# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/192 data_global _publ_contact_author_email jparise@notes.cc.sunysb.edu _publ_contact_author_fax 516-632-8240 _publ_contact_author_phone 516-632-8196 # AUTHORS LIST loop_ _publ_author_name _publ_author_address 'Tripathi, Akhilesh' ; Dept. of Chemistry SUNY, Stony Brook NY 11794-3400 USA ; 'Johnson, Geoffrey. M.' ; Dept. of Geosciences SUNY, Stony Brook NY 11794-2100 USA ; 'Kim Sun Jin' ; Dept. of Geosciences SUNY, Stony Brook NY 11794-2100 USA ; 'Parise, John. B.' ; Dept. of Chemistry & Dept. of Geosciences SUNY, Stony Brook NY 11794-2100 USA ; _publ_requested_journal ; Journal of Materials Chemistry ; _publ_section_title ;Na~2~Al~2~Ge~3~O~10~.2H~2~O: An Aluminogermanate with the Tetranatrolite Topology ; data_9/07933E _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AlGe-NATROLITE _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al1.87 Ge2.80 Na2 O10.2H2O' _chemical_formula_weight 495.79 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+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' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 13.3140(19) _cell_length_b 13.3140(19) _cell_length_c 6.8188(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1208.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2272 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.29 _exptl_crystal_description octahedral _exptl_crystal_colour 'white tanslucent ' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 927 _exptl_absorpt_coefficient_mu 7.179 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Bruker P4' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2272 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.29 _reflns_number_total 703 _reflns_number_gt 654 _reflns_threshold_expression >2sigma(I) _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^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Not refined' _refine_ls_hydrogen_treatment 'Not refined ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 703 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Ge1 Ge 0.06039(6) 0.63226(6) 0.62779(13) 0.0114(3) Uani 0.560(5) 1 d P . . Al1 Al 0.06039(6) 0.63226(6) 0.62779(13) 0.0114(3) Uani 0.373(3) 1 d P . . Ge2 Ge 0.0000 0.0000 0.0000 0.0104(4) Uani 0.560(5) 4 d SP . . Al2 Al 0.0000 0.0000 0.0000 0.0104(4) Uani 0.373(3) 4 d SP . . Na1 Na 0.3072(3) 0.2500 0.1250 0.0271(10) Uani 1 2 d S . . OW1 O 0.8653(5) 0.2500 0.1250 0.0363(17) Uani 1 2 d S . . O1 O 0.6177(4) 0.2500 0.1250 0.0183(12) Uani 1 2 d S . . O2 O 0.0910(3) 0.0603(4) 0.1383(7) 0.0276(11) Uani 1 1 d . . . O3 O 0.0607(3) 0.1383(3) 0.5287(8) 0.0242(11) Uani 1 1 d . . . 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 Ge1 0.0092(4) 0.0074(4) 0.0175(4) 0.0011(3) -0.0007(4) -0.0002(3) Al1 0.0092(4) 0.0074(4) 0.0175(4) 0.0011(3) -0.0007(4) -0.0002(3) Ge2 0.0089(5) 0.0089(5) 0.0133(7) 0.000 0.000 0.000 Al2 0.0089(5) 0.0089(5) 0.0133(7) 0.000 0.000 0.000 Na1 0.0269(18) 0.0195(18) 0.0348(19) 0.0063(17) 0.000 0.000 OW1 0.030(3) 0.037(4) 0.042(4) 0.005(4) 0.000 0.000 O1 0.012(3) 0.014(3) 0.029(3) 0.001(3) 0.000 0.000 O2 0.028(2) 0.030(3) 0.025(2) 0.002(2) -0.007(2) -0.012(2) O3 0.010(2) 0.023(2) 0.040(3) -0.010(2) 0.0072(18) -0.0002(17) _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 Ge1 O2 1.723(5) 16_454 ? Ge1 O3 1.735(4) 13_455 ? Ge1 O1 1.743(2) 9_455 ? Ge1 O3 1.745(4) 16_454 ? Ge1 Na1 3.1408(13) 3_566 ? Ge2 O2 1.732(4) . ? Ge2 O2 1.732(4) 2 ? Ge2 O2 1.732(4) 3 ? Ge2 O2 1.732(4) 4 ? Na1 O3 2.396(5) 10_554 ? Na1 O3 2.396(5) 5 ? Na1 OW1 2.417(5) 3_565 ? Na1 OW1 2.417(5) 12_545 ? Na1 O1 2.567(4) 12_545 ? Na1 O1 2.567(4) 3_565 ? Na1 Ge1 3.1408(13) 15_553 ? Na1 Al1 3.1408(13) 15_553 ? Na1 Al1 3.1408(13) 4_656 ? Na1 Ge1 3.1408(13) 4_656 ? Na1 Na1 3.734(3) 10_554 ? Na1 Na1 3.734(3) 10 ? OW1 Na1 2.417(5) 4_655 ? OW1 Na1 2.417(5) 11 ? O1 Al1 1.743(2) 9_544 ? O1 Ge1 1.743(2) 9_544 ? O1 Al1 1.743(2) 6_565 ? O1 Ge1 1.743(2) 6_565 ? O1 Na1 2.567(4) 11 ? O1 Na1 2.567(4) 4_655 ? O2 Al1 1.723(5) 8_454 ? O2 Ge1 1.723(5) 8_454 ? O3 Al1 1.735(4) 13_445 ? O3 Ge1 1.735(4) 13_445 ? O3 Al1 1.745(4) 8_454 ? O3 Ge1 1.745(4) 8_454 ? O3 Na1 2.396(5) 10 ? 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 Ge1 O3 111.2(3) 16_454 13_455 ? O2 Ge1 O1 106.07(16) 16_454 9_455 ? O3 Ge1 O1 111.6(2) 13_455 9_455 ? O2 Ge1 O3 112.7(2) 16_454 16_454 ? O3 Ge1 O3 111.1(2) 13_455 16_454 ? O1 Ge1 O3 103.75(19) 9_455 16_454 ? O2 Ge1 Na1 126.23(18) 16_454 3_566 ? O3 Ge1 Na1 122.52(18) 13_455 3_566 ? O1 Ge1 Na1 54.79(14) 9_455 3_566 ? O3 Ge1 Na1 49.15(16) 16_454 3_566 ? O2 Ge2 O2 114.0(3) . 2 ? O2 Ge2 O2 107.24(16) . 3 ? O2 Ge2 O2 107.24(16) 2 3 ? O2 Ge2 O2 107.24(16) . 4 ? O2 Ge2 O2 107.24(16) 2 4 ? O2 Ge2 O2 114.0(3) 3 4 ? O3 Na1 O3 85.5(2) 10_554 5 ? O3 Na1 OW1 115.62(15) 10_554 3_565 ? O3 Na1 OW1 91.73(16) 5 3_565 ? O3 Na1 OW1 91.73(16) 10_554 12_545 ? O3 Na1 OW1 115.62(15) 5 12_545 ? OW1 Na1 OW1 143.29(18) 3_565 12_545 ? O3 Na1 O1 145.68(16) 10_554 12_545 ? O3 Na1 O1 67.03(12) 5 12_545 ? OW1 Na1 O1 86.50(13) 3_565 12_545 ? OW1 Na1 O1 82.78(15) 12_545 12_545 ? O3 Na1 O1 67.03(12) 10_554 3_565 ? O3 Na1 O1 145.68(16) 5 3_565 ? OW1 Na1 O1 82.78(15) 3_565 3_565 ? OW1 Na1 O1 86.50(13) 12_545 3_565 ? O1 Na1 O1 145.50(15) 12_545 3_565 ? O3 Na1 Ge1 33.42(10) 10_554 15_553 ? O3 Na1 Ge1 117.23(16) 5 15_553 ? OW1 Na1 Ge1 102.29(12) 3_565 15_553 ? OW1 Na1 Ge1 87.07(13) 12_545 15_553 ? O1 Na1 Ge1 169.80(9) 12_545 15_553 ? O1 Na1 Ge1 33.70(5) 3_565 15_553 ? O3 Na1 Al1 33.42(10) 10_554 15_553 ? O3 Na1 Al1 117.23(16) 5 15_553 ? OW1 Na1 Al1 102.29(12) 3_565 15_553 ? OW1 Na1 Al1 87.07(13) 12_545 15_553 ? O1 Na1 Al1 169.80(9) 12_545 15_553 ? O1 Na1 Al1 33.70(5) 3_565 15_553 ? Ge1 Na1 Al1 0.00(3) 15_553 15_553 ? O3 Na1 Al1 117.23(16) 10_554 4_656 ? O3 Na1 Al1 33.42(10) 5 4_656 ? OW1 Na1 Al1 87.07(13) 3_565 4_656 ? OW1 Na1 Al1 102.29(12) 12_545 4_656 ? O1 Na1 Al1 33.70(5) 12_545 4_656 ? O1 Na1 Al1 169.80(9) 3_565 4_656 ? Ge1 Na1 Al1 150.25(13) 15_553 4_656 ? Al1 Na1 Al1 150.25(13) 15_553 4_656 ? O3 Na1 Ge1 117.23(16) 10_554 4_656 ? O3 Na1 Ge1 33.42(10) 5 4_656 ? OW1 Na1 Ge1 87.07(13) 3_565 4_656 ? OW1 Na1 Ge1 102.29(12) 12_545 4_656 ? O1 Na1 Ge1 33.70(5) 12_545 4_656 ? O1 Na1 Ge1 169.80(9) 3_565 4_656 ? Ge1 Na1 Ge1 150.25(13) 15_553 4_656 ? Al1 Na1 Ge1 150.25(13) 15_553 4_656 ? Al1 Na1 Ge1 0.000(16) 4_656 4_656 ? O3 Na1 Na1 92.83(13) 10_554 10_554 ? O3 Na1 Na1 123.34(14) 5 10_554 ? OW1 Na1 Na1 39.44(13) 3_565 10_554 ? OW1 Na1 Na1 121.03(14) 12_545 10_554 ? O1 Na1 Na1 119.04(13) 12_545 10_554 ? O1 Na1 Na1 43.34(9) 3_565 10_554 ? Ge1 Na1 Na1 67.33(2) 15_553 10_554 ? Al1 Na1 Na1 67.33(2) 15_553 10_554 ? Al1 Na1 Na1 126.50(2) 4_656 10_554 ? Ge1 Na1 Na1 126.50(2) 4_656 10_554 ? O3 Na1 Na1 123.34(14) 10_554 10 ? O3 Na1 Na1 92.83(13) 5 10 ? OW1 Na1 Na1 121.03(14) 3_565 10 ? OW1 Na1 Na1 39.44(13) 12_545 10 ? O1 Na1 Na1 43.34(9) 12_545 10 ? O1 Na1 Na1 119.04(13) 3_565 10 ? Ge1 Na1 Na1 126.50(2) 15_553 10 ? Al1 Na1 Na1 126.50(2) 15_553 10 ? Al1 Na1 Na1 67.33(2) 4_656 10 ? Ge1 Na1 Na1 67.33(2) 4_656 10 ? Na1 Na1 Na1 131.9(2) 10_554 10 ? Na1 OW1 Na1 101.1(3) 4_655 11 ? Al1 O1 Ge1 0.00(7) 9_544 9_544 ? Al1 O1 Al1 128.1(3) 9_544 6_565 ? Ge1 O1 Al1 128.1(3) 9_544 6_565 ? Al1 O1 Ge1 128.1(3) 9_544 6_565 ? Ge1 O1 Ge1 128.1(3) 9_544 6_565 ? Al1 O1 Ge1 0.00(7) 6_565 6_565 ? Al1 O1 Na1 91.51(11) 9_544 11 ? Ge1 O1 Na1 91.51(11) 9_544 11 ? Al1 O1 Na1 125.04(11) 6_565 11 ? Ge1 O1 Na1 125.04(11) 6_565 11 ? Al1 O1 Na1 125.04(11) 9_544 4_655 ? Ge1 O1 Na1 125.04(11) 9_544 4_655 ? Al1 O1 Na1 91.51(11) 6_565 4_655 ? Ge1 O1 Na1 91.51(11) 6_565 4_655 ? Na1 O1 Na1 93.32(17) 11 4_655 ? Al1 O2 Ge1 0.000(18) 8_454 8_454 ? Al1 O2 Ge2 137.7(3) 8_454 . ? Ge1 O2 Ge2 137.7(3) 8_454 . ? Al1 O3 Ge1 0.00(5) 13_445 13_445 ? Al1 O3 Al1 134.2(3) 13_445 8_454 ? Ge1 O3 Al1 134.2(3) 13_445 8_454 ? Al1 O3 Ge1 134.2(3) 13_445 8_454 ? Ge1 O3 Ge1 134.2(3) 13_445 8_454 ? Al1 O3 Ge1 0.00(6) 8_454 8_454 ? Al1 O3 Na1 127.6(2) 13_445 10 ? Ge1 O3 Na1 127.6(2) 13_445 10 ? Al1 O3 Na1 97.43(19) 8_454 10 ? Ge1 O3 Na1 97.43(19) 8_454 10 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.365 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.228