Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi + NaAlSi.
Dong, Yongkwan; Chai, Ping; Beekman, Matt; Zeng, Xiaoyu; Tritt, Terry M.; Nolas, George S.; Inorganic chemistry 54 (2015) 5316–5321; doi:10.1021/acs.inorgchem.5b00348

data_4343034
_publ_section_title
;
 Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and
 Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi +
 NaAlSi.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5316
_journal_page_last               5321
_journal_paper_doi               10.1021/acs.inorgchem.5b00348
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Al8 Na8 Si38'
_chemical_formula_weight         1467.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           223
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_atom_sites_solution_hydrogens   none
_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            1
_cell_length_a                   10.31700(10)
_cell_length_b                   10.31700(10)
_cell_length_c                   10.31700(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1098.147(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0108
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6231
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         72.00
_diffrn_reflns_theta_min         6.07
_exptl_absorpt_coefficient_mu    12.725
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.5112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0339
_refine_ls_wR_factor_ref         0.0348
_reflns_number_gt                201
_reflns_number_total             220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00348_si_001.cif
_cod_data_source_block           ping_na8al8si38
_cod_depositor_comments          'Adding full bibliography for 4343034.cif.'
_cod_database_code               4343034