# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1790 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; E. Gutiirrez-Puebla Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; _publ_contact_author_phone '34 1 334-9024' _publ_contact_author_fax '34 1 372-0623' _publ_contact_author_email enrique@immrx1.icmm.csic.es _publ_requested_journal 'Angewante Chemie' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Diversity of Interlayer Connections in germanium Zeotypes. GeO16[(OH)(CH3NH3)(CH3NH2)]: A Third Way. ; loop_ _publ_author_name _publ_author_address 'Concepcion Cascales' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Enrique Gutierrez-Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Marta Iglesias' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Maria Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Caridad Ruiz-Valero' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Natalia Snejko' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; This work has been supported by th CICYT (project MAT1999-0892) ; data_ICMM3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H12 Ge8 N2 O17' _chemical_formula_weight 916.86 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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+1/2, -z' _cell_length_a 7.4933(8) _cell_length_b 19.145(2) _cell_length_c 7.4944(8) _cell_angle_alpha 90.00 _cell_angle_beta 120.006(2) _cell_angle_gamma 90.00 _cell_volume 931.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.271 _exptl_crystal_density_method ? _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 12.817 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8132 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 32.36 _reflns_number_total 5751 _reflns_number_observed 4636 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0485P)^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 ? _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 0.48(6) _refine_ls_number_reflns 5751 _refine_ls_number_parameters 167 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_obs 0.0528 _refine_ls_wR_factor_all 0.1074 _refine_ls_wR_factor_obs 0.1033 _refine_ls_goodness_of_fit_all 0.873 _refine_ls_goodness_of_fit_obs 0.936 _refine_ls_restrained_S_all 0.873 _refine_ls_restrained_S_obs 0.936 _refine_ls_shift/esd_max -0.876 _refine_ls_shift/esd_mean 0.104 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ge1 Ge 0.2697(4) 0.19245(11) 0.1460(3) 0.0113(4) Uani 1 d . . Ge2 Ge 0.6757(4) -0.16437(13) 0.2863(4) 0.0129(5) Uani 1 d . . Ge3 Ge 0.5187(5) -0.07631(9) -0.4467(4) 0.0105(4) Uani 1 d . . Ge4 Ge 0.3651(4) 0.18271(14) -0.1935(4) 0.0127(5) Uani 1 d . . Ge5 Ge 0.5173(5) 0.09546(9) -0.4409(4) 0.0108(4) Uani 1 d . . Ge6 Ge -0.0651(4) 0.17530(12) -0.2946(3) 0.0114(4) Uani 1 d . . Ge7 Ge 1.1188(4) -0.17254(12) 0.3898(4) 0.0119(5) Uani 1 d . . Ge8 Ge 0.7826(4) -0.15634(11) -0.0419(3) 0.0112(4) Uani 1 d . . O1 O 0.4478(20) 0.1692(8) 0.0684(22) 0.015(3) Uiso 1 d . . O2 O 0.6141(22) -0.1287(8) 0.0444(22) 0.014(3) Uiso 1 d . . O3 O 1.0486(20) -0.1349(7) 0.1449(22) 0.014(3) Uiso 1 d . . O4 O 0.0181(17) 0.1609(7) -0.0290(17) 0.007(2) Uiso 1 d . . O5 O 0.1216(22) 0.1450(7) -0.3568(23) 0.015(3) Uiso 1 d . . O6 O -0.2430(22) 0.1055(8) -0.4156(22) 0.017(3) Uiso 1 d . . O7 O 0.7240(22) -0.2202(8) -0.2271(24) 0.019(3) Uiso 1 d . . O8 O 0.4371(16) 0.0093(10) -0.5020(20) 0.016(3) Uiso 1 d . . O9 O 0.3159(20) 0.1408(7) -0.6404(20) 0.014(3) Uiso 1 d . . O10 O 1.3220(20) -0.1197(6) 0.5676(20) 0.011(2) Uiso 1 d . . O11 O -0.2309(20) 0.2448(8) -0.4429(22) 0.011(3) Uiso 1 d . . O12 O 0.7454(22) -0.0844(8) -0.2112(22) 0.015(3) Uiso 1 d . . O13 O 0.5397(24) -0.1030(8) -0.6547(23) 0.021(3) Uiso 1 d . . O14 O 0.4485(21) 0.2561(8) -0.2684(26) 0.019(3) Uiso 1 d . . O15 O 0.9375(22) -0.1534(9) 0.4727(23) 0.025(3) Uiso 1 d . . O16 O 0.5330(21) 0.1189(8) -0.2069(20) 0.017(3) Uiso 1 d . . O17 O 0.1604(25) 0.2551(13) -0.1586(28) 0.020(3) Uiso 1 d . . H17 H 0.0593(257) 0.2610(104) -0.1425(325) 0.000(43) Uiso 1 d . . N1 N 1.1919(32) -0.0873(10) -0.1209(29) 0.017(3) Uiso 1 d . . H1A H 1.0991(121) -0.1015(10) -0.2469(53) 0.025 Uiso 1 calc R . H1B H 1.1611(160) -0.1050(10) -0.0297(117) 0.025 Uiso 1 calc R . H1C H 1.3165(57) -0.1018(10) -0.0915(162) 0.025 Uiso 1 calc R . C1 C 1.1900(64) -0.0059(20) -0.1114(61) 0.053(7) Uiso 1 d . . H1D H 1.0519(76) 0.0108(21) -0.1972(187) 0.080 Uiso 1 calc R . H1E H 1.2774(202) 0.0129(20) -0.1593(238) 0.080 Uiso 1 calc R . H1F H 1.2397(227) 0.0087(20) 0.0282(67) 0.080 Uiso 1 calc R . C2 C -0.1231(59) 0.0281(21) 0.2250(62) 0.049(7) Uiso 1 d . . H2A H -0.0066(140) 0.0138(21) 0.2132(237) 0.073 Uiso 1 calc R . H2B H -0.2471(108) 0.0100(21) 0.1105(153) 0.073 Uiso 1 calc R . H2C H -0.1091(246) 0.0103(21) 0.3512(119) 0.073 Uiso 1 calc R . N2 N -0.1328(35) 0.1022(11) 0.2249(34) 0.023(4) Uiso 1 d . . H2D H -0.2453(100) 0.1154(11) 0.2278(183) 0.035 Uiso 1 calc R . H2E H -0.1378(182) 0.1187(11) 0.1116(90) 0.035 Uiso 1 calc R . H2F H -0.0216(92) 0.1188(11) 0.3355(100) 0.035 Uiso 1 calc R . 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 0.0158(10) 0.0070(11) 0.0122(10) -0.0004(9) 0.0076(9) 0.0010(9) Ge2 0.0138(11) 0.0106(13) 0.0160(11) -0.0009(10) 0.0087(10) -0.0011(10) Ge3 0.0144(11) 0.0034(10) 0.0130(10) 0.0008(10) 0.0064(11) 0.0003(10) Ge4 0.0145(11) 0.0102(13) 0.0115(10) 0.0000(9) 0.0052(9) -0.0009(9) Ge5 0.0137(10) 0.0062(11) 0.0128(10) 0.0016(10) 0.0068(10) 0.0005(10) Ge6 0.0121(10) 0.0117(12) 0.0091(10) 0.0004(10) 0.0043(9) 0.0011(10) Ge7 0.0133(11) 0.0082(12) 0.0149(11) 0.0004(10) 0.0077(9) -0.0001(10) Ge8 0.0132(11) 0.0091(12) 0.0133(10) -0.0007(10) 0.0081(10) -0.0006(10) _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 O1 1.759(13) . ? Ge1 O9 1.762(14) 1_556 ? Ge1 O4 1.780(11) . ? Ge1 O7 1.77(2) 2_655 ? Ge1 O17 2.33(2) . ? Ge2 O13 1.75(2) 1_556 ? Ge2 O2 1.769(15) . ? Ge2 O14 1.75(2) 2_645 ? Ge2 O15 1.762(14) . ? Ge3 O13 1.72(2) . ? Ge3 O8 1.73(2) . ? Ge3 O12 1.739(14) . ? Ge3 O10 1.742(12) 1_454 ? Ge4 O14 1.74(2) . ? Ge4 O1 1.757(14) . ? Ge4 O5 1.765(15) . ? Ge4 O16 1.792(15) . ? Ge4 O17 2.18(2) . ? Ge4 Ge6 2.923(3) . ? Ge5 O6 1.719(14) 1_655 ? Ge5 O8 1.74(2) . ? Ge5 O9 1.735(14) . ? Ge5 O16 1.757(14) . ? Ge6 O5 1.778(14) . ? Ge6 O11 1.780(15) . ? Ge6 O6 1.78(2) . ? Ge6 O4 1.785(12) . ? Ge6 O17 2.12(2) . ? Ge7 O11 1.742(15) 2_645 ? Ge7 O10 1.757(13) . ? Ge7 O3 1.789(14) . ? Ge7 O15 1.79(2) . ? Ge7 O17 2.38(2) 2_645 ? Ge8 O7 1.73(2) . ? Ge8 O2 1.764(13) . ? Ge8 O12 1.798(15) . ? Ge8 O3 1.819(13) . ? Ge8 O17 2.16(2) 2_645 ? O6 Ge5 1.720(14) 1_455 ? O7 Ge1 1.77(2) 2_645 ? O9 Ge1 1.762(14) 1_554 ? O10 Ge3 1.742(12) 1_656 ? O11 Ge7 1.742(15) 2_655 ? O13 Ge2 1.75(2) 1_554 ? O14 Ge2 1.75(2) 2_655 ? O17 Ge8 2.16(2) 2_655 ? O17 Ge7 2.38(2) 2_655 ? O17 H17 0.83(15) . ? N1 C1 1.56(4) . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? C1 H1D 0.96 . ? C1 H1E 0.96 . ? C1 H1F 0.96 . ? C2 N2 1.42(4) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? N2 H2D 0.89 . ? N2 H2E 0.89 . ? 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 Ge1 O9 108.7(7) . 1_556 ? O1 Ge1 O4 111.7(6) . . ? O9 Ge1 O4 97.7(6) 1_556 . ? O1 Ge1 O7 117.3(7) . 2_655 ? O9 Ge1 O7 105.0(7) 1_556 2_655 ? O4 Ge1 O7 114.2(6) . 2_655 ? O1 Ge1 O17 76.1(7) . . ? O9 Ge1 O17 171.9(6) 1_556 . ? O4 Ge1 O17 74.3(6) . . ? O7 Ge1 O17 77.7(8) 2_655 . ? O13 Ge2 O2 96.5(7) 1_556 . ? O13 Ge2 O14 104.4(7) 1_556 2_645 ? O2 Ge2 O14 113.6(7) . 2_645 ? O13 Ge2 O15 106.1(8) 1_556 . ? O2 Ge2 O15 112.5(7) . . ? O14 Ge2 O15 120.1(7) 2_645 . ? O13 Ge3 O8 104.3(7) . . ? O13 Ge3 O12 114.1(7) . . ? O8 Ge3 O12 112.1(6) . . ? O13 Ge3 O10 112.2(7) . 1_454 ? O8 Ge3 O10 105.0(5) . 1_454 ? O12 Ge3 O10 108.8(7) . 1_454 ? O14 Ge4 O1 119.7(7) . . ? O14 Ge4 O5 121.3(7) . . ? O1 Ge4 O5 112.3(6) . . ? O14 Ge4 O16 99.0(6) . . ? O1 Ge4 O16 95.5(7) . . ? O5 Ge4 O16 101.2(6) . . ? O14 Ge4 O17 85.0(7) . . ? O1 Ge4 O17 80.5(6) . . ? O5 Ge4 O17 78.3(7) . . ? O16 Ge4 O17 175.4(7) . . ? O14 Ge4 Ge6 118.8(5) . . ? O1 Ge4 Ge6 90.5(4) . . ? O5 Ge4 Ge6 34.6(4) . . ? O16 Ge4 Ge6 131.8(5) . . ? O17 Ge4 Ge6 46.4(6) . . ? O6 Ge5 O8 109.9(6) 1_655 . ? O6 Ge5 O9 116.7(6) 1_655 . ? O8 Ge5 O9 102.2(6) . . ? O6 Ge5 O16 108.4(7) 1_655 . ? O8 Ge5 O16 110.3(7) . . ? O9 Ge5 O16 109.1(6) . . ? O5 Ge6 O11 118.4(6) . . ? O5 Ge6 O6 96.2(7) . . ? O11 Ge6 O6 97.6(6) . . ? O5 Ge6 O4 111.1(6) . . ? O11 Ge6 O4 123.9(6) . . ? O6 Ge6 O4 101.9(6) . . ? O5 Ge6 O17 79.6(7) . . ? O11 Ge6 O17 84.3(7) . . ? O6 Ge6 O17 175.8(7) . . ? O4 Ge6 O17 80.0(6) . . ? O5 Ge6 Ge4 34.3(5) . . ? O11 Ge6 Ge4 117.4(4) . . ? O6 Ge6 Ge4 128.0(5) . . ? O4 Ge6 Ge4 89.6(4) . . ? O17 Ge6 Ge4 48.0(6) . . ? O11 Ge7 O10 102.3(6) 2_645 . ? O11 Ge7 O3 117.5(6) 2_645 . ? O10 Ge7 O3 104.2(6) . . ? O11 Ge7 O15 118.0(7) 2_645 . ? O10 Ge7 O15 98.0(6) . . ? O3 Ge7 O15 112.9(7) . . ? O11 Ge7 O17 77.6(7) 2_645 2_645 ? O10 Ge7 O17 177.8(6) . 2_645 ? O3 Ge7 O17 77.7(7) . 2_645 ? O15 Ge7 O17 80.1(6) . 2_645 ? O7 Ge8 O2 124.4(7) . . ? O7 Ge8 O12 95.0(7) . . ? O2 Ge8 O12 98.2(7) . . ? O7 Ge8 O3 121.1(7) . . ? O2 Ge8 O3 111.1(6) . . ? O12 Ge8 O3 95.4(6) . . ? O7 Ge8 O17 83.5(7) . 2_645 ? O2 Ge8 O17 84.8(7) . 2_645 ? O12 Ge8 O17 177.0(6) . 2_645 ? O3 Ge8 O17 83.3(6) . 2_645 ? Ge4 O1 Ge1 115.5(8) . . ? Ge2 O2 Ge8 113.1(8) . . ? Ge7 O3 Ge8 110.2(7) . . ? Ge1 O4 Ge6 114.8(7) . . ? Ge4 O5 Ge6 111.2(8) . . ? Ge5 O6 Ge6 127.9(9) 1_455 . ? Ge8 O7 Ge1 116.0(9) . 2_645 ? Ge3 O8 Ge5 143.5(7) . . ? Ge5 O9 Ge1 139.0(8) . 1_554 ? Ge3 O10 Ge7 131.8(8) 1_656 . ? Ge7 O11 Ge6 115.5(8) 2_655 . ? Ge3 O12 Ge8 120.8(8) . . ? Ge3 O13 Ge2 139.1(9) . 1_554 ? Ge4 O14 Ge2 117.6(8) . 2_655 ? Ge2 O15 Ge7 115.9(9) . . ? Ge5 O16 Ge4 122.1(8) . . ? Ge6 O17 Ge8 137.0(9) . 2_655 ? Ge6 O17 Ge4 85.6(9) . . ? Ge8 O17 Ge4 132.6(8) 2_655 . ? Ge6 O17 Ge1 84.6(7) . . ? Ge8 O17 Ge1 82.7(6) 2_655 . ? Ge4 O17 Ge1 82.4(7) . . ? Ge6 O17 Ge7 82.6(6) . 2_655 ? Ge8 O17 Ge7 81.1(8) 2_655 2_655 ? Ge4 O17 Ge7 134.3(9) . 2_655 ? Ge1 O17 Ge7 139.6(8) . 2_655 ? Ge6 O17 H17 66.7(100) . . ? Ge8 O17 H17 70.7(100) 2_655 . ? Ge4 O17 H17 148.3(100) . . ? Ge1 O17 H17 80.1(100) . . ? Ge7 O17 H17 59.6(100) 2_655 . ? C1 N1 H1A 110.6(16) . . ? C1 N1 H1B 108.7(17) . . ? H1A N1 H1B 109.45(9) . . ? C1 N1 H1C 109.2(17) . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 H1D 108.9(16) . . ? N1 C1 H1E 109.0(17) . . ? H1D C1 H1E 109.4 . . ? N1 C1 H1F 110.6(16) . . ? H1D C1 H1F 109.37(8) . . ? H1E C1 H1F 109.47(9) . . ? N2 C2 H2A 109.7(17) . . ? N2 C2 H2B 110.4(18) . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 108.4(19) . . ? H2A C2 H2C 109.45(6) . . ? H2B C2 H2C 109.48(6) . . ? C2 N2 H2D 109.6(17) . . ? C2 N2 H2E 108.4(18) . . ? H2D N2 H2E 109.5 . . ? _refine_diff_density_max 1.839 _refine_diff_density_min -1.941 _refine_diff_density_rms 0.296