data_shelxs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_sum 'Na8 Si46' _chemical_formula_weight 1476.06 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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pm-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-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' '-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' '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, -y+1/2, -x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' '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' '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' '-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, y-1/2, x-1/2' _cell_length_a 10.1961(7) _cell_length_b 10.1961(7) _cell_length_c 10.1961(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1059.99(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 4.62 _cell_measurement_theta_max 38.08 _exptl_crystal_description prism _exptl_crystal_colour back _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5748 _exptl_absorpt_correction_T_max 0.6637 _exptl_absorpt_process_details 'X-Shape2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 948 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.90 _diffrn_reflns_theta_max 38.07 _reflns_number_total 547 _reflns_number_gt 429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 547 _refine_ls_number_parameters 16 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0358 _refine_ls_wR_factor_gt 0.0333 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.11733(3) 0.30777(4) 0.0000 0.00681(7) Uani 1 2 d S . . Si2 Si 0.18413(2) 0.18413(2) 0.18413(2) 0.00677(7) Uani 1 3 d S . . Si3 Si 0.2500 0.5000 0.0000 0.00666(14) Uani 1 8 d S . . Na1 Na 0.0000 0.0000 0.0000 0.0185(4) Uani 1 24 d S . . Na2 Na 0.0000 0.5000 0.2500 0.0416(8) Uani 1 8 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.00653(14) 0.00661(15) 0.00729(15) 0.000 0.000 -0.00057(13) Si2 0.00677(7) 0.00677(7) 0.00677(7) -0.00024(8) -0.00024(8) -0.00024(8) Si3 0.0070(3) 0.00651(19) 0.00651(19) 0.000 0.000 0.000 Na1 0.0185(4) 0.0185(4) 0.0185(4) 0.000 0.000 0.000 Na2 0.0490(10) 0.0490(10) 0.0267(10) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 Si2 2.3617(3) 26 ? Si1 Si2 2.3617(3) . ? Si1 Si3 2.3815(4) . ? Si1 Si1 2.3926(7) 3 ? Si1 Na1 3.3584(4) . ? Si1 Na2 3.4308(3) . ? Si1 Na2 3.4308(3) 25_565 ? Si2 Si2 2.3266(8) 14 ? Si2 Si1 2.3617(3) 9 ? Si2 Si1 2.3617(3) 5 ? Si2 Na1 3.2517(5) . ? Si3 Si1 2.3815(4) 19 ? Si3 Si1 2.3815(4) 27_565 ? Si3 Si1 2.3815(4) 41_665 ? Na1 Si2 3.2517(5) 25 ? Na1 Si2 3.2517(5) 28 ? Na1 Si2 3.2517(5) 4 ? Na1 Si2 3.2517(5) 27 ? Na1 Si2 3.2517(5) 3 ? Na1 Si2 3.2517(5) 26 ? Na1 Si2 3.2517(5) 2 ? Na1 Si1 3.3584(4) 25 ? Na1 Si1 3.3584(4) 9 ? Na1 Si1 3.3584(4) 33 ? Na2 Si1 3.4308(3) 39_666 ? Na2 Si1 3.4308(3) 3 ? Na2 Si1 3.4308(3) 37_666 ? Na2 Si1 3.4308(3) 25_565 ? Na2 Si1 3.4308(3) 13_455 ? Na2 Si1 3.4308(3) 27_565 ? Na2 Si1 3.4308(3) 15_455 ? 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 _geom_angle_publ_flag Si2 Si1 Si2 105.295(17) 26 . ? Si2 Si1 Si3 105.992(14) 26 . ? Si2 Si1 Si3 105.992(14) . . ? Si2 Si1 Si1 106.761(10) 26 3 ? Si2 Si1 Si1 106.761(10) . 3 ? Si3 Si1 Si1 124.613(9) . 3 ? Si2 Si1 Na1 66.668(12) 26 . ? Si2 Si1 Na1 66.668(12) . . ? Si3 Si1 Na1 166.255(14) . . ? Si1 Si1 Na1 69.132(6) 3 . ? Si2 Si1 Na2 174.958(12) 26 . ? Si2 Si1 Na2 79.333(5) . . ? Si3 Si1 Na2 74.210(8) . . ? Si1 Si1 Na2 69.592(6) 3 . ? Na1 Si1 Na2 114.180(8) . . ? Si2 Si1 Na2 79.333(5) 26 25_565 ? Si2 Si1 Na2 174.958(12) . 25_565 ? Si3 Si1 Na2 74.210(8) . 25_565 ? Si1 Si1 Na2 69.592(6) 3 25_565 ? Na1 Si1 Na2 114.180(8) . 25_565 ? Na2 Si1 Na2 95.974(9) . 25_565 ? Si2 Si2 Si1 108.497(12) 14 . ? Si2 Si2 Si1 108.497(12) 14 9 ? Si1 Si2 Si1 110.427(12) . 9 ? Si2 Si2 Si1 108.497(12) 14 5 ? Si1 Si2 Si1 110.427(12) . 5 ? Si1 Si2 Si1 110.427(12) 9 5 ? Si2 Si2 Na1 180.00(3) 14 . ? Si1 Si2 Na1 71.503(12) . . ? Si1 Si2 Na1 71.503(12) 9 . ? Si1 Si2 Na1 71.503(12) 5 . ? Si1 Si3 Si1 108.824(8) 19 . ? Si1 Si3 Si1 108.823(8) 19 27_565 ? Si1 Si3 Si1 110.775(17) . 27_565 ? Si1 Si3 Si1 110.775(17) 19 41_665 ? Si1 Si3 Si1 108.823(8) . 41_665 ? Si1 Si3 Si1 108.824(8) 27_565 41_665 ? Si2 Na1 Si2 180.000(13) . 25 ? Si2 Na1 Si2 70.5 . 28 ? Si2 Na1 Si2 109.5 25 28 ? Si2 Na1 Si2 109.5 . 4 ? Si2 Na1 Si2 70.5 25 4 ? Si2 Na1 Si2 180.000(7) 28 4 ? Si2 Na1 Si2 70.5 . 27 ? Si2 Na1 Si2 109.5 25 27 ? Si2 Na1 Si2 109.5 28 27 ? Si2 Na1 Si2 70.5 4 27 ? Si2 Na1 Si2 109.5 . 3 ? Si2 Na1 Si2 70.5 25 3 ? Si2 Na1 Si2 70.5 28 3 ? Si2 Na1 Si2 109.5 4 3 ? Si2 Na1 Si2 180.000(7) 27 3 ? Si2 Na1 Si2 70.5 . 26 ? Si2 Na1 Si2 109.5 25 26 ? Si2 Na1 Si2 109.5 28 26 ? Si2 Na1 Si2 70.5 4 26 ? Si2 Na1 Si2 109.5 27 26 ? Si2 Na1 Si2 70.5 3 26 ? Si2 Na1 Si2 109.5 . 2 ? Si2 Na1 Si2 70.5 25 2 ? Si2 Na1 Si2 70.5 28 2 ? Si2 Na1 Si2 109.5 4 2 ? Si2 Na1 Si2 70.5 27 2 ? Si2 Na1 Si2 109.5 3 2 ? Si2 Na1 Si2 180.000(13) 26 2 ? Si2 Na1 Si1 41.829(3) . . ? Si2 Na1 Si1 138.171(3) 25 . ? Si2 Na1 Si1 70.499(5) 28 . ? Si2 Na1 Si1 109.501(5) 4 . ? Si2 Na1 Si1 109.501(5) 27 . ? Si2 Na1 Si1 70.499(5) 3 . ? Si2 Na1 Si1 41.829(3) 26 . ? Si2 Na1 Si1 138.171(3) 2 . ? Si2 Na1 Si1 138.171(3) . 25 ? Si2 Na1 Si1 41.829(3) 25 25 ? Si2 Na1 Si1 109.501(5) 28 25 ? Si2 Na1 Si1 70.499(5) 4 25 ? Si2 Na1 Si1 70.499(5) 27 25 ? Si2 Na1 Si1 109.501(5) 3 25 ? Si2 Na1 Si1 138.171(3) 26 25 ? Si2 Na1 Si1 41.829(3) 2 25 ? Si1 Na1 Si1 180.000(5) . 25 ? Si2 Na1 Si1 41.829(3) . 9 ? Si2 Na1 Si1 138.171(3) 25 9 ? Si2 Na1 Si1 109.501(5) 28 9 ? Si2 Na1 Si1 70.499(5) 4 9 ? Si2 Na1 Si1 41.829(3) 27 9 ? Si2 Na1 Si1 138.171(3) 3 9 ? Si2 Na1 Si1 70.499(5) 26 9 ? Si2 Na1 Si1 109.501(5) 2 9 ? Si1 Na1 Si1 70.558(5) . 9 ? Si1 Na1 Si1 109.442(5) 25 9 ? Si2 Na1 Si1 138.171(3) . 33 ? Si2 Na1 Si1 41.829(3) 25 33 ? Si2 Na1 Si1 70.499(5) 28 33 ? Si2 Na1 Si1 109.501(5) 4 33 ? Si2 Na1 Si1 138.171(3) 27 33 ? Si2 Na1 Si1 41.829(3) 3 33 ? Si2 Na1 Si1 109.501(5) 26 33 ? Si2 Na1 Si1 70.499(5) 2 33 ? Si1 Na1 Si1 109.442(5) . 33 ? Si1 Na1 Si1 70.558(5) 25 33 ? Si1 Na1 Si1 180.000(12) 9 33 ? Si1 Na2 Si1 161.888(12) 39_666 3 ? Si1 Na2 Si1 40.815(12) 39_666 37_666 ? Si1 Na2 Si1 123.507(5) 3 37_666 ? Si1 Na2 Si1 123.507(5) 39_666 . ? Si1 Na2 Si1 40.815(12) 3 . ? Si1 Na2 Si1 98.837(9) 37_666 . ? Si1 Na2 Si1 123.507(5) 39_666 25_565 ? Si1 Na2 Si1 69.681(11) 3 25_565 ? Si1 Na2 Si1 161.888(12) 37_666 25_565 ? Si1 Na2 Si1 84.026(9) . 25_565 ? Si1 Na2 Si1 69.681(11) 39_666 13_455 ? Si1 Na2 Si1 123.507(5) 3 13_455 ? Si1 Na2 Si1 84.026(9) 37_666 13_455 ? Si1 Na2 Si1 161.888(12) . 13_455 ? Si1 Na2 Si1 98.837(9) 25_565 13_455 ? Si1 Na2 Si1 98.837(9) 39_666 27_565 ? Si1 Na2 Si1 84.026(9) 3 27_565 ? Si1 Na2 Si1 123.507(5) 37_666 27_565 ? Si1 Na2 Si1 69.681(11) . 27_565 ? Si1 Na2 Si1 40.815(12) 25_565 27_565 ? Si1 Na2 Si1 123.507(5) 13_455 27_565 ? Si1 Na2 Si1 84.026(9) 39_666 15_455 ? Si1 Na2 Si1 98.837(9) 3 15_455 ? Si1 Na2 Si1 69.681(11) 37_666 15_455 ? Si1 Na2 Si1 123.507(5) . 15_455 ? Si1 Na2 Si1 123.507(5) 25_565 15_455 ? Si1 Na2 Si1 40.815(12) 13_455 15_455 ? Si1 Na2 Si1 161.888(12) 27_565 15_455 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 38.07 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.422 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.082