# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Atsushi Kawachi' _publ_contact_author_email KAWACHI@SCI.HIROSHIMA-U.AC.JP _publ_section_title ; Synthesis, structure and reactions of triarylgermyl anion with alpha,delta-ambiphilic character ; loop_ _publ_author_name 'Atsushi Kawachi' 'Koji Machida' 'Yohsuke Yamamoto' # Attachment 'Revised_CIF_Compound3.cif' data_(Triarylgermyl)potassium_3 _database_code_depnum_ccdc_archive 'CCDC 733620' #TrackingRef 'Revised_CIF_Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Potassium [2.2.2]cryptand tris[2-(fluorodimethylsilyl)phenyl]germanide ; _chemical_name_common ;Potassium (2.2.2)cryptand tris(2- (fluorodimethylsilyl)phenyl)germanide ; _chemical_melting_point 335 _chemical_formula_moiety 'C18 H36 K N2 O6, C24 H30 F3 Ge Si3' _chemical_formula_sum 'C42 H66 F3 Ge K N2 O6 Si3' _chemical_formula_weight 947.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5904(9) _cell_length_b 13.6336(10) _cell_length_c 16.5928(12) _cell_angle_alpha 77.929(2) _cell_angle_beta 83.078(2) _cell_angle_gamma 71.543(2) _cell_volume 2427.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11047 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Scx-mini _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 6.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24640 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11047 _reflns_number_gt 8800 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction Yadokari _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep-3 _computing_publication_material Yadokari _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+1.4991P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11047 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.06350(2) 0.298340(19) 0.777471(15) 0.02737(7) Uani 1 1 d . . . Si1 Si 0.08692(7) 0.14976(6) 0.63053(4) 0.03435(16) Uani 1 1 d . . . Si2 Si 0.33702(6) 0.29154(6) 0.84048(4) 0.03572(17) Uani 1 1 d . . . Si3 Si -0.04861(7) 0.55553(5) 0.67343(4) 0.03437(16) Uani 1 1 d . . . F1 F 0.05992(17) 0.08166(14) 0.56982(10) 0.0566(5) Uani 1 1 d . . . F2 F 0.45471(15) 0.26898(17) 0.89297(11) 0.0632(5) Uani 1 1 d . . . F3 F -0.11440(16) 0.68139(12) 0.65178(10) 0.0518(4) Uani 1 1 d . . . C1 C -0.0663(2) 0.23300(18) 0.76547(15) 0.0283(5) Uani 1 1 d . . . C2 C -0.0510(2) 0.17352(18) 0.70284(15) 0.0303(5) Uani 1 1 d . . . C3 C -0.1411(2) 0.1273(2) 0.69626(19) 0.0429(6) Uani 1 1 d . . . H3A H -0.1307 0.0863 0.6546 0.051 Uiso 1 1 calc R . . C4 C -0.2438(3) 0.1398(2) 0.7484(2) 0.0505(8) Uani 1 1 d . . . H4A H -0.3035 0.1080 0.7424 0.061 Uiso 1 1 calc R . . C5 C -0.2605(2) 0.1984(2) 0.80927(19) 0.0460(7) Uani 1 1 d . . . H5A H -0.3316 0.2073 0.8455 0.055 Uiso 1 1 calc R . . C6 C -0.1726(2) 0.2445(2) 0.81720(16) 0.0357(6) Uani 1 1 d . . . H6A H -0.1850 0.2853 0.8592 0.043 Uiso 1 1 calc R . . C7 C 0.1120(3) 0.2656(2) 0.55932(17) 0.0521(8) Uani 1 1 d . . . H7A H 0.1589 0.2437 0.5095 0.078 Uiso 1 1 calc R . . H7B H 0.1571 0.2981 0.5865 0.078 Uiso 1 1 calc R . . H7C H 0.0332 0.3165 0.5441 0.078 Uiso 1 1 calc R . . C8 C 0.2245(2) 0.0631(2) 0.68276(17) 0.0417(6) Uani 1 1 d . . . H8A H 0.2083 -0.0013 0.7135 0.063 Uiso 1 1 calc R . . H8B H 0.2462 0.0994 0.7210 0.063 Uiso 1 1 calc R . . H8C H 0.2920 0.0451 0.6415 0.063 Uiso 1 1 calc R . . C9 C 0.1395(2) 0.19961(19) 0.87922(14) 0.0300(5) Uani 1 1 d . . . C10 C 0.2516(2) 0.2029(2) 0.90213(15) 0.0338(5) Uani 1 1 d . . . C11 C 0.3034(3) 0.1361(2) 0.97344(17) 0.0466(7) Uani 1 1 d . . . H11A H 0.3789 0.1384 0.9885 0.056 Uiso 1 1 calc R . . C12 C 0.2478(3) 0.0672(2) 1.02222(17) 0.0491(7) Uani 1 1 d . . . H12A H 0.2837 0.0236 1.0709 0.059 Uiso 1 1 calc R . . C13 C 0.1394(3) 0.0621(2) 0.99982(16) 0.0431(6) Uani 1 1 d . . . H13A H 0.1006 0.0143 1.0327 0.052 Uiso 1 1 calc R . . C14 C 0.0871(2) 0.1270(2) 0.92920(16) 0.0365(6) Uani 1 1 d . . . H14A H 0.0129 0.1218 0.9142 0.044 Uiso 1 1 calc R . . C15 C 0.4011(3) 0.2578(2) 0.73849(18) 0.0447(7) Uani 1 1 d . . . H15A H 0.4601 0.2960 0.7159 0.067 Uiso 1 1 calc R . . H15B H 0.3353 0.2776 0.7008 0.067 Uiso 1 1 calc R . . H15C H 0.4420 0.1820 0.7448 0.067 Uiso 1 1 calc R . . C16 C 0.2599(3) 0.4339(2) 0.83542(19) 0.0476(7) Uani 1 1 d . . . H16A H 0.1757 0.4507 0.8205 0.071 Uiso 1 1 calc R . . H16B H 0.3031 0.4740 0.7937 0.071 Uiso 1 1 calc R . . H16C H 0.2602 0.4524 0.8894 0.071 Uiso 1 1 calc R . . C17 C -0.0377(2) 0.41954(19) 0.83312(14) 0.0302(5) Uani 1 1 d . . . C18 C -0.0733(2) 0.52341(19) 0.78772(15) 0.0316(5) Uani 1 1 d . . . C19 C -0.1316(3) 0.6069(2) 0.82960(18) 0.0437(6) Uani 1 1 d . . . H19A H -0.1557 0.6766 0.7991 0.052 Uiso 1 1 calc R . . C20 C -0.1547(3) 0.5902(3) 0.91388(19) 0.0540(8) Uani 1 1 d . . . H20A H -0.1934 0.6478 0.9413 0.065 Uiso 1 1 calc R . . C21 C -0.1213(3) 0.4894(2) 0.95782(18) 0.0519(8) Uani 1 1 d . . . H21A H -0.1377 0.4770 1.0159 0.062 Uiso 1 1 calc R . . C22 C -0.0640(3) 0.4061(2) 0.91792(16) 0.0416(6) Uani 1 1 d . . . H22A H -0.0417 0.3370 0.9496 0.050 Uiso 1 1 calc R . . C23 C 0.1101(3) 0.5397(2) 0.63067(17) 0.0432(6) Uani 1 1 d . . . H23A H 0.1099 0.5678 0.5713 0.065 Uiso 1 1 calc R . . H23B H 0.1567 0.4650 0.6400 0.065 Uiso 1 1 calc R . . H23C H 0.1476 0.5781 0.6581 0.065 Uiso 1 1 calc R . . C24 C -0.1330(3) 0.4980(2) 0.61821(16) 0.0406(6) Uani 1 1 d . . . H24A H -0.2208 0.5294 0.6286 0.061 Uiso 1 1 calc R . . H24B H -0.1111 0.4218 0.6380 0.061 Uiso 1 1 calc R . . H24C H -0.1119 0.5122 0.5588 0.061 Uiso 1 1 calc R . . K1 K 0.39531(5) 0.75727(4) 0.71676(3) 0.03520(13) Uani 1 1 d . . . N1 N 0.4410(3) 0.7436(2) 0.53483(16) 0.0571(7) Uani 1 1 d . . . N2 N 0.3537(3) 0.7711(2) 0.89698(16) 0.0606(8) Uani 1 1 d . . . O1 O 0.19997(19) 0.77844(17) 0.62431(16) 0.0603(6) Uani 1 1 d . . . O2 O 0.15514(18) 0.81281(16) 0.78758(15) 0.0555(6) Uani 1 1 d . . . O3 O 0.55209(17) 0.57146(13) 0.66304(12) 0.0422(4) Uani 1 1 d . . . O4 O 0.4910(2) 0.57684(16) 0.83132(14) 0.0583(6) Uani 1 1 d . . . O5 O 0.52558(18) 0.88693(15) 0.61166(13) 0.0498(5) Uani 1 1 d . . . O6 O 0.5055(2) 0.87383(16) 0.78476(13) 0.0520(5) Uani 1 1 d . . . C25 C 0.3269(4) 0.7438(4) 0.5035(3) 0.0867(14) Uani 1 1 d . . . H25A H 0.3206 0.6714 0.5167 0.104 Uiso 1 1 calc R . . H25B H 0.3309 0.7649 0.4427 0.104 Uiso 1 1 calc R . . C26 C 0.2140(4) 0.8161(4) 0.5385(3) 0.0896(15) Uani 1 1 d . . . H26A H 0.2211 0.8882 0.5291 0.108 Uiso 1 1 calc R . . H26B H 0.1420 0.8185 0.5107 0.108 Uiso 1 1 calc R . . C27 C 0.0811(3) 0.8269(3) 0.6578(3) 0.0711(12) Uani 1 1 d . . . H27A H 0.0192 0.8128 0.6295 0.085 Uiso 1 1 calc R . . H27B H 0.0657 0.9040 0.6489 0.085 Uiso 1 1 calc R . . C28 C 0.0719(3) 0.7850(3) 0.7463(3) 0.0750(12) Uani 1 1 d . . . H28A H -0.0123 0.8141 0.7689 0.090 Uiso 1 1 calc R . . H28B H 0.0914 0.7075 0.7554 0.090 Uiso 1 1 calc R . . C29 C 0.1406(4) 0.7841(3) 0.8745(2) 0.0787(12) Uani 1 1 d . . . H29A H 0.1606 0.7067 0.8904 0.094 Uiso 1 1 calc R . . H29B H 0.0550 0.8158 0.8934 0.094 Uiso 1 1 calc R . . C30 C 0.2227(4) 0.8219(3) 0.9136(2) 0.0703(11) Uani 1 1 d . . . H30A H 0.2049 0.8986 0.8940 0.084 Uiso 1 1 calc R . . H30B H 0.2042 0.8102 0.9741 0.084 Uiso 1 1 calc R . . C31 C 0.5377(3) 0.6475(3) 0.5219(2) 0.0613(9) Uani 1 1 d . . . H31A H 0.6178 0.6587 0.5228 0.074 Uiso 1 1 calc R . . H31B H 0.5319 0.6331 0.4667 0.074 Uiso 1 1 calc R . . C32 C 0.5309(3) 0.5547(3) 0.5855(2) 0.0583(9) Uani 1 1 d . . . H32A H 0.4494 0.5449 0.5875 0.070 Uiso 1 1 calc R . . H32B H 0.5928 0.4906 0.5716 0.070 Uiso 1 1 calc R . . C33 C 0.5683(3) 0.4789(2) 0.7240(2) 0.0591(9) Uani 1 1 d . . . H33A H 0.6368 0.4213 0.7062 0.071 Uiso 1 1 calc R . . H33B H 0.4936 0.4567 0.7318 0.071 Uiso 1 1 calc R . . C34 C 0.5944(3) 0.5009(2) 0.8028(2) 0.0651(10) Uani 1 1 d . . . H34A H 0.6135 0.4354 0.8445 0.078 Uiso 1 1 calc R . . H34B H 0.6658 0.5277 0.7940 0.078 Uiso 1 1 calc R . . C35 C 0.5110(5) 0.5969(3) 0.9088(2) 0.1024(18) Uani 1 1 d . . . H35A H 0.5725 0.6350 0.9012 0.123 Uiso 1 1 calc R . . H35B H 0.5416 0.5297 0.9476 0.123 Uiso 1 1 calc R . . C36 C 0.3918(5) 0.6623(3) 0.9432(2) 0.1026(18) Uani 1 1 d . . . H36A H 0.3279 0.6290 0.9416 0.123 Uiso 1 1 calc R . . H36B H 0.3998 0.6638 1.0016 0.123 Uiso 1 1 calc R . . C37 C 0.4769(4) 0.8368(3) 0.4940(2) 0.0828(14) Uani 1 1 d . . . H37A H 0.4043 0.8996 0.4919 0.099 Uiso 1 1 calc R . . H37B H 0.5067 0.8293 0.4364 0.099 Uiso 1 1 calc R . . C38 C 0.5744(4) 0.8540(3) 0.5366(2) 0.0773(13) Uani 1 1 d . . . H38A H 0.6422 0.7878 0.5472 0.093 Uiso 1 1 calc R . . H38B H 0.6071 0.9080 0.5007 0.093 Uiso 1 1 calc R . . C39 C 0.6174(3) 0.8948(3) 0.6580(3) 0.0666(10) Uani 1 1 d . . . H39A H 0.6645 0.9388 0.6230 0.080 Uiso 1 1 calc R . . H39B H 0.6743 0.8240 0.6762 0.080 Uiso 1 1 calc R . . C40 C 0.5588(3) 0.9428(3) 0.7312(2) 0.0629(10) Uani 1 1 d . . . H40A H 0.6205 0.9569 0.7597 0.075 Uiso 1 1 calc R . . H40B H 0.4959 1.0103 0.7133 0.075 Uiso 1 1 calc R . . C41 C 0.4401(3) 0.9174(3) 0.8545(2) 0.0642(10) Uani 1 1 d . . . H41A H 0.3591 0.9657 0.8388 0.077 Uiso 1 1 calc R . . H41B H 0.4855 0.9575 0.8741 0.077 Uiso 1 1 calc R . . C42 C 0.4261(4) 0.8303(3) 0.9203(2) 0.0777(12) Uani 1 1 d . . . H42A H 0.5078 0.7818 0.9343 0.093 Uiso 1 1 calc R . . H42B H 0.3866 0.8589 0.9703 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02489(13) 0.02973(14) 0.02836(14) -0.00491(10) 0.00063(9) -0.01045(10) Si1 0.0352(4) 0.0349(4) 0.0283(4) -0.0064(3) -0.0036(3) -0.0031(3) Si2 0.0278(4) 0.0513(4) 0.0328(4) -0.0115(3) 0.0017(3) -0.0172(3) Si3 0.0388(4) 0.0299(3) 0.0324(4) -0.0035(3) 0.0018(3) -0.0104(3) F1 0.0654(12) 0.0586(11) 0.0473(10) -0.0249(8) -0.0142(8) -0.0072(9) F2 0.0370(9) 0.1000(15) 0.0576(11) -0.0038(10) -0.0108(8) -0.0314(10) F3 0.0669(11) 0.0317(8) 0.0467(10) -0.0009(7) 0.0022(8) -0.0066(8) C1 0.0231(11) 0.0270(12) 0.0318(12) -0.0002(9) -0.0027(9) -0.0065(9) C2 0.0271(12) 0.0261(12) 0.0355(13) -0.0027(10) -0.0070(10) -0.0049(10) C3 0.0381(15) 0.0396(15) 0.0562(18) -0.0112(13) -0.0125(13) -0.0137(12) C4 0.0339(15) 0.0454(17) 0.078(2) -0.0057(15) -0.0104(14) -0.0210(13) C5 0.0248(13) 0.0447(16) 0.0626(19) 0.0009(14) 0.0054(12) -0.0120(12) C6 0.0283(13) 0.0338(13) 0.0413(15) -0.0018(11) 0.0019(10) -0.0088(11) C7 0.0592(19) 0.0460(17) 0.0342(15) 0.0001(12) 0.0108(13) -0.0018(14) C8 0.0343(14) 0.0416(15) 0.0419(15) -0.0077(12) 0.0005(11) -0.0020(12) C9 0.0282(12) 0.0337(13) 0.0279(12) -0.0091(10) 0.0024(9) -0.0083(10) C10 0.0313(13) 0.0424(14) 0.0282(13) -0.0089(10) 0.0000(10) -0.0108(11) C11 0.0427(16) 0.0621(19) 0.0363(15) -0.0055(13) -0.0125(12) -0.0160(14) C12 0.0585(19) 0.0507(17) 0.0326(15) 0.0042(12) -0.0133(13) -0.0122(15) C13 0.0533(17) 0.0378(15) 0.0344(14) -0.0006(11) 0.0015(12) -0.0140(13) C14 0.0369(14) 0.0336(13) 0.0389(14) -0.0036(11) -0.0017(11) -0.0126(11) C15 0.0369(15) 0.0501(17) 0.0534(17) -0.0229(14) 0.0158(12) -0.0200(13) C16 0.0413(16) 0.0566(18) 0.0567(18) -0.0292(15) 0.0127(13) -0.0247(14) C17 0.0289(12) 0.0342(13) 0.0290(12) -0.0072(10) 0.0007(9) -0.0116(10) C18 0.0323(13) 0.0309(12) 0.0344(13) -0.0093(10) 0.0015(10) -0.0124(10) C19 0.0493(17) 0.0344(14) 0.0476(17) -0.0127(12) 0.0042(13) -0.0121(13) C20 0.067(2) 0.0500(18) 0.0494(18) -0.0271(15) 0.0110(15) -0.0166(16) C21 0.068(2) 0.0552(19) 0.0325(15) -0.0164(13) 0.0096(14) -0.0180(16) C22 0.0501(17) 0.0416(15) 0.0320(14) -0.0088(11) 0.0057(12) -0.0136(13) C23 0.0483(16) 0.0431(15) 0.0405(15) -0.0067(12) 0.0080(12) -0.0212(13) C24 0.0404(15) 0.0443(15) 0.0341(14) -0.0034(11) -0.0041(11) -0.0103(12) K1 0.0339(3) 0.0311(3) 0.0409(3) -0.0087(2) -0.0008(2) -0.0092(2) N1 0.0668(18) 0.0493(15) 0.0428(14) -0.0185(12) -0.0146(13) 0.0106(13) N2 0.079(2) 0.0410(14) 0.0406(14) 0.0023(11) 0.0064(13) 0.0021(14) O1 0.0446(12) 0.0524(13) 0.0849(18) -0.0275(12) -0.0259(12) 0.0016(10) O2 0.0430(12) 0.0470(12) 0.0797(16) -0.0196(11) 0.0164(11) -0.0201(10) O3 0.0418(11) 0.0267(9) 0.0582(12) -0.0103(8) -0.0028(9) -0.0089(8) O4 0.0557(13) 0.0353(11) 0.0677(15) -0.0027(10) 0.0182(11) -0.0034(10) O5 0.0437(11) 0.0430(11) 0.0524(12) -0.0047(9) 0.0145(9) -0.0077(9) O6 0.0623(13) 0.0412(11) 0.0595(13) -0.0084(10) -0.0166(11) -0.0209(10) C25 0.084(3) 0.095(3) 0.070(3) -0.047(2) -0.041(2) 0.023(2) C26 0.075(3) 0.096(3) 0.087(3) -0.043(3) -0.047(2) 0.023(2) C27 0.0347(17) 0.050(2) 0.134(4) -0.033(2) -0.021(2) -0.0053(15) C28 0.0392(18) 0.054(2) 0.138(4) -0.030(2) 0.012(2) -0.0201(16) C29 0.073(3) 0.071(3) 0.083(3) -0.025(2) 0.049(2) -0.022(2) C30 0.089(3) 0.051(2) 0.053(2) -0.0127(16) 0.0221(19) -0.0024(19) C31 0.070(2) 0.056(2) 0.0531(19) -0.0316(16) -0.0083(16) 0.0043(17) C32 0.0540(19) 0.0470(18) 0.080(2) -0.0358(17) -0.0122(17) -0.0053(15) C33 0.0555(19) 0.0277(14) 0.084(3) -0.0054(15) 0.0211(17) -0.0105(14) C34 0.064(2) 0.0385(17) 0.060(2) 0.0108(15) 0.0181(17) 0.0092(15) C35 0.132(4) 0.065(2) 0.048(2) 0.0156(19) 0.010(2) 0.034(3) C36 0.141(4) 0.053(2) 0.057(2) 0.0172(18) 0.033(2) 0.019(2) C37 0.129(4) 0.057(2) 0.0291(17) -0.0056(15) 0.011(2) 0.010(2) C38 0.091(3) 0.048(2) 0.076(3) -0.0142(18) 0.051(2) -0.016(2) C39 0.0332(16) 0.0490(19) 0.108(3) 0.0101(19) 0.0012(18) -0.0169(14) C40 0.055(2) 0.0449(18) 0.098(3) -0.0067(18) -0.0268(19) -0.0232(16) C41 0.080(2) 0.064(2) 0.057(2) -0.0292(17) -0.0279(18) -0.0140(19) C42 0.097(3) 0.076(3) 0.045(2) -0.0107(18) -0.030(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 C1 2.023(2) . ? Ge1 C9 2.024(2) . ? Ge1 C17 2.027(2) . ? Si1 F1 1.6206(17) . ? Si1 C8 1.844(3) . ? Si1 C7 1.844(3) . ? Si1 C2 1.864(3) . ? Si2 F2 1.6194(17) . ? Si2 C16 1.851(3) . ? Si2 C15 1.853(3) . ? Si2 C10 1.866(3) . ? Si3 F3 1.6232(17) . ? Si3 C24 1.848(3) . ? Si3 C23 1.852(3) . ? Si3 C18 1.863(3) . ? C1 C6 1.399(3) . ? C1 C2 1.409(3) . ? C2 C3 1.404(3) . ? C3 C4 1.370(4) . ? C3 H3A 0.9500 . ? C4 C5 1.374(4) . ? C4 H4A 0.9500 . ? C5 C6 1.386(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.398(3) . ? C9 C10 1.413(3) . ? C10 C11 1.402(4) . ? C11 C12 1.376(4) . ? C11 H11A 0.9500 . ? C12 C13 1.378(4) . ? C12 H12A 0.9500 . ? C13 C14 1.386(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.390(3) . ? C17 C18 1.415(3) . ? C18 C19 1.402(4) . ? C19 C20 1.376(4) . ? C19 H19A 0.9500 . ? C20 C21 1.371(4) . ? C20 H20A 0.9500 . ? C21 C22 1.379(4) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? K1 O4 2.778(2) . ? K1 O1 2.793(2) . ? K1 O6 2.795(2) . ? K1 O2 2.820(2) . ? K1 O3 2.8553(19) . ? K1 O5 2.866(2) . ? K1 N2 3.007(3) . ? K1 N1 3.036(3) . ? N1 C31 1.466(4) . ? N1 C37 1.468(5) . ? N1 C25 1.476(5) . ? N2 C42 1.463(5) . ? N2 C36 1.474(4) . ? N2 C30 1.475(5) . ? O1 C26 1.418(5) . ? O1 C27 1.427(4) . ? O2 C29 1.417(4) . ? O2 C28 1.429(4) . ? O3 C32 1.416(4) . ? O3 C33 1.419(3) . ? O4 C34 1.420(4) . ? O4 C35 1.429(5) . ? O5 C38 1.406(4) . ? O5 C39 1.428(4) . ? O6 C40 1.393(4) . ? O6 C41 1.434(4) . ? C25 C26 1.503(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.465(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.480(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.485(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.485(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.507(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.504(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.488(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.471(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 C9 99.23(9) . . ? C1 Ge1 C17 100.23(9) . . ? C9 Ge1 C17 97.78(9) . . ? F1 Si1 C8 104.96(11) . . ? F1 Si1 C7 103.60(13) . . ? C8 Si1 C7 113.53(14) . . ? F1 Si1 C2 103.86(11) . . ? C8 Si1 C2 112.31(12) . . ? C7 Si1 C2 116.88(12) . . ? F2 Si2 C16 103.75(12) . . ? F2 Si2 C15 104.77(12) . . ? C16 Si2 C15 112.86(14) . . ? F2 Si2 C10 104.08(11) . . ? C16 Si2 C10 115.33(12) . . ? C15 Si2 C10 114.39(12) . . ? F3 Si3 C24 104.61(11) . . ? F3 Si3 C23 103.84(11) . . ? C24 Si3 C23 112.90(13) . . ? F3 Si3 C18 103.63(10) . . ? C24 Si3 C18 112.65(12) . . ? C23 Si3 C18 117.42(12) . . ? C6 C1 C2 117.8(2) . . ? C6 C1 Ge1 122.55(19) . . ? C2 C1 Ge1 119.65(17) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 Si1 118.6(2) . . ? C1 C2 Si1 122.53(18) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C1 122.2(3) . . ? C5 C6 H6A 118.9 . . ? C1 C6 H6A 118.9 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 117.2(2) . . ? C14 C9 Ge1 123.50(18) . . ? C10 C9 Ge1 119.28(18) . . ? C11 C10 C9 119.5(2) . . ? C11 C10 Si2 117.58(19) . . ? C9 C10 Si2 122.94(19) . . ? C12 C11 C10 121.7(3) . . ? C12 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C13 C14 C9 122.4(2) . . ? C13 C14 H14A 118.8 . . ? C9 C14 H14A 118.8 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 117.3(2) . . ? C22 C17 Ge1 121.72(19) . . ? C18 C17 Ge1 120.63(17) . . ? C19 C18 C17 119.2(2) . . ? C19 C18 Si3 117.7(2) . . ? C17 C18 Si3 123.09(18) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C17 122.4(3) . . ? C21 C22 H22A 118.8 . . ? C17 C22 H22A 118.8 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 K1 O1 121.82(7) . . ? O4 K1 O6 92.15(7) . . ? O1 K1 O6 142.24(6) . . ? O4 K1 O2 97.81(7) . . ? O1 K1 O2 59.96(7) . . ? O6 K1 O2 102.81(7) . . ? O4 K1 O3 59.75(6) . . ? O1 K1 O3 95.97(6) . . ? O6 K1 O3 116.85(6) . . ? O2 K1 O3 133.70(6) . . ? O4 K1 O5 127.37(7) . . ? O1 K1 O5 103.28(7) . . ? O6 K1 O5 59.89(6) . . ? O2 K1 O5 129.62(6) . . ? O3 K1 O5 92.27(6) . . ? O4 K1 N2 61.75(7) . . ? O1 K1 N2 120.23(8) . . ? O6 K1 N2 59.03(8) . . ? O2 K1 N2 60.58(8) . . ? O3 K1 N2 121.11(7) . . ? O5 K1 N2 118.47(8) . . ? O4 K1 N1 118.10(7) . . ? O1 K1 N1 60.58(8) . . ? O6 K1 N1 120.27(8) . . ? O2 K1 N1 120.20(8) . . ? O3 K1 N1 58.65(6) . . ? O5 K1 N1 60.90(7) . . ? N2 K1 N1 179.17(9) . . ? C31 N1 C37 110.3(3) . . ? C31 N1 C25 109.5(3) . . ? C37 N1 C25 111.2(3) . . ? C31 N1 K1 111.27(18) . . ? C37 N1 K1 106.24(18) . . ? C25 N1 K1 108.4(2) . . ? C42 N2 C36 109.0(3) . . ? C42 N2 C30 110.4(3) . . ? C36 N2 C30 110.9(3) . . ? C42 N2 K1 111.8(2) . . ? C36 N2 K1 106.7(2) . . ? C30 N2 K1 108.0(2) . . ? C26 O1 C27 111.9(3) . . ? C26 O1 K1 115.7(2) . . ? C27 O1 K1 116.6(2) . . ? C29 O2 C28 111.7(3) . . ? C29 O2 K1 116.7(2) . . ? C28 O2 K1 113.19(19) . . ? C32 O3 C33 111.7(2) . . ? C32 O3 K1 116.67(16) . . ? C33 O3 K1 114.19(17) . . ? C34 O4 C35 110.8(3) . . ? C34 O4 K1 115.87(17) . . ? C35 O4 K1 114.03(19) . . ? C38 O5 C39 111.7(3) . . ? C38 O5 K1 114.84(19) . . ? C39 O5 K1 107.98(17) . . ? C40 O6 C41 112.5(3) . . ? C40 O6 K1 118.24(19) . . ? C41 O6 K1 115.73(18) . . ? N1 C25 C26 113.9(3) . . ? N1 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? N1 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? O1 C26 C25 108.9(3) . . ? O1 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O1 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? O1 C27 C28 109.5(3) . . ? O1 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? O1 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? O2 C28 C27 109.4(3) . . ? O2 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? O2 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? O2 C29 C30 109.0(3) . . ? O2 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? O2 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? N2 C30 C29 114.7(3) . . ? N2 C30 H30A 108.6 . . ? C29 C30 H30A 108.6 . . ? N2 C30 H30B 108.6 . . ? C29 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? N1 C31 C32 112.6(3) . . ? N1 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? N1 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? O3 C32 C31 108.7(2) . . ? O3 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? O3 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.3 . . ? O3 C33 C34 108.9(2) . . ? O3 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? O3 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O4 C34 C33 109.2(3) . . ? O4 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O4 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? O4 C35 C36 108.3(4) . . ? O4 C35 H35A 110.0 . . ? C36 C35 H35A 110.0 . . ? O4 C35 H35B 110.0 . . ? C36 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? N2 C36 C35 112.6(3) . . ? N2 C36 H36A 109.1 . . ? C35 C36 H36A 109.1 . . ? N2 C36 H36B 109.1 . . ? C35 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? N1 C37 C38 113.3(3) . . ? N1 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? N1 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? O5 C38 C37 109.7(3) . . ? O5 C38 H38A 109.7 . . ? C37 C38 H38A 109.7 . . ? O5 C38 H38B 109.7 . . ? C37 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? O5 C39 C40 109.3(2) . . ? O5 C39 H39A 109.8 . . ? C40 C39 H39A 109.8 . . ? O5 C39 H39B 109.8 . . ? C40 C39 H39B 109.8 . . ? H39A C39 H39B 108.3 . . ? O6 C40 C39 109.1(3) . . ? O6 C40 H40A 109.9 . . ? C39 C40 H40A 109.9 . . ? O6 C40 H40B 109.9 . . ? C39 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? O6 C41 C42 108.3(3) . . ? O6 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O6 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N2 C42 C41 112.9(3) . . ? N2 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? N2 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Ge1 C1 C6 74.8(2) . . . . ? C17 Ge1 C1 C6 -24.9(2) . . . . ? C9 Ge1 C1 C2 -105.41(19) . . . . ? C17 Ge1 C1 C2 154.88(19) . . . . ? C6 C1 C2 C3 -1.2(3) . . . . ? Ge1 C1 C2 C3 178.97(18) . . . . ? C6 C1 C2 Si1 -178.99(17) . . . . ? Ge1 C1 C2 Si1 1.2(3) . . . . ? F1 Si1 C2 C3 3.8(2) . . . . ? C8 Si1 C2 C3 -109.1(2) . . . . ? C7 Si1 C2 C3 117.1(2) . . . . ? F1 Si1 C2 C1 -178.44(19) . . . . ? C8 Si1 C2 C1 68.7(2) . . . . ? C7 Si1 C2 C1 -65.1(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? Si1 C2 C3 C4 178.8(2) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? Ge1 C1 C6 C5 -179.2(2) . . . . ? C1 Ge1 C9 C14 -12.1(2) . . . . ? C17 Ge1 C9 C14 89.7(2) . . . . ? C1 Ge1 C9 C10 167.90(19) . . . . ? C17 Ge1 C9 C10 -90.3(2) . . . . ? C14 C9 C10 C11 -1.2(4) . . . . ? Ge1 C9 C10 C11 178.8(2) . . . . ? C14 C9 C10 Si2 177.75(18) . . . . ? Ge1 C9 C10 Si2 -2.2(3) . . . . ? F2 Si2 C10 C11 -2.7(2) . . . . ? C16 Si2 C10 C11 -115.7(2) . . . . ? C15 Si2 C10 C11 111.0(2) . . . . ? F2 Si2 C10 C9 178.2(2) . . . . ? C16 Si2 C10 C9 65.3(2) . . . . ? C15 Si2 C10 C9 -68.0(2) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? Si2 C10 C11 C12 -179.3(2) . . . . ? C10 C11 C12 C13 1.2(5) . . . . ? C11 C12 C13 C14 -0.7(4) . . . . ? C12 C13 C14 C9 -0.8(4) . . . . ? C10 C9 C14 C13 1.8(4) . . . . ? Ge1 C9 C14 C13 -178.2(2) . . . . ? C1 Ge1 C17 C22 83.3(2) . . . . ? C9 Ge1 C17 C22 -17.6(2) . . . . ? C1 Ge1 C17 C18 -103.4(2) . . . . ? C9 Ge1 C17 C18 155.74(19) . . . . ? C22 C17 C18 C19 0.6(4) . . . . ? Ge1 C17 C18 C19 -173.04(19) . . . . ? C22 C17 C18 Si3 -178.52(19) . . . . ? Ge1 C17 C18 Si3 7.8(3) . . . . ? F3 Si3 C18 C19 -3.6(2) . . . . ? C24 Si3 C18 C19 -116.1(2) . . . . ? C23 Si3 C18 C19 110.2(2) . . . . ? F3 Si3 C18 C17 175.6(2) . . . . ? C24 Si3 C18 C17 63.1(2) . . . . ? C23 Si3 C18 C17 -70.7(2) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? Si3 C18 C19 C20 179.3(2) . . . . ? C18 C19 C20 C21 -0.8(5) . . . . ? C19 C20 C21 C22 0.7(5) . . . . ? C20 C21 C22 C17 0.0(5) . . . . ? C18 C17 C22 C21 -0.7(4) . . . . ? Ge1 C17 C22 C21 172.9(2) . . . . ? O4 K1 N1 C31 -14.7(3) . . . . ? O1 K1 N1 C31 -127.4(2) . . . . ? O6 K1 N1 C31 96.4(2) . . . . ? O2 K1 N1 C31 -134.0(2) . . . . ? O3 K1 N1 C31 -8.5(2) . . . . ? O5 K1 N1 C31 104.6(2) . . . . ? O4 K1 N1 C37 -134.8(2) . . . . ? O1 K1 N1 C37 112.5(2) . . . . ? O6 K1 N1 C37 -23.7(2) . . . . ? O2 K1 N1 C37 105.9(2) . . . . ? O3 K1 N1 C37 -128.6(2) . . . . ? O5 K1 N1 C37 -15.5(2) . . . . ? O4 K1 N1 C25 105.6(2) . . . . ? O1 K1 N1 C25 -7.0(2) . . . . ? O6 K1 N1 C25 -143.2(2) . . . . ? O2 K1 N1 C25 -13.6(2) . . . . ? O3 K1 N1 C25 111.9(2) . . . . ? O5 K1 N1 C25 -135.0(2) . . . . ? O4 K1 N2 C42 108.2(2) . . . . ? O1 K1 N2 C42 -139.5(2) . . . . ? O6 K1 N2 C42 -3.7(2) . . . . ? O2 K1 N2 C42 -133.1(2) . . . . ? O3 K1 N2 C42 101.0(2) . . . . ? O5 K1 N2 C42 -11.3(2) . . . . ? O4 K1 N2 C36 -10.9(3) . . . . ? O1 K1 N2 C36 101.4(3) . . . . ? O6 K1 N2 C36 -122.7(3) . . . . ? O2 K1 N2 C36 107.8(3) . . . . ? O3 K1 N2 C36 -18.1(3) . . . . ? O5 K1 N2 C36 -130.4(3) . . . . ? O4 K1 N2 C30 -130.2(2) . . . . ? O1 K1 N2 C30 -17.9(2) . . . . ? O6 K1 N2 C30 118.0(2) . . . . ? O2 K1 N2 C30 -11.5(2) . . . . ? O3 K1 N2 C30 -137.4(2) . . . . ? O5 K1 N2 C30 110.3(2) . . . . ? O4 K1 O1 C26 -132.9(2) . . . . ? O6 K1 O1 C26 76.3(2) . . . . ? O2 K1 O1 C26 147.1(2) . . . . ? O3 K1 O1 C26 -75.0(2) . . . . ? O5 K1 O1 C26 18.8(2) . . . . ? N2 K1 O1 C26 153.6(2) . . . . ? N1 K1 O1 C26 -26.2(2) . . . . ? O4 K1 O1 C27 92.3(2) . . . . ? O6 K1 O1 C27 -58.5(3) . . . . ? O2 K1 O1 C27 12.3(2) . . . . ? O3 K1 O1 C27 150.2(2) . . . . ? O5 K1 O1 C27 -116.0(2) . . . . ? N2 K1 O1 C27 18.8(3) . . . . ? N1 K1 O1 C27 -161.0(3) . . . . ? O4 K1 O2 C29 30.3(2) . . . . ? O1 K1 O2 C29 152.7(2) . . . . ? O6 K1 O2 C29 -63.7(2) . . . . ? O3 K1 O2 C29 85.4(2) . . . . ? O5 K1 O2 C29 -125.1(2) . . . . ? N2 K1 O2 C29 -21.0(2) . . . . ? N1 K1 O2 C29 159.4(2) . . . . ? O4 K1 O2 C28 -101.5(2) . . . . ? O1 K1 O2 C28 20.9(2) . . . . ? O6 K1 O2 C28 164.5(2) . . . . ? O3 K1 O2 C28 -46.4(2) . . . . ? O5 K1 O2 C28 103.2(2) . . . . ? N2 K1 O2 C28 -152.7(2) . . . . ? N1 K1 O2 C28 27.6(2) . . . . ? O4 K1 O3 C32 148.6(2) . . . . ? O1 K1 O3 C32 25.1(2) . . . . ? O6 K1 O3 C32 -135.7(2) . . . . ? O2 K1 O3 C32 78.5(2) . . . . ? O5 K1 O3 C32 -78.5(2) . . . . ? N2 K1 O3 C32 155.9(2) . . . . ? N1 K1 O3 C32 -25.0(2) . . . . ? O4 K1 O3 C33 15.8(2) . . . . ? O1 K1 O3 C33 -107.7(2) . . . . ? O6 K1 O3 C33 91.5(2) . . . . ? O2 K1 O3 C33 -54.3(2) . . . . ? O5 K1 O3 C33 148.7(2) . . . . ? N2 K1 O3 C33 23.1(2) . . . . ? N1 K1 O3 C33 -157.8(2) . . . . ? O1 K1 O4 C34 95.9(2) . . . . ? O6 K1 O4 C34 -101.5(2) . . . . ? O2 K1 O4 C34 155.2(2) . . . . ? O3 K1 O4 C34 18.6(2) . . . . ? O5 K1 O4 C34 -48.6(3) . . . . ? N2 K1 O4 C34 -154.3(3) . . . . ? N1 K1 O4 C34 24.8(3) . . . . ? O1 K1 O4 C35 -133.8(3) . . . . ? O6 K1 O4 C35 28.9(3) . . . . ? O2 K1 O4 C35 -74.4(3) . . . . ? O3 K1 O4 C35 149.0(3) . . . . ? O5 K1 O4 C35 81.8(3) . . . . ? N2 K1 O4 C35 -23.9(3) . . . . ? N1 K1 O4 C35 155.2(3) . . . . ? O4 K1 O5 C38 86.2(3) . . . . ? O1 K1 O5 C38 -63.3(3) . . . . ? O6 K1 O5 C38 153.3(3) . . . . ? O2 K1 O5 C38 -125.2(2) . . . . ? O3 K1 O5 C38 33.3(3) . . . . ? N2 K1 O5 C38 160.9(2) . . . . ? N1 K1 O5 C38 -18.5(2) . . . . ? O4 K1 O5 C39 -39.2(2) . . . . ? O1 K1 O5 C39 171.26(18) . . . . ? O6 K1 O5 C39 27.92(18) . . . . ? O2 K1 O5 C39 109.45(19) . . . . ? O3 K1 O5 C39 -92.06(19) . . . . ? N2 K1 O5 C39 35.5(2) . . . . ? N1 K1 O5 C39 -143.9(2) . . . . ? O4 K1 O6 C40 138.4(2) . . . . ? O1 K1 O6 C40 -66.1(3) . . . . ? O2 K1 O6 C40 -123.1(2) . . . . ? O3 K1 O6 C40 81.5(2) . . . . ? O5 K1 O6 C40 5.5(2) . . . . ? N2 K1 O6 C40 -166.7(2) . . . . ? N1 K1 O6 C40 13.8(2) . . . . ? O4 K1 O6 C41 -83.8(2) . . . . ? O1 K1 O6 C41 71.7(2) . . . . ? O2 K1 O6 C41 14.7(2) . . . . ? O3 K1 O6 C41 -140.73(19) . . . . ? O5 K1 O6 C41 143.3(2) . . . . ? N2 K1 O6 C41 -28.9(2) . . . . ? N1 K1 O6 C41 151.58(19) . . . . ? C31 N1 C25 C26 159.9(4) . . . . ? C37 N1 C25 C26 -78.0(4) . . . . ? K1 N1 C25 C26 38.4(4) . . . . ? C27 O1 C26 C25 -165.7(3) . . . . ? K1 O1 C26 C25 57.5(4) . . . . ? N1 C25 C26 O1 -65.6(5) . . . . ? C26 O1 C27 C28 179.9(3) . . . . ? K1 O1 C27 C28 -43.6(3) . . . . ? C29 O2 C28 C27 173.6(3) . . . . ? K1 O2 C28 C27 -52.2(3) . . . . ? O1 C27 C28 O2 63.9(3) . . . . ? C28 O2 C29 C30 -175.9(3) . . . . ? K1 O2 C29 C30 51.7(3) . . . . ? C42 N2 C30 C29 166.1(3) . . . . ? C36 N2 C30 C29 -73.0(4) . . . . ? K1 N2 C30 C29 43.6(3) . . . . ? O2 C29 C30 N2 -65.8(4) . . . . ? C37 N1 C31 C32 157.6(3) . . . . ? C25 N1 C31 C32 -79.8(4) . . . . ? K1 N1 C31 C32 40.0(3) . . . . ? C33 O3 C32 C31 -169.6(3) . . . . ? K1 O3 C32 C31 56.5(3) . . . . ? N1 C31 C32 O3 -64.8(4) . . . . ? C32 O3 C33 C34 178.0(3) . . . . ? K1 O3 C33 C34 -46.9(3) . . . . ? C35 O4 C34 C33 177.7(3) . . . . ? K1 O4 C34 C33 -50.4(3) . . . . ? O3 C33 C34 O4 64.8(3) . . . . ? C34 O4 C35 C36 -170.0(3) . . . . ? K1 O4 C35 C36 57.2(4) . . . . ? C42 N2 C36 C35 -76.5(5) . . . . ? C30 N2 C36 C35 161.7(4) . . . . ? K1 N2 C36 C35 44.3(5) . . . . ? O4 C35 C36 N2 -71.0(5) . . . . ? C31 N1 C37 C38 -71.9(3) . . . . ? C25 N1 C37 C38 166.5(3) . . . . ? K1 N1 C37 C38 48.8(3) . . . . ? C39 O5 C38 C37 174.6(3) . . . . ? K1 O5 C38 C37 51.1(3) . . . . ? N1 C37 C38 O5 -71.1(4) . . . . ? C38 O5 C39 C40 172.8(3) . . . . ? K1 O5 C39 C40 -60.0(3) . . . . ? C41 O6 C40 C39 -176.2(3) . . . . ? K1 O6 C40 C39 -37.1(3) . . . . ? O5 C39 C40 O6 66.7(3) . . . . ? C40 O6 C41 C42 -159.8(3) . . . . ? K1 O6 C41 C42 60.1(3) . . . . ? C36 N2 C42 C41 152.5(3) . . . . ? C30 N2 C42 C41 -85.4(4) . . . . ? K1 N2 C42 C41 34.9(4) . . . . ? O6 C41 C42 N2 -62.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.541 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.059