# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _publ_contact_author ; Nikolaus Korber Institut f\"ur Anorganische Chemie Universit\"at Regensburg Universit\"atsstr.31 93053 Regensburg Deutschland ; _publ_contact_author_email nikolaus.korber@chemie.uni-regensburg.de _publ_contact_author_fax '+49 941 9431812' _publ_contact_author_phone '+49 941 9434448' #========================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structures of the compounds [K(2.2.2-crypt)]Ge5 x 4 NH3 and [K(2.2.2-crypt)]Ge5 x 4 NH3, both containing Ge52- anions. ; loop_ _publ_author_name _publ_author_address #Prof. Dr. C.Suchentrunk ; Institut f\"ur Anorganische Chemie Universit\"at Regensburg Universit\"atsstr.31 93053 Regensburg Deutschland ; N.Korber ; Insitut f\"ur Anorganische Chemie Universit\"at Regensburg Universit\"atsstr.31 93053 Regensburg Deutschland ; _publ_contact_author_name 'Nikolaus Korber' #======================================================================== data_K-Crypt_Ge5 _database_code_depnum_ccdc_archive 'CCDC 615430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[potassium-(4,7,13,1621,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)]- nonagermanid - ammonia(1/4) ; _chemical_formula_moiety 'C36 H84 Ge5 N8 O12 K2' _chemical_formula_sum 'C36 H84 Ge5 K2 N8 O12' _chemical_formula_weight 1262.26 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' 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' K K 0.2009 0.2494 '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' H H 0.0000 0.0000 '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' _cell_length_a 11.2887(9) _cell_length_b 11.8949(9) _cell_length_c 11.9433(9) _cell_angle_alpha 117.911(8) _cell_angle_beta 98.650(9) _cell_angle_gamma 91.797(9) _cell_volume 1391.51(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.90 _cell_measurement_theta_max 51.86 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 0.649 _exptl_absorpt_process_details '(A.L.Spek, Platon 2004' _exptl_special_details ; crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) ; _diffrn_ambient_temperature 123(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 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method Phi _diffrn_standards_number 8934 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 6.0 _diffrn_standards_decay_% ? _diffrn_reflns_number 10669 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.93 _reflns_number_total 8934 _reflns_number_gt 8001 _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^)+(0.0866P)^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 constr _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 0.668(11) _refine_ls_number_reflns 8934 _refine_ls_number_parameters 572 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.57784(5) 0.39973(6) 0.87466(7) 0.03746(17) Uani 1 1 d . . . Ge2 Ge 0.39963(6) 0.51811(6) 0.87003(7) 0.04148(18) Uani 1 1 d . . . Ge3 Ge 0.40687(7) 0.34805(8) 0.96081(7) 0.0463(2) Uani 1 1 d . . . Ge4 Ge 0.39579(6) 0.26700(7) 0.70766(7) 0.04020(17) Uani 1 1 d . . . Ge5 Ge 0.22418(6) 0.35681(7) 0.81855(7) 0.03962(18) Uani 1 1 d . . . K1 K 0.94281(12) 0.95998(11) 1.05721(12) 0.0290(3) Uani 1 1 d . . . K2 K 0.10364(10) -0.33330(11) 0.43643(12) 0.0246(2) Uani 1 1 d . . . O11 O 0.2319(4) -0.5334(5) 0.4356(5) 0.0422(12) Uani 1 1 d . . . O8 O -0.0114(4) -0.1249(4) 0.5835(4) 0.0350(10) Uani 1 1 d . . . O5 O 1.0356(4) 1.1623(4) 1.0270(4) 0.0331(9) Uani 1 1 d . . . O12 O -0.0057(4) -0.5099(4) 0.4897(4) 0.0340(10) Uani 1 1 d . . . O2 O 0.8138(4) 0.9410(4) 1.2389(4) 0.0379(10) Uani 1 1 d . . . O9 O 0.2055(5) -0.2856(8) 0.2560(7) 0.068(2) Uani 1 1 d . . . O10 O -0.0345(6) -0.4036(6) 0.2002(5) 0.0544(15) Uani 1 1 d . . . O1 O 1.0544(4) 1.0620(4) 1.3178(4) 0.0364(10) Uani 1 1 d . . . O6 O 0.7815(4) 1.1142(5) 1.0010(6) 0.0470(13) Uani 1 1 d . . . O3 O 1.1040(6) 0.7859(5) 0.9348(5) 0.0545(15) Uani 1 1 d . . . O7 O 0.2370(5) -0.1280(5) 0.6595(6) 0.0629(18) Uani 1 1 d . . . O4 O 0.8580(6) 0.7164(5) 0.8279(5) 0.0506(13) Uani 1 1 d . . . N1 N 1.2088(5) 1.0423(6) 1.1359(5) 0.0369(12) Uani 1 1 d . . . N3 N 0.3690(5) -0.3040(5) 0.4639(7) 0.0411(14) Uani 1 1 d . . . N4 N -0.1651(5) -0.3652(5) 0.4035(6) 0.0373(13) Uani 1 1 d . . . N2 N 0.6788(6) 0.8691(7) 0.9762(7) 0.0492(15) Uani 1 1 d . . . N5 N 0.6372(6) 0.0514(7) 0.5817(9) 0.062(2) Uani 1 1 d . . . H5C H 0.5985 0.1203 0.6157 0.093 Uiso 1 1 calc R . . H5D H 0.5842 -0.0169 0.5291 0.093 Uiso 1 1 calc R . . H5E H 0.6887 0.0629 0.5373 0.093 Uiso 1 1 calc R . . N6 N 0.6194(8) 0.2994(14) 0.5020(12) 0.104(4) Uani 1 1 d . . . H6C H 0.6585 0.3158 0.5795 0.156 Uiso 1 1 calc R . . H6D H 0.5480 0.2549 0.4846 0.156 Uiso 1 1 calc R . . H6E H 0.6084 0.3728 0.5011 0.156 Uiso 1 1 calc R . . N7 N 0.8606(6) 0.2882(7) 0.6926(7) 0.0551(16) Uani 1 1 d . . . H7C H 0.9304 0.3313 0.7436 0.083 Uiso 1 1 calc R . . H7D H 0.8344 0.2326 0.7162 0.083 Uiso 1 1 calc R . . H7E H 0.8065 0.3428 0.6993 0.083 Uiso 1 1 calc R . . N8 N 0.5865(9) 0.2780(12) 0.2156(10) 0.104(4) Uani 1 1 d . . . H8C H 0.6109 0.3378 0.2974 0.156 Uiso 1 1 calc R . . H8D H 0.5194 0.2321 0.2087 0.156 Uiso 1 1 calc R . . H8E H 0.5719 0.3153 0.1662 0.156 Uiso 1 1 calc R . . C1 C -0.2171(7) -0.4345(7) 0.2652(8) 0.049(2) Uani 1 1 d . . . H1A H -0.3025 -0.4251 0.2536 0.059 Uiso 1 1 calc R . . H1B H -0.2095 -0.5250 0.2330 0.059 Uiso 1 1 calc R . . C2 C 0.8356(7) 1.1878(7) 0.9513(8) 0.0454(17) Uani 1 1 d . . . H2A H 0.7831 1.2502 0.9496 0.055 Uiso 1 1 calc R . . H2B H 0.8457 1.1317 0.8637 0.055 Uiso 1 1 calc R . . C3 C -0.1302(6) -0.5537(6) 0.4401(7) 0.0356(14) Uani 1 1 d . . . H3A H -0.1591 -0.6012 0.4801 0.043 Uiso 1 1 calc R . . H3B H -0.1428 -0.6102 0.3477 0.043 Uiso 1 1 calc R . . C4 C 1.2439(6) 1.1172(7) 1.2784(6) 0.0404(15) Uani 1 1 d . . . H4A H 1.2239 1.2039 1.3064 0.049 Uiso 1 1 calc R . . H4B H 1.3305 1.1217 1.3027 0.049 Uiso 1 1 calc R . . C5 C 0.9542(7) 1.2545(6) 1.0324(8) 0.0436(16) Uani 1 1 d . . . H5A H 0.9870 1.3093 1.0021 0.052 Uiso 1 1 calc R . . H5B H 0.9447 1.3078 1.1209 0.052 Uiso 1 1 calc R . . C6 C 1.2382(7) 1.1240(8) 1.0785(8) 0.0482(18) Uani 1 1 d . . . H6A H 1.2373 1.0695 0.9873 0.058 Uiso 1 1 calc R . . H6B H 1.3195 1.1670 1.1183 0.058 Uiso 1 1 calc R . . C7 C 0.0610(6) -0.6129(7) 0.4826(8) 0.0407(16) Uani 1 1 d . . . H7A H 0.0454 -0.6828 0.3948 0.049 Uiso 1 1 calc R . . H7B H 0.0355 -0.6445 0.5378 0.049 Uiso 1 1 calc R . . C8 C -0.1996(6) -0.4373(6) 0.4688(8) 0.0397(15) Uani 1 1 d . . . H8A H -0.2854 -0.4660 0.4413 0.048 Uiso 1 1 calc R . . H8B H -0.1844 -0.3806 0.5612 0.048 Uiso 1 1 calc R . . C9 C 0.6668(7) 1.0452(10) 0.9179(10) 0.062(2) Uani 1 1 d . . . H9A H 0.6797 0.9861 0.8322 0.075 Uiso 1 1 calc R . . H9B H 0.6136 1.1051 0.9110 0.075 Uiso 1 1 calc R . . C10 C 0.9454(11) 0.6247(7) 0.8013(7) 0.063(3) Uani 1 1 d . . . H10A H 0.9517 0.5937 0.8637 0.076 Uiso 1 1 calc R . . H10B H 0.9184 0.5522 0.7161 0.076 Uiso 1 1 calc R . . C11 C 1.2731(8) 0.9289(9) 1.0882(8) 0.055(2) Uani 1 1 d . . . H11A H 1.2677 0.8884 1.1416 0.066 Uiso 1 1 calc R . . H11B H 1.3577 0.9563 1.0983 0.066 Uiso 1 1 calc R . . C12 C 0.9937(8) 1.0322(7) 1.3996(6) 0.0426(17) Uani 1 1 d . . . H12A H 1.0249 1.0931 1.4893 0.051 Uiso 1 1 calc R . . H12B H 1.0075 0.9471 1.3863 0.051 Uiso 1 1 calc R . . C13 C 0.0590(6) -0.0288(6) 0.7026(7) 0.0384(15) Uani 1 1 d . . . H13A H 0.0571 -0.0533 0.7692 0.046 Uiso 1 1 calc R . . H13B H 0.0252 0.0518 0.7289 0.046 Uiso 1 1 calc R . . C14 C 0.1840(7) -0.0132(7) 0.6873(7) 0.0399(15) Uani 1 1 d . . . H14A H 0.1855 0.0071 0.6177 0.048 Uiso 1 1 calc R . . H14B H 0.2299 0.0571 0.7660 0.048 Uiso 1 1 calc R . . C15 C 0.4182(7) -0.2012(10) 0.5908(8) 0.059(2) Uani 1 1 d . . . H15A H 0.4260 -0.2376 0.6488 0.071 Uiso 1 1 calc R . . H15B H 0.4993 -0.1739 0.5888 0.071 Uiso 1 1 calc R . . C16 C 0.8627(8) 1.0382(7) 1.3678(7) 0.0459(17) Uani 1 1 d . . . H16A H 0.8215 1.0263 1.4279 0.055 Uiso 1 1 calc R . . H16B H 0.8498 1.1218 1.3761 0.055 Uiso 1 1 calc R . . C17 C -0.2063(6) -0.2365(6) 0.4647(8) 0.0460(18) Uani 1 1 d . . . H17A H -0.2898 -0.2461 0.4725 0.055 Uiso 1 1 calc R . . H17B H -0.2033 -0.1990 0.4083 0.055 Uiso 1 1 calc R . . C18 C 0.1931(7) -0.5665(8) 0.5246(7) 0.0470(17) Uani 1 1 d . . . H18A H 0.2080 -0.4924 0.6099 0.056 Uiso 1 1 calc R . . H18B H 0.2379 -0.6332 0.5288 0.056 Uiso 1 1 calc R . . C19 C 0.4134(8) -0.4234(11) 0.448(2) 0.148(9) Uani 1 1 d . . . H19A H 0.4290 -0.4667 0.3605 0.178 Uiso 1 1 calc R . . H19B H 0.4917 -0.3988 0.5043 0.178 Uiso 1 1 calc R . . C20 C -0.1335(6) -0.1447(7) 0.5966(8) 0.0465(18) Uani 1 1 d . . . H20A H -0.1673 -0.0638 0.6318 0.056 Uiso 1 1 calc R . . H20B H -0.1357 -0.1801 0.6549 0.056 Uiso 1 1 calc R . . C21 C 0.7450(9) 0.6574(8) 0.8193(8) 0.062(3) Uani 1 1 d . . . H21A H 0.7497 0.6278 0.8828 0.075 Uiso 1 1 calc R . . H21B H 0.7194 0.5842 0.7343 0.075 Uiso 1 1 calc R . . C22 C 1.1540(7) 1.2232(7) 1.0933(7) 0.0424(16) Uani 1 1 d . . . H22A H 1.1532 1.2780 1.1840 0.051 Uiso 1 1 calc R . . H22B H 1.1816 1.2762 1.0584 0.051 Uiso 1 1 calc R . . C23 C 0.4018(8) -0.2752(11) 0.3659(9) 0.073(3) Uani 1 1 d . . . H23A H 0.4401 -0.1875 0.4119 0.088 Uiso 1 1 calc R . . H23B H 0.4644 -0.3285 0.3318 0.088 Uiso 1 1 calc R . . C24 C 1.2276(8) 0.8303(9) 0.9490(8) 0.060(2) Uani 1 1 d . . . H24A H 1.2343 0.8681 0.8934 0.071 Uiso 1 1 calc R . . H24B H 1.2757 0.7591 0.9246 0.071 Uiso 1 1 calc R . . C25 C 0.6561(9) 0.7547(10) 0.8438(8) 0.066(3) Uani 1 1 d . . . H25A H 0.6558 0.7851 0.7812 0.080 Uiso 1 1 calc R . . H25B H 0.5762 0.7119 0.8283 0.080 Uiso 1 1 calc R . . C26 C 0.3636(9) -0.0955(10) 0.6455(12) 0.079(3) Uani 1 1 d . . . H26A H 0.3590 -0.0529 0.5929 0.095 Uiso 1 1 calc R . . H26B H 0.4107 -0.0371 0.7298 0.095 Uiso 1 1 calc R . . C27 C 0.3288(12) -0.285(3) 0.267(2) 0.240(17) Uani 1 1 d . . . H27A H 0.3424 -0.3627 0.1942 0.288 Uiso 1 1 calc R . . H27B H 0.3569 -0.2146 0.2540 0.288 Uiso 1 1 calc R . . C28 C 1.0622(10) 0.6830(7) 0.8077(7) 0.060(3) Uani 1 1 d . . . H28A H 1.1190 0.6197 0.7861 0.072 Uiso 1 1 calc R . . H28B H 1.0562 0.7149 0.7460 0.072 Uiso 1 1 calc R . . C29 C 1.1819(7) 1.0600(7) 1.3468(6) 0.0414(16) Uani 1 1 d . . . H29A H 1.1998 0.9726 1.3184 0.050 Uiso 1 1 calc R . . H29B H 1.2107 1.1091 1.4391 0.050 Uiso 1 1 calc R . . C30 C 0.6100(7) 0.9721(11) 0.9757(12) 0.068(3) Uani 1 1 d . . . H30A H 0.6033 1.0317 1.0636 0.081 Uiso 1 1 calc R . . H30B H 0.5291 0.9352 0.9271 0.081 Uiso 1 1 calc R . . C31 C 0.3601(7) -0.5103(10) 0.4638(18) 0.107(6) Uani 1 1 d . . . H31A H 0.3859 -0.4896 0.5532 0.128 Uiso 1 1 calc R . . H31B H 0.3904 -0.5904 0.4116 0.128 Uiso 1 1 calc R . . C32 C 0.6864(7) 0.9294(8) 1.2101(9) 0.0500(18) Uani 1 1 d . . . H32A H 0.6605 1.0120 1.2273 0.060 Uiso 1 1 calc R . . H32B H 0.6530 0.9024 1.2650 0.060 Uiso 1 1 calc R . . C33 C -0.1582(9) -0.3886(8) 0.1859(8) 0.065(3) Uani 1 1 d . . . H33A H -0.1963 -0.4378 0.0958 0.078 Uiso 1 1 calc R . . H33B H -0.1683 -0.2992 0.2144 0.078 Uiso 1 1 calc R . . C34 C 0.6396(7) 0.8324(8) 1.0693(8) 0.0505(19) Uani 1 1 d . . . H34A H 0.6671 0.7506 1.0530 0.061 Uiso 1 1 calc R . . H34B H 0.5522 0.8212 1.0542 0.061 Uiso 1 1 calc R . . C35 C 0.145(2) -0.3805(13) 0.1317(16) 0.135(8) Uani 1 1 d . . . H35A H 0.1759 -0.3685 0.0660 0.162 Uiso 1 1 calc R . . H35B H 0.1601 -0.4649 0.1197 0.162 Uiso 1 1 calc R . . C36 C 0.0227(17) -0.3712(15) 0.1198(9) 0.118(7) Uani 1 1 d . . . H36A H -0.0156 -0.4270 0.0308 0.142 Uiso 1 1 calc R . . H36B H 0.0099 -0.2841 0.1396 0.142 Uiso 1 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 0.0262(3) 0.0396(4) 0.0446(4) 0.0199(3) 0.0022(3) 0.0030(3) Ge2 0.0369(4) 0.0324(3) 0.0572(5) 0.0236(3) 0.0066(3) 0.0069(3) Ge3 0.0429(4) 0.0649(5) 0.0473(4) 0.0398(4) 0.0093(3) 0.0064(3) Ge4 0.0309(3) 0.0412(4) 0.0356(4) 0.0080(3) 0.0061(3) 0.0040(3) Ge5 0.0270(3) 0.0439(4) 0.0493(4) 0.0223(3) 0.0099(3) 0.0065(3) K1 0.0361(6) 0.0263(6) 0.0283(6) 0.0151(5) 0.0089(5) 0.0064(5) K2 0.0247(6) 0.0267(5) 0.0237(6) 0.0128(5) 0.0056(5) 0.0046(4) O11 0.026(2) 0.042(2) 0.069(3) 0.034(3) 0.013(2) 0.0102(18) O8 0.033(2) 0.031(2) 0.036(2) 0.0124(19) 0.006(2) 0.0046(18) O5 0.037(2) 0.030(2) 0.035(2) 0.0165(19) 0.011(2) 0.0041(17) O12 0.033(2) 0.039(2) 0.040(3) 0.025(2) 0.014(2) 0.0116(19) O2 0.047(3) 0.033(2) 0.033(2) 0.013(2) 0.017(2) 0.0027(19) O9 0.049(3) 0.126(6) 0.080(5) 0.083(5) 0.033(3) 0.033(4) O10 0.071(4) 0.063(3) 0.028(2) 0.026(2) -0.004(3) -0.019(3) O1 0.047(3) 0.039(2) 0.029(2) 0.021(2) 0.009(2) 0.000(2) O6 0.040(3) 0.063(3) 0.066(3) 0.051(3) 0.018(2) 0.016(2) O3 0.078(4) 0.044(3) 0.028(2) 0.007(2) 0.003(3) 0.030(3) O7 0.035(3) 0.045(3) 0.059(4) -0.010(3) -0.010(3) 0.013(2) O4 0.080(4) 0.034(2) 0.031(2) 0.012(2) 0.008(3) -0.014(2) N1 0.038(3) 0.048(3) 0.026(3) 0.019(3) 0.007(2) 0.010(2) N3 0.029(3) 0.035(3) 0.065(4) 0.028(3) 0.012(3) 0.007(2) N4 0.030(3) 0.033(3) 0.041(3) 0.015(3) -0.003(2) 0.005(2) N2 0.044(3) 0.062(4) 0.054(4) 0.038(3) 0.011(3) -0.002(3) N5 0.048(4) 0.042(3) 0.098(6) 0.030(4) 0.030(4) 0.017(3) N6 0.062(5) 0.194(12) 0.124(9) 0.127(10) 0.029(6) 0.019(6) N7 0.040(3) 0.058(4) 0.055(4) 0.019(3) 0.005(3) -0.002(3) N8 0.078(6) 0.154(11) 0.074(6) 0.061(7) -0.016(6) -0.030(7) C1 0.039(4) 0.042(4) 0.058(5) 0.025(4) -0.019(4) -0.006(3) C2 0.052(4) 0.050(4) 0.054(4) 0.038(4) 0.018(4) 0.020(3) C3 0.033(3) 0.033(3) 0.040(4) 0.016(3) 0.009(3) 0.005(3) C4 0.038(3) 0.052(4) 0.031(3) 0.021(3) 0.004(3) 0.001(3) C5 0.061(4) 0.028(3) 0.052(4) 0.024(3) 0.021(4) 0.014(3) C6 0.034(3) 0.074(5) 0.046(4) 0.036(4) 0.010(3) 0.002(3) C7 0.045(4) 0.043(4) 0.054(4) 0.035(3) 0.022(3) 0.020(3) C8 0.029(3) 0.038(3) 0.049(4) 0.017(3) 0.011(3) 0.005(3) C9 0.044(4) 0.087(6) 0.088(7) 0.067(6) 0.013(4) 0.015(4) C10 0.128(9) 0.026(3) 0.029(4) 0.009(3) 0.010(5) 0.012(4) C11 0.047(4) 0.078(6) 0.038(4) 0.023(4) 0.014(4) 0.033(4) C12 0.067(5) 0.036(3) 0.020(3) 0.009(3) 0.015(3) -0.010(3) C13 0.045(4) 0.021(3) 0.038(4) 0.005(3) 0.008(3) 0.009(3) C14 0.047(4) 0.037(3) 0.033(3) 0.017(3) 0.005(3) -0.006(3) C15 0.026(3) 0.096(7) 0.046(5) 0.027(5) 0.004(3) 0.001(4) C16 0.065(5) 0.036(4) 0.039(4) 0.015(3) 0.026(4) 0.002(3) C17 0.028(3) 0.034(3) 0.059(5) 0.012(3) -0.005(3) 0.007(3) C18 0.045(4) 0.061(4) 0.039(4) 0.026(4) 0.010(3) 0.024(4) C19 0.033(4) 0.080(7) 0.39(3) 0.148(14) 0.066(9) 0.032(5) C20 0.035(3) 0.033(3) 0.058(5) 0.010(3) 0.010(3) 0.011(3) C21 0.091(7) 0.045(4) 0.042(4) 0.017(4) 0.004(5) -0.024(4) C22 0.046(4) 0.044(4) 0.040(4) 0.025(3) 0.005(3) -0.012(3) C23 0.042(4) 0.102(8) 0.049(5) 0.011(5) 0.027(4) -0.024(5) C24 0.064(5) 0.071(5) 0.039(4) 0.017(4) 0.021(4) 0.047(5) C25 0.066(5) 0.090(7) 0.041(4) 0.038(5) -0.011(4) -0.044(5) C26 0.056(5) 0.070(6) 0.086(8) 0.022(6) -0.006(6) -0.011(5) C27 0.063(7) 0.61(5) 0.33(3) 0.43(4) 0.114(13) 0.141(16) C28 0.103(7) 0.039(4) 0.027(3) 0.007(3) 0.010(4) 0.033(4) C29 0.049(4) 0.045(4) 0.027(3) 0.017(3) 0.001(3) 0.002(3) C30 0.037(4) 0.101(7) 0.105(8) 0.081(7) 0.014(5) 0.009(4) C31 0.030(4) 0.072(6) 0.254(18) 0.105(10) 0.029(7) 0.020(4) C32 0.044(4) 0.052(4) 0.066(5) 0.035(4) 0.024(4) 0.005(3) C33 0.091(6) 0.044(4) 0.047(4) 0.027(4) -0.036(5) -0.021(4) C34 0.044(4) 0.059(5) 0.062(5) 0.041(4) 0.009(4) -0.009(3) C35 0.27(2) 0.058(7) 0.116(12) 0.037(7) 0.153(16) 0.025(11) C36 0.191(16) 0.124(11) 0.026(4) 0.039(6) -0.009(7) -0.088(12) _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 Ge2 2.5000(9) . ? Ge1 Ge3 2.5053(11) . ? Ge1 Ge4 2.5119(10) . ? Ge1 Ge5 7.4385(11) 1_655 ? Ge2 Ge5 2.5046(10) . ? Ge2 Ge4 2.6885(11) . ? Ge2 Ge3 2.7039(9) . ? Ge3 Ge5 2.5051(9) . ? Ge3 Ge4 2.6899(11) . ? Ge4 Ge5 2.4950(11) . ? K1 O5 2.791(4) . ? K1 O1 2.817(4) . ? K1 O3 2.818(6) . ? K1 O6 2.851(4) . ? K1 O2 2.875(5) . ? K1 O4 2.902(5) . ? K1 N2 2.990(7) . ? K1 N1 2.994(6) . ? K2 O10 2.735(5) . ? K2 O12 2.769(4) . ? K2 O8 2.780(5) . ? K2 O7 2.793(5) . ? K2 O11 2.821(4) . ? K2 O9 2.852(6) . ? K2 N3 2.955(6) . ? K2 N4 2.988(6) . ? K2 C35 3.521(13) . ? K2 C18 3.523(7) . ? O11 C18 1.413(9) . ? O11 C31 1.424(9) . ? O8 C13 1.429(8) . ? O8 C20 1.434(9) . ? O5 C22 1.422(8) . ? O5 C5 1.437(8) . ? O12 C3 1.419(8) . ? O12 C7 1.434(7) . ? O2 C32 1.414(9) . ? O2 C16 1.432(9) . ? O9 C27 1.377(13) . ? O9 C35 1.42(2) . ? O10 C33 1.408(12) . ? O10 C36 1.415(12) . ? O1 C29 1.432(9) . ? O1 C12 1.435(8) . ? O6 C2 1.434(8) . ? O6 C9 1.456(11) . ? O3 C28 1.426(9) . ? O3 C24 1.433(12) . ? O7 C14 1.421(9) . ? O7 C26 1.523(13) . ? O4 C21 1.403(11) . ? O4 C10 1.450(11) . ? N1 C11 1.461(10) . ? N1 C6 1.483(9) . ? N1 C4 1.484(8) . ? N3 C15 1.438(11) . ? N3 C23 1.457(11) . ? N3 C19 1.458(9) . ? N4 C1 1.469(9) . ? N4 C8 1.481(9) . ? N4 C17 1.481(9) . ? N2 C30 1.473(11) . ? N2 C34 1.488(9) . ? N2 C25 1.503(12) . ? N5 K1 6.743(8) 1_545 ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N6 K1 6.673(12) 1_544 ? N6 H6C 0.8900 . ? N6 H6D 0.8900 . ? N6 H6E 0.8900 . ? N7 K1 6.950(8) 1_544 ? N7 H7C 0.8900 . ? N7 H7D 0.8900 . ? N7 H7E 0.8900 . ? N8 K1 5.533(13) 1_544 ? N8 H8C 0.8900 . ? N8 H8D 0.8900 . ? N8 H8E 0.8900 . ? C1 C33 1.512(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C5 1.478(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.533(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C29 1.511(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C22 1.502(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C18 1.498(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C30 1.518(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C28 1.446(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C24 1.511(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C16 1.484(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.467(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C26 1.338(15) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C20 1.514(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C31 1.283(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C25 1.509(15) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C27 1.287(18) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C34 1.521(12) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.38(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? 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 Ge2 Ge1 Ge3 65.39(3) . . ? Ge2 Ge1 Ge4 64.88(3) . . ? Ge3 Ge1 Ge4 64.84(3) . . ? Ge2 Ge1 Ge5 146.06(3) . 1_655 ? Ge3 Ge1 Ge5 146.94(2) . 1_655 ? Ge4 Ge1 Ge5 128.04(3) . 1_655 ? Ge1 Ge2 Ge5 103.26(3) . . ? Ge1 Ge2 Ge4 57.77(3) . . ? Ge5 Ge2 Ge4 57.30(3) . . ? Ge1 Ge2 Ge3 57.40(3) . . ? Ge5 Ge2 Ge3 57.34(3) . . ? Ge4 Ge2 Ge3 59.85(3) . . ? Ge5 Ge3 Ge1 103.09(3) . . ? Ge5 Ge3 Ge4 57.27(3) . . ? Ge1 Ge3 Ge4 57.70(3) . . ? Ge5 Ge3 Ge2 57.33(3) . . ? Ge1 Ge3 Ge2 57.21(3) . . ? Ge4 Ge3 Ge2 59.79(3) . . ? Ge5 Ge4 Ge1 103.19(4) . . ? Ge5 Ge4 Ge2 57.64(3) . . ? Ge1 Ge4 Ge2 57.35(3) . . ? Ge5 Ge4 Ge3 57.64(3) . . ? Ge1 Ge4 Ge3 57.46(3) . . ? Ge2 Ge4 Ge3 60.36(3) . . ? Ge4 Ge5 Ge2 65.06(3) . . ? Ge4 Ge5 Ge3 65.09(3) . . ? Ge2 Ge5 Ge3 65.33(3) . . ? O5 K1 O1 95.42(13) . . ? O5 K1 O3 97.25(17) . . ? O1 K1 O3 100.80(15) . . ? O5 K1 O6 60.65(14) . . ? O1 K1 O6 115.62(16) . . ? O3 K1 O6 137.96(16) . . ? O5 K1 O2 134.63(14) . . ? O1 K1 O2 59.78(14) . . ? O3 K1 O2 122.92(16) . . ? O6 K1 O2 94.43(15) . . ? O5 K1 O4 118.33(14) . . ? O1 K1 O4 141.00(14) . . ? O3 K1 O4 58.56(18) . . ? O6 K1 O4 98.66(17) . . ? O2 K1 O4 101.54(15) . . ? O5 K1 N2 120.35(15) . . ? O1 K1 N2 120.05(17) . . ? O3 K1 N2 118.1(2) . . ? O6 K1 N2 61.02(16) . . ? O2 K1 N2 60.97(16) . . ? O4 K1 N2 60.5(2) . . ? O5 K1 N1 61.21(14) . . ? O1 K1 N1 60.15(15) . . ? O3 K1 N1 60.24(17) . . ? O6 K1 N1 120.73(15) . . ? O2 K1 N1 118.88(15) . . ? O4 K1 N1 118.02(18) . . ? N2 K1 N1 178.14(18) . . ? O10 K2 O12 98.73(14) . . ? O10 K2 O8 98.27(17) . . ? O12 K2 O8 97.72(14) . . ? O10 K2 O7 144.47(18) . . ? O12 K2 O7 111.67(19) . . ? O8 K2 O7 60.83(14) . . ? O10 K2 O11 111.72(19) . . ? O12 K2 O11 61.15(13) . . ? O8 K2 O11 144.96(15) . . ? O7 K2 O11 99.18(15) . . ? O10 K2 O9 61.20(18) . . ? O12 K2 O9 147.8(2) . . ? O8 K2 O9 109.38(18) . . ? O7 K2 O9 96.9(2) . . ? O11 K2 O9 100.97(18) . . ? O10 K2 N3 118.51(19) . . ? O12 K2 N3 119.41(14) . . ? O8 K2 N3 119.64(15) . . ? O7 K2 N3 61.77(18) . . ? O11 K2 N3 61.25(14) . . ? O9 K2 N3 61.30(17) . . ? O10 K2 N4 60.49(18) . . ? O12 K2 N4 60.93(13) . . ? O8 K2 N4 61.04(14) . . ? O7 K2 N4 119.12(17) . . ? O11 K2 N4 118.73(14) . . ? O9 K2 N4 117.86(16) . . ? N3 K2 N4 178.98(19) . . ? O10 K2 C35 41.9(4) . . ? O12 K2 C35 126.8(3) . . ? O8 K2 C35 118.1(3) . . ? O7 K2 C35 119.7(4) . . ? O11 K2 C35 96.7(3) . . ? O9 K2 C35 22.8(3) . . ? N3 K2 C35 76.9(4) . . ? N4 K2 C35 102.1(4) . . ? O10 K2 C18 120.67(18) . . ? O12 K2 C18 42.70(15) . . ? O8 K2 C18 124.37(16) . . ? O7 K2 C18 94.55(19) . . ? O11 K2 C18 22.43(17) . . ? O9 K2 C18 123.39(19) . . ? N3 K2 C18 76.77(17) . . ? N4 K2 C18 103.52(17) . . ? C35 K2 C18 117.4(3) . . ? C18 O11 C31 108.7(8) . . ? C18 O11 K2 107.9(4) . . ? C31 O11 K2 117.2(4) . . ? C13 O8 C20 111.1(5) . . ? C13 O8 K2 116.3(4) . . ? C20 O8 K2 119.9(4) . . ? C22 O5 C5 111.2(5) . . ? C22 O5 K1 118.8(3) . . ? C5 O5 K1 115.7(4) . . ? C3 O12 C7 110.8(5) . . ? C3 O12 K2 119.5(3) . . ? C7 O12 K2 116.7(4) . . ? C32 O2 C16 112.7(6) . . ? C32 O2 K1 117.2(4) . . ? C16 O2 K1 111.1(4) . . ? C27 O9 C35 111.2(16) . . ? C27 O9 K2 115.6(5) . . ? C35 O9 K2 106.0(6) . . ? C33 O10 C36 111.5(9) . . ? C33 O10 K2 121.6(5) . . ? C36 O10 K2 114.4(6) . . ? C29 O1 C12 110.8(5) . . ? C29 O1 K1 118.2(4) . . ? C12 O1 K1 117.8(4) . . ? C2 O6 C9 110.0(5) . . ? C2 O6 K1 112.9(4) . . ? C9 O6 K1 114.8(4) . . ? C28 O3 C24 110.0(7) . . ? C28 O3 K1 118.8(5) . . ? C24 O3 K1 120.4(4) . . ? C14 O7 C26 102.7(7) . . ? C14 O7 K2 110.4(4) . . ? C26 O7 K2 113.5(5) . . ? C21 O4 C10 109.6(7) . . ? C21 O4 K1 116.6(5) . . ? C10 O4 K1 113.4(4) . . ? C11 N1 C6 110.5(6) . . ? C11 N1 C4 109.6(5) . . ? C6 N1 C4 109.2(6) . . ? C11 N1 K1 109.2(5) . . ? C6 N1 K1 107.7(4) . . ? C4 N1 K1 110.6(4) . . ? C15 N3 C23 110.4(7) . . ? C15 N3 C19 110.2(10) . . ? C23 N3 C19 109.6(10) . . ? C15 N3 K2 108.1(5) . . ? C23 N3 K2 109.8(5) . . ? C19 N3 K2 108.7(4) . . ? C1 N4 C8 110.7(5) . . ? C1 N4 C17 110.6(5) . . ? C8 N4 C17 109.3(6) . . ? C1 N4 K2 109.0(5) . . ? C8 N4 K2 108.8(3) . . ? C17 N4 K2 108.4(4) . . ? C30 N2 C34 108.7(7) . . ? C30 N2 C25 110.2(7) . . ? C34 N2 C25 109.7(6) . . ? C30 N2 K1 110.2(5) . . ? C34 N2 K1 109.1(4) . . ? C25 N2 K1 109.0(5) . . ? K1 N5 H5C 109.5 1_545 . ? K1 N5 H5D 109.5 1_545 . ? H5C N5 H5D 109.5 . . ? K1 N5 H5E 109.5 1_545 . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? K1 N6 H6C 109.5 1_544 . ? K1 N6 H6D 109.5 1_544 . ? H6C N6 H6D 109.5 . . ? K1 N6 H6E 109.5 1_544 . ? H6C N6 H6E 109.5 . . ? H6D N6 H6E 109.5 . . ? K1 N7 H7C 109.5 1_544 . ? K1 N7 H7D 109.5 1_544 . ? H7C N7 H7D 109.5 . . ? K1 N7 H7E 109.5 1_544 . ? H7C N7 H7E 109.5 . . ? H7D N7 H7E 109.5 . . ? K1 N8 H8C 109.5 1_544 . ? K1 N8 H8D 109.5 1_544 . ? H8C N8 H8D 109.5 . . ? K1 N8 H8E 109.5 1_544 . ? H8C N8 H8E 109.5 . . ? H8D N8 H8E 109.5 . . ? N4 C1 C33 113.6(6) . . ? N4 C1 H1A 108.8 . . ? C33 C1 H1A 108.8 . . ? N4 C1 H1B 108.8 . . ? C33 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O6 C2 C5 110.4(5) . . ? O6 C2 H2A 109.6 . . ? C5 C2 H2A 109.6 . . ? O6 C2 H2B 109.6 . . ? C5 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O12 C3 C8 108.6(5) . . ? O12 C3 H3A 110.0 . . ? C8 C3 H3A 110.0 . . ? O12 C3 H3B 110.0 . . ? C8 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N1 C4 C29 112.7(6) . . ? N1 C4 H4A 109.0 . . ? C29 C4 H4A 109.0 . . ? N1 C4 H4B 109.0 . . ? C29 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O5 C5 C2 109.9(5) . . ? O5 C5 H5A 109.7 . . ? C2 C5 H5A 109.7 . . ? O5 C5 H5B 109.7 . . ? C2 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N1 C6 C22 114.4(6) . . ? N1 C6 H6A 108.7 . . ? C22 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C22 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O12 C7 C18 109.6(6) . . ? O12 C7 H7A 109.8 . . ? C18 C7 H7A 109.8 . . ? O12 C7 H7B 109.8 . . ? C18 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C3 112.7(6) . . ? N4 C8 H8A 109.1 . . ? C3 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C3 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? O6 C9 C30 108.6(7) . . ? O6 C9 H9A 110.0 . . ? C30 C9 H9A 110.0 . . ? O6 C9 H9B 110.0 . . ? C30 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C28 C10 O4 110.6(6) . . ? C28 C10 H10A 109.5 . . ? O4 C10 H10A 109.5 . . ? C28 C10 H10B 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N1 C11 C24 115.1(6) . . ? N1 C11 H11A 108.5 . . ? C24 C11 H11A 108.5 . . ? N1 C11 H11B 108.5 . . ? C24 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O1 C12 C16 108.8(5) . . ? O1 C12 H12A 109.9 . . ? C16 C12 H12A 109.9 . . ? O1 C12 H12B 109.9 . . ? C16 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O8 C13 C14 109.9(6) . . ? O8 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? O8 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O7 C14 C13 109.8(5) . . ? O7 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? O7 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C26 C15 N3 121.5(7) . . ? C26 C15 H15A 106.9 . . ? N3 C15 H15A 106.9 . . ? C26 C15 H15B 106.9 . . ? N3 C15 H15B 106.9 . . ? H15A C15 H15B 106.7 . . ? O2 C16 C12 110.3(6) . . ? O2 C16 H16A 109.6 . . ? C12 C16 H16A 109.6 . . ? O2 C16 H16B 109.6 . . ? C12 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N4 C17 C20 114.6(5) . . ? N4 C17 H17A 108.6 . . ? C20 C17 H17A 108.6 . . ? N4 C17 H17B 108.6 . . ? C20 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? O11 C18 C7 109.2(5) . . ? O11 C18 K2 49.6(3) . . ? C7 C18 K2 82.6(3) . . ? O11 C18 H18A 109.8 . . ? C7 C18 H18A 109.8 . . ? K2 C18 H18A 81.4 . . ? O11 C18 H18B 109.8 . . ? C7 C18 H18B 109.8 . . ? K2 C18 H18B 159.4 . . ? H18A C18 H18B 108.3 . . ? C31 C19 N3 126.8(9) . . ? C31 C19 H19A 105.6 . . ? N3 C19 H19A 105.6 . . ? C31 C19 H19B 105.6 . . ? N3 C19 H19B 105.6 . . ? H19A C19 H19B 106.1 . . ? O8 C20 C17 108.5(7) . . ? O8 C20 H20A 110.0 . . ? C17 C20 H20A 110.0 . . ? O8 C20 H20B 110.0 . . ? C17 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O4 C21 C25 107.9(6) . . ? O4 C21 H21A 110.1 . . ? C25 C21 H21A 110.1 . . ? O4 C21 H21B 110.1 . . ? C25 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? O5 C22 C6 109.8(6) . . ? O5 C22 H22A 109.7 . . ? C6 C22 H22A 109.7 . . ? O5 C22 H22B 109.7 . . ? C6 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C27 C23 N3 125.7(8) . . ? C27 C23 H23A 105.9 . . ? N3 C23 H23A 105.9 . . ? C27 C23 H23B 105.9 . . ? N3 C23 H23B 105.9 . . ? H23A C23 H23B 106.2 . . ? O3 C24 C11 108.7(7) . . ? O3 C24 H24A 110.0 . . ? C11 C24 H24A 110.0 . . ? O3 C24 H24B 110.0 . . ? C11 C24 H24B 110.0 . . ? H24A C24 H24B 108.3 . . ? N2 C25 C21 116.1(7) . . ? N2 C25 H25A 108.3 . . ? C21 C25 H25A 108.3 . . ? N2 C25 H25B 108.3 . . ? C21 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C15 C26 O7 111.0(8) . . ? C15 C26 H26A 109.4 . . ? O7 C26 H26A 109.4 . . ? C15 C26 H26B 109.4 . . ? O7 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C23 C27 O9 125.3(11) . . ? C23 C27 H27A 106.0 . . ? O9 C27 H27A 106.0 . . ? C23 C27 H27B 106.0 . . ? O9 C27 H27B 106.0 . . ? H27A C27 H27B 106.3 . . ? O3 C28 C10 109.3(8) . . ? O3 C28 H28A 109.8 . . ? C10 C28 H28A 109.8 . . ? O3 C28 H28B 109.8 . . ? C10 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? O1 C29 C4 108.9(5) . . ? O1 C29 H29A 109.9 . . ? C4 C29 H29A 109.9 . . ? O1 C29 H29B 109.9 . . ? C4 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? N2 C30 C9 113.4(8) . . ? N2 C30 H30A 108.9 . . ? C9 C30 H30A 108.9 . . ? N2 C30 H30B 108.9 . . ? C9 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C19 C31 O11 119.9(9) . . ? C19 C31 H31A 107.3 . . ? O11 C31 H31A 107.3 . . ? C19 C31 H31B 107.3 . . ? O11 C31 H31B 107.3 . . ? H31A C31 H31B 106.9 . . ? O2 C32 C34 110.6(7) . . ? O2 C32 H32A 109.5 . . ? C34 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? C34 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? O10 C33 C1 109.5(5) . . ? O10 C33 H33A 109.8 . . ? C1 C33 H33A 109.8 . . ? O10 C33 H33B 109.8 . . ? C1 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? N2 C34 C32 114.0(6) . . ? N2 C34 H34A 108.7 . . ? C32 C34 H34A 108.7 . . ? N2 C34 H34B 108.7 . . ? C32 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C36 C35 O9 109.7(11) . . ? C36 C35 K2 80.4(6) . . ? O9 C35 K2 51.1(4) . . ? C36 C35 H35A 109.7 . . ? O9 C35 H35A 109.7 . . ? K2 C35 H35A 160.9 . . ? C36 C35 H35B 109.7 . . ? O9 C35 H35B 109.7 . . ? K2 C35 H35B 82.2 . . ? H35A C35 H35B 108.2 . . ? C35 C36 O10 114.5(12) . . ? C35 C36 H36A 108.6 . . ? O10 C36 H36A 108.6 . . ? C35 C36 H36B 108.6 . . ? O10 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.313 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.073 _chemical_name_common ; Bis(potassium-(4,7,13,1621,24-Hexaoxa-1,10- diazabicyclo(8.8.8)hexacosane))-nonagermanid - ammonia(1/4) ; #======================================================================== data_Rb_crypt_Ge5 _database_code_depnum_ccdc_archive 'CCDC 615431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[rubidium-(4,7,13,1621,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)]- nonagermanid - ammonia(1/4) ; _chemical_formula_moiety 'C36 H84 Ge5 N8 O12 Rb2' _chemical_formula_sum 'C36 H84 Ge5 N8 O12 Rb2' _chemical_formula_weight 1355.00 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' 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' Rb Rb -0.9393 2.9676 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3169(15) _cell_length_b 12.3333(15) _cell_length_c 20.915(3) _cell_angle_alpha 89.183(13) _cell_angle_beta 83.60(2) _cell_angle_gamma 78.266(15) _cell_volume 2840.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.88 _cell_measurement_theta_max 51.84 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 4.374 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.216 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details '(A.L.Spek, Platon 2004)' _exptl_special_details ; crystal mounting in perfluorether (T. Kottke, D. Stalke, J. Appl. Crystallogr. 26, 1993, p. 615) ; _diffrn_ambient_temperature 123(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 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method Phi _diffrn_standards_number 10249 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7 _diffrn_standards_decay_% ? _diffrn_reflns_number 36788 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.92 _reflns_number_total 10249 _reflns_number_gt 7057 _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^)+(0.0576P)^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 10249 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _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 Rb1 Rb 0.42558(4) 0.26530(4) 0.43756(2) 0.02180(11) Uani 1 1 d . . . Rb2 Rb 0.43050(4) -0.24280(4) 0.91848(2) 0.02322(11) Uani 1 1 d . . . Ge3 Ge -0.15446(5) 0.28026(5) 0.77364(3) 0.03275(14) Uani 1 1 d . . . Ge4 Ge -0.12438(6) 0.06454(5) 0.74163(3) 0.03692(16) Uani 1 1 d . . . Ge2 Ge -0.14553(5) 0.21830(5) 0.64869(3) 0.03429(15) Uani 1 1 d . . . Ge1 Ge 0.03495(5) 0.17702(6) 0.71080(3) 0.03722(16) Uani 1 1 d . . . Ge5 Ge -0.31971(5) 0.20407(5) 0.73228(3) 0.03482(15) Uani 1 1 d . . . O1 O 0.2397(3) 0.3759(3) 0.35929(18) 0.0307(8) Uani 1 1 d . . . O2 O 0.4907(3) 0.3938(3) 0.32679(15) 0.0261(8) Uani 1 1 d . . . O3 O 0.3207(3) 0.0668(3) 0.45187(16) 0.0282(8) Uani 1 1 d . . . O4 O 0.5549(3) 0.0606(3) 0.37901(17) 0.0281(8) Uani 1 1 d . . . O5 O 0.3428(3) 0.3719(3) 0.56318(16) 0.0312(8) Uani 1 1 d . . . O6 O 0.5955(3) 0.3152(3) 0.51939(16) 0.0319(9) Uani 1 1 d . . . O7 O 0.3147(3) -0.1105(3) 0.81685(17) 0.0312(9) Uani 1 1 d . . . O8 O 0.5622(3) -0.1142(3) 0.83529(16) 0.0322(9) Uani 1 1 d . . . O9 O 0.3203(4) -0.4377(4) 0.91511(18) 0.0412(10) Uani 1 1 d . . . O10 O 0.5770(4) -0.4600(3) 0.89080(17) 0.0339(9) Uani 1 1 d . . . O11 O 0.2754(3) -0.1172(3) 1.02484(17) 0.0347(9) Uani 1 1 d . . . O12 O 0.5315(3) -0.1980(3) 1.03274(16) 0.0290(8) Uani 1 1 d . . . N1 N 0.1620(4) 0.2870(4) 0.4906(2) 0.0309(10) Uani 1 1 d . . . N2 N 0.6911(4) 0.2436(4) 0.38561(19) 0.0262(9) Uani 1 1 d . . . N3 N 0.1585(4) -0.2079(5) 0.9195(2) 0.0460(14) Uani 1 1 d . . . N4 N 0.7035(4) -0.2803(4) 0.9183(2) 0.0292(10) Uani 1 1 d . . . N5 N 0.0819(6) 0.4903(5) 0.7581(3) 0.0570(16) Uani 1 1 d . . . H5C H 0.0278 0.4665 0.7862 0.086 Uiso 1 1 calc R . . H5D H 0.1289 0.4328 0.7366 0.086 Uiso 1 1 calc R . . H5E H 0.0433 0.5366 0.7307 0.086 Uiso 1 1 calc R . . N6 N -0.0503(6) -0.2527(7) 0.7219(4) 0.0582(17) Uani 1 1 d . . . H6C H -0.037(9) -0.193(9) 0.735(5) 0.09(4) Uiso 1 1 d . . . H6D H -0.110(7) -0.273(6) 0.702(3) 0.06(2) Uiso 1 1 d . . . H6E H 0.016(15) -0.287(14) 0.747(7) 0.21(7) Uiso 1 1 d . . . N7 N 0.3086(6) 0.2742(6) 0.7840(3) 0.0502(15) Uani 1 1 d . . . H7C H 0.303(5) 0.336(5) 0.765(3) 0.024(15) Uiso 1 1 d . . . H7D H 0.388(6) 0.260(5) 0.770(3) 0.040(18) Uiso 1 1 d . . . H7E H 0.288(7) 0.238(7) 0.758(3) 0.05(2) Uiso 1 1 d . . . N8 N 0.0689(7) 0.2993(12) 0.8923(3) 0.143(5) Uani 1 1 d . . . H8C H 0.0501 0.3164 0.8527 0.215 Uiso 1 1 calc R . . H8D H 0.1234 0.2360 0.8912 0.215 Uiso 1 1 calc R . . H8E H 0.0998 0.3530 0.9078 0.215 Uiso 1 1 calc R . . C1 C 0.1899(5) 0.0873(5) 0.4573(3) 0.0361(14) Uani 1 1 d . . . H1A H 0.1620 0.0197 0.4695 0.043 Uiso 1 1 calc R . . H1B H 0.1620 0.1109 0.4161 0.043 Uiso 1 1 calc R . . C2 C 0.1318(5) 0.4250(5) 0.4003(3) 0.0360(13) Uani 1 1 d . . . H2A H 0.0700 0.4616 0.3742 0.043 Uiso 1 1 calc R . . H2B H 0.1502 0.4803 0.4281 0.043 Uiso 1 1 calc R . . C3 C 0.2353(5) 0.3394(5) 0.5933(2) 0.0361(13) Uani 1 1 d . . . H3A H 0.2065 0.3815 0.6328 0.043 Uiso 1 1 calc R . . H3B H 0.2534 0.2614 0.6041 0.043 Uiso 1 1 calc R . . C4 C 0.2770(5) 0.4568(4) 0.3159(3) 0.0301(12) Uani 1 1 d . . . H4A H 0.2783 0.5234 0.3397 0.036 Uiso 1 1 calc R . . H4B H 0.2192 0.4761 0.2846 0.036 Uiso 1 1 calc R . . C5 C 0.1382(5) 0.1767(5) 0.5078(3) 0.0367(13) Uani 1 1 d . . . H5A H 0.0511 0.1821 0.5156 0.044 Uiso 1 1 calc R . . H5B H 0.1720 0.1543 0.5477 0.044 Uiso 1 1 calc R . . C6 C 0.1387(5) 0.3604(5) 0.5480(3) 0.0377(13) Uani 1 1 d . . . H6A H 0.0622 0.3525 0.5716 0.045 Uiso 1 1 calc R . . H6B H 0.1294 0.4365 0.5336 0.045 Uiso 1 1 calc R . . C7 C 0.7114(5) 0.3331(5) 0.4905(3) 0.0351(13) Uani 1 1 d . . . H7A H 0.7664 0.3299 0.5232 0.042 Uiso 1 1 calc R . . H7B H 0.7016 0.4059 0.4711 0.042 Uiso 1 1 calc R . . C8 C 0.3294(5) -0.1322(5) 1.0843(2) 0.0328(12) Uani 1 1 d . . . H8A H 0.3288 -0.2064 1.1001 0.039 Uiso 1 1 calc R . . H8B H 0.2820 -0.0800 1.1163 0.039 Uiso 1 1 calc R . . C9 C 0.7631(5) 0.2457(5) 0.4400(3) 0.0332(13) Uani 1 1 d . . . H9A H 0.8433 0.2561 0.4230 0.040 Uiso 1 1 calc R . . H9B H 0.7730 0.1739 0.4605 0.040 Uiso 1 1 calc R . . C10 C 0.5083(5) -0.0357(5) 0.3995(3) 0.0358(13) Uani 1 1 d . . . H10A H 0.5318 -0.0576 0.4418 0.043 Uiso 1 1 calc R . . H10B H 0.5422 -0.0965 0.3698 0.043 Uiso 1 1 calc R . . C11 C 0.6577(5) -0.1886(5) 1.0277(3) 0.0345(13) Uani 1 1 d . . . H11A H 0.6854 -0.1927 1.0700 0.041 Uiso 1 1 calc R . . H11B H 0.6668 -0.1179 1.0090 0.041 Uiso 1 1 calc R . . C12 C 0.4581(5) -0.1146(5) 1.0747(2) 0.0345(13) Uani 1 1 d . . . H12A H 0.4594 -0.0422 1.0563 0.041 Uiso 1 1 calc R . . H12B H 0.4904 -0.1175 1.1158 0.041 Uiso 1 1 calc R . . C13 C 0.5492(5) 0.3892(4) 0.5717(2) 0.0327(13) Uani 1 1 d . . . H13A H 0.5299 0.4644 0.5561 0.039 Uiso 1 1 calc R . . H13B H 0.6098 0.3856 0.6014 0.039 Uiso 1 1 calc R . . C14 C 0.7597(5) -0.3868(5) 0.8863(3) 0.0401(15) Uani 1 1 d . . . H14A H 0.8441 -0.4056 0.8945 0.048 Uiso 1 1 calc R . . H14B H 0.7582 -0.3775 0.8403 0.048 Uiso 1 1 calc R . . C15 C 0.7328(5) 0.1387(5) 0.3496(2) 0.0306(12) Uani 1 1 d . . . H15A H 0.8209 0.1203 0.3457 0.037 Uiso 1 1 calc R . . H15B H 0.7084 0.1490 0.3066 0.037 Uiso 1 1 calc R . . C16 C 0.7467(5) -0.1880(5) 0.8826(3) 0.0387(14) Uani 1 1 d . . . H16A H 0.8341 -0.2088 0.8722 0.046 Uiso 1 1 calc R . . H16B H 0.7300 -0.1234 0.9105 0.046 Uiso 1 1 calc R . . C17 C 0.0841(5) 0.3371(5) 0.4411(3) 0.0351(13) Uani 1 1 d . . . H17A H 0.0045 0.3699 0.4623 0.042 Uiso 1 1 calc R . . H17B H 0.0742 0.2787 0.4129 0.042 Uiso 1 1 calc R . . C18 C 0.6839(5) 0.0423(5) 0.3805(3) 0.0301(12) Uani 1 1 d . . . H18A H 0.7226 -0.0257 0.3574 0.036 Uiso 1 1 calc R . . H18B H 0.7026 0.0345 0.4246 0.036 Uiso 1 1 calc R . . C19 C 0.6894(5) -0.1566(5) 0.8207(3) 0.0373(14) Uani 1 1 d . . . H19A H 0.7272 -0.1010 0.7982 0.045 Uiso 1 1 calc R . . H19B H 0.7024 -0.2212 0.7929 0.045 Uiso 1 1 calc R . . C20 C 0.4368(5) 0.3578(5) 0.6056(2) 0.0324(12) Uani 1 1 d . . . H20A H 0.4555 0.2812 0.6192 0.039 Uiso 1 1 calc R . . H20B H 0.4087 0.4039 0.6437 0.039 Uiso 1 1 calc R . . C21 C 0.5076(6) -0.0686(5) 0.7786(3) 0.0376(14) Uani 1 1 d . . . H21A H 0.5179 -0.1261 0.7461 0.045 Uiso 1 1 calc R . . H21B H 0.5473 -0.0104 0.7609 0.045 Uiso 1 1 calc R . . C22 C 0.4012(5) 0.4125(5) 0.2816(2) 0.0317(13) Uani 1 1 d . . . H22A H 0.4012 0.3435 0.2599 0.038 Uiso 1 1 calc R . . H22B H 0.4217 0.4649 0.2494 0.038 Uiso 1 1 calc R . . C23 C 0.7021(5) 0.3400(5) 0.3434(3) 0.0321(12) Uani 1 1 d . . . H23A H 0.7832 0.3271 0.3206 0.039 Uiso 1 1 calc R . . H23B H 0.6925 0.4054 0.3702 0.039 Uiso 1 1 calc R . . C24 C 0.3727(6) -0.0107(5) 0.4021(3) 0.0388(14) Uani 1 1 d . . . H24A H 0.3492 0.0191 0.3611 0.047 Uiso 1 1 calc R . . H24B H 0.3424 -0.0785 0.4096 0.047 Uiso 1 1 calc R . . C25 C 0.3766(6) -0.0233(5) 0.7964(3) 0.0384(14) Uani 1 1 d . . . H25A H 0.3665 0.0306 0.8310 0.046 Uiso 1 1 calc R . . H25B H 0.3415 0.0139 0.7597 0.046 Uiso 1 1 calc R . . C26 C 0.3974(7) -0.5279(5) 0.8800(3) 0.0476(17) Uani 1 1 d . . . H26A H 0.4053 -0.5098 0.8346 0.057 Uiso 1 1 calc R . . H26B H 0.3612 -0.5929 0.8849 0.057 Uiso 1 1 calc R . . C27 C 0.6103(5) 0.3629(5) 0.2944(2) 0.0307(12) Uani 1 1 d . . . H27A H 0.6277 0.4220 0.2661 0.037 Uiso 1 1 calc R . . H27B H 0.6163 0.2971 0.2683 0.037 Uiso 1 1 calc R . . C28 C 0.7323(5) -0.2819(5) 0.9857(3) 0.0375(14) Uani 1 1 d . . . H28A H 0.8174 -0.2793 0.9854 0.045 Uiso 1 1 calc R . . H28B H 0.7206 -0.3516 1.0048 0.045 Uiso 1 1 calc R . . C29 C 0.1582(5) -0.1467(6) 1.0342(3) 0.0451(16) Uani 1 1 d . . . H29A H 0.1069 -0.1006 1.0678 0.054 Uiso 1 1 calc R . . H29B H 0.1669 -0.2233 1.0474 0.054 Uiso 1 1 calc R . . C30 C 0.5197(7) -0.5530(5) 0.9030(3) 0.0462(16) Uani 1 1 d . . . H30A H 0.5121 -0.5682 0.9488 0.055 Uiso 1 1 calc R . . H30B H 0.5689 -0.6181 0.8808 0.055 Uiso 1 1 calc R . . C31 C 0.1228(6) -0.3170(7) 0.9305(3) 0.057(2) Uani 1 1 d . . . H31A H 0.0400 -0.3103 0.9203 0.068 Uiso 1 1 calc R . . H31B H 0.1236 -0.3345 0.9758 0.068 Uiso 1 1 calc R . . C32 C 0.1246(5) -0.1639(7) 0.8560(3) 0.0525(19) Uani 1 1 d . . . H32A H 0.0372 -0.1384 0.8591 0.063 Uiso 1 1 calc R . . H32B H 0.1467 -0.2235 0.8244 0.063 Uiso 1 1 calc R . . C33 C 0.1855(5) -0.0694(6) 0.8329(3) 0.0499(18) Uani 1 1 d . . . H33A H 0.1503 -0.0359 0.7953 0.060 Uiso 1 1 calc R . . H33B H 0.1721 -0.0131 0.8663 0.060 Uiso 1 1 calc R . . C34 C 0.0998(5) -0.1305(7) 0.9712(3) 0.057(2) Uani 1 1 d . . . H34A H 0.0156 -0.1374 0.9800 0.068 Uiso 1 1 calc R . . H34B H 0.1002 -0.0557 0.9563 0.068 Uiso 1 1 calc R . . C35 C 0.6998(6) -0.4830(5) 0.9072(3) 0.0431(16) Uani 1 1 d . . . H35A H 0.7448 -0.5505 0.8857 0.052 Uiso 1 1 calc R . . H35B H 0.6998 -0.4934 0.9532 0.052 Uiso 1 1 calc R . . C36 C 0.2014(7) -0.4110(7) 0.8923(3) 0.059(2) Uani 1 1 d . . . H36A H 0.1640 -0.4752 0.8963 0.071 Uiso 1 1 calc R . . H36B H 0.2098 -0.3911 0.8472 0.071 Uiso 1 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 Rb1 0.0217(2) 0.0183(2) 0.0239(2) 0.00133(19) -0.00345(18) -0.00010(18) Rb2 0.0209(2) 0.0236(3) 0.0245(2) 0.00061(19) -0.00443(18) -0.00203(19) Ge3 0.0356(3) 0.0302(3) 0.0320(3) -0.0054(3) -0.0045(2) -0.0048(3) Ge4 0.0379(3) 0.0221(3) 0.0493(3) 0.0094(3) -0.0043(3) -0.0036(3) Ge2 0.0363(3) 0.0408(4) 0.0242(3) 0.0051(3) -0.0036(2) -0.0043(3) Ge1 0.0266(3) 0.0407(4) 0.0423(3) 0.0025(3) -0.0024(3) -0.0029(3) Ge5 0.0255(3) 0.0421(4) 0.0366(3) 0.0038(3) -0.0047(2) -0.0059(3) O1 0.0274(19) 0.0190(19) 0.044(2) 0.0056(17) -0.0069(17) 0.0006(16) O2 0.0267(18) 0.029(2) 0.0206(16) 0.0039(15) -0.0061(14) 0.0000(16) O3 0.0302(19) 0.026(2) 0.0281(17) -0.0043(16) -0.0023(15) -0.0044(16) O4 0.0279(18) 0.0170(19) 0.0369(19) -0.0009(16) -0.0031(16) 0.0010(15) O5 0.037(2) 0.028(2) 0.0258(17) 0.0014(16) 0.0022(16) -0.0023(17) O6 0.041(2) 0.027(2) 0.0283(18) -0.0043(16) -0.0101(17) -0.0054(18) O7 0.0298(19) 0.027(2) 0.0339(19) 0.0009(17) -0.0094(16) 0.0035(16) O8 0.035(2) 0.038(2) 0.0261(17) 0.0095(17) -0.0099(16) -0.0126(18) O9 0.047(2) 0.047(3) 0.036(2) -0.006(2) -0.0059(19) -0.025(2) O10 0.043(2) 0.021(2) 0.0347(19) 0.0038(17) -0.0072(18) 0.0007(18) O11 0.0293(19) 0.042(2) 0.0278(18) 0.0015(17) -0.0006(16) 0.0040(18) O12 0.0236(18) 0.034(2) 0.0299(18) -0.0040(17) -0.0037(15) -0.0065(16) N1 0.027(2) 0.027(3) 0.036(2) 0.006(2) 0.0003(19) -0.001(2) N2 0.027(2) 0.024(2) 0.026(2) 0.0044(19) -0.0041(18) -0.0002(19) N3 0.024(2) 0.073(4) 0.037(3) -0.004(3) -0.002(2) 0.000(3) N4 0.021(2) 0.038(3) 0.029(2) 0.001(2) -0.0049(18) -0.004(2) N5 0.059(4) 0.048(4) 0.066(4) 0.006(3) -0.017(3) -0.010(3) N6 0.049(4) 0.052(4) 0.072(4) -0.008(4) -0.011(3) -0.003(3) N7 0.045(4) 0.049(4) 0.059(4) -0.006(3) -0.009(3) -0.013(3) N8 0.065(5) 0.324(16) 0.056(4) -0.008(7) -0.026(4) -0.062(7) C1 0.034(3) 0.034(3) 0.043(3) 0.010(3) -0.008(3) -0.014(3) C2 0.024(3) 0.032(3) 0.048(3) 0.004(3) -0.003(2) 0.003(2) C3 0.039(3) 0.035(3) 0.028(3) -0.003(2) 0.008(2) 0.001(3) C4 0.031(3) 0.023(3) 0.035(3) 0.008(2) -0.010(2) -0.002(2) C5 0.033(3) 0.029(3) 0.045(3) 0.004(3) 0.006(3) -0.005(3) C6 0.038(3) 0.025(3) 0.044(3) 0.000(3) 0.009(3) -0.001(3) C7 0.034(3) 0.037(3) 0.039(3) 0.004(3) -0.017(3) -0.010(3) C8 0.037(3) 0.034(3) 0.024(2) -0.002(2) -0.002(2) -0.001(3) C9 0.023(3) 0.034(3) 0.042(3) -0.001(3) -0.008(2) -0.001(2) C10 0.047(3) 0.014(3) 0.042(3) -0.004(2) 0.007(3) -0.002(3) C11 0.028(3) 0.046(4) 0.034(3) 0.005(3) -0.012(2) -0.014(3) C12 0.043(3) 0.034(3) 0.027(2) -0.004(2) -0.003(2) -0.007(3) C13 0.046(3) 0.025(3) 0.028(3) 0.001(2) -0.014(2) -0.005(3) C14 0.027(3) 0.053(4) 0.034(3) -0.001(3) -0.001(2) 0.006(3) C15 0.028(3) 0.032(3) 0.030(3) 0.004(2) -0.004(2) -0.002(2) C16 0.030(3) 0.057(4) 0.034(3) 0.006(3) -0.008(2) -0.018(3) C17 0.022(3) 0.034(3) 0.046(3) 0.007(3) -0.004(2) 0.000(2) C18 0.031(3) 0.024(3) 0.031(3) 0.000(2) -0.001(2) 0.001(2) C19 0.034(3) 0.050(4) 0.034(3) 0.012(3) -0.004(2) -0.025(3) C20 0.044(3) 0.026(3) 0.024(2) -0.001(2) -0.006(2) -0.001(3) C21 0.056(4) 0.036(3) 0.028(3) 0.014(2) -0.017(3) -0.022(3) C22 0.038(3) 0.032(3) 0.027(2) 0.005(2) -0.015(2) -0.006(3) C23 0.031(3) 0.030(3) 0.036(3) 0.007(2) -0.002(2) -0.009(2) C24 0.052(4) 0.030(3) 0.036(3) -0.003(3) 0.001(3) -0.016(3) C25 0.049(3) 0.027(3) 0.041(3) 0.005(3) -0.023(3) -0.005(3) C26 0.084(5) 0.041(4) 0.028(3) -0.001(3) -0.004(3) -0.038(4) C27 0.035(3) 0.027(3) 0.027(2) 0.004(2) 0.001(2) -0.002(2) C28 0.024(3) 0.051(4) 0.035(3) -0.001(3) -0.007(2) 0.001(3) C29 0.021(3) 0.070(5) 0.039(3) 0.002(3) 0.004(2) -0.003(3) C30 0.081(5) 0.022(3) 0.036(3) 0.005(3) -0.007(3) -0.010(3) C31 0.033(3) 0.092(6) 0.054(4) 0.008(4) -0.012(3) -0.031(4) C32 0.025(3) 0.084(6) 0.047(3) -0.001(4) -0.012(3) -0.002(3) C33 0.036(3) 0.067(5) 0.038(3) 0.002(3) -0.015(3) 0.013(3) C34 0.025(3) 0.091(6) 0.049(4) -0.006(4) -0.001(3) 0.002(3) C35 0.043(3) 0.036(4) 0.039(3) 0.002(3) -0.004(3) 0.019(3) C36 0.061(4) 0.084(6) 0.046(4) 0.000(4) -0.010(3) -0.045(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 Rb1 O4 2.864(4) . ? Rb1 O6 2.873(3) . ? Rb1 O2 2.900(3) . ? Rb1 O1 2.916(3) . ? Rb1 O5 2.926(4) . ? Rb1 O3 2.928(4) . ? Rb1 N1 3.024(4) . ? Rb1 N2 3.039(4) . ? Rb1 C2 3.662(5) . ? Rb1 C24 3.674(6) . ? Rb1 C18 3.686(6) . ? Rb1 C10 3.714(6) . ? Rb2 O8 2.841(4) . ? Rb2 O12 2.868(3) . ? Rb2 O10 2.878(4) . ? Rb2 O7 2.924(3) . ? Rb2 O11 2.924(4) . ? Rb2 O9 2.930(4) . ? Rb2 N3 3.017(5) . ? Rb2 N4 3.029(4) . ? Rb2 C29 3.700(6) . ? Rb2 C25 3.700(5) . ? Rb2 C19 3.710(5) . ? Rb2 C8 3.717(5) . ? Ge3 Ge5 2.4956(9) . ? Ge3 Ge1 2.5006(11) . ? Ge3 Ge4 2.6970(10) . ? Ge3 Ge2 2.7187(9) . ? Ge4 Ge1 2.5148(10) . ? Ge4 Ge5 2.5348(9) . ? Ge4 Ge2 2.6918(9) . ? Ge2 Ge1 2.5035(9) . ? Ge2 Ge5 2.5173(10) . ? Ge2 Rb1 6.8264(13) 2_566 ? Ge1 Ge5 7.4416(13) 1_655 ? O1 C4 1.435(6) . ? O1 C2 1.440(7) . ? O2 C27 1.424(6) . ? O2 C22 1.444(5) . ? O3 C24 1.417(7) . ? O3 C1 1.443(6) . ? O4 C18 1.435(6) . ? O4 C10 1.436(6) . ? O5 C3 1.434(7) . ? O5 C20 1.443(6) . ? O6 C13 1.418(7) . ? O6 C7 1.439(7) . ? O7 C25 1.433(7) . ? O7 C33 1.450(7) . ? O8 C19 1.428(7) . ? O8 C21 1.451(5) . ? O9 C26 1.423(8) . ? O9 C36 1.450(8) . ? O10 C30 1.435(7) . ? O10 C35 1.439(7) . ? O11 C29 1.438(7) . ? O11 C8 1.439(6) . ? O12 C12 1.426(7) . ? O12 C11 1.449(6) . ? N1 C5 1.472(7) . ? N1 C6 1.480(8) . ? N1 C17 1.482(6) . ? N2 C15 1.470(7) . ? N2 C9 1.475(6) . ? N2 C23 1.488(6) . ? N3 C34 1.461(9) . ? N3 C32 1.488(7) . ? N3 C31 1.490(10) . ? N4 C14 1.472(8) . ? N4 C28 1.480(6) . ? N4 C16 1.488(7) . ? N5 Rb2 6.797(6) 1_565 ? N5 H5C 0.8900 . ? N5 H5D 0.8900 . ? N5 H5E 0.8900 . ? N6 H6C 0.83(11) . ? N6 H6D 0.90(8) . ? N6 H6E 0.98(15) . ? N7 H7C 0.85(6) . ? N7 H7D 0.89(7) . ? N7 H7E 0.80(8) . ? N8 Rb2 6.680(8) 2_557 ? N8 H8C 0.8900 . ? N8 H8D 0.8900 . ? N8 H8E 0.8900 . ? C1 C5 1.520(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C17 1.517(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C6 1.508(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C22 1.503(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.503(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C12 1.507(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C24 1.497(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C28 1.509(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C20 1.504(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C35 1.518(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C18 1.517(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C19 1.522(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C25 1.482(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C27 1.523(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C30 1.488(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.532(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.491(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.518(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? 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 O4 Rb1 O6 101.89(10) . . ? O4 Rb1 O2 92.87(10) . . ? O6 Rb1 O2 98.26(10) . . ? O4 Rb1 O1 110.89(10) . . ? O6 Rb1 O1 140.58(11) . . ? O2 Rb1 O1 59.79(10) . . ? O4 Rb1 O5 141.94(9) . . ? O6 Rb1 O5 58.90(11) . . ? O2 Rb1 O5 120.65(10) . . ? O1 Rb1 O5 102.07(10) . . ? O4 Rb1 O3 59.93(10) . . ? O6 Rb1 O3 123.16(9) . . ? O2 Rb1 O3 132.89(10) . . ? O1 Rb1 O3 92.73(10) . . ? O5 Rb1 O3 101.00(10) . . ? O4 Rb1 N1 119.35(12) . . ? O6 Rb1 N1 119.33(12) . . ? O2 Rb1 N1 120.03(10) . . ? O1 Rb1 N1 61.70(11) . . ? O5 Rb1 N1 61.25(12) . . ? O3 Rb1 N1 60.55(11) . . ? O4 Rb1 N2 60.86(11) . . ? O6 Rb1 N2 60.11(11) . . ? O2 Rb1 N2 60.38(9) . . ? O1 Rb1 N2 118.80(10) . . ? O5 Rb1 N2 118.23(11) . . ? O3 Rb1 N2 119.53(11) . . ? N1 Rb1 N2 179.43(11) . . ? O4 Rb1 C2 126.73(12) . . ? O6 Rb1 C2 131.14(13) . . ? O2 Rb1 C2 76.89(11) . . ? O1 Rb1 C2 21.73(12) . . ? O5 Rb1 C2 81.62(12) . . ? O3 Rb1 C2 89.48(12) . . ? N1 Rb1 C2 43.15(11) . . ? N2 Rb1 C2 137.26(11) . . ? O4 Rb1 C24 40.76(12) . . ? O6 Rb1 C24 126.56(12) . . ? O2 Rb1 C24 115.76(11) . . ? O1 Rb1 C24 92.84(12) . . ? O5 Rb1 C24 121.50(12) . . ? O3 Rb1 C24 21.17(12) . . ? N1 Rb1 C24 78.58(14) . . ? N2 Rb1 C24 101.62(13) . . ? C2 Rb1 C24 97.39(14) . . ? O4 Rb1 C18 20.87(11) . . ? O6 Rb1 C18 82.40(11) . . ? O2 Rb1 C18 88.37(11) . . ? O1 Rb1 C18 125.05(11) . . ? O5 Rb1 C18 132.84(10) . . ? O3 Rb1 C18 77.15(11) . . ? N1 Rb1 C18 137.70(12) . . ? N2 Rb1 C18 42.38(12) . . ? C2 Rb1 C18 144.53(13) . . ? C24 Rb1 C18 60.17(13) . . ? O4 Rb1 C10 20.44(12) . . ? O6 Rb1 C10 107.85(12) . . ? O2 Rb1 C10 110.71(12) . . ? O1 Rb1 C10 110.52(12) . . ? O5 Rb1 C10 127.97(11) . . ? O3 Rb1 C10 40.10(12) . . ? N1 Rb1 C10 100.49(13) . . ? N2 Rb1 C10 79.63(13) . . ? C2 Rb1 C10 119.45(14) . . ? C24 Rb1 C10 23.38(13) . . ? C18 Rb1 C10 37.39(13) . . ? O8 Rb2 O12 95.83(10) . . ? O8 Rb2 O10 99.95(11) . . ? O12 Rb2 O10 97.88(10) . . ? O8 Rb2 O7 59.47(10) . . ? O12 Rb2 O7 135.93(11) . . ? O10 Rb2 O7 120.64(10) . . ? O8 Rb2 O11 114.18(12) . . ? O12 Rb2 O11 59.84(10) . . ? O10 Rb2 O11 139.95(10) . . ? O7 Rb2 O11 95.38(10) . . ? O8 Rb2 O9 140.18(11) . . ? O12 Rb2 O9 118.77(10) . . ? O10 Rb2 O9 58.78(12) . . ? O7 Rb2 O9 100.32(11) . . ? O11 Rb2 O9 100.77(12) . . ? O8 Rb2 N3 119.42(13) . . ? O12 Rb2 N3 119.63(12) . . ? O10 Rb2 N3 119.29(15) . . ? O7 Rb2 N3 61.07(12) . . ? O11 Rb2 N3 61.29(13) . . ? O9 Rb2 N3 61.50(15) . . ? O8 Rb2 N4 61.21(10) . . ? O12 Rb2 N4 60.23(11) . . ? O10 Rb2 N4 60.23(12) . . ? O7 Rb2 N4 119.51(11) . . ? O11 Rb2 N4 118.72(11) . . ? O9 Rb2 N4 117.94(13) . . ? N3 Rb2 N4 179.35(14) . . ? O8 Rb2 C29 128.42(14) . . ? O12 Rb2 C29 76.98(11) . . ? O10 Rb2 C29 131.55(14) . . ? O7 Rb2 C29 90.60(12) . . ? O11 Rb2 C29 21.20(13) . . ? O9 Rb2 C29 81.33(15) . . ? N3 Rb2 C29 42.65(13) . . ? N4 Rb2 C29 137.21(12) . . ? O8 Rb2 C25 40.28(12) . . ? O12 Rb2 C25 119.08(12) . . ? O10 Rb2 C25 123.62(13) . . ? O7 Rb2 C25 21.10(11) . . ? O11 Rb2 C25 96.34(13) . . ? O9 Rb2 C25 120.54(11) . . ? N3 Rb2 C25 79.15(14) . . ? N4 Rb2 C25 101.49(13) . . ? C29 Rb2 C25 99.11(14) . . ? O8 Rb2 C19 20.10(12) . . ? O12 Rb2 C19 89.12(11) . . ? O10 Rb2 C19 82.15(13) . . ? O7 Rb2 C19 76.90(11) . . ? O11 Rb2 C19 126.06(13) . . ? O9 Rb2 C19 133.17(14) . . ? N3 Rb2 C19 137.95(13) . . ? N4 Rb2 C19 42.64(11) . . ? C29 Rb2 C19 144.54(16) . . ? C25 Rb2 C19 59.44(13) . . ? O8 Rb2 C8 116.37(12) . . ? O12 Rb2 C8 40.28(11) . . ? O10 Rb2 C8 123.50(11) . . ? O7 Rb2 C8 114.97(11) . . ? O11 Rb2 C8 20.99(10) . . ? O9 Rb2 C8 103.15(12) . . ? N3 Rb2 C8 79.43(13) . . ? N4 Rb2 C8 100.45(12) . . ? C29 Rb2 C8 36.81(12) . . ? C25 Rb2 C8 111.71(13) . . ? C19 Rb2 C8 120.62(13) . . ? Ge5 Ge3 Ge1 103.90(3) . . ? Ge5 Ge3 Ge4 58.29(3) . . ? Ge1 Ge3 Ge4 57.72(3) . . ? Ge5 Ge3 Ge2 57.54(3) . . ? Ge1 Ge3 Ge2 57.14(3) . . ? Ge4 Ge3 Ge2 59.61(2) . . ? Ge1 Ge4 Ge5 102.37(3) . . ? Ge1 Ge4 Ge2 57.36(2) . . ? Ge5 Ge4 Ge2 57.49(3) . . ? Ge1 Ge4 Ge3 57.22(3) . . ? Ge5 Ge4 Ge3 56.88(3) . . ? Ge2 Ge4 Ge3 60.60(2) . . ? Ge1 Ge2 Ge5 103.19(3) . . ? Ge1 Ge2 Ge4 57.76(3) . . ? Ge5 Ge2 Ge4 58.12(3) . . ? Ge1 Ge2 Ge3 57.04(3) . . ? Ge5 Ge2 Ge3 56.77(3) . . ? Ge4 Ge2 Ge3 59.80(2) . . ? Ge1 Ge2 Rb1 125.09(3) . 2_566 ? Ge5 Ge2 Rb1 91.74(3) . 2_566 ? Ge4 Ge2 Rb1 146.48(3) . 2_566 ? Ge3 Ge2 Rb1 92.58(3) . 2_566 ? Ge3 Ge1 Ge2 65.81(3) . . ? Ge3 Ge1 Ge4 65.06(3) . . ? Ge2 Ge1 Ge4 64.88(3) . . ? Ge3 Ge1 Ge5 129.82(3) . 1_655 ? Ge2 Ge1 Ge5 148.44(2) . 1_655 ? Ge4 Ge1 Ge5 143.77(2) . 1_655 ? Ge3 Ge5 Ge2 65.68(3) . . ? Ge3 Ge5 Ge4 64.84(3) . . ? Ge2 Ge5 Ge4 64.39(3) . . ? C4 O1 C2 110.4(4) . . ? C4 O1 Rb1 114.6(3) . . ? C2 O1 Rb1 109.7(3) . . ? C27 O2 C22 111.1(4) . . ? C27 O2 Rb1 117.9(2) . . ? C22 O2 Rb1 113.5(3) . . ? C24 O3 C1 111.2(4) . . ? C24 O3 Rb1 110.6(3) . . ? C1 O3 Rb1 115.0(3) . . ? C18 O4 C10 111.4(4) . . ? C18 O4 Rb1 113.8(3) . . ? C10 O4 Rb1 115.4(3) . . ? C3 O5 C20 111.6(4) . . ? C3 O5 Rb1 112.4(3) . . ? C20 O5 Rb1 113.1(3) . . ? C13 O6 C7 111.2(4) . . ? C13 O6 Rb1 117.6(3) . . ? C7 O6 Rb1 118.8(3) . . ? C25 O7 C33 111.8(5) . . ? C25 O7 Rb2 111.6(2) . . ? C33 O7 Rb2 113.6(3) . . ? C19 O8 C21 111.3(4) . . ? C19 O8 Rb2 116.8(3) . . ? C21 O8 Rb2 117.2(3) . . ? C26 O9 C36 111.6(5) . . ? C26 O9 Rb2 112.8(3) . . ? C36 O9 Rb2 111.9(4) . . ? C30 O10 C35 111.7(4) . . ? C30 O10 Rb2 117.5(4) . . ? C35 O10 Rb2 118.5(3) . . ? C29 O11 C8 109.0(4) . . ? C29 O11 Rb2 111.4(4) . . ? C8 O11 Rb2 112.3(3) . . ? C12 O12 C11 110.8(4) . . ? C12 O12 Rb2 116.0(3) . . ? C11 O12 Rb2 118.8(3) . . ? C5 N1 C6 110.7(4) . . ? C5 N1 C17 110.0(4) . . ? C6 N1 C17 109.6(4) . . ? C5 N1 Rb1 109.4(3) . . ? C6 N1 Rb1 108.0(3) . . ? C17 N1 Rb1 109.0(3) . . ? C15 N2 C9 110.1(4) . . ? C15 N2 C23 111.0(4) . . ? C9 N2 C23 109.1(4) . . ? C15 N2 Rb1 109.4(3) . . ? C9 N2 Rb1 109.0(3) . . ? C23 N2 Rb1 108.2(3) . . ? C34 N3 C32 110.7(5) . . ? C34 N3 C31 110.1(6) . . ? C32 N3 C31 109.5(5) . . ? C34 N3 Rb2 109.3(3) . . ? C32 N3 Rb2 109.0(3) . . ? C31 N3 Rb2 108.1(4) . . ? C14 N4 C28 110.1(4) . . ? C14 N4 C16 110.1(5) . . ? C28 N4 C16 110.5(4) . . ? C14 N4 Rb2 109.2(3) . . ? C28 N4 Rb2 108.8(3) . . ? C16 N4 Rb2 108.2(3) . . ? Rb2 N5 H5C 109.5 1_565 . ? Rb2 N5 H5D 109.5 1_565 . ? H5C N5 H5D 109.5 . . ? Rb2 N5 H5E 109.5 1_565 . ? H5C N5 H5E 109.5 . . ? H5D N5 H5E 109.5 . . ? H6C N6 H6D 135(8) . . ? H6C N6 H6E 84(10) . . ? H6D N6 H6E 139(10) . . ? H7C N7 H7D 88(6) . . ? H7C N7 H7E 101(6) . . ? H7D N7 H7E 97(7) . . ? Rb2 N8 H8C 109.5 2_557 . ? Rb2 N8 H8D 109.5 2_557 . ? H8C N8 H8D 109.5 . . ? Rb2 N8 H8E 109.5 2_557 . ? H8C N8 H8E 109.5 . . ? H8D N8 H8E 109.5 . . ? O3 C1 C5 109.3(4) . . ? O3 C1 H1A 109.8 . . ? C5 C1 H1A 109.8 . . ? O3 C1 H1B 109.8 . . ? C5 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? O1 C2 C17 110.5(5) . . ? O1 C2 Rb1 48.6(2) . . ? C17 C2 Rb1 82.5(3) . . ? O1 C2 H2A 109.6 . . ? C17 C2 H2A 109.6 . . ? Rb1 C2 H2A 158.1 . . ? O1 C2 H2B 109.6 . . ? C17 C2 H2B 109.6 . . ? Rb1 C2 H2B 83.5 . . ? H2A C2 H2B 108.1 . . ? O5 C3 C6 109.2(4) . . ? O5 C3 Rb1 46.7(2) . . ? C6 C3 Rb1 79.8(3) . . ? O5 C3 H3A 109.8 . . ? C6 C3 H3A 109.8 . . ? Rb1 C3 H3A 156.1 . . ? O5 C3 H3B 109.8 . . ? C6 C3 H3B 109.8 . . ? Rb1 C3 H3B 87.6 . . ? H3A C3 H3B 108.3 . . ? O1 C4 C22 110.6(4) . . ? O1 C4 Rb1 45.01(19) . . ? C22 C4 Rb1 77.3(2) . . ? O1 C4 H4A 109.5 . . ? C22 C4 H4A 109.5 . . ? Rb1 C4 H4A 94.2 . . ? O1 C4 H4B 109.5 . . ? C22 C4 H4B 109.5 . . ? Rb1 C4 H4B 152.0 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C1 114.6(5) . . ? N1 C5 H5A 108.6 . . ? C1 C5 H5A 108.6 . . ? N1 C5 H5B 108.6 . . ? C1 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N1 C6 C3 115.4(5) . . ? N1 C6 H6A 108.4 . . ? C3 C6 H6A 108.4 . . ? N1 C6 H6B 108.4 . . ? C3 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? O6 C7 C9 109.4(4) . . ? O6 C7 H7A 109.8 . . ? C9 C7 H7A 109.8 . . ? O6 C7 H7B 109.8 . . ? C9 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O11 C8 C12 110.6(4) . . ? O11 C8 Rb2 46.7(2) . . ? C12 C8 Rb2 78.4(3) . . ? O11 C8 H8A 109.5 . . ? C12 C8 H8A 109.5 . . ? Rb2 C8 H8A 90.5 . . ? O11 C8 H8B 109.5 . . ? C12 C8 H8B 109.5 . . ? Rb2 C8 H8B 154.9 . . ? H8A C8 H8B 108.1 . . ? N2 C9 C7 115.9(4) . . ? N2 C9 H9A 108.3 . . ? C7 C9 H9A 108.3 . . ? N2 C9 H9B 108.3 . . ? C7 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? O4 C10 C24 109.8(4) . . ? O4 C10 Rb1 44.2(2) . . ? C24 C10 Rb1 76.8(3) . . ? O4 C10 H10A 109.7 . . ? C24 C10 H10A 109.7 . . ? Rb1 C10 H10A 95.2 . . ? O4 C10 H10B 109.7 . . ? C24 C10 H10B 109.7 . . ? Rb1 C10 H10B 151.0 . . ? H10A C10 H10B 108.2 . . ? O12 C11 C28 108.7(4) . . ? O12 C11 H11A 110.0 . . ? C28 C11 H11A 110.0 . . ? O12 C11 H11B 110.0 . . ? C28 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? O12 C12 C8 110.0(5) . . ? O12 C12 Rb2 43.9(2) . . ? C8 C12 Rb2 78.2(3) . . ? O12 C12 H12A 109.7 . . ? C8 C12 H12A 109.7 . . ? Rb2 C12 H12A 94.0 . . ? O12 C12 H12B 109.7 . . ? C8 C12 H12B 109.7 . . ? Rb2 C12 H12B 151.4 . . ? H12A C12 H12B 108.2 . . ? O6 C13 C20 109.2(4) . . ? O6 C13 Rb1 42.8(2) . . ? C20 C13 Rb1 78.0(3) . . ? O6 C13 H13A 109.8 . . ? C20 C13 H13A 109.8 . . ? Rb1 C13 H13A 94.7 . . ? O6 C13 H13B 109.8 . . ? C20 C13 H13B 109.8 . . ? Rb1 C13 H13B 150.4 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C35 115.1(5) . . ? N4 C14 H14A 108.5 . . ? C35 C14 H14A 108.5 . . ? N4 C14 H14B 108.5 . . ? C35 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N2 C15 C18 113.9(4) . . ? N2 C15 H15A 108.8 . . ? C18 C15 H15A 108.8 . . ? N2 C15 H15B 108.8 . . ? C18 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N4 C16 C19 114.4(4) . . ? N4 C16 H16A 108.6 . . ? C19 C16 H16A 108.6 . . ? N4 C16 H16B 108.6 . . ? C19 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N1 C17 C2 115.0(4) . . ? N1 C17 H17A 108.5 . . ? C2 C17 H17A 108.5 . . ? N1 C17 H17B 108.5 . . ? C2 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? O4 C18 C15 110.1(4) . . ? O4 C18 Rb1 45.3(2) . . ? C15 C18 Rb1 82.1(3) . . ? O4 C18 H18A 109.6 . . ? C15 C18 H18A 109.6 . . ? Rb1 C18 H18A 154.7 . . ? O4 C18 H18B 109.6 . . ? C15 C18 H18B 109.6 . . ? Rb1 C18 H18B 87.5 . . ? H18A C18 H18B 108.2 . . ? O8 C19 C16 109.8(4) . . ? O8 C19 Rb2 43.1(2) . . ? C16 C19 Rb2 80.4(3) . . ? O8 C19 H19A 109.7 . . ? C16 C19 H19A 109.7 . . ? Rb2 C19 H19A 151.7 . . ? O8 C19 H19B 109.7 . . ? C16 C19 H19B 109.7 . . ? Rb2 C19 H19B 92.0 . . ? H19A C19 H19B 108.2 . . ? O5 C20 C13 110.1(4) . . ? O5 C20 Rb1 46.1(2) . . ? C13 C20 Rb1 78.8(3) . . ? O5 C20 H20A 109.6 . . ? C13 C20 H20A 109.6 . . ? Rb1 C20 H20A 90.2 . . ? O5 C20 H20B 109.6 . . ? C13 C20 H20B 109.6 . . ? Rb1 C20 H20B 154.7 . . ? H20A C20 H20B 108.2 . . ? O8 C21 C25 109.3(4) . . ? O8 C21 Rb2 42.5(2) . . ? C25 C21 Rb2 77.2(3) . . ? O8 C21 H21A 109.8 . . ? C25 C21 H21A 109.8 . . ? Rb2 C21 H21A 96.3 . . ? O8 C21 H21B 109.8 . . ? C25 C21 H21B 109.8 . . ? Rb2 C21 H21B 149.4 . . ? H21A C21 H21B 108.3 . . ? O2 C22 C4 110.4(4) . . ? O2 C22 Rb1 45.7(2) . . ? C4 C22 Rb1 79.4(3) . . ? O2 C22 H22A 109.6 . . ? C4 C22 H22A 109.6 . . ? Rb1 C22 H22A 90.4 . . ? O2 C22 H22B 109.6 . . ? C4 C22 H22B 109.6 . . ? Rb1 C22 H22B 154.2 . . ? H22A C22 H22B 108.1 . . ? N2 C23 C27 114.4(4) . . ? N2 C23 H23A 108.7 . . ? C27 C23 H23A 108.7 . . ? N2 C23 H23B 108.7 . . ? C27 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? O3 C24 C10 110.4(5) . . ? O3 C24 Rb1 48.3(2) . . ? C10 C24 Rb1 79.8(3) . . ? O3 C24 H24A 109.6 . . ? C10 C24 H24A 109.6 . . ? Rb1 C24 H24A 86.8 . . ? O3 C24 H24B 109.6 . . ? C10 C24 H24B 109.6 . . ? Rb1 C24 H24B 157.4 . . ? H24A C24 H24B 108.1 . . ? O7 C25 C21 110.4(4) . . ? O7 C25 Rb2 47.27(19) . . ? C21 C25 Rb2 79.8(3) . . ? O7 C25 H25A 109.6 . . ? C21 C25 H25A 109.6 . . ? Rb2 C25 H25A 87.9 . . ? O7 C25 H25B 109.6 . . ? C21 C25 H25B 109.6 . . ? Rb2 C25 H25B 156.3 . . ? H25A C25 H25B 108.1 . . ? O9 C26 C30 111.0(5) . . ? O9 C26 Rb2 46.6(3) . . ? C30 C26 Rb2 80.1(3) . . ? O9 C26 H26A 109.4 . . ? C30 C26 H26A 109.4 . . ? Rb2 C26 H26A 89.0 . . ? O9 C26 H26B 109.4 . . ? C30 C26 H26B 109.4 . . ? Rb2 C26 H26B 155.2 . . ? H26A C26 H26B 108.0 . . ? O2 C27 C23 109.8(4) . . ? O2 C27 H27A 109.7 . . ? C23 C27 H27A 109.7 . . ? O2 C27 H27B 109.7 . . ? C23 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N4 C28 C11 114.9(4) . . ? N4 C28 H28A 108.5 . . ? C11 C28 H28A 108.5 . . ? N4 C28 H28B 108.5 . . ? C11 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? O11 C29 C34 109.4(5) . . ? O11 C29 Rb2 47.4(3) . . ? C34 C29 Rb2 80.5(3) . . ? O11 C29 H29A 109.8 . . ? C34 C29 H29A 109.8 . . ? Rb2 C29 H29A 157.0 . . ? O11 C29 H29B 109.8 . . ? C34 C29 H29B 109.8 . . ? Rb2 C29 H29B 86.2 . . ? H29A C29 H29B 108.3 . . ? O10 C30 C26 109.3(4) . . ? O10 C30 H30A 109.8 . . ? C26 C30 H30A 109.8 . . ? O10 C30 H30B 109.8 . . ? C26 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? N3 C31 C36 115.0(6) . . ? N3 C31 H31A 108.5 . . ? C36 C31 H31A 108.5 . . ? N3 C31 H31B 108.5 . . ? C36 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? N3 C32 C33 113.1(5) . . ? N3 C32 H32A 109.0 . . ? C33 C32 H32A 109.0 . . ? N3 C32 H32B 109.0 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? O7 C33 C32 109.9(5) . . ? O7 C33 Rb2 45.6(2) . . ? C32 C33 Rb2 79.3(3) . . ? O7 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? Rb2 C33 H33A 154.3 . . ? O7 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? Rb2 C33 H33B 90.2 . . ? H33A C33 H33B 108.2 . . ? N3 C34 C29 115.0(5) . . ? N3 C34 H34A 108.5 . . ? C29 C34 H34A 108.5 . . ? N3 C34 H34B 108.5 . . ? C29 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? O10 C35 C14 109.2(4) . . ? O10 C35 H35A 109.9 . . ? C14 C35 H35A 109.9 . . ? O10 C35 H35B 109.9 . . ? C14 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? O9 C36 C31 110.2(5) . . ? O9 C36 Rb2 46.9(3) . . ? C31 C36 Rb2 79.8(4) . . ? O9 C36 H36A 109.6 . . ? C31 C36 H36A 109.6 . . ? Rb2 C36 H36A 156.0 . . ? O9 C36 H36B 109.6 . . ? C31 C36 H36B 109.6 . . ? Rb2 C36 H36B 88.2 . . ? H36A C36 H36B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.875 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.118 _chemical_name_common ; Bis(rubidium-(4,7,13,1621,24-Hexaoxa-1,10- diazabicyclo(8.8.8)hexacosane))-nonagermanid - ammonia(1/4) ;