# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1908 data_dr068 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Ge N3 Se2 Si2' _chemical_formula_weight 766.46 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' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 10.828(1) _cell_length_b 25.140(3) _cell_length_c 26.674(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.304(2) _cell_angle_gamma 90.00 _cell_volume 7185(1) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 2.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.577694 _exptl_absorpt_correction_T_max 0.801525 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 56421 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.77 _reflns_number_total 16791 _reflns_number_gt 9809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 16791 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.004 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 0.06648(3) 0.553348(12) 0.200401(12) 0.02178(8) Uani 1 1 d . . . Ge2 Ge 0.51218(3) 0.806555(13) 0.035563(12) 0.02318(8) Uani 1 1 d . . . Se1 Se 0.04608(3) 0.478388(13) 0.254369(13) 0.03193(9) Uani 1 1 d . . . Se2 Se -0.13333(3) 0.590568(13) 0.178462(13) 0.03015(9) Uani 1 1 d . . . Se3 Se 0.45142(3) 0.877813(13) -0.021972(13) 0.03506(9) Uani 1 1 d . . . Se4 Se 0.33118(3) 0.778504(14) 0.067145(13) 0.03052(9) Uani 1 1 d . . . Si1 Si 0.16857(9) 0.46506(4) 0.13409(4) 0.0330(2) Uani 1 1 d . . . Si2 Si 0.16436(8) 0.58194(4) 0.10064(4) 0.0311(2) Uani 1 1 d . . . Si3 Si 0.64177(8) 0.69695(4) 0.03629(4) 0.0300(2) Uani 1 1 d . . . Si4 Si 0.59633(9) 0.75929(4) -0.06343(4) 0.0319(2) Uani 1 1 d . . . N1 N 0.1787(2) 0.59783(10) 0.23962(9) 0.0246(6) Uani 1 1 d . . . N2 N 0.0265(2) 0.65926(10) 0.24498(10) 0.0277(6) Uani 1 1 d . . . N3 N 0.1347(2) 0.53242(9) 0.14425(9) 0.0246(6) Uani 1 1 d . . . N4 N 0.6355(2) 0.83520(10) 0.08451(9) 0.0244(6) Uani 1 1 d . . . N5 N 0.5058(2) 0.82714(10) 0.14422(9) 0.0253(6) Uani 1 1 d . . . N6 N 0.5830(2) 0.75343(9) 0.00121(9) 0.0254(6) Uani 1 1 d . . . C1 C 0.3764(3) 0.55251(13) 0.28253(12) 0.0343(8) Uani 1 1 d . . . H1A H 0.3284 0.5195 0.2835 0.041 Uiso 1 1 calc R . . H1B H 0.3771 0.5708 0.3150 0.041 Uiso 1 1 calc R . . C2 C 0.5100(3) 0.53931(15) 0.27469(15) 0.0496(11) Uani 1 1 d . . . H2B H 0.5501 0.5183 0.3034 0.060 Uiso 1 1 calc R . . H2C H 0.5083 0.5178 0.2440 0.060 Uiso 1 1 calc R . . C3 C 0.5859(3) 0.58953(16) 0.26980(15) 0.0552(11) Uani 1 1 d . . . H3A H 0.5939 0.6096 0.3016 0.066 Uiso 1 1 calc R . . H3B H 0.6699 0.5798 0.2634 0.066 Uiso 1 1 calc R . . C4 C 0.5233(3) 0.62378(16) 0.22691(15) 0.0571(12) Uani 1 1 d . . . H4A H 0.5223 0.6047 0.1948 0.068 Uiso 1 1 calc R . . H4B H 0.5717 0.6565 0.2252 0.068 Uiso 1 1 calc R . . C5 C 0.3908(3) 0.63803(14) 0.23373(14) 0.0435(10) Uani 1 1 d . . . H5B H 0.3518 0.6584 0.2043 0.052 Uiso 1 1 calc R . . H5C H 0.3920 0.6604 0.2639 0.052 Uiso 1 1 calc R . . C6 C 0.3142(3) 0.58805(12) 0.23942(12) 0.0284(8) Uani 1 1 d . . . H6A H 0.3186 0.5674 0.2081 0.034 Uiso 1 1 calc R . . C7 C -0.1694(3) 0.69222(13) 0.26871(15) 0.0440(10) Uani 1 1 d . . . H7A H -0.1790 0.6602 0.2887 0.053 Uiso 1 1 calc R . . H7B H -0.2093 0.6856 0.2339 0.053 Uiso 1 1 calc R . . C8 C -0.2342(3) 0.73889(14) 0.29079(15) 0.0512(11) Uani 1 1 d . . . H8A H -0.3232 0.7309 0.2895 0.061 Uiso 1 1 calc R . . H8B H -0.1985 0.7439 0.3264 0.061 Uiso 1 1 calc R . . C9 C -0.2190(3) 0.78925(14) 0.26169(14) 0.0473(10) Uani 1 1 d . . . H9A H -0.2572 0.8190 0.2775 0.057 Uiso 1 1 calc R . . H9B H -0.2617 0.7855 0.2269 0.057 Uiso 1 1 calc R . . C10 C -0.0809(3) 0.80082(13) 0.26095(15) 0.0472(10) Uani 1 1 d . . . H10A H -0.0726 0.8321 0.2398 0.057 Uiso 1 1 calc R . . H10B H -0.0406 0.8089 0.2954 0.057 Uiso 1 1 calc R . . C11 C -0.0160(3) 0.75376(12) 0.24042(14) 0.0382(9) Uani 1 1 d . . . H11A H -0.0496 0.7487 0.2046 0.046 Uiso 1 1 calc R . . H11B H 0.0733 0.7615 0.2426 0.046 Uiso 1 1 calc R . . C12 C -0.0325(3) 0.70322(12) 0.26881(12) 0.0299(8) Uani 1 1 d . . . H12A H 0.0086 0.7072 0.3043 0.036 Uiso 1 1 calc R . . C13 C 0.1317(3) 0.64051(12) 0.26443(12) 0.0259(7) Uani 1 1 d . . . C14 C 0.2032(3) 0.65861(13) 0.31452(13) 0.0417(9) Uani 1 1 d . . . H14A H 0.1599 0.6882 0.3275 0.063 Uiso 1 1 calc R . . H14B H 0.2864 0.6697 0.3096 0.063 Uiso 1 1 calc R . . H14C H 0.2092 0.6295 0.3386 0.063 Uiso 1 1 calc R . . C15 C -0.0668(3) 0.54897(15) 0.32052(14) 0.0457(10) Uani 1 1 d . . . H15A H -0.1337 0.5510 0.2939 0.055 Uiso 1 1 calc R . . C16 C -0.0727(4) 0.57631(15) 0.36556(16) 0.0531(11) Uani 1 1 d . . . H16A H -0.1424 0.5976 0.3689 0.064 Uiso 1 1 calc R . . C17 C 0.0225(4) 0.57220(15) 0.40468(15) 0.0550(11) Uani 1 1 d . . . H17A H 0.0176 0.5903 0.4352 0.066 Uiso 1 1 calc R . . C18 C 0.1255(4) 0.54189(15) 0.40000(14) 0.0532(11) Uani 1 1 d . . . H18A H 0.1902 0.5386 0.4274 0.064 Uiso 1 1 calc R . . C19 C 0.1335(3) 0.51647(14) 0.35509(13) 0.0426(9) Uani 1 1 d . . . H19A H 0.2058 0.4970 0.3514 0.051 Uiso 1 1 calc R . . C20 C 0.0367(3) 0.51890(12) 0.31495(12) 0.0278(8) Uani 1 1 d . . . C21 C -0.2676(3) 0.49126(14) 0.16760(13) 0.0420(10) Uani 1 1 d . . . H21A H -0.2542 0.4908 0.2032 0.050 Uiso 1 1 calc R . . C22 C -0.3385(3) 0.45117(16) 0.14101(16) 0.0574(11) Uani 1 1 d . . . H22A H -0.3726 0.4238 0.1587 0.069 Uiso 1 1 calc R . . C23 C -0.3582(4) 0.45188(17) 0.08948(17) 0.0622(12) Uani 1 1 d . . . H23A H -0.4063 0.4250 0.0715 0.075 Uiso 1 1 calc R . . C24 C -0.3080(4) 0.49163(18) 0.06370(15) 0.0657(13) Uani 1 1 d . . . H24A H -0.3213 0.4919 0.0281 0.079 Uiso 1 1 calc R . . C25 C -0.2383(3) 0.53105(15) 0.08983(14) 0.0480(10) Uani 1 1 d . . . H25A H -0.2043 0.5583 0.0719 0.058 Uiso 1 1 calc R . . C26 C -0.2174(3) 0.53130(13) 0.14196(13) 0.0304(8) Uani 1 1 d . . . C27 C 0.2183(4) 0.45407(14) 0.07040(13) 0.0551(11) Uani 1 1 d . . . H27A H 0.1523 0.4655 0.0441 0.083 Uiso 1 1 calc R . . H27B H 0.2351 0.4166 0.0661 0.083 Uiso 1 1 calc R . . H27C H 0.2934 0.4744 0.0681 0.083 Uiso 1 1 calc R . . C28 C 0.3010(3) 0.44103(13) 0.18083(13) 0.0471(10) Uani 1 1 d . . . H28A H 0.2820 0.4466 0.2149 0.071 Uiso 1 1 calc R . . H28B H 0.3760 0.4606 0.1765 0.071 Uiso 1 1 calc R . . H28C H 0.3141 0.4034 0.1755 0.071 Uiso 1 1 calc R . . C29 C 0.0291(3) 0.42212(13) 0.13484(15) 0.0521(11) Uani 1 1 d . . . H29A H -0.0024 0.4265 0.1668 0.078 Uiso 1 1 calc R . . H29B H 0.0520 0.3852 0.1308 0.078 Uiso 1 1 calc R . . H29C H -0.0350 0.4323 0.1073 0.078 Uiso 1 1 calc R . . C30 C 0.3341(3) 0.58137(15) 0.09368(14) 0.0475(10) Uani 1 1 d . . . H30A H 0.3572 0.5463 0.0830 0.071 Uiso 1 1 calc R . . H30B H 0.3835 0.5901 0.1259 0.071 Uiso 1 1 calc R . . H30C H 0.3496 0.6074 0.0685 0.071 Uiso 1 1 calc R . . C31 C 0.1256(3) 0.65008(12) 0.12105(13) 0.0368(9) Uani 1 1 d . . . H31A H 0.0379 0.6517 0.1249 0.055 Uiso 1 1 calc R . . H31B H 0.1426 0.6757 0.0957 0.055 Uiso 1 1 calc R . . H31C H 0.1761 0.6584 0.1532 0.055 Uiso 1 1 calc R . . C32 C 0.0685(3) 0.57122(14) 0.03715(13) 0.0474(10) Uani 1 1 d . . . H32A H 0.0847 0.5360 0.0249 0.071 Uiso 1 1 calc R . . H32B H 0.0905 0.5977 0.0135 0.071 Uiso 1 1 calc R . . H32C H -0.0194 0.5745 0.0402 0.071 Uiso 1 1 calc R . . C33 C 0.8034(3) 0.89181(13) 0.05320(13) 0.0338(8) Uani 1 1 d . . . H33A H 0.7991 0.9187 0.0795 0.041 Uiso 1 1 calc R . . H33B H 0.7448 0.9021 0.0233 0.041 Uiso 1 1 calc R . . C34 C 0.9359(3) 0.89024(15) 0.03954(13) 0.0435(10) Uani 1 1 d . . . H34A H 0.9379 0.8668 0.0103 0.052 Uiso 1 1 calc R . . H34B H 0.9604 0.9260 0.0302 0.052 Uiso 1 1 calc R . . C35 C 1.0279(3) 0.87000(15) 0.08417(14) 0.0475(10) Uani 1 1 d . . . H35A H 1.1120 0.8689 0.0746 0.057 Uiso 1 1 calc R . . H35B H 1.0294 0.8946 0.1128 0.057 Uiso 1 1 calc R . . C36 C 0.9925(3) 0.81561(15) 0.09993(14) 0.0451(10) Uani 1 1 d . . . H36A H 1.0524 0.8038 0.1289 0.054 Uiso 1 1 calc R . . H36B H 0.9964 0.7906 0.0720 0.054 Uiso 1 1 calc R . . C37 C 0.8617(3) 0.81495(14) 0.11446(13) 0.0372(9) Uani 1 1 d . . . H37A H 0.8609 0.8359 0.1454 0.045 Uiso 1 1 calc R . . H37B H 0.8388 0.7783 0.1216 0.045 Uiso 1 1 calc R . . C38 C 0.7652(3) 0.83781(13) 0.07220(12) 0.0294(8) Uani 1 1 d . . . H38A H 0.7660 0.8133 0.0432 0.035 Uiso 1 1 calc R . . C39 C 0.3538(3) 0.88723(13) 0.17333(12) 0.0354(8) Uani 1 1 d . . . H39A H 0.3921 0.9178 0.1588 0.042 Uiso 1 1 calc R . . H39B H 0.2895 0.8728 0.1473 0.042 Uiso 1 1 calc R . . C40 C 0.2934(3) 0.90556(14) 0.21843(14) 0.0453(10) Uani 1 1 d . . . H40A H 0.3559 0.9234 0.2430 0.054 Uiso 1 1 calc R . . H40B H 0.2272 0.9312 0.2070 0.054 Uiso 1 1 calc R . . C41 C 0.2388(3) 0.85895(15) 0.24373(15) 0.0531(11) Uani 1 1 d . . . H41A H 0.2054 0.8714 0.2739 0.064 Uiso 1 1 calc R . . H41B H 0.1698 0.8436 0.2204 0.064 Uiso 1 1 calc R . . C42 C 0.3372(4) 0.81639(15) 0.25898(14) 0.0517(11) Uani 1 1 d . . . H42A H 0.2985 0.7858 0.2734 0.062 Uiso 1 1 calc R . . H42B H 0.4019 0.8306 0.2850 0.062 Uiso 1 1 calc R . . C43 C 0.3966(3) 0.79839(13) 0.21317(13) 0.0385(9) Uani 1 1 d . . . H43A H 0.4620 0.7722 0.2240 0.046 Uiso 1 1 calc R . . H43B H 0.3332 0.7813 0.1885 0.046 Uiso 1 1 calc R . . C44 C 0.4526(3) 0.84507(13) 0.18842(12) 0.0290(8) Uani 1 1 d . . . H44A H 0.5199 0.8607 0.2131 0.035 Uiso 1 1 calc R . . C45 C 0.6007(3) 0.84976(12) 0.13082(12) 0.0258(7) Uani 1 1 d . . . C46 C 0.6727(3) 0.89390(12) 0.16124(12) 0.0332(8) Uani 1 1 d . . . H46A H 0.6377 0.8998 0.1923 0.050 Uiso 1 1 calc R . . H46B H 0.6666 0.9264 0.1414 0.050 Uiso 1 1 calc R . . H46C H 0.7596 0.8837 0.1695 0.050 Uiso 1 1 calc R . . C47 C 0.5034(3) 0.96214(13) 0.05236(13) 0.0376(9) Uani 1 1 d . . . H47A H 0.5876 0.9565 0.0490 0.045 Uiso 1 1 calc R . . C48 C 0.4711(3) 1.00262(14) 0.08270(13) 0.0437(10) Uani 1 1 d . . . H48A H 0.5338 1.0242 0.1003 0.052 Uiso 1 1 calc R . . C49 C 0.3480(4) 1.01181(14) 0.08748(14) 0.0456(10) Uani 1 1 d . . . H49A H 0.3264 1.0400 0.1077 0.055 Uiso 1 1 calc R . . C50 C 0.2564(3) 0.97930(15) 0.06234(14) 0.0488(10) Uani 1 1 d . . . H50A H 0.1722 0.9850 0.0659 0.059 Uiso 1 1 calc R . . C51 C 0.2886(3) 0.93810(14) 0.03168(13) 0.0397(9) Uani 1 1 d . . . H51A H 0.2262 0.9161 0.0144 0.048 Uiso 1 1 calc R . . C52 C 0.4117(3) 0.92966(12) 0.02677(12) 0.0327(8) Uani 1 1 d . . . C53 C 0.1585(3) 0.79043(14) -0.02615(13) 0.0379(9) Uani 1 1 d . . . H53A H 0.1547 0.8263 -0.0165 0.045 Uiso 1 1 calc R . . C54 C 0.0858(3) 0.77255(16) -0.07008(13) 0.0457(10) Uani 1 1 d . . . H54A H 0.0336 0.7965 -0.0902 0.055 Uiso 1 1 calc R . . C55 C 0.0894(4) 0.72047(17) -0.08435(15) 0.0586(12) Uani 1 1 d . . . H55A H 0.0400 0.7087 -0.1142 0.070 Uiso 1 1 calc R . . C56 C 0.1657(4) 0.68525(15) -0.05492(15) 0.0605(12) Uani 1 1 d . . . H56A H 0.1681 0.6493 -0.0645 0.073 Uiso 1 1 calc R . . C57 C 0.2391(3) 0.70293(14) -0.01094(14) 0.0457(10) Uani 1 1 d . . . H57A H 0.2910 0.6788 0.0091 0.055 Uiso 1 1 calc R . . C58 C 0.2367(3) 0.75530(13) 0.00346(12) 0.0300(8) Uani 1 1 d . . . C59 C 0.6151(3) 0.69985(13) 0.10392(12) 0.0398(9) Uani 1 1 d . . . H59A H 0.5265 0.7034 0.1054 0.060 Uiso 1 1 calc R . . H59B H 0.6592 0.7302 0.1204 0.060 Uiso 1 1 calc R . . H59C H 0.6459 0.6675 0.1211 0.060 Uiso 1 1 calc R . . C60 C 0.5639(3) 0.63438(13) 0.00932(13) 0.0408(9) Uani 1 1 d . . . H60A H 0.5730 0.6315 -0.0262 0.061 Uiso 1 1 calc R . . H60B H 0.4759 0.6355 0.0127 0.061 Uiso 1 1 calc R . . H60C H 0.6025 0.6039 0.0275 0.061 Uiso 1 1 calc R . . C61 C 0.8138(3) 0.69050(14) 0.03556(14) 0.0476(10) Uani 1 1 d . . . H61A H 0.8302 0.6890 0.0008 0.071 Uiso 1 1 calc R . . H61B H 0.8439 0.6582 0.0531 0.071 Uiso 1 1 calc R . . H61C H 0.8563 0.7210 0.0524 0.071 Uiso 1 1 calc R . . C62 C 0.6584(4) 0.69777(14) -0.08976(13) 0.0539(11) Uani 1 1 d . . . H62A H 0.6029 0.6682 -0.0860 0.081 Uiso 1 1 calc R . . H62B H 0.7407 0.6900 -0.0716 0.081 Uiso 1 1 calc R . . H62C H 0.6640 0.7030 -0.1254 0.081 Uiso 1 1 calc R . . C63 C 0.4429(3) 0.77005(15) -0.10312(13) 0.0520(11) Uani 1 1 d . . . H63A H 0.4178 0.8068 -0.1004 0.078 Uiso 1 1 calc R . . H63B H 0.3810 0.7469 -0.0916 0.078 Uiso 1 1 calc R . . H63C H 0.4497 0.7620 -0.1382 0.078 Uiso 1 1 calc R . . C64 C 0.7085(3) 0.81346(14) -0.07391(13) 0.0509(10) Uani 1 1 d . . . H64A H 0.6694 0.8478 -0.0708 0.076 Uiso 1 1 calc R . . H64B H 0.7318 0.8100 -0.1075 0.076 Uiso 1 1 calc R . . H64C H 0.7825 0.8107 -0.0488 0.076 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 0.02150(16) 0.02052(18) 0.02316(19) -0.00123(16) 0.00271(14) -0.00181(14) Ge2 0.02227(17) 0.02376(19) 0.02326(19) -0.00042(16) 0.00251(14) 0.00001(15) Se1 0.0427(2) 0.02358(18) 0.0303(2) 0.00159(16) 0.00781(16) -0.00393(16) Se2 0.02296(16) 0.02943(19) 0.0370(2) -0.00363(17) 0.00089(14) 0.00032(14) Se3 0.0466(2) 0.0295(2) 0.0287(2) 0.00377(17) 0.00409(16) 0.00725(16) Se4 0.02433(17) 0.0389(2) 0.0285(2) -0.00290(17) 0.00424(14) -0.00469(15) Si1 0.0424(6) 0.0258(5) 0.0316(6) -0.0041(5) 0.0084(4) 0.0041(4) Si2 0.0358(5) 0.0318(6) 0.0266(5) 0.0035(5) 0.0080(4) -0.0015(4) Si3 0.0319(5) 0.0270(5) 0.0308(6) 0.0027(5) 0.0033(4) 0.0045(4) Si4 0.0407(5) 0.0312(5) 0.0244(6) -0.0004(5) 0.0072(4) 0.0041(4) N1 0.0207(13) 0.0243(15) 0.0280(16) -0.0051(13) 0.0007(11) -0.0013(11) N2 0.0242(14) 0.0275(15) 0.0311(17) -0.0078(13) 0.0034(12) 0.0003(12) N3 0.0279(14) 0.0218(14) 0.0251(16) -0.0029(12) 0.0072(11) 0.0002(11) N4 0.0193(13) 0.0329(16) 0.0221(15) -0.0050(13) 0.0062(11) -0.0033(11) N5 0.0262(14) 0.0289(15) 0.0218(15) -0.0020(13) 0.0070(12) -0.0003(12) N6 0.0258(14) 0.0262(15) 0.0246(15) 0.0001(12) 0.0052(11) 0.0066(12) C1 0.0327(19) 0.033(2) 0.035(2) 0.0024(17) -0.0006(15) 0.0070(16) C2 0.034(2) 0.057(3) 0.053(3) -0.007(2) -0.0087(18) 0.0169(19) C3 0.0206(18) 0.082(3) 0.059(3) -0.003(3) -0.0056(18) 0.001(2) C4 0.027(2) 0.078(3) 0.065(3) 0.014(3) 0.0008(19) -0.011(2) C5 0.0284(19) 0.051(2) 0.049(2) 0.013(2) -0.0010(17) -0.0094(17) C6 0.0225(16) 0.0326(19) 0.029(2) -0.0054(16) 0.0005(14) -0.0006(14) C7 0.043(2) 0.031(2) 0.063(3) 0.002(2) 0.0252(19) 0.0040(17) C8 0.054(2) 0.048(2) 0.057(3) 0.000(2) 0.026(2) 0.015(2) C9 0.055(2) 0.041(2) 0.047(3) 0.000(2) 0.0128(19) 0.0184(19) C10 0.059(3) 0.027(2) 0.053(3) 0.0018(19) 0.001(2) 0.0078(18) C11 0.036(2) 0.030(2) 0.050(2) 0.0010(18) 0.0091(17) -0.0008(16) C12 0.0322(18) 0.0295(19) 0.0264(19) -0.0063(16) -0.0012(15) 0.0046(15) C13 0.0266(17) 0.0240(18) 0.0269(19) 0.0018(15) 0.0030(14) -0.0055(14) C14 0.039(2) 0.037(2) 0.045(2) -0.0118(19) -0.0092(17) 0.0035(17) C15 0.042(2) 0.063(3) 0.034(2) 0.002(2) 0.0096(17) 0.010(2) C16 0.053(2) 0.057(3) 0.055(3) 0.002(2) 0.027(2) 0.017(2) C17 0.090(3) 0.044(3) 0.036(3) -0.009(2) 0.025(2) -0.008(2) C18 0.070(3) 0.058(3) 0.030(2) -0.005(2) 0.000(2) 0.010(2) C19 0.046(2) 0.045(2) 0.036(2) 0.003(2) 0.0041(18) 0.0138(18) C20 0.0357(19) 0.0238(18) 0.0244(19) 0.0063(15) 0.0064(15) -0.0019(15) C21 0.040(2) 0.054(3) 0.030(2) -0.0005(19) 0.0007(17) -0.0185(18) C22 0.059(3) 0.056(3) 0.055(3) 0.002(2) -0.001(2) -0.026(2) C23 0.060(3) 0.059(3) 0.061(3) -0.015(3) -0.009(2) -0.025(2) C24 0.080(3) 0.080(3) 0.034(3) -0.017(2) -0.002(2) -0.017(3) C25 0.054(2) 0.051(3) 0.040(3) 0.003(2) 0.0072(19) -0.015(2) C26 0.0228(17) 0.037(2) 0.031(2) -0.0039(17) 0.0009(15) -0.0021(15) C27 0.082(3) 0.046(2) 0.041(2) -0.009(2) 0.020(2) 0.020(2) C28 0.054(2) 0.040(2) 0.048(3) 0.003(2) 0.0078(19) 0.0202(19) C29 0.063(3) 0.031(2) 0.063(3) -0.014(2) 0.012(2) -0.0058(19) C30 0.042(2) 0.054(3) 0.050(3) 0.007(2) 0.0187(18) -0.0041(19) C31 0.044(2) 0.032(2) 0.034(2) 0.0082(17) 0.0064(17) -0.0033(16) C32 0.056(2) 0.048(2) 0.037(2) 0.0020(19) 0.0022(19) 0.0037(19) C33 0.0305(18) 0.040(2) 0.032(2) 0.0001(17) 0.0078(15) -0.0048(16) C34 0.032(2) 0.055(3) 0.045(2) 0.002(2) 0.0118(17) -0.0103(18) C35 0.0279(19) 0.063(3) 0.052(3) -0.001(2) 0.0075(17) -0.0090(19) C36 0.0240(18) 0.066(3) 0.044(2) 0.006(2) -0.0002(16) -0.0004(18) C37 0.0322(19) 0.048(2) 0.032(2) 0.0063(18) 0.0061(16) -0.0024(17) C38 0.0229(17) 0.037(2) 0.029(2) -0.0012(17) 0.0066(14) -0.0002(15) C39 0.0355(19) 0.035(2) 0.038(2) 0.0010(17) 0.0133(16) -0.0019(16) C40 0.045(2) 0.041(2) 0.054(3) -0.008(2) 0.0206(19) 0.0013(18) C41 0.049(2) 0.062(3) 0.054(3) -0.013(2) 0.026(2) -0.012(2) C42 0.062(3) 0.056(3) 0.043(3) 0.005(2) 0.026(2) -0.013(2) C43 0.044(2) 0.038(2) 0.035(2) 0.0061(18) 0.0106(17) 0.0008(17) C44 0.0255(17) 0.037(2) 0.0246(19) -0.0001(16) 0.0043(14) -0.0041(15) C45 0.0243(17) 0.0277(19) 0.0245(19) 0.0027(15) 0.0009(14) 0.0017(14) C46 0.0371(19) 0.038(2) 0.025(2) -0.0081(16) 0.0078(15) -0.0132(16) C47 0.040(2) 0.031(2) 0.041(2) 0.0012(18) 0.0038(17) -0.0009(16) C48 0.055(3) 0.032(2) 0.039(2) -0.0029(19) -0.0096(19) -0.0031(18) C49 0.066(3) 0.028(2) 0.042(2) -0.0024(19) 0.007(2) 0.0091(19) C50 0.045(2) 0.047(2) 0.057(3) 0.002(2) 0.016(2) 0.009(2) C51 0.044(2) 0.035(2) 0.040(2) -0.0016(18) 0.0049(17) -0.0009(17) C52 0.046(2) 0.0224(18) 0.029(2) 0.0081(16) 0.0038(16) 0.0060(16) C53 0.0337(19) 0.036(2) 0.042(2) -0.0021(18) 0.0004(17) 0.0000(16) C54 0.041(2) 0.054(3) 0.038(2) 0.007(2) -0.0091(17) -0.0055(19) C55 0.066(3) 0.057(3) 0.044(3) -0.006(2) -0.020(2) -0.020(2) C56 0.084(3) 0.039(2) 0.052(3) -0.011(2) -0.012(2) -0.014(2) C57 0.047(2) 0.036(2) 0.049(3) 0.000(2) -0.0075(19) -0.0050(18) C58 0.0275(17) 0.035(2) 0.028(2) -0.0007(17) 0.0041(15) -0.0084(15) C59 0.049(2) 0.034(2) 0.035(2) 0.0122(18) 0.0016(17) 0.0074(17) C60 0.047(2) 0.033(2) 0.044(2) 0.0015(18) 0.0114(18) 0.0000(17) C61 0.037(2) 0.041(2) 0.062(3) 0.002(2) -0.0012(18) 0.0118(18) C62 0.086(3) 0.044(2) 0.036(2) 0.003(2) 0.024(2) 0.014(2) C63 0.062(3) 0.061(3) 0.030(2) -0.013(2) -0.0047(19) 0.013(2) C64 0.066(3) 0.052(3) 0.039(2) 0.001(2) 0.021(2) -0.006(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 N3 1.840(2) . ? Ge1 N1 1.859(2) . ? Ge1 Se2 2.3522(5) . ? Ge1 Se1 2.4009(5) . ? Ge2 N6 1.848(2) . ? Ge2 N4 1.871(2) . ? Ge2 Se4 2.3505(5) . ? Ge2 Se3 2.3886(5) . ? Se1 C20 1.925(3) . ? Se2 C26 1.934(3) . ? Se3 C52 1.933(3) . ? Se4 C58 1.942(3) . ? Si1 N3 1.762(2) . ? Si1 C28 1.860(3) . ? Si1 C29 1.859(3) . ? Si1 C27 1.876(3) . ? Si2 N3 1.765(3) . ? Si2 C30 1.874(3) . ? Si2 C31 1.864(3) . ? Si2 C32 1.874(3) . ? Si3 N6 1.768(2) . ? Si3 C59 1.869(3) . ? Si3 C61 1.872(3) . ? Si3 C60 1.878(3) . ? Si4 N6 1.757(3) . ? Si4 C63 1.856(3) . ? Si4 C64 1.873(3) . ? Si4 C62 1.864(3) . ? N1 C13 1.395(4) . ? N1 C6 1.489(3) . ? N2 C13 1.272(3) . ? N2 C12 1.467(4) . ? N4 C45 1.392(4) . ? N4 C38 1.490(3) . ? N5 C45 1.270(4) . ? N5 C44 1.456(4) . ? C1 C6 1.533(4) . ? C1 C2 1.528(4) . ? C2 C3 1.522(5) . ? C3 C4 1.512(5) . ? C4 C5 1.514(4) . ? C5 C6 1.525(4) . ? C7 C12 1.508(4) . ? C7 C8 1.528(4) . ? C8 C9 1.506(5) . ? C9 C10 1.526(5) . ? C10 C11 1.518(4) . ? C11 C12 1.503(4) . ? C13 C14 1.514(4) . ? C15 C20 1.378(4) . ? C15 C16 1.394(5) . ? C16 C17 1.361(5) . ? C17 C18 1.371(5) . ? C18 C19 1.372(5) . ? C19 C20 1.387(4) . ? C21 C22 1.397(5) . ? C21 C26 1.372(4) . ? C22 C23 1.360(5) . ? C23 C24 1.369(5) . ? C24 C25 1.373(5) . ? C25 C26 1.376(4) . ? C33 C38 1.527(4) . ? C33 C34 1.531(4) . ? C34 C35 1.525(4) . ? C35 C36 1.497(5) . ? C36 C37 1.521(4) . ? C37 C38 1.534(4) . ? C39 C40 1.521(4) . ? C39 C44 1.518(4) . ? C40 C41 1.514(5) . ? C41 C42 1.523(5) . ? C42 C43 1.529(4) . ? C43 C44 1.515(4) . ? C45 C46 1.521(4) . ? C47 C48 1.376(4) . ? C47 C52 1.386(4) . ? C48 C49 1.377(5) . ? C49 C50 1.382(5) . ? C50 C51 1.395(5) . ? C51 C52 1.375(4) . ? C53 C54 1.389(4) . ? C53 C58 1.389(4) . ? C54 C55 1.366(5) . ? C55 C56 1.376(5) . ? C56 C57 1.392(5) . ? C57 C58 1.373(4) . ? 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 N3 Ge1 N1 108.87(11) . . ? N3 Ge1 Se2 111.98(7) . . ? N1 Ge1 Se2 113.81(7) . . ? N3 Ge1 Se1 110.26(7) . . ? N1 Ge1 Se1 104.13(8) . . ? Se2 Ge1 Se1 107.484(17) . . ? N6 Ge2 N4 108.58(10) . . ? N6 Ge2 Se4 112.84(8) . . ? N4 Ge2 Se4 114.40(8) . . ? N6 Ge2 Se3 108.61(8) . . ? N4 Ge2 Se3 105.20(8) . . ? Se4 Ge2 Se3 106.782(17) . . ? C20 Se1 Ge1 96.23(9) . . ? C26 Se2 Ge1 99.67(9) . . ? C52 Se3 Ge2 98.10(9) . . ? C58 Se4 Ge2 97.91(9) . . ? N3 Si1 C28 111.50(14) . . ? N3 Si1 C29 111.67(14) . . ? C28 Si1 C29 110.68(17) . . ? N3 Si1 C27 111.99(15) . . ? C28 Si1 C27 105.34(17) . . ? C29 Si1 C27 105.32(17) . . ? N3 Si2 C30 109.54(14) . . ? N3 Si2 C31 112.69(13) . . ? C30 Si2 C31 107.54(16) . . ? N3 Si2 C32 111.38(14) . . ? C30 Si2 C32 109.45(17) . . ? C31 Si2 C32 106.11(16) . . ? N6 Si3 C59 112.69(13) . . ? N6 Si3 C61 110.27(14) . . ? C59 Si3 C61 107.81(16) . . ? N6 Si3 C60 111.26(14) . . ? C59 Si3 C60 106.20(15) . . ? C61 Si3 C60 108.41(16) . . ? N6 Si4 C63 112.24(15) . . ? N6 Si4 C64 110.76(14) . . ? C63 Si4 C64 110.81(17) . . ? N6 Si4 C62 112.67(14) . . ? C63 Si4 C62 104.34(17) . . ? C64 Si4 C62 105.67(17) . . ? C13 N1 C6 123.8(2) . . ? C13 N1 Ge1 118.45(18) . . ? C6 N1 Ge1 117.60(19) . . ? C13 N2 C12 121.5(3) . . ? Si1 N3 Si2 120.99(14) . . ? Si1 N3 Ge1 121.12(14) . . ? Si2 N3 Ge1 117.88(13) . . ? C45 N4 C38 124.7(2) . . ? C45 N4 Ge2 117.60(18) . . ? C38 N4 Ge2 117.63(19) . . ? C45 N5 C44 121.3(3) . . ? Si4 N6 Si3 120.84(14) . . ? Si4 N6 Ge2 121.65(13) . . ? Si3 N6 Ge2 117.48(14) . . ? C6 C1 C2 110.2(3) . . ? C3 C2 C1 111.4(3) . . ? C4 C3 C2 110.4(3) . . ? C3 C4 C5 111.9(3) . . ? C4 C5 C6 110.8(3) . . ? N1 C6 C1 114.8(3) . . ? N1 C6 C5 114.5(3) . . ? C1 C6 C5 111.6(2) . . ? C12 C7 C8 111.4(3) . . ? C9 C8 C7 110.9(3) . . ? C8 C9 C10 110.3(3) . . ? C11 C10 C9 111.2(3) . . ? C12 C11 C10 112.5(3) . . ? N2 C12 C11 109.1(3) . . ? N2 C12 C7 110.5(3) . . ? C11 C12 C7 110.0(3) . . ? N2 C13 N1 117.3(3) . . ? N2 C13 C14 124.2(3) . . ? N1 C13 C14 118.4(3) . . ? C20 C15 C16 120.2(3) . . ? C17 C16 C15 120.0(4) . . ? C18 C17 C16 120.6(4) . . ? C17 C18 C19 119.5(4) . . ? C20 C19 C18 121.2(3) . . ? C19 C20 C15 118.5(3) . . ? C19 C20 Se1 120.0(2) . . ? C15 C20 Se1 121.5(2) . . ? C22 C21 C26 120.3(3) . . ? C21 C22 C23 119.9(4) . . ? C22 C23 C24 120.1(4) . . ? C25 C24 C23 120.0(4) . . ? C24 C25 C26 120.9(4) . . ? C25 C26 C21 118.8(3) . . ? C25 C26 Se2 120.6(3) . . ? C21 C26 Se2 120.4(3) . . ? C38 C33 C34 111.4(3) . . ? C35 C34 C33 110.6(3) . . ? C36 C35 C34 111.0(3) . . ? C35 C36 C37 111.5(3) . . ? C36 C37 C38 111.7(3) . . ? N4 C38 C33 114.9(3) . . ? N4 C38 C37 112.7(3) . . ? C33 C38 C37 112.9(3) . . ? C40 C39 C44 111.6(3) . . ? C41 C40 C39 111.0(3) . . ? C42 C41 C40 111.1(3) . . ? C41 C42 C43 110.7(3) . . ? C44 C43 C42 111.1(3) . . ? N5 C44 C43 110.1(3) . . ? N5 C44 C39 110.3(3) . . ? C43 C44 C39 110.2(3) . . ? N5 C45 N4 117.8(3) . . ? N5 C45 C46 123.3(3) . . ? N4 C45 C46 118.8(3) . . ? C48 C47 C52 120.0(3) . . ? C47 C48 C49 120.7(3) . . ? C50 C49 C48 119.5(3) . . ? C49 C50 C51 120.0(3) . . ? C52 C51 C50 119.9(3) . . ? C51 C52 C47 119.8(3) . . ? C51 C52 Se3 118.8(3) . . ? C47 C52 Se3 121.0(3) . . ? C54 C53 C58 119.9(3) . . ? C55 C54 C53 120.7(3) . . ? C54 C55 C56 119.8(3) . . ? C55 C56 C57 119.9(4) . . ? C58 C57 C56 120.7(3) . . ? C57 C58 C53 119.1(3) . . ? C57 C58 Se4 120.3(3) . . ? C53 C58 Se4 120.5(2) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.627 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.096 data_dr070 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 N3 S2 Si2 Sn' _chemical_formula_weight 718.76 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 '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 13.234(2) _cell_length_b 15.834(2) _cell_length_c 19.023(2) _cell_angle_alpha 88.728(2) _cell_angle_beta 80.465(2) _cell_angle_gamma 67.232(2) _cell_volume 3621.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.470766 _exptl_absorpt_correction_T_max 0.801496 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption correction (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 27303 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_sigmaI/netI 0.1718 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.46 _reflns_number_total 15949 _reflns_number_gt 9694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.001P)^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 15949 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 Sn1 Sn 0.398326(19) 0.781490(16) 0.109401(11) 0.02574(6) Uani 1 1 d . . . Sn2 Sn 0.470682(18) 0.259349(15) 0.412088(11) 0.02293(6) Uani 1 1 d . . . S1 S 0.38722(9) 0.93682(7) 0.11902(5) 0.0444(3) Uani 1 1 d . . . S2 S 0.50152(8) 0.74206(8) -0.01484(5) 0.0443(3) Uani 1 1 d . . . S3 S 0.49493(8) 0.09960(6) 0.40791(5) 0.0379(2) Uani 1 1 d . . . S4 S 0.58442(7) 0.27847(6) 0.49802(5) 0.0337(2) Uani 1 1 d . . . Si1 Si 0.16487(9) 0.85763(8) 0.04340(6) 0.0371(2) Uani 1 1 d . . . Si2 Si 0.28039(8) 0.65289(7) 0.06027(5) 0.0328(2) Uani 1 1 d . . . Si3 Si 0.27521(8) 0.27195(7) 0.54685(5) 0.0309(2) Uani 1 1 d . . . Si4 Si 0.29579(8) 0.45017(6) 0.49342(5) 0.0260(2) Uani 1 1 d . . . N1 N 0.3596(2) 0.74683(19) 0.22125(14) 0.0272(6) Uani 1 1 d . . . N2 N 0.5299(2) 0.6995(2) 0.16389(14) 0.0313(7) Uani 1 1 d . . . N3 N 0.2654(2) 0.76514(19) 0.07624(14) 0.0279(6) Uani 1 1 d . . . N4 N 0.3972(2) 0.30490(19) 0.31396(14) 0.0278(6) Uani 1 1 d . . . N5 N 0.5711(2) 0.2784(2) 0.31724(14) 0.0289(7) Uani 1 1 d . . . N6 N 0.3292(2) 0.33313(18) 0.48499(13) 0.0252(6) Uani 1 1 d . . . C1 C 0.7008(3) 0.7235(3) 0.1777(2) 0.0485(11) Uani 1 1 d . . . H1A H 0.6879 0.7216 0.2299 0.058 Uiso 1 1 calc R . . H1B H 0.6642 0.7872 0.1650 0.058 Uiso 1 1 calc R . . C2 C 0.8255(3) 0.6897(3) 0.1499(3) 0.0619(13) Uani 1 1 d . . . H2A H 0.8372 0.7026 0.0992 0.074 Uiso 1 1 calc R . . H2B H 0.8572 0.7239 0.1755 0.074 Uiso 1 1 calc R . . C3 C 0.8851(3) 0.5903(4) 0.1583(3) 0.0654(14) Uani 1 1 d . . . H3A H 0.8839 0.5789 0.2092 0.079 Uiso 1 1 calc R . . H3B H 0.9629 0.5717 0.1354 0.079 Uiso 1 1 calc R . . C4 C 0.8350(3) 0.5330(3) 0.1266(3) 0.0576(12) Uani 1 1 d . . . H4A H 0.8735 0.4686 0.1368 0.069 Uiso 1 1 calc R . . H4B H 0.8445 0.5380 0.0747 0.069 Uiso 1 1 calc R . . C5 C 0.7107(3) 0.5649(3) 0.1576(2) 0.0513(11) Uani 1 1 d . . . H5A H 0.6781 0.5294 0.1342 0.062 Uiso 1 1 calc R . . H5B H 0.7015 0.5541 0.2087 0.062 Uiso 1 1 calc R . . C6 C 0.6517(3) 0.6647(3) 0.1464(2) 0.0378(9) Uani 1 1 d . . . H6A H 0.6677 0.6703 0.0942 0.045 Uiso 1 1 calc R . . C7 C 0.1664(3) 0.8427(2) 0.2659(2) 0.0396(9) Uani 1 1 d . . . H7A H 0.1483 0.8329 0.2196 0.048 Uiso 1 1 calc R . . H7B H 0.1848 0.8971 0.2634 0.048 Uiso 1 1 calc R . . C8 C 0.0649(4) 0.8601(3) 0.3235(2) 0.0554(12) Uani 1 1 d . . . H8A H 0.0804 0.8745 0.3694 0.066 Uiso 1 1 calc R . . H8B H 0.0016 0.9127 0.3117 0.066 Uiso 1 1 calc R . . C9 C 0.0363(4) 0.7762(3) 0.3294(3) 0.0659(14) Uani 1 1 d . . . H9A H 0.0145 0.7650 0.2848 0.079 Uiso 1 1 calc R . . H9B H -0.0268 0.7868 0.3681 0.079 Uiso 1 1 calc R . . C10 C 0.1354(4) 0.6929(3) 0.3441(2) 0.0585(13) Uani 1 1 d . . . H10A H 0.1528 0.7020 0.3907 0.070 Uiso 1 1 calc R . . H10B H 0.1165 0.6387 0.3458 0.070 Uiso 1 1 calc R . . C11 C 0.2367(3) 0.6763(3) 0.2872(2) 0.0398(9) Uani 1 1 d . . . H11A H 0.2219 0.6607 0.2414 0.048 Uiso 1 1 calc R . . H11B H 0.2999 0.6241 0.2996 0.048 Uiso 1 1 calc R . . C12 C 0.2666(3) 0.7607(2) 0.27949(18) 0.0319(8) Uani 1 1 d . . . H12A H 0.2878 0.7727 0.3246 0.038 Uiso 1 1 calc R . . C13 C 0.4640(3) 0.7027(2) 0.22595(18) 0.0303(8) Uani 1 1 d . . . C14 C 0.5053(3) 0.6587(3) 0.29280(19) 0.0436(10) Uani 1 1 d . . . H14A H 0.4599 0.6261 0.3142 0.065 Uiso 1 1 calc R . . H14B H 0.5003 0.7058 0.3265 0.065 Uiso 1 1 calc R . . H14C H 0.5821 0.6159 0.2805 0.065 Uiso 1 1 calc R . . C15 C 0.3953(3) 0.9279(3) 0.2637(2) 0.0407(9) Uani 1 1 d . . . H15A H 0.4651 0.8794 0.2515 0.049 Uiso 1 1 calc R . . C16 C 0.3512(4) 0.9555(3) 0.3346(2) 0.0479(10) Uani 1 1 d . . . H16A H 0.3903 0.9247 0.3706 0.057 Uiso 1 1 calc R . . C17 C 0.2509(4) 1.0274(3) 0.3523(2) 0.0514(11) Uani 1 1 d . . . H17A H 0.2215 1.0455 0.4006 0.062 Uiso 1 1 calc R . . C18 C 0.1922(4) 1.0739(3) 0.3002(2) 0.0483(11) Uani 1 1 d . . . H18A H 0.1239 1.1238 0.3126 0.058 Uiso 1 1 calc R . . C19 C 0.2356(3) 1.0459(3) 0.2291(2) 0.0438(10) Uani 1 1 d . . . H19A H 0.1965 1.0773 0.1932 0.053 Uiso 1 1 calc R . . C20 C 0.3356(3) 0.9724(3) 0.2106(2) 0.0371(9) Uani 1 1 d . . . C21 C 0.7274(4) 0.6738(3) -0.0550(2) 0.0578(12) Uani 1 1 d . . . H21A H 0.7211 0.6178 -0.0629 0.069 Uiso 1 1 calc R . . C22 C 0.8304(4) 0.6793(4) -0.0709(3) 0.0815(18) Uani 1 1 d . . . H22A H 0.8934 0.6277 -0.0904 0.098 Uiso 1 1 calc R . . C23 C 0.8404(4) 0.7602(5) -0.0580(3) 0.0782(18) Uani 1 1 d . . . H23A H 0.9107 0.7637 -0.0679 0.094 Uiso 1 1 calc R . . C24 C 0.7505(5) 0.8347(4) -0.0313(3) 0.0756(16) Uani 1 1 d . . . H24A H 0.7583 0.8899 -0.0226 0.091 Uiso 1 1 calc R . . C25 C 0.6464(4) 0.8306(3) -0.0164(2) 0.0565(12) Uani 1 1 d . . . H25A H 0.5839 0.8833 0.0016 0.068 Uiso 1 1 calc R . . C26 C 0.6339(3) 0.7495(3) -0.02781(18) 0.0409(10) Uani 1 1 d . . . C27 C 0.0919(4) 0.9563(3) 0.1096(2) 0.0665(13) Uani 1 1 d . . . H27A H 0.0577 0.9363 0.1522 0.100 Uiso 1 1 calc R . . H27B H 0.0350 1.0045 0.0891 0.100 Uiso 1 1 calc R . . H27C H 0.1451 0.9794 0.1219 0.100 Uiso 1 1 calc R . . C28 C 0.2251(4) 0.9025(3) -0.0363(2) 0.0719(15) Uani 1 1 d . . . H28A H 0.2837 0.9193 -0.0248 0.108 Uiso 1 1 calc R . . H28B H 0.1675 0.9560 -0.0512 0.108 Uiso 1 1 calc R . . H28C H 0.2555 0.8556 -0.0747 0.108 Uiso 1 1 calc R . . C29 C 0.0512(4) 0.8270(3) 0.0198(3) 0.0813(17) Uani 1 1 d . . . H29A H 0.0189 0.8032 0.0610 0.122 Uiso 1 1 calc R . . H29B H 0.0815 0.7807 -0.0190 0.122 Uiso 1 1 calc R . . H29C H -0.0057 0.8812 0.0051 0.122 Uiso 1 1 calc R . . C30 C 0.3045(4) 0.6232(3) -0.0372(2) 0.0546(11) Uani 1 1 d . . . H30A H 0.2424 0.6645 -0.0580 0.082 Uiso 1 1 calc R . . H30B H 0.3113 0.5606 -0.0440 0.082 Uiso 1 1 calc R . . H30C H 0.3724 0.6291 -0.0602 0.082 Uiso 1 1 calc R . . C31 C 0.1562(3) 0.6293(3) 0.1020(2) 0.0519(11) Uani 1 1 d . . . H31A H 0.0910 0.6708 0.0841 0.078 Uiso 1 1 calc R . . H31B H 0.1450 0.6384 0.1534 0.078 Uiso 1 1 calc R . . H31C H 0.1683 0.5665 0.0901 0.078 Uiso 1 1 calc R . . C32 C 0.4032(3) 0.5702(2) 0.0957(2) 0.0438(10) Uani 1 1 d . . . H32A H 0.3945 0.5831 0.1464 0.066 Uiso 1 1 calc R . . H32B H 0.4703 0.5763 0.0713 0.066 Uiso 1 1 calc R . . H32C H 0.4086 0.5082 0.0877 0.066 Uiso 1 1 calc R . . C33 C 0.2164(3) 0.2935(2) 0.33176(19) 0.0339(8) Uani 1 1 d . . . H33A H 0.2522 0.2266 0.3327 0.041 Uiso 1 1 calc R . . H33B H 0.2017 0.3189 0.3807 0.041 Uiso 1 1 calc R . . C34 C 0.1068(3) 0.3194(3) 0.3045(2) 0.0446(10) Uani 1 1 d . . . H34A H 0.1208 0.2887 0.2576 0.053 Uiso 1 1 calc R . . H34B H 0.0572 0.2980 0.3372 0.053 Uiso 1 1 calc R . . C35 C 0.0503(3) 0.4219(3) 0.2982(2) 0.0468(10) Uani 1 1 d . . . H35A H 0.0286 0.4523 0.3458 0.056 Uiso 1 1 calc R . . H35B H -0.0172 0.4356 0.2777 0.056 Uiso 1 1 calc R . . C36 C 0.1277(3) 0.4588(3) 0.2511(2) 0.0424(9) Uani 1 1 d . . . H36A H 0.1417 0.4343 0.2020 0.051 Uiso 1 1 calc R . . H36B H 0.0917 0.5258 0.2510 0.051 Uiso 1 1 calc R . . C37 C 0.2375(3) 0.4322(2) 0.2780(2) 0.0355(9) Uani 1 1 d . . . H37A H 0.2871 0.4534 0.2450 0.043 Uiso 1 1 calc R . . H37B H 0.2240 0.4631 0.3247 0.043 Uiso 1 1 calc R . . C38 C 0.2946(3) 0.3295(2) 0.28467(18) 0.0304(8) Uani 1 1 d . . . H38A H 0.3135 0.2994 0.2365 0.036 Uiso 1 1 calc R . . C39 C 0.7021(3) 0.3538(3) 0.2707(2) 0.0397(9) Uani 1 1 d . . . H39A H 0.6565 0.4060 0.3040 0.048 Uiso 1 1 calc R . . H39B H 0.6774 0.3670 0.2244 0.048 Uiso 1 1 calc R . . C40 C 0.8240(3) 0.3402(3) 0.2627(2) 0.0501(11) Uani 1 1 d . . . H40A H 0.8331 0.3953 0.2436 0.060 Uiso 1 1 calc R . . H40B H 0.8468 0.3314 0.3097 0.060 Uiso 1 1 calc R . . C41 C 0.8977(3) 0.2582(3) 0.2135(2) 0.0587(13) Uani 1 1 d . . . H41A H 0.9756 0.2497 0.2109 0.070 Uiso 1 1 calc R . . H41B H 0.8794 0.2692 0.1654 0.070 Uiso 1 1 calc R . . C42 C 0.8822(3) 0.1722(3) 0.2401(3) 0.0635(13) Uani 1 1 d . . . H42A H 0.9086 0.1574 0.2858 0.076 Uiso 1 1 calc R . . H42B H 0.9269 0.1208 0.2059 0.076 Uiso 1 1 calc R . . C43 C 0.7607(3) 0.1848(3) 0.2498(3) 0.0534(11) Uani 1 1 d . . . H43A H 0.7367 0.1924 0.2032 0.064 Uiso 1 1 calc R . . H43B H 0.7526 0.1298 0.2701 0.064 Uiso 1 1 calc R . . C44 C 0.6877(3) 0.2675(2) 0.29850(17) 0.0292(8) Uani 1 1 d . . . H44A H 0.7171 0.2566 0.3439 0.035 Uiso 1 1 calc R . . C45 C 0.4922(3) 0.2999(2) 0.27679(17) 0.0284(8) Uani 1 1 d . . . C46 C 0.5107(3) 0.3134(3) 0.19767(18) 0.0404(9) Uani 1 1 d . . . H46A H 0.4745 0.3779 0.1889 0.061 Uiso 1 1 calc R . . H46B H 0.4797 0.2782 0.1734 0.061 Uiso 1 1 calc R . . H46C H 0.5898 0.2927 0.1798 0.061 Uiso 1 1 calc R . . C47 C 0.5201(4) 0.0811(3) 0.2604(2) 0.0515(11) Uani 1 1 d . . . H47A H 0.4463 0.1239 0.2645 0.062 Uiso 1 1 calc R . . C48 C 0.5793(5) 0.0408(4) 0.1943(2) 0.0647(14) Uani 1 1 d . . . H48A H 0.5458 0.0564 0.1534 0.078 Uiso 1 1 calc R . . C49 C 0.6869(6) -0.0219(4) 0.1886(3) 0.0762(18) Uani 1 1 d . . . H49A H 0.7269 -0.0483 0.1436 0.091 Uiso 1 1 calc R . . C50 C 0.7370(5) -0.0464(3) 0.2476(3) 0.0730(16) Uani 1 1 d . . . H50A H 0.8101 -0.0906 0.2432 0.088 Uiso 1 1 calc R . . C51 C 0.6794(4) -0.0057(3) 0.3138(2) 0.0527(11) Uani 1 1 d . . . H51A H 0.7141 -0.0210 0.3542 0.063 Uiso 1 1 calc R . . C52 C 0.5703(3) 0.0578(3) 0.32044(19) 0.0381(9) Uani 1 1 d . . . C53 C 0.8091(3) 0.2337(3) 0.46856(19) 0.0404(9) Uani 1 1 d . . . H53A H 0.7914 0.2965 0.4767 0.048 Uiso 1 1 calc R . . C54 C 0.9195(3) 0.1735(3) 0.4516(2) 0.0527(11) Uani 1 1 d . . . H54A H 0.9763 0.1959 0.4481 0.063 Uiso 1 1 calc R . . C55 C 0.9462(3) 0.0819(3) 0.4400(2) 0.0571(12) Uani 1 1 d . . . H55A H 1.0211 0.0417 0.4280 0.069 Uiso 1 1 calc R . . C56 C 0.8638(3) 0.0487(3) 0.4458(2) 0.0567(12) Uani 1 1 d . . . H56A H 0.8822 -0.0143 0.4379 0.068 Uiso 1 1 calc R . . C57 C 0.7532(3) 0.1082(3) 0.4634(2) 0.0418(9) Uani 1 1 d . . . H57A H 0.6972 0.0848 0.4685 0.050 Uiso 1 1 calc R . . C58 C 0.7242(3) 0.2009(3) 0.47359(17) 0.0320(8) Uani 1 1 d . . . C59 C 0.3855(3) 0.1875(3) 0.5913(2) 0.0502(11) Uani 1 1 d . . . H59A H 0.4231 0.2190 0.6133 0.075 Uiso 1 1 calc R . . H59B H 0.4390 0.1417 0.5561 0.075 Uiso 1 1 calc R . . H59C H 0.3520 0.1578 0.6276 0.075 Uiso 1 1 calc R . . C60 C 0.2056(4) 0.2087(3) 0.5055(2) 0.0524(12) Uani 1 1 d . . . H60A H 0.1475 0.2514 0.4822 0.079 Uiso 1 1 calc R . . H60B H 0.1732 0.1786 0.5421 0.079 Uiso 1 1 calc R . . H60C H 0.2598 0.1630 0.4705 0.079 Uiso 1 1 calc R . . C61 C 0.1683(4) 0.3482(3) 0.6194(2) 0.0579(13) Uani 1 1 d . . . H61A H 0.2005 0.3829 0.6431 0.087 Uiso 1 1 calc R . . H61B H 0.1430 0.3113 0.6537 0.087 Uiso 1 1 calc R . . H61C H 0.1059 0.3901 0.5992 0.087 Uiso 1 1 calc R . . C62 C 0.3259(3) 0.4857(3) 0.57831(18) 0.0380(9) Uani 1 1 d . . . H62A H 0.4036 0.4519 0.5814 0.057 Uiso 1 1 calc R . . H62B H 0.2796 0.4728 0.6187 0.057 Uiso 1 1 calc R . . H62C H 0.3100 0.5509 0.5788 0.057 Uiso 1 1 calc R . . C63 C 0.1449(3) 0.5176(3) 0.4898(2) 0.0387(9) Uani 1 1 d . . . H63A H 0.1270 0.5002 0.4463 0.058 Uiso 1 1 calc R . . H63B H 0.1303 0.5826 0.4904 0.058 Uiso 1 1 calc R . . H63C H 0.0995 0.5049 0.5308 0.058 Uiso 1 1 calc R . . C64 C 0.3811(3) 0.4870(2) 0.42120(18) 0.0320(8) Uani 1 1 d . . . H64A H 0.4594 0.4532 0.4229 0.048 Uiso 1 1 calc R . . H64B H 0.3630 0.5521 0.4278 0.048 Uiso 1 1 calc R . . H64C H 0.3655 0.4748 0.3753 0.048 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 Sn1 0.02400(13) 0.02964(15) 0.02317(13) -0.00090(10) -0.00302(10) -0.01027(11) Sn2 0.02309(13) 0.02435(13) 0.02139(12) -0.00226(9) -0.00027(9) -0.01050(11) S1 0.0586(7) 0.0377(6) 0.0400(6) -0.0005(4) 0.0029(5) -0.0267(6) S2 0.0363(6) 0.0744(8) 0.0251(5) -0.0076(5) 0.0014(4) -0.0267(6) S3 0.0498(6) 0.0302(5) 0.0342(5) -0.0048(4) 0.0054(4) -0.0210(5) S4 0.0285(5) 0.0361(6) 0.0308(5) -0.0107(4) -0.0067(4) -0.0052(4) Si1 0.0316(6) 0.0380(7) 0.0388(6) 0.0035(5) -0.0119(5) -0.0083(5) Si2 0.0324(6) 0.0332(6) 0.0341(6) -0.0053(4) -0.0042(4) -0.0143(5) Si3 0.0344(6) 0.0331(6) 0.0269(5) -0.0021(4) 0.0046(4) -0.0187(5) Si4 0.0241(5) 0.0264(5) 0.0264(5) -0.0031(4) -0.0028(4) -0.0090(4) N1 0.0230(15) 0.0287(17) 0.0250(15) 0.0005(12) -0.0014(12) -0.0059(13) N2 0.0249(16) 0.0343(18) 0.0255(16) -0.0081(12) -0.0027(13) -0.0018(14) N3 0.0251(15) 0.0312(17) 0.0295(16) 0.0000(12) -0.0067(12) -0.0122(14) N4 0.0234(15) 0.0361(18) 0.0254(15) -0.0012(12) -0.0022(12) -0.0137(14) N5 0.0242(16) 0.0414(19) 0.0233(15) 0.0017(12) -0.0012(12) -0.0162(14) N6 0.0255(15) 0.0258(16) 0.0231(14) -0.0004(11) 0.0007(12) -0.0106(13) C1 0.043(3) 0.039(3) 0.067(3) 0.003(2) -0.013(2) -0.019(2) C2 0.040(3) 0.064(3) 0.092(4) 0.008(3) -0.017(3) -0.030(3) C3 0.028(2) 0.082(4) 0.078(4) 0.014(3) -0.011(2) -0.013(3) C4 0.034(2) 0.049(3) 0.074(3) 0.001(2) -0.002(2) 0.000(2) C5 0.033(2) 0.043(3) 0.074(3) -0.012(2) -0.003(2) -0.011(2) C6 0.028(2) 0.047(3) 0.035(2) -0.0020(17) -0.0063(17) -0.0104(19) C7 0.032(2) 0.033(2) 0.048(2) -0.0010(17) 0.0094(18) -0.0114(18) C8 0.044(3) 0.049(3) 0.061(3) -0.011(2) 0.021(2) -0.015(2) C9 0.053(3) 0.060(3) 0.077(3) -0.011(2) 0.033(3) -0.029(3) C10 0.074(3) 0.054(3) 0.049(3) 0.003(2) 0.015(2) -0.036(3) C11 0.047(2) 0.031(2) 0.038(2) 0.0011(16) 0.0020(18) -0.016(2) C12 0.037(2) 0.034(2) 0.0228(18) -0.0010(14) 0.0003(15) -0.0133(18) C13 0.038(2) 0.028(2) 0.0269(19) -0.0013(14) -0.0113(16) -0.0129(17) C14 0.040(2) 0.058(3) 0.029(2) 0.0081(18) -0.0148(18) -0.012(2) C15 0.038(2) 0.037(2) 0.050(3) -0.0104(18) -0.0070(19) -0.0179(19) C16 0.050(3) 0.050(3) 0.047(3) -0.009(2) -0.014(2) -0.020(2) C17 0.057(3) 0.054(3) 0.047(3) -0.021(2) 0.001(2) -0.029(3) C18 0.045(3) 0.031(2) 0.065(3) -0.015(2) 0.000(2) -0.013(2) C19 0.046(3) 0.031(2) 0.056(3) -0.0015(18) -0.010(2) -0.017(2) C20 0.044(2) 0.030(2) 0.041(2) -0.0021(16) -0.0010(18) -0.021(2) C21 0.048(3) 0.073(4) 0.048(3) -0.021(2) 0.000(2) -0.020(3) C22 0.034(3) 0.141(6) 0.053(3) -0.035(3) 0.006(2) -0.020(3) C23 0.052(3) 0.144(6) 0.055(3) -0.012(3) 0.000(3) -0.058(4) C24 0.072(4) 0.094(5) 0.079(4) 0.015(3) -0.002(3) -0.057(4) C25 0.050(3) 0.059(3) 0.061(3) 0.016(2) -0.004(2) -0.025(3) C26 0.033(2) 0.064(3) 0.0240(19) 0.0012(18) -0.0007(16) -0.018(2) C27 0.069(3) 0.044(3) 0.062(3) -0.001(2) -0.022(3) 0.009(2) C28 0.069(3) 0.067(4) 0.060(3) 0.026(3) -0.012(3) -0.006(3) C29 0.055(3) 0.064(4) 0.131(5) 0.015(3) -0.058(3) -0.014(3) C30 0.055(3) 0.066(3) 0.043(3) -0.019(2) -0.008(2) -0.024(2) C31 0.050(3) 0.051(3) 0.064(3) 0.006(2) -0.006(2) -0.032(2) C32 0.047(3) 0.030(2) 0.051(3) -0.0053(18) -0.012(2) -0.011(2) C33 0.028(2) 0.035(2) 0.043(2) 0.0036(16) -0.0068(17) -0.0160(18) C34 0.033(2) 0.047(3) 0.063(3) 0.007(2) -0.016(2) -0.023(2) C35 0.031(2) 0.046(3) 0.066(3) 0.005(2) -0.017(2) -0.015(2) C36 0.039(2) 0.040(2) 0.049(2) 0.0076(18) -0.0174(19) -0.013(2) C37 0.031(2) 0.039(2) 0.041(2) 0.0041(17) -0.0097(17) -0.0156(18) C38 0.029(2) 0.041(2) 0.0271(19) 0.0035(15) -0.0088(15) -0.0189(18) C39 0.038(2) 0.039(2) 0.046(2) -0.0032(17) -0.0027(18) -0.0208(19) C40 0.044(3) 0.059(3) 0.060(3) 0.005(2) -0.005(2) -0.034(2) C41 0.037(2) 0.107(4) 0.042(3) 0.000(2) 0.002(2) -0.043(3) C42 0.033(2) 0.059(3) 0.083(4) -0.026(2) 0.009(2) -0.007(2) C43 0.034(2) 0.039(3) 0.082(3) -0.015(2) 0.007(2) -0.013(2) C44 0.0231(18) 0.041(2) 0.0263(18) -0.0014(15) -0.0005(14) -0.0163(17) C45 0.032(2) 0.032(2) 0.0250(18) -0.0014(14) -0.0037(15) -0.0174(17) C46 0.037(2) 0.065(3) 0.0251(19) 0.0041(17) -0.0046(16) -0.026(2) C47 0.065(3) 0.049(3) 0.048(3) -0.014(2) 0.000(2) -0.032(2) C48 0.105(5) 0.066(4) 0.040(3) -0.011(2) 0.000(3) -0.054(4) C49 0.114(5) 0.059(4) 0.057(3) -0.028(3) 0.038(3) -0.053(4) C50 0.079(4) 0.040(3) 0.084(4) -0.023(3) 0.035(3) -0.024(3) C51 0.060(3) 0.033(3) 0.060(3) -0.0105(19) 0.011(2) -0.019(2) C52 0.052(3) 0.029(2) 0.037(2) -0.0086(16) 0.0059(19) -0.026(2) C53 0.035(2) 0.048(3) 0.041(2) 0.0005(18) -0.0120(18) -0.017(2) C54 0.031(2) 0.074(4) 0.056(3) 0.005(2) -0.010(2) -0.023(2) C55 0.031(2) 0.069(4) 0.056(3) 0.001(2) -0.001(2) -0.006(2) C56 0.041(3) 0.038(3) 0.075(3) -0.005(2) -0.001(2) 0.000(2) C57 0.033(2) 0.039(3) 0.049(2) -0.0040(18) -0.0047(19) -0.0093(19) C58 0.0265(19) 0.039(2) 0.0256(19) 0.0010(15) -0.0057(15) -0.0072(17) C59 0.062(3) 0.050(3) 0.044(2) 0.014(2) -0.005(2) -0.030(2) C60 0.063(3) 0.066(3) 0.043(2) -0.008(2) 0.007(2) -0.047(3) C61 0.067(3) 0.058(3) 0.045(3) -0.004(2) 0.023(2) -0.033(3) C62 0.045(2) 0.037(2) 0.032(2) -0.0079(16) -0.0068(17) -0.0162(19) C63 0.027(2) 0.039(2) 0.044(2) 0.0035(17) -0.0030(17) -0.0076(18) C64 0.035(2) 0.027(2) 0.036(2) -0.0012(15) -0.0056(16) -0.0149(17) _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 Sn1 N3 2.070(2) . ? Sn1 N2 2.140(3) . ? Sn1 N1 2.213(2) . ? Sn1 S1 2.4158(10) . ? Sn1 S2 2.4854(10) . ? Sn1 C13 2.628(3) . ? Sn2 N6 2.077(3) . ? Sn2 N5 2.146(2) . ? Sn2 N4 2.225(3) . ? Sn2 S3 2.4249(9) . ? Sn2 S4 2.4939(9) . ? Sn2 C45 2.635(3) . ? S1 C20 1.781(4) . ? S2 C26 1.777(4) . ? S3 C52 1.786(4) . ? S4 C58 1.768(4) . ? Si1 N3 1.741(3) . ? Si1 C28 1.852(4) . ? Si1 C27 1.864(5) . ? Si1 C29 1.870(4) . ? Si2 N3 1.738(3) . ? Si2 C32 1.867(4) . ? Si2 C30 1.867(4) . ? Si2 C31 1.870(3) . ? Si3 N6 1.744(2) . ? Si3 C60 1.861(4) . ? Si3 C61 1.862(4) . ? Si3 C59 1.866(4) . ? Si4 N6 1.735(3) . ? Si4 C64 1.861(3) . ? Si4 C62 1.873(3) . ? Si4 C63 1.877(4) . ? N1 C13 1.303(4) . ? N1 C12 1.463(4) . ? N2 C13 1.336(4) . ? N2 C6 1.468(4) . ? N4 C45 1.310(4) . ? N4 C38 1.462(4) . ? N5 C45 1.333(4) . ? N5 C44 1.467(4) . ? C1 C6 1.506(5) . ? C1 C2 1.526(5) . ? C2 C3 1.482(6) . ? C3 C4 1.500(6) . ? C4 C5 1.535(5) . ? C5 C6 1.496(5) . ? C7 C12 1.509(5) . ? C7 C8 1.524(5) . ? C8 C9 1.513(5) . ? C9 C10 1.519(6) . ? C10 C11 1.515(5) . ? C11 C12 1.532(4) . ? C13 C14 1.516(4) . ? C15 C16 1.385(5) . ? C15 C20 1.394(5) . ? C16 C17 1.368(6) . ? C17 C18 1.382(6) . ? C18 C19 1.388(5) . ? C19 C20 1.379(5) . ? C21 C22 1.382(6) . ? C21 C26 1.379(6) . ? C22 C23 1.369(7) . ? C23 C24 1.343(7) . ? C24 C25 1.386(6) . ? C25 C26 1.384(6) . ? C33 C34 1.523(5) . ? C33 C38 1.525(4) . ? C34 C35 1.512(5) . ? C35 C36 1.526(5) . ? C36 C37 1.521(5) . ? C37 C38 1.518(5) . ? C39 C44 1.522(4) . ? C39 C40 1.524(5) . ? C40 C41 1.511(6) . ? C41 C42 1.517(6) . ? C42 C43 1.522(5) . ? C43 C44 1.513(5) . ? C45 C46 1.508(4) . ? C47 C52 1.388(5) . ? C47 C48 1.386(6) . ? C48 C49 1.373(7) . ? C49 C50 1.370(7) . ? C50 C51 1.386(6) . ? C51 C52 1.390(6) . ? C53 C54 1.388(5) . ? C53 C58 1.399(5) . ? C54 C55 1.367(6) . ? C55 C56 1.371(6) . ? C56 C57 1.389(5) . ? C57 C58 1.375(5) . ? 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 N3 Sn1 N2 135.18(11) . . ? N3 Sn1 N1 95.56(10) . . ? N2 Sn1 N1 60.05(10) . . ? N3 Sn1 S1 116.44(8) . . ? N2 Sn1 S1 106.28(8) . . ? N1 Sn1 S1 104.03(8) . . ? N3 Sn1 S2 88.81(8) . . ? N2 Sn1 S2 98.23(8) . . ? N1 Sn1 S2 152.35(8) . . ? S1 Sn1 S2 98.29(3) . . ? N3 Sn1 C13 118.25(10) . . ? N2 Sn1 C13 30.40(10) . . ? N1 Sn1 C13 29.68(10) . . ? S1 Sn1 C13 106.52(8) . . ? S2 Sn1 C13 127.18(9) . . ? N6 Sn2 N5 140.30(10) . . ? N6 Sn2 N4 96.95(10) . . ? N5 Sn2 N4 59.96(10) . . ? N6 Sn2 S3 109.37(7) . . ? N5 Sn2 S3 106.40(8) . . ? N4 Sn2 S3 99.93(7) . . ? N6 Sn2 S4 88.30(7) . . ? N5 Sn2 S4 96.63(7) . . ? N4 Sn2 S4 148.01(7) . . ? S3 Sn2 S4 108.05(3) . . ? N6 Sn2 C45 121.66(10) . . ? N5 Sn2 C45 30.24(10) . . ? N4 Sn2 C45 29.78(9) . . ? S3 Sn2 C45 103.79(8) . . ? S4 Sn2 C45 124.65(7) . . ? C20 S1 Sn1 105.61(11) . . ? C26 S2 Sn1 114.00(13) . . ? C52 S3 Sn2 104.17(11) . . ? C58 S4 Sn2 109.75(12) . . ? N3 Si1 C28 111.96(18) . . ? N3 Si1 C27 113.14(17) . . ? C28 Si1 C27 106.4(2) . . ? N3 Si1 C29 111.93(18) . . ? C28 Si1 C29 108.5(2) . . ? C27 Si1 C29 104.5(2) . . ? N3 Si2 C32 110.76(15) . . ? N3 Si2 C30 111.81(17) . . ? C32 Si2 C30 106.4(2) . . ? N3 Si2 C31 113.15(17) . . ? C32 Si2 C31 107.45(18) . . ? C30 Si2 C31 106.88(19) . . ? N6 Si3 C60 112.25(15) . . ? N6 Si3 C61 112.15(16) . . ? C60 Si3 C61 105.97(19) . . ? N6 Si3 C59 111.66(15) . . ? C60 Si3 C59 108.0(2) . . ? C61 Si3 C59 106.4(2) . . ? N6 Si4 C64 110.79(14) . . ? N6 Si4 C62 113.11(15) . . ? C64 Si4 C62 104.80(15) . . ? N6 Si4 C63 111.42(15) . . ? C64 Si4 C63 108.60(16) . . ? C62 Si4 C63 107.82(18) . . ? C13 N1 C12 124.8(3) . . ? C13 N1 Sn1 93.1(2) . . ? C12 N1 Sn1 142.1(2) . . ? C13 N2 C6 130.0(3) . . ? C13 N2 Sn1 95.4(2) . . ? C6 N2 Sn1 133.8(2) . . ? Si2 N3 Si1 121.65(15) . . ? Si2 N3 Sn1 116.18(15) . . ? Si1 N3 Sn1 119.88(14) . . ? C45 N4 C38 124.1(3) . . ? C45 N4 Sn2 92.7(2) . . ? C38 N4 Sn2 143.1(2) . . ? C45 N5 C44 130.0(3) . . ? C45 N5 Sn2 95.62(19) . . ? C44 N5 Sn2 134.3(2) . . ? Si4 N6 Si3 124.12(16) . . ? Si4 N6 Sn2 116.05(12) . . ? Si3 N6 Sn2 117.79(14) . . ? C6 C1 C2 110.6(4) . . ? C3 C2 C1 112.9(3) . . ? C2 C3 C4 112.7(4) . . ? C3 C4 C5 110.5(4) . . ? C6 C5 C4 110.4(3) . . ? N2 C6 C5 115.0(3) . . ? N2 C6 C1 113.7(3) . . ? C5 C6 C1 112.7(3) . . ? C12 C7 C8 112.6(3) . . ? C9 C8 C7 110.1(3) . . ? C8 C9 C10 110.4(4) . . ? C11 C10 C9 111.4(3) . . ? C10 C11 C12 111.6(3) . . ? N1 C12 C7 109.6(3) . . ? N1 C12 C11 111.6(3) . . ? C7 C12 C11 109.3(3) . . ? N1 C13 N2 111.3(3) . . ? N1 C13 C14 124.3(3) . . ? N2 C13 C14 124.3(3) . . ? N1 C13 Sn1 57.23(16) . . ? N2 C13 Sn1 54.19(17) . . ? C14 C13 Sn1 177.8(2) . . ? C16 C15 C20 119.5(4) . . ? C17 C16 C15 120.3(4) . . ? C16 C17 C18 120.8(4) . . ? C17 C18 C19 119.2(4) . . ? C20 C19 C18 120.6(4) . . ? C19 C20 C15 119.6(4) . . ? C19 C20 S1 119.3(3) . . ? C15 C20 S1 121.1(3) . . ? C22 C21 C26 120.9(5) . . ? C23 C22 C21 119.7(5) . . ? C24 C23 C22 120.4(5) . . ? C23 C24 C25 120.4(5) . . ? C26 C25 C24 120.5(5) . . ? C25 C26 C21 118.1(4) . . ? C25 C26 S2 122.3(3) . . ? C21 C26 S2 119.4(3) . . ? C34 C33 C38 111.4(3) . . ? C35 C34 C33 111.8(3) . . ? C34 C35 C36 110.9(3) . . ? C37 C36 C35 111.0(3) . . ? C38 C37 C36 112.6(3) . . ? N4 C38 C37 112.2(3) . . ? N4 C38 C33 109.3(3) . . ? C37 C38 C33 110.2(3) . . ? C44 C39 C40 109.8(3) . . ? C41 C40 C39 111.3(3) . . ? C40 C41 C42 110.7(3) . . ? C41 C42 C43 111.3(4) . . ? C44 C43 C42 111.1(3) . . ? N5 C44 C43 114.5(3) . . ? N5 C44 C39 113.7(3) . . ? C43 C44 C39 111.1(3) . . ? N4 C45 N5 111.5(3) . . ? N4 C45 C46 124.1(3) . . ? N5 C45 C46 124.4(3) . . ? N4 C45 Sn2 57.49(16) . . ? N5 C45 Sn2 54.14(15) . . ? C46 C45 Sn2 174.5(3) . . ? C52 C47 C48 119.6(5) . . ? C49 C48 C47 120.0(5) . . ? C50 C49 C48 121.0(4) . . ? C49 C50 C51 119.6(5) . . ? C50 C51 C52 120.0(5) . . ? C47 C52 C51 119.7(4) . . ? C47 C52 S3 121.7(3) . . ? C51 C52 S3 118.3(3) . . ? C54 C53 C58 120.0(4) . . ? C55 C54 C53 120.5(4) . . ? C54 C55 C56 120.0(4) . . ? C55 C56 C57 119.9(4) . . ? C58 C57 C56 121.1(3) . . ? C57 C58 C53 118.4(3) . . ? C57 C58 S4 122.4(3) . . ? C53 C58 S4 119.1(3) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.921 _refine_diff_density_min -1.465 _refine_diff_density_rms 0.139 data_dr135 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 Ge N4 Se2' _chemical_formula_weight 827.43 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' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 10.953(2) _cell_length_b 19.181(4) _cell_length_c 18.909(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.72(3) _cell_angle_gamma 90.00 _cell_volume 3959(1) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 2.645 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.25631 _exptl_absorpt_correction_T_max 0.98253 _exptl_absorpt_process_details 'psi-scans method by North' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3879 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 20.70 _reflns_number_total 3879 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku AFC6S' _computing_cell_refinement 'Rigaku AFC6S' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+34.1127P] 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 3879 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1997 _refine_ls_wR_factor_gt 0.1931 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.003 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 Se1 Se 0.22164(10) 0.21103(6) 1.10085(5) 0.0465(4) Uani 1 1 d . . . Se2 Se 0.03105(11) 0.31425(6) 0.97601(5) 0.0561(4) Uani 1 1 d . . . Ge Ge 0.24740(10) 0.27508(6) 0.98975(5) 0.0445(4) Uani 1 1 d . . . N1 N 0.2293(8) 0.1981(4) 0.9219(4) 0.041(2) Uani 1 1 d . . . N2 N 0.2454(8) 0.3033(4) 0.8821(4) 0.043(2) Uani 1 1 d . . . N3 N 0.4362(8) 0.2774(4) 0.9981(4) 0.043(2) Uani 1 1 d . . . N4 N 0.3238(9) 0.3607(4) 1.0315(4) 0.048(2) Uani 1 1 d . . . C1 C 0.2567(9) 0.0688(5) 0.9179(5) 0.046(3) Uani 1 1 d . . . H1A H 0.3331 0.0747 0.9491 0.055 Uiso 1 1 calc R . . H1B H 0.2784 0.0677 0.8682 0.055 Uiso 1 1 calc R . . C2 C 0.1945(10) 0.0002(6) 0.9358(6) 0.058(3) Uani 1 1 d . . . H2A H 0.2482 -0.0392 0.9248 0.070 Uiso 1 1 calc R . . H2B H 0.1838 -0.0010 0.9873 0.070 Uiso 1 1 calc R . . C3 C 0.0710(11) -0.0085(6) 0.8947(6) 0.063(3) Uani 1 1 d . . . H3A H 0.0828 -0.0144 0.8437 0.075 Uiso 1 1 calc R . . H3B H 0.0312 -0.0512 0.9111 0.075 Uiso 1 1 calc R . . C4 C -0.0108(10) 0.0526(5) 0.9039(5) 0.053(3) Uani 1 1 d . . . H4A H -0.0319 0.0546 0.9538 0.064 Uiso 1 1 calc R . . H4B H -0.0878 0.0466 0.8733 0.064 Uiso 1 1 calc R . . C5 C 0.0497(10) 0.1211(5) 0.8850(5) 0.049(3) Uani 1 1 d . . . H5A H 0.0629 0.1214 0.8339 0.059 Uiso 1 1 calc R . . H5B H -0.0049 0.1606 0.8945 0.059 Uiso 1 1 calc R . . C6 C 0.1709(9) 0.1299(5) 0.9281(5) 0.044(3) Uani 1 1 d . . . H6A H 0.1511 0.1269 0.9787 0.052 Uiso 1 1 calc R . . C7 C 0.3482(12) 0.4137(6) 0.8560(6) 0.067(3) Uani 1 1 d . . . H7A H 0.4292 0.3909 0.8640 0.080 Uiso 1 1 calc R . . H7B H 0.3268 0.4334 0.9017 0.080 Uiso 1 1 calc R . . C8 C 0.3561(13) 0.4719(6) 0.8028(6) 0.073(4) Uani 1 1 d . . . H8A H 0.4190 0.5059 0.8211 0.088 Uiso 1 1 calc R . . H8B H 0.3820 0.4525 0.7579 0.088 Uiso 1 1 calc R . . C9 C 0.2409(17) 0.5071(8) 0.7890(7) 0.098(5) Uani 1 1 d . . . H9A H 0.2488 0.5432 0.7522 0.117 Uiso 1 1 calc R . . H9B H 0.2192 0.5307 0.8328 0.117 Uiso 1 1 calc R . . C10 C 0.1393(14) 0.4567(11) 0.7640(10) 0.136(8) Uani 1 1 d . . . H10A H 0.1542 0.4386 0.7165 0.163 Uiso 1 1 calc R . . H10B H 0.0598 0.4816 0.7600 0.163 Uiso 1 1 calc R . . C11 C 0.1334(13) 0.3954(9) 0.8163(9) 0.116(7) Uani 1 1 d . . . H11A H 0.1054 0.4129 0.8615 0.139 Uiso 1 1 calc R . . H11B H 0.0725 0.3610 0.7964 0.139 Uiso 1 1 calc R . . C12 C 0.2537(10) 0.3601(5) 0.8309(5) 0.047(3) Uani 1 1 d . . . H12A H 0.2780 0.3397 0.7854 0.057 Uiso 1 1 calc R . . C13 C 0.2316(9) 0.2374(5) 0.8645(5) 0.045(3) Uani 1 1 d . . . C14 C 0.2255(12) 0.2108(6) 0.7889(5) 0.066(4) Uani 1 1 d . . . H14A H 0.2278 0.2503 0.7562 0.099 Uiso 1 1 calc R . . H14B H 0.1491 0.1847 0.7785 0.099 Uiso 1 1 calc R . . H14C H 0.2955 0.1801 0.7831 0.099 Uiso 1 1 calc R . . C15 C 0.5427(13) 0.1730(7) 0.9670(7) 0.075(4) Uani 1 1 d . . . H15A H 0.4731 0.1602 0.9328 0.090 Uiso 1 1 calc R . . H15B H 0.5269 0.1529 1.0137 0.090 Uiso 1 1 calc R . . C16 C 0.6623(11) 0.1401(6) 0.9421(7) 0.070(3) Uani 1 1 d . . . H16A H 0.7317 0.1488 0.9779 0.084 Uiso 1 1 calc R . . H16B H 0.6520 0.0890 0.9365 0.084 Uiso 1 1 calc R . . C17 C 0.6882(13) 0.1730(7) 0.8712(7) 0.079(4) Uani 1 1 d . . . H17A H 0.7648 0.1535 0.8550 0.095 Uiso 1 1 calc R . . H17B H 0.6205 0.1622 0.8349 0.095 Uiso 1 1 calc R . . C18 C 0.7007(15) 0.2513(9) 0.8799(8) 0.100(5) Uani 1 1 d . . . H18A H 0.7185 0.2730 0.8344 0.120 Uiso 1 1 calc R . . H18B H 0.7687 0.2624 0.9159 0.120 Uiso 1 1 calc R . . C19 C 0.5783(12) 0.2797(8) 0.9038(7) 0.088(5) Uani 1 1 d . . . H19A H 0.5841 0.3309 0.9096 0.105 Uiso 1 1 calc R . . H19B H 0.5115 0.2696 0.8667 0.105 Uiso 1 1 calc R . . C20 C 0.5480(12) 0.2469(7) 0.9732(6) 0.073(4) Uani 1 1 d . . . H20A H 0.6169 0.2583 1.0094 0.088 Uiso 1 1 calc R . . C21 C 0.2988(15) 0.4118(6) 1.1507(5) 0.081(4) Uani 1 1 d . . . H21A H 0.3885 0.4150 1.1623 0.097 Uiso 1 1 calc R . . H21B H 0.2720 0.3654 1.1664 0.097 Uiso 1 1 calc R . . C22 C 0.2370(16) 0.4674(7) 1.1919(6) 0.090(5) Uani 1 1 d . . . H22A H 0.1516 0.4524 1.1969 0.108 Uiso 1 1 calc R . . H22B H 0.2791 0.4697 1.2402 0.108 Uiso 1 1 calc R . . C23 C 0.2340(16) 0.5364(7) 1.1624(7) 0.092(5) Uani 1 1 d . . . H23A H 0.3137 0.5591 1.1757 0.110 Uiso 1 1 calc R . . H23B H 0.1702 0.5635 1.1844 0.110 Uiso 1 1 calc R . . C24 C 0.2091(12) 0.5405(6) 1.0835(6) 0.068(3) Uani 1 1 d . . . H24A H 0.2339 0.5872 1.0676 0.081 Uiso 1 1 calc R . . H24B H 0.1198 0.5359 1.0715 0.081 Uiso 1 1 calc R . . C25 C 0.2734(13) 0.4864(6) 1.0429(6) 0.070(4) Uani 1 1 d . . . H25A H 0.2339 0.4843 0.9940 0.084 Uiso 1 1 calc R . . H25B H 0.3593 0.5013 1.0399 0.084 Uiso 1 1 calc R . . C26 C 0.2732(14) 0.4168(6) 1.0735(5) 0.072(4) Uani 1 1 d . . . H26A H 0.1838 0.4054 1.0681 0.087 Uiso 1 1 calc R . . C27 C 0.4367(11) 0.3392(6) 1.0280(5) 0.051(3) Uani 1 1 d . . . C28 C 0.5514(12) 0.3784(7) 1.0558(7) 0.078(4) Uani 1 1 d . . . H28A H 0.5290 0.4253 1.0707 0.117 Uiso 1 1 calc R . . H28B H 0.6077 0.3818 1.0183 0.117 Uiso 1 1 calc R . . H28C H 0.5916 0.3532 1.0964 0.117 Uiso 1 1 calc R . . C29 C 0.4710(8) 0.1975(4) 1.1627(4) 0.062(3) Uani 1 1 d G . . H29A H 0.4643 0.2456 1.1740 0.074 Uiso 1 1 calc R . . C30 C 0.5768(6) 0.1609(6) 1.1848(4) 0.076(4) Uani 1 1 d G . . H30A H 0.6426 0.1840 1.2111 0.091 Uiso 1 1 calc R . . C31 C 0.5866(6) 0.0906(6) 1.1683(4) 0.089(5) Uani 1 1 d G . . H31A H 0.6590 0.0656 1.1834 0.107 Uiso 1 1 calc R . . C32 C 0.4904(9) 0.0569(4) 1.1298(4) 0.081(4) Uani 1 1 d G . . H32A H 0.4971 0.0089 1.1186 0.097 Uiso 1 1 calc R . . C33 C 0.3845(7) 0.0935(4) 1.1077(4) 0.062(3) Uani 1 1 d G . . H33A H 0.3188 0.0704 1.0814 0.074 Uiso 1 1 calc R . . C34 C 0.3748(5) 0.1638(4) 1.1242(3) 0.045(3) Uani 1 1 d G . . C35 C -0.0746(7) 0.2223(3) 1.0769(4) 0.056(3) Uani 1 1 d G . . H35A H -0.0685 0.1874 1.0416 0.067 Uiso 1 1 calc R . . C36 C -0.1191(8) 0.2053(3) 1.1414(4) 0.076(4) Uani 1 1 d G . . H36A H -0.1434 0.1588 1.1503 0.092 Uiso 1 1 calc R . . C37 C -0.1279(8) 0.2563(4) 1.1929(3) 0.077(4) Uani 1 1 d G . . H37A H -0.1583 0.2447 1.2371 0.092 Uiso 1 1 calc R . . C38 C -0.0923(7) 0.3244(3) 1.1799(3) 0.066(3) Uani 1 1 d G . . H38A H -0.0984 0.3592 1.2151 0.079 Uiso 1 1 calc R . . C39 C -0.0479(7) 0.3414(3) 1.1153(4) 0.053(3) Uani 1 1 d G . . H39A H -0.0235 0.3879 1.1064 0.064 Uiso 1 1 calc R . . C40 C -0.0390(6) 0.2904(3) 1.0638(3) 0.048(3) Uani 1 1 d G . . 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 Se1 0.0658(8) 0.0585(7) 0.0153(6) 0.0037(4) 0.0027(5) 0.0002(5) Se2 0.0673(8) 0.0730(9) 0.0269(7) 0.0014(5) -0.0026(5) 0.0092(6) Ge 0.0661(8) 0.0525(7) 0.0144(6) 0.0006(5) -0.0004(5) -0.0019(5) N1 0.066(6) 0.050(5) 0.007(4) 0.004(4) -0.001(4) -0.006(4) N2 0.068(6) 0.048(6) 0.012(4) 0.002(4) 0.000(4) 0.001(4) N3 0.070(6) 0.044(5) 0.016(4) 0.011(4) 0.005(4) -0.002(4) N4 0.073(7) 0.052(5) 0.017(4) -0.001(4) -0.007(4) -0.009(5) C1 0.063(7) 0.049(6) 0.026(5) 0.007(5) 0.003(5) 0.002(5) C2 0.073(8) 0.054(7) 0.047(7) -0.002(5) 0.003(6) -0.001(6) C3 0.095(9) 0.052(7) 0.042(7) -0.005(5) 0.008(6) -0.015(6) C4 0.068(7) 0.062(7) 0.029(6) -0.008(5) 0.003(5) -0.012(6) C5 0.065(7) 0.055(7) 0.026(5) -0.001(5) -0.005(5) 0.000(5) C6 0.066(7) 0.049(6) 0.017(5) -0.002(4) 0.004(5) 0.003(5) C7 0.096(9) 0.060(8) 0.041(7) 0.013(6) -0.017(6) -0.009(7) C8 0.118(11) 0.056(7) 0.041(7) 0.019(6) -0.017(7) -0.007(8) C9 0.154(16) 0.084(11) 0.060(9) 0.030(8) 0.038(10) 0.037(11) C10 0.080(10) 0.21(2) 0.121(15) 0.128(15) -0.002(10) 0.029(12) C11 0.079(10) 0.162(16) 0.104(12) 0.098(12) -0.014(9) 0.007(10) C12 0.080(8) 0.046(6) 0.015(5) 0.005(5) 0.001(5) 0.010(6) C13 0.064(7) 0.049(7) 0.020(6) -0.003(5) -0.001(5) -0.005(5) C14 0.108(10) 0.069(8) 0.022(6) -0.007(5) 0.013(6) -0.018(7) C15 0.100(10) 0.081(10) 0.049(8) 0.010(7) 0.027(7) 0.007(8) C16 0.072(8) 0.072(8) 0.070(9) 0.005(7) 0.017(7) 0.008(6) C17 0.090(10) 0.096(11) 0.054(8) -0.012(7) 0.030(7) -0.004(8) C18 0.107(12) 0.132(14) 0.064(10) 0.031(9) 0.025(8) 0.006(10) C19 0.081(9) 0.126(12) 0.060(9) 0.045(8) 0.037(7) 0.041(8) C20 0.079(9) 0.099(11) 0.046(7) 0.039(7) 0.031(7) 0.014(7) C21 0.160(14) 0.059(8) 0.024(6) 0.001(6) 0.014(7) 0.002(8) C22 0.175(15) 0.066(9) 0.031(7) -0.026(7) 0.017(8) -0.008(9) C23 0.163(15) 0.067(9) 0.047(8) -0.011(7) 0.022(8) 0.014(9) C24 0.099(9) 0.052(7) 0.050(7) -0.010(6) -0.005(6) 0.013(6) C25 0.113(10) 0.062(8) 0.037(7) 0.006(6) 0.013(6) 0.019(7) C26 0.127(11) 0.071(9) 0.019(6) -0.020(6) 0.005(6) -0.001(7) C27 0.066(8) 0.059(8) 0.024(6) 0.022(5) -0.014(5) -0.029(6) C28 0.081(9) 0.088(10) 0.061(8) 0.021(7) -0.011(7) -0.026(7) C29 0.072(8) 0.100(9) 0.015(6) 0.000(6) 0.010(6) -0.008(7) C30 0.056(8) 0.142(14) 0.028(7) 0.000(8) -0.003(6) -0.008(8) C31 0.087(11) 0.155(16) 0.027(7) 0.031(8) 0.007(7) 0.022(10) C32 0.111(11) 0.086(9) 0.047(8) 0.031(7) 0.017(8) 0.035(9) C33 0.084(9) 0.068(9) 0.034(6) 0.011(6) 0.003(6) 0.009(7) C34 0.057(7) 0.070(8) 0.009(5) 0.011(5) 0.003(5) 0.007(6) C35 0.058(7) 0.051(7) 0.062(8) -0.016(6) 0.024(6) -0.006(5) C36 0.094(10) 0.051(7) 0.090(10) -0.003(7) 0.044(8) -0.011(6) C37 0.093(10) 0.074(9) 0.067(9) -0.008(8) 0.031(7) -0.001(7) C38 0.080(8) 0.068(9) 0.050(8) -0.017(6) 0.012(6) 0.007(6) C39 0.074(8) 0.052(7) 0.035(7) -0.009(5) 0.011(6) 0.010(5) C40 0.050(6) 0.063(8) 0.030(6) -0.006(5) -0.007(5) 0.015(5) _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 Se1 C34 1.926(5) . ? Se1 Ge 2.4698(14) . ? Se2 C40 1.940(5) . ? Se2 Ge 2.4790(17) . ? Ge N1 1.955(7) . ? Ge N4 1.978(8) . ? Ge N3 2.062(9) . ? Ge N2 2.105(7) . ? Ge C27 2.467(10) . ? Ge C13 2.468(9) . ? N1 C13 1.322(12) . ? N1 C6 1.466(12) . ? N2 C13 1.313(12) . ? N2 C12 1.465(12) . ? N3 C27 1.313(14) . ? N3 C20 1.468(14) . ? N4 C27 1.310(14) . ? N4 C26 1.472(14) . ? C1 C6 1.525(14) . ? C1 C2 1.531(14) . ? C2 C3 1.513(16) . ? C3 C4 1.495(15) . ? C4 C5 1.527(14) . ? C5 C6 1.508(14) . ? C7 C12 1.508(15) . ? C7 C8 1.509(15) . ? C8 C9 1.436(19) . ? C9 C10 1.52(2) . ? C10 C11 1.541(19) . ? C11 C12 1.486(17) . ? C13 C14 1.515(14) . ? C15 C20 1.424(18) . ? C15 C16 1.561(16) . ? C16 C17 1.531(17) . ? C17 C18 1.52(2) . ? C18 C19 1.548(18) . ? C19 C20 1.516(15) . ? C21 C26 1.466(15) . ? C21 C22 1.513(17) . ? C22 C23 1.436(18) . ? C23 C24 1.496(16) . ? C24 C25 1.499(15) . ? C25 C26 1.455(16) . ? C27 C28 1.520(15) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 Se1 Ge 105.7(2) . . ? C40 Se2 Ge 106.3(2) . . ? N1 Ge N4 154.9(4) . . ? N1 Ge N3 96.5(3) . . ? N4 Ge N3 64.1(4) . . ? N1 Ge N2 64.4(3) . . ? N4 Ge N2 98.2(3) . . ? N3 Ge N2 89.9(3) . . ? N1 Ge C27 127.3(4) . . ? N4 Ge C27 31.9(4) . . ? N3 Ge C27 32.1(4) . . ? N2 Ge C27 95.5(3) . . ? N1 Ge C13 32.2(3) . . ? N4 Ge C13 128.3(3) . . ? N3 Ge C13 94.0(3) . . ? N2 Ge C13 32.1(3) . . ? C27 Ge C13 114.7(4) . . ? N1 Ge Se1 99.8(2) . . ? N4 Ge Se1 98.5(2) . . ? N3 Ge Se1 97.5(2) . . ? N2 Ge Se1 163.3(2) . . ? C27 Ge Se1 98.7(2) . . ? C13 Ge Se1 131.8(2) . . ? N1 Ge Se2 96.6(2) . . ? N4 Ge Se2 99.2(3) . . ? N3 Ge Se2 161.0(2) . . ? N2 Ge Se2 83.5(2) . . ? C27 Ge Se2 130.7(3) . . ? C13 Ge Se2 89.8(2) . . ? Se1 Ge Se2 93.71(6) . . ? C13 N1 C6 127.8(8) . . ? C13 N1 Ge 95.8(6) . . ? C6 N1 Ge 130.0(6) . . ? C13 N2 C12 124.1(8) . . ? C13 N2 Ge 89.3(6) . . ? C12 N2 Ge 146.6(6) . . ? C27 N3 C20 121.6(10) . . ? C27 N3 Ge 91.2(7) . . ? C20 N3 Ge 145.5(8) . . ? C27 N4 C26 131.0(10) . . ? C27 N4 Ge 95.0(7) . . ? C26 N4 Ge 131.0(8) . . ? C6 C1 C2 110.0(8) . . ? C3 C2 C1 112.2(9) . . ? C4 C3 C2 111.8(9) . . ? C3 C4 C5 111.9(9) . . ? C6 C5 C4 110.5(8) . . ? N1 C6 C5 115.3(8) . . ? N1 C6 C1 113.5(8) . . ? C5 C6 C1 111.7(8) . . ? C12 C7 C8 111.7(9) . . ? C9 C8 C7 111.8(12) . . ? C8 C9 C10 111.5(13) . . ? C9 C10 C11 110.8(13) . . ? C12 C11 C10 112.6(12) . . ? N2 C12 C11 111.1(9) . . ? N2 C12 C7 112.1(8) . . ? C11 C12 C7 108.8(11) . . ? N2 C13 N1 110.5(8) . . ? N2 C13 C14 124.0(9) . . ? N1 C13 C14 125.4(9) . . ? N2 C13 Ge 58.5(5) . . ? N1 C13 Ge 52.0(5) . . ? C14 C13 Ge 177.0(8) . . ? C20 C15 C16 113.5(11) . . ? C17 C16 C15 108.5(10) . . ? C18 C17 C16 109.6(10) . . ? C17 C18 C19 107.9(13) . . ? C20 C19 C18 111.3(10) . . ? C15 C20 N3 113.2(10) . . ? C15 C20 C19 110.6(12) . . ? N3 C20 C19 111.1(9) . . ? C26 C21 C22 114.2(11) . . ? C23 C22 C21 116.5(11) . . ? C22 C23 C24 115.7(11) . . ? C23 C24 C25 114.8(10) . . ? C26 C25 C24 114.6(10) . . ? C25 C26 N4 116.3(9) . . ? C25 C26 C21 116.7(10) . . ? N4 C26 C21 116.1(10) . . ? N4 C27 N3 109.6(9) . . ? N4 C27 C28 125.7(12) . . ? N3 C27 C28 124.6(12) . . ? N4 C27 Ge 53.0(5) . . ? N3 C27 Ge 56.7(5) . . ? C28 C27 Ge 176.8(8) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 Se1 119.1(5) . . ? C29 C34 Se1 120.6(5) . . ? C36 C35 C40 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 Se2 119.3(4) . . ? C35 C40 Se2 120.7(4) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 20.70 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.924 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.131