 
data_tombstoneite
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_mineral            'tombstoneite' 
_chemical_compound_source         'Grand Central mine, Arizona'
_chemical_formula_sum
 'Ca0.50 H6 Cu5.90 O41 Pb3.50 S2 Se1.67 Te8.33' 
_chemical_formula_weight          3041.03

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Se'  'Se'  -0.0929   2.2259
 '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'
 'Ca'  'Ca'   0.2262   0.3064
 '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'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            150
_space_group_name_H-M_alt         'P 3 2 1'
_space_group_name_Hall            'P 3 2"'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 '-x, -x+y, -z'
 'x-y, -y, -z'
 
_cell_length_a                    9.1377(9)
_cell_length_b                    9.1377(9)
_cell_length_c                    12.2797(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      887.96(18)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     4959
_cell_measurement_theta_min       3.1
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        'tablet'
_exptl_crystal_colour             'green'
_exptl_crystal_density_diffrn     5.687          
_exptl_crystal_F_000              1324
_exptl_crystal_size_max           0.090
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.030
_exptl_absorpt_coefficient_mu     28.730
_shelx_estimated_absorpt_T_min    0.182
_shelx_estimated_absorpt_T_max    0.479
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_correction_T_min   0.254
_exptl_absorpt_process_details    'Higashi2001'
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71075
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Sealed Tube'
_diffrn_radiation_monochromator   'Graphite Monochromator'
_diffrn_measurement_device_type   'Rigaku R-axis RAPID II'
_diffrn_measurement_method        'profile data from ω-scans'
_diffrn_reflns_number             5529
_diffrn_reflns_av_unetI/netI      0.0668
_diffrn_reflns_av_R_equivalents   0.0968
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.062
_diffrn_reflns_theta_max          27.480
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.973
_diffrn_reflns_point_group_measured_fraction_full  0.976
_reflns_number_total              1328
_reflns_number_gt                 1205
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.650
_reflns_Friedel_fraction_max      0.942
_reflns_Friedel_fraction_full     0.946
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+24.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef        0.0005(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 402 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.023(12)
_refine_ls_number_reflns          1328
_refine_ls_number_parameters      101
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0499
_refine_ls_R_factor_gt            0.0432
_refine_ls_wR_factor_ref          0.0910
_refine_ls_wR_factor_gt           0.0846
_refine_ls_goodness_of_fit_ref    1.101
_refine_ls_restrained_S_all       1.101
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 0.500000 0.0175(12) Uani 0.497(12) 6 d S T P . .
Ca1 Ca 0.000000 0.000000 0.500000 0.0175(12) Uani 0.503(12) 6 d S T P . .
Pb2 Pb 0.73370(12) 0.73370(12) 0.000000 0.0174(3) Uani 1 2 d S T P . .
Cu Cu 0.3756(3) 0.3826(4) 0.8465(2) 0.0177(10) Uani 0.984(13) 1 d . . P . .
Te1 Te 0.000000 0.000000 0.78402(17) 0.0120(5) Uani 1 3 d S T P . .
Te2 Te 0.58885(17) 0.67484(18) 0.68160(9) 0.0136(3) Uani 1 1 d . . . . .
Se Se 0.666667 0.333333 0.8918(3) 0.0152(11) Uani 0.84(3) 3 d S T P . .
Te Te 0.666667 0.333333 0.8918(3) 0.0152(11) Uani 0.16(3) 3 d S T P . .
S S 0.333333 0.666667 0.4009(7) 0.0197(19) Uani 1 3 d S T P . .
O1 O 0.333333 0.666667 0.5205(19) 0.028(7) Uani 1 3 d S T P . .
O2 O 0.299(2) 0.501(2) 0.3593(13) 0.031(4) Uani 1 1 d . . . . .
O3 O 0.6779(18) 0.1701(18) 0.9602(11) 0.015(3) Uani 1 1 d . . . . .
O4 O 0.5316(19) 0.8351(18) 0.7255(13) 0.020(3) Uani 1 1 d . . . . .
O5 O 0.5918(18) 0.5867(19) 0.8184(12) 0.020(3) Uani 1 1 d . . . . .
O6 O 0.8341(17) 0.8332(18) 0.6826(11) 0.015(3) Uani 1 1 d . . . . .
O7 O 0.1656(18) 0.1737(17) 0.8760(11) 0.012(3) Uani 1 1 d . . . . .
O8 O 0.739(3) 0.000000 0.500000 0.042(8) Uani 1 2 d S T P . .
 
 
_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 2.38(3) 3_665 ?
Pb1 O8 2.38(3) 2_545 ?
Pb1 O8 2.38(3) 1_455 ?
Pb1 O6 2.709(13) 4_446 ?
Pb1 O6 2.709(13) 3_565 ?
Pb1 O6 2.709(13) 2_655 ?
Pb1 O6 2.709(13) 5_656 ?
Pb1 O6 2.709(13) 6_566 ?
Pb1 O6 2.709(13) 1_445 ?
Pb1 Te1 3.488(2) . ?
Pb1 Te1 3.488(2) 4_556 ?
Pb1 Te2 4.0930(14) 4_446 ?
Pb2 O7 2.570(14) 6_666 ?
Pb2 O7 2.570(14) 2_664 ?
Pb2 O5 2.592(15) 1_554 ?
Pb2 O5 2.592(15) 4_556 ?
Pb2 O3 2.662(15) 2_654 ?
Pb2 O3 2.662(15) 6_566 ?
Pb2 O7 2.673(13) 5_666 ?
Pb2 O7 2.673(13) 3_664 ?
Pb2 O3 3.310(15) 3_664 ?
Pb2 O3 3.310(15) 5_666 ?
Pb2 Cu 3.580(3) 6_666 ?
Pb2 Cu 3.580(3) 2_664 ?
Cu O4 1.942(15) 3_565 ?
Cu O7 1.948(15) . ?
Cu O5 1.953(15) . ?
Cu O3 1.995(14) 3_665 ?
Cu O3 2.714(14) 5_667 ?
Te1 O7 1.919(13) 3 ?
Te1 O7 1.919(13) 2 ?
Te1 O7 1.919(13) . ?
Te1 O6 1.965(14) 1_445 ?
Te1 O6 1.965(14) 3_565 ?
Te1 O6 1.965(14) 2_655 ?
Te2 O4 1.865(15) . ?
Te2 O5 1.869(15) . ?
Te2 O6 1.968(14) . ?
Te2 O4 2.393(15) 3_565 ?
Te2 O1 3.033(16) . ?
Te2 O2 3.093(18) 6_666 ?
Te2 O2 3.150(18) 4_556 ?
Se O3 1.759(15) . ?
Se O3 1.759(15) 2_655 ?
Se O3 1.759(15) 3_665 ?
Se O5 2.868(16) 2_655 ?
Se O5 2.868(16) 3_665 ?
Se O5 2.868(16) . ?
S O1 1.47(3) . ?
S O2 1.477(15) 3_565 ?
S O2 1.477(16) 2_665 ?
S O2 1.477(15) . ?
 
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 O8 120.000(3) 3_665 2_545 ?
O8 Pb1 O8 120.000(3) 3_665 1_455 ?
O8 Pb1 O8 120.000(8) 2_545 1_455 ?
O8 Pb1 O6 124.1(3) 3_665 4_446 ?
O8 Pb1 O6 73.9(3) 2_545 4_446 ?
O8 Pb1 O6 73.6(3) 1_455 4_446 ?
O8 Pb1 O6 73.9(3) 3_665 3_565 ?
O8 Pb1 O6 124.1(3) 2_545 3_565 ?
O8 Pb1 O6 73.6(3) 1_455 3_565 ?
O6 Pb1 O6 147.1(6) 4_446 3_565 ?
O8 Pb1 O6 73.6(3) 3_665 2_655 ?
O8 Pb1 O6 73.9(3) 2_545 2_655 ?
O8 Pb1 O6 124.1(3) 1_455 2_655 ?
O6 Pb1 O6 147.7(6) 4_446 2_655 ?
O6 Pb1 O6 58.1(5) 3_565 2_655 ?
O8 Pb1 O6 73.9(3) 3_665 5_656 ?
O8 Pb1 O6 73.6(3) 2_545 5_656 ?
O8 Pb1 O6 124.1(3) 1_455 5_656 ?
O6 Pb1 O6 58.1(5) 4_446 5_656 ?
O6 Pb1 O6 147.7(6) 3_565 5_656 ?
O6 Pb1 O6 111.7(6) 2_655 5_656 ?
O8 Pb1 O6 73.6(3) 3_665 6_566 ?
O8 Pb1 O6 124.1(3) 2_545 6_566 ?
O8 Pb1 O6 73.9(3) 1_455 6_566 ?
O6 Pb1 O6 58.1(5) 4_446 6_566 ?
O6 Pb1 O6 111.7(6) 3_565 6_566 ?
O6 Pb1 O6 147.1(6) 2_655 6_566 ?
O6 Pb1 O6 58.1(5) 5_656 6_566 ?
O8 Pb1 O6 124.1(3) 3_665 1_445 ?
O8 Pb1 O6 73.6(3) 2_545 1_445 ?
O8 Pb1 O6 73.9(3) 1_455 1_445 ?
O6 Pb1 O6 111.7(6) 4_446 1_445 ?
O6 Pb1 O6 58.1(5) 3_565 1_445 ?
O6 Pb1 O6 58.1(5) 2_655 1_445 ?
O6 Pb1 O6 147.1(6) 5_656 1_445 ?
O6 Pb1 O6 147.7(6) 6_566 1_445 ?
O8 Pb1 Te1 90.000(2) 3_665 . ?
O8 Pb1 Te1 90.0 2_545 . ?
O8 Pb1 Te1 90.0 1_455 . ?
O6 Pb1 Te1 145.9(3) 4_446 . ?
O6 Pb1 Te1 34.1(3) 3_565 . ?
O6 Pb1 Te1 34.1(3) 2_655 . ?
O6 Pb1 Te1 145.9(3) 5_656 . ?
O6 Pb1 Te1 145.9(3) 6_566 . ?
O6 Pb1 Te1 34.1(3) 1_445 . ?
O8 Pb1 Te1 90.000(2) 3_665 4_556 ?
O8 Pb1 Te1 90.0 2_545 4_556 ?
O8 Pb1 Te1 90.0 1_455 4_556 ?
O6 Pb1 Te1 34.1(3) 4_446 4_556 ?
O6 Pb1 Te1 145.9(3) 3_565 4_556 ?
O6 Pb1 Te1 145.9(3) 2_655 4_556 ?
O6 Pb1 Te1 34.1(3) 5_656 4_556 ?
O6 Pb1 Te1 34.1(3) 6_566 4_556 ?
O6 Pb1 Te1 145.9(3) 1_445 4_556 ?
Te1 Pb1 Te1 180.0 . 4_556 ?
O8 Pb1 Te2 145.275(18) 3_665 4_446 ?
O8 Pb1 Te2 56.294(18) 2_545 4_446 ?
O8 Pb1 Te2 74.516(18) 1_455 4_446 ?
O6 Pb1 Te2 24.3(3) 4_446 4_446 ?
O6 Pb1 Te2 139.5(3) 3_565 4_446 ?
O6 Pb1 Te2 127.1(3) 2_655 4_446 ?
O6 Pb1 Te2 72.3(3) 5_656 4_446 ?
O6 Pb1 Te2 82.1(3) 6_566 4_446 ?
O6 Pb1 Te2 89.4(3) 1_445 4_446 ?
Te1 Pb1 Te2 123.013(17) . 4_446 ?
Te1 Pb1 Te2 56.987(17) 4_556 4_446 ?
O7 Pb2 O7 102.8(6) 6_666 2_664 ?
O7 Pb2 O5 145.0(4) 6_666 1_554 ?
O7 Pb2 O5 79.4(4) 2_664 1_554 ?
O7 Pb2 O5 79.4(4) 6_666 4_556 ?
O7 Pb2 O5 145.0(4) 2_664 4_556 ?
O5 Pb2 O5 118.8(6) 1_554 4_556 ?
O7 Pb2 O3 76.1(4) 6_666 2_654 ?
O7 Pb2 O3 121.2(4) 2_664 2_654 ?
O5 Pb2 O3 73.4(5) 1_554 2_654 ?
O5 Pb2 O3 93.4(5) 4_556 2_654 ?
O7 Pb2 O3 121.2(4) 6_666 6_566 ?
O7 Pb2 O3 76.1(4) 2_664 6_566 ?
O5 Pb2 O3 93.4(5) 1_554 6_566 ?
O5 Pb2 O3 73.4(5) 4_556 6_566 ?
O3 Pb2 O3 154.3(6) 2_654 6_566 ?
O7 Pb2 O7 61.6(6) 6_666 5_666 ?
O7 Pb2 O7 71.1(5) 2_664 5_666 ?
O5 Pb2 O7 145.6(5) 1_554 5_666 ?
O5 Pb2 O7 80.1(4) 4_556 5_666 ?
O3 Pb2 O7 137.7(4) 2_654 5_666 ?
O3 Pb2 O7 63.0(4) 6_566 5_666 ?
O7 Pb2 O7 71.1(5) 6_666 3_664 ?
O7 Pb2 O7 61.6(6) 2_664 3_664 ?
O5 Pb2 O7 80.1(4) 1_554 3_664 ?
O5 Pb2 O7 145.6(5) 4_556 3_664 ?
O3 Pb2 O7 63.0(4) 2_654 3_664 ?
O3 Pb2 O7 137.7(4) 6_566 3_664 ?
O7 Pb2 O7 100.3(6) 5_666 3_664 ?
O7 Pb2 O3 116.3(4) 6_666 3_664 ?
O7 Pb2 O3 133.0(4) 2_664 3_664 ?
O5 Pb2 O3 53.7(4) 1_554 3_664 ?
O5 Pb2 O3 71.0(4) 4_556 3_664 ?
O3 Pb2 O3 51.9(6) 2_654 3_664 ?
O3 Pb2 O3 102.47(10) 6_566 3_664 ?
O7 Pb2 O3 150.6(4) 5_666 3_664 ?
O7 Pb2 O3 106.5(4) 3_664 3_664 ?
O7 Pb2 O3 133.0(4) 6_666 5_666 ?
O7 Pb2 O3 116.3(4) 2_664 5_666 ?
O5 Pb2 O3 71.0(4) 1_554 5_666 ?
O5 Pb2 O3 53.7(4) 4_556 5_666 ?
O3 Pb2 O3 102.47(10) 2_654 5_666 ?
O3 Pb2 O3 51.9(6) 6_566 5_666 ?
O7 Pb2 O3 106.5(4) 5_666 5_666 ?
O7 Pb2 O3 150.6(4) 3_664 5_666 ?
O3 Pb2 O3 51.3(5) 3_664 5_666 ?
O7 Pb2 Cu 31.9(3) 6_666 6_666 ?
O7 Pb2 Cu 128.4(3) 2_664 6_666 ?
O5 Pb2 Cu 122.2(4) 1_554 6_666 ?
O5 Pb2 Cu 69.7(3) 4_556 6_666 ?
O3 Pb2 Cu 48.9(3) 2_654 6_666 ?
O3 Pb2 Cu 137.6(3) 6_566 6_666 ?
O7 Pb2 Cu 90.6(3) 5_666 6_666 ?
O7 Pb2 Cu 75.9(3) 3_664 6_666 ?
O3 Pb2 Cu 84.5(2) 3_664 6_666 ?
O3 Pb2 Cu 115.1(2) 5_666 6_666 ?
O7 Pb2 Cu 128.4(3) 6_666 2_664 ?
O7 Pb2 Cu 31.9(3) 2_664 2_664 ?
O5 Pb2 Cu 69.7(3) 1_554 2_664 ?
O5 Pb2 Cu 122.2(4) 4_556 2_664 ?
O3 Pb2 Cu 137.6(3) 2_654 2_664 ?
O3 Pb2 Cu 48.9(3) 6_566 2_664 ?
O7 Pb2 Cu 75.9(3) 5_666 2_664 ?
O7 Pb2 Cu 90.6(3) 3_664 2_664 ?
O3 Pb2 Cu 115.1(2) 3_664 2_664 ?
O3 Pb2 Cu 84.5(2) 5_666 2_664 ?
Cu Pb2 Cu 158.98(10) 6_666 2_664 ?
O4 Cu O7 99.9(6) 3_565 . ?
O4 Cu O5 82.2(6) 3_565 . ?
O7 Cu O5 177.4(6) . . ?
O4 Cu O3 169.5(7) 3_565 3_665 ?
O7 Cu O3 89.9(6) . 3_665 ?
O5 Cu O3 87.9(6) . 3_665 ?
O4 Cu O3 111.1(6) 3_565 5_667 ?
O7 Cu O3 85.9(5) . 5_667 ?
O5 Cu O3 94.9(6) . 5_667 ?
O3 Cu O3 73.1(6) 3_665 5_667 ?
O7 Te1 O7 88.9(6) 3 2 ?
O7 Te1 O7 88.9(6) 3 . ?
O7 Te1 O7 88.9(6) 2 . ?
O7 Te1 O6 94.6(6) 3 1_445 ?
O7 Te1 O6 92.3(6) 2 1_445 ?
O7 Te1 O6 176.4(6) . 1_445 ?
O7 Te1 O6 176.4(6) 3 3_565 ?
O7 Te1 O6 94.6(6) 2 3_565 ?
O7 Te1 O6 92.3(6) . 3_565 ?
O6 Te1 O6 84.1(6) 1_445 3_565 ?
O7 Te1 O6 92.3(6) 3 2_655 ?
O7 Te1 O6 176.4(6) 2 2_655 ?
O7 Te1 O6 94.6(6) . 2_655 ?
O6 Te1 O6 84.1(6) 1_445 2_655 ?
O6 Te1 O6 84.1(6) 3_565 2_655 ?
O7 Te1 Pb1 126.1(4) 3 . ?
O7 Te1 Pb1 126.1(4) 2 . ?
O7 Te1 Pb1 126.1(4) . . ?
O6 Te1 Pb1 50.7(4) 1_445 . ?
O6 Te1 Pb1 50.7(4) 3_565 . ?
O6 Te1 Pb1 50.7(4) 2_655 . ?
O7 Te1 Cu 106.5(4) 3 2 ?
O7 Te1 Cu 23.6(4) 2 2 ?
O7 Te1 Cu 104.5(4) . 2 ?
O6 Te1 Cu 75.6(4) 1_445 2 ?
O6 Te1 Cu 76.5(4) 3_565 2 ?
O6 Te1 Cu 153.2(4) 2_655 2 ?
Pb1 Te1 Cu 102.49(6) . 2 ?
O7 Te1 Cu 104.5(4) 3 . ?
O7 Te1 Cu 106.5(4) 2 . ?
O7 Te1 Cu 23.6(4) . . ?
O6 Te1 Cu 153.2(4) 1_445 . ?
O6 Te1 Cu 75.6(4) 3_565 . ?
O6 Te1 Cu 76.5(4) 2_655 . ?
Pb1 Te1 Cu 102.49(6) . . ?
Cu Te1 Cu 115.46(4) 2 . ?
O7 Te1 Cu 23.6(4) 3 3 ?
O7 Te1 Cu 104.5(4) 2 3 ?
O7 Te1 Cu 106.5(4) . 3 ?
O6 Te1 Cu 76.5(4) 1_445 3 ?
O6 Te1 Cu 153.2(4) 3_565 3 ?
O6 Te1 Cu 75.6(4) 2_655 3 ?
Pb1 Te1 Cu 102.49(6) . 3 ?
Cu Te1 Cu 115.46(4) 2 3 ?
Cu Te1 Cu 115.46(4) . 3 ?
O7 Te1 Pb2 96.5(4) 3 3_566 ?
O7 Te1 Pb2 46.6(4) 2 3_566 ?
O7 Te1 Pb2 43.4(4) . 3_566 ?
O6 Te1 Pb2 136.9(4) 1_445 3_566 ?
O6 Te1 Pb2 86.8(4) 3_565 3_566 ?
O6 Te1 Pb2 136.6(4) 2_655 3_566 ?
Pb1 Te1 Pb2 137.46(3) . 3_566 ?
Cu Te1 Pb2 61.31(5) 2 3_566 ?
Cu Te1 Pb2 60.10(5) . 3_566 ?
Cu Te1 Pb2 120.05(7) 3 3_566 ?
O4 Te2 O5 98.6(7) . . ?
O4 Te2 O6 94.8(6) . . ?
O5 Te2 O6 93.1(6) . . ?
O4 Te2 O4 86.0(8) . 3_565 ?
O5 Te2 O4 72.7(6) . 3_565 ?
O6 Te2 O4 165.7(5) . 3_565 ?
O4 Te2 O1 72.1(5) . . ?
O5 Te2 O1 138.8(5) . . ?
O6 Te2 O1 127.0(5) . . ?
O4 Te2 O1 66.8(4) 3_565 . ?
O4 Te2 O2 160.8(6) . 6_666 ?
O5 Te2 O2 77.1(6) . 6_666 ?
O6 Te2 O2 67.0(5) . 6_666 ?
O4 Te2 O2 109.9(5) 3_565 6_666 ?
O1 Te2 O2 123.4(4) . 6_666 ?
O4 Te2 Cu 100.6(5) . . ?
O5 Te2 Cu 35.8(4) . . ?
O6 Te2 Cu 128.1(4) . . ?
O4 Te2 Cu 38.3(3) 3_565 . ?
O1 Te2 Cu 104.9(2) . . ?
O2 Te2 Cu 86.9(3) 6_666 . ?
O4 Te2 O2 152.0(6) . 4_556 ?
O5 Te2 O2 74.0(6) . 4_556 ?
O6 Te2 O2 112.2(5) . 4_556 ?
O4 Te2 O2 66.0(5) 3_565 4_556 ?
O1 Te2 O2 95.5(3) . 4_556 ?
O2 Te2 O2 45.2(6) 6_666 4_556 ?
Cu Te2 O2 57.5(3) . 4_556 ?
O3 Se O3 99.1(6) . 2_655 ?
O3 Se O3 99.1(6) . 3_665 ?
O3 Se O3 99.1(6) 2_655 3_665 ?
O3 Se O5 67.8(5) . 2_655 ?
O3 Se O5 166.7(6) 2_655 2_655 ?
O3 Se O5 81.7(6) 3_665 2_655 ?
O3 Se O5 81.7(6) . 3_665 ?
O3 Se O5 67.8(5) 2_655 3_665 ?
O3 Se O5 166.7(6) 3_665 3_665 ?
O5 Se O5 110.6(3) 2_655 3_665 ?
O3 Se O5 166.7(6) . . ?
O3 Se O5 81.7(6) 2_655 . ?
O3 Se O5 67.8(5) 3_665 . ?
O5 Se O5 110.6(3) 2_655 . ?
O5 Se O5 110.6(3) 3_665 . ?
O1 S O2 110.3(7) . 3_565 ?
O1 S O2 110.3(7) . 2_665 ?
O2 S O2 108.7(7) 3_565 2_665 ?
O1 S O2 110.3(7) . . ?
O2 S O2 108.7(7) 3_565 . ?
O2 S O2 108.7(7) 2_665 . ?
O1 S Se 180.0 . 4_556 ?
O2 S Se 69.7(7) 3_565 4_556 ?
O2 S Se 69.7(7) 2_665 4_556 ?
O2 S Se 69.7(7) . 4_556 ?
O1 S Te2 106.02(14) . 6_566 ?
O2 S Te2 58.0(7) 3_565 6_566 ?
O2 S Te2 143.7(8) 2_665 6_566 ?
O2 S Te2 55.8(7) . 6_566 ?
Se S Te2 73.98(14) 4_556 6_566 ?
O1 S Te2 106.02(14) . 5_666 ?
O2 S Te2 55.8(7) 3_565 5_666 ?
O2 S Te2 58.0(7) 2_665 5_666 ?
O2 S Te2 143.7(8) . 5_666 ?
Se S Te2 73.98(14) 4_556 5_666 ?
Te2 S Te2 112.69(12) 6_566 5_666 ?
O1 S Te2 106.02(14) . 4_556 ?
O2 S Te2 143.7(8) 3_565 4_556 ?
O2 S Te2 55.8(7) 2_665 4_556 ?
O2 S Te2 58.0(7) . 4_556 ?
Se S Te2 73.98(14) 4_556 4_556 ?
Te2 S Te2 112.69(12) 6_566 4_556 ?
Te2 S Te2 112.69(12) 5_666 4_556 ?
O1 S Te2 33.70(7) . 2_665 ?
O2 S Te2 86.2(7) 3_565 2_665 ?
O2 S Te2 97.7(7) 2_665 2_665 ?
O2 S Te2 142.7(7) . 2_665 ?
Se S Te2 146.30(7) 4_556 2_665 ?
Te2 S Te2 113.41(12) 6_566 2_665 ?
Te2 S Te2 72.98(7) 5_666 2_665 ?
Te2 S Te2 125.74(15) 4_556 2_665 ?
O1 S Te2 33.70(7) . . ?
O2 S Te2 142.7(7) 3_565 . ?
O2 S Te2 86.2(7) 2_665 . ?
O2 S Te2 97.7(7) . . ?
Se S Te2 146.30(7) 4_556 . ?
Te2 S Te2 125.74(15) 6_566 . ?
Te2 S Te2 113.41(12) 5_666 . ?
Te2 S Te2 72.98(7) 4_556 . ?
Te2 S Te2 57.43(12) 2_665 . ?
O1 S Te2 33.70(7) . 3_565 ?
O2 S Te2 97.7(7) 3_565 3_565 ?
O2 S Te2 142.7(7) 2_665 3_565 ?
O2 S Te2 86.2(7) . 3_565 ?
Se S Te2 146.30(7) 4_556 3_565 ?
Te2 S Te2 72.98(7) 6_566 3_565 ?
Te2 S Te2 125.74(15) 5_666 3_565 ?
Te2 S Te2 113.41(12) 4_556 3_565 ?
Te2 S Te2 57.43(12) 2_665 3_565 ?
Te2 S Te2 57.43(12) . 3_565 ?
O1 S Cu 136.22(10) . 4_556 ?
O2 S Cu 103.9(7) 3_565 4_556 ?
O2 S Cu 82.8(7) 2_665 4_556 ?
O2 S Cu 30.2(7) . 4_556 ?
Se S Cu 43.78(10) 4_556 4_556 ?
Te2 S Cu 70.10(11) 6_566 4_556 ?
Te2 S Cu 115.7(2) 5_666 4_556 ?
Te2 S Cu 46.26(8) 4_556 4_556 ?
Te2 S Cu 169.24(15) 2_665 4_556 ?
Te2 S Cu 112.00(5) . 4_556 ?
Te2 S Cu 116.43(5) 3_565 4_556 ?
S O1 Te2 130.7(3) . 2_665 ?
S O1 Te2 130.7(3) . . ?
Te2 O1 Te2 82.0(5) 2_665 . ?
S O1 Te2 130.7(3) . 3_565 ?
Te2 O1 Te2 82.0(5) 2_665 3_565 ?
Te2 O1 Te2 82.0(5) . 3_565 ?
S O2 Cu 135.5(10) . 4_556 ?
S O2 Te2 101.0(8) . 6_566 ?
Cu O2 Te2 96.0(4) 4_556 6_566 ?
S O2 Te2 98.6(8) . 4_556 ?
Cu O2 Te2 61.0(3) 4_556 4_556 ?
Te2 O2 Te2 156.7(5) 6_566 4_556 ?
S O2 Se 86.1(8) . 4_556 ?
Cu O2 Se 54.8(3) 4_556 4_556 ?
Te2 O2 Se 84.9(4) 6_566 4_556 ?
Te2 O2 Se 84.0(4) 4_556 4_556 ?
Se O3 Cu 104.1(7) . 2_655 ?
Se O3 Pb2 109.3(6) . 3_666 ?
Cu O3 Pb2 102.0(6) 2_655 3_666 ?
Se O3 Cu 144.3(7) . 5_657 ?
Cu O3 Cu 105.4(6) 2_655 5_657 ?
Pb2 O3 Cu 83.5(4) 3_666 5_657 ?
Se O3 Pb2 86.2(5) . 2_656 ?
Cu O3 Pb2 86.2(5) 2_655 2_656 ?
Pb2 O3 Pb2 159.6(5) 3_666 2_656 ?
Cu O3 Pb2 76.3(3) 5_657 2_656 ?
Se O3 Cu 43.9(3) . 3_665 ?
Cu O3 Cu 111.1(5) 2_655 3_665 ?
Pb2 O3 Cu 65.5(3) 3_666 3_665 ?
Cu O3 Cu 135.8(5) 5_657 3_665 ?
Pb2 O3 Cu 129.2(4) 2_656 3_665 ?
Te2 O4 Cu 129.6(8) . 2_665 ?
Te2 O4 Te2 138.1(7) . 2_665 ?
Cu O4 Te2 92.0(6) 2_665 2_665 ?
Te2 O4 Cu 51.6(4) . . ?
Cu O4 Cu 107.0(6) 2_665 . ?
Te2 O4 Cu 118.4(5) 2_665 . ?
Te2 O4 Te2 75.6(4) . 3_565 ?
Cu O4 Te2 131.1(7) 2_665 3_565 ?
Te2 O4 Te2 71.9(4) 2_665 3_565 ?
Cu O4 Te2 51.38(19) . 3_565 ?
Te2 O5 Cu 110.2(7) . . ?
Te2 O5 Pb2 131.4(7) . 1_556 ?
Cu O5 Pb2 110.4(6) . 1_556 ?
Te2 O5 Se 133.7(7) . . ?
Cu O5 Se 73.1(5) . . ?
Pb2 O5 Se 83.6(4) 1_556 . ?
Te2 O5 Cu 69.6(5) . 2_665 ?
Cu O5 Cu 118.6(6) . 2_665 ?
Pb2 O5 Cu 68.1(3) 1_556 2_665 ?
Se O5 Cu 151.6(5) . 2_665 ?
Te2 O5 Cu 106.4(6) . 3_665 ?
Cu O5 Cu 125.5(6) . 3_665 ?
Pb2 O5 Cu 69.1(3) 1_556 3_665 ?
Se O5 Cu 52.4(3) . 3_665 ?
Cu O5 Cu 111.3(4) 2_665 3_665 ?
Te1 O6 Te2 136.7(7) 1_665 . ?
Te1 O6 Pb1 95.2(5) 1_665 1_665 ?
Te2 O6 Pb1 121.3(6) . 1_665 ?
Te1 O6 Cu 72.5(4) 1_665 2_665 ?
Te2 O6 Cu 69.3(4) . 2_665 ?
Pb1 O6 Cu 120.0(5) 1_665 2_665 ?
Te1 O6 Cu 71.8(4) 1_665 3_665 ?
Te2 O6 Cu 104.6(5) . 3_665 ?
Pb1 O6 Cu 119.1(4) 1_665 3_665 ?
Cu O6 Cu 112.0(4) 2_665 3_665 ?
Te1 O6 Pb2 63.9(4) 1_665 1_556 ?
Te2 O6 Pb2 78.0(4) . 1_556 ?
Pb1 O6 Pb2 159.1(5) 1_665 1_556 ?
Cu O6 Pb2 55.84(19) 2_665 1_556 ?
Cu O6 Pb2 56.8(2) 3_665 1_556 ?
Te1 O7 Cu 133.2(8) . . ?
Te1 O7 Pb2 105.7(6) . 3_566 ?
Cu O7 Pb2 103.9(6) . 3_566 ?
Te1 O7 Pb2 102.0(5) . 2_656 ?
Cu O7 Pb2 103.0(5) . 2_656 ?
Pb2 O7 Pb2 107.0(5) 3_566 2_656 ?
Te1 O7 Te2 77.9(4) . 3_565 ?
Cu O7 Te2 71.2(4) . 3_565 ?
Pb2 O7 Te2 82.1(3) 3_566 3_565 ?
Pb2 O7 Te2 170.4(5) 2_656 3_565 ?
Te1 O7 Cu 155.1(6) . 4_557 ?
Cu O7 Cu 71.4(4) . 4_557 ?
Pb2 O7 Cu 64.6(3) 3_566 4_557 ?
Pb2 O7 Cu 62.6(3) 2_656 4_557 ?
Te2 O7 Cu 120.7(4) 3_565 4_557 ?
Te1 O7 Se 127.4(5) . . ?
Cu O7 Se 43.5(3) . . ?
Pb2 O7 Se 126.7(4) 3_566 . ?
Pb2 O7 Se 61.6(3) 2_656 . ?
Te2 O7 Se 110.7(4) 3_565 . ?
Cu O7 Se 64.8(2) 4_557 . ?
Te1 O7 Te2 62.7(4) . 2_655 ?
Cu O7 Te2 89.9(5) . 2_655 ?
Pb2 O7 Te2 166.1(5) 3_566 2_655 ?
Pb2 O7 Te2 70.2(3) 2_656 2_655 ?
Te2 O7 Te2 101.7(3) 3_565 2_655 ?
Cu O7 Te2 122.4(3) 4_557 2_655 ?
Se O7 Te2 64.7(2) . 2_655 ?
Pb1 O8 O2 118.4(6) 1_655 5_656 ?
Pb1 O8 Te2 88.1(4) 1_655 1_545 ?
O2 O8 Te2 92.5(4) 5_656 1_545 ?
Pb1 O8 Te2 88.1(4) 1_655 6_666 ?
O2 O8 Te2 89.3(4) 5_656 6_666 ?
Te2 O8 Te2 176.2(9) 1_545 6_666 ?
Pb1 O8 Te2 145.5(2) 1_655 5_656 ?
O2 O8 Te2 81.9(6) 5_656 5_656 ?
Te2 O8 Te2 120.4(6) 1_545 5_656 ?
Te2 O8 Te2 63.1(3) 6_666 5_656 ?
Pb1 O8 Te2 145.5(2) 1_655 2_655 ?
O2 O8 Te2 50.0(5) 5_656 2_655 ?
Te2 O8 Te2 63.1(3) 1_545 2_655 ?
Te2 O8 Te2 120.4(6) 6_666 2_655 ?
Te2 O8 Te2 69.0(4) 5_656 2_655 ?
Pb1 O8 Te2 71.9(3) 1_655 3_665 ?
O2 O8 Te2 48.2(4) 5_656 3_665 ?
Te2 O8 Te2 103.31(19) 1_545 3_665 ?
Te2 O8 Te2 75.49(13) 6_666 3_665 ?
Te2 O8 Te2 114.7(3) 5_656 3_665 ?
Te2 O8 Te2 95.4(2) 2_655 3_665 ?
Pb1 O8 Te2 71.9(3) 1_655 4_546 ?
O2 O8 Te2 164.4(7) 5_656 4_546 ?
Te2 O8 Te2 75.49(13) 1_545 4_546 ?
Te2 O8 Te2 103.31(19) 6_666 4_546 ?
Te2 O8 Te2 95.4(2) 5_656 4_546 ?
Te2 O8 Te2 114.7(3) 2_655 4_546 ?
Te2 O8 Te2 143.8(7) 3_665 4_546 ?
 
_refine_diff_density_max    2.965
_refine_diff_density_min   -2.797
_refine_diff_density_rms    0.478



