data_pbna _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As Cl7 O3 Pb5' _chemical_formula_weight 1407.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' '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+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 16.894(2) _cell_length_b 10.9135(15) _cell_length_c 16.760(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3090.1(7) _cell_formula_units_Z 8 _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 6.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4688 _exptl_absorpt_coefficient_mu 57.620 _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 50938 _diffrn_reflns_av_R_equivalents 0.1763 _diffrn_reflns_av_sigmaI/netI 0.1412 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 36.22 _reflns_number_total 7159 _reflns_number_gt 4952 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0614P)^2^+74.2023P] 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 0.00042(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7159 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Pb1 Pb 0.63854(3) 0.91802(5) 0.69372(3) 0.00997(12) Uani 1 1 d . . . Pb2 Pb 0.63979(3) 0.30367(4) 0.69943(3) 0.00950(12) Uani 1 1 d . . . Pb3 Pb 0.60787(3) 0.10384(5) 0.89609(3) 0.01152(12) Uani 1 1 d . . . Pb4 Pb 0.78948(3) 0.11977(5) 0.55211(4) 0.01303(13) Uani 1 1 d . . . Pb5 Pb 0.43385(3) 0.62600(5) 0.59510(4) 0.01302(13) Uani 1 1 d . . . As As 0.78307(8) 0.11105(11) 0.75379(9) 0.0042(2) Uani 1 1 d . . . Cl1 Cl 0.5000 0.1106(6) 0.7500 0.0192(11) Uani 1 2 d S . . Cl2 Cl 0.7502(2) 0.1254(3) 0.9840(3) 0.0159(7) Uani 1 1 d . . . Cl3 Cl 0.5668(2) 0.4631(3) 0.5714(2) 0.0146(6) Uani 1 1 d . . . Cl4 Cl 0.5560(2) 0.7859(4) 0.5571(2) 0.0165(7) Uani 1 1 d . . . Cl5 Cl 0.6199(3) 0.1211(4) 0.5688(3) 0.0185(7) Uani 1 1 d . . . Cl6 Cl 0.6523(3) 0.8569(4) 0.8591(3) 0.0253(9) Uani 1 1 d . . . Cl7 Cl 0.6275(3) 0.3676(3) 0.8712(3) 0.0209(8) Uani 1 1 d . . . Cl8 Cl 0.5000 0.6529(14) 0.7500 0.065(3) Uani 1 2 d S . . O1 O 0.6810(6) 0.1187(8) 0.7789(6) 0.0085(17) Uiso 1 1 d . . . O2 O 0.7781(6) 0.2343(9) 0.6815(6) 0.0082(17) Uiso 1 1 d . . . O3 O 0.7730(6) 0.9908(9) 0.6832(6) 0.0101(18) 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 0.0052(2) 0.0085(2) 0.0162(3) -0.00186(18) -0.00129(17) 0.00131(15) Pb2 0.0058(2) 0.0064(2) 0.0163(3) 0.00124(17) -0.00218(17) 0.00112(14) Pb3 0.0091(2) 0.0127(2) 0.0127(2) -0.00275(18) 0.00255(18) -0.00075(16) Pb4 0.0138(3) 0.0091(2) 0.0162(3) -0.00246(18) 0.0039(2) 0.00038(17) Pb5 0.0089(2) 0.0129(2) 0.0172(3) -0.00138(19) 0.00079(19) -0.00280(16) As 0.0013(5) 0.0009(5) 0.0103(6) -0.0002(4) -0.0022(4) 0.0002(4) Cl1 0.0015(18) 0.035(3) 0.021(3) 0.000 -0.0017(17) 0.000 Cl2 0.0086(15) 0.0095(14) 0.030(2) 0.0028(13) -0.0040(13) 0.0043(11) Cl3 0.0081(14) 0.0166(16) 0.0191(16) 0.0042(13) -0.0025(12) 0.0058(11) Cl4 0.0163(16) 0.0177(16) 0.0155(16) 0.0021(13) 0.0016(13) -0.0128(13) Cl5 0.0165(17) 0.0194(18) 0.0195(18) 0.0010(14) -0.0017(14) -0.0013(13) Cl6 0.048(3) 0.0067(14) 0.0208(19) 0.0019(14) 0.0132(19) -0.0006(15) Cl7 0.034(2) 0.0082(14) 0.0203(19) -0.0039(13) 0.0030(17) 0.0055(14) Cl8 0.036(5) 0.143(11) 0.014(3) 0.000 -0.003(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 Pb1 O3 2.412(10) . ? Pb1 O2 2.459(10) 7_765 ? Pb1 O1 2.711(10) 1_565 ? Pb1 Cl6 2.860(5) . ? Pb1 Cl4 3.044(4) . ? Pb1 Cl5 3.064(4) 1_565 ? Pb2 O2 2.475(10) . ? Pb2 O1 2.517(10) . ? Pb2 O3 2.533(10) 7_755 ? Pb2 Cl7 2.969(4) . ? Pb2 Cl5 2.979(4) . ? Pb2 Cl3 3.025(4) . ? Pb3 O1 2.326(10) . ? Pb3 Cl2 2.830(4) . ? Pb3 Cl6 2.866(4) 1_545 ? Pb3 Cl7 2.928(4) . ? Pb3 Cl1 3.0531(7) . ? Pb3 Cl4 3.082(4) 8_566 ? Pb4 O2 2.510(10) . ? Pb4 O3 2.624(11) 1_545 ? Pb4 Cl5 2.878(4) . ? Pb4 Cl2 2.984(3) 8 ? Pb4 Cl3 2.987(4) 7_755 ? Pb4 Cl2 3.080(4) 2_654 ? Pb5 Cl4 2.776(3) . ? Pb5 Cl8 2.8417(17) . ? Pb5 Cl3 2.892(3) . ? Pb5 Cl3 2.955(4) 5_666 ? Pb5 Cl6 3.009(4) 4_656 ? Pb5 Cl7 3.057(4) 4_656 ? As O3 1.776(10) 1_545 ? As O1 1.777(10) . ? As O2 1.813(10) . ? Cl1 Pb3 3.0531(7) 4_656 ? Cl2 Pb4 2.984(3) 8_556 ? Cl2 Pb4 3.080(4) 2_655 ? Cl3 Pb5 2.955(4) 5_666 ? Cl3 Pb4 2.987(4) 7_765 ? Cl4 Pb3 3.082(4) 8_565 ? Cl5 Pb1 3.064(4) 1_545 ? Cl6 Pb3 2.866(4) 1_565 ? Cl6 Pb5 3.009(4) 4_656 ? Cl7 Pb5 3.057(4) 4_656 ? Cl8 Pb5 2.8417(17) 4_656 ? O1 Pb1 2.711(10) 1_545 ? O2 Pb1 2.459(10) 7_755 ? O3 As 1.776(10) 1_565 ? O3 Pb2 2.533(10) 7_765 ? O3 Pb4 2.624(10) 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 O3 Pb1 O2 73.9(3) . 7_765 ? O3 Pb1 O1 61.6(3) . 1_565 ? O2 Pb1 O1 123.5(3) 7_765 1_565 ? O3 Pb1 Cl6 94.1(3) . . ? O2 Pb1 Cl6 81.0(3) 7_765 . ? O1 Pb1 Cl6 69.9(2) 1_565 . ? O3 Pb1 Cl4 122.2(3) . . ? O2 Pb1 Cl4 79.2(2) 7_765 . ? O1 Pb1 Cl4 154.2(2) 1_565 . ? Cl6 Pb1 Cl4 130.96(11) . . ? O3 Pb1 Cl5 79.0(3) . 1_565 ? O2 Pb1 Cl5 126.3(3) 7_765 1_565 ? O1 Pb1 Cl5 78.6(2) 1_565 1_565 ? Cl6 Pb1 Cl5 147.02(11) . 1_565 ? Cl4 Pb1 Cl5 77.40(11) . 1_565 ? O2 Pb2 O1 63.8(3) . . ? O2 Pb2 O3 71.6(3) . 7_755 ? O1 Pb2 O3 122.9(3) . 7_755 ? O2 Pb2 Cl7 104.8(3) . . ? O1 Pb2 Cl7 72.2(2) . . ? O3 Pb2 Cl7 87.4(3) 7_755 . ? O2 Pb2 Cl5 79.2(2) . . ? O1 Pb2 Cl5 83.3(2) . . ? O3 Pb2 Cl5 121.7(3) 7_755 . ? Cl7 Pb2 Cl5 149.51(11) . . ? O2 Pb2 Cl3 118.3(2) . . ? O1 Pb2 Cl3 161.7(2) . . ? O3 Pb2 Cl3 72.4(2) 7_755 . ? Cl7 Pb2 Cl3 121.60(11) . . ? Cl5 Pb2 Cl3 79.50(11) . . ? O1 Pb3 Cl2 89.0(3) . . ? O1 Pb3 Cl6 75.1(2) . 1_545 ? Cl2 Pb3 Cl6 88.19(13) . 1_545 ? O1 Pb3 Cl7 75.6(2) . . ? Cl2 Pb3 Cl7 84.04(12) . . ? Cl6 Pb3 Cl7 149.80(13) 1_545 . ? O1 Pb3 Cl1 68.8(3) . . ? Cl2 Pb3 Cl1 157.33(10) . . ? Cl6 Pb3 Cl1 90.31(15) 1_545 . ? Cl7 Pb3 Cl1 85.97(15) . . ? O1 Pb3 Cl4 149.7(2) . 8_566 ? Cl2 Pb3 Cl4 75.71(12) . 8_566 ? Cl6 Pb3 Cl4 129.12(11) 1_545 8_566 ? Cl7 Pb3 Cl4 76.91(12) . 8_566 ? Cl1 Pb3 Cl4 121.54(9) . 8_566 ? O2 Pb4 O3 62.3(3) . 1_545 ? O2 Pb4 Cl5 80.6(2) . . ? O3 Pb4 Cl5 79.4(2) 1_545 . ? O2 Pb4 Cl2 139.5(2) . 8 ? O3 Pb4 Cl2 79.4(2) 1_545 8 ? Cl5 Pb4 Cl2 79.65(11) . 8 ? O2 Pb4 Cl3 104.7(2) . 7_755 ? O3 Pb4 Cl3 71.9(2) 1_545 7_755 ? Cl5 Pb4 Cl3 143.25(10) . 7_755 ? Cl2 Pb4 Cl3 73.08(10) 8 7_755 ? O2 Pb4 Cl2 81.6(2) . 2_654 ? O3 Pb4 Cl2 140.5(2) 1_545 2_654 ? Cl5 Pb4 Cl2 79.35(10) . 2_654 ? Cl2 Pb4 Cl2 128.28(14) 8 2_654 ? Cl3 Pb4 Cl2 137.20(10) 7_755 2_654 ? Cl4 Pb5 Cl8 81.5(2) . . ? Cl4 Pb5 Cl3 77.16(12) . . ? Cl8 Pb5 Cl3 83.3(2) . . ? Cl4 Pb5 Cl3 89.62(11) . 5_666 ? Cl8 Pb5 Cl3 153.93(18) . 5_666 ? Cl3 Pb5 Cl3 70.79(11) . 5_666 ? Cl4 Pb5 Cl6 83.76(13) . 4_656 ? Cl8 Pb5 Cl6 82.6(3) . 4_656 ? Cl3 Pb5 Cl6 157.72(13) . 4_656 ? Cl3 Pb5 Cl6 120.97(12) 5_666 4_656 ? Cl4 Pb5 Cl7 150.96(13) . 4_656 ? Cl8 Pb5 Cl7 93.4(3) . 4_656 ? Cl3 Pb5 Cl7 73.85(12) . 4_656 ? Cl3 Pb5 Cl7 82.52(11) 5_666 4_656 ? Cl6 Pb5 Cl7 124.14(13) 4_656 4_656 ? O3 As O1 95.7(5) 1_545 . ? O3 As O2 95.6(5) 1_545 . ? O1 As O2 94.5(4) . . ? Pb3 Cl1 Pb3 177.2(2) . 4_656 ? Pb3 Cl2 Pb4 108.28(11) . 8_556 ? Pb3 Cl2 Pb4 94.78(9) . 2_655 ? Pb4 Cl2 Pb4 135.75(17) 8_556 2_655 ? Pb5 Cl3 Pb5 109.21(11) . 5_666 ? Pb5 Cl3 Pb4 107.11(12) . 7_765 ? Pb5 Cl3 Pb4 95.12(11) 5_666 7_765 ? Pb5 Cl3 Pb2 124.93(14) . . ? Pb5 Cl3 Pb2 118.82(12) 5_666 . ? Pb4 Cl3 Pb2 94.29(10) 7_765 . ? Pb5 Cl4 Pb1 117.77(13) . . ? Pb5 Cl4 Pb3 131.10(14) . 8_565 ? Pb1 Cl4 Pb3 110.09(10) . 8_565 ? Pb4 Cl5 Pb2 87.87(11) . . ? Pb4 Cl5 Pb1 87.75(11) . 1_545 ? Pb2 Cl5 Pb1 88.30(12) . 1_545 ? Pb1 Cl6 Pb3 88.22(12) . 1_565 ? Pb1 Cl6 Pb5 113.79(16) . 4_656 ? Pb3 Cl6 Pb5 127.29(16) 1_565 4_656 ? Pb3 Cl7 Pb2 85.12(10) . . ? Pb3 Cl7 Pb5 147.36(17) . 4_656 ? Pb2 Cl7 Pb5 114.82(14) . 4_656 ? Pb5 Cl8 Pb5 168.1(6) . 4_656 ? As O1 Pb3 135.4(6) . . ? As O1 Pb2 100.4(4) . . ? Pb3 O1 Pb2 110.8(4) . . ? As O1 Pb1 95.4(4) . 1_545 ? Pb3 O1 Pb1 104.4(3) . 1_545 ? Pb2 O1 Pb1 107.2(4) . 1_545 ? As O2 Pb1 121.5(5) . 7_755 ? As O2 Pb2 100.9(4) . . ? Pb1 O2 Pb2 106.3(4) 7_755 . ? As O2 Pb4 101.8(4) . . ? Pb1 O2 Pb4 115.7(4) 7_755 . ? Pb2 O2 Pb4 109.3(4) . . ? As O3 Pb1 106.6(5) 1_565 . ? As O3 Pb2 117.9(5) 1_565 7_765 ? Pb1 O3 Pb2 105.9(4) . 7_765 ? As O3 Pb4 98.7(4) 1_565 1_565 ? Pb1 O3 Pb4 109.8(4) . 1_565 ? Pb2 O3 Pb4 117.4(4) 7_765 1_565 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 36.22 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 8.110 _refine_diff_density_min -7.768 _refine_diff_density_rms 1.089