Sn3S4: a new mixed-valence tin sulfide
Gajda, Roman; Podsiadło, Sławomir; Jastrzębski, Cezariusz; Dłużewski, Piotr; Woźniak, Krzysztof; CrystEngComm 26 (2024) 6553–6561; doi:10.1039/D4CE00629A

data_7249450
_publ_section_title
;
 Sn3S4: a new mixed-valence tin sulfide
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              6553
_journal_page_last               6561
_journal_paper_doi               10.1039/D4CE00629A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_sum            'S4 Sn3'
_chemical_formula_weight         484.31
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-16
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2018-02-23 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.50180(6)
_cell_length_b                   10.50180(6)
_cell_length_c                   10.50180(6)
_cell_measurement_reflns_used    16436
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      44.2760
_cell_measurement_theta_min      2.6350
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_measurement_details
;
  1 omega -118.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249 -160.0000  -60.0000 69

  2 omega -118.00  -49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249 -160.0000   30.0000 69

  3 omega -113.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249   19.0000  150.0000 179

  4 omega  -71.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249   38.0000  -60.0000 131

  5 omega -102.00   18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249  -57.0000  150.0000 120

  6 omega -112.00   22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.9249  -77.0000   30.0000 134

  7 omega  -18.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9249   57.0000  -60.0000 120

  8 omega   21.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9249 -160.0000   90.0000 95

  9 omega   21.00  154.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   76.0000  129.5881 133

 10 omega   20.00  154.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000 -120.0000 134

 11 omega   79.00  153.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  111.0000 -180.0000 74

 12 omega   19.00  146.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   50.0000   60.0000 127

 13 omega   19.00   46.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   80.0000  157.2538 27

 14 omega   20.00  154.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000    0.0000 134

 15 omega   87.00  153.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  111.0000   90.0000 66

 16 omega   17.00   75.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  -50.0000  150.0000 58

 17 omega   59.00  137.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -30.0000 78

 18 omega   18.00   43.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   81.0000   56.7121 25

 19 omega   20.00   45.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -60.0000 25

 20 omega   21.00   47.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -90.0000 26

 21 omega   22.00   48.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -30.0000 26

 22 omega   63.00  157.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  160.0000  120.0000 94

 23 omega   20.00  114.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000   90.0000 94

 24 omega   20.00   46.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000   30.0000 26

 25 omega   94.00  154.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000   30.0000 60

 26 omega  101.00  153.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  111.0000   60.0000 52

 27 omega   74.00  143.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  160.0000 -150.0000 69

 28 omega  -23.00  119.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478  -92.0000  150.0000 142

 29 omega   20.00  151.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000 -150.0000 131

 30 omega   41.00  145.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   64.0000 -180.0000 104

 31 omega   19.00   44.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   80.0000  -47.0570 25

 32 omega   60.00   99.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -90.0000 39

 33 omega   18.00   43.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   82.0000 -107.8784 25

 34 omega   58.00  147.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   77.0000  -60.0000 89

 35 omega   18.00   45.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       65.7478   81.0000  142.6908 27
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0326440000
_diffrn_orient_matrix_UB_12      -0.0353973000
_diffrn_orient_matrix_UB_13      0.0227733000
_diffrn_orient_matrix_UB_21      0.0153100000
_diffrn_orient_matrix_UB_22      0.0368242000
_diffrn_orient_matrix_UB_23      0.0353101000
_diffrn_orient_matrix_UB_31      -0.0392128000
_diffrn_orient_matrix_UB_32      -0.0150757000
_diffrn_orient_matrix_UB_33      0.0327567000
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0059
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7568
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.664
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_diffrn_reflns_theta_min         2.651
_diffrn_source                   'Enhance (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    7.431
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.555
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1712
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_exptl_crystal_size_mid          0.1017
_exptl_crystal_size_min          0.0608
_refine_diff_density_max         1.584
_refine_diff_density_min         -2.460
_refine_diff_density_rms         0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0265
_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/[\s^2^(Fo^2^)+(0.0470P)^2^+52.0902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                109
_reflns_number_total             109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00629a1.cif
_cod_data_source_block           Sn3S4
_cod_depositor_comments          'Adding full bibliography for 7249450.cif.'
_cod_original_cell_volume        1158.22(2)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               7249450
_shelxl_version_number           2013-3
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.55
_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.
;
_shelx_res_checksum              51510
_shelx_hkl_checksum              13092