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_4115474
_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         'Cs1.72 Na0.35 Rb2.03 Sn20.31'
_chemical_formula_sum            'Cs1.72 Na0.35 Rb2.03 Sn20.31'
_chemical_formula_weight         2820.22
_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                   23.490(1)
_cell_length_b                   23.490(1)
_cell_length_c                   12.087(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.99
_cell_measurement_theta_min      13.09
_cell_volume                     6669.4(7)
_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  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6171
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    19.687
_exptl_absorpt_correction_T_max  0.3846
_exptl_absorpt_correction_T_min  0.2435
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'average of 4 psi-scan reflections'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.617
_exptl_crystal_description       bar
_exptl_crystal_F_000             9511
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.882
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.355
_refine_ls_extinction_coef       0.000030(2)
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                2087
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010010f_3.cif
_cod_data_source_block           Cs13.75Rb16.25Na2.79Sn162.45
_cod_database_code               4115474