# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'James M. Boncella' 'Aaron Odom' 'Brian Scott' 'Liam P. Spencer' 'Douglas Swartz' _publ_contact_author_name 'James M. Boncella' _publ_contact_author_address ; Material Physics and Applications Division Los Alamos Natl. Lab P.O. Box 1663 Los Alamos NM 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email BONCELLA@LANL.GOV _publ_section_title ; Exploring the Coordination Modes of Pyrrolyl Ligands in Bis(imido) Uranium(VI) Complexes ; # Attachment 'UNtBu2dpmmes.cif' data_apx764 _database_code_depnum_ccdc_archive 'CCDC 765726' #TrackingRef 'UNtBu2dpmmes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 N4 U' _chemical_formula_weight 788.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1415(9) _cell_length_b 12.5846(11) _cell_length_c 12.7942(11) _cell_angle_alpha 87.3010(10) _cell_angle_beta 80.7680(10) _cell_angle_gamma 73.3150(10) _cell_volume 1696.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 4.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4777 _exptl_absorpt_correction_T_max 0.6993 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 15658 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.36 _reflns_number_total 7516 _reflns_number_gt 6664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (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^)+(0.0488P)^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 7516 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.098236(15) 0.203606(12) 0.256047(12) 0.01269(6) Uani 1 1 d . . . N1 N 0.1517(4) 0.1086(3) 0.3728(3) 0.0180(8) Uani 1 1 d . . . N2 N -0.0725(3) 0.2180(3) 0.2285(3) 0.0153(8) Uani 1 1 d . . . N3 N 0.3152(4) 0.1266(3) 0.1398(3) 0.0150(8) Uani 1 1 d . . . N4 N 0.0832(4) 0.4108(3) 0.2182(3) 0.0164(8) Uani 1 1 d . . . C1 C 0.2137(5) 0.0456(4) 0.4589(4) 0.0191(9) Uani 1 1 d . . . C2 C 0.3539(6) 0.0386(5) 0.4357(5) 0.0432(16) Uani 1 1 d . . . H2A H 0.3904 0.0014 0.3694 0.065 Uiso 1 1 calc R . . H2B H 0.3960 -0.0021 0.4912 0.065 Uiso 1 1 calc R . . H2C H 0.3638 0.1120 0.4319 0.065 Uiso 1 1 calc R . . C3 C 0.1983(6) -0.0709(4) 0.4617(4) 0.0322(12) Uani 1 1 d . . . H3A H 0.1097 -0.0666 0.4760 0.048 Uiso 1 1 calc R . . H3B H 0.2405 -0.1132 0.5164 0.048 Uiso 1 1 calc R . . H3C H 0.2348 -0.1063 0.3946 0.048 Uiso 1 1 calc R . . C4 C 0.1542(6) 0.1050(4) 0.5640(4) 0.0352(14) Uani 1 1 d . . . H4A H 0.0655 0.1098 0.5775 0.053 Uiso 1 1 calc R . . H4B H 0.1645 0.1783 0.5606 0.053 Uiso 1 1 calc R . . H4C H 0.1952 0.0641 0.6200 0.053 Uiso 1 1 calc R . . C5 C -0.1932(5) 0.2391(4) 0.1899(4) 0.0195(10) Uani 1 1 d . . . C6 C -0.2097(6) 0.1305(5) 0.1549(6) 0.0506(18) Uani 1 1 d . . . H6A H -0.1421 0.0980 0.0991 0.076 Uiso 1 1 calc R . . H6B H -0.2895 0.1450 0.1297 0.076 Uiso 1 1 calc R . . H6C H -0.2078 0.0803 0.2138 0.076 Uiso 1 1 calc R . . C7 C -0.2988(5) 0.2894(6) 0.2785(5) 0.0465(17) Uani 1 1 d . . . H7A H -0.2965 0.2384 0.3369 0.070 Uiso 1 1 calc R . . H7B H -0.3790 0.3045 0.2537 0.070 Uiso 1 1 calc R . . H7C H -0.2881 0.3573 0.3012 0.070 Uiso 1 1 calc R . . C8 C -0.1969(7) 0.3184(7) 0.0971(6) 0.063(2) Uani 1 1 d . . . H8A H -0.1303 0.2857 0.0408 0.094 Uiso 1 1 calc R . . H8B H -0.1856 0.3864 0.1189 0.094 Uiso 1 1 calc R . . H8C H -0.2774 0.3335 0.0729 0.094 Uiso 1 1 calc R . . C9 C 0.3085(5) -0.0712(4) 0.1529(3) 0.0170(9) Uani 1 1 d . . . C10 C 0.2261(5) -0.1390(4) 0.1747(4) 0.0188(10) Uani 1 1 d . . . C11 C 0.2754(5) -0.2510(4) 0.1991(4) 0.0231(10) Uani 1 1 d . . . H11 H 0.2205 -0.2951 0.2131 0.028 Uiso 1 1 calc R . . C12 C 0.4026(5) -0.2983(4) 0.2032(4) 0.0233(11) Uani 1 1 d . . . C13 C 0.4817(5) -0.2297(4) 0.1855(4) 0.0225(10) Uani 1 1 d . . . H13 H 0.5672 -0.2598 0.1904 0.027 Uiso 1 1 calc R . . C14 C 0.4380(5) -0.1167(4) 0.1605(3) 0.0188(10) Uani 1 1 d . . . C15 C 0.0834(5) -0.0964(4) 0.1789(4) 0.0254(11) Uani 1 1 d . . . H15A H 0.0603 -0.0188 0.1617 0.038 Uiso 1 1 calc R . . H15B H 0.0422 -0.1071 0.2489 0.038 Uiso 1 1 calc R . . H15C H 0.0573 -0.1364 0.1289 0.038 Uiso 1 1 calc R . . C16 C 0.4557(6) -0.4201(4) 0.2245(5) 0.0332(13) Uani 1 1 d . . . H16A H 0.5454 -0.4370 0.2245 0.050 Uiso 1 1 calc R . . H16B H 0.4401 -0.4624 0.1703 0.050 Uiso 1 1 calc R . . H16C H 0.4155 -0.4385 0.2922 0.050 Uiso 1 1 calc R . . C17 C 0.5358(5) -0.0532(4) 0.1430(4) 0.0228(10) Uani 1 1 d . . . H17A H 0.4958 0.0229 0.1271 0.034 Uiso 1 1 calc R . . H17B H 0.6002 -0.0853 0.0848 0.034 Uiso 1 1 calc R . . H17C H 0.5737 -0.0567 0.2058 0.034 Uiso 1 1 calc R . . C18 C 0.2590(4) 0.0454(3) 0.1185(3) 0.0153(9) Uani 1 1 d . . . C19 C 0.1660(4) 0.0926(4) 0.0544(3) 0.0164(9) Uani 1 1 d . . . H19 H 0.1130 0.0571 0.0304 0.020 Uiso 1 1 calc R . . C20 C 0.1668(4) 0.2022(4) 0.0328(3) 0.0163(9) Uani 1 1 d . . . H20 H 0.1152 0.2530 -0.0079 0.020 Uiso 1 1 calc R . . C21 C 0.2610(4) 0.2204(4) 0.0847(3) 0.0156(9) Uani 1 1 d . . . C22 C 0.2903(4) 0.3275(4) 0.1048(3) 0.0182(9) Uani 1 1 d . . . C23 C 0.4329(4) 0.3041(4) 0.1076(4) 0.0218(10) Uani 1 1 d . . . H23A H 0.4794 0.2821 0.0385 0.033 Uiso 1 1 calc R . . H23B H 0.4588 0.2457 0.1573 0.033 Uiso 1 1 calc R . . H23C H 0.4497 0.3700 0.1288 0.033 Uiso 1 1 calc R . . C24 C 0.2482(5) 0.4149(4) 0.0207(4) 0.0264(11) Uani 1 1 d . . . H24A H 0.2995 0.3915 -0.0465 0.040 Uiso 1 1 calc R . . H24B H 0.2578 0.4844 0.0403 0.040 Uiso 1 1 calc R . . H24C H 0.1609 0.4236 0.0156 0.040 Uiso 1 1 calc R . . C25 C 0.2120(4) 0.3632(3) 0.2111(3) 0.0164(9) Uani 1 1 d . . . C26 C 0.2443(4) 0.3360(3) 0.3126(3) 0.0163(9) Uani 1 1 d . . . H26 H 0.3247 0.3015 0.3292 0.020 Uiso 1 1 calc R . . C27 C 0.1306(4) 0.3713(4) 0.3844(3) 0.0174(9) Uani 1 1 d . . . H27 H 0.1215 0.3642 0.4577 0.021 Uiso 1 1 calc R . . C28 C 0.0342(5) 0.4190(4) 0.3247(3) 0.0170(9) Uani 1 1 d . . . C29 C -0.0984(5) 0.4844(4) 0.3619(3) 0.0165(9) Uani 1 1 d . . . C30 C -0.1770(4) 0.4469(4) 0.4458(3) 0.0175(9) Uani 1 1 d . . . C31 C -0.2989(5) 0.5139(4) 0.4783(4) 0.0201(10) Uani 1 1 d . . . H31 H -0.3505 0.4879 0.5317 0.024 Uiso 1 1 calc R . . C32 C -0.3482(4) 0.6183(4) 0.4352(4) 0.0203(10) Uani 1 1 d . . . C33 C -0.2678(5) 0.6540(4) 0.3552(4) 0.0194(10) Uani 1 1 d . . . H33 H -0.2972 0.7240 0.3261 0.023 Uiso 1 1 calc R . . C34 C -0.1462(5) 0.5900(4) 0.3170(3) 0.0173(9) Uani 1 1 d . . . C35 C -0.1321(5) 0.3388(4) 0.5006(4) 0.0257(11) Uani 1 1 d . . . H35A H -0.0465 0.3019 0.4697 0.039 Uiso 1 1 calc R . . H35B H -0.1858 0.2930 0.4929 0.039 Uiso 1 1 calc R . . H35C H -0.1349 0.3517 0.5744 0.039 Uiso 1 1 calc R . . C36 C -0.0665(5) 0.6391(4) 0.2324(4) 0.0232(10) Uani 1 1 d . . . H36A H 0.0150 0.5864 0.2135 0.035 Uiso 1 1 calc R . . H36B H -0.0556 0.7053 0.2589 0.035 Uiso 1 1 calc R . . H36C H -0.1081 0.6569 0.1711 0.035 Uiso 1 1 calc R . . C37 C -0.4786(5) 0.6901(4) 0.4752(4) 0.0287(11) Uani 1 1 d . . . H37A H -0.5189 0.6518 0.5303 0.043 Uiso 1 1 calc R . . H37B H -0.5276 0.7068 0.4182 0.043 Uiso 1 1 calc R . . H37C H -0.4730 0.7579 0.5028 0.043 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 0.01207(10) 0.01246(9) 0.01356(9) -0.00137(5) -0.00302(6) -0.00271(6) N1 0.022(2) 0.0150(19) 0.0166(18) 0.0012(14) -0.0027(16) -0.0053(16) N2 0.013(2) 0.0174(19) 0.0154(18) -0.0020(14) -0.0019(15) -0.0043(15) N3 0.013(2) 0.0173(19) 0.0137(17) -0.0048(14) -0.0018(14) -0.0028(15) N4 0.019(2) 0.0170(19) 0.0163(18) -0.0014(14) -0.0037(15) -0.0083(16) C1 0.019(3) 0.020(2) 0.019(2) 0.0020(17) -0.0095(19) -0.0039(19) C2 0.031(4) 0.055(4) 0.048(4) 0.025(3) -0.017(3) -0.017(3) C3 0.038(3) 0.021(3) 0.037(3) 0.012(2) -0.016(3) -0.005(2) C4 0.052(4) 0.028(3) 0.022(3) 0.002(2) -0.017(3) -0.001(3) C5 0.018(3) 0.019(2) 0.019(2) -0.0033(18) -0.0028(18) -0.0007(19) C6 0.034(4) 0.035(3) 0.088(5) -0.023(3) -0.031(4) -0.002(3) C7 0.017(3) 0.078(5) 0.037(3) -0.030(3) -0.010(2) 0.007(3) C8 0.032(4) 0.099(6) 0.070(5) 0.056(4) -0.035(4) -0.034(4) C9 0.022(3) 0.015(2) 0.015(2) -0.0023(16) -0.0034(18) -0.0061(18) C10 0.019(3) 0.019(2) 0.019(2) -0.0036(17) 0.0003(18) -0.0063(19) C11 0.025(3) 0.018(2) 0.027(3) -0.0095(19) 0.002(2) -0.009(2) C12 0.031(3) 0.016(2) 0.021(2) -0.0031(18) -0.006(2) -0.001(2) C13 0.020(3) 0.023(2) 0.022(2) -0.0025(19) -0.0062(19) 0.001(2) C14 0.019(3) 0.018(2) 0.017(2) -0.0056(17) -0.0003(18) -0.0017(19) C15 0.020(3) 0.019(2) 0.038(3) -0.002(2) -0.002(2) -0.007(2) C16 0.037(3) 0.016(2) 0.044(3) -0.002(2) -0.009(3) -0.002(2) C17 0.017(3) 0.024(3) 0.024(2) -0.0020(19) -0.0016(19) -0.001(2) C18 0.016(2) 0.012(2) 0.017(2) -0.0027(16) -0.0005(17) -0.0033(17) C19 0.011(2) 0.019(2) 0.019(2) -0.0040(17) -0.0024(17) -0.0038(18) C20 0.013(2) 0.021(2) 0.014(2) -0.0012(16) -0.0039(17) -0.0018(18) C21 0.013(2) 0.016(2) 0.015(2) -0.0034(16) 0.0001(17) -0.0009(17) C22 0.018(2) 0.017(2) 0.018(2) -0.0025(17) 0.0023(18) -0.0052(18) C23 0.016(3) 0.023(2) 0.028(3) -0.0017(19) -0.0013(19) -0.010(2) C24 0.032(3) 0.022(3) 0.023(2) 0.0016(19) 0.001(2) -0.008(2) C25 0.019(2) 0.010(2) 0.019(2) -0.0021(16) 0.0001(18) -0.0053(18) C26 0.016(2) 0.012(2) 0.022(2) 0.0008(16) -0.0057(18) -0.0040(17) C27 0.021(3) 0.016(2) 0.017(2) -0.0032(17) -0.0049(18) -0.0071(19) C28 0.021(3) 0.012(2) 0.020(2) -0.0030(16) -0.0013(18) -0.0072(18) C29 0.020(2) 0.017(2) 0.013(2) -0.0065(16) 0.0019(17) -0.0081(19) C30 0.022(3) 0.014(2) 0.017(2) -0.0042(16) -0.0014(18) -0.0067(19) C31 0.020(3) 0.023(2) 0.020(2) -0.0057(18) 0.0024(19) -0.013(2) C32 0.017(3) 0.022(2) 0.026(2) -0.0093(19) -0.0071(19) -0.0072(19) C33 0.019(3) 0.017(2) 0.022(2) -0.0014(18) -0.0077(19) -0.0021(19) C34 0.019(2) 0.018(2) 0.016(2) -0.0023(17) -0.0067(18) -0.0055(19) C35 0.031(3) 0.020(2) 0.023(2) -0.0017(19) 0.007(2) -0.010(2) C36 0.027(3) 0.015(2) 0.025(2) 0.0048(18) -0.005(2) -0.003(2) C37 0.021(3) 0.033(3) 0.030(3) -0.009(2) -0.004(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 1.930(4) . ? U1 N2 1.946(4) . ? U1 N3 2.575(4) . ? U1 N4 2.592(4) . ? U1 C21 2.654(4) . ? U1 C25 2.663(4) . ? U1 C18 2.746(4) . ? U1 C28 2.746(4) . ? U1 C26 2.828(4) . ? U1 C20 2.835(4) . ? U1 C27 2.870(4) . ? U1 C19 2.879(4) . ? N1 C1 1.471(6) . ? N2 C5 1.455(6) . ? N3 C21 1.381(6) . ? N3 C18 1.399(5) . ? N4 C25 1.377(6) . ? N4 C28 1.381(6) . ? C1 C2 1.519(7) . ? C1 C3 1.523(7) . ? C1 C4 1.526(7) . ? C5 C7 1.511(7) . ? C5 C8 1.512(7) . ? C5 C6 1.526(7) . ? C9 C14 1.409(7) . ? C9 C10 1.412(6) . ? C9 C18 1.484(6) . ? C10 C11 1.398(7) . ? C10 C15 1.518(7) . ? C11 C12 1.380(7) . ? C12 C13 1.388(7) . ? C12 C16 1.505(7) . ? C13 C14 1.404(6) . ? C14 C17 1.511(6) . ? C18 C19 1.406(6) . ? C19 C20 1.395(6) . ? C20 C21 1.404(6) . ? C21 C22 1.517(6) . ? C22 C25 1.505(6) . ? C22 C24 1.530(7) . ? C22 C23 1.537(7) . ? C25 C26 1.404(6) . ? C26 C27 1.410(6) . ? C27 C28 1.395(7) . ? C28 C29 1.484(6) . ? C29 C34 1.413(6) . ? C29 C30 1.425(6) . ? C30 C31 1.387(6) . ? C30 C35 1.492(6) . ? C31 C32 1.395(7) . ? C32 C33 1.395(7) . ? C32 C37 1.497(7) . ? C33 C34 1.386(7) . ? C34 C36 1.512(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N2 116.06(15) . . ? N1 U1 N3 91.90(14) . . ? N2 U1 N3 130.79(13) . . ? N1 U1 N4 131.47(13) . . ? N2 U1 N4 94.11(14) . . ? N3 U1 N4 95.72(12) . . ? N1 U1 C21 121.43(15) . . ? N2 U1 C21 114.18(14) . . ? N3 U1 C21 30.58(12) . . ? N4 U1 C21 70.45(12) . . ? N1 U1 C25 115.01(15) . . ? N2 U1 C25 122.85(15) . . ? N3 U1 C25 69.76(12) . . ? N4 U1 C25 30.35(13) . . ? C21 U1 C25 52.71(13) . . ? N1 U1 C18 89.10(14) . . ? N2 U1 C18 106.45(14) . . ? N3 U1 C18 30.28(12) . . ? N4 U1 C18 119.14(12) . . ? C21 U1 C18 48.77(13) . . ? C25 U1 C18 98.22(13) . . ? N1 U1 C28 107.45(14) . . ? N2 U1 C28 92.65(14) . . ? N3 U1 C28 117.79(12) . . ? N4 U1 C28 29.81(12) . . ? C21 U1 C28 98.22(13) . . ? C25 U1 C28 48.29(13) . . ? C18 U1 C28 146.27(13) . . ? N1 U1 C26 86.61(14) . . ? N2 U1 C26 139.91(14) . . ? N3 U1 C26 76.58(12) . . ? N4 U1 C26 49.47(12) . . ? C21 U1 C26 73.29(13) . . ? C25 U1 C26 29.43(13) . . ? C18 U1 C26 106.50(13) . . ? C28 U1 C26 47.72(14) . . ? N1 U1 C20 136.76(14) . . ? N2 U1 C20 85.79(14) . . ? N3 U1 C20 49.64(12) . . ? N4 U1 C20 78.63(12) . . ? C21 U1 C20 29.40(13) . . ? C25 U1 C20 73.96(13) . . ? C18 U1 C20 47.93(13) . . ? C28 U1 C20 108.23(13) . . ? C26 U1 C20 99.90(13) . . ? N1 U1 C27 82.92(14) . . ? N2 U1 C27 117.28(14) . . ? N3 U1 C27 105.09(12) . . ? N4 U1 C27 48.82(12) . . ? C21 U1 C27 99.29(13) . . ? C25 U1 C27 47.86(13) . . ? C18 U1 C27 134.53(13) . . ? C28 U1 C27 28.65(13) . . ? C26 U1 C27 28.65(13) . . ? C20 U1 C27 121.42(13) . . ? N1 U1 C19 113.93(14) . . ? N2 U1 C19 82.09(13) . . ? N3 U1 C19 48.93(12) . . ? N4 U1 C19 106.83(12) . . ? C21 U1 C19 47.60(13) . . ? C25 U1 C19 99.31(13) . . ? C18 U1 C19 28.82(13) . . ? C28 U1 C19 136.17(13) . . ? C26 U1 C19 120.19(13) . . ? C20 U1 C19 28.25(12) . . ? C27 U1 C19 146.84(13) . . ? C1 N1 U1 168.7(3) . . ? C5 N2 U1 169.3(3) . . ? C21 N3 C18 106.7(4) . . ? C21 N3 U1 77.9(2) . . ? C18 N3 U1 81.6(2) . . ? C25 N4 C28 106.7(4) . . ? C25 N4 U1 77.7(2) . . ? C28 N4 U1 81.3(2) . . ? N1 C1 C2 108.2(4) . . ? N1 C1 C3 109.0(4) . . ? C2 C1 C3 109.3(4) . . ? N1 C1 C4 109.5(4) . . ? C2 C1 C4 110.1(5) . . ? C3 C1 C4 110.7(4) . . ? N2 C5 C7 108.7(4) . . ? N2 C5 C8 109.7(4) . . ? C7 C5 C8 109.8(5) . . ? N2 C5 C6 109.9(4) . . ? C7 C5 C6 109.3(5) . . ? C8 C5 C6 109.4(5) . . ? C14 C9 C10 119.3(4) . . ? C14 C9 C18 120.8(4) . . ? C10 C9 C18 119.9(4) . . ? C11 C10 C9 119.5(5) . . ? C11 C10 C15 116.7(4) . . ? C9 C10 C15 123.8(4) . . ? C12 C11 C10 122.2(4) . . ? C11 C12 C13 117.7(4) . . ? C11 C12 C16 121.8(5) . . ? C13 C12 C16 120.5(5) . . ? C12 C13 C14 122.7(5) . . ? C13 C14 C9 118.6(4) . . ? C13 C14 C17 116.5(4) . . ? C9 C14 C17 125.0(4) . . ? N3 C18 C19 108.5(4) . . ? N3 C18 C9 120.9(4) . . ? C19 C18 C9 130.3(4) . . ? N3 C18 U1 68.1(2) . . ? C19 C18 U1 80.9(3) . . ? C9 C18 U1 121.3(3) . . ? C20 C19 C18 108.1(4) . . ? C20 C19 U1 74.1(2) . . ? C18 C19 U1 70.3(2) . . ? C19 C20 C21 106.5(4) . . ? C19 C20 U1 77.6(2) . . ? C21 C20 U1 68.1(2) . . ? N3 C21 C20 110.2(4) . . ? N3 C21 C22 118.5(4) . . ? C20 C21 C22 130.2(4) . . ? N3 C21 U1 71.6(2) . . ? C20 C21 U1 82.5(3) . . ? C22 C21 U1 102.3(3) . . ? C25 C22 C21 102.7(3) . . ? C25 C22 C24 110.3(4) . . ? C21 C22 C24 111.3(4) . . ? C25 C22 C23 112.0(4) . . ? C21 C22 C23 109.6(4) . . ? C24 C22 C23 110.6(4) . . ? N4 C25 C26 110.0(4) . . ? N4 C25 C22 119.6(4) . . ? C26 C25 C22 129.1(4) . . ? N4 C25 U1 72.0(2) . . ? C26 C25 U1 81.8(3) . . ? C22 C25 U1 102.3(3) . . ? C25 C26 C27 106.3(4) . . ? C25 C26 U1 68.8(2) . . ? C27 C26 U1 77.3(3) . . ? C28 C27 C26 107.1(4) . . ? C28 C27 U1 70.7(2) . . ? C26 C27 U1 74.0(2) . . ? N4 C28 C27 109.8(4) . . ? N4 C28 C29 121.0(4) . . ? C27 C28 C29 128.6(4) . . ? N4 C28 U1 68.9(2) . . ? C27 C28 U1 80.6(3) . . ? C29 C28 U1 123.0(3) . . ? C34 C29 C30 118.8(4) . . ? C34 C29 C28 119.1(4) . . ? C30 C29 C28 122.0(4) . . ? C31 C30 C29 118.8(4) . . ? C31 C30 C35 119.0(4) . . ? C29 C30 C35 122.2(4) . . ? C30 C31 C32 123.4(4) . . ? C33 C32 C31 116.4(4) . . ? C33 C32 C37 121.6(4) . . ? C31 C32 C37 121.9(4) . . ? C34 C33 C32 123.1(4) . . ? C33 C34 C29 119.4(4) . . ? C33 C34 C36 118.2(4) . . ? C29 C34 C36 122.3(4) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.345 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.154 # Attachment 'UNtBu2dpmmes_dmpe_.cif' data_apx794as _database_code_depnum_ccdc_archive 'CCDC 765727' #TrackingRef 'UNtBu2dpmmes_dmpe_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H73 N4 P2 U' _chemical_formula_weight 982.05 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.649(3) _cell_length_b 17.676(4) _cell_length_c 22.136(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.986(3) _cell_angle_gamma 90.00 _cell_volume 4540.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 3.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5265 _exptl_absorpt_correction_T_max 0.9300 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _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 19728 _diffrn_reflns_av_R_equivalents 0.1745 _diffrn_reflns_av_sigmaI/netI 0.2870 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.41 _reflns_number_total 8079 _reflns_number_gt 3313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (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. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 219 125 'n-hexane ' 2 0.500 1.000 0.500 219 119 'n-hexane ' _platon_squeeze_details ; ; _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^)+(0.0569P)^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 8079 _refine_ls_number_parameters 469 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1850 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.27569(5) 0.16902(3) 0.15611(3) 0.02498(19) Uani 1 1 d . . . P1 P 0.2768(4) 0.3314(3) 0.11006(19) 0.0366(11) Uani 1 1 d . . . P2 P 0.5231(4) 0.2362(2) 0.1579(2) 0.0432(13) Uani 1 1 d . . . N1 N 0.2667(10) 0.2135(7) 0.2319(5) 0.028(3) Uani 1 1 d . . . N2 N 0.3082(10) 0.1449(6) 0.0781(5) 0.027(3) Uani 1 1 d . . . N3 N 0.3150(12) 0.0432(7) 0.1914(6) 0.036(4) Uani 1 1 d . . . N4 N 0.0721(10) 0.1459(7) 0.1308(5) 0.028(3) Uani 1 1 d . . . C1 C 0.2541(14) 0.2514(8) 0.2929(6) 0.026(4) Uani 1 1 d . . . C2 C 0.1698(14) 0.2030(9) 0.3269(7) 0.041(5) Uani 1 1 d . . . H2A H 0.2011 0.1532 0.3336 0.062 Uiso 1 1 calc R . . H2B H 0.0970 0.1996 0.3031 0.062 Uiso 1 1 calc R . . H2C H 0.1588 0.2261 0.3652 0.062 Uiso 1 1 calc R . . C3 C 0.3691(14) 0.2529(10) 0.3284(7) 0.050(5) Uani 1 1 d . . . H3A H 0.4021 0.2032 0.3292 0.074 Uiso 1 1 calc R . . H3B H 0.3600 0.2691 0.3691 0.074 Uiso 1 1 calc R . . H3C H 0.4189 0.2875 0.3098 0.074 Uiso 1 1 calc R . . C4 C 0.2027(13) 0.3310(8) 0.2809(7) 0.034(4) Uani 1 1 d . . . H4A H 0.1817 0.3523 0.3183 0.051 Uiso 1 1 calc R . . H4B H 0.1357 0.3274 0.2526 0.051 Uiso 1 1 calc R . . H4C H 0.2590 0.3629 0.2643 0.051 Uiso 1 1 calc R . . C5 C 0.3139(14) 0.1053(9) 0.0206(7) 0.034(4) Uani 1 1 d U . . C6 C 0.3093(14) 0.0194(10) 0.0287(7) 0.052(5) Uani 1 1 d U . . H6A H 0.3600 0.0049 0.0632 0.077 Uiso 1 1 calc R . . H6B H 0.3331 -0.0049 -0.0069 0.077 Uiso 1 1 calc R . . H6C H 0.2320 0.0044 0.0348 0.077 Uiso 1 1 calc R . . C7 C 0.4297(13) 0.1248(9) -0.0044(7) 0.041(5) Uani 1 1 d . . . H7A H 0.4389 0.1788 -0.0053 0.061 Uiso 1 1 calc R . . H7B H 0.4306 0.1050 -0.0448 0.061 Uiso 1 1 calc R . . H7C H 0.4916 0.1029 0.0212 0.061 Uiso 1 1 calc R . . C8 C 0.2201(14) 0.1328(9) -0.0254(7) 0.042(5) Uani 1 1 d . . . H8A H 0.1463 0.1200 -0.0121 0.063 Uiso 1 1 calc R . . H8B H 0.2286 0.1093 -0.0638 0.063 Uiso 1 1 calc R . . H8C H 0.2257 0.1867 -0.0295 0.063 Uiso 1 1 calc R . . C9 C 0.4199(13) 0.0043(8) 0.1964(6) 0.022(4) Uani 1 1 d U . . C10 C 0.4040(18) -0.0689(9) 0.1768(8) 0.052(6) Uani 1 1 d . . . H10 H 0.4613 -0.1051 0.1744 0.062 Uiso 1 1 calc R . . C11 C 0.2843(16) -0.0796(8) 0.1609(7) 0.033(4) Uani 1 1 d U . . H11 H 0.2495 -0.1247 0.1475 0.040 Uiso 1 1 calc R . . C12 C 0.2276(13) -0.0109(9) 0.1687(6) 0.024(4) Uani 1 1 d U . . C13 C 0.1037(13) 0.0072(9) 0.1659(7) 0.033(4) Uani 1 1 d U . . C14 C 0.0364(16) -0.0672(9) 0.1533(8) 0.057(6) Uani 1 1 d . . . H14A H 0.0486 -0.0852 0.1134 0.085 Uiso 1 1 calc R . . H14B H -0.0443 -0.0583 0.1559 0.085 Uiso 1 1 calc R . . H14C H 0.0631 -0.1045 0.1828 0.085 Uiso 1 1 calc R . . C15 C 0.0772(14) 0.0375(9) 0.2294(7) 0.042(5) Uani 1 1 d . . . H15A H 0.1099 0.0038 0.2604 0.063 Uiso 1 1 calc R . . H15B H -0.0047 0.0403 0.2314 0.063 Uiso 1 1 calc R . . H15C H 0.1101 0.0870 0.2357 0.063 Uiso 1 1 calc R . . C16 C 0.0596(15) 0.0668(10) 0.1209(7) 0.038(5) Uani 1 1 d U . . C17 C -0.0259(14) 0.0575(10) 0.0750(8) 0.042(5) Uani 1 1 d . . . H17 H -0.0545 0.0107 0.0618 0.050 Uiso 1 1 calc R . . C18 C -0.0660(14) 0.1278(9) 0.0499(8) 0.045(5) Uani 1 1 d U . . H18 H -0.1211 0.1373 0.0179 0.054 Uiso 1 1 calc R . . C19 C -0.0006(12) 0.1781(10) 0.0861(7) 0.034(4) Uani 1 1 d U . . C20 C 0.5250(13) 0.0358(8) 0.2302(7) 0.030(4) Uani 1 1 d U . . C21 C 0.6331(14) 0.0352(8) 0.2045(6) 0.027(4) Uani 1 1 d . . . C22 C 0.7292(13) 0.0613(8) 0.2395(7) 0.030(4) Uani 1 1 d U . . H22 H 0.7996 0.0625 0.2226 0.036 Uiso 1 1 calc R . . C23 C 0.7248(14) 0.0851(9) 0.2975(7) 0.033(4) Uani 1 1 d U . . C24 C 0.6209(15) 0.0804(9) 0.3238(7) 0.033(4) Uani 1 1 d U . . H24 H 0.6188 0.0931 0.3644 0.040 Uiso 1 1 calc R . . C25 C 0.5202(15) 0.0573(9) 0.2910(7) 0.032(4) Uani 1 1 d . . . C26 C 0.6412(14) 0.0058(9) 0.1405(7) 0.044(5) Uani 1 1 d . . . H26A H 0.7101 0.0248 0.1250 0.066 Uiso 1 1 calc R . . H26B H 0.5752 0.0224 0.1149 0.066 Uiso 1 1 calc R . . H26C H 0.6433 -0.0485 0.1411 0.066 Uiso 1 1 calc R . . C27 C 0.8294(13) 0.1150(10) 0.3346(7) 0.046(5) Uani 1 1 d . . . H27A H 0.8962 0.0872 0.3250 0.069 Uiso 1 1 calc R . . H27B H 0.8193 0.1094 0.3769 0.069 Uiso 1 1 calc R . . H27C H 0.8394 0.1676 0.3254 0.069 Uiso 1 1 calc R . . C28 C 0.4122(13) 0.0469(8) 0.3213(7) 0.037(5) Uani 1 1 d . . . H28A H 0.4259 0.0597 0.3635 0.055 Uiso 1 1 calc R . . H28B H 0.3878 -0.0049 0.3175 0.055 Uiso 1 1 calc R . . H28C H 0.3531 0.0792 0.3025 0.055 Uiso 1 1 calc R . . C29 C -0.0352(15) 0.2618(10) 0.0873(9) 0.045(5) Uani 1 1 d . . . C30 C -0.0440(15) 0.3069(9) 0.0323(7) 0.040(5) Uani 1 1 d U . . C31 C -0.0857(15) 0.3799(10) 0.0370(8) 0.054(6) Uani 1 1 d . . . H31 H -0.0923 0.4099 0.0024 0.065 Uiso 1 1 calc R . . C32 C -0.1178(17) 0.4102(10) 0.0900(9) 0.052(5) Uani 1 1 d . . . C33 C -0.1116(15) 0.3701(10) 0.1412(8) 0.043(5) Uani 1 1 d . . . H33 H -0.1348 0.3913 0.1766 0.052 Uiso 1 1 calc R . . C34 C -0.0696(13) 0.2955(9) 0.1411(7) 0.027(4) Uani 1 1 d . . . C35 C -0.0212(18) 0.2740(12) -0.0273(7) 0.077(7) Uani 1 1 d . . . H35A H -0.0900 0.2503 -0.0454 0.115 Uiso 1 1 calc R . . H35B H 0.0391 0.2370 -0.0216 0.115 Uiso 1 1 calc R . . H35C H 0.0020 0.3134 -0.0535 0.115 Uiso 1 1 calc R . . C36 C -0.1528(17) 0.4924(10) 0.0915(7) 0.064(6) Uani 1 1 d . . . H36A H -0.1954 0.5055 0.0538 0.096 Uiso 1 1 calc R . . H36B H -0.0852 0.5235 0.0973 0.096 Uiso 1 1 calc R . . H36C H -0.2002 0.5005 0.1243 0.096 Uiso 1 1 calc R . . C37 C -0.0694(13) 0.2493(8) 0.1994(6) 0.030(4) Uani 1 1 d . . . H37A H -0.1188 0.2061 0.1924 0.045 Uiso 1 1 calc R . . H37B H -0.0969 0.2800 0.2308 0.045 Uiso 1 1 calc R . . H37C H 0.0076 0.2326 0.2115 0.045 Uiso 1 1 calc R . . C38 C 0.4145(15) 0.3766(9) 0.1355(9) 0.056(6) Uani 1 1 d . . . H38A H 0.4178 0.4263 0.1171 0.068 Uiso 1 1 calc R . . H38B H 0.4194 0.3832 0.1791 0.068 Uiso 1 1 calc R . . C39 C 0.5125(17) 0.3311(11) 0.1190(10) 0.082(7) Uani 1 1 d . . . H39A H 0.5831 0.3590 0.1294 0.099 Uiso 1 1 calc R . . H39B H 0.5054 0.3232 0.0755 0.099 Uiso 1 1 calc R . . C40 C 0.1849(13) 0.4091(8) 0.1287(7) 0.041(5) Uani 1 1 d . . . H40A H 0.2004 0.4523 0.1045 0.062 Uiso 1 1 calc R . . H40B H 0.2000 0.4215 0.1708 0.062 Uiso 1 1 calc R . . H40C H 0.1057 0.3946 0.1206 0.062 Uiso 1 1 calc R . . C41 C 0.2718(15) 0.3408(10) 0.0259(7) 0.057(6) Uani 1 1 d . . . H41A H 0.1979 0.3245 0.0081 0.086 Uiso 1 1 calc R . . H41B H 0.3310 0.3100 0.0110 0.086 Uiso 1 1 calc R . . H41C H 0.2839 0.3927 0.0155 0.086 Uiso 1 1 calc R . . C42 C 0.6383(15) 0.1976(10) 0.1154(8) 0.053(5) Uani 1 1 d . . . H42A H 0.6865 0.2380 0.1035 0.079 Uiso 1 1 calc R . . H42B H 0.6049 0.1719 0.0799 0.079 Uiso 1 1 calc R . . H42C H 0.6837 0.1625 0.1405 0.079 Uiso 1 1 calc R . . C43 C 0.6033(13) 0.2550(10) 0.2299(8) 0.050(5) Uani 1 1 d . . . H43A H 0.6359 0.3049 0.2294 0.075 Uiso 1 1 calc R . . H43B H 0.6640 0.2184 0.2367 0.075 Uiso 1 1 calc R . . H43C H 0.5527 0.2516 0.2618 0.075 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 0.0209(4) 0.0231(3) 0.0301(3) -0.0020(4) -0.0023(2) 0.0016(4) P1 0.034(3) 0.028(2) 0.047(3) 0.005(3) 0.000(2) 0.008(3) P2 0.030(3) 0.027(3) 0.069(4) 0.006(2) -0.016(3) -0.002(2) N1 0.018(8) 0.040(8) 0.026(7) 0.007(6) 0.002(6) -0.007(6) N2 0.023(8) 0.036(8) 0.021(7) 0.001(6) -0.004(6) 0.009(6) N3 0.043(10) 0.028(8) 0.034(8) 0.001(7) -0.010(7) 0.007(8) N4 0.019(8) 0.028(8) 0.033(8) 0.001(6) -0.016(6) -0.006(6) C1 0.026(11) 0.036(10) 0.015(8) -0.003(7) -0.002(8) -0.005(8) C2 0.033(11) 0.061(12) 0.031(10) -0.013(9) 0.006(9) -0.016(10) C3 0.033(12) 0.069(13) 0.045(11) -0.023(10) -0.002(10) 0.020(11) C4 0.026(10) 0.023(8) 0.052(10) 0.009(9) 0.002(8) -0.008(9) C5 0.025(11) 0.043(10) 0.032(9) 0.013(8) -0.014(8) 0.009(8) C6 0.042(13) 0.083(15) 0.025(9) -0.027(10) -0.023(9) 0.016(11) C7 0.032(12) 0.049(11) 0.040(11) -0.003(9) -0.008(9) 0.000(9) C8 0.042(12) 0.043(10) 0.038(10) -0.016(9) -0.012(9) 0.006(9) C9 0.016(9) 0.024(8) 0.025(8) 0.013(7) 0.005(7) 0.004(7) C10 0.071(17) 0.022(10) 0.066(14) 0.007(9) 0.030(12) 0.014(10) C11 0.043(8) 0.019(6) 0.038(7) -0.015(6) 0.004(7) -0.009(7) C12 0.023(10) 0.033(9) 0.016(8) 0.002(7) -0.009(7) 0.014(8) C13 0.020(10) 0.039(10) 0.039(10) 0.005(8) -0.007(8) -0.005(8) C14 0.073(16) 0.031(10) 0.066(14) 0.010(10) 0.007(12) -0.015(10) C15 0.027(11) 0.045(11) 0.052(12) 0.000(9) -0.008(9) -0.002(9) C16 0.029(11) 0.047(11) 0.034(10) 0.010(8) -0.014(9) 0.021(9) C17 0.014(11) 0.053(12) 0.059(13) -0.004(10) 0.009(10) 0.011(9) C18 0.028(11) 0.044(11) 0.058(12) 0.000(9) -0.021(9) -0.017(9) C19 0.008(8) 0.059(11) 0.036(9) -0.024(9) 0.001(7) -0.006(9) C20 0.012(9) 0.034(9) 0.045(10) -0.001(8) 0.007(8) 0.008(8) C21 0.023(11) 0.033(9) 0.023(9) -0.003(7) -0.006(8) 0.015(8) C22 0.010(9) 0.041(10) 0.039(10) -0.005(8) -0.005(8) -0.003(8) C23 0.020(10) 0.035(9) 0.039(10) 0.015(8) -0.018(9) -0.016(8) C24 0.032(11) 0.040(10) 0.028(9) 0.013(8) 0.003(9) 0.007(9) C25 0.026(11) 0.037(10) 0.035(10) 0.000(8) 0.017(9) -0.001(9) C26 0.042(12) 0.045(11) 0.048(11) 0.001(9) 0.015(10) 0.006(10) C27 0.024(11) 0.076(14) 0.035(10) -0.008(10) -0.007(9) -0.006(10) C28 0.031(11) 0.043(10) 0.036(10) -0.021(8) -0.005(9) 0.023(9) C29 0.022(12) 0.041(11) 0.069(14) -0.001(10) -0.015(10) 0.014(9) C30 0.044(9) 0.049(8) 0.023(7) 0.003(6) -0.010(7) 0.007(7) C31 0.058(14) 0.067(14) 0.034(11) -0.018(10) -0.018(10) 0.051(11) C32 0.055(15) 0.037(11) 0.062(14) 0.007(10) 0.002(11) 0.027(10) C33 0.043(13) 0.040(11) 0.047(12) -0.008(10) 0.008(10) 0.022(10) C34 0.017(10) 0.044(10) 0.018(9) -0.010(8) -0.010(7) 0.002(8) C35 0.081(18) 0.121(19) 0.029(11) -0.014(12) 0.010(12) 0.042(15) C36 0.098(18) 0.059(13) 0.036(11) -0.014(10) 0.007(11) 0.042(13) C37 0.016(10) 0.043(10) 0.031(9) -0.009(8) 0.001(8) -0.001(8) C38 0.036(13) 0.019(10) 0.114(18) -0.006(10) 0.006(12) 0.018(9) C39 0.066(16) 0.041(12) 0.13(2) 0.037(14) -0.023(14) -0.038(13) C40 0.018(11) 0.037(10) 0.065(12) 0.013(9) -0.016(9) 0.009(8) C41 0.060(14) 0.063(13) 0.048(11) 0.008(11) 0.006(10) -0.028(12) C42 0.038(13) 0.059(13) 0.060(13) -0.008(10) 0.006(10) -0.012(10) C43 0.010(10) 0.072(13) 0.067(13) -0.029(11) 0.001(10) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N2 1.849(11) . ? U1 N1 1.864(12) . ? U1 N3 2.388(12) . ? U1 N4 2.424(12) . ? U1 P1 3.047(5) . ? U1 P2 3.114(5) . ? P1 C40 1.810(15) . ? P1 C38 1.836(18) . ? P1 C41 1.865(15) . ? P2 C43 1.806(17) . ? P2 C42 1.837(16) . ? P2 C39 1.884(18) . ? N1 C1 1.525(17) . ? N2 C5 1.460(18) . ? N3 C9 1.398(17) . ? N3 C12 1.454(18) . ? N4 C19 1.369(19) . ? N4 C16 1.422(19) . ? C1 C3 1.49(2) . ? C1 C4 1.542(19) . ? C1 C2 1.547(19) . ? C5 C8 1.51(2) . ? C5 C6 1.53(2) . ? C5 C7 1.54(2) . ? C9 C10 1.37(2) . ? C9 C20 1.49(2) . ? C10 C11 1.42(2) . ? C11 C12 1.402(19) . ? C12 C13 1.474(19) . ? C13 C16 1.51(2) . ? C13 C14 1.55(2) . ? C13 C15 1.56(2) . ? C16 C17 1.37(2) . ? C17 C18 1.42(2) . ? C18 C19 1.38(2) . ? C19 C29 1.53(2) . ? C20 C25 1.40(2) . ? C20 C21 1.427(18) . ? C21 C22 1.38(2) . ? C21 C26 1.520(19) . ? C22 C23 1.36(2) . ? C23 C24 1.39(2) . ? C23 C27 1.50(2) . ? C24 C25 1.39(2) . ? C25 C28 1.488(19) . ? C29 C34 1.42(2) . ? C29 C30 1.45(2) . ? C30 C31 1.39(2) . ? C30 C35 1.49(2) . ? C31 C32 1.37(2) . ? C32 C33 1.33(2) . ? C32 C36 1.51(2) . ? C33 C34 1.41(2) . ? C34 C37 1.526(19) . ? C38 C39 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 N2 U1 N1 165.9(5) . . ? N2 U1 N3 92.4(5) . . ? N1 U1 N3 97.0(5) . . ? N2 U1 N4 91.2(5) . . ? N1 U1 N4 98.6(5) . . ? N3 U1 N4 94.3(4) . . ? N2 U1 P1 84.1(4) . . ? N1 U1 P1 84.6(4) . . ? N3 U1 P1 168.7(3) . . ? N4 U1 P1 96.5(3) . . ? N2 U1 P2 80.5(4) . . ? N1 U1 P2 87.2(4) . . ? N3 U1 P2 101.5(3) . . ? N4 U1 P2 162.4(3) . . ? P1 U1 P2 67.30(12) . . ? C40 P1 C38 96.8(7) . . ? C40 P1 C41 101.1(8) . . ? C38 P1 C41 102.6(9) . . ? C40 P1 U1 128.2(5) . . ? C38 P1 U1 109.7(6) . . ? C41 P1 U1 114.6(6) . . ? C43 P2 C42 100.1(8) . . ? C43 P2 C39 104.4(9) . . ? C42 P2 C39 96.8(9) . . ? C43 P2 U1 119.3(6) . . ? C42 P2 U1 124.6(6) . . ? C39 P2 U1 108.0(6) . . ? C1 N1 U1 177.4(11) . . ? C5 N2 U1 162.5(10) . . ? C9 N3 C12 106.5(12) . . ? C9 N3 U1 128.7(10) . . ? C12 N3 U1 113.0(9) . . ? C19 N4 C16 104.3(12) . . ? C19 N4 U1 128.9(10) . . ? C16 N4 U1 106.7(10) . . ? C3 C1 N1 108.8(12) . . ? C3 C1 C4 113.0(13) . . ? N1 C1 C4 108.4(12) . . ? C3 C1 C2 109.3(13) . . ? N1 C1 C2 107.6(11) . . ? C4 C1 C2 109.6(13) . . ? N2 C5 C8 110.4(13) . . ? N2 C5 C6 111.6(12) . . ? C8 C5 C6 111.6(14) . . ? N2 C5 C7 108.3(13) . . ? C8 C5 C7 106.9(13) . . ? C6 C5 C7 107.8(14) . . ? C10 C9 N3 110.2(15) . . ? C10 C9 C20 126.5(16) . . ? N3 C9 C20 122.1(13) . . ? C9 C10 C11 107.9(15) . . ? C12 C11 C10 108.5(14) . . ? C11 C12 N3 106.8(13) . . ? C11 C12 C13 130.8(16) . . ? N3 C12 C13 121.7(13) . . ? C12 C13 C16 117.2(13) . . ? C12 C13 C14 107.6(14) . . ? C16 C13 C14 109.7(14) . . ? C12 C13 C15 107.8(13) . . ? C16 C13 C15 105.9(13) . . ? C14 C13 C15 108.5(13) . . ? C17 C16 N4 106.9(14) . . ? C17 C16 C13 126.2(17) . . ? N4 C16 C13 124.0(14) . . ? C16 C17 C18 112.2(16) . . ? C19 C18 C17 100.9(16) . . ? N4 C19 C18 115.3(16) . . ? N4 C19 C29 122.3(14) . . ? C18 C19 C29 119.9(15) . . ? C25 C20 C21 119.6(15) . . ? C25 C20 C9 119.0(14) . . ? C21 C20 C9 120.9(14) . . ? C22 C21 C20 118.3(14) . . ? C22 C21 C26 121.5(15) . . ? C20 C21 C26 120.2(14) . . ? C23 C22 C21 122.5(15) . . ? C22 C23 C24 118.9(15) . . ? C22 C23 C27 122.0(15) . . ? C24 C23 C27 119.1(15) . . ? C25 C24 C23 121.8(15) . . ? C24 C25 C20 118.7(15) . . ? C24 C25 C28 120.7(14) . . ? C20 C25 C28 120.3(15) . . ? C34 C29 C30 118.0(15) . . ? C34 C29 C19 120.8(16) . . ? C30 C29 C19 120.9(15) . . ? C31 C30 C29 116.6(15) . . ? C31 C30 C35 121.4(16) . . ? C29 C30 C35 121.7(15) . . ? C32 C31 C30 123.5(17) . . ? C33 C32 C31 121.4(16) . . ? C33 C32 C36 119.1(16) . . ? C31 C32 C36 119.3(16) . . ? C32 C33 C34 119.4(16) . . ? C33 C34 C29 121.1(16) . . ? C33 C34 C37 118.4(14) . . ? C29 C34 C37 120.3(14) . . ? C39 C38 P1 111.2(12) . . ? C38 C39 P2 113.4(13) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.864 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.234 # Attachment 'UNtBu2dpmthf2.cif' data_apx801a _database_code_depnum_ccdc_archive 'CCDC 765728' #TrackingRef 'UNtBu2dpmthf2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H46 I0 N4 O2 U' _chemical_formula_weight 696.71 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.189(8) _cell_length_b 14.566(7) _cell_length_c 11.246(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2816(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 5.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2586 _exptl_absorpt_correction_T_max 0.7225 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 26633 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.75 _reflns_number_total 2793 _reflns_number_gt 2306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (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. There was a 12.1(2) percent substitional disorder of iodide at the bis pyrrole ligand site. ; _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^)+(0.0440P)^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 2793 _refine_ls_number_parameters 197 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.407266(15) 0.2500 1.02226(3) 0.01952(12) Uani 1 2 d S . . I1 I 0.3893(6) 0.0833(7) 0.8701(7) 0.062(3) Uani 0.121(3) 1 d P A 1 N1 N 0.5152(4) 0.2500 1.0213(5) 0.0209(14) Uani 1 2 d S A . N2 N 0.3002(3) 0.2500 1.0438(5) 0.0208(14) Uani 1 2 d S A . N3 N 0.3966(3) 0.1529(5) 0.8555(4) 0.0247(12) Uani 0.879(3) 1 d PD A 2 O1 O 0.4154(2) 0.1323(3) 1.1787(4) 0.0322(10) Uani 1 1 d . A . C1 C 0.3682(8) 0.0669(8) 0.8906(11) 0.033(4) Uani 0.879(3) 1 d PD A 2 C2 C 0.3326(4) 0.0241(5) 0.7948(7) 0.0368(18) Uani 0.879(3) 1 d PD A 2 C3 C 0.3378(4) 0.0859(5) 0.6989(6) 0.0307(16) Uani 0.879(3) 1 d P A 2 C4 C 0.3754(4) 0.1632(4) 0.7374(5) 0.0244(14) Uani 0.879(3) 1 d PD A 2 C5 C 0.3972(5) 0.2500 0.6710(9) 0.042(2) Uani 1 2 d S . . C6 C 0.4848(5) 0.2500 0.6449(10) 0.051(3) Uani 1 2 d S A . H6A H 0.5131 0.2500 0.7184 0.076 Uiso 1 2 calc SR . . H6B H 0.4980 0.3038 0.5999 0.076 Uiso 0.50 1 calc PR . . H6C H 0.4980 0.1962 0.5999 0.076 Uiso 0.50 1 calc PR . . C7 C 0.3559(7) 0.2500 0.5512(10) 0.064(3) Uani 1 2 d S A . H7A H 0.3006 0.2500 0.5636 0.096 Uiso 1 2 calc SR . . H7B H 0.3705 0.1962 0.5072 0.096 Uiso 0.50 1 calc PR . . H7C H 0.3705 0.3038 0.5072 0.096 Uiso 0.50 1 calc PR . . C8 C 0.5985(4) 0.2500 0.9901(7) 0.0252(18) Uani 1 2 d S . . C9 C 0.6164(3) 0.1640(4) 0.9193(6) 0.0315(14) Uani 1 1 d . A . H9A H 0.6044 0.1108 0.9663 0.047 Uiso 1 1 calc R . . H9B H 0.6706 0.1633 0.8986 0.047 Uiso 1 1 calc R . . H9C H 0.5856 0.1634 0.8481 0.047 Uiso 1 1 calc R . . C10 C 0.6455(5) 0.2500 1.1038(8) 0.041(2) Uani 1 2 d S A . H10A H 0.6341 0.1955 1.1484 0.061 Uiso 0.50 1 calc PR . . H10B H 0.6323 0.3031 1.1502 0.061 Uiso 0.50 1 calc PR . . H10C H 0.6999 0.2515 1.0848 0.061 Uiso 1 2 calc SR . . C11 C 0.2165(5) 0.2500 1.0104(7) 0.0250(18) Uani 1 2 d S . . C12 C 0.2081(4) 0.2500 0.8747(7) 0.0311(19) Uani 1 2 d S A . H12A H 0.2314 0.3046 0.8428 0.047 Uiso 0.50 1 calc PR . . H12B H 0.1539 0.2484 0.8540 0.047 Uiso 1 2 calc SR . . H12C H 0.2337 0.1970 0.8425 0.047 Uiso 0.50 1 calc PR . . C13 C 0.1799(3) 0.1634(4) 1.0620(5) 0.0323(14) Uani 1 1 d . A . H13A H 0.1853 0.1638 1.1469 0.048 Uiso 1 1 calc R . . H13B H 0.2057 0.1104 1.0300 0.048 Uiso 1 1 calc R . . H13C H 0.1257 0.1614 1.0414 0.048 Uiso 1 1 calc R . . C14 C 0.4871(14) 0.1116(17) 1.245(2) 0.077(9) Uani 0.50 1 d P A 1 H14A H 0.5245 0.0822 1.1929 0.093 Uiso 0.50 1 calc PR A 1 H14B H 0.5099 0.1681 1.2745 0.093 Uiso 0.50 1 calc PR A 1 C14' C 0.4820(11) 0.0727(12) 1.201(2) 0.035(5) Uani 0.50 1 d P A 2 H14C H 0.4874 0.0273 1.1381 0.042 Uiso 0.50 1 calc PR A 2 H14D H 0.5297 0.1080 1.2062 0.042 Uiso 0.50 1 calc PR A 2 C15 C 0.470(2) 0.053(3) 1.341(4) 0.055(10) Uani 0.50 1 d P A 1 H15A H 0.4768 0.0853 1.4160 0.066 Uiso 0.50 1 calc PR A 1 H15B H 0.5043 0.0002 1.3405 0.066 Uiso 0.50 1 calc PR A 1 C15' C 0.463(2) 0.029(2) 1.315(4) 0.052(9) Uani 0.50 1 d P A 2 H15C H 0.4839 0.0653 1.3798 0.062 Uiso 0.50 1 calc PR A 2 H15D H 0.4859 -0.0317 1.3185 0.062 Uiso 0.50 1 calc PR A 2 C16 C 0.3836(4) 0.0229(4) 1.3249(6) 0.0410(16) Uani 1 1 d . . . H16A H 0.3807 -0.0384 1.2915 0.049 Uiso 1 1 calc R A 1 H16B H 0.3564 0.0236 1.4004 0.049 Uiso 1 1 calc R A 1 C17 C 0.3492(3) 0.0916(4) 1.2414(6) 0.0369(16) Uani 1 1 d . A . H17A H 0.3142 0.0619 1.1858 0.044 Uiso 1 1 calc R . . H17B H 0.3206 0.1382 1.2849 0.044 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 0.01974(18) 0.01755(17) 0.02127(19) 0.000 -0.00073(12) 0.000 I1 0.059(6) 0.057(6) 0.069(5) -0.035(4) 0.012(3) -0.001(3) N1 0.023(3) 0.020(3) 0.019(3) 0.000 -0.002(3) 0.000 N2 0.017(3) 0.019(3) 0.027(4) 0.000 -0.001(3) 0.000 N3 0.028(3) 0.016(3) 0.030(4) -0.001(2) 0.000(2) 0.001(2) O1 0.019(2) 0.033(2) 0.044(3) 0.018(2) 0.0025(17) 0.0005(17) C1 0.025(7) 0.023(6) 0.051(7) -0.003(4) 0.015(5) 0.006(4) C2 0.027(4) 0.030(4) 0.053(5) -0.019(4) 0.001(3) 0.005(3) C3 0.022(3) 0.033(4) 0.037(4) -0.012(3) -0.003(3) 0.007(3) C4 0.020(3) 0.028(4) 0.025(4) -0.004(3) 0.004(3) 0.004(3) C5 0.030(5) 0.066(7) 0.030(5) 0.000 -0.009(4) 0.000 C6 0.030(5) 0.062(7) 0.061(7) 0.000 0.001(5) 0.000 C7 0.053(7) 0.091(9) 0.049(8) 0.000 -0.007(6) 0.000 C8 0.023(4) 0.028(5) 0.025(5) 0.000 0.004(3) 0.000 C9 0.024(3) 0.032(3) 0.039(4) -0.001(3) 0.004(3) 0.005(2) C10 0.020(4) 0.061(6) 0.041(6) 0.000 -0.011(4) 0.000 C11 0.018(4) 0.029(4) 0.028(5) 0.000 0.004(3) 0.000 C12 0.021(4) 0.041(5) 0.032(5) 0.000 -0.003(4) 0.000 C13 0.026(3) 0.038(4) 0.032(3) 0.006(3) 0.001(3) -0.006(3) C14 0.039(10) 0.10(2) 0.09(2) 0.061(16) -0.013(13) 0.011(15) C14' 0.013(7) 0.030(10) 0.061(15) 0.019(7) 0.014(8) 0.019(7) C15 0.033(11) 0.07(2) 0.064(18) 0.038(14) -0.006(12) -0.027(12) C15' 0.042(15) 0.042(14) 0.070(18) 0.037(13) -0.030(11) 0.005(13) C16 0.051(4) 0.030(3) 0.042(4) 0.011(3) 0.007(3) -0.004(3) C17 0.033(4) 0.040(4) 0.037(4) 0.014(3) 0.008(3) -0.010(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 U1 N2 1.856(6) . ? U1 N1 1.856(7) . ? U1 N3 2.356(6) 7_565 ? U1 N3 2.356(6) . ? U1 O1 2.461(4) 7_565 ? U1 O1 2.461(4) . ? U1 I1 2.987(8) 7_565 ? U1 I1 2.987(8) . ? N1 C8 1.473(10) . ? N2 C11 1.489(10) . ? N3 C4 1.385(6) . ? N3 C1 1.401(9) . ? O1 C14' 1.46(2) . ? O1 C17 1.464(6) . ? O1 C14 1.47(3) . ? C1 C2 1.388(9) . ? C2 C3 1.407(10) . ? C3 C4 1.368(9) . ? C4 C5 1.515(8) . ? C5 C4 1.515(8) 7_565 ? C5 C7 1.523(13) . ? C5 C6 1.534(12) . ? C8 C10 1.512(11) . ? C8 C9 1.516(7) . ? C8 C9 1.516(7) 7_565 ? C11 C13 1.524(7) . ? C11 C13 1.524(7) 7_565 ? C11 C12 1.532(11) . ? C14 C15 1.40(5) . ? C14' C15' 1.47(5) . ? C15 C16 1.56(4) . ? C15' C16 1.37(4) . ? C16 C17 1.493(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 N2 U1 N1 172.8(3) . . ? N2 U1 N3 91.52(19) . 7_565 ? N1 U1 N3 94.23(19) . 7_565 ? N2 U1 N3 91.52(19) . . ? N1 U1 N3 94.23(19) . . ? N3 U1 N3 73.8(3) 7_565 . ? N2 U1 O1 87.87(16) . 7_565 ? N1 U1 O1 86.97(15) . 7_565 ? N3 U1 O1 98.96(19) 7_565 7_565 ? N3 U1 O1 172.67(17) . 7_565 ? N2 U1 O1 87.87(16) . . ? N1 U1 O1 86.97(15) . . ? N3 U1 O1 172.67(17) 7_565 . ? N3 U1 O1 98.96(19) . . ? O1 U1 O1 88.3(2) 7_565 . ? N2 U1 I1 88.4(2) . 7_565 ? N1 U1 I1 95.7(2) . 7_565 ? N3 U1 I1 17.8(2) 7_565 7_565 ? N3 U1 I1 91.4(2) . 7_565 ? O1 U1 I1 81.3(2) 7_565 7_565 ? O1 U1 I1 169.1(2) . 7_565 ? N2 U1 I1 88.4(2) . . ? N1 U1 I1 95.7(2) . . ? N3 U1 I1 91.4(2) 7_565 . ? N3 U1 I1 17.8(2) . . ? O1 U1 I1 169.1(2) 7_565 . ? O1 U1 I1 81.3(2) . . ? I1 U1 I1 108.8(4) 7_565 . ? C8 N1 U1 166.5(5) . . ? C11 N2 U1 157.8(5) . . ? C4 N3 C1 106.0(7) . . ? C4 N3 U1 136.0(5) . . ? C1 N3 U1 109.8(6) . . ? C14' O1 C17 106.7(10) . . ? C14' O1 C14 30.1(11) . . ? C17 O1 C14 108.8(12) . . ? C14' O1 U1 125.5(10) . . ? C17 O1 U1 125.6(3) . . ? C14 O1 U1 123.6(11) . . ? C2 C1 N3 109.6(9) . . ? C1 C2 C3 106.2(7) . . ? C4 C3 C2 108.4(6) . . ? C3 C4 N3 109.7(6) . . ? C3 C4 C5 130.4(6) . . ? N3 C4 C5 119.8(6) . . ? C4 C5 C4 113.0(8) 7_565 . ? C4 C5 C7 108.7(5) 7_565 . ? C4 C5 C7 108.7(5) . . ? C4 C5 C6 109.7(5) 7_565 . ? C4 C5 C6 109.7(5) . . ? C7 C5 C6 106.8(8) . . ? N1 C8 C10 108.5(6) . . ? N1 C8 C9 108.8(4) . . ? C10 C8 C9 109.6(4) . . ? N1 C8 C9 108.8(4) . 7_565 ? C10 C8 C9 109.6(4) . 7_565 ? C9 C8 C9 111.4(7) . 7_565 ? N2 C11 C13 107.6(4) . . ? N2 C11 C13 107.6(4) . 7_565 ? C13 C11 C13 111.7(7) . 7_565 ? N2 C11 C12 110.0(6) . . ? C13 C11 C12 109.9(4) . . ? C13 C11 C12 109.9(4) 7_565 . ? C15 C14 O1 110(2) . . ? C15' C14' O1 103.3(19) . . ? C14 C15 C16 106(3) . . ? C14' C15' C16 109(2) . . ? C15' C16 C17 107.3(15) . . ? C15' C16 C15 17(3) . . ? C17 C16 C15 105.2(15) . . ? O1 C17 C16 105.5(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.871 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.139 # Attachment 'UNtBu2pyr2tppo2.cif' data_apx615s _database_code_depnum_ccdc_archive 'CCDC 765729' #TrackingRef 'UNtBu2pyr2tppo2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H68 Cl4 N4 O2 P2 U' _chemical_formula_weight 1294.93 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 17.705(2) _cell_length_b 19.068(3) _cell_length_c 16.984(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.5310(10) _cell_angle_gamma 90.00 _cell_volume 5369.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 3.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6529 _exptl_absorpt_correction_T_max 0.7319 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 27712 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.56 _reflns_number_total 5550 _reflns_number_gt 4828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (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. ; _platon_squeeze_details ; Eight disordered dichloromethane solvent molecules per cell were squeezed. ; _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^)+(0.0397P)^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 5550 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.5000 0.322289(10) 0.7500 0.02133(7) Uani 1 2 d S . . P1 P 0.62992(6) 0.28376(5) 0.61321(6) 0.0253(2) Uani 1 1 d . . . N1 N 0.40495(18) 0.32952(15) 0.65974(19) 0.0265(7) Uani 1 1 d . . . N2 N 0.5000 0.4512(2) 0.7500 0.0318(10) Uani 1 2 d S . . N3 N 0.5000 0.1925(2) 0.7500 0.0253(10) Uani 1 2 d S . . O1 O 0.57984(15) 0.30701(12) 0.66379(15) 0.0279(6) Uani 1 1 d . . . C1 C 0.5669(2) 0.25830(19) 0.5094(2) 0.0278(8) Uani 1 1 d . . . C2 C 0.5896(3) 0.2087(2) 0.4625(2) 0.0376(10) Uani 1 1 d . . . H2 H 0.6392 0.1863 0.4851 0.045 Uiso 1 1 calc R . . C3 C 0.5390(3) 0.1923(2) 0.3827(3) 0.0491(12) Uani 1 1 d . . . H3 H 0.5544 0.1585 0.3517 0.059 Uiso 1 1 calc R . . C4 C 0.4655(3) 0.2256(2) 0.3481(3) 0.0412(10) Uani 1 1 d . . . H4 H 0.4318 0.2143 0.2940 0.049 Uiso 1 1 calc R . . C5 C 0.4421(2) 0.2751(2) 0.3930(2) 0.0375(10) Uani 1 1 d . . . H5 H 0.3926 0.2975 0.3693 0.045 Uiso 1 1 calc R . . C6 C 0.4918(2) 0.2916(2) 0.4736(2) 0.0329(9) Uani 1 1 d . . . H6 H 0.4756 0.3250 0.5043 0.039 Uiso 1 1 calc R . . C7 C 0.6945(2) 0.2114(2) 0.6608(2) 0.0283(8) Uani 1 1 d . . . C8 C 0.7675(2) 0.2006(2) 0.6495(2) 0.0322(9) Uani 1 1 d . . . H8 H 0.7844 0.2316 0.6168 0.039 Uiso 1 1 calc R . . C9 C 0.8149(2) 0.1441(2) 0.6868(2) 0.0373(10) Uani 1 1 d . . . H9 H 0.8639 0.1369 0.6793 0.045 Uiso 1 1 calc R . . C10 C 0.7900(2) 0.0981(2) 0.7351(3) 0.0373(10) Uani 1 1 d . . . H10 H 0.8219 0.0596 0.7595 0.045 Uiso 1 1 calc R . . C11 C 0.7181(2) 0.1087(2) 0.7476(3) 0.0411(10) Uani 1 1 d . . . H11 H 0.7021 0.0780 0.7813 0.049 Uiso 1 1 calc R . . C12 C 0.6692(2) 0.1654(2) 0.7098(3) 0.0356(10) Uani 1 1 d . . . H12 H 0.6201 0.1722 0.7173 0.043 Uiso 1 1 calc R . . C13 C 0.6947(2) 0.3522(2) 0.6004(2) 0.0270(8) Uani 1 1 d . . . C14 C 0.6803(3) 0.3847(2) 0.5243(3) 0.0371(10) Uani 1 1 d . . . H14 H 0.6370 0.3706 0.4774 0.045 Uiso 1 1 calc R . . C15 C 0.7300(3) 0.4383(2) 0.5172(3) 0.0483(12) Uani 1 1 d . . . H15 H 0.7206 0.4595 0.4653 0.058 Uiso 1 1 calc R . . C16 C 0.7928(3) 0.4605(2) 0.5858(3) 0.0436(11) Uani 1 1 d . . . H16 H 0.8252 0.4973 0.5807 0.052 Uiso 1 1 calc R . . C17 C 0.8083(2) 0.4285(2) 0.6627(3) 0.0382(10) Uani 1 1 d . . . H17 H 0.8517 0.4431 0.7092 0.046 Uiso 1 1 calc R . . C18 C 0.7593(2) 0.3750(2) 0.6701(2) 0.0345(9) Uani 1 1 d . . . H18 H 0.7693 0.3537 0.7221 0.041 Uiso 1 1 calc R . . C19 C 0.3223(2) 0.3550(2) 0.6123(2) 0.0330(9) Uani 1 1 d . . . C20 C 0.3153(2) 0.3665(2) 0.5203(2) 0.0402(10) Uani 1 1 d . . . H20A H 0.3512 0.4034 0.5176 0.060 Uiso 1 1 calc R . . H20B H 0.2609 0.3792 0.4874 0.060 Uiso 1 1 calc R . . H20C H 0.3295 0.3240 0.4985 0.060 Uiso 1 1 calc R . . C21 C 0.2615(2) 0.3004(2) 0.6169(3) 0.0392(10) Uani 1 1 d . . . H21A H 0.2692 0.2579 0.5903 0.059 Uiso 1 1 calc R . . H21B H 0.2078 0.3177 0.5886 0.059 Uiso 1 1 calc R . . H21C H 0.2690 0.2910 0.6747 0.059 Uiso 1 1 calc R . . C22 C 0.3077(3) 0.4234(2) 0.6500(3) 0.0406(10) Uani 1 1 d . . . H22A H 0.3165 0.4167 0.7086 0.061 Uiso 1 1 calc R . . H22B H 0.2531 0.4383 0.6214 0.061 Uiso 1 1 calc R . . H22C H 0.3441 0.4585 0.6438 0.061 Uiso 1 1 calc R . . C23 C 0.4922(2) 0.4944(2) 0.8106(2) 0.0284(8) Uani 1 1 d . . . C24 C 0.4954(2) 0.5624(2) 0.7892(2) 0.0327(9) Uani 1 1 d . . . H24 H 0.4920 0.6015 0.8206 0.039 Uiso 1 1 calc R . . C25 C 0.4770(3) 0.4682(2) 0.8868(2) 0.0435(10) Uani 1 1 d . . . H25A H 0.4863 0.5054 0.9272 0.065 Uiso 1 1 calc R . . H25B H 0.5128 0.4299 0.9111 0.065 Uiso 1 1 calc R . . H25C H 0.4222 0.4525 0.8710 0.065 Uiso 1 1 calc R . . C26 C 0.4651(2) 0.1479(2) 0.6811(2) 0.0284(8) Uani 1 1 d . . . C27 C 0.4782(2) 0.0796(2) 0.7071(3) 0.0376(10) Uani 1 1 d . . . H27 H 0.4610 0.0401 0.6733 0.045 Uiso 1 1 calc R . . C28 C 0.4229(2) 0.1733(2) 0.5948(2) 0.0366(9) Uani 1 1 d . . . H28A H 0.4328 0.1417 0.5555 0.055 Uiso 1 1 calc R . . H28B H 0.4423 0.2192 0.5885 0.055 Uiso 1 1 calc R . . H28C H 0.3660 0.1755 0.5842 0.055 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 0.02360(11) 0.02390(11) 0.01687(10) 0.000 0.00755(7) 0.000 P1 0.0260(5) 0.0294(5) 0.0227(5) 0.0017(4) 0.0114(4) 0.0039(4) N1 0.0292(16) 0.0278(17) 0.0222(15) 0.0018(13) 0.0089(13) 0.0023(13) N2 0.043(3) 0.033(3) 0.021(2) 0.000 0.014(2) 0.000 N3 0.026(2) 0.026(2) 0.023(2) 0.000 0.0076(18) 0.000 O1 0.0293(14) 0.0327(15) 0.0244(13) 0.0032(11) 0.0127(11) 0.0059(11) C1 0.034(2) 0.031(2) 0.026(2) 0.0017(16) 0.0188(17) 0.0014(16) C2 0.038(2) 0.046(2) 0.029(2) -0.0037(19) 0.0126(19) 0.007(2) C3 0.049(3) 0.063(3) 0.035(2) -0.018(2) 0.014(2) 0.002(2) C4 0.041(2) 0.055(3) 0.024(2) -0.003(2) 0.0072(19) -0.003(2) C5 0.034(2) 0.046(3) 0.030(2) 0.0069(19) 0.0096(18) -0.0003(19) C6 0.031(2) 0.041(2) 0.029(2) 0.0023(18) 0.0126(18) 0.0041(18) C7 0.031(2) 0.030(2) 0.0230(19) -0.0045(16) 0.0072(16) 0.0029(16) C8 0.033(2) 0.041(2) 0.026(2) 0.0039(17) 0.0141(17) 0.0054(18) C9 0.033(2) 0.049(3) 0.032(2) 0.000(2) 0.0141(19) 0.013(2) C10 0.037(2) 0.032(2) 0.037(2) -0.0026(18) 0.0052(19) 0.0124(18) C11 0.040(2) 0.032(2) 0.054(3) 0.009(2) 0.019(2) 0.0002(19) C12 0.027(2) 0.035(2) 0.047(3) 0.0055(18) 0.0156(19) 0.0021(16) C13 0.028(2) 0.0271(19) 0.030(2) -0.0012(16) 0.0160(17) 0.0032(16) C14 0.042(2) 0.036(2) 0.033(2) 0.0021(18) 0.0130(19) -0.0052(18) C15 0.062(3) 0.040(3) 0.043(3) 0.009(2) 0.019(2) -0.013(2) C16 0.053(3) 0.028(2) 0.055(3) -0.001(2) 0.026(2) -0.005(2) C17 0.031(2) 0.041(2) 0.043(2) -0.012(2) 0.0141(19) -0.0035(19) C18 0.038(2) 0.039(2) 0.030(2) 0.0015(18) 0.0167(19) 0.0024(18) C19 0.029(2) 0.042(2) 0.025(2) 0.0024(18) 0.0057(17) 0.0051(18) C20 0.038(2) 0.052(3) 0.027(2) 0.006(2) 0.0067(18) 0.008(2) C21 0.036(2) 0.046(2) 0.032(2) 0.0006(19) 0.0064(19) -0.0004(19) C22 0.043(2) 0.044(3) 0.039(2) 0.007(2) 0.020(2) 0.013(2) C23 0.028(2) 0.029(2) 0.0282(19) -0.0009(16) 0.0102(16) -0.0025(16) C24 0.027(2) 0.032(2) 0.041(2) -0.0075(18) 0.0154(18) -0.0012(17) C25 0.063(3) 0.037(2) 0.031(2) -0.0051(19) 0.018(2) -0.005(2) C26 0.0241(19) 0.0285(19) 0.034(2) -0.0051(17) 0.0122(17) -0.0031(16) C27 0.035(2) 0.027(2) 0.048(2) -0.0086(18) 0.0100(19) -0.0027(17) C28 0.037(2) 0.038(2) 0.031(2) -0.0083(18) 0.0076(18) -0.0057(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 1.842(3) 2_656 ? U1 N1 1.842(3) . ? U1 O1 2.383(2) . ? U1 O1 2.383(2) 2_656 ? U1 N2 2.459(4) . ? U1 N3 2.476(4) . ? P1 O1 1.502(3) . ? P1 C1 1.791(4) . ? P1 C7 1.793(4) . ? P1 C13 1.800(4) . ? N1 C19 1.483(5) . ? N2 C23 1.362(4) 2_656 ? N2 C23 1.362(4) . ? N3 C26 1.402(4) . ? N3 C26 1.402(4) 2_656 ? C1 C2 1.385(5) . ? C1 C6 1.405(5) . ? C2 C3 1.372(6) . ? C3 C4 1.380(6) . ? C4 C5 1.366(6) . ? C5 C6 1.379(5) . ? C7 C8 1.387(5) . ? C7 C12 1.388(5) . ? C8 C9 1.377(6) . ? C9 C10 1.375(6) . ? C10 C11 1.377(6) . ? C11 C12 1.393(5) . ? C13 C14 1.375(5) . ? C13 C18 1.397(5) . ? C14 C15 1.381(6) . ? C15 C16 1.365(6) . ? C16 C17 1.378(6) . ? C17 C18 1.374(5) . ? C19 C22 1.514(6) . ? C19 C21 1.519(6) . ? C19 C20 1.540(5) . ? C23 C24 1.355(5) . ? C23 C25 1.496(5) . ? C24 C24 1.399(8) 2_656 ? C26 C27 1.370(5) . ? C26 C28 1.473(5) . ? C27 C27 1.388(8) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N1 171.42(17) 2_656 . ? N1 U1 O1 87.41(11) 2_656 . ? N1 U1 O1 93.64(11) . . ? N1 U1 O1 93.64(11) 2_656 2_656 ? N1 U1 O1 87.41(11) . 2_656 ? O1 U1 O1 165.95(12) . 2_656 ? N1 U1 N2 85.71(9) 2_656 . ? N1 U1 N2 85.71(9) . . ? O1 U1 N2 97.02(6) . . ? O1 U1 N2 97.02(6) 2_656 . ? N1 U1 N3 94.29(9) 2_656 . ? N1 U1 N3 94.29(9) . . ? O1 U1 N3 82.98(6) . . ? O1 U1 N3 82.98(6) 2_656 . ? N2 U1 N3 180.000(1) . . ? O1 P1 C1 110.74(16) . . ? O1 P1 C7 112.36(16) . . ? C1 P1 C7 108.28(17) . . ? O1 P1 C13 112.58(16) . . ? C1 P1 C13 106.30(17) . . ? C7 P1 C13 106.26(18) . . ? C19 N1 U1 156.4(3) . . ? C23 N2 C23 105.7(4) 2_656 . ? C23 N2 U1 127.1(2) 2_656 . ? C23 N2 U1 127.1(2) . . ? C26 N3 C26 105.5(4) . 2_656 ? C26 N3 U1 127.3(2) . . ? C26 N3 U1 127.3(2) 2_656 . ? P1 O1 U1 169.77(15) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 P1 123.1(3) . . ? C6 C1 P1 118.1(3) . . ? C3 C2 C1 120.2(4) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 119.9(4) . . ? C5 C6 C1 120.2(4) . . ? C8 C7 C12 120.1(4) . . ? C8 C7 P1 122.0(3) . . ? C12 C7 P1 117.9(3) . . ? C9 C8 C7 120.0(4) . . ? C10 C9 C8 120.1(4) . . ? C9 C10 C11 120.4(4) . . ? C10 C11 C12 120.2(4) . . ? C7 C12 C11 119.2(4) . . ? C14 C13 C18 118.9(4) . . ? C14 C13 P1 121.7(3) . . ? C18 C13 P1 119.4(3) . . ? C13 C14 C15 120.2(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C17 120.3(4) . . ? C18 C17 C16 119.5(4) . . ? C17 C18 C13 120.6(4) . . ? N1 C19 C22 109.6(3) . . ? N1 C19 C21 109.3(3) . . ? C22 C19 C21 109.9(3) . . ? N1 C19 C20 108.1(3) . . ? C22 C19 C20 109.9(3) . . ? C21 C19 C20 110.1(3) . . ? C24 C23 N2 110.5(3) . . ? C24 C23 C25 126.0(4) . . ? N2 C23 C25 123.3(3) . . ? C23 C24 C24 106.6(2) . 2_656 ? C27 C26 N3 109.3(3) . . ? C27 C26 C28 127.1(4) . . ? N3 C26 C28 123.6(3) . . ? C26 C27 C27 107.9(2) . 2_656 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.732 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.101