# 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 _publ_contact_author_name 'Jason Love' _publ_contact_author_email JASON.LOVE@ED.AC.UK _publ_section_title ; Equatorial ligand substitution by hydroxide in uranyl Pacman complexes of a Schiff-base pyrrole macrocycle ; loop_ _publ_author_name 'Jason Love' 'Polly L. Arnold' 'Dipti Patel' 'Anne-Frederique Pecharman' 'Claire Wilson' # Attachment 'combined.cif' data_uo2mbz _database_code_depnum_ccdc_archive 'CCDC 752122' #TrackingRef 'combined.cif' _refine_special_details ; Two half-occupied THF solvent molecules per asymmetric unit were refined isotropically using distance and similarity restraints. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H50 N8 O3 U, C4 H8 O' _chemical_formula_sum 'C50 H58 N8 O4 U' _chemical_formula_weight 1073.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 13.3919(7) _cell_length_b 14.7012(8) _cell_length_c 26.5250(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5222.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6562 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 22.3 _exptl_crystal_description Column _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 3.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS version 2.05; Bruker, 2001)' _exptl_special_details ; crystals were grown from the slow diffusion of hexane into a thf solution at rt ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 33639 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.54 _reflns_number_total 11976 _reflns_number_gt 11239 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.044P)^2^+4.411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'methyl H atoms from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.084(6) _refine_ls_number_reflns 11976 _refine_ls_number_parameters 576 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.292978(12) 0.156837(11) 0.699099(6) 0.01874(5) Uani 1 1 d . . . O1 O 0.2281(2) 0.1896(2) 0.64309(12) 0.0200(7) Uani 1 1 d . . . O2 O 0.3527(3) 0.1195(2) 0.75494(13) 0.0245(8) Uani 1 1 d . . . O3 O 0.1929(3) 0.0180(2) 0.70914(13) 0.0302(8) Uani 1 1 d D . . N1 N 0.1622(3) 0.2126(3) 0.76217(16) 0.0255(9) Uani 1 1 d . . . N2 N 0.3173(3) 0.3164(3) 0.72604(16) 0.0211(9) Uani 1 1 d . . . N3 N 0.4553(3) 0.2102(3) 0.66919(15) 0.0187(8) Uani 1 1 d . . . N4 N 0.3996(3) 0.0309(3) 0.65773(16) 0.0224(9) Uani 1 1 d . . . N5 N 0.2724(3) -0.0070(3) 0.57908(16) 0.0264(10) Uani 1 1 d . . . N6 N 0.1772(3) 0.1362(3) 0.53144(16) 0.0238(10) Uani 1 1 d . . . H6 H 0.1882 0.1462 0.5637 0.029 Uiso 1 1 calc R . . N7 N 0.0178(3) 0.2368(3) 0.60209(17) 0.0241(9) Uani 1 1 d . . . H7 H 0.073(5) 0.232(4) 0.620(2) 0.035(18) Uiso 1 1 d . . . N8 N 0.0057(3) 0.1724(3) 0.70153(17) 0.0258(9) Uani 1 1 d . . . C1 C 0.1840(4) 0.2885(4) 0.78522(18) 0.0234(11) Uani 1 1 d . . . H1B H 0.1471 0.3063 0.8142 0.028 Uiso 1 1 calc R . . C2 C 0.2620(3) 0.3439(4) 0.76724(17) 0.0220(9) Uani 1 1 d . . . C3 C 0.2934(4) 0.4299(3) 0.78290(18) 0.0262(10) Uani 1 1 d . . . H3A H 0.2682 0.4638 0.8106 0.031 Uiso 1 1 calc R . . C4 C 0.3684(4) 0.4560(3) 0.75010(19) 0.0241(11) Uani 1 1 d . . . H4A H 0.4040 0.5119 0.7506 0.029 Uiso 1 1 calc R . . C5 C 0.3818(4) 0.3846(3) 0.71608(18) 0.0204(10) Uani 1 1 d . . . C6 C 0.4531(4) 0.3793(3) 0.67155(18) 0.0194(10) Uani 1 1 d . . . C7 C 0.3911(4) 0.3870(4) 0.6224(2) 0.0275(12) Uani 1 1 d . . . H7B H 0.3420 0.3377 0.6212 0.041 Uiso 1 1 calc R . . H7C H 0.4358 0.3825 0.5932 0.041 Uiso 1 1 calc R . . H7D H 0.3565 0.4457 0.6217 0.041 Uiso 1 1 calc R . . C8 C 0.5277(4) 0.4576(4) 0.6733(2) 0.0293(12) Uani 1 1 d . . . H8B H 0.5636 0.4563 0.7054 0.044 Uiso 1 1 calc R . . H8C H 0.4920 0.5155 0.6700 0.044 Uiso 1 1 calc R . . H8D H 0.5754 0.4512 0.6455 0.044 Uiso 1 1 calc R . . C9 C 0.5068(4) 0.2892(3) 0.67194(17) 0.0175(10) Uani 1 1 d . . . C10 C 0.6100(4) 0.2718(3) 0.67142(19) 0.0231(10) Uani 1 1 d . . . H10A H 0.6618 0.3159 0.6735 0.028 Uiso 1 1 calc R . . C11 C 0.6223(4) 0.1786(3) 0.66733(19) 0.0259(11) Uani 1 1 d . . . H11A H 0.6837 0.1464 0.6658 0.031 Uiso 1 1 calc R . . C12 C 0.5264(4) 0.1413(3) 0.66586(18) 0.0208(10) Uani 1 1 d . . . C13 C 0.4940(4) 0.0511(3) 0.65806(18) 0.0218(11) Uani 1 1 d . . . H13A H 0.5420 0.0043 0.6530 0.026 Uiso 1 1 calc R . . C14 C 0.3750(4) -0.0611(3) 0.6467(2) 0.0253(11) Uani 1 1 d . . . C15 C 0.4142(4) -0.1327(3) 0.6755(2) 0.0281(12) Uani 1 1 d . . . H15A H 0.4576 -0.1191 0.7028 0.034 Uiso 1 1 calc R . . C16 C 0.3914(5) -0.2230(4) 0.6651(2) 0.0325(13) Uani 1 1 d . . . C16A C 0.4354(6) -0.2961(4) 0.6975(3) 0.0496(17) Uani 1 1 d . . . H16A H 0.4792 -0.2685 0.7228 0.074 Uiso 1 1 calc R . . H16B H 0.4742 -0.3380 0.6765 0.074 Uiso 1 1 calc R . . H16C H 0.3817 -0.3295 0.7144 0.074 Uiso 1 1 calc R . . C17 C 0.3294(5) -0.2417(4) 0.6235(2) 0.0332(13) Uani 1 1 d . . . C17A C 0.3029(6) -0.3402(4) 0.6114(3) 0.0546(18) Uani 1 1 d . . . H17A H 0.2542 -0.3417 0.5838 0.082 Uiso 1 1 calc R . . H17B H 0.2740 -0.3692 0.6413 0.082 Uiso 1 1 calc R . . H17C H 0.3633 -0.3731 0.6012 0.082 Uiso 1 1 calc R . . C18 C 0.2927(5) -0.1719(3) 0.5953(2) 0.0348(12) Uani 1 1 d . . . H18A H 0.2509 -0.1857 0.5674 0.042 Uiso 1 1 calc R . . C19 C 0.3143(4) -0.0812(3) 0.6057(2) 0.0258(12) Uani 1 1 d . . . C20 C 0.2574(4) -0.0126(4) 0.5318(2) 0.0286(12) Uani 1 1 d . . . H20A H 0.2795 -0.0645 0.5136 0.034 Uiso 1 1 calc R . . C21 C 0.2070(5) 0.0600(3) 0.50627(18) 0.0269(10) Uani 1 1 d . . . C22 C 0.1771(4) 0.0701(4) 0.4570(2) 0.0313(13) Uani 1 1 d . . . H22A H 0.1885 0.0281 0.4304 0.038 Uiso 1 1 calc R . . C23 C 0.1273(4) 0.1524(4) 0.45296(17) 0.0274(10) Uani 1 1 d . . . H23A H 0.0978 0.1756 0.4230 0.033 Uiso 1 1 calc R . . C24 C 0.1273(4) 0.1957(4) 0.49973(19) 0.0245(10) Uani 1 1 d . . . C25 C 0.0850(4) 0.2839(4) 0.5169(2) 0.0285(12) Uani 1 1 d . . . C26 C 0.1684(4) 0.3416(4) 0.5403(2) 0.0322(11) Uani 1 1 d . . . H26A H 0.1970 0.3093 0.5693 0.048 Uiso 1 1 calc R . . H26B H 0.1409 0.4000 0.5516 0.048 Uiso 1 1 calc R . . H26C H 0.2207 0.3524 0.5152 0.048 Uiso 1 1 calc R . . C27 C 0.0438(5) 0.3368(5) 0.4715(2) 0.0369(13) Uani 1 1 d . . . H27A H -0.0069 0.2999 0.4544 0.055 Uiso 1 1 calc R . . H27B H 0.0982 0.3503 0.4480 0.055 Uiso 1 1 calc R . . H27C H 0.0136 0.3938 0.4832 0.055 Uiso 1 1 calc R . . C28 C 0.0012(4) 0.2679(4) 0.5543(2) 0.0267(11) Uani 1 1 d . . . C29 C -0.1009(4) 0.2764(4) 0.5484(2) 0.0336(13) Uani 1 1 d . . . H29A H -0.1346 0.2966 0.5189 0.040 Uiso 1 1 calc R . . C30 C -0.1460(4) 0.2499(4) 0.5940(2) 0.0311(12) Uani 1 1 d . . . H30A H -0.2156 0.2494 0.6008 0.037 Uiso 1 1 calc R . . C31 C -0.0712(4) 0.2245(4) 0.6273(2) 0.0264(11) Uani 1 1 d . . . C32 C -0.0751(4) 0.1919(4) 0.6774(2) 0.0273(12) Uani 1 1 d . . . H32A H -0.1379 0.1842 0.6935 0.033 Uiso 1 1 calc R . . C33 C 0.0035(4) 0.1362(4) 0.75065(19) 0.0246(11) Uani 1 1 d . . . C34 C -0.0682(4) 0.0759(4) 0.7696(2) 0.0291(12) Uani 1 1 d . . . H34A H -0.1237 0.0608 0.7489 0.035 Uiso 1 1 calc R . . C35 C -0.0622(4) 0.0373(4) 0.8170(2) 0.0303(12) Uani 1 1 d . . . C35A C -0.1364(5) -0.0325(4) 0.8338(2) 0.0382(14) Uani 1 1 d . . . H35A H -0.1960 -0.0290 0.8125 0.057 Uiso 1 1 calc R . . H35B H -0.1550 -0.0209 0.8690 0.057 Uiso 1 1 calc R . . H35C H -0.1068 -0.0932 0.8311 0.057 Uiso 1 1 calc R . . C36 C 0.0181(5) 0.0620(4) 0.8481(2) 0.0349(14) Uani 1 1 d . . . C36A C 0.0294(6) 0.0191(6) 0.9000(3) 0.058(2) Uani 1 1 d . . . H36A H 0.0894 0.0433 0.9164 0.088 Uiso 1 1 calc R . . H36B H 0.0356 -0.0470 0.8964 0.088 Uiso 1 1 calc R . . H36C H -0.0294 0.0334 0.9205 0.088 Uiso 1 1 calc R . . C37 C 0.0903(4) 0.1220(4) 0.8301(2) 0.0369(14) Uani 1 1 d . . . H37A H 0.1442 0.1390 0.8514 0.044 Uiso 1 1 calc R . . C38 C 0.0850(3) 0.1572(4) 0.78179(18) 0.0251(10) Uani 1 1 d . . . C39 C 0.2112(5) -0.0451(4) 0.7504(2) 0.0432(14) Uani 1 1 d D . . H39A H 0.2037 -0.0136 0.7831 0.052 Uiso 1 1 calc R . . H39B H 0.2798 -0.0698 0.7481 0.052 Uiso 1 1 calc R . . C40 C 0.1380(7) -0.1185(6) 0.7460(4) 0.083(3) Uani 1 1 d D . . H40A H 0.1693 -0.1780 0.7536 0.100 Uiso 1 1 calc R . . H40B H 0.0818 -0.1088 0.7696 0.100 Uiso 1 1 calc R . . C41 C 0.1031(8) -0.1160(5) 0.6943(3) 0.087(3) Uani 1 1 d D . . H41A H 0.0320 -0.1341 0.6924 0.105 Uiso 1 1 calc R . . H41B H 0.1428 -0.1579 0.6730 0.105 Uiso 1 1 calc R . . C42 C 0.1160(4) -0.0214(4) 0.6773(2) 0.0356(13) Uani 1 1 d D . . H42A H 0.1367 -0.0198 0.6415 0.043 Uiso 1 1 calc R . . H42B H 0.0527 0.0127 0.6809 0.043 Uiso 1 1 calc R . . O4 O 0.6764(12) -0.2527(11) 0.5191(6) 0.107(5) Uiso 0.50 1 d PD . . C43 C 0.7095(19) -0.2825(17) 0.5680(7) 0.117(8) Uiso 0.50 1 d PD . . H43A H 0.7781 -0.2626 0.5766 0.140 Uiso 0.50 1 calc PR . . H43B H 0.7016 -0.3487 0.5736 0.140 Uiso 0.50 1 calc PR . . C44 C 0.632(2) -0.2280(16) 0.5915(10) 0.124(9) Uiso 0.50 1 d PD . . H44A H 0.6562 -0.2100 0.6253 0.149 Uiso 0.50 1 calc PR . . H44B H 0.5732 -0.2679 0.5967 0.149 Uiso 0.50 1 calc PR . . C45 C 0.5970(18) -0.1459(15) 0.5662(7) 0.101(7) Uiso 0.50 1 d PD . . H45A H 0.5258 -0.1332 0.5734 0.121 Uiso 0.50 1 calc PR . . H45B H 0.6379 -0.0921 0.5750 0.121 Uiso 0.50 1 calc PR . . C46 C 0.6129(18) -0.1753(14) 0.5146(8) 0.118(8) Uiso 0.50 1 d PD . . H46A H 0.5488 -0.1918 0.4983 0.142 Uiso 0.50 1 calc PR . . H46B H 0.6454 -0.1268 0.4945 0.142 Uiso 0.50 1 calc PR . . O5 O -0.0913(7) -0.0976(6) 0.6034(4) 0.054(2) Uiso 0.50 1 d PD . . C47 C -0.0282(12) -0.1395(11) 0.5667(5) 0.069(5) Uiso 0.50 1 d PD . . H47A H -0.0484 -0.2033 0.5606 0.083 Uiso 0.50 1 calc PR . . H47B H 0.0424 -0.1384 0.5776 0.083 Uiso 0.50 1 calc PR . . C48 C -0.0426(19) -0.0841(11) 0.5215(7) 0.096(7) Uiso 0.50 1 d PD . . H48A H 0.0194 -0.0810 0.5012 0.115 Uiso 0.50 1 calc PR . . H48B H -0.0971 -0.1088 0.5003 0.115 Uiso 0.50 1 calc PR . . C49 C -0.0689(16) 0.0048(12) 0.5416(6) 0.090(6) Uiso 0.50 1 d PD . . H49A H -0.1143 0.0365 0.5180 0.109 Uiso 0.50 1 calc PR . . H49B H -0.0080 0.0422 0.5456 0.109 Uiso 0.50 1 calc PR . . C50 C -0.1180(11) -0.0069(7) 0.5905(5) 0.051(3) Uiso 0.50 1 d PD . . H50A H -0.0924 0.0371 0.6156 0.061 Uiso 0.50 1 calc PR . . H50B H -0.1913 0.0000 0.5875 0.061 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 U1 0.01732(8) 0.01713(8) 0.02176(8) 0.00073(7) -0.00160(8) -0.00213(7) O1 0.0155(18) 0.0229(16) 0.0215(16) 0.0008(13) -0.0015(13) -0.0008(13) O2 0.0228(19) 0.0267(18) 0.0241(18) 0.0044(15) -0.0064(15) -0.0035(15) O3 0.029(2) 0.0238(17) 0.038(2) 0.0064(15) 0.0001(17) -0.0033(15) N1 0.020(2) 0.031(2) 0.025(2) 0.0024(19) 0.0021(17) -0.0057(18) N2 0.020(2) 0.017(2) 0.026(2) 0.0007(16) -0.0022(16) -0.0002(15) N3 0.023(2) 0.016(2) 0.017(2) 0.0009(16) 0.0007(16) -0.0020(16) N4 0.026(2) 0.0152(19) 0.027(2) 0.0001(17) -0.0065(18) 0.0004(17) N5 0.030(3) 0.021(2) 0.028(2) -0.0010(17) -0.0063(19) 0.0020(18) N6 0.023(2) 0.029(2) 0.020(2) 0.0032(17) -0.0041(16) 0.0033(16) N7 0.019(2) 0.031(2) 0.023(2) 0.0033(19) -0.0012(18) 0.0043(17) N8 0.0168(19) 0.033(2) 0.028(2) -0.003(2) 0.0022(18) -0.0066(16) C1 0.017(3) 0.035(3) 0.018(2) 0.001(2) 0.0029(17) 0.002(2) C2 0.020(2) 0.024(2) 0.023(2) -0.002(2) 0.0014(17) 0.000(2) C3 0.030(3) 0.023(2) 0.025(2) -0.0064(19) 0.001(2) 0.005(2) C4 0.027(3) 0.020(2) 0.025(3) -0.001(2) -0.001(2) -0.003(2) C5 0.020(2) 0.016(2) 0.025(2) 0.0017(18) -0.003(2) -0.0025(19) C6 0.020(2) 0.016(2) 0.023(2) -0.0001(19) 0.003(2) -0.0022(18) C7 0.026(3) 0.023(3) 0.034(3) 0.005(2) 0.001(2) 0.005(2) C8 0.028(3) 0.021(3) 0.040(3) 0.002(2) 0.008(2) -0.002(2) C9 0.017(2) 0.020(2) 0.016(2) 0.0005(19) 0.0006(18) -0.0009(18) C10 0.022(3) 0.021(2) 0.026(3) 0.001(2) 0.001(2) -0.002(2) C11 0.018(2) 0.028(3) 0.031(3) 0.003(2) 0.002(2) 0.005(2) C12 0.022(2) 0.022(3) 0.018(2) 0.0006(19) -0.0026(18) 0.003(2) C13 0.028(3) 0.019(3) 0.018(2) -0.0018(19) -0.002(2) 0.006(2) C14 0.026(3) 0.019(2) 0.031(3) -0.005(2) 0.003(2) 0.003(2) C15 0.038(3) 0.020(3) 0.026(3) -0.001(2) -0.004(2) 0.004(2) C16 0.047(4) 0.023(3) 0.028(3) -0.003(2) -0.004(3) 0.003(3) C16A 0.085(5) 0.023(3) 0.041(3) 0.002(3) -0.009(4) 0.014(3) C17 0.046(4) 0.021(3) 0.033(3) -0.005(2) -0.001(3) 0.001(2) C17A 0.087(5) 0.021(3) 0.056(4) 0.000(3) -0.017(4) -0.012(4) C18 0.046(3) 0.023(3) 0.035(3) -0.007(2) -0.013(3) -0.002(3) C19 0.029(3) 0.018(2) 0.030(3) -0.002(2) -0.003(2) 0.001(2) C20 0.029(3) 0.027(3) 0.030(3) -0.003(2) -0.001(2) 0.001(2) C21 0.026(3) 0.031(3) 0.024(2) 0.000(2) -0.003(3) -0.003(3) C22 0.038(3) 0.029(3) 0.027(3) -0.003(2) 0.000(2) 0.001(2) C23 0.026(3) 0.038(3) 0.018(2) 0.003(2) -0.0018(19) -0.006(3) C24 0.016(2) 0.037(3) 0.021(2) 0.003(2) -0.003(2) -0.001(2) C25 0.024(3) 0.032(3) 0.030(3) 0.006(2) -0.002(2) 0.003(2) C26 0.034(3) 0.027(3) 0.036(3) 0.002(3) 0.005(2) -0.001(3) C27 0.039(3) 0.040(3) 0.032(3) 0.012(3) -0.002(2) 0.008(3) C28 0.029(3) 0.029(3) 0.022(3) 0.001(2) -0.003(2) 0.004(2) C29 0.024(3) 0.043(3) 0.034(3) -0.003(3) -0.006(2) 0.002(2) C30 0.019(3) 0.043(3) 0.031(3) 0.003(3) 0.002(2) 0.006(2) C31 0.019(3) 0.030(3) 0.030(3) 0.001(2) 0.001(2) -0.001(2) C32 0.024(3) 0.027(3) 0.031(3) 0.000(2) 0.002(2) 0.002(2) C33 0.016(2) 0.033(3) 0.025(2) -0.001(2) 0.0081(19) -0.002(2) C34 0.022(3) 0.033(3) 0.032(3) -0.002(2) -0.003(2) -0.005(2) C35 0.020(3) 0.039(3) 0.032(3) 0.001(2) 0.001(2) -0.005(2) C35A 0.029(3) 0.044(3) 0.042(3) 0.010(3) 0.002(3) -0.012(3) C36 0.035(3) 0.042(3) 0.027(3) 0.008(3) -0.002(2) -0.010(3) C36A 0.053(4) 0.082(5) 0.040(4) 0.024(4) -0.017(3) -0.025(4) C37 0.026(3) 0.051(4) 0.033(3) 0.008(3) -0.001(2) -0.008(3) C38 0.018(2) 0.031(3) 0.027(2) -0.001(2) 0.0048(18) -0.002(2) C39 0.049(4) 0.029(3) 0.052(4) 0.021(3) 0.001(4) -0.002(3) C40 0.064(6) 0.058(5) 0.128(9) 0.044(6) -0.021(6) -0.025(4) C41 0.110(8) 0.057(5) 0.095(7) -0.016(5) 0.011(7) -0.060(5) C42 0.022(3) 0.038(3) 0.047(3) -0.014(3) -0.005(3) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.787(3) . ? U1 O2 1.770(3) . ? U1 O3 2.457(3) . ? U1 N1 2.557(4) . ? U1 N2 2.473(4) . ? U1 N3 2.443(4) . ? U1 N4 2.583(4) . ? O3 C42 1.452(5) . ? O3 C39 1.454(5) . ? N1 C1 1.305(7) . ? N1 C38 1.415(6) . ? N2 C5 1.350(6) . ? N2 C2 1.381(6) . ? N3 C9 1.353(6) . ? N3 C12 1.394(6) . ? N4 C13 1.298(7) . ? N4 C14 1.422(6) . ? N5 C20 1.272(7) . ? N5 C19 1.416(6) . ? N6 C21 1.363(6) . ? N6 C24 1.385(6) . ? N7 C28 1.365(7) . ? N7 C31 1.378(7) . ? N8 C32 1.289(7) . ? N8 C33 1.408(7) . ? C1 C2 1.408(7) . ? C2 C3 1.396(7) . ? C3 C4 1.383(7) . ? C4 C5 1.396(7) . ? C5 C6 1.521(7) . ? C6 C9 1.507(7) . ? C6 C8 1.525(7) . ? C6 C7 1.550(7) . ? C9 C10 1.405(7) . ? C10 C11 1.384(7) . ? C11 C12 1.398(7) . ? C12 C13 1.411(7) . ? C14 C19 1.388(7) . ? C14 C15 1.403(7) . ? C15 C16 1.391(8) . ? C16 C17 1.407(8) . ? C16 C16A 1.497(8) . ? C17 C18 1.362(8) . ? C17 C17A 1.526(8) . ? C18 C19 1.392(7) . ? C20 C21 1.434(7) . ? C21 C22 1.375(7) . ? C22 C23 1.384(8) . ? C23 C24 1.394(7) . ? C24 C25 1.487(7) . ? C25 C28 1.516(8) . ? C25 C26 1.534(8) . ? C25 C27 1.536(7) . ? C28 C29 1.383(8) . ? C29 C30 1.407(8) . ? C30 C31 1.385(8) . ? C31 C32 1.416(8) . ? C33 C34 1.400(7) . ? C33 C38 1.403(7) . ? C34 C35 1.381(8) . ? C35 C36 1.402(8) . ? C35 C35A 1.497(8) . ? C36 C37 1.392(8) . ? C36 C36A 1.522(8) . ? C37 C38 1.384(8) . ? C39 C40 1.464(7) . ? C40 C41 1.450(7) . ? C41 C42 1.471(7) . ? O4 C46 1.426(9) . ? O4 C43 1.440(9) . ? C43 C44 1.453(9) . ? C44 C45 1.457(9) . ? C45 C46 1.453(9) . ? O5 C50 1.422(8) . ? O5 C47 1.429(8) . ? C47 C48 1.461(9) . ? C48 C49 1.455(9) . ? C49 C50 1.464(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 176.97(16) . . ? O1 U1 O3 92.82(13) . . ? O1 U1 N1 97.17(15) . . ? O1 U1 N2 92.77(14) . . ? O1 U1 N3 94.34(14) . . ? O1 U1 N4 96.25(14) . . ? O2 U1 O3 84.16(14) . . ? O2 U1 N1 82.03(16) . . ? O2 U1 N2 89.58(15) . . ? O2 U1 N3 88.24(15) . . ? O2 U1 N4 83.30(15) . . ? O3 U1 N1 79.72(13) . . ? O3 U1 N2 145.94(13) . . ? O3 U1 N3 141.96(13) . . ? O3 U1 N4 75.64(13) . . ? N1 U1 N2 66.25(14) . . ? N1 U1 N3 135.96(14) . . ? N1 U1 N4 152.42(14) . . ? N2 U1 N3 70.86(13) . . ? N2 U1 N4 136.86(13) . . ? N3 U1 N4 66.46(13) . . ? C42 O3 C39 107.6(4) . . ? C42 O3 U1 131.0(3) . . ? C39 O3 U1 121.3(3) . . ? C1 N1 C38 118.8(4) . . ? C1 N1 U1 115.3(3) . . ? C38 N1 U1 123.9(3) . . ? C5 N2 C2 106.3(4) . . ? C5 N2 U1 137.1(3) . . ? C2 N2 U1 115.9(3) . . ? C9 N3 C12 106.2(4) . . ? C9 N3 U1 135.4(3) . . ? C12 N3 U1 113.2(3) . . ? C13 N4 C14 116.4(4) . . ? C13 N4 U1 111.8(3) . . ? C14 N4 U1 129.8(3) . . ? C20 N5 C19 120.3(5) . . ? C21 N6 C24 111.3(4) . . ? C28 N7 C31 110.7(5) . . ? C32 N8 C33 121.7(4) . . ? N1 C1 C2 120.1(4) . . ? N2 C2 C3 109.8(4) . . ? N2 C2 C1 119.8(5) . . ? C3 C2 C1 130.3(5) . . ? C4 C3 C2 106.4(4) . . ? C3 C4 C5 106.9(4) . . ? N2 C5 C4 110.5(4) . . ? N2 C5 C6 121.0(4) . . ? C4 C5 C6 128.5(4) . . ? C9 C6 C5 109.9(4) . . ? C9 C6 C8 110.5(4) . . ? C5 C6 C8 110.4(4) . . ? C9 C6 C7 109.0(4) . . ? C5 C6 C7 108.3(4) . . ? C8 C6 C7 108.7(4) . . ? N3 C9 C10 110.2(4) . . ? N3 C9 C6 120.6(4) . . ? C10 C9 C6 129.0(4) . . ? C11 C10 C9 107.3(5) . . ? C10 C11 C12 106.4(5) . . ? N3 C12 C11 109.9(4) . . ? N3 C12 C13 118.9(4) . . ? C11 C12 C13 131.0(5) . . ? N4 C13 C12 121.0(5) . . ? C19 C14 C15 119.1(5) . . ? C19 C14 N4 120.0(5) . . ? C15 C14 N4 120.9(5) . . ? C16 C15 C14 121.7(5) . . ? C15 C16 C17 118.2(5) . . ? C15 C16 C16A 119.0(5) . . ? C17 C16 C16A 122.8(5) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 C17A 121.0(5) . . ? C16 C17 C17A 119.2(5) . . ? C17 C18 C19 122.6(5) . . ? C14 C19 C18 118.7(5) . . ? C14 C19 N5 117.3(4) . . ? C18 C19 N5 123.9(5) . . ? N5 C20 C21 119.4(5) . . ? N6 C21 C22 106.9(5) . . ? N6 C21 C20 121.2(4) . . ? C22 C21 C20 131.9(5) . . ? C21 C22 C23 108.0(5) . . ? C22 C23 C24 109.2(5) . . ? N6 C24 C23 104.6(5) . . ? N6 C24 C25 123.3(4) . . ? C23 C24 C25 132.1(5) . . ? C24 C25 C28 110.3(5) . . ? C24 C25 C26 109.2(4) . . ? C28 C25 C26 111.1(5) . . ? C24 C25 C27 109.8(5) . . ? C28 C25 C27 109.0(4) . . ? C26 C25 C27 107.5(5) . . ? N7 C28 C29 107.3(5) . . ? N7 C28 C25 122.6(5) . . ? C29 C28 C25 130.0(5) . . ? C28 C29 C30 107.5(5) . . ? C31 C30 C29 108.2(5) . . ? N7 C31 C30 106.3(5) . . ? N7 C31 C32 122.1(5) . . ? C30 C31 C32 131.6(5) . . ? N8 C32 C31 120.7(5) . . ? C34 C33 C38 117.5(5) . . ? C34 C33 N8 125.9(5) . . ? C38 C33 N8 116.4(4) . . ? C35 C34 C33 123.1(5) . . ? C34 C35 C36 118.2(5) . . ? C34 C35 C35A 120.9(5) . . ? C36 C35 C35A 120.8(5) . . ? C37 C36 C35 119.7(5) . . ? C37 C36 C36A 120.2(6) . . ? C35 C36 C36A 120.0(5) . . ? C38 C37 C36 121.3(6) . . ? C37 C38 C33 120.1(5) . . ? C37 C38 N1 121.2(5) . . ? C33 C38 N1 118.6(4) . . ? O3 C39 C40 107.3(5) . . ? C41 C40 C39 105.8(6) . . ? C40 C41 C42 106.0(6) . . ? O3 C42 C41 106.4(5) . . ? C46 O4 C43 120.2(17) . . ? O4 C43 C44 89.8(17) . . ? C43 C44 C45 119(2) . . ? C46 C45 C44 98.1(19) . . ? O4 C46 C45 104.2(17) . . ? C50 O5 C47 112.8(11) . . ? O5 C47 C48 104.0(13) . . ? C49 C48 C47 103.4(15) . . ? C48 C49 C50 109.1(15) . . ? O5 C50 C49 102.2(11) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.14 _refine_diff_density_min -0.67 _refine_diff_density_rms 0.11 data_po7012 _database_code_depnum_ccdc_archive 'CCDC 752123' #TrackingRef 'combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H73 K N8 O3 U' _chemical_formula_sum 'C72 H73 K N8 O3 U' _chemical_formula_weight 1375.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.864(5) _cell_length_b 15.187(5) _cell_length_c 18.151(5) _cell_angle_alpha 92.186(5) _cell_angle_beta 105.716(5) _cell_angle_gamma 116.998(5) _cell_volume 3219.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17777 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 30 _exptl_crystal_description Irregular _exptl_crystal_colour Orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 1.42 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4586 _exptl_absorpt_correction_T_max 0.4856 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker x8' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 73027 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 30.02 _reflns_number_total 17777 _reflns_number_gt 15880 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (GIACOVAZZO, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP(Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al.,2004)' _refine_special_details ; One molecule of benzene C25s C27s c28s c29s c30s modelled isotropically over two sites with 50:50 occupancy except C26s fully occupied 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^ > 2\s(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^)+(0.0393P)^2^+1.2907P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17777 _refine_ls_number_parameters 731 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.687214(7) 0.604608(6) 0.667291(5) 0.01757(3) Uani 1 1 d . . . K1 K 0.45560(5) 0.34952(4) 0.54747(3) 0.02712(11) Uani 1 1 d . . . O1 O 0.75407(14) 0.65947(12) 0.76914(9) 0.0221(3) Uani 1 1 d . . . O2 O 0.62113(14) 0.55137(12) 0.56469(9) 0.0204(3) Uani 1 1 d . . . O3 O 0.60954(14) 0.44974(12) 0.68651(10) 0.0235(3) Uani 1 1 d . . . H3A H 0.6261 0.4252 0.7317 0.035 Uiso 1 1 calc R . . N1 N 0.83787(17) 0.55713(15) 0.66025(12) 0.0231(4) Uani 1 1 d . . . N2 N 0.84903(16) 0.74255(15) 0.63889(11) 0.0213(4) Uani 1 1 d . . . N3 N 0.63866(17) 0.74047(14) 0.63099(11) 0.0209(4) Uani 1 1 d . . . N4 N 0.48016(16) 0.56301(15) 0.65897(11) 0.0218(4) Uani 1 1 d . . . N5 N 0.51768(18) 0.52638(16) 0.80751(12) 0.0265(4) Uani 1 1 d . . . N6 N 0.71310(18) 0.67181(15) 0.92549(11) 0.0246(4) Uani 1 1 d . . . H6 H 0.7260 0.6669 0.8822 0.030 Uiso 1 1 calc R . . N7 N 0.93698(19) 0.66900(16) 0.92560(12) 0.0278(4) Uani 1 1 d . . . H7 H 0.8829 0.6593 0.8839 0.033 Uiso 1 1 calc R . . N8 N 0.8957(2) 0.52283(17) 0.80906(13) 0.0317(5) Uani 1 1 d . . . C1 C 0.9292(2) 0.62895(19) 0.65148(15) 0.0267(5) Uani 1 1 d . . . H1 H 0.9899 0.6176 0.6523 0.032 Uiso 1 1 calc R . . C2 C 0.9386(2) 0.72348(19) 0.64075(15) 0.0263(5) Uani 1 1 d . . . C3 C 1.0309(2) 0.8091(2) 0.63366(18) 0.0367(6) Uani 1 1 d . . . H3 H 1.1008 0.8156 0.6333 0.044 Uiso 1 1 calc R . . C4 C 0.9981(2) 0.8828(2) 0.62724(17) 0.0343(6) Uani 1 1 d . . . H4 H 1.0419 0.9484 0.6216 0.041 Uiso 1 1 calc R . . C5 C 0.8862(2) 0.83990(18) 0.63076(14) 0.0237(5) Uani 1 1 d . . . C6 C 0.8195(2) 0.89525(17) 0.63443(14) 0.0242(5) Uani 1 1 d . . . C7 C 0.8507(2) 0.9782(2) 0.58583(17) 0.0350(6) Uani 1 1 d . . . H7A H 0.8272 0.9483 0.5321 0.053 Uiso 1 1 calc R . . H7B H 0.9320 1.0219 0.6043 0.053 Uiso 1 1 calc R . . H7C H 0.8126 1.0163 0.5906 0.053 Uiso 1 1 calc R . . C8 C 0.8564(2) 0.9436(2) 0.72075(16) 0.0338(6) Uani 1 1 d . . . H8A H 0.8159 0.9797 0.7253 0.051 Uiso 1 1 calc R . . H8B H 0.9372 0.9893 0.7390 0.051 Uiso 1 1 calc R . . H8C H 0.8390 0.8920 0.7516 0.051 Uiso 1 1 calc R . . C9 C 0.6907(2) 0.82851(17) 0.60686(13) 0.0220(4) Uani 1 1 d . . . C10 C 0.6082(2) 0.85334(19) 0.56362(15) 0.0282(5) Uani 1 1 d . . . H10 H 0.6222 0.9093 0.5401 0.034 Uiso 1 1 calc R . . C11 C 0.5021(2) 0.7781(2) 0.56297(15) 0.0291(5) Uani 1 1 d . . . H11 H 0.4315 0.7743 0.5394 0.035 Uiso 1 1 calc R . . C12 C 0.5224(2) 0.70932(18) 0.60473(14) 0.0229(5) Uani 1 1 d . . . C13 C 0.4445(2) 0.61934(19) 0.62149(14) 0.0241(5) Uani 1 1 d . . . H13 H 0.3670 0.6003 0.6055 0.029 Uiso 1 1 calc R . . C14 C 0.3985(2) 0.47251(18) 0.67339(14) 0.0234(5) Uani 1 1 d . . . C15 C 0.3002(2) 0.4018(2) 0.61467(15) 0.0268(5) Uani 1 1 d . . . H15 H 0.2855 0.4155 0.5646 0.032 Uiso 1 1 calc R . . C16 C 0.2235(2) 0.3114(2) 0.62889(15) 0.0300(5) Uani 1 1 d . . . C16A C 0.1179(3) 0.2373(2) 0.56341(18) 0.0443(7) Uani 1 1 d . . . H16A H 0.1176 0.2633 0.5160 0.066 Uiso 1 1 calc R . . H16B H 0.0509 0.2271 0.5757 0.066 Uiso 1 1 calc R . . H16C H 0.1182 0.1744 0.5569 0.066 Uiso 1 1 calc R . . C17 C 0.2457(2) 0.2903(2) 0.70435(16) 0.0305(5) Uani 1 1 d . . . C17A C 0.1670(3) 0.1924(2) 0.72279(19) 0.0439(7) Uani 1 1 d . . . H17A H 0.2045 0.1843 0.7728 0.066 Uiso 1 1 calc R . . H17B H 0.1480 0.1375 0.6837 0.066 Uiso 1 1 calc R . . H17C H 0.0983 0.1930 0.7235 0.066 Uiso 1 1 calc R . . C18 C 0.3428(2) 0.3617(2) 0.76302(15) 0.0295(5) Uani 1 1 d . . . H18 H 0.3575 0.3479 0.8131 0.035 Uiso 1 1 calc R . . C19 C 0.4187(2) 0.45307(19) 0.74942(14) 0.0251(5) Uani 1 1 d . . . C20 C 0.5099(2) 0.54708(19) 0.87394(15) 0.0270(5) Uani 1 1 d . . . H20 H 0.4394 0.5150 0.8820 0.032 Uiso 1 1 calc R . . C21 C 0.6087(2) 0.61910(19) 0.93610(14) 0.0269(5) Uani 1 1 d . . . C22 C 0.6234(3) 0.6479(2) 1.01312(16) 0.0350(6) Uani 1 1 d . . . H22 H 0.5671 0.6247 1.0369 0.042 Uiso 1 1 calc R . . C23 C 0.7389(3) 0.7185(2) 1.04878(15) 0.0347(6) Uani 1 1 d . . . H23 H 0.7731 0.7503 1.1008 0.042 Uiso 1 1 calc R . . C24 C 0.7934(2) 0.73299(18) 0.99360(14) 0.0267(5) Uani 1 1 d . . . C25 C 0.9173(2) 0.80026(18) 0.99999(14) 0.0269(5) Uani 1 1 d . . . C26 C 0.9803(2) 0.8702(2) 1.07993(16) 0.0344(6) Uani 1 1 d . . . H26A H 0.9767 0.8307 1.1201 0.052 Uiso 1 1 calc R . . H26B H 0.9448 0.9105 1.0854 0.052 Uiso 1 1 calc R . . H26C H 1.0588 0.9132 1.0844 0.052 Uiso 1 1 calc R . . C27 C 0.9246(2) 0.86354(19) 0.93561(16) 0.0306(5) Uani 1 1 d . . . H27A H 1.0033 0.9054 0.9400 0.046 Uiso 1 1 calc R . . H27B H 0.8905 0.9050 0.9411 0.046 Uiso 1 1 calc R . . H27C H 0.8844 0.8197 0.8856 0.046 Uiso 1 1 calc R . . C28 C 0.9722(2) 0.73564(19) 0.99243(14) 0.0277(5) Uani 1 1 d . . . C29 C 1.0608(3) 0.7285(2) 1.04524(16) 0.0365(6) Uani 1 1 d . . . H29 H 1.1015 0.7650 1.0958 0.044 Uiso 1 1 calc R . . C30 C 1.0782(3) 0.6561(2) 1.00859(18) 0.0406(7) Uani 1 1 d . . . H30 H 1.1325 0.6365 1.0305 0.049 Uiso 1 1 calc R . . C31 C 1.0006(2) 0.6197(2) 0.93472(16) 0.0331(6) Uani 1 1 d . . . C32 C 0.9779(3) 0.5456(2) 0.87208(16) 0.0358(6) Uani 1 1 d . . . H32 H 1.0227 0.5141 0.8772 0.043 Uiso 1 1 calc R . . C33 C 0.8715(2) 0.4487(2) 0.74760(15) 0.0294(5) Uani 1 1 d . . . C34 C 0.8754(3) 0.3603(2) 0.75805(17) 0.0372(6) Uani 1 1 d . . . H34 H 0.8954 0.3486 0.8085 0.045 Uiso 1 1 calc R . . C35 C 0.8506(3) 0.2883(2) 0.69604(17) 0.0341(6) Uani 1 1 d . . . C35A C 0.8594(3) 0.1950(2) 0.7109(2) 0.0488(8) Uani 1 1 d . . . H35A H 0.8833 0.1968 0.7660 0.073 Uiso 1 1 calc R . . H35B H 0.9144 0.1921 0.6896 0.073 Uiso 1 1 calc R . . H35C H 0.7861 0.1367 0.6866 0.073 Uiso 1 1 calc R . . C36 C 0.8188(2) 0.3055(2) 0.61997(16) 0.0309(6) Uani 1 1 d . . . C36A C 0.7939(3) 0.2305(2) 0.55096(18) 0.0402(7) Uani 1 1 d . . . H36A H 0.7673 0.2507 0.5036 0.060 Uiso 1 1 calc R . . H36B H 0.7362 0.1651 0.5527 0.060 Uiso 1 1 calc R . . H36C H 0.8625 0.2281 0.5528 0.060 Uiso 1 1 calc R . . C37 C 0.8121(2) 0.3929(2) 0.60936(16) 0.0287(5) Uani 1 1 d . . . H37 H 0.7891 0.4035 0.5589 0.034 Uiso 1 1 calc R . . C38 C 0.8389(2) 0.46500(19) 0.67177(15) 0.0253(5) Uani 1 1 d . . . C1S C 0.5294(3) 0.1909(3) 0.6578(2) 0.0529(9) Uani 1 1 d . . . H1S H 0.5939 0.2542 0.6724 0.064 Uiso 1 1 calc R . . C2S C 0.4311(4) 0.1793(3) 0.6651(2) 0.0582(9) Uani 1 1 d . . . H2S H 0.4271 0.2345 0.6849 0.070 Uiso 1 1 calc R . . C3S C 0.3369(4) 0.0866(4) 0.6435(3) 0.0787(14) Uani 1 1 d . . . H3S H 0.2684 0.0789 0.6482 0.094 Uiso 1 1 calc R . . C4S C 0.3417(4) 0.0043(3) 0.6150(3) 0.0758(13) Uani 1 1 d . . . H4S H 0.2768 -0.0587 0.5999 0.091 Uiso 1 1 calc R . . C5S C 0.4425(4) 0.0156(3) 0.6089(2) 0.0614(10) Uani 1 1 d . . . H5S H 0.4479 -0.0398 0.5914 0.074 Uiso 1 1 calc R . . C6S C 0.5351(3) 0.1095(3) 0.6289(2) 0.0580(9) Uani 1 1 d . . . H6S H 0.6032 0.1183 0.6227 0.070 Uiso 1 1 calc R . . C7S C 1.1504(4) 0.5906(5) 0.6031(3) 0.0846(16) Uani 1 1 d . . . H7S H 1.1242 0.5945 0.5511 0.102 Uiso 1 1 calc R . . C8S C 1.1115(4) 0.5014(5) 0.6234(5) 0.103(2) Uani 1 1 d . . . H8S H 1.0579 0.4447 0.5854 0.123 Uiso 1 1 calc R . . C9S C 1.1460(9) 0.4904(8) 0.6949(7) 0.139(4) Uani 1 1 d . . . H9S H 1.1189 0.4270 0.7081 0.167 Uiso 1 1 calc R . . C10S C 1.2238(12) 0.5755(14) 0.7503(6) 0.209(7) Uani 1 1 d . . . H10S H 1.2482 0.5709 0.8024 0.250 Uiso 1 1 calc R . . C11S C 1.2649(8) 0.6669(9) 0.7277(6) 0.164(5) Uani 1 1 d . . . H11S H 1.3211 0.7245 0.7639 0.197 Uiso 1 1 calc R . . C12S C 1.2244(5) 0.6736(5) 0.6536(4) 0.0930(18) Uani 1 1 d . . . H12S H 1.2482 0.7358 0.6383 0.112 Uiso 1 1 calc R . . C13S C 1.1570(5) 0.8552(5) 0.8582(5) 0.118(3) Uani 1 1 d . . . H13S H 1.0859 0.8096 0.8612 0.142 Uiso 1 1 calc R . . C14S C 1.2462(7) 0.8355(5) 0.8805(5) 0.140(3) Uani 1 1 d . . . H14S H 1.2367 0.7779 0.9008 0.168 Uiso 1 1 calc R . . C15S C 1.3458(6) 0.8974(4) 0.8734(4) 0.107(2) Uani 1 1 d . . . H15S H 1.4057 0.8826 0.8873 0.128 Uiso 1 1 calc R . . C16S C 1.3603(4) 0.9805(4) 0.8466(4) 0.1006(19) Uani 1 1 d . . . H16S H 1.4307 1.0240 0.8415 0.121 Uiso 1 1 calc R . . C17S C 1.2754(6) 1.0032(6) 0.8266(4) 0.119(2) Uani 1 1 d . . . H17S H 1.2873 1.0627 0.8087 0.143 Uiso 1 1 calc R . . C18S C 1.1715(5) 0.9394(6) 0.8323(3) 0.105(2) Uani 1 1 d . . . H18S H 1.1118 0.9545 0.8184 0.126 Uiso 1 1 calc R . . C19S C 0.6008(4) 0.9072(4) 0.7809(3) 0.0744(13) Uani 1 1 d . . . H19S H 0.5779 0.8900 0.7270 0.089 Uiso 1 1 calc R . . C20S C 0.6334(4) 1.0026(4) 0.8142(3) 0.0721(13) Uani 1 1 d . . . H20S H 0.6318 1.0496 0.7833 0.087 Uiso 1 1 calc R . . C21S C 0.6688(3) 1.0286(3) 0.8945(3) 0.0657(11) Uani 1 1 d . . . H21S H 0.6927 1.0938 0.9180 0.079 Uiso 1 1 calc R . . C22S C 0.6687(3) 0.9575(3) 0.9395(2) 0.0587(9) Uani 1 1 d . . . H22S H 0.6915 0.9738 0.9935 0.070 Uiso 1 1 calc R . . C23S C 0.6345(3) 0.8627(3) 0.9036(2) 0.0604(10) Uani 1 1 d . . . H23S H 0.6338 0.8142 0.9335 0.072 Uiso 1 1 calc R . . C24S C 0.60098(17) 0.83775(17) 0.82404(13) 0.0702(12) Uani 1 1 d . . . H24S H 0.5786 0.7731 0.8003 0.084 Uiso 1 1 calc R . . C26S C 0.42402(17) 0.74693(17) 1.04458(13) 0.0836(14) Uiso 1 1 d R . . H26S H 0.4726 0.8151 1.0487 0.100 Uiso 1 1 d R . . C25S C 0.37480(17) 0.68232(17) 0.97297(13) 0.064(2) Uiso 0.50 1 d PR A 1 H25S H 0.3904 0.7073 0.9291 0.077 Uiso 0.50 1 d PR B 1 C27S C 0.40068(17) 0.70965(17) 1.11008(13) 0.097(3) Uiso 0.50 1 d PR A 1 H27S H 0.4336 0.7529 1.1580 0.116 Uiso 0.50 1 calc PR C 1 C28S C 0.32811(17) 0.60775(17) 1.10397(13) 0.089(3) Uiso 0.50 1 d PR A 1 H28S H 0.3125 0.5828 1.1478 0.107 Uiso 0.50 1 calc PR D 1 C29S C 0.27889(17) 0.54315(17) 1.03236(13) 0.061(2) Uiso 0.50 1 d PR A 1 H29S H 0.2303 0.4750 1.0283 0.073 Uiso 0.50 1 calc PR E 1 C30S C 0.30223(17) 0.58043(17) 0.96686(13) 0.0562(18) Uiso 0.50 1 d PR A 1 H30S H 0.2693 0.5372 0.9190 0.067 Uiso 0.50 1 calc PR F 1 C29' C 0.29910(17) 0.56879(17) 1.08455(13) 0.0352(12) Uiso 0.50 1 d PR A 2 H29' H 0.2609 0.5087 1.1007 0.042 Uiso 0.50 1 calc PR G 2 C28' C 0.34996(17) 0.66053(17) 1.13730(13) 0.0476(15) Uiso 0.50 1 d PR A 2 H28' H 0.3425 0.6617 1.1867 0.057 Uiso 0.50 1 calc PR H 2 C27' C 0.41276(17) 0.75095(17) 1.11264(13) 0.066(2) Uiso 0.50 1 d PR A 2 H27' H 0.4456 0.8127 1.1454 0.079 Uiso 0.50 1 calc PR I 2 C30' C 0.30450(17) 0.56593(17) 1.01081(13) 0.0608(19) Uiso 0.50 1 d PR A 2 H30' H 0.2665 0.5072 0.9736 0.073 Uiso 0.50 1 calc PR J 2 C25' C 0.37330(17) 0.66083(17) 0.99698(13) 0.087(3) Uiso 0.50 1 d PR A 2 H25' H 0.3840 0.6627 0.9485 0.105 Uiso 0.50 1 calc PR K 2 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 0.01749(4) 0.01696(4) 0.01875(4) 0.00424(3) 0.00495(3) 0.00916(3) K1 0.0317(3) 0.0224(3) 0.0238(2) 0.0027(2) 0.0068(2) 0.0115(2) O1 0.0225(8) 0.0242(8) 0.0175(7) 0.0023(6) 0.0036(6) 0.0111(7) O2 0.0219(8) 0.0203(8) 0.0169(7) 0.0024(6) 0.0046(6) 0.0096(7) O3 0.0261(8) 0.0200(8) 0.0250(8) 0.0087(7) 0.0071(7) 0.0119(7) N1 0.0232(10) 0.0242(10) 0.0270(10) 0.0064(8) 0.0082(8) 0.0155(9) N2 0.0206(9) 0.0205(10) 0.0222(9) 0.0055(7) 0.0062(8) 0.0098(8) N3 0.0228(9) 0.0194(9) 0.0218(9) 0.0036(7) 0.0054(8) 0.0123(8) N4 0.0198(9) 0.0232(10) 0.0223(9) 0.0044(8) 0.0073(8) 0.0100(8) N5 0.0234(10) 0.0248(11) 0.0248(10) 0.0054(8) 0.0064(8) 0.0069(9) N6 0.0292(11) 0.0230(10) 0.0184(9) 0.0032(8) 0.0064(8) 0.0105(9) N7 0.0312(11) 0.0242(11) 0.0241(10) 0.0018(8) -0.0002(9) 0.0154(9) N8 0.0431(13) 0.0295(12) 0.0281(11) 0.0048(9) 0.0066(10) 0.0249(11) C1 0.0228(11) 0.0310(13) 0.0308(13) 0.0062(10) 0.0084(10) 0.0168(11) C2 0.0213(11) 0.0252(12) 0.0333(13) 0.0091(10) 0.0106(10) 0.0108(10) C3 0.0212(12) 0.0327(15) 0.0534(18) 0.0123(13) 0.0137(12) 0.0097(11) C4 0.0251(13) 0.0229(13) 0.0454(16) 0.0078(11) 0.0090(12) 0.0049(11) C5 0.0238(11) 0.0196(11) 0.0219(11) 0.0021(9) 0.0047(9) 0.0075(10) C6 0.0269(12) 0.0170(11) 0.0242(11) 0.0036(9) 0.0045(9) 0.0092(10) C7 0.0338(14) 0.0214(13) 0.0433(16) 0.0108(11) 0.0091(12) 0.0095(11) C8 0.0369(14) 0.0266(13) 0.0306(13) -0.0038(11) 0.0034(11) 0.0142(12) C9 0.0278(12) 0.0175(11) 0.0208(11) 0.0024(8) 0.0055(9) 0.0125(10) C10 0.0349(13) 0.0229(12) 0.0308(13) 0.0093(10) 0.0070(11) 0.0189(11) C11 0.0296(13) 0.0305(13) 0.0317(13) 0.0059(10) 0.0049(10) 0.0210(11) C12 0.0236(11) 0.0248(12) 0.0234(11) 0.0039(9) 0.0061(9) 0.0150(10) C13 0.0201(11) 0.0297(13) 0.0255(12) 0.0038(10) 0.0069(9) 0.0150(10) C14 0.0214(11) 0.0239(12) 0.0262(12) 0.0039(9) 0.0102(9) 0.0106(10) C15 0.0222(11) 0.0330(13) 0.0239(12) 0.0035(10) 0.0075(9) 0.0125(11) C16 0.0225(12) 0.0301(13) 0.0298(13) -0.0013(10) 0.0082(10) 0.0070(11) C16A 0.0315(15) 0.0425(18) 0.0349(15) -0.0023(13) 0.0042(12) 0.0027(13) C17 0.0261(12) 0.0267(13) 0.0326(13) 0.0013(10) 0.0132(11) 0.0060(11) C17A 0.0417(17) 0.0299(15) 0.0416(17) 0.0008(12) 0.0168(14) 0.0008(13) C18 0.0301(13) 0.0282(13) 0.0250(12) 0.0040(10) 0.0118(10) 0.0082(11) C19 0.0219(11) 0.0249(12) 0.0246(12) 0.0029(9) 0.0077(9) 0.0082(10) C20 0.0273(12) 0.0232(12) 0.0276(12) 0.0072(10) 0.0088(10) 0.0097(10) C21 0.0320(13) 0.0242(12) 0.0226(11) 0.0053(9) 0.0080(10) 0.0124(11) C22 0.0390(15) 0.0365(15) 0.0259(13) 0.0060(11) 0.0136(12) 0.0135(13) C23 0.0417(15) 0.0314(14) 0.0225(12) 0.0008(10) 0.0083(11) 0.0121(12) C24 0.0327(13) 0.0200(12) 0.0230(12) 0.0037(9) 0.0044(10) 0.0116(10) C25 0.0320(13) 0.0180(11) 0.0232(12) 0.0012(9) 0.0020(10) 0.0101(10) C26 0.0372(15) 0.0236(13) 0.0303(14) -0.0035(10) 0.0011(11) 0.0109(12) C27 0.0352(14) 0.0213(12) 0.0332(14) 0.0074(10) 0.0091(11) 0.0128(11) C28 0.0316(13) 0.0202(12) 0.0255(12) 0.0039(9) 0.0041(10) 0.0108(11) C29 0.0413(16) 0.0336(15) 0.0267(13) 0.0007(11) -0.0035(12) 0.0201(13) C30 0.0439(17) 0.0392(16) 0.0364(15) 0.0033(12) -0.0031(13) 0.0273(14) C31 0.0388(15) 0.0308(14) 0.0321(14) 0.0063(11) 0.0044(12) 0.0226(13) C32 0.0449(16) 0.0331(15) 0.0357(15) 0.0060(12) 0.0069(12) 0.0273(13) C33 0.0356(14) 0.0270(13) 0.0307(13) 0.0037(10) 0.0075(11) 0.0212(12) C34 0.0508(17) 0.0361(15) 0.0331(14) 0.0074(12) 0.0074(13) 0.0312(14) C35 0.0431(15) 0.0301(14) 0.0379(15) 0.0052(11) 0.0092(12) 0.0269(13) C35A 0.073(2) 0.0380(17) 0.0460(18) 0.0041(14) 0.0084(16) 0.0412(18) C36 0.0320(13) 0.0300(13) 0.0348(14) 0.0017(11) 0.0082(11) 0.0201(12) C36A 0.0482(17) 0.0399(16) 0.0403(16) 0.0000(13) 0.0096(14) 0.0306(15) C37 0.0308(13) 0.0313(13) 0.0305(13) 0.0076(10) 0.0104(11) 0.0198(11) C38 0.0231(11) 0.0264(12) 0.0315(13) 0.0061(10) 0.0083(10) 0.0162(10) C1S 0.054(2) 0.0398(18) 0.0442(18) 0.0085(15) 0.0012(16) 0.0141(16) C2S 0.075(3) 0.062(2) 0.0421(19) 0.0072(17) 0.0173(18) 0.038(2) C3S 0.055(2) 0.102(4) 0.074(3) 0.008(3) 0.036(2) 0.026(3) C4S 0.074(3) 0.051(2) 0.065(3) 0.007(2) 0.026(2) -0.002(2) C5S 0.084(3) 0.048(2) 0.053(2) 0.0098(17) 0.013(2) 0.037(2) C6S 0.047(2) 0.070(3) 0.058(2) 0.0182(19) 0.0109(17) 0.032(2) C7S 0.056(3) 0.121(5) 0.088(4) 0.004(4) 0.033(3) 0.048(3) C8S 0.050(3) 0.083(4) 0.173(7) -0.018(4) 0.049(4) 0.027(3) C9S 0.164(9) 0.167(9) 0.189(9) 0.104(8) 0.105(8) 0.131(8) C10S 0.211(14) 0.35(2) 0.074(5) 0.050(9) 0.013(7) 0.155(15) C11S 0.111(6) 0.179(10) 0.122(8) -0.069(7) 0.024(6) 0.020(7) C12S 0.079(4) 0.089(4) 0.139(6) 0.009(4) 0.067(4) 0.046(3) C13S 0.089(4) 0.081(4) 0.154(6) -0.028(4) 0.085(4) -0.005(3) C14S 0.178(7) 0.078(4) 0.243(9) 0.061(5) 0.157(7) 0.076(5) C15S 0.102(4) 0.076(4) 0.173(6) 0.024(4) 0.060(4) 0.059(4) C16S 0.063(3) 0.064(3) 0.170(6) 0.012(4) 0.050(4) 0.021(3) C17S 0.121(5) 0.155(6) 0.148(6) 0.103(5) 0.079(5) 0.096(5) C18S 0.073(3) 0.202(8) 0.053(3) 0.034(4) 0.018(2) 0.079(5) C19S 0.074(3) 0.109(4) 0.048(2) 0.010(2) 0.023(2) 0.050(3) C20S 0.070(3) 0.083(3) 0.084(3) 0.052(3) 0.044(3) 0.041(3) C21S 0.055(2) 0.044(2) 0.089(3) 0.001(2) 0.024(2) 0.0171(18) C22S 0.059(2) 0.071(3) 0.045(2) 0.0056(18) 0.0113(17) 0.035(2) C23S 0.067(2) 0.063(2) 0.070(3) 0.025(2) 0.025(2) 0.044(2) C24S 0.069(3) 0.069(3) 0.074(3) -0.009(2) 0.019(2) 0.039(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.7956(16) . ? U1 O2 1.8027(16) . ? U1 O3 2.1864(18) . ? U1 N2 2.476(2) . ? U1 N3 2.504(2) . ? U1 N1 2.531(2) . ? U1 N4 2.603(2) . ? U1 K1 3.7853(11) . ? U1 K1 4.1084(11) 2_666 ? K1 O3 2.6609(19) . ? K1 O2 2.8130(19) . ? K1 O2 2.8382(17) 2_666 ? K1 C12 3.007(2) 2_666 ? K1 C11 3.081(3) 2_666 ? K1 C15 3.109(3) . ? K1 N3 3.133(2) 2_666 ? K1 C10 3.229(3) 2_666 ? K1 C9 3.261(2) 2_666 ? K1 C14 3.367(2) . ? K1 C2S 3.373(4) . ? K1 C1S 3.516(4) . ? O2 K1 2.8382(18) 2_666 ? O3 H3A 0.9300 . ? N1 C1 1.298(3) . ? N1 C38 1.428(3) . ? N2 C5 1.356(3) . ? N2 C2 1.390(3) . ? N3 C9 1.356(3) . ? N3 C12 1.387(3) . ? N3 K1 3.133(2) 2_666 ? N4 C13 1.298(3) . ? N4 C14 1.420(3) . ? N5 C20 1.279(3) . ? N5 C19 1.405(3) . ? N6 C24 1.363(3) . ? N6 C21 1.373(3) . ? N6 H6 0.8600 . ? N7 C28 1.368(3) . ? N7 C31 1.377(3) . ? N7 H7 0.8600 . ? N8 C32 1.278(4) . ? N8 C33 1.409(3) . ? C1 C2 1.407(4) . ? C1 H1 0.9300 . ? C2 C3 1.392(4) . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.405(4) . ? C4 H4 0.9300 . ? C5 C6 1.517(3) . ? C6 C9 1.517(3) . ? C6 C7 1.533(4) . ? C6 C8 1.547(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.412(3) . ? C9 K1 3.261(2) 2_666 ? C10 C11 1.391(4) . ? C10 K1 3.229(3) 2_666 ? C10 H10 0.9300 . ? C11 C12 1.399(3) . ? C11 K1 3.081(3) 2_666 ? C11 H11 0.9300 . ? C12 C13 1.413(4) . ? C12 K1 3.007(2) 2_666 ? C13 H13 0.9300 . ? C14 C15 1.394(3) . ? C14 C19 1.402(3) . ? C15 C16 1.389(4) . ? C15 H15 0.9300 . ? C16 C17 1.403(4) . ? C16 C16A 1.511(4) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17 C18 1.389(4) . ? C17 C17A 1.510(4) . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18 C19 1.391(4) . ? C18 H18 0.9300 . ? C20 C21 1.433(4) . ? C20 H20 0.9300 . ? C21 C22 1.380(4) . ? C22 C23 1.400(4) . ? C22 H22 0.9300 . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 C25 1.516(4) . ? C25 C28 1.511(3) . ? C25 C26 1.533(3) . ? C25 C27 1.537(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.391(4) . ? C29 C30 1.407(4) . ? C29 H29 0.9300 . ? C30 C31 1.372(4) . ? C30 H30 0.9300 . ? C31 C32 1.431(4) . ? C32 H32 0.9300 . ? C33 C34 1.386(4) . ? C33 C38 1.397(4) . ? C34 C35 1.391(4) . ? C34 H34 0.9300 . ? C35 C36 1.404(4) . ? C35 C35A 1.504(4) . ? C35A H35A 0.9600 . ? C35A H35B 0.9600 . ? C35A H35C 0.9600 . ? C36 C37 1.389(4) . ? C36 C36A 1.512(4) . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37 C38 1.389(3) . ? C37 H37 0.9300 . ? C1S C2S 1.338(6) . ? C1S C6S 1.369(5) . ? C1S H1S 0.9300 . ? C2S C3S 1.362(6) . ? C2S H2S 0.9300 . ? C3S C4S 1.370(7) . ? C3S H3S 0.9300 . ? C4S C5S 1.365(7) . ? C4S H4S 0.9300 . ? C5S C6S 1.363(6) . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? C7S C12S 1.308(8) . ? C7S C8S 1.321(9) . ? C7S H7S 0.9300 . ? C8S C9S 1.301(10) . ? C8S H8S 0.9300 . ? C9S C10S 1.376(15) . ? C9S H9S 0.9300 . ? C10S C11S 1.369(16) . ? C10S H10S 0.9300 . ? C11S C12S 1.337(12) . ? C11S H11S 0.9300 . ? C12S H12S 0.9300 . ? C13S C18S 1.327(9) . ? C13S C14S 1.363(10) . ? C13S H13S 0.9300 . ? C14S C15S 1.317(8) . ? C14S H14S 0.9300 . ? C15S C16S 1.319(8) . ? C15S H15S 0.9300 . ? C16S C17S 1.335(7) . ? C16S H16S 0.9300 . ? C17S C18S 1.358(9) . ? C17S H17S 0.9300 . ? C18S H18S 0.9300 . ? C19S C24S 1.337(6) . ? C19S C20S 1.364(7) . ? C19S H19S 0.9300 . ? C20S C21S 1.383(6) . ? C20S H20S 0.9300 . ? C21S C22S 1.379(6) . ? C21S H21S 0.9300 . ? C22S C23S 1.365(5) . ? C22S H22S 0.9300 . ? C23S C24S 1.371(5) . ? C23S H23S 0.9300 . ? C24S H24S 0.9300 . ? C26S C27' 1.2891 . ? C26S C25' 1.3041 . ? C26S C25S 1.3900 . ? C26S C27S 1.3900 . ? C26S H26S 0.9300 . ? C25S C30S 1.3900 . ? C25S H25S 0.9300 . ? C27S C28S 1.3900 . ? C27S H27S 0.9300 . ? C28S C29S 1.3900 . ? C28S H28S 0.9300 . ? C29S C30S 1.3900 . ? C29S H29S 0.9300 . ? C30S H30S 0.9300 . ? C29' C30' 1.3607 . ? C29' C28' 1.4127 . ? C29' H29' 0.9300 . ? C28' C27' 1.4201 . ? C28' H28' 0.9300 . ? C27' H27' 0.9300 . ? C30' C25' 1.3998 . ? C30' H30' 0.9300 . ? C25' H25S 1.4636 . ? C25' H25' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 179.14(7) . . ? O1 U1 O3 94.52(7) . . ? O2 U1 O3 86.33(7) . . ? O1 U1 N2 89.79(7) . . ? O2 U1 N2 89.46(7) . . ? O3 U1 N2 147.01(6) . . ? O1 U1 N3 94.57(7) . . ? O2 U1 N3 84.79(7) . . ? O3 U1 N3 141.48(7) . . ? N2 U1 N3 70.29(7) . . ? O1 U1 N1 94.38(7) . . ? O2 U1 N1 85.72(7) . . ? O3 U1 N1 79.13(7) . . ? N2 U1 N1 67.93(7) . . ? N3 U1 N1 137.15(7) . . ? O1 U1 N4 97.25(7) . . ? O2 U1 N4 83.01(7) . . ? O3 U1 N4 76.04(6) . . ? N2 U1 N4 135.83(6) . . ? N3 U1 N4 65.71(7) . . ? N1 U1 N4 153.28(7) . . ? O1 U1 K1 135.94(6) . . ? O2 U1 K1 44.91(5) . . ? O3 U1 K1 43.39(5) . . ? N2 U1 K1 131.65(5) . . ? N3 U1 K1 111.48(5) . . ? N1 U1 K1 89.84(5) . . ? N4 U1 K1 65.24(5) . . ? O1 U1 K1 143.90(6) . 2_666 ? O2 U1 K1 35.40(5) . 2_666 ? O3 U1 K1 116.08(5) . 2_666 ? N2 U1 K1 75.09(5) . 2_666 ? N3 U1 K1 49.61(4) . 2_666 ? N1 U1 K1 109.18(5) . 2_666 ? N4 U1 K1 73.87(5) . 2_666 ? K1 U1 K1 72.81(2) . 2_666 ? O3 K1 O2 60.08(5) . . ? O3 K1 O2 121.65(5) . 2_666 ? O2 K1 O2 67.74(6) . 2_666 ? O3 K1 C12 132.37(6) . 2_666 ? O2 K1 C12 92.52(6) . 2_666 ? O2 K1 C12 71.02(6) 2_666 2_666 ? O3 K1 C11 121.01(7) . 2_666 ? O2 K1 C11 107.22(7) . 2_666 ? O2 K1 C11 97.14(6) 2_666 2_666 ? C12 K1 C11 26.53(7) 2_666 2_666 ? O3 K1 C15 82.86(6) . . ? O2 K1 C15 94.51(6) . . ? O2 K1 C15 76.80(6) 2_666 . ? C12 K1 C15 141.44(7) 2_666 . ? C11 K1 C15 153.45(7) 2_666 . ? O3 K1 N3 158.04(6) . 2_666 ? O2 K1 N3 106.07(5) . 2_666 ? O2 K1 N3 58.95(5) 2_666 2_666 ? C12 K1 N3 26.00(6) 2_666 2_666 ? C11 K1 N3 43.07(6) 2_666 2_666 ? C15 K1 N3 116.75(6) . 2_666 ? O3 K1 C10 133.24(6) . 2_666 ? O2 K1 C10 131.89(6) . 2_666 ? O2 K1 C10 100.48(6) 2_666 2_666 ? C12 K1 C10 41.84(7) 2_666 2_666 ? C11 K1 C10 25.33(7) 2_666 2_666 ? C15 K1 C10 129.41(7) . 2_666 ? N3 K1 C10 41.76(6) 2_666 2_666 ? O3 K1 C9 158.31(6) . 2_666 ? O2 K1 C9 130.08(6) . 2_666 ? O2 K1 C9 78.18(6) 2_666 2_666 ? C12 K1 C9 40.81(7) 2_666 2_666 ? C11 K1 C9 41.44(7) 2_666 2_666 ? C15 K1 C9 112.38(7) . 2_666 ? N3 K1 C9 24.39(5) 2_666 2_666 ? C10 K1 C9 25.12(6) 2_666 2_666 ? O3 K1 C14 59.37(6) . . ? O2 K1 C14 76.97(6) . . ? O2 K1 C14 85.92(6) 2_666 . ? C12 K1 C14 156.90(6) 2_666 . ? C11 K1 C14 175.50(7) 2_666 . ? C15 K1 C14 24.44(6) . . ? N3 K1 C14 138.00(6) 2_666 . ? C10 K1 C14 150.81(7) 2_666 . ? C9 K1 C14 136.83(6) 2_666 . ? O3 K1 C2S 73.21(8) . . ? O2 K1 C2S 132.33(8) . . ? O2 K1 C2S 156.65(8) 2_666 . ? C12 K1 C2S 113.87(8) 2_666 . ? C11 K1 C2S 88.04(9) 2_666 . ? C15 K1 C2S 88.40(9) . . ? N3 K1 C2S 114.81(8) 2_666 . ? C10 K1 C2S 74.97(8) 2_666 . ? C9 K1 C2S 91.26(8) 2_666 . ? C14 K1 C2S 87.87(8) . . ? O3 K1 C1S 68.30(7) . . ? O2 K1 C1S 119.45(7) . . ? O2 K1 C1S 169.65(7) 2_666 . ? C12 K1 C1S 100.38(8) 2_666 . ? C11 K1 C1S 73.93(8) 2_666 . ? C15 K1 C1S 108.77(9) . . ? N3 K1 C1S 110.81(7) 2_666 . ? C10 K1 C1S 69.20(8) 2_666 . ? C9 K1 C1S 91.54(8) 2_666 . ? C14 K1 C1S 102.70(8) . . ? C2S K1 C1S 22.27(9) . . ? U1 O2 K1 108.19(7) . . ? U1 O2 K1 123.01(8) . 2_666 ? K1 O2 K1 112.26(6) . 2_666 ? U1 O3 K1 102.25(6) . . ? U1 O3 H3A 128.9 . . ? K1 O3 H3A 128.9 . . ? C1 N1 C38 116.7(2) . . ? C1 N1 U1 115.07(15) . . ? C38 N1 U1 127.97(15) . . ? C5 N2 C2 105.9(2) . . ? C5 N2 U1 139.06(15) . . ? C2 N2 U1 114.38(15) . . ? C9 N3 C12 106.52(19) . . ? C9 N3 U1 135.24(15) . . ? C12 N3 U1 114.49(15) . . ? C9 N3 K1 83.11(13) . 2_666 ? C12 N3 K1 71.90(12) . 2_666 ? U1 N3 K1 92.90(6) . 2_666 ? C13 N4 C14 118.5(2) . . ? C13 N4 U1 114.37(16) . . ? C14 N4 U1 125.01(14) . . ? C20 N5 C19 118.3(2) . . ? C24 N6 C21 110.2(2) . . ? C24 N6 H6 124.9 . . ? C21 N6 H6 124.9 . . ? C28 N7 C31 110.2(2) . . ? C28 N7 H7 124.9 . . ? C31 N7 H7 124.9 . . ? C32 N8 C33 120.0(2) . . ? N1 C1 C2 121.8(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? N2 C2 C3 110.3(2) . . ? N2 C2 C1 120.5(2) . . ? C3 C2 C1 129.2(2) . . ? C4 C3 C2 106.3(2) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? C3 C4 C5 107.3(2) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? N2 C5 C4 110.2(2) . . ? N2 C5 C6 123.5(2) . . ? C4 C5 C6 126.0(2) . . ? C9 C6 C5 114.33(19) . . ? C9 C6 C7 109.3(2) . . ? C5 C6 C7 109.1(2) . . ? C9 C6 C8 107.6(2) . . ? C5 C6 C8 107.2(2) . . ? C7 C6 C8 109.3(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 110.1(2) . . ? N3 C9 C6 122.8(2) . . ? C10 C9 C6 126.5(2) . . ? N3 C9 K1 72.50(12) . 2_666 ? C10 C9 K1 76.15(14) . 2_666 ? C6 C9 K1 125.17(14) . 2_666 ? C11 C10 C9 106.8(2) . . ? C11 C10 K1 71.38(14) . 2_666 ? C9 C10 K1 78.74(14) . 2_666 ? C11 C10 H10 126.6 . . ? C9 C10 H10 126.6 . . ? K1 C10 H10 115.6 2_666 . ? C10 C11 C12 106.6(2) . . ? C10 C11 K1 83.29(15) . 2_666 ? C12 C11 K1 73.77(14) . 2_666 ? C10 C11 H11 126.7 . . ? C12 C11 H11 126.7 . . ? K1 C11 H11 109.4 2_666 . ? N3 C12 C11 110.0(2) . . ? N3 C12 C13 120.2(2) . . ? C11 C12 C13 129.9(2) . . ? N3 C12 K1 82.10(13) . 2_666 ? C11 C12 K1 79.70(15) . 2_666 ? C13 C12 K1 105.91(15) . 2_666 ? N4 C13 C12 120.6(2) . . ? N4 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C19 119.0(2) . . ? C15 C14 N4 122.5(2) . . ? C19 C14 N4 118.5(2) . . ? C15 C14 K1 67.34(13) . . ? C19 C14 K1 116.21(16) . . ? N4 C14 K1 86.97(13) . . ? C16 C15 C14 121.9(2) . . ? C16 C15 K1 104.94(16) . . ? C14 C15 K1 88.22(14) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? K1 C15 H15 76.5 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 C16A 119.9(3) . . ? C17 C16 C16A 120.9(3) . . ? C16 C16A H16A 109.5 . . ? C16 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C16 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C18 C17 C16 118.8(2) . . ? C18 C17 C17A 119.7(3) . . ? C16 C17 C17A 121.5(2) . . ? C17 C17A H17A 109.5 . . ? C17 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C17 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C17 C18 C19 122.3(2) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C18 C19 C14 118.8(2) . . ? C18 C19 N5 123.5(2) . . ? C14 C19 N5 117.6(2) . . ? N5 C20 C21 120.7(2) . . ? N5 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? N6 C21 C22 107.3(2) . . ? N6 C21 C20 121.5(2) . . ? C22 C21 C20 131.3(3) . . ? C21 C22 C23 107.3(2) . . ? C21 C22 H22 126.4 . . ? C23 C22 H22 126.4 . . ? C24 C23 C22 108.4(2) . . ? C24 C23 H23 125.8 . . ? C22 C23 H23 125.8 . . ? N6 C24 C23 107.0(2) . . ? N6 C24 C25 122.2(2) . . ? C23 C24 C25 130.8(2) . . ? C28 C25 C24 109.1(2) . . ? C28 C25 C26 109.2(2) . . ? C24 C25 C26 109.0(2) . . ? C28 C25 C27 109.8(2) . . ? C24 C25 C27 110.2(2) . . ? C26 C25 C27 109.5(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N7 C28 C29 106.8(2) . . ? N7 C28 C25 122.2(2) . . ? C29 C28 C25 131.0(2) . . ? C28 C29 C30 107.9(2) . . ? C28 C29 H29 126.1 . . ? C30 C29 H29 126.1 . . ? C31 C30 C29 107.7(2) . . ? C31 C30 H30 126.1 . . ? C29 C30 H30 126.1 . . ? C30 C31 N7 107.5(2) . . ? C30 C31 C32 132.6(3) . . ? N7 C31 C32 119.9(2) . . ? N8 C32 C31 119.6(2) . . ? N8 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C34 C33 C38 118.7(2) . . ? C34 C33 N8 124.0(2) . . ? C38 C33 N8 117.3(2) . . ? C33 C34 C35 122.5(3) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C34 C35 C36 118.5(2) . . ? C34 C35 C35A 120.3(3) . . ? C36 C35 C35A 121.2(2) . . ? C35 C35A H35A 109.5 . . ? C35 C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C35 C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C37 C36 C35 119.0(2) . . ? C37 C36 C36A 120.7(3) . . ? C35 C36 C36A 120.3(2) . . ? C36 C36A H36A 109.5 . . ? C36 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C36 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C38 C37 C36 122.0(2) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C33 119.3(2) . . ? C37 C38 N1 121.4(2) . . ? C33 C38 N1 119.2(2) . . ? C2S C1S C6S 119.9(4) . . ? C2S C1S K1 72.8(2) . . ? C6S C1S K1 125.8(2) . . ? C2S C1S H1S 120.0 . . ? C6S C1S H1S 120.0 . . ? K1 C1S H1S 73.1 . . ? C1S C2S C3S 119.9(4) . . ? C1S C2S K1 84.9(2) . . ? C3S C2S K1 119.9(3) . . ? C1S C2S H2S 120.1 . . ? C3S C2S H2S 120.1 . . ? K1 C2S H2S 65.8 . . ? C2S C3S C4S 120.8(4) . . ? C2S C3S H3S 119.6 . . ? C4S C3S H3S 119.6 . . ? C5S C4S C3S 119.5(4) . . ? C5S C4S H4S 120.3 . . ? C3S C4S H4S 120.3 . . ? C6S C5S C4S 118.9(4) . . ? C6S C5S H5S 120.5 . . ? C4S C5S H5S 120.5 . . ? C5S C6S C1S 121.0(4) . . ? C5S C6S H6S 119.5 . . ? C1S C6S H6S 119.5 . . ? C12S C7S C8S 122.3(7) . . ? C12S C7S H7S 118.8 . . ? C8S C7S H7S 118.8 . . ? C9S C8S C7S 122.0(7) . . ? C9S C8S H8S 119.0 . . ? C7S C8S H8S 119.0 . . ? C8S C9S C10S 118.0(9) . . ? C8S C9S H9S 121.0 . . ? C10S C9S H9S 121.0 . . ? C11S C10S C9S 119.0(9) . . ? C11S C10S H10S 120.5 . . ? C9S C10S H10S 120.5 . . ? C12S C11S C10S 120.2(9) . . ? C12S C11S H11S 119.9 . . ? C10S C11S H11S 119.9 . . ? C7S C12S C11S 118.4(8) . . ? C7S C12S H12S 120.8 . . ? C11S C12S H12S 120.8 . . ? C18S C13S C14S 120.0(5) . . ? C18S C13S H13S 120.0 . . ? C14S C13S H13S 120.0 . . ? C15S C14S C13S 120.4(6) . . ? C15S C14S H14S 119.8 . . ? C13S C14S H14S 119.8 . . ? C14S C15S C16S 119.8(6) . . ? C14S C15S H15S 120.1 . . ? C16S C15S H15S 120.1 . . ? C15S C16S C17S 120.9(6) . . ? C15S C16S H16S 119.5 . . ? C17S C16S H16S 119.5 . . ? C16S C17S C18S 120.1(6) . . ? C16S C17S H17S 120.0 . . ? C18S C17S H17S 120.0 . . ? C13S C18S C17S 118.7(6) . . ? C13S C18S H18S 120.7 . . ? C17S C18S H18S 120.7 . . ? C24S C19S C20S 121.5(4) . . ? C24S C19S H19S 119.2 . . ? C20S C19S H19S 119.2 . . ? C19S C20S C21S 119.3(4) . . ? C19S C20S H20S 120.3 . . ? C21S C20S H20S 120.3 . . ? C22S C21S C20S 119.6(4) . . ? C22S C21S H21S 120.2 . . ? C20S C21S H21S 120.2 . . ? C23S C22S C21S 119.0(4) . . ? C23S C22S H22S 120.5 . . ? C21S C22S H22S 120.5 . . ? C22S C23S C24S 121.1(3) . . ? C22S C23S H23S 119.5 . . ? C24S C23S H23S 119.5 . . ? C19S C24S C23S 119.4(3) . . ? C19S C24S H24S 120.3 . . ? C23S C24S H24S 120.3 . . ? C27' C26S C25' 120.3 . . ? C27' C26S C25S 140.7 . . ? C25' C26S C25S 23.4 . . ? C27' C26S C27S 24.1 . . ? C25' C26S C27S 97.6 . . ? C25S C26S C27S 120.0 . . ? C27' C26S H26S 98.0 . . ? C25' C26S H26S 141.7 . . ? C25S C26S H26S 120.0 . . ? C27S C26S H26S 120.0 . . ? C26S C25S C30S 120.0 . . ? C26S C25S H25S 120.0 . . ? C30S C25S H25S 120.0 . . ? C26S C27S C28S 120.0 . . ? C26S C27S H27S 120.0 . . ? C28S C27S H27S 120.0 . . ? C29S C28S C27S 120.0 . . ? C29S C28S H28S 120.0 . . ? C27S C28S H28S 120.0 . . ? C30S C29S C28S 120.0 . . ? C30S C29S H29S 120.0 . . ? C28S C29S H29S 120.0 . . ? C29S C30S C25S 120.0 . . ? C29S C30S H30S 120.0 . . ? C25S C30S H30S 120.0 . . ? C30' C29' C28' 121.8 . . ? C30' C29' H29' 119.1 . . ? C28' C29' H29' 119.1 . . ? C29' C28' C27' 118.0 . . ? C29' C28' H28' 121.0 . . ? C27' C28' H28' 121.0 . . ? C26S C27' C28' 119.7 . . ? C26S C27' H27' 120.2 . . ? C28' C27' H27' 120.2 . . ? C29' C30' C25' 112.8 . . ? C29' C30' H30' 123.6 . . ? C25' C30' H30' 123.6 . . ? C26S C25' C30' 127.1 . . ? C26S C25' H25S 93.7 . . ? C30' C25' H25S 137.1 . . ? C26S C25' H25' 116.4 . . ? C30' C25' H25' 116.4 . . ? H25S C25' H25' 26.5 . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.219 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.104 data_po7030 _database_code_depnum_ccdc_archive 'CCDC 752124' #TrackingRef 'combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H66 K N8 O5.50 U' _chemical_formula_sum 'C55 H66 K N8 O5.50 U' _chemical_formula_weight 1204.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, z' _cell_length_a 22.7824(11) _cell_length_b 23.0693(10) _cell_length_c 10.9145(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5736.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11782 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2428 _exptl_absorpt_coefficient_mu 2.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5140 _exptl_absorpt_correction_T_max 0.7001 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 60407 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11782 _reflns_number_gt 11517 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (GIACOVAZZO, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP(Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al.,2004)' _refine_special_details ; Twin law 0 -1 0 -1 0 0 0 0 -1 applied, twin component 0.1199(11) Benzene solvent carbons C40s C41s C42s C43s C20s C21s C22s and THF atoms O5 O6 O30s C39 c40-C46 C31s- C34s were refined isotropically 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^ > 2\s(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^)+(0.0726P)^2^+28.6785P] 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 riding _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 0.052(11) _refine_ls_number_reflns 11782 _refine_ls_number_parameters 563 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.735572(15) 0.787663(14) 0.13608(3) 0.01390(8) Uani 1 1 d . . . K1 K 0.81118(11) 0.70426(11) -0.1396(2) 0.0340(5) Uani 1 1 d . . . O1 O 0.7242(3) 0.7990(3) -0.0273(5) 0.0161(14) Uani 1 1 d . . . O2 O 0.7481(3) 0.7752(3) 0.2955(5) 0.0232(17) Uani 1 1 d . . . O3 O 0.7965(3) 0.7174(4) 0.0926(6) 0.0265(15) Uani 1 1 d . . . H300 H 0.8151 0.6948 0.1515 0.040 Uiso 1 1 calc R . . N1 N 0.8360(4) 0.8404(3) 0.1523(7) 0.0155(16) Uani 1 1 d . . . N2 N 0.7286(4) 0.8931(3) 0.1860(8) 0.0180(16) Uani 1 1 d . . . N3 N 0.6316(4) 0.8133(4) 0.1929(7) 0.0192(18) Uani 1 1 d . . . N4 N 0.6668(3) 0.7009(3) 0.1557(6) 0.0140(17) Uani 1 1 d . . . N5 N 0.6909(4) 0.6578(4) -0.0743(7) 0.0202(18) Uani 1 1 d . . . N6 N 0.6861(4) 0.7389(4) -0.2635(8) 0.0222(19) Uani 1 1 d . . . H6 H 0.6950 0.7543 -0.1942 0.027 Uiso 1 1 calc R . . N7 N 0.7904(4) 0.8314(4) -0.2639(7) 0.0173(16) Uani 1 1 d . . . H7 H 0.7750 0.8189 -0.1971 0.021 Uiso 1 1 calc R . . N8 N 0.8715(4) 0.8114(4) -0.0803(7) 0.0177(16) Uani 1 1 d . . . C1 C 0.8338(5) 0.8892(5) 0.2081(9) 0.021(2) Uani 1 1 d . . . H1 H 0.8683 0.9059 0.2370 0.026 Uiso 1 1 calc R . . C2 C 0.7797(4) 0.9181(4) 0.2263(9) 0.016(2) Uani 1 1 d . . . C3 C 0.7666(7) 0.9718(4) 0.2798(9) 0.030(2) Uani 1 1 d . . . H3 H 0.7932 0.9966 0.3177 0.036 Uiso 1 1 calc R . . C4 C 0.7090(6) 0.9809(5) 0.2665(10) 0.026(2) Uani 1 1 d . . . H4 H 0.6886 1.0138 0.2908 0.031 Uiso 1 1 calc R . . C5 C 0.6846(6) 0.9318(4) 0.2092(9) 0.023(2) Uani 1 1 d . . . C6 C 0.6219(5) 0.9202(5) 0.1717(9) 0.025(2) Uani 1 1 d . . . C7 C 0.6179(6) 0.9209(5) 0.0304(10) 0.032(3) Uani 1 1 d . . . H7A H 0.5781 0.9138 0.0058 0.047 Uiso 1 1 calc R . . H7B H 0.6429 0.8913 -0.0026 0.047 Uiso 1 1 calc R . . H7C H 0.6303 0.9580 0.0003 0.047 Uiso 1 1 calc R . . C8 C 0.5823(6) 0.9674(6) 0.2191(12) 0.039(3) Uani 1 1 d . . . H8A H 0.5426 0.9597 0.1942 0.058 Uiso 1 1 calc R . . H8B H 0.5946 1.0041 0.1864 0.058 Uiso 1 1 calc R . . H8C H 0.5843 0.9685 0.3069 0.058 Uiso 1 1 calc R . . C9 C 0.6005(4) 0.8615(4) 0.2154(9) 0.018(2) Uani 1 1 d . . . C10 C 0.5488(5) 0.8474(5) 0.2745(10) 0.028(2) Uani 1 1 d . . . H10 H 0.5201 0.8735 0.2996 0.034 Uiso 1 1 calc R . . C11 C 0.5472(5) 0.7871(6) 0.2900(9) 0.028(2) Uani 1 1 d . . . H11 H 0.5182 0.7651 0.3279 0.034 Uiso 1 1 calc R . . C12 C 0.5988(5) 0.7676(4) 0.2359(10) 0.020(2) Uani 1 1 d . . . C13 C 0.6182(5) 0.7100(5) 0.2162(8) 0.021(2) Uani 1 1 d . . . H13 H 0.5966 0.6789 0.2462 0.025 Uiso 1 1 calc R . . C14 C 0.6818(4) 0.6420(4) 0.1423(9) 0.0140(16) Uani 1 1 d . . . C15 C 0.6895(6) 0.6058(5) 0.2438(10) 0.028(3) Uani 1 1 d . . . H15 H 0.6851 0.6210 0.3222 0.034 Uiso 1 1 calc R . . C16 C 0.7036(6) 0.5470(5) 0.2297(11) 0.030(3) Uani 1 1 d . . . C16A C 0.7146(8) 0.5104(5) 0.3434(11) 0.053(4) Uani 1 1 d . . . H16A H 0.6925 0.4751 0.3379 0.080 Uiso 1 1 calc R . . H16B H 0.7027 0.5315 0.4149 0.080 Uiso 1 1 calc R . . H16C H 0.7557 0.5014 0.3492 0.080 Uiso 1 1 calc R . . C17 C 0.7119(4) 0.5242(5) 0.1134(11) 0.026(2) Uani 1 1 d . . . C17A C 0.7280(7) 0.4614(5) 0.0926(12) 0.038(3) Uani 1 1 d . . . H17A H 0.7625 0.4521 0.1390 0.057 Uiso 1 1 calc R . . H17B H 0.7355 0.4552 0.0071 0.057 Uiso 1 1 calc R . . H17C H 0.6961 0.4371 0.1185 0.057 Uiso 1 1 calc R . . C18 C 0.7070(5) 0.5601(5) 0.0124(10) 0.023(2) Uani 1 1 d . . . H18 H 0.7132 0.5450 -0.0656 0.027 Uiso 1 1 calc R . . C19 C 0.6929(5) 0.6185(4) 0.0254(9) 0.018(2) Uani 1 1 d . . . C20 C 0.6739(5) 0.6419(4) -0.1819(9) 0.022(2) Uani 1 1 d . . . H20 H 0.6616 0.6040 -0.1946 0.026 Uiso 1 1 calc R . . C21 C 0.6739(5) 0.6818(5) -0.2817(10) 0.024(2) Uani 1 1 d . . . C22 C 0.6610(6) 0.6756(5) -0.4046(11) 0.033(3) Uani 1 1 d . . . H22 H 0.6493 0.6413 -0.4421 0.040 Uiso 1 1 calc R . . C23 C 0.6683(5) 0.7288(5) -0.4642(11) 0.025(2) Uiso 1 1 d . . . H23 H 0.6647 0.7358 -0.5478 0.030 Uiso 1 1 calc R . . C24 C 0.6819(4) 0.7691(4) -0.3747(10) 0.0178(19) Uiso 1 1 d . . . C25 C 0.6936(4) 0.8322(4) -0.3813(9) 0.0155(18) Uiso 1 1 d . . . C26 C 0.6734(5) 0.8552(5) -0.5043(9) 0.023(2) Uani 1 1 d . . . H26A H 0.6813 0.8960 -0.5090 0.034 Uiso 1 1 calc R . . H26B H 0.6320 0.8486 -0.5132 0.034 Uiso 1 1 calc R . . H26C H 0.6941 0.8355 -0.5686 0.034 Uiso 1 1 calc R . . C27 C 0.6620(5) 0.8646(5) -0.2784(8) 0.021(2) Uani 1 1 d . . . H27A H 0.6705 0.9053 -0.2843 0.031 Uiso 1 1 calc R . . H27B H 0.6753 0.8503 -0.2006 0.031 Uiso 1 1 calc R . . H27C H 0.6205 0.8586 -0.2856 0.031 Uiso 1 1 calc R . . C28 C 0.7597(4) 0.8426(4) -0.3705(9) 0.0178(17) Uani 1 1 d . . . C29 C 0.8011(6) 0.8587(5) -0.4560(9) 0.027(2) Uani 1 1 d . . . H29 H 0.7935 0.8680 -0.5374 0.033 Uiso 1 1 calc R . . C30 C 0.8568(5) 0.8587(5) -0.4001(10) 0.028(2) Uani 1 1 d . . . H30 H 0.8922 0.8677 -0.4380 0.033 Uiso 1 1 calc R . . C31 C 0.8495(5) 0.8431(5) -0.2793(9) 0.019(2) Uani 1 1 d . . . C32 C 0.8905(5) 0.8332(4) -0.1815(9) 0.020(2) Uani 1 1 d . . . H32 H 0.9300 0.8424 -0.1910 0.025 Uiso 1 1 calc R . . C33 C 0.9106(5) 0.8004(4) 0.0167(9) 0.020(2) Uani 1 1 d . . . C34 C 0.9635(5) 0.7742(5) 0.0026(10) 0.024(2) Uani 1 1 d . . . H34 H 0.9760 0.7655 -0.0764 0.029 Uiso 1 1 calc R . . C35 C 1.0002(5) 0.7597(5) 0.1005(10) 0.029(2) Uani 1 1 d . . . C35A C 1.0578(5) 0.7300(6) 0.0802(13) 0.041(3) Uani 1 1 d . . . H35A H 1.0581 0.7124 0.0006 0.062 Uiso 1 1 calc R . . H35B H 1.0634 0.7008 0.1417 0.062 Uiso 1 1 calc R . . H35C H 1.0890 0.7580 0.0854 0.062 Uiso 1 1 calc R . . C36 C 0.9797(5) 0.7704(6) 0.2220(11) 0.033(3) Uani 1 1 d . . . C36A C 1.0144(7) 0.7520(9) 0.3332(12) 0.062(5) Uani 1 1 d . . . H36A H 1.0429 0.7813 0.3526 0.094 Uiso 1 1 calc R . . H36B H 1.0341 0.7161 0.3163 0.094 Uiso 1 1 calc R . . H36C H 0.9883 0.7470 0.4014 0.094 Uiso 1 1 calc R . . C37 C 0.9256(5) 0.7974(6) 0.2340(10) 0.028(3) Uani 1 1 d . . . H37 H 0.9115 0.8046 0.3125 0.033 Uiso 1 1 calc R . . C38 C 0.8918(4) 0.8138(4) 0.1358(10) 0.0166(17) Uani 1 1 d . . . O5 O 0.8503(6) 0.6789(6) -0.3658(14) 0.073(3) Uiso 1 1 d . . . C39 C 0.8379(11) 0.7068(12) -0.477(2) 0.093(7) Uiso 1 1 d . . . H39A H 0.8013 0.7280 -0.4701 0.111 Uiso 1 1 calc R . . H39B H 0.8688 0.7344 -0.4956 0.111 Uiso 1 1 calc R . . C40 C 0.8337(12) 0.6667(11) -0.571(2) 0.096(7) Uiso 1 1 d . . . H40A H 0.8607 0.6759 -0.6373 0.116 Uiso 1 1 calc R . . H40B H 0.7941 0.6653 -0.6041 0.116 Uiso 1 1 calc R . . C41 C 0.850(2) 0.611(2) -0.512(4) 0.188(18) Uiso 1 1 d . . . H41A H 0.8724 0.5864 -0.5653 0.225 Uiso 1 1 calc R . . H41B H 0.8152 0.5903 -0.4829 0.225 Uiso 1 1 calc R . . C42 C 0.8873(14) 0.6350(14) -0.403(3) 0.124(9) Uiso 1 1 d . . . H42A H 0.8930 0.6062 -0.3389 0.149 Uiso 1 1 calc R . . H42B H 0.9251 0.6496 -0.4297 0.149 Uiso 1 1 calc R . . O6 O 0.8836(6) 0.6141(6) -0.0711(12) 0.068(3) Uiso 1 1 d . . . C43 C 0.8510(10) 0.5869(11) 0.020(2) 0.083(6) Uiso 1 1 d . . . H43A H 0.8153 0.6090 0.0339 0.099 Uiso 1 1 calc R . . H43B H 0.8396 0.5487 -0.0086 0.099 Uiso 1 1 calc R . . C44 C 0.8801(11) 0.5811(11) 0.129(3) 0.104(7) Uiso 1 1 d . . . H44A H 0.8941 0.5418 0.1407 0.124 Uiso 1 1 calc R . . H44B H 0.8553 0.5919 0.1977 0.124 Uiso 1 1 calc R . . C45 C 0.9286(13) 0.6215(13) 0.114(3) 0.120(9) Uiso 1 1 d . . . H45A H 0.9622 0.6098 0.1626 0.144 Uiso 1 1 calc R . . H45B H 0.9171 0.6605 0.1376 0.144 Uiso 1 1 calc R . . C46 C 0.9420(8) 0.6180(8) -0.0229(17) 0.062(5) Uiso 1 1 d . . . H46A H 0.9621 0.6524 -0.0520 0.075 Uiso 1 1 calc R . . H46B H 0.9650 0.5839 -0.0428 0.075 Uiso 1 1 calc R . . C20S C 0.9453(14) 0.9772(13) 0.997(3) 0.050(7) Uiso 0.50 1 d P . . H20S H 0.9076 0.9619 1.0022 0.060 Uiso 0.50 1 calc PR . . C21S C 0.9922(14) 0.9426(14) 0.992(3) 0.049(7) Uiso 0.50 1 d P . . H21S H 0.9883 0.9026 0.9858 0.058 Uiso 0.50 1 calc PR . . C22S C 0.9537(15) 1.0314(14) 0.996(3) 0.055(8) Uiso 0.50 1 d P . . H22S H 0.9208 1.0553 0.9973 0.066 Uiso 0.50 1 calc PR . . C33S C 0.531(2) 0.5905(17) 0.447(2) 0.084(12) Uiso 0.50 1 d PD . . H33A H 0.4925 0.5946 0.4102 0.100 Uiso 0.50 1 calc PR . . H33B H 0.5554 0.6228 0.4217 0.100 Uiso 0.50 1 calc PR . . C31S C 0.559(2) 0.5338(17) 0.411(3) 0.093(14) Uiso 0.50 1 d PD . . H31A H 0.5303 0.5080 0.3726 0.112 Uiso 0.50 1 calc PR . . H31B H 0.5915 0.5395 0.3556 0.112 Uiso 0.50 1 calc PR . . C32S C 0.5780(19) 0.5118(18) 0.533(3) 0.078(11) Uiso 0.50 1 d PD . . H32A H 0.5678 0.4710 0.5362 0.094 Uiso 0.50 1 calc PR . . H32B H 0.6205 0.5139 0.5341 0.094 Uiso 0.50 1 calc PR . . O30S O 0.5571(17) 0.5381(14) 0.647(3) 0.140(14) Uiso 0.50 1 d PD . . C34S C 0.5263(8) 0.5879(7) 0.5864(16) 0.106(16) Uiso 0.50 1 d PD . . H34A H 0.5420 0.6236 0.6197 0.127 Uiso 0.50 1 calc PR . . H34B H 0.4851 0.5862 0.6082 0.127 Uiso 0.50 1 calc PR . . C40S C 0.5000(8) 1.0000(7) 0.5394(16) 0.083(17) Uiso 0.50 2 d SPRD . . H40S H 0.5000 1.0000 0.4542 0.099 Uiso 0.50 2 calc SPR . . C41S C 0.5393(8) 0.9652(7) 0.5921(16) 0.048(7) Uiso 0.50 1 d PRD . . H41S H 0.5672 0.9442 0.5486 0.057 Uiso 0.50 1 d PR . . C42S C 0.5348(8) 0.9635(7) 0.7128(16) 0.058(8) Uiso 0.50 1 d PRD . . H42S H 0.5565 0.9360 0.7558 0.070 Uiso 0.50 1 d PR . . C43S C 0.5000 1.0000 0.767(3) 0.055(11) Uiso 0.50 2 d SPD . . H43S H 0.5000 1.0000 0.8519 0.066 Uiso 0.50 2 calc SPR . . 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 0.01679(15) 0.01601(14) 0.00889(12) -0.00032(13) 0.00118(14) 0.00180(15) K1 0.0405(13) 0.0351(13) 0.0263(10) -0.0069(12) 0.0039(11) -0.0006(10) O1 0.021(4) 0.015(3) 0.013(3) 0.003(2) -0.004(2) -0.001(2) O2 0.033(5) 0.028(4) 0.008(3) -0.003(2) -0.004(2) 0.002(3) O3 0.032(4) 0.031(4) 0.016(3) 0.001(3) 0.005(3) 0.007(4) N1 0.019(4) 0.017(4) 0.011(4) 0.004(3) 0.004(3) -0.006(3) N2 0.003(4) 0.023(4) 0.028(4) 0.008(3) -0.006(3) 0.000(3) N3 0.022(4) 0.028(4) 0.007(4) -0.003(3) 0.004(3) 0.008(4) N4 0.011(3) 0.024(4) 0.006(4) 0.000(3) -0.005(3) 0.003(3) N5 0.032(5) 0.017(4) 0.011(4) -0.001(3) 0.002(3) -0.005(4) N6 0.028(5) 0.026(5) 0.012(4) 0.006(3) 0.005(4) -0.004(4) N7 0.022(4) 0.018(4) 0.011(4) 0.002(3) 0.003(3) 0.001(3) N8 0.016(4) 0.025(4) 0.013(4) 0.002(3) 0.001(3) -0.001(3) C1 0.018(5) 0.027(5) 0.019(5) 0.001(4) 0.002(4) -0.003(4) C2 0.013(5) 0.020(5) 0.016(4) 0.012(4) 0.004(3) 0.004(4) C3 0.052(7) 0.023(5) 0.015(4) -0.001(4) -0.006(6) -0.004(6) C4 0.038(7) 0.018(5) 0.022(5) -0.001(4) 0.001(5) 0.001(5) C5 0.049(7) 0.010(4) 0.011(5) 0.004(3) 0.002(4) 0.010(4) C6 0.031(6) 0.028(5) 0.016(5) 0.003(4) 0.003(4) 0.011(5) C7 0.041(7) 0.031(6) 0.022(6) 0.007(5) 0.003(5) 0.003(5) C8 0.040(7) 0.037(7) 0.039(7) 0.007(5) 0.008(6) 0.017(6) C9 0.022(5) 0.016(4) 0.017(5) -0.003(4) 0.005(4) 0.004(4) C10 0.035(6) 0.031(6) 0.020(5) 0.000(4) 0.001(5) 0.006(5) C11 0.026(5) 0.044(6) 0.014(5) -0.004(5) 0.007(4) 0.000(6) C12 0.018(5) 0.024(5) 0.019(5) 0.002(4) 0.002(4) 0.005(4) C13 0.033(5) 0.015(4) 0.015(4) 0.003(4) -0.004(4) -0.003(5) C14 0.011(4) 0.017(4) 0.014(4) -0.002(4) 0.000(4) -0.005(3) C15 0.041(7) 0.032(6) 0.012(5) 0.005(4) 0.003(5) -0.005(5) C16 0.041(7) 0.026(6) 0.024(6) 0.009(5) -0.005(5) -0.002(5) C16A 0.111(14) 0.025(6) 0.023(7) 0.007(5) 0.009(7) 0.006(7) C17 0.018(5) 0.025(5) 0.035(7) -0.002(4) 0.003(4) 0.000(4) C17A 0.051(8) 0.023(5) 0.041(6) -0.002(5) 0.000(6) 0.004(6) C18 0.028(6) 0.022(5) 0.017(5) 0.000(4) 0.002(4) -0.004(4) C19 0.022(5) 0.022(5) 0.011(4) -0.001(4) -0.008(4) -0.013(4) C20 0.027(6) 0.016(5) 0.022(5) -0.005(4) -0.002(4) -0.007(4) C21 0.030(6) 0.031(6) 0.012(5) -0.004(4) 0.002(4) -0.011(5) C22 0.048(7) 0.030(6) 0.022(6) -0.004(5) -0.001(5) -0.022(5) C26 0.028(6) 0.027(5) 0.014(5) 0.006(4) -0.004(4) 0.007(4) C27 0.026(6) 0.023(5) 0.014(4) 0.003(4) -0.003(4) 0.010(5) C28 0.020(4) 0.021(4) 0.012(4) -0.005(3) -0.001(5) 0.010(4) C29 0.042(7) 0.031(6) 0.009(4) 0.008(4) 0.007(5) -0.003(5) C30 0.024(5) 0.040(6) 0.020(5) 0.005(5) 0.007(4) -0.004(5) C31 0.018(5) 0.026(5) 0.013(5) 0.002(4) 0.001(4) 0.003(4) C32 0.020(5) 0.021(5) 0.020(5) -0.002(4) -0.001(4) -0.003(4) C33 0.025(5) 0.020(5) 0.013(4) 0.005(3) 0.001(4) 0.000(4) C34 0.018(5) 0.034(6) 0.021(5) 0.002(4) 0.008(4) -0.002(4) C35 0.016(5) 0.043(6) 0.029(6) 0.000(5) -0.003(4) 0.000(5) C35A 0.027(6) 0.063(9) 0.034(7) 0.004(6) 0.000(5) 0.009(6) C36 0.013(5) 0.056(8) 0.029(6) -0.001(5) -0.006(5) 0.000(5) C36A 0.050(10) 0.117(14) 0.020(7) 0.003(7) -0.005(6) 0.018(9) C37 0.022(5) 0.049(8) 0.012(5) -0.002(5) -0.002(4) -0.006(5) C38 0.012(4) 0.019(4) 0.018(4) 0.001(4) 0.002(4) -0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 1.787(6) . ? U1 O1 1.821(6) . ? U1 O3 2.185(8) . ? U1 N2 2.498(8) . ? U1 N3 2.520(9) . ? U1 N4 2.550(8) . ? U1 N1 2.598(8) . ? U1 K1 3.966(2) . ? K1 O3 2.575(7) . ? K1 O5 2.689(15) . ? K1 O6 2.757(14) . ? K1 N8 2.901(9) . ? K1 N5 3.027(9) . ? K1 O1 3.194(7) . ? K1 N6 3.255(10) . ? K1 N7 3.266(9) . ? K1 C43 3.35(2) . ? K1 C20 3.472(11) . ? K1 C32 3.510(10) . ? K1 C21 3.530(12) . ? O3 H300 0.9300 . ? N1 C1 1.281(13) . ? N1 C38 1.422(12) . ? N2 C5 1.367(14) . ? N2 C2 1.369(13) . ? N3 C9 1.340(13) . ? N3 C12 1.376(14) . ? N4 C13 1.307(13) . ? N4 C14 1.409(11) . ? N5 C20 1.290(13) . ? N5 C19 1.417(12) . ? N6 C21 1.361(13) . ? N6 C24 1.401(13) . ? N6 H6 0.8600 . ? N7 C28 1.382(12) . ? N7 C31 1.383(13) . ? N7 H7 0.8600 . ? N8 C32 1.288(13) . ? N8 C33 1.406(13) . ? C1 C2 1.417(14) . ? C1 H1 0.9300 . ? C2 C3 1.402(15) . ? C3 C4 1.338(18) . ? C3 H3 0.9300 . ? C4 C5 1.407(16) . ? C4 H4 0.9300 . ? C5 C6 1.510(17) . ? C6 C8 1.505(16) . ? C6 C9 1.518(15) . ? C6 C7 1.545(15) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.381(16) . ? C10 C11 1.403(19) . ? C10 H10 0.9300 . ? C11 C12 1.391(15) . ? C11 H11 0.9300 . ? C12 C13 1.416(15) . ? C13 H13 0.9300 . ? C14 C15 1.398(14) . ? C14 C19 1.409(14) . ? C15 C16 1.403(17) . ? C15 H15 0.9300 . ? C16 C17 1.388(16) . ? C16 C16A 1.523(15) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17 C18 1.384(15) . ? C17 C17A 1.510(15) . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18 C19 1.391(15) . ? C18 H18 0.9300 . ? C20 C21 1.426(15) . ? C20 H20 0.9300 . ? C21 C22 1.381(16) . ? C22 C23 1.399(16) . ? C22 H22 0.9300 . ? C23 C24 1.382(14) . ? C23 H23 0.9300 . ? C24 C25 1.483(12) . ? C25 C26 1.514(13) . ? C25 C28 1.529(13) . ? C25 C27 1.529(13) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.379(15) . ? C29 C30 1.408(17) . ? C29 H29 0.9300 . ? C30 C31 1.376(14) . ? C30 H30 0.9300 . ? C31 C32 1.437(14) . ? C32 H32 0.9300 . ? C33 C34 1.356(15) . ? C33 C38 1.403(14) . ? C34 C35 1.398(15) . ? C34 H34 0.9300 . ? C35 C36 1.427(16) . ? C35 C35A 1.497(17) . ? C35A H35A 0.9600 . ? C35A H35B 0.9600 . ? C35A H35C 0.9600 . ? C36 C37 1.386(17) . ? C36 C36A 1.510(17) . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37 C38 1.374(15) . ? C37 H37 0.9300 . ? O5 C42 1.38(3) . ? O5 C39 1.41(3) . ? C39 C40 1.39(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.48(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.57(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? O6 C43 1.39(2) . ? O6 C46 1.43(2) . ? C43 C44 1.37(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.45(3) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.53(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C20S C22S 1.27(4) . ? C20S C21S 1.33(4) . ? C20S H20S 0.9300 . ? C21S C22S 1.37(5) 4_775 ? C21S H21S 0.9300 . ? C22S C21S 1.37(5) 4_775 ? C22S H22S 0.9300 . ? C33S C31S 1.504(19) . ? C33S C34S 1.525(19) . ? C33S H33A 0.9700 . ? C33S H33B 0.9700 . ? C31S C32S 1.495(19) . ? C31S H31A 0.9700 . ? C31S H31B 0.9700 . ? C32S O30S 1.463(19) . ? C32S H32A 0.9700 . ? C32S H32B 0.9700 . ? O30S C34S 1.500(19) . ? C34S H34A 0.9700 . ? C34S H34B 0.9700 . ? C40S C41S 1.3333 . ? C40S C41S 1.33(3) 4_675 ? C40S H40S 0.9300 . ? C41S C42S 1.3218 . ? C41S H41S 0.9300 . ? C42S C43S 1.298(13) . ? C42S H42S 0.9300 . ? C43S C42S 1.298(13) 4_675 ? C43S H43S 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O1 178.6(3) . . ? O2 U1 O3 89.5(3) . . ? O1 U1 O3 89.1(3) . . ? O2 U1 N2 87.4(3) . . ? O1 U1 N2 93.7(3) . . ? O3 U1 N2 144.0(3) . . ? O2 U1 N3 87.0(3) . . ? O1 U1 N3 94.2(3) . . ? O3 U1 N3 145.6(3) . . ? N2 U1 N3 70.0(3) . . ? O2 U1 N4 83.7(3) . . ? O1 U1 N4 96.2(3) . . ? O3 U1 N4 80.0(3) . . ? N2 U1 N4 135.0(3) . . ? N3 U1 N4 65.6(3) . . ? O2 U1 N1 82.4(3) . . ? O1 U1 N1 97.2(3) . . ? O3 U1 N1 78.6(3) . . ? N2 U1 N1 65.5(3) . . ? N3 U1 N1 134.6(3) . . ? N4 U1 N1 154.5(2) . . ? O2 U1 K1 126.3(2) . . ? O1 U1 K1 52.3(2) . . ? O3 U1 K1 36.83(18) . . ? N2 U1 K1 131.7(2) . . ? N3 U1 K1 135.17(19) . . ? N4 U1 K1 87.11(17) . . ? N1 U1 K1 84.04(18) . . ? O3 K1 O5 166.5(3) . . ? O3 K1 O6 84.2(3) . . ? O5 K1 O6 83.5(4) . . ? O3 K1 N8 75.0(3) . . ? O5 K1 N8 103.5(3) . . ? O6 K1 N8 107.4(3) . . ? O3 K1 N5 72.1(2) . . ? O5 K1 N5 116.0(3) . . ? O6 K1 N5 102.1(3) . . ? N8 K1 N5 132.7(2) . . ? O3 K1 O1 57.4(2) . . ? O5 K1 O1 135.0(3) . . ? O6 K1 O1 141.5(3) . . ? N8 K1 O1 68.0(2) . . ? N5 K1 O1 65.8(2) . . ? O3 K1 N6 105.4(2) . . ? O5 K1 N6 87.8(3) . . ? O6 K1 N6 145.3(3) . . ? N8 K1 N6 107.4(2) . . ? N5 K1 N6 52.6(2) . . ? O1 K1 N6 56.5(2) . . ? O3 K1 N7 106.5(2) . . ? O5 K1 N7 82.1(3) . . ? O6 K1 N7 151.2(3) . . ? N8 K1 N7 52.8(2) . . ? N5 K1 N7 106.6(2) . . ? O1 K1 N7 56.99(18) . . ? N6 K1 N7 58.7(2) . . ? O3 K1 C43 67.5(4) . . ? O5 K1 C43 102.3(5) . . ? O6 K1 C43 24.0(5) . . ? N8 K1 C43 116.4(4) . . ? N5 K1 C43 80.5(4) . . ? O1 K1 C43 121.4(4) . . ? N6 K1 C43 130.7(4) . . ? N7 K1 C43 169.3(4) . . ? O3 K1 C20 93.6(3) . . ? O5 K1 C20 94.9(3) . . ? O6 K1 C20 105.2(3) . . ? N8 K1 C20 144.0(3) . . ? N5 K1 C20 21.5(2) . . ? O1 K1 C20 77.0(2) . . ? N6 K1 C20 42.1(2) . . ? N7 K1 C20 100.8(2) . . ? C43 K1 C20 88.7(4) . . ? O3 K1 C32 95.4(3) . . ? O5 K1 C32 84.0(3) . . ? O6 K1 C32 111.5(3) . . ? N8 K1 C32 20.5(2) . . ? N5 K1 C32 142.8(2) . . ? O1 K1 C32 77.9(2) . . ? N6 K1 C32 100.9(2) . . ? N7 K1 C32 42.2(2) . . ? C43 K1 C32 127.9(4) . . ? C20 K1 C32 142.9(3) . . ? O3 K1 C21 109.5(3) . . ? O5 K1 C21 81.9(3) . . ? O6 K1 C21 122.6(3) . . ? N8 K1 C21 130.0(3) . . ? N5 K1 C21 41.4(2) . . ? O1 K1 C21 73.7(2) . . ? N6 K1 C21 22.7(2) . . ? N7 K1 C21 79.7(2) . . ? C43 K1 C21 110.5(4) . . ? C20 K1 C21 23.5(2) . . ? C32 K1 C21 121.6(3) . . ? U1 O1 K1 100.9(2) . . ? U1 O3 K1 112.6(3) . . ? U1 O3 H300 123.7 . . ? K1 O3 H300 123.7 . . ? C1 N1 C38 118.2(9) . . ? C1 N1 U1 114.2(7) . . ? C38 N1 U1 125.3(6) . . ? C5 N2 C2 106.8(8) . . ? C5 N2 U1 136.3(7) . . ? C2 N2 U1 115.2(6) . . ? C9 N3 C12 106.7(8) . . ? C9 N3 U1 137.5(7) . . ? C12 N3 U1 114.4(6) . . ? C13 N4 C14 114.3(8) . . ? C13 N4 U1 115.9(7) . . ? C14 N4 U1 126.9(5) . . ? C20 N5 C19 121.8(8) . . ? C20 N5 K1 99.1(6) . . ? C19 N5 K1 112.3(6) . . ? C21 N6 C24 109.9(9) . . ? C21 N6 K1 90.1(7) . . ? C24 N6 K1 122.8(6) . . ? C21 N6 H6 125.1 . . ? C24 N6 H6 125.1 . . ? K1 N6 H6 61.8 . . ? C28 N7 C31 110.8(8) . . ? C28 N7 K1 126.1(6) . . ? C31 N7 K1 94.9(6) . . ? C28 N7 H7 124.6 . . ? C31 N7 H7 124.6 . . ? K1 N7 H7 53.6 . . ? C32 N8 C33 120.2(9) . . ? C32 N8 K1 107.5(6) . . ? C33 N8 K1 108.3(6) . . ? N1 C1 C2 120.9(10) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? N2 C2 C3 109.0(10) . . ? N2 C2 C1 119.8(9) . . ? C3 C2 C1 131.2(11) . . ? C4 C3 C2 107.5(11) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? C3 C4 C5 108.0(11) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? N2 C5 C4 108.6(11) . . ? N2 C5 C6 121.9(9) . . ? C4 C5 C6 129.5(10) . . ? C8 C6 C5 110.3(10) . . ? C8 C6 C9 110.2(9) . . ? C5 C6 C9 112.2(8) . . ? C8 C6 C7 107.5(9) . . ? C5 C6 C7 108.9(9) . . ? C9 C6 C7 107.7(9) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 110.0(9) . . ? N3 C9 C6 120.9(9) . . ? C10 C9 C6 129.1(9) . . ? C9 C10 C11 108.1(10) . . ? C9 C10 H10 125.9 . . ? C11 C10 H10 125.9 . . ? C12 C11 C10 104.4(10) . . ? C12 C11 H11 127.8 . . ? C10 C11 H11 127.8 . . ? N3 C12 C11 110.8(10) . . ? N3 C12 C13 119.9(9) . . ? C11 C12 C13 129.2(11) . . ? N4 C13 C12 119.5(10) . . ? N4 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 N4 121.6(9) . . ? C15 C14 C19 117.7(9) . . ? N4 C14 C19 120.6(9) . . ? C14 C15 C16 121.2(10) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 120.0(10) . . ? C17 C16 C16A 120.8(11) . . ? C15 C16 C16A 119.0(11) . . ? C16 C16A H16A 109.5 . . ? C16 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C16 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C18 C17 C16 119.3(10) . . ? C18 C17 C17A 118.3(10) . . ? C16 C17 C17A 122.3(10) . . ? C17 C17A H17A 109.5 . . ? C17 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C17 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C17 C18 C19 121.1(10) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 120.4(9) . . ? C18 C19 N5 123.2(9) . . ? C14 C19 N5 116.3(9) . . ? N5 C20 C21 120.8(9) . . ? N5 C20 K1 59.4(5) . . ? C21 C20 K1 80.5(6) . . ? N5 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? K1 C20 H20 133.0 . . ? N6 C21 C22 106.5(10) . . ? N6 C21 C20 120.9(10) . . ? C22 C21 C20 132.5(10) . . ? N6 C21 K1 67.2(6) . . ? C22 C21 K1 129.0(9) . . ? C20 C21 K1 76.0(6) . . ? C21 C22 C23 109.7(10) . . ? C21 C22 H22 125.2 . . ? C23 C22 H22 125.2 . . ? C24 C23 C22 106.6(10) . . ? C24 C23 H23 126.7 . . ? C22 C23 H23 126.7 . . ? C23 C24 N6 107.1(8) . . ? C23 C24 C25 131.7(10) . . ? N6 C24 C25 121.1(9) . . ? C24 C25 C26 109.4(9) . . ? C24 C25 C28 109.1(8) . . ? C26 C25 C28 108.2(8) . . ? C24 C25 C27 111.1(8) . . ? C26 C25 C27 109.7(8) . . ? C28 C25 C27 109.3(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N7 105.8(9) . . ? C29 C28 C25 131.6(9) . . ? N7 C28 C25 122.4(9) . . ? C28 C29 C30 108.9(9) . . ? C28 C29 H29 125.6 . . ? C30 C29 H29 125.6 . . ? C31 C30 C29 107.9(10) . . ? C31 C30 H30 126.1 . . ? C29 C30 H30 126.1 . . ? C30 C31 N7 106.5(9) . . ? C30 C31 C32 132.5(10) . . ? N7 C31 C32 120.7(9) . . ? N8 C32 C31 118.7(9) . . ? N8 C32 K1 52.0(5) . . ? C31 C32 K1 84.1(6) . . ? N8 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? K1 C32 H32 134.8 . . ? C34 C33 C38 118.3(9) . . ? C34 C33 N8 123.9(9) . . ? C38 C33 N8 117.7(9) . . ? C33 C34 C35 123.5(10) . . ? C33 C34 H34 118.2 . . ? C35 C34 H34 118.2 . . ? C34 C35 C36 118.1(10) . . ? C34 C35 C35A 121.5(11) . . ? C36 C35 C35A 120.3(10) . . ? C35 C35A H35A 109.5 . . ? C35 C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C35 C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C37 C36 C35 117.2(10) . . ? C37 C36 C36A 121.0(11) . . ? C35 C36 C36A 121.7(11) . . ? C36 C36A H36A 109.5 . . ? C36 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C36 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C38 C37 C36 123.2(10) . . ? C38 C37 H37 118.4 . . ? C36 C37 H37 118.4 . . ? C37 C38 C33 119.4(9) . . ? C37 C38 N1 121.4(10) . . ? C33 C38 N1 119.0(9) . . ? C42 O5 C39 102.0(19) . . ? C42 O5 K1 129.1(16) . . ? C39 O5 K1 128.9(13) . . ? C40 C39 O5 110(2) . . ? C40 C39 H39A 109.6 . . ? O5 C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? O5 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C39 C40 C41 103(2) . . ? C39 C40 H40A 111.1 . . ? C41 C40 H40A 111.1 . . ? C39 C40 H40B 111.1 . . ? C41 C40 H40B 111.1 . . ? H40A C40 H40B 109.0 . . ? C40 C41 C42 99(3) . . ? C40 C41 H41A 111.9 . . ? C42 C41 H41A 111.9 . . ? C40 C41 H41B 111.9 . . ? C42 C41 H41B 111.9 . . ? H41A C41 H41B 109.6 . . ? O5 C42 C41 98(3) . . ? O5 C42 H42A 112.1 . . ? C41 C42 H42A 112.1 . . ? O5 C42 H42B 112.1 . . ? C41 C42 H42B 112.1 . . ? H42A C42 H42B 109.8 . . ? C43 O6 C46 105.1(15) . . ? C43 O6 K1 102.4(12) . . ? C46 O6 K1 127.4(11) . . ? C44 C43 O6 114(2) . . ? C44 C43 K1 131.5(18) . . ? O6 C43 K1 53.6(10) . . ? C44 C43 H43A 108.8 . . ? O6 C43 H43A 108.8 . . ? K1 C43 H43A 55.2 . . ? C44 C43 H43B 108.8 . . ? O6 C43 H43B 108.8 . . ? K1 C43 H43B 119.6 . . ? H43A C43 H43B 107.6 . . ? C43 C44 C45 102(3) . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44B 111.4 . . ? C45 C44 H44B 111.4 . . ? H44A C44 H44B 109.2 . . ? C44 C45 C46 103(2) . . ? C44 C45 H45A 111.1 . . ? C46 C45 H45A 111.1 . . ? C44 C45 H45B 111.1 . . ? C46 C45 H45B 111.1 . . ? H45A C45 H45B 109.1 . . ? O6 C46 C45 100.2(17) . . ? O6 C46 H46A 111.7 . . ? C45 C46 H46A 111.7 . . ? O6 C46 H46B 111.7 . . ? C45 C46 H46B 111.7 . . ? H46A C46 H46B 109.5 . . ? C22S C20S C21S 118(3) . . ? C22S C20S H20S 120.9 . . ? C21S C20S H20S 120.9 . . ? C20S C21S C22S 117(3) . 4_775 ? C20S C21S H21S 121.4 . . ? C22S C21S H21S 121.4 4_775 . ? C20S C22S C21S 125(3) . 4_775 ? C20S C22S H22S 117.7 . . ? C21S C22S H22S 117.7 4_775 . ? C31S C33S C34S 105(3) . . ? C31S C33S H33A 110.7 . . ? C34S C33S H33A 110.7 . . ? C31S C33S H33B 110.7 . . ? C34S C33S H33B 110.7 . . ? H33A C33S H33B 108.8 . . ? C32S C31S C33S 101(3) . . ? C32S C31S H31A 111.7 . . ? C33S C31S H31A 111.7 . . ? C32S C31S H31B 111.7 . . ? C33S C31S H31B 111.7 . . ? H31A C31S H31B 109.4 . . ? O30S C32S C31S 121(3) . . ? O30S C32S H32A 107.0 . . ? C31S C32S H32A 107.0 . . ? O30S C32S H32B 107.0 . . ? C31S C32S H32B 107.0 . . ? H32A C32S H32B 106.7 . . ? C32S O30S C34S 95(3) . . ? O30S C34S C33S 116(2) . . ? O30S C34S H34A 108.3 . . ? C33S C34S H34A 108.3 . . ? O30S C34S H34B 108.3 . . ? C33S C34S H34B 108.3 . . ? H34A C34S H34B 107.4 . . ? C41S C40S C41S 128.9(6) . 4_675 ? C41S C40S H40S 115.6 . . ? C41S C40S H40S 115.6 4_675 . ? C42S C41S C40S 113.3 . . ? C42S C41S H41S 123.2 . . ? C40S C41S H41S 123.5 . . ? C43S C42S C41S 118.7(12) . . ? C43S C42S H42S 122.5 . . ? C41S C42S H42S 118.8 . . ? C42S C43S C42S 126(2) 4_675 . ? C42S C43S H43S 117.0 4_675 . ? C42S C43S H43S 117.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O1 K1 3(13) . . . . ? O3 U1 O1 K1 -1.7(3) . . . . ? N2 U1 O1 K1 142.4(2) . . . . ? N3 U1 O1 K1 -147.4(3) . . . . ? N4 U1 O1 K1 -81.5(2) . . . . ? N1 U1 O1 K1 76.7(2) . . . . ? O3 K1 O1 U1 1.7(3) . . . . ? O5 K1 O1 U1 -171.4(4) . . . . ? O6 K1 O1 U1 6.4(6) . . . . ? N8 K1 O1 U1 -84.1(3) . . . . ? N5 K1 O1 U1 85.2(3) . . . . ? N6 K1 O1 U1 145.1(3) . . . . ? N7 K1 O1 U1 -143.2(3) . . . . ? C43 K1 O1 U1 24.2(6) . . . . ? C20 K1 O1 U1 104.6(3) . . . . ? C32 K1 O1 U1 -103.0(3) . . . . ? C21 K1 O1 U1 128.6(3) . . . . ? O2 U1 O3 K1 -177.7(4) . . . . ? O1 U1 O3 K1 2.2(4) . . . . ? N2 U1 O3 K1 -92.9(5) . . . . ? N3 U1 O3 K1 98.3(5) . . . . ? N4 U1 O3 K1 98.6(3) . . . . ? N1 U1 O3 K1 -95.3(4) . . . . ? O5 K1 O3 U1 157.1(14) . . . . ? O6 K1 O3 U1 -178.5(4) . . . . ? N8 K1 O3 U1 71.7(4) . . . . ? N5 K1 O3 U1 -73.8(3) . . . . ? O1 K1 O3 U1 -1.5(2) . . . . ? N6 K1 O3 U1 -32.5(4) . . . . ? N7 K1 O3 U1 28.7(4) . . . . ? C43 K1 O3 U1 -160.8(6) . . . . ? C20 K1 O3 U1 -73.6(4) . . . . ? C32 K1 O3 U1 70.3(4) . . . . ? C21 K1 O3 U1 -56.0(4) . . . . ? O2 U1 N1 C1 -73.2(7) . . . . ? O1 U1 N1 C1 108.2(7) . . . . ? O3 U1 N1 C1 -164.2(7) . . . . ? N2 U1 N1 C1 17.3(6) . . . . ? N3 U1 N1 C1 5.0(8) . . . . ? N4 U1 N1 C1 -130.8(7) . . . . ? K1 U1 N1 C1 158.9(7) . . . . ? O2 U1 N1 C38 89.2(8) . . . . ? O1 U1 N1 C38 -89.4(8) . . . . ? O3 U1 N1 C38 -1.9(7) . . . . ? N2 U1 N1 C38 179.7(8) . . . . ? N3 U1 N1 C38 167.4(7) . . . . ? N4 U1 N1 C38 31.6(11) . . . . ? K1 U1 N1 C38 -38.7(7) . . . . ? O2 U1 N2 C5 -96.2(9) . . . . ? O1 U1 N2 C5 84.7(9) . . . . ? O3 U1 N2 C5 178.3(8) . . . . ? N3 U1 N2 C5 -8.4(9) . . . . ? N4 U1 N2 C5 -17.8(11) . . . . ? N1 U1 N2 C5 -179.1(10) . . . . ? K1 U1 N2 C5 125.0(9) . . . . ? O2 U1 N2 C2 66.5(7) . . . . ? O1 U1 N2 C2 -112.6(7) . . . . ? O3 U1 N2 C2 -19.0(9) . . . . ? N3 U1 N2 C2 154.3(7) . . . . ? N4 U1 N2 C2 144.8(6) . . . . ? N1 U1 N2 C2 -16.4(6) . . . . ? K1 U1 N2 C2 -72.4(7) . . . . ? O2 U1 N3 C9 96.6(10) . . . . ? O1 U1 N3 C9 -84.1(10) . . . . ? O3 U1 N3 C9 -178.7(8) . . . . ? N2 U1 N3 C9 8.3(9) . . . . ? N4 U1 N3 C9 -179.0(10) . . . . ? N1 U1 N3 C9 20.3(11) . . . . ? K1 U1 N3 C9 -121.4(9) . . . . ? O2 U1 N3 C12 -67.5(7) . . . . ? O1 U1 N3 C12 111.7(7) . . . . ? O3 U1 N3 C12 17.2(9) . . . . ? N2 U1 N3 C12 -155.8(7) . . . . ? N4 U1 N3 C12 16.9(6) . . . . ? N1 U1 N3 C12 -143.8(6) . . . . ? K1 U1 N3 C12 74.5(7) . . . . ? O2 U1 N4 C13 71.5(6) . . . . ? O1 U1 N4 C13 -109.9(6) . . . . ? O3 U1 N4 C13 162.1(7) . . . . ? N2 U1 N4 C13 -8.4(8) . . . . ? N3 U1 N4 C13 -18.1(6) . . . . ? N1 U1 N4 C13 128.8(7) . . . . ? K1 U1 N4 C13 -161.5(6) . . . . ? O2 U1 N4 C14 -88.1(7) . . . . ? O1 U1 N4 C14 90.5(7) . . . . ? O3 U1 N4 C14 2.5(7) . . . . ? N2 U1 N4 C14 -168.0(7) . . . . ? N3 U1 N4 C14 -177.7(8) . . . . ? N1 U1 N4 C14 -30.8(10) . . . . ? K1 U1 N4 C14 38.9(7) . . . . ? O3 K1 N5 C20 179.5(7) . . . . ? O5 K1 N5 C20 -12.1(8) . . . . ? O6 K1 N5 C20 -100.7(7) . . . . ? N8 K1 N5 C20 131.4(6) . . . . ? O1 K1 N5 C20 117.9(7) . . . . ? N6 K1 N5 C20 52.7(6) . . . . ? N7 K1 N5 C20 77.1(7) . . . . ? C43 K1 N5 C20 -111.2(8) . . . . ? C32 K1 N5 C20 104.7(7) . . . . ? C21 K1 N5 C20 25.4(6) . . . . ? O3 K1 N5 C19 -50.5(6) . . . . ? O5 K1 N5 C19 117.9(7) . . . . ? O6 K1 N5 C19 29.3(7) . . . . ? N8 K1 N5 C19 -98.6(7) . . . . ? O1 K1 N5 C19 -112.1(6) . . . . ? N6 K1 N5 C19 -177.4(7) . . . . ? N7 K1 N5 C19 -153.0(6) . . . . ? C43 K1 N5 C19 18.8(7) . . . . ? C20 K1 N5 C19 130.0(10) . . . . ? C32 K1 N5 C19 -125.4(6) . . . . ? C21 K1 N5 C19 155.4(8) . . . . ? O3 K1 N6 C21 -103.8(7) . . . . ? O5 K1 N6 C21 73.9(7) . . . . ? O6 K1 N6 C21 -1.4(9) . . . . ? N8 K1 N6 C21 177.4(6) . . . . ? N5 K1 N6 C21 -51.7(6) . . . . ? O1 K1 N6 C21 -135.2(7) . . . . ? N7 K1 N6 C21 156.0(7) . . . . ? C43 K1 N6 C21 -30.4(9) . . . . ? C20 K1 N6 C21 -25.9(6) . . . . ? C32 K1 N6 C21 157.4(6) . . . . ? O3 K1 N6 C24 142.2(7) . . . . ? O5 K1 N6 C24 -40.0(8) . . . . ? O6 K1 N6 C24 -115.3(8) . . . . ? N8 K1 N6 C24 63.5(8) . . . . ? N5 K1 N6 C24 -165.6(8) . . . . ? O1 K1 N6 C24 110.8(8) . . . . ? N7 K1 N6 C24 42.1(7) . . . . ? C43 K1 N6 C24 -144.4(8) . . . . ? C20 K1 N6 C24 -139.8(9) . . . . ? C32 K1 N6 C24 43.4(8) . . . . ? C21 K1 N6 C24 -113.9(11) . . . . ? O3 K1 N7 C28 -137.7(7) . . . . ? O5 K1 N7 C28 52.9(8) . . . . ? O6 K1 N7 C28 113.5(9) . . . . ? N8 K1 N7 C28 166.5(8) . . . . ? N5 K1 N7 C28 -62.0(8) . . . . ? O1 K1 N7 C28 -107.4(8) . . . . ? N6 K1 N7 C28 -39.4(7) . . . . ? C43 K1 N7 C28 168(2) . . . . ? C20 K1 N7 C28 -40.7(8) . . . . ? C32 K1 N7 C28 142.6(9) . . . . ? C21 K1 N7 C28 -30.2(7) . . . . ? O3 K1 N7 C31 102.0(6) . . . . ? O5 K1 N7 C31 -67.3(6) . . . . ? O6 K1 N7 C31 -6.7(9) . . . . ? N8 K1 N7 C31 46.3(6) . . . . ? N5 K1 N7 C31 177.7(6) . . . . ? O1 K1 N7 C31 132.4(6) . . . . ? N6 K1 N7 C31 -159.6(6) . . . . ? C43 K1 N7 C31 47(2) . . . . ? C20 K1 N7 C31 -160.9(6) . . . . ? C32 K1 N7 C31 22.4(5) . . . . ? C21 K1 N7 C31 -150.5(6) . . . . ? O3 K1 N8 C32 -176.0(7) . . . . ? O5 K1 N8 C32 17.8(8) . . . . ? O6 K1 N8 C32 105.1(7) . . . . ? N5 K1 N8 C32 -128.9(7) . . . . ? O1 K1 N8 C32 -115.6(7) . . . . ? N6 K1 N8 C32 -74.2(7) . . . . ? N7 K1 N8 C32 -51.2(7) . . . . ? C43 K1 N8 C32 129.1(8) . . . . ? C20 K1 N8 C32 -101.0(8) . . . . ? C21 K1 N8 C32 -72.9(8) . . . . ? O3 K1 N8 C33 52.6(6) . . . . ? O5 K1 N8 C33 -113.5(7) . . . . ? O6 K1 N8 C33 -26.3(7) . . . . ? N5 K1 N8 C33 99.8(7) . . . . ? O1 K1 N8 C33 113.1(6) . . . . ? N6 K1 N8 C33 154.5(6) . . . . ? N7 K1 N8 C33 177.5(7) . . . . ? C43 K1 N8 C33 -2.3(8) . . . . ? C20 K1 N8 C33 127.7(6) . . . . ? C32 K1 N8 C33 -131.3(11) . . . . ? C21 K1 N8 C33 155.8(6) . . . . ? C38 N1 C1 C2 179.3(9) . . . . ? U1 N1 C1 C2 -17.0(11) . . . . ? C5 N2 C2 C3 2.6(10) . . . . ? U1 N2 C2 C3 -165.0(6) . . . . ? C5 N2 C2 C1 -176.5(9) . . . . ? U1 N2 C2 C1 15.9(11) . . . . ? N1 C1 C2 N2 1.3(14) . . . . ? N1 C1 C2 C3 -177.5(10) . . . . ? N2 C2 C3 C4 -3.2(12) . . . . ? C1 C2 C3 C4 175.7(10) . . . . ? C2 C3 C4 C5 2.6(12) . . . . ? C2 N2 C5 C4 -1.0(11) . . . . ? U1 N2 C5 C4 162.7(7) . . . . ? C2 N2 C5 C6 177.2(9) . . . . ? U1 N2 C5 C6 -19.2(14) . . . . ? C3 C4 C5 N2 -1.0(12) . . . . ? C3 C4 C5 C6 -179.0(10) . . . . ? N2 C5 C6 C8 174.8(9) . . . . ? C4 C5 C6 C8 -7.5(15) . . . . ? N2 C5 C6 C9 51.6(12) . . . . ? C4 C5 C6 C9 -130.7(11) . . . . ? N2 C5 C6 C7 -67.5(12) . . . . ? C4 C5 C6 C7 110.2(12) . . . . ? C12 N3 C9 C10 1.3(12) . . . . ? U1 N3 C9 C10 -163.7(8) . . . . ? C12 N3 C9 C6 -175.8(9) . . . . ? U1 N3 C9 C6 19.3(15) . . . . ? C8 C6 C9 N3 -174.5(10) . . . . ? C5 C6 C9 N3 -51.3(12) . . . . ? C7 C6 C9 N3 68.5(12) . . . . ? C8 C6 C9 C10 9.0(16) . . . . ? C5 C6 C9 C10 132.3(12) . . . . ? C7 C6 C9 C10 -107.9(12) . . . . ? N3 C9 C10 C11 -0.1(12) . . . . ? C6 C9 C10 C11 176.7(10) . . . . ? C9 C10 C11 C12 -1.1(12) . . . . ? C9 N3 C12 C11 -2.0(12) . . . . ? U1 N3 C12 C11 166.8(7) . . . . ? C9 N3 C12 C13 174.9(9) . . . . ? U1 N3 C12 C13 -16.2(12) . . . . ? C10 C11 C12 N3 2.0(12) . . . . ? C10 C11 C12 C13 -174.7(11) . . . . ? C14 N4 C13 C12 179.8(9) . . . . ? U1 N4 C13 C12 17.6(11) . . . . ? N3 C12 C13 N4 -1.0(14) . . . . ? C11 C12 C13 N4 175.4(10) . . . . ? C13 N4 C14 C15 -57.7(12) . . . . ? U1 N4 C14 C15 102.2(10) . . . . ? C13 N4 C14 C19 126.1(9) . . . . ? U1 N4 C14 C19 -74.0(10) . . . . ? N4 C14 C15 C16 179.2(10) . . . . ? C19 C14 C15 C16 -4.6(16) . . . . ? C14 C15 C16 C17 1.9(19) . . . . ? C14 C15 C16 C16A 176.8(12) . . . . ? C15 C16 C17 C18 0.9(18) . . . . ? C16A C16 C17 C18 -173.8(13) . . . . ? C15 C16 C17 C17A 179.2(12) . . . . ? C16A C16 C17 C17A 4.4(19) . . . . ? C16 C17 C18 C19 -1.0(16) . . . . ? C17A C17 C18 C19 -179.4(11) . . . . ? C17 C18 C19 C14 -1.7(16) . . . . ? C17 C18 C19 N5 176.0(10) . . . . ? C15 C14 C19 C18 4.4(14) . . . . ? N4 C14 C19 C18 -179.3(9) . . . . ? C15 C14 C19 N5 -173.4(10) . . . . ? N4 C14 C19 N5 2.9(13) . . . . ? C20 N5 C19 C18 34.2(16) . . . . ? K1 N5 C19 C18 -82.8(11) . . . . ? C20 N5 C19 C14 -148.0(10) . . . . ? K1 N5 C19 C14 95.0(9) . . . . ? C19 N5 C20 C21 -178.2(10) . . . . ? K1 N5 C20 C21 -54.9(11) . . . . ? C19 N5 C20 K1 -123.4(11) . . . . ? O3 K1 C20 N5 -0.5(7) . . . . ? O5 K1 C20 N5 169.1(7) . . . . ? O6 K1 C20 N5 84.5(7) . . . . ? N8 K1 C20 N5 -69.7(8) . . . . ? O1 K1 C20 N5 -55.8(6) . . . . ? N6 K1 C20 N5 -109.6(7) . . . . ? N7 K1 C20 N5 -108.0(6) . . . . ? C43 K1 C20 N5 66.9(7) . . . . ? C32 K1 C20 N5 -104.4(7) . . . . ? C21 K1 C20 N5 -134.6(10) . . . . ? O3 K1 C20 C21 134.1(6) . . . . ? O5 K1 C20 C21 -56.3(7) . . . . ? O6 K1 C20 C21 -140.9(7) . . . . ? N8 K1 C20 C21 64.9(8) . . . . ? N5 K1 C20 C21 134.6(10) . . . . ? O1 K1 C20 C21 78.8(6) . . . . ? N6 K1 C20 C21 25.0(6) . . . . ? N7 K1 C20 C21 26.6(7) . . . . ? C43 K1 C20 C21 -158.5(7) . . . . ? C32 K1 C20 C21 30.2(8) . . . . ? C24 N6 C21 C22 -0.8(14) . . . . ? K1 N6 C21 C22 -126.0(10) . . . . ? C24 N6 C21 C20 -178.7(10) . . . . ? K1 N6 C21 C20 56.1(11) . . . . ? C24 N6 C21 K1 125.2(8) . . . . ? N5 C20 C21 N6 -6.6(18) . . . . ? K1 C20 C21 N6 -52.1(11) . . . . ? N5 C20 C21 C22 176.2(14) . . . . ? K1 C20 C21 C22 130.7(15) . . . . ? N5 C20 C21 K1 45.5(10) . . . . ? O3 K1 C21 N6 83.3(7) . . . . ? O5 K1 C21 N6 -104.1(7) . . . . ? O6 K1 C21 N6 179.1(6) . . . . ? N8 K1 C21 N6 -3.2(8) . . . . ? N5 K1 C21 N6 109.5(8) . . . . ? O1 K1 C21 N6 37.7(6) . . . . ? N7 K1 C21 N6 -20.7(6) . . . . ? C43 K1 C21 N6 155.8(7) . . . . ? C20 K1 C21 N6 132.8(10) . . . . ? C32 K1 C21 N6 -26.3(7) . . . . ? O3 K1 C21 C22 176.6(10) . . . . ? O5 K1 C21 C22 -10.8(11) . . . . ? O6 K1 C21 C22 -87.7(11) . . . . ? N8 K1 C21 C22 90.0(11) . . . . ? N5 K1 C21 C22 -157.3(13) . . . . ? O1 K1 C21 C22 131.0(11) . . . . ? N6 K1 C21 C22 93.3(12) . . . . ? N7 K1 C21 C22 72.6(11) . . . . ? C43 K1 C21 C22 -110.9(11) . . . . ? C20 K1 C21 C22 -134.0(14) . . . . ? C32 K1 C21 C22 66.9(11) . . . . ? O3 K1 C21 C20 -49.5(7) . . . . ? O5 K1 C21 C20 123.2(7) . . . . ? O6 K1 C21 C20 46.3(7) . . . . ? N8 K1 C21 C20 -136.0(6) . . . . ? N5 K1 C21 C20 -23.3(6) . . . . ? O1 K1 C21 C20 -95.0(6) . . . . ? N6 K1 C21 C20 -132.8(10) . . . . ? N7 K1 C21 C20 -153.5(6) . . . . ? C43 K1 C21 C20 23.1(8) . . . . ? C32 K1 C21 C20 -159.1(6) . . . . ? N6 C21 C22 C23 3.1(16) . . . . ? C20 C21 C22 C23 -179.4(13) . . . . ? K1 C21 C22 C23 -70.7(15) . . . . ? C21 C22 C23 C24 -4.1(15) . . . . ? C22 C23 C24 N6 3.5(13) . . . . ? C22 C23 C24 C25 -179.1(11) . . . . ? C21 N6 C24 C23 -1.7(13) . . . . ? K1 N6 C24 C23 101.8(9) . . . . ? C21 N6 C24 C25 -179.4(10) . . . . ? K1 N6 C24 C25 -75.8(10) . . . . ? C23 C24 C25 C26 15.0(15) . . . . ? N6 C24 C25 C26 -168.0(9) . . . . ? C23 C24 C25 C28 -103.2(12) . . . . ? N6 C24 C25 C28 73.8(12) . . . . ? C23 C24 C25 C27 136.2(12) . . . . ? N6 C24 C25 C27 -46.7(12) . . . . ? C31 N7 C28 C29 3.1(11) . . . . ? K1 N7 C28 C29 -109.9(8) . . . . ? C31 N7 C28 C25 178.6(8) . . . . ? K1 N7 C28 C25 65.6(10) . . . . ? C24 C25 C28 C29 106.8(12) . . . . ? C26 C25 C28 C29 -12.1(14) . . . . ? C27 C25 C28 C29 -131.6(11) . . . . ? C24 C25 C28 N7 -67.4(11) . . . . ? C26 C25 C28 N7 173.7(8) . . . . ? C27 C25 C28 N7 54.3(11) . . . . ? N7 C28 C29 C30 -1.5(12) . . . . ? C25 C28 C29 C30 -176.4(10) . . . . ? C28 C29 C30 C31 -0.6(14) . . . . ? C29 C30 C31 N7 2.4(13) . . . . ? C29 C30 C31 C32 176.4(11) . . . . ? C28 N7 C31 C30 -3.5(12) . . . . ? K1 N7 C31 C30 128.3(8) . . . . ? C28 N7 C31 C32 -178.3(9) . . . . ? K1 N7 C31 C32 -46.6(10) . . . . ? C33 N8 C32 C31 179.1(9) . . . . ? K1 N8 C32 C31 54.7(11) . . . . ? C33 N8 C32 K1 124.4(10) . . . . ? C30 C31 C32 N8 -171.0(12) . . . . ? N7 C31 C32 N8 2.3(15) . . . . ? C30 C31 C32 K1 -130.7(13) . . . . ? N7 C31 C32 K1 42.6(9) . . . . ? O3 K1 C32 N8 3.8(7) . . . . ? O5 K1 C32 N8 -162.6(8) . . . . ? O6 K1 C32 N8 -82.1(8) . . . . ? N5 K1 C32 N8 71.1(8) . . . . ? O1 K1 C32 N8 58.8(7) . . . . ? N6 K1 C32 N8 110.7(7) . . . . ? N7 K1 C32 N8 112.5(8) . . . . ? C43 K1 C32 N8 -61.8(9) . . . . ? C20 K1 C32 N8 107.2(7) . . . . ? C21 K1 C32 N8 120.8(7) . . . . ? O3 K1 C32 C31 -130.1(6) . . . . ? O5 K1 C32 C31 63.4(6) . . . . ? O6 K1 C32 C31 143.9(6) . . . . ? N8 K1 C32 C31 -134.0(11) . . . . ? N5 K1 C32 C31 -62.8(7) . . . . ? O1 K1 C32 C31 -75.2(6) . . . . ? N6 K1 C32 C31 -23.2(6) . . . . ? N7 K1 C32 C31 -21.5(5) . . . . ? C43 K1 C32 C31 164.2(7) . . . . ? C20 K1 C32 C31 -26.8(8) . . . . ? C21 K1 C32 C31 -13.2(7) . . . . ? C32 N8 C33 C34 -45.6(15) . . . . ? K1 N8 C33 C34 78.4(11) . . . . ? C32 N8 C33 C38 138.8(10) . . . . ? K1 N8 C33 C38 -97.2(8) . . . . ? C38 C33 C34 C35 0.4(16) . . . . ? N8 C33 C34 C35 -175.2(10) . . . . ? C33 C34 C35 C36 3.1(18) . . . . ? C33 C34 C35 C35A 179.1(11) . . . . ? C34 C35 C36 C37 -3.1(18) . . . . ? C35A C35 C36 C37 -179.2(12) . . . . ? C34 C35 C36 C36A 175.4(14) . . . . ? C35A C35 C36 C36A -1(2) . . . . ? C35 C36 C37 C38 -0.2(19) . . . . ? C36A C36 C37 C38 -178.6(13) . . . . ? C36 C37 C38 C33 3.6(17) . . . . ? C36 C37 C38 N1 178.8(11) . . . . ? C34 C33 C38 C37 -3.7(14) . . . . ? N8 C33 C38 C37 172.1(10) . . . . ? C34 C33 C38 N1 -178.9(9) . . . . ? N8 C33 C38 N1 -3.1(13) . . . . ? C1 N1 C38 C37 62.1(13) . . . . ? U1 N1 C38 C37 -99.6(10) . . . . ? C1 N1 C38 C33 -122.7(10) . . . . ? U1 N1 C38 C33 75.5(10) . . . . ? O3 K1 O5 C42 28(3) . . . . ? O6 K1 O5 C42 3(2) . . . . ? N8 K1 O5 C42 110(2) . . . . ? N5 K1 O5 C42 -97(2) . . . . ? O1 K1 O5 C42 -178.1(19) . . . . ? N6 K1 O5 C42 -143(2) . . . . ? N7 K1 O5 C42 158(2) . . . . ? C43 K1 O5 C42 -12(2) . . . . ? C20 K1 O5 C42 -101(2) . . . . ? C32 K1 O5 C42 116(2) . . . . ? C21 K1 O5 C42 -121(2) . . . . ? O3 K1 O5 C39 -152.7(17) . . . . ? O6 K1 O5 C39 -177.1(17) . . . . ? N8 K1 O5 C39 -70.7(17) . . . . ? N5 K1 O5 C39 82.6(17) . . . . ? O1 K1 O5 C39 1.5(18) . . . . ? N6 K1 O5 C39 36.6(16) . . . . ? N7 K1 O5 C39 -22.1(16) . . . . ? C43 K1 O5 C39 167.9(17) . . . . ? C20 K1 O5 C39 78.1(17) . . . . ? C32 K1 O5 C39 -64.6(16) . . . . ? C21 K1 O5 C39 58.6(16) . . . . ? C42 O5 C39 C40 37(3) . . . . ? K1 O5 C39 C40 -143.2(17) . . . . ? O5 C39 C40 C41 -5(3) . . . . ? C39 C40 C41 C42 -24(3) . . . . ? C39 O5 C42 C41 -49(3) . . . . ? K1 O5 C42 C41 131(2) . . . . ? C40 C41 C42 O5 46(3) . . . . ? O3 K1 O6 C43 44.0(12) . . . . ? O5 K1 O6 C43 -141.5(12) . . . . ? N8 K1 O6 C43 116.3(12) . . . . ? N5 K1 O6 C43 -26.2(12) . . . . ? O1 K1 O6 C43 40.0(14) . . . . ? N6 K1 O6 C43 -64.9(14) . . . . ? N7 K1 O6 C43 158.2(11) . . . . ? C20 K1 O6 C43 -48.2(12) . . . . ? C32 K1 O6 C43 137.6(12) . . . . ? C21 K1 O6 C43 -65.5(12) . . . . ? O3 K1 O6 C46 -76.3(13) . . . . ? O5 K1 O6 C46 98.1(13) . . . . ? N8 K1 O6 C46 -4.0(13) . . . . ? N5 K1 O6 C46 -146.5(13) . . . . ? O1 K1 O6 C46 -80.3(14) . . . . ? N6 K1 O6 C46 174.8(11) . . . . ? N7 K1 O6 C46 37.8(17) . . . . ? C43 K1 O6 C46 -120.3(19) . . . . ? C20 K1 O6 C46 -168.5(13) . . . . ? C32 K1 O6 C46 17.3(14) . . . . ? C21 K1 O6 C46 174.1(12) . . . . ? C46 O6 C43 C44 10(3) . . . . ? K1 O6 C43 C44 -125(2) . . . . ? C46 O6 C43 K1 134.8(14) . . . . ? O3 K1 C43 C44 -40(2) . . . . ? O5 K1 C43 C44 131(2) . . . . ? O6 K1 C43 C44 91(3) . . . . ? N8 K1 C43 C44 19(2) . . . . ? N5 K1 C43 C44 -115(2) . . . . ? O1 K1 C43 C44 -61(2) . . . . ? N6 K1 C43 C44 -132(2) . . . . ? N7 K1 C43 C44 18(4) . . . . ? C20 K1 C43 C44 -135(2) . . . . ? C32 K1 C43 C44 39(2) . . . . ? C21 K1 C43 C44 -144(2) . . . . ? O3 K1 C43 O6 -131.6(13) . . . . ? O5 K1 C43 O6 39.2(12) . . . . ? N8 K1 C43 O6 -72.8(12) . . . . ? N5 K1 C43 O6 154.0(12) . . . . ? O1 K1 C43 O6 -152.0(10) . . . . ? N6 K1 C43 O6 137.1(10) . . . . ? N7 K1 C43 O6 -74(3) . . . . ? C20 K1 C43 O6 134.0(12) . . . . ? C32 K1 C43 O6 -52.6(13) . . . . ? C21 K1 C43 O6 125.0(11) . . . . ? O6 C43 C44 C45 16(3) . . . . ? K1 C43 C44 C45 -46(3) . . . . ? C43 C44 C45 C46 -33(3) . . . . ? C43 O6 C46 C45 -29(2) . . . . ? K1 O6 C46 C45 89.9(17) . . . . ? C44 C45 C46 O6 39(2) . . . . ? C22S C20S C21S C22S 6(4) . . . 4_775 ? C21S C20S C22S C21S -2(5) . . . 4_775 ? C34S C33S C31S C32S -12(4) . . . . ? C33S C31S C32S O30S 13(6) . . . . ? C31S C32S O30S C34S -8(5) . . . . ? C32S O30S C34S C33S -2(4) . . . . ? C31S C33S C34S O30S 9(4) . . . . ? C41S C40S C41S C42S 5(2) 4_675 . . . ? C40S C41S C42S C43S -9.2(9) . . . . ? C41S C42S C43S C42S 5.05(7) . . . 4_675 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.216 _refine_diff_density_min -3.381 _refine_diff_density_rms 0.174 #===END of CIF