Crystal Growth Conditions of Types I and II Na‒Si Clathrates by Evaporation of Na from a Na‒Si‒Sn Solution
Morito, Haruhiko; Shimoda, Masashi; Yamane, Hisanori; Fujiwara, Kozo; Crystal Growth & Design 18 (2017) 351–; doi:10.1021/acs.cgd.7b01342

data_4514317
_publ_section_title
;
 Crystal Growth Conditions of Types I and II Na--Si Clathrates by
 Evaporation of Na from a Na--Si--Sn Solution
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              351
_journal_paper_doi               10.1021/acs.cgd.7b01342
_journal_volume                  18
_journal_year                    2017
_chemical_formula_moiety         'Na24 Si136'
_chemical_formula_sum            'Na24 Si136'
_chemical_formula_weight         4372.00
_chemical_name_common            'Type II silicon clathrate'
_chemical_name_systematic        '24 sodium 136 silicon'
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   14.7088(3)
_cell_length_b                   14.7088(3)
_cell_length_c                   14.7088(3)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    301.(2)
_cell_measurement_theta_max      36.2846
_cell_measurement_theta_min      2.3983
_cell_volume                     3182.23(11)
_computing_cell_refinement       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_collection       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_reduction        'APEX3 v2015.9-0 (Bruker AXS)'
_computing_molecular_graphics    'VESTA v3.3.2 (Momma & Izumi, 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      301(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Burker, D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0047
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46945
_diffrn_reflns_theta_full        31.96
_diffrn_reflns_theta_max         31.96
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'micro focus sealed tube'
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.206
_refine_ls_extinction_coef       0.00039(8)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0082
_refine_ls_R_factor_gt           0.0077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.9257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0268
_refine_ls_wR_factor_ref         0.0279
_reflns_number_gt                291
_reflns_number_total             300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg7b01342_si_002.cif
_cod_data_source_block           TypeII_0m_a
_cod_depositor_comments          'Adding full bibliography for 4514317.cif.'
_cod_original_cell_volume        3182.23(19)
_cod_database_code               4514317
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              22833
_shelx_hkl_checksum              51806