data_8342-4
_audit_creation_date               2021-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '0.67(Co4.5 S3 Sb0.15 Sn2.85)'
_chemical_formula_sum              'Co3 S2 Sb0.10 Sn1.90'
_chemical_formula_weight           478.60
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'Co' 'Co' 0.3494 0.9721 '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'
 'Sn' 'Sn' -0.6537 1.4246
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'trigonal'
_space_group_IT_number             166
_space_group_name_H-M_alt          'R -3 m'
_space_group_name_Hall             '-R 3 2"'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -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'
 'y+2/3, x+1/3, -z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '-x+2/3, -x+y+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'
 'y+1/3, x+2/3, -z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, 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'
 '-y+2/3, -x+1/3, z+1/3'
 '-x+y+2/3, y+1/3, z+1/3'
 'x+2/3, x-y+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'
 '-y+1/3, -x+2/3, z+2/3'
 '-x+y+1/3, y+2/3, z+2/3'
 'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                     5.3658(4)
_cell_length_b                     5.3658(4)
_cell_length_c                     13.1382(15)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  120
_cell_volume                       327.59(6)
_cell_formula_units_Z              3
_cell_measurement_reflns_used      595
_cell_measurement_temperature      298.00(10)
_cell_measurement_theta_max        28.4690
_cell_measurement_theta_min        4.6020
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      23.228
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.51960
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              black
_exptl_crystal_colour_primary      black
_exptl_crystal_density_diffrn      7.278
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               639
_exptl_crystal_size_max            0.04
_exptl_crystal_size_mid            0.04
_exptl_crystal_size_min            0.03
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0523
_diffrn_reflns_av_unetI/netI       0.0299
_diffrn_reflns_Laue_measured_fraction_full  0.989
_diffrn_reflns_Laue_measured_fraction_max  0.944
_diffrn_reflns_limit_h_max         7
_diffrn_reflns_limit_h_min         -6
_diffrn_reflns_limit_k_max         7
_diffrn_reflns_limit_k_min         -6
_diffrn_reflns_limit_l_max         14
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              785
_diffrn_reflns_point_group_measured_fraction_full  0.989
_diffrn_reflns_point_group_measured_fraction_max  0.944
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           28.530
_diffrn_reflns_theta_min           4.653
_diffrn_ambient_environment        air
_diffrn_ambient_temperature        298.00(10)
_diffrn_detector                   'CCD area detector'
_diffrn_detector_area_resol_mean   7.9
_diffrn_detector_type              'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full  0.989
_diffrn_measured_fraction_theta_max  0.944
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -68.00  68.00   0.50    0.50    --  -20.50  57.00   0.00  272
  2  ω    -48.00  30.00   0.50    0.50    --  -20.50 -77.00 -90.00  156
  3  ω    -39.00  15.00   0.50    0.50    --  -20.50 -82.00  30.00  108
  4  ω    -68.00  68.00   0.50    0.50    --  -20.50  57.00-150.00  272
;
_diffrn_measurement_device         'three-circle diffractometer'
_diffrn_measurement_device_type    'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0471511697
_diffrn_orient_matrix_UB_12        -0.1020498652
_diffrn_orient_matrix_UB_13        -0.0018493652
_diffrn_orient_matrix_UB_21        0.0308358722
_diffrn_orient_matrix_UB_22        0.0195359361
_diffrn_orient_matrix_UB_23        0.0528731361
_diffrn_orient_matrix_UB_31        -0.1417928754
_diffrn_orient_matrix_UB_32        -0.1118136377
_diffrn_orient_matrix_UB_33        0.0108719623
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed X-ray tube'
_diffrn_source_target              Mo
_diffrn_source_type                'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  110
_reflns_number_total               117
_reflns_odcompleteness_completeness  98.06
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       26.32
_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.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max           0.697
_refine_diff_density_min           -0.792
_refine_diff_density_rms           0.255
_refine_ls_extinction_coef         0.0272(12)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref     1.167
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       13
_refine_ls_number_reflns           117
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0171
_refine_ls_R_factor_gt             0.0165
_refine_ls_restrained_S_all        1.167
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0115P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0345
_refine_ls_wR_factor_ref           0.0351
_refine_special_details            ?
_olex2_refinement_description
;
1. Shared sites
{Sb1, Sn1}
2. Uiso/Uaniso restraints and constraints
Uanis(Sb1) = Uanis(Sn1)
3. Others
 Fixed Sof: Sn1(0.075) Sb1(0.00833)
;
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary       ?
_atom_sites_solution_secondary     ?
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
 Sn2 Sn 1.0000 1.0000 0.5000 0.0107(3) Uani 1 12 d S T P A .
 Sn1 Sn 0.6667 0.3333 0.3333 0.0107(3) Uani 0.9 12 d S T P A 1
 Co1 Co 0.5000 0.5000 0.5000 0.0096(3) Uani 1 4 d S T P . .
 S1 S 0.3333 0.6667 0.38385(17) 0.0089(4) Uani 1 6 d S T P A .
 Sb1 Sb 0.6667 0.3333 0.3333 0.0107(3) Uani 0.1 12 d S T P A 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
 Sn2 Co1 2.6829(2) 1_665 ?
 Sn2 Co1 2.6829(2) 3_665 ?
 Sn2 Co1 2.6829(2) 2_765 ?
 Sn2 Co1 2.6829(2) . ?
 Sn2 Co1 2.68290(19) 3_675 ?
 Sn2 Co1 2.6829(2) 2_665 ?
 Sn2 S1 2.853(2) 7 ?
 Sn2 S1 2.853(2) 31_665 ?
 Sn1 Co1 2.6822(2) 15_554 ?
 Sn1 Co1 2.6822(2) . ?
 Sn1 Co1 2.6822(2) 2_655 ?
 Sn1 Co1 2.6822(2) 14_654 ?
 Sn1 Co1 2.6822(2) 3_665 ?
 Sn1 Co1 2.6822(2) 13_544 ?
 Co1 Sn2 2.6829(2) 1_445 ?
 Co1 Sn1 2.6822(2) 7_455 ?
 Co1 Co1 2.6829(2) 3_565 ?
 Co1 Co1 2.6829(2) 2_665 ?
 Co1 Co1 2.68290(19) 2_655 ?
 Co1 Co1 2.6829(2) 3_665 ?
 Co1 S1 2.1744(15) 19_666 ?
 Co1 S1 2.1744(15) . ?
 Co1 Sb1 2.6822(2) 7_455 ?
 Co1 Sb1 2.6822(2) . ?
 S1 Sn2 2.853(2) 13_444 ?
 S1 Co1 2.1744(15) 2_665 ?
 S1 Co1 2.1744(15) 3_565 ?
 Sb1 Co1 2.6822(2) 13_544 ?
 Sb1 Co1 2.6822(2) 2_655 ?
 Sb1 Co1 2.6822(2) 3_665 ?
 Sb1 Co1 2.6822(2) 15_554 ?
 Sb1 Co1 2.6822(2) 14_654 ?

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
 Co1 Sn2 Co1 180.0 1_665 . ?
 Co1 Sn2 Co1 120.0 3_675 2_765 ?
 Co1 Sn2 Co1 120.0 2_665 3_665 ?
 Co1 Sn2 Co1 60.0 1_665 3_675 ?
 Co1 Sn2 Co1 120.0 1_665 3_665 ?
 Co1 Sn2 Co1 120.0 . 3_675 ?
 Co1 Sn2 Co1 120.0 . 2_765 ?
 Co1 Sn2 Co1 120.0 1_665 2_665 ?
 Co1 Sn2 Co1 180.0 2_665 2_765 ?
 Co1 Sn2 Co1 60.0 . 2_665 ?
 Co1 Sn2 Co1 60.0 . 3_665 ?
 Co1 Sn2 Co1 60.0 3_675 2_665 ?
 Co1 Sn2 Co1 60.0 2_765 3_665 ?
 Co1 Sn2 Co1 60.0 1_665 2_765 ?
 Co1 Sn2 Co1 180.0 3_675 3_665 ?
 Co1 Sn2 S1 90.0 1_665 31_665 ?
 Co1 Sn2 S1 90.0 2_665 7 ?
 Co1 Sn2 S1 90.0 . 7 ?
 Co1 Sn2 S1 90.0 . 31_665 ?
 Co1 Sn2 S1 90.0 3_665 7 ?
 Co1 Sn2 S1 90.0 3_675 31_665 ?
 Co1 Sn2 S1 90.0 3_675 7 ?
 Co1 Sn2 S1 90.0 2_665 31_665 ?
 Co1 Sn2 S1 90.0 2_765 7 ?
 Co1 Sn2 S1 90.0 2_765 31_665 ?
 Co1 Sn2 S1 90.0 1_665 7 ?
 Co1 Sn2 S1 90.0 3_665 31_665 ?
 S1 Sn2 S1 180.0 31_665 7 ?
 Co1 Sn1 Co1 180.0 14_654 2_655 ?
 Co1 Sn1 Co1 119.983(7) 14_654 . ?
 Co1 Sn1 Co1 60.017(6) 13_544 15_554 ?
 Co1 Sn1 Co1 180.0 13_544 . ?
 Co1 Sn1 Co1 60.017(7) 13_544 14_654 ?
 Co1 Sn1 Co1 60.018(6) 2_655 . ?
 Co1 Sn1 Co1 60.017(6) 15_554 14_654 ?
 Co1 Sn1 Co1 60.018(6) 3_665 2_655 ?
 Co1 Sn1 Co1 180.0 15_554 3_665 ?
 Co1 Sn1 Co1 119.983(7) 15_554 . ?
 Co1 Sn1 Co1 119.983(6) 14_654 3_665 ?
 Co1 Sn1 Co1 60.018(6) 3_665 . ?
 Co1 Sn1 Co1 119.982(6) 13_544 2_655 ?
 Co1 Sn1 Co1 119.983(6) 15_554 2_655 ?
 Co1 Sn1 Co1 119.982(6) 13_544 3_665 ?
 Sn2 Co1 Sn2 180.0 . 1_445 ?
 Sn2 Co1 Co1 60.0 1_445 3_565 ?
 Sn2 Co1 Co1 120.0 1_445 3_665 ?
 Sn2 Co1 Co1 120.0 . 2_655 ?
 Sn2 Co1 Co1 60.0 . 3_665 ?
 Sn2 Co1 Co1 120.0 1_445 2_665 ?
 Sn2 Co1 Co1 60.0 . 2_665 ?
 Sn2 Co1 Co1 120.0 . 3_565 ?
 Sn2 Co1 Co1 60.0 1_445 2_655 ?
 Sn1 Co1 Sn2 90.0 7_455 . ?
 Sn1 Co1 Sn2 90.0 7_455 1_445 ?
 Sn1 Co1 Sn2 90.0 . . ?
 Sn1 Co1 Sn2 90.0 . 1_445 ?
 Sn1 Co1 Sn1 180.0 7_455 . ?
 Sn1 Co1 Co1 120.009(4) 7_455 2_655 ?
 Sn1 Co1 Co1 120.009(3) 7_455 3_665 ?
 Sn1 Co1 Co1 120.009(3) . 2_665 ?
 Sn1 Co1 Co1 59.991(4) . 2_655 ?
 Sn1 Co1 Co1 59.991(4) 7_455 2_665 ?
 Sn1 Co1 Co1 59.991(3) 7_455 3_565 ?
 Sn1 Co1 Co1 120.009(4) . 3_565 ?
 Sn1 Co1 Co1 59.991(4) . 3_665 ?
 Co1 Co1 Co1 180.0 3_565 3_665 ?
 Co1 Co1 Co1 60.0 2_655 3_665 ?
 Co1 Co1 Co1 180.0 2_655 2_665 ?
 Co1 Co1 Co1 120.0 2_655 3_565 ?
 Co1 Co1 Co1 60.0 3_565 2_665 ?
 Co1 Co1 Co1 120.0 3_665 2_665 ?
 S1 Co1 Sn2 90.0 19_666 . ?
 S1 Co1 Sn2 90.0 . . ?
 S1 Co1 Sn2 90.0 . 1_445 ?
 S1 Co1 Sn2 90.0 19_666 1_445 ?
 S1 Co1 Sn1 99.30(4) 19_666 . ?
 S1 Co1 Sn1 80.70(4) . . ?
 S1 Co1 Sn1 80.70(4) 19_666 7_455 ?
 S1 Co1 Sn1 99.30(4) . 7_455 ?
 S1 Co1 Co1 128.09(3) . 3_665 ?
 S1 Co1 Co1 128.09(3) . 2_655 ?
 S1 Co1 Co1 51.91(3) 19_666 2_655 ?
 S1 Co1 Co1 128.09(3) 19_666 3_565 ?
 S1 Co1 Co1 51.91(3) . 3_565 ?
 S1 Co1 Co1 128.09(3) 19_666 2_665 ?
 S1 Co1 Co1 51.91(3) . 2_665 ?
 S1 Co1 Co1 51.91(3) 19_666 3_665 ?
 S1 Co1 S1 180.0 . 19_666 ?
 S1 Co1 Sb1 80.70(4) 19_666 7_455 ?
 S1 Co1 Sb1 99.30(4) . 7_455 ?
 S1 Co1 Sb1 99.30(4) 19_666 . ?
 S1 Co1 Sb1 80.70(4) . . ?
 Sb1 Co1 Sn2 90.0 . . ?
 Sb1 Co1 Sn2 90.0 7_455 . ?
 Sb1 Co1 Sn2 90.0 7_455 1_445 ?
 Sb1 Co1 Sn2 90.0 . 1_445 ?
 Sb1 Co1 Co1 59.991(4) . 3_665 ?
 Sb1 Co1 Co1 59.991(4) . 2_655 ?
 Sb1 Co1 Co1 59.991(3) 7_455 3_565 ?
 Sb1 Co1 Co1 120.009(4) . 3_565 ?
 Sb1 Co1 Co1 120.009(3) 7_455 3_665 ?
 Sb1 Co1 Co1 59.991(4) 7_455 2_665 ?
 Sb1 Co1 Co1 120.009(4) 7_455 2_655 ?
 Sb1 Co1 Co1 120.009(3) . 2_665 ?
 Sb1 Co1 Sb1 180.0 7_455 . ?
 Co1 S1 Sn2 134.57(4) . 13_444 ?
 Co1 S1 Sn2 134.57(4) 3_565 13_444 ?
 Co1 S1 Sn2 134.57(4) 2_665 13_444 ?
 Co1 S1 Co1 76.18(6) 2_665 3_565 ?
 Co1 S1 Co1 76.18(6) 2_665 . ?
 Co1 S1 Co1 76.18(6) 3_565 . ?
 Co1 Sb1 Co1 60.017(6) 13_544 15_554 ?
 Co1 Sb1 Co1 60.018(6) 2_655 . ?
 Co1 Sb1 Co1 60.018(6) 3_665 2_655 ?
 Co1 Sb1 Co1 119.983(7) 15_554 . ?
 Co1 Sb1 Co1 119.983(6) 15_554 2_655 ?
 Co1 Sb1 Co1 119.982(6) 13_544 2_655 ?
 Co1 Sb1 Co1 60.018(6) 3_665 . ?
 Co1 Sb1 Co1 180.0 14_654 2_655 ?
 Co1 Sb1 Co1 60.017(6) 15_554 14_654 ?
 Co1 Sb1 Co1 180.0 13_544 . ?
 Co1 Sb1 Co1 119.982(6) 13_544 3_665 ?
 Co1 Sb1 Co1 119.983(7) 14_654 . ?
 Co1 Sb1 Co1 180.0 15_554 3_665 ?
 Co1 Sb1 Co1 60.017(7) 13_544 14_654 ?
 Co1 Sb1 Co1 119.983(6) 14_654 3_665 ?

_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  4.518
_oxdiff_exptl_absorpt_empirical_full_min  0.327
