Ordering of Vacancies in Type-I Tin Clathrate: Superstructure of Rb8Sn44 2
Franck Dubois; Thomas F. Fässler; Journal of the American Chemical Society 127 (2005) 3264–3265; doi:10.1021/ja043500r

data_4111518
_publ_contact_author_address
;Department Chemie
Technische Universit\"at M\"unchen
 Lichtenbergstrasse 4
 85747 Garching, Germany
;
_publ_contact_author_email       Thomas.Faessler@lrz.tum.de
_publ_contact_author_fax         '+49-(0) 89 28913134'
_publ_contact_author_name        'Thomas F. F\"assler'
_publ_contact_author_phone       '+49-(0) 89 28913186'
_publ_section_title
;
 Ordering of Vacancies in Type-I Tin Clathrate: Superstructure of Rb8Sn44
 2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3264
_journal_page_last               3265
_journal_paper_doi               10.1021/ja043500r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'Rb2 Sn11'
_chemical_formula_weight         4849.68
_space_group_IT_number           230
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      230
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_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            32
_cell_length_a                   24.1162(3)
_cell_length_b                   24.1162(3)
_cell_length_c                   24.1162(3)
_cell_measurement_temperature    293(2)
_cell_volume                     14025.8(3)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'KappaCCD control sofware (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS FR 591 rotating anode'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1713
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            138238
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    20.855
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Platon Delabs
(see: Walker, N.& Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'black-metallic luster'
_exptl_crystal_density_diffrn    5.594
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             19968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.019
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.402
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+149.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                906
_reflns_number_total             1076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043500rsi20041027_113125.cif
_cod_data_source_block           Rb8Sn44
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_sg_symbol_H-M      'I a 3 d'
_cod_database_code               4111518