Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Ian Rothwell' 'P. Fanwick' 'Andrew E. Fenwick' 'Charles Weinert' _publ_contact_author_name 'Prof Ian Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Drive West Lafayette IN 47907 UNITED STATES OF AMERICA ; _publ_contact_author_email 'ROTHWELL@PURDUE.EDU ' _publ_contact_author_email 'rothwell@purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4947012' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Structures, and Reactivity of Novel Germanium(II) Aryloxide and Arylthiolato Complexes ; _publ_section_references ; P. T. Beurskens, G. Beurskens, R. deGelder,S. Garcia-Granda, R. O. Gould, R. Israel, J. M. M. Smits, '(1999). The DIRDIF-99 Program System. 'Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. 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 ; data_SW2302 _database_code_CSD 195674 _audit_creation_date 26-09-02 _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 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C36 H26 Ge1 O2' _chemical_formula_moiety 'C36 H26 Ge1 O2' _chemical_formula_structural ? _chemical_formula_weight 563.20 _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 23.9641(3) _cell_length_b 12.3175(2) _cell_length_c 20.0053(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.3914(6) _cell_angle_gamma 90.00 _cell_volume 5498.32(14) _cell_measurement_reflns_used 31603 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 8 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.128 _cell_measurement_temperature 150 _exptl_crystal_F_000 2320 # 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 0.3629 _exptl_absorpt_correction_T_max 0.6369 _diffrn_reflns_number 31603 _diffrn_measured_fraction_theta_max 0.9802 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9802 _reflns_number_total 6361 _reflns_number_gt 5391 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 24 # 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 0.032 _refine_ls_wR_factor_ref 0.083 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6331 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.31 _refine_diff_density_min -0.58 _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 Ge Ge 0.087309(8) 0.218099(17) 0.308166(9) 0.02576(8) Uani 1 1 d . . . O(1) O 0.13684(5) 0.25550(10) 0.39844(6) 0.0243(3) Uani 1 1 d . . . O(2) O 0.14995(5) 0.17591(10) 0.28360(6) 0.0244(3) Uani 1 1 d . . . C(11) C 0.11220(7) 0.25973(15) 0.45065(9) 0.0222(4) Uani 1 1 d . . . C(12) C 0.08033(7) 0.17070(15) 0.46216(9) 0.0228(4) Uani 1 1 d . . . C(13) C 0.05436(8) 0.17936(16) 0.51442(9) 0.0270(4) Uani 1 1 d . . . C(14) C 0.05999(9) 0.27315(16) 0.55397(10) 0.0309(4) Uani 1 1 d . . . C(15) C 0.09170(8) 0.36030(16) 0.54236(9) 0.0292(4) Uani 1 1 d . . . C(16) C 0.11772(7) 0.35604(15) 0.49015(9) 0.0242(4) Uani 1 1 d . . . C(21) C 0.13907(7) 0.16319(14) 0.21161(8) 0.0213(3) Uani 1 1 d . . . C(22) C 0.15571(7) 0.06610(14) 0.18760(9) 0.0228(4) Uani 1 1 d . . . C(23) C 0.14240(8) 0.05419(15) 0.11343(9) 0.0258(4) Uani 1 1 d . . . C(24) C 0.11323(8) 0.13505(15) 0.06544(9) 0.0273(4) Uani 1 1 d . . . C(25) C 0.09802(8) 0.23079(15) 0.09022(9) 0.0251(4) Uani 1 1 d . . . C(26) C 0.11127(7) 0.24746(15) 0.16344(9) 0.0220(4) Uani 1 1 d . . . C(121) C 0.07181(7) 0.06956(14) 0.41875(8) 0.0223(4) Uani 1 1 d . . . C(122) C 0.01458(8) 0.02278(15) 0.38873(9) 0.0269(4) Uani 1 1 d . . . C(123) C 0.00608(9) -0.07212(16) 0.34945(10) 0.0318(4) Uani 1 1 d . . . C(124) C 0.05398(9) -0.12229(16) 0.33912(10) 0.0330(4) Uani 1 1 d . . . C(125) C 0.11064(8) -0.07698(16) 0.36742(10) 0.0299(4) Uani 1 1 d . . . C(126) C 0.11950(8) 0.01811(15) 0.40673(9) 0.0259(4) Uani 1 1 d . . . C(161) C 0.14736(8) 0.45397(15) 0.47519(9) 0.0258(4) Uani 1 1 d . . . C(162) C 0.20366(9) 0.45085(17) 0.46965(10) 0.0330(4) Uani 1 1 d . . . C(163) C 0.22944(10) 0.5455(2) 0.45711(11) 0.0417(5) Uani 1 1 d . . . C(164) C 0.19952(11) 0.64383(19) 0.44906(10) 0.0432(6) Uani 1 1 d . . . C(165) C 0.14441(11) 0.64771(18) 0.45413(11) 0.0410(5) Uani 1 1 d . . . C(166) C 0.11821(9) 0.55395(15) 0.46750(9) 0.0311(4) Uani 1 1 d . . . C(221) C 0.18670(7) -0.02478(15) 0.23641(9) 0.0231(4) Uani 1 1 d . . . C(222) C 0.23111(8) -0.00555(16) 0.30397(9) 0.0270(4) Uani 1 1 d . . . C(223) C 0.26105(8) -0.09206(17) 0.34668(10) 0.0319(4) Uani 1 1 d . . . C(224) C 0.24716(9) -0.19817(17) 0.32347(11) 0.0338(5) Uani 1 1 d . . . C(225) C 0.20308(9) -0.21802(16) 0.25703(11) 0.0327(4) Uani 1 1 d . . . C(226) C 0.17304(8) -0.13170(16) 0.21411(10) 0.0296(4) Uani 1 1 d . . . C(261) C 0.09705(7) 0.35412(15) 0.18855(9) 0.0235(4) Uani 1 1 d . . . C(262) C 0.04133(8) 0.40284(16) 0.15411(10) 0.0301(4) Uani 1 1 d . . . C(263) C 0.02880(10) 0.50346(18) 0.17603(11) 0.0404(5) Uani 1 1 d . . . C(264) C 0.07129(10) 0.55744(18) 0.23231(11) 0.0415(5) Uani 1 1 d . . . C(265) C 0.12681(9) 0.51028(17) 0.26703(10) 0.0356(5) Uani 1 1 d . . . C(266) C 0.13971(8) 0.40988(15) 0.24560(9) 0.0274(4) Uani 1 1 d . . . H(13) H 0.0326 0.1197 0.5227 0.032 Uiso 1 1 calc R . . H(14) H 0.0421 0.2779 0.5892 0.037 Uiso 1 1 calc R . . H(15) H 0.0959 0.4242 0.5703 0.035 Uiso 1 1 calc R . . H(23) H 0.1537 -0.0107 0.0960 0.031 Uiso 1 1 calc R . . H(24) H 0.1037 0.1246 0.0154 0.033 Uiso 1 1 calc R . . H(25) H 0.0783 0.2862 0.0570 0.030 Uiso 1 1 calc R . . H(122) H -0.0186 0.0567 0.3955 0.032 Uiso 1 1 calc R . . H(123) H -0.0328 -0.1031 0.3294 0.038 Uiso 1 1 calc R . . H(124) H 0.0480 -0.1880 0.3125 0.040 Uiso 1 1 calc R . . H(125) H 0.1434 -0.1111 0.3599 0.036 Uiso 1 1 calc R . . H(126) H 0.1585 0.0490 0.4259 0.031 Uiso 1 1 calc R . . H(162) H 0.2243 0.3838 0.4745 0.040 Uiso 1 1 calc R . . H(163) H 0.2680 0.5431 0.4540 0.050 Uiso 1 1 calc R . . H(164) H 0.2174 0.7083 0.4400 0.052 Uiso 1 1 calc R . . H(165) H 0.1238 0.7150 0.4485 0.049 Uiso 1 1 calc R . . H(166) H 0.0799 0.5578 0.4715 0.037 Uiso 1 1 calc R . . H(222) H 0.2408 0.0668 0.3206 0.032 Uiso 1 1 calc R . . H(223) H 0.2913 -0.0783 0.3922 0.038 Uiso 1 1 calc R . . H(224) H 0.2677 -0.2569 0.3530 0.041 Uiso 1 1 calc R . . H(225) H 0.1934 -0.2905 0.2408 0.039 Uiso 1 1 calc R . . H(226) H 0.1427 -0.1460 0.1688 0.036 Uiso 1 1 calc R . . H(262) H 0.0118 0.3666 0.1153 0.036 Uiso 1 1 calc R . . H(263) H -0.0093 0.5357 0.1522 0.048 Uiso 1 1 calc R . . H(264) H 0.0624 0.6265 0.2471 0.050 Uiso 1 1 calc R . . H(265) H 0.1561 0.5471 0.3057 0.043 Uiso 1 1 calc R . . H(266) H 0.1779 0.3782 0.2698 0.033 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 0.02632(12) 0.03256(13) 0.02058(11) 0.00111(8) 0.01113(8) 0.00154(8) O(1) 0.0297(7) 0.0254(7) 0.0222(6) -0.0033(5) 0.0147(5) -0.0020(5) O(2) 0.0300(6) 0.0271(7) 0.0178(6) 0.0019(5) 0.0107(5) -0.0012(5) C(11) 0.0235(8) 0.0269(10) 0.0168(8) 0.0017(7) 0.0079(7) 0.0003(7) C(12) 0.0259(9) 0.0229(9) 0.0202(8) 0.0023(7) 0.0093(7) 0.0025(7) C(13) 0.0304(9) 0.0282(10) 0.0254(9) -0.0012(8) 0.0137(8) 0.0049(8) C(14) 0.0398(11) 0.0348(12) 0.0245(9) 0.0008(8) 0.0194(8) 0.0003(8) C(15) 0.0353(10) 0.0300(11) 0.0239(9) 0.0005(8) 0.0126(8) -0.0036(7) C(16) 0.0273(9) 0.0245(10) 0.0213(8) 0.0004(7) 0.0095(7) -0.0003(7) C(21) 0.0225(8) 0.0254(10) 0.0184(8) -0.0028(7) 0.0103(7) -0.0018(7) C(22) 0.0246(8) 0.0235(9) 0.0224(8) -0.0038(7) 0.0112(7) -0.0008(7) C(23) 0.0302(9) 0.0241(10) 0.0266(9) -0.0050(7) 0.0146(8) -0.0057(7) C(24) 0.0359(10) 0.0294(11) 0.0187(8) -0.0064(8) 0.0123(7) -0.0040(7) C(25) 0.0282(9) 0.0273(10) 0.0201(8) -0.0039(7) 0.0093(7) 0.0022(7) C(26) 0.0236(9) 0.0222(9) 0.0224(8) -0.0037(7) 0.0109(7) -0.0016(7) C(121) 0.0275(9) 0.0215(9) 0.0198(8) -0.0008(7) 0.0110(7) 0.0047(7) C(122) 0.0305(9) 0.0261(10) 0.0279(9) 0.0002(7) 0.0151(8) 0.0026(7) C(123) 0.0341(10) 0.0306(11) 0.0310(9) -0.0083(8) 0.0123(8) -0.0018(8) C(124) 0.0465(11) 0.0242(10) 0.0318(10) -0.0023(8) 0.0184(9) -0.0028(8) C(125) 0.0369(10) 0.0258(10) 0.0333(10) 0.0051(8) 0.0204(8) 0.0054(8) C(126) 0.0283(9) 0.0226(10) 0.0286(9) 0.0005(7) 0.0125(8) 0.0055(7) C(161) 0.0329(9) 0.0270(10) 0.0180(8) -0.0047(7) 0.0098(7) -0.0046(7) C(162) 0.0347(10) 0.0348(12) 0.0306(10) -0.0057(8) 0.0133(8) -0.0043(8) C(163) 0.0417(12) 0.0521(15) 0.0340(11) -0.0197(10) 0.0167(9) -0.0073(10) C(164) 0.0688(15) 0.0357(13) 0.0263(10) -0.0230(11) 0.0185(10) -0.0069(9) C(165) 0.0688(14) 0.0263(11) 0.0297(10) -0.0017(10) 0.0198(10) -0.0038(8) C(166) 0.0440(11) 0.0268(11) 0.0233(9) -0.0004(8) 0.0132(8) -0.0031(7) C(221) 0.0234(8) 0.0237(10) 0.0261(8) 0.0008(7) 0.0138(7) 0.0005(7) C(222) 0.0292(9) 0.0266(10) 0.0280(9) 0.0015(7) 0.0138(8) -0.0014(8) C(223) 0.0278(9) 0.0424(13) 0.0271(9) 0.0059(8) 0.0118(8) 0.0018(8) C(224) 0.0340(10) 0.0355(12) 0.0401(11) 0.0102(8) 0.0231(9) 0.0110(9) C(225) 0.0376(11) 0.0238(10) 0.0429(11) 0.0012(8) 0.0220(9) 0.0017(8) C(226) 0.0298(9) 0.0284(11) 0.0316(9) -0.0001(8) 0.0124(8) -0.0009(8) C(261) 0.0303(9) 0.0224(9) 0.0216(8) -0.0017(7) 0.0140(7) 0.0027(7) C(262) 0.0332(10) 0.0320(11) 0.0267(9) 0.0022(8) 0.0131(8) 0.0021(8) C(263) 0.0457(12) 0.0397(13) 0.0373(11) 0.0158(10) 0.0169(10) 0.0066(9) C(264) 0.0628(14) 0.0280(12) 0.0386(11) 0.0117(10) 0.0241(10) -0.0016(9) C(265) 0.0486(12) 0.0289(11) 0.0312(10) -0.0035(9) 0.0167(9) -0.0042(8) C(266) 0.0336(10) 0.0234(10) 0.0278(9) -0.0019(7) 0.0142(8) 0.0005(7) # 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(2) 1.8174(12) YES Ge O(1) 1.8218(12) YES O(1) C(11) 1.376(2) YES O(2) C(21) 1.3759(19) YES C(11) C(12) 1.402(3) YES C(11) C(16) 1.405(2) YES C(12) C(13) 1.402(2) YES C(12) C(121) 1.490(2) YES C(13) C(14) 1.379(3) YES C(14) C(15) 1.383(3) YES C(15) C(16) 1.399(2) YES C(16) C(161) 1.485(3) YES C(21) C(22) 1.400(2) YES C(21) C(26) 1.408(2) YES C(22) C(23) 1.407(2) YES C(22) C(221) 1.493(2) YES C(23) C(24) 1.383(3) YES C(24) C(25) 1.379(3) YES C(25) C(26) 1.396(2) YES C(26) C(261) 1.490(2) YES C(121) C(126) 1.402(2) YES C(121) C(122) 1.405(2) YES C(122) C(123) 1.382(3) YES C(123) C(124) 1.384(3) YES C(124) C(125) 1.384(3) YES C(125) C(126) 1.383(3) YES C(161) C(162) 1.394(3) YES C(161) C(166) 1.396(3) YES C(162) C(163) 1.385(3) YES C(163) C(164) 1.386(3) YES C(164) C(165) 1.362(3) YES C(165) C(166) 1.386(3) YES C(221) C(226) 1.391(3) YES C(221) C(222) 1.402(2) YES C(222) C(223) 1.390(3) YES C(223) C(224) 1.386(3) YES C(224) C(225) 1.385(3) YES C(225) C(226) 1.391(3) YES C(261) C(262) 1.395(2) YES C(261) C(266) 1.403(2) YES C(262) C(263) 1.384(3) YES C(263) C(264) 1.382(3) YES C(264) C(265) 1.384(3) YES C(265) C(266) 1.380(3) 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) Ge O(1) 92.10(5) YES C(11) O(1) Ge 117.22(10) YES C(21) O(2) Ge 117.11(10) YES O(1) C(11) C(12) 120.35(15) YES O(1) C(11) C(16) 118.73(16) YES C(12) C(11) C(16) 120.88(16) YES C(13) C(12) C(11) 118.64(17) YES C(13) C(12) C(121) 119.64(16) YES C(11) C(12) C(121) 121.69(15) YES C(14) C(13) C(12) 120.96(18) YES C(13) C(14) C(15) 119.92(17) YES C(14) C(15) C(16) 121.21(18) YES C(15) C(16) C(11) 118.38(17) YES C(15) C(16) C(161) 119.75(16) YES C(11) C(16) C(161) 121.79(15) YES O(2) C(21) C(22) 119.18(15) YES O(2) C(21) C(26) 119.62(15) YES C(22) C(21) C(26) 121.20(15) YES C(21) C(22) C(23) 117.87(16) YES C(21) C(22) C(221) 123.51(15) YES C(23) C(22) C(221) 118.61(16) YES C(24) C(23) C(22) 121.32(17) YES C(25) C(24) C(23) 119.94(16) YES C(24) C(25) C(26) 120.95(17) YES C(25) C(26) C(21) 118.65(16) YES C(25) C(26) C(261) 119.41(16) YES C(21) C(26) C(261) 121.93(15) YES C(126) C(121) C(122) 118.11(17) YES C(126) C(121) C(12) 122.07(15) YES C(122) C(121) C(12) 119.82(16) YES C(123) C(122) C(121) 120.57(17) YES C(122) C(123) C(124) 120.30(18) YES C(125) C(124) C(123) 120.16(18) YES C(126) C(125) C(124) 119.89(18) YES C(125) C(126) C(121) 120.95(17) YES C(162) C(161) C(166) 118.38(18) YES C(162) C(161) C(16) 122.79(17) YES C(166) C(161) C(16) 118.82(17) YES C(163) C(162) C(161) 120.0(2) YES C(162) C(163) C(164) 120.7(2) YES C(165) C(164) C(163) 119.8(2) YES C(164) C(165) C(166) 120.3(2) YES C(165) C(166) C(161) 120.8(2) YES C(226) C(221) C(222) 118.44(16) YES C(226) C(221) C(22) 119.84(16) YES C(222) C(221) C(22) 121.69(16) YES C(223) C(222) C(221) 120.20(18) YES C(224) C(223) C(222) 120.64(18) YES C(225) C(224) C(223) 119.59(18) YES C(224) C(225) C(226) 119.95(18) YES C(221) C(226) C(225) 121.17(17) YES C(262) C(261) C(266) 118.25(17) YES C(262) C(261) C(26) 120.54(16) YES C(266) C(261) C(26) 121.18(15) YES C(263) C(262) C(261) 120.53(18) YES C(264) C(263) C(262) 120.56(19) YES C(263) C(264) C(265) 119.65(19) YES C(266) C(265) C(264) 120.22(19) YES C(265) C(266) C(261) 120.80(17) YES #===END data_AF2050 _database_code_CSD 195675 _audit_creation_date 14-06-02 _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 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C45 H70 Ge1 S3' _chemical_formula_moiety 'C45 H70 Ge1 S3' _chemical_formula_structural ? _chemical_formula_weight 779.84 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7180(3) _cell_length_b 18.5142(4) _cell_length_c 19.0815(5) _cell_angle_alpha 114.7659(9) _cell_angle_beta 101.0489(9) _cell_angle_gamma 91.0279(15) _cell_volume 4605.6(4) _cell_measurement_reflns_used 46626 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.12 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.812 _cell_measurement_temperature 150 _exptl_crystal_F_000 1680 # 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 0.5798 _exptl_absorpt_correction_T_max 0.7756 _diffrn_reflns_number 46626 _diffrn_measured_fraction_theta_max 0.9875 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9875 _reflns_number_total 21512 _reflns_number_gt 15618 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.95 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_max 24 # 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 0.049 _refine_ls_wR_factor_ref 0.106 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 21485 _refine_ls_number_parameters 927 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.83 _refine_diff_density_min -0.72 _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(1) Ge 0.073269(18) 0.328313(16) 0.750994(16) 0.02733(8) Uani 1 1 d . . . Ge(2) Ge 0.444946(19) 0.174513(17) 0.240981(17) 0.03081(8) Uani 1 1 d . . . S(11) S 0.13444(4) 0.37003(4) 0.87881(4) 0.03073(15) Uani 1 1 d . . . S(12) S -0.05065(4) 0.38982(4) 0.73280(4) 0.03190(16) Uani 1 1 d . . . S(13) S 0.18025(5) 0.34630(4) 0.69074(4) 0.03293(16) Uani 1 1 d . . . S(21) S 0.43462(5) 0.13232(4) 0.11269(4) 0.03546(17) Uani 1 1 d . . . S(22) S 0.58054(5) 0.15443(4) 0.30011(4) 0.03650(17) Uani 1 1 d . . . S(23) S 0.32847(5) 0.11286(4) 0.26036(4) 0.03637(17) Uani 1 1 d . . . C(111) C 0.19383(18) 0.28230(16) 0.86355(15) 0.0307(6) Uani 1 1 d . . . C(112) C 0.28906(17) 0.28559(16) 0.86153(15) 0.0301(6) Uani 1 1 d . . . C(113) C 0.33282(19) 0.21725(17) 0.84996(16) 0.0358(6) Uani 1 1 d . . . C(114) C 0.2868(2) 0.14631(17) 0.83958(17) 0.0394(7) Uani 1 1 d . . . C(115) C 0.1937(2) 0.14491(17) 0.84179(17) 0.0418(7) Uani 1 1 d . . . C(116) C 0.14498(19) 0.21118(17) 0.85349(17) 0.0368(7) Uani 1 1 d . . . C(11A) C 0.3859(2) 0.41071(18) 0.96325(18) 0.0462(8) Uani 1 1 d . . . C(11B) C 0.34447(18) 0.36227(16) 0.87504(16) 0.0333(6) Uani 1 1 d . . . C(11C) C 0.4215(2) 0.3479(2) 0.8284(2) 0.0519(8) Uani 1 1 d . . . C(11D) C 0.3845(4) 0.0745(3) 0.9036(3) 0.127(2) Uani 1 1 d . . . C(11E) C 0.3374(2) 0.07244(19) 0.8275(2) 0.0498(8) Uani 1 1 d . . . C(11F) C 0.4138(7) 0.0653(4) 0.7829(5) 0.238(6) Uani 1 1 d . . . C(11G) C 0.0342(2) 0.2225(3) 0.9413(2) 0.0641(10) Uani 1 1 d . . . C(11H) C 0.0425(2) 0.20605(19) 0.85765(19) 0.0468(8) Uani 1 1 d . . . C(11I) C -0.0124(2) 0.1256(2) 0.7963(3) 0.0760(12) Uani 1 1 d . . . C(121) C -0.13070(17) 0.32384(16) 0.74506(16) 0.0324(6) Uani 1 1 d . . . C(122) C -0.15819(18) 0.34790(17) 0.81786(16) 0.0365(7) Uani 1 1 d . . . C(123) C -0.2263(2) 0.2989(2) 0.82275(18) 0.0493(8) Uani 1 1 d . . . C(124) C -0.2664(2) 0.2272(2) 0.76004(19) 0.0535(9) Uani 1 1 d . . . C(125) C -0.2351(2) 0.20366(19) 0.69032(18) 0.0464(8) Uani 1 1 d . . . C(126) C -0.16813(18) 0.24962(17) 0.68047(16) 0.0353(6) Uani 1 1 d . . . C(12A) C -0.0965(2) 0.4178(2) 0.96655(17) 0.0451(8) Uani 1 1 d . . . C(12B) C -0.11876(19) 0.42674(18) 0.88892(16) 0.0387(7) Uani 1 1 d . . . C(12C) C -0.1857(2) 0.4899(2) 0.8932(2) 0.0592(9) Uani 1 1 d . . . C(12D) C -0.3138(4) 0.1097(4) 0.7752(5) 0.167(3) Uani 1 1 d . . . C(12E) C -0.3446(3) 0.1774(3) 0.7660(2) 0.0752(13) Uani 1 1 d . . . C(12F) C -0.4305(3) 0.1603(3) 0.7028(3) 0.0997(17) Uani 1 1 d . . . C(12G) C -0.1400(2) 0.13139(18) 0.55914(19) 0.0516(8) Uani 1 1 d . . . C(12H) C -0.14167(19) 0.22238(17) 0.60101(16) 0.0361(7) Uani 1 1 d . . . C(12I) C -0.2052(2) 0.25281(19) 0.54877(17) 0.0427(7) Uani 1 1 d . . . C(131) C 0.11637(19) 0.28077(17) 0.59259(16) 0.0359(7) Uani 1 1 d . . . C(132) C 0.0624(2) 0.3139(2) 0.54720(17) 0.0425(8) Uani 1 1 d . . . C(133) C 0.0154(2) 0.2602(3) 0.46992(19) 0.0646(12) Uani 1 1 d . . . C(134) C 0.0224(3) 0.1773(3) 0.4400(2) 0.0775(15) Uani 1 1 d . . . C(135) C 0.0756(3) 0.1494(2) 0.4878(2) 0.0686(12) Uani 1 1 d . . . C(136) C 0.1232(2) 0.19794(18) 0.56354(18) 0.0480(8) Uani 1 1 d . . . C(13A) C 0.1392(2) 0.4442(2) 0.5638(2) 0.0612(10) Uani 1 1 d . . . C(13B) C 0.0571(2) 0.4033(2) 0.5778(2) 0.0485(8) Uani 1 1 d . . . C(13C) C -0.0354(2) 0.4259(3) 0.5442(3) 0.0786(13) Uani 1 1 d . . . C(13D) C 0.0283(3) 0.1135(3) 0.2973(2) 0.0867(15) Uani 1 1 d . . . C(13E) C -0.0280(4) 0.1242(4) 0.3551(2) 0.147(3) Uani 1 1 d . . . C(13F) C -0.1217(3) 0.1128(4) 0.3365(3) 0.124(2) Uani 1 1 d . . . C(13G) C 0.2791(3) 0.1538(3) 0.5931(3) 0.1007(17) Uani 1 1 d . . . C(13H) C 0.1819(3) 0.1613(2) 0.6115(2) 0.0631(11) Uani 1 1 d . . . C(13I) C 0.1383(4) 0.0805(2) 0.6005(3) 0.112(2) Uani 1 1 d . . . C(211) C 0.50188(19) 0.21804(16) 0.11945(16) 0.0318(6) Uani 1 1 d . . . C(212) C 0.46079(19) 0.28867(16) 0.13038(15) 0.0326(6) Uani 1 1 d . . . C(213) C 0.5137(2) 0.35181(17) 0.13018(17) 0.0383(7) Uani 1 1 d . . . C(214) C 0.6033(2) 0.34664(17) 0.11870(19) 0.0420(7) Uani 1 1 d . . . C(215) C 0.6432(2) 0.27657(17) 0.10979(19) 0.0444(8) Uani 1 1 d . . . C(216) C 0.5947(2) 0.21140(16) 0.11020(18) 0.0395(7) Uani 1 1 d . . . C(21A) C 0.3484(2) 0.3812(2) 0.2007(2) 0.0583(10) Uani 1 1 d . . . C(21B) C 0.36031(19) 0.29809(17) 0.13967(17) 0.0363(7) Uani 1 1 d . . . C(21C) C 0.2938(2) 0.2773(2) 0.06062(19) 0.0560(9) Uani 1 1 d . . . C(21D) C 0.7531(3) 0.4394(2) 0.1707(3) 0.0985(16) Uani 1 1 d . . . C(21E) C 0.6580(2) 0.41452(19) 0.1143(2) 0.0553(9) Uani 1 1 d . . . C(21F) C 0.6698(3) 0.3911(2) 0.0303(2) 0.0697(11) Uani 1 1 d . . . C(21G) C 0.7401(3) 0.1535(2) 0.1517(2) 0.0668(10) Uani 1 1 d . . . C(21H) C 0.6436(2) 0.13687(18) 0.0992(2) 0.0539(9) Uani 1 1 d . . . C(21I) C 0.6473(3) 0.0904(2) 0.0127(2) 0.0848(15) Uani 1 1 d . . . C(221) C 0.57077(19) 0.22481(17) 0.39701(17) 0.0368(7) Uani 1 1 d . . . C(222) C 0.53644(19) 0.19686(17) 0.44630(17) 0.0372(7) Uani 1 1 d . . . C(223) C 0.5304(2) 0.25355(19) 0.52135(18) 0.0441(7) Uani 1 1 d . . . C(224) C 0.5571(2) 0.33551(18) 0.54755(18) 0.0442(8) Uani 1 1 d . . . C(225) C 0.5893(2) 0.35991(18) 0.49677(19) 0.0463(8) Uani 1 1 d . . . C(226) C 0.59685(19) 0.30660(18) 0.42093(18) 0.0412(7) Uani 1 1 d . . . C(22A) C 0.5971(2) 0.06973(19) 0.4422(2) 0.0498(8) Uani 1 1 d . . . C(22B) C 0.51078(19) 0.10794(17) 0.42123(17) 0.0379(7) Uani 1 1 d . . . C(22C) C 0.4319(2) 0.0913(2) 0.4557(2) 0.0521(8) Uani 1 1 d . . . C(22D) C 0.6300(3) 0.3868(3) 0.6924(2) 0.1070(19) Uani 1 1 d . . . C(22E) C 0.5533(2) 0.3958(2) 0.63051(19) 0.0542(9) Uani 1 1 d . . . C(22F) C 0.4593(3) 0.3930(2) 0.6500(2) 0.0706(11) Uani 1 1 d . . . C(22H) C 0.7412(2) 0.3356(2) 0.3826(2) 0.0698(11) Uani 1 1 d . . . C(22I) C 0.6355(2) 0.33779(18) 0.3692(2) 0.0482(8) Uani 1 1 d . . . C(22J) C 0.6100(3) 0.4202(2) 0.3794(3) 0.0730(12) Uani 1 1 d . . . C(231) C 0.24194(18) 0.17441(17) 0.24236(17) 0.0353(6) Uani 1 1 d . . . C(232) C 0.23690(19) 0.24997(18) 0.30267(17) 0.0372(7) Uani 1 1 d . . . C(233) C 0.1655(2) 0.29314(19) 0.28782(19) 0.0442(8) Uani 1 1 d . . . C(234) C 0.1003(2) 0.26468(19) 0.21657(19) 0.0440(7) Uani 1 1 d . . . C(235) C 0.1089(2) 0.19111(19) 0.15805(18) 0.0427(7) Uani 1 1 d . . . C(236) C 0.17876(18) 0.14440(17) 0.16831(17) 0.0354(7) Uani 1 1 d . . . C(23A) C 0.3287(2) 0.37339(19) 0.4204(2) 0.0562(9) Uani 1 1 d . . . C(23B) C 0.3034(2) 0.28276(18) 0.38405(17) 0.0401(7) Uani 1 1 d . . . C(23C) C 0.2623(2) 0.2580(2) 0.43941(18) 0.0518(8) Uani 1 1 d . . . C(23D) C 0.0530(3) 0.3828(3) 0.1937(4) 0.1060(18) Uani 1 1 d . . . C(23E) C 0.0206(2) 0.3121(2) 0.2035(2) 0.0599(9) Uani 1 1 d . . . C(23F) C -0.0383(3) 0.3314(3) 0.2641(3) 0.0894(15) Uani 1 1 d . . . C(23H) C 0.1508(2) 0.0590(2) 0.01956(18) 0.0553(9) Uani 1 1 d . . . C(23I) C 0.1827(2) 0.06278(18) 0.10232(17) 0.0398(7) Uani 1 1 d . . . C(23J) C 0.1271(2) -0.0018(2) 0.1116(2) 0.0575(9) Uani 1 1 d . . . H(1) H 0.0416(16) 0.2436(14) 0.7153(14) 0.026(7) Uiso 1 1 d . . . H(2) H 0.4389(17) 0.2606(15) 0.2799(15) 0.034(7) Uiso 1 1 d . . . H(113) H 0.3971 0.2190 0.8491 0.043 Uiso 1 1 calc R . . H(115) H 0.1616 0.0967 0.8351 0.050 Uiso 1 1 calc R . . H(11A) H 0.3356 0.4235 0.9921 0.069 Uiso 1 1 calc R . . H(11B) H 0.4206 0.4604 0.9718 0.069 Uiso 1 1 calc R . . H(11C) H 0.4280 0.3793 0.9824 0.069 Uiso 1 1 calc R . . H(11D) H 0.3002 0.3948 0.8575 0.040 Uiso 1 1 calc R . . H(11E) H 0.4698 0.3215 0.8489 0.078 Uiso 1 1 calc R . . H(11F) H 0.4489 0.3992 0.8342 0.078 Uiso 1 1 calc R . . H(11G) H 0.3951 0.3136 0.7724 0.078 Uiso 1 1 calc R . . H(11H) H 0.4010 0.0210 0.8956 0.191 Uiso 1 1 calc R . . H(11I) H 0.3427 0.0916 0.9405 0.191 Uiso 1 1 calc R . . H(11J) H 0.4411 0.1123 0.9254 0.191 Uiso 1 1 calc R . . H(11K) H 0.2913 0.0236 0.7982 0.060 Uiso 1 1 calc R . . H(11L) H 0.4501 0.1176 0.8032 0.356 Uiso 1 1 calc R . . H(11M) H 0.3861 0.0471 0.7265 0.356 Uiso 1 1 calc R . . H(11N) H 0.4547 0.0266 0.7900 0.356 Uiso 1 1 calc R . . H(11O) H 0.0638 0.1823 0.9559 0.096 Uiso 1 1 calc R . . H(11P) H -0.0317 0.2197 0.9433 0.096 Uiso 1 1 calc R . . H(11Q) H 0.0651 0.2759 0.9783 0.096 Uiso 1 1 calc R . . H(11R) H 0.0142 0.2492 0.8454 0.056 Uiso 1 1 calc R . . H(11S) H 0.0079 0.0828 0.8111 0.114 Uiso 1 1 calc R . . H(11T) H -0.0010 0.1143 0.7440 0.114 Uiso 1 1 calc R . . H(11U) H -0.0791 0.1286 0.7950 0.114 Uiso 1 1 calc R . . H(123) H -0.2462 0.3150 0.8711 0.059 Uiso 1 1 calc R . . H(125) H -0.2610 0.1537 0.6475 0.056 Uiso 1 1 calc R . . H(12A) H -0.1540 0.4005 0.9766 0.068 Uiso 1 1 calc R . . H(12B) H -0.0688 0.4694 1.0101 0.068 Uiso 1 1 calc R . . H(12C) H -0.0525 0.3779 0.9625 0.068 Uiso 1 1 calc R . . H(12D) H -0.0592 0.4454 0.8807 0.046 Uiso 1 1 calc R . . H(12E) H -0.1986 0.4944 0.8430 0.089 Uiso 1 1 calc R . . H(12F) H -0.1574 0.5416 0.9362 0.089 Uiso 1 1 calc R . . H(12G) H -0.2441 0.4741 0.9033 0.089 Uiso 1 1 calc R . . H(12H) H -0.2692 0.0870 0.7417 0.251 Uiso 1 1 calc R . . H(12I) H -0.3672 0.0696 0.7595 0.251 Uiso 1 1 calc R . . H(12J) H -0.2836 0.1253 0.8306 0.251 Uiso 1 1 calc R . . H(12K) H -0.3627 0.2118 0.8167 0.090 Uiso 1 1 calc R . . H(12L) H -0.4162 0.1297 0.6509 0.149 Uiso 1 1 calc R . . H(12M) H -0.4526 0.2108 0.7055 0.149 Uiso 1 1 calc R . . H(12N) H -0.4790 0.1292 0.7105 0.149 Uiso 1 1 calc R . . H(12O) H -0.2038 0.1048 0.5412 0.077 Uiso 1 1 calc R . . H(12P) H -0.1036 0.1130 0.5960 0.077 Uiso 1 1 calc R . . H(12Q) H -0.1114 0.1182 0.5135 0.077 Uiso 1 1 calc R . . H(12R) H -0.0771 0.2477 0.6111 0.043 Uiso 1 1 calc R . . H(12S) H -0.2696 0.2301 0.5387 0.064 Uiso 1 1 calc R . . H(12T) H -0.1858 0.2366 0.4984 0.064 Uiso 1 1 calc R . . H(12U) H -0.2011 0.3113 0.5755 0.064 Uiso 1 1 calc R . . H(133) H -0.0220 0.2805 0.4373 0.078 Uiso 1 1 calc R . . H(135) H 0.0801 0.0935 0.4679 0.082 Uiso 1 1 calc R . . H(13A) H 0.1979 0.4296 0.5859 0.092 Uiso 1 1 calc R . . H(13B) H 0.1388 0.5024 0.5897 0.092 Uiso 1 1 calc R . . H(13C) H 0.1333 0.4266 0.5069 0.092 Uiso 1 1 calc R . . H(13D) H 0.0634 0.4251 0.6364 0.058 Uiso 1 1 calc R . . H(13E) H -0.0410 0.4105 0.4876 0.118 Uiso 1 1 calc R . . H(13F) H -0.0371 0.4839 0.5718 0.118 Uiso 1 1 calc R . . H(13G) H -0.0873 0.3979 0.5516 0.118 Uiso 1 1 calc R . . H(13H) H -0.0058 0.0746 0.2449 0.130 Uiso 1 1 calc R . . H(13I) H 0.0869 0.0939 0.3121 0.130 Uiso 1 1 calc R . . H(13J) H 0.0416 0.1649 0.2958 0.130 Uiso 1 1 calc R . . H(13K) H -0.0185 0.0721 0.3580 0.176 Uiso 1 1 calc R . . H(13L) H -0.1463 0.1617 0.3367 0.186 Uiso 1 1 calc R . . H(13M) H -0.1442 0.0999 0.3755 0.186 Uiso 1 1 calc R . . H(13N) H -0.1428 0.0685 0.2838 0.186 Uiso 1 1 calc R . . H(13O) H 0.2740 0.1161 0.5377 0.151 Uiso 1 1 calc R . . H(13P) H 0.3183 0.1341 0.6275 0.151 Uiso 1 1 calc R . . H(13Q) H 0.3071 0.2063 0.6023 0.151 Uiso 1 1 calc R . . H(13R) H 0.1897 0.1992 0.6686 0.076 Uiso 1 1 calc R . . H(13S) H 0.0759 0.0860 0.6115 0.168 Uiso 1 1 calc R . . H(13T) H 0.1772 0.0630 0.6369 0.168 Uiso 1 1 calc R . . H(13U) H 0.1341 0.0409 0.5459 0.168 Uiso 1 1 calc R . . H(213) H 0.4869 0.4002 0.1383 0.046 Uiso 1 1 calc R . . H(215) H 0.7056 0.2730 0.1032 0.053 Uiso 1 1 calc R . . H(21A) H 0.3595 0.4210 0.1810 0.088 Uiso 1 1 calc R . . H(21B) H 0.3932 0.3941 0.2506 0.088 Uiso 1 1 calc R . . H(21C) H 0.2850 0.3816 0.2095 0.088 Uiso 1 1 calc R . . H(21D) H 0.3425 0.2587 0.1593 0.044 Uiso 1 1 calc R . . H(21E) H 0.2296 0.2797 0.0678 0.084 Uiso 1 1 calc R . . H(21F) H 0.3009 0.2231 0.0230 0.084 Uiso 1 1 calc R . . H(21G) H 0.3082 0.3156 0.0401 0.084 Uiso 1 1 calc R . . H(21H) H 0.7456 0.4536 0.2247 0.148 Uiso 1 1 calc R . . H(21I) H 0.7837 0.4858 0.1687 0.148 Uiso 1 1 calc R . . H(21J) H 0.7914 0.3950 0.1551 0.148 Uiso 1 1 calc R . . H(21K) H 0.6217 0.4618 0.1293 0.066 Uiso 1 1 calc R . . H(21L) H 0.7106 0.3483 0.0162 0.105 Uiso 1 1 calc R . . H(21M) H 0.6976 0.4377 0.0269 0.105 Uiso 1 1 calc R . . H(21N) H 0.6088 0.3723 -0.0064 0.105 Uiso 1 1 calc R . . H(21O) H 0.7824 0.1811 0.1346 0.100 Uiso 1 1 calc R . . H(21P) H 0.7630 0.1029 0.1479 0.100 Uiso 1 1 calc R . . H(21Q) H 0.7375 0.1874 0.2067 0.100 Uiso 1 1 calc R . . H(21R) H 0.6047 0.1020 0.1131 0.065 Uiso 1 1 calc R . . H(21S) H 0.6858 0.1226 -0.0026 0.127 Uiso 1 1 calc R . . H(21T) H 0.5841 0.0782 -0.0203 0.127 Uiso 1 1 calc R . . H(21U) H 0.6743 0.0404 0.0052 0.127 Uiso 1 1 calc R . . H(223) H 0.5076 0.2362 0.5557 0.053 Uiso 1 1 calc R . . H(225) H 0.6071 0.4153 0.5141 0.056 Uiso 1 1 calc R . . H(22A) H 0.6458 0.0787 0.4173 0.075 Uiso 1 1 calc R . . H(22B) H 0.5807 0.0121 0.4230 0.075 Uiso 1 1 calc R . . H(22C) H 0.6200 0.0940 0.4998 0.075 Uiso 1 1 calc R . . H(22D) H 0.4892 0.0819 0.3623 0.045 Uiso 1 1 calc R . . H(22E) H 0.4526 0.1125 0.5133 0.078 Uiso 1 1 calc R . . H(22F) H 0.4144 0.0334 0.4332 0.078 Uiso 1 1 calc R . . H(22G) H 0.3780 0.1173 0.4429 0.078 Uiso 1 1 calc R . . H(22H) H 0.6185 0.3343 0.6920 0.160 Uiso 1 1 calc R . . H(22I) H 0.6297 0.4290 0.7449 0.160 Uiso 1 1 calc R . . H(22J) H 0.6907 0.3915 0.6797 0.160 Uiso 1 1 calc R . . H(22K) H 0.5669 0.4502 0.6334 0.065 Uiso 1 1 calc R . . H(22L) H 0.4114 0.3967 0.6086 0.106 Uiso 1 1 calc R . . H(22M) H 0.4591 0.4379 0.7009 0.106 Uiso 1 1 calc R . . H(22N) H 0.4462 0.3425 0.6532 0.106 Uiso 1 1 calc R . . H(22O) H 0.7702 0.3718 0.4376 0.105 Uiso 1 1 calc R . . H(22P) H 0.7654 0.3527 0.3470 0.105 Uiso 1 1 calc R . . H(22Q) H 0.7555 0.2810 0.3720 0.105 Uiso 1 1 calc R . . H(22R) H 0.6084 0.2997 0.3130 0.058 Uiso 1 1 calc R . . H(22S) H 0.5426 0.4212 0.3746 0.109 Uiso 1 1 calc R . . H(22T) H 0.6283 0.4322 0.3383 0.109 Uiso 1 1 calc R . . H(22U) H 0.6425 0.4604 0.4316 0.109 Uiso 1 1 calc R . . H(233) H 0.1610 0.3443 0.3281 0.053 Uiso 1 1 calc R . . H(235) H 0.0653 0.1715 0.1087 0.051 Uiso 1 1 calc R . . H(23A) H 0.3510 0.3879 0.3823 0.084 Uiso 1 1 calc R . . H(23B) H 0.3778 0.3899 0.4684 0.084 Uiso 1 1 calc R . . H(23C) H 0.2735 0.4004 0.4337 0.084 Uiso 1 1 calc R . . H(23D) H 0.3623 0.2573 0.3769 0.048 Uiso 1 1 calc R . . H(23E) H 0.2039 0.2816 0.4472 0.078 Uiso 1 1 calc R . . H(23F) H 0.3065 0.2769 0.4905 0.078 Uiso 1 1 calc R . . H(23G) H 0.2500 0.1995 0.4161 0.078 Uiso 1 1 calc R . . H(23H) H 0.0000 0.4121 0.1863 0.159 Uiso 1 1 calc R . . H(23I) H 0.0809 0.3652 0.1473 0.159 Uiso 1 1 calc R . . H(23J) H 0.0995 0.4179 0.2410 0.159 Uiso 1 1 calc R . . H(23K) H -0.0211 0.2759 0.1517 0.072 Uiso 1 1 calc R . . H(23L) H -0.0002 0.3655 0.3167 0.134 Uiso 1 1 calc R . . H(23M) H -0.0630 0.2817 0.2637 0.134 Uiso 1 1 calc R . . H(23N) H -0.0900 0.3596 0.2514 0.134 Uiso 1 1 calc R . . H(23O) H 0.0844 0.0657 0.0101 0.083 Uiso 1 1 calc R . . H(23P) H 0.1612 0.0070 -0.0200 0.083 Uiso 1 1 calc R . . H(23Q) H 0.1865 0.1018 0.0156 0.083 Uiso 1 1 calc R . . H(23R) H 0.2492 0.0514 0.1084 0.048 Uiso 1 1 calc R . . H(23S) H 0.1511 -0.0001 0.1639 0.086 Uiso 1 1 calc R . . H(23T) H 0.1330 -0.0545 0.0706 0.086 Uiso 1 1 calc R . . H(23U) H 0.0613 0.0076 0.1062 0.086 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) 0.03024(15) 0.02657(15) 0.02352(15) 0.00301(11) 0.00271(11) 0.01053(12) Ge(2) 0.03630(16) 0.02620(15) 0.02753(16) -0.00172(12) -0.00015(12) 0.01250(13) S(11) 0.0341(3) 0.0323(4) 0.0236(3) 0.0043(3) 0.0029(3) 0.0114(3) S(12) 0.0330(3) 0.0335(4) 0.0303(4) 0.0067(3) 0.0050(3) 0.0155(3) S(13) 0.0337(3) 0.0373(4) 0.0273(4) 0.0029(3) 0.0055(3) 0.0139(3) S(21) 0.0460(4) 0.0279(4) 0.0275(4) -0.0022(3) 0.0026(3) 0.0097(3) S(22) 0.0374(4) 0.0359(4) 0.0337(4) -0.0003(3) -0.0007(3) 0.0163(3) S(23) 0.0369(4) 0.0370(4) 0.0372(4) -0.0024(3) -0.0004(3) 0.0217(3) C(111) 0.0354(14) 0.0315(15) 0.0255(14) 0.0018(11) 0.0011(11) 0.0150(12) C(112) 0.0335(14) 0.0305(15) 0.0268(15) 0.0048(11) 0.0032(11) 0.0142(12) C(113) 0.0401(15) 0.0362(16) 0.0322(16) 0.0072(12) 0.0050(12) 0.0168(13) C(114) 0.0547(18) 0.0301(15) 0.0317(16) 0.0088(13) 0.0025(13) 0.0145(13) C(115) 0.0508(18) 0.0325(16) 0.0392(18) -0.0065(13) -0.0058(14) 0.0198(14) C(116) 0.0364(15) 0.0382(17) 0.0358(17) -0.0040(12) -0.0037(12) 0.0210(14) C(11A) 0.0455(17) 0.0386(18) 0.047(2) -0.0072(14) 0.0000(14) 0.0166(15) C(11B) 0.0335(14) 0.0321(15) 0.0380(17) 0.0031(12) 0.0060(12) 0.0193(13) C(11C) 0.0507(18) 0.054(2) 0.064(2) 0.0061(16) 0.0221(17) 0.0329(18) C(11D) 0.163(5) 0.059(3) 0.112(4) 0.048(3) -0.049(4) 0.023(3) C(11E) 0.073(2) 0.0325(17) 0.046(2) 0.0121(15) 0.0159(17) 0.0171(15) C(11F) 0.471(14) 0.126(5) 0.299(10) 0.201(7) 0.335(11) 0.154(6) C(11G) 0.0457(19) 0.097(3) 0.073(3) 0.0139(19) 0.0161(18) 0.057(2) C(11H) 0.0359(16) 0.054(2) 0.060(2) -0.0071(14) 0.0001(14) 0.0378(18) C(11I) 0.051(2) 0.075(3) 0.095(3) -0.0264(19) -0.005(2) 0.040(3) C(121) 0.0293(13) 0.0370(16) 0.0282(15) 0.0043(12) 0.0024(11) 0.0130(13) C(122) 0.0327(14) 0.0441(17) 0.0279(15) 0.0014(13) 0.0034(12) 0.0123(14) C(123) 0.0419(17) 0.067(2) 0.0339(18) -0.0085(16) 0.0087(14) 0.0168(17) C(124) 0.0484(18) 0.062(2) 0.0404(19) -0.0180(16) 0.0023(15) 0.0175(17) C(125) 0.0461(17) 0.0452(19) 0.0346(18) -0.0096(14) -0.0009(14) 0.0092(15) C(126) 0.0336(14) 0.0410(17) 0.0291(15) 0.0032(12) 0.0027(12) 0.0148(13) C(12A) 0.0411(16) 0.056(2) 0.0275(16) -0.0001(14) 0.0031(13) 0.0096(15) C(12B) 0.0369(15) 0.0447(18) 0.0286(16) 0.0010(13) 0.0068(12) 0.0106(14) C(12C) 0.067(2) 0.053(2) 0.044(2) 0.0158(17) 0.0055(17) 0.0102(17) C(12D) 0.075(3) 0.154(6) 0.363(11) 0.018(3) 0.049(5) 0.196(7) C(12E) 0.077(3) 0.083(3) 0.056(2) -0.037(2) 0.011(2) 0.025(2) C(12F) 0.059(2) 0.116(4) 0.101(4) -0.034(3) 0.010(2) 0.029(3) C(12G) 0.059(2) 0.0416(19) 0.045(2) 0.0092(15) 0.0095(16) 0.0108(16) C(12H) 0.0356(15) 0.0400(17) 0.0260(15) 0.0023(12) 0.0018(12) 0.0099(13) C(12I) 0.0420(16) 0.0494(19) 0.0306(16) 0.0021(14) 0.0027(13) 0.0138(15) C(131) 0.0433(16) 0.0373(16) 0.0243(15) -0.0041(13) 0.0070(12) 0.0111(13) C(132) 0.0390(16) 0.061(2) 0.0314(17) -0.0101(14) 0.0040(13) 0.0254(16) C(133) 0.0443(18) 0.116(4) 0.0339(19) -0.024(2) -0.0012(15) 0.038(2) C(134) 0.074(3) 0.089(3) 0.034(2) -0.047(2) 0.0204(19) -0.009(2) C(135) 0.092(3) 0.055(2) 0.040(2) -0.022(2) 0.034(2) -0.0042(19) C(136) 0.065(2) 0.0387(18) 0.0387(19) -0.0051(15) 0.0268(16) 0.0095(15) C(13A) 0.051(2) 0.067(2) 0.087(3) 0.0017(17) 0.0142(19) 0.055(2) C(13B) 0.0404(17) 0.064(2) 0.058(2) 0.0004(15) 0.0042(15) 0.0444(19) C(13C) 0.050(2) 0.116(4) 0.109(4) 0.009(2) 0.003(2) 0.092(3) C(13D) 0.112(3) 0.087(3) 0.035(2) -0.036(3) 0.022(2) 0.000(2) C(13E) 0.109(4) 0.219(7) 0.030(2) -0.107(4) 0.021(2) -0.022(3) C(13F) 0.076(3) 0.172(6) 0.045(3) -0.007(3) -0.011(2) -0.017(3) C(13G) 0.113(4) 0.121(4) 0.130(4) 0.067(3) 0.084(3) 0.088(4) C(13H) 0.097(3) 0.0385(19) 0.071(3) 0.0244(19) 0.053(2) 0.0252(19) C(13I) 0.190(6) 0.042(2) 0.127(5) 0.023(3) 0.083(4) 0.038(3) C(211) 0.0412(15) 0.0267(14) 0.0271(15) 0.0035(12) 0.0068(12) 0.0115(12) C(212) 0.0417(15) 0.0322(15) 0.0238(14) 0.0062(12) 0.0057(12) 0.0126(12) C(213) 0.0505(17) 0.0321(16) 0.0391(17) 0.0114(13) 0.0152(14) 0.0193(14) C(214) 0.0528(18) 0.0332(16) 0.0473(19) 0.0075(14) 0.0192(15) 0.0208(15) C(215) 0.0477(17) 0.0338(16) 0.056(2) 0.0078(13) 0.0217(15) 0.0188(15) C(216) 0.0476(17) 0.0273(15) 0.0452(19) 0.0074(13) 0.0152(14) 0.0147(14) C(21A) 0.0520(19) 0.053(2) 0.062(2) 0.0148(16) 0.0201(17) 0.0134(19) C(21B) 0.0408(15) 0.0373(16) 0.0345(16) 0.0083(13) 0.0072(13) 0.0194(14) C(21C) 0.0451(18) 0.081(3) 0.043(2) 0.0036(17) 0.0021(15) 0.0311(19) C(21D) 0.113(4) 0.053(3) 0.109(4) -0.041(2) -0.011(3) 0.032(3) C(21E) 0.058(2) 0.0383(18) 0.082(3) 0.0099(15) 0.030(2) 0.0317(19) C(21F) 0.067(2) 0.077(3) 0.097(3) 0.011(2) 0.037(2) 0.060(3) C(21G) 0.081(3) 0.058(2) 0.063(3) 0.031(2) 0.015(2) 0.027(2) C(21H) 0.0507(19) 0.0325(17) 0.084(3) 0.0105(14) 0.0275(19) 0.0251(18) C(21I) 0.070(2) 0.053(2) 0.077(3) 0.026(2) -0.010(2) -0.013(2) C(221) 0.0379(15) 0.0331(16) 0.0315(16) -0.0021(12) -0.0073(12) 0.0128(13) C(222) 0.0368(15) 0.0366(16) 0.0307(16) 0.0041(12) -0.0038(12) 0.0122(14) C(223) 0.0448(17) 0.0492(19) 0.0353(18) 0.0060(14) 0.0016(13) 0.0183(15) C(224) 0.0434(17) 0.0322(16) 0.0396(18) 0.0057(13) -0.0076(14) 0.0059(14) C(225) 0.0482(18) 0.0313(16) 0.049(2) -0.0017(13) -0.0079(15) 0.0149(15) C(226) 0.0378(15) 0.0375(17) 0.0398(18) -0.0021(13) -0.0086(13) 0.0161(15) C(22A) 0.0552(19) 0.0432(19) 0.049(2) 0.0074(15) -0.0026(15) 0.0236(16) C(22B) 0.0424(16) 0.0378(17) 0.0311(16) -0.0014(13) 0.0002(12) 0.0162(14) C(22C) 0.058(2) 0.054(2) 0.050(2) -0.0018(16) 0.0108(16) 0.0287(18) C(22D) 0.129(4) 0.090(3) 0.041(2) 0.050(3) -0.030(2) -0.011(2) C(22E) 0.066(2) 0.0410(19) 0.042(2) 0.0137(16) -0.0003(16) 0.0093(16) C(22F) 0.094(3) 0.067(3) 0.041(2) 0.004(2) 0.019(2) 0.0127(19) C(22H) 0.054(2) 0.079(3) 0.083(3) -0.0124(19) -0.0006(19) 0.048(2) C(22I) 0.0509(18) 0.0384(18) 0.048(2) -0.0123(14) -0.0087(15) 0.0203(16) C(22J) 0.096(3) 0.044(2) 0.080(3) -0.001(2) 0.002(2) 0.036(2) C(231) 0.0343(14) 0.0393(16) 0.0362(17) -0.0005(12) 0.0034(12) 0.0218(14) C(232) 0.0350(15) 0.0431(17) 0.0349(17) 0.0010(13) 0.0055(12) 0.0192(14) C(233) 0.0440(17) 0.0408(18) 0.0453(19) 0.0050(14) 0.0106(14) 0.0156(15) C(234) 0.0385(16) 0.053(2) 0.048(2) 0.0070(14) 0.0063(14) 0.0303(17) C(235) 0.0387(16) 0.052(2) 0.0363(17) 0.0026(14) 0.0025(13) 0.0211(16) C(236) 0.0307(14) 0.0424(17) 0.0354(16) -0.0032(12) 0.0037(12) 0.0206(14) C(23A) 0.058(2) 0.047(2) 0.046(2) -0.0084(16) 0.0040(16) 0.0078(17) C(23B) 0.0406(16) 0.0436(18) 0.0313(16) 0.0009(13) 0.0047(13) 0.0129(14) C(23C) 0.0550(19) 0.062(2) 0.0335(18) -0.0023(16) 0.0035(15) 0.0187(17) C(23D) 0.086(3) 0.088(3) 0.184(6) 0.035(3) 0.038(3) 0.093(4) C(23E) 0.053(2) 0.066(2) 0.067(3) 0.0203(18) 0.0085(18) 0.036(2) C(23F) 0.062(2) 0.125(4) 0.109(4) 0.045(3) 0.035(2) 0.069(3) C(23H) 0.058(2) 0.062(2) 0.0347(19) 0.0050(17) -0.0019(15) 0.0156(17) C(23I) 0.0377(15) 0.0430(17) 0.0339(17) -0.0040(13) -0.0014(12) 0.0163(14) C(23J) 0.062(2) 0.045(2) 0.060(2) -0.0084(16) 0.0092(18) 0.0191(18) # 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) S(12) 2.2150(7) YES Ge(1) S(13) 2.2154(7) YES Ge(1) S(11) 2.2160(7) YES Ge(1) H(1) 1.45(2) YES Ge(2) S(21) 2.2083(8) YES Ge(2) S(23) 2.2147(7) YES Ge(2) S(22) 2.2156(8) YES Ge(2) H(2) 1.46(3) YES S(11) C(111) 1.800(3) YES S(12) C(121) 1.797(3) YES S(13) C(131) 1.801(3) YES S(21) C(211) 1.800(3) YES S(22) C(221) 1.796(3) YES S(23) C(231) 1.803(3) YES C(111) C(116) 1.410(4) YES C(111) C(112) 1.411(3) YES C(112) C(113) 1.383(4) YES C(112) C(11B) 1.523(4) YES C(113) C(114) 1.386(4) YES C(114) C(115) 1.378(4) YES C(114) C(11E) 1.522(4) YES C(115) C(116) 1.390(4) YES C(116) C(11H) 1.528(4) YES C(11A) C(11B) 1.527(4) YES C(11B) C(11C) 1.532(4) YES C(11D) C(11E) 1.468(6) YES C(11E) C(11F) 1.511(6) YES C(11G) C(11H) 1.524(5) YES C(11H) C(11I) 1.541(4) YES C(121) C(122) 1.413(4) YES C(121) C(126) 1.416(4) YES C(122) C(123) 1.382(4) YES C(122) C(12B) 1.522(4) YES C(123) C(124) 1.383(4) YES C(124) C(125) 1.389(4) YES C(124) C(12E) 1.511(4) YES C(125) C(126) 1.381(4) YES C(126) C(12H) 1.516(4) YES C(12A) C(12B) 1.533(4) YES C(12B) C(12C) 1.529(4) YES C(12D) C(12E) 1.409(6) YES C(12E) C(12F) 1.495(6) YES C(12G) C(12H) 1.536(4) YES C(12H) C(12I) 1.522(4) YES C(131) C(132) 1.399(4) YES C(131) C(136) 1.408(4) YES C(132) C(133) 1.413(4) YES C(132) C(13B) 1.516(5) YES C(133) C(134) 1.409(6) YES C(134) C(135) 1.360(6) YES C(134) C(13E) 1.523(5) YES C(135) C(136) 1.373(5) YES C(136) C(13H) 1.510(5) YES C(13A) C(13B) 1.539(4) YES C(13B) C(13C) 1.534(4) YES C(13D) C(13E) 1.456(5) YES C(13E) C(13F) 1.346(6) YES C(13G) C(13H) 1.532(5) YES C(13H) C(13I) 1.531(5) YES C(211) C(212) 1.403(4) YES C(211) C(216) 1.412(4) YES C(212) C(213) 1.395(4) YES C(212) C(21B) 1.527(4) YES C(213) C(214) 1.375(4) YES C(214) C(215) 1.392(4) YES C(214) C(21E) 1.521(4) YES C(215) C(216) 1.395(4) YES C(216) C(21H) 1.522(4) YES C(21A) C(21B) 1.529(4) YES C(21B) C(21C) 1.521(4) YES C(21D) C(21E) 1.521(5) YES C(21E) C(21F) 1.522(5) YES C(21G) C(21H) 1.516(5) YES C(21H) C(21I) 1.523(5) YES C(221) C(226) 1.408(4) YES C(221) C(222) 1.410(4) YES C(222) C(223) 1.397(4) YES C(222) C(22B) 1.527(4) YES C(223) C(224) 1.405(4) YES C(224) C(225) 1.379(4) YES C(224) C(22E) 1.520(4) YES C(225) C(226) 1.396(4) YES C(226) C(22I) 1.520(4) YES C(22A) C(22B) 1.533(4) YES C(22B) C(22C) 1.525(4) YES C(22D) C(22E) 1.535(5) YES C(22E) C(22F) 1.505(5) YES C(22H) C(22I) 1.531(4) YES C(22I) C(22J) 1.519(5) YES C(231) C(232) 1.405(4) YES C(231) C(236) 1.411(4) YES C(232) C(233) 1.389(4) YES C(232) C(23B) 1.531(4) YES C(233) C(234) 1.388(4) YES C(234) C(235) 1.380(4) YES C(234) C(23E) 1.521(4) YES C(235) C(236) 1.393(4) YES C(236) C(23I) 1.520(4) YES C(23A) C(23B) 1.529(4) YES C(23B) C(23C) 1.528(4) YES C(23D) C(23E) 1.481(5) YES C(23E) C(23F) 1.506(5) YES C(23H) C(23I) 1.530(4) YES C(23I) C(23J) 1.526(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 S(12) Ge(1) S(13) 111.70(3) YES S(12) Ge(1) S(11) 110.77(3) YES S(13) Ge(1) S(11) 109.80(3) YES S(12) Ge(1) H(1) 106.5(9) YES S(13) Ge(1) H(1) 107.9(9) YES S(11) Ge(1) H(1) 110.1(10) YES S(21) Ge(2) S(23) 109.38(3) YES S(21) Ge(2) S(22) 111.47(3) YES S(23) Ge(2) S(22) 110.56(3) YES S(21) Ge(2) H(2) 111.6(10) YES S(23) Ge(2) H(2) 107.7(9) YES S(22) Ge(2) H(2) 106.0(10) YES C(111) S(11) Ge(1) 93.33(9) YES C(121) S(12) Ge(1) 95.41(9) YES C(131) S(13) Ge(1) 94.94(9) YES C(211) S(21) Ge(2) 96.51(9) YES C(221) S(22) Ge(2) 93.79(9) YES C(231) S(23) Ge(2) 95.76(9) YES C(116) C(111) C(112) 120.7(3) YES C(116) C(111) S(11) 119.9(2) YES C(112) C(111) S(11) 119.32(19) YES C(113) C(112) C(111) 117.9(2) YES C(113) C(112) C(11B) 120.1(2) YES C(111) C(112) C(11B) 121.9(2) YES C(112) C(113) C(114) 122.8(3) YES C(115) C(114) C(113) 118.0(3) YES C(115) C(114) C(11E) 120.7(3) YES C(113) C(114) C(11E) 121.3(3) YES C(114) C(115) C(116) 122.7(3) YES C(115) C(116) C(111) 117.9(2) YES C(115) C(116) C(11H) 119.9(3) YES C(111) C(116) C(11H) 122.2(3) YES C(112) C(11B) C(11A) 109.7(2) YES C(112) C(11B) C(11C) 113.6(2) YES C(11A) C(11B) C(11C) 110.0(2) YES C(11D) C(11E) C(11F) 104.8(5) YES C(11D) C(11E) C(114) 111.1(3) YES C(11F) C(11E) C(114) 113.4(3) YES C(11G) C(11H) C(116) 110.3(3) YES C(11G) C(11H) C(11I) 111.3(3) YES C(116) C(11H) C(11I) 112.6(3) YES C(122) C(121) C(126) 120.9(3) YES C(122) C(121) S(12) 119.7(2) YES C(126) C(121) S(12) 119.4(2) YES C(123) C(122) C(121) 118.0(3) YES C(123) C(122) C(12B) 119.5(3) YES C(121) C(122) C(12B) 122.4(3) YES C(122) C(123) C(124) 122.6(3) YES C(123) C(124) C(125) 118.0(3) YES C(123) C(124) C(12E) 121.1(3) YES C(125) C(124) C(12E) 120.9(3) YES C(126) C(125) C(124) 122.9(3) YES C(125) C(126) C(121) 117.5(3) YES C(125) C(126) C(12H) 119.9(3) YES C(121) C(126) C(12H) 122.4(2) YES C(122) C(12B) C(12C) 109.9(2) YES C(122) C(12B) C(12A) 112.4(3) YES C(12C) C(12B) C(12A) 111.2(3) YES C(12D) C(12E) C(12F) 114.6(4) YES C(12D) C(12E) C(124) 111.9(4) YES C(12F) C(12E) C(124) 113.3(4) YES C(126) C(12H) C(12I) 110.3(2) YES C(126) C(12H) C(12G) 113.0(3) YES C(12I) C(12H) C(12G) 111.5(2) YES C(132) C(131) C(136) 122.1(3) YES C(132) C(131) S(13) 118.9(2) YES C(136) C(131) S(13) 119.0(2) YES C(131) C(132) C(133) 116.7(3) YES C(131) C(132) C(13B) 121.9(3) YES C(133) C(132) C(13B) 121.3(3) YES C(134) C(133) C(132) 121.7(4) YES C(135) C(134) C(133) 118.2(3) YES C(135) C(134) C(13E) 123.6(5) YES C(133) C(134) C(13E) 118.2(5) YES C(134) C(135) C(136) 123.4(4) YES C(135) C(136) C(131) 117.9(4) YES C(135) C(136) C(13H) 119.3(3) YES C(131) C(136) C(13H) 122.7(3) YES C(132) C(13B) C(13C) 114.1(3) YES C(132) C(13B) C(13A) 110.8(3) YES C(13C) C(13B) C(13A) 110.2(3) YES C(13F) C(13E) C(13D) 123.2(4) YES C(13F) C(13E) C(134) 119.6(4) YES C(13D) C(13E) C(134) 113.7(3) YES C(136) C(13H) C(13I) 114.1(4) YES C(136) C(13H) C(13G) 109.9(3) YES C(13I) C(13H) C(13G) 110.3(3) YES C(212) C(211) C(216) 121.2(2) YES C(212) C(211) S(21) 120.0(2) YES C(216) C(211) S(21) 118.7(2) YES C(213) C(212) C(211) 118.0(2) YES C(213) C(212) C(21B) 119.1(2) YES C(211) C(212) C(21B) 122.9(2) YES C(214) C(213) C(212) 122.5(3) YES C(213) C(214) C(215) 118.4(3) YES C(213) C(214) C(21E) 121.7(3) YES C(215) C(214) C(21E) 119.9(3) YES C(214) C(215) C(216) 122.2(3) YES C(215) C(216) C(211) 117.7(3) YES C(215) C(216) C(21H) 118.6(3) YES C(211) C(216) C(21H) 123.7(2) YES C(21C) C(21B) C(212) 111.4(2) YES C(21C) C(21B) C(21A) 110.7(3) YES C(212) C(21B) C(21A) 113.0(2) YES C(214) C(21E) C(21D) 112.5(3) YES C(214) C(21E) C(21F) 110.5(3) YES C(21D) C(21E) C(21F) 109.5(3) YES C(21G) C(21H) C(216) 114.1(3) YES C(21G) C(21H) C(21I) 110.5(3) YES C(216) C(21H) C(21I) 109.8(3) YES C(226) C(221) C(222) 122.1(3) YES C(226) C(221) S(22) 118.6(2) YES C(222) C(221) S(22) 119.3(2) YES C(223) C(222) C(221) 117.5(3) YES C(223) C(222) C(22B) 120.5(3) YES C(221) C(222) C(22B) 122.0(2) YES C(222) C(223) C(224) 122.0(3) YES C(225) C(224) C(223) 118.3(3) YES C(225) C(224) C(22E) 120.6(3) YES C(223) C(224) C(22E) 121.1(3) YES C(224) C(225) C(226) 122.8(3) YES C(225) C(226) C(221) 117.4(3) YES C(225) C(226) C(22I) 119.7(3) YES C(221) C(226) C(22I) 122.9(3) YES C(22C) C(22B) C(222) 113.5(2) YES C(22C) C(22B) C(22A) 110.7(3) YES C(222) C(22B) C(22A) 110.1(2) YES C(22F) C(22E) C(224) 113.7(3) YES C(22F) C(22E) C(22D) 111.1(4) YES C(224) C(22E) C(22D) 110.7(3) YES C(22J) C(22I) C(226) 114.5(3) YES C(22J) C(22I) C(22H) 111.1(3) YES C(226) C(22I) C(22H) 109.6(3) YES C(232) C(231) C(236) 121.3(3) YES C(232) C(231) S(23) 119.7(2) YES C(236) C(231) S(23) 118.9(2) YES C(233) C(232) C(231) 117.6(3) YES C(233) C(232) C(23B) 120.2(3) YES C(231) C(232) C(23B) 122.1(3) YES C(234) C(233) C(232) 122.7(3) YES C(235) C(234) C(233) 117.9(3) YES C(235) C(234) C(23E) 120.7(3) YES C(233) C(234) C(23E) 121.3(3) YES C(234) C(235) C(236) 122.7(3) YES C(235) C(236) C(231) 117.6(3) YES C(235) C(236) C(23I) 120.1(3) YES C(231) C(236) C(23I) 122.3(3) YES C(23C) C(23B) C(23A) 111.2(3) YES C(23C) C(23B) C(232) 109.9(2) YES C(23A) C(23B) C(232) 113.1(3) YES C(23D) C(23E) C(23F) 113.4(4) YES C(23D) C(23E) C(234) 112.0(3) YES C(23F) C(23E) C(234) 113.0(3) YES C(236) C(23I) C(23J) 110.1(2) YES C(236) C(23I) C(23H) 113.4(3) YES C(23J) C(23I) C(23H) 111.1(3) YES #===END data_SW2234 _database_code_CSD 195676 _audit_creation_date 14-05-02 _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 0.35 _exptl_crystal_size_min 0.23 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C48 H68 Ge2 O4' _chemical_formula_moiety 'C48 H68 Ge2 O4' _chemical_formula_structural ? _chemical_formula_weight 854.25 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.2589(3) _cell_length_b 13.0851(2) _cell_length_c 23.0812(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.1600(10) _cell_angle_gamma 90.00 _cell_volume 4638.5(2) _cell_measurement_reflns_used 45027 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.315 _cell_measurement_temperature 150 _exptl_crystal_F_000 1808 # 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 0.5276 _exptl_absorpt_correction_T_max 0.7438 _diffrn_reflns_number 45027 _diffrn_measured_fraction_theta_max 0.9988 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9988 _reflns_number_total 10573 _reflns_number_gt 7759 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 29 # 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 0.039 _refine_ls_wR_factor_ref 0.082 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10548 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.55 _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(1) Ge 0.099371(18) 0.07379(2) 0.280434(11) 0.02713(8) Uani 1 1 d . . . Ge(2) Ge 0.101022(17) -0.03443(2) 0.405694(11) 0.02498(8) Uani 1 1 d . . . O(1) O 0.06991(12) 0.19413(13) 0.30830(7) 0.0340(4) Uani 1 1 d . . . O(2) O 0.12213(11) -0.16772(13) 0.39226(7) 0.0292(4) Uani 1 1 d . . . O(3) O 0.17693(11) 0.02730(13) 0.36169(7) 0.0267(4) Uani 1 1 d . . . O(4) O 0.02655(10) -0.00698(12) 0.31976(7) 0.0244(4) Uani 1 1 d . . . C(11) C 0.03052(17) 0.27891(19) 0.27550(11) 0.0290(6) Uani 1 1 d . . . C(12) C -0.03634(18) 0.2727(2) 0.21817(11) 0.0310(6) Uani 1 1 d . . . C(13) C -0.07465(19) 0.3634(2) 0.19095(13) 0.0384(7) Uani 1 1 d . . . C(14) C -0.0485(2) 0.4570(2) 0.21789(14) 0.0452(7) Uani 1 1 d . . . C(15) C 0.0175(2) 0.4623(2) 0.27390(14) 0.0419(7) Uani 1 1 d . . . C(16) C 0.05743(18) 0.3746(2) 0.30421(12) 0.0318(6) Uani 1 1 d . . . C(21) C 0.12765(18) -0.24185(19) 0.43691(11) 0.0295(6) Uani 1 1 d . . . C(22) C 0.20957(19) -0.2677(2) 0.47808(11) 0.0341(6) Uani 1 1 d . . . C(23) C 0.2125(2) -0.3430(2) 0.52215(12) 0.0420(7) Uani 1 1 d . . . C(24) C 0.1387(2) -0.3909(2) 0.52464(13) 0.0445(8) Uani 1 1 d . . . C(25) C 0.0587(2) -0.3654(2) 0.48273(12) 0.0394(7) Uani 1 1 d . . . C(26) C 0.05155(18) -0.29122(19) 0.43796(11) 0.0319(6) Uani 1 1 d . . . C(31) C 0.26598(16) 0.0107(2) 0.37324(10) 0.0302(6) Uani 1 1 d . . . C(32) C 0.32450(18) 0.0775(2) 0.41426(12) 0.0365(6) Uani 1 1 d . . . C(33) C 0.4128(2) 0.0575(3) 0.42731(14) 0.0517(9) Uani 1 1 d . . . C(34) C 0.4415(2) -0.0206(3) 0.39917(14) 0.0573(9) Uani 1 1 d . . . C(35) C 0.3825(2) -0.0825(3) 0.35682(13) 0.0498(8) Uani 1 1 d . . . C(36) C 0.29310(18) -0.0693(2) 0.34321(11) 0.0352(6) Uani 1 1 d . . . C(41) C -0.06327(16) -0.02478(18) 0.29553(11) 0.0255(5) Uani 1 1 d . . . C(42) C -0.09174(18) -0.0986(2) 0.24886(12) 0.0333(6) Uani 1 1 d . . . C(43) C -0.1808(2) -0.1154(2) 0.22480(14) 0.0446(7) Uani 1 1 d . . . C(44) C -0.2386(2) -0.0643(3) 0.24643(15) 0.0531(8) Uani 1 1 d . . . C(45) C -0.20917(19) 0.0078(2) 0.29174(14) 0.0444(7) Uani 1 1 d . . . C(46) C -0.12046(17) 0.0312(2) 0.31711(11) 0.0311(6) Uani 1 1 d . . . C(121) C -0.0317(2) 0.1631(2) 0.13017(12) 0.0471(8) Uani 1 1 d . . . C(122) C -0.06757(18) 0.1739(2) 0.18380(12) 0.0365(6) Uani 1 1 d . . . C(123) C -0.1671(2) 0.1633(3) 0.16119(14) 0.0528(8) Uani 1 1 d . . . C(161) C 0.1719(2) 0.4836(2) 0.38226(15) 0.0484(8) Uani 1 1 d . . . C(162) C 0.12838(19) 0.3790(2) 0.36646(12) 0.0366(7) Uani 1 1 d . . . C(163) C 0.0916(2) 0.3464(3) 0.41733(13) 0.0527(9) Uani 1 1 d . . . C(221) C 0.3277(2) -0.1438(3) 0.53184(16) 0.0640(10) Uani 1 1 d . . . C(222) C 0.29255(19) -0.2167(2) 0.47730(13) 0.0425(7) Uani 1 1 d . . . C(223) C 0.3626(2) -0.2934(3) 0.47503(16) 0.0603(9) Uani 1 1 d . . . C(261) C -0.0886(2) -0.1980(3) 0.42345(17) 0.0613(9) Uani 1 1 d . . . C(262) C -0.03732(19) -0.2648(2) 0.39322(13) 0.0404(7) Uani 1 1 d . . . C(263) C -0.0915(2) -0.3589(3) 0.36469(15) 0.0549(8) Uani 1 1 d . . . C(321) C 0.3477(2) 0.2623(3) 0.44908(15) 0.0577(9) Uani 1 1 d . . . C(322) C 0.29236(19) 0.1659(2) 0.44342(12) 0.0413(7) Uani 1 1 d . . . C(323) C 0.2864(2) 0.1374(3) 0.50610(13) 0.0514(8) Uani 1 1 d . . . C(361) C 0.2335(2) -0.1106(3) 0.23095(12) 0.0568(9) Uani 1 1 d . . . C(362) C 0.23024(19) -0.1370(2) 0.29520(11) 0.0379(7) Uani 1 1 d . . . C(363) C 0.2461(2) -0.2517(3) 0.30750(15) 0.0578(9) Uani 1 1 d . . . C(421) C -0.0316(3) -0.1217(3) 0.16267(16) 0.0686(11) Uani 1 1 d . . . C(422) C -0.02940(19) -0.1571(2) 0.22490(12) 0.0399(7) Uani 1 1 d . . . C(423) C -0.0455(4) -0.2715(3) 0.2226(2) 0.1038(19) Uani 1 1 d . . . C(461) C -0.1366(2) 0.2159(2) 0.33999(14) 0.0452(7) Uani 1 1 d . . . C(462) C -0.09110(19) 0.1152(2) 0.36482(11) 0.0338(6) Uani 1 1 d . . . C(463) C -0.1058(3) 0.0885(3) 0.42542(14) 0.0573(9) Uani 1 1 d . . . H(13) H -0.1202 0.3607 0.1526 0.046 Uiso 1 1 calc R . . H(14) H -0.0756 0.5178 0.1981 0.054 Uiso 1 1 calc R . . H(15) H 0.0358 0.5272 0.2920 0.050 Uiso 1 1 calc R . . H(23) H 0.2672 -0.3613 0.5510 0.050 Uiso 1 1 calc R . . H(24) H 0.1425 -0.4413 0.5550 0.053 Uiso 1 1 calc R . . H(25) H 0.0078 -0.3990 0.4845 0.047 Uiso 1 1 calc R . . H(33) H 0.4542 0.0990 0.4564 0.062 Uiso 1 1 calc R . . H(34) H 0.5022 -0.0323 0.4088 0.069 Uiso 1 1 calc R . . H(35) H 0.4033 -0.1348 0.3367 0.060 Uiso 1 1 calc R . . H(43) H -0.2024 -0.1635 0.1925 0.054 Uiso 1 1 calc R . . H(44) H -0.2991 -0.0788 0.2300 0.064 Uiso 1 1 calc R . . H(45) H -0.2499 0.0426 0.3062 0.053 Uiso 1 1 calc R . . H(122) H -0.0433 0.1164 0.2129 0.044 Uiso 1 1 calc R . . H(12A) H -0.0491 0.2226 0.1031 0.071 Uiso 1 1 calc R . . H(12B) H -0.0551 0.1009 0.1070 0.071 Uiso 1 1 calc R . . H(12C) H 0.0320 0.1591 0.1462 0.071 Uiso 1 1 calc R . . H(12D) H -0.1887 0.1715 0.1959 0.079 Uiso 1 1 calc R . . H(12E) H -0.1833 0.0956 0.1429 0.079 Uiso 1 1 calc R . . H(12F) H -0.1928 0.2160 0.1304 0.079 Uiso 1 1 calc R . . H(162) H 0.1744 0.3285 0.3660 0.044 Uiso 1 1 calc R . . H(16A) H 0.1939 0.5054 0.3494 0.073 Uiso 1 1 calc R . . H(16B) H 0.2204 0.4790 0.4209 0.073 Uiso 1 1 calc R . . H(16C) H 0.1293 0.5335 0.3865 0.073 Uiso 1 1 calc R . . H(16D) H 0.1384 0.3472 0.4570 0.079 Uiso 1 1 calc R . . H(16E) H 0.0674 0.2773 0.4089 0.079 Uiso 1 1 calc R . . H(16F) H 0.0457 0.3941 0.4185 0.079 Uiso 1 1 calc R . . H(222) H 0.2778 -0.1745 0.4391 0.051 Uiso 1 1 calc R . . H(22A) H 0.2823 -0.0947 0.5320 0.096 Uiso 1 1 calc R . . H(22B) H 0.3784 -0.1071 0.5283 0.096 Uiso 1 1 calc R . . H(22C) H 0.3450 -0.1831 0.5701 0.096 Uiso 1 1 calc R . . H(22D) H 0.3821 -0.3324 0.5134 0.091 Uiso 1 1 calc R . . H(22E) H 0.4122 -0.2565 0.4698 0.091 Uiso 1 1 calc R . . H(22F) H 0.3385 -0.3402 0.4405 0.091 Uiso 1 1 calc R . . H(262) H -0.0281 -0.2242 0.3591 0.048 Uiso 1 1 calc R . . H(26A) H -0.1037 -0.2380 0.4544 0.092 Uiso 1 1 calc R . . H(26B) H -0.1420 -0.1740 0.3923 0.092 Uiso 1 1 calc R . . H(26C) H -0.0531 -0.1391 0.4431 0.092 Uiso 1 1 calc R . . H(26D) H -0.0566 -0.4049 0.3487 0.082 Uiso 1 1 calc R . . H(26E) H -0.1434 -0.3374 0.3312 0.082 Uiso 1 1 calc R . . H(26F) H -0.1093 -0.3946 0.3960 0.082 Uiso 1 1 calc R . . H(322) H 0.2321 0.1828 0.4161 0.050 Uiso 1 1 calc R . . H(32A) H 0.4065 0.2496 0.4776 0.087 Uiso 1 1 calc R . . H(32B) H 0.3211 0.3187 0.4645 0.087 Uiso 1 1 calc R . . H(32C) H 0.3511 0.2804 0.4087 0.087 Uiso 1 1 calc R . . H(32D) H 0.2461 0.0799 0.5015 0.077 Uiso 1 1 calc R . . H(32E) H 0.2652 0.1962 0.5234 0.077 Uiso 1 1 calc R . . H(32F) H 0.3442 0.1177 0.5336 0.077 Uiso 1 1 calc R . . H(362) H 0.1701 -0.1216 0.2954 0.045 Uiso 1 1 calc R . . H(36A) H 0.2245 -0.0370 0.2238 0.085 Uiso 1 1 calc R . . H(36B) H 0.1875 -0.1480 0.1999 0.085 Uiso 1 1 calc R . . H(36C) H 0.2903 -0.1299 0.2283 0.085 Uiso 1 1 calc R . . H(36D) H 0.3048 -0.2692 0.3077 0.087 Uiso 1 1 calc R . . H(36E) H 0.2031 -0.2906 0.2752 0.087 Uiso 1 1 calc R . . H(36F) H 0.2404 -0.2686 0.3474 0.087 Uiso 1 1 calc R . . H(422) H 0.0308 -0.1449 0.2538 0.048 Uiso 1 1 calc R . . H(42A) H -0.0905 -0.1301 0.1335 0.103 Uiso 1 1 calc R . . H(42B) H 0.0093 -0.1624 0.1491 0.103 Uiso 1 1 calc R . . H(42C) H -0.0149 -0.0495 0.1647 0.103 Uiso 1 1 calc R . . H(42D) H -0.0440 -0.2955 0.2632 0.156 Uiso 1 1 calc R . . H(42E) H -0.0002 -0.3065 0.2107 0.156 Uiso 1 1 calc R . . H(42F) H -0.1027 -0.2864 0.1925 0.156 Uiso 1 1 calc R . . H(462) H -0.0272 0.1254 0.3738 0.041 Uiso 1 1 calc R . . H(46A) H -0.1276 0.2322 0.3011 0.068 Uiso 1 1 calc R . . H(46B) H -0.1122 0.2706 0.3696 0.068 Uiso 1 1 calc R . . H(46C) H -0.1991 0.2094 0.3333 0.068 Uiso 1 1 calc R . . H(46D) H -0.1673 0.0719 0.4174 0.086 Uiso 1 1 calc R . . H(46E) H -0.0897 0.1470 0.4534 0.086 Uiso 1 1 calc R . . H(46F) H -0.0698 0.0295 0.4442 0.086 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) 0.02686(16) 0.03006(15) 0.02258(13) -0.00259(12) 0.00555(10) 0.00162(11) Ge(2) 0.02461(15) 0.02791(15) 0.02232(13) 0.00122(12) 0.00759(10) 0.00060(10) O(1) 0.0455(12) 0.0238(9) 0.0272(9) -0.0026(9) 0.0045(8) 0.0017(7) O(2) 0.0307(10) 0.0273(10) 0.0308(9) 0.0035(8) 0.0117(7) 0.0056(7) O(3) 0.0208(9) 0.0348(10) 0.0233(8) -0.0007(8) 0.0055(7) 0.0008(7) O(4) 0.0200(9) 0.0258(9) 0.0248(8) -0.0004(7) 0.0040(7) -0.0013(7) C(11) 0.0308(15) 0.0281(14) 0.0316(13) 0.0019(12) 0.0148(11) 0.0040(11) C(12) 0.0313(15) 0.0329(15) 0.0315(13) -0.0005(12) 0.0140(11) 0.0050(11) C(13) 0.0347(17) 0.0359(16) 0.0453(16) 0.0057(13) 0.0142(13) 0.0085(13) C(14) 0.047(2) 0.0331(16) 0.0569(19) 0.0110(14) 0.0193(15) 0.0078(14) C(15) 0.0483(19) 0.0279(15) 0.0557(18) 0.0016(14) 0.0255(15) -0.0029(13) C(16) 0.0332(16) 0.0287(15) 0.0394(14) -0.0021(12) 0.0199(12) -0.0030(11) C(21) 0.0376(16) 0.0262(14) 0.0274(13) 0.0038(12) 0.0146(11) 0.0025(10) C(22) 0.0379(17) 0.0331(15) 0.0311(13) 0.0056(13) 0.0111(12) 0.0022(11) C(23) 0.0459(19) 0.0398(17) 0.0336(14) 0.0104(14) 0.0039(13) 0.0067(12) C(24) 0.066(2) 0.0319(16) 0.0385(16) 0.0061(15) 0.0217(15) 0.0131(13) C(25) 0.052(2) 0.0296(15) 0.0430(16) -0.0020(14) 0.0244(14) 0.0037(12) C(26) 0.0394(17) 0.0270(14) 0.0333(14) 0.0023(12) 0.0175(12) 0.0000(11) C(31) 0.0204(14) 0.0451(17) 0.0233(12) -0.0017(12) 0.0046(10) 0.0024(11) C(32) 0.0248(15) 0.0507(18) 0.0300(13) -0.0029(13) 0.0035(11) -0.0055(12) C(33) 0.0284(17) 0.078(3) 0.0432(17) -0.0073(16) 0.0038(13) -0.0151(16) C(34) 0.0213(17) 0.093(3) 0.0541(19) 0.0018(17) 0.0076(14) -0.0173(19) C(35) 0.0333(18) 0.078(2) 0.0405(16) 0.0064(16) 0.0149(13) -0.0118(16) C(36) 0.0281(15) 0.0511(18) 0.0270(13) 0.0037(13) 0.0098(11) -0.0013(12) C(41) 0.0218(13) 0.0229(13) 0.0295(12) -0.0006(11) 0.0051(10) 0.0064(10) C(42) 0.0314(16) 0.0293(15) 0.0347(14) -0.0038(12) 0.0050(11) 0.0001(11) C(43) 0.0362(18) 0.0407(18) 0.0510(17) -0.0144(14) 0.0063(13) -0.0112(14) C(44) 0.0268(18) 0.063(2) 0.067(2) -0.0127(16) 0.0117(15) -0.0045(17) C(45) 0.0264(16) 0.0519(19) 0.0563(18) -0.0002(14) 0.0153(13) 0.0011(15) C(46) 0.0275(15) 0.0326(14) 0.0332(13) 0.0010(12) 0.0100(11) 0.0029(11) C(121) 0.062(2) 0.0407(18) 0.0355(15) 0.0001(16) 0.0121(14) -0.0021(13) C(122) 0.0355(17) 0.0346(16) 0.0340(14) -0.0026(13) 0.0042(11) 0.0070(12) C(123) 0.039(2) 0.054(2) 0.0520(18) -0.0104(16) -0.0023(14) 0.0120(15) C(161) 0.053(2) 0.0384(18) 0.0575(19) -0.0099(16) 0.0238(16) -0.0148(14) C(162) 0.0424(18) 0.0312(15) 0.0396(15) -0.0063(13) 0.0182(13) -0.0071(12) C(163) 0.061(2) 0.060(2) 0.0410(17) -0.0157(18) 0.0228(15) -0.0111(15) C(221) 0.052(2) 0.062(2) 0.070(2) -0.0157(19) 0.0081(18) -0.0077(19) C(222) 0.0318(17) 0.0486(19) 0.0416(15) 0.0054(14) 0.0046(12) 0.0089(13) C(223) 0.044(2) 0.072(3) 0.065(2) 0.0161(18) 0.0168(17) 0.0127(18) C(261) 0.050(2) 0.041(2) 0.090(3) 0.0105(17) 0.0196(19) -0.0022(18) C(262) 0.0345(17) 0.0442(18) 0.0447(16) 0.0007(14) 0.0159(13) 0.0139(13) C(263) 0.041(2) 0.058(2) 0.064(2) -0.0059(17) 0.0151(16) -0.0077(17) C(321) 0.052(2) 0.053(2) 0.057(2) -0.0128(17) 0.0021(16) -0.0043(16) C(322) 0.0319(17) 0.0467(18) 0.0373(15) -0.0043(14) 0.0003(12) -0.0089(13) C(323) 0.055(2) 0.056(2) 0.0433(17) 0.0029(17) 0.0163(15) -0.0128(15) C(361) 0.043(2) 0.097(3) 0.0302(15) 0.0011(19) 0.0126(13) -0.0131(16) C(362) 0.0285(16) 0.0537(19) 0.0317(14) 0.0017(14) 0.0103(11) -0.0104(13) C(363) 0.054(2) 0.054(2) 0.060(2) 0.0117(18) 0.0113(17) -0.0183(17) C(421) 0.085(3) 0.064(2) 0.071(2) 0.018(2) 0.046(2) 0.009(2) C(422) 0.0363(17) 0.0398(17) 0.0353(14) 0.0026(13) 0.0006(12) -0.0126(12) C(423) 0.199(6) 0.043(2) 0.112(4) 0.030(3) 0.109(4) 0.013(2) C(461) 0.048(2) 0.0348(17) 0.0542(18) 0.0089(15) 0.0188(15) 0.0044(14) C(462) 0.0336(16) 0.0306(15) 0.0380(14) 0.0062(12) 0.0129(12) -0.0021(12) C(463) 0.087(3) 0.046(2) 0.0481(19) 0.0100(19) 0.0338(18) 0.0023(15) # 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(1) 1.8234(18) YES Ge(1) O(3) 1.9812(16) YES Ge(1) O(4) 2.0121(16) YES Ge(2) O(2) 1.8236(17) YES Ge(2) O(4) 1.9881(15) YES Ge(2) O(3) 2.0075(16) YES O(1) C(11) 1.377(3) YES O(2) C(21) 1.397(3) YES O(3) C(31) 1.401(3) YES O(4) C(41) 1.401(3) YES C(11) C(12) 1.413(4) YES C(11) C(16) 1.417(4) YES C(12) C(13) 1.391(4) YES C(12) C(122) 1.515(4) YES C(13) C(14) 1.376(4) YES C(14) C(15) 1.384(4) YES C(15) C(16) 1.389(4) YES C(16) C(162) 1.520(4) YES C(21) C(22) 1.400(4) YES C(21) C(26) 1.403(4) YES C(22) C(23) 1.406(4) YES C(22) C(222) 1.511(4) YES C(23) C(24) 1.372(4) YES C(24) C(25) 1.383(4) YES C(25) C(26) 1.394(3) YES C(26) C(262) 1.515(4) YES C(31) C(36) 1.403(4) YES C(31) C(32) 1.405(4) YES C(32) C(33) 1.391(4) YES C(32) C(322) 1.515(4) YES C(33) C(34) 1.373(4) YES C(34) C(35) 1.384(4) YES C(35) C(36) 1.394(4) YES C(36) C(362) 1.522(4) YES C(41) C(46) 1.397(3) YES C(41) C(42) 1.407(3) YES C(42) C(43) 1.388(4) YES C(42) C(422) 1.512(4) YES C(43) C(44) 1.374(4) YES C(44) C(45) 1.372(4) YES C(45) C(46) 1.401(4) YES C(46) C(462) 1.518(4) YES C(121) C(122) 1.538(4) YES C(122) C(123) 1.535(4) YES C(161) C(162) 1.530(4) YES C(162) C(163) 1.542(4) YES C(221) C(222) 1.532(4) YES C(222) C(223) 1.532(4) YES C(261) C(262) 1.526(4) YES C(262) C(263) 1.532(4) YES C(321) C(322) 1.530(4) YES C(322) C(323) 1.527(4) YES C(361) C(362) 1.540(4) YES C(362) C(363) 1.533(4) YES C(421) C(422) 1.498(4) YES C(422) C(423) 1.518(5) YES C(461) C(462) 1.527(4) YES C(462) C(463) 1.535(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(1) O(3) 95.19(7) YES O(1) Ge(1) O(4) 91.88(7) YES O(3) Ge(1) O(4) 72.40(6) YES O(2) Ge(2) O(4) 95.17(7) YES O(2) Ge(2) O(3) 96.75(7) YES O(4) Ge(2) O(3) 72.35(6) YES C(11) O(1) Ge(1) 129.09(15) YES C(21) O(2) Ge(2) 120.59(14) YES C(31) O(3) Ge(1) 121.66(13) YES C(31) O(3) Ge(2) 127.59(14) YES Ge(1) O(3) Ge(2) 107.25(8) YES C(41) O(4) Ge(2) 125.59(13) YES C(41) O(4) Ge(1) 126.70(13) YES Ge(2) O(4) Ge(1) 106.80(7) YES O(1) C(11) C(12) 123.0(2) YES O(1) C(11) C(16) 116.0(2) YES C(12) C(11) C(16) 120.9(2) YES C(13) C(12) C(11) 117.9(2) YES C(13) C(12) C(122) 117.9(2) YES C(11) C(12) C(122) 124.2(2) YES C(14) C(13) C(12) 122.0(3) YES C(13) C(14) C(15) 119.7(3) YES C(14) C(15) C(16) 121.4(3) YES C(15) C(16) C(11) 118.2(3) YES C(15) C(16) C(162) 122.0(3) YES C(11) C(16) C(162) 119.8(2) YES O(2) C(21) C(22) 119.0(2) YES O(2) C(21) C(26) 119.3(2) YES C(22) C(21) C(26) 121.7(2) YES C(21) C(22) C(23) 117.4(3) YES C(21) C(22) C(222) 122.7(2) YES C(23) C(22) C(222) 120.0(3) YES C(24) C(23) C(22) 121.8(3) YES C(23) C(24) C(25) 119.7(3) YES C(24) C(25) C(26) 121.1(3) YES C(25) C(26) C(21) 118.3(3) YES C(25) C(26) C(262) 119.6(2) YES C(21) C(26) C(262) 122.2(2) YES O(3) C(31) C(36) 119.6(2) YES O(3) C(31) C(32) 117.4(2) YES C(36) C(31) C(32) 122.9(2) YES C(33) C(32) C(31) 116.8(3) YES C(33) C(32) C(322) 121.9(3) YES C(31) C(32) C(322) 121.2(2) YES C(34) C(33) C(32) 121.6(3) YES C(33) C(34) C(35) 120.4(3) YES C(34) C(35) C(36) 121.1(3) YES C(35) C(36) C(31) 117.0(3) YES C(35) C(36) C(362) 119.6(2) YES C(31) C(36) C(362) 123.3(2) YES C(46) C(41) O(4) 119.9(2) YES C(46) C(41) C(42) 122.8(2) YES O(4) C(41) C(42) 117.2(2) YES C(43) C(42) C(41) 116.9(3) YES C(43) C(42) C(422) 120.7(3) YES C(41) C(42) C(422) 122.4(2) YES C(44) C(43) C(42) 121.7(3) YES C(45) C(44) C(43) 120.2(3) YES C(44) C(45) C(46) 121.5(3) YES C(41) C(46) C(45) 116.8(3) YES C(41) C(46) C(462) 123.4(2) YES C(45) C(46) C(462) 119.8(2) YES C(12) C(122) C(123) 113.0(2) YES C(12) C(122) C(121) 110.4(2) YES C(123) C(122) C(121) 110.7(2) YES C(16) C(162) C(161) 114.0(2) YES C(16) C(162) C(163) 110.2(2) YES C(161) C(162) C(163) 109.3(2) YES C(22) C(222) C(223) 112.9(3) YES C(22) C(222) C(221) 111.0(2) YES C(223) C(222) C(221) 110.7(3) YES C(26) C(262) C(261) 111.2(3) YES C(26) C(262) C(263) 113.2(3) YES C(261) C(262) C(263) 109.5(3) YES C(32) C(322) C(323) 111.9(3) YES C(32) C(322) C(321) 112.9(3) YES C(323) C(322) C(321) 109.8(2) YES C(36) C(362) C(363) 113.8(2) YES C(36) C(362) C(361) 110.1(2) YES C(363) C(362) C(361) 110.0(3) YES C(421) C(422) C(42) 112.7(3) YES C(421) C(422) C(423) 108.8(3) YES C(42) C(422) C(423) 112.5(3) YES C(46) C(462) C(461) 110.8(2) YES C(46) C(462) C(463) 112.9(2) YES C(461) C(462) C(463) 109.7(2) YES #===END data_SW2237 _database_code_CSD 195677 _audit_creation_date 7-05-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C43 H38 Ge1 O5' _chemical_formula_moiety 'C37 H32 Ge1 O5,C6 H6' _chemical_formula_structural ? _chemical_formula_weight 707.37 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.6278(2) _cell_length_b 18.8016(4) _cell_length_c 19.4563(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.8770(10) _cell_angle_gamma 90.00 _cell_volume 3517.5(2) _cell_measurement_reflns_used 26054 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.901 _cell_measurement_temperature 150 _exptl_crystal_F_000 1472 # 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 0.7958 _exptl_absorpt_correction_T_max 0.8935 _diffrn_reflns_number 26054 _diffrn_measured_fraction_theta_max 0.9950 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9950 _reflns_number_total 8001 _reflns_number_gt 6252 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 24 _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 0.038 _refine_ls_wR_factor_ref 0.088 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7965 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.33 _refine_diff_density_min -0.51 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.88E-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) # 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 0.09088(2) 0.014451(12) 0.153460(11) 0.02672(9) Uani 1 1 d . . . O(1) O 0.05579(13) -0.03346(8) 0.07599(7) 0.0296(3) Uani 1 1 d . . . O(2) O 0.29249(14) -0.00287(8) 0.13103(7) 0.0302(3) Uani 1 1 d . . . O(3) O 0.13296(14) 0.10733(8) 0.15751(8) 0.0304(3) Uani 1 1 d . . . O(4) O -0.09076(14) 0.03600(8) 0.16287(8) 0.0310(3) Uani 1 1 d . . . O(5) O 0.12929(14) -0.03634(8) 0.22880(8) 0.0302(3) Uani 1 1 d . . . C(1) C 0.16798(19) -0.06772(11) 0.04465(11) 0.0275(4) Uani 1 1 d . . . C(2) C 0.3035(2) -0.04219(11) 0.07994(11) 0.0277(4) Uani 1 1 d . . . C(3) C 0.0166(2) 0.14485(11) 0.17855(11) 0.0280(4) Uani 1 1 d . . . C(4) C -0.1012(2) 0.10706(11) 0.17988(11) 0.0274(4) Uani 1 1 d . . . C(11) C 0.15653(19) -0.14793(11) 0.04971(11) 0.0272(4) Uani 1 1 d . . . C(12) C 0.0972(2) -0.18666(12) -0.00487(12) 0.0340(5) Uani 1 1 d . . . C(13) C 0.0860(3) -0.25971(13) -0.00042(14) 0.0451(6) Uani 1 1 d . . . C(14) C 0.1345(2) -0.29479(13) 0.05822(14) 0.0447(6) Uani 1 1 d . . . C(15) C 0.1923(2) -0.25702(13) 0.11319(13) 0.0421(6) Uani 1 1 d . . . C(16) C 0.2034(2) -0.18384(12) 0.10917(12) 0.0359(5) Uani 1 1 d . . . C(21) C 0.4401(2) -0.06332(11) 0.05767(11) 0.0287(4) Uani 1 1 d . . . C(22) C 0.4550(2) -0.10212(12) -0.00283(12) 0.0332(5) Uani 1 1 d . . . C(23) C 0.5859(2) -0.12103(13) -0.02238(13) 0.0400(5) Uani 1 1 d . . . C(24) C 0.7027(2) -0.10230(12) 0.01825(13) 0.0399(6) Uani 1 1 d . . . C(25) C 0.6891(2) -0.06299(12) 0.07814(13) 0.0372(5) Uani 1 1 d . . . C(26) C 0.5580(2) -0.04335(12) 0.09779(12) 0.0323(5) Uani 1 1 d . . . C(31) C 0.0441(2) 0.21999(11) 0.19639(11) 0.0285(5) Uani 1 1 d . . . C(32) C 0.1520(2) 0.25685(12) 0.16695(12) 0.0360(5) Uani 1 1 d . . . C(33) C 0.1782(2) 0.32744(13) 0.18468(13) 0.0424(6) Uani 1 1 d . . . C(34) C 0.0970(2) 0.36230(13) 0.23018(13) 0.0414(6) Uani 1 1 d . . . C(35) C -0.0086(2) 0.32593(13) 0.25969(13) 0.0437(6) Uani 1 1 d . . . C(36) C -0.0342(2) 0.25543(13) 0.24370(12) 0.0384(5) Uani 1 1 d . . . C(41) C -0.2446(2) 0.12720(11) 0.19657(11) 0.0286(4) Uani 1 1 d . . . C(42) C -0.3180(2) 0.08295(12) 0.23886(12) 0.0371(5) Uani 1 1 d . . . C(43) C -0.4551(2) 0.09780(14) 0.25201(13) 0.0439(6) Uani 1 1 d . . . C(44) C -0.5203(2) 0.15674(14) 0.22333(13) 0.0444(6) Uani 1 1 d . . . C(45) C -0.4479(2) 0.20125(14) 0.18144(13) 0.0427(6) Uani 1 1 d . . . C(46) C -0.3112(2) 0.18677(12) 0.16758(12) 0.0341(5) Uani 1 1 d . . . C(51) C 0.0315(2) -0.04067(12) 0.27912(11) 0.0302(5) Uani 1 1 d . . . C(52) C 0.0390(2) 0.00718(12) 0.33385(12) 0.0349(5) Uani 1 1 d . . . C(53) C -0.0609(3) 0.00220(13) 0.38341(13) 0.0437(6) Uani 1 1 d . . . C(54) C -0.1646(3) -0.04905(14) 0.37946(14) 0.0460(6) Uani 1 1 d . . . C(55) C -0.1661(2) -0.09660(13) 0.32516(13) 0.0419(6) Uani 1 1 d . . . C(56) C -0.0695(2) -0.09404(12) 0.27442(12) 0.0339(5) Uani 1 1 d . . . C(57) C 0.1510(3) 0.06316(14) 0.33936(13) 0.0462(6) Uani 1 1 d . . . C(58) C -0.2724(3) -0.05308(18) 0.43320(17) 0.0696(9) Uani 1 1 d . . . C(59) C -0.0729(3) -0.14661(12) 0.21596(13) 0.0413(6) Uani 1 1 d . . . C(901) C -0.2006(4) 0.1965(2) 0.4067(2) 0.0904(12) Uani 1 1 d . . . C(902) C -0.0721(4) 0.2174(2) 0.42894(19) 0.0820(11) Uani 1 1 d . . . C(903) C -0.0181(3) 0.19516(19) 0.49222(18) 0.0693(9) Uani 1 1 d . . . C(904) C -0.0960(3) 0.15311(17) 0.53211(17) 0.0638(8) Uani 1 1 d . . . C(905) C -0.2256(4) 0.1328(2) 0.50900(18) 0.0780(10) Uani 1 1 d . . . C(906) C -0.2762(3) 0.1541(3) 0.4461(2) 0.0917(14) Uani 1 1 d . . . H(1) H 0.1666 -0.0539 -0.0050 0.033 Uiso 1 1 calc R . . H(12) H 0.0640 -0.1628 -0.0455 0.041 Uiso 1 1 calc R . . H(13) H 0.0448 -0.2859 -0.0379 0.054 Uiso 1 1 calc R . . H(14) H 0.1280 -0.3451 0.0607 0.054 Uiso 1 1 calc R . . H(15) H 0.2245 -0.2812 0.1538 0.051 Uiso 1 1 calc R . . H(16) H 0.2431 -0.1579 0.1471 0.043 Uiso 1 1 calc R . . H(22) H 0.3751 -0.1155 -0.0305 0.040 Uiso 1 1 calc R . . H(23) H 0.5960 -0.1469 -0.0638 0.048 Uiso 1 1 calc R . . H(24) H 0.7923 -0.1164 0.0051 0.048 Uiso 1 1 calc R . . H(25) H 0.7694 -0.0496 0.1055 0.045 Uiso 1 1 calc R . . H(26) H 0.5485 -0.0163 0.1385 0.039 Uiso 1 1 calc R . . H(32) H 0.2077 0.2337 0.1348 0.043 Uiso 1 1 calc R . . H(33) H 0.2530 0.3519 0.1651 0.051 Uiso 1 1 calc R . . H(34) H 0.1137 0.4109 0.2411 0.050 Uiso 1 1 calc R . . H(35) H -0.0646 0.3496 0.2914 0.052 Uiso 1 1 calc R . . H(36) H -0.1063 0.2308 0.2654 0.046 Uiso 1 1 calc R . . H(42) H -0.2739 0.0422 0.2589 0.045 Uiso 1 1 calc R . . H(43) H -0.5045 0.0672 0.2810 0.053 Uiso 1 1 calc R . . H(44) H -0.6144 0.1667 0.2323 0.053 Uiso 1 1 calc R . . H(45) H -0.4924 0.2422 0.1620 0.051 Uiso 1 1 calc R . . H(46) H -0.2626 0.2174 0.1383 0.041 Uiso 1 1 calc R . . H(53) H -0.0576 0.0348 0.4208 0.052 Uiso 1 1 calc R . . H(55) H -0.2359 -0.1324 0.3224 0.050 Uiso 1 1 calc R . . H(57A) H 0.2425 0.0402 0.3407 0.069 Uiso 1 1 calc R . . H(57B) H 0.1415 0.0908 0.3816 0.069 Uiso 1 1 calc R . . H(57C) H 0.1419 0.0949 0.2994 0.069 Uiso 1 1 calc R . . H(58A) H -0.2280 -0.0683 0.4772 0.104 Uiso 1 1 calc R . . H(58B) H -0.3446 -0.0874 0.4186 0.104 Uiso 1 1 calc R . . H(58C) H -0.3147 -0.0061 0.4387 0.104 Uiso 1 1 calc R . . H(59A) H -0.1553 -0.1769 0.2183 0.062 Uiso 1 1 calc R . . H(59B) H 0.0110 -0.1762 0.2194 0.062 Uiso 1 1 calc R . . H(59C) H -0.0766 -0.1209 0.1721 0.062 Uiso 1 1 calc R . . H(901) H -0.2379 0.2119 0.3630 0.108 Uiso 1 1 calc R . . H(902) H -0.0189 0.2473 0.4010 0.098 Uiso 1 1 calc R . . H(903) H 0.0729 0.2091 0.5079 0.083 Uiso 1 1 calc R . . H(904) H -0.0599 0.1379 0.5760 0.077 Uiso 1 1 calc R . . H(905) H -0.2806 0.1037 0.5369 0.094 Uiso 1 1 calc R . . H(906) H -0.3660 0.1389 0.4297 0.110 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 0.02350(12) 0.02639(13) 0.03035(14) 0.00024(9) 0.00195(8) -0.00162(10) O(1) 0.0241(7) 0.0331(8) 0.0314(8) 0.0025(6) 0.0002(6) -0.0049(6) O(2) 0.0247(7) 0.0361(9) 0.0300(8) -0.0006(6) 0.0027(6) -0.0050(6) O(3) 0.0265(7) 0.0274(8) 0.0377(9) -0.0004(6) 0.0046(6) -0.0024(7) O(4) 0.0254(7) 0.0252(7) 0.0425(9) -0.0005(6) 0.0034(6) -0.0039(7) O(5) 0.0268(7) 0.0336(8) 0.0305(8) 0.0047(6) 0.0041(6) 0.0016(6) C(1) 0.0248(10) 0.0333(11) 0.0245(11) 0.0002(8) 0.0024(8) -0.0016(9) C(2) 0.0299(10) 0.0268(10) 0.0265(11) -0.0012(9) 0.0017(8) 0.0033(9) C(3) 0.0277(10) 0.0297(11) 0.0264(11) 0.0019(8) 0.0008(8) -0.0001(9) C(4) 0.0286(10) 0.0268(11) 0.0268(11) 0.0011(8) 0.0014(8) -0.0011(9) C(11) 0.0228(9) 0.0323(11) 0.0269(11) 0.0021(8) 0.0039(8) -0.0010(9) C(12) 0.0342(11) 0.0364(13) 0.0311(13) -0.0014(9) -0.0016(9) -0.0018(10) C(13) 0.0490(14) 0.0383(14) 0.0471(16) -0.0062(11) -0.0057(11) -0.0098(12) C(14) 0.0437(13) 0.0310(12) 0.0595(17) 0.0007(10) 0.0040(11) -0.0021(12) C(15) 0.0451(13) 0.0374(14) 0.0437(15) 0.0052(10) 0.0009(10) 0.0070(11) C(16) 0.0389(11) 0.0361(13) 0.0323(13) 0.0037(10) -0.0021(9) -0.0013(10) C(21) 0.0281(10) 0.0271(11) 0.0310(12) -0.0018(8) 0.0024(8) 0.0010(9) C(22) 0.0304(10) 0.0337(12) 0.0356(13) -0.0016(9) 0.0030(9) -0.0028(10) C(23) 0.0373(12) 0.0389(13) 0.0446(15) -0.0004(10) 0.0098(10) -0.0098(11) C(24) 0.0288(11) 0.0348(12) 0.0567(16) 0.0020(10) 0.0091(10) 0.0005(11) C(25) 0.0278(11) 0.0364(13) 0.0470(15) 0.0001(9) -0.0019(9) 0.0024(11) C(26) 0.0305(11) 0.0302(11) 0.0360(13) -0.0026(9) -0.0002(9) 0.0005(10) C(31) 0.0292(10) 0.0285(11) 0.0273(11) 0.0001(8) -0.0045(8) 0.0015(9) C(32) 0.0353(11) 0.0350(12) 0.0377(14) -0.0032(10) 0.0036(9) -0.0014(10) C(33) 0.0433(13) 0.0383(13) 0.0454(15) -0.0124(11) 0.0002(11) 0.0041(11) C(34) 0.0466(13) 0.0285(12) 0.0477(15) -0.0020(10) -0.0117(11) -0.0067(11) C(35) 0.0403(12) 0.0426(14) 0.0476(16) -0.0020(11) -0.0024(11) -0.0172(12) C(36) 0.0368(12) 0.0401(13) 0.0383(14) -0.0062(10) 0.0025(9) -0.0105(11) C(41) 0.0264(10) 0.0298(11) 0.0296(12) 0.0003(8) 0.0003(8) -0.0069(9) C(42) 0.0349(11) 0.0373(13) 0.0393(14) 0.0008(10) 0.0045(9) -0.0002(10) C(43) 0.0322(12) 0.0513(15) 0.0493(16) -0.0053(11) 0.0114(10) -0.0030(12) C(44) 0.0281(11) 0.0566(16) 0.0487(16) 0.0065(11) 0.0034(10) -0.0176(13) C(45) 0.0364(12) 0.0449(14) 0.0461(15) 0.0127(11) -0.0045(10) -0.0113(12) C(46) 0.0349(11) 0.0335(12) 0.0336(13) 0.0031(9) -0.0002(9) -0.0053(10) C(51) 0.0291(10) 0.0316(11) 0.0302(12) 0.0025(9) 0.0042(8) 0.0044(9) C(52) 0.0362(11) 0.0355(12) 0.0330(13) -0.0014(10) 0.0028(9) 0.0001(10) C(53) 0.0515(15) 0.0471(16) 0.0333(14) -0.0017(11) 0.0098(11) -0.0017(11) C(54) 0.0477(14) 0.0465(15) 0.0453(16) 0.0006(12) 0.0168(11) 0.0072(12) C(55) 0.0391(12) 0.0400(14) 0.0469(15) -0.0052(10) 0.0053(10) 0.0092(12) C(56) 0.0364(11) 0.0315(12) 0.0337(13) 0.0004(9) 0.0016(9) 0.0045(10) C(57) 0.0518(14) 0.0467(15) 0.0405(15) -0.0118(12) 0.0040(11) -0.0094(12) C(58) 0.076(2) 0.073(2) 0.064(2) -0.0097(17) 0.0365(17) 0.0065(17) C(59) 0.0476(13) 0.0335(13) 0.0426(15) -0.0047(10) 0.0013(11) 0.0003(11) C(901) 0.082(2) 0.128(4) 0.061(2) 0.039(3) 0.0016(19) 0.015(2) C(902) 0.113(3) 0.073(2) 0.062(2) -0.009(2) 0.023(2) 0.0007(19) C(903) 0.0547(17) 0.081(2) 0.073(2) -0.0008(16) 0.0067(16) -0.0324(19) C(904) 0.071(2) 0.071(2) 0.0490(18) 0.0172(17) 0.0027(15) -0.0080(16) C(905) 0.082(2) 0.097(3) 0.057(2) -0.014(2) 0.0253(18) -0.0129(19) C(906) 0.0454(16) 0.165(4) 0.065(2) 0.016(2) 0.0087(16) -0.028(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 O(5) 1.7729(15) YES Ge O(1) 1.7738(14) YES Ge O(3) 1.7935(14) YES Ge O(4) 1.8132(13) YES Ge O(2) 2.0370(14) YES O(1) C(1) 1.421(2) YES O(2) C(2) 1.248(2) YES O(3) C(3) 1.402(2) YES O(4) C(4) 1.381(2) YES O(5) C(51) 1.394(2) YES C(1) C(11) 1.516(3) YES C(1) C(2) 1.521(3) YES C(2) C(21) 1.460(3) YES C(3) C(4) 1.339(3) YES C(3) C(31) 1.476(3) YES C(4) C(41) 1.484(3) YES C(11) C(12) 1.387(3) YES C(11) C(16) 1.395(3) YES C(12) C(13) 1.381(3) YES C(13) C(14) 1.379(4) YES C(14) C(15) 1.378(3) YES C(15) C(16) 1.383(3) YES C(21) C(26) 1.397(3) YES C(21) C(22) 1.399(3) YES C(22) C(23) 1.381(3) YES C(23) C(24) 1.387(3) YES C(24) C(25) 1.391(3) YES C(25) C(26) 1.387(3) YES C(31) C(36) 1.389(3) YES C(31) C(32) 1.396(3) YES C(32) C(33) 1.391(3) YES C(33) C(34) 1.376(4) YES C(34) C(35) 1.375(3) YES C(35) C(36) 1.381(3) YES C(41) C(42) 1.388(3) YES C(41) C(46) 1.395(3) YES C(42) C(43) 1.386(3) YES C(43) C(44) 1.378(4) YES C(44) C(45) 1.381(4) YES C(45) C(46) 1.384(3) YES C(51) C(52) 1.393(3) YES C(51) C(56) 1.397(3) YES C(52) C(53) 1.399(3) YES C(52) C(57) 1.507(3) YES C(53) C(54) 1.387(4) YES C(54) C(55) 1.383(4) YES C(54) C(58) 1.512(3) YES C(55) C(56) 1.391(3) YES C(56) C(59) 1.506(3) YES C(901) C(906) 1.347(5) YES C(901) C(902) 1.348(5) YES C(902) C(903) 1.377(5) YES C(903) C(904) 1.360(4) YES C(904) C(905) 1.360(4) YES C(905) C(906) 1.354(5) 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(5) Ge O(1) 116.87(7) YES O(5) Ge O(3) 116.80(7) YES O(1) Ge O(3) 124.38(7) YES O(5) Ge O(4) 101.48(7) YES O(1) Ge O(4) 93.20(6) YES O(3) Ge O(4) 89.71(6) YES O(5) Ge O(2) 85.96(6) YES O(1) Ge O(2) 83.09(6) YES O(3) Ge O(2) 87.10(6) YES O(4) Ge O(2) 172.55(6) YES C(1) O(1) Ge 118.58(11) YES C(2) O(2) Ge 112.65(12) YES C(3) O(3) Ge 108.69(12) YES C(4) O(4) Ge 108.81(11) YES C(51) O(5) Ge 119.46(12) YES O(1) C(1) C(11) 111.34(16) YES O(1) C(1) C(2) 108.43(16) YES C(11) C(1) C(2) 110.37(16) YES O(2) C(2) C(21) 120.74(18) YES O(2) C(2) C(1) 116.22(17) YES C(21) C(2) C(1) 123.02(18) YES C(4) C(3) O(3) 115.36(19) YES C(4) C(3) C(31) 130.18(19) YES O(3) C(3) C(31) 114.45(17) YES C(3) C(4) O(4) 115.89(18) YES C(3) C(4) C(41) 131.8(2) YES O(4) C(4) C(41) 112.27(16) YES C(12) C(11) C(16) 119.0(2) YES C(12) C(11) C(1) 120.07(19) YES C(16) C(11) C(1) 120.94(19) YES C(13) C(12) C(11) 120.3(2) YES C(14) C(13) C(12) 120.2(2) YES C(15) C(14) C(13) 120.2(2) YES C(14) C(15) C(16) 119.9(2) YES C(15) C(16) C(11) 120.4(2) YES C(26) C(21) C(22) 119.71(19) YES C(26) C(21) C(2) 118.70(19) YES C(22) C(21) C(2) 121.59(18) YES C(23) C(22) C(21) 120.0(2) YES C(22) C(23) C(24) 120.2(2) YES C(23) C(24) C(25) 120.3(2) YES C(26) C(25) C(24) 119.8(2) YES C(25) C(26) C(21) 120.0(2) YES C(36) C(31) C(32) 118.3(2) YES C(36) C(31) C(3) 121.23(19) YES C(32) C(31) C(3) 120.5(2) YES C(33) C(32) C(31) 120.1(2) YES C(34) C(33) C(32) 120.8(2) YES C(35) C(34) C(33) 119.2(2) YES C(34) C(35) C(36) 120.7(2) YES C(35) C(36) C(31) 120.9(2) YES C(42) C(41) C(46) 118.93(19) YES C(42) C(41) C(4) 118.93(19) YES C(46) C(41) C(4) 122.02(19) YES C(43) C(42) C(41) 120.4(2) YES C(44) C(43) C(42) 120.4(2) YES C(43) C(44) C(45) 119.6(2) YES C(44) C(45) C(46) 120.6(2) YES C(45) C(46) C(41) 120.1(2) YES C(52) C(51) O(5) 119.21(19) YES C(52) C(51) C(56) 121.5(2) YES O(5) C(51) C(56) 119.2(2) YES C(51) C(52) C(53) 118.2(2) YES C(51) C(52) C(57) 121.0(2) YES C(53) C(52) C(57) 120.8(2) YES C(54) C(53) C(52) 121.8(2) YES C(55) C(54) C(53) 118.1(2) YES C(55) C(54) C(58) 121.0(2) YES C(53) C(54) C(58) 120.9(3) YES C(54) C(55) C(56) 122.5(2) YES C(55) C(56) C(51) 117.8(2) YES C(55) C(56) C(59) 121.6(2) YES C(51) C(56) C(59) 120.6(2) YES C(906) C(901) C(902) 120.2(4) YES C(901) C(902) C(903) 119.9(4) YES C(904) C(903) C(902) 119.5(3) YES C(903) C(904) C(905) 119.9(3) YES C(906) C(905) C(904) 119.9(3) YES C(901) C(906) C(905) 120.6(3) YES #===END data_SW2227 _database_code_CSD 195678 _audit_creation_date 19-04-02 _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 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C36 H44 Ge2 O4' _chemical_formula_moiety 'C36 H44 Ge2 O4' _chemical_formula_structural ? _chemical_formula_weight 685.93 _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 7.8478(4) _cell_length_b 20.5354(12) _cell_length_c 21.1481(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.804(3) _cell_angle_gamma 90.00 _cell_volume 3358.4(6) _cell_measurement_reflns_used 15483 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.800 _cell_measurement_temperature 150 _exptl_crystal_F_000 1424 # 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 0.6685 _exptl_absorpt_correction_T_max 0.8353 _diffrn_reflns_number 15483 _diffrn_measured_fraction_theta_max 0.9946 _diffrn_reflns_theta_full 23.8 _diffrn_measured_fraction_theta_full 0.9946 _reflns_number_total 5131 _reflns_number_gt 3967 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 23.85 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_max 24 # 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 0.048 _refine_ls_wR_factor_ref 0.109 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 5127 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 1.95 _refine_diff_density_min -0.60 _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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ge(1) 0.22869(6) 0.19014(3) 0.20409(2) 0.02885(15) Uani ? Ge(2) 0.26948(6) 0.07475(3) 0.30790(2) 0.02918(15) Uani ? O(1) 0.4558(4) 0.21485(17) 0.21961(15) 0.0335(10) Uani ? O(2) 0.0445(4) 0.04859(16) 0.29083(14) 0.0325(10) Uani ? O(3) 0.2199(4) 0.16915(16) 0.29505(14) 0.0307(9) Uani ? O(4) 0.2781(4) 0.09590(16) 0.21712(14) 0.0292(9) Uani ? C(11) 0.4929(6) 0.2671(2) 0.1824(2) 0.0307(15) Uani ? C(12) 0.5675(6) 0.2554(3) 0.1278(2) 0.0325(15) Uani ? C(13) 0.5968(6) 0.3077(3) 0.0902(2) 0.0370(17) Uani ? C(14) 0.5547(6) 0.3713(3) 0.1043(2) 0.0342(15) Uani ? C(15) 0.4867(6) 0.3818(3) 0.1596(2) 0.0375(15) Uani ? C(16) 0.4562(6) 0.3308(3) 0.1999(2) 0.0335(15) Uani ? C(17) 0.6151(7) 0.1877(3) 0.1119(2) 0.0420(16) Uani ? C(18) 0.5799(7) 0.4274(3) 0.0600(2) 0.0470(19) Uani ? C(19) 0.3859(7) 0.3435(3) 0.2608(2) 0.0432(16) Uani ? C(21) 0.0057(6) -0.0038(2) 0.3279(2) 0.0290(15) Uani ? C(22) -0.0608(6) 0.0088(3) 0.3840(2) 0.0339(15) Uani ? C(23) -0.0956(6) -0.0442(3) 0.4210(2) 0.0399(17) Uani ? C(24) -0.0661(6) -0.1077(3) 0.4048(2) 0.0389(17) Uani ? C(25) -0.0019(6) -0.1185(3) 0.3480(2) 0.0385(15) Uani ? C(26) 0.0345(6) -0.0675(3) 0.3085(2) 0.0354(15) Uani ? C(27) -0.0972(7) 0.0773(3) 0.4018(2) 0.0430(17) Uani ? C(28) -0.1003(7) -0.1648(3) 0.4460(3) 0.0501(19) Uani ? C(29) 0.0993(7) -0.0812(3) 0.2467(3) 0.0465(17) Uani ? C(31) 0.1880(6) 0.2120(2) 0.3434(2) 0.0288(14) Uani ? C(32) 0.3215(6) 0.2269(3) 0.3936(2) 0.0320(14) Uani ? C(33) 0.2841(7) 0.2670(3) 0.4414(2) 0.0391(15) Uani ? C(34) 0.1221(7) 0.2940(3) 0.4408(2) 0.0395(16) Uani ? C(35) -0.0066(6) 0.2792(3) 0.3888(2) 0.0371(15) Uani ? C(36) 0.0209(6) 0.2378(2) 0.3396(2) 0.0320(15) Uani ? C(37) 0.5019(6) 0.1996(3) 0.3954(2) 0.0417(17) Uani ? C(38) 0.0846(8) 0.3385(3) 0.4939(3) 0.0548(19) Uani ? C(39) -0.1195(6) 0.2207(3) 0.2842(2) 0.0421(17) Uani ? C(41) 0.3172(6) 0.0526(2) 0.1709(2) 0.0282(14) Uani ? C(42) 0.1845(6) 0.0323(2) 0.1221(2) 0.0297(14) Uani ? C(43) 0.2259(7) -0.0105(3) 0.0769(2) 0.0373(15) Uani ? C(44) 0.3927(7) -0.0356(3) 0.0796(2) 0.0397(16) Uani ? C(45) 0.5185(6) -0.0142(3) 0.1289(2) 0.0379(15) Uani ? C(46) 0.4861(6) 0.0295(2) 0.1756(2) 0.0305(15) Uani ? C(47) 0.0003(6) 0.0555(3) 0.1199(2) 0.0393(17) Uani ? C(48) 0.4322(8) -0.0833(3) 0.0302(3) 0.061(2) Uani ? C(49) 0.6248(6) 0.0512(3) 0.2295(2) 0.0379(17) Uani ? H(13) 0.6477 0.3000 0.0533 0.0440 Uiso calc H(15) 0.4599 0.4250 0.1704 0.0450 Uiso calc H(23) -0.1416 -0.0362 0.4590 0.0480 Uiso calc H(25) 0.0176 -0.1621 0.3357 0.0460 Uiso calc H(33) 0.3734 0.2767 0.4764 0.0470 Uiso calc H(35) -0.1177 0.2983 0.3870 0.0440 Uiso calc H(43) 0.1378 -0.0235 0.0426 0.0440 Uiso calc H(45) 0.6330 -0.0301 0.1310 0.0460 Uiso calc H(17A) 0.6710 0.1886 0.0738 0.0630 Uiso calc H(17B) 0.5105 0.1609 0.1032 0.0630 Uiso calc H(17C) 0.6949 0.1693 0.1482 0.0630 Uiso calc H(18A) 0.5204 0.4661 0.0724 0.0700 Uiso calc H(18B) 0.5318 0.4156 0.0157 0.0700 Uiso calc H(18C) 0.7036 0.4367 0.0634 0.0700 Uiso calc H(19A) 0.3729 0.3906 0.2663 0.0650 Uiso calc H(19B) 0.4661 0.3260 0.2975 0.0650 Uiso calc H(19C) 0.2731 0.3223 0.2582 0.0650 Uiso calc H(27A) 0.0106 0.1024 0.4084 0.0650 Uiso calc H(27B) -0.1460 0.0773 0.4415 0.0650 Uiso calc H(27C) -0.1799 0.0971 0.3673 0.0650 Uiso calc H(28A) -0.1595 -0.1495 0.4805 0.0750 Uiso calc H(28B) 0.0096 -0.1852 0.4647 0.0750 Uiso calc H(28C) -0.1733 -0.1967 0.4196 0.0750 Uiso calc H(29A) 0.0141 -0.0658 0.2105 0.0700 Uiso calc H(29B) 0.1167 -0.1281 0.2426 0.0700 Uiso calc H(29C) 0.2092 -0.0584 0.2470 0.0700 Uiso calc H(37A) 0.5852 0.2257 0.4247 0.0620 Uiso calc H(37B) 0.5315 0.2010 0.3523 0.0620 Uiso calc H(37C) 0.5054 0.1544 0.4105 0.0620 Uiso calc H(38A) 0.1570 0.3258 0.5345 0.0820 Uiso calc H(38B) -0.0376 0.3347 0.4979 0.0820 Uiso calc H(38C) 0.1102 0.3836 0.4837 0.0820 Uiso calc H(39A) -0.2308 0.2368 0.2929 0.0630 Uiso calc H(39B) -0.1251 0.1733 0.2788 0.0630 Uiso calc H(39C) -0.0940 0.2409 0.2449 0.0630 Uiso calc H(47A) -0.0096 0.1009 0.1052 0.0590 Uiso calc H(47B) -0.0301 0.0526 0.1629 0.0590 Uiso calc H(47C) -0.0785 0.0282 0.0901 0.0590 Uiso calc H(48A) 0.5563 -0.0931 0.0380 0.0910 Uiso calc H(48B) 0.3992 -0.0645 -0.0127 0.0910 Uiso calc H(48C) 0.3669 -0.1236 0.0332 0.0910 Uiso calc H(49A) 0.6146 0.0267 0.2685 0.0570 Uiso calc H(49B) 0.6115 0.0978 0.2374 0.0570 Uiso calc H(49C) 0.7386 0.0432 0.2179 0.0570 Uiso calc 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) 0.0293(3) 0.0292(3) 0.0264(3) 0.0007(2) 0.0000(2) 0.0008(2) Ge(2) 0.0292(3) 0.0293(3) 0.0274(3) 0.0000(2) 0.0001(2) 0.0015(2) O(1) 0.0313(19) 0.033(2) 0.0342(18) -0.0018(15) -0.0003(15) 0.0043(15) O(2) 0.0313(18) 0.030(2) 0.0340(18) -0.0022(15) -0.0011(14) 0.0081(15) O(3) 0.0366(19) 0.030(2) 0.0250(16) -0.0009(15) 0.0037(14) -0.0039(14) O(4) 0.0312(18) 0.028(2) 0.0280(17) 0.0012(15) 0.0035(14) -0.0023(14) C(11) 0.032(3) 0.028(3) 0.029(3) -0.001(2) -0.004(2) 0.003(2) C(12) 0.028(3) 0.038(3) 0.030(3) -0.004(2) 0.001(2) 0.001(2) C(13) 0.037(3) 0.044(4) 0.029(3) -0.006(3) 0.003(2) -0.001(2) C(14) 0.032(3) 0.036(3) 0.031(3) -0.008(2) -0.005(2) 0.005(2) C(15) 0.035(3) 0.034(3) 0.040(3) 0.001(2) -0.004(2) -0.003(2) C(16) 0.034(3) 0.033(3) 0.031(3) -0.002(2) -0.002(2) 0.000(2) C(17) 0.051(3) 0.036(3) 0.040(3) 0.006(3) 0.011(3) -0.007(2) C(18) 0.056(4) 0.041(4) 0.042(3) -0.009(3) 0.003(3) 0.006(3) C(19) 0.052(3) 0.037(3) 0.040(3) 0.002(3) 0.006(3) -0.005(3) C(21) 0.025(3) 0.028(3) 0.030(3) -0.004(2) -0.007(2) 0.008(2) C(22) 0.028(3) 0.040(3) 0.032(3) -0.001(2) 0.000(2) 0.004(2) C(23) 0.032(3) 0.052(4) 0.034(3) -0.007(3) 0.001(2) 0.003(3) C(24) 0.032(3) 0.043(4) 0.038(3) -0.012(3) -0.005(2) 0.011(3) C(25) 0.039(3) 0.030(3) 0.042(3) -0.004(2) -0.006(2) 0.005(2) C(26) 0.032(3) 0.036(3) 0.035(3) -0.003(2) -0.003(2) 0.003(2) C(27) 0.046(3) 0.048(4) 0.035(3) 0.006(3) 0.007(2) -0.001(3) C(28) 0.054(4) 0.046(4) 0.046(3) -0.013(3) -0.004(3) 0.013(3) C(29) 0.050(3) 0.043(4) 0.045(3) 0.005(3) 0.004(3) 0.000(3) C(31) 0.034(3) 0.026(3) 0.027(2) -0.003(2) 0.007(2) -0.001(2) C(32) 0.033(3) 0.035(3) 0.027(2) -0.006(2) 0.002(2) 0.000(2) C(33) 0.042(3) 0.045(3) 0.029(3) -0.008(3) 0.002(2) 0.002(2) C(34) 0.052(3) 0.033(3) 0.035(3) 0.002(3) 0.012(3) -0.001(2) C(35) 0.035(3) 0.036(3) 0.042(3) 0.004(2) 0.011(2) -0.002(2) C(36) 0.028(3) 0.033(3) 0.034(3) -0.002(2) 0.002(2) 0.004(2) C(37) 0.032(3) 0.052(4) 0.038(3) -0.005(3) -0.003(2) -0.006(3) C(38) 0.079(4) 0.044(4) 0.043(3) 0.005(3) 0.015(3) -0.011(3) C(39) 0.026(3) 0.050(4) 0.048(3) 0.002(3) 0.000(2) 0.003(3) C(41) 0.029(3) 0.030(3) 0.025(2) -0.002(2) 0.003(2) 0.001(2) C(42) 0.032(3) 0.030(3) 0.026(2) 0.000(2) 0.002(2) 0.006(2) C(43) 0.043(3) 0.039(3) 0.028(3) -0.005(3) 0.001(2) -0.004(2) C(44) 0.052(3) 0.031(3) 0.039(3) 0.002(3) 0.016(3) -0.005(2) C(45) 0.033(3) 0.039(3) 0.043(3) 0.006(2) 0.010(2) 0.007(3) C(46) 0.031(3) 0.028(3) 0.031(3) -0.002(2) 0.001(2) 0.002(2) C(47) 0.031(3) 0.052(4) 0.033(3) -0.003(3) 0.000(2) -0.002(2) C(48) 0.082(5) 0.047(4) 0.054(4) 0.014(3) 0.012(3) -0.014(3) C(49) 0.028(3) 0.047(4) 0.037(3) -0.001(2) 0.001(2) 0.000(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(1) O(1) 1.828(3) YES Ge(1) O(4) 1.984(3) YES Ge(1) O(3) 1.984(3) YES Ge(2) O(2) 1.822(3) YES Ge(2) O(4) 1.981(3) YES Ge(2) O(3) 1.987(3) YES O(1) C(11) 1.391(6) YES O(2) C(21) 1.394(5) YES O(3) C(31) 1.404(5) YES O(4) C(41) 1.393(5) YES C(11) C(12) 1.401(6) YES C(11) C(16) 1.403(7) YES C(12) C(13) 1.378(7) YES C(12) C(17) 1.492(7) YES C(13) C(14) 1.391(7) YES C(14) C(15) 1.382(7) YES C(14) C(18) 1.519(7) YES C(15) C(16) 1.397(7) YES C(16) C(19) 1.507(6) YES C(21) C(22) 1.401(6) YES C(21) C(26) 1.402(7) YES C(22) C(23) 1.394(7) YES C(22) C(27) 1.496(7) YES C(23) C(24) 1.378(8) YES C(24) C(25) 1.398(7) YES C(24) C(28) 1.512(7) YES C(25) C(26) 1.398(7) YES C(26) C(29) 1.507(7) YES C(31) C(32) 1.392(6) YES C(31) C(36) 1.403(6) YES C(32) C(33) 1.374(7) YES C(32) C(37) 1.517(7) YES C(33) C(34) 1.386(7) YES C(34) C(35) 1.394(7) YES C(34) C(38) 1.514(7) YES C(35) C(36) 1.390(7) YES C(36) C(39) 1.506(7) YES C(41) C(46) 1.395(6) YES C(41) C(42) 1.400(6) YES C(42) C(43) 1.377(6) YES C(42) C(47) 1.516(6) YES C(43) C(44) 1.399(7) YES C(44) C(45) 1.380(7) YES C(44) C(48) 1.502(7) YES C(45) C(46) 1.391(7) YES C(46) C(49) 1.503(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) Ge(1) O(4) 94.84(14) YES O(1) Ge(1) O(3) 94.59(13) YES O(4) Ge(1) O(3) 72.04(13) YES O(2) Ge(2) O(4) 93.70(13) YES O(2) Ge(2) O(3) 95.74(14) YES O(4) Ge(2) O(3) 72.03(12) YES C(11) O(1) Ge(1) 113.8(3) YES C(21) O(2) Ge(2) 114.4(3) YES C(31) O(3) Ge(1) 127.6(3) YES C(31) O(3) Ge(2) 124.6(3) YES Ge(1) O(3) Ge(2) 107.84(14) YES C(41) O(4) Ge(2) 126.0(3) YES C(41) O(4) Ge(1) 125.9(3) YES Ge(2) O(4) Ge(1) 108.09(14) YES O(1) C(11) C(12) 119.4(4) YES O(1) C(11) C(16) 119.8(4) YES C(12) C(11) C(16) 120.8(4) YES C(13) C(12) C(11) 118.3(5) YES C(13) C(12) C(17) 121.5(4) YES C(11) C(12) C(17) 120.1(4) YES C(12) C(13) C(14) 122.6(5) YES C(15) C(14) C(13) 117.9(5) YES C(15) C(14) C(18) 120.8(5) YES C(13) C(14) C(18) 121.3(5) YES C(14) C(15) C(16) 122.1(5) YES C(15) C(16) C(11) 118.2(4) YES C(15) C(16) C(19) 121.2(5) YES C(11) C(16) C(19) 120.6(4) YES O(2) C(21) C(22) 118.9(4) YES O(2) C(21) C(26) 119.7(4) YES C(22) C(21) C(26) 121.5(4) YES C(23) C(22) C(21) 117.9(5) YES C(23) C(22) C(27) 122.0(5) YES C(21) C(22) C(27) 120.1(4) YES C(24) C(23) C(22) 122.8(5) YES C(23) C(24) C(25) 117.7(5) YES C(23) C(24) C(28) 122.4(5) YES C(25) C(24) C(28) 119.8(5) YES C(24) C(25) C(26) 122.2(5) YES C(25) C(26) C(21) 117.8(5) YES C(25) C(26) C(29) 120.8(5) YES C(21) C(26) C(29) 121.4(4) YES C(32) C(31) C(36) 122.4(4) YES C(32) C(31) O(3) 119.2(4) YES C(36) C(31) O(3) 118.4(4) YES C(33) C(32) C(31) 117.7(5) YES C(33) C(32) C(37) 121.2(4) YES C(31) C(32) C(37) 121.1(4) YES C(32) C(33) C(34) 123.0(5) YES C(33) C(34) C(35) 117.3(5) YES C(33) C(34) C(38) 122.0(5) YES C(35) C(34) C(38) 120.7(5) YES C(36) C(35) C(34) 122.7(5) YES C(35) C(36) C(31) 116.8(4) YES C(35) C(36) C(39) 122.6(4) YES C(31) C(36) C(39) 120.6(4) YES O(4) C(41) C(46) 119.1(4) YES O(4) C(41) C(42) 118.9(4) YES C(46) C(41) C(42) 122.0(4) YES C(43) C(42) C(41) 118.0(4) YES C(43) C(42) C(47) 121.1(4) YES C(41) C(42) C(47) 121.0(4) YES C(42) C(43) C(44) 122.4(5) YES C(45) C(44) C(43) 117.2(4) YES C(45) C(44) C(48) 121.8(5) YES C(43) C(44) C(48) 121.0(5) YES C(44) C(45) C(46) 123.3(5) YES C(45) C(46) C(41) 117.1(4) YES C(45) C(46) C(49) 122.2(4) YES C(41) C(46) C(49) 120.7(4) YES #===END data_SW2228 _database_code_CSD 195679 _audit_creation_date 23-04-02 _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 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C78 H60 Ge1 O2' _chemical_formula_moiety 'C60 H42 Ge1 O2,3(C6 H6)' _chemical_formula_structural ? _chemical_formula_weight 1101.94 _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 23.9853(5) _cell_length_b 11.2746(3) _cell_length_c 22.0664(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.6330(10) _cell_angle_gamma 90.00 _cell_volume 5947.8(4) _cell_measurement_reflns_used 24772 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.23 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.553 _cell_measurement_temperature 150 _exptl_crystal_F_000 2304 # 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 0.8022 _exptl_absorpt_correction_T_max 0.9078 _diffrn_reflns_number 24772 _diffrn_measured_fraction_theta_max 0.9917 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9917 _reflns_number_total 6774 _reflns_number_gt 5805 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 28 # 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 0.039 _refine_ls_wR_factor_ref 0.096 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6769 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.1634P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.27 _refine_diff_density_min -0.46 _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_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ge 0.0000 0.18719(2) 0.2500 0.02983(7) Uani ? O(1) 0.05422(4) 0.30066(10) 0.26115(5) 0.0288(3) Uani ? C(1) 0.10423(6) 0.28434(14) 0.29496(7) 0.0262(4) Uani ? C(2) 0.15334(6) 0.32130(14) 0.26978(7) 0.0267(4) Uani ? C(3) 0.20472(6) 0.30849(14) 0.30483(7) 0.0269(4) Uani ? C(4) 0.20581(6) 0.25715(15) 0.36218(7) 0.0286(4) Uani ? C(5) 0.15752(6) 0.21827(14) 0.38714(7) 0.0273(4) Uani ? C(6) 0.10557(6) 0.23172(14) 0.35295(7) 0.0264(4) Uani ? C(21) 0.15138(6) 0.37002(16) 0.20678(7) 0.0310(4) Uani ? C(22) 0.12059(8) 0.47062(17) 0.19040(8) 0.0393(5) Uani ? C(23) 0.12146(9) 0.5198(2) 0.13308(9) 0.0538(6) Uani ? C(24) 0.15330(9) 0.4680(2) 0.09098(9) 0.0597(7) Uani ? C(25) 0.18330(8) 0.3660(2) 0.10551(9) 0.0547(7) Uani ? C(26) 0.18238(7) 0.31660(19) 0.16335(8) 0.0404(5) Uani ? C(31) 0.25900(6) 0.34980(15) 0.28360(7) 0.0282(4) Uani ? C(32) 0.26573(7) 0.46453(16) 0.26199(7) 0.0331(4) Uani ? C(33) 0.31736(7) 0.50275(17) 0.24553(8) 0.0402(5) Uani ? C(34) 0.36287(7) 0.42689(18) 0.25013(9) 0.0422(5) Uani ? C(35) 0.35685(7) 0.31209(17) 0.27138(9) 0.0393(5) Uani ? C(36) 0.30523(7) 0.27407(16) 0.28815(7) 0.0317(4) Uani ? C(51) 0.16354(7) 0.16611(15) 0.44943(7) 0.0309(4) Uani ? C(52) 0.20374(7) 0.07928(18) 0.46314(8) 0.0395(5) Uani ? C(53) 0.21128(8) 0.03078(19) 0.52140(9) 0.0475(6) Uani ? C(54) 0.17888(9) 0.0702(2) 0.56640(8) 0.0497(6) Uani ? C(55) 0.13945(9) 0.15743(19) 0.55362(8) 0.0463(6) Uani ? C(56) 0.13144(8) 0.20524(17) 0.49572(8) 0.0374(5) Uani ? C(61) 0.05285(6) 0.18543(15) 0.37569(7) 0.0278(4) Uani ? C(62) 0.04858(7) 0.06678(16) 0.39255(7) 0.0332(4) Uani ? C(63) -0.00111(8) 0.02319(18) 0.41221(8) 0.0426(5) Uani ? C(64) -0.04712(8) 0.0972(2) 0.41425(9) 0.0472(6) Uani ? C(65) -0.04364(7) 0.21422(19) 0.39763(8) 0.0419(5) Uani ? C(66) 0.00615(7) 0.25913(17) 0.37873(7) 0.0333(4) Uani ? C(81) 0.99380(8) 0.1837(2) 0.71961(10) 0.0527(6) Uani ? C(82) 0.98642(10) 0.2881(3) 0.68870(12) 0.0700(8) Uani ? C(83) 0.99306(11) 0.3933(3) 0.71928(15) 0.0854(11) Uani ? C(91) 0.83218(13) 0.3372(4) 0.62179(14) 0.0838(12) Uani ? C(92) 0.84368(13) 0.2345(3) 0.59200(14) 0.0785(10) Uani ? C(93) 0.88274(14) 0.2326(3) 0.55175(12) 0.0751(9) Uani ? C(94) 0.91073(16) 0.3329(3) 0.53961(12) 0.0861(11) Uani ? C(95) 0.89918(16) 0.4378(3) 0.56922(13) 0.0881(11) Uani ? C(96) 0.86009(14) 0.4392(3) 0.61034(13) 0.0812(9) Uani ? H(4) 0.2408 0.2482 0.3852 0.0340 Uiso calc H(22) 0.0984 0.5065 0.2191 0.0470 Uiso calc H(23) 0.1002 0.5890 0.1227 0.0650 Uiso calc H(24) 0.1546 0.5027 0.0519 0.0720 Uiso calc H(25) 0.2045 0.3294 0.0761 0.0660 Uiso calc H(26) 0.2030 0.2463 0.1733 0.0490 Uiso calc H(32) 0.2347 0.5171 0.2585 0.0400 Uiso calc H(33) 0.3215 0.5813 0.2310 0.0480 Uiso calc H(34) 0.3982 0.4533 0.2388 0.0510 Uiso calc H(35) 0.3880 0.2597 0.2744 0.0470 Uiso calc H(36) 0.3013 0.1956 0.3029 0.0380 Uiso calc H(52) 0.2264 0.0526 0.4325 0.0470 Uiso calc H(53) 0.2386 -0.0292 0.5301 0.0570 Uiso calc H(54) 0.1838 0.0372 0.6061 0.0600 Uiso calc H(55) 0.1176 0.1850 0.5848 0.0560 Uiso calc H(56) 0.1040 0.2650 0.4874 0.0450 Uiso calc H(62) 0.0798 0.0154 0.3906 0.0400 Uiso calc H(63) -0.0035 -0.0574 0.4243 0.0510 Uiso calc H(64) -0.0812 0.0669 0.4272 0.0570 Uiso calc H(65) -0.0753 0.2646 0.3990 0.0500 Uiso calc H(66) 0.0085 0.3404 0.3678 0.0400 Uiso calc H(81) 0.9902 0.1106 0.6982 0.0630 Uiso calc H(82) 0.9767 0.2877 0.6461 0.0840 Uiso calc H(83) 0.9881 0.4662 0.6980 0.1030 Uiso calc H(91) 0.8047 0.3373 0.6505 0.1010 Uiso calc H(92) 0.8238 0.1640 0.5999 0.0940 Uiso calc H(93) 0.8907 0.1607 0.5317 0.0900 Uiso calc H(94) 0.9382 0.3316 0.5109 0.1040 Uiso calc H(95) 0.9186 0.5085 0.5607 0.1060 Uiso calc H(96) 0.8522 0.5104 0.6310 0.0970 Uiso calc 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 0.02441(13) 0.02675(14) 0.03721(14) 0.0000 -0.00440(9) 0.0000 O(1) 0.0211(5) 0.0311(6) 0.0332(5) 0.0002(5) -0.0035(4) 0.0033(4) C(1) 0.0216(7) 0.0228(8) 0.0333(8) 0.0008(6) -0.0029(6) -0.0020(6) C(2) 0.0236(7) 0.0237(8) 0.0321(8) -0.0006(6) -0.0013(6) -0.0010(6) C(3) 0.0223(7) 0.0230(8) 0.0349(8) -0.0010(6) -0.0015(6) -0.0017(6) C(4) 0.0237(8) 0.0262(8) 0.0349(8) -0.0006(6) -0.0040(6) 0.0004(6) C(5) 0.0259(8) 0.0244(8) 0.0310(8) 0.0001(6) -0.0005(6) -0.0008(6) C(6) 0.0235(7) 0.0221(7) 0.0333(8) 0.0010(6) 0.0006(6) -0.0027(6) C(21) 0.0239(8) 0.0332(9) 0.0351(8) -0.0070(7) -0.0032(6) 0.0028(7) C(22) 0.0362(9) 0.0354(10) 0.0443(9) -0.0051(8) -0.0087(7) 0.0078(8) C(23) 0.0537(12) 0.0480(13) 0.0561(12) -0.0153(10) -0.0172(10) 0.0203(10) C(24) 0.0544(13) 0.0790(17) 0.0428(11) -0.0314(12) -0.0132(9) 0.0259(11) C(25) 0.0366(10) 0.0894(18) 0.0384(10) -0.0216(11) 0.0044(8) 0.0019(11) C(26) 0.0287(8) 0.0580(12) 0.0343(8) -0.0070(8) 0.0009(7) 0.0026(8) C(31) 0.0245(7) 0.0280(8) 0.0312(8) -0.0024(6) -0.0028(6) 0.0000(6) C(32) 0.0266(8) 0.0286(9) 0.0432(9) -0.0010(7) -0.0029(6) 0.0046(7) C(33) 0.0363(9) 0.0315(10) 0.0524(10) -0.0060(8) 0.0017(8) 0.0100(8) C(34) 0.0260(8) 0.0439(11) 0.0573(11) -0.0063(8) 0.0070(7) 0.0083(9) C(35) 0.0263(8) 0.0381(10) 0.0536(10) 0.0032(8) 0.0034(7) 0.0055(8) C(36) 0.0265(8) 0.0269(8) 0.0413(9) -0.0005(7) 0.0004(6) 0.0038(7) C(51) 0.0278(8) 0.0316(9) 0.0322(8) -0.0078(7) -0.0041(6) 0.0017(6) C(52) 0.0339(9) 0.0404(11) 0.0431(9) -0.0012(8) -0.0040(7) 0.0079(8) C(53) 0.0431(11) 0.0468(12) 0.0497(11) -0.0055(9) -0.0149(8) 0.0151(9) C(54) 0.0599(13) 0.0498(12) 0.0363(9) -0.0243(10) -0.0154(9) 0.0137(8) C(55) 0.0577(12) 0.0483(12) 0.0326(9) -0.0172(10) 0.0022(8) -0.0014(8) C(56) 0.0390(9) 0.0384(10) 0.0342(8) -0.0052(8) -0.0013(7) -0.0003(7) C(61) 0.0237(7) 0.0307(8) 0.0285(7) -0.0020(7) -0.0006(6) -0.0011(6) C(62) 0.0312(8) 0.0313(9) 0.0369(8) -0.0014(7) 0.0017(6) 0.0002(7) C(63) 0.0416(10) 0.0401(11) 0.0466(10) -0.0115(8) 0.0066(8) 0.0032(8) C(64) 0.0330(10) 0.0598(14) 0.0502(11) -0.0113(9) 0.0120(8) -0.0005(10) C(65) 0.0268(9) 0.0566(13) 0.0429(10) 0.0047(8) 0.0074(7) -0.0016(8) C(66) 0.0305(8) 0.0357(10) 0.0337(8) 0.0033(7) 0.0020(6) 0.0001(7) C(81) 0.0375(10) 0.0550(13) 0.0666(12) -0.0072(10) 0.0104(9) -0.0120(10) C(82) 0.0487(13) 0.099(2) 0.0610(14) -0.0029(14) -0.0035(10) 0.0153(14) C(83) 0.0573(16) 0.0572(17) 0.141(3) 0.0045(14) 0.0042(18) 0.0387(17) C(91) 0.0679(18) 0.103(3) 0.0788(19) 0.0187(17) -0.0042(14) -0.0172(17) C(92) 0.082(2) 0.0605(17) 0.089(2) -0.0038(15) -0.0180(16) -0.0036(15) C(93) 0.109(2) 0.0527(16) 0.0601(15) 0.0243(16) -0.0149(15) -0.0142(12) C(94) 0.125(3) 0.087(2) 0.0457(13) 0.012(2) 0.0030(14) -0.0005(14) C(95) 0.137(3) 0.0574(17) 0.0648(16) -0.0059(18) -0.0235(18) 0.0123(13) C(96) 0.108(2) 0.0617(18) 0.0687(17) 0.0324(17) -0.0249(16) -0.0234(14) # 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) 1.8265(11) YES Ge O(1) 1.8266(11) YES O(1) C(1) 1.3730(17) YES C(1) C(2) 1.406(2) YES C(1) C(6) 1.408(2) YES C(2) C(3) 1.409(2) YES C(2) C(21) 1.492(2) YES C(3) C(4) 1.390(2) YES C(3) C(31) 1.493(2) YES C(4) C(5) 1.393(2) YES C(5) C(6) 1.412(2) YES C(5) C(51) 1.491(2) YES C(6) C(61) 1.492(2) YES C(21) C(22) 1.385(3) YES C(21) C(26) 1.396(3) YES C(22) C(23) 1.383(3) YES C(23) C(24) 1.379(3) YES C(24) C(25) 1.381(4) YES C(25) C(26) 1.394(3) YES C(31) C(32) 1.392(2) YES C(31) C(36) 1.397(2) YES C(32) C(33) 1.387(2) YES C(33) C(34) 1.384(3) YES C(34) C(35) 1.388(3) YES C(35) C(36) 1.388(2) YES C(51) C(52) 1.390(3) YES C(51) C(56) 1.399(3) YES C(52) C(53) 1.395(2) YES C(53) C(54) 1.383(3) YES C(54) C(55) 1.377(3) YES C(55) C(56) 1.386(3) YES C(61) C(62) 1.395(2) YES C(61) C(66) 1.401(2) YES C(62) C(63) 1.390(2) YES C(63) C(64) 1.387(3) YES C(64) C(65) 1.374(3) YES C(65) C(66) 1.392(2) YES C(81) C(81) 1.350(4) YES C(81) C(82) 1.365(4) YES C(82) C(83) 1.368(4) YES C(83) C(83) 1.370(6) YES C(91) C(96) 1.365(5) YES C(91) C(92) 1.370(4) YES C(92) C(93) 1.342(4) YES C(93) C(94) 1.352(4) YES C(94) C(95) 1.390(4) YES C(95) C(96) 1.356(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) 91.09(7) YES C(1) O(1) Ge 124.10(10) YES O(1) C(1) C(2) 117.96(14) YES O(1) C(1) C(6) 120.32(14) YES C(2) C(1) C(6) 121.72(14) YES C(1) C(2) C(3) 118.46(14) YES C(1) C(2) C(21) 120.87(13) YES C(3) C(2) C(21) 120.65(14) YES C(4) C(3) C(2) 119.60(14) YES C(4) C(3) C(31) 117.58(13) YES C(2) C(3) C(31) 122.82(14) YES C(3) C(4) C(5) 122.42(14) YES C(4) C(5) C(6) 118.75(14) YES C(4) C(5) C(51) 117.83(14) YES C(6) C(5) C(51) 123.41(14) YES C(1) C(6) C(5) 119.02(14) YES C(1) C(6) C(61) 119.69(13) YES C(5) C(6) C(61) 121.20(14) YES C(22) C(21) C(26) 118.45(16) YES C(22) C(21) C(2) 121.36(16) YES C(26) C(21) C(2) 120.15(16) YES C(23) C(22) C(21) 121.3(2) YES C(24) C(23) C(22) 119.8(2) YES C(23) C(24) C(25) 120.18(19) YES C(24) C(25) C(26) 119.9(2) YES C(25) C(26) C(21) 120.3(2) YES C(32) C(31) C(36) 118.63(15) YES C(32) C(31) C(3) 121.69(15) YES C(36) C(31) C(3) 119.60(15) YES C(33) C(32) C(31) 120.59(16) YES C(34) C(33) C(32) 120.29(17) YES C(33) C(34) C(35) 119.87(16) YES C(34) C(35) C(36) 119.83(17) YES C(35) C(36) C(31) 120.79(17) YES C(52) C(51) C(56) 118.43(16) YES C(52) C(51) C(5) 119.47(15) YES C(56) C(51) C(5) 122.04(15) YES C(51) C(52) C(53) 120.82(19) YES C(54) C(53) C(52) 119.81(19) YES C(55) C(54) C(53) 119.92(17) YES C(54) C(55) C(56) 120.55(19) YES C(55) C(56) C(51) 120.46(18) YES C(62) C(61) C(66) 118.68(15) YES C(62) C(61) C(6) 120.53(14) YES C(66) C(61) C(6) 120.76(15) YES C(63) C(62) C(61) 120.37(17) YES C(64) C(63) C(62) 120.11(19) YES C(65) C(64) C(63) 120.22(17) YES C(64) C(65) C(66) 120.10(17) YES C(65) C(66) C(61) 120.50(18) YES C(81) C(81) C(82) 120.38(15) YES C(81) C(82) C(83) 119.8(2) YES C(82) C(83) C(83) 119.84(16) YES C(96) C(91) C(92) 120.2(3) YES C(93) C(92) C(91) 120.6(3) YES C(92) C(93) C(94) 120.1(3) YES C(93) C(94) C(95) 119.8(3) YES C(96) C(95) C(94) 119.9(3) YES C(95) C(96) C(91) 119.4(3) YES #===END data_SW2271 _database_code_CSD 195680 _audit_creation_date 15-08-02 _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 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C77 H55 Ge1 O4' _chemical_formula_moiety 'C74 H52 Ge1 O4,0.5(C6 H6)' _chemical_formula_structural ? _chemical_formula_weight 1116.88 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9950(5) _cell_length_b 13.7686(5) _cell_length_c 18.9644(10) _cell_angle_alpha 87.5822(16) _cell_angle_beta 83.3595(17) _cell_angle_gamma 86.5014(19) _cell_volume 2844.6(2) _cell_measurement_reflns_used 29897 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _cell_formula_units_z 2 _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 0.581 _cell_measurement_temperature 150 _exptl_crystal_F_000 1162 # 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 0.5908 _exptl_absorpt_correction_T_max 0.9435 _diffrn_reflns_number 29897 _diffrn_measured_fraction_theta_max 0.9957 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 0.9957 _reflns_number_total 9953 _reflns_number_gt 8100 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.211 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 22 # 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 0.081 _refine_ls_wR_factor_ref 0.144 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7361 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0323P)^2^+5.0007P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.41 _refine_diff_density_min -0.48 _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 Ge Ge 0.18517(6) 0.25052(5) 0.28646(4) 0.0297(2) Uani 1 1 d . . . O(2) O 0.1234(3) 0.2012(3) 0.3665(2) 0.0313(10) Uani 1 1 d . . . O(3) O 0.1809(3) 0.3740(3) 0.3014(2) 0.0305(10) Uani 1 1 d . . . O(11) O 0.3325(3) 0.1954(3) 0.2603(2) 0.0336(10) Uani 1 1 d . . . O(14) O 0.1258(4) 0.2284(3) 0.2061(2) 0.0337(10) Uani 1 1 d . . . C(12) C 0.3310(5) 0.1711(4) 0.1889(3) 0.0289(14) Uani 1 1 d . . . C(13) C 0.2265(5) 0.1912(4) 0.1609(3) 0.0319(15) Uani 1 1 d . . . C(21) C 0.1741(5) 0.1202(4) 0.4025(3) 0.0296(15) Uani 1 1 d . . . C(22) C 0.2386(5) 0.1397(4) 0.4594(3) 0.0295(15) Uani 1 1 d . . . C(23) C 0.2786(5) 0.0600(4) 0.5025(3) 0.0282(14) Uani 1 1 d . . . C(24) C 0.2566(5) -0.0337(4) 0.4821(3) 0.0336(15) Uani 1 1 d . . . C(25) C 0.2015(5) -0.0528(4) 0.4223(3) 0.0294(15) Uani 1 1 d . . . C(26) C 0.1557(5) 0.0270(4) 0.3821(3) 0.0275(14) Uani 1 1 d . . . C(31) C 0.1280(5) 0.4498(4) 0.2608(3) 0.0264(14) Uani 1 1 d . . . C(32) C 0.2059(5) 0.5064(4) 0.2142(3) 0.0271(14) Uani 1 1 d . . . C(33) C 0.1519(5) 0.5907(4) 0.1836(3) 0.0280(14) Uani 1 1 d . . . C(34) C 0.0271(5) 0.6136(4) 0.1990(3) 0.0278(14) Uani 1 1 d . . . C(35) C -0.0492(5) 0.5537(4) 0.2425(3) 0.0248(14) Uani 1 1 d . . . C(36) C 0.0013(5) 0.4695(4) 0.2732(3) 0.0239(13) Uani 1 1 d . . . C(121) C 0.4482(5) 0.1239(4) 0.1593(3) 0.0309(15) Uani 1 1 d . . . C(122) C 0.5604(6) 0.1552(4) 0.1764(3) 0.0364(16) Uani 1 1 d . . . C(123) C 0.6704(6) 0.1144(5) 0.1483(3) 0.0362(16) Uani 1 1 d . . . C(124) C 0.6731(6) 0.0389(5) 0.1024(3) 0.0363(16) Uani 1 1 d . . . C(125) C 0.5648(6) 0.0045(4) 0.0853(3) 0.0370(16) Uani 1 1 d . . . C(126) C 0.4528(6) 0.0462(4) 0.1129(3) 0.0325(15) Uani 1 1 d . . . C(131) C 0.2008(6) 0.1867(4) 0.0869(3) 0.0350(16) Uani 1 1 d . . . C(132) C 0.2853(6) 0.2138(4) 0.0306(3) 0.0410(17) Uani 1 1 d . . . C(133) C 0.2560(8) 0.2132(5) -0.0380(4) 0.051(2) Uani 1 1 d . . . C(134) C 0.1432(8) 0.1867(5) -0.0524(4) 0.055(2) Uani 1 1 d . . . C(135) C 0.0579(7) 0.1586(5) 0.0021(4) 0.054(2) Uani 1 1 d . . . C(136) C 0.0850(7) 0.1589(5) 0.0716(4) 0.0468(18) Uani 1 1 d . . . C(221) C 0.2748(6) 0.2418(4) 0.4678(3) 0.0316(15) Uani 1 1 d . . . C(222) C 0.3997(6) 0.2619(5) 0.4556(3) 0.0401(17) Uani 1 1 d . . . C(223) C 0.4347(6) 0.3556(5) 0.4580(4) 0.0470(18) Uani 1 1 d . . . C(224) C 0.3487(7) 0.4308(5) 0.4729(4) 0.0490(19) Uani 1 1 d . . . C(225) C 0.2263(7) 0.4122(5) 0.4850(3) 0.0421(17) Uani 1 1 d . . . C(226) C 0.1904(6) 0.3191(4) 0.4814(3) 0.0364(16) Uani 1 1 d . . . C(231) C 0.3327(5) 0.0690(4) 0.5702(3) 0.0290(14) Uani 1 1 d . . . C(232) C 0.2857(6) 0.1366(4) 0.6192(3) 0.0366(16) Uani 1 1 d . . . C(233) C 0.3266(6) 0.1373(5) 0.6851(4) 0.0420(17) Uani 1 1 d . . . C(234) C 0.4194(6) 0.0715(5) 0.7029(4) 0.0443(18) Uani 1 1 d . . . C(235) C 0.4687(6) 0.0045(5) 0.6541(4) 0.0437(18) Uani 1 1 d . . . C(236) C 0.4257(5) 0.0036(4) 0.5885(3) 0.0354(16) Uani 1 1 d . . . C(251) C 0.1884(6) -0.1556(4) 0.4053(3) 0.0305(15) Uani 1 1 d . . . C(252) C 0.2903(6) -0.2220(4) 0.4014(3) 0.0342(16) Uani 1 1 d . . . C(253) C 0.2792(6) -0.3185(5) 0.3867(3) 0.0412(17) Uani 1 1 d . . . C(254) C 0.1673(7) -0.3500(5) 0.3753(3) 0.0468(19) Uani 1 1 d . . . C(255) C 0.0662(6) -0.2847(5) 0.3781(3) 0.0409(17) Uani 1 1 d . . . C(256) C 0.0767(6) -0.1892(4) 0.3940(3) 0.0363(16) Uani 1 1 d . . . C(261) C 0.0937(6) 0.0132(4) 0.3187(3) 0.0327(15) Uani 1 1 d . . . C(262) C 0.1550(6) -0.0332(5) 0.2593(3) 0.0415(17) Uani 1 1 d . . . C(263) C 0.0932(7) -0.0540(5) 0.2023(4) 0.0513(19) Uani 1 1 d . . . C(264) C -0.0305(8) -0.0264(5) 0.2040(4) 0.058(2) Uani 1 1 d . . . C(265) C -0.0912(7) 0.0207(5) 0.2616(4) 0.052(2) Uani 1 1 d . . . C(266) C -0.0300(6) 0.0408(4) 0.3176(4) 0.0429(18) Uani 1 1 d . . . C(321) C 0.3359(5) 0.4731(4) 0.1951(3) 0.0312(15) Uani 1 1 d . . . C(322) C 0.4170(6) 0.4515(4) 0.2468(4) 0.0393(17) Uani 1 1 d . . . C(323) C 0.5378(6) 0.4199(5) 0.2263(5) 0.0498(19) Uani 1 1 d . . . C(324) C 0.5795(6) 0.4087(5) 0.1557(5) 0.053(2) Uani 1 1 d . . . C(325) C 0.5013(7) 0.4286(5) 0.1045(4) 0.055(2) Uani 1 1 d . . . C(326) C 0.3798(6) 0.4613(4) 0.1241(4) 0.0393(17) Uani 1 1 d . . . C(331) C 0.2260(5) 0.6621(4) 0.1376(3) 0.0319(15) Uani 1 1 d . . . C(332) C 0.2016(6) 0.6817(4) 0.0679(3) 0.0406(17) Uani 1 1 d . . . C(333) C 0.2682(7) 0.7487(5) 0.0258(4) 0.0499(19) Uani 1 1 d . . . C(334) C 0.3585(7) 0.7969(5) 0.0522(4) 0.054(2) Uani 1 1 d . . . C(335) C 0.3806(6) 0.7807(5) 0.1222(4) 0.052(2) Uani 1 1 d . . . C(336) C 0.3150(6) 0.7124(5) 0.1641(4) 0.0462(18) Uani 1 1 d . . . C(351) C -0.1826(5) 0.5837(4) 0.2547(3) 0.0287(15) Uani 1 1 d . . . C(352) C -0.2476(5) 0.6163(4) 0.1981(3) 0.0294(15) Uani 1 1 d . . . C(353) C -0.3696(5) 0.6475(4) 0.2083(3) 0.0339(15) Uani 1 1 d . . . C(354) C -0.4295(6) 0.6479(4) 0.2759(4) 0.0391(17) Uani 1 1 d . . . C(355) C -0.3668(6) 0.6176(4) 0.3337(3) 0.0347(16) Uani 1 1 d . . . C(356) C -0.2448(5) 0.5854(4) 0.3236(3) 0.0306(15) Uani 1 1 d . . . C(361) C -0.0756(5) 0.3962(4) 0.3148(3) 0.0265(14) Uani 1 1 d . . . C(362) C -0.0789(6) 0.3838(5) 0.3876(3) 0.0383(16) Uani 1 1 d . . . C(363) C -0.1542(6) 0.3187(5) 0.4254(4) 0.0450(18) Uani 1 1 d . . . C(364) C -0.2296(6) 0.2656(5) 0.3902(4) 0.049(2) Uani 1 1 d . . . C(365) C -0.2252(6) 0.2744(5) 0.3182(4) 0.0456(18) Uani 1 1 d . . . C(366) C -0.1476(6) 0.3400(4) 0.2800(3) 0.0371(16) Uani 1 1 d . . . C(911) C 1.1201(7) 0.4667(5) -0.0161(4) 0.054(2) Uani 1 1 d . . . C(912) C 1.0526(8) 0.4356(5) 0.0454(4) 0.052(2) Uani 1 1 d . . . C(913) C 0.9340(7) 0.4682(5) 0.0610(4) 0.0511(19) Uani 1 1 d . . . H(24) H 0.2810 -0.0876 0.5112 0.040 Uiso 1 1 calc R . . H(34) H -0.0073 0.6720 0.1791 0.033 Uiso 1 1 calc R . . H(122) H 0.5593 0.2065 0.2085 0.044 Uiso 1 1 calc R . . H(123) H 0.7447 0.1378 0.1602 0.043 Uiso 1 1 calc R . . H(124) H 0.7495 0.0104 0.0824 0.044 Uiso 1 1 calc R . . H(125) H 0.5676 -0.0482 0.0544 0.044 Uiso 1 1 calc R . . H(126) H 0.3790 0.0226 0.1005 0.039 Uiso 1 1 calc R . . H(132) H 0.3636 0.2328 0.0394 0.049 Uiso 1 1 calc R . . H(133) H 0.3150 0.2314 -0.0761 0.062 Uiso 1 1 calc R . . H(134) H 0.1242 0.1878 -0.1000 0.066 Uiso 1 1 calc R . . H(135) H -0.0195 0.1391 -0.0078 0.064 Uiso 1 1 calc R . . H(136) H 0.0255 0.1402 0.1093 0.056 Uiso 1 1 calc R . . H(222) H 0.4599 0.2104 0.4457 0.048 Uiso 1 1 calc R . . H(223) H 0.5191 0.3686 0.4494 0.056 Uiso 1 1 calc R . . H(224) H 0.3736 0.4954 0.4747 0.059 Uiso 1 1 calc R . . H(225) H 0.1667 0.4639 0.4959 0.051 Uiso 1 1 calc R . . H(226) H 0.1055 0.3075 0.4885 0.044 Uiso 1 1 calc R . . H(232) H 0.2239 0.1836 0.6073 0.044 Uiso 1 1 calc R . . H(233) H 0.2908 0.1832 0.7186 0.050 Uiso 1 1 calc R . . H(234) H 0.4486 0.0726 0.7481 0.053 Uiso 1 1 calc R . . H(235) H 0.5324 -0.0411 0.6656 0.052 Uiso 1 1 calc R . . H(236) H 0.4607 -0.0428 0.5553 0.043 Uiso 1 1 calc R . . H(252) H 0.3682 -0.2007 0.4090 0.041 Uiso 1 1 calc R . . H(253) H 0.3490 -0.3629 0.3844 0.049 Uiso 1 1 calc R . . H(254) H 0.1593 -0.4163 0.3655 0.056 Uiso 1 1 calc R . . H(255) H -0.0109 -0.3059 0.3689 0.049 Uiso 1 1 calc R . . H(256) H 0.0059 -0.1457 0.3974 0.044 Uiso 1 1 calc R . . H(262) H 0.2402 -0.0506 0.2579 0.050 Uiso 1 1 calc R . . H(263) H 0.1352 -0.0867 0.1628 0.062 Uiso 1 1 calc R . . H(264) H -0.0735 -0.0400 0.1652 0.070 Uiso 1 1 calc R . . H(265) H -0.1760 0.0392 0.2624 0.062 Uiso 1 1 calc R . . H(266) H -0.0729 0.0744 0.3565 0.052 Uiso 1 1 calc R . . H(322) H 0.3889 0.4584 0.2958 0.047 Uiso 1 1 calc R . . H(323) H 0.5922 0.4060 0.2614 0.060 Uiso 1 1 calc R . . H(324) H 0.6623 0.3871 0.1422 0.064 Uiso 1 1 calc R . . H(325) H 0.5301 0.4202 0.0559 0.067 Uiso 1 1 calc R . . H(326) H 0.3266 0.4756 0.0885 0.047 Uiso 1 1 calc R . . H(332) H 0.1392 0.6492 0.0493 0.049 Uiso 1 1 calc R . . H(333) H 0.2516 0.7617 -0.0218 0.060 Uiso 1 1 calc R . . H(334) H 0.4055 0.8413 0.0223 0.065 Uiso 1 1 calc R . . H(335) H 0.4400 0.8159 0.1413 0.063 Uiso 1 1 calc R . . H(336) H 0.3313 0.6999 0.2118 0.055 Uiso 1 1 calc R . . H(352) H -0.2063 0.6170 0.1513 0.035 Uiso 1 1 calc R . . H(353) H -0.4119 0.6685 0.1690 0.041 Uiso 1 1 calc R . . H(354) H -0.5138 0.6688 0.2834 0.047 Uiso 1 1 calc R . . H(355) H -0.4085 0.6191 0.3805 0.042 Uiso 1 1 calc R . . H(356) H -0.2031 0.5644 0.3632 0.037 Uiso 1 1 calc R . . H(362) H -0.0281 0.4207 0.4121 0.046 Uiso 1 1 calc R . . H(363) H -0.1544 0.3105 0.4753 0.054 Uiso 1 1 calc R . . H(364) H -0.2845 0.2230 0.4163 0.059 Uiso 1 1 calc R . . H(365) H -0.2746 0.2361 0.2939 0.055 Uiso 1 1 calc R . . H(366) H -0.1446 0.3457 0.2298 0.045 Uiso 1 1 calc R . . H(911) H 1.2029 0.4434 -0.0273 0.065 Uiso 1 1 calc R . . H(912) H 1.0894 0.3909 0.0773 0.062 Uiso 1 1 calc R . . H(913) H 0.8881 0.4456 0.1034 0.061 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 0.0296(4) 0.0281(4) 0.0310(4) 0.0018(3) -0.0049(3) 0.0019(3) O(2) 0.032(2) 0.029(2) 0.032(2) 0.0028(19) -0.0064(19) 0.0067(19) O(3) 0.031(2) 0.022(2) 0.039(3) -0.0013(18) -0.0076(19) 0.0053(19) O(11) 0.027(2) 0.042(3) 0.031(3) 0.009(2) -0.0065(19) -0.004(2) O(14) 0.039(3) 0.036(2) 0.027(2) 0.004(2) -0.008(2) -0.0075(19) C(12) 0.028(4) 0.026(3) 0.031(4) 0.002(3) -0.001(3) -0.002(3) C(13) 0.028(4) 0.035(4) 0.031(4) 0.004(3) 0.000(3) 0.000(3) C(21) 0.032(4) 0.029(4) 0.027(4) -0.002(3) -0.006(3) 0.007(3) C(22) 0.028(3) 0.024(4) 0.035(4) -0.002(3) 0.003(3) -0.001(3) C(23) 0.031(4) 0.025(4) 0.028(4) -0.001(3) -0.005(3) 0.002(3) C(24) 0.034(4) 0.026(4) 0.039(4) 0.002(3) -0.003(3) 0.004(3) C(25) 0.031(4) 0.025(3) 0.033(4) -0.005(3) -0.006(3) 0.004(3) C(26) 0.028(3) 0.026(4) 0.029(4) -0.002(3) -0.004(3) 0.000(3) C(31) 0.032(4) 0.018(3) 0.029(3) 0.004(3) -0.011(3) 0.003(3) C(32) 0.025(3) 0.024(3) 0.034(4) -0.006(3) -0.007(3) -0.003(3) C(33) 0.030(4) 0.025(3) 0.030(4) -0.003(3) -0.007(3) 0.001(3) C(34) 0.030(4) 0.022(3) 0.033(4) 0.003(3) -0.014(3) 0.004(3) C(35) 0.024(3) 0.027(3) 0.024(3) -0.002(3) -0.006(3) 0.002(3) C(36) 0.023(3) 0.023(3) 0.027(3) -0.003(3) -0.008(3) -0.001(3) C(121) 0.033(4) 0.032(4) 0.026(4) 0.004(3) -0.005(3) 0.005(3) C(122) 0.045(4) 0.028(4) 0.038(4) 0.000(3) -0.013(3) 0.000(3) C(123) 0.025(4) 0.040(4) 0.044(4) 0.001(3) -0.006(3) 0.007(3) C(124) 0.034(4) 0.038(4) 0.033(4) 0.010(3) 0.004(3) 0.011(3) C(125) 0.047(4) 0.028(4) 0.035(4) 0.004(3) -0.003(3) -0.002(3) C(126) 0.036(4) 0.031(4) 0.030(4) 0.004(3) -0.002(3) 0.001(3) C(131) 0.037(4) 0.034(4) 0.035(4) 0.008(3) -0.015(3) -0.004(3) C(132) 0.047(4) 0.038(4) 0.035(4) 0.008(3) 0.000(3) 0.005(3) C(133) 0.078(6) 0.037(4) 0.035(5) 0.020(4) 0.000(4) 0.002(3) C(134) 0.094(7) 0.043(5) 0.031(4) 0.023(4) -0.028(5) -0.005(3) C(135) 0.062(5) 0.049(5) 0.057(5) -0.003(4) -0.034(4) -0.001(4) C(136) 0.064(5) 0.045(4) 0.031(4) 0.000(4) -0.008(4) 0.001(3) C(221) 0.039(4) 0.030(4) 0.027(4) -0.003(3) -0.007(3) 0.000(3) C(222) 0.038(4) 0.029(4) 0.053(5) 0.000(3) -0.006(3) -0.001(3) C(223) 0.043(4) 0.033(4) 0.067(5) -0.016(4) -0.009(4) 0.000(3) C(224) 0.077(6) 0.025(4) 0.049(5) -0.006(4) -0.022(4) -0.001(3) C(225) 0.056(5) 0.032(4) 0.039(4) 0.009(4) -0.012(3) -0.004(3) C(226) 0.038(4) 0.034(4) 0.037(4) -0.001(3) -0.002(3) 0.003(3) C(231) 0.031(4) 0.026(3) 0.031(4) -0.004(3) -0.006(3) -0.003(3) C(232) 0.040(4) 0.031(4) 0.040(4) -0.005(3) -0.011(3) 0.006(3) C(233) 0.052(5) 0.034(4) 0.041(4) -0.016(3) -0.003(4) -0.003(3) C(234) 0.054(5) 0.049(5) 0.036(4) -0.018(4) -0.022(4) 0.004(4) C(235) 0.039(4) 0.042(4) 0.052(5) -0.006(3) -0.017(4) 0.007(4) C(236) 0.037(4) 0.036(4) 0.033(4) 0.001(3) -0.006(3) 0.001(3) C(251) 0.042(4) 0.020(3) 0.029(4) -0.006(3) -0.003(3) 0.003(3) C(252) 0.036(4) 0.033(4) 0.032(4) -0.001(3) -0.002(3) 0.008(3) C(253) 0.052(5) 0.031(4) 0.037(4) 0.000(3) 0.007(3) 0.000(3) C(254) 0.078(6) 0.026(4) 0.033(4) -0.012(4) 0.009(4) -0.004(3) C(255) 0.053(5) 0.039(4) 0.034(4) -0.013(4) -0.012(3) -0.002(3) C(256) 0.042(4) 0.029(4) 0.038(4) -0.006(3) -0.003(3) 0.006(3) C(261) 0.039(4) 0.022(3) 0.039(4) -0.006(3) -0.011(3) 0.004(3) C(262) 0.043(4) 0.038(4) 0.045(4) 0.000(3) -0.016(4) 0.003(3) C(263) 0.077(6) 0.043(4) 0.038(4) -0.009(4) -0.020(4) -0.001(3) C(264) 0.078(6) 0.049(5) 0.058(6) -0.020(4) -0.043(5) 0.007(4) C(265) 0.051(5) 0.045(5) 0.063(5) -0.011(4) -0.025(4) 0.013(4) C(266) 0.051(5) 0.032(4) 0.047(4) 0.005(3) -0.014(4) 0.009(3) C(321) 0.025(4) 0.024(3) 0.043(4) -0.003(3) 0.001(3) 0.001(3) C(322) 0.028(4) 0.031(4) 0.060(5) -0.005(3) -0.008(3) -0.001(3) C(323) 0.031(4) 0.036(4) 0.083(6) -0.001(3) -0.014(4) 0.011(4) C(324) 0.022(4) 0.036(4) 0.101(7) -0.001(3) -0.004(4) 0.004(4) C(325) 0.045(5) 0.045(5) 0.070(6) -0.005(4) 0.018(4) 0.002(4) C(326) 0.029(4) 0.037(4) 0.050(5) 0.001(3) 0.001(3) 0.009(3) C(331) 0.023(3) 0.032(4) 0.039(4) 0.001(3) -0.003(3) 0.007(3) C(332) 0.044(4) 0.039(4) 0.039(4) -0.016(3) 0.000(3) 0.007(3) C(333) 0.060(5) 0.039(4) 0.049(5) 0.001(4) -0.002(4) 0.010(4) C(334) 0.043(5) 0.045(5) 0.068(6) 0.001(4) 0.012(4) 0.026(4) C(335) 0.032(4) 0.035(4) 0.093(6) -0.014(3) -0.023(4) 0.022(4) C(336) 0.039(4) 0.045(4) 0.058(5) -0.012(4) -0.024(4) 0.019(4) C(351) 0.026(3) 0.024(3) 0.037(4) -0.004(3) -0.006(3) -0.001(3) C(352) 0.029(4) 0.029(4) 0.029(4) -0.002(3) -0.001(3) 0.000(3) C(353) 0.032(4) 0.038(4) 0.032(4) 0.002(3) -0.008(3) 0.004(3) C(354) 0.029(4) 0.038(4) 0.050(5) 0.006(3) -0.007(3) -0.002(3) C(355) 0.037(4) 0.031(4) 0.033(4) -0.001(3) 0.007(3) -0.002(3) C(356) 0.027(4) 0.028(4) 0.036(4) 0.002(3) -0.003(3) 0.001(3) C(361) 0.024(3) 0.023(3) 0.033(4) -0.003(3) -0.002(3) 0.002(3) C(362) 0.040(4) 0.038(4) 0.035(4) -0.006(3) 0.002(3) 0.004(3) C(363) 0.045(4) 0.047(4) 0.038(4) 0.007(4) 0.003(4) 0.013(3) C(364) 0.036(4) 0.048(5) 0.061(5) -0.005(4) 0.001(4) 0.029(4) C(365) 0.036(4) 0.039(4) 0.065(5) -0.014(3) -0.019(4) 0.015(4) C(366) 0.039(4) 0.036(4) 0.036(4) -0.003(3) -0.006(3) 0.007(3) C(911) 0.053(5) 0.049(5) 0.062(6) 0.003(4) -0.009(4) -0.024(4) C(912) 0.072(6) 0.036(4) 0.051(5) 0.015(4) -0.031(4) -0.008(4) C(913) 0.066(6) 0.043(5) 0.045(5) 0.000(4) -0.009(4) -0.002(4) # 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(2) 1.720(4) YES Ge O(3) 1.733(4) YES Ge O(14) 1.770(4) YES Ge O(11) 1.772(4) YES O(2) C(21) 1.402(6) YES O(3) C(31) 1.407(6) YES O(11) C(12) 1.411(7) YES O(14) C(13) 1.404(7) YES C(12) C(13) 1.330(8) YES C(12) C(121) 1.470(8) YES C(13) C(131) 1.468(8) YES C(21) C(26) 1.389(8) YES C(21) C(22) 1.402(8) YES C(22) C(23) 1.419(8) YES C(22) C(221) 1.504(8) YES C(23) C(24) 1.407(8) YES C(23) C(231) 1.487(8) YES C(24) C(25) 1.386(8) YES C(25) C(26) 1.412(8) YES C(25) C(251) 1.484(8) YES C(26) C(261) 1.474(8) YES C(31) C(36) 1.398(7) YES C(31) C(32) 1.404(8) YES C(32) C(33) 1.406(8) YES C(32) C(321) 1.482(8) YES C(33) C(34) 1.390(8) YES C(33) C(331) 1.500(8) YES C(34) C(35) 1.389(7) YES C(35) C(36) 1.390(7) YES C(35) C(351) 1.494(8) YES C(36) C(361) 1.495(7) YES C(121) C(122) 1.408(8) YES C(121) C(126) 1.409(8) YES C(122) C(123) 1.362(8) YES C(123) C(124) 1.382(8) YES C(124) C(125) 1.384(8) YES C(125) C(126) 1.382(8) YES C(131) C(132) 1.385(8) YES C(131) C(136) 1.416(9) YES C(132) C(133) 1.377(9) YES C(133) C(134) 1.375(10) YES C(134) C(135) 1.372(10) YES C(135) C(136) 1.384(9) YES C(221) C(226) 1.381(8) YES C(221) C(222) 1.408(8) YES C(222) C(223) 1.374(8) YES C(223) C(224) 1.374(9) YES C(224) C(225) 1.376(9) YES C(225) C(226) 1.370(8) YES C(231) C(232) 1.379(8) YES C(231) C(236) 1.386(8) YES C(232) C(233) 1.376(8) YES C(233) C(234) 1.384(9) YES C(234) C(235) 1.377(9) YES C(235) C(236) 1.381(8) YES C(251) C(256) 1.382(8) YES C(251) C(252) 1.400(8) YES C(252) C(253) 1.384(8) YES C(253) C(254) 1.372(9) YES C(254) C(255) 1.384(9) YES C(255) C(256) 1.376(8) YES C(261) C(266) 1.392(8) YES C(261) C(262) 1.402(8) YES C(262) C(263) 1.389(9) YES C(263) C(264) 1.387(10) YES C(264) C(265) 1.377(10) YES C(265) C(266) 1.368(9) YES C(321) C(326) 1.389(8) YES C(321) C(322) 1.412(8) YES C(322) C(323) 1.388(9) YES C(323) C(324) 1.376(10) YES C(324) C(325) 1.378(10) YES C(325) C(326) 1.397(9) YES C(331) C(336) 1.384(8) YES C(331) C(332) 1.390(8) YES C(332) C(333) 1.382(8) YES C(333) C(334) 1.378(10) YES C(334) C(335) 1.384(10) YES C(335) C(336) 1.387(9) YES C(351) C(352) 1.401(8) YES C(351) C(356) 1.403(8) YES C(352) C(353) 1.378(8) YES C(353) C(354) 1.370(8) YES C(354) C(355) 1.398(8) YES C(355) C(356) 1.381(8) YES C(361) C(362) 1.380(8) YES C(361) C(366) 1.379(8) YES C(362) C(363) 1.379(8) YES C(363) C(364) 1.382(9) YES C(364) C(365) 1.361(9) YES C(365) C(366) 1.401(8) YES C(911) C(913) 1.366(10) YES C(911) C(912) 1.376(10) YES C(912) C(913) 1.356(10) YES C(913) C(911) 1.366(10) 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) Ge O(3) 103.41(18) YES O(2) Ge O(14) 121.60(18) YES O(3) Ge O(14) 111.27(18) YES O(2) Ge O(11) 110.82(18) YES O(3) Ge O(11) 115.54(18) YES O(14) Ge O(11) 94.83(18) YES C(21) O(2) Ge 125.3(3) YES C(31) O(3) Ge 126.8(3) YES C(12) O(11) Ge 105.4(3) YES C(13) O(14) Ge 105.3(3) YES C(13) C(12) O(11) 116.7(5) YES C(13) C(12) C(121) 131.3(6) YES O(11) C(12) C(121) 111.9(5) YES C(12) C(13) O(14) 117.2(5) YES C(12) C(13) C(131) 129.5(6) YES O(14) C(13) C(131) 113.1(5) YES C(26) C(21) C(22) 123.9(5) YES C(26) C(21) O(2) 119.7(5) YES C(22) C(21) O(2) 116.5(5) YES C(21) C(22) C(23) 118.2(5) YES C(21) C(22) C(221) 119.2(5) YES C(23) C(22) C(221) 122.3(5) YES C(24) C(23) C(22) 116.9(5) YES C(24) C(23) C(231) 118.1(5) YES C(22) C(23) C(231) 124.8(5) YES C(25) C(24) C(23) 124.4(6) YES C(24) C(25) C(26) 118.2(5) YES C(24) C(25) C(251) 118.8(5) YES C(26) C(25) C(251) 123.0(5) YES C(21) C(26) C(25) 118.1(5) YES C(21) C(26) C(261) 120.2(5) YES C(25) C(26) C(261) 121.7(5) YES C(36) C(31) C(32) 123.3(5) YES C(36) C(31) O(3) 118.0(5) YES C(32) C(31) O(3) 118.4(5) YES C(31) C(32) C(33) 116.6(5) YES C(31) C(32) C(321) 120.5(5) YES C(33) C(32) C(321) 122.8(5) YES C(34) C(33) C(32) 120.1(5) YES C(34) C(33) C(331) 117.6(5) YES C(32) C(33) C(331) 122.2(5) YES C(33) C(34) C(35) 122.2(5) YES C(34) C(35) C(36) 119.1(5) YES C(34) C(35) C(351) 118.1(5) YES C(36) C(35) C(351) 122.8(5) YES C(35) C(36) C(31) 118.5(5) YES C(35) C(36) C(361) 122.5(5) YES C(31) C(36) C(361) 118.9(5) YES C(122) C(121) C(126) 117.6(6) YES C(122) C(121) C(12) 120.9(6) YES C(126) C(121) C(12) 121.5(6) YES C(123) C(122) C(121) 122.1(6) YES C(122) C(123) C(124) 119.5(6) YES C(123) C(124) C(125) 120.3(6) YES C(126) C(125) C(124) 120.7(6) YES C(125) C(126) C(121) 119.9(6) YES C(132) C(131) C(136) 118.2(6) YES C(132) C(131) C(13) 121.6(6) YES C(136) C(131) C(13) 120.1(6) YES C(133) C(132) C(131) 120.1(7) YES C(134) C(133) C(132) 121.3(7) YES C(135) C(134) C(133) 120.0(7) YES C(134) C(135) C(136) 119.8(7) YES C(135) C(136) C(131) 120.5(7) YES C(226) C(221) C(222) 117.8(6) YES C(226) C(221) C(22) 123.1(5) YES C(222) C(221) C(22) 118.9(5) YES C(223) C(222) C(221) 120.3(6) YES C(222) C(223) C(224) 120.5(6) YES C(223) C(224) C(225) 119.8(6) YES C(226) C(225) C(224) 120.0(6) YES C(225) C(226) C(221) 121.6(6) YES C(232) C(231) C(236) 117.7(6) YES C(232) C(231) C(23) 121.6(5) YES C(236) C(231) C(23) 120.5(5) YES C(233) C(232) C(231) 121.4(6) YES C(232) C(233) C(234) 120.4(6) YES C(235) C(234) C(233) 118.9(6) YES C(234) C(235) C(236) 120.1(6) YES C(235) C(236) C(231) 121.5(6) YES C(256) C(251) C(252) 118.0(6) YES C(256) C(251) C(25) 121.8(6) YES C(252) C(251) C(25) 120.2(5) YES C(253) C(252) C(251) 120.8(6) YES C(254) C(253) C(252) 120.1(6) YES C(253) C(254) C(255) 119.6(6) YES C(256) C(255) C(254) 120.4(6) YES C(255) C(256) C(251) 121.1(6) YES C(266) C(261) C(262) 117.8(6) YES C(266) C(261) C(26) 120.9(6) YES C(262) C(261) C(26) 121.3(6) YES C(263) C(262) C(261) 121.0(6) YES C(264) C(263) C(262) 119.2(7) YES C(265) C(264) C(263) 120.3(7) YES C(266) C(265) C(264) 120.3(7) YES C(265) C(266) C(261) 121.4(7) YES C(326) C(321) C(322) 118.4(6) YES C(326) C(321) C(32) 119.4(5) YES C(322) C(321) C(32) 122.2(6) YES C(323) C(322) C(321) 120.1(7) YES C(324) C(323) C(322) 120.6(7) YES C(323) C(324) C(325) 120.1(7) YES C(324) C(325) C(326) 120.1(7) YES C(321) C(326) C(325) 120.7(6) YES C(336) C(331) C(332) 119.0(6) YES C(336) C(331) C(33) 121.2(6) YES C(332) C(331) C(33) 119.7(5) YES C(333) C(332) C(331) 119.8(6) YES C(334) C(333) C(332) 120.8(7) YES C(333) C(334) C(335) 120.0(6) YES C(334) C(335) C(336) 119.2(7) YES C(331) C(336) C(335) 121.2(6) YES C(352) C(351) C(356) 118.0(5) YES C(352) C(351) C(35) 120.9(5) YES C(356) C(351) C(35) 121.0(5) YES C(353) C(352) C(351) 122.0(5) YES C(354) C(353) C(352) 119.3(6) YES C(353) C(354) C(355) 120.2(6) YES C(356) C(355) C(354) 120.6(6) YES C(355) C(356) C(351) 119.8(6) YES C(362) C(361) C(366) 118.3(5) YES C(362) C(361) C(36) 122.2(5) YES C(366) C(361) C(36) 119.5(5) YES C(363) C(362) C(361) 121.4(6) YES C(362) C(363) C(364) 119.8(6) YES C(365) C(364) C(363) 119.9(6) YES C(364) C(365) C(366) 120.0(6) YES C(361) C(366) C(365) 120.5(6) YES C(913) C(911) C(912) 118.9(7) YES C(913) C(912) C(911) 120.5(7) YES C(912) C(913) C(911) 120.5(7) YES #===END