) 0.0071(2) Uani 1 1 d . . . P1 P 0.6555(3) 0.0000(3) -0.00149(7) 0.0071(3) Uani 1 1 d . . . P2 P 0.7504(3) 0.3399(2) 0.24944(6) 0.0067(3) Uani 1 1 d . . . O12 O 0.9395(8) 0.3315(9) 0.2114(2) 0.0110(10) Uani 1 1 d . . . O13 O 1.2417(9) 0.0346(8) 0.21546(19) 0.0107(9) Uani 1 1 d . . . O14 O 0.7563(10) -0.1444(9) 0.2095(2) 0.0165(10) Uani 1 1 d . . . O15 O 0.5574(8) 0.3367(9) 0.2130(2) 0.0123(10) Uani 1 1 d . . . O16 O 1.2520(9) 0.6518(7) 0.2120(2) 0.0113(9) Uani 1 1 d . . . O31 O 1.1353(10) 0.0103(9) 0.0408(2) 0.0172(10) Uani 1 1 d . . . O32 O 0.8442(8) -0.0011(9) -0.0401(2) 0.0106(10) Uani 1 1 d . . . O34 O 0.4587(8) 0.0074(9) -0.0361(2) 0.0123(10) Uani 1 1 d . . . O35 O 0.6645(9) 0.1884(8) 0.0366(2) 0.0113(10) Uani 1 1 d . . . O36 O 0.6578(9) -0.1935(7) 0.0348(2) 0.0119(10) Uani 1 1 d . . . OW1 O 1.0173(10) -0.2596(8) 0.1273(3) 0.0170(10) Uani 1 1 d . . . OW2 O 0.4903(10) -0.0419(9) 0.1247(3) 0.0203(11) Uani 1 1 d . . . OW3 O 1.2514(9) 0.3006(7) 0.1328(2) 0.0137(10) Uani 1 1 d . . . OW4 O 0.6782(8) 0.4959(9) 0.1156(2) 0.0147(10) 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 Pb 0.01905(14) 0.01738(14) 0.02109(15) -0.00262(12) -0.00448(13) 0.00114(11) V1 0.0064(5) 0.0065(4) 0.0075(5) 0.0002(4) 0.0004(4) 0.0001(4) V3 0.0077(5) 0.0062(4) 0.0076(5) 0.0004(4) 0.0001(4) -0.0001(4) P1 0.0061(7) 0.0062(6) 0.0091(8) 0.0004(5) -0.0001(6) 0.0001(6) P2 0.0068(7) 0.0055(6) 0.0079(8) -0.0004(5) 0.0007(7) 0.0006(5) O12 0.007(2) 0.018(3) 0.008(2) 0.0015(18) 0.0029(19) 0.0009(17) O13 0.015(2) 0.009(2) 0.008(2) 0.0026(16) 0.000(2) -0.0001(19) O14 0.022(3) 0.020(3) 0.008(2) -0.0004(19) 0.002(2) 0.004(2) O15 0.007(2) 0.018(3) 0.011(2) 0.0013(19) -0.0003(19) -0.0005(18) O16 0.014(2) 0.009(2) 0.011(2) -0.0044(16) -0.002(2) 0.0013(19) O31 0.020(3) 0.016(2) 0.016(3) 0.0001(19) 0.000(3) -0.001(3) O32 0.007(2) 0.014(2) 0.011(2) 0.0014(18) 0.0042(18) 0.0003(19) O34 0.008(2) 0.013(2) 0.016(3) -0.001(2) -0.004(2) -0.0014(19) O35 0.017(3) 0.0048(19) 0.012(2) 0.0006(16) -0.001(2) -0.0009(17) O36 0.018(3) 0.0063(19) 0.011(2) -0.0006(16) 0.001(2) 0.0005(18) OW1 0.019(3) 0.014(2) 0.018(3) 0.000(2) -0.005(3) 0.0009(18) OW2 0.023(3) 0.022(2) 0.015(3) -0.002(2) 0.001(3) 0.006(2) OW3 0.013(2) 0.017(2) 0.012(3) 0.0014(18) 0.003(2) 0.0014(18) OW4 0.017(3) 0.020(2) 0.007(2) 0.0009(18) 0.0031(19) -0.0041(19) _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 Pb OW1 2.571(5) . ? Pb O12 2.628(6) . ? Pb O35 2.641(6) . ? Pb OW2 2.668(7) . ? Pb OW3 2.667(7) . ? Pb OW4 2.736(6) . ? V1 O14 1.597(5) 4_755 ? V1 O13 1.980(5) . ? V1 O15 1.999(6) 1_655 ? V1 O16 2.025(5) . ? V1 O12 2.020(6) . ? V1 OW3 2.418(6) . ? V3 O31 1.604(6) . ? V3 O34 1.988(6) 1_655 ? V3 O36 2.000(5) 3_545 ? V3 O35 2.006(5) 3 ? V3 O32 2.014(6) . ? V3 OW4 2.372(5) 3 ? P1 O34 1.532(6) . ? P1 O36 1.540(5) . ? P1 O35 1.545(5) . ? P1 O32 1.551(5) . ? P2 O13 1.529(5) 4_755 ? P2 O15 1.539(6) . ? P2 O12 1.545(6) . ? P2 O16 1.548(5) 4_745 ? O13 P2 1.529(5) 4_745 ? O14 V1 1.597(5) 4_745 ? O15 V1 1.999(6) 1_455 ? O16 P2 1.548(5) 4_755 ? O34 V3 1.988(6) 1_455 ? O35 V3 2.006(5) 3_455 ? O36 V3 2.000(5) 3_445 ? OW4 V3 2.372(5) 3_455 ? 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 OW1 Pb O12 114.14(18) . . ? OW1 Pb O35 111.33(18) . . ? O12 Pb O35 134.13(16) . . ? OW1 Pb OW2 87.9(2) . . ? O12 Pb OW2 109.60(18) . . ? O35 Pb OW2 66.07(19) . . ? OW1 Pb OW3 95.51(18) . . ? O12 Pb OW3 64.42(16) . . ? O35 Pb OW3 116.93(17) . . ? OW2 Pb OW3 173.92(18) . . ? OW1 Pb OW4 172.15(17) . . ? O12 Pb OW4 71.29(16) . . ? O35 Pb OW4 62.87(15) . . ? OW2 Pb OW4 84.79(18) . . ? OW3 Pb OW4 92.00(17) . . ? O14 V1 O13 102.3(3) 4_755 . ? O14 V1 O15 102.0(3) 4_755 1_655 ? O13 V1 O15 89.0(2) . 1_655 ? O14 V1 O16 97.9(3) 4_755 . ? O13 V1 O16 159.7(2) . . ? O15 V1 O16 88.2(2) 1_655 . ? O14 V1 O12 100.5(3) 4_755 . ? O13 V1 O12 85.1(2) . . ? O15 V1 O12 157.4(2) 1_655 . ? O16 V1 O12 89.8(2) . . ? O14 V1 OW3 177.1(2) 4_755 . ? O13 V1 OW3 74.94(18) . . ? O15 V1 OW3 79.0(2) 1_655 . ? O16 V1 OW3 84.83(19) . . ? O12 V1 OW3 78.4(2) . . ? O31 V3 O34 103.9(3) . 1_655 ? O31 V3 O36 100.9(3) . 3_545 ? O34 V3 O36 88.2(2) 1_655 3_545 ? O31 V3 O35 98.8(3) . 3 ? O34 V3 O35 85.1(2) 1_655 3 ? O36 V3 O35 160.2(2) 3_545 3 ? O31 V3 O32 99.2(3) . . ? O34 V3 O32 156.9(2) 1_655 . ? O36 V3 O32 88.3(2) 3_545 . ? O35 V3 O32 90.6(2) 3 . ? O31 V3 OW4 178.0(2) . 3 ? O34 V3 OW4 75.8(2) 1_655 3 ? O36 V3 OW4 81.1(2) 3_545 3 ? O35 V3 OW4 79.2(2) 3 3 ? O32 V3 OW4 81.1(2) . 3 ? O34 P1 O36 112.0(3) . . ? O34 P1 O35 111.4(3) . . ? O36 P1 O35 104.5(3) . . ? O34 P1 O32 105.9(3) . . ? O36 P1 O32 111.5(3) . . ? O35 P1 O32 111.7(3) . . ? O13 P2 O15 112.7(3) 4_755 . ? O13 P2 O12 111.4(3) 4_755 . ? O15 P2 O12 104.4(3) . . ? O13 P2 O16 105.3(3) 4_755 4_745 ? O15 P2 O16 111.1(3) . 4_745 ? O12 P2 O16 112.0(3) . 4_745 ? P2 O12 V1 129.5(3) . . ? P2 O12 Pb 115.1(3) . . ? V1 O12 Pb 109.6(2) . . ? P2 O13 V1 135.3(3) 4_745 . ? P2 O15 V1 132.4(4) . 1_455 ? P2 O16 V1 129.6(3) 4_755 . ? P1 O32 V3 127.9(3) . . ? P1 O34 V3 134.8(4) . 1_455 ? P1 O35 V3 130.6(3) . 3_455 ? P1 O35 Pb 114.4(3) . . ? V3 O35 Pb 109.9(2) 3_455 . ? P1 O36 V3 134.2(3) . 3_445 ? V1 OW3 Pb 97.05(19) . . ? V3 OW4 Pb 96.66(19) 3_455 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.91 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.033 _refine_diff_density_min -2.704 _refine_diff_density_rms 0.328