Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_hj3 _database_code_CSD 190099 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Michael, Tsapatsis' 'Annamalai, Chandrasekaran' 'Hae-Kwon, Jeong' _publ_contact_author_name 'Michael Tsapatsis' _publ_contact_author_address ; Department of Chemical Engineering University of Massachusetts Goessmann Laboratory Amherst Massachusetts MA 01003 UNITED STATES OF AMERICA ; _publ_contact_author_email 'TSAPATSI@ECS.UMASS.EDU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis of a New Microporous Cerium Silicate Material and its Structure Determination by Single Crystal X-ray Diffraction ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Ce2 Na4.80 O34 Si12' _chemical_formula_weight 1279.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' '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' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' _cell_length_a 7.3093(4) _cell_length_b 7.1350(4) _cell_length_c 14.9713(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 780.78(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 835 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 25.03 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 617 _exptl_absorpt_coefficient_mu 3.533 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.9655 _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 'Nonius Kappa-CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1298 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 25.03 _reflns_number_total 749 _reflns_number_gt 656 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0513P)^2^+8.5861P] 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 749 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _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 Ce Ce 0.5000 0.5000 0.0000 0.0219(4) Uani 1 4 d S . . Si1 Si 0.2134(3) 0.7779(3) 0.15196(15) 0.0180(5) Uani 1 1 d . . . Si2 Si 0.5000 1.0666(5) 0.1026(2) 0.0237(8) Uani 1 2 d S . . O1 O 0.2729(9) 0.6390(8) 0.0752(4) 0.0324(15) Uani 1 1 d . . . O2 O 0.2500 0.6842(10) 0.2500 0.0244(18) Uani 1 2 d S . . O3 O 0.0000 0.8327(12) 0.1440(6) 0.0249(19) Uani 1 2 d S . . O4 O 0.3208(8) 0.9777(8) 0.1489(4) 0.0289(14) Uani 1 1 d . . . O5 O 0.5000 1.2865(13) 0.1095(7) 0.041(2) Uani 1 2 d S . . O6 O 0.5000 1.0000 0.0000 0.060(5) Uani 1 4 d S . . O1W O 0.0000 0.2862(18) 0.1475(11) 0.085(5) Uani 1 2 d S . . Na1 Na 0.0000 0.5000 0.0000 0.050(2) Uani 1 4 d S . . Na2 Na 0.2500 0.3300(16) 0.2500 0.104(5) Uani 0.70 2 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 Ce 0.0168(5) 0.0217(5) 0.0273(6) -0.0014(4) 0.000 0.000 Si1 0.0084(11) 0.0237(11) 0.0219(11) -0.0048(9) -0.0001(8) 0.0005(9) Si2 0.0114(14) 0.0289(17) 0.0309(19) 0.0119(15) 0.000 0.000 O1 0.026(3) 0.037(3) 0.034(3) -0.017(3) 0.001(3) 0.004(3) O2 0.024(4) 0.020(4) 0.029(4) 0.000 -0.006(4) 0.000 O3 0.005(4) 0.033(5) 0.037(5) 0.006(4) 0.000 0.000 O4 0.017(3) 0.033(3) 0.036(3) -0.001(3) 0.009(3) -0.006(3) O5 0.034(5) 0.028(5) 0.063(7) 0.012(5) 0.000 0.000 O6 0.042(8) 0.121(15) 0.016(7) 0.007(9) 0.000 0.000 O1W 0.081(10) 0.049(8) 0.126(13) 0.016(8) 0.000 0.000 Na1 0.021(4) 0.064(6) 0.066(6) -0.035(5) 0.000 0.000 Na2 0.070(8) 0.054(7) 0.186(15) 0.000 -0.016(9) 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 Ce O1 2.237(6) 7_655 ? Ce O1 2.237(6) 3_565 ? Ce O1 2.237(6) . ? Ce O1 2.237(6) 5_665 ? Ce O5 2.238(10) 5_675 ? Ce O5 2.238(10) 1_545 ? Ce Si2 3.453(3) 1_545 ? Ce Si2 3.453(3) 5_675 ? Ce Na1 3.6546(2) 1_655 ? Ce Na1 3.6546(2) . ? Si1 O1 1.579(6) . ? Si1 O3 1.612(3) . ? Si1 O4 1.628(6) . ? Si1 O2 1.635(4) . ? Si1 Na1 3.397(2) . ? Si1 Na2 3.526(10) . ? Si2 O5 1.572(10) . ? Si2 O6 1.608(4) . ? Si2 O4 1.612(6) 7_655 ? Si2 O4 1.612(6) . ? Si2 Na2 3.426(7) 6_666 ? Si2 Na2 3.426(7) 1_565 ? Si2 Ce 3.453(3) 1_565 ? O1 Na1 2.496(6) . ? O2 Si1 1.635(4) 4 ? O2 Na2 2.527(14) . ? O3 Si1 1.612(3) 7 ? O4 Na2 2.980(11) 1_565 ? O5 Ce 2.238(10) 1_565 ? O5 Na2 2.804(9) 6_666 ? O5 Na2 2.804(9) 1_565 ? O6 Si2 1.608(4) 5_675 ? O1W Na2 2.407(11) . ? O1W Na2 2.407(11) 6_556 ? O1W Na1 2.684(15) . ? Na1 O1 2.496(6) 5_565 ? Na1 O1 2.496(6) 7 ? Na1 O1 2.496(6) 3_565 ? Na1 O1W 2.684(15) 5_565 ? Na1 Si1 3.397(2) 5_565 ? Na1 Si1 3.397(2) 7 ? Na1 Si1 3.397(2) 3_565 ? Na1 Ce 3.6546(2) 1_455 ? Na2 O1W 2.407(11) 6_656 ? Na2 O5 2.804(9) 1_545 ? Na2 O5 2.804(9) 6_546 ? Na2 O4 2.980(11) 1_545 ? Na2 O4 2.980(11) 4_545 ? Na2 Si2 3.426(7) 1_545 ? Na2 Si2 3.426(7) 6_546 ? Na2 Si1 3.526(10) 4 ? Na2 Na2 3.6546(2) 6_656 ? 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 O1 Ce O1 180.0 7_655 3_565 ? O1 Ce O1 95.8(3) 7_655 . ? O1 Ce O1 84.2(3) 3_565 . ? O1 Ce O1 84.2(3) 7_655 5_665 ? O1 Ce O1 95.8(3) 3_565 5_665 ? O1 Ce O1 180.0(3) . 5_665 ? O1 Ce O5 93.8(2) 7_655 5_675 ? O1 Ce O5 86.2(2) 3_565 5_675 ? O1 Ce O5 93.8(2) . 5_675 ? O1 Ce O5 86.2(2) 5_665 5_675 ? O1 Ce O5 86.2(2) 7_655 1_545 ? O1 Ce O5 93.8(2) 3_565 1_545 ? O1 Ce O5 86.2(2) . 1_545 ? O1 Ce O5 93.8(2) 5_665 1_545 ? O5 Ce O5 180.0(5) 5_675 1_545 ? O1 Ce Si2 99.98(17) 7_655 1_545 ? O1 Ce Si2 80.02(17) 3_565 1_545 ? O1 Ce Si2 99.98(17) . 1_545 ? O1 Ce Si2 80.02(17) 5_665 1_545 ? O5 Ce Si2 159.3(3) 5_675 1_545 ? O5 Ce Si2 20.7(3) 1_545 1_545 ? O1 Ce Si2 80.02(17) 7_655 5_675 ? O1 Ce Si2 99.98(17) 3_565 5_675 ? O1 Ce Si2 80.02(17) . 5_675 ? O1 Ce Si2 99.98(17) 5_665 5_675 ? O5 Ce Si2 20.7(3) 5_675 5_675 ? O5 Ce Si2 159.3(3) 1_545 5_675 ? Si2 Ce Si2 180.00(11) 1_545 5_675 ? O1 Ce Na1 42.10(15) 7_655 1_655 ? O1 Ce Na1 137.90(15) 3_565 1_655 ? O1 Ce Na1 137.90(15) . 1_655 ? O1 Ce Na1 42.10(15) 5_665 1_655 ? O5 Ce Na1 90.0 5_675 1_655 ? O5 Ce Na1 90.0 1_545 1_655 ? Si2 Ce Na1 90.0 1_545 1_655 ? Si2 Ce Na1 90.0 5_675 1_655 ? O1 Ce Na1 137.90(15) 7_655 . ? O1 Ce Na1 42.10(15) 3_565 . ? O1 Ce Na1 42.10(15) . . ? O1 Ce Na1 137.90(15) 5_665 . ? O5 Ce Na1 90.000(1) 5_675 . ? O5 Ce Na1 90.000(1) 1_545 . ? Si2 Ce Na1 90.0 1_545 . ? Si2 Ce Na1 90.0 5_675 . ? Na1 Ce Na1 180.0 1_655 . ? O1 Si1 O3 111.4(4) . . ? O1 Si1 O4 113.3(3) . . ? O3 Si1 O4 104.6(4) . . ? O1 Si1 O2 110.6(3) . . ? O3 Si1 O2 108.9(3) . . ? O4 Si1 O2 107.7(3) . . ? O1 Si1 Na1 43.3(2) . . ? O3 Si1 Na1 69.4(3) . . ? O4 Si1 Na1 135.5(2) . . ? O2 Si1 Na1 116.0(2) . . ? O1 Si1 Na2 73.4(3) . . ? O3 Si1 Na2 108.9(3) . . ? O4 Si1 Na2 140.2(2) . . ? O2 Si1 Na2 40.9(3) . . ? Na1 Si1 Na2 77.57(9) . . ? O5 Si2 O6 110.9(4) . . ? O5 Si2 O4 111.4(3) . 7_655 ? O6 Si2 O4 107.1(3) . 7_655 ? O5 Si2 O4 111.4(3) . . ? O6 Si2 O4 107.1(3) . . ? O4 Si2 O4 108.7(5) 7_655 . ? O5 Si2 Na2 53.9(3) . 6_666 ? O6 Si2 Na2 141.00(10) . 6_666 ? O4 Si2 Na2 60.4(3) 7_655 6_666 ? O4 Si2 Na2 111.9(3) . 6_666 ? O5 Si2 Na2 53.9(3) . 1_565 ? O6 Si2 Na2 141.00(10) . 1_565 ? O4 Si2 Na2 111.9(3) 7_655 1_565 ? O4 Si2 Na2 60.4(3) . 1_565 ? Na2 Si2 Na2 64.46(14) 6_666 1_565 ? O5 Si2 Ce 30.2(4) . 1_565 ? O6 Si2 Ce 80.76(12) . 1_565 ? O4 Si2 Ce 122.9(2) 7_655 1_565 ? O4 Si2 Ce 122.9(2) . 1_565 ? Na2 Si2 Ce 78.18(16) 6_666 1_565 ? Na2 Si2 Ce 78.18(16) 1_565 1_565 ? Si1 O1 Ce 148.1(4) . . ? Si1 O1 Na1 110.9(3) . . ? Ce O1 Na1 101.0(2) . . ? Si1 O2 Si1 131.8(5) 4 . ? Si1 O2 Na2 114.1(2) 4 . ? Si1 O2 Na2 114.1(2) . . ? Si1 O3 Si1 150.6(6) 7 . ? Si2 O4 Si1 138.5(4) . . ? Si2 O4 Na2 91.6(3) . 1_565 ? Si1 O4 Na2 129.8(3) . 1_565 ? Si2 O5 Ce 129.2(6) . 1_565 ? Si2 O5 Na2 99.2(4) . 6_666 ? Ce O5 Na2 118.3(3) 1_565 6_666 ? Si2 O5 Na2 99.2(4) . 1_565 ? Ce O5 Na2 118.3(3) 1_565 1_565 ? Na2 O5 Na2 81.3(3) 6_666 1_565 ? Si2 O6 Si2 180.00(7) 5_675 . ? Na2 O1W Na2 98.8(6) . 6_556 ? Na2 O1W Na1 116.8(4) . . ? Na2 O1W Na1 116.8(4) 6_556 . ? O1 Na1 O1 180.0 . 5_565 ? O1 Na1 O1 106.1(3) . 7 ? O1 Na1 O1 73.9(3) 5_565 7 ? O1 Na1 O1 73.9(3) . 3_565 ? O1 Na1 O1 106.1(3) 5_565 3_565 ? O1 Na1 O1 180.0(2) 7 3_565 ? O1 Na1 O1W 98.3(2) . 5_565 ? O1 Na1 O1W 81.7(2) 5_565 5_565 ? O1 Na1 O1W 98.3(2) 7 5_565 ? O1 Na1 O1W 81.7(2) 3_565 5_565 ? O1 Na1 O1W 81.7(2) . . ? O1 Na1 O1W 98.3(2) 5_565 . ? O1 Na1 O1W 81.7(2) 7 . ? O1 Na1 O1W 98.3(2) 3_565 . ? O1W Na1 O1W 180.0(6) 5_565 . ? O1 Na1 Si1 154.27(13) . 5_565 ? O1 Na1 Si1 25.73(13) 5_565 5_565 ? O1 Na1 Si1 99.61(14) 7 5_565 ? O1 Na1 Si1 80.39(14) 3_565 5_565 ? O1W Na1 Si1 77.3(3) 5_565 5_565 ? O1W Na1 Si1 102.7(3) . 5_565 ? O1 Na1 Si1 25.73(13) . . ? O1 Na1 Si1 154.27(13) 5_565 . ? O1 Na1 Si1 80.39(14) 7 . ? O1 Na1 Si1 99.61(14) 3_565 . ? O1W Na1 Si1 102.7(3) 5_565 . ? O1W Na1 Si1 77.3(3) . . ? Si1 Na1 Si1 180.00(5) 5_565 . ? O1 Na1 Si1 80.39(14) . 7 ? O1 Na1 Si1 99.61(14) 5_565 7 ? O1 Na1 Si1 25.73(13) 7 7 ? O1 Na1 Si1 154.27(13) 3_565 7 ? O1W Na1 Si1 102.7(3) 5_565 7 ? O1W Na1 Si1 77.3(3) . 7 ? Si1 Na1 Si1 125.34(7) 5_565 7 ? Si1 Na1 Si1 54.66(7) . 7 ? O1 Na1 Si1 99.61(14) . 3_565 ? O1 Na1 Si1 80.39(14) 5_565 3_565 ? O1 Na1 Si1 154.27(13) 7 3_565 ? O1 Na1 Si1 25.73(13) 3_565 3_565 ? O1W Na1 Si1 77.3(3) 5_565 3_565 ? O1W Na1 Si1 102.7(3) . 3_565 ? Si1 Na1 Si1 54.66(7) 5_565 3_565 ? Si1 Na1 Si1 125.34(7) . 3_565 ? Si1 Na1 Si1 180.0 7 3_565 ? O1 Na1 Ce 143.06(13) . 1_455 ? O1 Na1 Ce 36.94(13) 5_565 1_455 ? O1 Na1 Ce 36.94(13) 7 1_455 ? O1 Na1 Ce 143.06(13) 3_565 1_455 ? O1W Na1 Ce 90.000(1) 5_565 1_455 ? O1W Na1 Ce 90.000(1) . 1_455 ? Si1 Na1 Ce 62.67(3) 5_565 1_455 ? Si1 Na1 Ce 117.33(3) . 1_455 ? Si1 Na1 Ce 62.67(3) 7 1_455 ? Si1 Na1 Ce 117.33(3) 3_565 1_455 ? O1 Na1 Ce 36.94(13) . . ? O1 Na1 Ce 143.06(13) 5_565 . ? O1 Na1 Ce 143.06(13) 7 . ? O1 Na1 Ce 36.94(13) 3_565 . ? O1W Na1 Ce 90.000(1) 5_565 . ? O1W Na1 Ce 90.000(1) . . ? Si1 Na1 Ce 117.33(3) 5_565 . ? Si1 Na1 Ce 62.67(3) . . ? Si1 Na1 Ce 117.33(3) 7 . ? Si1 Na1 Ce 62.67(3) 3_565 . ? Ce Na1 Ce 180.0 1_455 . ? O1W Na2 O1W 165.1(8) . 6_656 ? O1W Na2 O2 97.5(4) . . ? O1W Na2 O2 97.5(4) 6_656 . ? O1W Na2 O5 90.1(4) . 1_545 ? O1W Na2 O5 88.2(4) 6_656 1_545 ? O2 Na2 O5 96.4(3) . 1_545 ? O1W Na2 O5 88.2(4) . 6_546 ? O1W Na2 O5 90.1(4) 6_656 6_546 ? O2 Na2 O5 96.4(3) . 6_546 ? O5 Na2 O5 167.3(6) 1_545 6_546 ? O1W Na2 O4 72.4(4) . 1_545 ? O1W Na2 O4 94.7(4) 6_656 1_545 ? O2 Na2 O4 147.53(16) . 1_545 ? O5 Na2 O4 54.0(2) 1_545 1_545 ? O5 Na2 O4 113.6(4) 6_546 1_545 ? O1W Na2 O4 94.7(4) . 4_545 ? O1W Na2 O4 72.4(4) 6_656 4_545 ? O2 Na2 O4 147.53(16) . 4_545 ? O5 Na2 O4 113.6(4) 1_545 4_545 ? O5 Na2 O4 54.0(2) 6_546 4_545 ? O4 Na2 O4 64.9(3) 1_545 4_545 ? O1W Na2 Si2 85.6(4) . 1_545 ? O1W Na2 Si2 86.2(4) 6_656 1_545 ? O2 Na2 Si2 123.27(16) . 1_545 ? O5 Na2 Si2 26.9(2) 1_545 1_545 ? O5 Na2 Si2 140.3(4) 6_546 1_545 ? O4 Na2 Si2 28.05(12) 1_545 1_545 ? O4 Na2 Si2 87.5(3) 4_545 1_545 ? O1W Na2 Si2 86.2(4) . 6_546 ? O1W Na2 Si2 85.6(4) 6_656 6_546 ? O2 Na2 Si2 123.27(16) . 6_546 ? O5 Na2 Si2 140.3(4) 1_545 6_546 ? O5 Na2 Si2 26.9(2) 6_546 6_546 ? O4 Na2 Si2 87.5(3) 1_545 6_546 ? O4 Na2 Si2 28.05(12) 4_545 6_546 ? Si2 Na2 Si2 113.5(3) 1_545 6_546 ? O1W Na2 Si1 116.2(4) . 4 ? O1W Na2 Si1 78.2(4) 6_656 4 ? O2 Na2 Si1 25.03(8) . 4 ? O5 Na2 Si1 111.3(3) 1_545 4 ? O5 Na2 Si1 80.7(2) 6_546 4 ? O4 Na2 Si1 164.30(15) 1_545 4 ? O4 Na2 Si1 124.49(12) 4_545 4 ? Si2 Na2 Si1 136.44(17) 1_545 4 ? Si2 Na2 Si1 105.64(11) 6_546 4 ? O1W Na2 Si1 78.2(4) . . ? O1W Na2 Si1 116.2(4) 6_656 . ? O2 Na2 Si1 25.03(8) . . ? O5 Na2 Si1 80.7(2) 1_545 . ? O5 Na2 Si1 111.3(3) 6_546 . ? O4 Na2 Si1 124.49(12) 1_545 . ? O4 Na2 Si1 164.30(15) 4_545 . ? Si2 Na2 Si1 105.64(11) 1_545 . ? Si2 Na2 Si1 136.44(17) 6_546 . ? Si1 Na2 Si1 50.06(17) 4 . ? O1W Na2 Na2 139.4(3) . 6_656 ? O1W Na2 Na2 40.6(3) 6_656 6_656 ? O2 Na2 Na2 90.000(1) . 6_656 ? O5 Na2 Na2 49.33(15) 1_545 6_656 ? O5 Na2 Na2 130.67(15) 6_546 6_656 ? O4 Na2 Na2 80.01(11) 1_545 6_656 ? O4 Na2 Na2 99.99(11) 4_545 6_656 ? Si2 Na2 Na2 57.77(7) 1_545 6_656 ? Si2 Na2 Na2 122.23(7) 6_546 6_656 ? Si1 Na2 Na2 85.64(4) 4 6_656 ? Si1 Na2 Na2 94.36(3) . 6_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.113 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.179