# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Trevor Hayton' _publ_contact_author_email HAYTON@CHEM.UCSB.EDU _publ_section_title ; U(IV) and U(V) azide complexes supported by amide or aryloxide ligands ; loop_ _publ_author_name 'Trevor Hayton' 'Skye Fortier' 'Guang Wu' # Attachment 'Allcif_azide.cif' data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 733176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lithium tris(tetrahydrofuran) Uranium(IV) tetrakis(2,6-dimethylphenoxide) bis(azide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H84 Li2 N6 O10 U' _chemical_formula_weight 1253.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 11.4965(8) _cell_length_b 22.5245(16) _cell_length_c 12.6040(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.922(2) _cell_angle_gamma 90.00 _cell_volume 2959.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 2.800 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.292 _exptl_absorpt_correction_T_max 0.595 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23433 _diffrn_reflns_av_R_equivalents 0.1679 _diffrn_reflns_av_sigmaI/netI 0.1105 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6184 _reflns_number_gt 3802 _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^)+(0.0554P)^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 6184 _refine_ls_number_parameters 354 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.029 _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 0.5000 1.0000 0.5000 0.02498(10) Uani 1 2 d S . . N2 N 0.1938(5) 1.0005(2) 0.2788(4) 0.0305(10) Uani 1 1 d . . . O1 O 0.4716(4) 1.08269(17) 0.5775(3) 0.0348(9) Uani 1 1 d . . . O2 O 0.6058(4) 1.04804(17) 0.4198(3) 0.0388(10) Uani 1 1 d . . . C2 C 0.3477(6) 1.1680(2) 0.5706(4) 0.0327(13) Uani 1 1 d . . . N1 N 0.2992(6) 1.0190(2) 0.3291(5) 0.0389(12) Uani 1 1 d . . . C1 C 0.4522(6) 1.1304(2) 0.6304(5) 0.0299(13) Uani 1 1 d . . . C6 C 0.5365(6) 1.1425(2) 0.7471(5) 0.0330(13) Uani 1 1 d . . . C9 C 0.6565(6) 1.0721(3) 0.3506(5) 0.0369(14) Uani 1 1 d . . . C5 C 0.5142(6) 1.1928(3) 0.8004(5) 0.0405(15) Uani 1 1 d . . . H5 H 0.5693 1.2014 0.8776 0.049 Uiso 1 1 calc R . . C10 C 0.6068(7) 1.1253(3) 0.2923(6) 0.0483(17) Uani 1 1 d . . . C14 C 0.7611(6) 1.0452(3) 0.3429(6) 0.0443(16) Uani 1 1 d . . . C4 C 0.4123(7) 1.2301(3) 0.7414(5) 0.0468(17) Uani 1 1 d . . . H4 H 0.3987 1.2632 0.7787 0.056 Uiso 1 1 calc R . . C7 C 0.6440(6) 1.1009(3) 0.8109(5) 0.0453(16) Uani 1 1 d . . . H7A H 0.7098 1.1059 0.7836 0.068 Uiso 1 1 calc R . . H7B H 0.6129 1.0608 0.7968 0.068 Uiso 1 1 calc R . . H7C H 0.6787 1.1091 0.8932 0.068 Uiso 1 1 calc R . . C3 C 0.3311(6) 1.2182(2) 0.6272(5) 0.0406(15) Uani 1 1 d . . . H3 H 0.2637 1.2440 0.5870 0.049 Uiso 1 1 calc R . . C13 C 0.8120(7) 1.0708(3) 0.2707(6) 0.058(2) Uani 1 1 d . . . H13 H 0.8803 1.0525 0.2625 0.069 Uiso 1 1 calc R . . C8 C 0.2575(7) 1.1551(3) 0.4465(5) 0.0467(17) Uani 1 1 d . . . H8A H 0.3052 1.1513 0.4000 0.070 Uiso 1 1 calc R . . H8B H 0.1969 1.1869 0.4166 0.070 Uiso 1 1 calc R . . H8C H 0.2126 1.1187 0.4433 0.070 Uiso 1 1 calc R . . N3 N 0.0877(6) 0.9842(3) 0.2274(6) 0.0515(15) Uani 1 1 d . . . C12 C 0.7630(9) 1.1223(4) 0.2122(7) 0.071(3) Uani 1 1 d . . . H12 H 0.7988 1.1392 0.1654 0.086 Uiso 1 1 calc R . . C11 C 0.6589(8) 1.1500(3) 0.2221(6) 0.065(2) Uani 1 1 d . . . H11 H 0.6251 1.1849 0.1815 0.078 Uiso 1 1 calc R . . C16 C 0.4960(8) 1.1542(3) 0.3085(7) 0.069(2) Uani 1 1 d . . . H16A H 0.4210 1.1297 0.2736 0.104 Uiso 1 1 calc R . . H16B H 0.4788 1.1925 0.2717 0.104 Uiso 1 1 calc R . . H16C H 0.5181 1.1587 0.3905 0.104 Uiso 1 1 calc R . . C15 C 0.8164(8) 0.9892(3) 0.4102(8) 0.064(2) Uani 1 1 d . . . H15A H 0.8422 0.9963 0.4921 0.096 Uiso 1 1 calc R . . H15B H 0.8895 0.9772 0.3972 0.096 Uiso 1 1 calc R . . H15C H 0.7527 0.9584 0.3842 0.096 Uiso 1 1 calc R . . O3 O 0.0290(5) 0.8572(2) 0.3109(4) 0.0562(13) Uani 1 1 d . . . O5 O 0.0089(6) 0.8690(2) 0.0630(4) 0.0639(15) Uani 1 1 d . . . O4 O -0.2012(5) 0.9284(2) 0.1173(5) 0.0840(17) Uani 1 1 d . . . C27 C -0.0702(8) 0.8598(3) -0.1409(6) 0.064(2) Uani 1 1 d . . . H27A H -0.0232 0.8504 -0.1871 0.077 Uiso 1 1 calc R . . H27B H -0.1485 0.8804 -0.1903 0.077 Uiso 1 1 calc R . . C26 C -0.0997(9) 0.8055(4) -0.0924(7) 0.072(2) Uani 1 1 d . . . H26A H -0.0824 0.7706 -0.1284 0.086 Uiso 1 1 calc R . . H26B H -0.1891 0.8050 -0.1056 0.086 Uiso 1 1 calc R . . C20 C 0.1608(8) 0.8399(4) 0.3744(6) 0.068(2) Uani 1 1 d . . . H20A H 0.2122 0.8733 0.4178 0.081 Uiso 1 1 calc R . . H20B H 0.1957 0.8252 0.3215 0.081 Uiso 1 1 calc R . . C18 C 0.0470(9) 0.8081(3) 0.4806(6) 0.067(2) Uani 1 1 d . . . H18A H 0.0088 0.7737 0.4998 0.080 Uiso 1 1 calc R . . H18B H 0.0716 0.8365 0.5442 0.080 Uiso 1 1 calc R . . C19 C 0.1589(8) 0.7908(3) 0.4578(6) 0.071(2) Uani 1 1 d . . . H19A H 0.1466 0.7521 0.4211 0.085 Uiso 1 1 calc R . . H19B H 0.2374 0.7906 0.5293 0.085 Uiso 1 1 calc R . . C28 C 0.0076(8) 0.8964(4) -0.0407(6) 0.071(3) Uani 1 1 d . . . H28A H 0.0943 0.8995 -0.0347 0.085 Uiso 1 1 calc R . . H28B H -0.0283 0.9361 -0.0497 0.085 Uiso 1 1 calc R . . C17 C -0.0424(9) 0.8351(4) 0.3689(8) 0.101(4) Uani 1 1 d . . . H17A H -0.1030 0.8055 0.3208 0.121 Uiso 1 1 calc R . . H17B H -0.0901 0.8670 0.3840 0.121 Uiso 1 1 calc R . . Li1 Li -0.0234(10) 0.9110(5) 0.1806(9) 0.047(3) Uani 1 1 d . . . C25 C -0.0144(11) 0.8071(4) 0.0354(8) 0.104(4) Uani 1 1 d . . . H25A H -0.0562 0.7890 0.0800 0.125 Uiso 1 1 calc R . . H25B H 0.0653 0.7862 0.0522 0.125 Uiso 1 1 calc R . . C22A C -0.3611(17) 0.9383(8) -0.0548(14) 0.082(2) Uani 0.583(16) 1 d P . . C23A C -0.3955(16) 0.8894(8) 0.0126(15) 0.082(2) Uani 0.583(16) 1 d P . . C24A C -0.305(2) 0.8848(9) 0.104(2) 0.082(2) Uani 0.583(16) 1 d P . . C23B C -0.415(2) 0.9288(10) 0.067(2) 0.076(7) Uani 0.417(16) 1 d PU . . C22B C -0.395(2) 0.9724(11) -0.019(2) 0.087(8) Uani 0.417(16) 1 d PU . . C21 C -0.2552(9) 0.9704(4) 0.0222(8) 0.082(2) Uani 1 1 d . . . C24B C -0.301(2) 0.9052(13) 0.148(2) 0.077(7) Uani 0.417(16) 1 d PU . . 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 0.01884(16) 0.02385(15) 0.03206(15) -0.00298(13) 0.01055(12) -0.00013(15) N2 0.023(3) 0.028(2) 0.033(2) 0.000(2) 0.005(2) 0.005(3) O1 0.029(2) 0.034(2) 0.036(2) -0.0061(17) 0.0091(19) 0.0044(19) O2 0.034(3) 0.038(2) 0.051(2) 0.0020(19) 0.024(2) -0.004(2) C2 0.034(4) 0.031(3) 0.036(3) -0.004(2) 0.017(3) 0.005(3) N1 0.031(3) 0.038(3) 0.045(3) -0.006(2) 0.013(3) -0.001(2) C1 0.030(3) 0.027(3) 0.039(3) -0.005(2) 0.021(3) -0.002(3) C6 0.028(4) 0.030(3) 0.045(3) -0.007(3) 0.019(3) -0.001(3) C9 0.038(4) 0.038(3) 0.041(3) -0.008(3) 0.022(3) -0.010(3) C5 0.048(4) 0.036(3) 0.034(3) -0.010(3) 0.014(3) 0.000(3) C10 0.055(5) 0.037(4) 0.065(4) 0.001(3) 0.036(4) -0.006(3) C14 0.038(4) 0.045(4) 0.058(4) -0.013(3) 0.028(4) -0.009(3) C4 0.065(5) 0.031(3) 0.049(4) -0.011(3) 0.028(4) 0.005(3) C7 0.044(4) 0.051(4) 0.036(3) -0.005(3) 0.012(3) 0.012(3) C3 0.048(4) 0.030(3) 0.042(3) 0.000(3) 0.017(3) 0.013(3) C13 0.064(6) 0.056(5) 0.075(5) -0.016(4) 0.050(5) -0.019(4) C8 0.051(5) 0.042(4) 0.041(3) -0.002(3) 0.013(3) 0.016(3) N3 0.026(4) 0.052(4) 0.062(4) 0.002(3) 0.005(3) -0.002(3) C12 0.102(8) 0.062(5) 0.077(5) -0.018(4) 0.064(6) -0.039(5) C11 0.089(7) 0.046(4) 0.078(5) 0.003(4) 0.053(5) -0.008(4) C16 0.074(7) 0.047(4) 0.102(6) 0.019(4) 0.053(6) 0.014(4) C15 0.043(5) 0.070(6) 0.093(6) 0.003(4) 0.042(5) 0.006(4) O3 0.045(3) 0.070(3) 0.052(3) 0.026(2) 0.019(2) 0.006(3) O5 0.089(5) 0.057(3) 0.041(3) 0.000(2) 0.023(3) -0.021(3) O4 0.031(3) 0.089(4) 0.112(4) 0.046(4) 0.012(3) -0.006(3) C27 0.059(6) 0.073(5) 0.058(5) -0.008(4) 0.023(4) -0.014(5) C26 0.077(7) 0.076(6) 0.073(5) -0.023(4) 0.042(5) -0.023(5) C20 0.045(5) 0.094(6) 0.057(4) 0.013(4) 0.015(4) -0.005(5) C18 0.089(7) 0.060(5) 0.053(4) 0.013(4) 0.032(5) 0.002(5) C19 0.073(7) 0.063(5) 0.060(4) 0.018(4) 0.013(4) 0.016(5) C28 0.060(6) 0.104(7) 0.044(4) 0.010(5) 0.016(4) -0.024(5) C17 0.104(8) 0.122(8) 0.113(7) 0.072(6) 0.081(7) 0.058(7) Li1 0.019(6) 0.063(7) 0.047(6) 0.019(5) 0.002(5) -0.005(5) C25 0.179(14) 0.047(5) 0.084(6) 0.000(5) 0.052(8) -0.014(6) C22A 0.060(5) 0.075(5) 0.088(5) 0.012(4) 0.010(4) -0.021(4) C23A 0.060(5) 0.075(5) 0.088(5) 0.012(4) 0.010(4) -0.021(4) C24A 0.060(5) 0.075(5) 0.088(5) 0.012(4) 0.010(4) -0.021(4) C23B 0.048(10) 0.059(13) 0.136(16) 0.035(11) 0.054(11) 0.003(9) C22B 0.059(13) 0.060(12) 0.17(2) 0.049(13) 0.076(14) 0.022(11) C21 0.060(5) 0.075(5) 0.088(5) 0.012(4) 0.010(4) -0.021(4) C24B 0.030(9) 0.116(19) 0.072(14) 0.003(10) 0.009(10) -0.050(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.169(4) . ? U1 O2 2.169(4) 3_676 ? U1 O1 2.191(4) . ? U1 O1 2.191(4) 3_676 ? U1 N1 2.442(6) 3_676 ? U1 N1 2.442(6) . ? N2 N3 1.173(8) . ? N2 N1 1.181(8) . ? O1 C1 1.333(6) . ? O2 C9 1.350(6) . ? C2 C3 1.393(7) . ? C2 C1 1.401(8) . ? C2 C8 1.496(8) . ? C1 C6 1.406(8) . ? C6 C5 1.395(7) . ? C6 C7 1.489(8) . ? C9 C14 1.387(8) . ? C9 C10 1.395(8) . ? C5 C4 1.377(8) . ? C5 H5 0.9300 . ? C10 C11 1.378(8) . ? C10 C16 1.519(9) . ? C14 C13 1.397(8) . ? C14 C15 1.504(10) . ? C4 C3 1.372(8) . ? C4 H4 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C3 H3 0.9300 . ? C13 C12 1.362(11) . ? C13 H13 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N3 Li1 2.016(13) . ? C12 C11 1.402(10) . ? C12 H12 0.9300 . ? C11 H11 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O3 C17 1.401(8) . ? O3 C20 1.437(8) . ? O3 Li1 1.923(11) . ? O5 C25 1.435(9) . ? O5 C28 1.439(8) . ? O5 Li1 1.921(12) . ? O4 C21 1.444(9) . ? O4 C24B 1.45(2) . ? O4 C24A 1.50(2) . ? O4 Li1 1.897(12) . ? C27 C28 1.457(10) . ? C27 C26 1.469(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C26 C25 1.493(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C20 C19 1.532(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C18 C17 1.479(10) . ? C18 C19 1.484(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C22A C21 1.396(16) . ? C22A C23A 1.541(18) . ? C23A C24A 1.18(2) . ? C23B C24B 1.38(3) . ? C23B C22B 1.55(2) . ? C22B C21 1.47(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O2 180.00(18) . 3_676 ? O2 U1 O1 90.10(13) . . ? O2 U1 O1 89.90(13) 3_676 . ? O2 U1 O1 89.90(13) . 3_676 ? O2 U1 O1 90.10(13) 3_676 3_676 ? O1 U1 O1 180.000(1) . 3_676 ? O2 U1 N1 89.49(17) . 3_676 ? O2 U1 N1 90.51(17) 3_676 3_676 ? O1 U1 N1 91.10(15) . 3_676 ? O1 U1 N1 88.90(15) 3_676 3_676 ? O2 U1 N1 90.51(17) . . ? O2 U1 N1 89.49(17) 3_676 . ? O1 U1 N1 88.90(15) . . ? O1 U1 N1 91.10(15) 3_676 . ? N1 U1 N1 180.000(1) 3_676 . ? N3 N2 N1 177.6(7) . . ? C1 O1 U1 175.6(3) . . ? C9 O2 U1 168.7(4) . . ? C3 C2 C1 119.1(5) . . ? C3 C2 C8 120.6(5) . . ? C1 C2 C8 120.3(5) . . ? N2 N1 U1 141.9(4) . . ? O1 C1 C2 120.2(5) . . ? O1 C1 C6 119.6(5) . . ? C2 C1 C6 120.2(5) . . ? C5 C6 C1 118.4(5) . . ? C5 C6 C7 122.1(5) . . ? C1 C6 C7 119.5(5) . . ? O2 C9 C14 119.5(5) . . ? O2 C9 C10 119.5(5) . . ? C14 C9 C10 120.9(5) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 C16 121.9(6) . . ? C9 C10 C16 118.5(5) . . ? C9 C14 C13 118.6(6) . . ? C9 C14 C15 120.0(5) . . ? C13 C14 C15 121.4(6) . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C12 C13 C14 120.9(7) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 N3 Li1 143.3(6) . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C10 C11 C12 119.8(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 O3 C20 109.0(5) . . ? C17 O3 Li1 128.9(6) . . ? C20 O3 Li1 121.5(5) . . ? C25 O5 C28 105.5(6) . . ? C25 O5 Li1 126.0(6) . . ? C28 O5 Li1 123.9(6) . . ? C21 O4 C24B 110.3(13) . . ? C21 O4 C24A 106.8(10) . . ? C24B O4 C24A 27.7(11) . . ? C21 O4 Li1 119.6(6) . . ? C24B O4 Li1 130.1(12) . . ? C24A O4 Li1 125.4(10) . . ? C28 C27 C26 106.0(6) . . ? C28 C27 H27A 110.5 . . ? C26 C27 H27A 110.5 . . ? C28 C27 H27B 110.5 . . ? C26 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C27 C26 C25 105.5(7) . . ? C27 C26 H26A 110.6 . . ? C25 C26 H26A 110.6 . . ? C27 C26 H26B 110.6 . . ? C25 C26 H26B 110.6 . . ? H26A C26 H26B 108.8 . . ? O3 C20 C19 105.1(6) . . ? O3 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O3 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? C17 C18 C19 103.6(6) . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18B 111.0 . . ? C19 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C18 C19 C20 102.0(6) . . ? C18 C19 H19A 111.4 . . ? C20 C19 H19A 111.4 . . ? C18 C19 H19B 111.4 . . ? C20 C19 H19B 111.4 . . ? H19A C19 H19B 109.2 . . ? O5 C28 C27 108.2(6) . . ? O5 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O5 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? O3 C17 C18 108.5(7) . . ? O3 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O3 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? O4 Li1 O5 107.6(6) . . ? O4 Li1 O3 112.6(5) . . ? O5 Li1 O3 104.8(6) . . ? O4 Li1 N3 113.0(6) . . ? O5 Li1 N3 108.9(5) . . ? O3 Li1 N3 109.5(6) . . ? O5 C25 C26 104.8(7) . . ? O5 C25 H25A 110.8 . . ? C26 C25 H25A 110.8 . . ? O5 C25 H25B 110.8 . . ? C26 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? C21 C22A C23A 109.8(12) . . ? C24A C23A C22A 105.9(16) . . ? C23A C24A O4 112.6(17) . . ? C24B C23B C22B 112.6(16) . . ? C21 C22B C23B 101.3(15) . . ? C22A C21 O4 100.5(9) . . ? C22A C21 C22B 42.8(11) . . ? O4 C21 C22B 109.6(10) . . ? C23B C24B O4 106.0(17) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 4.342 _refine_diff_density_min -1.796 _refine_diff_density_rms 0.148 #===========END================================= data_Complex_2 _database_code_depnum_ccdc_archive 'CCDC 733177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lithium tris(tetrahydrofuran) Uranium(IV) pentakis(2,6-dimethylphenoxide) azide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H69 Li N3 O8 U' _chemical_formula_weight 1109.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 12.5251(14) _cell_length_b 20.098(2) _cell_length_c 20.536(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5169.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 3.193 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.191 _exptl_absorpt_correction_T_max 0.293 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42047 _diffrn_reflns_av_R_equivalents 0.1611 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.10 _reflns_number_total 11085 _reflns_number_gt 7010 _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^)+(0.0411P)^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 -0.023(10) _refine_ls_number_reflns 11085 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.089 _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 O6 O 0.6414(7) 0.5791(4) 0.4325(5) 0.060(2) Uani 1 1 d . . . U1 U 0.400035(19) 0.503439(18) 0.124052(18) 0.03002(10) Uani 1 1 d . . . C14 C 0.0725(7) 0.4370(5) 0.1416(5) 0.040(2) Uani 1 1 d . . . O8 O 0.7780(5) 0.5018(5) 0.3306(4) 0.065(2) Uani 1 1 d . . . O2 O 0.2580(4) 0.4463(3) 0.1262(4) 0.0374(16) Uani 1 1 d . . . O1 O 0.3904(4) 0.5285(3) 0.0254(3) 0.0372(15) Uani 1 1 d . . . O4 O 0.5405(4) 0.5589(3) 0.1439(3) 0.0346(15) Uani 1 1 d . . . N2 N 0.4715(6) 0.4909(5) 0.2757(4) 0.043(2) Uani 1 1 d . . . O7 O 0.6221(6) 0.4169(3) 0.4253(4) 0.051(2) Uani 1 1 d . . . N1 N 0.4121(6) 0.4725(4) 0.2357(4) 0.0388(19) Uani 1 1 d . . . C15 C 0.0563(6) 0.5073(5) 0.1273(5) 0.046(2) Uani 1 1 d . . . H15A H 0.1043 0.5335 0.1532 0.069 Uiso 1 1 calc R . . H15B H -0.0160 0.5194 0.1373 0.069 Uiso 1 1 calc R . . H15C H 0.0700 0.5153 0.0820 0.069 Uiso 1 1 calc R . . O5 O 0.4951(5) 0.4201(3) 0.1033(3) 0.0429(17) Uani 1 1 d . . . C19 C 0.1063(10) 0.7134(5) 0.1325(7) 0.070(4) Uani 1 1 d . . . H19 H 0.0724 0.7376 0.0999 0.084 Uiso 1 1 calc R . . C18 C 0.1874(8) 0.6711(5) 0.1160(6) 0.047(3) Uani 1 1 d . . . N3 N 0.5258(7) 0.5097(6) 0.3169(5) 0.069(3) Uani 1 1 d . . . O3 O 0.3100(5) 0.5875(3) 0.1517(3) 0.0423(17) Uani 1 1 d . . . C25 C 0.6229(7) 0.6028(5) 0.1410(5) 0.041(3) Uani 1 1 d . . . C35 C 0.7000(9) 0.2940(5) 0.1168(9) 0.077(5) Uani 1 1 d . . . H35 H 0.7461 0.2766 0.1479 0.092 Uiso 1 1 calc R . . C31 C 0.7187(9) 0.5195(5) 0.0690(6) 0.064(4) Uani 1 1 d . . . H31A H 0.7739 0.5204 0.0365 0.096 Uiso 1 1 calc R . . H31B H 0.6516 0.5096 0.0486 0.096 Uiso 1 1 calc R . . H31C H 0.7348 0.4859 0.1007 0.096 Uiso 1 1 calc R . . C26 C 0.6158(8) 0.6613(5) 0.1760(6) 0.043(3) Uani 1 1 d . . . C34 C 0.6312(7) 0.3442(5) 0.1335(8) 0.056(3) Uani 1 1 d . . . C33 C 0.5613(7) 0.3699(4) 0.0863(6) 0.044(3) Uani 1 1 d . . . C2 C 0.2881(8) 0.5261(5) -0.0732(5) 0.044(3) Uani 1 1 d . . . C9 C 0.1743(7) 0.4093(4) 0.1403(5) 0.040(3) Uani 1 1 d . . . C8 C 0.2181(8) 0.4708(5) -0.0465(6) 0.056(3) Uani 1 1 d . . . H8A H 0.1872 0.4846 -0.0059 0.085 Uiso 1 1 calc R . . H8B H 0.2607 0.4316 -0.0396 0.085 Uiso 1 1 calc R . . H8C H 0.1623 0.4610 -0.0770 0.085 Uiso 1 1 calc R . . C17 C 0.2352(7) 0.6340(5) 0.1656(5) 0.031(2) Uani 1 1 d . . . C46 C 0.6810(10) 0.3597(6) 0.4075(9) 0.093(3) Uani 1 1 d . . . H46A H 0.7341 0.3494 0.4404 0.112 Uiso 1 1 calc R . . H46B H 0.7169 0.3666 0.3662 0.112 Uiso 1 1 calc R . . C49 C 0.8774(9) 0.4974(9) 0.3580(7) 0.102(3) Uani 1 1 d . . . H49A H 0.8970 0.4511 0.3638 0.123 Uiso 1 1 calc R . . H49B H 0.8779 0.5190 0.4002 0.123 Uiso 1 1 calc R . . C7 C 0.5196(10) 0.6333(5) -0.0159(6) 0.053(3) Uani 1 1 d . . . H7A H 0.5547 0.5980 0.0071 0.080 Uiso 1 1 calc R . . H7B H 0.4881 0.6636 0.0147 0.080 Uiso 1 1 calc R . . H7C H 0.5707 0.6567 -0.0422 0.080 Uiso 1 1 calc R . . C22 C 0.2037(7) 0.6428(4) 0.2307(5) 0.035(2) Uani 1 1 d . . . C5 C 0.4141(9) 0.6292(5) -0.1204(6) 0.059(3) Uani 1 1 d . . . H5 H 0.4573 0.6634 -0.1358 0.071 Uiso 1 1 calc R . . C28 C 0.7871(10) 0.6930(7) 0.1318(8) 0.084(4) Uani 1 1 d . . . H28 H 0.8414 0.7242 0.1271 0.101 Uiso 1 1 calc R . . C47 C 0.6026(10) 0.3054(6) 0.4023(9) 0.093(3) Uani 1 1 d . . . H47A H 0.6116 0.2817 0.3615 0.112 Uiso 1 1 calc R . . H47B H 0.6111 0.2742 0.4379 0.112 Uiso 1 1 calc R . . C30 C 0.7122(7) 0.5872(4) 0.1024(5) 0.039(2) Uani 1 1 d . . . C3 C 0.2709(8) 0.5547(6) -0.1346(6) 0.055(3) Uani 1 1 d . . . H3 H 0.2145 0.5387 -0.1596 0.067 Uiso 1 1 calc R . . C6 C 0.4334(7) 0.6046(5) -0.0591(6) 0.043(3) Uani 1 1 d . . . C38 C 0.5593(9) 0.3440(5) 0.0235(6) 0.051(3) Uani 1 1 d . . . C1 C 0.3722(7) 0.5531(4) -0.0361(5) 0.037(2) Uani 1 1 d . . . Li1 Li 0.6475(10) 0.5000(9) 0.3808(8) 0.046(3) Uani 1 1 d . . . C44 C 0.5883(10) 0.5908(6) 0.4950(7) 0.0715(19) Uani 1 1 d . . . H44A H 0.6408 0.5984 0.5289 0.086 Uiso 1 1 calc R . . H44B H 0.5456 0.5524 0.5069 0.086 Uiso 1 1 calc R . . C24 C 0.2245(9) 0.6606(5) 0.0475(6) 0.054(3) Uani 1 1 d . . . H24A H 0.3011 0.6616 0.0462 0.081 Uiso 1 1 calc R . . H24B H 0.1965 0.6951 0.0202 0.081 Uiso 1 1 calc R . . H24C H 0.1998 0.6182 0.0323 0.081 Uiso 1 1 calc R . . C21 C 0.1217(8) 0.6869(5) 0.2457(6) 0.049(3) Uani 1 1 d . . . H21 H 0.1007 0.6927 0.2888 0.059 Uiso 1 1 calc R . . C43 C 0.5177(10) 0.6515(6) 0.4870(7) 0.0715(19) Uani 1 1 d . . . H43A H 0.4435 0.6402 0.4947 0.086 Uiso 1 1 calc R . . H43B H 0.5385 0.6862 0.5173 0.086 Uiso 1 1 calc R . . C29 C 0.7944(9) 0.6335(7) 0.1010(7) 0.074(4) Uani 1 1 d . . . H29 H 0.8565 0.6235 0.0782 0.088 Uiso 1 1 calc R . . C11 C 0.0986(10) 0.3029(5) 0.1711(6) 0.055(3) Uani 1 1 d . . . H11 H 0.1072 0.2583 0.1822 0.066 Uiso 1 1 calc R . . C20 C 0.0722(11) 0.7215(6) 0.1980(7) 0.080(5) Uani 1 1 d . . . H20 H 0.0164 0.7503 0.2079 0.096 Uiso 1 1 calc R . . C10 C 0.1895(9) 0.3429(5) 0.1553(6) 0.045(3) Uani 1 1 d . . . C13 C -0.0168(8) 0.3966(5) 0.1566(6) 0.051(3) Uani 1 1 d . . . H13 H -0.0849 0.4150 0.1572 0.061 Uiso 1 1 calc R . . C37 C 0.6330(9) 0.2939(5) 0.0071(8) 0.068(4) Uani 1 1 d . . . H37 H 0.6359 0.2772 -0.0351 0.082 Uiso 1 1 calc R . . C32 C 0.5182(9) 0.6752(5) 0.2166(6) 0.055(3) Uani 1 1 d . . . H32A H 0.4562 0.6755 0.1892 0.083 Uiso 1 1 calc R . . H32B H 0.5257 0.7178 0.2373 0.083 Uiso 1 1 calc R . . H32C H 0.5107 0.6413 0.2492 0.083 Uiso 1 1 calc R . . C48 C 0.5006(10) 0.3363(6) 0.4049(9) 0.093(3) Uani 1 1 d . . . H48A H 0.4500 0.3074 0.4268 0.112 Uiso 1 1 calc R . . H48B H 0.4746 0.3449 0.3612 0.112 Uiso 1 1 calc R . . C45 C 0.5115(10) 0.3976(7) 0.4400(9) 0.093(3) Uani 1 1 d . . . H45A H 0.5011 0.3910 0.4863 0.112 Uiso 1 1 calc R . . H45B H 0.4612 0.4307 0.4245 0.112 Uiso 1 1 calc R . . C12 C -0.0029(9) 0.3313(6) 0.1698(6) 0.062(3) Uani 1 1 d . . . H12 H -0.0623 0.3049 0.1783 0.074 Uiso 1 1 calc R . . C52 C 0.7895(12) 0.5358(8) 0.2699(8) 0.102(3) Uani 1 1 d . . . H52A H 0.7282 0.5641 0.2615 0.123 Uiso 1 1 calc R . . H52B H 0.7969 0.5044 0.2343 0.123 Uiso 1 1 calc R . . C4 C 0.3336(11) 0.6056(6) -0.1602(6) 0.067(4) Uani 1 1 d . . . H4 H 0.3219 0.6227 -0.2017 0.080 Uiso 1 1 calc R . . C51 C 0.8863(11) 0.5757(8) 0.2771(8) 0.102(3) Uani 1 1 d . . . H51A H 0.9164 0.5873 0.2351 0.123 Uiso 1 1 calc R . . H51B H 0.8725 0.6161 0.3016 0.123 Uiso 1 1 calc R . . C16 C 0.3004(9) 0.3136(5) 0.1563(6) 0.057(3) Uani 1 1 d . . . H16A H 0.3324 0.3183 0.1140 0.086 Uiso 1 1 calc R . . H16B H 0.2964 0.2673 0.1674 0.086 Uiso 1 1 calc R . . H16C H 0.3430 0.3366 0.1880 0.086 Uiso 1 1 calc R . . C40 C 0.6305(10) 0.3717(6) 0.2022(7) 0.076(4) Uani 1 1 d . . . H40A H 0.5655 0.3591 0.2235 0.115 Uiso 1 1 calc R . . H40B H 0.6354 0.4194 0.2006 0.115 Uiso 1 1 calc R . . H40C H 0.6903 0.3542 0.2259 0.115 Uiso 1 1 calc R . . C50 C 0.9561(11) 0.5314(8) 0.3126(8) 0.102(3) Uani 1 1 d . . . H50A H 1.0101 0.5557 0.3366 0.123 Uiso 1 1 calc R . . H50B H 0.9905 0.4997 0.2838 0.123 Uiso 1 1 calc R . . C41 C 0.6362(9) 0.6415(6) 0.3982(7) 0.0715(19) Uani 1 1 d . . . H41A H 0.6355 0.6343 0.3515 0.086 Uiso 1 1 calc R . . H41B H 0.6968 0.6694 0.4092 0.086 Uiso 1 1 calc R . . C27 C 0.6995(11) 0.7078(6) 0.1703(8) 0.074(4) Uani 1 1 d . . . H27 H 0.6959 0.7483 0.1922 0.089 Uiso 1 1 calc R . . C23 C 0.2536(7) 0.6024(6) 0.2836(6) 0.054(3) Uani 1 1 d . . . H23A H 0.2114 0.6060 0.3224 0.082 Uiso 1 1 calc R . . H23B H 0.3244 0.6187 0.2920 0.082 Uiso 1 1 calc R . . H23C H 0.2572 0.5567 0.2703 0.082 Uiso 1 1 calc R . . C42 C 0.5330(10) 0.6733(6) 0.4205(7) 0.0715(19) Uani 1 1 d . . . H42A H 0.5382 0.7214 0.4184 0.086 Uiso 1 1 calc R . . H42B H 0.4740 0.6590 0.3933 0.086 Uiso 1 1 calc R . . C39 C 0.4808(13) 0.3683(6) -0.0251(7) 0.080(5) Uani 1 1 d . . . H39A H 0.4098 0.3623 -0.0085 0.119 Uiso 1 1 calc R . . H39B H 0.4888 0.3436 -0.0649 0.119 Uiso 1 1 calc R . . H39C H 0.4932 0.4146 -0.0335 0.119 Uiso 1 1 calc R . . C36 C 0.7015(10) 0.2694(6) 0.0548(9) 0.087(5) Uani 1 1 d . . . H36 H 0.7492 0.2357 0.0443 0.104 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 O6 0.074(6) 0.047(5) 0.058(6) 0.000(4) -0.004(5) 0.011(4) U1 0.02198(12) 0.03396(16) 0.03412(17) 0.0010(2) 0.00050(15) -0.00006(19) C14 0.035(5) 0.047(6) 0.038(7) -0.008(5) 0.005(4) -0.005(4) O8 0.043(3) 0.076(5) 0.075(5) 0.023(6) -0.005(4) 0.000(6) O2 0.027(3) 0.020(3) 0.066(5) 0.007(5) 0.005(3) -0.005(2) O1 0.027(3) 0.032(3) 0.053(4) 0.000(3) -0.003(3) -0.003(2) O4 0.032(3) 0.030(3) 0.042(4) -0.004(3) 0.001(3) -0.011(3) N2 0.031(4) 0.056(6) 0.041(5) 0.002(5) -0.004(4) 0.011(4) O7 0.046(5) 0.037(4) 0.070(6) 0.006(4) -0.008(4) 0.002(3) N1 0.030(4) 0.050(5) 0.037(5) 0.014(4) 0.009(4) 0.004(3) C15 0.035(4) 0.051(6) 0.051(5) 0.000(8) 0.015(5) -0.024(5) O5 0.054(4) 0.041(4) 0.035(4) -0.002(3) -0.007(3) 0.001(3) C19 0.083(8) 0.059(7) 0.067(9) -0.001(7) 0.014(9) 0.046(6) C18 0.042(5) 0.044(6) 0.056(8) -0.004(6) -0.013(6) 0.013(4) N3 0.049(5) 0.094(8) 0.064(6) 0.017(7) -0.019(5) -0.011(6) O3 0.039(4) 0.051(4) 0.037(4) -0.004(3) 0.003(3) -0.011(3) C25 0.035(5) 0.037(5) 0.050(7) 0.010(5) -0.007(5) -0.005(4) C35 0.038(6) 0.044(7) 0.149(16) -0.013(10) -0.014(10) 0.010(5) C31 0.051(6) 0.046(7) 0.096(10) -0.021(6) 0.038(7) -0.002(5) C26 0.041(6) 0.040(6) 0.048(7) -0.006(5) -0.004(6) -0.013(5) C34 0.026(5) 0.043(6) 0.098(11) 0.001(8) -0.008(7) -0.001(4) C33 0.040(5) 0.010(4) 0.083(9) -0.013(5) 0.019(6) -0.003(4) C2 0.038(5) 0.047(6) 0.046(7) -0.009(5) -0.007(5) 0.012(4) C9 0.039(5) 0.030(5) 0.053(8) 0.004(5) 0.006(5) -0.001(4) C8 0.034(5) 0.071(8) 0.064(8) -0.009(6) -0.013(6) 0.002(5) C17 0.029(5) 0.027(5) 0.036(7) -0.015(5) 0.003(4) 0.001(4) C46 0.063(4) 0.072(5) 0.145(8) -0.015(5) 0.006(5) -0.002(3) C49 0.067(5) 0.151(8) 0.088(6) 0.029(6) -0.004(4) -0.012(5) C7 0.071(8) 0.041(6) 0.047(8) 0.006(6) 0.009(6) -0.017(5) C22 0.036(5) 0.025(5) 0.044(6) -0.010(4) -0.003(5) 0.006(4) C5 0.079(8) 0.049(6) 0.050(7) 0.017(6) 0.001(7) -0.009(5) C28 0.050(7) 0.083(9) 0.120(13) -0.007(11) 0.003(10) -0.035(7) C47 0.063(4) 0.072(5) 0.145(8) -0.015(5) 0.006(5) -0.002(3) C30 0.032(5) 0.037(5) 0.049(7) 0.015(5) 0.001(5) 0.006(4) C3 0.054(6) 0.058(7) 0.054(9) -0.008(7) -0.023(7) 0.018(5) C6 0.037(5) 0.037(6) 0.055(8) 0.002(5) -0.005(5) 0.004(4) C38 0.054(6) 0.033(6) 0.066(9) -0.007(6) 0.021(6) 0.005(5) C1 0.039(5) 0.034(5) 0.038(6) 0.008(4) 0.000(4) 0.004(4) Li1 0.050(7) 0.039(7) 0.048(9) -0.008(14) -0.002(8) -0.006(9) C44 0.075(4) 0.057(4) 0.082(5) 0.012(4) 0.003(4) 0.010(3) C24 0.063(7) 0.043(7) 0.057(9) -0.005(6) -0.002(6) 0.017(6) C21 0.053(7) 0.049(6) 0.046(7) 0.001(5) 0.012(5) 0.020(5) C43 0.075(4) 0.057(4) 0.082(5) 0.012(4) 0.003(4) 0.010(3) C29 0.040(6) 0.081(9) 0.099(12) 0.007(8) 0.019(7) -0.019(6) C11 0.066(7) 0.039(6) 0.060(8) 0.008(5) 0.005(7) -0.011(6) C20 0.096(11) 0.074(9) 0.071(10) -0.007(8) 0.007(8) 0.065(8) C10 0.046(6) 0.044(6) 0.046(7) 0.010(5) -0.002(6) -0.012(5) C13 0.043(6) 0.051(7) 0.059(8) 0.001(6) 0.003(5) -0.008(5) C37 0.055(7) 0.041(7) 0.109(12) -0.011(7) 0.034(7) -0.001(5) C32 0.061(7) 0.045(7) 0.061(8) -0.012(6) 0.000(6) 0.003(5) C48 0.063(4) 0.072(5) 0.145(8) -0.015(5) 0.006(5) -0.002(3) C45 0.063(4) 0.072(5) 0.145(8) -0.015(5) 0.006(5) -0.002(3) C12 0.047(7) 0.066(8) 0.072(9) 0.021(7) 0.009(6) -0.019(6) C52 0.067(5) 0.151(8) 0.088(6) 0.029(6) -0.004(4) -0.012(5) C4 0.102(10) 0.064(8) 0.035(7) 0.010(6) -0.018(7) 0.013(7) C51 0.067(5) 0.151(8) 0.088(6) 0.029(6) -0.004(4) -0.012(5) C16 0.054(7) 0.043(6) 0.075(9) 0.004(6) 0.019(7) -0.004(5) C40 0.070(9) 0.063(8) 0.096(13) 0.000(8) -0.035(8) 0.020(7) C50 0.067(5) 0.151(8) 0.088(6) 0.029(6) -0.004(4) -0.012(5) C41 0.075(4) 0.057(4) 0.082(5) 0.012(4) 0.003(4) 0.010(3) C27 0.070(9) 0.050(7) 0.103(12) -0.015(7) -0.014(9) -0.015(7) C23 0.050(7) 0.061(8) 0.052(9) 0.008(7) 0.015(5) 0.015(5) C42 0.075(4) 0.057(4) 0.082(5) 0.012(4) 0.003(4) 0.010(3) C39 0.125(14) 0.068(9) 0.045(9) -0.012(7) 0.013(9) 0.025(9) C36 0.034(6) 0.052(8) 0.175(17) -0.014(10) 0.015(9) 0.007(6) _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 O6 C41 1.441(13) . ? O6 C44 1.463(15) . ? O6 Li1 1.912(19) . ? U1 O1 2.092(7) . ? U1 O5 2.098(6) . ? U1 O3 2.109(7) . ? U1 O2 2.118(5) . ? U1 O4 2.122(5) . ? U1 N1 2.381(8) . ? C14 C9 1.392(12) . ? C14 C13 1.415(13) . ? C14 C15 1.457(13) . ? O8 C49 1.368(13) . ? O8 C52 1.430(15) . ? O8 Li1 1.933(16) . ? O2 C9 1.317(10) . ? O1 C1 1.375(11) . ? O4 C25 1.361(10) . ? N2 N3 1.150(11) . ? N2 N1 1.168(10) . ? O7 C46 1.415(14) . ? O7 C45 1.470(14) . ? O7 Li1 1.931(19) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O5 C33 1.353(10) . ? C19 C18 1.367(13) . ? C19 C20 1.420(18) . ? C19 H19 0.9300 . ? C18 C17 1.395(14) . ? C18 C24 1.497(16) . ? N3 Li1 2.021(17) . ? O3 C17 1.355(11) . ? C25 C26 1.380(14) . ? C25 C30 1.405(13) . ? C35 C36 1.36(2) . ? C35 C34 1.370(15) . ? C35 H35 0.9300 . ? C31 C30 1.527(13) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C26 C27 1.411(15) . ? C26 C32 1.505(15) . ? C34 C33 1.405(17) . ? C34 C40 1.51(2) . ? C33 C38 1.391(16) . ? C2 C3 1.402(15) . ? C2 C1 1.408(13) . ? C2 C8 1.519(14) . ? C9 C10 1.382(13) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C17 C22 1.406(14) . ? C46 C47 1.471(16) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C49 C50 1.518(18) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C7 C6 1.511(15) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C22 C21 1.392(12) . ? C22 C23 1.492(14) . ? C5 C6 1.373(15) . ? C5 C4 1.383(16) . ? C5 H5 0.9300 . ? C28 C29 1.356(17) . ? C28 C27 1.38(2) . ? C28 H28 0.9300 . ? C47 C48 1.422(16) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C30 C29 1.389(14) . ? C3 C4 1.394(16) . ? C3 H3 0.9300 . ? C6 C1 1.372(13) . ? C38 C37 1.407(14) . ? C38 C39 1.484(17) . ? C44 C43 1.517(15) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C21 C20 1.351(16) . ? C21 H21 0.9300 . ? C43 C42 1.447(18) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C29 H29 0.9300 . ? C11 C12 1.395(16) . ? C11 C10 1.431(15) . ? C11 H11 0.9300 . ? C20 H20 0.9300 . ? C10 C16 1.509(16) . ? C13 C12 1.352(15) . ? C13 H13 0.9300 . ? C37 C36 1.392(19) . ? C37 H37 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C48 C45 1.433(17) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C12 H12 0.9300 . ? C52 C51 1.462(18) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C4 H4 0.9300 . ? C51 C50 1.445(19) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C41 C42 1.512(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C27 H27 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C36 H36 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 O6 C44 105.6(9) . . ? C41 O6 Li1 117.0(9) . . ? C44 O6 Li1 129.6(9) . . ? O1 U1 O5 91.6(2) . . ? O1 U1 O3 92.1(2) . . ? O5 U1 O3 175.8(3) . . ? O1 U1 O2 95.9(3) . . ? O5 U1 O2 92.8(2) . . ? O3 U1 O2 88.8(2) . . ? O1 U1 O4 96.2(2) . . ? O5 U1 O4 89.3(2) . . ? O3 U1 O4 88.3(2) . . ? O2 U1 O4 167.7(3) . . ? O1 U1 N1 178.8(2) . . ? O5 U1 N1 87.2(3) . . ? O3 U1 N1 89.0(3) . . ? O2 U1 N1 83.8(3) . . ? O4 U1 N1 84.2(3) . . ? C9 C14 C13 119.9(9) . . ? C9 C14 C15 120.8(8) . . ? C13 C14 C15 119.4(8) . . ? C49 O8 C52 107.3(10) . . ? C49 O8 Li1 123.3(8) . . ? C52 O8 Li1 124.0(9) . . ? C9 O2 U1 168.3(8) . . ? C1 O1 U1 170.4(6) . . ? C25 O4 U1 164.1(6) . . ? N3 N2 N1 176.7(9) . . ? C46 O7 C45 109.2(9) . . ? C46 O7 Li1 119.7(9) . . ? C45 O7 Li1 118.7(8) . . ? N2 N1 U1 129.4(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C33 O5 U1 175.0(6) . . ? C18 C19 C20 121.9(12) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C18 C17 118.0(12) . . ? C19 C18 C24 123.5(11) . . ? C17 C18 C24 118.4(9) . . ? N2 N3 Li1 153.2(12) . . ? C17 O3 U1 168.5(6) . . ? O4 C25 C26 118.7(9) . . ? O4 C25 C30 118.9(9) . . ? C26 C25 C30 122.4(9) . . ? C36 C35 C34 120.6(15) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C26 C27 118.2(11) . . ? C25 C26 C32 120.0(9) . . ? C27 C26 C32 121.7(10) . . ? C35 C34 C33 119.3(15) . . ? C35 C34 C40 120.4(13) . . ? C33 C34 C40 120.3(10) . . ? O5 C33 C38 120.5(10) . . ? O5 C33 C34 118.6(11) . . ? C38 C33 C34 120.9(10) . . ? C3 C2 C1 116.3(10) . . ? C3 C2 C8 122.4(10) . . ? C1 C2 C8 121.2(10) . . ? O2 C9 C10 118.9(8) . . ? O2 C9 C14 120.5(8) . . ? C10 C9 C14 120.6(8) . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C17 C18 120.9(9) . . ? O3 C17 C22 118.7(9) . . ? C18 C17 C22 120.4(9) . . ? O7 C46 C47 105.9(10) . . ? O7 C46 H46A 110.6 . . ? C47 C46 H46A 110.6 . . ? O7 C46 H46B 110.6 . . ? C47 C46 H46B 110.6 . . ? H46A C46 H46B 108.7 . . ? O8 C49 C50 108.0(11) . . ? O8 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? O8 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C21 C22 C17 119.8(9) . . ? C21 C22 C23 119.6(9) . . ? C17 C22 C23 120.5(9) . . ? C6 C5 C4 123.2(10) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C29 C28 C27 120.7(11) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C48 C47 C46 105.9(11) . . ? C48 C47 H47A 110.6 . . ? C46 C47 H47A 110.6 . . ? C48 C47 H47B 110.6 . . ? C46 C47 H47B 110.6 . . ? H47A C47 H47B 108.7 . . ? C29 C30 C25 116.9(10) . . ? C29 C30 C31 123.2(10) . . ? C25 C30 C31 119.7(8) . . ? C4 C3 C2 123.6(10) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C5 C6 C1 119.3(10) . . ? C5 C6 C7 121.7(10) . . ? C1 C6 C7 119.0(10) . . ? C33 C38 C37 118.6(12) . . ? C33 C38 C39 120.8(10) . . ? C37 C38 C39 120.6(12) . . ? O1 C1 C6 119.7(9) . . ? O1 C1 C2 118.8(8) . . ? C6 C1 C2 121.5(10) . . ? O6 Li1 O7 116.7(9) . . ? O6 Li1 O8 108.3(9) . . ? O7 Li1 O8 114.1(9) . . ? O6 Li1 N3 104.5(9) . . ? O7 Li1 N3 105.5(8) . . ? O8 Li1 N3 106.9(8) . . ? O6 C44 C43 107.4(10) . . ? O6 C44 H44A 110.2 . . ? C43 C44 H44A 110.2 . . ? O6 C44 H44B 110.2 . . ? C43 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C21 C22 120.4(10) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C42 C43 C44 105.6(11) . . ? C42 C43 H43A 110.6 . . ? C44 C43 H43A 110.6 . . ? C42 C43 H43B 110.6 . . ? C44 C43 H43B 110.6 . . ? H43A C43 H43B 108.8 . . ? C28 C29 C30 122.1(11) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C12 C11 C10 119.4(10) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C21 C20 C19 119.4(10) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C9 C10 C11 118.9(10) . . ? C9 C10 C16 120.4(9) . . ? C11 C10 C16 120.6(9) . . ? C12 C13 C14 120.0(10) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C36 C37 C38 119.2(14) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C47 C48 C45 108.0(12) . . ? C47 C48 H48A 110.1 . . ? C45 C48 H48A 110.1 . . ? C47 C48 H48B 110.1 . . ? C45 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? C48 C45 O7 102.4(11) . . ? C48 C45 H45A 111.3 . . ? O7 C45 H45A 111.3 . . ? C48 C45 H45B 111.3 . . ? O7 C45 H45B 111.3 . . ? H45A C45 H45B 109.2 . . ? C13 C12 C11 121.2(10) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? O8 C52 C51 104.9(12) . . ? O8 C52 H52A 110.8 . . ? C51 C52 H52A 110.8 . . ? O8 C52 H52B 110.8 . . ? C51 C52 H52B 110.8 . . ? H52A C52 H52B 108.9 . . ? C5 C4 C3 116.1(10) . . ? C5 C4 H4 122.0 . . ? C3 C4 H4 122.0 . . ? C50 C51 C52 102.4(13) . . ? C50 C51 H51A 111.3 . . ? C52 C51 H51A 111.3 . . ? C50 C51 H51B 111.3 . . ? C52 C51 H51B 111.3 . . ? H51A C51 H51B 109.2 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C51 C50 C49 101.2(12) . . ? C51 C50 H50A 111.5 . . ? C49 C50 H50A 111.5 . . ? C51 C50 H50B 111.5 . . ? C49 C50 H50B 111.5 . . ? H50A C50 H50B 109.3 . . ? O6 C41 C42 105.0(10) . . ? O6 C41 H41A 110.7 . . ? C42 C41 H41A 110.7 . . ? O6 C41 H41B 110.7 . . ? C42 C41 H41B 110.7 . . ? H41A C41 H41B 108.8 . . ? C28 C27 C26 119.6(12) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C43 C42 C41 105.7(11) . . ? C43 C42 H42A 110.6 . . ? C41 C42 H42A 110.6 . . ? C43 C42 H42B 110.6 . . ? C41 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C36 C37 121.3(12) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.252 _refine_diff_density_min -1.478 _refine_diff_density_rms 0.144 #================================END======================================== data_c:Complex_2 _database_code_depnum_ccdc_archive 'CCDC 733178' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Sodium tetrakis(tetrahydrofuran) Uranium(IV) tris(hexamethyldisilazide) bis(azide) ; _chemical_name_common ; Sodium tetrakis(tetrahydrofuran) Uranium(IV) tris(hexamethyldisilazide) bis(azide) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H86 N9 Na O4 Si6 U' _chemical_formula_weight 1114.68 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 19.4247(13) _cell_length_b 11.8336(8) _cell_length_c 25.3187(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.369(2) _cell_angle_gamma 90.00 _cell_volume 5637.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min 8.901 _cell_measurement_theta_max 19.258 _exptl_crystal_description rod _exptl_crystal_colour pink _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 3.053 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.147 _exptl_absorpt_correction_T_max 0.432 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23319 _diffrn_reflns_av_R_equivalents 0.1600 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5716 _reflns_number_gt 4793 _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^)+(0.0594P)^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 5716 _refine_ls_number_parameters 242 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.5000 0.77012(2) 0.7500 0.03292(13) Uani 1 2 d S . . Si1 Si 0.60132(9) 0.71968(15) 0.65661(8) 0.0447(4) Uani 1 1 d . . . Si2 Si 0.63028(7) 0.56625(14) 0.75344(7) 0.0418(4) Uani 1 1 d . . . Si3 Si 0.57770(8) 1.03429(15) 0.77784(9) 0.0505(5) Uani 1 1 d . . . Na Na 0.7500 0.7500 1.0000 0.0804(15) Uani 1 2 d S . . N1 N 0.5742(3) 0.7680(4) 0.8381(2) 0.0474(13) Uani 1 1 d . . . N4 N 0.5836(2) 0.6786(4) 0.71718(18) 0.0348(10) Uani 1 1 d . . . N2 N 0.6233(3) 0.7752(5) 0.8760(2) 0.0504(14) Uani 1 1 d . . . C5 C 0.5830(3) 0.5005(6) 0.8014(3) 0.0577(18) Uani 1 1 d . . . H5A H 0.5605 0.5585 0.8178 0.087 Uiso 1 1 calc R . . H5B H 0.6164 0.4603 0.8293 0.087 Uiso 1 1 calc R . . H5C H 0.5476 0.4490 0.7818 0.087 Uiso 1 1 calc R . . N5 N 0.5000 0.9621(5) 0.7500 0.0410(16) Uani 1 2 d S . . C1 C 0.6992(4) 0.7182(6) 0.6588(4) 0.062(2) Uani 1 1 d . . . H1A H 0.7244 0.7646 0.6883 0.094 Uiso 1 1 calc R . . H1B H 0.7061 0.7470 0.6250 0.094 Uiso 1 1 calc R . . H1C H 0.7167 0.6421 0.6640 0.094 Uiso 1 1 calc R . . C7 C 0.6580(3) 0.9445(6) 0.7803(3) 0.0547(17) Uani 1 1 d . . . H7A H 0.6850 0.9370 0.8174 0.082 Uiso 1 1 calc R . . H7B H 0.6868 0.9794 0.7591 0.082 Uiso 1 1 calc R . . H7C H 0.6432 0.8711 0.7656 0.082 Uiso 1 1 calc R . . C3 C 0.5726(4) 0.8692(6) 0.6376(3) 0.0579(18) Uani 1 1 d . . . H3A H 0.5270 0.8824 0.6447 0.087 Uiso 1 1 calc R . . H3B H 0.5695 0.8809 0.5995 0.087 Uiso 1 1 calc R . . H3C H 0.6068 0.9206 0.6588 0.087 Uiso 1 1 calc R . . C4 C 0.6434(3) 0.4492(6) 0.7074(3) 0.0580(18) Uani 1 1 d . . . H4A H 0.5983 0.4162 0.6902 0.087 Uiso 1 1 calc R . . H4B H 0.6738 0.3926 0.7284 0.087 Uiso 1 1 calc R . . H4C H 0.6650 0.4787 0.6801 0.087 Uiso 1 1 calc R . . C6 C 0.7191(3) 0.6130(6) 0.7955(3) 0.0543(17) Uani 1 1 d . . . H6A H 0.7446 0.6506 0.7725 0.081 Uiso 1 1 calc R . . H6B H 0.7457 0.5483 0.8121 0.081 Uiso 1 1 calc R . . H6C H 0.7127 0.6640 0.8233 0.081 Uiso 1 1 calc R . . O1 O 0.8464(4) 0.6996(9) 0.9609(3) 0.126(3) Uani 1 1 d . . . C2 C 0.5529(4) 0.6278(7) 0.5986(3) 0.066(2) Uani 1 1 d . . . H2A H 0.5700 0.5516 0.6046 0.099 Uiso 1 1 calc R . . H2B H 0.5612 0.6555 0.5650 0.099 Uiso 1 1 calc R . . H2C H 0.5029 0.6295 0.5965 0.099 Uiso 1 1 calc R . . N3 N 0.6722(4) 0.7868(8) 0.9116(3) 0.101(3) Uani 1 1 d . . . C8 C 0.5902(3) 1.1607(6) 0.7364(4) 0.081(3) Uani 1 1 d . . . H8A H 0.5888 1.1374 0.6998 0.122 Uiso 1 1 calc R . . H8B H 0.6353 1.1951 0.7524 0.122 Uiso 1 1 calc R . . H8C H 0.5529 1.2143 0.7357 0.122 Uiso 1 1 calc R . . C9 C 0.5834(4) 1.0835(7) 0.8484(3) 0.080(3) Uani 1 1 d . . . H9A H 0.5508 1.1449 0.8475 0.120 Uiso 1 1 calc R . . H9B H 0.6309 1.1087 0.8647 0.120 Uiso 1 1 calc R . . H9C H 0.5715 1.0225 0.8695 0.120 Uiso 1 1 calc R . . C10 C 0.8616(7) 0.7519(10) 0.9157(5) 0.118(5) Uani 1 1 d . . . H10A H 0.8398 0.8262 0.9098 0.142 Uiso 1 1 calc R . . H10B H 0.8444 0.7068 0.8831 0.142 Uiso 1 1 calc R . . C11 C 0.9415(7) 0.7611(11) 0.9295(6) 0.117(4) Uani 1 1 d . . . H11A H 0.9590 0.7597 0.8968 0.140 Uiso 1 1 calc R . . H11B H 0.9574 0.8302 0.9494 0.140 Uiso 1 1 calc R . . C12 C 0.9650(7) 0.6639(13) 0.9627(6) 0.153(4) Uani 1 1 d . . . H12A H 1.0066 0.6819 0.9916 0.183 Uiso 1 1 calc R . . H12B H 0.9770 0.6030 0.9409 0.183 Uiso 1 1 calc R . . C13 C 0.9067(6) 0.6313(13) 0.9851(6) 0.153(4) Uani 1 1 d . . . H13A H 0.8955 0.5521 0.9776 0.183 Uiso 1 1 calc R . . H13B H 0.9195 0.6420 1.0243 0.183 Uiso 1 1 calc R . . O2 O 0.7163(7) 0.5612(10) 0.9973(4) 0.207(4) Uani 1 1 d DU . . C14 C 0.7371(9) 0.4635(13) 1.0274(7) 0.207(4) Uani 1 1 d DU . . H14A H 0.7437 0.4750 1.0663 0.249 Uiso 1 1 calc R . . H14B H 0.7792 0.4292 1.0202 0.249 Uiso 1 1 calc R . . C16 C 0.6794(13) 0.3874(14) 0.9463(6) 0.325(10) Uani 1 1 d DU . . H16A H 0.6380 0.3590 0.9199 0.390 Uiso 1 1 calc R . . H16B H 0.7220 0.3466 0.9443 0.390 Uiso 1 1 calc R . . C17 C 0.6870(14) 0.5124(15) 0.9465(6) 0.307(7) Uani 1 1 d DU . . H17A H 0.7164 0.5325 0.9220 0.368 Uiso 1 1 calc R . . H17B H 0.6404 0.5453 0.9318 0.368 Uiso 1 1 calc R . . C15 C 0.6697(10) 0.3992(17) 1.0018(7) 0.307(7) Uani 1 1 d DU . . H15A H 0.6681 0.3264 1.0191 0.368 Uiso 1 1 calc R . . H15B H 0.6274 0.4423 1.0024 0.368 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 0.02404(15) 0.0322(2) 0.04191(19) 0.000 0.00695(11) 0.000 Si1 0.0434(8) 0.0436(11) 0.0498(10) 0.0023(8) 0.0169(8) 0.0047(7) Si2 0.0316(7) 0.0370(9) 0.0561(10) 0.0034(8) 0.0097(7) 0.0052(6) Si3 0.0373(8) 0.0331(9) 0.0842(14) -0.0072(9) 0.0211(9) -0.0078(7) Na 0.050(2) 0.141(5) 0.041(2) 0.012(2) -0.0054(19) -0.008(2) N1 0.037(3) 0.050(3) 0.053(3) 0.001(2) 0.008(3) -0.004(2) N4 0.030(2) 0.031(3) 0.045(3) -0.001(2) 0.0103(18) 0.0015(18) N2 0.042(3) 0.067(4) 0.037(3) 0.005(2) -0.001(2) 0.000(2) C5 0.042(3) 0.050(4) 0.079(5) 0.019(4) 0.012(3) 0.008(3) N5 0.031(3) 0.029(4) 0.065(4) 0.000 0.014(3) 0.000 C1 0.055(4) 0.059(5) 0.085(6) 0.003(4) 0.039(4) 0.005(3) C7 0.029(3) 0.050(4) 0.089(5) 0.002(4) 0.023(3) -0.010(3) C3 0.067(4) 0.052(4) 0.063(4) 0.016(3) 0.032(4) 0.004(3) C4 0.048(3) 0.039(4) 0.087(5) -0.006(3) 0.018(3) 0.003(3) C6 0.036(3) 0.057(4) 0.064(4) 0.002(3) 0.001(3) 0.010(3) O1 0.091(5) 0.197(9) 0.098(6) 0.048(6) 0.041(4) 0.028(5) C2 0.079(5) 0.066(5) 0.054(4) -0.008(4) 0.020(4) 0.007(4) N3 0.080(5) 0.141(8) 0.066(5) 0.009(5) -0.016(4) 0.003(5) C8 0.053(4) 0.038(4) 0.158(8) 0.024(5) 0.037(5) 0.001(3) C9 0.063(4) 0.079(6) 0.095(6) -0.047(5) 0.016(4) -0.024(4) C10 0.095(8) 0.195(15) 0.067(7) 0.021(6) 0.024(6) -0.003(7) C11 0.095(8) 0.148(12) 0.101(10) 0.024(7) 0.011(7) 0.010(7) C12 0.141(8) 0.157(10) 0.183(9) 0.061(8) 0.085(7) 0.054(7) C13 0.141(8) 0.157(10) 0.183(9) 0.061(8) 0.085(7) 0.054(7) O2 0.230(7) 0.208(9) 0.140(7) 0.082(6) -0.039(6) -0.067(8) C14 0.230(7) 0.208(9) 0.140(7) 0.082(6) -0.039(6) -0.067(8) C16 0.53(2) 0.215(13) 0.153(10) 0.077(10) -0.069(14) -0.100(19) C17 0.421(14) 0.242(12) 0.188(8) 0.061(9) -0.055(11) -0.150(12) C15 0.421(14) 0.242(12) 0.188(8) 0.061(9) -0.055(11) -0.150(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N5 2.272(7) . ? U1 N4 2.274(4) . ? U1 N4 2.274(4) 6_657 ? U1 N1 2.337(6) . ? U1 N1 2.337(6) 6_657 ? U1 Si3 3.4669(17) 6_657 ? Si1 N4 1.723(5) . ? Si1 C2 1.881(7) . ? Si1 C3 1.881(7) . ? Si1 C1 1.888(7) . ? Si2 N4 1.738(5) . ? Si2 C5 1.865(7) . ? Si2 C4 1.867(7) . ? Si2 C6 1.872(6) . ? Si3 N5 1.725(4) . ? Si3 C9 1.856(8) . ? Si3 C7 1.876(6) . ? Si3 C8 1.878(7) . ? Na O2 2.324(11) . ? Na O2 2.324(11) 7_667 ? Na O1 2.401(7) . ? Na O1 2.401(7) 7_667 ? Na N3 2.408(8) . ? Na N3 2.408(8) 7_667 ? N1 N2 1.175(7) . ? N2 N3 1.146(9) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? N5 Si3 1.725(4) 6_657 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O1 C10 1.395(13) . ? O1 C13 1.430(12) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.509(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.431(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.440(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O2 C14 1.389(9) . ? O2 C17 1.396(9) . ? C14 C15 1.514(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C15 1.469(10) . ? C16 C17 1.487(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? 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 N5 U1 N4 118.45(12) . . ? N5 U1 N4 118.45(12) . 6_657 ? N4 U1 N4 123.1(2) . 6_657 ? N5 U1 N1 90.61(13) . . ? N4 U1 N1 90.97(17) . . ? N4 U1 N1 88.45(17) 6_657 . ? N5 U1 N1 90.61(13) . 6_657 ? N4 U1 N1 88.45(16) . 6_657 ? N4 U1 N1 90.97(17) 6_657 6_657 ? N1 U1 N1 178.8(3) . 6_657 ? N5 U1 Si3 25.62(3) . 6_657 ? N4 U1 Si3 132.03(12) . 6_657 ? N4 U1 Si3 100.92(12) 6_657 6_657 ? N1 U1 Si3 109.75(13) . 6_657 ? N1 U1 Si3 71.42(13) 6_657 6_657 ? N4 Si1 C2 111.1(3) . . ? N4 Si1 C3 112.4(3) . . ? C2 Si1 C3 106.5(3) . . ? N4 Si1 C1 113.2(3) . . ? C2 Si1 C1 108.8(4) . . ? C3 Si1 C1 104.4(3) . . ? N4 Si2 C5 112.7(2) . . ? N4 Si2 C4 111.8(3) . . ? C5 Si2 C4 105.2(3) . . ? N4 Si2 C6 111.1(3) . . ? C5 Si2 C6 106.7(3) . . ? C4 Si2 C6 108.9(3) . . ? N5 Si3 C9 112.7(2) . . ? N5 Si3 C7 111.6(3) . . ? C9 Si3 C7 107.2(4) . . ? N5 Si3 C8 112.8(3) . . ? C9 Si3 C8 107.6(4) . . ? C7 Si3 C8 104.4(3) . . ? O2 Na O2 180.0(5) . 7_667 ? O2 Na O1 89.5(4) . . ? O2 Na O1 90.5(4) 7_667 . ? O2 Na O1 90.5(4) . 7_667 ? O2 Na O1 89.5(4) 7_667 7_667 ? O1 Na O1 180.000(3) . 7_667 ? O2 Na N3 92.2(3) . . ? O2 Na N3 87.8(3) 7_667 . ? O1 Na N3 92.0(3) . . ? O1 Na N3 88.0(3) 7_667 . ? O2 Na N3 87.8(3) . 7_667 ? O2 Na N3 92.2(3) 7_667 7_667 ? O1 Na N3 88.0(3) . 7_667 ? O1 Na N3 92.0(3) 7_667 7_667 ? N3 Na N3 180.000(3) . 7_667 ? N2 N1 U1 163.9(5) . . ? Si1 N4 Si2 119.5(2) . . ? Si1 N4 U1 120.6(2) . . ? Si2 N4 U1 119.8(2) . . ? N3 N2 N1 176.7(8) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 N5 Si3 120.6(4) . 6_657 ? Si3 N5 U1 119.7(2) . . ? Si3 N5 U1 119.7(2) 6_657 . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 O1 C13 106.6(9) . . ? C10 O1 Na 125.0(8) . . ? C13 O1 Na 127.0(7) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 N3 Na 156.6(7) . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 104.8(11) . . ? O1 C10 H10A 110.8 . . ? C11 C10 H10A 110.8 . . ? O1 C10 H10B 110.8 . . ? C11 C10 H10B 110.8 . . ? H10A C10 H10B 108.9 . . ? C12 C11 C10 103.7(11) . . ? C12 C11 H11A 111.0 . . ? C10 C11 H11A 111.0 . . ? C12 C11 H11B 111.0 . . ? C10 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? C11 C12 C13 106.3(10) . . ? C11 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? C11 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? O1 C13 C12 108.6(10) . . ? O1 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? O1 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.3 . . ? C14 O2 C17 99.2(11) . . ? C14 O2 Na 138.0(9) . . ? C17 O2 Na 118.2(9) . . ? O2 C14 C15 94.6(11) . . ? O2 C14 H14A 112.8 . . ? C15 C14 H14A 112.8 . . ? O2 C14 H14B 112.8 . . ? C15 C14 H14B 112.8 . . ? H14A C14 H14B 110.3 . . ? C15 C16 C17 86.5(12) . . ? C15 C16 H16A 114.2 . . ? C17 C16 H16A 114.3 . . ? C15 C16 H16B 114.3 . . ? C17 C16 H16B 114.2 . . ? H16A C16 H16B 111.4 . . ? O2 C17 C16 115.5(12) . . ? O2 C17 H17A 108.4 . . ? C16 C17 H17A 108.5 . . ? O2 C17 H17B 108.3 . . ? C16 C17 H17B 108.3 . . ? H17A C17 H17B 107.5 . . ? C16 C15 C14 98.9(13) . . ? C16 C15 H15A 112.0 . . ? C14 C15 H15A 112.0 . . ? C16 C15 H15B 112.0 . . ? C14 C15 H15B 112.0 . . ? H15A C15 H15B 109.7 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.781 _refine_diff_density_min -1.811 _refine_diff_density_rms 0.145 #============================END============================ data_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 733179' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Uranium(V) tris(hexamethyldisilazide) bis(azide) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H68 N9 Si6 U' _chemical_formula_weight 889.44 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7670(10) _cell_length_b 14.6497(8) _cell_length_c 16.8791(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.295(2) _cell_angle_gamma 90.00 _cell_volume 4323.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 3.946 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.323 _exptl_absorpt_correction_T_max 0.470 _exptl_absorpt_process_details 'Psi Scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17620 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.73 _reflns_number_total 4513 _reflns_number_gt 4016 _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^)+(0.0303P)^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 4513 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.028 _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 0.5000 0.816434(10) 0.7500 0.03184(6) Uani 1 2 d S . . Si2 Si 0.69497(5) 0.84912(7) 0.83321(6) 0.0449(2) Uani 1 1 d . . . Si1 Si 0.60261(5) 0.97329(6) 0.68782(6) 0.0461(2) Uani 1 1 d . . . Si3 Si 0.53154(5) 0.60583(6) 0.67940(7) 0.0494(2) Uani 1 1 d . . . N4 N 0.60549(13) 0.88266(16) 0.75761(15) 0.0365(5) Uani 1 1 d . . . N1 N 0.46020(15) 0.81563(18) 0.60864(17) 0.0433(6) Uani 1 1 d . . . N2 N 0.43516(16) 0.81107(18) 0.53312(18) 0.0459(7) Uani 1 1 d . . . C6 C 0.69210(17) 0.7324(2) 0.8756(2) 0.0494(8) Uani 1 1 d . . . H6A H 0.6708 0.7353 0.9194 0.074 Uiso 1 1 calc R . . H6B H 0.7430 0.7082 0.8989 0.074 Uiso 1 1 calc R . . H6C H 0.6610 0.6936 0.8305 0.074 Uiso 1 1 calc R . . N3 N 0.4112(3) 0.8060(3) 0.4611(2) 0.0798(12) Uani 1 1 d . . . N5 N 0.5000 0.6684(2) 0.7500 0.0371(8) Uani 1 2 d S . . C7 C 0.5988(2) 0.6725(3) 0.6445(3) 0.0663(11) Uani 1 1 d . . . H7A H 0.5746 0.7281 0.6180 0.099 Uiso 1 1 calc R . . H7B H 0.6129 0.6372 0.6045 0.099 Uiso 1 1 calc R . . H7C H 0.6438 0.6867 0.6929 0.099 Uiso 1 1 calc R . . C2 C 0.5055(2) 1.0258(3) 0.6465(3) 0.0655(11) Uani 1 1 d . . . H2A H 0.4807 1.0107 0.5875 0.098 Uiso 1 1 calc R . . H2B H 0.5101 1.0909 0.6527 0.098 Uiso 1 1 calc R . . H2C H 0.4758 1.0028 0.6780 0.098 Uiso 1 1 calc R . . C3 C 0.6695(2) 1.0667(2) 0.7425(3) 0.0653(11) Uani 1 1 d . . . H3A H 0.6570 1.0888 0.7894 0.098 Uiso 1 1 calc R . . H3B H 0.6651 1.1157 0.7032 0.098 Uiso 1 1 calc R . . H3C H 0.7210 1.0440 0.7631 0.098 Uiso 1 1 calc R . . C4 C 0.7683(2) 0.8424(3) 0.7829(3) 0.0705(12) Uani 1 1 d . . . H4A H 0.7539 0.7961 0.7396 0.106 Uiso 1 1 calc R . . H4B H 0.8170 0.8273 0.8253 0.106 Uiso 1 1 calc R . . H4C H 0.7718 0.9002 0.7578 0.106 Uiso 1 1 calc R . . C1 C 0.6264(2) 0.9336(3) 0.5957(2) 0.0688(11) Uani 1 1 d . . . H1A H 0.6767 0.9074 0.6158 0.103 Uiso 1 1 calc R . . H1B H 0.6250 0.9845 0.5593 0.103 Uiso 1 1 calc R . . H1C H 0.5898 0.8886 0.5645 0.103 Uiso 1 1 calc R . . C8 C 0.4497(2) 0.5701(3) 0.5831(3) 0.0680(11) Uani 1 1 d . . . H8A H 0.4118 0.5403 0.6000 0.102 Uiso 1 1 calc R . . H8B H 0.4674 0.5286 0.5502 0.102 Uiso 1 1 calc R . . H8C H 0.4275 0.6228 0.5494 0.102 Uiso 1 1 calc R . . C9 C 0.5876(2) 0.5034(3) 0.7321(3) 0.0787(14) Uani 1 1 d . . . H9A H 0.6323 0.5223 0.7787 0.118 Uiso 1 1 calc R . . H9B H 0.6026 0.4699 0.6918 0.118 Uiso 1 1 calc R . . H9C H 0.5567 0.4651 0.7529 0.118 Uiso 1 1 calc R . . C5 C 0.7248(2) 0.9300(3) 0.9252(2) 0.0670(12) Uani 1 1 d . . . H5A H 0.7339 0.9892 0.9064 0.101 Uiso 1 1 calc R . . H5B H 0.7707 0.9081 0.9684 0.101 Uiso 1 1 calc R . . H5C H 0.6849 0.9342 0.9481 0.101 Uiso 1 1 calc R . . C11 C 0.6561(6) 0.6898(5) 0.4321(6) 0.136(3) Uani 1 1 d . . . H11A H 0.6496 0.6571 0.4790 0.163 Uiso 1 1 calc R . . H11B H 0.6765 0.6467 0.4022 0.163 Uiso 1 1 calc R . . C10 C 0.7115(5) 0.7583(5) 0.4666(5) 0.150(4) Uani 1 1 d . . . H10A H 0.6873 0.8047 0.4893 0.180 Uiso 1 1 calc R . . H10B H 0.7206 0.7860 0.4190 0.180 Uiso 1 1 calc R . . C12 C 0.5806(6) 0.7175(6) 0.3742(7) 0.184(4) Uani 1 1 d . . . H12A H 0.5755 0.7825 0.3772 0.277 Uiso 1 1 calc R . . H12B H 0.5422 0.6880 0.3901 0.277 Uiso 1 1 calc R . . H12C H 0.5744 0.7004 0.3172 0.277 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 0.02371(8) 0.03535(9) 0.03254(9) 0.000 0.00555(6) 0.000 Si2 0.0263(4) 0.0479(5) 0.0496(5) 0.0148(4) 0.0006(4) -0.0080(3) Si1 0.0407(5) 0.0474(5) 0.0422(5) 0.0149(4) 0.0057(4) -0.0076(4) Si3 0.0325(4) 0.0440(5) 0.0713(7) -0.0118(5) 0.0184(4) 0.0041(4) N4 0.0311(12) 0.0379(13) 0.0342(13) 0.0074(11) 0.0043(10) -0.0020(10) N1 0.0367(14) 0.0525(16) 0.0358(15) -0.0010(12) 0.0072(11) -0.0006(11) N2 0.0434(15) 0.0514(17) 0.0371(18) 0.0008(12) 0.0076(13) -0.0053(12) C6 0.0307(15) 0.051(2) 0.058(2) 0.0144(17) 0.0060(14) -0.0031(14) N3 0.092(3) 0.099(3) 0.0357(19) 0.0006(18) 0.0085(18) -0.017(2) N5 0.0217(15) 0.0376(19) 0.050(2) 0.000 0.0103(15) 0.000 C7 0.043(2) 0.080(3) 0.085(3) -0.021(2) 0.033(2) 0.0032(18) C2 0.055(2) 0.055(2) 0.074(3) 0.029(2) 0.0090(19) 0.0023(17) C3 0.061(2) 0.051(2) 0.067(2) 0.0201(19) 0.0042(19) -0.0162(17) C4 0.0333(18) 0.078(3) 0.098(3) 0.034(2) 0.022(2) -0.0034(17) C1 0.074(3) 0.083(3) 0.050(2) 0.019(2) 0.024(2) -0.011(2) C8 0.054(2) 0.064(2) 0.082(3) -0.032(2) 0.020(2) 0.0024(18) C9 0.051(2) 0.055(2) 0.125(4) -0.009(3) 0.026(2) 0.0155(18) C5 0.058(2) 0.057(2) 0.054(2) 0.0090(18) -0.0179(18) -0.0122(17) C11 0.207(10) 0.105(5) 0.130(7) -0.020(5) 0.101(7) -0.008(5) C10 0.242(12) 0.097(5) 0.131(7) -0.041(6) 0.092(7) -0.003(7) C12 0.203(10) 0.105(5) 0.217(11) 0.001(7) 0.042(9) 0.067(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N4 2.166(2) . ? U1 N4 2.166(2) 2_656 ? U1 N5 2.168(3) . ? U1 N1 2.226(3) 2_656 ? U1 N1 2.226(3) . ? U1 Si1 3.3997(9) 2_656 ? U1 Si3 3.4355(9) 2_656 ? U1 Si2 3.4435(8) 2_656 ? Si2 N4 1.770(2) . ? Si2 C6 1.862(3) . ? Si2 C4 1.864(4) . ? Si2 C5 1.870(4) . ? Si1 N4 1.763(2) . ? Si1 C1 1.859(4) . ? Si1 C3 1.861(4) . ? Si1 C2 1.864(4) . ? Si3 N5 1.7674(19) . ? Si3 C7 1.854(4) . ? Si3 C8 1.861(4) . ? Si3 C9 1.863(4) . ? N1 N2 1.190(4) . ? N2 N3 1.136(5) . ? N5 Si3 1.7674(19) 2_656 ? C11 C10 1.411(11) . ? C11 C12 1.456(12) . ? C10 C10 1.494(16) 7_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 U1 N4 126.78(13) . 2_656 ? N4 U1 N5 116.61(6) . . ? N4 U1 N5 116.61(7) 2_656 . ? N4 U1 N1 89.73(9) . 2_656 ? N4 U1 N1 90.55(9) 2_656 2_656 ? N5 U1 N1 89.70(7) . 2_656 ? N4 U1 N1 90.55(9) . . ? N4 U1 N1 89.73(9) 2_656 . ? N5 U1 N1 89.70(7) . . ? N1 U1 N1 179.40(13) 2_656 . ? N4 U1 Si1 106.67(7) . 2_656 ? N4 U1 Si1 26.83(6) 2_656 2_656 ? N5 U1 Si1 132.523(18) . 2_656 ? N1 U1 Si1 71.33(7) 2_656 2_656 ? N1 U1 Si1 109.10(7) . 2_656 ? N4 U1 Si3 130.59(6) . 2_656 ? N4 U1 Si3 98.85(7) 2_656 2_656 ? N5 U1 Si3 26.092(18) . 2_656 ? N1 U1 Si3 69.91(7) 2_656 2_656 ? N1 U1 Si3 109.51(7) . 2_656 ? Si1 U1 Si3 108.16(2) 2_656 2_656 ? N4 U1 Si2 140.78(6) . 2_656 ? N4 U1 Si2 25.93(6) 2_656 2_656 ? N5 U1 Si2 97.993(17) . 2_656 ? N1 U1 Si2 109.33(7) 2_656 2_656 ? N1 U1 Si2 70.76(7) . 2_656 ? Si1 U1 Si2 52.76(2) 2_656 2_656 ? Si3 U1 Si2 88.56(2) 2_656 2_656 ? N4 Si2 C6 112.32(13) . . ? N4 Si2 C4 110.50(16) . . ? C6 Si2 C4 104.82(18) . . ? N4 Si2 C5 109.99(15) . . ? C6 Si2 C5 107.70(17) . . ? C4 Si2 C5 111.4(2) . . ? N4 Si1 C1 111.41(16) . . ? N4 Si1 C3 111.80(14) . . ? C1 Si1 C3 108.7(2) . . ? N4 Si1 C2 110.45(15) . . ? C1 Si1 C2 108.3(2) . . ? C3 Si1 C2 105.91(19) . . ? N5 Si3 C7 112.01(16) . . ? N5 Si3 C8 111.25(13) . . ? C7 Si3 C8 108.2(2) . . ? N5 Si3 C9 111.43(18) . . ? C7 Si3 C9 104.2(2) . . ? C8 Si3 C9 109.5(2) . . ? Si1 N4 Si2 118.79(14) . . ? Si1 N4 U1 119.49(12) . . ? Si2 N4 U1 121.71(12) . . ? N2 N1 U1 175.5(2) . . ? N3 N2 N1 179.5(4) . . ? Si3 N5 Si3 117.49(19) . 2_656 ? Si3 N5 U1 121.25(10) . . ? Si3 N5 U1 121.25(10) 2_656 . ? C10 C11 C12 118.1(8) . . ? C11 C10 C10 124.2(10) . 7_666 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.540 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.085