 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'tennantite-(Cu)'
_chemical_compound_source         'Layo, Peru'
_chemical_formula_analytical
;      
As3.80 Cu11.36 Fe0.58 S12.67 Sb0.23 Zn0.02
; 
_chemical_formula_sum
 'As3.775 Cu11.90 S13 Sb0.225' 
_chemical_formula_weight         1483.07

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'
 '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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 '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                    10.1710(8)
_cell_length_b                    10.1710(8)
_cell_length_c                    10.1710(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1052.2(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     819
_cell_measurement_theta_min       2.83
_cell_measurement_theta_max       28.79
 
_exptl_crystal_description        'anhedral'
_exptl_crystal_colour             'black'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.681          
_exptl_crystal_F_000              1378.1
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.060
_exptl_crystal_size_mid           0.040
_exptl_crystal_size_min           0.030
_exptl_absorpt_coefficient_mu     19.211
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_T_max  0.7458
_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             1693
_diffrn_reflns_av_unetI/netI      0.0301
_diffrn_reflns_av_R_equivalents   0.0296
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          4.007
_diffrn_reflns_theta_max          28.790
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.988
_diffrn_measured_fraction_theta_full  0.983
_diffrn_reflns_Laue_measured_fraction_max    0.988
_diffrn_reflns_Laue_measured_fraction_full   0.983
_diffrn_reflns_point_group_measured_fraction_max   0.989
_diffrn_reflns_point_group_measured_fraction_full  0.985
_reflns_number_total              279
_reflns_number_gt                 263
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.733
_reflns_Friedel_fraction_max      0.992
_reflns_Friedel_fraction_full     0.988
 
_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)+1.3875P] 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        0.00039(14)
_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    0.03(3)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          279
_refine_ls_number_parameters      24
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0202
_refine_ls_R_factor_gt            0.0178
_refine_ls_wR_factor_ref          0.0375
_refine_ls_wR_factor_gt           0.0368
_refine_ls_goodness_of_fit_ref    0.968
_refine_ls_restrained_S_all       0.968
_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
M2A Cu 0.7830(3) 0.000000 0.000000 0.034(2) Uani 0.669(18) 4 d S T P . .
M2B Cu 0.7814(6) 0.0417(8) -0.0417(8) 0.034(2) Uani 0.166(9) 2 d S T P . .
M1CU Cu 0.750000 0.500000 0.000000 0.0195(4) Uani 0.86(4) 4 d S T P . .
M1FE Fe 0.750000 0.500000 0.000000 0.0195(4) Uani 0.14(4) 4 d S T P . .
XAS As 0.73827(6) 0.73827(6) 0.73827(6) 0.0158(3) Uani 0.947(11) 6 d S T P . .
XSB Sb 0.73827(6) 0.73827(6) 0.73827(6) 0.0158(3) Uani 0.053(11) 6 d S T P . .
S1 S 0.88030(12) 0.88030(12) 0.64200(15) 0.0151(4) Uani 1 2 d S T P . .
S2 S 0.000000 0.000000 0.000000 0.0221(10) 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
M2A M2B 0.600(11) . ?
M2A M2B 0.600(11) 2 ?
M2A S2 2.207(3) 1_655 ?
M2A S1 2.2410(19) 14_544 ?
M2A S1 2.2410(19) 13_566 ?
M2A M2B 2.881(5) 6_665 ?
M2A M2B 2.881(5) 12_656 ?
M2A M2B 2.881(5) 10_654 ?
M2A M2B 2.881(5) 7_645 ?
M2B M2B 1.20(2) 2 ?
M2B S2 2.302(7) 1_655 ?
M2B S1 2.310(4) 14_544 ?
M2B S1 2.310(4) 13_566 ?
M2B M2B 2.544(13) 6_665 ?
M2B M2B 2.544(13) 10_654 ?
M2B XAS 2.835(11) 28_645 ?
M1CU S1 2.3075(10) 28_645 ?
M1CU S1 2.3075(10) 9_554 ?
M1CU S1 2.3075(10) 11_566 ?
M1CU S1 2.3075(10) 27_664 ?
XAS S1 2.2655(15) 14 ?
XAS S1 2.2655(15) 9 ?
XAS S1 2.2655(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
M2B M2A M2B 176.9(14) . 2 ?
M2B M2A S2 91.5(7) . 1_655 ?
M2B M2A S2 91.5(7) 2 1_655 ?
M2B M2A S1 89.0(5) . 14_544 ?
M2B M2A S1 89.0(5) 2 14_544 ?
S2 M2A S1 129.80(7) 1_655 14_544 ?
M2B M2A S1 89.0(5) . 13_566 ?
M2B M2A S1 89.0(5) 2 13_566 ?
S2 M2A S1 129.80(7) 1_655 13_566 ?
S1 M2A S1 100.40(13) 14_544 13_566 ?
M2B M2A M2B 50.7(5) . 6_665 ?
M2B M2A M2B 131.8(7) 2 6_665 ?
S2 M2A M2B 51.77(19) 1_655 6_665 ?
S1 M2A M2B 137.3(2) 14_544 6_665 ?
S1 M2A M2B 93.26(8) 13_566 6_665 ?
M2B M2A M2B 131.8(7) . 12_656 ?
M2B M2A M2B 50.7(5) 2 12_656 ?
S2 M2A M2B 51.77(19) 1_655 12_656 ?
S1 M2A M2B 137.3(2) 14_544 12_656 ?
S1 M2A M2B 93.26(8) 13_566 12_656 ?
M2B M2A M2B 81.0(5) 6_665 12_656 ?
M2B M2A M2B 50.7(5) . 10_654 ?
M2B M2A M2B 131.8(7) 2 10_654 ?
S2 M2A M2B 51.77(19) 1_655 10_654 ?
S1 M2A M2B 93.26(8) 14_544 10_654 ?
S1 M2A M2B 137.3(2) 13_566 10_654 ?
M2B M2A M2B 52.40(19) 6_665 10_654 ?
M2B M2A M2B 103.5(4) 12_656 10_654 ?
M2B M2A M2B 131.8(7) . 7_645 ?
M2B M2A M2B 50.7(5) 2 7_645 ?
S2 M2A M2B 51.77(19) 1_655 7_645 ?
S1 M2A M2B 93.26(8) 14_544 7_645 ?
S1 M2A M2B 137.3(2) 13_566 7_645 ?
M2B M2A M2B 103.5(4) 6_665 7_645 ?
M2B M2A M2B 52.40(19) 12_656 7_645 ?
M2B M2A M2B 81.0(5) 10_654 7_645 ?
M2A M2B M2B 1.5(7) . 2 ?
M2A M2B S2 73.4(8) . 1_655 ?
M2B M2B S2 74.9(3) 2 1_655 ?
M2A M2B S1 75.9(5) . 14_544 ?
M2B M2B S1 75.0(3) 2 14_544 ?
S2 M2B S1 121.7(3) 1_655 14_544 ?
M2A M2B S1 75.9(5) . 13_566 ?
M2B M2B S1 75.0(3) 2 13_566 ?
S2 M2B S1 121.7(3) 1_655 13_566 ?
S1 M2B S1 96.4(3) 14_544 13_566 ?
M2A M2B M2B 118.7(6) . 6_665 ?
M2B M2B M2B 120.0 2 6_665 ?
S2 M2B M2B 56.5(2) 1_655 6_665 ?
S1 M2B M2B 159.5(2) 14_544 6_665 ?
S1 M2B M2B 101.03(15) 13_566 6_665 ?
M2A M2B M2B 118.7(6) . 10_654 ?
M2B M2B M2B 120.000(1) 2 10_654 ?
S2 M2B M2B 56.5(2) 1_655 10_654 ?
S1 M2B M2B 101.03(15) 14_544 10_654 ?
S1 M2B M2B 159.5(2) 13_566 10_654 ?
M2B M2B M2B 60.000(1) 6_665 10_654 ?
M2A M2B XAS 177.5(8) . 28_645 ?
M2B M2B XAS 175.94(12) 2 28_645 ?
S2 M2B XAS 109.2(3) 1_655 28_645 ?
S1 M2B XAS 102.4(3) 14_544 28_645 ?
S1 M2B XAS 102.4(3) 13_566 28_645 ?
M2B M2B XAS 63.34(10) 6_665 28_645 ?
M2B M2B XAS 63.34(10) 10_654 28_645 ?
M2A M2B M2A 108.2(7) . 5_665 ?
M2B M2B M2A 109.5(2) 2 5_665 ?
S2 M2B M2A 48.84(12) 1_655 5_665 ?
S1 M2B M2A 164.6(2) 14_544 5_665 ?
S1 M2B M2A 99.01(6) 13_566 5_665 ?
M2B M2B M2A 10.5(2) 6_665 5_665 ?
M2B M2B M2A 63.80(10) 10_654 5_665 ?
XAS M2B M2A 73.9(2) 28_645 5_665 ?
M2A M2B M2A 108.2(7) . 9_654 ?
M2B M2B M2A 109.5(2) 2 9_654 ?
S2 M2B M2A 48.84(12) 1_655 9_654 ?
S1 M2B M2A 99.01(6) 14_544 9_654 ?
S1 M2B M2A 164.6(2) 13_566 9_654 ?
M2B M2B M2A 63.80(10) 6_665 9_654 ?
M2B M2B M2A 10.5(2) 10_654 9_654 ?
XAS M2B M2A 73.9(2) 28_645 9_654 ?
M2A M2B M2A 65.59(16) 5_665 9_654 ?
S1 M1CU S1 109.26(4) 28_645 9_554 ?
S1 M1CU S1 109.26(4) 28_645 11_566 ?
S1 M1CU S1 109.89(8) 9_554 11_566 ?
S1 M1CU S1 109.89(8) 28_645 27_664 ?
S1 M1CU S1 109.26(4) 9_554 27_664 ?
S1 M1CU S1 109.26(4) 11_566 27_664 ?
S1 XAS S1 98.31(5) 14 9 ?
S1 XAS S1 98.31(5) 14 . ?
S1 XAS S1 98.31(5) 9 . ?
S1 XAS M2B 100.95(8) 14 29_565 ?
S1 XAS M2B 150.34(13) 9 29_565 ?
S1 XAS M2B 100.95(8) . 29_565 ?
S1 XAS M2B 150.34(13) 14 28_655 ?
S1 XAS M2B 100.95(8) 9 28_655 ?
S1 XAS M2B 100.95(8) . 28_655 ?
M2B XAS M2B 53.3(2) 29_565 28_655 ?
S1 XAS M2B 100.95(8) 14 35_556 ?
S1 XAS M2B 100.95(8) 9 35_556 ?
S1 XAS M2B 150.34(13) . 35_556 ?
M2B XAS M2B 53.3(2) 29_565 35_556 ?
M2B XAS M2B 53.3(2) 28_655 35_556 ?
M2A S1 XAS 114.59(8) 9_665 . ?
M2A S1 M1CU 115.22(6) 9_665 29_565 ?
XAS S1 M1CU 103.93(5) . 29_565 ?
M2A S1 M1CU 115.22(6) 9_665 27_665 ?
XAS S1 M1CU 103.93(5) . 27_665 ?
M1CU S1 M1CU 102.38(6) 29_565 27_665 ?
M2A S1 M2B 15.1(3) 9_665 9_665 ?
XAS S1 M2B 114.00(13) . 9_665 ?
M1CU S1 M2B 101.9(3) 29_565 9_665 ?
M1CU S1 M2B 127.7(2) 27_665 9_665 ?
M2A S1 M2B 15.1(3) 9_665 10_665 ?
XAS S1 M2B 114.00(13) . 10_665 ?
M1CU S1 M2B 127.7(2) 29_565 10_665 ?
M1CU S1 M2B 101.9(3) 27_665 10_665 ?
M2B S1 M2B 30.1(6) 9_665 10_665 ?
M2A S2 M2A 90.0 11_556 1_455 ?
M2A S2 M2A 90.0 11_556 3_655 ?
M2A S2 M2A 180.0 1_455 3_655 ?
M2A S2 M2A 90.0 11_556 5_565 ?
M2A S2 M2A 90.0 1_455 5_565 ?
M2A S2 M2A 90.0 3_655 5_565 ?
M2A S2 M2A 90.0 11_556 7_545 ?
M2A S2 M2A 90.0 1_455 7_545 ?
M2A S2 M2A 90.0 3_655 7_545 ?
M2A S2 M2A 180.0 5_565 7_545 ?
M2A S2 M2A 180.0 11_556 9_554 ?
M2A S2 M2A 90.0 1_455 9_554 ?
M2A S2 M2A 90.0 3_655 9_554 ?
M2A S2 M2A 90.0 5_565 9_554 ?
M2A S2 M2A 90.0 7_545 9_554 ?
M2A S2 M2B 15.1(3) 11_556 11_556 ?
M2A S2 M2B 100.61(19) 1_455 11_556 ?
M2A S2 M2B 79.39(19) 3_655 11_556 ?
M2A S2 M2B 79.39(19) 5_565 11_556 ?
M2A S2 M2B 100.61(19) 7_545 11_556 ?
M2A S2 M2B 164.9(3) 9_554 11_556 ?
M2A S2 M2B 79.39(19) 11_556 5_565 ?
M2A S2 M2B 100.61(19) 1_455 5_565 ?
M2A S2 M2B 79.39(19) 3_655 5_565 ?
M2A S2 M2B 15.1(3) 5_565 5_565 ?
M2A S2 M2B 164.9(3) 7_545 5_565 ?
M2A S2 M2B 100.61(19) 9_554 5_565 ?
M2B S2 M2B 67.1(4) 11_556 5_565 ?
M2A S2 M2B 79.39(19) 11_556 4_655 ?
M2A S2 M2B 164.9(3) 1_455 4_655 ?
M2A S2 M2B 15.1(3) 3_655 4_655 ?
M2A S2 M2B 79.39(19) 5_565 4_655 ?
M2A S2 M2B 100.61(19) 7_545 4_655 ?
M2A S2 M2B 100.61(19) 9_554 4_655 ?
M2B S2 M2B 67.1(4) 11_556 4_655 ?
M2B S2 M2B 67.1(4) 5_565 4_655 ?
M2A S2 M2B 164.9(3) 11_556 10_554 ?
M2A S2 M2B 79.39(19) 1_455 10_554 ?
M2A S2 M2B 100.61(19) 3_655 10_554 ?
M2A S2 M2B 79.39(19) 5_565 10_554 ?
M2A S2 M2B 100.61(19) 7_545 10_554 ?
M2A S2 M2B 15.1(3) 9_554 10_554 ?
M2B S2 M2B 158.8(4) 11_556 10_554 ?
M2B S2 M2B 91.94(7) 5_565 10_554 ?
M2B S2 M2B 108.8(3) 4_655 10_554 ?
M2A S2 M2B 164.9(3) 11_556 9_554 ?
M2A S2 M2B 100.61(19) 1_455 9_554 ?
M2A S2 M2B 79.39(19) 3_655 9_554 ?
M2A S2 M2B 100.61(19) 5_565 9_554 ?
M2A S2 M2B 79.39(19) 7_545 9_554 ?
M2A S2 M2B 15.1(3) 9_554 9_554 ?
M2B S2 M2B 158.8(4) 11_556 9_554 ?
M2B S2 M2B 108.8(3) 5_565 9_554 ?
M2B S2 M2B 91.94(7) 4_655 9_554 ?
M2B S2 M2B 30.2(5) 10_554 9_554 ?
M2A S2 M2B 79.39(19) 11_556 2_455 ?
M2A S2 M2B 15.1(3) 1_455 2_455 ?
M2A S2 M2B 164.9(3) 3_655 2_455 ?
M2A S2 M2B 100.61(19) 5_565 2_455 ?
M2A S2 M2B 79.39(19) 7_545 2_455 ?
M2A S2 M2B 100.61(19) 9_554 2_455 ?
M2B S2 M2B 91.94(7) 11_556 2_455 ?
M2B S2 M2B 108.8(3) 5_565 2_455 ?
M2B S2 M2B 158.8(4) 4_655 2_455 ?
M2B S2 M2B 91.94(7) 10_554 2_455 ?
M2B S2 M2B 108.8(3) 9_554 2_455 ?
 
_refine_diff_density_max    0.267
_refine_diff_density_min   -0.284
_refine_diff_density_rms    0.067



