# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Angeles Monge' _publ_contact_author_address ; Synthesis and Oxide structure Instituto de Ciencia de Materiales de Madrid Cantoblanco s/n Madrid S 28049 SPAIN ; _publ_contact_author_phone '34 91 334-9025' _publ_contact_author_fax '34 91 372-0623' _publ_contact_author_email amonge@icmm.csic.es _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Germanium zeotype with a three-dimensional net of interconnected 14-, 12- and 12-Ring Channels. Ge13O26(OH)4[C6 N2 H16 ]22+ (H2O)1,5 . ; loop_ _publ_author_name _publ_author_address 'Manuela Eloisa Medina' ; 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 ; 'M. Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'N. Snejko' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; data_ICMM7 _database_code_depnum_ccdc_archive 'CCDC 247518' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ICMM7 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H39 Ge13 N4 O31.50' _chemical_formula_weight 1687.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4739(4) _cell_length_b 12.6016(5) _cell_length_c 15.5505(6) _cell_angle_alpha 86.0710(10) _cell_angle_beta 79.1620(10) _cell_angle_gamma 83.7800(10) _cell_volume 2001.56(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5676 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.09 _exptl_crystal_description laminar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1614 _exptl_absorpt_coefficient_mu 9.713 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4434 _exptl_absorpt_correction_T_max 0.6973 _exptl_absorpt_process_details ? _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23393 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.1127 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 29.35 _reflns_number_total 9719 _reflns_number_gt 6353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Population factors of Ge12 and Ge14 were constricted to the unit and refined. One of the aminomethylpiperidine molecule is involved in positional disorded, consecuently the population factor were introduced on the basis of the thermal parameter values following the model of disorded given in the paper. ; _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^)+(0.0612P)^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 9719 _refine_ls_number_parameters 564 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.284 _refine_ls_shift/su_mean 0.006 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 0.51837(8) 0.26008(6) 0.41261(6) 0.00997(18) Uani 1 1 d . . 1 Ge2 Ge 0.52036(8) 0.32058(6) 0.74118(6) 0.00981(18) Uani 1 1 d . . 1 Ge3 Ge 0.35674(8) 0.14334(6) 0.73221(6) 0.01069(18) Uani 1 1 d . . 1 Ge4 Ge 0.80015(8) 0.21140(6) 0.69854(6) 0.01038(18) Uani 1 1 d . . 1 Ge5 Ge 0.36510(8) 0.32813(6) 0.59718(6) 0.00927(18) Uani 1 1 d . . 1 Ge6 Ge 0.10348(8) 0.27248(6) 0.70416(6) 0.01059(18) Uani 1 1 d . . 1 Ge7 Ge 0.13966(8) 0.44485(7) 0.84112(6) 0.01391(19) Uani 1 1 d . . 1 Ge8 Ge 0.36476(8) 0.53245(6) 0.69546(6) 0.01102(18) Uani 1 1 d . . 1 Ge9 Ge 0.69953(8) 0.01508(7) 0.82582(6) 0.01314(19) Uani 1 1 d . . 1 Ge10 Ge 0.54532(8) -0.05217(6) 0.67946(6) 0.01112(18) Uani 1 1 d . . 1 Ge11 Ge 0.59377(8) 0.17030(6) 0.59203(6) 0.00958(18) Uani 1 1 d . . 1 Ge12 Ge 0.44696(9) 0.16943(7) 0.90277(6) 0.0123(2) Uani 0.9083(18) 1 d P . 1 Ge13 Ge 0.79144(11) -0.18450(9) 0.94471(8) 0.0348(3) Uani 1 1 d . . 1 Ge14 Ge 0.3433(9) 0.2642(7) 0.9107(6) 0.0123(2) Uani 0.0917(18) 1 d P . 1 O1 O 0.4035(5) 0.1742(4) 0.6060(3) 0.0099(11) Uani 1 1 d . . 1 O2 O 0.5463(5) 0.3186(4) 0.6128(3) 0.0101(11) Uani 1 1 d . . 1 O3 O 0.6181(5) 0.0251(4) 0.5916(4) 0.0121(12) Uani 1 1 d . . 1 O4 O 0.3452(5) 0.3033(4) 0.7299(4) 0.0104(11) Uani 1 1 d . . 1 O5 O 0.1813(5) 0.1489(4) 0.7335(4) 0.0123(12) Uani 1 1 d . . 1 O6 O 0.1919(5) 0.3200(4) 0.6065(4) 0.0143(12) Uani 1 1 d . . 1 O7 O 0.4898(5) 0.4672(4) 0.7444(4) 0.0160(13) Uani 1 1 d . . 1 O8 O 0.3992(5) 0.3389(4) 0.4776(3) 0.0125(12) Uani 1 1 d . . 1 O9 O 0.3855(5) -0.0019(4) 0.7165(4) 0.0169(13) Uani 1 1 d . . 1 O10 O 0.7640(5) 0.1818(4) 0.5998(4) 0.0151(12) Uani 1 1 d . . 1 O11 O 0.3471(5) 0.4733(4) 0.6032(4) 0.0127(12) Uani 1 1 d . . 1 O12 O 0.6383(6) -0.0703(4) 0.7642(4) 0.0217(14) Uani 1 1 d . . 1 O13 O 0.0573(5) 0.3615(4) 0.7886(4) 0.0205(14) Uani 1 1 d . . 1 O14 O 0.6233(5) 0.1851(4) 0.4724(4) 0.0136(12) Uani 1 1 d . . 1 O15 O 0.4811(5) 0.2988(4) 0.8617(4) 0.0164(13) Uani 1 1 d . . 1 O16 O 0.8112(5) 0.1000(4) 0.7710(4) 0.0204(14) Uani 1 1 d . . 1 O17 O 0.2166(5) 0.5419(4) 0.7707(4) 0.0193(13) Uani 1 1 d . . 1 O18 O 0.5860(5) 0.0768(5) 0.9088(4) 0.0190(13) Uani 1 1 d . . 1 O19 O 0.6960(5) 0.3188(4) 0.7430(4) 0.0152(12) Uani 1 1 d . . 1 O20 O 0.6117(5) 0.3338(4) 0.3275(4) 0.0163(13) Uani 1 1 d . . 1 O21 O 0.3338(5) 0.1241(5) 0.8523(4) 0.0186(13) Uani 1 1 d . . 1 O22 O 0.0057(5) 0.5135(5) 0.9094(4) 0.0201(13) Uani 1 1 d D . 1 H22 H -0.0079 0.5920 0.8952 0.024 Uiso 1 1 d RD . 1 O23 O 0.4423(5) 0.1827(4) 0.3508(4) 0.0161(13) Uani 1 1 d . . 1 O24 O 0.8078(5) -0.0677(5) 0.8797(4) 0.0219(14) Uani 1 1 d . . 1 O25 O 0.9557(5) 0.2522(4) 0.6772(4) 0.0186(13) Uani 1 1 d . . 1 O26 O 0.2355(6) 0.3889(5) 0.9160(4) 0.0271(15) Uani 1 1 d . . 1 O27 O 0.8942(8) -0.1839(8) 1.0212(6) 0.069(3) Uani 1 1 d D A 1 H27 H 0.8175 -0.1864 1.0711 0.083 Uiso 1 1 d RD A 1 O28 O 0.5399(5) 0.1633(4) 0.7255(4) 0.0131(12) Uani 1 1 d . . 1 O29 O 0.8519(9) -0.2934(7) 0.8779(6) 0.065(3) Uani 1 1 d D B 1 H29 H 0.7949 -0.3161 0.8450 0.078 Uiso 1 1 d RD B 1 O30 O 0.3752(6) 0.1864(5) 1.0141(4) 0.0278(15) Uani 1 1 d . . 1 N1 N 0.7128(18) 0.1414(10) 0.0893(11) 0.167(10) Uani 1 1 d . C 2 H1A H 0.6560 0.1019 0.0726 0.200 Uiso 1 1 calc R C 2 H1B H 0.7514 0.1008 0.1288 0.200 Uiso 1 1 calc R C 2 N2 N 0.7627(8) 0.4553(7) -0.1418(5) 0.041(2) Uani 1 1 d . C 2 H2A H 0.8461 0.4523 -0.1363 0.061 Uiso 1 1 calc R C 2 H2B H 0.7392 0.5182 -0.1668 0.061 Uiso 1 1 calc R C 2 H2C H 0.7525 0.4032 -0.1751 0.061 Uiso 1 1 calc R C 2 C1 C 0.8108(13) 0.1588(10) 0.0150(9) 0.058(4) Uani 1 1 d . C 2 H1C H 0.8212 0.0972 -0.0206 0.070 Uiso 1 1 calc R C 2 H1D H 0.8924 0.1613 0.0354 0.070 Uiso 1 1 calc R C 2 C2 C 0.7912(15) 0.2548(10) -0.0418(10) 0.080(5) Uani 1 1 d . C 2 H2D H 0.8764 0.2744 -0.0707 0.096 Uiso 1 1 calc R C 2 H2E H 0.7463 0.2362 -0.0871 0.096 Uiso 1 1 calc R C 2 C3 C 0.7197(12) 0.3468(11) -0.0009(8) 0.062(4) Uani 1 1 d . C 2 H3 H 0.7861 0.3737 0.0264 0.074 Uiso 1 1 calc R C 2 C4 C 0.6803(12) 0.4422(9) -0.0544(7) 0.047(3) Uani 1 1 d . C 2 H4A H 0.5911 0.4386 -0.0619 0.056 Uiso 1 1 calc R C 2 H4B H 0.6815 0.5053 -0.0223 0.056 Uiso 1 1 calc R C 2 C5 C 0.6160(12) 0.3260(10) 0.0780(8) 0.055(3) Uani 1 1 d . C 2 H5A H 0.6056 0.3859 0.1155 0.066 Uiso 1 1 calc R C 2 H5B H 0.5339 0.3238 0.0582 0.066 Uiso 1 1 calc R C 2 C6 C 0.6416(18) 0.2248(11) 0.1319(9) 0.081(5) Uani 1 1 d . C 2 H6A H 0.6860 0.2419 0.1779 0.097 Uiso 1 1 calc R C 2 H6B H 0.5579 0.2014 0.1602 0.097 Uiso 1 1 calc R C 2 N3 N 0.2403(9) 0.5524(7) 0.4551(6) 0.045(3) Uani 1 1 d . D 2 H3A H 0.2961 0.6002 0.4306 0.054 Uiso 1 1 calc R D 2 H3B H 0.2798 0.5051 0.4901 0.054 Uiso 1 1 calc R D 2 C8 C 0.1191(11) 0.6055(9) 0.5036(8) 0.049(3) Uani 1 1 d . D 2 H8A H 0.0846 0.6613 0.4657 0.059 Uiso 1 1 calc R D 2 H8B H 0.1390 0.6392 0.5531 0.059 Uiso 1 1 calc R D 2 C9 C 0.0141(11) 0.5292(9) 0.5372(9) 0.058(4) Uani 1 1 d . . 2 H9 H 0.0464 0.4767 0.5795 0.069 Uiso 1 1 calc R . 2 C10 C 0.0932(17) 0.4237(14) 0.4260(12) 0.021(4) Uiso 0.50 1 d P . 2 H10A H 0.0775 0.3831 0.3789 0.026 Uiso 0.50 1 calc PR . 2 H10B H 0.1273 0.3736 0.4683 0.026 Uiso 0.50 1 calc PR . 2 C11 C 0.1943(19) 0.4994(16) 0.3892(13) 0.032(5) Uani 0.50 1 d P D 2 H11A H 0.2682 0.4599 0.3541 0.038 Uiso 0.50 1 calc PR D 2 H11B H 0.1572 0.5531 0.3508 0.038 Uiso 0.50 1 calc PR D 2 N4 N 0.7903(9) 0.9631(10) 0.4419(7) 0.078(4) Uani 1 1 d . . 2 H12A H 0.7286 0.9980 0.4810 0.093 Uiso 1 1 calc R . 2 H12B H 0.7503 0.9214 0.4127 0.093 Uiso 1 1 calc R . 2 C13 C 1.125(3) 0.937(2) 0.6375(19) 0.075(9) Uiso 0.50 1 d P . 2 H13A H 1.1879 0.8840 0.6581 0.090 Uiso 1 1 calc R . 2 H13B H 1.0720 0.9722 0.6876 0.090 Uiso 1 1 calc R . 2 C14 C 1.044(2) 0.889(2) 0.5883(17) 0.059(8) Uani 0.50 1 d P E 2 H14A H 0.9864 0.8462 0.6292 0.071 Uiso 0.50 1 calc PR E 2 H14B H 1.1009 0.8402 0.5487 0.071 Uiso 0.50 1 calc PR E 2 C15 C 0.9601(10) 0.9643(9) 0.5338(8) 0.047(3) Uani 1 1 d . . 2 H15 H 0.8982 1.0101 0.5740 0.056 Uiso 1 1 calc R . 2 C16 C 0.8820(10) 0.8940(10) 0.4898(9) 0.054(4) Uani 1 1 d . F 2 H16A H 0.9415 0.8485 0.4491 0.065 Uiso 1 1 calc R F 2 H16B H 0.8330 0.8485 0.5340 0.065 Uiso 1 1 calc R F 2 O31 O 0.0777(15) 0.9900(13) 0.8468(11) 0.055(4) Uiso 0.50 1 d P G 2 O32 O 0.685(2) 0.6409(17) 0.7572(14) 0.090(7) Uiso 0.50 1 d P H 2 O33 O 0.083(3) 0.752(2) 0.777(2) 0.043(8) Uiso 0.25 1 d P I 2 O34 O 0.883(3) 0.767(3) 0.708(2) 0.060(10) Uiso 0.25 1 d P J 2 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 0.0124(4) 0.0087(4) 0.0090(4) 0.0001(3) -0.0016(3) -0.0025(3) Ge2 0.0083(4) 0.0108(4) 0.0107(5) -0.0003(3) -0.0024(3) -0.0017(3) Ge3 0.0081(4) 0.0109(4) 0.0132(5) 0.0017(3) -0.0018(3) -0.0027(3) Ge4 0.0076(4) 0.0121(4) 0.0119(5) 0.0011(3) -0.0029(3) -0.0017(3) Ge5 0.0088(4) 0.0092(4) 0.0097(4) 0.0006(3) -0.0018(3) -0.0011(3) Ge6 0.0073(4) 0.0119(4) 0.0128(5) -0.0002(3) -0.0021(3) -0.0019(3) Ge7 0.0132(4) 0.0162(4) 0.0114(5) -0.0014(3) 0.0014(3) -0.0034(3) Ge8 0.0121(4) 0.0088(4) 0.0113(5) -0.0002(3) 0.0005(3) -0.0022(3) Ge9 0.0136(4) 0.0143(4) 0.0125(5) 0.0010(3) -0.0043(4) -0.0034(3) Ge10 0.0116(4) 0.0086(4) 0.0140(5) -0.0001(3) -0.0040(3) -0.0023(3) Ge11 0.0085(4) 0.0099(4) 0.0104(5) 0.0001(3) -0.0019(3) -0.0013(3) Ge12 0.0125(5) 0.0148(5) 0.0098(5) 0.0016(4) -0.0024(4) -0.0031(4) Ge13 0.0307(6) 0.0344(6) 0.0351(7) 0.0076(5) -0.0001(5) 0.0002(5) Ge14 0.0125(5) 0.0148(5) 0.0098(5) 0.0016(4) -0.0024(4) -0.0031(4) O1 0.015(3) 0.004(3) 0.012(3) 0.000(2) -0.004(2) -0.003(2) O2 0.013(3) 0.010(3) 0.006(3) 0.000(2) 0.001(2) -0.002(2) O3 0.015(3) 0.006(3) 0.014(3) -0.002(2) 0.000(2) 0.001(2) O4 0.006(3) 0.011(3) 0.014(3) 0.003(2) -0.004(2) -0.003(2) O5 0.007(3) 0.014(3) 0.016(3) 0.002(2) 0.000(2) -0.004(2) O6 0.012(3) 0.018(3) 0.013(3) 0.004(2) -0.003(2) -0.003(2) O7 0.014(3) 0.012(3) 0.024(4) -0.005(2) -0.007(3) 0.000(2) O8 0.015(3) 0.018(3) 0.004(3) 0.000(2) -0.003(2) 0.000(2) O9 0.010(3) 0.017(3) 0.024(4) 0.001(3) -0.001(2) -0.004(2) O10 0.009(3) 0.018(3) 0.018(3) -0.003(2) -0.001(2) -0.003(2) O11 0.020(3) 0.008(3) 0.010(3) -0.004(2) -0.004(2) 0.000(2) O12 0.030(3) 0.011(3) 0.026(4) 0.001(3) -0.014(3) -0.002(2) O13 0.021(3) 0.021(3) 0.019(4) -0.005(3) 0.001(3) -0.009(2) O14 0.014(3) 0.019(3) 0.008(3) 0.001(2) -0.003(2) 0.001(2) O15 0.012(3) 0.018(3) 0.018(3) 0.001(2) -0.002(2) -0.002(2) O16 0.012(3) 0.022(3) 0.028(4) 0.008(3) -0.006(3) -0.006(2) O17 0.017(3) 0.015(3) 0.022(4) 0.001(3) 0.006(3) -0.001(2) O18 0.016(3) 0.032(4) 0.010(3) -0.001(3) -0.005(2) 0.002(2) O19 0.012(3) 0.019(3) 0.016(3) -0.007(2) -0.004(2) -0.004(2) O20 0.021(3) 0.009(3) 0.016(3) -0.001(2) 0.005(3) -0.004(2) O21 0.016(3) 0.026(3) 0.015(3) 0.006(3) -0.006(3) -0.007(2) O22 0.018(3) 0.019(3) 0.019(3) 0.000(3) 0.006(3) 0.000(2) O23 0.022(3) 0.012(3) 0.019(3) -0.007(2) -0.012(3) -0.004(2) O24 0.017(3) 0.020(3) 0.028(4) 0.011(3) -0.009(3) -0.002(2) O25 0.010(3) 0.025(3) 0.020(4) 0.005(3) -0.003(2) -0.004(2) O26 0.034(4) 0.037(4) 0.008(3) 0.004(3) -0.004(3) 0.010(3) O27 0.048(5) 0.103(8) 0.061(6) 0.036(6) -0.029(5) -0.020(5) O28 0.010(3) 0.015(3) 0.015(3) 0.001(2) -0.005(2) -0.003(2) O29 0.074(6) 0.045(5) 0.071(7) -0.020(5) -0.004(5) 0.006(5) O30 0.022(3) 0.051(4) 0.012(3) 0.004(3) -0.002(3) -0.013(3) N1 0.217(19) 0.044(8) 0.160(17) 0.044(10) 0.120(15) 0.039(10) N2 0.037(5) 0.060(6) 0.025(5) -0.006(5) 0.005(4) -0.019(4) C1 0.054(8) 0.054(8) 0.061(10) -0.016(7) -0.009(7) 0.017(6) C2 0.091(12) 0.046(9) 0.078(12) 0.011(8) 0.033(9) 0.008(8) C3 0.048(8) 0.083(10) 0.044(8) 0.017(8) -0.002(6) 0.016(7) C4 0.055(8) 0.056(8) 0.030(7) -0.014(6) 0.000(6) -0.020(6) C5 0.060(8) 0.054(8) 0.051(9) -0.011(7) 0.001(7) -0.017(6) C6 0.141(15) 0.055(9) 0.033(8) 0.015(7) 0.003(9) 0.002(10) N3 0.040(5) 0.042(6) 0.060(7) 0.036(5) -0.029(5) -0.026(4) C8 0.043(7) 0.042(7) 0.066(9) 0.028(6) -0.023(7) -0.020(5) C9 0.039(7) 0.051(8) 0.089(11) 0.045(8) -0.029(7) -0.026(6) C11 0.035(12) 0.037(12) 0.023(11) 0.016(9) -0.002(9) -0.013(9) N4 0.031(5) 0.134(11) 0.079(9) -0.098(8) -0.019(6) 0.017(6) C14 0.046(15) 0.068(18) 0.059(18) -0.052(15) 0.023(13) -0.008(13) C15 0.024(6) 0.063(8) 0.060(9) -0.036(7) -0.016(6) 0.000(5) C16 0.014(5) 0.079(9) 0.071(10) -0.045(8) 0.002(6) -0.005(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 Ge1 O8 1.720(5) . ? Ge1 O14 1.734(5) . ? Ge1 O23 1.759(5) . ? Ge1 O20 1.764(5) . ? Ge2 O19 1.843(5) . ? Ge2 O7 1.844(5) . ? Ge2 O15 1.850(6) . ? Ge2 O4 1.912(5) . ? Ge2 O2 1.965(5) . ? Ge2 O28 1.998(5) . ? Ge3 O5 1.828(5) . ? Ge3 O21 1.840(6) . ? Ge3 O9 1.848(5) . ? Ge3 O28 1.945(5) . ? Ge3 O1 1.954(5) . ? Ge3 O4 2.004(5) . ? Ge4 O10 1.722(6) . ? Ge4 O25 1.727(5) . ? Ge4 O19 1.739(5) . ? Ge4 O16 1.747(6) . ? Ge5 O6 1.806(5) . ? Ge5 O8 1.824(5) . ? Ge5 O11 1.825(5) . ? Ge5 O1 1.939(5) . ? Ge5 O2 1.948(5) . ? Ge5 O4 2.041(5) . ? Ge5 Ge11 2.9353(11) . ? Ge6 O25 1.727(5) 1_455 ? Ge6 O6 1.729(5) . ? Ge6 O13 1.749(6) . ? Ge6 O5 1.751(5) . ? Ge7 O26 1.742(6) . ? Ge7 O17 1.744(5) . ? Ge7 O13 1.759(6) . ? Ge7 O22 1.774(6) . ? Ge8 O11 1.710(5) . ? Ge8 O20 1.733(5) 2_666 ? Ge8 O7 1.739(5) . ? Ge8 O17 1.757(6) . ? Ge9 O12 1.735(6) . ? Ge9 O16 1.735(5) . ? Ge9 O18 1.745(6) . ? Ge9 O24 1.749(6) . ? Ge10 O23 1.726(5) 2_656 ? Ge10 O3 1.727(5) . ? Ge10 O9 1.730(5) . ? Ge10 O12 1.769(6) . ? Ge11 O3 1.820(5) . ? Ge11 O14 1.827(5) . ? Ge11 O10 1.832(5) . ? Ge11 O2 1.914(5) . ? Ge11 O1 1.960(5) . ? Ge11 O28 2.044(6) . ? Ge12 Ge14 1.519(9) . ? Ge12 O21 1.704(5) . ? Ge12 O15 1.758(5) . ? Ge12 O30 1.771(6) . ? Ge12 O18 1.777(6) . ? Ge13 O24 1.732(6) . ? Ge13 O30 1.744(6) 2_657 ? Ge13 O27 1.748(8) . ? Ge13 O29 1.767(8) . ? Ge13 Ge14 2.619(9) 2_657 ? Ge13 H27 2.0324 . ? Ge14 O15 1.591(10) . ? Ge14 O26 1.830(11) . ? Ge14 O30 1.890(11) . ? Ge14 O21 2.060(11) . ? Ge14 Ge13 2.619(9) 2_657 ? O20 Ge8 1.733(5) 2_666 ? O22 H22 0.9989 . ? O23 Ge10 1.726(5) 2_656 ? O25 Ge6 1.727(5) 1_655 ? O27 H27 1.0084 . ? O29 H29 0.9342 . ? O30 Ge13 1.744(6) 2_657 ? N1 C6 1.357(18) . ? N1 C1 1.415(16) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C4 1.476(13) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? C1 C2 1.467(17) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C3 1.430(17) . ? C2 H2D 0.9700 . ? C2 H2E 0.9700 . ? C3 C4 1.480(16) . ? C3 C5 1.506(16) . ? C3 H3 0.9800 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.505(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N3 C11 1.44(2) . ? N3 C8 1.467(14) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C8 C9 1.533(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.27(2) 2_566 ? C9 C9 1.50(3) 2_566 ? C9 H9 0.9800 . ? C10 C9 1.27(2) 2_566 ? C10 C11 1.51(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N4 C16 1.495(16) . ? N4 C13 1.87(3) 2_776 ? N4 H12A 0.9000 . ? N4 H12B 0.9000 . ? C13 C14 1.45(3) . ? C13 N4 1.87(3) 2_776 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.55(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C15 1.52(2) 2_776 ? C15 C16 1.541(14) . ? C15 H15 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? O31 H311 0.7126 . ? O31 H312 0.7834 . ? O32 H321 0.8858 . ? O32 H322 0.6932 . ? 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 O8 Ge1 O14 112.4(3) . . ? O8 Ge1 O23 108.5(3) . . ? O14 Ge1 O23 113.6(3) . . ? O8 Ge1 O20 113.0(2) . . ? O14 Ge1 O20 108.7(3) . . ? O23 Ge1 O20 100.1(3) . . ? O19 Ge2 O7 94.1(2) . . ? O19 Ge2 O15 91.8(2) . . ? O7 Ge2 O15 94.0(3) . . ? O19 Ge2 O4 171.4(2) . . ? O7 Ge2 O4 93.5(2) . . ? O15 Ge2 O4 91.8(2) . . ? O19 Ge2 O2 93.9(2) . . ? O7 Ge2 O2 94.9(2) . . ? O15 Ge2 O2 169.1(2) . . ? O4 Ge2 O2 81.3(2) . . ? O19 Ge2 O28 91.1(2) . . ? O7 Ge2 O28 172.7(2) . . ? O15 Ge2 O28 91.1(2) . . ? O4 Ge2 O28 81.1(2) . . ? O2 Ge2 O28 79.5(2) . . ? O5 Ge3 O21 92.2(2) . . ? O5 Ge3 O9 94.0(2) . . ? O21 Ge3 O9 92.7(3) . . ? O5 Ge3 O28 170.3(2) . . ? O21 Ge3 O28 91.0(2) . . ? O9 Ge3 O28 95.0(2) . . ? O5 Ge3 O1 95.1(2) . . ? O21 Ge3 O1 171.6(2) . . ? O9 Ge3 O1 91.0(2) . . ? O28 Ge3 O1 81.2(2) . . ? O5 Ge3 O4 90.4(2) . . ? O21 Ge3 O4 95.6(2) . . ? O9 Ge3 O4 170.4(2) . . ? O28 Ge3 O4 80.1(2) . . ? O1 Ge3 O4 80.2(2) . . ? O10 Ge4 O25 107.2(3) . . ? O10 Ge4 O19 110.7(3) . . ? O25 Ge4 O19 106.6(3) . . ? O10 Ge4 O16 113.3(3) . . ? O25 Ge4 O16 104.2(3) . . ? O19 Ge4 O16 114.2(3) . . ? O6 Ge5 O8 95.3(2) . . ? O6 Ge5 O11 93.6(2) . . ? O8 Ge5 O11 91.5(2) . . ? O6 Ge5 O1 93.1(2) . . ? O8 Ge5 O1 95.3(2) . . ? O11 Ge5 O1 170.0(2) . . ? O6 Ge5 O2 166.9(2) . . ? O8 Ge5 O2 96.4(2) . . ? O11 Ge5 O2 92.0(2) . . ? O1 Ge5 O2 80.0(2) . . ? O6 Ge5 O4 89.3(2) . . ? O8 Ge5 O4 173.4(2) . . ? O11 Ge5 O4 93.0(2) . . ? O1 Ge5 O4 79.6(2) . . ? O2 Ge5 O4 78.6(2) . . ? O6 Ge5 Ge11 134.49(17) . . ? O8 Ge5 Ge11 88.89(17) . . ? O11 Ge5 Ge11 131.64(17) . . ? O1 Ge5 Ge11 41.42(15) . . ? O2 Ge5 Ge11 40.12(15) . . ? O4 Ge5 Ge11 84.47(14) . . ? O25 Ge6 O6 103.6(3) 1_455 . ? O25 Ge6 O13 102.7(3) 1_455 . ? O6 Ge6 O13 117.2(3) . . ? O25 Ge6 O5 108.8(2) 1_455 . ? O6 Ge6 O5 108.2(3) . . ? O13 Ge6 O5 115.2(3) . . ? O26 Ge7 O17 112.0(3) . . ? O26 Ge7 O13 119.6(3) . . ? O17 Ge7 O13 113.6(3) . . ? O26 Ge7 O22 102.5(3) . . ? O17 Ge7 O22 106.4(3) . . ? O13 Ge7 O22 100.5(3) . . ? O11 Ge8 O20 110.7(3) . 2_666 ? O11 Ge8 O7 112.7(3) . . ? O20 Ge8 O7 110.6(3) 2_666 . ? O11 Ge8 O17 110.5(3) . . ? O20 Ge8 O17 101.2(2) 2_666 . ? O7 Ge8 O17 110.6(3) . . ? O12 Ge9 O16 117.9(3) . . ? O12 Ge9 O18 115.7(3) . . ? O16 Ge9 O18 112.8(3) . . ? O12 Ge9 O24 104.6(3) . . ? O16 Ge9 O24 97.2(3) . . ? O18 Ge9 O24 105.4(3) . . ? O23 Ge10 O3 108.8(3) 2_656 . ? O23 Ge10 O9 112.5(3) 2_656 . ? O3 Ge10 O9 111.2(3) . . ? O23 Ge10 O12 99.2(3) 2_656 . ? O3 Ge10 O12 112.1(3) . . ? O9 Ge10 O12 112.5(3) . . ? O3 Ge11 O14 92.8(2) . . ? O3 Ge11 O10 93.0(2) . . ? O14 Ge11 O10 94.1(2) . . ? O3 Ge11 O2 169.3(2) . . ? O14 Ge11 O2 96.5(2) . . ? O10 Ge11 O2 91.8(2) . . ? O3 Ge11 O1 93.5(2) . . ? O14 Ge11 O1 95.5(2) . . ? O10 Ge11 O1 168.1(2) . . ? O2 Ge11 O1 80.3(2) . . ? O3 Ge11 O28 90.7(2) . . ? O14 Ge11 O28 173.3(2) . . ? O10 Ge11 O28 91.4(2) . . ? O2 Ge11 O28 79.5(2) . . ? O1 Ge11 O28 78.6(2) . . ? O3 Ge11 Ge5 134.20(17) . . ? O14 Ge11 Ge5 89.05(17) . . ? O10 Ge11 Ge5 132.55(17) . . ? O2 Ge11 Ge5 40.97(15) . . ? O1 Ge11 Ge5 40.89(14) . . ? O28 Ge11 Ge5 84.45(15) . . ? Ge14 Ge12 O21 79.2(4) . . ? Ge14 Ge12 O15 57.5(4) . . ? O21 Ge12 O15 110.7(3) . . ? Ge14 Ge12 O30 69.6(4) . . ? O21 Ge12 O30 107.9(3) . . ? O15 Ge12 O30 104.1(3) . . ? Ge14 Ge12 O18 166.4(4) . . ? O21 Ge12 O18 114.3(3) . . ? O15 Ge12 O18 115.3(3) . . ? O30 Ge12 O18 103.4(3) . . ? O24 Ge13 O30 106.2(3) . 2_657 ? O24 Ge13 O27 106.9(4) . . ? O30 Ge13 O27 117.0(4) 2_657 . ? O24 Ge13 O29 108.1(4) . . ? O30 Ge13 O29 111.3(4) 2_657 . ? O27 Ge13 O29 107.0(5) . . ? O24 Ge13 Ge14 142.5(3) . 2_657 ? O30 Ge13 Ge14 46.2(3) 2_657 2_657 ? O27 Ge13 Ge14 76.3(3) . 2_657 ? O29 Ge13 Ge14 106.4(4) . 2_657 ? Ge12 Ge14 O15 68.8(4) . . ? Ge12 Ge14 O26 172.8(6) . . ? O15 Ge14 O26 104.1(5) . . ? Ge12 Ge14 O30 61.5(4) . . ? O15 Ge14 O30 105.9(5) . . ? O26 Ge14 O30 120.9(6) . . ? Ge12 Ge14 O21 54.3(3) . . ? O15 Ge14 O21 101.7(5) . . ? O26 Ge14 O21 130.6(5) . . ? O30 Ge14 O21 90.5(4) . . ? Ge12 Ge14 Ge13 93.3(4) . 2_657 ? O15 Ge14 Ge13 146.7(5) . 2_657 ? O26 Ge14 Ge13 92.2(4) . 2_657 ? O30 Ge14 Ge13 41.7(3) . 2_657 ? O21 Ge14 Ge13 88.5(3) . 2_657 ? Ge5 O1 Ge3 101.9(2) . . ? Ge5 O1 Ge11 97.7(2) . . ? Ge3 O1 Ge11 100.7(2) . . ? Ge11 O2 Ge5 98.9(2) . . ? Ge11 O2 Ge2 102.6(2) . . ? Ge5 O2 Ge2 99.9(2) . . ? Ge10 O3 Ge11 120.5(3) . . ? Ge2 O4 Ge3 99.3(2) . . ? Ge2 O4 Ge5 98.5(2) . . ? Ge3 O4 Ge5 96.8(2) . . ? Ge6 O5 Ge3 116.6(3) . . ? Ge6 O6 Ge5 119.4(3) . . ? Ge8 O7 Ge2 118.9(3) . . ? Ge1 O8 Ge5 124.6(3) . . ? Ge10 O9 Ge3 116.5(3) . . ? Ge4 O10 Ge11 119.1(3) . . ? Ge8 O11 Ge5 121.3(3) . . ? Ge9 O12 Ge10 134.6(3) . . ? Ge6 O13 Ge7 135.1(3) . . ? Ge1 O14 Ge11 124.0(3) . . ? Ge14 O15 Ge12 53.7(4) . . ? Ge14 O15 Ge2 122.2(5) . . ? Ge12 O15 Ge2 117.1(3) . . ? Ge9 O16 Ge4 133.8(3) . . ? Ge7 O17 Ge8 130.7(3) . . ? Ge9 O18 Ge12 130.5(3) . . ? Ge4 O19 Ge2 118.1(3) . . ? Ge8 O20 Ge1 135.5(3) 2_666 . ? Ge12 O21 Ge3 117.3(3) . . ? Ge12 O21 Ge14 46.4(3) . . ? Ge3 O21 Ge14 111.7(4) . . ? Ge10 O23 Ge1 138.3(3) 2_656 . ? Ge13 O24 Ge9 132.8(3) . . ? Ge6 O25 Ge4 154.3(4) 1_655 . ? Ge7 O26 Ge14 128.9(5) . . ? Ge3 O28 Ge2 98.4(2) . . ? Ge3 O28 Ge11 98.1(2) . . ? Ge2 O28 Ge11 97.0(2) . . ? Ge13 O30 Ge12 123.9(3) 2_657 . ? Ge13 O30 Ge14 92.1(4) 2_657 . ? Ge12 O30 Ge14 48.9(3) . . ? C6 N1 C1 120.9(12) . . ? C6 N1 H1A 107.1 . . ? C1 N1 H1A 107.1 . . ? C6 N1 H1B 107.1 . . ? C1 N1 H1B 107.1 . . ? H1A N1 H1B 106.8 . . ? C4 N2 H2A 109.5 . . ? C4 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C4 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? N1 C1 C2 117.8(12) . . ? N1 C1 H1C 107.8 . . ? C2 C1 H1C 107.9 . . ? N1 C1 H1D 107.8 . . ? C2 C1 H1D 107.8 . . ? H1C C1 H1D 107.2 . . ? C3 C2 C1 117.0(13) . . ? C3 C2 H2D 108.1 . . ? C1 C2 H2D 108.1 . . ? C3 C2 H2E 108.0 . . ? C1 C2 H2E 108.0 . . ? H2D C2 H2E 107.3 . . ? C2 C3 C4 120.6(12) . . ? C2 C3 C5 116.4(12) . . ? C4 C3 C5 111.8(10) . . ? C2 C3 H3 101.2 . . ? C4 C3 H3 101.3 . . ? C5 C3 H3 101.3 . . ? N2 C4 C3 115.1(10) . . ? N2 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C3 115.7(12) . . ? C6 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? C6 C5 H5B 108.4 . . ? C3 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? N1 C6 C5 117.1(13) . . ? N1 C6 H6A 108.0 . . ? C5 C6 H6A 108.0 . . ? N1 C6 H6B 108.0 . . ? C5 C6 H6B 108.0 . . ? H6A C6 H6B 107.3 . . ? C11 N3 C8 102.5(11) . . ? C11 N3 H3A 111.3 . . ? C8 N3 H3A 111.3 . . ? C11 N3 H3B 111.3 . . ? C8 N3 H3B 111.3 . . ? H3A N3 H3B 109.2 . . ? N3 C8 C9 113.4(10) . . ? N3 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N3 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C9 107.1(14) 2_566 2_566 ? C10 C9 C8 113.2(13) 2_566 . ? C9 C9 C8 110.5(13) 2_566 . ? C10 C9 H9 108.6 2_566 . ? C9 C9 H9 108.6 2_566 . ? C8 C9 H9 108.6 . . ? C9 C10 C11 113.1(15) 2_566 . ? C9 C10 H10A 108.9 2_566 . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 2_566 . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N3 C11 C10 113.9(15) . . ? N3 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? N3 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C16 N4 C13 112.6(11) . 2_776 ? C16 N4 H12A 109.1 . . ? C13 N4 H12A 109.0 2_776 . ? C16 N4 H12B 109.1 . . ? C13 N4 H12B 109.1 2_776 . ? H12A N4 H12B 107.8 . . ? C14 C13 N4 105(2) . 2_776 ? C14 C13 H13A 111.0 . . ? N4 C13 H13A 110.9 2_776 . ? C14 C13 H13B 110.7 . . ? N4 C13 H13B 110.7 2_776 . ? H13A C13 H13B 108.8 . . ? C13 C14 C15 118(2) . . ? C13 C14 H14A 107.8 . . ? C15 C14 H14A 108.0 . . ? C13 C14 H14B 107.9 . . ? C15 C14 H14B 108.0 . . ? H14A C14 H14B 107.2 . . ? C15 C15 C16 111.2(12) 2_776 . ? C15 C15 C14 113.3(14) 2_776 . ? C16 C15 C14 107.4(12) . . ? C15 C15 H15 108.3 2_776 . ? C16 C15 H15 108.3 . . ? C14 C15 H15 108.3 . . ? N4 C16 C15 109.8(10) . . ? N4 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? N4 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? H311 O31 H312 169.1 . . ? H321 O32 H322 160.5 . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 2.603 _refine_diff_density_min -2.883 _refine_diff_density_rms 0.243