# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sh3241a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H89 Cl Ge N2 Si2' _chemical_formula_sum 'C56 H89 Cl Ge N2 Si2' _chemical_formula_weight 954.51 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' Ge Ge 0.1547 1.8001 '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' Si Si 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3816(11) _cell_length_b 10.9027(6) _cell_length_c 25.5288(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.840(3) _cell_angle_gamma 90.00 _cell_volume 5672.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 1966 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 21.24 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9035 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details 'SADABS, BrukerAXS 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48361 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.1843 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.33 _reflns_number_total 14017 _reflns_number_gt 6354 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14017 _refine_ls_number_parameters 589 _refine_ls_number_restraints 179 _refine_ls_R_factor_all 0.1802 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.117535(19) 0.36265(4) 0.263942(16) 0.03194(13) Uani 1 1 d U . . Cl1 Cl 0.27188(4) 0.77086(7) 0.28104(3) 0.0266(2) Uani 1 1 d U . . Si2 Si 0.25596(5) 0.60448(8) 0.32175(4) 0.0213(2) Uani 1 1 d U . . Si1 Si 0.21648(5) 0.45856(9) 0.25967(4) 0.0223(2) Uani 1 1 d U . . N1 N 0.14025(13) 0.1893(2) 0.16846(11) 0.0235(7) Uani 1 1 d U A . N2 N 0.12028(14) 0.0947(3) 0.24038(11) 0.0294(7) Uani 1 1 d U . . C1 C 0.21194(17) 0.6780(3) 0.37949(13) 0.0234(8) Uani 1 1 d U . . C2 C 0.24647(17) 0.7634(3) 0.41177(13) 0.0246(8) Uani 1 1 d U . . C3 C 0.21365(18) 0.8251(3) 0.45112(14) 0.0306(9) Uani 1 1 d U . . H3 H 0.2376 0.8811 0.4725 0.037 Uiso 1 1 calc R . . C4 C 0.14765(19) 0.8085(3) 0.46049(14) 0.0331(9) Uani 1 1 d U . . C5 C 0.11485(18) 0.7242(3) 0.42961(14) 0.0339(9) Uani 1 1 d U . . H5 H 0.0695 0.7110 0.4354 0.041 Uiso 1 1 calc R . . C6 C 0.14490(17) 0.6581(3) 0.39056(13) 0.0273(8) Uani 1 1 d U . . C7 C 0.31880(16) 0.7959(3) 0.40586(14) 0.0267(9) Uani 1 1 d U . . H7 H 0.3359 0.7503 0.3749 0.032 Uiso 1 1 calc R . . C8 C 0.35866(18) 0.7555(3) 0.45460(14) 0.0350(10) Uani 1 1 d U . . H8A H 0.3434 0.8007 0.4853 0.052 Uiso 1 1 calc R . . H8B H 0.4053 0.7728 0.4493 0.052 Uiso 1 1 calc R . . H8C H 0.3526 0.6673 0.4602 0.052 Uiso 1 1 calc R . . C9 C 0.32871(18) 0.9331(3) 0.39620(15) 0.0362(10) Uani 1 1 d U . . H9A H 0.3039 0.9578 0.3648 0.054 Uiso 1 1 calc R . . H9B H 0.3754 0.9498 0.3912 0.054 Uiso 1 1 calc R . . H9C H 0.3132 0.9795 0.4264 0.054 Uiso 1 1 calc R . . C10 C 0.11306(19) 0.8882(4) 0.50009(14) 0.0393(10) Uani 1 1 d U . . H10 H 0.1473 0.9225 0.5245 0.047 Uiso 1 1 calc R . . C11 C 0.0807(2) 0.9954(3) 0.47175(15) 0.0431(11) Uani 1 1 d U . . H11A H 0.1141 1.0430 0.4535 0.065 Uiso 1 1 calc R . . H11B H 0.0587 1.0480 0.4972 0.065 Uiso 1 1 calc R . . H11C H 0.0483 0.9643 0.4463 0.065 Uiso 1 1 calc R . . C12 C 0.0648(2) 0.8169(4) 0.53270(15) 0.0485(12) Uani 1 1 d U . . H12A H 0.0274 0.7919 0.5106 0.073 Uiso 1 1 calc R . . H12B H 0.0494 0.8686 0.5614 0.073 Uiso 1 1 calc R . . H12C H 0.0864 0.7438 0.5472 0.073 Uiso 1 1 calc R . . C13 C 0.10243(17) 0.5692(3) 0.35957(14) 0.0290(9) Uani 1 1 d U . . H13 H 0.1323 0.5216 0.3364 0.035 Uiso 1 1 calc R . . C14 C 0.05330(19) 0.6366(4) 0.32378(16) 0.0495(12) Uani 1 1 d U . . H14A H 0.0231 0.6845 0.3452 0.074 Uiso 1 1 calc R . . H14B H 0.0284 0.5766 0.3029 0.074 Uiso 1 1 calc R . . H14C H 0.0770 0.6916 0.3003 0.074 Uiso 1 1 calc R . . C15 C 0.0676(2) 0.4768(4) 0.39432(16) 0.0524(12) Uani 1 1 d U . . H15A H 0.1001 0.4329 0.4159 0.079 Uiso 1 1 calc R . . H15B H 0.0434 0.4180 0.3723 0.079 Uiso 1 1 calc R . . H15C H 0.0369 0.5200 0.4170 0.079 Uiso 1 1 calc R . . C16 C 0.33565(16) 0.5351(3) 0.34800(13) 0.0210(8) Uani 1 1 d U . . C17 C 0.33070(16) 0.4580(3) 0.39227(13) 0.0224(8) Uani 1 1 d U . . C18 C 0.38701(17) 0.4181(3) 0.41854(14) 0.0259(8) Uani 1 1 d U . . H18 H 0.3826 0.3685 0.4489 0.031 Uiso 1 1 calc R . . C19 C 0.44958(17) 0.4484(3) 0.40181(14) 0.0248(8) Uani 1 1 d U . . C20 C 0.45413(17) 0.5174(3) 0.35670(13) 0.0250(8) Uani 1 1 d U . . H20 H 0.4965 0.5376 0.3443 0.030 Uiso 1 1 calc R . . C21 C 0.39929(16) 0.5586(3) 0.32858(13) 0.0207(8) Uani 1 1 d U . . C22 C 0.26494(17) 0.4111(3) 0.41267(14) 0.0265(8) Uani 1 1 d U . . H22 H 0.2296 0.4459 0.3895 0.032 Uiso 1 1 calc R . . C23 C 0.26117(18) 0.2706(3) 0.40797(15) 0.0362(10) Uani 1 1 d U . . H23A H 0.2699 0.2463 0.3718 0.054 Uiso 1 1 calc R . . H23B H 0.2173 0.2428 0.4176 0.054 Uiso 1 1 calc R . . H23C H 0.2939 0.2332 0.4315 0.054 Uiso 1 1 calc R . . C24 C 0.25082(18) 0.4522(3) 0.46835(14) 0.0357(10) Uani 1 1 d U . . H24A H 0.2848 0.4202 0.4922 0.054 Uiso 1 1 calc R . . H24B H 0.2079 0.4208 0.4788 0.054 Uiso 1 1 calc R . . H24C H 0.2506 0.5420 0.4699 0.054 Uiso 1 1 calc R . . C25 C 0.50943(17) 0.3973(3) 0.43056(15) 0.0333(9) Uani 1 1 d U . . H25 H 0.4969 0.3863 0.4680 0.040 Uiso 1 1 calc R . . C26 C 0.5257(2) 0.2730(4) 0.4099(2) 0.0712(16) Uani 1 1 d U . . H26A H 0.4868 0.2202 0.4116 0.107 Uiso 1 1 calc R . . H26B H 0.5613 0.2371 0.4310 0.107 Uiso 1 1 calc R . . H26C H 0.5395 0.2801 0.3734 0.107 Uiso 1 1 calc R . . C27 C 0.56895(19) 0.4811(4) 0.43027(17) 0.0535(13) Uani 1 1 d U . . H27A H 0.6032 0.4475 0.4535 0.080 Uiso 1 1 calc R . . H27B H 0.5564 0.5629 0.4425 0.080 Uiso 1 1 calc R . . H27C H 0.5857 0.4870 0.3946 0.080 Uiso 1 1 calc R . . C28 C 0.41164(16) 0.6241(3) 0.27694(13) 0.0233(8) Uani 1 1 d U . . H28 H 0.3683 0.6343 0.2586 0.028 Uiso 1 1 calc R . . C29 C 0.44089(18) 0.7525(3) 0.28542(14) 0.0329(9) Uani 1 1 d U . . H29A H 0.4109 0.8019 0.3064 0.049 Uiso 1 1 calc R . . H29B H 0.4472 0.7922 0.2514 0.049 Uiso 1 1 calc R . . H29C H 0.4832 0.7455 0.3039 0.049 Uiso 1 1 calc R . . C30 C 0.45569(17) 0.5486(3) 0.24119(14) 0.0307(9) Uani 1 1 d U . . H30A H 0.4994 0.5407 0.2574 0.046 Uiso 1 1 calc R . . H30B H 0.4593 0.5898 0.2072 0.046 Uiso 1 1 calc R . . H30C H 0.4366 0.4669 0.2361 0.046 Uiso 1 1 calc R . . C31 C 0.28440(16) 0.4276(3) 0.21067(12) 0.0197(8) Uani 1 1 d U . . C32 C 0.29513(16) 0.5121(3) 0.16910(13) 0.0211(8) Uani 1 1 d U . . C33 C 0.33993(16) 0.4834(3) 0.13058(13) 0.0256(8) Uani 1 1 d U . . H33 H 0.3464 0.5405 0.1030 0.031 Uiso 1 1 calc R . . C34 C 0.37587(16) 0.3748(3) 0.13043(14) 0.0250(8) Uani 1 1 d U . . C35 C 0.36541(16) 0.2947(3) 0.17131(14) 0.0257(8) Uani 1 1 d U . . H35 H 0.3897 0.2204 0.1723 0.031 Uiso 1 1 calc R . . C36 C 0.32153(16) 0.3169(3) 0.21086(13) 0.0225(8) Uani 1 1 d U . . C37 C 0.25690(16) 0.6318(3) 0.16380(13) 0.0264(8) Uani 1 1 d U . . H37 H 0.2342 0.6468 0.1976 0.032 Uiso 1 1 calc R . . C38 C 0.30165(18) 0.7425(3) 0.15337(14) 0.0342(10) Uani 1 1 d U . . H38A H 0.3377 0.7435 0.1792 0.051 Uiso 1 1 calc R . . H38B H 0.2762 0.8183 0.1562 0.051 Uiso 1 1 calc R . . H38C H 0.3196 0.7361 0.1181 0.051 Uiso 1 1 calc R . . C39 C 0.20460(18) 0.6227(3) 0.12078(14) 0.0387(10) Uani 1 1 d U . . H39A H 0.2252 0.5994 0.0878 0.058 Uiso 1 1 calc R . . H39B H 0.1828 0.7022 0.1165 0.058 Uiso 1 1 calc R . . H39C H 0.1722 0.5605 0.1303 0.058 Uiso 1 1 calc R . . C40 C 0.42301(18) 0.3461(3) 0.08734(14) 0.0329(9) Uani 1 1 d U . . H40 H 0.4455 0.2675 0.0966 0.040 Uiso 1 1 calc R . . C41 C 0.47555(19) 0.4436(4) 0.08176(17) 0.0511(12) Uani 1 1 d U . . H41A H 0.4551 0.5213 0.0711 0.077 Uiso 1 1 calc R . . H41B H 0.5069 0.4180 0.0552 0.077 Uiso 1 1 calc R . . H41C H 0.4986 0.4546 0.1154 0.077 Uiso 1 1 calc R . . C42 C 0.3874(2) 0.3268(4) 0.03568(15) 0.0575(13) Uani 1 1 d U . . H42A H 0.3550 0.2610 0.0394 0.086 Uiso 1 1 calc R . . H42B H 0.4190 0.3041 0.0088 0.086 Uiso 1 1 calc R . . H42C H 0.3650 0.4027 0.0253 0.086 Uiso 1 1 calc R . . C43 C 0.31518(17) 0.2214(3) 0.25393(14) 0.0276(9) Uani 1 1 d U . . H43 H 0.2766 0.2441 0.2756 0.033 Uiso 1 1 calc R . . C44 C 0.30313(19) 0.0927(3) 0.23213(15) 0.0394(10) Uani 1 1 d U . . H44A H 0.2652 0.0942 0.2081 0.059 Uiso 1 1 calc R . . H44B H 0.2945 0.0361 0.2610 0.059 Uiso 1 1 calc R . . H44C H 0.3420 0.0652 0.2132 0.059 Uiso 1 1 calc R . . C45 C 0.37624(17) 0.2219(3) 0.28991(14) 0.0323(9) Uani 1 1 d U . . H45A H 0.4154 0.2063 0.2691 0.048 Uiso 1 1 calc R . . H45B H 0.3720 0.1577 0.3165 0.048 Uiso 1 1 calc R . . H45C H 0.3803 0.3019 0.3071 0.048 Uiso 1 1 calc R . . C46 C 0.13342(16) 0.2069(3) 0.22016(13) 0.0256(8) Uani 1 1 d U A . C47 C 0.13093(17) 0.0661(3) 0.15546(15) 0.0282(9) Uani 1 1 d U . . C48 C 0.11842(17) 0.0069(3) 0.20053(15) 0.0285(9) Uani 1 1 d U A . C49 C 0.15125(17) 0.2929(3) 0.13193(14) 0.0288(9) Uani 1 1 d U . . H49 H 0.1643 0.3646 0.1542 0.035 Uiso 1 1 calc R A . C50 C 0.20768(18) 0.2712(4) 0.09458(14) 0.0396(10) Uani 1 1 d U A . H50A H 0.2455 0.2384 0.1141 0.059 Uiso 1 1 calc R . . H50B H 0.2198 0.3490 0.0781 0.059 Uiso 1 1 calc R . . H50C H 0.1940 0.2124 0.0675 0.059 Uiso 1 1 calc R . . C51 C 0.08759(18) 0.3288(3) 0.10442(15) 0.0404(10) Uani 1 1 d U A . H51A H 0.0738 0.2628 0.0806 0.061 Uiso 1 1 calc R . . H51B H 0.0943 0.4043 0.0844 0.061 Uiso 1 1 calc R . . H51C H 0.0536 0.3424 0.1305 0.061 Uiso 1 1 calc R . . C52 C 0.1345(2) 0.0140(3) 0.10160(15) 0.0445(11) Uani 1 1 d U A . H52A H 0.1803 0.0126 0.0905 0.067 Uiso 1 1 calc R . . H52B H 0.1086 0.0648 0.0774 0.067 Uiso 1 1 calc R . . H52C H 0.1170 -0.0698 0.1015 0.067 Uiso 1 1 calc R . . C53 C 0.1043(2) -0.1264(3) 0.20895(16) 0.0439(11) Uani 1 1 d U . . H53A H 0.1009 -0.1680 0.1750 0.066 Uiso 1 1 calc R A . H53B H 0.0629 -0.1352 0.2276 0.066 Uiso 1 1 calc R . . H53C H 0.1400 -0.1632 0.2298 0.066 Uiso 1 1 calc R . . C54A C 0.1081(2) 0.0829(4) 0.29742(19) 0.0292(11) Uani 0.85 1 d PDU A 1 H54A H 0.1193 0.1641 0.3134 0.035 Uiso 0.85 1 calc PR A 1 C56A C 0.1537(2) -0.0102(5) 0.3230(2) 0.0476(14) Uani 0.85 1 d PDU A 1 H56A H 0.1415 -0.0929 0.3112 0.071 Uiso 0.85 1 calc PR A 1 H56B H 0.1500 -0.0051 0.3611 0.071 Uiso 0.85 1 calc PR A 1 H56C H 0.1990 0.0071 0.3130 0.071 Uiso 0.85 1 calc PR A 1 C54B C 0.1099(7) 0.027(3) 0.2962(12) 0.0292(11) Uani 0.15 1 d PDU A 2 H54B H 0.1127 -0.0636 0.2905 0.035 Uiso 0.15 1 calc PR A 2 C56B C 0.1700(13) 0.067(3) 0.3287(12) 0.0476(14) Uani 0.15 1 d PDU A 2 H56D H 0.2099 0.0362 0.3125 0.071 Uiso 0.15 1 calc PR A 2 H56E H 0.1667 0.0348 0.3643 0.071 Uiso 0.15 1 calc PR A 2 H56F H 0.1717 0.1572 0.3300 0.071 Uiso 0.15 1 calc PR A 2 C55 C 0.03773(18) 0.0598(4) 0.30892(15) 0.0464(11) Uani 1 1 d DU . . H55A H 0.0230 -0.0143 0.2904 0.070 Uiso 0.85 1 calc PR A 1 H55B H 0.0114 0.1300 0.2972 0.070 Uiso 0.85 1 calc PR A 1 H55C H 0.0325 0.0484 0.3467 0.070 Uiso 0.85 1 calc PR A 1 H55D H 0.0084 -0.0035 0.2945 0.070 Uiso 0.15 1 calc PR A 2 H55E H 0.0266 0.1393 0.2933 0.070 Uiso 0.15 1 calc PR A 2 H55F H 0.0327 0.0642 0.3470 0.070 Uiso 0.15 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 0.0220(2) 0.0380(2) 0.0359(2) -0.0120(2) 0.00604(18) -0.0081(2) Cl1 0.0281(5) 0.0213(4) 0.0302(5) -0.0006(4) -0.0036(4) 0.0011(4) Si2 0.0175(5) 0.0222(5) 0.0243(5) -0.0016(4) -0.0009(4) 0.0009(4) Si1 0.0178(5) 0.0227(5) 0.0262(6) -0.0040(4) 0.0005(4) -0.0007(4) N1 0.0212(17) 0.0232(16) 0.0261(17) -0.0033(13) -0.0009(13) -0.0017(13) N2 0.0241(18) 0.0353(18) 0.0287(17) 0.0035(15) -0.0040(14) 0.0003(15) C1 0.0234(19) 0.0201(19) 0.026(2) -0.0004(15) -0.0036(16) 0.0097(15) C2 0.0231(19) 0.0220(19) 0.029(2) -0.0014(16) -0.0079(16) 0.0054(16) C3 0.030(2) 0.032(2) 0.030(2) -0.0055(17) -0.0068(17) 0.0062(18) C4 0.032(2) 0.039(2) 0.028(2) -0.0062(18) -0.0067(18) 0.0146(19) C5 0.022(2) 0.047(2) 0.033(2) -0.0082(19) -0.0017(17) 0.0099(19) C6 0.023(2) 0.035(2) 0.024(2) -0.0047(17) -0.0017(16) 0.0077(17) C7 0.022(2) 0.026(2) 0.032(2) -0.0018(17) -0.0079(17) 0.0047(17) C8 0.029(2) 0.032(2) 0.043(2) -0.0041(19) -0.0133(19) 0.0032(18) C9 0.036(2) 0.028(2) 0.045(3) -0.0045(18) -0.009(2) 0.0024(19) C10 0.037(2) 0.055(3) 0.025(2) -0.0103(19) -0.0022(18) 0.019(2) C11 0.047(3) 0.045(2) 0.038(2) -0.013(2) 0.001(2) 0.013(2) C12 0.059(3) 0.051(3) 0.036(2) 0.001(2) 0.004(2) 0.027(2) C13 0.020(2) 0.036(2) 0.031(2) -0.0097(17) 0.0022(17) 0.0004(17) C14 0.038(3) 0.058(3) 0.052(3) -0.022(2) -0.014(2) 0.012(2) C15 0.045(3) 0.064(3) 0.048(3) -0.016(2) 0.014(2) -0.015(2) C16 0.0234(19) 0.0148(17) 0.0247(19) -0.0030(15) -0.0010(15) -0.0009(15) C17 0.0199(19) 0.0196(18) 0.028(2) -0.0021(16) 0.0010(16) 0.0019(16) C18 0.025(2) 0.0218(19) 0.031(2) 0.0037(16) 0.0009(17) 0.0067(17) C19 0.0210(19) 0.0198(19) 0.033(2) -0.0002(16) -0.0052(17) 0.0060(16) C20 0.0177(19) 0.024(2) 0.034(2) 0.0013(17) -0.0015(16) 0.0000(16) C21 0.0193(19) 0.0185(18) 0.0243(19) -0.0013(15) 0.0013(15) 0.0001(15) C22 0.022(2) 0.028(2) 0.029(2) 0.0036(17) 0.0063(16) 0.0041(17) C23 0.036(2) 0.028(2) 0.045(3) 0.0055(19) 0.011(2) -0.0008(19) C24 0.030(2) 0.039(2) 0.038(2) 0.0046(19) 0.0088(19) 0.0019(19) C25 0.022(2) 0.036(2) 0.042(2) 0.0087(19) -0.0031(18) 0.0083(18) C26 0.047(3) 0.038(3) 0.128(5) -0.009(3) -0.029(3) 0.019(2) C27 0.036(3) 0.048(3) 0.076(3) 0.013(2) -0.032(2) -0.004(2) C28 0.0177(19) 0.0231(19) 0.029(2) 0.0024(16) -0.0019(15) -0.0042(16) C29 0.037(2) 0.027(2) 0.036(2) 0.0035(17) 0.0018(19) -0.0052(18) C30 0.027(2) 0.033(2) 0.032(2) -0.0007(18) 0.0048(17) -0.0059(18) C31 0.0166(18) 0.0215(18) 0.0209(19) -0.0052(15) -0.0041(15) -0.0017(15) C32 0.022(2) 0.0179(18) 0.0232(19) -0.0044(15) -0.0030(15) -0.0021(15) C33 0.027(2) 0.024(2) 0.026(2) 0.0007(16) 0.0012(16) -0.0067(16) C34 0.0203(19) 0.025(2) 0.030(2) -0.0078(17) 0.0010(16) -0.0032(16) C35 0.020(2) 0.0189(19) 0.039(2) -0.0041(17) 0.0024(17) 0.0046(16) C36 0.0189(19) 0.0192(18) 0.029(2) -0.0014(15) -0.0001(16) -0.0020(15) C37 0.028(2) 0.0239(19) 0.028(2) 0.0001(17) -0.0025(16) 0.0001(17) C38 0.045(3) 0.023(2) 0.035(2) 0.0026(18) 0.0028(19) 0.0006(18) C39 0.044(3) 0.030(2) 0.041(2) -0.0041(19) -0.012(2) 0.0088(19) C40 0.037(2) 0.026(2) 0.035(2) -0.0044(18) 0.0106(18) -0.0011(18) C41 0.036(3) 0.045(3) 0.073(3) -0.010(2) 0.026(2) -0.001(2) C42 0.056(3) 0.078(3) 0.039(3) -0.022(2) 0.011(2) 0.004(3) C43 0.024(2) 0.0221(19) 0.037(2) 0.0017(17) 0.0048(17) 0.0040(17) C44 0.039(3) 0.027(2) 0.052(3) 0.0042(19) 0.003(2) -0.0041(19) C45 0.036(2) 0.027(2) 0.033(2) 0.0052(17) 0.0020(18) 0.0046(18) C46 0.0167(19) 0.036(2) 0.024(2) -0.0008(17) 0.0005(16) -0.0058(17) C47 0.023(2) 0.025(2) 0.037(2) -0.0054(17) -0.0036(18) -0.0035(17) C48 0.024(2) 0.0222(19) 0.039(2) 0.0007(18) -0.0054(18) 0.0022(17) C49 0.032(2) 0.026(2) 0.028(2) 0.0019(17) 0.0013(17) -0.0071(17) C50 0.037(2) 0.049(3) 0.033(2) -0.003(2) 0.0070(19) -0.012(2) C51 0.038(2) 0.043(2) 0.041(3) 0.011(2) -0.006(2) -0.005(2) C52 0.055(3) 0.036(2) 0.043(2) -0.014(2) 0.004(2) -0.005(2) C53 0.047(3) 0.028(2) 0.057(3) 0.004(2) -0.001(2) 0.004(2) C54A 0.029(2) 0.028(3) 0.031(2) 0.009(3) -0.0006(19) -0.005(2) C56A 0.043(3) 0.062(4) 0.039(3) 0.010(3) 0.000(2) 0.021(3) C54B 0.029(2) 0.028(3) 0.031(2) 0.009(3) -0.0006(19) -0.005(2) C56B 0.043(3) 0.062(4) 0.039(3) 0.010(3) 0.000(2) 0.021(3) C55 0.031(2) 0.069(3) 0.039(3) 0.003(2) 0.0043(19) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 C46 2.061(4) . ? Ge1 Si1 2.2757(10) . ? Cl1 Si2 2.1179(13) . ? Si2 C16 1.904(3) . ? Si2 C1 1.913(4) . ? Si2 Si1 2.3776(13) . ? Si1 C31 1.909(3) . ? N1 C46 1.343(4) . ? N1 C47 1.396(4) . ? N1 C49 1.484(4) . ? N2 C46 1.356(4) . ? N2 C48 1.397(4) . ? N2 C54A 1.486(5) . ? N2 C54B 1.62(3) . ? C1 C6 1.416(5) . ? C1 C2 1.423(4) . ? C2 C3 1.389(5) . ? C2 C7 1.526(5) . ? C3 C4 1.382(5) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 C10 1.515(5) . ? C5 C6 1.381(5) . ? C5 H5 0.9500 . ? C6 C13 1.515(5) . ? C7 C9 1.530(4) . ? C7 C8 1.540(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.513(5) . ? C10 C11 1.520(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.525(5) . ? C13 C14 1.533(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.413(4) . ? C16 C21 1.419(4) . ? C17 C18 1.390(4) . ? C17 C22 1.533(5) . ? C18 C19 1.391(5) . ? C18 H18 0.9500 . ? C19 C20 1.379(5) . ? C19 C25 1.521(4) . ? C20 C21 1.394(4) . ? C20 H20 0.9500 . ? C21 C28 1.524(4) . ? C22 C24 1.522(5) . ? C22 C23 1.538(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.493(5) . ? C25 C27 1.519(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.530(4) . ? C28 C29 1.536(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.424(4) . ? C31 C36 1.424(4) . ? C32 C33 1.387(4) . ? C32 C37 1.525(4) . ? C33 C34 1.392(4) . ? C33 H33 0.9500 . ? C34 C35 1.380(5) . ? C34 C40 1.504(5) . ? C35 C36 1.380(5) . ? C35 H35 0.9500 . ? C36 C43 1.522(5) . ? C37 C39 1.522(4) . ? C37 C38 1.538(4) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.511(5) . ? C40 C41 1.517(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.528(4) . ? C43 C45 1.536(5) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.347(5) . ? C47 C52 1.491(5) . ? C48 C53 1.497(5) . ? C49 C51 1.518(5) . ? C49 C50 1.523(5) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54A C55 1.490(5) . ? C54A C56A 1.516(5) . ? C54A H54A 1.0000 . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C54B C56B 1.534(16) . ? C54B C55 1.552(15) . ? C54B H54B 1.0000 . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C55 H55D 0.9800 . ? C55 H55E 0.9800 . ? C55 H55F 0.9800 . ? 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 C46 Ge1 Si1 101.90(10) . . ? C16 Si2 C1 107.61(14) . . ? C16 Si2 Cl1 112.14(11) . . ? C1 Si2 Cl1 95.51(11) . . ? C16 Si2 Si1 104.32(10) . . ? C1 Si2 Si1 129.50(11) . . ? Cl1 Si2 Si1 107.39(5) . . ? C31 Si1 Ge1 127.00(10) . . ? C31 Si1 Si2 108.26(10) . . ? Ge1 Si1 Si2 124.54(5) . . ? C46 N1 C47 110.8(3) . . ? C46 N1 C49 121.8(3) . . ? C47 N1 C49 127.2(3) . . ? C46 N2 C48 110.1(3) . . ? C46 N2 C54A 119.2(3) . . ? C48 N2 C54A 130.6(3) . . ? C46 N2 C54B 140.7(10) . . ? C48 N2 C54B 109.0(10) . . ? C54A N2 C54B 22.1(9) . . ? C6 C1 C2 117.1(3) . . ? C6 C1 Si2 123.7(3) . . ? C2 C1 Si2 119.1(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 C7 115.8(3) . . ? C1 C2 C7 124.4(3) . . ? C4 C3 C2 122.8(3) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C5 C4 C3 117.0(3) . . ? C5 C4 C10 122.5(4) . . ? C3 C4 C10 120.3(3) . . ? C4 C5 C6 123.0(4) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C13 117.1(3) . . ? C1 C6 C13 122.7(3) . . ? C2 C7 C9 111.9(3) . . ? C2 C7 C8 110.7(3) . . ? C9 C7 C8 109.9(3) . . ? C2 C7 H7 108.1 . . ? C9 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C4 112.6(3) . . ? C12 C10 C11 112.1(3) . . ? C4 C10 C11 109.0(3) . . ? C12 C10 H10 107.6 . . ? C4 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C15 112.7(3) . . ? C6 C13 C14 111.6(3) . . ? C15 C13 C14 111.0(3) . . ? C6 C13 H13 107.1 . . ? C15 C13 H13 107.1 . . ? C14 C13 H13 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 117.6(3) . . ? C17 C16 Si2 116.6(2) . . ? C21 C16 Si2 125.8(2) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 C22 116.8(3) . . ? C16 C17 C22 122.9(3) . . ? C17 C18 C19 122.1(3) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 117.3(3) . . ? C20 C19 C25 122.7(3) . . ? C18 C19 C25 119.8(3) . . ? C19 C20 C21 122.8(3) . . ? C19 C20 H20 118.6 . . ? C21 C20 H20 118.6 . . ? C20 C21 C16 119.5(3) . . ? C20 C21 C28 117.1(3) . . ? C16 C21 C28 123.4(3) . . ? C24 C22 C17 113.4(3) . . ? C24 C22 C23 110.9(3) . . ? C17 C22 C23 110.4(3) . . ? C24 C22 H22 107.3 . . ? C17 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.3(3) . . ? C26 C25 C19 110.0(3) . . ? C27 C25 C19 114.3(3) . . ? C26 C25 H25 106.9 . . ? C27 C25 H25 106.9 . . ? C19 C25 H25 106.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C30 111.7(3) . . ? C21 C28 C29 112.0(3) . . ? C30 C28 C29 110.2(3) . . ? C21 C28 H28 107.6 . . ? C30 C28 H28 107.6 . . ? C29 C28 H28 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 117.6(3) . . ? C32 C31 Si1 119.7(2) . . ? C36 C31 Si1 122.5(2) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 C37 118.1(3) . . ? C31 C32 C37 122.4(3) . . ? C32 C33 C34 123.0(3) . . ? C32 C33 H33 118.5 . . ? C34 C33 H33 118.5 . . ? C35 C34 C33 116.7(3) . . ? C35 C34 C40 121.9(3) . . ? C33 C34 C40 121.4(3) . . ? C36 C35 C34 123.5(3) . . ? C36 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C35 C36 C31 119.7(3) . . ? C35 C36 C43 118.1(3) . . ? C31 C36 C43 122.1(3) . . ? C39 C37 C32 111.1(3) . . ? C39 C37 C38 109.7(3) . . ? C32 C37 C38 112.5(3) . . ? C39 C37 H37 107.8 . . ? C32 C37 H37 107.8 . . ? C38 C37 H37 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 C42 111.3(3) . . ? C34 C40 C41 112.5(3) . . ? C42 C40 C41 110.3(3) . . ? C34 C40 H40 107.5 . . ? C42 C40 H40 107.5 . . ? C41 C40 H40 107.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C36 C43 C44 112.4(3) . . ? C36 C43 C45 110.7(3) . . ? C44 C43 C45 110.2(3) . . ? C36 C43 H43 107.8 . . ? C44 C43 H43 107.8 . . ? C45 C43 H43 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N1 C46 N2 105.6(3) . . ? N1 C46 Ge1 132.1(3) . . ? N2 C46 Ge1 120.2(2) . . ? C48 C47 N1 106.6(3) . . ? C48 C47 C52 128.2(3) . . ? N1 C47 C52 125.3(3) . . ? C47 C48 N2 106.9(3) . . ? C47 C48 C53 128.8(3) . . ? N2 C48 C53 124.3(3) . . ? N1 C49 C51 110.5(3) . . ? N1 C49 C50 113.4(3) . . ? C51 C49 C50 113.5(3) . . ? N1 C49 H49 106.2 . . ? C51 C49 H49 106.2 . . ? C50 C49 H49 106.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54A C55 112.5(3) . . ? N2 C54A C56A 111.7(4) . . ? C55 C54A C56A 112.8(4) . . ? N2 C54A H54A 106.4 . . ? C55 C54A H54A 106.4 . . ? C56A C54A H54A 106.4 . . ? C56B C54B C55 125(2) . . ? C56B C54B N2 103.4(18) . . ? C55 C54B N2 102.5(14) . . ? C56B C54B H54B 108.3 . . ? C55 C54B H54B 108.3 . . ? N2 C54B H54B 108.3 . . ? C54B C56B H56D 109.5 . . ? C54B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C54B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C54A C55 C54B 23.0(10) . . ? C54A C55 H55A 109.5 . . ? C54B C55 H55A 89.7 . . ? C54A C55 H55B 109.5 . . ? C54B C55 H55B 129.2 . . ? H55A C55 H55B 109.5 . . ? C54A C55 H55C 109.5 . . ? C54B C55 H55C 107.1 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54A C55 H55D 128.9 . . ? C54B C55 H55D 109.5 . . ? H55A C55 H55D 19.8 . . ? H55B C55 H55D 96.1 . . ? H55C C55 H55D 101.9 . . ? C54A C55 H55E 89.4 . . ? C54B C55 H55E 109.5 . . ? H55A C55 H55E 117.7 . . ? H55B C55 H55E 20.1 . . ? H55C C55 H55E 119.0 . . ? H55D C55 H55E 109.5 . . ? C54A C55 H55F 107.6 . . ? C54B C55 H55F 109.5 . . ? H55A C55 H55F 118.8 . . ? H55B C55 H55F 101.5 . . ? H55C C55 H55F 10.1 . . ? H55D C55 H55F 109.5 . . ? H55E C55 H55F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.827 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.083 _database_code_depnum_ccdc_archive 'CCDC 953520' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sh3315 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H89 Cl Fe Ge N2 O3 Si2' _chemical_formula_sum 'C59 H89 Cl Fe Ge N2 O3 Si2' _chemical_formula_weight 1094.39 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.6288(5) _cell_length_b 24.6607(7) _cell_length_c 24.6974(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11955.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 132(2) _cell_measurement_reflns_used 9402 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.88 _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6026 _exptl_absorpt_correction_T_max 0.8448 _exptl_absorpt_process_details 'SADABS, BrukerAXS 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 132(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 104743 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.92 _reflns_number_total 14312 _reflns_number_gt 10361 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0461P)^2^+14.1786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14312 _refine_ls_number_parameters 646 _refine_ls_number_restraints 200 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.016 _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 0.011992(12) 0.175229(10) 0.550710(10) 0.01603(7) Uani 1 1 d U . . Fe1 Fe -0.102888(16) 0.181745(14) 0.609556(14) 0.01869(8) Uani 1 1 d U . . Cl1 Cl -0.02090(4) 0.04208(3) 0.60283(3) 0.03457(16) Uani 1 1 d U . . Si1 Si -0.03538(3) 0.25699(3) 0.58620(3) 0.01616(13) Uani 1 1 d U . . Si2 Si -0.01226(4) 0.12434(3) 0.62757(3) 0.02128(15) Uani 1 1 d U . . N1 N -0.05130(10) 0.10930(8) 0.45377(8) 0.0194(4) Uani 1 1 d U . . N2 N 0.05267(10) 0.13635(8) 0.44142(8) 0.0183(4) Uani 1 1 d U . . O1 O -0.17919(11) 0.08020(9) 0.61036(10) 0.0457(6) Uani 1 1 d U . . O2 O -0.16178(11) 0.22231(10) 0.71004(9) 0.0489(6) Uani 1 1 d U . . O3 O -0.20384(9) 0.23471(9) 0.54023(9) 0.0361(5) Uani 1 1 d U . . C1 C -0.07423(12) 0.31352(10) 0.54242(10) 0.0198(5) Uani 1 1 d U . . C2 C -0.08270(12) 0.31231(11) 0.48493(11) 0.0233(5) Uani 1 1 d U . . C3 C -0.10188(13) 0.35910(11) 0.45728(11) 0.0285(6) Uani 1 1 d U . . H3 H -0.1060 0.3575 0.4190 0.034 Uiso 1 1 calc R . . C4 C -0.11514(14) 0.40748(11) 0.48282(12) 0.0311(6) Uani 1 1 d U . . C5 C -0.11206(14) 0.40765(11) 0.53887(12) 0.0313(6) Uani 1 1 d U . . H5 H -0.1236 0.4400 0.5576 0.038 Uiso 1 1 calc R . . C6 C -0.09264(12) 0.36207(11) 0.56900(11) 0.0243(5) Uani 1 1 d U . . C7 C -0.07321(13) 0.26188(11) 0.45044(11) 0.0257(5) Uani 1 1 d U . . H7 H -0.0681 0.2301 0.4753 0.031 Uiso 1 1 calc R . . C8 C -0.13494(15) 0.25117(13) 0.41359(12) 0.0366(7) Uani 1 1 d U . . H8A H -0.1766 0.2505 0.4355 0.055 Uiso 1 1 calc R . . H8B H -0.1292 0.2162 0.3954 0.055 Uiso 1 1 calc R . . H8C H -0.1383 0.2800 0.3865 0.055 Uiso 1 1 calc R . . C9 C -0.00902(14) 0.26541(12) 0.41548(12) 0.0323(6) Uani 1 1 d U . . H9A H -0.0117 0.2975 0.3922 0.048 Uiso 1 1 calc R . . H9B H -0.0054 0.2328 0.3930 0.048 Uiso 1 1 calc R . . H9C H 0.0311 0.2682 0.4389 0.048 Uiso 1 1 calc R . . C10 C -0.13200(15) 0.45724(12) 0.44894(13) 0.0367(7) Uani 1 1 d U . . H10 H -0.1527 0.4434 0.4146 0.044 Uiso 1 1 calc R . . C11 C -0.06745(16) 0.48625(13) 0.43276(15) 0.0419(8) Uani 1 1 d U . . H11A H -0.0442 0.4995 0.4653 0.063 Uiso 1 1 calc R . . H11B H -0.0787 0.5169 0.4092 0.063 Uiso 1 1 calc R . . H11C H -0.0375 0.4611 0.4133 0.063 Uiso 1 1 calc R . . C12 C -0.18448(15) 0.49331(12) 0.47450(14) 0.0383(7) Uani 1 1 d U . . H12A H -0.2256 0.4722 0.4823 0.057 Uiso 1 1 calc R . . H12B H -0.1958 0.5229 0.4496 0.057 Uiso 1 1 calc R . . H12C H -0.1663 0.5084 0.5083 0.057 Uiso 1 1 calc R . . C13 C -0.09734(13) 0.36570(11) 0.63014(11) 0.0269(6) Uani 1 1 d U . . H13 H -0.0809 0.3304 0.6451 0.032 Uiso 1 1 calc R . . C14 C -0.17207(14) 0.37226(14) 0.64751(13) 0.0393(7) Uani 1 1 d U . . H14A H -0.1893 0.4074 0.6349 0.059 Uiso 1 1 calc R . . H14B H -0.1752 0.3706 0.6871 0.059 Uiso 1 1 calc R . . H14C H -0.1994 0.3430 0.6317 0.059 Uiso 1 1 calc R . . C15 C -0.05226(16) 0.41022(12) 0.65375(13) 0.0374(7) Uani 1 1 d U . . H15A H -0.0047 0.4034 0.6438 0.056 Uiso 1 1 calc R . . H15B H -0.0566 0.4104 0.6933 0.056 Uiso 1 1 calc R . . H15C H -0.0665 0.4455 0.6393 0.056 Uiso 1 1 calc R . . C16 C 0.03805(12) 0.29215(10) 0.62553(10) 0.0195(5) Uani 1 1 d U . . C17 C 0.08618(12) 0.32109(10) 0.59388(10) 0.0215(5) Uani 1 1 d U . . C18 C 0.13701(13) 0.35216(12) 0.61840(11) 0.0295(6) Uani 1 1 d U . . H18 H 0.1682 0.3714 0.5961 0.035 Uiso 1 1 calc R . . C19 C 0.14350(14) 0.35586(13) 0.67396(12) 0.0346(7) Uani 1 1 d U . . C20 C 0.09787(13) 0.32654(12) 0.70468(11) 0.0315(6) Uani 1 1 d U . . H20 H 0.1019 0.3281 0.7430 0.038 Uiso 1 1 calc R . . C21 C 0.04588(12) 0.29459(11) 0.68260(11) 0.0236(5) Uani 1 1 d U . . C22 C 0.08846(12) 0.31854(10) 0.53252(10) 0.0216(5) Uani 1 1 d U . . H22 H 0.0508 0.2940 0.5204 0.026 Uiso 1 1 calc R . . C23 C 0.07692(14) 0.37397(11) 0.50596(12) 0.0310(6) Uani 1 1 d U . . H23A H 0.0337 0.3893 0.5187 0.047 Uiso 1 1 calc R . . H23B H 0.0753 0.3697 0.4665 0.047 Uiso 1 1 calc R . . H23C H 0.1144 0.3984 0.5156 0.047 Uiso 1 1 calc R . . C24 C 0.15563(13) 0.29361(12) 0.51330(11) 0.0289(6) Uani 1 1 d U . . H24A H 0.1935 0.3175 0.5233 0.043 Uiso 1 1 calc R . . H24B H 0.1545 0.2893 0.4739 0.043 Uiso 1 1 calc R . . H24C H 0.1619 0.2581 0.5304 0.043 Uiso 1 1 calc R . . C25 C 0.20249(17) 0.38594(16) 0.70086(13) 0.0503(9) Uani 1 1 d U . . H25 H 0.1897 0.3917 0.7396 0.060 Uiso 1 1 calc R . . C26 C 0.21605(18) 0.44123(15) 0.67654(16) 0.0589(10) Uani 1 1 d U . . H26A H 0.2320 0.4370 0.6392 0.088 Uiso 1 1 calc R . . H26B H 0.2510 0.4599 0.6979 0.088 Uiso 1 1 calc R . . H26C H 0.1740 0.4626 0.6768 0.088 Uiso 1 1 calc R . . C27 C 0.26566(17) 0.34946(17) 0.70025(15) 0.0564(10) Uani 1 1 d U . . H27A H 0.2560 0.3159 0.7201 0.085 Uiso 1 1 calc R . . H27B H 0.3038 0.3684 0.7175 0.085 Uiso 1 1 calc R . . H27C H 0.2776 0.3407 0.6627 0.085 Uiso 1 1 calc R . . C28 C 0.00317(13) 0.26334(12) 0.72373(10) 0.0271(6) Uani 1 1 d U . . H28 H -0.0242 0.2356 0.7038 0.033 Uiso 1 1 calc R . . C29 C -0.04654(15) 0.30031(13) 0.75498(12) 0.0353(7) Uani 1 1 d U . . H29A H -0.0210 0.3295 0.7726 0.053 Uiso 1 1 calc R . . H29B H -0.0705 0.2790 0.7825 0.053 Uiso 1 1 calc R . . H29C H -0.0797 0.3159 0.7297 0.053 Uiso 1 1 calc R . . C30 C 0.04814(16) 0.23379(13) 0.76512(12) 0.0375(7) Uani 1 1 d U . . H30A H 0.0847 0.2145 0.7462 0.056 Uiso 1 1 calc R . . H30B H 0.0204 0.2078 0.7855 0.056 Uiso 1 1 calc R . . H30C H 0.0680 0.2602 0.7902 0.056 Uiso 1 1 calc R . . C31 C 0.04523(15) 0.11517(12) 0.68878(11) 0.0306(6) Uani 1 1 d U . . C32 C 0.11717(16) 0.12125(15) 0.68731(12) 0.0417(8) Uani 1 1 d U . . C33 C 0.15524(17) 0.11430(15) 0.73458(13) 0.0473(9) Uani 1 1 d U . . H33 H 0.2032 0.1194 0.7329 0.057 Uiso 1 1 calc R . . C34 C 0.12673(18) 0.10046(14) 0.78313(13) 0.0425(8) Uani 1 1 d U . . C35 C 0.05724(19) 0.09171(13) 0.78400(12) 0.0431(8) Uani 1 1 d U . . H35 H 0.0367 0.0803 0.8169 0.052 Uiso 1 1 calc R . . C36 C 0.01532(16) 0.09910(12) 0.73791(12) 0.0353(7) Uani 1 1 d U . . C37 C 0.15709(16) 0.1347(2) 0.63686(14) 0.0670(13) Uani 1 1 d U . . H37 H 0.1242 0.1361 0.6060 0.080 Uiso 1 1 calc R . . C38 C 0.1904(2) 0.1902(2) 0.6412(2) 0.0917(17) Uani 1 1 d U . . H38A H 0.1552 0.2179 0.6465 0.138 Uiso 1 1 calc R . . H38B H 0.2156 0.1980 0.6079 0.138 Uiso 1 1 calc R . . H38C H 0.2218 0.1906 0.6721 0.138 Uiso 1 1 calc R . . C39 C 0.20984(19) 0.0906(2) 0.62398(16) 0.0729(14) Uani 1 1 d U . . H39A H 0.2432 0.0886 0.6534 0.109 Uiso 1 1 calc R . . H39B H 0.2332 0.0995 0.5900 0.109 Uiso 1 1 calc R . . H39C H 0.1868 0.0555 0.6203 0.109 Uiso 1 1 calc R . . C40 C 0.17122(19) 0.09867(16) 0.83392(14) 0.0499(9) Uani 1 1 d U . . H40 H 0.2190 0.0923 0.8214 0.060 Uiso 1 1 calc R . . C41 C 0.17112(19) 0.15137(19) 0.86212(15) 0.0615(11) Uani 1 1 d U . . H41A H 0.1888 0.1795 0.8378 0.092 Uiso 1 1 calc R . . H41B H 0.2000 0.1491 0.8944 0.092 Uiso 1 1 calc R . . H41C H 0.1245 0.1606 0.8729 0.092 Uiso 1 1 calc R . . C42 C 0.1538(2) 0.05308(19) 0.87037(18) 0.0750(13) Uani 1 1 d U . . H42A H 0.1826 0.0546 0.9027 0.112 Uiso 1 1 calc R . . H42B H 0.1614 0.0186 0.8515 0.112 Uiso 1 1 calc R . . H42C H 0.1058 0.0558 0.8810 0.112 Uiso 1 1 calc R . . C43 C -0.06014(18) 0.08712(14) 0.74230(12) 0.0439(8) Uani 1 1 d U . . H43 H -0.0818 0.0978 0.7072 0.053 Uiso 1 1 calc R . . C44 C -0.09534(19) 0.11902(17) 0.78742(14) 0.0570(10) Uani 1 1 d U . . H44A H -0.0769 0.1079 0.8226 0.085 Uiso 1 1 calc R . . H44B H -0.1444 0.1118 0.7865 0.085 Uiso 1 1 calc R . . H44C H -0.0873 0.1579 0.7821 0.085 Uiso 1 1 calc R . . C45 C -0.0718(3) 0.02626(16) 0.75015(19) 0.0786(14) Uani 1 1 d U . . H45A H -0.0446 0.0060 0.7237 0.118 Uiso 1 1 calc R . . H45B H -0.1202 0.0180 0.7449 0.118 Uiso 1 1 calc R . . H45C H -0.0581 0.0158 0.7868 0.118 Uiso 1 1 calc R . . C46 C 0.00064(11) 0.13616(10) 0.47785(10) 0.0177(5) Uani 1 1 d U . . C47 C -0.03272(13) 0.09397(10) 0.40163(10) 0.0224(5) Uani 1 1 d U . . C48 C 0.03305(13) 0.10978(10) 0.39439(10) 0.0216(5) Uani 1 1 d U . . C49 C -0.11247(12) 0.09070(10) 0.48374(11) 0.0236(5) Uani 1 1 d U . . H49 H -0.1065 0.1030 0.5220 0.028 Uiso 1 1 calc R . . C50 C -0.17815(13) 0.11619(13) 0.46359(13) 0.0360(7) Uani 1 1 d U . . H50A H -0.1740 0.1558 0.4647 0.054 Uiso 1 1 calc R . . H50B H -0.2160 0.1047 0.4868 0.054 Uiso 1 1 calc R . . H50C H -0.1868 0.1045 0.4263 0.054 Uiso 1 1 calc R . . C51 C -0.11621(14) 0.02866(11) 0.48537(13) 0.0344(7) Uani 1 1 d U . . H51A H -0.1318 0.0151 0.4502 0.052 Uiso 1 1 calc R . . H51B H -0.1482 0.0174 0.5136 0.052 Uiso 1 1 calc R . . H51C H -0.0710 0.0139 0.4933 0.052 Uiso 1 1 calc R . . C52 C -0.07905(14) 0.06756(12) 0.36114(12) 0.0323(6) Uani 1 1 d U . . H52A H -0.0572 0.0677 0.3254 0.048 Uiso 1 1 calc R . . H52B H -0.1221 0.0877 0.3593 0.048 Uiso 1 1 calc R . . H52C H -0.0881 0.0301 0.3722 0.048 Uiso 1 1 calc R . . C53 C 0.07719(15) 0.09934(12) 0.34641(11) 0.0328(6) Uani 1 1 d U . . H53A H 0.0523 0.0771 0.3201 0.049 Uiso 1 1 calc R . . H53B H 0.1184 0.0801 0.3579 0.049 Uiso 1 1 calc R . . H53C H 0.0899 0.1339 0.3297 0.049 Uiso 1 1 calc R . . C54 C 0.12179(12) 0.15742(11) 0.45402(11) 0.0232(5) Uani 1 1 d U . . H54 H 0.1165 0.1828 0.4853 0.028 Uiso 1 1 calc R . . C55 C 0.15416(13) 0.18978(11) 0.40858(12) 0.0293(6) Uani 1 1 d U . . H55A H 0.1697 0.1650 0.3801 0.044 Uiso 1 1 calc R . . H55B H 0.1931 0.2102 0.4227 0.044 Uiso 1 1 calc R . . H55C H 0.1206 0.2150 0.3935 0.044 Uiso 1 1 calc R . . C56 C 0.16710(14) 0.11137(13) 0.47341(13) 0.0354(7) Uani 1 1 d U . . H56A H 0.1458 0.0935 0.5046 0.053 Uiso 1 1 calc R . . H56B H 0.2116 0.1259 0.4840 0.053 Uiso 1 1 calc R . . H56C H 0.1731 0.0850 0.4441 0.053 Uiso 1 1 calc R . . C57 C -0.14751(13) 0.11957(11) 0.60973(12) 0.0293(6) Uani 1 1 d U . . C58 C -0.13492(13) 0.20677(11) 0.67174(12) 0.0291(6) Uani 1 1 d U . . C59 C -0.16201(12) 0.21456(11) 0.56584(11) 0.0249(6) Uani 1 1 d U . . 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 0.01541(11) 0.01664(12) 0.01604(12) -0.00089(10) 0.00124(10) 0.00063(10) Fe1 0.01509(15) 0.01894(18) 0.02205(18) -0.00250(14) 0.00437(13) -0.00107(13) Cl1 0.0492(4) 0.0185(3) 0.0360(4) 0.0008(3) 0.0065(3) 0.0053(3) Si1 0.0147(3) 0.0158(3) 0.0180(3) -0.0009(3) 0.0005(2) 0.0007(2) Si2 0.0251(3) 0.0194(3) 0.0194(3) 0.0018(3) 0.0049(3) 0.0030(3) N1 0.0188(9) 0.0190(10) 0.0203(11) -0.0034(8) -0.0013(8) -0.0006(8) N2 0.0195(9) 0.0172(10) 0.0181(10) -0.0004(8) 0.0019(8) 0.0007(8) O1 0.0380(11) 0.0328(12) 0.0665(16) -0.0111(11) 0.0233(11) -0.0159(10) O2 0.0381(12) 0.0679(16) 0.0406(13) -0.0226(12) 0.0173(10) -0.0051(11) O3 0.0190(9) 0.0430(12) 0.0462(13) 0.0018(10) -0.0069(9) 0.0015(9) C1 0.0165(10) 0.0168(12) 0.0260(13) 0.0025(10) 0.0027(10) 0.0022(9) C2 0.0184(11) 0.0261(14) 0.0254(13) 0.0038(11) 0.0016(10) 0.0025(10) C3 0.0281(13) 0.0301(14) 0.0273(14) 0.0069(11) 0.0049(11) 0.0088(11) C4 0.0297(14) 0.0272(14) 0.0365(16) 0.0091(12) 0.0054(12) 0.0066(12) C5 0.0295(14) 0.0216(14) 0.0430(17) 0.0006(12) 0.0085(12) 0.0081(11) C6 0.0194(11) 0.0220(13) 0.0315(14) -0.0004(11) 0.0046(10) 0.0015(10) C7 0.0289(13) 0.0275(14) 0.0207(13) 0.0012(11) -0.0040(11) 0.0057(11) C8 0.0353(15) 0.0409(17) 0.0335(16) -0.0002(14) -0.0083(13) 0.0001(14) C9 0.0308(14) 0.0397(17) 0.0264(14) -0.0046(13) 0.0009(12) 0.0087(13) C10 0.0378(15) 0.0288(15) 0.0434(18) 0.0082(13) 0.0003(14) 0.0067(13) C11 0.0392(16) 0.0303(16) 0.056(2) 0.0098(15) 0.0038(15) 0.0006(13) C12 0.0360(15) 0.0282(16) 0.051(2) 0.0091(14) -0.0002(14) 0.0081(13) C13 0.0262(13) 0.0205(13) 0.0340(15) -0.0033(11) 0.0034(11) 0.0041(11) C14 0.0299(14) 0.052(2) 0.0358(17) -0.0044(15) 0.0069(13) 0.0118(14) C15 0.0407(16) 0.0252(15) 0.0462(19) -0.0105(13) -0.0019(14) 0.0009(13) C16 0.0162(10) 0.0190(12) 0.0233(13) -0.0051(10) 0.0003(9) 0.0008(9) C17 0.0176(11) 0.0214(13) 0.0256(13) -0.0063(10) 0.0010(10) 0.0010(10) C18 0.0233(12) 0.0328(15) 0.0322(15) -0.0102(12) 0.0062(11) -0.0099(11) C19 0.0248(13) 0.0459(18) 0.0330(16) -0.0148(14) 0.0004(12) -0.0101(12) C20 0.0278(13) 0.0451(18) 0.0216(13) -0.0108(12) 0.0004(11) -0.0047(13) C21 0.0201(12) 0.0261(14) 0.0247(13) -0.0060(11) 0.0020(10) 0.0007(10) C22 0.0218(11) 0.0190(12) 0.0240(13) -0.0054(10) 0.0035(10) -0.0060(10) C23 0.0345(14) 0.0254(14) 0.0333(16) 0.0024(12) 0.0078(12) -0.0054(12) C24 0.0227(12) 0.0335(15) 0.0304(15) -0.0084(12) 0.0048(11) -0.0043(11) C25 0.0422(17) 0.079(3) 0.0295(17) -0.0189(17) 0.0040(14) -0.0313(18) C26 0.0459(19) 0.061(2) 0.069(3) -0.034(2) 0.0058(18) -0.0193(18) C27 0.0380(17) 0.086(3) 0.045(2) 0.013(2) -0.0170(15) -0.0241(18) C28 0.0284(13) 0.0346(15) 0.0183(13) -0.0026(11) 0.0022(10) -0.0022(11) C29 0.0355(15) 0.0465(18) 0.0239(15) -0.0058(13) 0.0080(12) -0.0027(14) C30 0.0450(17) 0.0410(18) 0.0265(15) -0.0003(13) -0.0037(13) 0.0007(14) C31 0.0403(15) 0.0294(15) 0.0220(14) 0.0019(11) 0.0020(12) 0.0112(12) C32 0.0375(16) 0.063(2) 0.0243(15) 0.0050(15) -0.0024(12) 0.0236(15) C33 0.0432(18) 0.070(2) 0.0286(16) 0.0002(16) -0.0044(14) 0.0239(17) C34 0.0519(19) 0.0456(19) 0.0300(16) 0.0033(14) -0.0081(14) 0.0193(16) C35 0.072(2) 0.0390(18) 0.0179(14) 0.0054(13) 0.0042(14) 0.0065(17) C36 0.0520(17) 0.0294(15) 0.0244(14) 0.0036(12) 0.0062(13) 0.0076(14) C37 0.0269(16) 0.143(4) 0.0309(18) 0.021(2) 0.0005(14) 0.029(2) C38 0.066(3) 0.109(4) 0.100(4) 0.055(3) 0.035(3) 0.042(3) C39 0.0403(19) 0.137(4) 0.042(2) -0.025(2) -0.0017(17) 0.021(2) C40 0.052(2) 0.063(2) 0.0349(18) 0.0093(16) -0.0090(16) 0.0122(18) C41 0.048(2) 0.099(3) 0.038(2) -0.007(2) -0.0064(17) 0.002(2) C42 0.071(3) 0.085(3) 0.069(3) 0.031(2) -0.023(2) -0.024(2) C43 0.064(2) 0.0456(19) 0.0222(15) 0.0061(14) 0.0083(15) -0.0130(17) C44 0.055(2) 0.079(3) 0.0366(19) 0.0024(19) 0.0133(17) -0.004(2) C45 0.114(4) 0.058(3) 0.064(3) 0.002(2) 0.025(3) -0.037(3) C46 0.0179(11) 0.0163(11) 0.0189(12) 0.0005(9) 0.0012(9) 0.0016(9) C47 0.0271(12) 0.0191(12) 0.0210(13) -0.0027(10) -0.0022(10) 0.0051(10) C48 0.0277(12) 0.0192(12) 0.0178(12) -0.0016(10) 0.0019(10) 0.0033(10) C49 0.0183(11) 0.0239(13) 0.0287(14) -0.0061(11) 0.0026(10) -0.0027(10) C50 0.0196(12) 0.0414(18) 0.0470(19) -0.0077(15) -0.0042(12) 0.0016(12) C51 0.0319(14) 0.0263(15) 0.0450(18) -0.0066(13) 0.0058(13) -0.0084(12) C52 0.0316(14) 0.0370(16) 0.0283(15) -0.0106(13) -0.0094(12) 0.0040(12) C53 0.0380(15) 0.0362(16) 0.0243(14) -0.0061(12) 0.0074(12) -0.0005(13) C54 0.0179(11) 0.0258(13) 0.0258(14) -0.0036(11) 0.0026(10) -0.0027(10) C55 0.0238(12) 0.0289(15) 0.0350(16) -0.0001(12) 0.0129(11) -0.0025(11) C56 0.0246(13) 0.0431(18) 0.0384(17) 0.0056(14) -0.0024(12) 0.0033(12) C57 0.0247(12) 0.0296(14) 0.0337(15) -0.0056(12) 0.0128(12) -0.0020(11) C58 0.0235(12) 0.0323(15) 0.0315(15) -0.0060(12) 0.0056(11) -0.0035(11) C59 0.0150(11) 0.0281(14) 0.0316(15) -0.0058(11) 0.0024(10) -0.0039(10) _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 C46 2.053(2) . ? Ge1 Si2 2.3249(7) . ? Ge1 Si1 2.3870(7) . ? Ge1 Fe1 2.6875(4) . ? Fe1 C57 1.766(3) . ? Fe1 C58 1.770(3) . ? Fe1 C59 1.780(3) . ? Fe1 Si2 2.3166(8) . ? Fe1 Si1 2.3520(7) . ? Cl1 Si2 2.1251(10) . ? Si1 C1 1.922(2) . ? Si1 C16 1.942(2) . ? Si2 C31 1.900(3) . ? N1 C46 1.354(3) . ? N1 C47 1.391(3) . ? N1 C49 1.483(3) . ? N2 C46 1.361(3) . ? N2 C48 1.388(3) . ? N2 C54 1.486(3) . ? O1 C57 1.153(3) . ? O2 C58 1.149(3) . ? O3 C59 1.149(3) . ? C1 C6 1.413(3) . ? C1 C2 1.430(4) . ? C2 C3 1.393(4) . ? C2 C7 1.519(4) . ? C3 C4 1.374(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 C10 1.522(4) . ? C5 C6 1.401(4) . ? C5 H5 0.9500 . ? C6 C13 1.516(4) . ? C7 C9 1.530(4) . ? C7 C8 1.538(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.500(4) . ? C10 C11 1.509(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.526(4) . ? C13 C14 1.537(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.419(3) . ? C16 C21 1.419(4) . ? C17 C18 1.396(3) . ? C17 C22 1.517(4) . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 C25 1.527(4) . ? C20 C21 1.400(4) . ? C20 H20 0.9500 . ? C21 C28 1.526(4) . ? C22 C24 1.530(3) . ? C22 C23 1.533(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.513(5) . ? C25 C27 1.532(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.535(4) . ? C28 C29 1.542(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.405(4) . ? C31 C32 1.420(4) . ? C32 C33 1.397(4) . ? C32 C37 1.509(5) . ? C33 C34 1.366(5) . ? C33 H33 0.9500 . ? C34 C35 1.381(5) . ? C34 C40 1.529(4) . ? C35 C36 1.416(4) . ? C35 H35 0.9500 . ? C36 C43 1.514(5) . ? C37 C38 1.521(7) . ? C37 C39 1.536(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.475(5) . ? C40 C42 1.481(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.529(5) . ? C43 C45 1.530(5) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.360(4) . ? C47 C52 1.500(4) . ? C48 C53 1.490(4) . ? C49 C50 1.518(4) . ? C49 C51 1.532(4) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.517(4) . ? C54 C56 1.520(4) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? 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 C46 Ge1 Si2 116.10(7) . . ? C46 Ge1 Si1 132.52(7) . . ? Si2 Ge1 Si1 94.38(2) . . ? C46 Ge1 Fe1 114.26(6) . . ? Si2 Ge1 Fe1 54.473(19) . . ? Si1 Ge1 Fe1 54.837(18) . . ? C57 Fe1 C58 97.14(12) . . ? C57 Fe1 C59 94.18(13) . . ? C58 Fe1 C59 97.82(13) . . ? C57 Fe1 Si2 81.36(9) . . ? C58 Fe1 Si2 108.61(10) . . ? C59 Fe1 Si2 153.53(9) . . ? C57 Fe1 Si1 164.82(9) . . ? C58 Fe1 Si1 97.93(9) . . ? C59 Fe1 Si1 81.94(8) . . ? Si2 Fe1 Si1 95.54(3) . . ? C57 Fe1 Ge1 111.44(8) . . ? C58 Fe1 Ge1 141.99(9) . . ? C59 Fe1 Ge1 104.26(8) . . ? Si2 Fe1 Ge1 54.762(19) . . ? Si1 Fe1 Ge1 56.069(18) . . ? C1 Si1 C16 104.60(11) . . ? C1 Si1 Fe1 119.12(8) . . ? C16 Si1 Fe1 130.36(8) . . ? C1 Si1 Ge1 124.10(8) . . ? C16 Si1 Ge1 105.76(7) . . ? Fe1 Si1 Ge1 69.09(2) . . ? C31 Si2 Cl1 99.35(9) . . ? C31 Si2 Fe1 132.97(9) . . ? Cl1 Si2 Fe1 117.83(4) . . ? C31 Si2 Ge1 126.31(10) . . ? Cl1 Si2 Ge1 107.27(4) . . ? Fe1 Si2 Ge1 70.77(2) . . ? C46 N1 C47 110.0(2) . . ? C46 N1 C49 122.8(2) . . ? C47 N1 C49 126.2(2) . . ? C46 N2 C48 110.1(2) . . ? C46 N2 C54 123.2(2) . . ? C48 N2 C54 126.4(2) . . ? C6 C1 C2 116.7(2) . . ? C6 C1 Si1 117.07(19) . . ? C2 C1 Si1 126.13(18) . . ? C3 C2 C1 120.1(2) . . ? C3 C2 C7 115.9(2) . . ? C1 C2 C7 124.0(2) . . ? C4 C3 C2 123.1(3) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 116.9(3) . . ? C3 C4 C10 119.3(3) . . ? C5 C4 C10 123.8(3) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C13 117.7(2) . . ? C1 C6 C13 121.9(2) . . ? C2 C7 C9 111.8(2) . . ? C2 C7 C8 112.1(2) . . ? C9 C7 C8 108.9(2) . . ? C2 C7 H7 108.0 . . ? C9 C7 H7 108.0 . . ? C8 C7 H7 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 114.0(3) . . ? C12 C10 C4 113.3(3) . . ? C11 C10 C4 110.2(2) . . ? C12 C10 H10 106.2 . . ? C11 C10 H10 106.2 . . ? C4 C10 H10 106.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 C15 112.8(2) . . ? C6 C13 C14 110.0(2) . . ? C15 C13 C14 111.8(2) . . ? C6 C13 H13 107.3 . . ? C15 C13 H13 107.3 . . ? C14 C13 H13 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 117.0(2) . . ? C17 C16 Si1 116.30(18) . . ? C21 C16 Si1 126.58(18) . . ? C18 C17 C16 120.9(2) . . ? C18 C17 C22 115.8(2) . . ? C16 C17 C22 123.3(2) . . ? C19 C18 C17 122.2(3) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C20 C19 C18 116.9(2) . . ? C20 C19 C25 120.5(3) . . ? C18 C19 C25 122.3(3) . . ? C19 C20 C21 123.7(3) . . ? C19 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? C20 C21 C16 119.3(2) . . ? C20 C21 C28 115.2(2) . . ? C16 C21 C28 125.5(2) . . ? C17 C22 C24 110.6(2) . . ? C17 C22 C23 112.7(2) . . ? C24 C22 C23 110.7(2) . . ? C17 C22 H22 107.5 . . ? C24 C22 H22 107.5 . . ? C23 C22 H22 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C19 113.5(3) . . ? C26 C25 C27 112.5(3) . . ? C19 C25 C27 108.9(3) . . ? C26 C25 H25 107.2 . . ? C19 C25 H25 107.2 . . ? C27 C25 H25 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C30 111.5(2) . . ? C21 C28 C29 112.5(2) . . ? C30 C28 C29 108.1(2) . . ? C21 C28 H28 108.2 . . ? C30 C28 H28 108.2 . . ? C29 C28 H28 108.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.9(3) . . ? C36 C31 Si2 118.2(2) . . ? C32 C31 Si2 123.9(2) . . ? C33 C32 C31 119.8(3) . . ? C33 C32 C37 116.1(3) . . ? C31 C32 C37 124.1(3) . . ? C34 C33 C32 123.0(3) . . ? C34 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 C34 C35 117.2(3) . . ? C33 C34 C40 119.5(3) . . ? C35 C34 C40 123.1(3) . . ? C34 C35 C36 122.8(3) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? C31 C36 C35 119.2(3) . . ? C31 C36 C43 121.7(3) . . ? C35 C36 C43 119.0(3) . . ? C32 C37 C38 111.3(4) . . ? C32 C37 C39 111.4(3) . . ? C38 C37 C39 111.3(3) . . ? C32 C37 H37 107.5 . . ? C38 C37 H37 107.5 . . ? C39 C37 H37 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C42 112.4(3) . . ? C41 C40 C34 111.2(3) . . ? C42 C40 C34 112.9(3) . . ? C41 C40 H40 106.6 . . ? C42 C40 H40 106.6 . . ? C34 C40 H40 106.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C36 C43 C44 113.2(3) . . ? C36 C43 C45 110.3(3) . . ? C44 C43 C45 110.2(3) . . ? C36 C43 H43 107.7 . . ? C44 C43 H43 107.7 . . ? C45 C43 H43 107.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N1 C46 N2 106.0(2) . . ? N1 C46 Ge1 134.14(17) . . ? N2 C46 Ge1 119.76(16) . . ? C48 C47 N1 107.0(2) . . ? C48 C47 C52 127.7(2) . . ? N1 C47 C52 125.2(2) . . ? C47 C48 N2 106.8(2) . . ? C47 C48 C53 127.3(2) . . ? N2 C48 C53 125.8(2) . . ? N1 C49 C50 113.3(2) . . ? N1 C49 C51 111.1(2) . . ? C50 C49 C51 112.4(2) . . ? N1 C49 H49 106.5 . . ? C50 C49 H49 106.5 . . ? C51 C49 H49 106.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C54 C55 114.3(2) . . ? N2 C54 C56 109.8(2) . . ? C55 C54 C56 112.4(2) . . ? N2 C54 H54 106.6 . . ? C55 C54 H54 106.6 . . ? C56 C54 H54 106.6 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O1 C57 Fe1 177.0(2) . . ? O2 C58 Fe1 173.5(3) . . ? O3 C59 Fe1 175.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.184 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 953521' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sh3359 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H89 Cl Fe Ge N2 O4 Si2, 0.25 C5 H12' _chemical_formula_sum 'C61.25 H92 Cl Fe Ge N2 O4 Si2' _chemical_formula_weight 1140.44 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Cl Cl 0.1484 0.1585 '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' _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 13.2910(4) _cell_length_b 19.9842(5) _cell_length_c 24.8636(7) _cell_angle_alpha 89.1430(10) _cell_angle_beta 88.102(2) _cell_angle_gamma 76.122(2) _cell_volume 6407.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 122(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.14 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2434 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7684 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details 'SADABS, BrukerAXS 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 105034 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.10 _reflns_number_total 28114 _reflns_number_gt 19520 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28114 _refine_ls_number_parameters 1408 _refine_ls_number_restraints 504 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.427 _refine_ls_restrained_S_all 1.439 _refine_ls_shift/su_max 1.098 _refine_ls_shift/su_mean 0.011 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 0.31492(3) 0.089311(18) 0.704780(14) 0.02404(10) Uani 1 1 d U . . Ge2 Ge 0.54586(3) 0.74808(2) 0.911464(17) 0.04255(13) Uani 1 1 d U . . Fe1 Fe 0.47528(4) 0.06028(3) 0.74941(2) 0.03178(13) Uani 1 1 d U . . Fe2 Fe 0.36567(4) 0.79861(3) 0.91541(2) 0.03609(14) Uani 1 1 d U . . Si1 Si 0.27565(6) 0.15493(4) 0.63064(4) 0.02052(19) Uani 1 1 d U . . Si2 Si 0.12160(6) 0.16113(4) 0.58294(4) 0.01988(19) Uani 1 1 d U . . Si3 Si 0.63987(7) 0.66602(6) 0.85935(4) 0.0356(3) Uani 1 1 d U . . Si4 Si 0.81176(7) 0.60410(5) 0.87542(4) 0.0246(2) Uani 1 1 d U . . Cl1 Cl 0.06961(6) 0.08237(4) 0.62473(3) 0.02503(18) Uani 1 1 d U . . Cl2 Cl 0.83982(6) 0.65795(4) 0.94356(3) 0.02911(19) Uani 1 1 d U . . N1 N 0.1598(2) 0.02083(15) 0.75577(12) 0.0349(7) Uani 1 1 d U B . N2 N 0.2534(2) -0.04792(14) 0.69751(12) 0.0282(6) Uani 1 1 d U . . N3 N 0.6547(2) 0.83513(16) 0.97130(12) 0.0364(7) Uani 1 1 d U . . N4 N 0.6078(2) 0.76302(15) 1.02613(12) 0.0368(7) Uani 1 1 d U . . C1 C 0.3316(2) 0.23350(15) 0.63880(14) 0.0222(7) Uani 1 1 d U . . C2 C 0.2807(2) 0.28808(17) 0.67277(15) 0.0293(8) Uani 1 1 d U . . C3 C 0.3300(3) 0.33974(19) 0.68505(19) 0.0458(11) Uani 1 1 d U . . H3 H 0.2950 0.3758 0.7083 0.055 Uiso 1 1 calc R . . C4 C 0.4274(3) 0.3408(2) 0.6649(2) 0.0597(14) Uani 1 1 d U A . C5 C 0.4756(3) 0.28851(19) 0.62985(19) 0.0445(11) Uani 1 1 d U . . H5 H 0.5419 0.2892 0.6146 0.053 Uiso 1 1 calc R . . C6 C 0.4308(2) 0.23552(16) 0.61629(14) 0.0266(7) Uani 1 1 d U . . C7 C 0.1730(2) 0.29454(18) 0.69801(15) 0.0307(8) Uani 1 1 d U . . H7 H 0.1436 0.2580 0.6821 0.037 Uiso 1 1 calc R . . C8 C 0.1011(3) 0.36421(18) 0.68449(18) 0.0413(10) Uani 1 1 d U . . H8A H 0.1238 0.4009 0.7028 0.062 Uiso 1 1 calc R . . H8B H 0.0300 0.3644 0.6965 0.062 Uiso 1 1 calc R . . H8C H 0.1032 0.3720 0.6455 0.062 Uiso 1 1 calc R . . C9 C 0.1775(3) 0.2820(2) 0.75869(16) 0.0451(10) Uani 1 1 d U . . H9A H 0.2212 0.2360 0.7660 0.068 Uiso 1 1 calc R . . H9B H 0.1073 0.2851 0.7736 0.068 Uiso 1 1 calc R . . H9C H 0.2068 0.3168 0.7755 0.068 Uiso 1 1 calc R . . C10 C 0.4830(4) 0.3933(2) 0.6875(2) 0.0729(15) Uani 1 1 d DU . . H10A H 0.4306 0.4292 0.7077 0.087 Uiso 0.838(7) 1 calc PR A 1 H10B H 0.4435 0.4194 0.7186 0.087 Uiso 0.162(7) 1 calc PR A 2 C11A C 0.5290(6) 0.4277(4) 0.6434(3) 0.089(2) Uani 0.838(7) 1 d PDU A 1 H11A H 0.4770 0.4444 0.6162 0.134 Uiso 0.838(7) 1 calc PR A 1 H11B H 0.5884 0.3948 0.6269 0.134 Uiso 0.838(7) 1 calc PR A 1 H11C H 0.5522 0.4666 0.6578 0.134 Uiso 0.838(7) 1 calc PR A 1 C12A C 0.5689(4) 0.3600(3) 0.7259(3) 0.0697(19) Uani 0.838(7) 1 d PDU A 1 H12A H 0.6194 0.3231 0.7073 0.105 Uiso 0.838(7) 1 calc PR A 1 H12B H 0.5385 0.3407 0.7572 0.105 Uiso 0.838(7) 1 calc PR A 1 H12C H 0.6037 0.3949 0.7380 0.105 Uiso 0.838(7) 1 calc PR A 1 C11B C 0.446(2) 0.4253(16) 0.6341(8) 0.082(4) Uani 0.162(7) 1 d PDU A 2 H11D H 0.3893 0.4664 0.6404 0.123 Uiso 0.162(7) 1 calc PR A 2 H11E H 0.4207 0.3920 0.6130 0.123 Uiso 0.162(7) 1 calc PR A 2 H11F H 0.5032 0.4385 0.6144 0.123 Uiso 0.162(7) 1 calc PR A 2 C12B C 0.5979(9) 0.3856(18) 0.6910(14) 0.084(4) Uani 0.162(7) 1 d PDU A 2 H12D H 0.6257 0.3499 0.7178 0.126 Uiso 0.162(7) 1 calc PR A 2 H12E H 0.6113 0.4295 0.7018 0.126 Uiso 0.162(7) 1 calc PR A 2 H12F H 0.6315 0.3722 0.6558 0.126 Uiso 0.162(7) 1 calc PR A 2 C13 C 0.4934(2) 0.18080(18) 0.57881(14) 0.0291(8) Uani 1 1 d U . . H13 H 0.4495 0.1485 0.5700 0.035 Uiso 1 1 calc R . . C14 C 0.5902(3) 0.1396(2) 0.60522(18) 0.0461(10) Uani 1 1 d U . . H14A H 0.6384 0.1691 0.6099 0.069 Uiso 1 1 calc R . . H14B H 0.6233 0.1004 0.5824 0.069 Uiso 1 1 calc R . . H14C H 0.5713 0.1226 0.6404 0.069 Uiso 1 1 calc R . . C15 C 0.5234(4) 0.2130(3) 0.52609(18) 0.0622(13) Uani 1 1 d U . . H15A H 0.5601 0.2486 0.5342 0.093 Uiso 1 1 calc R . . H15B H 0.4607 0.2338 0.5065 0.093 Uiso 1 1 calc R . . H15C H 0.5687 0.1772 0.5039 0.093 Uiso 1 1 calc R . . C16 C 0.2346(3) 0.01619(17) 0.71691(14) 0.0268(7) Uani 1 1 d U . . C17 C 0.1313(3) -0.0414(2) 0.76077(17) 0.0403(9) Uani 1 1 d U . . C18 C 0.1893(3) -0.08391(19) 0.72436(18) 0.0414(10) Uani 1 1 d U . . C19 C 0.1103(4) 0.0865(2) 0.78389(18) 0.0689(15) Uani 1 1 d DU . . H19A H 0.1293 0.1236 0.7612 0.083 Uiso 0.54(2) 1 calc PR B 1 H19B H 0.1537 0.1196 0.7742 0.083 Uiso 0.46(2) 1 calc PR B 2 C20A C 0.1439(8) 0.0973(7) 0.8386(3) 0.058(3) Uani 0.54(2) 1 d PDU B 1 H20A H 0.1006 0.1403 0.8533 0.087 Uiso 0.54(2) 1 calc PR B 1 H20B H 0.2166 0.1001 0.8369 0.087 Uiso 0.54(2) 1 calc PR B 1 H20C H 0.1368 0.0587 0.8620 0.087 Uiso 0.54(2) 1 calc PR B 1 C21A C -0.0085(5) 0.0984(7) 0.7798(5) 0.049(3) Uani 0.54(2) 1 d PDU B 1 H21A H -0.0419 0.1459 0.7900 0.074 Uiso 0.54(2) 1 calc PR B 1 H21B H -0.0334 0.0664 0.8041 0.074 Uiso 0.54(2) 1 calc PR B 1 H21C H -0.0254 0.0906 0.7427 0.074 Uiso 0.54(2) 1 calc PR B 1 C20B C 0.1328(11) 0.0651(9) 0.8436(3) 0.070(3) Uani 0.46(2) 1 d PDU B 2 H20D H 0.0947 0.1019 0.8673 0.105 Uiso 0.46(2) 1 calc PR B 2 H20E H 0.2073 0.0574 0.8494 0.105 Uiso 0.46(2) 1 calc PR B 2 H20F H 0.1106 0.0226 0.8516 0.105 Uiso 0.46(2) 1 calc PR B 2 C21B C 0.0003(9) 0.1237(10) 0.7744(8) 0.084(4) Uani 0.46(2) 1 d PDU B 2 H21D H -0.0066 0.1735 0.7769 0.126 Uiso 0.46(2) 1 calc PR B 2 H21E H -0.0455 0.1094 0.8015 0.126 Uiso 0.46(2) 1 calc PR B 2 H21F H -0.0190 0.1127 0.7384 0.126 Uiso 0.46(2) 1 calc PR B 2 C22 C 0.0506(4) -0.0556(2) 0.7998(2) 0.0616(14) Uani 1 1 d U . . H22A H 0.0442 -0.1030 0.7952 0.092 Uiso 1 1 calc R . . H22B H -0.0161 -0.0235 0.7931 0.092 Uiso 1 1 calc R . . H22C H 0.0710 -0.0497 0.8366 0.092 Uiso 1 1 calc R . . C23 C 0.1884(4) -0.1581(2) 0.7142(2) 0.0720(16) Uani 1 1 d U . . H23A H 0.1459 -0.1740 0.7423 0.108 Uiso 1 1 calc R . . H23B H 0.2595 -0.1867 0.7148 0.108 Uiso 1 1 calc R . . H23C H 0.1593 -0.1617 0.6790 0.108 Uiso 1 1 calc R . . C24 C 0.3327(3) -0.07323(18) 0.65442(15) 0.0307(8) Uani 1 1 d U . . H24 H 0.3594 -0.0328 0.6419 0.037 Uiso 1 1 calc R . . C25 C 0.4240(3) -0.12571(19) 0.67594(17) 0.0402(9) Uani 1 1 d U . . H25A H 0.4474 -0.1079 0.7086 0.060 Uiso 1 1 calc R . . H25B H 0.4806 -0.1346 0.6488 0.060 Uiso 1 1 calc R . . H25C H 0.4033 -0.1687 0.6844 0.060 Uiso 1 1 calc R . . C26 C 0.2843(3) -0.0977(2) 0.60620(17) 0.0472(10) Uani 1 1 d U . . H26A H 0.2615 -0.1395 0.6160 0.071 Uiso 1 1 calc R . . H26B H 0.3356 -0.1077 0.5764 0.071 Uiso 1 1 calc R . . H26C H 0.2245 -0.0616 0.5951 0.071 Uiso 1 1 calc R . . C27 C 0.1220(2) 0.12954(16) 0.51009(13) 0.0224(7) Uani 1 1 d U . . C28 C 0.2117(3) 0.10587(17) 0.47738(14) 0.0281(7) Uani 1 1 d U . . C29 C 0.2033(3) 0.08282(18) 0.42560(14) 0.0336(8) Uani 1 1 d U . . H29 H 0.2648 0.0667 0.4043 0.040 Uiso 1 1 calc R . . C30 C 0.1073(3) 0.08251(19) 0.40352(15) 0.0343(8) Uani 1 1 d U . . C31 C 0.0210(3) 0.10628(18) 0.43532(14) 0.0331(8) Uani 1 1 d U . . H31 H -0.0450 0.1074 0.4212 0.040 Uiso 1 1 calc R . . C32 C 0.0255(2) 0.12899(16) 0.48768(14) 0.0262(7) Uani 1 1 d U . . C33 C 0.3198(3) 0.1008(2) 0.49771(15) 0.0374(9) Uani 1 1 d U . . H33 H 0.3136 0.1361 0.5265 0.045 Uiso 1 1 calc R . . C34 C 0.3594(4) 0.0301(2) 0.5238(2) 0.0691(15) Uani 1 1 d U . . H34A H 0.3088 0.0224 0.5514 0.104 Uiso 1 1 calc R . . H34B H 0.4258 0.0283 0.5405 0.104 Uiso 1 1 calc R . . H34C H 0.3689 -0.0057 0.4964 0.104 Uiso 1 1 calc R . . C35 C 0.3969(4) 0.1156(4) 0.4548(2) 0.0852(19) Uani 1 1 d U . . H35A H 0.4088 0.0798 0.4271 0.128 Uiso 1 1 calc R . . H35B H 0.4627 0.1156 0.4715 0.128 Uiso 1 1 calc R . . H35C H 0.3687 0.1607 0.4382 0.128 Uiso 1 1 calc R . . C36 C 0.0999(3) 0.0584(2) 0.34664(15) 0.0429(10) Uani 1 1 d U . . H36 H 0.0263 0.0563 0.3417 0.051 Uiso 1 1 calc R . . C37 C 0.1662(3) -0.0116(2) 0.33578(15) 0.0408(9) Uani 1 1 d U . . H37A H 0.1590 -0.0239 0.2983 0.061 Uiso 1 1 calc R . . H37B H 0.1445 -0.0451 0.3599 0.061 Uiso 1 1 calc R . . H37C H 0.2388 -0.0119 0.3419 0.061 Uiso 1 1 calc R . . C38 C 0.1227(5) 0.1082(3) 0.3084(2) 0.0800(17) Uani 1 1 d U . . H38A H 0.1912 0.1160 0.3151 0.120 Uiso 1 1 calc R . . H38B H 0.0701 0.1518 0.3122 0.120 Uiso 1 1 calc R . . H38C H 0.1222 0.0908 0.2718 0.120 Uiso 1 1 calc R . . C39 C -0.0787(2) 0.14990(17) 0.51797(15) 0.0292(8) Uani 1 1 d U . . H39 H -0.0646 0.1627 0.5552 0.035 Uiso 1 1 calc R . . C40 C -0.1305(3) 0.0887(2) 0.52308(16) 0.0380(9) Uani 1 1 d U . . H40A H -0.1481 0.0761 0.4873 0.057 Uiso 1 1 calc R . . H40B H -0.1938 0.1020 0.5457 0.057 Uiso 1 1 calc R . . H40C H -0.0826 0.0493 0.5395 0.057 Uiso 1 1 calc R . . C41 C -0.1501(3) 0.2136(2) 0.49268(17) 0.0409(9) Uani 1 1 d U . . H41A H -0.1150 0.2515 0.4911 0.061 Uiso 1 1 calc R . . H41B H -0.2142 0.2274 0.5146 0.061 Uiso 1 1 calc R . . H41C H -0.1667 0.2027 0.4562 0.061 Uiso 1 1 calc R . . C42 C 0.0301(2) 0.25082(16) 0.58616(14) 0.0251(7) Uani 1 1 d U . . C43 C -0.0613(2) 0.27292(17) 0.61892(15) 0.0295(8) Uani 1 1 d U . . C44 C -0.1267(3) 0.33687(18) 0.60959(16) 0.0345(9) Uani 1 1 d U . . H44 H -0.1886 0.3503 0.6310 0.041 Uiso 1 1 calc R . . C45 C -0.1063(3) 0.38184(19) 0.57085(17) 0.0395(9) Uani 1 1 d U C . C46 C -0.0133(3) 0.36226(19) 0.54093(17) 0.0378(9) Uani 1 1 d U . . H46 H 0.0038 0.3931 0.5147 0.045 Uiso 1 1 calc R . . C47 C 0.0549(3) 0.29847(17) 0.54874(15) 0.0289(8) Uani 1 1 d U . . C48 C -0.0925(3) 0.23130(18) 0.66505(16) 0.0329(8) Uani 1 1 d U . . H48 H -0.0344 0.1897 0.6704 0.039 Uiso 1 1 calc R . . C49 C -0.1904(3) 0.2063(2) 0.65258(18) 0.0463(11) Uani 1 1 d U . . H49A H -0.2491 0.2462 0.6483 0.069 Uiso 1 1 calc R . . H49B H -0.2060 0.1772 0.6823 0.069 Uiso 1 1 calc R . . H49C H -0.1783 0.1796 0.6192 0.069 Uiso 1 1 calc R . . C50 C -0.1120(3) 0.2714(2) 0.71836(17) 0.0420(10) Uani 1 1 d U . . H50A H -0.0486 0.2845 0.7282 0.063 Uiso 1 1 calc R . . H50B H -0.1319 0.2422 0.7468 0.063 Uiso 1 1 calc R . . H50C H -0.1679 0.3130 0.7140 0.063 Uiso 1 1 calc R . . C51 C -0.1813(3) 0.4522(2) 0.56237(19) 0.0517(11) Uani 1 1 d DU . . H51A H -0.2397 0.4565 0.5895 0.062 Uiso 0.907(10) 1 calc PR C 1 H51B H -0.2073 0.4534 0.6006 0.062 Uiso 0.093(10) 1 calc PR C 2 C52 C -0.1292(4) 0.5108(2) 0.57166(19) 0.0535(12) Uani 1 1 d DU C . H52A H -0.0718 0.5080 0.5453 0.080 Uiso 1 1 calc R . . H52B H -0.1023 0.5071 0.6081 0.080 Uiso 1 1 calc R . . H52C H -0.1798 0.5550 0.5675 0.080 Uiso 1 1 calc R . . C53A C -0.2268(5) 0.4576(3) 0.5070(3) 0.082(3) Uani 0.907(10) 1 d PDU C 1 H53A H -0.2635 0.4210 0.5027 0.123 Uiso 0.907(10) 1 calc PR C 1 H53B H -0.1710 0.4527 0.4795 0.123 Uiso 0.907(10) 1 calc PR C 1 H53C H -0.2755 0.5026 0.5029 0.123 Uiso 0.907(10) 1 calc PR C 1 C53B C -0.269(3) 0.422(3) 0.544(3) 0.077(5) Uani 0.093(10) 1 d PDU C 2 H53D H -0.2626 0.3764 0.5596 0.116 Uiso 0.093(10) 1 calc PR C 2 H53E H -0.2658 0.4192 0.5045 0.116 Uiso 0.093(10) 1 calc PR C 2 H53F H -0.3357 0.4525 0.5554 0.116 Uiso 0.093(10) 1 calc PR C 2 C54 C 0.1573(3) 0.28464(18) 0.51556(16) 0.0339(8) Uani 1 1 d U . . H54 H 0.1993 0.2381 0.5262 0.041 Uiso 1 1 calc R . . C55 C 0.2198(3) 0.33779(19) 0.52905(18) 0.0411(10) Uani 1 1 d U . . H55A H 0.1794 0.3842 0.5203 0.062 Uiso 1 1 calc R . . H55B H 0.2852 0.3279 0.5080 0.062 Uiso 1 1 calc R . . H55C H 0.2344 0.3350 0.5675 0.062 Uiso 1 1 calc R . . C56 C 0.1398(3) 0.2834(2) 0.45518(17) 0.0476(10) Uani 1 1 d U . . H56A H 0.0977 0.2507 0.4480 0.071 Uiso 1 1 calc R . . H56B H 0.2069 0.2693 0.4358 0.071 Uiso 1 1 calc R . . H56C H 0.1037 0.3296 0.4430 0.071 Uiso 1 1 calc R . . C57 C 0.4681(3) 0.1506(2) 0.75526(15) 0.0379(9) Uani 1 1 d U . . C58 C 0.5231(3) 0.0168(2) 0.68936(19) 0.0450(10) Uani 1 1 d U . . C59 C 0.4156(3) 0.0165(2) 0.79885(17) 0.0436(10) Uani 1 1 d U . . C60 C 0.5991(3) 0.0370(2) 0.77750(18) 0.0498(11) Uani 1 1 d U . . C61 C 0.5853(3) 0.6686(2) 0.78950(15) 0.0404(9) Uani 1 1 d U . . C62 C 0.6236(3) 0.7069(2) 0.74735(16) 0.0455(10) Uani 1 1 d U . . C63 C 0.5841(3) 0.7093(3) 0.69596(17) 0.0525(12) Uani 1 1 d U . . H63 H 0.6095 0.7354 0.6688 0.063 Uiso 1 1 calc R . . C64 C 0.5103(3) 0.6756(3) 0.68301(18) 0.0667(15) Uani 1 1 d U . . C65 C 0.4722(3) 0.6390(3) 0.72356(18) 0.0607(13) Uani 1 1 d U . . H65 H 0.4201 0.6158 0.7153 0.073 Uiso 1 1 calc R . . C66 C 0.5082(3) 0.6351(3) 0.77668(17) 0.0510(11) Uani 1 1 d U . . C67 C 0.7051(3) 0.7464(2) 0.75623(16) 0.0431(10) Uani 1 1 d U . . H67 H 0.7415 0.7279 0.7898 0.052 Uiso 1 1 calc R . . C68 C 0.6556(3) 0.8233(2) 0.76508(18) 0.0524(11) Uani 1 1 d U . . H68A H 0.6228 0.8436 0.7320 0.079 Uiso 1 1 calc R . . H68B H 0.7092 0.8468 0.7745 0.079 Uiso 1 1 calc R . . H68C H 0.6032 0.8285 0.7944 0.079 Uiso 1 1 calc R . . C69 C 0.7862(3) 0.7361(3) 0.71024(17) 0.0533(12) Uani 1 1 d U . . H69A H 0.8109 0.6868 0.7026 0.080 Uiso 1 1 calc R . . H69B H 0.8446 0.7547 0.7205 0.080 Uiso 1 1 calc R . . H69C H 0.7552 0.7603 0.6780 0.080 Uiso 1 1 calc R . . C70 C 0.4780(4) 0.6789(4) 0.6244(2) 0.090(2) Uani 1 1 d U . . H70 H 0.4874 0.7248 0.6116 0.108 Uiso 1 1 calc R . . C71 C 0.5586(3) 0.6279(2) 0.59127(16) 0.0520(11) Uani 1 1 d U . . H71A H 0.5656 0.5814 0.6061 0.078 Uiso 1 1 calc R . . H71B H 0.6255 0.6404 0.5924 0.078 Uiso 1 1 calc R . . H71C H 0.5368 0.6291 0.5539 0.078 Uiso 1 1 calc R . . C72 C 0.3736(4) 0.6824(4) 0.6151(2) 0.092(2) Uani 1 1 d U . . H72A H 0.3567 0.6393 0.6269 0.137 Uiso 1 1 calc R . . H72B H 0.3611 0.6895 0.5765 0.137 Uiso 1 1 calc R . . H72C H 0.3299 0.7210 0.6353 0.137 Uiso 1 1 calc R . . C73 C 0.4607(3) 0.5937(3) 0.81755(18) 0.0546(12) Uani 1 1 d U . . H73 H 0.4939 0.5960 0.8528 0.066 Uiso 1 1 calc R . . C74 C 0.4819(4) 0.5182(3) 0.8016(2) 0.0754(16) Uani 1 1 d U . . H74A H 0.4583 0.5149 0.7650 0.113 Uiso 1 1 calc R . . H74B H 0.4447 0.4937 0.8267 0.113 Uiso 1 1 calc R . . H74C H 0.5565 0.4973 0.8028 0.113 Uiso 1 1 calc R . . C75 C 0.3435(3) 0.6230(3) 0.8258(2) 0.0639(14) Uani 1 1 d U . . H75A H 0.3300 0.6717 0.8356 0.096 Uiso 1 1 calc R . . H75B H 0.3171 0.5973 0.8546 0.096 Uiso 1 1 calc R . . H75C H 0.3086 0.6186 0.7924 0.096 Uiso 1 1 calc R . . C76 C 0.6149(3) 0.77939(18) 0.97369(14) 0.0319(8) Uani 1 1 d U . . C77 C 0.6719(3) 0.8557(2) 1.02215(16) 0.0383(9) Uani 1 1 d U . . C78 C 0.6417(3) 0.8111(2) 1.05695(16) 0.0435(10) Uani 1 1 d U . . C79 C 0.6732(4) 0.8700(3) 0.91961(18) 0.0618(13) Uani 1 1 d U . . H79 H 0.6580 0.8408 0.8900 0.074 Uiso 1 1 calc R . . C80 C 0.7861(4) 0.8713(3) 0.9125(2) 0.0843(18) Uani 1 1 d U . . H80A H 0.8029 0.9029 0.9387 0.126 Uiso 1 1 calc R . . H80B H 0.7991 0.8870 0.8760 0.126 Uiso 1 1 calc R . . H80C H 0.8297 0.8249 0.9183 0.126 Uiso 1 1 calc R . . C81 C 0.5993(5) 0.9400(3) 0.9140(3) 0.099(2) Uani 1 1 d U . . H81A H 0.5277 0.9348 0.9154 0.148 Uiso 1 1 calc R . . H81B H 0.6132 0.9608 0.8794 0.148 Uiso 1 1 calc R . . H81C H 0.6090 0.9697 0.9434 0.148 Uiso 1 1 calc R . . C82 C 0.7104(4) 0.9176(2) 1.03552(19) 0.0572(12) Uani 1 1 d U . . H82A H 0.6943 0.9292 1.0735 0.086 Uiso 1 1 calc R . . H82B H 0.6767 0.9565 1.0129 0.086 Uiso 1 1 calc R . . H82C H 0.7856 0.9076 1.0290 0.086 Uiso 1 1 calc R . . C83 C 0.6438(5) 0.8107(3) 1.11724(18) 0.0763(17) Uani 1 1 d U . . H83A H 0.7048 0.7762 1.1291 0.114 Uiso 1 1 calc R . . H83B H 0.5808 0.7992 1.1322 0.114 Uiso 1 1 calc R . . H83C H 0.6472 0.8563 1.1298 0.114 Uiso 1 1 calc R . . C84 C 0.5644(3) 0.7059(2) 1.04560(17) 0.0453(10) Uani 1 1 d U . . H84 H 0.5504 0.6812 1.0130 0.054 Uiso 1 1 calc R . . C85 C 0.6412(4) 0.6538(2) 1.0783(2) 0.0637(13) Uani 1 1 d U . . H85A H 0.7079 0.6410 1.0584 0.096 Uiso 1 1 calc R . . H85B H 0.6146 0.6126 1.0847 0.096 Uiso 1 1 calc R . . H85C H 0.6508 0.6741 1.1128 0.096 Uiso 1 1 calc R . . C86 C 0.4595(4) 0.7327(2) 1.0751(2) 0.0605(13) Uani 1 1 d U . . H86A H 0.4698 0.7560 1.1082 0.091 Uiso 1 1 calc R . . H86B H 0.4286 0.6940 1.0841 0.091 Uiso 1 1 calc R . . H86C H 0.4131 0.7654 1.0518 0.091 Uiso 1 1 calc R . . C87 C 0.8515(3) 0.51105(18) 0.90069(15) 0.0322(8) Uani 1 1 d U . . C88 C 0.9592(3) 0.47983(19) 0.90352(16) 0.0353(9) Uani 1 1 d U . . C89 C 0.9920(3) 0.4098(2) 0.91551(18) 0.0473(11) Uani 1 1 d U . . H89 H 1.0643 0.3894 0.9165 0.057 Uiso 1 1 calc R . . C90 C 0.9229(4) 0.3690(2) 0.92604(19) 0.0523(11) Uani 1 1 d U . . C91 C 0.8186(3) 0.4005(2) 0.92672(18) 0.0476(11) Uani 1 1 d U . . H91 H 0.7705 0.3734 0.9354 0.057 Uiso 1 1 calc R . . C92 C 0.7808(3) 0.46944(19) 0.91544(16) 0.0380(9) Uani 1 1 d U . . C93 C 1.0449(3) 0.5182(2) 0.89601(16) 0.0364(9) Uani 1 1 d U . . H93 H 1.0112 0.5673 0.8873 0.044 Uiso 1 1 calc R . . C94 C 1.1198(3) 0.4893(2) 0.84822(18) 0.0499(11) Uani 1 1 d U . . H94A H 1.1541 0.4410 0.8555 0.075 Uiso 1 1 calc R . . H94B H 1.1721 0.5163 0.8437 0.075 Uiso 1 1 calc R . . H94C H 1.0805 0.4922 0.8152 0.075 Uiso 1 1 calc R . . C95 C 1.1040(3) 0.5177(2) 0.94751(18) 0.0482(11) Uani 1 1 d U . . H95A H 1.0558 0.5393 0.9765 0.072 Uiso 1 1 calc R . . H95B H 1.1575 0.5435 0.9416 0.072 Uiso 1 1 calc R . . H95C H 1.1366 0.4701 0.9576 0.072 Uiso 1 1 calc R . . C96 C 0.9567(5) 0.2918(2) 0.9353(2) 0.0765(17) Uani 1 1 d U . . H96 H 0.9161 0.2690 0.9115 0.092 Uiso 1 1 calc R . . C97 C 0.9373(6) 0.2731(3) 0.9901(3) 0.109(2) Uani 1 1 d U . . H97A H 0.9591 0.2229 0.9943 0.164 Uiso 1 1 calc R . . H97B H 0.8631 0.2887 0.9991 0.164 Uiso 1 1 calc R . . H97C H 0.9765 0.2950 1.0143 0.164 Uiso 1 1 calc R . . C98 C 1.0675(6) 0.2611(3) 0.9247(4) 0.158(4) Uani 1 1 d U . . H98A H 1.1087 0.2808 0.9492 0.238 Uiso 1 1 calc R . . H98B H 1.0860 0.2708 0.8875 0.238 Uiso 1 1 calc R . . H98C H 1.0816 0.2111 0.9305 0.238 Uiso 1 1 calc R . . C99 C 0.6650(3) 0.50079(19) 0.92078(17) 0.0381(9) Uani 1 1 d U . . H99 H 0.6458 0.5344 0.8905 0.046 Uiso 1 1 calc R . . C100 C 0.6403(3) 0.5407(2) 0.97304(17) 0.0428(10) Uani 1 1 d U . . H10C H 0.6582 0.5089 1.0036 0.064 Uiso 1 1 calc R . . H10D H 0.5661 0.5631 0.9753 0.064 Uiso 1 1 calc R . . H10E H 0.6806 0.5757 0.9740 0.064 Uiso 1 1 calc R . . C101 C 0.5973(3) 0.4490(2) 0.9182(2) 0.0569(13) Uani 1 1 d U . . H10F H 0.6157 0.4214 0.8856 0.085 Uiso 1 1 calc R . . H10G H 0.5242 0.4739 0.9176 0.085 Uiso 1 1 calc R . . H10H H 0.6086 0.4187 0.9499 0.085 Uiso 1 1 calc R . . C102 C 0.8949(2) 0.60871(17) 0.81214(14) 0.0271(7) Uani 1 1 d U . . C103 C 0.9664(2) 0.65125(18) 0.80357(14) 0.0291(8) Uani 1 1 d U . . C104 C 1.0314(3) 0.6407(2) 0.75749(15) 0.0353(9) Uani 1 1 d U . . H104 H 1.0803 0.6682 0.7524 0.042 Uiso 1 1 calc R . . C105 C 1.0279(3) 0.5922(2) 0.71893(16) 0.0404(9) Uani 1 1 d U . . C106 C 0.9544(3) 0.5547(2) 0.72599(16) 0.0410(10) Uani 1 1 d U . . H106 H 0.9490 0.5225 0.6992 0.049 Uiso 1 1 calc R . . C107 C 0.8871(3) 0.56204(19) 0.77121(15) 0.0324(8) Uani 1 1 d U . . C108 C 0.9766(3) 0.70763(18) 0.84135(15) 0.0314(8) Uani 1 1 d U . . H108 H 0.9228 0.7110 0.8709 0.038 Uiso 1 1 calc R . . C109 C 0.9591(3) 0.7780(2) 0.81271(19) 0.0517(11) Uani 1 1 d U . . H10I H 1.0093 0.7752 0.7826 0.078 Uiso 1 1 calc R . . H10J H 0.9681 0.8129 0.8382 0.078 Uiso 1 1 calc R . . H10K H 0.8886 0.7907 0.7991 0.078 Uiso 1 1 calc R . . C110 C 1.0820(4) 0.6941(2) 0.8664(2) 0.0692(15) Uani 1 1 d U . . H11G H 1.0989 0.6477 0.8822 0.104 Uiso 1 1 calc R . . H11H H 1.0807 0.7281 0.8946 0.104 Uiso 1 1 calc R . . H11I H 1.1346 0.6979 0.8387 0.104 Uiso 1 1 calc R . . C111 C 1.0996(3) 0.5842(3) 0.66861(18) 0.0582(13) Uani 1 1 d U . . H111 H 1.0754 0.5528 0.6438 0.070 Uiso 1 1 calc R . . C112 C 1.0938(4) 0.6502(3) 0.6388(2) 0.0816(18) Uani 1 1 d U . . H11J H 1.1219 0.6813 0.6608 0.122 Uiso 1 1 calc R . . H11K H 1.0213 0.6717 0.6311 0.122 Uiso 1 1 calc R . . H11L H 1.1343 0.6409 0.6049 0.122 Uiso 1 1 calc R . . C113 C 1.2090(3) 0.5486(3) 0.6831(2) 0.0640(14) Uani 1 1 d U . . H11M H 1.2379 0.5795 0.7049 0.096 Uiso 1 1 calc R . . H11N H 1.2517 0.5368 0.6501 0.096 Uiso 1 1 calc R . . H11O H 1.2084 0.5065 0.7037 0.096 Uiso 1 1 calc R . . C114 C 0.8074(3) 0.5185(2) 0.77264(17) 0.0413(10) Uani 1 1 d U . . H114 H 0.7586 0.5342 0.8039 0.050 Uiso 1 1 calc R . . C115 C 0.8571(3) 0.4425(2) 0.7810(2) 0.0543(12) Uani 1 1 d U . . H11P H 0.9001 0.4245 0.7492 0.082 Uiso 1 1 calc R . . H11Q H 0.8029 0.4172 0.7866 0.082 Uiso 1 1 calc R . . H11R H 0.9004 0.4367 0.8127 0.082 Uiso 1 1 calc R . . C116 C 0.7427(3) 0.5294(3) 0.72109(18) 0.0564(12) Uani 1 1 d U . . H11S H 0.7874 0.5107 0.6901 0.085 Uiso 1 1 calc R . . H11T H 0.7134 0.5788 0.7154 0.085 Uiso 1 1 calc R . . H11U H 0.6864 0.5056 0.7252 0.085 Uiso 1 1 calc R . . C117 C 0.3554(3) 0.7171(2) 0.94168(17) 0.0446(10) Uani 1 1 d U . . C118 C 0.3773(3) 0.8119(2) 0.8445(2) 0.0531(11) Uani 1 1 d U . . C119 C 0.3883(3) 0.8607(2) 0.96083(19) 0.0476(11) Uani 1 1 d U . . C120 C 0.2304(3) 0.8339(2) 0.91652(18) 0.0442(10) Uani 1 1 d U . . O1 O 0.4675(2) 0.20803(15) 0.76031(12) 0.0513(8) Uani 1 1 d U . . O2 O 0.5588(2) -0.01342(18) 0.65105(15) 0.0746(11) Uani 1 1 d U . . O3 O 0.3795(2) -0.01366(18) 0.83146(14) 0.0674(10) Uani 1 1 d U . . O4 O 0.6809(3) 0.0210(2) 0.79462(14) 0.0770(11) Uani 1 1 d U . . O5 O 0.3465(3) 0.66505(17) 0.95932(14) 0.0611(9) Uani 1 1 d U . . O6 O 0.3811(3) 0.8211(2) 0.79872(15) 0.0831(12) Uani 1 1 d U . . O7 O 0.4004(3) 0.90028(16) 0.99196(15) 0.0674(10) Uani 1 1 d U . . O8 O 0.1425(2) 0.85645(17) 0.91728(14) 0.0625(9) Uani 1 1 d U . . C1A1 C 0.0068(18) 0.9644(13) 1.0166(11) 0.149(12) Uiso 0.30 1 d PDU D 1 H1A1 H -0.0137 1.0134 1.0070 0.223 Uiso 0.30 1 calc PR D 1 H1A2 H -0.0504 0.9513 1.0368 0.223 Uiso 0.30 1 calc PR D 1 H1A3 H 0.0230 0.9369 0.9838 0.223 Uiso 0.30 1 calc PR D 1 C1A2 C 0.0996(11) 0.9515(6) 1.0504(6) 0.073(4) Uiso 0.40 1 d PDU D 1 H1A4 H 0.1567 0.9631 1.0285 0.088 Uiso 0.40 1 calc PR D 1 H1A5 H 0.0840 0.9844 1.0807 0.088 Uiso 0.40 1 calc PR D 1 C1B1 C 0.0561(12) 0.9934(7) 1.0229(7) 0.091(5) Uiso 0.40 1 d PDU D 2 H1B1 H 0.0773 1.0323 1.0054 0.136 Uiso 0.40 1 calc PR D 2 H1B2 H 0.0238 1.0076 1.0583 0.136 Uiso 0.40 1 calc PR D 2 H1B3 H 0.0061 0.9785 1.0006 0.136 Uiso 0.40 1 calc PR D 2 C1B2 C 0.1486(18) 0.9352(16) 1.0297(9) 0.42(5) Uiso 0.30 1 d PDU D 2 H1B4 H 0.2084 0.9545 1.0378 0.504 Uiso 0.30 1 calc PR D 2 H1B5 H 0.1647 0.9106 0.9951 0.504 Uiso 0.30 1 calc PR D 2 C123 C 0.1384(18) 0.8836(8) 1.0730(10) 0.154(11) Uiso 0.30 1 d PDU . . H12G H 0.1675 0.8515 1.0434 0.185 Uiso 0.02 1 calc PR D 1 H12H H 0.0795 0.8679 1.0899 0.185 Uiso 0.02 1 calc PR D 1 H12I H 0.0689 0.8974 1.0908 0.185 Uiso 0.02 1 calc PR D 2 H12J H 0.1454 0.8378 1.0567 0.185 Uiso 0.02 1 calc PR D 2 C124 C 0.2196(13) 0.8790(8) 1.1139(7) 0.159(7) Uiso 0.50 1 d PDU D . H1AA H 0.1969 0.9180 1.1391 0.191 Uiso 0.02 1 calc PR . . H1BA H 0.2843 0.8842 1.0953 0.191 Uiso 0.02 1 calc PR . . C125 C 0.2428(18) 0.8131(10) 1.1460(9) 0.118(8) Uiso 0.30 1 d PDU . . H1F5 H 0.2939 0.8153 1.1730 0.142 Uiso 0.02 1 calc PR D . H1G5 H 0.2708 0.7743 1.1218 0.142 Uiso 0.02 1 calc PR . . H1H5 H 0.1789 0.8068 1.1639 0.142 Uiso 0.02 1 calc PR . . 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 0.02939(19) 0.02421(19) 0.02128(19) -0.00295(15) -0.00179(14) -0.01155(15) Ge2 0.0315(2) 0.0558(3) 0.0354(2) -0.0263(2) -0.00414(18) 0.00117(19) Fe1 0.0327(3) 0.0349(3) 0.0289(3) -0.0018(2) -0.0040(2) -0.0099(2) Fe2 0.0320(3) 0.0369(3) 0.0358(3) -0.0082(3) 0.0052(2) -0.0016(2) Si1 0.0195(4) 0.0215(4) 0.0220(5) -0.0039(4) -0.0002(4) -0.0076(3) Si2 0.0167(4) 0.0195(4) 0.0227(5) -0.0048(4) -0.0003(3) -0.0027(3) Si3 0.0249(5) 0.0518(7) 0.0264(5) -0.0181(5) -0.0011(4) -0.0006(4) Si4 0.0212(4) 0.0280(5) 0.0260(5) -0.0073(4) 0.0039(4) -0.0091(4) Cl1 0.0260(4) 0.0244(4) 0.0268(4) -0.0054(3) -0.0009(3) -0.0100(3) Cl2 0.0318(4) 0.0340(5) 0.0248(4) -0.0052(4) -0.0004(3) -0.0141(4) N1 0.0482(18) 0.0363(17) 0.0269(17) -0.0074(14) 0.0067(14) -0.0237(14) N2 0.0323(15) 0.0230(14) 0.0325(17) -0.0060(13) 0.0000(13) -0.0127(12) N3 0.0480(19) 0.0440(19) 0.0222(16) -0.0001(14) -0.0007(14) -0.0210(15) N4 0.053(2) 0.0329(17) 0.0271(17) -0.0058(14) -0.0008(14) -0.0155(15) C1 0.0195(15) 0.0169(15) 0.0306(19) -0.0017(14) -0.0005(13) -0.0051(12) C2 0.0202(16) 0.0258(18) 0.043(2) -0.0102(16) 0.0016(15) -0.0064(13) C3 0.0241(18) 0.031(2) 0.082(3) -0.024(2) 0.0076(19) -0.0067(15) C4 0.030(2) 0.032(2) 0.120(4) -0.033(2) 0.012(2) -0.0120(17) C5 0.0233(18) 0.0287(19) 0.083(3) -0.011(2) 0.0115(19) -0.0104(15) C6 0.0215(16) 0.0222(17) 0.036(2) -0.0021(15) 0.0009(14) -0.0054(13) C7 0.0229(17) 0.0304(19) 0.041(2) -0.0173(17) 0.0040(15) -0.0101(14) C8 0.0226(17) 0.034(2) 0.067(3) -0.0219(19) 0.0055(18) -0.0071(15) C9 0.040(2) 0.059(3) 0.039(2) -0.026(2) 0.0037(18) -0.0177(19) C10 0.044(2) 0.054(3) 0.126(5) -0.038(3) 0.013(3) -0.020(2) C11A 0.097(4) 0.077(4) 0.116(5) -0.027(3) 0.026(4) -0.065(3) C12A 0.042(3) 0.059(3) 0.113(5) -0.039(3) -0.008(3) -0.020(2) C11B 0.082(7) 0.073(7) 0.103(7) -0.031(6) 0.015(6) -0.043(6) C12B 0.073(5) 0.077(6) 0.114(7) -0.025(6) 0.010(5) -0.041(5) C13 0.0198(16) 0.0355(19) 0.033(2) -0.0056(16) 0.0065(14) -0.0094(14) C14 0.0294(19) 0.043(2) 0.060(3) -0.021(2) 0.0006(19) 0.0028(17) C15 0.082(3) 0.069(3) 0.042(3) 0.000(2) 0.023(2) -0.033(3) C16 0.0323(18) 0.0285(18) 0.0224(18) -0.0022(15) -0.0019(14) -0.0128(14) C17 0.047(2) 0.037(2) 0.043(2) 0.0002(19) 0.0048(18) -0.0217(18) C18 0.042(2) 0.029(2) 0.057(3) -0.0023(19) 0.0028(19) -0.0181(17) C19 0.105(4) 0.067(3) 0.055(3) -0.036(2) 0.053(3) -0.064(3) C20A 0.050(4) 0.061(6) 0.072(5) -0.052(4) 0.009(3) -0.029(4) C21A 0.075(4) 0.035(5) 0.033(4) 0.004(4) 0.005(3) -0.005(4) C20B 0.048(5) 0.088(7) 0.076(5) -0.071(5) -0.011(4) -0.017(5) C21B 0.132(6) 0.046(7) 0.051(6) 0.000(6) 0.013(5) 0.019(5) C22 0.068(3) 0.053(3) 0.071(3) 0.002(3) 0.021(3) -0.033(2) C23 0.075(3) 0.039(2) 0.110(5) -0.017(3) 0.027(3) -0.032(2) C24 0.0331(19) 0.0277(18) 0.034(2) -0.0082(16) -0.0024(15) -0.0107(15) C25 0.035(2) 0.032(2) 0.051(3) 0.0043(19) -0.0004(18) -0.0044(16) C26 0.046(2) 0.047(2) 0.049(3) -0.022(2) -0.010(2) -0.0118(19) C27 0.0236(15) 0.0193(16) 0.0226(17) -0.0023(14) -0.0043(13) -0.0010(13) C28 0.0285(17) 0.0259(18) 0.0246(18) -0.0024(15) -0.0023(14) 0.0040(14) C29 0.0350(19) 0.035(2) 0.0235(19) -0.0067(16) -0.0019(15) 0.0067(16) C30 0.039(2) 0.032(2) 0.0261(19) -0.0056(16) -0.0095(15) 0.0044(16) C31 0.0295(18) 0.037(2) 0.0289(19) -0.0069(17) -0.0105(15) 0.0022(15) C32 0.0282(17) 0.0210(17) 0.0271(18) -0.0030(15) -0.0062(14) -0.0002(13) C33 0.0252(17) 0.054(2) 0.028(2) -0.0210(18) -0.0001(15) 0.0018(16) C34 0.059(3) 0.052(3) 0.079(4) -0.032(2) -0.044(3) 0.028(2) C35 0.048(3) 0.175(6) 0.043(3) -0.046(3) 0.020(2) -0.047(3) C36 0.049(2) 0.046(2) 0.029(2) -0.0047(19) -0.0122(18) -0.0005(19) C37 0.038(2) 0.060(3) 0.024(2) -0.0156(19) -0.0019(16) -0.0086(18) C38 0.140(5) 0.071(3) 0.037(3) -0.006(3) -0.007(3) -0.038(4) C39 0.0230(16) 0.0327(19) 0.030(2) -0.0092(16) -0.0078(14) -0.0017(14) C40 0.033(2) 0.043(2) 0.040(2) -0.0134(18) -0.0092(17) -0.0121(17) C41 0.0274(19) 0.040(2) 0.050(3) -0.0088(19) -0.0068(17) 0.0041(16) C42 0.0204(15) 0.0218(16) 0.0324(19) -0.0072(14) -0.0040(14) -0.0025(12) C43 0.0199(16) 0.0256(17) 0.043(2) -0.0123(16) -0.0030(15) -0.0048(13) C44 0.0215(17) 0.0283(18) 0.051(2) -0.0124(17) -0.0013(16) -0.0007(14) C45 0.0324(19) 0.0292(19) 0.052(3) -0.0100(18) -0.0071(18) 0.0032(15) C46 0.037(2) 0.0274(19) 0.047(2) -0.0013(18) -0.0047(17) -0.0039(15) C47 0.0267(17) 0.0222(17) 0.035(2) -0.0014(16) -0.0047(15) -0.0006(13) C48 0.0229(17) 0.0279(18) 0.048(2) -0.0144(17) 0.0082(16) -0.0069(14) C49 0.036(2) 0.050(2) 0.059(3) -0.032(2) 0.0191(19) -0.0221(18) C50 0.033(2) 0.045(2) 0.050(3) -0.016(2) 0.0014(18) -0.0127(17) C51 0.042(2) 0.038(2) 0.064(3) -0.003(2) -0.008(2) 0.0124(18) C52 0.071(3) 0.028(2) 0.051(3) 0.003(2) 0.015(2) 0.0051(19) C53A 0.088(5) 0.053(4) 0.084(5) -0.012(3) -0.047(4) 0.030(3) C53B 0.073(8) 0.049(10) 0.094(11) -0.013(10) -0.047(10) 0.021(7) C54 0.0333(19) 0.0253(18) 0.040(2) 0.0083(17) 0.0002(16) -0.0006(15) C55 0.034(2) 0.034(2) 0.054(3) 0.0073(19) 0.0003(18) -0.0069(16) C56 0.055(3) 0.044(2) 0.040(2) 0.008(2) 0.001(2) -0.004(2) C57 0.043(2) 0.048(2) 0.026(2) -0.0015(18) -0.0070(17) -0.0168(18) C58 0.032(2) 0.050(2) 0.057(3) -0.016(2) 0.0075(19) -0.0184(18) C59 0.040(2) 0.048(2) 0.039(2) 0.002(2) -0.0038(18) -0.0028(19) C60 0.043(2) 0.064(3) 0.043(3) 0.013(2) -0.0082(19) -0.016(2) C61 0.0238(18) 0.065(3) 0.029(2) -0.0216(19) 0.0001(15) -0.0027(17) C62 0.0235(18) 0.072(3) 0.031(2) -0.011(2) -0.0027(16) 0.0079(18) C63 0.030(2) 0.088(3) 0.029(2) -0.009(2) -0.0030(17) 0.008(2) C64 0.029(2) 0.127(5) 0.032(2) -0.036(3) -0.0020(18) 0.006(2) C65 0.029(2) 0.109(4) 0.044(2) -0.039(3) -0.0035(19) -0.015(2) C66 0.0232(19) 0.091(3) 0.039(2) -0.038(2) 0.0061(16) -0.011(2) C67 0.032(2) 0.065(3) 0.026(2) 0.002(2) -0.0026(16) -0.0008(18) C68 0.040(2) 0.069(3) 0.039(3) 0.004(2) 0.0016(19) 0.003(2) C69 0.037(2) 0.080(3) 0.035(2) 0.004(2) 0.0009(18) 0.000(2) C70 0.055(3) 0.165(6) 0.040(3) -0.043(3) -0.012(2) -0.004(3) C71 0.056(3) 0.073(3) 0.026(2) -0.012(2) 0.0014(19) -0.014(2) C72 0.064(3) 0.146(6) 0.044(3) -0.005(3) -0.019(3) 0.019(3) C73 0.036(2) 0.089(3) 0.044(3) -0.037(2) 0.0059(19) -0.023(2) C74 0.061(3) 0.102(4) 0.068(4) -0.046(3) 0.005(3) -0.029(3) C75 0.036(2) 0.105(4) 0.058(3) -0.038(3) 0.010(2) -0.030(2) C76 0.039(2) 0.0325(19) 0.0229(19) -0.0085(16) 0.0025(15) -0.0053(16) C77 0.050(2) 0.039(2) 0.030(2) -0.0060(18) -0.0028(18) -0.0169(18) C78 0.067(3) 0.044(2) 0.024(2) -0.0070(18) -0.0042(19) -0.022(2) C79 0.096(4) 0.077(3) 0.027(2) 0.008(2) -0.003(2) -0.049(3) C80 0.090(4) 0.083(4) 0.083(4) 0.000(3) 0.046(3) -0.034(3) C81 0.081(4) 0.119(5) 0.103(5) 0.079(4) -0.027(3) -0.037(3) C82 0.082(3) 0.052(3) 0.048(3) -0.006(2) -0.005(2) -0.036(2) C83 0.133(5) 0.089(4) 0.026(2) -0.005(3) -0.007(3) -0.062(4) C84 0.073(3) 0.032(2) 0.037(2) -0.0031(18) 0.000(2) -0.023(2) C85 0.099(4) 0.046(3) 0.050(3) 0.005(2) -0.015(3) -0.024(3) C86 0.083(3) 0.049(3) 0.057(3) -0.004(2) 0.013(3) -0.032(2) C87 0.0320(18) 0.0277(18) 0.037(2) -0.0077(16) 0.0083(16) -0.0091(14) C88 0.0323(18) 0.0326(19) 0.040(2) -0.0038(17) 0.0092(16) -0.0063(15) C89 0.044(2) 0.036(2) 0.054(3) 0.001(2) 0.011(2) 0.0015(17) C90 0.064(3) 0.030(2) 0.056(3) 0.000(2) 0.014(2) -0.0017(19) C91 0.055(2) 0.029(2) 0.060(3) -0.007(2) 0.017(2) -0.0161(18) C92 0.041(2) 0.033(2) 0.042(2) -0.0101(18) 0.0138(18) -0.0150(16) C93 0.0253(18) 0.041(2) 0.039(2) 0.0060(19) 0.0039(16) -0.0021(16) C94 0.031(2) 0.063(3) 0.051(3) 0.001(2) 0.0110(19) -0.0038(19) C95 0.034(2) 0.054(3) 0.056(3) 0.015(2) -0.0054(19) -0.0089(19) C96 0.108(4) 0.033(2) 0.078(4) 0.000(3) 0.029(3) -0.001(3) C97 0.133(6) 0.069(4) 0.113(5) 0.022(4) 0.004(4) -0.005(4) C98 0.140(6) 0.055(4) 0.261(12) 0.007(6) 0.021(7) 0.010(4) C99 0.0362(19) 0.037(2) 0.047(2) -0.0047(18) 0.0091(18) -0.0205(16) C100 0.034(2) 0.044(2) 0.051(3) -0.008(2) 0.0144(18) -0.0124(17) C101 0.053(3) 0.056(3) 0.072(3) -0.011(2) 0.015(2) -0.036(2) C102 0.0183(15) 0.0324(19) 0.0292(19) -0.0048(15) 0.0027(14) -0.0035(13) C103 0.0230(16) 0.0331(19) 0.0302(19) -0.0017(16) -0.0005(14) -0.0050(14) C104 0.0234(17) 0.050(2) 0.034(2) 0.0018(18) 0.0038(15) -0.0129(16) C105 0.0249(18) 0.060(3) 0.036(2) -0.0112(19) 0.0085(16) -0.0098(17) C106 0.0274(19) 0.059(3) 0.036(2) -0.020(2) 0.0074(16) -0.0093(17) C107 0.0224(17) 0.043(2) 0.031(2) -0.0150(17) 0.0074(14) -0.0073(15) C108 0.0317(18) 0.0314(19) 0.033(2) -0.0007(16) 0.0037(15) -0.0121(15) C109 0.059(3) 0.037(2) 0.061(3) 0.006(2) 0.003(2) -0.017(2) C110 0.072(3) 0.048(3) 0.092(4) -0.012(3) -0.045(3) -0.015(2) C111 0.043(2) 0.097(4) 0.040(3) -0.028(3) 0.018(2) -0.030(2) C112 0.057(3) 0.136(5) 0.037(3) 0.021(3) 0.014(2) 0.001(3) C113 0.037(2) 0.071(3) 0.079(4) -0.013(3) 0.033(2) -0.006(2) C114 0.0308(19) 0.055(2) 0.042(2) -0.030(2) 0.0135(17) -0.0169(17) C115 0.048(2) 0.050(2) 0.068(3) -0.034(2) 0.024(2) -0.020(2) C116 0.036(2) 0.092(3) 0.049(3) -0.045(2) 0.0135(19) -0.030(2) C117 0.045(2) 0.045(2) 0.042(2) -0.010(2) -0.0035(19) -0.0058(19) C118 0.036(2) 0.064(3) 0.052(3) -0.006(2) 0.007(2) 0.002(2) C119 0.039(2) 0.042(2) 0.059(3) -0.014(2) 0.015(2) -0.0040(18) C120 0.039(2) 0.042(2) 0.048(3) 0.000(2) 0.0069(19) -0.0030(18) O1 0.076(2) 0.0400(16) 0.0455(18) -0.0071(14) -0.0086(15) -0.0288(15) O2 0.0539(19) 0.086(2) 0.093(3) -0.061(2) 0.0366(19) -0.0379(18) O3 0.059(2) 0.078(2) 0.062(2) 0.0294(19) 0.0054(17) -0.0124(17) O4 0.049(2) 0.119(3) 0.064(2) 0.030(2) -0.0184(17) -0.022(2) O5 0.072(2) 0.0476(19) 0.065(2) 0.0024(17) -0.0038(17) -0.0157(16) O6 0.073(2) 0.118(3) 0.043(2) 0.015(2) 0.0194(18) 0.003(2) O7 0.064(2) 0.053(2) 0.085(3) -0.0379(19) 0.0128(18) -0.0141(16) O8 0.0405(17) 0.066(2) 0.072(2) -0.0009(18) 0.0087(16) 0.0033(15) _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 C16 2.020(3) . ? Ge1 Si1 2.2480(10) . ? Ge1 Fe1 2.3780(6) . ? Ge2 C76 2.007(4) . ? Ge2 Si3 2.2143(11) . ? Ge2 Fe2 2.3648(6) . ? Fe1 C58 1.760(4) . ? Fe1 C60 1.764(4) . ? Fe1 C59 1.772(4) . ? Fe1 C57 1.791(4) . ? Fe2 C120 1.766(4) . ? Fe2 C119 1.774(5) . ? Fe2 C117 1.781(5) . ? Fe2 C118 1.786(5) . ? Si1 C1 1.907(3) . ? Si1 Si2 2.3767(12) . ? Si2 C42 1.910(3) . ? Si2 C27 1.926(3) . ? Si2 Cl1 2.1118(11) . ? Si3 C61 1.899(4) . ? Si3 Si4 2.3663(13) . ? Si4 C102 1.906(3) . ? Si4 C87 1.910(4) . ? Si4 Cl2 2.1109(12) . ? N1 C16 1.351(4) . ? N1 C17 1.388(4) . ? N1 C19 1.492(5) . ? N2 C16 1.339(4) . ? N2 C18 1.390(4) . ? N2 C24 1.483(4) . ? N3 C76 1.342(4) . ? N3 C77 1.378(5) . ? N3 C79 1.494(5) . ? N4 C76 1.345(5) . ? N4 C78 1.402(5) . ? N4 C84 1.467(5) . ? C1 C2 1.413(5) . ? C1 C6 1.425(4) . ? C2 C3 1.391(5) . ? C2 C7 1.520(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 C10 1.542(6) . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C13 1.516(5) . ? C7 C8 1.528(5) . ? C7 C9 1.526(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11A 1.478(6) . ? C10 C12B 1.503(9) . ? C10 C11B 1.510(9) . ? C10 C12A 1.533(6) . ? C10 H10A 1.0000 . ? C10 H10B 1.0000 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C11B H11D 0.9842 . ? C11B H11E 0.9840 . ? C11B H11F 0.9843 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13 C14 1.514(5) . ? C13 C15 1.534(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.341(6) . ? C17 C22 1.496(5) . ? C18 C23 1.510(5) . ? C19 C20A 1.481(7) . ? C19 C21B 1.498(8) . ? C19 C21A 1.545(7) . ? C19 C20B 1.557(8) . ? C19 H19A 1.0000 . ? C19 H19B 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.508(5) . ? C24 C26 1.520(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.408(4) . ? C27 C32 1.418(5) . ? C28 C29 1.391(5) . ? C28 C33 1.519(5) . ? C29 C30 1.407(5) . ? C29 H29 0.9500 . ? C30 C31 1.363(5) . ? C30 C36 1.515(5) . ? C31 C32 1.393(5) . ? C31 H31 0.9500 . ? C32 C39 1.523(5) . ? C33 C34 1.528(6) . ? C33 C35 1.530(6) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.444(6) . ? C36 C37 1.487(5) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.534(5) . ? C39 C40 1.542(5) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.409(5) . ? C42 C43 1.423(4) . ? C43 C44 1.383(5) . ? C43 C48 1.511(5) . ? C44 C45 1.372(5) . ? C44 H44 0.9500 . ? C45 C46 1.397(5) . ? C45 C51 1.532(5) . ? C46 C47 1.391(5) . ? C46 H46 0.9500 . ? C47 C54 1.537(5) . ? C48 C50 1.541(5) . ? C48 C49 1.543(5) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53A 1.514(6) . ? C51 C52 1.520(5) . ? C51 C53B 1.519(10) . ? C51 H51A 1.0000 . ? C51 H51B 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? C54 C56 1.528(6) . ? C54 C55 1.543(5) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O1 1.155(4) . ? C58 O2 1.161(5) . ? C59 O3 1.162(5) . ? C60 O4 1.151(5) . ? C61 C66 1.399(5) . ? C61 C62 1.439(6) . ? C62 C63 1.393(5) . ? C62 C67 1.508(6) . ? C63 C64 1.363(7) . ? C63 H63 0.9500 . ? C64 C65 1.389(7) . ? C64 C70 1.529(6) . ? C65 C66 1.414(6) . ? C65 H65 0.9500 . ? C66 C73 1.516(6) . ? C67 C69 1.527(5) . ? C67 C68 1.536(6) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C72 1.399(7) . ? C70 C71 1.519(7) . ? C70 H70 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.524(7) . ? C73 C75 1.535(6) . ? C73 H73 1.0000 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C77 C78 1.353(5) . ? C77 C82 1.492(5) . ? C78 C83 1.500(6) . ? C79 C80 1.513(7) . ? C79 C81 1.512(8) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.519(6) . ? C84 C86 1.534(6) . ? C84 H84 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.421(5) . ? C87 C92 1.432(5) . ? C88 C89 1.392(5) . ? C88 C93 1.523(5) . ? C89 C90 1.384(6) . ? C89 H89 0.9500 . ? C90 C91 1.378(6) . ? C90 C96 1.516(6) . ? C91 C92 1.376(5) . ? C91 H91 0.9500 . ? C92 C99 1.518(5) . ? C93 C95 1.523(6) . ? C93 C94 1.550(5) . ? C93 H93 1.0000 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.438(8) . ? C96 C98 1.469(9) . ? C96 H96 1.0000 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C100 1.519(5) . ? C99 C101 1.528(5) . ? C99 H99 1.0000 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C101 H10F 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C102 C107 1.413(5) . ? C102 C103 1.428(4) . ? C103 C104 1.399(5) . ? C103 C108 1.511(5) . ? C104 C105 1.383(5) . ? C104 H104 0.9500 . ? C105 C106 1.372(5) . ? C105 C111 1.534(5) . ? C106 C107 1.400(5) . ? C106 H106 0.9500 . ? C107 C114 1.523(5) . ? C108 C110 1.516(6) . ? C108 C109 1.537(5) . ? C108 H108 1.0000 . ? C109 H10I 0.9800 . ? C109 H10J 0.9800 . ? C109 H10K 0.9800 . ? C110 H11G 0.9800 . ? C110 H11H 0.9800 . ? C110 H11I 0.9800 . ? C111 C112 1.490(7) . ? C111 C113 1.510(7) . ? C111 H111 1.0000 . ? C112 H11J 0.9800 . ? C112 H11K 0.9800 . ? C112 H11L 0.9800 . ? C113 H11M 0.9800 . ? C113 H11N 0.9800 . ? C113 H11O 0.9800 . ? C114 C115 1.520(6) . ? C114 C116 1.551(6) . ? C114 H114 1.0000 . ? C115 H11P 0.9800 . ? C115 H11Q 0.9800 . ? C115 H11R 0.9800 . ? C116 H11S 0.9800 . ? C116 H11T 0.9800 . ? C116 H11U 0.9800 . ? C117 O5 1.153(5) . ? C118 O6 1.152(5) . ? C119 O7 1.157(5) . ? C120 O8 1.146(5) . ? C1A1 C1A2 1.485(9) . ? C1A1 H1A1 0.9800 . ? C1A1 H1A2 0.9800 . ? C1A1 H1A3 0.9800 . ? C1A2 C123 1.443(9) . ? C1A2 H1A4 0.9900 . ? C1A2 H1A5 0.9900 . ? C1B1 C1B2 1.488(10) . ? C1B1 H1B1 0.9800 . ? C1B1 H1B2 0.9800 . ? C1B1 H1B3 0.9800 . ? C1B2 C123 1.505(10) . ? C1B2 H1B4 0.9900 . ? C1B2 H1B5 0.9900 . ? C123 C124 1.493(10) . ? C123 H12G 0.9900 . ? C123 H12H 0.9900 . ? C123 H12I 0.9900 . ? C123 H12J 0.9900 . ? C124 C125 1.501(9) . ? C124 H1AA 0.9900 . ? C124 H1BA 0.9900 . ? C125 H1F5 0.9800 . ? C125 H1G5 0.9800 . ? C125 H1H5 0.9800 . ? 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 C16 Ge1 Si1 115.59(10) . . ? C16 Ge1 Fe1 111.19(10) . . ? Si1 Ge1 Fe1 127.95(3) . . ? C76 Ge2 Si3 117.95(10) . . ? C76 Ge2 Fe2 110.32(10) . . ? Si3 Ge2 Fe2 131.16(4) . . ? C58 Fe1 C60 91.3(2) . . ? C58 Fe1 C59 118.31(19) . . ? C60 Fe1 C59 94.87(19) . . ? C58 Fe1 C57 120.17(18) . . ? C60 Fe1 C57 92.7(2) . . ? C59 Fe1 C57 120.72(19) . . ? C58 Fe1 Ge1 84.33(14) . . ? C60 Fe1 Ge1 175.46(15) . . ? C59 Fe1 Ge1 88.33(13) . . ? C57 Fe1 Ge1 88.40(12) . . ? C120 Fe2 C119 93.13(19) . . ? C120 Fe2 C117 94.37(19) . . ? C119 Fe2 C117 118.3(2) . . ? C120 Fe2 C118 92.54(19) . . ? C119 Fe2 C118 120.1(2) . . ? C117 Fe2 C118 120.6(2) . . ? C120 Fe2 Ge2 177.75(15) . . ? C119 Fe2 Ge2 89.12(13) . . ? C117 Fe2 Ge2 84.61(13) . . ? C118 Fe2 Ge2 86.27(13) . . ? C1 Si1 Ge1 106.89(11) . . ? C1 Si1 Si2 121.78(11) . . ? Ge1 Si1 Si2 122.58(4) . . ? C42 Si2 C27 106.95(14) . . ? C42 Si2 Cl1 115.76(11) . . ? C27 Si2 Cl1 100.12(10) . . ? C42 Si2 Si1 112.13(11) . . ? C27 Si2 Si1 123.09(10) . . ? Cl1 Si2 Si1 98.32(5) . . ? C61 Si3 Ge2 111.81(12) . . ? C61 Si3 Si4 120.46(12) . . ? Ge2 Si3 Si4 125.32(5) . . ? C102 Si4 C87 106.23(15) . . ? C102 Si4 Cl2 117.23(11) . . ? C87 Si4 Cl2 101.01(12) . . ? C102 Si4 Si3 108.47(11) . . ? C87 Si4 Si3 125.34(11) . . ? Cl2 Si4 Si3 99.04(5) . . ? C16 N1 C17 109.8(3) . . ? C16 N1 C19 123.1(3) . . ? C17 N1 C19 126.8(3) . . ? C16 N2 C18 109.3(3) . . ? C16 N2 C24 122.7(3) . . ? C18 N2 C24 127.9(3) . . ? C76 N3 C77 110.9(3) . . ? C76 N3 C79 123.0(3) . . ? C77 N3 C79 126.1(3) . . ? C76 N4 C78 109.1(3) . . ? C76 N4 C84 123.2(3) . . ? C78 N4 C84 127.6(3) . . ? C2 C1 C6 117.9(3) . . ? C2 C1 Si1 120.3(2) . . ? C6 C1 Si1 121.4(2) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 C7 116.3(3) . . ? C1 C2 C7 124.0(3) . . ? C4 C3 C2 122.7(4) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 117.5(3) . . ? C3 C4 C10 119.1(4) . . ? C5 C4 C10 123.0(3) . . ? C4 C5 C6 122.5(3) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C13 116.9(3) . . ? C1 C6 C13 123.4(3) . . ? C2 C7 C8 111.2(3) . . ? C2 C7 C9 111.4(3) . . ? C8 C7 C9 111.4(3) . . ? C2 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11A C10 C12B 65.8(12) . . ? C11A C10 C11B 45.2(11) . . ? C12B C10 C11B 110.2(10) . . ? C11A C10 C4 110.8(5) . . ? C12B C10 C4 127.3(15) . . ? C11B C10 C4 77.5(13) . . ? C11A C10 C12A 108.5(5) . . ? C12B C10 C12A 42.7(12) . . ? C11B C10 C12A 152.2(12) . . ? C4 C10 C12A 112.5(4) . . ? C11A C10 H10A 108.4 . . ? C12B C10 H10A 123.0 . . ? C11B C10 H10A 91.6 . . ? C4 C10 H10A 108.3 . . ? C12A C10 H10A 108.3 . . ? C11A C10 H10B 122.2 . . ? C12B C10 H10B 111.9 . . ? C11B C10 H10B 112.2 . . ? C4 C10 H10B 112.2 . . ? C12A C10 H10B 88.6 . . ? H10A C10 H10B 20.6 . . ? C10 C11A H11A 109.4 . . ? C10 C11A H11B 109.5 . . ? C10 C11A H11C 109.4 . . ? C10 C12A H12A 109.5 . . ? C10 C12A H12B 109.5 . . ? C10 C12A H12C 109.5 . . ? C10 C11B H11D 109.9 . . ? C10 C11B H11E 109.6 . . ? H11D C11B H11E 109.0 . . ? C10 C11B H11F 110.1 . . ? H11D C11B H11F 109.0 . . ? H11E C11B H11F 109.1 . . ? C10 C12B H12D 109.7 . . ? C10 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C10 C12B H12F 109.2 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C14 C13 C6 111.4(3) . . ? C14 C13 C15 109.7(3) . . ? C6 C13 C15 111.1(3) . . ? C14 C13 H13 108.2 . . ? C6 C13 H13 108.2 . . ? C15 C13 H13 108.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 N1 106.6(3) . . ? N2 C16 Ge1 129.6(2) . . ? N1 C16 Ge1 122.8(2) . . ? C18 C17 N1 106.5(3) . . ? C18 C17 C22 128.5(4) . . ? N1 C17 C22 125.0(4) . . ? C17 C18 N2 107.7(3) . . ? C17 C18 C23 127.2(4) . . ? N2 C18 C23 125.1(4) . . ? C20A C19 N1 118.6(6) . . ? C20A C19 C21B 113.0(9) . . ? N1 C19 C21B 121.6(8) . . ? C20A C19 C21A 113.6(7) . . ? N1 C19 C21A 108.0(6) . . ? C21B C19 C21A 21.1(7) . . ? C20A C19 C20B 26.6(4) . . ? N1 C19 C20B 100.9(6) . . ? C21B C19 C20B 114.3(10) . . ? C21A C19 C20B 104.9(7) . . ? C20A C19 H19A 105.1 . . ? N1 C19 H19A 105.1 . . ? C21B C19 H19A 85.4 . . ? C21A C19 H19A 105.1 . . ? C20B C19 H19A 131.2 . . ? C20A C19 H19B 81.9 . . ? N1 C19 H19B 106.3 . . ? C21B C19 H19B 106.3 . . ? C21A C19 H19B 127.3 . . ? C20B C19 H19B 106.3 . . ? H19A C19 H19B 26.6 . . ? C19 C20A H20A 109.5 . . ? C19 C20A H20B 109.5 . . ? C19 C20A H20C 109.5 . . ? C19 C21A H21A 109.5 . . ? C19 C21A H21B 109.5 . . ? C19 C21A H21C 109.5 . . ? C19 C20B H20D 109.5 . . ? C19 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19 C21B H21D 109.5 . . ? C19 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C25 111.3(3) . . ? N2 C24 C26 111.0(3) . . ? C25 C24 C26 114.1(3) . . ? N2 C24 H24 106.7 . . ? C25 C24 H24 106.7 . . ? C26 C24 H24 106.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 117.2(3) . . ? C28 C27 Si2 124.7(2) . . ? C32 C27 Si2 118.1(2) . . ? C29 C28 C27 120.0(3) . . ? C29 C28 C33 117.8(3) . . ? C27 C28 C33 122.1(3) . . ? C28 C29 C30 122.6(3) . . ? C28 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C31 C30 C29 116.9(3) . . ? C31 C30 C36 121.4(3) . . ? C29 C30 C36 121.7(3) . . ? C30 C31 C32 122.7(3) . . ? C30 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C31 C32 C27 120.6(3) . . ? C31 C32 C39 115.0(3) . . ? C27 C32 C39 124.3(3) . . ? C28 C33 C34 109.0(3) . . ? C28 C33 C35 114.1(3) . . ? C34 C33 C35 111.4(4) . . ? C28 C33 H33 107.3 . . ? C34 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 111.1(4) . . ? C38 C36 C30 110.1(4) . . ? C37 C36 C30 113.3(3) . . ? C38 C36 H36 107.3 . . ? C37 C36 H36 107.3 . . ? C30 C36 H36 107.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C32 C39 C41 111.9(3) . . ? C32 C39 C40 110.9(3) . . ? C41 C39 C40 112.1(3) . . ? C32 C39 H39 107.2 . . ? C41 C39 H39 107.2 . . ? C40 C39 H39 107.2 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C47 C42 C43 117.6(3) . . ? C47 C42 Si2 114.4(2) . . ? C43 C42 Si2 127.9(3) . . ? C44 C43 C42 119.4(3) . . ? C44 C43 C48 116.4(3) . . ? C42 C43 C48 124.2(3) . . ? C45 C44 C43 123.1(3) . . ? C45 C44 H44 118.4 . . ? C43 C44 H44 118.4 . . ? C44 C45 C46 117.7(3) . . ? C44 C45 C51 120.9(4) . . ? C46 C45 C51 121.4(4) . . ? C47 C46 C45 121.3(4) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C42 120.6(3) . . ? C46 C47 C54 116.3(3) . . ? C42 C47 C54 123.1(3) . . ? C43 C48 C50 112.8(3) . . ? C43 C48 C49 111.6(3) . . ? C50 C48 C49 108.7(3) . . ? C43 C48 H48 107.9 . . ? C50 C48 H48 107.9 . . ? C49 C48 H48 107.9 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C53A C51 C52 110.9(4) . . ? C53A C51 C53B 52(3) . . ? C52 C51 C53B 154(2) . . ? C53A C51 C45 111.1(4) . . ? C52 C51 C45 111.4(3) . . ? C53B C51 C45 95(2) . . ? C53A C51 H51A 107.7 . . ? C52 C51 H51A 107.7 . . ? C53B C51 H51A 66.3 . . ? C45 C51 H51A 107.7 . . ? C53A C51 H51B 137.1 . . ? C52 C51 H51B 91.9 . . ? C53B C51 H51B 91.6 . . ? C45 C51 H51B 91.9 . . ? H51A C51 H51B 29.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53A H53A 109.5 . . ? C51 C53A H53B 109.5 . . ? C51 C53A H53C 109.5 . . ? C51 C53B H53D 109.7 . . ? C51 C53B H53E 109.2 . . ? H53D C53B H53E 109.5 . . ? C51 C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? C56 C54 C47 112.1(3) . . ? C56 C54 C55 111.2(3) . . ? C47 C54 C55 110.5(3) . . ? C56 C54 H54 107.6 . . ? C47 C54 H54 107.6 . . ? C55 C54 H54 107.6 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O1 C57 Fe1 176.9(4) . . ? O2 C58 Fe1 176.8(4) . . ? O3 C59 Fe1 177.8(4) . . ? O4 C60 Fe1 178.3(5) . . ? C66 C61 C62 117.6(4) . . ? C66 C61 Si3 123.1(3) . . ? C62 C61 Si3 119.3(3) . . ? C63 C62 C61 119.9(4) . . ? C63 C62 C67 117.3(4) . . ? C61 C62 C67 122.8(3) . . ? C64 C63 C62 122.7(5) . . ? C64 C63 H63 118.6 . . ? C62 C63 H63 118.6 . . ? C63 C64 C65 117.8(4) . . ? C63 C64 C70 117.6(5) . . ? C65 C64 C70 124.5(5) . . ? C64 C65 C66 122.3(4) . . ? C64 C65 H65 118.8 . . ? C66 C65 H65 118.9 . . ? C61 C66 C65 119.7(4) . . ? C61 C66 C73 122.7(4) . . ? C65 C66 C73 117.6(4) . . ? C62 C67 C69 111.9(4) . . ? C62 C67 C68 111.1(3) . . ? C69 C67 C68 111.0(4) . . ? C62 C67 H67 107.6 . . ? C69 C67 H67 107.6 . . ? C68 C67 H67 107.6 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C72 C70 C71 117.4(5) . . ? C72 C70 C64 117.2(5) . . ? C71 C70 C64 109.5(4) . . ? C72 C70 H70 103.5 . . ? C71 C70 H70 103.5 . . ? C64 C70 H70 103.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C66 C73 C74 111.3(4) . . ? C66 C73 C75 112.2(4) . . ? C74 C73 C75 109.7(4) . . ? C66 C73 H73 107.9 . . ? C74 C73 H73 107.9 . . ? C75 C73 H73 107.9 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N3 C76 N4 106.5(3) . . ? N3 C76 Ge2 123.0(3) . . ? N4 C76 Ge2 128.4(3) . . ? C78 C77 N3 106.3(3) . . ? C78 C77 C82 127.4(4) . . ? N3 C77 C82 126.2(4) . . ? C77 C78 N4 107.1(3) . . ? C77 C78 C83 128.0(4) . . ? N4 C78 C83 124.9(4) . . ? N3 C79 C80 110.7(4) . . ? N3 C79 C81 111.9(4) . . ? C80 C79 C81 113.7(4) . . ? N3 C79 H79 106.7 . . ? C80 C79 H79 106.7 . . ? C81 C79 H79 106.7 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C77 C82 H82A 109.5 . . ? C77 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C77 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C78 C83 H83A 109.5 . . ? C78 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C78 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N4 C84 C85 112.1(4) . . ? N4 C84 C86 111.1(3) . . ? C85 C84 C86 113.4(4) . . ? N4 C84 H84 106.6 . . ? C85 C84 H84 106.6 . . ? C86 C84 H84 106.6 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 C92 117.3(3) . . ? C88 C87 Si4 117.8(2) . . ? C92 C87 Si4 124.9(3) . . ? C89 C88 C87 119.8(3) . . ? C89 C88 C93 115.6(3) . . ? C87 C88 C93 124.6(3) . . ? C90 C89 C88 122.2(4) . . ? C90 C89 H89 118.9 . . ? C88 C89 H89 118.9 . . ? C91 C90 C89 117.7(4) . . ? C91 C90 C96 119.2(4) . . ? C89 C90 C96 123.1(4) . . ? C90 C91 C92 123.1(4) . . ? C90 C91 H91 118.5 . . ? C92 C91 H91 118.5 . . ? C91 C92 C87 119.6(3) . . ? C91 C92 C99 119.4(3) . . ? C87 C92 C99 120.9(3) . . ? C95 C93 C88 111.5(3) . . ? C95 C93 C94 111.0(3) . . ? C88 C93 C94 111.7(3) . . ? C95 C93 H93 107.5 . . ? C88 C93 H93 107.5 . . ? C94 C93 H93 107.5 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C93 C95 H95A 109.5 . . ? C93 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C93 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C97 C96 C98 105.0(6) . . ? C97 C96 C90 112.0(5) . . ? C98 C96 C90 115.2(5) . . ? C97 C96 H96 108.1 . . ? C98 C96 H96 108.1 . . ? C90 C96 H96 108.1 . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C96 C98 H98A 109.5 . . ? C96 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C96 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C92 C99 C100 109.8(3) . . ? C92 C99 C101 114.8(3) . . ? C100 C99 C101 109.1(3) . . ? C92 C99 H99 107.7 . . ? C100 C99 H99 107.6 . . ? C101 C99 H99 107.7 . . ? C99 C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C99 C101 H10F 109.5 . . ? C99 C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? C99 C101 H10H 109.5 . . ? H10F C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? C107 C102 C103 118.0(3) . . ? C107 C102 Si4 115.1(2) . . ? C103 C102 Si4 126.8(3) . . ? C104 C103 C102 118.7(3) . . ? C104 C103 C108 117.3(3) . . ? C102 C103 C108 124.0(3) . . ? C105 C104 C103 123.1(3) . . ? C105 C104 H104 118.5 . . ? C103 C104 H104 118.5 . . ? C106 C105 C104 117.6(3) . . ? C106 C105 C111 121.6(4) . . ? C104 C105 C111 120.7(4) . . ? C105 C106 C107 122.5(4) . . ? C105 C106 H106 118.7 . . ? C107 C106 H106 118.7 . . ? C106 C107 C102 119.8(3) . . ? C106 C107 C114 116.6(3) . . ? C102 C107 C114 123.6(3) . . ? C103 C108 C110 113.0(3) . . ? C103 C108 C109 111.8(3) . . ? C110 C108 C109 107.1(3) . . ? C103 C108 H108 108.3 . . ? C110 C108 H108 108.3 . . ? C109 C108 H108 108.3 . . ? C108 C109 H10I 109.5 . . ? C108 C109 H10J 109.5 . . ? H10I C109 H10J 109.5 . . ? C108 C109 H10K 109.5 . . ? H10I C109 H10K 109.5 . . ? H10J C109 H10K 109.5 . . ? C108 C110 H11G 109.5 . . ? C108 C110 H11H 109.5 . . ? H11G C110 H11H 109.5 . . ? C108 C110 H11I 109.5 . . ? H11G C110 H11I 109.5 . . ? H11H C110 H11I 109.5 . . ? C112 C111 C113 112.6(4) . . ? C112 C111 C105 113.3(4) . . ? C113 C111 C105 110.1(4) . . ? C112 C111 H111 106.8 . . ? C113 C111 H111 106.8 . . ? C105 C111 H111 106.8 . . ? C111 C112 H11J 109.5 . . ? C111 C112 H11K 109.5 . . ? H11J C112 H11K 109.5 . . ? C111 C112 H11L 109.5 . . ? H11J C112 H11L 109.5 . . ? H11K C112 H11L 109.5 . . ? C111 C113 H11M 109.5 . . ? C111 C113 H11N 109.5 . . ? H11M C113 H11N 109.5 . . ? C111 C113 H11O 109.5 . . ? H11M C113 H11O 109.5 . . ? H11N C113 H11O 109.5 . . ? C115 C114 C107 112.0(3) . . ? C115 C114 C116 110.4(3) . . ? C107 C114 C116 111.4(3) . . ? C115 C114 H114 107.6 . . ? C107 C114 H114 107.6 . . ? C116 C114 H114 107.6 . . ? C114 C115 H11P 109.5 . . ? C114 C115 H11Q 109.5 . . ? H11P C115 H11Q 109.5 . . ? C114 C115 H11R 109.5 . . ? H11P C115 H11R 109.5 . . ? H11Q C115 H11R 109.5 . . ? C114 C116 H11S 109.5 . . ? C114 C116 H11T 109.5 . . ? H11S C116 H11T 109.5 . . ? C114 C116 H11U 109.5 . . ? H11S C116 H11U 109.5 . . ? H11T C116 H11U 109.5 . . ? O5 C117 Fe2 178.4(4) . . ? O6 C118 Fe2 177.7(4) . . ? O7 C119 Fe2 177.2(4) . . ? O8 C120 Fe2 179.5(4) . . ? C1A2 C1A1 H1A1 109.5 . . ? C1A2 C1A1 H1A2 109.6 . . ? H1A1 C1A1 H1A2 109.5 . . ? C1A2 C1A1 H1A3 109.4 . . ? H1A1 C1A1 H1A3 109.5 . . ? H1A2 C1A1 H1A3 109.5 . . ? C123 C1A2 C1A1 119.1(10) . . ? C123 C1A2 H1A4 107.7 . . ? C1A1 C1A2 H1A4 107.6 . . ? C123 C1A2 H1A5 107.5 . . ? C1A1 C1A2 H1A5 107.4 . . ? H1A4 C1A2 H1A5 107.0 . . ? C1B2 C1B1 H1B1 109.7 . . ? C1B2 C1B1 H1B2 109.7 . . ? H1B1 C1B1 H1B2 109.5 . . ? C1B2 C1B1 H1B3 109.1 . . ? H1B1 C1B1 H1B3 109.5 . . ? H1B2 C1B1 H1B3 109.5 . . ? C1B1 C1B2 C123 115.7(11) . . ? C1B1 C1B2 H1B4 108.0 . . ? C123 C1B2 H1B4 108.1 . . ? C1B1 C1B2 H1B5 108.7 . . ? C123 C1B2 H1B5 108.7 . . ? H1B4 C1B2 H1B5 107.4 . . ? C1A2 C123 C124 114.8(10) . . ? C1A2 C123 C1B2 32.3(11) . . ? C124 C123 C1B2 110.7(10) . . ? C1A2 C123 H12G 108.4 . . ? C124 C123 H12G 108.5 . . ? C1B2 C123 H12G 80.5 . . ? C1A2 C123 H12H 108.7 . . ? C124 C123 H12H 108.7 . . ? C1B2 C123 H12H 134.5 . . ? H12G C123 H12H 107.5 . . ? C1A2 C123 H12I 78.6 . . ? C124 C123 H12I 109.6 . . ? C1B2 C123 H12I 109.6 . . ? H12G C123 H12I 133.2 . . ? H12H C123 H12I 33.6 . . ? C1A2 C123 H12J 129.5 . . ? C124 C123 H12J 109.5 . . ? C1B2 C123 H12J 109.2 . . ? H12G C123 H12J 32.0 . . ? H12H C123 H12J 77.3 . . ? H12I C123 H12J 108.1 . . ? C123 C124 C125 114.6(10) . . ? C123 C124 H1AA 108.6 . . ? C125 C124 H1AA 108.5 . . ? C123 C124 H1BA 108.7 . . ? C125 C124 H1BA 108.6 . . ? H1AA C124 H1BA 107.6 . . ? C124 C125 H1F5 109.6 . . ? C124 C125 H1G5 109.4 . . ? H1F5 C125 H1G5 109.5 . . ? C124 C125 H1H5 109.5 . . ? H1F5 C125 H1H5 109.5 . . ? H1G5 C125 H1H5 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.142 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 953522'