Tin Clathrates with the Type II Structure
Marion C. Schäfer; Svilen Bobev; Journal of the American Chemical Society 135 (2013) 1696–1699; doi:10.1021/ja3112934

data_4119283
_publ_section_title
;
 Tin Clathrates with the Type II Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1696
_journal_page_last               1699
_journal_paper_doi               10.1021/ja3112934
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'Ba13.3 Ga36.4 Rb9.9 Sn99.6'
_chemical_formula_weight         17019.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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            1
_cell_length_a                   17.0367(5)
_cell_length_b                   17.0367(5)
_cell_length_c                   17.0367(5)
_cell_measurement_reflns_used    945
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      3.38
_cell_volume                     4944.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16396
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    22.145
_exptl_absorpt_correction_T_max  0.257
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Sheldrick, 2003) 
;
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    5.715
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7214
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.000031(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   1.190
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+63.4788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0403
_reflns_number_gt                307
_reflns_number_total             335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3112934_si_002_05.cif
_cod_data_source_block           V
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               4119283