data_beryl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H0 Al0.50 Be Fe0.67 Na0.17 O6.33 Si2' _chemical_formula_weight 221.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Be' 'Be' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, -x, -z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -x+y, -z+1/2' '-y, x-y, z' 'y, -x+y, z' 'x-y, x, z' '-x+y, -x, z' '-x, -y, -z' 'x, y, -z' 'y, x, z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 'x, x-y, z-1/2' 'y, -x+y, -z' '-y, x-y, -z' '-x+y, -x, -z' 'x-y, x, -z' _cell_length_a 9.258(3) _cell_length_b 9.258(3) _cell_length_c 9.156(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 679.6(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 3.00 _exptl_crystal_size_mid 2.00 _exptl_crystal_size_min 2.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 370 _exptl_absorpt_coefficient_mu 0.001 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9962 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3357 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.13 _diffrn_reflns_theta_max 45.74 _reflns_number_total 892 _reflns_number_gt 815 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0333P)^2^+3.1912P] 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 892 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _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 Be Be 0.5000 0.0000 0.2500 0.00733(13) Uani 1 4 d S . . Al* Al 0.3333 0.6667 0.2500 0.0056(4) Uani 0.831(13) 6 d SP . . Fe Fe 0.3333 0.6667 0.2500 0.0056(4) Uani 0.169(13) 6 d SP . . Si Si 0.38548(12) 0.11230(12) 0.0000 0.00518(15) Uani 1 2 d S . . O1 O 0.30468(11) 0.23022(11) 0.0000 0.01129(16) Uani 1 2 d S . . O2 O 0.49500(8) 0.14196(8) 0.14519(7) 0.00886(11) Uani 1 1 d . . . Na Na 0.0000 0.0000 0.0000 0.011(2) Uani 0.44(3) 12 d SP . . OW O 0.0000 0.0000 0.2500 0.0186(8) Uani 0.91(2) 12 d SP . . H1 H 0.025(4) 0.094(3) 0.181(3) 0.052(5) Uiso 0.152(4) 1 d P . . 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 Be 0.00777(18) 0.0074(2) 0.0067(3) 0.000 0.000 0.00370(12) Al* 0.0056(4) 0.0056(4) 0.0056(6) 0.000 0.000 0.0028(2) Fe 0.0056(4) 0.0056(4) 0.0056(6) 0.000 0.000 0.0028(2) Si 0.0057(3) 0.0052(3) 0.0050(3) 0.000 0.000 0.0029(2) O1 0.0118(3) 0.0112(3) 0.0151(4) 0.000 0.000 0.0089(2) O2 0.01095(19) 0.0124(2) 0.0061(2) -0.00062(15) -0.00110(16) 0.00796(16) Na 0.009(2) 0.009(2) 0.015(4) 0.000 0.000 0.0044(10) OW 0.0210(10) 0.0210(10) 0.0139(12) 0.000 0.000 0.0105(5) _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 Be O2 1.6465(7) 6_655 ? Be O2 1.6465(7) 2_655 ? Be O2 1.6465(7) 5 ? Be O2 1.6465(7) . ? Be Fe 2.6726(9) 1_545 ? Be Fe 2.6726(9) 2_665 ? Be Al* 2.6726(9) 1_545 ? Be Al* 2.6726(9) 2_665 ? Al* O2 1.9417(8) 10_565 ? Al* O2 1.9417(8) 5_565 ? Al* O2 1.9417(8) 2_665 ? Al* O2 1.9417(8) 4 ? Al* O2 1.9417(8) 11 ? Al* O2 1.9417(8) 8_665 ? Al* Be 2.6726(9) 1_565 ? Al* Be 2.6726(9) 3_565 ? Al* Be 2.6726(9) 7 ? Fe O2 1.9417(8) 10_565 ? Fe O2 1.9417(8) 5_565 ? Fe O2 1.9417(8) 2_665 ? Fe O2 1.9417(8) 4 ? Fe O2 1.9417(8) 11 ? Fe O2 1.9417(8) 8_665 ? Fe Be 2.6726(9) 1_565 ? Fe Be 2.6726(9) 3_565 ? Fe Be 2.6726(9) 7 ? Si O1 1.6026(14) . ? Si O1 1.6032(14) 21 ? Si O2 1.6100(9) . ? Si O2 1.6100(9) 14 ? Si Na 3.1791(14) . ? O1 Si 1.6032(14) 11 ? O1 Na 2.5470(12) . ? O2 Fe 1.9417(8) 2_665 ? O2 Al* 1.9417(8) 2_665 ? Na OW 2.2890(8) 13 ? Na OW 2.2890(8) . ? Na O1 2.5470(12) 21 ? Na O1 2.5470(12) 9 ? Na O1 2.5470(12) 13 ? Na O1 2.5470(12) 23 ? Na O1 2.5470(12) 11 ? Na Si 3.1791(14) 11 ? Na Si 3.1791(14) 23 ? Na Si 3.1791(14) 13 ? Na Si 3.1791(14) 21 ? Na H1 1.83(2) . ? OW Na 2.2890(8) 3 ? OW H1 1.00(2) . ? 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 O2 Be O2 129.42(4) 6_655 2_655 ? O2 Be O2 108.70(5) 6_655 5 ? O2 Be O2 92.54(5) 2_655 5 ? O2 Be O2 92.54(5) 6_655 . ? O2 Be O2 108.70(5) 2_655 . ? O2 Be O2 129.42(4) 5 . ? O2 Be Fe 133.73(2) 6_655 1_545 ? O2 Be Fe 46.27(2) 2_655 1_545 ? O2 Be Fe 46.27(2) 5 1_545 ? O2 Be Fe 133.73(2) . 1_545 ? O2 Be Fe 46.27(2) 6_655 2_665 ? O2 Be Fe 133.73(2) 2_655 2_665 ? O2 Be Fe 133.73(2) 5 2_665 ? O2 Be Fe 46.27(2) . 2_665 ? Fe Be Fe 180.0 1_545 2_665 ? O2 Be Al* 133.73(2) 6_655 1_545 ? O2 Be Al* 46.27(2) 2_655 1_545 ? O2 Be Al* 46.27(2) 5 1_545 ? O2 Be Al* 133.73(2) . 1_545 ? Fe Be Al* 0.0 1_545 1_545 ? Fe Be Al* 180.0 2_665 1_545 ? O2 Be Al* 46.27(2) 6_655 2_665 ? O2 Be Al* 133.73(2) 2_655 2_665 ? O2 Be Al* 133.73(2) 5 2_665 ? O2 Be Al* 46.27(2) . 2_665 ? Fe Be Al* 180.0 1_545 2_665 ? Fe Be Al* 0.0 2_665 2_665 ? Al* Be Al* 180.0 1_545 2_665 ? O2 Al* O2 89.72(4) 10_565 5_565 ? O2 Al* O2 97.68(3) 10_565 2_665 ? O2 Al* O2 75.58(4) 5_565 2_665 ? O2 Al* O2 75.58(4) 10_565 4 ? O2 Al* O2 97.68(3) 5_565 4 ? O2 Al* O2 170.66(3) 2_665 4 ? O2 Al* O2 97.68(3) 10_565 11 ? O2 Al* O2 170.66(3) 5_565 11 ? O2 Al* O2 97.68(3) 2_665 11 ? O2 Al* O2 89.72(4) 4 11 ? O2 Al* O2 170.66(3) 10_565 8_665 ? O2 Al* O2 97.68(3) 5_565 8_665 ? O2 Al* O2 89.72(4) 2_665 8_665 ? O2 Al* O2 97.68(3) 4 8_665 ? O2 Al* O2 75.58(4) 11 8_665 ? O2 Al* Be 94.670(16) 10_565 1_565 ? O2 Al* Be 37.791(19) 5_565 1_565 ? O2 Al* Be 37.791(19) 2_665 1_565 ? O2 Al* Be 135.141(19) 4 1_565 ? O2 Al* Be 135.141(19) 11 1_565 ? O2 Al* Be 94.670(16) 8_665 1_565 ? O2 Al* Be 37.791(19) 10_565 3_565 ? O2 Al* Be 94.670(16) 5_565 3_565 ? O2 Al* Be 135.141(19) 2_665 3_565 ? O2 Al* Be 37.791(19) 4 3_565 ? O2 Al* Be 94.670(16) 11 3_565 ? O2 Al* Be 135.141(19) 8_665 3_565 ? Be Al* Be 120.0 1_565 3_565 ? O2 Al* Be 135.141(19) 10_565 7 ? O2 Al* Be 135.141(19) 5_565 7 ? O2 Al* Be 94.670(16) 2_665 7 ? O2 Al* Be 94.670(16) 4 7 ? O2 Al* Be 37.791(19) 11 7 ? O2 Al* Be 37.791(19) 8_665 7 ? Be Al* Be 120.0 1_565 7 ? Be Al* Be 120.0 3_565 7 ? O2 Fe O2 89.72(4) 10_565 5_565 ? O2 Fe O2 97.68(3) 10_565 2_665 ? O2 Fe O2 75.58(4) 5_565 2_665 ? O2 Fe O2 75.58(4) 10_565 4 ? O2 Fe O2 97.68(3) 5_565 4 ? O2 Fe O2 170.66(3) 2_665 4 ? O2 Fe O2 97.68(3) 10_565 11 ? O2 Fe O2 170.66(3) 5_565 11 ? O2 Fe O2 97.68(3) 2_665 11 ? O2 Fe O2 89.72(4) 4 11 ? O2 Fe O2 170.66(3) 10_565 8_665 ? O2 Fe O2 97.68(3) 5_565 8_665 ? O2 Fe O2 89.72(4) 2_665 8_665 ? O2 Fe O2 97.68(3) 4 8_665 ? O2 Fe O2 75.58(4) 11 8_665 ? O2 Fe Be 94.670(16) 10_565 1_565 ? O2 Fe Be 37.791(19) 5_565 1_565 ? O2 Fe Be 37.791(19) 2_665 1_565 ? O2 Fe Be 135.141(19) 4 1_565 ? O2 Fe Be 135.141(19) 11 1_565 ? O2 Fe Be 94.670(16) 8_665 1_565 ? O2 Fe Be 37.791(19) 10_565 3_565 ? O2 Fe Be 94.670(16) 5_565 3_565 ? O2 Fe Be 135.141(19) 2_665 3_565 ? O2 Fe Be 37.791(19) 4 3_565 ? O2 Fe Be 94.670(16) 11 3_565 ? O2 Fe Be 135.141(19) 8_665 3_565 ? Be Fe Be 120.0 1_565 3_565 ? O2 Fe Be 135.141(19) 10_565 7 ? O2 Fe Be 135.141(19) 5_565 7 ? O2 Fe Be 94.670(16) 2_665 7 ? O2 Fe Be 94.670(16) 4 7 ? O2 Fe Be 37.791(19) 11 7 ? O2 Fe Be 37.791(19) 8_665 7 ? Be Fe Be 120.0 1_565 7 ? Be Fe Be 120.0 3_565 7 ? O1 Si O1 105.22(8) . 21 ? O1 Si O2 110.64(5) . . ? O1 Si O2 109.42(5) 21 . ? O1 Si O2 110.64(5) . 14 ? O1 Si O2 109.42(5) 21 14 ? O2 Si O2 111.31(8) . 14 ? O1 Si Na 52.61(4) . . ? O1 Si Na 52.61(4) 21 . ? O2 Si Na 124.34(4) . . ? O2 Si Na 124.34(4) 14 . ? Si O1 Si 165.22(8) . 11 ? Si O1 Na 97.40(5) . . ? Si O1 Na 97.38(5) 11 . ? Si O2 Be 127.71(5) . . ? Si O2 Fe 136.22(5) . 2_665 ? Be O2 Fe 95.94(3) . 2_665 ? Si O2 Al* 136.22(5) . 2_665 ? Be O2 Al* 95.94(3) . 2_665 ? Fe O2 Al* 0.0 2_665 2_665 ? OW Na OW 180.0 13 . ? OW Na O1 90.0 13 21 ? OW Na O1 90.0 . 21 ? OW Na O1 90.0 13 9 ? OW Na O1 90.0 . 9 ? O1 Na O1 180.00(3) 21 9 ? OW Na O1 90.0 13 . ? OW Na O1 90.0 . . ? O1 Na O1 60.0 21 . ? O1 Na O1 120.0 9 . ? OW Na O1 90.0 13 13 ? OW Na O1 90.0 . 13 ? O1 Na O1 120.0 21 13 ? O1 Na O1 60.0 9 13 ? O1 Na O1 180.0 . 13 ? OW Na O1 90.0 13 23 ? OW Na O1 90.0 . 23 ? O1 Na O1 60.0 21 23 ? O1 Na O1 120.0 9 23 ? O1 Na O1 120.0 . 23 ? O1 Na O1 60.0 13 23 ? OW Na O1 90.0 13 11 ? OW Na O1 90.0 . 11 ? O1 Na O1 120.0 21 11 ? O1 Na O1 60.0 9 11 ? O1 Na O1 60.0 . 11 ? O1 Na O1 120.0 13 11 ? O1 Na O1 180.00(4) 23 11 ? OW Na Si 90.0 13 11 ? OW Na Si 90.0 . 11 ? O1 Na Si 90.01(3) 21 11 ? O1 Na Si 89.99(3) 9 11 ? O1 Na Si 30.01(3) . 11 ? O1 Na Si 149.99(3) 13 11 ? O1 Na Si 150.01(3) 23 11 ? O1 Na Si 29.99(3) 11 11 ? OW Na Si 90.0 13 23 ? OW Na Si 90.0 . 23 ? O1 Na Si 89.99(3) 21 23 ? O1 Na Si 90.01(3) 9 23 ? O1 Na Si 149.99(3) . 23 ? O1 Na Si 30.01(3) 13 23 ? O1 Na Si 29.99(3) 23 23 ? O1 Na Si 150.01(3) 11 23 ? Si Na Si 180.00(3) 11 23 ? OW Na Si 90.0 13 13 ? OW Na Si 90.0 . 13 ? O1 Na Si 149.99(3) 21 13 ? O1 Na Si 30.01(3) 9 13 ? O1 Na Si 150.01(3) . 13 ? O1 Na Si 29.99(3) 13 13 ? O1 Na Si 89.99(3) 23 13 ? O1 Na Si 90.01(3) 11 13 ? Si Na Si 120.0 11 13 ? Si Na Si 60.0 23 13 ? OW Na Si 90.0 13 21 ? OW Na Si 90.0 . 21 ? O1 Na Si 29.99(3) 21 21 ? O1 Na Si 150.01(3) 9 21 ? O1 Na Si 89.99(3) . 21 ? O1 Na Si 90.01(3) 13 21 ? O1 Na Si 30.01(3) 23 21 ? O1 Na Si 149.99(3) 11 21 ? Si Na Si 120.0 11 21 ? Si Na Si 60.0 23 21 ? Si Na Si 120.0 13 21 ? OW Na H1 154.8(7) 13 . ? OW Na H1 25.2(7) . . ? O1 Na H1 101.8(9) 21 . ? O1 Na H1 78.2(9) 9 . ? O1 Na H1 77.2(9) . . ? O1 Na H1 102.8(9) 13 . ? O1 Na H1 115.2(7) 23 . ? O1 Na H1 64.8(7) 11 . ? Si Na H1 68.1(8) 11 . ? Si Na H1 111.9(8) 23 . ? Si Na H1 90.6(10) 13 . ? Si Na H1 111.3(8) 21 . ? Na OW Na 180.0 3 . ? Na OW H1 128.9(14) 3 . ? Na OW H1 51.1(14) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 45.74 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 1.306 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.257