 
data_otto13 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H7 Cl5 Cu6 O13 Pb3 Te' 
_chemical_formula_weight          1522.72 
 
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' 
 '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' 
 '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    R-3 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 '-x+2/3, -y+1/3, -z+1/3' 
 'y+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, x+1/3, -z+1/3' 
 '-x+1/3, -y+2/3, -z+2/3' 
 'y+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, x+2/3, -z+2/3' 
 
_cell_length_a                    8.4035(12) 
_cell_length_b                    8.4035(12) 
_cell_length_c                    44.681(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      2732.6(6) 
_cell_formula_units_Z             6 
_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           0.04 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.552 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              4008 
_exptl_absorpt_coefficient_mu     36.835 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.2603 
_exptl_absorpt_correction_T_max   0.3588 
_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             7475 
_diffrn_reflns_av_R_equivalents   0.0864 
_diffrn_reflns_av_sigmaI/netI     0.0587 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -52 
_diffrn_reflns_limit_l_max        52 
_diffrn_reflns_theta_min          3.34 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              1074 
_reflns_number_gt                 971 
_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^)+(0.0122P)^2^+42.3265P] 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_number_reflns          1074 
_refine_ls_number_parameters      93 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0350 
_refine_ls_R_factor_gt            0.0307 
_refine_ls_wR_factor_ref          0.0649 
_refine_ls_wR_factor_gt           0.0629 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.051 
_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 
Pb Pb 0.31093(5) 0.08441(5) 0.292530(8) 0.02421(16) Uani 1 1 d . . . 
Te Te 0.0000 0.0000 0.21811(2) 0.0151(2) Uani 1 3 d S . . 
Cu1 Cu 0.29295(15) 0.87164(15) 0.21204(2) 0.0182(3) Uani 1 1 d . . . 
Cu2 Cu 0.42162(15) 0.29485(15) 0.21574(2) 0.0185(3) Uani 1 1 d . . . 
Cl1 Cl 0.3333 0.6667 0.1667 0.0238(13) Uani 1 6 d S . . 
Cl2 Cl 0.6667 0.3333 0.3333 0.0308(14) Uani 1 6 d S . . 
Cl3 Cl 0.6667 0.3333 0.25842(8) 0.0217(9) Uani 1 3 d S . . 
Cl4 Cl 0.3307(4) 0.4253(3) 0.30055(5) 0.0282(6) Uani 1 1 d . . . 
O1 O 0.0805(8) 0.8642(8) 0.19380(12) 0.0169(14) Uani 1 1 d . . . 
O2 O 0.8640(9) 0.7773(8) 0.24186(12) 0.0192(14) Uani 1 1 d . . . 
OH3 O 0.4826(8) 0.1181(9) 0.19776(13) 0.0195(15) Uani 1 1 d D . . 
H3 H 0.490(12) 0.107(12) 0.1781(6) 0.023 Uiso 1 1 d D . . 
OH4 O 0.3710(8) 0.4889(8) 0.23097(13) 0.0169(14) Uani 1 1 d D . . 
H4 H 0.361(12) 0.477(12) 0.2509(5) 0.020 Uiso 1 1 d D . . 
OH5 O 0.0000 0.0000 0.3046(2) 0.027(3) Uani 1 3 d SD . . 
H5 H 0.0000 0.0000 0.3247(5) 0.033 Uiso 1 3 d SD . . 
 
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 0.0252(3) 0.0258(3) 0.0215(2) 0.00081(14) -0.00011(15) 0.01269(19) 
Te 0.0156(4) 0.0156(4) 0.0142(5) 0.000 0.000 0.00781(18) 
Cu1 0.0174(6) 0.0177(7) 0.0194(6) 0.0004(4) -0.0015(4) 0.0087(5) 
Cu2 0.0173(6) 0.0177(6) 0.0203(6) -0.0004(4) 0.0004(4) 0.0087(5) 
Cl1 0.027(2) 0.027(2) 0.018(3) 0.000 0.000 0.0133(10) 
Cl2 0.036(2) 0.036(2) 0.020(3) 0.000 0.000 0.0181(12) 
Cl3 0.0238(14) 0.0238(14) 0.0175(19) 0.000 0.000 0.0119(7) 
Cl4 0.0279(14) 0.0250(14) 0.0293(13) -0.0021(10) -0.0002(10) 0.0113(11) 
O1 0.026(4) 0.017(3) 0.014(3) -0.003(2) -0.001(2) 0.016(3) 
O2 0.022(4) 0.026(4) 0.013(3) 0.002(3) 0.003(3) 0.014(3) 
OH3 0.020(4) 0.025(4) 0.012(3) 0.000(3) -0.001(3) 0.010(3) 
OH4 0.017(3) 0.017(3) 0.016(3) 0.000(3) -0.001(3) 0.007(3) 
OH5 0.031(4) 0.031(4) 0.019(6) 0.000 0.000 0.016(2) 
 
_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 2.385(5) 2_655 ? 
Pb OH5 2.402(2) . ? 
Pb Cl4 2.808(2) . ? 
Pb Cl4 3.043(3) 3 ? 
Pb Cl3 3.0630(18) . ? 
Pb Cl2 3.2222(5) . ? 
Pb Cl4 3.262(3) 2_655 ? 
Pb Cl4 3.357(2) 18_545 ? 
Pb OH4 4.018(6) 2_655 ? 
Pb O2 4.025(6) 1_445 ? 
Te O1 1.927(6) 3_455 ? 
Te O1 1.927(6) 1_545 ? 
Te O1 1.927(6) 2_665 ? 
Te O2 1.948(6) 2_655 ? 
Te O2 1.948(6) 3_565 ? 
Te O2 1.948(6) 1_445 ? 
Cu1 O1 1.935(6) . ? 
Cu1 OH4 1.981(6) 2_665 ? 
Cu1 OH3 1.984(7) 1_565 ? 
Cu1 OH4 2.009(6) 3_565 ? 
Cu1 O2 2.541(6) 2_665 ? 
Cu1 Cl1 2.7888(11) . ? 
Cu2 OH3 1.968(6) . ? 
Cu2 OH4 1.999(6) . ? 
Cu2 OH3 2.003(6) 3_665 ? 
Cu2 O2 2.071(6) 2_655 ? 
Cu2 O1 2.362(6) 2_665 ? 
Cu2 Cl3 2.705(3) . ? 
Cl1 Cu1 2.7886(11) 13_565 ? 
Cl1 Cu1 2.7887(11) 14_455 ? 
Cl1 Cu1 2.7887(11) 15 ? 
Cl1 Cu1 2.7889(11) 3_565 ? 
Cl1 Cu1 2.7889(11) 2_665 ? 
Cl1 Cu2 4.1760(12) 15 ? 
Cl1 Cu2 4.1760(12) 14_455 ? 
Cl1 Cu2 4.1760(12) 2_665 ? 
Cl1 Cu2 4.1760(12) 3_565 ? 
Cl1 Cu2 4.1760(12) 13_565 ? 
Cl2 Pb 3.2221(5) 17 ? 
Cl2 Pb 3.2221(5) 16_655 ? 
Cl2 Pb 3.2221(5) 18_545 ? 
Cl2 Pb 3.2222(5) 2_655 ? 
Cl2 Pb 3.2222(5) 3_665 ? 
Cl3 Cu2 2.705(3) 2_655 ? 
Cl3 Cu2 2.705(3) 3_665 ? 
Cl3 Pb 3.0629(18) 2_655 ? 
Cl3 Pb 3.0629(18) 3_665 ? 
Cl3 Cu1 4.126(2) 1_545 ? 
Cl3 Cu1 4.126(2) 2_765 ? 
Cl3 Cu1 4.126(2) 3_565 ? 
Cl4 Pb 3.043(3) 2 ? 
Cl4 Pb 3.262(3) 3_665 ? 
Cl4 Pb 3.357(2) 17 ? 
Cl4 Cu1 4.298(3) 2_665 ? 
O1 Te 1.927(6) 1_565 ? 
O1 Cu2 2.362(6) 3_565 ? 
O1 Cu2 3.450(6) 1_565 ? 
O1 Cu2 3.692(6) 13_565 ? 
O1 Cu1 3.824(6) 3_465 ? 
O1 Cu1 3.824(6) 15 ? 
O1 Cu2 4.005(6) 15_455 ? 
O1 Cu1 4.022(6) 2_665 ? 
O2 Te 1.948(6) 1_665 ? 
O2 Cu2 2.071(6) 3_665 ? 
O2 Pb 2.385(5) 3_665 ? 
O2 Cu1 2.541(6) 3_565 ? 
O2 Cu1 3.541(6) 1_655 ? 
O2 Cu2 3.962(6) 2_665 ? 
O2 Pb 4.025(6) 1_665 ? 
OH3 Cu1 1.984(6) 1_545 ? 
OH3 Cu2 2.003(6) 2_655 ? 
OH3 Cu2 3.699(6) 3_665 ? 
OH3 Cu1 3.963(6) 14_445 ? 
OH3 Cu1 3.973(6) 3 ? 
OH3 Cu2 3.991(6) 13 ? 
OH4 Cu1 1.981(6) 3_565 ? 
OH4 Cu1 2.009(6) 2_665 ? 
OH4 Cu2 3.958(6) 3_665 ? 
OH4 Pb 4.018(6) 3_665 ? 
OH5 Pb 2.402(2) 3 ? 
OH5 Pb 2.402(2) 2 ? 
 
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 OH5 85.4(3) 2_655 . ? 
O2 Pb Cl4 88.44(15) 2_655 . ? 
OH5 Pb Cl4 76.90(6) . . ? 
O2 Pb Cl4 96.39(15) 2_655 3 ? 
OH5 Pb Cl4 72.35(5) . 3 ? 
Cl4 Pb Cl4 148.33(8) . 3 ? 
O2 Pb Cl3 73.94(15) 2_655 . ? 
OH5 Pb Cl3 149.30(15) . . ? 
Cl4 Pb Cl3 80.04(5) . . ? 
Cl4 Pb Cl3 131.39(5) 3 . ? 
O2 Pb Cl2 136.29(14) 2_655 . ? 
OH5 Pb Cl2 125.7(2) . . ? 
Cl4 Pb Cl2 72.72(5) . . ? 
Cl4 Pb Cl2 120.40(4) 3 . ? 
Cl3 Pb Cl2 64.30(6) . . ? 
O2 Pb Cl4 113.19(16) 2_655 2_655 ? 
OH5 Pb Cl4 136.78(11) . 2_655 ? 
Cl4 Pb Cl4 138.51(8) . 2_655 ? 
Cl4 Pb Cl4 67.21(9) 3 2_655 ? 
Cl3 Pb Cl4 73.35(5) . 2_655 ? 
Cl2 Pb Cl4 67.25(4) . 2_655 ? 
O2 Pb Cl4 155.27(15) 2_655 18_545 ? 
OH5 Pb Cl4 70.3(2) . 18_545 ? 
Cl4 Pb Cl4 90.53(5) . 18_545 ? 
Cl4 Pb Cl4 72.28(7) 3 18_545 ? 
Cl3 Pb Cl4 130.12(7) . 18_545 ? 
Cl2 Pb Cl4 66.12(4) . 18_545 ? 
Cl4 Pb Cl4 83.24(5) 2_655 18_545 ? 
O2 Pb Cu2 30.04(14) 2_655 . ? 
OH5 Pb Cu2 108.7(2) . . ? 
Cl4 Pb Cu2 76.23(5) . . ? 
Cl4 Pb Cu2 120.83(5) 3 . ? 
Cl3 Pb Cu2 45.32(6) . . ? 
Cl2 Pb Cu2 106.27(2) . . ? 
Cl4 Pb Cu2 104.60(4) 2_655 . ? 
Cl4 Pb Cu2 166.43(5) 18_545 . ? 
O2 Pb Cu1 37.35(15) 2_655 1_545 ? 
OH5 Pb Cu1 106.2(2) . 1_545 ? 
Cl4 Pb Cu1 122.85(5) . 1_545 ? 
Cl4 Pb Cu1 74.04(5) 3 1_545 ? 
Cl3 Pb Cu1 70.28(5) . 1_545 ? 
Cl2 Pb Cu1 128.07(2) . 1_545 ? 
Cl4 Pb Cu1 76.96(5) 2_655 1_545 ? 
Cl4 Pb Cu1 145.48(5) 18_545 1_545 ? 
Cu2 Pb Cu1 48.10(2) . 1_545 ? 
O2 Pb OH4 63.35(17) 2_655 2_655 ? 
OH5 Pb OH4 130.8(2) . 2_655 ? 
Cl4 Pb OH4 134.04(10) . 2_655 ? 
Cl4 Pb OH4 74.47(10) 3 2_655 ? 
Cl3 Pb OH4 58.41(9) . 2_655 ? 
Cl2 Pb OH4 102.31(9) . 2_655 ? 
Cl4 Pb OH4 49.86(9) 2_655 2_655 ? 
Cl4 Pb OH4 130.28(9) 18_545 2_655 ? 
Cu2 Pb OH4 61.09(9) . 2_655 ? 
Cu1 Pb OH4 28.65(8) 1_545 2_655 ? 
O2 Pb O2 43.72(19) 2_655 1_445 ? 
OH5 Pb O2 53.8(2) . 1_445 ? 
Cl4 Pb O2 106.64(10) . 1_445 ? 
Cl4 Pb O2 60.00(9) 3 1_445 ? 
Cl3 Pb O2 115.93(10) . 1_445 ? 
Cl2 Pb O2 179.31(9) . 1_445 ? 
Cl4 Pb O2 113.42(10) 2_655 1_445 ? 
Cl4 Pb O2 113.72(9) 18_545 1_445 ? 
Cu2 Pb O2 73.75(8) . 1_445 ? 
Cu1 Pb O2 52.47(8) 1_545 1_445 ? 
OH4 Pb O2 78.31(12) 2_655 1_445 ? 
O2 Pb Pb 72.16(15) 2_655 2 ? 
OH5 Pb Pb 32.46(9) . 2 ? 
Cl4 Pb Pb 48.60(5) . 2 ? 
Cl4 Pb Pb 103.29(5) 3 2 ? 
Cl3 Pb Pb 117.56(2) . 2 ? 
Cl2 Pb Pb 116.088(13) . 2 ? 
Cl4 Pb Pb 169.10(4) 2_655 2 ? 
Cl4 Pb Pb 88.78(4) 18_545 2 ? 
Cu2 Pb Pb 84.712(18) . 2 ? 
Cu1 Pb Pb 106.222(17) 1_545 2 ? 
OH4 Pb Pb 134.65(8) 2_655 2 ? 
O2 Pb Pb 63.23(8) 1_445 2 ? 
O2 Pb Pb 77.48(14) 2_655 3 ? 
OH5 Pb Pb 32.46(9) . 3 ? 
Cl4 Pb Pb 108.03(5) . 3 ? 
Cl4 Pb Pb 43.80(5) 3 3 ? 
Cl3 Pb Pb 150.08(6) . 3 ? 
Cl2 Pb Pb 145.480(8) . 3 ? 
Cl4 Pb Pb 110.96(5) 2_655 3 ? 
Cl4 Pb Pb 79.37(4) 18_545 3 ? 
Cu2 Pb Pb 107.331(18) . 3 ? 
Cu1 Pb Pb 81.692(18) 1_545 3 ? 
OH4 Pb Pb 100.60(9) 2_655 3 ? 
O2 Pb Pb 34.35(8) 1_445 3 ? 
Pb Pb Pb 60.0 2 3 ? 
O2 Pb Te 18.21(15) 2_655 . ? 
OH5 Pb Te 67.9(2) . . ? 
Cl4 Pb Te 89.28(5) . . ? 
Cl4 Pb Te 86.15(4) 3 . ? 
Cl3 Pb Te 92.00(6) . . ? 
Cl2 Pb Te 151.958(12) . . ? 
Cl4 Pb Te 122.35(4) 2_655 . ? 
Cl4 Pb Te 137.10(4) 18_545 . ? 
Cu2 Pb Te 47.29(2) . . ? 
Cu1 Pb Te 46.124(18) 1_545 . ? 
OH4 Pb Te 74.63(8) 2_655 . ? 
O2 Pb Te 27.86(8) 1_445 . ? 
Pb Pb Te 60.101(8) 2 . ? 
Pb Pb Te 60.101(9) 3 . ? 
O2 Pb Pb 136.16(15) 2_655 17 ? 
OH5 Pb Pb 80.81(19) . 17 ? 
Cl4 Pb Pb 47.95(5) . 17 ? 
Cl4 Pb Pb 118.12(5) 3 17 ? 
Cl3 Pb Pb 98.44(5) . 17 ? 
Cl2 Pb Pb 45.567(5) . 17 ? 
Cl4 Pb Pb 105.12(4) 2_655 17 ? 
Cl4 Pb Pb 46.15(4) 18_545 17 ? 
Cu2 Pb Pb 120.38(2) . 17 ? 
Cu1 Pb Pb 167.671(18) 1_545 17 ? 
OH4 Pb Pb 147.88(8) 2_655 17 ? 
O2 Pb Pb 133.81(8) 1_445 17 ? 
Pb Pb Pb 74.075(10) 2 17 ? 
Pb Pb Pb 108.306(9) 3 17 ? 
Te Pb Pb 132.384(11) . 17 ? 
O1 Te O1 91.3(2) 3_455 1_545 ? 
O1 Te O1 91.3(2) 3_455 2_665 ? 
O1 Te O1 91.3(2) 1_545 2_665 ? 
O1 Te O2 178.4(3) 3_455 2_655 ? 
O1 Te O2 88.4(2) 1_545 2_655 ? 
O1 Te O2 87.1(2) 2_665 2_655 ? 
O1 Te O2 87.1(2) 3_455 3_565 ? 
O1 Te O2 178.4(2) 1_545 3_565 ? 
O1 Te O2 88.4(2) 2_665 3_565 ? 
O2 Te O2 93.2(2) 2_655 3_565 ? 
O1 Te O2 88.4(2) 3_455 1_445 ? 
O1 Te O2 87.1(2) 1_545 1_445 ? 
O1 Te O2 178.4(2) 2_665 1_445 ? 
O2 Te O2 93.2(2) 2_655 1_445 ? 
O2 Te O2 93.2(2) 3_565 1_445 ? 
O1 Te Cu2 138.57(18) 3_455 . ? 
O1 Te Cu2 81.79(18) 1_545 . ? 
O1 Te Cu2 48.40(18) 2_665 . ? 
O2 Te Cu2 39.81(17) 2_655 . ? 
O2 Te Cu2 99.24(18) 3_565 . ? 
O2 Te Cu2 131.50(18) 1_445 . ? 
O1 Te Cu2 81.79(18) 3_455 3 ? 
O1 Te Cu2 48.41(18) 1_545 3 ? 
O1 Te Cu2 138.57(17) 2_665 3 ? 
O2 Te Cu2 99.24(18) 2_655 3 ? 
O2 Te Cu2 131.50(18) 3_565 3 ? 
O2 Te Cu2 39.81(17) 1_445 3 ? 
Cu2 Te Cu2 119.887(3) . 3 ? 
O1 Te Cu2 48.41(18) 3_455 2 ? 
O1 Te Cu2 138.57(17) 1_545 2 ? 
O1 Te Cu2 81.79(18) 2_665 2 ? 
O2 Te Cu2 131.50(18) 2_655 2 ? 
O2 Te Cu2 39.81(17) 3_565 2 ? 
O2 Te Cu2 99.24(18) 1_445 2 ? 
Cu2 Te Cu2 119.888(3) . 2 ? 
Cu2 Te Cu2 119.888(3) 3 2 ? 
O1 Te Cu1 35.31(17) 3_455 3_455 ? 
O1 Te Cu1 94.51(18) 1_545 3_455 ? 
O1 Te Cu1 126.31(18) 2_665 3_455 ? 
O2 Te Cu1 146.32(17) 2_655 3_455 ? 
O2 Te Cu1 84.34(18) 3_565 3_455 ? 
O2 Te Cu1 53.62(18) 1_445 3_455 ? 
Cu2 Te Cu1 173.14(4) . 3_455 ? 
Cu2 Te Cu1 60.20(3) 3 3_455 ? 
Cu2 Te Cu1 59.70(3) 2 3_455 ? 
O1 Te Cu1 94.51(18) 3_455 2_665 ? 
O1 Te Cu1 126.31(18) 1_545 2_665 ? 
O1 Te Cu1 35.31(17) 2_665 2_665 ? 
O2 Te Cu1 84.34(18) 2_655 2_665 ? 
O2 Te Cu1 53.62(18) 3_565 2_665 ? 
O2 Te Cu1 146.32(17) 1_445 2_665 ? 
Cu2 Te Cu1 59.70(3) . 2_665 ? 
Cu2 Te Cu1 173.14(4) 3 2_665 ? 
Cu2 Te Cu1 60.20(3) 2 2_665 ? 
Cu1 Te Cu1 119.270(8) 3_455 2_665 ? 
O1 Te Cu1 126.31(18) 3_455 1_545 ? 
O1 Te Cu1 35.31(17) 1_545 1_545 ? 
O1 Te Cu1 94.51(18) 2_665 1_545 ? 
O2 Te Cu1 53.62(18) 2_655 1_545 ? 
O2 Te Cu1 146.32(17) 3_565 1_545 ? 
O2 Te Cu1 84.34(18) 1_445 1_545 ? 
Cu2 Te Cu1 60.20(3) . 1_545 ? 
Cu2 Te Cu1 59.70(3) 3 1_545 ? 
Cu2 Te Cu1 173.14(4) 2 1_545 ? 
Cu1 Te Cu1 119.270(7) 3_455 1_545 ? 
Cu1 Te Cu1 119.270(8) 2_665 1_545 ? 
O1 Cu1 OH4 179.3(3) . 2_665 ? 
O1 Cu1 OH3 98.3(3) . 1_565 ? 
OH4 Cu1 OH3 81.3(2) 2_665 1_565 ? 
O1 Cu1 OH4 87.1(2) . 3_565 ? 
OH4 Cu1 OH4 93.3(3) 2_665 3_565 ? 
OH3 Cu1 OH4 173.3(2) 1_565 3_565 ? 
O1 Cu1 O2 72.9(2) . 2_665 ? 
OH4 Cu1 O2 106.5(2) 2_665 2_665 ? 
OH3 Cu1 O2 77.1(2) 1_565 2_665 ? 
OH4 Cu1 O2 100.9(2) 3_565 2_665 ? 
O1 Cu1 Cl1 93.96(17) . . ? 
OH4 Cu1 Cl1 86.68(17) 2_665 . ? 
OH3 Cu1 Cl1 97.39(18) 1_565 . ? 
OH4 Cu1 Cl1 86.14(17) 3_565 . ? 
O2 Cu1 Cl1 164.53(13) 2_665 . ? 
OH3 Cu2 OH4 175.0(3) . . ? 
OH3 Cu2 OH3 95.2(4) . 3_665 ? 
OH4 Cu2 OH3 80.4(2) . 3_665 ? 
OH3 Cu2 O2 89.9(3) . 2_655 ? 
OH4 Cu2 O2 94.9(2) . 2_655 ? 
OH3 Cu2 O2 169.3(2) 3_665 2_655 ? 
OH3 Cu2 O1 103.4(2) . 2_665 ? 
OH4 Cu2 O1 76.6(2) . 2_665 ? 
OH3 Cu2 O1 114.0(2) 3_665 2_665 ? 
O2 Cu2 O1 73.7(2) 2_655 2_665 ? 
OH3 Cu2 Cl3 84.73(18) . . ? 
OH4 Cu2 Cl3 97.02(17) . . ? 
OH3 Cu2 Cl3 84.08(18) 3_665 . ? 
O2 Cu2 Cl3 87.04(17) 2_655 . ? 
O1 Cu2 Cl3 158.89(15) 2_665 . ? 
Cu1 Cl1 Cu1 72.98(3) 13_565 14_455 ? 
Cu1 Cl1 Cu1 72.98(4) 13_565 15 ? 
Cu1 Cl1 Cu1 72.98(3) 14_455 15 ? 
Cu1 Cl1 Cu1 180.0 13_565 . ? 
Cu1 Cl1 Cu1 107.02(3) 14_455 . ? 
Cu1 Cl1 Cu1 107.02(3) 15 . ? 
Cu1 Cl1 Cu1 107.03(4) 13_565 3_565 ? 
Cu1 Cl1 Cu1 107.02(4) 14_455 3_565 ? 
Cu1 Cl1 Cu1 180.0 15 3_565 ? 
Cu1 Cl1 Cu1 72.97(3) . 3_565 ? 
Cu1 Cl1 Cu1 107.02(3) 13_565 2_665 ? 
Cu1 Cl1 Cu1 180.0 14_455 2_665 ? 
Cu1 Cl1 Cu1 107.02(3) 15 2_665 ? 
Cu1 Cl1 Cu1 72.97(4) . 2_665 ? 
Cu1 Cl1 Cu1 72.97(3) 3_565 2_665 ? 
Cu1 Cl1 Cu2 78.32(3) 13_565 . ? 
Cu1 Cl1 Cu2 131.28(3) 14_455 . ? 
Cu1 Cl1 Cu2 133.46(3) 15 . ? 
Cu1 Cl1 Cu2 101.68(3) . . ? 
Cu1 Cl1 Cu2 46.54(3) 3_565 . ? 
Cu1 Cl1 Cu2 48.72(3) 2_665 . ? 
Cu1 Cl1 Cu2 48.72(3) 13_565 15 ? 
Cu1 Cl1 Cu2 46.54(3) 14_455 15 ? 
Cu1 Cl1 Cu2 101.68(3) 15 15 ? 
Cu1 Cl1 Cu2 131.28(3) . 15 ? 
Cu1 Cl1 Cu2 78.32(3) 3_565 15 ? 
Cu1 Cl1 Cu2 133.46(3) 2_665 15 ? 
Cu2 Cl1 Cu2 85.04(2) . 15 ? 
Cu1 Cl1 Cu2 46.54(3) 13_565 14_455 ? 
Cu1 Cl1 Cu2 101.68(3) 14_455 14_455 ? 
Cu1 Cl1 Cu2 48.72(3) 15 14_455 ? 
Cu1 Cl1 Cu2 133.46(3) . 14_455 ? 
Cu1 Cl1 Cu2 131.28(3) 3_565 14_455 ? 
Cu1 Cl1 Cu2 78.32(3) 2_665 14_455 ? 
Cu2 Cl1 Cu2 85.04(2) . 14_455 ? 
Cu2 Cl1 Cu2 94.96(2) 15 14_455 ? 
Cu1 Cl1 Cu2 133.46(3) 13_565 2_665 ? 
Cu1 Cl1 Cu2 78.32(3) 14_455 2_665 ? 
Cu1 Cl1 Cu2 131.28(3) 15 2_665 ? 
Cu1 Cl1 Cu2 46.54(3) . 2_665 ? 
Cu1 Cl1 Cu2 48.72(3) 3_565 2_665 ? 
Cu1 Cl1 Cu2 101.68(3) 2_665 2_665 ? 
Cu2 Cl1 Cu2 94.96(2) . 2_665 ? 
Cu2 Cl1 Cu2 85.04(2) 15 2_665 ? 
Cu2 Cl1 Cu2 180.00(2) 14_455 2_665 ? 
Cu1 Cl1 Cu2 131.28(3) 13_565 3_565 ? 
Cu1 Cl1 Cu2 133.46(3) 14_455 3_565 ? 
Cu1 Cl1 Cu2 78.32(3) 15 3_565 ? 
Cu1 Cl1 Cu2 48.72(3) . 3_565 ? 
Cu1 Cl1 Cu2 101.68(3) 3_565 3_565 ? 
Cu1 Cl1 Cu2 46.54(3) 2_665 3_565 ? 
Cu2 Cl1 Cu2 94.96(2) . 3_565 ? 
Cu2 Cl1 Cu2 180.0 15 3_565 ? 
Cu2 Cl1 Cu2 85.04(2) 14_455 3_565 ? 
Cu2 Cl1 Cu2 94.96(2) 2_665 3_565 ? 
Cu1 Cl1 Cu2 101.68(3) 13_565 13_565 ? 
Cu1 Cl1 Cu2 48.72(3) 14_455 13_565 ? 
Cu1 Cl1 Cu2 46.54(3) 15 13_565 ? 
Cu1 Cl1 Cu2 78.32(3) . 13_565 ? 
Cu1 Cl1 Cu2 133.46(3) 3_565 13_565 ? 
Cu1 Cl1 Cu2 131.28(3) 2_665 13_565 ? 
Cu2 Cl1 Cu2 180.00(2) . 13_565 ? 
Cu2 Cl1 Cu2 94.96(2) 15 13_565 ? 
Cu2 Cl1 Cu2 94.96(2) 14_455 13_565 ? 
Cu2 Cl1 Cu2 85.04(2) 2_665 13_565 ? 
Cu2 Cl1 Cu2 85.04(2) 3_565 13_565 ? 
Pb Cl2 Pb 91.139(11) 17 16_655 ? 
Pb Cl2 Pb 91.139(11) 17 18_545 ? 
Pb Cl2 Pb 91.138(11) 16_655 18_545 ? 
Pb Cl2 Pb 88.863(11) 17 . ? 
Pb Cl2 Pb 180.0 16_655 . ? 
Pb Cl2 Pb 88.863(11) 18_545 . ? 
Pb Cl2 Pb 180.0 17 2_655 ? 
Pb Cl2 Pb 88.863(11) 16_655 2_655 ? 
Pb Cl2 Pb 88.863(11) 18_545 2_655 ? 
Pb Cl2 Pb 91.135(11) . 2_655 ? 
Pb Cl2 Pb 88.864(11) 17 3_665 ? 
Pb Cl2 Pb 88.864(11) 16_655 3_665 ? 
Pb Cl2 Pb 180.0 18_545 3_665 ? 
Pb Cl2 Pb 91.135(11) . 3_665 ? 
Pb Cl2 Pb 91.134(11) 2_655 3_665 ? 
Cu2 Cl3 Cu2 75.78(9) 2_655 3_665 ? 
Cu2 Cl3 Cu2 75.78(9) 2_655 . ? 
Cu2 Cl3 Cu2 75.78(9) 3_665 . ? 
Cu2 Cl3 Pb 81.05(3) 2_655 2_655 ? 
Cu2 Cl3 Pb 107.55(3) 3_665 2_655 ? 
Cu2 Cl3 Pb 155.02(7) . 2_655 ? 
Cu2 Cl3 Pb 155.02(7) 2_655 3_665 ? 
Cu2 Cl3 Pb 81.05(3) 3_665 3_665 ? 
Cu2 Cl3 Pb 107.55(3) . 3_665 ? 
Pb Cl3 Pb 97.39(7) 2_655 3_665 ? 
Cu2 Cl3 Pb 107.55(3) 2_655 . ? 
Cu2 Cl3 Pb 155.02(7) 3_665 . ? 
Cu2 Cl3 Pb 81.05(3) . . ? 
Pb Cl3 Pb 97.39(7) 2_655 . ? 
Pb Cl3 Pb 97.39(7) 3_665 . ? 
Cu2 Cl3 Cu1 47.27(4) 2_655 1_545 ? 
Cu2 Cl3 Cu1 105.00(10) 3_665 1_545 ? 
Cu2 Cl3 Cu1 50.02(4) . 1_545 ? 
Pb Cl3 Cu1 106.533(18) 2_655 1_545 ? 
Pb Cl3 Cu1 151.817(17) 3_665 1_545 ? 
Pb Cl3 Cu1 65.39(2) . 1_545 ? 
Cu2 Cl3 Cu1 50.02(4) 2_655 2_765 ? 
Cu2 Cl3 Cu1 47.27(4) 3_665 2_765 ? 
Cu2 Cl3 Cu1 105.00(10) . 2_765 ? 
Pb Cl3 Cu1 65.39(2) 2_655 2_765 ? 
Pb Cl3 Cu1 106.533(19) 3_665 2_765 ? 
Pb Cl3 Cu1 151.817(17) . 2_765 ? 
Cu1 Cl3 Cu1 96.99(6) 1_545 2_765 ? 
Cu2 Cl3 Cu1 105.00(10) 2_655 3_565 ? 
Cu2 Cl3 Cu1 50.02(4) 3_665 3_565 ? 
Cu2 Cl3 Cu1 47.27(4) . 3_565 ? 
Pb Cl3 Cu1 151.817(18) 2_655 3_565 ? 
Pb Cl3 Cu1 65.39(2) 3_665 3_565 ? 
Pb Cl3 Cu1 106.533(18) . 3_565 ? 
Cu1 Cl3 Cu1 96.99(6) 1_545 3_565 ? 
Cu1 Cl3 Cu1 96.99(6) 2_765 3_565 ? 
Pb Cl4 Pb 87.60(7) . 2 ? 
Pb Cl4 Pb 98.33(7) . 3_665 ? 
Pb Cl4 Pb 164.83(9) 2 3_665 ? 
Pb Cl4 Pb 93.65(7) . 17 ? 
Pb Cl4 Pb 107.72(7) 2 17 ? 
Pb Cl4 Pb 85.94(6) 3_665 17 ? 
Pb Cl4 Cu2 62.33(5) . . ? 
Pb Cl4 Cu2 93.42(6) 2 . ? 
Pb Cl4 Cu2 77.26(5) 3_665 . ? 
Pb Cl4 Cu2 147.63(7) 17 . ? 
Pb Cl4 Cu1 93.05(6) . 2_665 ? 
Pb Cl4 Cu1 63.05(4) 2 2_665 ? 
Pb Cl4 Cu1 102.51(6) 3_665 2_665 ? 
Pb Cl4 Cu1 168.35(8) 17 2_665 ? 
Cu2 Cl4 Cu1 43.71(3) . 2_665 ? 
Te O1 Cu1 109.6(3) 1_565 . ? 
Te O1 Cu2 94.0(2) 1_565 3_565 ? 
Cu1 O1 Cu2 93.3(2) . 3_565 ? 
Te O1 Cu2 64.66(16) 1_565 1_565 ? 
Cu1 O1 Cu2 64.97(17) . 1_565 ? 
Cu2 O1 Cu2 138.8(2) 3_565 1_565 ? 
Te O1 Cu2 117.2(2) 1_565 13_565 ? 
Cu1 O1 Cu2 102.7(2) . 13_565 ? 
Cu2 O1 Cu2 136.5(2) 3_565 13_565 ? 
Cu2 O1 Cu2 84.02(13) 1_565 13_565 ? 
Te O1 Cu1 55.34(14) 1_565 3_465 ? 
Cu1 O1 Cu1 139.6(2) . 3_465 ? 
Cu2 O1 Cu1 55.62(12) 3_565 3_465 ? 
Cu2 O1 Cu1 119.74(15) 1_565 3_465 ? 
Cu2 O1 Cu1 117.60(15) 13_565 3_465 ? 
Te O1 Cu1 152.8(2) 1_565 15 ? 
Cu1 O1 Cu1 96.8(2) . 15 ? 
Cu2 O1 Cu1 90.95(17) 3_565 15 ? 
Cu2 O1 Cu1 124.53(16) 1_565 15 ? 
Cu2 O1 Cu1 47.56(7) 13_565 15 ? 
Cu1 O1 Cu1 107.68(14) 3_465 15 ? 
Te O1 Cu2 105.4(2) 1_565 15_455 ? 
Cu1 O1 Cu2 143.7(2) . 15_455 ? 
Cu2 O1 Cu2 93.81(17) 3_565 15_455 ? 
Cu2 O1 Cu2 124.84(16) 1_565 15_455 ? 
Cu2 O1 Cu2 50.95(8) 13_565 15_455 ? 
Cu1 O1 Cu2 70.63(10) 3_465 15_455 ? 
Cu1 O1 Cu2 47.58(7) 15 15_455 ? 
Te O1 Cu1 131.4(2) 1_565 2_665 ? 
Cu1 O1 Cu1 55.04(15) . 2_665 ? 
Cu2 O1 Cu1 48.63(11) 3_565 2_665 ? 
Cu2 O1 Cu1 119.87(15) 1_565 2_665 ? 
Cu2 O1 Cu1 111.30(14) 13_565 2_665 ? 
Cu1 O1 Cu1 103.92(14) 3_465 2_665 ? 
Cu1 O1 Cu1 69.67(10) 15 2_665 ? 
Cu2 O1 Cu1 106.72(13) 15_455 2_665 ? 
Te O2 Cu2 103.2(2) 1_665 3_665 ? 
Te O2 Pb 139.3(3) 1_665 3_665 ? 
Cu2 O2 Pb 114.8(3) 3_665 3_665 ? 
Te O2 Cu1 88.3(2) 1_665 3_565 ? 
Cu2 O2 Cu1 85.9(2) 3_665 3_565 ? 
Pb O2 Cu1 107.9(2) 3_665 3_565 ? 
Te O2 Cu1 62.46(16) 1_665 1_655 ? 
Cu2 O2 Cu1 61.59(15) 3_665 1_655 ? 
Pb O2 Cu1 123.9(2) 3_665 1_655 ? 
Cu1 O2 Cu1 126.26(19) 3_565 1_655 ? 
Te O2 Cu2 51.72(14) 1_665 2_665 ? 
Cu2 O2 Cu2 126.5(2) 3_665 2_665 ? 
Pb O2 Cu2 109.67(19) 3_665 2_665 ? 
Cu1 O2 Cu2 52.34(11) 3_565 2_665 ? 
Cu1 O2 Cu2 113.94(15) 1_655 2_665 ? 
Te O2 Pb 77.25(18) 1_665 1_665 ? 
Cu2 O2 Pb 115.8(2) 3_665 1_665 ? 
Pb O2 Pb 73.49(14) 3_665 1_665 ? 
Cu1 O2 Pb 156.0(2) 3_565 1_665 ? 
Cu1 O2 Pb 63.19(10) 1_655 1_665 ? 
Cu2 O2 Pb 104.04(14) 2_665 1_665 ? 
Te O2 Cu2 127.3(2) 1_665 . ? 
Cu2 O2 Cu2 54.44(15) 3_665 . ? 
Pb O2 Cu2 88.40(17) 3_665 . ? 
Cu1 O2 Cu2 48.09(11) 3_565 . ? 
Cu1 O2 Cu2 115.85(15) 1_655 . ? 
Cu2 O2 Cu2 100.10(14) 2_665 . ? 
Pb O2 Cu2 153.55(16) 1_665 . ? 
Cu2 OH3 Cu1 106.3(3) . 1_545 ? 
Cu2 OH3 Cu2 113.5(3) . 2_655 ? 
Cu1 OH3 Cu2 99.0(3) 1_545 2_655 ? 
Cu2 OH3 Cu2 63.40(17) . 3_665 ? 
Cu1 OH3 Cu2 148.4(2) 1_545 3_665 ? 
Cu2 OH3 Cu2 63.30(16) 2_655 3_665 ? 
Cu2 OH3 Cu1 144.5(2) . 14_445 ? 
Cu1 OH3 Cu1 91.7(2) 1_545 14_445 ? 
Cu2 OH3 Cu1 92.8(2) 2_655 14_445 ? 
Cu2 OH3 Cu1 114.03(15) 3_665 14_445 ? 
Cu2 OH3 Cu1 146.4(2) . 3 ? 
Cu1 OH3 Cu1 56.43(16) 1_545 3 ? 
Cu2 OH3 Cu1 51.32(15) 2_655 3 ? 
Cu2 OH3 Cu1 114.48(15) 3_665 3 ? 
Cu1 OH3 Cu1 68.82(11) 14_445 3 ? 
Cu2 OH3 Cu2 101.3(2) . 13 ? 
Cu1 OH3 Cu2 92.3(2) 1_545 13 ? 
Cu2 OH3 Cu2 138.2(2) 2_655 13 ? 
Cu2 OH3 Cu2 118.57(16) 3_665 13 ? 
Cu1 OH3 Cu2 46.48(7) 14_445 13 ? 
Cu1 OH3 Cu2 107.49(15) 3 13 ? 
Cu1 OH4 Cu2 99.3(3) 3_565 . ? 
Cu1 OH4 Cu1 112.5(3) 3_565 2_665 ? 
Cu2 OH4 Cu1 103.1(3) . 2_665 ? 
Cu1 OH4 Cu1 63.48(16) 3_565 . ? 
Cu2 OH4 Cu1 146.8(2) . . ? 
Cu1 OH4 Cu1 63.39(15) 2_665 . ? 
Cu1 OH4 Cu2 52.29(14) 3_565 3_665 ? 
Cu2 OH4 Cu2 56.97(15) . 3_665 ? 
Cu1 OH4 Cu2 144.7(2) 2_665 3_665 ? 
Cu1 OH4 Cu2 115.63(15) . 3_665 ? 
Cu1 OH4 Pb 74.75(17) 3_565 3_665 ? 
Cu2 OH4 Pb 95.5(2) . 3_665 ? 
Cu1 OH4 Pb 158.3(2) 2_665 3_665 ? 
Cu1 OH4 Pb 105.74(14) . 3_665 ? 
Cu2 OH4 Pb 56.20(8) 3_665 3_665 ? 
Pb OH5 Pb 115.08(18) . 3 ? 
Pb OH5 Pb 115.08(18) . 2 ? 
Pb OH5 Pb 115.08(18) 3 2 ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
OH3 H3 O1  0.89(2) 1.75(3) 2.634(8) 172(9) 14_445 
OH4 H4 Cl4  0.90(2) 2.25(2) 3.144(6) 176(8) . 
OH5 H5 Cl4  0.90(2) 2.737(16) 3.408(9) 132.5(4) 16 
OH5 H5 Cl4  0.90(2) 2.737(16) 3.408(9) 132.5(4) 17_445 
OH5 H5 Cl4  0.90(2) 2.737(16) 3.408(9) 132.5(4) 18_545 
 
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              25.02 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    2.234 
_refine_diff_density_min   -1.429 
_refine_diff_density_rms    0.297 
