data_paratimroseite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Cu2 O7 Pb Te' _chemical_formula_weight 575.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 '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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'H' 'H' 0.0000 0.0000 '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' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 5.1943(4) _cell_length_b 9.6198(10) _cell_length_c 11.6745(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 583.35(9) _cell_formula_units_Z 4 _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 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 40.901 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2605 _exptl_absorpt_correction_T_max 0.7914 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _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 4431 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.0884 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 24.70 _reflns_number_total 984 _reflns_number_gt 842 _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^)+(0.0000P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(16) _refine_ls_number_reflns 984 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.002 _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 Pb Pb 0.48658(16) 0.37646(9) 0.71849(6) 0.0199(2) Uani 1 1 d . . . Te Te 0.8986(2) 0.49499(15) 0.49034(11) 0.0124(3) Uani 1 1 d . . . Cu1 Cu 0.3802(4) 0.6442(3) 0.5457(2) 0.0148(6) Uani 1 1 d . . . Cu2 Cu 0.4205(4) 0.3513(3) 0.4222(2) 0.0145(6) Uani 1 1 d . . . O1 O 0.608(3) 0.5291(15) 0.3914(11) 0.016(3) Uani 1 1 d . . . O2 O 0.195(3) 0.4730(15) 0.5870(11) 0.012(3) Uiso 1 1 d . . . O3 O 0.544(3) 0.8222(14) 0.5322(11) 0.023(4) Uiso 1 1 d . . . O4 O 0.741(3) 0.3179(14) 0.5188(12) 0.022(4) Uani 1 1 d . . . O5 O 0.415(3) 0.5715(15) 0.8624(11) 0.017(4) Uani 1 1 d . . . O6 O 0.696(3) 0.5660(16) 0.6193(11) 0.019(4) Uani 1 1 d . . . OW O 0.473(3) 0.7477(14) 0.2604(10) 0.024(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 Pb 0.0182(4) 0.0224(5) 0.0192(4) 0.0041(4) 0.0004(4) 0.0012(5) Te 0.0100(6) 0.0117(7) 0.0155(7) -0.0003(6) -0.0003(5) 0.0000(6) Cu1 0.0090(12) 0.0157(15) 0.0196(14) 0.0012(11) -0.0011(9) 0.0007(12) Cu2 0.0090(13) 0.0159(15) 0.0184(14) 0.0005(11) -0.0015(10) -0.0012(11) O1 0.018(8) 0.015(8) 0.016(8) 0.002(6) -0.012(6) -0.007(7) O4 0.018(8) 0.007(8) 0.041(10) 0.005(7) 0.003(7) -0.010(6) O5 0.007(8) 0.032(10) 0.012(8) -0.003(6) 0.000(5) 0.000(7) O6 0.018(8) 0.028(10) 0.011(8) -0.002(6) 0.010(6) 0.001(7) OW 0.043(10) 0.008(8) 0.020(8) -0.005(6) 0.008(7) -0.003(8) _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 O2 2.348(13) . ? Pb O6 2.419(14) . ? Pb O5 2.546(13) . ? Pb OW 2.714(17) 4_565 ? Pb O4 2.737(15) . ? Pb O3 2.962(13) 3_646 ? Pb O1 3.055(15) 4_665 ? Pb OW 3.090(17) 4_665 ? Pb O5 3.124(14) 3_646 ? Pb Cu1 3.318(3) . ? Pb Te 3.4579(15) 4_665 ? Pb Cu2 3.484(3) . ? Pb Cu2 3.547(2) 2_556 ? Pb O4 3.578(15) 2_456 ? Pb Te 3.6022(15) . ? Pb Cu1 3.613(3) 3_646 ? Pb O6 3.662(15) 3_646 ? Pb O1 3.799(13) 4_565 ? Pb Cu2 4.018(2) 2_456 ? Pb O2 4.093(13) 1_655 ? Te O5 1.892(13) 4_664 ? Te O2 1.920(13) 1_655 ? Te O4 1.920(13) . ? Te O3 1.932(14) 2_566 ? Te O1 1.929(13) . ? Te O6 1.959(13) . ? Te Cu2 2.952(3) . ? Te Cu1 2.955(3) 1_655 ? Te Cu1 3.119(3) . ? Te Cu2 3.145(3) 1_655 ? Te Pb 3.4580(15) 4_664 ? Te Cu2 3.486(3) 2_556 ? Cu1 O3 1.919(14) . ? Cu1 O2 1.967(14) . ? Cu1 O3 1.995(14) 2_466 ? Cu1 O6 2.000(15) . ? Cu1 O1 2.423(15) . ? Cu1 Te 2.955(3) 1_455 ? Cu2 O4 1.999(14) 2_456 ? Cu2 O1 2.001(15) . ? Cu2 O5 2.018(13) 4_564 ? Cu2 O4 2.034(14) . ? Cu2 OW 2.418(13) 3_645 ? Cu2 O2 2.539(13) . ? O1 OW 2.693(19) . ? O1 Pb 3.055(14) 4_664 ? O1 Cu1 3.524(14) 2_566 ? O1 Pb 3.799(13) 4_564 ? O2 Te 1.920(13) 1_455 ? O2 Cu2 3.432(14) 2_456 ? O2 Pb 4.093(13) 1_455 ? O3 Te 1.932(14) 2_466 ? O3 Cu1 1.995(14) 2_566 ? O3 Pb 2.962(13) 3_656 ? O3 Cu1 3.580(13) 2_466 ? O3 Cu2 3.738(14) 2_566 ? O4 Cu2 1.999(14) 2_556 ? O4 Pb 3.578(15) 2_556 ? O4 Cu2 3.721(13) 1_655 ? O5 Te 1.892(13) 4_665 ? O5 Cu2 2.018(13) 4_565 ? O5 Pb 3.124(14) 3_656 ? O5 Cu1 3.351(14) 4_565 ? O5 Cu2 3.600(14) 4_665 ? O5 Cu2 3.781(14) 3_656 ? O6 Cu1 3.520(14) 2_566 ? O6 Pb 3.662(14) 3_656 ? O6 Cu1 3.731(14) 1_655 ? O6 Cu2 4.136(14) 4_665 ? O6 OW 4.685(19) . ? OW Cu2 2.418(13) 3_655 ? OW Pb 2.714(17) 4_564 ? OW Pb 3.090(17) 4_664 ? OW Cu1 3.268(16) 2_566 ? OW Cu1 3.960(15) 2_466 ? 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 O2 Pb O6 71.3(5) . . ? O2 Pb O5 92.6(5) . . ? O6 Pb O5 80.0(5) . . ? O2 Pb OW 74.0(4) . 4_565 ? O6 Pb OW 144.5(5) . 4_565 ? O5 Pb OW 94.4(4) . 4_565 ? O2 Pb O4 80.5(4) . . ? O6 Pb O4 62.0(4) . . ? O5 Pb O4 141.7(4) . . ? OW Pb O4 119.1(4) 4_565 . ? O2 Pb O3 132.6(4) . 3_646 ? O6 Pb O3 128.9(4) . 3_646 ? O5 Pb O3 58.2(4) . 3_646 ? OW Pb O3 72.4(4) 4_565 3_646 ? O4 Pb O3 145.8(4) . 3_646 ? O2 Pb O1 139.4(4) . 4_665 ? O6 Pb O1 77.4(4) . 4_665 ? O5 Pb O1 56.3(4) . 4_665 ? OW Pb O1 128.2(4) 4_565 4_665 ? O4 Pb O1 107.0(4) . 4_665 ? O3 Pb O1 55.9(3) 3_646 4_665 ? O2 Pb OW 147.4(4) . 4_665 ? O6 Pb OW 87.6(5) . 4_665 ? O5 Pb OW 108.3(4) . 4_665 ? OW Pb OW 126.9(5) 4_565 4_665 ? O4 Pb OW 67.5(4) . 4_665 ? O3 Pb OW 79.9(4) 3_646 4_665 ? O1 Pb OW 52.0(4) 4_665 4_665 ? O2 Pb O5 106.2(4) . 3_646 ? O6 Pb O5 119.3(4) . 3_646 ? O5 Pb O5 156.3(3) . 3_646 ? OW Pb O5 77.6(4) 4_565 3_646 ? O4 Pb O5 58.0(4) . 3_646 ? O3 Pb O5 98.1(4) 3_646 3_646 ? O1 Pb O5 111.5(4) 4_665 3_646 ? OW Pb O5 62.4(4) 4_665 3_646 ? O2 Pb Cu1 35.7(3) . . ? O6 Pb Cu1 36.8(4) . . ? O5 Pb Cu1 78.8(3) . . ? OW Pb Cu1 107.8(3) 4_565 . ? O4 Pb Cu1 73.9(3) . . ? O3 Pb Cu1 136.5(3) 3_646 . ? O1 Pb Cu1 106.6(3) 4_665 . ? OW Pb Cu1 123.2(3) 4_665 . ? O5 Pb Cu1 124.9(2) 3_646 . ? O2 Pb Te 124.7(3) . 4_665 ? O6 Pb Te 95.3(3) . 4_665 ? O5 Pb Te 32.4(3) . 4_665 ? OW Pb Te 98.2(3) 4_565 4_665 ? O4 Pb Te 140.6(3) . 4_665 ? O3 Pb Te 33.9(3) 3_646 4_665 ? O1 Pb Te 33.7(2) 4_665 4_665 ? OW Pb Te 80.6(2) 4_665 4_665 ? O5 Pb Te 125.8(2) 3_646 4_665 ? Cu1 Pb Te 108.02(5) . 4_665 ? O2 Pb Cu2 46.8(3) . . ? O6 Pb Cu2 67.8(3) . . ? O5 Pb Cu2 133.8(3) . . ? OW Pb Cu2 93.5(3) 4_565 . ? O4 Pb Cu2 35.7(3) . . ? O3 Pb Cu2 163.4(3) 3_646 . ? O1 Pb Cu2 138.1(2) 4_665 . ? OW Pb Cu2 102.7(2) 4_665 . ? O5 Pb Cu2 69.6(2) 3_646 . ? Cu1 Pb Cu2 55.52(6) . . ? Te Pb Cu2 162.36(6) 4_665 . ? O2 Pb Cu2 110.6(3) . 2_556 ? O6 Pb Cu2 87.6(3) . 2_556 ? O5 Pb Cu2 148.6(3) . 2_556 ? OW Pb Cu2 111.8(3) 4_565 2_556 ? O4 Pb Cu2 34.1(3) . 2_556 ? O3 Pb Cu2 112.4(3) 3_646 2_556 ? O1 Pb Cu2 93.0(3) 4_665 2_556 ? OW Pb Cu2 42.0(2) 4_665 2_556 ? O5 Pb Cu2 34.5(2) 3_646 2_556 ? Cu1 Pb Cu2 107.67(6) . 2_556 ? Te Pb Cu2 122.45(5) 4_665 2_556 ? Cu2 Pb Cu2 63.88(5) . 2_556 ? O2 Pb O4 58.0(4) . 2_456 ? O6 Pb O4 100.6(4) . 2_456 ? O5 Pb O4 147.5(4) . 2_456 ? OW Pb O4 66.1(4) 4_565 2_456 ? O4 Pb O4 53.50(18) . 2_456 ? O3 Pb O4 130.5(4) 3_646 2_456 ? O1 Pb O4 155.9(3) 4_665 2_456 ? OW Pb O4 104.2(3) 4_665 2_456 ? O5 Pb O4 48.2(3) 3_646 2_456 ? Cu1 Pb O4 82.8(2) . 2_456 ? Te Pb O4 163.5(2) 4_665 2_456 ? Cu2 Pb O4 32.9(2) . 2_456 ? Cu2 Pb O4 63.0(2) 2_556 2_456 ? O2 Pb Te 77.0(3) . . ? O6 Pb Te 30.7(3) . . ? O5 Pb Te 110.0(3) . . ? OW Pb Te 142.7(3) 4_565 . ? O4 Pb Te 31.7(3) . . ? O3 Pb Te 144.5(3) 3_646 . ? O1 Pb Te 89.1(2) 4_665 . ? OW Pb Te 72.5(3) 4_665 . ? O5 Pb Te 88.6(2) 3_646 . ? Cu1 Pb Te 53.39(5) . . ? Te Pb Te 117.58(2) 4_665 . ? Cu2 Pb Te 49.20(4) . . ? Cu2 Pb Te 58.36(5) 2_556 . ? O4 Pb Te 78.8(2) 2_456 . ? O2 Pb Cu1 150.0(3) . 3_646 ? O6 Pb Cu1 138.1(3) . 3_646 ? O5 Pb Cu1 88.9(3) . 3_646 ? OW Pb Cu1 76.0(3) 4_565 3_646 ? O4 Pb Cu1 115.4(3) . 3_646 ? O3 Pb Cu1 32.0(3) 3_646 3_646 ? O1 Pb Cu1 63.2(3) 4_665 3_646 ? OW Pb Cu1 57.7(3) 4_665 3_646 ? O5 Pb Cu1 67.6(2) 3_646 3_646 ? Cu1 Pb Cu1 167.26(7) . 3_646 ? Te Pb Cu1 59.25(5) 4_665 3_646 ? Cu2 Pb Cu1 137.09(7) . 3_646 ? Cu2 Pb Cu1 81.33(6) 2_556 3_646 ? O4 Pb Cu1 109.6(2) 2_456 3_646 ? Te Pb Cu1 130.20(5) . 3_646 ? O2 Pb O6 119.5(4) . 3_646 ? O6 Pb O6 168.3(2) . 3_646 ? O5 Pb O6 102.8(4) . 3_646 ? OW Pb O6 47.1(4) 4_565 3_646 ? O4 Pb O6 113.4(4) . 3_646 ? O3 Pb O6 48.2(3) 3_646 3_646 ? O1 Pb O6 94.6(3) 4_665 3_646 ? OW Pb O6 80.7(4) 4_665 3_646 ? O5 Pb O6 55.5(3) 3_646 3_646 ? Cu1 Pb O6 154.7(2) . 3_646 ? Te Pb O6 82.0(2) 4_665 3_646 ? Cu2 Pb O6 115.5(2) . 3_646 ? Cu2 Pb O6 84.3(2) 2_556 3_646 ? O4 Pb O6 83.2(3) 2_456 3_646 ? Te Pb O6 142.6(2) . 3_646 ? Cu1 Pb O6 31.9(2) 3_646 3_646 ? O2 Pb O1 74.2(4) . 4_565 ? O6 Pb O1 116.1(4) . 4_565 ? O5 Pb O1 49.8(4) . 4_565 ? OW Pb O1 45.1(4) 4_565 4_565 ? O4 Pb O1 153.3(4) . 4_565 ? O3 Pb O1 58.4(3) 3_646 4_565 ? O1 Pb O1 97.9(3) 4_665 4_565 ? OW Pb O1 138.3(3) 4_665 4_565 ? O5 Pb O1 121.2(3) 3_646 4_565 ? Cu1 Pb O1 90.1(2) . 4_565 ? Te Pb O1 64.3(2) 4_665 4_565 ? Cu2 Pb O1 117.6(2) . 4_565 ? Cu2 Pb O1 155.5(2) 2_556 4_565 ? O4 Pb O1 104.2(3) 2_456 4_565 ? Te Pb O1 143.1(2) . 4_565 ? Cu1 Pb O1 84.2(2) 3_646 4_565 ? O6 Pb O1 73.1(3) 3_646 4_565 ? O2 Pb Cu2 58.4(3) . 2_456 ? O6 Pb Cu2 123.0(3) . 2_456 ? O5 Pb Cu2 124.4(3) . 2_456 ? OW Pb Cu2 35.9(3) 4_565 2_456 ? O4 Pb Cu2 83.8(3) . 2_456 ? O3 Pb Cu2 105.5(3) 3_646 2_456 ? O1 Pb Cu2 159.5(3) 4_665 2_456 ? OW Pb Cu2 121.3(3) 4_665 2_456 ? O5 Pb Cu2 59.0(3) 3_646 2_456 ? Cu1 Pb Cu2 93.02(6) . 2_456 ? Te Pb Cu2 134.14(5) 4_665 2_456 ? Cu2 Pb Cu2 58.94(5) . 2_456 ? Cu2 Pb Cu2 86.49(6) 2_556 2_456 ? O4 Pb Cu2 30.4(2) 2_456 2_456 ? Te Pb Cu2 107.76(4) . 2_456 ? Cu1 Pb Cu2 96.58(5) 3_646 2_456 ? O6 Pb Cu2 65.0(2) 3_646 2_456 ? O1 Pb Cu2 75.7(2) 4_565 2_456 ? O2 Pb O2 104.2(4) . 1_655 ? O6 Pb O2 40.9(4) . 1_655 ? O5 Pb O2 102.2(4) . 1_655 ? OW Pb O2 163.4(4) 4_565 1_655 ? O4 Pb O2 45.1(3) . 1_655 ? O3 Pb O2 117.2(3) 3_646 1_655 ? O1 Pb O2 63.9(3) 4_665 1_655 ? OW Pb O2 48.0(3) 4_665 1_655 ? O5 Pb O2 87.3(3) 3_646 1_655 ? Cu1 Pb O2 75.25(19) . 1_655 ? Te Pb O2 96.20(19) 4_665 1_655 ? Cu2 Pb O2 74.47(18) . 1_655 ? Cu2 Pb O2 52.8(2) 2_556 1_655 ? O4 Pb O2 98.6(3) 2_456 1_655 ? Te Pb O2 27.97(18) . 1_655 ? Cu1 Pb O2 104.72(19) 3_646 1_655 ? O6 Pb O2 127.8(3) 3_646 1_655 ? O1 Pb O2 151.1(3) 4_565 1_655 ? Cu2 Pb O2 128.92(19) 2_456 1_655 ? O5 Te O2 90.9(6) 4_664 1_655 ? O5 Te O4 93.2(6) 4_664 . ? O2 Te O4 98.3(6) 1_655 . ? O5 Te O3 90.0(6) 4_664 2_566 ? O2 Te O3 82.4(6) 1_655 2_566 ? O4 Te O3 176.7(6) . 2_566 ? O5 Te O1 89.2(6) 4_664 . ? O2 Te O1 176.4(6) 1_655 . ? O4 Te O1 85.4(6) . . ? O3 Te O1 94.0(6) 2_566 . ? O5 Te O6 178.1(6) 4_664 . ? O2 Te O6 90.9(6) 1_655 . ? O4 Te O6 87.0(6) . . ? O3 Te O6 89.8(6) 2_566 . ? O1 Te O6 88.9(6) . . ? O5 Te Cu2 93.4(4) 4_664 . ? O2 Te Cu2 141.4(4) 1_655 . ? O4 Te Cu2 43.2(4) . . ? O3 Te Cu2 135.9(4) 2_566 . ? O1 Te Cu2 42.2(4) . . ? O6 Te Cu2 85.4(4) . . ? O5 Te Cu1 84.4(4) 4_664 1_655 ? O2 Te Cu1 41.1(4) 1_655 1_655 ? O4 Te Cu1 139.0(4) . 1_655 ? O3 Te Cu1 42.0(4) 2_566 1_655 ? O1 Te Cu1 135.3(4) . 1_655 ? O6 Te Cu1 96.7(4) . 1_655 ? Cu2 Te Cu1 176.92(9) . 1_655 ? O5 Te Cu1 139.6(4) 4_664 . ? O2 Te Cu1 128.4(4) 1_655 . ? O4 Te Cu1 90.2(4) . . ? O3 Te Cu1 86.9(4) 2_566 . ? O1 Te Cu1 51.0(4) . . ? O6 Te Cu1 38.5(4) . . ? Cu2 Te Cu1 62.92(7) . . ? Cu1 Te Cu1 117.52(10) 1_655 . ? O5 Te Cu2 37.8(4) 4_664 1_655 ? O2 Te Cu2 53.8(4) 1_655 1_655 ? O4 Te Cu2 91.3(4) . 1_655 ? O3 Te Cu2 91.7(4) 2_566 1_655 ? O1 Te Cu2 126.7(4) . 1_655 ? O6 Te Cu2 144.1(4) . 1_655 ? Cu2 Te Cu2 116.82(10) . 1_655 ? Cu1 Te Cu2 62.56(7) 1_655 1_655 ? Cu1 Te Cu2 177.13(8) . 1_655 ? O5 Te Pb 46.2(4) 4_664 4_664 ? O2 Te Pb 116.2(4) 1_655 4_664 ? O4 Te Pb 123.3(4) . 4_664 ? O3 Te Pb 58.8(4) 2_566 4_664 ? O1 Te Pb 61.6(4) . 4_664 ? O6 Te Pb 132.3(4) . 4_664 ? Cu2 Te Pb 93.75(6) . 4_664 ? Cu1 Te Pb 83.17(6) 1_655 4_664 ? Cu1 Te Pb 100.04(6) . 4_664 ? Cu2 Te Pb 77.09(5) 1_655 4_664 ? O5 Te Cu2 83.8(4) 4_664 2_556 ? O2 Te Cu2 72.3(4) 1_655 2_556 ? O4 Te Cu2 27.8(4) . 2_556 ? O3 Te Cu2 153.8(4) 2_566 2_556 ? O1 Te Cu2 111.3(4) . 2_556 ? O6 Te Cu2 97.2(4) . 2_556 ? Cu2 Te Cu2 70.04(6) . 2_556 ? Cu1 Te Cu2 111.87(8) 1_655 2_556 ? Cu1 Te Cu2 114.02(7) . 2_556 ? Cu2 Te Cu2 68.03(6) 1_655 2_556 ? Pb Te Cu2 127.22(6) 4_664 2_556 ? O3 Cu1 O2 169.7(6) . . ? O3 Cu1 O3 101.9(4) . 2_466 ? O2 Cu1 O3 79.6(6) . 2_466 ? O3 Cu1 O6 90.4(6) . . ? O2 Cu1 O6 89.0(6) . . ? O3 Cu1 O6 167.2(6) 2_466 . ? O3 Cu1 O1 97.5(5) . . ? O2 Cu1 O1 92.2(5) . . ? O3 Cu1 O1 99.4(5) 2_466 . ? O6 Cu1 O1 75.3(5) . . ? O3 Cu1 Te 142.2(4) . 1_455 ? O2 Cu1 Te 39.9(4) . 1_455 ? O3 Cu1 Te 40.4(4) 2_466 1_455 ? O6 Cu1 Te 127.3(4) . 1_455 ? O1 Cu1 Te 91.7(3) . 1_455 ? O4 Cu2 O1 170.2(6) 2_456 . ? O4 Cu2 O5 90.9(6) 2_456 4_564 ? O1 Cu2 O5 92.5(6) . 4_564 ? O4 Cu2 O4 93.6(3) 2_456 . ? O1 Cu2 O4 80.6(5) . . ? O5 Cu2 O4 162.8(6) 4_564 . ? O4 Cu2 OW 94.3(5) 2_456 3_645 ? O1 Cu2 OW 94.7(5) . 3_645 ? O5 Cu2 OW 92.5(6) 4_564 3_645 ? O4 Cu2 OW 103.7(6) . 3_645 ? O4 Cu2 O2 84.2(5) 2_456 . ? O1 Cu2 O2 88.1(5) . . ? O5 Cu2 O2 72.2(5) 4_564 . ? O4 Cu2 O2 91.7(5) . . ? OW Cu2 O2 164.6(5) 3_645 . ? Te O1 Cu2 97.3(6) . . ? Te O1 Cu1 90.8(5) . . ? Cu2 O1 Cu1 91.1(5) . . ? Te O1 OW 132.6(7) . . ? Cu2 O1 OW 130.0(7) . . ? Cu1 O1 OW 86.4(5) . . ? Te O1 Pb 84.6(5) . 4_664 ? Cu2 O1 Pb 135.1(6) . 4_664 ? Cu1 O1 Pb 133.8(6) . 4_664 ? OW O1 Pb 64.7(5) . 4_664 ? Te O1 Cu1 73.3(4) . 2_566 ? Cu2 O1 Cu1 156.9(6) . 2_566 ? Cu1 O1 Cu1 68.5(3) . 2_566 ? OW O1 Cu1 61.7(4) . 2_566 ? Pb O1 Cu1 66.2(3) 4_664 2_566 ? Te O1 Pb 174.2(7) . 4_564 ? Cu2 O1 Pb 84.5(4) . 4_564 ? Cu1 O1 Pb 83.6(4) . 4_564 ? OW O1 Pb 45.6(4) . 4_564 ? Pb O1 Pb 97.9(3) 4_664 4_564 ? Cu1 O1 Pb 102.9(4) 2_566 4_564 ? Te O1 Pb 60.4(3) . . ? Cu2 O1 Pb 57.1(3) . . ? Cu1 O1 Pb 53.3(3) . . ? OW O1 Pb 139.6(6) . . ? Pb O1 Pb 145.1(4) 4_664 . ? Cu1 O1 Pb 100.7(3) 2_566 . ? Pb O1 Pb 116.8(4) 4_564 . ? Te O2 Cu1 99.0(6) 1_455 . ? Te O2 Pb 160.9(7) 1_455 . ? Cu1 O2 Pb 100.1(6) . . ? Te O2 Cu2 88.6(5) 1_455 . ? Cu1 O2 Cu2 88.5(5) . . ? Pb O2 Cu2 90.8(5) . . ? Te O2 Cu2 75.4(4) 1_455 2_456 ? Cu1 O2 Cu2 163.0(6) . 2_456 ? Pb O2 Cu2 85.9(4) . 2_456 ? Cu2 O2 Cu2 75.4(3) . 2_456 ? Te O2 Pb 61.6(3) 1_455 1_455 ? Cu1 O2 Pb 136.2(6) . 1_455 ? Pb O2 Pb 104.2(4) . 1_455 ? Cu2 O2 Pb 126.5(5) . 1_455 ? Cu2 O2 Pb 55.4(2) 2_456 1_455 ? Te O3 Cu1 130.6(7) 2_466 . ? Te O3 Cu1 97.6(6) 2_466 2_566 ? Cu1 O3 Cu1 124.8(7) . 2_566 ? Te O3 Pb 87.3(5) 2_466 3_656 ? Cu1 O3 Pb 93.0(5) . 3_656 ? Cu1 O3 Pb 117.8(5) 2_566 3_656 ? Te O3 Cu1 60.5(4) 2_466 2_466 ? Cu1 O3 Cu1 71.0(4) . 2_466 ? Cu1 O3 Cu1 135.5(5) 2_566 2_466 ? Pb O3 Cu1 100.5(4) 3_656 2_466 ? Te O3 Cu2 57.2(3) 2_466 2_566 ? Cu1 O3 Cu2 166.0(6) . 2_566 ? Cu1 O3 Cu2 58.0(3) 2_566 2_566 ? Pb O3 Cu2 74.9(3) 3_656 2_566 ? Cu1 O3 Cu2 117.6(4) 2_466 2_566 ? Te O4 Cu2 125.6(7) . 2_556 ? Te O4 Cu2 96.5(6) . . ? Cu2 O4 Cu2 134.5(7) 2_556 . ? Te O4 Pb 99.8(6) . . ? Cu2 O4 Pb 95.7(5) 2_556 . ? Cu2 O4 Pb 92.6(5) . . ? Te O4 Pb 100.2(5) . 2_556 ? Cu2 O4 Pb 71.0(4) 2_556 2_556 ? Cu2 O4 Pb 86.9(5) . 2_556 ? Pb O4 Pb 159.9(5) . 2_556 ? Te O4 Cu1 58.3(4) . . ? Cu2 O4 Cu1 154.9(6) 2_556 . ? Cu2 O4 Cu1 59.7(4) . . ? Pb O4 Cu1 60.3(3) . . ? Pb O4 Cu1 134.1(4) 2_556 . ? Te O4 Cu2 57.7(3) . 1_655 ? Cu2 O4 Cu2 74.4(4) 2_556 1_655 ? Cu2 O4 Cu2 126.5(6) . 1_655 ? Pb O4 Cu2 134.2(5) . 1_655 ? Pb O4 Cu2 58.1(2) 2_556 1_655 ? Cu1 O4 Cu2 115.9(4) . 1_655 ? Te O5 Cu2 107.0(6) 4_665 4_565 ? Te O5 Pb 101.4(6) 4_665 . ? Cu2 O5 Pb 128.8(7) 4_565 . ? Te O5 Pb 118.2(6) 4_665 3_656 ? Cu2 O5 Pb 84.3(5) 4_565 3_656 ? Pb O5 Pb 117.9(5) . 3_656 ? Te O5 Cu1 61.4(4) 4_665 4_565 ? Cu2 O5 Cu1 67.2(4) 4_565 4_565 ? Pb O5 Cu1 91.8(4) . 4_565 ? Pb O5 Cu1 148.1(4) 3_656 4_565 ? Te O5 Cu2 54.9(4) 4_665 4_665 ? Cu2 O5 Cu2 133.2(6) 4_565 4_665 ? Pb O5 Cu2 98.0(4) . 4_665 ? Pb O5 Cu2 73.0(3) 3_656 4_665 ? Cu1 O5 Cu2 116.3(4) 4_565 4_665 ? Te O5 Cu1 149.5(6) 4_665 . ? Cu2 O5 Cu1 103.3(5) 4_565 . ? Pb O5 Cu1 59.7(3) . . ? Pb O5 Cu1 62.4(2) 3_656 . ? Cu1 O5 Cu1 136.0(4) 4_565 . ? Cu2 O5 Cu1 101.4(3) 4_665 . ? Te O5 Cu2 66.4(4) 4_665 3_656 ? Cu2 O5 Cu2 72.7(4) 4_565 3_656 ? Pb O5 Cu2 158.5(5) . 3_656 ? Pb O5 Cu2 59.7(2) 3_656 3_656 ? Cu1 O5 Cu2 96.9(3) 4_565 3_656 ? Cu2 O5 Cu2 60.5(2) 4_665 3_656 ? Cu1 O5 Cu2 122.1(4) . 3_656 ? Te O6 Cu1 104.0(6) . . ? Te O6 Pb 110.3(7) . . ? Cu1 O6 Pb 96.8(6) . . ? Te O6 Cu2 59.7(4) . . ? Cu1 O6 Cu2 66.0(4) . . ? Pb O6 Cu2 71.1(4) . . ? Te O6 Cu1 73.2(4) . 2_566 ? Cu1 O6 Cu1 71.9(4) . 2_566 ? Pb O6 Cu1 168.8(6) . 2_566 ? Cu2 O6 Cu1 103.0(3) . 2_566 ? Te O6 Pb 145.2(6) . 3_656 ? Cu1 O6 Pb 72.7(4) . 3_656 ? Pb O6 Pb 104.5(4) . 3_656 ? Cu2 O6 Pb 137.3(4) . 3_656 ? Cu1 O6 Pb 73.0(3) 2_566 3_656 ? Te O6 Cu1 51.9(3) . 1_655 ? Cu1 O6 Cu1 127.4(5) . 1_655 ? Pb O6 Cu1 133.7(5) . 1_655 ? Cu2 O6 Cu1 111.5(3) . 1_655 ? Cu1 O6 Cu1 57.1(2) 2_566 1_655 ? Pb O6 Cu1 101.6(4) 3_656 1_655 ? Te O6 Cu2 117.8(6) . 4_665 ? Cu1 O6 Cu2 133.6(6) . 4_665 ? Pb O6 Cu2 87.3(3) . 4_665 ? Cu2 O6 Cu2 153.7(4) . 4_665 ? Cu1 O6 Cu2 100.7(3) 2_566 4_665 ? Pb O6 Cu2 61.7(2) 3_656 4_665 ? Cu1 O6 Cu2 72.5(3) 1_655 4_665 ? Te O6 OW 64.9(4) . . ? Cu1 O6 OW 43.3(4) . . ? Pb O6 OW 126.7(5) . . ? Cu2 O6 OW 61.2(3) . . ? Cu1 O6 OW 44.2(2) 2_566 . ? Pb O6 OW 95.4(3) 3_656 . ? Cu1 O6 OW 87.4(3) 1_655 . ? Cu2 O6 OW 144.3(4) 4_665 . ? Cu2 OW O1 139.7(7) 3_655 . ? Cu2 OW Pb 102.9(5) 3_655 4_564 ? O1 OW Pb 89.3(5) . 4_564 ? Cu2 OW Pb 79.1(4) 3_655 4_664 ? O1 OW Pb 63.4(5) . 4_664 ? Pb OW Pb 126.9(5) 4_564 4_664 ? Cu2 OW Cu1 109.4(6) 3_655 2_566 ? O1 OW Cu1 71.8(4) . 2_566 ? Pb OW Cu1 146.6(5) 4_564 2_566 ? Pb OW Cu1 69.2(4) 4_664 2_566 ? Cu2 OW Cu1 170.2(6) 3_655 . ? O1 OW Cu1 43.6(4) . . ? Pb OW Cu1 85.7(4) 4_564 . ? Pb OW Cu1 99.5(4) 4_664 . ? Cu1 OW Cu1 61.4(2) 2_566 . ? Cu2 OW Cu1 125.0(5) 3_655 2_466 ? O1 OW Cu1 94.8(5) . 2_466 ? Pb OW Cu1 62.3(3) 4_564 2_466 ? Pb OW Cu1 153.9(4) 4_664 2_466 ? Cu1 OW Cu1 91.4(3) 2_566 2_466 ? Cu1 OW Cu1 54.9(2) . 2_466 ? Cu2 OW O6 152.3(7) 3_655 . ? O1 OW O6 30.3(4) . . ? Pb OW O6 102.4(4) 4_564 . ? Pb OW O6 76.8(4) 4_664 . ? Cu1 OW O6 48.6(3) 2_566 . ? Cu1 OW O6 23.0(2) . . ? Cu1 OW O6 77.3(3) 2_466 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.708 _refine_diff_density_min -2.210 _refine_diff_density_rms 0.417