# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1350 data_uch _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 N4 Si3 U' _chemical_formula_weight 723.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7602(5) _cell_length_b 13.3286(5) _cell_length_c 13.3902(5) _cell_angle_alpha 119.3350(10) _cell_angle_beta 109.0980(10) _cell_angle_gamma 92.8980(10) _cell_volume 1813.56(12) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9181 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 28.51 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 4.590 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.2074 _exptl_absorpt_correction_T_max 0.4604 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11113 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.51 _reflns_number_total 8070 _reflns_number_gt 6567 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8070 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.294904(18) 0.28011(2) 0.57337(2) 0.02666(10) Uani 1 1 d . . . Si11 Si 0.25735(17) 0.08644(16) 0.64352(18) 0.0337(4) Uani 1 1 d . . . Si12 Si 0.25712(15) 0.54327(16) 0.74669(17) 0.0303(4) Uani 1 1 d . . . Si13 Si 0.25031(15) 0.17688(17) 0.27505(17) 0.0310(4) Uani 1 1 d . . . N11 N 0.3696(5) 0.1764(5) 0.6554(5) 0.0366(13) Uani 1 1 d . . . N12 N 0.3639(5) 0.4713(5) 0.7250(5) 0.0375(14) Uani 1 1 d . . . N13 N 0.3577(5) 0.2468(5) 0.4235(5) 0.0353(13) Uiso 1 1 d . . . N14 N 0.5158(4) 0.3399(5) 0.6639(5) 0.0298(12) Uani 1 1 d . . . C101 C 0.5551(6) 0.2363(7) 0.6621(8) 0.0471(19) Uani 1 1 d . . . H10A H 0.5429 0.1748 0.5754 0.056 Uiso 1 1 calc R . . H10B H 0.6382 0.2619 0.7151 0.056 Uiso 1 1 calc R . . C102 C 0.4923(7) 0.1844(8) 0.7087(9) 0.053(2) Uani 1 1 d . . . H10C H 0.5036 0.1041 0.6848 0.064 Uiso 1 1 calc R . . H10D H 0.5230 0.2349 0.8012 0.064 Uiso 1 1 calc R . . C103 C 0.5556(6) 0.4432(7) 0.7924(7) 0.0453(19) Uani 1 1 d . . . H10E H 0.6376 0.4808 0.8227 0.054 Uiso 1 1 calc R . . H10F H 0.5486 0.4165 0.8477 0.054 Uiso 1 1 calc R . . C104 C 0.4876(6) 0.5330(7) 0.7996(8) 0.053(2) Uani 1 1 d . . . H10G H 0.5011 0.5902 0.8880 0.064 Uiso 1 1 calc R . . H10H H 0.5122 0.5778 0.7668 0.064 Uiso 1 1 calc R . . C105 C 0.5480(6) 0.3701(8) 0.5845(7) 0.048(2) Uani 1 1 d . . . H10I H 0.6305 0.3750 0.6033 0.058 Uiso 1 1 calc R . . H10J H 0.5353 0.4489 0.6029 0.058 Uiso 1 1 calc R . . C106 C 0.4782(6) 0.2779(9) 0.4485(7) 0.055(2) Uani 1 1 d . . . H10K H 0.4865 0.3090 0.3970 0.066 Uiso 1 1 calc R . . H10L H 0.5075 0.2057 0.4243 0.066 Uiso 1 1 calc R . . C107 C 0.2670(9) -0.0720(7) 0.5657(8) 0.060(2) Uani 1 1 d . . . H10M H 0.2048 -0.1215 0.5622 0.091 Uiso 1 1 calc R . . H10N H 0.3411 -0.0768 0.6138 0.091 Uiso 1 1 calc R . . H10O H 0.2601 -0.1004 0.4806 0.091 Uiso 1 1 calc R . . C108 C 0.1335(8) 0.1126(9) 0.5454(8) 0.067(3) Uani 1 1 d . . . H10P H 0.0799 0.1457 0.5847 0.080 Uiso 1 1 calc R . . H10Q H 0.0922 0.0437 0.4583 0.080 Uiso 1 1 calc R . . C109 C 0.2544(6) 0.1374(6) 0.8019(6) 0.0380(16) Uani 1 1 d . . . C110 C 0.3610(8) 0.1226(8) 0.8844(8) 0.060(2) Uani 1 1 d . . . H11A H 0.3582 0.1490 0.9657 0.090 Uiso 1 1 calc R . . H11B H 0.4303 0.1707 0.8970 0.090 Uiso 1 1 calc R . . H11C H 0.3624 0.0386 0.8430 0.090 Uiso 1 1 calc R . . C111 C 0.2542(8) 0.2683(7) 0.8669(7) 0.055(2) Uani 1 1 d . . . H11D H 0.2530 0.2953 0.9489 0.082 Uiso 1 1 calc R . . H11E H 0.1860 0.2786 0.8156 0.082 Uiso 1 1 calc R . . H11F H 0.3233 0.3153 0.8779 0.082 Uiso 1 1 calc R . . C112 C 0.1474(8) 0.0659(9) 0.7870(8) 0.064(3) Uani 1 1 d . . . H11G H 0.1497 0.0906 0.8698 0.096 Uiso 1 1 calc R . . H11H H 0.1445 -0.0190 0.7410 0.096 Uiso 1 1 calc R . . H11I H 0.0792 0.0802 0.7405 0.096 Uiso 1 1 calc R . . C113 C 0.2747(8) 0.6207(7) 0.9135(7) 0.051(2) Uani 1 1 d . . . H11J H 0.2122 0.6594 0.9227 0.077 Uiso 1 1 calc R . . H11K H 0.3484 0.6808 0.9674 0.077 Uiso 1 1 calc R . . H11L H 0.2727 0.5625 0.9379 0.077 Uiso 1 1 calc R . . C114 C 0.1213(8) 0.4203(8) 0.6431(9) 0.068(3) Uani 1 1 d . . . H11M H 0.0562 0.4528 0.6554 0.102 Uiso 1 1 calc R . . H11N H 0.1269 0.3597 0.6644 0.102 Uiso 1 1 calc R . . H12L H 0.1098 0.3843 0.5553 0.102 Uiso 1 1 calc R . . C115 C 0.2511(6) 0.6539(6) 0.6954(7) 0.0387(16) Uani 1 1 d . . . C116 C 0.1444(8) 0.7017(8) 0.6997(9) 0.062(2) Uani 1 1 d . . . H11O H 0.1381 0.7538 0.6669 0.093 Uiso 1 1 calc R . . H11P H 0.1515 0.7470 0.7864 0.093 Uiso 1 1 calc R . . H11Q H 0.0758 0.6349 0.6484 0.093 Uiso 1 1 calc R . . C117 C 0.3590(8) 0.7584(7) 0.7810(9) 0.058(2) Uani 1 1 d . . . H11R H 0.3569 0.8108 0.7490 0.087 Uiso 1 1 calc R . . H11S H 0.4273 0.7277 0.7827 0.087 Uiso 1 1 calc R . . H11T H 0.3615 0.8033 0.8660 0.087 Uiso 1 1 calc R . . C118 C 0.2438(8) 0.5921(8) 0.5610(8) 0.055(2) Uani 1 1 d . . . H11U H 0.2450 0.6504 0.5367 0.083 Uiso 1 1 calc R . . H11V H 0.1724 0.5288 0.5039 0.083 Uiso 1 1 calc R . . H11W H 0.3094 0.5575 0.5566 0.083 Uiso 1 1 calc R . . C119 C 0.1127(6) 0.1850(7) 0.2950(8) 0.0470(19) Uiso 1 1 d . . . H11X H 0.0486 0.1465 0.2127 0.071 Uiso 1 1 calc R . . H11Y H 0.1127 0.2686 0.3456 0.071 Uiso 1 1 calc R . . H11Z H 0.1043 0.1443 0.3372 0.071 Uiso 1 1 calc R . . C120 C 0.2614(8) 0.2555(7) 0.1944(8) 0.052(2) Uani 1 1 d . . . H12A H 0.1974 0.2152 0.1118 0.079 Uiso 1 1 calc R . . H12B H 0.3341 0.2544 0.1843 0.079 Uiso 1 1 calc R . . H12C H 0.2585 0.3380 0.2446 0.079 Uiso 1 1 calc R . . C121 C 0.2455(6) 0.0137(7) 0.1742(7) 0.0407(17) Uani 1 1 d . . . C122 C 0.3510(8) 0.0018(8) 0.1425(9) 0.062(2) Uani 1 1 d . . . H12D H 0.3509 -0.0824 0.0966 0.093 Uiso 1 1 calc R . . H12E H 0.4208 0.0459 0.2200 0.093 Uiso 1 1 calc R . . H12G H 0.3489 0.0345 0.0905 0.093 Uiso 1 1 calc R . . C123 C 0.2421(8) -0.0473(7) 0.2461(8) 0.055(2) Uani 1 1 d . . . H12F H 0.2497 -0.1286 0.1996 0.082 Uiso 1 1 calc R . . H12J H 0.1689 -0.0499 0.2550 0.082 Uiso 1 1 calc R . . H12H H 0.3054 -0.0023 0.3292 0.082 Uiso 1 1 calc R . . C124 C 0.1381(8) -0.0498(8) 0.0512(7) 0.060(3) Uani 1 1 d . . . H12I H 0.1346 -0.1348 0.0036 0.091 Uiso 1 1 calc R . . H12M H 0.1413 -0.0156 0.0017 0.091 Uiso 1 1 calc R . . H12K H 0.0696 -0.0398 0.0694 0.091 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 0.02283(13) 0.03591(16) 0.02401(14) 0.01820(11) 0.00945(9) 0.00509(9) Si11 0.0436(10) 0.0315(9) 0.0287(10) 0.0183(8) 0.0148(8) 0.0055(8) Si12 0.0334(9) 0.0330(9) 0.0254(9) 0.0162(8) 0.0123(7) 0.0080(7) Si13 0.0342(9) 0.0405(10) 0.0245(9) 0.0198(8) 0.0148(8) 0.0109(8) N11 0.039(3) 0.046(3) 0.040(3) 0.033(3) 0.017(3) 0.015(3) N12 0.038(3) 0.033(3) 0.033(3) 0.014(3) 0.009(3) 0.010(2) N14 0.026(3) 0.041(3) 0.026(3) 0.021(3) 0.012(2) 0.005(2) C101 0.034(4) 0.054(5) 0.060(5) 0.032(4) 0.023(4) 0.021(3) C102 0.049(4) 0.066(5) 0.072(6) 0.054(5) 0.026(4) 0.024(4) C103 0.029(3) 0.053(5) 0.033(4) 0.015(4) 0.003(3) 0.006(3) C104 0.042(4) 0.041(4) 0.044(5) 0.007(4) 0.008(4) 0.003(3) C105 0.031(4) 0.071(5) 0.047(5) 0.037(4) 0.014(3) -0.003(4) C106 0.041(4) 0.093(7) 0.041(5) 0.039(5) 0.021(4) 0.009(4) C107 0.095(7) 0.041(5) 0.053(5) 0.026(4) 0.036(5) 0.019(4) C108 0.057(5) 0.099(7) 0.031(4) 0.032(5) 0.008(4) 0.024(5) C109 0.047(4) 0.040(4) 0.028(4) 0.021(3) 0.013(3) 0.003(3) C110 0.072(6) 0.079(6) 0.040(5) 0.043(5) 0.019(4) 0.019(5) C111 0.078(6) 0.053(5) 0.030(4) 0.018(4) 0.025(4) 0.019(4) C112 0.066(6) 0.084(7) 0.037(5) 0.031(5) 0.020(4) -0.005(5) C113 0.068(5) 0.052(5) 0.033(4) 0.020(4) 0.023(4) 0.010(4) C114 0.066(6) 0.070(6) 0.050(5) 0.036(5) 0.005(5) -0.017(5) C115 0.049(4) 0.040(4) 0.039(4) 0.026(3) 0.023(3) 0.018(3) C116 0.071(6) 0.076(6) 0.079(7) 0.056(6) 0.046(5) 0.047(5) C117 0.078(6) 0.042(5) 0.062(6) 0.032(4) 0.031(5) 0.013(4) C118 0.081(6) 0.065(5) 0.048(5) 0.041(5) 0.038(5) 0.028(5) C120 0.067(5) 0.060(5) 0.040(5) 0.034(4) 0.021(4) 0.012(4) C121 0.047(4) 0.047(4) 0.032(4) 0.022(3) 0.018(3) 0.019(3) C122 0.065(6) 0.063(6) 0.053(5) 0.021(5) 0.033(5) 0.033(5) C123 0.081(6) 0.048(5) 0.055(5) 0.036(4) 0.032(5) 0.029(4) C124 0.068(6) 0.054(5) 0.033(4) 0.012(4) 0.008(4) 0.021(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 N12 2.219(5) . y U1 N11 2.228(5) . y U1 N13 2.254(6) . y U1 N14 2.577(5) . y U1 C108 2.752(11) . y U1 C114 3.055(12) . y U1 Si11 3.2124(19) . ? U1 Si12 3.2937(19) . ? U1 Si13 3.3500(18) . ? Si11 N11 1.733(6) . ? Si11 C108 1.868(8) . ? Si11 C107 1.874(8) . ? Si11 C109 1.899(7) . ? Si12 N12 1.726(6) . ? Si12 C113 1.869(8) . ? Si12 C114 1.878(8) . ? Si12 C115 1.903(7) . ? Si13 N13 1.724(6) . ? Si13 C119 1.862(8) . ? Si13 C120 1.865(8) . ? Si13 C121 1.901(8) . ? N11 C102 1.465(9) . ? N12 C104 1.482(9) . ? N13 C106 1.453(9) . ? N14 C105 1.466(9) . ? N14 C103 1.467(9) . ? N14 C101 1.484(9) . ? C101 C102 1.484(12) . ? C103 C104 1.497(10) . ? C105 C106 1.502(11) . ? C109 C112 1.521(11) . ? C109 C111 1.522(10) . ? C109 C110 1.538(10) . ? C115 C117 1.535(11) . ? C115 C118 1.535(10) . ? C115 C116 1.538(10) . ? C121 C124 1.532(10) . ? C121 C122 1.533(11) . ? C121 C123 1.543(11) . ? 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 N12 U1 N11 107.2(2) . . y N12 U1 N13 108.5(2) . . y N11 U1 N13 107.7(2) . . y N12 U1 N14 69.02(19) . . y N11 U1 N14 68.79(19) . . y N13 U1 N14 68.96(19) . . y N12 U1 C108 127.7(3) . . y N11 U1 C108 66.1(2) . . y N13 U1 C108 123.1(2) . . y N14 U1 C108 134.8(2) . . y N12 U1 C114 62.9(2) . . y N11 U1 C114 123.8(2) . . y N13 U1 C114 128.3(2) . . y N14 U1 C114 131.90(19) . . y C108 U1 C114 78.3(3) . . y N12 U1 Si11 119.16(16) . . y N11 U1 Si11 30.93(15) . . y N13 U1 Si11 122.78(14) . . y N14 U1 Si11 99.68(12) . . y C108 U1 Si11 35.45(17) . . y C114 U1 Si11 101.66(18) . . y N12 U1 Si12 28.94(15) . . y N11 U1 Si12 121.46(16) . . y N13 U1 Si12 120.14(14) . . y N14 U1 Si12 97.92(13) . . y C108 U1 Si12 107.4(2) . . y C114 U1 Si12 34.14(15) . . y Si11 U1 Si12 116.91(5) . . y N12 U1 Si13 123.45(17) . . y N11 U1 Si13 118.11(16) . . y N13 U1 Si13 28.03(14) . . y N14 U1 Si13 96.90(12) . . y C108 U1 Si13 101.57(18) . . y C114 U1 Si13 110.44(18) . . y Si11 U1 Si13 117.12(5) . . y Si12 U1 Si13 120.04(5) . . y N11 Si11 C108 99.6(4) . . ? N11 Si11 C107 110.1(4) . . ? C108 Si11 C107 113.5(4) . . ? N11 Si11 C109 112.1(3) . . ? C108 Si11 C109 111.2(4) . . ? C107 Si11 C109 109.9(4) . . ? N11 Si11 U1 41.35(18) . . ? C108 Si11 U1 58.7(3) . . ? C107 Si11 U1 129.5(3) . . ? C109 Si11 U1 119.3(2) . . ? N12 Si12 C113 111.3(3) . . ? N12 Si12 C114 104.1(4) . . ? C113 Si12 C114 110.1(4) . . ? N12 Si12 C115 112.1(3) . . ? C113 Si12 C115 109.7(4) . . ? C114 Si12 C115 109.3(4) . . ? N12 Si12 U1 38.47(19) . . ? C113 Si12 U1 128.7(3) . . ? C114 Si12 U1 66.0(4) . . ? C115 Si12 U1 119.8(2) . . ? N13 Si13 C119 106.4(3) . . ? N13 Si13 C120 111.8(3) . . ? C119 Si13 C120 107.5(4) . . ? N13 Si13 C121 112.6(3) . . ? C119 Si13 C121 108.0(3) . . ? C120 Si13 C121 110.3(4) . . ? N13 Si13 U1 37.9(2) . . ? C119 Si13 U1 69.4(3) . . ? C120 Si13 U1 131.5(3) . . ? C121 Si13 U1 116.6(2) . . ? C102 N11 Si11 127.3(5) . . ? C102 N11 U1 125.0(5) . . ? Si11 N11 U1 107.7(3) . . ? C104 N12 Si12 122.7(5) . . ? C104 N12 U1 124.7(4) . . ? Si12 N12 U1 112.6(3) . . ? C106 N13 Si13 122.6(5) . . ? C106 N13 U1 123.3(5) . . ? Si13 N13 U1 114.1(3) . . ? C105 N14 C103 111.3(6) . . ? C105 N14 C101 112.8(6) . . ? C103 N14 C101 111.1(6) . . ? C105 N14 U1 107.1(4) . . ? C103 N14 U1 107.2(4) . . ? C101 N14 U1 106.9(4) . . ? C102 C101 N14 111.5(6) . . ? N11 C102 C101 110.1(6) . . ? N14 C103 C104 111.4(6) . . ? N12 C104 C103 109.5(6) . . ? N14 C105 C106 110.6(6) . . ? N13 C106 C105 111.2(6) . . ? Si11 C108 U1 85.8(4) . . ? C112 C109 C111 108.8(7) . . ? C112 C109 C110 108.9(7) . . ? C111 C109 C110 108.8(6) . . ? C112 C109 Si11 110.8(5) . . ? C111 C109 Si11 109.0(5) . . ? C110 C109 Si11 110.4(5) . . ? Si12 C114 U1 79.9(4) . . ? C117 C115 C118 108.3(7) . . ? C117 C115 C116 109.3(7) . . ? C118 C115 C116 109.0(7) . . ? C117 C115 Si12 110.9(5) . . ? C118 C115 Si12 109.8(5) . . ? C116 C115 Si12 109.5(6) . . ? C124 C121 C122 108.2(7) . . ? C124 C121 C123 108.4(7) . . ? C122 C121 C123 110.0(7) . . ? C124 C121 Si13 111.0(5) . . ? C122 C121 Si13 110.3(6) . . ? C123 C121 Si13 109.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 U1 Si11 N11 -74.2(4) . . . . y N13 U1 Si11 N11 68.3(4) . . . . y N14 U1 Si11 N11 -2.9(3) . . . . y C108 U1 Si11 N11 170.8(5) . . . . y C114 U1 Si11 N11 -139.5(3) . . . . y Si12 U1 Si11 N11 -107.0(3) . . . . y Si13 U1 Si11 N11 100.1(3) . . . . y N12 U1 Si11 C108 115.1(4) . . . . y N11 U1 Si11 C108 -170.8(5) . . . . y N13 U1 Si11 C108 -102.5(4) . . . . y N14 U1 Si11 C108 -173.6(4) . . . . y C114 U1 Si11 C108 49.7(4) . . . . y Si12 U1 Si11 C108 82.3(4) . . . . y Si13 U1 Si11 C108 -70.7(4) . . . . y N12 U1 Si11 C107 -148.9(4) . . . . y N11 U1 Si11 C107 -74.8(5) . . . . y N13 U1 Si11 C107 -6.5(4) . . . . y N14 U1 Si11 C107 -77.6(4) . . . . y C108 U1 Si11 C107 96.0(5) . . . . y C114 U1 Si11 C107 145.7(4) . . . . y Si12 U1 Si11 C107 178.3(4) . . . . y Si13 U1 Si11 C107 25.3(4) . . . . y N12 U1 Si11 C109 16.8(3) . . . . y N11 U1 Si11 C109 91.0(4) . . . . y N13 U1 Si11 C109 159.2(3) . . . . y N14 U1 Si11 C109 88.1(3) . . . . y C108 U1 Si11 C109 -98.3(4) . . . . y C114 U1 Si11 C109 -48.5(3) . . . . y Si12 U1 Si11 C109 -16.0(3) . . . . y Si13 U1 Si11 C109 -169.0(3) . . . . y N11 U1 Si12 N12 67.0(4) . . . . y N13 U1 Si12 N12 -73.2(4) . . . . y N14 U1 Si12 N12 -2.9(4) . . . . y C108 U1 Si12 N12 139.2(4) . . . . y C114 U1 Si12 N12 172.0(5) . . . . y Si11 U1 Si12 N12 102.2(3) . . . . y Si13 U1 Si12 N12 -105.7(3) . . . . y N12 U1 Si12 C113 -74.9(5) . . . . y N11 U1 Si12 C113 -7.9(4) . . . . y N13 U1 Si12 C113 -148.0(4) . . . . y N14 U1 Si12 C113 -77.8(4) . . . . y C108 U1 Si12 C113 64.4(4) . . . . y C114 U1 Si12 C113 97.2(5) . . . . y Si11 U1 Si12 C113 27.3(4) . . . . y Si13 U1 Si12 C113 179.5(4) . . . . y N12 U1 Si12 C114 -172.0(5) . . . . y N11 U1 Si12 C114 -105.0(4) . . . . y N13 U1 Si12 C114 114.8(4) . . . . y N14 U1 Si12 C114 -175.0(3) . . . . y C108 U1 Si12 C114 -32.8(4) . . . . y Si11 U1 Si12 C114 -69.8(3) . . . . y Si13 U1 Si12 C114 82.3(3) . . . . y N12 U1 Si12 C115 88.7(4) . . . . y N11 U1 Si12 C115 155.7(3) . . . . y N13 U1 Si12 C115 15.5(3) . . . . y N14 U1 Si12 C115 85.7(3) . . . . y C108 U1 Si12 C115 -132.1(3) . . . . y C114 U1 Si12 C115 -99.3(4) . . . . y Si11 U1 Si12 C115 -169.1(3) . . . . y Si13 U1 Si12 C115 -17.0(3) . . . . y N12 U1 Si13 N13 64.6(4) . . . . y N11 U1 Si13 N13 -74.4(3) . . . . y N14 U1 Si13 N13 -4.8(3) . . . . y C108 U1 Si13 N13 -143.4(4) . . . . y C114 U1 Si13 N13 134.9(3) . . . . y Si11 U1 Si13 N13 -109.4(3) . . . . y Si12 U1 Si13 N13 98.5(3) . . . . y N12 U1 Si13 C119 -101.8(3) . . . . y N11 U1 Si13 C119 119.3(3) . . . . y N13 U1 Si13 C119 -166.3(4) . . . . y N14 U1 Si13 C119 -171.1(3) . . . . y C108 U1 Si13 C119 50.3(3) . . . . y C114 U1 Si13 C119 -31.4(3) . . . . y Si11 U1 Si13 C119 84.3(3) . . . . y Si12 U1 Si13 C119 -67.8(3) . . . . y N12 U1 Si13 C120 -6.2(4) . . . . y N11 U1 Si13 C120 -145.2(4) . . . . y N13 U1 Si13 C120 -70.8(5) . . . . y N14 U1 Si13 C120 -75.6(4) . . . . y C108 U1 Si13 C120 145.9(4) . . . . y C114 U1 Si13 C120 64.2(4) . . . . y Si11 U1 Si13 C120 179.8(4) . . . . y Si12 U1 Si13 C120 27.8(4) . . . . y N12 U1 Si13 C121 157.8(3) . . . . y N11 U1 Si13 C121 18.8(3) . . . . y N13 U1 Si13 C121 93.2(4) . . . . y N14 U1 Si13 C121 88.4(3) . . . . y C108 U1 Si13 C121 -50.2(3) . . . . y C114 U1 Si13 C121 -131.9(3) . . . . y Si11 U1 Si13 C121 -16.2(3) . . . . y Si12 U1 Si13 C121 -168.3(3) . . . . y C108 Si11 N11 C102 -171.7(7) . . . . ? C107 Si11 N11 C102 -52.2(8) . . . . ? C109 Si11 N11 C102 70.6(7) . . . . ? U1 Si11 N11 C102 -179.7(8) . . . . ? C108 Si11 N11 U1 8.0(4) . . . . ? C107 Si11 N11 U1 127.6(4) . . . . ? C109 Si11 N11 U1 -109.7(3) . . . . ? N12 U1 N11 C102 -61.8(6) . . . . ? N13 U1 N11 C102 54.8(6) . . . . ? N14 U1 N11 C102 -3.3(6) . . . . ? C108 U1 N11 C102 173.9(7) . . . . ? C114 U1 N11 C102 -130.3(6) . . . . ? Si11 U1 N11 C102 179.8(8) . . . . ? Si12 U1 N11 C102 -89.6(6) . . . . ? Si13 U1 N11 C102 83.2(6) . . . . ? N12 U1 N11 Si11 118.4(3) . . . . ? N13 U1 N11 Si11 -124.9(3) . . . . ? N14 U1 N11 Si11 177.0(4) . . . . ? C108 U1 N11 Si11 -5.8(3) . . . . ? C114 U1 N11 Si11 49.9(4) . . . . ? Si12 U1 N11 Si11 90.6(3) . . . . ? Si13 U1 N11 Si11 -96.5(3) . . . . ? C113 Si12 N12 C104 -54.7(7) . . . . ? C114 Si12 N12 C104 -173.3(7) . . . . ? C115 Si12 N12 C104 68.7(7) . . . . ? U1 Si12 N12 C104 179.2(8) . . . . ? C113 Si12 N12 U1 126.1(4) . . . . ? C114 Si12 N12 U1 7.5(5) . . . . ? C115 Si12 N12 U1 -110.6(3) . . . . ? N11 U1 N12 C104 56.1(7) . . . . ? N13 U1 N12 C104 -60.0(7) . . . . ? N14 U1 N12 C104 -2.3(6) . . . . ? C108 U1 N12 C104 128.8(6) . . . . ? C114 U1 N12 C104 175.8(7) . . . . ? Si11 U1 N12 C104 87.2(6) . . . . ? Si12 U1 N12 C104 -179.2(8) . . . . ? Si13 U1 N12 C104 -86.6(6) . . . . ? N11 U1 N12 Si12 -124.7(3) . . . . ? N13 U1 N12 Si12 119.2(3) . . . . ? N14 U1 N12 Si12 176.9(4) . . . . ? C108 U1 N12 Si12 -51.9(4) . . . . ? C114 U1 N12 Si12 -5.0(3) . . . . ? Si11 U1 N12 Si12 -93.5(3) . . . . ? Si13 U1 N12 Si12 92.6(3) . . . . ? C119 Si13 N13 C106 -168.4(6) . . . . ? C120 Si13 N13 C106 -51.3(7) . . . . ? C121 Si13 N13 C106 73.5(7) . . . . ? U1 Si13 N13 C106 178.3(8) . . . . ? C119 Si13 N13 U1 13.3(4) . . . . ? C120 Si13 N13 U1 130.4(4) . . . . ? C121 Si13 N13 U1 -104.8(4) . . . . ? N12 U1 N13 C106 54.3(6) . . . . ? N11 U1 N13 C106 -61.4(6) . . . . ? N14 U1 N13 C106 -3.4(6) . . . . ? C108 U1 N13 C106 -134.0(6) . . . . ? C114 U1 N13 C106 124.0(6) . . . . ? Si11 U1 N13 C106 -91.5(6) . . . . ? Si12 U1 N13 C106 83.6(6) . . . . ? Si13 U1 N13 C106 -178.3(8) . . . . ? N12 U1 N13 Si13 -127.4(3) . . . . ? N11 U1 N13 Si13 116.9(3) . . . . ? N14 U1 N13 Si13 174.9(3) . . . . ? C108 U1 N13 Si13 44.2(4) . . . . ? C114 U1 N13 Si13 -57.7(4) . . . . ? Si11 U1 N13 Si13 86.8(3) . . . . ? Si12 U1 N13 Si13 -98.1(3) . . . . ? N12 U1 N14 C105 -94.4(5) . . . . ? N11 U1 N14 C105 146.4(5) . . . . ? N13 U1 N14 C105 26.4(5) . . . . ? C108 U1 N14 C105 142.7(5) . . . . ? C114 U1 N14 C105 -96.7(5) . . . . ? Si11 U1 N14 C105 147.9(5) . . . . ? Si12 U1 N14 C105 -92.9(5) . . . . ? Si13 U1 N14 C105 28.8(5) . . . . ? N12 U1 N14 C103 25.2(4) . . . . ? N11 U1 N14 C103 -94.0(5) . . . . ? N13 U1 N14 C103 146.0(5) . . . . ? C108 U1 N14 C103 -97.7(5) . . . . ? C114 U1 N14 C103 22.9(6) . . . . ? Si11 U1 N14 C103 -92.5(4) . . . . ? Si12 U1 N14 C103 26.7(4) . . . . ? Si13 U1 N14 C103 148.4(4) . . . . ? N12 U1 N14 C101 144.5(5) . . . . ? N11 U1 N14 C101 25.2(5) . . . . ? N13 U1 N14 C101 -94.7(5) . . . . ? C108 U1 N14 C101 21.6(6) . . . . ? C114 U1 N14 C101 142.2(5) . . . . ? Si11 U1 N14 C101 26.8(5) . . . . ? Si12 U1 N14 C101 146.0(4) . . . . ? Si13 U1 N14 C101 -92.3(4) . . . . ? C105 N14 C101 C102 -162.2(6) . . . . ? C103 N14 C101 C102 72.0(8) . . . . ? U1 N14 C101 C102 -44.7(7) . . . . ? Si11 N11 C102 C101 160.0(6) . . . . ? U1 N11 C102 C101 -19.7(10) . . . . ? N14 C101 C102 N11 43.5(9) . . . . ? C105 N14 C103 C104 71.8(8) . . . . ? C101 N14 C103 C104 -161.6(7) . . . . ? U1 N14 C103 C104 -45.1(7) . . . . ? Si12 N12 C104 C103 160.1(6) . . . . ? U1 N12 C104 C103 -20.8(10) . . . . ? N14 C103 C104 N12 44.3(10) . . . . ? C103 N14 C105 C106 -162.8(6) . . . . ? C101 N14 C105 C106 71.5(8) . . . . ? U1 N14 C105 C106 -45.9(7) . . . . ? Si13 N13 C106 C105 161.7(6) . . . . ? U1 N13 C106 C105 -20.2(10) . . . . ? N14 C105 C106 N13 45.0(10) . . . . ? N11 Si11 C108 U1 -6.2(3) . . . . ? C107 Si11 C108 U1 -123.2(4) . . . . ? C109 Si11 C108 U1 112.2(3) . . . . ? N12 U1 C108 Si11 -88.6(4) . . . . ? N11 U1 C108 Si11 5.2(3) . . . . ? N13 U1 C108 Si11 101.4(3) . . . . ? N14 U1 C108 Si11 8.9(5) . . . . ? C114 U1 C108 Si11 -130.3(4) . . . . ? Si12 U1 C108 Si11 -112.2(3) . . . . ? Si13 U1 C108 Si11 121.0(3) . . . . ? N11 Si11 C109 C112 173.4(6) . . . . ? C108 Si11 C109 C112 62.8(7) . . . . ? C107 Si11 C109 C112 -63.8(7) . . . . ? U1 Si11 C109 C112 127.9(5) . . . . ? N11 Si11 C109 C111 53.6(6) . . . . ? C108 Si11 C109 C111 -56.9(7) . . . . ? C107 Si11 C109 C111 176.5(6) . . . . ? U1 Si11 C109 C111 8.2(6) . . . . ? N11 Si11 C109 C110 -65.8(6) . . . . ? C108 Si11 C109 C110 -176.4(6) . . . . ? C107 Si11 C109 C110 57.0(7) . . . . ? U1 Si11 C109 C110 -111.3(5) . . . . ? N12 Si12 C114 U1 -5.1(3) . . . . ? C113 Si12 C114 U1 -124.5(3) . . . . ? C115 Si12 C114 U1 114.9(3) . . . . ? N12 U1 C114 Si12 4.3(3) . . . . ? N11 U1 C114 Si12 97.6(3) . . . . ? N13 U1 C114 Si12 -88.6(3) . . . . ? N14 U1 C114 Si12 6.7(5) . . . . ? C108 U1 C114 Si12 148.1(3) . . . . ? Si11 U1 C114 Si12 121.3(3) . . . . ? Si13 U1 C114 Si12 -113.7(2) . . . . ? N12 Si12 C115 C117 -67.2(6) . . . . ? C113 Si12 C115 C117 57.1(7) . . . . ? C114 Si12 C115 C117 177.9(6) . . . . ? U1 Si12 C115 C117 -109.3(5) . . . . ? N12 Si12 C115 C118 52.4(6) . . . . ? C113 Si12 C115 C118 176.7(6) . . . . ? C114 Si12 C115 C118 -62.5(7) . . . . ? U1 Si12 C115 C118 10.3(6) . . . . ? N12 Si12 C115 C116 172.1(5) . . . . ? C113 Si12 C115 C116 -63.6(6) . . . . ? C114 Si12 C115 C116 57.2(7) . . . . ? U1 Si12 C115 C116 130.0(5) . . . . ? N13 Si13 C121 C124 171.0(6) . . . . ? C119 Si13 C121 C124 53.8(7) . . . . ? C120 Si13 C121 C124 -63.4(7) . . . . ? U1 Si13 C121 C124 129.4(6) . . . . ? N13 Si13 C121 C122 -69.1(6) . . . . ? C119 Si13 C121 C122 173.7(6) . . . . ? C120 Si13 C121 C122 56.5(7) . . . . ? U1 Si13 C121 C122 -110.8(5) . . . . ? N13 Si13 C121 C123 51.7(6) . . . . ? C119 Si13 C121 C123 -65.4(6) . . . . ? C120 Si13 C121 C123 177.4(6) . . . . ? U1 Si13 C121 C123 10.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 2.834 _refine_diff_density_min -4.478 _refine_diff_density_rms 0.220 #===END data_rbm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H64 N4 Si3 U' _chemical_formula_weight 839.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.3244(10) _cell_length_b 12.7945(10) _cell_length_c 18.6257(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.7090(10) _cell_angle_gamma 90.00 _cell_volume 4091.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7606 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 28.55 _exptl_crystal_description Block _exptl_crystal_colour 'Light green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 4.080 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.2349 _exptl_absorpt_correction_T_max 0.4959 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24202 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.55 _reflns_number_total 9593 _reflns_number_gt 8001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+14.3580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9593 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.295602(12) 0.222536(17) 0.037595(11) 0.02798(9) Uani 1 1 d . . . Si1 Si 0.24606(11) -0.03092(15) 0.07693(11) 0.0389(4) Uani 1 1 d . . . Si2 Si 0.16464(11) 0.37415(15) -0.07471(11) 0.0381(4) Uani 1 1 d . . . Si3 Si 0.48243(11) 0.31608(17) 0.09833(13) 0.0436(5) Uani 1 1 d . . . N1 N 0.2518(3) 0.0618(4) 0.0107(3) 0.0368(12) Uani 1 1 d . . . N2 N 0.2578(3) 0.3257(5) -0.0561(3) 0.0391(13) Uani 1 1 d . . . N3 N 0.4257(3) 0.2181(4) 0.0554(3) 0.0341(12) Uani 1 1 d . . . N4 N 0.3509(3) 0.1509(5) -0.0805(3) 0.0389(13) Uani 1 1 d . . . C1 C 0.3230(5) 0.0429(7) -0.0934(4) 0.0504(19) Uani 1 1 d . . . H1A H 0.3613 -0.0065 -0.0679 0.060 Uiso 1 1 calc R . . H1B H 0.3176 0.0271 -0.1459 0.060 Uiso 1 1 calc R . . C2 C 0.2446(5) 0.0291(7) -0.0660(4) 0.0488(18) Uani 1 1 d . . . H2A H 0.2046 0.0721 -0.0954 0.059 Uiso 1 1 calc R . . H2B H 0.2282 -0.0450 -0.0706 0.059 Uiso 1 1 calc R . . C3 C 0.3189(6) 0.2205(7) -0.1412(4) 0.054(2) Uani 1 1 d . . . H3A H 0.2677 0.1937 -0.1636 0.065 Uiso 1 1 calc R . . H3B H 0.3544 0.2210 -0.1786 0.065 Uiso 1 1 calc R . . C4 C 0.3097(5) 0.3294(7) -0.1142(4) 0.0504(18) Uani 1 1 d . . . H4A H 0.2864 0.3748 -0.1545 0.060 Uiso 1 1 calc R . . H4B H 0.3611 0.3585 -0.0946 0.060 Uiso 1 1 calc R . . C5 C 0.4369(4) 0.1555(6) -0.0670(4) 0.0424(16) Uani 1 1 d . . . H5A H 0.4552 0.2242 -0.0824 0.051 Uiso 1 1 calc R . . H5B H 0.4594 0.1004 -0.0953 0.051 Uiso 1 1 calc R . . C6 C 0.4635(4) 0.1395(6) 0.0130(4) 0.0430(16) Uani 1 1 d . . . H6A H 0.4495 0.0683 0.0274 0.052 Uiso 1 1 calc R . . H6B H 0.5208 0.1469 0.0230 0.052 Uiso 1 1 calc R . . C7 C 0.2895(6) 0.0320(7) 0.1640(4) 0.057(2) Uani 1 1 d . . . H7A H 0.2837 -0.0148 0.2045 0.086 Uiso 1 1 calc R . . H7B H 0.2625 0.0980 0.1704 0.086 Uiso 1 1 calc R . . H7C H 0.3449 0.0458 0.1625 0.086 Uiso 1 1 calc R . . C8 C 0.3043(5) -0.1507(7) 0.0608(6) 0.065(2) Uani 1 1 d . . . H8A H 0.2997 -0.2021 0.0990 0.097 Uiso 1 1 calc R . . H8B H 0.3591 -0.1315 0.0613 0.097 Uiso 1 1 calc R . . H8C H 0.2843 -0.1810 0.0136 0.097 Uiso 1 1 calc R . . C9 C 0.1417(5) -0.0701(7) 0.0845(4) 0.0511(18) Uani 1 1 d . . . C10 C 0.0946(6) 0.0254(8) 0.1008(6) 0.068(3) Uani 1 1 d . . . H10A H 0.0394 0.0066 0.0973 0.101 Uiso 1 1 calc R . . H10B H 0.1012 0.0807 0.0657 0.101 Uiso 1 1 calc R . . H10C H 0.1129 0.0505 0.1499 0.101 Uiso 1 1 calc R . . C11 C 0.1042(5) -0.1177(9) 0.0129(6) 0.072(3) Uani 1 1 d . . . H11A H 0.0497 -0.1351 0.0163 0.107 Uiso 1 1 calc R . . H11B H 0.1324 -0.1814 0.0029 0.107 Uiso 1 1 calc R . . H11C H 0.1065 -0.0673 -0.0264 0.107 Uiso 1 1 calc R . . C12 C 0.1387(8) -0.1520(9) 0.1442(7) 0.088(4) Uani 1 1 d . . . H12A H 0.0849 -0.1763 0.1437 0.132 Uiso 1 1 calc R . . H12B H 0.1572 -0.1208 0.1915 0.132 Uiso 1 1 calc R . . H12C H 0.1720 -0.2114 0.1357 0.132 Uiso 1 1 calc R . . C13 C 0.1039(5) 0.2989(6) -0.0158(6) 0.057(2) Uani 1 1 d . . . H13A H 0.0490 0.3179 -0.0285 0.085 Uiso 1 1 calc R . . H13B H 0.1209 0.3158 0.0352 0.085 Uiso 1 1 calc R . . H13C H 0.1104 0.2238 -0.0235 0.085 Uiso 1 1 calc R . . C14 C 0.1231(6) 0.3479(8) -0.1706(5) 0.069(3) Uani 1 1 d . . . H14A H 0.0661 0.3515 -0.1754 0.104 Uiso 1 1 calc R . . H14B H 0.1389 0.2780 -0.1846 0.104 Uiso 1 1 calc R . . H14C H 0.1424 0.4002 -0.2023 0.104 Uiso 1 1 calc R . . C15 C 0.1586(4) 0.5192(6) -0.0564(4) 0.0426(16) Uani 1 1 d . . . C16 C 0.2116(5) 0.5810(7) -0.1004(6) 0.068(3) Uani 1 1 d . . . H16A H 0.2119 0.6548 -0.0861 0.103 Uiso 1 1 calc R . . H16B H 0.1921 0.5748 -0.1521 0.103 Uiso 1 1 calc R . . H16C H 0.2646 0.5531 -0.0912 0.103 Uiso 1 1 calc R . . C17 C 0.0741(5) 0.5580(7) -0.0757(5) 0.059(2) Uani 1 1 d . . . H17A H 0.0709 0.6316 -0.0618 0.089 Uiso 1 1 calc R . . H17B H 0.0395 0.5161 -0.0496 0.089 Uiso 1 1 calc R . . H17C H 0.0583 0.5509 -0.1280 0.089 Uiso 1 1 calc R . . C18 C 0.1823(8) 0.5415(7) 0.0245(6) 0.087(4) Uani 1 1 d . . . H18A H 0.1752 0.6160 0.0339 0.130 Uiso 1 1 calc R . . H18B H 0.2371 0.5227 0.0382 0.130 Uiso 1 1 calc R . . H18C H 0.1498 0.5001 0.0530 0.130 Uiso 1 1 calc R . . C19 C 0.4151(5) 0.4274(7) 0.1122(6) 0.067(3) Uani 1 1 d . . . H19A H 0.3878 0.4499 0.0652 0.100 Uiso 1 1 calc R . . H19B H 0.4453 0.4859 0.1353 0.100 Uiso 1 1 calc R . . H19C H 0.3769 0.4044 0.1432 0.100 Uiso 1 1 calc R . . C20 C 0.5548(5) 0.3666(8) 0.0405(6) 0.071(3) Uani 1 1 d . . . H20A H 0.5276 0.3881 -0.0067 0.106 Uiso 1 1 calc R . . H20B H 0.5924 0.3113 0.0336 0.106 Uiso 1 1 calc R . . H20C H 0.5825 0.4267 0.0644 0.106 Uiso 1 1 calc R . . C21 C 0.5363(5) 0.2717(8) 0.1887(5) 0.061(2) Uani 1 1 d . . . C22 C 0.5823(14) 0.3603(15) 0.2250(10) 0.209(13) Uani 1 1 d . . . H22A H 0.5790 0.3586 0.2771 0.314 Uiso 1 1 calc R . . H22B H 0.5612 0.4266 0.2047 0.314 Uiso 1 1 calc R . . H22C H 0.6369 0.3537 0.2171 0.314 Uiso 1 1 calc R . . C23 C 0.5915(11) 0.1856(19) 0.1785(7) 0.178(11) Uani 1 1 d . . . H23A H 0.6355 0.1878 0.2175 0.267 Uiso 1 1 calc R . . H23B H 0.6107 0.1940 0.1317 0.267 Uiso 1 1 calc R . . H23C H 0.5646 0.1183 0.1797 0.267 Uiso 1 1 calc R . . C24 C 0.4799(9) 0.2341(16) 0.2355(8) 0.129(7) Uani 1 1 d . . . H24A H 0.5054 0.2292 0.2856 0.194 Uiso 1 1 calc R . . H24B H 0.4605 0.1651 0.2189 0.194 Uiso 1 1 calc R . . H24C H 0.4362 0.2832 0.2330 0.194 Uiso 1 1 calc R . . C101 C 0.2446(5) 0.2969(6) 0.1441(4) 0.0431(16) Uani 1 1 d . . . C102 C 0.2140(4) 0.3606(5) 0.1778(3) 0.0357(14) Uani 1 1 d . . . C103 C 0.1768(4) 0.4428(5) 0.2143(3) 0.0292(12) Uani 1 1 d . . . C104 C 0.1024(4) 0.4292(5) 0.2331(4) 0.0376(14) Uani 1 1 d . . . H10E H 0.0764 0.3642 0.2238 0.045 Uiso 1 1 calc R . . C105 C 0.0657(4) 0.5094(5) 0.2654(4) 0.0400(15) Uani 1 1 d . . . H10F H 0.0151 0.4984 0.2783 0.048 Uiso 1 1 calc R . . C106 C 0.1017(4) 0.6057(5) 0.2791(4) 0.0379(15) Uani 1 1 d . . . C107 C 0.1761(4) 0.6184(6) 0.2616(4) 0.0432(16) Uani 1 1 d . . . H10G H 0.2022 0.6831 0.2715 0.052 Uiso 1 1 calc R . . C108 C 0.2132(4) 0.5381(5) 0.2299(4) 0.0386(14) Uani 1 1 d . . . H10H H 0.2646 0.5485 0.2188 0.046 Uiso 1 1 calc R . . C109 C 0.0606(6) 0.6953(6) 0.3130(5) 0.055(2) Uani 1 1 d . . . H10I H 0.0146 0.6682 0.3323 0.083 Uiso 1 1 calc R . . H10J H 0.0444 0.7483 0.2760 0.083 Uiso 1 1 calc R . . H10K H 0.0963 0.7267 0.3524 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02587(13) 0.02831(13) 0.02945(13) -0.00255(8) 0.00258(8) 0.00423(8) Si1 0.0397(10) 0.0287(9) 0.0456(10) 0.0002(8) -0.0040(8) 0.0045(7) Si2 0.0372(9) 0.0327(9) 0.0418(10) 0.0042(8) -0.0036(7) 0.0032(8) Si3 0.0297(9) 0.0417(11) 0.0595(12) -0.0121(10) 0.0060(8) -0.0032(8) N1 0.039(3) 0.032(3) 0.038(3) -0.009(2) -0.002(2) 0.001(2) N2 0.039(3) 0.045(3) 0.033(3) 0.009(2) 0.003(2) 0.009(3) N3 0.034(3) 0.028(3) 0.042(3) -0.007(2) 0.008(2) 0.000(2) N4 0.029(3) 0.052(4) 0.036(3) -0.005(3) 0.008(2) 0.010(2) C1 0.055(4) 0.059(5) 0.036(4) -0.024(3) 0.001(3) 0.005(4) C2 0.050(4) 0.052(4) 0.041(4) -0.014(3) -0.006(3) -0.009(4) C3 0.067(5) 0.062(5) 0.032(4) 0.006(3) 0.008(4) 0.008(4) C4 0.055(4) 0.058(5) 0.039(4) 0.016(4) 0.011(3) 0.007(4) C5 0.036(3) 0.047(4) 0.046(4) -0.006(3) 0.012(3) 0.013(3) C6 0.031(3) 0.049(4) 0.048(4) -0.012(3) 0.002(3) 0.015(3) C7 0.074(6) 0.047(4) 0.044(4) 0.005(3) -0.014(4) 0.006(4) C8 0.063(5) 0.037(4) 0.091(7) -0.003(4) 0.002(5) 0.016(4) C9 0.053(4) 0.046(4) 0.053(4) 0.012(4) 0.002(4) -0.008(4) C10 0.057(5) 0.064(6) 0.088(7) 0.011(5) 0.033(5) 0.009(4) C11 0.049(5) 0.070(6) 0.092(7) -0.001(6) -0.004(5) -0.021(5) C12 0.102(9) 0.072(7) 0.089(8) 0.037(6) 0.012(7) -0.012(6) C13 0.039(4) 0.033(4) 0.096(7) 0.012(4) 0.005(4) 0.004(3) C14 0.080(6) 0.059(6) 0.058(5) -0.012(4) -0.027(5) 0.013(5) C15 0.050(4) 0.035(3) 0.041(4) 0.009(3) 0.000(3) 0.010(3) C16 0.056(5) 0.043(5) 0.110(8) 0.017(5) 0.022(5) -0.011(4) C17 0.051(4) 0.044(4) 0.086(6) 0.021(4) 0.017(4) 0.015(4) C18 0.139(11) 0.036(5) 0.076(7) -0.007(4) -0.023(7) 0.032(6) C19 0.057(5) 0.043(5) 0.102(8) -0.018(5) 0.014(5) 0.007(4) C20 0.043(4) 0.069(6) 0.100(8) 0.014(6) 0.014(5) -0.016(4) C21 0.048(5) 0.073(6) 0.059(5) -0.020(4) -0.004(4) -0.004(4) C22 0.31(3) 0.133(15) 0.135(14) 0.012(12) -0.145(18) -0.101(18) C23 0.170(16) 0.30(3) 0.063(8) 0.024(12) -0.004(9) 0.177(19) C24 0.089(10) 0.23(2) 0.070(9) 0.040(10) 0.011(7) -0.014(11) C101 0.044(4) 0.045(4) 0.041(4) 0.003(3) 0.011(3) 0.003(3) C102 0.043(3) 0.030(3) 0.035(3) 0.002(3) 0.007(3) 0.007(3) C103 0.034(3) 0.024(3) 0.028(3) -0.002(2) -0.001(2) 0.004(2) C104 0.037(3) 0.030(3) 0.045(4) -0.005(3) 0.003(3) 0.001(3) C105 0.037(3) 0.034(3) 0.048(4) 0.000(3) 0.003(3) 0.008(3) C106 0.047(4) 0.027(3) 0.036(3) -0.001(3) -0.006(3) 0.013(3) C107 0.052(4) 0.029(3) 0.045(4) -0.004(3) -0.007(3) -0.007(3) C108 0.042(4) 0.034(3) 0.039(3) -0.004(3) 0.006(3) -0.002(3) C109 0.083(6) 0.030(3) 0.051(4) -0.012(3) 0.002(4) 0.017(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 N2 2.216(5) . y U1 N1 2.226(6) . y U1 N3 2.235(6) . y U1 C101 2.468(7) . y U1 N4 2.676(5) . y U1 Si1 3.458(2) . y U1 Si2 3.4660(18) . y Si1 N1 1.725(6) . y Si1 C7 1.875(8) . y Si1 C8 1.881(8) . y Si1 C9 1.900(8) . y Si2 N2 1.720(6) . y Si2 C14 1.865(8) . y Si2 C13 1.883(9) . y Si2 C15 1.893(8) . y Si3 N3 1.721(6) . y Si3 C20 1.875(9) . y Si3 C19 1.881(9) . y Si3 C21 1.899(10) . y N1 C2 1.477(9) . y N2 C4 1.498(9) . y N3 C6 1.484(8) . y N4 C1 1.473(10) . y N4 C5 1.479(8) . y N4 C3 1.486(10) . y C1 C2 1.524(11) . ? C3 C4 1.497(13) . ? C5 C6 1.513(10) . ? C9 C10 1.522(12) . ? C9 C11 1.530(13) . ? C9 C12 1.535(12) . ? C15 C16 1.531(11) . ? C15 C18 1.533(12) . ? C15 C17 1.541(10) . ? C21 C24 1.475(17) . ? C21 C23 1.486(17) . ? C21 C22 1.494(16) . ? C101 C102 1.196(10) . y C102 C103 1.449(8) . y C103 C108 1.386(9) . y C103 C104 1.392(9) . y C104 C105 1.386(9) . y C105 C106 1.389(10) . y C106 C107 1.381(11) . y C106 C109 1.529(10) . y C107 C108 1.385(10) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 U1 N1 108.5(2) . . y N2 U1 N3 108.5(2) . . y N1 U1 N3 108.47(19) . . y N2 U1 C101 107.7(2) . . y N1 U1 C101 112.9(2) . . y N3 U1 C101 110.7(2) . . y N2 U1 N4 70.0(2) . . y N1 U1 N4 69.3(2) . . y N3 U1 N4 69.42(19) . . y C101 U1 N4 177.3(2) . . y N2 U1 Si1 132.06(17) . . y N1 U1 Si1 25.12(15) . . y N3 U1 Si1 102.64(14) . . y C101 U1 Si1 93.74(19) . . y N4 U1 Si1 88.82(14) . . y N2 U1 Si2 24.62(15) . . y N1 U1 Si2 101.84(15) . . y N3 U1 Si2 132.03(15) . . y C101 U1 Si2 89.63(18) . . y N4 U1 Si2 88.45(13) . . y Si1 U1 Si2 119.45(5) . . y N1 Si1 C7 105.6(3) . . ? N1 Si1 C8 111.3(4) . . ? C7 Si1 C8 109.1(4) . . ? N1 Si1 C9 112.4(3) . . ? C7 Si1 C9 108.9(4) . . ? C8 Si1 C9 109.5(4) . . ? N1 Si1 U1 33.22(18) . . y C7 Si1 U1 72.4(3) . . ? C8 Si1 U1 125.2(3) . . ? C9 Si1 U1 121.9(3) . . ? N2 Si2 C14 111.0(4) . . ? N2 Si2 C13 106.3(3) . . ? C14 Si2 C13 107.0(5) . . ? N2 Si2 C15 112.9(3) . . ? C14 Si2 C15 109.1(4) . . ? C13 Si2 C15 110.3(4) . . ? N2 Si2 U1 32.47(19) . . y C14 Si2 U1 127.9(3) . . ? C13 Si2 U1 74.5(3) . . ? C15 Si2 U1 119.2(2) . . ? N3 Si3 C20 111.6(4) . . ? N3 Si3 C19 106.8(4) . . ? C20 Si3 C19 107.1(5) . . ? N3 Si3 C21 112.1(4) . . ? C20 Si3 C21 109.0(5) . . ? C19 Si3 C21 110.2(5) . . ? C2 N1 Si1 119.5(5) . . ? C2 N1 U1 117.5(5) . . ? Si1 N1 U1 121.7(3) . . y C4 N2 Si2 118.8(5) . . ? C4 N2 U1 116.4(4) . . ? Si2 N2 U1 122.9(3) . . ? C6 N3 Si3 118.4(5) . . ? C6 N3 U1 116.5(4) . . ? Si3 N3 U1 123.5(3) . . ? C1 N4 C5 111.5(6) . . ? C1 N4 C3 111.0(6) . . ? C5 N4 C3 111.8(6) . . ? C1 N4 U1 108.0(4) . . ? C5 N4 U1 108.0(4) . . ? C3 N4 U1 106.3(4) . . ? N4 C1 C2 110.0(6) . . ? N1 C2 C1 109.1(5) . . ? N4 C3 C4 110.4(6) . . ? C3 C4 N2 108.3(7) . . ? N4 C5 C6 109.2(6) . . ? N3 C6 C5 109.6(6) . . ? C10 C9 C11 108.5(8) . . ? C10 C9 C12 109.5(8) . . ? C11 C9 C12 107.9(8) . . ? C10 C9 Si1 110.1(6) . . ? C11 C9 Si1 109.7(6) . . ? C12 C9 Si1 111.1(7) . . ? C16 C15 C18 109.3(8) . . ? C16 C15 C17 109.1(6) . . ? C18 C15 C17 106.9(8) . . ? C16 C15 Si2 111.0(6) . . ? C18 C15 Si2 110.2(5) . . ? C17 C15 Si2 110.3(6) . . ? C24 C21 C23 108.8(14) . . ? C24 C21 C22 109.6(14) . . ? C23 C21 C22 107.9(15) . . ? C24 C21 Si3 109.6(8) . . ? C23 C21 Si3 110.9(7) . . ? C22 C21 Si3 110.1(9) . . ? C102 C101 U1 156.4(6) . . y C101 C102 C103 176.0(7) . . y C108 C103 C104 117.9(6) . . ? C108 C103 C102 121.2(6) . . y C104 C103 C102 120.9(6) . . y C105 C104 C103 120.7(6) . . ? C104 C105 C106 121.1(7) . . ? C107 C106 C105 118.1(6) . . ? C107 C106 C109 120.7(7) . . ? C105 C106 C109 121.2(7) . . ? C106 C107 C108 121.0(6) . . ? C107 C108 C103 121.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 U1 Si1 N1 23.2(4) . . . . y N3 U1 Si1 N1 -106.6(4) . . . . y C101 U1 Si1 N1 141.2(4) . . . . y N4 U1 Si1 N1 -38.0(4) . . . . y Si2 U1 Si1 N1 49.5(4) . . . . y N2 U1 Si1 C7 -161.0(4) . . . . ? N1 U1 Si1 C7 175.8(5) . . . . ? N3 U1 Si1 C7 69.1(4) . . . . ? C101 U1 Si1 C7 -43.0(4) . . . . y N4 U1 Si1 C7 137.7(3) . . . . ? Si2 U1 Si1 C7 -134.7(3) . . . . ? N2 U1 Si1 C8 97.7(5) . . . . ? N1 U1 Si1 C8 74.5(5) . . . . ? N3 U1 Si1 C8 -32.2(4) . . . . ? C101 U1 Si1 C8 -144.3(4) . . . . y N4 U1 Si1 C8 36.4(4) . . . . ? Si2 U1 Si1 C8 124.0(4) . . . . ? N2 U1 Si1 C9 -59.3(4) . . . . ? N1 U1 Si1 C9 -82.5(5) . . . . ? N3 U1 Si1 C9 170.9(3) . . . . ? C101 U1 Si1 C9 58.7(4) . . . . y N4 U1 Si1 C9 -120.5(3) . . . . ? Si2 U1 Si1 C9 -33.0(3) . . . . ? N1 U1 Si2 N2 -108.7(4) . . . . y N3 U1 Si2 N2 20.0(5) . . . . y C101 U1 Si2 N2 138.0(4) . . . . y N4 U1 Si2 N2 -40.2(4) . . . . y Si1 U1 Si2 N2 -127.9(4) . . . . y N2 U1 Si2 C14 67.9(6) . . . . ? N1 U1 Si2 C14 -40.8(5) . . . . ? N3 U1 Si2 C14 87.9(5) . . . . ? C101 U1 Si2 C14 -154.1(5) . . . . ? N4 U1 Si2 C14 27.7(5) . . . . ? Si1 U1 Si2 C14 -60.0(5) . . . . ? N2 U1 Si2 C13 167.6(5) . . . . ? N1 U1 Si2 C13 59.0(4) . . . . ? N3 U1 Si2 C13 -172.4(4) . . . . ? C101 U1 Si2 C13 -54.4(4) . . . . ? N4 U1 Si2 C13 127.5(4) . . . . ? Si1 U1 Si2 C13 39.7(3) . . . . ? N2 U1 Si2 C15 -87.4(5) . . . . ? N1 U1 Si2 C15 163.9(3) . . . . ? N3 U1 Si2 C15 -67.4(3) . . . . ? C101 U1 Si2 C15 50.6(3) . . . . y N4 U1 Si2 C15 -127.5(3) . . . . ? Si1 U1 Si2 C15 144.7(3) . . . . ? C7 Si1 N1 C2 162.0(6) . . . . ? C8 Si1 N1 C2 43.8(6) . . . . ? C9 Si1 N1 C2 -79.4(6) . . . . ? U1 Si1 N1 C2 166.2(7) . . . . ? C7 Si1 N1 U1 -4.2(5) . . . . ? C8 Si1 N1 U1 -122.4(4) . . . . ? C9 Si1 N1 U1 114.4(4) . . . . ? N2 U1 N1 C2 31.6(5) . . . . ? N3 U1 N1 C2 -86.2(5) . . . . ? C101 U1 N1 C2 150.8(5) . . . . y N4 U1 N1 C2 -27.6(5) . . . . ? Si1 U1 N1 C2 -166.4(7) . . . . ? Si2 U1 N1 C2 56.1(5) . . . . ? N2 U1 N1 Si1 -162.0(3) . . . . y N3 U1 N1 Si1 80.3(4) . . . . y C101 U1 N1 Si1 -42.7(4) . . . . y N4 U1 N1 Si1 138.8(4) . . . . y Si2 U1 N1 Si1 -137.4(3) . . . . y C14 Si2 N2 C4 35.3(7) . . . . ? C13 Si2 N2 C4 151.4(6) . . . . ? C15 Si2 N2 C4 -87.5(6) . . . . ? U1 Si2 N2 C4 163.8(9) . . . . ? C14 Si2 N2 U1 -128.4(5) . . . . ? C13 Si2 N2 U1 -12.4(5) . . . . ? C15 Si2 N2 U1 108.7(4) . . . . ? N1 U1 N2 C4 -86.3(6) . . . . ? N3 U1 N2 C4 31.4(6) . . . . ? C101 U1 N2 C4 151.2(6) . . . . y N4 U1 N2 C4 -27.5(5) . . . . ? Si1 U1 N2 C4 -96.4(5) . . . . ? Si2 U1 N2 C4 -164.1(8) . . . . ? N1 U1 N2 Si2 77.9(4) . . . . ? N3 U1 N2 Si2 -164.5(3) . . . . ? C101 U1 N2 Si2 -44.6(5) . . . . ? N4 U1 N2 Si2 136.7(4) . . . . ? Si1 U1 N2 Si2 67.7(4) . . . . ? C20 Si3 N3 C6 40.2(7) . . . . ? C19 Si3 N3 C6 156.9(6) . . . . ? C21 Si3 N3 C6 -82.3(6) . . . . ? C20 Si3 N3 U1 -124.8(5) . . . . ? C19 Si3 N3 U1 -8.1(5) . . . . ? C21 Si3 N3 U1 112.7(4) . . . . ? N2 U1 N3 C6 -86.5(5) . . . . ? N1 U1 N3 C6 31.2(5) . . . . ? C101 U1 N3 C6 155.6(5) . . . . ? N4 U1 N3 C6 -27.3(5) . . . . ? Si1 U1 N3 C6 56.6(5) . . . . ? Si2 U1 N3 C6 -95.1(5) . . . . ? N2 U1 N3 Si3 78.8(4) . . . . ? N1 U1 N3 Si3 -163.5(3) . . . . ? C101 U1 N3 Si3 -39.2(4) . . . . ? N4 U1 N3 Si3 138.0(4) . . . . ? Si1 U1 N3 Si3 -138.1(3) . . . . ? Si2 U1 N3 Si3 70.1(4) . . . . ? N2 U1 N4 C1 -122.6(5) . . . . ? N1 U1 N4 C1 -2.7(4) . . . . ? N3 U1 N4 C1 117.5(5) . . . . ? C101 U1 N4 C1 -150(5) . . . . y Si1 U1 N4 C1 13.5(4) . . . . ? Si2 U1 N4 C1 -106.0(4) . . . . ? N2 U1 N4 C5 116.7(5) . . . . ? N1 U1 N4 C5 -123.4(5) . . . . ? N3 U1 N4 C5 -3.2(4) . . . . ? C101 U1 N4 C5 89(5) . . . . ? Si1 U1 N4 C5 -107.1(5) . . . . ? Si2 U1 N4 C5 133.3(5) . . . . ? N2 U1 N4 C3 -3.4(5) . . . . ? N1 U1 N4 C3 116.5(5) . . . . ? N3 U1 N4 C3 -123.3(5) . . . . ? C101 U1 N4 C3 -31(5) . . . . y Si1 U1 N4 C3 132.7(5) . . . . ? Si2 U1 N4 C3 13.2(5) . . . . ? C5 N4 C1 C2 148.5(6) . . . . ? C3 N4 C1 C2 -86.2(7) . . . . ? U1 N4 C1 C2 30.0(7) . . . . ? Si1 N1 C2 C1 -111.2(7) . . . . ? U1 N1 C2 C1 55.6(8) . . . . ? N4 C1 C2 N1 -54.4(9) . . . . ? C1 N4 C3 C4 149.7(7) . . . . ? C5 N4 C3 C4 -85.2(8) . . . . ? U1 N4 C3 C4 32.5(8) . . . . ? N4 C3 C4 N2 -57.4(9) . . . . ? Si2 N2 C4 C3 -107.9(7) . . . . ? U1 N2 C4 C3 56.9(8) . . . . ? C1 N4 C5 C6 -87.6(7) . . . . ? C3 N4 C5 C6 147.6(6) . . . . ? U1 N4 C5 C6 30.9(7) . . . . ? Si3 N3 C6 C5 -109.6(6) . . . . ? U1 N3 C6 C5 56.4(7) . . . . ? N4 C5 C6 N3 -55.9(8) . . . . ? N1 Si1 C9 C10 -58.2(7) . . . . ? C7 Si1 C9 C10 58.4(7) . . . . ? C8 Si1 C9 C10 177.6(7) . . . . ? U1 Si1 C9 C10 -22.2(7) . . . . ? N1 Si1 C9 C11 61.1(7) . . . . ? C7 Si1 C9 C11 177.8(6) . . . . ? C8 Si1 C9 C11 -63.0(7) . . . . ? U1 Si1 C9 C11 97.1(6) . . . . ? N1 Si1 C9 C12 -179.6(7) . . . . ? C7 Si1 C9 C12 -63.0(8) . . . . ? C8 Si1 C9 C12 56.2(8) . . . . ? U1 Si1 C9 C12 -143.7(7) . . . . ? N2 Si2 C15 C16 57.7(7) . . . . ? C14 Si2 C15 C16 -66.3(7) . . . . ? C13 Si2 C15 C16 176.5(6) . . . . ? U1 Si2 C15 C16 93.3(6) . . . . ? N2 Si2 C15 C18 -63.5(8) . . . . ? C14 Si2 C15 C18 172.6(8) . . . . ? C13 Si2 C15 C18 55.3(8) . . . . ? U1 Si2 C15 C18 -27.9(8) . . . . ? N2 Si2 C15 C17 178.7(5) . . . . ? C14 Si2 C15 C17 54.8(7) . . . . ? C13 Si2 C15 C17 -62.4(6) . . . . ? U1 Si2 C15 C17 -145.6(5) . . . . ? N3 Si3 C21 C24 -57.3(11) . . . . ? C20 Si3 C21 C24 178.6(11) . . . . ? C19 Si3 C21 C24 61.4(11) . . . . ? N3 Si3 C21 C23 62.8(13) . . . . ? C20 Si3 C21 C23 -61.3(14) . . . . ? C19 Si3 C21 C23 -178.5(13) . . . . ? N3 Si3 C21 C22 -177.9(13) . . . . ? C20 Si3 C21 C22 58.1(14) . . . . ? C19 Si3 C21 C22 -59.1(14) . . . . ? N2 U1 C101 C102 -8.9(17) . . . . y N1 U1 C101 C102 -128.6(16) . . . . y N3 U1 C101 C102 109.6(16) . . . . y N4 U1 C101 C102 18(6) . . . . y Si1 U1 C101 C102 -145.4(16) . . . . ? Si2 U1 C101 C102 -25.9(16) . . . . ? U1 C101 C102 C103 -6(12) . . . . ? C101 C102 C103 C108 -62(11) . . . . y C101 C102 C103 C104 116(11) . . . . y C108 C103 C104 C105 1.1(10) . . . . y C102 C103 C104 C105 -177.4(6) . . . . y C103 C104 C105 C106 0.6(11) . . . . ? C104 C105 C106 C107 -1.8(10) . . . . ? C104 C105 C106 C109 178.5(7) . . . . ? C105 C106 C107 C108 1.2(10) . . . . ? C109 C106 C107 C108 -179.0(7) . . . . ? C106 C107 C108 C103 0.5(11) . . . . ? C104 C103 C108 C107 -1.7(10) . . . . ? C102 C103 C108 C107 176.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 3.191 _refine_diff_density_min -2.965 _refine_diff_density_rms 0.177