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_4115473
_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         Cs3.75Na0.36Sn20.29
_chemical_formula_sum            'Cs3.75 Na0.36 Sn20.29'
_chemical_formula_weight         2914.67
_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                   23.5566(9)
_cell_length_b                   23.5566(9)
_cell_length_c                   12.1040(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.66
_cell_measurement_theta_min      13.94
_cell_volume                     6716.7(6)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7865
_diffrn_reflns_theta_full        34.98
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         2.08
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    18.780
_exptl_absorpt_correction_T_max  0.3150
_exptl_absorpt_correction_T_min  0.2115
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'average of 5 psi-scan reflections'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.765
_exptl_crystal_description       bar
_exptl_crystal_F_000             9797
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.679
_refine_diff_density_min         -5.884
_refine_diff_density_rms         0.611
_refine_ls_extinction_coef       0.000003(1)
_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   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         7865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+724.7363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1611
_reflns_number_gt                6298
_reflns_number_total             7865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010010f_2.cif
_cod_data_source_block           CAD4
_cod_database_code               4115473