 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'stibiogoldfieldite'
_chemical_compound_source         'Mohawk mine, Nevada, U.S.A.'
_chemical_formula_analytical
;      
Ag0.04 As0.63 Bi0.22 Cu12.05 Fe0.01 S12.98 Sb1.12
Se0.11 Te2.02 Zn0.03
; 
_chemical_formula_sum
 'As0.44 Cu12 S13 Te3.56' 
_chemical_formula_weight         1666.6

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Te'  'Te'  -0.5308   1.6751
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'   0.2839   1.4301
 '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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'As'  'As'   0.0499   2.0058
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            217
_space_group_name_H-M_alt         'I -4 3 m'
_space_group_name_Hall            'I -4 2 3'
 
_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'
 'x, -y, -z'
 '-x, -y, z'
 '-x, y, -z'
 'y, -x, -z'
 '-y, -x, z'
 '-y, x, -z'
 'y, x, z'
 'y, z, x'
 '-y, -z, x'
 'y, -z, -x'
 '-y, z, -x'
 'z, -y, -x'
 'z, y, x'
 '-z, y, -x'
 '-z, -y, x'
 'z, x, y'
 '-z, x, -y'
 '-z, -x, y'
 'z, -x, -y'
 'x, z, y'
 'x, -z, -y'
 '-x, z, -y'
 '-x, -z, y'
 'x+1/2, y+1/2, z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 '-y+1/2, -x+1/2, z+1/2'
 '-y+1/2, x+1/2, -z+1/2'
 'y+1/2, x+1/2, z+1/2'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, -z+1/2, x+1/2'
 'y+1/2, -z+1/2, -x+1/2'
 '-y+1/2, z+1/2, -x+1/2'
 'z+1/2, -y+1/2, -x+1/2'
 'z+1/2, y+1/2, x+1/2'
 '-z+1/2, y+1/2, -x+1/2'
 '-z+1/2, -y+1/2, x+1/2'
 'z+1/2, x+1/2, y+1/2'
 '-z+1/2, x+1/2, -y+1/2'
 '-z+1/2, -x+1/2, y+1/2'
 'z+1/2, -x+1/2, -y+1/2'
 'x+1/2, z+1/2, y+1/2'
 'x+1/2, -z+1/2, -y+1/2'
 '-x+1/2, z+1/2, -y+1/2'
 '-x+1/2, -z+1/2, y+1/2'
 
_cell_length_a                    10.3466(17)
_cell_length_b                    10.3466(17)
_cell_length_c                    10.3466(17)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1107.6(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     896
_cell_measurement_theta_min       2.784
_cell_measurement_theta_max       31.392
 
_exptl_crystal_description        'anhedral'
_exptl_crystal_colour             'dark grey'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.997          
_exptl_crystal_F_000              1511.3
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.110
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.075
_exptl_absorpt_coefficient_mu     17.729
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5100
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_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   'Bruker Apex II'
_diffrn_reflns_number             1560
_diffrn_reflns_av_unetI/netI      0.0400
_diffrn_reflns_av_R_equivalents   0.0391
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          4.826
_diffrn_reflns_theta_max          32.744
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.899
_diffrn_measured_fraction_theta_full  0.976
_diffrn_reflns_Laue_measured_fraction_max    0.899
_diffrn_reflns_Laue_measured_fraction_full   0.976
_diffrn_reflns_point_group_measured_fraction_max   0.899
_diffrn_reflns_point_group_measured_fraction_full  0.982
_reflns_number_total              331
_reflns_number_gt                 285
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.761
_reflns_Friedel_fraction_max      0.900
_reflns_Friedel_fraction_full     0.989
 
_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_data_collection      'Apex3 (Bruker AXS Inc., 2016)'
_computing_cell_refinement      'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_reduction       'Apex3 (Bruker AXS Inc., 2016)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+18.1789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.00071(15)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    -0.05(9)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          331
_refine_ls_number_parameters      20
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0485
_refine_ls_R_factor_gt            0.0316
_refine_ls_wR_factor_ref          0.0715
_refine_ls_wR_factor_gt           0.0647
_refine_ls_goodness_of_fit_ref    1.124
_refine_ls_restrained_S_all       1.124
_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
M2CU Cu 0.7827(4) 0.000000 0.000000 0.0562(12) Uani 1 4 d S T P . .
M1 Cu 0.750000 0.500000 0.000000 0.0271(9) Uani 1 4 d S T P . .
Te Te 0.73695(8) 0.73695(8) 0.73695(8) 0.0192(4) Uani 0.89(3) 6 d S T P . .
As As 0.73695(8) 0.73695(8) 0.73695(8) 0.0192(4) Uani 0.11(3) 6 d S T P . .
S1 S 0.8845(2) 0.8845(2) 0.6387(3) 0.0175(7) Uani 1 2 d S T P . .
S2 S 0.000000 0.000000 0.000000 0.023(2) Uani 1 24 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
M2CU S2 2.249(4) 1_655 ?
M2CU S1 2.252(3) 14_544 ?
M2CU S1 2.252(3) 13_566 ?
M1 S1 2.3291(19) 28_645 ?
M1 S1 2.3291(19) 9_554 ?
M1 S1 2.3291(19) 27_664 ?
M1 S1 2.3291(19) 11_566 ?
As S1 2.387(3) 14 ?
As S1 2.387(3) 9 ?
As S1 2.387(3) . ?
 
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
S2 M2CU S1 131.40(13) 1_655 14_544 ?
S2 M2CU S1 131.40(13) 1_655 13_566 ?
S1 M2CU S1 97.2(3) 14_544 13_566 ?
S1 M1 S1 110.93(8) 28_645 9_554 ?
S1 M1 S1 106.60(16) 28_645 27_664 ?
S1 M1 S1 110.93(8) 9_554 27_664 ?
S1 M1 S1 110.93(8) 28_645 11_566 ?
S1 M1 S1 106.60(16) 9_554 11_566 ?
S1 M1 S1 110.93(8) 27_664 11_566 ?
S1 As S1 97.80(10) 14 9 ?
S1 As S1 97.80(10) 14 . ?
S1 As S1 97.80(10) 9 . ?
M2CU S1 M1 116.90(12) 9_665 29_565 ?
M2CU S1 M1 116.90(12) 9_665 27_665 ?
M1 S1 M1 103.50(12) 29_565 27_665 ?
M2CU S1 As 113.40(16) 9_665 . ?
M1 S1 As 102.02(10) 29_565 . ?
M1 S1 As 102.02(10) 27_665 . ?
M2CU S2 M2CU 90.0 11_556 1_455 ?
M2CU S2 M2CU 90.0 11_556 3_655 ?
M2CU S2 M2CU 180.0 1_455 3_655 ?
M2CU S2 M2CU 90.0 11_556 5_565 ?
M2CU S2 M2CU 90.0 1_455 5_565 ?
M2CU S2 M2CU 90.0 3_655 5_565 ?
M2CU S2 M2CU 90.0 11_556 7_545 ?
M2CU S2 M2CU 90.0 1_455 7_545 ?
M2CU S2 M2CU 90.0 3_655 7_545 ?
M2CU S2 M2CU 180.0 5_565 7_545 ?
M2CU S2 M2CU 180.0 11_556 9_554 ?
M2CU S2 M2CU 90.0 1_455 9_554 ?
M2CU S2 M2CU 90.0 3_655 9_554 ?
M2CU S2 M2CU 90.0 5_565 9_554 ?
M2CU S2 M2CU 90.0 7_545 9_554 ?
 
_refine_diff_density_max    1.512
_refine_diff_density_min   -1.570
_refine_diff_density_rms    0.242



