# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1915 data_s92 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H56 N4 S4 U' _chemical_formula_weight 959.16 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -10.6700 9.6540 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.287(4) _cell_length_b 18.278(35) _cell_length_c 20.606(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4251.1(88) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method ? _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 3.887 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12265 _diffrn_reflns_av_R_equivalents 0.1704 _diffrn_reflns_av_sigmaI/netI 0.8348 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.23 _reflns_number_total 6162 _reflns_number_observed 968 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 6162 _refine_ls_number_parameters 406 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_obs 0.0497 _refine_ls_wR_factor_all 0.1343 _refine_ls_wR_factor_obs 0.0804 _refine_ls_goodness_of_fit_all 0.369 _refine_ls_goodness_of_fit_obs 0.682 _refine_ls_restrained_S_all 0.384 _refine_ls_restrained_S_obs 0.713 _refine_ls_shift/esd_max 1.627 _refine_ls_shift/esd_mean 0.163 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U1 U 0.87200(10) 0.07311(7) 0.84998(6) 0.0421(3) Uani 1 d . . S1 S 0.8533(7) 0.1326(5) 0.7216(3) 0.049(2) Uani 1 d . . S2 S 0.8454(7) -0.0191(5) 0.9599(4) 0.051(2) Uani 1 d . . S3 S 0.6976(6) 0.1817(5) 0.8846(4) 0.045(2) Uani 1 d . . S4 S 1.0984(6) 0.0028(4) 0.8371(4) 0.047(2) Uani 1 d . . N1 N 0.8449(17) 0.0434(13) 0.7425(9) 0.043(7) Uani 1 d . . N2 N 0.7414(20) -0.0062(16) 0.8992(13) 0.051(6) Uani 1 d U . N3 N 0.8385(16) 0.1741(12) 0.9128(11) 0.044(7) Uani 1 d . . N4 N 1.0731(13) 0.0926(12) 0.8444(13) 0.047(7) Uani 1 d . . C1 C 0.7066(9) 0.1632(8) 0.7008(8) 0.042(8) Uani 1 d G . C2 C 0.6058(13) 0.1240(7) 0.7179(7) 0.035(7) Uani 1 d G . H2 H 0.6129(18) 0.0799(9) 0.7400(10) 0.043 Uiso 1 calc R . C3 C 0.4943(10) 0.1509(8) 0.7020(8) 0.029(7) Uani 1 d GU . H3 H 0.4268(13) 0.1247(11) 0.7134(12) 0.034 Uiso 1 calc R . C4 C 0.4837(9) 0.2169(9) 0.6690(8) 0.055(9) Uani 1 d G . H4 H 0.4091(10) 0.2349(12) 0.6583(12) 0.066 Uiso 1 calc R . C5 C 0.5845(12) 0.2561(7) 0.6519(8) 0.045(6) Uani 1 d GU . H5 H 0.5774(17) 0.3002(9) 0.6299(12) 0.054 Uiso 1 calc R . C6 C 0.6960(10) 0.2292(8) 0.6679(9) 0.047(10) Uani 1 d G . H6 H 0.7635(12) 0.2554(11) 0.6564(13) 0.056 Uiso 1 calc R . C7 C 0.9032(14) -0.1106(7) 0.9510(9) 0.034(7) Uani 1 d GU . C8 C 0.8922(14) -0.1468(10) 0.8920(7) 0.064(9) Uani 1 d G . H8 H 0.8534(20) -0.1243(14) 0.8575(9) 0.077 Uiso 1 calc R . C9 C 0.9391(15) -0.2166(10) 0.8845(7) 0.087(12) Uani 1 d GU . H9 H 0.9317(23) -0.2408(14) 0.8450(9) 0.104 Uiso 1 calc R . C10 C 0.9971(15) -0.2502(8) 0.9360(10) 0.073(9) Uani 1 d GU . H10 H 1.0285(21) -0.2969(9) 0.9310(15) 0.087 Uiso 1 calc R . C11 C 1.0081(14) -0.2140(11) 0.9951(8) 0.065(11) Uani 1 d G . H11 H 1.0469(20) -0.2364(15) 1.0295(11) 0.078 Uiso 1 calc R . C12 C 0.9611(14) -0.1442(11) 1.0025(6) 0.071(12) Uani 1 d G . H12 H 0.9685(22) -0.1199(15) 1.0420(8) 0.085 Uiso 1 calc R . C13 C 0.6918(16) 0.2639(8) 0.8389(9) 0.051(8) Uani 1 d GU . C14 C 0.5810(13) 0.2915(10) 0.8224(9) 0.069(11) Uani 1 d G . H14 H 0.5128(16) 0.2662(13) 0.8340(13) 0.083 Uiso 1 calc R . C15 C 0.5723(11) 0.3571(10) 0.7885(8) 0.066(9) Uani 1 d GU . H15 H 0.4982(12) 0.3756(14) 0.7775(12) 0.079 Uiso 1 calc R . C16 C 0.6742(15) 0.3950(8) 0.7711(8) 0.048(8) Uani 1 d GU . H16 H 0.6683(22) 0.4388(10) 0.7485(12) 0.058 Uiso 1 calc R . C17 C 0.7849(11) 0.3673(10) 0.7876(9) 0.070(12) Uani 1 d G . H17 H 0.8531(14) 0.3927(14) 0.7759(13) 0.084 Uiso 1 calc R . C18 C 0.7937(12) 0.3018(10) 0.8215(9) 0.056(9) Uani 1 d G . H18 H 0.8678(14) 0.2833(15) 0.8325(13) 0.067 Uiso 1 calc R . C19 C 1.1693(12) -0.0222(9) 0.9105(7) 0.028(7) Uani 1 d G . C20 C 1.1726(12) 0.0202(7) 0.9664(9) 0.028(7) Uani 1 d GU . H20 H 1.1419(18) 0.0674(8) 0.9660(13) 0.033 Uiso 1 calc R . C21 C 1.2218(13) -0.0079(11) 1.0230(7) 0.070(11) Uani 1 d G . H21 H 1.2240(20) 0.0205(15) 1.0604(8) 0.084 Uiso 1 calc R . C22 C 1.2677(13) -0.0784(12) 1.0236(7) 0.117(15) Uani 1 d G . H22 H 1.3006(19) -0.0972(16) 1.0615(9) 0.140 Uiso 1 calc R . C23 C 1.2644(13) -0.1209(8) 0.9677(10) 0.057(9) Uani 1 d GU . H23 H 1.2951(19) -0.1681(8) 0.9681(14) 0.068 Uiso 1 calc R . C24 C 1.2152(13) -0.0928(8) 0.9111(7) 0.040(8) Uani 1 d G . H24 H 1.2130(20) -0.1212(11) 0.8737(9) 0.048 Uiso 1 calc R . C25 C 0.8583(26) -0.0155(16) 0.6906(14) 0.054(8) Uani 1 d U . C26 C 0.7616(22) -0.0092(20) 0.6482(20) 0.104(15) Uani 1 d . . H26A H 0.6892(22) -0.0137(142) 0.6724(27) 0.157 Uiso 1 calc R . H26B H 0.7655(121) -0.0472(79) 0.6162(75) 0.157 Uiso 1 calc R . H26C H 0.7639(123) 0.0376(52) 0.6272(92) 0.157 Uiso 1 calc R . C27 C 0.9758(18) -0.0031(15) 0.6565(17) 0.070(9) Uani 1 d U . H27A H 0.9778(80) -0.0309(93) 0.6170(57) 0.106 Uiso 1 calc R . H27B H 1.0394(21) -0.0185(114) 0.6842(46) 0.106 Uiso 1 calc R . H27C H 0.9847(87) 0.0479(22) 0.6466(94) 0.106 Uiso 1 calc R . C28 C 0.8487(19) -0.0916(14) 0.7245(11) 0.041(8) Uani 1 d . . H28A H 0.7718(50) -0.0966(34) 0.7439(60) 0.061 Uiso 1 calc R . H28B H 0.9085(85) -0.0955(33) 0.7575(47) 0.061 Uiso 1 calc R . H28C H 0.8600(122) -0.1297(14) 0.6930(16) 0.061 Uiso 1 calc R . C29 C 0.6172(26) -0.0287(15) 0.9119(12) 0.036(7) Uani 1 d U . C30 C 0.6079(18) -0.1044(12) 0.9360(10) 0.020(6) Uani 1 d U . H30A H 0.6529(82) -0.1093(19) 0.9753(29) 0.030 Uiso 1 calc R . H30B H 0.6384(92) -0.1374(13) 0.9038(23) 0.030 Uiso 1 calc R . H30C H 0.5263(21) -0.1158(24) 0.9444(54) 0.030 Uiso 1 calc R . C31 C 0.5643(20) 0.0188(17) 0.9671(14) 0.069(10) Uani 1 d U . H31A H 0.6088(105) 0.0113(77) 1.0062(26) 0.104 Uiso 1 calc R . H31B H 0.4832(55) 0.0051(70) 0.9742(61) 0.104 Uiso 1 calc R . H31C H 0.5680(143) 0.0695(19) 0.9550(39) 0.104 Uiso 1 calc R . C32 C 0.5502(19) -0.0183(17) 0.8532(17) 0.080(12) Uani 1 d . . H32A H 0.5810(117) -0.0497(77) 0.8199(33) 0.120 Uiso 1 calc R . H32B H 0.5565(143) 0.0317(27) 0.8395(55) 0.120 Uiso 1 calc R . H32C H 0.4686(38) -0.0301(110) 0.8610(31) 0.120 Uiso 1 calc R . C33 C 0.8493(19) 0.2044(14) 0.9765(12) 0.031(7) Uani 1 d U . C34 C 0.7559(21) 0.1915(18) 1.0351(14) 0.060(9) Uani 1 d U . H34A H 0.6778(34) 0.2047(98) 1.0208(33) 0.090 Uiso 1 calc R . H34B H 0.7778(99) 0.2211(76) 1.0716(36) 0.090 Uiso 1 calc R . H34C H 0.7567(118) 0.1408(26) 1.0475(60) 0.090 Uiso 1 calc R . C35 C 0.8868(28) 0.2908(18) 0.9685(16) 0.100(11) Uani 1 d U . H35A H 0.8739(193) 0.3159(33) 1.0088(34) 0.151 Uiso 1 calc R . H35B H 0.8394(146) 0.3129(37) 0.9351(77) 0.151 Uiso 1 calc R . H35C H 0.9689(59) 0.2940(18) 0.9568(113) 0.151 Uiso 1 calc R . C36 C 0.9728(24) 0.1791(18) 1.0053(14) 0.068(11) Uani 1 d . . H36A H 0.9608(33) 0.1384(75) 1.0341(81) 0.102 Uiso 1 calc R . H36B H 1.0082(89) 0.2188(39) 1.0288(87) 0.102 Uiso 1 calc R . H36C H 1.0243(69) 0.1646(112) 0.9705(15) 0.102 Uiso 1 calc R . C37 C 1.1688(22) 0.1460(19) 0.8165(15) 0.061(12) Uani 1 d . . C38 C 1.1235(24) 0.2181(12) 0.8189(11) 0.045(7) Uani 1 d . . H38A H 1.0776(103) 0.2276(29) 0.7806(31) 0.067 Uiso 1 calc R . H38B H 1.1879(24) 0.2522(13) 0.8213(70) 0.067 Uiso 1 calc R . H38C H 1.0740(100) 0.2234(25) 0.8566(35) 0.067 Uiso 1 calc R . C39 C 1.1774(21) 0.1202(18) 0.7405(15) 0.076(13) Uani 1 d . . H39A H 1.2402(133) 0.1465(85) 0.7194(30) 0.113 Uiso 1 calc R . H39B H 1.1037(75) 0.1304(109) 0.7190(31) 0.113 Uiso 1 calc R . H39C H 1.1934(177) 0.0687(28) 0.7385(15) 0.113 Uiso 1 calc R . C40 C 1.2794(20) 0.1356(15) 0.8459(18) 0.063(9) Uani 1 d . . H40A H 1.3395(32) 0.1595(91) 0.8207(55) 0.095 Uiso 1 calc R . H40B H 1.2963(79) 0.0842(15) 0.8485(88) 0.095 Uiso 1 calc R . H40C H 1.2781(60) 0.1561(98) 0.8888(40) 0.095 Uiso 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 0.0487(5) 0.0371(5) 0.0406(6) -0.0040(8) 0.0003(8) 0.0001(8) S1 0.066(5) 0.050(5) 0.029(5) 0.009(4) -0.000(4) 0.005(5) S2 0.065(6) 0.054(6) 0.035(5) 0.002(4) 0.003(4) -0.011(5) S3 0.064(5) 0.041(6) 0.029(5) 0.002(4) 0.010(4) -0.002(4) S4 0.058(5) 0.041(5) 0.043(6) -0.001(4) -0.000(4) 0.000(4) N1 0.049(15) 0.065(20) 0.015(13) 0.019(11) 0.000(10) -0.022(12) N2 0.056(9) 0.054(10) 0.043(9) -0.009(8) 0.017(8) -0.012(8) N3 0.050(16) 0.032(16) 0.052(17) -0.003(13) -0.014(12) -0.011(11) N4 0.035(10) 0.051(19) 0.055(16) -0.015(17) -0.003(12) 0.008(10) C1 0.033(16) 0.032(20) 0.061(23) 0.020(17) -0.031(15) -0.016(14) C2 0.051(18) 0.031(18) 0.024(16) -0.009(12) 0.023(14) -0.006(14) C3 0.023(9) 0.040(10) 0.023(10) -0.002(8) 0.009(8) -0.013(8) C4 0.110(22) 0.034(19) 0.021(22) -0.009(15) -0.010(16) -0.009(17) C5 0.044(9) 0.050(10) 0.040(10) -0.006(9) -0.014(8) 0.015(7) C6 0.033(16) 0.023(18) 0.084(30) -0.016(18) -0.034(16) 0.016(13) C7 0.038(10) 0.037(10) 0.028(10) -0.011(8) -0.012(8) 0.010(8) C8 0.096(23) 0.046(19) 0.049(20) 0.002(15) 0.009(18) 0.010(19) C9 0.092(13) 0.087(15) 0.081(14) -0.005(9) 0.045(9) 0.014(9) C10 0.069(12) 0.069(13) 0.079(13) -0.006(9) -0.006(9) 0.003(9) C11 0.078(23) 0.082(30) 0.035(22) 0.039(20) 0.028(17) 0.033(22) C12 0.055(20) 0.094(34) 0.063(26) 0.054(24) 0.000(18) -0.032(21) C13 0.062(10) 0.040(11) 0.050(11) -0.003(9) -0.013(9) 0.007(8) C14 0.096(25) 0.073(28) 0.039(23) 0.028(19) 0.006(16) 0.001(19) C15 0.066(11) 0.063(12) 0.070(12) -0.010(9) 0.002(9) 0.017(9) C16 0.059(11) 0.049(11) 0.037(11) 0.005(9) 0.011(8) -0.009(8) C17 0.069(20) 0.083(32) 0.058(26) 0.039(22) -0.039(18) -0.010(20) C18 0.077(20) 0.072(27) 0.019(19) -0.011(17) -0.001(14) -0.031(19) C19 0.042(18) 0.010(15) 0.031(17) 0.001(13) 0.013(12) 0.007(11) C20 0.024(10) 0.032(10) 0.027(10) 0.011(8) -0.008(8) 0.001(8) C21 0.061(21) 0.048(24) 0.100(31) 0.005(22) 0.052(20) -0.029(18) C22 0.093(26) 0.106(39) 0.151(42) 0.040(39) -0.027(24) 0.055(30) C23 0.059(12) 0.057(13) 0.054(13) 0.004(9) 0.013(9) -0.005(9) C24 0.057(17) 0.027(21) 0.035(19) 0.007(14) 0.016(14) -0.008(13) C25 0.053(11) 0.053(11) 0.056(11) 0.004(9) -0.006(9) 0.007(9) C26 0.113(26) 0.090(32) 0.110(35) -0.069(34) 0.049(30) -0.033(22) C27 0.075(11) 0.065(12) 0.071(12) -0.009(10) -0.002(9) -0.003(9) C28 0.027(15) 0.051(23) 0.045(18) -0.029(15) -0.001(13) 0.010(13) C29 0.032(10) 0.034(10) 0.042(10) -0.011(8) -0.006(9) 0.003(9) C30 0.016(9) 0.031(10) 0.013(9) 0.017(8) 0.003(7) 0.001(8) C31 0.071(13) 0.068(14) 0.068(13) -0.005(9) 0.005(9) 0.006(9) C32 0.058(18) 0.090(30) 0.091(28) 0.044(29) -0.045(23) -0.002(17) C33 0.022(10) 0.039(10) 0.034(10) 0.006(8) 0.010(8) 0.000(8) C34 0.062(11) 0.055(12) 0.063(12) -0.005(9) -0.008(9) -0.013(9) C35 0.112(13) 0.089(14) 0.100(14) 0.007(9) 0.011(9) 0.002(10) C36 0.095(23) 0.075(31) 0.033(22) -0.008(19) -0.034(18) -0.022(21) C37 0.044(21) 0.076(27) 0.063(25) 0.059(20) 0.038(16) 0.044(17) C38 0.058(16) 0.025(16) 0.052(19) 0.001(13) -0.022(17) -0.007(18) C39 0.020(17) 0.070(30) 0.136(39) -0.037(26) -0.012(18) -0.005(15) C40 0.110(21) 0.025(18) 0.054(23) 0.000(22) 0.014(25) 0.034(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N3 2.28(2) . ? U1 N4 2.30(2) . ? U1 N1 2.30(2) . ? U1 N2 2.30(3) . ? U1 S2 2.840(8) . ? U1 S1 2.867(7) . ? U1 S4 2.873(7) . ? U1 S3 2.885(8) . ? S1 N1 1.69(2) . ? S1 C1 1.799(13) . ? S2 N2 1.73(3) . ? S2 C7 1.80(2) . ? S3 N3 1.70(2) . ? S3 C13 1.774(15) . ? S4 N4 1.67(2) . ? S4 C19 1.771(14) . ? N1 C25 1.53(3) . ? N2 C29 1.48(4) . ? N3 C33 1.43(3) . ? N4 C37 1.57(3) . ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C3 C4 1.39 . ? C4 C5 1.39 . ? C5 C6 1.39 . ? C7 C8 1.39 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C9 C10 1.39 . ? C10 C11 1.39 . ? C11 C12 1.39 . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C25 C26 1.40(4) . ? C25 C28 1.56(4) . ? C25 C27 1.52(3) . ? C29 C32 1.44(4) . ? C29 C30 1.47(3) . ? C29 C31 1.55(3) . ? C33 C36 1.58(3) . ? C33 C34 1.62(3) . ? C33 C35 1.64(4) . ? C37 C40 1.40(3) . ? C37 C38 1.41(4) . ? C37 C39 1.64(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U1 N4 93.8(7) . . ? N3 U1 N1 135.5(8) . . ? N4 U1 N1 96.9(8) . . ? N3 U1 N2 98.8(9) . . ? N4 U1 N2 138.7(9) . . ? N1 U1 N2 100.9(8) . . ? N3 U1 S2 90.6(6) . . ? N4 U1 S2 103.7(7) . . ? N1 U1 S2 127.8(6) . . ? N2 U1 S2 37.6(7) . . ? N3 U1 S1 101.8(6) . . ? N4 U1 S1 88.2(7) . . ? N1 U1 S1 36.1(6) . . ? N2 U1 S1 126.7(7) . . ? S2 U1 S1 162.4(2) . . ? N3 U1 S4 124.1(5) . . ? N4 U1 S4 35.6(6) . . ? N1 U1 S4 85.6(5) . . ? N2 U1 S4 109.2(7) . . ? S2 U1 S4 84.4(2) . . ? S1 U1 S4 98.6(2) . . ? N3 U1 S3 36.0(5) . . ? N4 U1 S3 125.4(6) . . ? N1 U1 S3 108.0(6) . . ? N2 U1 S3 83.6(7) . . ? S2 U1 S3 98.0(2) . . ? S1 U1 S3 85.2(2) . . ? S4 U1 S3 159.6(2) . . ? N1 S1 C1 108.0(10) . . ? N1 S1 U1 53.3(7) . . ? C1 S1 U1 113.9(6) . . ? N2 S2 C7 107.3(12) . . ? N2 S2 U1 54.2(9) . . ? C7 S2 U1 115.5(7) . . ? N3 S3 C13 106.6(10) . . ? N3 S3 U1 52.3(8) . . ? C13 S3 U1 118.4(7) . . ? N4 S4 C19 104.7(11) . . ? N4 S4 U1 53.2(6) . . ? C19 S4 U1 116.0(6) . . ? C25 N1 S1 119.7(17) . . ? C25 N1 U1 146.0(18) . . ? S1 N1 U1 90.6(10) . . ? C29 N2 S2 118.4(20) . . ? C29 N2 U1 148.9(21) . . ? S2 N2 U1 88.3(10) . . ? C33 N3 S3 111.2(16) . . ? C33 N3 U1 144.9(17) . . ? S3 N3 U1 91.6(9) . . ? C37 N4 S4 117.4(17) . . ? C37 N4 U1 142.7(16) . . ? S4 N4 U1 91.2(9) . . ? C2 C1 C6 120.0 . . ? C2 C1 S1 122.2(9) . . ? C6 C1 S1 117.7(9) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 S2 119.8(12) . . ? C12 C7 S2 120.1(12) . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 S3 118.1(12) . . ? C18 C13 S3 121.9(12) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 S4 125.2(11) . . ? C24 C19 S4 114.6(11) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C28 107.3(27) . . ? C26 C25 N1 107.6(25) . . ? C28 C25 N1 107.9(21) . . ? C26 C25 C27 112.3(26) . . ? C28 C25 C27 113.6(23) . . ? N1 C25 C27 107.9(24) . . ? C32 C29 C30 111.6(24) . . ? C32 C29 N2 108.1(25) . . ? C30 C29 N2 112.7(24) . . ? C32 C29 C31 109.9(25) . . ? C30 C29 C31 104.6(23) . . ? N2 C29 C31 109.8(23) . . ? N3 C33 C36 107.8(20) . . ? N3 C33 C34 124.9(21) . . ? C36 C33 C34 104.6(21) . . ? N3 C33 C35 107.5(21) . . ? C36 C33 C35 95.3(20) . . ? C34 C33 C35 112.6(22) . . ? C40 C37 C38 115.6(32) . . ? C40 C37 N4 111.8(23) . . ? C38 C37 N4 108.5(20) . . ? C40 C37 C39 108.8(23) . . ? C38 C37 C39 108.9(23) . . ? N4 C37 C39 102.4(28) . . ? _refine_diff_density_max 1.067 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.110 #===END data_s92-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 Cl N S U' _chemical_formula_weight 724.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/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 9.680(6) _cell_length_b 17.226(10) _cell_length_c 18.166(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.23(7) _cell_angle_gamma 90.00 _cell_volume 2936(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 5.708 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10605 _diffrn_reflns_av_R_equivalents 0.2626 _diffrn_reflns_av_sigmaI/netI 0.5448 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 24.83 _reflns_number_total 4078 _reflns_number_gt 1145 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4078 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2035 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.599 _refine_ls_restrained_S_all 0.599 _refine_ls_shift/su_max 0.587 _refine_ls_shift/su_mean 0.015 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 0.32714(9) 0.43362(6) 0.23128(6) 0.0288(3) Uani 1 1 d . . . Cl Cl 0.2834(6) 0.2877(4) 0.1899(5) 0.052(2) Uani 1 1 d . . . S1 S 0.3723(6) 0.4844(4) 0.3832(4) 0.034(2) Uani 1 1 d . . . N1 N 0.2961(18) 0.3992(11) 0.3429(11) 0.023(5) Uiso 1 1 d . . . C1 C 0.619(2) 0.435(2) 0.2970(15) 0.036(7) Uiso 1 1 d . . . C2 C 0.589(2) 0.5034(16) 0.2502(15) 0.023(7) Uiso 1 1 d . . . C3 C 0.551(2) 0.4859(14) 0.1751(14) 0.017(6) Uiso 1 1 d . . . C4 C 0.558(2) 0.4065(13) 0.1673(13) 0.015(6) Uiso 1 1 d . . . C5 C 0.595(2) 0.3809(16) 0.2410(15) 0.025(7) Uiso 1 1 d . . . C6 C 0.685(2) 0.4324(19) 0.3782(13) 0.038(7) Uiso 1 1 d . . . H6A H 0.6449 0.3892 0.4014 0.056 Uiso 1 1 calc R . . H6B H 0.6669 0.4813 0.4017 0.056 Uiso 1 1 calc R . . H6C H 0.7881 0.4249 0.3863 0.056 Uiso 1 1 calc R . . C7 C 0.610(2) 0.5901(13) 0.2846(14) 0.028(7) Uiso 1 1 d . . . H7A H 0.5468 0.6258 0.2499 0.042 Uiso 1 1 calc R . . H7B H 0.7091 0.6062 0.2910 0.042 Uiso 1 1 calc R . . H7C H 0.5860 0.5909 0.3341 0.042 Uiso 1 1 calc R . . C8 C 0.553(3) 0.5419(17) 0.1090(15) 0.050(9) Uiso 1 1 d . . . H8A H 0.5510 0.5956 0.1265 0.076 Uiso 1 1 calc R . . H8B H 0.4686 0.5324 0.0672 0.076 Uiso 1 1 calc R . . H8C H 0.6391 0.5333 0.0912 0.076 Uiso 1 1 calc R . . C9 C 0.541(3) 0.3560(19) 0.1007(16) 0.055(9) Uiso 1 1 d . . . H9A H 0.5095 0.3870 0.0543 0.083 Uiso 1 1 calc R . . H9B H 0.4704 0.3157 0.1020 0.083 Uiso 1 1 calc R . . H9C H 0.6329 0.3315 0.1011 0.083 Uiso 1 1 calc R . . C10 C 0.644(3) 0.2958(17) 0.2631(18) 0.051(8) Uiso 1 1 d . . . H10A H 0.7474 0.2917 0.2700 0.076 Uiso 1 1 calc R . . H10B H 0.5960 0.2604 0.2227 0.076 Uiso 1 1 calc R . . H10C H 0.6193 0.2818 0.3106 0.076 Uiso 1 1 calc R . . C11 C 0.041(2) 0.4706(13) 0.1869(13) 0.011(5) Uiso 1 1 d . . . C12 C 0.109(2) 0.5469(15) 0.1884(15) 0.029(7) Uiso 1 1 d . . . C13 C 0.191(2) 0.5472(14) 0.1351(13) 0.021(6) Uiso 1 1 d . . . C14 C 0.166(2) 0.4782(16) 0.0891(15) 0.033(7) Uiso 1 1 d . . . C15 C 0.068(2) 0.4292(17) 0.1252(13) 0.024(6) Uiso 1 1 d . . . C16 C -0.068(2) 0.4527(15) 0.2295(13) 0.031(7) Uiso 1 1 d . . . H16A H -0.1293 0.4105 0.2040 0.047 Uiso 1 1 calc R . . H16B H -0.1259 0.4990 0.2312 0.047 Uiso 1 1 calc R . . H16C H -0.0206 0.4368 0.2814 0.047 Uiso 1 1 calc R . . C17 C 0.095(3) 0.6181(17) 0.2361(16) 0.048(8) Uiso 1 1 d . . . H17A H 0.1398 0.6628 0.2177 0.072 Uiso 1 1 calc R . . H17B H 0.1429 0.6081 0.2893 0.072 Uiso 1 1 calc R . . H17C H -0.0058 0.6292 0.2317 0.072 Uiso 1 1 calc R . . C18 C 0.247(2) 0.6182(16) 0.1088(15) 0.040(8) Uiso 1 1 d . . . H18A H 0.1811 0.6612 0.1098 0.060 Uiso 1 1 calc R . . H18B H 0.2563 0.6107 0.0568 0.060 Uiso 1 1 calc R . . H18C H 0.3404 0.6303 0.1422 0.060 Uiso 1 1 calc R . . C19 C 0.197(2) 0.4520(16) 0.0181(14) 0.037(7) Uiso 1 1 d . . . H19A H 0.2338 0.4957 -0.0061 0.056 Uiso 1 1 calc R . . H19B H 0.1101 0.4321 -0.0162 0.056 Uiso 1 1 calc R . . H19C H 0.2693 0.4108 0.0291 0.056 Uiso 1 1 calc R . . C20 C -0.010(3) 0.3596(18) 0.0984(17) 0.058(9) Uiso 1 1 d . . . H20A H -0.0113 0.3258 0.1417 0.088 Uiso 1 1 calc R . . H20B H 0.0352 0.3324 0.0633 0.088 Uiso 1 1 calc R . . H20C H -0.1083 0.3732 0.0722 0.088 Uiso 1 1 calc R . . C21 C 0.237(2) 0.5452(14) 0.4057(14) 0.027(7) Uiso 1 1 d . . . C22 C 0.105(2) 0.5225(16) 0.4092(14) 0.033(7) Uiso 1 1 d . . . H22 H 0.0761 0.4703 0.3978 0.039 Uiso 1 1 calc R . . C23 C 0.014(2) 0.5730(19) 0.4286(14) 0.038(7) Uiso 1 1 d . . . H23 H -0.0783 0.5560 0.4302 0.045 Uiso 1 1 calc R . . C24 C 0.056(2) 0.6533(16) 0.4472(15) 0.037(7) Uiso 1 1 d . . . H24 H -0.0078 0.6890 0.4615 0.044 Uiso 1 1 calc R . . C25 C 0.187(2) 0.6749(16) 0.4434(13) 0.029(7) Uiso 1 1 d . . . H25 H 0.2149 0.7274 0.4542 0.035 Uiso 1 1 calc R . . C26 C 0.285(3) 0.6246(18) 0.4246(16) 0.045(8) Uiso 1 1 d . . . H26 H 0.3780 0.6411 0.4241 0.054 Uiso 1 1 calc R . . C27 C 0.288(2) 0.3301(15) 0.4030(14) 0.025(7) Uiso 1 1 d . . . C28 C 0.305(3) 0.3618(18) 0.4822(15) 0.049(8) Uiso 1 1 d . . . H28A H 0.3070 0.3187 0.5177 0.073 Uiso 1 1 calc R . . H28B H 0.2238 0.3958 0.4830 0.073 Uiso 1 1 calc R . . H28C H 0.3935 0.3915 0.4973 0.073 Uiso 1 1 calc R . . C29 C 0.144(2) 0.2972(18) 0.3667(16) 0.049(8) Uiso 1 1 d . . . H29A H 0.1383 0.2855 0.3132 0.074 Uiso 1 1 calc R . . H29B H 0.0704 0.3352 0.3700 0.074 Uiso 1 1 calc R . . H29C H 0.1292 0.2495 0.3931 0.074 Uiso 1 1 calc R . . C30 C 0.408(2) 0.2759(17) 0.3985(16) 0.047(8) Uiso 1 1 d . . . H30A H 0.4991 0.3029 0.4156 0.070 Uiso 1 1 calc R . . H30B H 0.3959 0.2587 0.3459 0.070 Uiso 1 1 calc R . . H30C H 0.4061 0.2307 0.4311 0.070 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 0.0233(5) 0.0229(5) 0.0379(7) 0.0004(9) 0.0031(4) 0.0003(6) Cl 0.036(4) 0.016(4) 0.095(7) -0.010(5) -0.001(4) 0.003(3) S1 0.030(4) 0.036(5) 0.033(5) 0.010(4) 0.002(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 2.20(2) . ? U1 Cl 2.628(7) . ? U1 C5 2.72(2) . ? U1 C13 2.74(2) . ? U1 C2 2.75(2) . ? U1 C11 2.759(19) . ? U1 C15 2.761(19) . ? U1 C3 2.76(2) . ? U1 C14 2.78(2) . ? U1 C1 2.78(2) . ? U1 C4 2.80(2) . ? U1 S1 2.825(8) . ? S1 N1 1.72(2) . ? S1 C21 1.80(2) . ? N1 C27 1.63(3) . ? C1 C5 1.35(4) . ? C1 C2 1.44(4) . ? C1 C6 1.46(3) . ? C2 C3 1.36(3) . ? C2 C7 1.61(3) . ? C3 C4 1.38(3) . ? C3 C8 1.54(3) . ? C4 C5 1.37(3) . ? C4 C9 1.47(3) . ? C5 C10 1.56(4) . ? C11 C15 1.41(3) . ? C11 C12 1.46(3) . ? C11 C16 1.49(3) . ? C12 C13 1.40(3) . ? C12 C17 1.52(3) . ? C13 C14 1.44(3) . ? C13 C18 1.46(3) . ? C14 C19 1.47(3) . ? C14 C15 1.53(3) . ? C15 C20 1.44(4) . ? C21 C22 1.35(3) . ? C21 C26 1.46(4) . ? C22 C23 1.34(3) . ? C23 C24 1.46(4) . ? C24 C25 1.35(3) . ? C25 C26 1.38(3) . ? C27 C29 1.50(3) . ? C27 C30 1.50(3) . ? C27 C28 1.51(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 Cl 87.5(5) . . ? N1 U1 C5 101.2(7) . . ? Cl U1 C5 77.5(6) . . ? N1 U1 C13 128.9(7) . . ? Cl U1 C13 118.9(5) . . ? C5 U1 C13 125.6(8) . . ? N1 U1 C2 109.4(7) . . ? Cl U1 C2 122.2(6) . . ? C5 U1 C2 45.6(7) . . ? C13 U1 C2 92.9(7) . . ? N1 U1 C11 88.7(7) . . ? Cl U1 C11 93.3(5) . . ? C5 U1 C11 166.0(7) . . ? C13 U1 C11 50.1(7) . . ? C2 U1 C11 139.7(8) . . ? N1 U1 C15 109.2(7) . . ? Cl U1 C15 73.7(6) . . ? C5 U1 C15 136.5(8) . . ? C13 U1 C15 50.4(7) . . ? C2 U1 C15 138.6(8) . . ? C11 U1 C15 29.5(6) . . ? N1 U1 C3 136.4(6) . . ? Cl U1 C3 107.0(5) . . ? C5 U1 C3 46.3(7) . . ? C13 U1 C3 80.1(7) . . ? C2 U1 C3 28.5(7) . . ? C11 U1 C3 129.7(7) . . ? C15 U1 C3 114.2(7) . . ? N1 U1 C14 139.3(7) . . ? Cl U1 C14 89.1(6) . . ? C5 U1 C14 117.6(8) . . ? C13 U1 C14 30.3(7) . . ? C2 U1 C14 106.6(8) . . ? C11 U1 C14 51.0(7) . . ? C15 U1 C14 32.1(7) . . ? C3 U1 C14 83.0(7) . . ? N1 U1 C1 87.8(7) . . ? Cl U1 C1 101.8(7) . . ? C5 U1 C1 28.5(7) . . ? C13 U1 C1 123.1(8) . . ? C2 U1 C1 30.2(8) . . ? C11 U1 C1 164.3(9) . . ? C15 U1 C1 161.9(7) . . ? C3 U1 C1 49.5(7) . . ? C14 U1 C1 132.5(8) . . ? N1 U1 C4 129.8(6) . . ? Cl U1 C4 79.1(5) . . ? C5 U1 C4 28.7(7) . . ? C13 U1 C4 99.3(7) . . ? C2 U1 C4 47.1(7) . . ? C11 U1 C4 139.7(7) . . ? C15 U1 C4 112.7(7) . . ? C3 U1 C4 28.7(6) . . ? C14 U1 C4 89.0(7) . . ? C1 U1 C4 49.5(7) . . ? N1 U1 S1 37.6(5) . . ? Cl U1 S1 123.4(2) . . ? C5 U1 S1 97.1(6) . . ? C13 U1 S1 109.7(5) . . ? C2 U1 S1 80.0(6) . . ? C11 U1 S1 96.7(5) . . ? C15 U1 S1 125.9(5) . . ? C3 U1 S1 108.2(5) . . ? C14 U1 S1 137.7(6) . . ? C1 U1 S1 71.4(6) . . ? C4 U1 S1 120.6(5) . . ? N1 S1 C21 109.4(10) . . ? N1 S1 U1 51.2(7) . . ? C21 S1 U1 117.1(8) . . ? C27 N1 S1 115.0(14) . . ? C27 N1 U1 148.5(15) . . ? S1 N1 U1 91.2(9) . . ? C5 C1 C2 99(2) . . ? C5 C1 C6 134(3) . . ? C2 C1 C6 126(3) . . ? C5 C1 U1 73.0(13) . . ? C2 C1 U1 73.7(12) . . ? C6 C1 U1 125.6(16) . . ? C3 C2 C1 112(2) . . ? C3 C2 C7 125(2) . . ? C1 C2 C7 123(2) . . ? C3 C2 U1 76.3(13) . . ? C1 C2 U1 76.1(13) . . ? C7 C2 U1 118.4(15) . . ? C2 C3 C4 108(2) . . ? C2 C3 C8 126(2) . . ? C4 C3 C8 122(2) . . ? C2 C3 U1 75.2(14) . . ? C4 C3 U1 77.1(15) . . ? C8 C3 U1 130.5(14) . . ? C5 C4 C3 103(2) . . ? C5 C4 C9 124(2) . . ? C3 C4 C9 132(2) . . ? C5 C4 U1 72.2(14) . . ? C3 C4 U1 74.3(15) . . ? C9 C4 U1 120.3(15) . . ? C1 C5 C4 118(3) . . ? C1 C5 C10 118(3) . . ? C4 C5 C10 123(3) . . ? C1 C5 U1 78.5(14) . . ? C4 C5 U1 79.0(13) . . ? C10 C5 U1 123.6(17) . . ? C15 C11 C12 108(2) . . ? C15 C11 C16 127(2) . . ? C12 C11 C16 123(2) . . ? C15 C11 U1 75.3(12) . . ? C12 C11 U1 78.0(12) . . ? C16 C11 U1 126.2(15) . . ? C13 C12 C11 108(2) . . ? C13 C12 C17 122(2) . . ? C11 C12 C17 129(2) . . ? C13 C12 U1 71.2(13) . . ? C11 C12 U1 71.7(12) . . ? C17 C12 U1 123.9(15) . . ? C12 C13 C14 111(2) . . ? C12 C13 C18 123(2) . . ? C14 C13 C18 122(2) . . ? C12 C13 U1 79.8(14) . . ? C14 C13 U1 76.5(14) . . ? C18 C13 U1 130.5(15) . . ? C13 C14 C19 136(3) . . ? C13 C14 C15 104(2) . . ? C19 C14 C15 119(2) . . ? C13 C14 U1 73.3(13) . . ? C19 C14 U1 122.8(17) . . ? C15 C14 U1 73.4(13) . . ? C11 C15 C20 120(2) . . ? C11 C15 C14 109(2) . . ? C20 C15 C14 130(2) . . ? C11 C15 U1 75.2(12) . . ? C20 C15 U1 124.9(19) . . ? C14 C15 U1 74.5(11) . . ? C22 C21 C26 120(2) . . ? C22 C21 S1 126(2) . . ? C26 C21 S1 113.3(19) . . ? C23 C22 C21 121(3) . . ? C22 C23 C24 121(2) . . ? C25 C24 C23 117(3) . . ? C24 C25 C26 123(3) . . ? C25 C26 C21 117(2) . . ? C29 C27 C30 113(2) . . ? C29 C27 C28 115(2) . . ? C30 C27 C28 112(2) . . ? C29 C27 N1 99.9(18) . . ? C30 C27 N1 105(2) . . ? C28 C27 N1 111(2) . . ? _diffrn_measured_fraction_theta_max 0.802 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.802 _refine_diff_density_max 2.005 _refine_diff_density_min -1.610 _refine_diff_density_rms 0.244 #===END data_s92-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 Br N S U' _chemical_formula_weight 768.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.724(4) _cell_length_b 17.377(15) _cell_length_c 18.196(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.74(4) _cell_angle_gamma 90.00 _cell_volume 2987(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.860 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8557 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.2232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4050 _reflns_number_gt 2044 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4050 _refine_ls_number_parameters 320 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.601 _refine_ls_restrained_S_all 0.600 _refine_ls_shift/su_max 7.940 _refine_ls_shift/su_mean 0.204 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 Br1 Br 0.22966(14) 0.22309(6) 0.31336(9) 0.0417(4) Uani 1 1 d . . . U1 U 0.17748(5) 0.06982(2) 0.26920(3) 0.02290(13) Uani 1 1 d . . . S1 S 0.1297(3) 0.01891(15) 0.1169(2) 0.0279(8) Uani 1 1 d . . . N1 N 0.2054(9) 0.1037(4) 0.1509(5) 0.021(2) Uani 1 1 d . . . C1 C -0.0553(13) 0.0977(6) 0.3315(8) 0.034(4) Uani 1 1 d . . . C2 C -0.0497(12) 0.0150(6) 0.3259(8) 0.023(3) Uani 1 1 d . . . C3 C -0.0826(14) -0.0022(6) 0.2471(7) 0.026(3) Uani 1 1 d . . . C4 C -0.1131(12) 0.0672(7) 0.2032(7) 0.031(3) Uani 1 1 d . . . C5 C -0.0933(11) 0.1302(6) 0.2589(7) 0.018(3) Uani 1 1 d U . . C6 C -0.0442(14) 0.1445(7) 0.4051(7) 0.041(4) Uani 1 1 d . . . H6A H -0.0008 0.1134 0.4479 0.061 Uiso 1 1 calc R . . H6B H -0.1372 0.1595 0.4090 0.061 Uiso 1 1 calc R . . H6C H 0.0123 0.1896 0.4040 0.061 Uiso 1 1 calc R . . C7 C -0.0516(14) -0.0386(6) 0.3906(8) 0.041(4) Uani 1 1 d . . . H7A H -0.1475 -0.0469 0.3938 0.062 Uiso 1 1 calc R . . H7B H 0.0014 -0.0161 0.4369 0.062 Uiso 1 1 calc R . . H7C H -0.0097 -0.0868 0.3824 0.062 Uiso 1 1 calc R . . C8 C -0.1062(12) -0.0813(7) 0.2149(7) 0.035(3) Uani 1 1 d . . . H8A H -0.0840 -0.0823 0.1662 0.052 Uiso 1 1 calc R . . H8B H -0.2035 -0.0955 0.2095 0.052 Uiso 1 1 calc R . . H8C H -0.0463 -0.1169 0.2481 0.052 Uiso 1 1 calc R . . C9 C -0.1862(12) 0.0728(8) 0.1213(7) 0.045(3) Uani 1 1 d . . . H9A H -0.1792 0.1245 0.1041 0.067 Uiso 1 1 calc R . . H9B H -0.2841 0.0592 0.1146 0.067 Uiso 1 1 calc R . . H9C H -0.1423 0.0382 0.0927 0.067 Uiso 1 1 calc R . . C10 C -0.1422(13) 0.2122(5) 0.2393(8) 0.047(4) Uani 1 1 d . . . H10A H -0.1305 0.2247 0.1897 0.070 Uiso 1 1 calc R . . H10B H -0.0868 0.2469 0.2757 0.070 Uiso 1 1 calc R . . H10C H -0.2402 0.2169 0.2400 0.070 Uiso 1 1 calc R . . C11 C 0.3439(14) 0.0259(6) 0.4091(7) 0.031(3) Uani 1 1 d . . . C12 C 0.3157(12) -0.0424(6) 0.3693(7) 0.025(3) Uani 1 1 d . . . C13 C 0.3878(13) -0.0440(6) 0.3090(7) 0.029(3) Uani 1 1 d . . . C14 C 0.4637(13) 0.0248(7) 0.3145(9) 0.040(4) Uani 1 1 d . . . C15 C 0.4392(11) 0.0697(7) 0.3748(7) 0.032(3) Uani 1 1 d . . . C16 C 0.3070(13) 0.0484(6) 0.4801(7) 0.036(3) Uani 1 1 d . . . H16A H 0.2534 0.0954 0.4723 0.055 Uiso 1 1 calc R . . H16B H 0.3921 0.0560 0.5188 0.055 Uiso 1 1 calc R . . H16C H 0.2514 0.0085 0.4954 0.055 Uiso 1 1 calc R . . C17 C 0.2497(13) -0.1175(5) 0.3955(7) 0.035(3) Uani 1 1 d . . . H17A H 0.3236 -0.1541 0.4146 0.052 Uiso 1 1 calc R . . H17B H 0.1829 -0.1395 0.3532 0.052 Uiso 1 1 calc R . . H17C H 0.2025 -0.1048 0.4346 0.052 Uiso 1 1 calc R . . C18 C 0.4059(14) -0.1146(5) 0.2630(7) 0.037(4) Uani 1 1 d . . . H18A H 0.3147 -0.1363 0.2408 0.055 Uiso 1 1 calc R . . H18B H 0.4628 -0.1520 0.2955 0.055 Uiso 1 1 calc R . . H18C H 0.4517 -0.1002 0.2238 0.055 Uiso 1 1 calc R . . C19 C 0.5657(13) 0.0477(6) 0.2634(7) 0.041(4) Uani 1 1 d . . . H19A H 0.6494 0.0710 0.2939 0.062 Uiso 1 1 calc R . . H19B H 0.5189 0.0835 0.2255 0.062 Uiso 1 1 calc R . . H19C H 0.5913 0.0025 0.2393 0.062 Uiso 1 1 calc R . . C20 C 0.5209(13) 0.1397(6) 0.4087(8) 0.043(4) Uani 1 1 d . . . H20A H 0.4879 0.1565 0.4517 0.064 Uiso 1 1 calc R . . H20B H 0.5072 0.1802 0.3717 0.064 Uiso 1 1 calc R . . H20C H 0.6197 0.1273 0.4242 0.064 Uiso 1 1 calc R . . C21 C 0.2600(14) -0.0442(6) 0.0944(7) 0.027(3) Uani 1 1 d . . . C22 C 0.2151(12) -0.1203(6) 0.0785(6) 0.026(3) Uani 1 1 d . . . H22 H 0.1244 -0.1358 0.0802 0.032 Uiso 1 1 calc R . . C23 C 0.3133(14) -0.1728(6) 0.0597(7) 0.038(4) Uani 1 1 d . . . H23 H 0.2873 -0.2239 0.0495 0.046 Uiso 1 1 calc R . . C24 C 0.4442(13) -0.1494(7) 0.0563(8) 0.038(4) Uani 1 1 d . . . H24 H 0.5066 -0.1847 0.0436 0.046 Uiso 1 1 calc R . . C25 C 0.4861(13) -0.0758(7) 0.0709(7) 0.036(3) Uani 1 1 d . . . H25 H 0.5767 -0.0611 0.0681 0.043 Uiso 1 1 calc R . . C26 C 0.3947(12) -0.0212(6) 0.0905(7) 0.025(3) Uani 1 1 d . . . H26 H 0.4239 0.0295 0.1007 0.029 Uiso 1 1 calc R . . C27 C 0.2144(12) 0.1681(6) 0.0978(8) 0.026(3) Uani 1 1 d . . . C28 C 0.3626(15) 0.2067(6) 0.1292(8) 0.050(5) Uani 1 1 d . . . H28A H 0.3732 0.2494 0.0977 0.076 Uiso 1 1 calc R . . H28B H 0.4361 0.1697 0.1293 0.076 Uiso 1 1 calc R . . H28C H 0.3692 0.2244 0.1799 0.076 Uiso 1 1 calc R . . C29 C 0.1954(14) 0.1416(7) 0.0163(8) 0.042(4) Uani 1 1 d . . . H29A H 0.1929 0.1856 -0.0159 0.062 Uiso 1 1 calc R . . H29B H 0.1082 0.1135 0.0009 0.062 Uiso 1 1 calc R . . H29C H 0.2730 0.1089 0.0126 0.062 Uiso 1 1 calc R . . C30 C 0.0964(13) 0.2284(6) 0.1005(8) 0.039(4) Uani 1 1 d . . . H30A H 0.1065 0.2720 0.0698 0.059 Uiso 1 1 calc R . . H30B H 0.1051 0.2448 0.1518 0.059 Uiso 1 1 calc R . . H30C H 0.0050 0.2054 0.0816 0.059 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 Br1 0.0422(10) 0.0280(7) 0.0498(11) -0.0039(7) 0.0006(8) -0.0002(5) U1 0.0211(3) 0.0237(2) 0.0228(3) 0.0002(3) 0.00307(18) 0.0008(2) S1 0.031(2) 0.0279(16) 0.026(2) -0.0011(16) 0.0093(17) -0.0038(13) N1 0.008(6) 0.020(5) 0.030(6) 0.003(5) -0.005(5) 0.003(3) C1 0.017(9) 0.036(7) 0.054(10) 0.021(7) 0.021(7) 0.016(5) C2 0.004(7) 0.022(6) 0.041(9) -0.013(6) 0.004(6) -0.002(4) C3 0.045(10) 0.026(7) 0.010(8) 0.003(7) 0.010(7) 0.008(6) C4 0.019(8) 0.044(7) 0.028(8) -0.005(8) 0.002(6) 0.003(6) C5 0.009(6) 0.017(5) 0.021(6) -0.001(5) -0.009(5) 0.003(4) C6 0.050(11) 0.065(9) 0.011(8) -0.017(7) 0.014(7) -0.008(7) C7 0.029(10) 0.057(8) 0.044(10) 0.019(8) 0.023(8) 0.005(6) C8 0.028(8) 0.049(8) 0.025(8) 0.001(7) 0.002(6) -0.008(6) C9 0.011(8) 0.085(9) 0.032(8) 0.011(9) -0.008(6) -0.009(7) C10 0.059(12) 0.022(6) 0.054(11) 0.022(8) 0.005(9) 0.024(6) C11 0.055(10) 0.018(6) 0.023(8) 0.000(6) 0.016(7) 0.002(6) C12 0.022(8) 0.032(7) 0.018(8) 0.003(6) -0.003(6) 0.005(5) C13 0.029(9) 0.032(7) 0.016(8) -0.013(6) -0.011(6) 0.003(5) C14 0.004(9) 0.047(8) 0.071(12) 0.008(8) 0.013(8) -0.006(6) C15 0.019(8) 0.039(6) 0.031(8) -0.009(8) -0.004(6) 0.006(6) C16 0.038(10) 0.045(8) 0.021(8) -0.010(7) -0.003(6) -0.002(6) C17 0.043(10) 0.017(6) 0.035(9) -0.004(6) -0.007(7) 0.003(5) C18 0.043(10) 0.029(7) 0.036(9) 0.000(7) 0.003(7) 0.005(5) C19 0.048(10) 0.052(9) 0.019(8) -0.002(7) -0.001(7) -0.007(6) C20 0.043(10) 0.031(7) 0.048(11) -0.003(7) -0.002(8) -0.008(6) C21 0.047(10) 0.024(7) 0.008(7) -0.005(6) 0.003(7) -0.004(5) C22 0.024(9) 0.045(8) 0.008(7) 0.002(6) -0.003(6) 0.000(5) C23 0.045(11) 0.031(7) 0.040(10) 0.008(7) 0.012(8) 0.013(6) C24 0.018(9) 0.051(8) 0.040(10) -0.009(7) -0.003(7) 0.007(6) C25 0.045(9) 0.036(7) 0.025(8) 0.003(8) 0.006(6) 0.002(7) C26 0.020(8) 0.037(7) 0.017(8) -0.009(6) 0.005(6) -0.006(5) C27 0.010(8) 0.041(7) 0.029(9) 0.004(7) 0.009(6) 0.003(5) C28 0.082(13) 0.027(7) 0.056(12) 0.029(8) 0.044(10) 0.019(7) C29 0.031(10) 0.055(8) 0.042(10) 0.015(8) 0.015(8) 0.014(6) C30 0.058(11) 0.018(6) 0.046(10) 0.006(7) 0.021(8) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 U1 2.793(3) . ? U1 N1 2.309(9) . ? U1 C3 2.764(13) . ? U1 C11 2.779(13) . ? U1 C12 2.787(11) . ? U1 C4 2.796(12) . ? U1 C15 2.801(11) . ? U1 C5 2.799(10) . ? U1 C1 2.804(11) . ? U1 C13 2.814(11) . ? U1 C2 2.817(11) . ? U1 C14 2.819(13) . ? S1 N1 1.696(8) . ? S1 C21 1.795(12) . ? N1 C27 1.494(13) . ? C1 C5 1.403(16) . ? C1 C2 1.444(13) . ? C1 C6 1.548(16) . ? C2 C3 1.424(16) . ? C2 C7 1.504(15) . ? C3 C4 1.438(16) . ? C3 C8 1.490(15) . ? C4 C9 1.493(16) . ? C4 C5 1.475(15) . ? C5 C10 1.517(13) . ? C11 C12 1.383(14) . ? C11 C15 1.450(15) . ? C11 C16 1.474(15) . ? C12 C13 1.437(15) . ? C12 C17 1.577(13) . ? C13 C14 1.395(14) . ? C13 C18 1.518(13) . ? C14 C15 1.412(16) . ? C14 C19 1.565(15) . ? C15 C20 1.503(15) . ? C21 C26 1.387(15) . ? C21 C22 1.401(13) . ? C22 C23 1.421(14) . ? C23 C24 1.351(15) . ? C24 C25 1.350(15) . ? C25 C26 1.402(14) . ? C27 C29 1.521(16) . ? C27 C28 1.569(16) . ? C27 C30 1.563(14) . ? 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 C3 106.6(3) . . ? N1 U1 C11 138.8(3) . . ? C3 U1 C11 108.8(4) . . ? N1 U1 C12 130.0(3) . . ? C3 U1 C12 93.5(3) . . ? C11 U1 C12 28.8(3) . . ? N1 U1 C4 86.2(3) . . ? C3 U1 C4 30.0(3) . . ? C11 U1 C4 134.3(4) . . ? C12 U1 C4 123.4(4) . . ? N1 U1 Br1 88.37(19) . . ? C3 U1 Br1 124.8(2) . . ? C11 U1 Br1 88.4(2) . . ? C12 U1 Br1 116.9(2) . . ? C4 U1 Br1 103.6(3) . . ? N1 U1 C15 110.6(3) . . ? C3 U1 C15 138.6(4) . . ? C11 U1 C15 30.1(3) . . ? C12 U1 C15 48.1(3) . . ? C4 U1 C15 162.9(3) . . ? Br1 U1 C15 74.3(3) . . ? N1 U1 C5 99.1(3) . . ? C3 U1 C5 49.2(3) . . ? C11 U1 C5 119.9(4) . . ? C12 U1 C5 127.3(3) . . ? C4 U1 C5 30.6(3) . . ? Br1 U1 C5 76.4(2) . . ? C15 U1 C5 137.1(3) . . ? N1 U1 C1 128.1(3) . . ? C3 U1 C1 48.6(4) . . ? C11 U1 C1 91.6(4) . . ? C12 U1 C1 99.6(3) . . ? C4 U1 C1 49.2(4) . . ? Br1 U1 C1 80.1(2) . . ? C15 U1 C1 114.3(4) . . ? C5 U1 C1 29.0(3) . . ? N1 U1 C13 100.3(3) . . ? C3 U1 C13 107.7(3) . . ? C11 U1 C13 48.8(3) . . ? C12 U1 C13 29.7(3) . . ? C4 U1 C13 134.2(4) . . ? Br1 U1 C13 121.7(2) . . ? C15 U1 C13 48.4(3) . . ? C5 U1 C13 153.6(3) . . ? C1 U1 C13 128.7(3) . . ? N1 U1 C2 134.7(3) . . ? C3 U1 C2 29.5(3) . . ? C11 U1 C2 84.8(4) . . ? C12 U1 C2 79.8(3) . . ? C4 U1 C2 49.6(4) . . ? Br1 U1 C2 108.8(2) . . ? C15 U1 C2 114.4(4) . . ? C5 U1 C2 49.0(3) . . ? C1 U1 C2 29.8(3) . . ? C13 U1 C2 104.7(3) . . ? N1 U1 C14 91.0(4) . . ? C3 U1 C14 136.2(3) . . ? C11 U1 C14 48.4(4) . . ? C12 U1 C14 47.6(3) . . ? C4 U1 C14 161.4(4) . . ? Br1 U1 C14 94.7(3) . . ? C15 U1 C14 29.1(3) . . ? C5 U1 C14 166.2(4) . . ? C1 U1 C14 139.9(4) . . ? C13 U1 C14 28.7(3) . . ? C2 U1 C14 127.2(4) . . ? N1 S1 C21 110.2(5) . . ? N1 S1 U1 54.4(3) . . ? C21 S1 U1 116.9(4) . . ? C27 N1 S1 120.1(8) . . ? C27 N1 U1 146.2(7) . . ? S1 N1 U1 89.0(4) . . ? C5 C1 C2 109.9(12) . . ? C5 C1 C6 123.5(9) . . ? C2 C1 C6 126.0(12) . . ? C5 C1 U1 75.3(6) . . ? C2 C1 U1 75.6(6) . . ? C6 C1 U1 122.9(8) . . ? C3 C2 C1 106.1(11) . . ? C3 C2 C7 128.1(10) . . ? C1 C2 C7 123.5(12) . . ? C3 C2 U1 73.2(7) . . ? C1 C2 U1 74.6(6) . . ? C7 C2 U1 130.7(8) . . ? C2 C3 C4 110.5(10) . . ? C2 C3 C8 124.5(10) . . ? C4 C3 C8 124.2(11) . . ? C2 C3 U1 77.3(7) . . ? C4 C3 U1 76.2(7) . . ? C8 C3 U1 121.7(7) . . ? C3 C4 C9 126.5(12) . . ? C3 C4 C5 105.4(10) . . ? C9 C4 C5 126.2(12) . . ? C3 C4 U1 73.8(7) . . ? C9 C4 U1 128.4(8) . . ? C5 C4 U1 74.9(6) . . ? C1 C5 C4 108.1(9) . . ? C1 C5 C10 126.7(11) . . ? C4 C5 C10 123.6(11) . . ? C1 C5 U1 75.7(6) . . ? C4 C5 U1 74.6(6) . . ? C10 C5 U1 127.2(7) . . ? C12 C11 C15 107.1(10) . . ? C12 C11 C16 128.8(11) . . ? C15 C11 C16 123.4(11) . . ? C12 C11 U1 75.9(7) . . ? C15 C11 U1 75.8(7) . . ? C16 C11 U1 121.3(8) . . ? C11 C12 C13 110.1(10) . . ? C11 C12 C17 126.6(11) . . ? C13 C12 C17 121.5(9) . . ? C11 C12 U1 75.3(7) . . ? C13 C12 U1 76.2(6) . . ? C17 C12 U1 127.5(8) . . ? C14 C13 C12 105.9(10) . . ? C14 C13 C18 127.2(11) . . ? C12 C13 C18 125.3(10) . . ? C14 C13 U1 75.9(7) . . ? C12 C13 U1 74.1(6) . . ? C18 C13 U1 126.8(8) . . ? C13 C14 C15 110.3(11) . . ? C13 C14 C19 125.0(12) . . ? C15 C14 C19 124.7(11) . . ? C13 C14 U1 75.4(7) . . ? C15 C14 U1 74.7(6) . . ? C19 C14 U1 118.5(9) . . ? C14 C15 C11 106.6(10) . . ? C14 C15 C20 126.6(11) . . ? C11 C15 C20 125.4(11) . . ? C14 C15 U1 76.2(7) . . ? C11 C15 U1 74.1(7) . . ? C20 C15 U1 125.9(8) . . ? C26 C21 C22 120.9(11) . . ? C26 C21 S1 124.2(8) . . ? C22 C21 S1 114.9(10) . . ? C21 C22 C23 117.5(12) . . ? C24 C23 C22 120.8(11) . . ? C23 C24 C25 121.3(11) . . ? C24 C25 C26 120.8(12) . . ? C21 C26 C25 118.7(11) . . ? N1 C27 C29 113.0(9) . . ? N1 C27 C28 105.9(10) . . ? C29 C27 C28 111.9(10) . . ? N1 C27 C30 109.0(9) . . ? C29 C27 C30 108.2(11) . . ? C28 C27 C30 108.6(10) . . ? _diffrn_measured_fraction_theta_max 0.771 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.771 _refine_diff_density_max 1.429 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.153