Synthesis and Structural Characterization of NaxSi136 (0 < x <= 24) Single Crystals and Low-Temperature Transport of Polycrystalline Specimens
Stevce Stefanoski; Christos D. Malliakas; Mercouri G. Kanatzidis; George S. Nolas; Inorganic Chemistry 51 (2012) 8686–8692; doi:10.1021/ic202199t

data_4329988
_publ_section_title
;
 Synthesis and Structural Characterization of NaxSi136 (0 < x <= 24)
 Single Crystals and Low-Temperature Transport of Polycrystalline
 Specimens
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8686
_journal_page_last               8692
_journal_paper_doi               10.1021/ic202199t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Si136, Na5.1'
_chemical_formula_sum            'Na5.1 Si136'
_chemical_formula_weight         3937.49
_chemical_name_common            'Sodium Silicide'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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                   14.6437(7)
_cell_length_b                   14.6437(7)
_cell_length_c                   14.6437(7)
_cell_measurement_reflns_used    18628
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      38.15
_cell_measurement_theta_min      4.62
_cell_volume                     3140.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0062
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10991
_diffrn_reflns_theta_full        34.91
_diffrn_reflns_theta_max         34.91
_diffrn_reflns_theta_min         3.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.7610
_exptl_absorpt_correction_T_min  0.7315
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape2
_exptl_crystal_colour            'dark gray'
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_description       cuboctahedral
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.496
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.496
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0076P)^2^+18.1759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                364
_reflns_number_total             370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202199t_si_002.cif
_cod_data_source_block           na5.1si136
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'Na5.10 Si136'
_cod_database_code               4329988