Synthesis and Characterization of A3Na10Sn23 (A = Cs, Rb, K) with a New Clathrate-Like Structure and of the Chiral Clathrate Rb5Na3Sn25
Svilen Bobev; Slavi C. Sevov; Inorganic Chemistry 39 (2000) 5930–5937; doi:10.1021/ic0007714

data_4321706
_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
;
 Synthesis and Characterization of A3Na10Sn23 (A = Cs, Rb, K) with a New
 Clathrate-Like Structure and of the Chiral Clathrate Rb5Na3Sn25
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5930
_journal_page_last               5937
_journal_paper_doi               10.1021/ic0007714
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         K21.30Na56.70Sn138
_chemical_formula_sum            'K21.3 Na56.7 Sn138'
_chemical_formula_weight         18515.58
_chemical_melting_point          ?
_chemical_name_common            K21.30Na56.70Sn138
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :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            1
_cell_length_a                   12.456(2)
_cell_length_b                   12.456(2)
_cell_length_c                   50.559(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.317
_cell_measurement_theta_min      13.097
_cell_volume                     6793.4(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.1070
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            4360
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.05
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.837
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'average of two psi-scan reflections'
_exptl_crystal_colour            'gray, metallic luster'
_exptl_crystal_density_diffrn    4.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             7928
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         7.049
_refine_diff_density_min         -3.311
_refine_diff_density_rms         0.480
_refine_ls_extinction_coef       0.000000(8)
_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   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2493
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          1.427
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                1492
_reflns_number_total             2493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0007714_3.cif
_cod_data_source_block           K21.30Na56.70Sn138
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6793.9(9)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'K21.30 Na56.70 Sn138'
_cod_database_code               4321706