#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:29:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179020 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/18/4121824.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4121824
loop_
_publ_author_name
'Yamanaka, Shoji'
'Komatsu, Masaya'
'Tanaka, Masashi'
'Sawa, Hiroshi'
'Inumaru, Kei'
_publ_section_title
;
 High-Pressure Synthesis and Structural Characterization of the Type II
 Clathrate Compound Na30.5Si136 Encapsulating Two Sodium Atoms in the Same
 Silicon Polyhedral Cages.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7717
_journal_page_last               7725
_journal_paper_doi               10.1021/ja502733e
_journal_volume                  136
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Na4 Si23'
_chemical_formula_sum            'Na4 Si23'
_chemical_formula_weight         738.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      223
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2013-01-12T17:49:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2004(4)
_cell_length_b                   10.2004(4)
_cell_length_c                   10.2004(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1061.33(7)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 'not relevant'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigakau CCD Mercury'
_diffrn_measurement_method       'phi and kai scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7256
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         4
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Rigaku CrystalClear'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0521P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                209
_reflns_number_total             243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja502733e_si_007.cif
_cod_data_source_block           Na8Si46
_cod_depositor_comments
'Adding full bibliography for 4121822--4121827.cif.'
_cod_database_code               4121824
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'x+1/2, z+1/2, -y+1/2'
'-z+1/2, y+1/2, x+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, z+1/2, y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-z, -x, -y'
'-y, -z, -x'
'z, x, -y'
'y, -z, x'
'-z, x, y'
'y, z, -x'
'z, -x, y'
'-y, z, x'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'x-1/2, z-1/2, y-1/2'
'z-1/2, y-1/2, x-1/2'
'-x-1/2, -z-1/2, y-1/2'
'z-1/2, -y-1/2, -x-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'x-1/2, -z-1/2, -y-1/2'
'-z-1/2, y-1/2, -x-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.18412(5) 0.18412(5) 0.18412(5) 0.0128(3) Uani 1 3 d S
Si2 Si 0 0.11719(7) 0.30776(7) 0.0134(3) Uani 1 2 d S
Si3 Si 0.25 0.5 0 0.0131(4) Uani 1 8 d S
Na4 Na 0 0 0 0.0243(10) Uani 1 24 d S
Na5 Na 0.25 0 0.5 0.0461(9) Uani 1 8 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Si1 Si1 Si2 108.51(3) 13 .
Si1 Si1 Si2 108.51(3) 13 6
Si2 Si1 Si2 110.41(3) . 6
Si1 Si1 Si2 108.51(3) 13 5
Si2 Si1 Si2 110.41(3) . 5
Si2 Si1 Si2 110.41(3) 6 5
Si1 Si1 Na4 180.00(7) 13 .
Si2 Si1 Na4 71.49(3) . .
Si2 Si1 Na4 71.49(3) 6 .
Si2 Si1 Na4 71.49(3) 5 .
Si1 Si2 Si1 105.27(4) 27 .
Si1 Si2 Si3 105.96(3) 27 5
Si1 Si2 Si3 105.96(3) . 5
Si1 Si2 Si2 106.79(2) 27 2
Si1 Si2 Si2 106.79(2) . 2
Si3 Si2 Si2 124.638(18) 5 2
Si1 Si2 Na4 66.67(3) 27 .
Si1 Si2 Na4 66.67(3) . .
Si3 Si2 Na4 166.21(3) 5 .
Si2 Si2 Na4 69.154(13) 2 .
Si1 Si2 Na5 175.00(3) 27 .
Si1 Si2 Na5 79.340(13) . .
Si3 Si2 Na5 74.208(15) 5 .
Si2 Si2 Na5 69.615(12) 2 .
Na4 Si2 Na5 114.208(15) . .
Si1 Si2 Na5 79.340(13) 27 25_556
Si1 Si2 Na5 175.00(3) . 25_556
Si3 Si2 Na5 74.208(15) 5 25_556
Si2 Si2 Na5 69.615(12) 2 25_556
Na4 Si2 Na5 114.208(15) . 25_556
Na5 Si2 Na5 95.988(19) . 25_556
Si2 Si3 Si2 108.849(18) 13 6
Si2 Si3 Si2 110.72(4) 13 38_665
Si2 Si3 Si2 108.849(18) 6 38_665
Si2 Si3 Si2 108.849(18) 13 32_565
Si2 Si3 Si2 110.72(4) 6 32_565
Si2 Si3 Si2 108.849(18) 38_665 32_565
Si1 Na4 Si1 180.00(3) 25 .
Si1 Na4 Si1 109.5 25 28
Si1 Na4 Si1 70.5 . 28
Si1 Na4 Si1 70.5 25 4
Si1 Na4 Si1 109.5 . 4
Si1 Na4 Si1 180.000(15) 28 4
Si1 Na4 Si1 70.5 25 2
Si1 Na4 Si1 109.5 . 2
Si1 Na4 Si1 70.5 28 2
Si1 Na4 Si1 109.5 4 2
Si1 Na4 Si1 109.5 25 26
Si1 Na4 Si1 70.5 . 26
Si1 Na4 Si1 109.5 28 26
Si1 Na4 Si1 70.5 4 26
Si1 Na4 Si1 180.00(3) 2 26
Si1 Na4 Si1 70.5 25 3
Si1 Na4 Si1 109.5 . 3
Si1 Na4 Si1 70.5 28 3
Si1 Na4 Si1 109.5 4 3
Si1 Na4 Si1 109.5 2 3
Si1 Na4 Si1 70.5 26 3
Si1 Na4 Si1 109.5 25 27
Si1 Na4 Si1 70.5 . 27
Si1 Na4 Si1 109.5 28 27
Si1 Na4 Si1 70.5 4 27
Si1 Na4 Si1 70.5 2 27
Si1 Na4 Si1 109.5 26 27
Si1 Na4 Si1 180.00(3) 3 27
Si1 Na4 Si2 41.840(6) 25 25
Si1 Na4 Si2 138.160(6) . 25
Si1 Na4 Si2 109.518(10) 28 25
Si1 Na4 Si2 70.482(10) 4 25
Si1 Na4 Si2 109.518(10) 2 25
Si1 Na4 Si2 70.482(10) 26 25
Si1 Na4 Si2 41.840(6) 3 25
Si1 Na4 Si2 138.160(6) 27 25
Si1 Na4 Si2 41.840(6) 25 30
Si1 Na4 Si2 138.160(6) . 30
Si1 Na4 Si2 70.482(10) 28 30
Si1 Na4 Si2 109.518(10) 4 30
Si1 Na4 Si2 41.840(6) 2 30
Si1 Na4 Si2 138.160(6) 26 30
Si1 Na4 Si2 70.482(10) 3 30
Si1 Na4 Si2 109.518(10) 27 30
Si2 Na4 Si2 70.575(10) 25 30
Si1 Na4 Si2 41.840(6) 25 29
Si1 Na4 Si2 138.160(6) . 29
Si1 Na4 Si2 138.160(6) 28 29
Si1 Na4 Si2 41.840(6) 4 29
Si1 Na4 Si2 70.482(10) 2 29
Si1 Na4 Si2 109.518(10) 26 29
Si1 Na4 Si2 109.518(10) 3 29
Si1 Na4 Si2 70.482(10) 27 29
Si2 Na4 Si2 70.575(10) 25 29
Si2 Na4 Si2 70.575(10) 30 29
Si1 Na4 Si2 138.160(6) 25 6
Si1 Na4 Si2 41.840(6) . 6
Si1 Na4 Si2 109.518(10) 28 6
Si1 Na4 Si2 70.482(10) 4 6
Si1 Na4 Si2 138.160(6) 2 6
Si1 Na4 Si2 41.840(6) 26 6
Si1 Na4 Si2 109.518(10) 3 6
Si1 Na4 Si2 70.482(10) 27 6
Si2 Na4 Si2 109.425(10) 25 6
Si2 Na4 Si2 180 30 6
Si2 Na4 Si2 109.425(10) 29 6
Si2 Na5 Si2 161.85(2) 43_666 2
Si2 Na5 Si2 123.516(11) 43_666 .
Si2 Na5 Si2 40.77(2) 2 .
Si2 Na5 Si2 40.77(2) 43_666 17
Si2 Na5 Si2 123.516(11) 2 17
Si2 Na5 Si2 98.86(2) . 17
Si2 Na5 Si2 98.86(2) 43_666 26_556
Si2 Na5 Si2 84.012(19) 2 26_556
Si2 Na5 Si2 69.70(2) . 26_556
Si2 Na5 Si2 123.516(11) 17 26_556
Si2 Na5 Si2 123.516(11) 43_666 25_556
Si2 Na5 Si2 69.70(2) 2 25_556
Si2 Na5 Si2 84.012(19) . 25_556
Si2 Na5 Si2 161.85(2) 17 25_556
Si2 Na5 Si2 40.77(2) 26_556 25_556
Si2 Na5 Si2 69.70(2) 43_666 41_656
Si2 Na5 Si2 123.516(11) 2 41_656
Si2 Na5 Si2 161.85(2) . 41_656
Si2 Na5 Si2 84.012(19) 17 41_656
Si2 Na5 Si2 123.516(11) 26_556 41_656
Si2 Na5 Si2 98.86(2) 25_556 41_656
Si2 Na5 Si2 84.012(19) 43_666 19_545
Si2 Na5 Si2 98.86(2) 2 19_545
Si2 Na5 Si2 123.516(11) . 19_545
Si2 Na5 Si2 69.70(2) 17 19_545
Si2 Na5 Si2 161.85(2) 26_556 19_545
Si2 Na5 Si2 123.516(11) 25_556 19_545
Si2 Na5 Si2 40.77(2) 41_656 19_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Si1 2.3279(19) 13
Si1 Si2 2.3630(5) .
Si1 Si2 2.3630(5) 6
Si1 Si2 2.3630(5) 5
Si1 Na4 3.2529(9) .
Si2 Si1 2.3630(5) 27
Si2 Si3 2.3834(7) 5
Si2 Si2 2.3908(15) 2
Si2 Na4 3.3591(7) .
Si2 Na5 3.4318(5) .
Si2 Na5 3.4318(5) 25_556
Si3 Si2 2.3834(7) 13
Si3 Si2 2.3834(7) 6
Si3 Si2 2.3834(7) 38_665
Si3 Si2 2.3834(7) 32_565
Na4 Si1 3.2529(9) 25
Na4 Si1 3.2529(9) 28
Na4 Si1 3.2529(9) 4
Na4 Si1 3.2529(9) 2
Na4 Si1 3.2529(9) 26
Na4 Si1 3.2529(9) 3
Na4 Si1 3.2529(9) 27
Na4 Si2 3.3591(7) 25
Na4 Si2 3.3591(7) 30
Na4 Si2 3.3591(7) 29
Na4 Si2 3.3591(7) 6
Na5 Si2 3.4318(5) 43_666
Na5 Si2 3.4318(5) 2
Na5 Si2 3.4318(5) 17
Na5 Si2 3.4318(5) 26_556
Na5 Si2 3.4318(5) 25_556
Na5 Si2 3.4318(5) 41_656
Na5 Si2 3.4318(5) 19_545
