Pressure Effects on the Size of Type-I and Type-II Si-Clathrates Synthesized by Spark Plasma Sintering
Stefanoski, S.; Blosser, M. C.; Nolas, G. S.; Crystal Growth & Design 13 (2013) 195–; doi:10.1021/cg3013443

data_4507227
_publ_section_title
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 Pressure Effects on the Size of Type-I and Type-II Si-Clathrates
 Synthesized by Spark Plasma Sintering
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_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              195
_journal_paper_doi               10.1021/cg3013443
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'Na24 Si136'
_chemical_formula_weight         4372.00
_chemical_name_systematic
;
 ?
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_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   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            1
_cell_length_a                   14.71560(10)
_cell_length_b                   14.71560(10)
_cell_length_c                   14.71560(10)
_cell_measurement_reflns_used    16108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.08
_cell_measurement_theta_min      4.62
_cell_volume                     3186.65(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 180 frames, detector distance = 40 mm'
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5934
_diffrn_reflns_theta_full        38.04
_diffrn_reflns_theta_max         38.04
_diffrn_reflns_theta_min         4.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.6637
_exptl_absorpt_correction_T_min  0.5748
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape2
_exptl_crystal_colour            'dark gray'
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboctahedral
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.577
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.577
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0000P)^2^+48.1954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                440
_reflns_number_total             460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3013443_si_004.cif
_cod_data_source_block           shelxs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Fd-3m
_cod_database_code               4507227