# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gaunt@lanl.gov _publ_contact_author_name 'Gaunt, Andrew' loop_ _publ_author_name 'Andrew Gaunt' 'Enrique Batista' 'Trevor Hayton' 'Iain May' 'Brian Scott' 'Sean Reilly' 'Guang Wu' 'David Schnaars' data_e:\xray\ds-5-17\work\ds_5_17m _database_code_depnum_ccdc_archive 'CCDC 824025' #TrackingRef '- Compound 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H64 Cl2 N2 O2 U' _chemical_formula_weight 1130.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2220(16) _cell_length_b 11.5941(18) _cell_length_c 12.512(2) _cell_angle_alpha 76.814(2) _cell_angle_beta 80.226(2) _cell_angle_gamma 65.223(2) _cell_volume 1306.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Deep_Orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _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_000 568 _exptl_absorpt_coefficient_mu 3.251 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.44207 _exptl_absorpt_correction_T_max 0.50696 _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 10501 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.36 _reflns_number_total 5108 _reflns_number_gt 4762 _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^)+(0.0375P)^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 5108 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2827(3) 0.5059(3) 0.5451(2) 0.0247(7) Uani 1 1 d . . . U1 U 0.5000 0.5000 0.5000 0.02859(11) Uani 1 2 d S . . Cl1 Cl 0.57230(12) 0.32309(11) 0.37658(10) 0.0329(3) Uani 1 1 d . . . N1 N 0.3388(4) 0.6711(3) 0.3758(3) 0.0205(8) Uani 1 1 d . . . C5 C 0.5579(4) 0.8624(4) 0.2486(4) 0.0217(10) Uani 1 1 d . . . C1 C 0.4348(5) 0.7177(4) 0.3016(4) 0.0221(10) Uani 1 1 d . . . C6 C 0.4598(4) 0.8206(4) 0.3196(4) 0.0215(10) Uani 1 1 d . . . H6 H 0.4110 0.8614 0.3792 0.026 Uiso 1 1 calc R . . C15 C 0.1981(5) 0.7394(4) 0.3830(3) 0.0217(10) Uani 1 1 d . . . C24 C 0.0421(4) 0.5398(4) 0.6149(3) 0.0207(10) Uani 1 1 d . . . C23 C 0.1458(4) 0.5843(4) 0.5382(4) 0.0210(10) Uani 1 1 d . . . C3 C 0.6101(4) 0.6923(4) 0.1436(4) 0.0217(10) Uani 1 1 d . . . C2 C 0.5129(4) 0.6527(4) 0.2161(4) 0.0220(10) Uani 1 1 d . . . H2 H 0.4996 0.5809 0.2074 0.026 Uiso 1 1 calc R . . C22 C 0.1056(5) 0.6962(4) 0.4638(4) 0.0230(10) Uani 1 1 d . . . H22 H 0.0077 0.7497 0.4663 0.028 Uiso 1 1 calc R . . C25 C -0.1065(5) 0.6114(5) 0.6215(4) 0.0249(10) Uani 1 1 d . . . H25 H -0.1447 0.6918 0.5769 0.030 Uiso 1 1 calc R . . C29 C 0.0950(5) 0.4210(4) 0.6830(4) 0.0266(11) Uani 1 1 d . . . H29 H 0.1941 0.3717 0.6798 0.032 Uiso 1 1 calc R . . C4 C 0.6280(5) 0.7996(4) 0.1612(4) 0.0241(10) Uani 1 1 d . . . H4 H 0.6901 0.8299 0.1117 0.029 Uiso 1 1 calc R . . C17 C 0.1633(5) 0.8784(5) 0.1948(4) 0.0311(12) Uani 1 1 d . . . H17 H 0.2289 0.8082 0.1634 0.037 Uiso 1 1 calc R . . C27 C -0.1436(5) 0.4466(5) 0.7610(4) 0.0270(11) Uani 1 1 d . . . H27 H -0.2061 0.4163 0.8101 0.032 Uiso 1 1 calc R . . C16 C 0.1296(5) 0.8642(4) 0.3077(4) 0.0261(11) Uani 1 1 d . . . C7 C 0.6890(5) 0.6214(5) 0.0475(4) 0.0279(11) Uani 1 1 d . . . C26 C -0.1964(5) 0.5646(5) 0.6928(4) 0.0309(12) Uani 1 1 d . . . H26 H -0.2956 0.6132 0.6954 0.037 Uiso 1 1 calc R . . C11 C 0.5834(5) 0.9751(4) 0.2725(4) 0.0286(11) Uani 1 1 d . . . C28 C 0.0037(5) 0.3741(5) 0.7556(4) 0.0320(12) Uani 1 1 d . . . H28 H 0.0411 0.2939 0.8006 0.038 Uiso 1 1 calc R . . C8 C 0.5749(5) 0.6375(5) -0.0266(4) 0.0347(12) Uani 1 1 d . . . H8A H 0.5097 0.6002 0.0148 0.052 Uiso 1 1 calc R . . H8B H 0.6220 0.5946 -0.0882 0.052 Uiso 1 1 calc R . . H8C H 0.5219 0.7276 -0.0526 0.052 Uiso 1 1 calc R . . C13 C 0.4386(5) 1.0891(5) 0.2863(4) 0.0367(13) Uani 1 1 d . . . H13A H 0.3865 1.1114 0.2225 0.055 Uiso 1 1 calc R . . H13B H 0.4558 1.1618 0.2945 0.055 Uiso 1 1 calc R . . H13C H 0.3827 1.0657 0.3506 0.055 Uiso 1 1 calc R . . C14 C 0.6790(6) 1.0202(5) 0.1812(5) 0.0402(13) Uani 1 1 d . . . H14A H 0.7740 0.9528 0.1776 0.060 Uiso 1 1 calc R . . H14B H 0.6851 1.0953 0.1963 0.060 Uiso 1 1 calc R . . H14C H 0.6384 1.0411 0.1121 0.060 Uiso 1 1 calc R . . C10 C 0.7704(5) 0.4778(5) 0.0925(4) 0.0413(13) Uani 1 1 d . . . H10A H 0.8389 0.4682 0.1412 0.062 Uiso 1 1 calc R . . H10B H 0.8205 0.4330 0.0324 0.062 Uiso 1 1 calc R . . H10C H 0.7028 0.4423 0.1321 0.062 Uiso 1 1 calc R . . C18 C 0.0990(5) 0.9972(5) 0.1286(5) 0.0426(14) Uani 1 1 d . . . H18 H 0.1219 1.0059 0.0528 0.051 Uiso 1 1 calc R . . C9 C 0.7967(5) 0.6737(5) -0.0212(4) 0.0390(13) Uani 1 1 d . . . H9A H 0.7475 0.7642 -0.0482 0.059 Uiso 1 1 calc R . . H9B H 0.8395 0.6291 -0.0823 0.059 Uiso 1 1 calc R . . H9C H 0.8708 0.6609 0.0235 0.059 Uiso 1 1 calc R . . C21 C 0.0278(6) 0.9698(5) 0.3514(5) 0.0392(13) Uani 1 1 d . . . H21 H 0.0001 0.9613 0.4265 0.047 Uiso 1 1 calc R . . C12 C 0.6587(6) 0.9313(5) 0.3791(4) 0.0397(13) Uani 1 1 d . . . H12A H 0.6014 0.9004 0.4378 0.060 Uiso 1 1 calc R . . H12B H 0.6699 1.0027 0.3970 0.060 Uiso 1 1 calc R . . H12C H 0.7521 0.8632 0.3693 0.060 Uiso 1 1 calc R . . C19 C 0.0027(6) 1.1016(6) 0.1726(5) 0.0503(16) Uani 1 1 d . . . H19 H -0.0382 1.1812 0.1274 0.060 Uiso 1 1 calc R . . C20 C -0.0327(6) 1.0880(5) 0.2833(6) 0.0512(16) Uani 1 1 d . . . H20 H -0.0985 1.1589 0.3137 0.061 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 O1 0.0184(16) 0.0242(17) 0.0293(18) -0.0020(14) -0.0022(14) -0.0074(14) U1 0.01995(15) 0.02841(17) 0.03779(18) -0.00940(12) -0.00104(11) -0.00863(12) Cl1 0.0297(6) 0.0288(7) 0.0413(7) -0.0148(6) -0.0027(6) -0.0084(5) N1 0.021(2) 0.022(2) 0.020(2) -0.0079(17) 0.0049(16) -0.0111(17) C5 0.019(2) 0.016(2) 0.025(3) 0.001(2) -0.006(2) -0.0027(19) C1 0.022(2) 0.020(2) 0.021(2) 0.000(2) -0.005(2) -0.006(2) C6 0.022(2) 0.019(2) 0.019(2) -0.005(2) -0.0022(19) -0.003(2) C15 0.025(2) 0.022(2) 0.019(2) -0.006(2) -0.0021(19) -0.008(2) C24 0.019(2) 0.026(3) 0.020(2) -0.008(2) -0.0033(19) -0.009(2) C23 0.019(2) 0.025(3) 0.021(2) -0.008(2) -0.0007(19) -0.008(2) C3 0.018(2) 0.023(3) 0.022(2) -0.006(2) -0.0003(19) -0.006(2) C2 0.021(2) 0.018(2) 0.025(3) -0.006(2) -0.003(2) -0.005(2) C22 0.016(2) 0.024(3) 0.026(3) -0.008(2) -0.0005(19) -0.004(2) C25 0.023(2) 0.026(3) 0.023(3) -0.001(2) -0.001(2) -0.009(2) C29 0.018(2) 0.029(3) 0.029(3) -0.002(2) -0.004(2) -0.007(2) C4 0.017(2) 0.029(3) 0.022(3) 0.003(2) -0.0011(19) -0.009(2) C17 0.021(2) 0.035(3) 0.033(3) 0.000(2) -0.001(2) -0.011(2) C27 0.029(3) 0.035(3) 0.025(3) -0.014(2) 0.005(2) -0.019(2) C16 0.024(2) 0.026(3) 0.031(3) -0.003(2) -0.005(2) -0.012(2) C7 0.027(3) 0.028(3) 0.029(3) -0.005(2) 0.000(2) -0.013(2) C26 0.018(2) 0.036(3) 0.038(3) -0.013(3) 0.003(2) -0.008(2) C11 0.034(3) 0.019(3) 0.034(3) -0.002(2) -0.004(2) -0.013(2) C28 0.034(3) 0.030(3) 0.029(3) 0.003(2) -0.006(2) -0.014(2) C8 0.042(3) 0.035(3) 0.029(3) -0.009(2) 0.001(2) -0.017(3) C13 0.039(3) 0.020(3) 0.049(3) -0.006(2) -0.005(3) -0.010(2) C14 0.041(3) 0.027(3) 0.055(4) -0.011(3) 0.005(3) -0.017(3) C10 0.037(3) 0.032(3) 0.041(3) -0.013(3) 0.002(3) 0.001(2) C18 0.029(3) 0.046(4) 0.044(3) 0.010(3) -0.004(3) -0.016(3) C9 0.031(3) 0.057(4) 0.034(3) -0.023(3) 0.014(2) -0.021(3) C21 0.042(3) 0.030(3) 0.041(3) -0.011(3) 0.000(3) -0.009(3) C12 0.042(3) 0.038(3) 0.048(3) -0.011(3) -0.010(3) -0.021(3) C19 0.036(3) 0.036(4) 0.068(5) 0.019(3) -0.014(3) -0.015(3) C20 0.045(3) 0.024(3) 0.074(5) -0.013(3) -0.003(3) -0.001(3) _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 O1 C23 1.316(5) . ? O1 U1 2.173(3) . ? U1 O1 2.173(3) 2_666 ? U1 N1 2.406(3) . ? U1 N1 2.406(3) 2_666 ? U1 Cl1 2.6315(12) . ? U1 Cl1 2.6315(12) 2_666 ? U1 C1 3.045(4) . ? U1 C1 3.045(4) 2_666 ? N1 C15 1.318(5) . ? N1 C1 1.423(5) . ? C5 C4 1.377(6) . ? C5 C6 1.392(6) . ? C5 C11 1.535(6) . ? C1 C2 1.387(6) . ? C1 C6 1.392(6) . ? C6 H6 0.9300 . ? C15 C22 1.418(6) . ? C15 C16 1.491(6) . ? C24 C29 1.383(6) . ? C24 C25 1.391(6) . ? C24 C23 1.483(6) . ? C23 C22 1.360(6) . ? C3 C2 1.380(6) . ? C3 C4 1.401(6) . ? C3 C7 1.528(6) . ? C2 H2 0.9300 . ? C22 H22 0.9300 . ? C25 C26 1.362(6) . ? C25 H25 0.9300 . ? C29 C28 1.380(6) . ? C29 H29 0.9300 . ? C4 H4 0.9300 . ? C17 C16 1.385(6) . ? C17 C18 1.386(7) . ? C17 H17 0.9300 . ? C27 C26 1.377(7) . ? C27 C28 1.381(6) . ? C27 H27 0.9300 . ? C16 C21 1.387(7) . ? C7 C9 1.523(7) . ? C7 C10 1.533(7) . ? C7 C8 1.537(6) . ? C26 H26 0.9300 . ? C11 C14 1.521(7) . ? C11 C12 1.530(6) . ? C11 C13 1.532(7) . ? C28 H28 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C18 C19 1.363(8) . ? C18 H18 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C21 C20 1.386(7) . ? C21 H21 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C19 C20 1.362(8) . ? C19 H19 0.9300 . ? C20 H20 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 C23 O1 U1 141.9(3) . . ? O1 U1 O1 180.000(1) . 2_666 ? O1 U1 N1 71.19(11) . . ? O1 U1 N1 108.81(11) 2_666 . ? O1 U1 N1 108.81(11) . 2_666 ? O1 U1 N1 71.19(11) 2_666 2_666 ? N1 U1 N1 180.00(14) . 2_666 ? O1 U1 Cl1 93.57(8) . . ? O1 U1 Cl1 86.43(8) 2_666 . ? N1 U1 Cl1 95.36(8) . . ? N1 U1 Cl1 84.64(8) 2_666 . ? O1 U1 Cl1 86.43(8) . 2_666 ? O1 U1 Cl1 93.57(8) 2_666 2_666 ? N1 U1 Cl1 84.64(8) . 2_666 ? N1 U1 Cl1 95.36(8) 2_666 2_666 ? Cl1 U1 Cl1 180.00(4) . 2_666 ? O1 U1 C1 98.32(11) . . ? O1 U1 C1 81.68(11) 2_666 . ? N1 U1 C1 27.16(11) . . ? N1 U1 C1 152.84(11) 2_666 . ? Cl1 U1 C1 92.47(9) . . ? Cl1 U1 C1 87.53(9) 2_666 . ? O1 U1 C1 81.68(11) . 2_666 ? O1 U1 C1 98.32(11) 2_666 2_666 ? N1 U1 C1 152.84(11) . 2_666 ? N1 U1 C1 27.16(11) 2_666 2_666 ? Cl1 U1 C1 87.53(9) . 2_666 ? Cl1 U1 C1 92.47(9) 2_666 2_666 ? C1 U1 C1 180.0 . 2_666 ? C15 N1 C1 121.5(4) . . ? C15 N1 U1 133.3(3) . . ? C1 N1 U1 102.3(2) . . ? C4 C5 C6 118.4(4) . . ? C4 C5 C11 123.4(4) . . ? C6 C5 C11 118.2(4) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 N1 119.3(4) . . ? C6 C1 N1 120.5(4) . . ? C2 C1 U1 101.9(3) . . ? C6 C1 U1 111.3(3) . . ? N1 C1 U1 50.51(19) . . ? C1 C6 C5 120.0(4) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? N1 C15 C22 120.7(4) . . ? N1 C15 C16 122.1(4) . . ? C22 C15 C16 117.3(4) . . ? C29 C24 C25 118.1(4) . . ? C29 C24 C23 118.6(4) . . ? C25 C24 C23 123.2(4) . . ? O1 C23 C22 121.2(4) . . ? O1 C23 C24 115.1(4) . . ? C22 C23 C24 123.8(4) . . ? C2 C3 C4 117.1(4) . . ? C2 C3 C7 119.7(4) . . ? C4 C3 C7 123.2(4) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C23 C22 C15 126.5(4) . . ? C23 C22 H22 116.8 . . ? C15 C22 H22 116.8 . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C28 C29 C24 121.2(4) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C5 C4 C3 123.0(4) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C16 C17 C18 119.9(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C26 C27 C28 119.0(5) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C17 C16 C21 118.5(4) . . ? C17 C16 C15 122.2(4) . . ? C21 C16 C15 119.3(4) . . ? C9 C7 C3 112.8(4) . . ? C9 C7 C10 108.7(4) . . ? C3 C7 C10 109.2(4) . . ? C9 C7 C8 108.7(4) . . ? C3 C7 C8 107.8(4) . . ? C10 C7 C8 109.6(4) . . ? C25 C26 C27 121.4(4) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C14 C11 C12 107.8(4) . . ? C14 C11 C13 108.6(4) . . ? C12 C11 C13 109.2(4) . . ? C14 C11 C5 112.3(4) . . ? C12 C11 C5 109.0(4) . . ? C13 C11 C5 110.0(4) . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C19 C18 C17 121.2(5) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C20 C21 C16 120.2(5) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C20 C19 C18 119.2(5) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 O1 U1 O1 99(100) . . . 2_666 ? C23 O1 U1 N1 -24.6(4) . . . . ? C23 O1 U1 N1 155.4(4) . . . 2_666 ? C23 O1 U1 Cl1 -119.1(4) . . . . ? C23 O1 U1 Cl1 60.9(4) . . . 2_666 ? C23 O1 U1 C1 -26.1(4) . . . . ? C23 O1 U1 C1 153.9(4) . . . 2_666 ? O1 U1 N1 C15 22.9(4) . . . . ? O1 U1 N1 C15 -157.1(4) 2_666 . . . ? N1 U1 N1 C15 -153(100) 2_666 . . . ? Cl1 U1 N1 C15 114.9(4) . . . . ? Cl1 U1 N1 C15 -65.1(4) 2_666 . . . ? C1 U1 N1 C15 -160.2(5) . . . . ? C1 U1 N1 C15 19.8(5) 2_666 . . . ? O1 U1 N1 C1 -176.9(3) . . . . ? O1 U1 N1 C1 3.1(3) 2_666 . . . ? N1 U1 N1 C1 7(100) 2_666 . . . ? Cl1 U1 N1 C1 -84.9(2) . . . . ? Cl1 U1 N1 C1 95.1(2) 2_666 . . . ? C1 U1 N1 C1 180.0 2_666 . . . ? C15 N1 C1 C2 -115.8(5) . . . . ? U1 N1 C1 C2 81.1(4) . . . . ? C15 N1 C1 C6 69.8(5) . . . . ? U1 N1 C1 C6 -93.4(4) . . . . ? C15 N1 C1 U1 163.2(4) . . . . ? O1 U1 C1 C2 -115.3(3) . . . . ? O1 U1 C1 C2 64.7(3) 2_666 . . . ? N1 U1 C1 C2 -118.3(4) . . . . ? N1 U1 C1 C2 61.7(4) 2_666 . . . ? Cl1 U1 C1 C2 -21.4(3) . . . . ? Cl1 U1 C1 C2 158.6(3) 2_666 . . . ? C1 U1 C1 C2 72(100) 2_666 . . . ? O1 U1 C1 C6 115.7(3) . . . . ? O1 U1 C1 C6 -64.3(3) 2_666 . . . ? N1 U1 C1 C6 112.7(4) . . . . ? N1 U1 C1 C6 -67.3(4) 2_666 . . . ? Cl1 U1 C1 C6 -150.4(3) . . . . ? Cl1 U1 C1 C6 29.6(3) 2_666 . . . ? C1 U1 C1 C6 -57(100) 2_666 . . . ? O1 U1 C1 N1 3.0(3) . . . . ? O1 U1 C1 N1 -177.0(3) 2_666 . . . ? N1 U1 C1 N1 180.000(1) 2_666 . . . ? Cl1 U1 C1 N1 96.9(2) . . . . ? Cl1 U1 C1 N1 -83.1(2) 2_666 . . . ? C1 U1 C1 N1 -170(100) 2_666 . . . ? C2 C1 C6 C5 3.3(6) . . . . ? N1 C1 C6 C5 177.7(4) . . . . ? U1 C1 C6 C5 121.9(3) . . . . ? C4 C5 C6 C1 0.1(6) . . . . ? C11 C5 C6 C1 -179.3(4) . . . . ? C1 N1 C15 C22 -174.7(4) . . . . ? U1 N1 C15 C22 -17.5(6) . . . . ? C1 N1 C15 C16 5.2(6) . . . . ? U1 N1 C15 C16 162.4(3) . . . . ? U1 O1 C23 C22 18.3(7) . . . . ? U1 O1 C23 C24 -162.8(3) . . . . ? C29 C24 C23 O1 -2.2(6) . . . . ? C25 C24 C23 O1 178.3(4) . . . . ? C29 C24 C23 C22 176.6(4) . . . . ? C25 C24 C23 C22 -2.9(7) . . . . ? C4 C3 C2 C1 1.0(6) . . . . ? C7 C3 C2 C1 -177.3(4) . . . . ? C6 C1 C2 C3 -3.8(6) . . . . ? N1 C1 C2 C3 -178.3(4) . . . . ? U1 C1 C2 C3 -127.2(4) . . . . ? O1 C23 C22 C15 3.7(7) . . . . ? C24 C23 C22 C15 -175.0(4) . . . . ? N1 C15 C22 C23 -1.8(7) . . . . ? C16 C15 C22 C23 178.3(4) . . . . ? C29 C24 C25 C26 -0.3(6) . . . . ? C23 C24 C25 C26 179.2(4) . . . . ? C25 C24 C29 C28 0.0(7) . . . . ? C23 C24 C29 C28 -179.5(4) . . . . ? C6 C5 C4 C3 -3.0(6) . . . . ? C11 C5 C4 C3 176.3(4) . . . . ? C2 C3 C4 C5 2.5(6) . . . . ? C7 C3 C4 C5 -179.3(4) . . . . ? C18 C17 C16 C21 2.0(7) . . . . ? C18 C17 C16 C15 -178.5(4) . . . . ? N1 C15 C16 C17 47.0(6) . . . . ? C22 C15 C16 C17 -133.1(5) . . . . ? N1 C15 C16 C21 -133.6(5) . . . . ? C22 C15 C16 C21 46.3(6) . . . . ? C2 C3 C7 C9 -177.5(4) . . . . ? C4 C3 C7 C9 4.2(6) . . . . ? C2 C3 C7 C10 -56.6(5) . . . . ? C4 C3 C7 C10 125.2(5) . . . . ? C2 C3 C7 C8 62.4(5) . . . . ? C4 C3 C7 C8 -115.8(4) . . . . ? C24 C25 C26 C27 0.8(7) . . . . ? C28 C27 C26 C25 -0.9(7) . . . . ? C4 C5 C11 C14 7.4(6) . . . . ? C6 C5 C11 C14 -173.3(4) . . . . ? C4 C5 C11 C12 -111.9(5) . . . . ? C6 C5 C11 C12 67.4(5) . . . . ? C4 C5 C11 C13 128.5(5) . . . . ? C6 C5 C11 C13 -52.2(5) . . . . ? C24 C29 C28 C27 -0.1(7) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C16 C17 C18 C19 0.2(7) . . . . ? C17 C16 C21 C20 -3.2(7) . . . . ? C15 C16 C21 C20 177.4(5) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C16 C21 C20 C19 2.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.684 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.131 # Attachment '- Compound 2.cif' data_apx1185 _database_code_depnum_ccdc_archive 'CCDC 824026' #TrackingRef '- Compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 Cl4 I2 N2 O2 U' _chemical_formula_weight 1482.79 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5036(13) _cell_length_b 20.834(2) _cell_length_c 12.6003(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.7370(10) _cell_angle_gamma 90.00 _cell_volume 3004.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 3.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4044 _exptl_absorpt_correction_T_max 0.5057 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28627 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.41 _reflns_number_total 5531 _reflns_number_gt 4295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0463P)^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 5531 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.002 _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 1.0000 0.0000 0.0000 0.01819(10) Uani 1 2 d S . . I1 I 1.12651(3) 0.03958(2) 0.21227(3) 0.02786(12) Uani 1 1 d . . . Cl1 Cl 0.6393(3) 0.14737(17) 0.5235(3) 0.1183(13) Uani 1 1 d . . . Cl2 Cl 0.5881(3) 0.1353(3) 0.7411(3) 0.171(2) Uani 1 1 d . . . N1 N 0.8157(4) 0.0307(2) 0.0604(4) 0.0194(10) Uani 1 1 d . . . O1 O 0.9604(3) 0.09764(18) -0.0497(3) 0.0211(9) Uani 1 1 d . . . C1 C 0.8813(5) 0.1429(3) -0.0541(4) 0.0208(13) Uani 1 1 d . . . C2 C 0.7834(5) 0.1380(3) -0.0013(4) 0.0212(13) Uani 1 1 d . . . H2 H 0.7319 0.1725 -0.0059 0.025 Uiso 1 1 calc R . . C3 C 0.7543(5) 0.0838(3) 0.0603(4) 0.0197(12) Uani 1 1 d . . . C4 C 0.9027(5) 0.1987(3) -0.1226(5) 0.0240(14) Uani 1 1 d . . . C5 C 0.9574(5) 0.1874(3) -0.2155(5) 0.0312(15) Uani 1 1 d . . . H5 H 0.9803 0.1461 -0.2323 0.037 Uiso 1 1 calc R . . C6 C 0.9770(5) 0.2385(3) -0.2822(5) 0.0370(17) Uani 1 1 d . . . H6 H 1.0116 0.2310 -0.3446 0.044 Uiso 1 1 calc R . . C7 C 0.9463(6) 0.2995(4) -0.2577(6) 0.0394(18) Uani 1 1 d . . . H7 H 0.9600 0.3334 -0.3029 0.047 Uiso 1 1 calc R . . C8 C 0.8948(6) 0.3106(3) -0.1655(6) 0.0433(19) Uani 1 1 d . . . H8 H 0.8750 0.3523 -0.1480 0.052 Uiso 1 1 calc R . . C9 C 0.8718(5) 0.2600(3) -0.0976(5) 0.0312(15) Uani 1 1 d . . . H9 H 0.8358 0.2679 -0.0360 0.037 Uiso 1 1 calc R . . C10 C 0.6499(5) 0.0909(3) 0.1213(4) 0.0243(14) Uani 1 1 d . . . C11 C 0.6371(5) 0.1460(3) 0.1804(5) 0.0314(16) Uani 1 1 d . . . H11 H 0.6926 0.1784 0.1813 0.038 Uiso 1 1 calc R . . C12 C 0.5415(6) 0.1527(4) 0.2382(5) 0.0421(18) Uani 1 1 d . . . H12 H 0.5336 0.1893 0.2791 0.051 Uiso 1 1 calc R . . C13 C 0.4586(6) 0.1052(4) 0.2350(6) 0.044(2) Uani 1 1 d . . . H13 H 0.3949 0.1100 0.2744 0.053 Uiso 1 1 calc R . . C14 C 0.4675(5) 0.0512(3) 0.1754(5) 0.0342(16) Uani 1 1 d . . . H14 H 0.4094 0.0200 0.1727 0.041 Uiso 1 1 calc R . . C15 C 0.5647(5) 0.0432(3) 0.1183(5) 0.0269(14) Uani 1 1 d . . . H15 H 0.5725 0.0061 0.0785 0.032 Uiso 1 1 calc R . . C16 C 0.7908(5) -0.0227(3) 0.1273(5) 0.0205(13) Uani 1 1 d . . . C17 C 0.7602(5) -0.0804(3) 0.0784(5) 0.0220(13) Uani 1 1 d . . . H17 H 0.7523 -0.0832 0.0044 0.026 Uiso 1 1 calc R . . C18 C 0.7412(5) -0.1346(3) 0.1395(5) 0.0200(13) Uani 1 1 d . . . C19 C 0.7531(5) -0.1277(3) 0.2488(5) 0.0230(13) Uani 1 1 d . . . H19 H 0.7398 -0.1632 0.2905 0.028 Uiso 1 1 calc R . . C20 C 0.7845(5) -0.0692(3) 0.3003(5) 0.0240(14) Uani 1 1 d . . . C21 C 0.8051(5) -0.0169(3) 0.2374(5) 0.0213(14) Uani 1 1 d . . . H21 H 0.8284 0.0221 0.2688 0.026 Uiso 1 1 calc R . . C22 C 0.7018(5) -0.1974(3) 0.0830(5) 0.0242(14) Uani 1 1 d . . . C23 C 0.5734(5) -0.1902(3) 0.0386(5) 0.0403(18) Uani 1 1 d . . . H23A H 0.5262 -0.1838 0.0964 0.060 Uiso 1 1 calc R . . H23B H 0.5483 -0.2284 0.0002 0.060 Uiso 1 1 calc R . . H23C H 0.5652 -0.1540 -0.0086 0.060 Uiso 1 1 calc R . . C24 C 0.7756(6) -0.2106(3) -0.0082(5) 0.0403(18) Uani 1 1 d . . . H24A H 0.7701 -0.1748 -0.0566 0.060 Uiso 1 1 calc R . . H24B H 0.7478 -0.2487 -0.0454 0.060 Uiso 1 1 calc R . . H24C H 0.8556 -0.2165 0.0197 0.060 Uiso 1 1 calc R . . C25 C 0.7121(6) -0.2549(3) 0.1591(5) 0.0359(17) Uani 1 1 d . . . H25A H 0.7906 -0.2576 0.1927 0.054 Uiso 1 1 calc R . . H25B H 0.6932 -0.2935 0.1197 0.054 Uiso 1 1 calc R . . H25C H 0.6591 -0.2495 0.2126 0.054 Uiso 1 1 calc R . . C26 C 0.7976(5) -0.0643(3) 0.4218(5) 0.0266(14) Uani 1 1 d . . . C27 C 0.8907(6) -0.1110(3) 0.4691(5) 0.0366(17) Uani 1 1 d . . . H27A H 0.8698 -0.1539 0.4468 0.055 Uiso 1 1 calc R . . H27B H 0.8964 -0.1085 0.5455 0.055 Uiso 1 1 calc R . . H27C H 0.9646 -0.0999 0.4448 0.055 Uiso 1 1 calc R . . C28 C 0.6795(5) -0.0810(4) 0.4640(5) 0.0384(17) Uani 1 1 d . . . H28A H 0.6209 -0.0512 0.4355 0.058 Uiso 1 1 calc R . . H28B H 0.6876 -0.0785 0.5405 0.058 Uiso 1 1 calc R . . H28C H 0.6568 -0.1238 0.4423 0.058 Uiso 1 1 calc R . . C29 C 0.8326(6) 0.0028(3) 0.4599(5) 0.0371(17) Uani 1 1 d . . . H29A H 0.9061 0.0140 0.4349 0.056 Uiso 1 1 calc R . . H29B H 0.8398 0.0039 0.5365 0.056 Uiso 1 1 calc R . . H29C H 0.7740 0.0330 0.4325 0.056 Uiso 1 1 calc R . . C30 C 0.6718(8) 0.1114(6) 0.6476(8) 0.096(4) Uani 1 1 d . . . H30A H 0.6639 0.0653 0.6391 0.115 Uiso 1 1 calc R . . H30B H 0.7527 0.1203 0.6723 0.115 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 0.01675(16) 0.01970(17) 0.01799(17) 0.00130(14) 0.00116(12) 0.00375(14) I1 0.0214(2) 0.0415(3) 0.0202(2) -0.00415(19) 0.00014(16) -0.00161(19) Cl1 0.094(2) 0.133(3) 0.138(3) 0.076(2) 0.063(2) 0.046(2) Cl2 0.118(3) 0.312(6) 0.079(2) -0.076(3) -0.0151(19) 0.091(3) N1 0.020(3) 0.021(3) 0.017(2) 0.002(2) 0.000(2) -0.001(2) O1 0.019(2) 0.020(2) 0.024(2) 0.0049(17) 0.0014(17) 0.0050(17) C1 0.018(3) 0.025(3) 0.018(3) -0.003(3) -0.006(2) 0.000(3) C2 0.013(3) 0.026(3) 0.024(3) -0.001(3) -0.003(2) 0.005(2) C3 0.015(3) 0.027(3) 0.017(3) -0.007(3) -0.001(2) 0.001(3) C4 0.014(3) 0.030(4) 0.026(3) 0.005(3) -0.006(2) -0.003(3) C5 0.019(3) 0.039(4) 0.036(4) 0.005(3) 0.003(3) -0.005(3) C6 0.029(4) 0.044(5) 0.037(4) 0.018(3) 0.002(3) -0.004(3) C7 0.027(4) 0.039(4) 0.049(5) 0.021(4) -0.012(3) -0.001(3) C8 0.031(4) 0.031(4) 0.063(5) 0.006(4) -0.020(4) 0.001(3) C9 0.033(4) 0.028(4) 0.031(4) 0.002(3) -0.009(3) 0.004(3) C10 0.015(3) 0.038(4) 0.019(3) 0.007(3) -0.002(2) 0.000(3) C11 0.017(3) 0.051(4) 0.026(3) -0.008(3) 0.000(3) 0.001(3) C12 0.029(4) 0.058(5) 0.039(4) -0.017(4) 0.003(3) 0.010(4) C13 0.020(4) 0.075(6) 0.037(4) -0.001(4) 0.005(3) 0.004(4) C14 0.016(3) 0.046(4) 0.040(4) 0.003(3) 0.003(3) -0.001(3) C15 0.019(3) 0.031(4) 0.030(4) 0.004(3) 0.000(3) 0.004(3) C16 0.016(3) 0.025(3) 0.021(3) -0.002(3) 0.003(2) -0.003(2) C17 0.017(3) 0.028(3) 0.021(3) 0.001(3) 0.001(2) -0.001(3) C18 0.012(3) 0.024(3) 0.023(3) -0.001(3) -0.001(2) 0.003(2) C19 0.019(3) 0.020(3) 0.030(4) 0.006(3) 0.003(3) 0.000(3) C20 0.018(3) 0.031(4) 0.022(3) 0.006(3) -0.001(2) -0.001(3) C21 0.015(3) 0.026(4) 0.022(3) -0.004(3) -0.002(2) 0.001(2) C22 0.026(3) 0.026(3) 0.020(3) 0.003(3) -0.002(3) -0.001(3) C23 0.030(4) 0.039(4) 0.048(4) -0.009(4) -0.017(3) -0.005(3) C24 0.050(4) 0.034(4) 0.039(4) -0.012(3) 0.012(3) -0.008(3) C25 0.048(4) 0.020(3) 0.038(4) -0.001(3) -0.004(3) -0.012(3) C26 0.030(3) 0.031(4) 0.019(3) 0.001(3) 0.003(3) -0.005(3) C27 0.049(4) 0.033(4) 0.026(4) 0.000(3) -0.008(3) -0.006(3) C28 0.040(4) 0.050(5) 0.027(4) 0.001(3) 0.010(3) -0.001(4) C29 0.057(5) 0.032(4) 0.021(3) -0.001(3) 0.002(3) -0.008(4) C30 0.065(7) 0.125(10) 0.100(8) 0.032(7) 0.014(6) 0.024(7) _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 O1 2.163(4) 3_755 ? U1 O1 2.163(4) . ? U1 N1 2.409(5) . ? U1 N1 2.409(5) 3_755 ? U1 I1 3.0288(5) . ? U1 I1 3.0288(5) 3_755 ? U1 C16 3.060(6) 3_755 ? U1 C16 3.060(6) . ? Cl1 C30 1.741(10) . ? Cl2 C30 1.671(10) . ? N1 C3 1.313(7) . ? N1 C16 1.443(7) . ? O1 C1 1.308(6) . ? C1 C2 1.368(8) . ? C1 C4 1.483(8) . ? C2 C3 1.429(8) . ? C3 C10 1.496(8) . ? C4 C9 1.370(8) . ? C4 C5 1.404(8) . ? C5 C6 1.389(9) . ? C6 C7 1.363(10) . ? C7 C8 1.375(10) . ? C8 C9 1.399(9) . ? C10 C15 1.393(8) . ? C10 C11 1.384(9) . ? C11 C12 1.386(8) . ? C12 C13 1.372(10) . ? C13 C14 1.362(10) . ? C14 C15 1.400(8) . ? C16 C17 1.380(8) . ? C16 C21 1.386(8) . ? C17 C18 1.396(8) . ? C18 C19 1.378(8) . ? C18 C22 1.535(8) . ? C19 C20 1.410(8) . ? C20 C21 1.383(8) . ? C20 C26 1.526(8) . ? C22 C24 1.521(8) . ? C22 C25 1.531(8) . ? C22 C23 1.533(8) . ? C26 C29 1.521(8) . ? C26 C27 1.523(9) . ? C26 C28 1.547(8) . ? 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 O1 U1 O1 180.0 3_755 . ? O1 U1 N1 108.94(15) 3_755 . ? O1 U1 N1 71.06(15) . . ? O1 U1 N1 71.06(15) 3_755 3_755 ? O1 U1 N1 108.94(15) . 3_755 ? N1 U1 N1 180.0 . 3_755 ? O1 U1 I1 86.08(10) 3_755 . ? O1 U1 I1 93.92(10) . . ? N1 U1 I1 90.53(11) . . ? N1 U1 I1 89.48(11) 3_755 . ? O1 U1 I1 93.92(10) 3_755 3_755 ? O1 U1 I1 86.08(10) . 3_755 ? N1 U1 I1 89.48(11) . 3_755 ? N1 U1 I1 90.52(11) 3_755 3_755 ? I1 U1 I1 180.0 . 3_755 ? O1 U1 C16 98.25(15) 3_755 3_755 ? O1 U1 C16 81.75(15) . 3_755 ? N1 U1 C16 152.56(16) . 3_755 ? N1 U1 C16 27.44(16) 3_755 3_755 ? I1 U1 C16 95.01(11) . 3_755 ? I1 U1 C16 84.99(11) 3_755 3_755 ? O1 U1 C16 81.75(15) 3_755 . ? O1 U1 C16 98.25(15) . . ? N1 U1 C16 27.44(16) . . ? N1 U1 C16 152.56(16) 3_755 . ? I1 U1 C16 84.99(11) . . ? I1 U1 C16 95.01(11) 3_755 . ? C16 U1 C16 180.0 3_755 . ? C3 N1 C16 120.8(5) . . ? C3 N1 U1 135.6(4) . . ? C16 N1 U1 102.3(3) . . ? C1 O1 U1 144.7(4) . . ? O1 C1 C2 121.9(5) . . ? O1 C1 C4 115.8(5) . . ? C2 C1 C4 122.3(5) . . ? C1 C2 C3 125.0(5) . . ? N1 C3 C2 120.7(5) . . ? N1 C3 C10 122.9(5) . . ? C2 C3 C10 116.5(5) . . ? C9 C4 C5 119.9(6) . . ? C9 C4 C1 122.3(6) . . ? C5 C4 C1 117.8(6) . . ? C6 C5 C4 119.2(7) . . ? C7 C6 C5 121.1(7) . . ? C6 C7 C8 119.4(7) . . ? C7 C8 C9 121.0(7) . . ? C4 C9 C8 119.4(7) . . ? C15 C10 C11 119.6(6) . . ? C15 C10 C3 121.0(6) . . ? C11 C10 C3 119.5(5) . . ? C12 C11 C10 120.0(6) . . ? C13 C12 C11 119.9(7) . . ? C14 C13 C12 121.4(6) . . ? C13 C14 C15 119.4(6) . . ? C10 C15 C14 119.8(6) . . ? C17 C16 C21 121.5(6) . . ? C17 C16 N1 117.9(5) . . ? C21 C16 N1 120.5(5) . . ? C17 C16 U1 94.5(3) . . ? C21 C16 U1 119.4(4) . . ? N1 C16 U1 50.3(3) . . ? C16 C17 C18 120.3(5) . . ? C19 C18 C17 117.5(5) . . ? C19 C18 C22 123.2(5) . . ? C17 C18 C22 119.3(5) . . ? C18 C19 C20 123.1(5) . . ? C21 C20 C19 117.9(5) . . ? C21 C20 C26 121.1(5) . . ? C19 C20 C26 120.9(5) . . ? C20 C21 C16 119.6(5) . . ? C24 C22 C25 108.5(5) . . ? C24 C22 C23 109.4(5) . . ? C25 C22 C23 108.5(5) . . ? C24 C22 C18 110.0(5) . . ? C25 C22 C18 112.0(5) . . ? C23 C22 C18 108.4(5) . . ? C29 C26 C27 108.0(5) . . ? C29 C26 C20 112.0(5) . . ? C27 C26 C20 110.2(5) . . ? C29 C26 C28 108.2(5) . . ? C27 C26 C28 109.2(5) . . ? C20 C26 C28 109.2(5) . . ? Cl2 C30 Cl1 114.7(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.720 _refine_diff_density_min -1.665 _refine_diff_density_rms 0.139 # Attachment '- Compound 3.cif' data_apx1147s _database_code_depnum_ccdc_archive 'CCDC 824027' #TrackingRef '- Compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H74 I2 N2 O3 Pu' _chemical_formula_weight 1388.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 '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 10.1318(10) _cell_length_b 11.8288(11) _cell_length_c 13.1117(13) _cell_angle_alpha 105.2990(10) _cell_angle_beta 103.8160(10) _cell_angle_gamma 93.7570(10) _cell_volume 1457.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5351 _exptl_absorpt_correction_T_max 0.8416 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16551 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.38 _reflns_number_total 6681 _reflns_number_gt 5910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0311P)^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 6681 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _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 Pu1 Pu 1.0000 1.0000 0.0000 0.01644(5) Uani 1 2 d S . . I1 I 1.224401(17) 0.854463(16) 0.046960(16) 0.03110(6) Uani 1 1 d . . . O1 O 1.02177(17) 1.06981(15) 0.17483(14) 0.0208(4) Uani 1 1 d . . . N1 N 0.8543(2) 0.86893(18) 0.04655(17) 0.0180(4) Uani 1 1 d . . . C1 C 0.7808(2) 0.7846(2) -0.0559(2) 0.0177(5) Uani 1 1 d . . . C2 C 0.6514(3) 0.8036(2) -0.1098(2) 0.0204(5) Uani 1 1 d . . . H2 H 0.6116 0.8674 -0.0774 0.025 Uiso 1 1 calc R . . C3 C 0.5825(2) 0.7276(2) -0.2113(2) 0.0183(5) Uani 1 1 d . . . C4 C 0.6451(2) 0.6317(2) -0.2560(2) 0.0187(5) Uani 1 1 d . . . H4 H 0.5978 0.5786 -0.3231 0.022 Uiso 1 1 calc R . . C5 C 0.7752(3) 0.6121(2) -0.2046(2) 0.0187(5) Uani 1 1 d . . . C6 C 0.8431(2) 0.6924(2) -0.1032(2) 0.0188(5) Uani 1 1 d . . . H6 H 0.9312 0.6835 -0.0674 0.023 Uiso 1 1 calc R . . C7 C 0.8447(3) 0.5076(2) -0.2515(2) 0.0257(6) Uani 1 1 d . . . C8 C 0.9836(3) 0.5535(3) -0.2645(3) 0.0365(7) Uani 1 1 d . . . H8A H 0.9684 0.5932 -0.3205 0.055 Uiso 1 1 calc R . . H8B H 1.0327 0.4881 -0.2848 0.055 Uiso 1 1 calc R . . H8C H 1.0364 0.6077 -0.1962 0.055 Uiso 1 1 calc R . . C9 C 0.7584(3) 0.4298(3) -0.3636(3) 0.0399(8) Uani 1 1 d . . . H9A H 0.6728 0.3973 -0.3564 0.060 Uiso 1 1 calc R . . H9B H 0.8071 0.3667 -0.3908 0.060 Uiso 1 1 calc R . . H9C H 0.7409 0.4766 -0.4138 0.060 Uiso 1 1 calc R . . C10 C 0.8683(3) 0.4311(3) -0.1718(3) 0.0329(7) Uani 1 1 d . . . H10A H 0.9297 0.4766 -0.1030 0.049 Uiso 1 1 calc R . . H10B H 0.9077 0.3628 -0.2025 0.049 Uiso 1 1 calc R . . H10C H 0.7823 0.4063 -0.1603 0.049 Uiso 1 1 calc R . . C11 C 0.4432(3) 0.7484(2) -0.2762(2) 0.0231(6) Uani 1 1 d . . . C12 C 0.4561(3) 0.7600(3) -0.3868(3) 0.0363(7) Uani 1 1 d . . . H12A H 0.4824 0.6886 -0.4268 0.054 Uiso 1 1 calc R . . H12B H 0.5244 0.8256 -0.3751 0.054 Uiso 1 1 calc R . . H12C H 0.3694 0.7731 -0.4280 0.054 Uiso 1 1 calc R . . C13 C 0.3343(3) 0.6442(3) -0.2967(3) 0.0494(10) Uani 1 1 d . . . H13A H 0.3232 0.6373 -0.2278 0.074 Uiso 1 1 calc R . . H13B H 0.3624 0.5728 -0.3351 0.074 Uiso 1 1 calc R . . H13C H 0.2488 0.6566 -0.3401 0.074 Uiso 1 1 calc R . . C14 C 0.3979(4) 0.8620(3) -0.2179(3) 0.0473(9) Uani 1 1 d . . . H14A H 0.3136 0.8743 -0.2630 0.071 Uiso 1 1 calc R . . H14B H 0.4673 0.9274 -0.2042 0.071 Uiso 1 1 calc R . . H14C H 0.3841 0.8560 -0.1494 0.071 Uiso 1 1 calc R . . C15 C 0.7316(3) 0.7639(2) 0.1410(2) 0.0203(5) Uani 1 1 d . . . C16 C 0.6145(3) 0.7851(3) 0.1751(3) 0.0346(7) Uani 1 1 d . . . H16 H 0.5955 0.8622 0.1976 0.042 Uiso 1 1 calc R . . C17 C 0.5253(3) 0.6917(3) 0.1759(3) 0.0461(9) Uani 1 1 d . . . H17 H 0.4453 0.7062 0.1971 0.055 Uiso 1 1 calc R . . C18 C 0.5546(3) 0.5772(3) 0.1454(3) 0.0425(9) Uani 1 1 d . . . H18 H 0.4942 0.5149 0.1459 0.051 Uiso 1 1 calc R . . C19 C 0.6723(3) 0.5554(3) 0.1145(2) 0.0352(8) Uani 1 1 d . . . H19 H 0.6932 0.4785 0.0958 0.042 Uiso 1 1 calc R . . C20 C 0.7604(3) 0.6485(2) 0.1111(2) 0.0268(6) Uani 1 1 d . . . H20 H 0.8395 0.6334 0.0887 0.032 Uiso 1 1 calc R . . C21 C 0.8278(2) 0.8646(2) 0.1392(2) 0.0161(5) Uani 1 1 d . . . C22 C 0.8887(2) 0.9502(2) 0.2408(2) 0.0187(5) Uani 1 1 d . . . H22 H 0.8655 0.9394 0.3024 0.022 Uiso 1 1 calc R . . C23 C 0.9801(2) 1.0490(2) 0.25584(19) 0.0168(5) Uani 1 1 d . . . C24 C 1.0401(2) 1.1344(2) 0.3652(2) 0.0173(5) Uani 1 1 d . . . C25 C 1.1599(3) 1.2100(2) 0.3823(2) 0.0241(6) Uani 1 1 d . . . H25 H 1.1985 1.2083 0.3244 0.029 Uiso 1 1 calc R . . C26 C 1.2216(3) 1.2873(3) 0.4848(2) 0.0314(7) Uani 1 1 d . . . H26 H 1.3023 1.3364 0.4954 0.038 Uiso 1 1 calc R . . C27 C 1.1654(3) 1.2926(2) 0.5714(2) 0.0279(6) Uani 1 1 d . . . H27 H 1.2078 1.3449 0.6402 0.033 Uiso 1 1 calc R . . C28 C 1.0447(3) 1.2193(2) 0.5554(2) 0.0264(6) Uani 1 1 d . . . H28 H 1.0056 1.2230 0.6134 0.032 Uiso 1 1 calc R . . C29 C 0.9824(3) 1.1408(2) 0.4530(2) 0.0232(5) Uani 1 1 d . . . H29 H 0.9017 1.0920 0.4427 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.01792(7) 0.02158(8) 0.00982(7) 0.00415(5) 0.00490(5) -0.00029(5) I1 0.02407(10) 0.03124(12) 0.03843(12) 0.01379(10) 0.00479(8) 0.00449(8) O1 0.0246(9) 0.0220(9) 0.0145(9) 0.0043(7) 0.0054(7) -0.0037(7) N1 0.0181(10) 0.0189(11) 0.0151(10) 0.0027(9) 0.0038(8) 0.0010(8) C1 0.0187(12) 0.0186(12) 0.0148(12) 0.0037(10) 0.0047(9) -0.0018(9) C2 0.0226(13) 0.0193(13) 0.0218(13) 0.0084(11) 0.0074(10) 0.0039(10) C3 0.0175(12) 0.0204(13) 0.0178(12) 0.0076(10) 0.0047(9) -0.0010(9) C4 0.0209(12) 0.0194(13) 0.0137(12) 0.0043(10) 0.0027(9) -0.0031(10) C5 0.0219(13) 0.0163(12) 0.0165(12) 0.0034(10) 0.0051(10) -0.0007(10) C6 0.0169(12) 0.0193(13) 0.0196(12) 0.0068(10) 0.0029(9) -0.0005(9) C7 0.0259(14) 0.0192(13) 0.0254(14) -0.0005(11) 0.0020(11) 0.0044(11) C8 0.0361(17) 0.0336(17) 0.0395(18) 0.0009(14) 0.0188(14) 0.0092(14) C9 0.0448(19) 0.0278(17) 0.0314(17) -0.0093(13) -0.0006(14) 0.0108(14) C10 0.0325(16) 0.0223(15) 0.0409(18) 0.0079(13) 0.0046(13) 0.0059(12) C11 0.0186(13) 0.0280(14) 0.0223(14) 0.0100(11) 0.0019(10) 0.0027(10) C12 0.0326(16) 0.0475(19) 0.0312(16) 0.0217(15) 0.0019(13) 0.0039(14) C13 0.0202(15) 0.058(2) 0.074(3) 0.043(2) -0.0041(15) -0.0082(14) C14 0.0372(18) 0.059(2) 0.0378(19) 0.0058(17) 0.0004(15) 0.0244(17) C15 0.0208(12) 0.0231(13) 0.0155(12) 0.0077(10) 0.0006(9) -0.0004(10) C16 0.0244(15) 0.0331(17) 0.054(2) 0.0218(15) 0.0138(14) 0.0036(12) C17 0.0224(15) 0.053(2) 0.074(3) 0.037(2) 0.0140(16) 0.0008(14) C18 0.0350(17) 0.0427(19) 0.0435(19) 0.0264(16) -0.0103(14) -0.0204(14) C19 0.057(2) 0.0220(15) 0.0229(15) 0.0109(12) 0.0018(14) -0.0065(13) C20 0.0382(16) 0.0229(14) 0.0199(13) 0.0084(11) 0.0079(11) -0.0001(12) C21 0.0141(11) 0.0156(12) 0.0192(12) 0.0053(10) 0.0047(9) 0.0040(9) C22 0.0226(12) 0.0208(13) 0.0161(12) 0.0080(10) 0.0086(10) 0.0038(10) C23 0.0178(12) 0.0208(13) 0.0148(12) 0.0061(10) 0.0079(9) 0.0066(9) C24 0.0212(12) 0.0150(12) 0.0163(12) 0.0057(10) 0.0045(9) 0.0034(9) C25 0.0286(14) 0.0237(14) 0.0194(13) 0.0040(11) 0.0092(11) -0.0029(11) C26 0.0327(15) 0.0282(15) 0.0252(15) -0.0006(12) 0.0056(12) -0.0093(12) C27 0.0362(16) 0.0241(14) 0.0160(13) -0.0032(11) 0.0038(11) 0.0025(12) C28 0.0352(15) 0.0265(14) 0.0195(13) 0.0050(11) 0.0121(11) 0.0065(12) C29 0.0284(14) 0.0216(13) 0.0192(13) 0.0028(11) 0.0095(11) 0.0017(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 Pu1 O1 2.1727(17) . ? Pu1 O1 2.1728(17) 2_775 ? Pu1 N1 2.3634(19) 2_775 ? Pu1 N1 2.3635(19) . ? Pu1 I1 2.9859(3) . ? Pu1 I1 2.9859(3) 2_775 ? O1 C23 1.306(3) . ? N1 C21 1.318(3) . ? N1 C1 1.439(3) . ? C1 C6 1.376(4) . ? C1 C2 1.396(3) . ? C2 C3 1.382(4) . ? C3 C4 1.398(4) . ? C3 C11 1.536(3) . ? C4 C5 1.395(3) . ? C5 C6 1.399(3) . ? C5 C7 1.523(4) . ? C7 C9 1.529(4) . ? C7 C8 1.539(4) . ? C7 C10 1.541(4) . ? C11 C14 1.519(4) . ? C11 C13 1.522(4) . ? C11 C12 1.526(4) . ? C15 C16 1.379(4) . ? C15 C20 1.388(4) . ? C15 C21 1.498(3) . ? C16 C17 1.384(4) . ? C17 C18 1.381(5) . ? C18 C19 1.366(5) . ? C19 C20 1.388(4) . ? C21 C22 1.413(3) . ? C22 C23 1.382(3) . ? C23 C24 1.478(3) . ? C24 C25 1.395(3) . ? C24 C29 1.397(3) . ? C25 C26 1.381(4) . ? C26 C27 1.377(4) . ? C27 C28 1.390(4) . ? C28 C29 1.387(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pu1 O1 180.0 . 2_775 ? O1 Pu1 N1 106.70(7) . 2_775 ? O1 Pu1 N1 73.29(7) 2_775 2_775 ? O1 Pu1 N1 73.29(7) . . ? O1 Pu1 N1 106.71(7) 2_775 . ? N1 Pu1 N1 180.00(7) 2_775 . ? O1 Pu1 I1 89.79(5) . . ? O1 Pu1 I1 90.21(5) 2_775 . ? N1 Pu1 I1 91.36(5) 2_775 . ? N1 Pu1 I1 88.64(5) . . ? O1 Pu1 I1 90.21(5) . 2_775 ? O1 Pu1 I1 89.79(5) 2_775 2_775 ? N1 Pu1 I1 88.64(5) 2_775 2_775 ? N1 Pu1 I1 91.36(5) . 2_775 ? I1 Pu1 I1 180.0 . 2_775 ? C23 O1 Pu1 142.69(16) . . ? C21 N1 C1 120.7(2) . . ? C21 N1 Pu1 133.84(16) . . ? C1 N1 Pu1 105.33(14) . . ? C6 C1 C2 121.1(2) . . ? C6 C1 N1 119.7(2) . . ? C2 C1 N1 119.0(2) . . ? C3 C2 C1 119.9(2) . . ? C2 C3 C4 118.1(2) . . ? C2 C3 C11 121.8(2) . . ? C4 C3 C11 120.0(2) . . ? C5 C4 C3 122.9(2) . . ? C4 C5 C6 117.3(2) . . ? C4 C5 C7 123.7(2) . . ? C6 C5 C7 118.9(2) . . ? C1 C6 C5 120.5(2) . . ? C5 C7 C9 112.4(2) . . ? C5 C7 C8 109.5(2) . . ? C9 C7 C8 108.3(3) . . ? C5 C7 C10 108.9(2) . . ? C9 C7 C10 108.4(2) . . ? C8 C7 C10 109.4(2) . . ? C14 C11 C13 109.7(3) . . ? C14 C11 C12 107.3(2) . . ? C13 C11 C12 108.6(3) . . ? C14 C11 C3 112.0(2) . . ? C13 C11 C3 110.3(2) . . ? C12 C11 C3 108.9(2) . . ? C16 C15 C20 119.1(2) . . ? C16 C15 C21 120.3(2) . . ? C20 C15 C21 120.7(2) . . ? C15 C16 C17 120.1(3) . . ? C18 C17 C16 120.3(3) . . ? C19 C18 C17 120.2(3) . . ? C18 C19 C20 119.7(3) . . ? C15 C20 C19 120.6(3) . . ? N1 C21 C22 123.2(2) . . ? N1 C21 C15 120.2(2) . . ? C22 C21 C15 116.5(2) . . ? C23 C22 C21 125.1(2) . . ? O1 C23 C22 121.8(2) . . ? O1 C23 C24 116.3(2) . . ? C22 C23 C24 121.8(2) . . ? C25 C24 C29 118.6(2) . . ? C25 C24 C23 119.0(2) . . ? C29 C24 C23 122.3(2) . . ? C26 C25 C24 120.4(3) . . ? C27 C26 C25 120.9(3) . . ? C26 C27 C28 119.5(3) . . ? C29 C28 C27 120.1(3) . . ? C28 C29 C24 120.5(2) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.243 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.094