Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Noemia Marques' _publ_contact_author_address ; Department of Chemistry ITN Estrada Nacional 10 Sacave m 2686-953 PORTUGAL ; _publ_contact_author_email NMARQUES@ITN.PT _publ_section_title ; Synthesis and Reactivity of Uranium(IV) Amide Complexes Supported by a Triamidotriazacyclononane Ligand ; loop_ _publ_author_name 'Noemia Marques' 'Maria Augusta Antunes' 'Marta Dias' 'Angela Domingos' 'Bernardo Monteiro' 'Isabel Santos' # Attachment 'finalcifutacnX.cif' data_utacnnet _database_code_depnum_ccdc_archive 'CCDC 269724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[U{(SiMe2NPh)3-tacn}(NEt)2]' _chemical_formula_sum 'C34 H55 N7 Si3 U' _chemical_formula_weight 884.15 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 12.8662(17) _cell_length_b 10.7009(10) _cell_length_c 16.9568(19) _cell_angle_alpha 100.262(9) _cell_angle_beta 98.029(10) _cell_angle_gamma 119.404(9) _cell_volume 1929.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.7 _cell_measurement_theta_max 9.9 _exptl_crystal_description irregular-plate _exptl_crystal_colour golden-brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 4.331 _exptl_absorpt_correction_type 'empirical via \y-scan North et al (1968)' _exptl_absorpt_correction_T_min 0.6274 _exptl_absorpt_correction_T_max 0.9995 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were obtained from a concentrated toluene solution of the compound ; _diffrn_ambient_temperature 293(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 CAD4-Enraf-Nonius _diffrn_measurement_method \w/2\qscans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 11.8 _diffrn_reflns_number 7011 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.1816 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6758 _reflns_number_gt 4017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction process-MOLEN(Fair,1990) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997)' _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^)+(0.0308P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6758 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.83000(6) 0.54949(7) 0.73467(4) 0.03187(18) Uani 1 1 d . . . Si1 Si 0.7398(4) 0.4946(5) 0.5354(3) 0.0400(11) Uani 1 1 d . . . Si2 Si 1.1303(4) 0.7372(5) 0.7960(3) 0.0468(13) Uani 1 1 d . . . Si3 Si 0.7317(5) 0.7532(5) 0.8287(3) 0.0490(13) Uani 1 1 d . . . N1 N 0.6773(10) 0.4156(12) 0.6097(7) 0.037(3) Uani 1 1 d . . . N2 N 1.0231(9) 0.5586(12) 0.7363(7) 0.038(3) Uani 1 1 d . . . N3 N 0.7515(11) 0.6110(13) 0.8406(7) 0.046(3) Uani 1 1 d . . . N4 N 1.0473(10) 0.8154(12) 0.7589(8) 0.044(3) Uani 1 1 d . . . N5 N 0.8213(12) 0.8145(13) 0.7576(8) 0.049(4) Uani 1 1 d . . . N6 N 0.8529(11) 0.6760(13) 0.6045(7) 0.047(3) Uani 1 1 d . . . N7 N 0.7727(10) 0.3411(13) 0.7627(8) 0.046(3) Uani 1 1 d . . . C1 C 1.0461(18) 0.9366(17) 0.8162(11) 0.073(6) Uani 1 1 d . . . H1A H 1.0500 0.9200 0.8707 0.088 Uiso 1 1 calc R . . H1B H 1.1209 1.0307 0.8214 0.088 Uiso 1 1 calc R . . C2 C 0.943(2) 0.9528(19) 0.7941(14) 0.107(9) Uani 1 1 d . . . H2A H 0.9588 1.0117 0.7549 0.129 Uiso 1 1 calc R . . H2B H 0.9388 1.0098 0.8436 0.129 Uiso 1 1 calc R . . C3 C 0.7592(16) 0.800(2) 0.6732(11) 0.067(6) Uani 1 1 d . . . H3A H 0.6759 0.7128 0.6576 0.080 Uiso 1 1 calc R . . H3B H 0.7522 0.8867 0.6759 0.080 Uiso 1 1 calc R . . C4 C 0.818(2) 0.786(2) 0.6068(11) 0.094(8) Uani 1 1 d . . . H4A H 0.7610 0.7592 0.5538 0.113 Uiso 1 1 calc R . . H4B H 0.8910 0.8828 0.6138 0.113 Uiso 1 1 calc R . . C5 C 0.9896(14) 0.7455(18) 0.6061(10) 0.070(6) Uani 1 1 d . . . H5A H 1.0065 0.6661 0.5948 0.084 Uiso 1 1 calc R . . H5B H 1.0049 0.7928 0.5617 0.084 Uiso 1 1 calc R . . C6 C 1.0724(15) 0.852(2) 0.6815(12) 0.079(6) Uani 1 1 d . . . H6A H 1.0750 0.9446 0.6829 0.095 Uiso 1 1 calc R . . H6B H 1.1543 0.8716 0.6811 0.095 Uiso 1 1 calc R . . C10 C 0.6330(13) 0.5012(18) 0.4541(9) 0.057(5) Uani 1 1 d . . . H10A H 0.6763 0.5469 0.4157 0.086 Uiso 1 1 calc R . . H10B H 0.6017 0.5588 0.4792 0.086 Uiso 1 1 calc R . . H10C H 0.5654 0.4013 0.4251 0.086 Uiso 1 1 calc R . . C11 C 0.8205(13) 0.4180(17) 0.4819(9) 0.062(5) Uani 1 1 d . . . H11A H 0.8520 0.4705 0.4421 0.093 Uiso 1 1 calc R . . H11B H 0.7637 0.3136 0.4538 0.093 Uiso 1 1 calc R . . H11C H 0.8879 0.4302 0.5219 0.093 Uiso 1 1 calc R . . C12 C 0.5555(12) 0.2957(15) 0.5943(9) 0.031(4) Uani 1 1 d . . . C13 C 0.4895(13) 0.2902(17) 0.6519(9) 0.044(4) Uani 1 1 d . . . H13 H 0.5264 0.3690 0.7005 0.053 Uiso 1 1 calc R . . C14 C 0.3703(13) 0.1723(16) 0.6407(11) 0.057(5) Uani 1 1 d . . . H14 H 0.3288 0.1723 0.6815 0.068 Uiso 1 1 calc R . . C15 C 0.3141(14) 0.0568(18) 0.5702(11) 0.063(5) Uani 1 1 d . . . H15 H 0.2348 -0.0243 0.5626 0.076 Uiso 1 1 calc R . . C16 C 0.3747(15) 0.0616(18) 0.5116(10) 0.073(6) Uani 1 1 d . . . H16 H 0.3353 -0.0162 0.4625 0.088 Uiso 1 1 calc R . . C17 C 0.4931(14) 0.1778(17) 0.5217(10) 0.060(5) Uani 1 1 d . . . H17 H 0.5319 0.1775 0.4794 0.072 Uiso 1 1 calc R . . C20 C 1.2891(12) 0.8305(18) 0.7826(11) 0.079(6) Uani 1 1 d . . . H20A H 1.3378 0.9299 0.8202 0.119 Uiso 1 1 calc R . . H20B H 1.2858 0.8358 0.7265 0.119 Uiso 1 1 calc R . . H20C H 1.3259 0.7743 0.7943 0.119 Uiso 1 1 calc R . . C21 C 1.1450(15) 0.7625(19) 0.9109(10) 0.084(7) Uani 1 1 d . . . H21A H 1.2058 0.8649 0.9411 0.125 Uiso 1 1 calc R . . H21B H 1.1700 0.6986 0.9285 0.125 Uiso 1 1 calc R . . H21C H 1.0666 0.7369 0.9216 0.125 Uiso 1 1 calc R . . C22 C 1.0487(12) 0.4477(15) 0.7098(9) 0.038(4) Uani 1 1 d . . . C23 C 1.1569(13) 0.4575(16) 0.7347(9) 0.046(4) Uani 1 1 d . . . H23 H 1.2189 0.5411 0.7772 0.055 Uiso 1 1 calc R . . C24 C 1.1816(15) 0.3510(18) 0.7011(10) 0.054(5) Uani 1 1 d . . . H24 H 1.2597 0.3662 0.7193 0.064 Uiso 1 1 calc R . . C25 C 1.0929(16) 0.2250(18) 0.6418(11) 0.060(5) Uani 1 1 d . . . H25 H 1.1091 0.1523 0.6197 0.071 Uiso 1 1 calc R . . C26 C 0.9773(15) 0.2042(16) 0.6139(9) 0.047(4) Uani 1 1 d . . . H26 H 0.9147 0.1174 0.5736 0.057 Uiso 1 1 calc R . . C27 C 0.9579(13) 0.3142(15) 0.6472(9) 0.038(4) Uani 1 1 d . . . H27 H 0.8809 0.3009 0.6278 0.046 Uiso 1 1 calc R . . C30 C 0.5693(14) 0.695(2) 0.7833(11) 0.079(6) Uani 1 1 d . . . H30A H 0.5662 0.7808 0.7779 0.119 Uiso 1 1 calc R . . H30B H 0.5193 0.6494 0.8190 0.119 Uiso 1 1 calc R . . H30C H 0.5383 0.6239 0.7295 0.119 Uiso 1 1 calc R . . C31 C 0.7886(18) 0.9042(19) 0.9269(10) 0.095(7) Uani 1 1 d . . . H31A H 0.7755 0.9810 0.9157 0.142 Uiso 1 1 calc R . . H31B H 0.8754 0.9462 0.9496 0.142 Uiso 1 1 calc R . . H31C H 0.7444 0.8634 0.9661 0.142 Uiso 1 1 calc R . . C32 C 0.7092(16) 0.548(2) 0.9074(11) 0.052(5) Uani 1 1 d . . . C33 C 0.5914(18) 0.428(2) 0.8955(13) 0.080(6) Uani 1 1 d . . . H33 H 0.5363 0.3869 0.8431 0.096 Uiso 1 1 calc R . . C34 C 0.552(2) 0.365(3) 0.9584(17) 0.116(10) Uani 1 1 d . . . H34 H 0.4745 0.2800 0.9494 0.140 Uiso 1 1 calc R . . C35 C 0.636(3) 0.438(4) 1.0347(16) 0.126(12) Uani 1 1 d . . . H35 H 0.6105 0.4026 1.0791 0.151 Uiso 1 1 calc R . . C36 C 0.752(3) 0.556(4) 1.0512(17) 0.137(12) Uani 1 1 d . . . H36 H 0.8062 0.5992 1.1040 0.165 Uiso 1 1 calc R . . C37 C 0.7853(19) 0.610(3) 0.9853(12) 0.088(7) Uani 1 1 d . . . H37 H 0.8641 0.6933 0.9947 0.105 Uiso 1 1 calc R . . C38 C 0.6979(14) 0.1784(16) 0.7203(11) 0.066(6) Uani 1 1 d . . . H38A H 0.7532 0.1414 0.7201 0.080 Uiso 1 1 calc R . . H38B H 0.6615 0.1641 0.6628 0.080 Uiso 1 1 calc R . . C39 C 0.5958(17) 0.084(2) 0.7563(13) 0.104(8) Uani 1 1 d . . . H39A H 0.5507 -0.0182 0.7222 0.155 Uiso 1 1 calc R . . H39B H 0.5409 0.1201 0.7580 0.155 Uiso 1 1 calc R . . H39C H 0.6307 0.0892 0.8115 0.155 Uiso 1 1 calc R . . C40 C 0.8366(15) 0.3672(19) 0.8505(9) 0.055(5) Uani 1 1 d . . . H40A H 0.8856 0.4744 0.8767 0.066 Uiso 1 1 calc R . . H40B H 0.7733 0.3245 0.8796 0.066 Uiso 1 1 calc R . . C41 C 0.9171(17) 0.309(2) 0.8642(11) 0.089(7) Uani 1 1 d . . . H41A H 0.9537 0.3364 0.9226 0.133 Uiso 1 1 calc R . . H41B H 0.9811 0.3501 0.8363 0.133 Uiso 1 1 calc R . . H41C H 0.8693 0.2018 0.8424 0.133 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 0.0327(3) 0.0318(3) 0.0319(3) 0.0107(2) 0.0125(2) 0.0162(2) Si1 0.035(3) 0.053(3) 0.027(2) 0.015(2) 0.011(2) 0.018(2) Si2 0.033(3) 0.042(3) 0.053(3) 0.005(2) 0.009(2) 0.015(2) Si3 0.067(3) 0.050(3) 0.040(3) 0.009(2) 0.017(3) 0.039(3) N1 0.038(7) 0.044(8) 0.030(7) 0.019(6) 0.013(6) 0.019(6) N2 0.032(7) 0.033(7) 0.050(8) 0.018(6) 0.019(6) 0.015(6) N3 0.049(8) 0.048(8) 0.030(7) 0.001(6) 0.004(6) 0.022(7) N4 0.036(7) 0.026(7) 0.056(9) 0.012(6) 0.015(7) 0.004(6) N5 0.068(10) 0.041(8) 0.046(9) 0.011(7) 0.017(8) 0.034(8) N6 0.044(8) 0.044(8) 0.052(9) 0.017(7) 0.015(7) 0.022(7) N7 0.042(8) 0.049(8) 0.051(9) 0.013(7) 0.004(7) 0.030(7) C1 0.096(16) 0.036(10) 0.082(14) -0.004(10) 0.002(13) 0.043(11) C2 0.116(19) 0.045(13) 0.13(2) -0.010(13) 0.063(17) 0.026(14) C3 0.083(14) 0.105(15) 0.078(14) 0.076(12) 0.066(12) 0.069(12) C4 0.15(2) 0.078(15) 0.064(14) 0.041(12) -0.007(14) 0.071(15) C5 0.057(12) 0.054(11) 0.063(13) 0.009(10) 0.034(10) 0.001(10) C6 0.049(12) 0.081(14) 0.099(16) 0.040(13) 0.041(12) 0.018(11) C10 0.043(10) 0.083(13) 0.053(11) 0.028(10) 0.014(9) 0.035(10) C11 0.045(10) 0.076(12) 0.057(12) 0.002(10) 0.029(9) 0.028(10) C12 0.029(8) 0.030(8) 0.042(10) 0.018(8) 0.011(7) 0.018(7) C13 0.040(10) 0.055(11) 0.031(9) 0.005(8) 0.005(8) 0.024(9) C14 0.028(9) 0.043(10) 0.079(13) 0.001(10) 0.017(9) 0.009(8) C15 0.029(9) 0.055(11) 0.064(13) 0.013(10) 0.006(9) -0.004(9) C16 0.052(12) 0.052(11) 0.048(12) -0.017(9) 0.004(10) -0.009(9) C17 0.044(10) 0.067(12) 0.044(11) 0.015(9) 0.031(9) 0.006(9) C20 0.024(9) 0.078(13) 0.114(17) 0.022(12) 0.008(10) 0.016(9) C21 0.067(13) 0.077(14) 0.074(14) -0.022(11) -0.009(11) 0.036(11) C22 0.028(8) 0.033(9) 0.050(10) 0.021(8) 0.007(8) 0.013(7) C23 0.029(9) 0.045(10) 0.054(11) 0.004(9) 0.003(8) 0.018(8) C24 0.062(12) 0.054(11) 0.064(12) 0.019(10) 0.023(10) 0.043(10) C25 0.068(12) 0.052(11) 0.080(14) 0.024(10) 0.050(11) 0.038(10) C26 0.053(11) 0.041(10) 0.047(10) 0.017(8) 0.019(9) 0.022(9) C27 0.030(9) 0.038(9) 0.055(11) 0.018(8) 0.012(8) 0.022(8) C30 0.061(13) 0.098(15) 0.107(17) 0.052(13) 0.044(12) 0.050(12) C31 0.139(19) 0.093(15) 0.066(14) -0.001(12) 0.032(13) 0.077(15) C32 0.058(12) 0.097(15) 0.056(12) 0.041(11) 0.037(10) 0.067(12) C33 0.066(14) 0.102(16) 0.093(17) 0.055(14) 0.037(13) 0.045(13) C34 0.13(2) 0.17(3) 0.14(2) 0.13(2) 0.11(2) 0.10(2) C35 0.16(3) 0.24(4) 0.07(2) 0.09(2) 0.06(2) 0.15(3) C36 0.12(2) 0.21(3) 0.08(2) 0.06(2) 0.03(2) 0.08(2) C37 0.076(15) 0.14(2) 0.048(13) 0.033(14) 0.003(12) 0.058(15) C38 0.045(11) 0.032(10) 0.103(16) 0.014(10) -0.002(11) 0.013(9) C39 0.095(16) 0.074(14) 0.15(2) 0.059(15) 0.055(16) 0.032(13) C40 0.063(12) 0.088(13) 0.055(12) 0.052(10) 0.031(10) 0.056(11) C41 0.109(17) 0.134(18) 0.092(16) 0.057(14) 0.050(13) 0.100(16) _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 N7 2.146(12) . ? U1 N1 2.322(11) . ? U1 N3 2.327(12) . ? U1 N2 2.435(11) . ? U1 N4 2.744(11) . ? U1 N6 2.765(13) . ? U1 N5 2.853(12) . ? U1 C40 3.025(15) . ? U1 Si2 3.249(4) . ? U1 Si1 3.261(4) . ? U1 Si3 3.305(4) . ? Si1 N1 1.716(11) . ? Si1 N6 1.788(12) . ? Si1 C11 1.846(14) . ? Si1 C10 1.842(14) . ? Si2 N2 1.707(11) . ? Si2 N4 1.765(13) . ? Si2 C20 1.851(15) . ? Si2 C21 1.889(17) . ? Si3 N3 1.702(13) . ? Si3 N5 1.772(13) . ? Si3 C30 1.856(16) . ? Si3 C31 1.860(15) . ? N1 C12 1.400(15) . ? N2 C22 1.397(16) . ? N3 C32 1.456(18) . ? N4 C6 1.470(19) . ? N4 C1 1.483(17) . ? N5 C2 1.47(2) . ? N5 C3 1.479(18) . ? N6 C4 1.451(19) . ? N6 C5 1.531(17) . ? N7 C38 1.480(16) . ? N7 C40 1.500(17) . ? C1 C2 1.43(2) . ? C3 C4 1.46(2) . ? C5 C6 1.406(19) . ? C12 C13 1.372(18) . ? C12 C17 1.388(18) . ? C13 C14 1.383(18) . ? C14 C15 1.354(18) . ? C15 C16 1.34(2) . ? C16 C17 1.374(19) . ? C22 C23 1.344(18) . ? C22 C27 1.416(17) . ? C23 C24 1.378(19) . ? C24 C25 1.348(19) . ? C25 C26 1.388(19) . ? C26 C27 1.363(18) . ? C32 C37 1.35(2) . ? C32 C33 1.38(2) . ? C33 C34 1.38(2) . ? C34 C35 1.37(3) . ? C35 C36 1.35(3) . ? C36 C37 1.37(3) . ? C38 C39 1.50(2) . ? C40 C41 1.461(19) . ? 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 N7 U1 N1 88.2(4) . . ? N7 U1 N3 88.0(4) . . ? N1 U1 N3 111.0(4) . . ? N7 U1 N2 83.8(4) . . ? N1 U1 N2 115.7(4) . . ? N3 U1 N2 132.2(4) . . ? N7 U1 N4 137.5(4) . . ? N1 U1 N4 124.5(4) . . ? N3 U1 N4 101.8(4) . . ? N2 U1 N4 58.9(4) . . ? N7 U1 N6 142.6(4) . . ? N1 U1 N6 61.1(4) . . ? N3 U1 N6 121.4(4) . . ? N2 U1 N6 90.6(4) . . ? N4 U1 N6 63.7(4) . . ? N7 U1 N5 148.0(4) . . ? N1 U1 N5 96.6(4) . . ? N3 U1 N5 60.7(4) . . ? N2 U1 N5 121.2(4) . . ? N4 U1 N5 62.4(4) . . ? N6 U1 N5 63.0(4) . . ? N7 U1 C40 27.6(4) . . ? N1 U1 C40 115.5(4) . . ? N3 U1 C40 75.1(4) . . ? N2 U1 C40 76.3(4) . . ? N4 U1 C40 115.5(4) . . ? N6 U1 C40 163.5(4) . . ? N5 U1 C40 132.6(4) . . ? N7 U1 Si2 104.8(3) . . ? N1 U1 Si2 137.5(3) . . ? N3 U1 Si2 109.7(3) . . ? N2 U1 Si2 30.9(3) . . ? N4 U1 Si2 32.9(3) . . ? N6 U1 Si2 87.5(3) . . ? N5 U1 Si2 92.8(3) . . ? C40 U1 Si2 86.2(3) . . ? N7 U1 Si1 110.8(3) . . ? N1 U1 Si1 30.3(3) . . ? N3 U1 Si1 129.2(3) . . ? N2 U1 Si1 97.4(3) . . ? N4 U1 Si1 94.7(3) . . ? N6 U1 Si1 33.2(2) . . ? N5 U1 Si1 87.0(3) . . ? C40 U1 Si1 137.6(3) . . ? Si2 U1 Si1 109.90(11) . . ? N7 U1 Si3 115.6(3) . . ? N1 U1 Si3 101.3(3) . . ? N3 U1 Si3 29.1(3) . . ? N2 U1 Si3 139.0(3) . . ? N4 U1 Si3 86.3(3) . . ? N6 U1 Si3 92.5(3) . . ? N5 U1 Si3 32.4(3) . . ? C40 U1 Si3 104.0(3) . . ? Si2 U1 Si3 108.40(12) . . ? Si1 U1 Si3 107.15(12) . . ? N1 Si1 N6 96.5(6) . . ? N1 Si1 C11 116.6(7) . . ? N6 Si1 C11 108.5(6) . . ? N1 Si1 C10 115.7(6) . . ? N6 Si1 C10 112.3(7) . . ? C11 Si1 C10 106.8(7) . . ? N1 Si1 U1 43.0(4) . . ? N6 Si1 U1 58.0(4) . . ? C11 Si1 U1 108.7(6) . . ? C10 Si1 U1 144.4(5) . . ? N2 Si2 N4 95.0(6) . . ? N2 Si2 C20 119.5(7) . . ? N4 Si2 C20 112.1(7) . . ? N2 Si2 C21 113.3(7) . . ? N4 Si2 C21 109.0(7) . . ? C20 Si2 C21 107.2(8) . . ? N2 Si2 U1 47.1(4) . . ? N4 Si2 U1 57.6(4) . . ? C20 Si2 U1 155.6(6) . . ? C21 Si2 U1 97.2(5) . . ? N3 Si3 N5 99.7(6) . . ? N3 Si3 C30 114.7(7) . . ? N5 Si3 C30 110.2(8) . . ? N3 Si3 C31 113.8(7) . . ? N5 Si3 C31 112.2(8) . . ? C30 Si3 C31 106.3(8) . . ? N3 Si3 U1 41.7(4) . . ? N5 Si3 U1 59.6(4) . . ? C30 Si3 U1 116.2(6) . . ? C31 Si3 U1 137.0(6) . . ? C12 N1 Si1 124.3(9) . . ? C12 N1 U1 128.9(9) . . ? Si1 N1 U1 106.7(5) . . ? C22 N2 Si2 125.0(9) . . ? C22 N2 U1 132.3(8) . . ? Si2 N2 U1 101.9(5) . . ? C32 N3 Si3 116.4(10) . . ? C32 N3 U1 134.1(10) . . ? Si3 N3 U1 109.2(6) . . ? C6 N4 C1 111.1(14) . . ? C6 N4 Si2 111.5(11) . . ? C1 N4 Si2 120.3(11) . . ? C6 N4 U1 113.7(9) . . ? C1 N4 U1 109.0(10) . . ? Si2 N4 U1 89.5(5) . . ? C2 N5 C3 114.2(15) . . ? C2 N5 Si3 114.9(11) . . ? C3 N5 Si3 119.2(10) . . ? C2 N5 U1 113.6(11) . . ? C3 N5 U1 103.0(9) . . ? Si3 N5 U1 88.0(5) . . ? C4 N6 C5 110.8(14) . . ? C4 N6 Si1 114.4(11) . . ? C5 N6 Si1 120.0(10) . . ? C4 N6 U1 117.0(10) . . ? C5 N6 U1 103.9(9) . . ? Si1 N6 U1 88.8(5) . . ? C38 N7 C40 109.3(13) . . ? C38 N7 U1 139.5(10) . . ? C40 N7 U1 110.9(9) . . ? C2 C1 N4 117.0(15) . . ? C1 C2 N5 116.8(16) . . ? C4 C3 N5 117.1(14) . . ? N6 C4 C3 114.0(15) . . ? C6 C5 N6 114.4(13) . . ? C5 C6 N4 117.6(14) . . ? C13 C12 C17 115.7(13) . . ? C13 C12 N1 120.5(13) . . ? C17 C12 N1 123.9(13) . . ? C12 C13 C14 122.7(14) . . ? C15 C14 C13 119.8(15) . . ? C16 C15 C14 118.8(15) . . ? C15 C16 C17 122.2(15) . . ? C16 C17 C12 120.8(14) . . ? C23 C22 N2 126.0(13) . . ? C23 C22 C27 114.3(14) . . ? N2 C22 C27 119.5(13) . . ? C22 C23 C24 123.9(15) . . ? C25 C24 C23 120.1(16) . . ? C24 C25 C26 119.7(15) . . ? C27 C26 C25 118.3(15) . . ? C26 C27 C22 123.6(14) . . ? C37 C32 C33 117.4(19) . . ? C37 C32 N3 120.0(18) . . ? C33 C32 N3 122.5(17) . . ? C34 C33 C32 123(2) . . ? C35 C34 C33 115(3) . . ? C36 C35 C34 126(3) . . ? C35 C36 C37 116(3) . . ? C32 C37 C36 123(2) . . ? N7 C38 C39 116.6(15) . . ? C41 C40 N7 118.4(14) . . ? C41 C40 U1 129.1(11) . . ? N7 C40 U1 41.5(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.864 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.235 # ===END data_U(TACN)SPY _database_code_depnum_ccdc_archive 'CCDC 269725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 N7 S Si3 U' _chemical_formula_weight 922.17 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' S S 0.1246 0.1234 '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' 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 P21/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 14.213(3) _cell_length_b 17.6693(17) _cell_length_c 15.321(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.273(15) _cell_angle_gamma 90.00 _cell_volume 3837.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 4.413 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3619 _exptl_absorpt_correction_T_max 0.5258 _exptl_absorpt_process_details 'psi-scan (North,1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 cad4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 6975 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6689 _reflns_number_gt 4637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0545P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6689 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.93490(2) 0.223077(17) 0.25921(2) 0.02622(11) Uani 1 1 d . . . S1 S 1.10013(17) 0.26713(14) 0.36758(15) 0.0435(6) Uani 1 1 d . . . N1 N 1.0199(5) 0.1114(4) 0.2470(4) 0.0316(17) Uani 1 1 d . . . N2 N 0.8576(5) 0.2163(4) 0.1197(4) 0.0338(16) Uani 1 1 d . . . N3 N 0.8949(5) 0.3488(4) 0.2746(4) 0.0361(18) Uani 1 1 d . . . N4 N 0.7598(5) 0.1758(4) 0.2520(4) 0.0292(16) Uani 1 1 d . . . N5 N 0.8428(5) 0.2595(4) 0.4005(4) 0.0313(17) Uani 1 1 d . . . N6 N 0.9099(5) 0.1095(4) 0.3804(4) 0.0325(17) Uani 1 1 d . . . N7 N 1.0723(5) 0.2917(4) 0.1981(5) 0.0381(18) Uani 1 1 d . . . Si1 Si 1.00620(18) 0.06112(13) 0.33976(16) 0.0342(6) Uani 1 1 d . . . Si2 Si 0.74307(17) 0.19797(13) 0.13765(16) 0.0327(6) Uani 1 1 d . . . Si3 Si 0.85429(18) 0.35776(13) 0.37659(16) 0.0328(6) Uani 1 1 d . . . C1 C 0.6986(6) 0.2141(5) 0.3108(6) 0.036(2) Uani 1 1 d . . . H1A H 0.6435 0.1826 0.3167 0.043 Uiso 1 1 calc R . . H1B H 0.6770 0.2611 0.2835 0.043 Uiso 1 1 calc R . . C2 C 0.7438(6) 0.2322(5) 0.4035(6) 0.039(2) Uani 1 1 d . . . H2A H 0.7067 0.2706 0.4303 0.047 Uiso 1 1 calc R . . H2B H 0.7433 0.1870 0.4394 0.047 Uiso 1 1 calc R . . C3 C 0.9023(7) 0.2272(5) 0.4754(5) 0.041(2) Uani 1 1 d . . . H3A H 0.8736 0.2391 0.5293 0.049 Uiso 1 1 calc R . . H3B H 0.9638 0.2512 0.4781 0.049 Uiso 1 1 calc R . . C4 C 0.9152(7) 0.1412(5) 0.4696(5) 0.040(2) Uani 1 1 d . . . H4A H 0.9761 0.1282 0.4985 0.048 Uiso 1 1 calc R . . H4B H 0.8673 0.1170 0.5019 0.048 Uiso 1 1 calc R . . C5 C 0.8148(7) 0.0721(5) 0.3576(6) 0.044(2) Uani 1 1 d . . . H5A H 0.8227 0.0176 0.3598 0.053 Uiso 1 1 calc R . . H5B H 0.7720 0.0860 0.4013 0.053 Uiso 1 1 calc R . . C6 C 0.7711(6) 0.0940(5) 0.2682(6) 0.036(2) Uani 1 1 d . . . H6A H 0.8098 0.0733 0.2244 0.043 Uiso 1 1 calc R . . H6B H 0.7095 0.0704 0.2599 0.043 Uiso 1 1 calc R . . C10 C 1.0934(7) 0.0864(5) 0.1964(6) 0.037(2) Uani 1 1 d . . . C11 C 1.0787(8) 0.0264(5) 0.1377(6) 0.050(3) Uani 1 1 d . . . H11 H 1.0195 0.0039 0.1295 0.060 Uiso 1 1 calc R . . C12 C 1.1533(9) 0.0003(6) 0.0913(7) 0.063(3) Uani 1 1 d . . . H12 H 1.1430 -0.0389 0.0511 0.075 Uiso 1 1 calc R . . C13 C 1.2410(8) 0.0314(7) 0.1043(7) 0.059(3) Uani 1 1 d . . . H13 H 1.2910 0.0122 0.0753 0.071 Uiso 1 1 calc R . . C14 C 1.2542(8) 0.0908(7) 0.1600(8) 0.065(3) Uani 1 1 d . . . H14 H 1.3131 0.1137 0.1673 0.078 Uiso 1 1 calc R . . C15 C 1.1823(7) 0.1172(6) 0.2052(7) 0.049(3) Uani 1 1 d . . . H15 H 1.1937 0.1575 0.2435 0.059 Uiso 1 1 calc R . . C20 C 0.8886(6) 0.2202(5) 0.0355(5) 0.036(2) Uani 1 1 d . . . C21 C 0.8475(7) 0.2696(6) -0.0294(6) 0.053(3) Uani 1 1 d . . . H21 H 0.7982 0.3012 -0.0159 0.063 Uiso 1 1 calc R . . C22 C 0.8785(9) 0.2716(8) -0.1106(8) 0.079(4) Uani 1 1 d . . . H22 H 0.8476 0.3031 -0.1521 0.095 Uiso 1 1 calc R . . C23 C 0.9523(10) 0.2304(9) -0.1345(7) 0.084(5) Uani 1 1 d . . . H23 H 0.9739 0.2337 -0.1902 0.101 Uiso 1 1 calc R . . C24 C 0.9941(8) 0.1825(7) -0.0706(8) 0.068(3) Uani 1 1 d . . . H24 H 1.0439 0.1517 -0.0847 0.082 Uiso 1 1 calc R . . C25 C 0.9648(6) 0.1793(6) 0.0115(6) 0.045(2) Uani 1 1 d . . . H25 H 0.9972 0.1485 0.0528 0.054 Uiso 1 1 calc R . . C30 C 0.9152(6) 0.4116(4) 0.2226(6) 0.031(2) Uani 1 1 d . . . C31 C 0.8763(7) 0.4183(5) 0.1377(6) 0.046(2) Uani 1 1 d . . . H31 H 0.8345 0.3813 0.1156 0.055 Uiso 1 1 calc R . . C32 C 0.8971(8) 0.4778(6) 0.0849(7) 0.061(3) Uani 1 1 d . . . H32 H 0.8690 0.4804 0.0282 0.073 Uiso 1 1 calc R . . C33 C 0.9585(8) 0.5333(6) 0.1144(8) 0.062(3) Uani 1 1 d . . . H33 H 0.9755 0.5722 0.0778 0.074 Uiso 1 1 calc R . . C34 C 0.9937(8) 0.5293(6) 0.1992(8) 0.062(3) Uani 1 1 d . . . H34 H 1.0315 0.5685 0.2222 0.074 Uiso 1 1 calc R . . C35 C 0.9753(7) 0.4697(5) 0.2513(7) 0.050(3) Uani 1 1 d . . . H35 H 1.0038 0.4678 0.3079 0.060 Uiso 1 1 calc R . . C41 C 0.6578(7) 0.2766(5) 0.1215(6) 0.052(3) Uani 1 1 d . . . H41A H 0.5961 0.2593 0.1335 0.077 Uiso 1 1 calc R . . H41B H 0.6567 0.2941 0.0621 0.077 Uiso 1 1 calc R . . H41C H 0.6764 0.3174 0.1605 0.077 Uiso 1 1 calc R . . C42 C 0.6931(7) 0.1172(5) 0.0732(6) 0.054(3) Uani 1 1 d . . . H42A H 0.6287 0.1095 0.0861 0.081 Uiso 1 1 calc R . . H42B H 0.7291 0.0724 0.0881 0.081 Uiso 1 1 calc R . . H42C H 0.6956 0.1277 0.0119 0.081 Uiso 1 1 calc R . . C51 C 0.7380(7) 0.4070(5) 0.3715(6) 0.043(2) Uani 1 1 d . . . H51A H 0.7170 0.4112 0.4294 0.065 Uiso 1 1 calc R . . H51B H 0.6928 0.3785 0.3353 0.065 Uiso 1 1 calc R . . H51C H 0.7444 0.4566 0.3471 0.065 Uiso 1 1 calc R . . C52 C 0.9334(7) 0.4049(5) 0.4638(6) 0.046(3) Uani 1 1 d . . . H52A H 0.9024 0.4066 0.5173 0.069 Uiso 1 1 calc R . . H52B H 0.9473 0.4555 0.4458 0.069 Uiso 1 1 calc R . . H52C H 0.9911 0.3768 0.4729 0.069 Uiso 1 1 calc R . . C61 C 1.1118(6) 0.0626(5) 0.4199(6) 0.044(2) Uani 1 1 d . . . H61A H 1.0993 0.0330 0.4703 0.066 Uiso 1 1 calc R . . H61B H 1.1254 0.1138 0.4376 0.066 Uiso 1 1 calc R . . H61C H 1.1650 0.0417 0.3932 0.066 Uiso 1 1 calc R . . C62 C 0.9793(7) -0.0407(5) 0.3178(6) 0.051(3) Uani 1 1 d . . . H62A H 0.9727 -0.0665 0.3721 0.076 Uiso 1 1 calc R . . H62B H 1.0299 -0.0632 0.2886 0.076 Uiso 1 1 calc R . . H62C H 0.9217 -0.0448 0.2813 0.076 Uiso 1 1 calc R . . C70 C 1.0911(7) 0.3258(5) 0.1228(7) 0.047(3) Uani 1 1 d . . . H70 H 1.0511 0.3166 0.0730 0.056 Uiso 1 1 calc R . . C71 C 1.1658(8) 0.3734(6) 0.1157(8) 0.066(3) Uani 1 1 d . . . H71 H 1.1768 0.3956 0.0624 0.080 Uiso 1 1 calc R . . C72 C 1.2242(8) 0.3878(6) 0.1889(9) 0.071(4) Uani 1 1 d . . . H72 H 1.2753 0.4202 0.1853 0.085 Uiso 1 1 calc R . . C73 C 1.2084(7) 0.3554(5) 0.2663(8) 0.052(3) Uani 1 1 d . . . H73 H 1.2499 0.3638 0.3153 0.063 Uiso 1 1 calc R . . C74 C 1.1288(6) 0.3090(5) 0.2723(6) 0.038(2) 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 U1 0.02558(17) 0.02594(16) 0.02573(16) 0.00196(16) -0.00761(11) -0.00040(17) S1 0.0389(13) 0.0501(15) 0.0388(13) -0.0029(12) -0.0149(10) -0.0041(12) N1 0.028(4) 0.034(4) 0.031(4) -0.003(3) -0.008(3) -0.003(3) N2 0.032(4) 0.046(4) 0.023(4) 0.004(3) -0.006(3) 0.000(4) N3 0.043(5) 0.028(4) 0.035(4) 0.004(3) -0.008(4) -0.003(3) N4 0.027(4) 0.028(4) 0.030(4) 0.002(3) -0.010(3) 0.003(3) N5 0.031(4) 0.025(4) 0.036(4) 0.004(3) -0.007(3) 0.002(3) N6 0.037(4) 0.029(4) 0.029(4) 0.007(3) -0.008(3) 0.005(3) N7 0.035(4) 0.042(5) 0.038(4) 0.003(4) 0.002(3) -0.005(3) Si1 0.0365(15) 0.0307(13) 0.0335(14) 0.0033(11) -0.0108(11) 0.0039(11) Si2 0.0299(14) 0.0343(13) 0.0321(14) 0.0006(10) -0.0104(11) 0.0003(10) Si3 0.0349(14) 0.0304(13) 0.0318(14) -0.0022(10) -0.0057(11) -0.0006(11) C1 0.026(5) 0.037(5) 0.043(5) -0.001(4) -0.005(4) 0.001(4) C2 0.041(5) 0.040(5) 0.036(5) 0.007(4) 0.002(4) 0.004(5) C3 0.047(6) 0.048(5) 0.025(4) 0.010(5) -0.009(4) 0.004(5) C4 0.045(6) 0.049(6) 0.025(5) 0.014(4) -0.006(4) 0.010(5) C5 0.039(6) 0.038(5) 0.055(7) 0.014(5) -0.005(5) -0.002(4) C6 0.029(5) 0.041(5) 0.036(5) 0.002(4) -0.004(4) -0.001(4) C10 0.047(6) 0.038(5) 0.026(5) 0.006(4) 0.000(4) 0.009(5) C11 0.054(7) 0.046(6) 0.050(6) -0.004(5) 0.006(5) -0.003(5) C12 0.094(10) 0.043(6) 0.052(7) -0.013(5) 0.016(7) 0.010(6) C13 0.039(7) 0.073(8) 0.068(8) 0.009(6) 0.023(6) 0.024(6) C14 0.036(6) 0.075(8) 0.085(9) -0.009(7) 0.009(6) 0.007(6) C15 0.043(6) 0.053(6) 0.052(6) -0.009(5) -0.003(5) 0.002(5) C20 0.027(5) 0.050(5) 0.031(5) -0.001(5) -0.010(4) -0.010(5) C21 0.047(6) 0.078(7) 0.032(5) 0.013(6) -0.007(4) 0.005(6) C22 0.063(8) 0.128(12) 0.045(7) 0.025(8) -0.007(6) -0.016(9) C23 0.072(9) 0.146(13) 0.036(7) -0.014(8) 0.021(6) -0.050(10) C24 0.049(7) 0.098(9) 0.058(8) -0.021(7) 0.006(6) 0.002(7) C25 0.029(5) 0.063(7) 0.043(6) -0.003(5) -0.005(4) -0.004(5) C30 0.032(5) 0.023(4) 0.039(5) 0.003(4) 0.009(4) 0.005(4) C31 0.055(7) 0.045(6) 0.039(6) 0.004(5) 0.004(5) 0.003(5) C32 0.081(9) 0.057(7) 0.045(7) 0.025(5) 0.004(6) 0.010(6) C33 0.067(8) 0.044(6) 0.077(9) 0.020(6) 0.026(7) 0.001(6) C34 0.067(8) 0.041(6) 0.077(9) 0.011(6) 0.002(7) -0.017(6) C35 0.048(6) 0.045(6) 0.056(7) 0.010(5) -0.008(5) -0.016(5) C41 0.048(6) 0.056(6) 0.048(6) 0.022(6) -0.010(5) 0.005(6) C42 0.061(7) 0.049(6) 0.047(6) -0.002(5) -0.025(5) -0.010(5) C51 0.050(6) 0.036(5) 0.043(6) -0.002(4) -0.010(5) 0.011(5) C52 0.042(6) 0.039(5) 0.056(7) -0.010(5) -0.008(5) -0.005(5) C61 0.041(6) 0.048(6) 0.040(6) 0.004(4) -0.017(5) 0.006(5) C62 0.060(7) 0.040(6) 0.050(6) 0.002(5) -0.007(5) -0.006(5) C70 0.042(6) 0.040(6) 0.061(7) 0.004(5) 0.012(5) 0.001(5) C71 0.066(8) 0.057(7) 0.079(9) 0.014(6) 0.023(7) -0.010(6) C72 0.045(7) 0.057(7) 0.112(11) 0.008(7) 0.015(7) -0.026(6) C73 0.030(6) 0.051(6) 0.074(8) 0.006(6) -0.009(5) -0.020(5) C74 0.027(5) 0.034(5) 0.050(6) -0.006(4) -0.005(4) 0.003(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 N3 2.309(7) . ? U1 N1 2.328(7) . ? U1 N2 2.332(6) . ? U1 N7 2.536(7) . ? U1 N4 2.619(7) . ? U1 N5 2.689(7) . ? U1 N6 2.775(6) . ? U1 S1 2.880(2) . ? U1 Si2 3.216(2) . ? U1 Si3 3.243(2) . ? U1 Si1 3.249(2) . ? S1 C74 1.713(10) . ? N1 C10 1.417(11) . ? N1 Si1 1.699(7) . ? N2 C20 1.396(10) . ? N2 Si2 1.702(7) . ? N3 C30 1.409(10) . ? N3 Si3 1.713(8) . ? N4 C1 1.464(10) . ? N4 C6 1.472(10) . ? N4 Si2 1.794(7) . ? N5 C3 1.488(10) . ? N5 C2 1.491(11) . ? N5 Si3 1.785(6) . ? N6 C4 1.474(10) . ? N6 C5 1.521(11) . ? N6 Si1 1.766(7) . ? N7 C70 1.347(11) . ? N7 C74 1.376(11) . ? Si1 C62 1.864(9) . ? Si1 C61 1.867(8) . ? Si2 C42 1.847(9) . ? Si2 C41 1.849(9) . ? Si3 C51 1.864(9) . ? Si3 C52 1.876(9) . ? C1 C2 1.548(11) . ? C3 C4 1.534(11) . ? C5 C6 1.512(11) . ? C10 C15 1.373(13) . ? C10 C11 1.396(12) . ? C11 C12 1.399(14) . ? C12 C13 1.363(15) . ? C13 C14 1.357(15) . ? C14 C15 1.360(14) . ? C20 C25 1.376(12) . ? C20 C21 1.415(12) . ? C21 C22 1.351(15) . ? C22 C23 1.350(18) . ? C23 C24 1.393(17) . ? C24 C25 1.355(14) . ? C30 C31 1.380(12) . ? C30 C35 1.384(12) . ? C31 C32 1.372(13) . ? C32 C33 1.366(15) . ? C33 C34 1.359(15) . ? C34 C35 1.360(13) . ? C70 C71 1.366(13) . ? C71 C72 1.368(16) . ? C72 C73 1.350(14) . ? C73 C74 1.407(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U1 N1 163.1(2) . . ? N3 U1 N2 92.3(2) . . ? N1 U1 N2 95.4(2) . . ? N3 U1 N7 77.3(2) . . ? N1 U1 N7 87.5(2) . . ? N2 U1 N7 90.6(2) . . ? N3 U1 N4 94.0(2) . . ? N1 U1 N4 102.9(2) . . ? N2 U1 N4 64.1(2) . . ? N7 U1 N4 153.1(2) . . ? N3 U1 N5 63.2(2) . . ? N1 U1 N5 123.6(2) . . ? N2 U1 N5 121.7(2) . . ? N7 U1 N5 128.1(2) . . ? N4 U1 N5 65.9(2) . . ? N3 U1 N6 125.6(2) . . ? N1 U1 N6 62.2(2) . . ? N2 U1 N6 120.0(2) . . ? N7 U1 N6 137.1(2) . . ? N4 U1 N6 68.2(2) . . ? N5 U1 N6 62.62(19) . . ? N3 U1 S1 82.98(18) . . ? N1 U1 S1 82.53(17) . . ? N2 U1 S1 148.25(18) . . ? N7 U1 S1 57.74(18) . . ? N4 U1 S1 147.32(15) . . ? N5 U1 S1 84.06(15) . . ? N6 U1 S1 87.10(15) . . ? N3 U1 Si2 89.26(17) . . ? N1 U1 Si2 105.00(16) . . ? N2 U1 Si2 30.80(17) . . ? N7 U1 Si2 119.69(17) . . ? N4 U1 Si2 33.88(15) . . ? N5 U1 Si2 93.24(15) . . ? N6 U1 Si2 98.18(15) . . ? S1 U1 Si2 172.19(6) . . ? N3 U1 Si3 30.43(18) . . ? N1 U1 Si3 150.85(17) . . ? N2 U1 Si3 112.59(18) . . ? N7 U1 Si3 99.65(17) . . ? N4 U1 Si3 83.32(15) . . ? N5 U1 Si3 33.39(14) . . ? N6 U1 Si3 95.26(15) . . ? S1 U1 Si3 77.80(7) . . ? Si2 U1 Si3 95.91(6) . . ? N3 U1 Si1 151.75(17) . . ? N1 U1 Si1 30.11(18) . . ? N2 U1 Si1 114.52(18) . . ? N7 U1 Si1 109.52(17) . . ? N4 U1 Si1 90.20(14) . . ? N5 U1 Si1 93.53(14) . . ? N6 U1 Si1 32.92(15) . . ? S1 U1 Si1 78.53(7) . . ? Si2 U1 Si1 109.00(6) . . ? Si3 U1 Si1 123.29(6) . . ? C74 S1 U1 82.0(3) . . ? C10 N1 Si1 115.4(6) . . ? C10 N1 U1 135.8(5) . . ? Si1 N1 U1 106.5(3) . . ? C20 N2 Si2 122.0(5) . . ? C20 N2 U1 133.2(5) . . ? Si2 N2 U1 104.7(3) . . ? C30 N3 Si3 122.7(6) . . ? C30 N3 U1 129.6(6) . . ? Si3 N3 U1 106.5(3) . . ? C1 N4 C6 114.3(7) . . ? C1 N4 Si2 117.2(5) . . ? C6 N4 Si2 112.5(5) . . ? C1 N4 U1 115.7(5) . . ? C6 N4 U1 102.4(5) . . ? Si2 N4 U1 91.6(3) . . ? C3 N5 C2 109.6(7) . . ? C3 N5 Si3 118.4(6) . . ? C2 N5 Si3 115.0(5) . . ? C3 N5 U1 104.3(5) . . ? C2 N5 U1 117.7(5) . . ? Si3 N5 U1 90.6(3) . . ? C4 N6 C5 111.2(7) . . ? C4 N6 Si1 121.6(6) . . ? C5 N6 Si1 114.1(6) . . ? C4 N6 U1 110.2(5) . . ? C5 N6 U1 108.4(5) . . ? Si1 N6 U1 88.4(3) . . ? C70 N7 C74 117.9(8) . . ? C70 N7 U1 137.5(6) . . ? C74 N7 U1 102.7(6) . . ? N1 Si1 N6 100.5(3) . . ? N1 Si1 C62 112.8(4) . . ? N6 Si1 C62 112.1(4) . . ? N1 Si1 C61 114.0(4) . . ? N6 Si1 C61 111.6(4) . . ? C62 Si1 C61 106.0(4) . . ? N1 Si1 U1 43.4(2) . . ? N6 Si1 U1 58.7(2) . . ? C62 Si1 U1 136.7(3) . . ? C61 Si1 U1 116.8(3) . . ? N2 Si2 N4 98.0(3) . . ? N2 Si2 C42 113.2(4) . . ? N4 Si2 C42 111.8(4) . . ? N2 Si2 C41 117.4(4) . . ? N4 Si2 C41 109.4(4) . . ? C42 Si2 C41 106.7(5) . . ? N2 Si2 U1 44.6(2) . . ? N4 Si2 U1 54.5(2) . . ? C42 Si2 U1 133.8(3) . . ? C41 Si2 U1 119.5(3) . . ? N3 Si3 N5 98.0(3) . . ? N3 Si3 C51 111.3(4) . . ? N5 Si3 C51 111.6(4) . . ? N3 Si3 C52 117.8(4) . . ? N5 Si3 C52 110.2(4) . . ? C51 Si3 C52 107.8(4) . . ? N3 Si3 U1 43.1(2) . . ? N5 Si3 U1 56.0(2) . . ? C51 Si3 U1 131.9(3) . . ? C52 Si3 U1 120.2(3) . . ? N4 C1 C2 115.7(7) . . ? N5 C2 C1 111.5(7) . . ? N5 C3 C4 113.5(7) . . ? N6 C4 C3 115.7(6) . . ? C6 C5 N6 113.3(7) . . ? N4 C6 C5 115.8(7) . . ? C15 C10 C11 117.2(9) . . ? C15 C10 N1 122.2(8) . . ? C11 C10 N1 120.5(9) . . ? C10 C11 C12 119.7(10) . . ? C13 C12 C11 120.8(10) . . ? C14 C13 C12 119.1(10) . . ? C13 C14 C15 120.8(11) . . ? C14 C15 C10 122.4(10) . . ? C25 C20 N2 122.0(8) . . ? C25 C20 C21 115.4(9) . . ? N2 C20 C21 122.5(8) . . ? C22 C21 C20 121.1(11) . . ? C23 C22 C21 123.3(12) . . ? C22 C23 C24 115.9(11) . . ? C25 C24 C23 122.2(11) . . ? C24 C25 C20 122.0(10) . . ? C31 C30 C35 115.5(8) . . ? C31 C30 N3 121.0(8) . . ? C35 C30 N3 123.5(8) . . ? C32 C31 C30 122.1(10) . . ? C33 C32 C31 121.0(10) . . ? C34 C33 C32 117.3(10) . . ? C33 C34 C35 121.9(10) . . ? C34 C35 C30 121.9(10) . . ? N7 C70 C71 123.2(10) . . ? C70 C71 C72 118.5(11) . . ? C73 C72 C71 120.7(10) . . ? C72 C73 C74 119.4(10) . . ? N7 C74 C73 120.0(9) . . ? N7 C74 S1 116.5(7) . . ? C73 C74 S1 123.4(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.275 _refine_diff_density_min -2.199 _refine_diff_density_rms 0.161 # ===END data_Utacn[(NCMe)2CCN] _database_code_depnum_ccdc_archive 'CCDC 269726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H53 N9 Si3 U' _chemical_formula_weight 934.17 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 11.1504(15) _cell_length_b 11.274(3) _cell_length_c 19.834(4) _cell_angle_alpha 77.114(19) _cell_angle_beta 83.551(13) _cell_angle_gamma 62.636(15) _cell_volume 2158.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 11 _exptl_crystal_description needle _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 3.878 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 7742 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.3187 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7509 _reflns_number_gt 3381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL(Keller, 1989),ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0762P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7509 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2408 _refine_ls_R_factor_gt 0.1035 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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 U U 0.86922(8) 0.21684(9) 0.25612(5) 0.0322(3) Uani 1 1 d . . . N1 N 1.0008(15) 0.0167(15) 0.3281(9) 0.042(5) Uani 1 1 d . . . N3 N 0.7474(16) 0.3630(18) 0.1577(9) 0.050(5) Uani 1 1 d . . . N2 N 0.7190(15) 0.3349(17) 0.3314(8) 0.042(5) Uani 1 1 d . . . N5 N 0.9852(16) 0.3469(16) 0.1596(9) 0.046(5) Uani 1 1 d . . . N4 N 0.9162(16) 0.4024(16) 0.3012(9) 0.041(4) Uani 1 1 d . . . N6 N 1.1374(14) 0.1449(16) 0.2764(10) 0.046(5) Uani 1 1 d . . . N7 N 0.7109(16) 0.1192(15) 0.2781(9) 0.041(4) Uani 1 1 d . . . H7 H 0.6617 0.1455 0.3136 0.050 Uiso 1 1 calc R . . N8 N 0.9182(18) 0.0510(19) 0.1817(10) 0.057(5) Uani 1 1 d . . . H8 H 0.9878 0.0425 0.1558 0.069 Uiso 1 1 calc R . . N9 N 0.654(3) -0.166(2) 0.1580(14) 0.109(10) Uani 1 1 d . . . Si1 Si 1.1660(6) -0.0271(6) 0.3105(4) 0.0479(17) Uani 1 1 d . . . Si2 Si 0.7771(6) 0.4316(6) 0.3603(4) 0.0490(18) Uani 1 1 d . . . Si3 Si 0.8576(6) 0.3896(6) 0.1006(3) 0.0479(17) Uani 1 1 d . . . C1 C 0.895(3) 0.509(3) 0.2385(16) 0.086(10) Uani 1 1 d . . . H1A H 0.8010 0.5483 0.2251 0.104 Uiso 1 1 calc R . . H1B H 0.9083 0.5808 0.2506 0.104 Uiso 1 1 calc R . . C2 C 0.979(2) 0.468(2) 0.1787(13) 0.063(7) Uani 1 1 d . . . H2A H 1.0696 0.4508 0.1877 0.075 Uiso 1 1 calc R . . H2B H 0.9451 0.5431 0.1395 0.075 Uiso 1 1 calc R . . C3 C 1.134(2) 0.243(3) 0.1552(15) 0.095(11) Uani 1 1 d . . . H3A H 1.1371 0.1760 0.1308 0.114 Uiso 1 1 calc R . . H3B H 1.1805 0.2906 0.1260 0.114 Uiso 1 1 calc R . . C4 C 1.211(2) 0.172(3) 0.2134(13) 0.078(9) Uani 1 1 d . . . H4A H 1.2558 0.2224 0.2224 0.094 Uiso 1 1 calc R . . H4B H 1.2798 0.0855 0.2038 0.094 Uiso 1 1 calc R . . C5 C 1.132(3) 0.211(2) 0.3352(13) 0.068(8) Uani 1 1 d . . . H5A H 1.1028 0.1637 0.3759 0.082 Uiso 1 1 calc R . . H5B H 1.2234 0.1915 0.3435 0.082 Uiso 1 1 calc R . . C6 C 1.052(2) 0.350(3) 0.3328(13) 0.065(8) Uani 1 1 d . . . H6A H 1.0994 0.3990 0.3061 0.078 Uiso 1 1 calc R . . H6B H 1.0392 0.3675 0.3794 0.078 Uiso 1 1 calc R . . C10 C 0.9580(19) -0.080(2) 0.3660(11) 0.038(5) Uani 1 1 d . . . C11 C 0.994(3) -0.207(3) 0.3509(14) 0.082(8) Uani 1 1 d . . . H11 H 1.0531 -0.2354 0.3144 0.099 Uiso 1 1 calc R . . C12 C 0.939(3) -0.295(3) 0.3913(18) 0.094(10) Uani 1 1 d . . . H12 H 0.9676 -0.3796 0.3797 0.113 Uiso 1 1 calc R . . C13 C 0.855(3) -0.267(3) 0.4415(15) 0.086(10) Uani 1 1 d . . . H13 H 0.8195 -0.3255 0.4638 0.103 Uiso 1 1 calc R . . C14 C 0.821(2) -0.147(3) 0.4607(12) 0.063(7) Uani 1 1 d . . . H14 H 0.7621 -0.1244 0.4981 0.075 Uiso 1 1 calc R . . C15 C 0.873(2) -0.053(2) 0.4243(11) 0.055(6) Uani 1 1 d . . . H15 H 0.8495 0.0272 0.4399 0.067 Uiso 1 1 calc R . . C20 C 0.588(2) 0.350(2) 0.3567(10) 0.041(5) Uani 1 1 d . . . C21 C 0.567(2) 0.290(3) 0.4253(13) 0.073(8) Uani 1 1 d . . . H21 H 0.6419 0.2352 0.4533 0.088 Uiso 1 1 calc R . . C22 C 0.440(2) 0.307(3) 0.4528(13) 0.085(10) Uani 1 1 d . . . H22 H 0.4276 0.2734 0.4989 0.102 Uiso 1 1 calc R . . C23 C 0.333(3) 0.379(3) 0.4072(16) 0.078(8) Uani 1 1 d . . . H23 H 0.2481 0.3841 0.4213 0.094 Uiso 1 1 calc R . . C24 C 0.349(3) 0.441(3) 0.3421(15) 0.096(11) Uani 1 1 d . . . H24 H 0.2753 0.4960 0.3136 0.116 Uiso 1 1 calc R . . C25 C 0.474(2) 0.423(3) 0.3191(12) 0.067(8) Uani 1 1 d . . . H25 H 0.4826 0.4646 0.2739 0.080 Uiso 1 1 calc R . . C30 C 0.609(2) 0.416(3) 0.1439(12) 0.063(8) Uani 1 1 d . . . C31 C 0.517(2) 0.556(2) 0.1424(12) 0.062(8) Uani 1 1 d . . . H31 H 0.5475 0.6168 0.1498 0.074 Uiso 1 1 calc R . . C32 C 0.382(3) 0.600(3) 0.1295(15) 0.099(11) Uani 1 1 d . . . H32 H 0.3227 0.6921 0.1270 0.119 Uiso 1 1 calc R . . C33 C 0.331(2) 0.515(3) 0.1204(17) 0.097(12) Uani 1 1 d . . . H33 H 0.2386 0.5481 0.1145 0.117 Uiso 1 1 calc R . . C34 C 0.417(3) 0.382(3) 0.1200(14) 0.087(10) Uani 1 1 d . . . H34 H 0.3836 0.3257 0.1104 0.105 Uiso 1 1 calc R . . C35 C 0.561(2) 0.326(3) 0.1346(13) 0.073(8) Uani 1 1 d . . . H35 H 0.6180 0.2342 0.1377 0.088 Uiso 1 1 calc R . . C41 C 0.654(2) 0.618(2) 0.3466(14) 0.076(8) Uani 1 1 d . . . H41A H 0.6918 0.6669 0.3629 0.114 Uiso 1 1 calc R . . H41B H 0.5714 0.6288 0.3717 0.114 Uiso 1 1 calc R . . H41C H 0.6345 0.6523 0.2982 0.114 Uiso 1 1 calc R . . C42 C 0.841(3) 0.371(3) 0.4491(13) 0.097(10) Uani 1 1 d . . . H42A H 0.8712 0.4314 0.4599 0.146 Uiso 1 1 calc R . . H42B H 0.9141 0.2811 0.4532 0.146 Uiso 1 1 calc R . . H42C H 0.7693 0.3690 0.4807 0.146 Uiso 1 1 calc R . . C51 C 0.794(2) 0.565(2) 0.0488(11) 0.060(7) Uani 1 1 d . . . H51A H 0.8634 0.5719 0.0168 0.089 Uiso 1 1 calc R . . H51B H 0.7709 0.6287 0.0791 0.089 Uiso 1 1 calc R . . H51C H 0.7159 0.5867 0.0236 0.089 Uiso 1 1 calc R . . C52 C 0.922(2) 0.277(2) 0.0357(12) 0.069(8) Uani 1 1 d . . . H52A H 0.9847 0.2986 0.0048 0.103 Uiso 1 1 calc R . . H52B H 0.8477 0.2897 0.0097 0.103 Uiso 1 1 calc R . . H52C H 0.9665 0.1833 0.0590 0.103 Uiso 1 1 calc R . . C61 C 1.257(2) -0.133(3) 0.2452(13) 0.075(8) Uani 1 1 d . . . H61A H 1.3490 -0.1471 0.2417 0.113 Uiso 1 1 calc R . . H61B H 1.2143 -0.0876 0.2012 0.113 Uiso 1 1 calc R . . H61C H 1.2551 -0.2194 0.2588 0.113 Uiso 1 1 calc R . . C62 C 1.275(2) -0.104(2) 0.3844(13) 0.076(8) Uani 1 1 d . . . H62A H 1.3663 -0.1253 0.3694 0.114 Uiso 1 1 calc R . . H62B H 1.2702 -0.1865 0.4074 0.114 Uiso 1 1 calc R . . H62C H 1.2467 -0.0423 0.4157 0.114 Uiso 1 1 calc R . . C70 C 0.675(2) 0.043(2) 0.2556(11) 0.039(5) Uani 1 1 d . . . C71 C 0.870(2) -0.026(2) 0.1706(12) 0.054(6) Uani 1 1 d . . . C72 C 0.750(2) -0.023(2) 0.2001(13) 0.056(6) Uani 1 1 d . . . C73 C 0.696(2) -0.106(3) 0.1758(13) 0.064(7) Uani 1 1 d . . . C74 C 0.561(2) 0.022(3) 0.2890(15) 0.094(10) Uani 1 1 d . . . H74A H 0.5253 0.0739 0.3251 0.141 Uiso 1 1 calc R . . H74B H 0.5909 -0.0728 0.3085 0.141 Uiso 1 1 calc R . . H74C H 0.4925 0.0513 0.2555 0.141 Uiso 1 1 calc R . . C75 C 0.944(3) -0.117(2) 0.1175(16) 0.109(12) Uani 1 1 d . . . H75A H 1.0235 -0.1066 0.1011 0.163 Uiso 1 1 calc R . . H75B H 0.8856 -0.0917 0.0793 0.163 Uiso 1 1 calc R . . H75C H 0.9694 -0.2106 0.1389 0.163 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 U 0.0278(4) 0.0311(4) 0.0390(5) -0.0059(3) 0.0009(3) -0.0150(3) N1 0.030(9) 0.031(10) 0.059(13) 0.010(9) -0.007(9) -0.016(8) N3 0.042(11) 0.060(12) 0.050(13) 0.006(10) -0.005(9) -0.031(10) N2 0.038(10) 0.069(12) 0.036(11) -0.004(9) 0.014(8) -0.044(10) N5 0.041(10) 0.040(11) 0.062(13) -0.003(10) 0.000(9) -0.027(9) N4 0.039(10) 0.035(10) 0.056(13) -0.022(10) 0.016(9) -0.021(9) N6 0.017(8) 0.040(10) 0.073(14) 0.007(10) 0.000(9) -0.015(8) N7 0.053(11) 0.027(9) 0.046(12) -0.005(9) 0.000(9) -0.021(9) N8 0.047(12) 0.058(13) 0.069(15) -0.018(11) 0.005(11) -0.024(11) N9 0.17(3) 0.087(19) 0.12(2) -0.036(16) -0.033(19) -0.083(19) Si1 0.039(3) 0.041(4) 0.060(5) -0.012(3) 0.009(3) -0.016(3) Si2 0.035(3) 0.049(4) 0.067(5) -0.021(4) 0.003(3) -0.019(3) Si3 0.044(4) 0.054(4) 0.045(4) -0.002(3) 0.000(3) -0.025(3) C1 0.09(2) 0.064(19) 0.13(3) -0.06(2) 0.04(2) -0.055(17) C2 0.064(16) 0.055(16) 0.08(2) -0.013(15) 0.001(15) -0.034(14) C3 0.058(18) 0.15(3) 0.07(2) 0.02(2) 0.007(17) -0.07(2) C4 0.058(17) 0.10(2) 0.060(19) 0.028(17) 0.008(15) -0.047(16) C5 0.11(2) 0.051(16) 0.07(2) -0.004(14) -0.044(17) -0.057(16) C6 0.052(16) 0.08(2) 0.08(2) -0.064(17) 0.028(14) -0.027(15) C10 0.029(11) 0.036(13) 0.035(14) 0.008(11) -0.016(10) -0.007(10) C11 0.09(2) 0.09(2) 0.07(2) -0.032(18) 0.000(17) -0.038(19) C12 0.13(3) 0.08(2) 0.11(3) -0.03(2) 0.03(2) -0.08(2) C13 0.14(3) 0.12(3) 0.05(2) -0.024(19) 0.017(19) -0.11(2) C14 0.071(17) 0.09(2) 0.040(16) -0.015(15) 0.007(13) -0.053(16) C15 0.091(19) 0.061(16) 0.033(15) -0.026(13) 0.005(14) -0.043(15) C20 0.067(15) 0.053(14) 0.017(12) 0.005(11) -0.003(11) -0.043(13) C21 0.052(16) 0.10(2) 0.054(18) 0.004(16) -0.003(14) -0.029(15) C22 0.045(15) 0.12(2) 0.035(16) 0.009(16) 0.031(13) -0.008(16) C23 0.061(18) 0.07(2) 0.10(3) -0.003(18) -0.003(18) -0.033(16) C24 0.07(2) 0.15(3) 0.08(2) 0.04(2) -0.035(17) -0.08(2) C25 0.036(13) 0.11(2) 0.053(17) 0.024(15) -0.031(12) -0.037(14) C30 0.069(17) 0.12(2) 0.045(16) -0.014(16) -0.001(13) -0.083(19) C31 0.033(13) 0.033(13) 0.08(2) 0.008(13) -0.025(13) 0.016(11) C32 0.08(2) 0.07(2) 0.08(2) -0.006(19) -0.029(19) 0.030(18) C33 0.021(14) 0.08(2) 0.13(3) 0.02(2) -0.024(16) 0.015(15) C34 0.062(18) 0.12(3) 0.09(2) 0.02(2) -0.025(17) -0.06(2) C35 0.047(15) 0.071(18) 0.09(2) -0.008(16) -0.018(15) -0.017(14) C41 0.048(15) 0.072(18) 0.11(2) -0.021(17) -0.011(15) -0.024(14) C42 0.11(2) 0.16(3) 0.08(2) -0.07(2) 0.039(19) -0.10(2) C51 0.075(17) 0.065(16) 0.031(14) 0.013(12) -0.014(12) -0.031(14) C52 0.088(19) 0.050(15) 0.08(2) -0.038(14) -0.003(15) -0.025(14) C61 0.053(16) 0.09(2) 0.08(2) -0.022(17) 0.003(14) -0.027(15) C62 0.065(17) 0.065(18) 0.08(2) 0.007(15) -0.033(15) -0.015(14) C70 0.039(12) 0.037(12) 0.053(16) -0.011(11) -0.018(11) -0.021(11) C71 0.048(15) 0.055(16) 0.040(16) -0.019(13) -0.003(12) -0.002(13) C72 0.060(16) 0.036(14) 0.069(19) -0.022(13) 0.005(14) -0.015(12) C73 0.069(17) 0.058(17) 0.063(19) -0.007(15) -0.015(14) -0.024(15) C74 0.08(2) 0.12(3) 0.11(3) -0.03(2) -0.010(18) -0.064(19) C75 0.13(3) 0.047(16) 0.15(3) -0.061(19) 0.07(2) -0.038(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 U N2 2.254(16) . ? U N1 2.296(15) . ? U N3 2.340(17) . ? U N7 2.433(15) . ? U N8 2.47(2) . ? U N4 2.719(16) . ? U N5 2.724(16) . ? U N6 2.767(14) . ? U Si3 3.240(6) . ? U Si2 3.264(7) . ? U Si1 3.285(6) . ? N1 C10 1.42(2) . ? N1 Si1 1.690(16) . ? N3 C30 1.41(3) . ? N3 Si3 1.660(17) . ? N2 C20 1.43(2) . ? N2 Si2 1.718(17) . ? N5 C2 1.46(3) . ? N5 C3 1.54(3) . ? N5 Si3 1.765(18) . ? N4 C1 1.48(3) . ? N4 C6 1.50(3) . ? N4 Si2 1.784(16) . ? N6 C4 1.47(3) . ? N6 C5 1.50(3) . ? N6 Si1 1.794(16) . ? N7 C70 1.28(2) . ? N8 C71 1.28(3) . ? N9 C73 1.12(3) . ? Si1 C62 1.80(2) . ? Si1 C61 1.85(2) . ? Si2 C42 1.84(3) . ? Si2 C41 1.88(2) . ? Si3 C51 1.86(2) . ? Si3 C52 1.87(2) . ? C1 C2 1.45(3) . ? C3 C4 1.37(3) . ? C5 C6 1.39(3) . ? C10 C11 1.39(3) . ? C10 C15 1.41(3) . ? C11 C12 1.44(3) . ? C12 C13 1.27(3) . ? C13 C14 1.35(3) . ? C14 C15 1.46(3) . ? C20 C25 1.35(3) . ? C20 C21 1.43(3) . ? C21 C22 1.40(3) . ? C22 C23 1.39(3) . ? C23 C24 1.36(3) . ? C24 C25 1.35(3) . ? C30 C35 1.40(3) . ? C30 C31 1.43(3) . ? C31 C32 1.39(3) . ? C32 C33 1.37(4) . ? C33 C34 1.36(4) . ? C34 C35 1.47(3) . ? C70 C72 1.43(3) . ? C70 C74 1.45(3) . ? C71 C72 1.39(3) . ? C71 C75 1.53(3) . ? C72 C73 1.50(3) . ? 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 U N1 101.6(6) . . ? N2 U N3 94.7(6) . . ? N1 U N3 158.8(6) . . ? N2 U N7 76.3(5) . . ? N1 U N7 81.5(5) . . ? N3 U N7 89.6(5) . . ? N2 U N8 144.4(6) . . ? N1 U N8 79.0(6) . . ? N3 U N8 79.9(6) . . ? N7 U N8 68.6(6) . . ? N2 U N4 62.5(5) . . ? N1 U N4 102.6(6) . . ? N3 U N4 96.8(6) . . ? N7 U N4 138.7(5) . . ? N8 U N4 152.8(5) . . ? N2 U N5 118.3(5) . . ? N1 U N5 120.5(5) . . ? N3 U N5 60.6(5) . . ? N7 U N5 146.4(5) . . ? N8 U N5 89.8(6) . . ? N4 U N5 65.7(5) . . ? N2 U N6 116.3(6) . . ? N1 U N6 59.5(5) . . ? N3 U N6 124.1(5) . . ? N7 U N6 140.3(5) . . ? N8 U N6 95.0(6) . . ? N4 U N6 64.3(5) . . ? N5 U N6 63.7(5) . . ? N2 U Si3 115.0(4) . . ? N1 U Si3 142.4(4) . . ? N3 U Si3 29.4(4) . . ? N7 U Si3 114.1(4) . . ? N8 U Si3 76.1(5) . . ? N4 U Si3 87.7(4) . . ? N5 U Si3 33.0(4) . . ? N6 U Si3 95.0(4) . . ? N2 U Si2 29.7(4) . . ? N1 U Si2 100.9(5) . . ? N3 U Si2 100.0(5) . . ? N7 U Si2 105.5(4) . . ? N8 U Si2 174.1(4) . . ? N4 U Si2 33.1(3) . . ? N5 U Si2 95.3(4) . . ? N6 U Si2 90.0(4) . . ? Si3 U Si2 106.63(17) . . ? N2 U Si1 119.9(4) . . ? N1 U Si1 28.9(4) . . ? N3 U Si1 143.9(4) . . ? N7 U Si1 107.3(4) . . ? N8 U Si1 77.2(4) . . ? N4 U Si1 91.2(4) . . ? N5 U Si1 91.6(4) . . ? N6 U Si1 33.1(3) . . ? Si3 U Si1 116.73(16) . . ? Si2 U Si1 105.64(16) . . ? C10 N1 Si1 121.1(13) . . ? C10 N1 U 126.0(11) . . ? Si1 N1 U 110.1(8) . . ? C30 N3 Si3 123.5(15) . . ? C30 N3 U 129.5(14) . . ? Si3 N3 U 107.0(8) . . ? C20 N2 Si2 115.6(13) . . ? C20 N2 U 134.5(13) . . ? Si2 N2 U 109.8(7) . . ? C2 N5 C3 108.9(18) . . ? C2 N5 Si3 111.8(14) . . ? C3 N5 Si3 126.1(16) . . ? C2 N5 U 113.0(13) . . ? C3 N5 U 105.5(12) . . ? Si3 N5 U 89.8(6) . . ? C1 N4 C6 112.4(18) . . ? C1 N4 Si2 116.4(15) . . ? C6 N4 Si2 116.0(14) . . ? C1 N4 U 103.0(13) . . ? C6 N4 U 116.0(12) . . ? Si2 N4 U 90.5(6) . . ? C4 N6 C5 117.9(19) . . ? C4 N6 Si1 118.6(16) . . ? C5 N6 Si1 108.6(13) . . ? C4 N6 U 114.4(14) . . ? C5 N6 U 103.4(12) . . ? Si1 N6 U 89.5(6) . . ? C70 N7 U 142.3(15) . . ? C71 N8 U 138.3(16) . . ? N1 Si1 N6 93.8(7) . . ? N1 Si1 C62 115.5(11) . . ? N6 Si1 C62 112.5(11) . . ? N1 Si1 C61 120.8(10) . . ? N6 Si1 C61 109.3(11) . . ? C62 Si1 C61 104.7(12) . . ? N1 Si1 U 41.0(5) . . ? N6 Si1 U 57.4(5) . . ? C62 Si1 U 143.0(9) . . ? C61 Si1 U 112.2(8) . . ? N2 Si2 N4 96.4(8) . . ? N2 Si2 C42 116.1(10) . . ? N4 Si2 C42 109.2(10) . . ? N2 Si2 C41 113.1(10) . . ? N4 Si2 C41 110.9(10) . . ? C42 Si2 C41 110.3(13) . . ? N2 Si2 U 40.5(5) . . ? N4 Si2 U 56.4(5) . . ? C42 Si2 U 119.7(9) . . ? C41 Si2 U 129.9(9) . . ? N3 Si3 N5 97.6(9) . . ? N3 Si3 C51 114.8(10) . . ? N5 Si3 C51 114.0(9) . . ? N3 Si3 C52 114.9(10) . . ? N5 Si3 C52 110.9(10) . . ? C51 Si3 C52 105.0(11) . . ? N3 Si3 U 43.7(6) . . ? N5 Si3 U 57.2(5) . . ? C51 Si3 U 143.2(8) . . ? C52 Si3 U 111.4(8) . . ? C2 C1 N4 117(2) . . ? C1 C2 N5 115.0(19) . . ? C4 C3 N5 121(2) . . ? C3 C4 N6 116(2) . . ? C6 C5 N6 122(2) . . ? C5 C6 N4 112.8(19) . . ? C11 C10 C15 114(2) . . ? C11 C10 N1 125(2) . . ? C15 C10 N1 121(2) . . ? C10 C11 C12 121(3) . . ? C13 C12 C11 126(3) . . ? C12 C13 C14 117(3) . . ? C13 C14 C15 122(2) . . ? C10 C15 C14 121(2) . . ? C25 C20 C21 114(2) . . ? C25 C20 N2 123.9(18) . . ? C21 C20 N2 122.1(19) . . ? C22 C21 C20 124(2) . . ? C23 C22 C21 116(2) . . ? C24 C23 C22 121(2) . . ? C25 C24 C23 120(3) . . ? C20 C25 C24 125(2) . . ? C35 C30 N3 118(2) . . ? C35 C30 C31 120(2) . . ? N3 C30 C31 122(2) . . ? C32 C31 C30 118(3) . . ? C33 C32 C31 123(3) . . ? C34 C33 C32 119(3) . . ? C33 C34 C35 121(3) . . ? C30 C35 C34 118(2) . . ? N7 C70 C72 119(2) . . ? N7 C70 C74 119(2) . . ? C72 C70 C74 122(2) . . ? N8 C71 C72 123(2) . . ? N8 C71 C75 117(2) . . ? C72 C71 C75 119(2) . . ? C71 C72 C70 127(2) . . ? C71 C72 C73 118(2) . . ? C70 C72 C73 115(2) . . ? N9 C73 C72 179(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.771 _refine_diff_density_min -1.645 _refine_diff_density_rms 0.235 # ===END data_UtacnOPPh3 _database_code_depnum_ccdc_archive 'CCDC 299439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 N6 O P Si3 U, 2(C7 H8)' _chemical_formula_sum 'C62 H76 N6 O P Si3 U' _chemical_formula_weight 1274.56 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' 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.2797(4) _cell_length_b 17.8483(6) _cell_length_c 27.1851(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5958.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2588 _exptl_absorpt_coefficient_mu 2.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5018 _exptl_absorpt_correction_T_max 0.6905 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 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 70126 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1257 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 34.41 _reflns_number_total 24465 _reflns_number_gt 18480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(3) _refine_ls_number_reflns 24465 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.004 _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 U U 0.824213(9) 0.591352(6) 0.095529(4) 0.00897(2) Uani 1 1 d . . . N1 N 0.8651(2) 0.64475(15) 0.01440(10) 0.0137(6) Uani 1 1 d . . . N2 N 0.9716(2) 0.56679(14) 0.15507(10) 0.0132(6) Uani 1 1 d . . . N3 N 0.65380(19) 0.52279(14) 0.10439(10) 0.0117(6) Uani 1 1 d . . . N4 N 0.8807(2) 0.69827(15) 0.16442(11) 0.0140(6) Uani 1 1 d . . . N5 N 0.6536(2) 0.65061(15) 0.15070(10) 0.0143(6) Uani 1 1 d . . . N6 N 0.7636(2) 0.73601(14) 0.07408(11) 0.0148(6) Uani 1 1 d . . . Si1 Si 0.77465(7) 0.71640(5) 0.01016(4) 0.0141(2) Uani 1 1 d . . . Si2 Si 1.00827(8) 0.65421(5) 0.17286(4) 0.0147(2) Uani 1 1 d . . . Si3 Si 0.59684(8) 0.55964(5) 0.15561(4) 0.0141(2) Uani 1 1 d . . . C1 C 0.8065(3) 0.68279(19) 0.20652(13) 0.0183(8) Uani 1 1 d . . . H1A H 0.8254 0.7161 0.2334 0.022 Uiso 1 1 calc R . . H1B H 0.8188 0.6319 0.2177 0.022 Uiso 1 1 calc R . . C2 C 0.6865(3) 0.69217(18) 0.19506(13) 0.0179(7) Uani 1 1 d . . . H2A H 0.6440 0.6747 0.2228 0.021 Uiso 1 1 calc R . . H2B H 0.6707 0.7449 0.1904 0.021 Uiso 1 1 calc R . . C3 C 0.5922(3) 0.69723(19) 0.11535(13) 0.0190(8) Uani 1 1 d . . . H3A H 0.5286 0.7175 0.1317 0.023 Uiso 1 1 calc R . . H3B H 0.5671 0.6657 0.0886 0.023 Uiso 1 1 calc R . . C4 C 0.6579(2) 0.76138(16) 0.09406(15) 0.0188(7) Uani 1 1 d . . . H4A H 0.6163 0.7852 0.0681 0.023 Uiso 1 1 calc R . . H4B H 0.6708 0.7984 0.1195 0.023 Uiso 1 1 calc R . . C5 C 0.8561(2) 0.78170(17) 0.09222(14) 0.0181(7) Uani 1 1 d . . . H5A H 0.8433 0.8336 0.0834 0.022 Uiso 1 1 calc R . . H5B H 0.9218 0.7656 0.0755 0.022 Uiso 1 1 calc R . . C6 C 0.8750(3) 0.77724(18) 0.14732(13) 0.0189(8) Uani 1 1 d . . . H6A H 0.9426 0.8026 0.1554 0.023 Uiso 1 1 calc R . . H6B H 0.8163 0.8027 0.1643 0.023 Uiso 1 1 calc R . . C10 C 0.6361(3) 0.69092(19) -0.01269(14) 0.0199(8) Uani 1 1 d . . . H10A H 0.5913 0.7350 -0.0139 0.030 Uiso 1 1 calc R . . H10B H 0.6038 0.6549 0.0091 0.030 Uiso 1 1 calc R . . H10C H 0.6418 0.6698 -0.0451 0.030 Uiso 1 1 calc R . . C11 C 0.8223(3) 0.80032(17) -0.02513(13) 0.0204(7) Uani 1 1 d . . . H11A H 0.7658 0.8375 -0.0256 0.031 Uiso 1 1 calc R . . H11B H 0.8396 0.7858 -0.0582 0.031 Uiso 1 1 calc R . . H11C H 0.8860 0.8207 -0.0096 0.031 Uiso 1 1 calc R . . C12 C 0.9312(3) 0.61849(17) -0.02352(12) 0.0123(7) Uani 1 1 d . . . C13 C 1.0320(2) 0.58671(19) -0.01323(12) 0.0150(6) Uani 1 1 d . . . H13 H 1.0563 0.5856 0.0192 0.018 Uiso 1 1 calc R . . C14 C 1.0975(3) 0.55655(18) -0.04977(14) 0.0173(7) Uani 1 1 d . . . H14 H 1.1639 0.5349 -0.0414 0.021 Uiso 1 1 calc R . . C15 C 1.0658(3) 0.55826(17) -0.09813(15) 0.0197(7) Uani 1 1 d . . . H15 H 1.1095 0.5375 -0.1225 0.024 Uiso 1 1 calc R . . C16 C 0.9670(3) 0.5916(2) -0.10992(12) 0.0195(7) Uani 1 1 d . . . H16 H 0.9451 0.5939 -0.1426 0.023 Uiso 1 1 calc R . . C17 C 0.9007(3) 0.62152(18) -0.07370(13) 0.0165(7) Uani 1 1 d . . . H17 H 0.8352 0.6439 -0.0825 0.020 Uiso 1 1 calc R . . C20 C 1.1118(3) 0.7021(2) 0.13330(14) 0.0236(8) Uani 1 1 d . . . H20A H 1.1270 0.7509 0.1464 0.035 Uiso 1 1 calc R . . H20B H 1.0839 0.7069 0.1005 0.035 Uiso 1 1 calc R . . H20C H 1.1775 0.6730 0.1327 0.035 Uiso 1 1 calc R . . C21 C 1.0543(3) 0.6629(2) 0.23795(14) 0.0265(9) Uani 1 1 d . . . H21A H 1.0733 0.7141 0.2447 0.040 Uiso 1 1 calc R . . H21B H 1.1166 0.6315 0.2432 0.040 Uiso 1 1 calc R . . H21C H 0.9965 0.6477 0.2596 0.040 Uiso 1 1 calc R . . C22 C 1.0234(3) 0.50197(18) 0.17112(12) 0.0145(7) Uani 1 1 d . . . C23 C 1.1366(3) 0.4995(2) 0.18250(13) 0.0196(8) Uani 1 1 d . . . H23 H 1.1780 0.5430 0.1801 0.023 Uiso 1 1 calc R . . C24 C 1.1857(3) 0.4339(2) 0.19702(14) 0.0271(9) Uani 1 1 d . . . H24 H 1.2597 0.4338 0.2042 0.033 Uiso 1 1 calc R . . C25 C 1.1274(3) 0.3682(2) 0.20109(15) 0.0302(10) Uani 1 1 d . . . H25 H 1.1611 0.3242 0.2113 0.036 Uiso 1 1 calc R . . C26 C 1.0172(3) 0.3692(2) 0.18966(13) 0.0238(9) Uani 1 1 d . . . H26 H 0.9770 0.3251 0.1914 0.029 Uiso 1 1 calc R . . C27 C 0.9671(3) 0.43437(17) 0.17590(12) 0.0152(7) Uani 1 1 d . . . H27 H 0.8927 0.4336 0.1695 0.018 Uiso 1 1 calc R . . C30 C 0.4443(3) 0.5622(2) 0.15511(15) 0.0248(9) Uani 1 1 d . . . H30A H 0.4185 0.5838 0.1853 0.037 Uiso 1 1 calc R . . H30B H 0.4164 0.5122 0.1519 0.037 Uiso 1 1 calc R . . H30C H 0.4197 0.5920 0.1279 0.037 Uiso 1 1 calc R . . C31 C 0.6424(3) 0.5178(2) 0.21494(14) 0.0243(9) Uani 1 1 d . . . H31A H 0.6058 0.5422 0.2417 0.036 Uiso 1 1 calc R . . H31B H 0.7197 0.5244 0.2184 0.036 Uiso 1 1 calc R . . H31C H 0.6254 0.4653 0.2153 0.036 Uiso 1 1 calc R . . C32 C 0.6135(2) 0.46107(17) 0.07930(12) 0.0107(7) Uani 1 1 d . . . C33 C 0.5576(2) 0.40212(19) 0.10258(12) 0.0155(7) Uani 1 1 d . . . H33 H 0.5427 0.4057 0.1360 0.019 Uiso 1 1 calc R . . C34 C 0.5242(3) 0.33919(19) 0.07728(13) 0.0169(7) Uani 1 1 d . . . H34 H 0.4869 0.3013 0.0937 0.020 Uiso 1 1 calc R . . C35 C 0.5463(3) 0.33227(19) 0.02751(13) 0.0177(8) Uani 1 1 d . . . H35 H 0.5271 0.2889 0.0106 0.021 Uiso 1 1 calc R . . C36 C 0.5969(2) 0.39023(17) 0.00337(13) 0.0129(7) Uani 1 1 d . . . H36 H 0.6090 0.3868 -0.0303 0.015 Uiso 1 1 calc R . . C37 C 0.6301(2) 0.45360(18) 0.02854(13) 0.0126(7) Uani 1 1 d . . . H37 H 0.6642 0.4921 0.0114 0.015 Uiso 1 1 calc R . . O O 0.88622(17) 0.47191(12) 0.05802(8) 0.0111(5) Uani 1 1 d . . . P P 0.92844(6) 0.39910(5) 0.03734(3) 0.00977(16) Uani 1 1 d . . . C40 C 1.0721(2) 0.40271(19) 0.02544(11) 0.0118(6) Uani 1 1 d . . . C41 C 1.1381(3) 0.4412(2) 0.05929(13) 0.0183(8) Uani 1 1 d . . . H41 H 1.1067 0.4633 0.0868 0.022 Uiso 1 1 calc R . . C42 C 1.2484(3) 0.4463(2) 0.05213(15) 0.0269(9) Uani 1 1 d . . . H42 H 1.2914 0.4712 0.0750 0.032 Uiso 1 1 calc R . . C43 C 1.2953(3) 0.4149(2) 0.01123(14) 0.0241(9) Uani 1 1 d . . . H43 H 1.3699 0.4195 0.0061 0.029 Uiso 1 1 calc R . . C44 C 1.2323(3) 0.3766(2) -0.02228(15) 0.0231(9) Uani 1 1 d . . . H44 H 1.2648 0.3550 -0.0497 0.028 Uiso 1 1 calc R . . C45 C 1.1203(3) 0.36983(18) -0.01538(14) 0.0162(8) Uani 1 1 d . . . H45 H 1.0782 0.3435 -0.0380 0.019 Uiso 1 1 calc R . . C50 C 0.8651(2) 0.37335(17) -0.01985(13) 0.0115(7) Uani 1 1 d . . . C51 C 0.8518(3) 0.42748(17) -0.05645(13) 0.0167(7) Uani 1 1 d . . . H51 H 0.8761 0.4762 -0.0510 0.020 Uiso 1 1 calc R . . C52 C 0.8031(2) 0.4093(2) -0.10052(13) 0.0204(7) Uani 1 1 d . . . H52 H 0.7946 0.4458 -0.1247 0.024 Uiso 1 1 calc R . . C53 C 0.7666(3) 0.3369(2) -0.10905(13) 0.0195(8) Uani 1 1 d . . . H53 H 0.7329 0.3251 -0.1387 0.023 Uiso 1 1 calc R . . C54 C 0.7802(3) 0.28254(19) -0.07364(13) 0.0169(7) Uani 1 1 d . . . H54 H 0.7573 0.2337 -0.0796 0.020 Uiso 1 1 calc R . . C55 C 0.8281(3) 0.30064(16) -0.02915(12) 0.0133(6) Uani 1 1 d . . . H55 H 0.8359 0.2640 -0.0051 0.016 Uiso 1 1 calc R . . C60 C 0.9057(3) 0.32143(17) 0.07793(12) 0.0121(7) Uani 1 1 d . . . C61 C 0.9817(3) 0.26401(17) 0.08488(12) 0.0143(7) Uani 1 1 d . . . H61 H 1.0490 0.2663 0.0693 0.017 Uiso 1 1 calc R . . C62 C 0.9566(3) 0.20406(19) 0.11482(13) 0.0182(8) Uani 1 1 d . . . H62 H 1.0066 0.1653 0.1184 0.022 Uiso 1 1 calc R . . C63 C 0.8594(3) 0.20083(19) 0.13930(13) 0.0188(8) Uani 1 1 d . . . H63 H 0.8441 0.1608 0.1601 0.023 Uiso 1 1 calc R . . C64 C 0.7841(3) 0.25760(19) 0.13292(13) 0.0201(8) Uani 1 1 d . . . H64 H 0.7179 0.2556 0.1495 0.024 Uiso 1 1 calc R . . C65 C 0.8063(3) 0.31757(17) 0.10205(14) 0.0182(8) Uani 1 1 d . . . H65 H 0.7547 0.3551 0.0975 0.022 Uiso 1 1 calc R . . C70 C 0.6142(4) 0.1035(3) 0.2023(2) 0.0552(15) Uani 1 1 d . . . H70A H 0.6365 0.1029 0.1685 0.083 Uiso 1 1 calc R . . H70B H 0.5579 0.0669 0.2073 0.083 Uiso 1 1 calc R . . H70C H 0.6754 0.0917 0.2229 0.083 Uiso 1 1 calc R . . C71 C 0.5720(3) 0.1792(2) 0.21519(16) 0.0287(9) Uani 1 1 d . . . C72 C 0.6189(3) 0.2200(3) 0.25319(15) 0.0328(10) Uani 1 1 d . . . H72 H 0.6768 0.1998 0.2709 0.039 Uiso 1 1 calc R . . C73 C 0.5794(4) 0.2914(3) 0.26497(19) 0.0510(15) Uani 1 1 d . . . H73 H 0.6107 0.3187 0.2904 0.061 Uiso 1 1 calc R . . C74 C 0.4941(4) 0.3206(3) 0.2386(2) 0.0506(15) Uani 1 1 d . . . H74 H 0.4677 0.3681 0.2461 0.061 Uiso 1 1 calc R . . C75 C 0.4487(4) 0.2809(3) 0.20208(19) 0.0451(13) Uani 1 1 d . . . H75 H 0.3906 0.3009 0.1845 0.054 Uiso 1 1 calc R . . C76 C 0.4868(3) 0.2115(3) 0.19049(15) 0.0331(10) Uani 1 1 d . . . H76 H 0.4539 0.1852 0.1650 0.040 Uiso 1 1 calc R . . C80 C 0.1743(3) 0.9240(2) 0.18622(15) 0.0390(11) Uani 1 1 d . . . H80A H 0.2238 0.9044 0.1621 0.058 Uiso 1 1 calc R . . H80B H 0.1568 0.8855 0.2096 0.058 Uiso 1 1 calc R . . H80C H 0.2077 0.9654 0.2029 0.058 Uiso 1 1 calc R . . C81 C 0.0712(3) 0.9501(2) 0.16104(15) 0.0228(8) Uani 1 1 d . . . C82 C 0.0680(3) 0.9588(2) 0.11051(14) 0.0265(9) Uani 1 1 d . . . H82 H 0.1298 0.9490 0.0918 0.032 Uiso 1 1 calc R . . C83 C -0.0268(3) 0.9822(2) 0.08754(15) 0.0301(10) Uani 1 1 d . . . H83 H -0.0280 0.9883 0.0536 0.036 Uiso 1 1 calc R . . C84 C -0.1193(3) 0.9964(2) 0.11471(15) 0.0285(10) Uani 1 1 d . . . H84 H -0.1832 1.0113 0.0993 0.034 Uiso 1 1 calc R . . C85 C -0.1157(3) 0.9881(2) 0.16505(16) 0.0285(9) Uani 1 1 d . . . H85 H -0.1777 0.9979 0.1836 0.034 Uiso 1 1 calc R . . C86 C -0.0222(3) 0.9656(2) 0.18807(14) 0.0240(8) Uani 1 1 d . . . H86 H -0.0212 0.9606 0.2221 0.029 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 U 0.00945(4) 0.00682(4) 0.01065(5) -0.00090(5) 0.00078(5) 0.00011(5) N1 0.0146(14) 0.0104(13) 0.0161(16) 0.0023(11) 0.0029(11) 0.0013(10) N2 0.0144(14) 0.0102(13) 0.0151(15) 0.0014(11) -0.0018(11) 0.0003(11) N3 0.0063(13) 0.0127(12) 0.0160(16) -0.0020(11) 0.0013(10) -0.0015(9) N4 0.0175(14) 0.0087(13) 0.0159(16) -0.0038(11) 0.0033(12) -0.0038(11) N5 0.0144(15) 0.0124(13) 0.0162(15) -0.0031(11) 0.0004(11) 0.0041(11) N6 0.0117(13) 0.0084(13) 0.0243(17) -0.0001(12) 0.0034(12) -0.0011(11) Si1 0.0127(5) 0.0110(5) 0.0187(5) 0.0050(4) -0.0006(4) 0.0012(4) Si2 0.0152(5) 0.0138(5) 0.0150(5) -0.0015(4) -0.0015(4) -0.0039(4) Si3 0.0133(5) 0.0154(5) 0.0137(5) -0.0028(4) 0.0044(4) -0.0026(4) C1 0.021(2) 0.0183(17) 0.0160(18) -0.0079(14) 0.0009(15) -0.0033(14) C2 0.0171(18) 0.0156(16) 0.0210(19) -0.0092(13) 0.0043(16) 0.0001(15) C3 0.0129(17) 0.0179(18) 0.026(2) 0.0003(15) 0.0050(14) 0.0066(14) C4 0.0168(17) 0.0141(14) 0.0256(18) 0.0009(16) 0.0035(17) 0.0077(12) C5 0.0193(16) 0.0068(14) 0.028(2) 0.0015(16) 0.0018(16) -0.0009(11) C6 0.0202(18) 0.0097(16) 0.027(2) -0.0019(15) -0.0028(15) -0.0005(14) C10 0.0165(18) 0.0195(18) 0.024(2) 0.0049(16) -0.0004(15) 0.0022(14) C11 0.0141(16) 0.0169(16) 0.030(2) 0.0086(14) 0.0008(18) 0.0022(16) C12 0.0140(16) 0.0078(14) 0.0150(18) 0.0017(12) 0.0034(13) -0.0036(12) C13 0.0170(15) 0.0104(15) 0.0177(17) 0.0041(15) 0.0013(13) -0.0018(14) C14 0.0174(17) 0.0104(16) 0.024(2) 0.0031(14) 0.0038(15) 0.0032(13) C15 0.0265(18) 0.0133(16) 0.0194(19) -0.0010(16) 0.0091(18) -0.0010(13) C16 0.0297(18) 0.0166(16) 0.0122(16) 0.0005(16) 0.0025(13) -0.0063(17) C17 0.0152(17) 0.0152(17) 0.0190(19) 0.0053(14) 0.0006(14) -0.0038(13) C20 0.022(2) 0.0172(19) 0.031(2) 0.0022(16) 0.0015(17) -0.0023(15) C21 0.030(2) 0.029(2) 0.021(2) -0.0046(17) -0.0066(17) -0.0042(17) C22 0.0186(17) 0.0187(18) 0.0062(17) -0.0013(13) -0.0016(14) 0.0031(14) C23 0.0169(17) 0.0225(19) 0.019(2) 0.0002(15) -0.0017(15) -0.0002(14) C24 0.021(2) 0.034(2) 0.026(2) 0.0029(16) -0.0063(18) 0.0077(18) C25 0.040(3) 0.026(2) 0.024(2) 0.0090(18) -0.0058(19) 0.0118(18) C26 0.038(2) 0.0200(19) 0.014(2) 0.0028(15) -0.0023(17) -0.0006(17) C27 0.0197(17) 0.0126(16) 0.0133(18) -0.0020(13) -0.0016(14) -0.0036(13) C30 0.0184(19) 0.026(2) 0.030(2) -0.0090(17) 0.0076(16) -0.0019(15) C31 0.033(2) 0.0208(19) 0.020(2) 0.0040(16) 0.0064(17) -0.0019(15) C32 0.0024(13) 0.0101(15) 0.0198(19) -0.0030(13) -0.0017(12) 0.0023(11) C33 0.0137(14) 0.0193(16) 0.0135(18) -0.0005(16) 0.0029(12) -0.0020(13) C34 0.0130(16) 0.0155(17) 0.022(2) 0.0033(14) -0.0016(14) -0.0019(13) C35 0.0133(17) 0.0155(17) 0.024(2) -0.0079(15) -0.0031(14) -0.0009(13) C36 0.0115(15) 0.0141(17) 0.0130(17) -0.0020(13) -0.0025(13) 0.0027(12) C37 0.0086(15) 0.0111(16) 0.0182(19) 0.0018(13) 0.0004(13) 0.0010(12) O 0.0102(11) 0.0081(11) 0.0149(13) -0.0004(9) 0.0018(9) -0.0004(9) P 0.0101(4) 0.0079(4) 0.0113(4) -0.0003(3) 0.0020(3) 0.0007(3) C40 0.0129(14) 0.0082(15) 0.0141(16) 0.0055(14) 0.0041(12) 0.0017(13) C41 0.0147(17) 0.0260(19) 0.0144(19) 0.0018(15) 0.0002(14) -0.0004(14) C42 0.0145(19) 0.038(2) 0.028(2) 0.0115(19) -0.0035(16) -0.0051(17) C43 0.0122(16) 0.025(2) 0.035(2) 0.0137(19) 0.0101(14) 0.0036(15) C44 0.026(2) 0.0174(19) 0.026(2) 0.0094(16) 0.0167(18) 0.0140(16) C45 0.0220(19) 0.0068(16) 0.020(2) 0.0001(14) 0.0048(16) 0.0016(14) C50 0.0090(15) 0.0099(15) 0.0157(18) -0.0022(13) 0.0012(13) 0.0025(12) C51 0.0189(18) 0.0102(16) 0.0210(19) -0.0014(13) 0.0020(14) -0.0019(12) C52 0.0230(18) 0.0217(15) 0.0164(17) 0.0053(18) -0.0003(14) 0.0017(16) C53 0.0137(17) 0.030(2) 0.015(2) -0.0077(15) 0.0017(13) -0.0007(15) C54 0.0126(16) 0.0135(17) 0.024(2) -0.0075(15) 0.0022(14) -0.0021(13) C55 0.0116(14) 0.0109(14) 0.0174(17) -0.0002(12) 0.0018(15) 0.0026(14) C60 0.0163(17) 0.0069(15) 0.0130(17) -0.0022(12) -0.0010(13) 0.0015(12) C61 0.0134(15) 0.0160(16) 0.0134(19) -0.0016(13) 0.0003(13) 0.0027(13) C62 0.0212(19) 0.0130(17) 0.020(2) 0.0000(14) -0.0071(15) 0.0033(14) C63 0.028(2) 0.0117(17) 0.0166(19) 0.0028(14) -0.0013(15) -0.0055(14) C64 0.0217(18) 0.0183(18) 0.020(2) 0.0070(15) 0.0050(15) -0.0058(14) C65 0.0176(19) 0.0126(15) 0.025(2) 0.0010(14) 0.0034(16) -0.0009(12) C70 0.051(3) 0.043(3) 0.071(4) -0.011(3) 0.034(3) -0.011(3) C71 0.029(2) 0.030(2) 0.027(2) 0.0003(18) 0.0166(18) -0.0081(17) C72 0.020(2) 0.053(3) 0.025(2) 0.008(2) 0.0028(17) -0.005(2) C73 0.053(3) 0.052(3) 0.047(3) -0.020(3) 0.023(3) -0.035(3) C74 0.053(3) 0.025(3) 0.073(4) 0.011(3) 0.033(3) -0.002(2) C75 0.034(3) 0.054(3) 0.048(3) 0.027(3) 0.014(2) 0.003(2) C76 0.024(2) 0.055(3) 0.020(2) 0.001(2) 0.0031(17) -0.010(2) C80 0.031(2) 0.051(3) 0.035(2) -0.006(2) -0.004(2) 0.004(2) C81 0.028(2) 0.0145(18) 0.026(2) -0.0032(16) 0.0006(17) -0.0041(15) C82 0.030(2) 0.028(2) 0.021(2) -0.0053(16) 0.0044(17) -0.0101(17) C83 0.048(3) 0.025(2) 0.018(2) 0.0015(16) -0.0010(19) -0.0137(18) C84 0.034(2) 0.019(2) 0.033(3) 0.0066(17) -0.0093(19) -0.0021(17) C85 0.031(2) 0.020(2) 0.034(3) -0.0003(18) 0.0069(19) 0.0033(17) C86 0.040(2) 0.0170(19) 0.015(2) 0.0003(15) 0.0013(17) 0.0001(16) _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 U N3 2.436(2) . ? U N1 2.454(3) . ? U N2 2.468(3) . ? U O 2.483(2) . ? U N6 2.750(3) . ? U N4 2.762(3) . ? U N5 2.785(3) . ? U Si1 3.2768(10) . ? U Si3 3.2839(9) . ? U Si2 3.2843(10) . ? N1 C12 1.394(4) . ? N1 Si1 1.698(3) . ? N2 C22 1.390(4) . ? N2 Si2 1.694(3) . ? N3 C32 1.387(4) . ? N3 Si3 1.692(3) . ? N4 C6 1.486(4) . ? N4 C1 1.489(4) . ? N4 Si2 1.767(3) . ? N5 C2 1.472(4) . ? N5 C3 1.478(4) . ? N5 Si3 1.772(3) . ? N6 C4 1.477(4) . ? N6 C5 1.483(4) . ? N6 Si1 1.778(3) . ? Si1 C10 1.868(3) . ? Si1 C11 1.873(3) . ? Si2 C21 1.864(4) . ? Si2 C20 1.872(4) . ? Si3 C31 1.863(4) . ? Si3 C30 1.874(3) . ? C1 C2 1.516(5) . ? C3 C4 1.516(4) . ? C5 C6 1.518(5) . ? C12 C13 1.390(4) . ? C12 C17 1.416(5) . ? C13 C14 1.387(5) . ? C14 C15 1.372(5) . ? C15 C16 1.388(5) . ? C16 C17 1.385(5) . ? C22 C27 1.397(4) . ? C22 C23 1.425(5) . ? C23 C24 1.375(5) . ? C24 C25 1.378(5) . ? C25 C26 1.389(5) . ? C26 C27 1.368(5) . ? C32 C37 1.401(4) . ? C32 C33 1.407(4) . ? C33 C34 1.379(4) . ? C34 C35 1.385(5) . ? C35 C36 1.374(5) . ? C36 C37 1.383(4) . ? O P 1.508(2) . ? P C60 1.794(3) . ? P C40 1.795(3) . ? P C50 1.798(3) . ? C40 C45 1.388(5) . ? C40 C41 1.405(5) . ? C41 C42 1.371(5) . ? C42 C43 1.372(5) . ? C43 C44 1.377(5) . ? C44 C45 1.393(4) . ? C50 C51 1.396(5) . ? C50 C55 1.398(4) . ? C51 C52 1.378(5) . ? C52 C53 1.387(5) . ? C53 C54 1.377(5) . ? C54 C55 1.383(5) . ? C60 C65 1.387(5) . ? C60 C61 1.399(4) . ? C61 C62 1.379(4) . ? C62 C63 1.368(5) . ? C63 C64 1.383(5) . ? C64 C65 1.387(5) . ? C70 C71 1.489(6) . ? C71 C76 1.371(6) . ? C71 C72 1.389(6) . ? C72 C73 1.400(6) . ? C73 C74 1.372(7) . ? C74 C75 1.341(7) . ? C75 C76 1.360(6) . ? C80 C81 1.513(5) . ? C81 C82 1.383(5) . ? C81 C86 1.390(5) . ? C82 C83 1.384(5) . ? C83 C84 1.378(5) . ? C84 C85 1.377(5) . ? C85 C86 1.367(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U N1 117.35(9) . . ? N3 U N2 118.43(9) . . ? N1 U N2 120.56(9) . . ? N3 U O 82.69(8) . . ? N1 U O 84.36(8) . . ? N2 U O 83.79(8) . . ? N3 U N6 105.07(8) . . ? N1 U N6 60.02(9) . . ? N2 U N6 120.30(8) . . ? O U N6 143.34(8) . . ? N3 U N4 119.73(8) . . ? N1 U N4 106.83(9) . . ? N2 U N4 59.58(8) . . ? O U N4 142.61(8) . . ? N6 U N4 64.10(8) . . ? N3 U N5 59.43(8) . . ? N1 U N5 119.36(8) . . ? N2 U N5 105.42(9) . . ? O U N5 141.07(7) . . ? N6 U N5 63.51(8) . . ? N4 U N5 63.99(8) . . ? N3 U Si1 104.63(6) . . ? N1 U Si1 30.36(6) . . ? N2 U Si1 136.20(6) . . ? O U Si1 110.54(5) . . ? N6 U Si1 32.86(6) . . ? N4 U Si1 93.23(6) . . ? N5 U Si1 89.03(6) . . ? N3 U Si3 29.99(6) . . ? N1 U Si3 133.45(6) . . ? N2 U Si3 105.48(7) . . ? O U Si3 108.48(5) . . ? N6 U Si3 92.12(6) . . ? N4 U Si3 89.74(6) . . ? N5 U Si3 32.66(6) . . ? Si1 U Si3 108.16(2) . . ? N3 U Si2 134.38(6) . . ? N1 U Si2 107.57(7) . . ? N2 U Si2 30.22(6) . . ? O U Si2 110.19(5) . . ? N6 U Si2 90.08(6) . . ? N4 U Si2 32.55(6) . . ? N5 U Si2 92.47(6) . . ? Si1 U Si2 110.40(2) . . ? Si3 U Si2 109.00(2) . . ? C12 N1 Si1 125.8(2) . . ? C12 N1 U 130.8(2) . . ? Si1 N1 U 102.70(13) . . ? C22 N2 Si2 123.7(2) . . ? C22 N2 U 133.6(2) . . ? Si2 N2 U 102.62(12) . . ? C32 N3 Si3 124.5(2) . . ? C32 N3 U 131.1(2) . . ? Si3 N3 U 103.96(12) . . ? C6 N4 C1 112.8(3) . . ? C6 N4 Si2 120.3(2) . . ? C1 N4 Si2 111.1(2) . . ? C6 N4 U 115.6(2) . . ? C1 N4 U 103.83(18) . . ? Si2 N4 U 90.19(11) . . ? C2 N5 C3 112.9(3) . . ? C2 N5 Si3 120.5(2) . . ? C3 N5 Si3 111.3(2) . . ? C2 N5 U 115.2(2) . . ? C3 N5 U 104.32(19) . . ? Si3 N5 U 89.35(10) . . ? C4 N6 C5 112.4(3) . . ? C4 N6 Si1 119.1(2) . . ? C5 N6 Si1 112.0(2) . . ? C4 N6 U 116.59(18) . . ? C5 N6 U 103.80(18) . . ? Si1 N6 U 90.10(11) . . ? N1 Si1 N6 97.59(14) . . ? N1 Si1 C10 115.80(15) . . ? N6 Si1 C10 107.65(15) . . ? N1 Si1 C11 115.65(15) . . ? N6 Si1 C11 111.54(15) . . ? C10 Si1 C11 108.00(17) . . ? N1 Si1 U 46.95(10) . . ? N6 Si1 U 57.05(9) . . ? C10 Si1 U 103.83(11) . . ? C11 Si1 U 148.17(12) . . ? N2 Si2 N4 97.91(13) . . ? N2 Si2 C21 115.37(16) . . ? N4 Si2 C21 110.77(16) . . ? N2 Si2 C20 115.89(16) . . ? N4 Si2 C20 108.90(15) . . ? C21 Si2 C20 107.55(18) . . ? N2 Si2 U 47.16(9) . . ? N4 Si2 U 57.26(9) . . ? C21 Si2 U 147.65(13) . . ? C20 Si2 U 104.80(13) . . ? N3 Si3 N5 97.55(13) . . ? N3 Si3 C31 115.63(15) . . ? N5 Si3 C31 108.30(15) . . ? N3 Si3 C30 114.64(15) . . ? N5 Si3 C30 111.74(15) . . ? C31 Si3 C30 108.46(18) . . ? N3 Si3 U 46.05(8) . . ? N5 Si3 U 57.99(9) . . ? C31 Si3 U 104.12(12) . . ? C30 Si3 U 147.36(14) . . ? N4 C1 C2 114.6(3) . . ? N5 C2 C1 112.3(3) . . ? N5 C3 C4 113.7(3) . . ? N6 C4 C3 112.1(2) . . ? N6 C5 C6 114.6(3) . . ? N4 C6 C5 111.5(3) . . ? C13 C12 N1 120.5(3) . . ? C13 C12 C17 116.4(3) . . ? N1 C12 C17 123.1(3) . . ? C14 C13 C12 122.1(3) . . ? C15 C14 C13 120.9(3) . . ? C14 C15 C16 118.6(3) . . ? C17 C16 C15 121.0(3) . . ? C16 C17 C12 121.0(3) . . ? N2 C22 C27 121.4(3) . . ? N2 C22 C23 122.7(3) . . ? C27 C22 C23 115.9(3) . . ? C24 C23 C22 121.1(3) . . ? C23 C24 C25 121.4(4) . . ? C24 C25 C26 118.5(4) . . ? C27 C26 C25 120.7(4) . . ? C26 C27 C22 122.5(3) . . ? N3 C32 C37 120.5(3) . . ? N3 C32 C33 123.2(3) . . ? C37 C32 C33 116.3(3) . . ? C34 C33 C32 122.0(3) . . ? C33 C34 C35 120.1(3) . . ? C36 C35 C34 119.2(3) . . ? C35 C36 C37 120.8(3) . . ? C36 C37 C32 121.5(3) . . ? P O U 176.96(14) . . ? O P C60 112.54(14) . . ? O P C40 111.98(15) . . ? C60 P C40 106.95(15) . . ? O P C50 113.20(14) . . ? C60 P C50 105.49(15) . . ? C40 P C50 106.17(15) . . ? C45 C40 C41 119.0(3) . . ? C45 C40 P 123.2(3) . . ? C41 C40 P 117.8(2) . . ? C42 C41 C40 120.6(4) . . ? C41 C42 C43 120.2(4) . . ? C42 C43 C44 120.2(3) . . ? C43 C44 C45 120.6(4) . . ? C40 C45 C44 119.5(4) . . ? C51 C50 C55 118.4(3) . . ? C51 C50 P 119.3(2) . . ? C55 C50 P 122.3(3) . . ? C52 C51 C50 120.5(3) . . ? C51 C52 C53 120.3(3) . . ? C54 C53 C52 120.0(3) . . ? C53 C54 C55 119.9(3) . . ? C54 C55 C50 120.9(3) . . ? C65 C60 C61 119.1(3) . . ? C65 C60 P 117.8(2) . . ? C61 C60 P 123.1(3) . . ? C62 C61 C60 120.0(3) . . ? C63 C62 C61 121.0(3) . . ? C62 C63 C64 119.4(3) . . ? C63 C64 C65 120.6(3) . . ? C60 C65 C64 119.8(3) . . ? C76 C71 C72 117.4(4) . . ? C76 C71 C70 122.2(4) . . ? C72 C71 C70 120.4(4) . . ? C71 C72 C73 120.2(4) . . ? C74 C73 C72 119.4(5) . . ? C75 C74 C73 120.2(5) . . ? C74 C75 C76 120.6(5) . . ? C75 C76 C71 122.2(4) . . ? C82 C81 C86 118.6(4) . . ? C82 C81 C80 120.5(4) . . ? C86 C81 C80 120.9(4) . . ? C81 C82 C83 120.4(4) . . ? C84 C83 C82 120.4(4) . . ? C85 C84 C83 119.1(4) . . ? C86 C85 C84 120.9(4) . . ? C85 C86 C81 120.6(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 34.41 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.249 _refine_diff_density_min -1.764 _refine_diff_density_rms 0.156 #eof # End of Crystallographic Information