# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Stephen Liddle' 'Alexander Blake' 'William Lewis' 'Dipti Patel' _publ_contact_author_name 'Stephen Liddle' _publ_contact_author_email STEPHEN.LIDDLE@NOTTINGHAM.AC.UK _publ_section_title ; Uranium(IV) amide and halide derivatives of two tripodal tris(N-arylamido-dimethylsilyl)methanes ; # Attachment '1.cif' data_sidpna _database_code_depnum_ccdc_archive 'CCDC 757624' #TrackingRef '1.cif' _audit_creation_method 'enCIFer editing of SHELXL-97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H49 N3 Si3' _chemical_formula_sum 'C31 H49 N3 Si3' _chemical_formula_weight 548.00 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2572(15) _cell_length_b 8.9742(8) _cell_length_c 20.6548(17) _cell_angle_alpha 90.00 _cell_angle_beta 110.523(2) _cell_angle_gamma 90.00 _cell_volume 3169.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10962 _cell_measurement_theta_min 2.383 _cell_measurement_theta_max 27.549 _exptl_crystal_description Hexagonal _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9369 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 27443 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.57 _reflns_number_total 7324 _reflns_number_gt 6725 _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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0572P)^2^+1.3531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me and NH from difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7324 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 C1 C 0.28606(8) 0.04465(15) 0.68133(7) 0.0188(3) Uani 1 1 d . . . H1 H 0.2727 0.0956 0.7188 0.023 Uiso 1 1 calc R . . C2 C 0.38370(9) 0.31356(18) 0.65647(9) 0.0299(3) Uani 1 1 d . . . H2A H 0.3589 0.3811 0.6799 0.045 Uiso 1 1 calc R . . H2B H 0.3538 0.3138 0.6067 0.045 Uiso 1 1 calc R . . H2C H 0.4373 0.3469 0.6645 0.045 Uiso 1 1 calc R . . C3 C 0.43816(9) -0.00027(19) 0.64852(8) 0.0291(3) Uani 1 1 d . . . H3A H 0.4886 0.0450 0.6532 0.044 Uiso 1 1 calc R . . H3B H 0.4066 -0.0107 0.5994 0.044 Uiso 1 1 calc R . . H3C H 0.4469 -0.0987 0.6704 0.044 Uiso 1 1 calc R . . C4 C 0.43395(8) 0.19789(16) 0.83381(7) 0.0224(3) Uani 1 1 d . . . C5 C 0.48667(9) 0.17632(16) 0.90109(8) 0.0257(3) Uani 1 1 d . . . H5 H 0.5278 0.1060 0.9090 0.031 Uiso 1 1 calc R . . C6 C 0.48009(9) 0.25578(17) 0.95656(8) 0.0286(3) Uani 1 1 d . . . C7 C 0.53769(12) 0.2300(2) 1.02870(9) 0.0422(4) Uani 1 1 d . . . H7A H 0.5259 0.1351 1.0464 0.063 Uiso 1 1 calc R . . H7B H 0.5337 0.3112 1.0590 0.063 Uiso 1 1 calc R . . H7C H 0.5909 0.2268 1.0275 0.063 Uiso 1 1 calc R . . C8 C 0.41943(9) 0.35801(18) 0.94483(8) 0.0286(3) Uani 1 1 d . . . H8 H 0.4153 0.4142 0.9824 0.034 Uiso 1 1 calc R . . C9 C 0.36459(9) 0.37901(16) 0.87868(8) 0.0250(3) Uani 1 1 d . . . C10 C 0.29688(9) 0.48497(19) 0.86651(9) 0.0317(3) Uani 1 1 d . . . H10A H 0.2687 0.4955 0.8167 0.048 Uiso 1 1 calc R . . H10B H 0.3166 0.5825 0.8864 0.048 Uiso 1 1 calc R . . H10C H 0.2613 0.4457 0.8886 0.048 Uiso 1 1 calc R . . C11 C 0.37228(8) 0.29879(16) 0.82379(7) 0.0231(3) Uani 1 1 d . . . H11 H 0.3350 0.3126 0.7787 0.028 Uiso 1 1 calc R . . C12 C 0.37770(9) -0.22390(19) 0.77102(8) 0.0308(3) Uani 1 1 d . . . H12A H 0.3881 -0.1622 0.8124 0.046 Uiso 1 1 calc R . . H12B H 0.4212 -0.2146 0.7539 0.046 Uiso 1 1 calc R . . H12C H 0.3722 -0.3283 0.7825 0.046 Uiso 1 1 calc R . . C13 C 0.26968(10) -0.28103(18) 0.62561(8) 0.0305(3) Uani 1 1 d . . . H13A H 0.2703 -0.3859 0.6390 0.046 Uiso 1 1 calc R . . H13B H 0.3114 -0.2633 0.6070 0.046 Uiso 1 1 calc R . . H13C H 0.2190 -0.2574 0.5903 0.046 Uiso 1 1 calc R . . C14 C 0.19978(8) -0.17106(16) 0.79438(7) 0.0225(3) Uani 1 1 d . . . C15 C 0.24806(9) -0.06921(17) 0.84122(8) 0.0253(3) Uani 1 1 d . . . H15 H 0.2860 -0.0149 0.8290 0.030 Uiso 1 1 calc R . . C16 C 0.24140(9) -0.04621(17) 0.90556(8) 0.0285(3) Uani 1 1 d . . . C17 C 0.29475(12) 0.0632(2) 0.95570(10) 0.0450(5) Uani 1 1 d . . . H17A H 0.2696 0.1612 0.9494 0.067 Uiso 1 1 calc R . . H17B H 0.3441 0.0707 0.9471 0.067 Uiso 1 1 calc R . . H17C H 0.3052 0.0287 1.0031 0.067 Uiso 1 1 calc R . . C18 C 0.18500(10) -0.12415(18) 0.92293(8) 0.0292(3) Uani 1 1 d . . . H18 H 0.1805 -0.1086 0.9669 0.035 Uiso 1 1 calc R . . C19 C 0.13521(8) -0.22422(17) 0.87706(8) 0.0259(3) Uani 1 1 d . . . C20 C 0.07495(10) -0.3096(2) 0.89695(9) 0.0342(4) Uani 1 1 d . . . H20A H 0.0363 -0.3531 0.8554 0.051 Uiso 1 1 calc R . . H20B H 0.0486 -0.2419 0.9190 0.051 Uiso 1 1 calc R . . H20C H 0.1008 -0.3893 0.9293 0.051 Uiso 1 1 calc R . . C21 C 0.14301(8) -0.24641(17) 0.81327(8) 0.0237(3) Uani 1 1 d . . . H21 H 0.1090 -0.3145 0.7816 0.028 Uiso 1 1 calc R . . C22 C 0.11124(9) 0.00792(19) 0.58868(9) 0.0311(3) Uani 1 1 d . . . H22A H 0.0984 0.0211 0.6306 0.047 Uiso 1 1 calc R . . H22B H 0.1161 -0.0986 0.5805 0.047 Uiso 1 1 calc R . . H22C H 0.0696 0.0511 0.5491 0.047 Uiso 1 1 calc R . . C23 C 0.23346(9) 0.06907(19) 0.52228(8) 0.0285(3) Uani 1 1 d . . . H23A H 0.1915 0.1041 0.4808 0.043 Uiso 1 1 calc R . . H23B H 0.2416 -0.0379 0.5181 0.043 Uiso 1 1 calc R . . H23C H 0.2818 0.1229 0.5273 0.043 Uiso 1 1 calc R . . C24 C 0.13921(8) 0.36863(16) 0.62662(8) 0.0231(3) Uani 1 1 d . . . C25 C 0.13610(8) 0.32208(17) 0.69022(8) 0.0248(3) Uani 1 1 d . . . H25 H 0.1703 0.2456 0.7153 0.030 Uiso 1 1 calc R . . C26 C 0.08375(9) 0.38600(17) 0.71736(8) 0.0256(3) Uani 1 1 d . . . C27 C 0.08072(10) 0.3326(2) 0.78550(9) 0.0346(4) Uani 1 1 d . . . H27A H 0.1049 0.2339 0.7960 0.052 Uiso 1 1 calc R . . H27B H 0.0261 0.3266 0.7828 0.052 Uiso 1 1 calc R . . H27C H 0.1092 0.4027 0.8221 0.052 Uiso 1 1 calc R . . C28 C 0.03435(9) 0.49887(17) 0.68088(8) 0.0268(3) Uani 1 1 d . . . H28 H -0.0026 0.5405 0.6987 0.032 Uiso 1 1 calc R . . C29 C 0.03798(8) 0.55216(16) 0.61859(8) 0.0250(3) Uani 1 1 d . . . C30 C -0.01588(10) 0.67526(18) 0.58000(9) 0.0320(3) Uani 1 1 d . . . H30A H -0.0114 0.6878 0.5344 0.048 Uiso 1 1 calc R . . H30B H -0.0013 0.7684 0.6061 0.048 Uiso 1 1 calc R . . H30C H -0.0699 0.6496 0.5744 0.048 Uiso 1 1 calc R . . C31 C 0.09100(8) 0.48710(16) 0.59228(8) 0.0243(3) Uani 1 1 d . . . H31 H 0.0946 0.5236 0.5503 0.029 Uiso 1 1 calc R . . N1 N 0.44425(7) 0.12315(15) 0.77840(7) 0.0248(3) Uani 1 1 d . . . N2 N 0.20764(7) -0.20103(15) 0.73061(6) 0.0245(3) Uani 1 1 d . . . N3 N 0.18832(7) 0.29601(15) 0.59761(7) 0.0258(3) Uani 1 1 d . . . Si1 Si 0.38577(2) 0.12044(4) 0.69127(2) 0.01990(10) Uani 1 1 d . . . Si2 Si 0.28542(2) -0.16024(4) 0.70282(2) 0.02083(10) Uani 1 1 d . . . Si3 Si 0.20578(2) 0.10345(4) 0.59973(2) 0.02105(10) Uani 1 1 d . . . H01 H 0.4775(12) 0.069(2) 0.7886(11) 0.038(6) Uiso 1 1 d . . . H02 H 0.1755(12) -0.264(2) 0.7070(10) 0.037(5) Uiso 1 1 d . . . H03 H 0.1908(12) 0.339(2) 0.5623(11) 0.041(6) Uiso 1 1 d . . . 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 C1 0.0180(6) 0.0211(6) 0.0181(6) -0.0006(5) 0.0074(5) 0.0011(5) C2 0.0263(7) 0.0270(8) 0.0346(8) 0.0060(6) 0.0083(6) -0.0022(6) C3 0.0252(7) 0.0346(8) 0.0310(8) -0.0007(6) 0.0143(6) 0.0032(6) C4 0.0217(6) 0.0200(7) 0.0242(7) -0.0003(5) 0.0065(5) -0.0048(5) C5 0.0256(7) 0.0211(7) 0.0263(7) 0.0030(6) 0.0039(6) -0.0029(5) C6 0.0337(8) 0.0250(7) 0.0227(7) 0.0024(6) 0.0042(6) -0.0077(6) C7 0.0542(11) 0.0373(9) 0.0247(8) 0.0016(7) 0.0008(8) -0.0014(8) C8 0.0375(8) 0.0258(7) 0.0231(7) -0.0020(6) 0.0114(6) -0.0060(6) C9 0.0279(7) 0.0221(7) 0.0273(7) -0.0004(6) 0.0126(6) -0.0054(5) C10 0.0322(8) 0.0328(8) 0.0322(8) -0.0035(7) 0.0138(7) 0.0008(7) C11 0.0219(6) 0.0241(7) 0.0214(6) -0.0005(5) 0.0052(5) -0.0036(5) C12 0.0262(7) 0.0321(8) 0.0334(8) 0.0104(7) 0.0094(6) 0.0035(6) C13 0.0383(8) 0.0254(8) 0.0313(8) -0.0039(6) 0.0164(7) -0.0006(6) C14 0.0228(7) 0.0232(7) 0.0214(7) 0.0023(5) 0.0080(5) 0.0022(5) C15 0.0279(7) 0.0239(7) 0.0261(7) 0.0005(6) 0.0120(6) -0.0039(6) C16 0.0352(8) 0.0254(7) 0.0259(7) -0.0039(6) 0.0120(6) -0.0026(6) C17 0.0592(12) 0.0417(10) 0.0368(9) -0.0159(8) 0.0202(9) -0.0168(9) C18 0.0356(8) 0.0310(8) 0.0254(7) 0.0007(6) 0.0161(7) 0.0041(6) C19 0.0236(7) 0.0265(7) 0.0304(7) 0.0067(6) 0.0129(6) 0.0046(6) C20 0.0302(8) 0.0383(9) 0.0391(9) 0.0103(7) 0.0186(7) 0.0023(7) C21 0.0199(6) 0.0242(7) 0.0267(7) 0.0016(6) 0.0075(6) -0.0007(5) C22 0.0215(7) 0.0357(9) 0.0330(8) 0.0002(7) 0.0056(6) -0.0026(6) C23 0.0310(8) 0.0340(8) 0.0206(7) -0.0002(6) 0.0092(6) 0.0016(6) C24 0.0199(6) 0.0231(7) 0.0258(7) -0.0015(6) 0.0076(6) -0.0021(5) C25 0.0226(7) 0.0251(7) 0.0252(7) 0.0009(6) 0.0065(6) 0.0004(5) C26 0.0256(7) 0.0268(7) 0.0245(7) -0.0039(6) 0.0090(6) -0.0060(6) C27 0.0384(9) 0.0386(9) 0.0317(8) 0.0019(7) 0.0184(7) -0.0012(7) C28 0.0240(7) 0.0272(7) 0.0302(8) -0.0068(6) 0.0106(6) -0.0015(6) C29 0.0221(7) 0.0210(7) 0.0285(7) -0.0053(6) 0.0047(6) -0.0018(5) C30 0.0320(8) 0.0281(8) 0.0345(8) -0.0010(7) 0.0097(7) 0.0060(6) C31 0.0241(7) 0.0235(7) 0.0247(7) -0.0001(6) 0.0078(6) -0.0013(5) N1 0.0204(6) 0.0267(6) 0.0241(6) -0.0010(5) 0.0036(5) 0.0047(5) N2 0.0246(6) 0.0281(6) 0.0222(6) -0.0029(5) 0.0098(5) -0.0072(5) N3 0.0259(6) 0.0273(6) 0.0276(6) 0.0061(5) 0.0136(5) 0.0053(5) Si1 0.01790(18) 0.02120(19) 0.02055(19) 0.00028(14) 0.00667(15) 0.00056(13) Si2 0.02174(19) 0.02125(19) 0.02037(19) 0.00062(14) 0.00847(15) 0.00018(14) Si3 0.01843(18) 0.0250(2) 0.01941(19) 0.00041(15) 0.00627(15) 0.00096(14) _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 C1 Si3 1.8803(14) . ? C1 Si1 1.8859(14) . ? C1 Si2 1.8925(14) . ? C1 H1 1.0000 . ? C2 Si1 1.8715(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.8601(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.3951(19) . ? C4 C5 1.399(2) . ? C4 C11 1.403(2) . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C6 C8 1.392(2) . ? C6 C7 1.510(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.395(2) . ? C8 H8 0.9500 . ? C9 C11 1.391(2) . ? C9 C10 1.509(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C12 Si2 1.8667(16) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si2 1.8654(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.397(2) . ? C14 N2 1.4001(18) . ? C14 C21 1.403(2) . ? C15 C16 1.392(2) . ? C15 H15 0.9500 . ? C16 C18 1.392(2) . ? C16 C17 1.509(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.388(2) . ? C18 H18 0.9500 . ? C19 C21 1.388(2) . ? C19 C20 1.511(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21 0.9500 . ? C22 Si3 1.8682(16) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Si3 1.8645(15) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.398(2) . ? C24 N3 1.4016(19) . ? C24 C31 1.404(2) . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 C28 1.390(2) . ? C26 C27 1.506(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.396(2) . ? C28 H28 0.9500 . ? C29 C31 1.394(2) . ? C29 C30 1.508(2) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? N1 Si1 1.7413(13) . ? N1 H01 0.75(2) . ? N2 Si2 1.7468(13) . ? N2 H02 0.84(2) . ? N3 Si3 1.7550(14) . ? N3 H03 0.84(2) . ? 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 Si3 C1 Si1 114.56(7) . . ? Si3 C1 Si2 114.58(7) . . ? Si1 C1 Si2 114.20(7) . . ? Si3 C1 H1 103.9 . . ? Si1 C1 H1 103.9 . . ? Si2 C1 H1 103.9 . . ? 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 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 120.31(14) . . ? N1 C4 C11 121.43(13) . . ? C5 C4 C11 118.23(14) . . ? C6 C5 C4 121.30(14) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C8 119.21(14) . . ? C5 C6 C7 120.20(15) . . ? C8 C6 C7 120.59(15) . . ? 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 . . ? C6 C8 C9 120.89(14) . . ? C6 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C11 C9 C8 119.05(14) . . ? C11 C9 C10 120.08(14) . . ? C8 C9 C10 120.86(14) . . ? 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 121.27(14) . . ? C9 C11 H11 119.4 . . ? C4 C11 H11 119.4 . . ? 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 . . ? C15 C14 N2 121.97(13) . . ? C15 C14 C21 118.12(13) . . ? N2 C14 C21 119.90(13) . . ? C16 C15 C14 120.89(14) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C18 119.47(14) . . ? C15 C16 C17 120.02(15) . . ? C18 C16 C17 120.51(15) . . ? 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 . . ? C19 C18 C16 121.05(14) . . ? C19 C18 H18 119.5 . . ? C16 C18 H18 119.5 . . ? C18 C19 C21 118.69(14) . . ? C18 C19 C20 120.51(14) . . ? C21 C19 C20 120.79(14) . . ? 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 121.77(14) . . ? C19 C21 H21 119.1 . . ? C14 C21 H21 119.1 . . ? 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 N3 120.36(13) . . ? C25 C24 C31 118.44(13) . . ? N3 C24 C31 121.19(13) . . ? C26 C25 C24 121.03(14) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C28 C26 C25 119.31(14) . . ? C28 C26 C27 120.60(14) . . ? C25 C26 C27 120.09(14) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 C29 121.20(14) . . ? C26 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C31 C29 C28 118.68(14) . . ? C31 C29 C30 120.94(14) . . ? C28 C29 C30 120.36(14) . . ? 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 121.22(14) . . ? C29 C31 H31 119.4 . . ? C24 C31 H31 119.4 . . ? C4 N1 Si1 130.13(11) . . ? C4 N1 H01 114.3(16) . . ? Si1 N1 H01 115.1(16) . . ? C14 N2 Si2 129.20(10) . . ? C14 N2 H02 113.3(14) . . ? Si2 N2 H02 115.8(14) . . ? C24 N3 Si3 125.80(11) . . ? C24 N3 H03 113.2(15) . . ? Si3 N3 H03 114.2(15) . . ? N1 Si1 C3 105.53(7) . . ? N1 Si1 C2 107.85(7) . . ? C3 Si1 C2 107.55(8) . . ? N1 Si1 C1 109.64(6) . . ? C3 Si1 C1 112.07(7) . . ? C2 Si1 C1 113.79(7) . . ? N2 Si2 C13 105.05(7) . . ? N2 Si2 C12 108.09(7) . . ? C13 Si2 C12 107.16(8) . . ? N2 Si2 C1 110.69(6) . . ? C13 Si2 C1 112.08(7) . . ? C12 Si2 C1 113.34(7) . . ? N3 Si3 C23 104.07(7) . . ? N3 Si3 C22 107.27(7) . . ? C23 Si3 C22 109.64(8) . . ? N3 Si3 C1 112.11(6) . . ? C23 Si3 C1 111.22(7) . . ? C22 Si3 C1 112.16(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.434 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.052 # Attachment '2.cif' data_udpsic _database_code_depnum_ccdc_archive 'CCDC 757625' #TrackingRef '2.cif' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H112 Li6 N6 O2 Si6' _chemical_formula_sum 'C70 H112 Li6 N6 O2 Si6' _chemical_formula_weight 1279.84 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5806(11) _cell_length_b 25.054(3) _cell_length_c 14.7926(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.997(2) _cell_angle_gamma 90.00 _cell_volume 3820.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5582 _cell_measurement_theta_min 2.115 _cell_measurement_theta_max 27.475 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART1000 CCD area detector' _diffrn_measurement_method \W _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% 0 _diffrn_reflns_number 23692 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8648 _reflns_number_gt 5915 _reflns_threshold_expression >2sigma(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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0637P)^2^+1.2287P] 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 8648 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 Si1 Si 0.17187(5) 0.06119(2) 0.30145(4) 0.02456(14) Uani 1 1 d . A . Si2 Si 0.26120(5) 0.04886(2) 0.52225(4) 0.02568(14) Uani 1 1 d . A . Si3 Si 0.27511(6) 0.16339(2) 0.41946(4) 0.02944(15) Uani 1 1 d . A . N1 N 0.01300(16) 0.06718(6) 0.31380(11) 0.0247(4) Uani 1 1 d . A . N2 N 0.10124(16) 0.05037(7) 0.53227(11) 0.0254(4) Uani 1 1 d . . . N3 N 0.11406(16) 0.18030(7) 0.38973(12) 0.0281(4) Uani 1 1 d . A . Li1 Li -0.0202(3) 0.01516(14) 0.4154(2) 0.0308(8) Uani 1 1 d . . . Li2 Li 0.0514(3) 0.11212(14) 0.4335(3) 0.0312(8) Uani 1 1 d . A . Li3 Li 0.0003(4) 0.15138(15) 0.2745(3) 0.0359(8) Uani 1 1 d . . . O1 O -0.14521(18) 0.18492(8) 0.19859(13) 0.0593(5) Uani 1 1 d . A . C1 C 0.27648(19) 0.08749(8) 0.41400(14) 0.0250(4) Uani 1 1 d . . . H1 H 0.3667 0.0791 0.4081 0.030 Uiso 1 1 calc R A . C2 C 0.2202(2) -0.00825(8) 0.27434(16) 0.0329(5) Uani 1 1 d . . . H2A H 0.2046 -0.0128 0.2069 0.049 Uiso 1 1 calc R A . H2B H 0.1687 -0.0343 0.2999 0.049 Uiso 1 1 calc R . . H2C H 0.3125 -0.0137 0.3021 0.049 Uiso 1 1 calc R . . C3 C 0.1971(2) 0.10260(9) 0.20008(16) 0.0329(5) Uani 1 1 d . . . H3A H 0.2890 0.1021 0.1982 0.049 Uiso 1 1 calc R A . H3B H 0.1699 0.1394 0.2073 0.049 Uiso 1 1 calc R . . H3C H 0.1453 0.0877 0.1422 0.049 Uiso 1 1 calc R . . C4 C -0.09566(19) 0.05041(8) 0.24712(14) 0.0257(4) Uani 1 1 d . A . C5 C -0.2200(2) 0.05919(8) 0.26382(15) 0.0288(5) Uani 1 1 d . . . H5A H -0.2266 0.0757 0.3204 0.035 Uiso 1 1 calc R A . C6 C -0.3333(2) 0.04478(9) 0.20099(16) 0.0346(5) Uani 1 1 d . A . C7 C -0.3247(2) 0.02041(10) 0.11857(17) 0.0422(6) Uani 1 1 d . . . H7A H -0.4016 0.0102 0.0753 0.051 Uiso 1 1 calc R A . C8 C -0.2046(2) 0.01075(10) 0.09861(16) 0.0404(6) Uani 1 1 d . A . C9 C -0.0923(2) 0.02520(9) 0.16252(15) 0.0333(5) Uani 1 1 d . . . H9A H -0.0106 0.0178 0.1487 0.040 Uiso 1 1 calc R A . C10 C -0.4641(2) 0.05759(11) 0.22005(19) 0.0455(6) Uani 1 1 d . . . H10A H -0.5262 0.0297 0.1933 0.068 Uiso 1 1 calc R A . H10B H -0.4942 0.0921 0.1921 0.068 Uiso 1 1 calc R . . H10C H -0.4569 0.0593 0.2872 0.068 Uiso 1 1 calc R . . C11 C -0.1967(3) -0.01276(14) 0.00567(19) 0.0624(8) Uani 1 1 d . . . H11A H -0.1105 -0.0283 0.0101 0.094 Uiso 1 1 calc R A . H11B H -0.2118 0.0154 -0.0415 0.094 Uiso 1 1 calc R . . H11C H -0.2627 -0.0406 -0.0117 0.094 Uiso 1 1 calc R . . C12 C 0.3850(2) 0.07126(10) 0.62663(16) 0.0378(5) Uani 1 1 d . . . H12A H 0.4691 0.0754 0.6102 0.057 Uiso 1 1 calc R A . H12B H 0.3923 0.0446 0.6760 0.057 Uiso 1 1 calc R . . H12C H 0.3582 0.1055 0.6484 0.057 Uiso 1 1 calc R . . C13 C 0.3125(2) -0.02125(8) 0.50604(16) 0.0323(5) Uani 1 1 d . . . H13A H 0.3975 -0.0210 0.4900 0.048 Uiso 1 1 calc R A . H13B H 0.2487 -0.0382 0.4559 0.048 Uiso 1 1 calc R . . H13C H 0.3182 -0.0413 0.5637 0.048 Uiso 1 1 calc R . . C14 C 0.0503(2) 0.08396(8) 0.59261(14) 0.0262(4) Uani 1 1 d . . . C15 C 0.1069(2) 0.09147(9) 0.68736(16) 0.0343(5) Uani 1 1 d . A . H15A H 0.1853 0.0734 0.7141 0.041 Uiso 1 1 calc R . . C16 C 0.0508(3) 0.12476(10) 0.74284(17) 0.0437(6) Uani 1 1 d . . . C17 C -0.0650(2) 0.15053(9) 0.70481(18) 0.0434(6) Uani 1 1 d . A . H17A H -0.1020 0.1738 0.7425 0.052 Uiso 1 1 calc R . . C18 C -0.1274(2) 0.14306(9) 0.61327(18) 0.0374(5) Uani 1 1 d . . . C19 C -0.0687(2) 0.11027(8) 0.55814(16) 0.0306(5) Uani 1 1 d . A . H19A H -0.1107 0.1055 0.4948 0.037 Uiso 1 1 calc R . . C20 C 0.1144(4) 0.13096(15) 0.8444(2) 0.0732(10) Uani 1 1 d . A . H20A H 0.1011 0.1674 0.8643 0.110 Uiso 1 1 calc R . . H20B H 0.2076 0.1239 0.8539 0.110 Uiso 1 1 calc R . . H20C H 0.0758 0.1056 0.8809 0.110 Uiso 1 1 calc R . . C21 C -0.2578(2) 0.16781(11) 0.5722(2) 0.0529(7) Uani 1 1 d . A . H21A H -0.2792 0.1938 0.6160 0.079 Uiso 1 1 calc R . . H21B H -0.3242 0.1399 0.5600 0.079 Uiso 1 1 calc R . . H21C H -0.2545 0.1858 0.5140 0.079 Uiso 1 1 calc R . . C22 C 0.3861(2) 0.19089(10) 0.3469(2) 0.0468(6) Uani 1 1 d . . . H22A H 0.3963 0.2295 0.3571 0.070 Uiso 1 1 calc R A . H22B H 0.3484 0.1840 0.2811 0.070 Uiso 1 1 calc R . . H22C H 0.4710 0.1735 0.3648 0.070 Uiso 1 1 calc R . . C23 C 0.3498(3) 0.19059(10) 0.53732(19) 0.0471(6) Uani 1 1 d . . . H23A H 0.4371 0.1757 0.5588 0.071 Uiso 1 1 calc R A . H23B H 0.2962 0.1807 0.5808 0.071 Uiso 1 1 calc R . . H23C H 0.3553 0.2296 0.5340 0.071 Uiso 1 1 calc R . . C24 C 0.0795(2) 0.23377(8) 0.40420(15) 0.0287(4) Uani 1 1 d . . . C25 C 0.0024(2) 0.24558(8) 0.46726(16) 0.0316(5) Uani 1 1 d . A . H25A H -0.0235 0.2174 0.5020 0.038 Uiso 1 1 calc R . . C26 C -0.0375(2) 0.29751(9) 0.48055(17) 0.0375(5) Uani 1 1 d . . . C27 C 0.0028(2) 0.33889(9) 0.43146(17) 0.0385(5) Uani 1 1 d . A . H27A H -0.0234 0.3744 0.4404 0.046 Uiso 1 1 calc R . . C28 C 0.0809(2) 0.32904(9) 0.36946(16) 0.0360(5) Uani 1 1 d . . . C29 C 0.1172(2) 0.27708(9) 0.35601(16) 0.0332(5) Uani 1 1 d . A . H29A H 0.1695 0.2705 0.3127 0.040 Uiso 1 1 calc R . . C30 C -0.1201(3) 0.30844(11) 0.5498(2) 0.0569(8) Uani 1 1 d . A . H30A H -0.1190 0.3467 0.5633 0.085 Uiso 1 1 calc R . . H30B H -0.0853 0.2887 0.6072 0.085 Uiso 1 1 calc R . . H30C H -0.2094 0.2970 0.5237 0.085 Uiso 1 1 calc R . . C31 C 0.1271(3) 0.37478(10) 0.3179(2) 0.0516(7) Uani 1 1 d . A . H31A H 0.0801 0.4074 0.3266 0.077 Uiso 1 1 calc R . . H31B H 0.1109 0.3662 0.2517 0.077 Uiso 1 1 calc R . . H31C H 0.2203 0.3803 0.3422 0.077 Uiso 1 1 calc R . . C32 C -0.2449(6) 0.1952(2) 0.2589(4) 0.0518(15) Uani 0.618(9) 1 d P A 1 H32A H -0.3216 0.1719 0.2387 0.062 Uiso 0.618(9) 1 calc PR A 1 H32B H -0.2056 0.1877 0.3249 0.062 Uiso 0.618(9) 1 calc PR A 1 C33 C -0.2834(6) 0.2521(2) 0.2468(4) 0.0673(19) Uani 0.618(9) 1 d P A 1 H33A H -0.3397 0.2611 0.2890 0.101 Uiso 0.618(9) 1 calc PR A 1 H33B H -0.3303 0.2583 0.1826 0.101 Uiso 0.618(9) 1 calc PR A 1 H33C H -0.2057 0.2746 0.2609 0.101 Uiso 0.618(9) 1 calc PR A 1 C32A C -0.2072(7) 0.2311(3) 0.2324(5) 0.038(2) Uani 0.382(9) 1 d P A 2 H32C H -0.2555 0.2530 0.1803 0.045 Uiso 0.382(9) 1 calc PR A 2 H32D H -0.1423 0.2538 0.2737 0.045 Uiso 0.382(9) 1 calc PR A 2 C33A C -0.2975(10) 0.2054(4) 0.2847(8) 0.065(3) Uani 0.382(9) 1 d P A 2 H33D H -0.3448 0.2332 0.3101 0.097 Uiso 0.382(9) 1 calc PR A 2 H33E H -0.2472 0.1838 0.3355 0.097 Uiso 0.382(9) 1 calc PR A 2 H33G H -0.3592 0.1825 0.2426 0.097 Uiso 0.382(9) 1 calc PR A 2 C34 C -0.2103(3) 0.16994(10) 0.10640(17) 0.0465(6) Uani 1 1 d . . . H34A H -0.2647 0.1999 0.0759 0.056 Uiso 1 1 calc R A . H34C H -0.2673 0.1389 0.1086 0.056 Uiso 1 1 calc R . . C35 C -0.1112(3) 0.15605(11) 0.0527(2) 0.0562(7) Uani 1 1 d . A . H35D H -0.1545 0.1487 -0.0119 0.084 Uiso 1 1 calc R . . H35A H -0.0631 0.1243 0.0799 0.084 Uiso 1 1 calc R . . H35B H -0.0510 0.1860 0.0549 0.084 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 Si1 0.0232(3) 0.0281(3) 0.0244(3) -0.0011(2) 0.0094(2) 0.0005(2) Si2 0.0217(3) 0.0304(3) 0.0249(3) -0.0021(2) 0.0051(2) -0.0016(2) Si3 0.0251(3) 0.0269(3) 0.0369(4) -0.0027(2) 0.0081(3) -0.0025(2) N1 0.0213(8) 0.0311(9) 0.0224(9) -0.0034(7) 0.0063(7) -0.0009(7) N2 0.0241(9) 0.0303(9) 0.0231(9) -0.0028(7) 0.0081(7) -0.0023(7) N3 0.0263(9) 0.0269(9) 0.0319(10) -0.0018(7) 0.0082(8) -0.0002(7) Li1 0.032(2) 0.0346(19) 0.0267(19) 0.0018(15) 0.0080(16) -0.0029(15) Li2 0.0295(19) 0.0361(19) 0.029(2) -0.0039(15) 0.0099(16) -0.0019(15) Li3 0.040(2) 0.037(2) 0.030(2) -0.0002(16) 0.0056(17) 0.0023(16) O1 0.0476(11) 0.0723(13) 0.0477(12) -0.0161(10) -0.0108(9) 0.0234(10) C1 0.0204(10) 0.0277(10) 0.0284(11) -0.0018(8) 0.0089(8) -0.0002(8) C2 0.0350(12) 0.0346(11) 0.0301(12) -0.0032(9) 0.0099(10) 0.0039(9) C3 0.0325(12) 0.0383(12) 0.0314(12) 0.0033(10) 0.0145(10) 0.0028(9) C4 0.0260(10) 0.0286(10) 0.0224(11) 0.0014(8) 0.0055(8) -0.0017(8) C5 0.0299(11) 0.0330(11) 0.0239(11) 0.0015(9) 0.0071(9) 0.0001(9) C6 0.0258(11) 0.0405(12) 0.0354(13) 0.0057(10) 0.0027(10) -0.0018(9) C7 0.0330(13) 0.0515(15) 0.0366(14) -0.0018(11) -0.0037(11) -0.0087(11) C8 0.0427(14) 0.0507(14) 0.0252(12) -0.0049(10) 0.0026(10) -0.0038(11) C9 0.0289(12) 0.0433(13) 0.0279(12) -0.0036(10) 0.0070(9) -0.0005(9) C10 0.0238(12) 0.0604(16) 0.0496(16) 0.0058(13) 0.0026(11) 0.0003(11) C11 0.0615(19) 0.088(2) 0.0340(15) -0.0220(15) 0.0041(14) -0.0080(16) C12 0.0285(12) 0.0484(14) 0.0338(13) -0.0006(10) 0.0016(10) -0.0020(10) C13 0.0290(11) 0.0351(12) 0.0343(13) 0.0039(10) 0.0103(10) 0.0028(9) C14 0.0251(10) 0.0284(10) 0.0271(11) -0.0026(8) 0.0099(9) -0.0049(8) C15 0.0360(13) 0.0396(12) 0.0279(12) -0.0049(10) 0.0082(10) -0.0010(9) C16 0.0521(16) 0.0464(14) 0.0353(14) -0.0122(11) 0.0158(12) -0.0046(12) C17 0.0492(15) 0.0385(13) 0.0502(16) -0.0124(11) 0.0272(13) -0.0020(11) C18 0.0334(12) 0.0328(12) 0.0514(16) 0.0006(10) 0.0210(11) -0.0002(9) C19 0.0276(11) 0.0343(11) 0.0320(12) -0.0001(9) 0.0110(9) -0.0033(9) C20 0.091(3) 0.089(2) 0.0384(17) -0.0268(16) 0.0108(17) 0.0090(19) C21 0.0378(14) 0.0488(15) 0.078(2) -0.0009(14) 0.0246(14) 0.0085(11) C22 0.0371(14) 0.0382(13) 0.0696(19) 0.0035(12) 0.0214(13) -0.0065(10) C23 0.0439(15) 0.0343(13) 0.0556(17) -0.0128(12) -0.0050(12) 0.0002(11) C24 0.0246(11) 0.0301(11) 0.0300(12) -0.0018(9) 0.0031(9) 0.0011(8) C25 0.0317(12) 0.0304(11) 0.0331(12) -0.0012(9) 0.0082(10) -0.0015(9) C26 0.0349(13) 0.0393(13) 0.0382(14) -0.0073(10) 0.0082(10) 0.0018(10) C27 0.0356(13) 0.0284(11) 0.0481(15) -0.0048(10) 0.0023(11) 0.0048(9) C28 0.0313(12) 0.0335(12) 0.0391(14) 0.0061(10) -0.0006(10) 0.0010(9) C29 0.0317(12) 0.0347(12) 0.0334(13) 0.0038(9) 0.0075(10) 0.0021(9) C30 0.0672(19) 0.0489(16) 0.0622(19) -0.0117(14) 0.0309(16) 0.0097(13) C31 0.0515(16) 0.0390(14) 0.0618(18) 0.0173(13) 0.0077(14) 0.0026(12) C32 0.046(3) 0.050(3) 0.055(3) 0.005(2) 0.005(3) 0.003(2) C33 0.070(4) 0.052(3) 0.080(4) -0.002(3) 0.017(3) 0.012(3) C32A 0.035(4) 0.036(4) 0.040(4) 0.008(3) 0.005(3) 0.002(3) C33A 0.065(6) 0.057(6) 0.088(7) -0.004(5) 0.048(5) -0.005(4) C34 0.0468(15) 0.0429(14) 0.0410(15) 0.0087(11) -0.0087(12) -0.0018(11) C35 0.0640(19) 0.0519(16) 0.0454(16) 0.0053(13) -0.0033(14) 0.0128(14) _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 Si1 N1 1.7376(17) . ? Si1 C2 1.882(2) . ? Si1 C3 1.891(2) . ? Si1 C1 1.898(2) . ? Si1 Li2 2.861(3) . ? Si1 Li3 2.869(4) . ? Si1 Li1 3.137(3) . ? Si2 N2 1.7323(17) . ? Si2 C13 1.870(2) . ? Si2 C12 1.872(2) . ? Si2 C1 1.909(2) . ? Si2 Li2 2.802(4) . ? Si2 Li1 3.156(4) . ? Si3 N3 1.7145(18) . ? Si3 C23 1.873(3) . ? Si3 C22 1.890(2) . ? Si3 C1 1.903(2) . ? Si3 Li2 2.741(4) . ? N1 C4 1.400(3) . ? N1 Li2 2.060(4) . ? N1 Li1 2.078(4) . ? N1 Li3 2.184(4) . ? N2 C14 1.418(2) . ? N2 Li1 2.081(4) 3_556 ? N2 Li1 2.102(4) . ? N2 Li2 2.112(4) . ? N3 C24 1.418(3) . ? N3 Li3 1.990(4) . ? N3 Li2 1.992(4) . ? Li1 N2 2.081(4) 3_556 ? Li1 C14 2.503(4) 3_556 ? Li1 Li2 2.541(5) . ? Li1 Li1 2.558(7) 3_556 ? Li1 C4 2.592(4) . ? Li2 C14 2.460(4) . ? Li2 C19 2.464(4) . ? Li2 Li3 2.495(5) . ? Li2 C1 2.538(4) . ? Li3 O1 1.887(4) . ? Li3 C4 2.722(4) . ? Li3 C32 2.779(7) . ? O1 C34 1.433(3) . ? O1 C32A 1.472(8) . ? O1 C32 1.549(7) . ? C1 H1 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 1.409(3) . ? C4 C9 1.409(3) . ? C5 C6 1.389(3) . ? C5 H5A 0.9500 . ? C6 C7 1.384(3) . ? C6 C10 1.508(3) . ? C7 C8 1.389(3) . ? C7 H7A 0.9500 . ? C8 C9 1.389(3) . ? C8 C11 1.515(3) . ? C9 H9A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.407(3) . ? C14 C19 1.411(3) . ? C14 Li1 2.503(4) 3_556 ? C15 C16 1.393(3) . ? C15 H15A 0.9500 . ? C16 C17 1.387(4) . ? C16 C20 1.510(4) . ? C17 C18 1.379(4) . ? C17 H17A 0.9500 . ? C18 C19 1.398(3) . ? C18 C21 1.510(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.402(3) . ? C24 C29 1.405(3) . ? C25 C26 1.395(3) . ? C25 H25A 0.9500 . ? C26 C27 1.387(3) . ? C26 C30 1.513(3) . ? C27 C28 1.387(3) . ? C27 H27A 0.9500 . ? C28 C29 1.385(3) . ? C28 C31 1.517(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.482(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C32A C33A 1.502(12) . ? C32A H32C 0.9900 . ? C32A H32D 0.9900 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33G 0.9800 . ? C34 C35 1.491(4) . ? C34 H34A 0.9900 . ? C34 H34C 0.9900 . ? C35 H35D 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C2 114.70(9) . . ? N1 Si1 C3 110.38(9) . . ? C2 Si1 C3 104.16(10) . . ? N1 Si1 C1 105.36(8) . . ? C2 Si1 C1 112.03(10) . . ? C3 Si1 C1 110.29(10) . . ? N1 Si1 Li2 45.56(9) . . ? C2 Si1 Li2 137.89(10) . . ? C3 Si1 Li2 117.43(10) . . ? C1 Si1 Li2 60.51(9) . . ? N1 Si1 Li3 49.46(9) . . ? C2 Si1 Li3 153.13(11) . . ? C3 Si1 Li3 69.83(10) . . ? C1 Si1 Li3 94.28(10) . . ? Li2 Si1 Li3 51.61(11) . . ? N1 Si1 Li1 38.41(9) . . ? C2 Si1 Li1 90.84(10) . . ? C3 Si1 Li1 148.39(10) . . ? C1 Si1 Li1 88.67(9) . . ? Li2 Si1 Li1 49.86(10) . . ? Li3 Si1 Li1 84.16(10) . . ? N2 Si2 C13 110.42(9) . . ? N2 Si2 C12 116.00(10) . . ? C13 Si2 C12 102.60(11) . . ? N2 Si2 C1 109.23(9) . . ? C13 Si2 C1 106.68(9) . . ? C12 Si2 C1 111.37(10) . . ? N2 Si2 Li2 48.81(9) . . ? C13 Si2 Li2 133.91(11) . . ? C12 Si2 Li2 123.38(11) . . ? C1 Si2 Li2 61.82(9) . . ? N2 Si2 Li1 38.63(9) . . ? C13 Si2 Li1 87.30(10) . . ? C12 Si2 Li1 154.08(10) . . ? C1 Si2 Li1 87.93(9) . . ? Li2 Si2 Li1 50.05(10) . . ? N3 Si3 C23 109.63(10) . . ? N3 Si3 C22 118.21(11) . . ? C23 Si3 C22 102.11(13) . . ? N3 Si3 C1 104.64(9) . . ? C23 Si3 C1 113.40(11) . . ? C22 Si3 C1 109.17(10) . . ? N3 Si3 Li2 46.38(10) . . ? C23 Si3 Li2 106.91(12) . . ? C22 Si3 Li2 150.57(12) . . ? C1 Si3 Li2 63.26(10) . . ? C4 N1 Si1 124.09(13) . . ? C4 N1 Li2 137.85(16) . . ? Si1 N1 Li2 97.41(12) . . ? C4 N1 Li1 94.34(15) . . ? Si1 N1 Li1 110.29(13) . . ? Li2 N1 Li1 75.75(15) . . ? C4 N1 Li3 96.35(16) . . ? Si1 N1 Li3 93.34(12) . . ? Li2 N1 Li3 71.92(15) . . ? Li1 N1 Li3 142.01(16) . . ? C14 N2 Si2 125.70(14) . . ? C14 N2 Li1 89.28(15) . 3_556 ? Si2 N2 Li1 120.45(13) . 3_556 ? C14 N2 Li1 121.21(16) . . ? Si2 N2 Li1 110.41(13) . . ? Li1 N2 Li1 75.40(16) 3_556 . ? C14 N2 Li2 85.97(15) . . ? Si2 N2 Li2 93.06(12) . . ? Li1 N2 Li2 140.89(16) 3_556 . ? Li1 N2 Li2 74.17(15) . . ? C24 N3 Si3 118.06(14) . . ? C24 N3 Li3 110.28(17) . . ? Si3 N3 Li3 120.30(14) . . ? C24 N3 Li2 130.17(17) . . ? Si3 N3 Li2 95.09(13) . . ? Li3 N3 Li2 77.58(16) . . ? N1 Li1 N2 156.2(2) . 3_556 ? N1 Li1 N2 99.21(16) . . ? N2 Li1 N2 104.60(16) 3_556 . ? N1 Li1 C14 128.93(18) . 3_556 ? N2 Li1 C14 34.51(8) 3_556 3_556 ? N2 Li1 C14 120.20(17) . 3_556 ? N1 Li1 Li2 51.81(12) . . ? N2 Li1 Li2 148.59(19) 3_556 . ? N2 Li1 Li2 53.09(13) . . ? C14 Li1 Li2 170.15(19) 3_556 . ? N1 Li1 Li1 151.1(3) . 3_556 ? N2 Li1 Li1 52.68(13) 3_556 3_556 ? N2 Li1 Li1 51.92(14) . 3_556 ? C14 Li1 Li1 75.12(16) 3_556 3_556 ? Li2 Li1 Li1 101.6(2) . 3_556 ? N1 Li1 C4 32.59(8) . . ? N2 Li1 C4 124.23(17) 3_556 . ? N2 Li1 C4 130.24(17) . . ? C14 Li1 C4 106.50(15) 3_556 . ? Li2 Li1 C4 78.21(14) . . ? Li1 Li1 C4 171.3(2) 3_556 . ? N1 Li1 Si1 31.30(7) . . ? N2 Li1 Si1 149.42(16) 3_556 . ? N2 Li1 Si1 86.42(12) . . ? C14 Li1 Si1 115.48(13) 3_556 . ? Li2 Li1 Si1 59.42(10) . . ? Li1 Li1 Si1 130.5(2) 3_556 . ? C4 Li1 Si1 57.02(8) . . ? N1 Li1 Si2 84.29(12) . . ? N2 Li1 Si2 116.49(15) 3_556 . ? N2 Li1 Si2 30.96(7) . . ? C14 Li1 Si2 112.63(13) 3_556 . ? Li2 Li1 Si2 57.72(11) . . ? Li1 Li1 Si2 70.01(16) 3_556 . ? C4 Li1 Si2 116.22(12) . . ? Si1 Li1 Si2 61.22(7) . . ? N3 Li2 N1 101.83(17) . . ? N3 Li2 N2 143.5(2) . . ? N1 Li2 N2 99.47(16) . . ? N3 Li2 C14 129.08(18) . . ? N1 Li2 C14 128.55(18) . . ? N2 Li2 C14 35.11(8) . . ? N3 Li2 C19 121.64(17) . . ? N1 Li2 C19 126.70(17) . . ? N2 Li2 C19 63.83(12) . . ? C14 Li2 C19 33.31(8) . . ? N3 Li2 Li3 51.16(13) . . ? N1 Li2 Li3 56.35(13) . . ? N2 Li2 Li3 155.3(2) . . ? C14 Li2 Li3 165.67(19) . . ? C19 Li2 Li3 132.40(18) . . ? N3 Li2 C1 77.43(13) . . ? N1 Li2 C1 77.19(12) . . ? N2 Li2 C1 78.82(13) . . ? C14 Li2 C1 104.21(15) . . ? C19 Li2 C1 137.34(18) . . ? Li3 Li2 C1 89.92(15) . . ? N3 Li2 Li1 154.0(2) . . ? N1 Li2 Li1 52.44(12) . . ? N2 Li2 Li1 52.74(13) . . ? C14 Li2 Li1 76.18(14) . . ? C19 Li2 Li1 82.47(14) . . ? Li3 Li2 Li1 106.34(18) . . ? C1 Li2 Li1 91.20(15) . . ? N3 Li2 Si3 38.53(8) . . ? N1 Li2 Si3 101.41(14) . . ? N2 Li2 Si3 108.08(15) . . ? C14 Li2 Si3 113.39(15) . . ? C19 Li2 Si3 131.67(15) . . ? Li3 Li2 Si3 75.61(13) . . ? C1 Li2 Si3 42.04(7) . . ? Li1 Li2 Si3 133.01(16) . . ? N3 Li2 Si2 110.55(15) . . ? N1 Li2 Si2 94.36(13) . . ? N2 Li2 Si2 38.12(8) . . ? C14 Li2 Si2 64.10(10) . . ? C19 Li2 Si2 97.26(13) . . ? Li3 Li2 Si2 130.22(16) . . ? C1 Li2 Si2 41.52(7) . . ? Li1 Li2 Si2 72.22(13) . . ? Si3 Li2 Si2 72.19(9) . . ? N3 Li2 Si1 85.91(13) . . ? N1 Li2 Si1 37.03(7) . . ? N2 Li2 Si1 93.75(13) . . ? C14 Li2 Si1 128.61(15) . . ? C19 Li2 Si1 152.42(16) . . ? Li3 Li2 Si1 64.36(12) . . ? C1 Li2 Si1 40.61(7) . . ? Li1 Li2 Si1 70.72(12) . . ? Si3 Li2 Si1 68.44(8) . . ? Si2 Li2 Si1 68.91(8) . . ? O1 Li3 N3 127.1(2) . . ? O1 Li3 N1 125.6(2) . . ? N3 Li3 N1 97.72(17) . . ? O1 Li3 Li2 135.4(2) . . ? N3 Li3 Li2 51.26(13) . . ? N1 Li3 Li2 51.73(12) . . ? O1 Li3 C4 95.64(17) . . ? N3 Li3 C4 126.83(18) . . ? N1 Li3 C4 30.75(8) . . ? Li2 Li3 C4 76.60(14) . . ? O1 Li3 C32 32.09(15) . . ? N3 Li3 C32 107.5(2) . . ? N1 Li3 C32 113.8(2) . . ? Li2 Li3 C32 103.55(19) . . ? C4 Li3 C32 92.58(17) . . ? O1 Li3 Si1 147.11(19) . . ? N3 Li3 Si1 85.75(14) . . ? N1 Li3 Si1 37.20(7) . . ? Li2 Li3 Si1 64.03(12) . . ? C4 Li3 Si1 59.47(9) . . ? C32 Li3 Si1 150.74(19) . . ? C34 O1 C32A 112.0(3) . . ? C34 O1 C32 110.4(3) . . ? C32A O1 C32 42.2(3) . . ? C34 O1 Li3 127.06(19) . . ? C32A O1 Li3 120.9(3) . . ? C32 O1 Li3 107.6(2) . . ? Si1 C1 Si3 112.06(11) . . ? Si1 C1 Si2 114.65(10) . . ? Si3 C1 Si2 117.91(10) . . ? Si1 C1 Li2 78.88(11) . . ? Si3 C1 Li2 74.69(10) . . ? Si2 C1 Li2 76.66(10) . . ? Si1 C1 H1 103.3 . . ? Si3 C1 H1 103.3 . . ? Si2 C1 H1 103.3 . . ? Li2 C1 H1 177.5 . . ? 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 118.73(18) . . ? N1 C4 C9 125.41(18) . . ? C5 C4 C9 115.86(19) . . ? N1 C4 Li1 53.07(12) . . ? C5 C4 Li1 89.02(15) . . ? C9 C4 Li1 129.51(17) . . ? N1 C4 Li3 52.90(12) . . ? C5 C4 Li3 99.25(15) . . ? C9 C4 Li3 117.74(16) . . ? Li1 C4 Li3 98.62(13) . . ? C6 C5 C4 122.8(2) . . ? C6 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? C7 C6 C5 119.1(2) . . ? C7 C6 C10 120.2(2) . . ? C5 C6 C10 120.6(2) . . ? C6 C7 C8 120.5(2) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C7 C8 C9 119.5(2) . . ? C7 C8 C11 120.0(2) . . ? C9 C8 C11 120.4(2) . . ? C8 C9 C4 122.2(2) . . ? C8 C9 H9A 118.9 . . ? C4 C9 H9A 118.9 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 . . ? C15 C14 C19 116.28(19) . . ? C15 C14 N2 124.70(19) . . ? C19 C14 N2 118.95(19) . . ? C15 C14 Li2 145.29(17) . . ? C19 C14 Li2 73.50(15) . . ? N2 C14 Li2 58.91(13) . . ? C15 C14 Li1 101.59(16) . 3_556 ? C19 C14 Li1 110.65(16) . 3_556 ? N2 C14 Li1 56.21(12) . 3_556 ? Li2 C14 Li1 105.49(14) . 3_556 ? C16 C15 C14 121.6(2) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C17 C16 C15 119.6(2) . . ? C17 C16 C20 120.7(2) . . ? C15 C16 C20 119.6(2) . . ? C18 C17 C16 121.3(2) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 118.4(2) . . ? C17 C18 C21 122.1(2) . . ? C19 C18 C21 119.5(2) . . ? C18 C19 C14 122.8(2) . . ? C18 C19 Li2 142.87(18) . . ? C14 C19 Li2 73.19(14) . . ? C18 C19 H19A 118.6 . . ? C14 C19 H19A 118.6 . . ? Li2 C19 H19A 58.0 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 C29 116.69(19) . . ? C25 C24 N3 120.57(18) . . ? C29 C24 N3 122.73(19) . . ? C26 C25 C24 122.0(2) . . ? C26 C25 H25A 119.0 . . ? C24 C25 H25A 119.0 . . ? C27 C26 C25 119.0(2) . . ? C27 C26 C30 120.8(2) . . ? C25 C26 C30 120.2(2) . . ? C26 C27 C28 120.8(2) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C29 C28 C27 119.2(2) . . ? C29 C28 C31 120.4(2) . . ? C27 C28 C31 120.3(2) . . ? C28 C29 C24 122.2(2) . . ? C28 C29 H29A 118.9 . . ? C24 C29 H29A 118.9 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 O1 107.2(5) . . ? C33 C32 Li3 128.1(4) . . ? O1 C32 Li3 40.32(17) . . ? C33 C32 H32A 110.3 . . ? O1 C32 H32A 110.3 . . ? Li3 C32 H32A 118.6 . . ? C33 C32 H32B 110.3 . . ? O1 C32 H32B 110.3 . . ? Li3 C32 H32B 70.4 . . ? H32A C32 H32B 108.5 . . ? O1 C32A C33A 102.8(6) . . ? O1 C32A H32C 111.2 . . ? C33A C32A H32C 111.2 . . ? O1 C32A H32D 111.2 . . ? C33A C32A H32D 111.2 . . ? H32C C32A H32D 109.1 . . ? C32A C33A H33D 109.5 . . ? C32A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C32A C33A H33G 109.5 . . ? H33D C33A H33G 109.5 . . ? H33E C33A H33G 109.5 . . ? O1 C34 C35 108.9(2) . . ? O1 C34 H34A 109.9 . . ? C35 C34 H34A 109.9 . . ? O1 C34 H34C 109.9 . . ? C35 C34 H34C 109.9 . . ? H34A C34 H34C 108.3 . . ? C34 C35 H35D 109.5 . . ? C34 C35 H35A 109.5 . . ? H35D C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35D C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.413 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.053 # Attachment '3.cif' data_lidpla _database_code_depnum_ccdc_archive 'CCDC 757626' #TrackingRef '3.cif' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H60 Li3 N3 O2 Si3' _chemical_formula_sum 'C36 H60 Li3 N3 O2 Si3' _chemical_formula_weight 671.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 9.8635(8) _cell_length_b 12.6161(10) _cell_length_c 17.7573(14) _cell_angle_alpha 110.4560(20) _cell_angle_beta 96.7570(20) _cell_angle_gamma 96.8310(20) _cell_volume 2025.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7861 _cell_measurement_theta_min 2.259 _cell_measurement_theta_max 27.363 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17759 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8960 _reflns_number_gt 7246 _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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0661P)^2^+0.6537P] 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 8960 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 C1 C 0.25257(15) 0.13164(12) 0.61849(9) 0.0260(3) Uani 1 1 d . . . H1 H 0.2251 0.0648 0.5655 0.031 Uiso 1 1 calc R . . C2 C -0.06398(18) 0.07523(15) 0.61936(11) 0.0398(4) Uani 1 1 d . . . H2A H -0.0648 0.0591 0.6695 0.060 Uiso 1 1 calc R . . H2B H -0.0551 0.0054 0.5746 0.060 Uiso 1 1 calc R . . H2C H -0.1506 0.1005 0.6057 0.060 Uiso 1 1 calc R . . C3 C 0.02748(18) 0.25128(15) 0.55553(10) 0.0362(4) Uani 1 1 d . . . H3A H -0.0624 0.2752 0.5636 0.054 Uiso 1 1 calc R . . H3B H 0.0184 0.1920 0.5011 0.054 Uiso 1 1 calc R . . H3C H 0.0957 0.3176 0.5606 0.054 Uiso 1 1 calc R . . C4 C 0.03814(15) 0.36234(12) 0.77615(9) 0.0262(3) Uani 1 1 d . . . C5 C -0.10567(17) 0.34947(15) 0.75078(10) 0.0353(4) Uani 1 1 d . . . H5 H -0.1470 0.2963 0.6979 0.042 Uiso 1 1 calc R . . C6 C -0.18823(18) 0.41234(16) 0.80094(10) 0.0389(4) Uani 1 1 d . . . H6 H -0.2849 0.4006 0.7816 0.047 Uiso 1 1 calc R . . C7 C -0.13429(18) 0.49192(14) 0.87857(10) 0.0352(4) Uani 1 1 d . . . C8 C 0.00805(17) 0.50889(14) 0.90355(9) 0.0329(3) Uani 1 1 d . . . H8 H 0.0490 0.5645 0.9557 0.039 Uiso 1 1 calc R . . C9 C 0.09178(16) 0.44592(13) 0.85369(9) 0.0291(3) Uani 1 1 d . . . H9 H 0.1887 0.4600 0.8728 0.035 Uiso 1 1 calc R . . C10 C -0.2278(2) 0.55576(18) 0.93340(11) 0.0469(5) Uani 1 1 d . . . H10A H -0.1715 0.6105 0.9845 0.070 Uiso 1 1 calc R . . H10B H -0.2925 0.5009 0.9453 0.070 Uiso 1 1 calc R . . H10C H -0.2800 0.5973 0.9060 0.070 Uiso 1 1 calc R . . C11 C 0.1703(2) -0.05434(16) 0.69079(13) 0.0504(5) Uani 1 1 d . . . H11A H 0.2054 -0.0944 0.7253 0.076 Uiso 1 1 calc R . . H11B H 0.1416 -0.1089 0.6345 0.076 Uiso 1 1 calc R . . H11C H 0.0907 -0.0208 0.7107 0.076 Uiso 1 1 calc R . . C12 C 0.4570(2) -0.01607(19) 0.66377(12) 0.0536(5) Uani 1 1 d . . . H12A H 0.5456 0.0368 0.6857 0.080 Uiso 1 1 calc R . . H12B H 0.4455 -0.0491 0.6041 0.080 Uiso 1 1 calc R . . H12C H 0.4558 -0.0777 0.6854 0.080 Uiso 1 1 calc R . . C13 C 0.42872(15) 0.17441(13) 0.85771(9) 0.0272(3) Uani 1 1 d . . . C14 C 0.47975(18) 0.27908(15) 0.92314(10) 0.0361(4) Uani 1 1 d . . . H14 H 0.4570 0.3479 0.9186 0.043 Uiso 1 1 calc R . . C15 C 0.5618(2) 0.28545(16) 0.99385(11) 0.0428(4) Uani 1 1 d . . . H15 H 0.5939 0.3583 1.0362 0.051 Uiso 1 1 calc R . . C16 C 0.59856(18) 0.18825(17) 1.00454(10) 0.0383(4) Uani 1 1 d . . . C17 C 0.54775(17) 0.08421(16) 0.94142(10) 0.0367(4) Uani 1 1 d . . . H17 H 0.5704 0.0159 0.9470 0.044 Uiso 1 1 calc R . . C18 C 0.46456(17) 0.07614(14) 0.87005(10) 0.0319(3) Uani 1 1 d . . . H18 H 0.4311 0.0027 0.8287 0.038 Uiso 1 1 calc R . . C19 C 0.6936(2) 0.1968(2) 1.08078(12) 0.0525(5) Uani 1 1 d . . . H19A H 0.6666 0.1294 1.0945 0.079 Uiso 1 1 calc R . . H19B H 0.6861 0.2665 1.1261 0.079 Uiso 1 1 calc R . . H19C H 0.7895 0.2002 1.0710 0.079 Uiso 1 1 calc R . . C20 C 0.33820(19) 0.22188(17) 0.48791(10) 0.0418(4) Uani 1 1 d . . . H20A H 0.2589 0.2609 0.4840 0.063 Uiso 1 1 calc R . . H20B H 0.3129 0.1408 0.4520 0.063 Uiso 1 1 calc R . . H20C H 0.4166 0.2583 0.4713 0.063 Uiso 1 1 calc R . . C21 C 0.56455(18) 0.19051(17) 0.59827(12) 0.0439(4) Uani 1 1 d . . . H21A H 0.6278 0.2435 0.5838 0.066 Uiso 1 1 calc R . . H21B H 0.5579 0.1122 0.5589 0.066 Uiso 1 1 calc R . . H21C H 0.5999 0.1937 0.6531 0.066 Uiso 1 1 calc R . . C22 C 0.48014(16) 0.46646(14) 0.68774(10) 0.0310(3) Uani 1 1 d . . . C23 C 0.49337(19) 0.55517(15) 0.76463(11) 0.0380(4) Uani 1 1 d . . . H23 H 0.4493 0.5398 0.8054 0.046 Uiso 1 1 calc R . . C24 C 0.5679(2) 0.66353(16) 0.78306(12) 0.0451(4) Uani 1 1 d . . . H24 H 0.5729 0.7205 0.8356 0.054 Uiso 1 1 calc R . . C25 C 0.63547(19) 0.69077(16) 0.72650(13) 0.0456(5) Uani 1 1 d . . . C26 C 0.62768(19) 0.60362(17) 0.65161(13) 0.0451(4) Uani 1 1 d . . . H26 H 0.6753 0.6192 0.6121 0.054 Uiso 1 1 calc R . . C27 C 0.55301(18) 0.49443(15) 0.63196(11) 0.0383(4) Uani 1 1 d . . . H27 H 0.5511 0.4375 0.5798 0.046 Uiso 1 1 calc R . . C28 C 0.7134(2) 0.81073(18) 0.74636(16) 0.0629(6) Uani 1 1 d . . . H28A H 0.6491 0.8656 0.7586 0.094 Uiso 1 1 calc R . . H28B H 0.7550 0.8137 0.6995 0.094 Uiso 1 1 calc R . . H28C H 0.7865 0.8306 0.7939 0.094 Uiso 1 1 calc R . . C50 C 0.0055(2) 0.65491(19) 0.75149(14) 0.0543(5) Uani 1 1 d . . . H50A H 0.0454 0.6301 0.7945 0.082 Uiso 1 1 calc R . . H50B H -0.0918 0.6612 0.7553 0.082 Uiso 1 1 calc R . . H50C H 0.0572 0.7298 0.7581 0.082 Uiso 1 1 calc R . . C51 C 0.0140(2) 0.56943(17) 0.67042(13) 0.0489(5) Uani 1 1 d . . . H51A H -0.0490 0.4970 0.6607 0.059 Uiso 1 1 calc R . . H51B H -0.0176 0.5986 0.6275 0.059 Uiso 1 1 calc R . . C52 C 0.2373(2) 0.62732(17) 0.64171(13) 0.0510(5) Uani 1 1 d . . . H52A H 0.3352 0.6360 0.6666 0.061 Uiso 1 1 calc R . . H52B H 0.2081 0.7031 0.6633 0.061 Uiso 1 1 calc R . . C53 C 0.2266(3) 0.5902(3) 0.55175(17) 0.0865(9) Uani 1 1 d . . . H53A H 0.2539 0.5146 0.5301 0.130 Uiso 1 1 calc R . . H53B H 0.2880 0.6459 0.5387 0.130 Uiso 1 1 calc R . . H53C H 0.1307 0.5857 0.5271 0.130 Uiso 1 1 calc R . . C54 C 0.1611(3) 0.1161(2) 0.99511(15) 0.0669(6) Uani 1 1 d . . . H54A H 0.2487 0.1679 1.0041 0.100 Uiso 1 1 calc R . . H54B H 0.1789 0.0501 1.0095 0.100 Uiso 1 1 calc R . . H54C H 0.0986 0.1571 1.0293 0.100 Uiso 1 1 calc R . . C55 C 0.0952(2) 0.07477(18) 0.90695(14) 0.0519(5) Uani 1 1 d . . . H55A H 0.1592 0.0339 0.8728 0.062 Uiso 1 1 calc R . . H55B H 0.0093 0.0193 0.8977 0.062 Uiso 1 1 calc R . . C56 C -0.0680(2) 0.20348(17) 0.90005(12) 0.0459(4) Uani 1 1 d . . . H56A H -0.0621 0.2851 0.9062 0.055 Uiso 1 1 calc R . . H56B H -0.0841 0.1975 0.9525 0.055 Uiso 1 1 calc R . . C57 C -0.1867(2) 0.1338(2) 0.83545(16) 0.0652(6) Uani 1 1 d . . . H57A H -0.1691 0.1362 0.7829 0.098 Uiso 1 1 calc R . . H57B H -0.2712 0.1649 0.8482 0.098 Uiso 1 1 calc R . . H57C H -0.1983 0.0541 0.8325 0.098 Uiso 1 1 calc R . . N1 N 0.12778(13) 0.29805(11) 0.73122(7) 0.0268(3) Uani 1 1 d . . . N2 N 0.34722(13) 0.17361(11) 0.78804(8) 0.0269(3) Uani 1 1 d . . . N3 N 0.39309(14) 0.36334(11) 0.67169(8) 0.0305(3) Uani 1 1 d . . . O1 O 0.15277(13) 0.54624(10) 0.66439(9) 0.0442(3) Uani 1 1 d . . . O2 O 0.06216(13) 0.16674(11) 0.88187(8) 0.0425(3) Uani 1 1 d . . . Si1 Si 0.08678(4) 0.19153(3) 0.63518(2) 0.02548(11) Uani 1 1 d . . . Si2 Si 0.31177(5) 0.06384(4) 0.69445(3) 0.03005(11) Uani 1 1 d . . . Si3 Si 0.38843(4) 0.23276(4) 0.59629(3) 0.02858(11) Uani 1 1 d . . . Li1 Li 0.3387(3) 0.3045(2) 0.75417(16) 0.0299(5) Uani 1 1 d . . . Li2 Li 0.2183(3) 0.4248(2) 0.69022(18) 0.0367(6) Uani 1 1 d . . . Li3 Li 0.1660(3) 0.2196(2) 0.81514(17) 0.0342(6) Uani 1 1 d . . . 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 C1 0.0298(7) 0.0243(7) 0.0211(7) 0.0041(6) 0.0019(6) 0.0101(6) C2 0.0356(9) 0.0308(8) 0.0446(10) 0.0036(7) 0.0082(7) 0.0044(7) C3 0.0377(9) 0.0394(9) 0.0281(8) 0.0077(7) -0.0018(7) 0.0154(7) C4 0.0280(7) 0.0248(7) 0.0243(7) 0.0064(6) 0.0034(6) 0.0076(6) C5 0.0301(8) 0.0392(9) 0.0266(8) 0.0000(7) 0.0003(6) 0.0102(7) C6 0.0307(8) 0.0450(10) 0.0350(9) 0.0056(8) 0.0035(7) 0.0140(7) C7 0.0382(9) 0.0348(9) 0.0321(8) 0.0083(7) 0.0086(7) 0.0150(7) C8 0.0406(9) 0.0289(8) 0.0238(7) 0.0024(6) 0.0040(6) 0.0093(7) C9 0.0293(8) 0.0282(8) 0.0265(7) 0.0065(6) 0.0019(6) 0.0066(6) C10 0.0469(11) 0.0538(11) 0.0356(9) 0.0048(8) 0.0115(8) 0.0245(9) C11 0.0661(13) 0.0289(9) 0.0489(11) 0.0153(8) -0.0112(10) -0.0018(8) C12 0.0730(14) 0.0611(13) 0.0401(10) 0.0214(9) 0.0179(10) 0.0454(11) C13 0.0256(7) 0.0328(8) 0.0245(7) 0.0116(6) 0.0052(6) 0.0056(6) C14 0.0439(9) 0.0330(8) 0.0299(8) 0.0113(7) 0.0009(7) 0.0074(7) C15 0.0490(10) 0.0421(10) 0.0283(8) 0.0071(7) -0.0030(7) 0.0011(8) C16 0.0347(9) 0.0535(11) 0.0283(8) 0.0187(8) 0.0016(7) 0.0068(8) C17 0.0373(9) 0.0450(10) 0.0363(9) 0.0242(8) 0.0057(7) 0.0120(7) C18 0.0341(8) 0.0325(8) 0.0303(8) 0.0136(7) 0.0035(6) 0.0057(6) C19 0.0499(11) 0.0699(14) 0.0365(10) 0.0225(10) -0.0055(8) 0.0096(10) C20 0.0426(10) 0.0547(11) 0.0272(8) 0.0142(8) 0.0072(7) 0.0062(8) C21 0.0320(9) 0.0456(10) 0.0482(11) 0.0085(8) 0.0063(8) 0.0119(8) C22 0.0297(8) 0.0304(8) 0.0326(8) 0.0115(7) 0.0014(6) 0.0086(6) C23 0.0423(9) 0.0353(9) 0.0338(9) 0.0101(7) 0.0031(7) 0.0083(7) C24 0.0485(11) 0.0337(9) 0.0435(10) 0.0073(8) -0.0067(8) 0.0067(8) C25 0.0380(9) 0.0338(9) 0.0612(12) 0.0189(9) -0.0075(9) 0.0032(7) C26 0.0393(10) 0.0464(11) 0.0555(12) 0.0279(9) 0.0059(8) 0.0038(8) C27 0.0387(9) 0.0372(9) 0.0391(9) 0.0146(8) 0.0064(7) 0.0053(7) C28 0.0523(12) 0.0400(11) 0.0899(18) 0.0272(12) -0.0125(12) -0.0031(9) C50 0.0473(11) 0.0546(12) 0.0624(13) 0.0225(11) 0.0055(10) 0.0146(9) C51 0.0393(10) 0.0414(10) 0.0618(12) 0.0175(9) -0.0063(9) 0.0109(8) C52 0.0550(12) 0.0422(11) 0.0630(13) 0.0270(10) 0.0075(10) 0.0137(9) C53 0.084(2) 0.122(3) 0.0669(17) 0.0476(18) 0.0150(15) 0.0273(18) C54 0.0769(16) 0.0736(16) 0.0678(15) 0.0423(14) 0.0198(13) 0.0220(13) C55 0.0574(12) 0.0444(11) 0.0626(13) 0.0264(10) 0.0241(10) 0.0071(9) C56 0.0450(10) 0.0449(10) 0.0477(11) 0.0124(9) 0.0214(9) 0.0087(8) C57 0.0443(12) 0.0595(14) 0.0817(17) 0.0149(12) 0.0172(11) -0.0012(10) N1 0.0259(6) 0.0268(6) 0.0225(6) 0.0023(5) 0.0016(5) 0.0086(5) N2 0.0297(6) 0.0267(6) 0.0240(6) 0.0087(5) 0.0027(5) 0.0077(5) N3 0.0348(7) 0.0280(7) 0.0277(7) 0.0085(5) 0.0069(5) 0.0061(5) O1 0.0432(7) 0.0332(6) 0.0610(8) 0.0229(6) 0.0043(6) 0.0127(5) O2 0.0396(7) 0.0457(7) 0.0499(8) 0.0218(6) 0.0202(6) 0.0106(6) Si1 0.0263(2) 0.0238(2) 0.0216(2) 0.00282(16) 0.00051(15) 0.00720(15) Si2 0.0390(2) 0.0255(2) 0.0245(2) 0.00661(17) 0.00176(17) 0.01292(18) Si3 0.0284(2) 0.0322(2) 0.0232(2) 0.00656(17) 0.00462(16) 0.00892(17) Li1 0.0321(13) 0.0302(13) 0.0278(13) 0.0102(11) 0.0053(10) 0.0084(11) Li2 0.0427(16) 0.0293(14) 0.0395(15) 0.0125(12) 0.0062(12) 0.0133(12) Li3 0.0342(14) 0.0360(14) 0.0323(14) 0.0116(12) 0.0081(11) 0.0063(11) _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 C1 Si1 1.8933(15) . ? C1 Si2 1.9056(15) . ? C1 Si3 1.9100(16) . ? C1 Li1 2.586(3) . ? C1 H1 1.0000 . ? C2 Si1 1.8808(18) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.8884(17) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.4001(18) . ? C4 C9 1.403(2) . ? C4 C5 1.409(2) . ? C4 Li3 2.553(3) . ? C4 Li2 2.693(3) . ? C5 C6 1.384(2) . ? C5 H5 0.9500 . ? C6 C7 1.387(2) . ? C6 H6 0.9500 . ? C7 C8 1.389(2) . ? C7 C10 1.512(2) . ? C8 C9 1.390(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si2 1.895(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.8728(19) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.3901(19) . ? C13 C14 1.407(2) . ? C13 C18 1.409(2) . ? C14 C15 1.383(2) . ? C14 H14 0.9500 . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.383(3) . ? C16 C19 1.516(2) . ? C17 C18 1.391(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 Si3 1.8822(17) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 Si3 1.8767(18) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.389(2) . ? C22 C27 1.405(2) . ? C22 C23 1.410(2) . ? C22 Li2 2.583(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.385(3) . ? C25 C28 1.514(3) . ? C26 C27 1.387(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C50 C51 1.486(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 O1 1.442(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O1 1.438(2) . ? C52 C53 1.486(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.501(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O2 1.438(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O2 1.450(2) . ? C56 C57 1.481(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? N1 Si1 1.7275(12) . ? N1 Li1 2.058(3) . ? N1 Li3 2.081(3) . ? N1 Li2 2.124(3) . ? N2 Si2 1.7151(13) . ? N2 Li1 1.953(3) . ? N2 Li3 2.004(3) . ? N3 Si3 1.7131(13) . ? N3 Li1 1.958(3) . ? N3 Li2 1.989(3) . ? O1 Li2 1.905(3) . ? O2 Li3 1.891(3) . ? Si1 Li2 2.843(3) . ? Si1 Li1 2.913(3) . ? Si1 Li3 3.083(3) . ? Si2 Li1 2.812(3) . ? Si2 Li3 2.996(3) . ? Si3 Li1 2.752(3) . ? Li1 Li3 2.456(4) . ? Li1 Li2 2.514(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 C1 Si2 113.67(8) . . ? Si1 C1 Si3 112.22(7) . . ? Si2 C1 Si3 117.80(8) . . ? Si1 C1 Li1 79.49(8) . . ? Si2 C1 Li1 75.83(7) . . ? Si3 C1 Li1 73.77(8) . . ? Si1 C1 H1 103.7 . . ? Si2 C1 H1 103.7 . . ? Si3 C1 H1 103.7 . . ? Li1 C1 H1 176.6 . . ? 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 C9 119.09(13) . . ? N1 C4 C5 125.37(14) . . ? C9 C4 C5 115.53(14) . . ? N1 C4 Li3 54.52(9) . . ? C9 C4 Li3 89.34(11) . . ? C5 C4 Li3 126.70(13) . . ? N1 C4 Li2 51.44(9) . . ? C9 C4 Li2 99.32(12) . . ? C5 C4 Li2 120.33(12) . . ? Li3 C4 Li2 98.72(10) . . ? C6 C5 C4 121.67(15) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.07(16) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 117.10(15) . . ? C6 C7 C10 120.93(16) . . ? C8 C7 C10 121.97(15) . . ? C7 C8 C9 121.22(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 122.33(14) . . ? C8 C9 H9 118.8 . . ? C4 C9 H9 118.8 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 . . ? N2 C13 C14 119.75(14) . . ? N2 C13 C18 125.01(14) . . ? C14 C13 C18 115.23(14) . . ? C15 C14 C13 122.42(16) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 121.73(17) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C17 C16 C15 116.79(15) . . ? C17 C16 C19 121.95(17) . . ? C15 C16 C19 121.23(17) . . ? C16 C17 C18 122.26(16) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C17 C18 C13 121.55(15) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C27 125.68(15) . . ? N3 C22 C23 118.95(15) . . ? C27 C22 C23 115.28(15) . . ? N3 C22 Li2 49.68(9) . . ? C27 C22 Li2 131.93(13) . . ? C23 C22 Li2 87.88(12) . . ? C24 C23 C22 122.62(17) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 121.34(18) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 116.86(17) . . ? C24 C25 C28 121.0(2) . . ? C26 C25 C28 122.2(2) . . ? C25 C26 C27 122.56(18) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C22 121.26(17) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O1 C51 C50 112.16(16) . . ? O1 C51 H51A 109.2 . . ? C50 C51 H51A 109.2 . . ? O1 C51 H51B 109.2 . . ? C50 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? O1 C52 C53 111.8(2) . . ? O1 C52 H52A 109.3 . . ? C53 C52 H52A 109.3 . . ? O1 C52 H52B 109.3 . . ? C53 C52 H52B 109.3 . . ? H52A C52 H52B 107.9 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O2 C55 C54 112.71(18) . . ? O2 C55 H55A 109.0 . . ? C54 C55 H55A 109.0 . . ? O2 C55 H55B 109.0 . . ? C54 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? O2 C56 C57 112.20(16) . . ? O2 C56 H56A 109.2 . . ? C57 C56 H56A 109.2 . . ? O2 C56 H56B 109.2 . . ? C57 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C4 N1 Si1 127.63(10) . . ? C4 N1 Li1 132.06(12) . . ? Si1 N1 Li1 100.25(9) . . ? C4 N1 Li3 92.25(12) . . ? Si1 N1 Li3 107.73(10) . . ? Li1 N1 Li3 72.78(11) . . ? C4 N1 Li2 97.53(12) . . ? Si1 N1 Li2 94.59(10) . . ? Li1 N1 Li2 73.87(11) . . ? Li3 N1 Li2 142.50(13) . . ? C13 N2 Si2 126.13(10) . . ? C13 N2 Li1 126.01(13) . . ? Si2 N2 Li1 99.91(10) . . ? C13 N2 Li3 109.44(12) . . ? Si2 N2 Li3 107.06(10) . . ? Li1 N2 Li3 76.71(12) . . ? C22 N3 Si3 128.45(11) . . ? C22 N3 Li1 125.32(13) . . ? Si3 N3 Li1 96.92(10) . . ? C22 N3 Li2 98.16(12) . . ? Si3 N3 Li2 119.74(11) . . ? Li1 N3 Li2 79.12(12) . . ? C52 O1 C51 113.32(14) . . ? C52 O1 Li2 124.02(14) . . ? C51 O1 Li2 122.57(15) . . ? C55 O2 C56 115.40(14) . . ? C55 O2 Li3 122.11(14) . . ? C56 O2 Li3 121.79(14) . . ? N1 Si1 C2 116.04(7) . . ? N1 Si1 C3 111.18(7) . . ? C2 Si1 C3 101.79(8) . . ? N1 Si1 C1 104.32(6) . . ? C2 Si1 C1 111.62(7) . . ? C3 Si1 C1 112.18(7) . . ? N1 Si1 Li2 48.14(8) . . ? C2 Si1 Li2 153.15(8) . . ? C3 Si1 Li2 72.14(8) . . ? C1 Si1 Li2 94.57(8) . . ? N1 Si1 Li1 44.05(7) . . ? C2 Si1 Li1 137.19(8) . . ? C3 Si1 Li1 120.40(8) . . ? C1 Si1 Li1 60.79(7) . . ? Li2 Si1 Li1 51.77(8) . . ? N1 Si1 Li3 40.01(7) . . ? C2 Si1 Li3 91.22(8) . . ? C3 Si1 Li3 150.60(8) . . ? C1 Si1 Li3 86.49(7) . . ? Li2 Si1 Li3 84.33(8) . . ? Li1 Si1 Li3 48.25(7) . . ? N2 Si2 C12 115.90(9) . . ? N2 Si2 C11 111.59(8) . . ? C12 Si2 C11 102.34(11) . . ? N2 Si2 C1 105.53(6) . . ? C12 Si2 C1 111.39(8) . . ? C11 Si2 C1 110.15(8) . . ? N2 Si2 Li1 43.16(7) . . ? C12 Si2 Li1 124.12(10) . . ? C11 Si2 Li1 132.77(9) . . ? C1 Si2 Li1 63.09(7) . . ? N2 Si2 Li3 39.76(7) . . ? C12 Si2 Li3 153.91(9) . . ? C11 Si2 Li3 84.85(9) . . ? C1 Si2 Li3 88.82(7) . . ? Li1 Si2 Li3 49.90(8) . . ? N3 Si3 C21 110.64(8) . . ? N3 Si3 C20 117.06(8) . . ? C21 Si3 C20 103.42(9) . . ? N3 Si3 C1 103.91(6) . . ? C21 Si3 C1 113.71(8) . . ? C20 Si3 C1 108.43(8) . . ? N3 Si3 Li1 44.92(7) . . ? C21 Si3 Li1 107.05(8) . . ? C20 Si3 Li1 148.88(8) . . ? C1 Si3 Li1 64.45(7) . . ? N2 Li1 N3 141.41(15) . . ? N2 Li1 N1 100.90(13) . . ? N3 Li1 N1 99.43(12) . . ? N2 Li1 Li3 52.59(10) . . ? N3 Li1 Li3 152.55(15) . . ? N1 Li1 Li3 54.03(10) . . ? N2 Li1 Li2 154.15(16) . . ? N3 Li1 Li2 50.99(10) . . ? N1 Li1 Li2 54.26(10) . . ? Li3 Li1 Li2 106.48(14) . . ? N2 Li1 C1 77.54(10) . . ? N3 Li1 C1 76.49(10) . . ? N1 Li1 C1 75.09(9) . . ? Li3 Li1 C1 88.43(11) . . ? Li2 Li1 C1 87.87(11) . . ? N2 Li1 Si3 105.97(11) . . ? N3 Li1 Si3 38.16(6) . . ? N1 Li1 Si3 99.09(10) . . ? Li3 Li1 Si3 130.09(12) . . ? Li2 Li1 Si3 74.82(10) . . ? C1 Li1 Si3 41.78(5) . . ? N2 Li1 Si2 36.93(6) . . ? N3 Li1 Si2 110.00(11) . . ? N1 Li1 Si2 92.53(10) . . ? Li3 Li1 Si2 68.94(9) . . ? Li2 Li1 Si2 127.43(12) . . ? C1 Li1 Si2 41.08(5) . . ? Si3 Li1 Si2 71.90(6) . . ? N2 Li1 Si1 93.25(10) . . ? N3 Li1 Si1 84.60(10) . . ? N1 Li1 Si1 35.70(6) . . ? Li3 Li1 Si1 69.48(9) . . ? Li2 Li1 Si1 62.68(9) . . ? C1 Li1 Si1 39.72(5) . . ? Si3 Li1 Si1 67.66(6) . . ? Si2 Li1 Si1 67.46(6) . . ? O1 Li2 N3 129.39(17) . . ? O1 Li2 N1 133.90(16) . . ? N3 Li2 N1 96.26(12) . . ? O1 Li2 Li1 165.94(17) . . ? N3 Li2 Li1 49.89(9) . . ? N1 Li2 Li1 51.87(9) . . ? O1 Li2 C22 102.08(13) . . ? N3 Li2 C22 32.16(7) . . ? N1 Li2 C22 123.33(13) . . ? Li1 Li2 C22 71.67(10) . . ? O1 Li2 C4 106.07(13) . . ? N3 Li2 C4 124.21(13) . . ? N1 Li2 C4 31.03(6) . . ? Li1 Li2 C4 74.96(10) . . ? C22 Li2 C4 142.02(13) . . ? O1 Li2 Si1 127.60(14) . . ? N3 Li2 Si1 85.97(10) . . ? N1 Li2 Si1 37.28(6) . . ? Li1 Li2 Si1 65.55(9) . . ? C22 Li2 Si1 117.96(11) . . ? C4 Li2 Si1 60.94(7) . . ? O2 Li3 N2 124.04(16) . . ? O2 Li3 N1 136.08(16) . . ? N2 Li3 N1 98.44(13) . . ? O2 Li3 Li1 167.95(17) . . ? N2 Li3 Li1 50.70(9) . . ? N1 Li3 Li1 53.19(9) . . ? O2 Li3 C4 107.17(13) . . ? N2 Li3 C4 128.71(14) . . ? N1 Li3 C4 33.23(6) . . ? Li1 Li3 C4 78.55(11) . . ? O2 Li3 Si2 121.63(13) . . ? N2 Li3 Si2 33.18(6) . . ? N1 Li3 Si2 87.02(10) . . ? Li1 Li3 Si2 61.16(9) . . ? C4 Li3 Si2 119.78(10) . . ? O2 Li3 Si1 129.78(13) . . ? N2 Li3 Si1 87.33(10) . . ? N1 Li3 Si1 32.26(5) . . ? Li1 Li3 Si1 62.27(9) . . ? C4 Li3 Si1 58.93(7) . . ? Si2 Li3 Si1 63.07(6) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.392 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.047 # Attachment '4.cif' data_udpsia _database_code_depnum_ccdc_archive 'CCDC 757627' #TrackingRef '4.cif' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H54 Cl N3 O Si3 U' _chemical_formula_sum 'C35 H54 Cl N3 O Si3 U' _chemical_formula_weight 890.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 13.5913(3) _cell_length_b 13.2334(3) _cell_length_c 21.9614(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.054(2) _cell_angle_gamma 90.00 _cell_volume 3947.42(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6899 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.40 _exptl_crystal_description TABLET _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 4.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.21 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 37076 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.029 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.43 _reflns_number_total 8878 _reflns_number_gt 6260 _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 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0237P)^2^+3.8289P] 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 8878 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.316623(8) 0.751603(10) 0.144661(5) 0.02430(4) Uani 1 1 d . . . Cl1 Cl 0.37784(7) 0.77325(8) 0.25941(4) 0.0438(2) Uani 1 1 d . . . C1 C 0.1864(2) 0.8089(2) 0.01606(15) 0.0273(7) Uani 1 1 d . . . H1A H 0.1467 0.8273 -0.0215 0.033 Uiso 1 1 calc R . . N1 N 0.2248(2) 0.8893(2) 0.13886(13) 0.0291(6) Uani 1 1 d . . . N2 N 0.19504(19) 0.6545(2) 0.10572(12) 0.0292(6) Uani 1 1 d . . . N3 N 0.3879(2) 0.7870(2) 0.05732(13) 0.0316(6) Uani 1 1 d . . . Si1 Si 0.13829(7) 0.89391(7) 0.07745(4) 0.0282(2) Uani 1 1 d . . . Si2 Si 0.15597(7) 0.67139(7) 0.03013(5) 0.0302(2) Uani 1 1 d . . . Si3 Si 0.31895(7) 0.83656(8) -0.00350(4) 0.0312(2) Uani 1 1 d . . . C2 C 0.1200(3) 1.0262(3) 0.04912(19) 0.0430(10) Uani 1 1 d . . . H2A H 0.0884 1.0246 0.0083 0.065 Uiso 1 1 calc R . . H2B H 0.1840 1.0600 0.0473 0.065 Uiso 1 1 calc R . . H2C H 0.0781 1.0631 0.0769 0.065 Uiso 1 1 calc R . . C3 C 0.0164(2) 0.8529(3) 0.10635(18) 0.0389(9) Uani 1 1 d . . . H3A H -0.0329 0.8526 0.0726 0.058 Uiso 1 1 calc R . . H3B H -0.0042 0.8999 0.1380 0.058 Uiso 1 1 calc R . . H3C H 0.0225 0.7848 0.1236 0.058 Uiso 1 1 calc R . . C4 C 0.2183(3) 0.5831(3) -0.02293(18) 0.0461(10) Uani 1 1 d . . . H4A H 0.2004 0.6012 -0.0652 0.069 Uiso 1 1 calc R . . H4B H 0.1974 0.5136 -0.0150 0.069 Uiso 1 1 calc R . . H4C H 0.2899 0.5884 -0.0164 0.069 Uiso 1 1 calc R . . C5 C 0.0209(3) 0.6454(3) 0.01796(19) 0.0424(9) Uani 1 1 d . . . H5A H 0.0084 0.6187 -0.0232 0.064 Uiso 1 1 calc R . . H5B H -0.0162 0.7083 0.0228 0.064 Uiso 1 1 calc R . . H5C H -0.0001 0.5958 0.0480 0.064 Uiso 1 1 calc R . . C6 C 0.3461(3) 0.9739(3) -0.00962(19) 0.0484(10) Uani 1 1 d . . . H6A H 0.2989 1.0052 -0.0387 0.073 Uiso 1 1 calc R . . H6B H 0.4130 0.9831 -0.0238 0.073 Uiso 1 1 calc R . . H6C H 0.3407 1.0057 0.0304 0.073 Uiso 1 1 calc R . . C7 C 0.3501(3) 0.7847(4) -0.07932(18) 0.0513(11) Uani 1 1 d . . . H7A H 0.3070 0.8152 -0.1110 0.077 Uiso 1 1 calc R . . H7B H 0.3407 0.7112 -0.0794 0.077 Uiso 1 1 calc R . . H7C H 0.4189 0.8003 -0.0874 0.077 Uiso 1 1 calc R . . C8 C 0.2308(2) 0.9745(2) 0.17879(16) 0.0289(7) Uani 1 1 d . . . C9 C 0.1775(3) 0.9804(3) 0.23149(16) 0.0321(8) Uani 1 1 d . . . H9A H 0.1361 0.9257 0.2419 0.039 Uiso 1 1 calc R . . C10 C 0.1835(3) 1.0650(3) 0.26957(17) 0.0367(9) Uani 1 1 d . . . C11 C 0.2435(3) 1.1448(3) 0.25352(18) 0.0409(9) Uani 1 1 d . . . H11A H 0.2477 1.2028 0.2790 0.049 Uiso 1 1 calc R . . C12 C 0.2974(3) 1.1419(3) 0.20115(19) 0.0395(9) Uani 1 1 d . . . C13 C 0.2911(3) 1.0563(3) 0.16488(17) 0.0355(8) Uani 1 1 d . . . H13A H 0.3289 1.0530 0.1294 0.043 Uiso 1 1 calc R . . C14 C 0.1263(3) 1.0686(4) 0.32736(19) 0.0533(11) Uani 1 1 d . . . H14A H 0.0882 1.1314 0.3284 0.080 Uiso 1 1 calc R . . H14B H 0.1721 1.0660 0.3628 0.080 Uiso 1 1 calc R . . H14C H 0.0814 1.0107 0.3284 0.080 Uiso 1 1 calc R . . C15 C 0.3599(3) 1.2310(3) 0.1826(2) 0.0581(12) Uani 1 1 d . . . H15A H 0.4114 1.2434 0.2141 0.087 Uiso 1 1 calc R . . H15B H 0.3183 1.2912 0.1779 0.087 Uiso 1 1 calc R . . H15C H 0.3903 1.2160 0.1438 0.087 Uiso 1 1 calc R . . C16 C 0.1601(2) 0.5814(3) 0.14718(16) 0.0285(7) Uani 1 1 d . . . C17 C 0.1391(2) 0.4808(3) 0.13125(17) 0.0330(8) Uani 1 1 d . . . H17A H 0.1461 0.4593 0.0904 0.040 Uiso 1 1 calc R . . C18 C 0.1082(3) 0.4119(3) 0.17456(18) 0.0373(9) Uani 1 1 d . . . C19 C 0.1022(3) 0.4426(3) 0.23497(18) 0.0407(9) Uani 1 1 d . . . H19A H 0.0838 0.3949 0.2648 0.049 Uiso 1 1 calc R . . C20 C 0.1228(3) 0.5421(3) 0.25268(17) 0.0371(9) Uani 1 1 d . . . C21 C 0.1501(2) 0.6106(3) 0.20810(16) 0.0330(8) Uani 1 1 d . . . H21A H 0.1623 0.6790 0.2193 0.040 Uiso 1 1 calc R . . C22 C 0.0807(3) 0.3055(3) 0.1558(2) 0.0512(11) Uani 1 1 d . . . H22A H 0.1222 0.2838 0.1226 0.077 Uiso 1 1 calc R . . H22B H 0.0114 0.3037 0.1419 0.077 Uiso 1 1 calc R . . H22C H 0.0907 0.2600 0.1907 0.077 Uiso 1 1 calc R . . C23 C 0.1126(3) 0.5769(3) 0.31728(18) 0.0509(11) Uani 1 1 d . . . H23A H 0.1441 0.6431 0.3227 0.076 Uiso 1 1 calc R . . H23B H 0.1444 0.5281 0.3451 0.076 Uiso 1 1 calc R . . H23C H 0.0426 0.5823 0.3262 0.076 Uiso 1 1 calc R . . C24 C 0.4883(2) 0.8047(3) 0.07150(16) 0.0305(8) Uani 1 1 d . . . C25 C 0.5638(2) 0.7566(3) 0.04048(17) 0.0360(8) Uani 1 1 d . . . H25A H 0.5479 0.7163 0.0057 0.043 Uiso 1 1 calc R . . C26 C 0.6622(3) 0.7675(3) 0.0603(2) 0.0421(10) Uani 1 1 d . . . C27 C 0.6839(3) 0.8252(3) 0.11206(19) 0.0439(10) Uani 1 1 d . . . H27A H 0.7505 0.8304 0.1264 0.053 Uiso 1 1 calc R . . C28 C 0.6120(3) 0.8752(3) 0.14331(18) 0.0396(9) Uani 1 1 d . . . C29 C 0.5146(3) 0.8652(3) 0.12148(16) 0.0323(8) Uani 1 1 d . . . H29A H 0.4644 0.9010 0.1414 0.039 Uiso 1 1 calc R . . C30 C 0.7418(3) 0.7185(3) 0.0247(2) 0.0617(14) Uani 1 1 d . . . H30A H 0.7928 0.6917 0.0529 0.093 Uiso 1 1 calc R . . H30B H 0.7708 0.7686 -0.0022 0.093 Uiso 1 1 calc R . . H30C H 0.7135 0.6631 0.0001 0.093 Uiso 1 1 calc R . . C31 C 0.6354(3) 0.9431(3) 0.1970(2) 0.0592(12) Uani 1 1 d . . . H31A H 0.7020 0.9286 0.2132 0.089 Uiso 1 1 calc R . . H31B H 0.5879 0.9311 0.2287 0.089 Uiso 1 1 calc R . . H31C H 0.6315 1.0139 0.1839 0.089 Uiso 1 1 calc R . . O1 O 0.42509(17) 0.60092(17) 0.14720(11) 0.0338(6) Uani 1 1 d . . . C32 C 0.4175(3) 0.5221(3) 0.1018(2) 0.0561(12) Uani 1 1 d . . . H32A H 0.4218 0.5510 0.0604 0.067 Uiso 1 1 calc R . . H32B H 0.3540 0.4859 0.1044 0.067 Uiso 1 1 calc R . . C33 C 0.5009(3) 0.4524(3) 0.1150(3) 0.0646(14) Uani 1 1 d . . . H33A H 0.5238 0.4212 0.0770 0.078 Uiso 1 1 calc R . . H33B H 0.4816 0.3981 0.1431 0.078 Uiso 1 1 calc R . . C34 C 0.5791(3) 0.5171(3) 0.1436(2) 0.0521(11) Uani 1 1 d . . . H34A H 0.6193 0.5492 0.1123 0.063 Uiso 1 1 calc R . . H34C H 0.6228 0.4771 0.1714 0.063 Uiso 1 1 calc R . . C35 C 0.5229(3) 0.5954(3) 0.17834(18) 0.0409(9) Uani 1 1 d . . . H35C H 0.5169 0.5748 0.2214 0.049 Uiso 1 1 calc R . . H35A H 0.5565 0.6617 0.1772 0.049 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 0.02440(6) 0.02516(6) 0.02327(6) 0.00267(6) -0.00020(4) -0.00145(6) Cl1 0.0469(5) 0.0591(7) 0.0251(4) -0.0003(4) -0.0050(4) 0.0032(5) C1 0.0281(17) 0.0286(18) 0.0248(17) 0.0036(14) -0.0058(14) -0.0018(14) N1 0.0341(16) 0.0251(14) 0.0280(15) -0.0027(12) -0.0004(12) -0.0030(12) N2 0.0311(15) 0.0268(15) 0.0296(15) -0.0010(12) 0.0002(12) -0.0019(12) N3 0.0238(14) 0.0388(15) 0.0320(16) 0.0070(13) -0.0002(12) -0.0040(12) Si1 0.0291(5) 0.0251(5) 0.0301(5) -0.0005(4) -0.0011(4) 0.0014(4) Si2 0.0304(5) 0.0281(5) 0.0319(5) -0.0045(4) -0.0017(4) -0.0014(4) Si3 0.0287(5) 0.0400(6) 0.0252(5) 0.0072(4) 0.0023(4) -0.0003(4) C2 0.044(2) 0.032(2) 0.052(3) 0.0039(18) -0.0108(19) 0.0042(17) C3 0.0305(19) 0.041(2) 0.045(2) -0.0042(18) 0.0052(16) 0.0026(17) C4 0.061(3) 0.041(2) 0.036(2) -0.0085(18) -0.0009(19) 0.006(2) C5 0.035(2) 0.040(2) 0.052(3) -0.0037(18) -0.0090(17) -0.0086(17) C6 0.045(2) 0.052(3) 0.048(3) 0.020(2) 0.0043(19) -0.010(2) C7 0.045(2) 0.077(3) 0.032(2) 0.006(2) 0.0079(18) 0.010(2) C8 0.0290(18) 0.0266(17) 0.0305(19) -0.0013(14) -0.0057(14) 0.0035(14) C9 0.0287(18) 0.0353(19) 0.0318(19) -0.0020(15) -0.0061(15) 0.0001(15) C10 0.0311(19) 0.046(2) 0.032(2) -0.0090(17) -0.0081(15) 0.0063(17) C11 0.040(2) 0.033(2) 0.049(2) -0.0160(18) -0.0145(18) 0.0073(17) C12 0.036(2) 0.0275(18) 0.054(3) -0.0034(17) -0.0102(18) -0.0041(16) C13 0.0328(19) 0.035(2) 0.039(2) -0.0025(16) -0.0003(16) -0.0008(16) C14 0.047(2) 0.071(3) 0.042(2) -0.019(2) -0.0012(19) 0.007(2) C15 0.061(3) 0.039(3) 0.074(3) -0.004(2) -0.008(2) -0.017(2) C16 0.0209(16) 0.0290(18) 0.0353(19) 0.0037(14) -0.0017(14) -0.0006(14) C17 0.0302(18) 0.0307(18) 0.038(2) 0.0000(15) -0.0034(15) -0.0021(15) C18 0.0294(18) 0.0302(19) 0.052(2) 0.0081(17) -0.0089(17) -0.0011(15) C19 0.035(2) 0.040(2) 0.046(2) 0.0149(18) -0.0017(17) -0.0039(17) C20 0.0298(19) 0.044(2) 0.037(2) 0.0051(17) 0.0009(16) 0.0001(17) C21 0.0262(17) 0.0331(19) 0.040(2) 0.0007(16) 0.0022(15) -0.0045(15) C22 0.062(3) 0.030(2) 0.060(3) 0.0088(19) -0.013(2) -0.011(2) C23 0.058(3) 0.053(3) 0.042(2) 0.007(2) 0.009(2) -0.005(2) C24 0.0282(17) 0.0301(19) 0.0330(19) 0.0101(15) 0.0000(14) -0.0026(15) C25 0.0313(17) 0.0319(18) 0.045(2) 0.0106(18) 0.0063(14) -0.0033(17) C26 0.0296(18) 0.035(2) 0.062(3) 0.0230(19) 0.0056(17) 0.0015(16) C27 0.0289(19) 0.043(2) 0.059(3) 0.026(2) -0.0118(18) -0.0084(18) C28 0.040(2) 0.038(2) 0.040(2) 0.0177(17) -0.0071(17) -0.0125(18) C29 0.0321(18) 0.0340(19) 0.0308(19) 0.0093(15) 0.0021(15) -0.0020(15) C30 0.037(2) 0.048(2) 0.101(4) 0.017(2) 0.021(2) 0.0087(19) C31 0.064(3) 0.060(3) 0.052(3) 0.008(2) -0.019(2) -0.023(2) O1 0.0306(13) 0.0318(13) 0.0385(14) -0.0002(11) -0.0032(11) 0.0026(11) C32 0.052(3) 0.047(3) 0.068(3) -0.026(2) -0.013(2) 0.010(2) C33 0.048(3) 0.049(3) 0.096(4) -0.022(3) -0.007(3) 0.010(2) C34 0.042(2) 0.041(2) 0.073(3) 0.000(2) -0.004(2) 0.0066(19) C35 0.033(2) 0.041(2) 0.048(2) 0.0046(18) -0.0104(17) 0.0022(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 2.210(3) . ? U1 N2 2.239(3) . ? U1 N3 2.229(3) . ? U1 O1 2.479(2) . ? U1 Cl1 2.6409(9) . ? U1 C24 2.964(3) . ? C1 Si1 1.891(3) . ? C1 Si2 1.894(3) . ? C1 Si3 1.903(3) . ? N1 C8 1.429(4) . ? N1 Si1 1.758(3) . ? N2 C16 1.421(4) . ? N2 Si2 1.739(3) . ? N3 C24 1.408(4) . ? N3 Si3 1.733(3) . ? Si1 C2 1.871(4) . ? Si1 C3 1.876(4) . ? Si2 C4 1.874(4) . ? Si2 C5 1.878(4) . ? Si3 C6 1.860(4) . ? Si3 C7 1.864(4) . ? C8 C9 1.389(5) . ? C8 C13 1.398(5) . ? C9 C10 1.398(5) . ? C10 C11 1.387(5) . ? C10 C14 1.513(5) . ? C11 C12 1.386(5) . ? C12 C13 1.386(5) . ? C12 C15 1.517(5) . ? C16 C21 1.404(5) . ? C16 C17 1.404(5) . ? C17 C18 1.393(5) . ? C18 C19 1.393(5) . ? C18 C22 1.511(5) . ? C19 C20 1.398(5) . ? C20 C21 1.395(5) . ? C20 C23 1.503(5) . ? C24 C29 1.395(5) . ? C24 C25 1.404(5) . ? C25 C26 1.399(5) . ? C26 C27 1.392(6) . ? C26 C30 1.505(6) . ? C27 C28 1.382(6) . ? C28 C29 1.399(5) . ? C28 C31 1.507(6) . ? O1 C32 1.445(4) . ? O1 C35 1.474(4) . ? C32 C33 1.482(6) . ? C33 C34 1.486(6) . ? C34 C35 1.511(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N3 92.24(10) . . ? N1 U1 N2 92.51(10) . . ? N3 U1 N2 97.43(10) . . ? N1 U1 O1 177.07(9) . . ? N3 U1 O1 84.95(9) . . ? N2 U1 O1 88.68(9) . . ? N1 U1 Cl1 97.10(7) . . ? N3 U1 Cl1 131.80(8) . . ? N2 U1 Cl1 129.03(7) . . ? O1 U1 Cl1 84.20(6) . . ? N1 U1 C24 103.14(10) . . ? N3 U1 C24 27.03(9) . . ? N2 U1 C24 120.89(10) . . ? O1 U1 C24 73.97(8) . . ? Cl1 U1 C24 105.33(7) . . ? Si1 C1 Si2 111.87(17) . . ? Si1 C1 Si3 113.63(17) . . ? Si2 C1 Si3 115.84(17) . . ? C8 N1 Si1 117.7(2) . . ? C8 N1 U1 126.6(2) . . ? Si1 N1 U1 115.69(14) . . ? C16 N2 Si2 127.0(2) . . ? C16 N2 U1 113.9(2) . . ? Si2 N2 U1 119.12(14) . . ? C24 N3 Si3 126.9(2) . . ? C24 N3 U1 107.0(2) . . ? Si3 N3 U1 120.21(14) . . ? N1 Si1 C2 111.38(16) . . ? N1 Si1 C3 107.75(16) . . ? C2 Si1 C3 105.96(18) . . ? N1 Si1 C1 106.71(14) . . ? C2 Si1 C1 111.40(17) . . ? C3 Si1 C1 113.66(16) . . ? N2 Si2 C4 112.57(16) . . ? N2 Si2 C5 112.08(16) . . ? C4 Si2 C5 105.03(19) . . ? N2 Si2 C1 102.62(14) . . ? C4 Si2 C1 113.03(17) . . ? C5 Si2 C1 111.75(16) . . ? N3 Si3 C6 108.81(17) . . ? N3 Si3 C7 114.55(17) . . ? C6 Si3 C7 104.1(2) . . ? N3 Si3 C1 104.07(14) . . ? C6 Si3 C1 113.35(17) . . ? C7 Si3 C1 112.20(18) . . ? C9 C8 C13 117.8(3) . . ? C9 C8 N1 122.4(3) . . ? C13 C8 N1 119.8(3) . . ? C8 C9 C10 121.5(3) . . ? C11 C10 C9 118.7(3) . . ? C11 C10 C14 120.9(4) . . ? C9 C10 C14 120.4(4) . . ? C12 C11 C10 121.5(3) . . ? C13 C12 C11 118.4(3) . . ? C13 C12 C15 120.3(4) . . ? C11 C12 C15 121.3(4) . . ? C12 C13 C8 122.2(4) . . ? C21 C16 C17 118.2(3) . . ? C21 C16 N2 118.0(3) . . ? C17 C16 N2 123.7(3) . . ? C18 C17 C16 120.9(3) . . ? C17 C18 C19 119.3(3) . . ? C17 C18 C22 120.1(4) . . ? C19 C18 C22 120.6(4) . . ? C18 C19 C20 121.5(3) . . ? C21 C20 C19 118.2(4) . . ? C21 C20 C23 119.9(4) . . ? C19 C20 C23 121.8(3) . . ? C20 C21 C16 121.8(3) . . ? C29 C24 C25 118.1(3) . . ? C29 C24 N3 119.2(3) . . ? C25 C24 N3 122.4(3) . . ? C29 C24 U1 83.9(2) . . ? C25 C24 U1 139.3(2) . . ? N3 C24 U1 45.99(15) . . ? C26 C25 C24 120.6(4) . . ? C27 C26 C25 118.9(4) . . ? C27 C26 C30 121.7(4) . . ? C25 C26 C30 119.4(4) . . ? C28 C27 C26 122.3(3) . . ? C27 C28 C29 117.5(4) . . ? C27 C28 C31 122.7(4) . . ? C29 C28 C31 119.7(4) . . ? C24 C29 C28 122.5(3) . . ? C32 O1 C35 109.0(3) . . ? C32 O1 U1 122.5(2) . . ? C35 O1 U1 125.1(2) . . ? O1 C32 C33 106.2(3) . . ? C32 C33 C34 104.7(4) . . ? C33 C34 C35 104.0(3) . . ? O1 C35 C34 105.3(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.09 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.08 #=== END of CIF # Attachment '5.cif' data_ucltol _database_code_depnum_ccdc_archive 'CCDC 757628' #TrackingRef '5.cif' _refine_special_details ; Highly disordered lattice solvent moleculess (158 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 453.3 \%A**3, equating to 3 molecules of hexane per unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. Other than C10, C19, C28, C46, and C55 the methyl groups within the molecule were ill defined and could not be refined using a rigid rotor AFIX 137 code. Instead they were refined in fixed, calculated positions using the AFIX 33 code. The CSi3 groups were disordered over two orientations which was resolved wit a two-part model and restraints. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H96 Cl2 N6 O2 Si6 U2, 1.5 (C6 H14)' _chemical_formula_sum 'C73 H117 Cl2 N6 O2 Si6 U2' _chemical_formula_weight 1826.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2778(15) _cell_length_b 16.5243(17) _cell_length_c 17.9252(19) _cell_angle_alpha 98.985(2) _cell_angle_beta 94.570(2) _cell_angle_gamma 104.373(2) _cell_volume 4015.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7837 _cell_measurement_theta_min 2.4405 _cell_measurement_theta_max 26.595 _exptl_crystal_description Lath _exptl_crystal_colour Green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1830 _exptl_absorpt_coefficient_mu 4.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4060 _exptl_absorpt_correction_T_max 0.7021 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 35028 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.91 _reflns_number_total 18075 _reflns_number_gt 10575 _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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00046(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18075 _refine_ls_number_parameters 796 _refine_ls_number_restraints 903 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.975 _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 0.703191(19) 0.283825(16) 0.355045(15) 0.03368(9) Uani 1 1 d U . . U2 U 0.74746(2) -0.033803(16) 0.249499(16) 0.03532(9) Uani 1 1 d U . . Cl1 Cl 0.71535(14) 0.12866(10) 0.26234(10) 0.0415(4) Uani 1 1 d U B . Cl2 Cl 0.73298(14) -0.02253(12) 0.39925(11) 0.0455(4) Uani 1 1 d U B . O1 O 0.5806(4) 0.1885(3) 0.4195(3) 0.0481(12) Uani 1 1 d U B . O2 O 0.8077(4) 0.2274(3) 0.4402(3) 0.0439(11) Uani 1 1 d U B . N1 N 0.7132(4) 0.4030(3) 0.4417(3) 0.0421(13) Uani 1 1 d U B . N2 N 0.5709(4) 0.2908(4) 0.2831(3) 0.0405(13) Uani 1 1 d U B . N3 N 0.8144(4) 0.3546(4) 0.2896(4) 0.0429(13) Uani 1 1 d U B . C1 C 0.6846(5) 0.4652(4) 0.3013(4) 0.0443(14) Uani 1 1 d DU . . H1 H 0.6798 0.5191 0.2845 0.053 Uiso 1 1 calc R A 1 Si1 Si 0.72927(19) 0.49850(14) 0.40681(14) 0.0503(7) Uani 0.938(3) 1 d PDU B 1 C2 C 0.8634(5) 0.5610(5) 0.4279(5) 0.067(2) Uani 0.938(3) 1 d PDU B 1 H2A H 0.8822 0.5759 0.4831 0.100 Uiso 0.938(3) 1 calc PR B 1 H2B H 0.8728 0.6131 0.4064 0.100 Uiso 0.938(3) 1 calc PR B 1 H2C H 0.9037 0.5262 0.4050 0.100 Uiso 0.938(3) 1 calc PR B 1 C3 C 0.6631(6) 0.5715(5) 0.4587(5) 0.064(2) Uani 0.938(3) 1 d PDU B 1 H3A H 0.5950 0.5405 0.4587 0.096 Uiso 0.938(3) 1 calc PR B 1 H3B H 0.6655 0.6200 0.4329 0.096 Uiso 0.938(3) 1 calc PR B 1 H3C H 0.6944 0.5920 0.5112 0.096 Uiso 0.938(3) 1 calc PR B 1 Si2 Si 0.55686(19) 0.39291(15) 0.27734(15) 0.0543(7) Uani 0.938(3) 1 d PDU B 1 C11 C 0.4961(7) 0.3945(6) 0.1816(5) 0.085(3) Uani 0.938(3) 1 d PDU B 1 H11A H 0.5330 0.3744 0.1421 0.127 Uiso 0.938(3) 1 calc PR B 1 H11B H 0.4938 0.4526 0.1783 0.127 Uiso 0.938(3) 1 calc PR B 1 H11C H 0.4297 0.3572 0.1740 0.127 Uiso 0.938(3) 1 calc PR B 1 C12 C 0.4757(6) 0.4274(6) 0.3487(6) 0.081(2) Uani 0.938(3) 1 d PDU B 1 H12A H 0.4078 0.3954 0.3318 0.122 Uiso 0.938(3) 1 calc PR B 1 H12B H 0.4817 0.4883 0.3522 0.122 Uiso 0.938(3) 1 calc PR B 1 H12C H 0.4959 0.4162 0.3988 0.122 Uiso 0.938(3) 1 calc PR B 1 Si3 Si 0.77585(19) 0.42814(15) 0.24218(14) 0.0505(6) Uani 0.938(3) 1 d PDU B 1 C20 C 0.7200(7) 0.3758(6) 0.1406(4) 0.074(2) Uani 0.938(3) 1 d PDU B 1 H20A H 0.7698 0.3582 0.1123 0.110 Uiso 0.938(3) 1 calc PR B 1 H20B H 0.6952 0.4164 0.1157 0.110 Uiso 0.938(3) 1 calc PR B 1 H20C H 0.6663 0.3259 0.1415 0.110 Uiso 0.938(3) 1 calc PR B 1 C21 C 0.8800(6) 0.5196(5) 0.2331(5) 0.066(2) Uani 0.938(3) 1 d PDU B 1 H21A H 0.9028 0.5563 0.2830 0.098 Uiso 0.938(3) 1 calc PR B 1 H21B H 0.8582 0.5522 0.1973 0.098 Uiso 0.938(3) 1 calc PR B 1 H21C H 0.9333 0.4979 0.2143 0.098 Uiso 0.938(3) 1 calc PR B 1 Si1A Si 0.6106(10) 0.4644(11) 0.3930(12) 0.053(3) Uani 0.062(3) 1 d PDU B 2 C3A C 0.6631(6) 0.5715(5) 0.4587(5) 0.064(2) Uani 0.062(3) 1 d PDU B 2 H3A1 H 0.6519 0.6169 0.4326 0.096 Uiso 0.062(3) 1 calc PR B 2 H3A2 H 0.7332 0.5804 0.4721 0.096 Uiso 0.062(3) 1 calc PR B 2 H3A3 H 0.6311 0.5725 0.5050 0.096 Uiso 0.062(3) 1 calc PR B 2 C12A C 0.4757(6) 0.4274(6) 0.3487(6) 0.081(2) Uani 0.062(3) 1 d PDU B 2 H12D H 0.4454 0.4744 0.3592 0.122 Uiso 0.062(3) 1 calc PR B 2 H12E H 0.4412 0.3796 0.3709 0.122 Uiso 0.062(3) 1 calc PR B 2 H12F H 0.4720 0.4094 0.2935 0.122 Uiso 0.062(3) 1 calc PR B 2 Si2A Si 0.6208(10) 0.3769(18) 0.2080(10) 0.058(4) Uani 0.062(3) 1 d PDU B 2 C11A C 0.4961(7) 0.3945(6) 0.1816(5) 0.085(3) Uani 0.062(3) 1 d PDU B 2 H11D H 0.5041 0.4535 0.1750 0.127 Uiso 0.062(3) 1 calc PR B 2 H11E H 0.4555 0.3828 0.2222 0.127 Uiso 0.062(3) 1 calc PR B 2 H11F H 0.4648 0.3561 0.1339 0.127 Uiso 0.062(3) 1 calc PR B 2 C20A C 0.7200(7) 0.3758(6) 0.1406(4) 0.074(2) Uani 0.062(3) 1 d PDU B 2 H20D H 0.7080 0.3188 0.1101 0.110 Uiso 0.062(3) 1 calc PR B 2 H20E H 0.7843 0.3913 0.1707 0.110 Uiso 0.062(3) 1 calc PR B 2 H20F H 0.7180 0.4168 0.1068 0.110 Uiso 0.062(3) 1 calc PR B 2 Si3A Si 0.8319(15) 0.4949(14) 0.3258(6) 0.056(4) Uani 0.062(3) 1 d PDU B 2 C21A C 0.8800(6) 0.5196(5) 0.2331(5) 0.066(2) Uani 0.062(3) 1 d PDU B 2 H21D H 0.8839 0.5790 0.2301 0.098 Uiso 0.062(3) 1 calc PR B 2 H21E H 0.8357 0.4823 0.1898 0.098 Uiso 0.062(3) 1 calc PR B 2 H21F H 0.9449 0.5100 0.2319 0.098 Uiso 0.062(3) 1 calc PR B 2 C2A C 0.8634(5) 0.5610(5) 0.4279(5) 0.067(2) Uani 0.062(3) 1 d PDU B 2 H2A1 H 0.9039 0.6180 0.4265 0.100 Uiso 0.062(3) 1 calc PR B 2 H2A2 H 0.8991 0.5331 0.4601 0.100 Uiso 0.062(3) 1 calc PR B 2 H2A3 H 0.8031 0.5656 0.4488 0.100 Uiso 0.062(3) 1 calc PR B 2 N4 N 0.6366(4) -0.1587(4) 0.2270(4) 0.0475(13) Uani 1 1 d U B . N5 N 0.8826(4) -0.0756(4) 0.2691(4) 0.0451(13) Uani 1 1 d U B . N6 N 0.7639(5) -0.0465(4) 0.1251(4) 0.0564(15) Uani 1 1 d U B . Si4 Si 0.6527(2) -0.24221(18) 0.1594(2) 0.0564(9) Uani 0.758(3) 1 d PDU B 1 C38 C 0.6023(9) -0.3519(4) 0.1836(7) 0.120(3) Uani 0.758(3) 1 d PDU B 1 H38A H 0.6284 -0.3523 0.2358 0.179 Uiso 0.758(3) 1 calc PR B 1 H38B H 0.6216 -0.3945 0.1482 0.179 Uiso 0.758(3) 1 calc PR B 1 H38C H 0.5311 -0.3651 0.1794 0.179 Uiso 0.758(3) 1 calc PR B 1 C39 C 0.5830(7) -0.2458(7) 0.0614(5) 0.110(3) Uani 0.758(3) 1 d PDU B 1 H39A H 0.5129 -0.2673 0.0630 0.164 Uiso 0.758(3) 1 calc PR B 1 H39B H 0.6041 -0.2834 0.0223 0.164 Uiso 0.758(3) 1 calc PR B 1 H39C H 0.5968 -0.1884 0.0495 0.164 Uiso 0.758(3) 1 calc PR B 1 Si5 Si 0.8738(2) -0.18347(17) 0.24017(18) 0.0478(8) Uani 0.758(3) 1 d PDU B 1 C47 C 0.7990(8) -0.2513(6) 0.3078(5) 0.129(3) Uani 0.758(3) 1 d PDU B 1 H47A H 0.8386 -0.2423 0.3572 0.193 Uiso 0.758(3) 1 calc PR B 1 H47B H 0.7820 -0.3117 0.2847 0.193 Uiso 0.758(3) 1 calc PR B 1 H47C H 0.7392 -0.2336 0.3152 0.193 Uiso 0.758(3) 1 calc PR B 1 C48 C 0.9928(7) -0.2093(7) 0.2295(7) 0.124(3) Uani 0.758(3) 1 d PDU B 1 H48A H 1.0292 -0.1733 0.1972 0.187 Uiso 0.758(3) 1 calc PR B 1 H48B H 0.9810 -0.2691 0.2060 0.187 Uiso 0.758(3) 1 calc PR B 1 H48C H 1.0307 -0.1988 0.2797 0.187 Uiso 0.758(3) 1 calc PR B 1 Si6 Si 0.8217(3) -0.12668(19) 0.08737(17) 0.0544(9) Uani 0.758(3) 1 d PDU B 1 C56 C 0.9607(6) -0.0973(8) 0.1042(6) 0.123(3) Uani 0.758(3) 1 d PDU B 1 H56A H 0.9873 -0.0723 0.0618 0.184 Uiso 0.758(3) 1 calc PR B 1 H56B H 0.9825 -0.1485 0.1078 0.184 Uiso 0.758(3) 1 calc PR B 1 H56C H 0.9837 -0.0562 0.1518 0.184 Uiso 0.758(3) 1 calc PR B 1 C57 C 0.7773(8) -0.1695(6) -0.0154(4) 0.086(2) Uani 0.758(3) 1 d PDU B 1 H57A H 0.7065 -0.1790 -0.0238 0.129 Uiso 0.758(3) 1 calc PR B 1 H57B H 0.7938 -0.2235 -0.0303 0.129 Uiso 0.758(3) 1 calc PR B 1 H57C H 0.8083 -0.1287 -0.0461 0.129 Uiso 0.758(3) 1 calc PR B 1 Si4A Si 0.6923(7) -0.2496(5) 0.2236(5) 0.060(2) Uani 0.242(3) 1 d PDU B 2 C38A C 0.6023(9) -0.3519(4) 0.1836(7) 0.120(3) Uani 0.242(3) 1 d PDU B 2 H38D H 0.5695 -0.3751 0.2247 0.179 Uiso 0.242(3) 1 calc PR B 2 H38E H 0.6357 -0.3920 0.1590 0.179 Uiso 0.242(3) 1 calc PR B 2 H38F H 0.5540 -0.3428 0.1461 0.179 Uiso 0.242(3) 1 calc PR B 2 C47A C 0.7990(8) -0.2513(6) 0.3078(5) 0.129(3) Uani 0.242(3) 1 d PDU B 2 H47D H 0.7839 -0.2268 0.3574 0.193 Uiso 0.242(3) 1 calc PR B 2 H47E H 0.8623 -0.2178 0.2981 0.193 Uiso 0.242(3) 1 calc PR B 2 H47F H 0.8014 -0.3100 0.3080 0.193 Uiso 0.242(3) 1 calc PR B 2 Si5A Si 0.9050(6) -0.1530(6) 0.1912(5) 0.049(2) Uiso 0.242(3) 1 d PDU B 2 C48A C 0.9928(7) -0.2093(7) 0.2295(7) 0.124(3) Uani 0.242(3) 1 d PDU B 2 H48D H 1.0375 -0.1709 0.2720 0.187 Uiso 0.242(3) 1 calc PR B 2 H48E H 1.0302 -0.2264 0.1892 0.187 Uiso 0.242(3) 1 calc PR B 2 H48F H 0.9565 -0.2597 0.2473 0.187 Uiso 0.242(3) 1 calc PR B 2 C56A C 0.9607(6) -0.0973(8) 0.1042(6) 0.123(3) Uani 0.242(3) 1 d PDU B 2 H56D H 0.9073 -0.0986 0.0658 0.184 Uiso 0.242(3) 1 calc PR B 2 H56E H 1.0044 -0.1284 0.0810 0.184 Uiso 0.242(3) 1 calc PR B 2 H56F H 0.9971 -0.0383 0.1242 0.184 Uiso 0.242(3) 1 calc PR B 2 Si6A Si 0.7168(6) -0.1651(5) 0.0765(4) 0.047(2) Uani 0.242(3) 1 d PDU B 2 C57A C 0.7773(8) -0.1695(6) -0.0154(4) 0.086(2) Uani 0.242(3) 1 d PDU B 2 H57D H 0.8454 -0.1359 -0.0043 0.129 Uiso 0.242(3) 1 calc PR B 2 H57E H 0.7426 -0.1464 -0.0527 0.129 Uiso 0.242(3) 1 calc PR B 2 H57F H 0.7748 -0.2287 -0.0361 0.129 Uiso 0.242(3) 1 calc PR B 2 C39A C 0.5830(7) -0.2458(7) 0.0614(5) 0.110(3) Uani 0.242(3) 1 d PDU B 2 H39D H 0.5812 -0.2959 0.0234 0.164 Uiso 0.242(3) 1 calc PR B 2 H39E H 0.5350 -0.2174 0.0438 0.164 Uiso 0.242(3) 1 calc PR B 2 H39F H 0.5677 -0.2633 0.1098 0.164 Uiso 0.242(3) 1 calc PR B 2 C4 C 0.7371(6) 0.4080(4) 0.5207(5) 0.0464(16) Uani 1 1 d U . . C5 C 0.8327(6) 0.4075(5) 0.5505(5) 0.0552(18) Uani 1 1 d U B . H5 H 0.8815 0.4074 0.5174 0.066 Uiso 1 1 calc R . . C6 C 0.8553(7) 0.4072(5) 0.6273(5) 0.066(2) Uani 1 1 d U . . H6 H 0.9180 0.4026 0.6451 0.079 Uiso 1 1 calc R B . C7 C 0.7895(9) 0.4134(6) 0.6778(6) 0.077(2) Uani 1 1 d U B . C8 C 0.6989(8) 0.4191(6) 0.6504(5) 0.071(2) Uani 1 1 d U . . H8 H 0.6527 0.4238 0.6850 0.085 Uiso 1 1 calc R B . C9 C 0.6723(7) 0.4183(5) 0.5728(5) 0.0577(19) Uani 1 1 d U B . H9 H 0.6101 0.4248 0.5563 0.069 Uiso 1 1 calc R . . C10 C 0.8144(10) 0.4118(8) 0.7611(6) 0.116(4) Uani 1 1 d U . . H10A H 0.8482 0.3676 0.7658 0.174 Uiso 1 1 calc R B . H10B H 0.7544 0.3995 0.7851 0.174 Uiso 1 1 calc R . . H10C H 0.8567 0.4672 0.7864 0.174 Uiso 1 1 calc R . . C13 C 0.4882(5) 0.2218(4) 0.2524(4) 0.0407(15) Uani 1 1 d U . . C14 C 0.4878(6) 0.1676(5) 0.1834(4) 0.0479(17) Uani 1 1 d U B . H14 H 0.5442 0.1755 0.1577 0.057 Uiso 1 1 calc R . . C15 C 0.4043(6) 0.1017(5) 0.1524(5) 0.0509(18) Uani 1 1 d U . . H15 H 0.4060 0.0660 0.1058 0.061 Uiso 1 1 calc R B . C16 C 0.3200(6) 0.0867(5) 0.1868(5) 0.0490(17) Uani 1 1 d U B . C17 C 0.3219(6) 0.1410(5) 0.2566(5) 0.0497(18) Uani 1 1 d U . . H17 H 0.2659 0.1326 0.2826 0.060 Uiso 1 1 calc R B . C18 C 0.4042(5) 0.2061(5) 0.2879(5) 0.0469(17) Uani 1 1 d U B . H18 H 0.4028 0.2411 0.3350 0.056 Uiso 1 1 calc R . . C19 C 0.2303(6) 0.0160(6) 0.1538(5) 0.067(2) Uani 1 1 d U . . H19A H 0.2220 0.0101 0.0983 0.100 Uiso 1 1 calc R B . H19B H 0.1731 0.0294 0.1741 0.100 Uiso 1 1 calc R . . H19C H 0.2377 -0.0373 0.1678 0.100 Uiso 1 1 calc R . . C22 C 0.9066(6) 0.3395(5) 0.2753(5) 0.0439(15) Uani 1 1 d U . . C23 C 0.9141(6) 0.2822(5) 0.2105(5) 0.0498(17) Uani 1 1 d U B . H23 H 0.8572 0.2504 0.1774 0.060 Uiso 1 1 calc R . . C24 C 1.0060(6) 0.2721(5) 0.1949(5) 0.0548(19) Uani 1 1 d U . . H24 H 1.0104 0.2338 0.1507 0.066 Uiso 1 1 calc R B . C25 C 1.0913(6) 0.3173(5) 0.2432(5) 0.0529(17) Uani 1 1 d U B . C26 C 1.0828(6) 0.3719(5) 0.3063(5) 0.0543(18) Uani 1 1 d U . . H26 H 1.1397 0.4037 0.3394 0.065 Uiso 1 1 calc R B . C27 C 0.9919(6) 0.3818(5) 0.3229(5) 0.0494(17) Uani 1 1 d U B . H27 H 0.9884 0.4186 0.3682 0.059 Uiso 1 1 calc R . . C28 C 1.1910(6) 0.3071(6) 0.2235(6) 0.071(2) Uani 1 1 d U . . H28A H 1.2174 0.3479 0.1913 0.106 Uiso 1 1 calc R B . H28B H 1.1835 0.2492 0.1962 0.106 Uiso 1 1 calc R . . H28C H 1.2357 0.3177 0.2705 0.106 Uiso 1 1 calc R . . C29 C 0.5344(6) 0.0951(5) 0.3883(5) 0.0574(19) Uani 1 1 d U . . H29A H 0.5793 0.0603 0.3995 0.069 Uiso 1 1 calc R B . H29B H 0.5154 0.0850 0.3327 0.069 Uiso 1 1 calc R . . C30 C 0.4450(7) 0.0751(6) 0.4306(5) 0.068(2) Uani 1 1 d U B . H30A H 0.3873 0.0835 0.4016 0.082 Uiso 1 1 calc R . . H30B H 0.4301 0.0159 0.4395 0.082 Uiso 1 1 calc R . . C31 C 0.4739(7) 0.1374(6) 0.5047(6) 0.075(2) Uani 1 1 d U . . H31A H 0.5142 0.1169 0.5412 0.090 Uiso 1 1 calc R B . H31B H 0.4155 0.1460 0.5277 0.090 Uiso 1 1 calc R . . C32 C 0.5316(6) 0.2188(5) 0.4836(5) 0.060(2) Uani 1 1 d U B . H32A H 0.4881 0.2529 0.4678 0.073 Uiso 1 1 calc R . . H32B H 0.5797 0.2534 0.5268 0.073 Uiso 1 1 calc R . . C33 C 0.7844(6) 0.1948(5) 0.5099(4) 0.0471(17) Uani 1 1 d U . . H33A H 0.7402 0.1367 0.4977 0.057 Uiso 1 1 calc R B . H33B H 0.7532 0.2321 0.5421 0.057 Uiso 1 1 calc R . . C34 C 0.8833(6) 0.1945(6) 0.5501(5) 0.0542(19) Uani 1 1 d U B . H34A H 0.9097 0.2461 0.5896 0.065 Uiso 1 1 calc R . . H34B H 0.8777 0.1437 0.5739 0.065 Uiso 1 1 calc R . . C35 C 0.9467(7) 0.1932(8) 0.4870(5) 0.080(2) Uani 1 1 d U . . H35A H 1.0118 0.2331 0.5044 0.096 Uiso 1 1 calc R B . H35B H 0.9553 0.1354 0.4722 0.096 Uiso 1 1 calc R . . C36 C 0.9018(6) 0.2171(7) 0.4242(5) 0.071(2) Uani 1 1 d U B . H36A H 0.8942 0.1729 0.3783 0.085 Uiso 1 1 calc R . . H36B H 0.9430 0.2711 0.4143 0.085 Uiso 1 1 calc R . . C37 C 0.7806(5) -0.2136(5) 0.1499(4) 0.0534(15) Uani 1 1 d DU . . H37 H 0.7925 -0.2662 0.1209 0.064 Uiso 1 1 calc R B 1 C40 C 0.5430(6) -0.1555(5) 0.2455(5) 0.0492(16) Uani 1 1 d U . . C41 C 0.5034(5) -0.0890(5) 0.2262(4) 0.0469(17) Uani 1 1 d U B . H41 H 0.5381 -0.0502 0.1977 0.056 Uiso 1 1 calc R . . C42 C 0.4143(6) -0.0805(6) 0.2485(5) 0.0589(19) Uani 1 1 d U . . H42 H 0.3918 -0.0335 0.2377 0.071 Uiso 1 1 calc R B . C43 C 0.3580(6) -0.1381(7) 0.2855(6) 0.073(2) Uani 1 1 d U B . C44 C 0.3945(7) -0.2040(6) 0.3035(5) 0.074(2) Uani 1 1 d U . . H44 H 0.3569 -0.2446 0.3290 0.088 Uiso 1 1 calc R B . C45 C 0.4847(7) -0.2120(6) 0.2849(5) 0.066(2) Uani 1 1 d U B . H45 H 0.5079 -0.2571 0.2994 0.080 Uiso 1 1 calc R . . C46 C 0.2589(7) -0.1305(8) 0.3074(7) 0.097(3) Uani 1 1 d U . . H46A H 0.2681 -0.0917 0.3563 0.146 Uiso 1 1 calc R B . H46B H 0.2188 -0.1866 0.3118 0.146 Uiso 1 1 calc R . . H46C H 0.2263 -0.1083 0.2681 0.146 Uiso 1 1 calc R . . C49 C 0.9642(5) -0.0133(4) 0.3129(4) 0.0384(15) Uani 1 1 d U . . C50 C 0.9978(5) 0.0670(4) 0.2931(4) 0.0418(16) Uani 1 1 d U B . H50 H 0.9673 0.0791 0.2486 0.050 Uiso 1 1 calc R . . C51 C 1.0742(6) 0.1288(5) 0.3370(4) 0.0478(17) Uani 1 1 d U . . H51 H 1.0941 0.1827 0.3223 0.057 Uiso 1 1 calc R B . C52 C 1.1233(6) 0.1143(5) 0.4025(5) 0.0500(17) Uani 1 1 d U B . C53 C 1.0895(6) 0.0349(5) 0.4227(5) 0.0505(18) Uani 1 1 d U . . H53 H 1.1207 0.0226 0.4667 0.061 Uiso 1 1 calc R B . C54 C 1.0108(6) -0.0269(5) 0.3794(4) 0.0488(18) Uani 1 1 d U B . H54 H 0.9883 -0.0796 0.3957 0.059 Uiso 1 1 calc R . . C55 C 1.2071(6) 0.1812(5) 0.4503(5) 0.065(2) Uani 1 1 d U . . H55A H 1.2595 0.1977 0.4190 0.097 Uiso 1 1 calc R B . H55B H 1.2314 0.1585 0.4930 0.097 Uiso 1 1 calc R . . H55C H 1.1849 0.2311 0.4699 0.097 Uiso 1 1 calc R . . C58 C 0.7490(6) 0.0163(5) 0.0820(4) 0.0495(17) Uani 1 1 d U . . C59 C 0.8275(6) 0.0753(5) 0.0642(4) 0.0543(18) Uani 1 1 d U B . H59 H 0.8921 0.0731 0.0789 0.065 Uiso 1 1 calc R . . C60 C 0.8110(6) 0.1387(5) 0.0241(5) 0.0541(18) Uani 1 1 d U . . H60 H 0.8654 0.1784 0.0117 0.065 Uiso 1 1 calc R B . C61 C 0.7187(7) 0.1449(5) 0.0024(5) 0.0570(18) Uani 1 1 d U B . C62 C 0.6424(6) 0.0862(5) 0.0227(5) 0.0536(18) Uani 1 1 d U . . H62 H 0.5779 0.0893 0.0091 0.064 Uiso 1 1 calc R B . C63 C 0.6551(6) 0.0233(5) 0.0616(4) 0.0510(18) Uani 1 1 d U B . H63 H 0.6002 -0.0152 0.0746 0.061 Uiso 1 1 calc R . . C64 C 0.7039(7) 0.2128(6) -0.0409(5) 0.074(3) Uani 1 1 d U . . H64A H 0.6341 0.2044 -0.0556 0.111 Uiso 1 1 calc R B . H64B H 0.7370 0.2094 -0.0867 0.111 Uiso 1 1 calc R . . H64C H 0.7310 0.2688 -0.0086 0.111 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 0.03779(17) 0.02675(15) 0.03958(18) 0.00755(12) 0.00352(13) 0.01369(12) U2 0.04164(18) 0.02564(15) 0.04030(18) 0.00710(12) 0.00013(13) 0.01278(12) Cl1 0.0556(11) 0.0297(9) 0.0427(11) 0.0069(8) 0.0045(9) 0.0180(8) Cl2 0.0537(11) 0.0437(11) 0.0433(11) 0.0144(9) 0.0103(9) 0.0156(9) O1 0.043(3) 0.045(3) 0.062(3) 0.022(2) 0.016(2) 0.012(2) O2 0.050(3) 0.053(3) 0.040(3) 0.018(2) 0.007(2) 0.026(2) N1 0.055(3) 0.030(3) 0.044(3) 0.009(2) 0.005(3) 0.016(3) N2 0.038(3) 0.035(3) 0.048(3) 0.008(2) -0.003(2) 0.011(2) N3 0.049(3) 0.034(3) 0.053(3) 0.016(2) 0.011(3) 0.019(2) C1 0.056(4) 0.033(3) 0.051(4) 0.015(3) -0.003(3) 0.024(3) Si1 0.0676(16) 0.0306(12) 0.0547(15) 0.0044(11) 0.0016(13) 0.0207(11) C2 0.071(4) 0.037(4) 0.083(5) 0.010(4) -0.013(4) 0.005(3) C3 0.083(5) 0.032(4) 0.076(5) -0.002(4) 0.019(4) 0.020(4) Si2 0.0588(15) 0.0412(13) 0.0659(17) 0.0076(12) -0.0088(13) 0.0253(12) C11 0.091(5) 0.063(5) 0.098(5) 0.020(5) -0.042(4) 0.030(4) C12 0.056(4) 0.060(5) 0.136(6) 0.015(5) 0.018(4) 0.031(4) Si3 0.0664(16) 0.0389(13) 0.0516(15) 0.0174(11) 0.0078(13) 0.0181(12) C20 0.123(6) 0.068(5) 0.040(4) 0.021(3) 0.010(4) 0.039(4) C21 0.077(5) 0.047(4) 0.088(5) 0.036(4) 0.021(4) 0.024(4) Si1A 0.076(7) 0.023(7) 0.066(7) 0.013(7) 0.011(6) 0.022(6) C3A 0.083(5) 0.032(4) 0.076(5) -0.002(4) 0.019(4) 0.020(4) C12A 0.056(4) 0.060(5) 0.136(6) 0.015(5) 0.018(4) 0.031(4) Si2A 0.072(7) 0.038(8) 0.064(7) 0.018(5) -0.012(6) 0.015(7) C11A 0.091(5) 0.063(5) 0.098(5) 0.020(5) -0.042(4) 0.030(4) C20A 0.123(6) 0.068(5) 0.040(4) 0.021(3) 0.010(4) 0.039(4) Si3A 0.060(8) 0.046(7) 0.073(10) 0.034(9) 0.004(9) 0.025(9) C21A 0.077(5) 0.047(4) 0.088(5) 0.036(4) 0.021(4) 0.024(4) C2A 0.071(4) 0.037(4) 0.083(5) 0.010(4) -0.013(4) 0.005(3) N4 0.046(3) 0.029(3) 0.062(4) 0.007(3) 0.002(3) 0.003(2) N5 0.048(3) 0.036(3) 0.053(3) 0.001(3) -0.003(3) 0.022(2) N6 0.096(5) 0.045(3) 0.041(3) 0.013(2) 0.006(3) 0.039(3) Si4 0.0613(19) 0.0305(15) 0.074(2) 0.0033(14) -0.0103(16) 0.0144(13) C38 0.161(7) 0.026(3) 0.171(7) 0.012(5) 0.065(6) 0.015(4) C39 0.086(5) 0.120(6) 0.090(5) -0.041(5) -0.040(4) 0.020(5) Si5 0.0512(17) 0.0355(15) 0.0568(19) -0.0013(13) -0.0107(15) 0.0230(13) C47 0.272(7) 0.076(5) 0.069(5) 0.044(5) 0.011(5) 0.087(5) C48 0.110(5) 0.096(6) 0.157(7) -0.054(5) -0.069(5) 0.083(5) Si6 0.080(2) 0.0466(18) 0.0434(17) 0.0063(14) 0.0066(16) 0.0308(16) C56 0.081(5) 0.133(7) 0.141(6) -0.018(6) 0.055(5) 0.019(5) C57 0.151(6) 0.079(6) 0.045(4) 0.010(4) 0.014(4) 0.060(5) Si4A 0.092(6) 0.028(3) 0.064(5) 0.014(3) 0.012(4) 0.021(3) C38A 0.161(7) 0.026(3) 0.171(7) 0.012(5) 0.065(6) 0.015(4) C47A 0.272(7) 0.076(5) 0.069(5) 0.044(5) 0.011(5) 0.087(5) C48A 0.110(5) 0.096(6) 0.157(7) -0.054(5) -0.069(5) 0.083(5) C56A 0.081(5) 0.133(7) 0.141(6) -0.018(6) 0.055(5) 0.019(5) Si6A 0.067(5) 0.039(4) 0.039(4) 0.004(3) -0.005(4) 0.028(4) C57A 0.151(6) 0.079(6) 0.045(4) 0.010(4) 0.014(4) 0.060(5) C39A 0.086(5) 0.120(6) 0.090(5) -0.041(5) -0.040(4) 0.020(5) C4 0.067(4) 0.023(3) 0.050(3) 0.000(3) 0.007(3) 0.018(3) C5 0.068(4) 0.033(4) 0.060(4) -0.002(3) -0.005(4) 0.014(3) C6 0.084(5) 0.042(4) 0.064(4) 0.003(4) -0.013(4) 0.014(4) C7 0.114(6) 0.054(4) 0.055(4) 0.006(4) -0.003(4) 0.013(4) C8 0.101(5) 0.051(4) 0.058(4) 0.004(4) 0.020(4) 0.015(4) C9 0.077(5) 0.043(4) 0.059(4) 0.010(4) 0.019(4) 0.022(4) C10 0.168(9) 0.098(7) 0.062(5) 0.008(6) -0.014(6) 0.010(7) C13 0.043(3) 0.037(3) 0.045(4) 0.009(3) -0.002(3) 0.018(3) C14 0.057(4) 0.048(4) 0.039(4) 0.008(3) 0.006(3) 0.015(3) C15 0.061(4) 0.049(4) 0.043(4) 0.006(3) 0.001(3) 0.017(3) C16 0.052(4) 0.049(4) 0.045(4) 0.011(3) -0.009(3) 0.014(3) C17 0.044(4) 0.050(4) 0.056(4) 0.008(3) 0.000(3) 0.016(3) C18 0.042(4) 0.047(4) 0.052(4) 0.003(3) 0.001(3) 0.017(3) C19 0.065(5) 0.061(5) 0.064(5) 0.011(4) -0.016(4) 0.006(4) C22 0.046(3) 0.036(3) 0.055(4) 0.019(3) 0.009(3) 0.013(3) C23 0.049(4) 0.046(4) 0.057(4) 0.013(3) 0.005(3) 0.015(3) C24 0.051(4) 0.053(4) 0.066(5) 0.011(4) 0.007(3) 0.025(3) C25 0.045(3) 0.051(4) 0.075(5) 0.026(3) 0.014(3) 0.023(3) C26 0.047(4) 0.045(4) 0.072(5) 0.014(3) -0.001(4) 0.016(3) C27 0.054(4) 0.035(4) 0.061(4) 0.010(3) 0.000(3) 0.017(3) C28 0.051(4) 0.079(6) 0.092(6) 0.028(5) 0.020(4) 0.025(4) C29 0.051(4) 0.051(4) 0.077(5) 0.025(4) 0.014(4) 0.015(3) C30 0.064(5) 0.056(4) 0.083(5) 0.022(4) 0.017(4) 0.003(4) C31 0.067(5) 0.071(5) 0.077(5) 0.020(4) 0.024(4) -0.007(4) C32 0.059(4) 0.054(4) 0.070(5) 0.018(4) 0.019(4) 0.012(4) C33 0.055(4) 0.052(4) 0.041(4) 0.018(3) 0.004(3) 0.022(3) C34 0.054(4) 0.069(5) 0.050(4) 0.025(4) 0.004(3) 0.027(4) C35 0.063(5) 0.130(6) 0.061(5) 0.039(5) 0.010(4) 0.037(5) C36 0.065(4) 0.108(6) 0.059(4) 0.030(4) 0.013(4) 0.049(4) C37 0.072(4) 0.047(4) 0.043(4) -0.002(3) -0.007(3) 0.029(3) C40 0.051(3) 0.038(3) 0.054(4) 0.012(3) 0.000(3) 0.004(3) C41 0.041(4) 0.051(4) 0.050(4) 0.019(3) 0.004(3) 0.007(3) C42 0.044(4) 0.073(5) 0.066(5) 0.031(4) 0.006(4) 0.016(4) C43 0.051(4) 0.099(5) 0.076(5) 0.043(4) 0.014(4) 0.012(4) C44 0.059(4) 0.088(5) 0.076(5) 0.049(4) 0.012(4) 0.001(4) C45 0.063(4) 0.067(5) 0.071(5) 0.040(4) 0.004(4) 0.003(4) C46 0.063(5) 0.138(8) 0.102(7) 0.055(6) 0.027(5) 0.022(5) C49 0.045(3) 0.032(3) 0.044(4) 0.003(3) 0.004(3) 0.024(3) C50 0.048(4) 0.035(3) 0.047(4) 0.009(3) 0.007(3) 0.019(3) C51 0.055(4) 0.036(4) 0.052(4) 0.009(3) 0.010(3) 0.010(3) C52 0.049(4) 0.045(4) 0.054(4) 0.003(3) 0.008(3) 0.011(3) C53 0.052(4) 0.047(4) 0.053(4) 0.010(3) -0.006(3) 0.016(3) C54 0.054(4) 0.040(4) 0.052(4) 0.014(3) 0.002(3) 0.010(3) C55 0.062(5) 0.057(5) 0.063(5) -0.010(4) 0.003(4) 0.007(4) C58 0.075(4) 0.048(3) 0.034(3) 0.013(3) 0.001(3) 0.031(3) C59 0.065(4) 0.060(4) 0.044(4) 0.014(3) -0.002(4) 0.027(3) C60 0.065(4) 0.048(4) 0.048(4) 0.010(3) 0.003(4) 0.012(4) C61 0.075(4) 0.046(4) 0.051(4) 0.009(3) -0.005(4) 0.023(3) C62 0.056(4) 0.055(4) 0.055(4) 0.011(3) -0.003(4) 0.028(3) C63 0.062(4) 0.049(4) 0.045(4) 0.010(3) 0.008(4) 0.019(3) C64 0.106(6) 0.059(5) 0.058(5) 0.019(4) -0.008(5) 0.028(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 2.238(6) . ? U1 N3 2.251(6) . ? U1 N1 2.276(6) . ? U1 O2 2.490(4) . ? U1 O1 2.530(5) . ? U1 Cl1 2.8813(17) . ? U1 Si3 3.387(2) . ? U1 Si2 3.427(2) . ? U1 Si1 3.442(2) . ? U2 N4 2.224(6) . ? U2 N5 2.225(6) . ? U2 N6 2.243(6) . ? U2 Cl2 2.6897(19) . ? U2 Cl1 2.8116(17) . ? U2 Si5 3.396(3) . ? U2 Si4A 3.404(8) . ? U2 Si6A 3.423(8) . ? U2 Si6 3.440(3) . ? U2 Si4 3.450(3) . ? U2 Si5A 3.459(9) . ? O1 C32 1.477(9) . ? O1 C29 1.516(9) . ? O2 C36 1.442(9) . ? O2 C33 1.465(8) . ? N1 C4 1.414(9) . ? N1 Si1 1.756(6) . ? N1 Si1A 2.18(2) . ? N2 C13 1.424(9) . ? N2 Si2 1.766(6) . ? N2 Si2A 2.14(2) . ? N3 C22 1.435(9) . ? N3 Si3 1.755(6) . ? N3 Si3A 2.25(2) . ? C1 Si2 1.891(7) . ? C1 Si1 1.896(7) . ? C1 Si3 1.900(7) . ? C1 Si2A 2.02(2) . ? C1 Si1A 2.02(2) . ? C1 Si3A 2.03(2) . ? Si1 C3 1.889(6) . ? Si1 C2 1.912(7) . ? Si2 C11 1.867(7) . ? Si2 C12 1.908(7) . ? Si3 C21 1.876(7) . ? Si3 C20 1.906(7) . ? N4 C40 1.414(10) . ? N4 Si4 1.762(7) . ? N4 Si4A 1.862(11) . ? N5 C49 1.429(9) . ? N5 Si5 1.747(6) . ? N5 Si5A 1.845(11) . ? N6 C58 1.433(9) . ? N6 Si6 1.802(7) . ? N6 Si6A 1.942(10) . ? Si4 C37 1.799(7) . ? Si4 C38 1.908(7) . ? Si4 C39 1.932(7) . ? Si5 C48 1.868(7) . ? Si5 C37 1.927(6) . ? Si5 C47 1.976(8) . ? Si6 C57 1.866(7) . ? Si6 C56 1.910(8) . ? Si6 C37 1.963(7) . ? Si4A C37 1.956(10) . ? Si5A C37 1.839(9) . ? Si6A C37 1.924(9) . ? C4 C9 1.388(11) . ? C4 C5 1.429(11) . ? C5 C6 1.390(12) . ? C6 C7 1.367(13) . ? C7 C8 1.377(14) . ? C7 C10 1.514(13) . ? C8 C9 1.408(12) . ? C13 C18 1.390(10) . ? C13 C14 1.408(10) . ? C14 C15 1.405(10) . ? C15 C16 1.381(11) . ? C16 C17 1.414(11) . ? C16 C19 1.508(11) . ? C17 C18 1.390(10) . ? C22 C27 1.387(10) . ? C22 C23 1.408(11) . ? C23 C24 1.408(10) . ? C24 C25 1.403(11) . ? C25 C26 1.364(12) . ? C25 C28 1.536(11) . ? C26 C27 1.397(10) . ? C29 C30 1.528(11) . ? C30 C31 1.505(12) . ? C31 C32 1.513(11) . ? C33 C34 1.534(10) . ? C34 C35 1.505(11) . ? C35 C36 1.408(11) . ? C40 C45 1.406(11) . ? C40 C41 1.428(10) . ? C41 C42 1.397(11) . ? C42 C43 1.377(11) . ? C43 C44 1.388(13) . ? C43 C46 1.527(13) . ? C44 C45 1.387(12) . ? C49 C54 1.394(10) . ? C49 C50 1.406(10) . ? C50 C51 1.383(10) . ? C51 C52 1.402(11) . ? C52 C53 1.396(11) . ? C52 C55 1.507(10) . ? C53 C54 1.397(10) . ? C58 C59 1.385(11) . ? C58 C63 1.398(11) . ? C59 C60 1.415(10) . ? C60 C61 1.377(11) . ? C61 C62 1.381(12) . ? C61 C64 1.507(11) . ? C62 C63 1.378(10) . ? 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 96.9(2) . . ? N2 U1 N1 95.7(2) . . ? N3 U1 N1 92.4(2) . . ? N2 U1 O2 159.09(19) . . ? N3 U1 O2 101.14(19) . . ? N1 U1 O2 93.97(19) . . ? N2 U1 O1 83.87(19) . . ? N3 U1 O1 173.32(19) . . ? N1 U1 O1 94.14(19) . . ? O2 U1 O1 76.99(16) . . ? N2 U1 Cl1 93.61(15) . . ? N3 U1 Cl1 87.84(15) . . ? N1 U1 Cl1 170.55(15) . . ? O2 U1 Cl1 76.73(12) . . ? O1 U1 Cl1 85.49(13) . . ? N2 U1 Si3 72.11(16) . . ? N3 U1 Si3 28.05(15) . . ? N1 U1 Si3 82.17(15) . . ? O2 U1 Si3 127.70(12) . . ? O1 U1 Si3 155.11(12) . . ? Cl1 U1 Si3 102.07(6) . . ? N2 U1 Si2 27.27(15) . . ? N3 U1 Si2 83.39(15) . . ? N1 U1 Si2 72.77(15) . . ? O2 U1 Si2 166.26(12) . . ? O1 U1 Si2 99.92(12) . . ? Cl1 U1 Si2 116.62(6) . . ? Si3 U1 Si2 55.41(6) . . ? N2 U1 Si1 82.27(15) . . ? N3 U1 Si1 70.82(15) . . ? N1 U1 Si1 27.15(15) . . ? O2 U1 Si1 113.58(12) . . ? O1 U1 Si1 115.84(13) . . ? Cl1 U1 Si1 157.48(6) . . ? Si3 U1 Si1 55.55(6) . . ? Si2 U1 Si1 55.37(6) . . ? N4 U2 N5 100.2(2) . . ? N4 U2 N6 90.1(2) . . ? N5 U2 N6 89.3(2) . . ? N4 U2 Cl2 89.63(18) . . ? N5 U2 Cl2 88.45(17) . . ? N6 U2 Cl2 177.63(16) . . ? N4 U2 Cl1 127.79(17) . . ? N5 U2 Cl1 131.75(16) . . ? N6 U2 Cl1 94.61(15) . . ? Cl2 U2 Cl1 87.41(5) . . ? N4 U2 Si5 73.88(17) . . ? N5 U2 Si5 27.29(16) . . ? N6 U2 Si5 82.39(16) . . ? Cl2 U2 Si5 95.28(7) . . ? Cl1 U2 Si5 158.26(7) . . ? N4 U2 Si4A 30.3(2) . . ? N5 U2 Si4A 70.0(2) . . ? N6 U2 Si4A 87.2(2) . . ? Cl2 U2 Si4A 91.41(17) . . ? Cl1 U2 Si4A 158.13(17) . . ? Si5 U2 Si4A 43.57(17) . . ? N4 U2 Si6A 60.1(2) . . ? N5 U2 Si6A 83.9(2) . . ? N6 U2 Si6A 32.3(2) . . ? Cl2 U2 Si6A 146.57(14) . . ? Cl1 U2 Si6A 121.43(14) . . ? Si5 U2 Si6A 64.62(14) . . ? Si4A U2 Si6A 55.4(2) . . ? N4 U2 Si6 80.71(18) . . ? N5 U2 Si6 65.37(17) . . ? N6 U2 Si6 28.08(16) . . ? Cl2 U2 Si6 149.61(6) . . ? Cl1 U2 Si6 121.19(6) . . ? Si5 U2 Si6 54.39(7) . . ? Si4A U2 Si6 66.04(18) . . ? Si6A U2 Si6 24.53(15) . . ? N4 U2 Si4 26.42(18) . . ? N5 U2 Si4 83.14(16) . . ? N6 U2 Si4 69.79(18) . . ? Cl2 U2 Si4 109.25(7) . . ? Cl1 U2 Si4 142.73(6) . . ? Si5 U2 Si4 55.97(7) . . ? Si4A U2 Si4 21.50(16) . . ? Si6A U2 Si4 37.56(15) . . ? Si6 U2 Si4 54.98(8) . . ? N4 U2 Si5A 84.1(2) . . ? N5 U2 Si5A 28.6(2) . . ? N6 U2 Si5A 65.6(2) . . ? Cl2 U2 Si5A 111.99(15) . . ? Cl1 U2 Si5A 143.87(15) . . ? Si5 U2 Si5A 19.20(14) . . ? Si4A U2 Si5A 55.7(2) . . ? Si6A U2 Si5A 55.3(2) . . ? Si6 U2 Si5A 38.71(15) . . ? Si4 U2 Si5A 60.89(15) . . ? U2 Cl1 U1 150.17(7) . . ? C32 O1 C29 110.6(5) . . ? C32 O1 U1 124.7(4) . . ? C29 O1 U1 123.8(4) . . ? C36 O2 C33 108.7(6) . . ? C36 O2 U1 123.3(4) . . ? C33 O2 U1 127.9(4) . . ? C4 N1 Si1 117.9(5) . . ? C4 N1 Si1A 124.2(7) . . ? Si1 N1 Si1A 47.5(5) . . ? C4 N1 U1 122.5(4) . . ? Si1 N1 U1 116.6(3) . . ? Si1A N1 U1 105.5(4) . . ? C13 N2 Si2 115.5(4) . . ? C13 N2 Si2A 115.5(7) . . ? Si2 N2 Si2A 48.0(5) . . ? C13 N2 U1 126.3(4) . . ? Si2 N2 U1 117.2(3) . . ? Si2A N2 U1 106.7(4) . . ? C22 N3 Si3 117.1(5) . . ? C22 N3 U1 127.6(4) . . ? Si3 N3 U1 114.9(3) . . ? C22 N3 Si3A 110.0(7) . . ? Si3 N3 Si3A 48.9(5) . . ? U1 N3 Si3A 108.5(5) . . ? Si2 C1 Si1 114.9(4) . . ? Si2 C1 Si3 113.4(3) . . ? Si1 C1 Si3 114.0(3) . . ? Si2 C1 Si2A 49.0(4) . . ? Si1 C1 Si2A 152.2(8) . . ? Si3 C1 Si2A 66.9(4) . . ? Si2 C1 Si1A 68.1(4) . . ? Si1 C1 Si1A 49.1(4) . . ? Si3 C1 Si1A 151.3(7) . . ? Si2A C1 Si1A 116.1(6) . . ? Si2 C1 Si3A 156.2(8) . . ? Si1 C1 Si3A 66.2(4) . . ? Si3 C1 Si3A 51.8(4) . . ? Si2A C1 Si3A 118.4(6) . . ? Si1A C1 Si3A 114.9(6) . . ? N1 Si1 C3 111.8(4) . . ? N1 Si1 C1 105.1(3) . . ? C3 Si1 C1 113.3(4) . . ? N1 Si1 C2 109.5(3) . . ? C3 Si1 C2 104.0(4) . . ? C1 Si1 C2 113.3(4) . . ? N1 Si1 U1 36.2(2) . . ? C3 Si1 U1 138.4(3) . . ? C1 Si1 U1 71.2(2) . . ? C2 Si1 U1 111.7(3) . . ? N2 Si2 C11 110.9(4) . . ? N2 Si2 C1 104.4(3) . . ? C11 Si2 C1 114.2(4) . . ? N2 Si2 C12 111.9(4) . . ? C11 Si2 C12 105.8(5) . . ? C1 Si2 C12 109.8(4) . . ? N2 Si2 U1 35.50(19) . . ? C11 Si2 U1 138.0(3) . . ? C1 Si2 U1 71.7(2) . . ? C12 Si2 U1 110.9(3) . . ? N3 Si3 C21 112.1(4) . . ? N3 Si3 C1 105.2(3) . . ? C21 Si3 C1 111.3(4) . . ? N3 Si3 C20 110.2(3) . . ? C21 Si3 C20 105.6(4) . . ? C1 Si3 C20 112.5(4) . . ? N3 Si3 U1 37.1(2) . . ? C21 Si3 U1 141.8(3) . . ? C1 Si3 U1 72.6(2) . . ? C20 Si3 U1 107.3(3) . . ? C1 Si1A N1 87.2(7) . . ? C1 Si2A N2 87.8(7) . . ? C1 Si3A N3 85.2(7) . . ? C40 N4 Si4 121.3(5) . . ? C40 N4 Si4A 128.1(6) . . ? Si4 N4 Si4A 41.2(3) . . ? C40 N4 U2 114.8(5) . . ? Si4 N4 U2 119.4(3) . . ? Si4A N4 U2 112.5(4) . . ? C49 N5 Si5 126.4(5) . . ? C49 N5 Si5A 118.6(5) . . ? Si5 N5 Si5A 37.0(3) . . ? C49 N5 U2 116.1(4) . . ? Si5 N5 U2 117.0(3) . . ? Si5A N5 U2 116.1(4) . . ? C58 N6 Si6 120.8(5) . . ? C58 N6 Si6A 117.9(5) . . ? Si6 N6 Si6A 45.6(3) . . ? C58 N6 U2 121.8(5) . . ? Si6 N6 U2 116.1(3) . . ? Si6A N6 U2 109.6(4) . . ? N4 Si4 C37 104.7(3) . . ? N4 Si4 C38 113.4(4) . . ? C37 Si4 C38 115.7(5) . . ? N4 Si4 C39 110.5(4) . . ? C37 Si4 C39 107.3(4) . . ? C38 Si4 C39 105.1(5) . . ? N4 Si4 U2 34.1(2) . . ? C37 Si4 U2 72.5(3) . . ? C38 Si4 U2 139.7(4) . . ? C39 Si4 U2 109.6(3) . . ? N5 Si5 C48 114.7(4) . . ? N5 Si5 C37 102.5(3) . . ? C48 Si5 C37 116.3(4) . . ? N5 Si5 C47 110.5(4) . . ? C48 Si5 C47 111.3(5) . . ? C37 Si5 C47 100.3(4) . . ? N5 Si5 U2 35.7(2) . . ? C48 Si5 U2 147.5(4) . . ? C37 Si5 U2 73.0(2) . . ? C47 Si5 U2 96.3(3) . . ? N6 Si6 C57 111.4(4) . . ? N6 Si6 C56 116.7(5) . . ? C57 Si6 C56 110.6(5) . . ? N6 Si6 C37 102.0(3) . . ? C57 Si6 C37 111.2(4) . . ? C56 Si6 C37 104.3(4) . . ? N6 Si6 U2 35.9(2) . . ? C57 Si6 U2 140.6(3) . . ? C56 Si6 U2 106.2(4) . . ? C37 Si6 U2 71.6(2) . . ? N4 Si4A C37 95.2(5) . . ? N4 Si4A U2 37.1(2) . . ? C37 Si4A U2 72.5(3) . . ? C37 Si5A N5 102.2(5) . . ? C37 Si5A U2 72.0(3) . . ? N5 Si5A U2 35.3(2) . . ? C37 Si6A N6 98.5(5) . . ? C37 Si6A U2 72.3(3) . . ? N6 Si6A U2 38.1(2) . . ? C9 C4 N1 122.6(8) . . ? C9 C4 C5 117.0(8) . . ? N1 C4 C5 120.3(7) . . ? C6 C5 C4 120.9(9) . . ? C7 C6 C5 121.4(10) . . ? C6 C7 C8 118.1(10) . . ? C6 C7 C10 121.0(11) . . ? C8 C7 C10 120.9(11) . . ? C7 C8 C9 122.4(10) . . ? C4 C9 C8 119.8(9) . . ? C18 C13 C14 117.2(7) . . ? C18 C13 N2 121.8(7) . . ? C14 C13 N2 121.0(7) . . ? C15 C14 C13 120.2(8) . . ? C16 C15 C14 122.8(8) . . ? C15 C16 C17 116.3(7) . . ? C15 C16 C19 123.0(8) . . ? C17 C16 C19 120.7(8) . . ? C18 C17 C16 121.4(8) . . ? C17 C18 C13 122.0(8) . . ? C27 C22 C23 117.3(7) . . ? C27 C22 N3 121.9(7) . . ? C23 C22 N3 120.8(7) . . ? C22 C23 C24 119.9(8) . . ? C25 C24 C23 121.4(8) . . ? C26 C25 C24 118.1(8) . . ? C26 C25 C28 121.6(8) . . ? C24 C25 C28 120.3(8) . . ? C25 C26 C27 121.1(8) . . ? C22 C27 C26 122.2(8) . . ? O1 C29 C30 103.0(6) . . ? C31 C30 C29 104.1(7) . . ? C30 C31 C32 104.7(8) . . ? O1 C32 C31 103.4(7) . . ? O2 C33 C34 104.5(6) . . ? C35 C34 C33 103.8(7) . . ? C36 C35 C34 108.7(8) . . ? C35 C36 O2 109.3(7) . . ? Si4 C37 Si5A 148.4(6) . . ? Si4 C37 Si6A 72.9(3) . . ? Si5A C37 Si6A 116.2(5) . . ? Si4 C37 Si5 119.1(4) . . ? Si5A C37 Si5 35.3(3) . . ? Si6A C37 Si5 142.4(5) . . ? Si4 C37 Si4A 39.6(3) . . ? Si5A C37 Si4A 115.2(5) . . ? Si6A C37 Si4A 109.8(5) . . ? Si5 C37 Si4A 81.1(4) . . ? Si4 C37 Si6 115.4(4) . . ? Si5A C37 Si6 73.8(4) . . ? Si6A C37 Si6 44.0(3) . . ? Si5 C37 Si6 106.9(3) . . ? Si4A C37 Si6 144.2(5) . . ? C45 C40 N4 124.9(8) . . ? C45 C40 C41 115.6(8) . . ? N4 C40 C41 119.5(7) . . ? C42 C41 C40 120.9(7) . . ? C43 C42 C41 122.0(9) . . ? C42 C43 C44 117.8(9) . . ? C42 C43 C46 122.0(9) . . ? C44 C43 C46 120.2(9) . . ? C45 C44 C43 121.4(8) . . ? C44 C45 C40 122.3(9) . . ? C54 C49 C50 116.7(7) . . ? C54 C49 N5 122.1(6) . . ? C50 C49 N5 121.0(6) . . ? C51 C50 C49 121.4(7) . . ? C50 C51 C52 122.0(7) . . ? C53 C52 C51 116.7(7) . . ? C53 C52 C55 121.0(8) . . ? C51 C52 C55 122.2(7) . . ? C52 C53 C54 121.3(7) . . ? C49 C54 C53 121.8(7) . . ? C59 C58 C63 118.4(7) . . ? C59 C58 N6 120.7(7) . . ? C63 C58 N6 120.8(8) . . ? C58 C59 C60 119.7(8) . . ? C61 C60 C59 122.2(8) . . ? C60 C61 C62 116.4(8) . . ? C60 C61 C64 120.7(9) . . ? C62 C61 C64 122.9(8) . . ? C63 C62 C61 123.3(8) . . ? C62 C63 C58 120.0(8) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.569 _refine_diff_density_min -1.816 _refine_diff_density_rms 0.141 # Attachment '6.cif' data_uidpsi _database_code_depnum_ccdc_archive 'CCDC 757629' #TrackingRef '6.cif' _refine_special_details ; Highly disordered lattice solvent molecules (51 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 151.3 \%A**3, equating to a 0.5 molecule of THF per monomer molecule in the unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 I N3 O2 Si3 U, 2.5(C4 H8 O)' _chemical_formula_sum 'C49 H82 I N3 O4.50 Si3 U' _chemical_formula_weight 1234.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7867(7) _cell_length_b 12.9462(7) _cell_length_c 18.9711(10) _cell_angle_alpha 104.553(2) _cell_angle_beta 94.333(2) _cell_angle_gamma 114.813(2) _cell_volume 2699.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12921 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.44 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 3.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.17 _exptl_absorpt_correction_T_max 0.47 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 23847 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12016 _reflns_number_gt 10661 _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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12016 _refine_ls_number_parameters 544 _refine_ls_number_restraints 291 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.088 _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 0.261478(9) -0.198127(10) -0.216204(6) 0.01799(4) Uani 1 1 d . . . I1 I 0.25835(2) -0.19888(2) -0.050141(12) 0.03148(6) Uani 1 1 d . . . Si1 Si -0.01033(7) -0.34541(8) -0.33522(5) 0.02221(18) Uani 1 1 d . . . Si2 Si 0.13926(8) -0.48656(8) -0.33448(5) 0.02016(17) Uani 1 1 d . . . Si3 Si 0.21471(8) -0.27840(8) -0.40604(5) 0.02056(18) Uani 1 1 d . . . N1 N 0.0671(2) -0.2651(2) -0.24456(14) 0.0221(6) Uani 1 1 d . . . N2 N 0.2561(2) -0.3778(2) -0.26297(14) 0.0203(5) Uani 1 1 d . . . N3 N 0.2766(2) -0.1568(2) -0.32482(15) 0.0223(6) Uani 1 1 d . . . O1 O 0.3576(2) 0.02585(19) -0.14550(13) 0.0266(5) Uani 1 1 d . . . O2 O 0.47703(19) -0.1319(2) -0.19499(13) 0.0259(5) Uani 1 1 d . . . O3 O -0.0833(6) 0.3213(6) -0.1156(3) 0.134(2) Uani 1 1 d . . . O4 O 0.0854(6) 0.9743(6) 0.4208(3) 0.134(2) Uani 1 1 d . . . C1 C 0.0894(3) -0.4000(3) -0.38290(16) 0.0184(6) Uani 1 1 d . . . H1 H 0.0398 -0.4589 -0.4320 0.022 Uiso 1 1 calc R . . C2 C -0.0496(3) -0.2473(3) -0.3773(2) 0.0327(8) Uani 1 1 d . . . H2A H -0.0969 -0.2184 -0.3475 0.049 Uiso 1 1 calc R . . H2B H -0.0951 -0.2932 -0.4282 0.049 Uiso 1 1 calc R . . H2C H 0.0225 -0.1789 -0.3782 0.049 Uiso 1 1 calc R . . C3 C -0.1562(3) -0.4727(3) -0.3405(2) 0.0353(8) Uani 1 1 d . . . H3A H -0.1508 -0.5034 -0.2988 0.053 Uiso 1 1 calc R . . H3B H -0.1778 -0.5368 -0.3875 0.053 Uiso 1 1 calc R . . H3C H -0.2163 -0.4444 -0.3378 0.053 Uiso 1 1 calc R . . C4 C 0.0114(3) -0.2187(3) -0.19251(17) 0.0222(6) Uani 1 1 d U . . C5 C 0.0218(3) -0.1041(3) -0.18196(19) 0.0260(7) Uani 1 1 d U . . H5 H 0.0624 -0.0592 -0.2124 0.031 Uiso 1 1 calc R . . C6 C -0.0258(3) -0.0538(3) -0.1279(2) 0.0291(7) Uani 1 1 d U . . C7 C -0.0861(3) -0.1211(3) -0.08437(19) 0.0297(7) Uani 1 1 d U . . H7 H -0.1163 -0.0865 -0.0460 0.036 Uiso 1 1 calc R . . C8 C -0.1032(3) -0.2378(3) -0.09583(19) 0.0279(7) Uani 1 1 d U . . C9 C -0.0538(3) -0.2854(3) -0.14960(18) 0.0244(7) Uani 1 1 d U . . H9 H -0.0645 -0.3649 -0.1574 0.029 Uiso 1 1 calc R . . C10 C -0.0138(4) 0.0704(3) -0.1184(2) 0.0408(9) Uani 1 1 d U . . H10A H 0.0694 0.1268 -0.1113 0.061 Uiso 1 1 calc R . . H10B H -0.0444 0.0950 -0.0747 0.061 Uiso 1 1 calc R . . H10C H -0.0587 0.0698 -0.1628 0.061 Uiso 1 1 calc R . . C11 C -0.1733(4) -0.3111(4) -0.0504(2) 0.0415(9) Uani 1 1 d U . . H11A H -0.1202 -0.3205 -0.0154 0.062 Uiso 1 1 calc R . . H11B H -0.2312 -0.3901 -0.0835 0.062 Uiso 1 1 calc R . . H11C H -0.2142 -0.2703 -0.0228 0.062 Uiso 1 1 calc R . . C12 C 0.1822(3) -0.5886(3) -0.4008(2) 0.0310(8) Uani 1 1 d . . . H12A H 0.2349 -0.5439 -0.4291 0.046 Uiso 1 1 calc R . . H12B H 0.1114 -0.6552 -0.4351 0.046 Uiso 1 1 calc R . . H12C H 0.2227 -0.6201 -0.3728 0.046 Uiso 1 1 calc R . . C13 C 0.0258(3) -0.5880(3) -0.2939(2) 0.0329(8) Uani 1 1 d . . . H13A H 0.0582 -0.6326 -0.2726 0.049 Uiso 1 1 calc R . . H13B H -0.0439 -0.6444 -0.3331 0.049 Uiso 1 1 calc R . . H13C H 0.0037 -0.5402 -0.2548 0.049 Uiso 1 1 calc R . . C14 C 0.3265(3) -0.4180(3) -0.22620(17) 0.0208(6) Uani 1 1 d U . . C15 C 0.2984(3) -0.4540(3) -0.16432(18) 0.0242(7) Uani 1 1 d U . . H15 H 0.2293 -0.4560 -0.1481 0.029 Uiso 1 1 calc R . . C16 C 0.3693(3) -0.4872(3) -0.12546(19) 0.0286(7) Uani 1 1 d U . . C17 C 0.4695(3) -0.4848(3) -0.1501(2) 0.0313(8) Uani 1 1 d U . . H17 H 0.5190 -0.5059 -0.1232 0.038 Uiso 1 1 calc R . . C18 C 0.4991(3) -0.4528(3) -0.2125(2) 0.0268(7) Uani 1 1 d U . . C19 C 0.4261(3) -0.4208(3) -0.25115(18) 0.0237(6) Uani 1 1 d U . . H19 H 0.4442 -0.4006 -0.2950 0.028 Uiso 1 1 calc R . . C20 C 0.3342(4) -0.5268(4) -0.0592(2) 0.0411(9) Uani 1 1 d U . . H20A H 0.2806 -0.6129 -0.0759 0.062 Uiso 1 1 calc R . . H20B H 0.2946 -0.4827 -0.0336 0.062 Uiso 1 1 calc R . . H20C H 0.4046 -0.5106 -0.0251 0.062 Uiso 1 1 calc R . . C21 C 0.6065(3) -0.4533(4) -0.2399(2) 0.0367(8) Uani 1 1 d U . . H21A H 0.6746 -0.3749 -0.2162 0.055 Uiso 1 1 calc R . . H21B H 0.5930 -0.4702 -0.2940 0.055 Uiso 1 1 calc R . . H21C H 0.6219 -0.5153 -0.2273 0.055 Uiso 1 1 calc R . . C22 C 0.3272(3) -0.3254(3) -0.43940(19) 0.0294(7) Uani 1 1 d . . . H22A H 0.3896 -0.2592 -0.4507 0.044 Uiso 1 1 calc R . . H22B H 0.2895 -0.3950 -0.4844 0.044 Uiso 1 1 calc R . . H22C H 0.3613 -0.3465 -0.4005 0.044 Uiso 1 1 calc R . . C23 C 0.1605(3) -0.2385(3) -0.48447(19) 0.0321(8) Uani 1 1 d . . . H23A H 0.1140 -0.1968 -0.4676 0.048 Uiso 1 1 calc R . . H23B H 0.1113 -0.3117 -0.5258 0.048 Uiso 1 1 calc R . . H23C H 0.2278 -0.1862 -0.5012 0.048 Uiso 1 1 calc R . . C24 C 0.3220(3) -0.0396(3) -0.33077(18) 0.0247(7) Uani 1 1 d U . . C25 C 0.2655(3) 0.0313(3) -0.30607(19) 0.0277(7) Uani 1 1 d U . . H25 H 0.1957 -0.0018 -0.2877 0.033 Uiso 1 1 calc R . . C26 C 0.3089(3) 0.1487(3) -0.3078(2) 0.0343(8) Uani 1 1 d U . . C27 C 0.4091(4) 0.1957(3) -0.3361(2) 0.0404(9) Uani 1 1 d U . . H27 H 0.4393 0.2759 -0.3372 0.049 Uiso 1 1 calc R . . C28 C 0.4667(3) 0.1279(3) -0.3630(2) 0.0379(9) Uani 1 1 d U . . C29 C 0.4231(3) 0.0102(3) -0.36001(19) 0.0298(7) Uani 1 1 d U . . H29 H 0.4621 -0.0363 -0.3779 0.036 Uiso 1 1 calc R . . C30 C 0.2451(4) 0.2209(4) -0.2803(3) 0.0501(11) Uani 1 1 d U . . H30A H 0.2975 0.3061 -0.2710 0.075 Uiso 1 1 calc R . . H30B H 0.2214 0.2081 -0.2341 0.075 Uiso 1 1 calc R . . H30C H 0.1751 0.1956 -0.3181 0.075 Uiso 1 1 calc R . . C31 C 0.5741(4) 0.1778(4) -0.3942(3) 0.0584(13) Uani 1 1 d U . . H31A H 0.5526 0.1473 -0.4487 0.088 Uiso 1 1 calc R . . H31B H 0.6315 0.1534 -0.3767 0.088 Uiso 1 1 calc R . . H31C H 0.6086 0.2655 -0.3778 0.088 Uiso 1 1 calc R . . C32 C 0.4746(3) 0.1112(3) -0.1490(2) 0.0317(8) Uani 1 1 d U . . H32A H 0.4812 0.1061 -0.2013 0.038 Uiso 1 1 calc R . . H32B H 0.5358 0.0950 -0.1259 0.038 Uiso 1 1 calc R . . C33 C 0.4880(4) 0.2322(3) -0.1067(2) 0.0411(9) Uani 1 1 d U . . H33A H 0.4561 0.2658 -0.1391 0.049 Uiso 1 1 calc R . . H33B H 0.5715 0.2890 -0.0836 0.049 Uiso 1 1 calc R . . C34 C 0.4162(4) 0.2039(4) -0.0487(2) 0.0432(9) Uani 1 1 d U . . H34A H 0.3929 0.2673 -0.0278 0.052 Uiso 1 1 calc R . . H34B H 0.4597 0.1934 -0.0078 0.052 Uiso 1 1 calc R . . C35 C 0.3110(3) 0.0880(3) -0.0928(2) 0.0414(9) Uani 1 1 d U . . H35A H 0.2741 0.0407 -0.0599 0.050 Uiso 1 1 calc R . . H35B H 0.2516 0.1033 -0.1189 0.050 Uiso 1 1 calc R . . C36 C 0.5523(3) -0.1145(4) -0.2496(2) 0.0330(8) Uani 1 1 d U . . H36A H 0.5754 -0.0350 -0.2563 0.040 Uiso 1 1 calc R . . H36B H 0.5111 -0.1772 -0.2983 0.040 Uiso 1 1 calc R . . C37 C 0.6585(3) -0.1234(4) -0.2179(2) 0.0402(9) Uani 1 1 d U . . H37A H 0.6466 -0.2071 -0.2343 0.048 Uiso 1 1 calc R . . H37B H 0.7297 -0.0721 -0.2330 0.048 Uiso 1 1 calc R . . C38 C 0.6684(3) -0.0798(4) -0.1356(2) 0.0443(10) Uani 1 1 d U . . H38A H 0.7097 0.0088 -0.1163 0.053 Uiso 1 1 calc R . . H38B H 0.7112 -0.1121 -0.1092 0.053 Uiso 1 1 calc R . . C39 C 0.5425(3) -0.1270(3) -0.1267(2) 0.0308(8) Uani 1 1 d U . . H39A H 0.5138 -0.2077 -0.1209 0.037 Uiso 1 1 calc R . . H39B H 0.5344 -0.0729 -0.0827 0.037 Uiso 1 1 calc R . . C40 C -0.1129(6) 0.4262(5) -0.0879(4) 0.0852(18) Uani 1 1 d U . . H40A H -0.1321 0.4300 -0.0380 0.102 Uiso 1 1 calc R . . H40B H -0.0437 0.5025 -0.0835 0.102 Uiso 1 1 calc R . . C41 C -0.2061(6) 0.4115(5) -0.1361(4) 0.090(2) Uani 1 1 d DU . . H41A H -0.1838 0.4827 -0.1532 0.108 Uiso 1 1 calc R . . H41B H -0.2724 0.4036 -0.1105 0.108 Uiso 1 1 calc R . . C42 C -0.2412(5) 0.3093(5) -0.1973(3) 0.0803(17) Uani 1 1 d DU . . H42A H -0.2042 0.3304 -0.2389 0.096 Uiso 1 1 calc R . . H42B H -0.3278 0.2684 -0.2144 0.096 Uiso 1 1 calc R . . C43 C -0.2009(6) 0.2325(6) -0.1702(4) 0.0877(18) Uani 1 1 d U . . H43A H -0.1893 0.1772 -0.2118 0.105 Uiso 1 1 calc R . . H43B H -0.2584 0.1849 -0.1446 0.105 Uiso 1 1 calc R . . C44 C 0.1945(5) 1.0725(6) 0.4774(4) 0.0791(16) Uani 1 1 d U . . H44A H 0.1979 1.1521 0.4837 0.095 Uiso 1 1 calc R . . H44B H 0.1959 1.0584 0.5263 0.095 Uiso 1 1 calc R . . C45 C 0.2938(6) 1.0638(7) 0.4446(5) 0.102(2) Uani 1 1 d U . . H45A H 0.3590 1.1449 0.4538 0.122 Uiso 1 1 calc R . . H45B H 0.3236 1.0182 0.4677 0.122 Uiso 1 1 calc R . . C46 C 0.2538(6) 1.0072(7) 0.3704(3) 0.0799(16) Uani 1 1 d U . . H46A H 0.2729 0.9392 0.3563 0.096 Uiso 1 1 calc R . . H46B H 0.2949 1.0635 0.3433 0.096 Uiso 1 1 calc R . . C47 C 0.1357(7) 0.9658(7) 0.3496(4) 0.0967(19) Uani 1 1 d U . . H47A H 0.0991 0.8816 0.3168 0.116 Uiso 1 1 calc R . . H47B H 0.1193 1.0146 0.3220 0.116 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 0.01797(6) 0.01908(6) 0.01505(6) 0.00471(4) 0.00269(4) 0.00719(5) I1 0.03804(13) 0.03876(13) 0.01906(11) 0.01044(10) 0.00726(9) 0.01773(11) Si1 0.0190(4) 0.0263(5) 0.0195(4) 0.0037(4) 0.0026(3) 0.0108(4) Si2 0.0217(4) 0.0191(4) 0.0185(4) 0.0060(3) 0.0041(3) 0.0082(3) Si3 0.0230(4) 0.0239(4) 0.0150(4) 0.0082(3) 0.0046(3) 0.0095(4) N1 0.0199(13) 0.0280(14) 0.0167(13) 0.0026(11) 0.0018(10) 0.0119(11) N2 0.0198(13) 0.0217(13) 0.0199(13) 0.0084(11) 0.0038(11) 0.0090(11) N3 0.0229(13) 0.0185(13) 0.0222(14) 0.0057(11) 0.0041(11) 0.0069(11) O1 0.0256(12) 0.0199(11) 0.0268(13) 0.0025(10) 0.0064(10) 0.0061(10) O2 0.0202(11) 0.0312(13) 0.0241(12) 0.0070(10) 0.0026(9) 0.0107(10) O3 0.154(5) 0.135(5) 0.124(5) 0.047(4) 0.026(4) 0.073(4) O4 0.154(5) 0.135(5) 0.108(4) 0.049(4) 0.021(4) 0.055(4) C1 0.0180(14) 0.0210(15) 0.0141(14) 0.0041(12) 0.0022(11) 0.0078(12) C2 0.036(2) 0.040(2) 0.0263(19) 0.0067(16) 0.0011(15) 0.0245(17) C3 0.0214(17) 0.041(2) 0.032(2) 0.0030(17) 0.0033(15) 0.0086(16) C4 0.0165(14) 0.0279(16) 0.0165(15) 0.0026(12) -0.0001(12) 0.0079(12) C5 0.0231(15) 0.0262(16) 0.0237(17) 0.0044(13) 0.0022(13) 0.0088(13) C6 0.0251(16) 0.0282(17) 0.0276(17) 0.0002(13) -0.0021(13) 0.0125(14) C7 0.0249(16) 0.0409(19) 0.0210(17) 0.0005(14) 0.0026(13) 0.0185(15) C8 0.0228(15) 0.0359(18) 0.0220(16) 0.0058(14) 0.0053(13) 0.0123(14) C9 0.0218(15) 0.0277(16) 0.0233(16) 0.0084(13) 0.0040(13) 0.0107(13) C10 0.042(2) 0.033(2) 0.042(2) 0.0011(17) 0.0020(18) 0.0190(17) C11 0.041(2) 0.050(2) 0.032(2) 0.0121(18) 0.0180(17) 0.0179(19) C12 0.0359(19) 0.0234(17) 0.032(2) 0.0029(15) 0.0015(15) 0.0160(15) C13 0.0296(18) 0.0289(19) 0.033(2) 0.0134(16) 0.0054(15) 0.0045(15) C14 0.0213(14) 0.0180(14) 0.0198(15) 0.0041(12) 0.0004(12) 0.0076(12) C15 0.0255(16) 0.0217(15) 0.0250(17) 0.0076(13) 0.0057(13) 0.0102(13) C16 0.0356(18) 0.0272(17) 0.0231(17) 0.0099(13) 0.0026(14) 0.0139(14) C17 0.0324(18) 0.0287(18) 0.0336(19) 0.0109(15) -0.0020(15) 0.0154(15) C18 0.0220(15) 0.0238(16) 0.0312(18) 0.0030(13) 0.0010(13) 0.0111(13) C19 0.0249(15) 0.0246(16) 0.0204(16) 0.0065(13) 0.0035(13) 0.0106(13) C20 0.047(2) 0.047(2) 0.032(2) 0.0224(18) 0.0050(17) 0.0184(19) C21 0.0276(18) 0.046(2) 0.041(2) 0.0122(18) 0.0055(16) 0.0218(17) C22 0.0275(17) 0.0340(19) 0.0254(18) 0.0094(15) 0.0108(14) 0.0118(15) C23 0.037(2) 0.036(2) 0.0231(18) 0.0135(15) 0.0034(15) 0.0138(16) C24 0.0282(16) 0.0238(16) 0.0183(15) 0.0079(13) 0.0003(13) 0.0082(13) C25 0.0275(16) 0.0239(16) 0.0253(17) 0.0060(13) -0.0005(14) 0.0077(13) C26 0.0415(19) 0.0265(17) 0.0291(18) 0.0086(14) -0.0032(15) 0.0118(15) C27 0.047(2) 0.0229(17) 0.039(2) 0.0162(16) -0.0005(17) 0.0023(16) C28 0.0375(19) 0.0357(19) 0.0289(19) 0.0174(16) 0.0054(15) 0.0022(15) C29 0.0303(17) 0.0306(18) 0.0236(17) 0.0107(14) 0.0056(14) 0.0079(14) C30 0.059(3) 0.031(2) 0.059(3) 0.010(2) 0.000(2) 0.024(2) C31 0.051(3) 0.052(3) 0.056(3) 0.029(2) 0.018(2) 0.000(2) C32 0.0269(17) 0.0262(18) 0.0308(19) 0.0064(15) 0.0052(15) 0.0036(14) C33 0.038(2) 0.0248(18) 0.045(2) 0.0047(16) 0.0073(17) 0.0046(16) C34 0.047(2) 0.034(2) 0.040(2) 0.0012(17) 0.0068(18) 0.0173(18) C35 0.038(2) 0.0294(19) 0.050(2) 0.0029(17) 0.0172(18) 0.0130(16) C36 0.0290(18) 0.040(2) 0.0281(19) 0.0099(16) 0.0077(15) 0.0136(16) C37 0.0257(18) 0.049(2) 0.046(2) 0.0154(19) 0.0097(16) 0.0163(17) C38 0.0254(18) 0.065(3) 0.038(2) 0.012(2) 0.0001(16) 0.0199(18) C39 0.0277(17) 0.037(2) 0.0261(18) 0.0087(15) -0.0011(14) 0.0149(15) C40 0.092(4) 0.054(3) 0.104(4) 0.016(3) -0.017(3) 0.039(3) C41 0.086(4) 0.049(3) 0.115(4) 0.004(3) -0.050(3) 0.036(3) C42 0.055(3) 0.091(4) 0.075(3) 0.046(3) 0.008(3) 0.005(3) C43 0.086(4) 0.061(3) 0.088(4) 0.004(3) 0.022(3) 0.018(3) C44 0.081(4) 0.081(4) 0.068(4) 0.013(3) 0.003(3) 0.039(3) C45 0.088(4) 0.093(4) 0.123(5) 0.027(4) 0.027(4) 0.042(3) C46 0.089(4) 0.134(5) 0.070(3) 0.057(3) 0.050(3) 0.080(4) C47 0.139(5) 0.109(5) 0.064(4) 0.028(3) 0.039(4) 0.073(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 2.230(3) . ? U1 N2 2.241(3) . ? U1 N3 2.258(3) . ? U1 O2 2.484(2) . ? U1 O1 2.554(2) . ? U1 I1 3.1561(3) . ? Si1 N1 1.732(3) . ? Si1 C2 1.867(4) . ? Si1 C3 1.875(4) . ? Si1 C1 1.885(3) . ? Si2 N2 1.739(3) . ? Si2 C13 1.870(3) . ? Si2 C12 1.872(3) . ? Si2 C1 1.880(3) . ? Si3 N3 1.741(3) . ? Si3 C23 1.868(3) . ? Si3 C22 1.875(3) . ? Si3 C1 1.890(3) . ? N1 C4 1.418(4) . ? N2 C14 1.432(4) . ? N3 C24 1.417(4) . ? O1 C35 1.446(4) . ? O1 C32 1.458(4) . ? O2 C39 1.460(4) . ? O2 C36 1.462(4) . ? O3 C40 1.538(8) . ? O3 C43 1.540(8) . ? O4 C44 1.521(8) . ? O4 C47 1.540(8) . ? C4 C5 1.393(5) . ? C4 C9 1.398(4) . ? C5 C6 1.391(5) . ? C6 C7 1.390(5) . ? C6 C10 1.511(5) . ? C7 C8 1.389(5) . ? C8 C9 1.388(5) . ? C8 C11 1.503(5) . ? C14 C15 1.387(4) . ? C14 C19 1.402(4) . ? C15 C16 1.391(4) . ? C16 C17 1.387(5) . ? C16 C20 1.503(5) . ? C17 C18 1.378(5) . ? C18 C19 1.398(4) . ? C18 C21 1.507(5) . ? C24 C25 1.406(5) . ? C24 C29 1.408(5) . ? C25 C26 1.392(5) . ? C26 C27 1.383(5) . ? C26 C30 1.507(5) . ? C27 C28 1.396(6) . ? C28 C29 1.404(5) . ? C28 C31 1.491(5) . ? C32 C33 1.500(5) . ? C33 C34 1.503(6) . ? C34 C35 1.505(5) . ? C36 C37 1.502(5) . ? C37 C38 1.497(6) . ? C38 C39 1.504(5) . ? C40 C41 1.361(7) . ? C41 C42 1.396(6) . ? C42 C43 1.470(8) . ? C44 C45 1.488(9) . ? C45 C46 1.355(9) . ? C46 C47 1.359(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N2 95.32(9) . . ? N1 U1 N3 89.58(9) . . ? N2 U1 N3 93.50(9) . . ? N1 U1 O2 175.47(8) . . ? N2 U1 O2 81.85(8) . . ? N3 U1 O2 87.07(8) . . ? N1 U1 O1 108.78(9) . . ? N2 U1 O1 155.69(8) . . ? N3 U1 O1 89.92(8) . . ? O2 U1 O1 74.29(7) . . ? N1 U1 I1 92.74(7) . . ? N2 U1 I1 97.78(6) . . ? N3 U1 I1 168.22(7) . . ? O2 U1 I1 91.15(5) . . ? O1 U1 I1 78.40(5) . . ? N1 Si1 C2 109.40(15) . . ? N1 Si1 C3 112.55(15) . . ? C2 Si1 C3 103.95(18) . . ? N1 Si1 C1 105.02(13) . . ? C2 Si1 C1 114.41(15) . . ? C3 Si1 C1 111.70(16) . . ? N2 Si2 C13 108.93(15) . . ? N2 Si2 C12 112.80(15) . . ? C13 Si2 C12 104.21(17) . . ? N2 Si2 C1 104.77(13) . . ? C13 Si2 C1 115.38(15) . . ? C12 Si2 C1 110.97(15) . . ? N3 Si3 C23 111.33(15) . . ? N3 Si3 C22 111.32(15) . . ? C23 Si3 C22 104.45(16) . . ? N3 Si3 C1 105.74(13) . . ? C23 Si3 C1 111.04(15) . . ? C22 Si3 C1 113.10(15) . . ? C4 N1 Si1 118.7(2) . . ? C4 N1 U1 119.11(19) . . ? Si1 N1 U1 120.59(13) . . ? C14 N2 Si2 116.5(2) . . ? C14 N2 U1 123.06(19) . . ? Si2 N2 U1 118.67(13) . . ? C24 N3 Si3 118.7(2) . . ? C24 N3 U1 124.2(2) . . ? Si3 N3 U1 116.85(13) . . ? C35 O1 C32 108.8(3) . . ? C35 O1 U1 126.9(2) . . ? C32 O1 U1 124.19(19) . . ? C39 O2 C36 109.5(2) . . ? C39 O2 U1 122.10(19) . . ? C36 O2 U1 127.49(19) . . ? C40 O3 C43 98.0(5) . . ? C44 O4 C47 100.3(5) . . ? Si2 C1 Si1 113.72(15) . . ? Si2 C1 Si3 113.04(15) . . ? Si1 C1 Si3 113.01(15) . . ? C5 C4 C9 118.1(3) . . ? C5 C4 N1 120.7(3) . . ? C9 C4 N1 121.3(3) . . ? C6 C5 C4 121.7(3) . . ? C7 C6 C5 118.6(3) . . ? C7 C6 C10 121.1(3) . . ? C5 C6 C10 120.3(3) . . ? C8 C7 C6 121.3(3) . . ? C9 C8 C7 118.9(3) . . ? C9 C8 C11 120.6(3) . . ? C7 C8 C11 120.6(3) . . ? C8 C9 C4 121.4(3) . . ? C15 C14 C19 118.4(3) . . ? C15 C14 N2 120.6(3) . . ? C19 C14 N2 121.1(3) . . ? C14 C15 C16 121.4(3) . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C20 121.9(3) . . ? C15 C16 C20 119.3(3) . . ? C18 C17 C16 121.8(3) . . ? C17 C18 C19 118.5(3) . . ? C17 C18 C21 121.5(3) . . ? C19 C18 C21 120.0(3) . . ? C18 C19 C14 121.1(3) . . ? C25 C24 C29 117.9(3) . . ? C25 C24 N3 119.4(3) . . ? C29 C24 N3 122.7(3) . . ? C26 C25 C24 121.8(3) . . ? C27 C26 C25 118.9(4) . . ? C27 C26 C30 121.4(3) . . ? C25 C26 C30 119.7(4) . . ? C26 C27 C28 121.4(3) . . ? C27 C28 C29 119.1(3) . . ? C27 C28 C31 121.6(4) . . ? C29 C28 C31 119.2(4) . . ? C28 C29 C24 120.7(3) . . ? O1 C32 C33 105.5(3) . . ? C32 C33 C34 101.9(3) . . ? C33 C34 C35 102.0(3) . . ? O1 C35 C34 104.7(3) . . ? O2 C36 C37 105.2(3) . . ? C38 C37 C36 103.5(3) . . ? C37 C38 C39 103.7(3) . . ? O2 C39 C38 105.0(3) . . ? C41 C40 O3 110.0(5) . . ? C40 C41 C42 110.2(5) . . ? C41 C42 C43 105.0(5) . . ? C42 C43 O3 104.1(5) . . ? C45 C44 O4 103.9(6) . . ? C46 C45 C44 108.3(6) . . ? C45 C46 C47 112.5(6) . . ? C46 C47 O4 107.5(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.380 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.101 # Attachment '8.cif' data_udpsid _database_code_depnum_ccdc_archive 'CCDC 757630' #TrackingRef '8.cif' _refine_special_details ; Highly disordered lattice solvent moleculess (92 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 527.9 \%A**3, equating to 0.5 molecules of hexane per U-complex molecule in the unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. The N(3) aryl ring was disordered over two positions as was refined with a two part model in a 50:50 ratio. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H76 N4 O Si3 U, 0.5 (C6 H14)' _chemical_formula_sum 'C50 H83 N4 O Si3 U' _chemical_formula_weight 1078.50 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7504(3) _cell_length_b 21.2641(6) _cell_length_c 19.8990(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.515(2) _cell_angle_gamma 90.00 _cell_volume 5335.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18989 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.35 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 3.146 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.43 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 52857 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.38 _reflns_number_total 12052 _reflns_number_gt 9854 _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; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0427P)^2^+1.9480P] 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 12052 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _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 0.936207(9) 0.214191(5) 0.608581(6) 0.02426(5) Uani 1 1 d . A . N1 N 0.8480(2) 0.29772(13) 0.55652(15) 0.0323(6) Uani 1 1 d . . . N2 N 1.0450(2) 0.20261(13) 0.52939(15) 0.0316(6) Uani 1 1 d . . . N3 N 0.8008(2) 0.14706(14) 0.57310(14) 0.0319(6) Uani 1 1 d . . . N4 N 0.9825(2) 0.25246(15) 0.71197(14) 0.0343(7) Uani 1 1 d . . . Si1 Si 0.77451(8) 0.27961(5) 0.47798(5) 0.0330(2) Uani 1 1 d . A . Si2 Si 0.98321(8) 0.21315(5) 0.44640(5) 0.0389(2) Uani 1 1 d . A . Si3 Si 0.78787(8) 0.13157(5) 0.48638(5) 0.0327(2) Uani 1 1 d . A . O1 O 1.0351(2) 0.11601(13) 0.65774(14) 0.0463(7) Uani 1 1 d . . . C1 C 0.8363(3) 0.20617(17) 0.44798(18) 0.0333(8) Uani 1 1 d . . . H1A H 0.8054 0.2033 0.3989 0.040 Uiso 1 1 calc R A . C2 C 0.7709(4) 0.3452(2) 0.4140(2) 0.0550(11) Uani 1 1 d . . . H2A H 0.7343 0.3307 0.3699 0.083 Uiso 1 1 calc R A . H2B H 0.8435 0.3576 0.4095 0.083 Uiso 1 1 calc R . . H2C H 0.7330 0.3813 0.4293 0.083 Uiso 1 1 calc R . . C3 C 0.6313(3) 0.2692(2) 0.4879(2) 0.0434(9) Uani 1 1 d . . . H3A H 0.5900 0.2593 0.4436 0.065 Uiso 1 1 calc R A . H3B H 0.6046 0.3081 0.5055 0.065 Uiso 1 1 calc R . . H3C H 0.6247 0.2347 0.5196 0.065 Uiso 1 1 calc R . . C4 C 0.8292(3) 0.35659(18) 0.58598(19) 0.0399(8) Uani 1 1 d . . . C5 C 0.8907(5) 0.4095(2) 0.5750(2) 0.0620(13) Uani 1 1 d . . . H5A H 0.9439 0.4063 0.5464 0.074 Uiso 1 1 calc R . . C6 C 0.8733(6) 0.4672(2) 0.6065(3) 0.0825(19) Uani 1 1 d . . . C7 C 0.7960(6) 0.4713(3) 0.6479(3) 0.087(2) Uani 1 1 d . . . H7A H 0.7846 0.5105 0.6686 0.104 Uiso 1 1 calc R . . C8 C 0.7354(5) 0.4208(3) 0.6600(3) 0.0749(16) Uani 1 1 d . . . C9 C 0.7509(3) 0.3629(2) 0.6288(2) 0.0497(10) Uani 1 1 d . . . H9A H 0.7084 0.3278 0.6366 0.060 Uiso 1 1 calc R . . C10 C 0.9435(8) 0.5246(3) 0.5937(4) 0.154(4) Uani 1 1 d . . . H10A H 0.9700 0.5449 0.6371 0.231 Uiso 1 1 calc R . . H10B H 0.9012 0.5548 0.5639 0.231 Uiso 1 1 calc R . . H10C H 1.0035 0.5103 0.5722 0.231 Uiso 1 1 calc R . . C11 C 0.6504(5) 0.4254(4) 0.7071(4) 0.118(3) Uani 1 1 d . . . H11A H 0.6433 0.4693 0.7208 0.177 Uiso 1 1 calc R . . H11B H 0.6714 0.3995 0.7476 0.177 Uiso 1 1 calc R . . H11C H 0.5824 0.4105 0.6830 0.177 Uiso 1 1 calc R . . C12 C 1.0278(4) 0.1557(3) 0.3851(2) 0.0631(14) Uani 1 1 d . . . H12A H 0.9844 0.1608 0.3405 0.095 Uiso 1 1 calc R A . H12B H 1.0201 0.1128 0.4016 0.095 Uiso 1 1 calc R . . H12C H 1.1024 0.1636 0.3811 0.095 Uiso 1 1 calc R . . C13 C 1.0195(4) 0.2927(2) 0.4153(3) 0.0663(15) Uani 1 1 d . . . H13A H 0.9780 0.3010 0.3707 0.099 Uiso 1 1 calc R A . H13B H 1.0952 0.2935 0.4115 0.099 Uiso 1 1 calc R . . H13C H 1.0041 0.3251 0.4475 0.099 Uiso 1 1 calc R . . C14 C 1.1575(3) 0.19887(17) 0.53915(18) 0.0324(8) Uani 1 1 d . . . C15 C 1.2207(3) 0.2519(2) 0.5530(2) 0.0457(10) Uani 1 1 d . . . H15A H 1.1878 0.2917 0.5557 0.055 Uiso 1 1 calc R . . C16 C 1.3314(3) 0.2481(2) 0.5630(2) 0.0531(12) Uani 1 1 d . . . C17 C 1.3788(3) 0.1894(2) 0.5591(2) 0.0466(10) Uani 1 1 d . . . H17A H 1.4539 0.1863 0.5664 0.056 Uiso 1 1 calc R . . C18 C 1.3193(3) 0.1358(2) 0.5451(2) 0.0447(9) Uani 1 1 d . . . C19 C 1.2083(3) 0.14115(19) 0.5355(2) 0.0398(8) Uani 1 1 d . . . H19A H 1.1665 0.1043 0.5263 0.048 Uiso 1 1 calc R . . C20 C 1.3976(4) 0.3076(3) 0.5745(4) 0.091(2) Uani 1 1 d . . . H20A H 1.3525 0.3426 0.5848 0.137 Uiso 1 1 calc R . . H20B H 1.4283 0.3174 0.5334 0.137 Uiso 1 1 calc R . . H20C H 1.4547 0.3012 0.6126 0.137 Uiso 1 1 calc R . . C21 C 1.3721(4) 0.0721(2) 0.5418(3) 0.0754(16) Uani 1 1 d . . . H21A H 1.4483 0.0780 0.5416 0.113 Uiso 1 1 calc R . . H21B H 1.3411 0.0503 0.5002 0.113 Uiso 1 1 calc R . . H21C H 1.3610 0.0470 0.5814 0.113 Uiso 1 1 calc R . . C22 C 0.8672(3) 0.0613(2) 0.4671(2) 0.0532(11) Uani 1 1 d . . . H22A H 0.8620 0.0563 0.4178 0.080 Uiso 1 1 calc R A . H22B H 0.8394 0.0236 0.4867 0.080 Uiso 1 1 calc R . . H22C H 0.9416 0.0674 0.4868 0.080 Uiso 1 1 calc R . . C23 C 0.6470(3) 0.1128(2) 0.4499(2) 0.0468(10) Uani 1 1 d . . . H23A H 0.6420 0.1063 0.4008 0.070 Uiso 1 1 calc R A . H23B H 0.6009 0.1478 0.4586 0.070 Uiso 1 1 calc R . . H23C H 0.6245 0.0745 0.4712 0.070 Uiso 1 1 calc R . . C24 C 0.7198(15) 0.1305(7) 0.6195(10) 0.034(4) Uani 0.38(3) 1 d PG A 1 C25 C 0.6938(13) 0.0677(7) 0.6271(9) 0.033(3) Uani 0.38(3) 1 d PG A 1 H25A H 0.7264 0.0360 0.6037 0.039 Uiso 0.38(3) 1 calc PR A 1 C26 C 0.6201(11) 0.0513(9) 0.6690(9) 0.049(5) Uani 0.38(3) 1 d PG A 1 C27 C 0.5724(10) 0.0977(12) 0.7033(7) 0.061(6) Uani 0.38(3) 1 d PG A 1 H27A H 0.5220 0.0865 0.7319 0.073 Uiso 0.38(3) 1 calc PR A 1 C28 C 0.5984(12) 0.1605(11) 0.6957(7) 0.049(4) Uani 0.38(3) 1 d PG A 1 C29 C 0.6722(15) 0.1769(8) 0.6538(10) 0.033(3) Uani 0.38(3) 1 d PG A 1 H29A H 0.6900 0.2199 0.6486 0.040 Uiso 0.38(3) 1 calc PR A 1 C30 C 0.583(2) -0.0172(12) 0.6732(15) 0.080(8) Uani 0.38(3) 1 d P A 1 H30A H 0.5949 -0.0310 0.7207 0.120 Uiso 0.38(3) 1 calc PR A 1 H30B H 0.6239 -0.0441 0.6464 0.120 Uiso 0.38(3) 1 calc PR A 1 H30C H 0.5077 -0.0202 0.6551 0.120 Uiso 0.38(3) 1 calc PR A 1 C31 C 0.5460(18) 0.2135(15) 0.7294(12) 0.077(6) Uani 0.38(3) 1 d P A 1 H31A H 0.5425 0.2024 0.7768 0.115 Uiso 0.38(3) 1 calc PR A 1 H31B H 0.4742 0.2202 0.7053 0.115 Uiso 0.38(3) 1 calc PR A 1 H31C H 0.5876 0.2521 0.7279 0.115 Uiso 0.38(3) 1 calc PR A 1 C24A C 0.7313(9) 0.1174(5) 0.6109(6) 0.030(2) Uani 0.62(3) 1 d PG A 2 C25A C 0.7175(9) 0.0525(5) 0.6117(6) 0.039(2) Uani 0.62(3) 1 d PG A 2 H25B H 0.7559 0.0263 0.5854 0.046 Uiso 0.62(3) 1 calc PR A 2 C26A C 0.6475(9) 0.0262(7) 0.6511(5) 0.052(3) Uani 0.62(3) 1 d PG A 2 C27A C 0.5913(7) 0.0646(9) 0.6897(5) 0.063(5) Uani 0.62(3) 1 d PG A 2 H27B H 0.5435 0.0466 0.7166 0.076 Uiso 0.62(3) 1 calc PR A 2 C28A C 0.6051(7) 0.1294(9) 0.6888(5) 0.061(4) Uani 0.62(3) 1 d PG A 2 C29A C 0.6751(9) 0.1558(6) 0.6494(6) 0.035(2) Uani 0.62(3) 1 d PG A 2 H29B H 0.6845 0.2001 0.6488 0.042 Uiso 0.62(3) 1 calc PR A 2 C30A C 0.6318(17) -0.0455(9) 0.6517(8) 0.093(6) Uani 0.62(3) 1 d P A 2 H30D H 0.6866 -0.0659 0.6295 0.139 Uiso 0.62(3) 1 calc PR A 2 H30E H 0.5617 -0.0561 0.6271 0.139 Uiso 0.62(3) 1 calc PR A 2 H30F H 0.6372 -0.0603 0.6987 0.139 Uiso 0.62(3) 1 calc PR A 2 C31A C 0.5404(11) 0.1704(14) 0.7289(7) 0.097(7) Uani 0.62(3) 1 d P A 2 H31D H 0.5645 0.2141 0.7273 0.145 Uiso 0.62(3) 1 calc PR A 2 H31E H 0.5494 0.1561 0.7762 0.145 Uiso 0.62(3) 1 calc PR A 2 H31F H 0.4654 0.1678 0.7092 0.145 Uiso 0.62(3) 1 calc PR A 2 C32 C 0.9500(3) 0.2401(2) 0.77915(19) 0.0440(9) Uani 1 1 d . A . H32A H 1.0104 0.2520 0.8149 0.053 Uiso 1 1 calc R . . C33 C 0.9277(4) 0.1686(3) 0.7872(2) 0.0632(13) Uani 1 1 d . . . H33A H 0.8708 0.1556 0.7504 0.076 Uiso 1 1 calc R A . H33B H 0.9924 0.1447 0.7814 0.076 Uiso 1 1 calc R . . C34 C 0.8949(4) 0.1513(3) 0.8552(3) 0.0741(16) Uani 1 1 d . A . H34A H 0.8786 0.1058 0.8555 0.089 Uiso 1 1 calc R . . H34B H 0.9549 0.1595 0.8918 0.089 Uiso 1 1 calc R . . C35 C 0.8034(5) 0.1865(4) 0.8688(3) 0.0898(19) Uani 1 1 d . . . H35A H 0.7884 0.1758 0.9148 0.108 Uiso 1 1 calc R A . H35B H 0.7411 0.1738 0.8358 0.108 Uiso 1 1 calc R . . C36 C 0.8176(5) 0.2554(4) 0.8644(3) 0.095(2) Uani 1 1 d . A . H36A H 0.8720 0.2692 0.9022 0.114 Uiso 1 1 calc R . . H36B H 0.7501 0.2765 0.8696 0.114 Uiso 1 1 calc R . . C37 C 0.8536(4) 0.2765(3) 0.7923(3) 0.0793(18) Uani 1 1 d . . . H37A H 0.7946 0.2689 0.7549 0.095 Uiso 1 1 calc R A . H37B H 0.8697 0.3221 0.7934 0.095 Uiso 1 1 calc R . . C38 C 1.0655(3) 0.29932(19) 0.7100(2) 0.0442(10) Uani 1 1 d . A . H38A H 1.0728 0.3044 0.6609 0.053 Uiso 1 1 calc R . . C39 C 1.0380(5) 0.3640(2) 0.7342(3) 0.0729(15) Uani 1 1 d . . . H39A H 1.0335 0.3623 0.7835 0.088 Uiso 1 1 calc R A . H39B H 0.9679 0.3770 0.7101 0.088 Uiso 1 1 calc R . . C40 C 1.1212(6) 0.4120(3) 0.7215(4) 0.112(3) Uani 1 1 d . A . H40A H 1.1038 0.4533 0.7401 0.134 Uiso 1 1 calc R . . H40B H 1.1205 0.4169 0.6719 0.134 Uiso 1 1 calc R . . C41 C 1.2327(5) 0.3915(3) 0.7550(4) 0.098(2) Uani 1 1 d . . . H41A H 1.2858 0.4217 0.7428 0.118 Uiso 1 1 calc R A . H41B H 1.2359 0.3923 0.8050 0.118 Uiso 1 1 calc R . . C42 C 1.2596(5) 0.3272(3) 0.7333(3) 0.0839(19) Uani 1 1 d . A . H42A H 1.3292 0.3145 0.7587 0.101 Uiso 1 1 calc R . . H42B H 1.2658 0.3277 0.6843 0.101 Uiso 1 1 calc R . . C43 C 1.1757(3) 0.2790(2) 0.7460(3) 0.0559(12) Uani 1 1 d . . . H43A H 1.1743 0.2752 0.7954 0.067 Uiso 1 1 calc R A . H43B H 1.1941 0.2374 0.7287 0.067 Uiso 1 1 calc R . . C44 C 0.9912(4) 0.05352(19) 0.6576(3) 0.0610(13) Uani 1 1 d . A . H44A H 0.9875 0.0342 0.6120 0.073 Uiso 1 1 calc R . . H44B H 0.9188 0.0548 0.6700 0.073 Uiso 1 1 calc R . . C45 C 1.0639(4) 0.0165(2) 0.7092(3) 0.0689(14) Uani 1 1 d . . . H45A H 1.0640 -0.0287 0.6971 0.083 Uiso 1 1 calc R A . H45B H 1.0445 0.0211 0.7553 0.083 Uiso 1 1 calc R . . C46 C 1.1708(4) 0.0472(2) 0.7041(3) 0.0722(15) Uani 1 1 d . A . H46A H 1.2217 0.0403 0.7461 0.087 Uiso 1 1 calc R . . H46B H 1.2015 0.0307 0.6648 0.087 Uiso 1 1 calc R . . C47 C 1.1427(3) 0.1152(2) 0.6950(2) 0.0543(11) Uani 1 1 d . A . H47A H 1.1453 0.1363 0.7395 0.065 Uiso 1 1 calc R . . H47B H 1.1923 0.1368 0.6688 0.065 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 0.02222(6) 0.02738(7) 0.02324(7) -0.00196(5) 0.00356(4) -0.00031(5) N1 0.0336(16) 0.0294(15) 0.0338(16) -0.0024(12) 0.0042(13) 0.0008(12) N2 0.0269(14) 0.0363(16) 0.0323(15) -0.0021(12) 0.0068(12) 0.0023(12) N3 0.0281(14) 0.0350(15) 0.0316(15) 0.0006(13) 0.0010(12) -0.0027(12) N4 0.0306(15) 0.0435(18) 0.0286(15) -0.0092(13) 0.0036(12) 0.0006(13) Si1 0.0343(5) 0.0348(5) 0.0292(5) 0.0035(4) 0.0028(4) 0.0047(4) Si2 0.0308(5) 0.0586(7) 0.0292(5) -0.0026(5) 0.0102(4) -0.0001(5) Si3 0.0295(5) 0.0328(5) 0.0334(5) -0.0059(4) -0.0027(4) 0.0000(4) O1 0.0504(16) 0.0429(15) 0.0423(16) 0.0022(12) -0.0047(13) 0.0123(13) C1 0.0302(18) 0.043(2) 0.0265(17) -0.0037(15) 0.0038(14) 0.0020(15) C2 0.071(3) 0.047(3) 0.045(2) 0.014(2) 0.003(2) 0.008(2) C3 0.0311(19) 0.053(2) 0.044(2) -0.0044(18) -0.0018(17) 0.0124(17) C4 0.049(2) 0.0326(19) 0.0349(19) -0.0009(16) -0.0055(16) 0.0081(17) C5 0.101(4) 0.037(2) 0.048(3) 0.001(2) 0.010(3) -0.011(2) C6 0.141(6) 0.030(2) 0.069(4) 0.002(2) -0.012(4) -0.011(3) C7 0.139(6) 0.042(3) 0.071(4) -0.019(3) -0.012(4) 0.037(3) C8 0.079(4) 0.070(4) 0.069(3) -0.024(3) -0.011(3) 0.038(3) C9 0.049(2) 0.050(2) 0.048(2) -0.012(2) -0.0012(19) 0.013(2) C10 0.303(14) 0.042(3) 0.115(6) -0.006(3) 0.024(7) -0.063(5) C11 0.083(4) 0.160(7) 0.110(6) -0.069(5) 0.008(4) 0.050(5) C12 0.043(2) 0.105(4) 0.044(3) -0.027(3) 0.014(2) 0.008(3) C13 0.054(3) 0.093(4) 0.055(3) 0.031(3) 0.021(2) -0.006(3) C14 0.0267(17) 0.042(2) 0.0300(18) 0.0001(15) 0.0090(14) -0.0001(14) C15 0.036(2) 0.046(2) 0.059(3) -0.012(2) 0.0197(19) -0.0077(18) C16 0.035(2) 0.062(3) 0.067(3) -0.020(2) 0.022(2) -0.015(2) C17 0.0283(19) 0.066(3) 0.047(2) -0.013(2) 0.0099(17) -0.0023(19) C18 0.0326(19) 0.056(3) 0.046(2) -0.0043(19) 0.0061(17) 0.0059(18) C19 0.0303(18) 0.044(2) 0.045(2) -0.0073(18) 0.0047(16) -0.0039(16) C20 0.051(3) 0.078(4) 0.151(6) -0.039(4) 0.038(4) -0.030(3) C21 0.040(2) 0.066(3) 0.119(5) -0.018(3) 0.007(3) 0.016(2) C22 0.050(2) 0.043(2) 0.063(3) -0.018(2) -0.003(2) 0.0046(19) C23 0.038(2) 0.050(2) 0.048(2) -0.0032(19) -0.0089(18) -0.0075(18) C24 0.037(10) 0.023(6) 0.038(10) 0.008(6) -0.008(6) -0.018(6) C25 0.036(7) 0.029(7) 0.032(7) 0.004(5) 0.002(5) -0.004(6) C26 0.029(7) 0.079(12) 0.039(9) 0.028(9) 0.008(7) -0.013(8) C27 0.051(9) 0.080(15) 0.051(10) 0.005(10) 0.002(7) -0.011(9) C28 0.039(7) 0.093(13) 0.017(5) -0.014(7) 0.005(5) 0.007(8) C29 0.034(6) 0.036(8) 0.028(6) -0.007(6) 0.000(5) -0.004(6) C30 0.067(13) 0.070(13) 0.092(15) 0.041(12) -0.023(11) -0.028(10) C31 0.061(10) 0.123(19) 0.052(9) -0.024(12) 0.028(7) 0.017(12) C24A 0.023(3) 0.043(5) 0.022(4) 0.000(4) 0.000(3) 0.002(4) C25A 0.041(5) 0.039(5) 0.033(5) 0.002(4) -0.001(3) -0.005(4) C26A 0.041(5) 0.072(7) 0.040(5) 0.022(5) -0.007(4) -0.022(5) C27A 0.035(5) 0.119(13) 0.036(5) 0.031(7) 0.005(4) -0.033(7) C28A 0.039(5) 0.108(12) 0.034(5) -0.011(7) 0.003(4) 0.007(6) C29A 0.031(4) 0.049(6) 0.025(4) -0.005(5) 0.007(3) 0.002(5) C30A 0.090(11) 0.091(11) 0.086(9) 0.047(8) -0.024(7) -0.060(9) C31A 0.057(6) 0.19(2) 0.043(5) -0.024(10) 0.014(5) 0.007(10) C32 0.0307(19) 0.071(3) 0.0295(19) -0.0089(19) 0.0035(15) 0.0045(19) C33 0.056(3) 0.091(4) 0.044(3) 0.005(2) 0.011(2) -0.026(3) C34 0.059(3) 0.115(5) 0.048(3) 0.009(3) 0.008(2) -0.026(3) C35 0.078(4) 0.125(6) 0.067(4) 0.015(4) 0.014(3) 0.014(4) C36 0.088(4) 0.159(6) 0.042(3) -0.006(4) 0.024(3) 0.070(5) C37 0.060(3) 0.125(5) 0.055(3) -0.006(3) 0.014(3) 0.038(3) C38 0.048(2) 0.051(2) 0.032(2) -0.0032(17) 0.0025(17) -0.0114(18) C39 0.095(4) 0.040(3) 0.073(3) -0.014(2) -0.021(3) -0.004(3) C40 0.135(6) 0.061(4) 0.121(6) -0.001(4) -0.037(5) -0.041(4) C41 0.102(5) 0.079(4) 0.102(5) -0.006(4) -0.026(4) -0.058(4) C42 0.068(3) 0.115(5) 0.067(4) -0.021(3) 0.006(3) -0.047(3) C43 0.038(2) 0.068(3) 0.062(3) -0.013(2) 0.008(2) -0.012(2) C44 0.076(3) 0.031(2) 0.066(3) -0.006(2) -0.021(2) 0.012(2) C45 0.080(4) 0.046(3) 0.072(3) 0.010(2) -0.018(3) 0.010(2) C46 0.069(3) 0.061(3) 0.077(4) -0.001(3) -0.018(3) 0.019(3) C47 0.048(2) 0.061(3) 0.048(3) 0.002(2) -0.010(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N4 2.210(3) . ? U1 N2 2.262(3) . ? U1 N1 2.269(3) . ? U1 N3 2.271(3) . ? U1 O1 2.557(3) . ? U1 C38 3.013(4) . ? N1 C4 1.418(5) . ? N1 Si1 1.742(3) . ? N2 C14 1.421(4) . ? N2 Si2 1.736(3) . ? N3 C24A 1.395(6) . ? N3 C24 1.525(12) . ? N3 Si3 1.741(3) . ? N4 C38 1.458(5) . ? N4 C32 1.480(5) . ? Si1 C3 1.878(4) . ? Si1 C2 1.884(4) . ? Si1 C1 1.885(4) . ? Si2 C12 1.873(4) . ? Si2 C13 1.883(5) . ? Si2 C1 1.884(4) . ? Si3 C22 1.875(4) . ? Si3 C23 1.878(4) . ? Si3 C1 1.903(4) . ? O1 C44 1.442(5) . ? O1 C47 1.460(5) . ? 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 1.407(6) . ? C4 C9 1.411(6) . ? C5 C6 1.412(7) . ? C5 H5A 0.9500 . ? C6 C7 1.377(9) . ? C6 C10 1.556(8) . ? C7 C8 1.367(9) . ? C7 H7A 0.9500 . ? C8 C9 1.406(6) . ? C8 C11 1.537(9) . ? C9 H9A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.389(5) . ? C14 C19 1.395(5) . ? C15 C16 1.399(5) . ? C15 H15A 0.9500 . ? C16 C17 1.394(6) . ? C16 C20 1.520(7) . ? C17 C18 1.374(6) . ? C17 H17A 0.9500 . ? C18 C19 1.405(5) . ? C18 C21 1.518(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C27 1.3900 . ? C26 C30 1.54(2) . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 C31 1.516(18) . ? C29 H29A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C24A C25A 1.3900 . ? C24A C29A 1.3900 . ? C25A C26A 1.3900 . ? C25A H25B 0.9500 . ? C26A C27A 1.3900 . ? C26A C30A 1.537(13) . ? C27A C28A 1.3900 . ? C27A H27B 0.9500 . ? C28A C29A 1.3900 . ? C28A C31A 1.507(13) . ? C29A H29B 0.9500 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32 C37 1.509(6) . ? C32 C33 1.558(7) . ? C32 H32A 1.0000 . ? C33 C34 1.520(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.446(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.478(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.633(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.515(6) . ? C38 C43 1.542(6) . ? C38 H38A 1.0000 . ? C39 C40 1.521(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.541(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.490(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.528(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.500(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.527(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.496(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 U1 N2 125.59(11) . . ? N4 U1 N1 100.53(11) . . ? N2 U1 N1 94.64(11) . . ? N4 U1 N3 127.36(11) . . ? N2 U1 N3 103.38(10) . . ? N1 U1 N3 92.72(10) . . ? N4 U1 O1 84.03(10) . . ? N2 U1 O1 81.91(10) . . ? N1 U1 O1 175.36(9) . . ? N3 U1 O1 85.11(10) . . ? N4 U1 C38 27.27(11) . . ? N2 U1 C38 101.60(11) . . ? N1 U1 C38 91.18(11) . . ? N3 U1 C38 154.31(11) . . ? O1 U1 C38 92.55(10) . . ? C4 N1 Si1 117.7(2) . . ? C4 N1 U1 127.2(2) . . ? Si1 N1 U1 113.64(14) . . ? C14 N2 Si2 116.4(2) . . ? C14 N2 U1 128.4(2) . . ? Si2 N2 U1 114.22(14) . . ? C24A N3 C24 13.6(7) . . ? C24A N3 Si3 118.3(6) . . ? C24 N3 Si3 125.7(8) . . ? C24A N3 U1 129.2(6) . . ? C24 N3 U1 120.6(8) . . ? Si3 N3 U1 112.54(14) . . ? C38 N4 C32 116.5(3) . . ? C38 N4 U1 108.7(2) . . ? C32 N4 U1 134.7(2) . . ? N1 Si1 C3 109.52(17) . . ? N1 Si1 C2 113.51(19) . . ? C3 Si1 C2 103.4(2) . . ? N1 Si1 C1 105.83(15) . . ? C3 Si1 C1 113.19(17) . . ? C2 Si1 C1 111.62(19) . . ? N2 Si2 C12 113.38(19) . . ? N2 Si2 C13 109.3(2) . . ? C12 Si2 C13 105.0(3) . . ? N2 Si2 C1 106.63(15) . . ? C12 Si2 C1 110.99(19) . . ? C13 Si2 C1 111.7(2) . . ? N3 Si3 C22 112.26(18) . . ? N3 Si3 C23 111.62(17) . . ? C22 Si3 C23 105.41(19) . . ? N3 Si3 C1 104.57(15) . . ? C22 Si3 C1 111.42(19) . . ? C23 Si3 C1 111.73(18) . . ? C44 O1 C47 109.0(3) . . ? C44 O1 U1 125.6(2) . . ? C47 O1 U1 125.2(2) . . ? Si2 C1 Si1 113.77(19) . . ? Si2 C1 Si3 117.05(19) . . ? Si1 C1 Si3 112.82(18) . . ? Si2 C1 H1A 103.7 . . ? Si1 C1 H1A 103.7 . . ? Si3 C1 H1A 103.7 . . ? 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 . . ? C5 C4 C9 118.6(4) . . ? C5 C4 N1 120.6(4) . . ? C9 C4 N1 120.8(4) . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C7 C6 C5 119.7(5) . . ? C7 C6 C10 121.9(6) . . ? C5 C6 C10 118.5(7) . . ? C8 C7 C6 122.0(5) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 119.3(5) . . ? C7 C8 C11 121.7(5) . . ? C9 C8 C11 119.0(6) . . ? C8 C9 C4 120.6(5) . . ? C8 C9 H9A 119.7 . . ? C4 C9 H9A 119.7 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 . . ? C15 C14 C19 117.7(3) . . ? C15 C14 N2 121.7(3) . . ? C19 C14 N2 120.6(3) . . ? C14 C15 C16 121.6(4) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C17 C16 C15 118.7(4) . . ? C17 C16 C20 121.2(4) . . ? C15 C16 C20 120.0(4) . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 118.4(4) . . ? C17 C18 C21 120.9(4) . . ? C19 C18 C21 120.7(4) . . ? C14 C19 C18 122.0(4) . . ? C14 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 C29 120.0 . . ? C25 C24 N3 118.8(8) . . ? C29 C24 N3 121.2(8) . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 C30 119.1(10) . . ? C25 C26 C30 120.6(10) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 C31 117.4(11) . . ? C27 C28 C31 122.6(11) . . ? C28 C29 C24 120.0 . . ? C28 C29 H29A 120.0 . . ? C24 C29 H29A 120.0 . . ? C25A C24A C29A 120.0 . . ? C25A C24A N3 123.2(5) . . ? C29A C24A N3 116.8(6) . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25B 120.0 . . ? C26A C25A H25B 120.0 . . ? C27A C26A C25A 120.0 . . ? C27A C26A C30A 120.1(7) . . ? C25A C26A C30A 119.9(7) . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27B 120.0 . . ? C28A C27A H27B 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A C31A 119.2(8) . . ? C29A C28A C31A 120.8(8) . . ? C28A C29A C24A 120.0 . . ? C28A C29A H29B 120.0 . . ? C24A C29A H29B 120.0 . . ? C26A C30A H30D 109.5 . . ? C26A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C26A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C28A C31A H31D 109.5 . . ? C28A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C28A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? N4 C32 C37 114.2(4) . . ? N4 C32 C33 110.2(3) . . ? C37 C32 C33 108.5(4) . . ? N4 C32 H32A 107.9 . . ? C37 C32 H32A 107.9 . . ? C33 C32 H32A 107.9 . . ? C34 C33 C32 113.9(4) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 112.1(5) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 113.1(5) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C37 112.1(5) . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C32 C37 C36 110.7(4) . . ? C32 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? N4 C38 C39 114.1(4) . . ? N4 C38 C43 114.3(3) . . ? C39 C38 C43 110.1(4) . . ? N4 C38 U1 43.99(16) . . ? C39 C38 U1 129.0(3) . . ? C43 C38 U1 120.9(3) . . ? N4 C38 H38A 105.8 . . ? C39 C38 H38A 105.8 . . ? C43 C38 H38A 105.8 . . ? U1 C38 H38A 62.1 . . ? C38 C39 C40 110.9(5) . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 111.0(5) . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C40 111.9(5) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 C43 111.7(5) . . ? C41 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C42 C43 C38 110.4(4) . . ? C42 C43 H43A 109.6 . . ? C38 C43 H43A 109.6 . . ? C42 C43 H43B 109.6 . . ? C38 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? O1 C44 C45 106.4(4) . . ? O1 C44 H44A 110.4 . . ? C45 C44 H44A 110.4 . . ? O1 C44 H44B 110.4 . . ? C45 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? C44 C45 C46 101.4(4) . . ? C44 C45 H45A 111.5 . . ? C46 C45 H45A 111.5 . . ? C44 C45 H45B 111.5 . . ? C46 C45 H45B 111.5 . . ? H45A C45 H45B 109.3 . . ? C47 C46 C45 102.8(4) . . ? C47 C46 H46A 111.2 . . ? C45 C46 H46A 111.2 . . ? C47 C46 H46B 111.2 . . ? C45 C46 H46B 111.2 . . ? H46A C46 H46B 109.1 . . ? O1 C47 C46 105.3(4) . . ? O1 C47 H47A 110.7 . . ? C46 C47 H47A 110.7 . . ? O1 C47 H47B 110.7 . . ? C46 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.401 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.093