Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' #============================================================================== _audit_creation_date 10-06-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Ian P. Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; _publ_contact_author_email rothwell@purdue.edu _publ_contact_author_fax 1(765)4940239 _publ_contact_author_phone 1(765)4945473 _publ_requested_category ? _publ_requested_coeditor_name ? _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Charles S. Weinert' ; Department of Chemistry Purdue University 560 Oval Drive W. Lafayette IN 47907 USA ; 'Ian P. Rothwell' ; Department of Chemistry Purdue University 560 Oval Drive W. Lafayette IN 47907 USA ; 'Phillip E. Fanwick' ; Department of Chemistry Purdue University 560 Oval Drive W. Lafayette IN 47907 USA ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G, Polidori, G. Spagna R. (1999). J. Appl. Cryst., 32, 115-119 Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; #============================================================================== data_SW1213 _database_code_CSD 203289 _audit_creation_date 16-12-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C60 H45 Ge1 O3 Rb1' _chemical_formula_moiety 'C54 H39 Ge1 O3 Rb1,C6 H6' _chemical_formula_structural ? _chemical_formula_weight 972.09 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 15.6217(3) _cell_length_b 17.1706(4) _cell_length_c 17.7554(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.6623(11) _cell_angle_gamma 90.00 _cell_volume 4680.37(18) _cell_measurement_reflns_used 31114 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.695 _cell_measurement_temperature 150 _exptl_crystal_F_000 1992 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6510 _exptl_absorpt_correction_T_max 0.8987 _diffrn_reflns_number 31114 _diffrn_measured_fraction_theta_max 0.9966 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 0.9966 _reflns_number_total 8230 _reflns_number_gt 7072 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_max 20 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.077 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 8196 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0296P)^2^+3.4935P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.28 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Rb Rb 0.223783(17) 0.187510(16) 0.385837(15) 0.02492(9) Uani 1 1 d . . . Ge Ge -0.295852(18) -0.476558(17) 0.212394(16) 0.02081(9) Uani 1 1 d . . . O(1) O -0.36468(11) -0.41026(11) 0.13662(10) 0.0223(4) Uani 1 1 d . . . O(2) O -0.20902(12) -0.47964(11) 0.14794(10) 0.0252(4) Uani 1 1 d . . . O(3) O -0.24013(11) -0.38212(11) 0.25723(10) 0.0221(4) Uani 1 1 d . . . C(11) C -0.45016(17) -0.39945(16) 0.13924(14) 0.0213(6) Uani 1 1 d . . . C(12) C -0.48231(18) -0.32308(17) 0.13896(15) 0.0239(6) Uani 1 1 d . . . C(13) C -0.57013(19) -0.31049(19) 0.14174(16) 0.0304(7) Uani 1 1 d . . . C(14) C -0.62549(19) -0.37247(19) 0.14599(17) 0.0333(7) Uani 1 1 d . . . C(15) C -0.59370(19) -0.44795(18) 0.14654(16) 0.0294(7) Uani 1 1 d . . . C(16) C -0.50710(17) -0.46313(17) 0.14082(15) 0.0241(6) Uani 1 1 d . . . C(21) C -0.18412(18) -0.54402(17) 0.11405(16) 0.0247(6) Uani 1 1 d . . . C(22) C -0.17438(18) -0.53796(18) 0.03680(16) 0.0281(7) Uani 1 1 d . . . C(23) C -0.1471(2) -0.6029(2) 0.00012(18) 0.0387(8) Uani 1 1 d . . . C(24) C -0.1303(2) -0.6734(2) 0.0377(2) 0.0457(9) Uani 1 1 d . . . C(25) C -0.1378(2) -0.67888(18) 0.11365(19) 0.0380(8) Uani 1 1 d . . . C(26) C -0.16342(18) -0.61518(17) 0.15341(16) 0.0271(7) Uani 1 1 d . . . C(31) C -0.19223(18) -0.38048(15) 0.32879(15) 0.0215(6) Uani 1 1 d . . . C(32) C -0.10645(18) -0.35159(17) 0.33908(15) 0.0243(6) Uani 1 1 d . . . C(33) C -0.05487(19) -0.35002(18) 0.41222(16) 0.0298(7) Uani 1 1 d . . . C(34) C -0.0876(2) -0.37626(19) 0.47502(16) 0.0329(7) Uani 1 1 d . . . C(35) C -0.17184(19) -0.40276(18) 0.46545(16) 0.0299(7) Uani 1 1 d . . . C(36) C -0.22601(18) -0.40527(16) 0.39359(15) 0.0224(6) Uani 1 1 d . . . C(121) C -0.42454(17) -0.25478(16) 0.13289(15) 0.0221(6) Uani 1 1 d . . . C(122) C -0.4238(2) -0.22077(18) 0.06188(17) 0.0326(7) Uani 1 1 d . . . C(123) C -0.3730(2) -0.1560(2) 0.05547(18) 0.0384(8) Uani 1 1 d . . . C(124) C -0.32154(19) -0.12406(18) 0.11956(17) 0.0308(7) Uani 1 1 d . . . C(125) C -0.32075(19) -0.15698(17) 0.19071(17) 0.0299(7) Uani 1 1 d . . . C(126) C -0.37212(19) -0.22192(18) 0.19706(16) 0.0290(7) Uani 1 1 d . . . C(161) C -0.47813(17) -0.54531(17) 0.13498(15) 0.0247(6) Uani 1 1 d . . . C(162) C -0.49368(19) -0.60207(18) 0.18680(17) 0.0317(7) Uani 1 1 d . . . C(163) C -0.4661(2) -0.67817(19) 0.18028(19) 0.0386(8) Uani 1 1 d . . . C(164) C -0.4227(2) -0.69882(19) 0.12215(19) 0.0383(8) Uani 1 1 d . . . C(165) C -0.4077(2) -0.64350(19) 0.06961(18) 0.0347(7) Uani 1 1 d . . . C(166) C -0.43566(19) -0.56738(18) 0.07552(16) 0.0289(7) Uani 1 1 d . . . C(221) C -0.18985(19) -0.46255(18) -0.00508(15) 0.0281(7) Uani 1 1 d . . . C(222) C -0.2730(2) -0.43105(18) -0.02608(16) 0.0298(7) Uani 1 1 d . . . C(223) C -0.2862(2) -0.36122(19) -0.06592(17) 0.0371(8) Uani 1 1 d . . . C(224) C -0.2158(3) -0.3211(2) -0.08465(18) 0.0453(9) Uani 1 1 d . . . C(225) C -0.1332(2) -0.3519(2) -0.0642(2) 0.0504(10) Uani 1 1 d . . . C(226) C -0.1206(2) -0.4224(2) -0.02573(18) 0.0404(8) Uani 1 1 d . . . C(261) C -0.16685(18) -0.62466(17) 0.23649(17) 0.0273(7) Uani 1 1 d . . . C(262) C -0.12476(19) -0.57201(17) 0.29127(17) 0.0288(7) Uani 1 1 d . . . C(263) C -0.1262(2) -0.58181(19) 0.36861(17) 0.0349(8) Uani 1 1 d . . . C(264) C -0.1692(2) -0.6440(2) 0.39290(19) 0.0413(8) Uani 1 1 d . . . C(265) C -0.2103(2) -0.6972(2) 0.3399(2) 0.0427(9) Uani 1 1 d . . . C(266) C -0.2091(2) -0.68757(18) 0.26240(19) 0.0362(8) Uani 1 1 d . . . C(321) C -0.07189(17) -0.32088(17) 0.27169(16) 0.0253(6) Uani 1 1 d . . . C(322) C -0.0746(2) -0.24217(19) 0.25495(18) 0.0399(8) Uani 1 1 d . . . C(323) C -0.0429(2) -0.2136(2) 0.19148(19) 0.0456(9) Uani 1 1 d . . . C(324) C -0.0076(2) -0.2635(2) 0.1453(2) 0.0441(9) Uani 1 1 d . . . C(325) C -0.0040(2) -0.3421(2) 0.1612(2) 0.0478(10) Uani 1 1 d . . . C(326) C -0.03588(19) -0.3708(2) 0.22413(18) 0.0371(8) Uani 1 1 d . . . C(361) C -0.31786(19) -0.43302(17) 0.38736(15) 0.0245(6) Uani 1 1 d . . . C(362) C -0.38737(19) -0.38933(19) 0.34754(16) 0.0296(7) Uani 1 1 d . . . C(363) C -0.4726(2) -0.4132(2) 0.34401(17) 0.0372(8) Uani 1 1 d . . . C(364) C -0.4902(2) -0.4808(2) 0.38055(19) 0.0417(8) Uani 1 1 d . . . C(365) C -0.4223(2) -0.5243(2) 0.4199(2) 0.0430(9) Uani 1 1 d . . . C(366) C -0.3369(2) -0.50075(18) 0.42335(18) 0.0336(7) Uani 1 1 d . . . C(911) C 0.8638(2) -0.0076(2) 0.2311(2) 0.0469(9) Uani 1 1 d . . . C(912) C 0.8863(2) 0.0078(2) 0.1610(2) 0.0463(9) Uani 1 1 d . . . C(913) C 0.8391(2) 0.0606(2) 0.1121(2) 0.0497(10) Uani 1 1 d . . . C(914) C 0.7693(3) 0.0978(2) 0.1323(2) 0.0607(11) Uani 1 1 d . . . C(915) C 0.7464(3) 0.0825(3) 0.2017(3) 0.0633(12) Uani 1 1 d . . . C(916) C 0.7937(3) 0.0297(2) 0.2518(2) 0.0545(10) Uani 1 1 d . . . H(13) H -0.5920 -0.2588 0.1407 0.036 Uiso 1 1 calc R . . H(14) H -0.6849 -0.3634 0.1485 0.040 Uiso 1 1 calc R . . H(15) H -0.6316 -0.4903 0.1509 0.035 Uiso 1 1 calc R . . H(23) H -0.1400 -0.5985 -0.0517 0.046 Uiso 1 1 calc R . . H(24) H -0.1137 -0.7175 0.0114 0.055 Uiso 1 1 calc R . . H(25) H -0.1253 -0.7271 0.1396 0.046 Uiso 1 1 calc R . . H(33) H 0.0031 -0.3308 0.4190 0.036 Uiso 1 1 calc R . . H(34) H -0.0520 -0.3759 0.5245 0.039 Uiso 1 1 calc R . . H(35) H -0.1939 -0.4199 0.5090 0.036 Uiso 1 1 calc R . . H(122) H -0.4587 -0.2423 0.0172 0.039 Uiso 1 1 calc R . . H(123) H -0.3735 -0.1334 0.0066 0.046 Uiso 1 1 calc R . . H(124) H -0.2868 -0.0796 0.1148 0.037 Uiso 1 1 calc R . . H(125) H -0.2853 -0.1354 0.2350 0.036 Uiso 1 1 calc R . . H(126) H -0.3715 -0.2443 0.2461 0.035 Uiso 1 1 calc R . . H(162) H -0.5235 -0.5886 0.2270 0.038 Uiso 1 1 calc R . . H(163) H -0.4771 -0.7163 0.2160 0.046 Uiso 1 1 calc R . . H(164) H -0.4033 -0.7508 0.1183 0.046 Uiso 1 1 calc R . . H(165) H -0.3782 -0.6576 0.0294 0.042 Uiso 1 1 calc R . . H(166) H -0.4258 -0.5298 0.0388 0.035 Uiso 1 1 calc R . . H(222) H -0.3214 -0.4578 -0.0129 0.036 Uiso 1 1 calc R . . H(223) H -0.3434 -0.3408 -0.0804 0.044 Uiso 1 1 calc R . . H(224) H -0.2244 -0.2730 -0.1113 0.054 Uiso 1 1 calc R . . H(225) H -0.0847 -0.3247 -0.0766 0.060 Uiso 1 1 calc R . . H(226) H -0.0636 -0.4436 -0.0132 0.048 Uiso 1 1 calc R . . H(262) H -0.0947 -0.5288 0.2752 0.035 Uiso 1 1 calc R . . H(263) H -0.0973 -0.5454 0.4049 0.042 Uiso 1 1 calc R . . H(264) H -0.1707 -0.6504 0.4458 0.050 Uiso 1 1 calc R . . H(265) H -0.2396 -0.7407 0.3565 0.051 Uiso 1 1 calc R . . H(266) H -0.2377 -0.7246 0.2266 0.043 Uiso 1 1 calc R . . H(322) H -0.0983 -0.2070 0.2870 0.048 Uiso 1 1 calc R . . H(323) H -0.0459 -0.1594 0.1804 0.055 Uiso 1 1 calc R . . H(324) H 0.0142 -0.2440 0.1025 0.053 Uiso 1 1 calc R . . H(325) H 0.0202 -0.3769 0.1292 0.057 Uiso 1 1 calc R . . H(326) H -0.0330 -0.4250 0.2347 0.044 Uiso 1 1 calc R . . H(362) H -0.3759 -0.3426 0.3226 0.035 Uiso 1 1 calc R . . H(363) H -0.5190 -0.3831 0.3164 0.045 Uiso 1 1 calc R . . H(364) H -0.5487 -0.4971 0.3785 0.050 Uiso 1 1 calc R . . H(365) H -0.4342 -0.5708 0.4450 0.052 Uiso 1 1 calc R . . H(366) H -0.2908 -0.5314 0.4507 0.040 Uiso 1 1 calc R . . H(911) H 0.8967 -0.0440 0.2651 0.056 Uiso 1 1 calc R . . H(912) H 0.9345 -0.0181 0.1467 0.056 Uiso 1 1 calc R . . H(913) H 0.8548 0.0712 0.0639 0.060 Uiso 1 1 calc R . . H(914) H 0.7367 0.1343 0.0983 0.073 Uiso 1 1 calc R . . H(915) H 0.6978 0.1083 0.2156 0.076 Uiso 1 1 calc R . . H(916) H 0.7779 0.0193 0.3000 0.065 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rb 0.02491(15) 0.02611(16) 0.02386(15) 0.00274(12) 0.00483(11) -0.00027(11) Ge 0.02046(16) 0.02303(17) 0.01903(15) 0.00115(13) 0.00393(12) -0.00035(12) O(1) 0.0177(10) 0.0270(11) 0.0219(10) 0.0013(8) 0.0034(8) -0.0024(8) O(2) 0.0270(10) 0.0248(11) 0.0256(10) -0.0026(9) 0.0094(8) 0.0004(8) O(3) 0.0232(10) 0.0276(11) 0.0151(9) 0.0053(8) 0.0027(8) -0.0005(8) C(11) 0.0195(14) 0.0285(16) 0.0153(13) 0.0022(12) 0.0018(11) 0.0020(11) C(12) 0.0222(15) 0.0294(16) 0.0204(14) 0.0020(13) 0.0050(12) 0.0002(12) C(13) 0.0276(16) 0.0340(18) 0.0298(16) -0.0017(14) 0.0062(13) 0.0018(13) C(14) 0.0188(15) 0.043(2) 0.0390(18) 0.0041(14) 0.0062(13) 0.0034(15) C(15) 0.0259(16) 0.0333(18) 0.0295(16) 0.0101(14) 0.0059(13) 0.0011(13) C(16) 0.0212(14) 0.0301(16) 0.0199(14) 0.0031(13) 0.0011(11) 0.0005(12) C(21) 0.0202(14) 0.0250(16) 0.0297(16) 0.0001(12) 0.0063(12) 0.0038(12) C(22) 0.0242(15) 0.0326(17) 0.0283(16) 0.0002(13) 0.0071(13) 0.0054(13) C(23) 0.045(2) 0.042(2) 0.0310(18) -0.0025(17) 0.0122(15) 0.0103(15) C(24) 0.056(2) 0.035(2) 0.046(2) -0.0108(17) 0.0105(18) 0.0145(16) C(25) 0.044(2) 0.0269(17) 0.041(2) -0.0071(15) 0.0023(16) 0.0042(14) C(26) 0.0250(15) 0.0252(16) 0.0295(16) 0.0004(13) 0.0012(13) 0.0031(12) C(31) 0.0249(15) 0.0193(15) 0.0200(15) -0.0002(12) 0.0037(12) 0.0031(11) C(32) 0.0266(15) 0.0223(15) 0.0234(15) -0.0001(13) 0.0029(12) 0.0013(12) C(33) 0.0254(16) 0.0341(17) 0.0281(16) 0.0017(14) 0.0004(13) 0.0023(13) C(34) 0.0336(18) 0.044(2) 0.0188(15) -0.0036(15) -0.0026(13) 0.0044(13) C(35) 0.0348(17) 0.0371(18) 0.0179(15) -0.0023(15) 0.0052(13) -0.0006(13) C(36) 0.0256(15) 0.0235(15) 0.0187(14) -0.0031(12) 0.0055(12) 0.0010(11) C(121) 0.0195(14) 0.0234(15) 0.0247(15) -0.0020(12) 0.0070(11) 0.0005(12) C(122) 0.0346(17) 0.0366(18) 0.0252(16) 0.0025(15) 0.0014(13) -0.0024(13) C(123) 0.048(2) 0.040(2) 0.0276(17) 0.0062(17) 0.0076(15) -0.0098(14) C(124) 0.0331(17) 0.0252(16) 0.0370(18) 0.0054(14) 0.0137(14) -0.0002(13) C(125) 0.0309(16) 0.0274(16) 0.0320(17) 0.0054(14) 0.0072(13) 0.0043(13) C(126) 0.0335(16) 0.0308(17) 0.0237(15) 0.0011(14) 0.0081(13) -0.0029(13) C(161) 0.0203(14) 0.0284(16) 0.0232(15) 0.0089(13) -0.0016(12) 0.0027(12) C(162) 0.0308(17) 0.0349(18) 0.0298(17) 0.0075(14) 0.0065(13) -0.0008(14) C(163) 0.0387(19) 0.0352(19) 0.0394(19) 0.0088(16) 0.0008(15) -0.0108(15) C(164) 0.0396(19) 0.0278(18) 0.043(2) -0.0001(15) -0.0027(16) 0.0016(15) C(165) 0.0347(17) 0.0373(19) 0.0313(17) -0.0003(15) 0.0040(14) 0.0071(14) C(166) 0.0298(16) 0.0318(17) 0.0242(15) 0.0059(14) 0.0022(13) 0.0004(13) C(221) 0.0346(17) 0.0347(17) 0.0157(14) 0.0055(14) 0.0066(12) 0.0069(12) C(222) 0.0318(17) 0.0334(17) 0.0241(15) 0.0055(14) 0.0046(13) 0.0035(13) C(223) 0.0422(19) 0.0379(19) 0.0280(17) 0.0005(16) -0.0017(14) 0.0034(14) C(224) 0.066(3) 0.040(2) 0.0288(18) 0.0068(19) 0.0049(17) -0.0067(15) C(225) 0.050(2) 0.062(3) 0.041(2) 0.018(2) 0.0129(17) -0.0119(18) C(226) 0.0341(18) 0.052(2) 0.0367(19) 0.0064(16) 0.0114(15) -0.0025(16) C(261) 0.0223(15) 0.0241(16) 0.0340(17) -0.0056(13) 0.0008(13) -0.0016(13) C(262) 0.0274(16) 0.0250(16) 0.0333(17) -0.0033(13) 0.0040(13) -0.0008(13) C(263) 0.0343(18) 0.0351(19) 0.0328(18) -0.0121(15) -0.0005(14) 0.0017(14) C(264) 0.048(2) 0.043(2) 0.0342(18) -0.0162(18) 0.0123(16) -0.0066(16) C(265) 0.0398(19) 0.039(2) 0.052(2) -0.0035(16) 0.0147(17) -0.0178(17) C(266) 0.0328(17) 0.0280(17) 0.046(2) 0.0036(15) 0.0024(15) -0.0003(15) C(321) 0.0161(14) 0.0325(17) 0.0253(15) 0.0056(13) -0.0013(12) -0.0030(13) C(322) 0.051(2) 0.0335(19) 0.0340(18) 0.0169(16) 0.0040(15) 0.0052(14) C(323) 0.055(2) 0.040(2) 0.041(2) 0.0245(18) 0.0048(17) -0.0061(16) C(324) 0.0258(17) 0.064(3) 0.043(2) 0.0065(17) 0.0095(15) -0.0193(19) C(325) 0.0376(19) 0.066(3) 0.046(2) -0.0192(19) 0.0251(17) -0.0153(19) C(326) 0.0315(17) 0.040(2) 0.0427(19) -0.0117(15) 0.0154(15) -0.0136(15) C(361) 0.0317(16) 0.0280(16) 0.0155(14) 0.0032(13) 0.0089(12) 0.0025(12) C(362) 0.0297(16) 0.0378(18) 0.0223(15) 0.0029(14) 0.0079(13) -0.0036(13) C(363) 0.0268(17) 0.054(2) 0.0300(17) 0.0005(16) 0.0035(14) -0.0001(15) C(364) 0.0302(18) 0.054(2) 0.043(2) 0.0108(17) 0.0126(15) 0.0056(17) C(365) 0.050(2) 0.0297(18) 0.054(2) 0.0094(17) 0.0225(18) -0.0017(16) C(366) 0.0385(18) 0.0295(18) 0.0355(18) -0.0026(15) 0.0138(14) -0.0023(14) C(911) 0.042(2) 0.049(2) 0.047(2) -0.0087(18) 0.0034(17) -0.0077(17) C(912) 0.0365(19) 0.058(2) 0.045(2) -0.0077(18) 0.0095(16) -0.0139(18) C(913) 0.054(2) 0.054(2) 0.041(2) -0.022(2) 0.0095(18) -0.0073(18) C(914) 0.067(3) 0.046(2) 0.066(3) 0.007(2) 0.004(2) -0.005(2) C(915) 0.058(3) 0.069(3) 0.065(3) 0.000(2) 0.018(2) -0.024(2) C(916) 0.057(2) 0.064(3) 0.047(2) -0.019(2) 0.0194(19) -0.017(2) # 10. MOLECULAR GEOMETRY _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_publ_flag Rb O(1) 2.8542(18) YES Rb O(3) 2.8614(17) YES Rb O(2) 2.9324(19) YES Rb C(222) 3.198(3) YES Rb C(223) 3.274(3) YES Rb C(322) 3.314(3) YES Rb C(321) 3.319(3) YES Rb C(126) 3.349(3) YES Rb C(326) 3.363(3) YES Rb C(121) 3.364(3) YES Rb C(323) 3.364(3) YES Rb C(325) 3.417(3) YES Ge O(2) 1.9305(18) YES Ge O(1) 1.9305(18) YES Ge O(3) 1.9402(18) YES Ge Rb 3.6018(4) YES O(1) C(11) 1.358(3) YES O(1) Rb 2.8542(18) YES O(2) C(21) 1.350(3) YES O(2) Rb 2.9325(19) YES O(3) C(31) 1.350(3) YES O(3) Rb 2.8614(17) YES C(11) C(12) 1.404(4) YES C(11) C(16) 1.413(4) YES C(12) C(13) 1.399(4) YES C(12) C(121) 1.496(4) YES C(13) C(14) 1.382(4) YES C(14) C(15) 1.387(4) YES C(15) C(16) 1.400(4) YES C(16) C(161) 1.491(4) YES C(21) C(22) 1.412(4) YES C(21) C(26) 1.415(4) YES C(22) C(23) 1.397(4) YES C(22) C(221) 1.490(4) YES C(23) C(24) 1.383(5) YES C(24) C(25) 1.379(5) YES C(25) C(26) 1.400(4) YES C(26) C(261) 1.495(4) YES C(31) C(32) 1.409(4) YES C(31) C(36) 1.417(4) YES C(32) C(33) 1.396(4) YES C(32) C(321) 1.497(4) YES C(33) C(34) 1.386(4) YES C(34) C(35) 1.372(4) YES C(35) C(36) 1.395(4) YES C(36) C(361) 1.496(4) YES C(121) C(122) 1.392(4) YES C(121) C(126) 1.393(4) YES C(121) Rb 3.364(3) YES C(122) C(123) 1.383(4) YES C(122) Rb 3.469(3) YES C(123) C(124) 1.380(4) YES C(123) Rb 3.583(3) YES C(124) C(125) 1.382(4) YES C(124) Rb 3.587(3) YES C(125) C(126) 1.391(4) YES C(125) Rb 3.469(3) YES C(126) Rb 3.349(3) YES C(161) C(162) 1.392(4) YES C(161) C(166) 1.399(4) YES C(162) C(163) 1.387(4) YES C(163) C(164) 1.382(5) YES C(164) C(165) 1.381(5) YES C(165) C(166) 1.388(4) YES C(221) C(226) 1.388(4) YES C(221) C(222) 1.392(4) YES C(221) Rb 3.438(3) YES C(222) C(223) 1.388(4) YES C(222) Rb 3.198(3) YES C(223) C(224) 1.389(5) YES C(223) Rb 3.274(3) YES C(224) C(225) 1.380(5) YES C(224) Rb 3.558(3) YES C(225) C(226) 1.385(5) YES C(226) Rb 3.716(3) YES C(261) C(266) 1.388(4) YES C(261) C(262) 1.400(4) YES C(262) C(263) 1.388(4) YES C(263) C(264) 1.373(5) YES C(264) C(265) 1.383(5) YES C(265) C(266) 1.389(5) YES C(321) C(322) 1.383(4) YES C(321) C(326) 1.392(4) YES C(321) Rb 3.319(3) YES C(322) C(323) 1.401(5) YES C(322) Rb 3.314(3) YES C(323) C(324) 1.370(5) YES C(323) Rb 3.364(3) YES C(324) C(325) 1.378(5) YES C(324) Rb 3.424(3) YES C(325) C(326) 1.394(4) YES C(325) Rb 3.417(3) YES C(326) Rb 3.363(3) YES C(361) C(366) 1.385(4) YES C(361) C(362) 1.399(4) YES C(362) C(363) 1.383(4) YES C(363) C(364) 1.382(5) YES C(364) C(365) 1.378(5) YES C(365) C(366) 1.384(4) YES C(911) C(916) 1.376(5) YES C(911) C(912) 1.380(5) YES C(912) C(913) 1.372(5) YES C(913) C(914) 1.368(5) YES C(914) C(915) 1.370(6) YES C(915) C(916) 1.383(6) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Rb O(3) 55.42(5) YES O(1) Rb O(2) 55.20(5) YES O(3) Rb O(2) 54.97(5) YES O(1) Rb C(222) 69.75(7) YES O(3) Rb C(222) 112.16(7) YES O(2) Rb C(222) 62.27(7) YES O(1) Rb C(223) 83.57(7) YES O(3) Rb C(223) 134.49(7) YES O(2) Rb C(223) 86.99(7) YES C(222) Rb C(223) 24.73(8) YES O(1) Rb C(322) 124.18(7) YES O(3) Rb C(322) 69.42(7) YES O(2) Rb C(322) 100.64(7) YES C(222) Rb C(322) 148.58(8) YES C(223) Rb C(322) 150.52(8) YES O(1) Rb C(321) 107.83(6) YES O(3) Rb C(321) 53.21(6) YES O(2) Rb C(321) 76.60(6) YES C(222) Rb C(321) 131.28(8) YES C(223) Rb C(321) 148.11(8) YES C(322) Rb C(321) 24.07(7) YES O(1) Rb C(126) 66.27(6) YES O(3) Rb C(126) 67.74(6) YES O(2) Rb C(126) 113.53(6) YES C(222) Rb C(126) 123.48(7) YES C(223) Rb C(126) 116.27(8) YES C(322) Rb C(126) 86.93(8) YES C(321) Rb C(126) 95.43(7) YES O(1) Rb C(326) 110.90(7) YES O(3) Rb C(326) 64.65(6) YES O(2) Rb C(326) 64.08(7) YES C(222) Rb C(326) 108.72(8) YES C(223) Rb C(326) 124.14(8) YES C(322) Rb C(326) 41.75(9) YES C(321) Rb C(326) 24.04(8) YES C(126) Rb C(326) 118.92(7) YES O(1) Rb C(121) 53.29(6) YES O(3) Rb C(121) 78.31(6) YES O(2) Rb C(121) 107.92(6) YES C(222) Rb C(121) 99.81(7) YES C(223) Rb C(121) 93.28(8) YES C(322) Rb C(121) 110.88(8) YES C(321) Rb C(121) 117.63(7) YES C(126) Rb C(121) 23.96(7) YES C(326) Rb C(121) 139.45(7) YES O(1) Rb C(323) 148.33(7) YES O(3) Rb C(323) 93.15(7) YES O(2) Rb C(323) 112.48(8) YES C(222) Rb C(323) 134.57(9) YES C(223) Rb C(323) 127.12(8) YES C(322) Rb C(323) 24.20(8) YES C(321) Rb C(323) 42.49(8) YES C(126) Rb C(323) 100.57(9) YES C(326) Rb C(323) 48.42(9) YES C(121) Rb C(323) 122.61(8) YES O(1) Rb C(325) 130.09(7) YES O(3) Rb C(325) 88.36(7) YES O(2) Rb C(325) 76.52(8) YES C(222) Rb C(325) 100.44(9) YES C(223) Rb C(325) 107.74(9) YES C(322) Rb C(325) 48.36(9) YES C(321) Rb C(325) 42.14(8) YES C(126) Rb C(325) 135.00(8) YES C(326) Rb C(325) 23.71(7) YES C(121) Rb C(325) 158.82(8) YES C(323) Rb C(325) 41.03(10) YES O(2) Ge O(1) 87.99(8) YES O(2) Ge O(3) 87.42(8) YES O(1) Ge O(3) 86.72(8) YES O(2) Ge Rb 54.38(6) YES O(1) Ge Rb 52.04(5) YES O(3) Ge Rb 52.29(5) YES C(11) O(1) Ge 118.77(16) YES C(11) O(1) Rb 135.50(16) YES Ge O(1) Rb 95.73(6) YES C(21) O(2) Ge 125.36(17) YES C(21) O(2) Rb 136.77(16) YES Ge O(2) Rb 93.27(7) YES C(31) O(3) Ge 122.14(16) YES C(31) O(3) Rb 134.57(15) YES Ge O(3) Rb 95.28(6) YES O(1) C(11) C(12) 118.8(2) YES O(1) C(11) C(16) 121.4(2) YES C(12) C(11) C(16) 119.8(2) YES C(13) C(12) C(11) 119.8(3) YES C(13) C(12) C(121) 119.4(3) YES C(11) C(12) C(121) 120.8(2) YES C(14) C(13) C(12) 120.7(3) YES C(13) C(14) C(15) 119.5(3) YES C(14) C(15) C(16) 121.5(3) YES C(15) C(16) C(11) 118.5(3) YES C(15) C(16) C(161) 119.4(3) YES C(11) C(16) C(161) 122.0(2) YES O(2) C(21) C(22) 117.7(3) YES O(2) C(21) C(26) 123.0(3) YES C(22) C(21) C(26) 119.2(3) YES C(23) C(22) C(21) 119.4(3) YES C(23) C(22) C(221) 119.7(3) YES C(21) C(22) C(221) 120.8(3) YES C(24) C(23) C(22) 121.4(3) YES C(25) C(24) C(23) 119.2(3) YES C(24) C(25) C(26) 121.6(3) YES C(25) C(26) C(21) 119.1(3) YES C(25) C(26) C(261) 118.6(3) YES C(21) C(26) C(261) 122.3(3) YES O(3) C(31) C(32) 118.5(2) YES O(3) C(31) C(36) 122.2(2) YES C(32) C(31) C(36) 119.3(2) YES C(33) C(32) C(31) 119.9(3) YES C(33) C(32) C(321) 120.3(2) YES C(31) C(32) C(321) 119.7(2) YES C(34) C(33) C(32) 120.4(3) YES C(35) C(34) C(33) 119.8(3) YES C(34) C(35) C(36) 121.9(3) YES C(35) C(36) C(31) 118.6(3) YES C(35) C(36) C(361) 119.2(2) YES C(31) C(36) C(361) 122.1(2) YES C(122) C(121) C(126) 118.0(3) YES C(122) C(121) C(12) 120.0(2) YES C(126) C(121) C(12) 122.0(2) YES C(122) C(121) Rb 82.54(17) YES C(126) C(121) Rb 77.44(16) YES C(12) C(121) Rb 111.23(16) YES C(123) C(122) C(121) 120.8(3) YES C(123) C(122) Rb 83.36(19) YES C(121) C(122) Rb 74.03(16) YES C(124) C(123) C(122) 120.5(3) YES C(124) C(123) Rb 79.05(19) YES C(122) C(123) Rb 74.10(19) YES C(123) C(124) C(125) 119.7(3) YES C(123) C(124) Rb 78.75(19) YES C(125) C(124) Rb 73.95(17) YES C(124) C(125) C(126) 119.6(3) YES C(124) C(125) Rb 83.54(18) YES C(126) C(125) Rb 73.44(17) YES C(125) C(126) C(121) 121.3(3) YES C(125) C(126) Rb 83.11(17) YES C(121) C(126) Rb 78.60(16) YES C(162) C(161) C(166) 118.3(3) YES C(162) C(161) C(16) 121.6(3) YES C(166) C(161) C(16) 120.1(3) YES C(163) C(162) C(161) 120.6(3) YES C(164) C(163) C(162) 120.5(3) YES C(163) C(164) C(165) 119.7(3) YES C(164) C(165) C(166) 120.1(3) YES C(165) C(166) C(161) 120.8(3) YES C(226) C(221) C(222) 118.0(3) YES C(226) C(221) C(22) 120.1(3) YES C(222) C(221) C(22) 121.9(3) YES C(226) C(221) Rb 90.38(19) YES C(222) C(221) Rb 68.37(16) YES C(22) C(221) Rb 111.91(17) YES C(223) C(222) C(221) 121.0(3) YES C(223) C(222) Rb 80.71(18) YES C(221) C(222) Rb 87.76(17) YES C(222) C(223) C(224) 120.0(3) YES C(222) C(223) Rb 74.56(17) YES C(224) C(223) Rb 90.06(19) YES C(225) C(224) C(223) 119.4(3) YES C(225) C(224) Rb 87.6(2) YES C(223) C(224) Rb 66.96(18) YES C(224) C(225) C(226) 120.3(3) YES C(225) C(226) C(221) 121.2(3) YES C(225) C(226) Rb 81.2(2) YES C(221) C(226) Rb 67.69(17) YES C(266) C(261) C(262) 117.6(3) YES C(266) C(261) C(26) 121.2(3) YES C(262) C(261) C(26) 121.2(3) YES C(263) C(262) C(261) 121.2(3) YES C(264) C(263) C(262) 120.2(3) YES C(263) C(264) C(265) 119.6(3) YES C(264) C(265) C(266) 120.4(3) YES C(261) C(266) C(265) 121.0(3) YES C(322) C(321) C(326) 118.1(3) YES C(322) C(321) C(32) 121.0(3) YES C(326) C(321) C(32) 120.9(3) YES C(322) C(321) Rb 77.75(17) YES C(326) C(321) Rb 79.73(17) YES C(32) C(321) Rb 112.43(16) YES C(321) C(322) C(323) 120.9(3) YES C(321) C(322) Rb 78.19(17) YES C(323) C(322) Rb 79.91(19) YES C(324) C(323) C(322) 120.2(3) YES C(324) C(323) Rb 80.80(19) YES C(322) C(323) Rb 75.89(18) YES C(323) C(324) C(325) 119.8(3) YES C(323) C(324) Rb 75.93(19) YES C(325) C(324) Rb 78.13(19) YES C(324) C(325) C(326) 120.1(3) YES C(324) C(325) Rb 78.63(19) YES C(326) C(325) Rb 75.95(18) YES C(321) C(326) C(325) 120.9(3) YES C(321) C(326) Rb 76.23(16) YES C(325) C(326) Rb 80.34(19) YES C(366) C(361) C(362) 118.1(3) YES C(366) C(361) C(36) 121.2(3) YES C(362) C(361) C(36) 120.7(3) YES C(363) C(362) C(361) 121.0(3) YES C(364) C(363) C(362) 120.1(3) YES C(365) C(364) C(363) 119.4(3) YES C(364) C(365) C(366) 120.6(3) YES C(365) C(366) C(361) 120.8(3) YES C(916) C(911) C(912) 119.9(4) YES C(913) C(912) C(911) 120.1(4) YES C(914) C(913) C(912) 120.2(4) YES C(913) C(914) C(915) 120.0(4) YES C(914) C(915) C(916) 120.4(4) YES C(911) C(916) C(915) 119.4(4) YES #============================================================================== data_SW2274 _database_code_CSD 203290 _audit_creation_date 19-08-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.33 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C57 H42 Ge1 Na1 O3' _chemical_formula_moiety 'C54 H39 Ge1 Na1 O3,0.5(C6 H6)' _chemical_formula_structural ? _chemical_formula_weight 870.55 _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x+1/2, y, -z+1/2' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-z, -x, -y' '-z+1/2, x+1/2, y' 'z+1/2, x, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z, -x' 'y, -z+1/2, x+1/2' '-y+1/2, z+1/2, x' 'y+1/2, z, -x+1/2' _cell_length_a 20.7127(3) _cell_length_b 20.7127(3) _cell_length_c 20.7127(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8886.1(2) _cell_measurement_reflns_used 19406 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.732 _cell_measurement_temperature 150 _exptl_crystal_F_000 3608 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7419 _exptl_absorpt_correction_T_max 0.7855 _diffrn_reflns_number 19406 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9991 _reflns_number_total 3396 _reflns_number_gt 2658 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 1 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_max 0 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.113 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 3380 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0646P)^2^+4.6860P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.91 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ge Ge 0.807999(12) 0.192001(12) 0.692001(12) 0.02676(16) Uani 1 3 d S . . Na Na 0.88996(4) 0.11004(4) 0.61004(4) 0.0276(4) Uani 1 3 d S . . O O 0.81315(7) 0.09857(8) 0.68980(7) 0.0259(4) Uani 1 1 d . . . C(1) C 0.80329(12) 0.06426(11) 0.74471(11) 0.0267(5) Uani 1 1 d . . . C(2) C 0.85306(12) 0.02490(12) 0.76848(11) 0.0291(5) Uani 1 1 d . . . C(3) C 0.84386(15) -0.00857(14) 0.82640(13) 0.0418(7) Uani 1 1 d . . . C(4) C 0.78607(16) -0.00401(16) 0.85948(14) 0.0500(8) Uani 1 1 d . . . C(5) C 0.73732(15) 0.03441(15) 0.83590(14) 0.0453(7) Uani 1 1 d . . . C(6) C 0.74433(12) 0.06870(13) 0.77824(12) 0.0334(6) Uani 1 1 d . . . C(21) C 0.91469(12) 0.01863(11) 0.73236(11) 0.0276(5) Uani 1 1 d . . . C(22) C 0.91558(13) -0.00551(12) 0.66939(12) 0.0287(5) Uani 1 1 d . . . C(23) C 0.97339(13) -0.01151(12) 0.63589(13) 0.0345(6) Uani 1 1 d . . . C(24) C 1.03105(13) 0.00580(13) 0.66483(15) 0.0393(6) Uani 1 1 d . . . C(25) C 1.03081(14) 0.02913(13) 0.72701(15) 0.0400(7) Uani 1 1 d . . . C(26) C 0.97343(13) 0.03541(12) 0.76033(13) 0.0347(6) Uani 1 1 d . . . C(61) C 0.69110(12) 0.11018(13) 0.75404(14) 0.0361(6) Uani 1 1 d . . . C(62) C 0.66159(15) 0.15520(16) 0.79472(17) 0.0526(9) Uani 1 1 d . . . C(63) C 0.61252(17) 0.19485(18) 0.7707(2) 0.0698(12) Uani 1 1 d . . . C(64) C 0.59267(17) 0.19049(17) 0.7070(2) 0.0661(11) Uani 1 1 d . . . C(65) C 0.62187(15) 0.14674(17) 0.66719(18) 0.0561(9) Uani 1 1 d . . . C(66) C 0.67009(13) 0.10643(15) 0.68988(14) 0.0405(7) Uani 1 1 d . . . C(911) C 0.9891(2) 0.0510(2) 0.9598(2) 0.0806(12) Uani 1 1 d . . . H(3) H 0.8776 -0.0347 0.8432 0.050 Uiso 1 1 calc R . . H(4) H 0.7800 -0.0274 0.8985 0.060 Uiso 1 1 calc R . . H(5) H 0.6980 0.0377 0.8593 0.054 Uiso 1 1 calc R . . H(22) H 1.0159(12) 0.1517(12) 0.6237(14) 0.030(7) Uiso 1 1 d . . . H(23) H 0.9733 -0.0276 0.5929 0.041 Uiso 1 1 calc R . . H(24) H 1.0706 0.0016 0.6419 0.047 Uiso 1 1 calc R . . H(25) H 1.0703 0.0410 0.7471 0.048 Uiso 1 1 calc R . . H(26) H 0.9741 0.0515 0.8033 0.042 Uiso 1 1 calc R . . H(62) H 0.6748 0.1588 0.8385 0.063 Uiso 1 1 calc R . . H(63) H 0.5925 0.2253 0.7985 0.084 Uiso 1 1 calc R . . H(64) H 0.5592 0.2176 0.6912 0.079 Uiso 1 1 calc R . . H(65) H 0.6089 0.1440 0.6233 0.067 Uiso 1 1 calc R . . H(66) H 0.6892 0.0758 0.6616 0.049 Uiso 1 1 calc R . . H(911) H 0.9816 0.0866 0.9319 0.097 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge 0.02676(16) 0.02676(16) 0.02676(16) 0.00124(10) 0.00124(10) -0.00124(10) Na 0.0276(4) 0.0276(4) 0.0276(4) 0.0008(4) 0.0008(4) -0.0008(4) O 0.0266(9) 0.0258(8) 0.0253(8) -0.0009(7) 0.0064(7) 0.0036(7) C(1) 0.0326(13) 0.0259(12) 0.0215(11) -0.0062(10) 0.0022(10) -0.0024(9) C(2) 0.0366(14) 0.0269(12) 0.0240(12) -0.0031(10) -0.0006(10) -0.0003(10) C(3) 0.0538(19) 0.0427(16) 0.0288(14) 0.0005(14) -0.0004(13) 0.0075(12) C(4) 0.065(2) 0.058(2) 0.0270(14) -0.0046(17) 0.0066(14) 0.0124(14) C(5) 0.0478(17) 0.0575(19) 0.0305(14) -0.0088(15) 0.0129(13) 0.0022(13) C(6) 0.0353(14) 0.0376(14) 0.0271(13) -0.0083(12) 0.0079(11) -0.0009(11) C(21) 0.0338(13) 0.0198(11) 0.0291(12) 0.0003(10) -0.0022(10) 0.0036(9) C(22) 0.0310(13) 0.0249(12) 0.0301(12) 0.0013(10) -0.0038(11) -0.0009(10) C(23) 0.0429(15) 0.0296(13) 0.0309(13) 0.0094(11) 0.0000(11) -0.0003(11) C(24) 0.0340(14) 0.0346(15) 0.0493(17) 0.0051(12) 0.0037(13) 0.0036(13) C(25) 0.0347(15) 0.0349(15) 0.0506(18) 0.0002(12) -0.0080(13) -0.0007(13) C(26) 0.0420(15) 0.0280(13) 0.0341(14) 0.0018(11) -0.0088(12) -0.0028(11) C(61) 0.0286(13) 0.0400(15) 0.0398(15) -0.0049(11) 0.0157(12) 0.0012(12) C(62) 0.0415(17) 0.056(2) 0.060(2) -0.0039(15) 0.0267(15) -0.0064(16) C(63) 0.049(2) 0.055(2) 0.106(3) 0.0075(17) 0.047(2) 0.000(2) C(64) 0.0408(18) 0.061(2) 0.097(3) 0.0117(16) 0.030(2) 0.031(2) C(65) 0.0345(16) 0.071(2) 0.062(2) -0.0005(16) 0.0097(15) 0.0248(18) C(66) 0.0285(13) 0.0497(17) 0.0434(16) -0.0009(12) 0.0118(12) 0.0080(13) C(911) 0.086(3) 0.079(3) 0.077(3) 0.013(2) 0.007(2) 0.021(2) # 10. MOLECULAR GEOMETRY _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_publ_flag Ge O 1.9387(16) YES Ge O 1.9387(16) YES Ge O 1.9388(16) YES Ge Na 2.9405(16) YES Na O 2.3059(19) YES Na O 2.3060(19) YES Na O 2.3060(19) YES Na C(22) 2.742(3) YES Na C(22) 2.742(3) YES Na C(22) 2.742(3) YES Na C(23) 3.100(3) YES Na C(23) 3.100(3) YES Na C(23) 3.100(3) YES O C(1) 1.356(3) YES C(1) C(2) 1.403(3) YES C(1) C(6) 1.408(3) YES C(2) C(3) 1.399(4) YES C(2) C(21) 1.485(3) YES C(3) C(4) 1.382(4) YES C(4) C(5) 1.375(4) YES C(5) C(6) 1.397(4) YES C(6) C(61) 1.485(4) YES C(21) C(26) 1.392(4) YES C(21) C(22) 1.397(3) YES C(22) C(23) 1.389(4) YES C(23) C(24) 1.384(4) YES C(24) C(25) 1.376(4) YES C(25) C(26) 1.380(4) YES C(61) C(62) 1.397(4) YES C(61) C(66) 1.401(4) YES C(62) C(63) 1.399(5) YES C(63) C(64) 1.384(6) YES C(64) C(65) 1.366(5) YES C(65) C(66) 1.384(4) YES C(911) C(911) 1.363(4) YES C(911) C(911) 1.363(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O Ge O 85.43(7) YES O Ge O 85.43(7) YES O Ge O 85.43(7) YES O Ge Na 51.56(5) YES O Ge Na 51.56(5) YES O Ge Na 51.56(5) YES O Na O 69.55(8) YES O Na O 69.55(8) YES O Na O 69.54(8) YES O Na C(22) 73.88(7) YES O Na C(22) 141.90(8) YES O Na C(22) 107.22(7) YES O Na C(22) 141.90(8) YES O Na C(22) 107.22(7) YES O Na C(22) 73.88(7) YES C(22) Na C(22) 108.01(7) YES O Na C(22) 107.22(7) YES O Na C(22) 73.88(7) YES O Na C(22) 141.90(8) YES C(22) Na C(22) 108.01(7) YES C(22) Na C(22) 108.01(7) YES O Na Ge 41.19(5) YES O Na Ge 41.19(5) YES O Na Ge 41.19(5) YES C(22) Na Ge 110.90(6) YES C(22) Na Ge 110.90(6) YES C(22) Na Ge 110.90(6) YES O Na C(23) 113.91(6) YES O Na C(23) 100.21(6) YES O Na C(23) 167.81(7) YES C(22) Na C(23) 84.90(8) YES C(22) Na C(23) 104.10(9) YES C(22) Na C(23) 26.62(7) YES Ge Na C(23) 133.70(5) YES O Na C(23) 167.81(7) YES O Na C(23) 113.91(6) YES O Na C(23) 100.20(6) YES C(22) Na C(23) 104.09(9) YES C(22) Na C(23) 26.62(7) YES C(22) Na C(23) 84.90(8) YES Ge Na C(23) 133.70(5) YES C(23) Na C(23) 77.52(8) YES O Na C(23) 100.20(6) YES O Na C(23) 167.81(7) YES O Na C(23) 113.91(6) YES C(22) Na C(23) 26.62(7) YES C(22) Na C(23) 84.90(8) YES C(22) Na C(23) 104.10(9) YES Ge Na C(23) 133.70(5) YES C(23) Na C(23) 77.52(8) YES C(23) Na C(23) 77.52(8) YES C(1) O Ge 119.67(14) YES C(1) O Na 139.33(14) YES Ge O Na 87.25(6) YES O C(1) C(2) 119.2(2) YES O C(1) C(6) 120.6(2) YES C(2) C(1) C(6) 120.1(2) YES C(3) C(2) C(1) 119.3(2) YES C(3) C(2) C(21) 120.4(2) YES C(1) C(2) C(21) 120.3(2) YES C(4) C(3) C(2) 120.6(3) YES C(5) C(4) C(3) 120.0(3) YES C(4) C(5) C(6) 121.4(3) YES C(5) C(6) C(1) 118.6(3) YES C(5) C(6) C(61) 120.4(2) YES C(1) C(6) C(61) 121.0(2) YES C(26) C(21) C(22) 117.8(2) YES C(26) C(21) C(2) 121.3(2) YES C(22) C(21) C(2) 120.9(2) YES C(23) C(22) C(21) 120.6(2) YES C(23) C(22) Na 91.20(16) YES C(21) C(22) Na 95.95(15) YES C(24) C(23) C(22) 120.3(2) YES C(24) C(23) Na 110.22(17) YES C(22) C(23) Na 62.18(14) YES C(25) C(24) C(23) 119.6(3) YES C(24) C(25) C(26) 120.3(3) YES C(25) C(26) C(21) 121.4(2) YES C(62) C(61) C(66) 118.2(3) YES C(62) C(61) C(6) 120.5(3) YES C(66) C(61) C(6) 121.3(2) YES C(61) C(62) C(63) 119.7(3) YES C(64) C(63) C(62) 121.1(3) YES C(65) C(64) C(63) 119.1(3) YES C(64) C(65) C(66) 121.0(4) YES C(65) C(66) C(61) 120.9(3) YES C(911) C(911) C(911) 120.000(2) YES data_SW2255 _database_code_CSD 203291 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C60 H45 Ge1 Li1 O3' _chemical_formula_moiety 'C54 H39 Ge1 Li1 O3,C6 H6' _chemical_formula_structural ? _chemical_formula_weight 893.56 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 15.7846(6) _cell_length_b 15.7846(6) _cell_length_c 15.839(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3417.7(7) _cell_measurement_reflns_used 5130 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 3 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.707 _cell_measurement_temperature 150 _exptl_crystal_F_000 1392 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7140 _exptl_absorpt_correction_T_max 0.8234 _diffrn_reflns_number 5130 _diffrn_measured_fraction_theta_max 0.8447 _diffrn_reflns_theta_full 21.7 _diffrn_measured_fraction_theta_full 0.9536 _reflns_number_total 3028 _reflns_friedl_coverage 0.8045 _reflns_number_gt 2952 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 20 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.061 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3021 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0109P)^2^+0.7616P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.37 _refine_diff_density_min -0.34 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.14E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.282(8) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ge Ge 1.0000 1.0000 0.283581(17) 0.01880(11) Uani 1 3 d S . . O(1) O 0.93722(9) 1.04511(10) 0.36438(8) 0.0173(3) Uani 1 1 d . . . C(1) C 0.85095(14) 1.04011(13) 0.34430(13) 0.0169(4) Uani 1 1 d . . . C(2) C 0.84417(14) 1.08960(14) 0.27310(13) 0.0174(4) Uani 1 1 d . . . C(3) C 0.75347(15) 1.07978(15) 0.25343(13) 0.0219(4) Uani 1 1 d . . . C(4) C 0.67131(15) 1.02373(15) 0.30235(14) 0.0234(4) Uani 1 1 d . . . C(5) C 0.67926(15) 0.97551(15) 0.37220(14) 0.0228(4) Uani 1 1 d . . . C(6) C 0.76802(14) 0.98316(14) 0.39508(13) 0.0189(4) Uani 1 1 d . . . C(21) C 0.92995(14) 1.14879(14) 0.21822(13) 0.0195(4) Uani 1 1 d . . . C(22) C 1.02177(15) 1.21378(15) 0.25222(15) 0.0228(5) Uani 1 1 d . . . C(23) C 1.10229(17) 1.26565(16) 0.19969(16) 0.0311(5) Uani 1 1 d . . . C(24) C 1.09254(19) 1.25402(19) 0.11350(17) 0.0409(6) Uani 1 1 d . . . C(25) C 1.0018(2) 1.1911(2) 0.07881(17) 0.0472(7) Uani 1 1 d . . . C(26) C 0.92155(19) 1.1390(2) 0.13046(16) 0.0323(6) Uani 1 1 d . . . C(61) C 0.77430(16) 0.93216(17) 0.47126(15) 0.0223(5) Uani 1 1 d . . . C(62) C 0.84294(16) 0.98318(17) 0.53486(14) 0.0254(5) Uani 1 1 d . . . C(63) C 0.84392(18) 0.93562(19) 0.60867(15) 0.0340(6) Uani 1 1 d . . . C(64) C 0.77774(19) 0.8369(2) 0.61907(17) 0.0419(7) Uani 1 1 d . . . C(65) C 0.71074(19) 0.78576(18) 0.55667(17) 0.0382(6) Uani 1 1 d . . . C(66) C 0.70890(16) 0.83312(16) 0.48320(16) 0.0294(5) Uani 1 1 d . . . C(91) C 0.9034(2) 0.9279(2) 0.84663(19) 0.0490(8) Uani 1 1 d . . . C(92) C 0.9284(2) 1.0256(2) 0.8469(2) 0.0497(7) Uani 1 1 d . . . Li Li 1.0000 1.0000 0.4492(4) 0.0323(15) Uani 1 3 d S . . H(3) H 0.7480 1.1124 0.2052 0.026 Uiso 1 1 calc R . . H(4) H 0.6104 1.0185 0.2882 0.028 Uiso 1 1 calc R . . H(5) H 0.6228 0.9362 0.4054 0.027 Uiso 1 1 calc R . . H(22) H 1.0292 1.2226 0.3116 0.027 Uiso 1 1 calc R . . H(23) H 1.1644 1.3094 0.2235 0.037 Uiso 1 1 calc R . . H(24) H 1.1478 1.2890 0.0779 0.049 Uiso 1 1 calc R . . H(25) H 0.9947 1.1837 0.0193 0.057 Uiso 1 1 calc R . . H(26) H 0.8597 1.0958 0.1060 0.039 Uiso 1 1 calc R . . H(62) H 0.8891 1.0507 0.5276 0.031 Uiso 1 1 calc R . . H(63) H 0.8900 0.9709 0.6519 0.041 Uiso 1 1 calc R . . H(64) H 0.7786 0.8044 0.6693 0.050 Uiso 1 1 calc R . . H(65) H 0.6656 0.7180 0.5638 0.046 Uiso 1 1 calc R . . H(66) H 0.6622 0.7972 0.4406 0.035 Uiso 1 1 calc R . . H(91) H 0.8365 0.8782 0.8462 0.059 Uiso 1 1 calc R . . H(92) H 0.8788 1.0429 0.8474 0.060 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge 0.01878(13) 0.01878(13) 0.01884(19) 0.00939(7) 0.0000 0.0000 O(1) 0.0159(7) 0.0203(7) 0.0187(7) 0.0112(6) 0.0019(6) 0.0021(6) C(1) 0.0162(10) 0.0155(9) 0.0191(10) 0.0080(8) 0.0016(8) -0.0022(8) C(2) 0.0175(10) 0.0155(9) 0.0182(9) 0.0075(8) -0.0010(8) -0.0017(8) C(3) 0.0233(11) 0.0244(11) 0.0214(11) 0.0144(9) -0.0047(9) -0.0029(9) C(4) 0.0168(10) 0.0270(11) 0.0286(12) 0.0125(9) -0.0038(9) -0.0065(9) C(5) 0.0153(9) 0.0230(11) 0.0267(11) 0.0069(8) 0.0029(9) -0.0047(9) C(6) 0.0180(10) 0.0173(10) 0.0213(10) 0.0087(8) 0.0014(8) -0.0034(8) C(21) 0.0212(10) 0.0186(10) 0.0224(10) 0.0126(8) 0.0006(8) 0.0035(8) C(22) 0.0236(11) 0.0166(10) 0.0268(11) 0.0088(9) 0.0008(9) 0.0041(9) C(23) 0.0228(11) 0.0248(11) 0.0436(15) 0.0102(9) 0.0016(10) 0.0107(10) C(24) 0.0316(13) 0.0480(16) 0.0400(15) 0.0175(12) 0.0139(12) 0.0208(13) C(25) 0.0445(17) 0.068(2) 0.0241(14) 0.0240(15) 0.0062(12) 0.0135(14) C(26) 0.0272(12) 0.0456(15) 0.0216(13) 0.0163(11) 0.0005(10) 0.0061(11) C(61) 0.0227(11) 0.0251(12) 0.0236(12) 0.0153(10) 0.0097(10) 0.0032(10) C(62) 0.0248(11) 0.0310(12) 0.0243(12) 0.0168(10) 0.0066(9) 0.0042(10) C(63) 0.0341(13) 0.0507(15) 0.0278(13) 0.0291(12) 0.0070(10) 0.0100(11) C(64) 0.0458(15) 0.0573(17) 0.0410(16) 0.0396(14) 0.0185(13) 0.0273(13) C(65) 0.0417(14) 0.0304(13) 0.0499(17) 0.0237(12) 0.0225(13) 0.0176(12) C(66) 0.0293(12) 0.0247(11) 0.0359(13) 0.0147(10) 0.0120(10) 0.0017(10) C(91) 0.0336(14) 0.0397(15) 0.068(2) 0.0139(12) -0.0055(13) 0.0016(14) C(92) 0.0406(15) 0.0443(16) 0.071(2) 0.0260(13) 0.0028(15) 0.0043(14) Li 0.032(2) 0.032(2) 0.032(4) 0.0161(11) 0.0000 0.0000 # 10. MOLECULAR GEOMETRY _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_publ_flag Ge O(1) 1.9576(13) YES Ge O(1) 1.9576(13) YES Ge O(1) 1.9577(13) YES Ge Li 2.624(7) YES Li O(1) 2.000(5) YES Li O(1) 2.000(5) YES Li O(1) 2.000(5) YES Li C(62) 2.720(4) YES Li C(62) 2.720(4) YES Li C(62) 2.720(4) YES O(1) C(1) 1.362(2) YES C(1) C(2) 1.406(3) YES C(1) C(6) 1.411(3) YES C(2) C(3) 1.396(3) YES C(2) C(21) 1.482(3) YES C(3) C(4) 1.385(3) YES C(4) C(5) 1.384(3) YES C(5) C(6) 1.393(3) YES C(6) C(61) 1.481(3) YES C(21) C(26) 1.398(3) YES C(21) C(22) 1.399(3) YES C(22) C(23) 1.392(3) YES C(23) C(24) 1.376(4) YES C(24) C(25) 1.385(4) YES C(25) C(26) 1.381(4) YES C(61) C(66) 1.390(3) YES C(61) C(62) 1.402(3) YES C(62) C(63) 1.394(3) YES C(63) C(64) 1.386(4) YES C(64) C(65) 1.376(4) YES C(65) C(66) 1.391(3) YES C(91) C(92) 1.361(4) YES C(91) C(92) 1.388(4) YES C(92) C(91) 1.361(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ge O(1) 81.89(6) YES O(1) Ge O(1) 81.89(6) YES O(1) Ge O(1) 81.89(6) YES O(1) Ge Li 49.17(4) YES O(1) Ge Li 49.17(4) YES O(1) Ge Li 49.18(4) YES O(1) Li O(1) 79.8(2) YES O(1) Li O(1) 79.8(2) YES O(1) Li O(1) 79.8(2) YES O(1) Li Ge 47.78(15) YES O(1) Li Ge 47.78(15) YES O(1) Li Ge 47.78(15) YES O(1) Li C(62) 153.14(13) YES O(1) Li C(62) 77.31(6) YES O(1) Li C(62) 109.44(7) YES Ge Li C(62) 119.91(14) YES O(1) Li C(62) 109.44(7) YES O(1) Li C(62) 153.14(13) YES O(1) Li C(62) 77.30(6) YES Ge Li C(62) 119.91(14) YES C(62) Li C(62) 97.30(18) YES O(1) Li C(62) 77.30(6) YES O(1) Li C(62) 109.44(7) YES O(1) Li C(62) 153.14(13) YES Ge Li C(62) 119.91(14) YES C(62) Li C(62) 97.29(18) YES C(62) Li C(62) 97.30(18) YES C(1) O(1) Ge 119.98(12) YES C(1) O(1) Li 142.69(16) YES Ge O(1) Li 83.04(16) YES O(1) C(1) C(2) 120.45(17) YES O(1) C(1) C(6) 119.07(18) YES C(2) C(1) C(6) 120.47(18) YES C(3) C(2) C(1) 118.43(18) YES C(3) C(2) C(21) 120.12(18) YES C(1) C(2) C(21) 121.42(17) YES C(4) C(3) C(2) 121.78(19) YES C(5) C(4) C(3) 119.03(19) YES C(4) C(5) C(6) 121.63(19) YES C(5) C(6) C(1) 118.64(19) YES C(5) C(6) C(61) 120.18(18) YES C(1) C(6) C(61) 121.18(18) YES C(26) C(21) C(22) 118.1(2) YES C(26) C(21) C(2) 120.5(2) YES C(22) C(21) C(2) 121.43(19) YES C(23) C(22) C(21) 120.5(2) YES C(24) C(23) C(22) 120.4(2) YES C(23) C(24) C(25) 119.7(2) YES C(26) C(25) C(24) 120.2(2) YES C(25) C(26) C(21) 121.0(2) YES C(66) C(61) C(62) 118.3(2) YES C(66) C(61) C(6) 120.6(2) YES C(62) C(61) C(6) 121.1(2) YES C(63) C(62) C(61) 120.5(2) YES C(63) C(62) Li 102.46(18) YES C(61) C(62) Li 95.89(18) YES C(64) C(63) C(62) 120.0(2) YES C(65) C(64) C(63) 120.0(2) YES C(64) C(65) C(66) 120.2(2) YES C(61) C(66) C(65) 121.0(2) YES C(92) C(91) C(92) 120.3(3) YES C(91) C(92) C(91) 119.7(3) YES #============================================================================== data_SW3329 _database_code_CSD 203292 _audit_creation_date 18-11-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.11 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C60 H45 Ge1 K1 O3' _chemical_formula_moiety 'C54 H39 Ge1 K1 O3,C6 H6' _chemical_formula_structural ? _chemical_formula_weight 925.72 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.7319(3) _cell_length_b 16.9873(3) _cell_length_c 31.0061(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9339.6(3) _cell_measurement_reflns_used 29711 _cell_measurement_theta_min 1 _cell_measurement_theta_max 23 _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.32 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.780 _cell_measurement_temperature 150 _exptl_crystal_F_000 3840 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6241 _exptl_absorpt_correction_T_max 0.9157 _diffrn_reflns_number 29711 _diffrn_measured_fraction_theta_max 0.9952 _diffrn_reflns_theta_full 23.3 _diffrn_measured_fraction_theta_full 0.9952 _reflns_number_total 12809 _reflns_friedl_coverage 0.9345 _reflns_number_gt 11910 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 23.26 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_max 34 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.078 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12796 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0177P)^2^+4.9324P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.35 _refine_diff_density_min -0.33 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.557(7) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ge(1) Ge 0.26162(2) 0.23210(2) 0.015726(13) 0.02517(10) Uani 1 1 d . . . Ge(2) Ge 0.61285(2) 0.27234(2) 0.220068(12) 0.02371(10) Uani 1 1 d . . . K(1) K 0.35220(5) 0.06503(5) -0.01611(3) 0.0316(2) Uani 1 1 d . . . K(2) K 0.50598(5) 0.42816(5) 0.25252(3) 0.0280(2) Uani 1 1 d . . . O(1) O 0.21527(14) 0.14061(15) -0.01021(8) 0.0281(6) Uani 1 1 d . . . O(2) O 0.34169(15) 0.22155(16) -0.02629(8) 0.0261(6) Uani 1 1 d . . . O(3) O 0.31744(15) 0.15953(16) 0.05140(8) 0.0282(6) Uani 1 1 d . . . O(4) O 0.53269(14) 0.26854(14) 0.26221(8) 0.0250(6) Uani 1 1 d . . . O(5) O 0.64769(14) 0.36742(15) 0.24830(8) 0.0246(6) Uani 1 1 d . . . O(6) O 0.54840(14) 0.33973(15) 0.18628(8) 0.0252(6) Uani 1 1 d . . . C(11) C 0.1527(2) 0.1504(2) -0.03446(13) 0.0289(10) Uani 1 1 d . . . C(12) C 0.0858(2) 0.1844(2) -0.01786(14) 0.0317(10) Uani 1 1 d . . . C(13) C 0.0242(2) 0.1955(3) -0.04492(15) 0.0404(11) Uani 1 1 d . . . C(14) C 0.0266(3) 0.1737(3) -0.08819(16) 0.0463(13) Uani 1 1 d . . . C(15) C 0.0914(3) 0.1382(3) -0.10432(14) 0.0404(12) Uani 1 1 d . . . C(16) C 0.1538(2) 0.1248(2) -0.07787(13) 0.0317(10) Uani 1 1 d . . . C(21) C 0.3911(2) 0.2785(2) -0.03741(12) 0.0276(9) Uani 1 1 d . . . C(22) C 0.3682(2) 0.3554(2) -0.04935(13) 0.0299(10) Uani 1 1 d . . . C(23) C 0.4229(3) 0.4110(3) -0.05958(14) 0.0424(12) Uani 1 1 d . . . C(24) C 0.4990(3) 0.3919(3) -0.05960(16) 0.0485(13) Uani 1 1 d . . . C(25) C 0.5213(3) 0.3168(3) -0.04962(14) 0.0433(12) Uani 1 1 d . . . C(26) C 0.4684(2) 0.2597(3) -0.03799(13) 0.0315(10) Uani 1 1 d . . . C(31) C 0.2989(2) 0.1474(3) 0.09349(12) 0.0277(10) Uani 1 1 d . . . C(32) C 0.2906(2) 0.0703(2) 0.10848(13) 0.0294(10) Uani 1 1 d . . . C(33) C 0.2703(2) 0.0574(3) 0.15120(14) 0.0345(11) Uani 1 1 d . . . C(34) C 0.2559(3) 0.1193(3) 0.17874(14) 0.0401(12) Uani 1 1 d . . . C(35) C 0.2655(2) 0.1954(3) 0.16397(14) 0.0367(11) Uani 1 1 d . . . C(36) C 0.2888(2) 0.2121(3) 0.12210(13) 0.0303(10) Uani 1 1 d . . . C(41) C 0.4937(2) 0.2014(2) 0.26931(12) 0.0261(9) Uani 1 1 d . . . C(42) C 0.5300(2) 0.1294(2) 0.27754(12) 0.0276(10) Uani 1 1 d . . . C(43) C 0.4859(3) 0.0619(3) 0.28287(14) 0.0377(11) Uani 1 1 d . . . C(44) C 0.4082(3) 0.0649(3) 0.28218(14) 0.0410(11) Uani 1 1 d . . . C(45) C 0.3731(2) 0.1366(3) 0.27680(13) 0.0354(10) Uani 1 1 d . . . C(46) C 0.4138(2) 0.2048(2) 0.27027(13) 0.0263(9) Uani 1 1 d . . . C(51) C 0.7091(2) 0.3682(2) 0.27436(13) 0.0258(9) Uani 1 1 d . . . C(52) C 0.7012(2) 0.3991(2) 0.31629(13) 0.0274(9) Uani 1 1 d . . . C(53) C 0.7622(2) 0.3988(3) 0.34442(14) 0.0339(10) Uani 1 1 d . . . C(54) C 0.8311(2) 0.3689(3) 0.33149(14) 0.0356(11) Uani 1 1 d . . . C(55) C 0.8394(2) 0.3412(3) 0.28965(14) 0.0340(11) Uani 1 1 d . . . C(56) C 0.7802(2) 0.3408(2) 0.26054(13) 0.0271(10) Uani 1 1 d . . . C(61) C 0.5652(2) 0.3528(2) 0.14400(12) 0.0248(9) Uani 1 1 d . . . C(62) C 0.5711(2) 0.4308(2) 0.12941(13) 0.0277(9) Uani 1 1 d . . . C(63) C 0.5886(2) 0.4460(3) 0.08619(14) 0.0356(11) Uani 1 1 d . . . C(64) C 0.5995(3) 0.3839(3) 0.05776(14) 0.0402(12) Uani 1 1 d . . . C(65) C 0.5924(3) 0.3071(3) 0.07205(14) 0.0368(11) Uani 1 1 d . . . C(66) C 0.5745(2) 0.2897(3) 0.11482(13) 0.0280(10) Uani 1 1 d . . . C(121) C 0.0776(2) 0.2066(3) 0.02841(13) 0.0341(11) Uani 1 1 d . . . C(122) C 0.0412(3) 0.2755(3) 0.04020(17) 0.0507(13) Uani 1 1 d . . . C(123) C 0.0287(3) 0.2938(4) 0.08343(19) 0.0621(16) Uani 1 1 d . . . C(124) C 0.0532(3) 0.2434(4) 0.1160(2) 0.0579(15) Uani 1 1 d . . . C(125) C 0.0893(3) 0.1741(3) 0.10482(15) 0.0464(13) Uani 1 1 d . . . C(126) C 0.1018(2) 0.1559(3) 0.06127(14) 0.0369(11) Uani 1 1 d . . . C(161) C 0.2203(2) 0.0803(2) -0.09418(12) 0.0308(10) Uani 1 1 d . . . C(162) C 0.2332(3) 0.0033(3) -0.08031(14) 0.0391(11) Uani 1 1 d . . . C(163) C 0.2953(3) -0.0392(3) -0.09425(14) 0.0440(12) Uani 1 1 d . . . C(164) C 0.3458(3) -0.0051(3) -0.12277(15) 0.0456(12) Uani 1 1 d . . . C(165) C 0.3333(3) 0.0697(3) -0.13701(16) 0.0492(13) Uani 1 1 d . . . C(166) C 0.2708(3) 0.1120(3) -0.12292(14) 0.0434(12) Uani 1 1 d . . . C(221) C 0.2868(3) 0.3774(2) -0.05198(13) 0.0315(10) Uani 1 1 d . . . C(222) C 0.2351(2) 0.3283(3) -0.07273(13) 0.0329(10) Uani 1 1 d . . . C(223) C 0.1591(3) 0.3466(3) -0.07398(13) 0.0382(11) Uani 1 1 d . . . C(224) C 0.1337(3) 0.4155(3) -0.05550(15) 0.0481(13) Uani 1 1 d . . . C(225) C 0.1848(3) 0.4651(3) -0.03593(17) 0.0593(15) Uani 1 1 d . . . C(226) C 0.2611(3) 0.4465(3) -0.03414(16) 0.0477(13) Uani 1 1 d . . . C(261) C 0.4929(2) 0.1782(3) -0.02802(13) 0.0331(11) Uani 1 1 d . . . C(262) C 0.5086(3) 0.1261(3) -0.06168(16) 0.0490(13) Uani 1 1 d . . . C(263) C 0.5313(3) 0.0496(3) -0.05321(19) 0.0627(15) Uani 1 1 d . . . C(264) C 0.5381(3) 0.0235(3) -0.0114(2) 0.0595(15) Uani 1 1 d . . . C(265) C 0.5228(3) 0.0748(3) 0.02254(17) 0.0482(13) Uani 1 1 d . . . C(266) C 0.4997(2) 0.1509(3) 0.01389(16) 0.0372(10) Uani 1 1 d . . . C(321) C 0.3066(2) 0.0018(2) 0.07932(13) 0.0289(10) Uani 1 1 d . . . C(322) C 0.3768(2) -0.0330(3) 0.07960(14) 0.0394(11) Uani 1 1 d . . . C(323) C 0.3926(3) -0.0973(3) 0.05281(16) 0.0460(12) Uani 1 1 d . . . C(324) C 0.3379(3) -0.1267(3) 0.02626(15) 0.0412(12) Uani 1 1 d . . . C(325) C 0.2667(3) -0.0929(3) 0.02605(14) 0.0375(12) Uani 1 1 d . . . C(326) C 0.2519(2) -0.0289(3) 0.05207(14) 0.0325(10) Uani 1 1 d . . . C(361) C 0.3028(2) 0.2944(3) 0.10846(13) 0.0300(10) Uani 1 1 d . . . C(362) C 0.2504(3) 0.3545(3) 0.11639(14) 0.0363(11) Uani 1 1 d . . . C(363) C 0.2644(3) 0.4306(3) 0.10378(15) 0.0458(13) Uani 1 1 d . . . C(364) C 0.3311(3) 0.4503(3) 0.08243(14) 0.0407(12) Uani 1 1 d . . . C(365) C 0.3839(3) 0.3907(3) 0.07490(14) 0.0372(11) Uani 1 1 d . . . C(366) C 0.3698(2) 0.3141(3) 0.08793(13) 0.0315(10) Uani 1 1 d . . . C(421) C 0.6133(2) 0.1229(2) 0.28183(13) 0.0303(10) Uani 1 1 d . . . C(422) C 0.6526(2) 0.1741(2) 0.30888(13) 0.0295(10) Uani 1 1 d . . . C(423) C 0.7298(2) 0.1676(2) 0.31422(14) 0.0351(10) Uani 1 1 d . . . C(424) C 0.7696(3) 0.1099(3) 0.29299(16) 0.0434(12) Uani 1 1 d . . . C(425) C 0.7315(3) 0.0581(3) 0.26622(16) 0.0465(12) Uani 1 1 d . . . C(426) C 0.6544(2) 0.0646(2) 0.26080(14) 0.0388(11) Uani 1 1 d . . . C(461) C 0.3754(2) 0.2827(2) 0.26684(13) 0.0267(9) Uani 1 1 d . . . C(462) C 0.3695(2) 0.3240(2) 0.22762(13) 0.0298(10) Uani 1 1 d . . . C(463) C 0.3332(2) 0.3966(3) 0.22586(15) 0.0366(11) Uani 1 1 d . . . C(464) C 0.3025(2) 0.4295(3) 0.26322(15) 0.0399(11) Uani 1 1 d . . . C(465) C 0.3070(3) 0.3881(3) 0.30134(15) 0.0439(12) Uani 1 1 d . . . C(466) C 0.3422(2) 0.3160(3) 0.30316(14) 0.0395(11) Uani 1 1 d . . . C(521) C 0.6260(2) 0.4300(2) 0.32983(12) 0.0268(9) Uani 1 1 d . . . C(522) C 0.5701(2) 0.3792(3) 0.34528(13) 0.0325(10) Uani 1 1 d . . . C(523) C 0.4983(2) 0.4067(3) 0.35567(13) 0.0365(11) Uani 1 1 d . . . C(524) C 0.4808(3) 0.4845(3) 0.35018(14) 0.0377(11) Uani 1 1 d . . . C(525) C 0.5346(3) 0.5359(3) 0.33505(14) 0.0389(11) Uani 1 1 d . . . C(526) C 0.6067(2) 0.5091(3) 0.32469(13) 0.0335(11) Uani 1 1 d . . . C(561) C 0.7926(2) 0.3128(2) 0.21542(15) 0.0305(10) Uani 1 1 d . . . C(562) C 0.7662(2) 0.3562(3) 0.18000(14) 0.0333(11) Uani 1 1 d . . . C(563) C 0.7788(3) 0.3306(3) 0.13837(15) 0.0458(13) Uani 1 1 d . . . C(564) C 0.8190(3) 0.2638(3) 0.13024(17) 0.0537(14) Uani 1 1 d . . . C(565) C 0.8451(3) 0.2200(3) 0.16485(18) 0.0540(14) Uani 1 1 d . . . C(566) C 0.8325(3) 0.2438(3) 0.20682(16) 0.0429(12) Uani 1 1 d . . . C(621) C 0.5568(2) 0.4973(2) 0.15984(13) 0.0272(10) Uani 1 1 d . . . C(622) C 0.4836(3) 0.5276(3) 0.16392(14) 0.0376(11) Uani 1 1 d . . . C(623) C 0.4685(3) 0.5890(3) 0.19205(15) 0.0408(11) Uani 1 1 d . . . C(624) C 0.5256(2) 0.6212(2) 0.21701(15) 0.0367(10) Uani 1 1 d . . . C(625) C 0.5980(2) 0.5924(2) 0.21301(15) 0.0347(11) Uani 1 1 d . . . C(626) C 0.6131(2) 0.5310(2) 0.18477(13) 0.0297(10) Uani 1 1 d . . . C(661) C 0.5618(2) 0.2065(3) 0.12809(13) 0.0271(10) Uani 1 1 d . . . C(662) C 0.6160(2) 0.1488(3) 0.11994(15) 0.0373(11) Uani 1 1 d . . . C(663) C 0.6039(3) 0.0712(3) 0.13366(15) 0.0417(12) Uani 1 1 d . . . C(664) C 0.5380(3) 0.0515(3) 0.15464(14) 0.0392(12) Uani 1 1 d . . . C(665) C 0.4837(3) 0.1073(3) 0.16229(14) 0.0374(11) Uani 1 1 d . . . C(666) C 0.4958(2) 0.1843(2) 0.14917(12) 0.0286(10) Uani 1 1 d . . . C(911) C 0.6423(3) 0.7702(3) 0.27664(19) 0.0558(15) Uani 1 1 d . . . C(912) C 0.6243(3) 0.7380(3) 0.31582(19) 0.0549(14) Uani 1 1 d . . . C(913) C 0.5559(4) 0.7516(3) 0.33399(18) 0.0587(15) Uani 1 1 d . . . C(914) C 0.5041(3) 0.7985(4) 0.3128(2) 0.0643(17) Uani 1 1 d . . . C(915) C 0.5214(3) 0.8315(3) 0.2728(2) 0.0601(16) Uani 1 1 d . . . C(916) C 0.5922(4) 0.8159(3) 0.25563(19) 0.0623(15) Uani 1 1 d . . . C(921) C 0.2506(3) -0.2633(4) -0.0560(2) 0.0630(16) Uani 1 1 d . . . C(922) C 0.3197(3) -0.2848(4) -0.07217(19) 0.0649(16) Uani 1 1 d . . . C(923) C 0.3668(4) -0.3327(4) -0.04928(18) 0.0634(16) Uani 1 1 d . . . C(924) C 0.3484(4) -0.3571(3) -0.0081(2) 0.0696(17) Uani 1 1 d . . . C(925) C 0.2784(4) -0.3355(4) 0.00824(19) 0.0761(19) Uani 1 1 d . . . C(926) C 0.2299(3) -0.2879(4) -0.01609(19) 0.0616(16) Uani 1 1 d . . . H(13) H -0.0204 0.2185 -0.0336 0.049 Uiso 1 1 calc R . . H(14) H -0.0155 0.1830 -0.1065 0.056 Uiso 1 1 calc R . . H(15) H 0.0932 0.1228 -0.1338 0.048 Uiso 1 1 calc R . . H(23) H 0.4079 0.4631 -0.0667 0.051 Uiso 1 1 calc R . . H(24) H 0.5355 0.4308 -0.0665 0.058 Uiso 1 1 calc R . . H(25) H 0.5733 0.3034 -0.0506 0.052 Uiso 1 1 calc R . . H(33) H 0.2664 0.0050 0.1616 0.041 Uiso 1 1 calc R . . H(34) H 0.2395 0.1097 0.2074 0.048 Uiso 1 1 calc R . . H(35) H 0.2558 0.2379 0.1831 0.044 Uiso 1 1 calc R . . H(43) H 0.5101 0.0126 0.2871 0.045 Uiso 1 1 calc R . . H(44) H 0.3792 0.0182 0.2854 0.049 Uiso 1 1 calc R . . H(45) H 0.3196 0.1391 0.2776 0.043 Uiso 1 1 calc R . . H(53) H 0.7565 0.4194 0.3727 0.041 Uiso 1 1 calc R . . H(54) H 0.8723 0.3673 0.3510 0.043 Uiso 1 1 calc R . . H(55) H 0.8872 0.3219 0.2807 0.041 Uiso 1 1 calc R . . H(63) H 0.5930 0.4987 0.0763 0.043 Uiso 1 1 calc R . . H(64) H 0.6118 0.3942 0.0285 0.048 Uiso 1 1 calc R . . H(65) H 0.6000 0.2651 0.0523 0.044 Uiso 1 1 calc R . . H(122) H 0.0245 0.3108 0.0185 0.061 Uiso 1 1 calc R . . H(123) H 0.0032 0.3411 0.0908 0.075 Uiso 1 1 calc R . . H(124) H 0.0453 0.2564 0.1454 0.070 Uiso 1 1 calc R . . H(125) H 0.1056 0.1388 0.1267 0.056 Uiso 1 1 calc R . . H(126) H 0.1271 0.1084 0.0539 0.044 Uiso 1 1 calc R . . H(162) H 0.1894 -0.0267 -0.0684 0.047 Uiso 1 1 calc R . . H(163) H 0.2949 -0.0978 -0.0911 0.053 Uiso 1 1 calc R . . H(164) H 0.3888 -0.0336 -0.1323 0.055 Uiso 1 1 calc R . . H(165) H 0.3675 0.0932 -0.1568 0.059 Uiso 1 1 calc R . . H(166) H 0.2629 0.1639 -0.1334 0.052 Uiso 1 1 calc R . . H(222) H 0.2524 0.2815 -0.0862 0.039 Uiso 1 1 calc R . . H(223) H 0.1245 0.3118 -0.0875 0.046 Uiso 1 1 calc R . . H(224) H 0.0816 0.4286 -0.0563 0.058 Uiso 1 1 calc R . . H(225) H 0.1676 0.5129 -0.0234 0.071 Uiso 1 1 calc R . . H(226) H 0.2955 0.4816 -0.0206 0.057 Uiso 1 1 calc R . . H(262) H 0.5075 0.1454 -0.0921 0.059 Uiso 1 1 calc R . . H(263) H 0.5422 0.0150 -0.0764 0.075 Uiso 1 1 calc R . . H(264) H 0.5532 -0.0291 -0.0058 0.071 Uiso 1 1 calc R . . H(265) H 0.5330 0.0582 0.0529 0.058 Uiso 1 1 calc R . . H(266) H 0.4966 0.1894 0.0382 0.045 Uiso 1 1 calc R . . H(322) H 0.4149 -0.0131 0.0982 0.047 Uiso 1 1 calc R . . H(323) H 0.4413 -0.1204 0.0531 0.055 Uiso 1 1 calc R . . H(324) H 0.3486 -0.1702 0.0080 0.049 Uiso 1 1 calc R . . H(325) H 0.2246 -0.1189 0.0100 0.045 Uiso 1 1 calc R . . H(326) H 0.1983 -0.0125 0.0564 0.039 Uiso 1 1 calc R . . H(362) H 0.2045 0.3424 0.1307 0.044 Uiso 1 1 calc R . . H(363) H 0.2282 0.4704 0.1097 0.055 Uiso 1 1 calc R . . H(364) H 0.3404 0.5028 0.0733 0.049 Uiso 1 1 calc R . . H(365) H 0.4299 0.4029 0.0607 0.045 Uiso 1 1 calc R . . H(366) H 0.4065 0.2745 0.0828 0.038 Uiso 1 1 calc R . . H(422) H 0.6259 0.2141 0.3239 0.035 Uiso 1 1 calc R . . H(423) H 0.7555 0.2033 0.3327 0.042 Uiso 1 1 calc R . . H(424) H 0.8227 0.1056 0.2967 0.052 Uiso 1 1 calc R . . H(425) H 0.7585 0.0180 0.2515 0.056 Uiso 1 1 calc R . . H(426) H 0.6290 0.0286 0.2424 0.047 Uiso 1 1 calc R . . H(462) H 0.3730 0.2929 0.2003 0.036 Uiso 1 1 calc R . . H(463) H 0.3151 0.4162 0.1973 0.044 Uiso 1 1 calc R . . H(464) H 0.2788 0.4796 0.2624 0.048 Uiso 1 1 calc R . . H(465) H 0.2855 0.4096 0.3268 0.053 Uiso 1 1 calc R . . H(466) H 0.3440 0.2884 0.3298 0.047 Uiso 1 1 calc R . . H(522) H 0.5830 0.3229 0.3510 0.039 Uiso 1 1 calc R . . H(523) H 0.4605 0.3700 0.3686 0.044 Uiso 1 1 calc R . . H(524) H 0.4304 0.5048 0.3595 0.045 Uiso 1 1 calc R . . H(525) H 0.5232 0.5935 0.3337 0.047 Uiso 1 1 calc R . . H(526) H 0.6464 0.5478 0.3161 0.040 Uiso 1 1 calc R . . H(562) H 0.7393 0.4038 0.1847 0.040 Uiso 1 1 calc R . . H(563) H 0.7591 0.3601 0.1149 0.055 Uiso 1 1 calc R . . H(564) H 0.8290 0.2477 0.1015 0.064 Uiso 1 1 calc R . . H(565) H 0.8721 0.1727 0.1596 0.065 Uiso 1 1 calc R . . H(566) H 0.8512 0.2130 0.2300 0.052 Uiso 1 1 calc R . . H(622) H 0.4438 0.5058 0.1472 0.045 Uiso 1 1 calc R . . H(623) H 0.4187 0.6092 0.1942 0.049 Uiso 1 1 calc R . . H(624) H 0.5149 0.6626 0.2367 0.044 Uiso 1 1 calc R . . H(625) H 0.6377 0.6146 0.2296 0.042 Uiso 1 1 calc R . . H(626) H 0.6632 0.5116 0.1825 0.036 Uiso 1 1 calc R . . H(662) H 0.6611 0.1621 0.1051 0.045 Uiso 1 1 calc R . . H(663) H 0.6411 0.0321 0.1285 0.050 Uiso 1 1 calc R . . H(664) H 0.5301 -0.0012 0.1639 0.047 Uiso 1 1 calc R . . H(665) H 0.4382 0.0933 0.1765 0.045 Uiso 1 1 calc R . . H(666) H 0.4582 0.2228 0.1547 0.034 Uiso 1 1 calc R . . H(911) H 0.6903 0.7603 0.2642 0.067 Uiso 1 1 calc R . . H(912) H 0.6600 0.7059 0.3304 0.066 Uiso 1 1 calc R . . H(913) H 0.5437 0.7291 0.3611 0.070 Uiso 1 1 calc R . . H(914) H 0.4563 0.8083 0.3256 0.077 Uiso 1 1 calc R . . H(915) H 0.4861 0.8635 0.2579 0.072 Uiso 1 1 calc R . . H(916) H 0.6055 0.8378 0.2285 0.075 Uiso 1 1 calc R . . H(921) H 0.2175 -0.2314 -0.0727 0.076 Uiso 1 1 calc R . . H(922) H 0.3350 -0.2661 -0.0997 0.078 Uiso 1 1 calc R . . H(923) H 0.4129 -0.3494 -0.0619 0.076 Uiso 1 1 calc R . . H(924) H 0.3826 -0.3878 0.0085 0.084 Uiso 1 1 calc R . . H(925) H 0.2634 -0.3530 0.0360 0.091 Uiso 1 1 calc R . . H(926) H 0.1824 -0.2729 -0.0046 0.074 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge(1) 0.0262(2) 0.0247(2) 0.0246(2) 0.00105(18) -0.0006(2) -0.0028(2) Ge(2) 0.0233(2) 0.0222(2) 0.0256(2) 0.00124(17) -0.00042(18) -0.0017(2) K(1) 0.0314(5) 0.0266(5) 0.0369(5) 0.0008(4) 0.0035(4) -0.0035(4) K(2) 0.0291(5) 0.0261(5) 0.0287(5) 0.0030(4) -0.0012(4) -0.0034(4) O(1) 0.0274(16) 0.0277(16) 0.0291(15) -0.0009(12) -0.0021(13) -0.0052(13) O(2) 0.0289(15) 0.0217(16) 0.0277(15) -0.0006(12) 0.0035(12) 0.0011(12) O(3) 0.0312(16) 0.0294(16) 0.0240(15) 0.0020(13) -0.0017(12) 0.0006(12) O(4) 0.0233(14) 0.0218(15) 0.0299(14) -0.0011(12) 0.0023(12) 0.0010(12) O(5) 0.0214(14) 0.0238(16) 0.0288(14) 0.0003(11) -0.0046(13) -0.0043(12) O(6) 0.0268(15) 0.0272(16) 0.0216(14) 0.0026(12) -0.0033(12) -0.0026(12) C(11) 0.030(2) 0.025(2) 0.032(2) -0.0070(19) -0.003(2) 0.0006(18) C(12) 0.027(2) 0.031(3) 0.038(2) -0.0042(19) -0.001(2) 0.000(2) C(13) 0.027(2) 0.047(3) 0.048(3) 0.004(2) -0.006(2) 0.007(2) C(14) 0.035(3) 0.052(3) 0.052(3) -0.009(2) -0.013(2) 0.011(3) C(15) 0.045(3) 0.045(3) 0.031(2) -0.013(2) -0.009(2) 0.003(2) C(16) 0.036(2) 0.033(3) 0.026(2) -0.011(2) -0.002(2) 0.0030(19) C(21) 0.032(2) 0.029(2) 0.022(2) -0.0095(19) -0.0007(18) 0.0004(18) C(22) 0.037(2) 0.025(2) 0.028(2) -0.003(2) -0.0043(19) 0.0000(19) C(23) 0.055(3) 0.030(3) 0.042(3) -0.005(2) -0.010(2) 0.013(2) C(24) 0.048(3) 0.046(3) 0.052(3) -0.018(3) -0.005(2) 0.010(2) C(25) 0.035(3) 0.048(3) 0.046(3) -0.010(2) -0.001(2) 0.011(2) C(26) 0.031(2) 0.033(3) 0.030(2) -0.003(2) -0.0028(19) 0.005(2) C(31) 0.023(2) 0.035(3) 0.025(2) -0.0032(19) -0.0016(18) -0.0034(19) C(32) 0.030(2) 0.029(3) 0.029(2) -0.0031(19) -0.0015(18) -0.0035(19) C(33) 0.035(3) 0.036(3) 0.033(3) -0.007(2) -0.002(2) 0.003(2) C(34) 0.042(3) 0.053(3) 0.025(2) -0.010(2) 0.000(2) 0.005(2) C(35) 0.036(3) 0.045(3) 0.029(2) -0.004(2) -0.001(2) -0.009(2) C(36) 0.032(2) 0.032(3) 0.027(2) 0.0008(19) -0.0042(19) -0.0024(19) C(41) 0.033(2) 0.023(2) 0.023(2) -0.0050(19) -0.0044(18) -0.0040(18) C(42) 0.031(2) 0.025(2) 0.026(2) -0.0032(19) -0.0038(18) 0.0003(17) C(43) 0.049(3) 0.023(2) 0.041(2) 0.002(2) -0.008(2) -0.002(2) C(44) 0.041(3) 0.031(3) 0.050(3) -0.015(2) -0.007(2) 0.006(2) C(45) 0.034(2) 0.037(3) 0.035(2) -0.009(2) -0.0026(19) 0.001(2) C(46) 0.027(2) 0.027(2) 0.025(2) -0.0012(19) -0.0038(18) -0.0022(18) C(51) 0.025(2) 0.020(2) 0.033(2) -0.0046(17) -0.0005(19) 0.0012(18) C(52) 0.024(2) 0.023(2) 0.034(2) -0.0060(17) 0.0009(19) -0.0007(19) C(53) 0.036(3) 0.036(3) 0.030(2) -0.008(2) -0.003(2) 0.000(2) C(54) 0.027(2) 0.039(3) 0.041(3) -0.003(2) -0.010(2) 0.005(2) C(55) 0.024(2) 0.030(3) 0.048(3) 0.0016(19) 0.001(2) 0.001(2) C(56) 0.023(2) 0.024(2) 0.034(2) -0.0014(17) -0.0002(19) 0.0059(19) C(61) 0.020(2) 0.032(3) 0.022(2) -0.0022(17) -0.0005(17) -0.0009(18) C(62) 0.027(2) 0.027(2) 0.029(2) -0.0028(18) 0.0009(18) -0.0021(19) C(63) 0.038(3) 0.037(3) 0.032(3) -0.008(2) 0.006(2) 0.000(2) C(64) 0.049(3) 0.044(3) 0.028(2) -0.012(2) 0.009(2) -0.005(2) C(65) 0.045(3) 0.037(3) 0.028(2) -0.008(2) 0.006(2) -0.009(2) C(66) 0.023(2) 0.031(3) 0.029(2) -0.0045(19) 0.0025(19) -0.004(2) C(121) 0.022(2) 0.040(3) 0.041(3) -0.0045(19) 0.0058(19) -0.006(2) C(122) 0.044(3) 0.044(3) 0.065(3) 0.006(2) 0.009(3) -0.003(3) C(123) 0.063(4) 0.055(4) 0.068(4) 0.007(3) 0.018(3) -0.030(3) C(124) 0.049(3) 0.075(4) 0.049(3) -0.003(3) 0.012(3) -0.025(3) C(125) 0.036(3) 0.063(4) 0.040(3) -0.009(2) 0.001(2) -0.008(3) C(126) 0.029(2) 0.043(3) 0.039(3) -0.002(2) 0.003(2) -0.006(2) C(161) 0.039(3) 0.031(3) 0.023(2) -0.008(2) -0.0017(19) -0.0073(19) C(162) 0.047(3) 0.032(3) 0.039(3) -0.012(2) 0.003(2) -0.004(2) C(163) 0.066(3) 0.026(3) 0.040(3) 0.000(2) 0.008(2) -0.005(2) C(164) 0.049(3) 0.040(3) 0.048(3) -0.002(2) 0.016(2) -0.016(2) C(165) 0.058(3) 0.039(3) 0.051(3) -0.008(2) 0.026(3) -0.005(2) C(166) 0.060(3) 0.031(3) 0.039(3) -0.009(2) 0.011(2) -0.003(2) C(221) 0.045(3) 0.021(2) 0.029(2) -0.001(2) -0.005(2) -0.0003(18) C(222) 0.041(3) 0.029(2) 0.029(2) 0.006(2) -0.003(2) -0.0012(19) C(223) 0.049(3) 0.033(3) 0.033(2) 0.004(2) -0.009(2) 0.001(2) C(224) 0.045(3) 0.048(3) 0.051(3) 0.019(3) -0.010(2) -0.006(3) C(225) 0.063(4) 0.042(3) 0.074(4) 0.024(3) -0.012(3) -0.021(3) C(226) 0.055(3) 0.037(3) 0.051(3) -0.002(2) -0.013(2) -0.007(2) C(261) 0.015(2) 0.037(3) 0.047(3) -0.0011(18) 0.0066(19) 0.002(2) C(262) 0.050(3) 0.050(3) 0.047(3) 0.008(3) 0.009(2) 0.003(3) C(263) 0.061(4) 0.054(4) 0.072(4) 0.019(3) 0.017(3) -0.010(3) C(264) 0.044(3) 0.043(3) 0.092(4) 0.015(2) -0.005(3) 0.007(3) C(265) 0.039(3) 0.049(3) 0.057(3) -0.002(2) -0.015(2) 0.014(3) C(266) 0.035(2) 0.035(3) 0.041(2) -0.0086(19) -0.010(2) 0.007(2) C(321) 0.033(2) 0.024(2) 0.029(2) -0.0015(19) 0.0017(19) 0.0060(18) C(322) 0.036(3) 0.040(3) 0.043(3) 0.002(2) -0.005(2) -0.003(2) C(323) 0.037(3) 0.042(3) 0.060(3) 0.007(2) 0.003(2) -0.002(3) C(324) 0.049(3) 0.028(3) 0.046(3) 0.002(2) 0.009(2) -0.001(2) C(325) 0.040(3) 0.028(2) 0.045(3) -0.008(2) 0.002(2) -0.001(2) C(326) 0.031(2) 0.033(3) 0.034(2) 0.000(2) 0.0026(19) 0.002(2) C(361) 0.031(2) 0.030(3) 0.029(2) -0.002(2) -0.0069(19) -0.0090(19) C(362) 0.035(3) 0.043(3) 0.031(3) 0.002(2) 0.000(2) -0.004(2) C(363) 0.055(3) 0.039(3) 0.044(3) 0.016(2) 0.000(2) -0.006(2) C(364) 0.049(3) 0.030(3) 0.043(3) -0.002(2) -0.006(2) 0.000(2) C(365) 0.037(3) 0.038(3) 0.037(2) -0.003(2) -0.007(2) -0.001(2) C(366) 0.029(2) 0.035(3) 0.031(2) 0.001(2) -0.0058(19) -0.006(2) C(421) 0.040(3) 0.022(2) 0.029(2) 0.0019(19) -0.0042(19) 0.0049(19) C(422) 0.036(3) 0.024(2) 0.029(2) 0.0059(19) -0.001(2) 0.0014(19) C(423) 0.039(3) 0.027(2) 0.040(3) -0.002(2) -0.009(2) 0.001(2) C(424) 0.033(3) 0.039(3) 0.058(3) 0.005(2) -0.007(2) -0.002(3) C(425) 0.043(3) 0.039(3) 0.057(3) 0.016(2) -0.003(2) -0.011(3) C(426) 0.043(3) 0.026(2) 0.047(3) 0.003(2) -0.009(2) -0.010(2) C(461) 0.017(2) 0.032(2) 0.031(2) -0.0057(17) -0.0023(18) -0.002(2) C(462) 0.028(2) 0.034(2) 0.028(2) 0.0000(18) -0.0051(18) 0.0021(19) C(463) 0.028(2) 0.041(3) 0.040(3) 0.003(2) -0.005(2) 0.001(2) C(464) 0.030(2) 0.032(2) 0.059(3) 0.005(2) -0.005(2) -0.006(2) C(465) 0.040(3) 0.048(3) 0.044(3) 0.006(2) 0.000(2) -0.018(2) C(466) 0.038(3) 0.044(3) 0.037(3) 0.004(2) -0.002(2) 0.000(2) C(521) 0.030(2) 0.031(2) 0.020(2) -0.0061(18) -0.0026(17) -0.0017(18) C(522) 0.034(3) 0.031(3) 0.032(2) 0.001(2) 0.0037(19) 0.0031(19) C(523) 0.037(3) 0.038(3) 0.034(2) -0.005(2) 0.006(2) 0.001(2) C(524) 0.039(3) 0.038(3) 0.037(2) 0.003(2) 0.010(2) -0.008(2) C(525) 0.044(3) 0.029(3) 0.043(3) 0.002(2) 0.003(2) -0.007(2) C(526) 0.037(3) 0.027(3) 0.036(2) -0.0053(19) 0.002(2) -0.005(2) C(561) 0.017(2) 0.028(2) 0.046(3) -0.0040(17) 0.003(2) -0.001(2) C(562) 0.030(3) 0.035(3) 0.035(3) 0.003(2) 0.008(2) 0.001(2) C(563) 0.043(3) 0.060(4) 0.034(3) 0.006(3) 0.005(2) 0.003(2) C(564) 0.057(3) 0.064(4) 0.039(3) 0.004(3) 0.009(3) -0.010(3) C(565) 0.049(3) 0.046(3) 0.067(4) 0.015(3) 0.014(3) -0.013(3) C(566) 0.041(3) 0.036(3) 0.052(3) 0.009(2) 0.009(2) 0.006(2) C(621) 0.031(2) 0.023(2) 0.028(2) 0.0015(18) 0.0027(19) 0.0071(18) C(622) 0.033(3) 0.035(3) 0.044(3) 0.001(2) -0.002(2) 0.000(2) C(623) 0.034(3) 0.035(3) 0.053(3) 0.009(2) 0.004(2) -0.002(2) C(624) 0.046(3) 0.025(2) 0.038(2) -0.001(2) 0.007(2) -0.006(2) C(625) 0.038(3) 0.027(2) 0.039(3) -0.0028(19) -0.002(2) -0.002(2) C(626) 0.028(2) 0.028(2) 0.034(2) 0.0027(18) 0.0013(19) -0.002(2) C(661) 0.027(2) 0.033(3) 0.021(2) 0.0005(19) -0.0030(18) -0.0083(19) C(662) 0.035(3) 0.038(3) 0.039(3) 0.003(2) 0.004(2) -0.013(2) C(663) 0.045(3) 0.036(3) 0.044(3) 0.012(2) -0.007(2) -0.009(2) C(664) 0.048(3) 0.032(3) 0.037(3) 0.001(2) -0.002(2) 0.000(2) C(665) 0.040(3) 0.038(3) 0.034(2) -0.002(2) -0.002(2) -0.004(2) C(666) 0.030(2) 0.028(3) 0.028(2) -0.0011(19) 0.0010(19) -0.0016(18) C(911) 0.044(3) 0.056(4) 0.067(4) -0.012(3) 0.007(3) -0.022(3) C(912) 0.064(4) 0.033(3) 0.068(4) -0.004(3) -0.008(3) -0.020(3) C(913) 0.079(4) 0.041(3) 0.056(3) -0.016(3) 0.011(3) -0.016(3) C(914) 0.047(3) 0.061(4) 0.086(5) -0.015(3) 0.016(3) -0.038(4) C(915) 0.062(4) 0.040(3) 0.079(4) -0.005(3) -0.021(3) -0.014(3) C(916) 0.082(4) 0.052(4) 0.053(3) -0.029(3) 0.001(3) -0.007(3) C(921) 0.059(4) 0.072(4) 0.058(4) -0.016(3) 0.009(3) -0.017(3) C(922) 0.071(4) 0.073(4) 0.050(3) -0.007(3) 0.014(3) -0.010(3) C(923) 0.076(4) 0.062(4) 0.053(4) -0.013(3) 0.008(3) -0.008(3) C(924) 0.077(4) 0.057(4) 0.075(4) -0.032(3) 0.005(4) -0.003(3) C(925) 0.089(5) 0.093(5) 0.046(3) -0.048(4) 0.011(4) 0.000(3) C(926) 0.059(4) 0.073(4) 0.052(4) -0.027(3) 0.016(3) -0.013(3) # 10. MOLECULAR GEOMETRY _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_publ_flag Ge(1) O(3) 1.929(3) YES Ge(1) O(1) 1.933(3) YES Ge(1) O(2) 1.935(3) YES Ge(1) K(1) 3.4071(10) YES Ge(2) O(6) 1.927(3) YES Ge(2) O(4) 1.932(3) YES Ge(2) O(5) 1.938(3) YES Ge(2) K(2) 3.4073(9) YES K(1) O(2) 2.684(3) YES K(1) O(3) 2.709(3) YES K(1) O(1) 2.753(3) YES K(1) C(162) 3.085(4) YES K(1) C(266) 3.135(4) YES K(1) C(163) 3.166(5) YES K(1) C(261) 3.171(4) YES K(1) C(326) 3.190(4) YES K(1) C(321) 3.250(4) YES K(1) C(265) 3.259(5) YES K(1) C(262) 3.281(5) YES K(1) C(325) 3.347(4) YES K(2) O(6) 2.653(3) YES K(2) O(5) 2.719(3) YES K(2) O(4) 2.769(3) YES K(2) C(462) 3.097(4) YES K(2) C(526) 3.177(4) YES K(2) C(525) 3.187(4) YES K(2) C(522) 3.202(4) YES K(2) C(521) 3.206(4) YES K(2) C(524) 3.207(4) YES K(2) C(463) 3.219(4) YES K(2) C(523) 3.222(4) YES K(2) C(621) 3.232(4) YES O(1) C(11) 1.350(5) YES O(2) C(21) 1.350(5) YES O(3) C(31) 1.361(5) YES O(4) C(41) 1.351(5) YES O(5) C(51) 1.356(5) YES O(6) C(61) 1.362(5) YES C(11) C(16) 1.414(6) YES C(11) C(12) 1.416(6) YES C(12) C(13) 1.390(6) YES C(12) C(121) 1.491(6) YES C(13) C(14) 1.392(6) YES C(14) C(15) 1.391(7) YES C(15) C(16) 1.396(6) YES C(16) C(161) 1.489(6) YES C(21) C(26) 1.409(6) YES C(21) C(22) 1.416(6) YES C(22) C(23) 1.391(6) YES C(22) C(221) 1.493(6) YES C(23) C(24) 1.387(7) YES C(24) C(25) 1.371(7) YES C(25) C(26) 1.395(6) YES C(26) C(261) 1.484(6) YES C(31) C(32) 1.398(6) YES C(31) C(36) 1.423(6) YES C(32) C(33) 1.390(6) YES C(32) C(321) 1.502(6) YES C(33) C(34) 1.378(6) YES C(34) C(35) 1.383(6) YES C(35) C(36) 1.392(6) YES C(36) C(361) 1.482(6) YES C(41) C(42) 1.406(6) YES C(41) C(46) 1.419(5) YES C(42) C(43) 1.397(6) YES C(42) C(421) 1.488(6) YES C(43) C(44) 1.379(6) YES C(44) C(45) 1.377(6) YES C(45) C(46) 1.379(6) YES C(46) C(461) 1.492(6) YES C(51) C(52) 1.409(6) YES C(51) C(56) 1.411(5) YES C(52) C(53) 1.390(6) YES C(52) C(521) 1.493(6) YES C(53) C(54) 1.383(6) YES C(54) C(55) 1.388(6) YES C(55) C(56) 1.384(6) YES C(56) C(561) 1.494(6) YES C(61) C(62) 1.405(6) YES C(61) C(66) 1.412(6) YES C(62) C(63) 1.399(6) YES C(62) C(621) 1.493(6) YES C(63) C(64) 1.388(6) YES C(64) C(65) 1.384(6) YES C(65) C(66) 1.395(6) YES C(66) C(661) 1.490(5) YES C(121) C(122) 1.385(6) YES C(121) C(126) 1.403(6) YES C(122) C(123) 1.394(7) YES C(123) C(124) 1.394(8) YES C(124) C(125) 1.384(8) YES C(125) C(126) 1.403(6) YES C(161) C(166) 1.373(6) YES C(161) C(162) 1.395(6) YES C(162) C(163) 1.386(6) YES C(163) C(164) 1.386(6) YES C(164) C(165) 1.363(7) YES C(165) C(166) 1.391(7) YES C(221) C(226) 1.376(6) YES C(221) C(222) 1.397(6) YES C(222) C(223) 1.383(6) YES C(223) C(224) 1.379(6) YES C(224) C(225) 1.378(7) YES C(225) C(226) 1.391(7) YES C(261) C(266) 1.385(6) YES C(261) C(262) 1.397(6) YES C(262) C(263) 1.385(7) YES C(263) C(264) 1.374(8) YES C(264) C(265) 1.394(7) YES C(265) C(266) 1.382(6) YES C(321) C(322) 1.378(6) YES C(321) C(326) 1.388(6) YES C(322) C(323) 1.400(6) YES C(323) C(324) 1.367(6) YES C(324) C(325) 1.388(6) YES C(325) C(326) 1.378(6) YES C(361) C(366) 1.389(6) YES C(361) C(362) 1.402(6) YES C(362) C(363) 1.373(7) YES C(363) C(364) 1.396(7) YES C(364) C(365) 1.399(6) YES C(365) C(366) 1.385(6) YES C(421) C(426) 1.392(6) YES C(421) C(422) 1.395(6) YES C(422) C(423) 1.384(6) YES C(423) C(424) 1.377(6) YES C(424) C(425) 1.386(6) YES C(425) C(426) 1.381(6) YES C(461) C(466) 1.391(6) YES C(461) C(462) 1.408(5) YES C(462) C(463) 1.393(6) YES C(463) C(464) 1.396(6) YES C(464) C(465) 1.378(6) YES C(465) C(466) 1.375(6) YES C(521) C(526) 1.395(6) YES C(521) C(522) 1.399(6) YES C(522) C(523) 1.393(6) YES C(523) C(524) 1.369(6) YES C(524) C(525) 1.377(6) YES C(525) C(526) 1.395(6) YES C(561) C(566) 1.394(6) YES C(561) C(562) 1.404(6) YES C(562) C(563) 1.381(6) YES C(563) C(564) 1.364(7) YES C(564) C(565) 1.385(7) YES C(565) C(566) 1.381(7) YES C(621) C(626) 1.387(6) YES C(621) C(622) 1.402(6) YES C(622) C(623) 1.386(6) YES C(623) C(624) 1.386(6) YES C(624) C(625) 1.380(6) YES C(625) C(626) 1.388(6) YES C(661) C(666) 1.392(6) YES C(661) C(662) 1.396(6) YES C(662) C(663) 1.402(7) YES C(663) C(664) 1.379(7) YES C(664) C(665) 1.371(6) YES C(665) C(666) 1.387(6) YES C(911) C(916) 1.347(8) YES C(911) C(912) 1.370(8) YES C(912) C(913) 1.357(8) YES C(913) C(914) 1.382(8) YES C(914) C(915) 1.394(8) YES C(915) C(916) 1.389(8) YES C(921) C(926) 1.358(8) YES C(921) C(922) 1.374(8) YES C(922) C(923) 1.365(8) YES C(923) C(924) 1.382(8) YES C(924) C(925) 1.391(8) YES C(925) C(926) 1.401(9) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(3) Ge(1) O(1) 86.72(11) YES O(3) Ge(1) O(2) 87.15(11) YES O(1) Ge(1) O(2) 87.56(11) YES O(3) Ge(1) K(1) 52.56(8) YES O(1) Ge(1) K(1) 53.86(8) YES O(2) Ge(1) K(1) 51.83(8) YES O(6) Ge(2) O(4) 87.21(11) YES O(6) Ge(2) O(5) 86.53(11) YES O(4) Ge(2) O(5) 87.53(11) YES O(6) Ge(2) K(2) 50.90(8) YES O(4) Ge(2) K(2) 54.34(8) YES O(5) Ge(2) K(2) 52.88(7) YES O(2) K(1) O(3) 59.21(8) YES O(2) K(1) O(1) 58.97(8) YES O(3) K(1) O(1) 58.10(8) YES O(2) K(1) C(162) 102.31(10) YES O(3) K(1) C(162) 122.97(11) YES O(1) K(1) C(162) 66.28(10) YES O(2) K(1) C(266) 68.41(10) YES O(3) K(1) C(266) 71.64(11) YES O(1) K(1) C(266) 119.94(10) YES C(162) K(1) C(266) 156.95(13) YES O(2) K(1) C(163) 116.22(11) YES O(3) K(1) C(163) 148.23(11) YES O(1) K(1) C(163) 91.75(11) YES C(162) K(1) C(163) 25.59(12) YES C(266) K(1) C(163) 138.85(13) YES O(2) K(1) C(261) 55.98(10) YES O(3) K(1) C(261) 84.82(10) YES O(1) K(1) C(261) 114.78(10) YES C(162) K(1) C(261) 132.00(12) YES C(266) K(1) C(261) 25.36(11) YES C(163) K(1) C(261) 120.05(12) YES O(2) K(1) C(326) 122.34(10) YES O(3) K(1) C(326) 69.98(10) YES O(1) K(1) C(326) 72.40(10) YES C(162) K(1) C(326) 82.89(12) YES C(266) K(1) C(326) 120.06(12) YES C(163) K(1) C(326) 92.84(12) YES C(261) K(1) C(326) 144.98(11) YES O(2) K(1) C(321) 114.68(10) YES O(3) K(1) C(321) 55.67(9) YES O(1) K(1) C(321) 82.78(10) YES C(162) K(1) C(321) 107.75(11) YES C(266) K(1) C(321) 95.24(12) YES C(163) K(1) C(321) 115.62(12) YES C(261) K(1) C(321) 120.15(11) YES C(326) K(1) C(321) 24.86(11) YES O(2) K(1) C(265) 93.28(11) YES O(3) K(1) C(265) 84.08(11) YES O(1) K(1) C(265) 140.42(11) YES C(162) K(1) C(265) 152.87(13) YES C(266) K(1) C(265) 24.86(11) YES C(163) K(1) C(265) 127.30(13) YES C(261) K(1) C(265) 44.05(11) YES C(326) K(1) C(265) 107.42(12) YES C(321) K(1) C(265) 85.01(12) YES O(2) K(1) C(262) 72.24(10) YES O(3) K(1) C(262) 109.74(11) YES O(1) K(1) C(262) 128.82(11) YES C(162) K(1) C(262) 114.07(13) YES C(266) K(1) C(262) 43.59(13) YES C(163) K(1) C(262) 96.70(13) YES C(261) K(1) C(262) 24.93(11) YES C(326) K(1) C(262) 156.16(12) YES C(321) K(1) C(262) 134.98(12) YES C(265) K(1) C(262) 50.01(13) YES O(2) K(1) C(325) 143.93(10) YES O(3) K(1) C(325) 94.02(10) YES O(1) K(1) C(325) 87.02(10) YES C(162) K(1) C(325) 70.71(11) YES C(266) K(1) C(325) 129.41(12) YES C(163) K(1) C(325) 72.91(12) YES C(261) K(1) C(325) 152.59(11) YES C(326) K(1) C(325) 24.19(11) YES C(321) K(1) C(325) 42.84(11) YES C(265) K(1) C(325) 108.55(12) YES C(262) K(1) C(325) 143.56(12) YES O(6) K(2) O(5) 59.07(8) YES O(6) K(2) O(4) 58.75(8) YES O(5) K(2) O(4) 58.37(8) YES O(6) K(2) C(462) 72.85(10) YES O(5) K(2) C(462) 119.57(10) YES O(4) K(2) C(462) 66.49(9) YES O(6) K(2) C(526) 129.12(10) YES O(5) K(2) C(526) 71.24(10) YES O(4) K(2) C(526) 104.54(10) YES C(462) K(2) C(526) 149.62(11) YES O(6) K(2) C(525) 154.35(10) YES O(5) K(2) C(525) 96.26(10) YES O(4) K(2) C(525) 116.60(10) YES C(462) K(2) C(525) 130.77(11) YES C(526) K(2) C(525) 25.32(11) YES O(6) K(2) C(522) 116.59(10) YES O(5) K(2) C(522) 67.47(9) YES O(4) K(2) C(522) 65.64(10) YES C(462) K(2) C(522) 110.67(11) YES C(526) K(2) C(522) 43.94(11) YES C(525) K(2) C(522) 51.04(11) YES O(6) K(2) C(521) 113.33(10) YES O(5) K(2) C(521) 54.98(9) YES O(4) K(2) C(521) 79.33(9) YES C(462) K(2) C(521) 135.33(11) YES C(526) K(2) C(521) 25.25(10) YES C(525) K(2) C(521) 44.60(11) YES C(522) K(2) C(521) 25.23(10) YES O(6) K(2) C(524) 159.93(10) YES O(5) K(2) C(524) 106.70(10) YES O(4) K(2) C(524) 102.33(10) YES C(462) K(2) C(524) 107.27(11) YES C(526) K(2) C(524) 44.28(11) YES C(525) K(2) C(524) 24.86(11) YES C(522) K(2) C(524) 43.85(11) YES C(521) K(2) C(524) 51.95(11) YES O(6) K(2) C(463) 88.67(10) YES O(5) K(2) C(463) 143.52(10) YES O(4) K(2) C(463) 91.58(10) YES C(462) K(2) C(463) 25.38(11) YES C(526) K(2) C(463) 142.04(11) YES C(525) K(2) C(463) 116.98(12) YES C(522) K(2) C(463) 121.69(11) YES C(521) K(2) C(463) 145.67(11) YES C(524) K(2) C(463) 99.18(11) YES O(6) K(2) C(523) 135.74(10) YES O(5) K(2) C(523) 92.51(10) YES O(4) K(2) C(523) 77.79(10) YES C(462) K(2) C(523) 98.61(11) YES C(526) K(2) C(523) 51.20(11) YES C(525) K(2) C(523) 43.50(12) YES C(522) K(2) C(523) 25.04(11) YES C(521) K(2) C(523) 44.51(11) YES C(524) K(2) C(523) 24.58(11) YES C(463) K(2) C(523) 101.30(11) YES O(6) K(2) C(621) 55.84(9) YES O(5) K(2) C(621) 80.65(9) YES O(4) K(2) C(621) 113.86(9) YES C(462) K(2) C(621) 101.76(11) YES C(526) K(2) C(621) 108.20(11) YES C(525) K(2) C(621) 117.45(11) YES C(522) K(2) C(621) 142.54(11) YES C(521) K(2) C(621) 118.43(11) YES C(524) K(2) C(621) 140.35(11) YES C(463) K(2) C(621) 95.60(11) YES C(523) K(2) C(621) 159.29(11) YES C(11) O(1) Ge(1) 118.8(2) YES C(11) O(1) K(1) 138.2(2) YES Ge(1) O(1) K(1) 91.58(10) YES C(21) O(2) Ge(1) 125.5(2) YES C(21) O(2) K(1) 134.1(2) YES Ge(1) O(2) K(1) 93.64(10) YES C(31) O(3) Ge(1) 121.5(2) YES C(31) O(3) K(1) 134.9(2) YES Ge(1) O(3) K(1) 93.00(10) YES C(41) O(4) Ge(2) 121.0(2) YES C(41) O(4) K(2) 139.1(2) YES Ge(2) O(4) K(2) 91.13(9) YES C(51) O(5) Ge(2) 122.2(2) YES C(51) O(5) K(2) 135.2(2) YES Ge(2) O(5) K(2) 92.49(9) YES C(61) O(6) Ge(2) 119.3(2) YES C(61) O(6) K(2) 135.6(2) YES Ge(2) O(6) K(2) 94.79(10) YES O(1) C(11) C(16) 118.8(4) YES O(1) C(11) C(12) 122.4(4) YES C(16) C(11) C(12) 118.8(4) YES C(13) C(12) C(11) 119.6(4) YES C(13) C(12) C(121) 118.0(4) YES C(11) C(12) C(121) 122.4(4) YES C(12) C(13) C(14) 121.5(4) YES C(15) C(14) C(13) 119.1(4) YES C(14) C(15) C(16) 120.9(4) YES C(15) C(16) C(11) 119.9(4) YES C(15) C(16) C(161) 120.7(4) YES C(11) C(16) C(161) 119.3(4) YES O(2) C(21) C(26) 118.2(4) YES O(2) C(21) C(22) 122.8(4) YES C(26) C(21) C(22) 119.0(4) YES C(23) C(22) C(21) 119.1(4) YES C(23) C(22) C(221) 119.4(4) YES C(21) C(22) C(221) 121.5(4) YES C(24) C(23) C(22) 121.2(4) YES C(25) C(24) C(23) 119.9(4) YES C(24) C(25) C(26) 120.7(4) YES C(25) C(26) C(21) 120.0(4) YES C(25) C(26) C(261) 120.4(4) YES C(21) C(26) C(261) 119.6(4) YES O(3) C(31) C(32) 119.1(4) YES O(3) C(31) C(36) 120.8(4) YES C(32) C(31) C(36) 120.1(4) YES C(33) C(32) C(31) 119.5(4) YES C(33) C(32) C(321) 120.0(4) YES C(31) C(32) C(321) 120.4(3) YES C(34) C(33) C(32) 121.2(4) YES C(33) C(34) C(35) 119.0(4) YES C(34) C(35) C(36) 122.4(4) YES C(35) C(36) C(31) 117.5(4) YES C(35) C(36) C(361) 120.5(4) YES C(31) C(36) C(361) 122.0(4) YES O(4) C(41) C(42) 122.0(4) YES O(4) C(41) C(46) 118.7(3) YES C(42) C(41) C(46) 119.2(4) YES C(43) C(42) C(41) 118.6(4) YES C(43) C(42) C(421) 119.0(4) YES C(41) C(42) C(421) 122.3(4) YES C(44) C(43) C(42) 121.8(4) YES C(45) C(44) C(43) 119.0(4) YES C(44) C(45) C(46) 121.7(4) YES C(45) C(46) C(41) 119.4(4) YES C(45) C(46) C(461) 121.1(4) YES C(41) C(46) C(461) 119.4(3) YES O(5) C(51) C(52) 118.3(3) YES O(5) C(51) C(56) 122.2(3) YES C(52) C(51) C(56) 119.5(4) YES C(53) C(52) C(51) 120.1(4) YES C(53) C(52) C(521) 121.3(4) YES C(51) C(52) C(521) 118.6(3) YES C(54) C(53) C(52) 120.4(4) YES C(53) C(54) C(55) 119.3(4) YES C(56) C(55) C(54) 122.1(4) YES C(55) C(56) C(51) 118.5(4) YES C(55) C(56) C(561) 120.0(4) YES C(51) C(56) C(561) 121.4(3) YES O(6) C(61) C(62) 118.7(3) YES O(6) C(61) C(66) 121.2(4) YES C(62) C(61) C(66) 120.1(4) YES C(63) C(62) C(61) 119.9(4) YES C(63) C(62) C(621) 120.3(4) YES C(61) C(62) C(621) 119.8(3) YES C(64) C(63) C(62) 120.0(4) YES C(65) C(64) C(63) 120.0(4) YES C(64) C(65) C(66) 121.6(4) YES C(65) C(66) C(61) 118.4(4) YES C(65) C(66) C(661) 119.8(4) YES C(61) C(66) C(661) 121.7(3) YES C(122) C(121) C(126) 118.1(4) YES C(122) C(121) C(12) 120.9(4) YES C(126) C(121) C(12) 120.8(4) YES C(121) C(122) C(123) 121.1(5) YES C(122) C(123) C(124) 120.6(5) YES C(125) C(124) C(123) 119.1(5) YES C(124) C(125) C(126) 120.1(5) YES C(125) C(126) C(121) 121.0(5) YES C(166) C(161) C(162) 117.4(4) YES C(166) C(161) C(16) 122.5(4) YES C(162) C(161) C(16) 120.0(4) YES C(166) C(161) K(1) 92.5(3) YES C(162) C(161) K(1) 66.0(2) YES C(16) C(161) K(1) 110.1(2) YES C(163) C(162) C(161) 121.5(4) YES C(163) C(162) K(1) 80.5(3) YES C(161) C(162) K(1) 89.6(3) YES C(162) C(163) C(164) 119.7(4) YES C(162) C(163) K(1) 73.9(3) YES C(164) C(163) K(1) 92.8(3) YES C(165) C(164) C(163) 119.4(4) YES C(165) C(164) K(1) 89.7(3) YES C(163) C(164) K(1) 64.1(3) YES C(164) C(165) C(166) 120.7(4) YES C(161) C(166) C(165) 121.4(4) YES C(226) C(221) C(222) 118.5(4) YES C(226) C(221) C(22) 120.8(4) YES C(222) C(221) C(22) 120.7(4) YES C(223) C(222) C(221) 121.2(4) YES C(224) C(223) C(222) 119.8(4) YES C(225) C(224) C(223) 119.1(5) YES C(224) C(225) C(226) 121.3(5) YES C(221) C(226) C(225) 120.0(5) YES C(266) C(261) C(262) 118.1(4) YES C(266) C(261) C(26) 122.3(4) YES C(262) C(261) C(26) 119.6(4) YES C(266) C(261) K(1) 75.9(2) YES C(262) C(261) K(1) 81.9(3) YES C(26) C(261) K(1) 111.1(2) YES C(263) C(262) C(261) 120.7(5) YES C(263) C(262) K(1) 82.4(3) YES C(261) C(262) K(1) 73.1(3) YES C(264) C(263) C(262) 120.5(5) YES C(264) C(263) K(1) 77.8(3) YES C(262) C(263) K(1) 73.7(3) YES C(263) C(264) C(265) 119.5(5) YES C(263) C(264) K(1) 78.8(3) YES C(265) C(264) K(1) 73.2(3) YES C(266) C(265) C(264) 119.7(5) YES C(266) C(265) K(1) 72.6(2) YES C(264) C(265) K(1) 82.6(3) YES C(265) C(266) C(261) 121.4(5) YES C(265) C(266) K(1) 82.6(3) YES C(261) C(266) K(1) 78.8(2) YES C(322) C(321) C(326) 118.3(4) YES C(322) C(321) C(32) 120.0(4) YES C(326) C(321) C(32) 121.7(4) YES C(322) C(321) K(1) 85.6(3) YES C(326) C(321) K(1) 75.2(2) YES C(32) C(321) K(1) 109.8(2) YES C(321) C(322) C(323) 120.7(4) YES C(321) C(322) K(1) 70.8(2) YES C(323) C(322) K(1) 83.7(3) YES C(324) C(323) C(322) 120.1(4) YES C(323) C(324) C(325) 119.8(4) YES C(323) C(324) K(1) 80.5(3) YES C(325) C(324) K(1) 71.4(3) YES C(326) C(325) C(324) 119.8(4) YES C(326) C(325) K(1) 71.5(2) YES C(324) C(325) K(1) 85.5(3) YES C(325) C(326) C(321) 121.3(4) YES C(325) C(326) K(1) 84.3(3) YES C(321) C(326) K(1) 80.0(2) YES C(366) C(361) C(362) 118.1(4) YES C(366) C(361) C(36) 120.1(4) YES C(362) C(361) C(36) 121.8(4) YES C(363) C(362) C(361) 121.0(4) YES C(362) C(363) C(364) 121.0(4) YES C(363) C(364) C(365) 118.2(4) YES C(366) C(365) C(364) 120.7(4) YES C(365) C(366) C(361) 121.0(4) YES C(426) C(421) C(422) 117.7(4) YES C(426) C(421) C(42) 122.0(4) YES C(422) C(421) C(42) 120.2(4) YES C(423) C(422) C(421) 121.1(4) YES C(424) C(423) C(422) 120.5(4) YES C(423) C(424) C(425) 119.2(4) YES C(426) C(425) C(424) 120.4(4) YES C(425) C(426) C(421) 121.2(4) YES C(466) C(461) C(462) 117.7(4) YES C(466) C(461) C(46) 119.8(4) YES C(462) C(461) C(46) 122.5(3) YES C(466) C(461) K(2) 95.6(3) YES C(462) C(461) K(2) 65.0(2) YES C(46) C(461) K(2) 110.0(2) YES C(463) C(462) C(461) 120.7(4) YES C(463) C(462) K(2) 82.2(2) YES C(461) C(462) K(2) 90.6(2) YES C(462) C(463) C(464) 120.1(4) YES C(462) C(463) K(2) 72.4(2) YES C(464) C(463) K(2) 95.3(3) YES C(465) C(464) C(463) 119.0(4) YES C(466) C(465) C(464) 121.1(4) YES C(465) C(466) C(461) 121.4(4) YES C(526) C(521) C(522) 117.3(4) YES C(526) C(521) C(52) 121.7(4) YES C(522) C(521) C(52) 120.8(4) YES C(526) C(521) K(2) 76.2(2) YES C(522) C(521) K(2) 77.2(2) YES C(52) C(521) K(2) 112.3(2) YES C(523) C(522) C(521) 121.4(4) YES C(523) C(522) K(2) 78.3(2) YES C(521) C(522) K(2) 77.5(2) YES C(524) C(523) C(522) 120.2(4) YES C(524) C(523) K(2) 77.1(3) YES C(522) C(523) K(2) 76.7(2) YES C(523) C(524) C(525) 119.8(4) YES C(523) C(524) K(2) 78.3(3) YES C(525) C(524) K(2) 76.7(2) YES C(524) C(525) C(526) 120.5(4) YES C(524) C(525) K(2) 78.4(3) YES C(526) C(525) K(2) 76.9(2) YES C(521) C(526) C(525) 120.8(4) YES C(521) C(526) K(2) 78.6(2) YES C(525) C(526) K(2) 77.7(3) YES C(566) C(561) C(562) 117.5(4) YES C(566) C(561) C(56) 121.4(4) YES C(562) C(561) C(56) 121.0(4) YES C(563) C(562) C(561) 120.7(4) YES C(564) C(563) C(562) 121.3(5) YES C(563) C(564) C(565) 118.6(5) YES C(566) C(565) C(564) 121.3(5) YES C(565) C(566) C(561) 120.6(5) YES C(626) C(621) C(622) 117.7(4) YES C(626) C(621) C(62) 122.9(4) YES C(622) C(621) C(62) 119.5(4) YES C(626) C(621) K(2) 81.7(2) YES C(622) C(621) K(2) 78.2(2) YES C(62) C(621) K(2) 109.6(2) YES C(623) C(622) C(621) 120.8(4) YES C(623) C(622) K(2) 83.3(3) YES C(621) C(622) K(2) 76.8(2) YES C(622) C(623) C(624) 120.5(4) YES C(622) C(623) K(2) 72.7(3) YES C(624) C(623) K(2) 82.3(3) YES C(625) C(624) C(623) 119.3(4) YES C(625) C(624) K(2) 77.7(2) YES C(623) C(624) K(2) 74.5(3) YES C(624) C(625) C(626) 120.1(4) YES C(624) C(625) K(2) 79.3(2) YES C(626) C(625) K(2) 73.0(2) YES C(625) C(626) C(621) 121.6(4) YES C(625) C(626) K(2) 83.5(2) YES C(621) C(626) K(2) 74.0(2) YES C(666) C(661) C(662) 118.3(4) YES C(666) C(661) C(66) 120.9(4) YES C(662) C(661) C(66) 120.8(4) YES C(661) C(662) C(663) 120.0(4) YES C(664) C(663) C(662) 120.1(4) YES C(665) C(664) C(663) 120.5(5) YES C(664) C(665) C(666) 119.6(4) YES C(665) C(666) C(661) 121.5(4) YES C(916) C(911) C(912) 120.3(6) YES C(913) C(912) C(911) 120.5(6) YES C(912) C(913) C(914) 119.7(6) YES C(913) C(914) C(915) 120.5(5) YES C(916) C(915) C(914) 117.6(6) YES C(911) C(916) C(915) 121.3(6) YES C(926) C(921) C(922) 119.4(7) YES C(923) C(922) C(921) 121.0(6) YES C(922) C(923) C(924) 121.0(6) YES C(923) C(924) C(925) 117.9(6) YES C(924) C(925) C(926) 120.3(5) YES C(921) C(926) C(925) 120.2(6) YES #============================================================================== data_SW3401 _database_code_CSD 203293 _audit_creation_date 23-12-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C54 H39 Cs1 Ge1 O3' _chemical_formula_moiety 'C54 H39 Cs1 Ge1 O3' _chemical_formula_structural ? _chemical_formula_weight 941.41 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 38.6426(9) _cell_length_b 10.7401(2) _cell_length_c 21.2400(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.1847(11) _cell_angle_gamma 90.00 _cell_volume 8374.9(3) _cell_measurement_reflns_used 30647 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.615 _cell_measurement_temperature 150 _exptl_crystal_F_000 3792 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_T_max 0.8172 _diffrn_reflns_number 30647 _diffrn_measured_fraction_theta_max 0.9929 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9929 _reflns_number_total 9425 _reflns_number_gt 7407 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 25 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.103 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9409 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0510P)^2^+5.4985P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 2.12 _refine_diff_density_min -0.73 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cs Cs 0.112200(7) 0.07147(2) 0.141930(12) 0.02839(10) Uani 1 1 d . . . Ge Ge 0.122463(12) 0.24985(4) -0.00839(2) 0.02253(12) Uani 1 1 d . . . O(1) O 0.12171(7) 0.3311(2) 0.07183(12) 0.0234(6) Uani 1 1 d . . . O(2) O 0.08351(7) 0.1435(2) 0.00258(12) 0.0262(7) Uani 1 1 d . . . O(3) O 0.15963(7) 0.1420(2) 0.04651(13) 0.0252(6) Uani 1 1 d . . . C(11) C 0.14510(11) 0.4058(3) 0.11643(19) 0.0208(9) Uani 1 1 d . . . C(12) C 0.13870(11) 0.4224(4) 0.17800(19) 0.0226(9) Uani 1 1 d . . . C(13) C 0.16302(12) 0.4924(4) 0.2286(2) 0.0299(10) Uani 1 1 d . . . C(14) C 0.19328(13) 0.5475(4) 0.2190(2) 0.0368(12) Uani 1 1 d . . . C(15) C 0.19871(12) 0.5349(4) 0.1581(2) 0.0327(11) Uani 1 1 d . . . C(16) C 0.17509(11) 0.4663(4) 0.1059(2) 0.0253(9) Uani 1 1 d . . . C(21) C 0.05572(11) 0.1013(4) -0.04917(19) 0.0236(9) Uani 1 1 d . . . C(22) C 0.04574(12) -0.0252(4) -0.04967(19) 0.0255(9) Uani 1 1 d . . . C(23) C 0.01726(13) -0.0707(4) -0.1031(2) 0.0394(12) Uani 1 1 d . . . C(24) C -0.00052(14) 0.0049(5) -0.1563(2) 0.0461(14) Uani 1 1 d . . . C(25) C 0.00886(12) 0.1288(4) -0.1545(2) 0.0330(11) Uani 1 1 d . . . C(26) C 0.03622(11) 0.1797(4) -0.10153(18) 0.0254(9) Uani 1 1 d . . . C(31) C 0.17759(11) 0.0386(3) 0.03860(19) 0.0208(9) Uani 1 1 d . . . C(32) C 0.19904(11) -0.0232(4) 0.0963(2) 0.0254(9) Uani 1 1 d . . . C(33) C 0.21534(12) -0.1375(4) 0.0900(2) 0.0316(10) Uani 1 1 d . . . C(34) C 0.21054(12) -0.1903(4) 0.0296(2) 0.0340(11) Uani 1 1 d . . . C(35) C 0.19099(12) -0.1280(4) -0.0268(2) 0.0307(10) Uani 1 1 d . . . C(36) C 0.17483(12) -0.0118(4) -0.0242(2) 0.0265(9) Uani 1 1 d . . . C(121) C 0.10564(12) 0.3709(4) 0.19017(19) 0.0259(9) Uani 1 1 d . . . C(122) C 0.07125(12) 0.3942(4) 0.1455(2) 0.0330(10) Uani 1 1 d . . . C(123) C 0.04041(14) 0.3516(5) 0.1572(3) 0.0509(14) Uani 1 1 d . . . C(124) C 0.04281(16) 0.2816(5) 0.2134(3) 0.0530(15) Uani 1 1 d . . . C(125) C 0.07624(18) 0.2561(5) 0.2582(3) 0.0502(15) Uani 1 1 d . . . C(126) C 0.10793(15) 0.3018(4) 0.2477(2) 0.0365(11) Uani 1 1 d . . . C(161) C 0.18249(12) 0.4679(4) 0.0412(2) 0.0269(10) Uani 1 1 d . . . C(162) C 0.21669(13) 0.4340(4) 0.0369(2) 0.0354(11) Uani 1 1 d . . . C(163) C 0.22515(14) 0.4490(5) -0.0210(2) 0.0419(12) Uani 1 1 d . . . C(164) C 0.19934(14) 0.4984(5) -0.0768(2) 0.0450(13) Uani 1 1 d . . . C(165) C 0.16520(14) 0.5308(5) -0.0739(2) 0.0397(12) Uani 1 1 d . . . C(166) C 0.15681(12) 0.5154(4) -0.0153(2) 0.0306(10) Uani 1 1 d . . . C(221) C 0.06442(11) -0.1118(4) 0.00557(19) 0.0245(9) Uani 1 1 d . . . C(222) C 0.10060(12) -0.1459(4) 0.0171(2) 0.0297(10) Uani 1 1 d . . . C(223) C 0.11782(12) -0.2289(4) 0.0679(2) 0.0312(10) Uani 1 1 d . . . C(224) C 0.09844(13) -0.2756(4) 0.1074(2) 0.0338(11) Uani 1 1 d . . . C(225) C 0.06282(14) -0.2428(4) 0.0974(2) 0.0375(11) Uani 1 1 d . . . C(226) C 0.04543(13) -0.1607(4) 0.0460(2) 0.0328(10) Uani 1 1 d . . . C(261) C 0.04320(11) 0.3163(4) -0.1012(2) 0.0293(10) Uani 1 1 d . . . C(262) C 0.04970(14) 0.3708(5) -0.1558(2) 0.0430(12) Uani 1 1 d . . . C(263) C 0.05702(16) 0.4969(5) -0.1566(3) 0.0612(17) Uani 1 1 d . . . C(264) C 0.05789(15) 0.5687(5) -0.1037(3) 0.0578(17) Uani 1 1 d . . . C(265) C 0.05090(15) 0.5178(5) -0.0491(3) 0.0509(15) Uani 1 1 d . . . C(266) C 0.04353(13) 0.3892(4) -0.0481(2) 0.0391(12) Uani 1 1 d . . . C(321) C 0.20347(11) 0.0307(4) 0.16343(19) 0.0250(9) Uani 1 1 d . . . C(322) C 0.21049(11) 0.1577(4) 0.1760(2) 0.0292(10) Uani 1 1 d . . . C(323) C 0.21338(12) 0.2082(5) 0.2378(2) 0.0380(12) Uani 1 1 d . . . C(324) C 0.20822(13) 0.1334(6) 0.2869(2) 0.0459(14) Uani 1 1 d . . . C(325) C 0.20195(13) 0.0083(6) 0.2759(2) 0.0448(13) Uani 1 1 d . . . C(326) C 0.19956(12) -0.0433(5) 0.2149(2) 0.0361(11) Uani 1 1 d . . . C(361) C 0.15557(12) 0.0549(4) -0.0866(2) 0.0293(10) Uani 1 1 d . . . C(362) C 0.12417(14) 0.0077(5) -0.1309(2) 0.0436(13) Uani 1 1 d . . . C(363) C 0.10632(17) 0.0713(6) -0.1894(2) 0.0594(16) Uani 1 1 d . . . C(364) C 0.12041(19) 0.1801(6) -0.2046(3) 0.0594(17) Uani 1 1 d . . . C(365) C 0.15198(19) 0.2271(5) -0.1615(3) 0.0540(16) Uani 1 1 d . . . C(366) C 0.16938(15) 0.1655(4) -0.1023(2) 0.0410(12) Uani 1 1 d . . . H(13) H 0.1586 0.5020 0.2699 0.036 Uiso 1 1 calc R . . H(14) H 0.2100 0.5932 0.2536 0.044 Uiso 1 1 calc R . . H(15) H 0.2193 0.5741 0.1512 0.039 Uiso 1 1 calc R . . H(23) H 0.0100 -0.1552 -0.1029 0.047 Uiso 1 1 calc R . . H(24) H -0.0189 -0.0283 -0.1934 0.055 Uiso 1 1 calc R . . H(25) H -0.0037 0.1811 -0.1904 0.040 Uiso 1 1 calc R . . H(33) H 0.2300 -0.1787 0.1287 0.038 Uiso 1 1 calc R . . H(34) H 0.2206 -0.2698 0.0265 0.041 Uiso 1 1 calc R . . H(35) H 0.1884 -0.1646 -0.0688 0.037 Uiso 1 1 calc R . . H(122) H 0.0692 0.4404 0.1064 0.040 Uiso 1 1 calc R . . H(123) H 0.0172 0.3701 0.1267 0.061 Uiso 1 1 calc R . . H(124) H 0.0213 0.2513 0.2208 0.064 Uiso 1 1 calc R . . H(125) H 0.0779 0.2073 0.2963 0.060 Uiso 1 1 calc R . . H(126) H 0.1310 0.2863 0.2795 0.044 Uiso 1 1 calc R . . H(162) H 0.2344 0.3999 0.0747 0.042 Uiso 1 1 calc R . . H(163) H 0.2485 0.4259 -0.0229 0.050 Uiso 1 1 calc R . . H(164) H 0.2052 0.5097 -0.1167 0.054 Uiso 1 1 calc R . . H(165) H 0.1475 0.5636 -0.1120 0.048 Uiso 1 1 calc R . . H(166) H 0.1333 0.5376 -0.0138 0.037 Uiso 1 1 calc R . . H(222) H 0.1138 -0.1122 -0.0099 0.036 Uiso 1 1 calc R . . H(223) H 0.1424 -0.2527 0.0751 0.037 Uiso 1 1 calc R . . H(224) H 0.1100 -0.3317 0.1421 0.041 Uiso 1 1 calc R . . H(225) H 0.0500 -0.2757 0.1252 0.045 Uiso 1 1 calc R . . H(226) H 0.0207 -0.1382 0.0388 0.039 Uiso 1 1 calc R . . H(262) H 0.0491 0.3209 -0.1930 0.052 Uiso 1 1 calc R . . H(263) H 0.0614 0.5330 -0.1942 0.073 Uiso 1 1 calc R . . H(264) H 0.0634 0.6548 -0.1041 0.069 Uiso 1 1 calc R . . H(265) H 0.0511 0.5690 -0.0126 0.061 Uiso 1 1 calc R . . H(266) H 0.0388 0.3533 -0.0107 0.047 Uiso 1 1 calc R . . H(322) H 0.2133 0.2101 0.1419 0.035 Uiso 1 1 calc R . . H(323) H 0.2189 0.2940 0.2461 0.046 Uiso 1 1 calc R . . H(324) H 0.2090 0.1686 0.3284 0.055 Uiso 1 1 calc R . . H(325) H 0.1992 -0.0433 0.3103 0.054 Uiso 1 1 calc R . . H(326) H 0.1952 -0.1301 0.2080 0.043 Uiso 1 1 calc R . . H(362) H 0.1146 -0.0690 -0.1216 0.052 Uiso 1 1 calc R . . H(363) H 0.0843 0.0389 -0.2188 0.071 Uiso 1 1 calc R . . H(364) H 0.1084 0.2227 -0.2447 0.071 Uiso 1 1 calc R . . H(365) H 0.1620 0.3020 -0.1720 0.065 Uiso 1 1 calc R . . H(366) H 0.1909 0.1998 -0.0724 0.049 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cs 0.03386(17) 0.02651(15) 0.02420(15) 0.00007(12) 0.00817(11) -0.00115(11) Ge 0.0240(2) 0.0212(2) 0.0209(2) -0.00070(18) 0.00471(18) -0.00020(17) O(1) 0.0214(15) 0.0221(15) 0.0274(14) -0.0049(12) 0.0084(12) -0.0059(12) O(2) 0.0254(16) 0.0236(15) 0.0232(14) -0.0055(12) -0.0016(12) 0.0006(12) O(3) 0.0260(16) 0.0254(16) 0.0232(14) 0.0070(12) 0.0061(12) 0.0010(12) C(11) 0.0181(19) 0.016(2) 0.023(2) 0.0000(16) -0.0014(16) -0.0021(16) C(12) 0.019(2) 0.020(2) 0.027(2) 0.0046(17) 0.0041(17) 0.0014(17) C(13) 0.027(2) 0.030(2) 0.026(2) 0.003(2) -0.0020(19) -0.0066(19) C(14) 0.030(3) 0.038(3) 0.035(3) -0.008(2) 0.000(2) -0.014(2) C(15) 0.028(2) 0.027(2) 0.038(3) -0.0098(19) 0.003(2) -0.003(2) C(16) 0.026(2) 0.022(2) 0.027(2) 0.0010(18) 0.0067(18) 0.0016(17) C(21) 0.023(2) 0.024(2) 0.022(2) -0.0039(18) 0.0044(17) -0.0008(17) C(22) 0.029(2) 0.021(2) 0.024(2) -0.0041(18) 0.0051(18) -0.0002(17) C(23) 0.040(3) 0.031(3) 0.035(3) -0.008(2) -0.006(2) 0.002(2) C(24) 0.044(3) 0.045(3) 0.032(3) -0.009(2) -0.013(2) -0.004(2) C(25) 0.033(3) 0.034(3) 0.025(2) -0.003(2) -0.0006(19) 0.0040(19) C(26) 0.027(2) 0.029(2) 0.020(2) -0.0006(18) 0.0074(17) 0.0011(17) C(31) 0.020(2) 0.017(2) 0.028(2) -0.0023(16) 0.0104(17) 0.0008(16) C(32) 0.022(2) 0.023(2) 0.033(2) 0.0000(18) 0.0109(18) 0.0065(18) C(33) 0.028(2) 0.025(2) 0.040(3) 0.0014(19) 0.007(2) 0.008(2) C(34) 0.035(3) 0.015(2) 0.056(3) -0.0014(19) 0.021(2) -0.001(2) C(35) 0.036(3) 0.024(2) 0.038(2) -0.002(2) 0.021(2) -0.005(2) C(36) 0.029(2) 0.025(2) 0.032(2) -0.0031(19) 0.0183(19) -0.0015(18) C(121) 0.032(2) 0.020(2) 0.027(2) 0.0001(18) 0.0113(19) -0.0076(17) C(122) 0.028(2) 0.035(3) 0.036(2) -0.003(2) 0.010(2) -0.012(2) C(123) 0.034(3) 0.065(4) 0.055(3) -0.013(3) 0.016(3) -0.026(3) C(124) 0.052(4) 0.060(4) 0.059(4) -0.026(3) 0.035(3) -0.031(3) C(125) 0.088(5) 0.035(3) 0.048(3) -0.011(3) 0.050(3) -0.010(2) C(126) 0.060(3) 0.024(2) 0.028(2) 0.004(2) 0.018(2) -0.0056(19) C(161) 0.027(2) 0.023(2) 0.029(2) -0.0117(18) 0.0068(19) -0.0030(18) C(162) 0.028(2) 0.037(3) 0.040(3) -0.010(2) 0.009(2) 0.002(2) C(163) 0.034(3) 0.049(3) 0.048(3) -0.014(2) 0.020(2) -0.005(2) C(164) 0.048(3) 0.055(3) 0.034(3) -0.024(3) 0.016(2) -0.006(2) C(165) 0.042(3) 0.043(3) 0.031(2) -0.016(2) 0.006(2) 0.000(2) C(166) 0.031(2) 0.025(2) 0.033(2) -0.0072(19) 0.006(2) 0.0011(19) C(221) 0.027(2) 0.0170(19) 0.025(2) -0.0051(18) 0.0016(18) -0.0036(17) C(222) 0.028(2) 0.030(2) 0.031(2) -0.008(2) 0.0092(19) -0.0059(19) C(223) 0.027(2) 0.024(2) 0.040(3) 0.0017(19) 0.006(2) -0.004(2) C(224) 0.045(3) 0.022(2) 0.029(2) 0.005(2) 0.003(2) 0.0055(19) C(225) 0.046(3) 0.028(2) 0.043(3) -0.002(2) 0.021(2) 0.011(2) C(226) 0.029(2) 0.029(2) 0.039(2) 0.000(2) 0.008(2) 0.004(2) C(261) 0.023(2) 0.027(2) 0.030(2) 0.0025(19) -0.0033(18) 0.0060(19) C(262) 0.044(3) 0.038(3) 0.045(3) 0.001(2) 0.011(2) 0.014(2) C(263) 0.059(4) 0.042(3) 0.077(4) -0.001(3) 0.013(3) 0.030(3) C(264) 0.050(3) 0.026(3) 0.078(4) 0.001(2) -0.008(3) 0.018(3) C(265) 0.048(3) 0.034(3) 0.054(3) 0.007(2) -0.008(3) -0.007(3) C(266) 0.036(3) 0.036(3) 0.037(3) 0.007(2) -0.001(2) 0.002(2) C(321) 0.017(2) 0.032(2) 0.025(2) 0.0028(17) 0.0047(17) 0.0080(18) C(322) 0.024(2) 0.033(2) 0.027(2) 0.0025(19) 0.0031(18) 0.0037(19) C(323) 0.027(3) 0.049(3) 0.030(2) 0.011(2) -0.002(2) -0.004(2) C(324) 0.030(3) 0.079(4) 0.025(2) 0.008(3) 0.004(2) -0.005(3) C(325) 0.030(3) 0.074(4) 0.030(3) -0.001(3) 0.008(2) 0.018(3) C(326) 0.027(2) 0.044(3) 0.035(2) 0.001(2) 0.007(2) 0.011(2) C(361) 0.037(3) 0.031(2) 0.023(2) 0.006(2) 0.0134(19) -0.0025(18) C(362) 0.053(3) 0.048(3) 0.029(2) -0.005(3) 0.012(2) 0.002(2) C(363) 0.057(4) 0.086(5) 0.029(3) 0.001(3) 0.004(3) -0.004(3) C(364) 0.091(5) 0.059(4) 0.030(3) 0.024(4) 0.022(3) 0.005(3) C(365) 0.099(5) 0.030(3) 0.044(3) 0.012(3) 0.039(3) 0.008(2) C(366) 0.068(4) 0.026(2) 0.034(3) 0.003(2) 0.022(2) 0.001(2) # 10. MOLECULAR GEOMETRY _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_publ_flag Cs O(2) 2.922(3) YES Cs O(3) 3.219(3) YES Cs O(1) 3.236(3) YES Cs C(126) 3.381(4) YES Cs C(121) 3.408(4) YES Cs C(321) 3.440(4) YES Cs C(222) 3.455(4) YES Cs C(326) 3.472(4) YES Cs C(221) 3.512(4) YES Cs C(223) 3.625(4) YES Cs C(226) 3.707(4) YES Cs C(322) 3.754(4) YES Ge O(1) 1.923(3) YES Ge O(3) 1.929(3) YES Ge O(2) 1.960(3) YES O(1) C(11) 1.350(4) YES O(2) C(21) 1.353(4) YES O(3) C(31) 1.347(5) YES C(11) C(16) 1.406(6) YES C(11) C(12) 1.416(6) YES C(12) C(13) 1.405(5) YES C(12) C(121) 1.487(6) YES C(13) C(14) 1.382(6) YES C(14) C(15) 1.379(6) YES C(15) C(16) 1.405(6) YES C(16) C(161) 1.488(6) YES C(21) C(26) 1.411(5) YES C(21) C(22) 1.411(5) YES C(22) C(23) 1.400(6) YES C(22) C(221) 1.495(6) YES C(23) C(24) 1.386(6) YES C(24) C(25) 1.377(6) YES C(25) C(26) 1.392(6) YES C(26) C(261) 1.491(6) YES C(31) C(36) 1.413(5) YES C(31) C(32) 1.413(5) YES C(32) C(33) 1.405(6) YES C(32) C(321) 1.498(6) YES C(33) C(34) 1.361(6) YES C(34) C(35) 1.375(6) YES C(35) C(36) 1.404(6) YES C(36) C(361) 1.486(6) YES C(121) C(122) 1.394(6) YES C(121) C(126) 1.409(6) YES C(122) C(123) 1.370(7) YES C(123) C(124) 1.389(8) YES C(124) C(125) 1.371(8) YES C(125) C(126) 1.400(7) YES C(161) C(166) 1.394(6) YES C(161) C(162) 1.401(6) YES C(162) C(163) 1.377(7) YES C(163) C(164) 1.394(7) YES C(164) C(165) 1.384(7) YES C(165) C(166) 1.390(6) YES C(221) C(222) 1.391(6) YES C(221) C(226) 1.395(6) YES C(222) C(223) 1.398(6) YES C(223) C(224) 1.381(6) YES C(224) C(225) 1.372(7) YES C(225) C(226) 1.401(6) YES C(261) C(266) 1.370(6) YES C(261) C(262) 1.389(6) YES C(262) C(263) 1.385(7) YES C(263) C(264) 1.354(8) YES C(264) C(265) 1.382(8) YES C(265) C(266) 1.411(7) YES C(321) C(326) 1.398(6) YES C(321) C(322) 1.399(6) YES C(322) C(323) 1.392(6) YES C(323) C(324) 1.379(7) YES C(324) C(325) 1.372(8) YES C(325) C(326) 1.386(7) YES C(361) C(362) 1.380(6) YES C(361) C(366) 1.385(6) YES C(362) C(363) 1.396(7) YES C(363) C(364) 1.370(8) YES C(364) C(365) 1.373(8) YES C(365) C(366) 1.394(7) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(2) Cs O(3) 53.88(7) YES O(2) Cs O(1) 50.76(7) YES O(3) Cs O(1) 48.60(7) YES O(2) Cs C(126) 113.43(9) YES O(3) Cs C(126) 113.69(10) YES O(1) Cs C(126) 73.22(9) YES O(2) Cs C(121) 90.82(9) YES O(3) Cs C(121) 94.45(9) YES O(1) Cs C(121) 49.83(9) YES C(126) Cs C(121) 23.95(10) YES O(2) Cs C(321) 102.55(9) YES O(3) Cs C(321) 49.59(8) YES O(1) Cs C(321) 84.94(8) YES C(126) Cs C(321) 105.40(12) YES C(121) Cs C(321) 104.45(10) YES O(2) Cs C(222) 58.96(9) YES O(3) Cs C(222) 68.82(9) YES O(1) Cs C(222) 103.61(9) YES C(126) Cs C(222) 169.40(11) YES C(121) Cs C(222) 149.78(10) YES C(321) Cs C(222) 84.15(10) YES O(2) Cs C(326) 123.70(10) YES O(3) Cs C(326) 72.49(9) YES O(1) Cs C(326) 106.10(9) YES C(126) Cs C(326) 101.86(12) YES C(121) Cs C(326) 110.74(11) YES C(321) Cs C(326) 23.33(10) YES C(222) Cs C(326) 88.73(11) YES O(2) Cs C(221) 51.51(8) YES O(3) Cs C(221) 82.46(8) YES O(1) Cs C(221) 102.10(8) YES C(126) Cs C(221) 146.74(11) YES C(121) Cs C(221) 135.03(9) YES C(321) Cs C(221) 106.95(10) YES C(222) Cs C(221) 23.01(10) YES C(326) Cs C(221) 110.90(11) YES O(2) Cs C(223) 81.46(9) YES O(3) Cs C(223) 79.24(9) YES O(1) Cs C(223) 122.45(9) YES C(126) Cs C(223) 164.07(10) YES C(121) Cs C(223) 171.97(10) YES C(321) Cs C(223) 75.32(10) YES C(222) Cs C(223) 22.61(9) YES C(326) Cs C(223) 72.30(11) YES C(221) Cs C(223) 39.71(9) YES O(2) Cs C(226) 69.06(8) YES O(3) Cs C(226) 104.35(9) YES O(1) Cs C(226) 119.10(8) YES C(126) Cs C(226) 133.42(12) YES C(121) Cs C(226) 134.06(10) YES C(321) Cs C(226) 119.76(10) YES C(222) Cs C(226) 38.98(11) YES C(326) Cs C(226) 114.80(11) YES C(221) Cs C(226) 22.07(10) YES C(223) Cs C(226) 44.67(10) YES O(2) Cs C(322) 99.86(9) YES O(3) Cs C(322) 47.37(8) YES O(1) Cs C(322) 67.84(8) YES C(126) Cs C(322) 87.00(11) YES C(121) Cs C(322) 82.82(10) YES C(321) Cs C(322) 21.88(10) YES C(222) Cs C(322) 101.29(10) YES C(326) Cs C(322) 38.47(10) YES C(221) Cs C(322) 122.50(10) YES C(223) Cs C(322) 96.27(10) YES C(226) Cs C(322) 139.53(10) YES O(1) Ge O(3) 87.20(11) YES O(1) Ge O(2) 86.25(11) YES O(3) Ge O(2) 91.88(12) YES O(1) Ge Cs 57.10(8) YES O(3) Ge Cs 56.59(9) YES O(2) Ge Cs 47.91(7) YES C(11) O(1) Ge 134.4(3) YES C(11) O(1) Cs 109.6(2) YES Ge O(1) Cs 92.97(9) YES C(21) O(2) Ge 122.9(2) YES C(21) O(2) Cs 133.5(2) YES Ge O(2) Cs 102.24(10) YES C(31) O(3) Ge 137.3(2) YES C(31) O(3) Cs 107.5(2) YES Ge O(3) Cs 93.39(10) YES O(1) C(11) C(16) 124.6(4) YES O(1) C(11) C(12) 116.8(4) YES C(16) C(11) C(12) 118.6(3) YES O(1) C(11) Cs 51.34(18) YES C(16) C(11) Cs 140.1(3) YES C(12) C(11) Cs 80.2(2) YES C(13) C(12) C(11) 120.4(4) YES C(13) C(12) C(121) 118.2(4) YES C(11) C(12) C(121) 121.4(3) YES C(13) C(12) Cs 137.4(3) YES C(11) C(12) Cs 79.0(2) YES C(121) C(12) Cs 59.3(2) YES C(14) C(13) C(12) 120.7(4) YES C(15) C(14) C(13) 118.7(4) YES C(14) C(15) C(16) 122.7(4) YES C(11) C(16) C(15) 118.8(4) YES C(11) C(16) C(161) 123.9(4) YES C(15) C(16) C(161) 117.3(4) YES O(2) C(21) C(26) 122.3(4) YES O(2) C(21) C(22) 118.3(3) YES C(26) C(21) C(22) 119.4(4) YES C(23) C(22) C(21) 119.1(4) YES C(23) C(22) C(221) 118.9(4) YES C(21) C(22) C(221) 122.0(4) YES C(24) C(23) C(22) 121.3(4) YES C(25) C(24) C(23) 119.0(4) YES C(24) C(25) C(26) 121.9(4) YES C(25) C(26) C(21) 119.1(4) YES C(25) C(26) C(261) 118.7(4) YES C(21) C(26) C(261) 122.2(4) YES O(3) C(31) C(36) 122.9(3) YES O(3) C(31) C(32) 117.7(3) YES C(36) C(31) C(32) 119.3(4) YES O(3) C(31) Cs 52.95(18) YES C(36) C(31) Cs 134.8(3) YES C(32) C(31) Cs 82.0(2) YES C(33) C(32) C(31) 119.2(4) YES C(33) C(32) C(321) 120.4(4) YES C(31) C(32) C(321) 120.4(4) YES C(33) C(32) Cs 134.1(3) YES C(31) C(32) Cs 77.1(2) YES C(321) C(32) Cs 61.0(2) YES C(34) C(33) C(32) 121.3(4) YES C(33) C(34) C(35) 119.7(4) YES C(34) C(35) C(36) 121.8(4) YES C(35) C(36) C(31) 118.3(4) YES C(35) C(36) C(361) 119.9(4) YES C(31) C(36) C(361) 121.7(4) YES C(122) C(121) C(126) 118.3(4) YES C(122) C(121) C(12) 120.2(4) YES C(126) C(121) C(12) 121.5(4) YES C(122) C(121) Cs 96.3(3) YES C(126) C(121) Cs 76.9(2) YES C(12) C(121) Cs 98.6(2) YES C(123) C(122) C(121) 121.0(5) YES C(123) C(122) Cs 95.1(3) YES C(121) C(122) Cs 62.4(2) YES C(122) C(123) C(124) 120.6(5) YES C(125) C(124) C(123) 120.0(5) YES C(124) C(125) C(126) 120.1(5) YES C(124) C(125) Cs 96.4(3) YES C(126) C(125) Cs 63.9(2) YES C(125) C(126) C(121) 120.1(5) YES C(125) C(126) Cs 94.3(3) YES C(121) C(126) Cs 79.1(2) YES C(166) C(161) C(162) 118.1(4) YES C(166) C(161) C(16) 120.6(4) YES C(162) C(161) C(16) 121.0(4) YES C(163) C(162) C(161) 121.3(4) YES C(162) C(163) C(164) 119.9(5) YES C(165) C(164) C(163) 119.8(5) YES C(164) C(165) C(166) 120.1(5) YES C(165) C(166) C(161) 120.8(5) YES C(222) C(221) C(226) 119.1(4) YES C(222) C(221) C(22) 121.0(4) YES C(226) C(221) C(22) 120.0(4) YES C(222) C(221) Cs 76.2(2) YES C(226) C(221) Cs 86.8(2) YES C(22) C(221) Cs 107.4(2) YES C(221) C(222) C(223) 120.9(4) YES C(221) C(222) Cs 80.8(2) YES C(223) C(222) Cs 85.5(2) YES C(224) C(223) C(222) 118.9(4) YES C(224) C(223) Cs 86.7(3) YES C(222) C(223) Cs 71.9(2) YES C(225) C(224) C(223) 121.4(4) YES C(225) C(224) Cs 81.4(3) YES C(223) C(224) Cs 72.0(2) YES C(224) C(225) C(226) 119.8(4) YES C(224) C(225) Cs 77.9(3) YES C(226) C(225) Cs 73.7(3) YES C(221) C(226) C(225) 120.0(4) YES C(221) C(226) Cs 71.1(2) YES C(225) C(226) Cs 85.0(3) YES C(266) C(261) C(262) 119.2(4) YES C(266) C(261) C(26) 121.4(4) YES C(262) C(261) C(26) 119.4(4) YES C(263) C(262) C(261) 120.9(5) YES C(264) C(263) C(262) 119.9(6) YES C(263) C(264) C(265) 120.6(5) YES C(264) C(265) C(266) 119.5(5) YES C(261) C(266) C(265) 119.8(5) YES C(326) C(321) C(322) 117.8(4) YES C(326) C(321) C(32) 121.1(4) YES C(322) C(321) C(32) 121.1(4) YES C(326) C(321) Cs 79.6(2) YES C(322) C(321) Cs 91.8(3) YES C(32) C(321) Cs 96.6(2) YES C(323) C(322) C(321) 120.9(4) YES C(323) C(322) Cs 93.3(3) YES C(321) C(322) Cs 66.4(2) YES C(324) C(323) C(322) 119.9(5) YES C(325) C(324) C(323) 120.0(5) YES C(324) C(325) C(326) 120.6(5) YES C(324) C(325) Cs 91.4(3) YES C(326) C(325) Cs 65.9(3) YES C(325) C(326) C(321) 120.7(5) YES C(325) C(326) Cs 92.7(3) YES C(321) C(326) Cs 77.1(2) YES C(362) C(361) C(366) 118.3(4) YES C(362) C(361) C(36) 121.4(4) YES C(366) C(361) C(36) 120.3(4) YES C(361) C(362) C(363) 120.8(5) YES C(364) C(363) C(362) 120.3(6) YES C(363) C(364) C(365) 119.5(5) YES C(364) C(365) C(366) 120.3(5) YES C(361) C(366) C(365) 120.7(5) YES