Revisiting [(RSn(IV))6Sn(III)2S12]: Directed Synthesis, Crystal Transformation, and Luminescence Properties.
Eußner, Jens P; Barth, Beatrix E. K.; Justus, Uwe; Rosemann, Nils W.; Chatterjee, Sangam; Dehnen, Stefanie; Inorganic chemistry 54 (2015) 22–24; doi:10.1021/ic502627h

data_4341968
_publ_section_title
;
 Revisiting [(RSn(IV))6Sn(III)2S12]: Directed Synthesis, Crystal
 Transformation, and Luminescence Properties.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              22
_journal_page_last               24
_journal_paper_doi               10.1021/ic502627h
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C36 H66 O6 S12 Sn8'
_chemical_formula_sum            'C36 H66 O6 S12 Sn8'
_chemical_formula_weight         1929.13
_chemical_melting_point          '125&#x00B0;C (decomp.)'
_chemical_name_systematic
;
dodecakis(\m~2~-sulfido)-hexakis(4-methylpentan-2-one-C,O)-di-tin(iii)-hexa-
tin(iv) dichloromethane hydrogen sulfide solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.372(3)
_cell_length_b                   24.291(2)
_cell_length_c                   24.673(2)
_cell_measurement_temperature    250(2)
_cell_volume                     14008(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_sigmaI/netI    0.1790
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12256
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7376
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_size_rad          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.723
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         12256
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                5108
_reflns_number_total             12256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502627h_si_002.cif
_cod_data_source_block           jepw003
_cod_depositor_comments          'Adding full bibliography for 4341968.cif.'
_cod_database_code               4341968
_exptl_absorpt_correction_t_ave  0.424