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_4316488
_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_moiety         'Cu7 Sn4 S12, 3(C2 H9 N2)'
_chemical_formula_sum            'C6 H27 Cu7 N6 S12 Sn4'
_chemical_formula_weight         1487.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_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                   13.5317(19)
_cell_length_b                   13.5317(19)
_cell_length_c                   28.933(6)
_cell_measurement_reflns_used    17299
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      6.43
_cell_measurement_theta_min      34.99
_cell_volume                     4588.1(13)
_computing_cell_refinement       'Bruker AXS Collect'
_computing_data_collection       'Bruker AXS Collect'
_computing_data_reduction        'Bruker AXS Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'omega scan'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            15872
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         6.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.800
_exptl_absorpt_correction_T_max  0.6562
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         2222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+96.2338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                1901
_reflns_number_total             2222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100688z_si_002_2.cif
_cod_data_source_block           r-3c
_cod_original_cell_volume        4588.0(13)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4316488