# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'M. Ephritikhine' 'Lionel Salmon' 'Pierre Thuery' _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_address ; Laboratoire de Chimie de coordinati Service de Chimie Moleculaire CEA Saclay, Batiment 125 Gif-sur-Yvette F91191 FRANCE ; _publ_contact_author_email EPHRI@DRECAM.CEA.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; Uranium(IV) complexes of calix[n]arenes (n = 4, 6 and 8) ; data_1.2thf _database_code_depnum_ccdc_archive 'CCDC 290602' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H54 Cl2 O8 U' _chemical_formula_weight 1019.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.7160(6) _cell_length_b 11.0604(2) _cell_length_c 21.3661(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.321(2) _cell_angle_gamma 90.00 _cell_volume 4120.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26622 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method ? _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 4.122 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method '\f scan with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 26622 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7706 _reflns_number_gt 6467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The tetrahydrofuran molecule containing O7 is disordered over two positions sharing three C atoms, which have been refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O2 and O4 were found on a Fourier-difference map and all the other ones were introduced at calculated positions, except those of the disordered molecule. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The highest residual electron density peak is located near the badly resolved, disordered tetrahydrofuran molecule. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+7.6284P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7706 _refine_ls_number_parameters 515 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.772 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.098 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.808393(8) 0.412039(12) 0.614470(7) 0.01639(5) Uani 1 1 d . . . Cl1 Cl 0.90558(6) 0.59818(9) 0.62299(5) 0.0251(2) Uani 1 1 d . . . Cl2 Cl 0.91089(6) 0.22682(9) 0.63556(5) 0.0262(2) Uani 1 1 d . . . O1 O 0.73590(15) 0.4993(2) 0.65802(13) 0.0177(6) Uani 1 1 d . . . O2 O 0.73748(15) 0.5715(2) 0.52964(13) 0.0198(6) Uani 1 1 d . . . H2 H 0.7634 0.6393 0.5255 0.024 Uiso 1 1 d R . . O3 O 0.71585(15) 0.3193(2) 0.54161(14) 0.0186(6) Uani 1 1 d . . . O4 O 0.77306(14) 0.2485(2) 0.68047(14) 0.0204(6) Uani 1 1 d . . . H4 H 0.7972 0.1843 0.6989 0.024 Uiso 1 1 d R . . O5 O 0.89439(16) 0.4334(2) 0.73943(14) 0.0236(6) Uani 1 1 d . . . O6 O 0.84462(16) 0.3834(2) 0.50676(15) 0.0242(6) Uani 1 1 d . . . C1 C 0.6798(2) 0.5016(4) 0.7421(2) 0.0192(8) Uani 1 1 d . . . C2 C 0.6939(2) 0.5563(4) 0.6886(2) 0.0189(8) Uani 1 1 d . . . C3 C 0.6652(2) 0.6727(4) 0.6669(2) 0.0197(9) Uani 1 1 d . . . C4 C 0.6247(2) 0.7333(4) 0.7004(2) 0.0250(9) Uani 1 1 d . . . H4A H 0.6067 0.8110 0.6869 0.030 Uiso 1 1 calc R . . C5 C 0.6106(2) 0.6803(4) 0.7537(2) 0.0289(10) Uani 1 1 d . . . H5 H 0.5837 0.7220 0.7759 0.035 Uiso 1 1 calc R . . C6 C 0.6375(2) 0.5640(4) 0.7734(2) 0.0240(9) Uani 1 1 d . . . H6 H 0.6270 0.5271 0.8082 0.029 Uiso 1 1 calc R . . C7 C 0.6770(2) 0.7292(4) 0.6068(2) 0.0230(9) Uani 1 1 d . . . H7A H 0.7305 0.7219 0.6121 0.028 Uiso 1 1 calc R . . H7B H 0.6645 0.8145 0.6049 0.028 Uiso 1 1 calc R . . C8 C 0.6274(2) 0.6688(4) 0.5418(2) 0.0206(9) Uani 1 1 d . . . C9 C 0.6575(2) 0.5898(4) 0.5066(2) 0.0207(8) Uani 1 1 d . . . C10 C 0.6117(2) 0.5278(4) 0.4492(2) 0.0198(9) Uani 1 1 d . . . C11 C 0.5330(2) 0.5490(4) 0.4257(2) 0.0256(10) Uani 1 1 d . . . H11 H 0.5011 0.5090 0.3874 0.031 Uiso 1 1 calc R . . C12 C 0.5014(3) 0.6289(4) 0.4585(2) 0.0279(10) Uani 1 1 d . . . H12 H 0.4489 0.6434 0.4418 0.034 Uiso 1 1 calc R . . C13 C 0.5481(2) 0.6869(4) 0.5159(2) 0.0255(10) Uani 1 1 d . . . H13 H 0.5263 0.7394 0.5380 0.031 Uiso 1 1 calc R . . C14 C 0.6454(2) 0.4371(4) 0.4145(2) 0.0224(9) Uani 1 1 d . . . H14A H 0.6245 0.4517 0.3664 0.027 Uiso 1 1 calc R . . H14B H 0.7005 0.4483 0.4299 0.027 Uiso 1 1 calc R . . C15 C 0.6282(2) 0.3080(4) 0.4282(2) 0.0215(9) Uani 1 1 d . . . C16 C 0.6645(2) 0.2554(4) 0.4919(2) 0.0195(8) Uani 1 1 d . . . C17 C 0.6494(2) 0.1354(4) 0.5044(2) 0.0211(9) Uani 1 1 d . . . C18 C 0.5972(2) 0.0687(4) 0.4523(2) 0.0239(9) Uani 1 1 d . . . H18 H 0.5868 -0.0110 0.4600 0.029 Uiso 1 1 calc R . . C19 C 0.5604(2) 0.1193(4) 0.3893(2) 0.0277(10) Uani 1 1 d . . . H19 H 0.5255 0.0741 0.3551 0.033 Uiso 1 1 calc R . . C20 C 0.5764(2) 0.2382(4) 0.3778(2) 0.0257(9) Uani 1 1 d . . . H20 H 0.5519 0.2719 0.3354 0.031 Uiso 1 1 calc R . . C21 C 0.6888(2) 0.0836(4) 0.5738(2) 0.0224(9) Uani 1 1 d . . . H21A H 0.7433 0.1001 0.5888 0.027 Uiso 1 1 calc R . . H21B H 0.6819 -0.0035 0.5722 0.027 Uiso 1 1 calc R . . C22 C 0.6566(2) 0.1375(4) 0.6238(2) 0.0200(9) Uani 1 1 d . . . C23 C 0.6968(2) 0.2210(4) 0.6722(2) 0.0193(9) Uani 1 1 d . . . C24 C 0.6650(2) 0.2792(4) 0.7135(2) 0.0197(9) Uani 1 1 d . . . C25 C 0.5903(2) 0.2485(4) 0.7066(2) 0.0238(9) Uani 1 1 d . . . H25 H 0.5674 0.2866 0.7333 0.029 Uiso 1 1 calc R . . C26 C 0.5499(2) 0.1627(4) 0.6607(2) 0.0261(10) Uani 1 1 d . . . H26 H 0.5005 0.1417 0.6574 0.031 Uiso 1 1 calc R . . C27 C 0.5827(2) 0.1074(4) 0.6194(2) 0.0236(9) Uani 1 1 d . . . H27 H 0.5550 0.0496 0.5884 0.028 Uiso 1 1 calc R . . C28 C 0.7089(2) 0.3743(4) 0.7644(2) 0.0219(9) Uani 1 1 d . . . H28A H 0.7629 0.3698 0.7708 0.026 Uiso 1 1 calc R . . H28B H 0.7041 0.3574 0.8072 0.026 Uiso 1 1 calc R . . C29 C 0.9011(3) 0.5503(4) 0.7735(2) 0.0264(10) Uani 1 1 d . . . H29A H 0.8516 0.5904 0.7598 0.032 Uiso 1 1 calc R . . H29B H 0.9370 0.6025 0.7632 0.032 Uiso 1 1 calc R . . C30 C 0.9297(3) 0.5208(4) 0.8471(2) 0.0302(10) Uani 1 1 d . . . H30A H 0.8879 0.4980 0.8614 0.036 Uiso 1 1 calc R . . H30B H 0.9573 0.5884 0.8740 0.036 Uiso 1 1 calc R . . C31 C 0.9826(2) 0.4149(4) 0.8511(2) 0.0305(10) Uani 1 1 d . . . H31A H 0.9902 0.3666 0.8909 0.037 Uiso 1 1 calc R . . H31B H 1.0321 0.4423 0.8516 0.037 Uiso 1 1 calc R . . C32 C 0.9398(3) 0.3441(4) 0.7875(2) 0.0289(10) Uani 1 1 d . . . H32A H 0.9755 0.3042 0.7708 0.035 Uiso 1 1 calc R . . H32B H 0.9070 0.2834 0.7959 0.035 Uiso 1 1 calc R . . C33 C 0.8249(3) 0.2698(4) 0.4702(2) 0.0281(10) Uani 1 1 d . . . H33A H 0.7770 0.2774 0.4322 0.034 Uiso 1 1 calc R . . H33B H 0.8195 0.2058 0.4992 0.034 Uiso 1 1 calc R . . C34 C 0.8894(3) 0.2425(5) 0.4468(3) 0.0536(16) Uani 1 1 d D . . H34A H 0.9288 0.1949 0.4798 0.064 Uiso 1 1 calc R . . H34B H 0.8712 0.1991 0.4045 0.064 Uiso 1 1 calc R . . C35 C 0.9184(4) 0.3624(5) 0.4389(4) 0.065(2) Uani 1 1 d D . . H35A H 0.8877 0.3983 0.3962 0.078 Uiso 1 1 calc R . . H35B H 0.9714 0.3583 0.4423 0.078 Uiso 1 1 calc R . . C36 C 0.9109(3) 0.4330(4) 0.4970(3) 0.0425(13) Uani 1 1 d . . . H36A H 0.9563 0.4230 0.5372 0.051 Uiso 1 1 calc R . . H36B H 0.9037 0.5184 0.4863 0.051 Uiso 1 1 calc R . . O7A O 0.7624(4) 0.8028(6) 0.5082(3) 0.031(2) Uani 0.489(7) 1 d P A 1 C37A C 0.8309(5) 0.8763(8) 0.5393(5) 0.030(2) Uani 0.489(7) 1 d P A 1 O7B O 0.7889(3) 0.7355(6) 0.4661(3) 0.036(2) Uani 0.511(7) 1 d P A 2 C37B C 0.8658(5) 0.7909(9) 0.4838(5) 0.036(3) Uani 0.511(7) 1 d P A 2 C38 C 0.8560(3) 0.9140(6) 0.4887(3) 0.0564(17) Uani 1 1 d . . . C39 C 0.7775(3) 0.9336(7) 0.4306(3) 0.075(2) Uani 1 1 d . A . C40 C 0.7320(3) 0.8229(5) 0.4390(3) 0.0426(14) Uani 1 1 d . . . O8 O 0.83032(18) 0.0532(3) 0.75199(19) 0.0406(9) Uani 1 1 d . . . C41 C 0.7760(3) -0.0253(4) 0.7645(3) 0.0398(13) Uani 1 1 d . . . H41A H 0.7370 -0.0510 0.7226 0.048 Uiso 1 1 calc R . . H41B H 0.7513 0.0155 0.7914 0.048 Uiso 1 1 calc R . . C42 C 0.8215(3) -0.1323(5) 0.8019(3) 0.0480(15) Uani 1 1 d . . . H42A H 0.7912 -0.2057 0.7920 0.058 Uiso 1 1 calc R . . H42B H 0.8417 -0.1187 0.8501 0.058 Uiso 1 1 calc R . . C43 C 0.8863(5) -0.1365(6) 0.7731(4) 0.084(2) Uani 1 1 d DU . . H43A H 0.9322 -0.1733 0.8049 0.100 Uiso 1 1 calc R . . H43B H 0.8703 -0.1821 0.7315 0.100 Uiso 1 1 calc R . . C44 C 0.9001(3) -0.0104(5) 0.7613(3) 0.0482(14) Uani 1 1 d D . . H44A H 0.9418 0.0221 0.7995 0.058 Uiso 1 1 calc R . . H44B H 0.9134 -0.0030 0.7217 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01545(8) 0.01598(8) 0.01789(8) 0.00008(7) 0.00623(6) -0.00126(6) Cl1 0.0256(5) 0.0245(5) 0.0260(5) -0.0009(4) 0.0105(4) -0.0083(4) Cl2 0.0219(5) 0.0247(5) 0.0313(6) -0.0005(4) 0.0088(4) 0.0045(4) O1 0.0191(14) 0.0176(14) 0.0183(14) 0.0016(11) 0.0092(12) 0.0029(11) O2 0.0184(13) 0.0197(14) 0.0218(15) 0.0030(12) 0.0078(12) -0.0026(11) O3 0.0175(14) 0.0168(14) 0.0202(15) -0.0026(11) 0.0053(12) -0.0033(11) O4 0.0159(13) 0.0177(14) 0.0253(15) 0.0049(12) 0.0049(11) 0.0019(12) O5 0.0267(15) 0.0186(15) 0.0205(15) -0.0003(12) 0.0027(12) -0.0017(12) O6 0.0263(15) 0.0222(15) 0.0278(16) -0.0037(12) 0.0144(13) -0.0023(12) C1 0.0168(19) 0.021(2) 0.017(2) -0.0021(17) 0.0029(16) -0.0030(16) C2 0.0172(19) 0.024(2) 0.017(2) -0.0028(16) 0.0068(16) -0.0031(16) C3 0.020(2) 0.022(2) 0.015(2) -0.0013(17) 0.0032(17) -0.0022(17) C4 0.025(2) 0.024(2) 0.022(2) -0.0025(18) 0.0047(18) 0.0028(18) C5 0.025(2) 0.037(3) 0.026(2) -0.009(2) 0.0103(19) 0.003(2) C6 0.024(2) 0.033(2) 0.014(2) -0.0032(18) 0.0056(17) -0.0062(18) C7 0.032(2) 0.016(2) 0.023(2) 0.0032(17) 0.0119(18) 0.0035(18) C8 0.026(2) 0.018(2) 0.017(2) 0.0047(16) 0.0071(17) 0.0016(17) C9 0.023(2) 0.020(2) 0.018(2) 0.0076(17) 0.0068(17) 0.0011(18) C10 0.025(2) 0.019(2) 0.017(2) 0.0035(16) 0.0091(17) 0.0008(17) C11 0.026(2) 0.027(2) 0.019(2) 0.0021(18) 0.0034(18) -0.0028(18) C12 0.023(2) 0.030(2) 0.028(2) 0.0077(19) 0.0065(19) 0.0064(19) C13 0.032(2) 0.021(2) 0.026(2) 0.0066(18) 0.014(2) 0.0077(18) C14 0.028(2) 0.025(2) 0.013(2) 0.0014(17) 0.0069(17) 0.0006(18) C15 0.020(2) 0.027(2) 0.020(2) -0.0056(17) 0.0092(17) -0.0017(17) C16 0.0167(19) 0.020(2) 0.025(2) -0.0066(18) 0.0109(17) -0.0007(17) C17 0.0151(19) 0.022(2) 0.028(2) -0.0052(18) 0.0090(17) -0.0007(16) C18 0.021(2) 0.020(2) 0.036(2) -0.0079(19) 0.0159(19) -0.0031(17) C19 0.022(2) 0.029(2) 0.033(3) -0.013(2) 0.0105(19) -0.0051(18) C20 0.022(2) 0.035(2) 0.019(2) -0.0032(19) 0.0075(17) 0.0011(19) C21 0.020(2) 0.0174(19) 0.031(2) -0.0006(18) 0.0097(17) -0.0033(17) C22 0.020(2) 0.0174(19) 0.024(2) 0.0057(17) 0.0086(17) 0.0005(16) C23 0.0170(19) 0.019(2) 0.021(2) 0.0070(17) 0.0065(16) -0.0029(16) C24 0.022(2) 0.020(2) 0.0142(19) 0.0053(16) 0.0026(16) -0.0028(17) C25 0.028(2) 0.025(2) 0.022(2) 0.0043(18) 0.0134(18) -0.0022(19) C26 0.021(2) 0.031(2) 0.029(2) 0.003(2) 0.0132(19) -0.0045(18) C27 0.021(2) 0.022(2) 0.024(2) 0.0008(18) 0.0050(17) -0.0070(17) C28 0.023(2) 0.025(2) 0.017(2) 0.0026(17) 0.0063(17) -0.0014(17) C29 0.027(2) 0.023(2) 0.026(2) -0.0060(18) 0.0048(19) -0.0034(18) C30 0.032(2) 0.036(3) 0.022(2) -0.003(2) 0.009(2) -0.009(2) C31 0.025(2) 0.045(3) 0.019(2) 0.006(2) 0.0043(18) -0.007(2) C32 0.033(2) 0.029(2) 0.022(2) 0.0075(19) 0.006(2) 0.007(2) C33 0.031(2) 0.027(2) 0.029(2) -0.012(2) 0.014(2) -0.010(2) C34 0.050(3) 0.058(4) 0.070(4) -0.034(3) 0.042(3) -0.020(3) C35 0.089(5) 0.057(4) 0.082(5) -0.031(3) 0.070(4) -0.032(4) C36 0.052(3) 0.034(3) 0.061(4) -0.017(3) 0.044(3) -0.019(2) O7A 0.039(4) 0.030(4) 0.019(3) 0.004(3) 0.005(3) -0.016(3) C37A 0.031(5) 0.030(5) 0.027(5) -0.006(4) 0.005(4) -0.008(4) O7B 0.027(3) 0.032(4) 0.045(4) 0.015(3) 0.007(3) -0.009(3) C37B 0.018(4) 0.041(6) 0.040(6) 0.004(4) 0.001(4) -0.005(4) C38 0.043(3) 0.076(4) 0.035(3) 0.022(3) -0.004(2) -0.015(3) C39 0.041(3) 0.092(5) 0.060(4) 0.044(4) -0.019(3) -0.037(3) C40 0.034(3) 0.041(3) 0.045(3) 0.025(3) 0.004(2) -0.004(2) O8 0.0260(17) 0.0354(19) 0.061(2) 0.0266(17) 0.0167(16) 0.0090(14) C41 0.025(2) 0.036(3) 0.056(3) 0.019(3) 0.013(2) 0.002(2) C42 0.038(3) 0.036(3) 0.057(4) 0.021(3) 0.001(3) 0.000(2) C43 0.076(3) 0.076(3) 0.097(3) 0.007(3) 0.030(3) 0.003(2) C44 0.036(3) 0.056(4) 0.055(4) 0.015(3) 0.020(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3 2.125(3) . ? U O1 2.135(3) . ? U O4 2.525(3) . ? U O2 2.531(3) . ? U O5 2.579(3) . ? U O6 2.644(3) . ? U Cl1 2.7092(10) . ? U Cl2 2.7297(10) . ? O1 C2 1.347(5) . ? O2 C9 1.410(5) . ? O3 C16 1.345(5) . ? O4 C23 1.406(4) . ? O5 C32 1.456(5) . ? O5 C29 1.466(5) . ? O6 C36 1.438(5) . ? O6 C33 1.456(5) . ? C1 C6 1.391(6) . ? C1 C2 1.401(6) . ? C1 C28 1.523(6) . ? C2 C3 1.406(6) . ? C3 C4 1.390(6) . ? C3 C7 1.513(6) . ? C4 C5 1.388(6) . ? C5 C6 1.389(6) . ? C7 C8 1.517(6) . ? C8 C13 1.397(6) . ? C8 C9 1.398(6) . ? C9 C10 1.394(6) . ? C10 C11 1.393(6) . ? C10 C14 1.515(6) . ? C11 C12 1.387(6) . ? C12 C13 1.379(6) . ? C14 C15 1.515(6) . ? C15 C20 1.392(6) . ? C15 C16 1.407(6) . ? C16 C17 1.404(6) . ? C17 C18 1.395(6) . ? C17 C21 1.508(6) . ? C18 C19 1.388(6) . ? C19 C20 1.391(6) . ? C21 C22 1.525(6) . ? C22 C23 1.387(6) . ? C22 C27 1.393(6) . ? C23 C24 1.389(6) . ? C24 C25 1.394(6) . ? C24 C28 1.521(6) . ? C25 C26 1.377(6) . ? C26 C27 1.387(6) . ? C29 C30 1.501(6) . ? C30 C31 1.516(7) . ? C31 C32 1.521(6) . ? C33 C34 1.496(6) . ? C34 C35 1.466(6) . ? C35 C36 1.516(7) . ? O7A C40 1.395(8) . ? O7A C37A 1.458(11) . ? C37A C38 1.390(11) . ? O7B C40 1.399(8) . ? O7B C37B 1.481(10) . ? C37B C38 1.383(11) . ? C38 C39 1.556(7) . ? C39 C40 1.538(7) . ? O8 C44 1.432(6) . ? O8 C41 1.434(5) . ? C41 C42 1.506(7) . ? C42 C43 1.548(10) . ? C43 C44 1.457(7) . ? 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 O3 U O1 93.43(10) . . ? O3 U O4 75.76(10) . . ? O1 U O4 75.14(9) . . ? O3 U O2 74.71(9) . . ? O1 U O2 75.29(9) . . ? O4 U O2 136.33(8) . . ? O3 U O5 146.97(10) . . ? O1 U O5 76.32(10) . . ? O4 U O5 71.27(9) . . ? O2 U O5 130.16(9) . . ? O3 U O6 72.74(10) . . ? O1 U O6 146.96(10) . . ? O4 U O6 127.06(9) . . ? O2 U O6 72.16(9) . . ? O5 U O6 130.63(9) . . ? O3 U Cl1 139.88(8) . . ? O1 U Cl1 98.31(8) . . ? O4 U Cl1 144.35(6) . . ? O2 U Cl1 71.53(6) . . ? O5 U Cl1 73.13(7) . . ? O6 U Cl1 76.76(6) . . ? O3 U Cl2 95.46(7) . . ? O1 U Cl2 141.94(7) . . ? O4 U Cl2 71.42(6) . . ? O2 U Cl2 142.66(7) . . ? O5 U Cl2 76.19(7) . . ? O6 U Cl2 70.53(7) . . ? Cl1 U Cl2 98.33(3) . . ? C2 O1 U 176.6(3) . . ? C9 O2 U 124.3(2) . . ? C16 O3 U 172.0(3) . . ? C23 O4 U 123.0(2) . . ? C32 O5 C29 109.0(3) . . ? C32 O5 U 130.7(2) . . ? C29 O5 U 120.2(2) . . ? C36 O6 C33 108.4(3) . . ? C36 O6 U 126.0(3) . . ? C33 O6 U 118.4(2) . . ? C6 C1 C2 119.2(4) . . ? C6 C1 C28 120.6(4) . . ? C2 C1 C28 120.2(4) . . ? O1 C2 C1 120.6(4) . . ? O1 C2 C3 119.3(4) . . ? C1 C2 C3 120.1(4) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 C7 120.9(4) . . ? C2 C3 C7 120.1(4) . . ? C5 C4 C3 121.4(4) . . ? C4 C5 C6 118.9(4) . . ? C5 C6 C1 121.3(4) . . ? C3 C7 C8 111.5(3) . . ? C13 C8 C9 117.1(4) . . ? C13 C8 C7 120.4(4) . . ? C9 C8 C7 122.4(4) . . ? C10 C9 C8 122.7(4) . . ? C10 C9 O2 118.2(4) . . ? C8 C9 O2 119.1(4) . . ? C11 C10 C9 117.8(4) . . ? C11 C10 C14 120.5(4) . . ? C9 C10 C14 121.6(4) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C8 121.6(4) . . ? C15 C14 C10 111.9(3) . . ? C20 C15 C16 118.4(4) . . ? C20 C15 C14 120.7(4) . . ? C16 C15 C14 120.9(4) . . ? O3 C16 C17 118.8(4) . . ? O3 C16 C15 120.2(4) . . ? C17 C16 C15 121.0(4) . . ? C18 C17 C16 118.6(4) . . ? C18 C17 C21 122.2(4) . . ? C16 C17 C21 119.2(4) . . ? C19 C18 C17 121.1(4) . . ? C18 C19 C20 119.4(4) . . ? C19 C20 C15 121.4(4) . . ? C17 C21 C22 111.3(3) . . ? C23 C22 C27 117.8(4) . . ? C23 C22 C21 122.5(4) . . ? C27 C22 C21 119.6(4) . . ? C22 C23 C24 122.8(4) . . ? C22 C23 O4 119.2(4) . . ? C24 C23 O4 118.0(3) . . ? C23 C24 C25 117.7(4) . . ? C23 C24 C28 122.0(4) . . ? C25 C24 C28 120.3(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 120.1(4) . . ? C26 C27 C22 120.7(4) . . ? C24 C28 C1 112.1(3) . . ? O5 C29 C30 105.2(3) . . ? C29 C30 C31 101.8(4) . . ? C30 C31 C32 103.1(3) . . ? O5 C32 C31 105.3(3) . . ? O6 C33 C34 106.0(3) . . ? C35 C34 C33 103.5(4) . . ? C34 C35 C36 102.9(4) . . ? O6 C36 C35 105.3(4) . . ? C40 O7A C37A 110.3(6) . . ? C38 C37A O7A 107.6(7) . . ? C40 O7B C37B 110.0(6) . . ? C38 C37B O7B 106.5(7) . . ? C37B C38 C37A 81.6(7) . . ? C37B C38 C39 100.9(6) . . ? C37A C38 C39 100.0(6) . . ? C40 C39 C38 101.4(4) . . ? O7A C40 O7B 59.7(4) . . ? O7A C40 C39 102.7(5) . . ? O7B C40 C39 103.2(5) . . ? C44 O8 C41 110.4(4) . . ? O8 C41 C42 105.8(4) . . ? C41 C42 C43 100.7(5) . . ? C44 C43 C42 104.7(6) . . ? O8 C44 C43 106.5(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O7A 0.92 1.85 2.670(6) 148.8 . O2 H2 O7B 0.92 1.85 2.647(6) 144.8 . O4 H4 O8 0.86 1.81 2.638(4) 163.3 . #===END data_2.6thf _database_code_depnum_ccdc_archive 'CCDC 290603' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H156 Cl4 O24 U4' _chemical_formula_weight 3220.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9003(6) _cell_length_b 15.8165(7) _cell_length_c 16.4023(10) _cell_angle_alpha 71.339(2) _cell_angle_beta 83.412(2) _cell_angle_gamma 64.607(4) _cell_volume 3085.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 77296 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method ? _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 5.390 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.318 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 77296 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.68 _reflns_number_total 11476 _reflns_number_gt 7096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths and/or displacement parameters for some badly behaving atoms, particularly in the very badly resolved solvent molecules. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some voids in the lattice likely indicate the presence of other, unresolved solvent molecules. Some short H...H contacts involving the solvent molecules indicate that their position is not determined perfectly. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+10.7891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11476 _refine_ls_number_parameters 739 _refine_ls_number_restraints 305 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.862 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.193 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 0.13266(4) 0.95273(4) 0.07305(3) 0.04348(17) Uani 1 1 d . . . U2 U 0.34006(4) 0.75885(4) 0.31426(3) 0.05125(19) Uani 1 1 d . . . Cl1 Cl 0.1641(3) 0.7972(3) 0.2243(2) 0.0591(9) Uani 1 1 d . . . Cl2 Cl 0.3177(2) 0.9205(3) 0.1609(2) 0.0480(8) Uani 1 1 d . . . O1 O 0.2209(7) 0.8303(8) 0.0283(6) 0.052(2) Uani 1 1 d . . . O2 O -0.0201(6) 0.9322(7) 0.0474(5) 0.043(2) Uani 1 1 d . . . O3 O 0.0368(6) 1.0316(7) 0.1579(5) 0.048(2) Uani 1 1 d . . . O4 O 0.2794(7) 0.8844(7) 0.3600(6) 0.056(2) Uani 1 1 d . . . O5 O 0.4564(8) 0.6749(7) 0.4248(6) 0.062(3) Uani 1 1 d . . . O6 O 0.4620(7) 0.6950(7) 0.2337(6) 0.053(2) Uani 1 1 d . . . C1 C 0.3762(10) 0.6779(11) 0.0599(11) 0.061(4) Uani 1 1 d . . . C2 C 0.2643(12) 0.7335(12) 0.0417(10) 0.058(4) Uani 1 1 d . . . C3 C 0.2007(12) 0.6879(14) 0.0422(13) 0.075(5) Uani 1 1 d . . . C4 C 0.2501(14) 0.5831(14) 0.0582(12) 0.081(5) Uani 1 1 d U . . H4 H 0.2091 0.5493 0.0594 0.098 Uiso 1 1 calc R . . C5 C 0.3588(17) 0.5336(17) 0.0718(14) 0.100(6) Uani 1 1 d U . . H5 H 0.3911 0.4664 0.0798 0.120 Uiso 1 1 calc R . . C6 C 0.4204(14) 0.5811(13) 0.0739(11) 0.070(4) Uani 1 1 d U . . H6 H 0.4933 0.5456 0.0850 0.084 Uiso 1 1 calc R . . C7 C 0.0835(12) 0.7448(13) 0.0244(11) 0.068(4) Uani 1 1 d U . . H7A H 0.0579 0.7097 0.0000 0.082 Uiso 1 1 calc R . . H7B H 0.0705 0.8078 -0.0181 0.082 Uiso 1 1 calc R . . C8 C 0.0193(11) 0.7623(11) 0.1066(11) 0.060(4) Uani 1 1 d . . . C9 C -0.0326(11) 0.8577(11) 0.1123(9) 0.054(4) Uani 1 1 d . . . C10 C -0.0895(10) 0.8750(12) 0.1852(10) 0.061(4) Uani 1 1 d . . . C11 C -0.0905(11) 0.7982(15) 0.2514(12) 0.080(6) Uani 1 1 d . . . H11 H -0.1252 0.8093 0.3014 0.096 Uiso 1 1 calc R . . C12 C -0.0422(16) 0.7055(17) 0.2466(14) 0.094(6) Uani 1 1 d U . . H12 H -0.0437 0.6531 0.2925 0.112 Uiso 1 1 calc R . . C13 C 0.0097(16) 0.6903(17) 0.1716(14) 0.094(6) Uani 1 1 d U . . H13 H 0.0388 0.6272 0.1665 0.113 Uiso 1 1 calc R . . C14 C -0.1448(11) 0.9815(13) 0.1910(9) 0.066(5) Uani 1 1 d . . . H14A H -0.1421 1.0260 0.1350 0.079 Uiso 1 1 calc R . . H14B H -0.2192 0.9964 0.2034 0.079 Uiso 1 1 calc R . . C15 C -0.0984(10) 1.0023(13) 0.2573(8) 0.060(4) Uani 1 1 d . . . C16 C -0.0076(10) 1.0260(11) 0.2379(8) 0.054(4) Uani 1 1 d . . . C17 C 0.0338(9) 1.0480(12) 0.2985(9) 0.060(4) Uani 1 1 d . . . C18 C -0.0107(11) 1.0425(14) 0.3791(9) 0.074(5) Uani 1 1 d . . . H18 H 0.0207 1.0514 0.4209 0.088 Uiso 1 1 calc R . . C19 C -0.1020(13) 1.0237(13) 0.3990(12) 0.073(4) Uani 1 1 d U . . H19 H -0.1356 1.0261 0.4511 0.088 Uiso 1 1 calc R . . C20 C -0.1413(12) 1.0004(12) 0.3351(10) 0.061(4) Uani 1 1 d U . . H20 H -0.1987 0.9834 0.3484 0.073 Uiso 1 1 calc R . . C21 C 0.1270(10) 1.0791(11) 0.2755(8) 0.053(4) Uani 1 1 d . . . H21A H 0.1709 1.0473 0.2343 0.063 Uiso 1 1 calc R . . H21B H 0.0980 1.1494 0.2472 0.063 Uiso 1 1 calc R . . C22 C 0.1976(10) 1.0557(12) 0.3505(8) 0.052(4) Uani 1 1 d . . . C23 C 0.2678(9) 0.9592(11) 0.3888(8) 0.048(3) Uani 1 1 d . . . C24 C 0.3373(10) 0.9334(11) 0.4610(9) 0.052(4) Uani 1 1 d . . . C25 C 0.3245(10) 1.0099(11) 0.4899(9) 0.049(3) Uani 1 1 d . . . H25 H 0.3656 0.9959 0.5373 0.059 Uiso 1 1 calc R . . C26 C 0.2571(12) 1.1028(13) 0.4544(10) 0.065(4) Uani 1 1 d . . . H26 H 0.2529 1.1516 0.4764 0.078 Uiso 1 1 calc R . . C27 C 0.1910(10) 1.1271(11) 0.3821(9) 0.053(3) Uani 1 1 d . . . H27 H 0.1438 1.1918 0.3570 0.063 Uiso 1 1 calc R . . C28 C 0.4138(10) 0.8287(11) 0.4990(9) 0.055(4) Uani 1 1 d . . . H28A H 0.3760 0.7872 0.5090 0.066 Uiso 1 1 calc R . . H28B H 0.4403 0.8211 0.5542 0.066 Uiso 1 1 calc R . . C29 C 0.5068(10) 0.7944(11) 0.4427(9) 0.054(4) Uani 1 1 d . . . C30 C 0.5273(10) 0.7184(11) 0.4126(9) 0.052(4) Uani 1 1 d . . . C31 C 0.6187(11) 0.6865(12) 0.3612(11) 0.066(4) Uani 1 1 d . . . C32 C 0.6847(11) 0.7315(14) 0.3451(12) 0.074(5) Uani 1 1 d . . . H32 H 0.7457 0.7098 0.3139 0.089 Uiso 1 1 calc R . . C33 C 0.6610(15) 0.8120(14) 0.3759(12) 0.082(5) Uani 1 1 d U . . H33 H 0.7050 0.8449 0.3624 0.098 Uiso 1 1 calc R . . C34 C 0.5772(11) 0.8409(13) 0.4234(10) 0.066(4) Uani 1 1 d . . . H34 H 0.5643 0.8927 0.4446 0.079 Uiso 1 1 calc R . . C35 C 0.6482(15) 0.5959(14) 0.3318(12) 0.080(5) Uani 1 1 d U . . H35A H 0.7183 0.5486 0.3561 0.096 Uiso 1 1 calc R . . H35B H 0.5987 0.5670 0.3575 0.096 Uiso 1 1 calc R . . C36 C 0.6500(13) 0.6073(13) 0.2391(11) 0.073(5) Uani 1 1 d . . . C37 C 0.5527(12) 0.6583(11) 0.1940(10) 0.060(4) Uani 1 1 d . . . C38 C 0.5512(11) 0.6728(12) 0.1042(11) 0.064(4) Uani 1 1 d . . . C39 C 0.6462(12) 0.6291(14) 0.0663(12) 0.077(5) Uani 1 1 d . . . H39 H 0.6467 0.6334 0.0084 0.093 Uiso 1 1 calc R . . C40 C 0.7373(16) 0.5808(15) 0.1126(13) 0.089(5) Uani 1 1 d U . . H40 H 0.8005 0.5543 0.0851 0.106 Uiso 1 1 calc R . . C41 C 0.7415(15) 0.5689(14) 0.1969(12) 0.084(5) Uani 1 1 d U . . H41 H 0.8067 0.5346 0.2268 0.101 Uiso 1 1 calc R . . C42 C 0.4458(11) 0.7314(12) 0.0546(10) 0.060(4) Uani 1 1 d . . . H42A H 0.4054 0.7877 0.0751 0.071 Uiso 1 1 calc R . . H42B H 0.4602 0.7561 -0.0055 0.071 Uiso 1 1 calc R . . O7 O 0.2338(8) 1.0465(8) -0.0175(6) 0.066(3) Uani 1 1 d . . . C43 C 0.3361(14) 0.9979(13) -0.0554(12) 0.079(5) Uani 1 1 d DU . . H43A H 0.3289 0.9624 -0.0911 0.095 Uiso 1 1 calc R . . H43B H 0.3902 0.9526 -0.0109 0.095 Uiso 1 1 calc R . . C44 C 0.363(2) 1.0818(17) -0.1088(17) 0.097(8) Uani 1 1 d PDU . . H44A H 0.4396 1.0630 -0.1092 0.116 Uiso 1 1 calc R . . H44B H 0.3358 1.1067 -0.1674 0.116 Uiso 1 1 calc R . . C45 C 0.311(3) 1.149(3) -0.064(2) 0.124(11) Uani 1 1 d PU . . H45A H 0.2784 1.2132 -0.1052 0.149 Uiso 1 1 calc R . . H45B H 0.3645 1.1500 -0.0312 0.149 Uiso 1 1 calc R . . C46 C 0.2283(15) 1.1346(14) -0.0032(12) 0.082(5) Uani 1 1 d U . . H46A H 0.2468 1.1232 0.0558 0.098 Uiso 1 1 calc R . . H46B H 0.1590 1.1890 -0.0192 0.098 Uiso 1 1 calc R . . O8 O 0.2137(8) 0.7280(9) 0.4307(7) 0.072(3) Uani 1 1 d U . . C47 C 0.116(2) 0.804(2) 0.4389(18) 0.098(8) Uani 1 1 d PDU . . H47A H 0.0768 0.8396 0.3841 0.118 Uiso 1 1 calc R . . H47B H 0.1260 0.8503 0.4604 0.118 Uiso 1 1 calc R . . C48 C 0.057(2) 0.751(2) 0.5035(19) 0.110(10) Uani 1 1 d PDU . . H48A H -0.0022 0.7954 0.5283 0.132 Uiso 1 1 calc R . . H48B H 0.0302 0.7175 0.4776 0.132 Uiso 1 1 calc R . . C49 C 0.1406(18) 0.6826(18) 0.5662(15) 0.113(7) Uani 1 1 d U . . H49A H 0.1386 0.7082 0.6131 0.136 Uiso 1 1 calc R . . H49B H 0.1356 0.6201 0.5895 0.136 Uiso 1 1 calc R . . C50 C 0.234(3) 0.673(3) 0.518(2) 0.128(11) Uani 1 1 d PU . . H50A H 0.2767 0.6940 0.5435 0.154 Uiso 1 1 calc R . . H50B H 0.2759 0.6043 0.5228 0.154 Uiso 1 1 calc R . . O9 O 0.3437(7) 0.5916(7) 0.3413(6) 0.058(2) Uani 1 1 d U . . C51 C 0.434(2) 0.5021(19) 0.3686(19) 0.092(8) Uani 1 1 d PDU . . H51A H 0.4638 0.4943 0.4225 0.111 Uiso 1 1 calc R . . H51B H 0.4882 0.4956 0.3255 0.111 Uiso 1 1 calc R . . C52 C 0.384(3) 0.430(2) 0.380(2) 0.086(10) Uani 1 1 d PDU . . H52A H 0.4394 0.3658 0.3804 0.103 Uiso 1 1 calc R . . H52B H 0.3477 0.4228 0.4338 0.103 Uiso 1 1 calc R . . C53 C 0.311(3) 0.464(2) 0.311(2) 0.070(8) Uani 1 1 d PU . . H53A H 0.2510 0.4470 0.3283 0.084 Uiso 1 1 calc R . . H53B H 0.3445 0.4425 0.2617 0.084 Uiso 1 1 calc R . . C54 C 0.284(5) 0.565(4) 0.297(4) 0.165(18) Uani 1 1 d PU . . H54A H 0.2097 0.5944 0.3124 0.198 Uiso 1 1 calc R . . H54B H 0.2877 0.5945 0.2360 0.198 Uiso 1 1 calc R . . O10 O 0.589(2) 0.864(2) 0.8237(19) 0.118(6) Uani 1 1 d PDU . . C55 C 0.542(4) 0.953(2) 0.756(2) 0.118(6) Uani 1 1 d PDU . . H55A H 0.5911 0.9802 0.7262 0.142 Uiso 1 1 calc R . . H55B H 0.4782 1.0018 0.7715 0.142 Uiso 1 1 calc R . . C56 C 0.520(3) 0.893(2) 0.711(3) 0.098(11) Uani 1 1 d PDU . . H56A H 0.5337 0.9145 0.6502 0.118 Uiso 1 1 calc R . . H56B H 0.4449 0.9061 0.7159 0.118 Uiso 1 1 calc R . . C57 C 0.584(3) 0.783(2) 0.744(2) 0.110(13) Uani 1 1 d PDU . . H57A H 0.5429 0.7479 0.7404 0.132 Uiso 1 1 calc R . . H57B H 0.6488 0.7622 0.7123 0.132 Uiso 1 1 calc R . . C58 C 0.610(6) 0.765(3) 0.837(3) 0.118(6) Uani 1 1 d PDU . . H58A H 0.5616 0.7435 0.8772 0.142 Uiso 1 1 calc R . . H58B H 0.6832 0.7197 0.8541 0.142 Uiso 1 1 calc R . . O11 O 0.5843(18) 0.3206(19) 0.2442(16) 0.090(5) Uani 1 1 d PDU . . C59 C 0.641(2) 0.284(3) 0.177(2) 0.090(5) Uani 1 1 d PDU . . H59A H 0.5972 0.3187 0.1241 0.108 Uiso 1 1 calc R . . H59B H 0.6550 0.2147 0.1908 0.108 Uiso 1 1 calc R . . C60 C 0.744(3) 0.295(4) 0.163(2) 0.111(13) Uani 1 1 d PDU . . H60A H 0.8011 0.2387 0.1496 0.133 Uiso 1 1 calc R . . H60B H 0.7371 0.3542 0.1167 0.133 Uiso 1 1 calc R . . C61 C 0.764(2) 0.301(3) 0.249(2) 0.086(10) Uani 1 1 d PDU . . H61A H 0.8048 0.2368 0.2876 0.103 Uiso 1 1 calc R . . H61B H 0.8004 0.3430 0.2424 0.103 Uiso 1 1 calc R . . C62 C 0.652(2) 0.346(3) 0.280(2) 0.090(5) Uani 1 1 d PDU . . H62A H 0.6522 0.3217 0.3422 0.107 Uiso 1 1 calc R . . H62B H 0.6267 0.4166 0.2630 0.107 Uiso 1 1 calc R . . O12 O 0.076(3) 0.406(3) 0.193(3) 0.190(8) Uani 1 1 d PDU . . C63 C 0.009(4) 0.355(4) 0.2165(19) 0.190(8) Uani 1 1 d PDU . . H63A H -0.0581 0.3943 0.2374 0.228 Uiso 1 1 calc R . . H63B H 0.0433 0.2931 0.2609 0.228 Uiso 1 1 calc R . . C64 C -0.008(2) 0.339(3) 0.1342(19) 0.080(9) Uani 1 1 d PDU . . H64A H -0.0066 0.2741 0.1459 0.096 Uiso 1 1 calc R . . H64B H -0.0754 0.3878 0.1064 0.096 Uiso 1 1 calc R . . C65 C 0.084(3) 0.347(3) 0.078(2) 0.111(13) Uani 1 1 d PDU . . H65A H 0.0625 0.3746 0.0177 0.134 Uiso 1 1 calc R . . H65B H 0.1439 0.2839 0.0870 0.134 Uiso 1 1 calc R . . C66 C 0.113(4) 0.416(4) 0.107(3) 0.190(8) Uani 1 1 d PDU . . H66A H 0.1893 0.3967 0.1051 0.228 Uiso 1 1 calc R . . H66B H 0.0776 0.4832 0.0701 0.228 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0459(3) 0.0597(4) 0.0368(3) -0.0221(3) 0.0098(2) -0.0295(3) U2 0.0509(3) 0.0511(4) 0.0466(3) -0.0184(3) 0.0057(2) -0.0150(3) Cl1 0.0477(18) 0.064(2) 0.061(2) -0.0085(19) 0.0105(16) -0.0281(17) Cl2 0.0461(17) 0.056(2) 0.0467(18) -0.0221(17) 0.0033(14) -0.0219(15) O1 0.053(5) 0.071(7) 0.053(6) -0.034(5) 0.019(4) -0.038(5) O2 0.044(5) 0.065(6) 0.036(5) -0.018(5) 0.009(4) -0.038(4) O3 0.042(5) 0.058(6) 0.041(5) -0.021(5) 0.001(4) -0.015(4) O4 0.054(5) 0.058(7) 0.045(5) -0.018(5) -0.007(4) -0.011(5) O5 0.068(6) 0.050(6) 0.048(6) -0.008(5) 0.000(5) -0.010(5) O6 0.051(5) 0.056(6) 0.052(6) -0.026(5) 0.011(4) -0.019(5) C1 0.038(7) 0.059(10) 0.113(13) -0.053(10) 0.023(8) -0.029(7) C2 0.062(9) 0.058(10) 0.069(10) -0.040(9) 0.012(7) -0.027(8) C3 0.049(9) 0.083(13) 0.107(14) -0.037(11) 0.020(9) -0.037(9) C4 0.081(5) 0.081(5) 0.082(5) -0.0248(18) 0.0020(10) -0.034(2) C5 0.100(6) 0.100(6) 0.100(6) -0.030(2) 0.0030(10) -0.042(3) C6 0.070(4) 0.070(4) 0.070(4) -0.0214(16) 0.0020(10) -0.029(2) C7 0.068(4) 0.068(4) 0.069(4) -0.0209(16) 0.0016(10) -0.029(2) C8 0.044(7) 0.048(9) 0.093(12) -0.026(9) 0.009(7) -0.022(7) C9 0.060(8) 0.055(10) 0.054(9) 0.002(7) -0.013(7) -0.040(8) C10 0.041(7) 0.060(10) 0.058(9) 0.012(8) 0.008(7) -0.024(7) C11 0.034(7) 0.104(15) 0.078(12) -0.002(11) 0.017(7) -0.028(9) C12 0.093(6) 0.093(6) 0.094(6) -0.028(2) 0.0028(10) -0.039(3) C13 0.094(6) 0.094(6) 0.094(6) -0.028(2) 0.0025(10) -0.039(3) C14 0.046(8) 0.107(14) 0.041(8) -0.023(9) 0.003(6) -0.031(8) C15 0.040(7) 0.109(14) 0.030(7) -0.027(8) 0.009(6) -0.027(8) C16 0.049(8) 0.062(10) 0.028(7) -0.016(7) 0.010(6) -0.004(7) C17 0.021(6) 0.091(12) 0.061(9) -0.043(9) 0.008(6) -0.005(6) C18 0.052(8) 0.133(17) 0.043(8) -0.048(10) 0.015(7) -0.032(9) C19 0.073(5) 0.074(5) 0.073(5) -0.0222(17) 0.0020(10) -0.030(2) C20 0.061(4) 0.061(4) 0.061(4) -0.0185(15) 0.0016(10) -0.0252(18) C21 0.054(8) 0.055(9) 0.032(7) -0.016(7) -0.003(6) -0.005(7) C22 0.048(8) 0.076(11) 0.041(8) -0.027(8) 0.006(6) -0.030(8) C23 0.036(7) 0.056(9) 0.043(7) -0.025(7) 0.000(5) -0.004(6) C24 0.043(7) 0.062(10) 0.046(8) -0.023(7) 0.006(6) -0.013(7) C25 0.045(7) 0.053(9) 0.054(8) -0.024(7) 0.000(6) -0.019(7) C26 0.075(10) 0.070(12) 0.063(10) -0.037(9) 0.015(8) -0.032(9) C27 0.051(8) 0.051(9) 0.054(9) -0.009(7) 0.000(6) -0.024(7) C28 0.052(8) 0.069(11) 0.043(8) -0.023(7) -0.003(6) -0.020(7) C29 0.042(7) 0.056(10) 0.052(8) -0.022(7) -0.004(6) -0.005(6) C30 0.043(7) 0.057(10) 0.050(8) -0.014(7) -0.006(6) -0.013(7) C31 0.044(8) 0.072(12) 0.075(11) -0.029(9) -0.008(7) -0.009(7) C32 0.037(8) 0.100(14) 0.092(13) -0.049(11) 0.000(8) -0.020(8) C33 0.082(5) 0.082(5) 0.082(5) -0.0248(18) 0.0021(10) -0.034(2) C34 0.046(8) 0.092(13) 0.078(11) -0.050(10) 0.005(7) -0.028(8) C35 0.080(5) 0.080(5) 0.080(5) -0.0243(18) 0.0021(10) -0.033(2) C36 0.061(10) 0.067(12) 0.076(12) -0.032(10) 0.004(8) -0.007(8) C37 0.063(9) 0.046(9) 0.067(10) -0.024(8) 0.017(8) -0.017(7) C38 0.046(8) 0.079(12) 0.091(12) -0.057(10) 0.018(8) -0.029(8) C39 0.052(9) 0.119(16) 0.082(12) -0.065(12) 0.019(8) -0.035(9) C40 0.089(6) 0.089(6) 0.089(6) -0.0270(19) 0.0025(10) -0.037(2) C41 0.084(5) 0.084(5) 0.084(5) -0.0256(18) 0.0020(10) -0.035(2) C42 0.062(9) 0.077(11) 0.066(10) -0.040(9) 0.025(7) -0.045(8) O7 0.071(7) 0.081(8) 0.055(6) -0.003(6) -0.005(5) -0.050(6) C43 0.079(5) 0.079(5) 0.079(5) -0.0239(18) 0.0019(10) -0.033(2) C44 0.097(8) 0.097(8) 0.097(8) -0.029(3) 0.0026(10) -0.040(4) C45 0.124(11) 0.124(11) 0.124(11) -0.037(3) 0.0034(11) -0.052(5) C46 0.082(5) 0.082(5) 0.082(5) -0.0246(18) 0.0018(10) -0.034(2) O8 0.072(3) 0.071(3) 0.071(3) -0.0214(13) 0.0025(10) -0.0292(15) C47 0.098(9) 0.098(9) 0.098(9) -0.030(3) 0.0027(10) -0.041(4) C48 0.110(10) 0.110(10) 0.110(10) -0.033(3) 0.0032(10) -0.046(4) C49 0.113(7) 0.113(7) 0.113(7) -0.034(2) 0.0032(10) -0.047(3) C50 0.128(11) 0.128(11) 0.128(11) -0.039(4) 0.0034(11) -0.054(5) O9 0.058(3) 0.057(3) 0.058(3) -0.0172(12) 0.0020(10) -0.0240(14) C51 0.092(8) 0.092(8) 0.092(8) -0.028(3) 0.0022(10) -0.038(3) C52 0.086(10) 0.086(10) 0.086(10) -0.026(3) 0.0021(10) -0.036(4) C53 0.070(8) 0.070(8) 0.070(8) -0.021(3) 0.0018(10) -0.029(4) C54 0.165(18) 0.165(18) 0.165(18) -0.050(6) 0.0042(11) -0.069(8) O10 0.118(6) 0.118(6) 0.118(6) -0.036(2) 0.0030(7) -0.049(3) C55 0.118(6) 0.118(6) 0.118(6) -0.036(2) 0.0030(8) -0.049(3) C56 0.098(11) 0.098(11) 0.098(11) -0.030(4) 0.0026(11) -0.041(5) C57 0.110(13) 0.110(13) 0.110(13) -0.033(4) 0.0029(11) -0.046(5) C58 0.118(6) 0.118(6) 0.118(6) -0.036(2) 0.0031(8) -0.049(3) O11 0.090(5) 0.089(5) 0.090(5) -0.0272(16) 0.0023(7) -0.037(2) C59 0.090(5) 0.090(5) 0.090(5) -0.0271(16) 0.0023(8) -0.037(2) C60 0.111(13) 0.111(13) 0.111(13) -0.034(4) 0.0029(11) -0.046(5) C61 0.086(10) 0.086(10) 0.086(10) -0.026(3) 0.0021(10) -0.036(4) C62 0.090(5) 0.089(5) 0.090(5) -0.0271(16) 0.0024(8) -0.037(2) O12 0.190(8) 0.190(8) 0.190(8) -0.057(2) 0.0050(7) -0.079(3) C63 0.190(8) 0.190(8) 0.190(8) -0.057(3) 0.0050(8) -0.079(3) C64 0.080(9) 0.080(9) 0.080(9) -0.024(3) 0.0021(10) -0.033(4) C65 0.111(13) 0.111(13) 0.111(13) -0.034(4) 0.0028(11) -0.046(5) C66 0.190(8) 0.190(8) 0.190(8) -0.057(3) 0.0050(8) -0.079(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.112(9) . ? U1 O3 2.128(8) . ? U1 O2 2.372(9) 2_575 ? U1 O2 2.383(7) . ? U1 O7 2.506(10) . ? U1 Cl1 2.795(4) . ? U1 Cl2 2.865(3) . ? U1 U1 4.0726(9) 2_575 ? U1 U2 4.5430(8) . ? U2 O6 2.123(8) . ? U2 O4 2.142(9) . ? U2 O5 2.227(10) . ? U2 O9 2.518(10) . ? U2 O8 2.518(11) . ? U2 Cl1 2.740(4) . ? U2 Cl2 2.888(4) . ? U2 C30 2.942(13) . ? O1 C2 1.333(17) . ? O2 C9 1.372(16) . ? O2 U1 2.372(9) 2_575 ? O3 C16 1.377(14) . ? O4 C23 1.352(16) . ? O5 C30 1.389(17) . ? O6 C37 1.334(16) . ? C1 C6 1.33(2) . ? C1 C2 1.431(19) . ? C1 C42 1.514(18) . ? C2 C3 1.36(2) . ? C3 C4 1.44(2) . ? C3 C7 1.49(2) . ? C4 C5 1.38(3) . ? C5 C6 1.37(3) . ? C7 C8 1.56(2) . ? C8 C13 1.33(3) . ? C8 C9 1.39(2) . ? C9 C10 1.39(2) . ? C10 C11 1.35(2) . ? C10 C14 1.55(2) . ? C11 C12 1.35(3) . ? C12 C13 1.39(3) . ? C14 C15 1.510(19) . ? C15 C20 1.342(19) . ? C15 C16 1.44(2) . ? C16 C17 1.402(19) . ? C17 C18 1.386(19) . ? C17 C21 1.54(2) . ? C18 C19 1.40(2) . ? C19 C20 1.44(2) . ? C21 C22 1.513(17) . ? C22 C27 1.352(19) . ? C22 C23 1.39(2) . ? C23 C24 1.455(18) . ? C24 C25 1.371(19) . ? C24 C28 1.50(2) . ? C25 C26 1.33(2) . ? C26 C27 1.43(2) . ? C28 C29 1.504(18) . ? C29 C30 1.35(2) . ? C29 C34 1.41(2) . ? C30 C31 1.43(2) . ? C31 C32 1.34(2) . ? C31 C35 1.53(2) . ? C32 C33 1.41(2) . ? C33 C34 1.32(2) . ? C35 C36 1.47(2) . ? C36 C41 1.37(2) . ? C36 C37 1.39(2) . ? C37 C38 1.42(2) . ? C38 C39 1.383(19) . ? C38 C42 1.51(2) . ? C39 C40 1.33(2) . ? C40 C41 1.34(2) . ? O7 C46 1.45(2) . ? O7 C43 1.47(2) . ? C43 C44 1.51(3) . ? C44 C45 1.39(4) . ? C45 C46 1.47(4) . ? O8 C50 1.41(4) . ? O8 C47 1.41(3) . ? C47 C48 1.52(4) . ? C48 C49 1.44(3) . ? C49 C50 1.42(4) . ? O9 C51 1.40(3) . ? O9 C54 1.43(6) . ? C51 C52 1.53(5) . ? C52 C53 1.41(4) . ? C53 C54 1.41(6) . ? O10 C58 1.41(6) . ? O10 C55 1.42(4) . ? C55 C56 1.51(6) . ? C56 C57 1.51(5) . ? C57 C58 1.52(6) . ? O11 C62 1.41(5) . ? O11 C59 1.41(4) . ? C59 C60 1.50(6) . ? C60 C61 1.51(5) . ? C61 C62 1.51(5) . ? O12 C63 1.43(8) . ? O12 C66 1.43(7) . ? C63 C64 1.51(5) . ? C64 C65 1.52(5) . ? C65 C66 1.53(7) . ? 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 O3 157.7(4) . . ? O1 U1 O2 102.5(3) . 2_575 ? O3 U1 O2 92.2(3) . 2_575 ? O1 U1 O2 85.6(3) . . ? O3 U1 O2 86.6(3) . . ? O2 U1 O2 62.2(4) 2_575 . ? O1 U1 O7 92.2(4) . . ? O3 U1 O7 108.2(4) . . ? O2 U1 O7 73.6(3) 2_575 . ? O2 U1 O7 133.9(3) . . ? O1 U1 Cl1 78.5(3) . . ? O3 U1 Cl1 80.1(3) . . ? O2 U1 Cl1 147.84(19) 2_575 . ? O2 U1 Cl1 86.1(2) . . ? O7 U1 Cl1 138.5(2) . . ? O1 U1 Cl2 91.0(2) . . ? O3 U1 Cl2 88.6(2) . . ? O2 U1 Cl2 139.0(2) 2_575 . ? O2 U1 Cl2 158.6(2) . . ? O7 U1 Cl2 67.3(2) . . ? Cl1 U1 Cl2 72.48(10) . . ? O1 U1 U1 94.7(2) . 2_575 ? O3 U1 U1 89.3(2) . 2_575 ? O2 U1 U1 31.15(19) 2_575 2_575 ? O2 U1 U1 31.0(2) . 2_575 ? O7 U1 U1 103.9(2) . 2_575 ? Cl1 U1 U1 116.97(7) . 2_575 ? Cl2 U1 U1 169.78(8) . 2_575 ? O1 U1 U2 83.1(3) . . ? O3 U1 U2 82.8(2) . . ? O2 U1 U2 174.1(2) 2_575 . ? O2 U1 U2 120.6(2) . . ? O7 U1 U2 104.8(2) . . ? Cl1 U1 U2 34.45(7) . . ? Cl2 U1 U2 38.03(7) . . ? U1 U1 U2 151.26(2) 2_575 . ? O6 U2 O4 138.8(4) . . ? O6 U2 O5 88.8(4) . . ? O4 U2 O5 89.8(3) . . ? O6 U2 O9 76.1(3) . . ? O4 U2 O9 143.9(4) . . ? O5 U2 O9 80.7(4) . . ? O6 U2 O8 144.9(4) . . ? O4 U2 O8 75.1(4) . . ? O5 U2 O8 81.5(4) . . ? O9 U2 O8 69.0(3) . . ? O6 U2 Cl1 99.9(3) . . ? O4 U2 Cl1 99.8(2) . . ? O5 U2 Cl1 152.8(3) . . ? O9 U2 Cl1 76.6(2) . . ? O8 U2 Cl1 76.6(3) . . ? O6 U2 Cl2 75.9(3) . . ? O4 U2 Cl2 76.0(3) . . ? O5 U2 Cl2 134.2(3) . . ? O9 U2 Cl2 133.7(2) . . ? O8 U2 Cl2 133.1(3) . . ? Cl1 U2 Cl2 72.91(10) . . ? O6 U2 C30 80.8(4) . . ? O4 U2 C30 79.7(4) . . ? O5 U2 C30 26.9(4) . . ? O9 U2 C30 103.6(4) . . ? O8 U2 C30 102.8(4) . . ? Cl1 U2 C30 179.3(3) . . ? Cl2 U2 C30 107.4(3) . . ? O6 U2 U1 87.8(3) . . ? O4 U2 U1 88.0(2) . . ? O5 U2 U1 171.9(3) . . ? O9 U2 U1 105.5(2) . . ? O8 U2 U1 105.4(2) . . ? Cl1 U2 U1 35.24(8) . . ? Cl2 U2 U1 37.67(6) . . ? C30 U2 U1 145.0(3) . . ? U2 Cl1 U1 110.31(12) . . ? U1 Cl2 U2 104.30(11) . . ? C2 O1 U1 150.1(9) . . ? C9 O2 U1 130.3(7) . 2_575 ? C9 O2 U1 111.5(7) . . ? U1 O2 U1 117.8(4) 2_575 . ? C16 O3 U1 146.5(9) . . ? C23 O4 U2 165.3(8) . . ? C30 O5 U2 106.6(8) . . ? C37 O6 U2 166.6(9) . . ? C6 C1 C2 120.5(13) . . ? C6 C1 C42 120.1(13) . . ? C2 C1 C42 119.2(13) . . ? O1 C2 C3 119.4(14) . . ? O1 C2 C1 120.0(12) . . ? C3 C2 C1 120.5(15) . . ? C2 C3 C4 117.9(15) . . ? C2 C3 C7 121.2(16) . . ? C4 C3 C7 120.9(15) . . ? C5 C4 C3 119.2(18) . . ? C6 C5 C4 122(2) . . ? C1 C6 C5 120.2(17) . . ? C3 C7 C8 113.0(14) . . ? C13 C8 C9 117.8(17) . . ? C13 C8 C7 123.0(16) . . ? C9 C8 C7 119.2(15) . . ? O2 C9 C10 121.2(14) . . ? O2 C9 C8 118.4(14) . . ? C10 C9 C8 120.2(14) . . ? C11 C10 C9 119.2(16) . . ? C11 C10 C14 121.3(15) . . ? C9 C10 C14 119.4(13) . . ? C12 C11 C10 121.4(19) . . ? C11 C12 C13 118(2) . . ? C8 C13 C12 123(2) . . ? C15 C14 C10 116.0(13) . . ? C20 C15 C16 118.4(12) . . ? C20 C15 C14 121.1(13) . . ? C16 C15 C14 120.5(11) . . ? O3 C16 C17 119.0(13) . . ? O3 C16 C15 120.3(12) . . ? C17 C16 C15 120.6(11) . . ? C18 C17 C16 119.2(14) . . ? C18 C17 C21 120.3(12) . . ? C16 C17 C21 120.4(12) . . ? C17 C18 C19 121.5(14) . . ? C18 C19 C20 117.1(15) . . ? C15 C20 C19 122.8(15) . . ? C22 C21 C17 115.5(12) . . ? C27 C22 C23 119.7(12) . . ? C27 C22 C21 120.9(14) . . ? C23 C22 C21 119.5(12) . . ? O4 C23 C22 122.9(11) . . ? O4 C23 C24 115.8(12) . . ? C22 C23 C24 121.3(13) . . ? C25 C24 C23 115.3(13) . . ? C25 C24 C28 125.2(12) . . ? C23 C24 C28 119.5(12) . . ? C26 C25 C24 124.3(13) . . ? C25 C26 C27 119.6(14) . . ? C22 C27 C26 119.8(14) . . ? C24 C28 C29 113.3(12) . . ? C30 C29 C34 119.0(13) . . ? C30 C29 C28 122.1(14) . . ? C34 C29 C28 118.9(13) . . ? C29 C30 O5 120.9(13) . . ? C29 C30 C31 120.1(15) . . ? O5 C30 C31 118.8(13) . . ? C29 C30 U2 109.4(9) . . ? O5 C30 U2 46.5(6) . . ? C31 C30 U2 107.3(9) . . ? C32 C31 C30 119.4(15) . . ? C32 C31 C35 119.3(15) . . ? C30 C31 C35 121.1(16) . . ? C31 C32 C33 119.8(16) . . ? C34 C33 C32 120.8(18) . . ? C33 C34 C29 121.0(16) . . ? C36 C35 C31 119.1(16) . . ? C41 C36 C37 119.7(16) . . ? C41 C36 C35 123.1(16) . . ? C37 C36 C35 117.3(15) . . ? O6 C37 C36 121.0(14) . . ? O6 C37 C38 119.9(14) . . ? C36 C37 C38 119.1(14) . . ? C39 C38 C37 118.1(15) . . ? C39 C38 C42 122.8(15) . . ? C37 C38 C42 119.0(12) . . ? C40 C39 C38 120.2(17) . . ? C39 C40 C41 122.8(19) . . ? C40 C41 C36 120.0(19) . . ? C1 C42 C38 116.7(14) . . ? C46 O7 C43 110.2(12) . . ? C46 O7 U1 121.5(10) . . ? C43 O7 U1 121.9(9) . . ? O7 C43 C44 103.8(17) . . ? C45 C44 C43 100(2) . . ? C44 C45 C46 119(3) . . ? O7 C46 C45 97.8(19) . . ? C50 O8 C47 99(2) . . ? C50 O8 U2 130.0(16) . . ? C47 O8 U2 121.0(12) . . ? O8 C47 C48 104(2) . . ? C49 C48 C47 101(2) . . ? C50 C49 C48 103(2) . . ? O8 C50 C49 113(3) . . ? C51 O9 C54 101(3) . . ? C51 O9 U2 125.3(11) . . ? C54 O9 U2 128(3) . . ? O9 C51 C52 100(2) . . ? C53 C52 C51 110(3) . . ? C52 C53 C54 95(3) . . ? C53 C54 O9 119(4) . . ? C58 O10 C55 135(3) . . ? O10 C55 C56 87(3) . . ? C55 C56 C57 116(3) . . ? C58 C57 C56 104(3) . . ? O10 C58 C57 93(3) . . ? C62 O11 C59 106(2) . . ? O11 C59 C60 110(3) . . ? C61 C60 C59 102(3) . . ? C62 C61 C60 102(3) . . ? O11 C62 C61 110(2) . . ? C63 O12 C66 114(4) . . ? O12 C63 C64 105(3) . . ? C65 C64 C63 105(3) . . ? C64 C65 C66 104(3) . . ? O12 C66 C65 104(4) . . ? #===END data_3.3py _database_code_depnum_ccdc_archive 'CCDC 290604' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H92 Cl11 N9 O8 U3' _chemical_formula_weight 2663.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.7818(14) _cell_length_b 30.660(3) _cell_length_c 19.4331(19) _cell_angle_alpha 90.00 _cell_angle_beta 112.569(5) _cell_angle_gamma 90.00 _cell_volume 10333.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 154259 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green-yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method ? _exptl_crystal_F_000 5152 _exptl_absorpt_coefficient_mu 5.033 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'one \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% none _diffrn_reflns_number 154259 _diffrn_reflns_av_R_equivalents 0.1292 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 19453 _reflns_number_gt 11541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. One of the solvent pyridine molecules is disordered around a symmetry centre (N atom not located) and another one has been affected with a 0.5 occupancy factor so as to keep reasonable displacement parameters. Due to their very bad resolution, four solvent pyridine molecules were refined as idealized hexagons and restraints on displacement parameters were applied for all of them. The location of the pyridinium ions was inferred from the contacts indicating hydrogen bonds and the N-bound H atoms were placed accordingly. The H atom bound to O6 was not found, nor introduced. All the other H atoms were introduced at calculated positions (except for the disordered pyridine molecule). All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some short H...H contacts involving the pyridine solvents are likely due to the imperfect location of these molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+63.5549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19453 _refine_ls_number_parameters 1156 _refine_ls_number_restraints 282 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.148 _refine_diff_density_min -1.625 _refine_diff_density_rms 0.344 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 1.19200(3) 0.486615(19) 0.33549(3) 0.04982(18) Uani 1 1 d . . . U2 U 0.76447(3) 0.641355(17) 0.12050(3) 0.04834(17) Uani 1 1 d . . . U3 U 0.75058(3) 0.351412(17) 0.10198(3) 0.04676(17) Uani 1 1 d . . . Cl1 Cl 1.0927(2) 0.47741(15) 0.4004(2) 0.0817(12) Uani 1 1 d . . . Cl2 Cl 1.2967(2) 0.42970(13) 0.42496(18) 0.0695(10) Uani 1 1 d . . . Cl3 Cl 1.26887(19) 0.55388(12) 0.42202(18) 0.0610(9) Uani 1 1 d . . . Cl4 Cl 0.76426(19) 0.55352(11) 0.12060(17) 0.0548(8) Uani 1 1 d . . . Cl5 Cl 0.7642(3) 0.72775(14) 0.1207(3) 0.0887(13) Uani 1 1 d . . . Cl6 Cl 0.8449(2) 0.64361(14) 0.0336(2) 0.0739(11) Uani 1 1 d . . . Cl7 Cl 0.6287(2) 0.63697(15) 0.0051(2) 0.0851(13) Uani 1 1 d . . . Cl8 Cl 0.76371(18) 0.43756(12) 0.10121(18) 0.0569(9) Uani 1 1 d . . . Cl9 Cl 0.7253(3) 0.26637(15) 0.0918(3) 0.0959(14) Uani 1 1 d . . . Cl10 Cl 0.6103(3) 0.36170(15) -0.0062(2) 0.0887(13) Uani 1 1 d . . . Cl11 Cl 0.8284(2) 0.34377(15) 0.0141(2) 0.0823(12) Uani 1 1 d . . . O1 O 1.1436(4) 0.4352(3) 0.2580(4) 0.053(2) Uani 1 1 d . . . O2 O 1.2804(4) 0.4890(3) 0.2840(4) 0.048(2) Uani 1 1 d . . . O3 O 1.1381(4) 0.5356(3) 0.2555(4) 0.050(2) Uani 1 1 d . . . O4 O 0.8694(5) 0.6352(3) 0.2154(5) 0.058(2) Uani 1 1 d . . . O5 O 0.7083(5) 0.6399(3) 0.1979(5) 0.049(2) Uani 1 1 d . . . O6 O 0.6640(5) 0.4996(3) 0.1862(5) 0.050(2) Uani 1 1 d . . . O7 O 0.6946(5) 0.3500(3) 0.1826(4) 0.045(2) Uani 1 1 d . . . O8 O 0.8539(4) 0.3527(3) 0.1973(4) 0.044(2) Uani 1 1 d . . . C1 C 1.0588(8) 0.3789(5) 0.1898(7) 0.051(3) Uani 1 1 d . . . C2 C 1.1298(7) 0.4000(4) 0.2137(6) 0.047(3) Uani 1 1 d . . . C3 C 1.1867(7) 0.3836(5) 0.1878(6) 0.047(3) Uani 1 1 d . . . C4 C 1.1713(8) 0.3483(5) 0.1434(7) 0.057(4) Uani 1 1 d . . . H4 H 1.2090 0.3376 0.1279 0.068 Uiso 1 1 calc R . . C5 C 1.0992(8) 0.3272(5) 0.1198(8) 0.067(4) Uani 1 1 d . . . H5A H 1.0897 0.3028 0.0891 0.080 Uiso 1 1 calc R . . C6 C 1.0442(8) 0.3423(5) 0.1416(8) 0.065(4) Uani 1 1 d . . . H6A H 0.9963 0.3288 0.1251 0.078 Uiso 1 1 calc R . . C7 C 1.2635(6) 0.4077(4) 0.2110(7) 0.053(3) Uani 1 1 d . . . H7A H 1.2829 0.4130 0.2642 0.063 Uiso 1 1 calc R . . H7B H 1.3003 0.3890 0.2012 0.063 Uiso 1 1 calc R . . C8 C 1.2587(6) 0.4499(5) 0.1719(7) 0.046(3) Uani 1 1 d . . . C9 C 1.2652(7) 0.4892(5) 0.2112(7) 0.047(3) Uani 1 1 d . . . C10 C 1.2542(6) 0.5298(5) 0.1727(7) 0.047(3) Uani 1 1 d . . . C11 C 1.2464(6) 0.5285(6) 0.0985(7) 0.058(4) Uani 1 1 d . . . H11 H 1.2420 0.5547 0.0731 0.070 Uiso 1 1 calc R . . C12 C 1.2450(7) 0.4911(5) 0.0619(7) 0.049(3) Uani 1 1 d . . . H12 H 1.2407 0.4918 0.0126 0.059 Uiso 1 1 calc R . . C13 C 1.2501(7) 0.4517(5) 0.0975(6) 0.054(4) Uani 1 1 d . . . H13 H 1.2477 0.4259 0.0715 0.065 Uiso 1 1 calc R . . C14 C 1.2598(7) 0.5720(4) 0.2164(7) 0.051(3) Uani 1 1 d . . . H14A H 1.2937 0.5922 0.2052 0.062 Uiso 1 1 calc R . . H14B H 1.2826 0.5656 0.2693 0.062 Uiso 1 1 calc R . . C15 C 1.1815(7) 0.5939(5) 0.1984(7) 0.057(4) Uani 1 1 d . . . C16 C 1.1249(7) 0.5754(5) 0.2212(7) 0.055(4) Uani 1 1 d . . . C17 C 1.0551(7) 0.5979(5) 0.2061(7) 0.054(4) Uani 1 1 d . . . C18 C 1.0435(8) 0.6381(5) 0.1706(8) 0.066(4) Uani 1 1 d . . . H18 H 0.9980 0.6534 0.1617 0.079 Uiso 1 1 calc R . . C19 C 1.0991(8) 0.6555(5) 0.1484(8) 0.058(4) Uani 1 1 d . . . H19 H 1.0902 0.6820 0.1234 0.070 Uiso 1 1 calc R . . C20 C 1.1673(8) 0.6339(5) 0.1629(7) 0.055(4) Uani 1 1 d . . . H20 H 1.2046 0.6464 0.1486 0.066 Uiso 1 1 calc R . . C21 C 0.9931(7) 0.5779(5) 0.2291(7) 0.063(4) Uani 1 1 d . . . H21A H 0.9441 0.5789 0.1870 0.075 Uiso 1 1 calc R . . H21B H 1.0057 0.5475 0.2417 0.075 Uiso 1 1 calc R . . C22 C 0.9846(7) 0.6002(5) 0.2936(7) 0.054(4) Uani 1 1 d . . . C23 C 0.9205(7) 0.6253(5) 0.2850(7) 0.060(4) Uani 1 1 d . . . C24 C 0.9062(9) 0.6424(6) 0.3453(9) 0.077(5) Uani 1 1 d . . . C25 C 0.9631(9) 0.6347(6) 0.4163(8) 0.076(5) Uani 1 1 d . . . H25 H 0.9557 0.6455 0.4578 0.092 Uiso 1 1 calc R . . C26 C 1.0306(9) 0.6114(6) 0.4270(9) 0.080(5) Uani 1 1 d . . . H26 H 1.0696 0.6087 0.4740 0.096 Uiso 1 1 calc R . . C27 C 1.0369(9) 0.5931(6) 0.3663(8) 0.074(4) Uani 1 1 d . . . H27 H 1.0786 0.5748 0.3735 0.089 Uiso 1 1 calc R . . C28 C 0.8334(8) 0.6671(5) 0.3357(8) 0.066(4) Uani 1 1 d . . . H28A H 0.8168 0.6839 0.2899 0.079 Uiso 1 1 calc R . . H28B H 0.8434 0.6871 0.3769 0.079 Uiso 1 1 calc R . . C29 C 0.7691(7) 0.6346(5) 0.3329(8) 0.058(4) Uani 1 1 d . . . C30 C 0.7108(8) 0.6231(5) 0.2639(7) 0.054(4) Uani 1 1 d . . . C31 C 0.6531(7) 0.5924(4) 0.2621(7) 0.046(3) Uani 1 1 d . . . C32 C 0.6590(9) 0.5749(5) 0.3272(8) 0.069(4) Uani 1 1 d . . . H32 H 0.6233 0.5538 0.3268 0.083 Uiso 1 1 calc R . . C33 C 0.7164(9) 0.5866(5) 0.3959(7) 0.068(4) Uani 1 1 d . . . H33 H 0.7179 0.5739 0.4399 0.081 Uiso 1 1 calc R . . C34 C 0.7687(8) 0.6163(6) 0.3968(8) 0.065(4) Uani 1 1 d . . . H34 H 0.8060 0.6247 0.4423 0.078 Uiso 1 1 calc R . . C35 C 0.5920(7) 0.5821(4) 0.1867(6) 0.049(3) Uani 1 1 d . . . H35A H 0.6155 0.5811 0.1502 0.059 Uiso 1 1 calc R . . H35B H 0.5539 0.6053 0.1724 0.059 Uiso 1 1 calc R . . C36 C 0.5511(7) 0.5385(5) 0.1854(6) 0.048(3) Uani 1 1 d . . . C37 C 0.5899(6) 0.4995(4) 0.1861(6) 0.041(3) Uani 1 1 d . . . C38 C 0.5571(6) 0.4592(4) 0.1859(6) 0.038(3) Uani 1 1 d . . . C39 C 0.4827(6) 0.4566(4) 0.1878(6) 0.045(3) Uani 1 1 d . . . H39 H 0.4595 0.4298 0.1879 0.054 Uiso 1 1 calc R . . C40 C 0.4460(7) 0.4952(5) 0.1895(8) 0.056(4) Uani 1 1 d . . . H40 H 0.3978 0.4943 0.1925 0.067 Uiso 1 1 calc R . . C41 C 0.4785(7) 0.5355(5) 0.1868(7) 0.054(4) Uani 1 1 d . . . H41 H 0.4509 0.5609 0.1860 0.065 Uiso 1 1 calc R . . C42 C 0.5996(7) 0.4178(4) 0.1835(6) 0.047(3) Uani 1 1 d . . . H42A H 0.6216 0.4215 0.1461 0.057 Uiso 1 1 calc R . . H42B H 0.5621 0.3944 0.1667 0.057 Uiso 1 1 calc R . . C43 C 0.6634(6) 0.4031(4) 0.2548(6) 0.042(3) Uani 1 1 d . . . C44 C 0.7097(6) 0.3683(4) 0.2511(6) 0.042(3) Uani 1 1 d . . . C45 C 0.7683(7) 0.3507(4) 0.3149(6) 0.042(3) Uani 1 1 d . . . C46 C 0.7785(7) 0.3701(5) 0.3828(7) 0.057(4) Uani 1 1 d . . . H46 H 0.8143 0.3584 0.4266 0.068 Uiso 1 1 calc R . . C47 C 0.7358(6) 0.4070(4) 0.3863(6) 0.043(3) Uani 1 1 d . . . H47 H 0.7460 0.4209 0.4317 0.052 Uiso 1 1 calc R . . C48 C 0.6783(7) 0.4226(5) 0.3218(8) 0.062(4) Uani 1 1 d . . . H48 H 0.6496 0.4468 0.3244 0.074 Uiso 1 1 calc R . . C49 C 0.8197(6) 0.3142(4) 0.3124(7) 0.049(3) Uani 1 1 d . . . H49A H 0.7963 0.2993 0.2649 0.059 Uiso 1 1 calc R . . H49B H 0.8236 0.2934 0.3513 0.059 Uiso 1 1 calc R . . C50 C 0.8995(7) 0.3284(4) 0.3219(6) 0.045(3) Uani 1 1 d . . . C51 C 0.9133(7) 0.3498(4) 0.2649(7) 0.046(3) Uani 1 1 d . . . C52 C 0.9836(7) 0.3676(4) 0.2753(7) 0.051(3) Uani 1 1 d . . . C53 C 1.0460(8) 0.3602(5) 0.3432(8) 0.070(4) Uani 1 1 d . . . H53 H 1.0948 0.3710 0.3511 0.083 Uiso 1 1 calc R . . C54 C 1.0335(8) 0.3366(5) 0.3979(8) 0.064(4) Uani 1 1 d . . . H54 H 1.0749 0.3306 0.4422 0.077 Uiso 1 1 calc R . . C55 C 0.9620(7) 0.3218(5) 0.3886(7) 0.058(4) Uani 1 1 d . . . H55 H 0.9549 0.3071 0.4273 0.070 Uiso 1 1 calc R . . C56 C 0.9947(7) 0.3961(5) 0.2134(7) 0.058(4) Uani 1 1 d . . . H56A H 0.9466 0.3969 0.1701 0.070 Uiso 1 1 calc R . . H56B H 1.0070 0.4257 0.2316 0.070 Uiso 1 1 calc R . . N1 N 1.4273(6) 0.4893(4) 0.3671(6) 0.063(4) Uani 1 1 d . . . H1 H 1.3786 0.4872 0.3416 0.075 Uiso 1 1 calc R . . C57 C 1.4560(9) 0.5282(6) 0.3872(8) 0.068(4) Uani 1 1 d U . . H57 H 1.4241 0.5526 0.3758 0.081 Uiso 1 1 calc R . . C58 C 1.5352(9) 0.5324(6) 0.4260(8) 0.073(4) Uani 1 1 d U . . H58 H 1.5574 0.5596 0.4413 0.088 Uiso 1 1 calc R . . C59 C 1.5790(9) 0.4962(5) 0.4408(8) 0.062(4) Uani 1 1 d U . . H59 H 1.6321 0.4988 0.4661 0.075 Uiso 1 1 calc R . . C60 C 1.5490(10) 0.4570(6) 0.4205(9) 0.082(5) Uani 1 1 d U . . H60 H 1.5807 0.4326 0.4306 0.099 Uiso 1 1 calc R . . C61 C 1.4689(9) 0.4525(6) 0.3837(8) 0.075(4) Uani 1 1 d U . . H61 H 1.4457 0.4253 0.3713 0.090 Uiso 1 1 calc R . . N2 N 0.8335(8) 0.4921(4) 0.2725(8) 0.077(4) Uani 1 1 d U . . H2 H 0.8073 0.4964 0.2259 0.092 Uiso 1 1 calc R . . C62 C 0.8389(10) 0.5247(6) 0.3224(10) 0.084(5) Uani 1 1 d U . . H62 H 0.8180 0.5521 0.3058 0.101 Uiso 1 1 calc R . . C63 C 0.8753(9) 0.5166(5) 0.3965(9) 0.075(5) Uani 1 1 d . . . H63 H 0.8760 0.5379 0.4309 0.089 Uiso 1 1 calc R . . C64 C 0.9108(8) 0.4775(5) 0.4207(8) 0.060(4) Uani 1 1 d . . . H64 H 0.9367 0.4718 0.4713 0.072 Uiso 1 1 calc R . . C65 C 0.9070(8) 0.4465(5) 0.3678(8) 0.063(4) Uani 1 1 d . . . H65 H 0.9320 0.4199 0.3831 0.076 Uiso 1 1 calc R . . C66 C 0.8683(8) 0.4537(6) 0.2954(9) 0.069(4) Uani 1 1 d . . . H66 H 0.8655 0.4321 0.2608 0.083 Uiso 1 1 calc R . . N3 N 0.5790(7) 0.2919(4) 0.1542(7) 0.069(3) Uani 1 1 d . . . H3 H 0.6137 0.3110 0.1576 0.083 Uiso 1 1 calc R . . C67 C 0.5153(10) 0.2912(5) 0.0919(11) 0.086(5) Uani 1 1 d . . . H67 H 0.5076 0.3122 0.0552 0.104 Uiso 1 1 calc R . . C68 C 0.4607(11) 0.2589(6) 0.0825(11) 0.098(6) Uani 1 1 d U . . H68 H 0.4171 0.2564 0.0387 0.118 Uiso 1 1 calc R . . C69 C 0.4745(11) 0.2299(7) 0.1429(11) 0.106(6) Uani 1 1 d U . . H69 H 0.4379 0.2088 0.1400 0.127 Uiso 1 1 calc R . . C70 C 0.5385(11) 0.2323(6) 0.2034(11) 0.097(6) Uani 1 1 d U . . H70 H 0.5473 0.2119 0.2412 0.117 Uiso 1 1 calc R . . C71 C 0.5924(9) 0.2645(5) 0.2116(10) 0.077(5) Uani 1 1 d . . . H71 H 0.6363 0.2671 0.2552 0.093 Uiso 1 1 calc R . . N4 N 1.1833(7) 0.2673(5) 0.3525(8) 0.080(5) Uani 1 1 d GU . . C72 C 1.2043(8) 0.3014(5) 0.3170(7) 0.085(7) Uani 1 1 d GU . . H72 H 1.1680 0.3138 0.2742 0.103 Uiso 1 1 calc R . . C73 C 1.2796(9) 0.3170(5) 0.3454(10) 0.084(10) Uani 1 1 d GU . . H73 H 1.2936 0.3398 0.3216 0.100 Uiso 1 1 calc R . . C74 C 1.3339(7) 0.2985(6) 0.4094(10) 0.076(9) Uani 1 1 d GU . . H74 H 1.3842 0.3089 0.4284 0.092 Uiso 1 1 calc R . . C75 C 1.3128(8) 0.2644(6) 0.4449(8) 0.084(10) Uani 1 1 d GU . . H75 H 1.3492 0.2520 0.4877 0.101 Uiso 1 1 calc R . . C76 C 1.2376(9) 0.2488(5) 0.4165(8) 0.114(9) Uani 1 1 d GU . . H76 H 1.2235 0.2261 0.4402 0.137 Uiso 1 1 calc R . . N5 N 1.0430(6) 0.2413(4) 0.3154(7) 0.113(5) Uani 1 1 d GU . . H5 H 1.0903 0.2493 0.3294 0.135 Uiso 1 1 calc R . . C77 C 0.9904(8) 0.2522(4) 0.2447(7) 0.110(6) Uani 1 1 d GU . . H77 H 1.0064 0.2682 0.2126 0.132 Uiso 1 1 calc R . . C78 C 0.9139(7) 0.2393(5) 0.2221(6) 0.137(8) Uani 1 1 d GU . . H78 H 0.8787 0.2466 0.1748 0.164 Uiso 1 1 calc R . . C79 C 0.8899(6) 0.2153(4) 0.2700(8) 0.109(6) Uani 1 1 d GU . . H79 H 0.8387 0.2066 0.2549 0.131 Uiso 1 1 calc R . . C80 C 0.9425(8) 0.2044(4) 0.3407(7) 0.118(7) Uani 1 1 d GU . . H80 H 0.9264 0.1884 0.3728 0.141 Uiso 1 1 calc R . . C81 C 1.0190(7) 0.2174(4) 0.3634(6) 0.127(7) Uani 1 1 d GU . . H81 H 1.0542 0.2100 0.4106 0.152 Uiso 1 1 calc R . . N6 N 0.9306(10) 0.4306(6) 0.0244(9) 0.072(5) Uani 1 1 d U . . H6 H 0.8864 0.4178 0.0070 0.087 Uiso 1 1 calc R . . C82 C 0.9402(11) 0.4659(6) 0.0739(10) 0.058(5) Uani 1 1 d U . . H82 H 0.9001 0.4739 0.0882 0.069 Uiso 1 1 calc R . . C83 C 1.0069(8) 0.4879(5) 0.1002(7) 0.058(4) Uani 1 1 d . . . H83 H 1.0131 0.5127 0.1297 0.069 Uiso 1 1 calc R . . C84 C 1.0680(9) 0.4715(6) 0.0809(8) 0.072(4) Uani 1 1 d . . . H84 H 1.1157 0.4854 0.0992 0.086 Uiso 1 1 calc R . . C85 C 1.0577(8) 0.4350(5) 0.0354(8) 0.067(4) Uani 1 1 d . . . H85 H 1.0998 0.4237 0.0272 0.081 Uiso 1 1 calc R . . C86 C 0.9870(9) 0.4153(7) 0.0023(10) 0.100(6) Uani 1 1 d U . . H86 H 0.9780 0.3931 -0.0327 0.121 Uiso 1 1 calc R . . N7 N 0.7399(9) 0.2939(5) 0.5268(5) 0.092(8) Uani 1 1 d GU . . H7 H 0.7197 0.2951 0.4789 0.110 Uiso 1 1 calc R . . C87 C 0.7485(7) 0.2539(4) 0.5627(6) 0.064(6) Uani 1 1 d GU . . H87 H 0.7322 0.2285 0.5351 0.077 Uiso 1 1 calc R . . C88 C 0.7812(7) 0.2520(3) 0.6401(7) 0.049(5) Uani 1 1 d GU . . H88A H 0.7869 0.2252 0.6642 0.059 Uiso 1 1 calc R . . C89 C 0.8055(7) 0.2900(4) 0.6815(5) 0.087(6) Uani 1 1 d GU . . H89 H 0.8274 0.2887 0.7332 0.105 Uiso 1 1 calc R . . C90 C 0.7970(6) 0.3300(3) 0.6455(7) 0.080(5) Uani 1 1 d G . . H90 H 0.8132 0.3554 0.6732 0.096 Uiso 1 1 calc R . . C91 C 0.7642(8) 0.3319(4) 0.5681(7) 0.045(6) Uani 1 1 d GU . . H91 H 0.7585 0.3587 0.5441 0.054 Uiso 1 1 calc R . . N8 N 0.5786(8) 0.2938(6) 0.3925(7) 0.125(8) Uani 1 1 d GU . . C92 C 0.5719(8) 0.3315(5) 0.3508(8) 0.064(6) Uani 1 1 d GU . . H92A H 0.6129 0.3509 0.3634 0.077 Uiso 1 1 calc R . . C93 C 0.5039(9) 0.3401(5) 0.2902(8) 0.086(7) Uani 1 1 d GU . . H93 H 0.4995 0.3653 0.2623 0.103 Uiso 1 1 calc R . . C94 C 0.4426(7) 0.3110(6) 0.2713(8) 0.092(8) Uani 1 1 d GU . . H94 H 0.3971 0.3168 0.2308 0.111 Uiso 1 1 calc R . . C95 C 0.4493(9) 0.2733(6) 0.3130(11) 0.085(10) Uani 1 1 d GU . . H95 H 0.4083 0.2538 0.3004 0.102 Uiso 1 1 calc R . . C96 C 0.5173(11) 0.2647(5) 0.3736(10) 0.092(11) Uani 1 1 d GU . . H96 H 0.5217 0.2394 0.4015 0.110 Uiso 1 1 calc R . . N9 N 0.5122(11) 0.6472(6) 0.3332(11) 0.074(7) Uani 0.50 1 d PGU . . C97 C 0.5462(10) 0.6491(8) 0.4105(12) 0.091(11) Uani 0.50 1 d PGU . . H97 H 0.5995 0.6473 0.4346 0.110 Uiso 0.50 1 calc PR . . C98 C 0.5005(16) 0.6539(10) 0.4519(10) 0.086(17) Uani 0.50 1 d PGU . . H98 H 0.5233 0.6552 0.5036 0.103 Uiso 0.50 1 calc PR . . C99 C 0.4209(15) 0.6566(11) 0.4159(15) 0.070(14) Uani 0.50 1 d PGU . . H99 H 0.3903 0.6598 0.4436 0.084 Uiso 0.50 1 calc PR . . C100 C 0.3869(10) 0.6547(9) 0.3386(15) 0.071(14) Uani 0.50 1 d PGU . . H100 H 0.3336 0.6565 0.3145 0.085 Uiso 0.50 1 calc PR . . C101 C 0.4326(12) 0.6500(7) 0.2973(10) 0.077(9) Uani 0.50 1 d PGU . . H101 H 0.4098 0.6487 0.2455 0.092 Uiso 0.50 1 calc PR . . C102 C 0.4360(10) 0.4775(8) -0.0005(8) 0.074(5) Uani 1 1 d . . . C103 C 0.4977(12) 0.4552(6) -0.0002(6) 0.070(5) Uani 1 1 d . . . C104 C 0.5607(10) 0.4767(8) 0.0009(7) 0.081(6) Uani 1 1 d . . . 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 0.0331(3) 0.0865(4) 0.0314(3) 0.0010(2) 0.0141(2) -0.0057(2) U2 0.0417(3) 0.0548(4) 0.0541(3) -0.0004(2) 0.0246(2) 0.0008(2) U3 0.0443(3) 0.0586(4) 0.0399(3) -0.0032(2) 0.0190(2) -0.0108(2) Cl1 0.080(2) 0.106(3) 0.084(2) -0.020(2) 0.060(2) -0.025(2) Cl2 0.067(2) 0.093(3) 0.0440(19) 0.0177(18) 0.0160(17) 0.006(2) Cl3 0.051(2) 0.080(3) 0.053(2) -0.0085(17) 0.0210(17) -0.0008(18) Cl4 0.054(2) 0.059(2) 0.0513(19) -0.0072(16) 0.0201(16) 0.0045(16) Cl5 0.108(3) 0.068(2) 0.110(3) -0.001(2) 0.064(2) 0.002(2) Cl6 0.062(2) 0.115(3) 0.055(2) -0.015(2) 0.0325(19) -0.019(2) Cl7 0.062(2) 0.095(3) 0.082(2) 0.023(2) 0.009(2) 0.008(2) Cl8 0.052(2) 0.061(2) 0.0541(19) 0.0088(16) 0.0155(16) -0.0096(17) Cl9 0.123(3) 0.079(3) 0.108(3) -0.013(2) 0.070(3) -0.019(2) Cl10 0.075(2) 0.105(3) 0.068(2) -0.004(2) 0.007(2) -0.024(2) Cl11 0.085(3) 0.112(3) 0.064(2) -0.010(2) 0.045(2) -0.015(2) O1 0.039(5) 0.092(7) 0.032(5) -0.002(5) 0.018(4) -0.013(5) O2 0.029(4) 0.087(7) 0.026(4) 0.005(4) 0.008(4) -0.009(4) O3 0.027(4) 0.083(7) 0.033(5) 0.021(5) 0.002(4) 0.004(4) O4 0.048(5) 0.065(6) 0.061(6) -0.012(5) 0.020(5) 0.000(5) O5 0.042(5) 0.054(6) 0.051(5) -0.005(4) 0.019(4) -0.003(4) O6 0.034(5) 0.078(7) 0.043(5) 0.002(4) 0.020(4) 0.000(4) O7 0.057(5) 0.053(5) 0.029(4) -0.002(4) 0.021(4) -0.003(4) O8 0.034(4) 0.051(5) 0.049(5) 0.014(4) 0.018(4) -0.004(4) C1 0.052(9) 0.063(10) 0.044(8) 0.009(7) 0.024(7) 0.004(7) C2 0.049(8) 0.065(10) 0.033(7) 0.009(6) 0.020(6) -0.006(7) C3 0.034(7) 0.075(10) 0.036(7) 0.009(7) 0.017(6) 0.005(7) C4 0.061(9) 0.066(10) 0.049(8) 0.015(7) 0.029(7) 0.009(8) C5 0.056(9) 0.076(11) 0.074(10) 0.003(8) 0.032(8) -0.008(8) C6 0.051(9) 0.074(11) 0.064(10) 0.021(8) 0.016(8) -0.015(8) C7 0.032(7) 0.076(10) 0.056(8) 0.016(7) 0.022(6) 0.002(7) C8 0.026(6) 0.070(10) 0.046(8) 0.007(7) 0.018(6) -0.009(6) C9 0.027(7) 0.080(11) 0.046(8) 0.006(7) 0.026(6) -0.004(6) C10 0.021(6) 0.080(10) 0.042(7) 0.010(7) 0.015(6) 0.002(6) C11 0.024(7) 0.106(13) 0.041(8) 0.006(8) 0.009(6) 0.007(7) C12 0.038(7) 0.078(11) 0.036(7) -0.005(7) 0.020(6) 0.001(7) C13 0.049(8) 0.087(11) 0.033(7) 0.000(7) 0.022(6) -0.001(7) C14 0.034(7) 0.073(10) 0.051(8) 0.006(7) 0.021(6) -0.005(7) C15 0.037(8) 0.071(11) 0.058(9) -0.021(8) 0.013(7) -0.003(7) C16 0.024(7) 0.093(12) 0.047(8) -0.008(8) 0.012(6) -0.008(7) C17 0.040(8) 0.075(11) 0.050(8) -0.003(7) 0.019(7) -0.002(7) C18 0.050(9) 0.084(12) 0.059(9) -0.017(8) 0.015(8) 0.014(8) C19 0.059(9) 0.061(10) 0.061(9) -0.006(7) 0.030(8) -0.003(8) C20 0.051(9) 0.072(11) 0.040(8) -0.008(7) 0.016(7) -0.008(8) C21 0.033(7) 0.086(11) 0.064(9) -0.013(8) 0.013(7) 0.007(7) C22 0.032(7) 0.086(11) 0.040(8) -0.003(7) 0.010(6) 0.003(7) C23 0.030(7) 0.106(12) 0.037(8) 0.001(8) 0.008(6) -0.007(8) C24 0.059(10) 0.112(14) 0.069(11) -0.043(9) 0.035(9) -0.023(9) C25 0.080(12) 0.110(14) 0.047(9) -0.031(8) 0.033(9) -0.021(10) C26 0.051(10) 0.116(15) 0.059(10) -0.021(10) 0.006(8) -0.013(9) C27 0.059(10) 0.099(13) 0.070(11) -0.007(9) 0.032(9) 0.005(9) C28 0.053(9) 0.089(12) 0.063(9) -0.039(8) 0.030(8) -0.017(8) C29 0.043(8) 0.079(11) 0.049(9) -0.015(7) 0.014(7) 0.008(7) C30 0.053(9) 0.066(10) 0.048(8) 0.009(7) 0.026(7) 0.022(7) C31 0.031(7) 0.068(9) 0.041(7) 0.000(6) 0.015(6) -0.002(6) C32 0.067(10) 0.083(12) 0.073(11) 0.004(9) 0.044(9) -0.012(8) C33 0.084(11) 0.088(12) 0.035(8) -0.013(7) 0.026(8) -0.009(10) C34 0.048(9) 0.109(14) 0.042(8) -0.014(8) 0.021(7) -0.007(9) C35 0.040(7) 0.067(10) 0.039(7) 0.004(6) 0.015(6) 0.011(7) C36 0.042(7) 0.075(10) 0.028(6) 0.001(6) 0.014(6) -0.004(7) C37 0.021(6) 0.072(10) 0.025(6) 0.007(6) 0.005(5) 0.007(6) C38 0.033(7) 0.047(8) 0.032(6) 0.008(5) 0.011(5) 0.006(6) C39 0.028(6) 0.059(9) 0.049(8) 0.017(6) 0.014(6) 0.014(6) C40 0.023(7) 0.083(12) 0.062(9) 0.010(7) 0.017(6) -0.004(7) C41 0.036(7) 0.082(11) 0.053(8) 0.007(7) 0.027(6) 0.010(7) C42 0.044(7) 0.072(10) 0.025(6) -0.003(6) 0.013(6) -0.006(7) C43 0.033(7) 0.059(9) 0.029(6) -0.011(6) 0.007(5) -0.009(6) C44 0.031(7) 0.068(9) 0.032(7) -0.008(6) 0.016(6) -0.013(6) C45 0.036(7) 0.063(9) 0.031(7) 0.004(6) 0.016(6) 0.000(6) C46 0.047(8) 0.079(11) 0.041(8) 0.015(7) 0.012(7) 0.011(8) C47 0.030(7) 0.061(9) 0.029(6) -0.004(6) 0.002(5) 0.003(6) C48 0.046(8) 0.069(10) 0.073(10) 0.009(8) 0.026(8) 0.005(7) C49 0.034(7) 0.060(9) 0.052(8) 0.004(6) 0.015(6) 0.003(6) C50 0.036(7) 0.059(9) 0.039(7) -0.006(6) 0.013(6) -0.009(6) C51 0.036(7) 0.060(9) 0.040(7) -0.006(6) 0.013(6) 0.001(6) C52 0.040(7) 0.064(9) 0.051(8) 0.014(7) 0.019(7) 0.001(6) C53 0.054(9) 0.103(13) 0.056(9) 0.010(8) 0.025(8) -0.013(8) C54 0.045(9) 0.095(12) 0.047(8) 0.001(8) 0.012(7) 0.003(8) C55 0.043(8) 0.080(11) 0.057(9) 0.015(7) 0.025(7) 0.013(7) C56 0.036(7) 0.078(11) 0.051(8) 0.012(7) 0.007(6) 0.001(7) N1 0.033(6) 0.121(12) 0.031(6) 0.005(6) 0.009(5) 0.000(7) C57 0.065(6) 0.073(6) 0.064(6) 0.009(4) 0.024(4) -0.002(4) C58 0.072(6) 0.078(6) 0.071(6) 0.006(4) 0.029(4) -0.006(4) C59 0.057(5) 0.073(6) 0.061(5) 0.004(4) 0.029(4) -0.001(4) C60 0.079(6) 0.088(7) 0.081(6) -0.005(4) 0.032(5) 0.004(5) C61 0.069(6) 0.077(6) 0.075(6) -0.008(4) 0.024(4) -0.002(4) N2 0.074(5) 0.085(6) 0.074(5) -0.001(4) 0.031(4) 0.011(4) C62 0.083(6) 0.082(6) 0.084(6) -0.001(5) 0.029(5) 0.005(5) C63 0.077(11) 0.069(12) 0.070(11) -0.018(9) 0.019(9) 0.002(9) C64 0.054(9) 0.066(11) 0.061(9) 0.005(8) 0.022(8) -0.004(8) C65 0.067(10) 0.076(11) 0.046(9) -0.005(8) 0.022(8) -0.012(8) C66 0.042(8) 0.093(13) 0.069(11) -0.006(9) 0.017(8) 0.010(8) N3 0.042(7) 0.077(10) 0.086(9) 0.001(8) 0.021(7) 0.002(6) C67 0.082(12) 0.052(11) 0.122(15) -0.008(10) 0.035(12) 0.001(9) C68 0.094(7) 0.098(7) 0.101(7) -0.001(5) 0.035(5) 0.001(5) C69 0.102(7) 0.104(8) 0.112(7) 0.002(5) 0.042(5) -0.006(5) C70 0.098(7) 0.096(7) 0.099(7) 0.004(5) 0.038(5) 0.000(5) C71 0.074(11) 0.069(12) 0.103(13) 0.019(10) 0.051(10) 0.037(9) N4 0.080(7) 0.080(7) 0.081(7) 0.007(5) 0.032(5) 0.005(5) C72 0.083(8) 0.089(8) 0.088(8) 0.012(5) 0.036(5) 0.000(5) C73 0.085(11) 0.082(11) 0.082(11) 0.005(5) 0.030(6) -0.003(5) C74 0.076(10) 0.076(10) 0.076(10) 0.002(5) 0.028(6) -0.003(5) C75 0.084(11) 0.083(11) 0.084(11) 0.008(5) 0.030(6) -0.004(5) C76 0.115(10) 0.113(10) 0.111(10) 0.008(5) 0.040(6) -0.004(5) N5 0.112(6) 0.114(6) 0.115(6) 0.004(3) 0.047(4) -0.002(3) C77 0.111(8) 0.108(8) 0.116(8) 0.001(5) 0.048(5) 0.000(5) C78 0.135(9) 0.135(9) 0.140(9) -0.006(5) 0.053(5) 0.007(5) C79 0.107(8) 0.108(8) 0.118(8) -0.003(5) 0.050(5) -0.004(5) C80 0.118(8) 0.115(8) 0.124(8) -0.001(5) 0.051(5) 0.000(5) C81 0.128(9) 0.126(9) 0.130(9) 0.002(5) 0.052(5) 0.000(5) N6 0.070(6) 0.069(6) 0.074(6) 0.007(3) 0.023(4) -0.006(3) C82 0.054(6) 0.060(7) 0.060(6) 0.011(5) 0.021(5) 0.002(5) C83 0.044(8) 0.091(11) 0.039(8) 0.002(7) 0.017(7) -0.009(8) C84 0.056(9) 0.096(13) 0.063(10) 0.001(9) 0.022(8) -0.003(9) C85 0.085(12) 0.057(10) 0.066(10) 0.006(8) 0.035(9) 0.002(8) C86 0.105(7) 0.094(7) 0.098(7) -0.002(5) 0.033(5) -0.005(5) N7 0.096(9) 0.090(9) 0.088(9) 0.000(4) 0.034(5) -0.001(4) C87 0.068(7) 0.063(7) 0.064(7) -0.005(5) 0.026(5) -0.004(5) C88 0.049(6) 0.046(6) 0.050(6) 0.001(4) 0.015(4) -0.006(4) C89 0.088(8) 0.086(8) 0.084(8) 0.000(5) 0.030(5) 0.002(5) C90 0.060(10) 0.078(12) 0.107(13) -0.019(10) 0.039(10) -0.004(9) C91 0.053(7) 0.042(7) 0.041(7) 0.000(5) 0.020(5) -0.003(5) N8 0.126(9) 0.126(9) 0.124(9) -0.002(4) 0.050(5) 0.003(4) C92 0.064(7) 0.065(7) 0.066(7) -0.005(5) 0.027(5) -0.003(5) C93 0.091(8) 0.086(8) 0.087(8) 0.002(5) 0.041(5) 0.007(5) C94 0.089(9) 0.098(9) 0.090(9) -0.007(5) 0.033(5) 0.012(5) C95 0.086(11) 0.082(11) 0.087(11) -0.002(5) 0.034(6) -0.005(5) C96 0.093(11) 0.091(12) 0.094(11) 0.000(5) 0.038(6) 0.000(5) N9 0.074(8) 0.073(8) 0.077(8) 0.004(4) 0.031(4) -0.001(4) C97 0.088(12) 0.092(12) 0.094(12) -0.004(5) 0.035(6) -0.001(5) C98 0.085(17) 0.087(17) 0.086(17) -0.003(5) 0.032(8) 0.001(5) C99 0.068(15) 0.071(15) 0.071(15) -0.001(5) 0.028(7) 0.002(5) C100 0.068(15) 0.072(15) 0.072(15) -0.004(5) 0.028(7) 0.002(5) C101 0.078(10) 0.074(10) 0.078(10) -0.001(5) 0.029(6) -0.004(5) C102 0.057(11) 0.111(16) 0.049(9) 0.003(9) 0.016(8) -0.030(10) C103 0.095(14) 0.084(12) 0.025(7) 0.001(7) 0.018(8) -0.011(11) C104 0.055(11) 0.148(19) 0.033(8) 0.013(9) 0.007(7) 0.050(12) _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 O3 2.120(8) . ? U1 O1 2.127(9) . ? U1 O2 2.244(8) . ? U1 Cl1 2.637(4) . ? U1 Cl3 2.702(4) . ? U1 Cl2 2.704(4) . ? U2 O4 2.128(9) . ? U2 O5 2.143(8) . ? U2 Cl5 2.649(4) . ? U2 Cl6 2.663(4) . ? U2 Cl7 2.675(4) . ? U2 Cl4 2.693(3) . ? U3 O8 2.107(8) . ? U3 O7 2.198(7) . ? U3 Cl9 2.644(5) . ? U3 Cl11 2.650(4) . ? U3 Cl8 2.653(4) . ? U3 Cl10 2.684(4) . ? Cl4 O6 3.124(9) . ? O1 C2 1.342(15) . ? O2 C9 1.332(14) . ? O3 C16 1.365(16) . ? O4 C23 1.359(15) . ? O5 C30 1.367(14) . ? O6 C37 1.390(14) . ? O7 C44 1.369(13) . ? O8 C51 1.361(14) . ? C1 C2 1.391(18) . ? C1 C6 1.42(2) . ? C1 C56 1.538(17) . ? C2 C3 1.436(17) . ? C3 C4 1.344(18) . ? C3 C7 1.527(17) . ? C4 C5 1.409(19) . ? C5 C6 1.339(19) . ? C7 C8 1.486(17) . ? C8 C13 1.393(16) . ? C8 C9 1.406(18) . ? C9 C10 1.427(18) . ? C10 C11 1.393(17) . ? C10 C14 1.529(18) . ? C11 C12 1.346(19) . ? C12 C13 1.377(18) . ? C14 C15 1.530(17) . ? C15 C20 1.382(19) . ? C15 C16 1.418(18) . ? C16 C17 1.410(18) . ? C17 C18 1.387(19) . ? C17 C21 1.528(18) . ? C18 C19 1.382(19) . ? C19 C20 1.370(18) . ? C21 C22 1.488(17) . ? C22 C23 1.386(18) . ? C22 C27 1.393(18) . ? C23 C24 1.399(19) . ? C24 C25 1.40(2) . ? C24 C28 1.51(2) . ? C25 C26 1.40(2) . ? C26 C27 1.35(2) . ? C28 C29 1.550(19) . ? C29 C34 1.366(19) . ? C29 C30 1.411(18) . ? C30 C31 1.425(18) . ? C31 C32 1.339(17) . ? C31 C35 1.508(16) . ? C32 C33 1.403(19) . ? C33 C34 1.33(2) . ? C35 C36 1.537(18) . ? C36 C41 1.378(16) . ? C36 C37 1.397(17) . ? C37 C38 1.379(16) . ? C38 C39 1.415(15) . ? C38 C42 1.510(17) . ? C39 C40 1.377(17) . ? C40 C41 1.389(18) . ? C42 C43 1.510(16) . ? C43 C48 1.361(17) . ? C43 C44 1.396(17) . ? C44 C45 1.413(16) . ? C45 C46 1.391(17) . ? C45 C49 1.492(16) . ? C46 C47 1.404(18) . ? C47 C48 1.389(17) . ? C49 C50 1.501(16) . ? C50 C55 1.389(17) . ? C50 C51 1.396(17) . ? C51 C52 1.370(17) . ? C52 C53 1.407(18) . ? C52 C56 1.564(17) . ? C53 C54 1.379(18) . ? C54 C55 1.363(18) . ? N1 C57 1.304(19) . ? N1 C61 1.340(18) . ? C57 C58 1.39(2) . ? C58 C59 1.35(2) . ? C59 C60 1.32(2) . ? C60 C61 1.40(2) . ? N2 C66 1.338(18) . ? N2 C62 1.37(2) . ? C62 C63 1.36(2) . ? C63 C64 1.37(2) . ? C64 C65 1.382(19) . ? C65 C66 1.331(18) . ? N3 C67 1.337(19) . ? N3 C71 1.342(18) . ? C67 C68 1.39(2) . ? C68 C69 1.42(2) . ? C69 C70 1.32(2) . ? C70 C71 1.38(2) . ? N4 C72 1.3900 . ? N4 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? N5 C77 1.3900 . ? N5 C81 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? N6 C86 1.37(2) . ? N6 C82 1.42(2) . ? C82 C83 1.34(2) . ? C83 C84 1.43(2) . ? C84 C85 1.39(2) . ? C85 C86 1.37(2) . ? N7 C87 1.3900 . ? N7 C91 1.3900 . ? C87 C88 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? N8 C92 1.3900 . ? N8 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? N9 C97 1.3900 . ? N9 C101 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? C100 C101 1.3900 . ? C102 C103 1.34(2) . ? C102 C104 1.40(3) 3_665 ? C103 C104 1.35(2) . ? C104 C102 1.40(3) 3_665 ? 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 O3 U1 O1 93.0(3) . . ? O3 U1 O2 82.9(3) . . ? O1 U1 O2 84.1(3) . . ? O3 U1 Cl1 101.5(2) . . ? O1 U1 Cl1 94.0(2) . . ? O2 U1 Cl1 175.3(2) . . ? O3 U1 Cl3 84.6(2) . . ? O1 U1 Cl3 170.7(2) . . ? O2 U1 Cl3 86.7(2) . . ? Cl1 U1 Cl3 95.22(12) . . ? O3 U1 Cl2 162.6(2) . . ? O1 U1 Cl2 89.1(2) . . ? O2 U1 Cl2 80.1(2) . . ? Cl1 U1 Cl2 95.53(13) . . ? Cl3 U1 Cl2 90.54(12) . . ? O4 U2 O5 86.1(3) . . ? O4 U2 Cl5 95.1(3) . . ? O5 U2 Cl5 91.1(2) . . ? O4 U2 Cl6 89.4(3) . . ? O5 U2 Cl6 175.4(2) . . ? Cl5 U2 Cl6 88.68(13) . . ? O4 U2 Cl7 171.6(3) . . ? O5 U2 Cl7 91.1(2) . . ? Cl5 U2 Cl7 92.84(14) . . ? Cl6 U2 Cl7 93.43(13) . . ? O4 U2 Cl4 85.0(3) . . ? O5 U2 Cl4 88.7(2) . . ? Cl5 U2 Cl4 179.73(12) . . ? Cl6 U2 Cl4 91.59(12) . . ? Cl7 U2 Cl4 87.08(12) . . ? O8 U3 O7 84.6(3) . . ? O8 U3 Cl9 99.4(2) . . ? O7 U3 Cl9 85.0(2) . . ? O8 U3 Cl11 91.0(2) . . ? O7 U3 Cl11 172.4(2) . . ? Cl9 U3 Cl11 89.54(14) . . ? O8 U3 Cl8 86.0(2) . . ? O7 U3 Cl8 95.4(2) . . ? Cl9 U3 Cl8 174.64(14) . . ? Cl11 U3 Cl8 90.51(12) . . ? O8 U3 Cl10 169.1(2) . . ? O7 U3 Cl10 88.1(2) . . ? Cl9 U3 Cl10 87.89(15) . . ? Cl11 U3 Cl10 97.13(14) . . ? Cl8 U3 Cl10 86.79(12) . . ? C2 O1 U1 167.0(8) . . ? C9 O2 U1 125.5(7) . . ? C16 O3 U1 159.5(8) . . ? C23 O4 U2 161.3(8) . . ? C30 O5 U2 144.9(7) . . ? C44 O7 U3 135.0(7) . . ? C51 O8 U3 169.8(7) . . ? C2 C1 C6 120.5(12) . . ? C2 C1 C56 120.0(13) . . ? C6 C1 C56 119.5(12) . . ? O1 C2 C1 120.9(12) . . ? O1 C2 C3 121.4(11) . . ? C1 C2 C3 117.7(12) . . ? C4 C3 C2 120.1(12) . . ? C4 C3 C7 121.6(12) . . ? C2 C3 C7 118.3(12) . . ? C3 C4 C5 121.4(13) . . ? C6 C5 C4 120.0(15) . . ? C5 C6 C1 120.3(13) . . ? C8 C7 C3 114.0(10) . . ? C13 C8 C9 118.8(12) . . ? C13 C8 C7 121.6(13) . . ? C9 C8 C7 119.5(11) . . ? O2 C9 C8 120.9(12) . . ? O2 C9 C10 119.2(12) . . ? C8 C9 C10 119.9(12) . . ? C11 C10 C9 117.1(13) . . ? C11 C10 C14 123.8(13) . . ? C9 C10 C14 118.8(11) . . ? C12 C11 C10 123.0(15) . . ? C11 C12 C13 120.0(13) . . ? C12 C13 C8 120.9(13) . . ? C10 C14 C15 113.0(10) . . ? C20 C15 C16 119.2(13) . . ? C20 C15 C14 119.2(13) . . ? C16 C15 C14 121.4(13) . . ? O3 C16 C17 121.3(11) . . ? O3 C16 C15 119.6(12) . . ? C17 C16 C15 119.1(14) . . ? C18 C17 C16 119.7(13) . . ? C18 C17 C21 120.7(13) . . ? C16 C17 C21 119.6(13) . . ? C19 C18 C17 120.2(13) . . ? C20 C19 C18 120.6(14) . . ? C19 C20 C15 121.1(13) . . ? C22 C21 C17 113.7(12) . . ? C23 C22 C27 116.8(12) . . ? C23 C22 C21 121.6(11) . . ? C27 C22 C21 121.4(12) . . ? O4 C23 C22 119.6(12) . . ? O4 C23 C24 117.5(13) . . ? C22 C23 C24 123.0(13) . . ? C23 C24 C25 116.3(14) . . ? C23 C24 C28 122.6(14) . . ? C25 C24 C28 121.1(13) . . ? C26 C25 C24 122.4(13) . . ? C27 C26 C25 117.4(14) . . ? C26 C27 C22 123.8(15) . . ? C24 C28 C29 109.8(13) . . ? C34 C29 C30 119.1(14) . . ? C34 C29 C28 120.6(13) . . ? C30 C29 C28 120.3(13) . . ? O5 C30 C29 122.1(13) . . ? O5 C30 C31 118.2(11) . . ? C29 C30 C31 119.6(12) . . ? C32 C31 C30 117.0(12) . . ? C32 C31 C35 126.2(12) . . ? C30 C31 C35 116.8(11) . . ? C31 C32 C33 123.5(14) . . ? C34 C33 C32 118.6(14) . . ? C33 C34 C29 122.0(13) . . ? C31 C35 C36 112.8(10) . . ? C41 C36 C37 117.4(12) . . ? C41 C36 C35 123.2(13) . . ? C37 C36 C35 119.3(11) . . ? C38 C37 O6 116.5(11) . . ? C38 C37 C36 122.4(11) . . ? O6 C37 C36 121.0(11) . . ? C37 C38 C39 119.7(11) . . ? C37 C38 C42 120.8(11) . . ? C39 C38 C42 119.5(11) . . ? C40 C39 C38 117.4(12) . . ? C39 C40 C41 122.3(12) . . ? C36 C41 C40 120.8(13) . . ? C38 C42 C43 117.7(10) . . ? C48 C43 C44 118.8(11) . . ? C48 C43 C42 123.1(12) . . ? C44 C43 C42 118.1(10) . . ? O7 C44 C43 117.5(10) . . ? O7 C44 C45 119.9(11) . . ? C43 C44 C45 122.6(10) . . ? C46 C45 C44 116.6(11) . . ? C46 C45 C49 119.8(11) . . ? C44 C45 C49 123.7(11) . . ? C45 C46 C47 121.1(11) . . ? C48 C47 C46 119.7(12) . . ? C43 C48 C47 121.0(13) . . ? C45 C49 C50 114.0(11) . . ? C55 C50 C51 117.5(11) . . ? C55 C50 C49 121.2(11) . . ? C51 C50 C49 121.3(11) . . ? O8 C51 C52 120.2(11) . . ? O8 C51 C50 117.7(10) . . ? C52 C51 C50 122.2(11) . . ? C51 C52 C53 118.9(12) . . ? C51 C52 C56 120.9(11) . . ? C53 C52 C56 120.2(11) . . ? C54 C53 C52 118.7(13) . . ? C55 C54 C53 121.6(13) . . ? C54 C55 C50 120.8(13) . . ? C1 C56 C52 112.9(11) . . ? C57 N1 C61 124.2(13) . . ? N1 C57 C58 118.6(15) . . ? C59 C58 C57 118.5(16) . . ? C60 C59 C58 122.0(17) . . ? C59 C60 C61 119.6(17) . . ? N1 C61 C60 116.9(15) . . ? C66 N2 C62 120.9(15) . . ? C63 C62 N2 119.2(16) . . ? C62 C63 C64 120.4(15) . . ? C63 C64 C65 117.9(14) . . ? C66 C65 C64 121.6(15) . . ? C65 C66 N2 119.7(15) . . ? C67 N3 C71 124.1(15) . . ? N3 C67 C68 119.3(17) . . ? C67 C68 C69 116.7(18) . . ? C70 C69 C68 121(2) . . ? C69 C70 C71 121.3(19) . . ? N3 C71 C70 117.2(17) . . ? C72 N4 C76 120.0 . . ? N4 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 N4 120.0 . . ? C77 N5 C81 120.0 . . ? N5 C77 C78 120.0 . . ? C77 C78 C79 120.0 . . ? C80 C79 C78 120.0 . . ? C79 C80 C81 120.0 . . ? C80 C81 N5 120.0 . . ? C86 N6 C82 124.3(17) . . ? C83 C82 N6 120.1(18) . . ? C82 C83 C84 116.8(16) . . ? C85 C84 C83 121.3(14) . . ? C86 C85 C84 121.6(16) . . ? N6 C86 C85 115.4(18) . . ? C87 N7 C91 120.0 . . ? N7 C87 C88 120.0 . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C89 C90 C91 120.0 . . ? C90 C91 N7 120.0 . . ? C92 N8 C96 120.0 . . ? N8 C92 C93 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C96 120.0 . . ? C95 C96 N8 120.0 . . ? C97 N9 C101 120.0 . . ? N9 C97 C98 120.0 . . ? C99 C98 C97 120.0 . . ? C100 C99 C98 120.0 . . ? C99 C100 C101 120.0 . . ? C100 C101 N9 120.0 . . ? C103 C102 C104 118.0(14) . 3_665 ? C102 C103 C104 120.1(17) . . ? C103 C104 C102 122.0(14) . 3_665 ? 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 C6 C1 C2 O1 178.6(11) . . . . ? C56 C1 C2 O1 0.6(18) . . . . ? C6 C1 C2 C3 0.2(18) . . . . ? C56 C1 C2 C3 -177.8(11) . . . . ? O1 C2 C3 C4 -179.9(11) . . . . ? C1 C2 C3 C4 -1.5(18) . . . . ? O1 C2 C3 C7 -1.0(17) . . . . ? C1 C2 C3 C7 177.4(11) . . . . ? C2 C3 C4 C5 1.4(19) . . . . ? C7 C3 C4 C5 -177.5(12) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C2 C1 C6 C5 1(2) . . . . ? C56 C1 C6 C5 179.3(12) . . . . ? C4 C3 C7 C8 105.2(15) . . . . ? C2 C3 C7 C8 -73.6(15) . . . . ? C3 C7 C8 C13 -73.6(15) . . . . ? C3 C7 C8 C9 108.2(13) . . . . ? C13 C8 C9 O2 -173.9(10) . . . . ? C7 C8 C9 O2 4.3(16) . . . . ? C13 C8 C9 C10 7.0(17) . . . . ? C7 C8 C9 C10 -174.8(10) . . . . ? O2 C9 C10 C11 173.5(10) . . . . ? C8 C9 C10 C11 -7.4(16) . . . . ? O2 C9 C10 C14 -0.4(15) . . . . ? C8 C9 C10 C14 178.7(10) . . . . ? C9 C10 C11 C12 3.4(17) . . . . ? C14 C10 C11 C12 177.0(11) . . . . ? C10 C11 C12 C13 1.2(19) . . . . ? C11 C12 C13 C8 -1.7(19) . . . . ? C9 C8 C13 C12 -2.4(18) . . . . ? C7 C8 C13 C12 179.4(11) . . . . ? C11 C10 C14 C15 78.6(15) . . . . ? C9 C10 C14 C15 -107.9(13) . . . . ? C10 C14 C15 C20 -113.8(13) . . . . ? C10 C14 C15 C16 69.9(15) . . . . ? C20 C15 C16 O3 179.2(11) . . . . ? C14 C15 C16 O3 -4.5(18) . . . . ? C20 C15 C16 C17 0.9(19) . . . . ? C14 C15 C16 C17 177.1(12) . . . . ? O3 C16 C17 C18 -179.5(12) . . . . ? C15 C16 C17 C18 -1.2(19) . . . . ? O3 C16 C17 C21 0.6(19) . . . . ? C15 C16 C17 C21 178.9(11) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C21 C17 C18 C19 -178.5(12) . . . . ? C17 C18 C19 C20 -2(2) . . . . ? C18 C19 C20 C15 2(2) . . . . ? C16 C15 C20 C19 -1.1(19) . . . . ? C14 C15 C20 C19 -177.4(12) . . . . ? C18 C17 C21 C22 -72.1(16) . . . . ? C16 C17 C21 C22 107.8(15) . . . . ? C17 C21 C22 C23 109.1(15) . . . . ? C17 C21 C22 C27 -77.4(18) . . . . ? C27 C22 C23 O4 176.7(13) . . . . ? C21 C22 C23 O4 -10(2) . . . . ? C27 C22 C23 C24 -2(2) . . . . ? C21 C22 C23 C24 172.1(14) . . . . ? O4 C23 C24 C25 -174.8(13) . . . . ? C22 C23 C24 C25 4(2) . . . . ? O4 C23 C24 C28 6(2) . . . . ? C22 C23 C24 C28 -175.6(14) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C28 C24 C25 C26 179.1(15) . . . . ? C24 C25 C26 C27 -5(3) . . . . ? C25 C26 C27 C22 7(3) . . . . ? C23 C22 C27 C26 -4(2) . . . . ? C21 C22 C27 C26 -177.9(15) . . . . ? C23 C24 C28 C29 86.1(18) . . . . ? C25 C24 C28 C29 -93.0(17) . . . . ? C24 C28 C29 C34 77.9(16) . . . . ? C24 C28 C29 C30 -101.1(15) . . . . ? C34 C29 C30 O5 -179.4(12) . . . . ? C28 C29 C30 O5 -0.3(19) . . . . ? C34 C29 C30 C31 0(2) . . . . ? C28 C29 C30 C31 178.6(12) . . . . ? O5 C30 C31 C32 176.8(12) . . . . ? C29 C30 C31 C32 -2.1(19) . . . . ? O5 C30 C31 C35 -1.8(17) . . . . ? C29 C30 C31 C35 179.2(11) . . . . ? C30 C31 C32 C33 3(2) . . . . ? C35 C31 C32 C33 -178.6(13) . . . . ? C31 C32 C33 C34 -1(2) . . . . ? C32 C33 C34 C29 -2(2) . . . . ? C30 C29 C34 C33 2(2) . . . . ? C28 C29 C34 C33 -176.6(14) . . . . ? C32 C31 C35 C36 -19.3(19) . . . . ? C30 C31 C35 C36 159.2(11) . . . . ? C31 C35 C36 C41 102.9(13) . . . . ? C31 C35 C36 C37 -74.2(14) . . . . ? Cl4 O6 C37 C38 144.2(9) . . . . ? Cl4 O6 C37 C36 -35.0(16) . . . . ? C41 C36 C37 C38 2.0(17) . . . . ? C35 C36 C37 C38 179.3(10) . . . . ? C41 C36 C37 O6 -178.8(10) . . . . ? C35 C36 C37 O6 -1.5(16) . . . . ? O6 C37 C38 C39 178.3(10) . . . . ? C36 C37 C38 C39 -2.4(17) . . . . ? O6 C37 C38 C42 -1.8(15) . . . . ? C36 C37 C38 C42 177.4(10) . . . . ? C37 C38 C39 C40 0.3(17) . . . . ? C42 C38 C39 C40 -179.6(11) . . . . ? C38 C39 C40 C41 2.2(19) . . . . ? C37 C36 C41 C40 0.5(18) . . . . ? C35 C36 C41 C40 -176.6(11) . . . . ? C39 C40 C41 C36 -3(2) . . . . ? C37 C38 C42 C43 77.1(14) . . . . ? C39 C38 C42 C43 -103.0(13) . . . . ? C38 C42 C43 C48 7.3(18) . . . . ? C38 C42 C43 C44 -171.6(11) . . . . ? C48 C43 C44 O7 -178.4(11) . . . . ? C42 C43 C44 O7 0.6(16) . . . . ? C48 C43 C44 C45 4.2(18) . . . . ? C42 C43 C44 C45 -176.7(11) . . . . ? O7 C44 C45 C46 -177.9(11) . . . . ? C43 C44 C45 C46 -0.6(18) . . . . ? O7 C44 C45 C49 4.2(18) . . . . ? C43 C44 C45 C49 -178.5(11) . . . . ? C44 C45 C46 C47 -3.9(19) . . . . ? C49 C45 C46 C47 174.1(12) . . . . ? C45 C46 C47 C48 5(2) . . . . ? C44 C43 C48 C47 -3.4(19) . . . . ? C42 C43 C48 C47 177.7(12) . . . . ? C46 C47 C48 C43 -1(2) . . . . ? C46 C45 C49 C50 -74.5(15) . . . . ? C44 C45 C49 C50 103.4(14) . . . . ? C45 C49 C50 C55 104.4(14) . . . . ? C45 C49 C50 C51 -73.9(15) . . . . ? C55 C50 C51 O8 173.8(11) . . . . ? C49 C50 C51 O8 -7.7(18) . . . . ? C55 C50 C51 C52 -6(2) . . . . ? C49 C50 C51 C52 172.2(12) . . . . ? O8 C51 C52 C53 -173.4(12) . . . . ? C50 C51 C52 C53 7(2) . . . . ? O8 C51 C52 C56 7.3(19) . . . . ? C50 C51 C52 C56 -172.7(12) . . . . ? C51 C52 C53 C54 -2(2) . . . . ? C56 C52 C53 C54 177.1(14) . . . . ? C52 C53 C54 C55 -2(2) . . . . ? C53 C54 C55 C50 3(2) . . . . ? C51 C50 C55 C54 1(2) . . . . ? C49 C50 C55 C54 -177.0(13) . . . . ? C2 C1 C56 C52 -104.6(14) . . . . ? C6 C1 C56 C52 77.4(15) . . . . ? C51 C52 C56 C1 -124.0(13) . . . . ? C53 C52 C56 C1 56.7(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.86 1.75 2.609(13) 172.7 . N2 H2 O6 0.86 2.50 2.984(16) 116.3 . N2 H2 Cl4 0.86 2.58 3.318(15) 145.0 . N3 H3 O7 0.86 1.85 2.697(15) 169.9 . N5 H5 N4 0.86 1.72 2.578(15) 176.4 . N6 H6 Cl11 0.86 2.55 3.243(18) 138.8 . N7 H7 N8 0.86 2.54 3.150(18) 129.2 .