Clathrate III of Group 14 Exists After All
Svilen Bobev; Slavi C. Sevov; Journal of the American Chemical Society 123 (2001) 3389–3390; doi:10.1021/ja010010f

data_4115472
_publ_contact_author
;
Slavi C. Sevov
Department of Chemistry and Biochemistry
251 Nieuwland Science Hall
University of Notre Dame
Notre Dame, IN 46556-5670
USA
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_fax         'Intl. Code + (219)631-6652'
_publ_contact_author_phone       'Intl. Code + (219)631-5891'
_publ_section_title
;
 Clathrate III of Group 14 Exists After All
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3389
_journal_page_last               3390
_journal_paper_doi               10.1021/ja010010f
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         Cs3.75Na0.31Sn20.33
_chemical_formula_sum            'Cs3.75 Na0.31 Sn20.33'
_chemical_formula_weight         2918.84
_chemical_name_common            clathrate-III
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_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                   23.5389(9)
_cell_length_b                   23.5389(9)
_cell_length_c                   12.1031(7)
_cell_measurement_reflns_used    8681
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.22
_cell_volume                     6706.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58707
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    18.843
_exptl_absorpt_correction_T_max  0.3977
_exptl_absorpt_correction_T_min  0.2108
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS semi-empirical absorption correction'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.782
_exptl_crystal_description       bar
_exptl_crystal_F_000             9810
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.299
_refine_diff_density_min         -3.163
_refine_diff_density_rms         0.403
_refine_ls_extinction_coef       0.0000066(17)
_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   1.304
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+421.2459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4213
_reflns_number_total             4462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010010f_1.cif
_cod_data_source_block           CCD
_cod_database_code               4115472