# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email yanchen169@gmail.com _publ_contact_author_name 'Yan Chen' _publ_author_name 'Yan Chen' data_3 _database_code_depnum_ccdc_archive 'CCDC 881578' #TrackingRef '- PbV2P2O13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'O13 P2 Pb V2' _chemical_formula_weight 579.01 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' P P 0.1023 0.0942 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 10.292(4) _cell_length_b 7.552(3) _cell_length_c 12.557(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.007(4) _cell_angle_gamma 90.00 _cell_volume 976.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2186 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.88 _exptl_crystal_description CUBIC _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 19.485 _exptl_absorpt_correction_type none _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2042 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2042 _reflns_number_gt 1853 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00160(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2042 _refine_ls_number_parameters 165 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.25279(7) 0.72413(4) 0.21272(3) 0.02232(15) Uani 1 1 d U . . V1 V 0.41082(15) 0.19896(17) 0.13423(14) 0.0064(3) Uani 1 1 d U . . V2 V 0.10039(15) 0.18093(18) 0.36374(13) 0.0071(3) Uani 1 1 d U . . P1 P 0.3792(2) 0.3746(3) 0.37336(17) 0.0067(4) Uani 1 1 d U . . P2 P 0.1209(2) 0.3600(3) 0.12455(17) 0.0061(4) Uani 1 1 d U . . O1 O 0.2306(6) 0.3699(7) 0.3647(5) 0.0125(12) Uani 1 1 d U . . O2 O 0.2696(6) 0.3815(6) 0.1297(5) 0.0100(12) Uani 1 1 d U . . O3 O 0.2646(13) 0.7416(6) 0.0159(6) 0.029(2) Uani 1 1 d U . . O4 O 0.0708(6) 0.5487(7) 0.1489(5) 0.0104(13) Uani 1 1 d U . . O5 O 0.0693(6) 0.2288(7) 0.2085(6) 0.0090(13) Uani 1 1 d U . . O6 O 0.4453(6) 0.2601(7) 0.2872(6) 0.0119(13) Uani 1 1 d U . . O7 O 0.0722(7) 0.2920(7) 0.0186(6) 0.0123(14) Uani 1 1 d U . . O8 O 0.4302(7) 0.3028(8) 0.4782(5) 0.0124(14) Uani 1 1 d U . . O9 O 0.1896(6) 1.0040(8) 0.3594(5) 0.0151(14) Uani 1 1 d . . . O10 O 0.4154(6) 0.5728(7) 0.3573(5) 0.0118(13) Uani 1 1 d U . . O11 O 0.0517(6) 0.9037(7) 0.1265(5) 0.0124(13) Uani 1 1 d U . . O12 O 0.3221(6) 1.0258(8) 0.1511(5) 0.0142(14) Uani 1 1 d U . . O13 O 0.5343(6) 0.4371(7) 0.1101(5) 0.0150(14) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0222(2) 0.01515(19) 0.0296(2) 0.00331(14) -0.0117(4) -0.0037(2) V1 0.0056(7) 0.0069(7) 0.0067(9) -0.0005(6) -0.0013(6) 0.0003(5) V2 0.0061(7) 0.0082(7) 0.0069(7) 0.0017(6) -0.0007(7) -0.0005(6) P1 0.0076(11) 0.0070(10) 0.0057(11) -0.0001(8) -0.0005(9) -0.0021(8) P2 0.0066(11) 0.0044(10) 0.0075(11) -0.0002(8) -0.0002(9) 0.0006(8) O1 0.005(3) 0.014(3) 0.019(3) 0.001(2) 0.000(3) -0.001(2) O2 0.005(3) 0.008(2) 0.017(3) -0.001(2) 0.001(3) 0.004(2) O3 0.040(6) 0.025(4) 0.021(3) -0.004(3) 0.015(5) -0.006(4) O4 0.011(3) 0.008(3) 0.012(3) -0.002(2) -0.001(2) 0.003(2) O5 0.011(3) 0.009(3) 0.006(4) 0.005(3) 0.001(3) -0.003(2) O6 0.013(3) 0.012(3) 0.011(3) -0.001(3) 0.001(3) 0.007(2) O7 0.015(4) 0.012(3) 0.010(3) -0.001(2) -0.006(3) -0.004(3) O8 0.018(4) 0.016(3) 0.003(3) 0.000(2) -0.001(3) 0.003(3) O9 0.012(3) 0.016(3) 0.018(3) 0.002(3) -0.002(3) 0.001(2) O10 0.006(3) 0.008(3) 0.021(4) 0.004(2) -0.002(3) -0.004(2) O11 0.013(3) 0.007(3) 0.018(4) 0.001(2) -0.003(3) -0.003(2) O12 0.008(3) 0.014(3) 0.021(4) 0.000(3) 0.003(3) 0.001(2) O13 0.013(3) 0.014(3) 0.019(4) -0.001(3) 0.000(3) -0.005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pb1 O4 2.430(6) . ? Pb1 O3 2.478(8) . ? Pb1 O12 2.510(6) . ? Pb1 O11 2.701(6) . ? Pb1 O10 2.720(6) . ? V1 O12 1.609(6) 1_545 ? V1 O8 1.969(7) 4_565 ? V1 O2 2.004(6) . ? V1 O6 2.007(8) . ? V1 O10 2.030(6) 2_645 ? V1 O13 2.223(6) . ? V2 O9 1.622(6) 1_545 ? V2 O1 1.958(6) . ? V2 O7 1.977(7) 4_566 ? V2 O5 2.008(8) . ? V2 O4 2.032(6) 2_545 ? V2 O11 2.301(6) 2_545 ? P1 O8 1.518(7) . ? P1 O1 1.534(6) . ? P1 O6 1.544(7) . ? P1 O10 1.556(6) . ? P2 O7 1.511(7) . ? P2 O2 1.540(6) . ? P2 O5 1.542(7) . ? P2 O4 1.546(6) . ? O4 V2 2.032(6) 2 ? O7 V2 1.977(7) 4_565 ? O8 V1 1.969(7) 4_566 ? O9 V2 1.622(6) 1_565 ? O10 V1 2.030(6) 2_655 ? O11 V2 2.301(6) 2 ? O12 V1 1.609(6) 1_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 O4 Pb1 O3 74.8(3) . . ? O4 Pb1 O12 127.7(2) . . ? O3 Pb1 O12 68.3(2) . . ? O4 Pb1 O11 63.32(18) . . ? O3 Pb1 O11 67.1(3) . . ? O12 Pb1 O11 68.80(18) . . ? O4 Pb1 O10 117.72(18) . . ? O3 Pb1 O10 131.1(3) . . ? O12 Pb1 O10 114.35(19) . . ? O11 Pb1 O10 161.7(2) . . ? O12 V1 O8 100.5(3) 1_545 4_565 ? O12 V1 O2 98.7(3) 1_545 . ? O8 V1 O2 92.9(3) 4_565 . ? O12 V1 O6 99.3(3) 1_545 . ? O8 V1 O6 159.3(3) 4_565 . ? O2 V1 O6 89.8(2) . . ? O12 V1 O10 96.4(3) 1_545 2_645 ? O8 V1 O10 87.7(3) 4_565 2_645 ? O2 V1 O10 164.5(2) . 2_645 ? O6 V1 O10 84.4(3) . 2_645 ? O12 V1 O13 179.6(3) 1_545 . ? O8 V1 O13 79.2(2) 4_565 . ? O2 V1 O13 81.6(2) . . ? O6 V1 O13 81.0(2) . . ? O10 V1 O13 83.3(2) 2_645 . ? O9 V2 O1 102.3(3) 1_545 . ? O9 V2 O7 101.6(3) 1_545 4_566 ? O1 V2 O7 91.1(3) . 4_566 ? O9 V2 O5 101.9(3) 1_545 . ? O1 V2 O5 89.1(2) . . ? O7 V2 O5 155.9(2) 4_566 . ? O9 V2 O4 94.8(3) 1_545 2_545 ? O1 V2 O4 162.3(2) . 2_545 ? O7 V2 O4 90.0(3) 4_566 2_545 ? O5 V2 O4 82.8(3) . 2_545 ? O9 V2 O11 171.5(3) 1_545 2_545 ? O1 V2 O11 86.1(2) . 2_545 ? O7 V2 O11 76.8(2) 4_566 2_545 ? O5 V2 O11 79.1(3) . 2_545 ? O4 V2 O11 76.9(2) 2_545 2_545 ? O8 P1 O1 113.5(4) . . ? O8 P1 O6 104.8(4) . . ? O1 P1 O6 112.2(3) . . ? O8 P1 O10 111.9(3) . . ? O1 P1 O10 104.6(3) . . ? O6 P1 O10 110.0(4) . . ? O7 P2 O2 113.7(4) . . ? O7 P2 O5 105.6(4) . . ? O2 P2 O5 112.4(3) . . ? O7 P2 O4 112.1(3) . . ? O2 P2 O4 103.1(3) . . ? O5 P2 O4 110.0(4) . . ? P1 O1 V2 134.4(3) . . ? P2 O2 V1 130.5(3) . . ? P2 O4 V2 136.7(3) . 2 ? P2 O4 Pb1 108.1(3) . . ? V2 O4 Pb1 115.2(2) 2 . ? P2 O5 V2 136.5(4) . . ? P1 O6 V1 136.2(4) . . ? P2 O7 V2 141.4(4) . 4_565 ? P1 O8 V1 146.2(4) . 4_566 ? P1 O10 V1 131.0(3) . 2_655 ? P1 O10 Pb1 110.1(3) . . ? V1 O10 Pb1 112.3(2) 2_655 . ? V2 O11 Pb1 97.63(19) 2 . ? V1 O12 Pb1 160.0(4) 1_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 P1 O1 V2 -63.0(6) . . . . ? O6 P1 O1 V2 55.5(6) . . . . ? O10 P1 O1 V2 174.7(5) . . . . ? O9 V2 O1 P1 -7.3(6) 1_545 . . . ? O7 V2 O1 P1 94.9(5) 4_566 . . . ? O5 V2 O1 P1 -109.2(5) . . . . ? O4 V2 O1 P1 -171.7(6) 2_545 . . . ? O11 V2 O1 P1 171.6(5) 2_545 . . . ? O7 P2 O2 V1 -70.8(5) . . . . ? O5 P2 O2 V1 49.2(6) . . . . ? O4 P2 O2 V1 167.6(4) . . . . ? O12 V1 O2 P2 -9.2(5) 1_545 . . . ? O8 V1 O2 P2 91.9(5) 4_565 . . . ? O6 V1 O2 P2 -108.6(5) . . . . ? O10 V1 O2 P2 -176.4(8) 2_645 . . . ? O13 V1 O2 P2 170.5(5) . . . . ? O7 P2 O4 V2 43.3(7) . . . 2 ? O2 P2 O4 V2 166.0(5) . . . 2 ? O5 P2 O4 V2 -73.9(6) . . . 2 ? O7 P2 O4 Pb1 -134.2(4) . . . . ? O2 P2 O4 Pb1 -11.5(4) . . . . ? O5 P2 O4 Pb1 108.5(4) . . . . ? O3 Pb1 O4 P2 84.8(4) . . . . ? O12 Pb1 O4 P2 130.8(3) . . . . ? O11 Pb1 O4 P2 156.5(4) . . . . ? O10 Pb1 O4 P2 -44.0(4) . . . . ? O3 Pb1 O4 V2 -93.3(3) . . . 2 ? O12 Pb1 O4 V2 -47.4(4) . . . 2 ? O11 Pb1 O4 V2 -21.6(3) . . . 2 ? O10 Pb1 O4 V2 137.8(3) . . . 2 ? O7 P2 O5 V2 168.8(6) . . . . ? O2 P2 O5 V2 44.2(7) . . . . ? O4 P2 O5 V2 -70.0(6) . . . . ? O9 V2 O5 P2 -103.9(6) 1_545 . . . ? O1 V2 O5 P2 -1.5(6) . . . . ? O7 V2 O5 P2 89.1(8) 4_566 . . . ? O4 V2 O5 P2 162.7(6) 2_545 . . . ? O11 V2 O5 P2 84.7(6) 2_545 . . . ? O8 P1 O6 V1 159.0(6) . . . . ? O1 P1 O6 V1 35.5(7) . . . . ? O10 P1 O6 V1 -80.5(6) . . . . ? O12 V1 O6 P1 -89.7(6) 1_545 . . . ? O8 V1 O6 P1 106.8(8) 4_565 . . . ? O2 V1 O6 P1 9.1(6) . . . . ? O10 V1 O6 P1 174.7(6) 2_645 . . . ? O13 V1 O6 P1 90.7(6) . . . . ? O2 P2 O7 V2 -41.1(7) . . . 4_565 ? O5 P2 O7 V2 -164.8(6) . . . 4_565 ? O4 P2 O7 V2 75.3(7) . . . 4_565 ? O1 P1 O8 V1 -45.0(8) . . . 4_566 ? O6 P1 O8 V1 -167.7(7) . . . 4_566 ? O10 P1 O8 V1 73.1(8) . . . 4_566 ? O8 P1 O10 V1 52.4(6) . . . 2_655 ? O1 P1 O10 V1 175.6(5) . . . 2_655 ? O6 P1 O10 V1 -63.7(6) . . . 2_655 ? O8 P1 O10 Pb1 -159.0(3) . . . . ? O1 P1 O10 Pb1 -35.8(4) . . . . ? O6 P1 O10 Pb1 84.9(4) . . . . ? O4 Pb1 O10 P1 6.5(4) . . . . ? O3 Pb1 O10 P1 -87.3(4) . . . . ? O12 Pb1 O10 P1 -169.0(3) . . . . ? O11 Pb1 O10 P1 95.0(6) . . . . ? O4 Pb1 O10 V1 161.3(2) . . . 2_655 ? O3 Pb1 O10 V1 67.6(4) . . . 2_655 ? O12 Pb1 O10 V1 -14.2(4) . . . 2_655 ? O11 Pb1 O10 V1 -110.2(5) . . . 2_655 ? O4 Pb1 O11 V2 17.3(2) . . . 2 ? O3 Pb1 O11 V2 101.2(3) . . . 2 ? O12 Pb1 O11 V2 175.7(3) . . . 2 ? O10 Pb1 O11 V2 -80.7(5) . . . 2 ? O4 Pb1 O12 V1 -165.5(10) . . . 1_565 ? O3 Pb1 O12 V1 -117.2(12) . . . 1_565 ? O11 Pb1 O12 V1 169.9(12) . . . 1_565 ? O10 Pb1 O12 V1 9.4(12) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.420 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.259 # Attachment '- PbVO2PO4.cif' data_difabs _database_code_depnum_ccdc_archive 'CCDC 881579' #TrackingRef '- PbVO2PO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'O18 P3 Pb3 V3' _chemical_formula_weight 1155.30 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' P P 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M 'p n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 9.7136(19) _cell_length_b 13.824(3) _cell_length_c 11.003(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1477.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 816 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.80 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 36.309 _exptl_absorpt_correction_type none _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1763 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1763 _reflns_number_gt 1374 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00056(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1763 _refine_ls_number_parameters 134 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.101 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb01 Pb 0.91064(4) 0.10977(3) 0.11898(4) 0.01229(16) Uani 1 1 d U . . Pb02 Pb 1.03632(8) 0.2500 0.48906(9) 0.0333(2) Uani 1 2 d SU . . V003 V 1.28959(17) 0.01844(12) 0.09632(18) 0.0086(4) Uani 1 1 d U . . V004 V 1.1218(3) -0.2500 0.1854(3) 0.0139(6) Uani 1 2 d SU . . P005 P 1.1035(3) -0.04952(19) 0.3256(3) 0.0069(5) Uani 1 1 d U . . P006 P 1.2178(4) 0.2500 0.2110(4) 0.0072(8) Uani 1 2 d SU . . O007 O 1.0694(10) 0.2500 0.1715(12) 0.013(2) Uani 1 2 d SU . . O008 O 1.2224(10) 0.2500 0.3534(11) 0.013(2) Uani 1 2 d SU . . O009 O 0.9935(7) 0.0282(5) 0.3175(7) 0.0108(15) Uani 1 1 d U . . O010 O 1.2879(11) -0.2500 0.1881(15) 0.032(3) Uani 1 2 d SU . . O011 O 1.0510(7) -0.1403(6) 0.2552(8) 0.0176(18) Uani 1 1 d U . . O012 O 1.0773(13) -0.2500 0.0425(11) 0.023(3) Uani 1 2 d SU . . O013 O 1.3230(7) -0.0909(5) 0.0442(8) 0.0129(16) Uani 1 1 d U . . O014 O 1.2389(6) -0.0149(5) 0.2701(7) 0.0096(15) Uani 1 1 d U . . O015 O 1.1307(7) 0.0321(5) 0.0502(8) 0.0135(16) Uani 1 1 d U . . O017 O 1.1256(7) -0.0844(5) 0.4573(7) 0.0105(15) Uani 1 1 d U . . O018 O 1.3012(7) 0.1607(5) 0.1701(8) 0.0133(16) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb01 0.0125(2) 0.0120(2) 0.0124(2) -0.00089(18) 0.00069(18) 0.00019(15) Pb02 0.0336(4) 0.0309(4) 0.0356(5) 0.000 0.0188(4) 0.000 V003 0.0065(8) 0.0102(8) 0.0091(10) -0.0025(7) -0.0004(8) -0.0004(7) V004 0.0205(14) 0.0125(13) 0.0085(15) 0.000 0.0013(12) 0.000 P005 0.0054(11) 0.0101(12) 0.0051(13) 0.0000(11) 0.0014(11) -0.0002(10) P006 0.0067(16) 0.0075(16) 0.007(2) 0.000 -0.0015(16) 0.000 O007 0.008(4) 0.009(4) 0.022(7) 0.000 -0.006(4) 0.000 O008 0.017(5) 0.014(5) 0.008(5) 0.000 0.000(4) 0.000 O009 0.015(3) 0.008(3) 0.010(4) -0.001(3) 0.006(3) 0.007(3) O010 0.013(5) 0.023(6) 0.059(11) 0.000 0.007(6) 0.000 O011 0.014(4) 0.019(4) 0.020(5) -0.017(4) 0.000(3) 0.000(3) O012 0.049(7) 0.017(6) 0.004(5) 0.000 -0.001(5) 0.000 O013 0.015(4) 0.009(3) 0.015(4) -0.002(3) 0.001(3) -0.001(3) O014 0.004(3) 0.017(3) 0.008(4) -0.002(3) 0.003(3) -0.001(3) O015 0.011(3) 0.020(4) 0.009(4) -0.004(3) 0.001(3) 0.000(3) O017 0.007(3) 0.019(4) 0.006(4) -0.002(3) -0.002(3) -0.001(3) O018 0.012(3) 0.010(3) 0.017(4) -0.001(3) 0.002(3) 0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pb01 O015 2.509(7) . ? Pb01 O007 2.544(6) . ? Pb01 O009 2.586(8) . ? Pb01 O012 2.632(9) 5_755 ? Pb01 O018 2.648(9) 6_556 ? Pb01 O008 2.682(7) 6_556 ? Pb01 O014 2.692(7) 6_556 ? Pb01 O015 2.734(8) 5_755 ? Pb02 O008 2.344(11) . ? Pb02 O013 2.659(7) 7_866 ? Pb02 O013 2.659(7) 2_755 ? V003 O015 1.635(7) . ? V003 O013 1.649(7) . ? V003 O017 1.962(8) 2_754 ? V003 O014 2.027(8) . ? V003 O018 2.130(7) . ? V003 O009 2.200(7) 6_656 ? V004 O010 1.613(11) . ? V004 O012 1.631(13) . ? V004 O011 1.834(8) . ? V004 O011 1.834(8) 8 ? P005 O009 1.518(7) . ? P005 O014 1.527(7) . ? P005 O017 1.542(8) . ? P005 O011 1.561(8) . ? P006 O007 1.506(10) . ? P006 O018 1.544(7) 8_565 ? P006 O018 1.544(7) . ? P006 O008 1.567(12) . ? O007 Pb01 2.544(6) 8_565 ? O008 Pb01 2.682(7) 3 ? O008 Pb01 2.682(7) 6_656 ? O009 V003 2.200(7) 6_556 ? O012 Pb01 2.632(9) 4_745 ? O012 Pb01 2.632(9) 5_755 ? O013 Pb02 2.659(7) 2_754 ? O014 Pb01 2.692(7) 6_656 ? O015 Pb01 2.734(8) 5_755 ? O017 V003 1.962(8) 2_755 ? O018 Pb01 2.648(9) 6_656 ? 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 O015 Pb01 O007 83.0(3) . . ? O015 Pb01 O009 78.6(2) . . ? O007 Pb01 O009 87.2(3) . . ? O015 Pb01 O012 94.2(3) . 5_755 ? O007 Pb01 O012 64.2(4) . 5_755 ? O009 Pb01 O012 151.3(3) . 5_755 ? O015 Pb01 O018 136.1(2) . 6_556 ? O007 Pb01 O018 80.9(3) . 6_556 ? O009 Pb01 O018 60.0(2) . 6_556 ? O012 Pb01 O018 114.4(3) 5_755 6_556 ? O015 Pb01 O008 157.6(3) . 6_556 ? O007 Pb01 O008 80.6(2) . 6_556 ? O009 Pb01 O008 115.6(3) . 6_556 ? O012 Pb01 O008 64.8(3) 5_755 6_556 ? O018 Pb01 O008 55.6(3) 6_556 6_556 ? O015 Pb01 O014 113.0(2) . 6_556 ? O007 Pb01 O014 139.5(3) . 6_556 ? O009 Pb01 O014 62.0(2) . 6_556 ? O012 Pb01 O014 143.6(3) 5_755 6_556 ? O018 Pb01 O014 61.6(2) 6_556 6_556 ? O008 Pb01 O014 89.4(2) 6_556 6_556 ? O015 Pb01 O015 67.2(3) . 5_755 ? O007 Pb01 O015 142.2(3) . 5_755 ? O009 Pb01 O015 108.0(2) . 5_755 ? O012 Pb01 O015 94.3(3) 5_755 5_755 ? O018 Pb01 O015 136.8(2) 6_556 5_755 ? O008 Pb01 O015 119.7(3) 6_556 5_755 ? O014 Pb01 O015 76.0(2) 6_556 5_755 ? O008 Pb02 O013 75.5(2) . 7_866 ? O008 Pb02 O013 75.5(2) . 2_755 ? O013 Pb02 O013 111.6(3) 7_866 2_755 ? O015 V003 O013 100.6(4) . . ? O015 V003 O017 95.8(4) . 2_754 ? O013 V003 O017 94.1(4) . 2_754 ? O015 V003 O014 95.1(3) . . ? O013 V003 O014 99.6(4) . . ? O017 V003 O014 160.5(3) 2_754 . ? O015 V003 O018 93.5(3) . . ? O013 V003 O018 165.5(3) . . ? O017 V003 O018 81.1(3) 2_754 . ? O014 V003 O018 82.2(3) . . ? O015 V003 O009 167.5(3) . 6_656 ? O013 V003 O009 91.7(3) . 6_656 ? O017 V003 O009 86.0(3) 2_754 6_656 ? O014 V003 O009 80.0(3) . 6_656 ? O018 V003 O009 74.4(3) . 6_656 ? O010 V004 O012 106.4(8) . . ? O010 V004 O011 111.6(4) . . ? O012 V004 O011 107.7(4) . . ? O010 V004 O011 111.6(4) . 8 ? O012 V004 O011 107.7(4) . 8 ? O011 V004 O011 111.6(6) . 8 ? O009 P005 O014 111.1(4) . . ? O009 P005 O017 112.0(4) . . ? O014 P005 O017 110.7(4) . . ? O009 P005 O011 108.1(4) . . ? O014 P005 O011 109.5(4) . . ? O017 P005 O011 105.1(5) . . ? O007 P006 O018 114.7(4) . 8_565 ? O007 P006 O018 114.7(4) . . ? O018 P006 O018 106.2(6) 8_565 . ? O007 P006 O008 108.4(7) . . ? O018 P006 O008 106.1(4) 8_565 . ? O018 P006 O008 106.1(4) . . ? P006 O007 Pb01 130.24(17) . . ? P006 O007 Pb01 130.24(17) . 8_565 ? Pb01 O007 Pb01 99.3(3) . 8_565 ? P006 O008 Pb02 127.9(6) . . ? P006 O008 Pb01 97.6(4) . 3 ? Pb02 O008 Pb01 117.0(3) . 3 ? P006 O008 Pb01 97.6(4) . 6_656 ? Pb02 O008 Pb01 117.0(3) . 6_656 ? Pb01 O008 Pb01 92.6(3) 3 6_656 ? P005 O009 V003 124.4(4) . 6_556 ? P005 O009 Pb01 125.3(4) . . ? V003 O009 Pb01 96.4(3) 6_556 . ? P005 O011 V004 138.6(5) . . ? V004 O012 Pb01 129.7(3) . 4_745 ? V004 O012 Pb01 129.7(3) . 5_755 ? Pb01 O012 Pb01 94.9(4) 4_745 5_755 ? V003 O013 Pb02 159.8(4) . 2_754 ? P005 O014 V003 131.1(5) . . ? P005 O014 Pb01 123.6(4) . 6_656 ? V003 O014 Pb01 97.6(3) . 6_656 ? V003 O015 Pb01 139.4(4) . . ? V003 O015 Pb01 105.5(3) . 5_755 ? Pb01 O015 Pb01 112.8(3) . 5_755 ? P005 O017 V003 130.2(5) . 2_755 ? P006 O018 V003 145.3(5) . . ? P006 O018 Pb01 99.6(4) . 6_656 ? V003 O018 Pb01 96.3(3) . 6_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.206 _refine_diff_density_min -4.740 _refine_diff_density_rms 0.424