# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Antonella Dalla Cort' 'Massimo Cametti' 'Luigi Mandolini' 'Maija Nissinen' 'Kari Rissanen' _publ_contact_author_name 'Dr Antonella Dalla Cort' _publ_contact_author_address ; Dept of Chemistry Universitą La Sapienza P.le Aldo Moro 5 Rome 00185 ITALY ; _publ_contact_author_email ANTONELLA.DALLACORT@UNIROMA1.IT _publ_section_title ; Uranyl-salophen based ditopic receptors for the recognition of quaternary ammonium halides ; data_2*TMACl _database_code_CSD 215272 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38 Cl N3 O6 U' _chemical_formula_weight 906.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 19.293(3) _cell_length_b 19.293(3) _cell_length_c 19.421(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7229(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 4.614 _exptl_absorpt_correction_type platmulabs _exptl_absorpt_correction_T_min 0.3382 _exptl_absorpt_correction_T_max 0.4588 _exptl_absorpt_process_details 'R. H. Blessing, Acta Crystallogr.A 1995, 51, 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16316 _diffrn_reflns_av_R_equivalents 0.1196 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6368 _reflns_number_gt 5827 _reflns_threshold_expression >2sigma(I) _computing_data_collection collect _computing_cell_refinement denzo-smn _computing_data_reduction denzo-smn _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+64.4995P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(11) _refine_ls_number_reflns 6368 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0822(7) 0.6563(6) 0.7639(6) 0.030(3) Uani 1 1 d . . . C2 C -0.0315(8) 0.6351(7) 0.8117(8) 0.045(3) Uani 1 1 d . . . H2 H 0.0162 0.6395 0.8007 0.054 Uiso 1 1 calc R . . C3 C -0.0510(10) 0.6081(8) 0.8739(8) 0.055(4) Uani 1 1 d . . . H3 H -0.0167 0.5942 0.9061 0.066 Uiso 1 1 calc R . . C4 C -0.1210(11) 0.6010(8) 0.8904(9) 0.063(5) Uani 1 1 d . . . H4 H -0.1344 0.5813 0.9332 0.076 Uiso 1 1 calc R . . C5 C -0.1698(9) 0.6225(8) 0.8445(9) 0.055(4) Uani 1 1 d . . . H5 H -0.2175 0.6187 0.8560 0.066 Uiso 1 1 calc R . . C6 C -0.1508(7) 0.6499(6) 0.7811(8) 0.040(3) Uani 1 1 d . . . H6 H -0.1856 0.6643 0.7496 0.048 Uiso 1 1 calc R . . C7 C -0.0612(6) 0.6883(5) 0.6973(7) 0.031(2) Uani 1 1 d . . . H7A H -0.0291 0.6571 0.6724 0.038 Uiso 1 1 calc R . . H7B H -0.1025 0.6961 0.6681 0.038 Uiso 1 1 calc R . . C9 C -0.0059(5) 0.7909(6) 0.6572(6) 0.022(2) Uani 1 1 d . . . C10 C 0.0353(5) 0.8507(5) 0.6765(5) 0.016(2) Uani 1 1 d . . . C11 C 0.0598(6) 0.8945(6) 0.6227(5) 0.020(2) Uani 1 1 d . . . C12 C 0.0432(6) 0.8809(6) 0.5532(6) 0.025(2) Uani 1 1 d . . . H12 H 0.0582 0.9113 0.5178 0.030 Uiso 1 1 calc R . . C13 C 0.0047(6) 0.8225(6) 0.5374(6) 0.029(3) Uani 1 1 d . . . H13 H -0.0058 0.8127 0.4906 0.034 Uiso 1 1 calc R . . C14 C -0.0191(6) 0.7778(6) 0.5885(6) 0.026(2) Uani 1 1 d . . . H14 H -0.0448 0.7377 0.5759 0.031 Uiso 1 1 calc R . . C15 C 0.1001(6) 0.9555(6) 0.6379(6) 0.025(2) Uani 1 1 d . . . H15 H 0.1066 0.9873 0.6011 0.030 Uiso 1 1 calc R . . C17 C 0.1618(5) 1.0374(5) 0.7011(6) 0.022(2) Uani 1 1 d . . . C18 C 0.2179(5) 1.0434(6) 0.7460(6) 0.024(2) Uani 1 1 d . . . C19 C 0.2511(6) 1.1073(6) 0.7553(6) 0.028(3) Uani 1 1 d . . . H19 H 0.2887 1.1106 0.7867 0.034 Uiso 1 1 calc R . . C20 C 0.2304(6) 1.1653(6) 0.7197(7) 0.033(3) Uani 1 1 d . . . H20 H 0.2542 1.2081 0.7251 0.039 Uiso 1 1 calc R . . C21 C 0.1734(7) 1.1600(7) 0.6754(7) 0.033(3) Uani 1 1 d . . . H21 H 0.1581 1.1999 0.6511 0.039 Uiso 1 1 calc R . . C22 C 0.1388(6) 1.0977(6) 0.6662(6) 0.026(2) Uani 1 1 d . . . H22 H 0.0997 1.0954 0.6365 0.031 Uiso 1 1 calc R . . C24 C 0.3037(5) 0.9747(6) 0.7969(7) 0.030(3) Uani 1 1 d . . . H24 H 0.3342 1.0083 0.7778 0.036 Uiso 1 1 calc R . . C25 C 0.3353(6) 0.9219(7) 0.8384(6) 0.032(3) Uani 1 1 d . . . C26 C 0.2928(6) 0.8778(6) 0.8807(6) 0.025(2) Uani 1 1 d . . . C27 C 0.3287(6) 0.8269(6) 0.9220(6) 0.027(3) Uani 1 1 d . . . C28 C 0.3997(7) 0.8220(7) 0.9196(7) 0.038(3) Uani 1 1 d . . . H28 H 0.4222 0.7881 0.9472 0.046 Uiso 1 1 calc R . . C29 C 0.4398(7) 0.8652(7) 0.8781(8) 0.041(3) Uani 1 1 d . . . H29 H 0.4888 0.8607 0.8770 0.050 Uiso 1 1 calc R . . C30 C 0.4067(7) 0.9148(7) 0.8385(7) 0.039(3) Uani 1 1 d . . . H30 H 0.4337 0.9449 0.8105 0.046 Uiso 1 1 calc R . . C32 C 0.3118(7) 0.7296(7) 0.9970(7) 0.037(3) Uani 1 1 d . . . H32A H 0.3415 0.7468 1.0349 0.044 Uiso 1 1 calc R . . H32B H 0.3400 0.6991 0.9671 0.044 Uiso 1 1 calc R . . C33 C 0.2508(7) 0.6903(6) 1.0257(7) 0.034(3) Uani 1 1 d . . . C34 C 0.1900(7) 0.6824(7) 0.9865(7) 0.038(3) Uani 1 1 d . . . H34 H 0.1879 0.6997 0.9408 0.046 Uiso 1 1 calc R . . C35 C 0.1336(9) 0.6494(7) 1.0148(9) 0.051(4) Uani 1 1 d . . . H35 H 0.0926 0.6432 0.9885 0.061 Uiso 1 1 calc R . . C36 C 0.1369(8) 0.6249(7) 1.0828(9) 0.048(4) Uani 1 1 d . . . H36 H 0.0971 0.6045 1.1032 0.057 Uiso 1 1 calc R . . C37 C 0.1963(9) 0.6300(8) 1.1197(8) 0.048(4) Uani 1 1 d . . . H37 H 0.1989 0.6099 1.1642 0.058 Uiso 1 1 calc R . . C38 C 0.2532(7) 0.6643(6) 1.0928(7) 0.038(3) Uani 1 1 d . . . H38 H 0.2937 0.6701 1.1199 0.045 Uiso 1 1 calc R . . C40 C -0.0833(7) 0.8580(9) 0.8412(6) 0.042(3) Uani 1 1 d . . . H40A H -0.0780 0.9066 0.8273 0.063 Uiso 1 1 calc R . . H40B H -0.1213 0.8369 0.8151 0.063 Uiso 1 1 calc R . . H40C H -0.0402 0.8328 0.8319 0.063 Uiso 1 1 calc R . . C41 C -0.0992(11) 0.7817(8) 0.9371(10) 0.069(5) Uani 1 1 d . . . H41A H -0.0517 0.7638 0.9361 0.104 Uiso 1 1 calc R . . H41B H -0.1281 0.7548 0.9054 0.104 Uiso 1 1 calc R . . H41C H -0.1177 0.7779 0.9839 0.104 Uiso 1 1 calc R . . C42 C -0.1705(7) 0.8854(9) 0.9288(7) 0.047(4) Uani 1 1 d . . . H42A H -0.1804 0.8848 0.9783 0.070 Uiso 1 1 calc R . . H42B H -0.2055 0.8579 0.9044 0.070 Uiso 1 1 calc R . . H42C H -0.1717 0.9333 0.9120 0.070 Uiso 1 1 calc R . . C43 C -0.0472(6) 0.8935(7) 0.9549(7) 0.036(3) Uani 1 1 d . . . H43A H -0.0588 0.8921 1.0040 0.055 Uiso 1 1 calc R . . H43B H -0.0465 0.9417 0.9392 0.055 Uiso 1 1 calc R . . H43C H -0.0014 0.8727 0.9477 0.055 Uiso 1 1 calc R . . N16 N 0.1287(4) 0.9719(4) 0.6965(5) 0.0193(17) Uani 1 1 d . . . N23 N 0.2391(5) 0.9820(5) 0.7825(4) 0.0223(19) Uani 1 1 d . . . N39 N -0.0991(5) 0.8546(5) 0.9158(4) 0.0261(19) Uani 1 1 d . . . O1 O 0.1897(4) 0.8346(4) 0.7503(4) 0.0235(16) Uani 1 1 d . . . O2 O 0.0957(4) 0.9501(4) 0.8552(4) 0.0232(16) Uani 1 1 d . . . O8 O -0.0278(4) 0.7527(4) 0.7115(4) 0.0286(18) Uani 1 1 d . . . O10 O 0.0458(4) 0.8646(4) 0.7415(4) 0.0231(16) Uani 1 1 d . . . O26 O 0.2257(4) 0.8841(4) 0.8842(4) 0.0275(17) Uani 1 1 d . . . O31 O 0.2849(5) 0.7864(4) 0.9581(5) 0.037(2) Uani 1 1 d . . . Cl1 Cl 0.08992(14) 0.78418(15) 0.87985(15) 0.0303(6) Uani 1 1 d . . . U1 U 0.141526(18) 0.890224(18) 0.803798(18) 0.01796(12) 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 C1 0.039(7) 0.020(6) 0.031(7) 0.009(5) -0.003(5) -0.019(5) C2 0.044(7) 0.049(8) 0.042(8) 0.004(7) 0.008(7) 0.004(6) C3 0.078(12) 0.049(9) 0.038(9) 0.012(7) -0.017(8) 0.000(8) C4 0.109(16) 0.033(8) 0.048(10) 0.002(7) 0.017(10) -0.030(9) C5 0.060(10) 0.046(9) 0.058(11) -0.010(8) 0.028(9) -0.018(8) C6 0.036(7) 0.021(6) 0.064(10) -0.010(6) 0.008(6) -0.009(5) C7 0.035(6) 0.022(5) 0.037(6) 0.000(6) -0.010(6) -0.008(4) C9 0.021(5) 0.023(5) 0.023(6) 0.003(4) 0.003(4) 0.006(4) C10 0.016(5) 0.015(5) 0.018(5) 0.003(4) 0.003(4) 0.002(4) C11 0.025(5) 0.022(5) 0.014(5) 0.003(4) -0.008(4) 0.002(4) C12 0.025(6) 0.031(6) 0.019(6) 0.003(5) -0.005(5) 0.001(5) C13 0.031(6) 0.039(7) 0.017(5) 0.003(5) -0.008(5) 0.003(5) C14 0.025(5) 0.025(6) 0.028(6) 0.000(5) -0.009(5) 0.004(4) C15 0.022(6) 0.024(6) 0.028(6) 0.008(5) 0.003(5) -0.005(4) C17 0.023(5) 0.023(5) 0.021(5) 0.005(5) -0.002(5) -0.001(4) C18 0.020(5) 0.026(6) 0.025(6) 0.002(5) 0.007(5) -0.001(4) C19 0.020(6) 0.033(7) 0.032(7) -0.009(5) 0.000(5) -0.005(5) C20 0.019(6) 0.029(6) 0.050(8) -0.003(5) 0.016(5) -0.003(5) C21 0.035(7) 0.031(6) 0.032(7) 0.006(5) 0.009(5) 0.010(5) C22 0.021(5) 0.022(6) 0.034(6) 0.001(5) 0.007(5) 0.000(4) C24 0.019(5) 0.035(6) 0.037(7) -0.010(6) 0.002(5) -0.001(4) C25 0.034(7) 0.038(7) 0.025(6) -0.007(5) -0.007(5) 0.001(5) C26 0.021(6) 0.030(6) 0.025(6) -0.003(5) -0.009(5) 0.002(4) C27 0.032(6) 0.031(6) 0.019(6) -0.007(5) -0.006(5) 0.010(5) C28 0.044(8) 0.044(7) 0.027(7) -0.009(6) -0.020(6) 0.014(6) C29 0.025(6) 0.050(8) 0.048(8) -0.006(7) -0.009(6) 0.016(6) C30 0.027(7) 0.045(8) 0.044(8) -0.007(6) -0.005(6) 0.005(6) C32 0.043(7) 0.039(7) 0.028(7) -0.002(5) -0.010(6) 0.023(6) C33 0.042(7) 0.025(6) 0.034(7) -0.005(5) -0.002(6) 0.018(5) C34 0.052(8) 0.028(6) 0.034(7) -0.012(6) -0.009(6) 0.015(6) C35 0.058(10) 0.032(7) 0.063(10) 0.001(7) -0.020(8) 0.008(6) C36 0.048(8) 0.029(7) 0.067(11) 0.002(7) 0.000(8) -0.002(6) C37 0.070(10) 0.043(8) 0.032(7) 0.008(6) -0.014(7) 0.005(7) C38 0.052(8) 0.033(7) 0.028(7) 0.002(6) -0.015(6) 0.016(6) C40 0.034(7) 0.073(10) 0.019(6) 0.001(7) 0.003(5) 0.016(7) C41 0.097(14) 0.034(8) 0.076(13) 0.009(8) 0.020(11) -0.020(9) C42 0.024(6) 0.077(10) 0.039(8) -0.009(7) 0.000(6) 0.012(7) C43 0.023(6) 0.047(8) 0.039(7) -0.023(6) -0.001(5) -0.002(5) N16 0.016(4) 0.025(4) 0.016(4) 0.005(4) -0.004(4) -0.001(3) N23 0.025(5) 0.023(4) 0.018(5) 0.000(4) 0.001(4) -0.005(4) N39 0.024(5) 0.038(6) 0.016(4) -0.002(4) 0.003(4) -0.006(4) O1 0.033(4) 0.023(4) 0.014(4) 0.008(3) 0.004(3) -0.006(3) O2 0.022(4) 0.031(4) 0.017(4) 0.006(3) 0.000(3) -0.001(3) O8 0.032(4) 0.029(4) 0.025(5) 0.002(3) 0.002(3) -0.008(3) O10 0.023(4) 0.038(5) 0.009(4) 0.005(3) -0.002(3) -0.007(3) O26 0.026(4) 0.034(4) 0.023(4) 0.005(3) 0.001(3) -0.001(3) O31 0.037(5) 0.038(5) 0.037(5) 0.010(4) 0.000(4) 0.018(4) Cl1 0.0263(14) 0.0370(15) 0.0276(14) 0.0116(12) -0.0016(11) -0.0029(12) U1 0.0182(2) 0.0210(2) 0.01469(17) 0.00007(16) 0.00050(16) 0.00174(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.371(18) . ? C1 C2 1.41(2) . ? C1 C7 1.489(18) . ? C2 C3 1.37(2) . ? C3 C4 1.39(3) . ? C4 C5 1.36(3) . ? C5 C6 1.39(2) . ? C7 O8 1.425(13) . ? C9 O8 1.354(13) . ? C9 C14 1.381(16) . ? C9 C10 1.452(15) . ? C10 O10 1.307(13) . ? C10 C11 1.424(15) . ? C11 C12 1.411(15) . ? C11 C15 1.441(16) . ? C12 C13 1.383(17) . ? C13 C14 1.393(17) . ? C15 N16 1.305(15) . ? C17 C18 1.395(16) . ? C17 C22 1.418(15) . ? C17 N16 1.419(13) . ? C18 C19 1.401(16) . ? C18 N23 1.440(14) . ? C19 C20 1.375(18) . ? C20 C21 1.400(19) . ? C21 C22 1.387(18) . ? C24 N23 1.284(14) . ? C24 C25 1.434(18) . ? C25 C30 1.385(18) . ? C25 C26 1.438(18) . ? C26 O26 1.302(13) . ? C26 C27 1.444(17) . ? C27 O31 1.349(15) . ? C27 C28 1.372(18) . ? C28 C29 1.39(2) . ? C29 C30 1.384(19) . ? C32 O31 1.429(14) . ? C32 C33 1.51(2) . ? C33 C38 1.398(19) . ? C33 C34 1.406(19) . ? C34 C35 1.38(2) . ? C35 C36 1.40(2) . ? C36 C37 1.35(2) . ? C37 C38 1.38(2) . ? C40 N39 1.483(14) . ? C41 N39 1.465(18) . ? C42 N39 1.521(16) . ? C43 N39 1.465(15) . ? N16 U1 2.624(9) . ? N23 U1 2.618(9) . ? O1 U1 1.759(8) . ? O2 U1 1.765(8) . ? O10 U1 2.263(7) . ? O26 U1 2.257(8) . ? Cl1 U1 2.713(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(12) . . ? C6 C1 C7 120.8(12) . . ? C2 C1 C7 120.2(11) . . ? C3 C2 C1 120.1(14) . . ? C2 C3 C4 120.4(16) . . ? C5 C4 C3 119.3(15) . . ? C4 C5 C6 121.0(15) . . ? C1 C6 C5 120.3(15) . . ? O8 C7 C1 108.5(10) . . ? O8 C9 C14 126.5(10) . . ? O8 C9 C10 113.8(9) . . ? C14 C9 C10 119.7(10) . . ? O10 C10 C11 122.5(9) . . ? O10 C10 C9 119.8(9) . . ? C11 C10 C9 117.6(9) . . ? C12 C11 C10 121.0(10) . . ? C12 C11 C15 118.1(10) . . ? C10 C11 C15 120.8(10) . . ? C13 C12 C11 119.1(10) . . ? C12 C13 C14 121.5(11) . . ? C9 C14 C13 120.9(11) . . ? N16 C15 C11 127.3(10) . . ? C18 C17 C22 118.3(10) . . ? C18 C17 N16 117.5(9) . . ? C22 C17 N16 124.1(10) . . ? C17 C18 C19 120.5(10) . . ? C17 C18 N23 117.5(9) . . ? C19 C18 N23 122.0(10) . . ? C20 C19 C18 121.3(11) . . ? C19 C20 C21 118.6(11) . . ? C22 C21 C20 121.4(11) . . ? C21 C22 C17 119.9(11) . . ? N23 C24 C25 127.7(11) . . ? C30 C25 C24 119.5(12) . . ? C30 C25 C26 120.5(12) . . ? C24 C25 C26 120.0(11) . . ? O26 C26 C25 122.7(10) . . ? O26 C26 C27 120.8(11) . . ? C25 C26 C27 116.5(10) . . ? O31 C27 C28 127.1(11) . . ? O31 C27 C26 112.4(10) . . ? C28 C27 C26 120.4(12) . . ? C27 C28 C29 122.1(12) . . ? C30 C29 C28 118.6(12) . . ? C29 C30 C25 121.9(14) . . ? O31 C32 C33 107.2(10) . . ? C38 C33 C34 119.5(14) . . ? C38 C33 C32 120.0(12) . . ? C34 C33 C32 120.5(12) . . ? C35 C34 C33 119.6(13) . . ? C34 C35 C36 119.7(14) . . ? C37 C36 C35 120.7(15) . . ? C36 C37 C38 120.4(14) . . ? C37 C38 C33 119.8(13) . . ? C15 N16 C17 117.5(10) . . ? C15 N16 U1 126.0(7) . . ? C17 N16 U1 116.2(7) . . ? C24 N23 C18 118.3(10) . . ? C24 N23 U1 126.1(8) . . ? C18 N23 U1 115.4(6) . . ? C43 N39 C41 110.3(12) . . ? C43 N39 C40 110.0(10) . . ? C41 N39 C40 108.5(12) . . ? C43 N39 C42 109.5(10) . . ? C41 N39 C42 109.1(12) . . ? C40 N39 C42 109.3(10) . . ? C9 O8 C7 117.7(9) . . ? C10 O10 U1 133.4(7) . . ? C26 O26 U1 133.2(7) . . ? C27 O31 C32 119.4(10) . . ? O1 U1 O2 176.7(3) . . ? O1 U1 O26 89.8(3) . . ? O2 U1 O26 90.2(3) . . ? O1 U1 O10 88.9(3) . . ? O2 U1 O10 92.1(3) . . ? O26 U1 O10 161.1(3) . . ? O1 U1 N23 86.6(3) . . ? O2 U1 N23 90.4(3) . . ? O26 U1 N23 68.1(3) . . ? O10 U1 N23 130.6(3) . . ? O1 U1 N16 87.0(3) . . ? O2 U1 N16 90.5(3) . . ? O26 U1 N16 130.5(3) . . ? O10 U1 N16 68.3(3) . . ? N23 U1 N16 62.4(3) . . ? O1 U1 Cl1 93.2(2) . . ? O2 U1 Cl1 90.1(2) . . ? O26 U1 Cl1 81.3(2) . . ? O10 U1 Cl1 80.0(2) . . ? N23 U1 Cl1 149.3(2) . . ? N16 U1 Cl1 148.28(18) . . ? 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 C3 1(2) . . . . ? C7 C1 C2 C3 177.4(13) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C2 C1 C6 C5 -0.5(19) . . . . ? C7 C1 C6 C5 -177.4(12) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C6 C1 C7 O8 112.0(12) . . . . ? C2 C1 C7 O8 -64.9(15) . . . . ? O8 C9 C10 O10 -2.6(13) . . . . ? C14 C9 C10 O10 177.6(10) . . . . ? O8 C9 C10 C11 -179.2(9) . . . . ? C14 C9 C10 C11 1.0(14) . . . . ? O10 C10 C11 C12 -175.2(10) . . . . ? C9 C10 C11 C12 1.3(15) . . . . ? O10 C10 C11 C15 2.5(16) . . . . ? C9 C10 C11 C15 179.0(10) . . . . ? C10 C11 C12 C13 -2.4(17) . . . . ? C15 C11 C12 C13 179.8(11) . . . . ? C11 C12 C13 C14 1.3(17) . . . . ? O8 C9 C14 C13 178.0(10) . . . . ? C10 C9 C14 C13 -2.2(16) . . . . ? C12 C13 C14 C9 1.1(17) . . . . ? C12 C11 C15 N16 -169.6(11) . . . . ? C10 C11 C15 N16 12.6(18) . . . . ? C22 C17 C18 C19 -1.0(16) . . . . ? N16 C17 C18 C19 -177.3(10) . . . . ? C22 C17 C18 N23 178.2(10) . . . . ? N16 C17 C18 N23 1.9(15) . . . . ? C17 C18 C19 C20 -1.2(17) . . . . ? N23 C18 C19 C20 179.7(10) . . . . ? C18 C19 C20 C21 2.2(17) . . . . ? C19 C20 C21 C22 -1.0(18) . . . . ? C20 C21 C22 C17 -1.2(18) . . . . ? C18 C17 C22 C21 2.2(17) . . . . ? N16 C17 C22 C21 178.2(11) . . . . ? N23 C24 C25 C30 168.5(12) . . . . ? N23 C24 C25 C26 -12.8(19) . . . . ? C30 C25 C26 O26 177.6(11) . . . . ? C24 C25 C26 O26 -1.1(17) . . . . ? C30 C25 C26 C27 -0.1(17) . . . . ? C24 C25 C26 C27 -178.8(11) . . . . ? O26 C26 C27 O31 4.4(15) . . . . ? C25 C26 C27 O31 -177.9(10) . . . . ? O26 C26 C27 C28 -178.0(11) . . . . ? C25 C26 C27 C28 -0.3(16) . . . . ? O31 C27 C28 C29 177.3(12) . . . . ? C26 C27 C28 C29 0.1(18) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C28 C29 C30 C25 -1(2) . . . . ? C24 C25 C30 C29 179.4(12) . . . . ? C26 C25 C30 C29 0.7(19) . . . . ? O31 C32 C33 C38 -139.8(11) . . . . ? O31 C32 C33 C34 37.1(15) . . . . ? C38 C33 C34 C35 0.3(18) . . . . ? C32 C33 C34 C35 -176.7(12) . . . . ? C33 C34 C35 C36 1(2) . . . . ? C34 C35 C36 C37 -4(2) . . . . ? C35 C36 C37 C38 5(2) . . . . ? C36 C37 C38 C33 -4(2) . . . . ? C34 C33 C38 C37 1.1(18) . . . . ? C32 C33 C38 C37 178.1(12) . . . . ? C11 C15 N16 C17 -175.3(11) . . . . ? C11 C15 N16 U1 11.0(16) . . . . ? C18 C17 N16 C15 -150.0(10) . . . . ? C22 C17 N16 C15 33.9(15) . . . . ? C18 C17 N16 U1 24.4(12) . . . . ? C22 C17 N16 U1 -151.7(9) . . . . ? C25 C24 N23 C18 173.2(11) . . . . ? C25 C24 N23 U1 -12.4(18) . . . . ? C17 C18 N23 C24 147.8(11) . . . . ? C19 C18 N23 C24 -33.0(15) . . . . ? C17 C18 N23 U1 -27.1(12) . . . . ? C19 C18 N23 U1 152.1(8) . . . . ? C14 C9 O8 C7 7.6(15) . . . . ? C10 C9 O8 C7 -172.3(9) . . . . ? C1 C7 O8 C9 -178.6(9) . . . . ? C11 C10 O10 U1 -52.0(14) . . . . ? C9 C10 O10 U1 131.6(8) . . . . ? C25 C26 O26 U1 50.9(15) . . . . ? C27 C26 O26 U1 -131.5(9) . . . . ? C28 C27 O31 C32 -2.7(17) . . . . ? C26 C27 O31 C32 174.7(10) . . . . ? C33 C32 O31 C27 -174.5(10) . . . . ? C26 O26 U1 O1 33.1(10) . . . . ? C26 O26 U1 O2 -143.6(10) . . . . ? C26 O26 U1 O10 119.4(11) . . . . ? C26 O26 U1 N23 -53.2(10) . . . . ? C26 O26 U1 N16 -52.7(11) . . . . ? C26 O26 U1 Cl1 126.4(10) . . . . ? C10 O10 U1 O1 -34.1(9) . . . . ? C10 O10 U1 O2 142.8(9) . . . . ? C10 O10 U1 O26 -120.4(11) . . . . ? C10 O10 U1 N23 50.5(10) . . . . ? C10 O10 U1 N16 53.1(9) . . . . ? C10 O10 U1 Cl1 -127.4(9) . . . . ? C24 N23 U1 O1 -59.1(10) . . . . ? C18 N23 U1 O1 115.4(7) . . . . ? C24 N23 U1 O2 122.2(10) . . . . ? C18 N23 U1 O2 -63.3(7) . . . . ? C24 N23 U1 O26 32.1(9) . . . . ? C18 N23 U1 O26 -153.4(8) . . . . ? C24 N23 U1 O10 -144.7(9) . . . . ? C18 N23 U1 O10 29.8(8) . . . . ? C24 N23 U1 N16 -147.4(10) . . . . ? C18 N23 U1 N16 27.1(7) . . . . ? C24 N23 U1 Cl1 31.3(12) . . . . ? C18 N23 U1 Cl1 -154.2(6) . . . . ? C15 N16 U1 O1 59.6(9) . . . . ? C17 N16 U1 O1 -114.2(7) . . . . ? C15 N16 U1 O2 -122.5(9) . . . . ? C17 N16 U1 O2 63.6(7) . . . . ? C15 N16 U1 O26 146.8(8) . . . . ? C17 N16 U1 O26 -27.0(8) . . . . ? C15 N16 U1 O10 -30.5(8) . . . . ? C17 N16 U1 O10 155.7(7) . . . . ? C15 N16 U1 N23 147.3(9) . . . . ? C17 N16 U1 N23 -26.5(7) . . . . ? C15 N16 U1 Cl1 -31.5(11) . . . . ? C17 N16 U1 Cl1 154.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.624 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.203 #===END data_2(2)*TBACl(2) _database_code_CSD 215273 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H26 Cl N2 O6 U * C16 H36 N' _chemical_formula_sum 'C50 H62 Cl1 N3 O6 U' _chemical_formula_weight 1074.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.3226(1) _cell_length_b 18.2936(1) _cell_length_c 20.3692(2) _cell_angle_alpha 94.6846(3) _cell_angle_beta 104.4632(3) _cell_angle_gamma 91.9727(3) _cell_volume 4783.22(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 3.499 _exptl_absorpt_correction_type platmulabs _exptl_absorpt_correction_T_min 0.2736 _exptl_absorpt_correction_T_max 0.3350 _exptl_absorpt_process_details 'R. H. Blessing, Acta Crystallogr.A 1995, 51, 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56033 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.28 _reflns_number_total 23316 _reflns_number_gt 17779 _reflns_threshold_expression >2sigma(I) _computing_data_collection collect _computing_cell_refinement denzo-smn _computing_data_reduction denzo-smn _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0109P)^2^+7.1894P] 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 23316 _refine_ls_number_parameters 1107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2A C 0.4826(3) 0.6474(2) 0.9798(2) 0.0377(10) Uani 1 1 d . . . H2A H 0.5116 0.6562 1.0275 0.045 Uiso 1 1 calc R . . C2B C 0.0039(3) 0.14445(19) 0.97634(19) 0.0297(8) Uani 1 1 d . . . H2B H 0.0117 0.1524 1.0241 0.036 Uiso 1 1 calc R . . C3A C 0.5339(3) 0.6854(2) 0.9373(2) 0.0381(10) Uani 1 1 d . . . C3B C -0.0776(3) 0.18194(19) 0.9344(2) 0.0305(8) Uani 1 1 d . . . C4A C 0.5095(3) 0.66839(19) 0.8659(2) 0.0358(9) Uani 1 1 d . . . C4B C -0.1059(3) 0.16851(18) 0.86248(19) 0.0280(8) Uani 1 1 d . . . C5A C 0.5656(3) 0.7078(2) 0.8280(3) 0.0420(11) Uani 1 1 d . . . C5B C -0.1872(3) 0.20939(19) 0.8257(2) 0.0324(9) Uani 1 1 d . . . C6A C 0.6408(3) 0.7621(2) 0.8612(3) 0.0512(13) Uani 1 1 d . . . H6A H 0.6767 0.7891 0.8354 0.061 Uiso 1 1 calc R . . C6B C -0.2351(3) 0.2597(2) 0.8594(2) 0.0410(10) Uani 1 1 d . . . H6B H -0.2877 0.2874 0.8338 0.049 Uiso 1 1 calc R . . C7A C 0.6647(3) 0.7776(2) 0.9319(3) 0.0569(14) Uani 1 1 d . . . H7A H 0.7171 0.8143 0.9540 0.068 Uiso 1 1 calc R . . C7B C -0.2084(3) 0.2711(2) 0.9301(3) 0.0439(11) Uani 1 1 d . . . H7B H -0.2434 0.3055 0.9525 0.053 Uiso 1 1 calc R . . C8A C 0.6123(3) 0.7395(2) 0.9687(3) 0.0482(12) Uani 1 1 d . . . H8A H 0.6290 0.7498 1.0168 0.058 Uiso 1 1 calc R . . C8B C -0.1315(3) 0.2325(2) 0.9670(2) 0.0388(9) Uani 1 1 d . . . H8B H -0.1140 0.2398 1.0153 0.047 Uiso 1 1 calc R . . C11A C 0.5438(3) 0.6241(2) 0.7275(2) 0.0444(11) Uani 1 1 d . . . H11A H 0.4818 0.5945 0.7306 0.053 Uiso 1 1 calc R . . H11B H 0.6065 0.6004 0.7516 0.053 Uiso 1 1 calc R . . C11B C -0.2453(3) 0.1318(2) 0.7210(2) 0.0358(9) Uani 1 1 d . . . H11C H -0.2850 0.1036 0.7466 0.043 Uiso 1 1 calc R . . H11D H -0.1833 0.1048 0.7177 0.043 Uiso 1 1 calc R . . C12A C 0.5440(4) 0.6285(3) 0.6546(3) 0.0494(12) Uani 1 1 d . . . C12B C -0.3118(3) 0.1403(2) 0.6508(2) 0.0365(9) Uani 1 1 d . . . C13A C 0.6103(4) 0.6787(3) 0.6365(3) 0.0675(15) Uani 1 1 d . . . H13A H 0.6544 0.7127 0.6700 0.081 Uiso 1 1 calc R . . C13B C -0.3832(3) 0.1944(2) 0.6396(2) 0.0456(11) Uani 1 1 d . . . H13B H -0.3899 0.2276 0.6764 0.055 Uiso 1 1 calc R . . C14A C 0.6112(6) 0.6784(4) 0.5675(4) 0.088(2) Uani 1 1 d . . . H14A H 0.6569 0.7118 0.5542 0.106 Uiso 1 1 calc R . . C14B C -0.4449(4) 0.1997(3) 0.5743(3) 0.0629(15) Uani 1 1 d . . . H14B H -0.4935 0.2369 0.5665 0.075 Uiso 1 1 calc R . . C15A C 0.5458(7) 0.6299(5) 0.5197(4) 0.095(2) Uani 1 1 d . . . H15A H 0.5474 0.6298 0.4733 0.113 Uiso 1 1 calc R . . C15B C -0.4360(5) 0.1518(4) 0.5211(3) 0.0822(19) Uani 1 1 d . . . H15B H -0.4792 0.1553 0.4768 0.099 Uiso 1 1 calc R . . C16A C 0.4784(6) 0.5815(4) 0.5371(3) 0.085(2) Uani 1 1 d . . . H16A H 0.4326 0.5489 0.5032 0.101 Uiso 1 1 calc R . . C16B C -0.3654(5) 0.0987(4) 0.5314(3) 0.0838(19) Uani 1 1 d . . . H16B H -0.3589 0.0658 0.4943 0.101 Uiso 1 1 calc R . . C17A C 0.4779(4) 0.5807(3) 0.6050(3) 0.0631(14) Uani 1 1 d . . . H17A H 0.4318 0.5470 0.6177 0.076 Uiso 1 1 calc R . . C17B C -0.3028(4) 0.0933(3) 0.5968(3) 0.0611(14) Uani 1 1 d . . . H17B H -0.2535 0.0566 0.6039 0.073 Uiso 1 1 calc R . . C18A C -0.0709(4) 0.5989(2) 0.5863(2) 0.0509(12) Uani 1 1 d . . . C18B C 0.2290(3) 0.0944(2) 0.58739(19) 0.0329(8) Uani 1 1 d . . . C19A C -0.1132(5) 0.6579(3) 0.5554(3) 0.0663(15) Uani 1 1 d . . . H19A H -0.1015 0.7050 0.5802 0.080 Uiso 1 1 calc R . . C19B C 0.1569(3) 0.0380(2) 0.5553(2) 0.0399(10) Uani 1 1 d . . . H19B H 0.1245 0.0088 0.5816 0.048 Uiso 1 1 calc R . . C20A C -0.1733(5) 0.6510(4) 0.4880(3) 0.0821(19) Uani 1 1 d . . . H20A H -0.2016 0.6929 0.4673 0.099 Uiso 1 1 calc R . . C20B C 0.1319(3) 0.0240(2) 0.4853(2) 0.0473(11) Uani 1 1 d . . . H20B H 0.0833 -0.0153 0.4639 0.057 Uiso 1 1 calc R . . C21A C -0.1908(5) 0.5838(4) 0.4527(3) 0.081(2) Uani 1 1 d . . . H21A H -0.2324 0.5783 0.4071 0.098 Uiso 1 1 calc R . . C21B C 0.1760(4) 0.0659(3) 0.4465(2) 0.0498(12) Uani 1 1 d . . . H21B H 0.1578 0.0564 0.3984 0.060 Uiso 1 1 calc R . . C22A C -0.1499(7) 0.5259(3) 0.4817(3) 0.125(4) Uani 1 1 d . . . H22A H -0.1629 0.4789 0.4567 0.150 Uiso 1 1 calc R . . C22B C 0.2472(4) 0.1221(3) 0.4780(3) 0.0616(14) Uani 1 1 d . . . H22B H 0.2784 0.1517 0.4515 0.074 Uiso 1 1 calc R . . C23A C -0.0876(7) 0.5327(3) 0.5488(3) 0.121(3) Uani 1 1 d . . . H23A H -0.0569 0.4907 0.5681 0.145 Uiso 1 1 calc R . . C23B C 0.2737(4) 0.1356(3) 0.5481(2) 0.0546(12) Uani 1 1 d . . . H23B H 0.3236 0.1742 0.5693 0.066 Uiso 1 1 calc R . . C24A C -0.0114(4) 0.6067(3) 0.6599(2) 0.0574(13) Uani 1 1 d . . . H24A H 0.0573 0.5857 0.6650 0.069 Uiso 1 1 calc R . . H24B H -0.0006 0.6592 0.6775 0.069 Uiso 1 1 calc R . . C24B C 0.2558(3) 0.1120(3) 0.6632(2) 0.0440(10) Uani 1 1 d . . . H24C H 0.2792 0.1645 0.6751 0.053 Uiso 1 1 calc R . . H24D H 0.1941 0.1026 0.6807 0.053 Uiso 1 1 calc R . . C26A C -0.0627(3) 0.5948(2) 0.7629(2) 0.0319(8) Uani 1 1 d . . . C26B C 0.3844(3) 0.08872(18) 0.76050(18) 0.0270(8) Uani 1 1 d . . . C27A C 0.0272(3) 0.58298(18) 0.81489(19) 0.0281(8) Uani 1 1 d . . . C27B C 0.3319(3) 0.07783(17) 0.81219(17) 0.0234(7) Uani 1 1 d . . . C28A C 0.0248(3) 0.6067(2) 0.88316(19) 0.0313(8) Uani 1 1 d . . . C28B C 0.3882(3) 0.09967(18) 0.88042(19) 0.0274(8) Uani 1 1 d . . . C29A C -0.0620(3) 0.6404(2) 0.8961(2) 0.0398(10) Uani 1 1 d . . . H29A H -0.0625 0.6552 0.9418 0.048 Uiso 1 1 calc R . . C29B C 0.4899(3) 0.1317(2) 0.8949(2) 0.0329(8) Uani 1 1 d . . . H29B H 0.5262 0.1460 0.9408 0.040 Uiso 1 1 calc R . . C30A C -0.1462(3) 0.6525(2) 0.8445(2) 0.0472(11) Uani 1 1 d . . . H30A H -0.2039 0.6765 0.8540 0.057 Uiso 1 1 calc R . . C30B C 0.5369(3) 0.1423(2) 0.8436(2) 0.0390(10) Uani 1 1 d . . . H30B H 0.6052 0.1645 0.8539 0.047 Uiso 1 1 calc R . . C31A C -0.1453(3) 0.6289(2) 0.7782(2) 0.0427(10) Uani 1 1 d . . . H31A H -0.2037 0.6366 0.7422 0.051 Uiso 1 1 calc R . . C31B C 0.4842(3) 0.1202(2) 0.7760(2) 0.0341(9) Uani 1 1 d . . . H31B H 0.5174 0.1269 0.7405 0.041 Uiso 1 1 calc R . . C33A C 0.1060(3) 0.59148(19) 0.94079(19) 0.0312(8) Uani 1 1 d . . . H33A H 0.0909 0.5973 0.9840 0.037 Uiso 1 1 calc R . . C33B C 0.3479(3) 0.08592(18) 0.93775(18) 0.0269(8) Uani 1 1 d . . . H33B H 0.3959 0.0921 0.9812 0.032 Uiso 1 1 calc R . . C35A C 0.2627(3) 0.55130(19) 1.00188(18) 0.0319(9) Uani 1 1 d . . . C35B C 0.2320(3) 0.04786(18) 0.99854(17) 0.0269(8) Uani 1 1 d . . . C36A C 0.2266(4) 0.5179(2) 1.0511(2) 0.0419(10) Uani 1 1 d . . . H36A H 0.1543 0.5074 1.0446 0.050 Uiso 1 1 calc R . . C36B C 0.3016(3) 0.0141(2) 1.04824(19) 0.0345(9) Uani 1 1 d . . . H36B H 0.3671 0.0017 1.0413 0.041 Uiso 1 1 calc R . . C37A C 0.2965(4) 0.4999(2) 1.1102(2) 0.0467(11) Uani 1 1 d . . . H37A H 0.2715 0.4782 1.1443 0.056 Uiso 1 1 calc R . . C37B C 0.2762(3) -0.0017(2) 1.1074(2) 0.0387(10) Uani 1 1 d . . . H37B H 0.3249 -0.0236 1.1415 0.046 Uiso 1 1 calc R . . C38A C 0.4014(4) 0.5134(2) 1.1189(2) 0.0498(12) Uani 1 1 d . . . H38A H 0.4486 0.5005 1.1589 0.060 Uiso 1 1 calc R . . C38B C 0.1807(3) 0.0142(2) 1.11716(19) 0.0379(10) Uani 1 1 d . . . H38B H 0.1632 0.0026 1.1577 0.045 Uiso 1 1 calc R . . C39A C 0.4385(3) 0.5457(2) 1.0702(2) 0.0421(10) Uani 1 1 d . . . H39A H 0.5113 0.5537 1.0762 0.051 Uiso 1 1 calc R . . C39B C 0.1098(3) 0.0472(2) 1.06814(19) 0.0343(9) Uani 1 1 d . . . H39B H 0.0436 0.0576 1.0749 0.041 Uiso 1 1 calc R . . C40A C 0.3696(3) 0.56677(19) 1.01171(18) 0.0321(9) Uani 1 1 d . . . C40B C 0.1356(3) 0.06510(18) 1.00878(17) 0.0263(8) Uani 1 1 d . . . C42A C 0.3727(3) 0.89014(19) 0.6970(2) 0.0337(9) Uani 1 1 d . . . H42A H 0.3434 0.8953 0.6480 0.040 Uiso 1 1 calc R . . H42B H 0.3704 0.9384 0.7222 0.040 Uiso 1 1 calc R . . C42B C -0.0051(3) 0.25871(18) 0.68303(19) 0.0311(8) Uani 1 1 d . . . H42C H 0.0386 0.2226 0.7087 0.037 Uiso 1 1 calc R . . H42D H -0.0785 0.2437 0.6798 0.037 Uiso 1 1 calc R . . C43A C 0.4848(3) 0.8719(2) 0.7073(2) 0.0394(10) Uani 1 1 d . . . H43A H 0.4887 0.8247 0.6809 0.047 Uiso 1 1 calc R . . H43B H 0.5152 0.8662 0.7561 0.047 Uiso 1 1 calc R . . C43B C 0.0109(3) 0.2552(2) 0.6115(2) 0.0356(9) Uani 1 1 d . . . H43C H 0.0862 0.2567 0.6141 0.043 Uiso 1 1 calc R . . H43D H -0.0185 0.2984 0.5889 0.043 Uiso 1 1 calc R . . C44A C 0.5472(4) 0.9317(2) 0.6848(3) 0.0507(12) Uani 1 1 d . . . H44A H 0.5164 0.9375 0.6361 0.061 Uiso 1 1 calc R . . H44B H 0.5429 0.9789 0.7112 0.061 Uiso 1 1 calc R . . C44B C -0.0414(4) 0.1849(2) 0.5695(2) 0.0410(10) Uani 1 1 d . . . H44C H -0.0132 0.1418 0.5927 0.049 Uiso 1 1 calc R . . H44D H -0.1169 0.1840 0.5659 0.049 Uiso 1 1 calc R . . C45A C 0.6600(4) 0.9147(3) 0.6946(3) 0.0626(14) Uani 1 1 d . . . H45A H 0.6911 0.9096 0.7428 0.094 Uiso 1 1 calc R . . H45B H 0.6972 0.9548 0.6798 0.094 Uiso 1 1 calc R . . H45C H 0.6647 0.8688 0.6675 0.094 Uiso 1 1 calc R . . C45B C -0.0233(4) 0.1800(2) 0.4984(2) 0.0522(12) Uani 1 1 d . . . H45D H -0.0494 0.2233 0.4758 0.078 Uiso 1 1 calc R . . H45E H -0.0601 0.1356 0.4719 0.078 Uiso 1 1 calc R . . H45F H 0.0512 0.1779 0.5018 0.078 Uiso 1 1 calc R . . C46A C 0.2999(3) 0.75939(19) 0.68096(19) 0.0330(9) Uani 1 1 d . . . H46A H 0.3665 0.7368 0.6988 0.040 Uiso 1 1 calc R . . H46B H 0.2443 0.7282 0.6909 0.040 Uiso 1 1 calc R . . C46B C 0.1243(3) 0.36669(19) 0.71890(19) 0.0290(8) Uani 1 1 d . . . H46C H 0.1338 0.4175 0.7411 0.035 Uiso 1 1 calc R . . H46D H 0.1223 0.3695 0.6703 0.035 Uiso 1 1 calc R . . C47A C 0.2808(4) 0.7589(2) 0.6041(2) 0.0470(11) Uani 1 1 d . . . H47A H 0.2262 0.7931 0.5872 0.056 Uiso 1 1 calc R . . H47B H 0.3452 0.7765 0.5930 0.056 Uiso 1 1 calc R . . C47B C 0.2184(3) 0.3246(2) 0.7513(2) 0.0339(9) Uani 1 1 d . . . H47C H 0.2351 0.3349 0.8014 0.041 Uiso 1 1 calc R . . H47D H 0.2016 0.2712 0.7400 0.041 Uiso 1 1 calc R . . C48A C 0.2480(4) 0.6840(2) 0.5688(2) 0.0534(12) Uani 1 1 d . . . H48A H 0.1786 0.6699 0.5746 0.064 Uiso 1 1 calc R . . H48B H 0.2970 0.6487 0.5913 0.064 Uiso 1 1 calc R . . C48B C 0.3119(3) 0.3466(2) 0.7260(2) 0.0418(10) Uani 1 1 d . . . H48C H 0.3194 0.4008 0.7284 0.050 Uiso 1 1 calc R . . H48D H 0.3002 0.3273 0.6776 0.050 Uiso 1 1 calc R . . C49A C 0.2432(4) 0.6767(3) 0.4944(2) 0.0572(13) Uani 1 1 d . . . H49A H 0.1984 0.7134 0.4719 0.086 Uiso 1 1 calc R . . H49B H 0.2148 0.6274 0.4746 0.086 Uiso 1 1 calc R . . H49C H 0.3131 0.6844 0.4881 0.086 Uiso 1 1 calc R . . C49B C 0.4114(4) 0.3179(3) 0.7671(3) 0.0618(14) Uani 1 1 d . . . H49D H 0.4275 0.3412 0.8139 0.093 Uiso 1 1 calc R . . H49E H 0.4684 0.3294 0.7465 0.093 Uiso 1 1 calc R . . H49F H 0.4025 0.2645 0.7676 0.093 Uiso 1 1 calc R . . C50A C 0.1952(3) 0.86479(19) 0.70540(19) 0.0318(9) Uani 1 1 d . . . H50A H 0.2023 0.9176 0.7217 0.038 Uiso 1 1 calc R . . H50B H 0.1655 0.8609 0.6555 0.038 Uiso 1 1 calc R . . C50B C -0.0610(3) 0.38789(19) 0.69588(19) 0.0309(8) Uani 1 1 d . . . H50C H -0.0395 0.4364 0.7219 0.037 Uiso 1 1 calc R . . H50D H -0.0611 0.3935 0.6479 0.037 Uiso 1 1 calc R . . C51A C 0.1184(3) 0.8274(2) 0.7374(2) 0.0403(10) Uani 1 1 d . . . H51A H 0.1353 0.8430 0.7868 0.048 Uiso 1 1 calc R . . H51B H 0.1230 0.7735 0.7316 0.048 Uiso 1 1 calc R . . C51B C -0.1706(3) 0.3674(2) 0.6985(2) 0.0365(9) Uani 1 1 d . . . H51C H -0.1703 0.3546 0.7448 0.044 Uiso 1 1 calc R . . H51D H -0.1978 0.3237 0.6662 0.044 Uiso 1 1 calc R . . C52A C 0.0087(3) 0.8476(2) 0.7038(3) 0.0484(11) Uani 1 1 d . . . H52A H 0.0074 0.9016 0.7031 0.058 Uiso 1 1 calc R . . H52B H -0.0116 0.8253 0.6561 0.058 Uiso 1 1 calc R . . C52B C -0.2416(3) 0.4303(2) 0.6805(2) 0.0441(10) Uani 1 1 d . . . H52C H -0.2142 0.4738 0.7131 0.053 Uiso 1 1 calc R . . H52D H -0.2408 0.4434 0.6344 0.053 Uiso 1 1 calc R . . C53A C -0.0693(4) 0.8214(3) 0.7412(4) 0.0770(18) Uani 1 1 d . . . H53A H -0.0688 0.7679 0.7417 0.116 Uiso 1 1 calc R . . H53B H -0.1389 0.8349 0.7180 0.116 Uiso 1 1 calc R . . H53C H -0.0506 0.8445 0.7881 0.116 Uiso 1 1 calc R . . C53B C -0.3527(4) 0.4118(3) 0.6821(3) 0.0642(15) Uani 1 1 d . . . H53D H -0.3823 0.3712 0.6474 0.096 Uiso 1 1 calc R . . H53E H -0.3937 0.4549 0.6727 0.096 Uiso 1 1 calc R . . H53F H -0.3539 0.3972 0.7271 0.096 Uiso 1 1 calc R . . C54A C 0.3451(3) 0.82520(18) 0.79476(18) 0.0290(8) Uani 1 1 d . . . H54A H 0.2962 0.7911 0.8083 0.035 Uiso 1 1 calc R . . H54B H 0.4123 0.8018 0.8011 0.035 Uiso 1 1 calc R . . C54B C 0.0222(3) 0.32135(18) 0.79647(17) 0.0275(8) Uani 1 1 d . . . H54C H 0.0796 0.2895 0.8139 0.033 Uiso 1 1 calc R . . H54D H -0.0435 0.2946 0.7968 0.033 Uiso 1 1 calc R . . C55A C 0.3608(3) 0.8952(2) 0.8419(2) 0.0352(9) Uani 1 1 d . . . H55A H 0.2981 0.9239 0.8304 0.042 Uiso 1 1 calc R . . H55B H 0.4203 0.9254 0.8358 0.042 Uiso 1 1 calc R . . C55B C 0.0357(3) 0.39101(19) 0.84468(18) 0.0330(9) Uani 1 1 d . . . H55C H -0.0289 0.4178 0.8345 0.040 Uiso 1 1 calc R . . H55D H 0.0926 0.4234 0.8378 0.040 Uiso 1 1 calc R . . C56A C 0.3814(3) 0.8773(2) 0.91600(19) 0.0344(9) Uani 1 1 d . . . H56A H 0.4346 0.8403 0.9241 0.041 Uiso 1 1 calc R . . H56B H 0.4102 0.9223 0.9462 0.041 Uiso 1 1 calc R . . C56B C 0.0608(3) 0.3727(2) 0.91870(19) 0.0363(9) Uani 1 1 d . . . H56C H 0.0543 0.4171 0.9482 0.044 Uiso 1 1 calc R . . H56D H 0.0093 0.3345 0.9236 0.044 Uiso 1 1 calc R . . C57A C 0.2861(4) 0.8483(2) 0.9351(2) 0.0484(11) Uani 1 1 d . . . H57A H 0.2314 0.8833 0.9247 0.073 Uiso 1 1 calc R . . H57B H 0.3034 0.8420 0.9839 0.073 Uiso 1 1 calc R . . H57C H 0.2615 0.8009 0.9090 0.073 Uiso 1 1 calc R . . C57B C 0.1694(4) 0.3454(3) 0.9428(2) 0.0483(11) Uani 1 1 d . . . H57D H 0.1726 0.2970 0.9192 0.073 Uiso 1 1 calc R . . H57E H 0.1854 0.3416 0.9920 0.073 Uiso 1 1 calc R . . H57F H 0.2200 0.3800 0.9327 0.073 Uiso 1 1 calc R . . N1A N 0.4016(2) 0.60257(16) 0.96045(16) 0.0305(7) Uani 1 1 d . . . N1B N 0.0680(2) 0.10104(15) 0.95686(15) 0.0256(6) Uani 1 1 d . . . N34A N 0.1972(2) 0.57078(15) 0.93988(15) 0.0284(7) Uani 1 1 d . . . N34B N 0.2536(2) 0.06615(15) 0.93659(14) 0.0251(6) Uani 1 1 d . . . N41A N 0.3036(2) 0.83523(15) 0.71923(15) 0.0289(7) Uani 1 1 d . . . N41B N 0.0202(2) 0.33389(15) 0.72342(15) 0.0259(6) Uani 1 1 d . . . O1A O 0.2463(2) 0.67208(13) 0.83868(14) 0.0351(6) Uani 1 1 d . . . O1B O 0.06119(19) -0.01697(12) 0.84201(12) 0.0286(5) Uani 1 1 d . . . O2A O 0.30762(19) 0.48443(13) 0.84573(13) 0.0306(6) Uani 1 1 d . . . O2B O 0.14295(19) 0.16934(12) 0.83583(13) 0.0292(6) Uani 1 1 d . . . O9A O 0.4396(2) 0.61645(14) 0.83507(14) 0.0375(6) Uani 1 1 d . . . O9B O -0.06095(19) 0.12016(13) 0.83045(13) 0.0317(6) Uani 1 1 d . . . O10A O 0.5427(2) 0.69819(15) 0.75835(17) 0.0449(7) Uani 1 1 d . . . O10B O -0.2140(2) 0.20403(14) 0.75562(14) 0.0365(6) Uani 1 1 d . . . O25A O -0.0709(2) 0.56829(14) 0.69656(13) 0.0380(7) Uani 1 1 d . . . O25B O 0.3374(2) 0.06630(13) 0.69320(12) 0.0309(6) Uani 1 1 d . . . O32A O 0.10429(18) 0.54862(12) 0.80024(12) 0.0255(5) Uani 1 1 d . . . O32B O 0.23945(18) 0.04492(12) 0.79727(12) 0.0257(5) Uani 1 1 d . . . Cl1A Cl 0.26174(8) 0.55641(6) 0.70196(5) 0.0390(2) Uani 1 1 d . . . Cl1B Cl 0.00669(7) 0.05524(5) 0.69893(5) 0.0350(2) Uani 1 1 d . . . U1A U 0.277894(10) 0.578083(6) 0.837862(7) 0.02458(4) Uani 1 1 d . . . U1B U 0.097183(10) 0.076255(6) 0.834668(6) 0.02158(4) 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 C2A 0.035(2) 0.0292(19) 0.039(2) -0.0072(17) -0.0063(18) 0.0070(16) C2B 0.034(2) 0.0276(18) 0.0274(19) -0.0028(15) 0.0115(17) -0.0070(15) C3A 0.025(2) 0.0259(18) 0.056(3) -0.0038(18) -0.0003(19) 0.0018(15) C3B 0.028(2) 0.0249(17) 0.040(2) -0.0014(16) 0.0134(17) -0.0018(14) C4A 0.023(2) 0.0229(17) 0.058(3) 0.0023(18) 0.0027(18) 0.0042(14) C4B 0.027(2) 0.0242(17) 0.036(2) 0.0032(15) 0.0141(17) -0.0018(14) C5A 0.030(2) 0.0264(19) 0.067(3) 0.007(2) 0.008(2) 0.0058(16) C5B 0.024(2) 0.0268(18) 0.047(2) 0.0054(17) 0.0099(18) -0.0016(14) C6A 0.031(2) 0.026(2) 0.100(4) 0.004(2) 0.022(3) 0.0015(16) C6B 0.027(2) 0.030(2) 0.064(3) 0.002(2) 0.009(2) 0.0028(16) C7A 0.032(3) 0.035(2) 0.096(4) -0.019(3) 0.011(3) -0.0050(18) C7B 0.031(2) 0.034(2) 0.068(3) -0.011(2) 0.020(2) 0.0019(17) C8A 0.032(2) 0.033(2) 0.070(3) -0.016(2) 0.001(2) 0.0011(17) C8B 0.033(2) 0.035(2) 0.049(3) -0.0071(19) 0.015(2) -0.0054(16) C11A 0.038(2) 0.035(2) 0.061(3) 0.011(2) 0.014(2) 0.0067(17) C11B 0.032(2) 0.035(2) 0.041(2) 0.0059(18) 0.0075(18) 0.0059(16) C12A 0.041(3) 0.052(3) 0.061(3) 0.022(2) 0.015(2) 0.019(2) C12B 0.027(2) 0.042(2) 0.041(2) 0.0100(19) 0.0086(18) 0.0020(16) C13A 0.063(4) 0.074(4) 0.076(4) 0.034(3) 0.028(3) 0.013(3) C13B 0.034(2) 0.048(2) 0.053(3) 0.014(2) 0.005(2) 0.0056(19) C14A 0.100(5) 0.090(5) 0.094(5) 0.048(4) 0.046(5) 0.026(4) C14B 0.048(3) 0.063(3) 0.072(4) 0.028(3) -0.003(3) 0.007(2) C15A 0.128(7) 0.105(6) 0.065(4) 0.027(4) 0.038(5) 0.057(5) C15B 0.079(5) 0.101(5) 0.055(4) 0.027(4) -0.010(3) 0.006(4) C16A 0.096(5) 0.083(5) 0.071(4) 0.005(4) 0.010(4) 0.038(4) C16B 0.097(5) 0.109(5) 0.041(3) 0.002(3) 0.009(3) 0.021(4) C17A 0.060(3) 0.061(3) 0.072(4) 0.012(3) 0.017(3) 0.026(3) C17B 0.068(4) 0.072(3) 0.044(3) 0.005(3) 0.013(3) 0.019(3) C18A 0.073(3) 0.047(3) 0.029(2) 0.003(2) 0.009(2) -0.018(2) C18B 0.032(2) 0.042(2) 0.0235(19) 0.0023(16) 0.0055(16) 0.0085(16) C19A 0.096(5) 0.058(3) 0.045(3) -0.003(3) 0.022(3) 0.002(3) C19B 0.048(3) 0.036(2) 0.039(2) 0.0018(18) 0.018(2) 0.0013(18) C20A 0.109(5) 0.094(5) 0.048(3) 0.022(3) 0.023(3) 0.025(4) C20B 0.041(3) 0.047(2) 0.048(3) -0.012(2) 0.006(2) 0.0002(19) C21A 0.107(5) 0.094(5) 0.036(3) 0.013(3) 0.006(3) -0.034(4) C21B 0.061(3) 0.062(3) 0.025(2) -0.001(2) 0.009(2) 0.017(2) C22A 0.245(10) 0.056(4) 0.043(3) 0.003(3) -0.013(5) -0.055(5) C22B 0.083(4) 0.064(3) 0.044(3) 0.008(2) 0.028(3) -0.012(3) C23A 0.240(10) 0.054(4) 0.046(4) 0.017(3) -0.006(5) -0.016(5) C23B 0.055(3) 0.059(3) 0.046(3) -0.004(2) 0.011(2) -0.018(2) C24A 0.053(3) 0.078(3) 0.035(2) 0.001(2) 0.005(2) -0.025(2) C24B 0.040(3) 0.060(3) 0.032(2) 0.007(2) 0.0059(19) 0.020(2) C26A 0.031(2) 0.0300(19) 0.033(2) 0.0085(16) 0.0037(17) -0.0015(15) C26B 0.031(2) 0.0248(17) 0.0266(19) 0.0052(15) 0.0079(16) 0.0059(14) C27A 0.032(2) 0.0223(16) 0.029(2) 0.0056(15) 0.0052(16) -0.0034(14) C27B 0.0258(19) 0.0198(16) 0.0249(18) 0.0029(14) 0.0060(15) 0.0046(13) C28A 0.030(2) 0.0318(19) 0.030(2) 0.0013(16) 0.0054(16) 0.0011(15) C28B 0.030(2) 0.0227(17) 0.030(2) 0.0026(15) 0.0071(16) 0.0033(14) C29A 0.036(2) 0.047(2) 0.038(2) -0.0008(19) 0.0151(19) 0.0046(18) C29B 0.026(2) 0.039(2) 0.031(2) 0.0027(17) 0.0019(17) -0.0020(15) C30A 0.032(2) 0.052(3) 0.060(3) 0.008(2) 0.016(2) 0.0089(19) C30B 0.029(2) 0.038(2) 0.046(3) 0.0047(19) 0.0031(19) -0.0006(16) C31A 0.030(2) 0.047(2) 0.048(3) 0.014(2) 0.002(2) 0.0053(18) C31B 0.032(2) 0.034(2) 0.041(2) 0.0116(17) 0.0148(18) 0.0056(16) C33A 0.037(2) 0.0289(18) 0.027(2) 0.0009(15) 0.0076(17) -0.0002(16) C33B 0.030(2) 0.0296(18) 0.0181(17) -0.0014(14) 0.0007(15) 0.0034(14) C35A 0.040(2) 0.0268(18) 0.0228(19) -0.0002(15) -0.0031(17) 0.0044(15) C35B 0.037(2) 0.0223(16) 0.0188(17) -0.0008(14) 0.0032(15) -0.0014(14) C36A 0.059(3) 0.031(2) 0.030(2) 0.0045(17) 0.002(2) -0.0014(18) C36B 0.041(2) 0.0314(19) 0.030(2) 0.0031(16) 0.0049(18) 0.0050(16) C37A 0.069(3) 0.035(2) 0.031(2) 0.0071(18) 0.003(2) 0.001(2) C37B 0.056(3) 0.033(2) 0.025(2) 0.0070(16) 0.0051(19) 0.0012(18) C38A 0.072(4) 0.040(2) 0.027(2) 0.0044(19) -0.008(2) 0.013(2) C38B 0.054(3) 0.036(2) 0.0224(19) 0.0052(16) 0.0091(19) -0.0089(18) C39A 0.044(3) 0.032(2) 0.040(2) -0.0023(18) -0.010(2) 0.0119(17) C39B 0.039(2) 0.034(2) 0.029(2) -0.0004(16) 0.0109(18) -0.0092(16) C40A 0.042(2) 0.0256(18) 0.0217(19) -0.0046(15) -0.0045(17) 0.0073(15) C40B 0.034(2) 0.0214(16) 0.0210(18) -0.0012(14) 0.0045(15) -0.0078(14) C42A 0.042(2) 0.0236(17) 0.033(2) 0.0065(16) 0.0047(18) -0.0023(15) C42B 0.038(2) 0.0237(17) 0.029(2) -0.0024(15) 0.0056(17) -0.0007(15) C43A 0.043(3) 0.037(2) 0.039(2) 0.0065(18) 0.010(2) 0.0005(17) C43B 0.041(2) 0.0318(19) 0.031(2) -0.0032(16) 0.0050(18) 0.0033(16) C44A 0.055(3) 0.047(3) 0.055(3) 0.005(2) 0.025(2) -0.005(2) C44B 0.059(3) 0.0267(19) 0.029(2) -0.0041(16) -0.003(2) 0.0052(18) C45A 0.061(3) 0.068(3) 0.067(4) 0.001(3) 0.035(3) -0.011(3) C45B 0.069(3) 0.047(3) 0.031(2) -0.005(2) -0.004(2) 0.021(2) C46A 0.040(2) 0.0248(18) 0.031(2) 0.0000(15) 0.0039(17) 0.0016(15) C46B 0.034(2) 0.0249(17) 0.0277(19) -0.0005(15) 0.0083(16) -0.0045(14) C47A 0.068(3) 0.033(2) 0.034(2) 0.0020(18) 0.002(2) 0.006(2) C47B 0.036(2) 0.0283(19) 0.035(2) 0.0014(16) 0.0058(18) 0.0015(15) C48A 0.080(4) 0.040(2) 0.036(3) -0.002(2) 0.009(2) 0.011(2) C48B 0.041(3) 0.041(2) 0.045(3) -0.0045(19) 0.015(2) 0.0040(18) C49A 0.079(4) 0.050(3) 0.034(2) -0.007(2) -0.002(2) 0.018(2) C49B 0.036(3) 0.055(3) 0.090(4) 0.002(3) 0.008(3) 0.005(2) C50A 0.035(2) 0.0241(17) 0.031(2) 0.0029(15) -0.0042(17) 0.0068(15) C50B 0.038(2) 0.0246(17) 0.030(2) 0.0068(15) 0.0065(17) 0.0056(15) C51A 0.035(2) 0.033(2) 0.051(3) 0.0025(19) 0.008(2) 0.0037(17) C51B 0.031(2) 0.033(2) 0.043(2) 0.0067(18) 0.0046(18) 0.0024(16) C52A 0.038(3) 0.042(2) 0.059(3) -0.006(2) 0.002(2) 0.0030(18) C52B 0.040(3) 0.037(2) 0.056(3) 0.002(2) 0.012(2) 0.0061(18) C53A 0.038(3) 0.067(3) 0.125(6) -0.001(4) 0.022(3) 0.003(2) C53B 0.040(3) 0.054(3) 0.096(4) 0.004(3) 0.011(3) 0.010(2) C54A 0.032(2) 0.0243(17) 0.0274(19) 0.0060(15) 0.0000(16) 0.0041(14) C54B 0.038(2) 0.0211(16) 0.0237(18) 0.0030(14) 0.0091(16) 0.0013(14) C55A 0.039(2) 0.0270(18) 0.035(2) 0.0015(16) 0.0015(18) -0.0005(15) C55B 0.048(2) 0.0263(18) 0.027(2) 0.0028(15) 0.0135(18) 0.0042(16) C56A 0.036(2) 0.033(2) 0.028(2) -0.0009(16) -0.0016(17) 0.0034(16) C56B 0.045(2) 0.035(2) 0.029(2) 0.0005(17) 0.0102(18) -0.0007(17) C57A 0.056(3) 0.049(3) 0.037(2) -0.007(2) 0.010(2) -0.007(2) C57B 0.055(3) 0.056(3) 0.029(2) -0.003(2) 0.002(2) 0.011(2) N1A 0.0301(18) 0.0265(15) 0.0284(17) -0.0052(13) -0.0024(14) 0.0044(12) N1B 0.0288(17) 0.0250(14) 0.0224(15) 0.0013(12) 0.0063(13) -0.0028(12) N34A 0.0342(18) 0.0262(15) 0.0207(15) 0.0024(12) -0.0006(13) -0.0006(12) N34B 0.0304(17) 0.0243(14) 0.0207(15) 0.0021(12) 0.0069(13) 0.0015(12) N41A 0.0349(18) 0.0215(14) 0.0271(16) 0.0023(12) 0.0019(14) 0.0022(12) N41B 0.0339(17) 0.0205(14) 0.0226(15) 0.0007(12) 0.0065(13) 0.0002(12) O1A 0.0364(16) 0.0237(12) 0.0402(16) 0.0029(11) 0.0011(12) -0.0009(10) O1B 0.0326(14) 0.0268(12) 0.0275(13) 0.0050(10) 0.0090(11) -0.0001(10) O2A 0.0310(14) 0.0267(12) 0.0308(14) 0.0019(11) 0.0020(11) 0.0027(10) O2B 0.0330(15) 0.0238(12) 0.0327(14) 0.0047(11) 0.0108(12) 0.0030(10) O9A 0.0289(15) 0.0385(15) 0.0395(16) 0.0021(12) 0.0003(12) -0.0082(11) O9B 0.0312(15) 0.0355(14) 0.0300(14) 0.0055(11) 0.0091(12) 0.0084(11) O10A 0.0386(17) 0.0353(15) 0.066(2) 0.0172(15) 0.0184(16) 0.0065(12) O10B 0.0343(15) 0.0309(14) 0.0442(17) 0.0127(12) 0.0066(13) 0.0027(11) O25A 0.0409(17) 0.0400(15) 0.0274(15) 0.0080(12) -0.0028(12) -0.0044(12) O25B 0.0389(15) 0.0299(13) 0.0248(13) 0.0047(11) 0.0081(12) 0.0095(11) O32A 0.0261(13) 0.0265(12) 0.0217(12) 0.0019(10) 0.0017(10) 0.0011(10) O32B 0.0266(14) 0.0251(12) 0.0243(13) 0.0014(10) 0.0049(11) 0.0007(10) Cl1A 0.0401(6) 0.0481(6) 0.0266(5) 0.0042(4) 0.0049(4) -0.0053(4) Cl1B 0.0362(5) 0.0432(5) 0.0223(4) 0.0022(4) 0.0015(4) 0.0020(4) U1A 0.02586(8) 0.01980(6) 0.02428(7) 0.00152(5) -0.00022(6) -0.00143(5) U1B 0.02436(7) 0.01971(6) 0.02024(7) 0.00195(5) 0.00486(5) 0.00092(5) _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 C2A N1A 1.292(5) . ? C2A C3A 1.435(6) . ? C2B N1B 1.298(5) . ? C2B C3B 1.435(5) . ? C3A C8A 1.404(5) . ? C3A C4A 1.416(6) . ? C3B C8B 1.413(5) . ? C3B C4B 1.417(5) . ? C4A O9A 1.308(4) . ? C4A C5A 1.420(6) . ? C4B O9B 1.305(4) . ? C4B C5B 1.427(5) . ? C5A O10A 1.370(6) . ? C5A C6A 1.389(6) . ? C5B C6B 1.372(6) . ? C5B O10B 1.377(5) . ? C6A C7A 1.397(7) . ? C6B C7B 1.391(6) . ? C7A C8A 1.360(7) . ? C7B C8B 1.366(6) . ? C11A O10A 1.449(5) . ? C11A C12A 1.494(6) . ? C11B O10B 1.443(5) . ? C11B C12B 1.506(5) . ? C12A C17A 1.386(7) . ? C12A C13A 1.387(7) . ? C12B C17B 1.373(6) . ? C12B C13B 1.389(6) . ? C13A C14A 1.407(8) . ? C13B C14B 1.392(7) . ? C14A C15A 1.370(10) . ? C14B C15B 1.368(8) . ? C15A C16A 1.369(10) . ? C15B C16B 1.367(8) . ? C16A C17A 1.386(8) . ? C16B C17B 1.396(7) . ? C18A C23A 1.359(8) . ? C18A C19A 1.362(7) . ? C18A C24A 1.503(6) . ? C18B C23B 1.367(6) . ? C18B C19B 1.387(6) . ? C18B C24B 1.501(5) . ? C19A C20A 1.400(8) . ? C19B C20B 1.381(6) . ? C20A C21A 1.354(8) . ? C20B C21B 1.363(6) . ? C21A C22A 1.323(9) . ? C21B C22B 1.374(7) . ? C22A C23A 1.405(8) . ? C22B C23B 1.381(7) . ? C24A O25A 1.422(5) . ? C24B O25B 1.438(4) . ? C26A C31A 1.372(6) . ? C26A O25A 1.375(5) . ? C26A C27A 1.423(5) . ? C26B O25B 1.379(4) . ? C26B C31B 1.382(5) . ? C26B C27B 1.425(5) . ? C27A O32A 1.306(4) . ? C27A C28A 1.431(5) . ? C27B O32B 1.305(4) . ? C27B C28B 1.422(5) . ? C28A C29A 1.401(5) . ? C28A C33A 1.437(5) . ? C28B C29B 1.407(5) . ? C28B C33B 1.438(5) . ? C29A C30A 1.370(6) . ? C29B C30B 1.367(6) . ? C30A C31A 1.387(6) . ? C30B C31B 1.400(6) . ? C33A N34A 1.289(5) . ? C33B N34B 1.289(5) . ? C35A C36A 1.390(6) . ? C35A C40A 1.403(6) . ? C35A N34A 1.424(4) . ? C35B C36B 1.393(5) . ? C35B C40B 1.393(5) . ? C35B N34B 1.425(4) . ? C36A C37A 1.395(6) . ? C36B C37B 1.379(5) . ? C37A C38A 1.375(7) . ? C37B C38B 1.373(6) . ? C38A C39A 1.378(6) . ? C38B C39B 1.385(5) . ? C39A C40A 1.401(5) . ? C39B C40B 1.397(5) . ? C40A N1A 1.420(5) . ? C40B N1B 1.428(4) . ? C42A C43A 1.508(5) . ? C42A N41A 1.510(4) . ? C42B C43B 1.522(5) . ? C42B N41B 1.525(4) . ? C43A C44A 1.520(5) . ? C43B C44B 1.527(5) . ? C44A C45A 1.512(7) . ? C44B C45B 1.522(6) . ? C46A C47A 1.522(5) . ? C46A N41A 1.528(4) . ? C46B N41B 1.518(4) . ? C46B C47B 1.528(5) . ? C47A C48A 1.492(6) . ? C47B C48B 1.517(6) . ? C48A C49A 1.494(6) . ? C48B C49B 1.517(6) . ? C50A C51A 1.516(5) . ? C50A N41A 1.527(5) . ? C50B C51B 1.511(5) . ? C50B N41B 1.524(4) . ? C51A C52A 1.524(6) . ? C51B C52B 1.524(5) . ? C52A C53A 1.520(7) . ? C52B C53B 1.515(6) . ? C54A C55A 1.512(5) . ? C54A N41A 1.528(4) . ? C54B N41B 1.518(4) . ? C54B C55B 1.521(5) . ? C55A C56A 1.530(5) . ? C55B C56B 1.528(5) . ? C56A C57A 1.510(6) . ? C56B C57B 1.522(6) . ? N1A U1A 2.619(3) . ? N1B U1B 2.619(3) . ? N34A U1A 2.577(3) . ? N34B U1B 2.572(3) . ? O1A U1A 1.784(2) . ? O1B U1B 1.784(2) . ? O2A U1A 1.783(2) . ? O2B U1B 1.785(2) . ? O9A U1A 2.259(3) . ? O9B U1B 2.265(2) . ? O32A U1A 2.278(2) . ? O32B U1B 2.286(2) . ? Cl1A U1A 2.7172(10) . ? Cl1B U1B 2.7157(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A C2A C3A 127.3(4) . . ? N1B C2B C3B 127.8(3) . . ? C8A C3A C4A 119.9(4) . . ? C8A C3A C2A 118.2(4) . . ? C4A C3A C2A 121.9(3) . . ? C8B C3B C4B 119.9(4) . . ? C8B C3B C2B 118.0(4) . . ? C4B C3B C2B 122.0(3) . . ? O9A C4A C3A 121.7(4) . . ? O9A C4A C5A 120.2(4) . . ? C3A C4A C5A 118.1(4) . . ? O9B C4B C3B 122.0(3) . . ? O9B C4B C5B 120.6(3) . . ? C3B C4B C5B 117.4(3) . . ? O10A C5A C6A 118.0(4) . . ? O10A C5A C4A 122.0(4) . . ? C6A C5A C4A 119.9(5) . . ? C6B C5B O10B 117.9(3) . . ? C6B C5B C4B 120.7(4) . . ? O10B C5B C4B 121.2(3) . . ? C5A C6A C7A 121.3(5) . . ? C5B C6B C7B 121.4(4) . . ? C8A C7A C6A 119.3(4) . . ? C8B C7B C6B 119.6(4) . . ? C7A C8A C3A 121.6(5) . . ? C7B C8B C3B 121.0(4) . . ? O10A C11A C12A 108.0(3) . . ? O10B C11B C12B 108.3(3) . . ? C17A C12A C13A 120.0(5) . . ? C17A C12A C11A 119.0(4) . . ? C13A C12A C11A 120.9(5) . . ? C17B C12B C13B 119.2(4) . . ? C17B C12B C11B 119.5(4) . . ? C13B C12B C11B 121.3(4) . . ? C12A C13A C14A 118.8(6) . . ? C12B C13B C14B 119.7(5) . . ? C15A C14A C13A 119.8(6) . . ? C15B C14B C13B 120.4(5) . . ? C16A C15A C14A 121.6(7) . . ? C16B C15B C14B 120.4(5) . . ? C15A C16A C17A 119.1(7) . . ? C15B C16B C17B 119.6(6) . . ? C12A C17A C16A 120.6(6) . . ? C12B C17B C16B 120.7(5) . . ? C23A C18A C19A 117.4(5) . . ? C23A C18A C24A 121.6(5) . . ? C19A C18A C24A 120.9(5) . . ? C23B C18B C19B 118.5(4) . . ? C23B C18B C24B 120.0(4) . . ? C19B C18B C24B 121.4(4) . . ? C18A C19A C20A 121.7(5) . . ? C20B C19B C18B 120.2(4) . . ? C21A C20A C19A 119.3(6) . . ? C21B C20B C19B 120.9(4) . . ? C22A C21A C20A 119.9(6) . . ? C20B C21B C22B 119.1(4) . . ? C21A C22A C23A 121.1(6) . . ? C21B C22B C23B 120.2(4) . . ? C18A C23A C22A 120.5(6) . . ? C18B C23B C22B 121.0(4) . . ? O25A C24A C18A 107.4(4) . . ? O25B C24B C18B 108.2(3) . . ? C31A C26A O25A 118.6(3) . . ? C31A C26A C27A 121.1(4) . . ? O25A C26A C27A 120.3(3) . . ? O25B C26B C31B 117.9(3) . . ? O25B C26B C27B 120.6(3) . . ? C31B C26B C27B 121.5(3) . . ? O32A C27A C26A 120.8(3) . . ? O32A C27A C28A 122.8(3) . . ? C26A C27A C28A 116.3(3) . . ? O32B C27B C28B 122.3(3) . . ? O32B C27B C26B 120.9(3) . . ? C28B C27B C26B 116.6(3) . . ? C29A C28A C27A 120.3(4) . . ? C29A C28A C33A 117.6(4) . . ? C27A C28A C33A 121.9(3) . . ? C29B C28B C27B 120.8(3) . . ? C29B C28B C33B 116.9(3) . . ? C27B C28B C33B 122.2(3) . . ? C30A C29A C28A 121.7(4) . . ? C30B C29B C28B 120.8(4) . . ? C29A C30A C31A 118.4(4) . . ? C29B C30B C31B 119.9(4) . . ? C26A C31A C30A 122.2(4) . . ? C26B C31B C30B 120.4(4) . . ? N34A C33A C28A 126.7(4) . . ? N34B C33B C28B 127.1(3) . . ? C36A C35A C40A 119.8(3) . . ? C36A C35A N34A 123.8(4) . . ? C40A C35A N34A 116.4(3) . . ? C36B C35B C40B 119.3(3) . . ? C36B C35B N34B 123.4(3) . . ? C40B C35B N34B 117.2(3) . . ? C35A C36A C37A 120.1(4) . . ? C37B C36B C35B 120.6(4) . . ? C38A C37A C36A 120.0(4) . . ? C38B C37B C36B 120.2(4) . . ? C37A C38A C39A 120.6(4) . . ? C37B C38B C39B 120.2(4) . . ? C38A C39A C40A 120.3(4) . . ? C38B C39B C40B 120.1(4) . . ? C39A C40A C35A 119.1(4) . . ? C39A C40A N1A 123.7(4) . . ? C35A C40A N1A 117.2(3) . . ? C35B C40B C39B 119.5(3) . . ? C35B C40B N1B 117.1(3) . . ? C39B C40B N1B 123.5(3) . . ? C43A C42A N41A 115.9(3) . . ? C43B C42B N41B 114.9(3) . . ? C42A C43A C44A 111.2(3) . . ? C42B C43B C44B 110.8(3) . . ? C45A C44A C43A 112.3(4) . . ? C45B C44B C43B 111.1(4) . . ? C47A C46A N41A 115.1(3) . . ? N41B C46B C47B 115.2(3) . . ? C48A C47A C46A 111.9(3) . . ? C48B C47B C46B 111.0(3) . . ? C47A C48A C49A 114.9(4) . . ? C47B C48B C49B 112.3(4) . . ? C51A C50A N41A 116.3(3) . . ? C51B C50B N41B 115.9(3) . . ? C50A C51A C52A 109.7(3) . . ? C50B C51B C52B 111.4(3) . . ? C53A C52A C51A 111.8(4) . . ? C53B C52B C51B 113.1(4) . . ? C55A C54A N41A 115.0(3) . . ? N41B C54B C55B 114.7(3) . . ? C54A C55A C56A 110.2(3) . . ? C54B C55B C56B 110.7(3) . . ? C57A C56A C55A 113.7(3) . . ? C57B C56B C55B 112.8(3) . . ? C2A N1A C40A 117.2(3) . . ? C2A N1A U1A 127.3(3) . . ? C40A N1A U1A 115.3(2) . . ? C2B N1B C40B 116.5(3) . . ? C2B N1B U1B 128.1(2) . . ? C40B N1B U1B 115.3(2) . . ? C33A N34A C35A 117.9(3) . . ? C33A N34A U1A 124.3(2) . . ? C35A N34A U1A 117.3(2) . . ? C33B N34B C35B 118.1(3) . . ? C33B N34B U1B 124.1(2) . . ? C35B N34B U1B 117.1(2) . . ? C42A N41A C50A 107.2(3) . . ? C42A N41A C54A 110.5(3) . . ? C50A N41A C54A 110.8(3) . . ? C42A N41A C46A 111.7(3) . . ? C50A N41A C46A 110.3(3) . . ? C54A N41A C46A 106.3(3) . . ? C54B N41B C46B 110.8(3) . . ? C54B N41B C50B 110.9(3) . . ? C46B N41B C50B 107.0(3) . . ? C54B N41B C42B 105.9(2) . . ? C46B N41B C42B 111.2(3) . . ? C50B N41B C42B 111.1(3) . . ? C4A O9A U1A 137.7(3) . . ? C4B O9B U1B 140.8(2) . . ? C5A O10A C11A 117.0(3) . . ? C5B O10B C11B 116.8(3) . . ? C26A O25A C24A 117.2(3) . . ? C26B O25B C24B 113.3(3) . . ? C27A O32A U1A 128.9(2) . . ? C27B O32B U1B 129.2(2) . . ? O2A U1A O1A 174.08(12) . . ? O2A U1A O9A 94.82(11) . . ? O1A U1A O9A 87.53(11) . . ? O2A U1A O32A 92.49(10) . . ? O1A U1A O32A 87.17(10) . . ? O9A U1A O32A 158.93(9) . . ? O2A U1A N34A 87.45(10) . . ? O1A U1A N34A 86.88(11) . . ? O9A U1A N34A 130.05(10) . . ? O32A U1A N34A 69.94(9) . . ? O2A U1A N1A 85.00(10) . . ? O1A U1A N1A 90.84(10) . . ? O9A U1A N1A 68.30(10) . . ? O32A U1A N1A 132.15(9) . . ? N34A U1A N1A 62.21(10) . . ? O2A U1A Cl1A 89.49(8) . . ? O1A U1A Cl1A 96.29(9) . . ? O9A U1A Cl1A 79.74(7) . . ? O32A U1A Cl1A 80.60(6) . . ? N34A U1A Cl1A 150.21(7) . . ? N1A U1A Cl1A 146.91(8) . . ? O1B U1B O2B 173.92(11) . . ? O1B U1B O9B 96.20(10) . . ? O2B U1B O9B 86.83(10) . . ? O1B U1B O32B 92.88(10) . . ? O2B U1B O32B 86.15(10) . . ? O9B U1B O32B 157.89(9) . . ? O1B U1B N34B 87.40(10) . . ? O2B U1B N34B 86.63(10) . . ? O9B U1B N34B 130.58(9) . . ? O32B U1B N34B 69.83(9) . . ? O1B U1B N1B 84.80(10) . . ? O2B U1B N1B 91.42(10) . . ? O9B U1B N1B 68.72(9) . . ? O32B U1B N1B 132.38(9) . . ? N34B U1B N1B 62.55(9) . . ? O1B U1B Cl1B 89.09(8) . . ? O2B U1B Cl1B 96.67(8) . . ? O9B U1B Cl1B 79.02(7) . . ? O32B U1B Cl1B 81.02(6) . . ? N34B U1B Cl1B 150.41(7) . . ? N1B U1B Cl1B 146.21(7) . . ? 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 N1A C2A C3A C8A 171.3(4) . . . . ? N1A C2A C3A C4A -10.4(6) . . . . ? N1B C2B C3B C8B -173.7(3) . . . . ? N1B C2B C3B C4B 7.5(6) . . . . ? C8A C3A C4A O9A 177.4(3) . . . . ? C2A C3A C4A O9A -0.8(6) . . . . ? C8A C3A C4A C5A -0.5(5) . . . . ? C2A C3A C4A C5A -178.7(3) . . . . ? C8B C3B C4B O9B -177.3(3) . . . . ? C2B C3B C4B O9B 1.5(5) . . . . ? C8B C3B C4B C5B 1.9(5) . . . . ? C2B C3B C4B C5B -179.4(3) . . . . ? O9A C4A C5A O10A 6.2(6) . . . . ? C3A C4A C5A O10A -175.8(3) . . . . ? O9A C4A C5A C6A -178.9(3) . . . . ? C3A C4A C5A C6A -1.0(5) . . . . ? O9B C4B C5B C6B 179.4(3) . . . . ? C3B C4B C5B C6B 0.2(5) . . . . ? O9B C4B C5B O10B -6.0(5) . . . . ? C3B C4B C5B O10B 174.9(3) . . . . ? O10A C5A C6A C7A 176.8(4) . . . . ? C4A C5A C6A C7A 1.8(6) . . . . ? O10B C5B C6B C7B -176.6(3) . . . . ? C4B C5B C6B C7B -1.8(6) . . . . ? C5A C6A C7A C8A -1.0(6) . . . . ? C5B C6B C7B C8B 1.3(6) . . . . ? C6A C7A C8A C3A -0.6(7) . . . . ? C4A C3A C8A C7A 1.3(6) . . . . ? C2A C3A C8A C7A 179.6(4) . . . . ? C6B C7B C8B C3B 0.9(6) . . . . ? C4B C3B C8B C7B -2.5(6) . . . . ? C2B C3B C8B C7B 178.7(3) . . . . ? O10A C11A C12A C17A -134.7(4) . . . . ? O10A C11A C12A C13A 46.3(5) . . . . ? O10B C11B C12B C17B 142.0(4) . . . . ? O10B C11B C12B C13B -38.8(5) . . . . ? C17A C12A C13A C14A -1.9(7) . . . . ? C11A C12A C13A C14A 177.0(5) . . . . ? C17B C12B C13B C14B 0.5(7) . . . . ? C11B C12B C13B C14B -178.7(4) . . . . ? C12A C13A C14A C15A 1.1(9) . . . . ? C12B C13B C14B C15B 0.4(8) . . . . ? C13A C14A C15A C16A 0.6(10) . . . . ? C13B C14B C15B C16B -0.9(10) . . . . ? C14A C15A C16A C17A -1.4(10) . . . . ? C14B C15B C16B C17B 0.6(11) . . . . ? C13A C12A C17A C16A 1.1(7) . . . . ? C11A C12A C17A C16A -177.8(4) . . . . ? C15A C16A C17A C12A 0.5(8) . . . . ? C13B C12B C17B C16B -0.8(8) . . . . ? C11B C12B C17B C16B 178.3(5) . . . . ? C15B C16B C17B C12B 0.3(10) . . . . ? C23A C18A C19A C20A 1.2(9) . . . . ? C24A C18A C19A C20A -176.6(5) . . . . ? C23B C18B C19B C20B 0.5(6) . . . . ? C24B C18B C19B C20B 178.5(4) . . . . ? C18A C19A C20A C21A 0.6(10) . . . . ? C18B C19B C20B C21B -1.1(7) . . . . ? C19A C20A C21A C22A -1.0(11) . . . . ? C19B C20B C21B C22B 0.8(7) . . . . ? C20A C21A C22A C23A -0.4(13) . . . . ? C20B C21B C22B C23B 0.2(8) . . . . ? C19A C18A C23A C22A -2.6(12) . . . . ? C24A C18A C23A C22A 175.2(7) . . . . ? C21A C22A C23A C18A 2.3(14) . . . . ? C19B C18B C23B C22B 0.5(7) . . . . ? C24B C18B C23B C22B -177.6(4) . . . . ? C21B C22B C23B C18B -0.8(8) . . . . ? C23A C18A C24A O25A -65.9(8) . . . . ? C19A C18A C24A O25A 111.9(5) . . . . ? C23B C18B C24B O25B -95.1(5) . . . . ? C19B C18B C24B O25B 86.9(5) . . . . ? C31A C26A C27A O32A 178.0(3) . . . . ? O25A C26A C27A O32A 1.8(5) . . . . ? C31A C26A C27A C28A 1.7(5) . . . . ? O25A C26A C27A C28A -174.6(3) . . . . ? O25B C26B C27B O32B 1.6(5) . . . . ? C31B C26B C27B O32B -176.8(3) . . . . ? O25B C26B C27B C28B 177.2(3) . . . . ? C31B C26B C27B C28B -1.2(5) . . . . ? O32A C27A C28A C29A -177.1(3) . . . . ? C26A C27A C28A C29A -0.9(5) . . . . ? O32A C27A C28A C33A -2.5(5) . . . . ? C26A C27A C28A C33A 173.7(3) . . . . ? O32B C27B C28B C29B 176.7(3) . . . . ? C26B C27B C28B C29B 1.2(5) . . . . ? O32B C27B C28B C33B 1.0(5) . . . . ? C26B C27B C28B C33B -174.5(3) . . . . ? C27A C28A C29A C30A -0.7(6) . . . . ? C33A C28A C29A C30A -175.5(4) . . . . ? C27B C28B C29B C30B -0.2(5) . . . . ? C33B C28B C29B C30B 175.7(3) . . . . ? C28A C29A C30A C31A 1.5(6) . . . . ? C28B C29B C30B C31B -0.9(6) . . . . ? O25A C26A C31A C30A 175.3(4) . . . . ? C27A C26A C31A C30A -1.0(6) . . . . ? C29A C30A C31A C26A -0.7(7) . . . . ? O25B C26B C31B C30B -178.3(3) . . . . ? C27B C26B C31B C30B 0.1(5) . . . . ? C29B C30B C31B C26B 0.9(6) . . . . ? C29A C28A C33A N34A -169.4(4) . . . . ? C27A C28A C33A N34A 15.9(6) . . . . ? C29B C28B C33B N34B 170.4(3) . . . . ? C27B C28B C33B N34B -13.7(6) . . . . ? C40A C35A C36A C37A 0.0(6) . . . . ? N34A C35A C36A C37A 179.2(4) . . . . ? C40B C35B C36B C37B -0.6(5) . . . . ? N34B C35B C36B C37B 179.5(3) . . . . ? C35A C36A C37A C38A -1.6(6) . . . . ? C35B C36B C37B C38B 1.6(6) . . . . ? C36A C37A C38A C39A 0.8(7) . . . . ? C36B C37B C38B C39B -0.9(6) . . . . ? C37A C38A C39A C40A 1.6(6) . . . . ? C37B C38B C39B C40B -0.7(6) . . . . ? C38A C39A C40A C35A -3.2(6) . . . . ? C38A C39A C40A N1A 177.7(4) . . . . ? C36A C35A C40A C39A 2.3(5) . . . . ? N34A C35A C40A C39A -176.9(3) . . . . ? C36A C35A C40A N1A -178.5(3) . . . . ? N34A C35A C40A N1A 2.3(5) . . . . ? C36B C35B C40B C39B -1.0(5) . . . . ? N34B C35B C40B C39B 178.9(3) . . . . ? C36B C35B C40B N1B 178.8(3) . . . . ? N34B C35B C40B N1B -1.3(4) . . . . ? C38B C39B C40B C35B 1.7(5) . . . . ? C38B C39B C40B N1B -178.1(3) . . . . ? N41A C42A C43A C44A -178.6(3) . . . . ? N41B C42B C43B C44B -165.7(3) . . . . ? C42A C43A C44A C45A -180.0(4) . . . . ? C42B C43B C44B C45B -178.5(3) . . . . ? N41A C46A C47A C48A -163.5(4) . . . . ? N41B C46B C47B C48B 162.5(3) . . . . ? C46A C47A C48A C49A -171.3(4) . . . . ? C46B C47B C48B C49B 168.5(3) . . . . ? N41A C50A C51A C52A -164.4(3) . . . . ? N41B C50B C51B C52B 170.9(3) . . . . ? C50A C51A C52A C53A -171.1(4) . . . . ? C50B C51B C52B C53B 179.6(4) . . . . ? N41A C54A C55A C56A 168.8(3) . . . . ? N41B C54B C55B C56B -167.4(3) . . . . ? C54A C55A C56A C57A -73.9(4) . . . . ? C54B C55B C56B C57B 70.7(4) . . . . ? C3A C2A N1A C40A 174.9(3) . . . . ? C3A C2A N1A U1A -10.9(6) . . . . ? C39A C40A N1A C2A -33.8(5) . . . . ? C35A C40A N1A C2A 147.1(3) . . . . ? C39A C40A N1A U1A 151.4(3) . . . . ? C35A C40A N1A U1A -27.8(4) . . . . ? C3B C2B N1B C40B -174.2(3) . . . . ? C3B C2B N1B U1B 9.6(5) . . . . ? C35B C40B N1B C2B -150.7(3) . . . . ? C39B C40B N1B C2B 29.1(5) . . . . ? C35B C40B N1B U1B 26.0(4) . . . . ? C39B C40B N1B U1B -154.2(3) . . . . ? C28A C33A N34A C35A -173.7(3) . . . . ? C28A C33A N34A U1A 14.6(5) . . . . ? C36A C35A N34A C33A 33.7(5) . . . . ? C40A C35A N34A C33A -147.1(3) . . . . ? C36A C35A N34A U1A -154.0(3) . . . . ? C40A C35A N34A U1A 25.2(4) . . . . ? C28B C33B N34B C35B 173.5(3) . . . . ? C28B C33B N34B U1B -16.3(5) . . . . ? C36B C35B N34B C33B -34.1(5) . . . . ? C40B C35B N34B C33B 146.0(3) . . . . ? C36B C35B N34B U1B 155.0(3) . . . . ? C40B C35B N34B U1B -24.9(4) . . . . ? C43A C42A N41A C50A 179.1(3) . . . . ? C43A C42A N41A C54A 58.2(4) . . . . ? C43A C42A N41A C46A -59.9(4) . . . . ? C51A C50A N41A C42A -167.3(3) . . . . ? C51A C50A N41A C54A -46.6(4) . . . . ? C51A C50A N41A C46A 70.9(4) . . . . ? C55A C54A N41A C42A 55.2(4) . . . . ? C55A C54A N41A C50A -63.5(4) . . . . ? C55A C54A N41A C46A 176.6(3) . . . . ? C47A C46A N41A C42A -47.9(4) . . . . ? C47A C46A N41A C50A 71.2(4) . . . . ? C47A C46A N41A C54A -168.6(3) . . . . ? C55B C54B N41B C46B 65.1(4) . . . . ? C55B C54B N41B C50B -53.5(4) . . . . ? C55B C54B N41B C42B -174.2(3) . . . . ? C47B C46B N41B C54B 52.8(4) . . . . ? C47B C46B N41B C50B 173.7(3) . . . . ? C47B C46B N41B C42B -64.8(4) . . . . ? C51B C50B N41B C54B -56.6(4) . . . . ? C51B C50B N41B C46B -177.4(3) . . . . ? C51B C50B N41B C42B 61.0(4) . . . . ? C43B C42B N41B C54B -167.8(3) . . . . ? C43B C42B N41B C46B -47.4(4) . . . . ? C43B C42B N41B C50B 71.7(4) . . . . ? C3A C4A O9A U1A 44.9(5) . . . . ? C5A C4A O9A U1A -137.3(3) . . . . ? C3B C4B O9B U1B -38.4(5) . . . . ? C5B C4B O9B U1B 142.4(3) . . . . ? C6A C5A O10A C11A 129.2(4) . . . . ? C4A C5A O10A C11A -55.9(5) . . . . ? C12A C11A O10A C5A -165.8(3) . . . . ? C6B C5B O10B C11B -127.4(4) . . . . ? C4B C5B O10B C11B 57.9(4) . . . . ? C12B C11B O10B C5B 156.6(3) . . . . ? C31A C26A O25A C24A 108.2(4) . . . . ? C27A C26A O25A C24A -75.5(5) . . . . ? C18A C24A O25A C26A -148.9(4) . . . . ? C31B C26B O25B C24B -108.4(4) . . . . ? C27B C26B O25B C24B 73.1(4) . . . . ? C18B C24B O25B C26B 166.2(3) . . . . ? C26A C27A O32A U1A 135.5(3) . . . . ? C28A C27A O32A U1A -48.4(4) . . . . ? C28B C27B O32B U1B 48.9(4) . . . . ? C26B C27B O32B U1B -135.7(3) . . . . ? C4A O9A U1A O2A -129.6(4) . . . . ? C4A O9A U1A O1A 45.0(4) . . . . ? C4A O9A U1A O32A 120.5(4) . . . . ? C4A O9A U1A N34A -38.8(4) . . . . ? C4A O9A U1A N1A -46.9(4) . . . . ? C4A O9A U1A Cl1A 141.8(4) . . . . ? C27A O32A U1A O2A 140.5(3) . . . . ? C27A O32A U1A O1A -33.6(3) . . . . ? C27A O32A U1A O9A -109.2(3) . . . . ? C27A O32A U1A N34A 54.1(3) . . . . ? C27A O32A U1A N1A 54.9(3) . . . . ? C27A O32A U1A Cl1A -130.5(3) . . . . ? C33A N34A U1A O2A -129.9(3) . . . . ? C35A N34A U1A O2A 58.3(2) . . . . ? C33A N34A U1A O1A 51.8(3) . . . . ? C35A N34A U1A O1A -120.0(2) . . . . ? C33A N34A U1A O9A 135.9(3) . . . . ? C35A N34A U1A O9A -35.9(3) . . . . ? C33A N34A U1A O32A -36.4(3) . . . . ? C35A N34A U1A O32A 151.9(3) . . . . ? C33A N34A U1A N1A 144.4(3) . . . . ? C35A N34A U1A N1A -27.4(2) . . . . ? C33A N34A U1A Cl1A -45.4(3) . . . . ? C35A N34A U1A Cl1A 142.8(2) . . . . ? C2A N1A U1A O2A 124.0(3) . . . . ? C40A N1A U1A O2A -61.8(2) . . . . ? C2A N1A U1A O1A -60.2(3) . . . . ? C40A N1A U1A O1A 114.0(2) . . . . ? C2A N1A U1A O9A 26.8(3) . . . . ? C40A N1A U1A O9A -159.0(3) . . . . ? C2A N1A U1A O32A -147.1(3) . . . . ? C40A N1A U1A O32A 27.1(3) . . . . ? C2A N1A U1A N34A -146.2(3) . . . . ? C40A N1A U1A N34A 28.0(2) . . . . ? C2A N1A U1A Cl1A 42.7(4) . . . . ? C40A N1A U1A Cl1A -143.1(2) . . . . ? C4B O9B U1B O1B 121.7(4) . . . . ? C4B O9B U1B O2B -53.0(4) . . . . ? C4B O9B U1B O32B -124.6(3) . . . . ? C4B O9B U1B N34B 29.8(4) . . . . ? C4B O9B U1B N1B 39.8(3) . . . . ? C4B O9B U1B Cl1B -150.4(4) . . . . ? C27B O32B U1B O1B -140.5(3) . . . . ? C27B O32B U1B O2B 33.5(3) . . . . ? C27B O32B U1B O9B 105.3(3) . . . . ? C27B O32B U1B N34B -54.3(3) . . . . ? C27B O32B U1B N1B -54.9(3) . . . . ? C27B O32B U1B Cl1B 130.9(3) . . . . ? C33B N34B U1B O1B 130.7(3) . . . . ? C35B N34B U1B O1B -59.0(2) . . . . ? C33B N34B U1B O2B -50.5(3) . . . . ? C35B N34B U1B O2B 119.8(2) . . . . ? C33B N34B U1B O9B -133.4(3) . . . . ? C35B N34B U1B O9B 36.9(3) . . . . ? C33B N34B U1B O32B 36.6(3) . . . . ? C35B N34B U1B O32B -153.0(2) . . . . ? C33B N34B U1B N1B -143.9(3) . . . . ? C35B N34B U1B N1B 26.5(2) . . . . ? C33B N34B U1B Cl1B 47.1(3) . . . . ? C35B N34B U1B Cl1B -142.57(19) . . . . ? C2B N1B U1B O1B -120.7(3) . . . . ? C40B N1B U1B O1B 63.1(2) . . . . ? C2B N1B U1B O2B 64.1(3) . . . . ? C40B N1B U1B O2B -112.2(2) . . . . ? C2B N1B U1B O9B -22.0(3) . . . . ? C40B N1B U1B O9B 161.8(2) . . . . ? C2B N1B U1B O32B 150.1(3) . . . . ? C40B N1B U1B O32B -26.1(3) . . . . ? C2B N1B U1B N34B 149.5(3) . . . . ? C40B N1B U1B N34B -26.7(2) . . . . ? C2B N1B U1B Cl1B -40.2(3) . . . . ? C40B N1B U1B Cl1B 143.58(18) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.057 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.109 #===END