# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michel Ephritikhine' _publ_contact_author_email MICHEL.EPHRITIKHINE@CEA.FR _publ_section_title ; Linear uranium metallocenes with polydentate aromatic nitrogen ligands ; loop_ _publ_author_name 'M Ephritikhine' 'Jean-Claude Berthet' 'Jerome Maynadie' 'Pierre Thuery' # Attachment 'revisedC002279ACIF.txt' data_2.2MeCN _database_code_depnum_ccdc_archive 'CCDC 764413' #TrackingRef 'revisedC002279ACIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H47 N5 U, 2(C24 H20 B), 2(C2 H3 N)' _chemical_formula_sum 'C90 H93 B2 N7 U' _chemical_formula_weight 1532.36 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' B B 0.0013 0.0007 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5130(14) _cell_length_b 28.901(6) _cell_length_c 28.972(5) _cell_angle_alpha 70.360(8) _cell_angle_beta 82.842(9) _cell_angle_gamma 85.270(11) _cell_volume 7437(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 145711 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method ? _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 2.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.522 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; Crystal-to-detector distance 50 mm. The Rint value is quite large, which is due to the low crystal quality. There is however no ambiguity on the crystal system (triclinic) choice. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 145711 _diffrn_reflns_av_R_equivalents 0.1128 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 27424 _reflns_number_gt 12723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some atoms, particularly in the solvent molecules. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^] 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 27424 _refine_ls_number_parameters 1831 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1941 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.407 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.218 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.46899(4) 0.191692(14) 0.779575(14) 0.03565(14) Uani 1 1 d . . . N1A N 0.4221(7) 0.2863(3) 0.7472(3) 0.035(2) Uani 1 1 d . . . N2A N 0.4715(7) 0.2370(3) 0.8439(3) 0.036(2) Uani 1 1 d . . . N3A N 0.5153(8) 0.1210(3) 0.8591(4) 0.050(3) Uani 1 1 d . . . N4A N 0.4951(8) 0.1088(3) 0.7649(3) 0.041(2) Uani 1 1 d . . . N5A N 0.4417(8) 0.2056(3) 0.6896(4) 0.045(3) Uani 1 1 d . . . C1A C 0.3986(9) 0.3112(4) 0.7007(4) 0.036(3) Uani 1 1 d . . . H1A H 0.3952 0.2937 0.6792 0.044 Uiso 1 1 calc R . . C2A C 0.3791(10) 0.3618(4) 0.6829(4) 0.046(3) Uani 1 1 d . . . H2A H 0.3647 0.3777 0.6501 0.055 Uiso 1 1 calc R . . C3A C 0.3811(10) 0.3881(4) 0.7137(5) 0.045(3) Uani 1 1 d . . . H3A H 0.3674 0.4222 0.7021 0.054 Uiso 1 1 calc R . . C4A C 0.4033(9) 0.3645(4) 0.7622(4) 0.038(3) Uani 1 1 d . . . C5A C 0.4245(9) 0.3128(4) 0.7778(4) 0.032(3) Uani 1 1 d . . . C6A C 0.4487(9) 0.2872(4) 0.8285(4) 0.037(3) Uani 1 1 d . . . C7A C 0.4923(9) 0.2155(4) 0.8909(4) 0.043(3) Uani 1 1 d . . . H7A H 0.5068 0.1815 0.9020 0.052 Uiso 1 1 calc R . . C8A C 0.4944(9) 0.2394(4) 0.9249(4) 0.043(3) Uani 1 1 d . . . H8A H 0.5071 0.2220 0.9576 0.052 Uiso 1 1 calc R . . C9A C 0.4768(9) 0.2898(4) 0.9085(4) 0.038(3) Uani 1 1 d . . . H9A H 0.4797 0.3073 0.9300 0.046 Uiso 1 1 calc R . . C10A C 0.4551(9) 0.3141(4) 0.8601(4) 0.037(3) Uani 1 1 d . . . C11A C 0.4316(9) 0.3664(4) 0.8428(5) 0.044(3) Uani 1 1 d . . . H11A H 0.4331 0.3841 0.8643 0.053 Uiso 1 1 calc R . . C12A C 0.4073(10) 0.3903(4) 0.7958(5) 0.045(3) Uani 1 1 d . . . H12A H 0.3928 0.4243 0.7852 0.054 Uiso 1 1 calc R . . C13A C 0.5360(9) 0.0878(4) 0.8931(4) 0.036(3) Uani 1 1 d . . . C14A C 0.5566(9) 0.0477(3) 0.9381(3) 0.040(3) Uani 1 1 d . . . H14A H 0.6001 0.0595 0.9599 0.060 Uiso 1 1 calc R . . H14B H 0.6169 0.0223 0.9306 0.060 Uiso 1 1 calc R . . H14C H 0.4666 0.0347 0.9537 0.060 Uiso 1 1 calc R . . C15A C 0.5140(11) 0.0701(5) 0.7600(4) 0.042(3) Uani 1 1 d . . . C16A C 0.5312(11) 0.0221(4) 0.7533(4) 0.054(3) Uani 1 1 d . . . H16A H 0.4857 0.0232 0.7252 0.081 Uiso 1 1 calc R . . H16B H 0.4889 -0.0022 0.7821 0.081 Uiso 1 1 calc R . . H16C H 0.6304 0.0138 0.7482 0.081 Uiso 1 1 calc R . . C17A C 0.4484(10) 0.2081(4) 0.6485(5) 0.048(3) Uani 1 1 d . . . C18A C 0.4617(11) 0.2115(4) 0.5978(4) 0.060(3) Uani 1 1 d . . . H18A H 0.5083 0.2410 0.5782 0.090 Uiso 1 1 calc R . . H18B H 0.3692 0.2122 0.5876 0.090 Uiso 1 1 calc R . . H18C H 0.5167 0.1835 0.5937 0.090 Uiso 1 1 calc R . . C19A C 0.7506(10) 0.1585(4) 0.7757(5) 0.043(3) Uani 1 1 d . . . C20A C 0.7538(9) 0.1938(4) 0.7984(4) 0.039(3) Uani 1 1 d . . . C21A C 0.7290(10) 0.2394(4) 0.7632(5) 0.043(3) Uani 1 1 d . . . C22A C 0.7156(10) 0.2331(4) 0.7182(4) 0.045(3) Uani 1 1 d . . . C23A C 0.7331(9) 0.1817(4) 0.7255(4) 0.038(3) Uani 1 1 d . . . C24A C 0.8062(10) 0.1058(4) 0.7974(4) 0.052(3) Uani 1 1 d . . . H24A H 0.8006 0.0886 0.7745 0.078 Uiso 1 1 calc R . . H24B H 0.7499 0.0899 0.8277 0.078 Uiso 1 1 calc R . . H24C H 0.9031 0.1055 0.8036 0.078 Uiso 1 1 calc R . . C25A C 0.8027(9) 0.1847(4) 0.8494(3) 0.048(3) Uani 1 1 d . . . H25A H 0.9044 0.1822 0.8471 0.072 Uiso 1 1 calc R . . H25B H 0.7652 0.1547 0.8721 0.072 Uiso 1 1 calc R . . H25C H 0.7690 0.2116 0.8609 0.072 Uiso 1 1 calc R . . C26A C 0.7518(9) 0.2887(4) 0.7691(4) 0.048(3) Uani 1 1 d . . . H26A H 0.7140 0.2882 0.8016 0.073 Uiso 1 1 calc R . . H26B H 0.7042 0.3145 0.7451 0.073 Uiso 1 1 calc R . . H26C H 0.8514 0.2943 0.7644 0.073 Uiso 1 1 calc R . . C27A C 0.7175(10) 0.2725(4) 0.6684(4) 0.051(3) Uani 1 1 d . . . H27A H 0.6739 0.3024 0.6720 0.076 Uiso 1 1 calc R . . H27B H 0.6661 0.2622 0.6473 0.076 Uiso 1 1 calc R . . H27C H 0.8138 0.2780 0.6540 0.076 Uiso 1 1 calc R . . C28A C 0.7512(10) 0.1585(4) 0.6865(4) 0.056(3) Uani 1 1 d . . . H28A H 0.8384 0.1390 0.6889 0.084 Uiso 1 1 calc R . . H28B H 0.7537 0.1836 0.6548 0.084 Uiso 1 1 calc R . . H28C H 0.6733 0.1379 0.6907 0.084 Uiso 1 1 calc R . . C29A C 0.2045(10) 0.1599(4) 0.7680(4) 0.039(3) Uani 1 1 d . . . C30A C 0.2264(10) 0.1347(4) 0.8185(5) 0.048(3) Uani 1 1 d . . . C31A C 0.2167(10) 0.1692(4) 0.8424(4) 0.041(3) Uani 1 1 d . . . C32A C 0.1855(10) 0.2166(4) 0.8085(4) 0.043(3) Uani 1 1 d . . . C33A C 0.1773(9) 0.2105(4) 0.7619(4) 0.040(3) Uani 1 1 d . . . C34A C 0.1799(10) 0.1369(4) 0.7300(4) 0.054(3) Uani 1 1 d . . . H34A H 0.2453 0.1093 0.7323 0.082 Uiso 1 1 calc R . . H34B H 0.1943 0.1608 0.6976 0.082 Uiso 1 1 calc R . . H34C H 0.0845 0.1261 0.7358 0.082 Uiso 1 1 calc R . . C35A C 0.2257(10) 0.0800(4) 0.8421(4) 0.052(3) Uani 1 1 d . . . H35A H 0.3132 0.0682 0.8563 0.078 Uiso 1 1 calc R . . H35B H 0.2158 0.0651 0.8176 0.078 Uiso 1 1 calc R . . H35C H 0.1478 0.0715 0.8674 0.078 Uiso 1 1 calc R . . C36A C 0.2064(9) 0.1561(4) 0.8977(4) 0.044(3) Uani 1 1 d . . . H36A H 0.1140 0.1445 0.9118 0.067 Uiso 1 1 calc R . . H36B H 0.2217 0.1848 0.9058 0.067 Uiso 1 1 calc R . . H36C H 0.2771 0.1309 0.9106 0.067 Uiso 1 1 calc R . . C37A C 0.1319(9) 0.2609(4) 0.8224(4) 0.048(3) Uani 1 1 d . . . H37A H 0.1520 0.2901 0.7949 0.071 Uiso 1 1 calc R . . H37B H 0.1780 0.2615 0.8498 0.071 Uiso 1 1 calc R . . H37C H 0.0314 0.2594 0.8313 0.071 Uiso 1 1 calc R . . C38A C 0.1221(9) 0.2478(4) 0.7180(4) 0.051(3) Uani 1 1 d . . . H38A H 0.0234 0.2431 0.7181 0.076 Uiso 1 1 calc R . . H38B H 0.1738 0.2443 0.6887 0.076 Uiso 1 1 calc R . . H38C H 0.1336 0.2802 0.7190 0.076 Uiso 1 1 calc R . . U2 U 0.99995(4) 0.305802(14) 0.219321(14) 0.03505(14) Uani 1 1 d . . . N1B N 1.0525(8) 0.2116(3) 0.2458(3) 0.036(2) Uani 1 1 d . . . N2B N 1.0026(7) 0.2645(3) 0.1521(3) 0.039(2) Uani 1 1 d . . . N3B N 0.9551(8) 0.3795(3) 0.1425(3) 0.039(2) Uani 1 1 d . . . N4B N 0.9651(8) 0.3862(3) 0.2391(3) 0.043(2) Uani 1 1 d . . . N5B N 1.0263(8) 0.2867(3) 0.3114(3) 0.036(2) Uani 1 1 d . . . C1B C 1.0827(9) 0.1861(4) 0.2915(4) 0.043(3) Uani 1 1 d . . . H1B H 1.0805 0.2028 0.3141 0.051 Uiso 1 1 calc R . . C2B C 1.1176(10) 0.1352(4) 0.3073(4) 0.050(3) Uani 1 1 d . . . H2B H 1.1415 0.1188 0.3390 0.060 Uiso 1 1 calc R . . C3B C 1.1152(10) 0.1107(4) 0.2742(5) 0.046(3) Uani 1 1 d . . . H3B H 1.1340 0.0769 0.2839 0.055 Uiso 1 1 calc R . . C4B C 1.0850(9) 0.1360(4) 0.2264(4) 0.034(3) Uani 1 1 d . . . C5B C 1.0555(9) 0.1886(4) 0.2131(4) 0.037(3) Uani 1 1 d . . . C6B C 1.0280(9) 0.2156(4) 0.1632(4) 0.034(3) Uani 1 1 d . . . C7B C 0.9781(9) 0.2888(4) 0.1048(4) 0.036(3) Uani 1 1 d . . . H7B H 0.9602 0.3227 0.0956 0.043 Uiso 1 1 calc R . . C8B C 0.9780(9) 0.2664(4) 0.0690(4) 0.036(3) Uani 1 1 d . . . H8B H 0.9631 0.2849 0.0367 0.043 Uiso 1 1 calc R . . C9B C 1.0004(9) 0.2165(4) 0.0826(4) 0.043(3) Uani 1 1 d . . . H9B H 0.9968 0.2009 0.0594 0.051 Uiso 1 1 calc R . . C10B C 1.0281(9) 0.1885(4) 0.1298(4) 0.034(3) Uani 1 1 d . . . C11B C 1.0584(9) 0.1376(4) 0.1446(4) 0.039(3) Uani 1 1 d . . . H11B H 1.0605 0.1210 0.1219 0.047 Uiso 1 1 calc R . . C12B C 1.0840(10) 0.1130(4) 0.1907(5) 0.046(3) Uani 1 1 d . . . H12B H 1.1020 0.0792 0.1997 0.055 Uiso 1 1 calc R . . C13B C 0.9413(10) 0.4125(4) 0.1080(5) 0.039(3) Uani 1 1 d . . . C14B C 0.9329(9) 0.4544(4) 0.0622(4) 0.043(3) Uani 1 1 d . . . H14D H 0.8733 0.4803 0.0688 0.064 Uiso 1 1 calc R . . H14E H 0.8938 0.4441 0.0384 0.064 Uiso 1 1 calc R . . H14F H 1.0262 0.4660 0.0494 0.064 Uiso 1 1 calc R . . C15B C 0.9586(11) 0.4235(4) 0.2446(4) 0.042(3) Uani 1 1 d . . . C16B C 0.9515(11) 0.4730(4) 0.2475(4) 0.052(3) Uani 1 1 d . . . H16D H 1.0158 0.4932 0.2218 0.077 Uiso 1 1 calc R . . H16E H 0.9774 0.4717 0.2790 0.077 Uiso 1 1 calc R . . H16F H 0.8567 0.4869 0.2438 0.077 Uiso 1 1 calc R . . C17B C 1.0265(9) 0.2841(4) 0.3518(4) 0.034(3) Uani 1 1 d . . . C18B C 1.0306(10) 0.2818(4) 0.4026(4) 0.050(3) Uani 1 1 d . . . H18D H 0.9398 0.2729 0.4208 0.075 Uiso 1 1 calc R . . H18E H 1.0530 0.3134 0.4032 0.075 Uiso 1 1 calc R . . H18F H 1.1017 0.2576 0.4174 0.075 Uiso 1 1 calc R . . C19B C 1.2870(9) 0.2845(4) 0.1902(4) 0.038(3) Uani 1 1 d . . . C20B C 1.2924(9) 0.2894(4) 0.2371(4) 0.033(3) Uani 1 1 d . . . C21B C 1.2631(10) 0.3379(5) 0.2327(4) 0.048(3) Uani 1 1 d . . . C22B C 1.2402(9) 0.3656(4) 0.1841(4) 0.037(3) Uani 1 1 d . . . C23B C 1.2559(9) 0.3329(4) 0.1567(4) 0.035(3) Uani 1 1 d . . . C24B C 1.3464(8) 0.2417(4) 0.1735(4) 0.042(3) Uani 1 1 d . . . H24D H 1.3006 0.2418 0.1458 0.062 Uiso 1 1 calc R . . H24E H 1.3297 0.2114 0.2000 0.062 Uiso 1 1 calc R . . H24F H 1.4465 0.2448 0.1643 0.062 Uiso 1 1 calc R . . C25B C 1.3542(9) 0.2505(4) 0.2787(4) 0.044(3) Uani 1 1 d . . . H25D H 1.4516 0.2569 0.2788 0.067 Uiso 1 1 calc R . . H25E H 1.3489 0.2189 0.2749 0.067 Uiso 1 1 calc R . . H25F H 1.3020 0.2505 0.3093 0.067 Uiso 1 1 calc R . . C26B C 1.2821(10) 0.3602(4) 0.2728(4) 0.053(3) Uani 1 1 d . . . H26D H 1.3752 0.3512 0.2833 0.080 Uiso 1 1 calc R . . H26E H 1.2122 0.3479 0.3003 0.080 Uiso 1 1 calc R . . H26F H 1.2708 0.3953 0.2596 0.080 Uiso 1 1 calc R . . C27B C 1.2370(10) 0.4212(3) 0.1610(4) 0.048(3) Uani 1 1 d . . . H27D H 1.1417 0.4342 0.1650 0.072 Uiso 1 1 calc R . . H27E H 1.2694 0.4300 0.1266 0.072 Uiso 1 1 calc R . . H27F H 1.2977 0.4346 0.1770 0.072 Uiso 1 1 calc R . . C28B C 1.2660(9) 0.3474(4) 0.1019(4) 0.043(3) Uani 1 1 d . . . H28D H 1.3593 0.3585 0.0881 0.064 Uiso 1 1 calc R . . H28E H 1.1971 0.3735 0.0895 0.064 Uiso 1 1 calc R . . H28F H 1.2480 0.3197 0.0927 0.064 Uiso 1 1 calc R . . C29B C 0.7457(10) 0.2572(4) 0.2302(4) 0.042(3) Uani 1 1 d . . . C30B C 0.7534(10) 0.2607(4) 0.2776(4) 0.043(3) Uani 1 1 d . . . C31B C 0.7317(9) 0.3113(4) 0.2729(4) 0.034(3) Uani 1 1 d . . . C32B C 0.7126(9) 0.3386(4) 0.2242(4) 0.039(3) Uani 1 1 d . . . C33B C 0.7169(8) 0.3048(4) 0.1972(4) 0.034(3) Uani 1 1 d . . . C34B C 0.7211(11) 0.2100(4) 0.2200(4) 0.062(3) Uani 1 1 d . . . H34D H 0.7864 0.1843 0.2363 0.093 Uiso 1 1 calc R . . H34E H 0.7359 0.2158 0.1851 0.093 Uiso 1 1 calc R . . H34F H 0.6257 0.2003 0.2320 0.093 Uiso 1 1 calc R . . C35B C 0.7552(10) 0.2162(4) 0.3232(4) 0.055(3) Uani 1 1 d . . . H35D H 0.6601 0.2097 0.3384 0.082 Uiso 1 1 calc R . . H35E H 0.8111 0.2222 0.3458 0.082 Uiso 1 1 calc R . . H35F H 0.7957 0.1884 0.3145 0.082 Uiso 1 1 calc R . . C36B C 0.7092(10) 0.3288(4) 0.3173(4) 0.059(3) Uani 1 1 d . . . H36D H 0.7746 0.3538 0.3131 0.089 Uiso 1 1 calc R . . H36E H 0.7249 0.3017 0.3465 0.089 Uiso 1 1 calc R . . H36F H 0.6138 0.3420 0.3202 0.089 Uiso 1 1 calc R . . C37B C 0.6602(9) 0.3913(3) 0.2063(4) 0.042(3) Uani 1 1 d . . . H37D H 0.5726 0.3937 0.1922 0.064 Uiso 1 1 calc R . . H37E H 0.7294 0.4103 0.1817 0.064 Uiso 1 1 calc R . . H37F H 0.6451 0.4038 0.2334 0.064 Uiso 1 1 calc R . . C38B C 0.6671(10) 0.3195(4) 0.1479(4) 0.052(3) Uani 1 1 d . . . H38D H 0.5655 0.3233 0.1508 0.078 Uiso 1 1 calc R . . H38E H 0.6965 0.2946 0.1331 0.078 Uiso 1 1 calc R . . H38F H 0.7069 0.3501 0.1276 0.078 Uiso 1 1 calc R . . B1 B 0.1061(12) 0.3532(5) 0.5219(5) 0.048(4) Uani 1 1 d . . . B2 B 0.8253(13) 0.1090(5) 0.4847(5) 0.048(4) Uani 1 1 d . . . B3 B 0.9566(11) 0.3962(4) 0.9098(5) 0.034(3) Uani 1 1 d . . . B4 B 0.5309(11) 0.1098(5) 0.0867(5) 0.041(3) Uani 1 1 d . . . C1 C 0.0115(11) 0.3707(4) 0.5640(4) 0.045(3) Uani 1 1 d . . . C2 C -0.1203(11) 0.3980(4) 0.5592(4) 0.048(3) Uani 1 1 d . . . H2 H -0.1569 0.4081 0.5289 0.058 Uiso 1 1 calc R . . C3 C -0.1942(12) 0.4096(4) 0.5966(4) 0.053(3) Uani 1 1 d . . . H3 H -0.2824 0.4259 0.5917 0.064 Uiso 1 1 calc R . . C4 C -0.1438(12) 0.3984(4) 0.6422(5) 0.058(3) Uani 1 1 d . . . H4 H -0.1946 0.4080 0.6673 0.069 Uiso 1 1 calc R . . C5 C -0.0130(11) 0.3717(4) 0.6492(4) 0.056(3) Uani 1 1 d . . . H5 H 0.0242 0.3627 0.6793 0.067 Uiso 1 1 calc R . . C6 C 0.0591(11) 0.3592(4) 0.6102(4) 0.051(3) Uani 1 1 d . . . H6 H 0.1458 0.3418 0.6153 0.061 Uiso 1 1 calc R . . C7 C 0.2621(10) 0.3780(4) 0.5147(4) 0.045(3) Uani 1 1 d . . . C8 C 0.2785(10) 0.4283(4) 0.4934(4) 0.054(3) Uani 1 1 d . . . H8 H 0.2000 0.4484 0.4819 0.065 Uiso 1 1 calc R . . C9 C 0.4076(11) 0.4502(4) 0.4886(4) 0.051(3) Uani 1 1 d . . . H9 H 0.4155 0.4838 0.4729 0.061 Uiso 1 1 calc R . . C10 C 0.5247(12) 0.4207(5) 0.5078(4) 0.059(3) Uani 1 1 d . . . H10 H 0.6118 0.4344 0.5050 0.071 Uiso 1 1 calc R . . C11 C 0.5087(11) 0.3718(5) 0.5306(4) 0.059(3) Uani 1 1 d . . . H11 H 0.5861 0.3521 0.5437 0.070 Uiso 1 1 calc R . . C12 C 0.3816(11) 0.3506(4) 0.5350(4) 0.062(4) Uani 1 1 d . . . H12 H 0.3744 0.3171 0.5519 0.075 Uiso 1 1 calc R . . C13 C 0.1228(10) 0.2929(4) 0.5361(4) 0.042(3) Uani 1 1 d . . . C14 C 0.0550(11) 0.2608(4) 0.5782(5) 0.057(3) Uani 1 1 d . . . H14 H 0.0019 0.2733 0.6008 0.068 Uiso 1 1 calc R . . C15 C 0.0637(11) 0.2093(5) 0.5879(5) 0.063(4) Uani 1 1 d . . . H15 H 0.0183 0.1887 0.6170 0.075 Uiso 1 1 calc R . . C16 C 0.1380(11) 0.1896(4) 0.5551(5) 0.054(3) Uani 1 1 d . . . H16 H 0.1404 0.1559 0.5609 0.064 Uiso 1 1 calc R . . C17 C 0.2093(11) 0.2205(4) 0.5133(4) 0.051(3) Uani 1 1 d . . . H17 H 0.2636 0.2076 0.4911 0.061 Uiso 1 1 calc R . . C18 C 0.2000(11) 0.2715(4) 0.5042(4) 0.046(3) Uani 1 1 d . . . H18 H 0.2478 0.2918 0.4755 0.056 Uiso 1 1 calc R . . C19 C 0.0363(10) 0.3730(4) 0.4670(4) 0.039(3) Uani 1 1 d . . . C20 C 0.1055(11) 0.3960(4) 0.4227(4) 0.053(3) Uani 1 1 d . . . H20 H 0.1999 0.4029 0.4218 0.063 Uiso 1 1 calc R . . C21 C 0.0461(11) 0.4105(4) 0.3782(4) 0.047(3) Uani 1 1 d . . . H21 H 0.1013 0.4239 0.3484 0.057 Uiso 1 1 calc R . . C22 C -0.0996(12) 0.4041(4) 0.3794(4) 0.055(3) Uani 1 1 d . . . H22 H -0.1443 0.4164 0.3507 0.065 Uiso 1 1 calc R . . C23 C -0.1757(11) 0.3795(4) 0.4234(4) 0.045(3) Uani 1 1 d . . . H23 H -0.2706 0.3731 0.4246 0.054 Uiso 1 1 calc R . . C24 C -0.1076(11) 0.3648(4) 0.4653(4) 0.042(3) Uani 1 1 d . . . H24 H -0.1596 0.3482 0.4948 0.051 Uiso 1 1 calc R . . C25 C 0.7909(10) 0.0738(4) 0.5422(4) 0.048(3) Uani 1 1 d . . . C26 C 0.7459(13) 0.0891(5) 0.5817(5) 0.073(4) Uani 1 1 d . . . H26 H 0.7386 0.1228 0.5766 0.088 Uiso 1 1 calc R . . C27 C 0.7116(14) 0.0579(6) 0.6278(6) 0.091(4) Uani 1 1 d U . . H27 H 0.6838 0.0705 0.6534 0.109 Uiso 1 1 calc R . . C28 C 0.7173(13) 0.0066(5) 0.6377(5) 0.073(4) Uani 1 1 d . . . H28 H 0.6873 -0.0146 0.6689 0.087 Uiso 1 1 calc R . . C29 C 0.7673(11) -0.0110(4) 0.6009(4) 0.050(3) Uani 1 1 d . . . H29 H 0.7775 -0.0446 0.6063 0.060 Uiso 1 1 calc R . . C30 C 0.8027(10) 0.0230(4) 0.5549(5) 0.057(3) Uani 1 1 d . . . H30 H 0.8381 0.0104 0.5299 0.069 Uiso 1 1 calc R . . C31 C 0.9961(10) 0.1144(4) 0.4707(4) 0.044(3) Uani 1 1 d . . . C32 C 1.0961(11) 0.0797(5) 0.4943(4) 0.060(3) Uani 1 1 d . . . H32 H 1.0666 0.0527 0.5211 0.072 Uiso 1 1 calc R . . C33 C 1.2424(12) 0.0848(5) 0.4783(5) 0.067(4) Uani 1 1 d U . . H33 H 1.3071 0.0616 0.4956 0.080 Uiso 1 1 calc R . . C34 C 1.2916(11) 0.1228(4) 0.4380(5) 0.067(4) Uani 1 1 d . . . H34 H 1.3876 0.1245 0.4267 0.081 Uiso 1 1 calc R . . C35 C 1.1941(12) 0.1588(4) 0.4147(4) 0.056(3) Uani 1 1 d . . . H35 H 1.2244 0.1859 0.3881 0.067 Uiso 1 1 calc R . . C36 C 1.0488(11) 0.1543(4) 0.4316(4) 0.055(3) Uani 1 1 d . . . H36 H 0.9851 0.1790 0.4158 0.066 Uiso 1 1 calc R . . C37 C 0.7667(11) 0.0843(4) 0.4484(4) 0.048(3) Uani 1 1 d . . . C38 C 0.8326(12) 0.0865(4) 0.4020(4) 0.059(3) Uani 1 1 d . . . H38 H 0.9182 0.1021 0.3919 0.070 Uiso 1 1 calc R . . C39 C 0.7809(13) 0.0671(5) 0.3695(5) 0.082(4) Uani 1 1 d U . . H39 H 0.8316 0.0699 0.3392 0.099 Uiso 1 1 calc R . . C40 C 0.6543(13) 0.0441(4) 0.3830(5) 0.067(4) Uani 1 1 d . . . H40 H 0.6182 0.0309 0.3619 0.080 Uiso 1 1 calc R . . C41 C 0.5831(11) 0.0408(4) 0.4270(5) 0.056(3) Uani 1 1 d . . . H41 H 0.4991 0.0242 0.4369 0.067 Uiso 1 1 calc R . . C42 C 0.6343(11) 0.0622(4) 0.4582(5) 0.061(4) Uani 1 1 d . . . H42 H 0.5779 0.0618 0.4870 0.073 Uiso 1 1 calc R . . C43 C 0.7529(10) 0.1635(4) 0.4789(4) 0.052(3) Uani 1 1 d . . . C44 C 0.6326(10) 0.1838(4) 0.4521(4) 0.056(3) Uani 1 1 d . . . H44 H 0.5947 0.1654 0.4362 0.067 Uiso 1 1 calc R . . C45 C 0.5705(12) 0.2299(5) 0.4489(5) 0.069(4) Uani 1 1 d . . . H45 H 0.4932 0.2415 0.4308 0.083 Uiso 1 1 calc R . . C46 C 0.6214(13) 0.2583(5) 0.4720(5) 0.064(3) Uani 1 1 d U . . H46 H 0.5755 0.2882 0.4710 0.077 Uiso 1 1 calc R . . C47 C 0.7409(11) 0.2426(4) 0.4969(4) 0.060(3) Uani 1 1 d . . . H47 H 0.7802 0.2623 0.5111 0.072 Uiso 1 1 calc R . . C48 C 0.8006(11) 0.1952(4) 0.4999(4) 0.057(3) Uani 1 1 d . . . H48 H 0.8791 0.1843 0.5175 0.068 Uiso 1 1 calc R . . C49 C 0.8363(9) 0.4135(4) 0.9471(4) 0.036(3) Uani 1 1 d . . . C50 C 0.7548(10) 0.3818(4) 0.9882(4) 0.043(3) Uani 1 1 d . . . H50 H 0.7675 0.3479 0.9952 0.052 Uiso 1 1 calc R . . C51 C 0.6560(10) 0.4001(4) 1.0183(4) 0.040(3) Uani 1 1 d . . . H51 H 0.6061 0.3783 1.0455 0.048 Uiso 1 1 calc R . . C52 C 0.6315(10) 0.4492(4) 1.0087(4) 0.039(3) Uani 1 1 d . . . H52 H 0.5630 0.4612 1.0282 0.047 Uiso 1 1 calc R . . C53 C 0.7099(10) 0.4806(4) 0.9697(4) 0.040(3) Uani 1 1 d . . . H53 H 0.6965 0.5144 0.9632 0.048 Uiso 1 1 calc R . . C54 C 0.8071(9) 0.4632(4) 0.9403(4) 0.038(3) Uani 1 1 d . . . H54 H 0.8572 0.4860 0.9140 0.046 Uiso 1 1 calc R . . C55 C 1.1059(10) 0.4192(4) 0.9123(4) 0.037(3) Uani 1 1 d . . . C56 C 1.1818(10) 0.4514(4) 0.8725(4) 0.040(3) Uani 1 1 d . . . H56 H 1.1459 0.4606 0.8421 0.049 Uiso 1 1 calc R . . C57 C 1.3066(11) 0.4708(4) 0.8747(4) 0.043(3) Uani 1 1 d . . . H57 H 1.3516 0.4930 0.8466 0.052 Uiso 1 1 calc R . . C58 C 1.3654(10) 0.4569(4) 0.9195(4) 0.042(3) Uani 1 1 d . . . H58 H 1.4515 0.4690 0.9214 0.051 Uiso 1 1 calc R . . C59 C 1.2928(10) 0.4247(4) 0.9613(4) 0.038(3) Uani 1 1 d . . . H59 H 1.3295 0.4154 0.9916 0.046 Uiso 1 1 calc R . . C60 C 1.1657(10) 0.4066(3) 0.9575(4) 0.036(3) Uani 1 1 d . . . H60 H 1.1179 0.3855 0.9857 0.043 Uiso 1 1 calc R . . C61 C 0.9731(10) 0.3352(4) 0.9263(4) 0.039(3) Uani 1 1 d . . . C62 C 1.0957(10) 0.3071(4) 0.9403(3) 0.037(3) Uani 1 1 d . . . H62 H 1.1761 0.3232 0.9406 0.044 Uiso 1 1 calc R . . C63 C 1.1045(10) 0.2560(4) 0.9538(3) 0.037(3) Uani 1 1 d . . . H63 H 1.1905 0.2390 0.9615 0.044 Uiso 1 1 calc R . . C64 C 0.9863(10) 0.2304(4) 0.9558(4) 0.040(3) Uani 1 1 d . . . H64 H 0.9902 0.1962 0.9664 0.048 Uiso 1 1 calc R . . C65 C 0.8616(11) 0.2568(4) 0.9415(4) 0.039(3) Uani 1 1 d . . . H65 H 0.7813 0.2402 0.9423 0.046 Uiso 1 1 calc R . . C66 C 0.8554(10) 0.3080(4) 0.9261(4) 0.046(3) Uani 1 1 d . . . H66 H 0.7717 0.3249 0.9153 0.055 Uiso 1 1 calc R . . C67 C 0.9033(11) 0.4144(4) 0.8537(4) 0.042(3) Uani 1 1 d . . . C68 C 0.9849(11) 0.4004(4) 0.8163(5) 0.048(3) Uani 1 1 d . . . H68 H 1.0698 0.3824 0.8233 0.057 Uiso 1 1 calc R . . C69 C 0.9440(14) 0.4124(4) 0.7694(4) 0.055(3) Uani 1 1 d . . . H69 H 1.0009 0.4023 0.7457 0.066 Uiso 1 1 calc R . . C70 C 0.8206(15) 0.4389(5) 0.7577(5) 0.064(4) Uani 1 1 d . . . H70 H 0.7928 0.4470 0.7262 0.077 Uiso 1 1 calc R . . C71 C 0.7375(13) 0.4538(4) 0.7932(5) 0.062(4) Uani 1 1 d . . . H71 H 0.6544 0.4726 0.7853 0.075 Uiso 1 1 calc R . . C72 C 0.7773(10) 0.4406(4) 0.8401(4) 0.046(3) Uani 1 1 d . . . H72 H 0.7174 0.4498 0.8638 0.055 Uiso 1 1 calc R . . C73 C 0.5085(10) 0.1697(4) 0.0676(3) 0.031(3) Uani 1 1 d . . . C74 C 0.3825(10) 0.1969(4) 0.0550(3) 0.033(3) Uani 1 1 d . . . H74 H 0.3024 0.1798 0.0565 0.040 Uiso 1 1 calc R . . C75 C 0.3693(11) 0.2479(4) 0.0402(4) 0.040(3) Uani 1 1 d . . . H75 H 0.2825 0.2643 0.0327 0.048 Uiso 1 1 calc R . . C76 C 0.4883(11) 0.2738(4) 0.0370(3) 0.038(3) Uani 1 1 d . . . H76 H 0.4831 0.3080 0.0261 0.046 Uiso 1 1 calc R . . C77 C 0.6132(10) 0.2488(4) 0.0498(4) 0.037(3) Uani 1 1 d . . . H77 H 0.6929 0.2662 0.0480 0.044 Uiso 1 1 calc R . . C78 C 0.6233(10) 0.1979(4) 0.0656(4) 0.041(3) Uani 1 1 d . . . H78 H 0.7091 0.1819 0.0752 0.049 Uiso 1 1 calc R . . C79 C 0.5769(10) 0.0949(4) 0.1421(4) 0.037(3) Uani 1 1 d . . . C80 C 0.4906(11) 0.1086(4) 0.1777(4) 0.042(3) Uani 1 1 d . . . H80 H 0.4034 0.1241 0.1691 0.050 Uiso 1 1 calc R . . C81 C 0.5227(12) 0.1011(4) 0.2254(4) 0.050(3) Uani 1 1 d . . . H81 H 0.4595 0.1109 0.2479 0.060 Uiso 1 1 calc R . . C82 C 0.6540(14) 0.0781(4) 0.2380(4) 0.059(4) Uani 1 1 d . . . H82 H 0.6795 0.0727 0.2694 0.071 Uiso 1 1 calc R . . C83 C 0.7451(12) 0.0636(4) 0.2051(4) 0.050(3) Uani 1 1 d . . . H83 H 0.8320 0.0481 0.2139 0.060 Uiso 1 1 calc R . . C84 C 0.7071(10) 0.0721(4) 0.1573(4) 0.043(3) Uani 1 1 d . . . H84 H 0.7707 0.0621 0.1350 0.051 Uiso 1 1 calc R . . C85 C 0.6512(9) 0.0904(4) 0.0508(4) 0.035(3) Uani 1 1 d . . . C86 C 0.7255(10) 0.1216(4) 0.0081(4) 0.038(3) Uani 1 1 d . . . H86 H 0.7073 0.1554 -0.0005 0.046 Uiso 1 1 calc R . . C87 C 0.8262(10) 0.1033(4) -0.0218(4) 0.044(3) Uani 1 1 d . . . H87 H 0.8718 0.1249 -0.0502 0.052 Uiso 1 1 calc R . . C88 C 0.8576(9) 0.0541(4) -0.0097(4) 0.041(3) Uani 1 1 d . . . H88 H 0.9239 0.0420 -0.0297 0.049 Uiso 1 1 calc R . . C89 C 0.7900(10) 0.0225(4) 0.0327(4) 0.040(3) Uani 1 1 d . . . H89 H 0.8132 -0.0111 0.0419 0.048 Uiso 1 1 calc R . . C90 C 0.6886(9) 0.0402(4) 0.0612(4) 0.032(3) Uani 1 1 d . . . H90 H 0.6423 0.0179 0.0889 0.038 Uiso 1 1 calc R . . C91 C 0.3821(9) 0.0829(4) 0.0843(4) 0.034(3) Uani 1 1 d . . . C92 C 0.3227(10) 0.0935(4) 0.0411(4) 0.039(3) Uani 1 1 d . . . H92 H 0.3682 0.1150 0.0126 0.047 Uiso 1 1 calc R . . C93 C 0.1989(11) 0.0738(4) 0.0376(4) 0.049(3) Uani 1 1 d . . . H93 H 0.1622 0.0824 0.0074 0.058 Uiso 1 1 calc R . . C94 C 0.1290(11) 0.0411(4) 0.0794(5) 0.045(3) Uani 1 1 d . . . H94 H 0.0440 0.0282 0.0779 0.054 Uiso 1 1 calc R . . C95 C 0.1880(10) 0.0285(4) 0.1224(4) 0.038(3) Uani 1 1 d . . . H95 H 0.1439 0.0058 0.1504 0.046 Uiso 1 1 calc R . . C96 C 0.3115(10) 0.0483(3) 0.1259(4) 0.040(3) Uani 1 1 d . . . H96 H 0.3490 0.0388 0.1560 0.047 Uiso 1 1 calc R . . N1 N 0.5880(12) 0.4792(4) 0.2755(5) 0.077(3) Uani 1 1 d . . . N2 N 0.3902(13) 0.0959(5) 0.6532(6) 0.118(5) Uani 1 1 d U . . N3 N 0.3237(13) 0.4803(5) 0.6153(5) 0.108(4) Uani 1 1 d U . . N4 N 0.9229(11) 0.0141(4) 0.7352(5) 0.069(3) Uani 1 1 d . . . C97 C 0.5313(13) 0.4675(5) 0.3126(5) 0.066(4) Uani 1 1 d . . . C98 C 0.4513(17) 0.4542(6) 0.3605(6) 0.134(6) Uani 1 1 d U . . H98A H 0.4778 0.4740 0.3785 0.201 Uiso 1 1 calc R . . H98B H 0.4709 0.4201 0.3781 0.201 Uiso 1 1 calc R . . H98C H 0.3518 0.4596 0.3566 0.201 Uiso 1 1 calc R . . C99 C 0.4017(16) 0.0936(6) 0.6130(7) 0.100(5) Uani 1 1 d U . . C100 C 0.4137(15) 0.0904(6) 0.5658(6) 0.112(6) Uani 1 1 d . . . H10A H 0.3241 0.0822 0.5593 0.168 Uiso 1 1 calc R . . H10B H 0.4844 0.0654 0.5634 0.168 Uiso 1 1 calc R . . H10C H 0.4407 0.1214 0.5421 0.168 Uiso 1 1 calc R . . C101 C 0.2222(16) 0.4866(5) 0.5945(6) 0.086(4) Uani 1 1 d U . . C102 C 0.1033(12) 0.4953(4) 0.5677(5) 0.074(4) Uani 1 1 d . . . H10D H 0.1343 0.4993 0.5338 0.111 Uiso 1 1 calc R . . H10E H 0.0520 0.5247 0.5698 0.111 Uiso 1 1 calc R . . H10F H 0.0428 0.4679 0.5812 0.111 Uiso 1 1 calc R . . C103 C 0.9853(15) 0.0287(5) 0.6973(6) 0.069(4) Uani 1 1 d . . . C104 C 1.0601(14) 0.0490(5) 0.6495(5) 0.100(5) Uani 1 1 d U . . H10G H 1.0190 0.0809 0.6332 0.150 Uiso 1 1 calc R . . H10H H 1.0535 0.0278 0.6305 0.150 Uiso 1 1 calc R . . H10I H 1.1579 0.0518 0.6528 0.150 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0322(2) 0.0328(3) 0.0402(3) -0.0095(2) -0.00343(19) -0.00325(19) N1A 0.034(5) 0.050(6) 0.023(6) -0.014(5) 0.004(4) -0.006(4) N2A 0.035(5) 0.039(6) 0.033(6) -0.014(5) 0.008(4) -0.007(4) N3A 0.043(5) 0.038(6) 0.067(8) -0.010(6) -0.006(5) -0.020(5) N4A 0.029(5) 0.050(7) 0.051(7) -0.026(6) -0.002(4) 0.002(5) N5A 0.027(5) 0.032(6) 0.069(8) -0.008(6) -0.004(5) -0.001(4) C1A 0.034(6) 0.031(7) 0.042(8) -0.012(6) 0.003(5) -0.002(5) C2A 0.043(7) 0.046(8) 0.044(8) -0.003(7) -0.013(5) -0.006(6) C3A 0.048(7) 0.027(7) 0.063(9) -0.016(7) -0.010(6) -0.006(5) C4A 0.019(5) 0.049(8) 0.045(8) -0.013(7) 0.005(5) -0.009(5) C5A 0.029(6) 0.042(8) 0.014(6) 0.006(6) 0.001(4) -0.009(5) C6A 0.023(6) 0.045(8) 0.042(8) -0.018(7) 0.006(5) -0.008(5) C7A 0.040(6) 0.041(8) 0.043(9) -0.011(7) 0.007(5) -0.006(5) C8A 0.022(6) 0.054(8) 0.067(9) -0.038(7) -0.002(5) -0.001(5) C9A 0.037(6) 0.047(8) 0.047(9) -0.039(7) 0.007(5) -0.013(6) C10A 0.026(6) 0.054(8) 0.038(8) -0.024(7) 0.006(5) -0.014(5) C11A 0.037(6) 0.042(8) 0.068(10) -0.037(7) 0.002(6) -0.011(6) C12A 0.043(7) 0.042(8) 0.050(9) -0.015(7) -0.004(6) -0.006(6) C13A 0.029(6) 0.036(8) 0.040(9) -0.012(6) 0.006(5) -0.010(5) C14A 0.042(6) 0.035(7) 0.041(8) -0.005(6) -0.003(5) -0.020(5) C15A 0.048(7) 0.050(9) 0.021(7) -0.004(6) -0.003(5) -0.002(7) C16A 0.057(7) 0.039(8) 0.068(9) -0.021(7) -0.005(6) 0.000(6) C17A 0.027(6) 0.048(8) 0.061(10) -0.006(8) -0.007(7) -0.006(5) C18A 0.068(8) 0.053(9) 0.049(9) -0.002(7) -0.014(6) 0.002(6) C19A 0.042(6) 0.018(7) 0.065(10) -0.007(7) -0.006(6) 0.002(5) C20A 0.025(6) 0.048(8) 0.045(8) -0.012(7) -0.008(5) -0.009(6) C21A 0.037(6) 0.045(8) 0.057(9) -0.029(7) -0.009(6) 0.001(6) C22A 0.030(6) 0.055(9) 0.047(9) -0.014(7) 0.017(5) -0.020(6) C23A 0.025(6) 0.042(8) 0.037(8) -0.008(7) 0.011(5) 0.002(5) C24A 0.038(6) 0.049(8) 0.067(9) -0.016(7) -0.005(5) -0.009(6) C25A 0.037(6) 0.057(8) 0.038(8) 0.002(6) 0.006(5) -0.024(6) C26A 0.028(6) 0.056(8) 0.063(8) -0.023(7) -0.002(5) -0.001(6) C27A 0.055(7) 0.049(8) 0.043(8) -0.010(7) 0.008(5) -0.005(6) C28A 0.046(7) 0.073(9) 0.058(9) -0.039(7) 0.008(6) 0.002(6) C29A 0.035(6) 0.034(7) 0.045(8) -0.012(6) 0.000(5) -0.006(5) C30A 0.039(6) 0.039(8) 0.059(10) -0.007(7) -0.009(6) 0.000(6) C31A 0.033(6) 0.050(9) 0.043(9) -0.019(7) 0.003(5) -0.015(6) C32A 0.034(6) 0.039(8) 0.052(9) -0.007(7) -0.015(6) -0.002(6) C33A 0.019(5) 0.044(8) 0.054(9) -0.010(7) -0.004(5) -0.006(5) C34A 0.048(7) 0.048(8) 0.063(9) -0.008(7) -0.008(6) -0.016(6) C35A 0.052(7) 0.039(8) 0.059(9) -0.010(7) -0.004(6) -0.002(6) C36A 0.040(6) 0.049(8) 0.038(8) -0.007(6) -0.003(5) -0.004(5) C37A 0.028(6) 0.054(8) 0.062(9) -0.020(7) -0.006(5) -0.003(5) C38A 0.033(6) 0.059(8) 0.053(8) -0.005(7) -0.016(5) -0.004(6) U2 0.0339(2) 0.0320(3) 0.0382(3) -0.0100(2) -0.00289(19) -0.0038(2) N1B 0.049(5) 0.035(6) 0.022(6) -0.009(5) 0.003(4) -0.008(4) N2B 0.030(5) 0.030(6) 0.050(7) -0.004(5) -0.005(4) -0.006(4) N3B 0.028(5) 0.054(7) 0.044(7) -0.026(6) -0.003(4) -0.002(5) N4B 0.034(5) 0.045(7) 0.050(7) -0.017(5) -0.005(4) 0.000(5) N5B 0.038(5) 0.025(5) 0.034(6) -0.003(5) 0.020(4) -0.009(4) C1B 0.039(6) 0.050(9) 0.051(9) -0.032(7) 0.005(5) -0.009(6) C2B 0.042(7) 0.050(9) 0.050(9) -0.006(7) 0.000(5) -0.007(6) C3B 0.046(7) 0.033(7) 0.066(10) -0.026(7) -0.004(6) -0.001(6) C4B 0.027(6) 0.033(7) 0.041(8) -0.013(6) 0.003(5) -0.004(5) C5B 0.023(6) 0.036(7) 0.063(9) -0.032(7) 0.001(5) -0.003(5) C6B 0.017(5) 0.040(7) 0.040(8) -0.005(6) 0.002(5) -0.012(5) C7B 0.031(6) 0.026(6) 0.041(8) -0.005(6) 0.005(5) 0.001(5) C8B 0.028(6) 0.052(8) 0.028(7) -0.014(6) 0.005(4) -0.011(5) C9B 0.043(6) 0.041(8) 0.047(8) -0.016(7) -0.001(5) -0.023(6) C10B 0.026(6) 0.044(8) 0.038(8) -0.022(7) 0.007(5) -0.011(5) C11B 0.042(6) 0.025(7) 0.055(9) -0.023(6) 0.010(5) -0.003(5) C12B 0.050(7) 0.033(7) 0.050(9) -0.006(7) 0.000(6) -0.013(6) C13B 0.025(6) 0.045(8) 0.049(9) -0.018(7) -0.006(6) -0.005(6) C14B 0.034(6) 0.055(8) 0.040(8) -0.016(7) -0.005(5) -0.005(5) C15B 0.046(7) 0.035(8) 0.044(8) -0.007(6) -0.011(5) -0.009(7) C16B 0.088(8) 0.029(7) 0.044(8) -0.020(6) -0.010(6) 0.000(6) C17B 0.024(6) 0.031(7) 0.040(8) -0.010(6) 0.012(5) 0.001(5) C18B 0.063(7) 0.064(9) 0.028(8) -0.025(6) 0.015(5) -0.013(6) C19B 0.027(6) 0.040(8) 0.041(8) -0.008(7) 0.003(5) 0.000(5) C20B 0.028(6) 0.042(8) 0.033(8) -0.016(6) -0.005(5) -0.010(5) C21B 0.038(6) 0.053(9) 0.057(10) -0.021(8) 0.008(6) -0.026(6) C22B 0.028(6) 0.044(8) 0.036(8) -0.009(7) -0.001(5) -0.009(5) C23B 0.032(6) 0.040(8) 0.035(8) -0.016(7) 0.010(5) -0.015(5) C24B 0.015(5) 0.048(7) 0.054(8) -0.011(6) -0.002(5) 0.008(5) C25B 0.023(5) 0.045(7) 0.042(8) 0.010(6) 0.006(5) 0.004(5) C26B 0.055(7) 0.068(9) 0.046(8) -0.032(7) 0.005(6) -0.012(6) C27B 0.052(7) 0.032(7) 0.060(9) -0.017(6) 0.003(6) -0.006(5) C28B 0.032(6) 0.040(7) 0.047(8) -0.001(6) -0.004(5) -0.006(5) C29B 0.050(7) 0.025(7) 0.043(8) -0.005(6) 0.004(5) -0.002(6) C30B 0.041(6) 0.051(9) 0.033(8) -0.011(7) 0.006(5) -0.010(6) C31B 0.023(5) 0.030(7) 0.050(9) -0.019(6) 0.002(5) 0.010(5) C32B 0.030(6) 0.039(8) 0.041(8) -0.010(7) 0.005(5) -0.001(5) C33B 0.013(5) 0.045(8) 0.048(8) -0.019(7) 0.002(5) -0.009(5) C34B 0.048(7) 0.050(8) 0.088(10) -0.026(7) 0.006(6) -0.010(6) C35B 0.038(6) 0.050(8) 0.063(9) 0.000(7) 0.000(5) -0.013(6) C36B 0.046(7) 0.082(10) 0.060(9) -0.034(8) -0.008(6) -0.007(6) C37B 0.038(6) 0.024(6) 0.069(9) -0.020(6) -0.012(5) 0.003(5) C38B 0.040(6) 0.057(8) 0.062(9) -0.020(7) -0.005(6) -0.020(6) B1 0.045(8) 0.042(9) 0.059(10) -0.018(7) -0.017(7) 0.002(7) B2 0.051(8) 0.034(8) 0.061(10) -0.014(7) -0.012(7) -0.008(7) B3 0.035(7) 0.018(7) 0.051(9) -0.017(6) 0.000(6) 0.007(5) B4 0.021(7) 0.038(8) 0.057(10) -0.007(7) 0.003(6) -0.004(6) C1 0.053(7) 0.039(7) 0.043(8) -0.012(6) -0.007(6) -0.006(6) C2 0.057(7) 0.069(9) 0.031(7) -0.031(7) -0.008(6) 0.001(7) C3 0.072(8) 0.051(8) 0.040(8) -0.016(7) -0.011(7) -0.011(6) C4 0.059(8) 0.040(8) 0.078(11) -0.031(7) 0.013(7) 0.001(6) C5 0.053(8) 0.067(9) 0.056(9) -0.032(7) -0.001(6) -0.004(7) C6 0.041(7) 0.052(8) 0.052(9) -0.006(7) -0.004(6) -0.014(6) C7 0.036(7) 0.056(9) 0.051(8) -0.028(7) -0.007(5) 0.001(6) C8 0.029(6) 0.045(8) 0.094(10) -0.028(7) -0.017(6) 0.004(6) C9 0.046(7) 0.037(7) 0.071(9) -0.020(6) -0.004(6) -0.006(6) C10 0.050(8) 0.059(9) 0.073(10) -0.023(8) -0.009(6) -0.017(7) C11 0.044(7) 0.058(9) 0.079(10) -0.023(8) -0.023(6) -0.002(7) C12 0.037(7) 0.059(9) 0.087(10) -0.015(7) -0.011(6) -0.017(7) C13 0.031(6) 0.050(8) 0.047(8) -0.021(7) -0.008(5) 0.006(6) C14 0.045(7) 0.047(8) 0.077(10) -0.020(7) 0.005(6) -0.006(6) C15 0.050(8) 0.053(9) 0.077(10) -0.013(8) 0.007(7) -0.013(7) C16 0.050(7) 0.038(8) 0.070(10) -0.016(7) -0.001(6) -0.002(6) C17 0.058(7) 0.041(8) 0.062(9) -0.025(7) -0.025(6) 0.014(6) C18 0.051(7) 0.050(8) 0.034(7) -0.005(6) -0.015(5) -0.002(6) C19 0.034(6) 0.027(6) 0.059(9) -0.023(6) 0.005(5) -0.004(5) C20 0.048(7) 0.049(8) 0.052(9) -0.001(7) -0.015(7) -0.005(6) C21 0.050(7) 0.040(7) 0.051(9) -0.017(6) 0.009(6) -0.012(6) C22 0.074(9) 0.038(7) 0.054(9) -0.013(7) -0.022(7) -0.004(6) C23 0.054(7) 0.040(7) 0.049(9) -0.024(7) -0.018(6) 0.010(6) C24 0.063(8) 0.041(7) 0.029(7) -0.020(6) 0.005(6) -0.012(6) C25 0.049(7) 0.043(8) 0.055(9) -0.014(7) -0.010(6) -0.012(6) C26 0.121(11) 0.056(9) 0.043(9) -0.020(8) -0.001(8) -0.005(8) C27 0.118(8) 0.078(8) 0.078(8) -0.031(7) 0.004(7) -0.012(7) C28 0.081(9) 0.068(10) 0.062(10) -0.003(8) -0.011(7) -0.031(8) C29 0.061(8) 0.041(8) 0.035(8) 0.004(7) -0.001(6) 0.000(6) C30 0.046(7) 0.051(9) 0.080(11) -0.029(8) -0.010(6) 0.001(6) C31 0.034(6) 0.033(7) 0.058(8) -0.009(6) -0.006(6) 0.004(6) C32 0.048(8) 0.068(10) 0.062(9) -0.018(7) -0.016(6) 0.008(7) C33 0.048(6) 0.060(7) 0.083(8) -0.008(6) -0.015(6) 0.001(6) C34 0.036(7) 0.051(9) 0.104(12) -0.013(8) -0.007(7) 0.003(7) C35 0.062(8) 0.037(8) 0.072(9) -0.022(7) 0.006(7) -0.018(7) C36 0.035(7) 0.062(9) 0.070(9) -0.021(7) -0.010(6) -0.007(6) C37 0.040(7) 0.039(7) 0.063(9) -0.016(6) -0.005(6) 0.002(6) C38 0.068(8) 0.057(9) 0.062(9) -0.033(7) 0.004(7) -0.022(7) C39 0.082(7) 0.091(8) 0.079(8) -0.030(7) -0.004(6) -0.032(7) C40 0.073(9) 0.070(10) 0.066(10) -0.027(8) -0.002(7) -0.037(8) C41 0.039(7) 0.052(8) 0.084(11) -0.024(8) -0.012(7) -0.019(6) C42 0.039(7) 0.057(9) 0.086(10) -0.022(8) -0.005(6) -0.011(6) C43 0.035(7) 0.048(8) 0.068(9) -0.016(7) -0.001(6) -0.004(6) C44 0.045(7) 0.044(8) 0.068(9) -0.008(7) -0.004(6) 0.009(6) C45 0.053(8) 0.053(9) 0.083(11) -0.009(8) 0.004(7) 0.022(7) C46 0.065(7) 0.052(7) 0.071(7) -0.020(6) 0.011(6) 0.000(6) C47 0.048(8) 0.048(9) 0.083(10) -0.028(7) 0.023(7) -0.016(6) C48 0.038(7) 0.048(8) 0.094(10) -0.036(8) -0.003(6) -0.008(6) C49 0.026(6) 0.038(7) 0.042(8) -0.012(6) -0.009(5) 0.001(5) C50 0.043(7) 0.028(7) 0.060(9) -0.015(6) -0.012(6) -0.001(6) C51 0.032(6) 0.048(8) 0.037(8) -0.011(6) -0.005(5) -0.003(6) C52 0.038(6) 0.034(7) 0.048(8) -0.017(6) -0.008(5) 0.007(6) C53 0.033(6) 0.039(7) 0.054(9) -0.018(7) -0.011(6) -0.002(6) C54 0.023(6) 0.035(7) 0.051(8) -0.004(6) -0.006(5) -0.005(5) C55 0.048(7) 0.031(7) 0.030(7) -0.009(6) 0.006(5) -0.006(5) C56 0.039(6) 0.037(7) 0.052(9) -0.022(6) -0.010(5) 0.004(5) C57 0.060(8) 0.032(7) 0.035(8) -0.009(6) 0.001(6) -0.001(6) C58 0.043(7) 0.038(7) 0.051(9) -0.023(7) 0.009(6) -0.013(6) C59 0.044(7) 0.038(7) 0.032(7) -0.012(6) -0.008(5) 0.000(6) C60 0.042(6) 0.025(6) 0.034(8) -0.004(5) 0.007(5) -0.009(5) C61 0.029(6) 0.035(7) 0.049(8) -0.011(6) 0.005(5) -0.002(5) C62 0.033(6) 0.037(7) 0.044(7) -0.018(6) 0.002(5) -0.013(6) C63 0.046(7) 0.040(7) 0.027(7) -0.019(6) 0.006(5) 0.008(6) C64 0.044(7) 0.035(7) 0.044(8) -0.015(6) 0.003(5) -0.015(6) C65 0.048(7) 0.026(7) 0.047(8) -0.013(6) -0.013(5) -0.008(6) C66 0.034(6) 0.056(8) 0.050(8) -0.017(6) -0.007(5) -0.010(6) C67 0.052(7) 0.039(7) 0.033(8) -0.006(6) 0.005(6) -0.024(6) C68 0.055(7) 0.025(7) 0.055(10) -0.006(6) 0.003(6) -0.004(5) C69 0.097(10) 0.029(7) 0.035(9) -0.008(6) -0.010(7) 0.007(7) C70 0.109(11) 0.042(9) 0.050(10) -0.016(7) -0.028(9) -0.021(8) C71 0.066(8) 0.054(9) 0.065(11) -0.005(8) -0.027(8) -0.022(7) C72 0.039(7) 0.061(8) 0.040(8) -0.013(6) -0.017(5) -0.009(6) C73 0.033(6) 0.038(7) 0.028(7) -0.018(5) -0.003(5) -0.001(5) C74 0.032(6) 0.045(8) 0.027(7) -0.014(6) -0.005(4) -0.006(5) C75 0.040(6) 0.029(7) 0.048(8) -0.007(6) -0.010(5) 0.010(6) C76 0.057(7) 0.016(6) 0.038(7) -0.008(5) 0.007(5) -0.004(6) C77 0.037(6) 0.040(8) 0.036(7) -0.015(6) 0.003(5) -0.006(6) C78 0.031(6) 0.049(8) 0.043(7) -0.016(6) 0.001(5) 0.000(6) C79 0.032(6) 0.029(6) 0.053(8) -0.013(6) -0.009(6) -0.010(5) C80 0.050(7) 0.027(7) 0.055(9) -0.022(6) 0.003(6) -0.008(5) C81 0.061(8) 0.050(8) 0.044(9) -0.022(6) -0.005(6) -0.008(6) C82 0.082(9) 0.047(9) 0.041(9) 0.005(7) -0.021(7) -0.027(7) C83 0.057(8) 0.044(8) 0.046(9) -0.011(7) -0.003(7) -0.016(6) C84 0.035(6) 0.052(8) 0.043(8) -0.016(6) -0.009(5) -0.008(6) C85 0.031(6) 0.034(7) 0.038(8) -0.006(6) -0.008(5) -0.005(5) C86 0.034(6) 0.037(7) 0.055(8) -0.029(7) -0.014(5) 0.005(5) C87 0.035(6) 0.041(8) 0.056(9) -0.011(7) -0.011(6) -0.012(6) C88 0.022(6) 0.060(9) 0.046(9) -0.026(7) -0.004(5) 0.008(6) C89 0.031(6) 0.038(7) 0.052(9) -0.018(7) -0.011(5) 0.007(5) C90 0.035(6) 0.024(7) 0.036(7) -0.009(6) -0.003(5) 0.000(5) C91 0.031(6) 0.031(7) 0.041(8) -0.016(6) -0.004(5) 0.005(5) C92 0.032(6) 0.050(8) 0.044(8) -0.025(6) -0.001(5) -0.012(5) C93 0.043(7) 0.046(8) 0.069(10) -0.034(7) -0.013(6) 0.009(6) C94 0.032(6) 0.032(7) 0.075(10) -0.022(7) -0.007(6) 0.002(5) C95 0.037(6) 0.033(7) 0.044(8) -0.014(6) 0.007(5) -0.006(5) C96 0.040(6) 0.035(7) 0.039(8) -0.006(6) -0.004(5) -0.007(5) N1 0.103(9) 0.051(8) 0.072(10) -0.018(7) 0.002(7) -0.005(6) N2 0.108(7) 0.124(7) 0.120(7) -0.039(6) -0.014(6) 0.006(5) N3 0.109(6) 0.094(7) 0.114(7) -0.020(5) -0.018(5) -0.011(5) N4 0.077(8) 0.046(8) 0.091(11) -0.029(8) -0.020(7) 0.004(6) C97 0.068(9) 0.079(11) 0.043(10) -0.003(8) -0.005(7) -0.027(8) C98 0.127(8) 0.141(9) 0.131(9) -0.038(6) -0.012(6) -0.023(6) C99 0.103(7) 0.101(8) 0.102(8) -0.042(6) -0.007(6) -0.001(6) C100 0.114(12) 0.143(17) 0.093(14) -0.062(12) -0.013(10) 0.013(11) C101 0.092(7) 0.073(7) 0.098(7) -0.027(5) -0.023(6) -0.011(6) C102 0.082(9) 0.045(8) 0.096(11) -0.017(8) -0.027(8) -0.013(7) C103 0.082(11) 0.050(10) 0.081(13) -0.032(10) -0.008(9) 0.001(8) C104 0.094(7) 0.096(7) 0.102(7) -0.025(6) 0.001(6) -0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N5A 2.544(11) . ? U1 N4A 2.557(9) . ? U1 N3A 2.573(10) . ? U1 N1A 2.596(8) . ? U1 N2A 2.615(8) . ? U1 C19A 2.772(10) . ? U1 C31A 2.805(10) . ? U1 C32A 2.831(10) . ? U1 C30A 2.835(10) . ? U1 C23A 2.837(9) . ? U1 C20A 2.839(9) . ? U1 C21A 2.842(9) . ? U1 C29A 2.844(9) . ? U1 C22A 2.845(9) . ? U1 C33A 2.859(9) . ? N1A C1A 1.333(11) . ? N1A C5A 1.355(12) . ? N2A C7A 1.328(12) . ? N2A C6A 1.375(12) . ? N3A C13A 1.145(12) . ? N4A C15A 1.171(12) . ? N5A C17A 1.163(13) . ? C1A C2A 1.382(13) . ? C1A H1A 0.9300 . ? C2A C3A 1.356(13) . ? C2A H2A 0.9300 . ? C3A C4A 1.375(13) . ? C3A H3A 0.9300 . ? C4A C5A 1.414(13) . ? C4A C12A 1.416(14) . ? C5A C6A 1.444(13) . ? C6A C10A 1.397(13) . ? C7A C8A 1.381(13) . ? C7A H7A 0.9300 . ? C8A C9A 1.375(13) . ? C8A H8A 0.9300 . ? C9A C10A 1.374(13) . ? C9A H9A 0.9300 . ? C10A C11A 1.432(14) . ? C11A C12A 1.343(13) . ? C11A H11A 0.9300 . ? C12A H12A 0.9300 . ? C13A C14A 1.447(13) . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C15A C16A 1.457(14) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A C18A 1.428(15) . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A C20A 1.391(14) . ? C19A C23A 1.406(13) . ? C19A C24A 1.518(13) . ? C20A C21A 1.391(14) . ? C20A C25A 1.537(13) . ? C21A C22A 1.400(14) . ? C21A C26A 1.526(13) . ? C22A C23A 1.427(14) . ? C22A C27A 1.507(13) . ? C23A C28A 1.482(13) . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A C33A 1.421(13) . ? C29A C30A 1.432(14) . ? C29A C34A 1.513(13) . ? C30A C31A 1.381(14) . ? C30A C35A 1.498(13) . ? C31A C32A 1.425(14) . ? C31A C36A 1.511(13) . ? C32A C33A 1.430(14) . ? C32A C37A 1.499(13) . ? C33A C38A 1.485(13) . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C35A H35A 0.9600 . ? C35A H35B 0.9600 . ? C35A H35C 0.9600 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37A H37A 0.9600 . ? C37A H37B 0.9600 . ? C37A H37C 0.9600 . ? C38A H38A 0.9600 . ? C38A H38B 0.9600 . ? C38A H38C 0.9600 . ? U2 N4B 2.561(9) . ? U2 N3B 2.564(10) . ? U2 N5B 2.577(9) . ? U2 N1B 2.591(8) . ? U2 N2B 2.603(8) . ? U2 C32B 2.820(9) . ? U2 C29B 2.829(9) . ? U2 C19B 2.836(9) . ? U2 C31B 2.839(9) . ? U2 C30B 2.844(9) . ? U2 C23B 2.844(9) . ? U2 C33B 2.849(8) . ? U2 C22B 2.852(9) . ? U2 C21B 2.853(9) . ? U2 C20B 2.864(9) . ? N1B C5B 1.327(12) . ? N1B C1B 1.336(12) . ? N2B C6B 1.346(11) . ? N2B C7B 1.352(11) . ? N3B C13B 1.139(12) . ? N4B C15B 1.137(12) . ? N5B C17B 1.145(11) . ? C1B C2B 1.411(14) . ? C1B H1B 0.9300 . ? C2B C3B 1.374(14) . ? C2B H2B 0.9300 . ? C3B C4B 1.385(13) . ? C3B H3B 0.9300 . ? C4B C12B 1.405(14) . ? C4B C5B 1.450(13) . ? C5B C6B 1.437(13) . ? C6B C10B 1.437(13) . ? C7B C8B 1.397(12) . ? C7B H7B 0.9300 . ? C8B C9B 1.368(13) . ? C8B H8B 0.9300 . ? C9B C10B 1.381(13) . ? C9B H9B 0.9300 . ? C10B C11B 1.401(13) . ? C11B C12B 1.328(13) . ? C11B H11B 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.471(14) . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B C16B 1.459(14) . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B C18B 1.459(14) . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B C20B 1.417(13) . ? C19B C23B 1.440(13) . ? C19B C24B 1.518(13) . ? C20B C21B 1.373(13) . ? C20B C25B 1.491(12) . ? C21B C22B 1.401(13) . ? C21B C26B 1.539(13) . ? C22B C23B 1.412(13) . ? C22B C27B 1.518(13) . ? C23B C28B 1.494(12) . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C25B H25D 0.9600 . ? C25B H25E 0.9600 . ? C25B H25F 0.9600 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B C33B 1.416(13) . ? C29B C30B 1.422(14) . ? C29B C34B 1.530(13) . ? C30B C31B 1.421(13) . ? C30B C35B 1.504(13) . ? C31B C32B 1.394(13) . ? C31B C36B 1.518(13) . ? C32B C33B 1.436(13) . ? C32B C37B 1.500(12) . ? C33B C38B 1.474(13) . ? C34B H34D 0.9600 . ? C34B H34E 0.9600 . ? C34B H34F 0.9600 . ? C35B H35D 0.9600 . ? C35B H35E 0.9600 . ? C35B H35F 0.9600 . ? C36B H36D 0.9600 . ? C36B H36E 0.9600 . ? C36B H36F 0.9600 . ? C37B H37D 0.9600 . ? C37B H37E 0.9600 . ? C37B H37F 0.9600 . ? C38B H38D 0.9600 . ? C38B H38E 0.9600 . ? C38B H38F 0.9600 . ? B1 C1 1.619(16) . ? B1 C13 1.650(15) . ? B1 C7 1.660(15) . ? B1 C19 1.700(16) . ? B2 C37 1.627(16) . ? B2 C43 1.629(16) . ? B2 C31 1.633(15) . ? B2 C25 1.644(16) . ? B3 C55 1.637(14) . ? B3 C49 1.641(14) . ? B3 C61 1.661(14) . ? B3 C67 1.662(15) . ? B4 C79 1.625(15) . ? B4 C73 1.636(15) . ? B4 C85 1.643(15) . ? B4 C91 1.689(14) . ? C1 C6 1.391(13) . ? C1 C2 1.420(14) . ? C2 C3 1.339(14) . ? C2 H2 0.9300 . ? C3 C4 1.389(14) . ? C3 H3 0.9300 . ? C4 C5 1.407(14) . ? C4 H4 0.9300 . ? C5 C6 1.386(14) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.389(14) . ? C7 C12 1.404(14) . ? C8 C9 1.397(12) . ? C8 H8 0.9300 . ? C9 C10 1.398(14) . ? C9 H9 0.9300 . ? C10 C11 1.356(14) . ? C10 H10 0.9300 . ? C11 C12 1.375(13) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.381(14) . ? C13 C18 1.385(14) . ? C14 C15 1.415(14) . ? C14 H14 0.9300 . ? C15 C16 1.361(14) . ? C15 H15 0.9300 . ? C16 C17 1.375(14) . ? C16 H16 0.9300 . ? C17 C18 1.405(14) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.344(13) . ? C19 C24 1.418(12) . ? C20 C21 1.393(13) . ? C20 H20 0.9300 . ? C21 C22 1.408(13) . ? C21 H21 0.9300 . ? C22 C23 1.378(14) . ? C22 H22 0.9300 . ? C23 C24 1.371(13) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.371(14) . ? C25 C30 1.386(14) . ? C26 C27 1.355(16) . ? C26 H26 0.9300 . ? C27 C28 1.410(16) . ? C27 H27 0.9300 . ? C28 C29 1.348(15) . ? C28 H28 0.9300 . ? C29 C30 1.385(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.387(14) . ? C31 C36 1.392(14) . ? C32 C33 1.414(14) . ? C32 H32 0.9300 . ? C33 C34 1.370(15) . ? C33 H33 0.9300 . ? C34 C35 1.387(14) . ? C34 H34 0.9300 . ? C35 C36 1.409(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.393(14) . ? C37 C42 1.413(13) . ? C38 C39 1.399(15) . ? C38 H38 0.9300 . ? C39 C40 1.374(14) . ? C39 H39 0.9300 . ? C40 C41 1.346(14) . ? C40 H40 0.9300 . ? C41 C42 1.403(14) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.388(14) . ? C43 C44 1.435(14) . ? C44 C45 1.388(14) . ? C44 H44 0.9300 . ? C45 C46 1.370(15) . ? C45 H45 0.9300 . ? C46 C47 1.385(14) . ? C46 H46 0.9300 . ? C47 C48 1.419(13) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.392(13) . ? C49 C50 1.418(13) . ? C50 C51 1.398(13) . ? C50 H50 0.9300 . ? C51 C52 1.356(13) . ? C51 H51 0.9300 . ? C52 C53 1.367(13) . ? C52 H52 0.9300 . ? C53 C54 1.359(13) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.379(13) . ? C55 C60 1.415(13) . ? C56 C57 1.370(12) . ? C56 H56 0.9300 . ? C57 C58 1.398(13) . ? C57 H57 0.9300 . ? C58 C59 1.397(13) . ? C58 H58 0.9300 . ? C59 C60 1.387(12) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.388(13) . ? C61 C66 1.422(12) . ? C62 C63 1.395(12) . ? C62 H62 0.9300 . ? C63 C64 1.382(12) . ? C63 H63 0.9300 . ? C64 C65 1.386(13) . ? C64 H64 0.9300 . ? C65 C66 1.392(13) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.391(14) . ? C67 C68 1.405(14) . ? C68 C69 1.381(14) . ? C68 H68 0.9300 . ? C69 C70 1.363(15) . ? C69 H69 0.9300 . ? C70 C71 1.378(16) . ? C70 H70 0.9300 . ? C71 C72 1.377(14) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 C74 1.397(12) . ? C73 C78 1.399(12) . ? C74 C75 1.389(12) . ? C74 H74 0.9300 . ? C75 C76 1.384(12) . ? C75 H75 0.9300 . ? C76 C77 1.364(13) . ? C76 H76 0.9300 . ? C77 C78 1.385(13) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? C79 C80 1.378(13) . ? C79 C84 1.403(13) . ? C80 C81 1.395(13) . ? C80 H80 0.9300 . ? C81 C82 1.395(15) . ? C81 H81 0.9300 . ? C82 C83 1.357(14) . ? C82 H82 0.9300 . ? C83 C84 1.409(13) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 C90 1.402(12) . ? C85 C86 1.408(13) . ? C86 C87 1.403(13) . ? C86 H86 0.9300 . ? C87 C88 1.361(13) . ? C87 H87 0.9300 . ? C88 C89 1.380(13) . ? C88 H88 0.9300 . ? C89 C90 1.372(12) . ? C89 H89 0.9300 . ? C90 H90 0.9300 . ? C91 C92 1.369(12) . ? C91 C96 1.414(12) . ? C92 C93 1.378(12) . ? C92 H92 0.9300 . ? C93 C94 1.393(14) . ? C93 H93 0.9300 . ? C94 C95 1.354(13) . ? C94 H94 0.9300 . ? C95 C96 1.377(12) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? N1 C97 1.097(13) . ? N2 C99 1.179(18) . ? N3 C101 1.170(15) . ? N4 C103 1.140(15) . ? C97 C98 1.441(18) . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 C100 1.392(19) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 C102 1.409(16) . ? C102 H10D 0.9600 . ? C102 H10E 0.9600 . ? C102 H10F 0.9600 . ? C103 C104 1.431(18) . ? C104 H10G 0.9602 . ? C104 H10H 0.9602 . ? C104 H10I 0.9602 . ? 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 N5A U1 N4A 71.0(3) . . ? N5A U1 N3A 139.8(3) . . ? N4A U1 N3A 68.8(3) . . ? N5A U1 N1A 79.2(3) . . ? N4A U1 N1A 150.2(3) . . ? N3A U1 N1A 141.0(3) . . ? N5A U1 N2A 143.2(3) . . ? N4A U1 N2A 145.8(3) . . ? N3A U1 N2A 77.0(3) . . ? N1A U1 N2A 64.1(3) . . ? C1A N1A C5A 117.0(9) . . ? C1A N1A U1 123.1(7) . . ? C5A N1A U1 119.8(7) . . ? C7A N2A C6A 116.2(9) . . ? C7A N2A U1 125.5(7) . . ? C6A N2A U1 118.3(7) . . ? C13A N3A U1 176.2(9) . . ? C15A N4A U1 175.8(8) . . ? C17A N5A U1 169.9(9) . . ? N1A C1A C2A 123.1(10) . . ? N1A C1A H1A 118.4 . . ? C2A C1A H1A 118.4 . . ? C3A C2A C1A 119.6(10) . . ? C3A C2A H2A 120.2 . . ? C1A C2A H2A 120.2 . . ? C2A C3A C4A 119.9(10) . . ? C2A C3A H3A 120.0 . . ? C4A C3A H3A 120.0 . . ? C3A C4A C5A 117.5(10) . . ? C3A C4A C12A 122.2(11) . . ? C5A C4A C12A 120.3(11) . . ? N1A C5A C4A 122.7(9) . . ? N1A C5A C6A 118.8(10) . . ? C4A C5A C6A 118.4(10) . . ? N2A C6A C10A 121.5(10) . . ? N2A C6A C5A 119.0(10) . . ? C10A C6A C5A 119.4(11) . . ? N2A C7A C8A 125.6(11) . . ? N2A C7A H7A 117.2 . . ? C8A C7A H7A 117.2 . . ? C9A C8A C7A 117.5(11) . . ? C9A C8A H8A 121.2 . . ? C7A C8A H8A 121.2 . . ? C10A C9A C8A 119.6(9) . . ? C10A C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? C9A C10A C6A 119.5(11) . . ? C9A C10A C11A 120.3(10) . . ? C6A C10A C11A 120.1(11) . . ? C12A C11A C10A 120.6(10) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C11A C12A C4A 121.1(11) . . ? C11A C12A H12A 119.4 . . ? C4A C12A H12A 119.4 . . ? N3A C13A C14A 175.9(13) . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? N4A C15A C16A 177.5(11) . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? N5A C17A C18A 178.1(11) . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C20A C19A C23A 109.7(9) . . ? C20A C19A C24A 123.4(11) . . ? C23A C19A C24A 124.0(10) . . ? C19A C20A C21A 107.1(10) . . ? C19A C20A C25A 125.7(11) . . ? C21A C20A C25A 126.3(10) . . ? C20A C21A C22A 109.5(10) . . ? C20A C21A C26A 124.5(10) . . ? C22A C21A C26A 124.2(11) . . ? C21A C22A C23A 107.2(10) . . ? C21A C22A C27A 127.1(11) . . ? C23A C22A C27A 124.3(11) . . ? C19A C23A C22A 106.3(10) . . ? C19A C23A C28A 126.8(11) . . ? C22A C23A C28A 126.2(10) . . ? C19A C24A H24A 109.5 . . ? C19A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C19A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C20A C25A H25A 109.5 . . ? C20A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C20A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C21A C26A H26A 109.5 . . ? C21A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C21A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C22A C27A H27A 109.5 . . ? C22A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C22A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C23A C28A H28A 109.5 . . ? C23A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C23A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C33A C29A C30A 107.8(10) . . ? C33A C29A C34A 123.7(10) . . ? C30A C29A C34A 127.1(10) . . ? C31A C30A C29A 108.1(10) . . ? C31A C30A C35A 126.8(11) . . ? C29A C30A C35A 123.7(11) . . ? C30A C31A C32A 109.4(10) . . ? C30A C31A C36A 123.8(11) . . ? C32A C31A C36A 125.4(11) . . ? C31A C32A C33A 107.0(10) . . ? C31A C32A C37A 125.3(11) . . ? C33A C32A C37A 125.7(10) . . ? C29A C33A C32A 107.6(10) . . ? C29A C33A C38A 125.1(11) . . ? C32A C33A C38A 126.2(11) . . ? C29A C34A H34A 109.5 . . ? C29A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C29A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C30A C35A H35A 109.5 . . ? C30A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C30A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C31A C36A H36A 109.5 . . ? C31A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C31A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C32A C37A H37A 109.5 . . ? C32A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C32A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C33A C38A H38A 109.5 . . ? C33A C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C33A C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? N4B U2 N3B 68.5(3) . . ? N4B U2 N5B 71.3(3) . . ? N3B U2 N5B 139.8(3) . . ? N4B U2 N1B 151.0(3) . . ? N3B U2 N1B 140.5(3) . . ? N5B U2 N1B 79.6(3) . . ? N4B U2 N2B 146.1(3) . . ? N3B U2 N2B 77.7(3) . . ? N5B U2 N2B 142.5(3) . . ? N1B U2 N2B 62.9(3) . . ? C5B N1B C1B 119.3(9) . . ? C5B N1B U2 119.8(7) . . ? C1B N1B U2 120.9(7) . . ? C6B N2B C7B 115.3(9) . . ? C6B N2B U2 120.4(7) . . ? C7B N2B U2 124.3(7) . . ? C13B N3B U2 177.1(7) . . ? C15B N4B U2 173.9(9) . . ? C17B N5B U2 170.5(8) . . ? N1B C1B C2B 123.2(10) . . ? N1B C1B H1B 118.4 . . ? C2B C1B H1B 118.4 . . ? C3B C2B C1B 117.9(11) . . ? C3B C2B H2B 121.0 . . ? C1B C2B H2B 121.0 . . ? C2B C3B C4B 120.5(11) . . ? C2B C3B H3B 119.8 . . ? C4B C3B H3B 119.8 . . ? C3B C4B C12B 123.0(11) . . ? C3B C4B C5B 117.6(10) . . ? C12B C4B C5B 119.4(10) . . ? N1B C5B C6B 120.1(10) . . ? N1B C5B C4B 121.4(11) . . ? C6B C5B C4B 118.4(10) . . ? N2B C6B C10B 125.5(10) . . ? N2B C6B C5B 116.8(10) . . ? C10B C6B C5B 117.6(10) . . ? N2B C7B C8B 124.1(10) . . ? N2B C7B H7B 117.9 . . ? C8B C7B H7B 117.9 . . ? C9B C8B C7B 118.3(10) . . ? C9B C8B H8B 120.9 . . ? C7B C8B H8B 120.9 . . ? C8B C9B C10B 121.8(10) . . ? C8B C9B H9B 119.1 . . ? C10B C9B H9B 119.1 . . ? C9B C10B C11B 123.5(10) . . ? C9B C10B C6B 114.9(10) . . ? C11B C10B C6B 121.5(10) . . ? C12B C11B C10B 120.3(10) . . ? C12B C11B H11B 119.9 . . ? C10B C11B H11B 119.9 . . ? C11B C12B C4B 122.7(11) . . ? C11B C12B H12B 118.7 . . ? C4B C12B H12B 118.7 . . ? N3B C13B C14B 176.2(12) . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? N4B C15B C16B 175.7(12) . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? N5B C17B C18B 178.2(10) . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C20B C19B C23B 107.0(9) . . ? C20B C19B C24B 126.9(10) . . ? C23B C19B C24B 123.5(10) . . ? C21B C20B C19B 107.9(10) . . ? C21B C20B C25B 127.0(10) . . ? C19B C20B C25B 123.5(10) . . ? C20B C21B C22B 110.5(10) . . ? C20B C21B C26B 124.3(11) . . ? C22B C21B C26B 124.2(11) . . ? C21B C22B C23B 107.1(10) . . ? C21B C22B C27B 127.2(10) . . ? C23B C22B C27B 123.9(10) . . ? C22B C23B C19B 107.5(9) . . ? C22B C23B C28B 125.6(10) . . ? C19B C23B C28B 126.0(10) . . ? C19B C24B H24D 109.5 . . ? C19B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C19B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C20B C25B H25D 109.5 . . ? C20B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C20B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C21B C26B H26D 109.5 . . ? C21B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C21B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C22B C27B H27D 109.5 . . ? C22B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C22B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C23B C28B H28D 109.5 . . ? C23B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C23B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C33B C29B C30B 108.4(10) . . ? C33B C29B C34B 123.2(10) . . ? C30B C29B C34B 125.3(10) . . ? C31B C30B C29B 107.0(10) . . ? C31B C30B C35B 129.6(11) . . ? C29B C30B C35B 122.3(10) . . ? C32B C31B C30B 109.3(10) . . ? C32B C31B C36B 127.5(10) . . ? C30B C31B C36B 122.4(10) . . ? C31B C32B C33B 107.8(9) . . ? C31B C32B C37B 125.3(10) . . ? C33B C32B C37B 125.2(10) . . ? C29B C33B C32B 107.4(9) . . ? C29B C33B C38B 129.3(10) . . ? C32B C33B C38B 121.9(10) . . ? C29B C34B H34D 109.5 . . ? C29B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C29B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C30B C35B H35D 109.5 . . ? C30B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C30B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C31B C36B H36D 109.5 . . ? C31B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C31B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C32B C37B H37D 109.5 . . ? C32B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C32B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C33B C38B H38D 109.5 . . ? C33B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C33B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C1 B1 C13 113.2(10) . . ? C1 B1 C7 105.4(8) . . ? C13 B1 C7 111.6(9) . . ? C1 B1 C19 113.2(9) . . ? C13 B1 C19 104.6(8) . . ? C7 B1 C19 108.9(9) . . ? C37 B2 C43 112.4(9) . . ? C37 B2 C31 108.3(10) . . ? C43 B2 C31 108.1(8) . . ? C37 B2 C25 109.4(9) . . ? C43 B2 C25 108.4(10) . . ? C31 B2 C25 110.3(9) . . ? C55 B3 C49 106.9(8) . . ? C55 B3 C61 110.7(8) . . ? C49 B3 C61 111.0(8) . . ? C55 B3 C67 113.8(8) . . ? C49 B3 C67 109.3(8) . . ? C61 B3 C67 105.1(8) . . ? C79 B4 C73 105.5(9) . . ? C79 B4 C85 111.3(8) . . ? C73 B4 C85 112.4(8) . . ? C79 B4 C91 113.0(8) . . ? C73 B4 C91 111.1(8) . . ? C85 B4 C91 103.8(8) . . ? C6 C1 C2 113.8(10) . . ? C6 C1 B1 119.5(10) . . ? C2 C1 B1 126.7(10) . . ? C3 C2 C1 122.8(11) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 122.4(12) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 117.5(11) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C6 C5 C4 118.6(11) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C1 124.8(11) . . ? C5 C6 H6 117.6 . . ? C1 C6 H6 117.6 . . ? C8 C7 C12 115.4(9) . . ? C8 C7 B1 121.9(9) . . ? C12 C7 B1 122.2(10) . . ? C7 C8 C9 122.9(10) . . ? C7 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? C8 C9 C10 119.0(10) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 118.7(10) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 122.0(11) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 121.8(11) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C14 C13 C18 115.7(10) . . ? C14 C13 B1 123.2(10) . . ? C18 C13 B1 121.0(10) . . ? C13 C14 C15 122.0(11) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 120.7(11) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 118.8(11) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C18 119.8(11) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 122.9(11) . . ? C13 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C20 C19 C24 114.1(10) . . ? C20 C19 B1 126.2(9) . . ? C24 C19 B1 119.7(9) . . ? C19 C20 C21 124.7(10) . . ? C19 C20 H20 117.6 . . ? C21 C20 H20 117.6 . . ? C20 C21 C22 118.2(10) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C23 C22 C21 119.8(10) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 118.0(10) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C23 C24 C19 124.9(10) . . ? C23 C24 H24 117.6 . . ? C19 C24 H24 117.6 . . ? C26 C25 C30 112.9(11) . . ? C26 C25 B2 126.5(11) . . ? C30 C25 B2 120.6(11) . . ? C27 C26 C25 123.4(13) . . ? C27 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? C26 C27 C28 121.0(14) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 118.5(13) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 117.4(12) . . ? C28 C29 H29 121.3 . . ? C30 C29 H29 121.3 . . ? C29 C30 C25 126.7(12) . . ? C29 C30 H30 116.7 . . ? C25 C30 H30 116.7 . . ? C32 C31 C36 116.1(10) . . ? C32 C31 B2 123.6(10) . . ? C36 C31 B2 120.2(9) . . ? C31 C32 C33 121.0(11) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 122.1(11) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 118.0(11) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? C34 C35 C36 119.7(11) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 123.0(11) . . ? C31 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? C38 C37 C42 111.6(10) . . ? C38 C37 B2 124.7(9) . . ? C42 C37 B2 123.4(10) . . ? C37 C38 C39 125.5(11) . . ? C37 C38 H38 117.2 . . ? C39 C38 H38 117.3 . . ? C40 C39 C38 119.1(12) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 119.2(11) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 120.7(10) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 123.7(11) . . ? C41 C42 H42 118.1 . . ? C37 C42 H42 118.1 . . ? C48 C43 C44 112.7(11) . . ? C48 C43 B2 123.2(10) . . ? C44 C43 B2 124.1(10) . . ? C45 C44 C43 122.9(11) . . ? C45 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C46 C45 C44 120.9(12) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 120.3(12) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C48 117.2(11) . . ? C46 C47 H47 121.4 . . ? C48 C47 H47 121.4 . . ? C43 C48 C47 126.0(11) . . ? C43 C48 H48 117.0 . . ? C47 C48 H48 117.0 . . ? C54 C49 C50 113.7(9) . . ? C54 C49 B3 120.5(9) . . ? C50 C49 B3 125.8(10) . . ? C51 C50 C49 121.5(10) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C52 C51 C50 121.2(10) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 118.3(10) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? C54 C53 C52 120.9(10) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 C49 124.2(10) . . ? C53 C54 H54 117.9 . . ? C49 C54 H54 117.9 . . ? C56 C55 C60 115.1(9) . . ? C56 C55 B3 124.5(9) . . ? C60 C55 B3 120.4(9) . . ? C57 C56 C55 124.4(10) . . ? C57 C56 H56 117.8 . . ? C55 C56 H56 117.8 . . ? C56 C57 C58 119.4(10) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C59 C58 C57 118.9(9) . . ? C59 C58 H58 120.6 . . ? C57 C58 H58 120.6 . . ? C60 C59 C58 119.7(9) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C59 C60 C55 122.4(9) . . ? C59 C60 H60 118.8 . . ? C55 C60 H60 118.8 . . ? C62 C61 C66 114.9(9) . . ? C62 C61 B3 125.4(8) . . ? C66 C61 B3 119.8(9) . . ? C61 C62 C63 123.4(9) . . ? C61 C62 H62 118.3 . . ? C63 C62 H62 118.3 . . ? C64 C63 C62 120.3(9) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 118.4(10) . . ? C63 C64 H64 120.8 . . ? C65 C64 H64 120.8 . . ? C64 C65 C66 120.8(9) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C65 C66 C61 122.1(10) . . ? C65 C66 H66 119.0 . . ? C61 C66 H66 119.0 . . ? C72 C67 C68 114.8(10) . . ? C72 C67 B3 125.6(10) . . ? C68 C67 B3 119.4(10) . . ? C69 C68 C67 122.6(11) . . ? C69 C68 H68 118.7 . . ? C67 C68 H68 118.7 . . ? C70 C69 C68 120.2(12) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C71 119.3(12) . . ? C69 C70 H70 120.4 . . ? C71 C70 H70 120.4 . . ? C72 C71 C70 120.1(12) . . ? C72 C71 H71 119.9 . . ? C70 C71 H71 119.9 . . ? C71 C72 C67 122.9(11) . . ? C71 C72 H72 118.5 . . ? C67 C72 H72 118.6 . . ? C74 C73 C78 114.7(9) . . ? C74 C73 B4 126.7(8) . . ? C78 C73 B4 118.5(9) . . ? C75 C74 C73 124.0(9) . . ? C75 C74 H74 118.0 . . ? C73 C74 H74 118.0 . . ? C76 C75 C74 118.5(9) . . ? C76 C75 H75 120.8 . . ? C74 C75 H75 120.8 . . ? C77 C76 C75 119.6(9) . . ? C77 C76 H76 120.2 . . ? C75 C76 H76 120.2 . . ? C76 C77 C78 121.0(9) . . ? C76 C77 H77 119.5 . . ? C78 C77 H77 119.5 . . ? C77 C78 C73 122.1(9) . . ? C77 C78 H78 118.9 . . ? C73 C78 H78 118.9 . . ? C80 C79 C84 114.4(10) . . ? C80 C79 B4 120.2(9) . . ? C84 C79 B4 125.3(10) . . ? C79 C80 C81 125.5(11) . . ? C79 C80 H80 117.2 . . ? C81 C80 H80 117.2 . . ? C80 C81 C82 117.1(11) . . ? C80 C81 H81 121.5 . . ? C82 C81 H81 121.5 . . ? C83 C82 C81 120.9(11) . . ? C83 C82 H82 119.5 . . ? C81 C82 H82 119.5 . . ? C82 C83 C84 119.6(11) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? C79 C84 C83 122.5(10) . . ? C79 C84 H84 118.8 . . ? C83 C84 H84 118.8 . . ? C90 C85 C86 114.7(9) . . ? C90 C85 B4 121.4(9) . . ? C86 C85 B4 123.9(9) . . ? C87 C86 C85 121.9(10) . . ? C87 C86 H86 119.1 . . ? C85 C86 H86 119.1 . . ? C88 C87 C86 120.6(10) . . ? C88 C87 H87 119.7 . . ? C86 C87 H87 119.7 . . ? C87 C88 C89 119.2(10) . . ? C87 C88 H88 120.4 . . ? C89 C88 H88 120.4 . . ? C90 C89 C88 120.3(10) . . ? C90 C89 H89 119.9 . . ? C88 C89 H89 119.9 . . ? C89 C90 C85 123.3(10) . . ? C89 C90 H90 118.3 . . ? C85 C90 H90 118.3 . . ? C92 C91 C96 115.7(9) . . ? C92 C91 B4 121.1(9) . . ? C96 C91 B4 123.2(9) . . ? C91 C92 C93 123.3(10) . . ? C91 C92 H92 118.4 . . ? C93 C92 H92 118.4 . . ? C92 C93 C94 119.8(10) . . ? C92 C93 H93 120.1 . . ? C94 C93 H93 120.1 . . ? C95 C94 C93 118.3(10) . . ? C95 C94 H94 120.9 . . ? C93 C94 H94 120.9 . . ? C94 C95 C96 121.8(10) . . ? C94 C95 H95 119.1 . . ? C96 C95 H95 119.1 . . ? C95 C96 C91 121.0(9) . . ? C95 C96 H96 119.5 . . ? C91 C96 H96 119.5 . . ? N1 C97 C98 177.0(18) . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N2 C99 C100 179.1(19) . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N3 C101 C102 177.6(18) . . ? C101 C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? N4 C103 C104 177.5(16) . . ? C103 C104 H10G 109.5 . . ? C103 C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? C103 C104 H10I 109.5 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 764414' #TrackingRef 'revisedC002279ACIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H47 N5 U, 2(C24 H20 B)' _chemical_formula_sum 'C87 H87 B2 N5 U' _chemical_formula_weight 1462.27 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' B B 0.0013 0.0007 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6247(8) _cell_length_b 25.487(2) _cell_length_c 29.339(3) _cell_angle_alpha 85.358(5) _cell_angle_beta 86.673(5) _cell_angle_gamma 81.625(6) _cell_volume 7089.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 159383 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 2.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; Crystal-to-detector distance 40 mm. The Rint value is quite large, which is due to the low crystal quality. There is however no ambiguity on the crystal system (triclinic) choice. The data completeness is only 0.93 since a significant part of the data was rejected during treatment with HKL2000, owing to the low quality of the crystal and, hence, the data. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and six \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 159383 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.68 _reflns_number_total 25070 _reflns_number_gt 9461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Due to the low quality of the data, restraints on displacement parameters had to be applied for several atoms, particularly in the acetonitrile molecules and the counter-ions. Restraints on bond lengths had also to be applied for the acetonitrile molecule containing N5B. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. The largest residual electron density peak is located near atom U1. There are some solvent accessible voids in the structure, but the corresponding solvent molecules are unresolved. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 25070 _refine_ls_number_parameters 1735 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.2249 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 3.180 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.132 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.73311(5) 0.743175(17) 0.631330(17) 0.04208(17) Uani 1 1 d . . . N1A N 0.7416(9) 0.7837(4) 0.7084(3) 0.042(3) Uani 1 1 d U . . N2A N 0.7517(10) 0.8422(4) 0.6261(4) 0.047(3) Uani 1 1 d . . . N3A N 0.7432(10) 0.7859(4) 0.5506(3) 0.045(3) Uani 1 1 d . . . N4A N 0.7188(10) 0.6592(4) 0.5881(4) 0.059(3) Uani 1 1 d . . . N5A N 0.7133(9) 0.6584(4) 0.6880(3) 0.045(3) Uani 1 1 d . . . C1A C 0.7382(12) 0.7562(5) 0.7470(5) 0.056(4) Uani 1 1 d U . . H1A H 0.7288 0.7204 0.7466 0.067 Uiso 1 1 calc R . . C2A C 0.7476(13) 0.7758(5) 0.7888(5) 0.055(4) Uani 1 1 d . . . H2A H 0.7437 0.7538 0.8156 0.066 Uiso 1 1 calc R . . C3A C 0.7623(13) 0.8269(5) 0.7904(4) 0.059(4) Uani 1 1 d . . . H3A H 0.7734 0.8408 0.8181 0.070 Uiso 1 1 calc R . . C4A C 0.7604(12) 0.8592(5) 0.7493(5) 0.055(4) Uani 1 1 d . . . H4A H 0.7656 0.8953 0.7498 0.066 Uiso 1 1 calc R . . C5A C 0.7511(12) 0.8378(5) 0.7083(4) 0.045(3) Uani 1 1 d . . . C6A C 0.7571(12) 0.8695(5) 0.6636(5) 0.048(4) Uani 1 1 d . . . C7A C 0.7688(12) 0.9221(5) 0.6602(4) 0.052(4) Uani 1 1 d . . . H7A H 0.7730 0.9396 0.6866 0.062 Uiso 1 1 calc R . . C8A C 0.7745(13) 0.9497(5) 0.6182(5) 0.061(4) Uani 1 1 d . . . H8A H 0.7817 0.9858 0.6162 0.074 Uiso 1 1 calc R . . C9A C 0.7698(12) 0.9245(5) 0.5801(5) 0.049(4) Uani 1 1 d . . . H9A H 0.7732 0.9427 0.5514 0.059 Uiso 1 1 calc R . . C10A C 0.7595(11) 0.8690(5) 0.5847(5) 0.044(4) Uani 1 1 d . . . C11A C 0.7517(11) 0.8399(5) 0.5441(5) 0.042(4) Uani 1 1 d . . . C12A C 0.7525(12) 0.8625(6) 0.4983(6) 0.068(5) Uani 1 1 d . . . H12A H 0.7569 0.8987 0.4930 0.082 Uiso 1 1 calc R . . C13A C 0.7471(12) 0.8325(5) 0.4609(5) 0.053(4) Uani 1 1 d . . . H13A H 0.7459 0.8488 0.4314 0.063 Uiso 1 1 calc R . . C14A C 0.7435(12) 0.7777(5) 0.4681(5) 0.057(4) Uani 1 1 d . . . H14A H 0.7427 0.7560 0.4442 0.069 Uiso 1 1 calc R . . C15A C 0.7413(11) 0.7584(5) 0.5136(4) 0.037(3) Uani 1 1 d . . . H15A H 0.7381 0.7221 0.5192 0.044 Uiso 1 1 calc R . . C16A C 0.7219(14) 0.6180(5) 0.5758(5) 0.059(4) Uani 1 1 d . . . C17A C 0.7214(15) 0.5640(5) 0.5636(5) 0.087(5) Uani 1 1 d . . . H17A H 0.8026 0.5417 0.5752 0.130 Uiso 1 1 calc R . . H17B H 0.7233 0.5635 0.5309 0.130 Uiso 1 1 calc R . . H17C H 0.6379 0.5511 0.5766 0.130 Uiso 1 1 calc R . . C18A C 0.6922(12) 0.6186(5) 0.7057(4) 0.047(4) Uani 1 1 d . . . C19A C 0.6626(12) 0.5685(4) 0.7289(4) 0.058(4) Uani 1 1 d . . . H19A H 0.7376 0.5544 0.7485 0.088 Uiso 1 1 calc R . . H19B H 0.6544 0.5437 0.7066 0.088 Uiso 1 1 calc R . . H19C H 0.5760 0.5745 0.7469 0.088 Uiso 1 1 calc R . . C20A C 1.0159(12) 0.7531(4) 0.6524(5) 0.044(4) Uani 1 1 d . . . C21A C 0.9988(13) 0.7010(5) 0.6705(5) 0.050(4) Uani 1 1 d . . . C22A C 0.9927(11) 0.6734(5) 0.6318(4) 0.036(3) Uani 1 1 d U . . C23A C 1.0010(13) 0.7064(6) 0.5891(6) 0.063(4) Uani 1 1 d . . . C24A C 1.0162(13) 0.7567(5) 0.6030(6) 0.050(4) Uani 1 1 d . . . C25A C 1.0629(13) 0.7960(4) 0.6802(4) 0.062(4) Uani 1 1 d . . . H25A H 1.0401 0.7886 0.7121 0.093 Uiso 1 1 calc R . . H25B H 1.0151 0.8304 0.6701 0.093 Uiso 1 1 calc R . . H25C H 1.1625 0.7957 0.6755 0.093 Uiso 1 1 calc R . . C26A C 1.0202(12) 0.6778(4) 0.7176(4) 0.050(4) Uani 1 1 d . . . H26A H 1.0067 0.7056 0.7383 0.075 Uiso 1 1 calc R . . H26B H 1.1141 0.6591 0.7195 0.075 Uiso 1 1 calc R . . H26C H 0.9539 0.6535 0.7257 0.075 Uiso 1 1 calc R . . C27A C 1.0045(12) 0.6131(4) 0.6328(4) 0.054(4) Uani 1 1 d . . . H27A H 1.0872 0.5972 0.6482 0.081 Uiso 1 1 calc R . . H27B H 1.0106 0.6024 0.6020 0.081 Uiso 1 1 calc R . . H27C H 0.9229 0.6016 0.6487 0.081 Uiso 1 1 calc R . . C28A C 1.0289(12) 0.6881(5) 0.5417(5) 0.066(4) Uani 1 1 d . . . H28A H 1.0176 0.7183 0.5198 0.099 Uiso 1 1 calc R . . H28B H 0.9637 0.6644 0.5362 0.099 Uiso 1 1 calc R . . H28C H 1.1232 0.6698 0.5388 0.099 Uiso 1 1 calc R . . C29A C 1.0679(13) 0.8003(5) 0.5724(4) 0.066(4) Uani 1 1 d . . . H29A H 1.1684 0.7968 0.5729 0.098 Uiso 1 1 calc R . . H29B H 1.0273 0.8341 0.5830 0.098 Uiso 1 1 calc R . . H29C H 1.0410 0.7980 0.5417 0.098 Uiso 1 1 calc R . . C30A C 0.4636(11) 0.8020(4) 0.6103(4) 0.034(3) Uani 1 1 d . . . C31A C 0.4650(11) 0.7985(4) 0.6579(4) 0.033(3) Uani 1 1 d . . . C32A C 0.4592(12) 0.7438(5) 0.6734(4) 0.046(4) Uani 1 1 d . . . C33A C 0.4541(11) 0.7161(4) 0.6346(4) 0.038(3) Uani 1 1 d . . . C34A C 0.4607(12) 0.7531(5) 0.5959(5) 0.047(4) Uani 1 1 d . . . C35A C 0.4346(11) 0.8549(4) 0.5818(4) 0.058(4) Uani 1 1 d . . . H35A H 0.4559 0.8493 0.5500 0.087 Uiso 1 1 calc R . . H35B H 0.4924 0.8793 0.5914 0.087 Uiso 1 1 calc R . . H35C H 0.3373 0.8694 0.5860 0.087 Uiso 1 1 calc R . . C36A C 0.4361(11) 0.8432(5) 0.6896(4) 0.060(4) Uani 1 1 d . . . H36A H 0.4839 0.8722 0.6775 0.090 Uiso 1 1 calc R . . H36B H 0.4692 0.8307 0.7193 0.090 Uiso 1 1 calc R . . H36C H 0.3368 0.8551 0.6920 0.090 Uiso 1 1 calc R . . C37A C 0.4251(12) 0.7229(5) 0.7224(4) 0.064(4) Uani 1 1 d . . . H37A H 0.3405 0.7432 0.7340 0.095 Uiso 1 1 calc R . . H37B H 0.5012 0.7260 0.7413 0.095 Uiso 1 1 calc R . . H37C H 0.4122 0.6862 0.7228 0.095 Uiso 1 1 calc R . . C38A C 0.4136(12) 0.6599(4) 0.6336(4) 0.056(4) Uani 1 1 d . . . H38A H 0.4739 0.6352 0.6528 0.084 Uiso 1 1 calc R . . H38B H 0.4240 0.6493 0.6028 0.084 Uiso 1 1 calc R . . H38C H 0.3177 0.6600 0.6447 0.084 Uiso 1 1 calc R . . C39A C 0.4359(12) 0.7398(5) 0.5485(4) 0.057(4) Uani 1 1 d . . . H39A H 0.3426 0.7309 0.5476 0.085 Uiso 1 1 calc R . . H39B H 0.5032 0.7101 0.5402 0.085 Uiso 1 1 calc R . . H39C H 0.4460 0.7699 0.5274 0.085 Uiso 1 1 calc R . . U2 U 0.77470(5) 0.261191(17) 0.890738(17) 0.04454(17) Uani 1 1 d . . . N1B N 0.7555(9) 0.1614(4) 0.9029(4) 0.045(3) Uani 1 1 d . . . N2B N 0.7519(10) 0.2225(4) 0.9743(4) 0.049(3) Uani 1 1 d . . . N3B N 0.7705(11) 0.3281(4) 0.9533(4) 0.062(3) Uani 1 1 d . . . N4B N 0.8003(11) 0.3465(4) 0.8393(4) 0.059(3) Uani 1 1 d . . . N5B N 0.7961(13) 0.2374(5) 0.8083(3) 0.088(4) Uani 1 1 d DU . . C1B C 0.7537(12) 0.1324(5) 0.8679(5) 0.051(4) Uani 1 1 d . . . H1B H 0.7586 0.1494 0.8387 0.061 Uiso 1 1 calc R . . C2B C 0.7446(12) 0.0766(5) 0.8715(5) 0.062(4) Uani 1 1 d . . . H2B H 0.7491 0.0568 0.8461 0.075 Uiso 1 1 calc R . . C3B C 0.7289(12) 0.0549(5) 0.9152(5) 0.052(4) Uani 1 1 d . . . H3B H 0.7165 0.0193 0.9198 0.063 Uiso 1 1 calc R . . C4B C 0.7306(12) 0.0840(5) 0.9526(5) 0.056(4) Uani 1 1 d . . . H4B H 0.7213 0.0682 0.9821 0.068 Uiso 1 1 calc R . . C5B C 0.7468(12) 0.1380(5) 0.9456(5) 0.043(4) Uani 1 1 d . . . C6B C 0.7499(12) 0.1696(6) 0.9843(5) 0.051(4) Uani 1 1 d . . . C7B C 0.7581(12) 0.1468(5) 1.0285(5) 0.048(4) Uani 1 1 d . . . H7B H 0.7561 0.1104 1.0343 0.057 Uiso 1 1 calc R . . C8B C 0.7687(12) 0.1765(5) 1.0625(5) 0.056(4) Uani 1 1 d . . . H8B H 0.7775 0.1614 1.0923 0.068 Uiso 1 1 calc R . . C9B C 0.7666(12) 0.2295(5) 1.0532(5) 0.060(4) Uani 1 1 d . . . H9B H 0.7721 0.2507 1.0772 0.072 Uiso 1 1 calc R . . C10B C 0.7565(13) 0.2534(5) 1.0088(6) 0.064(5) Uani 1 1 d . . . C11B C 0.7603(14) 0.3106(5) 0.9996(5) 0.065(4) Uani 1 1 d . . . C12B C 0.7483(12) 0.3492(5) 1.0335(4) 0.051(4) Uani 1 1 d . . . H12B H 0.7323 0.3384 1.0641 0.061 Uiso 1 1 calc R . . C13B C 0.7597(13) 0.4001(5) 1.0218(5) 0.072(5) Uani 1 1 d . . . H13B H 0.7614 0.4238 1.0442 0.086 Uiso 1 1 calc R . . C14B C 0.7692(12) 0.4174(5) 0.9751(5) 0.056(4) Uani 1 1 d . . . H14B H 0.7694 0.4531 0.9657 0.067 Uiso 1 1 calc R . . C15B C 0.7782(11) 0.3793(5) 0.9436(5) 0.045(3) Uani 1 1 d . . . H15B H 0.7908 0.3906 0.9129 0.054 Uiso 1 1 calc R . . C16B C 0.7976(12) 0.3851(5) 0.8174(4) 0.044(3) Uani 1 1 d . . . C17B C 0.8009(12) 0.4357(4) 0.7908(4) 0.051(4) Uani 1 1 d . . . H17D H 0.7083 0.4557 0.7911 0.077 Uiso 1 1 calc R . . H17E H 0.8324 0.4294 0.7599 0.077 Uiso 1 1 calc R . . H17F H 0.8642 0.4555 0.8040 0.077 Uiso 1 1 calc R . . C18B C 0.7936(13) 0.2278(5) 0.7706(4) 0.064(4) Uani 1 1 d DU . . C19B C 0.8005(15) 0.2143(5) 0.7215(4) 0.084(5) Uani 1 1 d DU . . H19D H 0.7543 0.1837 0.7192 0.126 Uiso 1 1 calc R . . H19E H 0.8970 0.2066 0.7109 0.126 Uiso 1 1 calc R . . H19F H 0.7544 0.2439 0.7031 0.126 Uiso 1 1 calc R . . C20B C 1.0428(12) 0.2558(5) 0.9310(5) 0.047(4) Uani 1 1 d . . . C21B C 1.0388(13) 0.2042(5) 0.9138(6) 0.059(4) Uani 1 1 d . . . C22B C 1.0446(13) 0.2064(6) 0.8658(5) 0.055(4) Uani 1 1 d . . . C23B C 1.0548(13) 0.2599(6) 0.8525(6) 0.060(5) Uani 1 1 d . . . C24B C 1.0508(13) 0.2883(5) 0.8903(6) 0.057(5) Uani 1 1 d . . . C25B C 1.0698(14) 0.2665(6) 0.9770(5) 0.081(5) Uani 1 1 d U . . H25D H 1.1688 0.2587 0.9815 0.122 Uiso 1 1 calc R . . H25E H 1.0203 0.2446 0.9985 0.122 Uiso 1 1 calc R . . H25F H 1.0381 0.3033 0.9815 0.122 Uiso 1 1 calc R . . C26B C 1.0647(14) 0.1515(5) 0.9448(5) 0.085(5) Uani 1 1 d U . . H26D H 1.0227 0.1244 0.9319 0.128 Uiso 1 1 calc R . . H26E H 1.0235 0.1572 0.9749 0.128 Uiso 1 1 calc R . . H26F H 1.1640 0.1403 0.9467 0.128 Uiso 1 1 calc R . . C27B C 1.0736(15) 0.1581(6) 0.8377(5) 0.092(5) Uani 1 1 d U . . H27D H 1.1727 0.1504 0.8305 0.138 Uiso 1 1 calc R . . H27E H 1.0243 0.1653 0.8098 0.138 Uiso 1 1 calc R . . H27F H 1.0422 0.1280 0.8549 0.138 Uiso 1 1 calc R . . C28B C 1.0876(14) 0.2775(6) 0.8024(5) 0.092(5) Uani 1 1 d . . . H28D H 1.0426 0.3133 0.7957 0.138 Uiso 1 1 calc R . . H28E H 1.0533 0.2543 0.7829 0.138 Uiso 1 1 calc R . . H28F H 1.1874 0.2761 0.7971 0.138 Uiso 1 1 calc R . . C29B C 1.0894(13) 0.3436(5) 0.8897(5) 0.076(4) Uani 1 1 d U . . H29D H 1.1890 0.3415 0.8923 0.114 Uiso 1 1 calc R . . H29E H 1.0412 0.3614 0.9150 0.114 Uiso 1 1 calc R . . H29F H 1.0624 0.3633 0.8615 0.114 Uiso 1 1 calc R . . C30B C 0.5144(12) 0.3313(5) 0.8847(5) 0.047(4) Uani 1 1 d . . . C31B C 0.4954(11) 0.2959(4) 0.9250(4) 0.029(3) Uani 1 1 d . . . C32B C 0.4903(10) 0.2436(4) 0.9098(4) 0.032(3) Uani 1 1 d . . . C33B C 0.5036(12) 0.2452(5) 0.8620(4) 0.037(3) Uani 1 1 d . . . C34B C 0.5190(11) 0.2999(5) 0.8467(5) 0.047(4) Uani 1 1 d . . . C35B C 0.4917(11) 0.3902(4) 0.8820(4) 0.048(3) Uani 1 1 d . . . H35D H 0.5325 0.4037 0.8536 0.072 Uiso 1 1 calc R . . H35E H 0.5351 0.4024 0.9071 0.072 Uiso 1 1 calc R . . H35F H 0.3926 0.4028 0.8837 0.072 Uiso 1 1 calc R . . C36B C 0.4486(13) 0.3136(4) 0.9715(4) 0.053(4) Uani 1 1 d . . . H36D H 0.4848 0.2869 0.9944 0.080 Uiso 1 1 calc R . . H36E H 0.3477 0.3191 0.9743 0.080 Uiso 1 1 calc R . . H36F H 0.4832 0.3463 0.9756 0.080 Uiso 1 1 calc R . . C37B C 0.4388(11) 0.1979(5) 0.9405(5) 0.065(4) Uani 1 1 d . . . H37D H 0.3380 0.2017 0.9410 0.097 Uiso 1 1 calc R . . H37E H 0.4688 0.1988 0.9711 0.097 Uiso 1 1 calc R . . H37F H 0.4773 0.1645 0.9287 0.097 Uiso 1 1 calc R . . C38B C 0.4710(13) 0.2061(5) 0.8316(5) 0.075(5) Uani 1 1 d . . . H38D H 0.4879 0.1712 0.8467 0.112 Uiso 1 1 calc R . . H38E H 0.5298 0.2076 0.8041 0.112 Uiso 1 1 calc R . . H38F H 0.3741 0.2141 0.8240 0.112 Uiso 1 1 calc R . . C39B C 0.5112(13) 0.3230(5) 0.7965(4) 0.057(4) Uani 1 1 d . . . H39D H 0.4227 0.3452 0.7925 0.086 Uiso 1 1 calc R . . H39E H 0.5200 0.2944 0.7766 0.086 Uiso 1 1 calc R . . H39F H 0.5863 0.3437 0.7893 0.086 Uiso 1 1 calc R . . B1 B 0.5584(15) 0.0574(6) 0.1424(5) 0.044(4) Uani 1 1 d . . . B2 B 0.2312(16) 0.4068(5) 0.1144(5) 0.050(4) Uani 1 1 d . . . B3 B 0.6966(18) 0.4050(6) 0.6317(5) 0.054(5) Uani 1 1 d . . . B4 B 0.9839(16) 0.9250(6) 0.3713(6) 0.055(4) Uani 1 1 d . . . C1 C 0.6595(13) 0.0292(5) 0.1025(4) 0.046(3) Uani 1 1 d . . . C2 C 0.6151(13) 0.0020(5) 0.0690(5) 0.055(4) Uani 1 1 d . . . H2 H 0.5189 0.0009 0.0692 0.066 Uiso 1 1 calc R . . C3 C 0.6947(14) -0.0234(5) 0.0356(4) 0.052(4) Uani 1 1 d . . . H3 H 0.6553 -0.0412 0.0143 0.062 Uiso 1 1 calc R . . C4 C 0.8384(13) -0.0214(5) 0.0349(5) 0.051(4) Uani 1 1 d . . . H4 H 0.8975 -0.0379 0.0125 0.061 Uiso 1 1 calc R . . C5 C 0.8928(14) 0.0044(5) 0.0667(5) 0.048(4) Uani 1 1 d . . . H5 H 0.9889 0.0059 0.0656 0.057 Uiso 1 1 calc R . . C6 C 0.8085(13) 0.0281(5) 0.1001(4) 0.044(3) Uani 1 1 d . . . H6 H 0.8494 0.0442 0.1222 0.053 Uiso 1 1 calc R . . C7 C 0.3994(13) 0.0741(5) 0.1209(5) 0.052(4) Uani 1 1 d . . . C8 C 0.3848(13) 0.1016(5) 0.0783(5) 0.053(4) Uani 1 1 d . . . H8 H 0.4650 0.1108 0.0623 0.064 Uiso 1 1 calc R . . C9 C 0.2578(14) 0.1160(5) 0.0589(4) 0.051(3) Uani 1 1 d . . . H9 H 0.2529 0.1349 0.0304 0.061 Uiso 1 1 calc R . . C10 C 0.1352(14) 0.1021(5) 0.0818(5) 0.053(4) Uani 1 1 d U . . H10 H 0.0491 0.1106 0.0683 0.063 Uiso 1 1 calc R . . C11 C 0.1434(13) 0.0753(5) 0.1250(5) 0.055(4) Uani 1 1 d . . . H11 H 0.0629 0.0664 0.1410 0.066 Uiso 1 1 calc R . . C12 C 0.2708(12) 0.0626(5) 0.1434(4) 0.045(3) Uani 1 1 d . . . H12 H 0.2746 0.0452 0.1725 0.055 Uiso 1 1 calc R . . C13 C 0.6129(12) 0.1130(5) 0.1580(4) 0.043(3) Uani 1 1 d . . . C14 C 0.5460(12) 0.1624(5) 0.1492(4) 0.047(3) Uani 1 1 d . . . H14 H 0.4609 0.1669 0.1350 0.056 Uiso 1 1 calc R . . C15 C 0.5993(13) 0.2073(5) 0.1608(4) 0.051(4) Uani 1 1 d . . . H15 H 0.5511 0.2410 0.1537 0.062 Uiso 1 1 calc R . . C16 C 0.7242(13) 0.2012(5) 0.1827(4) 0.050(4) Uani 1 1 d . . . H16 H 0.7632 0.2307 0.1897 0.060 Uiso 1 1 calc R . . C17 C 0.7893(15) 0.1513(5) 0.1940(4) 0.060(4) Uani 1 1 d . . . H17 H 0.8711 0.1465 0.2102 0.071 Uiso 1 1 calc R . . C18 C 0.7342(14) 0.1070(5) 0.1816(4) 0.056(4) Uani 1 1 d . . . H18 H 0.7800 0.0730 0.1895 0.067 Uiso 1 1 calc R . . C19 C 0.5483(12) 0.0131(4) 0.1875(4) 0.040(3) Uani 1 1 d . . . C20 C 0.5236(14) 0.0302(5) 0.2315(5) 0.070(5) Uani 1 1 d . . . H20 H 0.5170 0.0663 0.2355 0.085 Uiso 1 1 calc R . . C21 C 0.5085(14) -0.0051(6) 0.2702(5) 0.071(4) Uani 1 1 d . . . H21 H 0.4965 0.0073 0.2993 0.085 Uiso 1 1 calc R . . C22 C 0.5116(13) -0.0578(5) 0.2644(5) 0.062(4) Uani 1 1 d . . . H22 H 0.4984 -0.0814 0.2897 0.074 Uiso 1 1 calc R . . C23 C 0.5338(14) -0.0759(5) 0.2223(5) 0.063(4) Uani 1 1 d . . . H23 H 0.5357 -0.1118 0.2183 0.075 Uiso 1 1 calc R . . C24 C 0.5540(12) -0.0398(4) 0.1843(4) 0.049(3) Uani 1 1 d . . . H24 H 0.5724 -0.0530 0.1557 0.059 Uiso 1 1 calc R . . C25 C 0.1903(12) 0.3453(4) 0.1142(4) 0.039(3) Uani 1 1 d . . . C26 C 0.2763(13) 0.3057(5) 0.0918(4) 0.047(3) Uani 1 1 d . . . H26 H 0.3624 0.3134 0.0791 0.057 Uiso 1 1 calc R . . C27 C 0.2412(14) 0.2555(4) 0.0874(4) 0.053(4) Uani 1 1 d . . . H27 H 0.3049 0.2302 0.0732 0.063 Uiso 1 1 calc R . . C28 C 0.1155(14) 0.2434(4) 0.1035(4) 0.047(3) Uani 1 1 d . . . H28 H 0.0896 0.2103 0.0997 0.057 Uiso 1 1 calc R . . C29 C 0.0255(14) 0.2815(5) 0.1259(4) 0.059(4) Uani 1 1 d . . . H29 H -0.0605 0.2729 0.1380 0.071 Uiso 1 1 calc R . . C30 C 0.0582(13) 0.3321(5) 0.1311(4) 0.051(4) Uani 1 1 d . . . H30 H -0.0063 0.3571 0.1455 0.061 Uiso 1 1 calc R . . C31 C 0.2486(14) 0.4270(4) 0.0595(4) 0.043(3) Uani 1 1 d . . . C32 C 0.3663(12) 0.4423(5) 0.0366(5) 0.051(4) Uani 1 1 d . . . H32 H 0.4467 0.4425 0.0526 0.061 Uiso 1 1 calc R . . C33 C 0.3686(13) 0.4575(4) -0.0102(4) 0.039(3) Uani 1 1 d . . . H33 H 0.4523 0.4655 -0.0246 0.047 Uiso 1 1 calc R . . C34 C 0.2540(14) 0.4609(4) -0.0355(5) 0.052(4) Uani 1 1 d . . . H34 H 0.2553 0.4733 -0.0662 0.062 Uiso 1 1 calc R . . C35 C 0.1320(14) 0.4446(5) -0.0127(5) 0.057(4) Uani 1 1 d . . . H35 H 0.0515 0.4448 -0.0289 0.068 Uiso 1 1 calc R . . C36 C 0.1318(13) 0.4282(4) 0.0336(4) 0.038(3) Uani 1 1 d . . . H36 H 0.0504 0.4175 0.0478 0.045 Uiso 1 1 calc R . . C37 C 0.1146(12) 0.4430(4) 0.1430(4) 0.036(3) Uani 1 1 d . . . C38 C 0.0280(12) 0.4877(4) 0.1250(4) 0.036(3) Uani 1 1 d . . . H38 H 0.0410 0.4988 0.0943 0.043 Uiso 1 1 calc R . . C39 C -0.0786(13) 0.5167(5) 0.1518(4) 0.046(4) Uani 1 1 d . . . H39 H -0.1342 0.5460 0.1382 0.056 Uiso 1 1 calc R . . C40 C -0.1017(12) 0.5028(5) 0.1969(5) 0.048(3) Uani 1 1 d U . . H40 H -0.1727 0.5218 0.2143 0.057 Uiso 1 1 calc R . . C41 C -0.0161(12) 0.4592(4) 0.2161(4) 0.041(3) Uani 1 1 d . . . H41 H -0.0270 0.4494 0.2472 0.050 Uiso 1 1 calc R . . C42 C 0.0833(13) 0.4307(4) 0.1901(4) 0.040(3) Uani 1 1 d . . . H42 H 0.1352 0.4008 0.2042 0.048 Uiso 1 1 calc R . . C43 C 0.3802(11) 0.4068(4) 0.1396(4) 0.037(3) Uani 1 1 d . . . C44 C 0.4327(12) 0.4546(5) 0.1401(4) 0.049(3) Uani 1 1 d . . . H44 H 0.3783 0.4855 0.1286 0.059 Uiso 1 1 calc R . . C45 C 0.5653(14) 0.4586(5) 0.1571(4) 0.058(4) Uani 1 1 d . . . H45 H 0.5969 0.4914 0.1566 0.069 Uiso 1 1 calc R . . C46 C 0.6482(14) 0.4123(5) 0.1747(5) 0.063(4) Uani 1 1 d . . . H46 H 0.7369 0.4135 0.1853 0.075 Uiso 1 1 calc R . . C47 C 0.5956(12) 0.3661(5) 0.1759(4) 0.053(4) Uani 1 1 d . . . H47 H 0.6476 0.3353 0.1885 0.063 Uiso 1 1 calc R . . C48 C 0.4639(13) 0.3631(5) 0.1585(4) 0.051(4) Uani 1 1 d . . . H48 H 0.4324 0.3302 0.1598 0.061 Uiso 1 1 calc R . . C49 C 0.6416(14) 0.3457(5) 0.6351(5) 0.054(4) Uani 1 1 d U . . C50 C 0.7030(16) 0.3061(6) 0.6061(5) 0.083(5) Uani 1 1 d U . . H50 H 0.7762 0.3136 0.5857 0.100 Uiso 1 1 calc R . . C51 C 0.6589(17) 0.2564(6) 0.6068(6) 0.091(5) Uani 1 1 d U . . H51 H 0.6967 0.2321 0.5858 0.109 Uiso 1 1 calc R . . C52 C 0.5564(17) 0.2442(7) 0.6399(6) 0.102(6) Uani 1 1 d U . . H52 H 0.5250 0.2113 0.6405 0.122 Uiso 1 1 calc R . . C53 C 0.4992(17) 0.2796(7) 0.6723(6) 0.100(5) Uani 1 1 d U . . H53 H 0.4359 0.2703 0.6957 0.119 Uiso 1 1 calc R . . C54 C 0.5431(14) 0.3304(5) 0.6676(6) 0.093(6) Uani 1 1 d . . . H54 H 0.5029 0.3553 0.6878 0.111 Uiso 1 1 calc R . . C55 C 0.7249(14) 0.4213(5) 0.5767(5) 0.058(4) Uani 1 1 d . . . C56 C 0.8582(16) 0.4336(5) 0.5581(6) 0.065(4) Uani 1 1 d . . . H56 H 0.9309 0.4341 0.5775 0.078 Uiso 1 1 calc R . . C57 C 0.8798(17) 0.4448(6) 0.5122(7) 0.079(5) Uani 1 1 d . . . H57 H 0.9700 0.4487 0.5006 0.094 Uiso 1 1 calc R . . C58 C 0.772(2) 0.4504(6) 0.4824(6) 0.098(6) Uani 1 1 d . . . H58 H 0.7878 0.4620 0.4519 0.118 Uiso 1 1 calc R . . C59 C 0.6424(19) 0.4390(6) 0.4973(7) 0.092(6) Uani 1 1 d U . . H59 H 0.5709 0.4405 0.4771 0.111 Uiso 1 1 calc R . . C60 C 0.6203(17) 0.4252(6) 0.5429(6) 0.095(6) Uani 1 1 d . . . H60 H 0.5312 0.4178 0.5529 0.114 Uiso 1 1 calc R . . C61 C 0.5693(12) 0.4477(5) 0.6545(5) 0.045(3) Uani 1 1 d . . . C62 C 0.4812(13) 0.4870(5) 0.6297(4) 0.048(3) Uani 1 1 d . . . H62 H 0.4919 0.4903 0.5979 0.058 Uiso 1 1 calc R . . C63 C 0.3801(14) 0.5204(5) 0.6513(6) 0.057(4) Uani 1 1 d . . . H63 H 0.3265 0.5471 0.6338 0.069 Uiso 1 1 calc R . . C64 C 0.3545(14) 0.5164(5) 0.6965(6) 0.065(4) Uani 1 1 d . . . H64 H 0.2816 0.5393 0.7096 0.078 Uiso 1 1 calc R . . C65 C 0.4367(14) 0.4780(6) 0.7246(5) 0.060(4) Uani 1 1 d . . . H65 H 0.4218 0.4748 0.7563 0.072 Uiso 1 1 calc R . . C66 C 0.5423(13) 0.4449(5) 0.7017(5) 0.051(4) Uani 1 1 d . . . H66 H 0.5986 0.4192 0.7193 0.061 Uiso 1 1 calc R . . C67 C 0.8354(13) 0.4069(5) 0.6590(4) 0.046(3) Uani 1 1 d . . . C68 C 0.8824(13) 0.4544(5) 0.6632(5) 0.056(4) Uani 1 1 d . . . H68 H 0.8288 0.4855 0.6518 0.067 Uiso 1 1 calc R . . C69 C 1.0072(14) 0.4580(5) 0.6837(4) 0.059(4) Uani 1 1 d . . . H69 H 1.0371 0.4911 0.6841 0.070 Uiso 1 1 calc R . . C70 C 1.0881(13) 0.4133(5) 0.7035(4) 0.056(4) Uani 1 1 d . . . H70 H 1.1702 0.4158 0.7179 0.067 Uiso 1 1 calc R . . C71 C 1.0411(13) 0.3645(5) 0.7010(4) 0.054(4) Uani 1 1 d . . . H71 H 1.0923 0.3336 0.7138 0.064 Uiso 1 1 calc R . . C72 C 0.9204(16) 0.3620(5) 0.6798(5) 0.067(4) Uani 1 1 d . . . H72 H 0.8917 0.3288 0.6788 0.080 Uiso 1 1 calc R . . C73 C 1.1302(13) 0.9078(5) 0.3981(4) 0.049(4) Uani 1 1 d U . . C74 C 1.2703(15) 0.9101(5) 0.3800(5) 0.064(4) Uani 1 1 d . . . H74 H 1.2829 0.9252 0.3504 0.077 Uiso 1 1 calc R . . C75 C 1.3873(13) 0.8910(5) 0.4042(6) 0.064(4) Uani 1 1 d . . . H75 H 1.4758 0.8935 0.3904 0.076 Uiso 1 1 calc R . . C76 C 1.3777(15) 0.8687(5) 0.4476(5) 0.068(4) Uani 1 1 d . . . H76 H 1.4578 0.8561 0.4637 0.081 Uiso 1 1 calc R . . C77 C 1.2481(15) 0.8655(5) 0.4666(5) 0.061(4) Uani 1 1 d . . . H77 H 1.2392 0.8503 0.4964 0.073 Uiso 1 1 calc R . . C78 C 1.1295(13) 0.8839(5) 0.4436(5) 0.057(4) Uani 1 1 d . . . H78 H 1.0430 0.8806 0.4585 0.068 Uiso 1 1 calc R . . C79 C 0.9296(14) 0.8724(5) 0.3539(4) 0.049(4) Uani 1 1 d . . . C80 C 0.9712(13) 0.8203(5) 0.3715(4) 0.055(4) Uani 1 1 d . . . H80 H 1.0378 0.8152 0.3937 0.066 Uiso 1 1 calc R . . C81 C 0.9220(14) 0.7757(5) 0.3586(5) 0.059(4) Uani 1 1 d . . . H81 H 0.9541 0.7422 0.3721 0.071 Uiso 1 1 calc R . . C82 C 0.8275(14) 0.7815(6) 0.3264(5) 0.070(5) Uani 1 1 d . . . H82 H 0.7909 0.7519 0.3182 0.084 Uiso 1 1 calc R . . C83 C 0.7830(15) 0.8313(6) 0.3050(5) 0.075(4) Uani 1 1 d . . . H83 H 0.7202 0.8347 0.2816 0.090 Uiso 1 1 calc R . . C84 C 0.8337(15) 0.8771(6) 0.3187(5) 0.070(4) Uani 1 1 d . . . H84 H 0.8034 0.9104 0.3044 0.084 Uiso 1 1 calc R . . C85 C 1.0005(15) 0.9672(5) 0.3269(4) 0.056(4) Uani 1 1 d . . . C86 C 1.0827(17) 0.9528(5) 0.2892(5) 0.088(5) Uani 1 1 d . . . H86 H 1.1292 0.9181 0.2899 0.106 Uiso 1 1 calc R . . C87 C 1.1034(18) 0.9857(6) 0.2494(5) 0.089(6) Uani 1 1 d . . . H87 H 1.1661 0.9739 0.2258 0.107 Uiso 1 1 calc R . . C88 C 1.0285(15) 1.0354(7) 0.2464(5) 0.069(4) Uani 1 1 d . . . H88 H 1.0339 1.0568 0.2193 0.082 Uiso 1 1 calc R . . C89 C 0.9469(14) 1.0541(6) 0.2821(5) 0.066(4) Uani 1 1 d . . . H89 H 0.8997 1.0887 0.2805 0.079 Uiso 1 1 calc R . . C90 C 0.9346(12) 1.0186(5) 0.3230(4) 0.054(4) Uani 1 1 d . . . H90 H 0.8793 1.0315 0.3479 0.065 Uiso 1 1 calc R . . C91 C 0.8618(13) 0.9545(5) 0.4066(4) 0.041(3) Uani 1 1 d . . . C92 C 0.8948(12) 0.9868(5) 0.4413(4) 0.046(4) Uani 1 1 d . . . H92 H 0.9893 0.9880 0.4455 0.056 Uiso 1 1 calc R . . C93 C 0.7986(13) 1.0157(4) 0.4685(4) 0.043(3) Uani 1 1 d . . . H93 H 0.8279 1.0358 0.4903 0.051 Uiso 1 1 calc R . . C94 C 0.6570(13) 1.0150(4) 0.4636(4) 0.042(3) Uani 1 1 d . . . H94 H 0.5899 1.0336 0.4826 0.051 Uiso 1 1 calc R . . C95 C 0.6175(13) 0.9864(5) 0.4304(4) 0.043(3) Uani 1 1 d . . . H95 H 0.5226 0.9864 0.4260 0.051 Uiso 1 1 calc R . . C96 C 0.7176(14) 0.9578(5) 0.4033(4) 0.048(3) Uani 1 1 d . . . H96 H 0.6859 0.9390 0.3810 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0359(3) 0.0287(3) 0.0587(4) 0.0053(2) 0.0012(3) -0.0006(3) N1A 0.046(4) 0.045(4) 0.038(4) -0.015(4) -0.001(4) -0.007(4) N2A 0.059(8) 0.045(7) 0.026(7) 0.021(6) 0.005(6) 0.010(6) N3A 0.049(7) 0.051(7) 0.030(7) 0.010(5) -0.009(5) 0.002(6) N4A 0.041(7) 0.051(8) 0.077(9) 0.006(7) 0.002(6) 0.012(6) N5A 0.032(6) 0.036(6) 0.065(8) -0.003(5) -0.003(5) -0.001(5) C1A 0.055(7) 0.037(6) 0.074(8) 0.013(6) 0.003(6) -0.011(6) C2A 0.075(10) 0.042(8) 0.048(10) 0.003(7) -0.007(8) -0.015(8) C3A 0.066(10) 0.073(11) 0.041(10) -0.005(8) 0.000(7) -0.022(8) C4A 0.060(9) 0.028(7) 0.075(12) -0.009(8) 0.004(8) 0.005(7) C5A 0.042(8) 0.043(8) 0.048(10) 0.001(7) 0.002(7) -0.007(7) C6A 0.050(9) 0.034(8) 0.053(10) 0.011(7) 0.016(7) 0.006(7) C7A 0.067(10) 0.031(8) 0.052(10) 0.016(7) -0.004(7) 0.002(7) C8A 0.064(10) 0.042(9) 0.080(13) -0.022(9) -0.019(9) 0.000(7) C9A 0.044(9) 0.042(9) 0.056(11) 0.014(7) -0.005(7) 0.004(7) C10A 0.019(7) 0.050(9) 0.066(11) -0.023(8) -0.006(7) -0.003(7) C11A 0.029(8) 0.032(8) 0.060(11) 0.027(8) -0.008(7) 0.000(6) C12A 0.040(9) 0.051(10) 0.107(15) 0.017(10) 0.011(9) 0.002(8) C13A 0.037(9) 0.038(9) 0.076(13) -0.002(8) 0.013(7) 0.007(7) C14A 0.041(9) 0.075(11) 0.050(11) 0.005(8) 0.003(7) 0.002(8) C15A 0.046(8) 0.037(7) 0.029(9) -0.013(7) 0.000(6) -0.002(6) C16A 0.075(11) 0.018(7) 0.078(12) 0.004(7) 0.004(8) 0.014(8) C17A 0.101(13) 0.058(10) 0.101(13) -0.007(9) -0.002(10) -0.009(9) C18A 0.043(9) 0.029(7) 0.069(11) -0.002(7) -0.009(7) -0.006(7) C19A 0.069(10) 0.032(7) 0.076(11) 0.020(7) -0.024(8) -0.019(7) C20A 0.042(9) 0.019(7) 0.072(12) -0.020(7) -0.002(7) -0.003(6) C21A 0.049(9) 0.061(10) 0.042(10) -0.010(8) 0.009(7) -0.018(8) C22A 0.031(6) 0.030(6) 0.038(7) 0.007(6) 0.001(5) 0.019(5) C23A 0.023(8) 0.066(11) 0.096(15) -0.001(10) -0.008(8) 0.013(8) C24A 0.040(9) 0.054(10) 0.053(11) -0.005(8) 0.013(7) -0.001(8) C25A 0.058(10) 0.044(8) 0.079(11) -0.002(7) 0.002(8) 0.003(7) C26A 0.051(9) 0.044(8) 0.051(10) 0.008(6) -0.001(7) -0.002(7) C27A 0.063(9) 0.029(7) 0.069(10) -0.004(6) 0.004(7) -0.006(7) C28A 0.024(8) 0.066(10) 0.103(14) -0.014(9) 0.010(8) 0.005(7) C29A 0.052(9) 0.058(9) 0.079(12) 0.023(8) 0.012(7) -0.001(8) C30A 0.029(8) 0.022(7) 0.047(10) -0.006(6) 0.002(6) 0.018(6) C31A 0.037(8) 0.012(6) 0.047(10) -0.003(6) 0.006(6) 0.006(6) C32A 0.054(9) 0.050(9) 0.028(9) -0.012(7) 0.003(7) 0.019(7) C33A 0.037(8) 0.026(7) 0.045(10) 0.010(7) 0.010(6) 0.002(6) C34A 0.046(9) 0.039(9) 0.056(11) -0.008(8) -0.002(7) -0.006(7) C35A 0.023(7) 0.047(8) 0.098(12) 0.011(7) 0.006(7) 0.006(6) C36A 0.025(8) 0.055(9) 0.094(12) -0.007(8) 0.007(7) 0.011(7) C37A 0.055(10) 0.070(10) 0.064(11) 0.012(8) -0.009(7) -0.008(8) C38A 0.054(9) 0.027(7) 0.091(11) -0.005(7) -0.013(7) -0.013(7) C39A 0.041(9) 0.058(9) 0.068(12) 0.003(8) 0.001(7) 0.002(7) U2 0.0387(4) 0.0293(3) 0.0627(4) 0.0034(2) 0.0065(3) -0.0019(3) N1B 0.030(6) 0.042(7) 0.059(9) -0.017(6) 0.002(6) 0.015(5) N2B 0.037(7) 0.019(6) 0.085(10) 0.019(6) -0.002(6) 0.002(5) N3B 0.061(8) 0.028(6) 0.101(11) -0.007(6) 0.002(7) -0.017(6) N4B 0.066(8) 0.026(6) 0.080(9) 0.013(6) 0.002(6) 0.001(6) N5B 0.073(5) 0.076(5) 0.114(6) 0.003(4) -0.012(5) -0.014(4) C1B 0.038(8) 0.047(9) 0.065(12) -0.002(8) 0.019(7) -0.004(7) C2B 0.037(9) 0.059(10) 0.091(14) -0.008(9) 0.001(8) -0.006(8) C3B 0.042(9) 0.046(9) 0.066(12) 0.008(8) 0.005(7) -0.006(7) C4B 0.055(9) 0.037(8) 0.076(12) 0.012(8) 0.006(8) -0.014(7) C5B 0.044(9) 0.032(8) 0.049(10) 0.026(7) 0.000(7) -0.012(7) C6B 0.026(8) 0.071(11) 0.060(12) -0.022(9) 0.006(7) -0.011(7) C7B 0.051(9) 0.044(8) 0.049(11) -0.011(8) 0.012(7) -0.014(7) C8B 0.043(9) 0.045(9) 0.076(12) 0.025(8) 0.007(7) -0.007(7) C9B 0.061(10) 0.034(8) 0.082(12) 0.025(8) -0.013(8) -0.008(7) C10B 0.044(9) 0.020(8) 0.123(16) 0.013(9) -0.005(9) 0.000(7) C11B 0.059(10) 0.057(10) 0.076(12) 0.018(9) -0.023(8) 0.001(8) C12B 0.048(9) 0.056(9) 0.046(9) -0.016(7) 0.015(7) 0.001(7) C13B 0.067(11) 0.054(10) 0.098(14) 0.008(9) -0.025(9) -0.022(8) C14B 0.053(9) 0.023(7) 0.087(12) 0.010(8) -0.015(8) 0.003(7) C15B 0.020(7) 0.046(9) 0.068(11) -0.004(7) 0.010(6) -0.005(7) C16B 0.026(8) 0.050(9) 0.059(10) -0.007(7) -0.013(6) -0.008(7) C17B 0.049(9) 0.044(8) 0.059(10) 0.023(6) -0.013(7) -0.014(7) C18B 0.046(7) 0.066(7) 0.080(9) 0.002(7) -0.014(7) -0.008(6) C19B 0.095(8) 0.090(8) 0.069(8) -0.004(7) 0.004(7) -0.026(7) C20B 0.041(9) 0.057(10) 0.039(10) 0.005(8) 0.007(7) -0.001(7) C21B 0.036(9) 0.048(10) 0.088(14) 0.011(9) -0.007(8) 0.003(7) C22B 0.039(9) 0.062(11) 0.062(12) -0.023(9) 0.001(8) 0.007(8) C23B 0.030(9) 0.050(10) 0.094(15) 0.035(9) 0.018(8) -0.012(8) C24B 0.027(8) 0.030(8) 0.108(15) 0.004(9) 0.016(8) 0.004(7) C25B 0.062(8) 0.105(9) 0.077(9) -0.018(7) -0.006(7) -0.004(7) C26B 0.069(8) 0.079(8) 0.100(9) 0.028(7) -0.004(7) -0.004(7) C27B 0.081(8) 0.088(8) 0.110(9) -0.030(7) 0.008(7) -0.015(7) C28B 0.063(11) 0.104(14) 0.101(15) 0.000(11) 0.013(9) 0.005(10) C29B 0.058(7) 0.067(8) 0.105(9) -0.004(7) -0.005(7) -0.020(7) C30B 0.033(8) 0.038(8) 0.064(11) 0.006(7) 0.012(7) 0.006(6) C31B 0.047(8) 0.011(6) 0.028(8) -0.008(5) -0.001(6) 0.002(6) C32B 0.018(7) 0.024(7) 0.057(10) -0.007(6) 0.004(6) -0.007(6) C33B 0.036(8) 0.029(7) 0.044(10) -0.001(7) 0.009(7) 0.006(6) C34B 0.007(7) 0.045(9) 0.084(13) 0.000(8) 0.006(6) 0.007(6) C35B 0.036(8) 0.024(7) 0.078(10) 0.003(6) 0.004(6) 0.012(6) C36B 0.072(10) 0.042(8) 0.048(10) 0.002(6) -0.003(7) -0.019(7) C37B 0.016(7) 0.055(9) 0.119(13) 0.014(8) 0.010(7) -0.009(7) C38B 0.070(11) 0.064(10) 0.097(13) -0.052(9) 0.002(9) -0.008(9) C39B 0.072(10) 0.052(9) 0.043(10) -0.006(7) 0.001(7) 0.005(8) B1 0.049(11) 0.048(9) 0.038(10) -0.012(7) 0.004(8) -0.013(8) B2 0.049(11) 0.034(9) 0.067(13) -0.006(8) 0.000(9) -0.007(8) B3 0.093(14) 0.043(9) 0.032(11) -0.013(7) -0.016(9) -0.013(10) B4 0.056(11) 0.034(9) 0.074(13) -0.012(8) -0.010(9) 0.002(8) C1 0.052(10) 0.038(8) 0.046(10) 0.000(7) 0.007(7) -0.004(7) C2 0.028(8) 0.068(10) 0.068(11) -0.011(8) 0.004(7) -0.007(8) C3 0.055(10) 0.043(8) 0.058(11) -0.020(7) 0.012(8) -0.008(8) C4 0.046(9) 0.044(8) 0.052(11) 0.005(7) 0.031(7) 0.010(7) C5 0.049(9) 0.047(8) 0.049(11) 0.005(7) -0.006(8) -0.015(7) C6 0.039(9) 0.049(8) 0.045(10) -0.010(7) 0.012(7) -0.014(7) C7 0.047(9) 0.047(8) 0.060(10) -0.023(7) 0.020(7) 0.001(7) C8 0.036(9) 0.052(9) 0.067(12) 0.004(8) 0.000(8) 0.003(7) C9 0.060(10) 0.047(8) 0.045(9) -0.007(6) -0.008(8) 0.001(8) C10 0.052(7) 0.051(7) 0.058(8) -0.024(6) -0.002(6) -0.004(6) C11 0.043(9) 0.052(9) 0.073(11) -0.020(8) -0.014(8) -0.004(7) C12 0.035(8) 0.061(9) 0.040(9) -0.019(6) 0.011(7) -0.006(7) C13 0.025(8) 0.044(8) 0.058(10) -0.002(7) -0.004(6) 0.003(7) C14 0.043(9) 0.037(8) 0.061(10) -0.008(7) 0.006(7) -0.009(7) C15 0.035(9) 0.030(7) 0.085(11) -0.016(7) 0.016(7) 0.007(7) C16 0.046(9) 0.049(9) 0.057(10) -0.007(7) 0.009(7) -0.018(8) C17 0.082(11) 0.050(9) 0.049(10) -0.005(7) 0.006(7) -0.020(9) C18 0.076(11) 0.045(8) 0.048(10) 0.021(7) 0.003(8) -0.028(8) C19 0.043(8) 0.031(7) 0.051(10) -0.025(6) 0.012(6) -0.018(6) C20 0.090(12) 0.028(8) 0.096(14) -0.002(8) 0.012(9) -0.026(8) C21 0.085(12) 0.059(10) 0.070(12) -0.001(8) 0.002(8) -0.016(9) C22 0.069(11) 0.047(9) 0.065(12) 0.001(8) 0.011(8) 0.000(8) C23 0.092(12) 0.041(8) 0.057(11) -0.008(8) -0.005(9) -0.012(8) C24 0.072(10) 0.032(8) 0.047(10) -0.012(6) -0.003(7) -0.010(7) C25 0.038(8) 0.042(8) 0.041(9) -0.003(6) -0.021(6) -0.008(7) C26 0.048(9) 0.037(8) 0.054(10) 0.014(7) -0.006(7) -0.005(7) C27 0.053(10) 0.027(7) 0.071(10) 0.009(6) -0.003(7) 0.012(7) C28 0.064(10) 0.024(7) 0.054(10) -0.017(6) -0.004(7) -0.001(7) C29 0.051(9) 0.064(10) 0.072(11) 0.004(8) -0.016(8) -0.033(9) C30 0.050(9) 0.047(8) 0.060(10) 0.007(7) -0.019(7) -0.018(7) C31 0.057(9) 0.029(7) 0.039(9) 0.007(6) -0.022(7) 0.006(7) C32 0.030(8) 0.049(9) 0.073(12) -0.008(7) -0.004(7) 0.004(7) C33 0.051(9) 0.025(7) 0.044(10) -0.016(6) 0.016(7) -0.016(6) C34 0.045(9) 0.045(8) 0.068(11) -0.019(7) -0.011(8) -0.001(7) C35 0.057(10) 0.065(9) 0.050(11) -0.014(8) -0.031(8) 0.004(8) C36 0.052(9) 0.027(7) 0.030(9) -0.001(6) -0.002(7) 0.007(6) C37 0.033(8) 0.038(7) 0.040(9) 0.007(6) -0.008(6) -0.014(6) C38 0.047(8) 0.031(7) 0.027(8) -0.007(6) -0.001(6) 0.007(6) C39 0.052(9) 0.049(8) 0.041(10) 0.015(7) -0.012(7) -0.020(7) C40 0.041(7) 0.046(7) 0.057(8) -0.009(6) 0.001(6) -0.010(6) C41 0.046(9) 0.026(7) 0.050(10) 0.005(6) 0.000(7) -0.004(7) C42 0.057(9) 0.027(7) 0.037(9) -0.005(6) -0.004(7) -0.010(7) C43 0.028(7) 0.033(7) 0.051(9) 0.002(6) -0.007(6) -0.002(6) C44 0.036(9) 0.050(9) 0.057(10) -0.005(7) -0.006(7) 0.006(7) C45 0.053(10) 0.051(9) 0.074(11) -0.008(8) -0.014(8) -0.022(8) C46 0.041(9) 0.064(10) 0.084(12) -0.003(8) -0.013(8) -0.009(8) C47 0.028(8) 0.041(8) 0.086(11) 0.016(7) -0.017(7) -0.001(7) C48 0.048(9) 0.031(7) 0.071(11) -0.003(7) 0.003(7) 0.002(7) C49 0.053(7) 0.044(6) 0.062(8) -0.012(6) -0.018(6) 0.014(6) C50 0.088(8) 0.083(8) 0.083(9) -0.024(7) -0.022(7) -0.009(7) C51 0.101(9) 0.075(8) 0.094(9) -0.016(7) -0.011(7) -0.001(7) C52 0.093(9) 0.102(9) 0.120(10) -0.031(8) -0.017(8) -0.029(8) C53 0.097(9) 0.096(9) 0.109(9) -0.024(8) 0.000(7) -0.020(8) C54 0.052(11) 0.045(10) 0.182(18) -0.014(10) 0.013(10) -0.017(8) C55 0.043(9) 0.055(9) 0.075(12) -0.034(8) -0.006(8) 0.016(8) C56 0.076(12) 0.045(9) 0.079(13) -0.024(8) 0.013(9) -0.023(8) C57 0.057(12) 0.076(12) 0.104(18) -0.039(11) 0.028(11) -0.007(10) C58 0.116(17) 0.096(14) 0.065(14) -0.004(10) 0.041(12) 0.025(13) C59 0.086(9) 0.112(9) 0.072(9) -0.010(8) -0.011(8) 0.013(8) C60 0.078(13) 0.129(15) 0.077(15) -0.032(11) -0.042(11) 0.012(11) C61 0.035(8) 0.045(8) 0.059(11) -0.018(7) -0.002(7) -0.012(7) C62 0.053(9) 0.046(8) 0.039(9) -0.006(7) -0.014(7) 0.019(7) C63 0.060(11) 0.042(9) 0.067(12) 0.014(8) -0.018(9) -0.004(8) C64 0.055(10) 0.047(9) 0.094(14) 0.000(9) -0.020(10) -0.007(8) C65 0.048(10) 0.089(12) 0.045(10) -0.006(9) 0.013(8) -0.023(9) C66 0.049(10) 0.044(8) 0.061(12) 0.005(7) -0.003(8) -0.013(7) C67 0.049(9) 0.045(8) 0.046(9) -0.013(7) -0.022(7) 0.000(7) C68 0.039(9) 0.035(8) 0.094(12) -0.025(7) -0.026(8) 0.018(7) C69 0.057(10) 0.035(8) 0.082(12) -0.001(7) -0.005(8) -0.002(7) C70 0.053(9) 0.066(10) 0.048(9) -0.004(7) -0.013(7) -0.006(8) C71 0.051(9) 0.033(8) 0.075(11) -0.013(7) -0.029(8) 0.014(7) C72 0.101(13) 0.039(9) 0.067(11) -0.013(7) -0.013(9) -0.019(9) C73 0.049(7) 0.044(6) 0.055(7) -0.001(6) 0.007(6) -0.010(6) C74 0.058(11) 0.045(9) 0.090(12) -0.013(8) 0.024(9) -0.017(8) C75 0.020(8) 0.040(9) 0.126(16) -0.005(9) 0.007(9) 0.006(7) C76 0.056(11) 0.058(10) 0.089(13) -0.006(9) -0.001(9) -0.010(8) C77 0.051(10) 0.062(10) 0.074(11) -0.011(8) 0.003(9) -0.023(9) C78 0.019(8) 0.067(10) 0.084(12) -0.020(8) 0.002(7) -0.002(7) C79 0.064(10) 0.050(9) 0.031(9) -0.006(7) 0.023(7) -0.013(8) C80 0.041(9) 0.054(9) 0.068(11) 0.000(8) 0.016(7) -0.008(8) C81 0.047(10) 0.043(9) 0.090(13) -0.020(8) -0.006(8) -0.003(8) C82 0.039(10) 0.064(11) 0.111(15) -0.016(9) 0.001(9) -0.022(9) C83 0.089(12) 0.068(11) 0.069(12) -0.004(9) -0.022(9) -0.005(10) C84 0.103(13) 0.069(10) 0.045(11) 0.003(8) -0.012(9) -0.036(10) C85 0.073(11) 0.059(10) 0.036(10) -0.003(7) 0.004(7) -0.017(9) C86 0.144(16) 0.045(9) 0.074(13) -0.021(9) 0.034(11) -0.017(10) C87 0.137(17) 0.073(12) 0.054(12) 0.004(9) 0.033(10) -0.026(12) C88 0.051(11) 0.086(13) 0.059(12) 0.013(9) 0.003(8) 0.009(9) C89 0.048(10) 0.062(10) 0.089(14) 0.011(9) -0.021(9) -0.012(8) C90 0.043(9) 0.060(10) 0.056(10) 0.006(8) -0.009(7) 0.000(8) C91 0.049(9) 0.039(8) 0.034(9) 0.009(6) -0.006(7) -0.009(7) C92 0.027(8) 0.050(8) 0.055(10) 0.009(7) 0.015(7) 0.006(7) C93 0.037(9) 0.041(8) 0.044(10) 0.010(6) 0.001(7) 0.006(7) C94 0.059(10) 0.024(7) 0.032(9) -0.001(6) 0.018(7) 0.025(7) C95 0.036(8) 0.049(8) 0.041(10) 0.001(7) -0.006(7) 0.001(7) C96 0.045(9) 0.043(8) 0.051(10) 0.003(7) 0.005(7) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N3A 2.528(9) . ? U1 N2A 2.547(10) . ? U1 N1A 2.571(9) . ? U1 N4A 2.598(12) . ? U1 N5A 2.641(10) . ? U1 C32A 2.843(12) . ? U1 C34A 2.845(12) . ? U1 C22A 2.847(11) . ? U1 C31A 2.853(11) . ? U1 C23A 2.860(14) . ? U1 C33A 2.863(11) . ? U1 C24A 2.864(12) . ? U1 C30A 2.874(11) . ? U1 C20A 2.877(11) . ? U1 C21A 2.891(13) . ? N1A C1A 1.285(13) . ? N1A C5A 1.395(13) . ? N2A C10A 1.349(14) . ? N2A C6A 1.358(14) . ? N3A C15A 1.340(12) . ? N3A C11A 1.390(13) . ? N4A C16A 1.135(14) . ? N5A C18A 1.140(12) . ? C1A C2A 1.375(15) . ? C1A H1A 0.9300 . ? C2A C3A 1.337(15) . ? C2A H2A 0.9300 . ? C3A C4A 1.405(15) . ? C3A H3A 0.9300 . ? C4A C5A 1.373(15) . ? C4A H4A 0.9300 . ? C5A C6A 1.486(15) . ? C6A C7A 1.354(15) . ? C7A C8A 1.370(16) . ? C7A H7A 0.9300 . ? C8A C9A 1.340(15) . ? C8A H8A 0.9300 . ? C9A C10A 1.427(15) . ? C9A H9A 0.9300 . ? C10A C11A 1.463(16) . ? C11A C12A 1.419(16) . ? C12A C13A 1.392(17) . ? C12A H12A 0.9300 . ? C13A C14A 1.402(15) . ? C13A H13A 0.9300 . ? C14A C15A 1.386(14) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? C16A C17A 1.450(17) . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A C19A 1.454(14) . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A C21A 1.419(15) . ? C20A C24A 1.444(15) . ? C20A C25A 1.549(15) . ? C21A C22A 1.391(15) . ? C21A C26A 1.472(15) . ? C22A C23A 1.455(17) . ? C22A C27A 1.524(14) . ? C23A C24A 1.408(18) . ? C23A C28A 1.498(18) . ? C24A C29A 1.494(15) . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A C34A 1.353(15) . ? C30A C31A 1.391(14) . ? C30A C35A 1.527(14) . ? C31A C32A 1.438(14) . ? C31A C36A 1.514(15) . ? C32A C33A 1.392(15) . ? C32A C37A 1.529(15) . ? C33A C34A 1.420(15) . ? C33A C38A 1.543(14) . ? C34A C39A 1.497(15) . ? C35A H35A 0.9600 . ? C35A H35B 0.9600 . ? C35A H35C 0.9600 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37A H37A 0.9600 . ? C37A H37B 0.9600 . ? C37A H37C 0.9600 . ? C38A H38A 0.9600 . ? C38A H38B 0.9600 . ? C38A H38C 0.9600 . ? C39A H39A 0.9600 . ? C39A H39B 0.9600 . ? C39A H39C 0.9600 . ? U2 N5B 2.530(8) . ? U2 N1B 2.572(10) . ? U2 N2B 2.578(10) . ? U2 N4B 2.578(10) . ? U2 N3B 2.600(11) . ? U2 C21B 2.827(13) . ? U2 C24B 2.840(12) . ? U2 C22B 2.850(13) . ? U2 C32B 2.854(10) . ? U2 C34B 2.855(12) . ? U2 C31B 2.855(11) . ? U2 C23B 2.856(12) . ? U2 C30B 2.863(12) . ? U2 C20B 2.881(13) . ? U2 C33B 2.882(12) . ? N1B C1B 1.314(14) . ? N1B C5B 1.346(13) . ? N2B C10B 1.338(16) . ? N2B C6B 1.358(15) . ? N3B C15B 1.324(13) . ? N3B C11B 1.396(15) . ? N4B C16B 1.129(13) . ? N5B C18B 1.155(8) . ? C1B C2B 1.434(16) . ? C1B H1B 0.9300 . ? C2B C3B 1.362(16) . ? C2B H2B 0.9300 . ? C3B C4B 1.378(16) . ? C3B H3B 0.9300 . ? C4B C5B 1.404(15) . ? C4B H4B 0.9300 . ? C5B C6B 1.450(16) . ? C6B C7B 1.380(16) . ? C7B C8B 1.319(15) . ? C7B H7B 0.9300 . ? C8B C9B 1.353(15) . ? C8B H8B 0.9300 . ? C9B C10B 1.395(17) . ? C9B H9B 0.9300 . ? C10B C11B 1.466(17) . ? C11B C12B 1.445(17) . ? C12B C13B 1.332(15) . ? C12B H12B 0.9300 . ? C13B C14B 1.408(17) . ? C13B H13B 0.9300 . ? C14B C15B 1.384(15) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? C16B C17B 1.455(15) . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B C19B 1.502(9) . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B C24B 1.403(17) . ? C20B C25B 1.443(16) . ? C20B C21B 1.452(17) . ? C21B C22B 1.403(17) . ? C21B C26B 1.558(16) . ? C22B C23B 1.405(17) . ? C22B C27B 1.520(17) . ? C23B C24B 1.366(18) . ? C23B C28B 1.531(18) . ? C24B C29B 1.509(16) . ? C25B H25D 0.9600 . ? C25B H25E 0.9600 . ? C25B H25F 0.9600 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B C34B 1.418(16) . ? C30B C31B 1.447(15) . ? C30B C35B 1.483(14) . ? C31B C32B 1.447(13) . ? C31B C36B 1.496(14) . ? C32B C33B 1.400(15) . ? C32B C37B 1.537(14) . ? C33B C34B 1.453(15) . ? C33B C38B 1.468(15) . ? C34B C39B 1.543(16) . ? C35B H35D 0.9600 . ? C35B H35E 0.9600 . ? C35B H35F 0.9600 . ? C36B H36D 0.9601 . ? C36B H36E 0.9601 . ? C36B H36F 0.9601 . ? C37B H37D 0.9600 . ? C37B H37E 0.9600 . ? C37B H37F 0.9600 . ? C38B H38D 0.9600 . ? C38B H38E 0.9600 . ? C38B H38F 0.9600 . ? C39B H39D 0.9600 . ? C39B H39E 0.9600 . ? C39B H39F 0.9600 . ? B1 C1 1.622(18) . ? B1 C7 1.672(18) . ? B1 C19 1.677(17) . ? B1 C13 1.685(17) . ? B2 C37 1.591(18) . ? B2 C43 1.652(17) . ? B2 C31 1.659(18) . ? B2 C25 1.671(16) . ? B3 C67 1.605(18) . ? B3 C55 1.652(19) . ? B3 C61 1.662(19) . ? B3 C49 1.667(18) . ? B4 C79 1.636(18) . ? B4 C85 1.638(18) . ? B4 C73 1.639(19) . ? B4 C91 1.657(19) . ? C1 C2 1.370(15) . ? C1 C6 1.427(15) . ? C2 C3 1.357(16) . ? C2 H2 0.9300 . ? C3 C4 1.390(15) . ? C3 H3 0.9300 . ? C4 C5 1.354(15) . ? C4 H4 0.9300 . ? C5 C6 1.359(15) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.388(16) . ? C7 C12 1.426(14) . ? C8 C9 1.367(15) . ? C8 H8 0.9300 . ? C9 C10 1.401(15) . ? C9 H9 0.9300 . ? C10 C11 1.391(16) . ? C10 H10 0.9300 . ? C11 C12 1.353(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.341(14) . ? C13 C18 1.376(15) . ? C14 C15 1.391(14) . ? C14 H14 0.9300 . ? C15 C16 1.380(15) . ? C15 H15 0.9300 . ? C16 C17 1.358(15) . ? C16 H16 0.9300 . ? C17 C18 1.396(15) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.351(14) . ? C19 C20 1.393(15) . ? C20 C21 1.404(17) . ? C20 H20 0.9300 . ? C21 C22 1.362(16) . ? C21 H21 0.9300 . ? C22 C23 1.349(16) . ? C22 H22 0.9300 . ? C23 C24 1.409(15) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.390(15) . ? C25 C30 1.414(14) . ? C26 C27 1.389(14) . ? C26 H26 0.9300 . ? C27 C28 1.342(15) . ? C27 H27 0.9300 . ? C28 C29 1.384(16) . ? C28 H28 0.9300 . ? C29 C30 1.395(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.373(15) . ? C31 C36 1.388(14) . ? C32 C33 1.395(15) . ? C32 H32 0.9300 . ? C33 C34 1.353(15) . ? C33 H33 0.9300 . ? C34 C35 1.417(16) . ? C34 H34 0.9300 . ? C35 C36 1.390(15) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.394(14) . ? C37 C42 1.418(14) . ? C38 C39 1.413(15) . ? C38 H38 0.9300 . ? C39 C40 1.356(14) . ? C39 H39 0.9300 . ? C40 C41 1.385(15) . ? C40 H40 0.9300 . ? C41 C42 1.351(14) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.374(14) . ? C43 C44 1.384(14) . ? C44 C45 1.418(15) . ? C44 H44 0.9300 . ? C45 C46 1.404(16) . ? C45 H45 0.9300 . ? C46 C47 1.343(15) . ? C46 H46 0.9300 . ? C47 C48 1.408(14) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.380(17) . ? C49 C50 1.412(17) . ? C50 C51 1.392(17) . ? C50 H50 0.9300 . ? C51 C52 1.395(19) . ? C51 H51 0.9300 . ? C52 C53 1.398(19) . ? C52 H52 0.9300 . ? C53 C54 1.415(17) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.433(16) . ? C55 C60 1.441(17) . ? C56 C57 1.364(19) . ? C56 H56 0.9300 . ? C57 C58 1.38(2) . ? C57 H57 0.9300 . ? C58 C59 1.36(2) . ? C58 H58 0.9300 . ? C59 C60 1.368(19) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C66 1.393(15) . ? C61 C62 1.400(15) . ? C62 C63 1.359(16) . ? C62 H62 0.9300 . ? C63 C64 1.334(17) . ? C63 H63 0.9300 . ? C64 C65 1.409(17) . ? C64 H64 0.9300 . ? C65 C66 1.400(16) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.370(14) . ? C67 C72 1.422(16) . ? C68 C69 1.391(15) . ? C68 H68 0.9300 . ? C69 C70 1.391(15) . ? C69 H69 0.9300 . ? C70 C71 1.392(15) . ? C70 H70 0.9300 . ? C71 C72 1.361(16) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 C78 1.421(16) . ? C73 C74 1.429(16) . ? C74 C75 1.373(16) . ? C74 H74 0.9300 . ? C75 C76 1.357(17) . ? C75 H75 0.9300 . ? C76 C77 1.348(16) . ? C76 H76 0.9300 . ? C77 C78 1.365(16) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? C79 C80 1.395(15) . ? C79 C84 1.411(16) . ? C80 C81 1.382(15) . ? C80 H80 0.9300 . ? C81 C82 1.334(16) . ? C81 H81 0.9300 . ? C82 C83 1.392(17) . ? C82 H82 0.9300 . ? C83 C84 1.425(17) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 C86 1.366(17) . ? C85 C90 1.369(16) . ? C86 C87 1.402(17) . ? C86 H86 0.9300 . ? C87 C88 1.364(18) . ? C87 H87 0.9300 . ? C88 C89 1.346(17) . ? C88 H88 0.9300 . ? C89 C90 1.455(16) . ? C89 H89 0.9300 . ? C90 H90 0.9300 . ? C91 C96 1.387(15) . ? C91 C92 1.436(15) . ? C92 C93 1.360(15) . ? C92 H92 0.9300 . ? C93 C94 1.382(15) . ? C93 H93 0.9300 . ? C94 C95 1.365(15) . ? C94 H94 0.9300 . ? C95 C96 1.375(15) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A U1 N2A 65.5(3) . . ? N3A U1 N1A 130.2(3) . . ? N2A U1 N1A 64.7(3) . . ? N3A U1 N4A 81.9(3) . . ? N2A U1 N4A 147.5(3) . . ? N1A U1 N4A 147.9(3) . . ? N3A U1 N5A 149.9(3) . . ? N2A U1 N5A 144.6(3) . . ? N1A U1 N5A 79.9(3) . . ? N4A U1 N5A 67.9(3) . . ? C1A N1A C5A 118.6(11) . . ? C1A N1A U1 122.8(9) . . ? C5A N1A U1 118.6(8) . . ? C10A N2A C6A 117.7(11) . . ? C10A N2A U1 119.6(9) . . ? C6A N2A U1 122.6(8) . . ? C15A N3A C11A 118.4(10) . . ? C15A N3A U1 122.7(8) . . ? C11A N3A U1 118.9(8) . . ? C16A N4A U1 168.3(11) . . ? C18A N5A U1 166.8(9) . . ? N1A C1A C2A 124.7(12) . . ? N1A C1A H1A 117.7 . . ? C2A C1A H1A 117.7 . . ? C3A C2A C1A 119.0(12) . . ? C3A C2A H2A 120.5 . . ? C1A C2A H2A 120.5 . . ? C2A C3A C4A 118.4(13) . . ? C2A C3A H3A 120.8 . . ? C4A C3A H3A 120.8 . . ? C5A C4A C3A 120.4(12) . . ? C5A C4A H4A 119.8 . . ? C3A C4A H4A 119.8 . . ? C4A C5A N1A 118.8(11) . . ? C4A C5A C6A 122.4(12) . . ? N1A C5A C6A 118.7(12) . . ? C7A C6A N2A 121.8(12) . . ? C7A C6A C5A 122.8(13) . . ? N2A C6A C5A 115.4(11) . . ? C6A C7A C8A 120.8(13) . . ? C6A C7A H7A 119.6 . . ? C8A C7A H7A 119.6 . . ? C9A C8A C7A 119.7(13) . . ? C9A C8A H8A 120.2 . . ? C7A C8A H8A 120.2 . . ? C8A C9A C10A 118.4(13) . . ? C8A C9A H9A 120.8 . . ? C10A C9A H9A 120.8 . . ? N2A C10A C9A 121.5(13) . . ? N2A C10A C11A 118.0(12) . . ? C9A C10A C11A 120.4(13) . . ? N3A C11A C12A 116.9(13) . . ? N3A C11A C10A 117.9(11) . . ? C12A C11A C10A 125.2(14) . . ? C13A C12A C11A 122.6(15) . . ? C13A C12A H12A 118.7 . . ? C11A C12A H12A 118.7 . . ? C12A C13A C14A 119.6(14) . . ? C12A C13A H13A 120.2 . . ? C14A C13A H13A 120.2 . . ? C15A C14A C13A 114.8(13) . . ? C15A C14A H14A 122.6 . . ? C13A C14A H14A 122.6 . . ? N3A C15A C14A 127.6(12) . . ? N3A C15A H15A 116.2 . . ? C14A C15A H15A 116.2 . . ? N4A C16A C17A 175.4(15) . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? N5A C18A C19A 178.6(15) . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C24A 110.6(11) . . ? C21A C20A C25A 124.4(13) . . ? C24A C20A C25A 123.5(11) . . ? C22A C21A C20A 103.7(11) . . ? C22A C21A C26A 126.7(13) . . ? C20A C21A C26A 127.8(13) . . ? C21A C22A C23A 113.5(13) . . ? C21A C22A C27A 123.7(11) . . ? C23A C22A C27A 121.9(13) . . ? C24A C23A C22A 104.1(14) . . ? C24A C23A C28A 126.4(14) . . ? C22A C23A C28A 127.5(14) . . ? C23A C24A C20A 108.0(12) . . ? C23A C24A C29A 124.7(14) . . ? C20A C24A C29A 124.7(13) . . ? C20A C25A H25A 109.5 . . ? C20A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C20A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C21A C26A H26A 109.5 . . ? C21A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C21A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C22A C27A H27A 109.5 . . ? C22A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C22A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C23A C28A H28A 109.5 . . ? C23A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C23A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C24A C29A H29A 109.5 . . ? C24A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C24A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C34A C30A C31A 109.2(11) . . ? C34A C30A C35A 126.5(12) . . ? C31A C30A C35A 122.8(10) . . ? C30A C31A C32A 107.2(10) . . ? C30A C31A C36A 128.0(10) . . ? C32A C31A C36A 122.7(11) . . ? C33A C32A C31A 107.1(11) . . ? C33A C32A C37A 125.1(12) . . ? C31A C32A C37A 126.0(12) . . ? C32A C33A C34A 107.3(11) . . ? C32A C33A C38A 126.4(11) . . ? C34A C33A C38A 124.9(12) . . ? C30A C34A C33A 109.1(12) . . ? C30A C34A C39A 127.0(12) . . ? C33A C34A C39A 122.6(11) . . ? C30A C35A H35A 109.5 . . ? C30A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C30A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C31A C36A H36A 109.5 . . ? C31A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C31A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C32A C37A H37A 109.5 . . ? C32A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C32A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C33A C38A H38A 109.5 . . ? C33A C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C33A C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? C34A C39A H39A 109.5 . . ? C34A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C34A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? N5B U2 N1B 80.4(4) . . ? N5B U2 N2B 143.7(4) . . ? N1B U2 N2B 63.4(4) . . ? N5B U2 N4B 71.9(4) . . ? N1B U2 N4B 152.3(4) . . ? N2B U2 N4B 144.3(3) . . ? N5B U2 N3B 152.3(4) . . ? N1B U2 N3B 127.3(4) . . ? N2B U2 N3B 63.9(3) . . ? N4B U2 N3B 80.4(3) . . ? C1B N1B C5B 118.8(13) . . ? C1B N1B U2 121.0(9) . . ? C5B N1B U2 120.2(9) . . ? C10B N2B C6B 118.6(12) . . ? C10B N2B U2 120.1(9) . . ? C6B N2B U2 120.9(10) . . ? C15B N3B C11B 117.0(12) . . ? C15B N3B U2 122.9(9) . . ? C11B N3B U2 120.1(9) . . ? C16B N4B U2 173.2(10) . . ? C18B N5B U2 174.2(12) . . ? N1B C1B C2B 124.7(13) . . ? N1B C1B H1B 117.6 . . ? C2B C1B H1B 117.6 . . ? C3B C2B C1B 114.7(14) . . ? C3B C2B H2B 122.7 . . ? C1B C2B H2B 122.7 . . ? C2B C3B C4B 122.0(14) . . ? C2B C3B H3B 119.0 . . ? C4B C3B H3B 119.0 . . ? C3B C4B C5B 118.9(13) . . ? C3B C4B H4B 120.5 . . ? C5B C4B H4B 120.5 . . ? N1B C5B C4B 120.7(14) . . ? N1B C5B C6B 119.0(12) . . ? C4B C5B C6B 120.3(13) . . ? N2B C6B C7B 122.0(13) . . ? N2B C6B C5B 116.2(13) . . ? C7B C6B C5B 121.7(14) . . ? C8B C7B C6B 119.9(14) . . ? C8B C7B H7B 120.1 . . ? C6B C7B H7B 120.1 . . ? C7B C8B C9B 118.7(14) . . ? C7B C8B H8B 120.7 . . ? C9B C8B H8B 120.7 . . ? C8B C9B C10B 122.3(14) . . ? C8B C9B H9B 118.9 . . ? C10B C9B H9B 118.8 . . ? N2B C10B C9B 118.5(13) . . ? N2B C10B C11B 120.4(15) . . ? C9B C10B C11B 121.0(15) . . ? N3B C11B C12B 118.8(12) . . ? N3B C11B C10B 115.2(14) . . ? C12B C11B C10B 125.9(14) . . ? C13B C12B C11B 121.4(13) . . ? C13B C12B H12B 119.3 . . ? C11B C12B H12B 119.3 . . ? C12B C13B C14B 119.0(14) . . ? C12B C13B H13B 120.5 . . ? C14B C13B H13B 120.5 . . ? C15B C14B C13B 117.6(13) . . ? C15B C14B H14B 121.2 . . ? C13B C14B H14B 121.2 . . ? N3B C15B C14B 125.8(13) . . ? N3B C15B H15B 117.1 . . ? C14B C15B H15B 117.1 . . ? N4B C16B C17B 176.5(13) . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? N5B C18B C19B 176.3(15) . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C24B C20B C25B 129.2(14) . . ? C24B C20B C21B 101.7(12) . . ? C25B C20B C21B 127.2(13) . . ? C22B C21B C20B 112.4(12) . . ? C22B C21B C26B 123.6(14) . . ? C20B C21B C26B 122.2(14) . . ? C21B C22B C23B 103.9(13) . . ? C21B C22B C27B 124.7(14) . . ? C23B C22B C27B 129.4(16) . . ? C24B C23B C22B 110.1(14) . . ? C24B C23B C28B 128.7(15) . . ? C22B C23B C28B 120.5(16) . . ? C23B C24B C20B 111.8(13) . . ? C23B C24B C29B 124.5(14) . . ? C20B C24B C29B 121.8(16) . . ? C20B C25B H25D 109.5 . . ? C20B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C20B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C21B C26B H26D 109.5 . . ? C21B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C21B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C22B C27B H27D 109.5 . . ? C22B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C22B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C23B C28B H28D 109.5 . . ? C23B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C23B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C24B C29B H29D 109.5 . . ? C24B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C24B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C34B C30B C31B 106.0(11) . . ? C34B C30B C35B 125.1(12) . . ? C31B C30B C35B 126.7(12) . . ? C30B C31B C32B 107.6(11) . . ? C30B C31B C36B 124.7(10) . . ? C32B C31B C36B 125.5(9) . . ? C33B C32B C31B 109.8(10) . . ? C33B C32B C37B 124.5(10) . . ? C31B C32B C37B 123.8(11) . . ? C32B C33B C34B 105.9(11) . . ? C32B C33B C38B 128.5(11) . . ? C34B C33B C38B 123.7(13) . . ? C30B C34B C33B 110.6(12) . . ? C30B C34B C39B 123.9(12) . . ? C33B C34B C39B 124.4(13) . . ? C30B C35B H35D 109.4 . . ? C30B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C30B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C31B C36B H36D 109.5 . . ? C31B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C31B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C32B C37B H37D 109.5 . . ? C32B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C32B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C33B C38B H38D 109.5 . . ? C33B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C33B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C34B C39B H39D 109.5 . . ? C34B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C34B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C1 B1 C7 106.6(10) . . ? C1 B1 C19 108.6(10) . . ? C7 B1 C19 109.3(10) . . ? C1 B1 C13 113.0(10) . . ? C7 B1 C13 108.4(10) . . ? C19 B1 C13 110.8(10) . . ? C37 B2 C43 105.9(11) . . ? C37 B2 C31 114.5(11) . . ? C43 B2 C31 110.0(10) . . ? C37 B2 C25 110.6(10) . . ? C43 B2 C25 111.5(10) . . ? C31 B2 C25 104.4(10) . . ? C67 B3 C55 110.3(12) . . ? C67 B3 C61 107.0(10) . . ? C55 B3 C61 111.1(11) . . ? C67 B3 C49 114.6(11) . . ? C55 B3 C49 106.2(10) . . ? C61 B3 C49 107.7(11) . . ? C79 B4 C85 108.3(11) . . ? C79 B4 C73 110.2(11) . . ? C85 B4 C73 112.9(11) . . ? C79 B4 C91 109.2(11) . . ? C85 B4 C91 106.8(10) . . ? C73 B4 C91 109.4(11) . . ? C2 C1 C6 112.2(11) . . ? C2 C1 B1 125.0(12) . . ? C6 C1 B1 122.7(12) . . ? C3 C2 C1 127.7(13) . . ? C3 C2 H2 116.1 . . ? C1 C2 H2 116.1 . . ? C2 C3 C4 116.4(12) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C5 C4 C3 120.4(12) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.7(13) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 122.5(12) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? C8 C7 C12 114.6(12) . . ? C8 C7 B1 120.4(11) . . ? C12 C7 B1 125.1(12) . . ? C9 C8 C7 123.0(12) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C8 C9 C10 120.0(12) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.4(12) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 118.7(13) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C7 124.2(13) . . ? C11 C12 H12 117.9 . . ? C7 C12 H12 117.9 . . ? C14 C13 C18 117.9(12) . . ? C14 C13 B1 124.7(11) . . ? C18 C13 B1 117.4(11) . . ? C13 C14 C15 122.4(12) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C16 C15 C14 119.4(12) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 118.8(12) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 120.5(13) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.8(12) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C24 C19 C20 115.3(11) . . ? C24 C19 B1 124.2(11) . . ? C20 C19 B1 120.3(10) . . ? C19 C20 C21 122.5(12) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C22 C21 C20 119.1(14) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 120.2(13) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.4(12) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C19 C24 C23 123.4(12) . . ? C19 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? C26 C25 C30 115.4(10) . . ? C26 C25 B2 121.8(11) . . ? C30 C25 B2 122.2(11) . . ? C27 C26 C25 123.9(11) . . ? C27 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? C28 C27 C26 120.2(12) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 118.2(11) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C28 C29 C30 122.8(12) . . ? C28 C29 H29 118.6 . . ? C30 C29 H29 118.6 . . ? C29 C30 C25 119.3(12) . . ? C29 C30 H30 120.3 . . ? C25 C30 H30 120.3 . . ? C32 C31 C36 116.2(11) . . ? C32 C31 B2 127.2(12) . . ? C36 C31 B2 116.5(12) . . ? C31 C32 C33 121.7(11) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 122.7(12) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 116.4(13) . . ? C33 C34 H34 121.8 . . ? C35 C34 H34 121.8 . . ? C36 C35 C34 120.4(11) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C31 C36 C35 122.4(12) . . ? C31 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C38 C37 C42 112.7(11) . . ? C38 C37 B2 125.2(11) . . ? C42 C37 B2 122.0(11) . . ? C37 C38 C39 122.4(11) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C40 C39 C38 121.6(12) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 117.6(12) . . ? C39 C40 H40 121.2 . . ? C41 C40 H40 121.2 . . ? C42 C41 C40 120.6(12) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C37 125.0(12) . . ? C41 C42 H42 117.5 . . ? C37 C42 H42 117.5 . . ? C48 C43 C44 115.3(10) . . ? C48 C43 B2 126.3(10) . . ? C44 C43 B2 118.3(10) . . ? C43 C44 C45 123.1(11) . . ? C43 C44 H44 118.4 . . ? C45 C44 H44 118.4 . . ? C46 C45 C44 119.1(11) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C47 C46 C45 118.0(12) . . ? C47 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C46 C47 C48 121.9(11) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C43 C48 C47 122.5(11) . . ? C43 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C54 C49 C50 115.7(13) . . ? C54 C49 B3 123.4(12) . . ? C50 C49 B3 120.7(13) . . ? C51 C50 C49 123.1(15) . . ? C51 C50 H50 118.5 . . ? C49 C50 H50 118.5 . . ? C50 C51 C52 117.9(16) . . ? C50 C51 H51 121.1 . . ? C52 C51 H51 121.1 . . ? C51 C52 C53 122.3(16) . . ? C51 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C52 C53 C54 116.3(16) . . ? C52 C53 H53 121.9 . . ? C54 C53 H53 121.9 . . ? C49 C54 C53 124.4(15) . . ? C49 C54 H54 117.8 . . ? C53 C54 H54 117.8 . . ? C56 C55 C60 113.4(14) . . ? C56 C55 B3 122.2(13) . . ? C60 C55 B3 124.3(14) . . ? C57 C56 C55 120.8(15) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 122.0(16) . . ? C56 C57 H57 119.0 . . ? C58 C57 H57 119.0 . . ? C59 C58 C57 120.4(17) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C58 C59 C60 118.2(18) . . ? C58 C59 H59 120.9 . . ? C60 C59 H59 120.9 . . ? C59 C60 C55 124.8(17) . . ? C59 C60 H60 117.6 . . ? C55 C60 H60 117.6 . . ? C66 C61 C62 115.2(12) . . ? C66 C61 B3 119.7(12) . . ? C62 C61 B3 125.1(13) . . ? C63 C62 C61 121.0(13) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C64 C63 C62 122.8(13) . . ? C64 C63 H63 118.6 . . ? C62 C63 H63 118.6 . . ? C63 C64 C65 120.7(14) . . ? C63 C64 H64 119.7 . . ? C65 C64 H64 119.7 . . ? C66 C65 C64 115.5(13) . . ? C66 C65 H65 122.2 . . ? C64 C65 H65 122.3 . . ? C61 C66 C65 124.8(13) . . ? C61 C66 H66 117.6 . . ? C65 C66 H66 117.6 . . ? C68 C67 C72 114.3(11) . . ? C68 C67 B3 120.3(11) . . ? C72 C67 B3 125.4(11) . . ? C67 C68 C69 122.7(11) . . ? C67 C68 H68 118.6 . . ? C69 C68 H68 118.6 . . ? C70 C69 C68 121.4(12) . . ? C70 C69 H69 119.3 . . ? C68 C69 H69 119.3 . . ? C69 C70 C71 117.2(12) . . ? C69 C70 H70 121.4 . . ? C71 C70 H70 121.4 . . ? C72 C71 C70 120.1(12) . . ? C72 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C71 C72 C67 124.2(11) . . ? C71 C72 H72 117.9 . . ? C67 C72 H72 117.9 . . ? C78 C73 C74 111.3(12) . . ? C78 C73 B4 121.1(11) . . ? C74 C73 B4 127.4(13) . . ? C75 C74 C73 123.1(13) . . ? C75 C74 H74 118.5 . . ? C73 C74 H74 118.5 . . ? C76 C75 C74 122.0(13) . . ? C76 C75 H75 119.0 . . ? C74 C75 H75 119.0 . . ? C77 C76 C75 117.7(14) . . ? C77 C76 H76 121.2 . . ? C75 C76 H76 121.2 . . ? C76 C77 C78 122.0(14) . . ? C76 C77 H77 119.0 . . ? C78 C77 H77 119.0 . . ? C77 C78 C73 124.0(12) . . ? C77 C78 H78 118.0 . . ? C73 C78 H78 118.0 . . ? C80 C79 C84 114.4(12) . . ? C80 C79 B4 124.8(13) . . ? C84 C79 B4 120.9(12) . . ? C81 C80 C79 125.6(13) . . ? C81 C80 H80 117.2 . . ? C79 C80 H80 117.2 . . ? C82 C81 C80 118.8(13) . . ? C82 C81 H81 120.6 . . ? C80 C81 H81 120.6 . . ? C81 C82 C83 120.6(13) . . ? C81 C82 H82 119.7 . . ? C83 C82 H82 119.7 . . ? C82 C83 C84 120.0(14) . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C79 C84 C83 120.4(13) . . ? C79 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? C86 C85 C90 113.6(12) . . ? C86 C85 B4 121.3(13) . . ? C90 C85 B4 125.0(13) . . ? C85 C86 C87 125.8(14) . . ? C85 C86 H86 117.1 . . ? C87 C86 H86 117.1 . . ? C88 C87 C86 117.8(15) . . ? C88 C87 H87 121.1 . . ? C86 C87 H87 121.1 . . ? C89 C88 C87 121.0(14) . . ? C89 C88 H88 119.5 . . ? C87 C88 H88 119.5 . . ? C88 C89 C90 118.1(14) . . ? C88 C89 H89 120.9 . . ? C90 C89 H89 120.9 . . ? C85 C90 C89 123.3(13) . . ? C85 C90 H90 118.3 . . ? C89 C90 H90 118.4 . . ? C96 C91 C92 111.1(11) . . ? C96 C91 B4 126.0(12) . . ? C92 C91 B4 122.3(11) . . ? C93 C92 C91 125.1(12) . . ? C93 C92 H92 117.5 . . ? C91 C92 H92 117.5 . . ? C92 C93 C94 119.4(12) . . ? C92 C93 H93 120.3 . . ? C94 C93 H93 120.3 . . ? C95 C94 C93 118.8(11) . . ? C95 C94 H94 120.6 . . ? C93 C94 H94 120.6 . . ? C94 C95 C96 120.2(12) . . ? C94 C95 H95 119.9 . . ? C96 C95 H95 119.9 . . ? C95 C96 C91 125.3(13) . . ? C95 C96 H96 117.3 . . ? C91 C96 H96 117.3 . . ? #===END data_6'.2MeCN _database_code_depnum_ccdc_archive 'CCDC 764415' #TrackingRef 'revisedC002279ACIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H71 N9 U, I2, 2(C2 H3 N)' _chemical_formula_sum 'C58 H77 I2 N11 U' _chemical_formula_weight 1420.14 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' I I -0.4742 1.8119 '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' 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 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 54.595(5) _cell_length_b 9.4333(8) _cell_length_c 22.747(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.829(6) _cell_angle_gamma 90.00 _cell_volume 11700.7(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 136035 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method ? _exptl_crystal_F_000 5600 _exptl_absorpt_coefficient_mu 3.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 136035 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min -65 _diffrn_reflns_limit_h_max 66 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.68 _reflns_number_total 11069 _reflns_number_gt 6803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving atoms. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^] 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 11069 _refine_ls_number_parameters 670 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.516 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.140 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.113360(5) 0.69836(3) 0.575447(11) 0.02058(8) Uani 1 1 d . . . I1 I 0.040656(8) 0.21283(5) 0.377716(19) 0.03224(14) Uani 1 1 d . . . I2 I 0.194373(13) 0.21658(8) 0.41872(3) 0.0586(3) Uani 1 1 d . . . N1 N 0.07642(10) 0.7227(6) 0.5048(2) 0.0226(14) Uani 1 1 d . . . N2 N 0.07291(9) 0.7553(5) 0.6216(2) 0.0167(13) Uani 1 1 d . . . N3 N 0.11495(10) 0.7272(5) 0.6875(2) 0.0217(13) Uani 1 1 d . . . N4 N 0.15598(9) 0.6648(5) 0.6292(2) 0.0229(14) Uani 1 1 d . . . N5 N 0.07941(9) 0.7062(6) 0.4468(2) 0.0196(13) Uani 1 1 d . . . N6 N 0.03385(10) 0.7548(6) 0.4890(2) 0.0233(14) Uani 1 1 d . . . N7 N 0.17610(11) 0.6333(6) 0.5989(2) 0.0310(15) Uani 1 1 d . . . N8 N 0.17909(11) 0.6522(6) 0.7197(2) 0.0297(15) Uani 1 1 d . . . N9 N 0.13999(11) 0.6457(6) 0.4916(3) 0.0367(18) Uani 1 1 d . . . N10 N 0.14276(17) 0.8416(11) 0.3056(4) 0.095(3) Uani 1 1 d U . . N11 N 0.21616(14) 0.9457(9) 0.1569(3) 0.062(2) Uani 1 1 d . . . C1 C 0.05400(13) 0.7459(7) 0.5229(3) 0.0250(18) Uani 1 1 d . . . C2 C 0.05198(12) 0.7645(7) 0.5876(3) 0.0207(16) Uani 1 1 d . . . C3 C 0.02941(12) 0.7866(7) 0.6104(3) 0.0243(17) Uani 1 1 d . . . H3 H 0.0153 0.7915 0.5857 0.029 Uiso 1 1 calc R . . C4 C 0.02807(13) 0.8015(7) 0.6710(3) 0.0291(17) Uani 1 1 d . . . H4 H 0.0131 0.8150 0.6877 0.035 Uiso 1 1 calc R . . C5 C 0.04923(12) 0.7960(7) 0.7053(3) 0.0284(17) Uani 1 1 d . . . H5 H 0.0487 0.8085 0.7457 0.034 Uiso 1 1 calc R . . C6 C 0.07161(13) 0.7718(7) 0.6804(3) 0.0239(17) Uani 1 1 d . . . C7 C 0.09466(13) 0.7591(7) 0.7161(3) 0.0219(17) Uani 1 1 d . . . C8 C 0.09574(12) 0.7815(7) 0.7770(3) 0.0243(17) Uani 1 1 d . . . H8 H 0.0816 0.8051 0.7959 0.029 Uiso 1 1 calc R . . C9 C 0.11758(13) 0.7688(7) 0.8090(3) 0.0285(18) Uani 1 1 d . . . H9 H 0.1183 0.7823 0.8495 0.034 Uiso 1 1 calc R . . C10 C 0.13849(13) 0.7354(7) 0.7798(3) 0.0293(18) Uani 1 1 d . . . H10 H 0.1536 0.7274 0.8001 0.035 Uiso 1 1 calc R . . C11 C 0.13621(12) 0.7141(7) 0.7192(3) 0.0222(16) Uani 1 1 d . . . C12 C 0.15844(13) 0.6765(7) 0.6876(3) 0.0241(17) Uani 1 1 d . . . C13 C 0.06012(12) 0.7145(7) 0.4101(3) 0.0241(16) Uani 1 1 d . . . C14 C 0.03617(13) 0.7373(7) 0.4315(3) 0.0266(18) Uani 1 1 d . . . C15 C 0.01254(13) 0.7343(7) 0.3927(3) 0.0256(18) Uani 1 1 d . . . C16 C 0.01858(13) 0.7496(8) 0.3282(3) 0.032(2) Uani 1 1 d . . . H16A H 0.0222 0.8482 0.3202 0.039 Uiso 1 1 calc R . . H16B H 0.0043 0.7231 0.3035 0.039 Uiso 1 1 calc R . . C17 C 0.04035(12) 0.6582(8) 0.3120(3) 0.032(2) Uani 1 1 d . . . H17A H 0.0423 0.6651 0.2700 0.038 Uiso 1 1 calc R . . H17B H 0.0369 0.5600 0.3211 0.038 Uiso 1 1 calc R . . C18 C 0.06445(12) 0.7014(8) 0.3446(3) 0.0281(17) Uani 1 1 d . . . C19 C 0.00128(13) 0.5893(8) 0.4039(3) 0.037(2) Uani 1 1 d . . . H19A H -0.0139 0.5804 0.3811 0.055 Uiso 1 1 calc R . . H19B H -0.0017 0.5799 0.4449 0.055 Uiso 1 1 calc R . . H19C H 0.0124 0.5163 0.3926 0.055 Uiso 1 1 calc R . . C20 C -0.00470(13) 0.8510(7) 0.4108(3) 0.0332(19) Uani 1 1 d . . . H20A H 0.0031 0.9414 0.4066 0.050 Uiso 1 1 calc R . . H20B H -0.0086 0.8375 0.4511 0.050 Uiso 1 1 calc R . . H20C H -0.0195 0.8477 0.3861 0.050 Uiso 1 1 calc R . . C21 C 0.08435(13) 0.5897(8) 0.3353(3) 0.034(2) Uani 1 1 d . . . H21A H 0.0991 0.6156 0.3575 0.052 Uiso 1 1 calc R . . H21B H 0.0876 0.5846 0.2943 0.052 Uiso 1 1 calc R . . H21C H 0.0788 0.4990 0.3484 0.052 Uiso 1 1 calc R . . C22 C 0.07386(14) 0.8444(7) 0.3223(3) 0.037(2) Uani 1 1 d . . . H22A H 0.0624 0.9179 0.3312 0.055 Uiso 1 1 calc R . . H22B H 0.0755 0.8396 0.2805 0.055 Uiso 1 1 calc R . . H22C H 0.0895 0.8649 0.3414 0.055 Uiso 1 1 calc R . . C23 C 0.19708(13) 0.6123(8) 0.6290(3) 0.0316(19) Uani 1 1 d . . . C24 C 0.19884(14) 0.6189(7) 0.6909(3) 0.0293(18) Uani 1 1 d . . . C25 C 0.22156(14) 0.5903(9) 0.7288(3) 0.038(2) Uani 1 1 d . . . C26 C 0.24296(15) 0.5525(9) 0.6889(4) 0.062(3) Uani 1 1 d . . . H26A H 0.2581 0.5838 0.7087 0.074 Uiso 1 1 calc R . . H26B H 0.2438 0.4500 0.6858 0.074 Uiso 1 1 calc R . . C27 C 0.2420(2) 0.6102(14) 0.6299(5) 0.050(3) Uani 1 1 d U . . H27A H 0.2559 0.5732 0.6097 0.059 Uiso 1 1 calc R . . H27B H 0.2441 0.7121 0.6329 0.059 Uiso 1 1 calc R . . C28 C 0.21957(14) 0.5821(10) 0.5928(3) 0.045(2) Uani 1 1 d . . . C29 C 0.21683(14) 0.4713(8) 0.7718(3) 0.047(2) Uani 1 1 d . . . H29A H 0.2030 0.4954 0.7944 0.071 Uiso 1 1 calc R . . H29B H 0.2311 0.4582 0.7978 0.071 Uiso 1 1 calc R . . H29C H 0.2134 0.3852 0.7505 0.071 Uiso 1 1 calc R . . C30 C 0.22813(15) 0.7267(9) 0.7628(4) 0.058(3) Uani 1 1 d . . . H30A H 0.2308 0.8021 0.7355 0.087 Uiso 1 1 calc R . . H30B H 0.2428 0.7116 0.7871 0.087 Uiso 1 1 calc R . . H30C H 0.2149 0.7516 0.7872 0.087 Uiso 1 1 calc R . . C31 C 0.22051(19) 0.6816(11) 0.5405(4) 0.062(3) Uani 1 1 d U . . H31A H 0.2352 0.6639 0.5200 0.093 Uiso 1 1 calc R . . H31B H 0.2205 0.7780 0.5540 0.093 Uiso 1 1 calc R . . H31C H 0.2064 0.6659 0.5143 0.093 Uiso 1 1 calc R . . C32 C 0.21653(18) 0.4355(10) 0.5673(4) 0.058(3) Uani 1 1 d U . . H32A H 0.2317 0.4055 0.5516 0.087 Uiso 1 1 calc R . . H32B H 0.2039 0.4366 0.5364 0.087 Uiso 1 1 calc R . . H32C H 0.2121 0.3708 0.5975 0.087 Uiso 1 1 calc R . . C33 C 0.12185(15) 0.9458(7) 0.5099(3) 0.0295(19) Uani 1 1 d . . . C34 C 0.10126(14) 0.9840(7) 0.5413(3) 0.0297(19) Uani 1 1 d . . . C35 C 0.10884(14) 0.9927(7) 0.6015(3) 0.0262(18) Uani 1 1 d . . . C36 C 0.13410(13) 0.9674(7) 0.6065(3) 0.0272(18) Uani 1 1 d . . . C37 C 0.14257(14) 0.9371(7) 0.5498(3) 0.0327(19) Uani 1 1 d . . . C38 C 0.12318(15) 0.9449(8) 0.4430(3) 0.044(2) Uani 1 1 d . . . H38A H 0.1130 1.0189 0.4264 0.066 Uiso 1 1 calc R . . H38B H 0.1176 0.8550 0.4278 0.066 Uiso 1 1 calc R . . H38C H 0.1398 0.9602 0.4327 0.066 Uiso 1 1 calc R . . C39 C 0.07736(14) 1.0382(7) 0.5153(3) 0.044(2) Uani 1 1 d . . . H39A H 0.0744 0.9986 0.4768 0.067 Uiso 1 1 calc R . . H39B H 0.0780 1.1397 0.5125 0.067 Uiso 1 1 calc R . . H39C H 0.0644 1.0112 0.5400 0.067 Uiso 1 1 calc R . . C40 C 0.09360(14) 1.0630(7) 0.6462(3) 0.039(2) Uani 1 1 d . . . H40A H 0.0770 1.0296 0.6416 0.059 Uiso 1 1 calc R . . H40B H 0.0939 1.1638 0.6406 0.059 Uiso 1 1 calc R . . H40C H 0.1001 1.0404 0.6850 0.059 Uiso 1 1 calc R . . C41 C 0.15046(14) 1.0007(8) 0.6598(3) 0.038(2) Uani 1 1 d . . . H41A H 0.1562 1.0967 0.6575 0.056 Uiso 1 1 calc R . . H41B H 0.1642 0.9373 0.6614 0.056 Uiso 1 1 calc R . . H41C H 0.1414 0.9893 0.6947 0.056 Uiso 1 1 calc R . . C42 C 0.16868(13) 0.9278(8) 0.5350(3) 0.044(2) Uani 1 1 d . . . H42A H 0.1707 0.8511 0.5080 0.066 Uiso 1 1 calc R . . H42B H 0.1787 0.9112 0.5703 0.066 Uiso 1 1 calc R . . H42C H 0.1735 1.0150 0.5173 0.066 Uiso 1 1 calc R . . C43 C 0.10681(13) 0.4156(7) 0.5309(3) 0.0214(17) Uani 1 1 d . . . C44 C 0.08460(13) 0.4427(7) 0.5578(3) 0.0216(17) Uani 1 1 d . . . C45 C 0.09005(13) 0.4524(6) 0.6201(3) 0.0203(16) Uani 1 1 d . . . C46 C 0.11533(13) 0.4263(6) 0.6307(3) 0.0175(16) Uani 1 1 d . . . C47 C 0.12584(13) 0.4042(7) 0.5757(3) 0.0254(17) Uani 1 1 d . . . C48 C 0.10873(12) 0.3785(7) 0.4665(3) 0.0300(19) Uani 1 1 d . . . H48A H 0.1052 0.4609 0.4429 0.045 Uiso 1 1 calc R . . H48B H 0.0972 0.3049 0.4559 0.045 Uiso 1 1 calc R . . H48C H 0.1250 0.3462 0.4599 0.045 Uiso 1 1 calc R . . C49 C 0.05947(12) 0.4291(7) 0.5295(3) 0.0257(18) Uani 1 1 d . . . H49A H 0.0601 0.4455 0.4880 0.039 Uiso 1 1 calc R . . H49B H 0.0488 0.4977 0.5462 0.039 Uiso 1 1 calc R . . H49C H 0.0533 0.3355 0.5362 0.039 Uiso 1 1 calc R . . C50 C 0.07101(12) 0.4464(7) 0.6655(3) 0.0260(18) Uani 1 1 d . . . H50A H 0.0670 0.3493 0.6731 0.039 Uiso 1 1 calc R . . H50B H 0.0566 0.4960 0.6512 0.039 Uiso 1 1 calc R . . H50C H 0.0773 0.4900 0.7012 0.039 Uiso 1 1 calc R . . C51 C 0.12726(12) 0.3941(7) 0.6902(3) 0.0297(18) Uani 1 1 d . . . H51A H 0.1245 0.2965 0.6998 0.045 Uiso 1 1 calc R . . H51B H 0.1203 0.4537 0.7192 0.045 Uiso 1 1 calc R . . H51C H 0.1446 0.4115 0.6895 0.045 Uiso 1 1 calc R . . C52 C 0.15102(13) 0.3465(7) 0.5663(3) 0.0342(19) Uani 1 1 d . . . H52A H 0.1497 0.2499 0.5533 0.051 Uiso 1 1 calc R . . H52B H 0.1607 0.3506 0.6027 0.051 Uiso 1 1 calc R . . H52C H 0.1587 0.4022 0.5371 0.051 Uiso 1 1 calc R . . C53 C 0.15007(16) 0.6197(9) 0.4507(4) 0.050(2) Uani 1 1 d . . . C54 C 0.16385(17) 0.5806(10) 0.3982(3) 0.073(3) Uani 1 1 d U . . H54A H 0.1768 0.6476 0.3935 0.109 Uiso 1 1 calc R . . H54B H 0.1529 0.5816 0.3638 0.109 Uiso 1 1 calc R . . H54C H 0.1707 0.4874 0.4036 0.109 Uiso 1 1 calc R . . C55 C 0.16237(19) 0.8779(11) 0.3012(4) 0.069(3) Uani 1 1 d D . . C56 C 0.18724(15) 0.9349(10) 0.2946(4) 0.069(3) Uani 1 1 d D . . H56A H 0.1903 0.9437 0.2536 0.103 Uiso 1 1 calc R . . H56B H 0.1991 0.8718 0.3130 0.103 Uiso 1 1 calc R . . H56C H 0.1886 1.0264 0.3130 0.103 Uiso 1 1 calc R . . C57 C 0.22526(10) 0.9299(6) 0.1177(3) 0.058(2) Uani 1 1 d U . . C58 C 0.23875(18) 0.9162(10) 0.0651(4) 0.078(3) Uani 1 1 d . . . H58A H 0.2453 1.0067 0.0549 0.118 Uiso 1 1 calc R . . H58B H 0.2280 0.8828 0.0334 0.118 Uiso 1 1 calc R . . H58C H 0.2519 0.8498 0.0719 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02337(15) 0.01931(15) 0.01906(14) -0.00044(14) 0.00098(10) -0.00025(15) I1 0.0315(3) 0.0384(3) 0.0270(3) -0.0014(3) 0.0027(2) 0.0005(3) I2 0.0717(5) 0.0651(6) 0.0390(4) 0.0030(4) 0.0024(3) -0.0211(4) N1 0.029(4) 0.024(4) 0.015(3) 0.002(3) -0.001(3) -0.001(3) N2 0.020(3) 0.016(3) 0.014(3) -0.001(2) -0.002(2) -0.001(2) N3 0.021(3) 0.018(3) 0.026(3) 0.001(3) -0.004(3) 0.000(3) N4 0.018(3) 0.014(3) 0.037(4) 0.001(3) -0.005(3) -0.002(3) N5 0.022(3) 0.021(3) 0.015(3) 0.001(3) 0.001(2) -0.002(3) N6 0.023(4) 0.025(3) 0.022(3) -0.001(3) 0.000(3) 0.001(3) N7 0.030(4) 0.036(4) 0.028(3) -0.004(3) 0.008(3) -0.001(3) N8 0.034(4) 0.023(4) 0.030(3) -0.003(3) -0.011(3) 0.003(3) N9 0.045(4) 0.033(4) 0.034(4) -0.006(3) 0.018(3) -0.005(3) N10 0.086(6) 0.124(7) 0.073(5) -0.004(5) 0.009(5) -0.026(6) N11 0.041(5) 0.092(7) 0.052(5) 0.008(5) -0.011(4) 0.016(5) C1 0.024(4) 0.024(4) 0.027(4) 0.000(3) 0.003(4) -0.001(3) C2 0.022(4) 0.016(4) 0.023(4) -0.002(3) 0.001(3) 0.002(3) C3 0.025(4) 0.027(4) 0.021(4) -0.002(4) -0.004(3) -0.006(4) C4 0.026(4) 0.038(5) 0.024(4) -0.002(4) 0.007(3) 0.007(4) C5 0.029(4) 0.035(5) 0.021(4) -0.001(4) 0.001(3) 0.004(4) C6 0.030(4) 0.017(4) 0.025(4) 0.002(3) 0.002(3) 0.000(3) C7 0.029(4) 0.019(4) 0.017(4) 0.003(3) 0.002(3) -0.001(3) C8 0.026(4) 0.021(4) 0.026(4) -0.005(4) 0.003(3) 0.002(4) C9 0.044(5) 0.025(4) 0.016(4) 0.001(3) -0.004(4) -0.001(4) C10 0.033(5) 0.027(5) 0.027(4) -0.005(3) -0.008(4) -0.003(4) C11 0.028(4) 0.017(4) 0.022(4) -0.004(3) 0.003(3) -0.001(4) C12 0.035(5) 0.012(4) 0.026(4) -0.003(3) 0.006(4) 0.000(4) C13 0.025(4) 0.025(4) 0.022(4) 0.001(4) -0.003(3) -0.002(4) C14 0.042(5) 0.016(4) 0.022(4) -0.001(3) -0.001(3) -0.001(4) C15 0.029(4) 0.032(5) 0.016(4) 0.003(3) 0.002(3) -0.002(4) C16 0.035(5) 0.046(5) 0.015(4) 0.004(3) -0.004(3) -0.001(4) C17 0.034(5) 0.046(5) 0.016(4) 0.002(3) 0.004(3) -0.007(4) C18 0.037(4) 0.033(4) 0.014(3) -0.001(4) 0.001(3) 0.003(4) C19 0.034(5) 0.039(5) 0.036(4) 0.002(4) -0.005(4) -0.003(4) C20 0.030(5) 0.039(5) 0.030(4) -0.004(4) -0.005(4) 0.002(4) C21 0.047(5) 0.041(5) 0.016(4) -0.007(4) 0.005(4) -0.002(4) C22 0.044(5) 0.041(5) 0.025(4) 0.001(4) 0.005(4) -0.001(4) C23 0.014(4) 0.032(5) 0.047(5) -0.007(4) -0.010(4) -0.005(4) C24 0.030(5) 0.022(4) 0.035(5) -0.005(4) -0.004(4) 0.001(4) C25 0.025(5) 0.047(6) 0.041(5) 0.004(4) 0.000(4) 0.003(4) C26 0.030(5) 0.067(7) 0.088(7) 0.022(6) -0.003(5) 0.010(5) C27 0.034(5) 0.068(6) 0.049(5) -0.004(5) 0.016(5) 0.008(5) C28 0.026(5) 0.072(7) 0.037(5) -0.013(5) 0.000(4) 0.011(5) C29 0.029(5) 0.049(6) 0.062(6) 0.021(5) -0.010(4) 0.004(4) C30 0.045(6) 0.058(6) 0.068(6) -0.011(5) -0.024(5) -0.004(5) C31 0.053(5) 0.061(6) 0.075(6) 0.005(5) 0.034(5) 0.004(5) C32 0.048(5) 0.052(6) 0.078(6) -0.026(5) 0.036(5) 0.000(5) C33 0.052(6) 0.008(4) 0.029(4) 0.002(3) 0.004(4) -0.015(4) C34 0.035(5) 0.011(4) 0.042(5) -0.001(4) -0.004(4) -0.006(4) C35 0.040(5) 0.014(4) 0.025(4) -0.003(3) -0.002(4) -0.005(4) C36 0.029(5) 0.018(4) 0.035(4) 0.011(4) -0.002(4) -0.001(4) C37 0.030(5) 0.030(5) 0.038(5) -0.005(4) 0.006(4) -0.006(4) C38 0.060(6) 0.046(6) 0.026(4) 0.002(4) 0.007(4) -0.014(5) C39 0.053(6) 0.017(4) 0.062(6) 0.017(4) -0.006(5) 0.002(4) C40 0.053(6) 0.022(5) 0.043(5) -0.011(4) 0.008(4) -0.003(4) C41 0.046(5) 0.026(5) 0.039(5) -0.006(4) -0.009(4) -0.006(4) C42 0.028(5) 0.038(5) 0.067(6) 0.000(4) 0.006(4) -0.005(4) C43 0.025(5) 0.021(4) 0.019(4) 0.001(3) 0.004(3) -0.001(4) C44 0.026(4) 0.013(4) 0.026(4) -0.003(3) 0.001(3) 0.005(3) C45 0.029(5) 0.010(4) 0.022(4) 0.000(3) 0.003(3) 0.001(3) C46 0.030(5) 0.008(4) 0.014(3) 0.001(3) -0.001(3) 0.003(3) C47 0.031(5) 0.014(4) 0.031(4) 0.004(3) 0.001(4) 0.002(4) C48 0.031(5) 0.025(4) 0.034(4) -0.005(4) 0.004(4) -0.005(4) C49 0.027(5) 0.020(4) 0.030(4) 0.008(3) 0.003(3) 0.001(4) C50 0.033(5) 0.017(4) 0.027(4) -0.001(3) 0.001(4) -0.002(3) C51 0.031(5) 0.022(4) 0.036(4) 0.003(4) -0.003(4) 0.005(4) C52 0.037(5) 0.027(5) 0.038(4) 0.004(4) 0.003(4) 0.007(4) C53 0.052(6) 0.034(5) 0.062(6) 0.007(5) -0.010(5) -0.001(5) C54 0.083(6) 0.084(6) 0.053(5) -0.011(5) 0.030(5) 0.024(5) C55 0.084(9) 0.086(8) 0.037(5) -0.008(5) -0.005(6) -0.008(7) C56 0.047(7) 0.082(8) 0.076(7) -0.010(6) -0.007(5) -0.008(6) C57 0.054(4) 0.061(4) 0.057(4) -0.010(3) -0.009(3) 0.016(3) C58 0.096(9) 0.061(7) 0.078(7) 0.015(6) 0.000(7) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U N9 2.505(6) . ? U N1 2.526(5) . ? U N2 2.549(5) . ? U N3 2.560(5) . ? U N4 2.594(5) . ? U C33 2.821(6) . ? U C37 2.837(7) . ? U C35 2.853(7) . ? U C36 2.853(7) . ? U C46 2.857(6) . ? U C45 2.857(6) . ? U C47 2.857(7) . ? U C43 2.869(7) . ? U C34 2.872(7) . ? U C44 2.895(7) . ? N1 C1 1.328(8) . ? N1 N5 1.348(6) . ? N2 C6 1.350(7) . ? N2 C2 1.350(8) . ? N3 C11 1.342(8) . ? N3 C7 1.348(8) . ? N4 C12 1.333(7) . ? N4 N7 1.358(7) . ? N5 C13 1.313(7) . ? N6 C1 1.315(8) . ? N6 C14 1.330(7) . ? N7 C23 1.319(8) . ? N8 C24 1.326(8) . ? N8 C12 1.332(8) . ? N9 C53 1.131(9) . ? N10 C55 1.133(11) . ? N11 C57 1.053(8) . ? C1 C2 1.492(8) . ? C2 C3 1.376(8) . ? C3 C4 1.391(8) . ? C3 H3 0.9300 . ? C4 C5 1.363(9) . ? C4 H4 0.9300 . ? C5 C6 1.390(9) . ? C5 H5 0.9300 . ? C6 C7 1.470(9) . ? C7 C8 1.399(8) . ? C8 C9 1.372(9) . ? C8 H8 0.9300 . ? C9 C10 1.385(9) . ? C9 H9 0.9300 . ? C10 C11 1.392(8) . ? C10 H10 0.9300 . ? C11 C12 1.484(9) . ? C13 C14 1.434(9) . ? C13 C18 1.526(8) . ? C14 C15 1.526(9) . ? C15 C20 1.518(9) . ? C15 C19 1.526(9) . ? C15 C16 1.528(8) . ? C16 C17 1.528(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.533(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.536(9) . ? C18 C22 1.538(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.409(9) . ? C23 C28 1.537(9) . ? C24 C25 1.499(9) . ? C25 C29 1.520(9) . ? C25 C30 1.535(10) . ? C25 C26 1.556(10) . ? C26 C27 1.446(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.475(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C32 1.506(11) . ? C28 C31 1.519(11) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.409(9) . ? C33 C37 1.417(9) . ? C33 C38 1.527(8) . ? C34 C35 1.412(9) . ? C34 C39 1.496(10) . ? C35 C36 1.399(9) . ? C35 C40 1.499(9) . ? C36 C37 1.421(9) . ? C36 C41 1.503(9) . ? C37 C42 1.483(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.407(8) . ? C43 C47 1.422(9) . ? C43 C48 1.515(8) . ? C44 C45 1.437(8) . ? C44 C49 1.491(9) . ? C45 C46 1.411(9) . ? C45 C50 1.502(8) . ? C46 C47 1.416(8) . ? C46 C51 1.504(8) . ? C47 C52 1.504(9) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.488(11) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.475(8) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.441(10) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? 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 N9 U N1 90.51(18) . . ? N9 U N2 154.54(18) . . ? N1 U N2 64.03(16) . . ? N9 U N3 141.89(19) . . ? N1 U N3 127.60(17) . . ? N2 U N3 63.57(16) . . ? N9 U N4 78.11(19) . . ? N1 U N4 168.62(16) . . ? N2 U N4 127.35(17) . . ? N3 U N4 63.77(17) . . ? C1 N1 N5 118.7(5) . . ? C1 N1 U 122.5(4) . . ? N5 N1 U 118.7(4) . . ? C6 N2 C2 118.3(5) . . ? C6 N2 U 121.4(4) . . ? C2 N2 U 120.2(4) . . ? C11 N3 C7 118.0(5) . . ? C11 N3 U 120.8(4) . . ? C7 N3 U 121.2(4) . . ? C12 N4 N7 118.7(6) . . ? C12 N4 U 120.2(4) . . ? N7 N4 U 121.1(4) . . ? C13 N5 N1 118.9(5) . . ? C1 N6 C14 116.9(6) . . ? C23 N7 N4 118.3(6) . . ? C24 N8 C12 117.2(6) . . ? C53 N9 U 173.6(7) . . ? N6 C1 N1 125.8(6) . . ? N6 C1 C2 118.1(6) . . ? N1 C1 C2 116.0(6) . . ? N2 C2 C3 122.9(6) . . ? N2 C2 C1 117.1(6) . . ? C3 C2 C1 120.0(6) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 120.7(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? N2 C6 C5 120.8(6) . . ? N2 C6 C7 116.9(6) . . ? C5 C6 C7 122.2(6) . . ? N3 C7 C8 121.2(6) . . ? N3 C7 C6 116.9(6) . . ? C8 C7 C6 121.9(6) . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 118.7(6) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 118.2(7) . . ? C9 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? N3 C11 C10 123.5(6) . . ? N3 C11 C12 117.9(6) . . ? C10 C11 C12 118.6(6) . . ? N8 C12 N4 124.9(6) . . ? N8 C12 C11 117.8(6) . . ? N4 C12 C11 117.3(6) . . ? N5 C13 C14 120.6(6) . . ? N5 C13 C18 117.2(6) . . ? C14 C13 C18 122.2(6) . . ? N6 C14 C13 119.0(6) . . ? N6 C14 C15 116.8(6) . . ? C13 C14 C15 124.0(6) . . ? C20 C15 C19 110.2(6) . . ? C20 C15 C14 110.4(5) . . ? C19 C15 C14 104.9(5) . . ? C20 C15 C16 111.0(6) . . ? C19 C15 C16 110.6(6) . . ? C14 C15 C16 109.7(6) . . ? C15 C16 C17 112.7(5) . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 113.1(6) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C13 C18 C17 108.8(5) . . ? C13 C18 C21 109.5(5) . . ? C17 C18 C21 110.3(6) . . ? C13 C18 C22 108.7(6) . . ? C17 C18 C22 111.5(6) . . ? C21 C18 C22 107.9(5) . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N7 C23 C24 121.7(6) . . ? N7 C23 C28 116.5(6) . . ? C24 C23 C28 121.8(6) . . ? N8 C24 C23 119.1(7) . . ? N8 C24 C25 115.4(6) . . ? C23 C24 C25 125.4(7) . . ? C24 C25 C29 109.9(6) . . ? C24 C25 C30 107.7(6) . . ? C29 C25 C30 109.7(6) . . ? C24 C25 C26 109.3(6) . . ? C29 C25 C26 111.3(7) . . ? C30 C25 C26 108.8(7) . . ? C27 C26 C25 117.4(7) . . ? C27 C26 H26A 107.9 . . ? C25 C26 H26A 108.0 . . ? C27 C26 H26B 108.0 . . ? C25 C26 H26B 108.0 . . ? H26A C26 H26B 107.2 . . ? C26 C27 C28 117.0(9) . . ? C26 C27 H27A 108.0 . . ? C28 C27 H27A 108.0 . . ? C26 C27 H27B 108.0 . . ? C28 C27 H27B 108.0 . . ? H27A C27 H27B 107.3 . . ? C27 C28 C32 117.3(9) . . ? C27 C28 C31 106.1(8) . . ? C32 C28 C31 105.8(7) . . ? C27 C28 C23 108.8(7) . . ? C32 C28 C23 107.5(7) . . ? C31 C28 C23 111.3(7) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C37 108.8(6) . . ? C34 C33 C38 125.8(7) . . ? C37 C33 C38 124.2(7) . . ? C33 C34 C35 107.7(7) . . ? C33 C34 C39 126.1(7) . . ? C35 C34 C39 124.9(7) . . ? C36 C35 C34 108.0(6) . . ? C36 C35 C40 126.7(7) . . ? C34 C35 C40 122.5(7) . . ? C35 C36 C37 108.9(6) . . ? C35 C36 C41 125.0(6) . . ? C37 C36 C41 124.6(7) . . ? C33 C37 C36 106.5(6) . . ? C33 C37 C42 127.2(7) . . ? C36 C37 C42 125.2(7) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C47 108.5(6) . . ? C44 C43 C48 124.3(6) . . ? C47 C43 C48 126.3(6) . . ? C43 C44 C45 107.4(6) . . ? C43 C44 C49 126.3(6) . . ? C45 C44 C49 124.8(6) . . ? C46 C45 C44 108.1(5) . . ? C46 C45 C50 125.5(6) . . ? C44 C45 C50 124.0(6) . . ? C45 C46 C47 108.1(6) . . ? C45 C46 C51 124.4(6) . . ? C47 C46 C51 126.1(6) . . ? C46 C47 C43 107.9(6) . . ? C46 C47 C52 126.2(6) . . ? C43 C47 C52 124.5(6) . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N9 C53 C54 177.6(9) . . ? 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 . . ? N10 C55 C56 176.1(13) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N11 C57 C58 176.2(9) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ?