 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'tetrahedrite-(Hg)'
_chemical_compound_source         'Buca della Vena mine, Apuan Alps, Italy'
_chemical_formula_analytical
;      
Ag0.07 Cu9.43 Fe0.06 Hg1.66 S12.69 Sb4 
Se0.01 Zn0.34
; 
_chemical_formula_sum
 'Cu10.2 Hg1.8 Sb4 S13'
_chemical_formula_weight          1913.09

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Ag'  'Ag'  -0.8971   1.1015
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Hg'  'Hg'  -2.3894   9.2266
 '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'
 '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                    10.5057(8)
_cell_length_b                    10.5057(8)
_cell_length_c                    10.5057(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1159.5(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     1856
_cell_measurement_theta_min       4.753
_cell_measurement_theta_max       35.033
 
_exptl_crystal_description        'equant'
_exptl_crystal_colour             'black'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     5.480          
_exptl_crystal_F_000              1703.6
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.075
_exptl_crystal_size_min           0.050
_exptl_absorpt_coefficient_mu     26.734
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.658
_exptl_absorpt_correction_T_max   0.788
_exptl_absorpt_process_details    '(SADABS, Sheldrick, 1996)'
_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 Smart Breeze'
_diffrn_reflns_number             2243
_diffrn_reflns_av_unetI/netI      0.0396
_diffrn_reflns_av_R_equivalents   0.0274
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.742
_diffrn_reflns_theta_max          29.963
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              348
_reflns_number_gt                 335
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.741
_reflns_Friedel_fraction_max      1.000
_reflns_Friedel_fraction_full     1.000
 
_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)+13.9240P] 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        0.00031(11)
_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    0.06(4)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          348
_refine_ls_number_parameters      20
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0212
_refine_ls_R_factor_gt            0.0190
_refine_ls_wR_factor_ref          0.0696
_refine_ls_wR_factor_gt           0.0446
_refine_ls_goodness_of_fit_ref    1.350
_refine_ls_restrained_S_all       1.350
_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 0.000000 0.000000 0.7865(3) 0.0547(11) Uani 1 4 d S T P . .
M1CU Cu 0.250000 0.500000 0.000000 0.0252(6) Uani 0.700(6) 4 d S T P . .
M1HG Hg 0.250000 0.500000 0.000000 0.0252(6) Uani 0.300(6) 4 d S T P . .
X Sb 0.26540(6) 0.26540(6) 0.26540(6) 0.0157(3) Uani 1 6 d S T P . .
S1 S 0.1141(2) 0.1141(2) 0.3574(3) 0.0189(6) Uani 1 2 d S T P . .
S2 S 0.000000 0.000000 0.000000 0.0195(18) 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 2.242(4) 1_556 ?
M2CU S1 2.272(3) 2_556 ?
M2CU S1 2.272(3) 4_556 ?
M1CU S1 2.3913(18) 28 ?
M1CU S1 2.3913(18) 9 ?
M1CU S1 2.3913(18) 11_565 ?
M1CU S1 2.3913(18) 27_554 ?
X S1 2.447(3) 14 ?
X S1 2.447(3) 9 ?
X S1 2.447(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 131.74(10) 1_556 2_556 ?
S2 M2CU S1 131.74(10) 1_556 4_556 ?
S1 M2CU S1 96.5(2) 2_556 4_556 ?
S1 M1CU S1 110.88(7) 28 9 ?
S1 M1CU S1 110.88(7) 28 11_565 ?
S1 M1CU S1 106.68(13) 9 11_565 ?
S1 M1CU S1 106.68(13) 28 27_554 ?
S1 M1CU S1 110.88(7) 9 27_554 ?
S1 M1CU S1 110.88(7) 11_565 27_554 ?
S1 X S1 95.24(10) 14 9 ?
S1 X S1 95.24(10) 14 . ?
S1 X S1 95.24(10) 9 . ?
M2CU S1 M1CU 117.88(10) 2_556 29_455 ?
M2CU S1 M1CU 117.88(10) 2_556 27 ?
M1CU S1 M1CU 101.90(10) 29_455 27 ?
M2CU S1 X 114.98(13) 2_556 . ?
M1CU S1 X 100.67(9) 29_455 . ?
M1CU S1 X 100.67(9) 27 . ?
M2CU S2 M2CU 90.0 15_655 1_554 ?
M2CU S2 M2CU 90.0 15_655 2_556 ?
M2CU S2 M2CU 180.0 1_554 2_556 ?
M2CU S2 M2CU 90.0 15_655 9_545 ?
M2CU S2 M2CU 90.0 1_554 9_545 ?
M2CU S2 M2CU 90.0 2_556 9_545 ?
M2CU S2 M2CU 90.0 15_655 10_565 ?
M2CU S2 M2CU 90.0 1_554 10_565 ?
M2CU S2 M2CU 90.0 2_556 10_565 ?
M2CU S2 M2CU 180.0 9_545 10_565 ?
M2CU S2 M2CU 180.0 15_655 13_455 ?
M2CU S2 M2CU 90.0 1_554 13_455 ?
M2CU S2 M2CU 90.0 2_556 13_455 ?
M2CU S2 M2CU 90.0 9_545 13_455 ?
M2CU S2 M2CU 90.0 10_565 13_455 ?
 
_refine_diff_density_max    0.840
_refine_diff_density_min   -0.908
_refine_diff_density_rms    0.230



