# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_email MICHEL.EPHRITIKHINE@CEA.FR _publ_section_title ; Easy access to uranium nucleophilic carbene complexes ; loop_ _publ_author_name 'M. Ephritikhine' 'Jean-Claude Berthet' 'P.Le Floch' 'Nicolas Mezailles' 'Pierre Thuery' ; J.-C.Tourneux ; # Attachment 'revisedB926718M_2_CIF.txt' data_2' _database_code_depnum_ccdc_archive 'CCDC 753015' #TrackingRef 'revisedB926718M_2_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.50 H61.50 N3.50 O0.50 P4 S4 U' _chemical_formula_weight 1443.87 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 13.8488(4) _cell_length_b 28.6755(15) _cell_length_c 17.9735(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.481(3) _cell_angle_gamma 90.00 _cell_volume 7092.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 157915 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2892 _exptl_absorpt_coefficient_mu 2.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (374 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 157915 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0979 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.68 _reflns_number_total 13350 _reflns_number_gt 9598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. One pyridine solvent molecule is disordered around an inversion centre and has been refined as an entire molecule with an occupancy parameter of 0.5; the N atom was not located. The other two solvent pyridine molecules and the THF molecule were given 0.5 occupancy factors in order to retain acceptable displacement parameters. The N atoms of the pyridine molecules have been located at the positions affected with the smaller displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the solvent molecules (ISOR for all atoms, SIMU for the THF molecule and the pyridine molecule disordered around an inversion centre, DFIX for part of the THF molecule and the pyridine molecule disordered around an inversion centre). The H atoms were introduced at calculated positions, except for the disordered pyridine molecule, and they were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some voids in the lattice likely indicate the presence of other, unresolved solvent molecules. 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^)+(0.0600P)^2^+37.4468P] 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 13350 _refine_ls_number_parameters 847 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.609 _refine_diff_density_min -1.487 _refine_diff_density_rms 0.157 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.00684(2) 0.295664(10) 0.159109(16) 0.02900(11) Uani 1 1 d . . . S1 S 0.02215(15) 0.35868(8) 0.03538(12) 0.0375(5) Uani 1 1 d . . . S2 S -0.15676(15) 0.26711(8) 0.23969(12) 0.0391(5) Uani 1 1 d . . . S3 S 0.00847(14) 0.36596(7) 0.27338(11) 0.0347(5) Uani 1 1 d . . . S4 S 0.16323(14) 0.24622(7) 0.09277(11) 0.0348(5) Uani 1 1 d . . . P1 P -0.11967(15) 0.36819(8) 0.04638(12) 0.0326(5) Uani 1 1 d . . . P2 P -0.23023(14) 0.30506(8) 0.15722(12) 0.0336(5) Uani 1 1 d . . . P3 P 0.15233(14) 0.36711(7) 0.26065(11) 0.0311(5) Uani 1 1 d . . . P4 P 0.24321(14) 0.29558(8) 0.15077(11) 0.0313(4) Uani 1 1 d . . . N1 N 0.0602(5) 0.2279(2) 0.2572(4) 0.0367(16) Uani 1 1 d . . . N2 N -0.0639(5) 0.2246(2) 0.0724(4) 0.0342(15) Uani 1 1 d . . . N3 N 0.6995(11) 0.4477(5) 0.4939(9) 0.057(4) Uani 0.50 1 d PDU . . N4 N 0.9418(11) 0.5714(6) 0.4210(9) 0.058(4) Uani 0.50 1 d PDU . . O1 O 0.7051(13) 0.9376(7) 0.7932(10) 0.091(4) Uani 0.50 1 d PU . . C1 C -0.1456(5) 0.3291(3) 0.1092(4) 0.0301(17) Uani 1 1 d . . . C2 C -0.1359(6) 0.4287(3) 0.0717(5) 0.0334(18) Uani 1 1 d . . . C3 C -0.1181(6) 0.4641(3) 0.0238(5) 0.043(2) Uani 1 1 d . . . H3 H -0.1015 0.4569 -0.0236 0.052 Uiso 1 1 calc R . . C4 C -0.1244(7) 0.5106(3) 0.0444(6) 0.056(3) Uani 1 1 d . . . H4 H -0.1109 0.5341 0.0114 0.067 Uiso 1 1 calc R . . C5 C -0.1506(7) 0.5218(3) 0.1143(6) 0.058(3) Uani 1 1 d . . . H5 H -0.1553 0.5528 0.1284 0.070 Uiso 1 1 calc R . . C6 C -0.1696(8) 0.4870(4) 0.1623(6) 0.058(3) Uani 1 1 d . . . H6 H -0.1882 0.4946 0.2089 0.070 Uiso 1 1 calc R . . C7 C -0.1615(6) 0.4403(3) 0.1426(5) 0.043(2) Uani 1 1 d . . . H7 H -0.1729 0.4169 0.1763 0.052 Uiso 1 1 calc R . . C8 C -0.1916(6) 0.3644(3) -0.0451(5) 0.040(2) Uani 1 1 d . . . C9 C -0.1528(8) 0.3501(3) -0.1076(5) 0.055(3) Uani 1 1 d . . . H9 H -0.0863 0.3446 -0.1052 0.066 Uiso 1 1 calc R . . C10 C -0.2111(8) 0.3436(4) -0.1748(6) 0.063(3) Uani 1 1 d . . . H10 H -0.1843 0.3326 -0.2166 0.075 Uiso 1 1 calc R . . C11 C -0.3081(8) 0.3536(3) -0.1792(5) 0.056(3) Uani 1 1 d . . . H11 H -0.3467 0.3510 -0.2248 0.067 Uiso 1 1 calc R . . C12 C -0.3483(7) 0.3672(4) -0.1178(5) 0.051(2) Uani 1 1 d . . . H12 H -0.4151 0.3718 -0.1207 0.061 Uiso 1 1 calc R . . C13 C -0.2917(6) 0.3742(3) -0.0511(5) 0.041(2) Uani 1 1 d . . . H13 H -0.3195 0.3854 -0.0098 0.049 Uiso 1 1 calc R . . C14 C -0.3133(6) 0.2661(3) 0.1013(5) 0.041(2) Uani 1 1 d . . . C15 C -0.3040(7) 0.2592(3) 0.0252(5) 0.050(2) Uani 1 1 d . . . H15 H -0.2575 0.2762 0.0032 0.060 Uiso 1 1 calc R . . C16 C -0.3610(9) 0.2285(4) -0.0173(7) 0.070(3) Uani 1 1 d . . . H16 H -0.3519 0.2237 -0.0672 0.084 Uiso 1 1 calc R . . C17 C -0.4310(8) 0.2051(4) 0.0136(8) 0.077(4) Uani 1 1 d . . . H17 H -0.4708 0.1844 -0.0156 0.092 Uiso 1 1 calc R . . C18 C -0.4444(7) 0.2113(3) 0.0872(9) 0.075(4) Uani 1 1 d . . . H18 H -0.4936 0.1951 0.1071 0.090 Uiso 1 1 calc R . . C19 C -0.3842(7) 0.2422(3) 0.1338(7) 0.058(3) Uani 1 1 d . . . H19 H -0.3923 0.2461 0.1841 0.069 Uiso 1 1 calc R . . C20 C -0.3099(5) 0.3466(3) 0.1970(5) 0.039(2) Uani 1 1 d . . . C21 C -0.3914(6) 0.3635(3) 0.1541(6) 0.046(2) Uani 1 1 d . . . H21 H -0.4093 0.3519 0.1062 0.055 Uiso 1 1 calc R . . C22 C -0.4475(7) 0.3988(3) 0.1836(6) 0.053(3) Uani 1 1 d . . . H22 H -0.5022 0.4104 0.1548 0.064 Uiso 1 1 calc R . . C23 C -0.4230(8) 0.4155(4) 0.2521(7) 0.064(3) Uani 1 1 d . . . H23 H -0.4616 0.4382 0.2711 0.077 Uiso 1 1 calc R . . C24 C -0.3409(9) 0.3997(4) 0.2955(7) 0.078(4) Uani 1 1 d . . . H24 H -0.3237 0.4125 0.3427 0.093 Uiso 1 1 calc R . . C25 C -0.2828(7) 0.3643(3) 0.2689(5) 0.052(2) Uani 1 1 d . . . H25 H -0.2281 0.3531 0.2983 0.062 Uiso 1 1 calc R . . C26 C 0.1664(5) 0.3243(3) 0.1988(4) 0.0307(17) Uani 1 1 d . . . C27 C 0.1858(6) 0.4252(3) 0.2309(4) 0.0373(19) Uani 1 1 d . . . C28 C 0.1172(7) 0.4549(3) 0.1976(5) 0.043(2) Uani 1 1 d . . . H28 H 0.0520 0.4464 0.1930 0.052 Uiso 1 1 calc R . . C29 C 0.1444(8) 0.4984(3) 0.1702(6) 0.058(3) Uani 1 1 d . . . H29 H 0.0974 0.5188 0.1483 0.070 Uiso 1 1 calc R . . C30 C 0.2402(8) 0.5101(4) 0.1762(7) 0.069(3) Uani 1 1 d . . . H30 H 0.2592 0.5386 0.1576 0.082 Uiso 1 1 calc R . . C31 C 0.3098(7) 0.4794(4) 0.2101(7) 0.064(3) Uani 1 1 d . . . H31 H 0.3753 0.4873 0.2145 0.077 Uiso 1 1 calc R . . C32 C 0.2814(6) 0.4380(3) 0.2367(6) 0.050(2) Uani 1 1 d . . . H32 H 0.3282 0.4178 0.2595 0.061 Uiso 1 1 calc R . . C33 C 0.2209(6) 0.3606(3) 0.3530(5) 0.039(2) Uani 1 1 d . . . C34 C 0.2650(6) 0.3191(3) 0.3742(5) 0.040(2) Uani 1 1 d . . . H34 H 0.2667 0.2954 0.3389 0.048 Uiso 1 1 calc R . . C35 C 0.3068(6) 0.3117(4) 0.4463(5) 0.047(2) Uani 1 1 d . . . H35 H 0.3342 0.2828 0.4596 0.056 Uiso 1 1 calc R . . C36 C 0.3084(8) 0.3460(4) 0.4982(6) 0.069(3) Uani 1 1 d . . . H36 H 0.3383 0.3413 0.5466 0.082 Uiso 1 1 calc R . . C37 C 0.2637(10) 0.3892(5) 0.4773(6) 0.084(4) Uani 1 1 d . . . H37 H 0.2635 0.4132 0.5121 0.101 Uiso 1 1 calc R . . C38 C 0.2210(8) 0.3954(4) 0.4060(5) 0.062(3) Uani 1 1 d . . . H38 H 0.1913 0.4237 0.3927 0.074 Uiso 1 1 calc R . . C39 C 0.3436(6) 0.2698(3) 0.2109(4) 0.0351(19) Uani 1 1 d . . . C40 C 0.4194(6) 0.2975(3) 0.2395(5) 0.042(2) Uani 1 1 d . . . H40 H 0.4231 0.3281 0.2227 0.051 Uiso 1 1 calc R . . C41 C 0.4910(6) 0.2805(4) 0.2933(5) 0.049(2) Uani 1 1 d . . . H41 H 0.5418 0.2997 0.3128 0.059 Uiso 1 1 calc R . . C42 C 0.4860(7) 0.2348(4) 0.3176(6) 0.061(3) Uani 1 1 d . . . H42 H 0.5345 0.2229 0.3525 0.073 Uiso 1 1 calc R . . C43 C 0.4105(9) 0.2078(4) 0.2904(7) 0.071(3) Uani 1 1 d . . . H43 H 0.4061 0.1776 0.3083 0.085 Uiso 1 1 calc R . . C44 C 0.3388(7) 0.2242(3) 0.2358(6) 0.058(3) Uani 1 1 d . . . H44 H 0.2884 0.2047 0.2165 0.069 Uiso 1 1 calc R . . C45 C 0.3055(5) 0.3296(3) 0.0850(4) 0.0350(19) Uani 1 1 d . . . C46 C 0.2768(6) 0.3752(3) 0.0669(5) 0.039(2) Uani 1 1 d . . . H46 H 0.2272 0.3890 0.0899 0.046 Uiso 1 1 calc R . . C47 C 0.3228(6) 0.3996(3) 0.0144(5) 0.044(2) Uani 1 1 d . . . H47 H 0.3046 0.4303 0.0030 0.053 Uiso 1 1 calc R . . C48 C 0.3948(6) 0.3791(4) -0.0209(5) 0.050(2) Uani 1 1 d . . . H48 H 0.4240 0.3955 -0.0570 0.060 Uiso 1 1 calc R . . C49 C 0.4237(6) 0.3341(4) -0.0027(5) 0.047(2) Uani 1 1 d . . . H49 H 0.4735 0.3203 -0.0255 0.056 Uiso 1 1 calc R . . C50 C 0.3790(6) 0.3100(3) 0.0488(5) 0.040(2) Uani 1 1 d . . . H50 H 0.3983 0.2795 0.0601 0.048 Uiso 1 1 calc R . . C51 C 0.0766(6) 0.1835(3) 0.2395(5) 0.047(2) Uani 1 1 d . . . H51 H 0.0633 0.1740 0.1900 0.056 Uiso 1 1 calc R . . C52 C 0.1127(7) 0.1515(3) 0.2930(6) 0.054(3) Uani 1 1 d . . . H52 H 0.1198 0.1205 0.2793 0.064 Uiso 1 1 calc R . . C53 C 0.1379(6) 0.1644(3) 0.3649(5) 0.045(2) Uani 1 1 d . . . H53 H 0.1644 0.1432 0.4007 0.054 Uiso 1 1 calc R . . C54 C 0.1225(6) 0.2107(3) 0.3832(5) 0.043(2) Uani 1 1 d . . . H54 H 0.1394 0.2210 0.4319 0.051 Uiso 1 1 calc R . . C55 C 0.0827(6) 0.2409(3) 0.3299(5) 0.0360(19) Uani 1 1 d . . . H55 H 0.0706 0.2715 0.3436 0.043 Uiso 1 1 calc R . . C56 C -0.0565(6) 0.2274(3) -0.0012(5) 0.040(2) Uani 1 1 d . . . H56 H -0.0256 0.2534 -0.0187 0.048 Uiso 1 1 calc R . . C57 C -0.0918(8) 0.1943(4) -0.0522(6) 0.059(3) Uani 1 1 d . . . H57 H -0.0819 0.1967 -0.1023 0.071 Uiso 1 1 calc R . . C58 C -0.1429(9) 0.1570(4) -0.0266(6) 0.070(3) Uani 1 1 d . . . H58 H -0.1689 0.1341 -0.0596 0.084 Uiso 1 1 calc R . . C59 C -0.1542(9) 0.1545(4) 0.0466(6) 0.068(3) Uani 1 1 d . . . H59 H -0.1885 0.1299 0.0648 0.081 Uiso 1 1 calc R . . C60 C -0.1139(7) 0.1890(3) 0.0949(5) 0.048(2) Uani 1 1 d . . . H60 H -0.1226 0.1869 0.1453 0.058 Uiso 1 1 calc R . . C61 C 0.6256(15) 0.4203(8) 0.5045(13) 0.073(6) Uani 0.50 1 d PDU . . H61 H 0.5808 0.4071 0.4681 0.088 Uiso 0.50 1 calc PR . . C62 C 0.629(2) 0.4153(11) 0.5828(17) 0.102(9) Uani 0.50 1 d PU . . H62 H 0.5855 0.3935 0.5976 0.123 Uiso 0.50 1 calc PR . . C63 C 0.6844(18) 0.4365(9) 0.6412(14) 0.078(7) Uani 0.50 1 d PU . . H63 H 0.6765 0.4308 0.6911 0.093 Uiso 0.50 1 calc PR . . C64 C 0.7512(17) 0.4661(9) 0.6196(13) 0.071(6) Uani 0.50 1 d PU . . H64 H 0.7932 0.4819 0.6550 0.086 Uiso 0.50 1 calc PR . . C65 C 0.7565(15) 0.4727(7) 0.5439(11) 0.063(6) Uani 0.50 1 d PDU . . H65 H 0.7995 0.4944 0.5279 0.075 Uiso 0.50 1 calc PR . . C66 C 0.8977(15) 0.5333(6) 0.4430(12) 0.065(6) Uani 0.50 1 d PDU . . H66 H 0.8587 0.5342 0.4819 0.078 Uiso 0.50 1 calc PR . . C67 C 0.9127(16) 0.4926(9) 0.4053(12) 0.076(7) Uani 0.50 1 d PDU . . H67 H 0.8803 0.4659 0.4182 0.091 Uiso 0.50 1 calc PR . . C68 C 0.9730(12) 0.4890(6) 0.3494(9) 0.043(4) Uani 0.50 1 d PDU . . H68 H 0.9862 0.4607 0.3275 0.052 Uiso 0.50 1 calc PR . . C69 C 1.0120(17) 0.5302(6) 0.3286(12) 0.081(7) Uani 0.50 1 d PDU . . H69 H 1.0536 0.5302 0.2914 0.097 Uiso 0.50 1 calc PR . . C70 C 0.9905(14) 0.5718(7) 0.3617(10) 0.064(6) Uani 0.50 1 d PDU . . H70 H 1.0102 0.5999 0.3426 0.077 Uiso 0.50 1 calc PR . . C71 C 0.5674(15) 0.0177(10) 0.4601(11) 0.073(4) Uani 0.50 1 d PDU . 1 C72 C 0.5691(15) 0.0107(11) 0.5369(10) 0.074(4) Uani 0.50 1 d PDU . 1 C73 C 0.4872(16) -0.0074(11) 0.5655(9) 0.074(4) Uani 0.50 1 d PDU . 1 C74 C 0.4062(14) -0.0189(11) 0.5169(11) 0.074(4) Uani 0.50 1 d PDU . 1 C75 C 0.4061(15) -0.0135(11) 0.4402(10) 0.075(4) Uani 0.50 1 d PDU . 1 C76 C 0.4882(17) 0.0034(11) 0.4120(9) 0.075(4) Uani 0.50 1 d PDU . 1 C77 C 0.6481(18) 0.9249(10) 0.7328(15) 0.089(4) Uani 0.50 1 d PU . . H77A H 0.6698 0.8944 0.7184 0.106 Uiso 0.50 1 calc PR . . H77B H 0.6602 0.9463 0.6930 0.106 Uiso 0.50 1 calc PR . . C78 C 0.5456(17) 0.9222(10) 0.7330(14) 0.086(4) Uani 0.50 1 d PDU . . H78A H 0.5228 0.8903 0.7288 0.103 Uiso 0.50 1 calc PR . . H78B H 0.5118 0.9407 0.6930 0.103 Uiso 0.50 1 calc PR . . C79 C 0.534(2) 0.9428(13) 0.8097(15) 0.145(13) Uani 0.50 1 d PDU . . H79A H 0.5104 0.9191 0.8420 0.174 Uiso 0.50 1 calc PR . . H79B H 0.4870 0.9682 0.8049 0.174 Uiso 0.50 1 calc PR . . C80 C 0.6338(18) 0.9605(10) 0.8426(15) 0.089(8) Uani 0.50 1 d PDU . . H80A H 0.6482 0.9510 0.8944 0.107 Uiso 0.50 1 calc PR . . H80B H 0.6371 0.9942 0.8397 0.107 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02723(16) 0.02989(17) 0.02919(16) 0.00165(14) 0.00023(11) 0.00173(13) S1 0.0340(11) 0.0383(12) 0.0407(12) 0.0086(10) 0.0058(9) 0.0036(9) S2 0.0351(11) 0.0442(13) 0.0377(12) 0.0086(10) 0.0030(9) 0.0004(10) S3 0.0291(10) 0.0365(12) 0.0388(11) -0.0032(9) 0.0049(9) 0.0017(9) S4 0.0348(11) 0.0338(11) 0.0351(11) -0.0032(9) 0.0014(8) 0.0039(9) P1 0.0301(11) 0.0334(12) 0.0337(11) 0.0038(9) 0.0013(9) 0.0030(9) P2 0.0263(10) 0.0356(13) 0.0382(12) 0.0040(9) 0.0005(9) 0.0004(9) P3 0.0278(10) 0.0320(12) 0.0331(11) -0.0006(9) 0.0012(8) 0.0006(9) P4 0.0268(10) 0.0343(12) 0.0326(11) 0.0016(10) 0.0025(8) 0.0033(9) N1 0.033(4) 0.034(4) 0.040(4) -0.004(3) -0.008(3) 0.007(3) N2 0.034(4) 0.030(4) 0.037(4) -0.002(3) 0.000(3) -0.007(3) N3 0.063(8) 0.050(8) 0.056(7) -0.010(6) -0.002(6) 0.024(7) N4 0.046(7) 0.054(8) 0.070(8) -0.014(7) -0.013(6) 0.000(6) O1 0.081(6) 0.097(7) 0.090(6) -0.001(6) -0.003(5) -0.013(5) C1 0.027(4) 0.030(4) 0.034(4) 0.001(3) 0.004(3) 0.000(3) C2 0.031(4) 0.026(4) 0.043(5) -0.002(4) -0.002(3) 0.004(3) C3 0.047(5) 0.036(5) 0.048(5) 0.007(4) 0.009(4) 0.004(4) C4 0.055(6) 0.041(6) 0.069(7) 0.013(5) 0.004(5) 0.005(5) C5 0.065(7) 0.030(5) 0.074(7) -0.004(5) -0.013(5) 0.008(5) C6 0.070(7) 0.048(6) 0.056(6) -0.008(5) 0.003(5) 0.012(5) C7 0.043(5) 0.037(5) 0.046(5) -0.001(4) -0.005(4) 0.002(4) C8 0.042(5) 0.034(5) 0.041(5) 0.006(4) -0.002(4) 0.001(4) C9 0.073(7) 0.053(6) 0.039(5) -0.005(5) 0.007(5) 0.026(5) C10 0.088(8) 0.057(7) 0.042(6) -0.002(5) 0.000(5) 0.023(6) C11 0.070(7) 0.049(6) 0.040(6) -0.006(5) -0.028(5) -0.002(5) C12 0.038(5) 0.062(7) 0.049(6) 0.013(5) -0.010(4) -0.010(5) C13 0.038(5) 0.041(5) 0.044(5) 0.008(4) -0.001(4) -0.003(4) C14 0.027(4) 0.031(5) 0.064(6) -0.001(4) -0.005(4) 0.006(4) C15 0.047(5) 0.044(6) 0.052(6) 0.013(5) -0.019(4) -0.011(4) C16 0.072(8) 0.050(7) 0.079(8) -0.008(6) -0.027(6) 0.006(6) C17 0.046(7) 0.073(9) 0.106(10) -0.033(8) -0.017(7) 0.003(6) C18 0.026(5) 0.033(6) 0.167(14) 0.000(7) 0.016(6) -0.001(4) C19 0.052(6) 0.031(5) 0.091(8) -0.004(5) 0.011(5) 0.002(5) C20 0.024(4) 0.045(5) 0.048(5) 0.000(4) 0.004(4) -0.004(4) C21 0.038(5) 0.039(5) 0.061(6) -0.003(5) 0.007(4) 0.002(4) C22 0.039(5) 0.039(6) 0.083(8) 0.004(5) 0.011(5) 0.006(4) C23 0.055(6) 0.060(7) 0.080(8) -0.012(6) 0.014(6) 0.016(5) C24 0.077(8) 0.083(9) 0.073(8) -0.031(7) 0.011(6) 0.011(7) C25 0.043(5) 0.056(6) 0.054(6) -0.005(5) 0.003(4) 0.010(5) C26 0.031(4) 0.032(4) 0.029(4) 0.001(3) 0.002(3) 0.000(3) C27 0.038(5) 0.040(5) 0.033(4) 0.001(4) 0.000(4) -0.004(4) C28 0.045(5) 0.036(5) 0.048(5) 0.007(4) 0.008(4) -0.001(4) C29 0.079(8) 0.037(6) 0.059(7) 0.011(5) 0.012(5) 0.000(5) C30 0.072(8) 0.048(7) 0.088(9) 0.009(6) 0.020(6) -0.015(6) C31 0.040(5) 0.053(7) 0.099(9) 0.004(6) -0.001(5) -0.015(5) C32 0.038(5) 0.041(6) 0.071(7) 0.004(5) 0.006(5) -0.005(4) C33 0.036(5) 0.041(5) 0.037(5) -0.007(4) -0.003(4) 0.002(4) C34 0.039(5) 0.046(5) 0.035(5) -0.002(4) 0.008(4) 0.000(4) C35 0.042(5) 0.060(6) 0.038(5) 0.009(5) 0.002(4) 0.005(4) C36 0.078(8) 0.074(8) 0.051(7) 0.006(6) -0.007(6) 0.002(6) C37 0.117(10) 0.070(8) 0.057(7) -0.025(6) -0.028(7) 0.002(8) C38 0.078(7) 0.051(6) 0.050(6) -0.010(5) -0.020(5) 0.022(6) C39 0.033(4) 0.042(5) 0.030(4) -0.002(4) 0.003(3) 0.004(4) C40 0.033(4) 0.053(6) 0.040(5) 0.008(4) 0.000(4) -0.003(4) C41 0.030(5) 0.071(7) 0.046(5) 0.002(5) -0.002(4) -0.001(5) C42 0.040(6) 0.074(8) 0.062(7) 0.002(6) -0.021(5) 0.015(5) C43 0.079(8) 0.041(6) 0.084(8) 0.009(6) -0.024(6) 0.018(6) C44 0.061(6) 0.039(6) 0.067(7) 0.012(5) -0.023(5) 0.001(5) C45 0.026(4) 0.048(5) 0.031(4) 0.004(4) 0.001(3) 0.000(4) C46 0.040(5) 0.036(5) 0.039(5) -0.002(4) 0.002(4) -0.001(4) C47 0.044(5) 0.041(5) 0.047(5) 0.005(4) 0.001(4) -0.003(4) C48 0.037(5) 0.064(7) 0.050(6) 0.014(5) 0.008(4) -0.010(5) C49 0.033(5) 0.062(7) 0.046(5) -0.006(5) 0.008(4) -0.003(4) C50 0.036(5) 0.045(5) 0.040(5) 0.001(4) 0.008(4) 0.005(4) C51 0.047(5) 0.041(5) 0.052(6) 0.008(5) 0.000(4) 0.000(4) C52 0.062(6) 0.039(6) 0.059(6) 0.012(5) 0.003(5) 0.009(5) C53 0.051(5) 0.041(5) 0.041(5) 0.011(4) -0.001(4) 0.013(4) C54 0.049(5) 0.049(6) 0.031(4) 0.007(4) 0.004(4) 0.006(4) C55 0.033(4) 0.033(5) 0.043(5) 0.006(4) 0.012(4) 0.005(4) C56 0.042(5) 0.037(5) 0.039(5) 0.008(4) -0.006(4) 0.008(4) C57 0.082(8) 0.050(7) 0.043(6) -0.006(5) 0.003(5) -0.005(6) C58 0.093(9) 0.056(7) 0.056(7) -0.018(6) -0.014(6) -0.020(6) C59 0.094(9) 0.050(7) 0.054(7) 0.006(5) -0.010(6) -0.026(6) C60 0.059(6) 0.038(5) 0.046(5) 0.003(4) -0.005(4) 0.000(5) C61 0.087(10) 0.070(10) 0.067(9) 0.000(8) 0.027(8) 0.005(8) C62 0.099(12) 0.100(12) 0.109(12) -0.004(9) 0.017(9) -0.005(9) C63 0.087(10) 0.072(10) 0.075(10) -0.003(8) 0.011(8) -0.004(8) C64 0.069(9) 0.071(10) 0.074(10) -0.007(8) 0.008(8) 0.003(8) C65 0.073(9) 0.053(9) 0.063(9) 0.008(8) 0.011(8) -0.004(8) C66 0.063(9) 0.056(9) 0.078(9) -0.012(8) 0.022(8) 0.014(8) C67 0.079(10) 0.061(10) 0.087(10) 0.008(8) 0.005(8) -0.014(8) C68 0.051(8) 0.035(7) 0.039(7) -0.003(6) -0.014(6) 0.010(6) C69 0.094(10) 0.080(11) 0.069(10) -0.001(8) 0.010(8) -0.019(8) C70 0.077(9) 0.057(9) 0.058(9) -0.021(7) 0.009(8) -0.019(8) C71 0.076(5) 0.062(4) 0.079(6) -0.011(4) 0.000(4) 0.014(4) C72 0.076(5) 0.062(4) 0.079(6) -0.013(4) -0.005(4) 0.016(4) C73 0.078(5) 0.063(4) 0.077(6) -0.010(4) -0.002(4) 0.016(4) C74 0.077(5) 0.063(4) 0.079(6) -0.010(4) -0.001(4) 0.015(4) C75 0.079(5) 0.064(4) 0.080(6) -0.012(4) -0.002(4) 0.017(4) C76 0.079(5) 0.063(4) 0.079(6) -0.011(4) -0.002(4) 0.015(4) C77 0.081(6) 0.095(6) 0.086(6) -0.002(5) -0.006(5) -0.015(5) C78 0.077(6) 0.090(7) 0.084(7) -0.001(6) -0.017(6) -0.021(6) C79 0.132(15) 0.146(16) 0.162(16) 0.035(10) 0.034(10) 0.011(10) C80 0.102(11) 0.080(11) 0.081(10) 0.003(8) -0.007(8) -0.006(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U C26 2.390(8) . ? U C1 2.399(7) . ? U N1 2.670(7) . ? U N2 2.683(6) . ? U S3 2.876(2) . ? U S1 2.892(2) . ? U S2 2.940(2) . ? U S4 2.951(2) . ? S1 P1 2.015(3) . ? S2 P2 2.019(3) . ? S3 P3 2.031(3) . ? S4 P4 2.014(3) . ? P1 C1 1.658(8) . ? P1 C2 1.814(8) . ? P1 C8 1.827(8) . ? P2 C1 1.680(8) . ? P2 C14 1.823(9) . ? P2 C20 1.823(9) . ? P3 C26 1.681(8) . ? P3 C27 1.825(9) . ? P3 C33 1.827(8) . ? P4 C26 1.663(8) . ? P4 C39 1.819(8) . ? P4 C45 1.822(8) . ? N1 C51 1.337(11) . ? N1 C55 1.362(10) . ? N2 C60 1.323(11) . ? N2 C56 1.340(10) . ? N3 C61 1.320(10) . ? N3 C65 1.336(10) . ? N4 C70 1.323(10) . ? N4 C66 1.334(10) . ? O1 C77 1.32(3) . ? O1 C80 1.55(3) . ? C2 C3 1.373(12) . ? C2 C7 1.399(12) . ? C3 C4 1.388(13) . ? C3 H3 0.9300 . ? C4 C5 1.384(14) . ? C4 H4 0.9300 . ? C5 C6 1.363(14) . ? C5 H5 0.9300 . ? C6 C7 1.395(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.362(12) . ? C8 C13 1.408(12) . ? C9 C10 1.387(14) . ? C9 H9 0.9300 . ? C10 C11 1.368(14) . ? C10 H10 0.9300 . ? C11 C12 1.348(14) . ? C11 H11 0.9300 . ? C12 C13 1.371(12) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.380(13) . ? C14 C15 1.403(13) . ? C15 C16 1.359(13) . ? C15 H15 0.9300 . ? C16 C17 1.350(17) . ? C16 H16 0.9300 . ? C17 C18 1.368(18) . ? C17 H17 0.9300 . ? C18 C19 1.422(15) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.383(12) . ? C20 C25 1.399(12) . ? C21 C22 1.415(12) . ? C21 H21 0.9300 . ? C22 C23 1.329(14) . ? C22 H22 0.9300 . ? C23 C24 1.380(15) . ? C23 H23 0.9300 . ? C24 C25 1.413(14) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C27 C28 1.364(12) . ? C27 C32 1.367(12) . ? C28 C29 1.407(13) . ? C28 H28 0.9300 . ? C29 C30 1.362(14) . ? C29 H29 0.9300 . ? C30 C31 1.394(15) . ? C30 H30 0.9300 . ? C31 C32 1.355(13) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.372(12) . ? C33 C38 1.379(12) . ? C34 C35 1.376(12) . ? C34 H34 0.9300 . ? C35 C36 1.355(14) . ? C35 H35 0.9300 . ? C36 C37 1.417(16) . ? C36 H36 0.9300 . ? C37 C38 1.361(14) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.371(12) . ? C39 C44 1.387(13) . ? C40 C41 1.393(12) . ? C40 H40 0.9300 . ? C41 C42 1.385(15) . ? C41 H41 0.9300 . ? C42 C43 1.349(15) . ? C42 H42 0.9300 . ? C43 C44 1.395(13) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.386(11) . ? C45 C46 1.394(12) . ? C46 C47 1.387(12) . ? C46 H46 0.9300 . ? C47 C48 1.374(13) . ? C47 H47 0.9300 . ? C48 C49 1.379(13) . ? C48 H48 0.9300 . ? C49 C50 1.359(12) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.381(12) . ? C51 H51 0.9300 . ? C52 C53 1.352(13) . ? C52 H52 0.9300 . ? C53 C54 1.388(12) . ? C53 H53 0.9300 . ? C54 C55 1.362(11) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.371(13) . ? C56 H56 0.9300 . ? C57 C58 1.389(15) . ? C57 H57 0.9300 . ? C58 C59 1.344(15) . ? C58 H58 0.9300 . ? C59 C60 1.390(13) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.41(3) . ? C61 H61 0.9300 . ? C62 C63 1.37(4) . ? C62 H62 0.9300 . ? C63 C64 1.35(3) . ? C63 H63 0.9300 . ? C64 C65 1.38(3) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 C67 1.38(3) . ? C66 H66 0.9300 . ? C67 C68 1.381(10) . ? C67 H67 0.9300 . ? C68 C69 1.368(10) . ? C68 H68 0.9300 . ? C69 C70 1.380(10) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C76 1.381(8) . ? C71 C72 1.393(8) . ? C72 C73 1.396(8) . ? C73 C74 1.383(8) . ? C74 C75 1.386(8) . ? C75 C76 1.384(8) . ? C77 C78 1.42(3) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.525(10) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C80 1.533(10) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 U C1 136.0(3) . . ? C26 U N1 82.8(2) . . ? C1 U N1 134.8(2) . . ? C26 U N2 134.4(2) . . ? C1 U N2 80.7(2) . . ? N1 U N2 83.5(2) . . ? C26 U S3 67.24(19) . . ? C1 U S3 85.55(19) . . ? N1 U S3 93.40(15) . . ? N2 U S3 156.95(15) . . ? C26 U S1 82.49(19) . . ? C1 U S1 66.44(18) . . ? N1 U S1 157.40(15) . . ? N2 U S1 94.66(15) . . ? S3 U S1 96.65(6) . . ? C26 U S2 133.35(18) . . ? C1 U S2 66.49(19) . . ? N1 U S2 69.11(15) . . ? N2 U S2 79.83(15) . . ? S3 U S2 77.75(6) . . ? S1 U S2 132.88(6) . . ? C26 U S4 65.79(19) . . ? C1 U S4 134.12(19) . . ? N1 U S4 75.88(15) . . ? N2 U S4 68.71(15) . . ? S3 U S4 132.72(6) . . ? S1 U S4 82.45(6) . . ? S2 U S4 134.98(6) . . ? P1 S1 U 81.50(9) . . ? P2 S2 U 80.84(9) . . ? P3 S3 U 81.93(9) . . ? P4 S4 U 80.73(9) . . ? C1 P1 C2 115.6(4) . . ? C1 P1 C8 115.8(4) . . ? C2 P1 C8 102.3(4) . . ? C1 P1 S1 105.3(3) . . ? C2 P1 S1 107.7(3) . . ? C8 P1 S1 110.0(3) . . ? C1 P2 C14 113.7(4) . . ? C1 P2 C20 114.9(4) . . ? C14 P2 C20 104.2(4) . . ? C1 P2 S2 106.0(3) . . ? C14 P2 S2 108.0(3) . . ? C20 P2 S2 109.9(3) . . ? C26 P3 C27 114.9(4) . . ? C26 P3 C33 116.0(4) . . ? C27 P3 C33 103.7(4) . . ? C26 P3 S3 104.5(3) . . ? C27 P3 S3 109.4(3) . . ? C33 P3 S3 108.2(3) . . ? C26 P4 C39 112.6(4) . . ? C26 P4 C45 116.7(4) . . ? C39 P4 C45 102.5(4) . . ? C26 P4 S4 105.7(3) . . ? C39 P4 S4 111.1(3) . . ? C45 P4 S4 108.2(3) . . ? C51 N1 C55 117.5(7) . . ? C51 N1 U 125.3(6) . . ? C55 N1 U 116.8(5) . . ? C60 N2 C56 116.7(7) . . ? C60 N2 U 125.4(6) . . ? C56 N2 U 117.7(5) . . ? C61 N3 C65 129(2) . . ? C70 N4 C66 122.6(18) . . ? C77 O1 C80 103.1(19) . . ? P1 C1 P2 147.6(5) . . ? P1 C1 U 106.0(3) . . ? P2 C1 U 106.2(4) . . ? C3 C2 C7 118.5(8) . . ? C3 C2 P1 120.9(7) . . ? C7 C2 P1 120.4(6) . . ? C2 C3 C4 121.4(9) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.7(9) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 119.6(9) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.0(10) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.7(9) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? C9 C8 C13 118.3(8) . . ? C9 C8 P1 122.3(7) . . ? C13 C8 P1 119.3(7) . . ? C8 C9 C10 120.9(10) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.6(10) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 120.5(9) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.7(9) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 119.9(9) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C19 C14 C15 119.5(9) . . ? C19 C14 P2 120.4(8) . . ? C15 C14 P2 120.1(7) . . ? C16 C15 C14 121.9(10) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C17 C16 C15 119.3(12) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.0(11) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 121.2(11) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C14 C19 C18 117.2(11) . . ? C14 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? C21 C20 C25 120.3(8) . . ? C21 C20 P2 120.2(7) . . ? C25 C20 P2 119.2(6) . . ? C20 C21 C22 119.3(9) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.8(10) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.9(10) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 120.6(10) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 118.0(9) . . ? C20 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? P4 C26 P3 146.5(5) . . ? P4 C26 U 107.4(4) . . ? P3 C26 U 106.1(4) . . ? C28 C27 C32 119.1(8) . . ? C28 C27 P3 120.8(6) . . ? C32 C27 P3 120.0(7) . . ? C27 C28 C29 120.5(9) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.2(10) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 119.8(10) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.6(9) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C27 121.8(9) . . ? C31 C32 H32 119.1 . . ? C27 C32 H32 119.1 . . ? C34 C33 C38 118.1(8) . . ? C34 C33 P3 120.7(7) . . ? C38 C33 P3 120.9(7) . . ? C33 C34 C35 121.5(9) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 120.6(10) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 118.8(10) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 119.5(11) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C33 121.6(10) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? C40 C39 C44 119.3(8) . . ? C40 C39 P4 119.2(7) . . ? C44 C39 P4 121.0(7) . . ? C39 C40 C41 120.8(9) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 119.6(9) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 119.5(9) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 121.6(10) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C39 C44 C43 119.2(9) . . ? C39 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C50 C45 C46 118.3(8) . . ? C50 C45 P4 121.0(7) . . ? C46 C45 P4 120.6(6) . . ? C47 C46 C45 119.5(8) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C46 120.7(9) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 119.9(9) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C50 C49 C48 119.6(9) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C45 122.0(9) . . ? C49 C50 H50 119.0 . . ? C45 C50 H50 119.0 . . ? N1 C51 C52 121.8(9) . . ? N1 C51 H51 119.1 . . ? C52 C51 H51 119.1 . . ? C53 C52 C51 121.1(10) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 117.2(8) . . ? C52 C53 H53 121.4 . . ? C54 C53 H53 121.4 . . ? C55 C54 C53 120.2(8) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? N1 C55 C54 122.1(8) . . ? N1 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? N2 C56 C57 123.8(9) . . ? N2 C56 H56 118.1 . . ? C57 C56 H56 118.1 . . ? C56 C57 C58 117.9(9) . . ? C56 C57 H57 121.1 . . ? C58 C57 H57 121.1 . . ? C59 C58 C57 119.1(10) . . ? C59 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C58 C59 C60 119.3(10) . . ? C58 C59 H59 120.4 . . ? C60 C59 H59 120.4 . . ? N2 C60 C59 123.1(9) . . ? N2 C60 H60 118.4 . . ? C59 C60 H60 118.4 . . ? N3 C61 C62 105(2) . . ? N3 C61 H61 127.3 . . ? C62 C61 H61 127.3 . . ? C63 C62 C61 132(3) . . ? C63 C62 H62 113.8 . . ? C61 C62 H62 113.8 . . ? C64 C63 C62 114(3) . . ? C64 C63 H63 123.1 . . ? C62 C63 H63 123.1 . . ? C63 C64 C65 119(2) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? N3 C65 C64 120(2) . . ? N3 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? N4 C66 C67 116.6(18) . . ? N4 C66 H66 121.7 . . ? C67 C66 H66 121.7 . . ? C68 C67 C66 124(2) . . ? C68 C67 H67 118.1 . . ? C66 C67 H67 118.1 . . ? C69 C68 C67 115.2(18) . . ? C69 C68 H68 122.4 . . ? C67 C68 H68 122.4 . . ? C68 C69 C70 121(2) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? N4 C70 C69 119.7(19) . . ? N4 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C76 C71 C72 120.1(7) . . ? C71 C72 C73 119.7(7) . . ? C74 C73 C72 119.4(7) . . ? C73 C74 C75 120.7(7) . . ? C76 C75 C74 119.7(7) . . ? C71 C76 C75 120.1(7) . . ? O1 C77 C78 121(2) . . ? O1 C77 H77A 107.0 . . ? C78 C77 H77A 107.0 . . ? O1 C77 H77B 107.0 . . ? C78 C77 H77B 107.0 . . ? H77A C77 H77B 106.8 . . ? C77 C78 C79 101(2) . . ? C77 C78 H78A 111.5 . . ? C79 C78 H78A 111.5 . . ? C77 C78 H78B 111.5 . . ? C79 C78 H78B 111.5 . . ? H78A C78 H78B 109.3 . . ? C78 C79 C80 107(2) . . ? C78 C79 H79A 110.4 . . ? C80 C79 H79A 110.4 . . ? C78 C79 H79B 110.4 . . ? C80 C79 H79B 110.4 . . ? H79A C79 H79B 108.6 . . ? C79 C80 O1 104(2) . . ? C79 C80 H80A 110.9 . . ? O1 C80 H80A 110.9 . . ? C79 C80 H80B 110.9 . . ? O1 C80 H80B 110.9 . . ? H80A C80 H80B 108.9 . . ? #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 753016' #TrackingRef 'revisedB926718M_2_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H38 P2 S2 U' _chemical_formula_weight 906.81 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.0722(6) _cell_length_b 16.8709(9) _cell_length_c 16.7480(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.816(3) _cell_angle_gamma 90.00 _cell_volume 3693.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 108095 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 4.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and four \w scans with 2\% steps (397 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 108095 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6980 _reflns_number_gt 4921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the badly resolved toluene solvent molecule (DFIX for the C36-C42 bond length, ISOR and DELU for all atoms). The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0332P)^2^] 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 6980 _refine_ls_number_parameters 425 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.914 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.130 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.249966(12) 0.503295(11) 0.927388(9) 0.02284(7) Uani 1 1 d . . . S1 S 0.04366(8) 0.50313(8) 0.86719(7) 0.0306(3) Uani 1 1 d . . . S2 S 0.44885(9) 0.51469(8) 0.85799(7) 0.0281(3) Uani 1 1 d . . . P1 P 0.11861(9) 0.48499(7) 0.76315(7) 0.0240(3) Uani 1 1 d . . . P2 P 0.36499(8) 0.49144(8) 0.75739(7) 0.0239(3) Uani 1 1 d . . . C1 C 0.2436(3) 0.4888(3) 0.7887(3) 0.0226(10) Uani 1 1 d . . . C2 C 0.0791(3) 0.5588(3) 0.6899(3) 0.0259(11) Uani 1 1 d . . . C3 C 0.0580(4) 0.6362(3) 0.7154(3) 0.0403(14) Uani 1 1 d . . . H3 H 0.0559 0.6475 0.7697 0.048 Uiso 1 1 calc R . . C4 C 0.0402(4) 0.6960(3) 0.6602(3) 0.0443(15) Uani 1 1 d . . . H4 H 0.0271 0.7474 0.6774 0.053 Uiso 1 1 calc R . . C5 C 0.0420(4) 0.6790(4) 0.5792(3) 0.0432(14) Uani 1 1 d . . . H5 H 0.0293 0.7188 0.5420 0.052 Uiso 1 1 calc R . . C6 C 0.0627(4) 0.6025(4) 0.5540(3) 0.0432(14) Uani 1 1 d . . . H6 H 0.0640 0.5912 0.4997 0.052 Uiso 1 1 calc R . . C7 C 0.0815(4) 0.5429(3) 0.6090(3) 0.0346(12) Uani 1 1 d . . . H7 H 0.0959 0.4919 0.5915 0.042 Uiso 1 1 calc R . . C8 C 0.0787(4) 0.3928(3) 0.7176(3) 0.0265(11) Uani 1 1 d . . . C9 C -0.0210(4) 0.3838(3) 0.6866(3) 0.0348(13) Uani 1 1 d . . . H9 H -0.0695 0.4234 0.6938 0.042 Uiso 1 1 calc R . . C10 C -0.0464(4) 0.3157(3) 0.6454(3) 0.0343(13) Uani 1 1 d . . . H10 H -0.1126 0.3096 0.6253 0.041 Uiso 1 1 calc R . . C11 C 0.0244(4) 0.2566(3) 0.6333(3) 0.0360(13) Uani 1 1 d . . . H11 H 0.0068 0.2122 0.6031 0.043 Uiso 1 1 calc R . . C12 C 0.1207(4) 0.2632(3) 0.6657(3) 0.0389(13) Uani 1 1 d . . . H12 H 0.1677 0.2224 0.6595 0.047 Uiso 1 1 calc R . . C13 C 0.1482(4) 0.3315(3) 0.7081(3) 0.0316(12) Uani 1 1 d . . . H13 H 0.2137 0.3358 0.7302 0.038 Uiso 1 1 calc R . . C14 C 0.3909(3) 0.5651(3) 0.6816(3) 0.0269(11) Uani 1 1 d . . . C15 C 0.3272(4) 0.6310(3) 0.6735(3) 0.0321(12) Uani 1 1 d . . . H15 H 0.2706 0.6363 0.7061 0.038 Uiso 1 1 calc R . . C16 C 0.3479(4) 0.6887(3) 0.6170(3) 0.0363(13) Uani 1 1 d . . . H16 H 0.3040 0.7316 0.6104 0.044 Uiso 1 1 calc R . . C17 C 0.4336(4) 0.6821(4) 0.5706(3) 0.0429(14) Uani 1 1 d . . . H17 H 0.4477 0.7211 0.5330 0.051 Uiso 1 1 calc R . . C18 C 0.4982(4) 0.6189(4) 0.5795(3) 0.0450(15) Uani 1 1 d . . . H18 H 0.5562 0.6153 0.5482 0.054 Uiso 1 1 calc R . . C19 C 0.4778(4) 0.5602(3) 0.6346(3) 0.0369(13) Uani 1 1 d . . . H19 H 0.5222 0.5174 0.6404 0.044 Uiso 1 1 calc R . . C20 C 0.4055(3) 0.3973(3) 0.7141(3) 0.0241(10) Uani 1 1 d . . . C21 C 0.3776(4) 0.3786(3) 0.6359(3) 0.0325(12) Uani 1 1 d . . . H21 H 0.3492 0.4174 0.6029 0.039 Uiso 1 1 calc R . . C22 C 0.3920(4) 0.3026(3) 0.6071(3) 0.0354(13) Uani 1 1 d . . . H22 H 0.3710 0.2899 0.5554 0.042 Uiso 1 1 calc R . . C23 C 0.4375(4) 0.2453(3) 0.6551(3) 0.0368(13) Uani 1 1 d . . . H23 H 0.4482 0.1944 0.6356 0.044 Uiso 1 1 calc R . . C24 C 0.4668(4) 0.2649(3) 0.7324(3) 0.0409(14) Uani 1 1 d . . . H24 H 0.4974 0.2266 0.7648 0.049 Uiso 1 1 calc R . . C25 C 0.4516(4) 0.3398(3) 0.7621(3) 0.0310(12) Uani 1 1 d . . . H25 H 0.4720 0.3521 0.8141 0.037 Uiso 1 1 calc R . . C26 C 0.3211(4) 0.6489(3) 0.9692(3) 0.0379(13) Uani 1 1 d . . . H26 H 0.3781 0.6657 0.9413 0.046 Uiso 1 1 calc R . . C27 C 0.2183(5) 0.6606(3) 0.9461(3) 0.0409(14) Uani 1 1 d . . . H27 H 0.1954 0.6863 0.9001 0.049 Uiso 1 1 calc R . . C28 C 0.1570(4) 0.6269(3) 1.0044(3) 0.0378(13) Uani 1 1 d . . . H28 H 0.0858 0.6259 1.0036 0.045 Uiso 1 1 calc R . . C29 C 0.2202(4) 0.5948(3) 1.0640(3) 0.0355(13) Uani 1 1 d . . . H29 H 0.1987 0.5697 1.1103 0.043 Uiso 1 1 calc R . . C30 C 0.3223(4) 0.6073(3) 1.0416(3) 0.0378(14) Uani 1 1 d . . . H30 H 0.3803 0.5910 1.0699 0.045 Uiso 1 1 calc R . . C31 C 0.1812(4) 0.3563(3) 0.9683(4) 0.0424(15) Uani 1 1 d . . . H31 H 0.1191 0.3410 0.9455 0.051 Uiso 1 1 calc R . . C32 C 0.1940(4) 0.3965(3) 1.0395(3) 0.0367(13) Uani 1 1 d . . . H32 H 0.1418 0.4135 1.0725 0.044 Uiso 1 1 calc R . . C33 C 0.2981(4) 0.4073(3) 1.0534(3) 0.0358(13) Uani 1 1 d . . . H33 H 0.3276 0.4321 1.0977 0.043 Uiso 1 1 calc R . . C34 C 0.3505(4) 0.3743(3) 0.9894(3) 0.0381(13) Uani 1 1 d . . . H34 H 0.4211 0.3737 0.9830 0.046 Uiso 1 1 calc R . . C35 C 0.2779(5) 0.3425(3) 0.9366(3) 0.0424(14) Uani 1 1 d . . . H35 H 0.2914 0.3167 0.8889 0.051 Uiso 1 1 calc R . . C36 C 0.7503(6) 0.5444(6) 0.6604(6) 0.086(2) Uani 1 1 d DU . . C37 C 0.7483(5) 0.5207(6) 0.5786(5) 0.0791(18) Uani 1 1 d U . . H37 H 0.7670 0.5543 0.5373 0.095 Uiso 1 1 calc R . . C38 C 0.7177(7) 0.4471(6) 0.5663(6) 0.095(2) Uani 1 1 d U . . H38 H 0.7154 0.4308 0.5133 0.114 Uiso 1 1 calc R . . C39 C 0.6878(6) 0.3890(6) 0.6235(6) 0.092(2) Uani 1 1 d U . . H39 H 0.6660 0.3380 0.6107 0.110 Uiso 1 1 calc R . . C40 C 0.6953(7) 0.4175(7) 0.6981(6) 0.100(2) Uani 1 1 d U . . H40 H 0.6805 0.3831 0.7398 0.120 Uiso 1 1 calc R . . C41 C 0.7236(6) 0.4945(6) 0.7179(5) 0.0798(18) Uani 1 1 d U . . H41 H 0.7238 0.5110 0.7708 0.096 Uiso 1 1 calc R . . C42 C 0.7764(8) 0.6271(6) 0.6768(7) 0.131(3) Uani 1 1 d DU . . H42A H 0.7158 0.6555 0.6913 0.197 Uiso 1 1 calc R . . H42B H 0.8051 0.6506 0.6300 0.197 Uiso 1 1 calc R . . H42C H 0.8255 0.6294 0.7199 0.197 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02594(10) 0.02038(11) 0.02218(9) 0.00029(9) -0.00040(6) 0.00054(8) S1 0.0259(6) 0.0390(8) 0.0269(6) -0.0012(6) 0.0032(5) 0.0019(6) S2 0.0249(5) 0.0315(7) 0.0279(6) -0.0017(5) -0.0019(5) -0.0022(5) P1 0.0240(6) 0.0244(7) 0.0235(6) -0.0008(5) -0.0014(5) 0.0003(5) P2 0.0244(6) 0.0232(7) 0.0241(6) -0.0005(5) 0.0012(4) 0.0004(5) C1 0.028(2) 0.020(3) 0.020(2) -0.0018(19) 0.0000(17) 0.000(2) C2 0.023(2) 0.023(3) 0.031(3) 0.000(2) 0.001(2) 0.000(2) C3 0.044(3) 0.043(4) 0.034(3) -0.002(3) -0.003(3) 0.011(3) C4 0.059(4) 0.026(3) 0.048(4) 0.002(3) -0.002(3) 0.016(3) C5 0.050(3) 0.041(4) 0.039(3) 0.013(3) 0.002(3) 0.007(3) C6 0.055(4) 0.044(4) 0.031(3) 0.007(3) -0.001(3) 0.001(3) C7 0.045(3) 0.030(3) 0.029(3) -0.003(2) -0.003(2) 0.000(2) C8 0.032(3) 0.024(3) 0.023(3) 0.002(2) 0.004(2) -0.004(2) C9 0.033(3) 0.027(3) 0.045(3) 0.005(2) -0.008(2) -0.005(2) C10 0.032(3) 0.034(3) 0.037(3) 0.004(2) -0.012(2) -0.007(2) C11 0.046(3) 0.033(3) 0.029(3) -0.004(2) -0.002(2) -0.011(3) C12 0.038(3) 0.034(3) 0.045(3) -0.010(3) 0.004(3) 0.000(2) C13 0.031(3) 0.028(3) 0.037(3) -0.002(2) -0.001(2) -0.002(2) C14 0.024(3) 0.025(3) 0.031(3) -0.001(2) -0.004(2) -0.001(2) C15 0.032(3) 0.023(3) 0.041(3) 0.003(2) 0.001(2) -0.002(2) C16 0.031(3) 0.031(3) 0.047(3) 0.010(3) -0.001(3) 0.004(2) C17 0.044(3) 0.041(4) 0.044(3) 0.016(3) 0.005(3) -0.003(3) C18 0.037(3) 0.052(4) 0.046(3) 0.016(3) 0.015(3) 0.012(3) C19 0.033(3) 0.034(3) 0.044(3) 0.013(3) 0.009(2) 0.008(2) C20 0.017(2) 0.028(3) 0.026(3) 0.000(2) 0.003(2) 0.0002(19) C21 0.041(3) 0.026(3) 0.030(3) 0.000(2) 0.002(2) 0.002(2) C22 0.034(3) 0.041(3) 0.031(3) -0.010(2) 0.009(2) -0.007(2) C23 0.036(3) 0.029(3) 0.046(3) -0.011(3) 0.006(3) 0.001(2) C24 0.039(3) 0.032(3) 0.051(4) 0.000(3) -0.004(3) 0.010(2) C25 0.032(3) 0.032(3) 0.029(3) -0.001(2) -0.004(2) 0.005(2) C26 0.039(3) 0.028(3) 0.047(3) -0.010(3) 0.011(3) -0.006(2) C27 0.053(4) 0.026(3) 0.044(3) -0.004(3) 0.001(3) 0.010(3) C28 0.034(3) 0.034(3) 0.045(3) -0.010(3) 0.001(3) 0.009(2) C29 0.051(4) 0.031(3) 0.025(3) -0.006(2) 0.000(3) 0.004(2) C30 0.041(3) 0.029(3) 0.043(3) -0.009(3) -0.008(3) 0.004(2) C31 0.042(3) 0.034(3) 0.051(4) 0.012(3) -0.004(3) -0.009(3) C32 0.036(3) 0.032(3) 0.043(3) 0.011(3) 0.010(3) 0.004(2) C33 0.046(3) 0.032(3) 0.030(3) 0.005(2) -0.001(3) 0.003(3) C34 0.037(3) 0.033(3) 0.044(3) 0.012(3) 0.007(3) 0.006(2) C35 0.072(4) 0.023(3) 0.033(3) 0.005(2) 0.006(3) 0.002(3) C36 0.069(4) 0.095(3) 0.094(3) -0.009(3) 0.003(3) 0.013(3) C37 0.060(4) 0.103(4) 0.074(3) 0.006(3) 0.005(3) 0.021(3) C38 0.081(4) 0.107(4) 0.096(4) -0.015(3) 0.005(4) 0.020(4) C39 0.067(4) 0.095(4) 0.114(4) -0.007(3) -0.002(4) 0.014(3) C40 0.084(4) 0.108(4) 0.108(4) 0.017(3) -0.002(4) 0.013(4) C41 0.064(3) 0.111(4) 0.065(3) -0.004(3) -0.004(3) 0.022(3) C42 0.122(5) 0.117(4) 0.155(5) -0.021(4) -0.008(4) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U C1 2.336(4) . ? U C27 2.705(5) . ? U C32 2.710(5) . ? U C26 2.714(5) . ? U C33 2.727(5) . ? U C31 2.728(5) . ? U C34 2.739(5) . ? U C35 2.741(5) . ? U C28 2.745(5) . ? U C30 2.754(5) . ? U C29 2.792(5) . ? U S1 2.8656(11) . ? U S2 2.8694(12) . ? S1 P1 2.0344(16) . ? S2 P2 2.0352(16) . ? P1 C1 1.684(4) . ? P1 C8 1.806(5) . ? P1 C2 1.817(5) . ? P2 C1 1.678(5) . ? P2 C14 1.812(5) . ? P2 C20 1.828(5) . ? C2 C7 1.381(7) . ? C2 C3 1.404(7) . ? C3 C4 1.386(7) . ? C3 H3 0.9300 . ? C4 C5 1.386(8) . ? C4 H4 0.9300 . ? C5 C6 1.386(8) . ? C5 H5 0.9300 . ? C6 C7 1.384(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.388(7) . ? C8 C9 1.404(6) . ? C9 C10 1.378(7) . ? C9 H9 0.9300 . ? C10 C11 1.378(7) . ? C10 H10 0.9300 . ? C11 C12 1.368(7) . ? C11 H11 0.9300 . ? C12 C13 1.397(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.394(7) . ? C14 C15 1.394(7) . ? C15 C16 1.386(7) . ? C15 H15 0.9300 . ? C16 C17 1.377(7) . ? C16 H16 0.9300 . ? C17 C18 1.368(8) . ? C17 H17 0.9300 . ? C18 C19 1.383(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.389(6) . ? C20 C25 1.391(6) . ? C21 C22 1.384(7) . ? C21 H21 0.9300 . ? C22 C23 1.386(7) . ? C22 H22 0.9300 . ? C23 C24 1.385(7) . ? C23 H23 0.9300 . ? C24 C25 1.374(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C30 1.401(8) . ? C26 C27 1.406(7) . ? C26 H26 0.9300 . ? C27 C28 1.393(8) . ? C27 H27 0.9300 . ? C28 C29 1.397(7) . ? C28 H28 0.9300 . ? C29 C30 1.407(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.379(8) . ? C31 C35 1.397(8) . ? C31 H31 0.9300 . ? C32 C33 1.389(7) . ? C32 H32 0.9300 . ? C33 C34 1.397(7) . ? C33 H33 0.9300 . ? C34 C35 1.395(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.330(11) . ? C36 C37 1.427(11) . ? C36 C42 1.461(8) . ? C37 C38 1.320(13) . ? C37 H37 0.9300 . ? C38 C39 1.429(12) . ? C38 H38 0.9300 . ? C39 C40 1.341(12) . ? C39 H39 0.9300 . ? C40 C41 1.389(12) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 C1 U C27 102.38(16) . . ? C1 U C32 127.83(17) . . ? C27 U C32 121.91(18) . . ? C1 U C26 110.99(17) . . ? C27 U C26 30.08(15) . . ? C32 U C26 121.17(17) . . ? C1 U C33 135.43(16) . . ? C27 U C33 121.79(17) . . ? C32 U C33 29.60(15) . . ? C26 U C33 105.26(17) . . ? C1 U C31 98.51(17) . . ? C27 U C31 144.2(2) . . ? C32 U C31 29.38(17) . . ? C26 U C31 150.49(18) . . ? C33 U C31 48.61(17) . . ? C1 U C34 107.70(16) . . ? C27 U C34 143.99(17) . . ? C32 U C34 48.87(16) . . ? C26 U C34 117.41(18) . . ? C33 U C34 29.63(15) . . ? C31 U C34 48.74(17) . . ? C1 U C35 87.45(16) . . ? C27 U C35 170.02(18) . . ? C32 U C35 48.72(17) . . ? C26 U C35 146.72(18) . . ? C33 U C35 48.67(17) . . ? C31 U C35 29.60(17) . . ? C34 U C35 29.49(16) . . ? C1 U C28 122.46(16) . . ? C27 U C28 29.60(17) . . ? C32 U C28 93.09(18) . . ? C26 U C28 48.98(16) . . ? C33 U C28 100.74(17) . . ? C31 U C28 115.0(2) . . ? C34 U C28 129.72(17) . . ? C35 U C28 141.72(18) . . ? C1 U C30 139.85(17) . . ? C27 U C30 49.13(16) . . ? C32 U C30 92.06(18) . . ? C26 U C30 29.67(16) . . ? C33 U C30 76.56(17) . . ? C31 U C30 121.04(18) . . ? C34 U C30 94.87(17) . . ? C35 U C30 123.19(16) . . ? C28 U C30 48.65(16) . . ? C1 U C29 150.37(16) . . ? C27 U C29 48.63(17) . . ? C32 U C29 75.98(18) . . ? C26 U C29 48.65(17) . . ? C33 U C29 74.17(17) . . ? C31 U C29 104.26(18) . . ? C34 U C29 101.56(16) . . ? C35 U C29 121.40(16) . . ? C28 U C29 29.21(15) . . ? C30 U C29 29.38(16) . . ? C1 U S1 68.29(11) . . ? C27 U S1 84.09(13) . . ? C32 U S1 88.91(12) . . ? C26 U S1 114.12(12) . . ? C33 U S1 118.50(12) . . ? C31 U S1 77.05(12) . . ? C34 U S1 125.22(12) . . ? C35 U S1 98.21(13) . . ? C28 U S1 75.23(11) . . ? C30 U S1 123.86(12) . . ? C29 U S1 98.49(12) . . ? C1 U S2 67.90(11) . . ? C27 U S2 97.02(14) . . ? C32 U S2 125.47(12) . . ? C26 U S2 74.63(12) . . ? C33 U S2 98.81(12) . . ? C31 U S2 117.79(14) . . ? C34 U S2 76.94(12) . . ? C35 U S2 88.19(13) . . ? C28 U S2 123.31(13) . . ? C30 U S2 86.24(13) . . ? C29 U S2 115.62(12) . . ? S1 U S2 135.33(3) . . ? P1 S1 U 80.75(5) . . ? P2 S2 U 80.90(5) . . ? C1 P1 C8 114.4(2) . . ? C1 P1 C2 114.2(2) . . ? C8 P1 C2 103.1(2) . . ? C1 P1 S1 104.73(16) . . ? C8 P1 S1 110.62(17) . . ? C2 P1 S1 109.84(17) . . ? C1 P2 C14 115.1(2) . . ? C1 P2 C20 112.4(2) . . ? C14 P2 C20 105.1(2) . . ? C1 P2 S2 104.31(16) . . ? C14 P2 S2 110.12(16) . . ? C20 P2 S2 109.89(15) . . ? P2 C1 P1 147.1(3) . . ? P2 C1 U 106.7(2) . . ? P1 C1 U 106.1(2) . . ? C7 C2 C3 119.1(5) . . ? C7 C2 P1 121.3(4) . . ? C3 C2 P1 119.2(4) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 119.8(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C2 C7 C6 120.4(5) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C13 C8 C9 118.8(5) . . ? C13 C8 P1 120.3(4) . . ? C9 C8 P1 120.7(4) . . ? C10 C9 C8 119.5(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.3(5) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 120.6(5) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C19 C14 C15 118.9(5) . . ? C19 C14 P2 121.1(4) . . ? C15 C14 P2 119.9(4) . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.5(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 120.0(5) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C21 C20 C25 119.5(5) . . ? C21 C20 P2 119.8(4) . . ? C25 C20 P2 120.1(4) . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.1(5) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 121.2(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C20 119.7(5) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? C30 C26 C27 107.9(5) . . ? C30 C26 U 76.7(3) . . ? C27 C26 U 74.6(3) . . ? C30 C26 H26 126.0 . . ? C27 C26 H26 126.0 . . ? U C26 H26 114.9 . . ? C28 C27 C26 107.9(5) . . ? C28 C27 U 76.8(3) . . ? C26 C27 U 75.3(3) . . ? C28 C27 H27 126.1 . . ? C26 C27 H27 126.1 . . ? U C27 H27 114.2 . . ? C27 C28 C29 108.6(5) . . ? C27 C28 U 73.6(3) . . ? C29 C28 U 77.3(3) . . ? C27 C28 H28 125.7 . . ? C29 C28 H28 125.7 . . ? U C28 H28 115.5 . . ? C28 C29 C30 107.8(5) . . ? C28 C29 U 73.5(3) . . ? C30 C29 U 73.8(3) . . ? C28 C29 H29 126.1 . . ? C30 C29 H29 126.1 . . ? U C29 H29 118.5 . . ? C26 C30 C29 107.9(5) . . ? C26 C30 U 73.6(3) . . ? C29 C30 U 76.8(3) . . ? C26 C30 H30 126.1 . . ? C29 C30 H30 126.1 . . ? U C30 H30 115.7 . . ? C32 C31 C35 108.2(5) . . ? C32 C31 U 74.6(3) . . ? C35 C31 U 75.7(3) . . ? C32 C31 H31 125.9 . . ? C35 C31 H31 125.9 . . ? U C31 H31 115.9 . . ? C31 C32 C33 108.4(5) . . ? C31 C32 U 76.1(3) . . ? C33 C32 U 75.9(3) . . ? C31 C32 H32 125.8 . . ? C33 C32 H32 125.8 . . ? U C32 H32 114.5 . . ? C32 C33 C34 108.0(5) . . ? C32 C33 U 74.5(3) . . ? C34 C33 U 75.7(3) . . ? C32 C33 H33 126.0 . . ? C34 C33 H33 126.0 . . ? U C33 H33 116.0 . . ? C35 C34 C33 107.6(5) . . ? C35 C34 U 75.4(3) . . ? C33 C34 U 74.7(3) . . ? C35 C34 H34 126.2 . . ? C33 C34 H34 126.2 . . ? U C34 H34 115.9 . . ? C34 C35 C31 107.8(5) . . ? C34 C35 U 75.2(3) . . ? C31 C35 U 74.7(3) . . ? C34 C35 H35 126.1 . . ? C31 C35 H35 126.1 . . ? U C35 H35 116.2 . . ? C41 C36 C37 121.0(9) . . ? C41 C36 C42 122.1(10) . . ? C37 C36 C42 116.7(10) . . ? C38 C37 C36 114.5(9) . . ? C38 C37 H37 122.7 . . ? C36 C37 H37 122.7 . . ? C37 C38 C39 128.8(10) . . ? C37 C38 H38 115.6 . . ? C39 C38 H38 115.6 . . ? C40 C39 C38 111.2(10) . . ? C40 C39 H39 124.4 . . ? C38 C39 H39 124.4 . . ? C39 C40 C41 125.0(10) . . ? C39 C40 H40 117.5 . . ? C41 C40 H40 117.5 . . ? C36 C41 C40 119.4(9) . . ? C36 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ?