# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p12014c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Cl2 N2 Th' _chemical_formula_sum 'C32 H36 Cl2 N2 Th' _chemical_formula_weight 751.57 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.1650(2) _cell_length_b 15.5150(4) _cell_length_c 18.2424(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.134(2) _cell_angle_gamma 90.00 _cell_volume 2876.45(11) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 10980 _cell_measurement_theta_min 3.2423 _cell_measurement_theta_max 27.4241 _exptl_crystal_description PRISM _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.4563 _exptl_crystal_size_mid 0.2770 _exptl_crystal_size_min 0.2067 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 5.394 _exptl_absorpt_correction_type ANALYTICAL _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_reflns_number 34644 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6582 _reflns_number_gt 5907 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material MERCURY _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+3.4266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6582 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0389 _refine_ls_wR_factor_gt 0.0374 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5802(2) 0.67533(17) 0.92254(15) 0.0167(5) Uani 1 1 d . . . C2 C 0.5621(3) 0.60760(18) 0.87291(16) 0.0218(6) Uani 1 1 d . . . H2 H 0.6269 0.5831 0.8424 0.026 Uiso 1 1 calc R . . C3 C 0.4293(3) 0.58284(18) 0.87701(15) 0.0210(6) Uani 1 1 d . . . H3 H 0.3867 0.5385 0.8496 0.025 Uiso 1 1 calc R . . C4 C 0.3725(3) 0.63603(17) 0.92907(15) 0.0178(6) Uani 1 1 d . . . C5 C 0.2389(3) 0.62919(17) 0.96471(15) 0.0194(6) Uani 1 1 d . . . C6 C 0.1474(3) 0.56834(18) 0.92111(18) 0.0285(7) Uani 1 1 d . . . H6A H 0.0617 0.5657 0.9447 0.043 Uiso 1 1 calc R . . H6B H 0.1862 0.5106 0.9199 0.043 Uiso 1 1 calc R . . H6C H 0.1358 0.5900 0.8709 0.043 Uiso 1 1 calc R . . C30 C 0.7071(3) 0.71741(18) 0.95024(16) 0.0226(6) Uani 1 1 d . . . C7 C 0.2638(3) 0.5901(2) 1.04144(17) 0.0313(7) Uani 1 1 d . . . H7A H 0.3188 0.6295 1.0708 0.047 Uiso 1 1 calc R . . H7B H 0.3089 0.5347 1.0367 0.047 Uiso 1 1 calc R . . H7C H 0.1796 0.5815 1.0656 0.047 Uiso 1 1 calc R . . C8 C 0.1798(2) 0.71898(17) 0.96800(15) 0.0180(6) Uani 1 1 d . . . C28 C 0.6887(2) 0.81518(18) 0.95033(15) 0.0185(6) Uani 1 1 d . . . C9 C 0.1615(2) 0.76412(17) 0.90222(14) 0.0165(5) Uani 1 1 d . . . H9 H 0.1816 0.7358 0.8577 0.020 Uiso 1 1 calc R . . C10 C 0.1152(2) 0.84872(17) 0.89880(15) 0.0180(6) Uani 1 1 d . . . C11 C 0.0801(3) 0.88722(19) 0.96409(17) 0.0270(7) Uani 1 1 d . . . H11 H 0.0471 0.9445 0.9639 0.032 Uiso 1 1 calc R . . C12 C 0.0927(3) 0.8428(2) 1.02961(18) 0.0352(8) Uani 1 1 d . . . H12 H 0.0657 0.8695 1.0737 0.042 Uiso 1 1 calc R . . C29 C 0.6564(2) 0.85578(17) 0.88389(15) 0.0174(6) Uani 1 1 d . . . H29 H 0.6535 0.8221 0.8404 0.021 Uiso 1 1 calc R . . C13 C 0.1439(3) 0.7602(2) 1.03212(16) 0.0284(7) Uani 1 1 d . . . H13 H 0.1546 0.7316 1.0779 0.034 Uiso 1 1 calc R . . C14 C 0.1069(2) 0.89276(17) 0.82392(15) 0.0178(6) Uani 1 1 d . . . C15 C 0.0104(3) 0.84368(19) 0.77289(16) 0.0245(6) Uani 1 1 d . . . H15A H 0.0033 0.8735 0.7256 0.037 Uiso 1 1 calc R . . H15B H -0.0764 0.8414 0.7953 0.037 Uiso 1 1 calc R . . H15C H 0.0428 0.7849 0.7653 0.037 Uiso 1 1 calc R . . C16 C 0.0582(3) 0.98662(18) 0.83025(18) 0.0259(7) Uani 1 1 d . . . H16A H 0.1196 1.0195 0.8615 0.039 Uiso 1 1 calc R . . H16B H -0.0293 0.9872 0.8519 0.039 Uiso 1 1 calc R . . H16C H 0.0533 1.0128 0.7814 0.039 Uiso 1 1 calc R . . C17 C 0.2436(2) 0.89487(17) 0.79129(15) 0.0159(5) Uani 1 1 d . . . C24 C 0.6280(2) 0.94426(18) 0.87863(16) 0.0192(6) Uani 1 1 d . . . C18 C 0.2807(3) 0.87647(18) 0.71981(15) 0.0207(6) Uani 1 1 d . . . H18 H 0.2266 0.8525 0.6820 0.025 Uiso 1 1 calc R . . C19 C 0.4138(3) 0.90023(19) 0.71446(15) 0.0225(6) Uani 1 1 d . . . H19 H 0.4668 0.8952 0.6724 0.027 Uiso 1 1 calc R . . C20 C 0.4530(2) 0.93267(17) 0.78283(15) 0.0184(6) Uani 1 1 d . . . C25 C 0.6390(3) 0.99291(19) 0.94177(17) 0.0271(7) Uani 1 1 d . . . H25 H 0.6220 1.0531 0.9401 0.033 Uiso 1 1 calc R . . C26 C 0.6750(3) 0.9541(2) 1.00772(17) 0.0298(7) Uani 1 1 d . . . H26 H 0.6846 0.9886 1.0505 0.036 Uiso 1 1 calc R . . C27 C 0.6972(3) 0.8668(2) 1.01254(16) 0.0266(7) Uani 1 1 d . . . H27 H 0.7185 0.8416 1.0587 0.032 Uiso 1 1 calc R . . C32 C 0.7323(3) 0.6828(2) 1.02840(18) 0.0360(8) Uani 1 1 d . . . H32A H 0.6600 0.7003 1.0599 0.054 Uiso 1 1 calc R . . H32B H 0.8153 0.7063 1.0480 0.054 Uiso 1 1 calc R . . H32C H 0.7377 0.6197 1.0271 0.054 Uiso 1 1 calc R . . C31 C 0.8222(3) 0.6919(2) 0.90218(19) 0.0327(8) Uani 1 1 d . . . H31A H 0.8332 0.6292 0.9034 0.049 Uiso 1 1 calc R . . H31B H 0.9028 0.7196 0.9207 0.049 Uiso 1 1 calc R . . H31C H 0.8043 0.7106 0.8516 0.049 Uiso 1 1 calc R . . C21 C 0.5796(3) 0.97950(18) 0.80464(17) 0.0230(6) Uani 1 1 d . . . C23 C 0.6846(3) 0.9666(2) 0.74596(17) 0.0312(7) Uani 1 1 d . . . H23A H 0.7022 0.9049 0.7401 0.047 Uiso 1 1 calc R . . H23B H 0.7659 0.9961 0.7612 0.047 Uiso 1 1 calc R . . H23C H 0.6527 0.9905 0.6992 0.047 Uiso 1 1 calc R . . C22 C 0.5482(3) 1.07664(19) 0.80809(19) 0.0334(8) Uani 1 1 d . . . H22A H 0.5129 1.0958 0.7604 0.050 Uiso 1 1 calc R . . H22B H 0.6287 1.1088 0.8201 0.050 Uiso 1 1 calc R . . H22C H 0.4829 1.0870 0.8459 0.050 Uiso 1 1 calc R . . N1 N 0.4624(2) 0.69589(14) 0.95490(12) 0.0154(5) Uani 1 1 d . . . N2 N 0.3507(2) 0.92588(14) 0.83159(12) 0.0163(5) Uani 1 1 d . . . Cl1 Cl 0.60482(7) 0.72416(5) 0.72537(4) 0.02966(17) Uani 1 1 d . . . Cl2 Cl 0.26510(7) 0.66705(5) 0.73474(4) 0.02770(16) Uani 1 1 d . . . Th1 Th 0.419416(9) 0.761185(6) 0.822488(5) 0.01429(3) 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 0.0158(13) 0.0160(13) 0.0184(14) 0.0057(11) 0.0001(11) 0.0047(10) C2 0.0231(14) 0.0184(14) 0.0240(15) 0.0005(12) 0.0057(12) 0.0092(11) C3 0.0248(15) 0.0163(14) 0.0218(15) -0.0009(11) -0.0024(12) 0.0012(11) C4 0.0211(13) 0.0151(13) 0.0171(14) 0.0040(11) -0.0020(11) 0.0011(11) C5 0.0185(13) 0.0186(14) 0.0211(15) 0.0046(12) 0.0015(11) 0.0006(11) C6 0.0250(15) 0.0169(15) 0.043(2) 0.0058(14) -0.0009(14) -0.0029(12) C30 0.0184(13) 0.0236(15) 0.0255(15) 0.0073(12) -0.0045(11) 0.0001(11) C7 0.0319(17) 0.0337(18) 0.0287(18) 0.0130(14) 0.0078(14) 0.0036(14) C8 0.0145(12) 0.0186(14) 0.0211(14) 0.0018(11) 0.0051(10) -0.0017(10) C28 0.0129(12) 0.0220(14) 0.0205(14) 0.0035(11) -0.0014(11) -0.0026(11) C9 0.0146(12) 0.0178(13) 0.0172(13) 0.0000(11) 0.0043(10) -0.0001(10) C10 0.0117(12) 0.0198(14) 0.0225(15) -0.0012(11) 0.0013(11) -0.0024(10) C11 0.0326(17) 0.0205(15) 0.0282(17) -0.0024(13) 0.0093(13) 0.0063(13) C12 0.048(2) 0.0346(19) 0.0231(17) -0.0059(14) 0.0128(15) 0.0055(15) C29 0.0136(13) 0.0192(14) 0.0194(14) 0.0007(11) -0.0017(11) -0.0019(10) C13 0.0336(16) 0.0312(17) 0.0207(15) 0.0046(13) 0.0067(12) 0.0061(14) C14 0.0144(13) 0.0175(14) 0.0215(15) 0.0031(11) 0.0005(11) 0.0019(10) C15 0.0175(14) 0.0276(16) 0.0283(17) 0.0060(13) -0.0048(12) -0.0011(12) C16 0.0209(14) 0.0201(15) 0.0367(18) 0.0046(13) 0.0030(13) 0.0049(12) C17 0.0158(13) 0.0142(13) 0.0176(14) 0.0027(11) -0.0011(10) 0.0023(10) C24 0.0097(12) 0.0207(14) 0.0271(16) 0.0039(12) 0.0001(11) -0.0031(10) C18 0.0215(14) 0.0242(15) 0.0161(14) 0.0019(12) -0.0041(11) 0.0040(11) C19 0.0224(14) 0.0284(16) 0.0168(14) 0.0070(12) 0.0032(11) 0.0026(12) C20 0.0169(13) 0.0161(14) 0.0222(15) 0.0081(11) 0.0003(11) 0.0006(10) C25 0.0227(15) 0.0218(16) 0.0367(18) -0.0031(13) -0.0038(13) -0.0030(12) C26 0.0262(16) 0.0360(18) 0.0270(17) -0.0119(14) -0.0056(13) -0.0038(13) C27 0.0246(15) 0.0351(18) 0.0198(15) 0.0015(13) -0.0066(12) -0.0011(13) C32 0.0371(18) 0.0363(19) 0.0339(19) 0.0139(15) -0.0187(15) -0.0032(15) C31 0.0157(14) 0.0300(18) 0.052(2) 0.0051(16) 0.0015(14) 0.0060(12) C21 0.0176(14) 0.0208(15) 0.0305(16) 0.0087(13) -0.0022(12) -0.0023(11) C23 0.0175(15) 0.042(2) 0.0339(18) 0.0176(15) 0.0041(13) -0.0027(13) C22 0.0288(16) 0.0217(16) 0.049(2) 0.0128(15) -0.0087(15) -0.0049(13) N1 0.0173(11) 0.0159(11) 0.0131(11) 0.0023(9) -0.0003(9) 0.0010(9) N2 0.0154(11) 0.0152(11) 0.0183(12) 0.0014(9) -0.0006(9) 0.0011(9) Cl1 0.0318(4) 0.0385(4) 0.0189(3) -0.0019(3) 0.0085(3) 0.0083(3) Cl2 0.0303(4) 0.0265(4) 0.0260(4) -0.0104(3) -0.0074(3) 0.0013(3) Th1 0.01545(5) 0.01546(5) 0.01197(5) -0.00027(4) 0.00034(3) 0.00191(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.382(3) . ? C1 C2 1.397(4) . ? C1 C30 1.523(4) . ? C1 Th1 2.767(2) . ? C2 C3 1.407(4) . ? C2 H2 0.9500 . ? C3 C4 1.392(4) . ? C3 H3 0.9500 . ? C4 N1 1.379(3) . ? C4 C5 1.521(4) . ? C4 Th1 2.796(3) . ? C5 C8 1.519(4) . ? C5 C6 1.536(4) . ? C5 C7 1.542(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C30 C31 1.528(4) . ? C30 C28 1.528(4) . ? C30 C32 1.540(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.388(4) . ? C8 C9 1.399(4) . ? C28 C27 1.390(4) . ? C28 C29 1.399(4) . ? C9 C10 1.395(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C10 C14 1.528(4) . ? C11 C12 1.384(4) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C29 C24 1.406(4) . ? C29 H29 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.523(4) . ? C14 C15 1.540(4) . ? C14 C16 1.543(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N2 1.387(3) . ? C17 C18 1.394(4) . ? C17 Th1 2.789(2) . ? C24 C25 1.380(4) . ? C24 C21 1.529(4) . ? C18 C19 1.407(4) . ? C18 H18 0.9500 . ? C19 C20 1.396(4) . ? C19 H19 0.9500 . ? C20 N2 1.386(3) . ? C20 C21 1.523(4) . ? C20 Th1 2.780(3) . ? C25 C26 1.388(4) . ? C25 H25 0.9500 . ? C26 C27 1.375(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C21 C23 1.540(4) . ? C21 C22 1.542(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N1 Th1 2.648(2) . ? N2 Th1 2.655(2) . ? Cl1 Th1 2.6745(7) . ? Cl2 Th1 2.6564(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 N1 C1 C2 110.3(2) . . ? N1 C1 C30 119.6(2) . . ? C2 C1 C30 129.6(2) . . ? N1 C1 Th1 70.46(13) . . ? C2 C1 Th1 82.33(16) . . ? C30 C1 Th1 119.84(17) . . ? C1 C2 C3 106.5(2) . . ? C1 C2 H2 126.7 . . ? C3 C2 H2 126.7 . . ? C4 C3 C2 106.6(2) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? N1 C4 C3 110.6(2) . . ? N1 C4 C5 119.5(2) . . ? C3 C4 C5 129.5(2) . . ? N1 C4 Th1 69.45(14) . . ? C3 C4 Th1 81.87(16) . . ? C5 C4 Th1 120.78(17) . . ? C8 C5 C4 108.1(2) . . ? C8 C5 C6 110.4(2) . . ? C4 C5 C6 111.0(2) . . ? C8 C5 C7 112.5(2) . . ? C4 C5 C7 106.5(2) . . ? C6 C5 C7 108.4(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C30 C31 110.6(2) . . ? C1 C30 C28 108.8(2) . . ? C31 C30 C28 110.6(2) . . ? C1 C30 C32 106.4(2) . . ? C31 C30 C32 109.0(2) . . ? C28 C30 C32 111.3(3) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 117.3(2) . . ? C13 C8 C5 124.5(3) . . ? C9 C8 C5 118.1(2) . . ? C27 C28 C29 117.2(3) . . ? C27 C28 C30 124.5(3) . . ? C29 C28 C30 118.2(3) . . ? C10 C9 C8 123.3(3) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C11 C10 C9 117.4(3) . . ? C11 C10 C14 124.4(2) . . ? C9 C10 C14 118.2(2) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 121.2(3) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C28 C29 C24 122.9(3) . . ? C28 C29 H29 118.6 . . ? C24 C29 H29 118.6 . . ? C12 C13 C8 120.3(3) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C17 C14 C10 108.9(2) . . ? C17 C14 C15 110.5(2) . . ? C10 C14 C15 110.0(2) . . ? C17 C14 C16 107.8(2) . . ? C10 C14 C16 111.5(2) . . ? C15 C14 C16 108.1(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 110.0(2) . . ? N2 C17 C14 120.8(2) . . ? C18 C17 C14 128.8(2) . . ? N2 C17 Th1 69.95(13) . . ? C18 C17 Th1 81.64(15) . . ? C14 C17 Th1 119.35(16) . . ? C25 C24 C29 117.7(3) . . ? C25 C24 C21 124.1(3) . . ? C29 C24 C21 118.1(3) . . ? C17 C18 C19 106.8(2) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? C20 C19 C18 106.9(2) . . ? C20 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? N2 C20 C19 110.0(2) . . ? N2 C20 C21 120.6(2) . . ? C19 C20 C21 129.1(3) . . ? N2 C20 Th1 70.28(14) . . ? C19 C20 Th1 81.55(16) . . ? C21 C20 Th1 119.73(17) . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 121.5(3) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 120.5(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C20 C21 C24 108.4(2) . . ? C20 C21 C23 110.5(2) . . ? C24 C21 C23 110.6(2) . . ? C20 C21 C22 107.6(2) . . ? C24 C21 C22 112.1(3) . . ? C23 C21 C22 107.6(2) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 N1 C1 105.8(2) . . ? C4 N1 Th1 81.35(14) . . ? C1 N1 Th1 80.06(14) . . ? C20 N2 C17 106.1(2) . . ? C20 N2 Th1 80.29(14) . . ? C17 N2 Th1 80.66(14) . . ? N1 Th1 N2 110.49(7) . . ? N1 Th1 Cl2 115.10(5) . . ? N2 Th1 Cl2 114.45(5) . . ? N1 Th1 Cl1 114.61(5) . . ? N2 Th1 Cl1 115.97(5) . . ? Cl2 Th1 Cl1 84.16(2) . . ? N1 Th1 C1 29.47(7) . . ? N2 Th1 C1 125.08(7) . . ? Cl2 Th1 C1 117.82(6) . . ? Cl1 Th1 C1 85.35(6) . . ? N1 Th1 C20 125.78(7) . . ? N2 Th1 C20 29.43(7) . . ? Cl2 Th1 C20 116.33(6) . . ? Cl1 Th1 C20 86.64(6) . . ? C1 Th1 C20 123.94(8) . . ? N1 Th1 C17 124.35(7) . . ? N2 Th1 C17 29.39(7) . . ? Cl2 Th1 C17 85.28(6) . . ? Cl1 Th1 C17 118.79(6) . . ? C1 Th1 C17 149.33(8) . . ? C20 Th1 C17 46.90(7) . . ? N1 Th1 C4 29.20(7) . . ? N2 Th1 C4 125.19(7) . . ? Cl2 Th1 C4 86.01(6) . . ? Cl1 Th1 C4 116.33(6) . . ? C1 Th1 C4 46.64(8) . . ? C20 Th1 C4 150.38(8) . . ? C17 Th1 C4 122.76(8) . . ? 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 N1 C1 C2 C3 -2.5(3) . . . . ? C30 C1 C2 C3 169.0(3) . . . . ? Th1 C1 C2 C3 -68.4(2) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 N1 3.1(3) . . . . ? C2 C3 C4 C5 -169.0(3) . . . . ? C2 C3 C4 Th1 67.5(2) . . . . ? N1 C4 C5 C8 50.7(3) . . . . ? C3 C4 C5 C8 -137.8(3) . . . . ? Th1 C4 C5 C8 -31.6(3) . . . . ? N1 C4 C5 C6 171.9(2) . . . . ? C3 C4 C5 C6 -16.6(4) . . . . ? Th1 C4 C5 C6 89.5(2) . . . . ? N1 C4 C5 C7 -70.3(3) . . . . ? C3 C4 C5 C7 101.2(3) . . . . ? Th1 C4 C5 C7 -152.71(19) . . . . ? N1 C1 C30 C31 -174.7(2) . . . . ? C2 C1 C30 C31 14.5(4) . . . . ? Th1 C1 C30 C31 -91.4(2) . . . . ? N1 C1 C30 C28 -52.9(3) . . . . ? C2 C1 C30 C28 136.3(3) . . . . ? Th1 C1 C30 C28 30.4(3) . . . . ? N1 C1 C30 C32 67.1(3) . . . . ? C2 C1 C30 C32 -103.7(3) . . . . ? Th1 C1 C30 C32 150.37(19) . . . . ? C4 C5 C8 C13 -121.0(3) . . . . ? C6 C5 C8 C13 117.4(3) . . . . ? C7 C5 C8 C13 -3.8(4) . . . . ? C4 C5 C8 C9 58.1(3) . . . . ? C6 C5 C8 C9 -63.5(3) . . . . ? C7 C5 C8 C9 175.3(2) . . . . ? C1 C30 C28 C27 118.6(3) . . . . ? C31 C30 C28 C27 -119.7(3) . . . . ? C32 C30 C28 C27 1.7(4) . . . . ? C1 C30 C28 C29 -59.0(3) . . . . ? C31 C30 C28 C29 62.7(3) . . . . ? C32 C30 C28 C29 -175.9(2) . . . . ? C13 C8 C9 C10 3.0(4) . . . . ? C5 C8 C9 C10 -176.2(2) . . . . ? C8 C9 C10 C11 -3.3(4) . . . . ? C8 C9 C10 C14 176.6(2) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C14 C10 C11 C12 -179.1(3) . . . . ? C10 C11 C12 C13 1.9(5) . . . . ? C27 C28 C29 C24 -2.5(4) . . . . ? C30 C28 C29 C24 175.3(2) . . . . ? C11 C12 C13 C8 -2.2(5) . . . . ? C9 C8 C13 C12 -0.2(4) . . . . ? C5 C8 C13 C12 178.9(3) . . . . ? C11 C10 C14 C17 120.5(3) . . . . ? C9 C10 C14 C17 -59.3(3) . . . . ? C11 C10 C14 C15 -118.3(3) . . . . ? C9 C10 C14 C15 61.9(3) . . . . ? C11 C10 C14 C16 1.7(4) . . . . ? C9 C10 C14 C16 -178.2(2) . . . . ? C10 C14 C17 N2 -50.8(3) . . . . ? C15 C14 C17 N2 -171.7(2) . . . . ? C16 C14 C17 N2 70.4(3) . . . . ? C10 C14 C17 C18 136.0(3) . . . . ? C15 C14 C17 C18 15.1(4) . . . . ? C16 C14 C17 C18 -102.8(3) . . . . ? C10 C14 C17 Th1 32.2(3) . . . . ? C15 C14 C17 Th1 -88.7(2) . . . . ? C16 C14 C17 Th1 153.39(18) . . . . ? C28 C29 C24 C25 3.1(4) . . . . ? C28 C29 C24 C21 -173.5(2) . . . . ? N2 C17 C18 C19 -2.5(3) . . . . ? C14 C17 C18 C19 171.3(3) . . . . ? Th1 C17 C18 C19 -67.5(2) . . . . ? C17 C18 C19 C20 -0.3(3) . . . . ? C18 C19 C20 N2 3.0(3) . . . . ? C18 C19 C20 C21 -170.0(3) . . . . ? C18 C19 C20 Th1 68.3(2) . . . . ? C29 C24 C25 C26 -1.0(4) . . . . ? C21 C24 C25 C26 175.4(3) . . . . ? C24 C25 C26 C27 -1.7(5) . . . . ? C25 C26 C27 C28 2.4(5) . . . . ? C29 C28 C27 C26 -0.3(4) . . . . ? C30 C28 C27 C26 -177.9(3) . . . . ? N2 C20 C21 C24 50.3(3) . . . . ? C19 C20 C21 C24 -137.4(3) . . . . ? Th1 C20 C21 C24 -33.2(3) . . . . ? N2 C20 C21 C23 171.6(2) . . . . ? C19 C20 C21 C23 -16.1(4) . . . . ? Th1 C20 C21 C23 88.1(2) . . . . ? N2 C20 C21 C22 -71.2(3) . . . . ? C19 C20 C21 C22 101.1(3) . . . . ? Th1 C20 C21 C22 -154.7(2) . . . . ? C25 C24 C21 C20 -117.0(3) . . . . ? C29 C24 C21 C20 59.4(3) . . . . ? C25 C24 C21 C23 121.8(3) . . . . ? C29 C24 C21 C23 -61.8(3) . . . . ? C25 C24 C21 C22 1.7(4) . . . . ? C29 C24 C21 C22 178.1(2) . . . . ? C3 C4 N1 C1 -4.6(3) . . . . ? C5 C4 N1 C1 168.4(2) . . . . ? Th1 C4 N1 C1 -77.03(16) . . . . ? C3 C4 N1 Th1 72.4(2) . . . . ? C5 C4 N1 Th1 -114.6(2) . . . . ? C2 C1 N1 C4 4.4(3) . . . . ? C30 C1 N1 C4 -168.1(2) . . . . ? Th1 C1 N1 C4 77.99(16) . . . . ? C2 C1 N1 Th1 -73.6(2) . . . . ? C30 C1 N1 Th1 113.9(2) . . . . ? C19 C20 N2 C17 -4.5(3) . . . . ? C21 C20 N2 C17 169.2(2) . . . . ? Th1 C20 N2 C17 -77.25(16) . . . . ? C19 C20 N2 Th1 72.8(2) . . . . ? C21 C20 N2 Th1 -113.6(2) . . . . ? C18 C17 N2 C20 4.3(3) . . . . ? C14 C17 N2 C20 -170.1(2) . . . . ? Th1 C17 N2 C20 76.97(16) . . . . ? C18 C17 N2 Th1 -72.7(2) . . . . ? C14 C17 N2 Th1 112.9(2) . . . . ? C4 N1 Th1 N2 126.33(14) . . . . ? C1 N1 Th1 N2 -125.85(14) . . . . ? C4 N1 Th1 Cl2 -5.20(15) . . . . ? C1 N1 Th1 Cl2 102.62(14) . . . . ? C4 N1 Th1 Cl1 -100.41(14) . . . . ? C1 N1 Th1 Cl1 7.41(16) . . . . ? C4 N1 Th1 C1 -107.8(2) . . . . ? C4 N1 Th1 C20 155.08(14) . . . . ? C1 N1 Th1 C20 -97.10(16) . . . . ? C4 N1 Th1 C17 96.93(16) . . . . ? C1 N1 Th1 C17 -155.25(14) . . . . ? C1 N1 Th1 C4 107.8(2) . . . . ? C20 N2 Th1 N1 127.43(14) . . . . ? C17 N2 Th1 N1 -124.33(15) . . . . ? C20 N2 Th1 Cl2 -100.70(14) . . . . ? C17 N2 Th1 Cl2 7.54(16) . . . . ? C20 N2 Th1 Cl1 -5.13(16) . . . . ? C17 N2 Th1 Cl1 103.11(14) . . . . ? C20 N2 Th1 C1 98.27(16) . . . . ? C17 N2 Th1 C1 -153.49(14) . . . . ? C17 N2 Th1 C20 108.2(2) . . . . ? C20 N2 Th1 C17 -108.2(2) . . . . ? C20 N2 Th1 C4 156.18(14) . . . . ? C17 N2 Th1 C4 -95.58(16) . . . . ? C2 C1 Th1 N1 114.8(2) . . . . ? C30 C1 Th1 N1 -113.7(3) . . . . ? N1 C1 Th1 N2 68.09(16) . . . . ? C2 C1 Th1 N2 -177.12(14) . . . . ? C30 C1 Th1 N2 -45.6(2) . . . . ? N1 C1 Th1 Cl2 -92.36(14) . . . . ? C2 C1 Th1 Cl2 22.43(18) . . . . ? C30 C1 Th1 Cl2 153.99(18) . . . . ? N1 C1 Th1 Cl1 -173.24(14) . . . . ? C2 C1 Th1 Cl1 -58.46(15) . . . . ? C30 C1 Th1 Cl1 73.1(2) . . . . ? N1 C1 Th1 C20 103.98(15) . . . . ? C2 C1 Th1 C20 -141.24(16) . . . . ? C30 C1 Th1 C20 -9.7(2) . . . . ? N1 C1 Th1 C17 42.7(2) . . . . ? C2 C1 Th1 C17 157.44(16) . . . . ? C30 C1 Th1 C17 -71.0(3) . . . . ? N1 C1 Th1 C4 -39.70(14) . . . . ? C2 C1 Th1 C4 75.09(17) . . . . ? C30 C1 Th1 C4 -153.3(2) . . . . ? N2 C20 Th1 N1 -66.47(16) . . . . ? C19 C20 Th1 N1 178.71(14) . . . . ? C21 C20 Th1 N1 48.3(2) . . . . ? C19 C20 Th1 N2 -114.8(2) . . . . ? C21 C20 Th1 N2 114.7(3) . . . . ? N2 C20 Th1 Cl2 93.59(14) . . . . ? C19 C20 Th1 Cl2 -21.23(17) . . . . ? C21 C20 Th1 Cl2 -151.68(19) . . . . ? N2 C20 Th1 Cl1 175.38(14) . . . . ? C19 C20 Th1 Cl1 60.56(15) . . . . ? C21 C20 Th1 Cl1 -69.9(2) . . . . ? N2 C20 Th1 C1 -102.52(15) . . . . ? C19 C20 Th1 C1 142.66(15) . . . . ? C21 C20 Th1 C1 12.2(2) . . . . ? N2 C20 Th1 C17 39.68(14) . . . . ? C19 C20 Th1 C17 -75.14(17) . . . . ? C21 C20 Th1 C17 154.4(3) . . . . ? N2 C20 Th1 C4 -41.9(2) . . . . ? C19 C20 Th1 C4 -156.72(16) . . . . ? C21 C20 Th1 C4 72.8(3) . . . . ? N2 C17 Th1 N1 69.55(16) . . . . ? C18 C17 Th1 N1 -175.46(15) . . . . ? C14 C17 Th1 N1 -45.3(2) . . . . ? C18 C17 Th1 N2 115.0(2) . . . . ? C14 C17 Th1 N2 -114.9(3) . . . . ? N2 C17 Th1 Cl2 -173.12(14) . . . . ? C18 C17 Th1 Cl2 -58.12(16) . . . . ? C14 C17 Th1 Cl2 71.99(19) . . . . ? N2 C17 Th1 Cl1 -92.44(14) . . . . ? C18 C17 Th1 Cl1 22.55(18) . . . . ? C14 C17 Th1 Cl1 152.67(17) . . . . ? N2 C17 Th1 C1 45.7(2) . . . . ? C18 C17 Th1 C1 160.73(16) . . . . ? C14 C17 Th1 C1 -69.2(3) . . . . ? N2 C17 Th1 C20 -39.73(14) . . . . ? C18 C17 Th1 C20 75.26(17) . . . . ? C14 C17 Th1 C20 -154.6(2) . . . . ? N2 C17 Th1 C4 104.71(15) . . . . ? C18 C17 Th1 C4 -140.30(16) . . . . ? C14 C17 Th1 C4 -10.2(2) . . . . ? C3 C4 Th1 N1 -115.6(2) . . . . ? C5 C4 Th1 N1 112.9(3) . . . . ? N1 C4 Th1 N2 -67.43(16) . . . . ? C3 C4 Th1 N2 176.94(14) . . . . ? C5 C4 Th1 N2 45.4(2) . . . . ? N1 C4 Th1 Cl2 175.28(14) . . . . ? C3 C4 Th1 Cl2 59.65(15) . . . . ? C5 C4 Th1 Cl2 -71.9(2) . . . . ? N1 C4 Th1 Cl1 93.82(14) . . . . ? C3 C4 Th1 Cl1 -21.81(17) . . . . ? C5 C4 Th1 Cl1 -153.33(18) . . . . ? N1 C4 Th1 C1 40.10(14) . . . . ? C3 C4 Th1 C1 -75.53(17) . . . . ? C5 C4 Th1 C1 153.0(2) . . . . ? N1 C4 Th1 C20 -43.8(2) . . . . ? C3 C4 Th1 C20 -159.39(16) . . . . ? C5 C4 Th1 C20 69.1(3) . . . . ? N1 C4 Th1 C17 -102.94(15) . . . . ? C3 C4 Th1 C17 141.43(15) . . . . ? C5 C4 Th1 C17 9.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.573 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 951384' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po2011 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 I2 N2 U' _chemical_formula_weight 940.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.64710(10) _cell_length_b 22.5946(2) _cell_length_c 12.57570(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.4440(10) _cell_angle_gamma 90.00 _cell_volume 3011.65(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 37728 _cell_measurement_theta_min 3.5276 _cell_measurement_theta_max 73.8501 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2489 _exptl_crystal_size_mid 0.0439 _exptl_crystal_size_min 0.0167 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 31.431 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.087 _exptl_absorpt_correction_T_max 0.624 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90561 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 74.01 _reflns_number_total 6091 _reflns_number_gt 5507 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+3.7842P] 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 6091 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9494(5) 0.0678(2) 0.2813(4) 0.0214(11) Uani 1 1 d . . . C2 C 0.9827(6) 0.0457(2) 0.3832(5) 0.0268(12) Uani 1 1 d . . . H2 H 0.9818 0.0054 0.4043 0.032 Uiso 1 1 calc R . . C3 C 1.0179(5) 0.0944(3) 0.4492(4) 0.0244(11) Uani 1 1 d . . . H3 H 1.0467 0.0934 0.5230 0.029 Uiso 1 1 calc R . . C4 C 1.0018(6) 0.1450(2) 0.3839(4) 0.0255(12) Uani 1 1 d . . . C5 C 1.0495(6) 0.2073(2) 0.4056(5) 0.0258(12) Uani 1 1 d . . . C6 C 1.1693(6) 0.2135(3) 0.3467(6) 0.0339(14) Uani 1 1 d . . . H6A H 1.2319 0.1841 0.3743 0.051 Uiso 1 1 calc R . . H6B H 1.2043 0.2534 0.3583 0.051 Uiso 1 1 calc R . . H6C H 1.1479 0.2070 0.2701 0.051 Uiso 1 1 calc R . . C7 C 1.0852(7) 0.2172(3) 0.5251(5) 0.0340(14) Uani 1 1 d . . . H7A H 1.0126 0.2082 0.5647 0.051 Uiso 1 1 calc R . . H7B H 1.1102 0.2586 0.5374 0.051 Uiso 1 1 calc R . . H7C H 1.1557 0.1912 0.5497 0.051 Uiso 1 1 calc R . . C8 C 0.9462(5) 0.2495(2) 0.3629(4) 0.0221(11) Uani 1 1 d . . . C9 C 0.8279(6) 0.2430(2) 0.4001(4) 0.0252(12) Uani 1 1 d . . . H9 H 0.8191 0.2147 0.4548 0.030 Uiso 1 1 calc R . . C10 C 0.7215(5) 0.2753(2) 0.3623(4) 0.0220(11) Uani 1 1 d . . . C11 C 0.7389(6) 0.3193(2) 0.2875(5) 0.0281(12) Uani 1 1 d . . . H11 H 0.6696 0.3433 0.2608 0.034 Uiso 1 1 calc R . . C12 C 0.8569(6) 0.3285(3) 0.2517(5) 0.0318(13) Uani 1 1 d . . . H12 H 0.8675 0.3594 0.2022 0.038 Uiso 1 1 calc R . . C13 C 0.9596(6) 0.2934(2) 0.2868(4) 0.0264(12) Uani 1 1 d . . . H13 H 1.0386 0.2993 0.2590 0.032 Uiso 1 1 calc R . . C14 C 0.5961(6) 0.2599(2) 0.4035(5) 0.0253(12) Uani 1 1 d . . . C15 C 0.5995(7) 0.2723(3) 0.5238(5) 0.0336(14) Uani 1 1 d . . . H15A H 0.6722 0.2521 0.5613 0.050 Uiso 1 1 calc R . . H15B H 0.5217 0.2577 0.5504 0.050 Uiso 1 1 calc R . . H15C H 0.6069 0.3150 0.5365 0.050 Uiso 1 1 calc R . . C16 C 0.4862(6) 0.2949(2) 0.3453(5) 0.0319(13) Uani 1 1 d . . . H16A H 0.5023 0.3374 0.3538 0.048 Uiso 1 1 calc R . . H16B H 0.4075 0.2848 0.3757 0.048 Uiso 1 1 calc R . . H16C H 0.4786 0.2848 0.2692 0.048 Uiso 1 1 calc R . . C17 C 0.5688(5) 0.1945(2) 0.3784(4) 0.0225(11) Uani 1 1 d . . . C18 C 0.5158(6) 0.1516(3) 0.4414(5) 0.0278(12) Uani 1 1 d . . . H18 H 0.5035 0.1545 0.5150 0.033 Uiso 1 1 calc R . . C19 C 0.4846(5) 0.1033(3) 0.3730(5) 0.0254(12) Uani 1 1 d . . . H19 H 0.4473 0.0670 0.3918 0.031 Uiso 1 1 calc R . . C20 C 0.5193(6) 0.1192(2) 0.2713(5) 0.0243(12) Uani 1 1 d . . . C21 C 0.4825(6) 0.0905(2) 0.1629(5) 0.0258(12) Uani 1 1 d . . . C22 C 0.3770(6) 0.1286(3) 0.1075(5) 0.0315(13) Uani 1 1 d . . . H22A H 0.4089 0.1687 0.0968 0.047 Uiso 1 1 calc R . . H22B H 0.3064 0.1305 0.1521 0.047 Uiso 1 1 calc R . . H22C H 0.3481 0.1111 0.0381 0.047 Uiso 1 1 calc R . . C23 C 0.4335(6) 0.0268(3) 0.1764(5) 0.0311(13) Uani 1 1 d . . . H23A H 0.4047 0.0104 0.1061 0.047 Uiso 1 1 calc R . . H23B H 0.3631 0.0275 0.2213 0.047 Uiso 1 1 calc R . . H23C H 0.5017 0.0022 0.2103 0.047 Uiso 1 1 calc R . . C24 C 0.5990(6) 0.0897(2) 0.1018(4) 0.0226(11) Uani 1 1 d . . . C25 C 0.6063(6) 0.1137(2) 0.0015(5) 0.0250(12) Uani 1 1 d . . . H25 H 0.5335 0.1312 -0.0353 0.030 Uiso 1 1 calc R . . C26 C 0.7186(7) 0.1125(2) -0.0461(5) 0.0291(13) Uani 1 1 d . . . H26 H 0.7213 0.1282 -0.1159 0.035 Uiso 1 1 calc R . . C27 C 0.8281(6) 0.0883(2) 0.0076(5) 0.0286(12) Uani 1 1 d . . . H27 H 0.9056 0.0897 -0.0241 0.034 Uiso 1 1 calc R . . C28 C 0.8234(5) 0.0625(2) 0.1072(4) 0.0219(11) Uani 1 1 d . . . C29 C 0.7073(5) 0.0630(2) 0.1520(4) 0.0206(10) Uani 1 1 d . . . H29 H 0.7023 0.0445 0.2193 0.025 Uiso 1 1 calc R . . C30 C 0.9359(5) 0.0360(2) 0.1748(4) 0.0224(11) Uani 1 1 d . . . C31 C 0.9157(6) -0.0308(2) 0.1899(5) 0.0249(11) Uani 1 1 d . . . H31A H 0.8409 -0.0371 0.2283 0.037 Uiso 1 1 calc R . . H31B H 0.9898 -0.0477 0.2313 0.037 Uiso 1 1 calc R . . H31C H 0.9036 -0.0501 0.1199 0.037 Uiso 1 1 calc R . . C32 C 1.0612(6) 0.0459(3) 0.1276(5) 0.0289(12) Uani 1 1 d . . . H32A H 1.0600 0.0252 0.0590 0.043 Uiso 1 1 calc R . . H32B H 1.1303 0.0304 0.1769 0.043 Uiso 1 1 calc R . . H32C H 1.0738 0.0883 0.1168 0.043 Uiso 1 1 calc R . . N1 N 0.9540(4) 0.1291(2) 0.2825(4) 0.0205(9) Uani 1 1 d . . . N2 N 0.5766(5) 0.1741(2) 0.2766(4) 0.0229(9) Uani 1 1 d . . . I1 I 0.77984(4) 0.121070(17) 0.61991(3) 0.03091(11) Uani 1 1 d . . . I2 I 0.68962(4) -0.015193(14) 0.42429(3) 0.02723(11) Uani 1 1 d . . . U1 U 0.753851(17) 0.113198(7) 0.375035(13) 0.02008(8) 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 0.017(3) 0.022(2) 0.027(3) 0.001(2) 0.007(2) -0.0012(19) C2 0.029(3) 0.021(2) 0.030(3) 0.003(2) 0.005(2) 0.004(2) C3 0.021(3) 0.031(3) 0.021(3) 0.002(2) 0.001(2) 0.004(2) C4 0.027(3) 0.026(3) 0.024(3) 0.001(2) 0.007(2) 0.003(2) C5 0.024(3) 0.026(3) 0.027(3) 0.001(2) 0.003(2) 0.002(2) C6 0.021(3) 0.032(3) 0.049(4) 0.000(3) 0.003(3) -0.004(2) C7 0.039(4) 0.029(3) 0.031(3) -0.002(2) -0.008(3) -0.001(3) C8 0.021(3) 0.021(2) 0.025(3) -0.002(2) 0.002(2) -0.003(2) C9 0.034(3) 0.017(2) 0.025(3) 0.002(2) 0.006(2) 0.001(2) C10 0.021(3) 0.021(2) 0.024(3) -0.0034(19) 0.003(2) 0.002(2) C11 0.032(3) 0.024(3) 0.028(3) -0.002(2) 0.003(2) 0.003(2) C12 0.038(4) 0.031(3) 0.027(3) -0.002(2) 0.007(3) -0.006(3) C13 0.035(3) 0.025(3) 0.020(3) -0.002(2) 0.006(2) -0.004(2) C14 0.025(3) 0.024(3) 0.028(3) -0.003(2) 0.007(2) 0.001(2) C15 0.037(4) 0.039(3) 0.026(3) -0.007(2) 0.011(3) 0.002(3) C16 0.028(3) 0.025(3) 0.043(4) -0.001(2) 0.003(3) 0.007(2) C17 0.018(3) 0.024(2) 0.026(3) -0.002(2) 0.006(2) 0.001(2) C18 0.031(3) 0.030(3) 0.024(3) 0.000(2) 0.009(2) 0.002(2) C19 0.015(3) 0.031(3) 0.032(3) 0.003(2) 0.009(2) 0.001(2) C20 0.029(3) 0.021(2) 0.025(3) 0.0005(19) 0.008(2) 0.005(2) C21 0.023(3) 0.025(3) 0.029(3) -0.002(2) 0.002(2) -0.001(2) C22 0.023(3) 0.036(3) 0.035(3) -0.001(3) -0.001(3) 0.003(2) C23 0.026(3) 0.028(3) 0.039(3) -0.005(2) 0.007(3) -0.004(2) C24 0.029(3) 0.018(2) 0.021(3) -0.0009(19) 0.003(2) 0.001(2) C25 0.026(3) 0.023(3) 0.025(3) -0.0019(19) 0.001(2) 0.003(2) C26 0.041(4) 0.027(3) 0.020(3) 0.003(2) 0.008(3) 0.000(2) C27 0.038(4) 0.025(3) 0.025(3) 0.000(2) 0.013(3) -0.001(2) C28 0.028(3) 0.020(2) 0.018(2) -0.0017(19) 0.004(2) -0.001(2) C29 0.025(3) 0.021(2) 0.017(2) 0.0026(18) 0.007(2) 0.000(2) C30 0.020(3) 0.022(2) 0.026(3) -0.002(2) 0.010(2) 0.002(2) C31 0.027(3) 0.023(2) 0.027(3) -0.001(2) 0.010(2) 0.001(2) C32 0.026(3) 0.030(3) 0.033(3) 0.000(2) 0.011(3) 0.001(2) N1 0.018(2) 0.024(2) 0.020(2) 0.0016(17) 0.0054(18) 0.0008(18) N2 0.025(3) 0.025(2) 0.020(2) -0.0009(17) 0.0068(19) 0.0011(18) I1 0.0380(2) 0.0367(2) 0.01844(19) 0.00186(13) 0.00498(16) 0.00144(16) I2 0.0310(2) 0.02431(17) 0.02784(19) 0.00652(12) 0.01031(15) -0.00088(13) U1 0.02159(13) 0.02103(12) 0.01826(12) 0.00148(5) 0.00535(8) 0.00046(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.386(7) . ? C1 C2 1.389(8) . ? C1 C30 1.515(7) . ? C1 U1 2.692(5) . ? C2 C3 1.407(8) . ? C2 U1 2.868(6) . ? C2 H2 0.9500 . ? C3 C4 1.408(8) . ? C3 U1 2.908(6) . ? C3 H3 0.9500 . ? C4 N1 1.375(7) . ? C4 C5 1.512(8) . ? C4 U1 2.728(6) . ? C5 C8 1.515(8) . ? C5 C7 1.531(8) . ? C5 C6 1.542(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.393(9) . ? C8 C13 1.395(8) . ? C9 C10 1.392(8) . ? C9 U1 3.045(5) . ? C9 H9 0.9500 . ? C10 C11 1.394(8) . ? C10 C14 1.518(8) . ? C11 C12 1.389(9) . ? C11 H11 0.9500 . ? C12 C13 1.388(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.534(7) . ? C14 C15 1.535(8) . ? C14 C16 1.539(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N2 1.371(7) . ? C17 C18 1.404(8) . ? C17 U1 2.697(5) . ? C18 C19 1.409(8) . ? C18 U1 2.876(6) . ? C18 H18 0.9500 . ? C19 C20 1.411(8) . ? C19 U1 2.873(6) . ? C19 H19 0.9500 . ? C20 N2 1.381(7) . ? C20 C21 1.527(8) . ? C20 U1 2.709(6) . ? C21 C24 1.520(8) . ? C21 C22 1.530(8) . ? C21 C23 1.545(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.382(8) . ? C24 C29 1.398(8) . ? C25 C26 1.388(9) . ? C25 H25 0.9500 . ? C26 C27 1.402(9) . ? C26 H26 0.9500 . ? C27 C28 1.387(8) . ? C27 H27 0.9500 . ? C28 C29 1.406(8) . ? C28 C30 1.524(8) . ? C29 U1 3.022(5) . ? C29 H29 0.9500 . ? C30 C32 1.528(8) . ? C30 C31 1.538(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1 U1 2.549(5) . ? N2 U1 2.559(5) . ? I1 U1 3.0708(4) . ? I2 U1 3.0573(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.1(5) . . ? N1 C1 C30 119.0(5) . . ? C2 C1 C30 129.8(5) . . ? N1 C1 U1 69.0(3) . . ? C2 C1 U1 82.7(3) . . ? C30 C1 U1 123.7(4) . . ? C1 C2 C3 107.1(5) . . ? C1 C2 U1 68.6(3) . . ? C3 C2 U1 77.5(3) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? U1 C2 H2 119.3 . . ? C4 C3 C2 106.2(5) . . ? C4 C3 U1 68.6(3) . . ? C2 C3 U1 74.3(3) . . ? C4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? U1 C3 H3 122.0 . . ? N1 C4 C3 110.0(5) . . ? N1 C4 C5 119.9(5) . . ? C3 C4 C5 129.1(5) . . ? N1 C4 U1 67.8(3) . . ? C3 C4 U1 82.7(3) . . ? C5 C4 U1 124.0(4) . . ? C4 C5 C8 107.6(5) . . ? C4 C5 C7 111.2(5) . . ? C8 C5 C7 111.1(5) . . ? C4 C5 C6 106.1(5) . . ? C8 C5 C6 112.2(5) . . ? C7 C5 C6 108.6(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 117.4(5) . . ? C9 C8 C5 117.6(5) . . ? C13 C8 C5 125.0(5) . . ? C8 C9 C10 124.2(5) . . ? C8 C9 U1 107.5(3) . . ? C10 C9 U1 106.0(4) . . ? C8 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? U1 C9 H9 52.0 . . ? C11 C10 C9 116.7(5) . . ? C11 C10 C14 124.8(5) . . ? C9 C10 C14 118.5(5) . . ? C12 C11 C10 120.5(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 121.4(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C8 119.7(6) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C10 C14 C17 107.8(4) . . ? C10 C14 C15 110.8(5) . . ? C17 C14 C15 111.4(5) . . ? C10 C14 C16 112.0(5) . . ? C17 C14 C16 106.0(5) . . ? C15 C14 C16 108.7(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 111.0(5) . . ? N2 C17 C14 119.3(5) . . ? C18 C17 C14 128.9(5) . . ? N2 C17 U1 69.4(3) . . ? C18 C17 U1 82.6(3) . . ? C14 C17 U1 122.4(4) . . ? C17 C18 C19 105.9(5) . . ? C17 C18 U1 68.4(3) . . ? C19 C18 U1 75.7(3) . . ? C17 C18 H18 127.0 . . ? C19 C18 H18 127.0 . . ? U1 C18 H18 120.7 . . ? C18 C19 C20 106.8(5) . . ? C18 C19 U1 75.9(3) . . ? C20 C19 U1 69.0(3) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.6 . . ? U1 C19 H19 120.3 . . ? N2 C20 C19 109.7(5) . . ? N2 C20 C21 120.0(5) . . ? C19 C20 C21 129.3(5) . . ? N2 C20 U1 68.9(3) . . ? C19 C20 U1 81.9(4) . . ? C21 C20 U1 123.7(4) . . ? C24 C21 C20 107.6(5) . . ? C24 C21 C22 112.1(5) . . ? C20 C21 C22 106.4(5) . . ? C24 C21 C23 110.2(5) . . ? C20 C21 C23 111.0(5) . . ? C22 C21 C23 109.5(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 117.8(5) . . ? C25 C24 C21 125.2(5) . . ? C29 C24 C21 117.1(5) . . ? C24 C25 C26 120.8(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 117.9(5) . . ? C27 C28 C30 125.1(5) . . ? C29 C28 C30 117.0(5) . . ? C24 C29 C28 122.8(5) . . ? C24 C29 U1 108.2(3) . . ? C28 C29 U1 107.6(3) . . ? C24 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? U1 C29 H29 50.0 . . ? C1 C30 C28 108.1(4) . . ? C1 C30 C32 105.1(5) . . ? C28 C30 C32 113.3(5) . . ? C1 C30 C31 111.0(5) . . ? C28 C30 C31 110.1(5) . . ? C32 C30 C31 109.2(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C4 N1 C1 106.3(4) . . ? C4 N1 U1 82.3(3) . . ? C1 N1 U1 80.5(3) . . ? C17 N2 C20 106.3(5) . . ? C17 N2 U1 80.5(3) . . ? C20 N2 U1 80.9(3) . . ? N1 U1 N2 108.27(14) . . ? N1 U1 C1 30.52(14) . . ? N2 U1 C1 123.98(16) . . ? N1 U1 C17 123.70(15) . . ? N2 U1 C17 30.09(15) . . ? C1 U1 C17 149.67(16) . . ? N1 U1 C20 123.06(16) . . ? N2 U1 C20 30.23(15) . . ? C1 U1 C20 121.62(17) . . ? C17 U1 C20 48.09(16) . . ? N1 U1 C4 29.97(15) . . ? N2 U1 C4 123.01(16) . . ? C1 U1 C4 48.11(16) . . ? C17 U1 C4 121.71(16) . . ? C20 U1 C4 148.30(17) . . ? N1 U1 C2 49.22(15) . . ? N2 U1 C2 152.68(15) . . ? C1 U1 C2 28.72(16) . . ? C17 U1 C2 168.81(16) . . ? C20 U1 C2 141.73(16) . . ? C4 U1 C2 47.38(16) . . ? N1 U1 C19 152.10(16) . . ? N2 U1 C19 49.31(16) . . ? C1 U1 C19 141.19(17) . . ? C17 U1 C19 47.43(16) . . ? C20 U1 C19 29.10(17) . . ? C4 U1 C19 169.04(16) . . ? C2 U1 C19 143.37(16) . . ? N1 U1 C18 152.62(15) . . ? N2 U1 C18 49.34(15) . . ? C1 U1 C18 169.00(17) . . ? C17 U1 C18 28.96(16) . . ? C20 U1 C18 47.72(17) . . ? C4 U1 C18 141.70(17) . . ? C2 U1 C18 156.77(16) . . ? C19 U1 C18 28.37(16) . . ? N1 U1 C3 48.87(15) . . ? N2 U1 C3 151.65(16) . . ? C1 U1 C3 47.17(16) . . ? C17 U1 C3 141.24(16) . . ? C20 U1 C3 168.75(17) . . ? C4 U1 C3 28.70(16) . . ? C2 U1 C3 28.20(16) . . ? C19 U1 C3 157.66(17) . . ? C18 U1 C3 143.39(16) . . ? N1 U1 C29 72.53(15) . . ? N2 U1 C29 72.80(14) . . ? C1 U1 C29 61.06(16) . . ? C17 U1 C29 102.38(15) . . ? C20 U1 C29 60.62(16) . . ? C4 U1 C29 102.10(16) . . ? C2 U1 C29 84.12(16) . . ? C19 U1 C29 83.51(16) . . ? C18 U1 C29 108.11(16) . . ? C3 U1 C29 108.14(15) . . ? N1 U1 C9 72.07(15) . . ? N2 U1 C9 72.76(15) . . ? C1 U1 C9 102.06(16) . . ? C17 U1 C9 61.62(16) . . ? C20 U1 C9 102.66(16) . . ? C4 U1 C9 60.16(16) . . ? C2 U1 C9 107.32(16) . . ? C19 U1 C9 108.91(16) . . ? C18 U1 C9 84.62(16) . . ? C3 U1 C9 82.80(16) . . ? C29 U1 C9 118.38(14) . . ? 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 N1 C1 C2 C3 -4.2(7) . . . . ? C30 C1 C2 C3 162.9(6) . . . . ? U1 C1 C2 C3 -68.6(4) . . . . ? N1 C1 C2 U1 64.5(4) . . . . ? C30 C1 C2 U1 -128.4(6) . . . . ? C1 C2 C3 C4 1.2(7) . . . . ? U1 C2 C3 C4 -61.5(4) . . . . ? C1 C2 C3 U1 62.7(4) . . . . ? C2 C3 C4 N1 2.3(7) . . . . ? U1 C3 C4 N1 -63.1(4) . . . . ? C2 C3 C4 C5 -166.1(6) . . . . ? U1 C3 C4 C5 128.5(6) . . . . ? C2 C3 C4 U1 65.4(4) . . . . ? N1 C4 C5 C8 52.1(7) . . . . ? C3 C4 C5 C8 -140.5(6) . . . . ? U1 C4 C5 C8 -30.0(6) . . . . ? N1 C4 C5 C7 174.0(5) . . . . ? C3 C4 C5 C7 -18.6(9) . . . . ? U1 C4 C5 C7 91.9(5) . . . . ? N1 C4 C5 C6 -68.2(7) . . . . ? C3 C4 C5 C6 99.2(7) . . . . ? U1 C4 C5 C6 -150.2(4) . . . . ? C4 C5 C8 C9 55.7(6) . . . . ? C7 C5 C8 C9 -66.3(7) . . . . ? C6 C5 C8 C9 172.0(5) . . . . ? C4 C5 C8 C13 -122.4(6) . . . . ? C7 C5 C8 C13 115.6(6) . . . . ? C6 C5 C8 C13 -6.1(8) . . . . ? C13 C8 C9 C10 3.4(8) . . . . ? C5 C8 C9 C10 -174.9(5) . . . . ? C13 C8 C9 U1 127.7(4) . . . . ? C5 C8 C9 U1 -50.6(5) . . . . ? C8 C9 C10 C11 -4.3(8) . . . . ? U1 C9 C10 C11 -129.3(4) . . . . ? C8 C9 C10 C14 174.9(5) . . . . ? U1 C9 C10 C14 50.0(5) . . . . ? C9 C10 C11 C12 1.7(8) . . . . ? C14 C10 C11 C12 -177.5(5) . . . . ? C10 C11 C12 C13 1.7(9) . . . . ? C11 C12 C13 C8 -2.7(9) . . . . ? C9 C8 C13 C12 0.2(8) . . . . ? C5 C8 C13 C12 178.3(5) . . . . ? C11 C10 C14 C17 121.6(6) . . . . ? C9 C10 C14 C17 -57.6(6) . . . . ? C11 C10 C14 C15 -116.3(6) . . . . ? C9 C10 C14 C15 64.6(6) . . . . ? C11 C10 C14 C16 5.3(8) . . . . ? C9 C10 C14 C16 -173.8(5) . . . . ? C10 C14 C17 N2 -50.8(7) . . . . ? C15 C14 C17 N2 -172.6(5) . . . . ? C16 C14 C17 N2 69.2(7) . . . . ? C10 C14 C17 C18 140.6(6) . . . . ? C15 C14 C17 C18 18.8(8) . . . . ? C16 C14 C17 C18 -99.3(7) . . . . ? C10 C14 C17 U1 32.2(6) . . . . ? C15 C14 C17 U1 -89.6(5) . . . . ? C16 C14 C17 U1 152.2(4) . . . . ? N2 C17 C18 C19 -2.6(7) . . . . ? C14 C17 C18 C19 166.8(6) . . . . ? U1 C17 C18 C19 -67.1(4) . . . . ? N2 C17 C18 U1 64.5(4) . . . . ? C14 C17 C18 U1 -126.1(6) . . . . ? C17 C18 C19 C20 -0.4(7) . . . . ? U1 C18 C19 C20 -62.5(4) . . . . ? C17 C18 C19 U1 62.1(4) . . . . ? C18 C19 C20 N2 3.1(7) . . . . ? U1 C19 C20 N2 -64.0(4) . . . . ? C18 C19 C20 C21 -165.3(6) . . . . ? U1 C19 C20 C21 127.5(6) . . . . ? C18 C19 C20 U1 67.2(4) . . . . ? N2 C20 C21 C24 53.2(7) . . . . ? C19 C20 C21 C24 -139.4(6) . . . . ? U1 C20 C21 C24 -30.2(6) . . . . ? N2 C20 C21 C22 -67.1(7) . . . . ? C19 C20 C21 C22 100.3(7) . . . . ? U1 C20 C21 C22 -150.5(4) . . . . ? N2 C20 C21 C23 173.8(5) . . . . ? C19 C20 C21 C23 -18.7(8) . . . . ? U1 C20 C21 C23 90.5(5) . . . . ? C20 C21 C24 C25 -124.5(5) . . . . ? C22 C21 C24 C25 -7.9(7) . . . . ? C23 C21 C24 C25 114.3(6) . . . . ? C20 C21 C24 C29 54.9(6) . . . . ? C22 C21 C24 C29 171.5(5) . . . . ? C23 C21 C24 C29 -66.3(6) . . . . ? C29 C24 C25 C26 -1.6(8) . . . . ? C21 C24 C25 C26 177.8(5) . . . . ? C24 C25 C26 C27 -1.7(8) . . . . ? C25 C26 C27 C28 3.4(8) . . . . ? C26 C27 C28 C29 -1.6(8) . . . . ? C26 C27 C28 C30 -178.6(5) . . . . ? C25 C24 C29 C28 3.4(8) . . . . ? C21 C24 C29 C28 -176.0(5) . . . . ? C25 C24 C29 U1 129.6(4) . . . . ? C21 C24 C29 U1 -49.8(5) . . . . ? C27 C28 C29 C24 -1.8(8) . . . . ? C30 C28 C29 C24 175.4(5) . . . . ? C27 C28 C29 U1 -128.3(4) . . . . ? C30 C28 C29 U1 48.9(5) . . . . ? N1 C1 C30 C28 -52.0(6) . . . . ? C2 C1 C30 C28 141.9(6) . . . . ? U1 C1 C30 C28 31.0(6) . . . . ? N1 C1 C30 C32 69.3(6) . . . . ? C2 C1 C30 C32 -96.8(7) . . . . ? U1 C1 C30 C32 152.3(4) . . . . ? N1 C1 C30 C31 -172.8(5) . . . . ? C2 C1 C30 C31 21.1(8) . . . . ? U1 C1 C30 C31 -89.8(5) . . . . ? C27 C28 C30 C1 121.9(6) . . . . ? C29 C28 C30 C1 -55.0(6) . . . . ? C27 C28 C30 C32 5.9(7) . . . . ? C29 C28 C30 C32 -171.0(4) . . . . ? C27 C28 C30 C31 -116.7(6) . . . . ? C29 C28 C30 C31 66.4(6) . . . . ? C3 C4 N1 C1 -4.8(6) . . . . ? C5 C4 N1 C1 164.9(5) . . . . ? U1 C4 N1 C1 -77.6(4) . . . . ? C3 C4 N1 U1 72.9(4) . . . . ? C5 C4 N1 U1 -117.5(5) . . . . ? C2 C1 N1 C4 5.5(6) . . . . ? C30 C1 N1 C4 -163.2(5) . . . . ? U1 C1 N1 C4 79.0(4) . . . . ? C2 C1 N1 U1 -73.4(4) . . . . ? C30 C1 N1 U1 117.9(5) . . . . ? C18 C17 N2 C20 4.5(6) . . . . ? C14 C17 N2 C20 -166.0(5) . . . . ? U1 C17 N2 C20 77.5(4) . . . . ? C18 C17 N2 U1 -73.1(4) . . . . ? C14 C17 N2 U1 116.4(5) . . . . ? C19 C20 N2 C17 -4.7(6) . . . . ? C21 C20 N2 C17 165.1(5) . . . . ? U1 C20 N2 C17 -77.3(4) . . . . ? C19 C20 N2 U1 72.6(4) . . . . ? C21 C20 N2 U1 -117.7(5) . . . . ? C4 N1 U1 N2 125.2(3) . . . . ? C1 N1 U1 N2 -126.8(3) . . . . ? C4 N1 U1 C1 -108.1(4) . . . . ? C4 N1 U1 C17 96.2(3) . . . . ? C1 N1 U1 C17 -155.7(3) . . . . ? C4 N1 U1 C20 154.6(3) . . . . ? C1 N1 U1 C20 -97.3(3) . . . . ? C1 N1 U1 C4 108.1(4) . . . . ? C4 N1 U1 C2 -72.9(3) . . . . ? C1 N1 U1 C2 35.2(3) . . . . ? C4 N1 U1 C19 157.6(3) . . . . ? C1 N1 U1 C19 -94.3(4) . . . . ? C4 N1 U1 C18 93.9(4) . . . . ? C1 N1 U1 C18 -158.1(4) . . . . ? C4 N1 U1 C3 -35.2(3) . . . . ? C1 N1 U1 C3 72.8(3) . . . . ? C4 N1 U1 C29 -170.3(3) . . . . ? C1 N1 U1 C29 -62.3(3) . . . . ? C4 N1 U1 C9 60.9(3) . . . . ? C1 N1 U1 C9 169.0(3) . . . . ? C17 N2 U1 N1 -126.6(3) . . . . ? C20 N2 U1 N1 125.1(3) . . . . ? C17 N2 U1 C1 -155.9(3) . . . . ? C20 N2 U1 C1 95.7(3) . . . . ? C20 N2 U1 C17 -108.4(5) . . . . ? C17 N2 U1 C20 108.4(5) . . . . ? C17 N2 U1 C4 -97.4(3) . . . . ? C20 N2 U1 C4 154.2(3) . . . . ? C17 N2 U1 C2 -157.3(4) . . . . ? C20 N2 U1 C2 94.3(4) . . . . ? C17 N2 U1 C19 72.8(3) . . . . ? C20 N2 U1 C19 -35.6(3) . . . . ? C17 N2 U1 C18 35.1(3) . . . . ? C20 N2 U1 C18 -73.3(3) . . . . ? C17 N2 U1 C3 -94.4(4) . . . . ? C20 N2 U1 C3 157.2(4) . . . . ? C17 N2 U1 C29 169.1(3) . . . . ? C20 N2 U1 C29 60.7(3) . . . . ? C17 N2 U1 C9 -62.8(3) . . . . ? C20 N2 U1 C9 -171.2(3) . . . . ? C2 C1 U1 N1 114.8(5) . . . . ? C30 C1 U1 N1 -111.6(5) . . . . ? N1 C1 U1 N2 66.5(3) . . . . ? C2 C1 U1 N2 -178.7(3) . . . . ? C30 C1 U1 N2 -45.1(5) . . . . ? N1 C1 U1 C17 42.6(5) . . . . ? C2 C1 U1 C17 157.4(3) . . . . ? C30 C1 U1 C17 -69.0(5) . . . . ? N1 C1 U1 C20 102.5(3) . . . . ? C2 C1 U1 C20 -142.7(3) . . . . ? C30 C1 U1 C20 -9.0(5) . . . . ? N1 C1 U1 C4 -39.6(3) . . . . ? C2 C1 U1 C4 75.2(4) . . . . ? C30 C1 U1 C4 -151.2(5) . . . . ? N1 C1 U1 C2 -114.8(5) . . . . ? C30 C1 U1 C2 133.6(6) . . . . ? N1 C1 U1 C19 131.9(3) . . . . ? C2 C1 U1 C19 -113.3(4) . . . . ? C30 C1 U1 C19 20.3(5) . . . . ? N1 C1 U1 C18 115.9(8) . . . . ? C2 C1 U1 C18 -129.3(8) . . . . ? C30 C1 U1 C18 4.3(11) . . . . ? N1 C1 U1 C3 -78.8(3) . . . . ? C2 C1 U1 C3 36.0(3) . . . . ? C30 C1 U1 C3 169.6(5) . . . . ? N1 C1 U1 C29 105.2(3) . . . . ? C2 C1 U1 C29 -140.0(4) . . . . ? C30 C1 U1 C29 -6.4(4) . . . . ? N1 C1 U1 C9 -10.7(3) . . . . ? C2 C1 U1 C9 104.1(3) . . . . ? C30 C1 U1 C9 -122.3(4) . . . . ? N2 C17 U1 N1 66.5(3) . . . . ? C18 C17 U1 N1 -177.8(3) . . . . ? C14 C17 U1 N1 -45.9(5) . . . . ? C18 C17 U1 N2 115.8(5) . . . . ? C14 C17 U1 N2 -112.4(6) . . . . ? N2 C17 U1 C1 42.1(5) . . . . ? C18 C17 U1 C1 157.8(4) . . . . ? C14 C17 U1 C1 -70.3(6) . . . . ? N2 C17 U1 C20 -39.9(3) . . . . ? C18 C17 U1 C20 75.8(4) . . . . ? C14 C17 U1 C20 -152.3(5) . . . . ? N2 C17 U1 C4 102.2(3) . . . . ? C18 C17 U1 C4 -142.1(3) . . . . ? C14 C17 U1 C4 -10.2(5) . . . . ? N2 C17 U1 C2 114.1(8) . . . . ? C18 C17 U1 C2 -130.2(8) . . . . ? C14 C17 U1 C2 1.7(11) . . . . ? N2 C17 U1 C19 -79.6(3) . . . . ? C18 C17 U1 C19 36.1(3) . . . . ? C14 C17 U1 C19 168.0(5) . . . . ? N2 C17 U1 C18 -115.8(5) . . . . ? C14 C17 U1 C18 131.9(6) . . . . ? N2 C17 U1 C3 130.9(3) . . . . ? C18 C17 U1 C3 -113.4(4) . . . . ? C14 C17 U1 C3 18.5(6) . . . . ? N2 C17 U1 C29 -10.6(3) . . . . ? C18 C17 U1 C29 105.1(3) . . . . ? C14 C17 U1 C29 -123.0(4) . . . . ? N2 C17 U1 C9 105.1(3) . . . . ? C18 C17 U1 C9 -139.1(4) . . . . ? C14 C17 U1 C9 -7.2(4) . . . . ? N2 C20 U1 N1 -68.0(3) . . . . ? C19 C20 U1 N1 177.1(3) . . . . ? C21 C20 U1 N1 44.7(5) . . . . ? C19 C20 U1 N2 -114.9(5) . . . . ? C21 C20 U1 N2 112.7(6) . . . . ? N2 C20 U1 C1 -104.3(3) . . . . ? C19 C20 U1 C1 140.8(3) . . . . ? C21 C20 U1 C1 8.4(5) . . . . ? N2 C20 U1 C17 39.7(3) . . . . ? C19 C20 U1 C17 -75.1(4) . . . . ? C21 C20 U1 C17 152.4(5) . . . . ? N2 C20 U1 C4 -44.0(5) . . . . ? C19 C20 U1 C4 -158.9(3) . . . . ? C21 C20 U1 C4 68.7(5) . . . . ? N2 C20 U1 C2 -132.4(3) . . . . ? C19 C20 U1 C2 112.8(4) . . . . ? C21 C20 U1 C2 -19.7(6) . . . . ? N2 C20 U1 C19 114.9(5) . . . . ? C21 C20 U1 C19 -132.4(6) . . . . ? N2 C20 U1 C18 79.1(3) . . . . ? C19 C20 U1 C18 -35.8(3) . . . . ? C21 C20 U1 C18 -168.2(5) . . . . ? N2 C20 U1 C3 -109.4(8) . . . . ? C19 C20 U1 C3 135.7(8) . . . . ? C21 C20 U1 C3 3.3(11) . . . . ? N2 C20 U1 C29 -107.0(3) . . . . ? C19 C20 U1 C29 138.1(4) . . . . ? C21 C20 U1 C29 5.7(4) . . . . ? N2 C20 U1 C9 8.6(3) . . . . ? C19 C20 U1 C9 -106.2(3) . . . . ? C21 C20 U1 C9 121.3(4) . . . . ? C3 C4 U1 N1 -115.2(5) . . . . ? C5 C4 U1 N1 112.0(6) . . . . ? N1 C4 U1 N2 -67.8(3) . . . . ? C3 C4 U1 N2 177.0(3) . . . . ? C5 C4 U1 N2 44.2(5) . . . . ? N1 C4 U1 C1 40.4(3) . . . . ? C3 C4 U1 C1 -74.7(4) . . . . ? C5 C4 U1 C1 152.4(5) . . . . ? N1 C4 U1 C17 -103.5(3) . . . . ? C3 C4 U1 C17 141.3(3) . . . . ? C5 C4 U1 C17 8.4(5) . . . . ? N1 C4 U1 C20 -43.1(5) . . . . ? C3 C4 U1 C20 -158.3(3) . . . . ? C5 C4 U1 C20 68.8(6) . . . . ? N1 C4 U1 C2 79.6(3) . . . . ? C3 C4 U1 C2 -35.6(3) . . . . ? C5 C4 U1 C2 -168.5(5) . . . . ? N1 C4 U1 C19 -110.5(9) . . . . ? C3 C4 U1 C19 134.3(8) . . . . ? C5 C4 U1 C19 1.5(12) . . . . ? N1 C4 U1 C18 -132.2(3) . . . . ? C3 C4 U1 C18 112.6(4) . . . . ? C5 C4 U1 C18 -20.3(6) . . . . ? N1 C4 U1 C3 115.2(5) . . . . ? C5 C4 U1 C3 -132.9(6) . . . . ? N1 C4 U1 C29 9.4(3) . . . . ? C3 C4 U1 C29 -105.7(3) . . . . ? C5 C4 U1 C29 121.4(4) . . . . ? N1 C4 U1 C9 -106.5(3) . . . . ? C3 C4 U1 C9 138.3(4) . . . . ? C5 C4 U1 C9 5.5(4) . . . . ? C1 C2 U1 N1 -37.5(3) . . . . ? C3 C2 U1 N1 76.7(3) . . . . ? C1 C2 U1 N2 2.3(5) . . . . ? C3 C2 U1 N2 116.6(4) . . . . ? C3 C2 U1 C1 114.2(5) . . . . ? C1 C2 U1 C17 -91.7(9) . . . . ? C3 C2 U1 C17 22.5(10) . . . . ? C1 C2 U1 C20 56.5(4) . . . . ? C3 C2 U1 C20 170.7(3) . . . . ? C1 C2 U1 C4 -78.0(4) . . . . ? C3 C2 U1 C4 36.3(3) . . . . ? C1 C2 U1 C19 105.2(4) . . . . ? C3 C2 U1 C19 -140.5(3) . . . . ? C1 C2 U1 C18 158.0(4) . . . . ? C3 C2 U1 C18 -87.8(5) . . . . ? C1 C2 U1 C3 -114.2(5) . . . . ? C1 C2 U1 C29 34.5(3) . . . . ? C3 C2 U1 C29 148.7(3) . . . . ? C1 C2 U1 C9 -83.5(3) . . . . ? C3 C2 U1 C9 30.7(4) . . . . ? C18 C19 U1 N1 -119.8(4) . . . . ? C20 C19 U1 N1 -5.2(5) . . . . ? C18 C19 U1 N2 -77.5(4) . . . . ? C20 C19 U1 N2 37.0(3) . . . . ? C18 C19 U1 C1 -173.7(3) . . . . ? C20 C19 U1 C1 -59.1(4) . . . . ? C18 C19 U1 C17 -36.9(3) . . . . ? C20 C19 U1 C17 77.6(3) . . . . ? C18 C19 U1 C20 -114.6(5) . . . . ? C18 C19 U1 C4 -28.9(10) . . . . ? C20 C19 U1 C4 85.7(9) . . . . ? C18 C19 U1 C2 138.6(3) . . . . ? C20 C19 U1 C2 -106.8(4) . . . . ? C20 C19 U1 C18 114.6(5) . . . . ? C18 C19 U1 C3 86.5(5) . . . . ? C20 C19 U1 C3 -159.0(4) . . . . ? C18 C19 U1 C29 -150.4(3) . . . . ? C20 C19 U1 C29 -35.8(3) . . . . ? C18 C19 U1 C9 -32.5(4) . . . . ? C20 C19 U1 C9 82.0(3) . . . . ? C17 C18 U1 N1 4.0(6) . . . . ? C19 C18 U1 N1 117.9(4) . . . . ? C17 C18 U1 N2 -36.5(3) . . . . ? C19 C18 U1 N2 77.4(4) . . . . ? C17 C18 U1 C1 -92.6(9) . . . . ? C19 C18 U1 C1 21.3(10) . . . . ? C19 C18 U1 C17 113.9(5) . . . . ? C17 C18 U1 C20 -77.2(4) . . . . ? C19 C18 U1 C20 36.7(3) . . . . ? C17 C18 U1 C4 57.5(5) . . . . ? C19 C18 U1 C4 171.5(3) . . . . ? C17 C18 U1 C2 157.9(4) . . . . ? C19 C18 U1 C2 -88.2(5) . . . . ? C17 C18 U1 C19 -113.9(5) . . . . ? C17 C18 U1 C3 105.6(4) . . . . ? C19 C18 U1 C3 -140.5(3) . . . . ? C17 C18 U1 C29 -82.8(3) . . . . ? C19 C18 U1 C29 31.1(4) . . . . ? C17 C18 U1 C9 35.3(3) . . . . ? C19 C18 U1 C9 149.3(3) . . . . ? C4 C3 U1 N1 36.9(3) . . . . ? C2 C3 U1 N1 -78.1(4) . . . . ? C4 C3 U1 N2 -5.2(5) . . . . ? C2 C3 U1 N2 -120.2(4) . . . . ? C4 C3 U1 C1 78.3(4) . . . . ? C2 C3 U1 C1 -36.7(3) . . . . ? C4 C3 U1 C17 -58.2(4) . . . . ? C2 C3 U1 C17 -173.2(3) . . . . ? C4 C3 U1 C20 84.2(9) . . . . ? C2 C3 U1 C20 -30.8(10) . . . . ? C2 C3 U1 C4 -115.0(5) . . . . ? C4 C3 U1 C2 115.0(5) . . . . ? C4 C3 U1 C19 -159.0(4) . . . . ? C2 C3 U1 C19 86.0(5) . . . . ? C4 C3 U1 C18 -106.4(4) . . . . ? C2 C3 U1 C18 138.6(3) . . . . ? C4 C3 U1 C29 82.0(3) . . . . ? C2 C3 U1 C29 -33.0(4) . . . . ? C4 C3 U1 C9 -35.5(3) . . . . ? C2 C3 U1 C9 -150.5(3) . . . . ? C24 C29 U1 N1 -124.8(4) . . . . ? C28 C29 U1 N1 9.8(3) . . . . ? C24 C29 U1 N2 -8.6(3) . . . . ? C28 C29 U1 N2 126.0(3) . . . . ? C24 C29 U1 C1 -155.7(4) . . . . ? C28 C29 U1 C1 -21.1(3) . . . . ? C24 C29 U1 C17 -3.0(4) . . . . ? C28 C29 U1 C17 131.6(3) . . . . ? C24 C29 U1 C20 21.7(3) . . . . ? C28 C29 U1 C20 156.3(4) . . . . ? C24 C29 U1 C4 -129.7(4) . . . . ? C28 C29 U1 C4 4.9(3) . . . . ? C24 C29 U1 C2 -173.8(4) . . . . ? C28 C29 U1 C2 -39.2(3) . . . . ? C24 C29 U1 C19 40.8(4) . . . . ? C28 C29 U1 C19 175.4(3) . . . . ? C24 C29 U1 C18 26.5(4) . . . . ? C28 C29 U1 C18 161.1(3) . . . . ? C24 C29 U1 C3 -158.8(3) . . . . ? C28 C29 U1 C3 -24.2(4) . . . . ? C24 C29 U1 C9 -67.2(4) . . . . ? C28 C29 U1 C9 67.4(4) . . . . ? C8 C9 U1 N1 -8.3(4) . . . . ? C10 C9 U1 N1 126.4(4) . . . . ? C8 C9 U1 N2 -124.7(4) . . . . ? C10 C9 U1 N2 10.0(4) . . . . ? C8 C9 U1 C1 -2.6(4) . . . . ? C10 C9 U1 C1 132.1(4) . . . . ? C8 C9 U1 C17 -155.2(4) . . . . ? C10 C9 U1 C17 -20.5(4) . . . . ? C8 C9 U1 C20 -129.3(4) . . . . ? C10 C9 U1 C20 5.4(4) . . . . ? C8 C9 U1 C4 21.9(4) . . . . ? C10 C9 U1 C4 156.7(4) . . . . ? C8 C9 U1 C2 26.6(4) . . . . ? C10 C9 U1 C2 161.4(4) . . . . ? C8 C9 U1 C19 -158.9(4) . . . . ? C10 C9 U1 C19 -24.1(4) . . . . ? C8 C9 U1 C18 -173.7(4) . . . . ? C10 C9 U1 C18 -39.0(4) . . . . ? C8 C9 U1 C3 40.7(4) . . . . ? C10 C9 U1 C3 175.4(4) . . . . ? C8 C9 U1 C29 -66.0(4) . . . . ? C10 C9 U1 C29 68.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 74.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.304 _refine_diff_density_min -2.262 _refine_diff_density_rms 0.217 _database_code_depnum_ccdc_archive 'CCDC 951385' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p12117-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H114 Cl2 K2 N4 O4 Th2' _chemical_formula_weight 1880.99 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 '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' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/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 10.5523(2) _cell_length_b 18.0034(5) _cell_length_c 23.5696(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.237(2) _cell_angle_gamma 90.00 _cell_volume 4431.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 9453 _cell_measurement_theta_min 2.9815 _cell_measurement_theta_max 27.4244 _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.6124 _exptl_crystal_size_mid 0.0464 _exptl_crystal_size_min 0.0446 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 3.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55605 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method 'w\ scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10153 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10153 _reflns_number_gt 7806 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution sir-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep _computing_publication_material mercury _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 204 33 ' ' 2 0.500 1.000 0.500 204 33 ' ' _platon_squeeze_details ; ; _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^)+(0.0355P)^2^+50.3272P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10153 _refine_ls_number_parameters 460 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.148 _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 0.6448(7) 0.1771(5) 0.1097(3) 0.0268(17) Uani 1 1 d . . . C2 C 0.7070(7) 0.1256(5) 0.0787(4) 0.0308(19) Uani 1 1 d . . . H2 H 0.7421 0.1345 0.0444 0.037 Uiso 1 1 calc R . . C3 C 0.7071(7) 0.0575(5) 0.1088(4) 0.0301(18) Uani 1 1 d . . . H3 H 0.7434 0.0118 0.0990 0.036 Uiso 1 1 calc R . . C4 C 0.6434(7) 0.0709(4) 0.1555(3) 0.0252(17) Uani 1 1 d . . . C5 C 0.6309(8) 0.0205(5) 0.2055(4) 0.0322(19) Uani 1 1 d . . . C6 C 0.6684(9) -0.0575(5) 0.1939(5) 0.045(2) Uani 1 1 d . . . H6A H 0.6139 -0.0762 0.1597 0.067 Uiso 1 1 calc R . . H6B H 0.6579 -0.0889 0.2269 0.067 Uiso 1 1 calc R . . H6C H 0.7582 -0.0585 0.1875 0.067 Uiso 1 1 calc R . . C7 C 0.7233(10) 0.0508(6) 0.2577(4) 0.050(3) Uani 1 1 d . . . H7A H 0.7214 0.0179 0.2906 0.074 Uiso 1 1 calc R . . H7B H 0.6962 0.1008 0.2672 0.074 Uiso 1 1 calc R . . H7C H 0.8105 0.0528 0.2480 0.074 Uiso 1 1 calc R . . C8 C 0.4910(8) 0.0200(5) 0.2154(4) 0.0308(19) Uani 1 1 d . . . C9 C 0.3961(7) 0.0194(5) 0.1665(3) 0.0266(17) Uani 1 1 d . . . C10 C 0.2693(7) 0.0010(4) 0.1765(4) 0.0275(17) Uani 1 1 d . . . C11 C 0.2410(9) -0.0069(6) 0.2317(4) 0.043(2) Uani 1 1 d . . . H11 H 0.1558 -0.0183 0.2373 0.052 Uiso 1 1 calc R . . C12 C 0.3328(10) 0.0014(6) 0.2785(4) 0.049(3) Uani 1 1 d . . . H12 H 0.3107 -0.0005 0.3162 0.059 Uiso 1 1 calc R . . C13 C 0.4600(10) 0.0129(6) 0.2699(4) 0.045(2) Uani 1 1 d . . . H13 H 0.5255 0.0159 0.3020 0.055 Uiso 1 1 calc R . . C14 C 0.1702(8) -0.0152(5) 0.1251(4) 0.033(2) Uani 1 1 d . . . C15 C 0.1823(10) -0.0970(5) 0.1080(5) 0.049(3) Uani 1 1 d . . . H15A H 0.1136 -0.1094 0.0769 0.074 Uiso 1 1 calc R . . H15B H 0.1755 -0.1289 0.1412 0.074 Uiso 1 1 calc R . . H15C H 0.2655 -0.1050 0.0951 0.074 Uiso 1 1 calc R . . C16 C 0.0310(8) -0.0013(6) 0.1356(4) 0.044(2) Uani 1 1 d . . . H16A H 0.0221 0.0504 0.1475 0.065 Uiso 1 1 calc R . . H16B H 0.0103 -0.0346 0.1658 0.065 Uiso 1 1 calc R . . H16C H -0.0276 -0.0107 0.1002 0.065 Uiso 1 1 calc R . . C17 C 0.1909(7) 0.0345(5) 0.0758(4) 0.0287(18) Uani 1 1 d . . . C18 C 0.1980(7) 0.0178(5) 0.0187(4) 0.0317(19) Uani 1 1 d . . . H18 H 0.2014 -0.0303 0.0024 0.038 Uiso 1 1 calc R . . C19 C 0.1992(7) 0.0871(5) -0.0104(4) 0.0324(18) Uani 1 1 d . . . H19 H 0.2035 0.0948 -0.0499 0.039 Uiso 1 1 calc R . . C20 C 0.1927(7) 0.1414(5) 0.0314(3) 0.0275(18) Uani 1 1 d . . . C21 C 0.1710(8) 0.2233(5) 0.0238(4) 0.0305(19) Uani 1 1 d . . . C22 C 0.1891(11) 0.2473(6) -0.0366(4) 0.052(3) Uani 1 1 d . . . H22A H 0.2762 0.2351 -0.0434 0.078 Uiso 1 1 calc R . . H22B H 0.1755 0.3010 -0.0407 0.078 Uiso 1 1 calc R . . H22C H 0.1271 0.2212 -0.0646 0.078 Uiso 1 1 calc R . . C23 C 0.0308(9) 0.2384(6) 0.0318(5) 0.050(3) Uani 1 1 d . . . H23A H -0.0262 0.2064 0.0059 0.074 Uiso 1 1 calc R . . H23B H 0.0099 0.2906 0.0232 0.074 Uiso 1 1 calc R . . H23C H 0.0195 0.2276 0.0715 0.074 Uiso 1 1 calc R . . C24 C 0.2706(8) 0.2625(4) 0.0665(4) 0.0285(18) Uani 1 1 d . . . C29 C 0.3975(7) 0.2327(5) 0.0735(4) 0.0277(17) Uani 1 1 d . . . C28 C 0.4920(8) 0.2796(5) 0.1044(4) 0.0328(19) Uani 1 1 d . . . C27 C 0.4606(10) 0.3435(5) 0.1329(4) 0.044(2) Uani 1 1 d . . . H27 H 0.5262 0.3717 0.1549 0.052 Uiso 1 1 calc R . . C26 C 0.3342(11) 0.3658(6) 0.1294(5) 0.058(3) Uani 1 1 d . . . H26 H 0.3122 0.4072 0.1509 0.069 Uiso 1 1 calc R . . C25 C 0.2397(9) 0.3272(6) 0.0942(5) 0.046(2) Uani 1 1 d . . . H25 H 0.1539 0.3447 0.0890 0.055 Uiso 1 1 calc R . . C30 C 0.6323(8) 0.2590(5) 0.1016(4) 0.0332(19) Uani 1 1 d . . . C31 C 0.6626(10) 0.2826(6) 0.0423(5) 0.050(3) Uani 1 1 d . . . H31A H 0.7530 0.2729 0.0399 0.075 Uiso 1 1 calc R . . H31B H 0.6449 0.3357 0.0366 0.075 Uiso 1 1 calc R . . H31C H 0.6090 0.2541 0.0125 0.075 Uiso 1 1 calc R . . C32 C 0.7272(9) 0.2977(6) 0.1485(5) 0.046(3) Uani 1 1 d . . . H32A H 0.7008 0.2887 0.1861 0.069 Uiso 1 1 calc R . . H32B H 0.7275 0.3512 0.1411 0.069 Uiso 1 1 calc R . . H32C H 0.8133 0.2776 0.1481 0.069 Uiso 1 1 calc R . . C33 C 0.0814(13) 0.2944(8) 0.2335(8) 0.084(5) Uani 1 1 d U . . H33A H 0.0329 0.3139 0.1975 0.101 Uiso 1 1 calc R . . H33B H 0.1605 0.3240 0.2431 0.101 Uiso 1 1 calc R . . C34 C 0.0041(17) 0.2980(9) 0.2797(8) 0.101(6) Uani 1 1 d U . . H34A H 0.0550 0.3184 0.3149 0.121 Uiso 1 1 calc R . . H34B H -0.0713 0.3304 0.2688 0.121 Uiso 1 1 calc R . . C35 C -0.0357(18) 0.2235(10) 0.2894(8) 0.114(6) Uani 1 1 d U . . H35A H -0.1298 0.2208 0.2878 0.137 Uiso 1 1 calc R . . H35B H 0.0053 0.2051 0.3272 0.137 Uiso 1 1 calc R . . C36 C 0.0067(14) 0.1796(7) 0.2425(8) 0.091(5) Uani 1 1 d U . . H36A H 0.0333 0.1291 0.2558 0.110 Uiso 1 1 calc R . . H36B H -0.0627 0.1755 0.2096 0.110 Uiso 1 1 calc R . . C37 C 0.5643(14) 0.2636(11) 0.3047(7) 0.094(3) Uani 1 1 d U . . H37A H 0.5766 0.3181 0.3075 0.113 Uiso 1 1 calc R . . H37B H 0.6128 0.2443 0.2749 0.113 Uiso 1 1 calc R . . C38 C 0.6099(16) 0.2272(11) 0.3618(7) 0.104(4) Uani 1 1 d U . . H38A H 0.6541 0.1796 0.3567 0.125 Uiso 1 1 calc R . . H38B H 0.6683 0.2602 0.3869 0.125 Uiso 1 1 calc R . . C39 C 0.4954(16) 0.2156(12) 0.3840(7) 0.108(4) Uani 1 1 d U . . H39A H 0.4920 0.2492 0.4169 0.129 Uiso 1 1 calc R . . H39B H 0.4928 0.1638 0.3980 0.129 Uiso 1 1 calc R . . C40 C 0.3871(14) 0.2286(10) 0.3418(6) 0.090(3) Uani 1 1 d U . . H40A H 0.3324 0.1837 0.3368 0.108 Uiso 1 1 calc R . . H40B H 0.3355 0.2702 0.3539 0.108 Uiso 1 1 calc R . . N1 N 0.6015(6) 0.1434(4) 0.1555(3) 0.0268(15) Uani 1 1 d . . . N2 N 0.1953(6) 0.1102(4) 0.0843(3) 0.0279(15) Uani 1 1 d . . . K1 K 0.3317(2) 0.18474(14) 0.19420(10) 0.0502(6) Uani 1 1 d . . . Th1 Th 0.43687(3) 0.086397(17) 0.070215(13) 0.02560(10) Uani 1 1 d . . . O1 O 0.4311(9) 0.2462(6) 0.2906(4) 0.082(2) Uani 1 1 d U . . O2 O 0.1110(10) 0.2198(6) 0.2273(5) 0.098(4) Uani 1 1 d U . . Cl1 Cl 0.50626(19) 0.07489(12) -0.04150(9) 0.0326(5) Uani 1 1 d . . . C41 C -0.036(3) 0.500(2) 0.1281(12) 0.286(14) Uani 1 1 d DU . . H41A H -0.1058 0.4679 0.1105 0.428 Uiso 1 1 calc R . . H41B H -0.0714 0.5401 0.1493 0.428 Uiso 1 1 calc R . . H41C H 0.0244 0.4708 0.1546 0.428 Uiso 1 1 calc R . . C42 C 0.033(4) 0.533(2) 0.0812(9) 0.288(14) Uani 1 1 d DU . . H42A H 0.1260 0.5218 0.0880 0.345 Uiso 1 1 calc R . . H42B H 0.0218 0.5879 0.0788 0.345 Uiso 1 1 calc R . . C43 C -0.034(3) 0.494(3) 0.0263(7) 0.291(14) Uani 1 1 d DU . . H43A H -0.0391 0.4404 0.0339 0.350 Uiso 1 1 calc R . . H43B H -0.1226 0.5134 0.0175 0.350 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 C1 0.021(4) 0.030(4) 0.029(4) -0.009(3) 0.004(3) -0.002(3) C2 0.014(4) 0.041(5) 0.038(5) -0.005(4) 0.006(3) -0.010(3) C3 0.015(4) 0.035(5) 0.041(5) -0.005(4) 0.005(3) 0.003(3) C4 0.018(4) 0.027(5) 0.030(4) -0.002(3) -0.002(3) 0.003(3) C5 0.023(4) 0.037(5) 0.035(5) 0.010(4) -0.004(3) -0.005(4) C6 0.034(5) 0.033(5) 0.067(7) 0.019(5) 0.005(5) 0.003(4) C7 0.044(6) 0.059(7) 0.040(6) 0.013(5) -0.013(4) -0.014(5) C8 0.029(4) 0.022(4) 0.041(5) 0.006(4) 0.002(4) 0.002(3) C9 0.024(4) 0.028(4) 0.028(4) 0.000(3) 0.007(3) 0.003(3) C10 0.023(4) 0.023(4) 0.037(5) 0.004(3) 0.004(3) 0.004(3) C11 0.032(5) 0.056(6) 0.045(6) 0.007(5) 0.017(4) -0.002(4) C12 0.052(6) 0.065(7) 0.034(5) 0.018(5) 0.014(5) 0.004(5) C13 0.045(6) 0.048(6) 0.042(6) 0.014(5) 0.001(4) 0.001(5) C14 0.024(4) 0.031(5) 0.047(5) -0.005(4) 0.013(4) -0.001(3) C15 0.044(6) 0.037(6) 0.070(7) -0.008(5) 0.019(5) -0.010(4) C16 0.026(5) 0.056(7) 0.049(6) -0.001(5) 0.007(4) -0.001(4) C17 0.018(4) 0.026(4) 0.043(5) -0.012(4) 0.008(3) -0.003(3) C18 0.021(4) 0.037(5) 0.037(5) -0.015(4) 0.006(3) 0.003(3) C19 0.023(4) 0.045(5) 0.029(4) -0.007(4) 0.001(3) 0.009(4) C20 0.019(4) 0.039(5) 0.025(4) -0.002(4) 0.003(3) 0.006(3) C21 0.022(4) 0.037(5) 0.031(4) -0.002(4) 0.001(3) 0.007(3) C22 0.058(7) 0.054(7) 0.038(5) 0.009(5) -0.009(5) 0.010(5) C23 0.032(5) 0.046(6) 0.069(7) -0.008(5) -0.001(5) 0.009(4) C24 0.027(4) 0.021(4) 0.039(5) 0.004(4) 0.007(3) 0.002(3) C29 0.019(4) 0.025(4) 0.039(5) 0.001(4) 0.002(3) -0.001(3) C28 0.031(4) 0.028(5) 0.040(5) 0.002(4) 0.008(4) -0.001(4) C27 0.045(6) 0.032(5) 0.053(6) -0.013(5) 0.003(5) -0.004(4) C26 0.054(7) 0.043(6) 0.075(8) -0.018(6) 0.010(6) 0.009(5) C25 0.034(5) 0.044(6) 0.062(7) -0.009(5) 0.011(5) 0.012(4) C30 0.024(4) 0.030(5) 0.047(5) -0.002(4) 0.007(4) -0.003(3) C31 0.051(6) 0.038(6) 0.066(7) 0.014(5) 0.023(5) 0.000(5) C32 0.030(5) 0.035(5) 0.071(7) -0.013(5) -0.003(5) -0.009(4) C33 0.060(8) 0.062(9) 0.136(14) -0.026(9) 0.034(9) -0.009(7) C34 0.104(12) 0.080(11) 0.127(14) -0.050(10) 0.046(11) -0.003(9) C35 0.116(14) 0.110(14) 0.134(16) -0.030(12) 0.077(12) -0.019(11) C36 0.076(9) 0.051(8) 0.159(16) -0.008(9) 0.059(10) -0.014(7) C37 0.079(6) 0.125(8) 0.078(6) -0.005(6) 0.013(5) -0.005(6) C38 0.086(6) 0.138(9) 0.085(7) 0.000(7) 0.001(6) -0.004(7) C39 0.091(7) 0.152(9) 0.077(6) 0.009(7) 0.003(5) -0.001(7) C40 0.080(6) 0.133(8) 0.057(6) -0.002(6) 0.015(5) -0.006(6) N1 0.023(3) 0.028(4) 0.029(4) -0.003(3) 0.002(3) 0.000(3) N2 0.020(3) 0.033(4) 0.032(4) -0.005(3) 0.008(3) 0.005(3) K1 0.0616(14) 0.0525(14) 0.0404(12) -0.0079(10) 0.0205(11) 0.0058(11) Th1 0.01794(14) 0.02935(16) 0.02978(16) -0.00213(15) 0.00436(10) -0.00088(13) O1 0.075(5) 0.118(7) 0.057(4) -0.015(5) 0.019(4) -0.007(5) O2 0.092(7) 0.075(7) 0.145(10) -0.048(7) 0.075(7) -0.018(5) Cl1 0.0298(10) 0.0354(12) 0.0341(10) -0.0043(9) 0.0093(8) 0.0001(8) C41 0.20(3) 0.39(4) 0.26(4) 0.02(3) -0.01(2) 0.01(2) C42 0.20(3) 0.39(4) 0.26(4) 0.03(3) -0.01(2) 0.01(2) C43 0.21(3) 0.39(4) 0.27(4) 0.03(3) -0.01(2) 0.02(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.373(10) . ? C1 C2 1.399(11) . ? C1 C30 1.491(12) . ? C1 Th1 2.786(8) . ? C2 C3 1.416(12) . ? C2 Th1 2.915(7) . ? C2 H2 0.9500 . ? C3 C4 1.391(11) . ? C3 Th1 2.913(8) . ? C3 H3 0.9500 . ? C4 N1 1.379(10) . ? C4 C5 1.507(11) . ? C4 Th1 2.760(7) . ? C5 C6 1.494(13) . ? C5 C8 1.528(12) . ? C5 C7 1.554(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.376(13) . ? C8 C9 1.415(12) . ? C8 K1 3.411(8) . ? C9 C10 1.431(11) . ? C9 Th1 2.658(8) . ? C9 K1 3.143(8) . ? C10 C11 1.383(12) . ? C10 C14 1.512(12) . ? C10 K1 3.388(9) . ? C11 C12 1.367(14) . ? C11 H11 0.9500 . ? C12 C13 1.402(14) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.507(13) . ? C14 C15 1.537(13) . ? C14 C16 1.544(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N2 1.378(11) . ? C17 C18 1.392(12) . ? C17 Th1 2.780(8) . ? C18 C19 1.425(13) . ? C18 Th1 2.911(8) . ? C18 H18 0.9500 . ? C19 C20 1.396(12) . ? C19 Th1 2.921(8) . ? C19 H19 0.9500 . ? C20 N2 1.363(11) . ? C20 C21 1.499(12) . ? C20 Th1 2.790(8) . ? C21 C24 1.520(12) . ? C21 C22 1.524(13) . ? C21 C23 1.543(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.396(12) . ? C24 C29 1.431(11) . ? C24 K1 3.299(9) . ? C29 C28 1.424(12) . ? C29 Th1 2.670(8) . ? C29 K1 3.144(9) . ? C28 C27 1.396(13) . ? C28 C30 1.536(11) . ? C28 K1 3.360(9) . ? C27 C26 1.384(14) . ? C27 H27 0.9500 . ? C26 C25 1.389(15) . ? C26 H26 0.9500 . ? C25 K1 3.524(11) . ? C25 H25 0.9500 . ? C30 C31 1.539(13) . ? C30 C32 1.546(12) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 O2 1.392(16) . ? C33 C34 1.45(2) . ? C33 K1 3.526(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.43(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.48(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O2 1.406(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O1 1.432(17) . ? C37 C38 1.51(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.40(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.42(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O1 1.390(15) . ? C40 K1 3.534(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N1 Th1 2.666(7) . ? N1 K1 3.199(7) . ? N2 Th1 2.653(6) . ? N2 K1 3.084(7) . ? K1 O1 2.608(9) . ? K1 O2 2.636(9) . ? Th1 Cl1 2.840(2) . ? Cl1 Th1 3.060(2) 3_655 ? C41 C42 1.534(19) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.553(19) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C43 1.532(19) 3_565 ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.6(8) . . ? N1 C1 C30 120.2(7) . . ? C2 C1 C30 129.0(8) . . ? N1 C1 Th1 70.6(4) . . ? C2 C1 Th1 81.0(5) . . ? C30 C1 Th1 119.1(5) . . ? C1 C2 C3 106.2(7) . . ? C1 C2 Th1 70.7(4) . . ? C3 C2 Th1 75.8(4) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? Th1 C2 H2 118.6 . . ? C4 C3 C2 106.3(7) . . ? C4 C3 Th1 69.8(4) . . ? C2 C3 Th1 76.0(4) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? Th1 C3 H3 119.3 . . ? N1 C4 C3 110.7(7) . . ? N1 C4 C5 120.5(7) . . ? C3 C4 C5 128.4(8) . . ? N1 C4 Th1 71.6(4) . . ? C3 C4 Th1 82.0(5) . . ? C5 C4 Th1 118.8(5) . . ? C6 C5 C4 111.6(8) . . ? C6 C5 C8 108.1(7) . . ? C4 C5 C8 108.5(7) . . ? C6 C5 C7 108.8(8) . . ? C4 C5 C7 106.9(7) . . ? C8 C5 C7 113.1(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 121.7(8) . . ? C13 C8 C5 120.4(8) . . ? C9 C8 C5 117.6(8) . . ? C13 C8 K1 92.2(6) . . ? C9 C8 K1 67.1(5) . . ? C5 C8 K1 116.1(5) . . ? C8 C9 C10 115.8(7) . . ? C8 C9 Th1 120.7(6) . . ? C10 C9 Th1 121.1(6) . . ? C8 C9 K1 88.4(5) . . ? C10 C9 K1 87.1(5) . . ? Th1 C9 K1 79.3(2) . . ? C11 C10 C9 120.8(8) . . ? C11 C10 C14 121.1(8) . . ? C9 C10 C14 117.9(7) . . ? C11 C10 K1 92.7(6) . . ? C9 C10 K1 67.9(4) . . ? C14 C10 K1 112.7(5) . . ? C12 C11 C10 121.6(9) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 118.8(9) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C8 C13 C12 120.6(9) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C17 C14 C10 110.1(7) . . ? C17 C14 C15 109.9(8) . . ? C10 C14 C15 108.7(8) . . ? C17 C14 C16 105.9(7) . . ? C10 C14 C16 113.9(7) . . ? C15 C14 C16 108.4(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 110.4(8) . . ? N2 C17 C14 118.8(7) . . ? C18 C17 C14 130.6(8) . . ? N2 C17 Th1 70.3(4) . . ? C18 C17 Th1 81.2(5) . . ? C14 C17 Th1 118.4(5) . . ? C17 C18 C19 106.3(7) . . ? C17 C18 Th1 70.6(5) . . ? C19 C18 Th1 76.2(5) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? Th1 C18 H18 118.4 . . ? C20 C19 C18 105.6(7) . . ? C20 C19 Th1 70.7(4) . . ? C18 C19 Th1 75.5(5) . . ? C20 C19 H19 127.2 . . ? C18 C19 H19 127.2 . . ? Th1 C19 H19 118.8 . . ? N2 C20 C19 111.1(8) . . ? N2 C20 C21 119.9(7) . . ? C19 C20 C21 128.8(8) . . ? N2 C20 Th1 70.0(4) . . ? C19 C20 Th1 81.1(5) . . ? C21 C20 Th1 120.4(5) . . ? C20 C21 C24 107.3(7) . . ? C20 C21 C22 110.7(8) . . ? C24 C21 C22 108.7(8) . . ? C20 C21 C23 106.8(7) . . ? C24 C21 C23 114.9(7) . . ? C22 C21 C23 108.4(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 122.4(8) . . ? C25 C24 C21 120.8(8) . . ? C29 C24 C21 116.7(7) . . ? C25 C24 K1 87.4(6) . . ? C29 C24 K1 71.2(5) . . ? C21 C24 K1 115.7(5) . . ? C28 C29 C24 114.3(7) . . ? C28 C29 Th1 120.0(6) . . ? C24 C29 Th1 120.9(5) . . ? C28 C29 K1 86.0(5) . . ? C24 C29 K1 83.3(5) . . ? Th1 C29 K1 79.1(2) . . ? C27 C28 C29 122.5(8) . . ? C27 C28 C30 121.0(8) . . ? C29 C28 C30 116.4(7) . . ? C27 C28 K1 86.5(6) . . ? C29 C28 K1 69.0(5) . . ? C30 C28 K1 118.6(5) . . ? C26 C27 C28 120.2(9) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C26 C25 119.6(10) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C25 C24 120.1(9) . . ? C26 C25 K1 81.9(7) . . ? C24 C25 K1 69.3(5) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? K1 C25 H25 119.7 . . ? C1 C30 C28 107.6(7) . . ? C1 C30 C31 111.2(8) . . ? C28 C30 C31 107.3(8) . . ? C1 C30 C32 108.5(7) . . ? C28 C30 C32 113.0(8) . . ? C31 C30 C32 109.2(8) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 C34 106.4(13) . . ? O2 C33 K1 40.9(6) . . ? C34 C33 K1 138.1(12) . . ? O2 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? K1 C33 H33A 106.8 . . ? O2 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? K1 C33 H33B 73.9 . . ? H33A C33 H33B 108.6 . . ? C35 C34 C33 106.5(12) . . ? C35 C34 H34A 110.4 . . ? C33 C34 H34A 110.4 . . ? C35 C34 H34B 110.4 . . ? C33 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C36 104.8(13) . . ? C34 C35 H35A 110.8 . . ? C36 C35 H35A 110.8 . . ? C34 C35 H35B 110.8 . . ? C36 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? O2 C36 C35 104.4(12) . . ? O2 C36 H36A 110.9 . . ? C35 C36 H36A 110.9 . . ? O2 C36 H36B 110.9 . . ? C35 C36 H36B 110.9 . . ? H36A C36 H36B 108.9 . . ? O1 C37 C38 106.7(13) . . ? O1 C37 H37A 110.4 . . ? C38 C37 H37A 110.4 . . ? O1 C37 H37B 110.4 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C39 C38 C37 102.5(14) . . ? C39 C38 H38A 111.3 . . ? C37 C38 H38A 111.3 . . ? C39 C38 H38B 111.3 . . ? C37 C38 H38B 111.3 . . ? H38A C38 H38B 109.2 . . ? C38 C39 C40 111.4(15) . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? O1 C40 C39 108.0(13) . . ? O1 C40 K1 39.2(6) . . ? C39 C40 K1 130.8(11) . . ? O1 C40 H40A 110.1 . . ? C39 C40 H40A 110.1 . . ? K1 C40 H40A 71.9 . . ? O1 C40 H40B 110.1 . . ? C39 C40 H40B 110.1 . . ? K1 C40 H40B 115.6 . . ? H40A C40 H40B 108.4 . . ? C1 N1 C4 106.0(7) . . ? C1 N1 Th1 80.3(4) . . ? C4 N1 Th1 79.1(4) . . ? C1 N1 K1 122.1(5) . . ? C4 N1 K1 121.2(5) . . ? Th1 N1 K1 78.13(16) . . ? C20 N2 C17 106.3(7) . . ? C20 N2 Th1 81.1(4) . . ? C17 N2 Th1 80.5(4) . . ? C20 N2 K1 122.3(5) . . ? C17 N2 K1 123.6(5) . . ? Th1 N2 K1 80.45(18) . . ? O1 K1 O2 84.4(3) . . ? O1 K1 N2 175.6(2) . . ? O2 K1 N2 91.5(3) . . ? O1 K1 C9 120.7(3) . . ? O2 K1 C9 121.0(3) . . ? N2 K1 C9 60.2(2) . . ? O1 K1 C29 123.9(3) . . ? O2 K1 C29 121.4(3) . . ? N2 K1 C29 59.8(2) . . ? C9 K1 C29 89.4(2) . . ? O1 K1 N1 94.8(2) . . ? O2 K1 N1 179.2(3) . . ? N2 K1 N1 89.24(17) . . ? C9 K1 N1 59.51(19) . . ? C29 K1 N1 58.99(19) . . ? O1 K1 C24 128.1(3) . . ? O2 K1 C24 95.9(3) . . ? N2 K1 C24 53.9(2) . . ? C9 K1 C24 103.4(2) . . ? C29 K1 C24 25.51(19) . . ? N1 K1 C24 84.49(19) . . ? O1 K1 C28 99.1(3) . . ? O2 K1 C28 127.6(3) . . ? N2 K1 C28 84.7(2) . . ? C9 K1 C28 101.9(2) . . ? C29 K1 C28 25.0(2) . . ? N1 K1 C28 52.4(2) . . ? C24 K1 C28 42.2(2) . . ? O1 K1 C10 124.6(3) . . ? O2 K1 C10 96.1(3) . . ? N2 K1 C10 54.1(2) . . ? C9 K1 C10 24.95(19) . . ? C29 K1 C10 102.8(2) . . ? N1 K1 C10 84.43(19) . . ? C24 K1 C10 107.1(2) . . ? C28 K1 C10 121.7(2) . . ? O1 K1 C8 96.5(3) . . ? O2 K1 C8 127.0(3) . . ? N2 K1 C8 84.6(2) . . ? C9 K1 C8 24.5(2) . . ? C29 K1 C8 101.7(2) . . ? N1 K1 C8 53.09(19) . . ? C24 K1 C8 122.0(2) . . ? C28 K1 C8 104.6(2) . . ? C10 K1 C8 41.5(2) . . ? O1 K1 C25 108.2(3) . . ? O2 K1 C25 81.6(3) . . ? N2 K1 C25 72.8(2) . . ? C9 K1 C25 126.7(2) . . ? C29 K1 C25 43.1(2) . . ? N1 K1 C25 98.6(2) . . ? C24 K1 C25 23.3(2) . . ? C28 K1 C25 47.5(2) . . ? C10 K1 C25 126.8(2) . . ? C8 K1 C25 144.4(2) . . ? O1 K1 C33 75.9(3) . . ? O2 K1 C33 20.2(3) . . ? N2 K1 C33 100.8(3) . . ? C9 K1 C33 141.0(3) . . ? C29 K1 C33 110.8(3) . . ? N1 K1 C33 159.4(3) . . ? C24 K1 C33 86.9(3) . . ? C28 K1 C33 110.2(3) . . ? C10 K1 C33 116.1(3) . . ? C8 K1 C33 145.1(3) . . ? C25 K1 C33 67.9(3) . . ? N2 Th1 C9 72.0(2) . . ? N2 Th1 N1 112.2(2) . . ? C9 Th1 N1 72.5(2) . . ? N2 Th1 C29 71.4(2) . . ? C9 Th1 C29 112.2(3) . . ? N1 Th1 C29 71.7(2) . . ? N2 Th1 C4 126.7(2) . . ? C9 Th1 C4 62.6(2) . . ? N1 Th1 C4 29.4(2) . . ? C29 Th1 C4 100.9(2) . . ? N2 Th1 C17 29.3(2) . . ? C9 Th1 C17 62.6(3) . . ? N1 Th1 C17 127.3(2) . . ? C29 Th1 C17 100.4(2) . . ? C4 Th1 C17 125.2(3) . . ? N2 Th1 C1 126.1(2) . . ? C9 Th1 C1 101.4(2) . . ? N1 Th1 C1 29.1(2) . . ? C29 Th1 C1 62.0(2) . . ? C4 Th1 C1 46.7(2) . . ? C17 Th1 C1 151.3(2) . . ? N2 Th1 C20 28.9(2) . . ? C9 Th1 C20 100.7(2) . . ? N1 Th1 C20 125.6(2) . . ? C29 Th1 C20 61.2(2) . . ? C4 Th1 C20 150.5(2) . . ? C17 Th1 C20 46.4(3) . . ? C1 Th1 C20 123.2(3) . . ? N2 Th1 Cl1 120.52(16) . . ? C9 Th1 Cl1 148.53(18) . . ? N1 Th1 Cl1 120.02(15) . . ? C29 Th1 Cl1 99.26(19) . . ? C4 Th1 Cl1 112.75(17) . . ? C17 Th1 Cl1 112.73(18) . . ? C1 Th1 Cl1 93.26(17) . . ? C20 Th1 Cl1 94.05(17) . . ? N2 Th1 C18 48.0(2) . . ? C9 Th1 C18 85.8(3) . . ? N1 Th1 C18 155.4(2) . . ? C29 Th1 C18 107.6(2) . . ? C4 Th1 C18 143.8(3) . . ? C17 Th1 C18 28.2(2) . . ? C1 Th1 C18 168.9(3) . . ? C20 Th1 C18 46.4(2) . . ? Cl1 Th1 C18 84.58(17) . . ? N2 Th1 C3 154.8(2) . . ? C9 Th1 C3 85.6(2) . . ? N1 Th1 C3 48.0(2) . . ? C29 Th1 C3 108.4(2) . . ? C4 Th1 C3 28.2(2) . . ? C17 Th1 C3 143.5(3) . . ? C1 Th1 C3 46.5(2) . . ? C20 Th1 C3 169.3(3) . . ? Cl1 Th1 C3 84.59(17) . . ? C18 Th1 C3 143.6(2) . . ? N2 Th1 C2 154.2(2) . . ? C9 Th1 C2 109.1(2) . . ? N1 Th1 C2 47.9(2) . . ? C29 Th1 C2 85.1(2) . . ? C4 Th1 C2 46.5(2) . . ? C17 Th1 C2 171.3(3) . . ? C1 Th1 C2 28.3(2) . . ? C20 Th1 C2 141.7(3) . . ? Cl1 Th1 C2 72.67(18) . . ? C18 Th1 C2 155.7(2) . . ? C3 Th1 C2 28.1(2) . . ? C40 O1 C37 106.7(11) . . ? C40 O1 K1 121.2(9) . . ? C37 O1 K1 123.7(8) . . ? C33 O2 C36 105.8(10) . . ? C33 O2 K1 118.9(8) . . ? C36 O2 K1 135.2(8) . . ? Th1 Cl1 Th1 111.04(7) . 3_655 ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 C42 C43 102(2) . . ? C41 C42 H42A 111.3 . . ? C43 C42 H42A 111.3 . . ? C41 C42 H42B 111.3 . . ? C43 C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? C43 C43 C42 114(2) 3_565 . ? C43 C43 H43A 108.8 3_565 . ? C42 C43 H43A 108.8 . . ? C43 C43 H43B 108.8 3_565 . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? 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 N1 C1 C2 C3 -2.9(9) . . . . ? C30 C1 C2 C3 171.5(8) . . . . ? Th1 C1 C2 C3 -68.2(5) . . . . ? N1 C1 C2 Th1 65.3(5) . . . . ? C30 C1 C2 Th1 -120.3(9) . . . . ? C1 C2 C3 C4 1.0(9) . . . . ? Th1 C2 C3 C4 -63.6(5) . . . . ? C1 C2 C3 Th1 64.6(5) . . . . ? C2 C3 C4 N1 1.1(9) . . . . ? Th1 C3 C4 N1 -66.8(5) . . . . ? C2 C3 C4 C5 -171.4(7) . . . . ? Th1 C3 C4 C5 120.7(8) . . . . ? C2 C3 C4 Th1 67.9(6) . . . . ? N1 C4 C5 C6 173.6(7) . . . . ? C3 C4 C5 C6 -14.4(12) . . . . ? Th1 C4 C5 C6 89.1(7) . . . . ? N1 C4 C5 C8 54.7(10) . . . . ? C3 C4 C5 C8 -133.3(9) . . . . ? Th1 C4 C5 C8 -29.8(9) . . . . ? N1 C4 C5 C7 -67.5(10) . . . . ? C3 C4 C5 C7 104.4(10) . . . . ? Th1 C4 C5 C7 -152.1(6) . . . . ? C6 C5 C8 C13 92.2(10) . . . . ? C4 C5 C8 C13 -146.7(9) . . . . ? C7 C5 C8 C13 -28.2(12) . . . . ? C6 C5 C8 C9 -81.5(9) . . . . ? C4 C5 C8 C9 39.6(10) . . . . ? C7 C5 C8 C9 158.0(8) . . . . ? C6 C5 C8 K1 -158.0(6) . . . . ? C4 C5 C8 K1 -36.9(8) . . . . ? C7 C5 C8 K1 81.5(8) . . . . ? C13 C8 C9 C10 -8.3(12) . . . . ? C5 C8 C9 C10 165.4(7) . . . . ? K1 C8 C9 C10 -86.1(7) . . . . ? C13 C8 C9 Th1 154.3(7) . . . . ? C5 C8 C9 Th1 -32.0(10) . . . . ? K1 C8 C9 Th1 76.5(5) . . . . ? C13 C8 C9 K1 77.8(9) . . . . ? C5 C8 C9 K1 -108.5(7) . . . . ? C8 C9 C10 C11 7.3(12) . . . . ? Th1 C9 C10 C11 -155.2(7) . . . . ? K1 C9 C10 C11 -79.5(8) . . . . ? C8 C9 C10 C14 -168.2(7) . . . . ? Th1 C9 C10 C14 29.2(10) . . . . ? K1 C9 C10 C14 104.9(7) . . . . ? C8 C9 C10 K1 86.8(7) . . . . ? Th1 C9 C10 K1 -75.7(4) . . . . ? C9 C10 C11 C12 -1.1(15) . . . . ? C14 C10 C11 C12 174.3(9) . . . . ? K1 C10 C11 C12 -66.9(10) . . . . ? C10 C11 C12 C13 -4.6(16) . . . . ? C9 C8 C13 C12 3.0(15) . . . . ? C5 C8 C13 C12 -170.5(9) . . . . ? K1 C8 C13 C12 67.3(10) . . . . ? C11 C12 C13 C8 3.7(16) . . . . ? C11 C10 C14 C17 148.1(8) . . . . ? C9 C10 C14 C17 -36.3(10) . . . . ? K1 C10 C14 C17 39.8(7) . . . . ? C11 C10 C14 C15 -91.5(10) . . . . ? C9 C10 C14 C15 84.1(9) . . . . ? K1 C10 C14 C15 160.2(5) . . . . ? C11 C10 C14 C16 29.4(12) . . . . ? C9 C10 C14 C16 -155.0(8) . . . . ? K1 C10 C14 C16 -78.9(8) . . . . ? C10 C14 C17 N2 -54.6(9) . . . . ? C15 C14 C17 N2 -174.3(7) . . . . ? C16 C14 C17 N2 68.9(9) . . . . ? C10 C14 C17 C18 130.9(9) . . . . ? C15 C14 C17 C18 11.2(12) . . . . ? C16 C14 C17 C18 -105.6(10) . . . . ? C10 C14 C17 Th1 27.4(8) . . . . ? C15 C14 C17 Th1 -92.3(7) . . . . ? C16 C14 C17 Th1 150.8(6) . . . . ? N2 C17 C18 C19 -3.5(9) . . . . ? C14 C17 C18 C19 171.4(8) . . . . ? Th1 C17 C18 C19 -68.5(6) . . . . ? N2 C17 C18 Th1 65.0(5) . . . . ? C14 C17 C18 Th1 -120.1(9) . . . . ? C17 C18 C19 C20 0.0(8) . . . . ? Th1 C18 C19 C20 -64.7(5) . . . . ? C17 C18 C19 Th1 64.7(5) . . . . ? C18 C19 C20 N2 3.6(9) . . . . ? Th1 C19 C20 N2 -64.4(5) . . . . ? C18 C19 C20 C21 -169.8(8) . . . . ? Th1 C19 C20 C21 122.2(8) . . . . ? C18 C19 C20 Th1 68.0(5) . . . . ? N2 C20 C21 C24 54.2(9) . . . . ? C19 C20 C21 C24 -132.9(8) . . . . ? Th1 C20 C21 C24 -28.8(8) . . . . ? N2 C20 C21 C22 172.7(7) . . . . ? C19 C20 C21 C22 -14.4(12) . . . . ? Th1 C20 C21 C22 89.6(8) . . . . ? N2 C20 C21 C23 -69.5(9) . . . . ? C19 C20 C21 C23 103.4(10) . . . . ? Th1 C20 C21 C23 -152.6(6) . . . . ? C20 C21 C24 C25 -142.7(8) . . . . ? C22 C21 C24 C25 97.5(10) . . . . ? C23 C21 C24 C25 -24.1(12) . . . . ? C20 C21 C24 C29 41.3(10) . . . . ? C22 C21 C24 C29 -78.5(10) . . . . ? C23 C21 C24 C29 159.9(8) . . . . ? C20 C21 C24 K1 -39.6(8) . . . . ? C22 C21 C24 K1 -159.3(6) . . . . ? C23 C21 C24 K1 79.1(8) . . . . ? C25 C24 C29 C28 -8.4(13) . . . . ? C21 C24 C29 C28 167.5(8) . . . . ? K1 C24 C29 C28 -82.5(7) . . . . ? C25 C24 C29 Th1 147.1(7) . . . . ? C21 C24 C29 Th1 -36.9(10) . . . . ? K1 C24 C29 Th1 73.0(5) . . . . ? C25 C24 C29 K1 74.1(9) . . . . ? C21 C24 C29 K1 -109.9(7) . . . . ? C24 C29 C28 C27 9.6(13) . . . . ? Th1 C29 C28 C27 -146.2(8) . . . . ? K1 C29 C28 C27 -71.2(9) . . . . ? C24 C29 C28 C30 -166.7(8) . . . . ? Th1 C29 C28 C30 37.5(10) . . . . ? K1 C29 C28 C30 112.5(7) . . . . ? C24 C29 C28 K1 80.8(7) . . . . ? Th1 C29 C28 K1 -75.0(4) . . . . ? C29 C28 C27 C26 -3.6(16) . . . . ? C30 C28 C27 C26 172.6(10) . . . . ? K1 C28 C27 C26 -65.9(10) . . . . ? C28 C27 C26 C25 -4.3(18) . . . . ? C27 C26 C25 C24 5.5(18) . . . . ? C27 C26 C25 K1 65.8(11) . . . . ? C29 C24 C25 C26 1.2(15) . . . . ? C21 C24 C25 C26 -174.6(10) . . . . ? K1 C24 C25 C26 66.9(10) . . . . ? C29 C24 C25 K1 -65.7(8) . . . . ? C21 C24 C25 K1 118.5(8) . . . . ? N1 C1 C30 C28 -51.8(10) . . . . ? C2 C1 C30 C28 134.4(9) . . . . ? Th1 C1 C30 C28 31.6(9) . . . . ? N1 C1 C30 C31 -169.0(7) . . . . ? C2 C1 C30 C31 17.1(12) . . . . ? Th1 C1 C30 C31 -85.6(8) . . . . ? N1 C1 C30 C32 70.8(9) . . . . ? C2 C1 C30 C32 -103.0(10) . . . . ? Th1 C1 C30 C32 154.2(6) . . . . ? C27 C28 C30 C1 139.5(9) . . . . ? C29 C28 C30 C1 -44.1(10) . . . . ? K1 C28 C30 C1 35.2(9) . . . . ? C27 C28 C30 C31 -100.7(10) . . . . ? C29 C28 C30 C31 75.7(10) . . . . ? K1 C28 C30 C31 155.0(6) . . . . ? C27 C28 C30 C32 19.7(12) . . . . ? C29 C28 C30 C32 -163.9(8) . . . . ? K1 C28 C30 C32 -84.6(8) . . . . ? O2 C33 C34 C35 -14(2) . . . . ? K1 C33 C34 C35 -46(2) . . . . ? C33 C34 C35 C36 -7(2) . . . . ? C34 C35 C36 O2 26(2) . . . . ? O1 C37 C38 C39 -20(2) . . . . ? C37 C38 C39 C40 11(2) . . . . ? C38 C39 C40 O1 2(2) . . . . ? C38 C39 C40 K1 40(3) . . . . ? C2 C1 N1 C4 3.5(9) . . . . ? C30 C1 N1 C4 -171.4(7) . . . . ? Th1 C1 N1 C4 75.6(5) . . . . ? C2 C1 N1 Th1 -72.0(6) . . . . ? C30 C1 N1 Th1 113.1(7) . . . . ? C2 C1 N1 K1 -141.3(5) . . . . ? C30 C1 N1 K1 43.8(9) . . . . ? Th1 C1 N1 K1 -69.3(4) . . . . ? C3 C4 N1 C1 -2.9(9) . . . . ? C5 C4 N1 C1 170.4(7) . . . . ? Th1 C4 N1 C1 -76.5(5) . . . . ? C3 C4 N1 Th1 73.6(6) . . . . ? C5 C4 N1 Th1 -113.2(7) . . . . ? C3 C4 N1 K1 142.4(5) . . . . ? C5 C4 N1 K1 -44.4(9) . . . . ? Th1 C4 N1 K1 68.8(4) . . . . ? C19 C20 N2 C17 -5.7(9) . . . . ? C21 C20 N2 C17 168.3(7) . . . . ? Th1 C20 N2 C17 -77.3(5) . . . . ? C19 C20 N2 Th1 71.6(6) . . . . ? C21 C20 N2 Th1 -114.4(7) . . . . ? C19 C20 N2 K1 144.3(5) . . . . ? C21 C20 N2 K1 -41.6(9) . . . . ? Th1 C20 N2 K1 72.7(4) . . . . ? C18 C17 N2 C20 5.7(9) . . . . ? C14 C17 N2 C20 -169.9(7) . . . . ? Th1 C17 N2 C20 77.8(5) . . . . ? C18 C17 N2 Th1 -72.1(6) . . . . ? C14 C17 N2 Th1 112.3(7) . . . . ? C18 C17 N2 K1 -143.8(5) . . . . ? C14 C17 N2 K1 40.6(9) . . . . ? Th1 C17 N2 K1 -71.7(4) . . . . ? C20 N2 K1 O1 130(4) . . . . ? C17 N2 K1 O1 -85(4) . . . . ? Th1 N2 K1 O1 -157(4) . . . . ? C20 N2 K1 O2 107.5(6) . . . . ? C17 N2 K1 O2 -107.6(6) . . . . ? Th1 N2 K1 O2 -179.4(3) . . . . ? C20 N2 K1 C9 -127.1(6) . . . . ? C17 N2 K1 C9 17.7(5) . . . . ? Th1 N2 K1 C9 -54.04(19) . . . . ? C20 N2 K1 C29 -18.4(5) . . . . ? C17 N2 K1 C29 126.4(6) . . . . ? Th1 N2 K1 C29 54.6(2) . . . . ? C20 N2 K1 N1 -72.4(6) . . . . ? C17 N2 K1 N1 72.4(6) . . . . ? Th1 N2 K1 N1 0.69(19) . . . . ? C20 N2 K1 C24 11.4(5) . . . . ? C17 N2 K1 C24 156.2(6) . . . . ? Th1 N2 K1 C24 84.4(2) . . . . ? C20 N2 K1 C28 -20.1(6) . . . . ? C17 N2 K1 C28 124.7(6) . . . . ? Th1 N2 K1 C28 53.0(2) . . . . ? C20 N2 K1 C10 -156.1(6) . . . . ? C17 N2 K1 C10 -11.2(5) . . . . ? Th1 N2 K1 C10 -83.0(2) . . . . ? C20 N2 K1 C8 -125.4(6) . . . . ? C17 N2 K1 C8 19.5(6) . . . . ? Th1 N2 K1 C8 -52.29(19) . . . . ? C20 N2 K1 C25 26.9(5) . . . . ? C17 N2 K1 C25 171.7(6) . . . . ? Th1 N2 K1 C25 99.9(2) . . . . ? C20 N2 K1 C33 89.4(6) . . . . ? C17 N2 K1 C33 -125.7(6) . . . . ? Th1 N2 K1 C33 162.5(3) . . . . ? C8 C9 K1 O1 -9.2(6) . . . . ? C10 C9 K1 O1 106.8(5) . . . . ? Th1 C9 K1 O1 -130.8(3) . . . . ? C8 C9 K1 O2 -112.2(6) . . . . ? C10 C9 K1 O2 3.8(6) . . . . ? Th1 C9 K1 O2 126.2(4) . . . . ? C8 C9 K1 N2 175.8(5) . . . . ? C10 C9 K1 N2 -68.2(5) . . . . ? Th1 C9 K1 N2 54.17(19) . . . . ? C8 C9 K1 C29 120.9(5) . . . . ? C10 C9 K1 C29 -123.2(5) . . . . ? Th1 C9 K1 C29 -0.8(2) . . . . ? C8 C9 K1 N1 67.1(5) . . . . ? C10 C9 K1 N1 -176.9(6) . . . . ? Th1 C9 K1 N1 -54.50(18) . . . . ? C8 C9 K1 C24 142.4(5) . . . . ? C10 C9 K1 C24 -101.7(5) . . . . ? Th1 C9 K1 C24 20.7(2) . . . . ? C8 C9 K1 C28 99.1(5) . . . . ? C10 C9 K1 C28 -145.0(5) . . . . ? Th1 C9 K1 C28 -22.6(2) . . . . ? C8 C9 K1 C10 -116.0(7) . . . . ? Th1 C9 K1 C10 122.4(5) . . . . ? C10 C9 K1 C8 116.0(7) . . . . ? Th1 C9 K1 C8 -121.6(5) . . . . ? C8 C9 K1 C25 144.3(5) . . . . ? C10 C9 K1 C25 -99.7(5) . . . . ? Th1 C9 K1 C25 22.7(3) . . . . ? C8 C9 K1 C33 -115.7(7) . . . . ? C10 C9 K1 C33 0.3(8) . . . . ? Th1 C9 K1 C33 122.7(5) . . . . ? C28 C29 K1 O1 6.7(6) . . . . ? C24 C29 K1 O1 -108.4(5) . . . . ? Th1 C29 K1 O1 128.3(3) . . . . ? C28 C29 K1 O2 112.6(5) . . . . ? C24 C29 K1 O2 -2.5(6) . . . . ? Th1 C29 K1 O2 -125.9(3) . . . . ? C28 C29 K1 N2 -176.0(6) . . . . ? C24 C29 K1 N2 68.9(5) . . . . ? Th1 C29 K1 N2 -54.48(18) . . . . ? C28 C29 K1 C9 -120.8(5) . . . . ? C24 C29 K1 C9 124.1(5) . . . . ? Th1 C29 K1 C9 0.8(2) . . . . ? C28 C29 K1 N1 -66.6(5) . . . . ? C24 C29 K1 N1 178.3(5) . . . . ? Th1 C29 K1 N1 54.92(18) . . . . ? C28 C29 K1 C24 115.1(7) . . . . ? Th1 C29 K1 C24 -123.3(5) . . . . ? C24 C29 K1 C28 -115.1(7) . . . . ? Th1 C29 K1 C28 121.6(5) . . . . ? C28 C29 K1 C10 -142.0(5) . . . . ? C24 C29 K1 C10 102.9(5) . . . . ? Th1 C29 K1 C10 -20.5(2) . . . . ? C28 C29 K1 C8 -99.5(5) . . . . ? C24 C29 K1 C8 145.4(5) . . . . ? Th1 C29 K1 C8 22.1(2) . . . . ? C28 C29 K1 C25 87.1(6) . . . . ? C24 C29 K1 C25 -28.1(5) . . . . ? Th1 C29 K1 C25 -151.4(4) . . . . ? C28 C29 K1 C33 93.4(5) . . . . ? C24 C29 K1 C33 -21.7(6) . . . . ? Th1 C29 K1 C33 -145.1(3) . . . . ? C1 N1 K1 O1 -112.0(6) . . . . ? C4 N1 K1 O1 108.4(6) . . . . ? Th1 N1 K1 O1 177.6(3) . . . . ? C1 N1 K1 O2 -106(24) . . . . ? C4 N1 K1 O2 114(24) . . . . ? Th1 N1 K1 O2 -176(100) . . . . ? C1 N1 K1 N2 69.7(6) . . . . ? C4 N1 K1 N2 -70.0(6) . . . . ? Th1 N1 K1 N2 -0.70(19) . . . . ? C1 N1 K1 C9 125.0(6) . . . . ? C4 N1 K1 C9 -14.7(5) . . . . ? Th1 N1 K1 C9 54.6(2) . . . . ? C1 N1 K1 C29 15.1(5) . . . . ? C4 N1 K1 C29 -124.5(6) . . . . ? Th1 N1 K1 C29 -55.3(2) . . . . ? C1 N1 K1 C24 15.9(6) . . . . ? C4 N1 K1 C24 -123.8(6) . . . . ? Th1 N1 K1 C24 -54.54(19) . . . . ? C1 N1 K1 C28 -14.2(5) . . . . ? C4 N1 K1 C28 -153.9(6) . . . . ? Th1 N1 K1 C28 -84.6(2) . . . . ? C1 N1 K1 C10 123.7(6) . . . . ? C4 N1 K1 C10 -16.0(6) . . . . ? Th1 N1 K1 C10 53.26(19) . . . . ? C1 N1 K1 C8 153.5(7) . . . . ? C4 N1 K1 C8 13.8(5) . . . . ? Th1 N1 K1 C8 83.1(2) . . . . ? C1 N1 K1 C25 -2.7(6) . . . . ? C4 N1 K1 C25 -142.4(6) . . . . ? Th1 N1 K1 C25 -73.1(2) . . . . ? C1 N1 K1 C33 -50.0(12) . . . . ? C4 N1 K1 C33 170.4(9) . . . . ? Th1 N1 K1 C33 -120.4(9) . . . . ? C25 C24 K1 O1 -35.3(6) . . . . ? C29 C24 K1 O1 90.3(5) . . . . ? C21 C24 K1 O1 -158.4(5) . . . . ? C25 C24 K1 O2 52.2(6) . . . . ? C29 C24 K1 O2 177.8(5) . . . . ? C21 C24 K1 O2 -70.9(6) . . . . ? C25 C24 K1 N2 139.8(6) . . . . ? C29 C24 K1 N2 -94.6(5) . . . . ? C21 C24 K1 N2 16.7(5) . . . . ? C25 C24 K1 C9 176.0(5) . . . . ? C29 C24 K1 C9 -58.3(5) . . . . ? C21 C24 K1 C9 52.9(6) . . . . ? C25 C24 K1 C29 -125.6(8) . . . . ? C21 C24 K1 C29 111.3(8) . . . . ? C25 C24 K1 N1 -127.1(5) . . . . ? C29 C24 K1 N1 -1.5(5) . . . . ? C21 C24 K1 N1 109.8(5) . . . . ? C25 C24 K1 C28 -90.9(6) . . . . ? C29 C24 K1 C28 34.7(5) . . . . ? C21 C24 K1 C28 146.0(7) . . . . ? C25 C24 K1 C10 150.4(5) . . . . ? C29 C24 K1 C10 -83.9(5) . . . . ? C21 C24 K1 C10 27.3(6) . . . . ? C25 C24 K1 C8 -166.6(5) . . . . ? C29 C24 K1 C8 -41.0(5) . . . . ? C21 C24 K1 C8 70.3(6) . . . . ? C29 C24 K1 C25 125.6(8) . . . . ? C21 C24 K1 C25 -123.1(8) . . . . ? C25 C24 K1 C33 34.1(6) . . . . ? C29 C24 K1 C33 159.7(5) . . . . ? C21 C24 K1 C33 -89.0(6) . . . . ? C27 C28 K1 O1 -47.5(6) . . . . ? C29 C28 K1 O1 -174.4(5) . . . . ? C30 C28 K1 O1 76.2(7) . . . . ? C27 C28 K1 O2 42.4(7) . . . . ? C29 C28 K1 O2 -84.4(6) . . . . ? C30 C28 K1 O2 166.2(6) . . . . ? C27 C28 K1 N2 130.3(6) . . . . ? C29 C28 K1 N2 3.4(5) . . . . ? C30 C28 K1 N2 -106.0(6) . . . . ? C27 C28 K1 C9 -171.7(6) . . . . ? C29 C28 K1 C9 61.4(5) . . . . ? C30 C28 K1 C9 -48.0(6) . . . . ? C27 C28 K1 C29 126.9(8) . . . . ? C30 C28 K1 C29 -109.4(8) . . . . ? C27 C28 K1 N1 -136.6(6) . . . . ? C29 C28 K1 N1 96.5(5) . . . . ? C30 C28 K1 N1 -12.9(5) . . . . ? C27 C28 K1 C24 91.4(6) . . . . ? C29 C28 K1 C24 -35.5(5) . . . . ? C30 C28 K1 C24 -144.9(8) . . . . ? C27 C28 K1 C10 171.8(5) . . . . ? C29 C28 K1 C10 44.9(5) . . . . ? C30 C28 K1 C10 -64.5(7) . . . . ? C27 C28 K1 C8 -146.7(6) . . . . ? C29 C28 K1 C8 86.4(5) . . . . ? C30 C28 K1 C8 -23.0(7) . . . . ? C27 C28 K1 C25 58.9(6) . . . . ? C29 C28 K1 C25 -68.0(5) . . . . ? C30 C28 K1 C25 -177.4(8) . . . . ? C27 C28 K1 C33 30.7(7) . . . . ? C29 C28 K1 C33 -96.1(6) . . . . ? C30 C28 K1 C33 154.5(6) . . . . ? C11 C10 K1 O1 33.0(6) . . . . ? C9 C10 K1 O1 -89.3(5) . . . . ? C14 C10 K1 O1 158.5(5) . . . . ? C11 C10 K1 O2 -54.4(6) . . . . ? C9 C10 K1 O2 -176.7(5) . . . . ? C14 C10 K1 O2 71.1(6) . . . . ? C11 C10 K1 N2 -141.9(6) . . . . ? C9 C10 K1 N2 95.8(5) . . . . ? C14 C10 K1 N2 -16.4(5) . . . . ? C11 C10 K1 C9 122.3(8) . . . . ? C14 C10 K1 C9 -112.2(8) . . . . ? C11 C10 K1 C29 -178.6(5) . . . . ? C9 C10 K1 C29 59.1(5) . . . . ? C14 C10 K1 C29 -53.0(5) . . . . ? C11 C10 K1 N1 125.0(5) . . . . ? C9 C10 K1 N1 2.7(5) . . . . ? C14 C10 K1 N1 -109.5(5) . . . . ? C11 C10 K1 C24 -152.5(5) . . . . ? C9 C10 K1 C24 85.2(5) . . . . ? C14 C10 K1 C24 -27.0(6) . . . . ? C11 C10 K1 C28 163.6(5) . . . . ? C9 C10 K1 C28 41.3(5) . . . . ? C14 C10 K1 C28 -70.9(6) . . . . ? C11 C10 K1 C8 88.1(6) . . . . ? C9 C10 K1 C8 -34.2(5) . . . . ? C14 C10 K1 C8 -146.4(7) . . . . ? C11 C10 K1 C25 -138.4(5) . . . . ? C9 C10 K1 C25 99.3(5) . . . . ? C14 C10 K1 C25 -12.9(6) . . . . ? C11 C10 K1 C33 -57.5(6) . . . . ? C9 C10 K1 C33 -179.8(5) . . . . ? C14 C10 K1 C33 68.0(6) . . . . ? C13 C8 K1 O1 48.4(6) . . . . ? C9 C8 K1 O1 172.1(5) . . . . ? C5 C8 K1 O1 -77.3(6) . . . . ? C13 C8 K1 O2 -39.5(7) . . . . ? C9 C8 K1 O2 84.2(6) . . . . ? C5 C8 K1 O2 -165.2(6) . . . . ? C13 C8 K1 N2 -127.3(6) . . . . ? C9 C8 K1 N2 -3.7(5) . . . . ? C5 C8 K1 N2 107.0(6) . . . . ? C13 C8 K1 C9 -123.7(8) . . . . ? C5 C8 K1 C9 110.6(8) . . . . ? C13 C8 K1 C29 175.1(6) . . . . ? C9 C8 K1 C29 -61.2(5) . . . . ? C5 C8 K1 C29 49.4(6) . . . . ? C13 C8 K1 N1 139.6(7) . . . . ? C9 C8 K1 N1 -96.8(5) . . . . ? C5 C8 K1 N1 13.9(5) . . . . ? C13 C8 K1 C24 -168.2(6) . . . . ? C9 C8 K1 C24 -44.5(5) . . . . ? C5 C8 K1 C24 66.1(7) . . . . ? C13 C8 K1 C28 149.6(6) . . . . ? C9 C8 K1 C28 -86.8(5) . . . . ? C5 C8 K1 C28 23.9(6) . . . . ? C13 C8 K1 C10 -88.8(6) . . . . ? C9 C8 K1 C10 34.9(4) . . . . ? C5 C8 K1 C10 145.5(7) . . . . ? C13 C8 K1 C25 -177.2(6) . . . . ? C9 C8 K1 C25 -53.6(7) . . . . ? C5 C8 K1 C25 57.1(8) . . . . ? C13 C8 K1 C33 -26.2(9) . . . . ? C9 C8 K1 C33 97.5(7) . . . . ? C5 C8 K1 C33 -151.9(7) . . . . ? C26 C25 K1 O1 24.9(7) . . . . ? C24 C25 K1 O1 151.4(5) . . . . ? C26 C25 K1 O2 106.1(7) . . . . ? C24 C25 K1 O2 -127.4(6) . . . . ? C26 C25 K1 N2 -159.6(7) . . . . ? C24 C25 K1 N2 -33.1(5) . . . . ? C26 C25 K1 C9 -131.3(6) . . . . ? C24 C25 K1 C9 -4.8(6) . . . . ? C26 C25 K1 C29 -95.7(7) . . . . ? C24 C25 K1 C29 30.8(5) . . . . ? C26 C25 K1 N1 -73.1(6) . . . . ? C24 C25 K1 N1 53.4(5) . . . . ? C26 C25 K1 C24 -126.5(9) . . . . ? C26 C25 K1 C28 -60.8(6) . . . . ? C24 C25 K1 C28 65.8(5) . . . . ? C26 C25 K1 C10 -162.6(6) . . . . ? C24 C25 K1 C10 -36.1(6) . . . . ? C26 C25 K1 C8 -106.7(7) . . . . ? C24 C25 K1 C8 19.8(8) . . . . ? C26 C25 K1 C33 90.7(7) . . . . ? C24 C25 K1 C33 -142.8(6) . . . . ? O2 C33 K1 O1 -113.0(12) . . . . ? C34 C33 K1 O1 -63.1(15) . . . . ? C34 C33 K1 O2 49.9(15) . . . . ? O2 C33 K1 N2 64.0(12) . . . . ? C34 C33 K1 N2 113.9(15) . . . . ? O2 C33 K1 C9 8.8(15) . . . . ? C34 C33 K1 C9 58.7(18) . . . . ? O2 C33 K1 C29 125.6(11) . . . . ? C34 C33 K1 C29 175.5(15) . . . . ? O2 C33 K1 N1 -178.1(9) . . . . ? C34 C33 K1 N1 -128.2(14) . . . . ? O2 C33 K1 C24 116.4(12) . . . . ? C34 C33 K1 C24 166.3(15) . . . . ? O2 C33 K1 C28 152.3(11) . . . . ? C34 C33 K1 C28 -157.8(15) . . . . ? O2 C33 K1 C10 8.9(13) . . . . ? C34 C33 K1 C10 58.8(16) . . . . ? O2 C33 K1 C8 -32.0(15) . . . . ? C34 C33 K1 C8 17.9(18) . . . . ? O2 C33 K1 C25 130.3(12) . . . . ? C34 C33 K1 C25 -179.8(16) . . . . ? C20 N2 Th1 C9 -174.1(5) . . . . ? C17 N2 Th1 C9 -65.9(5) . . . . ? K1 N2 Th1 C9 60.8(2) . . . . ? C20 N2 Th1 N1 124.2(5) . . . . ? C17 N2 Th1 N1 -127.6(5) . . . . ? K1 N2 Th1 N1 -0.9(2) . . . . ? C20 N2 Th1 C29 63.9(5) . . . . ? C17 N2 Th1 C29 172.2(5) . . . . ? K1 N2 Th1 C29 -61.2(2) . . . . ? C20 N2 Th1 C4 153.7(5) . . . . ? C17 N2 Th1 C4 -98.0(5) . . . . ? K1 N2 Th1 C4 28.6(3) . . . . ? C20 N2 Th1 C17 -108.3(7) . . . . ? K1 N2 Th1 C17 126.7(5) . . . . ? C20 N2 Th1 C1 94.7(5) . . . . ? C17 N2 Th1 C1 -157.0(5) . . . . ? K1 N2 Th1 C1 -30.3(3) . . . . ? C17 N2 Th1 C20 108.3(7) . . . . ? K1 N2 Th1 C20 -125.1(5) . . . . ? C20 N2 Th1 Cl1 -26.0(5) . . . . ? C17 N2 Th1 Cl1 82.3(5) . . . . ? K1 N2 Th1 Cl1 -151.06(9) . . . . ? C20 N2 Th1 C18 -73.2(5) . . . . ? C17 N2 Th1 C18 35.0(5) . . . . ? K1 N2 Th1 C18 161.7(4) . . . . ? C20 N2 Th1 C3 157.7(6) . . . . ? C17 N2 Th1 C3 -94.0(7) . . . . ? K1 N2 Th1 C3 32.7(6) . . . . ? C20 N2 Th1 C2 89.1(7) . . . . ? C17 N2 Th1 C2 -162.7(6) . . . . ? K1 N2 Th1 C2 -36.0(6) . . . . ? C8 C9 Th1 N2 -141.0(7) . . . . ? C10 C9 Th1 N2 20.7(6) . . . . ? K1 C9 Th1 N2 -59.29(19) . . . . ? C8 C9 Th1 N1 -19.7(6) . . . . ? C10 C9 Th1 N1 142.0(7) . . . . ? K1 C9 Th1 N1 61.96(19) . . . . ? C8 C9 Th1 C29 -80.7(7) . . . . ? C10 C9 Th1 C29 81.0(7) . . . . ? K1 C9 Th1 C29 1.0(3) . . . . ? C8 C9 Th1 C4 10.3(6) . . . . ? C10 C9 Th1 C4 172.0(7) . . . . ? K1 C9 Th1 C4 92.0(2) . . . . ? C8 C9 Th1 C17 -171.1(7) . . . . ? C10 C9 Th1 C17 -9.4(6) . . . . ? K1 C9 Th1 C17 -89.4(2) . . . . ? C8 C9 Th1 C1 -16.5(7) . . . . ? C10 C9 Th1 C1 145.2(6) . . . . ? K1 C9 Th1 C1 65.2(2) . . . . ? C8 C9 Th1 C20 -143.8(6) . . . . ? C10 C9 Th1 C20 17.8(7) . . . . ? K1 C9 Th1 C20 -62.2(2) . . . . ? C8 C9 Th1 Cl1 99.6(7) . . . . ? C10 C9 Th1 Cl1 -98.7(6) . . . . ? K1 C9 Th1 Cl1 -178.74(19) . . . . ? C8 C9 Th1 C18 172.1(7) . . . . ? C10 C9 Th1 C18 -26.3(6) . . . . ? K1 C9 Th1 C18 -106.3(2) . . . . ? C8 C9 Th1 C3 27.5(6) . . . . ? C10 C9 Th1 C3 -170.9(7) . . . . ? K1 C9 Th1 C3 109.1(2) . . . . ? C8 C9 Th1 C2 11.8(7) . . . . ? C10 C9 Th1 C2 173.5(6) . . . . ? K1 C9 Th1 C2 93.4(2) . . . . ? C1 N1 Th1 N2 -125.1(4) . . . . ? C4 N1 Th1 N2 126.3(4) . . . . ? K1 N1 Th1 N2 0.9(2) . . . . ? C1 N1 Th1 C9 173.5(5) . . . . ? C4 N1 Th1 C9 64.9(5) . . . . ? K1 N1 Th1 C9 -60.5(2) . . . . ? C1 N1 Th1 C29 -65.0(5) . . . . ? C4 N1 Th1 C29 -173.6(5) . . . . ? K1 N1 Th1 C29 61.0(2) . . . . ? C1 N1 Th1 C4 108.6(6) . . . . ? K1 N1 Th1 C4 -125.5(5) . . . . ? C1 N1 Th1 C17 -154.2(4) . . . . ? C4 N1 Th1 C17 97.2(5) . . . . ? K1 N1 Th1 C17 -28.3(3) . . . . ? C4 N1 Th1 C1 -108.6(6) . . . . ? K1 N1 Th1 C1 126.0(5) . . . . ? C1 N1 Th1 C20 -95.7(5) . . . . ? C4 N1 Th1 C20 155.7(4) . . . . ? K1 N1 Th1 C20 30.3(3) . . . . ? C1 N1 Th1 Cl1 25.2(5) . . . . ? C4 N1 Th1 Cl1 -83.3(4) . . . . ? K1 N1 Th1 Cl1 151.20(8) . . . . ? C1 N1 Th1 C18 -157.3(6) . . . . ? C4 N1 Th1 C18 94.1(7) . . . . ? K1 N1 Th1 C18 -31.3(6) . . . . ? C1 N1 Th1 C3 73.3(5) . . . . ? C4 N1 Th1 C3 -35.2(4) . . . . ? K1 N1 Th1 C3 -160.7(3) . . . . ? C1 N1 Th1 C2 35.2(4) . . . . ? C4 N1 Th1 C2 -73.4(5) . . . . ? K1 N1 Th1 C2 161.1(3) . . . . ? C28 C29 Th1 N2 138.5(7) . . . . ? C24 C29 Th1 N2 -15.7(6) . . . . ? K1 C29 Th1 N2 59.66(19) . . . . ? C28 C29 Th1 C9 77.9(7) . . . . ? C24 C29 Th1 C9 -76.3(7) . . . . ? K1 C29 Th1 C9 -1.0(3) . . . . ? C28 C29 Th1 N1 16.4(6) . . . . ? C24 C29 Th1 N1 -137.8(7) . . . . ? K1 C29 Th1 N1 -62.45(19) . . . . ? C28 C29 Th1 C4 13.2(7) . . . . ? C24 C29 Th1 C4 -141.0(7) . . . . ? K1 C29 Th1 C4 -65.6(2) . . . . ? C28 C29 Th1 C17 142.4(7) . . . . ? C24 C29 Th1 C17 -11.8(7) . . . . ? K1 C29 Th1 C17 63.5(2) . . . . ? C28 C29 Th1 C1 -13.5(6) . . . . ? C24 C29 Th1 C1 -167.7(8) . . . . ? K1 C29 Th1 C1 -92.4(2) . . . . ? C28 C29 Th1 C20 168.2(7) . . . . ? C24 C29 Th1 C20 14.0(6) . . . . ? K1 C29 Th1 C20 89.3(2) . . . . ? C28 C29 Th1 Cl1 -102.3(6) . . . . ? C24 C29 Th1 Cl1 103.6(6) . . . . ? K1 C29 Th1 Cl1 178.87(10) . . . . ? C28 C29 Th1 C18 170.5(6) . . . . ? C24 C29 Th1 C18 16.4(7) . . . . ? K1 C29 Th1 C18 91.7(2) . . . . ? C28 C29 Th1 C3 -14.9(7) . . . . ? C24 C29 Th1 C3 -169.1(6) . . . . ? K1 C29 Th1 C3 -93.8(2) . . . . ? C28 C29 Th1 C2 -30.7(7) . . . . ? C24 C29 Th1 C2 175.1(7) . . . . ? K1 C29 Th1 C2 -109.6(2) . . . . ? N1 C4 Th1 N2 -68.6(5) . . . . ? C3 C4 Th1 N2 176.4(5) . . . . ? C5 C4 Th1 N2 46.7(7) . . . . ? N1 C4 Th1 C9 -103.3(5) . . . . ? C3 C4 Th1 C9 141.6(6) . . . . ? C5 C4 Th1 C9 11.9(6) . . . . ? C3 C4 Th1 N1 -115.1(7) . . . . ? C5 C4 Th1 N1 115.3(8) . . . . ? N1 C4 Th1 C29 6.2(5) . . . . ? C3 C4 Th1 C29 -108.9(5) . . . . ? C5 C4 Th1 C29 121.5(6) . . . . ? N1 C4 Th1 C17 -104.9(5) . . . . ? C3 C4 Th1 C17 140.1(5) . . . . ? C5 C4 Th1 C17 10.4(7) . . . . ? N1 C4 Th1 C1 39.2(4) . . . . ? C3 C4 Th1 C1 -75.8(5) . . . . ? C5 C4 Th1 C1 154.5(7) . . . . ? N1 C4 Th1 C20 -42.8(7) . . . . ? C3 C4 Th1 C20 -157.8(5) . . . . ? C5 C4 Th1 C20 72.5(8) . . . . ? N1 C4 Th1 Cl1 111.2(4) . . . . ? C3 C4 Th1 Cl1 -3.9(5) . . . . ? C5 C4 Th1 Cl1 -133.6(6) . . . . ? N1 C4 Th1 C18 -135.3(4) . . . . ? C3 C4 Th1 C18 109.6(6) . . . . ? C5 C4 Th1 C18 -20.0(8) . . . . ? N1 C4 Th1 C3 115.1(7) . . . . ? C5 C4 Th1 C3 -129.7(9) . . . . ? N1 C4 Th1 C2 78.6(5) . . . . ? C3 C4 Th1 C2 -36.5(5) . . . . ? C5 C4 Th1 C2 -166.2(7) . . . . ? C18 C17 Th1 N2 115.5(8) . . . . ? C14 C17 Th1 N2 -112.9(8) . . . . ? N2 C17 Th1 C9 102.2(5) . . . . ? C18 C17 Th1 C9 -142.3(6) . . . . ? C14 C17 Th1 C9 -10.7(6) . . . . ? N2 C17 Th1 N1 67.2(6) . . . . ? C18 C17 Th1 N1 -177.3(5) . . . . ? C14 C17 Th1 N1 -45.6(7) . . . . ? N2 C17 Th1 C29 -7.5(5) . . . . ? C18 C17 Th1 C29 107.9(5) . . . . ? C14 C17 Th1 C29 -120.4(6) . . . . ? N2 C17 Th1 C4 103.8(5) . . . . ? C18 C17 Th1 C4 -140.7(5) . . . . ? C14 C17 Th1 C4 -9.1(7) . . . . ? N2 C17 Th1 C1 41.1(8) . . . . ? C18 C17 Th1 C1 156.6(5) . . . . ? C14 C17 Th1 C1 -71.7(8) . . . . ? N2 C17 Th1 C20 -39.3(5) . . . . ? C18 C17 Th1 C20 76.2(6) . . . . ? C14 C17 Th1 C20 -152.2(7) . . . . ? N2 C17 Th1 Cl1 -112.3(4) . . . . ? C18 C17 Th1 Cl1 3.2(6) . . . . ? C14 C17 Th1 Cl1 134.9(5) . . . . ? N2 C17 Th1 C18 -115.5(8) . . . . ? C14 C17 Th1 C18 131.7(9) . . . . ? N2 C17 Th1 C3 134.5(5) . . . . ? C18 C17 Th1 C3 -110.0(6) . . . . ? C14 C17 Th1 C3 21.6(8) . . . . ? N2 C17 Th1 C2 120.6(15) . . . . ? C18 C17 Th1 C2 -123.9(16) . . . . ? C14 C17 Th1 C2 7.7(19) . . . . ? N1 C1 Th1 N2 69.6(5) . . . . ? C2 C1 Th1 N2 -174.8(5) . . . . ? C30 C1 Th1 N2 -45.0(7) . . . . ? N1 C1 Th1 C9 -6.3(5) . . . . ? C2 C1 Th1 C9 109.3(5) . . . . ? C30 C1 Th1 C9 -120.8(6) . . . . ? C2 C1 Th1 N1 115.6(7) . . . . ? C30 C1 Th1 N1 -114.5(8) . . . . ? N1 C1 Th1 C29 102.9(5) . . . . ? C2 C1 Th1 C29 -141.4(6) . . . . ? C30 C1 Th1 C29 -11.6(6) . . . . ? N1 C1 Th1 C4 -39.7(4) . . . . ? C2 C1 Th1 C4 75.9(6) . . . . ? C30 C1 Th1 C4 -154.2(7) . . . . ? N1 C1 Th1 C17 46.1(8) . . . . ? C2 C1 Th1 C17 161.8(6) . . . . ? C30 C1 Th1 C17 -68.4(9) . . . . ? N1 C1 Th1 C20 104.7(5) . . . . ? C2 C1 Th1 C20 -139.7(5) . . . . ? C30 C1 Th1 C20 -9.8(7) . . . . ? N1 C1 Th1 Cl1 -158.3(4) . . . . ? C2 C1 Th1 Cl1 -42.7(5) . . . . ? C30 C1 Th1 Cl1 87.2(6) . . . . ? N1 C1 Th1 C18 123.3(11) . . . . ? C2 C1 Th1 C18 -121.1(12) . . . . ? C30 C1 Th1 C18 8.8(16) . . . . ? N1 C1 Th1 C3 -78.9(5) . . . . ? C2 C1 Th1 C3 36.7(5) . . . . ? C30 C1 Th1 C3 166.5(8) . . . . ? N1 C1 Th1 C2 -115.6(7) . . . . ? C30 C1 Th1 C2 129.9(9) . . . . ? C19 C20 Th1 N2 -116.4(8) . . . . ? C21 C20 Th1 N2 113.6(8) . . . . ? N2 C20 Th1 C9 5.7(5) . . . . ? C19 C20 Th1 C9 -110.7(5) . . . . ? C21 C20 Th1 C9 119.3(6) . . . . ? N2 C20 Th1 N1 -70.4(5) . . . . ? C19 C20 Th1 N1 173.3(5) . . . . ? C21 C20 Th1 N1 43.2(7) . . . . ? N2 C20 Th1 C29 -103.9(5) . . . . ? C19 C20 Th1 C29 139.7(6) . . . . ? C21 C20 Th1 C29 9.7(6) . . . . ? N2 C20 Th1 C4 -46.2(8) . . . . ? C19 C20 Th1 C4 -162.5(5) . . . . ? C21 C20 Th1 C4 67.4(8) . . . . ? N2 C20 Th1 C17 39.9(5) . . . . ? C19 C20 Th1 C17 -76.5(6) . . . . ? C21 C20 Th1 C17 153.5(8) . . . . ? N2 C20 Th1 C1 -105.7(5) . . . . ? C19 C20 Th1 C1 138.0(5) . . . . ? C21 C20 Th1 C1 8.0(7) . . . . ? N2 C20 Th1 Cl1 157.8(4) . . . . ? C19 C20 Th1 Cl1 41.4(5) . . . . ? C21 C20 Th1 Cl1 -88.6(6) . . . . ? N2 C20 Th1 C18 79.2(5) . . . . ? C19 C20 Th1 C18 -37.1(5) . . . . ? C21 C20 Th1 C18 -167.2(8) . . . . ? N2 C20 Th1 C3 -119.9(12) . . . . ? C19 C20 Th1 C3 123.7(12) . . . . ? C21 C20 Th1 C3 -6.3(16) . . . . ? N2 C20 Th1 C2 -135.3(5) . . . . ? C19 C20 Th1 C2 108.3(6) . . . . ? C21 C20 Th1 C2 -21.7(8) . . . . ? C17 C18 Th1 N2 -36.4(5) . . . . ? C19 C18 Th1 N2 76.7(5) . . . . ? C17 C18 Th1 C9 33.0(5) . . . . ? C19 C18 Th1 C9 146.1(5) . . . . ? C17 C18 Th1 N1 5.2(9) . . . . ? C19 C18 Th1 N1 118.3(6) . . . . ? C17 C18 Th1 C29 -79.0(6) . . . . ? C19 C18 Th1 C29 34.2(5) . . . . ? C17 C18 Th1 C4 61.1(7) . . . . ? C19 C18 Th1 C4 174.3(4) . . . . ? C19 C18 Th1 C17 113.1(7) . . . . ? C17 C18 Th1 C1 -97.8(13) . . . . ? C19 C18 Th1 C1 15.3(14) . . . . ? C17 C18 Th1 C20 -76.1(5) . . . . ? C19 C18 Th1 C20 37.0(4) . . . . ? C17 C18 Th1 Cl1 -177.0(5) . . . . ? C19 C18 Th1 Cl1 -63.9(4) . . . . ? C17 C18 Th1 C3 109.8(6) . . . . ? C19 C18 Th1 C3 -137.1(5) . . . . ? C17 C18 Th1 C2 162.3(6) . . . . ? C19 C18 Th1 C2 -84.5(7) . . . . ? C4 C3 Th1 N2 -6.8(9) . . . . ? C2 C3 Th1 N2 -120.5(6) . . . . ? C4 C3 Th1 C9 -33.6(5) . . . . ? C2 C3 Th1 C9 -147.2(5) . . . . ? C4 C3 Th1 N1 36.7(5) . . . . ? C2 C3 Th1 N1 -76.9(5) . . . . ? C4 C3 Th1 C29 78.4(5) . . . . ? C2 C3 Th1 C29 -35.2(5) . . . . ? C2 C3 Th1 C4 -113.6(7) . . . . ? C4 C3 Th1 C17 -62.0(7) . . . . ? C2 C3 Th1 C17 -175.6(5) . . . . ? C4 C3 Th1 C1 76.7(5) . . . . ? C2 C3 Th1 C1 -37.0(5) . . . . ? C4 C3 Th1 C20 93.2(13) . . . . ? C2 C3 Th1 C20 -20.4(15) . . . . ? C4 C3 Th1 Cl1 176.4(5) . . . . ? C2 C3 Th1 Cl1 62.8(5) . . . . ? C4 C3 Th1 C18 -110.4(6) . . . . ? C2 C3 Th1 C18 136.0(5) . . . . ? C4 C3 Th1 C2 113.6(7) . . . . ? C1 C2 Th1 N2 9.7(9) . . . . ? C3 C2 Th1 N2 122.8(6) . . . . ? C1 C2 Th1 C9 -78.3(6) . . . . ? C3 C2 Th1 C9 34.9(5) . . . . ? C1 C2 Th1 N1 -36.2(5) . . . . ? C3 C2 Th1 N1 77.0(5) . . . . ? C1 C2 Th1 C29 33.5(5) . . . . ? C3 C2 Th1 C29 146.7(5) . . . . ? C1 C2 Th1 C4 -76.5(5) . . . . ? C3 C2 Th1 C4 36.7(5) . . . . ? C1 C2 Th1 C17 -95.5(16) . . . . ? C3 C2 Th1 C17 17.6(18) . . . . ? C3 C2 Th1 C1 113.2(7) . . . . ? C1 C2 Th1 C20 60.8(7) . . . . ? C3 C2 Th1 C20 174.0(5) . . . . ? C1 C2 Th1 Cl1 134.8(5) . . . . ? C3 C2 Th1 Cl1 -112.0(5) . . . . ? C1 C2 Th1 C18 156.4(6) . . . . ? C3 C2 Th1 C18 -90.4(8) . . . . ? C1 C2 Th1 C3 -113.2(7) . . . . ? C39 C40 O1 C37 -15.4(19) . . . . ? K1 C40 O1 C37 -149.0(15) . . . . ? C39 C40 O1 K1 133.6(13) . . . . ? C38 C37 O1 C40 22.1(18) . . . . ? C38 C37 O1 K1 -126.0(12) . . . . ? O2 K1 O1 C40 47.8(11) . . . . ? N2 K1 O1 C40 25(5) . . . . ? C9 K1 O1 C40 -75.1(11) . . . . ? C29 K1 O1 C40 172.3(10) . . . . ? N1 K1 O1 C40 -132.2(11) . . . . ? C24 K1 O1 C40 141.0(10) . . . . ? C28 K1 O1 C40 175.1(11) . . . . ? C10 K1 O1 C40 -45.7(12) . . . . ? C8 K1 O1 C40 -78.9(11) . . . . ? C25 K1 O1 C40 127.1(11) . . . . ? C33 K1 O1 C40 66.5(11) . . . . ? O2 K1 O1 C37 -168.5(12) . . . . ? N2 K1 O1 C37 169(3) . . . . ? C9 K1 O1 C37 68.6(12) . . . . ? C29 K1 O1 C37 -44.0(13) . . . . ? N1 K1 O1 C37 11.5(12) . . . . ? C24 K1 O1 C37 -75.3(12) . . . . ? C28 K1 O1 C37 -41.2(12) . . . . ? C10 K1 O1 C37 98.0(12) . . . . ? C8 K1 O1 C37 64.8(12) . . . . ? C25 K1 O1 C37 -89.2(12) . . . . ? C33 K1 O1 C37 -149.8(12) . . . . ? C34 C33 O2 C36 31.3(18) . . . . ? K1 C33 O2 C36 179.1(17) . . . . ? C34 C33 O2 K1 -147.8(11) . . . . ? C35 C36 O2 C33 -35.5(19) . . . . ? C35 C36 O2 K1 143.3(13) . . . . ? O1 K1 O2 C33 63.8(12) . . . . ? N2 K1 O2 C33 -117.9(12) . . . . ? C9 K1 O2 C33 -173.6(11) . . . . ? C29 K1 O2 C33 -62.9(12) . . . . ? N1 K1 O2 C33 58(25) . . . . ? C24 K1 O2 C33 -64.0(12) . . . . ? C28 K1 O2 C33 -33.4(13) . . . . ? C10 K1 O2 C33 -172.0(12) . . . . ? C8 K1 O2 C33 157.7(11) . . . . ? C25 K1 O2 C33 -45.6(12) . . . . ? O1 K1 O2 C36 -115.0(16) . . . . ? N2 K1 O2 C36 63.3(15) . . . . ? C9 K1 O2 C36 7.7(17) . . . . ? C29 K1 O2 C36 118.3(15) . . . . ? N1 K1 O2 C36 -121(24) . . . . ? C24 K1 O2 C36 117.2(15) . . . . ? C28 K1 O2 C36 147.8(15) . . . . ? C10 K1 O2 C36 9.3(16) . . . . ? C8 K1 O2 C36 -21.1(17) . . . . ? C25 K1 O2 C36 135.6(16) . . . . ? C33 K1 O2 C36 -179(2) . . . . ? N2 Th1 Cl1 Th1 -105.98(19) . . . 3_655 ? C9 Th1 Cl1 Th1 0.0(3) . . . 3_655 ? N1 Th1 Cl1 Th1 106.17(18) . . . 3_655 ? C29 Th1 Cl1 Th1 -179.72(17) . . . 3_655 ? C4 Th1 Cl1 Th1 74.28(19) . . . 3_655 ? C17 Th1 Cl1 Th1 -74.3(2) . . . 3_655 ? C1 Th1 Cl1 Th1 118.14(18) . . . 3_655 ? C20 Th1 Cl1 Th1 -118.23(19) . . . 3_655 ? C18 Th1 Cl1 Th1 -72.77(19) . . . 3_655 ? C3 Th1 Cl1 Th1 72.43(19) . . . 3_655 ? C2 Th1 Cl1 Th1 98.5(2) . . . 3_655 ? C41 C42 C43 C43 -169(5) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 5.089 _refine_diff_density_min -1.862 _refine_diff_density_rms 0.179 _database_code_depnum_ccdc_archive 'CCDC 951386' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po3003_refinalized _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H52 K N3 Si2 Th' _chemical_formula_weight 878.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.232(5) _cell_length_b 12.893(5) _cell_length_c 23.252(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3667(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15916 _cell_measurement_theta_min 3.7730 _cell_measurement_theta_max 73.5010 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1305 _exptl_crystal_size_mid 0.1069 _exptl_crystal_size_min 0.0426 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 14.978 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28994 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 73.45 _reflns_number_total 7189 _reflns_number_gt 6871 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_structure_solution sir-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material MERCURY _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+66.3051P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.055(14) _refine_ls_number_reflns 7189 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1628 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.006 _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 0.2600(9) -0.0045(12) 0.2372(4) 0.021(2) Uani 1 1 d . . . C2 C 0.3411(12) -0.0660(11) 0.2617(6) 0.028(3) Uani 1 1 d . . . H2 H 0.3508 -0.1386 0.2568 0.034 Uiso 1 1 calc R . . C3 C 0.4060(9) 0.0011(13) 0.2954(5) 0.024(2) Uani 1 1 d . . . H3 H 0.4688 -0.0174 0.3171 0.028 Uiso 1 1 calc R . . C4 C 0.3601(11) 0.0994(10) 0.2907(6) 0.024(3) Uani 1 1 d . . . C5 C 0.4078(11) 0.2006(11) 0.3093(6) 0.028(3) Uani 1 1 d . . . C6 C 0.5263(12) 0.1847(11) 0.3288(7) 0.034(3) Uani 1 1 d . . . H6A H 0.5273 0.1443 0.3645 0.051 Uiso 1 1 calc R . . H6B H 0.5607 0.2522 0.3354 0.051 Uiso 1 1 calc R . . H6C H 0.5666 0.1472 0.2989 0.051 Uiso 1 1 calc R . . C7 C 0.4066(12) 0.2735(11) 0.2569(6) 0.034(3) Uani 1 1 d . . . H7A H 0.4439 0.2399 0.2246 0.050 Uiso 1 1 calc R . . H7B H 0.4444 0.3382 0.2666 0.050 Uiso 1 1 calc R . . H7C H 0.3309 0.2888 0.2461 0.050 Uiso 1 1 calc R . . C8 C 0.3425(10) 0.2490(9) 0.3591(6) 0.024(3) Uani 1 1 d . . . C9 C 0.2549(11) 0.1927(12) 0.3853(6) 0.027(3) Uani 1 1 d . . . C10 C 0.2068(11) 0.2451(10) 0.4329(6) 0.027(3) Uani 1 1 d . . . C11 C 0.2423(13) 0.3418(11) 0.4516(7) 0.034(3) Uani 1 1 d . . . H11 H 0.2064 0.3740 0.4832 0.041 Uiso 1 1 calc R . . C12 C 0.3283(13) 0.3918(11) 0.4256(7) 0.036(3) Uani 1 1 d . . . H12 H 0.3527 0.4572 0.4393 0.044 Uiso 1 1 calc R . . C13 C 0.3781(12) 0.3454(11) 0.3793(6) 0.031(3) Uani 1 1 d . . . H13 H 0.4375 0.3793 0.3607 0.037 Uiso 1 1 calc R . . C14 C 0.1173(12) 0.1941(10) 0.4684(6) 0.029(3) Uani 1 1 d . . . C15 C 0.1577(14) 0.1739(12) 0.5299(6) 0.036(3) Uani 1 1 d . . . H15A H 0.1013 0.1364 0.5514 0.053 Uiso 1 1 calc R . . H15B H 0.1730 0.2401 0.5489 0.053 Uiso 1 1 calc R . . H15C H 0.2246 0.1321 0.5285 0.053 Uiso 1 1 calc R . . C16 C 0.0143(13) 0.2644(11) 0.4725(7) 0.037(3) Uani 1 1 d . . . H16A H -0.0148 0.2766 0.4338 0.056 Uiso 1 1 calc R . . H16B H 0.0342 0.3308 0.4901 0.056 Uiso 1 1 calc R . . H16C H -0.0413 0.2300 0.4961 0.056 Uiso 1 1 calc R . . C17 C 0.0815(12) 0.0930(10) 0.4421(6) 0.026(3) Uani 1 1 d . . . C18 C 0.0899(9) -0.0067(11) 0.4632(5) 0.022(2) Uani 1 1 d . . . H18 H 0.1327 -0.0279 0.4952 0.026 Uiso 1 1 calc R . . C19 C 0.0240(12) -0.0715(10) 0.4291(6) 0.026(3) Uani 1 1 d . . . H19 H 0.0134 -0.1441 0.4332 0.032 Uiso 1 1 calc R . . C20 C -0.0226(9) -0.0061(12) 0.3878(5) 0.022(2) Uani 1 1 d . . . C21 C -0.1149(10) -0.0309(10) 0.3463(6) 0.027(3) Uani 1 1 d . . . C22 C -0.2055(12) 0.0507(14) 0.3569(7) 0.039(3) Uani 1 1 d . . . H22A H -0.2235 0.0527 0.3979 0.059 Uiso 1 1 calc R . . H22B H -0.2708 0.0321 0.3348 0.059 Uiso 1 1 calc R . . H22C H -0.1794 0.1191 0.3446 0.059 Uiso 1 1 calc R . . C23 C -0.1639(13) -0.1380(13) 0.3598(7) 0.043(4) Uani 1 1 d . . . H23A H -0.1088 -0.1918 0.3529 0.064 Uiso 1 1 calc R . . H23B H -0.2273 -0.1503 0.3349 0.064 Uiso 1 1 calc R . . H23C H -0.1869 -0.1402 0.4002 0.064 Uiso 1 1 calc R . . C24 C -0.0755(11) -0.0285(9) 0.2842(5) 0.024(3) Uani 1 1 d . . . C25 C -0.1548(13) -0.0404(10) 0.2420(7) 0.035(3) Uani 1 1 d . . . H25 H -0.2296 -0.0440 0.2529 0.042 Uiso 1 1 calc R . . C26 C -0.1268(13) -0.0470(11) 0.1841(7) 0.035(3) Uani 1 1 d . . . H26 H -0.1815 -0.0543 0.1553 0.042 Uiso 1 1 calc R . . C27 C -0.0183(13) -0.0429(11) 0.1695(7) 0.033(3) Uani 1 1 d . . . H27 H 0.0020 -0.0495 0.1303 0.040 Uiso 1 1 calc R . . C28 C 0.0633(12) -0.0291(9) 0.2110(6) 0.026(3) Uani 1 1 d . . . C29 C 0.0396(10) -0.0209(10) 0.2705(5) 0.025(3) Uani 1 1 d . . . C30 C 0.1813(11) -0.0318(10) 0.1894(5) 0.026(3) Uani 1 1 d . . . C31 C 0.1996(14) 0.0478(13) 0.1408(6) 0.038(3) Uani 1 1 d . . . H31A H 0.1825 0.1175 0.1550 0.057 Uiso 1 1 calc R . . H31B H 0.1519 0.0312 0.1082 0.057 Uiso 1 1 calc R . . H31C H 0.2761 0.0453 0.1283 0.057 Uiso 1 1 calc R . . C32 C 0.2082(14) -0.1398(13) 0.1661(7) 0.041(4) Uani 1 1 d . . . H32A H 0.2841 -0.1412 0.1526 0.062 Uiso 1 1 calc R . . H32B H 0.1591 -0.1561 0.1340 0.062 Uiso 1 1 calc R . . H32C H 0.1986 -0.1912 0.1967 0.062 Uiso 1 1 calc R . . C33 C 0.3469(13) -0.3537(11) 0.3428(8) 0.041(4) Uani 1 1 d . . . H33A H 0.3787 -0.3191 0.3092 0.062 Uiso 1 1 calc R . . H33B H 0.3179 -0.4215 0.3314 0.062 Uiso 1 1 calc R . . H33C H 0.4034 -0.3632 0.3722 0.062 Uiso 1 1 calc R . . C34 C 0.1714(14) -0.3458(12) 0.4337(7) 0.037(3) Uani 1 1 d . . . H34A H 0.2290 -0.3672 0.4605 0.056 Uiso 1 1 calc R . . H34B H 0.1339 -0.4074 0.4188 0.056 Uiso 1 1 calc R . . H34C H 0.1187 -0.3015 0.4538 0.056 Uiso 1 1 calc R . . C35 C 0.1257(14) -0.2639(11) 0.3163(7) 0.038(3) Uani 1 1 d . . . H35A H 0.0720 -0.2109 0.3271 0.057 Uiso 1 1 calc R . . H35B H 0.0891 -0.3312 0.3127 0.057 Uiso 1 1 calc R . . H35C H 0.1592 -0.2451 0.2794 0.057 Uiso 1 1 calc R . . C36 C 0.4021(11) 0.0035(13) 0.4577(5) 0.034(3) Uani 1 1 d . . . H36A H 0.4174 0.0430 0.4226 0.051 Uiso 1 1 calc R . . H36B H 0.4636 0.0105 0.4844 0.051 Uiso 1 1 calc R . . H36C H 0.3355 0.0304 0.4758 0.051 Uiso 1 1 calc R . . C37 C 0.3567(15) -0.2031(13) 0.5090(7) 0.042(4) Uani 1 1 d . . . H37A H 0.2858 -0.1811 0.5245 0.063 Uiso 1 1 calc R . . H37B H 0.4146 -0.1853 0.5364 0.063 Uiso 1 1 calc R . . H37C H 0.3561 -0.2782 0.5028 0.063 Uiso 1 1 calc R . . C38 C 0.5200(14) -0.1818(15) 0.4127(8) 0.048(4) Uani 1 1 d . . . H38A H 0.5219 -0.2578 0.4132 0.072 Uiso 1 1 calc R . . H38B H 0.5776 -0.1546 0.4378 0.072 Uiso 1 1 calc R . . H38C H 0.5317 -0.1570 0.3734 0.072 Uiso 1 1 calc R . . N1 N 0.2670(9) 0.0961(8) 0.2573(5) 0.025(2) Uani 1 1 d . . . N2 N 0.0150(9) 0.0933(8) 0.3934(5) 0.024(2) Uani 1 1 d . . . N3 N 0.2766(11) -0.1500(10) 0.3909(5) 0.029(3) Uani 1 1 d . . . Si1 Si 0.3825(3) -0.1357(3) 0.43930(16) 0.0255(7) Uani 1 1 d . . . Si2 Si 0.2335(3) -0.2721(3) 0.37267(15) 0.0230(7) Uani 1 1 d . . . Th01 Th 0.19438(3) 0.00130(3) 0.351935(13) 0.01631(13) Uani 1 1 d . . . K1 K 0.0657(3) 0.2276(2) 0.28608(14) 0.0338(7) 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 0.024(5) 0.020(5) 0.020(5) -0.001(6) 0.007(4) -0.001(6) C2 0.030(7) 0.029(7) 0.027(7) -0.002(6) 0.007(6) 0.009(6) C3 0.018(5) 0.025(5) 0.028(5) 0.004(7) 0.004(4) 0.004(7) C4 0.022(6) 0.026(6) 0.026(6) 0.006(5) 0.001(5) 0.002(5) C5 0.022(7) 0.032(7) 0.031(7) 0.004(5) 0.002(6) -0.004(5) C6 0.022(7) 0.033(7) 0.046(8) 0.001(6) -0.006(6) -0.003(6) C7 0.033(8) 0.028(6) 0.039(7) 0.004(6) 0.002(6) -0.006(6) C8 0.017(6) 0.022(6) 0.034(7) 0.002(5) -0.006(5) -0.004(5) C9 0.024(7) 0.042(8) 0.016(6) 0.005(6) 0.000(5) 0.001(6) C10 0.026(7) 0.024(6) 0.031(7) 0.001(5) -0.001(6) 0.004(5) C11 0.039(8) 0.028(7) 0.034(8) -0.003(6) -0.012(6) 0.007(6) C12 0.043(9) 0.020(6) 0.046(8) 0.003(6) -0.010(7) -0.003(6) C13 0.030(7) 0.030(7) 0.034(7) 0.013(6) -0.009(6) -0.003(6) C14 0.038(8) 0.027(6) 0.021(6) -0.004(5) 0.008(6) 0.004(6) C15 0.046(9) 0.039(8) 0.021(6) -0.003(6) -0.002(6) 0.004(7) C16 0.043(9) 0.024(7) 0.044(8) -0.013(6) 0.011(7) 0.007(6) C17 0.026(7) 0.023(6) 0.028(6) 0.004(5) 0.006(6) 0.003(5) C18 0.026(5) 0.016(5) 0.024(5) 0.000(6) 0.005(4) 0.003(6) C19 0.029(7) 0.021(6) 0.028(7) -0.001(5) 0.013(6) -0.007(5) C20 0.021(5) 0.022(5) 0.023(5) -0.001(6) 0.004(4) -0.001(6) C21 0.016(6) 0.032(7) 0.034(7) 0.007(5) -0.002(5) 0.000(5) C22 0.026(7) 0.058(9) 0.035(7) 0.000(7) 0.003(6) 0.008(7) C23 0.034(8) 0.046(9) 0.049(9) 0.008(7) -0.009(7) -0.014(7) C24 0.026(6) 0.019(6) 0.027(6) 0.001(4) -0.004(5) 0.000(4) C25 0.033(8) 0.020(6) 0.050(9) 0.002(6) -0.007(7) -0.001(5) C26 0.037(8) 0.025(6) 0.042(8) -0.003(6) -0.012(7) -0.002(6) C27 0.041(8) 0.024(6) 0.035(7) -0.005(6) -0.008(6) -0.003(6) C28 0.032(7) 0.015(6) 0.030(6) 0.000(4) -0.006(6) 0.002(4) C29 0.019(6) 0.031(9) 0.026(6) 0.004(5) 0.000(4) 0.000(5) C30 0.028(7) 0.030(7) 0.020(6) -0.004(5) 0.000(5) 0.005(5) C31 0.049(9) 0.046(8) 0.020(6) -0.002(6) -0.003(6) -0.001(7) C32 0.043(9) 0.047(9) 0.034(8) -0.013(7) 0.002(7) 0.010(7) C33 0.038(9) 0.023(7) 0.063(11) -0.004(7) 0.018(8) -0.003(6) C34 0.039(9) 0.033(7) 0.039(8) -0.001(6) 0.004(7) -0.008(6) C35 0.053(10) 0.021(6) 0.041(8) 0.002(6) -0.007(7) -0.004(7) C36 0.042(7) 0.022(5) 0.038(6) 0.000(7) -0.016(5) -0.001(8) C37 0.052(10) 0.040(8) 0.034(8) 0.010(7) -0.012(7) 0.000(7) C38 0.038(9) 0.062(11) 0.044(9) -0.016(8) -0.009(7) 0.018(8) N1 0.023(6) 0.027(5) 0.025(5) 0.002(4) -0.001(4) 0.002(4) N2 0.025(6) 0.018(5) 0.029(6) 0.004(4) -0.002(5) 0.002(4) N3 0.032(6) 0.033(6) 0.023(5) 0.003(5) -0.003(5) 0.010(5) Si1 0.0288(18) 0.0215(16) 0.0261(16) 0.0002(13) -0.0035(15) 0.0043(13) Si2 0.0265(17) 0.0154(14) 0.0270(17) 0.0019(13) -0.0005(14) 0.0006(13) Th01 0.01680(19) 0.01547(18) 0.01665(18) 0.0011(2) -0.00069(12) 0.0012(2) K1 0.0380(17) 0.0223(13) 0.0410(16) 0.0033(12) -0.0073(14) 0.0034(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.382(18) . ? C1 C2 1.392(19) . ? C1 C30 1.512(17) . ? C1 Th01 2.788(10) . ? C2 C3 1.41(2) . ? C2 Th01 2.894(13) . ? C2 H2 0.9500 . ? C3 C4 1.390(19) . ? C3 Th01 2.903(10) . ? C3 H3 0.9500 . ? C4 N1 1.379(17) . ? C4 C5 1.493(19) . ? C4 Th01 2.781(13) . ? C5 C6 1.532(19) . ? C5 C8 1.538(19) . ? C5 C7 1.541(19) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.398(19) . ? C8 C9 1.430(19) . ? C9 C10 1.425(19) . ? C9 Th01 2.691(16) . ? C9 K1 3.298(14) . ? C10 C11 1.390(19) . ? C10 C14 1.520(19) . ? C11 C12 1.37(2) . ? C11 H11 0.9500 . ? C12 C13 1.38(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.505(19) . ? C14 C15 1.534(19) . ? C14 C16 1.554(19) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.380(18) . ? C17 N2 1.394(17) . ? C17 Th01 2.776(13) . ? C18 C19 1.406(19) . ? C18 Th01 2.888(10) . ? C18 H18 0.9500 . ? C19 C20 1.400(19) . ? C19 Th01 2.906(12) . ? C19 H19 0.9500 . ? C20 N2 1.368(18) . ? C20 C21 1.519(17) . ? C20 Th01 2.783(11) . ? C21 C24 1.522(18) . ? C21 C23 1.538(19) . ? C21 C22 1.55(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.388(19) . ? C24 C29 1.447(18) . ? C25 C26 1.39(2) . ? C25 K1 3.251(14) 4_545 ? C25 H25 0.9500 . ? C26 C27 1.37(2) . ? C26 K1 3.079(15) 4_545 ? C26 H26 0.9500 . ? C27 C28 1.400(19) . ? C27 K1 3.188(15) 4_545 ? C27 H27 0.9500 . ? C28 C29 1.417(18) . ? C28 C30 1.530(19) . ? C28 K1 3.512(12) 4_545 ? C29 Th01 2.693(12) . ? C29 K1 3.239(13) . ? C30 C32 1.529(19) . ? C30 C31 1.542(19) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Si2 1.875(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 Si2 1.869(15) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 Si2 1.863(16) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 Si1 1.861(16) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 Si1 1.866(16) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Si1 1.888(17) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? N1 Th01 2.669(11) . ? N1 K1 3.064(11) . ? N2 Th01 2.675(11) . ? N2 K1 3.100(11) . ? N3 Si2 1.713(13) . ? N3 Si1 1.726(12) . ? N3 Th01 2.375(12) . ? K1 C26 3.079(15) 4 ? K1 C27 3.188(15) 4 ? K1 C25 3.251(14) 4 ? K1 C35 3.340(16) 4 ? K1 C28 3.512(12) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.6(11) . . ? N1 C1 C30 120.5(11) . . ? C2 C1 C30 128.5(13) . . ? N1 C1 Th01 70.6(6) . . ? C2 C1 Th01 80.1(7) . . ? C30 C1 Th01 121.8(7) . . ? C1 C2 C3 106.2(12) . . ? C1 C2 Th01 71.6(7) . . ? C3 C2 Th01 76.2(7) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? Th01 C2 H2 117.4 . . ? C4 C3 C2 106.8(11) . . ? C4 C3 Th01 71.0(7) . . ? C2 C3 Th01 75.6(7) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? Th01 C3 H3 118.8 . . ? N1 C4 C3 110.5(12) . . ? N1 C4 C5 120.8(11) . . ? C3 C4 C5 128.1(12) . . ? N1 C4 Th01 70.9(7) . . ? C3 C4 Th01 80.8(7) . . ? C5 C4 Th01 122.2(9) . . ? C4 C5 C6 109.7(12) . . ? C4 C5 C8 111.7(11) . . ? C6 C5 C8 108.9(12) . . ? C4 C5 C7 107.5(11) . . ? C6 C5 C7 108.9(11) . . ? C8 C5 C7 110.1(11) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 122.9(13) . . ? C13 C8 C5 116.8(12) . . ? C9 C8 C5 120.2(12) . . ? C8 C9 C10 113.6(13) . . ? C8 C9 Th01 123.3(10) . . ? C10 C9 Th01 123.0(10) . . ? C8 C9 K1 99.2(8) . . ? C10 C9 K1 100.9(9) . . ? Th01 C9 K1 74.4(3) . . ? C11 C10 C9 122.6(13) . . ? C11 C10 C14 116.3(12) . . ? C9 C10 C14 121.0(12) . . ? C12 C11 C10 121.5(14) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.7(13) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C8 120.7(13) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? C17 C14 C10 111.3(10) . . ? C17 C14 C15 109.0(11) . . ? C10 C14 C15 110.3(12) . . ? C17 C14 C16 107.1(12) . . ? C10 C14 C16 111.4(11) . . ? C15 C14 C16 107.7(11) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 109.6(11) . . ? C18 C17 C14 129.9(12) . . ? N2 C17 C14 119.8(11) . . ? C18 C17 Th01 80.5(7) . . ? N2 C17 Th01 71.2(7) . . ? C14 C17 Th01 122.1(9) . . ? C17 C18 C19 108.1(12) . . ? C17 C18 Th01 71.4(7) . . ? C19 C18 Th01 76.7(7) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? Th01 C18 H18 117.9 . . ? C20 C19 C18 105.2(11) . . ? C20 C19 Th01 70.9(7) . . ? C18 C19 Th01 75.2(7) . . ? C20 C19 H19 127.4 . . ? C18 C19 H19 127.4 . . ? Th01 C19 H19 118.6 . . ? N2 C20 C19 111.2(11) . . ? N2 C20 C21 120.6(11) . . ? C19 C20 C21 127.6(13) . . ? N2 C20 Th01 71.1(6) . . ? C19 C20 Th01 80.7(7) . . ? C21 C20 Th01 121.7(7) . . ? C20 C21 C24 111.3(10) . . ? C20 C21 C23 110.5(11) . . ? C24 C21 C23 109.6(12) . . ? C20 C21 C22 106.7(12) . . ? C24 C21 C22 111.3(11) . . ? C23 C21 C22 107.4(12) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 122.1(13) . . ? C25 C24 C21 116.5(12) . . ? C29 C24 C21 121.2(11) . . ? C26 C25 C24 121.2(14) . . ? C26 C25 K1 70.5(8) . 4_545 ? C24 C25 K1 90.5(8) . 4_545 ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? K1 C25 H25 109.3 4_545 . ? C27 C26 C25 118.4(14) . . ? C27 C26 K1 81.8(9) . 4_545 ? C25 C26 K1 84.3(9) . 4_545 ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? K1 C26 H26 103.7 4_545 . ? C26 C27 C28 121.7(14) . . ? C26 C27 K1 73.0(9) . 4_545 ? C28 C27 K1 91.4(8) . 4_545 ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? K1 C27 H27 106.0 4_545 . ? C27 C28 C29 122.4(13) . . ? C27 C28 C30 116.3(12) . . ? C29 C28 C30 121.1(11) . . ? C27 C28 K1 65.1(8) . 4_545 ? C29 C28 K1 87.5(8) . 4_545 ? C30 C28 K1 114.2(7) . 4_545 ? C28 C29 C24 114.1(11) . . ? C28 C29 Th01 123.4(9) . . ? C24 C29 Th01 122.4(8) . . ? C28 C29 K1 99.4(8) . . ? C24 C29 K1 97.9(7) . . ? Th01 C29 K1 75.4(3) . . ? C1 C30 C28 110.7(10) . . ? C1 C30 C32 109.6(12) . . ? C28 C30 C32 109.9(12) . . ? C1 C30 C31 106.9(11) . . ? C28 C30 C31 111.3(11) . . ? C32 C30 C31 108.4(11) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C4 N1 C1 105.7(10) . . ? C4 N1 Th01 79.9(7) . . ? C1 N1 Th01 80.2(6) . . ? C4 N1 K1 121.6(8) . . ? C1 N1 K1 122.9(8) . . ? Th01 N1 K1 78.8(3) . . ? C20 N2 C17 105.8(10) . . ? C20 N2 Th01 79.9(7) . . ? C17 N2 Th01 79.2(7) . . ? C20 N2 K1 120.8(8) . . ? C17 N2 K1 122.6(8) . . ? Th01 N2 K1 78.1(3) . . ? Si2 N3 Si1 119.4(7) . . ? Si2 N3 Th01 122.0(6) . . ? Si1 N3 Th01 118.6(7) . . ? N3 Si1 C36 110.5(6) . . ? N3 Si1 C37 112.9(7) . . ? C36 Si1 C37 105.7(7) . . ? N3 Si1 C38 114.9(7) . . ? C36 Si1 C38 105.4(8) . . ? C37 Si1 C38 106.7(8) . . ? N3 Si2 C34 113.9(6) . . ? N3 Si2 C35 109.9(6) . . ? C34 Si2 C35 106.0(7) . . ? N3 Si2 C33 112.3(7) . . ? C34 Si2 C33 107.2(7) . . ? C35 Si2 C33 107.2(8) . . ? N3 Th01 N1 123.4(4) . . ? N3 Th01 N2 125.0(4) . . ? N1 Th01 N2 111.6(3) . . ? N3 Th01 C29 118.6(4) . . ? N1 Th01 C29 72.7(4) . . ? N2 Th01 C29 74.0(4) . . ? N3 Th01 C9 121.8(5) . . ? N1 Th01 C9 74.1(4) . . ? N2 Th01 C9 73.4(4) . . ? C29 Th01 C9 119.6(4) . . ? N3 Th01 C17 105.8(4) . . ? N1 Th01 C17 126.4(3) . . ? N2 Th01 C17 29.6(4) . . ? C29 Th01 C17 103.1(4) . . ? C9 Th01 C17 61.9(4) . . ? N3 Th01 C20 105.2(4) . . ? N1 Th01 C20 125.4(3) . . ? N2 Th01 C20 28.9(4) . . ? C29 Th01 C20 62.4(3) . . ? C9 Th01 C20 102.0(4) . . ? C17 Th01 C20 46.7(4) . . ? N3 Th01 C4 105.1(4) . . ? N1 Th01 C4 29.2(4) . . ? N2 Th01 C4 125.5(4) . . ? C29 Th01 C4 101.6(4) . . ? C9 Th01 C4 62.0(4) . . ? C17 Th01 C4 123.8(4) . . ? C20 Th01 C4 149.7(4) . . ? N3 Th01 C1 102.8(4) . . ? N1 Th01 C1 29.2(4) . . ? N2 Th01 C1 126.4(3) . . ? C29 Th01 C1 61.7(4) . . ? C9 Th01 C1 102.8(4) . . ? C17 Th01 C1 151.4(4) . . ? C20 Th01 C1 124.1(3) . . ? C4 Th01 C1 46.6(4) . . ? N3 Th01 C18 79.4(4) . . ? N1 Th01 C18 154.5(4) . . ? N2 Th01 C18 47.9(3) . . ? C29 Th01 C18 108.4(4) . . ? C9 Th01 C18 84.0(4) . . ? C17 Th01 C18 28.1(4) . . ? C20 Th01 C18 46.3(3) . . ? C4 Th01 C18 142.9(4) . . ? C1 Th01 C18 169.8(3) . . ? N3 Th01 C2 76.6(4) . . ? N1 Th01 C2 48.2(4) . . ? N2 Th01 C2 154.6(4) . . ? C29 Th01 C2 83.9(4) . . ? C9 Th01 C2 108.3(4) . . ? C17 Th01 C2 169.8(4) . . ? C20 Th01 C2 142.9(4) . . ? C4 Th01 C2 46.6(4) . . ? C1 Th01 C2 28.3(4) . . ? C18 Th01 C2 156.0(4) . . ? N3 Th01 C3 78.1(4) . . ? N1 Th01 C3 48.0(3) . . ? N2 Th01 C3 153.5(4) . . ? C29 Th01 C3 108.0(3) . . ? C9 Th01 C3 83.5(4) . . ? C17 Th01 C3 141.8(4) . . ? C20 Th01 C3 170.3(3) . . ? C4 Th01 C3 28.2(4) . . ? C1 Th01 C3 46.3(3) . . ? C18 Th01 C3 143.2(3) . . ? C2 Th01 C3 28.2(4) . . ? N1 K1 C26 112.1(4) . 4 ? N1 K1 N2 91.6(3) . . ? C26 K1 N2 113.2(4) 4 . ? N1 K1 C27 136.9(4) . 4 ? C26 K1 C27 25.2(4) 4 4 ? N2 K1 C27 102.8(3) . 4 ? N1 K1 C29 60.5(3) . . ? C26 K1 C29 169.1(4) 4 . ? N2 K1 C29 61.2(3) . . ? C27 K1 C29 159.5(4) 4 . ? N1 K1 C25 101.3(4) . 4 ? C26 K1 C25 25.3(4) 4 4 ? N2 K1 C25 138.0(4) . 4 ? C27 K1 C25 43.2(4) 4 4 ? C29 K1 C25 157.0(4) . 4 ? N1 K1 C9 60.9(3) . . ? C26 K1 C9 78.5(4) 4 . ? N2 K1 C9 60.1(3) . . ? C27 K1 C9 91.6(4) 4 . ? C29 K1 C9 90.7(4) . . ? C25 K1 C9 91.8(4) 4 . ? N1 K1 C35 115.2(4) . 4 ? C26 K1 C35 107.4(4) 4 4 ? N2 K1 C35 116.9(4) . 4 ? C27 K1 C35 94.2(4) 4 4 ? C29 K1 C35 83.3(3) . 4 ? C25 K1 C35 93.5(4) 4 4 ? C9 K1 C35 174.0(4) . 4 ? N1 K1 C28 149.3(3) . 4 ? C26 K1 C28 42.4(4) 4 4 ? N2 K1 C28 113.2(3) . 4 ? C27 K1 C28 23.5(3) 4 4 ? C29 K1 C28 147.3(3) . 4 ? C25 K1 C28 48.1(4) 4 4 ? C9 K1 C28 115.1(4) . 4 ? C35 K1 C28 70.7(3) 4 4 ? N1 K1 Th01 45.8(2) . . ? C26 K1 Th01 123.7(3) 4 . ? N2 K1 Th01 45.8(2) . . ? C27 K1 Th01 133.2(3) 4 . ? C29 K1 Th01 45.5(2) . . ? C25 K1 Th01 132.5(3) 4 . ? C9 K1 Th01 45.2(3) . . ? C35 K1 Th01 128.9(3) 4 . ? C28 K1 Th01 154.1(2) 4 . ? 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 N1 C1 C2 C3 -4.3(14) . . . . ? C30 C1 C2 C3 168.0(11) . . . . ? Th01 C1 C2 C3 -69.1(9) . . . . ? N1 C1 C2 Th01 64.8(8) . . . . ? C30 C1 C2 Th01 -123.0(13) . . . . ? C1 C2 C3 C4 1.2(14) . . . . ? Th01 C2 C3 C4 -64.7(8) . . . . ? C1 C2 C3 Th01 65.8(8) . . . . ? C2 C3 C4 N1 2.3(14) . . . . ? Th01 C3 C4 N1 -65.5(9) . . . . ? C2 C3 C4 C5 -168.3(12) . . . . ? Th01 C3 C4 C5 124.0(14) . . . . ? C2 C3 C4 Th01 67.7(9) . . . . ? N1 C4 C5 C6 -162.3(12) . . . . ? C3 C4 C5 C6 7.3(19) . . . . ? Th01 C4 C5 C6 112.0(11) . . . . ? N1 C4 C5 C8 76.8(15) . . . . ? C3 C4 C5 C8 -113.5(14) . . . . ? Th01 C4 C5 C8 -8.9(15) . . . . ? N1 C4 C5 C7 -44.1(16) . . . . ? C3 C4 C5 C7 125.6(14) . . . . ? Th01 C4 C5 C7 -129.8(10) . . . . ? C4 C5 C8 C13 -178.5(11) . . . . ? C6 C5 C8 C13 60.1(15) . . . . ? C7 C5 C8 C13 -59.2(15) . . . . ? C4 C5 C8 C9 5.8(17) . . . . ? C6 C5 C8 C9 -115.6(13) . . . . ? C7 C5 C8 C9 125.1(13) . . . . ? C13 C8 C9 C10 1.0(19) . . . . ? C5 C8 C9 C10 176.4(12) . . . . ? C13 C8 C9 Th01 -175.5(10) . . . . ? C5 C8 C9 Th01 -0.1(17) . . . . ? C13 C8 C9 K1 107.2(12) . . . . ? C5 C8 C9 K1 -77.4(12) . . . . ? C8 C9 C10 C11 0.1(19) . . . . ? Th01 C9 C10 C11 176.6(10) . . . . ? K1 C9 C10 C11 -105.0(13) . . . . ? C8 C9 C10 C14 -176.1(12) . . . . ? Th01 C9 C10 C14 0.4(17) . . . . ? K1 C9 C10 C14 78.8(12) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? C14 C10 C11 C12 175.1(13) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C11 C12 C13 C8 0(2) . . . . ? C9 C8 C13 C12 -1(2) . . . . ? C5 C8 C13 C12 -176.5(13) . . . . ? C11 C10 C14 C17 176.9(12) . . . . ? C9 C10 C14 C17 -6.7(18) . . . . ? C11 C10 C14 C15 -62.1(16) . . . . ? C9 C10 C14 C15 114.4(14) . . . . ? C11 C10 C14 C16 57.4(16) . . . . ? C9 C10 C14 C16 -126.1(13) . . . . ? C10 C14 C17 C18 115.6(15) . . . . ? C15 C14 C17 C18 -6(2) . . . . ? C16 C14 C17 C18 -122.4(15) . . . . ? C10 C14 C17 N2 -75.5(16) . . . . ? C15 C14 C17 N2 162.7(12) . . . . ? C16 C14 C17 N2 46.4(16) . . . . ? C10 C14 C17 Th01 10.0(15) . . . . ? C15 C14 C17 Th01 -111.9(11) . . . . ? C16 C14 C17 Th01 131.9(10) . . . . ? N2 C17 C18 C19 -2.5(14) . . . . ? C14 C17 C18 C19 167.3(13) . . . . ? Th01 C17 C18 C19 -68.5(9) . . . . ? N2 C17 C18 Th01 66.0(9) . . . . ? C14 C17 C18 Th01 -124.2(15) . . . . ? C17 C18 C19 C20 0.0(14) . . . . ? Th01 C18 C19 C20 -65.1(8) . . . . ? C17 C18 C19 Th01 65.0(9) . . . . ? C18 C19 C20 N2 2.6(14) . . . . ? Th01 C19 C20 N2 -65.5(8) . . . . ? C18 C19 C20 C21 -168.8(11) . . . . ? Th01 C19 C20 C21 123.1(12) . . . . ? C18 C19 C20 Th01 68.1(9) . . . . ? N2 C20 C21 C24 74.2(14) . . . . ? C19 C20 C21 C24 -115.1(13) . . . . ? Th01 C20 C21 C24 -11.5(15) . . . . ? N2 C20 C21 C23 -163.8(12) . . . . ? C19 C20 C21 C23 6.9(18) . . . . ? Th01 C20 C21 C23 110.5(12) . . . . ? N2 C20 C21 C22 -47.3(15) . . . . ? C19 C20 C21 C22 123.3(14) . . . . ? Th01 C20 C21 C22 -133.0(10) . . . . ? C20 C21 C24 C25 -174.1(12) . . . . ? C23 C21 C24 C25 63.4(15) . . . . ? C22 C21 C24 C25 -55.2(15) . . . . ? C20 C21 C24 C29 9.7(16) . . . . ? C23 C21 C24 C29 -112.8(13) . . . . ? C22 C21 C24 C29 128.6(13) . . . . ? C29 C24 C25 C26 1(2) . . . . ? C21 C24 C25 C26 -175.2(12) . . . . ? C29 C24 C25 K1 68.3(11) . . . 4_545 ? C21 C24 C25 K1 -107.8(10) . . . 4_545 ? C24 C25 C26 C27 1(2) . . . . ? K1 C25 C26 C27 -77.5(13) 4_545 . . . ? C24 C25 C26 K1 78.3(12) . . . 4_545 ? C25 C26 C27 C28 -2(2) . . . . ? K1 C26 C27 C28 -80.8(13) 4_545 . . . ? C25 C26 C27 K1 78.9(13) . . . 4_545 ? C26 C27 C28 C29 1(2) . . . . ? K1 C27 C28 C29 -69.4(12) 4_545 . . . ? C26 C27 C28 C30 176.7(13) . . . . ? K1 C27 C28 C30 105.9(10) 4_545 . . . ? C26 C27 C28 K1 70.8(13) . . . 4_545 ? C27 C28 C29 C24 0.3(18) . . . . ? C30 C28 C29 C24 -174.8(10) . . . . ? K1 C28 C29 C24 -57.9(10) 4_545 . . . ? C27 C28 C29 Th01 178.6(9) . . . . ? C30 C28 C29 Th01 3.4(16) . . . . ? K1 C28 C29 Th01 120.3(7) 4_545 . . . ? C27 C28 C29 K1 -102.9(12) . . . . ? C30 C28 C29 K1 82.0(11) . . . . ? K1 C28 C29 K1 -161.1(3) 4_545 . . . ? C25 C24 C29 C28 -1.4(18) . . . . ? C21 C24 C29 C28 174.5(11) . . . . ? C25 C24 C29 Th01 -179.7(9) . . . . ? C21 C24 C29 Th01 -3.8(15) . . . . ? C25 C24 C29 K1 102.6(11) . . . . ? C21 C24 C29 K1 -81.4(11) . . . . ? N1 C1 C30 C28 -71.6(14) . . . . ? C2 C1 C30 C28 116.8(13) . . . . ? Th01 C1 C30 C28 13.3(15) . . . . ? N1 C1 C30 C32 167.0(11) . . . . ? C2 C1 C30 C32 -4.6(18) . . . . ? Th01 C1 C30 C32 -108.1(12) . . . . ? N1 C1 C30 C31 49.7(14) . . . . ? C2 C1 C30 C31 -121.8(14) . . . . ? Th01 C1 C30 C31 134.7(10) . . . . ? C27 C28 C30 C1 173.9(12) . . . . ? C29 C28 C30 C1 -10.7(17) . . . . ? K1 C28 C30 C1 -113.1(10) 4_545 . . . ? C27 C28 C30 C32 -64.9(15) . . . . ? C29 C28 C30 C32 110.5(13) . . . . ? K1 C28 C30 C32 8.1(13) 4_545 . . . ? C27 C28 C30 C31 55.1(15) . . . . ? C29 C28 C30 C31 -129.5(12) . . . . ? K1 C28 C30 C31 128.1(9) 4_545 . . . ? C3 C4 N1 C1 -4.8(13) . . . . ? C5 C4 N1 C1 166.6(11) . . . . ? Th01 C4 N1 C1 -76.7(8) . . . . ? C3 C4 N1 Th01 71.9(9) . . . . ? C5 C4 N1 Th01 -116.8(11) . . . . ? C3 C4 N1 K1 141.9(8) . . . . ? C5 C4 N1 K1 -46.7(15) . . . . ? Th01 C4 N1 K1 70.1(6) . . . . ? C2 C1 N1 C4 5.6(13) . . . . ? C30 C1 N1 C4 -167.4(10) . . . . ? Th01 C1 N1 C4 76.5(8) . . . . ? C2 C1 N1 Th01 -70.9(9) . . . . ? C30 C1 N1 Th01 116.1(10) . . . . ? C2 C1 N1 K1 -140.6(8) . . . . ? C30 C1 N1 K1 46.4(13) . . . . ? Th01 C1 N1 K1 -69.7(6) . . . . ? C19 C20 N2 C17 -4.1(14) . . . . ? C21 C20 N2 C17 168.0(11) . . . . ? Th01 C20 N2 C17 -75.7(8) . . . . ? C19 C20 N2 Th01 71.6(9) . . . . ? C21 C20 N2 Th01 -116.4(10) . . . . ? C19 C20 N2 K1 141.0(8) . . . . ? C21 C20 N2 K1 -46.9(13) . . . . ? Th01 C20 N2 K1 69.5(6) . . . . ? C18 C17 N2 C20 4.0(14) . . . . ? C14 C17 N2 C20 -166.9(11) . . . . ? Th01 C17 N2 C20 76.2(8) . . . . ? C18 C17 N2 Th01 -72.2(9) . . . . ? C14 C17 N2 Th01 116.9(11) . . . . ? C18 C17 N2 K1 -140.3(8) . . . . ? C14 C17 N2 K1 48.7(15) . . . . ? Th01 C17 N2 K1 -68.2(6) . . . . ? Si2 N3 Si1 C36 -173.5(7) . . . . ? Th01 N3 Si1 C36 6.2(9) . . . . ? Si2 N3 Si1 C37 -55.4(10) . . . . ? Th01 N3 Si1 C37 124.3(8) . . . . ? Si2 N3 Si1 C38 67.4(11) . . . . ? Th01 N3 Si1 C38 -112.9(9) . . . . ? Si1 N3 Si2 C34 65.2(10) . . . . ? Th01 N3 Si2 C34 -114.4(8) . . . . ? Si1 N3 Si2 C35 -176.1(8) . . . . ? Th01 N3 Si2 C35 4.2(10) . . . . ? Si1 N3 Si2 C33 -56.9(11) . . . . ? Th01 N3 Si2 C33 123.4(8) . . . . ? Si2 N3 Th01 N1 -92.3(8) . . . . ? Si1 N3 Th01 N1 88.1(7) . . . . ? Si2 N3 Th01 N2 85.0(8) . . . . ? Si1 N3 Th01 N2 -94.6(8) . . . . ? Si2 N3 Th01 C29 -4.9(9) . . . . ? Si1 N3 Th01 C29 175.5(6) . . . . ? Si2 N3 Th01 C9 176.5(7) . . . . ? Si1 N3 Th01 C9 -3.2(8) . . . . ? Si2 N3 Th01 C17 110.1(7) . . . . ? Si1 N3 Th01 C17 -69.5(8) . . . . ? Si2 N3 Th01 C20 61.6(8) . . . . ? Si1 N3 Th01 C20 -118.1(7) . . . . ? Si2 N3 Th01 C4 -117.5(7) . . . . ? Si1 N3 Th01 C4 62.9(7) . . . . ? Si2 N3 Th01 C1 -69.5(8) . . . . ? Si1 N3 Th01 C1 110.9(7) . . . . ? Si2 N3 Th01 C18 100.4(8) . . . . ? Si1 N3 Th01 C18 -79.3(7) . . . . ? Si2 N3 Th01 C2 -80.2(7) . . . . ? Si1 N3 Th01 C2 100.2(7) . . . . ? Si2 N3 Th01 C3 -109.0(8) . . . . ? Si1 N3 Th01 C3 71.3(7) . . . . ? C4 N1 Th01 N3 -57.4(8) . . . . ? C1 N1 Th01 N3 50.7(8) . . . . ? K1 N1 Th01 N3 177.3(4) . . . . ? C4 N1 Th01 N2 125.0(7) . . . . ? C1 N1 Th01 N2 -126.9(7) . . . . ? K1 N1 Th01 N2 -0.3(4) . . . . ? C4 N1 Th01 C29 -170.7(8) . . . . ? C1 N1 Th01 C29 -62.6(7) . . . . ? K1 N1 Th01 C29 64.0(3) . . . . ? C4 N1 Th01 C9 60.6(8) . . . . ? C1 N1 Th01 C9 168.6(8) . . . . ? K1 N1 Th01 C9 -64.7(3) . . . . ? C4 N1 Th01 C17 95.5(8) . . . . ? C1 N1 Th01 C17 -156.4(7) . . . . ? K1 N1 Th01 C17 -29.8(5) . . . . ? C4 N1 Th01 C20 154.1(7) . . . . ? C1 N1 Th01 C20 -97.8(7) . . . . ? K1 N1 Th01 C20 28.8(5) . . . . ? C1 N1 Th01 C4 108.1(10) . . . . ? K1 N1 Th01 C4 -125.3(8) . . . . ? C4 N1 Th01 C1 -108.1(10) . . . . ? K1 N1 Th01 C1 126.6(7) . . . . ? C4 N1 Th01 C18 92.7(10) . . . . ? C1 N1 Th01 C18 -159.2(7) . . . . ? K1 N1 Th01 C18 -32.6(8) . . . . ? C4 N1 Th01 C2 -73.2(8) . . . . ? C1 N1 Th01 C2 34.8(7) . . . . ? K1 N1 Th01 C2 161.4(5) . . . . ? C4 N1 Th01 C3 -35.0(7) . . . . ? C1 N1 Th01 C3 73.0(7) . . . . ? K1 N1 Th01 C3 -160.4(5) . . . . ? C20 N2 Th01 N3 -52.5(8) . . . . ? C17 N2 Th01 N3 55.8(8) . . . . ? K1 N2 Th01 N3 -177.3(4) . . . . ? C20 N2 Th01 N1 125.0(7) . . . . ? C17 N2 Th01 N1 -126.6(7) . . . . ? K1 N2 Th01 N1 0.3(4) . . . . ? C20 N2 Th01 C29 61.5(7) . . . . ? C17 N2 Th01 C29 169.8(8) . . . . ? K1 N2 Th01 C29 -63.2(3) . . . . ? C20 N2 Th01 C9 -170.1(7) . . . . ? C17 N2 Th01 C9 -61.8(7) . . . . ? K1 N2 Th01 C9 65.1(3) . . . . ? C20 N2 Th01 C17 -108.3(10) . . . . ? K1 N2 Th01 C17 126.9(7) . . . . ? C17 N2 Th01 C20 108.3(10) . . . . ? K1 N2 Th01 C20 -124.7(7) . . . . ? C20 N2 Th01 C4 154.5(7) . . . . ? C17 N2 Th01 C4 -97.2(8) . . . . ? K1 N2 Th01 C4 29.7(5) . . . . ? C20 N2 Th01 C1 96.0(7) . . . . ? C17 N2 Th01 C1 -155.6(7) . . . . ? K1 N2 Th01 C1 -28.7(5) . . . . ? C20 N2 Th01 C18 -73.1(7) . . . . ? C17 N2 Th01 C18 35.3(7) . . . . ? K1 N2 Th01 C18 162.2(5) . . . . ? C20 N2 Th01 C2 92.1(10) . . . . ? C17 N2 Th01 C2 -159.6(9) . . . . ? K1 N2 Th01 C2 -32.7(9) . . . . ? C20 N2 Th01 C3 159.7(7) . . . . ? C17 N2 Th01 C3 -92.0(9) . . . . ? K1 N2 Th01 C3 35.0(8) . . . . ? C28 C29 Th01 N3 -86.9(11) . . . . ? C24 C29 Th01 N3 91.2(10) . . . . ? K1 C29 Th01 N3 -178.6(4) . . . . ? C28 C29 Th01 N1 32.2(10) . . . . ? C24 C29 Th01 N1 -149.7(10) . . . . ? K1 C29 Th01 N1 -59.5(3) . . . . ? C28 C29 Th01 N2 151.5(11) . . . . ? C24 C29 Th01 N2 -30.4(9) . . . . ? K1 C29 Th01 N2 59.8(3) . . . . ? C28 C29 Th01 C9 91.7(10) . . . . ? C24 C29 Th01 C9 -90.1(10) . . . . ? K1 C29 Th01 C9 0.1(5) . . . . ? C28 C29 Th01 C17 156.6(10) . . . . ? C24 C29 Th01 C17 -25.3(10) . . . . ? K1 C29 Th01 C17 64.9(3) . . . . ? C28 C29 Th01 C20 -179.9(12) . . . . ? C24 C29 Th01 C20 -1.7(9) . . . . ? K1 C29 Th01 C20 88.5(4) . . . . ? C28 C29 Th01 C4 27.5(11) . . . . ? C24 C29 Th01 C4 -154.3(9) . . . . ? K1 C29 Th01 C4 -64.1(3) . . . . ? C28 C29 Th01 C1 2.7(9) . . . . ? C24 C29 Th01 C1 -179.2(11) . . . . ? K1 C29 Th01 C1 -89.0(4) . . . . ? C28 C29 Th01 C18 -174.7(10) . . . . ? C24 C29 Th01 C18 3.5(10) . . . . ? K1 C29 Th01 C18 93.6(4) . . . . ? C28 C29 Th01 C2 -15.9(10) . . . . ? C24 C29 Th01 C2 162.3(10) . . . . ? K1 C29 Th01 C2 -107.5(3) . . . . ? C28 C29 Th01 C3 -0.9(11) . . . . ? C24 C29 Th01 C3 177.2(9) . . . . ? K1 C29 Th01 C3 -92.6(4) . . . . ? C8 C9 Th01 N3 87.8(11) . . . . ? C10 C9 Th01 N3 -88.4(12) . . . . ? K1 C9 Th01 N3 178.6(4) . . . . ? C8 C9 Th01 N1 -32.0(10) . . . . ? C10 C9 Th01 N1 151.9(11) . . . . ? K1 C9 Th01 N1 58.8(3) . . . . ? C8 C9 Th01 N2 -150.9(11) . . . . ? C10 C9 Th01 N2 33.0(10) . . . . ? K1 C9 Th01 N2 -60.1(3) . . . . ? C8 C9 Th01 C29 -90.9(11) . . . . ? C10 C9 Th01 C29 93.0(11) . . . . ? K1 C9 Th01 C29 -0.1(5) . . . . ? C8 C9 Th01 C17 179.6(12) . . . . ? C10 C9 Th01 C17 3.4(10) . . . . ? K1 C9 Th01 C17 -89.6(4) . . . . ? C8 C9 Th01 C20 -155.7(10) . . . . ? C10 C9 Th01 C20 28.1(11) . . . . ? K1 C9 Th01 C20 -64.9(3) . . . . ? C8 C9 Th01 C4 -3.2(10) . . . . ? C10 C9 Th01 C4 -179.4(12) . . . . ? K1 C9 Th01 C4 87.6(4) . . . . ? C8 C9 Th01 C1 -26.3(11) . . . . ? C10 C9 Th01 C1 157.5(10) . . . . ? K1 C9 Th01 C1 64.5(3) . . . . ? C8 C9 Th01 C18 161.4(11) . . . . ? C10 C9 Th01 C18 -14.8(11) . . . . ? K1 C9 Th01 C18 -107.8(3) . . . . ? C8 C9 Th01 C2 2.5(12) . . . . ? C10 C9 Th01 C2 -173.6(10) . . . . ? K1 C9 Th01 C2 93.4(4) . . . . ? C8 C9 Th01 C3 16.1(10) . . . . ? C10 C9 Th01 C3 -160.1(11) . . . . ? K1 C9 Th01 C3 106.9(3) . . . . ? C18 C17 Th01 N3 -20.7(9) . . . . ? N2 C17 Th01 N3 -135.3(7) . . . . ? C14 C17 Th01 N3 110.7(10) . . . . ? C18 C17 Th01 N1 -177.4(7) . . . . ? N2 C17 Th01 N1 68.0(8) . . . . ? C14 C17 Th01 N1 -46.0(12) . . . . ? C18 C17 Th01 N2 114.6(11) . . . . ? C14 C17 Th01 N2 -114.0(13) . . . . ? C18 C17 Th01 C29 104.5(8) . . . . ? N2 C17 Th01 C29 -10.0(7) . . . . ? C14 C17 Th01 C29 -124.0(10) . . . . ? C18 C17 Th01 C9 -138.7(9) . . . . ? N2 C17 Th01 C9 106.7(7) . . . . ? C14 C17 Th01 C9 -7.3(10) . . . . ? C18 C17 Th01 C20 75.4(9) . . . . ? N2 C17 Th01 C20 -39.1(7) . . . . ? C14 C17 Th01 C20 -153.1(12) . . . . ? C18 C17 Th01 C4 -141.7(7) . . . . ? N2 C17 Th01 C4 103.8(7) . . . . ? C14 C17 Th01 C4 -10.2(12) . . . . ? C18 C17 Th01 C1 158.5(8) . . . . ? N2 C17 Th01 C1 43.9(12) . . . . ? C14 C17 Th01 C1 -70.1(14) . . . . ? N2 C17 Th01 C18 -114.6(11) . . . . ? C14 C17 Th01 C18 131.5(15) . . . . ? C18 C17 Th01 C2 -123(2) . . . . ? N2 C17 Th01 C2 123(2) . . . . ? C14 C17 Th01 C2 9(3) . . . . ? C18 C17 Th01 C3 -111.5(8) . . . . ? N2 C17 Th01 C3 133.9(7) . . . . ? C14 C17 Th01 C3 19.9(13) . . . . ? N2 C20 Th01 N3 137.7(7) . . . . ? C19 C20 Th01 N3 21.3(9) . . . . ? C21 C20 Th01 N3 -107.4(11) . . . . ? N2 C20 Th01 N1 -69.2(7) . . . . ? C19 C20 Th01 N1 174.5(7) . . . . ? C21 C20 Th01 N1 45.7(12) . . . . ? C19 C20 Th01 N2 -116.3(11) . . . . ? C21 C20 Th01 N2 114.9(13) . . . . ? N2 C20 Th01 C29 -107.6(8) . . . . ? C19 C20 Th01 C29 136.1(9) . . . . ? C21 C20 Th01 C29 7.3(10) . . . . ? N2 C20 Th01 C9 9.7(7) . . . . ? C19 C20 Th01 C9 -106.7(8) . . . . ? C21 C20 Th01 C9 124.6(11) . . . . ? N2 C20 Th01 C17 40.1(7) . . . . ? C19 C20 Th01 C17 -76.3(8) . . . . ? C21 C20 Th01 C17 155.0(13) . . . . ? N2 C20 Th01 C4 -44.1(11) . . . . ? C19 C20 Th01 C4 -160.5(8) . . . . ? C21 C20 Th01 C4 70.7(14) . . . . ? N2 C20 Th01 C1 -104.9(7) . . . . ? C19 C20 Th01 C1 138.7(8) . . . . ? C21 C20 Th01 C1 10.0(13) . . . . ? N2 C20 Th01 C18 79.2(8) . . . . ? C19 C20 Th01 C18 -37.1(7) . . . . ? C21 C20 Th01 C18 -165.9(14) . . . . ? N2 C20 Th01 C2 -134.6(8) . . . . ? C19 C20 Th01 C2 109.0(8) . . . . ? C21 C20 Th01 C2 -19.8(15) . . . . ? N2 C20 Th01 C3 -114(3) . . . . ? C19 C20 Th01 C3 130(2) . . . . ? C21 C20 Th01 C3 1(3) . . . . ? N1 C4 Th01 N3 133.2(7) . . . . ? C3 C4 Th01 N3 17.7(8) . . . . ? C5 C4 Th01 N3 -111.8(10) . . . . ? C3 C4 Th01 N1 -115.5(11) . . . . ? C5 C4 Th01 N1 115.0(13) . . . . ? N1 C4 Th01 N2 -69.4(8) . . . . ? C3 C4 Th01 N2 175.1(7) . . . . ? C5 C4 Th01 N2 45.6(11) . . . . ? N1 C4 Th01 C29 9.1(8) . . . . ? C3 C4 Th01 C29 -106.5(8) . . . . ? C5 C4 Th01 C29 124.0(10) . . . . ? N1 C4 Th01 C9 -108.4(8) . . . . ? C3 C4 Th01 C9 136.1(9) . . . . ? C5 C4 Th01 C9 6.6(9) . . . . ? N1 C4 Th01 C17 -105.5(8) . . . . ? C3 C4 Th01 C17 139.0(7) . . . . ? C5 C4 Th01 C17 9.5(12) . . . . ? N1 C4 Th01 C20 -44.9(12) . . . . ? C3 C4 Th01 C20 -160.5(7) . . . . ? C5 C4 Th01 C20 70.0(13) . . . . ? N1 C4 Th01 C1 39.8(7) . . . . ? C3 C4 Th01 C1 -75.8(8) . . . . ? C5 C4 Th01 C1 154.7(12) . . . . ? N1 C4 Th01 C18 -134.4(7) . . . . ? C3 C4 Th01 C18 110.0(8) . . . . ? C5 C4 Th01 C18 -19.5(13) . . . . ? N1 C4 Th01 C2 79.1(8) . . . . ? C3 C4 Th01 C2 -36.5(7) . . . . ? C5 C4 Th01 C2 -166.0(12) . . . . ? N1 C4 Th01 C3 115.5(11) . . . . ? C5 C4 Th01 C3 -129.5(14) . . . . ? N1 C1 Th01 N3 -138.5(7) . . . . ? C2 C1 Th01 N3 -22.4(9) . . . . ? C30 C1 Th01 N3 107.0(11) . . . . ? C2 C1 Th01 N1 116.1(11) . . . . ? C30 C1 Th01 N1 -114.5(13) . . . . ? N1 C1 Th01 N2 67.5(8) . . . . ? C2 C1 Th01 N2 -176.4(7) . . . . ? C30 C1 Th01 N2 -47.0(13) . . . . ? N1 C1 Th01 C29 105.7(8) . . . . ? C2 C1 Th01 C29 -138.2(10) . . . . ? C30 C1 Th01 C29 -8.8(10) . . . . ? N1 C1 Th01 C9 -11.2(7) . . . . ? C2 C1 Th01 C9 104.9(9) . . . . ? C30 C1 Th01 C9 -125.7(11) . . . . ? N1 C1 Th01 C17 42.3(11) . . . . ? C2 C1 Th01 C17 158.4(9) . . . . ? C30 C1 Th01 C17 -72.2(15) . . . . ? N1 C1 Th01 C20 103.0(7) . . . . ? C2 C1 Th01 C20 -140.9(8) . . . . ? C30 C1 Th01 C20 -11.5(13) . . . . ? N1 C1 Th01 C4 -39.7(7) . . . . ? C2 C1 Th01 C4 76.4(8) . . . . ? C30 C1 Th01 C4 -154.2(13) . . . . ? N1 C1 Th01 C18 120(2) . . . . ? C2 C1 Th01 C18 -124(2) . . . . ? C30 C1 Th01 C18 6(3) . . . . ? N1 C1 Th01 C2 -116.1(11) . . . . ? C30 C1 Th01 C2 129.4(16) . . . . ? N1 C1 Th01 C3 -79.0(8) . . . . ? C2 C1 Th01 C3 37.1(8) . . . . ? C30 C1 Th01 C3 166.5(14) . . . . ? C17 C18 Th01 N3 159.7(9) . . . . ? C19 C18 Th01 N3 -85.6(8) . . . . ? C17 C18 Th01 N1 4.8(13) . . . . ? C19 C18 Th01 N1 119.4(10) . . . . ? C17 C18 Th01 N2 -37.2(8) . . . . ? C19 C18 Th01 N2 77.4(8) . . . . ? C17 C18 Th01 C29 -83.4(8) . . . . ? C19 C18 Th01 C29 31.2(9) . . . . ? C17 C18 Th01 C9 35.8(8) . . . . ? C19 C18 Th01 C9 150.4(8) . . . . ? C19 C18 Th01 C17 114.6(12) . . . . ? C17 C18 Th01 C20 -77.1(9) . . . . ? C19 C18 Th01 C20 37.5(8) . . . . ? C17 C18 Th01 C4 58.7(10) . . . . ? C19 C18 Th01 C4 173.3(8) . . . . ? C17 C18 Th01 C1 -97(2) . . . . ? C19 C18 Th01 C1 18(3) . . . . ? C17 C18 Th01 C2 158.5(10) . . . . ? C19 C18 Th01 C2 -86.9(12) . . . . ? C17 C18 Th01 C3 106.5(10) . . . . ? C19 C18 Th01 C3 -138.9(9) . . . . ? C1 C2 Th01 N3 157.5(9) . . . . ? C3 C2 Th01 N3 -89.9(9) . . . . ? C1 C2 Th01 N1 -36.1(8) . . . . ? C3 C2 Th01 N1 76.5(9) . . . . ? C1 C2 Th01 N2 6.7(14) . . . . ? C3 C2 Th01 N2 119.3(10) . . . . ? C1 C2 Th01 C29 36.2(8) . . . . ? C3 C2 Th01 C29 148.7(8) . . . . ? C1 C2 Th01 C9 -83.0(9) . . . . ? C3 C2 Th01 C9 29.6(9) . . . . ? C1 C2 Th01 C17 -98(2) . . . . ? C3 C2 Th01 C17 15(3) . . . . ? C1 C2 Th01 C20 60.1(11) . . . . ? C3 C2 Th01 C20 172.6(8) . . . . ? C1 C2 Th01 C4 -76.1(9) . . . . ? C3 C2 Th01 C4 36.5(8) . . . . ? C3 C2 Th01 C1 112.6(12) . . . . ? C1 C2 Th01 C18 158.8(9) . . . . ? C3 C2 Th01 C18 -88.6(12) . . . . ? C1 C2 Th01 C3 -112.6(12) . . . . ? C4 C3 Th01 N3 -162.6(8) . . . . ? C2 C3 Th01 N3 83.6(9) . . . . ? C4 C3 Th01 N1 36.4(7) . . . . ? C2 C3 Th01 N1 -77.4(8) . . . . ? C4 C3 Th01 N2 -9.1(12) . . . . ? C2 C3 Th01 N2 -122.9(10) . . . . ? C4 C3 Th01 C29 80.9(8) . . . . ? C2 C3 Th01 C29 -32.9(9) . . . . ? C4 C3 Th01 C9 -38.1(8) . . . . ? C2 C3 Th01 C9 -151.9(9) . . . . ? C4 C3 Th01 C17 -62.0(9) . . . . ? C2 C3 Th01 C17 -175.8(8) . . . . ? C4 C3 Th01 C20 87(3) . . . . ? C2 C3 Th01 C20 -27(3) . . . . ? C2 C3 Th01 C4 -113.8(12) . . . . ? C4 C3 Th01 C1 76.6(9) . . . . ? C2 C3 Th01 C1 -37.2(8) . . . . ? C4 C3 Th01 C18 -109.0(9) . . . . ? C2 C3 Th01 C18 137.2(8) . . . . ? C4 C3 Th01 C2 113.8(12) . . . . ? C4 N1 K1 C26 45.5(10) . . . 4 ? C1 N1 K1 C26 -173.5(9) . . . 4 ? Th01 N1 K1 C26 116.1(4) . . . 4 ? C4 N1 K1 N2 -70.4(9) . . . . ? C1 N1 K1 N2 70.6(9) . . . . ? Th01 N1 K1 N2 0.2(3) . . . . ? C4 N1 K1 C27 40.3(11) . . . 4 ? C1 N1 K1 C27 -178.7(8) . . . 4 ? Th01 N1 K1 C27 111.0(5) . . . 4 ? C4 N1 K1 C29 -125.7(10) . . . . ? C1 N1 K1 C29 15.3(8) . . . . ? Th01 N1 K1 C29 -55.0(3) . . . . ? C4 N1 K1 C25 69.4(9) . . . 4 ? C1 N1 K1 C25 -149.6(9) . . . 4 ? Th01 N1 K1 C25 140.0(3) . . . 4 ? C4 N1 K1 C9 -16.3(9) . . . . ? C1 N1 K1 C9 124.7(10) . . . . ? Th01 N1 K1 C9 54.3(3) . . . . ? C4 N1 K1 C35 168.8(9) . . . 4 ? C1 N1 K1 C35 -50.2(10) . . . 4 ? Th01 N1 K1 C35 -120.6(4) . . . 4 ? C4 N1 K1 C28 74.3(11) . . . 4 ? C1 N1 K1 C28 -144.6(8) . . . 4 ? Th01 N1 K1 C28 145.0(5) . . . 4 ? C4 N1 K1 Th01 -70.6(9) . . . . ? C1 N1 K1 Th01 70.4(8) . . . . ? C20 N2 K1 N1 -70.7(9) . . . . ? C17 N2 K1 N1 68.5(9) . . . . ? Th01 N2 K1 N1 -0.2(3) . . . . ? C20 N2 K1 C26 174.4(9) . . . 4 ? C17 N2 K1 C26 -46.4(10) . . . 4 ? Th01 N2 K1 C26 -115.2(4) . . . 4 ? C20 N2 K1 C27 150.2(9) . . . 4 ? C17 N2 K1 C27 -70.6(9) . . . 4 ? Th01 N2 K1 C27 -139.3(3) . . . 4 ? C20 N2 K1 C29 -16.0(8) . . . . ? C17 N2 K1 C29 123.3(10) . . . . ? Th01 N2 K1 C29 54.5(3) . . . . ? C20 N2 K1 C25 -179.5(8) . . . 4 ? C17 N2 K1 C25 -40.3(11) . . . 4 ? Th01 N2 K1 C25 -109.1(5) . . . 4 ? C20 N2 K1 C9 -125.4(10) . . . . ? C17 N2 K1 C9 13.8(9) . . . . ? Th01 N2 K1 C9 -54.9(3) . . . . ? C20 N2 K1 C35 48.8(10) . . . 4 ? C17 N2 K1 C35 -172.0(9) . . . 4 ? Th01 N2 K1 C35 119.2(4) . . . 4 ? C20 N2 K1 C28 128.0(9) . . . 4 ? C17 N2 K1 C28 -92.8(9) . . . 4 ? Th01 N2 K1 C28 -161.5(3) . . . 4 ? C20 N2 K1 Th01 -70.4(8) . . . . ? C17 N2 K1 Th01 68.8(9) . . . . ? C28 C29 K1 N1 -66.8(8) . . . . ? C24 C29 K1 N1 177.0(9) . . . . ? Th01 C29 K1 N1 55.5(3) . . . . ? C28 C29 K1 C26 -116(2) . . . 4 ? C24 C29 K1 C26 128(2) . . . 4 ? Th01 C29 K1 C26 6(2) . . . 4 ? C28 C29 K1 N2 -177.1(9) . . . . ? C24 C29 K1 N2 66.7(7) . . . . ? Th01 C29 K1 N2 -54.9(3) . . . . ? C28 C29 K1 C27 141.3(10) . . . 4 ? C24 C29 K1 C27 25.1(14) . . . 4 ? Th01 C29 K1 C27 -96.5(10) . . . 4 ? C28 C29 K1 C25 -26.1(14) . . . 4 ? C24 C29 K1 C25 -142.3(9) . . . 4 ? Th01 C29 K1 C25 96.2(9) . . . 4 ? C28 C29 K1 C9 -122.3(8) . . . . ? C24 C29 K1 C9 121.5(8) . . . . ? Th01 C29 K1 C9 0.0(3) . . . . ? C28 C29 K1 C35 57.2(8) . . . 4 ? C24 C29 K1 C35 -59.0(8) . . . 4 ? Th01 C29 K1 C35 179.4(4) . . . 4 ? C28 C29 K1 C28 94.3(10) . . . 4 ? C24 C29 K1 C28 -21.9(11) . . . 4 ? Th01 C29 K1 C28 -143.4(5) . . . 4 ? C28 C29 K1 Th01 -122.2(9) . . . . ? C24 C29 K1 Th01 121.6(8) . . . . ? C8 C9 K1 N1 67.0(8) . . . . ? C10 C9 K1 N1 -176.7(10) . . . . ? Th01 C9 K1 N1 -55.2(3) . . . . ? C8 C9 K1 C26 -56.6(9) . . . 4 ? C10 C9 K1 C26 59.8(9) . . . 4 ? Th01 C9 K1 C26 -178.7(4) . . . 4 ? C8 C9 K1 N2 177.9(10) . . . . ? C10 C9 K1 N2 -65.7(9) . . . . ? Th01 C9 K1 N2 55.8(3) . . . . ? C8 C9 K1 C27 -78.2(9) . . . 4 ? C10 C9 K1 C27 38.1(9) . . . 4 ? Th01 C9 K1 C27 159.6(4) . . . 4 ? C8 C9 K1 C29 122.2(9) . . . . ? C10 C9 K1 C29 -121.5(9) . . . . ? Th01 C9 K1 C29 0.0(3) . . . . ? C8 C9 K1 C25 -34.9(9) . . . 4 ? C10 C9 K1 C25 81.4(9) . . . 4 ? Th01 C9 K1 C25 -157.1(4) . . . 4 ? C8 C9 K1 C35 117(4) . . . 4 ? C10 C9 K1 C35 -127(4) . . . 4 ? Th01 C9 K1 C35 -5(4) . . . 4 ? C8 C9 K1 C28 -78.6(9) . . . 4 ? C10 C9 K1 C28 37.7(10) . . . 4 ? Th01 C9 K1 C28 159.2(3) . . . 4 ? C8 C9 K1 Th01 122.2(10) . . . . ? C10 C9 K1 Th01 -121.5(10) . . . . ? N3 Th01 K1 N1 -61(7) . . . . ? N2 Th01 K1 N1 179.7(4) . . . . ? C29 Th01 K1 N1 -89.6(4) . . . . ? C9 Th01 K1 N1 90.5(4) . . . . ? C17 Th01 K1 N1 155.7(4) . . . . ? C20 Th01 K1 N1 -156.0(4) . . . . ? C4 Th01 K1 N1 24.4(4) . . . . ? C1 Th01 K1 N1 -23.9(4) . . . . ? C18 Th01 K1 N1 166.2(4) . . . . ? C2 Th01 K1 N1 -14.0(4) . . . . ? C3 Th01 K1 N1 14.7(4) . . . . ? N3 Th01 K1 C26 -150(7) . . . 4 ? N1 Th01 K1 C26 -89.0(5) . . . 4 ? N2 Th01 K1 C26 90.7(5) . . . 4 ? C29 Th01 K1 C26 -178.6(5) . . . 4 ? C9 Th01 K1 C26 1.5(5) . . . 4 ? C17 Th01 K1 C26 66.7(5) . . . 4 ? C20 Th01 K1 C26 115.0(5) . . . 4 ? C4 Th01 K1 C26 -64.6(5) . . . 4 ? C1 Th01 K1 C26 -112.9(5) . . . 4 ? C18 Th01 K1 C26 77.3(5) . . . 4 ? C2 Th01 K1 C26 -103.0(5) . . . 4 ? C3 Th01 K1 C26 -74.2(5) . . . 4 ? N3 Th01 K1 N2 119(7) . . . . ? N1 Th01 K1 N2 -179.7(4) . . . . ? C29 Th01 K1 N2 90.8(4) . . . . ? C9 Th01 K1 N2 -89.2(4) . . . . ? C17 Th01 K1 N2 -24.0(4) . . . . ? C20 Th01 K1 N2 24.3(4) . . . . ? C4 Th01 K1 N2 -155.3(4) . . . . ? C1 Th01 K1 N2 156.4(4) . . . . ? C18 Th01 K1 N2 -13.4(4) . . . . ? C2 Th01 K1 N2 166.3(4) . . . . ? C3 Th01 K1 N2 -164.9(4) . . . . ? N3 Th01 K1 C27 180(100) . . . 4 ? N1 Th01 K1 C27 -119.0(5) . . . 4 ? N2 Th01 K1 C27 60.7(5) . . . 4 ? C29 Th01 K1 C27 151.4(5) . . . 4 ? C9 Th01 K1 C27 -28.5(5) . . . 4 ? C17 Th01 K1 C27 36.7(5) . . . 4 ? C20 Th01 K1 C27 85.0(5) . . . 4 ? C4 Th01 K1 C27 -94.6(5) . . . 4 ? C1 Th01 K1 C27 -142.9(5) . . . 4 ? C18 Th01 K1 C27 47.3(5) . . . 4 ? C2 Th01 K1 C27 -133.0(5) . . . 4 ? C3 Th01 K1 C27 -104.2(5) . . . 4 ? N3 Th01 K1 C29 28(7) . . . . ? N1 Th01 K1 C29 89.6(4) . . . . ? N2 Th01 K1 C29 -90.8(4) . . . . ? C9 Th01 K1 C29 -179.9(5) . . . . ? C17 Th01 K1 C29 -114.7(4) . . . . ? C20 Th01 K1 C29 -66.5(4) . . . . ? C4 Th01 K1 C29 114.0(4) . . . . ? C1 Th01 K1 C29 65.6(4) . . . . ? C18 Th01 K1 C29 -104.2(4) . . . . ? C2 Th01 K1 C29 75.6(4) . . . . ? C3 Th01 K1 C29 104.3(4) . . . . ? N3 Th01 K1 C25 -120(7) . . . 4 ? N1 Th01 K1 C25 -58.7(5) . . . 4 ? N2 Th01 K1 C25 121.0(5) . . . 4 ? C29 Th01 K1 C25 -148.3(5) . . . 4 ? C9 Th01 K1 C25 31.8(5) . . . 4 ? C17 Th01 K1 C25 97.0(5) . . . 4 ? C20 Th01 K1 C25 145.3(5) . . . 4 ? C4 Th01 K1 C25 -34.3(5) . . . 4 ? C1 Th01 K1 C25 -82.6(5) . . . 4 ? C18 Th01 K1 C25 107.6(5) . . . 4 ? C2 Th01 K1 C25 -72.7(5) . . . 4 ? C3 Th01 K1 C25 -43.9(5) . . . 4 ? N3 Th01 K1 C9 -152(7) . . . . ? N1 Th01 K1 C9 -90.5(4) . . . . ? N2 Th01 K1 C9 89.2(4) . . . . ? C29 Th01 K1 C9 179.9(5) . . . . ? C17 Th01 K1 C9 65.2(5) . . . . ? C20 Th01 K1 C9 113.5(4) . . . . ? C4 Th01 K1 C9 -66.1(5) . . . . ? C1 Th01 K1 C9 -114.4(4) . . . . ? C18 Th01 K1 C9 75.8(4) . . . . ? C2 Th01 K1 C9 -104.5(5) . . . . ? C3 Th01 K1 C9 -75.7(4) . . . . ? N3 Th01 K1 C35 28(7) . . . 4 ? N1 Th01 K1 C35 88.9(5) . . . 4 ? N2 Th01 K1 C35 -91.5(5) . . . 4 ? C29 Th01 K1 C35 -0.7(5) . . . 4 ? C9 Th01 K1 C35 179.3(5) . . . 4 ? C17 Th01 K1 C35 -115.5(5) . . . 4 ? C20 Th01 K1 C35 -67.2(5) . . . 4 ? C4 Th01 K1 C35 113.2(5) . . . 4 ? C1 Th01 K1 C35 64.9(5) . . . 4 ? C18 Th01 K1 C35 -104.9(5) . . . 4 ? C2 Th01 K1 C35 74.8(5) . . . 4 ? C3 Th01 K1 C35 103.6(5) . . . 4 ? N3 Th01 K1 C28 161(7) . . . 4 ? N1 Th01 K1 C28 -137.9(6) . . . 4 ? N2 Th01 K1 C28 41.8(6) . . . 4 ? C29 Th01 K1 C28 132.6(6) . . . 4 ? C9 Th01 K1 C28 -47.4(6) . . . 4 ? C17 Th01 K1 C28 17.8(6) . . . 4 ? C20 Th01 K1 C28 66.1(6) . . . 4 ? C4 Th01 K1 C28 -113.5(6) . . . 4 ? C1 Th01 K1 C28 -161.8(6) . . . 4 ? C18 Th01 K1 C28 28.4(6) . . . 4 ? C2 Th01 K1 C28 -151.9(6) . . . 4 ? C3 Th01 K1 C28 -123.1(6) . . . 4 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 73.45 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.973 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.141 _database_code_depnum_ccdc_archive 'CCDC 951387' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po3006_refinalized2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 I N2 O U, C6 H12 O1.5' _chemical_formula_sum 'C42 H56 I N2 O2.50 U' _chemical_formula_weight 993.82 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' I I -0.4742 1.8119 '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 10.112(5) _cell_length_b 11.224(5) _cell_length_c 18.141(5) _cell_angle_alpha 99.530(5) _cell_angle_beta 99.536(5) _cell_angle_gamma 108.352(5) _cell_volume 1874.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 27329 _cell_measurement_theta_min 2.6788 _cell_measurement_theta_max 25.2931 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.3004 _exptl_crystal_size_mid 0.1042 _exptl_crystal_size_min 0.0691 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 5.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87370 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6851 _reflns_number_gt 6421 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material Mercury _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+25.3904P] 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 6851 _refine_ls_number_parameters 468 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.000 _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 0.0265(8) 0.1562(7) 0.1519(4) 0.0192(15) Uani 1 1 d . . . C2 C -0.0857(8) 0.0405(7) 0.1313(4) 0.0240(16) Uani 1 1 d . . . H2 H -0.0896 -0.0372 0.0993 0.029 Uiso 1 1 calc R . . C3 C -0.1941(9) 0.0591(8) 0.1665(4) 0.0253(17) Uani 1 1 d . . . H3 H -0.2849 -0.0040 0.1628 0.030 Uiso 1 1 calc R . . C4 C -0.1440(8) 0.1857(7) 0.2074(4) 0.0208(15) Uani 1 1 d . . . C5 C -0.2268(8) 0.2533(7) 0.2505(4) 0.0217(16) Uani 1 1 d . . . C6 C -0.2809(9) 0.1822(8) 0.3111(5) 0.0280(18) Uani 1 1 d . . . H6A H -0.3466 0.0944 0.2856 0.042 Uiso 1 1 calc R . . H6B H -0.3313 0.2286 0.3394 0.042 Uiso 1 1 calc R . . H6C H -0.1993 0.1781 0.3469 0.042 Uiso 1 1 calc R . . C7 C -0.3598(8) 0.2497(8) 0.1928(5) 0.0276(18) Uani 1 1 d . . . H7A H -0.3289 0.2951 0.1535 0.041 Uiso 1 1 calc R . . H7B H -0.4149 0.2920 0.2201 0.041 Uiso 1 1 calc R . . H7C H -0.4198 0.1598 0.1683 0.041 Uiso 1 1 calc R . . C8 C -0.1318(8) 0.3959(8) 0.2872(4) 0.0221(16) Uani 1 1 d . . . C9 C -0.0868(8) 0.4753(7) 0.2377(5) 0.0250(17) Uani 1 1 d . . . H9 H -0.1205 0.4428 0.1837 0.030 Uiso 1 1 calc R . . C10 C 0.0083(9) 0.6032(8) 0.2677(5) 0.0314(19) Uani 1 1 d . . . C11 C 0.0574(8) 0.6477(8) 0.3472(5) 0.032(2) Uani 1 1 d . . . H11 H 0.1230 0.7332 0.3686 0.038 Uiso 1 1 calc R . . C12 C 0.0108(9) 0.5678(8) 0.3943(5) 0.033(2) Uani 1 1 d . . . H12 H 0.0436 0.5994 0.4484 0.039 Uiso 1 1 calc R . . C13 C -0.0835(9) 0.4414(8) 0.3646(5) 0.0286(18) Uani 1 1 d . . . H13 H -0.1139 0.3873 0.3982 0.034 Uiso 1 1 calc R . . C14 C 0.0646(10) 0.6932(9) 0.2163(7) 0.044(2) Uani 1 1 d U . . C15 C 0.0325(10) 0.8170(10) 0.2387(9) 0.072(4) Uani 1 1 d U . . H15A H 0.0656 0.8744 0.2050 0.108 Uiso 1 1 calc R . . H15B H 0.0824 0.8605 0.2922 0.108 Uiso 1 1 calc R . . H15C H -0.0709 0.7955 0.2331 0.108 Uiso 1 1 calc R . . C16 C -0.0048(11) 0.6324(12) 0.1315(7) 0.070(4) Uani 1 1 d U . . H16A H 0.0302 0.6949 0.1010 0.105 Uiso 1 1 calc R . . H16B H -0.1090 0.6074 0.1233 0.105 Uiso 1 1 calc R . . H16C H 0.0199 0.5559 0.1156 0.105 Uiso 1 1 calc R . . C17 C 0.2253(9) 0.7242(8) 0.2300(5) 0.0285(18) Uani 1 1 d . . . C18 C 0.3267(9) 0.8326(8) 0.2223(5) 0.0303(19) Uani 1 1 d . . . H18 H 0.3116 0.9082 0.2121 0.036 Uiso 1 1 calc R . . C19 C 0.4579(9) 0.8112(8) 0.2324(5) 0.0303(19) Uani 1 1 d . . . H19 H 0.5478 0.8692 0.2299 0.036 Uiso 1 1 calc R . . C20 C 0.4307(8) 0.6904(7) 0.2464(4) 0.0220(16) Uani 1 1 d . . . C21 C 0.5429(8) 0.6269(8) 0.2604(5) 0.0261(17) Uani 1 1 d . . . C22 C 0.6551(10) 0.7024(9) 0.3359(6) 0.041(2) Uani 1 1 d . . . H22A H 0.6073 0.7041 0.3786 0.061 Uiso 1 1 calc R . . H22B H 0.7036 0.7909 0.3320 0.061 Uiso 1 1 calc R . . H22C H 0.7256 0.6602 0.3450 0.061 Uiso 1 1 calc R . . C23 C 0.6214(9) 0.6276(9) 0.1944(5) 0.034(2) Uani 1 1 d . . . H23A H 0.6868 0.5798 0.2017 0.052 Uiso 1 1 calc R . . H23B H 0.6761 0.7168 0.1944 0.052 Uiso 1 1 calc R . . H23C H 0.5511 0.5865 0.1453 0.052 Uiso 1 1 calc R . . C24 C 0.4644(8) 0.4879(8) 0.2619(4) 0.0236(16) Uani 1 1 d . . . C25 C 0.4848(8) 0.4373(7) 0.3242(5) 0.0211(16) Uani 1 1 d . . . H25 H 0.5541 0.4900 0.3695 0.025 Uiso 1 1 calc R . . C26 C 0.4057(8) 0.3094(7) 0.3233(4) 0.0217(16) Uani 1 1 d . . . H26 H 0.4209 0.2762 0.3676 0.026 Uiso 1 1 calc R . . C27 C 0.3053(8) 0.2317(7) 0.2573(4) 0.0212(16) Uani 1 1 d . . . H27 H 0.2526 0.1445 0.2561 0.025 Uiso 1 1 calc R . . C28 C 0.2808(8) 0.2812(7) 0.1916(4) 0.0196(15) Uani 1 1 d . . . C29 C 0.3622(8) 0.4075(7) 0.1948(4) 0.0213(16) Uani 1 1 d . . . H29 H 0.3489 0.4413 0.1506 0.026 Uiso 1 1 calc R . . C30 C 0.1623(8) 0.1951(7) 0.1227(4) 0.0211(16) Uani 1 1 d . . . C31 C 0.1999(9) 0.0779(7) 0.0902(4) 0.0246(17) Uani 1 1 d . . . H31A H 0.2096 0.0295 0.1298 0.037 Uiso 1 1 calc R . . H31B H 0.2904 0.1073 0.0743 0.037 Uiso 1 1 calc R . . H31C H 0.1236 0.0220 0.0457 0.037 Uiso 1 1 calc R . . C32 C 0.1409(9) 0.2659(8) 0.0584(4) 0.0262(17) Uani 1 1 d . . . H32A H 0.0622 0.2076 0.0158 0.039 Uiso 1 1 calc R . . H32B H 0.2291 0.2935 0.0401 0.039 Uiso 1 1 calc R . . H32C H 0.1178 0.3416 0.0785 0.039 Uiso 1 1 calc R . . C33 C 0.0719(12) 0.1236(9) 0.3529(6) 0.041(2) Uani 1 1 d U . . H33A H 0.1597 0.1045 0.3483 0.049 Uiso 1 1 calc R . . H33B H 0.0033 0.0908 0.3021 0.049 Uiso 1 1 calc R . . C34 C 0.0066(15) 0.0639(12) 0.4126(7) 0.061(3) Uani 1 1 d U . . H34A H 0.0488 -0.0003 0.4262 0.073 Uiso 1 1 calc R . . H34B H -0.0981 0.0200 0.3929 0.073 Uiso 1 1 calc R . . C35 C 0.0388(15) 0.1738(12) 0.4831(7) 0.073(4) Uani 1 1 d DU . . H35A H -0.0489 0.1914 0.4901 0.087 Uiso 1 1 calc R . . H35B H 0.0828 0.1543 0.5305 0.087 Uiso 1 1 calc R . . C36 C 0.1402(11) 0.2820(10) 0.4628(5) 0.046(2) Uani 1 1 d DU . . H36A H 0.1318 0.3645 0.4865 0.055 Uiso 1 1 calc R . . H36B H 0.2397 0.2861 0.4813 0.055 Uiso 1 1 calc R . . C38 C 0.4669(12) 0.7176(16) 0.0126(8) 0.110(4) Uani 1 1 d DU . . H38A H 0.4948 0.6971 -0.0365 0.132 Uiso 1 1 calc R . . H38B H 0.5475 0.7294 0.0557 0.132 Uiso 1 1 calc R . . C37 C 0.3342(12) 0.6128(15) 0.0160(8) 0.121(4) Uani 1 1 d DU . . H37A H 0.3300 0.5265 -0.0101 0.145 Uiso 1 1 calc R . . H37B H 0.3251 0.6129 0.0695 0.145 Uiso 1 1 calc R . . O2 O 0.2272(11) 0.6536(13) -0.0259(6) 0.114(4) Uani 1 1 d DU . . C40 C 0.2673(13) 0.7877(14) 0.0015(9) 0.113(4) Uani 1 1 d DU . . H40A H 0.2328 0.8074 0.0484 0.135 Uiso 1 1 calc R . . H40B H 0.2275 0.8264 -0.0380 0.135 Uiso 1 1 calc R . . C39 C 0.4265(13) 0.8376(16) 0.0187(9) 0.114(4) Uani 1 1 d DU . . H39A H 0.4671 0.8943 0.0710 0.137 Uiso 1 1 calc R . . H39B H 0.4616 0.8868 -0.0190 0.137 Uiso 1 1 calc R . . N1 N -0.0047(7) 0.2479(6) 0.2009(3) 0.0208(13) Uani 1 1 d . . . N2 N 0.2862(7) 0.6332(6) 0.2464(4) 0.0290(16) Uani 1 1 d . . . O1 O 0.1052(7) 0.2602(6) 0.3800(3) 0.0317(13) Uani 1 1 d U . . I1 I 0.36310(6) 0.60653(6) 0.46688(3) 0.03739(17) Uani 1 1 d . . . U1 U 0.17944(3) 0.44104(3) 0.298506(16) 0.01974(10) Uani 1 1 d . . . O3 O 0.2948(15) 0.9601(18) 0.4467(8) 0.067(4) Uani 0.50 1 d PDU A -1 C42 C 0.543(2) 0.994(4) 0.4773(12) 0.057(6) Uani 0.50 1 d PDU A -1 H42A H 0.6206 1.0751 0.4785 0.069 Uiso 0.50 1 calc PR A -1 H42B H 0.5802 0.9221 0.4690 0.069 Uiso 0.50 1 calc PR A -1 C41 C 0.4170(19) 0.971(3) 0.4149(11) 0.065(5) Uani 0.50 1 d PDU A -1 H41A H 0.4353 1.0429 0.3887 0.078 Uiso 0.50 1 calc PR A -1 H41B H 0.3990 0.8902 0.3765 0.078 Uiso 0.50 1 calc PR A -1 C43 C 0.495(3) 1.003(3) 0.5526(12) 0.063(8) Uani 0.50 1 d PD A -1 H43A H 0.5005 0.9313 0.5763 0.075 Uiso 0.50 1 calc PR A -1 H43B H 0.5534 1.0862 0.5895 0.075 Uiso 0.50 1 calc PR A -1 C44 C 0.344(2) 0.995(3) 0.5280(9) 0.075(5) Uani 0.50 1 d PDU A -1 H44A H 0.2820 0.9303 0.5504 0.090 Uiso 0.50 1 calc PR A -1 H44B H 0.3362 1.0796 0.5480 0.090 Uiso 0.50 1 calc PR A -1 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 0.022(4) 0.021(4) 0.011(3) 0.004(3) 0.001(3) 0.005(3) C2 0.028(4) 0.016(4) 0.019(4) -0.003(3) 0.004(3) 0.002(3) C3 0.025(4) 0.021(4) 0.020(4) -0.001(3) 0.005(3) -0.001(3) C4 0.022(4) 0.021(4) 0.014(3) 0.002(3) 0.001(3) 0.003(3) C5 0.022(4) 0.021(4) 0.021(4) 0.005(3) 0.007(3) 0.006(3) C6 0.035(5) 0.019(4) 0.029(4) 0.004(3) 0.015(4) 0.005(3) C7 0.018(4) 0.029(4) 0.028(4) 0.005(3) 0.000(3) 0.003(3) C8 0.012(3) 0.033(4) 0.022(4) 0.012(3) 0.001(3) 0.007(3) C9 0.020(4) 0.018(4) 0.032(4) 0.005(3) -0.003(3) 0.005(3) C10 0.021(4) 0.020(4) 0.050(6) 0.010(4) -0.003(4) 0.008(3) C11 0.018(4) 0.017(4) 0.052(6) 0.000(4) -0.004(4) 0.005(3) C12 0.025(4) 0.030(5) 0.038(5) -0.009(4) 0.000(4) 0.015(4) C13 0.029(4) 0.025(4) 0.031(5) 0.000(3) 0.002(4) 0.014(4) C14 0.027(5) 0.023(4) 0.074(6) 0.029(4) -0.011(4) -0.001(4) C15 0.019(5) 0.033(5) 0.166(12) 0.051(6) 0.001(6) 0.008(4) C16 0.037(6) 0.072(7) 0.066(6) 0.054(5) -0.027(5) -0.026(5) C17 0.027(4) 0.017(4) 0.034(5) 0.008(3) -0.006(3) 0.003(3) C18 0.025(4) 0.017(4) 0.048(5) 0.010(4) 0.004(4) 0.007(3) C19 0.030(4) 0.018(4) 0.033(5) 0.002(3) 0.004(4) -0.002(3) C20 0.022(4) 0.021(4) 0.017(4) 0.003(3) -0.001(3) 0.002(3) C21 0.018(4) 0.022(4) 0.030(4) 0.006(3) -0.006(3) 0.000(3) C22 0.034(5) 0.027(5) 0.042(5) 0.005(4) -0.014(4) -0.002(4) C23 0.020(4) 0.034(5) 0.045(5) 0.015(4) 0.002(4) 0.003(4) C24 0.015(4) 0.024(4) 0.025(4) 0.000(3) -0.001(3) 0.003(3) C25 0.015(4) 0.013(3) 0.031(4) 0.001(3) 0.001(3) 0.004(3) C26 0.024(4) 0.026(4) 0.015(4) 0.005(3) 0.000(3) 0.011(3) C27 0.025(4) 0.018(4) 0.018(4) 0.003(3) 0.002(3) 0.006(3) C28 0.017(4) 0.024(4) 0.015(4) 0.001(3) 0.001(3) 0.006(3) C29 0.020(4) 0.020(4) 0.022(4) 0.008(3) 0.001(3) 0.004(3) C30 0.020(4) 0.019(4) 0.016(4) 0.003(3) -0.001(3) -0.001(3) C31 0.025(4) 0.024(4) 0.018(4) 0.000(3) 0.006(3) 0.002(3) C32 0.024(4) 0.029(4) 0.016(4) 0.004(3) -0.001(3) 0.000(3) C33 0.074(7) 0.028(4) 0.041(5) 0.018(4) 0.028(5) 0.032(5) C34 0.084(8) 0.057(6) 0.060(7) 0.025(5) 0.030(6) 0.036(6) C35 0.082(9) 0.085(9) 0.042(6) 0.011(5) 0.019(6) 0.015(7) C36 0.067(7) 0.067(6) 0.020(4) 0.013(4) 0.015(4) 0.041(5) C38 0.051(5) 0.199(10) 0.043(5) 0.062(7) -0.012(5) -0.009(6) C37 0.066(6) 0.188(9) 0.050(6) 0.042(7) -0.026(5) -0.020(6) O2 0.064(5) 0.166(9) 0.076(6) 0.020(6) 0.001(4) 0.003(5) C40 0.061(6) 0.170(9) 0.058(6) 0.001(7) 0.016(5) -0.012(6) C39 0.060(6) 0.187(10) 0.049(6) 0.027(7) 0.004(5) -0.017(6) N1 0.021(3) 0.017(3) 0.017(3) 0.003(2) -0.002(3) 0.001(3) N2 0.018(3) 0.016(3) 0.041(4) 0.008(3) -0.009(3) -0.002(3) O1 0.051(4) 0.030(3) 0.025(3) 0.010(2) 0.012(3) 0.026(3) I1 0.0369(3) 0.0362(3) 0.0292(3) -0.0137(2) -0.0138(2) 0.0212(3) U1 0.02114(16) 0.01372(15) 0.01853(15) 0.00137(10) -0.00390(10) 0.00378(11) O3 0.056(7) 0.087(9) 0.053(7) 0.002(7) 0.007(6) 0.027(7) C42 0.056(9) 0.064(11) 0.052(12) 0.007(11) 0.004(9) 0.030(10) C41 0.058(9) 0.081(10) 0.051(9) 0.009(9) 0.005(7) 0.023(9) C43 0.09(2) 0.038(13) 0.054(19) 0.018(14) -0.001(16) 0.017(15) C44 0.063(10) 0.095(12) 0.055(8) -0.002(10) 0.009(8) 0.023(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.372(11) . ? C1 N1 1.394(10) . ? C1 C30 1.516(10) . ? C2 C3 1.409(11) . ? C2 H2 0.9500 . ? C3 C4 1.378(11) . ? C3 H3 0.9500 . ? C4 N1 1.396(10) . ? C4 C5 1.520(11) . ? C5 C6 1.535(10) . ? C5 C7 1.546(11) . ? C5 C8 1.548(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.361(11) . ? C8 C9 1.396(11) . ? C8 U1 2.992(7) . ? C9 C10 1.407(11) . ? C9 U1 2.902(8) . ? C9 H9 0.9500 . ? C10 C11 1.395(13) . ? C10 C14 1.529(13) . ? C10 U1 2.936(8) . ? C11 C12 1.371(13) . ? C11 U1 3.028(8) . ? C11 H11 0.9500 . ? C12 C13 1.392(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.518(12) . ? C14 C16 1.523(16) . ? C14 C15 1.530(15) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.367(11) . ? C17 N2 1.396(10) . ? C18 C19 1.409(12) . ? C18 H18 0.9500 . ? C19 C20 1.371(11) . ? C19 H19 0.9500 . ? C20 N2 1.398(10) . ? C20 C21 1.528(11) . ? C21 C24 1.519(11) . ? C21 C22 1.541(11) . ? C21 C23 1.541(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.362(11) . ? C24 C29 1.412(11) . ? C24 U1 2.970(8) . ? C25 C26 1.402(11) . ? C25 U1 3.060(7) . ? C25 H25 0.9500 . ? C26 C27 1.386(10) . ? C26 H26 0.9500 . ? C27 C28 1.413(10) . ? C27 U1 3.053(8) . ? C27 H27 0.9500 . ? C28 C29 1.383(11) . ? C28 C30 1.519(10) . ? C28 U1 2.949(7) . ? C29 U1 2.907(8) . ? C29 H29 0.9500 . ? C30 C31 1.534(11) . ? C30 C32 1.539(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 O1 1.441(10) . ? C33 C34 1.502(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.533(17) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.467(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O1 1.444(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C38 C37 1.499(9) . ? C38 C39 1.519(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C37 O2 1.454(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O2 C40 1.406(9) . ? C40 C39 1.487(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? N1 U1 2.530(6) . ? N2 U1 2.501(7) . ? O1 U1 2.696(6) . ? I1 U1 3.2091(9) . ? O3 C44 1.421(10) . ? O3 C41 1.429(10) . ? C42 C41 1.481(10) . ? C42 C43 1.524(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 C44 1.485(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? 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 C2 C1 N1 110.5(7) . . ? C2 C1 C30 129.1(7) . . ? N1 C1 C30 120.1(6) . . ? C1 C2 C3 106.9(7) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? C4 C3 C2 107.3(7) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 N1 109.9(7) . . ? C3 C4 C5 126.5(7) . . ? N1 C4 C5 123.5(6) . . ? C4 C5 C6 110.6(6) . . ? C4 C5 C7 108.7(6) . . ? C6 C5 C7 107.4(6) . . ? C4 C5 C8 109.9(6) . . ? C6 C5 C8 111.6(6) . . ? C7 C5 C8 108.6(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 120.3(8) . . ? C13 C8 C5 121.9(7) . . ? C9 C8 C5 117.6(7) . . ? C13 C8 U1 81.3(5) . . ? C9 C8 U1 72.7(4) . . ? C5 C8 U1 112.1(5) . . ? C8 C9 C10 120.2(8) . . ? C8 C9 U1 79.9(4) . . ? C10 C9 U1 77.4(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? U1 C9 H9 113.2 . . ? C11 C10 C9 118.6(8) . . ? C11 C10 C14 118.8(8) . . ? C9 C10 C14 122.5(8) . . ? C11 C10 U1 80.2(5) . . ? C9 C10 U1 74.7(4) . . ? C14 C10 U1 113.1(6) . . ? C12 C11 C10 119.8(8) . . ? C12 C11 U1 80.3(5) . . ? C10 C11 U1 72.8(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? U1 C11 H11 117.6 . . ? C11 C12 C13 121.4(8) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 119.6(8) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C17 C14 C16 109.5(10) . . ? C17 C14 C10 107.7(7) . . ? C16 C14 C10 112.2(7) . . ? C17 C14 C15 110.0(7) . . ? C16 C14 C15 108.6(9) . . ? C10 C14 C15 108.8(10) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 110.8(7) . . ? C18 C17 C14 127.9(7) . . ? N2 C17 C14 121.1(7) . . ? C17 C18 C19 107.2(7) . . ? C17 C18 H18 126.4 . . ? C19 C18 H18 126.4 . . ? C20 C19 C18 106.7(7) . . ? C20 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? C19 C20 N2 110.9(7) . . ? C19 C20 C21 124.7(7) . . ? N2 C20 C21 124.5(7) . . ? C24 C21 C20 107.4(6) . . ? C24 C21 C22 112.4(7) . . ? C20 C21 C22 109.9(7) . . ? C24 C21 C23 108.7(7) . . ? C20 C21 C23 110.3(7) . . ? C22 C21 C23 108.0(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.4(7) . . ? C25 C24 C21 123.9(7) . . ? C29 C24 C21 117.7(7) . . ? C25 C24 U1 80.7(5) . . ? C29 C24 U1 73.6(4) . . ? C21 C24 U1 114.2(5) . . ? C24 C25 C26 121.6(7) . . ? C24 C25 U1 73.3(4) . . ? C26 C25 U1 78.6(4) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? U1 C25 H25 119.8 . . ? C27 C26 C25 119.5(7) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 120.5(7) . . ? C26 C27 U1 79.0(4) . . ? C28 C27 U1 72.3(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? U1 C27 H27 119.8 . . ? C29 C28 C27 118.1(7) . . ? C29 C28 C30 123.5(7) . . ? C27 C28 C30 118.4(7) . . ? C29 C28 U1 74.7(4) . . ? C27 C28 U1 80.5(4) . . ? C30 C28 U1 112.4(5) . . ? C28 C29 C24 122.0(7) . . ? C28 C29 U1 78.0(4) . . ? C24 C29 U1 78.6(4) . . ? C28 C29 H29 119.0 . . ? C24 C29 H29 119.0 . . ? U1 C29 H29 114.7 . . ? C1 C30 C28 106.1(6) . . ? C1 C30 C31 112.0(6) . . ? C28 C30 C31 109.2(6) . . ? C1 C30 C32 108.9(6) . . ? C28 C30 C32 112.2(6) . . ? C31 C30 C32 108.5(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O1 C33 C34 104.8(8) . . ? O1 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O1 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C33 C34 C35 107.0(9) . . ? C33 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? C33 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? C36 C35 C34 101.7(9) . . ? C36 C35 H35A 111.4 . . ? C34 C35 H35A 111.4 . . ? C36 C35 H35B 111.4 . . ? C34 C35 H35B 111.4 . . ? H35A C35 H35B 109.3 . . ? O1 C36 C35 107.3(9) . . ? O1 C36 H36A 110.3 . . ? C35 C36 H36A 110.3 . . ? O1 C36 H36B 110.3 . . ? C35 C36 H36B 110.3 . . ? H36A C36 H36B 108.5 . . ? C37 C38 C39 104.6(11) . . ? C37 C38 H38A 110.8 . . ? C39 C38 H38A 110.8 . . ? C37 C38 H38B 110.8 . . ? C39 C38 H38B 110.8 . . ? H38A C38 H38B 108.9 . . ? O2 C37 C38 99.2(9) . . ? O2 C37 H37A 111.9 . . ? C38 C37 H37A 111.9 . . ? O2 C37 H37B 111.9 . . ? C38 C37 H37B 111.9 . . ? H37A C37 H37B 109.6 . . ? C40 O2 C37 107.6(11) . . ? O2 C40 C39 104.9(11) . . ? O2 C40 H40A 110.8 . . ? C39 C40 H40A 110.8 . . ? O2 C40 H40B 110.8 . . ? C39 C40 H40B 110.8 . . ? H40A C40 H40B 108.8 . . ? C40 C39 C38 104.6(11) . . ? C40 C39 H39A 110.8 . . ? C38 C39 H39A 110.8 . . ? C40 C39 H39B 110.8 . . ? C38 C39 H39B 110.8 . . ? H39A C39 H39B 108.9 . . ? C1 N1 C4 105.3(6) . . ? C1 N1 U1 125.1(5) . . ? C4 N1 U1 124.8(5) . . ? C17 N2 C20 104.4(6) . . ? C17 N2 U1 127.3(5) . . ? C20 N2 U1 126.5(5) . . ? C33 O1 C36 104.5(7) . . ? C33 O1 U1 126.1(5) . . ? C36 O1 U1 126.0(5) . . ? N2 U1 N1 115.2(2) . . ? N2 U1 O1 168.6(2) . . ? N1 U1 O1 76.02(19) . . ? N2 U1 C9 82.9(2) . . ? N1 U1 C9 65.0(2) . . ? O1 U1 C9 104.5(2) . . ? N2 U1 C29 65.0(2) . . ? N1 U1 C29 82.8(2) . . ? O1 U1 C29 116.85(19) . . ? C9 U1 C29 118.6(2) . . ? N2 U1 C10 61.9(2) . . ? N1 U1 C10 91.5(2) . . ? O1 U1 C10 121.8(2) . . ? C9 U1 C10 27.9(2) . . ? C29 U1 C10 117.4(2) . . ? N2 U1 C28 90.8(2) . . ? N1 U1 C28 61.6(2) . . ? O1 U1 C28 93.39(19) . . ? C9 U1 C28 116.6(2) . . ? C29 U1 C28 27.3(2) . . ? C10 U1 C28 130.0(2) . . ? N2 U1 C24 60.8(2) . . ? N1 U1 C24 109.4(2) . . ? O1 U1 C24 115.0(2) . . ? C9 U1 C24 137.5(2) . . ? C29 U1 C24 27.8(2) . . ? C10 U1 C24 122.6(2) . . ? C28 U1 C24 48.8(2) . . ? N2 U1 C8 109.1(2) . . ? N1 U1 C8 61.0(2) . . ? O1 U1 C8 77.43(19) . . ? C9 U1 C8 27.4(2) . . ? C29 U1 C8 137.4(2) . . ? C10 U1 C8 48.4(2) . . ? C28 U1 C8 122.4(2) . . ? C24 U1 C8 163.2(2) . . ? N2 U1 C11 70.1(2) . . ? N1 U1 C11 112.0(2) . . ? O1 U1 C11 108.4(2) . . ? C9 U1 C11 47.9(2) . . ? C29 U1 C11 134.7(2) . . ? C10 U1 C11 27.0(3) . . ? C28 U1 C11 155.5(2) . . ? C24 U1 C11 125.4(2) . . ? C8 U1 C11 55.0(2) . . ? N2 U1 C27 111.7(2) . . ? N1 U1 C27 69.3(2) . . ? O1 U1 C27 69.50(18) . . ? C9 U1 C27 133.8(2) . . ? C29 U1 C27 47.4(2) . . ? C10 U1 C27 155.6(2) . . ? C28 U1 C27 27.2(2) . . ? C24 U1 C27 55.3(2) . . ? C8 U1 C27 125.3(2) . . ? C11 U1 C27 177.3(2) . . ? N2 U1 C25 82.9(2) . . ? N1 U1 C25 114.4(2) . . ? O1 U1 C25 90.77(19) . . ? C9 U1 C25 163.6(2) . . ? C29 U1 C25 47.0(2) . . ? C10 U1 C25 143.2(2) . . ? C28 U1 C25 55.3(2) . . ? C24 U1 C25 26.0(2) . . ? C8 U1 C25 168.0(2) . . ? C11 U1 C25 132.8(2) . . ? C27 U1 C25 46.40(19) . . ? C44 O3 C41 107.4(13) . . ? C41 C42 C43 107.2(17) . . ? C41 C42 H42A 110.3 . . ? C43 C42 H42A 110.3 . . ? C41 C42 H42B 110.3 . . ? C43 C42 H42B 110.3 . . ? H42A C42 H42B 108.5 . . ? O3 C41 C42 109.3(15) . . ? O3 C41 H41A 109.8 . . ? C42 C41 H41A 109.8 . . ? O3 C41 H41B 109.8 . . ? C42 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? C44 C43 C42 102.9(17) . . ? C44 C43 H43A 111.2 . . ? C42 C43 H43A 111.2 . . ? C44 C43 H43B 111.2 . . ? C42 C43 H43B 111.2 . . ? H43A C43 H43B 109.1 . . ? O3 C44 C43 111.9(15) . . ? O3 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? O3 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? 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 N1 C1 C2 C3 1.4(9) . . . . ? C30 C1 C2 C3 -171.8(7) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C2 C3 C4 N1 -1.6(9) . . . . ? C2 C3 C4 C5 175.6(7) . . . . ? C3 C4 C5 C6 57.5(10) . . . . ? N1 C4 C5 C6 -125.6(8) . . . . ? C3 C4 C5 C7 -60.2(10) . . . . ? N1 C4 C5 C7 116.7(8) . . . . ? C3 C4 C5 C8 -178.9(7) . . . . ? N1 C4 C5 C8 -2.0(10) . . . . ? C4 C5 C8 C13 -111.8(8) . . . . ? C6 C5 C8 C13 11.3(10) . . . . ? C7 C5 C8 C13 129.5(8) . . . . ? C4 C5 C8 C9 63.0(9) . . . . ? C6 C5 C8 C9 -173.9(7) . . . . ? C7 C5 C8 C9 -55.7(9) . . . . ? C4 C5 C8 U1 -18.4(7) . . . . ? C6 C5 C8 U1 104.7(6) . . . . ? C7 C5 C8 U1 -137.1(5) . . . . ? C13 C8 C9 C10 -0.4(12) . . . . ? C5 C8 C9 C10 -175.3(7) . . . . ? U1 C8 C9 C10 -68.9(7) . . . . ? C13 C8 C9 U1 68.5(7) . . . . ? C5 C8 C9 U1 -106.4(6) . . . . ? C8 C9 C10 C11 0.8(12) . . . . ? U1 C9 C10 C11 -69.5(7) . . . . ? C8 C9 C10 C14 178.2(8) . . . . ? U1 C9 C10 C14 107.9(8) . . . . ? C8 C9 C10 U1 70.3(7) . . . . ? C9 C10 C11 C12 -1.1(12) . . . . ? C14 C10 C11 C12 -178.6(8) . . . . ? U1 C10 C11 C12 -67.6(7) . . . . ? C9 C10 C11 U1 66.5(7) . . . . ? C14 C10 C11 U1 -111.0(8) . . . . ? C10 C11 C12 C13 1.0(12) . . . . ? U1 C11 C12 C13 -62.6(7) . . . . ? C9 C8 C13 C12 0.2(12) . . . . ? C5 C8 C13 C12 174.9(7) . . . . ? U1 C8 C13 C12 64.3(7) . . . . ? C11 C12 C13 C8 -0.6(12) . . . . ? C11 C10 C14 C17 62.2(11) . . . . ? C9 C10 C14 C17 -115.2(9) . . . . ? U1 C10 C14 C17 -29.1(9) . . . . ? C11 C10 C14 C16 -177.3(9) . . . . ? C9 C10 C14 C16 5.4(13) . . . . ? U1 C10 C14 C16 91.4(9) . . . . ? C11 C10 C14 C15 -57.1(10) . . . . ? C9 C10 C14 C15 125.5(9) . . . . ? U1 C10 C14 C15 -148.4(6) . . . . ? C16 C14 C17 C18 85.5(12) . . . . ? C10 C14 C17 C18 -152.2(9) . . . . ? C15 C14 C17 C18 -33.7(15) . . . . ? C16 C14 C17 N2 -88.5(10) . . . . ? C10 C14 C17 N2 33.7(12) . . . . ? C15 C14 C17 N2 152.2(10) . . . . ? N2 C17 C18 C19 1.2(10) . . . . ? C14 C17 C18 C19 -173.3(9) . . . . ? C17 C18 C19 C20 -0.4(10) . . . . ? C18 C19 C20 N2 -0.5(10) . . . . ? C18 C19 C20 C21 179.7(7) . . . . ? C19 C20 C21 C24 -171.9(7) . . . . ? N2 C20 C21 C24 8.3(10) . . . . ? C19 C20 C21 C22 65.5(10) . . . . ? N2 C20 C21 C22 -114.4(8) . . . . ? C19 C20 C21 C23 -53.6(10) . . . . ? N2 C20 C21 C23 126.6(8) . . . . ? C20 C21 C24 C25 -117.6(8) . . . . ? C22 C21 C24 C25 3.5(12) . . . . ? C23 C21 C24 C25 123.1(8) . . . . ? C20 C21 C24 C29 61.0(9) . . . . ? C22 C21 C24 C29 -177.9(7) . . . . ? C23 C21 C24 C29 -58.3(9) . . . . ? C20 C21 C24 U1 -22.5(7) . . . . ? C22 C21 C24 U1 98.6(7) . . . . ? C23 C21 C24 U1 -141.8(5) . . . . ? C29 C24 C25 C26 -0.8(11) . . . . ? C21 C24 C25 C26 177.7(7) . . . . ? U1 C24 C25 C26 64.7(7) . . . . ? C29 C24 C25 U1 -65.6(6) . . . . ? C21 C24 C25 U1 113.0(8) . . . . ? C24 C25 C26 C27 0.6(11) . . . . ? U1 C25 C26 C27 62.7(7) . . . . ? C25 C26 C27 C28 -1.0(11) . . . . ? C25 C26 C27 U1 -62.8(7) . . . . ? C26 C27 C28 C29 1.6(11) . . . . ? U1 C27 C28 C29 66.8(6) . . . . ? C26 C27 C28 C30 -175.7(7) . . . . ? U1 C27 C28 C30 -110.5(6) . . . . ? C26 C27 C28 U1 -65.2(7) . . . . ? C27 C28 C29 C24 -1.9(11) . . . . ? C30 C28 C29 C24 175.3(7) . . . . ? U1 C28 C29 C24 68.2(7) . . . . ? C27 C28 C29 U1 -70.1(6) . . . . ? C30 C28 C29 U1 107.0(7) . . . . ? C25 C24 C29 C28 1.5(12) . . . . ? C21 C24 C29 C28 -177.2(7) . . . . ? U1 C24 C29 C28 -68.0(7) . . . . ? C25 C24 C29 U1 69.5(7) . . . . ? C21 C24 C29 U1 -109.2(7) . . . . ? C2 C1 C30 C28 -143.2(8) . . . . ? N1 C1 C30 C28 44.2(9) . . . . ? C2 C1 C30 C31 -24.1(11) . . . . ? N1 C1 C30 C31 163.2(6) . . . . ? C2 C1 C30 C32 95.8(9) . . . . ? N1 C1 C30 C32 -76.8(8) . . . . ? C29 C28 C30 C1 -120.4(8) . . . . ? C27 C28 C30 C1 56.7(9) . . . . ? U1 C28 C30 C1 -34.4(7) . . . . ? C29 C28 C30 C31 118.7(8) . . . . ? C27 C28 C30 C31 -64.2(9) . . . . ? U1 C28 C30 C31 -155.3(5) . . . . ? C29 C28 C30 C32 -1.6(11) . . . . ? C27 C28 C30 C32 175.5(7) . . . . ? U1 C28 C30 C32 84.4(7) . . . . ? O1 C33 C34 C35 -13.8(13) . . . . ? C33 C34 C35 C36 -9.5(14) . . . . ? C34 C35 C36 O1 30.0(13) . . . . ? C39 C38 C37 O2 35.8(14) . . . . ? C38 C37 O2 C40 -44.6(15) . . . . ? C37 O2 C40 C39 35.2(16) . . . . ? O2 C40 C39 C38 -10.4(16) . . . . ? C37 C38 C39 C40 -16.5(15) . . . . ? C2 C1 N1 C4 -2.4(8) . . . . ? C30 C1 N1 C4 171.5(6) . . . . ? C2 C1 N1 U1 154.0(5) . . . . ? C30 C1 N1 U1 -32.1(9) . . . . ? C3 C4 N1 C1 2.4(8) . . . . ? C5 C4 N1 C1 -174.9(7) . . . . ? C3 C4 N1 U1 -154.1(5) . . . . ? C5 C4 N1 U1 28.6(9) . . . . ? C18 C17 N2 C20 -1.5(10) . . . . ? C14 C17 N2 C20 173.5(8) . . . . ? C18 C17 N2 U1 163.8(6) . . . . ? C14 C17 N2 U1 -21.3(12) . . . . ? C19 C20 N2 C17 1.2(9) . . . . ? C21 C20 N2 C17 -178.9(7) . . . . ? C19 C20 N2 U1 -164.2(6) . . . . ? C21 C20 N2 U1 15.6(11) . . . . ? C34 C33 O1 C36 32.3(11) . . . . ? C34 C33 O1 U1 -167.7(7) . . . . ? C35 C36 O1 C33 -40.3(11) . . . . ? C35 C36 O1 U1 159.6(8) . . . . ? C17 N2 U1 N1 79.4(7) . . . . ? C20 N2 U1 N1 -118.5(6) . . . . ? C17 N2 U1 O1 -110.4(10) . . . . ? C20 N2 U1 O1 51.7(14) . . . . ? C17 N2 U1 C9 21.4(7) . . . . ? C20 N2 U1 C9 -176.5(7) . . . . ? C17 N2 U1 C29 147.5(7) . . . . ? C20 N2 U1 C29 -50.3(6) . . . . ? C17 N2 U1 C10 2.0(6) . . . . ? C20 N2 U1 C10 164.1(7) . . . . ? C17 N2 U1 C28 138.1(7) . . . . ? C20 N2 U1 C28 -59.7(6) . . . . ? C17 N2 U1 C24 178.5(7) . . . . ? C20 N2 U1 C24 -19.4(6) . . . . ? C17 N2 U1 C8 13.2(7) . . . . ? C20 N2 U1 C8 175.4(6) . . . . ? C17 N2 U1 C11 -26.3(6) . . . . ? C20 N2 U1 C11 135.9(7) . . . . ? C17 N2 U1 C27 155.9(6) . . . . ? C20 N2 U1 C27 -41.9(7) . . . . ? C17 N2 U1 C25 -166.9(7) . . . . ? C20 N2 U1 C25 -4.8(6) . . . . ? C1 N1 U1 N2 83.0(6) . . . . ? C4 N1 U1 N2 -125.0(6) . . . . ? C1 N1 U1 O1 -95.0(6) . . . . ? C4 N1 U1 O1 57.0(6) . . . . ? C1 N1 U1 C9 151.4(6) . . . . ? C4 N1 U1 C9 -56.7(6) . . . . ? C1 N1 U1 C29 25.1(5) . . . . ? C4 N1 U1 C29 177.0(6) . . . . ? C1 N1 U1 C10 142.5(6) . . . . ? C4 N1 U1 C10 -65.5(6) . . . . ? C1 N1 U1 C28 6.8(5) . . . . ? C4 N1 U1 C28 158.7(6) . . . . ? C1 N1 U1 C24 17.0(6) . . . . ? C4 N1 U1 C24 169.0(5) . . . . ? C1 N1 U1 C8 -178.2(6) . . . . ? C4 N1 U1 C8 -26.2(5) . . . . ? C1 N1 U1 C11 160.6(5) . . . . ? C4 N1 U1 C11 -47.5(6) . . . . ? C1 N1 U1 C27 -21.9(5) . . . . ? C4 N1 U1 C27 130.0(6) . . . . ? C1 N1 U1 C25 -10.6(6) . . . . ? C4 N1 U1 C25 141.4(5) . . . . ? C33 O1 U1 N2 -134.4(11) . . . . ? C36 O1 U1 N2 21.5(14) . . . . ? C33 O1 U1 N1 36.5(7) . . . . ? C36 O1 U1 N1 -167.7(7) . . . . ? C33 O1 U1 C9 95.5(7) . . . . ? C36 O1 U1 C9 -108.7(7) . . . . ? C33 O1 U1 C29 -37.8(7) . . . . ? C36 O1 U1 C29 118.1(6) . . . . ? C33 O1 U1 C10 119.4(7) . . . . ? C36 O1 U1 C10 -84.7(7) . . . . ? C33 O1 U1 C28 -23.2(7) . . . . ? C36 O1 U1 C28 132.7(6) . . . . ? C33 O1 U1 C24 -68.7(7) . . . . ? C36 O1 U1 C24 87.2(7) . . . . ? C33 O1 U1 C8 99.3(7) . . . . ? C36 O1 U1 C8 -104.8(7) . . . . ? C33 O1 U1 C11 145.4(7) . . . . ? C36 O1 U1 C11 -58.7(7) . . . . ? C33 O1 U1 C27 -36.4(7) . . . . ? C36 O1 U1 C27 119.5(7) . . . . ? C33 O1 U1 C25 -78.5(7) . . . . ? C36 O1 U1 C25 77.4(7) . . . . ? C8 C9 U1 N2 -163.0(5) . . . . ? C10 C9 U1 N2 -38.8(5) . . . . ? C8 C9 U1 N1 74.9(5) . . . . ? C10 C9 U1 N1 -160.8(6) . . . . ? C8 C9 U1 O1 8.2(5) . . . . ? C10 C9 U1 O1 132.5(5) . . . . ? C8 C9 U1 C29 140.5(5) . . . . ? C10 C9 U1 C29 -95.2(6) . . . . ? C8 C9 U1 C10 -124.3(8) . . . . ? C8 C9 U1 C28 109.7(5) . . . . ? C10 C9 U1 C28 -126.0(5) . . . . ? C8 C9 U1 C24 166.7(4) . . . . ? C10 C9 U1 C24 -69.0(6) . . . . ? C10 C9 U1 C8 124.3(8) . . . . ? C8 C9 U1 C11 -93.6(6) . . . . ? C10 C9 U1 C11 30.7(5) . . . . ? C8 C9 U1 C27 83.6(6) . . . . ? C10 C9 U1 C27 -152.1(5) . . . . ? C8 C9 U1 C25 166.4(6) . . . . ? C10 C9 U1 C25 -69.3(10) . . . . ? C28 C29 U1 N2 -159.2(5) . . . . ? C24 C29 U1 N2 74.3(5) . . . . ? C28 C29 U1 N1 -37.0(4) . . . . ? C24 C29 U1 N1 -163.5(5) . . . . ? C28 C29 U1 O1 33.3(5) . . . . ? C24 C29 U1 O1 -93.2(5) . . . . ? C28 C29 U1 C9 -93.3(5) . . . . ? C24 C29 U1 C9 140.2(4) . . . . ? C28 C29 U1 C10 -124.9(4) . . . . ? C24 C29 U1 C10 108.5(5) . . . . ? C24 C29 U1 C28 -126.5(7) . . . . ? C28 C29 U1 C24 126.5(7) . . . . ? C28 C29 U1 C8 -67.7(5) . . . . ? C24 C29 U1 C8 165.8(4) . . . . ? C28 C29 U1 C11 -151.0(4) . . . . ? C24 C29 U1 C11 82.5(5) . . . . ? C28 C29 U1 C27 31.5(4) . . . . ? C24 C29 U1 C27 -95.1(5) . . . . ? C28 C29 U1 C25 96.4(5) . . . . ? C24 C29 U1 C25 -30.1(4) . . . . ? C11 C10 U1 N2 -101.3(5) . . . . ? C9 C10 U1 N2 135.2(6) . . . . ? C14 C10 U1 N2 15.9(6) . . . . ? C11 C10 U1 N1 140.8(5) . . . . ? C9 C10 U1 N1 17.3(5) . . . . ? C14 C10 U1 N1 -102.0(6) . . . . ? C11 C10 U1 O1 66.3(5) . . . . ? C9 C10 U1 O1 -57.1(6) . . . . ? C14 C10 U1 O1 -176.4(6) . . . . ? C11 C10 U1 C9 123.5(8) . . . . ? C14 C10 U1 C9 -119.3(9) . . . . ? C11 C10 U1 C29 -136.6(5) . . . . ? C9 C10 U1 C29 100.0(5) . . . . ? C14 C10 U1 C29 -19.4(7) . . . . ? C11 C10 U1 C28 -166.0(5) . . . . ? C9 C10 U1 C28 70.6(6) . . . . ? C14 C10 U1 C28 -48.8(7) . . . . ? C11 C10 U1 C24 -104.9(5) . . . . ? C9 C10 U1 C24 131.6(5) . . . . ? C14 C10 U1 C24 12.3(7) . . . . ? C11 C10 U1 C8 93.0(6) . . . . ? C9 C10 U1 C8 -30.5(5) . . . . ? C14 C10 U1 C8 -149.8(7) . . . . ? C9 C10 U1 C11 -123.5(8) . . . . ? C14 C10 U1 C11 117.2(8) . . . . ? C11 C10 U1 C27 178.0(5) . . . . ? C9 C10 U1 C27 54.6(8) . . . . ? C14 C10 U1 C27 -64.7(8) . . . . ? C11 C10 U1 C25 -82.7(6) . . . . ? C9 C10 U1 C25 153.8(5) . . . . ? C14 C10 U1 C25 34.5(8) . . . . ? C29 C28 U1 N2 18.8(4) . . . . ? C27 C28 U1 N2 141.5(4) . . . . ? C30 C28 U1 N2 -101.6(5) . . . . ? C29 C28 U1 N1 137.3(5) . . . . ? C27 C28 U1 N1 -100.0(5) . . . . ? C30 C28 U1 N1 16.9(4) . . . . ? C29 C28 U1 O1 -150.6(4) . . . . ? C27 C28 U1 O1 -27.9(4) . . . . ? C30 C28 U1 O1 89.0(5) . . . . ? C29 C28 U1 C9 101.3(5) . . . . ? C27 C28 U1 C9 -136.0(4) . . . . ? C30 C28 U1 C9 -19.1(6) . . . . ? C27 C28 U1 C29 122.7(7) . . . . ? C30 C28 U1 C29 -120.4(7) . . . . ? C29 C28 U1 C10 71.7(5) . . . . ? C27 C28 U1 C10 -165.5(4) . . . . ? C30 C28 U1 C10 -48.7(6) . . . . ? C29 C28 U1 C24 -29.9(4) . . . . ? C27 C28 U1 C24 92.9(5) . . . . ? C30 C28 U1 C24 -150.2(6) . . . . ? C29 C28 U1 C8 132.1(4) . . . . ? C27 C28 U1 C8 -105.1(4) . . . . ? C30 C28 U1 C8 11.7(6) . . . . ? C29 C28 U1 C11 56.3(7) . . . . ? C27 C28 U1 C11 179.1(5) . . . . ? C30 C28 U1 C11 -64.1(8) . . . . ? C29 C28 U1 C27 -122.7(7) . . . . ? C30 C28 U1 C27 116.9(7) . . . . ? C29 C28 U1 C25 -62.0(4) . . . . ? C27 C28 U1 C25 60.7(4) . . . . ? C30 C28 U1 C25 177.6(6) . . . . ? C25 C24 U1 N2 145.3(5) . . . . ? C29 C24 U1 N2 -91.3(5) . . . . ? C21 C24 U1 N2 22.2(5) . . . . ? C25 C24 U1 N1 -106.0(5) . . . . ? C29 C24 U1 N1 17.3(5) . . . . ? C21 C24 U1 N1 130.8(5) . . . . ? C25 C24 U1 O1 -22.8(5) . . . . ? C29 C24 U1 O1 100.6(5) . . . . ? C21 C24 U1 O1 -145.9(5) . . . . ? C25 C24 U1 C9 -179.8(4) . . . . ? C29 C24 U1 C9 -56.4(6) . . . . ? C21 C24 U1 C9 57.1(6) . . . . ? C25 C24 U1 C29 -123.4(7) . . . . ? C21 C24 U1 C29 113.5(7) . . . . ? C25 C24 U1 C10 149.0(4) . . . . ? C29 C24 U1 C10 -87.6(5) . . . . ? C21 C24 U1 C10 25.9(6) . . . . ? C25 C24 U1 C28 -94.0(5) . . . . ? C29 C24 U1 C28 29.3(4) . . . . ? C21 C24 U1 C28 142.8(6) . . . . ? C25 C24 U1 C8 -158.4(7) . . . . ? C29 C24 U1 C8 -35.1(10) . . . . ? C21 C24 U1 C8 78.4(9) . . . . ? C25 C24 U1 C11 116.5(5) . . . . ? C29 C24 U1 C11 -120.2(5) . . . . ? C21 C24 U1 C11 -6.7(6) . . . . ? C25 C24 U1 C27 -60.4(4) . . . . ? C29 C24 U1 C27 63.0(4) . . . . ? C21 C24 U1 C27 176.5(6) . . . . ? C29 C24 U1 C25 123.4(7) . . . . ? C21 C24 U1 C25 -123.1(8) . . . . ? C13 C8 U1 N2 -107.8(5) . . . . ? C9 C8 U1 N2 17.8(5) . . . . ? C5 C8 U1 N2 131.2(5) . . . . ? C13 C8 U1 N1 143.4(5) . . . . ? C9 C8 U1 N1 -91.0(5) . . . . ? C5 C8 U1 N1 22.4(4) . . . . ? C13 C8 U1 O1 62.6(5) . . . . ? C9 C8 U1 O1 -171.8(5) . . . . ? C5 C8 U1 O1 -58.4(5) . . . . ? C13 C8 U1 C9 -125.6(8) . . . . ? C5 C8 U1 C9 113.4(7) . . . . ? C13 C8 U1 C29 178.8(4) . . . . ? C9 C8 U1 C29 -55.6(6) . . . . ? C5 C8 U1 C29 57.7(6) . . . . ? C13 C8 U1 C10 -94.5(6) . . . . ? C9 C8 U1 C10 31.1(5) . . . . ? C5 C8 U1 C10 144.5(6) . . . . ? C13 C8 U1 C28 148.6(5) . . . . ? C9 C8 U1 C28 -85.8(5) . . . . ? C5 C8 U1 C28 27.5(6) . . . . ? C13 C8 U1 C24 -157.9(7) . . . . ? C9 C8 U1 C24 -32.3(10) . . . . ? C5 C8 U1 C24 81.1(9) . . . . ? C13 C8 U1 C11 -60.9(5) . . . . ? C9 C8 U1 C11 64.7(5) . . . . ? C5 C8 U1 C11 178.1(6) . . . . ? C13 C8 U1 C27 115.9(5) . . . . ? C9 C8 U1 C27 -118.5(5) . . . . ? C5 C8 U1 C27 -5.1(6) . . . . ? C13 C8 U1 C25 73.0(12) . . . . ? C9 C8 U1 C25 -161.4(9) . . . . ? C5 C8 U1 C25 -48.0(12) . . . . ? C12 C11 U1 N2 -167.5(6) . . . . ? C10 C11 U1 N2 67.0(5) . . . . ? C12 C11 U1 N1 82.6(5) . . . . ? C10 C11 U1 N1 -43.0(6) . . . . ? C12 C11 U1 O1 0.6(5) . . . . ? C10 C11 U1 O1 -124.9(5) . . . . ? C12 C11 U1 C9 93.8(5) . . . . ? C10 C11 U1 C9 -31.7(5) . . . . ? C12 C11 U1 C29 -175.4(4) . . . . ? C10 C11 U1 C29 59.1(6) . . . . ? C12 C11 U1 C10 125.6(8) . . . . ? C12 C11 U1 C28 152.2(5) . . . . ? C10 C11 U1 C28 26.6(8) . . . . ? C12 C11 U1 C24 -140.9(5) . . . . ? C10 C11 U1 C24 93.6(5) . . . . ? C12 C11 U1 C8 59.8(5) . . . . ? C10 C11 U1 C8 -65.8(5) . . . . ? C12 C11 U1 C27 -37(5) . . . . ? C10 C11 U1 C27 -162(4) . . . . ? C12 C11 U1 C25 -108.5(5) . . . . ? C10 C11 U1 C25 126.0(5) . . . . ? C26 C27 U1 N2 85.1(5) . . . . ? C28 C27 U1 N2 -42.0(5) . . . . ? C26 C27 U1 N1 -165.0(5) . . . . ? C28 C27 U1 N1 67.8(4) . . . . ? C26 C27 U1 O1 -82.8(5) . . . . ? C28 C27 U1 O1 150.1(5) . . . . ? C26 C27 U1 C9 -173.4(4) . . . . ? C28 C27 U1 C9 59.4(5) . . . . ? C26 C27 U1 C29 95.5(5) . . . . ? C28 C27 U1 C29 -31.6(4) . . . . ? C26 C27 U1 C10 154.7(5) . . . . ? C28 C27 U1 C10 27.5(8) . . . . ? C26 C27 U1 C28 127.1(7) . . . . ? C26 C27 U1 C24 61.1(5) . . . . ? C28 C27 U1 C24 -66.0(4) . . . . ? C26 C27 U1 C8 -139.4(4) . . . . ? C28 C27 U1 C8 93.4(5) . . . . ? C26 C27 U1 C11 -45(5) . . . . ? C28 C27 U1 C11 -172(4) . . . . ? C26 C27 U1 C25 29.3(4) . . . . ? C28 C27 U1 C25 -97.8(5) . . . . ? C24 C25 U1 N2 -30.0(5) . . . . ? C26 C25 U1 N2 -158.2(5) . . . . ? C24 C25 U1 N1 84.4(5) . . . . ? C26 C25 U1 N1 -43.7(5) . . . . ? C24 C25 U1 O1 159.4(5) . . . . ? C26 C25 U1 O1 31.2(4) . . . . ? C24 C25 U1 C9 0.5(10) . . . . ? C26 C25 U1 C9 -127.7(7) . . . . ? C24 C25 U1 C29 32.2(4) . . . . ? C26 C25 U1 C29 -96.0(5) . . . . ? C24 C25 U1 C10 -46.5(6) . . . . ? C26 C25 U1 C10 -174.7(4) . . . . ? C24 C25 U1 C28 65.8(5) . . . . ? C26 C25 U1 C28 -62.4(4) . . . . ? C26 C25 U1 C24 -128.2(7) . . . . ? C24 C25 U1 C8 149.2(9) . . . . ? C26 C25 U1 C8 21.0(12) . . . . ? C24 C25 U1 C11 -84.3(5) . . . . ? C26 C25 U1 C11 147.5(4) . . . . ? C24 C25 U1 C27 99.2(5) . . . . ? C26 C25 U1 C27 -29.0(4) . . . . ? C44 O3 C41 C42 9(3) . . . . ? C43 C42 C41 O3 -2(3) . . . . ? C41 C42 C43 C44 -4(3) . . . . ? C41 O3 C44 C43 -12(3) . . . . ? C42 C43 C44 O3 10(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.953 _refine_diff_density_min -2.637 _refine_diff_density_rms 0.179 _database_code_depnum_ccdc_archive 'CCDC 951388' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p12091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 I N2 U' _chemical_formula_sum 'C32 H36 I N2 U' _chemical_formula_weight 813.56 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' I I -0.4742 1.8119 '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 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 56.620(2) _cell_length_b 15.9509(5) _cell_length_c 24.5801(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.031(5) _cell_angle_gamma 90.00 _cell_volume 20114.2(13) _cell_formula_units_Z 28 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 14935 _cell_measurement_theta_min 2.8924 _cell_measurement_theta_max 27.4239 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.2962 _exptl_crystal_size_mid 0.2062 _exptl_crystal_size_min 0.1247 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10836 _exptl_absorpt_coefficient_mu 6.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.953 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116453 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -73 _diffrn_reflns_limit_h_max 73 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.48 _reflns_number_total 23044 _reflns_number_gt 11955 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+476.6965P] 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 23044 _refine_ls_number_parameters 1136 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3614(3) 0.9517(9) 0.7030(7) 0.026(3) Uani 1 1 d . . . C2 C 0.3744(3) 0.8947(9) 0.6844(8) 0.029(3) Uani 1 1 d . . . H2 H 0.3705 0.8794 0.6441 0.035 Uiso 1 1 calc R . . C3 C 0.3948(3) 0.8633(9) 0.7368(8) 0.030(4) Uani 1 1 d . . . H3 H 0.4070 0.8218 0.7379 0.037 Uiso 1 1 calc R . . C4 C 0.3942(3) 0.9018(8) 0.7859(8) 0.026(3) Uani 1 1 d . . . C5 C 0.4106(3) 0.8864(8) 0.8517(8) 0.027(3) Uani 1 1 d . . . C6 C 0.4023(3) 0.8024(9) 0.8690(8) 0.033(4) Uani 1 1 d . . . H6A H 0.4049 0.7572 0.8452 0.049 Uiso 1 1 calc R . . H6B H 0.3838 0.8050 0.8610 0.049 Uiso 1 1 calc R . . H6C H 0.4127 0.7914 0.9118 0.049 Uiso 1 1 calc R . . C7 C 0.4397(3) 0.8789(9) 0.8635(8) 0.031(4) Uani 1 1 d . . . H7A H 0.4419 0.8311 0.8410 0.047 Uiso 1 1 calc R . . H7B H 0.4503 0.8704 0.9065 0.047 Uiso 1 1 calc R . . H7C H 0.4452 0.9304 0.8504 0.047 Uiso 1 1 calc R . . C8 C 0.4072(3) 0.9593(8) 0.8861(7) 0.023(3) Uani 1 1 d U . . C9 C 0.3958(3) 0.9539(8) 0.9257(6) 0.020(3) Uani 1 1 d . . . H9 H 0.3912 0.9003 0.9350 0.024 Uiso 1 1 calc R . . C10 C 0.3906(3) 1.0260(9) 0.9532(7) 0.025(3) Uani 1 1 d . . . C11 C 0.3988(3) 1.1036(9) 0.9419(7) 0.027(3) Uani 1 1 d . . . H11 H 0.3962 1.1522 0.9609 0.032 Uiso 1 1 calc R . . C12 C 0.4109(3) 1.1108(9) 0.9030(8) 0.030(3) Uani 1 1 d . . . H12 H 0.4166 1.1642 0.8962 0.036 Uiso 1 1 calc R . . C13 C 0.4146(3) 1.0402(8) 0.8738(7) 0.024(3) Uani 1 1 d . . . H13 H 0.4221 1.0461 0.8460 0.029 Uiso 1 1 calc R . . C14 C 0.3751(3) 1.0142(11) 0.9902(7) 0.032(4) Uani 1 1 d . . . C15 C 0.3926(4) 0.9710(12) 1.0499(7) 0.042(4) Uani 1 1 d . . . H15A H 0.4077 1.0069 1.0726 0.063 Uiso 1 1 calc R . . H15B H 0.3987 0.9171 1.0416 0.063 Uiso 1 1 calc R . . H15C H 0.3826 0.9617 1.0736 0.063 Uiso 1 1 calc R . . C16 C 0.3660(4) 1.0980(11) 1.0048(8) 0.044(5) Uani 1 1 d . . . H16A H 0.3812 1.1328 1.0282 0.065 Uiso 1 1 calc R . . H16B H 0.3559 1.0879 1.0282 0.065 Uiso 1 1 calc R . . H16C H 0.3551 1.1269 0.9674 0.065 Uiso 1 1 calc R . . C17 C 0.3519(3) 0.9605(9) 0.9544(7) 0.027(3) Uani 1 1 d . . . C18 C 0.3384(3) 0.9063(9) 0.9742(7) 0.029(3) Uani 1 1 d . . . H18 H 0.3420 0.8949 1.0150 0.035 Uiso 1 1 calc R . . C19 C 0.3182(3) 0.8708(9) 0.9238(8) 0.031(4) Uani 1 1 d . . . H19 H 0.3057 0.8312 0.9240 0.037 Uiso 1 1 calc R . . C20 C 0.3199(3) 0.9039(9) 0.8739(7) 0.026(3) Uani 1 1 d . . . C21 C 0.3038(3) 0.8811(9) 0.8079(8) 0.029(3) Uani 1 1 d . . . C22 C 0.2750(4) 0.8668(12) 0.7949(9) 0.047(5) Uani 1 1 d . . . H22A H 0.2737 0.8202 0.8194 0.070 Uiso 1 1 calc R . . H22B H 0.2651 0.8535 0.7523 0.070 Uiso 1 1 calc R . . H22C H 0.2680 0.9178 0.8047 0.070 Uiso 1 1 calc R . . C23 C 0.3154(3) 0.7980(9) 0.7962(8) 0.036(4) Uani 1 1 d . . . H23A H 0.3136 0.7534 0.8216 0.055 Uiso 1 1 calc R . . H23B H 0.3339 0.8063 0.8056 0.055 Uiso 1 1 calc R . . H23C H 0.3060 0.7821 0.7539 0.055 Uiso 1 1 calc R . . C24 C 0.3058(3) 0.9534(8) 0.7700(7) 0.025(3) Uani 1 1 d . . . C25 C 0.3175(3) 0.9477(9) 0.7309(7) 0.026(3) Uani 1 1 d . . . H25 H 0.3225 0.8940 0.7228 0.031 Uiso 1 1 calc R . . C26 C 0.3223(3) 1.0175(10) 0.7028(7) 0.028(3) Uani 1 1 d . . . C27 C 0.3130(3) 1.0956(9) 0.7105(8) 0.031(4) Uani 1 1 d . . . H27 H 0.3154 1.1437 0.6905 0.037 Uiso 1 1 calc R . . C28 C 0.2999(3) 1.1026(9) 0.7484(7) 0.031(3) Uani 1 1 d . . . H28 H 0.2929 1.1551 0.7527 0.037 Uiso 1 1 calc R . . C29 C 0.2974(3) 1.0341(9) 0.7788(7) 0.027(3) Uani 1 1 d . . . H29 H 0.2898 1.0405 0.8064 0.033 Uiso 1 1 calc R . . C30 C 0.3382(3) 1.0040(10) 0.6664(7) 0.032(4) Uani 1 1 d . . . C31 C 0.3208(4) 0.9638(12) 0.6064(7) 0.044(5) Uani 1 1 d . . . H31A H 0.3060 1.0009 0.5844 0.066 Uiso 1 1 calc R . . H31B H 0.3143 0.9098 0.6136 0.066 Uiso 1 1 calc R . . H31C H 0.3308 0.9549 0.5827 0.066 Uiso 1 1 calc R . . C32 C 0.3480(4) 1.0897(10) 0.6526(8) 0.040(4) Uani 1 1 d . . . H32A H 0.3330 1.1247 0.6284 0.060 Uiso 1 1 calc R . . H32B H 0.3586 1.0796 0.6304 0.060 Uiso 1 1 calc R . . H32C H 0.3586 1.1185 0.6904 0.060 Uiso 1 1 calc R . . C33 C 0.2514(3) 0.8869(8) 0.3580(6) 0.022(3) Uani 1 1 d . . . C34 C 0.2529(3) 0.8474(8) 0.3097(8) 0.027(3) Uani 1 1 d . . . H34 H 0.2656 0.8074 0.3110 0.033 Uiso 1 1 calc R . . C35 C 0.2321(3) 0.8782(9) 0.2583(8) 0.030(3) Uani 1 1 d . . . H35 H 0.2280 0.8630 0.2179 0.036 Uiso 1 1 calc R . . C36 C 0.2187(3) 0.9348(10) 0.2772(7) 0.029(3) Uani 1 1 d . . . C37 C 0.1951(3) 0.9878(10) 0.2388(7) 0.033(4) Uani 1 1 d . . . C38 C 0.1779(3) 0.9442(12) 0.1796(7) 0.042(4) Uani 1 1 d . . . H38A H 0.1630 0.9802 0.1562 0.062 Uiso 1 1 calc R . . H38B H 0.1716 0.8908 0.1881 0.062 Uiso 1 1 calc R . . H38C H 0.1881 0.9337 0.1565 0.062 Uiso 1 1 calc R . . C39 C 0.2041(4) 1.0717(12) 0.2243(8) 0.046(5) Uani 1 1 d . . . H39A H 0.1889 1.1055 0.1995 0.069 Uiso 1 1 calc R . . H39B H 0.2149 1.0618 0.2025 0.069 Uiso 1 1 calc R . . H39C H 0.2144 1.1017 0.2618 0.069 Uiso 1 1 calc R . . C40 C 0.1788(3) 1.0010(9) 0.2751(7) 0.024(3) Uani 1 1 d . . . C41 C 0.1745(3) 0.9285(9) 0.3042(7) 0.026(3) Uani 1 1 d . . . H41 H 0.1797 0.8751 0.2962 0.032 Uiso 1 1 calc R . . C42 C 0.1628(3) 0.9341(9) 0.3443(7) 0.026(3) Uani 1 1 d . . . C43 C 0.1542(3) 1.0152(9) 0.3527(7) 0.027(3) Uani 1 1 d . . . H43 H 0.1469 1.0223 0.3808 0.032 Uiso 1 1 calc R . . C44 C 0.1564(3) 1.0835(9) 0.3207(7) 0.032(4) Uani 1 1 d . . . H44 H 0.1490 1.1355 0.3241 0.038 Uiso 1 1 calc R . . C45 C 0.1695(3) 1.0778(10) 0.2832(7) 0.030(3) Uani 1 1 d . . . H45 H 0.1718 1.1264 0.2636 0.036 Uiso 1 1 calc R . . C46 C 0.1611(3) 0.8624(10) 0.3827(8) 0.032(4) Uani 1 1 d . . . C47 C 0.1727(4) 0.7815(10) 0.3699(8) 0.045(5) Uani 1 1 d . . . H47A H 0.1630 0.7656 0.3277 0.068 Uiso 1 1 calc R . . H47B H 0.1716 0.7363 0.3957 0.068 Uiso 1 1 calc R . . H47C H 0.1910 0.7911 0.3781 0.068 Uiso 1 1 calc R . . C48 C 0.1319(4) 0.8473(13) 0.3675(9) 0.048(5) Uani 1 1 d . . . H48A H 0.1227 0.8313 0.3252 0.071 Uiso 1 1 calc R . . H48B H 0.1243 0.8988 0.3748 0.071 Uiso 1 1 calc R . . H48C H 0.1304 0.8022 0.3929 0.071 Uiso 1 1 calc R . . C49 C 0.1761(4) 0.8870(9) 0.4476(8) 0.030(4) Uani 1 1 d . . . C50 C 0.1739(4) 0.8554(10) 0.4963(8) 0.034(4) Uani 1 1 d . . . H50 H 0.1610 0.8170 0.4961 0.041 Uiso 1 1 calc R . . C51 C 0.1943(3) 0.8902(10) 0.5476(7) 0.031(3) Uani 1 1 d . . . H51 H 0.1977 0.8796 0.5882 0.037 Uiso 1 1 calc R . . C52 C 0.2083(3) 0.9416(10) 0.5280(7) 0.031(3) Uani 1 1 d . . . C53 C 0.2316(4) 0.9952(11) 0.5637(8) 0.038(4) Uani 1 1 d . . . C54 C 0.2227(4) 1.0813(13) 0.5793(9) 0.052(5) Uani 1 1 d . . . H54A H 0.2381 1.1155 0.6025 0.078 Uiso 1 1 calc R . . H54B H 0.2128 1.0717 0.6030 0.078 Uiso 1 1 calc R . . H54C H 0.2118 1.1107 0.5421 0.078 Uiso 1 1 calc R . . C55 C 0.2494(4) 0.9509(13) 0.6222(7) 0.047(5) Uani 1 1 d . . . H55A H 0.2645 0.9867 0.6448 0.071 Uiso 1 1 calc R . . H55B H 0.2555 0.8977 0.6127 0.071 Uiso 1 1 calc R . . H55C H 0.2397 0.9401 0.6463 0.071 Uiso 1 1 calc R . . C56 C 0.2475(3) 1.0074(10) 0.5275(7) 0.030(3) Uani 1 1 d . . . C57 C 0.2545(3) 1.0869(11) 0.5154(8) 0.036(4) Uani 1 1 d . . . H57 H 0.2507 1.1354 0.5327 0.043 Uiso 1 1 calc R . . C58 C 0.2673(3) 1.0939(9) 0.4767(8) 0.030(3) Uani 1 1 d . . . H58 H 0.2730 1.1473 0.4700 0.036 Uiso 1 1 calc R . . C59 C 0.2716(4) 1.0243(9) 0.4490(8) 0.031(4) Uani 1 1 d . . . H59 H 0.2794 1.0309 0.4219 0.038 Uiso 1 1 calc R . . C60 C 0.2646(3) 0.9440(9) 0.4600(7) 0.024(3) Uani 1 1 d . . . C61 C 0.2531(3) 0.9369(10) 0.4999(7) 0.031(3) Uani 1 1 d . . . H61 H 0.2489 0.8826 0.5091 0.037 Uiso 1 1 calc R . . C62 C 0.2684(3) 0.8704(9) 0.4246(7) 0.027(3) Uani 1 1 d . . . C63 C 0.2607(4) 0.7870(9) 0.4418(8) 0.036(4) Uani 1 1 d . . . H63A H 0.2635 0.7423 0.4178 0.054 Uiso 1 1 calc R . . H63B H 0.2423 0.7886 0.4343 0.054 Uiso 1 1 calc R . . H63C H 0.2714 0.7763 0.4846 0.054 Uiso 1 1 calc R . . C64 C 0.2973(3) 0.8652(10) 0.4365(8) 0.035(4) Uani 1 1 d . . . H64A H 0.2999 0.8181 0.4139 0.052 Uiso 1 1 calc R . . H64B H 0.3080 0.8567 0.4795 0.052 Uiso 1 1 calc R . . H64C H 0.3025 0.9175 0.4237 0.052 Uiso 1 1 calc R . . C65 C 0.1095(3) 0.1247(9) 0.4250(7) 0.027(3) Uani 1 1 d . . . C66 C 0.1118(4) 0.1606(10) 0.3769(8) 0.034(4) Uani 1 1 d . . . H66 H 0.1250 0.1985 0.3783 0.041 Uiso 1 1 calc R . . C67 C 0.0904(4) 0.1299(9) 0.3240(8) 0.032(4) Uani 1 1 d . . . H67 H 0.0865 0.1439 0.2836 0.039 Uiso 1 1 calc R . . C68 C 0.0766(3) 0.0766(9) 0.3433(7) 0.026(3) Uani 1 1 d . . . C69 C 0.0528(3) 0.0248(9) 0.3056(8) 0.031(3) Uani 1 1 d . . . C70 C 0.0620(4) -0.0600(11) 0.2909(9) 0.047(5) Uani 1 1 d . . . H70A H 0.0722 -0.0500 0.2677 0.070 Uiso 1 1 calc R . . H70B H 0.0468 -0.0946 0.2673 0.070 Uiso 1 1 calc R . . H70C H 0.0728 -0.0891 0.3283 0.070 Uiso 1 1 calc R . . C71 C 0.0357(4) 0.0687(12) 0.2474(8) 0.040(4) Uani 1 1 d . . . H71A H 0.0456 0.0772 0.2234 0.060 Uiso 1 1 calc R . . H71B H 0.0301 0.1231 0.2563 0.060 Uiso 1 1 calc R . . H71C H 0.0203 0.0341 0.2248 0.060 Uiso 1 1 calc R . . C72 C 0.0371(3) 0.0126(9) 0.3413(7) 0.026(3) Uani 1 1 d . . . C73 C 0.0319(3) 0.0830(9) 0.3698(7) 0.026(3) Uani 1 1 d . . . H73 H 0.0366 0.1375 0.3620 0.031 Uiso 1 1 calc R . . C74 C 0.0201(3) 0.0740(9) 0.4084(7) 0.027(3) Uani 1 1 d . . . C75 C 0.0116(3) -0.0038(9) 0.4184(7) 0.030(3) Uani 1 1 d . . . H75 H 0.0037 -0.0099 0.4454 0.036 Uiso 1 1 calc R . . C76 C 0.0151(4) -0.0732(9) 0.3872(8) 0.036(4) Uani 1 1 d . . . H76 H 0.0081 -0.1261 0.3906 0.044 Uiso 1 1 calc R . . C77 C 0.0285(3) -0.0662(10) 0.3516(8) 0.035(4) Uani 1 1 d . . . H77 H 0.0319 -0.1149 0.3338 0.042 Uiso 1 1 calc R . . C78 C 0.0176(3) 0.1486(9) 0.4466(8) 0.029(3) Uani 1 1 d . . . C79 C -0.0116(4) 0.1606(11) 0.4331(9) 0.041(4) Uani 1 1 d . . . H79A H -0.0215 0.1754 0.3908 0.062 Uiso 1 1 calc R . . H79B H -0.0133 0.2056 0.4584 0.062 Uiso 1 1 calc R . . H79C H -0.0185 0.1083 0.4417 0.062 Uiso 1 1 calc R . . C80 C 0.0281(4) 0.2308(9) 0.4332(9) 0.042(4) Uani 1 1 d . . . H80A H 0.0182 0.2455 0.3909 0.063 Uiso 1 1 calc R . . H80B H 0.0465 0.2238 0.4417 0.063 Uiso 1 1 calc R . . H80C H 0.0263 0.2756 0.4585 0.063 Uiso 1 1 calc R . . C81 C 0.0327(3) 0.1261(9) 0.5116(7) 0.026(3) Uani 1 1 d . . . C82 C 0.0306(4) 0.1590(9) 0.5614(8) 0.033(4) Uani 1 1 d . . . H82 H 0.0175 0.1969 0.5607 0.040 Uiso 1 1 calc R . . C83 C 0.0510(3) 0.1271(10) 0.6128(8) 0.036(4) Uani 1 1 d . . . H83 H 0.0542 0.1391 0.6532 0.043 Uiso 1 1 calc R . . C84 C 0.0655(3) 0.0749(9) 0.5942(7) 0.030(3) Uani 1 1 d . . . C85 C 0.0892(3) 0.0215(10) 0.6315(7) 0.028(3) Uani 1 1 d . . . C86 C 0.0801(4) -0.0621(10) 0.6482(8) 0.039(4) Uani 1 1 d . . . H86A H 0.0953 -0.0965 0.6722 0.058 Uiso 1 1 calc R . . H86B H 0.0691 -0.0924 0.6115 0.058 Uiso 1 1 calc R . . H86C H 0.0701 -0.0505 0.6717 0.058 Uiso 1 1 calc R . . C87 C 0.1066(4) 0.0665(11) 0.6906(8) 0.039(4) Uani 1 1 d . . . H87A H 0.1217 0.0312 0.7138 0.059 Uiso 1 1 calc R . . H87B H 0.0966 0.0767 0.7140 0.059 Uiso 1 1 calc R . . H87C H 0.1126 0.1201 0.6814 0.059 Uiso 1 1 calc R . . C88 C 0.1047(3) 0.0070(9) 0.5939(7) 0.029(3) Uani 1 1 d . . . C89 C 0.1107(3) 0.0781(9) 0.5675(6) 0.023(3) Uani 1 1 d . . . H89 H 0.1068 0.1323 0.5774 0.028 Uiso 1 1 calc R . . C90 C 0.1222(3) 0.0709(10) 0.5272(7) 0.030(3) Uani 1 1 d . . . C91 C 0.1297(3) -0.0105(10) 0.5174(8) 0.034(4) Uani 1 1 d . . . H91 H 0.1379 -0.0179 0.4911 0.041 Uiso 1 1 calc R . . C92 C 0.1251(3) -0.0786(10) 0.5457(8) 0.036(4) Uani 1 1 d . . . H92 H 0.1303 -0.1326 0.5388 0.044 Uiso 1 1 calc R . . C93 C 0.1128(3) -0.0712(10) 0.5846(7) 0.033(3) Uani 1 1 d . . . H93 H 0.1102 -0.1191 0.6042 0.039 Uiso 1 1 calc R . . C94 C 0.1261(3) 0.1432(8) 0.4923(8) 0.027(3) Uani 1 1 d . . . C95 C 0.1172(4) 0.2281(9) 0.5080(8) 0.038(4) Uani 1 1 d . . . H95A H 0.1202 0.2729 0.4844 0.057 Uiso 1 1 calc R . . H95B H 0.1272 0.2397 0.5509 0.057 Uiso 1 1 calc R . . H95C H 0.0986 0.2252 0.4986 0.057 Uiso 1 1 calc R . . C96 C 0.1550(4) 0.1503(11) 0.5056(9) 0.042(4) Uani 1 1 d . . . H96A H 0.1575 0.1973 0.4829 0.063 Uiso 1 1 calc R . . H96B H 0.1608 0.0982 0.4939 0.063 Uiso 1 1 calc R . . H96C H 0.1653 0.1599 0.5487 0.063 Uiso 1 1 calc R . . C97 C -0.0052(3) 0.4638(8) 0.3742(7) 0.024(3) Uani 1 1 d . . . C98 C -0.0178(4) 0.4065(10) 0.3941(8) 0.034(4) Uani 1 1 d . . . H98 H -0.0137 0.3934 0.4348 0.041 Uiso 1 1 calc R . . C99 C -0.0380(3) 0.3705(9) 0.3432(7) 0.027(3) Uani 1 1 d . . . H99 H -0.0498 0.3280 0.3428 0.032 Uiso 1 1 calc R . . C100 C 0.0370(3) 0.4104(8) 0.2067(7) 0.020(3) Uani 1 1 d . . . C101 C 0.0528(3) 0.3912(9) 0.2719(7) 0.027(3) Uani 1 1 d . . . C102 C 0.0434(4) 0.3101(9) 0.2888(9) 0.042(4) Uani 1 1 d . . . H10A H 0.0539 0.2982 0.3314 0.063 Uiso 1 1 calc R . . H10B H 0.0452 0.2640 0.2645 0.063 Uiso 1 1 calc R . . H10C H 0.0251 0.3161 0.2814 0.063 Uiso 1 1 calc R . . C103 C 0.0820(3) 0.3775(11) 0.2851(9) 0.040(4) Uani 1 1 d . . . H10D H 0.0920 0.3647 0.3278 0.060 Uiso 1 1 calc R . . H10E H 0.0889 0.4285 0.2749 0.060 Uiso 1 1 calc R . . H10F H 0.0835 0.3306 0.2608 0.060 Uiso 1 1 calc R . . C104 C 0.0505(3) 0.4654(8) 0.3078(6) 0.020(3) Uani 1 1 d . . . C105 C 0.0585(3) 0.5454(9) 0.2967(8) 0.031(4) Uani 1 1 d . . . H105 H 0.0662 0.5516 0.2694 0.037 Uiso 1 1 calc R . . C106 C 0.0549(3) 0.6133(9) 0.3262(7) 0.030(4) Uani 1 1 d . . . H106 H 0.0610 0.6664 0.3199 0.036 Uiso 1 1 calc R . . C107 C 0.0429(3) 0.6081(9) 0.3648(7) 0.030(3) Uani 1 1 d . . . H107 H 0.0408 0.6572 0.3840 0.036 Uiso 1 1 calc R . . C108 C 0.0340(3) 0.5316(9) 0.3756(7) 0.023(3) Uani 1 1 d . . . C109 C 0.0395(3) 0.4589(9) 0.3487(7) 0.025(3) Uani 1 1 d . . . H109 H 0.0355 0.4050 0.3590 0.031 Uiso 1 1 calc R . . C110 C 0.0181(3) 0.5192(9) 0.4116(7) 0.029(3) Uani 1 1 d . . . C111 C 0.0093(4) 0.6048(9) 0.4252(8) 0.036(4) Uani 1 1 d . . . H11A H -0.0010 0.5966 0.4485 0.054 Uiso 1 1 calc R . . H11B H -0.0015 0.6333 0.3874 0.054 Uiso 1 1 calc R . . H11C H 0.0246 0.6392 0.4483 0.054 Uiso 1 1 calc R . . C112 C 0.0354(3) 0.4761(11) 0.4716(8) 0.036(4) Uani 1 1 d . . . H11D H 0.0253 0.4680 0.4953 0.054 Uiso 1 1 calc R . . H11E H 0.0506 0.5114 0.4941 0.054 Uiso 1 1 calc R . . H11F H 0.0412 0.4216 0.4635 0.054 Uiso 1 1 calc R . . N1 N 0.3733(2) 0.9586(7) 0.7655(5) 0.022(3) Uani 1 1 d . . . N2 N 0.3408(3) 0.9594(7) 0.8911(6) 0.025(3) Uani 1 1 d . . . N3 N 0.2303(3) 0.9409(7) 0.3398(6) 0.026(3) Uani 1 1 d . . . N4 N 0.1969(3) 0.9412(8) 0.4648(6) 0.027(3) Uani 1 1 d . . . N5 N 0.0873(3) 0.0711(7) 0.4049(6) 0.025(3) Uani 1 1 d . . . N6 N 0.0545(3) 0.0721(7) 0.5310(6) 0.026(3) Uani 1 1 d . . . N7 N 0.0162(3) 0.4677(7) 0.1867(6) 0.024(3) Uani 1 1 d . . . I1 I 0.35417(3) 1.23286(8) 0.82696(7) 0.0760(5) Uani 1 1 d . . . I2 I 0.21024(3) 1.21528(7) 0.40078(8) 0.0696(4) Uani 1 1 d . . . I3 I 0.06948(4) -0.20084(6) 0.46862(9) 0.0798(5) Uani 1 1 d . . . I4 I 0.0000 0.74157(10) 0.2500 0.0794(7) Uani 1 2 d S . . U1 U 0.356266(10) 1.03795(3) 0.82746(2) 0.02433(14) Uani 1 1 d . . . U2 U 0.212984(12) 1.02035(3) 0.40088(3) 0.02403(13) Uani 1 1 d . . . U3 U 0.070794(14) -0.00622(3) 0.46819(3) 0.02326(11) Uani 1 1 d . . . U4 U 0.0000 0.54648(4) 0.2500 0.02164(17) Uani 1 2 d S . . 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 0.020(8) 0.036(7) 0.016(7) 0.001(5) 0.002(6) 0.003(6) C2 0.024(9) 0.035(7) 0.027(8) -0.006(6) 0.010(7) 0.001(6) C3 0.028(9) 0.036(7) 0.031(9) -0.008(6) 0.017(8) 0.001(6) C4 0.016(8) 0.023(6) 0.043(9) -0.001(6) 0.015(7) 0.002(5) C5 0.025(9) 0.020(6) 0.037(9) 0.005(6) 0.016(8) 0.005(5) C6 0.033(9) 0.036(8) 0.032(8) 0.007(6) 0.017(8) 0.009(6) C7 0.027(10) 0.035(7) 0.032(9) 0.000(6) 0.012(8) 0.005(6) C8 0.010(6) 0.028(6) 0.022(6) 0.004(5) -0.001(5) 0.005(4) C9 0.012(7) 0.022(6) 0.019(7) 0.005(5) 0.001(6) 0.007(5) C10 0.013(7) 0.031(7) 0.019(7) -0.001(5) -0.005(6) 0.000(5) C11 0.023(8) 0.033(7) 0.015(7) -0.004(5) 0.000(6) -0.003(6) C12 0.029(9) 0.024(7) 0.028(8) -0.007(6) 0.005(7) -0.005(6) C13 0.018(8) 0.027(6) 0.020(7) 0.003(5) -0.001(6) -0.008(5) C14 0.019(8) 0.057(9) 0.011(6) -0.011(6) -0.002(6) -0.002(7) C15 0.024(9) 0.070(11) 0.021(8) -0.010(7) -0.001(7) -0.005(8) C16 0.032(10) 0.062(11) 0.039(10) -0.029(8) 0.018(9) -0.010(8) C17 0.017(8) 0.045(8) 0.017(7) 0.004(6) 0.005(6) 0.007(6) C18 0.015(8) 0.046(8) 0.023(8) -0.002(6) 0.003(6) 0.004(6) C19 0.023(9) 0.036(7) 0.034(9) 0.000(6) 0.011(8) 0.008(6) C20 0.010(7) 0.038(7) 0.023(7) -0.007(6) 0.001(6) 0.003(5) C21 0.020(8) 0.031(7) 0.036(9) 0.002(6) 0.013(7) 0.004(6) C22 0.029(11) 0.077(12) 0.030(9) -0.013(8) 0.008(8) -0.015(9) C23 0.031(9) 0.036(8) 0.048(10) -0.005(7) 0.023(8) 0.004(6) C24 0.011(7) 0.030(7) 0.027(8) -0.002(6) 0.003(6) 0.004(5) C25 0.014(7) 0.033(7) 0.019(7) -0.007(5) -0.004(6) -0.001(5) C26 0.012(7) 0.051(9) 0.015(7) -0.013(6) -0.001(6) -0.007(6) C27 0.026(9) 0.032(7) 0.026(8) 0.003(6) 0.003(7) 0.012(6) C28 0.018(8) 0.035(8) 0.024(8) -0.007(6) -0.006(6) 0.005(6) C29 0.018(8) 0.036(7) 0.019(7) -0.002(6) 0.000(6) 0.007(6) C30 0.016(8) 0.054(9) 0.023(8) -0.007(7) 0.007(7) 0.004(6) C31 0.030(10) 0.082(12) 0.015(8) -0.014(7) 0.004(7) 0.004(8) C32 0.034(10) 0.050(9) 0.030(9) 0.011(7) 0.008(8) 0.010(7) C33 0.014(7) 0.036(7) 0.012(6) 0.002(5) 0.002(6) -0.004(5) C34 0.024(9) 0.024(6) 0.031(9) 0.000(6) 0.010(7) 0.005(6) C35 0.017(8) 0.045(8) 0.026(8) -0.008(6) 0.007(7) -0.004(6) C36 0.013(7) 0.049(8) 0.020(7) 0.000(6) 0.002(6) -0.001(6) C37 0.028(9) 0.052(9) 0.014(7) 0.005(6) 0.005(7) 0.007(7) C38 0.017(8) 0.080(12) 0.017(8) -0.003(7) -0.004(7) 0.008(8) C39 0.039(11) 0.068(11) 0.042(10) 0.021(9) 0.026(10) 0.005(9) C40 0.015(7) 0.034(7) 0.016(7) -0.003(5) -0.001(6) -0.001(6) C41 0.013(7) 0.042(8) 0.017(7) -0.008(6) 0.001(6) 0.003(6) C42 0.013(7) 0.037(7) 0.017(7) -0.002(6) -0.003(6) -0.002(6) C43 0.019(8) 0.036(7) 0.024(7) -0.004(6) 0.008(7) 0.009(6) C44 0.030(9) 0.032(7) 0.029(8) 0.004(6) 0.009(7) 0.015(6) C45 0.023(8) 0.044(8) 0.017(7) 0.001(6) 0.002(7) 0.006(6) C46 0.019(8) 0.050(9) 0.026(8) 0.000(6) 0.008(7) -0.007(6) C47 0.071(14) 0.035(8) 0.034(9) -0.009(7) 0.026(10) -0.011(8) C48 0.017(9) 0.087(13) 0.030(9) -0.002(8) 0.000(8) -0.022(8) C49 0.035(10) 0.033(7) 0.027(8) 0.001(6) 0.019(8) 0.003(6) C50 0.024(9) 0.053(9) 0.029(9) -0.001(7) 0.015(8) 0.001(7) C51 0.024(9) 0.052(9) 0.016(7) 0.011(6) 0.007(7) 0.004(6) C52 0.016(8) 0.047(8) 0.026(8) -0.004(6) 0.006(7) 0.008(6) C53 0.026(9) 0.067(11) 0.025(8) -0.001(7) 0.015(8) -0.002(8) C54 0.034(11) 0.086(13) 0.036(10) -0.016(9) 0.015(9) 0.003(9) C55 0.022(9) 0.103(15) 0.015(8) 0.001(8) 0.006(7) -0.001(9) C56 0.023(8) 0.048(9) 0.017(7) -0.007(6) 0.006(7) -0.005(6) C57 0.027(9) 0.050(9) 0.025(8) -0.012(7) 0.005(7) -0.011(7) C58 0.024(9) 0.031(7) 0.031(8) -0.005(6) 0.008(7) -0.013(6) C59 0.037(10) 0.034(7) 0.027(9) -0.003(6) 0.018(8) -0.001(7) C60 0.012(7) 0.034(7) 0.019(7) 0.002(5) 0.000(6) 0.005(5) C61 0.018(8) 0.046(8) 0.022(8) 0.006(6) 0.003(7) 0.004(6) C62 0.024(9) 0.033(7) 0.021(7) -0.002(6) 0.007(7) 0.005(6) C63 0.038(10) 0.029(7) 0.040(10) 0.004(6) 0.016(9) 0.003(6) C64 0.020(9) 0.052(9) 0.033(9) 0.007(7) 0.012(8) 0.004(7) C65 0.017(8) 0.032(7) 0.026(8) 0.000(6) 0.004(7) -0.005(6) C66 0.021(9) 0.057(9) 0.022(8) 0.002(7) 0.007(7) -0.003(7) C67 0.034(10) 0.043(8) 0.021(8) 0.003(6) 0.011(8) 0.003(7) C68 0.018(8) 0.031(7) 0.024(7) -0.006(6) 0.003(6) 0.004(6) C69 0.025(9) 0.030(7) 0.031(8) -0.012(6) 0.006(7) -0.006(6) C70 0.042(12) 0.050(10) 0.048(11) -0.018(8) 0.018(10) 0.000(8) C71 0.021(9) 0.066(10) 0.026(8) -0.006(8) 0.004(7) -0.012(8) C72 0.020(8) 0.030(7) 0.020(7) 0.001(6) 0.002(7) 0.003(6) C73 0.018(8) 0.026(6) 0.026(7) -0.002(6) 0.001(6) 0.003(5) C74 0.007(7) 0.036(7) 0.032(8) -0.004(6) 0.003(6) 0.005(6) C75 0.022(9) 0.036(8) 0.026(8) 0.005(6) 0.004(7) 0.006(6) C76 0.033(10) 0.027(7) 0.048(10) -0.007(7) 0.016(9) -0.007(7) C77 0.019(8) 0.032(7) 0.042(10) -0.013(7) 0.002(8) -0.008(6) C78 0.011(7) 0.042(8) 0.027(8) 0.004(6) 0.003(6) 0.012(6) C79 0.017(9) 0.055(10) 0.050(11) 0.002(8) 0.012(8) 0.012(7) C80 0.046(11) 0.026(7) 0.064(12) -0.001(7) 0.033(10) 0.014(7) C81 0.013(7) 0.032(7) 0.032(8) -0.003(6) 0.008(7) 0.002(5) C82 0.027(9) 0.034(7) 0.037(9) -0.007(6) 0.012(8) 0.002(6) C83 0.027(9) 0.053(9) 0.031(9) -0.006(7) 0.014(8) -0.001(7) C84 0.028(9) 0.034(7) 0.030(8) -0.007(6) 0.014(7) -0.007(6) C85 0.015(8) 0.048(8) 0.017(7) -0.004(6) 0.003(6) -0.001(6) C86 0.032(10) 0.043(8) 0.041(9) 0.004(7) 0.016(8) -0.007(7) C87 0.025(9) 0.059(10) 0.026(8) -0.013(7) 0.003(7) -0.005(7) C88 0.016(8) 0.042(8) 0.017(7) -0.009(6) -0.003(6) 0.001(6) C89 0.014(7) 0.028(6) 0.020(7) -0.007(5) 0.000(6) -0.001(5) C90 0.016(8) 0.041(8) 0.028(8) -0.007(6) 0.005(7) 0.009(6) C91 0.015(8) 0.051(9) 0.025(8) 0.003(7) -0.001(7) 0.015(7) C92 0.019(8) 0.043(8) 0.032(9) -0.008(7) -0.003(7) 0.014(7) C93 0.030(9) 0.035(8) 0.022(7) 0.005(6) 0.000(7) 0.004(6) C94 0.016(8) 0.032(7) 0.036(9) -0.011(6) 0.014(7) -0.002(5) C95 0.039(10) 0.039(8) 0.042(10) -0.012(7) 0.023(9) -0.002(7) C96 0.025(10) 0.066(11) 0.035(9) -0.017(8) 0.013(8) -0.012(8) C97 0.020(8) 0.027(6) 0.022(7) -0.002(5) 0.005(6) 0.002(5) C98 0.035(10) 0.046(8) 0.023(8) 0.005(6) 0.013(8) -0.003(7) C99 0.024(8) 0.031(7) 0.025(8) 0.005(6) 0.009(7) -0.001(6) C100 0.011(7) 0.021(6) 0.022(7) -0.004(5) 0.000(6) -0.004(5) C101 0.012(7) 0.043(8) 0.019(7) 0.005(6) 0.000(6) 0.004(6) C102 0.056(12) 0.030(8) 0.045(10) 0.008(7) 0.026(9) 0.007(7) C103 0.012(9) 0.060(10) 0.047(11) 0.000(8) 0.011(8) 0.008(7) C104 0.010(7) 0.027(6) 0.015(6) 0.009(5) -0.002(5) 0.003(5) C105 0.019(8) 0.044(8) 0.023(8) 0.003(6) 0.003(7) -0.006(6) C106 0.022(9) 0.039(8) 0.024(8) 0.000(6) 0.004(7) -0.015(6) C107 0.023(9) 0.035(7) 0.018(7) -0.005(6) -0.004(7) -0.009(6) C108 0.014(7) 0.033(7) 0.016(7) -0.003(5) 0.000(6) -0.001(5) C109 0.021(8) 0.030(7) 0.023(8) -0.001(6) 0.007(7) -0.001(6) C110 0.029(9) 0.036(7) 0.020(7) 0.000(6) 0.009(7) 0.006(6) C111 0.028(9) 0.037(8) 0.040(10) 0.000(7) 0.013(8) -0.004(6) C112 0.024(9) 0.052(9) 0.033(9) 0.014(7) 0.014(8) 0.008(7) N1 0.012(6) 0.041(6) 0.014(6) 0.006(5) 0.006(5) 0.012(5) N2 0.024(7) 0.034(6) 0.020(6) -0.003(5) 0.011(6) -0.008(5) N3 0.021(7) 0.034(6) 0.016(6) 0.003(5) 0.002(5) 0.001(5) N4 0.016(6) 0.044(7) 0.016(6) 0.003(5) 0.003(5) -0.006(5) N5 0.013(6) 0.037(6) 0.022(6) 0.000(5) 0.007(5) 0.003(5) N6 0.014(6) 0.033(6) 0.031(7) -0.002(5) 0.011(6) -0.004(5) N7 0.017(6) 0.025(5) 0.021(6) -0.005(4) -0.003(5) -0.007(5) I1 0.0769(12) 0.0292(6) 0.0654(10) -0.0045(5) -0.0246(8) 0.0069(5) I2 0.0642(10) 0.0325(6) 0.0642(9) -0.0013(6) -0.0191(7) 0.0029(6) I3 0.0744(9) 0.0243(5) 0.0752(8) -0.0023(6) -0.0320(6) 0.0019(6) I4 0.0804(16) 0.0217(7) 0.0698(14) 0.000 -0.0325(11) 0.000 U1 0.0173(3) 0.0320(3) 0.0182(3) -0.00337(18) 0.0021(2) 0.00190(18) U2 0.0165(3) 0.0354(3) 0.0164(3) -0.0004(2) 0.0031(2) 0.0000(2) U3 0.0169(2) 0.0251(2) 0.0216(2) -0.0032(2) 0.00206(17) 0.0008(2) U4 0.0167(4) 0.0221(3) 0.0194(4) 0.000 0.0011(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.367(19) . ? C1 N1 1.396(19) . ? C1 C30 1.49(2) . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C3 C4 1.367(19) . ? C3 H3 0.9500 . ? C4 N1 1.405(18) . ? C4 C5 1.51(2) . ? C5 C8 1.497(18) . ? C5 C6 1.539(19) . ? C5 C7 1.55(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.381(18) . ? C8 C13 1.429(18) . ? C8 U1 2.906(15) . ? C9 C10 1.424(18) . ? C9 U1 2.839(14) . ? C9 H9 0.9500 . ? C10 C11 1.39(2) . ? C10 C14 1.52(2) . ? C10 U1 2.878(16) . ? C11 C12 1.39(2) . ? C11 U1 3.013(16) . ? C11 H11 0.9500 . ? C12 C13 1.398(19) . ? C12 H12 0.9500 . ? C13 U1 3.004(16) . ? C13 H13 0.9500 . ? C14 C17 1.50(2) . ? C14 C16 1.53(2) . ? C14 C15 1.54(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.38(2) . ? C17 N2 1.410(19) . ? C18 C19 1.40(2) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 N2 1.393(19) . ? C20 C21 1.53(2) . ? C21 C24 1.52(2) . ? C21 C22 1.54(2) . ? C21 C23 1.561(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.382(19) . ? C24 C29 1.421(19) . ? C24 U1 2.927(16) . ? C25 C26 1.40(2) . ? C25 U1 2.848(15) . ? C25 H25 0.9500 . ? C26 C27 1.40(2) . ? C26 C30 1.531(18) . ? C26 U1 2.864(15) . ? C27 C28 1.42(2) . ? C27 U1 3.025(17) . ? C27 H27 0.9500 . ? C28 C29 1.37(2) . ? C28 H28 0.9500 . ? C29 U1 3.030(17) . ? C29 H29 0.9500 . ? C30 C31 1.53(2) . ? C30 C32 1.56(2) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.380(19) . ? C33 N3 1.382(19) . ? C33 C62 1.53(2) . ? C34 C35 1.40(2) . ? C34 H34 0.9500 . ? C35 C36 1.38(2) . ? C35 H35 0.9500 . ? C36 N3 1.397(19) . ? C36 C37 1.52(2) . ? C37 C39 1.53(2) . ? C37 C38 1.53(2) . ? C37 C40 1.542(18) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.382(19) . ? C40 C41 1.44(2) . ? C40 U2 2.887(16) . ? C41 C42 1.401(18) . ? C41 U2 2.855(15) . ? C41 H41 0.9500 . ? C42 C43 1.430(19) . ? C42 C46 1.51(2) . ? C42 U2 2.924(15) . ? C43 C44 1.38(2) . ? C43 U2 3.024(16) . ? C43 H43 0.9500 . ? C44 C45 1.408(19) . ? C44 H44 0.9500 . ? C45 U2 3.041(17) . ? C45 H45 0.9500 . ? C46 C49 1.51(2) . ? C46 C47 1.54(2) . ? C46 C48 1.55(2) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.35(2) . ? C49 N4 1.38(2) . ? C50 C51 1.41(2) . ? C50 H50 0.9500 . ? C51 C52 1.36(2) . ? C51 H51 0.9500 . ? C52 N4 1.409(19) . ? C52 C53 1.50(2) . ? C53 C56 1.524(18) . ? C53 C55 1.54(3) . ? C53 C54 1.57(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.40(2) . ? C56 C61 1.42(2) . ? C56 U2 2.898(17) . ? C57 C58 1.42(2) . ? C57 U2 2.995(17) . ? C57 H57 0.9500 . ? C58 C59 1.376(19) . ? C58 H58 0.9500 . ? C59 C60 1.40(2) . ? C59 U2 3.014(18) . ? C59 H59 0.9500 . ? C60 C61 1.392(19) . ? C60 C62 1.528(18) . ? C60 U2 2.922(15) . ? C61 U2 2.861(17) . ? C61 H61 0.9500 . ? C62 C63 1.51(2) . ? C62 C64 1.54(2) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.37(2) . ? C65 N5 1.420(19) . ? C65 C94 1.55(2) . ? C66 C67 1.44(2) . ? C66 H66 0.9500 . ? C67 C68 1.36(2) . ? C67 H67 0.9500 . ? C68 N5 1.375(19) . ? C68 C69 1.52(2) . ? C69 C72 1.50(2) . ? C69 C71 1.52(2) . ? C69 C70 1.55(2) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C77 1.41(2) . ? C72 C73 1.420(18) . ? C72 U3 2.901(16) . ? C73 C74 1.380(19) . ? C73 U3 2.868(16) . ? C73 H73 0.9500 . ? C74 C75 1.39(2) . ? C74 C78 1.559(19) . ? C74 U3 2.908(15) . ? C75 C76 1.41(2) . ? C75 U3 3.042(17) . ? C75 H75 0.9500 . ? C76 C77 1.38(2) . ? C76 H76 0.9500 . ? C77 U3 3.010(17) . ? C77 H77 0.9500 . ? C78 C81 1.50(2) . ? C78 C80 1.53(2) . ? C78 C79 1.55(2) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.38(2) . ? C81 N6 1.411(19) . ? C82 C83 1.40(3) . ? C82 H82 0.9500 . ? C83 C84 1.38(2) . ? C83 H83 0.9500 . ? C84 N6 1.41(2) . ? C84 C85 1.52(2) . ? C85 C88 1.537(19) . ? C85 C87 1.54(2) . ? C85 C86 1.55(2) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C93 1.38(2) . ? C88 C89 1.42(2) . ? C88 U3 2.874(16) . ? C89 C90 1.398(18) . ? C89 U3 2.864(15) . ? C89 H89 0.9500 . ? C90 C91 1.42(2) . ? C90 C94 1.51(2) . ? C90 U3 2.917(17) . ? C91 C92 1.37(2) . ? C91 U3 3.029(17) . ? C91 H91 0.9500 . ? C92 C93 1.40(2) . ? C92 H92 0.9500 . ? C93 U3 3.027(17) . ? C93 H93 0.9500 . ? C94 C96 1.53(2) . ? C94 C95 1.551(19) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 N7 1.359(19) 2 ? C97 C98 1.369(19) . ? C97 C110 1.53(2) . ? C98 C99 1.41(2) . ? C98 H98 0.9500 . ? C99 C100 1.404(18) 2 ? C99 H99 0.9500 . ? C100 C99 1.404(18) 2 ? C100 N7 1.406(18) . ? C100 C101 1.50(2) . ? C101 C104 1.517(19) . ? C101 C102 1.52(2) . ? C101 C103 1.56(2) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C104 C109 1.393(18) . ? C104 C105 1.420(19) . ? C104 U4 2.902(14) . ? C105 C106 1.36(2) . ? C105 U4 3.013(17) . ? C105 H105 0.9500 . ? C106 C107 1.38(2) . ? C106 U4 3.064(17) . ? C106 H106 0.9500 . ? C107 C108 1.389(19) . ? C107 U4 3.005(17) . ? C107 H107 0.9500 . ? C108 C109 1.432(18) . ? C108 C110 1.519(19) . ? C108 U4 2.875(16) . ? C109 U4 2.871(17) . ? C109 H109 0.9500 . ? C110 C111 1.54(2) . ? C110 C112 1.54(2) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? N1 U1 2.468(10) . ? N2 U1 2.438(10) . ? N3 U2 2.463(11) . ? N4 U2 2.469(10) . ? N5 U3 2.461(11) . ? N6 U3 2.449(11) . ? N7 C97 1.359(19) 2 ? N7 U4 2.459(11) . ? I1 U1 3.1112(15) . ? I2 U2 3.1131(13) . ? I3 U3 3.1054(10) . ? I4 U4 3.1119(17) . ? U4 N7 2.459(11) 2 ? U4 C109 2.871(17) 2 ? U4 C108 2.875(16) 2 ? U4 C104 2.902(14) 2 ? U4 C107 3.005(17) 2 ? U4 C105 3.013(17) 2 ? 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 C2 C1 N1 110.0(14) . . ? C2 C1 C30 129.1(14) . . ? N1 C1 C30 120.9(12) . . ? C1 C2 C3 106.2(14) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? C4 C3 C2 109.3(14) . . ? C4 C3 H3 125.3 . . ? C2 C3 H3 125.3 . . ? C3 C4 N1 107.9(15) . . ? C3 C4 C5 129.8(14) . . ? N1 C4 C5 122.1(12) . . ? C8 C5 C4 108.1(12) . . ? C8 C5 C6 113.1(11) . . ? C4 C5 C6 108.5(14) . . ? C8 C5 C7 109.6(13) . . ? C4 C5 C7 109.6(11) . . ? C6 C5 C7 107.9(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.1(12) . . ? C9 C8 C5 124.1(12) . . ? C13 C8 C5 117.6(12) . . ? C9 C8 U1 73.4(8) . . ? C13 C8 U1 79.9(9) . . ? C5 C8 U1 113.2(11) . . ? C8 C9 C10 122.4(12) . . ? C8 C9 U1 78.8(9) . . ? C10 C9 U1 77.1(8) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? U1 C9 H9 115.7 . . ? C11 C10 C9 118.0(12) . . ? C11 C10 C14 123.8(13) . . ? C9 C10 C14 118.1(13) . . ? C11 C10 U1 81.8(10) . . ? C9 C10 U1 74.1(8) . . ? C14 C10 U1 110.7(10) . . ? C10 C11 C12 120.9(13) . . ? C10 C11 U1 71.0(9) . . ? C12 C11 U1 79.6(10) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? U1 C11 H11 120.9 . . ? C11 C12 C13 120.6(13) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.9(13) . . ? C12 C13 U1 79.8(10) . . ? C8 C13 U1 72.2(9) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? U1 C13 H13 118.8 . . ? C17 C14 C10 107.7(12) . . ? C17 C14 C16 109.7(14) . . ? C10 C14 C16 111.8(14) . . ? C17 C14 C15 110.6(14) . . ? C10 C14 C15 109.0(13) . . ? C16 C14 C15 108.1(13) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 109.1(14) . . ? C18 C17 C14 129.2(14) . . ? N2 C17 C14 121.7(12) . . ? C17 C18 C19 107.9(14) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? C20 C19 C18 107.2(14) . . ? C20 C19 H19 126.4 . . ? C18 C19 H19 126.4 . . ? C19 C20 N2 110.2(14) . . ? C19 C20 C21 128.3(14) . . ? N2 C20 C21 121.3(12) . . ? C24 C21 C20 107.8(13) . . ? C24 C21 C22 109.4(14) . . ? C20 C21 C22 111.1(12) . . ? C24 C21 C23 112.6(11) . . ? C20 C21 C23 106.8(14) . . ? C22 C21 C23 109.1(13) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 117.1(13) . . ? C25 C24 C21 124.1(12) . . ? C29 C24 C21 118.5(12) . . ? C25 C24 U1 73.0(9) . . ? C29 C24 U1 80.3(9) . . ? C21 C24 U1 111.4(10) . . ? C24 C25 C26 122.9(13) . . ? C24 C25 U1 79.4(9) . . ? C26 C25 U1 76.5(9) . . ? C24 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? U1 C25 H25 115.9 . . ? C25 C26 C27 118.7(13) . . ? C25 C26 C30 117.7(13) . . ? C27 C26 C30 123.6(14) . . ? C25 C26 U1 75.2(9) . . ? C27 C26 U1 82.8(10) . . ? C30 C26 U1 110.3(10) . . ? C26 C27 C28 119.4(14) . . ? C26 C27 U1 69.9(9) . . ? C28 C27 U1 80.6(10) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? U1 C27 H27 120.1 . . ? C29 C28 C27 120.1(13) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C24 121.5(13) . . ? C28 C29 U1 81.1(10) . . ? C24 C29 U1 72.2(9) . . ? C28 C29 H29 119.3 . . ? C24 C29 H29 119.3 . . ? U1 C29 H29 118.1 . . ? C1 C30 C31 113.1(13) . . ? C1 C30 C26 108.0(13) . . ? C31 C30 C26 108.8(13) . . ? C1 C30 C32 108.6(13) . . ? C31 C30 C32 107.6(14) . . ? C26 C30 C32 110.8(12) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N3 111.5(14) . . ? C34 C33 C62 127.0(13) . . ? N3 C33 C62 121.3(11) . . ? C33 C34 C35 106.3(13) . . ? C33 C34 H34 126.9 . . ? C35 C34 H34 126.9 . . ? C36 C35 C34 107.3(14) . . ? C36 C35 H35 126.4 . . ? C34 C35 H35 126.4 . . ? C35 C36 N3 110.2(14) . . ? C35 C36 C37 128.0(14) . . ? N3 C36 C37 121.7(12) . . ? C36 C37 C39 109.6(14) . . ? C36 C37 C38 112.0(13) . . ? C39 C37 C38 108.5(14) . . ? C36 C37 C40 107.3(12) . . ? C39 C37 C40 110.8(12) . . ? C38 C37 C40 108.5(14) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 119.1(12) . . ? C45 C40 C37 124.3(13) . . ? C41 C40 C37 116.6(12) . . ? C45 C40 U2 82.8(9) . . ? C41 C40 U2 74.3(9) . . ? C37 C40 U2 110.0(10) . . ? C42 C41 C40 122.1(13) . . ? C42 C41 U2 78.7(9) . . ? C40 C41 U2 76.8(9) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? U2 C41 H41 116.0 . . ? C41 C42 C43 116.8(13) . . ? C41 C42 C46 124.5(13) . . ? C43 C42 C46 118.5(12) . . ? C41 C42 U2 73.3(9) . . ? C43 C42 U2 80.0(9) . . ? C46 C42 U2 111.4(10) . . ? C44 C43 C42 120.8(12) . . ? C44 C43 U2 81.5(10) . . ? C42 C43 U2 72.2(9) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? U2 C43 H43 117.4 . . ? C43 C44 C45 121.5(13) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C40 C45 C44 119.4(14) . . ? C40 C45 U2 70.4(9) . . ? C44 C45 U2 80.5(10) . . ? C40 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? U2 C45 H45 119.8 . . ? C49 C46 C42 108.0(13) . . ? C49 C46 C47 109.6(15) . . ? C42 C46 C47 111.0(12) . . ? C49 C46 C48 111.2(12) . . ? C42 C46 C48 108.1(14) . . ? C47 C46 C48 109.0(14) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N4 110.4(16) . . ? C50 C49 C46 128.3(15) . . ? N4 C49 C46 120.9(12) . . ? C49 C50 C51 107.3(14) . . ? C49 C50 H50 126.3 . . ? C51 C50 H50 126.3 . . ? C52 C51 C50 107.4(13) . . ? C52 C51 H51 126.3 . . ? C50 C51 H51 126.3 . . ? C51 C52 N4 108.9(15) . . ? C51 C52 C53 129.4(15) . . ? N4 C52 C53 121.6(13) . . ? C52 C53 C56 108.8(13) . . ? C52 C53 C55 110.5(15) . . ? C56 C53 C55 106.7(14) . . ? C52 C53 C54 110.5(14) . . ? C56 C53 C54 111.2(14) . . ? C55 C53 C54 109.0(14) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C61 118.6(13) . . ? C57 C56 C53 122.0(14) . . ? C61 C56 C53 119.1(14) . . ? C57 C56 U2 80.2(10) . . ? C61 C56 U2 74.3(9) . . ? C53 C56 U2 109.8(11) . . ? C56 C57 C58 118.9(14) . . ? C56 C57 U2 72.4(10) . . ? C58 C57 U2 79.6(10) . . ? C56 C57 H57 120.6 . . ? C58 C57 H57 120.6 . . ? U2 C57 H57 118.3 . . ? C59 C58 C57 120.9(13) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 121.4(13) . . ? C58 C59 U2 79.5(10) . . ? C60 C59 U2 72.7(10) . . ? C58 C59 H59 119.3 . . ? C60 C59 H59 119.3 . . ? U2 C59 H59 119.3 . . ? C61 C60 C59 117.6(13) . . ? C61 C60 C62 124.0(13) . . ? C59 C60 C62 118.3(12) . . ? C61 C60 U2 73.6(9) . . ? C59 C60 U2 80.0(10) . . ? C62 C60 U2 112.9(10) . . ? C60 C61 C56 122.6(14) . . ? C60 C61 U2 78.5(9) . . ? C56 C61 U2 77.2(10) . . ? C60 C61 H61 118.7 . . ? C56 C61 H61 118.7 . . ? U2 C61 H61 115.9 . . ? C63 C62 C60 112.9(11) . . ? C63 C62 C33 109.0(14) . . ? C60 C62 C33 107.5(12) . . ? C63 C62 C64 107.9(13) . . ? C60 C62 C64 109.1(13) . . ? C33 C62 C64 110.5(12) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N5 110.1(15) . . ? C66 C65 C94 127.2(14) . . ? N5 C65 C94 122.5(12) . . ? C65 C66 C67 106.6(14) . . ? C65 C66 H66 126.7 . . ? C67 C66 H66 126.7 . . ? C68 C67 C66 106.5(14) . . ? C68 C67 H67 126.7 . . ? C66 C67 H67 126.7 . . ? C67 C68 N5 111.8(15) . . ? C67 C68 C69 128.1(15) . . ? N5 C68 C69 120.1(13) . . ? C72 C69 C71 108.2(14) . . ? C72 C69 C68 107.8(12) . . ? C71 C69 C68 111.8(13) . . ? C72 C69 C70 111.4(13) . . ? C71 C69 C70 109.0(14) . . ? C68 C69 C70 108.6(14) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C77 C72 C73 117.2(13) . . ? C77 C72 C69 123.8(13) . . ? C73 C72 C69 119.0(12) . . ? C77 C72 U3 80.5(10) . . ? C73 C72 U3 74.4(9) . . ? C69 C72 U3 111.1(11) . . ? C74 C73 C72 121.3(13) . . ? C74 C73 U3 77.8(9) . . ? C72 C73 U3 77.1(9) . . ? C74 C73 H73 119.4 . . ? C72 C73 H73 119.4 . . ? U3 C73 H73 116.3 . . ? C73 C74 C75 121.3(13) . . ? C73 C74 C78 121.9(13) . . ? C75 C74 C78 116.7(12) . . ? C73 C74 U3 74.5(9) . . ? C75 C74 U3 81.9(10) . . ? C78 C74 U3 110.7(10) . . ? C74 C75 C76 117.9(14) . . ? C74 C75 U3 71.2(9) . . ? C76 C75 U3 79.9(11) . . ? C74 C75 H75 121.1 . . ? C76 C75 H75 121.1 . . ? U3 C75 H75 118.9 . . ? C77 C76 C75 121.4(14) . . ? C77 C76 H76 119.3 . . ? C75 C76 H76 119.3 . . ? C76 C77 C72 120.7(14) . . ? C76 C77 U3 81.5(11) . . ? C72 C77 U3 72.0(10) . . ? C76 C77 H77 119.7 . . ? C72 C77 H77 119.7 . . ? U3 C77 H77 117.6 . . ? C81 C78 C80 109.5(15) . . ? C81 C78 C79 109.5(12) . . ? C80 C78 C79 108.9(13) . . ? C81 C78 C74 107.5(12) . . ? C80 C78 C74 112.3(12) . . ? C79 C78 C74 109.0(14) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 N6 108.9(15) . . ? C82 C81 C78 128.7(14) . . ? N6 C81 C78 122.0(12) . . ? C81 C82 C83 108.3(14) . . ? C81 C82 H82 125.9 . . ? C83 C82 H82 125.9 . . ? C84 C83 C82 107.5(15) . . ? C84 C83 H83 126.2 . . ? C82 C83 H83 126.2 . . ? C83 C84 N6 109.7(15) . . ? C83 C84 C85 129.5(15) . . ? N6 C84 C85 120.7(12) . . ? C84 C85 C88 107.7(12) . . ? C84 C85 C87 110.7(13) . . ? C88 C85 C87 109.7(13) . . ? C84 C85 C86 109.5(13) . . ? C88 C85 C86 111.7(12) . . ? C87 C85 C86 107.5(13) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C93 C88 C89 119.1(13) . . ? C93 C88 C85 123.3(14) . . ? C89 C88 C85 117.6(12) . . ? C93 C88 U3 82.7(10) . . ? C89 C88 U3 75.3(9) . . ? C85 C88 U3 111.4(10) . . ? C90 C89 C88 122.1(13) . . ? C90 C89 U3 78.1(9) . . ? C88 C89 U3 76.1(9) . . ? C90 C89 H89 118.9 . . ? C88 C89 H89 118.9 . . ? U3 C89 H89 117.5 . . ? C89 C90 C91 117.3(14) . . ? C89 C90 C94 124.5(13) . . ? C91 C90 C94 118.2(12) . . ? C89 C90 U3 73.9(9) . . ? C91 C90 U3 80.6(10) . . ? C94 C90 U3 113.4(11) . . ? C92 C91 C90 120.1(14) . . ? C92 C91 U3 78.8(10) . . ? C90 C91 U3 71.8(9) . . ? C92 C91 H91 119.9 . . ? C90 C91 H91 119.9 . . ? U3 C91 H91 120.4 . . ? C91 C92 C93 122.2(14) . . ? C91 C92 H92 118.9 . . ? C93 C92 H92 118.9 . . ? C88 C93 C92 118.9(14) . . ? C88 C93 U3 70.4(10) . . ? C92 C93 U3 78.6(10) . . ? C88 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? U3 C93 H93 121.7 . . ? C90 C94 C96 109.7(14) . . ? C90 C94 C65 107.0(12) . . ? C96 C94 C65 111.0(12) . . ? C90 C94 C95 112.4(11) . . ? C96 C94 C95 108.3(13) . . ? C65 C94 C95 108.5(14) . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C94 C96 H96A 109.5 . . ? C94 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C94 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N7 C97 C98 111.0(15) 2 . ? N7 C97 C110 120.8(12) 2 . ? C98 C97 C110 128.2(15) . . ? C97 C98 C99 107.8(14) . . ? C97 C98 H98 126.1 . . ? C99 C98 H98 126.1 . . ? C100 C99 C98 105.8(13) 2 . ? C100 C99 H99 127.1 2 . ? C98 C99 H99 127.1 . . ? C99 C100 N7 109.1(13) 2 . ? C99 C100 C101 127.8(13) 2 . ? N7 C100 C101 122.8(12) . . ? C100 C101 C104 107.6(12) . . ? C100 C101 C102 110.2(14) . . ? C104 C101 C102 112.1(11) . . ? C100 C101 C103 110.7(12) . . ? C104 C101 C103 109.6(13) . . ? C102 C101 C103 106.7(13) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C101 C103 H10D 109.5 . . ? C101 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C101 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C109 C104 C105 118.9(13) . . ? C109 C104 C101 122.6(12) . . ? C105 C104 C101 118.4(12) . . ? C109 C104 U4 74.8(9) . . ? C105 C104 U4 80.5(9) . . ? C101 C104 U4 112.0(10) . . ? C106 C105 C104 118.6(13) . . ? C106 C105 U4 79.1(10) . . ? C104 C105 U4 71.8(9) . . ? C106 C105 H105 120.7 . . ? C104 C105 H105 120.7 . . ? U4 C105 H105 119.4 . . ? C105 C106 C107 122.9(13) . . ? C105 C106 U4 74.9(10) . . ? C107 C106 U4 74.4(10) . . ? C105 C106 H106 118.6 . . ? C107 C106 H106 118.6 . . ? U4 C106 H106 123.5 . . ? C106 C107 C108 120.6(14) . . ? C106 C107 U4 79.2(10) . . ? C108 C107 U4 71.2(9) . . ? C106 C107 H107 119.7 . . ? C108 C107 H107 119.7 . . ? U4 C107 H107 120.9 . . ? C107 C108 C109 117.1(13) . . ? C107 C108 C110 125.4(13) . . ? C109 C108 C110 117.4(12) . . ? C107 C108 U4 81.6(10) . . ? C109 C108 U4 75.4(9) . . ? C110 C108 U4 110.1(10) . . ? C104 C109 C108 121.5(12) . . ? C104 C109 U4 77.3(9) . . ? C108 C109 U4 75.7(9) . . ? C104 C109 H109 119.2 . . ? C108 C109 H109 119.2 . . ? U4 C109 H109 118.6 . . ? C108 C110 C97 107.3(12) . . ? C108 C110 C111 109.7(12) . . ? C97 C110 C111 111.5(14) . . ? C108 C110 C112 108.8(13) . . ? C97 C110 C112 110.7(13) . . ? C111 C110 C112 108.7(13) . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C110 C112 H11D 109.5 . . ? C110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C1 N1 C4 106.5(11) . . ? C1 N1 U1 125.9(9) . . ? C4 N1 U1 126.9(10) . . ? C20 N2 C17 105.5(11) . . ? C20 N2 U1 128.5(10) . . ? C17 N2 U1 125.9(10) . . ? C33 N3 C36 104.7(11) . . ? C33 N3 U2 129.4(9) . . ? C36 N3 U2 125.6(10) . . ? C49 N4 C52 105.9(11) . . ? C49 N4 U2 128.6(10) . . ? C52 N4 U2 125.5(10) . . ? C68 N5 C65 105.0(11) . . ? C68 N5 U3 128.3(10) . . ? C65 N5 U3 126.7(10) . . ? C84 N6 C81 105.6(11) . . ? C84 N6 U3 127.0(10) . . ? C81 N6 U3 127.3(10) . . ? C97 N7 C100 106.3(11) 2 . ? C97 N7 U4 127.0(10) 2 . ? C100 N7 U4 126.4(9) . . ? N2 U1 N1 118.2(4) . . ? N2 U1 C9 65.1(4) . . ? N1 U1 C9 84.8(4) . . ? N2 U1 C25 85.1(4) . . ? N1 U1 C25 65.9(4) . . ? C9 U1 C25 121.5(4) . . ? N2 U1 C26 111.5(4) . . ? N1 U1 C26 62.8(4) . . ? C9 U1 C26 141.9(4) . . ? C25 U1 C26 28.3(4) . . ? N2 U1 C10 62.6(4) . . ? N1 U1 C10 111.5(4) . . ? C9 U1 C10 28.8(4) . . ? C25 U1 C10 142.5(4) . . ? C26 U1 C10 169.7(5) . . ? N2 U1 C8 90.6(4) . . ? N1 U1 C8 61.3(4) . . ? C9 U1 C8 27.8(4) . . ? C25 U1 C8 116.6(4) . . ? C26 U1 C8 123.9(4) . . ? C10 U1 C8 50.3(4) . . ? N2 U1 C24 62.0(4) . . ? N1 U1 C24 91.3(4) . . ? C9 U1 C24 116.7(4) . . ? C25 U1 C24 27.7(4) . . ? C26 U1 C24 49.8(4) . . ? C10 U1 C24 124.4(4) . . ? C8 U1 C24 127.0(4) . . ? N2 U1 C13 113.5(4) . . ? N1 U1 C13 65.6(4) . . ? C9 U1 C13 48.6(4) . . ? C25 U1 C13 131.2(4) . . ? C26 U1 C13 122.7(4) . . ? C10 U1 C13 57.2(4) . . ? C8 U1 C13 27.9(4) . . ? C24 U1 C13 151.8(4) . . ? N2 U1 C11 86.7(4) . . ? N1 U1 C11 112.8(4) . . ? C9 U1 C11 48.6(4) . . ? C25 U1 C11 169.5(4) . . ? C26 U1 C11 161.4(4) . . ? C10 U1 C11 27.2(4) . . ? C8 U1 C11 56.9(4) . . ? C24 U1 C11 147.4(4) . . ? C13 U1 C11 47.5(4) . . ? N2 U1 C27 113.5(5) . . ? N1 U1 C27 86.6(4) . . ? C9 U1 C27 169.0(4) . . ? C25 U1 C27 48.2(4) . . ? C26 U1 C27 27.3(4) . . ? C10 U1 C27 161.5(4) . . ? C8 U1 C27 146.8(4) . . ? C24 U1 C27 56.6(4) . . ? C13 U1 C27 132.5(4) . . ? C11 U1 C27 142.0(5) . . ? N2 U1 C29 66.9(4) . . ? N1 U1 C29 113.4(4) . . ? C9 U1 C29 131.7(4) . . ? C25 U1 C29 47.9(4) . . ? C26 U1 C29 56.4(4) . . ? C10 U1 C29 123.6(4) . . ? C8 U1 C29 151.9(4) . . ? C24 U1 C29 27.5(4) . . ? C13 U1 C29 179.0(4) . . ? C11 U1 C29 133.4(4) . . ? C27 U1 C29 47.0(4) . . ? N3 U2 N4 118.3(4) . . ? N3 U2 C41 65.8(4) . . ? N4 U2 C41 84.8(4) . . ? N3 U2 C61 84.3(4) . . ? N4 U2 C61 66.1(4) . . ? C41 U2 C61 121.4(4) . . ? N3 U2 C40 63.4(4) . . ? N4 U2 C40 111.5(4) . . ? C41 U2 C40 28.9(4) . . ? C61 U2 C40 142.4(4) . . ? N3 U2 C56 110.8(4) . . ? N4 U2 C56 62.8(4) . . ? C41 U2 C56 141.9(4) . . ? C61 U2 C56 28.5(4) . . ? C40 U2 C56 169.8(4) . . ? N3 U2 C60 61.0(4) . . ? N4 U2 C60 91.7(4) . . ? C41 U2 C60 116.7(4) . . ? C61 U2 C60 27.8(4) . . ? C40 U2 C60 124.3(4) . . ? C56 U2 C60 50.1(4) . . ? N3 U2 C42 91.4(4) . . ? N4 U2 C42 61.1(4) . . ? C41 U2 C42 28.0(4) . . ? C61 U2 C42 116.6(4) . . ? C40 U2 C42 50.5(4) . . ? C56 U2 C42 123.7(4) . . ? C60 U2 C42 127.3(4) . . ? N3 U2 C57 113.5(5) . . ? N4 U2 C57 86.4(4) . . ? C41 U2 C57 169.2(4) . . ? C61 U2 C57 48.7(5) . . ? C40 U2 C57 161.4(4) . . ? C56 U2 C57 27.4(4) . . ? C60 U2 C57 57.2(4) . . ? C42 U2 C57 146.3(4) . . ? N3 U2 C59 66.0(4) . . ? N4 U2 C59 113.6(4) . . ? C41 U2 C59 131.5(4) . . ? C61 U2 C59 47.9(4) . . ? C40 U2 C59 123.4(4) . . ? C56 U2 C59 56.6(4) . . ? C60 U2 C59 27.2(4) . . ? C42 U2 C59 151.9(4) . . ? C57 U2 C59 47.8(4) . . ? N3 U2 C43 113.8(4) . . ? N4 U2 C43 66.1(4) . . ? C41 U2 C43 48.3(4) . . ? C61 U2 C43 131.8(4) . . ? C40 U2 C43 56.7(4) . . ? C56 U2 C43 123.3(4) . . ? C60 U2 C43 152.4(4) . . ? C42 U2 C43 27.8(4) . . ? C57 U2 C43 132.3(4) . . ? C59 U2 C43 179.6(4) . . ? N3 U2 C45 86.9(4) . . ? N4 U2 C45 113.0(4) . . ? C41 U2 C45 48.5(4) . . ? C61 U2 C45 169.1(4) . . ? C40 U2 C45 26.8(4) . . ? C56 U2 C45 161.8(4) . . ? C60 U2 C45 146.7(4) . . ? C42 U2 C45 57.1(4) . . ? C57 U2 C45 141.7(4) . . ? C59 U2 C45 132.9(4) . . ? C43 U2 C45 47.3(4) . . ? N6 U3 N5 119.2(3) . . ? N6 U3 C89 66.1(4) . . ? N5 U3 C89 85.9(4) . . ? N6 U3 C73 85.3(4) . . ? N5 U3 C73 65.2(4) . . ? C89 U3 C73 122.2(3) . . ? N6 U3 C88 62.8(4) . . ? N5 U3 C88 112.5(4) . . ? C89 U3 C88 28.6(4) . . ? C73 U3 C88 142.7(4) . . ? N6 U3 C72 111.9(4) . . ? N5 U3 C72 61.4(4) . . ? C89 U3 C72 142.2(4) . . ? C73 U3 C72 28.5(4) . . ? C88 U3 C72 169.8(3) . . ? N6 U3 C74 62.6(4) . . ? N5 U3 C74 91.1(4) . . ? C89 U3 C74 118.6(4) . . ? C73 U3 C74 27.6(4) . . ? C88 U3 C74 125.3(4) . . ? C72 U3 C74 49.7(4) . . ? N6 U3 C90 91.9(4) . . ? N5 U3 C90 62.4(4) . . ? C89 U3 C90 28.0(4) . . ? C73 U3 C90 117.3(4) . . ? C88 U3 C90 50.3(4) . . ? C72 U3 C90 123.6(4) . . ? C74 U3 C90 128.9(3) . . ? N6 U3 C77 113.8(4) . . ? N5 U3 C77 85.4(4) . . ? C89 U3 C77 169.6(4) . . ? C73 U3 C77 48.4(4) . . ? C88 U3 C77 161.5(4) . . ? C72 U3 C77 27.5(4) . . ? C74 U3 C77 56.0(4) . . ? C90 U3 C77 146.3(4) . . ? N6 U3 C93 86.2(4) . . ? N5 U3 C93 114.3(4) . . ? C89 U3 C93 48.2(4) . . ? C73 U3 C93 169.6(4) . . ? C88 U3 C93 26.9(4) . . ? C72 U3 C93 161.4(4) . . ? C74 U3 C93 147.2(4) . . ? C90 U3 C93 56.9(4) . . ? C77 U3 C93 141.5(4) . . ? N6 U3 C91 113.8(4) . . ? N5 U3 C91 67.3(4) . . ? C89 U3 C91 48.1(4) . . ? C73 U3 C91 132.1(4) . . ? C88 U3 C91 56.6(4) . . ? C72 U3 C91 122.9(4) . . ? C74 U3 C91 153.6(4) . . ? C90 U3 C91 27.5(4) . . ? C77 U3 C91 132.1(4) . . ? C93 U3 C91 47.3(4) . . ? N6 U3 C75 66.6(4) . . ? N5 U3 C75 112.9(4) . . ? C89 U3 C75 132.4(4) . . ? C73 U3 C75 48.1(4) . . ? C88 U3 C75 123.6(4) . . ? C72 U3 C75 57.0(4) . . ? C74 U3 C75 26.9(4) . . ? C90 U3 C75 153.0(4) . . ? C77 U3 C75 47.4(4) . . ? C93 U3 C75 132.6(4) . . ? C91 U3 C75 179.4(4) . . ? N7 U4 N7 118.5(5) . 2 ? N7 U4 C109 65.3(4) . 2 ? N7 U4 C109 85.5(4) 2 2 ? N7 U4 C109 85.5(4) . . ? N7 U4 C109 65.3(4) 2 . ? C109 U4 C109 121.8(6) 2 . ? N7 U4 C108 62.5(4) . 2 ? N7 U4 C108 112.2(4) 2 2 ? C109 U4 C108 28.9(4) 2 2 ? C109 U4 C108 142.7(4) . 2 ? N7 U4 C108 112.2(4) . . ? N7 U4 C108 62.5(4) 2 . ? C109 U4 C108 142.7(4) 2 . ? C109 U4 C108 28.9(4) . . ? C108 U4 C108 170.5(6) 2 . ? N7 U4 C104 90.9(4) . 2 ? N7 U4 C104 61.9(4) 2 2 ? C109 U4 C104 27.9(4) 2 2 ? C109 U4 C104 116.7(4) . 2 ? C108 U4 C104 50.5(4) 2 2 ? C108 U4 C104 124.2(4) . 2 ? N7 U4 C104 61.9(4) . . ? N7 U4 C104 90.9(4) 2 . ? C109 U4 C104 116.7(4) 2 . ? C109 U4 C104 27.9(4) . . ? C108 U4 C104 124.2(4) 2 . ? C108 U4 C104 50.5(4) . . ? C104 U4 C104 127.1(5) 2 . ? N7 U4 C107 86.7(4) . 2 ? N7 U4 C107 113.0(4) 2 2 ? C109 U4 C107 48.3(4) 2 2 ? C109 U4 C107 169.6(4) . 2 ? C108 U4 C107 27.2(4) 2 2 ? C108 U4 C107 160.6(4) . 2 ? C104 U4 C107 56.5(4) 2 2 ? C104 U4 C107 147.5(4) . 2 ? N7 U4 C107 113.0(4) . . ? N7 U4 C107 86.7(4) 2 . ? C109 U4 C107 169.6(4) 2 . ? C109 U4 C107 48.3(4) . . ? C108 U4 C107 160.6(4) 2 . ? C108 U4 C107 27.2(4) . . ? C104 U4 C107 147.5(4) 2 . ? C104 U4 C107 56.5(4) . . ? C107 U4 C107 141.8(6) 2 . ? N7 U4 C105 113.6(4) . 2 ? N7 U4 C105 66.1(4) 2 2 ? C109 U4 C105 48.6(4) 2 2 ? C109 U4 C105 131.0(4) . 2 ? C108 U4 C105 57.4(4) 2 2 ? C108 U4 C105 122.5(4) . 2 ? C104 U4 C105 27.7(4) 2 2 ? C104 U4 C105 151.7(4) . 2 ? C107 U4 C105 47.3(4) 2 2 ? C107 U4 C105 133.0(4) . 2 ? N7 U4 C105 66.1(4) . . ? N7 U4 C105 113.6(4) 2 . ? C109 U4 C105 131.0(4) 2 . ? C109 U4 C105 48.6(4) . . ? C108 U4 C105 122.5(4) 2 . ? C108 U4 C105 57.4(4) . . ? C104 U4 C105 151.7(4) 2 . ? C104 U4 C105 27.7(4) . . ? C107 U4 C105 133.0(4) 2 . ? C107 U4 C105 47.3(4) . . ? C105 U4 C105 179.4(6) 2 . ? 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 N1 C1 C2 C3 1.4(17) . . . . ? C30 C1 C2 C3 179.7(15) . . . . ? C1 C2 C3 C4 -1.0(18) . . . . ? C2 C3 C4 N1 0.3(17) . . . . ? C2 C3 C4 C5 175.6(14) . . . . ? C3 C4 C5 C8 165.1(14) . . . . ? N1 C4 C5 C8 -20.1(18) . . . . ? C3 C4 C5 C6 -71.9(19) . . . . ? N1 C4 C5 C6 102.9(14) . . . . ? C3 C4 C5 C7 46(2) . . . . ? N1 C4 C5 C7 -139.5(13) . . . . ? C4 C5 C8 C9 115.1(16) . . . . ? C6 C5 C8 C9 -5(2) . . . . ? C7 C5 C8 C9 -125.5(16) . . . . ? C4 C5 C8 C13 -60.4(18) . . . . ? C6 C5 C8 C13 179.4(15) . . . . ? C7 C5 C8 C13 59.0(18) . . . . ? C4 C5 C8 U1 30.0(13) . . . . ? C6 C5 C8 U1 -90.1(14) . . . . ? C7 C5 C8 U1 149.4(10) . . . . ? C13 C8 C9 C10 2(2) . . . . ? C5 C8 C9 C10 -173.8(15) . . . . ? U1 C8 C9 C10 -66.7(14) . . . . ? C13 C8 C9 U1 68.4(14) . . . . ? C5 C8 C9 U1 -107.1(15) . . . . ? C8 C9 C10 C11 -4(2) . . . . ? U1 C9 C10 C11 -71.4(14) . . . . ? C8 C9 C10 C14 172.9(15) . . . . ? U1 C9 C10 C14 105.3(13) . . . . ? C8 C9 C10 U1 67.6(14) . . . . ? C9 C10 C11 C12 2(3) . . . . ? C14 C10 C11 C12 -174.0(16) . . . . ? U1 C10 C11 C12 -64.6(16) . . . . ? C9 C10 C11 U1 67.0(13) . . . . ? C14 C10 C11 U1 -109.4(16) . . . . ? C10 C11 C12 C13 1(3) . . . . ? U1 C11 C12 C13 -59.4(16) . . . . ? C11 C12 C13 C8 -3(3) . . . . ? C11 C12 C13 U1 59.6(16) . . . . ? C9 C8 C13 C12 2(2) . . . . ? C5 C8 C13 C12 177.5(16) . . . . ? U1 C8 C13 C12 66.5(15) . . . . ? C9 C8 C13 U1 -64.9(13) . . . . ? C5 C8 C13 U1 111.0(14) . . . . ? C11 C10 C14 C17 129.7(17) . . . . ? C9 C10 C14 C17 -46.7(19) . . . . ? U1 C10 C14 C17 35.7(14) . . . . ? C11 C10 C14 C16 9(2) . . . . ? C9 C10 C14 C16 -167.3(15) . . . . ? U1 C10 C14 C16 -84.8(14) . . . . ? C11 C10 C14 C15 -110.3(18) . . . . ? C9 C10 C14 C15 73.3(18) . . . . ? U1 C10 C14 C15 155.8(10) . . . . ? C10 C14 C17 C18 151.5(15) . . . . ? C16 C14 C17 C18 -87(2) . . . . ? C15 C14 C17 C18 32(2) . . . . ? C10 C14 C17 N2 -27.9(19) . . . . ? C16 C14 C17 N2 93.9(16) . . . . ? C15 C14 C17 N2 -146.9(13) . . . . ? N2 C17 C18 C19 -0.7(17) . . . . ? C14 C17 C18 C19 179.8(14) . . . . ? C17 C18 C19 C20 0.2(17) . . . . ? C18 C19 C20 N2 0.4(16) . . . . ? C18 C19 C20 C21 175.1(14) . . . . ? C19 C20 C21 C24 160.0(14) . . . . ? N2 C20 C21 C24 -25.9(17) . . . . ? C19 C20 C21 C22 40(2) . . . . ? N2 C20 C21 C22 -145.8(14) . . . . ? C19 C20 C21 C23 -78.8(18) . . . . ? N2 C20 C21 C23 95.3(15) . . . . ? C20 C21 C24 C25 115.1(16) . . . . ? C22 C21 C24 C25 -123.9(16) . . . . ? C23 C21 C24 C25 -2(2) . . . . ? C20 C21 C24 C29 -58.8(18) . . . . ? C22 C21 C24 C29 62.2(19) . . . . ? C23 C21 C24 C29 -176.3(16) . . . . ? C20 C21 C24 U1 31.6(12) . . . . ? C22 C21 C24 U1 152.6(10) . . . . ? C23 C21 C24 U1 -85.9(14) . . . . ? C29 C24 C25 C26 3(2) . . . . ? C21 C24 C25 C26 -170.9(16) . . . . ? U1 C24 C25 C26 -66.1(14) . . . . ? C29 C24 C25 U1 69.2(14) . . . . ? C21 C24 C25 U1 -104.7(15) . . . . ? C24 C25 C26 C27 -5(2) . . . . ? U1 C25 C26 C27 -73.0(15) . . . . ? C24 C25 C26 C30 173.0(15) . . . . ? U1 C25 C26 C30 105.4(13) . . . . ? C24 C25 C26 U1 67.6(15) . . . . ? C25 C26 C27 C28 3(3) . . . . ? C30 C26 C27 C28 -175.8(15) . . . . ? U1 C26 C27 C28 -66.2(16) . . . . ? C25 C26 C27 U1 68.7(14) . . . . ? C30 C26 C27 U1 -109.6(16) . . . . ? C26 C27 C28 C29 2(3) . . . . ? U1 C27 C28 C29 -58.1(15) . . . . ? C27 C28 C29 C24 -5(3) . . . . ? C27 C28 C29 U1 57.8(15) . . . . ? C25 C24 C29 C28 2(2) . . . . ? C21 C24 C29 C28 176.5(16) . . . . ? U1 C24 C29 C28 67.3(16) . . . . ? C25 C24 C29 U1 -65.1(13) . . . . ? C21 C24 C29 U1 109.2(14) . . . . ? C2 C1 C30 C31 28(2) . . . . ? N1 C1 C30 C31 -153.7(14) . . . . ? C2 C1 C30 C26 148.6(16) . . . . ? N1 C1 C30 C26 -33.3(19) . . . . ? C2 C1 C30 C32 -91.2(19) . . . . ? N1 C1 C30 C32 86.9(16) . . . . ? C25 C26 C30 C1 -46.2(19) . . . . ? C27 C26 C30 C1 132.1(17) . . . . ? U1 C26 C30 C1 37.3(14) . . . . ? C25 C26 C30 C31 77.0(19) . . . . ? C27 C26 C30 C31 -104.7(19) . . . . ? U1 C26 C30 C31 160.4(11) . . . . ? C25 C26 C30 C32 -165.0(15) . . . . ? C27 C26 C30 C32 13(2) . . . . ? U1 C26 C30 C32 -81.5(14) . . . . ? N3 C33 C34 C35 0.7(17) . . . . ? C62 C33 C34 C35 175.1(14) . . . . ? C33 C34 C35 C36 -0.3(17) . . . . ? C34 C35 C36 N3 -0.2(17) . . . . ? C34 C35 C36 C37 177.7(15) . . . . ? C35 C36 C37 C39 -90.0(19) . . . . ? N3 C36 C37 C39 87.8(16) . . . . ? C35 C36 C37 C38 31(2) . . . . ? N3 C36 C37 C38 -151.7(14) . . . . ? C35 C36 C37 C40 149.6(15) . . . . ? N3 C36 C37 C40 -33(2) . . . . ? C36 C37 C40 C45 131.5(17) . . . . ? C39 C37 C40 C45 12(2) . . . . ? C38 C37 C40 C45 -107.2(19) . . . . ? C36 C37 C40 C41 -45.4(19) . . . . ? C39 C37 C40 C41 -165.1(15) . . . . ? C38 C37 C40 C41 75.9(18) . . . . ? C36 C37 C40 U2 36.5(14) . . . . ? C39 C37 C40 U2 -83.2(14) . . . . ? C38 C37 C40 U2 157.8(11) . . . . ? C45 C40 C41 C42 -5(2) . . . . ? C37 C40 C41 C42 172.2(15) . . . . ? U2 C40 C41 C42 67.4(14) . . . . ? C45 C40 C41 U2 -72.2(15) . . . . ? C37 C40 C41 U2 104.8(13) . . . . ? C40 C41 C42 C43 3(2) . . . . ? U2 C41 C42 C43 69.2(14) . . . . ? C40 C41 C42 C46 -171.2(16) . . . . ? U2 C41 C42 C46 -104.8(15) . . . . ? C40 C41 C42 U2 -66.4(14) . . . . ? C41 C42 C43 C44 3(2) . . . . ? C46 C42 C43 C44 177.1(16) . . . . ? U2 C42 C43 C44 68.1(16) . . . . ? C41 C42 C43 U2 -65.4(13) . . . . ? C46 C42 C43 U2 109.0(14) . . . . ? C42 C43 C44 C45 -6(3) . . . . ? U2 C43 C44 C45 56.9(16) . . . . ? C41 C40 C45 C44 1(3) . . . . ? C37 C40 C45 C44 -175.6(16) . . . . ? U2 C40 C45 C44 -66.3(16) . . . . ? C41 C40 C45 U2 67.5(14) . . . . ? C37 C40 C45 U2 -109.3(16) . . . . ? C43 C44 C45 C40 4(3) . . . . ? C43 C44 C45 U2 -56.7(17) . . . . ? C41 C42 C46 C49 117.6(16) . . . . ? C43 C42 C46 C49 -56.4(19) . . . . ? U2 C42 C46 C49 33.7(14) . . . . ? C41 C42 C46 C47 -3(2) . . . . ? C43 C42 C46 C47 -176.6(16) . . . . ? U2 C42 C46 C47 -86.5(14) . . . . ? C41 C42 C46 C48 -122.1(17) . . . . ? C43 C42 C46 C48 64.0(19) . . . . ? U2 C42 C46 C48 154.0(10) . . . . ? C42 C46 C49 C50 159.2(16) . . . . ? C47 C46 C49 C50 -80(2) . . . . ? C48 C46 C49 C50 41(2) . . . . ? C42 C46 C49 N4 -28.9(19) . . . . ? C47 C46 C49 N4 92.1(16) . . . . ? C48 C46 C49 N4 -147.3(15) . . . . ? N4 C49 C50 C51 -0.3(18) . . . . ? C46 C49 C50 C51 172.2(15) . . . . ? C49 C50 C51 C52 -0.3(18) . . . . ? C50 C51 C52 N4 0.8(17) . . . . ? C50 C51 C52 C53 178.5(15) . . . . ? C51 C52 C53 C56 153.6(16) . . . . ? N4 C52 C53 C56 -29(2) . . . . ? C51 C52 C53 C55 37(2) . . . . ? N4 C52 C53 C55 -145.9(13) . . . . ? C51 C52 C53 C54 -84(2) . . . . ? N4 C52 C53 C54 93.3(16) . . . . ? C52 C53 C56 C57 126.7(18) . . . . ? C55 C53 C56 C57 -114.1(19) . . . . ? C54 C53 C56 C57 5(3) . . . . ? C52 C53 C56 C61 -47(2) . . . . ? C55 C53 C56 C61 73(2) . . . . ? C54 C53 C56 C61 -168.6(16) . . . . ? C52 C53 C56 U2 36.0(15) . . . . ? C55 C53 C56 U2 155.3(11) . . . . ? C54 C53 C56 U2 -85.9(15) . . . . ? C61 C56 C57 C58 -1(3) . . . . ? C53 C56 C57 C58 -174.3(16) . . . . ? U2 C56 C57 C58 -67.0(16) . . . . ? C61 C56 C57 U2 66.0(15) . . . . ? C53 C56 C57 U2 -107.3(17) . . . . ? C56 C57 C58 C59 4(3) . . . . ? U2 C57 C58 C59 -59.7(17) . . . . ? C57 C58 C59 C60 -3(3) . . . . ? C57 C58 C59 U2 59.1(16) . . . . ? C58 C59 C60 C61 0(3) . . . . ? U2 C59 C60 C61 -65.5(14) . . . . ? C58 C59 C60 C62 176.3(17) . . . . ? U2 C59 C60 C62 110.7(14) . . . . ? C58 C59 C60 U2 65.6(17) . . . . ? C59 C60 C61 C56 3(3) . . . . ? C62 C60 C61 C56 -173.5(16) . . . . ? U2 C60 C61 C56 -66.6(15) . . . . ? C59 C60 C61 U2 69.1(15) . . . . ? C62 C60 C61 U2 -106.9(15) . . . . ? C57 C56 C61 C60 -2(3) . . . . ? C53 C56 C61 C60 171.5(16) . . . . ? U2 C56 C61 C60 67.2(15) . . . . ? C57 C56 C61 U2 -69.3(16) . . . . ? C53 C56 C61 U2 104.3(15) . . . . ? C61 C60 C62 C63 -6(2) . . . . ? C59 C60 C62 C63 178.5(16) . . . . ? U2 C60 C62 C63 -90.7(14) . . . . ? C61 C60 C62 C33 114.7(16) . . . . ? C59 C60 C62 C33 -61.3(19) . . . . ? U2 C60 C62 C33 29.6(13) . . . . ? C61 C60 C62 C64 -125.4(16) . . . . ? C59 C60 C62 C64 58.6(19) . . . . ? U2 C60 C62 C64 149.4(10) . . . . ? C34 C33 C62 C63 -72.6(18) . . . . ? N3 C33 C62 C63 101.4(15) . . . . ? C34 C33 C62 C60 164.8(14) . . . . ? N3 C33 C62 C60 -21.3(18) . . . . ? C34 C33 C62 C64 45.8(19) . . . . ? N3 C33 C62 C64 -140.3(13) . . . . ? N5 C65 C66 C67 0.5(18) . . . . ? C94 C65 C66 C67 -174.1(14) . . . . ? C65 C66 C67 C68 -0.7(18) . . . . ? C66 C67 C68 N5 0.8(17) . . . . ? C66 C67 C68 C69 -177.5(14) . . . . ? C67 C68 C69 C72 -151.6(15) . . . . ? N5 C68 C69 C72 30.3(18) . . . . ? C67 C68 C69 C71 -33(2) . . . . ? N5 C68 C69 C71 149.2(13) . . . . ? C67 C68 C69 C70 87.6(19) . . . . ? N5 C68 C69 C70 -90.6(16) . . . . ? C71 C69 C72 C77 110.4(19) . . . . ? C68 C69 C72 C77 -128.5(17) . . . . ? C70 C69 C72 C77 -9(3) . . . . ? C71 C69 C72 C73 -73.6(19) . . . . ? C68 C69 C72 C73 48(2) . . . . ? C70 C69 C72 C73 166.6(16) . . . . ? C71 C69 C72 U3 -157.0(10) . . . . ? C68 C69 C72 U3 -35.8(13) . . . . ? C70 C69 C72 U3 83.2(15) . . . . ? C77 C72 C73 C74 4(3) . . . . ? C69 C72 C73 C74 -172.7(16) . . . . ? U3 C72 C73 C74 -66.9(15) . . . . ? C77 C72 C73 U3 70.4(15) . . . . ? C69 C72 C73 U3 -105.9(15) . . . . ? C72 C73 C74 C75 -4(3) . . . . ? U3 C73 C74 C75 -70.2(15) . . . . ? C72 C73 C74 C78 171.6(15) . . . . ? U3 C73 C74 C78 105.1(14) . . . . ? C72 C73 C74 U3 66.5(15) . . . . ? C73 C74 C75 C76 -1(3) . . . . ? C78 C74 C75 C76 -176.2(16) . . . . ? U3 C74 C75 C76 -67.0(16) . . . . ? C73 C74 C75 U3 66.4(14) . . . . ? C78 C74 C75 U3 -109.2(14) . . . . ? C74 C75 C76 C77 5(3) . . . . ? U3 C75 C76 C77 -57.0(17) . . . . ? C75 C76 C77 C72 -5(3) . . . . ? C75 C76 C77 U3 57.6(17) . . . . ? C73 C72 C77 C76 1(3) . . . . ? C69 C72 C77 C76 177.1(17) . . . . ? U3 C72 C77 C76 68.0(17) . . . . ? C73 C72 C77 U3 -67.0(14) . . . . ? C69 C72 C77 U3 109.1(17) . . . . ? C73 C74 C78 C81 -117.5(16) . . . . ? C75 C74 C78 C81 58.1(18) . . . . ? U3 C74 C78 C81 -33.2(13) . . . . ? C73 C74 C78 C80 3(2) . . . . ? C75 C74 C78 C80 178.6(16) . . . . ? U3 C74 C78 C80 87.4(14) . . . . ? C73 C74 C78 C79 123.9(16) . . . . ? C75 C74 C78 C79 -60.6(19) . . . . ? U3 C74 C78 C79 -151.9(10) . . . . ? C80 C78 C81 C82 77.8(19) . . . . ? C79 C78 C81 C82 -42(2) . . . . ? C74 C78 C81 C82 -159.9(15) . . . . ? C80 C78 C81 N6 -93.8(15) . . . . ? C79 C78 C81 N6 146.8(13) . . . . ? C74 C78 C81 N6 28.5(19) . . . . ? N6 C81 C82 C83 0.4(17) . . . . ? C78 C81 C82 C83 -172.1(15) . . . . ? C81 C82 C83 C84 0.2(18) . . . . ? C82 C83 C84 N6 -0.7(18) . . . . ? C82 C83 C84 C85 -177.4(15) . . . . ? C83 C84 C85 C88 -155.8(16) . . . . ? N6 C84 C85 C88 27.9(18) . . . . ? C83 C84 C85 C87 -36(2) . . . . ? N6 C84 C85 C87 147.8(13) . . . . ? C83 C84 C85 C86 83(2) . . . . ? N6 C84 C85 C86 -93.8(15) . . . . ? C84 C85 C88 C93 -129.6(17) . . . . ? C87 C85 C88 C93 109.8(19) . . . . ? C86 C85 C88 C93 -9(2) . . . . ? C84 C85 C88 C89 49.9(19) . . . . ? C87 C85 C88 C89 -70.7(19) . . . . ? C86 C85 C88 C89 170.2(15) . . . . ? C84 C85 C88 U3 -34.2(13) . . . . ? C87 C85 C88 U3 -154.8(11) . . . . ? C86 C85 C88 U3 86.1(14) . . . . ? C93 C88 C89 C90 7(3) . . . . ? C85 C88 C89 C90 -172.8(15) . . . . ? U3 C88 C89 C90 -66.0(15) . . . . ? C93 C88 C89 U3 72.8(15) . . . . ? C85 C88 C89 U3 -106.8(14) . . . . ? C88 C89 C90 C91 -5(2) . . . . ? U3 C89 C90 C91 -70.2(14) . . . . ? C88 C89 C90 C94 172.6(16) . . . . ? U3 C89 C90 C94 107.6(16) . . . . ? C88 C89 C90 U3 65.0(14) . . . . ? C89 C90 C91 C92 2(3) . . . . ? C94 C90 C91 C92 -176.4(16) . . . . ? U3 C90 C91 C92 -64.8(16) . . . . ? C89 C90 C91 U3 66.4(14) . . . . ? C94 C90 C91 U3 -111.6(15) . . . . ? C90 C91 C92 C93 0(3) . . . . ? U3 C91 C92 C93 -60.8(16) . . . . ? C89 C88 C93 C92 -5(3) . . . . ? C85 C88 C93 C92 175.0(15) . . . . ? U3 C88 C93 C92 64.1(15) . . . . ? C89 C88 C93 U3 -68.7(14) . . . . ? C85 C88 C93 U3 110.9(16) . . . . ? C91 C92 C93 C88 1(3) . . . . ? C91 C92 C93 U3 61.0(16) . . . . ? C89 C90 C94 C96 123.1(16) . . . . ? C91 C90 C94 C96 -59(2) . . . . ? U3 C90 C94 C96 -150.8(10) . . . . ? C89 C90 C94 C65 -116.4(17) . . . . ? C91 C90 C94 C65 61.4(19) . . . . ? U3 C90 C94 C65 -30.3(12) . . . . ? C89 C90 C94 C95 3(2) . . . . ? C91 C90 C94 C95 -179.6(16) . . . . ? U3 C90 C94 C95 88.6(14) . . . . ? C66 C65 C94 C90 -162.4(15) . . . . ? N5 C65 C94 C90 23.6(18) . . . . ? C66 C65 C94 C96 -43(2) . . . . ? N5 C65 C94 C96 143.3(14) . . . . ? C66 C65 C94 C95 76.1(19) . . . . ? N5 C65 C94 C95 -97.8(15) . . . . ? N7 C97 C98 C99 0.6(18) 2 . . . ? C110 C97 C98 C99 -179.8(14) . . . . ? C97 C98 C99 C100 -1.4(17) . . . 2 ? C99 C100 C101 C104 164.0(13) 2 . . . ? N7 C100 C101 C104 -23.6(17) . . . . ? C99 C100 C101 C102 -73.5(18) 2 . . . ? N7 C100 C101 C102 98.9(15) . . . . ? C99 C100 C101 C103 44(2) 2 . . . ? N7 C100 C101 C103 -143.3(13) . . . . ? C100 C101 C104 C109 117.9(16) . . . . ? C102 C101 C104 C109 -3(2) . . . . ? C103 C101 C104 C109 -121.7(16) . . . . ? C100 C101 C104 C105 -58.6(18) . . . . ? C102 C101 C104 C105 -179.9(16) . . . . ? C103 C101 C104 C105 61.8(18) . . . . ? C100 C101 C104 U4 32.3(12) . . . . ? C102 C101 C104 U4 -89.0(14) . . . . ? C103 C101 C104 U4 152.7(10) . . . . ? C109 C104 C105 C106 -1(2) . . . . ? C101 C104 C105 C106 176.0(16) . . . . ? U4 C104 C105 C106 66.1(16) . . . . ? C109 C104 C105 U4 -66.7(13) . . . . ? C101 C104 C105 U4 109.9(13) . . . . ? C104 C105 C106 C107 -2(3) . . . . ? U4 C105 C106 C107 59.7(17) . . . . ? C104 C105 C106 U4 -62.1(15) . . . . ? C105 C106 C107 C108 0(3) . . . . ? U4 C106 C107 C108 60.4(16) . . . . ? C105 C106 C107 U4 -59.9(17) . . . . ? C106 C107 C108 C109 4(3) . . . . ? U4 C107 C108 C109 68.8(14) . . . . ? C106 C107 C108 C110 -173.3(16) . . . . ? U4 C107 C108 C110 -108.8(17) . . . . ? C106 C107 C108 U4 -64.5(16) . . . . ? C105 C104 C109 C108 6(2) . . . . ? C101 C104 C109 C108 -170.8(15) . . . . ? U4 C104 C109 C108 -64.2(15) . . . . ? C105 C104 C109 U4 69.8(14) . . . . ? C101 C104 C109 U4 -106.7(14) . . . . ? C107 C108 C109 C104 -7(2) . . . . ? C110 C108 C109 C104 170.4(15) . . . . ? U4 C108 C109 C104 65.0(15) . . . . ? C107 C108 C109 U4 -72.4(14) . . . . ? C110 C108 C109 U4 105.4(14) . . . . ? C107 C108 C110 C97 131.1(17) . . . . ? C109 C108 C110 C97 -46.5(19) . . . . ? U4 C108 C110 C97 37.1(13) . . . . ? C107 C108 C110 C111 10(2) . . . . ? C109 C108 C110 C111 -167.9(15) . . . . ? U4 C108 C110 C111 -84.3(14) . . . . ? C107 C108 C110 C112 -109.1(19) . . . . ? C109 C108 C110 C112 73.3(19) . . . . ? U4 C108 C110 C112 156.9(10) . . . . ? N7 C97 C110 C108 -32.3(18) 2 . . . ? C98 C97 C110 C108 148.1(15) . . . . ? N7 C97 C110 C111 87.9(16) 2 . . . ? C98 C97 C110 C111 -91.7(19) . . . . ? N7 C97 C110 C112 -150.9(13) 2 . . . ? C98 C97 C110 C112 29(2) . . . . ? C2 C1 N1 C4 -1.3(16) . . . . ? C30 C1 N1 C4 -179.8(13) . . . . ? C2 C1 N1 U1 -172.4(9) . . . . ? C30 C1 N1 U1 9.1(19) . . . . ? C3 C4 N1 C1 0.6(15) . . . . ? C5 C4 N1 C1 -175.2(13) . . . . ? C3 C4 N1 U1 171.6(9) . . . . ? C5 C4 N1 U1 -4.2(19) . . . . ? C19 C20 N2 C17 -0.9(16) . . . . ? C21 C20 N2 C17 -175.9(12) . . . . ? C19 C20 N2 U1 178.1(9) . . . . ? C21 C20 N2 U1 3.0(19) . . . . ? C18 C17 N2 C20 1.0(16) . . . . ? C14 C17 N2 C20 -179.5(13) . . . . ? C18 C17 N2 U1 -178.0(9) . . . . ? C14 C17 N2 U1 1.5(19) . . . . ? C34 C33 N3 C36 -0.8(16) . . . . ? C62 C33 N3 C36 -175.6(13) . . . . ? C34 C33 N3 U2 173.0(9) . . . . ? C62 C33 N3 U2 -1.8(19) . . . . ? C35 C36 N3 C33 0.6(16) . . . . ? C37 C36 N3 C33 -177.5(13) . . . . ? C35 C36 N3 U2 -173.5(9) . . . . ? C37 C36 N3 U2 8(2) . . . . ? C50 C49 N4 C52 0.8(17) . . . . ? C46 C49 N4 C52 -172.4(14) . . . . ? C50 C49 N4 U2 179.2(10) . . . . ? C46 C49 N4 U2 6(2) . . . . ? C51 C52 N4 C49 -1.0(16) . . . . ? C53 C52 N4 C49 -178.9(14) . . . . ? C51 C52 N4 U2 -179.5(10) . . . . ? C53 C52 N4 U2 2.7(19) . . . . ? C67 C68 N5 C65 -0.5(16) . . . . ? C69 C68 N5 C65 178.0(12) . . . . ? C67 C68 N5 U3 175.9(10) . . . . ? C69 C68 N5 U3 -5.7(18) . . . . ? C66 C65 N5 C68 0.0(16) . . . . ? C94 C65 N5 C68 174.8(13) . . . . ? C66 C65 N5 U3 -176.4(10) . . . . ? C94 C65 N5 U3 -1.5(19) . . . . ? C83 C84 N6 C81 0.9(16) . . . . ? C85 C84 N6 C81 177.9(13) . . . . ? C83 C84 N6 U3 179.0(10) . . . . ? C85 C84 N6 U3 -4.0(18) . . . . ? C82 C81 N6 C84 -0.8(15) . . . . ? C78 C81 N6 C84 172.3(13) . . . . ? C82 C81 N6 U3 -178.9(9) . . . . ? C78 C81 N6 U3 -5.8(19) . . . . ? C99 C100 N7 C97 -1.4(14) 2 . . 2 ? C101 C100 N7 C97 -175.0(12) . . . 2 ? C99 C100 N7 U4 172.2(9) 2 . . . ? C101 C100 N7 U4 -1.4(17) . . . . ? C20 N2 U1 N1 -63.9(12) . . . . ? C17 N2 U1 N1 114.9(11) . . . . ? C20 N2 U1 C9 -132.7(12) . . . . ? C17 N2 U1 C9 46.1(11) . . . . ? C20 N2 U1 C25 -4.6(11) . . . . ? C17 N2 U1 C25 174.2(12) . . . . ? C20 N2 U1 C26 5.8(13) . . . . ? C17 N2 U1 C26 -175.4(11) . . . . ? C20 N2 U1 C10 -164.8(13) . . . . ? C17 N2 U1 C10 14.0(10) . . . . ? C20 N2 U1 C8 -121.3(12) . . . . ? C17 N2 U1 C8 57.5(11) . . . . ? C20 N2 U1 C24 11.3(11) . . . . ? C17 N2 U1 C24 -170.0(12) . . . . ? C20 N2 U1 C13 -137.7(11) . . . . ? C17 N2 U1 C13 41.0(12) . . . . ? C20 N2 U1 C11 -178.0(12) . . . . ? C17 N2 U1 C11 0.7(11) . . . . ? C20 N2 U1 C27 35.3(12) . . . . ? C17 N2 U1 C27 -145.9(11) . . . . ? C20 N2 U1 C29 41.3(11) . . . . ? C17 N2 U1 C29 -139.9(12) . . . . ? C1 N1 U1 N2 110.6(11) . . . . ? C4 N1 U1 N2 -58.7(12) . . . . ? C1 N1 U1 C9 168.8(12) . . . . ? C4 N1 U1 C9 -0.6(11) . . . . ? C1 N1 U1 C25 40.8(11) . . . . ? C4 N1 U1 C25 -128.5(12) . . . . ? C1 N1 U1 C26 9.5(11) . . . . ? C4 N1 U1 C26 -159.8(12) . . . . ? C1 N1 U1 C10 -179.9(11) . . . . ? C4 N1 U1 C10 10.8(12) . . . . ? C1 N1 U1 C8 -175.6(12) . . . . ? C4 N1 U1 C8 15.0(10) . . . . ? C1 N1 U1 C24 52.0(11) . . . . ? C4 N1 U1 C24 -117.3(11) . . . . ? C1 N1 U1 C13 -144.7(12) . . . . ? C4 N1 U1 C13 46.0(11) . . . . ? C1 N1 U1 C11 -150.5(11) . . . . ? C4 N1 U1 C11 40.2(12) . . . . ? C1 N1 U1 C27 -4.4(11) . . . . ? C4 N1 U1 C27 -173.7(11) . . . . ? C1 N1 U1 C29 35.2(12) . . . . ? C4 N1 U1 C29 -134.1(11) . . . . ? C8 C9 U1 N2 154.8(9) . . . . ? C10 C9 U1 N2 -77.9(8) . . . . ? C8 C9 U1 N1 30.4(8) . . . . ? C10 C9 U1 N1 157.7(9) . . . . ? C8 C9 U1 C25 88.0(9) . . . . ? C10 C9 U1 C25 -144.8(8) . . . . ? C8 C9 U1 C26 61.1(11) . . . . ? C10 C9 U1 C26 -171.6(8) . . . . ? C8 C9 U1 C10 -127.3(13) . . . . ? C10 C9 U1 C8 127.3(13) . . . . ? C8 C9 U1 C24 119.3(8) . . . . ? C10 C9 U1 C24 -113.5(8) . . . . ? C8 C9 U1 C13 -31.3(8) . . . . ? C10 C9 U1 C13 96.0(9) . . . . ? C8 C9 U1 C11 -96.3(9) . . . . ? C10 C9 U1 C11 31.0(8) . . . . ? C8 C9 U1 C27 69(2) . . . . ? C10 C9 U1 C27 -163.5(19) . . . . ? C8 C9 U1 C29 147.5(8) . . . . ? C10 C9 U1 C29 -85.3(9) . . . . ? C24 C25 U1 N2 31.3(9) . . . . ? C26 C25 U1 N2 159.2(9) . . . . ? C24 C25 U1 N1 155.2(10) . . . . ? C26 C25 U1 N1 -76.9(9) . . . . ? C24 C25 U1 C9 88.1(9) . . . . ? C26 C25 U1 C9 -144.0(8) . . . . ? C24 C25 U1 C26 -127.9(13) . . . . ? C24 C25 U1 C10 60.9(11) . . . . ? C26 C25 U1 C10 -171.2(8) . . . . ? C24 C25 U1 C8 119.5(9) . . . . ? C26 C25 U1 C8 -112.6(8) . . . . ? C26 C25 U1 C24 127.9(13) . . . . ? C24 C25 U1 C13 148.5(8) . . . . ? C26 C25 U1 C13 -83.6(9) . . . . ? C24 C25 U1 C11 70(2) . . . . ? C26 C25 U1 C11 -161.8(19) . . . . ? C24 C25 U1 C27 -96.6(10) . . . . ? C26 C25 U1 C27 31.3(8) . . . . ? C24 C25 U1 C29 -31.7(8) . . . . ? C26 C25 U1 C29 96.1(10) . . . . ? C25 C26 U1 N2 -22.4(10) . . . . ? C27 C26 U1 N2 99.9(9) . . . . ? C30 C26 U1 N2 -136.8(10) . . . . ? C25 C26 U1 N1 89.2(9) . . . . ? C27 C26 U1 N1 -148.5(10) . . . . ? C30 C26 U1 N1 -25.2(9) . . . . ? C25 C26 U1 C9 54.3(11) . . . . ? C27 C26 U1 C9 176.7(8) . . . . ? C30 C26 U1 C9 -60.1(12) . . . . ? C27 C26 U1 C25 122.3(13) . . . . ? C30 C26 U1 C25 -114.5(15) . . . . ? C25 C26 U1 C10 31(3) . . . . ? C27 C26 U1 C10 154(2) . . . . ? C30 C26 U1 C10 -83(2) . . . . ? C25 C26 U1 C8 83.8(9) . . . . ? C27 C26 U1 C8 -153.9(9) . . . . ? C30 C26 U1 C8 -30.7(12) . . . . ? C25 C26 U1 C24 -28.6(8) . . . . ? C27 C26 U1 C24 93.7(10) . . . . ? C30 C26 U1 C24 -143.1(12) . . . . ? C25 C26 U1 C13 117.3(8) . . . . ? C27 C26 U1 C13 -120.4(9) . . . . ? C30 C26 U1 C13 2.8(12) . . . . ? C25 C26 U1 C11 169.8(11) . . . . ? C27 C26 U1 C11 -67.9(17) . . . . ? C30 C26 U1 C11 55.3(18) . . . . ? C25 C26 U1 C27 -122.3(13) . . . . ? C30 C26 U1 C27 123.2(15) . . . . ? C25 C26 U1 C29 -62.3(8) . . . . ? C27 C26 U1 C29 60.1(9) . . . . ? C30 C26 U1 C29 -176.7(12) . . . . ? C11 C10 U1 N2 -150.0(10) . . . . ? C9 C10 U1 N2 87.6(9) . . . . ? C14 C10 U1 N2 -26.9(9) . . . . ? C11 C10 U1 N1 98.4(9) . . . . ? C9 C10 U1 N1 -23.9(9) . . . . ? C14 C10 U1 N1 -138.5(9) . . . . ? C11 C10 U1 C9 122.3(13) . . . . ? C14 C10 U1 C9 -114.6(14) . . . . ? C11 C10 U1 C25 176.3(8) . . . . ? C9 C10 U1 C25 54.0(11) . . . . ? C14 C10 U1 C25 -60.6(12) . . . . ? C11 C10 U1 C26 152.5(19) . . . . ? C9 C10 U1 C26 30(3) . . . . ? C14 C10 U1 C26 -84(2) . . . . ? C11 C10 U1 C8 93.5(9) . . . . ? C9 C10 U1 C8 -28.8(7) . . . . ? C14 C10 U1 C8 -143.4(12) . . . . ? C11 C10 U1 C24 -154.3(8) . . . . ? C9 C10 U1 C24 83.4(9) . . . . ? C14 C10 U1 C24 -31.1(11) . . . . ? C11 C10 U1 C13 59.7(8) . . . . ? C9 C10 U1 C13 -62.6(8) . . . . ? C14 C10 U1 C13 -177.1(11) . . . . ? C9 C10 U1 C11 -122.3(13) . . . . ? C14 C10 U1 C11 123.1(14) . . . . ? C11 C10 U1 C27 -67.5(17) . . . . ? C9 C10 U1 C27 170.2(12) . . . . ? C14 C10 U1 C27 55.7(18) . . . . ? C11 C10 U1 C29 -120.9(9) . . . . ? C9 C10 U1 C29 116.8(8) . . . . ? C14 C10 U1 C29 2.2(11) . . . . ? C9 C8 U1 N2 -22.7(8) . . . . ? C13 C8 U1 N2 -146.3(9) . . . . ? C5 C8 U1 N2 97.9(9) . . . . ? C9 C8 U1 N1 -144.9(9) . . . . ? C13 C8 U1 N1 91.5(9) . . . . ? C5 C8 U1 N1 -24.3(8) . . . . ? C13 C8 U1 C9 -123.6(13) . . . . ? C5 C8 U1 C9 120.6(13) . . . . ? C9 C8 U1 C25 -107.6(9) . . . . ? C13 C8 U1 C25 128.8(8) . . . . ? C5 C8 U1 C25 13.0(10) . . . . ? C9 C8 U1 C26 -139.4(8) . . . . ? C13 C8 U1 C26 97.0(9) . . . . ? C5 C8 U1 C26 -18.8(11) . . . . ? C9 C8 U1 C10 29.9(8) . . . . ? C13 C8 U1 C10 -93.6(9) . . . . ? C5 C8 U1 C10 150.6(11) . . . . ? C9 C8 U1 C24 -77.2(9) . . . . ? C13 C8 U1 C24 159.2(8) . . . . ? C5 C8 U1 C24 43.4(11) . . . . ? C9 C8 U1 C13 123.6(13) . . . . ? C5 C8 U1 C13 -115.8(13) . . . . ? C9 C8 U1 C11 62.9(8) . . . . ? C13 C8 U1 C11 -60.6(8) . . . . ? C5 C8 U1 C11 -176.4(11) . . . . ? C9 C8 U1 C27 -161.0(8) . . . . ? C13 C8 U1 C27 75.4(11) . . . . ? C5 C8 U1 C27 -40.4(13) . . . . ? C9 C8 U1 C29 -58.4(13) . . . . ? C13 C8 U1 C29 178.0(8) . . . . ? C5 C8 U1 C29 62.2(13) . . . . ? C25 C24 U1 N2 -144.1(10) . . . . ? C29 C24 U1 N2 93.5(9) . . . . ? C21 C24 U1 N2 -23.4(8) . . . . ? C25 C24 U1 N1 -22.5(9) . . . . ? C29 C24 U1 N1 -144.9(9) . . . . ? C21 C24 U1 N1 98.1(9) . . . . ? C25 C24 U1 C9 -107.4(9) . . . . ? C29 C24 U1 C9 130.2(8) . . . . ? C21 C24 U1 C9 13.3(10) . . . . ? C29 C24 U1 C25 -122.4(13) . . . . ? C21 C24 U1 C25 120.7(13) . . . . ? C25 C24 U1 C26 29.3(8) . . . . ? C29 C24 U1 C26 -93.1(10) . . . . ? C21 C24 U1 C26 150.0(11) . . . . ? C25 C24 U1 C10 -139.8(8) . . . . ? C29 C24 U1 C10 97.8(9) . . . . ? C21 C24 U1 C10 -19.2(10) . . . . ? C25 C24 U1 C8 -76.8(10) . . . . ? C29 C24 U1 C8 160.8(8) . . . . ? C21 C24 U1 C8 43.9(10) . . . . ? C25 C24 U1 C13 -56.2(13) . . . . ? C29 C24 U1 C13 -178.6(8) . . . . ? C21 C24 U1 C13 64.5(12) . . . . ? C25 C24 U1 C11 -161.5(9) . . . . ? C29 C24 U1 C11 76.1(12) . . . . ? C21 C24 U1 C11 -40.8(12) . . . . ? C25 C24 U1 C27 62.5(9) . . . . ? C29 C24 U1 C27 -59.9(9) . . . . ? C21 C24 U1 C27 -176.8(10) . . . . ? C25 C24 U1 C29 122.4(13) . . . . ? C21 C24 U1 C29 -117.0(13) . . . . ? C12 C13 U1 N2 -88.9(9) . . . . ? C8 C13 U1 N2 37.2(9) . . . . ? C12 C13 U1 N1 159.5(10) . . . . ? C8 C13 U1 N1 -74.4(8) . . . . ? C12 C13 U1 C9 -94.9(10) . . . . ? C8 C13 U1 C9 31.2(8) . . . . ? C12 C13 U1 C25 166.2(8) . . . . ? C8 C13 U1 C25 -67.7(10) . . . . ? C12 C13 U1 C26 132.2(9) . . . . ? C8 C13 U1 C26 -101.7(9) . . . . ? C12 C13 U1 C10 -60.1(9) . . . . ? C8 C13 U1 C10 66.0(9) . . . . ? C12 C13 U1 C8 -126.1(13) . . . . ? C12 C13 U1 C24 -163.0(9) . . . . ? C8 C13 U1 C24 -36.9(13) . . . . ? C12 C13 U1 C11 -27.7(8) . . . . ? C8 C13 U1 C11 98.3(9) . . . . ? C12 C13 U1 C27 99.8(9) . . . . ? C8 C13 U1 C27 -134.1(8) . . . . ? C12 C13 U1 C29 155(25) . . . . ? C8 C13 U1 C29 -79(25) . . . . ? C10 C11 U1 N2 26.4(9) . . . . ? C12 C11 U1 N2 154.4(9) . . . . ? C10 C11 U1 N1 -92.9(9) . . . . ? C12 C11 U1 N1 35.1(9) . . . . ? C10 C11 U1 C9 -32.9(8) . . . . ? C12 C11 U1 C9 95.1(10) . . . . ? C10 C11 U1 C25 -13(3) . . . . ? C12 C11 U1 C25 115(2) . . . . ? C10 C11 U1 C26 -164.9(12) . . . . ? C12 C11 U1 C26 -37.0(17) . . . . ? C12 C11 U1 C10 128.0(13) . . . . ? C10 C11 U1 C8 -66.5(9) . . . . ? C12 C11 U1 C8 61.5(9) . . . . ? C10 C11 U1 C24 41.7(12) . . . . ? C12 C11 U1 C24 169.7(8) . . . . ? C10 C11 U1 C13 -100.1(10) . . . . ? C12 C11 U1 C13 27.9(8) . . . . ? C10 C11 U1 C27 151.5(8) . . . . ? C12 C11 U1 C27 -80.5(10) . . . . ? C10 C11 U1 C29 79.9(10) . . . . ? C12 C11 U1 C29 -152.2(8) . . . . ? C26 C27 U1 N2 -91.6(9) . . . . ? C28 C27 U1 N2 34.5(10) . . . . ? C26 C27 U1 N1 27.8(9) . . . . ? C28 C27 U1 N1 153.9(9) . . . . ? C26 C27 U1 C9 -11(3) . . . . ? C28 C27 U1 C9 115(2) . . . . ? C26 C27 U1 C25 -32.5(8) . . . . ? C28 C27 U1 C25 93.6(10) . . . . ? C28 C27 U1 C26 126.1(14) . . . . ? C26 C27 U1 C10 -165.4(12) . . . . ? C28 C27 U1 C10 -39.3(18) . . . . ? C26 C27 U1 C8 41.9(13) . . . . ? C28 C27 U1 C8 168.0(8) . . . . ? C26 C27 U1 C24 -66.0(9) . . . . ? C28 C27 U1 C24 60.1(9) . . . . ? C26 C27 U1 C13 79.8(10) . . . . ? C28 C27 U1 C13 -154.1(8) . . . . ? C26 C27 U1 C11 151.3(8) . . . . ? C28 C27 U1 C11 -82.6(10) . . . . ? C26 C27 U1 C29 -99.2(10) . . . . ? C28 C27 U1 C29 26.9(8) . . . . ? C28 C29 U1 N2 159.5(9) . . . . ? C24 C29 U1 N2 -73.2(9) . . . . ? C28 C29 U1 N1 -88.5(9) . . . . ? C24 C29 U1 N1 38.8(10) . . . . ? C28 C29 U1 C9 166.8(8) . . . . ? C24 C29 U1 C9 -66.0(10) . . . . ? C28 C29 U1 C25 -95.3(10) . . . . ? C24 C29 U1 C25 31.9(8) . . . . ? C28 C29 U1 C26 -60.9(9) . . . . ? C24 C29 U1 C26 66.3(9) . . . . ? C28 C29 U1 C10 131.5(8) . . . . ? C24 C29 U1 C10 -101.2(9) . . . . ? C28 C29 U1 C8 -161.1(9) . . . . ? C24 C29 U1 C8 -33.9(13) . . . . ? C28 C29 U1 C24 -127.2(13) . . . . ? C28 C29 U1 C13 -84(25) . . . . ? C24 C29 U1 C13 44(26) . . . . ? C28 C29 U1 C11 98.8(9) . . . . ? C24 C29 U1 C11 -133.9(8) . . . . ? C28 C29 U1 C27 -28.0(8) . . . . ? C24 C29 U1 C27 99.2(10) . . . . ? C33 N3 U2 N4 -61.4(13) . . . . ? C36 N3 U2 N4 111.3(11) . . . . ? C33 N3 U2 C41 -130.7(12) . . . . ? C36 N3 U2 C41 42.0(11) . . . . ? C33 N3 U2 C61 -2.5(12) . . . . ? C36 N3 U2 C61 170.2(12) . . . . ? C33 N3 U2 C40 -162.7(13) . . . . ? C36 N3 U2 C40 10.0(11) . . . . ? C33 N3 U2 C56 8.1(13) . . . . ? C36 N3 U2 C56 -179.2(11) . . . . ? C33 N3 U2 C60 13.6(11) . . . . ? C36 N3 U2 C60 -173.7(13) . . . . ? C33 N3 U2 C42 -119.1(12) . . . . ? C36 N3 U2 C42 53.6(11) . . . . ? C33 N3 U2 C57 37.5(13) . . . . ? C36 N3 U2 C57 -149.8(11) . . . . ? C33 N3 U2 C59 43.6(11) . . . . ? C36 N3 U2 C59 -143.7(12) . . . . ? C33 N3 U2 C43 -136.0(11) . . . . ? C36 N3 U2 C43 36.7(12) . . . . ? C33 N3 U2 C45 -176.0(12) . . . . ? C36 N3 U2 C45 -3.3(11) . . . . ? C49 N4 U2 N3 -64.7(13) . . . . ? C52 N4 U2 N3 113.5(11) . . . . ? C49 N4 U2 C41 -5.7(12) . . . . ? C52 N4 U2 C41 172.4(12) . . . . ? C49 N4 U2 C61 -133.5(13) . . . . ? C52 N4 U2 C61 44.6(11) . . . . ? C49 N4 U2 C40 5.7(13) . . . . ? C52 N4 U2 C40 -176.1(11) . . . . ? C49 N4 U2 C56 -164.9(13) . . . . ? C52 N4 U2 C56 13.2(11) . . . . ? C49 N4 U2 C60 -122.4(12) . . . . ? C52 N4 U2 C60 55.7(11) . . . . ? C49 N4 U2 C42 10.0(11) . . . . ? C52 N4 U2 C42 -171.8(13) . . . . ? C49 N4 U2 C57 -179.4(13) . . . . ? C52 N4 U2 C57 -1.3(11) . . . . ? C49 N4 U2 C59 -139.1(12) . . . . ? C52 N4 U2 C59 39.0(12) . . . . ? C49 N4 U2 C43 40.6(12) . . . . ? C52 N4 U2 C43 -141.3(12) . . . . ? C49 N4 U2 C45 34.7(13) . . . . ? C52 N4 U2 C45 -147.2(11) . . . . ? C42 C41 U2 N3 154.6(10) . . . . ? C40 C41 U2 N3 -78.3(8) . . . . ? C42 C41 U2 N4 30.4(9) . . . . ? C40 C41 U2 N4 157.5(8) . . . . ? C42 C41 U2 C61 88.3(9) . . . . ? C40 C41 U2 C61 -144.6(8) . . . . ? C42 C41 U2 C40 -127.1(13) . . . . ? C42 C41 U2 C56 61.3(11) . . . . ? C40 C41 U2 C56 -171.6(8) . . . . ? C42 C41 U2 C60 119.8(9) . . . . ? C40 C41 U2 C60 -113.1(8) . . . . ? C40 C41 U2 C42 127.1(13) . . . . ? C42 C41 U2 C57 66(2) . . . . ? C40 C41 U2 C57 -166.7(19) . . . . ? C42 C41 U2 C59 147.7(8) . . . . ? C40 C41 U2 C59 -85.2(9) . . . . ? C42 C41 U2 C43 -31.9(8) . . . . ? C40 C41 U2 C43 95.2(9) . . . . ? C42 C41 U2 C45 -96.7(10) . . . . ? C40 C41 U2 C45 30.3(7) . . . . ? C60 C61 U2 N3 31.4(9) . . . . ? C56 C61 U2 N3 159.0(9) . . . . ? C60 C61 U2 N4 155.8(10) . . . . ? C56 C61 U2 N4 -76.7(9) . . . . ? C60 C61 U2 C41 88.4(10) . . . . ? C56 C61 U2 C41 -144.0(8) . . . . ? C60 C61 U2 C40 61.1(12) . . . . ? C56 C61 U2 C40 -171.3(8) . . . . ? C60 C61 U2 C56 -127.6(14) . . . . ? C56 C61 U2 C60 127.6(14) . . . . ? C60 C61 U2 C42 120.1(9) . . . . ? C56 C61 U2 C42 -112.3(9) . . . . ? C60 C61 U2 C57 -96.9(10) . . . . ? C56 C61 U2 C57 30.6(8) . . . . ? C60 C61 U2 C59 -31.2(8) . . . . ? C56 C61 U2 C59 96.3(10) . . . . ? C60 C61 U2 C43 148.5(8) . . . . ? C56 C61 U2 C43 -83.9(10) . . . . ? C60 C61 U2 C45 68(3) . . . . ? C56 C61 U2 C45 -164.4(19) . . . . ? C45 C40 U2 N3 -149.4(10) . . . . ? C41 C40 U2 N3 87.6(8) . . . . ? C37 C40 U2 N3 -25.5(9) . . . . ? C45 C40 U2 N4 98.8(9) . . . . ? C41 C40 U2 N4 -24.2(9) . . . . ? C37 C40 U2 N4 -137.3(9) . . . . ? C45 C40 U2 C41 123.0(13) . . . . ? C37 C40 U2 C41 -113.1(13) . . . . ? C45 C40 U2 C61 177.1(8) . . . . ? C41 C40 U2 C61 54.2(11) . . . . ? C37 C40 U2 C61 -58.9(12) . . . . ? C45 C40 U2 C56 153(2) . . . . ? C41 C40 U2 C56 30(3) . . . . ? C37 C40 U2 C56 -83(3) . . . . ? C45 C40 U2 C60 -153.2(8) . . . . ? C41 C40 U2 C60 83.8(9) . . . . ? C37 C40 U2 C60 -29.3(11) . . . . ? C45 C40 U2 C42 93.9(10) . . . . ? C41 C40 U2 C42 -29.0(7) . . . . ? C37 C40 U2 C42 -142.2(11) . . . . ? C45 C40 U2 C57 -64.8(17) . . . . ? C41 C40 U2 C57 172.3(12) . . . . ? C37 C40 U2 C57 59.1(17) . . . . ? C45 C40 U2 C59 -120.4(9) . . . . ? C41 C40 U2 C59 116.7(8) . . . . ? C37 C40 U2 C59 3.6(11) . . . . ? C45 C40 U2 C43 60.1(9) . . . . ? C41 C40 U2 C43 -62.9(8) . . . . ? C37 C40 U2 C43 -176.0(11) . . . . ? C41 C40 U2 C45 -123.0(13) . . . . ? C37 C40 U2 C45 123.9(14) . . . . ? C57 C56 U2 N3 101.1(9) . . . . ? C61 C56 U2 N3 -22.5(10) . . . . ? C53 C56 U2 N3 -138.3(10) . . . . ? C57 C56 U2 N4 -147.0(10) . . . . ? C61 C56 U2 N4 89.5(9) . . . . ? C53 C56 U2 N4 -26.3(10) . . . . ? C57 C56 U2 C41 178.0(8) . . . . ? C61 C56 U2 C41 54.4(11) . . . . ? C53 C56 U2 C41 -61.4(12) . . . . ? C57 C56 U2 C61 123.6(14) . . . . ? C53 C56 U2 C61 -115.8(15) . . . . ? C57 C56 U2 C40 155(2) . . . . ? C61 C56 U2 C40 31(3) . . . . ? C53 C56 U2 C40 -85(3) . . . . ? C57 C56 U2 C60 94.7(10) . . . . ? C61 C56 U2 C60 -28.8(8) . . . . ? C53 C56 U2 C60 -144.7(12) . . . . ? C57 C56 U2 C42 -152.3(9) . . . . ? C61 C56 U2 C42 84.2(9) . . . . ? C53 C56 U2 C42 -31.7(12) . . . . ? C61 C56 U2 C57 -123.6(14) . . . . ? C53 C56 U2 C57 120.6(15) . . . . ? C57 C56 U2 C59 61.6(9) . . . . ? C61 C56 U2 C59 -62.0(9) . . . . ? C53 C56 U2 C59 -177.8(12) . . . . ? C57 C56 U2 C43 -118.9(9) . . . . ? C61 C56 U2 C43 117.6(9) . . . . ? C53 C56 U2 C43 1.8(12) . . . . ? C57 C56 U2 C45 -65.7(17) . . . . ? C61 C56 U2 C45 170.7(12) . . . . ? C53 C56 U2 C45 54.9(19) . . . . ? C61 C60 U2 N3 -143.7(10) . . . . ? C59 C60 U2 N3 93.5(9) . . . . ? C62 C60 U2 N3 -23.1(8) . . . . ? C61 C60 U2 N4 -22.1(9) . . . . ? C59 C60 U2 N4 -144.9(9) . . . . ? C62 C60 U2 N4 98.5(9) . . . . ? C61 C60 U2 C41 -107.2(9) . . . . ? C59 C60 U2 C41 130.0(8) . . . . ? C62 C60 U2 C41 13.4(10) . . . . ? C59 C60 U2 C61 -122.8(13) . . . . ? C62 C60 U2 C61 120.5(14) . . . . ? C61 C60 U2 C40 -139.8(9) . . . . ? C59 C60 U2 C40 97.4(9) . . . . ? C62 C60 U2 C40 -19.2(11) . . . . ? C61 C60 U2 C56 29.5(9) . . . . ? C59 C60 U2 C56 -93.3(10) . . . . ? C62 C60 U2 C56 150.1(11) . . . . ? C61 C60 U2 C42 -76.3(10) . . . . ? C59 C60 U2 C42 160.9(8) . . . . ? C62 C60 U2 C42 44.2(11) . . . . ? C61 C60 U2 C57 62.5(9) . . . . ? C59 C60 U2 C57 -60.3(9) . . . . ? C62 C60 U2 C57 -176.9(11) . . . . ? C61 C60 U2 C59 122.8(13) . . . . ? C62 C60 U2 C59 -116.6(13) . . . . ? C61 C60 U2 C43 -57.3(13) . . . . ? C59 C60 U2 C43 179.9(8) . . . . ? C62 C60 U2 C43 63.3(13) . . . . ? C61 C60 U2 C45 -161.4(9) . . . . ? C59 C60 U2 C45 75.7(11) . . . . ? C62 C60 U2 C45 -40.9(13) . . . . ? C41 C42 U2 N3 -23.0(9) . . . . ? C43 C42 U2 N3 -145.1(8) . . . . ? C46 C42 U2 N3 98.1(9) . . . . ? C41 C42 U2 N4 -144.8(10) . . . . ? C43 C42 U2 N4 93.1(9) . . . . ? C46 C42 U2 N4 -23.7(9) . . . . ? C43 C42 U2 C41 -122.1(13) . . . . ? C46 C42 U2 C41 121.1(14) . . . . ? C41 C42 U2 C61 -107.4(9) . . . . ? C43 C42 U2 C61 130.6(8) . . . . ? C46 C42 U2 C61 13.7(10) . . . . ? C41 C42 U2 C40 30.0(8) . . . . ? C43 C42 U2 C40 -92.1(9) . . . . ? C46 C42 U2 C40 151.1(11) . . . . ? C41 C42 U2 C56 -139.4(9) . . . . ? C43 C42 U2 C56 98.5(9) . . . . ? C46 C42 U2 C56 -18.3(11) . . . . ? C41 C42 U2 C60 -76.9(10) . . . . ? C43 C42 U2 C60 161.0(8) . . . . ? C46 C42 U2 C60 44.2(11) . . . . ? C41 C42 U2 C57 -162.0(9) . . . . ? C43 C42 U2 C57 75.9(12) . . . . ? C46 C42 U2 C57 -40.9(14) . . . . ? C41 C42 U2 C59 -58.3(13) . . . . ? C43 C42 U2 C59 179.6(9) . . . . ? C46 C42 U2 C59 62.8(13) . . . . ? C41 C42 U2 C43 122.1(13) . . . . ? C46 C42 U2 C43 -116.8(13) . . . . ? C41 C42 U2 C45 62.4(9) . . . . ? C43 C42 U2 C45 -59.7(8) . . . . ? C46 C42 U2 C45 -176.5(11) . . . . ? C56 C57 U2 N3 -90.2(9) . . . . ? C58 C57 U2 N3 34.7(11) . . . . ? C56 C57 U2 N4 29.1(9) . . . . ? C58 C57 U2 N4 154.0(10) . . . . ? C56 C57 U2 C41 -7(3) . . . . ? C58 C57 U2 C41 118(2) . . . . ? C56 C57 U2 C61 -31.9(8) . . . . ? C58 C57 U2 C61 93.0(10) . . . . ? C56 C57 U2 C40 -166.2(12) . . . . ? C58 C57 U2 C40 -41.3(19) . . . . ? C58 C57 U2 C56 124.9(15) . . . . ? C56 C57 U2 C60 -65.3(9) . . . . ? C58 C57 U2 C60 59.6(9) . . . . ? C56 C57 U2 C42 44.1(14) . . . . ? C58 C57 U2 C42 169.1(8) . . . . ? C56 C57 U2 C59 -97.8(11) . . . . ? C58 C57 U2 C59 27.2(9) . . . . ? C56 C57 U2 C43 81.8(11) . . . . ? C58 C57 U2 C43 -153.3(8) . . . . ? C56 C57 U2 C45 152.6(8) . . . . ? C58 C57 U2 C45 -82.4(11) . . . . ? C58 C59 U2 N3 159.4(10) . . . . ? C60 C59 U2 N3 -72.9(8) . . . . ? C58 C59 U2 N4 -88.9(10) . . . . ? C60 C59 U2 N4 38.9(9) . . . . ? C58 C59 U2 C41 166.3(8) . . . . ? C60 C59 U2 C41 -66.0(10) . . . . ? C58 C59 U2 C61 -95.8(10) . . . . ? C60 C59 U2 C61 31.9(8) . . . . ? C58 C59 U2 C40 131.0(9) . . . . ? C60 C59 U2 C40 -101.2(9) . . . . ? C58 C59 U2 C56 -61.3(9) . . . . ? C60 C59 U2 C56 66.5(9) . . . . ? C58 C59 U2 C60 -127.8(14) . . . . ? C58 C59 U2 C42 -161.5(9) . . . . ? C60 C59 U2 C42 -33.7(13) . . . . ? C58 C59 U2 C57 -28.2(9) . . . . ? C60 C59 U2 C57 99.6(10) . . . . ? C58 C59 U2 C43 -133(66) . . . . ? C60 C59 U2 C43 -5(66) . . . . ? C58 C59 U2 C45 98.9(10) . . . . ? C60 C59 U2 C45 -133.3(8) . . . . ? C44 C43 U2 N3 -87.6(9) . . . . ? C42 C43 U2 N3 38.7(9) . . . . ? C44 C43 U2 N4 160.6(10) . . . . ? C42 C43 U2 N4 -73.0(9) . . . . ? C44 C43 U2 C41 -94.1(10) . . . . ? C42 C43 U2 C41 32.2(8) . . . . ? C44 C43 U2 C61 167.9(8) . . . . ? C42 C43 U2 C61 -65.8(10) . . . . ? C44 C43 U2 C40 -58.9(9) . . . . ? C42 C43 U2 C40 67.4(8) . . . . ? C44 C43 U2 C56 133.4(9) . . . . ? C42 C43 U2 C56 -100.3(9) . . . . ? C44 C43 U2 C60 -160.3(9) . . . . ? C42 C43 U2 C60 -34.0(13) . . . . ? C44 C43 U2 C42 -126.3(13) . . . . ? C44 C43 U2 C57 100.4(10) . . . . ? C42 C43 U2 C57 -133.3(9) . . . . ? C44 C43 U2 C59 -155(71) . . . . ? C42 C43 U2 C59 -29(66) . . . . ? C44 C43 U2 C45 -26.8(8) . . . . ? C42 C43 U2 C45 99.6(9) . . . . ? C40 C45 U2 N3 27.1(9) . . . . ? C44 C45 U2 N3 153.1(10) . . . . ? C40 C45 U2 N4 -92.4(9) . . . . ? C44 C45 U2 N4 33.6(10) . . . . ? C40 C45 U2 C41 -32.8(8) . . . . ? C44 C45 U2 C41 93.2(10) . . . . ? C40 C45 U2 C61 -9(3) . . . . ? C44 C45 U2 C61 117(2) . . . . ? C44 C45 U2 C40 126.0(14) . . . . ? C40 C45 U2 C56 -165.2(12) . . . . ? C44 C45 U2 C56 -39.2(19) . . . . ? C40 C45 U2 C60 42.6(13) . . . . ? C44 C45 U2 C60 168.6(9) . . . . ? C40 C45 U2 C42 -66.6(9) . . . . ? C44 C45 U2 C42 59.4(9) . . . . ? C40 C45 U2 C57 152.3(8) . . . . ? C44 C45 U2 C57 -81.8(11) . . . . ? C40 C45 U2 C59 79.9(10) . . . . ? C44 C45 U2 C59 -154.1(9) . . . . ? C40 C45 U2 C43 -99.7(10) . . . . ? C44 C45 U2 C43 26.2(8) . . . . ? C84 N6 U3 N5 -113.5(11) . . . . ? C81 N6 U3 N5 64.1(13) . . . . ? C84 N6 U3 C89 -43.2(11) . . . . ? C81 N6 U3 C89 134.4(12) . . . . ? C84 N6 U3 C73 -171.6(11) . . . . ? C81 N6 U3 C73 6.0(11) . . . . ? C84 N6 U3 C88 -11.7(10) . . . . ? C81 N6 U3 C88 166.0(12) . . . . ? C84 N6 U3 C72 178.0(10) . . . . ? C81 N6 U3 C72 -4.4(12) . . . . ? C84 N6 U3 C74 171.9(12) . . . . ? C81 N6 U3 C74 -10.5(10) . . . . ? C84 N6 U3 C90 -54.4(11) . . . . ? C81 N6 U3 C90 123.3(11) . . . . ? C84 N6 U3 C77 148.1(11) . . . . ? C81 N6 U3 C77 -34.2(12) . . . . ? C84 N6 U3 C93 2.3(11) . . . . ? C81 N6 U3 C93 180.0(11) . . . . ? C84 N6 U3 C91 -37.2(12) . . . . ? C81 N6 U3 C91 140.4(11) . . . . ? C84 N6 U3 C75 142.4(12) . . . . ? C81 N6 U3 C75 -39.9(10) . . . . ? C68 N5 U3 N6 -111.5(11) . . . . ? C65 N5 U3 N6 64.0(13) . . . . ? C68 N5 U3 C89 -171.2(11) . . . . ? C65 N5 U3 C89 4.4(11) . . . . ? C68 N5 U3 C73 -42.7(11) . . . . ? C65 N5 U3 C73 132.9(12) . . . . ? C68 N5 U3 C88 178.0(11) . . . . ? C65 N5 U3 C88 -6.4(12) . . . . ? C68 N5 U3 C72 -11.0(10) . . . . ? C65 N5 U3 C72 164.6(12) . . . . ? C68 N5 U3 C74 -52.6(11) . . . . ? C65 N5 U3 C74 122.9(11) . . . . ? C68 N5 U3 C90 173.0(12) . . . . ? C65 N5 U3 C90 -11.5(10) . . . . ? C68 N5 U3 C77 3.2(11) . . . . ? C65 N5 U3 C77 178.7(11) . . . . ? C68 N5 U3 C93 148.7(11) . . . . ? C65 N5 U3 C93 -35.7(12) . . . . ? C68 N5 U3 C91 143.0(12) . . . . ? C65 N5 U3 C91 -41.5(11) . . . . ? C68 N5 U3 C75 -36.4(12) . . . . ? C65 N5 U3 C75 139.1(11) . . . . ? C90 C89 U3 N6 -155.6(10) . . . . ? C88 C89 U3 N6 76.6(8) . . . . ? C90 C89 U3 N5 -31.1(9) . . . . ? C88 C89 U3 N5 -158.8(8) . . . . ? C90 C89 U3 C73 -88.2(10) . . . . ? C88 C89 U3 C73 144.1(8) . . . . ? C90 C89 U3 C88 127.7(13) . . . . ? C90 C89 U3 C72 -60.1(11) . . . . ? C88 C89 U3 C72 172.2(9) . . . . ? C90 C89 U3 C74 -120.1(9) . . . . ? C88 C89 U3 C74 112.2(8) . . . . ? C88 C89 U3 C90 -127.7(13) . . . . ? C90 C89 U3 C77 -64(2) . . . . ? C88 C89 U3 C77 168(2) . . . . ? C90 C89 U3 C93 97.0(10) . . . . ? C88 C89 U3 C93 -30.7(8) . . . . ? C90 C89 U3 C91 31.8(9) . . . . ? C88 C89 U3 C91 -96.0(10) . . . . ? C90 C89 U3 C75 -148.6(8) . . . . ? C88 C89 U3 C75 83.6(9) . . . . ? C74 C73 U3 N6 -32.9(9) . . . . ? C72 C73 U3 N6 -159.4(9) . . . . ? C74 C73 U3 N5 -158.2(10) . . . . ? C72 C73 U3 N5 75.3(9) . . . . ? C74 C73 U3 C89 -90.8(10) . . . . ? C72 C73 U3 C89 142.7(8) . . . . ? C74 C73 U3 C88 -63.2(12) . . . . ? C72 C73 U3 C88 170.4(9) . . . . ? C74 C73 U3 C72 126.5(13) . . . . ? C72 C73 U3 C74 -126.5(13) . . . . ? C74 C73 U3 C90 -122.6(8) . . . . ? C72 C73 U3 C90 110.9(9) . . . . ? C74 C73 U3 C77 94.8(10) . . . . ? C72 C73 U3 C77 -31.6(8) . . . . ? C74 C73 U3 C93 -69(3) . . . . ? C72 C73 U3 C93 165(2) . . . . ? C74 C73 U3 C91 -151.1(8) . . . . ? C72 C73 U3 C91 82.4(10) . . . . ? C74 C73 U3 C75 29.6(8) . . . . ? C72 C73 U3 C75 -96.9(10) . . . . ? C93 C88 U3 N6 147.9(11) . . . . ? C89 C88 U3 N6 -89.5(8) . . . . ? C85 C88 U3 N6 24.9(9) . . . . ? C93 C88 U3 N5 -99.7(10) . . . . ? C89 C88 U3 N5 22.9(9) . . . . ? C85 C88 U3 N5 137.3(9) . . . . ? C93 C88 U3 C89 -122.7(13) . . . . ? C85 C88 U3 C89 114.3(13) . . . . ? C93 C88 U3 C73 -177.8(8) . . . . ? C89 C88 U3 C73 -55.1(10) . . . . ? C85 C88 U3 C73 59.2(13) . . . . ? C93 C88 U3 C72 -151(2) . . . . ? C89 C88 U3 C72 -28(3) . . . . ? C85 C88 U3 C72 86(3) . . . . ? C93 C88 U3 C74 151.7(9) . . . . ? C89 C88 U3 C74 -85.6(9) . . . . ? C85 C88 U3 C74 28.7(12) . . . . ? C93 C88 U3 C90 -93.9(10) . . . . ? C89 C88 U3 C90 28.8(8) . . . . ? C85 C88 U3 C90 143.1(12) . . . . ? C93 C88 U3 C77 64.0(16) . . . . ? C89 C88 U3 C77 -173.4(11) . . . . ? C85 C88 U3 C77 -59.0(18) . . . . ? C89 C88 U3 C93 122.7(13) . . . . ? C85 C88 U3 C93 -123.0(15) . . . . ? C93 C88 U3 C91 -60.3(9) . . . . ? C89 C88 U3 C91 62.4(8) . . . . ? C85 C88 U3 C91 176.7(12) . . . . ? C93 C88 U3 C75 119.1(9) . . . . ? C89 C88 U3 C75 -118.3(8) . . . . ? C85 C88 U3 C75 -3.9(11) . . . . ? C77 C72 U3 N6 -99.6(9) . . . . ? C73 C72 U3 N6 22.2(9) . . . . ? C69 C72 U3 N6 137.8(9) . . . . ? C77 C72 U3 N5 148.1(10) . . . . ? C73 C72 U3 N5 -90.1(9) . . . . ? C69 C72 U3 N5 25.5(8) . . . . ? C77 C72 U3 C89 -178.5(8) . . . . ? C73 C72 U3 C89 -56.7(10) . . . . ? C69 C72 U3 C89 58.9(11) . . . . ? C77 C72 U3 C73 -121.8(13) . . . . ? C69 C72 U3 C73 115.6(13) . . . . ? C77 C72 U3 C88 -157(2) . . . . ? C73 C72 U3 C88 -35(3) . . . . ? C69 C72 U3 C88 81(3) . . . . ? C77 C72 U3 C74 -92.5(10) . . . . ? C73 C72 U3 C74 29.3(8) . . . . ? C69 C72 U3 C74 144.8(11) . . . . ? C77 C72 U3 C90 152.3(8) . . . . ? C73 C72 U3 C90 -85.9(9) . . . . ? C69 C72 U3 C90 29.7(11) . . . . ? C73 C72 U3 C77 121.8(13) . . . . ? C69 C72 U3 C77 -122.7(14) . . . . ? C77 C72 U3 C93 66.8(15) . . . . ? C73 C72 U3 C93 -171.5(12) . . . . ? C69 C72 U3 C93 -55.9(17) . . . . ? C77 C72 U3 C91 119.3(9) . . . . ? C73 C72 U3 C91 -118.9(9) . . . . ? C69 C72 U3 C91 -3.4(11) . . . . ? C77 C72 U3 C75 -60.1(9) . . . . ? C73 C72 U3 C75 61.7(9) . . . . ? C69 C72 U3 C75 177.3(11) . . . . ? C73 C74 U3 N6 142.4(10) . . . . ? C75 C74 U3 N6 -91.9(9) . . . . ? C78 C74 U3 N6 23.6(8) . . . . ? C73 C74 U3 N5 19.7(9) . . . . ? C75 C74 U3 N5 145.4(9) . . . . ? C78 C74 U3 N5 -99.1(9) . . . . ? C73 C74 U3 C89 105.6(9) . . . . ? C75 C74 U3 C89 -128.7(9) . . . . ? C78 C74 U3 C89 -13.2(10) . . . . ? C75 C74 U3 C73 125.7(14) . . . . ? C78 C74 U3 C73 -118.8(14) . . . . ? C73 C74 U3 C88 138.5(8) . . . . ? C75 C74 U3 C88 -95.8(10) . . . . ? C78 C74 U3 C88 19.7(11) . . . . ? C73 C74 U3 C72 -30.2(8) . . . . ? C75 C74 U3 C72 95.4(10) . . . . ? C78 C74 U3 C72 -149.0(11) . . . . ? C73 C74 U3 C90 74.2(10) . . . . ? C75 C74 U3 C90 -160.2(8) . . . . ? C78 C74 U3 C90 -44.6(11) . . . . ? C73 C74 U3 C77 -64.0(9) . . . . ? C75 C74 U3 C77 61.7(9) . . . . ? C78 C74 U3 C77 177.2(11) . . . . ? C73 C74 U3 C93 161.9(9) . . . . ? C75 C74 U3 C93 -72.5(12) . . . . ? C78 C74 U3 C93 43.0(13) . . . . ? C73 C74 U3 C91 53.6(14) . . . . ? C75 C74 U3 C91 179.2(11) . . . . ? C78 C74 U3 C91 -65.3(13) . . . . ? C73 C74 U3 C75 -125.7(14) . . . . ? C78 C74 U3 C75 115.5(14) . . . . ? C89 C90 U3 N6 22.2(9) . . . . ? C91 C90 U3 N6 144.2(9) . . . . ? C94 C90 U3 N6 -98.9(9) . . . . ? C89 C90 U3 N5 144.5(10) . . . . ? C91 C90 U3 N5 -93.5(9) . . . . ? C94 C90 U3 N5 23.3(8) . . . . ? C91 C90 U3 C89 122.0(14) . . . . ? C94 C90 U3 C89 -121.1(13) . . . . ? C89 C90 U3 C73 107.9(9) . . . . ? C91 C90 U3 C73 -130.0(9) . . . . ? C94 C90 U3 C73 -13.2(10) . . . . ? C89 C90 U3 C88 -29.4(8) . . . . ? C91 C90 U3 C88 92.6(10) . . . . ? C94 C90 U3 C88 -150.6(11) . . . . ? C89 C90 U3 C72 140.3(8) . . . . ? C91 C90 U3 C72 -97.7(10) . . . . ? C94 C90 U3 C72 19.2(10) . . . . ? C89 C90 U3 C74 77.8(11) . . . . ? C91 C90 U3 C74 -160.2(8) . . . . ? C94 C90 U3 C74 -43.4(11) . . . . ? C89 C90 U3 C77 163.0(8) . . . . ? C91 C90 U3 C77 -74.9(12) . . . . ? C94 C90 U3 C77 41.9(13) . . . . ? C89 C90 U3 C93 -62.0(9) . . . . ? C91 C90 U3 C93 60.0(9) . . . . ? C94 C90 U3 C93 176.8(10) . . . . ? C89 C90 U3 C91 -122.0(14) . . . . ? C94 C90 U3 C91 116.8(13) . . . . ? C89 C90 U3 C75 58.0(14) . . . . ? C91 C90 U3 C75 -180.0(10) . . . . ? C94 C90 U3 C75 -63.1(13) . . . . ? C76 C77 U3 N6 -34.0(10) . . . . ? C72 C77 U3 N6 92.2(9) . . . . ? C76 C77 U3 N5 -154.0(10) . . . . ? C72 C77 U3 N5 -27.7(9) . . . . ? C76 C77 U3 C89 -121(2) . . . . ? C72 C77 U3 C89 5(3) . . . . ? C76 C77 U3 C73 -93.5(10) . . . . ? C72 C77 U3 C73 32.8(8) . . . . ? C76 C77 U3 C88 41.1(18) . . . . ? C72 C77 U3 C88 167.4(13) . . . . ? C76 C77 U3 C72 -126.3(14) . . . . ? C76 C77 U3 C74 -59.6(9) . . . . ? C72 C77 U3 C74 66.7(9) . . . . ? C76 C77 U3 C90 -170.5(9) . . . . ? C72 C77 U3 C90 -44.2(13) . . . . ? C76 C77 U3 C93 81.8(12) . . . . ? C72 C77 U3 C93 -151.9(8) . . . . ? C76 C77 U3 C91 152.5(9) . . . . ? C72 C77 U3 C91 -81.2(10) . . . . ? C76 C77 U3 C75 -26.9(8) . . . . ? C72 C77 U3 C75 99.4(10) . . . . ? C88 C93 U3 N6 -28.3(9) . . . . ? C92 C93 U3 N6 -154.9(10) . . . . ? C88 C93 U3 N5 92.1(10) . . . . ? C92 C93 U3 N5 -34.4(11) . . . . ? C88 C93 U3 C89 32.7(9) . . . . ? C92 C93 U3 C89 -93.9(10) . . . . ? C88 C93 U3 C73 7(3) . . . . ? C92 C93 U3 C73 -119(2) . . . . ? C92 C93 U3 C88 -126.6(15) . . . . ? C88 C93 U3 C72 164.4(13) . . . . ? C92 C93 U3 C72 37.8(18) . . . . ? C88 C93 U3 C74 -45.5(13) . . . . ? C92 C93 U3 C74 -172.1(9) . . . . ? C88 C93 U3 C90 66.4(9) . . . . ? C92 C93 U3 C90 -60.1(9) . . . . ? C88 C93 U3 C77 -152.7(9) . . . . ? C92 C93 U3 C77 80.8(12) . . . . ? C88 C93 U3 C91 99.4(11) . . . . ? C92 C93 U3 C91 -27.2(9) . . . . ? C88 C93 U3 C75 -81.4(11) . . . . ? C92 C93 U3 C75 152.1(9) . . . . ? C92 C91 U3 N6 87.4(10) . . . . ? C90 C91 U3 N6 -39.7(10) . . . . ? C92 C91 U3 N5 -159.4(10) . . . . ? C90 C91 U3 N5 73.5(9) . . . . ? C92 C91 U3 C89 94.8(10) . . . . ? C90 C91 U3 C89 -32.3(9) . . . . ? C92 C91 U3 C73 -166.4(8) . . . . ? C90 C91 U3 C73 66.6(11) . . . . ? C92 C91 U3 C88 60.0(9) . . . . ? C90 C91 U3 C88 -67.0(9) . . . . ? C92 C91 U3 C72 -132.1(9) . . . . ? C90 C91 U3 C72 100.8(9) . . . . ? C92 C91 U3 C74 163.4(10) . . . . ? C90 C91 U3 C74 36.4(13) . . . . ? C92 C91 U3 C90 127.1(15) . . . . ? C92 C91 U3 C77 -99.2(10) . . . . ? C90 C91 U3 C77 133.7(9) . . . . ? C92 C91 U3 C93 27.7(9) . . . . ? C90 C91 U3 C93 -99.3(10) . . . . ? C92 C91 U3 C75 -55(50) . . . . ? C90 C91 U3 C75 178(100) . . . . ? C74 C75 U3 N6 75.2(9) . . . . ? C76 C75 U3 N6 -160.6(10) . . . . ? C74 C75 U3 N5 -38.1(10) . . . . ? C76 C75 U3 N5 86.2(9) . . . . ? C74 C75 U3 C89 68.2(11) . . . . ? C76 C75 U3 C89 -167.6(8) . . . . ? C74 C75 U3 C73 -30.4(8) . . . . ? C76 C75 U3 C73 93.8(10) . . . . ? C74 C75 U3 C88 103.0(9) . . . . ? C76 C75 U3 C88 -132.7(9) . . . . ? C74 C75 U3 C72 -64.8(9) . . . . ? C76 C75 U3 C72 59.4(9) . . . . ? C76 C75 U3 C74 124.2(14) . . . . ? C74 C75 U3 C90 35.6(14) . . . . ? C76 C75 U3 C90 159.8(10) . . . . ? C74 C75 U3 C77 -97.7(10) . . . . ? C76 C75 U3 C77 26.5(9) . . . . ? C74 C75 U3 C93 135.5(9) . . . . ? C76 C75 U3 C93 -100.2(10) . . . . ? C74 C75 U3 C91 -142(49) . . . . ? C76 C75 U3 C91 -18(50) . . . . ? C97 N7 U4 N7 112.4(11) 2 . . 2 ? C100 N7 U4 N7 -59.9(9) . . . 2 ? C97 N7 U4 C109 42.8(11) 2 . . 2 ? C100 N7 U4 C109 -129.5(11) . . . 2 ? C97 N7 U4 C109 171.0(11) 2 . . . ? C100 N7 U4 C109 -1.3(10) . . . . ? C97 N7 U4 C108 10.7(10) 2 . . 2 ? C100 N7 U4 C108 -161.6(11) . . . 2 ? C97 N7 U4 C108 -177.9(10) 2 . . . ? C100 N7 U4 C108 9.8(11) . . . . ? C97 N7 U4 C104 54.3(11) 2 . . 2 ? C100 N7 U4 C104 -118.0(10) . . . 2 ? C97 N7 U4 C104 -173.3(12) 2 . . . ? C100 N7 U4 C104 14.4(9) . . . . ? C97 N7 U4 C107 -2.1(11) 2 . . 2 ? C100 N7 U4 C107 -174.4(10) . . . 2 ? C97 N7 U4 C107 -148.4(10) 2 . . . ? C100 N7 U4 C107 39.3(11) . . . . ? C97 N7 U4 C105 37.9(12) 2 . . 2 ? C100 N7 U4 C105 -134.4(10) . . . 2 ? C97 N7 U4 C105 -142.7(12) 2 . . . ? C100 N7 U4 C105 45.0(10) . . . . ? C104 C109 U4 N7 30.7(8) . . . . ? C108 C109 U4 N7 158.3(8) . . . . ? C104 C109 U4 N7 155.0(9) . . . 2 ? C108 C109 U4 N7 -77.4(8) . . . 2 ? C104 C109 U4 C109 87.8(8) . . . 2 ? C108 C109 U4 C109 -144.6(9) . . . 2 ? C104 C109 U4 C108 60.3(11) . . . 2 ? C108 C109 U4 C108 -172.1(5) . . . 2 ? C104 C109 U4 C108 -127.6(13) . . . . ? C104 C109 U4 C104 119.4(9) . . . 2 ? C108 C109 U4 C104 -113.0(8) . . . 2 ? C108 C109 U4 C104 127.6(13) . . . . ? C104 C109 U4 C107 72(3) . . . 2 ? C108 C109 U4 C107 -160(2) . . . 2 ? C104 C109 U4 C107 -95.9(9) . . . . ? C108 C109 U4 C107 31.7(8) . . . . ? C104 C109 U4 C105 148.3(8) . . . 2 ? C108 C109 U4 C105 -84.1(9) . . . 2 ? C104 C109 U4 C105 -31.1(8) . . . . ? C108 C109 U4 C105 96.5(9) . . . . ? C107 C108 U4 N7 97.5(9) . . . . ? C109 C108 U4 N7 -23.5(9) . . . . ? C110 C108 U4 N7 -137.7(9) . . . . ? C107 C108 U4 N7 -150.9(10) . . . 2 ? C109 C108 U4 N7 88.2(8) . . . 2 ? C110 C108 U4 N7 -26.1(8) . . . 2 ? C107 C108 U4 C109 175.4(9) . . . 2 ? C109 C108 U4 C109 54.4(13) . . . 2 ? C110 C108 U4 C109 -59.9(12) . . . 2 ? C107 C108 U4 C109 120.9(13) . . . . ? C110 C108 U4 C109 -114.3(13) . . . . ? C107 C108 U4 C108 151.5(9) . . . 2 ? C109 C108 U4 C108 30.5(8) . . . 2 ? C110 C108 U4 C108 -83.7(9) . . . 2 ? C107 C108 U4 C104 -155.2(8) . . . 2 ? C109 C108 U4 C104 83.9(9) . . . 2 ? C110 C108 U4 C104 -30.4(11) . . . 2 ? C107 C108 U4 C104 92.2(10) . . . . ? C109 C108 U4 C104 -28.7(7) . . . . ? C110 C108 U4 C104 -143.0(11) . . . . ? C107 C108 U4 C107 -70(2) . . . 2 ? C109 C108 U4 C107 169.4(12) . . . 2 ? C110 C108 U4 C107 55.1(17) . . . 2 ? C109 C108 U4 C107 -120.9(13) . . . . ? C110 C108 U4 C107 124.8(14) . . . . ? C107 C108 U4 C105 -121.9(9) . . . 2 ? C109 C108 U4 C105 117.1(8) . . . 2 ? C110 C108 U4 C105 2.8(11) . . . 2 ? C107 C108 U4 C105 58.8(9) . . . . ? C109 C108 U4 C105 -62.1(8) . . . . ? C110 C108 U4 C105 -176.4(11) . . . . ? C109 C104 U4 N7 -144.8(9) . . . . ? C105 C104 U4 N7 91.6(9) . . . . ? C101 C104 U4 N7 -25.3(8) . . . . ? C109 C104 U4 N7 -22.6(9) . . . 2 ? C105 C104 U4 N7 -146.2(9) . . . 2 ? C101 C104 U4 N7 97.0(9) . . . 2 ? C109 C104 U4 C109 -108.0(9) . . . 2 ? C105 C104 U4 C109 128.4(9) . . . 2 ? C101 C104 U4 C109 11.6(9) . . . 2 ? C105 C104 U4 C109 -123.6(13) . . . . ? C101 C104 U4 C109 119.5(13) . . . . ? C109 C104 U4 C108 -140.5(8) . . . 2 ? C105 C104 U4 C108 95.9(9) . . . 2 ? C101 C104 U4 C108 -20.9(10) . . . 2 ? C109 C104 U4 C108 29.7(8) . . . . ? C105 C104 U4 C108 -93.9(10) . . . . ? C101 C104 U4 C108 149.2(10) . . . . ? C109 C104 U4 C104 -77.2(8) . . . 2 ? C105 C104 U4 C104 159.2(9) . . . 2 ? C101 C104 U4 C104 42.3(8) . . . 2 ? C109 C104 U4 C107 -161.4(9) . . . 2 ? C105 C104 U4 C107 75.0(12) . . . 2 ? C101 C104 U4 C107 -41.9(12) . . . 2 ? C109 C104 U4 C107 62.9(8) . . . . ? C105 C104 U4 C107 -60.7(9) . . . . ? C101 C104 U4 C107 -177.6(10) . . . . ? C109 C104 U4 C105 -56.8(13) . . . 2 ? C105 C104 U4 C105 179.6(4) . . . 2 ? C101 C104 U4 C105 62.7(12) . . . 2 ? C109 C104 U4 C105 123.6(13) . . . . ? C101 C104 U4 C105 -116.9(12) . . . . ? C106 C107 U4 N7 33.6(10) . . . . ? C108 C107 U4 N7 -94.1(9) . . . . ? C106 C107 U4 N7 153.3(9) . . . 2 ? C108 C107 U4 N7 25.6(9) . . . 2 ? C106 C107 U4 C109 112(2) . . . 2 ? C108 C107 U4 C109 -16(3) . . . 2 ? C106 C107 U4 C109 94.0(10) . . . . ? C108 C107 U4 C109 -33.7(8) . . . . ? C106 C107 U4 C108 -38.6(18) . . . 2 ? C108 C107 U4 C108 -166.3(9) . . . 2 ? C106 C107 U4 C108 127.7(14) . . . . ? C106 C107 U4 C104 167.9(9) . . . 2 ? C108 C107 U4 C104 40.2(13) . . . 2 ? C106 C107 U4 C104 60.1(9) . . . . ? C108 C107 U4 C104 -67.6(9) . . . . ? C106 C107 U4 C107 -82.5(9) . . . 2 ? C108 C107 U4 C107 149.8(9) . . . 2 ? C106 C107 U4 C105 -154.2(9) . . . 2 ? C108 C107 U4 C105 78.1(10) . . . 2 ? C106 C107 U4 C105 26.6(9) . . . . ? C108 C107 U4 C105 -101.1(10) . . . . ? C106 C105 U4 N7 160.1(10) . . . . ? C104 C105 U4 N7 -74.7(9) . . . . ? C106 C105 U4 N7 -87.9(9) . . . 2 ? C104 C105 U4 N7 37.4(10) . . . 2 ? C106 C105 U4 C109 166.8(8) . . . 2 ? C104 C105 U4 C109 -68.0(10) . . . 2 ? C106 C105 U4 C109 -93.9(10) . . . . ? C104 C105 U4 C109 31.4(8) . . . . ? C106 C105 U4 C108 132.0(9) . . . 2 ? C104 C105 U4 C108 -102.7(9) . . . 2 ? C106 C105 U4 C108 -59.2(9) . . . . ? C104 C105 U4 C108 66.0(9) . . . . ? C106 C105 U4 C104 -161.9(9) . . . 2 ? C104 C105 U4 C104 -36.7(16) . . . 2 ? C106 C105 U4 C104 -125.2(13) . . . . ? C106 C105 U4 C107 100.0(10) . . . 2 ? C104 C105 U4 C107 -134.8(8) . . . 2 ? C106 C105 U4 C107 -27.0(8) . . . . ? C104 C105 U4 C107 98.2(10) . . . . ? C106 C105 U4 C105 -143.8(9) . . . 2 ? C104 C105 U4 C105 -18.5(8) . . . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.803 _refine_diff_density_min -2.097 _refine_diff_density_rms 0.225 _database_code_depnum_ccdc_archive 'CCDC 951389' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p12140 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common U2I4L _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 I4 N2 U2' _chemical_formula_sum 'C32 H36 I4 N2 U2' _chemical_formula_weight 1432.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 31.0498(7) _cell_length_b 11.5475(2) _cell_length_c 10.1812(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3650.44(13) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 10731 _cell_measurement_theta_min 2.9667 _cell_measurement_theta_max 27.4235 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3613 _exptl_crystal_size_mid 0.2657 _exptl_crystal_size_min 0.1180 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 12.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21023 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38038 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4380 _reflns_number_gt 3924 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material mercury _refine_special_details ; Alert level C for 98 Ang3 void space in crystal. Probably corresponds to ca 1/2 benzene but no obvious fragments to model and decided not to use SQUEEZE. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+35.6295P] 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 4380 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3366(2) 0.9488(5) 0.7864(6) 0.0150(13) Uani 1 1 d . . . C2 C 0.3020(2) 0.9926(5) 0.7168(7) 0.0184(14) Uani 1 1 d . . . H2 H 0.2752 1.0173 0.7521 0.022 Uiso 1 1 calc R . . C3 C 0.3143(2) 0.9936(5) 0.5821(6) 0.0165(13) Uani 1 1 d . . . H3 H 0.2973 1.0199 0.5105 0.020 Uiso 1 1 calc R . . C4 C 0.3558(2) 0.9490(5) 0.5746(6) 0.0143(13) Uani 1 1 d . . . C5 C 0.3467(2) 0.9620(6) 0.9300(7) 0.0193(14) Uani 1 1 d . . . C6 C 0.3060(2) 0.9702(6) 1.0147(7) 0.0255(16) Uani 1 1 d . . . H6A H 0.2893 1.0386 0.9887 0.038 Uiso 1 1 calc R . . H6B H 0.3142 0.9769 1.1074 0.038 Uiso 1 1 calc R . . H6C H 0.2885 0.9005 1.0021 0.038 Uiso 1 1 calc R . . C7 C 0.3729(3) 1.0752(6) 0.9447(8) 0.0290(17) Uani 1 1 d . . . H7A H 0.3990 1.0704 0.8906 0.043 Uiso 1 1 calc R . . H7B H 0.3810 1.0857 1.0369 0.043 Uiso 1 1 calc R . . H7C H 0.3554 1.1410 0.9158 0.043 Uiso 1 1 calc R . . C8 C 0.3730(2) 0.8563(6) 0.9715(6) 0.0186(14) Uani 1 1 d . . . C9 C 0.4148(2) 0.8551(6) 1.0225(6) 0.0208(15) Uani 1 1 d . . . H9 H 0.4294 0.9257 1.0399 0.025 Uiso 1 1 calc R . . C10 C 0.4347(3) 0.7500 1.0475(11) 0.025(2) Uani 1 2 d S . . H10 H 0.4630 0.7500 1.0829 0.030 Uiso 1 2 calc SR . . C11 C 0.3523(3) 0.7500 0.9469(9) 0.0159(18) Uani 1 2 d S . . H11 H 0.3237 0.7500 0.9130 0.019 Uiso 1 2 calc SR . . C12 C 0.3885(2) 0.9632(5) 0.4672(6) 0.0157(13) Uani 1 1 d . . . C13 C 0.4137(2) 1.0747(5) 0.5000(7) 0.0244(16) Uani 1 1 d . . . H13A H 0.3937 1.1399 0.5072 0.037 Uiso 1 1 calc R . . H13B H 0.4346 1.0904 0.4301 0.037 Uiso 1 1 calc R . . H13C H 0.4290 1.0646 0.5835 0.037 Uiso 1 1 calc R . . C14 C 0.3682(2) 0.9770(6) 0.3316(7) 0.0242(16) Uani 1 1 d . . . H14A H 0.3514 0.9077 0.3105 0.036 Uiso 1 1 calc R . . H14B H 0.3910 0.9874 0.2659 0.036 Uiso 1 1 calc R . . H14C H 0.3493 1.0450 0.3314 0.036 Uiso 1 1 calc R . . C15 C 0.4169(2) 0.8562(5) 0.4692(6) 0.0166(13) Uani 1 1 d . . . C16 C 0.4616(2) 0.8541(6) 0.4828(7) 0.0205(14) Uani 1 1 d . . . H16 H 0.4770 0.9249 0.4901 0.025 Uiso 1 1 calc R . . C17 C 0.4837(4) 0.7500 0.4858(11) 0.028(2) Uani 1 2 d S . . H17 H 0.5142 0.7500 0.4899 0.033 Uiso 1 2 calc SR . . C18 C 0.3955(3) 0.7500 0.4606(8) 0.0132(18) Uani 1 2 d S . . H18 H 0.3651 0.7500 0.4484 0.016 Uiso 1 2 calc SR . . N1 N 0.36906(17) 0.9137(4) 0.6993(5) 0.0142(11) Uani 1 1 d . . . I1 I 0.496228(18) 0.94077(5) 0.79935(5) 0.03852(15) Uani 1 1 d . . . I2 I 0.26763(2) 0.7500 0.37390(7) 0.02529(15) Uani 1 2 d S . . I3 I 0.22393(2) 0.7500 0.79891(8) 0.03026(17) Uani 1 2 d S . . U1 U 0.427615(11) 0.7500 0.74764(4) 0.01743(9) Uani 1 2 d S . . U2 U 0.307648(11) 0.7500 0.64678(4) 0.01585(9) Uani 1 2 d S . . 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 0.016(3) 0.009(3) 0.021(3) -0.001(2) 0.001(3) 0.000(2) C2 0.013(3) 0.018(3) 0.025(4) -0.002(3) 0.002(3) 0.003(3) C3 0.016(3) 0.012(3) 0.021(3) -0.001(2) -0.004(3) 0.001(2) C4 0.017(3) 0.009(3) 0.017(3) 0.002(2) 0.002(3) -0.001(2) C5 0.021(4) 0.018(3) 0.019(3) -0.002(3) 0.003(3) 0.000(3) C6 0.029(4) 0.027(4) 0.021(4) -0.003(3) 0.005(3) 0.007(3) C7 0.039(5) 0.017(3) 0.031(4) -0.004(3) -0.009(3) -0.006(3) C8 0.020(4) 0.019(3) 0.016(3) -0.003(3) 0.001(3) -0.001(3) C9 0.023(4) 0.025(3) 0.015(3) 0.000(3) -0.003(3) -0.002(3) C10 0.005(5) 0.037(6) 0.033(6) 0.000 -0.003(4) 0.000 C11 0.012(5) 0.019(4) 0.017(5) 0.000 0.000(4) 0.000 C12 0.017(3) 0.012(3) 0.018(3) 0.001(2) 0.003(3) 0.002(2) C13 0.029(4) 0.012(3) 0.032(4) 0.001(3) 0.005(3) -0.005(3) C14 0.028(4) 0.022(3) 0.023(4) 0.007(3) 0.005(3) 0.002(3) C15 0.020(4) 0.017(3) 0.013(3) 0.000(2) 0.004(3) -0.002(3) C16 0.015(4) 0.022(3) 0.024(4) 0.002(3) 0.000(3) -0.006(3) C17 0.020(6) 0.026(5) 0.037(6) 0.000 0.003(5) 0.000 C18 0.012(4) 0.012(4) 0.016(4) 0.000 -0.008(4) 0.000 N1 0.013(3) 0.019(3) 0.010(2) -0.005(2) 0.005(2) 0.003(2) I1 0.0312(3) 0.0558(3) 0.0286(3) -0.0077(2) 0.0026(2) -0.0258(3) I2 0.0247(4) 0.0229(3) 0.0282(4) 0.000 -0.0096(3) 0.000 I3 0.0179(4) 0.0301(4) 0.0428(4) 0.000 0.0083(3) 0.000 U1 0.01216(18) 0.01935(17) 0.02079(18) 0.000 -0.00120(15) 0.000 U2 0.01428(18) 0.01372(16) 0.01955(18) 0.000 0.00012(14) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(9) . ? C1 N1 1.403(8) . ? C1 C5 1.503(9) . ? C1 U2 2.846(6) . ? C2 C3 1.424(9) . ? C2 U2 2.896(6) . ? C2 H2 0.9500 . ? C3 C4 1.391(9) . ? C3 U2 2.897(6) . ? C3 H3 0.9500 . ? C4 N1 1.394(8) . ? C4 C12 1.500(9) . ? C4 U2 2.839(6) . ? C5 C8 1.528(9) . ? C5 C6 1.533(9) . ? C5 C7 1.547(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.399(10) . ? C8 C11 1.409(8) . ? C9 C10 1.386(8) . ? C9 H9 0.9500 . ? C10 C9 1.386(8) 7_575 ? C10 U1 3.061(11) . ? C10 H10 0.9500 . ? C11 C8 1.409(8) 7_575 ? C11 H11 0.9500 . ? C12 C15 1.518(9) . ? C12 C14 1.525(9) . ? C12 C13 1.544(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C18 1.397(7) . ? C15 C16 1.396(9) . ? C16 C17 1.384(9) . ? C16 H16 0.9500 . ? C17 C16 1.384(9) 7_575 ? C17 H17 0.9500 . ? C18 C15 1.397(7) 7_575 ? C18 H18 0.9500 . ? N1 U1 2.669(5) . ? N1 U2 2.738(5) . ? I1 U1 3.1095(6) . ? I2 U2 3.0434(7) . ? I3 U2 3.0258(8) . ? U1 N1 2.669(5) 7_575 ? U1 I1 3.1095(6) 7_575 ? U1 U2 3.8639(5) . ? U2 N1 2.738(5) 7_575 ? U2 C4 2.839(6) 7_575 ? U2 C1 2.846(6) 7_575 ? U2 C2 2.896(6) 7_575 ? U2 C3 2.897(6) 7_575 ? 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 C2 C1 N1 109.9(6) . . ? C2 C1 C5 128.6(6) . . ? N1 C1 C5 119.6(6) . . ? C2 C1 U2 78.1(4) . . ? N1 C1 U2 71.2(3) . . ? C5 C1 U2 129.3(4) . . ? C1 C2 C3 106.8(6) . . ? C1 C2 U2 74.1(4) . . ? C3 C2 U2 75.8(4) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? U2 C2 H2 115.8 . . ? C4 C3 C2 107.3(6) . . ? C4 C3 U2 73.7(3) . . ? C2 C3 U2 75.7(4) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? U2 C3 H3 116.4 . . ? C3 C4 N1 109.4(5) . . ? C3 C4 C12 128.7(6) . . ? N1 C4 C12 119.8(6) . . ? C3 C4 U2 78.3(4) . . ? N1 C4 U2 71.5(3) . . ? C12 C4 U2 129.3(4) . . ? C1 C5 C8 107.4(5) . . ? C1 C5 C6 112.4(6) . . ? C8 C5 C6 109.5(6) . . ? C1 C5 C7 106.8(5) . . ? C8 C5 C7 111.5(6) . . ? C6 C5 C7 109.1(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C11 118.7(7) . . ? C9 C8 C5 127.4(6) . . ? C11 C8 C5 113.8(6) . . ? C10 C9 C8 119.5(7) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C9 122.2(9) 7_575 . ? C9 C10 U1 77.6(5) 7_575 . ? C9 C10 U1 77.6(5) . . ? C9 C10 H10 118.9 7_575 . ? C9 C10 H10 118.9 . . ? U1 C10 H10 116.5 . . ? C8 C11 C8 121.3(9) . 7_575 ? C8 C11 H11 119.3 . . ? C8 C11 H11 119.3 7_575 . ? C4 C12 C15 107.1(5) . . ? C4 C12 C14 113.1(6) . . ? C15 C12 C14 109.7(5) . . ? C4 C12 C13 106.0(5) . . ? C15 C12 C13 112.4(5) . . ? C14 C12 C13 108.5(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C16 117.7(6) . . ? C18 C15 C12 115.9(6) . . ? C16 C15 C12 126.3(6) . . ? C17 C16 C15 120.6(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C16 120.6(10) 7_575 . ? C16 C17 H17 119.7 7_575 . ? C16 C17 H17 119.7 . . ? C15 C18 C15 122.7(9) . 7_575 ? C15 C18 H18 118.7 . . ? C15 C18 H18 118.7 7_575 . ? C4 N1 C1 106.2(5) . . ? C4 N1 U1 125.1(4) . . ? C1 N1 U1 125.3(4) . . ? C4 N1 U2 79.6(3) . . ? C1 N1 U2 79.8(3) . . ? U1 N1 U2 91.22(16) . . ? N1 U1 N1 90.2(2) 7_575 . ? N1 U1 C10 103.49(16) 7_575 . ? N1 U1 C10 103.49(16) . . ? N1 U1 I1 179.10(11) 7_575 . ? N1 U1 I1 89.78(12) . . ? C10 U1 I1 77.39(13) . . ? N1 U1 I1 89.78(11) 7_575 7_575 ? N1 U1 I1 179.10(11) . 7_575 ? C10 U1 I1 77.39(13) . 7_575 ? I1 U1 I1 90.22(3) . 7_575 ? N1 U1 U2 45.10(11) 7_575 . ? N1 U1 U2 45.10(11) . . ? C10 U1 U2 109.55(18) . . ? I1 U1 U2 134.870(13) . . ? I1 U1 U2 134.870(13) 7_575 . ? N1 U2 N1 87.3(2) . 7_575 ? N1 U2 C4 28.88(16) . . ? N1 U2 C4 104.02(17) 7_575 . ? N1 U2 C4 104.02(17) . 7_575 ? N1 U2 C4 28.88(16) 7_575 7_575 ? C4 U2 C4 108.1(3) . 7_575 ? N1 U2 C1 29.02(16) . . ? N1 U2 C1 103.88(17) 7_575 . ? C4 U2 C1 46.35(18) . . ? C4 U2 C1 128.02(18) 7_575 . ? N1 U2 C1 103.88(17) . 7_575 ? N1 U2 C1 29.02(16) 7_575 7_575 ? C4 U2 C1 128.02(18) . 7_575 ? C4 U2 C1 46.35(18) 7_575 7_575 ? C1 U2 C1 107.6(3) . 7_575 ? N1 U2 C2 47.61(17) . . ? N1 U2 C2 131.44(18) 7_575 . ? C4 U2 C2 46.56(18) . . ? C4 U2 C2 151.45(19) 7_575 . ? C1 U2 C2 27.81(18) . . ? C1 U2 C2 132.57(19) 7_575 . ? N1 U2 C2 131.44(17) . 7_575 ? N1 U2 C2 47.61(17) 7_575 7_575 ? C4 U2 C2 151.45(19) . 7_575 ? C4 U2 C2 46.56(18) 7_575 7_575 ? C1 U2 C2 132.57(19) . 7_575 ? C1 U2 C2 27.81(18) 7_575 7_575 ? C2 U2 C2 150.6(3) . 7_575 ? N1 U2 C3 47.47(17) . . ? N1 U2 C3 131.70(17) 7_575 . ? C4 U2 C3 28.04(17) . . ? C4 U2 C3 133.60(19) 7_575 . ? C1 U2 C3 46.17(18) . . ? C1 U2 C3 151.00(18) 7_575 . ? C2 U2 C3 28.46(18) . . ? C2 U2 C3 178.72(19) 7_575 . ? N1 U2 C3 131.70(17) . 7_575 ? N1 U2 C3 47.47(17) 7_575 7_575 ? C4 U2 C3 133.60(19) . 7_575 ? C4 U2 C3 28.04(18) 7_575 7_575 ? C1 U2 C3 151.00(18) . 7_575 ? C1 U2 C3 46.17(18) 7_575 7_575 ? C2 U2 C3 178.72(19) . 7_575 ? C2 U2 C3 28.46(18) 7_575 7_575 ? C3 U2 C3 152.4(3) . 7_575 ? N1 U2 I3 119.89(10) . . ? N1 U2 I3 119.89(10) 7_575 . ? C4 U2 I3 125.82(13) . . ? C4 U2 I3 125.82(13) 7_575 . ? C1 U2 I3 90.89(13) . . ? C1 U2 I3 90.89(13) 7_575 . ? C2 U2 I3 79.76(13) . . ? C2 U2 I3 79.76(13) 7_575 . ? C3 U2 I3 100.24(13) . . ? C3 U2 I3 100.24(13) 7_575 . ? N1 U2 I2 117.55(11) . . ? N1 U2 I2 117.55(11) 7_575 . ? C4 U2 I2 88.80(13) . . ? C4 U2 I2 88.80(13) 7_575 . ? C1 U2 I2 125.78(13) . . ? C1 U2 I2 125.78(13) 7_575 . ? C2 U2 I2 101.55(13) . . ? C2 U2 I2 101.55(13) 7_575 . ? C3 U2 I2 79.72(13) . . ? C3 U2 I2 79.72(13) 7_575 . ? I3 U2 I2 96.69(2) . . ? 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 N1 C1 C2 C3 -4.6(7) . . . . ? C5 C1 C2 C3 159.3(6) . . . . ? U2 C1 C2 C3 -69.3(4) . . . . ? N1 C1 C2 U2 64.8(4) . . . . ? C5 C1 C2 U2 -131.3(7) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? U2 C2 C3 C4 -67.5(4) . . . . ? C1 C2 C3 U2 68.1(4) . . . . ? C2 C3 C4 N1 3.5(7) . . . . ? U2 C3 C4 N1 -65.4(4) . . . . ? C2 C3 C4 C12 -159.6(6) . . . . ? U2 C3 C4 C12 131.5(7) . . . . ? C2 C3 C4 U2 68.9(4) . . . . ? C2 C1 C5 C8 152.6(7) . . . . ? N1 C1 C5 C8 -44.8(7) . . . . ? U2 C1 C5 C8 44.4(7) . . . . ? C2 C1 C5 C6 32.1(9) . . . . ? N1 C1 C5 C6 -165.4(6) . . . . ? U2 C1 C5 C6 -76.2(7) . . . . ? C2 C1 C5 C7 -87.6(8) . . . . ? N1 C1 C5 C7 74.9(7) . . . . ? U2 C1 C5 C7 164.1(5) . . . . ? C1 C5 C8 C9 119.4(7) . . . . ? C6 C5 C8 C9 -118.2(7) . . . . ? C7 C5 C8 C9 2.6(10) . . . . ? C1 C5 C8 C11 -56.9(8) . . . . ? C6 C5 C8 C11 65.5(8) . . . . ? C7 C5 C8 C11 -173.6(7) . . . . ? C11 C8 C9 C10 0.0(11) . . . . ? C5 C8 C9 C10 -176.1(8) . . . . ? C8 C9 C10 C9 0.6(15) . . . 7_575 ? C8 C9 C10 U1 67.0(6) . . . . ? C9 C8 C11 C8 -0.6(13) . . . 7_575 ? C5 C8 C11 C8 176.0(6) . . . 7_575 ? C3 C4 C12 C15 -151.5(6) . . . . ? N1 C4 C12 C15 46.9(7) . . . . ? U2 C4 C12 C15 -42.9(7) . . . . ? C3 C4 C12 C14 -30.6(9) . . . . ? N1 C4 C12 C14 167.8(5) . . . . ? U2 C4 C12 C14 78.1(7) . . . . ? C3 C4 C12 C13 88.3(8) . . . . ? N1 C4 C12 C13 -73.3(7) . . . . ? U2 C4 C12 C13 -163.1(4) . . . . ? C4 C12 C15 C18 54.4(8) . . . . ? C14 C12 C15 C18 -68.7(8) . . . . ? C13 C12 C15 C18 170.5(6) . . . . ? C4 C12 C15 C16 -123.4(7) . . . . ? C14 C12 C15 C16 113.5(7) . . . . ? C13 C12 C15 C16 -7.3(9) . . . . ? C18 C15 C16 C17 0.9(11) . . . . ? C12 C15 C16 C17 178.7(8) . . . . ? C15 C16 C17 C16 -3.7(15) . . . 7_575 ? C16 C15 C18 C15 2.0(13) . . . 7_575 ? C12 C15 C18 C15 -176.0(6) . . . 7_575 ? C3 C4 N1 C1 -6.2(7) . . . . ? C12 C4 N1 C1 158.7(5) . . . . ? U2 C4 N1 C1 -76.0(4) . . . . ? C3 C4 N1 U1 154.0(4) . . . . ? C12 C4 N1 U1 -41.2(7) . . . . ? U2 C4 N1 U1 84.1(4) . . . . ? C3 C4 N1 U2 69.8(4) . . . . ? C12 C4 N1 U2 -125.3(5) . . . . ? C2 C1 N1 C4 6.7(7) . . . . ? C5 C1 N1 C4 -158.9(5) . . . . ? U2 C1 N1 C4 75.9(4) . . . . ? C2 C1 N1 U1 -153.4(4) . . . . ? C5 C1 N1 U1 41.0(7) . . . . ? U2 C1 N1 U1 -84.2(4) . . . . ? C2 C1 N1 U2 -69.3(5) . . . . ? C5 C1 N1 U2 125.2(5) . . . . ? C4 N1 U1 N1 -78.5(5) . . . 7_575 ? C1 N1 U1 N1 78.0(5) . . . 7_575 ? U2 N1 U1 N1 -0.4(2) . . . 7_575 ? C4 N1 U1 C10 177.6(5) . . . . ? C1 N1 U1 C10 -26.0(5) . . . . ? U2 N1 U1 C10 -104.29(17) . . . . ? C4 N1 U1 I1 100.6(5) . . . . ? C1 N1 U1 I1 -102.9(5) . . . . ? U2 N1 U1 I1 178.74(11) . . . . ? C4 N1 U1 I1 11(8) . . . 7_575 ? C1 N1 U1 I1 167(7) . . . 7_575 ? U2 N1 U1 I1 89(7) . . . 7_575 ? C4 N1 U1 U2 -78.1(5) . . . . ? C1 N1 U1 U2 78.3(5) . . . . ? C9 C10 U1 N1 17.0(5) 7_575 . . 7_575 ? C9 C10 U1 N1 -110.5(4) . . . 7_575 ? C9 C10 U1 N1 110.5(4) 7_575 . . . ? C9 C10 U1 N1 -17.0(5) . . . . ? C9 C10 U1 I1 -162.8(5) 7_575 . . . ? C9 C10 U1 I1 69.7(4) . . . . ? C9 C10 U1 I1 -69.7(4) 7_575 . . 7_575 ? C9 C10 U1 I1 162.8(5) . . . 7_575 ? C9 C10 U1 U2 63.7(5) 7_575 . . . ? C9 C10 U1 U2 -63.7(5) . . . . ? C4 N1 U2 N1 125.9(3) . . . 7_575 ? C1 N1 U2 N1 -125.3(3) . . . 7_575 ? U1 N1 U2 N1 0.4(2) . . . 7_575 ? C1 N1 U2 C4 108.8(5) . . . . ? U1 N1 U2 C4 -125.5(4) . . . . ? C4 N1 U2 C4 102.1(4) . . . 7_575 ? C1 N1 U2 C4 -149.1(3) . . . 7_575 ? U1 N1 U2 C4 -23.44(19) . . . 7_575 ? C4 N1 U2 C1 -108.8(5) . . . . ? U1 N1 U2 C1 125.7(4) . . . . ? C4 N1 U2 C1 150.0(3) . . . 7_575 ? C1 N1 U2 C1 -101.3(4) . . . 7_575 ? U1 N1 U2 C1 24.41(19) . . . 7_575 ? C4 N1 U2 C2 -74.2(4) . . . . ? C1 N1 U2 C2 34.6(3) . . . . ? U1 N1 U2 C2 160.3(3) . . . . ? C4 N1 U2 C2 145.6(3) . . . 7_575 ? C1 N1 U2 C2 -105.6(4) . . . 7_575 ? U1 N1 U2 C2 20.1(3) . . . 7_575 ? C4 N1 U2 C3 -35.2(3) . . . . ? C1 N1 U2 C3 73.5(4) . . . . ? U1 N1 U2 C3 -160.8(3) . . . . ? C4 N1 U2 C3 107.3(4) . . . 7_575 ? C1 N1 U2 C3 -144.0(3) . . . 7_575 ? U1 N1 U2 C3 -18.3(3) . . . 7_575 ? C4 N1 U2 I3 -110.8(3) . . . . ? C1 N1 U2 I3 -2.1(4) . . . . ? U1 N1 U2 I3 123.64(9) . . . . ? C4 N1 U2 I2 6.0(4) . . . . ? C1 N1 U2 I2 114.8(3) . . . . ? U1 N1 U2 I2 -119.52(10) . . . . ? C3 C4 U2 N1 -115.2(5) . . . . ? C12 C4 U2 N1 113.8(7) . . . . ? C3 C4 U2 N1 -171.8(4) . . . 7_575 ? N1 C4 U2 N1 -56.5(3) . . . 7_575 ? C12 C4 U2 N1 57.3(6) . . . 7_575 ? C3 C4 U2 C4 158.5(3) . . . 7_575 ? N1 C4 U2 C4 -86.3(4) . . . 7_575 ? C12 C4 U2 C4 27.5(7) . . . 7_575 ? C3 C4 U2 C1 -75.8(4) . . . . ? N1 C4 U2 C1 39.4(3) . . . . ? C12 C4 U2 C1 153.2(7) . . . . ? C3 C4 U2 C1 -153.3(4) . . . 7_575 ? N1 C4 U2 C1 -38.1(4) . . . 7_575 ? C12 C4 U2 C1 75.7(6) . . . 7_575 ? C3 C4 U2 C2 -37.1(4) . . . . ? N1 C4 U2 C2 78.1(4) . . . . ? C12 C4 U2 C2 -168.1(7) . . . . ? C3 C4 U2 C2 -177.5(4) . . . 7_575 ? N1 C4 U2 C2 -62.3(5) . . . 7_575 ? C12 C4 U2 C2 51.5(7) . . . 7_575 ? N1 C4 U2 C3 115.2(5) . . . . ? C12 C4 U2 C3 -131.0(7) . . . . ? C3 C4 U2 C3 144.7(5) . . . 7_575 ? N1 C4 U2 C3 -100.1(4) . . . 7_575 ? C12 C4 U2 C3 13.7(7) . . . 7_575 ? C3 C4 U2 I3 -27.3(4) . . . . ? N1 C4 U2 I3 87.9(3) . . . . ? C12 C4 U2 I3 -158.3(5) . . . . ? C3 C4 U2 I2 70.1(4) . . . . ? N1 C4 U2 I2 -174.7(3) . . . . ? C12 C4 U2 I2 -60.9(5) . . . . ? C2 C1 U2 N1 116.0(6) . . . . ? C5 C1 U2 N1 -113.3(7) . . . . ? C2 C1 U2 N1 173.1(4) . . . 7_575 ? N1 C1 U2 N1 57.1(3) . . . 7_575 ? C5 C1 U2 N1 -56.3(6) . . . 7_575 ? C2 C1 U2 C4 76.8(4) . . . . ? N1 C1 U2 C4 -39.2(3) . . . . ? C5 C1 U2 C4 -152.5(7) . . . . ? C2 C1 U2 C4 155.2(4) . . . 7_575 ? N1 C1 U2 C4 39.2(4) . . . 7_575 ? C5 C1 U2 C4 -74.2(6) . . . 7_575 ? C2 C1 U2 C1 -157.0(3) . . . 7_575 ? N1 C1 U2 C1 87.0(4) . . . 7_575 ? C5 C1 U2 C1 -26.3(7) . . . 7_575 ? N1 C1 U2 C2 -116.0(6) . . . . ? C5 C1 U2 C2 130.7(8) . . . . ? C2 C1 U2 C2 -142.6(5) . . . 7_575 ? N1 C1 U2 C2 101.3(4) . . . 7_575 ? C5 C1 U2 C2 -12.0(7) . . . 7_575 ? C2 C1 U2 C3 37.6(4) . . . . ? N1 C1 U2 C3 -78.4(4) . . . . ? C5 C1 U2 C3 168.3(7) . . . . ? C2 C1 U2 C3 -179.0(4) . . . 7_575 ? N1 C1 U2 C3 65.0(5) . . . 7_575 ? C5 C1 U2 C3 -48.4(8) . . . 7_575 ? C2 C1 U2 I3 -65.8(4) . . . . ? N1 C1 U2 I3 178.2(3) . . . . ? C5 C1 U2 I3 64.9(5) . . . . ? C2 C1 U2 I2 33.1(4) . . . . ? N1 C1 U2 I2 -82.9(3) . . . . ? C5 C1 U2 I2 163.8(5) . . . . ? C1 C2 U2 N1 -36.2(4) . . . . ? C3 C2 U2 N1 76.3(4) . . . . ? C1 C2 U2 N1 -9.0(5) . . . 7_575 ? C3 C2 U2 N1 103.5(4) . . . 7_575 ? C1 C2 U2 C4 -76.0(4) . . . . ? C3 C2 U2 C4 36.5(4) . . . . ? C1 C2 U2 C4 -43.8(6) . . . 7_575 ? C3 C2 U2 C4 68.7(6) . . . 7_575 ? C3 C2 U2 C1 112.5(6) . . . . ? C1 C2 U2 C1 30.4(4) . . . 7_575 ? C3 C2 U2 C1 142.9(4) . . . 7_575 ? C1 C2 U2 C2 65.7(7) . . . 7_575 ? C3 C2 U2 C2 178.1(4) . . . 7_575 ? C1 C2 U2 C3 -112.5(6) . . . . ? C1 C2 U2 C3 22(9) . . . 7_575 ? C3 C2 U2 C3 134(9) . . . 7_575 ? C1 C2 U2 I3 112.1(4) . . . . ? C3 C2 U2 I3 -135.4(4) . . . . ? C1 C2 U2 I2 -153.1(4) . . . . ? C3 C2 U2 I2 -40.6(4) . . . . ? C4 C3 U2 N1 36.4(3) . . . . ? C2 C3 U2 N1 -76.9(4) . . . . ? C4 C3 U2 N1 10.7(5) . . . 7_575 ? C2 C3 U2 N1 -102.5(4) . . . 7_575 ? C2 C3 U2 C4 -113.2(6) . . . . ? C4 C3 U2 C4 -28.8(4) . . . 7_575 ? C2 C3 U2 C4 -142.1(4) . . . 7_575 ? C4 C3 U2 C1 76.5(4) . . . . ? C2 C3 U2 C1 -36.7(4) . . . . ? C4 C3 U2 C1 46.8(6) . . . 7_575 ? C2 C3 U2 C1 -66.4(6) . . . 7_575 ? C4 C3 U2 C2 113.2(6) . . . . ? C4 C3 U2 C2 68(9) . . . 7_575 ? C2 C3 U2 C2 -45(9) . . . 7_575 ? C4 C3 U2 C3 -64.8(7) . . . 7_575 ? C2 C3 U2 C3 -178.0(4) . . . 7_575 ? C4 C3 U2 I3 157.8(3) . . . . ? C2 C3 U2 I3 44.6(4) . . . . ? C4 C3 U2 I2 -107.2(4) . . . . ? C2 C3 U2 I2 139.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.867 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.207 _database_code_depnum_ccdc_archive 'CCDC 951390'