 
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Cu2 S4 Sn Zn' 
_chemical_formula_weight          439.38

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'S'  'S'   0.1246   0.1234
 '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'
 'Zn'  'Zn'   0.2839   1.4301
 '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'
 
_space_group_crystal_system       tetragonal
_space_group_IT_number            82
_space_group_name_H-M_alt         'I -4'
_space_group_name_Hall            'I -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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 'y, -x, -z'
 '-y, x, -z'
 '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'
 
_cell_length_a                    5.42820(10)
_cell_length_b                    5.42820(10)
_cell_length_c                    10.8198(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      318.809(19)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     1088
_cell_measurement_theta_min       4.1550
_cell_measurement_theta_max       31.7500
 
_exptl_crystal_description        "needle"
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.577          
_exptl_crystal_F_000              202
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     15.343
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'New Xcalibur, EosS2'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             3067
_diffrn_reflns_av_unetI/netI      0.0375
_diffrn_reflns_av_R_equivalents   0.0668
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.766
_diffrn_reflns_theta_max          31.949
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.966
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.966
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.942
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              519
_reflns_number_gt                 518
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.840
_reflns_Friedel_fraction_max      0.915
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0494P)²] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.050(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 229 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.89(5)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          519
_refine_ls_number_parameters      19
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0213
_refine_ls_R_factor_gt            0.0214
_refine_ls_wR_factor_ref          0.0624
_refine_ls_wR_factor_gt           0.0624
_refine_ls_goodness_of_fit_ref    1.038
_refine_ls_restrained_S_all       1.038
_refine_ls_shift/su_max           0.063
_refine_ls_shift/su_mean          0.027
 
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
Cu1 Cu 0.5000 0.0000 0.2500 0.0196(3) Uani 1 4 d S T P . .
Sn2 Sn 1.0000 0.5000 0.2500 0.0093(3) Uani 1 4 d S T P . .
Cu3 Cu 0.5000 0.5000 0.5000 0.0142(14) Uani 1 4 d S T P . .
Cu4 Cu 1.0000 0.0000 0.5000 0.0133(14) Uani 1 4 d S T P . .
S5 S 0.7435(4) 0.2436(4) 0.37792(10) 0.0098(4) Uani 1 1 d . . . . .
 
 
_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
Cu1 S5 2.3261(12) . ?
Cu1 S5 2.3262(12) 8_545 ?
Cu1 S5 2.3262(12) 2_655 ?
Cu1 S5 2.3262(12) 7 ?
Sn2 S5 2.4066(12) . ?
Sn2 S5 2.4067(12) 2_765 ?
Sn2 S5 2.4067(12) 8_645 ?
Sn2 S5 2.4067(12) 7_565 ?
Cu3 S5 2.330(2) 4_656 ?
Cu3 S5 2.330(2) 3_566 ?
Cu3 S5 2.330(2) 2_665 ?
Cu3 S5 2.330(2) . ?
Cu4 S5 2.331(2) 3_666 ?
Cu4 S5 2.331(2) 4_646 ?
Cu4 S5 2.331(2) 2_755 ?
Cu4 S5 2.331(2) . ?
 
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
S5 Cu1 S5 110.74(3) . 8_545 ?
S5 Cu1 S5 106.97(6) . 2_655 ?
S5 Cu1 S5 110.74(3) 8_545 2_655 ?
S5 Cu1 S5 110.74(3) . 7 ?
S5 Cu1 S5 106.97(6) 8_545 7 ?
S5 Cu1 S5 110.74(3) 2_655 7 ?
S5 Sn2 S5 109.78(5) . 2_765 ?
S5 Sn2 S5 109.32(3) . 8_645 ?
S5 Sn2 S5 109.32(3) 2_765 8_645 ?
S5 Sn2 S5 109.32(3) . 7_565 ?
S5 Sn2 S5 109.32(3) 2_765 7_565 ?
S5 Sn2 S5 109.78(5) 8_645 7_565 ?
S5 Cu3 S5 110.93(9) 4_656 3_566 ?
S5 Cu3 S5 108.75(4) 4_656 2_665 ?
S5 Cu3 S5 108.75(4) 3_566 2_665 ?
S5 Cu3 S5 108.75(4) 4_656 . ?
S5 Cu3 S5 108.75(4) 3_566 . ?
S5 Cu3 S5 110.93(9) 2_665 . ?
S5 Cu4 S5 110.96(9) 3_666 4_646 ?
S5 Cu4 S5 108.73(4) 3_666 2_755 ?
S5 Cu4 S5 108.73(4) 4_646 2_755 ?
S5 Cu4 S5 108.73(4) 3_666 . ?
S5 Cu4 S5 108.73(4) 4_646 . ?
S5 Cu4 S5 110.96(9) 2_755 . ?
Cu4 S5 Cu3 110.89(4) . . ?
Cu4 S5 Cu1 110.74(9) . . ?
Cu3 S5 Cu1 110.77(9) . . ?
Cu4 S5 Sn2 107.96(8) . . ?
Cu3 S5 Sn2 107.99(8) . . ?
Cu1 S5 Sn2 108.38(4) . . ?
 
_refine_diff_density_max    0.802
_refine_diff_density_min   -0.929
_refine_diff_density_rms    0.197



