data_twin4_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C33 H43 Cl Ge N3), 3(C7 H8), 2(Cl3 Ge)' _chemical_formula_sum 'C43.50 H55 Cl4 Ge2 N3' _chemical_formula_weight 906.89 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.330(3) _cell_length_b 13.013(3) _cell_length_c 16.873(7) _cell_angle_alpha 93.66(2) _cell_angle_beta 97.33(2) _cell_angle_gamma 103.26(2) _cell_volume 2179.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9725 _cell_measurement_theta_min 2.240 _cell_measurement_theta_max 26.743 _exptl_crystal_description needle _exptl_crystal_colour orange _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 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.654535 _exptl_absorpt_correction_T_max 0.745432 _exptl_absorpt_process_details 'TWINABS-2008/4' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker Smart Apex II Quazar' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9181 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.83 _reflns_number_total 9181 _reflns_number_gt 7897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2011.2' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'shelXle v0.477' _computing_publication_material ? _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^)+(0.0247P)^2^+0.9303P] 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 9181 _refine_ls_number_parameters 517 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.039 _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 0.905455(17) 0.591489(13) 0.309696(10) 0.01608(5) Uani 1 1 d . . . Ge2 Ge 0.389955(19) 0.557060(15) 0.229204(11) 0.02243(5) Uani 1 1 d . . . Cl1 Cl 0.71249(4) 0.59838(3) 0.35515(3) 0.02335(9) Uani 1 1 d . . . Cl2 Cl 0.42387(4) 0.40981(4) 0.15862(3) 0.02694(10) Uani 1 1 d . . . Cl3 Cl 0.17240(4) 0.54600(3) 0.16699(3) 0.02452(10) Uani 1 1 d . . . Cl4 Cl 0.49081(5) 0.67973(4) 0.14878(3) 0.02868(10) Uani 1 1 d . . . N1 N 0.81637(13) 0.55168(10) 0.19124(8) 0.0147(3) Uani 1 1 d . . . N2 N 0.82915(13) 0.41355(10) 0.29433(8) 0.0150(3) Uani 1 1 d . . . N3 N 0.90106(13) 0.74593(10) 0.25563(8) 0.0155(3) Uani 1 1 d . . . C1 C 0.80586(16) 0.62825(13) 0.14237(9) 0.0150(3) Uani 1 1 d . . . C2 C 0.74983(16) 0.60316(13) 0.06234(10) 0.0177(3) Uani 1 1 d . . . H2 H 0.7420 0.6577 0.0285 0.021 Uiso 1 1 calc R . . C3 C 0.70546(17) 0.49767(13) 0.03251(10) 0.0187(3) Uani 1 1 d . . . H3 H 0.6658 0.4788 -0.0220 0.022 Uiso 1 1 calc R . . C4 C 0.71948(16) 0.42001(13) 0.08286(10) 0.0181(3) Uani 1 1 d . . . H4 H 0.6913 0.3473 0.0629 0.022 Uiso 1 1 calc R . . C5 C 0.77473(16) 0.44872(13) 0.16234(9) 0.0157(3) Uani 1 1 d . . . C6 C 0.79018(16) 0.37225(13) 0.22214(10) 0.0161(3) Uani 1 1 d . . . C7 C 0.7609(2) 0.25667(13) 0.19449(10) 0.0250(4) Uani 1 1 d . . . H7A H 0.7838 0.2174 0.2398 0.038 Uiso 1 1 calc R . . H7B H 0.8147 0.2460 0.1522 0.038 Uiso 1 1 calc R . . H7C H 0.6652 0.2309 0.1734 0.038 Uiso 1 1 calc R . . C8 C 0.86049(16) 0.73821(13) 0.18030(10) 0.0161(3) Uani 1 1 d . . . C9 C 0.86691(19) 0.82858(13) 0.12957(10) 0.0222(4) Uani 1 1 d . . . H9A H 0.9126 0.8950 0.1623 0.033 Uiso 1 1 calc R . . H9B H 0.7755 0.8320 0.1078 0.033 Uiso 1 1 calc R . . H9C H 0.9168 0.8181 0.0853 0.033 Uiso 1 1 calc R . . C10 C 0.84560(16) 0.35038(12) 0.36026(9) 0.0158(3) Uani 1 1 d . . . C11 C 0.73158(17) 0.29715(13) 0.39167(10) 0.0177(3) Uani 1 1 d . . . C12 C 0.75364(17) 0.23789(13) 0.45598(10) 0.0202(4) Uani 1 1 d . . . H12 H 0.6786 0.1991 0.4774 0.024 Uiso 1 1 calc R . . C13 C 0.88116(18) 0.23407(14) 0.48921(10) 0.0210(4) Uani 1 1 d . . . H13 H 0.8932 0.1933 0.5331 0.025 Uiso 1 1 calc R . . C14 C 0.99175(17) 0.28971(13) 0.45860(10) 0.0188(3) Uani 1 1 d . . . H14 H 1.0795 0.2878 0.4824 0.023 Uiso 1 1 calc R . . C15 C 0.97620(17) 0.34860(13) 0.39319(9) 0.0163(3) Uani 1 1 d . . . C16 C 1.09907(16) 0.40273(13) 0.35773(10) 0.0176(3) Uani 1 1 d . . . H16 H 1.0692 0.4468 0.3159 0.021 Uiso 1 1 calc R . . C17 C 1.15657(18) 0.31894(15) 0.31610(11) 0.0253(4) Uani 1 1 d . . . H17A H 1.0869 0.2747 0.2751 0.038 Uiso 1 1 calc R . . H17B H 1.1867 0.2744 0.3558 0.038 Uiso 1 1 calc R . . H17C H 1.2329 0.3541 0.2907 0.038 Uiso 1 1 calc R . . C18 C 1.20400(18) 0.47667(14) 0.42070(11) 0.0254(4) Uani 1 1 d . . . H18A H 1.2364 0.4353 0.4621 0.038 Uiso 1 1 calc R . . H18B H 1.1635 0.5294 0.4454 0.038 Uiso 1 1 calc R . . H18C H 1.2795 0.5128 0.3951 0.038 Uiso 1 1 calc R . . C19 C 0.58900(17) 0.30317(14) 0.36036(10) 0.0205(4) Uani 1 1 d . . . H19 H 0.5933 0.3495 0.3152 0.025 Uiso 1 1 calc R . . C20 C 0.52678(19) 0.35335(16) 0.42582(12) 0.0292(4) Uani 1 1 d . . . H20A H 0.5851 0.4229 0.4466 0.044 Uiso 1 1 calc R . . H20B H 0.5174 0.3074 0.4696 0.044 Uiso 1 1 calc R . . H20C H 0.4381 0.3619 0.4032 0.044 Uiso 1 1 calc R . . C21 C 0.49944(19) 0.19363(15) 0.32776(12) 0.0303(4) Uani 1 1 d . . . H21A H 0.4911 0.1475 0.3714 0.045 Uiso 1 1 calc R . . H21B H 0.5399 0.1623 0.2857 0.045 Uiso 1 1 calc R . . H21C H 0.4102 0.2011 0.3053 0.045 Uiso 1 1 calc R . . C22 C 0.96525(16) 0.84649(12) 0.30116(9) 0.0161(3) Uani 1 1 d . . . C23 C 1.10580(17) 0.87909(13) 0.31117(9) 0.0170(3) Uani 1 1 d . . . C24 C 1.16619(18) 0.97377(13) 0.35900(10) 0.0210(4) Uani 1 1 d . . . H24 H 1.2613 0.9983 0.3666 0.025 Uiso 1 1 calc R . . C25 C 1.09094(18) 1.03247(14) 0.39551(10) 0.0229(4) Uani 1 1 d . . . H25 H 1.1343 1.0963 0.4282 0.027 Uiso 1 1 calc R . . C26 C 0.95269(18) 0.99837(14) 0.38452(11) 0.0233(4) Uani 1 1 d . . . H26 H 0.9017 1.0396 0.4096 0.028 Uiso 1 1 calc R . . C27 C 0.88630(17) 0.90478(13) 0.33743(10) 0.0192(3) Uani 1 1 d . . . C28 C 1.19337(17) 0.81817(14) 0.27166(10) 0.0194(4) Uani 1 1 d . . . H28 H 1.1330 0.7547 0.2385 0.023 Uiso 1 1 calc R . . C29 C 1.2743(2) 0.88642(16) 0.21580(11) 0.0291(4) Uani 1 1 d . . . H29A H 1.3355 0.9486 0.2473 0.044 Uiso 1 1 calc R . . H29B H 1.2127 0.9097 0.1756 0.044 Uiso 1 1 calc R . . H29C H 1.3265 0.8447 0.1887 0.044 Uiso 1 1 calc R . . C30 C 1.28694(19) 0.77931(15) 0.33386(11) 0.0265(4) Uani 1 1 d . . . H30A H 1.2335 0.7274 0.3638 0.040 Uiso 1 1 calc R . . H30B H 1.3400 0.8395 0.3710 0.040 Uiso 1 1 calc R . . H30C H 1.3474 0.7460 0.3067 0.040 Uiso 1 1 calc R . . C31 C 0.73382(18) 0.87296(15) 0.32548(11) 0.0244(4) Uani 1 1 d . . . H31 H 0.7039 0.8031 0.2921 0.029 Uiso 1 1 calc R . . C32 C 0.6763(2) 0.95481(17) 0.27981(13) 0.0355(5) Uani 1 1 d . . . H32A H 0.7134 0.9632 0.2293 0.053 Uiso 1 1 calc R . . H32B H 0.7006 1.0231 0.3127 0.053 Uiso 1 1 calc R . . H32C H 0.5781 0.9304 0.2682 0.053 Uiso 1 1 calc R . . C33 C 0.67959(19) 0.85998(16) 0.40530(12) 0.0317(4) Uani 1 1 d . . . H33A H 0.7023 0.9288 0.4375 0.048 Uiso 1 1 calc R . . H33B H 0.7200 0.8097 0.4346 0.048 Uiso 1 1 calc R . . H33C H 0.5817 0.8332 0.3951 0.048 Uiso 1 1 calc R . . C34 C 0.03627(18) 0.16438(14) 0.09181(10) 0.0230(4) Uani 1 1 d D . . C35 C -0.07964(19) 0.09860(14) 0.04840(10) 0.0249(4) Uani 1 1 d D . . H35 H -0.1001 0.0248 0.0546 0.030 Uiso 1 1 calc R . . C36 C -0.16566(18) 0.13892(15) -0.00366(10) 0.0250(4) Uani 1 1 d D . . H36 H -0.2453 0.0929 -0.0322 0.030 Uiso 1 1 calc R . . C37 C -0.13648(18) 0.24625(14) -0.01455(10) 0.0243(4) Uani 1 1 d D . . H37 H -0.1943 0.2736 -0.0514 0.029 Uiso 1 1 calc R . . C38 C -0.02238(18) 0.31262(14) 0.02894(11) 0.0248(4) Uani 1 1 d D . . H38 H -0.0024 0.3864 0.0226 0.030 Uiso 1 1 calc R . . C39 C 0.06322(18) 0.27237(14) 0.08179(11) 0.0235(4) Uani 1 1 d D . . H39 H 0.1412 0.3190 0.1115 0.028 Uiso 1 1 calc R . . C40 C 0.1302(2) 0.11930(17) 0.14787(12) 0.0376(5) Uani 1 1 d D . . H40A H 0.0844 0.0912 0.1921 0.056 Uiso 1 1 calc R . . H40B H 0.2103 0.1753 0.1695 0.056 Uiso 1 1 calc R . . H40C H 0.1570 0.0621 0.1184 0.056 Uiso 1 1 calc R . . C41' C 0.4231(4) 0.1766(3) 0.0424(2) 0.0283(8) Uani 0.50 1 d PDU A -1 H41A H 0.4581 0.2337 0.0100 0.043 Uiso 0.50 1 calc PR A -1 H41B H 0.4569 0.1991 0.0993 0.043 Uiso 0.50 1 calc PR A -1 H41C H 0.3246 0.1607 0.0341 0.043 Uiso 0.50 1 calc PR A -1 C42' C 0.4686(12) 0.0787(7) 0.0176(6) 0.0217(15) Uani 0.50 1 d PDU A -1 C43' C 0.5049(14) 0.0130(8) 0.0751(5) 0.0235(18) Uani 0.50 1 d PDU A -1 H43' H 0.5056 0.0322 0.1305 0.028 Uiso 0.50 1 calc PR A -1 C44' C 0.5395(16) -0.0795(9) 0.0514(7) 0.0271(18) Uani 0.50 1 d PDU A -1 H44' H 0.5615 -0.1242 0.0908 0.033 Uiso 0.50 1 calc PR A -1 C45' C 0.5427(13) -0.1081(7) -0.0284(6) 0.0256(17) Uani 0.50 1 d PDU A -1 H45' H 0.5673 -0.1716 -0.0442 0.031 Uiso 0.50 1 calc PR A -1 C46' C 0.5092(17) -0.0423(9) -0.0849(7) 0.0271(18) Uani 0.50 1 d PDU A -1 H46' H 0.5114 -0.0609 -0.1400 0.032 Uiso 0.50 1 calc PR A -1 C47' C 0.4729(13) 0.0495(8) -0.0628(6) 0.0224(18) Uani 0.50 1 d PDU A -1 H47' H 0.4504 0.0934 -0.1026 0.027 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01701(9) 0.01577(9) 0.01402(9) 0.00124(7) -0.00183(7) 0.00329(7) Ge2 0.02085(10) 0.02840(11) 0.01720(10) 0.00238(8) 0.00271(7) 0.00419(8) Cl1 0.0260(2) 0.0240(2) 0.0225(2) 0.00420(17) 0.00792(17) 0.00806(18) Cl2 0.0222(2) 0.0299(2) 0.0308(2) 0.00524(19) 0.00548(18) 0.00907(18) Cl3 0.0206(2) 0.0233(2) 0.0291(2) 0.00136(18) 0.00284(17) 0.00482(17) Cl4 0.0257(2) 0.0269(2) 0.0311(2) 0.00328(19) 0.00748(19) -0.00050(18) N1 0.0120(7) 0.0179(7) 0.0140(7) 0.0021(5) 0.0017(5) 0.0030(5) N2 0.0124(7) 0.0171(7) 0.0152(7) 0.0029(5) 0.0014(5) 0.0028(5) N3 0.0143(7) 0.0145(7) 0.0167(7) 0.0004(5) -0.0001(5) 0.0034(5) C1 0.0127(8) 0.0172(8) 0.0157(8) 0.0031(6) 0.0035(6) 0.0035(6) C2 0.0177(8) 0.0211(9) 0.0153(8) 0.0040(7) 0.0029(6) 0.0057(7) C3 0.0174(8) 0.0250(9) 0.0129(8) 0.0006(7) 0.0008(6) 0.0049(7) C4 0.0165(8) 0.0178(8) 0.0182(8) -0.0007(7) 0.0033(7) 0.0008(7) C5 0.0132(8) 0.0169(8) 0.0165(8) 0.0013(6) 0.0031(6) 0.0021(6) C6 0.0133(8) 0.0170(8) 0.0172(8) 0.0021(6) 0.0028(6) 0.0017(6) C7 0.0367(11) 0.0170(9) 0.0185(9) 0.0013(7) 0.0018(8) 0.0021(8) C8 0.0129(8) 0.0175(8) 0.0183(8) 0.0020(6) 0.0016(6) 0.0048(6) C9 0.0278(10) 0.0186(9) 0.0192(9) 0.0049(7) 0.0002(7) 0.0047(7) C10 0.0201(8) 0.0133(8) 0.0129(8) 0.0000(6) 0.0010(6) 0.0030(6) C11 0.0189(8) 0.0160(8) 0.0174(8) -0.0009(6) 0.0023(7) 0.0032(7) C12 0.0220(9) 0.0181(9) 0.0189(8) 0.0022(7) 0.0052(7) 0.0003(7) C13 0.0278(10) 0.0206(9) 0.0158(8) 0.0043(7) 0.0036(7) 0.0074(7) C14 0.0201(9) 0.0200(9) 0.0174(8) 0.0019(7) 0.0015(7) 0.0077(7) C15 0.0192(8) 0.0145(8) 0.0151(8) -0.0003(6) 0.0027(6) 0.0041(6) C16 0.0159(8) 0.0185(9) 0.0185(8) 0.0045(7) 0.0019(6) 0.0041(7) C17 0.0228(9) 0.0281(10) 0.0263(10) 0.0019(8) 0.0088(8) 0.0060(8) C18 0.0222(9) 0.0247(10) 0.0262(10) 0.0019(8) 0.0035(7) -0.0004(7) C19 0.0166(8) 0.0218(9) 0.0214(9) 0.0035(7) 0.0017(7) 0.0012(7) C20 0.0205(9) 0.0345(11) 0.0324(10) 0.0009(8) 0.0047(8) 0.0061(8) C21 0.0210(10) 0.0287(11) 0.0357(11) 0.0003(8) -0.0014(8) -0.0010(8) C22 0.0205(9) 0.0130(8) 0.0132(8) 0.0021(6) -0.0021(6) 0.0033(6) C23 0.0197(8) 0.0169(8) 0.0144(8) 0.0052(6) 0.0017(6) 0.0037(7) C24 0.0194(9) 0.0188(9) 0.0216(9) 0.0039(7) -0.0003(7) -0.0003(7) C25 0.0284(10) 0.0147(8) 0.0215(9) -0.0009(7) -0.0030(7) 0.0014(7) C26 0.0251(9) 0.0205(9) 0.0249(9) -0.0009(7) 0.0004(7) 0.0096(7) C27 0.0205(9) 0.0173(9) 0.0191(8) 0.0017(7) -0.0016(7) 0.0059(7) C28 0.0170(8) 0.0213(9) 0.0187(8) 0.0004(7) 0.0023(7) 0.0025(7) C29 0.0293(10) 0.0340(11) 0.0250(10) 0.0051(8) 0.0097(8) 0.0060(8) C30 0.0263(10) 0.0329(11) 0.0236(9) 0.0029(8) 0.0049(8) 0.0133(8) C31 0.0188(9) 0.0252(10) 0.0276(10) -0.0063(8) -0.0031(7) 0.0082(7) C32 0.0311(11) 0.0380(12) 0.0381(11) -0.0015(9) -0.0072(9) 0.0179(9) C33 0.0202(9) 0.0383(12) 0.0345(11) -0.0065(9) 0.0027(8) 0.0065(8) C34 0.0257(10) 0.0257(10) 0.0187(9) 0.0000(7) 0.0040(7) 0.0089(8) C35 0.0337(10) 0.0180(9) 0.0217(9) 0.0014(7) 0.0066(8) 0.0020(8) C36 0.0220(9) 0.0280(10) 0.0211(9) -0.0032(7) 0.0030(7) -0.0006(8) C37 0.0270(10) 0.0299(10) 0.0191(9) 0.0040(7) 0.0051(7) 0.0116(8) C38 0.0296(10) 0.0188(9) 0.0275(10) 0.0041(7) 0.0107(8) 0.0047(8) C39 0.0215(9) 0.0211(9) 0.0258(9) -0.0038(7) 0.0044(7) 0.0017(7) C40 0.0476(13) 0.0364(12) 0.0305(11) -0.0044(9) -0.0065(9) 0.0225(10) C41' 0.026(2) 0.030(2) 0.027(2) 0.0001(17) 0.0005(16) 0.0064(17) C42' 0.016(3) 0.017(4) 0.029(4) -0.001(3) 0.003(2) 0.000(3) C43' 0.019(3) 0.030(7) 0.019(3) 0.005(4) 0.000(3) 0.001(5) C44' 0.022(3) 0.024(5) 0.034(4) 0.009(3) 0.002(3) 0.001(4) C45' 0.023(3) 0.020(5) 0.031(3) -0.003(3) 0.001(2) 0.001(3) C46' 0.023(4) 0.021(5) 0.031(3) -0.004(3) 0.004(2) -0.004(3) C47' 0.023(4) 0.022(6) 0.018(3) 0.002(3) 0.000(2) -0.002(4) _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 2.0712(15) . ? Ge1 Cl1 2.2434(8) . ? Ge1 N2 2.2548(15) . ? Ge1 N3 2.2669(14) . ? Ge2 Cl2 2.3101(7) . ? Ge2 Cl4 2.3128(8) . ? Ge2 Cl3 2.3246(8) . ? N1 C1 1.348(2) . ? N1 C5 1.348(2) . ? N2 C6 1.275(2) . ? N2 C10 1.440(2) . ? N3 C8 1.277(2) . ? N3 C22 1.444(2) . ? C1 C2 1.387(2) . ? C1 C8 1.482(2) . ? C2 C3 1.383(2) . ? C3 C4 1.382(2) . ? C4 C5 1.381(2) . ? C5 C6 1.481(2) . ? C6 C7 1.496(2) . ? C8 C9 1.492(2) . ? C10 C15 1.398(2) . ? C10 C11 1.407(2) . ? C11 C12 1.396(2) . ? C11 C19 1.521(2) . ? C12 C13 1.377(2) . ? C13 C14 1.384(2) . ? C14 C15 1.397(2) . ? C15 C16 1.517(2) . ? C16 C18 1.525(2) . ? C16 C17 1.530(2) . ? C19 C20 1.530(3) . ? C19 C21 1.535(2) . ? C22 C23 1.401(2) . ? C22 C27 1.403(2) . ? C23 C24 1.397(2) . ? C23 C28 1.519(2) . ? C24 C25 1.379(3) . ? C25 C26 1.379(3) . ? C26 C27 1.392(2) . ? C27 C31 1.517(2) . ? C28 C30 1.525(2) . ? C28 C29 1.531(2) . ? C31 C33 1.528(3) . ? C31 C32 1.536(3) . ? C34 C35 1.389(3) . ? C34 C39 1.394(2) . ? C34 C40 1.510(3) . ? C35 C36 1.382(3) . ? C36 C37 1.389(3) . ? C37 C38 1.380(3) . ? C38 C39 1.387(3) . ? C41' C42' 1.510(6) . ? C42' C47' 1.393(9) . ? C42' C43' 1.405(9) . ? C43' C44' 1.382(7) . ? C44' C45' 1.380(9) . ? C45' C46' 1.386(9) . ? C46' C47' 1.375(7) . ? 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 Cl1 94.25(5) . . ? N1 Ge1 N2 73.52(5) . . ? Cl1 Ge1 N2 87.18(4) . . ? N1 Ge1 N3 73.28(5) . . ? Cl1 Ge1 N3 88.08(4) . . ? N2 Ge1 N3 145.99(5) . . ? Cl2 Ge2 Cl4 96.16(3) . . ? Cl2 Ge2 Cl3 97.18(3) . . ? Cl4 Ge2 Cl3 94.74(3) . . ? C1 N1 C5 120.17(14) . . ? C1 N1 Ge1 120.21(11) . . ? C5 N1 Ge1 119.55(11) . . ? C6 N2 C10 122.20(14) . . ? C6 N2 Ge1 115.58(11) . . ? C10 N2 Ge1 121.38(10) . . ? C8 N3 C22 122.30(14) . . ? C8 N3 Ge1 116.03(11) . . ? C22 N3 Ge1 120.59(10) . . ? N1 C1 C2 121.06(15) . . ? N1 C1 C8 115.07(14) . . ? C2 C1 C8 123.86(15) . . ? C3 C2 C1 119.07(15) . . ? C4 C3 C2 119.25(15) . . ? C5 C4 C3 119.65(16) . . ? N1 C5 C4 120.78(15) . . ? N1 C5 C6 115.01(14) . . ? C4 C5 C6 124.20(15) . . ? N2 C6 C5 114.96(14) . . ? N2 C6 C7 125.88(15) . . ? C5 C6 C7 119.16(14) . . ? N3 C8 C1 114.93(14) . . ? N3 C8 C9 125.69(15) . . ? C1 C8 C9 119.37(14) . . ? C15 C10 C11 122.36(15) . . ? C15 C10 N2 118.12(14) . . ? C11 C10 N2 119.45(15) . . ? C12 C11 C10 116.96(16) . . ? C12 C11 C19 119.51(15) . . ? C10 C11 C19 123.51(15) . . ? C13 C12 C11 121.86(16) . . ? C12 C13 C14 119.94(16) . . ? C13 C14 C15 120.95(16) . . ? C14 C15 C10 117.89(15) . . ? C14 C15 C16 119.53(15) . . ? C10 C15 C16 122.49(15) . . ? C15 C16 C18 111.87(14) . . ? C15 C16 C17 109.54(14) . . ? C18 C16 C17 112.09(14) . . ? C11 C19 C20 110.81(14) . . ? C11 C19 C21 111.76(15) . . ? C20 C19 C21 110.09(15) . . ? C23 C22 C27 122.40(15) . . ? C23 C22 N3 118.20(14) . . ? C27 C22 N3 119.30(15) . . ? C24 C23 C22 117.25(15) . . ? C24 C23 C28 119.35(15) . . ? C22 C23 C28 123.40(15) . . ? C25 C24 C23 121.52(17) . . ? C24 C25 C26 119.91(16) . . ? C25 C26 C27 121.40(16) . . ? C26 C27 C22 117.52(16) . . ? C26 C27 C31 119.04(15) . . ? C22 C27 C31 123.41(15) . . ? C23 C28 C30 111.51(14) . . ? C23 C28 C29 110.60(14) . . ? C30 C28 C29 110.46(15) . . ? C27 C31 C33 111.68(15) . . ? C27 C31 C32 110.14(16) . . ? C33 C31 C32 110.54(16) . . ? C35 C34 C39 118.21(17) . . ? C35 C34 C40 120.50(17) . . ? C39 C34 C40 121.29(17) . . ? C36 C35 C34 120.95(17) . . ? C35 C36 C37 120.43(17) . . ? C38 C37 C36 119.14(17) . . ? C37 C38 C39 120.43(17) . . ? C38 C39 C34 120.82(16) . . ? C47' C42' C43' 118.2(5) . . ? C47' C42' C41' 121.2(6) . . ? C43' C42' C41' 120.6(6) . . ? C44' C43' C42' 120.2(7) . . ? C45' C44' C43' 121.2(8) . . ? C44' C45' C46' 118.6(6) . . ? C47' C46' C45' 121.2(8) . . ? C46' C47' C42' 120.7(7) . . ? 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 Cl1 Ge1 N1 C1 89.98(12) . . . . ? N2 Ge1 N1 C1 175.77(13) . . . . ? N3 Ge1 N1 C1 3.27(11) . . . . ? Cl1 Ge1 N1 C5 -93.14(11) . . . . ? N2 Ge1 N1 C5 -7.34(11) . . . . ? N3 Ge1 N1 C5 -179.85(12) . . . . ? N1 Ge1 N2 C6 10.83(11) . . . . ? Cl1 Ge1 N2 C6 106.11(12) . . . . ? N3 Ge1 N2 C6 23.74(16) . . . . ? N1 Ge1 N2 C10 -179.47(13) . . . . ? Cl1 Ge1 N2 C10 -84.19(11) . . . . ? N3 Ge1 N2 C10 -166.57(10) . . . . ? N1 Ge1 N3 C8 -6.14(11) . . . . ? Cl1 Ge1 N3 C8 -101.16(12) . . . . ? N2 Ge1 N3 C8 -19.06(17) . . . . ? N1 Ge1 N3 C22 -174.49(13) . . . . ? Cl1 Ge1 N3 C22 90.49(12) . . . . ? N2 Ge1 N3 C22 172.59(10) . . . . ? C5 N1 C1 C2 1.4(2) . . . . ? Ge1 N1 C1 C2 178.24(12) . . . . ? C5 N1 C1 C8 -177.42(13) . . . . ? Ge1 N1 C1 C8 -0.56(18) . . . . ? N1 C1 C2 C3 -0.6(2) . . . . ? C8 C1 C2 C3 178.08(15) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? C2 C3 C4 C5 1.4(2) . . . . ? C1 N1 C5 C4 -0.7(2) . . . . ? Ge1 N1 C5 C4 -177.63(12) . . . . ? C1 N1 C5 C6 -179.34(14) . . . . ? Ge1 N1 C5 C6 3.78(18) . . . . ? C3 C4 C5 N1 -0.6(2) . . . . ? C3 C4 C5 C6 177.81(15) . . . . ? C10 N2 C6 C5 178.19(14) . . . . ? Ge1 N2 C6 C5 -12.20(18) . . . . ? C10 N2 C6 C7 -2.2(3) . . . . ? Ge1 N2 C6 C7 167.38(13) . . . . ? N1 C5 C6 N2 6.2(2) . . . . ? C4 C5 C6 N2 -172.38(15) . . . . ? N1 C5 C6 C7 -173.45(14) . . . . ? C4 C5 C6 C7 8.0(2) . . . . ? C22 N3 C8 C1 175.83(14) . . . . ? Ge1 N3 C8 C1 7.69(18) . . . . ? C22 N3 C8 C9 -2.8(3) . . . . ? Ge1 N3 C8 C9 -170.90(13) . . . . ? N1 C1 C8 N3 -5.0(2) . . . . ? C2 C1 C8 N3 176.23(15) . . . . ? N1 C1 C8 C9 173.68(14) . . . . ? C2 C1 C8 C9 -5.1(2) . . . . ? C6 N2 C10 C15 104.81(18) . . . . ? Ge1 N2 C10 C15 -64.20(17) . . . . ? C6 N2 C10 C11 -78.2(2) . . . . ? Ge1 N2 C10 C11 112.78(14) . . . . ? C15 C10 C11 C12 -2.6(2) . . . . ? N2 C10 C11 C12 -179.44(14) . . . . ? C15 C10 C11 C19 176.13(15) . . . . ? N2 C10 C11 C19 -0.7(2) . . . . ? C10 C11 C12 C13 2.1(2) . . . . ? C19 C11 C12 C13 -176.72(15) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C13 C14 C15 -1.2(3) . . . . ? C13 C14 C15 C10 0.7(2) . . . . ? C13 C14 C15 C16 -176.00(15) . . . . ? C11 C10 C15 C14 1.3(2) . . . . ? N2 C10 C15 C14 178.18(14) . . . . ? C11 C10 C15 C16 177.83(15) . . . . ? N2 C10 C15 C16 -5.3(2) . . . . ? C14 C15 C16 C18 -55.9(2) . . . . ? C10 C15 C16 C18 127.65(17) . . . . ? C14 C15 C16 C17 69.07(19) . . . . ? C10 C15 C16 C17 -107.42(18) . . . . ? C12 C11 C19 C20 61.1(2) . . . . ? C10 C11 C19 C20 -117.63(18) . . . . ? C12 C11 C19 C21 -62.1(2) . . . . ? C10 C11 C19 C21 119.18(18) . . . . ? C8 N3 C22 C23 -92.59(19) . . . . ? Ge1 N3 C22 C23 75.02(17) . . . . ? C8 N3 C22 C27 91.0(2) . . . . ? Ge1 N3 C22 C27 -101.34(15) . . . . ? C27 C22 C23 C24 -0.4(2) . . . . ? N3 C22 C23 C24 -176.63(14) . . . . ? C27 C22 C23 C28 -179.16(15) . . . . ? N3 C22 C23 C28 4.6(2) . . . . ? C22 C23 C24 C25 0.5(2) . . . . ? C28 C23 C24 C25 179.37(16) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C24 C25 C26 C27 0.4(3) . . . . ? C25 C26 C27 C22 -0.3(3) . . . . ? C25 C26 C27 C31 -178.18(16) . . . . ? C23 C22 C27 C26 0.3(2) . . . . ? N3 C22 C27 C26 176.47(14) . . . . ? C23 C22 C27 C31 178.06(16) . . . . ? N3 C22 C27 C31 -5.7(2) . . . . ? C24 C23 C28 C30 63.5(2) . . . . ? C22 C23 C28 C30 -117.70(18) . . . . ? C24 C23 C28 C29 -59.8(2) . . . . ? C22 C23 C28 C29 118.96(18) . . . . ? C26 C27 C31 C33 -59.1(2) . . . . ? C22 C27 C31 C33 123.13(18) . . . . ? C26 C27 C31 C32 64.1(2) . . . . ? C22 C27 C31 C32 -113.65(19) . . . . ? C39 C34 C35 C36 0.3(3) . . . . ? C40 C34 C35 C36 -179.37(17) . . . . ? C34 C35 C36 C37 1.1(3) . . . . ? C35 C36 C37 C38 -1.8(3) . . . . ? C36 C37 C38 C39 1.1(3) . . . . ? C37 C38 C39 C34 0.3(3) . . . . ? C35 C34 C39 C38 -1.0(3) . . . . ? C40 C34 C39 C38 178.70(17) . . . . ? C47' C42' C43' C44' -1.9(15) . . . . ? C41' C42' C43' C44' 176.5(10) . . . . ? C42' C43' C44' C45' 1.6(17) . . . . ? C43' C44' C45' C46' -0.5(19) . . . . ? C44' C45' C46' C47' -0.3(19) . . . . ? C45' C46' C47' C42' 0.0(18) . . . . ? C43' C42' C47' C46' 1.2(16) . . . . ? C41' C42' C47' C46' -177.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.357 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.051