# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Z.-G Ye' 'R. Batchelor' 'Hai-Yan Guo.' 'Shao-Yu Mao.' 'Yanping Mao.' 'Zhao-Xiong Xie.' 'Lan-sun Zheng.' _publ_contact_author_name 'Z.-G Ye' _publ_contact_author_email ZYE@SFU.CA _publ_section_title ; Polymorphic Structures and Properties of Lead Chromium Phosphate Pb3Cr2(PO4)4 ; # Attachment 'p21c_and_p41212.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 732710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cr2 O16 P4 Pb3' _chemical_formula_weight 1105.45 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' Cr Cr 0.3209 0.6236 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 8.9342(18) _cell_length_b 8.9680(18) _cell_length_c 9.2495(18) _cell_angle_alpha 90.00 _cell_angle_beta 116.74(3) _cell_angle_gamma 90.00 _cell_volume 661.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 21.5 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate-like _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 40.196 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2624 _exptl_absorpt_correction_T_max 0.3518 _exptl_absorpt_process_details 'NRCVAX (Gabe, 1989)' _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 Enraf-Nonius _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1hour _diffrn_standards_decay_% <2% _diffrn_reflns_number 1242 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.54 _reflns_number_total 1242 _reflns_number_gt 1091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NRCVAX (Gabe, 1989)' _computing_cell_refinement 'NRCVAX (Gabe, 1989)' _computing_data_reduction 'NRCVAX (Gabe, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2.1a(Brandenburg, 1996-2001)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.1006P)^2^+3.0587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1242 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.441 _refine_ls_restrained_S_all 1.441 _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 0.29936(10) 0.20698(9) 0.52651(8) 0.0121(4) Uani 1 1 d . . . Pb2 Pb 0.0000 0.5000 0.5000 0.0091(4) Uani 1 2 d S . . Cr3 Cr 0.2475(4) 0.6307(3) 0.2447(3) 0.0042(7) Uiso 1 1 d . . . P6 P 0.5744(6) 0.0897(6) 0.8582(6) 0.0056(10) Uiso 1 1 d . . . P7 P -0.0196(6) 0.1376(5) 0.6553(5) 0.0038(10) Uiso 1 1 d . . . O1 O 0.1615(17) 0.5919(16) 0.0126(16) 0.008(3) Uiso 1 1 d . . . O2 O 0.0943(18) 0.7062(14) 0.7390(16) 0.005(3) Uiso 1 1 d . . . O3 O 0.5903(19) 0.2168(15) 0.7562(16) 0.008(3) Uiso 1 1 d . . . O11 O 0.3881(18) 0.0447(16) 0.7582(15) 0.007(3) Uiso 1 1 d . . . O13 O 0.0831(19) 0.4951(15) 0.2568(16) 0.010(3) Uiso 1 1 d . . . O21 O 0.3900(19) 0.6491(16) 0.4791(16) 0.010(3) Uiso 1 1 d . . . O22 O 0.1034(19) 0.2453(17) 0.6349(16) 0.010(3) Uiso 1 1 d . . . O23 O 0.3141(19) 0.4593(17) 0.6301(17) 0.013(3) Uiso 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 Pb1 0.0146(6) 0.0127(6) 0.0049(5) 0.0016(3) 0.0007(4) 0.0029(3) Pb2 0.0098(6) 0.0080(7) 0.0068(6) -0.0004(4) 0.0014(4) 0.0002(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 Pb1 O22 2.402(14) . ? Pb1 O11 2.411(13) . ? Pb1 O23 2.437(15) . ? Pb1 O3 2.512(15) . ? Pb1 P6 3.126(5) . ? Pb1 Pb2 3.6781(9) . ? Pb2 O23 2.533(15) 3_566 ? Pb2 O23 2.533(15) . ? Pb2 O22 2.567(15) 3_566 ? Pb2 O22 2.567(15) . ? Pb2 O13 2.667(13) 3_566 ? Pb2 O13 2.667(13) . ? Pb2 O2 2.709(13) . ? Pb2 O2 2.709(13) 3_566 ? Pb2 Pb1 3.6781(9) 3_566 ? Cr3 O13 1.949(15) . ? Cr3 O1 1.958(13) . ? Cr3 O21 1.966(14) . ? Cr3 O11 1.981(14) 4_565 ? Cr3 O2 1.988(14) 4_575 ? Cr3 O3 1.995(14) 3_666 ? P6 O21 1.490(14) 2_646 ? P6 O23 1.509(16) 2_646 ? P6 O3 1.526(14) . ? P6 O11 1.550(15) . ? P7 O2 1.539(14) 2_546 ? P7 O22 1.537(16) . ? P7 O13 1.538(15) 4_566 ? P7 O1 1.554(14) 2_545 ? O1 P7 1.554(14) 2 ? O2 P7 1.539(14) 2_556 ? O2 Cr3 1.988(14) 4_576 ? O3 Cr3 1.995(14) 3_666 ? O11 Cr3 1.981(14) 4_566 ? O13 P7 1.538(15) 4_565 ? O21 P6 1.490(14) 2_656 ? O23 P6 1.509(16) 2_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 O22 Pb1 O11 74.1(5) . . ? O22 Pb1 O23 67.9(5) . . ? O11 Pb1 O23 105.8(5) . . ? O22 Pb1 O3 108.3(5) . . ? O11 Pb1 O3 57.9(5) . . ? O23 Pb1 O3 77.4(5) . . ? O22 Pb1 P6 92.1(4) . . ? O11 Pb1 P6 29.0(3) . . ? O23 Pb1 P6 92.7(4) . . ? O3 Pb1 P6 28.9(3) . . ? O22 Pb1 Pb2 44.0(4) . . ? O11 Pb1 Pb2 115.4(3) . . ? O23 Pb1 Pb2 43.3(4) . . ? O3 Pb1 Pb2 118.4(3) . . ? P6 Pb1 Pb2 122.19(9) . . ? O23 Pb2 O23 180.000(1) 3_566 . ? O23 Pb2 O22 64.0(5) 3_566 3_566 ? O23 Pb2 O22 116.0(5) . 3_566 ? O23 Pb2 O22 116.0(5) 3_566 . ? O23 Pb2 O22 64.0(5) . . ? O22 Pb2 O22 180.000(2) 3_566 . ? O23 Pb2 O13 74.3(4) 3_566 3_566 ? O23 Pb2 O13 105.7(4) . 3_566 ? O22 Pb2 O13 102.7(4) 3_566 3_566 ? O22 Pb2 O13 77.3(4) . 3_566 ? O23 Pb2 O13 105.7(4) 3_566 . ? O23 Pb2 O13 74.3(4) . . ? O22 Pb2 O13 77.3(4) 3_566 . ? O22 Pb2 O13 102.7(4) . . ? O13 Pb2 O13 180.000(1) 3_566 . ? O23 Pb2 O2 99.2(4) 3_566 . ? O23 Pb2 O2 80.8(4) . . ? O22 Pb2 O2 72.6(4) 3_566 . ? O22 Pb2 O2 107.4(4) . . ? O13 Pb2 O2 53.3(4) 3_566 . ? O13 Pb2 O2 126.7(4) . . ? O23 Pb2 O2 80.8(4) 3_566 3_566 ? O23 Pb2 O2 99.2(4) . 3_566 ? O22 Pb2 O2 107.4(4) 3_566 3_566 ? O22 Pb2 O2 72.6(4) . 3_566 ? O13 Pb2 O2 126.7(4) 3_566 3_566 ? O13 Pb2 O2 53.3(4) . 3_566 ? O2 Pb2 O2 180.000(1) . 3_566 ? O23 Pb2 Pb1 41.3(3) 3_566 3_566 ? O23 Pb2 Pb1 138.7(3) . 3_566 ? O22 Pb2 Pb1 40.6(3) 3_566 3_566 ? O22 Pb2 Pb1 139.4(3) . 3_566 ? O13 Pb2 Pb1 64.8(3) 3_566 3_566 ? O13 Pb2 Pb1 115.2(3) . 3_566 ? O2 Pb2 Pb1 61.1(3) . 3_566 ? O2 Pb2 Pb1 118.9(3) 3_566 3_566 ? O23 Pb2 Pb1 138.7(3) 3_566 . ? O23 Pb2 Pb1 41.3(3) . . ? O22 Pb2 Pb1 139.4(3) 3_566 . ? O22 Pb2 Pb1 40.6(3) . . ? O13 Pb2 Pb1 115.2(3) 3_566 . ? O13 Pb2 Pb1 64.8(3) . . ? O2 Pb2 Pb1 118.9(3) . . ? O2 Pb2 Pb1 61.1(3) 3_566 . ? Pb1 Pb2 Pb1 180.0 3_566 . ? O13 Cr3 O1 91.0(6) . . ? O13 Cr3 O21 96.9(6) . . ? O1 Cr3 O21 164.6(6) . . ? O13 Cr3 O11 88.5(6) . 4_565 ? O1 Cr3 O11 81.6(6) . 4_565 ? O21 Cr3 O11 85.4(6) . 4_565 ? O13 Cr3 O2 86.2(6) . 4_575 ? O1 Cr3 O2 100.1(6) . 4_575 ? O21 Cr3 O2 93.7(6) . 4_575 ? O11 Cr3 O2 174.4(6) 4_565 4_575 ? O13 Cr3 O3 174.6(5) . 3_666 ? O1 Cr3 O3 92.6(6) . 3_666 ? O21 Cr3 O3 80.5(6) . 3_666 ? O11 Cr3 O3 95.9(6) 4_565 3_666 ? O2 Cr3 O3 89.3(6) 4_575 3_666 ? O21 P6 O23 111.8(8) 2_646 2_646 ? O21 P6 O3 108.7(8) 2_646 . ? O23 P6 O3 112.4(8) 2_646 . ? O21 P6 O11 112.3(8) 2_646 . ? O23 P6 O11 109.7(8) 2_646 . ? O3 P6 O11 101.5(8) . . ? O21 P6 Pb1 126.0(6) 2_646 . ? O23 P6 Pb1 122.2(6) 2_646 . ? O3 P6 Pb1 52.6(6) . . ? O11 P6 Pb1 49.0(5) . . ? O2 P7 O22 111.4(8) 2_546 . ? O2 P7 O13 103.4(7) 2_546 4_566 ? O22 P7 O13 107.3(8) . 4_566 ? O2 P7 O1 110.4(8) 2_546 2_545 ? O22 P7 O1 110.5(8) . 2_545 ? O13 P7 O1 113.6(8) 4_566 2_545 ? P7 O1 Cr3 142.2(9) 2 . ? P7 O2 Cr3 140.1(8) 2_556 4_576 ? P7 O2 Pb2 100.4(6) 2_556 . ? Cr3 O2 Pb2 118.8(6) 4_576 . ? P6 O3 Cr3 141.6(9) . 3_666 ? P6 O3 Pb1 98.5(7) . . ? Cr3 O3 Pb1 119.9(6) 3_666 . ? P6 O11 Cr3 136.4(9) . 4_566 ? P6 O11 Pb1 102.0(7) . . ? Cr3 O11 Pb1 118.5(6) 4_566 . ? P7 O13 Cr3 134.9(8) 4_565 . ? P7 O13 Pb2 102.2(7) 4_565 . ? Cr3 O13 Pb2 122.8(6) . . ? P6 O21 Cr3 145.3(10) 2_656 . ? P7 O22 Pb1 131.1(8) . . ? P7 O22 Pb2 119.9(8) . . ? Pb1 O22 Pb2 95.4(5) . . ? P6 O23 Pb1 131.7(8) 2_656 . ? P6 O23 Pb2 118.5(8) 2_656 . ? Pb1 O23 Pb2 95.4(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.559 _refine_diff_density_min -4.646 _refine_diff_density_rms 0.791 #===END data_p41212 _database_code_depnum_ccdc_archive 'CCDC 732711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cr2 O16 P4 Pb3' _chemical_formula_weight 1105.45 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' Cr Cr 0.3209 0.6236 '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 tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 8.9455(13) _cell_length_b 8.9455(13) _cell_length_c 16.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1321.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 20 _cell_measurement_theta_max 24 _exptl_crystal_description plate-like _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 40.274 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1265 _exptl_absorpt_correction_T_max 0.2945 _exptl_absorpt_process_details 'NRCVAX (Gabe, 1989)' _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 Enraf-Nonius _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1hour _diffrn_standards_decay_% <2% _diffrn_reflns_number 1063 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1063 _reflns_number_gt 909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NRCVAX (Gabe, 1989)' _computing_cell_refinement 'NRCVAX (Gabe, 1989)' _computing_data_reduction 'NRCVAX (Gabe, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2.1a(Brandenburg, 1996-2001)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.1538P)^2^+8.0513P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(5) _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 0.68(6) _refine_ls_number_reflns 1063 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.07594(15) 0.34357(15) 0.26362(8) 0.0125(6) Uani 1 1 d . . . Pb2 Pb 0.13416(16) 0.13416(16) 0.0000 0.0092(6) Uani 1 2 d S . . Cr1 Cr 0.5007(6) 0.2643(5) 0.1213(4) 0.0043(11) Uiso 1 1 d . . . P1 P 0.2750(10) -0.0056(9) 0.1714(5) 0.0060(17) Uiso 1 1 d . . . P2 P -0.0446(10) 0.2261(9) 0.4292(5) 0.0040(16) Uiso 1 1 d . . . O3 O 0.628(3) 0.082(3) 0.1186(14) 0.006(5) Uiso 1 1 d . . . O4 O 0.330(3) 0.126(2) 0.1178(13) 0.004(5) Uiso 1 1 d . . . O5 O 0.666(3) 0.421(3) 0.1278(13) 0.007(5) Uiso 1 1 d . . . O6 O 0.514(2) 0.229(2) 0.2382(13) 0.009(5) Uiso 1 1 d . . . O7 O 0.324(3) 0.380(3) 0.3151(14) 0.011(5) Uiso 1 1 d . . . O8 O 0.109(3) 0.593(3) 0.3126(14) 0.011(5) Uiso 1 1 d . . . O9 O 0.354(3) 0.427(3) 0.1285(13) 0.009(5) Uiso 1 1 d . . . O10 O 0.544(3) 0.290(3) 0.0021(14) 0.014(5) Uiso 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 Pb1 0.0135(8) 0.0154(8) 0.0086(8) 0.0017(6) 0.0006(5) -0.0029(5) Pb2 0.0089(7) 0.0089(7) 0.0098(9) 0.0006(5) -0.0006(5) 0.0001(6) _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 Pb1 O8 2.39(2) . ? Pb1 O7 2.40(2) . ? Pb1 O3 2.41(2) 8_565 ? Pb1 O5 2.47(2) 3_545 ? Pb1 P2 3.120(8) . ? Pb1 Pb2 3.6788(13) 3 ? Pb2 O8 2.55(2) 4_454 ? Pb2 O8 2.55(2) 5_545 ? Pb2 O7 2.54(2) 5_545 ? Pb2 O7 2.54(2) 4_454 ? Pb2 O4 2.62(2) . ? Pb2 O4 2.62(2) 7 ? Pb2 O9 2.73(2) 4_454 ? Pb2 O9 2.73(2) 5_545 ? Pb2 Pb1 3.6788(13) 4_454 ? Pb2 Pb1 3.6788(13) 5_545 ? Cr1 O6 1.96(2) . ? Cr1 O9 1.96(2) . ? Cr1 O4 1.96(2) . ? Cr1 O3 1.99(2) . ? Cr1 O10 2.02(2) . ? Cr1 O5 2.04(2) . ? P1 O10 1.52(2) 3_545 ? P1 O8 1.52(2) 8_655 ? P1 O9 1.54(2) 5_545 ? P1 O4 1.55(2) . ? P2 O5 1.49(2) 3_545 ? P2 O7 1.51(2) 6_455 ? P2 O6 1.52(2) 6_455 ? P2 O3 1.56(2) 8_565 ? O3 P2 1.56(2) 8_655 ? O3 Pb1 2.41(2) 8_655 ? O5 P2 1.49(2) 4_554 ? O5 Pb1 2.47(2) 4_554 ? O6 P2 1.52(2) 6 ? O7 P2 1.51(2) 6 ? O7 Pb2 2.54(2) 3 ? O8 P1 1.52(2) 8_565 ? O8 Pb2 2.55(2) 3 ? O9 P1 1.54(2) 5 ? O9 Pb2 2.73(2) 3 ? O10 P1 1.52(2) 4_554 ? 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 O8 Pb1 O7 68.9(8) . . ? O8 Pb1 O3 72.7(8) . 8_565 ? O7 Pb1 O3 103.9(8) . 8_565 ? O8 Pb1 O5 110.0(7) . 3_545 ? O7 Pb1 O5 78.9(8) . 3_545 ? O3 Pb1 O5 57.2(7) 8_565 3_545 ? O8 Pb1 P2 93.5(6) . . ? O7 Pb1 P2 93.2(6) . . ? O3 Pb1 P2 29.3(5) 8_565 . ? O5 Pb1 P2 28.0(6) 3_545 . ? O8 Pb1 Pb2 43.5(6) . 3 ? O7 Pb1 Pb2 43.4(6) . 3 ? O3 Pb1 Pb2 112.8(6) 8_565 3 ? O5 Pb1 Pb2 119.7(5) 3_545 3 ? P2 Pb1 Pb2 122.35(15) . 3 ? O8 Pb2 O8 115.1(11) 4_454 5_545 ? O8 Pb2 O7 178.9(7) 4_454 5_545 ? O8 Pb2 O7 64.4(8) 5_545 5_545 ? O8 Pb2 O7 64.4(8) 4_454 4_454 ? O8 Pb2 O7 178.9(7) 5_545 4_454 ? O7 Pb2 O7 116.1(11) 5_545 4_454 ? O8 Pb2 O4 79.6(7) 4_454 . ? O8 Pb2 O4 72.2(7) 5_545 . ? O7 Pb2 O4 101.1(7) 5_545 . ? O7 Pb2 O4 106.8(7) 4_454 . ? O8 Pb2 O4 72.2(7) 4_454 7 ? O8 Pb2 O4 79.6(7) 5_545 7 ? O7 Pb2 O4 106.8(7) 5_545 7 ? O7 Pb2 O4 101.1(7) 4_454 7 ? O4 Pb2 O4 126.0(10) . 7 ? O8 Pb2 O9 99.5(7) 4_454 4_454 ? O8 Pb2 O9 108.7(7) 5_545 4_454 ? O7 Pb2 O9 79.9(7) 5_545 4_454 ? O7 Pb2 O9 72.4(7) 4_454 4_454 ? O4 Pb2 O9 179.0(7) . 4_454 ? O4 Pb2 O9 53.8(7) 7 4_454 ? O8 Pb2 O9 108.7(7) 4_454 5_545 ? O8 Pb2 O9 99.5(7) 5_545 5_545 ? O7 Pb2 O9 72.4(7) 5_545 5_545 ? O7 Pb2 O9 79.9(7) 4_454 5_545 ? O4 Pb2 O9 53.8(7) . 5_545 ? O4 Pb2 O9 179.0(7) 7 5_545 ? O9 Pb2 O9 126.3(10) 4_454 5_545 ? O8 Pb2 Pb1 40.3(6) 4_454 4_454 ? O8 Pb2 Pb1 139.8(6) 5_545 4_454 ? O7 Pb2 Pb1 139.4(5) 5_545 4_454 ? O7 Pb2 Pb1 40.4(5) 4_454 4_454 ? O4 Pb2 Pb1 116.5(5) . 4_454 ? O4 Pb2 Pb1 63.6(5) 7 4_454 ? O9 Pb2 Pb1 62.4(5) 4_454 4_454 ? O9 Pb2 Pb1 117.5(5) 5_545 4_454 ? O8 Pb2 Pb1 139.8(6) 4_454 5_545 ? O8 Pb2 Pb1 40.3(6) 5_545 5_545 ? O7 Pb2 Pb1 40.4(5) 5_545 5_545 ? O7 Pb2 Pb1 139.4(5) 4_454 5_545 ? O4 Pb2 Pb1 63.6(5) . 5_545 ? O4 Pb2 Pb1 116.5(5) 7 5_545 ? O9 Pb2 Pb1 117.5(5) 4_454 5_545 ? O9 Pb2 Pb1 62.4(5) 5_545 5_545 ? Pb1 Pb2 Pb1 179.87(8) 4_454 5_545 ? O6 Cr1 O9 95.8(10) . . ? O6 Cr1 O4 88.7(9) . . ? O9 Cr1 O4 87.0(10) . . ? O6 Cr1 O3 81.7(10) . . ? O9 Cr1 O3 172.5(10) . . ? O4 Cr1 O3 85.9(10) . . ? O6 Cr1 O10 165.1(10) . . ? O9 Cr1 O10 96.0(10) . . ? O4 Cr1 O10 101.0(10) . . ? O3 Cr1 O10 87.8(10) . . ? O6 Cr1 O5 90.7(9) . . ? O9 Cr1 O5 88.4(10) . . ? O4 Cr1 O5 175.3(10) . . ? O3 Cr1 O5 98.6(11) . . ? O10 Cr1 O5 80.5(10) . . ? O10 P1 O8 108.7(14) 3_545 8_655 ? O10 P1 O9 107.4(13) 3_545 5_545 ? O8 P1 O9 115.7(14) 8_655 5_545 ? O10 P1 O4 113.5(13) 3_545 . ? O8 P1 O4 108.4(14) 8_655 . ? O9 P1 O4 103.3(12) 5_545 . ? O5 P2 O7 112.5(14) 3_545 6_455 ? O5 P2 O6 110.4(13) 3_545 6_455 ? O7 P2 O6 112.2(13) 6_455 6_455 ? O5 P2 O3 99.8(12) 3_545 8_565 ? O7 P2 O3 113.1(13) 6_455 8_565 ? O6 P2 O3 108.1(13) 6_455 8_565 ? O5 P2 Pb1 50.8(9) 3_545 . ? O7 P2 Pb1 122.3(10) 6_455 . ? O6 P2 Pb1 125.4(9) 6_455 . ? O3 P2 Pb1 49.3(8) 8_565 . ? P2 O3 Cr1 131.6(14) 8_655 . ? P2 O3 Pb1 101.4(10) 8_655 8_655 ? Cr1 O3 Pb1 121.3(11) . 8_655 ? P1 O4 Cr1 134.9(14) . . ? P1 O4 Pb2 103.4(11) . . ? Cr1 O4 Pb2 121.7(10) . . ? P2 O5 Cr1 143.1(14) 4_554 . ? P2 O5 Pb1 101.2(11) 4_554 4_554 ? Cr1 O5 Pb1 115.7(10) . 4_554 ? P2 O6 Cr1 145.4(15) 6 . ? P2 O7 Pb1 131.0(14) 6 . ? P2 O7 Pb2 118.3(14) 6 3 ? Pb1 O7 Pb2 96.2(8) . 3 ? P1 O8 Pb1 134.9(14) 8_565 . ? P1 O8 Pb2 120.6(13) 8_565 3 ? Pb1 O8 Pb2 96.2(8) . 3 ? P1 O9 Cr1 139.3(15) 5 . ? P1 O9 Pb2 99.0(11) 5 3 ? Cr1 O9 Pb2 121.3(10) . 3 ? P1 O10 Cr1 139.2(16) 4_554 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 4.020 _refine_diff_density_min -3.677 _refine_diff_density_rms 0.800 #===END