# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Matioszek, Dimitri' 'Kocsor, Tibor' 'Castel, Annie' 'Nemes, Gabriela' 'Escudie, Jean' 'Saffon, Nathalie' _publ_contact_author_name 'Castel, Annie' _publ_contact_author_email castel@chem.ups-tlse.fr _publ_section_title ; Phosphaalkenyl germylenes and their gold, tungsten and molybdenum complexes ; # Attachment 'KT-chemcomm-2011.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 857220' #TrackingRef 'KT-chemcomm-2011.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H94 Cl2 Ge N2 P2' _chemical_formula_weight 1084.83 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 '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 13.9844(4) _cell_length_b 14.0830(4) _cell_length_c 18.5657(6) _cell_angle_alpha 79.5190(10) _cell_angle_beta 75.8570(10) _cell_angle_gamma 63.2850(10) _cell_volume 3156.09(16) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9877 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.78 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8271 _exptl_absorpt_correction_T_max 0.9371 _exptl_absorpt_process_details 'SADABS (BRUKER-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48874 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12787 _reflns_number_gt 9462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0621P)^2^+1.6858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12787 _refine_ls_number_parameters 720 _refine_ls_number_restraints 241 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.017 _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 0.53241(2) 0.71758(2) 0.567132(14) 0.02788(9) Uani 1 1 d . . . Cl1 Cl 0.58443(6) 0.49650(5) 0.65681(4) 0.03970(17) Uani 1 1 d . . . Cl2 Cl 0.43308(6) 0.92930(5) 0.64283(4) 0.03976(17) Uani 1 1 d . . . P1 P 0.77559(5) 0.51697(5) 0.54867(4) 0.03112(16) Uani 1 1 d . . . P2 P 0.52607(5) 0.72553(5) 0.74172(4) 0.02896(15) Uani 1 1 d . . . N1 N 0.63550(17) 0.75876(16) 0.41145(11) 0.0303(5) Uani 1 1 d . . . N2 N 0.70297(16) 0.81139(16) 0.48101(11) 0.0288(5) Uani 1 1 d . . . C1 C 0.63721(19) 0.76356(19) 0.48346(13) 0.0277(5) Uani 1 1 d . . . C2 C 0.6453(2) 0.5707(2) 0.59209(13) 0.0291(5) Uani 1 1 d . . . C3 C 0.51221(19) 0.79027(19) 0.65702(14) 0.0286(5) Uani 1 1 d . . . C4 C 0.7004(2) 0.8042(2) 0.36367(14) 0.0346(6) Uani 1 1 d . . . C5 C 0.7431(2) 0.8367(2) 0.40690(15) 0.0336(6) Uani 1 1 d . . . C6 C 0.7128(3) 0.8184(3) 0.28052(15) 0.0487(8) Uani 1 1 d . . . H6A H 0.7482 0.8663 0.2603 0.073 Uiso 1 1 calc R . . H6B H 0.6408 0.8491 0.2667 0.073 Uiso 1 1 calc R . . H6C H 0.7574 0.7489 0.2600 0.073 Uiso 1 1 calc R . . C7 C 0.8202(2) 0.8883(3) 0.38260(18) 0.0477(8) Uani 1 1 d . . . H7A H 0.8359 0.8977 0.3280 0.072 Uiso 1 1 calc R . . H7B H 0.8881 0.8430 0.4010 0.072 Uiso 1 1 calc R . . H7C H 0.7871 0.9580 0.4028 0.072 Uiso 1 1 calc R . . C8 C 0.5771(2) 0.7053(2) 0.38997(14) 0.0363(6) Uani 1 1 d . . . H8 H 0.5503 0.6702 0.4371 0.044 Uiso 1 1 calc R . . C9 C 0.4767(3) 0.7852(3) 0.3592(2) 0.0574(9) Uani 1 1 d . . . H9A H 0.4276 0.8353 0.3965 0.086 Uiso 1 1 calc R . . H9B H 0.4392 0.7473 0.3472 0.086 Uiso 1 1 calc R . . H9C H 0.4984 0.8244 0.3140 0.086 Uiso 1 1 calc R . . C10 C 0.6526(3) 0.6167(3) 0.33964(17) 0.0512(8) Uani 1 1 d . . . H10A H 0.6678 0.6477 0.2889 0.077 Uiso 1 1 calc R . . H10B H 0.6177 0.5700 0.3393 0.077 Uiso 1 1 calc R . . H10C H 0.7209 0.5750 0.3582 0.077 Uiso 1 1 calc R . . C11 C 0.7266(2) 0.8317(2) 0.54828(15) 0.0343(6) Uani 1 1 d . . . H11 H 0.6835 0.8060 0.5919 0.041 Uiso 1 1 calc R . . C12 C 0.8454(2) 0.7676(3) 0.55473(19) 0.0526(8) Uani 1 1 d . . . H12A H 0.8679 0.6928 0.5472 0.079 Uiso 1 1 calc R . . H12B H 0.8549 0.7722 0.6044 0.079 Uiso 1 1 calc R . . H12C H 0.8902 0.7963 0.5168 0.079 Uiso 1 1 calc R . . C13 C 0.6864(3) 0.9507(2) 0.55387(19) 0.0527(8) Uani 1 1 d . . . H13A H 0.7328 0.9777 0.5160 0.079 Uiso 1 1 calc R . . H13B H 0.6896 0.9624 0.6035 0.079 Uiso 1 1 calc R . . H13C H 0.6111 0.9885 0.5457 0.079 Uiso 1 1 calc R . . C14 C 0.8295(2) 0.37688(19) 0.59024(14) 0.0286(5) Uani 1 1 d . . . C15 C 0.8151(2) 0.2969(2) 0.56321(14) 0.0299(5) Uani 1 1 d . . . C16 C 0.8326(2) 0.2017(2) 0.60742(15) 0.0328(6) Uani 1 1 d . . . H16 H 0.8211 0.1488 0.5902 0.039 Uiso 1 1 calc R . . C17 C 0.8660(2) 0.1802(2) 0.67518(14) 0.0306(6) Uani 1 1 d . . . C18 C 0.8890(2) 0.2552(2) 0.69681(14) 0.0315(6) Uani 1 1 d . . . H18 H 0.9156 0.2401 0.7419 0.038 Uiso 1 1 calc R . . C19 C 0.87492(19) 0.3524(2) 0.65536(14) 0.0289(5) Uani 1 1 d . . . C20 C 0.7846(2) 0.3076(2) 0.48605(15) 0.0362(6) Uani 1 1 d . . . C21 C 0.6646(2) 0.3833(2) 0.48421(16) 0.0414(7) Uani 1 1 d . . . H21A H 0.6468 0.3792 0.4373 0.062 Uiso 1 1 calc R . . H21B H 0.6525 0.4565 0.4879 0.062 Uiso 1 1 calc R . . H21C H 0.6180 0.3624 0.5262 0.062 Uiso 1 1 calc R . . C22 C 0.8588(3) 0.3457(3) 0.42435(16) 0.0507(8) Uani 1 1 d . . . H22A H 0.9349 0.2939 0.4231 0.076 Uiso 1 1 calc R . . H22B H 0.8500 0.4153 0.4347 0.076 Uiso 1 1 calc R . . H22C H 0.8388 0.3521 0.3761 0.076 Uiso 1 1 calc R . . C23 C 0.8014(3) 0.1994(3) 0.46525(18) 0.0582(9) Uani 1 1 d . . . H23A H 0.7882 0.2073 0.4146 0.087 Uiso 1 1 calc R . . H23B H 0.7505 0.1750 0.5003 0.087 Uiso 1 1 calc R . . H23C H 0.8764 0.1469 0.4677 0.087 Uiso 1 1 calc R . . C24 C 0.8784(2) 0.0749(2) 0.72261(16) 0.0392(6) Uani 1 1 d . . . C25 C 0.9560(4) -0.0185(3) 0.6776(2) 0.0804(13) Uani 1 1 d . . . H25A H 0.9708 -0.0850 0.7098 0.121 Uiso 1 1 calc R . . H25B H 1.0243 -0.0116 0.6568 0.121 Uiso 1 1 calc R . . H25C H 0.9231 -0.0195 0.6369 0.121 Uiso 1 1 calc R . . C26 C 0.9244(4) 0.0632(3) 0.7929(2) 0.0695(11) Uani 1 1 d . . . H26A H 0.9267 -0.0022 0.8233 0.104 Uiso 1 1 calc R . . H26B H 0.8775 0.1249 0.8219 0.104 Uiso 1 1 calc R . . H26C H 0.9981 0.0595 0.7781 0.104 Uiso 1 1 calc R . . C27 C 0.7667(3) 0.0758(4) 0.7493(3) 0.0866(15) Uani 1 1 d . . . H27A H 0.7359 0.0794 0.7062 0.130 Uiso 1 1 calc R . . H27B H 0.7189 0.1380 0.7776 0.130 Uiso 1 1 calc R . . H27C H 0.7730 0.0105 0.7813 0.130 Uiso 1 1 calc R . . C28 C 0.9147(2) 0.4248(2) 0.68239(16) 0.0367(6) Uani 1 1 d . . . C29 C 0.9800(3) 0.3669(3) 0.74496(19) 0.0526(8) Uani 1 1 d . . . H29A H 1.0393 0.2991 0.7287 0.079 Uiso 1 1 calc R . . H29B H 0.9319 0.3531 0.7895 0.079 Uiso 1 1 calc R . . H29C H 1.0105 0.4116 0.7567 0.079 Uiso 1 1 calc R . . C30 C 0.8200(2) 0.5262(2) 0.71437(18) 0.0473(7) Uani 1 1 d . . . H30A H 0.7662 0.5069 0.7505 0.071 Uiso 1 1 calc R . . H30B H 0.7856 0.5748 0.6738 0.071 Uiso 1 1 calc R . . H30C H 0.8480 0.5616 0.7392 0.071 Uiso 1 1 calc R . . C31 C 0.9930(2) 0.4531(3) 0.61849(19) 0.0485(8) Uani 1 1 d . . . H31A H 1.0168 0.4995 0.6355 0.073 Uiso 1 1 calc R . . H31B H 0.9557 0.4903 0.5764 0.073 Uiso 1 1 calc R . . H31C H 1.0565 0.3876 0.6026 0.073 Uiso 1 1 calc R . . C32 C 0.4318(2) 0.82455(19) 0.80942(13) 0.0278(5) Uani 1 1 d . . . C33 C 0.4670(2) 0.8858(2) 0.84055(13) 0.0300(6) Uani 1 1 d . . . C34 C 0.3894(2) 0.9716(2) 0.87982(14) 0.0339(6) Uani 1 1 d . . . H34 H 0.4133 1.0139 0.8988 0.041 Uiso 1 1 calc R . . C35 C 0.2783(2) 0.9986(2) 0.89270(13) 0.0332(6) Uani 1 1 d . . . C36 C 0.2477(2) 0.9305(2) 0.86898(14) 0.0341(6) Uani 1 1 d . . . H36 H 0.1728 0.9445 0.8802 0.041 Uiso 1 1 calc R . . C37 C 0.3206(2) 0.8424(2) 0.82950(13) 0.0297(6) Uani 1 1 d . . . C38 C 0.5892(2) 0.8581(2) 0.83531(15) 0.0392(7) Uani 1 1 d . . . C39 C 0.6489(2) 0.7408(3) 0.86421(19) 0.0517(8) Uani 1 1 d . . . H39A H 0.6440 0.6943 0.8332 0.078 Uiso 1 1 calc R . . H39B H 0.6151 0.7295 0.9159 0.078 Uiso 1 1 calc R . . H39C H 0.7256 0.7237 0.8619 0.078 Uiso 1 1 calc R . . C40 C 0.6436(3) 0.8793(3) 0.75604(17) 0.0530(8) Uani 1 1 d . . . H40A H 0.7193 0.8644 0.7556 0.080 Uiso 1 1 calc R . . H40B H 0.6042 0.9541 0.7385 0.080 Uiso 1 1 calc R . . H40C H 0.6423 0.8330 0.7231 0.080 Uiso 1 1 calc R . . C41 C 0.6049(3) 0.9252(3) 0.88456(18) 0.0533(8) Uani 1 1 d . . . H41A H 0.6828 0.9003 0.8838 0.080 Uiso 1 1 calc R . . H41B H 0.5675 0.9177 0.9358 0.080 Uiso 1 1 calc R . . H41C H 0.5744 1.0004 0.8654 0.080 Uiso 1 1 calc R . . C42 C 0.1938(2) 1.0922(2) 0.93790(15) 0.0410(7) Uani 1 1 d . . . C43 C 0.2349(3) 1.1768(3) 0.9366(2) 0.0587(9) Uani 1 1 d . . . H43A H 0.1759 1.2386 0.9611 0.088 Uiso 1 1 calc R . . H43B H 0.2587 1.1990 0.8848 0.088 Uiso 1 1 calc R . . H43C H 0.2963 1.1468 0.9630 0.088 Uiso 1 1 calc R . . C44 C 0.0878(3) 1.1478(3) 0.9072(2) 0.0646(10) Uani 1 1 d . . . H44A H 0.0386 1.2116 0.9336 0.097 Uiso 1 1 calc R . . H44B H 0.0531 1.0990 0.9145 0.097 Uiso 1 1 calc R . . H44C H 0.1039 1.1685 0.8539 0.097 Uiso 1 1 calc R . . C45 C 0.1702(3) 1.0498(3) 1.01898(17) 0.0626(10) Uani 1 1 d . . . H45A H 0.2378 1.0151 1.0389 0.094 Uiso 1 1 calc R . . H45B H 0.1404 0.9979 1.0214 0.094 Uiso 1 1 calc R . . H45C H 0.1172 1.1091 1.0485 0.094 Uiso 1 1 calc R . . C46 C 0.2746(2) 0.7681(2) 0.81279(15) 0.0357(6) Uani 1 1 d . . . C47 C 0.1634(2) 0.7868(3) 0.86351(19) 0.0514(8) Uani 1 1 d . . . H47A H 0.1399 0.7341 0.8558 0.077 Uiso 1 1 calc R . . H47B H 0.1094 0.8587 0.8512 0.077 Uiso 1 1 calc R . . H47C H 0.1701 0.7796 0.9158 0.077 Uiso 1 1 calc R . . C48 C 0.2568(3) 0.7882(3) 0.73239(17) 0.0514(8) Uani 1 1 d . . . H48A H 0.3274 0.7651 0.6984 0.077 Uiso 1 1 calc R . . H48B H 0.2133 0.8644 0.7212 0.077 Uiso 1 1 calc R . . H48C H 0.2183 0.7478 0.7260 0.077 Uiso 1 1 calc R . . C49 C 0.3492(3) 0.6496(2) 0.8300(2) 0.0550(8) Uani 1 1 d . . . H49A H 0.3109 0.6059 0.8299 0.083 Uiso 1 1 calc R . . H49B H 0.3683 0.6397 0.8790 0.083 Uiso 1 1 calc R . . H49C H 0.4157 0.6278 0.7919 0.083 Uiso 1 1 calc R . . C50 C 0.1367(4) 0.5194(4) 0.9207(3) 0.0767(12) Uani 1 1 d . . . C51 C 0.0344(3) 0.5994(4) 0.9403(3) 0.0744(12) Uani 1 1 d . . . H51 H 0.0088 0.6174 0.9905 0.089 Uiso 1 1 calc R . . C52 C -0.0322(4) 0.6547(4) 0.8879(3) 0.0895(14) Uani 1 1 d . . . H52 H -0.1027 0.7094 0.9026 0.107 Uiso 1 1 calc R . . C53 C 0.0031(4) 0.6306(4) 0.8156(3) 0.0937(15) Uani 1 1 d . . . H53 H -0.0415 0.6690 0.7794 0.112 Uiso 1 1 calc R . . C54 C 0.1055(5) 0.5490(4) 0.7959(3) 0.0919(14) Uani 1 1 d . . . H54 H 0.1306 0.5308 0.7457 0.110 Uiso 1 1 calc R . . C55 C 0.1708(4) 0.4945(4) 0.8470(3) 0.0795(12) Uani 1 1 d . . . H55 H 0.2405 0.4387 0.8321 0.095 Uiso 1 1 calc R . . C56 C 0.2084(5) 0.4639(4) 0.9746(3) 0.1072(17) Uani 1 1 d . . . H56A H 0.1651 0.4729 1.0252 0.161 Uiso 1 1 calc R . . H56B H 0.2615 0.4936 0.9684 0.161 Uiso 1 1 calc R . . H56C H 0.2468 0.3878 0.9666 0.161 Uiso 1 1 calc R . . C63 C 0.656(2) 0.4167(19) 0.9441(12) 0.130(5) Uani 0.376(18) 1 d PDU A 1 H63A H 0.6916 0.4480 0.9008 0.195 Uiso 0.376(18) 1 calc PR A 1 H63B H 0.7105 0.3663 0.9737 0.195 Uiso 0.376(18) 1 calc PR A 1 H63C H 0.6001 0.4734 0.9748 0.195 Uiso 0.376(18) 1 calc PR A 1 C57 C 0.6048(14) 0.3596(14) 0.9184(10) 0.096(2) Uani 0.376(18) 1 d PDU A 1 C58 C 0.5681(19) 0.3833(18) 0.8543(12) 0.086(3) Uani 0.376(18) 1 d PDU A 1 H58 H 0.5811 0.4363 0.8192 0.103 Uiso 0.376(18) 1 calc PR A 1 C59 C 0.512(2) 0.334(2) 0.8375(11) 0.085(3) Uani 0.376(18) 1 d PDU A 1 H59 H 0.4790 0.3580 0.7948 0.101 Uiso 0.376(18) 1 calc PR A 1 C60 C 0.5052(18) 0.2469(17) 0.8840(13) 0.090(3) Uani 0.376(18) 1 d PDU A 1 H60 H 0.4673 0.2105 0.8742 0.108 Uiso 0.376(18) 1 calc PR A 1 C61 C 0.556(2) 0.2154(18) 0.9462(12) 0.096(3) Uani 0.376(18) 1 d PDU A 1 H61 H 0.5567 0.1538 0.9774 0.115 Uiso 0.376(18) 1 calc PR A 1 C62 C 0.6047(19) 0.2695(17) 0.9626(11) 0.101(3) Uani 0.376(18) 1 d PDU A 1 H62 H 0.6391 0.2460 1.0048 0.122 Uiso 0.376(18) 1 calc PR A 1 C63' C 0.7168(12) 0.3527(13) 0.9283(7) 0.128(4) Uani 0.624(18) 1 d PDU A 2 H63D H 0.7286 0.3224 0.9789 0.192 Uiso 0.624(18) 1 calc PR A 2 H63E H 0.6883 0.4305 0.9259 0.192 Uiso 0.624(18) 1 calc PR A 2 H63F H 0.7860 0.3243 0.8931 0.192 Uiso 0.624(18) 1 calc PR A 2 C57' C 0.6358(9) 0.3231(10) 0.9081(6) 0.092(2) Uani 0.624(18) 1 d PDU A 2 C58' C 0.5903(11) 0.3746(11) 0.8471(7) 0.084(2) Uani 0.624(18) 1 d PDU A 2 H58' H 0.6047 0.4327 0.8210 0.101 Uiso 0.624(18) 1 calc PR A 2 C59' C 0.5238(12) 0.3443(11) 0.8224(7) 0.083(2) Uani 0.624(18) 1 d PDU A 2 H59' H 0.4975 0.3776 0.7775 0.099 Uiso 0.624(18) 1 calc PR A 2 C60' C 0.4955(9) 0.2655(9) 0.8630(6) 0.080(2) Uani 0.624(18) 1 d PDU A 2 H60' H 0.4488 0.2445 0.8470 0.095 Uiso 0.624(18) 1 calc PR A 2 C61' C 0.5371(11) 0.2171(9) 0.9283(6) 0.083(2) Uani 0.624(18) 1 d PDU A 2 H61' H 0.5177 0.1636 0.9578 0.100 Uiso 0.624(18) 1 calc PR A 2 C62' C 0.6052(11) 0.2472(9) 0.9491(6) 0.088(2) Uani 0.624(18) 1 d PDU A 2 H62' H 0.6325 0.2143 0.9937 0.106 Uiso 0.624(18) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02744(14) 0.03368(16) 0.02394(15) 0.00027(11) -0.00538(11) -0.01488(12) Cl1 0.0477(4) 0.0374(4) 0.0352(4) 0.0014(3) 0.0027(3) -0.0259(3) Cl2 0.0431(4) 0.0290(3) 0.0382(4) 0.0009(3) -0.0078(3) -0.0087(3) P1 0.0306(3) 0.0286(4) 0.0342(4) 0.0050(3) -0.0067(3) -0.0151(3) P2 0.0287(3) 0.0308(4) 0.0268(3) -0.0005(3) -0.0066(3) -0.0122(3) N1 0.0318(11) 0.0317(12) 0.0234(11) 0.0021(9) -0.0056(9) -0.0116(9) N2 0.0251(10) 0.0286(11) 0.0289(11) 0.0025(9) -0.0043(9) -0.0101(9) C1 0.0263(12) 0.0261(13) 0.0266(13) 0.0020(10) -0.0068(10) -0.0083(10) C2 0.0374(14) 0.0285(13) 0.0253(13) 0.0032(10) -0.0067(11) -0.0191(11) C3 0.0269(12) 0.0279(13) 0.0318(13) -0.0018(10) -0.0054(11) -0.0125(11) C4 0.0313(13) 0.0345(15) 0.0263(13) 0.0049(11) -0.0013(11) -0.0085(12) C5 0.0261(12) 0.0300(14) 0.0343(14) 0.0063(11) 0.0009(11) -0.0094(11) C6 0.0469(17) 0.059(2) 0.0286(15) 0.0050(13) -0.0008(13) -0.0186(15) C7 0.0377(15) 0.0516(19) 0.0496(18) 0.0078(14) 0.0003(14) -0.0240(14) C8 0.0423(15) 0.0401(16) 0.0275(14) -0.0019(11) -0.0100(12) -0.0170(13) C9 0.0477(18) 0.061(2) 0.065(2) -0.0065(17) -0.0246(17) -0.0164(16) C10 0.0576(19) 0.0463(18) 0.0432(17) -0.0072(14) -0.0108(15) -0.0146(15) C11 0.0365(14) 0.0383(15) 0.0325(14) 0.0032(11) -0.0068(12) -0.0218(12) C12 0.0424(17) 0.070(2) 0.0558(19) 0.0067(16) -0.0210(15) -0.0308(16) C13 0.068(2) 0.0456(19) 0.0509(19) -0.0037(15) -0.0070(16) -0.0321(17) C14 0.0282(12) 0.0260(13) 0.0292(13) 0.0011(10) -0.0032(10) -0.0116(11) C15 0.0287(13) 0.0304(14) 0.0297(13) -0.0015(10) -0.0049(11) -0.0124(11) C16 0.0323(13) 0.0293(14) 0.0386(15) -0.0021(11) -0.0058(12) -0.0153(11) C17 0.0259(12) 0.0291(14) 0.0333(14) 0.0026(11) -0.0021(11) -0.0121(11) C18 0.0279(13) 0.0351(15) 0.0280(13) 0.0007(11) -0.0057(11) -0.0114(11) C19 0.0236(12) 0.0302(14) 0.0314(13) -0.0031(10) -0.0036(10) -0.0108(10) C20 0.0432(15) 0.0375(15) 0.0313(14) -0.0006(11) -0.0101(12) -0.0192(13) C21 0.0441(16) 0.0471(17) 0.0436(16) 0.0014(13) -0.0177(13) -0.0257(14) C22 0.0470(17) 0.072(2) 0.0301(15) -0.0007(14) -0.0086(13) -0.0237(16) C23 0.085(3) 0.049(2) 0.0437(18) -0.0100(15) -0.0246(17) -0.0225(18) C24 0.0405(15) 0.0337(15) 0.0436(16) 0.0091(12) -0.0102(13) -0.0191(13) C25 0.102(3) 0.036(2) 0.083(3) 0.0074(18) -0.019(2) -0.016(2) C26 0.096(3) 0.062(2) 0.061(2) 0.0303(18) -0.035(2) -0.045(2) C27 0.061(2) 0.084(3) 0.115(4) 0.051(3) -0.022(2) -0.049(2) C28 0.0342(14) 0.0341(15) 0.0454(16) -0.0054(12) -0.0145(12) -0.0133(12) C29 0.060(2) 0.0447(18) 0.064(2) -0.0043(15) -0.0337(17) -0.0207(16) C30 0.0478(17) 0.0428(17) 0.0552(19) -0.0144(14) -0.0189(15) -0.0142(14) C31 0.0410(16) 0.0497(19) 0.066(2) -0.0022(15) -0.0141(15) -0.0280(15) C32 0.0315(13) 0.0293(13) 0.0219(12) 0.0024(10) -0.0062(10) -0.0133(11) C33 0.0356(14) 0.0376(15) 0.0215(12) 0.0033(11) -0.0058(11) -0.0216(12) C34 0.0431(15) 0.0389(15) 0.0259(13) -0.0018(11) -0.0089(12) -0.0218(13) C35 0.0396(14) 0.0374(15) 0.0200(12) 0.0002(10) -0.0038(11) -0.0160(12) C36 0.0328(14) 0.0408(16) 0.0297(14) -0.0003(11) -0.0046(11) -0.0181(12) C37 0.0333(13) 0.0359(14) 0.0228(12) 0.0026(10) -0.0064(10) -0.0184(12) C38 0.0354(14) 0.0559(18) 0.0352(15) -0.0047(13) -0.0086(12) -0.0259(14) C39 0.0370(16) 0.063(2) 0.057(2) -0.0070(16) -0.0217(15) -0.0152(15) C40 0.0508(18) 0.085(3) 0.0433(17) -0.0088(16) -0.0038(15) -0.0480(18) C41 0.0504(18) 0.079(2) 0.0469(18) -0.0122(17) -0.0091(15) -0.0394(18) C42 0.0466(16) 0.0441(17) 0.0293(14) -0.0065(12) -0.0025(12) -0.0179(14) C43 0.069(2) 0.0436(19) 0.059(2) -0.0168(16) 0.0018(18) -0.0226(17) C44 0.0503(19) 0.061(2) 0.066(2) -0.0260(18) -0.0133(17) -0.0003(17) C45 0.087(3) 0.059(2) 0.0320(17) -0.0095(15) 0.0076(17) -0.030(2) C46 0.0331(14) 0.0434(16) 0.0378(15) -0.0042(12) -0.0030(12) -0.0239(13) C47 0.0445(17) 0.062(2) 0.058(2) -0.0089(16) 0.0036(15) -0.0366(16) C48 0.0520(18) 0.080(2) 0.0445(17) -0.0088(16) -0.0110(15) -0.0449(18) C49 0.0509(19) 0.0423(18) 0.077(2) -0.0058(16) -0.0001(17) -0.0295(16) C50 0.083(3) 0.077(3) 0.091(3) -0.011(2) -0.002(3) -0.057(3) C51 0.068(3) 0.084(3) 0.079(3) -0.033(2) 0.017(2) -0.044(2) C52 0.070(3) 0.096(4) 0.113(4) -0.033(3) -0.002(3) -0.042(3) C53 0.084(3) 0.106(4) 0.109(4) -0.039(3) 0.002(3) -0.055(3) C54 0.101(4) 0.110(4) 0.082(3) -0.034(3) 0.005(3) -0.061(3) C55 0.084(3) 0.082(3) 0.079(3) -0.035(2) 0.016(3) -0.046(3) C56 0.120(4) 0.101(4) 0.122(4) 0.011(3) -0.034(4) -0.067(3) C63 0.163(12) 0.128(11) 0.123(10) -0.029(9) -0.043(9) -0.068(9) C57 0.127(5) 0.097(5) 0.063(4) 0.000(4) -0.022(4) -0.048(4) C58 0.108(5) 0.090(4) 0.057(4) 0.009(4) -0.022(4) -0.042(4) C59 0.101(5) 0.086(4) 0.061(5) 0.019(4) -0.015(4) -0.043(4) C60 0.108(4) 0.088(5) 0.059(6) 0.017(4) -0.008(4) -0.041(4) C61 0.124(6) 0.088(5) 0.052(6) 0.015(5) -0.005(5) -0.038(4) C62 0.138(5) 0.094(5) 0.054(5) 0.010(5) -0.011(4) -0.043(4) C63' 0.142(8) 0.151(9) 0.115(7) -0.035(6) -0.033(6) -0.070(7) C57' 0.121(4) 0.094(4) 0.058(4) -0.001(3) -0.015(3) -0.046(3) C58' 0.105(5) 0.089(4) 0.055(3) 0.016(3) -0.018(3) -0.045(3) C59' 0.101(4) 0.085(4) 0.058(4) 0.021(3) -0.015(4) -0.046(3) C60' 0.099(4) 0.081(4) 0.055(5) 0.018(4) -0.009(3) -0.046(3) C61' 0.117(5) 0.076(4) 0.045(5) 0.009(3) -0.001(4) -0.044(3) C62' 0.132(4) 0.080(4) 0.049(4) 0.004(3) -0.015(3) -0.047(3) _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 C3 2.011(2) . ? Ge1 C2 2.014(2) . ? Ge1 C1 2.087(2) . ? Cl1 C2 1.762(2) . ? Cl2 C3 1.770(3) . ? P1 C2 1.675(3) . ? P1 C14 1.857(2) . ? P2 C3 1.676(3) . ? P2 C32 1.854(3) . ? N1 C1 1.357(3) . ? N1 C4 1.394(3) . ? N1 C8 1.487(3) . ? N2 C1 1.352(3) . ? N2 C5 1.399(3) . ? N2 C11 1.472(3) . ? C4 C5 1.349(4) . ? C4 C6 1.497(4) . ? C5 C7 1.499(4) . ? C8 C9 1.517(4) . ? C8 C10 1.518(4) . ? C11 C12 1.517(4) . ? C11 C13 1.524(4) . ? C14 C19 1.418(3) . ? C14 C15 1.421(4) . ? C15 C16 1.391(4) . ? C15 C20 1.555(4) . ? C16 C17 1.383(4) . ? C17 C18 1.379(4) . ? C17 C24 1.540(4) . ? C18 C19 1.398(4) . ? C19 C28 1.561(4) . ? C20 C21 1.535(4) . ? C20 C22 1.541(4) . ? C20 C23 1.541(4) . ? C24 C25 1.510(5) . ? C24 C27 1.514(4) . ? C24 C26 1.542(5) . ? C28 C31 1.533(4) . ? C28 C29 1.534(4) . ? C28 C30 1.540(4) . ? C32 C37 1.422(3) . ? C32 C33 1.423(3) . ? C33 C34 1.387(4) . ? C33 C38 1.554(4) . ? C34 C35 1.391(4) . ? C35 C36 1.383(4) . ? C35 C42 1.534(4) . ? C36 C37 1.394(4) . ? C37 C46 1.557(4) . ? C38 C40 1.527(4) . ? C38 C39 1.540(4) . ? C38 C41 1.542(4) . ? C42 C45 1.529(4) . ? C42 C44 1.530(4) . ? C42 C43 1.532(4) . ? C46 C48 1.528(4) . ? C46 C49 1.542(4) . ? C46 C47 1.544(4) . ? C50 C51 1.376(6) . ? C50 C55 1.389(6) . ? C50 C56 1.455(7) . ? C51 C52 1.391(7) . ? C52 C53 1.359(7) . ? C53 C54 1.387(7) . ? C54 C55 1.360(7) . ? C63 C57 1.488(14) . ? C57 C58 1.338(13) . ? C57 C62 1.381(14) . ? C58 C59 1.374(14) . ? C59 C60 1.387(14) . ? C60 C61 1.405(15) . ? C61 C62 1.332(15) . ? C63' C57' 1.511(11) . ? C57' C58' 1.361(9) . ? C57' C62' 1.365(10) . ? C58' C59' 1.375(10) . ? C59' C60' 1.379(9) . ? C60' C61' 1.400(10) . ? C61' C62' 1.356(11) . ? 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 C3 Ge1 C2 100.39(10) . . ? C3 Ge1 C1 105.76(10) . . ? C2 Ge1 C1 96.04(9) . . ? C2 P1 C14 103.95(11) . . ? C3 P2 C32 105.96(11) . . ? C1 N1 C4 110.1(2) . . ? C1 N1 C8 122.8(2) . . ? C4 N1 C8 127.0(2) . . ? C1 N2 C5 110.0(2) . . ? C1 N2 C11 123.1(2) . . ? C5 N2 C11 126.9(2) . . ? N2 C1 N1 106.0(2) . . ? N2 C1 Ge1 135.30(18) . . ? N1 C1 Ge1 118.20(18) . . ? P1 C2 Cl1 122.92(15) . . ? P1 C2 Ge1 125.76(13) . . ? Cl1 C2 Ge1 110.65(13) . . ? P2 C3 Cl2 123.17(15) . . ? P2 C3 Ge1 122.83(14) . . ? Cl2 C3 Ge1 110.24(12) . . ? C5 C4 N1 106.9(2) . . ? C5 C4 C6 128.1(3) . . ? N1 C4 C6 124.8(3) . . ? C4 C5 N2 106.9(2) . . ? C4 C5 C7 128.0(3) . . ? N2 C5 C7 125.1(3) . . ? N1 C8 C9 111.8(2) . . ? N1 C8 C10 112.2(2) . . ? C9 C8 C10 113.5(2) . . ? N2 C11 C12 112.0(2) . . ? N2 C11 C13 111.5(2) . . ? C12 C11 C13 113.2(3) . . ? C19 C14 C15 119.4(2) . . ? C19 C14 P1 118.88(19) . . ? C15 C14 P1 121.31(19) . . ? C16 C15 C14 118.1(2) . . ? C16 C15 C20 117.8(2) . . ? C14 C15 C20 124.1(2) . . ? C17 C16 C15 123.3(2) . . ? C18 C17 C16 117.4(2) . . ? C18 C17 C24 122.5(2) . . ? C16 C17 C24 120.1(2) . . ? C17 C18 C19 123.0(2) . . ? C18 C19 C14 118.1(2) . . ? C18 C19 C28 117.5(2) . . ? C14 C19 C28 124.3(2) . . ? C21 C20 C22 109.8(2) . . ? C21 C20 C23 106.0(2) . . ? C22 C20 C23 106.4(3) . . ? C21 C20 C15 112.6(2) . . ? C22 C20 C15 110.3(2) . . ? C23 C20 C15 111.4(2) . . ? C25 C24 C27 112.2(3) . . ? C25 C24 C17 109.9(2) . . ? C27 C24 C17 108.5(2) . . ? C25 C24 C26 107.8(3) . . ? C27 C24 C26 106.7(3) . . ? C17 C24 C26 111.7(2) . . ? C31 C28 C29 105.7(2) . . ? C31 C28 C30 110.9(2) . . ? C29 C28 C30 105.8(2) . . ? C31 C28 C19 109.8(2) . . ? C29 C28 C19 111.7(2) . . ? C30 C28 C19 112.7(2) . . ? C37 C32 C33 118.7(2) . . ? C37 C32 P2 119.54(19) . . ? C33 C32 P2 121.74(19) . . ? C34 C33 C32 118.8(2) . . ? C34 C33 C38 118.3(2) . . ? C32 C33 C38 122.8(2) . . ? C33 C34 C35 123.1(2) . . ? C36 C35 C34 116.6(2) . . ? C36 C35 C42 120.7(2) . . ? C34 C35 C42 122.4(2) . . ? C35 C36 C37 123.7(2) . . ? C36 C37 C32 118.1(2) . . ? C36 C37 C46 117.3(2) . . ? C32 C37 C46 124.5(2) . . ? C40 C38 C39 110.7(3) . . ? C40 C38 C41 106.2(2) . . ? C39 C38 C41 106.2(2) . . ? C40 C38 C33 112.0(2) . . ? C39 C38 C33 109.5(2) . . ? C41 C38 C33 112.1(2) . . ? C45 C42 C44 109.4(3) . . ? C45 C42 C43 108.1(3) . . ? C44 C42 C43 107.2(3) . . ? C45 C42 C35 108.8(2) . . ? C44 C42 C35 111.4(2) . . ? C43 C42 C35 112.0(2) . . ? C48 C46 C49 110.3(3) . . ? C48 C46 C47 106.8(2) . . ? C49 C46 C47 105.2(2) . . ? C48 C46 C37 111.8(2) . . ? C49 C46 C37 111.3(2) . . ? C47 C46 C37 111.0(2) . . ? C51 C50 C55 117.7(5) . . ? C51 C50 C56 121.6(5) . . ? C55 C50 C56 120.7(5) . . ? C50 C51 C52 121.3(4) . . ? C53 C52 C51 120.3(5) . . ? C52 C53 C54 118.7(5) . . ? C55 C54 C53 121.2(5) . . ? C54 C55 C50 120.8(5) . . ? C58 C57 C62 118.6(14) . . ? C58 C57 C63 125.6(15) . . ? C62 C57 C63 115.5(14) . . ? C57 C58 C59 122.2(15) . . ? C58 C59 C60 119.0(15) . . ? C59 C60 C61 117.2(14) . . ? C62 C61 C60 121.8(15) . . ? C61 C62 C57 120.2(15) . . ? C58' C57' C62' 118.2(9) . . ? C58' C57' C63' 119.2(9) . . ? C62' C57' C63' 122.7(9) . . ? C57' C58' C59' 121.5(9) . . ? C58' C59' C60' 119.8(9) . . ? C59' C60' C61' 118.5(8) . . ? C62' C61' C60' 119.5(8) . . ? C61' C62' C57' 122.2(9) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.060 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.062 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 857221' #TrackingRef 'KT-chemcomm-2011.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H84 Cl8 Ge N2 O4 P2 W' _chemical_formula_weight 1451.23 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' W W -0.8490 6.8722 '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 12.0774(6) _cell_length_b 14.8952(8) _cell_length_c 21.9932(16) _cell_angle_alpha 100.256(3) _cell_angle_beta 96.379(3) _cell_angle_gamma 113.219(2) _cell_volume 3505.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9847 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 29.36 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 2.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4551 _exptl_absorpt_correction_T_max 0.8276 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63975 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14094 _reflns_number_gt 12191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0443P)^2^+6.1541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14094 _refine_ls_number_parameters 748 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.468608(13) 0.288278(11) 0.342508(7) 0.02670(6) Uani 1 1 d . . . P1 P 0.35709(9) 0.23278(8) 0.23049(5) 0.0275(2) Uani 1 1 d . . . C1 C 0.2126(3) 0.1583(3) 0.23322(17) 0.0249(7) Uani 1 1 d . . . Cl1 Cl 0.09620(10) 0.08257(9) 0.16834(5) 0.0408(2) Uani 1 1 d . . . Ge1 Ge 0.23187(3) 0.16764(3) 0.326418(16) 0.02046(8) Uani 1 1 d . . . P2 P 0.06453(8) -0.02145(7) 0.37877(5) 0.0251(2) Uani 1 1 d . . . Cl2 Cl 0.22709(9) -0.04140(7) 0.28780(5) 0.0348(2) Uani 1 1 d . . . N1 N 0.0020(3) 0.2062(2) 0.33915(15) 0.0256(6) Uani 1 1 d . . . N2 N 0.1412(3) 0.2748(2) 0.42458(14) 0.0245(6) Uani 1 1 d . . . O1 O 0.5672(4) 0.3248(3) 0.48665(17) 0.0718(12) Uani 1 1 d . . . O2 O 0.4034(4) 0.4756(3) 0.37053(18) 0.0678(11) Uani 1 1 d . . . O3 O 0.7253(4) 0.4323(3) 0.3236(3) 0.0917(15) Uani 1 1 d U . . O4 O 0.5387(3) 0.1031(2) 0.33431(15) 0.0432(7) Uani 1 1 d . . . C2 C 0.1138(3) 0.2163(3) 0.36570(17) 0.0231(7) Uani 1 1 d . . . C3 C -0.0409(3) 0.2594(3) 0.38157(19) 0.0298(8) Uani 1 1 d . . . C4 C 0.0451(4) 0.3011(3) 0.43510(19) 0.0303(8) Uani 1 1 d . . . C5 C -0.1582(4) 0.2703(4) 0.3670(2) 0.0468(11) Uani 1 1 d . . . H5A H -0.1607 0.3212 0.4011 0.070 Uiso 1 1 calc R . . H5B H -0.2281 0.2056 0.3629 0.070 Uiso 1 1 calc R . . H5C H -0.1627 0.2912 0.3273 0.070 Uiso 1 1 calc R . . C6 C 0.0425(5) 0.3644(4) 0.4954(2) 0.0441(11) Uani 1 1 d . . . H6A H 0.1087 0.4322 0.5033 0.066 Uiso 1 1 calc R . . H6B H 0.0540 0.3340 0.5302 0.066 Uiso 1 1 calc R . . H6C H -0.0369 0.3684 0.4922 0.066 Uiso 1 1 calc R . . C7 C -0.0668(3) 0.1388(3) 0.27640(18) 0.0308(8) Uani 1 1 d . . . H7 H -0.0154 0.1043 0.2610 0.037 Uiso 1 1 calc R . . C8 C -0.1875(4) 0.0562(3) 0.2817(2) 0.0450(11) Uani 1 1 d . . . H8A H -0.1726 0.0270 0.3166 0.067 Uiso 1 1 calc R . . H8B H -0.2211 0.0036 0.2422 0.067 Uiso 1 1 calc R . . H8C H -0.2464 0.0849 0.2896 0.067 Uiso 1 1 calc R . . C9 C -0.0818(4) 0.1967(4) 0.2289(2) 0.0444(11) Uani 1 1 d . . . H9A H -0.1346 0.2298 0.2412 0.067 Uiso 1 1 calc R . . H9B H -0.1195 0.1504 0.1872 0.067 Uiso 1 1 calc R . . H9C H -0.0010 0.2477 0.2275 0.067 Uiso 1 1 calc R . . C10 C 0.2515(4) 0.2960(3) 0.47150(18) 0.0352(9) Uani 1 1 d . . . H10 H 0.3076 0.2762 0.4479 0.042 Uiso 1 1 calc R . . C11 C 0.2178(5) 0.2301(4) 0.5180(2) 0.0527(12) Uani 1 1 d . . . H11A H 0.1684 0.2512 0.5448 0.079 Uiso 1 1 calc R . . H11B H 0.2931 0.2371 0.5444 0.079 Uiso 1 1 calc R . . H11C H 0.1703 0.1597 0.4948 0.079 Uiso 1 1 calc R . . C12 C 0.3226(5) 0.4076(4) 0.5043(2) 0.0582(14) Uani 1 1 d . . . H12A H 0.3251 0.4480 0.4734 0.087 Uiso 1 1 calc R . . H12B H 0.4067 0.4209 0.5231 0.087 Uiso 1 1 calc R . . H12C H 0.2817 0.4256 0.5374 0.087 Uiso 1 1 calc R . . C13 C 0.1615(3) 0.0263(3) 0.33218(16) 0.0226(7) Uani 1 1 d . . . C14 C 0.3787(4) 0.2388(3) 0.14905(18) 0.0322(9) Uani 1 1 d . . . C15 C 0.3542(4) 0.3096(3) 0.1218(2) 0.0343(9) Uani 1 1 d . . . C16 C 0.3568(5) 0.3033(4) 0.0578(2) 0.0450(11) Uani 1 1 d . . . H16 H 0.3386 0.3500 0.0392 0.054 Uiso 1 1 calc R . . C17 C 0.3840(5) 0.2331(4) 0.0199(2) 0.0480(11) Uani 1 1 d . . . C18 C 0.4120(5) 0.1673(4) 0.0488(2) 0.0473(11) Uani 1 1 d . . . H18 H 0.4316 0.1187 0.0239 0.057 Uiso 1 1 calc R . . C19 C 0.4130(4) 0.1683(4) 0.1122(2) 0.0391(10) Uani 1 1 d . . . C20 C 0.3346(4) 0.4001(3) 0.1581(2) 0.0413(10) Uani 1 1 d . . . C21 C 0.2150(5) 0.3650(4) 0.1821(3) 0.0602(14) Uani 1 1 d . . . H21A H 0.2243 0.3369 0.2184 0.090 Uiso 1 1 calc R . . H21B H 0.1487 0.3132 0.1485 0.090 Uiso 1 1 calc R . . H21C H 0.1947 0.4222 0.1950 0.090 Uiso 1 1 calc R . . C22 C 0.4453(5) 0.4643(4) 0.2116(3) 0.0598(14) Uani 1 1 d . . . H22A H 0.4553 0.4229 0.2399 0.090 Uiso 1 1 calc R . . H22B H 0.4322 0.5204 0.2352 0.090 Uiso 1 1 calc R . . H22C H 0.5195 0.4909 0.1940 0.090 Uiso 1 1 calc R . . C23 C 0.3266(7) 0.4713(5) 0.1164(3) 0.0693(17) Uani 1 1 d . . . H23A H 0.3180 0.5284 0.1418 0.104 Uiso 1 1 calc R . . H23B H 0.2550 0.4346 0.0816 0.104 Uiso 1 1 calc R . . H23C H 0.4015 0.4960 0.0992 0.104 Uiso 1 1 calc R . . C24 C 0.3933(6) 0.2295(5) -0.0496(2) 0.0650(16) Uani 1 1 d . . . C25 C 0.3631(8) 0.3101(5) -0.0714(3) 0.086(2) Uani 1 1 d . . . H25A H 0.4173 0.3763 -0.0437 0.129 Uiso 1 1 calc R . . H25B H 0.2773 0.2963 -0.0698 0.129 Uiso 1 1 calc R . . H25C H 0.3752 0.3096 -0.1148 0.129 Uiso 1 1 calc R . . C26 C 0.5278(7) 0.2474(7) -0.0568(3) 0.094(2) Uani 1 1 d . . . H26A H 0.5862 0.3124 -0.0292 0.141 Uiso 1 1 calc R . . H26B H 0.5354 0.2474 -0.1007 0.141 Uiso 1 1 calc R . . H26C H 0.5459 0.1934 -0.0450 0.141 Uiso 1 1 calc R . . C27 C 0.3065(7) 0.1270(5) -0.0901(3) 0.0764(18) Uani 1 1 d . . . H27A H 0.3157 0.1238 -0.1340 0.115 Uiso 1 1 calc R . . H27B H 0.2217 0.1152 -0.0871 0.115 Uiso 1 1 calc R . . H27C H 0.3256 0.0754 -0.0754 0.115 Uiso 1 1 calc R . . C28 C 0.4617(6) 0.0977(5) 0.1381(2) 0.0574(15) Uani 1 1 d . . . C29 C 0.5800(6) 0.1639(6) 0.1887(3) 0.081(2) Uani 1 1 d . . . H29A H 0.6443 0.2045 0.1688 0.121 Uiso 1 1 calc R . . H29B H 0.6080 0.1206 0.2085 0.121 Uiso 1 1 calc R . . H29C H 0.5624 0.2084 0.2208 0.121 Uiso 1 1 calc R . . C30 C 0.4973(7) 0.0355(6) 0.0863(3) 0.082(2) Uani 1 1 d U . . H30A H 0.5620 0.0812 0.0688 0.124 Uiso 1 1 calc R . . H30B H 0.4251 -0.0060 0.0526 0.124 Uiso 1 1 calc R . . H30C H 0.5275 -0.0080 0.1045 0.124 Uiso 1 1 calc R . . C31 C 0.3672(7) 0.0218(5) 0.1647(3) 0.0709(19) Uani 1 1 d . . . H31A H 0.4002 -0.0236 0.1780 0.106 Uiso 1 1 calc R . . H31B H 0.2922 -0.0173 0.1322 0.106 Uiso 1 1 calc R . . H31C H 0.3478 0.0573 0.2010 0.106 Uiso 1 1 calc R . . C32 C 0.0603(3) -0.1482(3) 0.37231(18) 0.0258(8) Uani 1 1 d . . . C33 C -0.0244(3) -0.2314(3) 0.32364(18) 0.0310(8) Uani 1 1 d . . . C34 C -0.0055(4) -0.3188(3) 0.3121(2) 0.0356(9) Uani 1 1 d . . . H34 H -0.0618 -0.3745 0.2793 0.043 Uiso 1 1 calc R . . C35 C 0.0903(4) -0.3287(3) 0.3456(2) 0.0329(9) Uani 1 1 d . . . C36 C 0.1660(4) -0.2494(3) 0.39586(19) 0.0320(9) Uani 1 1 d . . . H36 H 0.2306 -0.2563 0.4206 0.038 Uiso 1 1 calc R . . C37 C 0.1527(3) -0.1596(3) 0.41228(17) 0.0267(8) Uani 1 1 d . . . C38 C -0.1367(4) -0.2309(3) 0.2823(2) 0.0409(10) Uani 1 1 d . . . C39 C -0.2098(4) -0.1896(5) 0.3219(3) 0.0581(14) Uani 1 1 d . . . H39A H -0.2464 -0.2350 0.3486 0.087 Uiso 1 1 calc R . . H39B H -0.2751 -0.1845 0.2941 0.087 Uiso 1 1 calc R . . H39C H -0.1548 -0.1227 0.3486 0.087 Uiso 1 1 calc R . . C40 C -0.0974(5) -0.1714(4) 0.2319(2) 0.0508(12) Uani 1 1 d . . . H40A H -0.1707 -0.1783 0.2039 0.076 Uiso 1 1 calc R . . H40B H -0.0494 -0.1980 0.2073 0.076 Uiso 1 1 calc R . . H40C H -0.0472 -0.1001 0.2526 0.076 Uiso 1 1 calc R . . C41 C -0.2285(5) -0.3394(4) 0.2457(3) 0.081(2) Uani 1 1 d . . . H41A H -0.2544 -0.3814 0.2757 0.121 Uiso 1 1 calc R . . H41B H -0.1884 -0.3679 0.2166 0.121 Uiso 1 1 calc R . . H41C H -0.3006 -0.3373 0.2219 0.121 Uiso 1 1 calc R . . C42 C 0.1139(4) -0.4230(3) 0.3302(2) 0.0429(11) Uani 1 1 d . . . C43 C 0.2407(5) -0.3952(4) 0.3134(3) 0.0652(16) Uani 1 1 d . . . H43A H 0.2434 -0.3675 0.2761 0.098 Uiso 1 1 calc R . . H43B H 0.2563 -0.4555 0.3044 0.098 Uiso 1 1 calc R . . H43C H 0.3036 -0.3448 0.3489 0.098 Uiso 1 1 calc R . . C44 C 0.0193(5) -0.5034(4) 0.2741(3) 0.0633(15) Uani 1 1 d . . . H44A H 0.0240 -0.4765 0.2364 0.095 Uiso 1 1 calc R . . H44B H -0.0634 -0.5221 0.2833 0.095 Uiso 1 1 calc R . . H44C H 0.0367 -0.5629 0.2667 0.095 Uiso 1 1 calc R . . C45 C 0.1094(7) -0.4680(4) 0.3877(3) 0.0708(18) Uani 1 1 d . . . H45A H 0.1238 -0.5288 0.3778 0.106 Uiso 1 1 calc R . . H45B H 0.0284 -0.4853 0.3989 0.106 Uiso 1 1 calc R . . H45C H 0.1731 -0.4186 0.4233 0.106 Uiso 1 1 calc R . . C46 C 0.2358(3) -0.0808(3) 0.47336(18) 0.0297(8) Uani 1 1 d . . . C47 C 0.3027(4) -0.1262(4) 0.5135(2) 0.0460(11) Uani 1 1 d . . . H47A H 0.3616 -0.1411 0.4912 0.069 Uiso 1 1 calc R . . H47B H 0.2425 -0.1884 0.5208 0.069 Uiso 1 1 calc R . . H47C H 0.3465 -0.0778 0.5541 0.069 Uiso 1 1 calc R . . C48 C 0.1571(4) -0.0495(3) 0.51476(19) 0.0386(10) Uani 1 1 d . . . H48A H 0.2103 0.0002 0.5533 0.058 Uiso 1 1 calc R . . H48B H 0.0987 -0.1087 0.5258 0.058 Uiso 1 1 calc R . . H48C H 0.1119 -0.0198 0.4916 0.058 Uiso 1 1 calc R . . C49 C 0.3372(4) 0.0112(3) 0.4597(2) 0.0367(9) Uani 1 1 d . . . H49A H 0.3917 0.0558 0.4995 0.055 Uiso 1 1 calc R . . H49B H 0.2995 0.0477 0.4384 0.055 Uiso 1 1 calc R . . H49C H 0.3849 -0.0114 0.4325 0.055 Uiso 1 1 calc R . . C50 C 0.5305(4) 0.3120(3) 0.4339(2) 0.0417(10) Uani 1 1 d . . . C51 C 0.4253(4) 0.4076(3) 0.3593(2) 0.0377(9) Uani 1 1 d . . . C52 C 0.6305(4) 0.3775(4) 0.3302(3) 0.0535(13) Uani 1 1 d . . . C53 C 0.5101(3) 0.1681(3) 0.33465(19) 0.0307(8) Uani 1 1 d . . . C54 C 0.4388(6) 0.8547(5) 0.3015(4) 0.086(2) Uani 1 1 d . . . H54A H 0.3503 0.8188 0.3016 0.103 Uiso 1 1 calc R . . H54B H 0.4573 0.9262 0.3035 0.103 Uiso 1 1 calc R . . Cl3 Cl 0.52462(18) 0.84694(18) 0.36695(9) 0.1043(7) Uani 1 1 d . . . Cl4 Cl 0.4703(2) 0.8030(3) 0.23280(10) 0.1336(10) Uani 1 1 d . . . C55 C 0.7091(10) 0.4014(7) 0.1243(5) 0.127(3) Uani 1 1 d . . . H55A H 0.6248 0.3471 0.1157 0.152 Uiso 1 1 calc R . . H55B H 0.7311 0.4340 0.1700 0.152 Uiso 1 1 calc R . . Cl5 Cl 0.8074(4) 0.3477(3) 0.1077(2) 0.1929(15) Uani 1 1 d . . . Cl6 Cl 0.7074(4) 0.4875(2) 0.08403(19) 0.1785(14) Uani 1 1 d . . . C56 C 0.1009(15) 0.9372(17) 0.9939(11) 0.113(5) Uani 0.398(7) 1 d PDU A 1 H56A H 0.1054 0.9914 0.9726 0.136 Uiso 0.398(7) 1 calc PR A 1 H56B H 0.1498 0.9685 1.0374 0.136 Uiso 0.398(7) 1 calc PR A 1 Cl7 Cl 0.1500(11) 0.8710(11) 0.9589(4) 0.153(4) Uani 0.398(7) 1 d PDU A 1 Cl8 Cl -0.0460(6) 0.8657(7) 0.9956(4) 0.152(4) Uani 0.398(7) 1 d PDU A 1 C57 C 0.180(3) -0.325(2) 0.1104(15) 0.201(8) Uani 0.396(6) 1 d PDU B 2 H57A H 0.2103 -0.2729 0.0865 0.241 Uiso 0.396(6) 1 calc PR B 2 H57B H 0.2521 -0.3315 0.1312 0.241 Uiso 0.396(6) 1 calc PR B 2 Cl9 Cl 0.1030(17) -0.4214(14) 0.0640(8) 0.312(8) Uani 0.396(6) 1 d PDU B 2 Cl10 Cl 0.1240(7) -0.2830(7) 0.1640(4) 0.154(4) Uani 0.396(6) 1 d PDU B 2 C58 C 0.107(3) 0.904(2) 1.0222(19) 0.110(6) Uani 0.206(7) 1 d PDU C 3 H58A H 0.0791 0.9437 0.9977 0.132 Uiso 0.206(7) 1 calc PR C 3 H58B H 0.1622 0.9528 1.0615 0.132 Uiso 0.206(7) 1 calc PR C 3 Cl11 Cl 0.1908(14) 0.8718(14) 0.9846(8) 0.109(5) Uani 0.206(7) 1 d PDU C 3 Cl12 Cl -0.0183(11) 0.8278(14) 1.0446(8) 0.149(6) Uani 0.206(7) 1 d PDU C 3 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 W1 0.02051(8) 0.02611(9) 0.03390(10) 0.00900(6) 0.00480(6) 0.00975(6) P1 0.0298(5) 0.0339(5) 0.0279(5) 0.0138(4) 0.0119(4) 0.0183(4) C1 0.0265(18) 0.0266(19) 0.0238(18) 0.0067(15) 0.0042(14) 0.0133(15) Cl1 0.0398(5) 0.0501(6) 0.0255(5) 0.0005(4) -0.0006(4) 0.0173(5) Ge1 0.01998(17) 0.02179(19) 0.02044(18) 0.00514(15) 0.00426(13) 0.00962(14) P2 0.0267(5) 0.0254(5) 0.0280(5) 0.0097(4) 0.0086(4) 0.0136(4) Cl2 0.0420(5) 0.0295(5) 0.0420(6) 0.0100(4) 0.0204(4) 0.0207(4) N1 0.0246(15) 0.0229(16) 0.0320(17) 0.0079(13) 0.0073(12) 0.0121(12) N2 0.0251(15) 0.0208(15) 0.0256(16) 0.0033(12) 0.0082(12) 0.0079(12) O1 0.087(3) 0.080(3) 0.041(2) 0.0000(19) -0.0202(19) 0.042(2) O2 0.099(3) 0.061(2) 0.064(2) 0.0084(19) 0.010(2) 0.060(2) O3 0.043(2) 0.073(3) 0.181(5) 0.070(3) 0.047(3) 0.0229(19) O4 0.0381(16) 0.0410(18) 0.058(2) 0.0164(15) 0.0047(14) 0.0242(14) C2 0.0220(16) 0.0201(18) 0.0271(19) 0.0078(15) 0.0060(14) 0.0077(13) C3 0.0308(19) 0.027(2) 0.040(2) 0.0131(17) 0.0155(17) 0.0173(16) C4 0.038(2) 0.025(2) 0.036(2) 0.0108(17) 0.0200(17) 0.0171(16) C5 0.042(2) 0.054(3) 0.060(3) 0.015(2) 0.019(2) 0.034(2) C6 0.057(3) 0.042(3) 0.044(3) 0.008(2) 0.025(2) 0.029(2) C7 0.0260(18) 0.031(2) 0.033(2) 0.0047(17) -0.0001(15) 0.0131(16) C8 0.032(2) 0.032(2) 0.058(3) 0.004(2) 0.003(2) 0.0054(18) C9 0.045(2) 0.056(3) 0.039(2) 0.017(2) 0.0055(19) 0.026(2) C10 0.033(2) 0.041(2) 0.026(2) -0.0026(17) 0.0037(16) 0.0154(18) C11 0.067(3) 0.066(3) 0.034(2) 0.014(2) 0.004(2) 0.037(3) C12 0.048(3) 0.053(3) 0.047(3) -0.012(2) 0.005(2) 0.005(2) C13 0.0236(17) 0.0215(18) 0.0239(18) 0.0032(14) 0.0025(13) 0.0124(14) C14 0.035(2) 0.043(2) 0.029(2) 0.0182(18) 0.0134(16) 0.0214(18) C15 0.035(2) 0.034(2) 0.038(2) 0.0146(18) 0.0095(17) 0.0147(17) C16 0.060(3) 0.041(3) 0.036(2) 0.017(2) 0.004(2) 0.023(2) C17 0.060(3) 0.052(3) 0.033(2) 0.013(2) 0.004(2) 0.025(2) C18 0.065(3) 0.055(3) 0.034(2) 0.016(2) 0.018(2) 0.034(2) C19 0.049(3) 0.053(3) 0.032(2) 0.021(2) 0.0192(19) 0.032(2) C20 0.053(3) 0.036(2) 0.047(3) 0.022(2) 0.020(2) 0.024(2) C21 0.066(3) 0.055(3) 0.084(4) 0.027(3) 0.037(3) 0.040(3) C22 0.077(4) 0.038(3) 0.058(3) 0.012(2) 0.011(3) 0.018(3) C23 0.112(5) 0.063(4) 0.067(4) 0.036(3) 0.037(4) 0.059(4) C24 0.096(5) 0.070(4) 0.034(3) 0.020(3) 0.009(3) 0.038(3) C25 0.148(7) 0.086(5) 0.032(3) 0.025(3) 0.011(3) 0.055(5) C26 0.103(6) 0.135(7) 0.053(4) 0.033(4) 0.040(4) 0.048(5) C27 0.107(5) 0.084(5) 0.039(3) 0.008(3) 0.000(3) 0.049(4) C28 0.091(4) 0.092(4) 0.042(3) 0.036(3) 0.039(3) 0.078(4) C29 0.082(4) 0.155(7) 0.059(4) 0.051(4) 0.029(3) 0.091(5) C30 0.131(5) 0.115(5) 0.065(4) 0.039(3) 0.053(4) 0.100(4) C31 0.122(5) 0.074(4) 0.074(4) 0.046(3) 0.058(4) 0.078(4) C32 0.0244(17) 0.0259(19) 0.033(2) 0.0133(16) 0.0107(15) 0.0126(14) C33 0.0290(19) 0.032(2) 0.029(2) 0.0105(17) 0.0034(15) 0.0097(16) C34 0.037(2) 0.026(2) 0.036(2) 0.0032(17) 0.0029(17) 0.0095(17) C35 0.039(2) 0.025(2) 0.042(2) 0.0147(18) 0.0185(18) 0.0154(17) C36 0.031(2) 0.035(2) 0.039(2) 0.0167(18) 0.0084(16) 0.0191(17) C37 0.0265(18) 0.027(2) 0.0276(19) 0.0108(16) 0.0068(15) 0.0104(15) C38 0.033(2) 0.032(2) 0.046(3) 0.0133(19) -0.0076(18) 0.0047(17) C39 0.030(2) 0.083(4) 0.066(3) 0.035(3) 0.005(2) 0.023(2) C40 0.053(3) 0.053(3) 0.038(3) 0.016(2) -0.006(2) 0.016(2) C41 0.057(3) 0.042(3) 0.107(5) 0.017(3) -0.041(3) -0.002(2) C42 0.046(2) 0.030(2) 0.062(3) 0.015(2) 0.024(2) 0.0206(19) C43 0.062(3) 0.050(3) 0.100(5) 0.018(3) 0.038(3) 0.036(3) C44 0.068(4) 0.035(3) 0.082(4) -0.003(3) 0.025(3) 0.022(2) C45 0.116(5) 0.048(3) 0.081(4) 0.036(3) 0.045(4) 0.054(4) C46 0.0308(19) 0.029(2) 0.029(2) 0.0092(16) 0.0017(15) 0.0120(16) C47 0.046(3) 0.049(3) 0.042(3) 0.015(2) -0.006(2) 0.021(2) C48 0.043(2) 0.042(3) 0.029(2) 0.0083(18) 0.0061(17) 0.0160(19) C49 0.0266(19) 0.039(2) 0.037(2) 0.0110(19) 0.0002(16) 0.0064(17) C50 0.044(2) 0.035(2) 0.045(3) 0.004(2) -0.003(2) 0.0218(19) C51 0.040(2) 0.039(2) 0.034(2) 0.0062(19) 0.0006(18) 0.0202(19) C52 0.028(2) 0.046(3) 0.100(4) 0.036(3) 0.020(2) 0.019(2) C53 0.0214(17) 0.036(2) 0.034(2) 0.0119(17) 0.0048(15) 0.0103(16) C54 0.071(4) 0.051(4) 0.142(7) 0.023(4) 0.017(4) 0.032(3) Cl3 0.0742(11) 0.1384(18) 0.0662(11) -0.0176(11) 0.0002(8) 0.0319(11) Cl4 0.1166(18) 0.216(3) 0.0677(12) 0.0373(15) 0.0147(12) 0.0694(19) C55 0.143(9) 0.086(6) 0.166(10) 0.027(6) 0.062(7) 0.055(6) Cl5 0.165(3) 0.205(4) 0.252(4) 0.093(3) 0.072(3) 0.098(3) Cl6 0.217(4) 0.112(2) 0.204(4) 0.040(2) 0.042(3) 0.067(2) C56 0.064(7) 0.156(10) 0.116(10) 0.053(8) -0.009(7) 0.042(7) Cl7 0.142(7) 0.199(7) 0.095(6) 0.049(6) 0.034(5) 0.039(6) Cl8 0.083(4) 0.218(8) 0.120(5) 0.039(5) -0.001(3) 0.036(4) C57 0.186(13) 0.223(13) 0.201(13) -0.002(10) 0.014(9) 0.124(10) Cl9 0.298(13) 0.289(12) 0.280(12) -0.064(9) -0.008(10) 0.129(10) Cl10 0.134(6) 0.189(8) 0.139(6) 0.018(5) 0.017(4) 0.080(5) C58 0.067(8) 0.160(10) 0.111(10) 0.025(9) 0.009(7) 0.064(7) Cl11 0.094(8) 0.123(8) 0.117(11) 0.011(8) 0.035(7) 0.059(6) Cl12 0.087(7) 0.226(12) 0.136(10) 0.037(9) 0.030(6) 0.068(7) _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 W1 C52 1.965(4) . ? W1 C50 1.983(5) . ? W1 C53 2.025(4) . ? W1 C51 2.027(4) . ? W1 P1 2.4952(10) . ? W1 Ge1 2.6508(4) . ? P1 C1 1.674(4) . ? P1 C14 1.851(4) . ? C1 Cl1 1.736(4) . ? C1 Ge1 2.010(4) . ? Ge1 C13 1.970(4) . ? Ge1 C2 2.042(3) . ? P2 C13 1.672(4) . ? P2 C32 1.847(4) . ? Cl2 C13 1.746(3) . ? N1 C2 1.349(4) . ? N1 C3 1.391(5) . ? N1 C7 1.482(5) . ? N2 C2 1.350(5) . ? N2 C4 1.392(5) . ? N2 C10 1.478(5) . ? O1 C50 1.148(5) . ? O2 C51 1.138(5) . ? O3 C52 1.157(6) . ? O4 C53 1.148(5) . ? C3 C4 1.345(6) . ? C3 C5 1.495(5) . ? C4 C6 1.495(6) . ? C7 C9 1.506(6) . ? C7 C8 1.525(6) . ? C10 C11 1.520(7) . ? C10 C12 1.527(6) . ? C14 C15 1.410(6) . ? C14 C19 1.430(6) . ? C15 C16 1.399(6) . ? C15 C20 1.556(6) . ? C16 C17 1.385(7) . ? C17 C18 1.383(7) . ? C17 C24 1.539(7) . ? C18 C19 1.392(6) . ? C19 C28 1.549(6) . ? C20 C21 1.521(7) . ? C20 C22 1.525(7) . ? C20 C23 1.545(6) . ? C24 C27 1.506(9) . ? C24 C25 1.522(8) . ? C24 C26 1.570(9) . ? C28 C31 1.514(8) . ? C28 C30 1.545(7) . ? C28 C29 1.548(9) . ? C32 C33 1.419(5) . ? C32 C37 1.425(5) . ? C33 C34 1.393(6) . ? C33 C38 1.551(5) . ? C34 C35 1.373(6) . ? C35 C36 1.383(6) . ? C35 C42 1.530(6) . ? C36 C37 1.398(5) . ? C37 C46 1.549(5) . ? C38 C39 1.524(7) . ? C38 C40 1.540(6) . ? C38 C41 1.554(6) . ? C42 C43 1.527(7) . ? C42 C45 1.529(7) . ? C42 C44 1.531(7) . ? C46 C48 1.530(6) . ? C46 C49 1.540(5) . ? C46 C47 1.541(5) . ? C54 Cl4 1.722(8) . ? C54 Cl3 1.726(8) . ? C55 Cl6 1.689(10) . ? C55 Cl5 1.711(9) . ? C56 Cl7 1.486(19) . ? C56 Cl8 1.680(18) . ? C57 Cl9 1.48(2) . ? C57 Cl10 1.57(2) . ? C58 Cl11 1.54(2) . ? C58 Cl12 1.69(2) . ? 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 C52 W1 C50 92.2(2) . . ? C52 W1 C53 93.26(17) . . ? C50 W1 C53 84.20(17) . . ? C52 W1 C51 89.36(19) . . ? C50 W1 C51 90.63(17) . . ? C53 W1 C51 174.28(16) . . ? C52 W1 P1 98.01(18) . . ? C50 W1 P1 169.52(14) . . ? C53 W1 P1 92.90(11) . . ? C51 W1 P1 91.76(12) . . ? C52 W1 Ge1 164.21(17) . . ? C50 W1 Ge1 103.46(14) . . ? C53 W1 Ge1 90.24(10) . . ? C51 W1 Ge1 88.59(13) . . ? P1 W1 Ge1 66.42(2) . . ? C1 P1 C14 112.61(19) . . ? C1 P1 W1 104.07(13) . . ? C14 P1 W1 143.19(14) . . ? P1 C1 Cl1 125.6(2) . . ? P1 C1 Ge1 99.56(17) . . ? Cl1 C1 Ge1 134.0(2) . . ? C13 Ge1 C1 104.09(15) . . ? C13 Ge1 C2 100.57(14) . . ? C1 Ge1 C2 112.45(14) . . ? C13 Ge1 W1 126.53(10) . . ? C1 Ge1 W1 89.94(10) . . ? C2 Ge1 W1 121.33(10) . . ? C13 P2 C32 102.78(16) . . ? C2 N1 C3 109.9(3) . . ? C2 N1 C7 123.2(3) . . ? C3 N1 C7 126.6(3) . . ? C2 N2 C4 109.8(3) . . ? C2 N2 C10 123.2(3) . . ? C4 N2 C10 126.7(3) . . ? N1 C2 N2 106.3(3) . . ? N1 C2 Ge1 129.4(3) . . ? N2 C2 Ge1 124.1(2) . . ? C4 C3 N1 107.0(3) . . ? C4 C3 C5 128.2(4) . . ? N1 C3 C5 124.8(4) . . ? C3 C4 N2 107.0(3) . . ? C3 C4 C6 128.2(4) . . ? N2 C4 C6 124.8(4) . . ? N1 C7 C9 112.1(3) . . ? N1 C7 C8 111.0(3) . . ? C9 C7 C8 113.8(3) . . ? N2 C10 C11 110.5(3) . . ? N2 C10 C12 113.0(4) . . ? C11 C10 C12 112.5(4) . . ? P2 C13 Cl2 123.5(2) . . ? P2 C13 Ge1 125.76(19) . . ? Cl2 C13 Ge1 110.40(18) . . ? C15 C14 C19 119.6(4) . . ? C15 C14 P1 119.8(3) . . ? C19 C14 P1 120.5(3) . . ? C16 C15 C14 117.9(4) . . ? C16 C15 C20 116.5(4) . . ? C14 C15 C20 125.4(4) . . ? C17 C16 C15 124.1(4) . . ? C18 C17 C16 116.5(4) . . ? C18 C17 C24 119.3(5) . . ? C16 C17 C24 124.1(4) . . ? C17 C18 C19 123.6(4) . . ? C18 C19 C14 118.2(4) . . ? C18 C19 C28 116.2(4) . . ? C14 C19 C28 125.4(4) . . ? C21 C20 C22 111.7(4) . . ? C21 C20 C23 105.9(4) . . ? C22 C20 C23 105.6(4) . . ? C21 C20 C15 111.5(4) . . ? C22 C20 C15 109.3(4) . . ? C23 C20 C15 112.6(4) . . ? C27 C24 C25 109.9(5) . . ? C27 C24 C17 109.6(5) . . ? C25 C24 C17 110.8(5) . . ? C27 C24 C26 108.2(6) . . ? C25 C24 C26 109.4(6) . . ? C17 C24 C26 108.9(5) . . ? C31 C28 C30 105.9(5) . . ? C31 C28 C29 111.1(5) . . ? C30 C28 C29 107.1(5) . . ? C31 C28 C19 112.4(4) . . ? C30 C28 C19 112.1(4) . . ? C29 C28 C19 108.2(5) . . ? C33 C32 C37 119.7(3) . . ? C33 C32 P2 120.9(3) . . ? C37 C32 P2 119.1(3) . . ? C34 C33 C32 118.2(4) . . ? C34 C33 C38 117.9(4) . . ? C32 C33 C38 123.9(4) . . ? C35 C34 C33 123.4(4) . . ? C34 C35 C36 117.3(4) . . ? C34 C35 C42 122.9(4) . . ? C36 C35 C42 119.8(4) . . ? C35 C36 C37 123.6(4) . . ? C36 C37 C32 117.3(3) . . ? C36 C37 C46 118.3(3) . . ? C32 C37 C46 124.3(3) . . ? C39 C38 C40 110.4(4) . . ? C39 C38 C33 111.9(4) . . ? C40 C38 C33 111.3(4) . . ? C39 C38 C41 105.8(5) . . ? C40 C38 C41 106.1(4) . . ? C33 C38 C41 111.1(4) . . ? C43 C42 C45 109.3(5) . . ? C43 C42 C35 109.6(4) . . ? C45 C42 C35 109.4(4) . . ? C43 C42 C44 107.5(4) . . ? C45 C42 C44 108.7(4) . . ? C35 C42 C44 112.3(4) . . ? C48 C46 C49 111.5(3) . . ? C48 C46 C47 105.6(3) . . ? C49 C46 C47 106.1(3) . . ? C48 C46 C37 110.0(3) . . ? C49 C46 C37 112.4(3) . . ? C47 C46 C37 111.0(3) . . ? O1 C50 W1 179.0(4) . . ? O2 C51 W1 177.8(4) . . ? O3 C52 W1 178.1(5) . . ? O4 C53 W1 175.2(4) . . ? Cl4 C54 Cl3 111.3(4) . . ? Cl6 C55 Cl5 115.8(6) . . ? Cl7 C56 Cl8 107.9(14) . . ? Cl9 C57 Cl10 120(2) . . ? Cl11 C58 Cl12 126(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.226 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.097 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 857222' #TrackingRef 'KT-chemcomm-2011.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51.50 H83 Au Cl8 Ge N2 P2' _chemical_formula_weight 1345.30 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Au Au -2.0133 8.8022 '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 11.3212(6) _cell_length_b 15.4945(7) _cell_length_c 18.5887(10) _cell_angle_alpha 79.533(2) _cell_angle_beta 87.667(2) _cell_angle_gamma 77.006(2) _cell_volume 3124.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.02 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1366 _exptl_absorpt_coefficient_mu 3.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5974 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65805 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 28.28 _reflns_number_total 15160 _reflns_number_gt 12211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0325P)^2^+2.9608P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15160 _refine_ls_number_parameters 706 _refine_ls_number_restraints 230 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.015 _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 Au1 Au -0.117806(11) 0.307106(8) 0.150123(7) 0.03648(5) Uani 1 1 d . . . Cl1 Cl -0.32358(8) 0.31844(8) 0.16865(6) 0.0601(3) Uani 1 1 d . . . Ge1 Ge 0.08955(3) 0.303022(19) 0.132720(17) 0.02960(7) Uani 1 1 d . . . P1 P 0.17823(8) 0.38588(5) 0.25471(5) 0.03770(19) Uani 1 1 d . . . P2 P 0.14085(7) 0.10528(5) 0.21102(5) 0.03445(18) Uani 1 1 d . . . Cl2 Cl 0.05629(8) 0.51082(5) 0.11879(5) 0.0488(2) Uani 1 1 d . . . Cl3 Cl 0.35214(7) 0.19851(5) 0.19521(5) 0.04016(18) Uani 1 1 d . . . N1 N 0.2327(2) 0.34111(17) -0.00931(14) 0.0338(6) Uani 1 1 d . . . N2 N 0.0910(2) 0.27167(17) -0.02218(15) 0.0372(6) Uani 1 1 d . . . C1 C 0.1237(3) 0.40596(19) 0.17002(18) 0.0336(7) Uani 1 1 d . . . C2 C 0.2016(3) 0.19444(19) 0.18369(16) 0.0301(6) Uani 1 1 d . . . C3 C 0.1441(3) 0.30596(19) 0.02703(17) 0.0325(6) Uani 1 1 d . . . C4 C 0.2359(3) 0.3296(2) -0.08212(19) 0.0429(8) Uani 1 1 d . . . C5 C 0.1472(3) 0.2868(2) -0.08974(19) 0.0438(8) Uani 1 1 d . . . C6 C 0.3208(4) 0.3613(4) -0.1388(2) 0.0654(12) Uani 1 1 d . . . H6A H 0.3082 0.3419 -0.1847 0.098 Uiso 1 1 calc R . . H6B H 0.4045 0.3358 -0.1223 0.098 Uiso 1 1 calc R . . H6C H 0.3056 0.4271 -0.1469 0.098 Uiso 1 1 calc R . . C7 C 0.1095(4) 0.2622(3) -0.1586(2) 0.0644(11) Uani 1 1 d . . . H7A H 0.1229 0.1965 -0.1529 0.097 Uiso 1 1 calc R . . H7B H 0.1577 0.2847 -0.1998 0.097 Uiso 1 1 calc R . . H7C H 0.0234 0.2892 -0.1680 0.097 Uiso 1 1 calc R . . C8 C 0.3184(3) 0.3819(2) 0.02487(19) 0.0427(8) Uani 1 1 d . . . H8 H 0.2924 0.3821 0.0769 0.051 Uiso 1 1 calc R . . C9 C 0.3091(5) 0.4793(3) -0.0107(2) 0.0650(12) Uani 1 1 d . . . H9A H 0.3483 0.4818 -0.0588 0.097 Uiso 1 1 calc R . . H9B H 0.3495 0.5089 0.0202 0.097 Uiso 1 1 calc R . . H9C H 0.2236 0.5102 -0.0166 0.097 Uiso 1 1 calc R . . C10 C 0.4460(3) 0.3250(4) 0.0265(2) 0.0664(12) Uani 1 1 d . . . H10A H 0.4438 0.2613 0.0408 0.100 Uiso 1 1 calc R . . H10B H 0.4946 0.3419 0.0619 0.100 Uiso 1 1 calc R . . H10C H 0.4824 0.3349 -0.0222 0.100 Uiso 1 1 calc R . . C11 C -0.0058(3) 0.2203(2) -0.0038(2) 0.0424(8) Uani 1 1 d . . . H11 H -0.0185 0.2148 0.0503 0.051 Uiso 1 1 calc R . . C12 C -0.1256(3) 0.2703(3) -0.0388(3) 0.0567(10) Uani 1 1 d . . . H12A H -0.1474 0.3306 -0.0262 0.085 Uiso 1 1 calc R . . H12B H -0.1885 0.2374 -0.0210 0.085 Uiso 1 1 calc R . . H12C H -0.1187 0.2754 -0.0921 0.085 Uiso 1 1 calc R . . C13 C 0.0344(4) 0.1249(2) -0.0188(3) 0.0606(11) Uani 1 1 d . . . H13A H 0.0249 0.1251 -0.0710 0.091 Uiso 1 1 calc R . . H13B H -0.0155 0.0869 0.0098 0.091 Uiso 1 1 calc R . . H13C H 0.1197 0.1011 -0.0049 0.091 Uiso 1 1 calc R . . C14 C 0.1540(3) 0.4940(2) 0.28753(18) 0.0359(7) Uani 1 1 d . . . C15 C 0.0448(3) 0.5257(2) 0.32430(19) 0.0394(7) Uani 1 1 d . . . C16 C 0.0274(3) 0.6106(2) 0.34402(19) 0.0381(7) Uani 1 1 d . . . H16 H -0.0470 0.6334 0.3666 0.046 Uiso 1 1 calc R . . C17 C 0.1126(3) 0.6630(2) 0.33238(18) 0.0356(7) Uani 1 1 d . A . C18 C 0.2214(3) 0.6270(2) 0.30173(19) 0.0407(8) Uani 1 1 d . . . H18 H 0.2822 0.6612 0.2949 0.049 Uiso 1 1 calc R . . C19 C 0.2470(3) 0.5431(2) 0.28029(19) 0.0390(7) Uani 1 1 d . . . C20 C -0.0542(3) 0.4712(2) 0.3481(2) 0.0495(9) Uani 1 1 d . . . C21 C 0.0021(5) 0.3781(3) 0.3889(4) 0.0963(19) Uani 1 1 d . . . H21A H 0.0577 0.3829 0.4263 0.145 Uiso 1 1 calc R . . H21B H 0.0470 0.3418 0.3545 0.145 Uiso 1 1 calc R . . H21C H -0.0618 0.3494 0.4123 0.145 Uiso 1 1 calc R . . C22 C -0.1258(4) 0.4636(4) 0.2831(3) 0.0878(17) Uani 1 1 d . . . H22A H -0.0722 0.4283 0.2512 0.132 Uiso 1 1 calc R . . H22B H -0.1595 0.5239 0.2557 0.132 Uiso 1 1 calc R . . H22C H -0.1920 0.4338 0.3004 0.132 Uiso 1 1 calc R . . C23 C -0.1426(5) 0.5113(4) 0.4032(3) 0.0946(17) Uani 1 1 d U . . H23A H -0.1953 0.4700 0.4219 0.142 Uiso 1 1 calc R . . H23B H -0.1921 0.5690 0.3794 0.142 Uiso 1 1 calc R . . H23C H -0.0975 0.5209 0.4438 0.142 Uiso 1 1 calc R . . C24 C 0.0901(3) 0.7552(2) 0.35586(19) 0.0411(7) Uani 1 1 d DU . . C25 C 0.0050(8) 0.8259(4) 0.2996(4) 0.061(2) Uani 0.596(8) 1 d PDU A 1 H25A H 0.0465 0.8341 0.2524 0.091 Uiso 0.596(8) 1 calc PR A 1 H25B H -0.0163 0.8834 0.3172 0.091 Uiso 0.596(8) 1 calc PR A 1 H25C H -0.0689 0.8049 0.2938 0.091 Uiso 0.596(8) 1 calc PR A 1 C26 C 0.0290(9) 0.7525(5) 0.4301(4) 0.066(2) Uani 0.596(8) 1 d PDU A 1 H26A H -0.0516 0.7403 0.4267 0.100 Uiso 0.596(8) 1 calc PR A 1 H26B H 0.0213 0.8106 0.4457 0.100 Uiso 0.596(8) 1 calc PR A 1 H26C H 0.0780 0.7048 0.4658 0.100 Uiso 0.596(8) 1 calc PR A 1 C27 C 0.2058(6) 0.7897(5) 0.3599(5) 0.064(2) Uani 0.596(8) 1 d PDU A 1 H27A H 0.2665 0.7431 0.3895 0.096 Uiso 0.596(8) 1 calc PR A 1 H27B H 0.1873 0.8438 0.3823 0.096 Uiso 0.596(8) 1 calc PR A 1 H27C H 0.2376 0.8044 0.3104 0.096 Uiso 0.596(8) 1 calc PR A 1 C25' C 0.1150(12) 0.8219(6) 0.2893(5) 0.062(3) Uani 0.404(8) 1 d PDU A 2 H25D H 0.1941 0.7983 0.2685 0.093 Uiso 0.404(8) 1 calc PR A 2 H25E H 0.1155 0.8795 0.3039 0.093 Uiso 0.404(8) 1 calc PR A 2 H25F H 0.0516 0.8310 0.2526 0.093 Uiso 0.404(8) 1 calc PR A 2 C26' C -0.0369(10) 0.7856(7) 0.3823(9) 0.070(4) Uani 0.404(8) 1 d PDU A 2 H26D H -0.0946 0.7823 0.3455 0.104 Uiso 0.404(8) 1 calc PR A 2 H26E H -0.0494 0.8478 0.3902 0.104 Uiso 0.404(8) 1 calc PR A 2 H26F H -0.0497 0.7466 0.4283 0.104 Uiso 0.404(8) 1 calc PR A 2 C27' C 0.1813(11) 0.7482(8) 0.4170(7) 0.066(3) Uani 0.404(8) 1 d PDU A 2 H27D H 0.1778 0.6956 0.4547 0.099 Uiso 0.404(8) 1 calc PR A 2 H27E H 0.1609 0.8027 0.4387 0.099 Uiso 0.404(8) 1 calc PR A 2 H27F H 0.2633 0.7416 0.3964 0.099 Uiso 0.404(8) 1 calc PR A 2 C28 C 0.3770(3) 0.5079(3) 0.2530(2) 0.0494(9) Uani 1 1 d . . . C29 C 0.4642(4) 0.5664(3) 0.2677(3) 0.0657(12) Uani 1 1 d . . . H29A H 0.5466 0.5397 0.2532 0.098 Uiso 1 1 calc R . . H29B H 0.4630 0.5695 0.3199 0.098 Uiso 1 1 calc R . . H29C H 0.4383 0.6272 0.2392 0.098 Uiso 1 1 calc R . . C30 C 0.4313(4) 0.4117(3) 0.2941(3) 0.0677(12) Uani 1 1 d . . . H30A H 0.3890 0.3692 0.2792 0.102 Uiso 1 1 calc R . . H30B H 0.4217 0.4101 0.3470 0.102 Uiso 1 1 calc R . . H30C H 0.5177 0.3949 0.2823 0.102 Uiso 1 1 calc R . . C31 C 0.3785(4) 0.5096(3) 0.1703(2) 0.0623(11) Uani 1 1 d . . . H31A H 0.3259 0.4716 0.1587 0.094 Uiso 1 1 calc R . . H31B H 0.4615 0.4867 0.1545 0.094 Uiso 1 1 calc R . . H31C H 0.3490 0.5715 0.1448 0.094 Uiso 1 1 calc R . . C32 C 0.2637(3) 0.01648(19) 0.25873(17) 0.0335(7) Uani 1 1 d . . . C33 C 0.2765(3) 0.0068(2) 0.33617(18) 0.0355(7) Uani 1 1 d . . . C34 C 0.3772(3) -0.0534(2) 0.36893(19) 0.0429(8) Uani 1 1 d . . . H34 H 0.3872 -0.0589 0.4202 0.051 Uiso 1 1 calc R . . C35 C 0.4642(3) -0.1061(2) 0.3314(2) 0.0442(8) Uani 1 1 d . B . C36 C 0.4449(3) -0.0998(2) 0.2573(2) 0.0432(8) Uani 1 1 d . . . H36 H 0.5020 -0.1372 0.2309 0.052 Uiso 1 1 calc R . . C37 C 0.3465(3) -0.0417(2) 0.21962(18) 0.0370(7) Uani 1 1 d . . . C38 C 0.1861(3) 0.0593(2) 0.38722(19) 0.0416(8) Uani 1 1 d . . . C39 C 0.0524(4) 0.0665(4) 0.3696(3) 0.0705(13) Uani 1 1 d . . . H39A H 0.0012 0.0882 0.4093 0.106 Uiso 1 1 calc R . . H39B H 0.0404 0.0072 0.3646 0.106 Uiso 1 1 calc R . . H39C H 0.0302 0.1089 0.3238 0.106 Uiso 1 1 calc R . . C40 C 0.2129(5) 0.1523(3) 0.3840(2) 0.0668(12) Uani 1 1 d . . . H40A H 0.1972 0.1871 0.3344 0.100 Uiso 1 1 calc R . . H40B H 0.2980 0.1457 0.3967 0.100 Uiso 1 1 calc R . . H40C H 0.1606 0.1838 0.4188 0.100 Uiso 1 1 calc R . . C41 C 0.2021(4) 0.0113(3) 0.4674(2) 0.0587(10) Uani 1 1 d . . . H41A H 0.1385 0.0417 0.4974 0.088 Uiso 1 1 calc R . . H41B H 0.2817 0.0131 0.4851 0.088 Uiso 1 1 calc R . . H41C H 0.1961 -0.0515 0.4709 0.088 Uiso 1 1 calc R . . C42 C 0.5742(4) -0.1715(3) 0.3713(2) 0.0628(11) Uani 1 1 d DU . . C43 C 0.6422(6) -0.1224(5) 0.4106(5) 0.092(2) Uani 0.825(8) 1 d PDU B 1 H43A H 0.5852 -0.0825 0.4378 0.137 Uiso 0.825(8) 1 calc PR B 1 H43B H 0.6866 -0.0866 0.3752 0.137 Uiso 0.825(8) 1 calc PR B 1 H43C H 0.6997 -0.1657 0.4448 0.137 Uiso 0.825(8) 1 calc PR B 1 C44 C 0.5284(6) -0.2446(5) 0.4281(4) 0.104(3) Uani 0.825(8) 1 d PDU B 1 H44A H 0.5968 -0.2825 0.4578 0.156 Uiso 0.825(8) 1 calc PR B 1 H44B H 0.4923 -0.2820 0.4022 0.156 Uiso 0.825(8) 1 calc PR B 1 H44C H 0.4674 -0.2151 0.4600 0.156 Uiso 0.825(8) 1 calc PR B 1 C45 C 0.6594(6) -0.2233(5) 0.3203(4) 0.080(2) Uani 0.825(8) 1 d PDU B 1 H45A H 0.7328 -0.2577 0.3470 0.119 Uiso 0.825(8) 1 calc PR B 1 H45B H 0.6814 -0.1808 0.2789 0.119 Uiso 0.825(8) 1 calc PR B 1 H45C H 0.6187 -0.2646 0.3021 0.119 Uiso 0.825(8) 1 calc PR B 1 C43' C 0.561(3) -0.174(2) 0.4532(9) 0.083(5) Uani 0.175(8) 1 d PDU B 2 H43D H 0.6204 -0.2252 0.4790 0.125 Uiso 0.175(8) 1 calc PR B 2 H43E H 0.4791 -0.1797 0.4684 0.125 Uiso 0.175(8) 1 calc PR B 2 H43F H 0.5758 -0.1179 0.4649 0.125 Uiso 0.175(8) 1 calc PR B 2 C44' C 0.671(2) -0.110(2) 0.350(2) 0.098(6) Uani 0.175(8) 1 d PDU B 2 H44D H 0.6351 -0.0484 0.3576 0.147 Uiso 0.175(8) 1 calc PR B 2 H44E H 0.6933 -0.1086 0.2982 0.147 Uiso 0.175(8) 1 calc PR B 2 H44F H 0.7433 -0.1344 0.3804 0.147 Uiso 0.175(8) 1 calc PR B 2 C45' C 0.605(3) -0.2538(16) 0.3432(19) 0.093(6) Uani 0.175(8) 1 d PDU B 2 H45D H 0.6310 -0.3043 0.3835 0.139 Uiso 0.175(8) 1 calc PR B 2 H45E H 0.6719 -0.2513 0.3079 0.139 Uiso 0.175(8) 1 calc PR B 2 H45F H 0.5347 -0.2622 0.3188 0.139 Uiso 0.175(8) 1 calc PR B 2 C46 C 0.3324(3) -0.0474(2) 0.13779(19) 0.0449(8) Uani 1 1 d . . . C47 C 0.4226(5) -0.1301(3) 0.1163(2) 0.0756(14) Uani 1 1 d . . . H47A H 0.4070 -0.1346 0.0658 0.113 Uiso 1 1 calc R . . H47B H 0.4119 -0.1849 0.1492 0.113 Uiso 1 1 calc R . . H47C H 0.5058 -0.1230 0.1204 0.113 Uiso 1 1 calc R . . C48 C 0.2054(4) -0.0606(3) 0.1236(2) 0.0601(11) Uani 1 1 d . . . H48A H 0.1975 -0.0629 0.0717 0.090 Uiso 1 1 calc R . . H48B H 0.1441 -0.0102 0.1366 0.090 Uiso 1 1 calc R . . H48C H 0.1938 -0.1171 0.1534 0.090 Uiso 1 1 calc R . . C49 C 0.3580(4) 0.0353(3) 0.0853(2) 0.0516(9) Uani 1 1 d . . . H49A H 0.4372 0.0450 0.0968 0.077 Uiso 1 1 calc R . . H49B H 0.2949 0.0885 0.0909 0.077 Uiso 1 1 calc R . . H49C H 0.3583 0.0250 0.0348 0.077 Uiso 1 1 calc R . . C50 C 0.7038(6) 0.1881(5) 0.3503(3) 0.105(2) Uani 1 1 d . . . H50A H 0.7739 0.1367 0.3504 0.126 Uiso 1 1 calc R . . H50B H 0.7033 0.2288 0.3026 0.126 Uiso 1 1 calc R . . Cl4 Cl 0.72411(18) 0.24423(13) 0.41751(9) 0.1140(5) Uani 1 1 d . . . Cl5 Cl 0.57344(17) 0.14814(16) 0.35745(12) 0.1293(7) Uani 1 1 d . . . C51 C 0.685(3) 0.078(6) 0.178(3) 0.093(4) Uani 0.354(10) 1 d PDU C 1 H51A H 0.6356 0.0494 0.2168 0.111 Uiso 0.354(10) 1 calc PR C 1 H51B H 0.6487 0.1431 0.1666 0.111 Uiso 0.354(10) 1 calc PR C 1 Cl6 Cl 0.8354(6) 0.0592(7) 0.2080(5) 0.112(2) Uani 0.354(10) 1 d PDU C 1 Cl7 Cl 0.6928(8) 0.0289(10) 0.1007(6) 0.126(3) Uani 0.354(10) 1 d PDU C 1 C51' C 0.6984(16) 0.081(3) 0.1767(14) 0.095(3) Uani 0.646(10) 1 d PDU C 2 H51C H 0.6207 0.0684 0.1973 0.114 Uiso 0.646(10) 1 calc PR C 2 H51D H 0.7002 0.1429 0.1827 0.114 Uiso 0.646(10) 1 calc PR C 2 Cl6' Cl 0.8177(4) 0.0056(5) 0.2281(3) 0.1415(17) Uani 0.646(10) 1 d PDU C 2 Cl7' Cl 0.7012(6) 0.0771(5) 0.0834(3) 0.1212(16) Uani 0.646(10) 1 d PDU C 2 Cl8 Cl -0.3577(7) 0.4589(6) 0.5372(4) 0.191(3) Uani 0.50 1 d PDU D -1 C52 C -0.4503(14) 0.450(2) 0.4745(11) 0.190(3) Uani 0.50 1 d PDU D -1 H52A H -0.4535 0.3866 0.4769 0.228 Uiso 0.50 1 calc PR D -1 H52B H -0.4216 0.4733 0.4252 0.228 Uiso 0.50 1 calc PR D -1 Cl9 Cl -0.5901(7) 0.5121(9) 0.4903(6) 0.256(5) Uani 0.50 1 d PDU D -1 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 Au1 0.02990(7) 0.03721(7) 0.04201(8) -0.00713(5) -0.00097(5) -0.00648(5) Cl1 0.0297(4) 0.0842(7) 0.0603(6) -0.0053(5) 0.0026(4) -0.0066(4) Ge1 0.03005(16) 0.02536(14) 0.03422(18) -0.00599(12) -0.00127(13) -0.00708(12) P1 0.0449(5) 0.0300(4) 0.0409(5) -0.0127(3) 0.0017(4) -0.0091(3) P2 0.0360(4) 0.0291(4) 0.0392(5) -0.0043(3) -0.0030(4) -0.0100(3) Cl2 0.0543(5) 0.0279(4) 0.0616(6) -0.0027(4) -0.0061(4) -0.0065(3) Cl3 0.0313(4) 0.0376(4) 0.0527(5) -0.0087(4) -0.0039(3) -0.0087(3) N1 0.0319(14) 0.0363(13) 0.0319(14) -0.0062(11) -0.0007(11) -0.0047(11) N2 0.0404(15) 0.0330(13) 0.0390(16) -0.0111(12) -0.0046(12) -0.0056(11) C1 0.0337(16) 0.0260(14) 0.0424(18) -0.0081(13) 0.0018(13) -0.0084(12) C2 0.0322(15) 0.0283(14) 0.0318(16) -0.0093(12) -0.0019(12) -0.0073(12) C3 0.0332(16) 0.0275(14) 0.0352(17) -0.0047(12) -0.0057(13) -0.0031(12) C4 0.0387(18) 0.052(2) 0.0354(18) -0.0110(15) -0.0012(14) -0.0024(15) C5 0.047(2) 0.0482(19) 0.0344(18) -0.0123(15) -0.0041(15) -0.0029(16) C6 0.057(3) 0.103(4) 0.040(2) -0.017(2) 0.0089(19) -0.023(2) C7 0.076(3) 0.084(3) 0.041(2) -0.024(2) -0.003(2) -0.022(2) C8 0.0407(19) 0.056(2) 0.0364(19) -0.0056(16) 0.0008(15) -0.0220(16) C9 0.094(3) 0.061(3) 0.049(2) -0.009(2) 0.014(2) -0.041(2) C10 0.039(2) 0.108(4) 0.053(2) -0.010(2) -0.0038(18) -0.019(2) C11 0.047(2) 0.0396(17) 0.046(2) -0.0111(15) -0.0051(16) -0.0180(15) C12 0.043(2) 0.050(2) 0.078(3) -0.012(2) -0.0066(19) -0.0118(17) C13 0.067(3) 0.0396(19) 0.079(3) -0.0170(19) -0.022(2) -0.0107(18) C14 0.0360(17) 0.0328(15) 0.0432(19) -0.0160(14) 0.0051(14) -0.0100(13) C15 0.0379(18) 0.0357(16) 0.050(2) -0.0147(15) 0.0049(15) -0.0146(14) C16 0.0335(17) 0.0358(16) 0.048(2) -0.0160(15) 0.0058(14) -0.0088(13) C17 0.0383(17) 0.0347(16) 0.0374(18) -0.0126(14) 0.0017(14) -0.0107(13) C18 0.0395(18) 0.0424(18) 0.048(2) -0.0151(15) 0.0032(15) -0.0203(15) C19 0.0363(17) 0.0431(17) 0.0421(19) -0.0151(15) 0.0079(14) -0.0136(14) C20 0.045(2) 0.0456(19) 0.069(3) -0.0262(18) 0.0207(18) -0.0240(16) C21 0.088(4) 0.073(3) 0.120(5) 0.017(3) 0.031(3) -0.035(3) C22 0.055(3) 0.119(4) 0.107(4) -0.024(3) 0.003(3) -0.053(3) C23 0.091(3) 0.094(3) 0.122(4) -0.049(3) 0.052(3) -0.053(3) C24 0.0471(19) 0.0332(16) 0.048(2) -0.0139(14) -0.0003(15) -0.0138(14) C25 0.077(5) 0.038(3) 0.065(4) -0.011(3) -0.011(4) -0.002(3) C26 0.098(7) 0.058(4) 0.054(4) -0.034(4) 0.016(4) -0.025(4) C27 0.068(4) 0.042(4) 0.096(7) -0.033(4) -0.005(4) -0.024(3) C25' 0.090(9) 0.035(5) 0.062(6) -0.008(4) 0.008(5) -0.019(5) C26' 0.068(6) 0.041(5) 0.107(11) -0.031(6) 0.024(6) -0.019(5) C27' 0.087(7) 0.059(6) 0.066(7) -0.032(5) -0.014(6) -0.027(6) C28 0.0351(18) 0.062(2) 0.060(2) -0.0288(19) 0.0124(17) -0.0163(16) C29 0.041(2) 0.088(3) 0.084(3) -0.042(3) 0.016(2) -0.029(2) C30 0.039(2) 0.074(3) 0.090(3) -0.031(3) 0.002(2) 0.001(2) C31 0.050(2) 0.088(3) 0.061(3) -0.034(2) 0.021(2) -0.028(2) C32 0.0381(17) 0.0271(14) 0.0368(17) -0.0063(13) -0.0013(13) -0.0100(12) C33 0.0398(17) 0.0326(15) 0.0372(18) -0.0091(13) 0.0026(14) -0.0126(13) C34 0.045(2) 0.051(2) 0.0331(18) -0.0079(15) -0.0064(15) -0.0096(16) C35 0.0381(18) 0.0491(19) 0.044(2) -0.0081(16) -0.0057(15) -0.0064(15) C36 0.0421(19) 0.0423(18) 0.044(2) -0.0125(15) 0.0001(15) -0.0040(15) C37 0.0443(18) 0.0342(16) 0.0343(17) -0.0083(13) 0.0000(14) -0.0107(14) C38 0.054(2) 0.0332(16) 0.0374(18) -0.0105(14) 0.0036(16) -0.0069(15) C39 0.053(3) 0.098(4) 0.060(3) -0.030(3) 0.014(2) -0.005(2) C40 0.108(4) 0.038(2) 0.056(3) -0.0169(18) 0.015(2) -0.016(2) C41 0.080(3) 0.048(2) 0.045(2) -0.0110(17) 0.017(2) -0.008(2) C42 0.041(2) 0.080(3) 0.059(2) -0.013(2) -0.0133(18) 0.0075(19) C43 0.063(4) 0.113(5) 0.095(5) -0.044(4) -0.044(4) 0.015(3) C44 0.071(4) 0.094(5) 0.111(5) 0.032(4) -0.019(4) 0.018(3) C45 0.050(4) 0.086(4) 0.094(5) -0.033(4) -0.020(3) 0.020(3) C43' 0.059(10) 0.101(11) 0.069(7) -0.004(8) -0.024(8) 0.019(9) C44' 0.046(10) 0.123(12) 0.110(12) 0.009(12) -0.028(10) -0.006(8) C45' 0.084(13) 0.086(10) 0.088(12) -0.013(9) -0.030(12) 0.026(10) C46 0.059(2) 0.0399(18) 0.0346(18) -0.0133(15) -0.0014(16) -0.0039(16) C47 0.110(4) 0.059(3) 0.048(2) -0.025(2) -0.010(2) 0.015(3) C48 0.080(3) 0.059(2) 0.051(2) -0.0157(19) -0.009(2) -0.030(2) C49 0.061(2) 0.058(2) 0.037(2) -0.0122(17) 0.0083(17) -0.0149(19) C50 0.105(5) 0.150(6) 0.062(3) -0.017(4) 0.003(3) -0.036(4) Cl4 0.1339(14) 0.1324(14) 0.0929(11) -0.0197(10) -0.0028(10) -0.0652(12) Cl5 0.1037(12) 0.1642(18) 0.1369(16) -0.0337(13) -0.0124(11) -0.0570(12) C51 0.085(6) 0.112(6) 0.082(5) -0.040(5) -0.017(5) -0.001(6) Cl6 0.083(3) 0.111(5) 0.140(5) -0.032(4) -0.050(3) 0.000(3) Cl7 0.088(3) 0.208(8) 0.107(6) -0.090(5) 0.000(3) -0.034(5) C51' 0.091(5) 0.110(5) 0.085(4) -0.040(4) -0.017(4) -0.001(5) Cl6' 0.123(3) 0.143(4) 0.144(3) -0.005(3) -0.035(2) -0.010(3) Cl7' 0.150(3) 0.158(4) 0.0686(18) -0.042(2) 0.0131(17) -0.045(3) Cl8 0.195(6) 0.244(6) 0.113(3) -0.016(4) 0.040(4) -0.024(4) C52 0.193(6) 0.241(6) 0.116(4) -0.019(4) 0.037(4) -0.025(5) Cl9 0.165(5) 0.324(9) 0.240(9) -0.030(7) 0.085(6) -0.005(6) _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 Au1 Cl1 2.3128(9) . ? Au1 Ge1 2.3449(3) . ? Ge1 C1 1.969(3) . ? Ge1 C2 1.974(3) . ? Ge1 C3 2.031(3) . ? P1 C1 1.665(3) . ? P1 C14 1.846(3) . ? P2 C2 1.668(3) . ? P2 C32 1.847(3) . ? Cl2 C1 1.752(3) . ? Cl3 C2 1.743(3) . ? N1 C3 1.348(4) . ? N1 C4 1.395(4) . ? N1 C8 1.489(4) . ? N2 C3 1.358(4) . ? N2 C5 1.390(4) . ? N2 C11 1.488(4) . ? C4 C5 1.347(5) . ? C4 C6 1.490(5) . ? C5 C7 1.504(5) . ? C8 C10 1.513(5) . ? C8 C9 1.515(5) . ? C11 C12 1.510(5) . ? C11 C13 1.520(5) . ? C14 C19 1.420(4) . ? C14 C15 1.421(4) . ? C15 C16 1.398(4) . ? C15 C20 1.555(4) . ? C16 C17 1.382(4) . ? C17 C18 1.380(5) . ? C17 C24 1.533(4) . ? C18 C19 1.393(4) . ? C19 C28 1.550(5) . ? C20 C21 1.512(6) . ? C20 C23 1.518(6) . ? C20 C22 1.519(6) . ? C24 C26' 1.501(10) . ? C24 C26 1.516(7) . ? C24 C25' 1.523(9) . ? C24 C27 1.531(7) . ? C24 C27' 1.539(9) . ? C24 C25 1.553(7) . ? C28 C31 1.531(6) . ? C28 C29 1.545(5) . ? C28 C30 1.548(6) . ? C32 C37 1.422(4) . ? C32 C33 1.430(5) . ? C33 C34 1.383(5) . ? C33 C38 1.561(5) . ? C34 C35 1.383(5) . ? C35 C36 1.387(5) . ? C35 C42 1.537(5) . ? C36 C37 1.387(5) . ? C37 C46 1.556(5) . ? C38 C40 1.529(5) . ? C38 C39 1.537(6) . ? C38 C41 1.538(5) . ? C42 C45' 1.432(17) . ? C42 C43 1.490(7) . ? C42 C43' 1.517(17) . ? C42 C45 1.526(7) . ? C42 C44 1.566(8) . ? C42 C44' 1.604(18) . ? C46 C48 1.536(5) . ? C46 C49 1.538(5) . ? C46 C47 1.552(5) . ? C50 Cl4 1.696(6) . ? C50 Cl5 1.716(7) . ? C51 Cl7 1.74(2) . ? C51 Cl6 1.75(2) . ? C51' Cl7' 1.745(15) . ? C51' Cl6' 1.76(2) . ? Cl8 C52 1.640(18) . ? C52 Cl9 1.700(17) . ? 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 Cl1 Au1 Ge1 177.07(3) . . ? C1 Ge1 C2 106.66(12) . . ? C1 Ge1 C3 110.53(12) . . ? C2 Ge1 C3 102.17(12) . . ? C1 Ge1 Au1 107.38(9) . . ? C2 Ge1 Au1 116.06(9) . . ? C3 Ge1 Au1 113.79(9) . . ? C1 P1 C14 108.30(15) . . ? C2 P2 C32 105.64(14) . . ? C3 N1 C4 110.2(3) . . ? C3 N1 C8 124.4(3) . . ? C4 N1 C8 125.3(3) . . ? C3 N2 C5 109.3(3) . . ? C3 N2 C11 124.3(3) . . ? C5 N2 C11 126.3(3) . . ? P1 C1 Cl2 126.91(18) . . ? P1 C1 Ge1 117.00(16) . . ? Cl2 C1 Ge1 113.87(17) . . ? P2 C2 Cl3 125.97(18) . . ? P2 C2 Ge1 115.28(16) . . ? Cl3 C2 Ge1 118.74(15) . . ? N1 C3 N2 106.3(3) . . ? N1 C3 Ge1 130.0(2) . . ? N2 C3 Ge1 123.7(2) . . ? C5 C4 N1 106.4(3) . . ? C5 C4 C6 128.3(3) . . ? N1 C4 C6 125.2(3) . . ? C4 C5 N2 107.8(3) . . ? C4 C5 C7 127.4(4) . . ? N2 C5 C7 124.8(3) . . ? N1 C8 C10 111.2(3) . . ? N1 C8 C9 111.2(3) . . ? C10 C8 C9 113.6(3) . . ? N2 C11 C12 112.3(3) . . ? N2 C11 C13 111.6(3) . . ? C12 C11 C13 113.4(3) . . ? C19 C14 C15 119.6(3) . . ? C19 C14 P1 120.4(2) . . ? C15 C14 P1 119.9(2) . . ? C16 C15 C14 117.8(3) . . ? C16 C15 C20 117.2(3) . . ? C14 C15 C20 125.0(3) . . ? C17 C16 C15 123.5(3) . . ? C18 C17 C16 117.0(3) . . ? C18 C17 C24 121.3(3) . . ? C16 C17 C24 121.7(3) . . ? C17 C18 C19 123.5(3) . . ? C18 C19 C14 118.1(3) . . ? C18 C19 C28 117.7(3) . . ? C14 C19 C28 124.2(3) . . ? C21 C20 C23 103.4(4) . . ? C21 C20 C22 109.7(4) . . ? C23 C20 C22 108.4(4) . . ? C21 C20 C15 110.6(3) . . ? C23 C20 C15 112.7(3) . . ? C22 C20 C15 111.7(3) . . ? C26' C24 C25' 109.6(7) . . ? C26 C24 C25' 140.9(6) . . ? C26' C24 C27 132.5(6) . . ? C26 C24 C27 107.9(5) . . ? C25' C24 C27 64.7(6) . . ? C26' C24 C17 113.0(5) . . ? C26 C24 C17 110.8(4) . . ? C25' C24 C17 106.8(5) . . ? C27 C24 C17 113.5(4) . . ? C26' C24 C27' 110.1(8) . . ? C26 C24 C27' 68.5(6) . . ? C25' C24 C27' 109.9(7) . . ? C27 C24 C27' 45.8(5) . . ? C17 C24 C27' 107.4(5) . . ? C26' C24 C25 65.1(7) . . ? C26 C24 C25 108.0(5) . . ? C25' C24 C25 47.6(5) . . ? C27 C24 C25 107.0(5) . . ? C17 C24 C25 109.4(4) . . ? C27' C24 C25 141.3(5) . . ? C31 C28 C29 106.8(3) . . ? C31 C28 C30 110.4(3) . . ? C29 C28 C30 105.8(3) . . ? C31 C28 C19 111.1(3) . . ? C29 C28 C19 111.6(3) . . ? C30 C28 C19 110.9(3) . . ? C37 C32 C33 119.5(3) . . ? C37 C32 P2 121.1(2) . . ? C33 C32 P2 119.4(2) . . ? C34 C33 C32 117.8(3) . . ? C34 C33 C38 116.9(3) . . ? C32 C33 C38 125.3(3) . . ? C35 C34 C33 123.8(3) . . ? C34 C35 C36 117.0(3) . . ? C34 C35 C42 121.1(3) . . ? C36 C35 C42 121.8(3) . . ? C35 C36 C37 123.3(3) . . ? C36 C37 C32 118.1(3) . . ? C36 C37 C46 117.2(3) . . ? C32 C37 C46 124.6(3) . . ? C40 C38 C39 111.1(4) . . ? C40 C38 C41 106.9(3) . . ? C39 C38 C41 104.9(3) . . ? C40 C38 C33 109.2(3) . . ? C39 C38 C33 113.4(3) . . ? C41 C38 C33 111.2(3) . . ? C45' C42 C43 134.3(15) . . ? C45' C42 C43' 120.1(17) . . ? C43 C42 C43' 58.2(13) . . ? C43 C42 C45 109.9(5) . . ? C43' C42 C45 136.8(11) . . ? C45' C42 C35 111.8(14) . . ? C43 C42 C35 110.3(4) . . ? C43' C42 C35 109.9(10) . . ? C45 C42 C35 112.9(4) . . ? C45' C42 C44 73.0(16) . . ? C43 C42 C44 109.1(6) . . ? C43' C42 C44 53.7(13) . . ? C45 C42 C44 105.6(5) . . ? C35 C42 C44 108.8(4) . . ? C45' C42 C44' 112.8(18) . . ? C43' C42 C44' 102.0(17) . . ? C45 C42 C44' 77.9(14) . . ? C35 C42 C44' 97.7(11) . . ? C44 C42 C44' 148.6(13) . . ? C48 C46 C49 110.3(3) . . ? C48 C46 C47 105.7(3) . . ? C49 C46 C47 106.0(3) . . ? C48 C46 C37 110.5(3) . . ? C49 C46 C37 112.7(3) . . ? C47 C46 C37 111.4(3) . . ? Cl4 C50 Cl5 114.9(4) . . ? Cl7 C51 Cl6 105.6(11) . . ? Cl7' C51' Cl6' 115.2(8) . . ? Cl8 C52 Cl9 108.0(15) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.906 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.079 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 857223' #TrackingRef 'KT-chemcomm-2011.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H87 Au Cl2 Ge I N2 P2' _chemical_formula_weight 1341.59 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' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz '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, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.1895(9) _cell_length_b 37.193(3) _cell_length_c 27.7641(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.446(3) _cell_angle_gamma 90.00 _cell_volume 12530.3(16) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5416 _exptl_absorpt_coefficient_mu 3.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7221 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124173 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 5.15 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12726 _reflns_number_gt 8650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0257P)^2^+62.5594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12726 _refine_ls_number_parameters 708 _refine_ls_number_restraints 244 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _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 Au1 Au 0.974688(18) 0.238843(6) 0.887739(8) 0.03084(7) Uani 1 1 d . . . Ge1 Ge 0.83200(4) 0.198140(15) 0.901490(19) 0.02420(13) Uani 1 1 d . . . I1 I 1.12342(3) 0.284578(12) 0.868538(19) 0.05416(14) Uani 1 1 d . . . P1 P 0.68272(11) 0.15558(4) 0.81908(5) 0.0263(3) Uani 1 1 d . . . Cl1 Cl 0.92538(11) 0.13909(4) 0.83799(5) 0.0348(3) Uani 1 1 d . . . P2 P 0.90535(13) 0.12965(4) 0.96490(5) 0.0319(4) Uani 1 1 d . . . Cl2 Cl 0.87478(12) 0.20186(4) 1.01349(5) 0.0356(3) Uani 1 1 d . . . N1 N 0.6479(4) 0.24978(12) 0.87184(16) 0.0299(11) Uani 1 1 d . . . N2 N 0.5956(4) 0.21306(13) 0.92601(16) 0.0314(11) Uani 1 1 d . . . C1 C 0.8053(4) 0.16103(13) 0.85062(18) 0.0218(11) Uani 1 1 d . . . C2 C 0.8646(4) 0.17258(15) 0.96381(18) 0.0270(12) Uani 1 1 d . . . C3 C 0.6808(4) 0.22116(16) 0.9002(2) 0.0310(14) Uani 1 1 d . . . C4 C 0.5409(5) 0.25934(17) 0.8803(2) 0.0381(15) Uani 1 1 d . . . C5 C 0.5085(4) 0.23665(18) 0.9139(2) 0.0388(15) Uani 1 1 d . . . C6 C 0.4782(6) 0.29123(19) 0.8581(3) 0.059(2) Uani 1 1 d . . . H6A H 0.4107 0.2947 0.8741 0.088 Uiso 1 1 calc R . . H6B H 0.4588 0.2868 0.8235 0.088 Uiso 1 1 calc R . . H6C H 0.5242 0.3128 0.8622 0.088 Uiso 1 1 calc R . . C7 C 0.3995(5) 0.2361(2) 0.9352(2) 0.0526(18) Uani 1 1 d . . . H7A H 0.3450 0.2496 0.9143 0.079 Uiso 1 1 calc R . . H7B H 0.4079 0.2470 0.9674 0.079 Uiso 1 1 calc R . . H7C H 0.3746 0.2111 0.9377 0.079 Uiso 1 1 calc R . . C8 C 0.7159(5) 0.26735(15) 0.8368(2) 0.0350(14) Uani 1 1 d . . . H8 H 0.7822 0.2518 0.8347 0.042 Uiso 1 1 calc R . . C9 C 0.6568(6) 0.26898(19) 0.7861(2) 0.0528(18) Uani 1 1 d . . . H9A H 0.6163 0.2465 0.7792 0.079 Uiso 1 1 calc R . . H9B H 0.7109 0.2723 0.7625 0.079 Uiso 1 1 calc R . . H9C H 0.6051 0.2892 0.7840 0.079 Uiso 1 1 calc R . . C10 C 0.7580(6) 0.30335(18) 0.8560(3) 0.058(2) Uani 1 1 d . . . H10A H 0.6967 0.3205 0.8550 0.087 Uiso 1 1 calc R . . H10B H 0.8140 0.3124 0.8359 0.087 Uiso 1 1 calc R . . H10C H 0.7904 0.3006 0.8894 0.087 Uiso 1 1 calc R . . C11 C 0.5946(4) 0.18302(16) 0.9602(2) 0.0335(14) Uani 1 1 d . . . H11 H 0.6720 0.1740 0.9654 0.040 Uiso 1 1 calc R . . C12 C 0.5624(5) 0.19457(18) 1.0097(2) 0.0447(16) Uani 1 1 d . . . H12A H 0.6045 0.2160 1.0206 0.067 Uiso 1 1 calc R . . H12B H 0.5786 0.1751 1.0330 0.067 Uiso 1 1 calc R . . H12C H 0.4835 0.2001 1.0074 0.067 Uiso 1 1 calc R . . C13 C 0.5248(5) 0.15187(17) 0.9376(2) 0.0453(17) Uani 1 1 d . . . H13A H 0.4476 0.1594 0.9321 0.068 Uiso 1 1 calc R . . H13B H 0.5306 0.1312 0.9596 0.068 Uiso 1 1 calc R . . H13C H 0.5517 0.1451 0.9067 0.068 Uiso 1 1 calc R . . C14 C 0.7079(4) 0.12097(14) 0.77378(18) 0.0234(12) Uani 1 1 d . . . C15 C 0.6971(4) 0.08409(15) 0.78473(18) 0.0270(13) Uani 1 1 d . . . C16 C 0.7403(4) 0.05880(15) 0.7550(2) 0.0304(13) Uani 1 1 d . . . H16 H 0.7356 0.0341 0.7633 0.036 Uiso 1 1 calc R . . C17 C 0.7898(4) 0.06790(15) 0.71382(19) 0.0277(13) Uani 1 1 d . . . C18 C 0.7898(4) 0.10387(15) 0.70122(19) 0.0269(13) Uani 1 1 d . . . H18 H 0.8194 0.1105 0.6720 0.032 Uiso 1 1 calc R . . C19 C 0.7485(4) 0.13085(15) 0.72926(18) 0.0251(12) Uani 1 1 d . . . C20 C 0.6356(5) 0.06965(16) 0.8273(2) 0.0333(14) Uani 1 1 d . . . C21 C 0.5225(5) 0.08816(19) 0.8293(2) 0.0462(17) Uani 1 1 d . . . H21A H 0.4862 0.0784 0.8565 0.069 Uiso 1 1 calc R . . H21B H 0.4764 0.0837 0.7991 0.069 Uiso 1 1 calc R . . H21C H 0.5333 0.1141 0.8337 0.069 Uiso 1 1 calc R . . C22 C 0.7058(5) 0.07385(18) 0.8759(2) 0.0422(16) Uani 1 1 d . . . H22A H 0.6656 0.0640 0.9019 0.063 Uiso 1 1 calc R . . H22B H 0.7210 0.0994 0.8821 0.063 Uiso 1 1 calc R . . H22C H 0.7754 0.0608 0.8748 0.063 Uiso 1 1 calc R . . C23 C 0.6087(6) 0.02908(18) 0.8216(2) 0.0550(19) Uani 1 1 d . . . H23A H 0.6775 0.0153 0.8240 0.083 Uiso 1 1 calc R . . H23B H 0.5678 0.0248 0.7901 0.083 Uiso 1 1 calc R . . H23C H 0.5640 0.0215 0.8473 0.083 Uiso 1 1 calc R . . C24 C 0.8368(5) 0.03966(16) 0.6816(2) 0.0351(14) Uani 1 1 d . . . C25 C 0.8445(6) 0.00221(17) 0.7052(2) 0.0485(17) Uani 1 1 d . . . H25A H 0.8872 0.0038 0.7369 0.073 Uiso 1 1 calc R . . H25B H 0.8810 -0.0144 0.6845 0.073 Uiso 1 1 calc R . . H25C H 0.7702 -0.0066 0.7094 0.073 Uiso 1 1 calc R . . C26 C 0.9527(5) 0.05022(17) 0.6700(2) 0.0471(17) Uani 1 1 d . . . H26A H 0.9490 0.0725 0.6511 0.071 Uiso 1 1 calc R . . H26B H 0.9837 0.0310 0.6514 0.071 Uiso 1 1 calc R . . H26C H 0.9997 0.0540 0.7003 0.071 Uiso 1 1 calc R . . C27 C 0.7619(6) 0.03739(18) 0.6339(2) 0.0491(17) Uani 1 1 d . . . H27A H 0.6899 0.0278 0.6403 0.074 Uiso 1 1 calc R . . H27B H 0.7956 0.0215 0.6113 0.074 Uiso 1 1 calc R . . H27C H 0.7525 0.0614 0.6197 0.074 Uiso 1 1 calc R . . C28 C 0.7460(4) 0.16966(15) 0.70885(19) 0.0274(13) Uani 1 1 d . . . C29 C 0.7655(5) 0.17059(16) 0.65483(19) 0.0354(14) Uani 1 1 d . . . H29A H 0.8405 0.1624 0.6509 0.053 Uiso 1 1 calc R . . H29B H 0.7560 0.1952 0.6426 0.053 Uiso 1 1 calc R . . H29C H 0.7124 0.1547 0.6366 0.053 Uiso 1 1 calc R . . C30 C 0.6302(4) 0.18622(15) 0.7111(2) 0.0336(14) Uani 1 1 d . . . H30A H 0.5752 0.1712 0.6925 0.050 Uiso 1 1 calc R . . H30B H 0.6288 0.2105 0.6973 0.050 Uiso 1 1 calc R . . H30C H 0.6133 0.1874 0.7449 0.050 Uiso 1 1 calc R . . C31 C 0.8336(5) 0.19382(15) 0.7351(2) 0.0348(14) Uani 1 1 d . . . H31A H 0.8177 0.1970 0.7688 0.052 Uiso 1 1 calc R . . H31B H 0.8330 0.2173 0.7191 0.052 Uiso 1 1 calc R . . H31C H 0.9063 0.1827 0.7343 0.052 Uiso 1 1 calc R . . C32 C 0.9734(5) 0.12013(15) 1.02596(19) 0.0306(13) Uani 1 1 d . . . C33 C 0.9164(5) 0.10300(16) 1.0621(2) 0.0368(15) Uani 1 1 d . B . C34 C 0.9735(5) 0.09669(18) 1.1071(2) 0.0473(17) Uani 1 1 d . . . H34 H 0.9356 0.0852 1.1312 0.057 Uiso 1 1 calc R . . C35 C 1.0818(5) 0.10624(19) 1.1186(2) 0.0496(18) Uani 1 1 d . A . C36 C 1.1370(5) 0.12176(17) 1.0826(2) 0.0400(16) Uani 1 1 d . . . H36 H 1.2118 0.1285 1.0900 0.048 Uiso 1 1 calc R . . C37 C 1.0882(5) 0.12787(15) 1.0361(2) 0.0318(13) Uani 1 1 d . . . C38 C 1.1658(5) 0.14062(16) 0.9984(2) 0.0363(14) Uani 1 1 d . . . C39 C 1.2882(5) 0.1373(2) 1.0187(3) 0.061(2) Uani 1 1 d . . . H39A H 1.3355 0.1419 0.9927 0.092 Uiso 1 1 calc R . . H39B H 1.3021 0.1129 1.0314 0.092 Uiso 1 1 calc R . . H39C H 1.3044 0.1548 1.0447 0.092 Uiso 1 1 calc R . . C40 C 1.1555(6) 0.11672(19) 0.9531(2) 0.0499(18) Uani 1 1 d . . . H40A H 1.0809 0.1188 0.9368 0.075 Uiso 1 1 calc R . . H40B H 1.1699 0.0916 0.9626 0.075 Uiso 1 1 calc R . . H40C H 1.2092 0.1245 0.9311 0.075 Uiso 1 1 calc R . . C41 C 1.1471(5) 0.18020(18) 0.9843(3) 0.0519(18) Uani 1 1 d . . . H41A H 1.2002 0.1874 0.9617 0.078 Uiso 1 1 calc R . . H41B H 1.1572 0.1952 1.0134 0.078 Uiso 1 1 calc R . . H41C H 1.0721 0.1833 0.9688 0.078 Uiso 1 1 calc R . . C42 C 1.1415(7) 0.0973(3) 1.1681(3) 0.079(2) Uani 1 1 d DU . . C43 C 1.0888(12) 0.0703(4) 1.1954(4) 0.086(3) Uani 0.685(9) 1 d PDU A 1 H43A H 1.0865 0.0475 1.1778 0.129 Uiso 0.685(9) 1 calc PR A 1 H43B H 1.0136 0.0780 1.2000 0.129 Uiso 0.685(9) 1 calc PR A 1 H43C H 1.1307 0.0672 1.2271 0.129 Uiso 0.685(9) 1 calc PR A 1 C44 C 1.1839(12) 0.1299(4) 1.1927(4) 0.082(3) Uani 0.685(9) 1 d PDU A 1 H44A H 1.2435 0.1236 1.2174 0.123 Uiso 0.685(9) 1 calc PR A 1 H44B H 1.1244 0.1418 1.2081 0.123 Uiso 0.685(9) 1 calc PR A 1 H44C H 1.2121 0.1463 1.1691 0.123 Uiso 0.685(9) 1 calc PR A 1 C45 C 1.2554(11) 0.0760(4) 1.1551(5) 0.102(3) Uani 0.685(9) 1 d PDU A 1 H45A H 1.2514 0.0507 1.1647 0.153 Uiso 0.685(9) 1 calc PR A 1 H45B H 1.3200 0.0873 1.1727 0.153 Uiso 0.685(9) 1 calc PR A 1 H45C H 1.2618 0.0775 1.1202 0.153 Uiso 0.685(9) 1 calc PR A 1 C43' C 1.158(3) 0.0610(5) 1.1778(10) 0.091(4) Uani 0.315(9) 1 d PDU A 2 H43D H 1.2284 0.0535 1.1669 0.137 Uiso 0.315(9) 1 calc PR A 2 H43E H 1.0980 0.0471 1.1605 0.137 Uiso 0.315(9) 1 calc PR A 2 H43F H 1.1584 0.0568 1.2126 0.137 Uiso 0.315(9) 1 calc PR A 2 C44' C 1.0637(18) 0.1153(7) 1.2039(7) 0.087(4) Uani 0.315(9) 1 d PDU A 2 H44D H 0.9891 0.1177 1.1877 0.130 Uiso 0.315(9) 1 calc PR A 2 H44E H 1.0922 0.1392 1.2134 0.130 Uiso 0.315(9) 1 calc PR A 2 H44F H 1.0617 0.1002 1.2327 0.130 Uiso 0.315(9) 1 calc PR A 2 C45' C 1.244(2) 0.1242(8) 1.1804(10) 0.084(4) Uani 0.315(9) 1 d PDU A 2 H45D H 1.2761 0.1202 1.2138 0.126 Uiso 0.315(9) 1 calc PR A 2 H45E H 1.2192 0.1491 1.1768 0.126 Uiso 0.315(9) 1 calc PR A 2 H45F H 1.3006 0.1196 1.1581 0.126 Uiso 0.315(9) 1 calc PR A 2 C46 C 0.7963(5) 0.08913(17) 1.0543(2) 0.0406(14) Uani 1 1 d DU . . C47 C 0.7814(8) 0.0628(3) 1.0116(3) 0.054(2) Uani 0.777(10) 1 d PDU B 1 H47A H 0.8137 0.0395 1.0215 0.081 Uiso 0.777(10) 1 calc PR B 1 H47B H 0.8184 0.0724 0.9845 0.081 Uiso 0.777(10) 1 calc PR B 1 H47C H 0.7027 0.0598 1.0016 0.081 Uiso 0.777(10) 1 calc PR B 1 C48 C 0.7148(7) 0.1204(2) 1.0460(4) 0.046(2) Uani 0.777(10) 1 d PDU B 1 H48A H 0.6398 0.1117 1.0487 0.069 Uiso 0.777(10) 1 calc PR B 1 H48B H 0.7195 0.1304 1.0136 0.069 Uiso 0.777(10) 1 calc PR B 1 H48C H 0.7330 0.1391 1.0703 0.069 Uiso 0.777(10) 1 calc PR B 1 C49 C 0.7613(8) 0.0678(3) 1.0985(4) 0.059(3) Uani 0.777(10) 1 d PDU B 1 H49A H 0.6852 0.0594 1.0915 0.089 Uiso 0.777(10) 1 calc PR B 1 H49B H 0.7662 0.0834 1.1270 0.089 Uiso 0.777(10) 1 calc PR B 1 H49C H 0.8102 0.0471 1.1047 0.089 Uiso 0.777(10) 1 calc PR B 1 C47' C 0.750(2) 0.0838(9) 1.0009(6) 0.048(4) Uani 0.223(10) 1 d PDU B 2 H47D H 0.8073 0.0734 0.9827 0.071 Uiso 0.223(10) 1 calc PR B 2 H47E H 0.7272 0.1071 0.9868 0.071 Uiso 0.223(10) 1 calc PR B 2 H47F H 0.6865 0.0676 0.9994 0.071 Uiso 0.223(10) 1 calc PR B 2 C48' C 0.723(2) 0.1166(7) 1.0768(12) 0.048(4) Uani 0.223(10) 1 d PDU B 2 H48D H 0.6459 0.1117 1.0661 0.072 Uiso 0.223(10) 1 calc PR B 2 H48E H 0.7425 0.1409 1.0665 0.072 Uiso 0.223(10) 1 calc PR B 2 H48F H 0.7350 0.1150 1.1121 0.072 Uiso 0.223(10) 1 calc PR B 2 C49' C 0.789(3) 0.0522(6) 1.0786(12) 0.051(4) Uani 0.223(10) 1 d PDU B 2 H49D H 0.8631 0.0417 1.0838 0.076 Uiso 0.223(10) 1 calc PR B 2 H49E H 0.7413 0.0364 1.0577 0.076 Uiso 0.223(10) 1 calc PR B 2 H49F H 0.7588 0.0551 1.1098 0.076 Uiso 0.223(10) 1 calc PR B 2 C50 C 0.0678(7) 0.0285(2) 1.0150(3) 0.066(2) Uani 1 1 d . . . H50 H 0.1133 0.0484 1.0249 0.080 Uiso 1 1 calc R . . C51 C 0.0231(8) 0.0256(2) 0.9679(3) 0.074(2) Uani 1 1 d . . . H51 H 0.0402 0.0434 0.9452 0.089 Uiso 1 1 calc R . . C52 C -0.0460(7) -0.0023(2) 0.9526(3) 0.070(2) Uani 1 1 d . . . H52 H -0.0781 -0.0033 0.9200 0.083 Uiso 1 1 calc R . . C53 C 0.561(2) -0.0064(4) 0.9672(9) 0.098(5) Uani 0.50 1 d PGDU C -1 H53 H 0.6000 -0.0166 0.9425 0.117 Uiso 0.50 1 calc PR C -1 C54 C 0.486(2) 0.0214(5) 0.9562(9) 0.093(5) Uani 0.50 1 d PGDU C -1 H54 H 0.4745 0.0301 0.9239 0.111 Uiso 0.50 1 calc PR C -1 C55 C 0.429(2) 0.0364(4) 0.9923(10) 0.106(5) Uani 0.50 1 d PGDU C -1 H55 H 0.3785 0.0553 0.9847 0.127 Uiso 0.50 1 calc PR C -1 C56 C 0.447(2) 0.0236(5) 1.0394(9) 0.112(5) Uani 0.50 1 d PGDU C -1 H56 H 0.4080 0.0339 1.0641 0.134 Uiso 0.50 1 calc PR C -1 C57 C 0.522(2) -0.0041(5) 1.0505(9) 0.095(5) Uani 0.50 1 d PGDU C -1 H57 H 0.5335 -0.0128 1.0827 0.114 Uiso 0.50 1 calc PR C -1 C58 C 0.579(2) -0.0191(4) 1.0144(9) 0.099(5) Uani 0.50 1 d PGDU C -1 H58 H 0.6295 -0.0381 1.0219 0.119 Uiso 0.50 1 calc PR C -1 C59 C 0.497(3) 0.1336(4) 0.2355(10) 0.141(11) Uani 0.50 1 d PGDU D -1 H59 H 0.4858 0.1589 0.2334 0.169 Uiso 0.50 1 calc PR D -1 C60 C 0.469(2) 0.1149(6) 0.2760(8) 0.145(10) Uani 0.50 1 d PGDU D -1 H60 H 0.4396 0.1275 0.3017 0.174 Uiso 0.50 1 calc PR D -1 C61 C 0.4849(19) 0.0780(6) 0.2790(8) 0.143(10) Uani 0.50 1 d PGDU D -1 H61 H 0.4662 0.0652 0.3068 0.172 Uiso 0.50 1 calc PR D -1 C62 C 0.528(2) 0.0596(4) 0.2415(11) 0.130(10) Uani 0.50 1 d PGDU D -1 H62 H 0.5389 0.0344 0.2436 0.156 Uiso 0.50 1 calc PR D -1 C63 C 0.5555(19) 0.0783(6) 0.2009(9) 0.146(10) Uani 0.50 1 d PGDU D -1 H63 H 0.5850 0.0658 0.1753 0.175 Uiso 0.50 1 calc PR D -1 C64 C 0.540(2) 0.1153(6) 0.1979(7) 0.152(11) Uani 0.50 1 d PGDU D -1 H64 H 0.5585 0.1280 0.1702 0.182 Uiso 0.50 1 calc PR D -1 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 Au1 0.02924(12) 0.02782(13) 0.03436(12) 0.00189(11) -0.00279(9) -0.00489(10) Ge1 0.0245(3) 0.0227(3) 0.0243(3) -0.0005(2) -0.0034(2) -0.0015(2) I1 0.0391(3) 0.0421(3) 0.0818(3) 0.0051(2) 0.0085(2) -0.0134(2) P1 0.0248(7) 0.0269(8) 0.0262(8) -0.0050(6) -0.0021(6) -0.0015(6) Cl1 0.0280(7) 0.0416(9) 0.0336(8) -0.0052(7) -0.0029(6) 0.0095(6) P2 0.0401(9) 0.0269(9) 0.0268(8) 0.0019(7) -0.0062(7) -0.0036(7) Cl2 0.0450(8) 0.0343(9) 0.0266(7) -0.0066(6) -0.0011(6) -0.0042(7) N1 0.032(3) 0.021(3) 0.035(3) -0.005(2) -0.004(2) 0.007(2) N2 0.029(3) 0.034(3) 0.031(3) -0.011(2) 0.001(2) 0.002(2) C1 0.024(3) 0.018(3) 0.023(3) 0.001(2) 0.000(2) -0.001(2) C2 0.029(3) 0.026(3) 0.026(3) -0.005(2) 0.001(2) -0.010(2) C3 0.030(3) 0.029(3) 0.031(3) -0.014(3) -0.009(3) 0.000(3) C4 0.035(3) 0.034(4) 0.043(4) -0.011(3) -0.008(3) 0.004(3) C5 0.026(3) 0.044(4) 0.044(4) -0.021(3) -0.006(3) 0.001(3) C6 0.056(4) 0.051(5) 0.066(5) 0.007(4) -0.015(4) 0.023(4) C7 0.029(3) 0.062(5) 0.066(5) -0.018(4) 0.000(3) 0.013(3) C8 0.035(3) 0.027(4) 0.041(3) 0.008(3) -0.004(3) 0.005(3) C9 0.071(5) 0.044(5) 0.041(4) 0.001(3) -0.007(3) 0.011(4) C10 0.065(5) 0.038(4) 0.070(5) 0.000(4) -0.006(4) -0.012(4) C11 0.026(3) 0.040(4) 0.035(3) -0.004(3) 0.001(2) -0.001(3) C12 0.044(4) 0.050(4) 0.040(4) -0.011(3) 0.003(3) -0.004(3) C13 0.051(4) 0.043(4) 0.044(4) -0.008(3) 0.016(3) -0.013(3) C14 0.022(3) 0.022(3) 0.024(3) -0.003(2) -0.005(2) 0.000(2) C15 0.029(3) 0.027(3) 0.023(3) -0.002(2) -0.003(2) -0.004(2) C16 0.036(3) 0.019(3) 0.034(3) 0.002(3) -0.003(3) -0.002(3) C17 0.025(3) 0.029(3) 0.027(3) -0.005(3) -0.006(2) 0.001(2) C18 0.026(3) 0.028(3) 0.025(3) -0.002(3) -0.005(2) 0.000(2) C19 0.021(3) 0.029(3) 0.025(3) -0.003(2) -0.006(2) -0.001(2) C20 0.040(3) 0.030(4) 0.029(3) 0.003(3) -0.001(3) -0.008(3) C21 0.037(4) 0.059(5) 0.043(4) -0.010(3) 0.006(3) -0.016(3) C22 0.052(4) 0.043(4) 0.029(3) 0.006(3) -0.002(3) -0.008(3) C23 0.082(5) 0.042(4) 0.042(4) 0.004(3) 0.013(4) -0.023(4) C24 0.042(4) 0.029(4) 0.034(3) -0.007(3) 0.000(3) 0.002(3) C25 0.070(5) 0.031(4) 0.044(4) -0.002(3) 0.004(3) 0.010(3) C26 0.048(4) 0.037(4) 0.058(4) -0.014(3) 0.009(3) 0.005(3) C27 0.069(5) 0.038(4) 0.038(4) -0.014(3) -0.006(3) 0.003(4) C28 0.032(3) 0.024(3) 0.026(3) -0.001(2) -0.002(2) 0.003(2) C29 0.042(4) 0.029(4) 0.033(3) 0.002(3) 0.000(3) 0.008(3) C30 0.033(3) 0.029(3) 0.037(3) 0.006(3) -0.005(3) 0.008(3) C31 0.038(3) 0.026(3) 0.040(3) 0.006(3) 0.001(3) -0.005(3) C32 0.044(3) 0.021(3) 0.026(3) 0.000(2) -0.001(3) -0.005(3) C33 0.043(4) 0.033(4) 0.034(3) 0.008(3) -0.002(3) -0.010(3) C34 0.050(4) 0.054(5) 0.037(4) 0.021(3) -0.003(3) -0.018(3) C35 0.052(4) 0.058(5) 0.036(4) 0.020(3) -0.010(3) -0.019(4) C36 0.036(3) 0.048(4) 0.035(3) 0.011(3) -0.005(3) -0.011(3) C37 0.036(3) 0.025(3) 0.033(3) 0.001(3) -0.004(3) 0.000(3) C38 0.041(4) 0.032(4) 0.035(3) 0.006(3) 0.004(3) -0.006(3) C39 0.043(4) 0.090(6) 0.050(4) 0.005(4) 0.008(3) -0.004(4) C40 0.056(4) 0.052(5) 0.044(4) 0.000(3) 0.016(3) -0.007(3) C41 0.047(4) 0.041(4) 0.069(5) 0.016(4) 0.014(3) -0.011(3) C42 0.077(5) 0.110(5) 0.046(4) 0.031(4) -0.024(3) -0.029(4) C43 0.094(7) 0.105(7) 0.052(6) 0.048(5) -0.031(5) -0.022(6) C44 0.092(7) 0.108(6) 0.039(5) 0.019(5) -0.031(5) -0.020(6) C45 0.098(6) 0.126(7) 0.074(6) 0.033(6) -0.027(5) 0.011(6) C43' 0.093(7) 0.112(7) 0.061(7) 0.039(6) -0.031(6) -0.011(6) C44' 0.091(8) 0.119(8) 0.042(7) 0.020(7) -0.037(6) -0.017(7) C45' 0.087(8) 0.113(8) 0.045(7) 0.027(7) -0.033(7) -0.027(7) C46 0.039(3) 0.039(3) 0.043(3) 0.010(3) 0.000(3) -0.010(3) C47 0.052(5) 0.039(5) 0.070(5) 0.003(4) 0.001(4) -0.016(4) C48 0.041(4) 0.050(5) 0.048(5) 0.007(4) 0.010(4) -0.001(4) C49 0.057(5) 0.059(6) 0.061(5) 0.023(5) 0.000(4) -0.021(5) C47' 0.045(7) 0.037(8) 0.059(7) 0.010(7) -0.004(7) -0.021(7) C48' 0.043(7) 0.048(7) 0.054(8) 0.006(7) 0.003(7) -0.007(7) C49' 0.049(7) 0.048(8) 0.054(8) 0.015(7) -0.002(7) -0.018(7) C50 0.089(6) 0.041(5) 0.072(6) -0.005(4) 0.023(5) -0.007(4) C51 0.116(7) 0.044(5) 0.066(6) 0.006(4) 0.025(5) -0.014(5) C52 0.103(7) 0.044(5) 0.063(5) 0.000(4) 0.015(5) -0.005(5) C53 0.114(9) 0.079(14) 0.093(9) -0.006(12) -0.023(7) -0.025(12) C54 0.101(9) 0.084(15) 0.086(9) 0.007(12) -0.031(7) -0.028(12) C55 0.107(9) 0.094(15) 0.111(10) 0.013(13) -0.020(8) -0.018(12) C56 0.115(10) 0.107(15) 0.110(10) 0.011(13) -0.008(8) -0.024(12) C57 0.105(9) 0.085(14) 0.092(10) 0.038(12) -0.013(8) -0.038(12) C58 0.112(9) 0.074(14) 0.105(10) 0.019(12) -0.025(8) -0.027(12) C59 0.085(17) 0.151(15) 0.17(3) 0.017(14) -0.08(2) -0.007(15) C60 0.073(18) 0.20(2) 0.15(2) -0.014(19) -0.016(18) 0.01(2) C61 0.10(2) 0.20(2) 0.12(2) 0.04(2) -0.022(16) -0.01(2) C62 0.08(2) 0.139(15) 0.17(3) 0.030(15) -0.024(16) -0.017(14) C63 0.082(17) 0.188(18) 0.17(3) 0.019(17) 0.022(15) -0.019(17) C64 0.103(17) 0.177(18) 0.17(3) 0.046(17) 0.007(17) -0.062(18) _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 Au1 Ge1 2.3641(6) . ? Au1 I1 2.5783(5) . ? Ge1 C1 1.979(5) . ? Ge1 C2 1.981(5) . ? Ge1 C3 2.030(6) . ? P1 C1 1.671(5) . ? P1 C14 1.846(5) . ? Cl1 C1 1.740(5) . ? P2 C2 1.671(6) . ? P2 C32 1.849(5) . ? Cl2 C2 1.752(5) . ? N1 C3 1.362(7) . ? N1 C4 1.394(7) . ? N1 C8 1.489(7) . ? N2 C3 1.350(7) . ? N2 C5 1.394(7) . ? N2 C11 1.467(7) . ? C4 C5 1.344(9) . ? C4 C6 1.510(8) . ? C5 C7 1.505(8) . ? C8 C10 1.513(8) . ? C8 C9 1.519(8) . ? C11 C12 1.527(8) . ? C11 C13 1.535(8) . ? C14 C15 1.414(7) . ? C14 C19 1.422(7) . ? C15 C16 1.387(7) . ? C15 C20 1.553(7) . ? C16 C17 1.385(7) . ? C17 C18 1.383(7) . ? C17 C24 1.526(8) . ? C18 C19 1.393(7) . ? C19 C28 1.550(7) . ? C20 C22 1.537(8) . ? C20 C21 1.547(8) . ? C20 C23 1.549(8) . ? C24 C26 1.530(8) . ? C24 C27 1.537(8) . ? C24 C25 1.539(8) . ? C28 C31 1.526(7) . ? C28 C29 1.541(7) . ? C28 C30 1.546(7) . ? C32 C33 1.423(8) . ? C32 C37 1.431(8) . ? C33 C34 1.393(8) . ? C33 C46 1.547(8) . ? C34 C35 1.375(8) . ? C35 C36 1.384(8) . ? C35 C42 1.529(9) . ? C36 C37 1.386(8) . ? C37 C38 1.550(8) . ? C38 C41 1.535(8) . ? C38 C40 1.535(8) . ? C38 C39 1.549(9) . ? C42 C43' 1.388(17) . ? C42 C43 1.446(12) . ? C42 C44 1.460(14) . ? C42 C44' 1.585(19) . ? C42 C45' 1.615(19) . ? C42 C45 1.669(15) . ? C46 C48' 1.527(17) . ? C46 C48 1.533(9) . ? C46 C47 1.533(10) . ? C46 C49' 1.535(17) . ? C46 C47' 1.547(17) . ? C46 C49 1.555(9) . ? C50 C51 1.371(11) . ? C50 C52 1.371(10) 5_557 ? C51 C52 1.378(11) . ? C52 C50 1.371(10) 5_557 ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? 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 Ge1 Au1 I1 176.75(2) . . ? C1 Ge1 C2 107.1(2) . . ? C1 Ge1 C3 101.2(2) . . ? C2 Ge1 C3 108.9(2) . . ? C1 Ge1 Au1 113.88(15) . . ? C2 Ge1 Au1 111.01(15) . . ? C3 Ge1 Au1 114.08(17) . . ? C1 P1 C14 104.1(2) . . ? C2 P2 C32 107.8(3) . . ? C3 N1 C4 109.3(5) . . ? C3 N1 C8 124.8(4) . . ? C4 N1 C8 125.9(5) . . ? C3 N2 C5 109.7(5) . . ? C3 N2 C11 124.6(5) . . ? C5 N2 C11 125.7(5) . . ? P1 C1 Cl1 124.4(3) . . ? P1 C1 Ge1 122.5(3) . . ? Cl1 C1 Ge1 112.7(3) . . ? P2 C2 Cl2 125.5(3) . . ? P2 C2 Ge1 120.6(3) . . ? Cl2 C2 Ge1 112.5(3) . . ? N2 C3 N1 106.4(5) . . ? N2 C3 Ge1 129.8(4) . . ? N1 C3 Ge1 123.8(4) . . ? C5 C4 N1 107.3(5) . . ? C5 C4 C6 127.3(6) . . ? N1 C4 C6 125.3(6) . . ? C4 C5 N2 107.3(5) . . ? C4 C5 C7 127.6(6) . . ? N2 C5 C7 125.2(6) . . ? N1 C8 C10 110.4(5) . . ? N1 C8 C9 112.2(5) . . ? C10 C8 C9 113.9(5) . . ? N2 C11 C12 112.8(5) . . ? N2 C11 C13 110.4(5) . . ? C12 C11 C13 113.6(5) . . ? C15 C14 C19 119.0(5) . . ? C15 C14 P1 120.3(4) . . ? C19 C14 P1 120.4(4) . . ? C16 C15 C14 118.8(5) . . ? C16 C15 C20 117.1(5) . . ? C14 C15 C20 124.1(5) . . ? C17 C16 C15 123.0(5) . . ? C18 C17 C16 117.1(5) . . ? C18 C17 C24 120.6(5) . . ? C16 C17 C24 122.2(5) . . ? C17 C18 C19 123.1(5) . . ? C18 C19 C14 118.3(5) . . ? C18 C19 C28 117.5(5) . . ? C14 C19 C28 124.2(5) . . ? C22 C20 C21 110.2(5) . . ? C22 C20 C23 106.4(5) . . ? C21 C20 C23 104.9(5) . . ? C22 C20 C15 111.4(5) . . ? C21 C20 C15 111.8(5) . . ? C23 C20 C15 111.9(5) . . ? C17 C24 C26 110.6(5) . . ? C17 C24 C27 108.5(5) . . ? C26 C24 C27 108.6(5) . . ? C17 C24 C25 112.6(5) . . ? C26 C24 C25 107.5(5) . . ? C27 C24 C25 109.0(5) . . ? C31 C28 C29 106.6(4) . . ? C31 C28 C30 110.2(5) . . ? C29 C28 C30 104.8(4) . . ? C31 C28 C19 112.7(4) . . ? C29 C28 C19 112.2(4) . . ? C30 C28 C19 110.0(4) . . ? C33 C32 C37 119.0(5) . . ? C33 C32 P2 121.6(4) . . ? C37 C32 P2 119.2(4) . . ? C34 C33 C32 118.2(5) . . ? C34 C33 C46 117.0(5) . . ? C32 C33 C46 124.7(5) . . ? C35 C34 C33 123.5(6) . . ? C34 C35 C36 117.5(5) . . ? C34 C35 C42 121.1(6) . . ? C36 C35 C42 121.2(6) . . ? C35 C36 C37 123.1(6) . . ? C36 C37 C32 118.4(5) . . ? C36 C37 C38 116.3(5) . . ? C32 C37 C38 125.2(5) . . ? C41 C38 C40 110.3(5) . . ? C41 C38 C39 106.5(5) . . ? C40 C38 C39 104.5(5) . . ? C41 C38 C37 112.4(5) . . ? C40 C38 C37 111.7(5) . . ? C39 C38 C37 111.0(5) . . ? C43' C42 C44 132.9(14) . . ? C43 C42 C44 119.2(10) . . ? C43' C42 C35 115.5(13) . . ? C43 C42 C35 115.1(7) . . ? C44 C42 C35 110.9(8) . . ? C43' C42 C44' 111.9(17) . . ? C43 C42 C44' 69.0(12) . . ? C44 C42 C44' 64.1(11) . . ? C35 C42 C44' 102.1(10) . . ? C43' C42 C45' 117.9(18) . . ? C43 C42 C45' 134.0(12) . . ? C35 C42 C45' 110.5(11) . . ? C44' C42 C45' 96.1(15) . . ? C43' C42 C45 58.1(16) . . ? C43 C42 C45 101.7(10) . . ? C44 C42 C45 103.4(9) . . ? C35 C42 C45 104.0(7) . . ? C44' C42 C45 153.7(10) . . ? C45' C42 C45 72.2(12) . . ? C48' C46 C47 135.4(13) . . ? C48 C46 C47 109.9(6) . . ? C48' C46 C49' 111.1(16) . . ? C48 C46 C49' 133.0(14) . . ? C47 C46 C49' 76.2(14) . . ? C48' C46 C47' 107.7(16) . . ? C48 C46 C47' 77.3(13) . . ? C49' C46 C47' 106.1(16) . . ? C48' C46 C33 107.4(12) . . ? C48 C46 C33 111.0(6) . . ? C47 C46 C33 111.2(6) . . ? C49' C46 C33 109.2(13) . . ? C47' C46 C33 115.4(12) . . ? C48' C46 C49 78.8(13) . . ? C48 C46 C49 106.5(6) . . ? C47 C46 C49 105.2(7) . . ? C47' C46 C49 126.0(12) . . ? C33 C46 C49 112.8(6) . . ? C51 C50 C52 119.1(8) . 5_557 ? C50 C51 C52 122.1(8) . . ? C50 C52 C51 118.8(8) 5_557 . ? C54 C53 C58 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C53 120.0 . . ? C60 C59 C64 120.0 . . ? C61 C60 C59 120.0 . . ? C60 C61 C62 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C59 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.598 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.116 #===END