# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Liddle, Stephen' 'Patel, Dipti' 'King, David' 'Gardner, Benedict' 'McMaster, Jonathan' 'Lewis, William' 'Blake, Alexander' _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_address ; University Park Nottingham Nottinghamshire United Kingdom NG7 2RD ; _publ_contact_author_email stephen.liddle@nottingham.ac.uk # Attachment '4.cif.txt' data_udpsih _database_code_depnum_ccdc_archive 'CCDC 777012' #TrackingRef '4.cif.txt' _refine_special_details ; The lattice iso-hexane molecule is poorly defined and was refined isotropically with constraints and restraints to ensure chemically sensible bond lengths. The THF molecules required restraints and constraints to obtain chemically sensible geometries and bond lengths. Anti-bumping restraints were employed to prevent spurious close approach of two methyl hydrogens. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H64 N3 O Re Si3 U, 0.5(C6 H14)' _chemical_formula_sum 'C48 H71 N3 O Re Si3 U' _chemical_formula_weight 1214.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 '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 17.0448(4) _cell_length_b 18.6938(4) _cell_length_c 19.3062(5) _cell_angle_alpha 63.838(3) _cell_angle_beta 89.402(2) _cell_angle_gamma 63.080(2) _cell_volume 4783.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 34304 _cell_measurement_theta_min 3.4478 _cell_measurement_theta_max 74.1301 _exptl_crystal_description Rod _exptl_crystal_colour Red _exptl_crystal_size_max 0.2935 _exptl_crystal_size_mid 0.0693 _exptl_crystal_size_min 0.0268 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 15.327 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.111 _exptl_absorpt_correction_T_max 0.706 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3613 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% 0 _diffrn_reflns_number 67044 _diffrn_reflns_av_R_equivalents 0.100 _diffrn_reflns_av_sigmaI/netI 0.062 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 67.50 _reflns_number_total 17172 _reflns_number_gt 13603 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution Direct _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ' ? ' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+248.31P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17172 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 1030 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.168 _refine_ls_wR_factor_gt 0.156 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.10 _refine_ls_shift/su_max 0.005 _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 U1 U 0.33992(3) 0.31975(3) 0.14998(3) 0.02156(12) Uani 1 1 d U . . Re1 Re 0.46040(5) 0.21353(4) 0.31317(4) 0.02299(15) Uani 1 1 d U . . Si1 Si 0.2932(3) 0.5064(3) -0.0278(2) 0.0236(8) Uani 1 1 d U . . Si2 Si 0.4178(3) 0.3076(3) -0.0102(2) 0.0267(9) Uani 1 1 d U . . Si3 Si 0.2105(3) 0.3824(3) -0.0218(2) 0.0257(8) Uani 1 1 d U . . N1 N 0.2835(8) 0.4723(8) 0.0696(7) 0.023(2) Uani 1 1 d U . . N2 N 0.4517(8) 0.2665(8) 0.0921(7) 0.023(2) Uani 1 1 d U . . N3 N 0.2458(9) 0.3053(9) 0.0799(8) 0.027(2) Uani 1 1 d U . . C1 C 0.3034(10) 0.4133(9) -0.0477(9) 0.024(2) Uani 1 1 d U . . H1 H 0.2922 0.4415 -0.1069 0.028 Uiso 1 1 calc R . . C2 C 0.3927(12) 0.5227(13) -0.0396(10) 0.037(4) Uani 1 1 d U . . H2C H 0.3825 0.5743 -0.0316 0.056 Uiso 1 1 calc R . . H2B H 0.4018 0.5360 -0.0932 0.056 Uiso 1 1 calc R . . H2A H 0.4466 0.4666 -0.0003 0.056 Uiso 1 1 calc R . . C3 C 0.1957(11) 0.6210(10) -0.0976(10) 0.033(3) Uani 1 1 d U . . H3C H 0.1878 0.6650 -0.0798 0.049 Uiso 1 1 calc R . . H3A H 0.1407 0.6166 -0.0988 0.049 Uiso 1 1 calc R . . H3B H 0.2071 0.6419 -0.1509 0.049 Uiso 1 1 calc R . . C4 C 0.2431(10) 0.5466(10) 0.0887(9) 0.026(2) Uani 1 1 d U . . C5 C 0.2960(10) 0.5728(9) 0.1152(8) 0.025(2) Uani 1 1 d U . . H5 H 0.3594 0.5426 0.1194 0.030 Uiso 1 1 calc R . . C6 C 0.2572(11) 0.6435(11) 0.1361(10) 0.030(2) Uani 1 1 d U . . C7 C 0.3186(12) 0.6644(12) 0.1661(11) 0.038(3) Uani 1 1 d U . . H7C H 0.2936 0.7312 0.1394 0.057 Uiso 1 1 calc R . . H7A H 0.3781 0.6355 0.1554 0.057 Uiso 1 1 calc R . . H7B H 0.3251 0.6406 0.2235 0.057 Uiso 1 1 calc R . . C8 C 0.1658(11) 0.6873(11) 0.1265(10) 0.032(3) Uani 1 1 d U . . H8 H 0.1394 0.7343 0.1406 0.038 Uiso 1 1 calc R . . C9 C 0.1092(11) 0.6676(11) 0.0974(10) 0.029(2) Uani 1 1 d U . . C10 C 0.0085(11) 0.7212(12) 0.0844(11) 0.040(3) Uani 1 1 d U . . H10A H -0.0206 0.7122 0.0478 0.060 Uiso 1 1 calc R . . H10C H -0.0113 0.7867 0.0615 0.060 Uiso 1 1 calc R . . H10B H -0.0084 0.6997 0.1352 0.060 Uiso 1 1 calc R . . C11 C 0.1498(10) 0.5967(10) 0.0784(9) 0.027(3) Uani 1 1 d U . . H11 H 0.1122 0.5822 0.0578 0.032 Uiso 1 1 calc R . . C12 C 0.5030(11) 0.3304(12) -0.0648(10) 0.035(4) Uani 1 1 d U . . H12C H 0.5093 0.3770 -0.0587 0.053 Uiso 1 1 calc R . . H12A H 0.4824 0.3527 -0.1213 0.053 Uiso 1 1 calc R . . H12B H 0.5616 0.2734 -0.0430 0.053 Uiso 1 1 calc R . . C13 C 0.4197(12) 0.2164(11) -0.0292(10) 0.038(4) Uani 1 1 d U . . H13A H 0.3807 0.1947 0.0001 0.056 Uiso 1 1 calc R . . H13C H 0.4818 0.1648 -0.0113 0.056 Uiso 1 1 calc R . . H13B H 0.3976 0.2423 -0.0862 0.056 Uiso 1 1 calc R . . C14 C 0.5426(10) 0.1937(10) 0.1276(9) 0.025(2) Uani 1 1 d U . . C15 C 0.6114(10) 0.2123(11) 0.1320(9) 0.027(3) Uani 1 1 d U . . H15 H 0.5981 0.2744 0.1081 0.033 Uiso 1 1 calc R . . C16 C 0.7006(11) 0.1411(12) 0.1710(10) 0.033(3) Uani 1 1 d U . . C17 C 0.7756(11) 0.1621(13) 0.1771(12) 0.040(3) Uani 1 1 d U . . H17B H 0.7499 0.2222 0.1743 0.060 Uiso 1 1 calc R . . H17A H 0.8052 0.1630 0.1331 0.060 Uiso 1 1 calc R . . H17C H 0.8202 0.1146 0.2277 0.060 Uiso 1 1 calc R . . C18 C 0.7195(12) 0.0490(12) 0.2062(10) 0.036(3) Uani 1 1 d U . . H18 H 0.7792 0.0003 0.2354 0.043 Uiso 1 1 calc R . . C19 C 0.6533(12) 0.0288(11) 0.1990(10) 0.035(3) Uani 1 1 d U . . C20 C 0.6736(14) -0.0696(12) 0.2358(12) 0.049(4) Uani 1 1 d U . . H20C H 0.7114 -0.1049 0.2898 0.074 Uiso 1 1 calc R . . H20B H 0.7058 -0.0968 0.2038 0.074 Uiso 1 1 calc R . . H20A H 0.6167 -0.0708 0.2377 0.074 Uiso 1 1 calc R . . C21 C 0.5656(11) 0.1024(11) 0.1589(9) 0.032(3) Uani 1 1 d U . . H21 H 0.5193 0.0892 0.1527 0.038 Uiso 1 1 calc R . . C22 C 0.0961(11) 0.4859(11) -0.0481(9) 0.031(3) Uani 1 1 d U . . H22A H 0.0533 0.4656 -0.0257 0.046 Uiso 1 1 calc R . . H22B H 0.0744 0.5233 -0.1060 0.046 Uiso 1 1 calc R . . H22C H 0.1009 0.5225 -0.0262 0.046 Uiso 1 1 calc R . . C23 C 0.1920(12) 0.3332(11) -0.0809(10) 0.033(3) Uani 1 1 d U . . H23A H 0.1408 0.3227 -0.0693 0.050 Uiso 1 1 calc R . . H23B H 0.2466 0.2746 -0.0671 0.050 Uiso 1 1 calc R . . H23C H 0.1787 0.3762 -0.1376 0.050 Uiso 1 1 calc R . . C24 C 0.2286(11) 0.2303(11) 0.1107(9) 0.028(2) Uani 1 1 d U . . C25 C 0.2998(11) 0.1422(11) 0.1371(9) 0.029(3) Uani 1 1 d U . . H25 H 0.3586 0.1336 0.1327 0.034 Uiso 1 1 calc R . . C26 C 0.2883(12) 0.0657(11) 0.1699(10) 0.034(3) Uani 1 1 d U . . C27 C 0.3680(12) -0.0271(11) 0.1978(11) 0.040(4) Uani 1 1 d U . . H27A H 0.3549 -0.0584 0.1740 0.059 Uiso 1 1 calc R . . H27B H 0.3811 -0.0630 0.2558 0.059 Uiso 1 1 calc R . . H27C H 0.4205 -0.0213 0.1821 0.059 Uiso 1 1 calc R . . C28 C 0.2024(12) 0.0805(12) 0.1720(10) 0.034(3) Uani 1 1 d U . . H28 H 0.1936 0.0289 0.1938 0.041 Uiso 1 1 calc R . . C29 C 0.1289(11) 0.1659(11) 0.1441(10) 0.030(3) Uani 1 1 d U . . C30 C 0.0335(11) 0.1813(12) 0.1457(11) 0.035(3) Uani 1 1 d U . . H30B H 0.0365 0.1231 0.1826 0.052 Uiso 1 1 calc R . . H30A H 0.0011 0.2041 0.0923 0.052 Uiso 1 1 calc R . . H30C H 0.0015 0.2267 0.1631 0.052 Uiso 1 1 calc R . . C31 C 0.1412(11) 0.2431(11) 0.1143(9) 0.029(3) Uani 1 1 d U . . H31 H 0.0910 0.3029 0.0969 0.035 Uiso 1 1 calc R . . O1 O 0.2111(6) 0.3738(9) 0.2140(7) 0.041(2) Uani 1 1 d DU . . C32 C 0.2157(8) 0.3955(16) 0.2774(10) 0.056(4) Uani 1 1 d DU . . H32A H 0.2320 0.4443 0.2602 0.068 Uiso 1 1 calc R . . H32B H 0.2618 0.3402 0.3254 0.068 Uiso 1 1 calc R . . C33 C 0.1231(8) 0.4278(14) 0.2944(8) 0.051(4) Uani 1 1 d DU . . H33B H 0.1082 0.4757 0.3097 0.061 Uiso 1 1 calc R . . H33A H 0.1192 0.3760 0.3375 0.061 Uiso 1 1 calc R . . C34 C 0.0606(7) 0.4667(11) 0.2163(9) 0.042(3) Uani 1 1 d DU . . H34A H 0.0062 0.4603 0.2255 0.050 Uiso 1 1 calc R . . H34B H 0.0411 0.5325 0.1816 0.050 Uiso 1 1 calc R . . C35 C 0.1169(7) 0.4098(12) 0.1797(9) 0.040(3) Uani 1 1 d DU . . H35A H 0.1050 0.3588 0.1921 0.048 Uiso 1 1 calc R . . H35B H 0.1025 0.4483 0.1213 0.048 Uiso 1 1 calc R . . C36 C 0.4966(12) 0.0777(11) 0.4121(9) 0.033(3) Uani 1 1 d U . . H36 H 0.5409 0.0455 0.4637 0.040 Uiso 1 1 calc R . . C37 C 0.4026(12) 0.1336(12) 0.3976(10) 0.037(3) Uani 1 1 d U . . H37 H 0.3690 0.1486 0.4364 0.045 Uiso 1 1 calc R . . C38 C 0.3632(12) 0.1643(13) 0.3176(10) 0.038(3) Uani 1 1 d U . . H38 H 0.2972 0.2034 0.2909 0.046 Uiso 1 1 calc R . . C39 C 0.4367(11) 0.1192(11) 0.2853(9) 0.031(2) Uani 1 1 d U . . H39 H 0.4310 0.1216 0.2327 0.038 Uiso 1 1 calc R . . C40 C 0.5178(12) 0.0693(11) 0.3456(9) 0.033(2) Uani 1 1 d U . . H40 H 0.5797 0.0297 0.3422 0.040 Uiso 1 1 calc R . . C41 C 0.4884(11) 0.3216(10) 0.2282(9) 0.028(2) Uani 1 1 d U . . H41 H 0.4809 0.3432 0.1699 0.033 Uiso 1 1 calc R . . C42 C 0.5676(11) 0.2509(11) 0.2857(9) 0.030(2) Uani 1 1 d U . . H42 H 0.6264 0.2143 0.2758 0.037 Uiso 1 1 calc R . . C43 C 0.5523(11) 0.2438(10) 0.3615(9) 0.029(2) Uani 1 1 d U . . H43 H 0.5986 0.2015 0.4133 0.035 Uiso 1 1 calc R . . C44 C 0.4607(12) 0.3124(11) 0.3486(10) 0.034(2) Uani 1 1 d U . . H44 H 0.4315 0.3263 0.3897 0.041 Uiso 1 1 calc R . . C45 C 0.4206(9) 0.3624(9) 0.2642(8) 0.031(2) Uani 1 1 d U . . H45 H 0.3585 0.4168 0.2361 0.037 Uiso 1 1 calc R . . U2 U 0.17336(3) 0.69795(3) -0.48496(3) 0.01789(12) Uani 1 1 d U . . Re2 Re 0.08378(5) 0.74912(4) -0.36926(4) 0.02178(15) Uani 1 1 d U . . Si4 Si 0.0665(3) 0.7919(3) -0.6739(2) 0.0214(8) Uani 1 1 d U . . Si5 Si 0.2032(3) 0.5757(3) -0.5785(2) 0.0235(8) Uani 1 1 d U . . Si6 Si 0.2767(3) 0.7190(3) -0.6347(2) 0.0233(8) Uani 1 1 d U . . N4 N 0.0428(8) 0.7735(7) -0.5802(7) 0.0195(19) Uani 1 1 d U . . N5 N 0.2220(8) 0.5624(8) -0.4848(7) 0.024(2) Uani 1 1 d U . . N6 N 0.2520(8) 0.7591(8) -0.5662(7) 0.0217(19) Uani 1 1 d U . . C46 C 0.1838(10) 0.6937(10) -0.6508(9) 0.024(2) Uani 1 1 d U . . H46 H 0.1877 0.6925 -0.7020 0.029 Uiso 1 1 calc R . . C47 C 0.0529(10) 0.9099(9) -0.7327(9) 0.025(3) Uani 1 1 d U . . H47A H -0.0064 0.9559 -0.7336 0.037 Uiso 1 1 calc R . . H47C H 0.0571 0.9228 -0.7872 0.037 Uiso 1 1 calc R . . H47B H 0.1007 0.9126 -0.7081 0.037 Uiso 1 1 calc R . . C48 C -0.0163(10) 0.7942(11) -0.7374(9) 0.027(3) Uani 1 1 d U . . H48A H -0.0122 0.7339 -0.7128 0.041 Uiso 1 1 calc R . . H48C H -0.0028 0.8088 -0.7899 0.041 Uiso 1 1 calc R . . H48B H -0.0776 0.8412 -0.7432 0.041 Uiso 1 1 calc R . . C49 C -0.0456(9) 0.8113(9) -0.5764(7) 0.022(2) Uani 1 1 d U . . C50 C -0.0915(9) 0.7614(10) -0.5616(8) 0.023(2) Uani 1 1 d U . . H50 H -0.0603 0.7021 -0.5573 0.027 Uiso 1 1 calc R . . C51 C -0.1804(10) 0.7946(10) -0.5530(9) 0.025(2) Uani 1 1 d U . . C52 C -0.2257(11) 0.7358(11) -0.5361(10) 0.030(3) Uani 1 1 d U . . H52B H -0.2137 0.7093 -0.5716 0.045 Uiso 1 1 calc R . . H52C H -0.2912 0.7744 -0.5452 0.045 Uiso 1 1 calc R . . H52A H -0.2012 0.6863 -0.4808 0.045 Uiso 1 1 calc R . . C53 C -0.2257(10) 0.8807(10) -0.5591(9) 0.027(2) Uani 1 1 d U . . H53 H -0.2858 0.9034 -0.5519 0.032 Uiso 1 1 calc R . . C54 C -0.1860(10) 0.9347(10) -0.5753(9) 0.026(2) Uani 1 1 d U . . C55 C -0.2382(11) 1.0289(10) -0.5849(10) 0.031(3) Uani 1 1 d U . . H55A H -0.3013 1.0447 -0.5841 0.047 Uiso 1 1 calc R . . H55C H -0.2361 1.0733 -0.6357 0.047 Uiso 1 1 calc R . . H55B H -0.2116 1.0306 -0.5413 0.047 Uiso 1 1 calc R . . C56 C -0.0979(10) 0.9013(9) -0.5845(9) 0.022(2) Uani 1 1 d U . . H56 H -0.0713 0.9391 -0.5966 0.026 Uiso 1 1 calc R . . C57 C 0.2985(11) 0.4830(11) -0.5892(10) 0.033(4) Uani 1 1 d U . . H57C H 0.3543 0.4842 -0.5802 0.050 Uiso 1 1 calc R . . H57B H 0.2855 0.4926 -0.6429 0.050 Uiso 1 1 calc R . . H57A H 0.3062 0.4232 -0.5502 0.050 Uiso 1 1 calc R . . C58 C 0.1039(11) 0.5612(11) -0.5977(10) 0.030(3) Uani 1 1 d U . . H58A H 0.1240 0.4956 -0.5739 0.046 Uiso 1 1 calc R . . H58C H 0.0802 0.5914 -0.6551 0.046 Uiso 1 1 calc R . . H58B H 0.0563 0.5891 -0.5740 0.046 Uiso 1 1 calc R . . C59 C 0.2492(10) 0.4759(10) -0.4169(9) 0.024(2) Uani 1 1 d U . . C60 C 0.1877(11) 0.4478(10) -0.3886(10) 0.029(3) Uani 1 1 d U . . H60 H 0.1259 0.4860 -0.4168 0.034 Uiso 1 1 calc R . . C61 C 0.2144(11) 0.3640(10) -0.3190(10) 0.029(3) Uani 1 1 d U . . C62 C 0.1443(11) 0.3360(11) -0.2889(11) 0.034(3) Uani 1 1 d U . . H62C H 0.0849 0.3913 -0.3058 0.051 Uiso 1 1 calc R . . H62A H 0.1618 0.3000 -0.2308 0.051 Uiso 1 1 calc R . . H62B H 0.1411 0.2988 -0.3108 0.051 Uiso 1 1 calc R . . C63 C 0.3056(11) 0.3078(11) -0.2782(10) 0.031(3) Uani 1 1 d U . . H63 H 0.3244 0.2508 -0.2313 0.038 Uiso 1 1 calc R . . C64 C 0.3693(11) 0.3345(11) -0.3058(10) 0.030(3) Uani 1 1 d U . . C65 C 0.4664(11) 0.2731(11) -0.2629(11) 0.036(3) Uani 1 1 d U . . H65C H 0.4907 0.3093 -0.2574 0.054 Uiso 1 1 calc R . . H65B H 0.5005 0.2437 -0.2929 0.054 Uiso 1 1 calc R . . H65A H 0.4721 0.2257 -0.2101 0.054 Uiso 1 1 calc R . . C66 C 0.3417(10) 0.4162(9) -0.3740(9) 0.023(2) Uani 1 1 d U . . H66 H 0.3853 0.4336 -0.3933 0.027 Uiso 1 1 calc R . . C67 C 0.3914(10) 0.6146(11) -0.6013(10) 0.030(3) Uani 1 1 d U . . H67C H 0.4379 0.6325 -0.6065 0.045 Uiso 1 1 calc R . . H67B H 0.3952 0.5861 -0.6343 0.045 Uiso 1 1 calc R . . H67A H 0.4010 0.5705 -0.5457 0.045 Uiso 1 1 calc R . . C68 C 0.2766(10) 0.8077(10) -0.7305(9) 0.026(3) Uani 1 1 d U . . H68C H 0.2933 0.8467 -0.7206 0.039 Uiso 1 1 calc R . . H68A H 0.2160 0.8457 -0.7658 0.039 Uiso 1 1 calc R . . H68B H 0.3204 0.7775 -0.7555 0.039 Uiso 1 1 calc R . . C69 C 0.2888(10) 0.8162(10) -0.5719(9) 0.022(2) Uani 1 1 d U . . C70 C 0.3812(10) 0.7849(10) -0.5613(9) 0.022(2) Uani 1 1 d U . . H70 H 0.4222 0.7223 -0.5457 0.027 Uiso 1 1 calc R . . C71 C 0.4151(10) 0.8446(10) -0.5734(9) 0.023(2) Uani 1 1 d U . . C72 C 0.5168(10) 0.8078(11) -0.5631(10) 0.030(3) Uani 1 1 d U . . H72B H 0.5392 0.8145 -0.5210 0.045 Uiso 1 1 calc R . . H72C H 0.5289 0.8426 -0.6130 0.045 Uiso 1 1 calc R . . H72A H 0.5476 0.7426 -0.5485 0.045 Uiso 1 1 calc R . . C73 C 0.3555(10) 0.9343(10) -0.5954(9) 0.025(2) Uani 1 1 d U . . H73 H 0.3786 0.9740 -0.6023 0.030 Uiso 1 1 calc R . . C74 C 0.2643(11) 0.9691(11) -0.6077(10) 0.027(2) Uani 1 1 d U . . C75 C 0.1990(11) 1.0701(11) -0.6340(11) 0.034(3) Uani 1 1 d U . . H75C H 0.2097 1.1089 -0.6828 0.051 Uiso 1 1 calc R . . H75B H 0.2089 1.0835 -0.5922 0.051 Uiso 1 1 calc R . . H75A H 0.1366 1.0829 -0.6439 0.051 Uiso 1 1 calc R . . C76 C 0.2300(10) 0.9084(10) -0.5940(9) 0.023(2) Uani 1 1 d U . . H76 H 0.1668 0.9308 -0.6000 0.027 Uiso 1 1 calc R . . O2 O 0.3191(6) 0.6004(7) -0.3745(5) 0.0251(19) Uani 1 1 d DU . . C77 C 0.3285(7) 0.5617(10) -0.2886(6) 0.030(3) Uani 1 1 d DU . . H77A H 0.3317 0.5012 -0.2648 0.036 Uiso 1 1 calc R . . H77B H 0.2768 0.6036 -0.2763 0.036 Uiso 1 1 calc R . . C78 C 0.4158(8) 0.5518(10) -0.2577(7) 0.030(3) Uani 1 1 d DU . . H78A H 0.4426 0.5038 -0.2012 0.035 Uiso 1 1 calc R . . H78B H 0.4068 0.6107 -0.2639 0.035 Uiso 1 1 calc R . . C79 C 0.4740(7) 0.5236(10) -0.3115(7) 0.029(3) Uani 1 1 d DU . . H79B H 0.5253 0.5352 -0.3121 0.035 Uiso 1 1 calc R . . H79A H 0.4977 0.4579 -0.2947 0.035 Uiso 1 1 calc R . . C80 C 0.4074(7) 0.5855(10) -0.3914(6) 0.030(3) Uani 1 1 d DU . . H80B H 0.4069 0.6447 -0.4194 0.036 Uiso 1 1 calc R . . H80A H 0.4234 0.5557 -0.4249 0.036 Uiso 1 1 calc R . . C81 C 0.0652(12) 0.8635(11) -0.3496(11) 0.034(2) Uani 1 1 d U . . H81 H 0.0350 0.8788 -0.3095 0.041 Uiso 1 1 calc R . . C82 C 0.0220(12) 0.8985(7) -0.4287(8) 0.036(3) Uani 1 1 d U . . H82 H -0.0438 0.9438 -0.4542 0.044 Uiso 1 1 calc R . . C83 C 0.0900(11) 0.8648(10) -0.4680(10) 0.027(2) Uani 1 1 d U . . H83 H 0.0805 0.8818 -0.5254 0.032 Uiso 1 1 calc R . . C84 C 0.1750(11) 0.8068(11) -0.4105(10) 0.030(2) Uani 1 1 d U . . H84 H 0.2352 0.7745 -0.4209 0.036 Uiso 1 1 calc R . . C85 C 0.1609(12) 0.8032(10) -0.3374(10) 0.030(2) Uani 1 1 d U . . H85 H 0.2088 0.7700 -0.2878 0.036 Uiso 1 1 calc R . . C86 C 0.0991(11) 0.6263(10) -0.2629(9) 0.028(2) Uani 1 1 d U . . H86 H 0.1397 0.5955 -0.2096 0.033 Uiso 1 1 calc R . . C87 C 0.0073(11) 0.6954(11) -0.2877(10) 0.029(2) Uani 1 1 d U . . H87 H -0.0280 0.7221 -0.2553 0.035 Uiso 1 1 calc R . . C88 C -0.0275(11) 0.7202(11) -0.3682(10) 0.028(2) Uani 1 1 d U . . H88 H -0.0912 0.7650 -0.4005 0.034 Uiso 1 1 calc R . . C89 C 0.0423(10) 0.6591(9) -0.3866(7) 0.025(2) Uani 1 1 d U . . H89 H 0.0371 0.6568 -0.4371 0.030 Uiso 1 1 calc R . . C90 C 0.1211(9) 0.5998(9) -0.3230(9) 0.023(2) Uani 1 1 d U . . H90 H 0.1797 0.5490 -0.3203 0.028 Uiso 1 1 calc R . . C1S C 0.344(3) 0.049(3) -0.032(3) 0.169(12) Uiso 1 1 d DU . . H1SC H 0.4096 0.0223 -0.0247 0.254 Uiso 1 1 calc R . . H1SA H 0.3223 0.0818 -0.0020 0.254 Uiso 1 1 calc R . . H1SB H 0.3145 0.0917 -0.0887 0.254 Uiso 1 1 calc R . . C2S C 0.321(3) -0.028(3) -0.003(3) 0.166(11) Uiso 1 1 d DU . . H2SA H 0.3346 -0.0584 -0.0357 0.199 Uiso 1 1 calc R . . H2SB H 0.3509 -0.0743 0.0537 0.199 Uiso 1 1 calc R . . C3S C 0.220(3) 0.031(3) -0.015(3) 0.167(10) Uiso 1 1 d DU . . H3SB H 0.2066 0.0682 0.0123 0.200 Uiso 1 1 calc R . . H3SA H 0.1892 0.0730 -0.0720 0.200 Uiso 1 1 calc R . . C4S C 0.191(3) -0.041(3) 0.023(3) 0.174(10) Uiso 1 1 d DU . . H4S H 0.2362 -0.0919 0.0740 0.208 Uiso 1 1 calc R . . C5S C 0.099(3) 0.002(4) 0.040(3) 0.182(12) Uiso 1 1 d DU . . H5SC H 0.0996 0.0345 0.0683 0.273 Uiso 1 1 calc R . . H5SB H 0.0851 -0.0462 0.0728 0.273 Uiso 1 1 calc R . . H5SA H 0.0527 0.0459 -0.0102 0.273 Uiso 1 1 calc R . . C6S C 0.174(3) -0.081(3) -0.025(3) 0.168(12) Uiso 1 1 d DU . . H6SB H 0.1711 -0.1361 0.0112 0.252 Uiso 1 1 calc R . . H6SC H 0.2242 -0.0982 -0.0507 0.252 Uiso 1 1 calc R . . H6SA H 0.1173 -0.0357 -0.0649 0.252 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 U1 0.0233(3) 0.0172(2) 0.0209(2) -0.00914(19) 0.00348(19) -0.0078(2) Re1 0.0248(3) 0.0187(3) 0.0221(3) -0.0088(3) 0.0034(3) -0.0095(3) Si1 0.028(2) 0.0191(18) 0.0248(19) -0.0114(16) 0.0033(17) -0.0115(17) Si2 0.030(2) 0.0202(19) 0.024(2) -0.0084(16) 0.0046(17) -0.0102(17) Si3 0.027(2) 0.027(2) 0.029(2) -0.0167(18) 0.0061(17) -0.0155(18) N1 0.027(5) 0.014(4) 0.028(4) -0.014(3) 0.004(4) -0.007(4) N2 0.024(4) 0.020(4) 0.031(4) -0.014(4) 0.010(4) -0.013(4) N3 0.026(5) 0.028(5) 0.035(5) -0.018(4) 0.011(4) -0.017(4) C1 0.031(5) 0.014(5) 0.025(6) -0.010(5) 0.005(5) -0.010(4) C2 0.039(8) 0.046(10) 0.036(9) -0.017(8) 0.010(7) -0.031(8) C3 0.037(8) 0.023(6) 0.031(7) -0.011(5) 0.002(6) -0.011(6) C4 0.029(5) 0.022(4) 0.025(5) -0.014(4) 0.007(4) -0.009(4) C5 0.030(5) 0.023(5) 0.028(5) -0.013(4) 0.009(5) -0.018(4) C6 0.039(5) 0.027(5) 0.037(5) -0.018(4) 0.008(5) -0.023(4) C7 0.043(7) 0.037(7) 0.044(7) -0.026(6) 0.008(6) -0.022(6) C8 0.038(5) 0.029(5) 0.037(6) -0.022(5) 0.011(5) -0.018(4) C9 0.030(5) 0.029(5) 0.036(5) -0.025(4) 0.013(4) -0.012(4) C10 0.031(6) 0.035(7) 0.050(8) -0.024(6) 0.015(6) -0.011(5) C11 0.026(5) 0.024(5) 0.032(6) -0.020(4) 0.006(5) -0.009(4) C12 0.034(8) 0.035(9) 0.028(8) -0.014(7) 0.012(7) -0.012(7) C13 0.045(10) 0.029(8) 0.039(9) -0.025(8) 0.016(8) -0.010(7) C14 0.028(4) 0.024(4) 0.029(5) -0.019(4) 0.009(4) -0.012(4) C15 0.028(5) 0.027(5) 0.034(6) -0.021(5) 0.008(5) -0.013(4) C16 0.027(5) 0.034(5) 0.041(6) -0.026(5) 0.009(5) -0.010(4) C17 0.027(6) 0.041(7) 0.055(8) -0.034(6) 0.006(6) -0.010(5) C18 0.032(5) 0.032(5) 0.038(6) -0.025(5) 0.006(5) -0.005(4) C19 0.035(5) 0.027(5) 0.039(6) -0.022(5) 0.009(5) -0.007(4) C20 0.044(8) 0.027(6) 0.053(8) -0.015(6) 0.008(7) -0.005(5) C21 0.032(5) 0.026(5) 0.036(6) -0.018(5) 0.010(5) -0.011(4) C22 0.026(6) 0.031(7) 0.029(8) -0.011(6) -0.001(6) -0.013(5) C23 0.041(10) 0.025(8) 0.040(8) -0.018(7) 0.005(8) -0.019(7) C24 0.031(5) 0.031(4) 0.030(5) -0.018(4) 0.010(4) -0.018(4) C25 0.031(5) 0.031(5) 0.028(5) -0.017(5) 0.008(5) -0.017(4) C26 0.037(5) 0.028(5) 0.034(5) -0.016(4) 0.007(5) -0.015(4) C27 0.039(7) 0.027(6) 0.045(7) -0.013(6) 0.008(6) -0.015(5) C28 0.038(5) 0.032(5) 0.032(6) -0.014(5) 0.009(5) -0.019(4) C29 0.035(5) 0.032(5) 0.032(5) -0.018(4) 0.008(5) -0.022(4) C30 0.036(6) 0.035(7) 0.042(7) -0.020(6) 0.007(6) -0.023(5) C31 0.032(5) 0.032(5) 0.032(6) -0.017(5) 0.009(5) -0.020(4) O1 0.031(4) 0.064(6) 0.040(5) -0.035(5) 0.010(4) -0.023(4) C32 0.042(6) 0.073(7) 0.054(7) -0.048(6) 0.006(5) -0.012(6) C33 0.042(7) 0.062(7) 0.056(7) -0.043(6) 0.010(5) -0.017(6) C34 0.035(6) 0.051(7) 0.050(7) -0.033(6) 0.013(5) -0.022(5) C35 0.033(5) 0.053(7) 0.043(6) -0.030(5) 0.011(5) -0.022(5) C36 0.041(6) 0.030(4) 0.024(4) -0.004(4) 0.000(4) -0.023(5) C37 0.038(6) 0.044(6) 0.027(5) -0.007(4) 0.006(4) -0.028(4) C38 0.038(5) 0.045(6) 0.027(5) -0.005(4) 0.003(4) -0.029(4) C39 0.039(6) 0.030(5) 0.028(5) -0.007(4) 0.000(4) -0.027(5) C40 0.042(5) 0.024(4) 0.029(5) -0.006(4) 0.002(4) -0.021(4) C41 0.036(6) 0.023(5) 0.028(5) -0.012(4) 0.004(4) -0.018(4) C42 0.033(5) 0.029(5) 0.029(5) -0.009(4) 0.004(4) -0.020(4) C43 0.039(5) 0.024(5) 0.030(5) -0.014(4) 0.002(4) -0.018(4) C44 0.046(6) 0.026(5) 0.028(5) -0.015(4) 0.004(4) -0.014(5) C45 0.046(6) 0.020(4) 0.025(5) -0.013(4) 0.003(4) -0.013(4) U2 0.0186(2) 0.0131(2) 0.0233(2) -0.01068(18) 0.00565(19) -0.00721(18) Re2 0.0282(4) 0.0171(3) 0.0251(3) -0.0130(3) 0.0108(3) -0.0126(3) Si4 0.0197(19) 0.0174(18) 0.028(2) -0.0142(16) 0.0051(16) -0.0070(15) Si5 0.021(2) 0.0165(18) 0.033(2) -0.0150(16) 0.0054(17) -0.0063(16) Si6 0.021(2) 0.0234(19) 0.031(2) -0.0166(17) 0.0098(17) -0.0122(17) N4 0.018(4) 0.011(4) 0.027(4) -0.006(4) 0.006(3) -0.008(3) N5 0.022(5) 0.016(4) 0.031(5) -0.013(4) 0.003(4) -0.005(4) N6 0.019(5) 0.025(5) 0.030(5) -0.014(4) 0.014(4) -0.017(4) C46 0.022(5) 0.020(5) 0.031(7) -0.015(5) 0.005(5) -0.008(4) C47 0.024(8) 0.017(5) 0.028(7) -0.006(5) 0.006(6) -0.011(6) C48 0.024(7) 0.025(8) 0.034(8) -0.018(7) 0.006(6) -0.011(6) C49 0.019(4) 0.017(4) 0.026(5) -0.011(4) 0.000(4) -0.006(3) C50 0.019(5) 0.022(5) 0.027(5) -0.013(4) 0.002(4) -0.008(4) C51 0.022(5) 0.023(4) 0.030(5) -0.013(4) 0.003(4) -0.011(4) C52 0.026(6) 0.024(6) 0.037(7) -0.013(5) 0.006(6) -0.012(5) C53 0.020(5) 0.024(5) 0.031(6) -0.013(4) 0.004(5) -0.008(4) C54 0.019(5) 0.021(4) 0.032(5) -0.013(4) 0.002(4) -0.004(4) C55 0.023(6) 0.021(5) 0.040(7) -0.014(5) 0.003(6) -0.004(5) C56 0.019(5) 0.016(4) 0.028(5) -0.010(4) 0.005(4) -0.007(4) C57 0.030(7) 0.023(7) 0.039(9) -0.020(7) 0.009(7) -0.003(6) C58 0.033(7) 0.024(8) 0.046(9) -0.026(7) 0.013(7) -0.015(7) C59 0.024(5) 0.016(4) 0.033(4) -0.014(4) 0.010(4) -0.008(4) C60 0.024(5) 0.017(5) 0.038(6) -0.013(4) 0.009(5) -0.006(4) C61 0.026(5) 0.021(5) 0.037(5) -0.013(4) 0.010(4) -0.012(4) C62 0.030(6) 0.027(6) 0.043(7) -0.013(6) 0.006(6) -0.017(5) C63 0.026(5) 0.022(5) 0.039(6) -0.011(4) 0.008(5) -0.010(4) C64 0.023(5) 0.023(5) 0.038(5) -0.013(4) 0.008(4) -0.008(4) C65 0.026(6) 0.029(6) 0.042(7) -0.010(6) 0.004(6) -0.011(5) C66 0.027(5) 0.013(4) 0.036(5) -0.019(4) 0.012(4) -0.007(4) C67 0.020(6) 0.032(7) 0.034(8) -0.019(6) 0.009(6) -0.008(5) C68 0.027(8) 0.027(7) 0.028(6) -0.016(5) 0.008(6) -0.013(6) C69 0.021(4) 0.025(4) 0.028(5) -0.016(4) 0.013(4) -0.015(4) C70 0.026(5) 0.025(5) 0.026(5) -0.016(4) 0.011(4) -0.017(4) C71 0.023(5) 0.029(5) 0.029(5) -0.017(4) 0.010(4) -0.019(4) C72 0.021(5) 0.034(6) 0.032(7) -0.011(6) 0.008(5) -0.017(5) C73 0.026(5) 0.029(5) 0.033(6) -0.021(5) 0.010(5) -0.018(4) C74 0.028(5) 0.026(5) 0.039(5) -0.020(4) 0.012(5) -0.017(4) C75 0.033(6) 0.024(5) 0.049(7) -0.022(6) 0.013(6) -0.014(5) C76 0.023(5) 0.022(4) 0.035(6) -0.017(4) 0.013(5) -0.016(4) O2 0.018(4) 0.028(4) 0.030(4) -0.016(3) 0.006(3) -0.010(3) C77 0.027(5) 0.024(5) 0.031(5) -0.009(5) 0.008(4) -0.011(5) C78 0.027(6) 0.026(5) 0.032(5) -0.012(5) 0.005(4) -0.013(5) C79 0.025(5) 0.025(5) 0.036(6) -0.017(5) 0.005(4) -0.009(5) C80 0.026(5) 0.029(5) 0.032(5) -0.016(5) 0.004(4) -0.011(5) C81 0.047(6) 0.022(5) 0.047(5) -0.025(4) 0.026(5) -0.019(4) C82 0.043(6) 0.018(4) 0.047(6) -0.017(4) 0.021(5) -0.013(4) C83 0.036(6) 0.021(4) 0.041(5) -0.020(4) 0.018(4) -0.023(4) C84 0.035(5) 0.030(5) 0.041(6) -0.023(4) 0.021(4) -0.023(4) C85 0.046(5) 0.023(5) 0.044(5) -0.028(4) 0.017(5) -0.023(4) C86 0.034(5) 0.023(4) 0.026(4) -0.010(3) 0.009(4) -0.016(4) C87 0.030(5) 0.028(5) 0.033(5) -0.014(4) 0.017(4) -0.018(4) C88 0.026(5) 0.025(5) 0.036(5) -0.017(4) 0.012(4) -0.013(4) C89 0.027(5) 0.022(5) 0.032(5) -0.017(4) 0.007(4) -0.013(4) C90 0.029(5) 0.015(4) 0.027(5) -0.010(4) 0.008(4) -0.012(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 U1 N1 2.261(12) . ? U1 N2 2.256(12) . ? U1 N3 2.288(13) . ? U1 O1 2.531(9) . ? U1 Re1 3.0021(8) . ? Re1 C40 2.180(16) . ? Re1 C36 2.192(15) . ? Re1 C38 2.216(17) . ? Re1 C42 2.218(16) . ? Re1 C41 2.221(15) . ? Re1 C43 2.224(15) . ? Re1 C44 2.237(16) . ? Re1 C37 2.240(16) . ? Re1 C39 2.247(15) . ? Re1 C45 2.253(14) . ? Si1 N1 1.731(13) . ? Si1 C2 1.850(16) . ? Si1 C3 1.855(16) . ? Si1 C1 1.877(14) . ? Si2 N2 1.763(13) . ? Si2 C1 1.873(15) . ? Si2 C12 1.880(17) . ? Si2 C13 1.882(17) . ? Si3 N3 1.744(14) . ? Si3 C23 1.857(16) . ? Si3 C22 1.882(16) . ? Si3 C1 1.910(16) . ? N1 C4 1.456(18) . ? N2 C14 1.418(19) . ? N3 C24 1.43(2) . ? C1 H1 1.0000 . ? C2 H2C 0.9800 . ? C2 H2B 0.9800 . ? C2 H2A 0.9800 . ? C3 H3C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C11 1.39(2) . ? C4 C5 1.39(2) . ? C5 C6 1.42(2) . ? C5 H5 0.9500 . ? C6 C8 1.36(2) . ? C6 C7 1.47(2) . ? C7 H7C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.38(2) . ? C8 H8 0.9500 . ? C9 C11 1.40(2) . ? C9 C10 1.50(2) . ? C10 H10A 0.9800 . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C11 H11 0.9500 . ? C12 H12C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.38(2) . ? C14 C21 1.39(2) . ? C15 C16 1.40(2) . ? C15 H15 0.9500 . ? C16 C18 1.42(2) . ? C16 C17 1.52(2) . ? C17 H17B 0.9800 . ? C17 H17A 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 C21 1.40(2) . ? C19 C20 1.51(2) . ? C20 H20C 0.9800 . ? C20 H20B 0.9800 . ? C20 H20A 0.9800 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.38(2) . ? C24 C31 1.40(2) . ? C25 C26 1.39(2) . ? C25 H25 0.9500 . ? C26 C28 1.37(2) . ? C26 C27 1.48(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.36(2) . ? C28 H28 0.9500 . ? C29 C31 1.41(2) . ? C29 C30 1.52(2) . ? C30 H30B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? O1 C32 1.46(3) . ? O1 C35 1.46(3) . ? C32 C33 1.51(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.52(3) . ? C33 H33B 0.9900 . ? C33 H33A 0.9900 . ? C34 C35 1.51(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C40 1.39(2) . ? C36 C37 1.40(2) . ? C36 H36 1.0000 . ? C37 C38 1.43(2) . ? C37 H37 1.0000 . ? C38 C39 1.47(2) . ? C38 H38 1.0000 . ? C39 C40 1.43(2) . ? C39 H39 1.0000 . ? C40 H40 1.0000 . ? C41 C42 1.39(2) . ? C41 C45 1.43(2) . ? C41 H41 1.0000 . ? C42 C43 1.44(2) . ? C42 H42 1.0000 . ? C43 C44 1.43(2) . ? C43 H43 1.0000 . ? C44 C45 1.45(2) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? U2 N5 2.279(11) . ? U2 N4 2.297(12) . ? U2 N6 2.308(11) . ? U2 O2 2.573(9) . ? U2 Re2 2.9541(8) . ? Re2 C82 2.182(10) . ? Re2 C88 2.193(16) . ? Re2 C86 2.206(15) . ? Re2 C83 2.212(15) . ? Re2 C85 2.214(15) . ? Re2 C81 2.218(15) . ? Re2 C87 2.221(15) . ? Re2 C84 2.226(15) . ? Re2 C89 2.243(14) . ? Re2 C90 2.281(14) . ? Si4 N4 1.765(12) . ? Si4 C48 1.853(15) . ? Si4 C46 1.882(15) . ? Si4 C47 1.882(14) . ? Si5 N5 1.728(13) . ? Si5 C57 1.856(15) . ? Si5 C46 1.886(15) . ? Si5 C58 1.894(16) . ? Si6 N6 1.751(12) . ? Si6 C68 1.861(15) . ? Si6 C67 1.873(15) . ? Si6 C46 1.909(15) . ? N4 C49 1.361(18) . ? N5 C59 1.418(19) . ? N6 C69 1.431(18) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47C 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48C 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.41(2) . ? C49 C56 1.436(19) . ? C50 C51 1.39(2) . ? C50 H50 0.9500 . ? C51 C53 1.38(2) . ? C51 C52 1.53(2) . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C52 H52A 0.9800 . ? C53 C54 1.38(2) . ? C53 H53 0.9500 . ? C54 C56 1.39(2) . ? C54 C55 1.49(2) . ? C55 H55A 0.9800 . ? C55 H55C 0.9800 . ? C55 H55B 0.9800 . ? C56 H56 0.9500 . ? C57 H57C 0.9800 . ? C57 H57B 0.9800 . ? C57 H57A 0.9800 . ? C58 H58A 0.9800 . ? C58 H58C 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.38(2) . ? C59 C66 1.43(2) . ? C60 C61 1.41(2) . ? C60 H60 0.9500 . ? C61 C63 1.40(2) . ? C61 C62 1.52(2) . ? C62 H62C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C63 C64 1.40(2) . ? C63 H63 0.9500 . ? C64 C66 1.37(2) . ? C64 C65 1.49(2) . ? C65 H65C 0.9800 . ? C65 H65B 0.9800 . ? C65 H65A 0.9800 . ? C66 H66 0.9500 . ? C67 H67C 0.9800 . ? C67 H67B 0.9800 . ? C67 H67A 0.9800 . ? C68 H68C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C69 C70 1.39(2) . ? C69 C76 1.40(2) . ? C70 C71 1.407(19) . ? C70 H70 0.9500 . ? C71 C73 1.37(2) . ? C71 C72 1.52(2) . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C72 H72A 0.9800 . ? C73 C74 1.36(2) . ? C73 H73 0.9500 . ? C74 C76 1.43(2) . ? C74 C75 1.53(2) . ? C75 H75C 0.9800 . ? C75 H75B 0.9800 . ? C75 H75A 0.9800 . ? C76 H76 0.9500 . ? O2 C80 1.463(9) . ? O2 C77 1.464(9) . ? C77 C78 1.509(9) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.525(11) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.511(9) . ? C79 H79B 0.9900 . ? C79 H79A 0.9900 . ? C80 H80B 0.9900 . ? C80 H80A 0.9900 . ? C81 C82 1.42(2) . ? C81 C85 1.45(2) . ? C81 H81 1.0000 . ? C82 C83 1.44(2) . ? C82 H82 1.0000 . ? C83 C84 1.43(2) . ? C83 H83 1.0000 . ? C84 C85 1.41(2) . ? C84 H84 1.0000 . ? C85 H85 1.0000 . ? C86 C87 1.41(2) . ? C86 C90 1.44(2) . ? C86 H86 1.0000 . ? C87 C88 1.46(2) . ? C87 H87 1.0000 . ? C88 C89 1.40(2) . ? C88 H88 1.0000 . ? C89 C90 1.425(18) . ? C89 H89 1.0000 . ? C90 H90 1.0000 . ? C1S C2S 1.53(8) . ? C1S H1SC 0.9800 . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C2S C3S 1.52(8) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.52(8) . ? C3S H3SB 0.9900 . ? C3S H3SA 0.9900 . ? C4S C5S 1.51(9) . ? C4S C6S 1.51(9) . ? C4S H4S 1.0000 . ? C5S H5SC 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? C6S H6SA 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 U1 N1 98.9(4) . . ? N2 U1 N3 90.8(4) . . ? N1 U1 N3 96.2(4) . . ? N2 U1 O1 176.6(4) . . ? N1 U1 O1 83.1(4) . . ? N3 U1 O1 86.3(4) . . ? N2 U1 Re1 95.4(3) . . ? N1 U1 Re1 123.6(3) . . ? N3 U1 Re1 138.0(3) . . ? O1 U1 Re1 85.7(2) . . ? C40 Re1 C36 36.9(6) . . ? C40 Re1 C38 63.4(7) . . ? C36 Re1 C38 62.8(6) . . ? C40 Re1 C42 108.3(6) . . ? C36 Re1 C42 118.9(6) . . ? C38 Re1 C42 165.2(7) . . ? C40 Re1 C41 131.3(6) . . ? C36 Re1 C41 155.1(6) . . ? C38 Re1 C41 139.3(6) . . ? C42 Re1 C41 36.4(6) . . ? C40 Re1 C43 114.4(6) . . ? C36 Re1 C43 100.2(6) . . ? C38 Re1 C43 155.6(6) . . ? C42 Re1 C43 37.9(6) . . ? C41 Re1 C43 62.1(6) . . ? C40 Re1 C44 145.7(6) . . ? C36 Re1 C44 115.1(6) . . ? C38 Re1 C44 131.1(7) . . ? C42 Re1 C44 62.9(6) . . ? C41 Re1 C44 62.5(6) . . ? C43 Re1 C44 37.5(6) . . ? C40 Re1 C37 62.1(7) . . ? C36 Re1 C37 36.9(6) . . ? C38 Re1 C37 37.6(6) . . ? C42 Re1 C37 151.7(6) . . ? C41 Re1 C37 166.2(6) . . ? C43 Re1 C37 118.5(6) . . ? C44 Re1 C37 108.7(7) . . ? C40 Re1 C39 37.7(6) . . ? C36 Re1 C39 62.4(6) . . ? C38 Re1 C39 38.4(6) . . ? C42 Re1 C39 127.5(6) . . ? C41 Re1 C39 124.4(5) . . ? C43 Re1 C39 150.8(6) . . ? C44 Re1 C39 169.5(6) . . ? C37 Re1 C39 62.8(6) . . ? C40 Re1 C45 168.7(6) . . ? C36 Re1 C45 151.7(6) . . ? C38 Re1 C45 124.3(6) . . ? C42 Re1 C45 62.1(5) . . ? C41 Re1 C45 37.3(5) . . ? C43 Re1 C45 62.5(5) . . ? C44 Re1 C45 37.6(5) . . ? C37 Re1 C45 129.2(6) . . ? C39 Re1 C45 142.3(5) . . ? C40 Re1 U1 105.1(4) . . ? C36 Re1 U1 130.5(4) . . ? C38 Re1 U1 71.8(4) . . ? C42 Re1 U1 100.2(4) . . ? C41 Re1 U1 67.7(4) . . ? C43 Re1 U1 128.9(4) . . ? C44 Re1 U1 109.1(4) . . ? C37 Re1 U1 108.0(4) . . ? C39 Re1 U1 70.0(4) . . ? C45 Re1 U1 72.4(4) . . ? N1 Si1 C2 109.4(7) . . ? N1 Si1 C3 111.6(7) . . ? C2 Si1 C3 104.5(8) . . ? N1 Si1 C1 106.0(6) . . ? C2 Si1 C1 112.7(8) . . ? C3 Si1 C1 112.7(7) . . ? N2 Si2 C1 106.9(6) . . ? N2 Si2 C12 111.5(7) . . ? C1 Si2 C12 112.5(7) . . ? N2 Si2 C13 111.5(7) . . ? C1 Si2 C13 113.4(7) . . ? C12 Si2 C13 101.2(8) . . ? N3 Si3 C23 112.4(7) . . ? N3 Si3 C22 111.5(7) . . ? C23 Si3 C22 103.1(8) . . ? N3 Si3 C1 105.5(6) . . ? C23 Si3 C1 111.6(7) . . ? C22 Si3 C1 112.9(7) . . ? C4 N1 Si1 114.6(9) . . ? C4 N1 U1 129.1(9) . . ? Si1 N1 U1 116.2(6) . . ? C14 N2 Si2 114.1(10) . . ? C14 N2 U1 129.5(10) . . ? Si2 N2 U1 115.6(6) . . ? C24 N3 Si3 119.5(10) . . ? C24 N3 U1 124.7(10) . . ? Si3 N3 U1 114.8(6) . . ? Si2 C1 Si1 116.7(8) . . ? Si2 C1 Si3 111.3(7) . . ? Si1 C1 Si3 114.0(8) . . ? Si2 C1 H1 104.4 . . ? Si1 C1 H1 104.4 . . ? Si3 C1 H1 104.4 . . ? Si1 C2 H2C 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? Si1 C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? Si1 C3 H3C 109.5 . . ? Si1 C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C11 C4 C5 117.3(13) . . ? C11 C4 N1 121.4(14) . . ? C5 C4 N1 121.3(13) . . ? C4 C5 C6 121.5(14) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C8 C6 C5 117.5(14) . . ? C8 C6 C7 124.7(15) . . ? C5 C6 C7 117.8(15) . . ? C6 C7 H7C 109.5 . . ? C6 C7 H7A 109.5 . . ? H7C C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C8 C9 124.1(15) . . ? C6 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C8 C9 C11 117.0(15) . . ? C8 C9 C10 121.8(14) . . ? C11 C9 C10 121.3(15) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C4 C11 C9 122.7(15) . . ? C4 C11 H11 118.7 . . ? C9 C11 H11 118.7 . . ? Si2 C12 H12C 109.5 . . ? Si2 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C15 C14 C21 117.8(15) . . ? C15 C14 N2 120.4(13) . . ? C21 C14 N2 121.9(14) . . ? C14 C15 C16 121.0(15) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C18 118.9(16) . . ? C15 C16 C17 120.7(15) . . ? C18 C16 C17 120.4(15) . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C16 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? C19 C18 C16 121.2(16) . . ? C19 C18 H18 119.4 . . ? C16 C18 H18 119.4 . . ? C18 C19 C21 117.6(16) . . ? C18 C19 C20 121.2(16) . . ? C21 C19 C20 121.2(17) . . ? C19 C20 H20C 109.5 . . ? C19 C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? C19 C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? C14 C21 C19 123.4(16) . . ? C14 C21 H21 118.3 . . ? C19 C21 H21 118.3 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C31 118.6(15) . . ? C25 C24 N3 119.2(14) . . ? C31 C24 N3 122.2(14) . . ? C24 C25 C26 122.3(15) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C28 C26 C25 117.7(16) . . ? C28 C26 C27 122.8(16) . . ? C25 C26 C27 119.5(16) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C26 122.9(16) . . ? C29 C28 H28 118.6 . . ? C26 C28 H28 118.6 . . ? C28 C29 C31 119.3(15) . . ? C28 C29 C30 122.3(15) . . ? C31 C29 C30 118.4(15) . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? C29 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? C24 C31 C29 119.1(15) . . ? C24 C31 H31 120.4 . . ? C29 C31 H31 120.4 . . ? C35 O1 C32 109.5(8) . . ? C35 O1 U1 123.8(7) . . ? C32 O1 U1 125.0(7) . . ? O1 C32 C33 106.4(8) . . ? O1 C32 H32A 110.4 . . ? C33 C32 H32A 110.4 . . ? O1 C32 H32B 110.4 . . ? C33 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C32 C33 C34 103.6(7) . . ? C32 C33 H33B 111.0 . . ? C34 C33 H33B 111.0 . . ? C32 C33 H33A 111.0 . . ? C34 C33 H33A 111.0 . . ? H33B C33 H33A 109.0 . . ? C35 C34 C33 104.4(7) . . ? C35 C34 H34A 110.9 . . ? C33 C34 H34A 110.9 . . ? C35 C34 H34B 110.9 . . ? C33 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? O1 C35 C34 106.4(8) . . ? O1 C35 H35A 110.5 . . ? C34 C35 H35A 110.5 . . ? O1 C35 H35B 110.5 . . ? C34 C35 H35B 110.5 . . ? H35A C35 H35B 108.6 . . ? C40 C36 C37 109.6(15) . . ? C40 C36 Re1 71.1(9) . . ? C37 C36 Re1 73.4(9) . . ? C40 C36 H36 125.1 . . ? C37 C36 H36 125.1 . . ? Re1 C36 H36 125.1 . . ? C36 C37 C38 107.9(16) . . ? C36 C37 Re1 69.7(9) . . ? C38 C37 Re1 70.3(9) . . ? C36 C37 H37 126.1 . . ? C38 C37 H37 126.1 . . ? Re1 C37 H37 126.1 . . ? C37 C38 C39 107.1(15) . . ? C37 C38 Re1 72.1(10) . . ? C39 C38 Re1 71.9(9) . . ? C37 C38 H38 126.3 . . ? C39 C38 H38 126.3 . . ? Re1 C38 H38 126.3 . . ? C40 C39 C38 105.7(14) . . ? C40 C39 Re1 68.6(9) . . ? C38 C39 Re1 69.6(9) . . ? C40 C39 H39 127.2 . . ? C38 C39 H39 127.2 . . ? Re1 C39 H39 127.2 . . ? C36 C40 C39 109.6(16) . . ? C36 C40 Re1 72.0(10) . . ? C39 C40 Re1 73.7(9) . . ? C36 C40 H40 125.1 . . ? C39 C40 H40 125.1 . . ? Re1 C40 H40 125.1 . . ? C42 C41 C45 109.8(14) . . ? C42 C41 Re1 71.7(9) . . ? C45 C41 Re1 72.6(8) . . ? C42 C41 H41 125.0 . . ? C45 C41 H41 125.0 . . ? Re1 C41 H41 125.0 . . ? C41 C42 C43 108.2(15) . . ? C41 C42 Re1 71.9(9) . . ? C43 C42 Re1 71.3(9) . . ? C41 C42 H42 125.9 . . ? C43 C42 H42 125.9 . . ? Re1 C42 H42 125.9 . . ? C44 C43 C42 107.8(14) . . ? C44 C43 Re1 71.7(9) . . ? C42 C43 Re1 70.8(9) . . ? C44 C43 H43 126.0 . . ? C42 C43 H43 126.0 . . ? Re1 C43 H43 126.0 . . ? C43 C44 C45 107.3(14) . . ? C43 C44 Re1 70.8(9) . . ? C45 C44 Re1 71.8(8) . . ? C43 C44 H44 126.3 . . ? C45 C44 H44 126.3 . . ? Re1 C44 H44 126.3 . . ? C41 C45 C44 106.9(13) . . ? C41 C45 Re1 70.1(8) . . ? C44 C45 Re1 70.6(8) . . ? C41 C45 H45 126.5 . . ? C44 C45 H45 126.5 . . ? Re1 C45 H45 126.5 . . ? N5 U2 N4 93.4(4) . . ? N5 U2 N6 102.7(4) . . ? N4 U2 N6 97.3(4) . . ? N5 U2 O2 82.3(4) . . ? N4 U2 O2 175.0(3) . . ? N6 U2 O2 86.1(4) . . ? N5 U2 Re2 126.9(3) . . ? N4 U2 Re2 96.0(3) . . ? N6 U2 Re2 127.4(3) . . ? O2 U2 Re2 84.81(19) . . ? C82 Re2 C88 106.4(6) . . ? C82 Re2 C86 145.2(6) . . ? C88 Re2 C86 63.7(6) . . ? C82 Re2 C83 38.1(5) . . ? C88 Re2 C83 125.0(6) . . ? C86 Re2 C83 171.2(6) . . ? C82 Re2 C85 63.8(7) . . ? C88 Re2 C85 154.2(6) . . ? C86 Re2 C85 109.6(6) . . ? C83 Re2 C85 63.3(6) . . ? C82 Re2 C81 37.6(6) . . ? C88 Re2 C81 119.4(6) . . ? C86 Re2 C81 115.2(6) . . ? C83 Re2 C81 62.9(6) . . ? C85 Re2 C81 38.2(6) . . ? C82 Re2 C87 113.9(6) . . ? C88 Re2 C87 38.5(6) . . ? C86 Re2 C87 37.1(6) . . ? C83 Re2 C87 150.2(6) . . ? C85 Re2 C87 120.7(6) . . ? C81 Re2 C87 101.1(6) . . ? C82 Re2 C84 63.0(6) . . ? C88 Re2 C84 162.0(6) . . ? C86 Re2 C84 133.5(6) . . ? C83 Re2 C84 37.7(6) . . ? C85 Re2 C84 36.9(6) . . ? C81 Re2 C84 62.2(6) . . ? C87 Re2 C84 157.6(6) . . ? C82 Re2 C89 131.0(6) . . ? C88 Re2 C89 36.8(5) . . ? C86 Re2 C89 61.9(5) . . ? C83 Re2 C89 123.5(5) . . ? C85 Re2 C89 164.4(5) . . ? C81 Re2 C89 156.1(6) . . ? C87 Re2 C89 61.5(6) . . ? C84 Re2 C89 138.7(5) . . ? C82 Re2 C90 167.6(6) . . ? C88 Re2 C90 62.5(5) . . ? C86 Re2 C90 37.3(5) . . ? C83 Re2 C90 142.4(5) . . ? C85 Re2 C90 128.6(5) . . ? C81 Re2 C90 151.4(6) . . ? C87 Re2 C90 61.7(5) . . ? C84 Re2 C90 125.9(5) . . ? C89 Re2 C90 36.7(5) . . ? C82 Re2 U2 104.3(4) . . ? C88 Re2 U2 102.5(4) . . ? C86 Re2 U2 110.4(4) . . ? C83 Re2 U2 68.0(4) . . ? C85 Re2 U2 103.1(4) . . ? C81 Re2 U2 127.8(4) . . ? C87 Re2 U2 130.9(4) . . ? C84 Re2 U2 68.4(4) . . ? C89 Re2 U2 70.3(4) . . ? C90 Re2 U2 74.4(4) . . ? N4 Si4 C48 112.5(7) . . ? N4 Si4 C46 104.7(6) . . ? C48 Si4 C46 111.3(7) . . ? N4 Si4 C47 110.3(6) . . ? C48 Si4 C47 103.1(7) . . ? C46 Si4 C47 115.1(7) . . ? N5 Si5 C57 111.7(7) . . ? N5 Si5 C46 106.3(6) . . ? C57 Si5 C46 112.6(7) . . ? N5 Si5 C58 111.6(7) . . ? C57 Si5 C58 102.7(7) . . ? C46 Si5 C58 112.0(7) . . ? N6 Si6 C68 110.7(6) . . ? N6 Si6 C67 113.4(7) . . ? C68 Si6 C67 105.6(7) . . ? N6 Si6 C46 106.4(6) . . ? C68 Si6 C46 109.9(7) . . ? C67 Si6 C46 110.9(7) . . ? C49 N4 Si4 118.0(9) . . ? C49 N4 U2 130.8(9) . . ? Si4 N4 U2 111.0(6) . . ? C59 N5 Si5 119.6(10) . . ? C59 N5 U2 125.9(9) . . ? Si5 N5 U2 113.5(6) . . ? C69 N6 Si6 113.4(9) . . ? C69 N6 U2 136.7(9) . . ? Si6 N6 U2 109.8(6) . . ? Si4 C46 Si5 115.5(8) . . ? Si4 C46 Si6 113.0(7) . . ? Si5 C46 Si6 116.1(8) . . ? Si4 C46 H46 103.3 . . ? Si5 C46 H46 103.3 . . ? Si6 C46 H46 103.3 . . ? Si4 C47 H47A 109.5 . . ? Si4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? Si4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? H47C C47 H47B 109.5 . . ? Si4 C48 H48A 109.5 . . ? Si4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? Si4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? H48C C48 H48B 109.5 . . ? N4 C49 C50 120.7(12) . . ? N4 C49 C56 124.1(13) . . ? C50 C49 C56 115.2(13) . . ? C51 C50 C49 123.3(13) . . ? C51 C50 H50 118.3 . . ? C49 C50 H50 118.3 . . ? C53 C51 C50 118.3(14) . . ? C53 C51 C52 121.3(14) . . ? C50 C51 C52 120.4(13) . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C52 H52A 109.5 . . ? H52B C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? C54 C53 C51 121.8(14) . . ? C54 C53 H53 119.1 . . ? C51 C53 H53 119.1 . . ? C53 C54 C56 119.4(14) . . ? C53 C54 C55 120.3(14) . . ? C56 C54 C55 120.3(14) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? H55C C55 H55B 109.5 . . ? C54 C56 C49 122.0(14) . . ? C54 C56 H56 119.0 . . ? C49 C56 H56 119.0 . . ? Si5 C57 H57C 109.5 . . ? Si5 C57 H57B 109.5 . . ? H57C C57 H57B 109.5 . . ? Si5 C57 H57A 109.5 . . ? H57C C57 H57A 109.5 . . ? H57B C57 H57A 109.5 . . ? Si5 C58 H58A 109.5 . . ? Si5 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? Si5 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? H58C C58 H58B 109.5 . . ? C60 C59 N5 121.8(14) . . ? C60 C59 C66 117.8(14) . . ? N5 C59 C66 120.4(13) . . ? C59 C60 C61 121.5(15) . . ? C59 C60 H60 119.3 . . ? C61 C60 H60 119.3 . . ? C63 C61 C60 119.0(14) . . ? C63 C61 C62 121.1(14) . . ? C60 C61 C62 119.9(14) . . ? C61 C62 H62C 109.5 . . ? C61 C62 H62A 109.5 . . ? H62C C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62C C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C63 C64 120.7(15) . . ? C61 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C66 C64 C63 119.2(15) . . ? C66 C64 C65 120.6(15) . . ? C63 C64 C65 120.2(14) . . ? C64 C65 H65C 109.5 . . ? C64 C65 H65B 109.5 . . ? H65C C65 H65B 109.5 . . ? C64 C65 H65A 109.5 . . ? H65C C65 H65A 109.5 . . ? H65B C65 H65A 109.5 . . ? C64 C66 C59 121.8(14) . . ? C64 C66 H66 119.1 . . ? C59 C66 H66 119.1 . . ? Si6 C67 H67C 109.5 . . ? Si6 C67 H67B 109.5 . . ? H67C C67 H67B 109.5 . . ? Si6 C67 H67A 109.5 . . ? H67C C67 H67A 109.5 . . ? H67B C67 H67A 109.5 . . ? Si6 C68 H68C 109.5 . . ? Si6 C68 H68A 109.5 . . ? H68C C68 H68A 109.5 . . ? Si6 C68 H68B 109.5 . . ? H68C C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C70 C69 C76 118.4(13) . . ? C70 C69 N6 122.2(13) . . ? C76 C69 N6 119.3(13) . . ? C69 C70 C71 121.1(14) . . ? C69 C70 H70 119.5 . . ? C71 C70 H70 119.5 . . ? C73 C71 C70 118.8(14) . . ? C73 C71 C72 121.9(13) . . ? C70 C71 C72 119.3(13) . . ? C71 C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C72 H72A 109.5 . . ? H72B C72 H72A 109.5 . . ? H72C C72 H72A 109.5 . . ? C74 C73 C71 122.7(14) . . ? C74 C73 H73 118.6 . . ? C71 C73 H73 118.6 . . ? C73 C74 C76 118.5(14) . . ? C73 C74 C75 121.7(14) . . ? C76 C74 C75 119.8(14) . . ? C74 C75 H75C 109.5 . . ? C74 C75 H75B 109.5 . . ? H75C C75 H75B 109.5 . . ? C74 C75 H75A 109.5 . . ? H75C C75 H75A 109.5 . . ? H75B C75 H75A 109.5 . . ? C69 C76 C74 120.4(13) . . ? C69 C76 H76 119.8 . . ? C74 C76 H76 119.8 . . ? C80 O2 C77 108.7(8) . . ? C80 O2 U2 122.5(6) . . ? C77 O2 U2 128.4(6) . . ? O2 C77 C78 104.8(7) . . ? O2 C77 H77A 110.8 . . ? C78 C77 H77A 110.8 . . ? O2 C77 H77B 110.8 . . ? C78 C77 H77B 110.8 . . ? H77A C77 H77B 108.9 . . ? C77 C78 C79 101.4(7) . . ? C77 C78 H78A 111.5 . . ? C79 C78 H78A 111.5 . . ? C77 C78 H78B 111.5 . . ? C79 C78 H78B 111.5 . . ? H78A C78 H78B 109.3 . . ? C80 C79 C78 102.1(7) . . ? C80 C79 H79B 111.3 . . ? C78 C79 H79B 111.3 . . ? C80 C79 H79A 111.3 . . ? C78 C79 H79A 111.3 . . ? H79B C79 H79A 109.2 . . ? O2 C80 C79 105.6(8) . . ? O2 C80 H80B 110.6 . . ? C79 C80 H80B 110.6 . . ? O2 C80 H80A 110.6 . . ? C79 C80 H80A 110.6 . . ? H80B C80 H80A 108.8 . . ? C82 C81 C85 108.2(14) . . ? C82 C81 Re2 69.8(8) . . ? C85 C81 Re2 70.8(8) . . ? C82 C81 H81 125.9 . . ? C85 C81 H81 125.9 . . ? Re2 C81 H81 125.9 . . ? C81 C82 C83 108.3(15) . . ? C81 C82 Re2 72.6(7) . . ? C83 C82 Re2 72.1(8) . . ? C81 C82 H82 125.7 . . ? C83 C82 H82 125.7 . . ? Re2 C82 H82 125.7 . . ? C84 C83 C82 106.8(14) . . ? C84 C83 Re2 71.7(9) . . ? C82 C83 Re2 69.8(7) . . ? C84 C83 H83 126.6 . . ? C82 C83 H83 126.6 . . ? Re2 C83 H83 126.6 . . ? C85 C84 C83 109.6(14) . . ? C85 C84 Re2 71.1(9) . . ? C83 C84 Re2 70.6(8) . . ? C85 C84 H84 125.2 . . ? C83 C84 H84 125.2 . . ? Re2 C84 H84 125.2 . . ? C84 C85 C81 107.0(15) . . ? C84 C85 Re2 72.0(9) . . ? C81 C85 Re2 71.1(9) . . ? C84 C85 H85 126.4 . . ? C81 C85 H85 126.4 . . ? Re2 C85 H85 126.4 . . ? C87 C86 C90 108.4(14) . . ? C87 C86 Re2 72.0(9) . . ? C90 C86 Re2 74.2(8) . . ? C87 C86 H86 125.6 . . ? C90 C86 H86 125.6 . . ? Re2 C86 H86 125.6 . . ? C86 C87 C88 108.3(14) . . ? C86 C87 Re2 70.9(9) . . ? C88 C87 Re2 69.7(8) . . ? C86 C87 H87 125.9 . . ? C88 C87 H87 125.9 . . ? Re2 C87 H87 125.9 . . ? C89 C88 C87 106.1(13) . . ? C89 C88 Re2 73.5(9) . . ? C87 C88 Re2 71.8(9) . . ? C89 C88 H88 126.6 . . ? C87 C88 H88 126.6 . . ? Re2 C88 H88 126.6 . . ? C88 C89 C90 110.6(13) . . ? C88 C89 Re2 69.7(9) . . ? C90 C89 Re2 73.1(8) . . ? C88 C89 H89 124.7 . . ? C90 C89 H89 124.7 . . ? Re2 C89 H89 124.7 . . ? C89 C90 C86 106.3(12) . . ? C89 C90 Re2 70.2(8) . . ? C86 C90 Re2 68.5(8) . . ? C89 C90 H90 126.8 . . ? C86 C90 H90 126.8 . . ? Re2 C90 H90 126.8 . . ? C2S C1S H1SC 109.5 . . ? C2S C1S H1SA 109.5 . . ? H1SC C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SC C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C3S C2S C1S 97(3) . . ? C3S C2S H2SA 112.3 . . ? C1S C2S H2SA 112.3 . . ? C3S C2S H2SB 112.3 . . ? C1S C2S H2SB 112.3 . . ? H2SA C2S H2SB 109.9 . . ? C4S C3S C2S 102(3) . . ? C4S C3S H3SB 111.4 . . ? C2S C3S H3SB 111.4 . . ? C4S C3S H3SA 111.4 . . ? C2S C3S H3SA 111.4 . . ? H3SB C3S H3SA 109.3 . . ? C3S C4S C5S 109(4) . . ? C3S C4S C6S 120(4) . . ? C5S C4S C6S 101(4) . . ? C3S C4S H4S 108.8 . . ? C5S C4S H4S 108.8 . . ? C6S C4S H4S 110.0 . . ? C4S C5S H5SC 109.5 . . ? C4S C5S H5SB 109.5 . . ? H5SC C5S H5SB 109.5 . . ? C4S C5S H5SA 109.5 . . ? H5SC C5S H5SA 109.5 . . ? H5SB C5S H5SA 109.5 . . ? C4S C6S H6SB 109.5 . . ? C4S C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? C4S C6S H6SA 109.5 . . ? H6SB C6S H6SA 109.5 . . ? H6SC C6S H6SA 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.13 _refine_diff_density_min -2.12 _refine_diff_density_rms 0.28 #===END of CIF # Attachment '6.cif.txt' data_udksia _database_code_depnum_ccdc_archive 'CCDC 777013' #TrackingRef '6.cif.txt' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H64 N4 Si5 U' _chemical_formula_sum 'C37 H64 N4 Si5 U' _chemical_formula_weight 943.40 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 16.1847(4) _cell_length_b 11.3466(2) _cell_length_c 23.8954(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.371(2) _cell_angle_gamma 90.00 _cell_volume 4375.42(16) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 12526 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 3.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44442 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.018 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7716 _reflns_number_gt 6870 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)' _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^)+(0.024P)^2^+5.295P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7716 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _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 U1 U 0.256837(6) 0.252277(8) 0.080708(4) 0.01340(4) Uani 1 1 d . . . Si1 Si 0.36388(4) 0.50472(6) 0.10938(3) 0.01424(14) Uani 1 1 d . . . Si2 Si 0.22959(4) 0.49658(6) 0.00313(3) 0.01405(14) Uani 1 1 d . . . Si3 Si 0.17173(4) 0.49812(6) 0.12925(3) 0.01322(14) Uani 1 1 d . . . Si4 Si 0.16298(4) -0.02331(6) 0.06710(3) 0.01830(16) Uani 1 1 d . . . Si5 Si 0.33829(5) 0.00490(6) 0.02886(3) 0.01722(15) Uani 1 1 d . . . N1 N 0.35649(13) 0.35810(19) 0.12873(9) 0.0158(5) Uani 1 1 d . . . N2 N 0.25166(13) 0.34667(19) -0.00048(8) 0.0154(5) Uani 1 1 d . . . N3 N 0.15655(13) 0.34677(18) 0.12249(8) 0.0146(4) Uani 1 1 d . . . N4 N 0.25121(14) 0.05917(19) 0.05810(9) 0.0172(5) Uani 1 1 d . . . C1 C 0.25377(14) 0.5378(2) 0.07963(9) 0.0133(5) Uani 1 1 d . . . H1A H 0.2521 0.6258 0.0789 0.016 Uiso 1 1 calc R . . C2 C 0.44316(16) 0.5266(2) 0.05731(11) 0.0206(6) Uani 1 1 d . . . H2A H 0.4377 0.6060 0.0414 0.031 Uiso 1 1 calc R . . H2B H 0.4346 0.4682 0.0272 0.031 Uiso 1 1 calc R . . H2C H 0.4987 0.5169 0.0761 0.031 Uiso 1 1 calc R . . C3 C 0.39756(17) 0.6048(2) 0.16852(11) 0.0220(6) Uani 1 1 d . . . H3A H 0.3998 0.6860 0.1547 0.033 Uiso 1 1 calc R . . H3B H 0.4526 0.5811 0.1845 0.033 Uiso 1 1 calc R . . H3C H 0.3580 0.6001 0.1975 0.033 Uiso 1 1 calc R . . C4 C 0.41403(16) 0.2790(2) 0.15472(10) 0.0156(5) Uani 1 1 d . . . C5 C 0.50037(16) 0.2896(2) 0.15399(11) 0.0171(5) Uani 1 1 d . . . H5A H 0.5233 0.3592 0.1394 0.021 Uiso 1 1 calc R . . C6 C 0.55291(16) 0.1994(2) 0.17429(10) 0.0181(6) Uani 1 1 d . . . C7 C 0.64562(17) 0.2140(3) 0.17519(12) 0.0244(6) Uani 1 1 d . . . H7A H 0.6592 0.2631 0.1434 0.037 Uiso 1 1 calc R . . H7B H 0.6716 0.1364 0.1723 0.037 Uiso 1 1 calc R . . H7C H 0.6662 0.2518 0.2104 0.037 Uiso 1 1 calc R . . C8 C 0.51883(17) 0.0965(2) 0.19481(11) 0.0211(6) Uani 1 1 d . . . H8A H 0.5545 0.0331 0.2064 0.025 Uiso 1 1 calc R . . C9 C 0.43413(17) 0.0848(2) 0.19867(11) 0.0200(6) Uani 1 1 d . . . C10 C 0.39841(18) -0.0219(3) 0.22567(12) 0.0270(7) Uani 1 1 d . . . H10A H 0.4384 -0.0867 0.2262 0.041 Uiso 1 1 calc R . . H10B H 0.3471 -0.0456 0.2042 0.041 Uiso 1 1 calc R . . H10C H 0.3864 -0.0026 0.2642 0.041 Uiso 1 1 calc R . . C11 C 0.38276(16) 0.1774(2) 0.17942(10) 0.0179(6) Uani 1 1 d . . . H11A H 0.3249 0.1716 0.1831 0.022 Uiso 1 1 calc R . . C12 C 0.11854(16) 0.5201(2) -0.02260(11) 0.0202(6) Uani 1 1 d . . . H12A H 0.1042 0.6034 -0.0186 0.030 Uiso 1 1 calc R . . H12B H 0.0829 0.4718 -0.0005 0.030 Uiso 1 1 calc R . . H12C H 0.1105 0.4973 -0.0622 0.030 Uiso 1 1 calc R . . C13 C 0.29014(18) 0.5852(2) -0.04572(11) 0.0214(6) Uani 1 1 d . . . H13A H 0.2808 0.6693 -0.0394 0.032 Uiso 1 1 calc R . . H13B H 0.2720 0.5652 -0.0846 0.032 Uiso 1 1 calc R . . H13C H 0.3493 0.5674 -0.0387 0.032 Uiso 1 1 calc R . . C14 C 0.24666(16) 0.2913(2) -0.05447(10) 0.0151(5) Uani 1 1 d . . . C15 C 0.17280(18) 0.2376(2) -0.07616(12) 0.0189(6) Uani 1 1 d . . . H15A H 0.1253 0.2401 -0.0552 0.023 Uiso 1 1 calc R . . C16 C 0.16815(17) 0.1812(2) -0.12768(11) 0.0216(6) Uani 1 1 d . . . C17 C 0.0878(2) 0.1239(3) -0.15032(13) 0.0333(7) Uani 1 1 d . . . H17A H 0.0422 0.1530 -0.1294 0.050 Uiso 1 1 calc R . . H17B H 0.0923 0.0382 -0.1460 0.050 Uiso 1 1 calc R . . H17C H 0.0771 0.1435 -0.1901 0.050 Uiso 1 1 calc R . . C18 C 0.23773(18) 0.1784(2) -0.15839(11) 0.0224(6) Uani 1 1 d . . . H18A H 0.2346 0.1397 -0.1937 0.027 Uiso 1 1 calc R . . C19 C 0.31175(18) 0.2312(2) -0.13841(12) 0.0199(6) Uani 1 1 d . . . C20 C 0.3878(2) 0.2254(3) -0.17123(13) 0.0320(7) Uani 1 1 d . . . H20A H 0.3723 0.1962 -0.2092 0.048 Uiso 1 1 calc R . . H20B H 0.4285 0.1721 -0.1523 0.048 Uiso 1 1 calc R . . H20C H 0.4120 0.3044 -0.1735 0.048 Uiso 1 1 calc R . . C21 C 0.31567(17) 0.2882(2) -0.08653(11) 0.0184(6) Uani 1 1 d . . . H21A H 0.3657 0.3254 -0.0727 0.022 Uiso 1 1 calc R . . C22 C 0.20399(16) 0.5291(2) 0.20495(10) 0.0185(6) Uani 1 1 d . . . H22A H 0.2141 0.6137 0.2100 0.028 Uiso 1 1 calc R . . H22B H 0.2549 0.4854 0.2161 0.028 Uiso 1 1 calc R . . H22C H 0.1599 0.5042 0.2283 0.028 Uiso 1 1 calc R . . C23 C 0.07602(16) 0.5885(2) 0.11393(11) 0.0202(6) Uani 1 1 d . . . H23A H 0.0902 0.6724 0.1167 0.030 Uiso 1 1 calc R . . H23B H 0.0357 0.5696 0.1412 0.030 Uiso 1 1 calc R . . H23C H 0.0520 0.5710 0.0759 0.030 Uiso 1 1 calc R . . C24 C 0.10137(16) 0.2902(2) 0.15760(11) 0.0163(5) Uani 1 1 d . . . C25 C 0.01537(16) 0.3003(2) 0.14776(11) 0.0181(5) Uani 1 1 d . . . H25A H -0.0069 0.3512 0.1189 0.022 Uiso 1 1 calc R . . C26 C -0.03828(18) 0.2371(2) 0.17944(13) 0.0220(6) Uani 1 1 d . . . C27 C -0.13090(19) 0.2469(3) 0.16724(15) 0.0319(8) Uani 1 1 d . . . H27A H -0.1435 0.3118 0.1409 0.048 Uiso 1 1 calc R . . H27B H -0.1569 0.2621 0.2022 0.048 Uiso 1 1 calc R . . H27C H -0.1525 0.1730 0.1506 0.048 Uiso 1 1 calc R . . C28 C -0.00473(17) 0.1627(2) 0.22188(11) 0.0222(6) Uani 1 1 d . . . H28A H -0.0409 0.1191 0.2435 0.027 Uiso 1 1 calc R . . C29 C 0.08023(17) 0.1511(2) 0.23315(11) 0.0200(6) Uani 1 1 d . . . C30 C 0.11567(19) 0.0694(3) 0.27895(12) 0.0287(7) Uani 1 1 d . . . H30A H 0.0826 -0.0030 0.2788 0.043 Uiso 1 1 calc R . . H30B H 0.1143 0.1084 0.3155 0.043 Uiso 1 1 calc R . . H30C H 0.1731 0.0498 0.2723 0.043 Uiso 1 1 calc R . . C31 C 0.13244(16) 0.2166(2) 0.20122(11) 0.0166(5) Uani 1 1 d . . . H31A H 0.1907 0.2110 0.2093 0.020 Uiso 1 1 calc R . . C32 C 0.14564(18) -0.1472(2) 0.01583(12) 0.0249(6) Uani 1 1 d . . . H32A H 0.1402 -0.1155 -0.0224 0.037 Uiso 1 1 calc R . . H32B H 0.0948 -0.1894 0.0234 0.037 Uiso 1 1 calc R . . H32C H 0.1928 -0.2015 0.0197 0.037 Uiso 1 1 calc R . . C33 C 0.07118(17) 0.0768(3) 0.05544(14) 0.0294(7) Uani 1 1 d . . . H33A H 0.0608 0.0929 0.0152 0.044 Uiso 1 1 calc R . . H33B H 0.0824 0.1511 0.0756 0.044 Uiso 1 1 calc R . . H33C H 0.0224 0.0389 0.0694 0.044 Uiso 1 1 calc R . . C34 C 0.16823(19) -0.0866(3) 0.13977(12) 0.0274(7) Uani 1 1 d . . . H34A H 0.1811 -0.0238 0.1672 0.041 Uiso 1 1 calc R . . H34B H 0.2116 -0.1470 0.1435 0.041 Uiso 1 1 calc R . . H34C H 0.1147 -0.1221 0.1466 0.041 Uiso 1 1 calc R . . C35 C 0.38341(18) -0.1244(2) 0.06928(12) 0.0237(6) Uani 1 1 d . . . H35A H 0.4307 -0.1554 0.0506 0.036 Uiso 1 1 calc R . . H35B H 0.3412 -0.1859 0.0710 0.036 Uiso 1 1 calc R . . H35C H 0.4020 -0.0995 0.1074 0.036 Uiso 1 1 calc R . . C36 C 0.41879(17) 0.1249(2) 0.03199(11) 0.0214(6) Uani 1 1 d . . . H36A H 0.4623 0.1046 0.0073 0.032 Uiso 1 1 calc R . . H36B H 0.4431 0.1331 0.0706 0.032 Uiso 1 1 calc R . . H36C H 0.3929 0.1995 0.0197 0.032 Uiso 1 1 calc R . . C37 C 0.31960(18) -0.0387(2) -0.04641(11) 0.0230(6) Uani 1 1 d . . . H37A H 0.3726 -0.0566 -0.0618 0.035 Uiso 1 1 calc R . . H37B H 0.2924 0.0262 -0.0677 0.035 Uiso 1 1 calc R . . H37C H 0.2840 -0.1086 -0.0493 0.035 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 U1 0.01513(6) 0.01165(6) 0.01335(6) -0.00009(4) 0.00071(4) 0.00037(4) Si1 0.0124(3) 0.0160(3) 0.0141(3) -0.0001(3) -0.0010(3) -0.0007(3) Si2 0.0161(3) 0.0145(3) 0.0113(3) 0.0005(3) -0.0010(3) 0.0005(3) Si3 0.0129(3) 0.0142(3) 0.0125(3) -0.0003(3) 0.0006(3) -0.0003(3) Si4 0.0182(4) 0.0162(4) 0.0202(4) -0.0024(3) -0.0007(3) -0.0015(3) Si5 0.0202(4) 0.0149(4) 0.0164(3) 0.0000(3) 0.0007(3) 0.0019(3) N1 0.0136(11) 0.0177(11) 0.0157(11) 0.0021(9) -0.0012(9) 0.0016(9) N2 0.0172(11) 0.0160(11) 0.0128(11) -0.0011(9) -0.0003(9) 0.0005(9) N3 0.0145(11) 0.0147(11) 0.0147(11) 0.0001(9) 0.0023(9) -0.0017(9) N4 0.0212(12) 0.0152(11) 0.0148(11) -0.0009(9) -0.0010(9) 0.0012(9) C1 0.0131(13) 0.0135(13) 0.0130(12) -0.0006(9) -0.0013(10) -0.0002(10) C2 0.0155(13) 0.0246(15) 0.0218(14) 0.0039(12) 0.0019(11) -0.0010(11) C3 0.0196(14) 0.0247(15) 0.0204(14) -0.0003(12) -0.0056(11) -0.0039(12) C4 0.0177(13) 0.0182(13) 0.0106(12) -0.0013(10) -0.0014(10) 0.0017(11) C5 0.0190(14) 0.0181(13) 0.0138(13) 0.0009(11) -0.0023(11) -0.0014(11) C6 0.0177(14) 0.0232(14) 0.0126(12) -0.0035(11) -0.0031(10) 0.0026(11) C7 0.0171(14) 0.0323(16) 0.0233(15) -0.0005(13) -0.0020(12) 0.0043(12) C8 0.0244(15) 0.0208(14) 0.0170(13) 0.0006(11) -0.0056(11) 0.0071(12) C9 0.0242(14) 0.0199(14) 0.0151(13) -0.0004(11) -0.0034(11) -0.0010(11) C10 0.0304(16) 0.0277(16) 0.0220(14) 0.0074(12) -0.0043(12) -0.0013(13) C11 0.0152(13) 0.0249(15) 0.0130(13) -0.0006(11) -0.0027(10) -0.0006(11) C12 0.0212(14) 0.0201(14) 0.0182(13) -0.0015(11) -0.0048(11) 0.0018(11) C13 0.0277(15) 0.0193(14) 0.0173(13) 0.0032(11) 0.0029(12) -0.0001(12) C14 0.0204(14) 0.0128(12) 0.0116(12) 0.0006(10) -0.0015(10) 0.0016(11) C15 0.0179(14) 0.0194(14) 0.0193(14) 0.0019(11) 0.0005(11) -0.0014(11) C16 0.0259(15) 0.0179(14) 0.0196(14) 0.0000(11) -0.0061(12) -0.0028(11) C17 0.0339(18) 0.0371(18) 0.0277(16) -0.0071(14) -0.0058(14) -0.0093(14) C18 0.0348(16) 0.0192(14) 0.0128(13) -0.0009(11) -0.0011(12) 0.0012(12) C19 0.0274(15) 0.0163(14) 0.0164(13) 0.0012(10) 0.0037(12) 0.0028(11) C20 0.0348(18) 0.0372(18) 0.0252(16) -0.0040(14) 0.0110(14) 0.0022(14) C21 0.0194(14) 0.0166(13) 0.0188(14) 0.0014(11) -0.0003(11) 0.0003(11) C22 0.0188(13) 0.0220(14) 0.0148(13) -0.0018(11) 0.0021(10) -0.0006(11) C23 0.0162(13) 0.0213(14) 0.0233(14) -0.0004(11) 0.0021(11) 0.0008(11) C24 0.0177(13) 0.0121(12) 0.0190(13) -0.0047(11) 0.0017(11) -0.0036(11) C25 0.0175(14) 0.0182(14) 0.0181(13) -0.0004(11) -0.0013(11) -0.0003(11) C26 0.0186(15) 0.0219(15) 0.0258(15) -0.0037(11) 0.0041(12) -0.0025(11) C27 0.0174(15) 0.0365(19) 0.0419(19) 0.0040(14) 0.0037(14) -0.0038(12) C28 0.0231(14) 0.0214(14) 0.0231(14) -0.0003(12) 0.0080(12) -0.0063(12) C29 0.0260(15) 0.0200(14) 0.0141(13) -0.0014(11) 0.0028(11) -0.0011(12) C30 0.0333(17) 0.0293(17) 0.0241(15) 0.0088(13) 0.0060(13) -0.0012(13) C31 0.0128(13) 0.0199(13) 0.0174(13) -0.0019(11) 0.0021(10) -0.0006(11) C32 0.0247(15) 0.0191(14) 0.0304(16) -0.0055(12) -0.0017(12) -0.0018(12) C33 0.0198(15) 0.0272(16) 0.0402(18) -0.0117(14) -0.0043(13) 0.0008(12) C34 0.0281(16) 0.0290(16) 0.0251(15) -0.0009(13) 0.0017(13) -0.0074(13) C35 0.0250(15) 0.0210(15) 0.0253(15) 0.0033(12) 0.0030(12) 0.0046(12) C36 0.0193(14) 0.0234(15) 0.0217(14) 0.0004(11) 0.0019(11) 0.0008(11) C37 0.0276(15) 0.0201(14) 0.0214(14) -0.0034(11) 0.0020(12) 0.0006(12) _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 U1 N1 2.253(2) . ? U1 N2 2.212(2) . ? U1 N3 2.242(2) . ? U1 N4 2.257(2) . ? U1 C4 3.001(3) . ? Si1 N1 1.733(2) . ? Si1 C3 1.862(3) . ? Si1 C2 1.871(3) . ? Si1 C1 1.905(2) . ? Si2 N2 1.742(2) . ? Si2 C13 1.873(3) . ? Si2 C12 1.874(3) . ? Si2 C1 1.899(2) . ? Si3 N3 1.741(2) . ? Si3 C23 1.871(3) . ? Si3 C22 1.877(3) . ? Si3 C1 1.900(2) . ? Si4 N4 1.734(2) . ? Si4 C32 1.872(3) . ? Si4 C33 1.874(3) . ? Si4 C34 1.875(3) . ? Si5 N4 1.733(2) . ? Si5 C37 1.868(3) . ? Si5 C35 1.874(3) . ? Si5 C36 1.882(3) . ? N1 C4 1.404(3) . ? N2 C14 1.432(3) . ? N3 C24 1.424(3) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.404(4) . ? C4 C11 1.407(4) . ? C5 C6 1.393(4) . ? C5 H5A 0.9500 . ? C6 C8 1.396(4) . ? C6 C7 1.508(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.387(4) . ? C8 H8A 0.9500 . ? C9 C11 1.396(4) . ? C9 C10 1.507(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C21 1.402(4) . ? C14 C15 1.405(4) . ? C15 C16 1.385(4) . ? C15 H15A 0.9500 . ? C16 C18 1.390(4) . ? C16 C17 1.515(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.391(4) . ? C18 H18A 0.9500 . ? C19 C21 1.395(4) . ? C19 C20 1.510(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.399(4) . ? C24 C31 1.399(4) . ? C25 C26 1.393(4) . ? C25 H25A 0.9500 . ? C26 C28 1.397(4) . ? C26 C27 1.509(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.387(4) . ? C28 H28A 0.9500 . ? C29 C31 1.395(4) . ? C29 C30 1.514(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 U1 N3 100.29(8) . . ? N2 U1 N1 99.58(8) . . ? N3 U1 N1 91.88(7) . . ? N2 U1 N4 105.19(8) . . ? N3 U1 N4 123.60(8) . . ? N1 U1 N4 130.80(8) . . ? N2 U1 C4 116.21(7) . . ? N3 U1 C4 107.41(7) . . ? N1 U1 C4 26.40(7) . . ? N4 U1 C4 104.84(7) . . ? N1 Si1 C3 113.90(11) . . ? N1 Si1 C2 111.67(12) . . ? C3 Si1 C2 104.37(13) . . ? N1 Si1 C1 101.93(11) . . ? C3 Si1 C1 112.01(12) . . ? C2 Si1 C1 113.28(11) . . ? N2 Si2 C13 111.99(11) . . ? N2 Si2 C12 108.54(11) . . ? C13 Si2 C12 104.69(12) . . ? N2 Si2 C1 105.07(11) . . ? C13 Si2 C1 112.88(12) . . ? C12 Si2 C1 113.77(11) . . ? N3 Si3 C23 114.46(11) . . ? N3 Si3 C22 107.51(11) . . ? C23 Si3 C22 104.55(12) . . ? N3 Si3 C1 106.03(11) . . ? C23 Si3 C1 110.84(12) . . ? C22 Si3 C1 113.62(11) . . ? N4 Si4 C32 114.07(12) . . ? N4 Si4 C33 107.78(12) . . ? C32 Si4 C33 106.27(13) . . ? N4 Si4 C34 110.00(12) . . ? C32 Si4 C34 108.20(14) . . ? C33 Si4 C34 110.45(14) . . ? N4 Si5 C37 113.91(12) . . ? N4 Si5 C35 111.55(12) . . ? C37 Si5 C35 108.49(13) . . ? N4 Si5 C36 107.98(12) . . ? C37 Si5 C36 106.91(13) . . ? C35 Si5 C36 107.73(13) . . ? C4 N1 Si1 132.43(18) . . ? C4 N1 U1 108.04(16) . . ? Si1 N1 U1 115.91(10) . . ? C14 N2 Si2 118.41(17) . . ? C14 N2 U1 124.98(16) . . ? Si2 N2 U1 115.07(10) . . ? C24 N3 Si3 118.74(17) . . ? C24 N3 U1 123.67(16) . . ? Si3 N3 U1 114.28(10) . . ? Si5 N4 Si4 124.12(13) . . ? Si5 N4 U1 114.97(11) . . ? Si4 N4 U1 120.84(11) . . ? Si2 C1 Si3 116.10(12) . . ? Si2 C1 Si1 115.42(12) . . ? Si3 C1 Si1 113.51(12) . . ? Si2 C1 H1A 103.1 . . ? Si3 C1 H1A 103.1 . . ? Si1 C1 H1A 103.1 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 124.6(2) . . ? N1 C4 C11 117.5(2) . . ? C5 C4 C11 117.7(2) . . ? N1 C4 U1 45.56(12) . . ? C5 C4 U1 143.24(18) . . ? C11 C4 U1 81.28(15) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C8 119.3(3) . . ? C5 C6 C7 120.3(3) . . ? C8 C6 C7 120.4(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 121.5(2) . . ? C9 C8 H8A 119.3 . . ? C6 C8 H8A 119.3 . . ? C8 C9 C11 118.2(2) . . ? C8 C9 C10 121.2(2) . . ? C11 C9 C10 120.5(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C4 122.1(2) . . ? C9 C11 H11A 119.0 . . ? C4 C11 H11A 119.0 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C21 C14 C15 118.6(2) . . ? C21 C14 N2 120.7(2) . . ? C15 C14 N2 120.7(2) . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C18 119.2(3) . . ? C15 C16 C17 120.2(3) . . ? C18 C16 C17 120.6(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 C19 121.4(3) . . ? C16 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C18 C19 C21 119.0(3) . . ? C18 C19 C20 121.2(3) . . ? C21 C19 C20 119.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 C14 120.9(3) . . ? C19 C21 H21A 119.6 . . ? C14 C21 H21A 119.6 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C31 118.1(2) . . ? C25 C24 N3 121.6(2) . . ? C31 C24 N3 120.2(2) . . ? C26 C25 C24 121.3(3) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C28 118.8(3) . . ? C25 C26 C27 120.6(3) . . ? C28 C26 C27 120.7(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C26 121.5(3) . . ? C29 C28 H28A 119.2 . . ? C26 C28 H28A 119.2 . . ? C28 C29 C31 118.4(2) . . ? C28 C29 C30 120.9(2) . . ? C31 C29 C30 120.6(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 C24 121.8(2) . . ? C29 C31 H31A 119.1 . . ? C24 C31 H31A 119.1 . . ? Si4 C32 H32A 109.5 . . ? Si4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si5 C35 H35A 109.5 . . ? Si5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si5 C36 H36A 109.5 . . ? Si5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si5 C37 H37A 109.5 . . ? Si5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.04 _refine_diff_density_min -0.43 _refine_diff_density_rms 0.08 #=== END of CIF # Attachment '8.cif.txt' data_udpsiu _database_code_depnum_ccdc_archive 'CCDC 777014' #TrackingRef '8.cif.txt' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H56 N3 Re Si3 U' _chemical_formula_sum 'C41 H56 N3 Re Si3 U' _chemical_formula_weight 1099.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.9356(4) _cell_length_b 15.1651(5) _cell_length_c 33.4591(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.052(3) _cell_angle_gamma 90.00 _cell_volume 8084.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 18125 _cell_measurement_theta_min 3.96 _cell_measurement_theta_max 73.95 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.2586 _exptl_crystal_size_mid 0.1350 _exptl_crystal_size_min 0.0347 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 18.045 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.085 _exptl_absorpt_correction_T_max 0.638 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3613 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% 0 _diffrn_reflns_number 25376 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 67.50 _reflns_number_total 7278 _reflns_number_gt 6354 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _refine_special_details ; ; _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^)+(0.0430P)^2^+953.5198P] 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 7278 _refine_ls_number_parameters 454 _refine_ls_number_restraints 442 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1755 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.150 _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 U1 U 0.22475(3) 0.07587(3) 0.368245(14) 0.01728(15) Uani 1 1 d U . . Re1 Re 0.21808(4) 0.26402(4) 0.348433(19) 0.01778(18) Uani 1 1 d U . . Si1 Si 0.1085(3) -0.1092(3) 0.36710(12) 0.0206(8) Uani 1 1 d U . . Si2 Si 0.2920(3) -0.1148(3) 0.40628(12) 0.0207(8) Uani 1 1 d U . . Si3 Si 0.2695(3) -0.0982(3) 0.31201(12) 0.0210(9) Uani 1 1 d U . . N1 N 0.1143(8) -0.0051(8) 0.3863(3) 0.016(2) Uani 1 1 d U . . N2 N 0.3155(8) -0.0026(9) 0.4040(3) 0.021(2) Uani 1 1 d U . . N3 N 0.2479(8) 0.0144(9) 0.3088(3) 0.018(2) Uani 1 1 d U . . C1 C 0.2247(9) -0.1330(10) 0.3613(4) 0.020(2) Uani 1 1 d U . . H1 H 0.2252 -0.1975 0.3590 0.023 Uiso 1 1 calc R . . C2 C 0.0454(10) -0.1091(12) 0.3191(5) 0.027(3) Uani 1 1 d U . . H2A H 0.0754 -0.0777 0.2990 0.040 Uiso 1 1 calc R . . H2B H -0.0076 -0.0809 0.3233 0.040 Uiso 1 1 calc R . . H2C H 0.0361 -0.1688 0.3105 0.040 Uiso 1 1 calc R . . C3 C 0.0538(10) -0.1888(11) 0.4001(5) 0.026(3) Uani 1 1 d U . . H3B H -0.0026 -0.1691 0.4043 0.039 Uiso 1 1 calc R . . H3A H 0.0832 -0.1926 0.4253 0.039 Uiso 1 1 calc R . . H3C H 0.0525 -0.2459 0.3877 0.039 Uiso 1 1 calc R . . C4 C 0.0617(9) 0.0304(10) 0.4159(4) 0.017(2) Uani 1 1 d U . . C5 C -0.0256(10) 0.0320(10) 0.4139(5) 0.020(2) Uani 1 1 d U . . H5 H -0.0528 0.0049 0.3923 0.024 Uiso 1 1 calc R . . C6 C -0.0735(10) 0.0725(11) 0.4429(5) 0.023(2) Uani 1 1 d U . . C7 C -0.1677(10) 0.0724(11) 0.4405(5) 0.024(3) Uani 1 1 d U . . H7A H -0.1858 0.0670 0.4130 0.037 Uiso 1 1 calc R . . H7B H -0.1887 0.1265 0.4513 0.037 Uiso 1 1 calc R . . H7C H -0.1889 0.0235 0.4555 0.037 Uiso 1 1 calc R . . C8 C -0.0331(10) 0.1153(11) 0.4751(5) 0.023(2) Uani 1 1 d U . . H8 H -0.0650 0.1439 0.4941 0.028 Uiso 1 1 calc R . . C9 C 0.0538(10) 0.1156(11) 0.4789(4) 0.023(2) Uani 1 1 d U . . C10 C 0.0984(11) 0.1533(12) 0.5150(5) 0.028(3) Uani 1 1 d U . . H10B H 0.1006 0.1098 0.5359 0.042 Uiso 1 1 calc R . . H10A H 0.0685 0.2042 0.5242 0.042 Uiso 1 1 calc R . . H10C H 0.1544 0.1700 0.5081 0.042 Uiso 1 1 calc R . . C11 C 0.1011(10) 0.0727(10) 0.4495(4) 0.019(2) Uani 1 1 d U . . H11 H 0.1593 0.0720 0.4520 0.023 Uiso 1 1 calc R . . C12 C 0.2386(10) -0.1402(11) 0.4545(4) 0.021(3) Uani 1 1 d U . . H12A H 0.1920 -0.1008 0.4577 0.032 Uiso 1 1 calc R . . H12B H 0.2777 -0.1327 0.4764 0.032 Uiso 1 1 calc R . . H12C H 0.2187 -0.1999 0.4540 0.032 Uiso 1 1 calc R . . C13 C 0.3861(10) -0.1872(12) 0.4060(5) 0.029(4) Uani 1 1 d U . . H13B H 0.3693 -0.2468 0.4005 0.043 Uiso 1 1 calc R . . H13A H 0.4140 -0.1847 0.4317 0.043 Uiso 1 1 calc R . . H13C H 0.4238 -0.1674 0.3858 0.043 Uiso 1 1 calc R . . C14 C 0.3794(10) 0.0339(10) 0.4314(4) 0.021(2) Uani 1 1 d U . . C15 C 0.3581(11) 0.0645(10) 0.4682(4) 0.023(2) Uani 1 1 d U . . H15 H 0.3035 0.0574 0.4770 0.027 Uiso 1 1 calc R . . C16 C 0.4176(11) 0.1064(11) 0.4929(5) 0.027(2) Uani 1 1 d U . . C17 C 0.3918(12) 0.1414(12) 0.5336(5) 0.034(3) Uani 1 1 d U . . H17A H 0.3319 0.1481 0.5339 0.051 Uiso 1 1 calc R . . H17B H 0.4180 0.1975 0.5383 0.051 Uiso 1 1 calc R . . H17C H 0.4092 0.1006 0.5540 0.051 Uiso 1 1 calc R . . C18 C 0.4997(11) 0.1123(12) 0.4803(5) 0.029(3) Uani 1 1 d U . . H18 H 0.5399 0.1384 0.4970 0.034 Uiso 1 1 calc R . . C19 C 0.5234(11) 0.0800(12) 0.4431(5) 0.029(2) Uani 1 1 d U . . C20 C 0.6129(11) 0.0846(13) 0.4318(6) 0.036(3) Uani 1 1 d U . . H20B H 0.6465 0.0524 0.4509 0.054 Uiso 1 1 calc R . . H20A H 0.6307 0.1451 0.4314 0.054 Uiso 1 1 calc R . . H20C H 0.6194 0.0592 0.4057 0.054 Uiso 1 1 calc R . . C21 C 0.4614(10) 0.0406(11) 0.4190(5) 0.024(2) Uani 1 1 d U . . H21 H 0.4757 0.0184 0.3941 0.029 Uiso 1 1 calc R . . C22 C 0.3845(10) -0.1198(11) 0.3088(4) 0.024(3) Uani 1 1 d U . . H22B H 0.3956 -0.1806 0.3149 0.036 Uiso 1 1 calc R . . H22A H 0.4142 -0.0829 0.3276 0.036 Uiso 1 1 calc R . . H22C H 0.4028 -0.1070 0.2822 0.036 Uiso 1 1 calc R . . C23 C 0.2204(10) -0.1553(11) 0.2677(5) 0.025(3) Uani 1 1 d U . . H23B H 0.1618 -0.1408 0.2659 0.038 Uiso 1 1 calc R . . H23A H 0.2267 -0.2180 0.2707 0.038 Uiso 1 1 calc R . . H23C H 0.2475 -0.1365 0.2438 0.038 Uiso 1 1 calc R . . C24 C 0.2555(10) 0.0524(11) 0.2704(4) 0.022(2) Uani 1 1 d U . . C25 C 0.3321(11) 0.0684(11) 0.2538(5) 0.025(3) Uani 1 1 d U . . H25 H 0.3805 0.0589 0.2692 0.031 Uiso 1 1 calc R . . C26 C 0.3399(11) 0.0988(11) 0.2143(5) 0.028(2) Uani 1 1 d U . . C27 C 0.4237(12) 0.1160(14) 0.1966(5) 0.037(3) Uani 1 1 d U . . H27A H 0.4167 0.1521 0.1732 0.056 Uiso 1 1 calc R . . H27B H 0.4492 0.0611 0.1894 0.056 Uiso 1 1 calc R . . H27C H 0.4589 0.1460 0.2158 0.056 Uiso 1 1 calc R . . C28 C 0.2658(11) 0.1114(11) 0.1919(5) 0.027(3) Uani 1 1 d U . . H28 H 0.2697 0.1293 0.1654 0.032 Uiso 1 1 calc R . . C29 C 0.1873(11) 0.0983(11) 0.2076(5) 0.027(2) Uani 1 1 d U . . C30 C 0.1074(12) 0.1153(12) 0.1838(5) 0.032(3) Uani 1 1 d U . . H30B H 0.0725 0.1552 0.1983 0.048 Uiso 1 1 calc R . . H30A H 0.0781 0.0607 0.1796 0.048 Uiso 1 1 calc R . . H30C H 0.1209 0.1407 0.1584 0.048 Uiso 1 1 calc R . . C31 C 0.1830(11) 0.0656(11) 0.2466(4) 0.025(3) Uani 1 1 d U . . H31 H 0.1309 0.0523 0.2570 0.030 Uiso 1 1 calc R . . C32 C 0.3481(9) 0.2106(11) 0.3519(5) 0.023(2) Uani 1 1 d U . . H1B H 0.3595 0.1523 0.3453 0.027 Uiso 1 1 calc R . . C33 C 0.3289(9) 0.2427(11) 0.3915(5) 0.022(2) Uani 1 1 d U . . H33 H 0.3301 0.2097 0.4149 0.026 Uiso 1 1 calc R . . C34 C 0.3080(10) 0.3338(11) 0.3881(5) 0.026(2) Uani 1 1 d U . . H34 H 0.2891 0.3708 0.4082 0.032 Uiso 1 1 calc R . . C35 C 0.3231(10) 0.3571(12) 0.3455(5) 0.027(2) Uani 1 1 d U . . H35 H 0.3176 0.4131 0.3344 0.033 Uiso 1 1 calc R . . C36 C 0.3465(9) 0.2816(11) 0.3251(5) 0.023(2) Uani 1 1 d U . . H36 H 0.3590 0.2786 0.2981 0.027 Uiso 1 1 calc R . . C37 C 0.1042(9) 0.1937(12) 0.3267(5) 0.024(2) Uani 1 1 d U . . H1A H 0.1047 0.1332 0.3222 0.029 Uiso 1 1 calc R . . C38 C 0.0838(9) 0.2351(12) 0.3644(5) 0.024(2) Uani 1 1 d U . . H38 H 0.0674 0.2075 0.3878 0.029 Uiso 1 1 calc R . . C39 C 0.0941(10) 0.3254(12) 0.3579(5) 0.026(2) Uani 1 1 d U . . H39 H 0.0869 0.3699 0.3766 0.031 Uiso 1 1 calc R . . C40 C 0.1174(10) 0.3370(12) 0.3178(5) 0.025(2) Uani 1 1 d U . . H40 H 0.1276 0.3916 0.3062 0.030 Uiso 1 1 calc R . . C41 C 0.1231(10) 0.2584(11) 0.2980(5) 0.023(2) Uani 1 1 d U . . H41 H 0.1365 0.2495 0.2714 0.028 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 U1 0.0161(3) 0.0204(3) 0.0152(3) -0.00026(19) -0.00085(18) -0.0003(2) Re1 0.0165(3) 0.0203(3) 0.0164(3) 0.0007(3) -0.0025(2) -0.0017(3) Si1 0.019(2) 0.025(2) 0.0171(19) -0.0009(16) 0.0009(16) 0.0003(17) Si2 0.018(2) 0.028(2) 0.0156(19) 0.0013(16) -0.0008(15) -0.0005(17) Si3 0.024(2) 0.024(2) 0.0144(18) -0.0007(16) 0.0003(16) 0.0013(18) N1 0.016(5) 0.022(5) 0.012(5) 0.000(4) 0.001(4) -0.011(4) N2 0.021(5) 0.031(5) 0.011(5) 0.002(4) -0.008(4) 0.005(4) N3 0.019(5) 0.029(4) 0.007(4) -0.001(4) -0.003(4) -0.010(4) C1 0.022(5) 0.021(6) 0.015(5) 0.014(5) -0.004(4) 0.005(5) C2 0.024(8) 0.030(9) 0.026(7) -0.012(6) -0.004(6) -0.004(7) C3 0.022(8) 0.026(7) 0.030(8) -0.006(6) 0.008(6) -0.002(6) C4 0.017(4) 0.019(5) 0.017(5) 0.004(4) 0.003(4) -0.004(4) C5 0.017(5) 0.022(6) 0.022(5) 0.001(5) 0.005(4) -0.001(5) C6 0.021(5) 0.023(5) 0.024(5) -0.002(4) 0.005(4) 0.000(5) C7 0.023(6) 0.025(7) 0.026(7) -0.003(6) 0.007(5) 0.005(6) C8 0.026(5) 0.024(6) 0.019(5) 0.000(5) 0.004(4) -0.001(5) C9 0.027(5) 0.026(5) 0.017(5) 0.003(4) -0.002(4) 0.000(5) C10 0.032(7) 0.033(7) 0.019(6) -0.005(5) -0.001(5) 0.000(6) C11 0.019(5) 0.023(5) 0.015(5) 0.004(4) -0.001(4) -0.003(5) C12 0.023(8) 0.024(8) 0.018(6) 0.000(6) -0.002(5) 0.004(6) C13 0.009(7) 0.035(8) 0.041(10) 0.006(8) -0.002(6) 0.009(6) C14 0.023(5) 0.024(5) 0.017(5) 0.005(4) -0.007(4) 0.002(4) C15 0.028(5) 0.021(6) 0.019(5) 0.005(4) -0.006(4) 0.003(5) C16 0.035(5) 0.026(5) 0.021(5) 0.004(4) -0.005(4) -0.002(5) C17 0.045(8) 0.033(7) 0.023(6) 0.004(6) -0.005(6) -0.002(7) C18 0.032(5) 0.030(6) 0.024(5) 0.009(5) -0.009(5) -0.004(5) C19 0.027(5) 0.033(6) 0.027(5) 0.010(5) -0.007(4) -0.001(5) C20 0.029(6) 0.044(8) 0.034(7) 0.009(7) -0.005(6) -0.005(7) C21 0.024(5) 0.027(6) 0.021(5) 0.008(5) -0.007(4) 0.001(5) C22 0.031(6) 0.025(8) 0.017(7) 0.008(6) -0.003(5) -0.005(6) C23 0.024(8) 0.029(8) 0.024(7) -0.008(6) 0.000(6) 0.004(7) C24 0.028(5) 0.025(5) 0.014(4) 0.002(4) -0.003(4) -0.004(5) C25 0.031(5) 0.027(6) 0.018(5) 0.005(5) 0.000(4) -0.002(5) C26 0.036(5) 0.030(6) 0.019(5) 0.001(5) 0.001(4) -0.005(5) C27 0.038(7) 0.045(8) 0.030(7) 0.000(7) 0.008(6) -0.010(7) C28 0.041(5) 0.025(6) 0.014(5) -0.002(5) -0.003(4) 0.001(5) C29 0.037(5) 0.029(6) 0.016(5) 0.002(5) -0.007(4) 0.004(5) C30 0.040(7) 0.032(7) 0.024(6) 0.000(6) -0.012(6) 0.004(7) C31 0.032(5) 0.030(6) 0.014(5) 0.002(5) -0.004(4) 0.000(5) C32 0.014(4) 0.030(5) 0.024(5) 0.006(4) -0.009(4) -0.001(4) C33 0.016(5) 0.028(5) 0.021(5) 0.009(4) -0.013(4) -0.008(4) C34 0.026(5) 0.028(5) 0.024(5) 0.006(4) -0.014(4) -0.009(4) C35 0.026(5) 0.029(5) 0.028(5) 0.008(4) -0.006(5) -0.009(4) C36 0.014(4) 0.032(5) 0.023(5) 0.011(4) -0.009(4) -0.004(4) C37 0.015(4) 0.033(5) 0.024(5) 0.001(4) -0.009(4) 0.002(4) C38 0.014(3) 0.037(5) 0.022(5) 0.005(4) -0.003(4) 0.003(4) C39 0.021(4) 0.035(5) 0.021(5) 0.001(4) -0.004(4) 0.012(4) C40 0.021(5) 0.034(5) 0.020(5) 0.003(4) -0.009(4) 0.003(4) C41 0.018(5) 0.034(6) 0.017(4) 0.003(4) -0.012(4) 0.001(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 U1 N2 2.207(12) . ? U1 N3 2.232(12) . ? U1 N1 2.239(12) . ? U1 Re1 2.9307(8) . ? Re1 C40 2.189(15) . ? Re1 C35 2.192(16) . ? Re1 C34 2.206(15) . ? Re1 C39 2.211(16) . ? Re1 C37 2.216(16) . ? Re1 C36 2.219(16) . ? Re1 C32 2.225(15) . ? Re1 C41 2.247(14) . ? Re1 C38 2.258(16) . ? Re1 C33 2.281(14) . ? Si1 N1 1.707(13) . ? Si1 C3 1.864(17) . ? Si1 C2 1.879(16) . ? Si1 C1 1.901(16) . ? Si2 N2 1.745(14) . ? Si2 C1 1.852(15) . ? Si2 C13 1.859(16) . ? Si2 C12 1.876(15) . ? Si3 N3 1.745(14) . ? Si3 C22 1.867(17) . ? Si3 C23 1.876(16) . ? Si3 C1 1.884(15) . ? N1 C4 1.416(19) . ? N2 C14 1.466(19) . ? N3 C24 1.415(19) . ? C1 H1 0.9800 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3B 0.9600 . ? C3 H3A 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.39(2) . ? C4 C11 1.43(2) . ? C5 C6 1.39(2) . ? C5 H5 0.9300 . ? C6 C8 1.40(2) . ? C6 C7 1.50(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.39(2) . ? C8 H8 0.9300 . ? C9 C11 1.41(2) . ? C9 C10 1.50(2) . ? C10 H10B 0.9600 . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13B 0.9600 . ? C13 H13A 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.37(2) . ? C14 C21 1.38(2) . ? C15 C16 1.40(2) . ? C15 H15 0.9300 . ? C16 C18 1.38(2) . ? C16 C17 1.52(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.40(2) . ? C18 H18 0.9300 . ? C19 C21 1.40(2) . ? C19 C20 1.48(2) . ? C20 H20B 0.9600 . ? C20 H20A 0.9600 . ? C20 H20C 0.9600 . ? C21 H21 0.9300 . ? C22 H22B 0.9600 . ? C22 H22A 0.9600 . ? C22 H22C 0.9600 . ? C23 H23B 0.9600 . ? C23 H23A 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.37(2) . ? C24 C31 1.41(2) . ? C25 C26 1.41(2) . ? C25 H25 0.9300 . ? C26 C28 1.40(2) . ? C26 C27 1.49(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.38(2) . ? C28 H28 0.9300 . ? C29 C31 1.40(2) . ? C29 C30 1.51(2) . ? C30 H30B 0.9600 . ? C30 H30A 0.9600 . ? C30 H30C 0.9600 . ? C31 H31 0.9300 . ? C32 C36 1.40(2) . ? C32 C33 1.45(2) . ? C32 H1B 0.9300 . ? C33 C34 1.43(2) . ? C33 H33 0.9300 . ? C34 C35 1.49(2) . ? C34 H34 0.9300 . ? C35 C36 1.39(2) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C41 1.41(2) . ? C37 C38 1.45(2) . ? C37 H1A 0.9300 . ? C38 C39 1.40(2) . ? C38 H38 0.9300 . ? C39 C40 1.41(2) . ? C39 H39 0.9300 . ? C40 C41 1.37(2) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? 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 N2 U1 N3 98.0(5) . . ? N2 U1 N1 93.9(5) . . ? N3 U1 N1 98.9(4) . . ? N2 U1 Re1 131.9(4) . . ? N3 U1 Re1 102.2(3) . . ? N1 U1 Re1 124.7(3) . . ? C40 Re1 C35 101.9(6) . . ? C40 Re1 C34 120.1(6) . . ? C35 Re1 C34 39.7(6) . . ? C40 Re1 C39 37.3(6) . . ? C35 Re1 C39 114.8(7) . . ? C34 Re1 C39 106.5(7) . . ? C40 Re1 C37 60.0(6) . . ? C35 Re1 C37 156.4(6) . . ? C34 Re1 C37 161.3(6) . . ? C39 Re1 C37 61.4(6) . . ? C40 Re1 C36 116.6(6) . . ? C35 Re1 C36 36.6(6) . . ? C34 Re1 C36 64.0(6) . . ? C39 Re1 C36 146.2(6) . . ? C37 Re1 C36 134.2(6) . . ? C40 Re1 C32 151.9(6) . . ? C35 Re1 C32 61.7(6) . . ? C34 Re1 C32 63.2(6) . . ? C39 Re1 C32 168.2(6) . . ? C37 Re1 C32 126.7(6) . . ? C36 Re1 C32 36.7(6) . . ? C40 Re1 C41 35.9(6) . . ? C35 Re1 C41 119.6(6) . . ? C34 Re1 C41 153.0(6) . . ? C39 Re1 C41 62.1(6) . . ? C37 Re1 C41 36.8(6) . . ? C36 Re1 C41 110.7(6) . . ? C32 Re1 C41 129.7(6) . . ? C40 Re1 C38 61.3(6) . . ? C35 Re1 C38 149.7(7) . . ? C34 Re1 C38 124.0(6) . . ? C39 Re1 C38 36.4(6) . . ? C37 Re1 C38 37.8(6) . . ? C36 Re1 C38 172.0(6) . . ? C32 Re1 C38 143.3(6) . . ? C41 Re1 C38 62.7(6) . . ? C40 Re1 C33 156.9(6) . . ? C35 Re1 C33 62.4(6) . . ? C34 Re1 C33 37.0(6) . . ? C39 Re1 C33 130.8(6) . . ? C37 Re1 C33 139.3(6) . . ? C36 Re1 C33 62.0(6) . . ? C32 Re1 C33 37.5(6) . . ? C41 Re1 C33 166.3(6) . . ? C38 Re1 C33 123.3(6) . . ? C40 Re1 U1 128.4(5) . . ? C35 Re1 U1 127.8(5) . . ? C34 Re1 U1 108.1(4) . . ? C39 Re1 U1 114.0(5) . . ? C37 Re1 U1 68.4(4) . . ? C36 Re1 U1 99.6(4) . . ? C32 Re1 U1 66.7(4) . . ? C41 Re1 U1 98.9(4) . . ? C38 Re1 U1 77.7(4) . . ? C33 Re1 U1 72.2(4) . . ? N1 Si1 C3 113.5(7) . . ? N1 Si1 C2 110.2(7) . . ? C3 Si1 C2 105.0(8) . . ? N1 Si1 C1 99.7(7) . . ? C3 Si1 C1 113.9(7) . . ? C2 Si1 C1 114.9(7) . . ? N2 Si2 C1 103.3(6) . . ? N2 Si2 C13 113.7(7) . . ? C1 Si2 C13 111.3(8) . . ? N2 Si2 C12 109.8(7) . . ? C1 Si2 C12 113.7(7) . . ? C13 Si2 C12 105.2(8) . . ? N3 Si3 C22 111.1(7) . . ? N3 Si3 C23 109.0(7) . . ? C22 Si3 C23 105.6(7) . . ? N3 Si3 C1 104.5(6) . . ? C22 Si3 C1 112.9(7) . . ? C23 Si3 C1 113.8(7) . . ? C4 N1 Si1 125.9(10) . . ? C4 N1 U1 117.3(9) . . ? Si1 N1 U1 116.3(6) . . ? C14 N2 Si2 119.2(10) . . ? C14 N2 U1 125.1(10) . . ? Si2 N2 U1 114.3(6) . . ? C24 N3 Si3 115.7(10) . . ? C24 N3 U1 131.1(10) . . ? Si3 N3 U1 113.0(6) . . ? Si2 C1 Si3 116.5(8) . . ? Si2 C1 Si1 116.1(8) . . ? Si3 C1 Si1 114.9(7) . . ? Si2 C1 H1 101.9 . . ? Si3 C1 H1 101.9 . . ? Si1 C1 H1 101.9 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? C5 C4 N1 125.1(13) . . ? C5 C4 C11 117.1(14) . . ? N1 C4 C11 117.6(13) . . ? C6 C5 C4 122.3(15) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C8 119.3(15) . . ? C5 C6 C7 121.6(14) . . ? C8 C6 C7 119.1(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C6 121.0(15) . . ? C9 C8 H8 119.5 . . ? C6 C8 H8 119.5 . . ? C8 C9 C11 118.7(14) . . ? C8 C9 C10 122.0(15) . . ? C11 C9 C10 119.1(14) . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? C9 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C9 C11 C4 121.5(14) . . ? C9 C11 H11 119.2 . . ? C4 C11 H11 119.2 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13B 109.5 . . ? Si2 C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C15 C14 C21 119.8(15) . . ? C15 C14 N2 120.8(14) . . ? C21 C14 N2 119.3(14) . . ? C14 C15 C16 120.7(16) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C18 C16 C15 118.9(16) . . ? C18 C16 C17 121.4(15) . . ? C15 C16 C17 119.6(16) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 C19 121.4(16) . . ? C16 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C21 117.7(16) . . ? C18 C19 C20 119.2(16) . . ? C21 C19 C20 123.0(16) . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? C19 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? C14 C21 C19 121.3(16) . . ? C14 C21 H21 119.4 . . ? C19 C21 H21 119.4 . . ? Si3 C22 H22B 109.5 . . ? Si3 C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? Si3 C23 H23B 109.5 . . ? Si3 C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? C25 C24 C31 118.1(14) . . ? C25 C24 N3 122.1(14) . . ? C31 C24 N3 119.4(14) . . ? C24 C25 C26 122.2(16) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C28 C26 C25 117.4(16) . . ? C28 C26 C27 120.9(15) . . ? C25 C26 C27 121.7(16) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C26 122.6(15) . . ? C29 C28 H28 118.7 . . ? C26 C28 H28 118.7 . . ? C28 C29 C31 117.7(15) . . ? C28 C29 C30 122.5(15) . . ? C31 C29 C30 119.8(16) . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? C29 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? C29 C31 C24 121.8(16) . . ? C29 C31 H31 119.1 . . ? C24 C31 H31 119.1 . . ? C36 C32 C33 109.0(15) . . ? C36 C32 Re1 71.4(9) . . ? C33 C32 Re1 73.4(9) . . ? C36 C32 H1B 125.5 . . ? C33 C32 H1B 125.5 . . ? Re1 C32 H1B 121.4 . . ? C34 C33 C32 107.8(14) . . ? C34 C33 Re1 68.6(8) . . ? C32 C33 Re1 69.1(8) . . ? C34 C33 H33 126.1 . . ? C32 C33 H33 126.1 . . ? Re1 C33 H33 127.7 . . ? C33 C34 C35 105.3(15) . . ? C33 C34 Re1 74.4(9) . . ? C35 C34 Re1 69.7(9) . . ? C33 C34 H34 127.4 . . ? C35 C34 H34 127.4 . . ? Re1 C34 H34 120.5 . . ? C36 C35 C34 108.9(15) . . ? C36 C35 Re1 72.7(9) . . ? C34 C35 Re1 70.6(9) . . ? C36 C35 H35 125.6 . . ? C34 C35 H35 125.6 . . ? Re1 C35 H35 122.7 . . ? C35 C36 C32 108.8(15) . . ? C35 C36 Re1 70.6(9) . . ? C32 C36 Re1 71.8(9) . . ? C35 C36 H36 125.6 . . ? C32 C36 H36 125.6 . . ? Re1 C36 H36 123.5 . . ? C41 C37 C38 110.2(15) . . ? C41 C37 Re1 72.8(9) . . ? C38 C37 Re1 72.7(9) . . ? C41 C37 H1A 124.9 . . ? C38 C37 H1A 124.9 . . ? Re1 C37 H1A 121.3 . . ? C39 C38 C37 105.1(14) . . ? C39 C38 Re1 70.0(9) . . ? C37 C38 Re1 69.6(9) . . ? C39 C38 H38 127.5 . . ? C37 C38 H38 127.5 . . ? Re1 C38 H38 124.6 . . ? C38 C39 C40 107.7(15) . . ? C38 C39 Re1 73.6(9) . . ? C40 C39 Re1 70.5(9) . . ? C38 C39 H39 126.1 . . ? C40 C39 H39 126.1 . . ? Re1 C39 H39 121.5 . . ? C41 C40 C39 111.9(16) . . ? C41 C40 Re1 74.4(9) . . ? C39 C40 Re1 72.2(9) . . ? C41 C40 H40 124.1 . . ? C39 C40 H40 124.1 . . ? Re1 C40 H40 120.9 . . ? C40 C41 C37 105.1(14) . . ? C40 C41 Re1 69.7(9) . . ? C37 C41 Re1 70.4(8) . . ? C40 C41 H41 127.4 . . ? C37 C41 H41 127.4 . . ? Re1 C41 H41 124.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.405 _refine_diff_density_min -2.045 _refine_diff_density_rms 0.324