New Three-Dimensional Thiostannates Composed of Linked Cu8S12 Clusters and the First Example of a Mixed-Metal Cu7SnS12 Cluster
Malte Behrens; Marie-Eve Ordolff; Christian Näther; Wolfgang Bensch; Klaus-Dieter Becker; Catherine Guillot-Deudon; Alain Lafond; Jason A. Cody; Inorganic Chemistry 49 (2010) 8305–8309; doi:10.1021/ic100688z

data_4316489
_publ_section_title
;
 New Three-Dimensional Thiostannates Composed of Linked Cu8S12 Clusters
 and the First Example of a Mixed-Metal Cu7SnS12 Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8305
_journal_page_last               8309
_journal_paper_doi               10.1021/ic100688z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C6 H21 Cu7 N4 S12 Sn4'
_chemical_formula_weight         1453.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.1059(6)
_cell_length_b                   13.1059(6)
_cell_length_c                   29.3468(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      16.5
_cell_volume                     4365.4(4)
_computing_cell_refinement       'STOE IPDS-1 program package'
_computing_data_collection       'STOE IPDS-1 program package'
_computing_data_reduction        'STOE IPDS-1 program package'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scans'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            13151
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.242
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE & CIE)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.200
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.262
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_coef       0.00033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2360
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+160.3965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                2263
_reflns_number_total             2360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100688z_si_002_3.cif
_cod_data_source_block           mb189
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4316489