Simple Approach for Selective Crystal Growth of Intermetallic Clathrates
Stefanoski, Stevce; Beekman, Matt; Wong-Ng, Winnie; Zavalij, Peter; Nolas, George S.; Chemistry of Materials 23 (2011) 1491–; doi:10.1021/cm103135k

data_4000729
_publ_section_title
;
 Simple Approach for Selective Crystal Growth of Intermetallic Clathrates
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1491
_journal_paper_doi               10.1021/cm103135k
_journal_volume                  23
_journal_year                    2011
_chemical_formula_moiety         'Si17, Na3'
_chemical_formula_sum            'Na3 Si17'
_chemical_formula_weight         546.50
_chemical_name_common            'Sodium Silicide'
_chemical_name_systematic
;
Sodium Silicide
;
_space_group_IT_number           227
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_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
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_cell_angle_gamma                90.00
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_cell_length_b                   14.7121(1)
_cell_length_c                   14.7121(1)
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_cell_measurement_temperature    200(2)
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_cell_measurement_theta_min      2.4
_cell_volume                     3184.37(4)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
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_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      610,610,610,1200
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
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_diffrn_orient_matrix_UB_11      0.0501099
_diffrn_orient_matrix_UB_12      0.0022089
_diffrn_orient_matrix_UB_13      0.0458741
_diffrn_orient_matrix_UB_21      -0.0088702
_diffrn_orient_matrix_UB_22      0.0670798
_diffrn_orient_matrix_UB_23      0.0064657
_diffrn_orient_matrix_UB_31      -0.0450580
_diffrn_orient_matrix_UB_32      -0.0107528
_diffrn_orient_matrix_UB_33      0.0497401
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0040
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12553
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.40
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_id                'NIST/Winnie 2.SS74 200K'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.122
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0116
_refine_ls_R_factor_gt           0.0115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+12.P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0290
_refine_ls_wR_factor_ref         0.0290
_reflns_number_gt                260
_reflns_number_total             262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm103135k_si_003.cif
_cod_data_source_block           1791__Na24Si136
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

 Adding full bibliography for 4000728--4000729.cif.
;
_cod_original_sg_symbol_H-M      Fd-3m
_cod_database_code               4000729
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 3030
_diffrn_measurement_frame_time-ccd 12
_diffrn_measurement_total_time-ccd 15.00
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512