# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_page_first ? _journal_page_last ? _journal_volume ? _journal_year ? #TrackingRef '4.cif' _publ_contact_author 'Prof. Dr. H. W. Roesky' _publ_contact_author_email hroesky@gwdg.de _publ_contact_author_name 'Prof. Dr. H. W. Roesky' loop_ _publ_author_name 'S. P. Sarish' 'S. S. Sen' 'I. Objartel' 'H. W. Roesky' 'D. Stalke' data_sad_p21n _database_code_depnum_ccdc_archive 'CCDC 819683' _ccdc_journal_depnumber ? _ccdc_compound_id 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H63 Cl Ge N4 Si' _chemical_formula_weight 784.11 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1815(10) _cell_length_b 22.4798(17) _cell_length_c 15.2220(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.3880(10) _cell_angle_gamma 90.00 _cell_volume 4327.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 9154 _cell_measurement_theta_min 2.4095 _cell_measurement_theta_max 27.241 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOTEC Mo Micro Source' _diffrn_radiation_monochromator 'INCOATEC quazar mirror optics' _diffrn_measurement_device_type 'Bruker Smart Apex II with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 96322 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.73 _reflns_number_total 9189 _reflns_number_gt 7576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 v2010.7-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL Version 2008/4' _computing_structure_refinement 'SHELXL in SHELXTL Version 2008/4' _computing_molecular_graphics 'XSHELL vers. 4.01' _computing_publication_material 'XSHELL vers. 4.01' _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^)+(0.0236P)^2^+3.5038P] 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 9189 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.444680(15) 0.170708(8) 0.394665(13) 0.01425(5) Uani 1 1 d . . . Cl1 Cl 0.40184(4) 0.08327(2) 0.30961(3) 0.02227(10) Uani 1 1 d . . . Si1 Si 0.33955(4) 0.14923(2) 0.70837(3) 0.01742(11) Uani 1 1 d . . . N1 N 0.38343(12) 0.09626(7) 0.80568(10) 0.0168(3) Uani 1 1 d . . . N2 N 0.22351(12) 0.12208(7) 0.74599(10) 0.0190(3) Uani 1 1 d . . . N3 N 0.36040(11) 0.14833(6) 0.47885(10) 0.0134(3) Uani 1 1 d . . . N4 N 0.57216(11) 0.14029(6) 0.48167(10) 0.0137(3) Uani 1 1 d . . . C1 C 0.28665(15) 0.09288(8) 0.81729(12) 0.0168(4) Uani 1 1 d . . . C2 C 0.25521(15) 0.06534(8) 0.89515(12) 0.0191(4) Uani 1 1 d . . . C3 C 0.20455(18) 0.01078(9) 0.88421(15) 0.0307(5) Uani 1 1 d . . . H3 H 0.1914 -0.0097 0.8276 0.037 Uiso 1 1 calc R . . C4 C 0.1729(2) -0.01405(10) 0.95575(18) 0.0413(6) Uani 1 1 d . . . H4 H 0.1379 -0.0514 0.9478 0.050 Uiso 1 1 calc R . . C5 C 0.1922(2) 0.01543(11) 1.03858(16) 0.0377(6) Uani 1 1 d . . . H5 H 0.1704 -0.0017 1.0874 0.045 Uiso 1 1 calc R . . C6 C 0.24306(18) 0.06977(10) 1.05010(14) 0.0327(5) Uani 1 1 d . . . H6 H 0.2567 0.0900 1.1070 0.039 Uiso 1 1 calc R . . C7 C 0.27428(17) 0.09479(9) 0.97853(13) 0.0257(4) Uani 1 1 d . . . H7 H 0.3089 0.1323 0.9866 0.031 Uiso 1 1 calc R . . C8 C 0.48406(15) 0.06718(8) 0.85404(13) 0.0194(4) Uani 1 1 d . . . C9 C 0.56685(15) 0.09116(9) 0.81033(13) 0.0228(4) Uani 1 1 d . . . H9A H 0.5462 0.0812 0.7450 0.034 Uiso 1 1 calc R . . H9B H 0.6357 0.0732 0.8403 0.034 Uiso 1 1 calc R . . H9C H 0.5718 0.1345 0.8177 0.034 Uiso 1 1 calc R . . C10 C 0.51737(17) 0.08130(11) 0.95594(13) 0.0296(5) Uani 1 1 d . . . H10A H 0.5168 0.1245 0.9646 0.044 Uiso 1 1 calc R . . H10B H 0.5888 0.0659 0.9838 0.044 Uiso 1 1 calc R . . H10C H 0.4679 0.0626 0.9850 0.044 Uiso 1 1 calc R . . C11 C 0.47262(17) -0.00006(9) 0.83777(15) 0.0293(5) Uani 1 1 d . . . H11A H 0.4183 -0.0155 0.8643 0.044 Uiso 1 1 calc R . . H11B H 0.5403 -0.0196 0.8668 0.044 Uiso 1 1 calc R . . H11C H 0.4520 -0.0081 0.7718 0.044 Uiso 1 1 calc R . . C12 C 0.11317(15) 0.14338(9) 0.72987(13) 0.0235(4) Uani 1 1 d . . . C13 C 0.0940(2) 0.18594(12) 0.64800(16) 0.0446(7) Uani 1 1 d . . . H13A H 0.1454 0.2185 0.6629 0.067 Uiso 1 1 calc R . . H13B H 0.0223 0.2022 0.6343 0.067 Uiso 1 1 calc R . . H13C H 0.1021 0.1643 0.5945 0.067 Uiso 1 1 calc R . . C14 C 0.03711(19) 0.09169(12) 0.7060(2) 0.0543(8) Uani 1 1 d . . . H14A H 0.0537 0.0675 0.6583 0.081 Uiso 1 1 calc R . . H14B H -0.0354 0.1068 0.6836 0.081 Uiso 1 1 calc R . . H14C H 0.0437 0.0673 0.7606 0.081 Uiso 1 1 calc R . . C15 C 0.09764(18) 0.17823(11) 0.81084(16) 0.0362(5) Uani 1 1 d . . . H15A H 0.1024 0.1511 0.8623 0.054 Uiso 1 1 calc R . . H15B H 0.0279 0.1972 0.7933 0.054 Uiso 1 1 calc R . . H15C H 0.1526 0.2088 0.8291 0.054 Uiso 1 1 calc R . . C16 C 0.31872(15) 0.09388(8) 0.60361(12) 0.0161(4) Uani 1 1 d . . . H16A H 0.2475(17) 0.0996(9) 0.5725(13) 0.017(5) Uiso 1 1 d . . . H16B H 0.3282(15) 0.0539(9) 0.6259(13) 0.015(5) Uiso 1 1 d . . . C17 C 0.38619(14) 0.10620(8) 0.54269(11) 0.0132(3) Uani 1 1 d . . . C18 C 0.48258(14) 0.07437(8) 0.55831(12) 0.0141(4) Uani 1 1 d . . . H18 H 0.4895(15) 0.0418(9) 0.5951(13) 0.012(5) Uiso 1 1 d . . . C19 C 0.57182(14) 0.09210(8) 0.53494(12) 0.0146(4) Uani 1 1 d . . . C20 C 0.67250(15) 0.05707(9) 0.57033(14) 0.0217(4) Uani 1 1 d . . . H20A H 0.6911 0.0383 0.5189 0.033 Uiso 1 1 calc R . . H20B H 0.6623 0.0263 0.6127 0.033 Uiso 1 1 calc R . . H20C H 0.7296 0.0838 0.6025 0.033 Uiso 1 1 calc R . . C21 C 0.25976(14) 0.17913(8) 0.45727(12) 0.0149(4) Uani 1 1 d . . . C22 C 0.25793(14) 0.24023(8) 0.47754(12) 0.0170(4) Uani 1 1 d . . . C23 C 0.16171(15) 0.27027(9) 0.44702(13) 0.0214(4) Uani 1 1 d . . . H23 H 0.1587 0.3113 0.4607 0.026 Uiso 1 1 calc R . . C24 C 0.07072(15) 0.24171(9) 0.39729(13) 0.0222(4) Uani 1 1 d . . . H24 H 0.0065 0.2633 0.3758 0.027 Uiso 1 1 calc R . . C25 C 0.07373(14) 0.18162(9) 0.37904(13) 0.0201(4) Uani 1 1 d . . . H25 H 0.0106 0.1621 0.3459 0.024 Uiso 1 1 calc R . . C26 C 0.16700(14) 0.14883(8) 0.40804(12) 0.0169(4) Uani 1 1 d . . . C27 C 0.35497(15) 0.27626(8) 0.52808(13) 0.0191(4) Uani 1 1 d . . . H27 H 0.4157 0.2482 0.5499 0.023 Uiso 1 1 calc R . . C28 C 0.38431(16) 0.32177(9) 0.46397(13) 0.0239(4) Uani 1 1 d . . . H28A H 0.4002 0.3009 0.4129 0.036 Uiso 1 1 calc R . . H28B H 0.4466 0.3444 0.4980 0.036 Uiso 1 1 calc R . . H28C H 0.3249 0.3490 0.4402 0.036 Uiso 1 1 calc R . . C29 C 0.33837(17) 0.30851(9) 0.61184(14) 0.0258(4) Uani 1 1 d . . . H29A H 0.2794 0.3366 0.5919 0.039 Uiso 1 1 calc R . . H29B H 0.4029 0.3302 0.6433 0.039 Uiso 1 1 calc R . . H29C H 0.3222 0.2793 0.6538 0.039 Uiso 1 1 calc R . . C30 C 0.16343(14) 0.08276(8) 0.38345(13) 0.0189(4) Uani 1 1 d . . . H30 H 0.2364 0.0662 0.4076 0.023 Uiso 1 1 calc R . . C31 C 0.08973(16) 0.04777(9) 0.42689(14) 0.0261(4) Uani 1 1 d . . . H31A H 0.1109 0.0545 0.4932 0.039 Uiso 1 1 calc R . . H31B H 0.0945 0.0052 0.4145 0.039 Uiso 1 1 calc R . . H31C H 0.0167 0.0613 0.4007 0.039 Uiso 1 1 calc R . . C32 C 0.12765(16) 0.07333(9) 0.27938(13) 0.0258(4) Uani 1 1 d . . . H32A H 0.1302 0.0308 0.2658 0.039 Uiso 1 1 calc R . . H32B H 0.1748 0.0952 0.2513 0.039 Uiso 1 1 calc R . . H32C H 0.0552 0.0880 0.2546 0.039 Uiso 1 1 calc R . . C33 C 0.66970(13) 0.17099(8) 0.48496(12) 0.0158(4) Uani 1 1 d . . . C34 C 0.71121(14) 0.21097(8) 0.55719(12) 0.0174(4) Uani 1 1 d . . . C35 C 0.80118(15) 0.24347(9) 0.55664(13) 0.0212(4) Uani 1 1 d . . . H35 H 0.8310 0.2702 0.6054 0.025 Uiso 1 1 calc R . . C36 C 0.84777(15) 0.23740(9) 0.48634(14) 0.0232(4) Uani 1 1 d . . . H36 H 0.9081 0.2605 0.4863 0.028 Uiso 1 1 calc R . . C37 C 0.80624(15) 0.19769(9) 0.41629(14) 0.0225(4) Uani 1 1 d . . . H37 H 0.8385 0.1938 0.3681 0.027 Uiso 1 1 calc R . . C38 C 0.71772(14) 0.16304(8) 0.41462(13) 0.0183(4) Uani 1 1 d . . . C39 C 0.66383(15) 0.21945(9) 0.63652(13) 0.0216(4) Uani 1 1 d . . . H39 H 0.5948 0.1978 0.6219 0.026 Uiso 1 1 calc R . . C40 C 0.64304(18) 0.28510(10) 0.65161(15) 0.0313(5) Uani 1 1 d . . . H40A H 0.7106 0.3060 0.6749 0.047 Uiso 1 1 calc R . . H40B H 0.6022 0.2884 0.6961 0.047 Uiso 1 1 calc R . . H40C H 0.6030 0.3030 0.5934 0.047 Uiso 1 1 calc R . . C41 C 0.73637(18) 0.19362(11) 0.72528(14) 0.0321(5) Uani 1 1 d . . . H41A H 0.7439 0.1507 0.7181 0.048 Uiso 1 1 calc R . . H41B H 0.7056 0.2011 0.7758 0.048 Uiso 1 1 calc R . . H41C H 0.8060 0.2126 0.7387 0.048 Uiso 1 1 calc R . . C42 C 0.67844(15) 0.11777(8) 0.33854(13) 0.0198(4) Uani 1 1 d . . . H42 H 0.6208 0.0941 0.3528 0.024 Uiso 1 1 calc R . . C43 C 0.76707(16) 0.07453(10) 0.33417(15) 0.0290(5) Uani 1 1 d . . . H43A H 0.8196 0.0955 0.3112 0.044 Uiso 1 1 calc R . . H43B H 0.7371 0.0415 0.2929 0.044 Uiso 1 1 calc R . . H43C H 0.8010 0.0589 0.3956 0.044 Uiso 1 1 calc R . . C44 C 0.63179(17) 0.14849(9) 0.24603(13) 0.0264(4) Uani 1 1 d . . . H44A H 0.5729 0.1741 0.2495 0.040 Uiso 1 1 calc R . . H44B H 0.6061 0.1184 0.1984 0.040 Uiso 1 1 calc R . . H44C H 0.6865 0.1726 0.2310 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01213(9) 0.01646(10) 0.01516(9) 0.00346(8) 0.00546(7) 0.00150(8) Cl1 0.0188(2) 0.0296(3) 0.0194(2) -0.00716(19) 0.00712(18) -0.00328(19) Si1 0.0200(3) 0.0166(2) 0.0164(2) 0.0024(2) 0.0064(2) 0.0017(2) N1 0.0166(8) 0.0181(8) 0.0153(7) 0.0026(6) 0.0039(6) 0.0006(6) N2 0.0171(8) 0.0233(8) 0.0180(8) 0.0014(6) 0.0071(6) 0.0047(7) N3 0.0105(7) 0.0144(7) 0.0160(7) 0.0002(6) 0.0047(6) 0.0009(6) N4 0.0111(7) 0.0150(7) 0.0160(7) -0.0003(6) 0.0056(6) 0.0005(6) C1 0.0225(10) 0.0142(9) 0.0143(8) -0.0025(7) 0.0062(7) 0.0001(7) C2 0.0204(10) 0.0204(10) 0.0186(9) 0.0028(7) 0.0090(8) 0.0034(8) C3 0.0425(13) 0.0241(11) 0.0334(12) -0.0047(9) 0.0236(10) -0.0056(10) C4 0.0552(16) 0.0248(12) 0.0567(16) 0.0050(11) 0.0366(13) -0.0048(11) C5 0.0480(15) 0.0405(14) 0.0351(13) 0.0159(11) 0.0291(11) 0.0105(11) C6 0.0403(13) 0.0410(13) 0.0202(10) 0.0035(9) 0.0140(10) 0.0098(11) C7 0.0313(12) 0.0266(11) 0.0213(10) -0.0002(8) 0.0111(9) 0.0026(9) C8 0.0162(9) 0.0221(10) 0.0185(9) 0.0039(7) 0.0027(7) 0.0008(8) C9 0.0171(10) 0.0314(11) 0.0195(9) 0.0011(8) 0.0046(8) -0.0005(8) C10 0.0225(11) 0.0466(14) 0.0184(10) 0.0029(9) 0.0037(8) -0.0054(10) C11 0.0272(11) 0.0232(11) 0.0390(12) 0.0066(9) 0.0118(10) 0.0047(9) C12 0.0156(10) 0.0325(11) 0.0227(10) -0.0010(8) 0.0060(8) 0.0060(8) C13 0.0347(13) 0.0679(18) 0.0336(13) 0.0176(12) 0.0136(11) 0.0285(13) C14 0.0233(13) 0.0459(16) 0.086(2) -0.0156(15) 0.0023(13) -0.0038(11) C15 0.0294(12) 0.0437(14) 0.0374(13) -0.0059(11) 0.0126(10) 0.0142(10) C16 0.0141(9) 0.0193(10) 0.0152(9) 0.0023(7) 0.0045(7) -0.0009(7) C17 0.0139(9) 0.0129(8) 0.0123(8) -0.0023(6) 0.0026(7) -0.0025(7) C18 0.0159(9) 0.0127(9) 0.0135(8) 0.0023(7) 0.0036(7) 0.0006(7) C19 0.0146(9) 0.0143(9) 0.0142(8) -0.0022(7) 0.0030(7) 0.0014(7) C20 0.0170(10) 0.0191(10) 0.0280(10) 0.0034(8) 0.0048(8) 0.0041(8) C21 0.0123(8) 0.0205(9) 0.0134(8) 0.0036(7) 0.0063(7) 0.0031(7) C22 0.0178(9) 0.0182(9) 0.0174(9) 0.0029(7) 0.0089(7) 0.0021(7) C23 0.0214(10) 0.0200(10) 0.0261(10) 0.0052(8) 0.0121(8) 0.0059(8) C24 0.0148(9) 0.0278(11) 0.0262(10) 0.0099(8) 0.0093(8) 0.0086(8) C25 0.0124(9) 0.0281(11) 0.0199(9) 0.0043(8) 0.0048(7) -0.0007(8) C26 0.0156(9) 0.0210(9) 0.0157(9) 0.0035(7) 0.0072(7) 0.0017(7) C27 0.0202(10) 0.0166(9) 0.0214(9) 0.0002(7) 0.0073(8) 0.0021(7) C28 0.0256(11) 0.0221(10) 0.0254(10) -0.0013(8) 0.0094(8) -0.0031(8) C29 0.0330(12) 0.0213(10) 0.0243(10) -0.0013(8) 0.0103(9) 0.0018(9) C30 0.0139(9) 0.0203(10) 0.0216(9) 0.0013(8) 0.0033(7) -0.0005(7) C31 0.0200(10) 0.0277(11) 0.0286(11) 0.0031(9) 0.0035(8) -0.0063(8) C32 0.0237(11) 0.0266(11) 0.0247(10) -0.0033(8) 0.0029(8) -0.0022(8) C33 0.0110(8) 0.0159(9) 0.0206(9) 0.0026(7) 0.0049(7) 0.0014(7) C34 0.0124(9) 0.0195(9) 0.0197(9) 0.0006(7) 0.0038(7) 0.0014(7) C35 0.0162(9) 0.0221(10) 0.0240(10) -0.0033(8) 0.0038(8) -0.0032(8) C36 0.0156(9) 0.0253(10) 0.0307(11) 0.0000(8) 0.0098(8) -0.0055(8) C37 0.0178(10) 0.0262(10) 0.0267(10) -0.0001(8) 0.0117(8) -0.0012(8) C38 0.0155(9) 0.0195(9) 0.0215(9) 0.0014(7) 0.0078(7) 0.0019(7) C39 0.0178(10) 0.0268(10) 0.0217(10) -0.0069(8) 0.0081(8) -0.0069(8) C40 0.0308(12) 0.0322(12) 0.0343(12) -0.0084(9) 0.0150(10) 0.0012(10) C41 0.0332(12) 0.0423(13) 0.0224(11) 0.0020(9) 0.0107(9) -0.0040(10) C42 0.0170(9) 0.0221(10) 0.0234(10) -0.0037(8) 0.0108(8) -0.0016(8) C43 0.0229(11) 0.0306(11) 0.0371(12) -0.0093(9) 0.0141(9) 0.0009(9) C44 0.0305(12) 0.0291(11) 0.0219(10) -0.0027(8) 0.0113(9) -0.0053(9) _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 N4 1.9467(14) . ? Ge1 N3 1.9832(14) . ? Ge1 Cl1 2.3337(5) . ? Si1 N1 1.8609(15) . ? Si1 N2 1.8800(17) . ? Si1 C16 1.9798(19) . ? N1 C1 1.338(2) . ? N1 C8 1.476(2) . ? N2 C1 1.339(2) . ? N2 C12 1.484(2) . ? N3 C17 1.330(2) . ? N3 C21 1.450(2) . ? N4 C19 1.354(2) . ? N4 C33 1.448(2) . ? C1 C2 1.496(2) . ? C2 C3 1.384(3) . ? C2 C7 1.390(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.522(3) . ? C8 C9 1.528(3) . ? C8 C11 1.532(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.511(3) . ? C12 C15 1.522(3) . ? C12 C13 1.534(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 1.481(2) . ? C16 H16A 0.93(2) . ? C16 H16B 0.96(2) . ? C17 C18 1.419(2) . ? C18 C19 1.380(2) . ? C18 H18 0.910(19) . ? C19 C20 1.506(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.409(3) . ? C21 C26 1.416(3) . ? C22 C23 1.396(3) . ? C22 C27 1.526(3) . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.382(3) . ? C24 H24 0.9500 . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C26 C30 1.529(3) . ? C27 C29 1.535(3) . ? C27 C28 1.537(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.535(3) . ? C30 C31 1.537(3) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.401(2) . ? C33 C34 1.406(3) . ? C34 C35 1.395(3) . ? C34 C39 1.520(3) . ? C35 C36 1.383(3) . ? C35 H35 0.9500 . ? C36 C37 1.380(3) . ? C36 H36 0.9500 . ? C37 C38 1.397(3) . ? C37 H37 0.9500 . ? C38 C42 1.519(3) . ? C39 C40 1.530(3) . ? C39 C41 1.532(3) . ? 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 C44 1.533(3) . ? C42 C43 1.536(3) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 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 N4 Ge1 N3 90.27(6) . . ? N4 Ge1 Cl1 96.25(4) . . ? N3 Ge1 Cl1 93.03(4) . . ? N1 Si1 N2 69.31(7) . . ? N1 Si1 C16 100.39(8) . . ? N2 Si1 C16 95.83(8) . . ? C1 N1 C8 131.68(15) . . ? C1 N1 Si1 92.73(11) . . ? C8 N1 Si1 135.59(12) . . ? C1 N2 C12 130.42(16) . . ? C1 N2 Si1 91.88(12) . . ? C12 N2 Si1 133.50(13) . . ? C17 N3 C21 122.31(14) . . ? C17 N3 Ge1 125.32(12) . . ? C21 N3 Ge1 112.09(11) . . ? C19 N4 C33 120.91(14) . . ? C19 N4 Ge1 122.71(12) . . ? C33 N4 Ge1 116.35(11) . . ? N1 C1 N2 105.25(15) . . ? N1 C1 C2 127.99(16) . . ? N2 C1 C2 126.69(17) . . ? C3 C2 C7 119.25(18) . . ? C3 C2 C1 120.25(17) . . ? C7 C2 C1 120.48(17) . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.8(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.4(2) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N1 C8 C10 112.10(16) . . ? N1 C8 C9 106.16(15) . . ? C10 C8 C9 109.53(16) . . ? N1 C8 C11 108.83(15) . . ? C10 C8 C11 110.95(17) . . ? C9 C8 C11 109.12(16) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C14 110.16(18) . . ? N2 C12 C15 112.42(16) . . ? C14 C12 C15 111.0(2) . . ? N2 C12 C13 105.34(16) . . ? C14 C12 C13 109.8(2) . . ? C15 C12 C13 107.92(19) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 Si1 114.55(12) . . ? C17 C16 H16A 110.6(12) . . ? Si1 C16 H16A 102.3(12) . . ? C17 C16 H16B 110.9(12) . . ? Si1 C16 H16B 109.3(11) . . ? H16A C16 H16B 108.8(17) . . ? N3 C17 C18 120.91(16) . . ? N3 C17 C16 121.04(16) . . ? C18 C17 C16 117.93(16) . . ? C19 C18 C17 126.82(16) . . ? C19 C18 H18 116.5(12) . . ? C17 C18 H18 116.0(12) . . ? N4 C19 C18 122.17(16) . . ? N4 C19 C20 118.76(16) . . ? C18 C19 C20 119.07(16) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 121.29(16) . . ? C22 C21 N3 119.14(16) . . ? C26 C21 N3 119.25(16) . . ? C23 C22 C21 117.95(17) . . ? C23 C22 C27 117.69(16) . . ? C21 C22 C27 124.33(16) . . ? C24 C23 C22 121.60(18) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C23 119.63(17) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 121.74(18) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 117.77(17) . . ? C25 C26 C30 118.21(17) . . ? C21 C26 C30 124.01(16) . . ? C22 C27 C29 111.95(16) . . ? C22 C27 C28 111.01(15) . . ? C29 C27 C28 109.47(16) . . ? C22 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 C32 111.48(15) . . ? C26 C30 C31 111.80(16) . . ? C32 C30 C31 109.02(16) . . ? C26 C30 H30 108.1 . . ? C32 C30 H30 108.1 . . ? C31 C30 H30 108.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 121.28(16) . . ? C38 C33 N4 120.09(16) . . ? C34 C33 N4 118.53(15) . . ? C35 C34 C33 118.29(17) . . ? C35 C34 C39 118.67(17) . . ? C33 C34 C39 123.02(16) . . ? C36 C35 C34 121.13(18) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C37 C36 C35 119.73(18) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 121.46(18) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C37 C38 C33 118.05(17) . . ? C37 C38 C42 119.39(16) . . ? C33 C38 C42 122.55(16) . . ? C34 C39 C40 111.79(16) . . ? C34 C39 C41 111.04(16) . . ? C40 C39 C41 109.07(17) . . ? C34 C39 H39 108.3 . . ? C40 C39 H39 108.3 . . ? C41 C39 H39 108.3 . . ? 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 . . ? C38 C42 C44 111.14(16) . . ? C38 C42 C43 110.94(16) . . ? C44 C42 C43 110.99(16) . . ? C38 C42 H42 107.9 . . ? C44 C42 H42 107.9 . . ? C43 C42 H42 107.9 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Si1 N1 C1 -5.92(10) . . . . ? C16 Si1 N1 C1 -98.27(12) . . . . ? N2 Si1 N1 C8 173.62(19) . . . . ? C16 Si1 N1 C8 81.26(18) . . . . ? N1 Si1 N2 C1 5.92(10) . . . . ? C16 Si1 N2 C1 104.84(12) . . . . ? N1 Si1 N2 C12 163.67(19) . . . . ? C16 Si1 N2 C12 -97.40(18) . . . . ? N4 Ge1 N3 C17 -24.36(14) . . . . ? Cl1 Ge1 N3 C17 71.91(14) . . . . ? N4 Ge1 N3 C21 161.62(12) . . . . ? Cl1 Ge1 N3 C21 -102.11(11) . . . . ? N3 Ge1 N4 C19 34.95(14) . . . . ? Cl1 Ge1 N4 C19 -58.12(13) . . . . ? N3 Ge1 N4 C33 -146.89(12) . . . . ? Cl1 Ge1 N4 C33 120.04(12) . . . . ? C8 N1 C1 N2 -171.49(17) . . . . ? Si1 N1 C1 N2 8.07(14) . . . . ? C8 N1 C1 C2 11.3(3) . . . . ? Si1 N1 C1 C2 -169.09(17) . . . . ? C12 N2 C1 N1 -166.85(18) . . . . ? Si1 N2 C1 N1 -7.99(14) . . . . ? C12 N2 C1 C2 10.4(3) . . . . ? Si1 N2 C1 C2 169.23(17) . . . . ? N1 C1 C2 C3 -104.4(2) . . . . ? N2 C1 C2 C3 79.0(3) . . . . ? N1 C1 C2 C7 77.0(3) . . . . ? N2 C1 C2 C7 -99.5(2) . . . . ? C7 C2 C3 C4 0.2(3) . . . . ? C1 C2 C3 C4 -178.3(2) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C7 0.3(3) . . . . ? C5 C6 C7 C2 -0.4(3) . . . . ? C3 C2 C7 C6 0.1(3) . . . . ? C1 C2 C7 C6 178.62(19) . . . . ? C1 N1 C8 C10 -58.5(3) . . . . ? Si1 N1 C8 C10 122.10(17) . . . . ? C1 N1 C8 C9 -178.07(18) . . . . ? Si1 N1 C8 C9 2.5(2) . . . . ? C1 N1 C8 C11 64.6(2) . . . . ? Si1 N1 C8 C11 -114.78(18) . . . . ? C1 N2 C12 C14 -74.8(3) . . . . ? Si1 N2 C12 C14 134.95(19) . . . . ? C1 N2 C12 C15 49.6(3) . . . . ? Si1 N2 C12 C15 -100.6(2) . . . . ? C1 N2 C12 C13 166.8(2) . . . . ? Si1 N2 C12 C13 16.6(3) . . . . ? N1 Si1 C16 C17 -119.20(14) . . . . ? N2 Si1 C16 C17 170.82(13) . . . . ? C21 N3 C17 C18 176.12(16) . . . . ? Ge1 N3 C17 C18 2.7(2) . . . . ? C21 N3 C17 C16 -8.0(2) . . . . ? Ge1 N3 C17 C16 178.59(12) . . . . ? Si1 C16 C17 N3 -80.80(18) . . . . ? Si1 C16 C17 C18 95.23(17) . . . . ? N3 C17 C18 C19 21.1(3) . . . . ? C16 C17 C18 C19 -154.94(17) . . . . ? C33 N4 C19 C18 156.98(16) . . . . ? Ge1 N4 C19 C18 -24.9(2) . . . . ? C33 N4 C19 C20 -22.5(2) . . . . ? Ge1 N4 C19 C20 155.54(13) . . . . ? C17 C18 C19 N4 -9.2(3) . . . . ? C17 C18 C19 C20 170.31(17) . . . . ? C17 N3 C21 C22 113.14(19) . . . . ? Ge1 N3 C21 C22 -72.63(17) . . . . ? C17 N3 C21 C26 -73.3(2) . . . . ? Ge1 N3 C21 C26 100.98(16) . . . . ? C26 C21 C22 C23 -0.4(3) . . . . ? N3 C21 C22 C23 173.06(15) . . . . ? C26 C21 C22 C27 -178.38(16) . . . . ? N3 C21 C22 C27 -4.9(3) . . . . ? C21 C22 C23 C24 -0.9(3) . . . . ? C27 C22 C23 C24 177.22(17) . . . . ? C22 C23 C24 C25 1.7(3) . . . . ? C23 C24 C25 C26 -1.2(3) . . . . ? C24 C25 C26 C21 0.0(3) . . . . ? C24 C25 C26 C30 -179.01(17) . . . . ? C22 C21 C26 C25 0.9(3) . . . . ? N3 C21 C26 C25 -172.61(15) . . . . ? C22 C21 C26 C30 179.76(16) . . . . ? N3 C21 C26 C30 6.3(3) . . . . ? C23 C22 C27 C29 56.4(2) . . . . ? C21 C22 C27 C29 -125.66(19) . . . . ? C23 C22 C27 C28 -66.3(2) . . . . ? C21 C22 C27 C28 111.67(19) . . . . ? C25 C26 C30 C32 59.7(2) . . . . ? C21 C26 C30 C32 -119.19(19) . . . . ? C25 C26 C30 C31 -62.6(2) . . . . ? C21 C26 C30 C31 118.50(19) . . . . ? C19 N4 C33 C38 103.8(2) . . . . ? Ge1 N4 C33 C38 -74.41(19) . . . . ? C19 N4 C33 C34 -79.6(2) . . . . ? Ge1 N4 C33 C34 102.19(16) . . . . ? C38 C33 C34 C35 0.9(3) . . . . ? N4 C33 C34 C35 -175.67(16) . . . . ? C38 C33 C34 C39 -177.89(17) . . . . ? N4 C33 C34 C39 5.6(3) . . . . ? C33 C34 C35 C36 1.0(3) . . . . ? C39 C34 C35 C36 179.81(18) . . . . ? C34 C35 C36 C37 -1.4(3) . . . . ? C35 C36 C37 C38 -0.2(3) . . . . ? C36 C37 C38 C33 2.0(3) . . . . ? C36 C37 C38 C42 -176.93(18) . . . . ? C34 C33 C38 C37 -2.3(3) . . . . ? N4 C33 C38 C37 174.19(16) . . . . ? C34 C33 C38 C42 176.53(17) . . . . ? N4 C33 C38 C42 -7.0(3) . . . . ? C35 C34 C39 C40 52.7(2) . . . . ? C33 C34 C39 C40 -128.53(19) . . . . ? C35 C34 C39 C41 -69.4(2) . . . . ? C33 C34 C39 C41 109.4(2) . . . . ? C37 C38 C42 C44 -68.7(2) . . . . ? C33 C38 C42 C44 112.4(2) . . . . ? C37 C38 C42 C43 55.3(2) . . . . ? C33 C38 C42 C43 -123.55(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.571 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.054 # Attachment '5.cif' data_p21n_sad _database_code_depnum_ccdc_archive 'CCDC 819684' _ccdc_journal_depnumber ? _ccdc_compound_id 5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H63 Cl Ge2 N4' _chemical_formula_weight 828.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.207(2) _cell_length_b 22.515(3) _cell_length_c 15.273(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.601(2) _cell_angle_gamma 90.00 _cell_volume 4352.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 2.2825 _cell_measurement_theta_max 23.804 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.820074 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC Mo micro source' _diffrn_radiation_monochromator 'INCOATEC quazar mirror optics' _diffrn_measurement_device_type 'Bruker Smart Apex2 with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 90869 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7962 _reflns_number_gt 6580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL Version 2008/4' _computing_structure_refinement 'SHELXL in SHELXTL Version 2008/4' _computing_molecular_graphics 'XSHELL vers. 4.01' _computing_publication_material 'XSHELL vers. 4.01' _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^)+(0.0160P)^2^+5.9383P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7962 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.55678(2) 0.169567(11) 0.608366(17) 0.01491(7) Uani 1 1 d . . . Ge2 Ge 0.65835(2) 0.155005(12) 0.295410(18) 0.01969(7) Uani 1 1 d . . . Cl1 Cl 0.59709(5) 0.08144(3) 0.69154(4) 0.02252(14) Uani 1 1 d . . . N1 N 0.42893(15) 0.14047(9) 0.52023(13) 0.0139(4) Uani 1 1 d . . . N2 N 0.64112(15) 0.14776(9) 0.52477(13) 0.0136(4) Uani 1 1 d . . . N3 N 0.61593(16) 0.09867(9) 0.19105(14) 0.0183(5) Uani 1 1 d . . . N4 N 0.77865(16) 0.12387(10) 0.25223(14) 0.0212(5) Uani 1 1 d . . . C1 C 0.61498(19) 0.10556(10) 0.46067(15) 0.0141(5) Uani 1 1 d . . . C2 C 0.51778(18) 0.07450(10) 0.44365(16) 0.0146(5) Uani 1 1 d . . . H2 H 0.5136 0.0373 0.4135 0.018 Uiso 1 1 calc R . . C3 C 0.42860(19) 0.09274(10) 0.46637(16) 0.0150(5) Uani 1 1 d . . . C4 C 0.3278(2) 0.05819(11) 0.43042(18) 0.0217(6) Uani 1 1 d . . . H4A H 0.3094 0.0390 0.4814 0.033 Uiso 1 1 calc R . . H4B H 0.3376 0.0279 0.3875 0.033 Uiso 1 1 calc R . . H4C H 0.2709 0.0852 0.3989 0.033 Uiso 1 1 calc R . . C5 C 0.33166(18) 0.17113(11) 0.51654(16) 0.0153(5) Uani 1 1 d . . . C6 C 0.29166(19) 0.21207(11) 0.44574(17) 0.0176(5) Uani 1 1 d . . . C7 C 0.2017(2) 0.24431(11) 0.44564(18) 0.0216(6) Uani 1 1 d . . . H7 H 0.1728 0.2716 0.3975 0.026 Uiso 1 1 calc R . . C8 C 0.1538(2) 0.23735(12) 0.51432(18) 0.0240(6) Uani 1 1 d . . . H8 H 0.0935 0.2605 0.5141 0.029 Uiso 1 1 calc R . . C9 C 0.1934(2) 0.19686(12) 0.58322(18) 0.0236(6) Uani 1 1 d . . . H9 H 0.1598 0.1922 0.6300 0.028 Uiso 1 1 calc R . . C10 C 0.28225(19) 0.16261(11) 0.58544(16) 0.0178(5) Uani 1 1 d . . . C11 C 0.3409(2) 0.22171(12) 0.36800(17) 0.0221(6) Uani 1 1 d . . . H11 H 0.4104 0.2006 0.3837 0.027 Uiso 1 1 calc R . . C12 C 0.3606(2) 0.28745(13) 0.3540(2) 0.0334(7) Uani 1 1 d . . . H12A H 0.2928 0.3078 0.3296 0.050 Uiso 1 1 calc R . . H12B H 0.4027 0.2914 0.3109 0.050 Uiso 1 1 calc R . . H12C H 0.3989 0.3053 0.4127 0.050 Uiso 1 1 calc R . . C13 C 0.2705(2) 0.19556(14) 0.27855(19) 0.0332(7) Uani 1 1 d . . . H13A H 0.2642 0.1525 0.2853 0.050 Uiso 1 1 calc R . . H13B H 0.3021 0.2037 0.2290 0.050 Uiso 1 1 calc R . . H13C H 0.2003 0.2138 0.2642 0.050 Uiso 1 1 calc R . . C14 C 0.3203(2) 0.11662(11) 0.66048(17) 0.0201(6) Uani 1 1 d . . . H14 H 0.3781 0.0932 0.6465 0.024 Uiso 1 1 calc R . . C15 C 0.3659(2) 0.14634(13) 0.75377(18) 0.0286(6) Uani 1 1 d . . . H15A H 0.4259 0.1715 0.7520 0.043 Uiso 1 1 calc R . . H15B H 0.3897 0.1158 0.8008 0.043 Uiso 1 1 calc R . . H15C H 0.3114 0.1708 0.7681 0.043 Uiso 1 1 calc R . . C16 C 0.2311(2) 0.07327(12) 0.6627(2) 0.0287(7) Uani 1 1 d . . . H16A H 0.1773 0.0942 0.6837 0.043 Uiso 1 1 calc R . . H16B H 0.2601 0.0405 0.7047 0.043 Uiso 1 1 calc R . . H16C H 0.1991 0.0574 0.6013 0.043 Uiso 1 1 calc R . . C17 C 0.74201(19) 0.17773(11) 0.54668(16) 0.0155(5) Uani 1 1 d . . . C18 C 0.74528(19) 0.23869(11) 0.52629(16) 0.0175(5) Uani 1 1 d . . . C19 C 0.8423(2) 0.26795(12) 0.55674(18) 0.0222(6) Uani 1 1 d . . . H19 H 0.8460 0.3090 0.5436 0.027 Uiso 1 1 calc R . . C20 C 0.9328(2) 0.23881(12) 0.60532(18) 0.0232(6) Uani 1 1 d . . . H20 H 0.9977 0.2597 0.6259 0.028 Uiso 1 1 calc R . . C21 C 0.9283(2) 0.17907(12) 0.62388(17) 0.0213(6) Uani 1 1 d . . . H21 H 0.9910 0.1592 0.6570 0.026 Uiso 1 1 calc R . . C22 C 0.83455(19) 0.14703(11) 0.59543(16) 0.0167(5) Uani 1 1 d . . . C23 C 0.6488(2) 0.27531(11) 0.47649(17) 0.0196(5) Uani 1 1 d . . . H23 H 0.5877 0.2477 0.4534 0.024 Uiso 1 1 calc R . . C24 C 0.6665(2) 0.30896(12) 0.39433(18) 0.0266(6) Uani 1 1 d . . . H24A H 0.7253 0.3369 0.4158 0.040 Uiso 1 1 calc R . . H24B H 0.6023 0.3309 0.3630 0.040 Uiso 1 1 calc R . . H24C H 0.6833 0.2805 0.3519 0.040 Uiso 1 1 calc R . . C25 C 0.6202(2) 0.32028(12) 0.54147(18) 0.0248(6) Uani 1 1 d . . . H25A H 0.6048 0.2990 0.5922 0.037 Uiso 1 1 calc R . . H25B H 0.5579 0.3431 0.5081 0.037 Uiso 1 1 calc R . . H25C H 0.6797 0.3474 0.5655 0.037 Uiso 1 1 calc R . . C26 C 0.83682(19) 0.08130(11) 0.61985(17) 0.0183(5) Uani 1 1 d . . . H26 H 0.7636 0.0652 0.5952 0.022 Uiso 1 1 calc R . . C27 C 0.9101(2) 0.04569(12) 0.57700(18) 0.0250(6) Uani 1 1 d . . . H27A H 0.8896 0.0526 0.5109 0.038 Uiso 1 1 calc R . . H27B H 0.9040 0.0033 0.5889 0.038 Uiso 1 1 calc R . . H27C H 0.9833 0.0585 0.6039 0.038 Uiso 1 1 calc R . . C28 C 0.8717(2) 0.07162(12) 0.72358(18) 0.0268(6) Uani 1 1 d . . . H28A H 0.9446 0.0855 0.7489 0.040 Uiso 1 1 calc R . . H28B H 0.8677 0.0292 0.7368 0.040 Uiso 1 1 calc R . . H28C H 0.8252 0.0940 0.7513 0.040 Uiso 1 1 calc R . . C29 C 0.68218(19) 0.09310(11) 0.40086(16) 0.0164(5) Uani 1 1 d . . . H29A H 0.6662 0.0528 0.3745 0.020 Uiso 1 1 calc R . . H29B H 0.7573 0.0939 0.4375 0.020 Uiso 1 1 calc R . . C30 C 0.7133(2) 0.09500(11) 0.18201(16) 0.0180(5) Uani 1 1 d . . . C31 C 0.7444(2) 0.06568(11) 0.10553(17) 0.0193(5) Uani 1 1 d . . . C32 C 0.7963(2) 0.01141(12) 0.1190(2) 0.0311(7) Uani 1 1 d . . . H32 H 0.8103 -0.0080 0.1765 0.037 Uiso 1 1 calc R . . C33 C 0.8277(3) -0.01438(14) 0.0486(2) 0.0430(9) Uani 1 1 d . . . H33 H 0.8631 -0.0516 0.0580 0.052 Uiso 1 1 calc R . . C34 C 0.8080(3) 0.01337(14) -0.0350(2) 0.0375(8) Uani 1 1 d . . . H34 H 0.8298 -0.0045 -0.0829 0.045 Uiso 1 1 calc R . . C35 C 0.7565(2) 0.06715(14) -0.04856(19) 0.0330(7) Uani 1 1 d . . . H35 H 0.7424 0.0863 -0.1062 0.040 Uiso 1 1 calc R . . C36 C 0.7253(2) 0.09342(12) 0.02132(18) 0.0274(6) Uani 1 1 d . . . H36 H 0.6904 0.1308 0.0116 0.033 Uiso 1 1 calc R . . C37 C 0.5171(2) 0.06804(11) 0.14405(17) 0.0206(6) Uani 1 1 d . . . C38 C 0.4816(2) 0.08138(15) 0.04252(18) 0.0341(7) Uani 1 1 d . . . H38A H 0.4822 0.1244 0.0331 0.051 Uiso 1 1 calc R . . H38B H 0.4098 0.0661 0.0160 0.051 Uiso 1 1 calc R . . H38C H 0.5297 0.0622 0.0129 0.051 Uiso 1 1 calc R . . C39 C 0.5313(2) 0.00132(12) 0.1618(2) 0.0320(7) Uani 1 1 d . . . H39A H 0.5862 -0.0136 0.1359 0.048 Uiso 1 1 calc R . . H39B H 0.4645 -0.0191 0.1332 0.048 Uiso 1 1 calc R . . H39C H 0.5522 -0.0060 0.2278 0.048 Uiso 1 1 calc R . . C40 C 0.4345(2) 0.09099(12) 0.18845(18) 0.0242(6) Uani 1 1 d . . . H40A H 0.4569 0.0816 0.2538 0.036 Uiso 1 1 calc R . . H40B H 0.3664 0.0720 0.1597 0.036 Uiso 1 1 calc R . . H40C H 0.4274 0.1341 0.1803 0.036 Uiso 1 1 calc R . . C41 C 0.8886(2) 0.14452(13) 0.26688(18) 0.0258(6) Uani 1 1 d . . . C42 C 0.9036(2) 0.17880(15) 0.1857(2) 0.0421(8) Uani 1 1 d . . . H42A H 0.8985 0.1514 0.1347 0.063 Uiso 1 1 calc R . . H42B H 0.9732 0.1978 0.2029 0.063 Uiso 1 1 calc R . . H42C H 0.8486 0.2093 0.1671 0.063 Uiso 1 1 calc R . . C43 C 0.9645(3) 0.09332(17) 0.2917(3) 0.0678(13) Uani 1 1 d . . . H43A H 0.9470 0.0690 0.3386 0.102 Uiso 1 1 calc R . . H43B H 1.0367 0.1085 0.3154 0.102 Uiso 1 1 calc R . . H43C H 0.9592 0.0690 0.2374 0.102 Uiso 1 1 calc R . . C44 C 0.9076(3) 0.18835(18) 0.3470(2) 0.0550(10) Uani 1 1 d . . . H44A H 0.8561 0.2207 0.3308 0.083 Uiso 1 1 calc R . . H44B H 0.9792 0.2046 0.3603 0.083 Uiso 1 1 calc R . . H44C H 0.8997 0.1676 0.4011 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01362(13) 0.01748(14) 0.01444(13) -0.00369(10) 0.00529(10) -0.00120(10) Ge2 0.02649(16) 0.01728(14) 0.01588(14) -0.00266(11) 0.00698(11) -0.00222(11) Cl1 0.0198(3) 0.0301(4) 0.0186(3) 0.0073(3) 0.0069(3) 0.0037(3) N1 0.0132(10) 0.0155(10) 0.0136(10) -0.0004(8) 0.0048(8) 0.0002(8) N2 0.0117(10) 0.0146(10) 0.0138(10) -0.0013(8) 0.0025(8) -0.0010(8) N3 0.0190(11) 0.0201(11) 0.0152(11) -0.0032(9) 0.0038(9) 0.0001(9) N4 0.0210(12) 0.0266(12) 0.0168(11) -0.0024(9) 0.0069(9) -0.0069(10) C1 0.0165(13) 0.0144(12) 0.0105(12) 0.0024(9) 0.0024(10) 0.0039(10) C2 0.0172(13) 0.0123(12) 0.0142(12) -0.0030(9) 0.0044(10) -0.0008(10) C3 0.0177(13) 0.0133(12) 0.0136(12) 0.0043(10) 0.0037(10) -0.0001(10) C4 0.0184(14) 0.0196(14) 0.0251(14) -0.0026(11) 0.0031(11) -0.0029(11) C5 0.0103(12) 0.0173(13) 0.0175(12) -0.0028(10) 0.0029(10) -0.0016(10) C6 0.0138(13) 0.0186(13) 0.0187(13) -0.0007(10) 0.0018(10) -0.0014(10) C7 0.0176(13) 0.0212(14) 0.0243(14) 0.0040(11) 0.0035(11) 0.0011(11) C8 0.0176(14) 0.0251(15) 0.0302(15) 0.0007(12) 0.0084(12) 0.0060(11) C9 0.0212(14) 0.0277(15) 0.0260(15) 0.0002(12) 0.0133(12) 0.0015(11) C10 0.0164(13) 0.0188(13) 0.0184(13) -0.0001(10) 0.0052(10) -0.0021(10) C11 0.0186(14) 0.0284(15) 0.0210(14) 0.0084(11) 0.0082(11) 0.0066(11) C12 0.0337(17) 0.0325(17) 0.0379(18) 0.0094(14) 0.0167(14) -0.0013(13) C13 0.0361(17) 0.0432(18) 0.0225(15) -0.0026(13) 0.0120(13) 0.0039(14) C14 0.0199(14) 0.0223(14) 0.0204(14) 0.0038(11) 0.0096(11) 0.0024(11) C15 0.0355(17) 0.0293(16) 0.0223(15) 0.0032(12) 0.0102(13) 0.0059(13) C16 0.0237(15) 0.0294(16) 0.0367(17) 0.0100(13) 0.0147(13) 0.0001(12) C17 0.0156(12) 0.0190(13) 0.0142(12) -0.0039(10) 0.0079(10) -0.0026(10) C18 0.0188(13) 0.0203(13) 0.0159(13) -0.0041(10) 0.0090(11) -0.0029(10) C19 0.0254(15) 0.0193(14) 0.0263(15) -0.0054(11) 0.0145(12) -0.0072(11) C20 0.0154(13) 0.0294(15) 0.0275(15) -0.0102(12) 0.0103(11) -0.0082(11) C21 0.0150(13) 0.0274(15) 0.0214(14) -0.0040(11) 0.0049(11) -0.0012(11) C22 0.0169(13) 0.0185(13) 0.0169(13) -0.0029(10) 0.0080(10) -0.0004(10) C23 0.0221(14) 0.0154(13) 0.0224(14) 0.0002(11) 0.0080(11) -0.0021(11) C24 0.0388(17) 0.0189(14) 0.0240(15) 0.0006(11) 0.0119(13) -0.0038(12) C25 0.0265(15) 0.0216(14) 0.0274(15) 0.0004(12) 0.0096(12) 0.0021(12) C26 0.0141(13) 0.0194(13) 0.0192(13) -0.0005(10) 0.0010(10) 0.0007(10) C27 0.0191(14) 0.0255(15) 0.0270(15) -0.0025(12) 0.0010(12) 0.0068(11) C28 0.0245(15) 0.0276(15) 0.0260(15) 0.0030(12) 0.0036(12) -0.0003(12) C29 0.0167(13) 0.0191(13) 0.0135(12) -0.0016(10) 0.0046(10) 0.0002(10) C30 0.0258(14) 0.0161(13) 0.0123(12) 0.0043(10) 0.0056(11) 0.0023(11) C31 0.0217(14) 0.0189(13) 0.0191(13) -0.0029(10) 0.0086(11) -0.0045(11) C32 0.0422(18) 0.0254(15) 0.0328(16) 0.0078(13) 0.0219(14) 0.0072(13) C33 0.062(2) 0.0242(16) 0.057(2) -0.0001(15) 0.0400(19) 0.0072(15) C34 0.046(2) 0.0390(19) 0.0386(18) -0.0159(15) 0.0305(16) -0.0089(15) C35 0.0407(18) 0.0430(19) 0.0194(15) -0.0031(13) 0.0150(13) -0.0087(15) C36 0.0371(17) 0.0239(15) 0.0222(14) 0.0013(12) 0.0101(13) 0.0013(12) C37 0.0188(13) 0.0241(14) 0.0184(13) -0.0038(11) 0.0043(11) 0.0002(11) C38 0.0256(16) 0.059(2) 0.0162(14) -0.0042(14) 0.0031(12) 0.0078(14) C39 0.0292(16) 0.0237(15) 0.0459(19) -0.0092(13) 0.0152(14) -0.0066(12) C40 0.0213(14) 0.0317(16) 0.0189(14) -0.0025(12) 0.0046(11) 0.0024(12) C41 0.0194(14) 0.0358(16) 0.0232(14) 0.0019(12) 0.0078(12) -0.0059(12) C42 0.0338(18) 0.049(2) 0.045(2) 0.0100(16) 0.0140(15) -0.0159(15) C43 0.0256(19) 0.050(2) 0.114(4) 0.025(2) -0.002(2) 0.0014(17) C44 0.045(2) 0.080(3) 0.044(2) -0.0210(19) 0.0181(17) -0.034(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 N1 1.948(2) . ? Ge1 N2 1.9811(19) . ? Ge1 Cl1 2.3340(7) . ? Ge2 N3 1.988(2) . ? Ge2 N4 2.012(2) . ? Ge2 C29 2.085(2) . ? Ge2 C30 2.464(2) . ? N1 C3 1.353(3) . ? N1 C5 1.445(3) . ? N2 C1 1.337(3) . ? N2 C17 1.445(3) . ? N3 C30 1.335(3) . ? N3 C37 1.470(3) . ? N4 C30 1.337(3) . ? N4 C41 1.480(3) . ? C1 C2 1.419(3) . ? C1 C29 1.471(3) . ? C2 C3 1.382(3) . ? C2 H2 0.9500 . ? C3 C4 1.503(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.401(3) . ? C5 C6 1.404(3) . ? C6 C7 1.392(3) . ? C6 C11 1.524(3) . ? C7 C8 1.380(4) . ? C7 H7 0.9500 . ? C8 C9 1.378(4) . ? C8 H8 0.9500 . ? C9 C10 1.396(3) . ? C9 H9 0.9500 . ? C10 C14 1.520(3) . ? C11 C12 1.528(4) . ? C11 C13 1.534(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.533(4) . ? C14 C16 1.538(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.411(3) . ? C17 C22 1.416(3) . ? C18 C19 1.397(3) . ? C18 C23 1.526(3) . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 C26 1.524(3) . ? C23 C25 1.539(3) . ? C23 C24 1.540(3) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.534(3) . ? C26 C27 1.539(3) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.498(3) . ? C31 C36 1.387(4) . ? C31 C32 1.387(4) . ? C32 C33 1.386(4) . ? C32 H32 0.9500 . ? C33 C34 1.378(4) . ? C33 H33 0.9500 . ? C34 C35 1.375(4) . ? C34 H34 0.9500 . ? C35 C36 1.382(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.516(4) . ? C37 C39 1.529(4) . ? C37 C40 1.529(3) . ? 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 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.503(4) . ? C41 C42 1.521(4) . ? C41 C44 1.536(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 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 N1 Ge1 N2 90.42(8) . . ? N1 Ge1 Cl1 96.20(6) . . ? N2 Ge1 Cl1 93.29(6) . . ? N3 Ge2 N4 65.36(8) . . ? N3 Ge2 C29 97.97(9) . . ? N4 Ge2 C29 93.52(9) . . ? N3 Ge2 C30 32.73(8) . . ? N4 Ge2 C30 32.84(8) . . ? C29 Ge2 C30 99.60(9) . . ? C3 N1 C5 120.5(2) . . ? C3 N1 Ge1 122.62(16) . . ? C5 N1 Ge1 116.85(15) . . ? C1 N2 C17 121.98(19) . . ? C1 N2 Ge1 124.95(16) . . ? C17 N2 Ge1 112.71(14) . . ? C30 N3 C37 131.9(2) . . ? C30 N3 Ge2 93.63(15) . . ? C37 N3 Ge2 134.31(16) . . ? C30 N4 C41 130.9(2) . . ? C30 N4 Ge2 92.47(16) . . ? C41 N4 Ge2 132.35(17) . . ? N2 C1 C2 121.0(2) . . ? N2 C1 C29 121.0(2) . . ? C2 C1 C29 117.8(2) . . ? C3 C2 C1 126.8(2) . . ? C3 C2 H2 116.6 . . ? C1 C2 H2 116.6 . . ? N1 C3 C2 122.3(2) . . ? N1 C3 C4 118.8(2) . . ? C2 C3 C4 118.9(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 121.0(2) . . ? C10 C5 N1 120.3(2) . . ? C6 C5 N1 118.6(2) . . ? C7 C6 C5 118.5(2) . . ? C7 C6 C11 118.6(2) . . ? C5 C6 C11 122.9(2) . . ? C8 C7 C6 121.1(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 121.2(2) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C5 118.3(2) . . ? C9 C10 C14 119.3(2) . . ? C5 C10 C14 122.4(2) . . ? C6 C11 C12 112.0(2) . . ? C6 C11 C13 110.7(2) . . ? C12 C11 C13 109.4(2) . . ? C6 C11 H11 108.2 . . ? C12 C11 H11 108.2 . . ? C13 C11 H11 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 C15 111.2(2) . . ? C10 C14 C16 111.0(2) . . ? C15 C14 C16 110.9(2) . . ? C10 C14 H14 107.9 . . ? C15 C14 H14 107.9 . . ? C16 C14 H14 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 121.0(2) . . ? C18 C17 N2 119.2(2) . . ? C22 C17 N2 119.6(2) . . ? C19 C18 C17 117.9(2) . . ? C19 C18 C23 117.8(2) . . ? C17 C18 C23 124.2(2) . . ? C20 C19 C18 121.7(2) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C19 119.5(2) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 121.9(2) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C21 C22 C17 117.9(2) . . ? C21 C22 C26 118.3(2) . . ? C17 C22 C26 123.8(2) . . ? C18 C23 C25 111.0(2) . . ? C18 C23 C24 111.9(2) . . ? C25 C23 C24 108.9(2) . . ? C18 C23 H23 108.3 . . ? C25 C23 H23 108.3 . . ? C24 C23 H23 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C28 111.7(2) . . ? C22 C26 C27 111.9(2) . . ? C28 C26 C27 109.0(2) . . ? C22 C26 H26 108.0 . . ? C28 C26 H26 108.0 . . ? C27 C26 H26 108.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C1 C29 Ge2 111.57(16) . . ? C1 C29 H29A 109.3 . . ? Ge2 C29 H29A 109.3 . . ? C1 C29 H29B 109.3 . . ? Ge2 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? N3 C30 N4 107.9(2) . . ? N3 C30 C31 126.5(2) . . ? N4 C30 C31 125.6(2) . . ? N3 C30 Ge2 53.64(12) . . ? N4 C30 Ge2 54.69(13) . . ? C31 C30 Ge2 172.53(17) . . ? C36 C31 C32 119.1(2) . . ? C36 C31 C30 120.5(2) . . ? C32 C31 C30 120.4(2) . . ? C33 C32 C31 119.9(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C33 119.6(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.5(3) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? N3 C37 C38 112.3(2) . . ? N3 C37 C39 109.1(2) . . ? C38 C37 C39 111.3(2) . . ? N3 C37 C40 105.7(2) . . ? C38 C37 C40 109.6(2) . . ? C39 C37 C40 108.7(2) . . ? 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 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C43 110.6(2) . . ? N4 C41 C42 112.7(2) . . ? C43 C41 C42 111.3(3) . . ? N4 C41 C44 104.6(2) . . ? C43 C41 C44 110.3(3) . . ? C42 C41 C44 107.1(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ge1 N1 C3 35.22(19) . . . . ? Cl1 Ge1 N1 C3 -58.13(18) . . . . ? N2 Ge1 N1 C5 -146.88(17) . . . . ? Cl1 Ge1 N1 C5 119.77(16) . . . . ? N1 Ge1 N2 C1 -25.32(19) . . . . ? Cl1 Ge1 N2 C1 70.91(18) . . . . ? N1 Ge1 N2 C17 161.41(16) . . . . ? Cl1 Ge1 N2 C17 -102.35(15) . . . . ? N4 Ge2 N3 C30 -5.15(14) . . . . ? C29 Ge2 N3 C30 -95.38(15) . . . . ? N4 Ge2 N3 C37 170.8(3) . . . . ? C29 Ge2 N3 C37 80.6(2) . . . . ? C30 Ge2 N3 C37 175.9(3) . . . . ? N3 Ge2 N4 C30 5.14(14) . . . . ? C29 Ge2 N4 C30 102.30(15) . . . . ? N3 Ge2 N4 C41 162.9(2) . . . . ? C29 Ge2 N4 C41 -99.9(2) . . . . ? C30 Ge2 N4 C41 157.8(3) . . . . ? C17 N2 C1 C2 176.6(2) . . . . ? Ge1 N2 C1 C2 3.9(3) . . . . ? C17 N2 C1 C29 -8.2(3) . . . . ? Ge1 N2 C1 C29 179.16(16) . . . . ? N2 C1 C2 C3 20.4(4) . . . . ? C29 C1 C2 C3 -155.0(2) . . . . ? C5 N1 C3 C2 157.5(2) . . . . ? Ge1 N1 C3 C2 -24.7(3) . . . . ? C5 N1 C3 C4 -22.8(3) . . . . ? Ge1 N1 C3 C4 155.00(17) . . . . ? C1 C2 C3 N1 -9.3(4) . . . . ? C1 C2 C3 C4 171.0(2) . . . . ? C3 N1 C5 C10 103.3(3) . . . . ? Ge1 N1 C5 C10 -74.7(3) . . . . ? C3 N1 C5 C6 -80.5(3) . . . . ? Ge1 N1 C5 C6 101.5(2) . . . . ? C10 C5 C6 C7 0.2(4) . . . . ? N1 C5 C6 C7 -176.0(2) . . . . ? C10 C5 C6 C11 -178.4(2) . . . . ? N1 C5 C6 C11 5.4(3) . . . . ? C5 C6 C7 C8 1.4(4) . . . . ? C11 C6 C7 C8 180.0(2) . . . . ? C6 C7 C8 C9 -1.7(4) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? C8 C9 C10 C5 1.1(4) . . . . ? C8 C9 C10 C14 -177.4(2) . . . . ? C6 C5 C10 C9 -1.4(4) . . . . ? N1 C5 C10 C9 174.7(2) . . . . ? C6 C5 C10 C14 177.0(2) . . . . ? N1 C5 C10 C14 -6.9(4) . . . . ? C7 C6 C11 C12 51.6(3) . . . . ? C5 C6 C11 C12 -129.8(3) . . . . ? C7 C6 C11 C13 -70.7(3) . . . . ? C5 C6 C11 C13 107.8(3) . . . . ? C9 C10 C14 C15 -69.1(3) . . . . ? C5 C10 C14 C15 112.5(3) . . . . ? C9 C10 C14 C16 54.9(3) . . . . ? C5 C10 C14 C16 -123.6(3) . . . . ? C1 N2 C17 C18 113.0(3) . . . . ? Ge1 N2 C17 C18 -73.5(2) . . . . ? C1 N2 C17 C22 -72.6(3) . . . . ? Ge1 N2 C17 C22 100.9(2) . . . . ? C22 C17 C18 C19 -0.8(3) . . . . ? N2 C17 C18 C19 173.4(2) . . . . ? C22 C17 C18 C23 -178.2(2) . . . . ? N2 C17 C18 C23 -4.0(3) . . . . ? C17 C18 C19 C20 0.0(4) . . . . ? C23 C18 C19 C20 177.6(2) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C20 C21 C22 C26 -179.4(2) . . . . ? C18 C17 C22 C21 1.1(3) . . . . ? N2 C17 C22 C21 -173.2(2) . . . . ? C18 C17 C22 C26 180.0(2) . . . . ? N2 C17 C22 C26 5.7(3) . . . . ? C19 C18 C23 C25 -67.1(3) . . . . ? C17 C18 C23 C25 110.3(3) . . . . ? C19 C18 C23 C24 54.8(3) . . . . ? C17 C18 C23 C24 -127.8(2) . . . . ? C21 C22 C26 C28 60.6(3) . . . . ? C17 C22 C26 C28 -118.3(3) . . . . ? C21 C22 C26 C27 -61.9(3) . . . . ? C17 C22 C26 C27 119.2(2) . . . . ? N2 C1 C29 Ge2 -79.3(2) . . . . ? C2 C1 C29 Ge2 96.1(2) . . . . ? N3 Ge2 C29 C1 -121.90(17) . . . . ? N4 Ge2 C29 C1 172.51(17) . . . . ? C30 Ge2 C29 C1 -154.98(17) . . . . ? C37 N3 C30 N4 -168.7(2) . . . . ? Ge2 N3 C30 N4 7.4(2) . . . . ? C37 N3 C30 C31 13.2(4) . . . . ? Ge2 N3 C30 C31 -170.7(2) . . . . ? C37 N3 C30 Ge2 -176.1(3) . . . . ? C41 N4 C30 N3 -165.6(2) . . . . ? Ge2 N4 C30 N3 -7.3(2) . . . . ? C41 N4 C30 C31 12.5(4) . . . . ? Ge2 N4 C30 C31 170.8(2) . . . . ? C41 N4 C30 Ge2 -158.3(3) . . . . ? N4 Ge2 C30 N3 171.3(2) . . . . ? C29 Ge2 C30 N3 89.82(16) . . . . ? N3 Ge2 C30 N4 -171.3(2) . . . . ? C29 Ge2 C30 N4 -81.52(16) . . . . ? N3 Ge2 C30 C31 94.0(14) . . . . ? N4 Ge2 C30 C31 -94.7(14) . . . . ? C29 Ge2 C30 C31 -176.2(14) . . . . ? N3 C30 C31 C36 76.7(3) . . . . ? N4 C30 C31 C36 -101.1(3) . . . . ? Ge2 C30 C31 C36 -11.7(16) . . . . ? N3 C30 C31 C32 -105.7(3) . . . . ? N4 C30 C31 C32 76.5(3) . . . . ? Ge2 C30 C31 C32 165.9(13) . . . . ? C36 C31 C32 C33 -0.3(4) . . . . ? C30 C31 C32 C33 -177.9(3) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C32 C33 C34 C35 -0.1(5) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C34 C35 C36 C31 -0.6(4) . . . . ? C32 C31 C36 C35 0.6(4) . . . . ? C30 C31 C36 C35 178.2(3) . . . . ? C30 N3 C37 C38 -62.2(3) . . . . ? Ge2 N3 C37 C38 123.2(2) . . . . ? C30 N3 C37 C39 61.6(3) . . . . ? Ge2 N3 C37 C39 -112.9(2) . . . . ? C30 N3 C37 C40 178.3(2) . . . . ? Ge2 N3 C37 C40 3.8(3) . . . . ? C30 N4 C41 C43 -76.1(4) . . . . ? Ge2 N4 C41 C43 133.8(3) . . . . ? C30 N4 C41 C42 49.2(4) . . . . ? Ge2 N4 C41 C42 -100.9(3) . . . . ? C30 N4 C41 C44 165.2(3) . . . . ? Ge2 N4 C41 C44 15.1(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.710 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.062