Supplementary information (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Teruo Shinmyozu' _publ_contact_author_address ; Institute for Materials Chemistry and Engineering Kyushu University Hakozaki 6-10-1, Higashi-ku Fukuoka 812-8581 JAPAN ; _publ_contact_author_email KISOYUKI@MS.IFOC.KYUSHU-U.AC.JP _publ_section_title ; The first X-ray crystallographic evidence of a cyclic aniline trimer via self-complementary N-H...pi Interactions: The aniline inclusion both inside and outside the macrocyclic cavity ; loop_ _publ_author_name 'Teruo Shinmyozu' 'Shin-ichiro Kato' 'Takeshi Nakagaki' 'Toshiaki Shimasaki' # Attachment 'CCDC658507.cif' data_toluene _database_code_depnum_ccdc_archive 'CCDC 658507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H104 N4 O12' _chemical_formula_weight 1505.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0793(4) _cell_length_b 29.4107(9) _cell_length_c 23.5417(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.9242(9) _cell_angle_gamma 90.00 _cell_volume 8283.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9337 _exptl_absorpt_correction_T_max 0.9906 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58764 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18092 _reflns_number_gt 10852 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+0.0000P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18092 _refine_ls_number_parameters 1071 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.46362(18) -0.00208(7) 0.81244(9) 0.0221(5) Uani 1 1 d . . . C2 C 0.40832(18) -0.04777(7) 0.80562(9) 0.0237(5) Uani 1 1 d . . . O1 O 0.33165(13) -0.05977(5) 0.77085(7) 0.0302(4) Uani 1 1 d . . . N1 N 0.46524(15) -0.07509(6) 0.84851(8) 0.0238(4) Uani 1 1 d . . . C3 C 0.54905(18) -0.05151(7) 0.88299(10) 0.0247(5) Uani 1 1 d . . . O2 O 0.60670(14) -0.06653(5) 0.92428(7) 0.0343(4) Uani 1 1 d . . . C4 C 0.54859(18) -0.00452(7) 0.85839(9) 0.0224(5) Uani 1 1 d . . . C5 C 0.61733(18) 0.03202(7) 0.87603(9) 0.0236(5) Uani 1 1 d . . . H1 H 0.6757 0.0303 0.9074 0.028 Uiso 1 1 calc R . . C6 C 0.59403(18) 0.07131(7) 0.84417(9) 0.0218(5) Uani 1 1 d . . . C7 C 0.64789(19) 0.11704(7) 0.85211(10) 0.0243(5) Uani 1 1 d . . . O3 O 0.72204(14) 0.12937(5) 0.88821(7) 0.0326(4) Uani 1 1 d . . . N2 N 0.59384(15) 0.14452(6) 0.80860(8) 0.0232(4) Uani 1 1 d . . . C8 C 0.50934(18) 0.12123(7) 0.77372(10) 0.0233(5) Uani 1 1 d . . . O4 O 0.45124(14) 0.13686(5) 0.73290(7) 0.0319(4) Uani 1 1 d . . . C9 C 0.50925(18) 0.07398(7) 0.79817(9) 0.0215(5) Uani 1 1 d . . . C10 C 0.43981(18) 0.03727(7) 0.78061(9) 0.0232(5) Uani 1 1 d . . . H2 H 0.3810 0.0391 0.7494 0.028 Uiso 1 1 calc R . . C11 C 0.62000(19) 0.19251(7) 0.80280(10) 0.0266(5) Uani 1 1 d . . . H3 H 0.6389 0.2059 0.8415 0.032 Uiso 1 1 calc R . . H4 H 0.5528 0.2084 0.7835 0.032 Uiso 1 1 calc R . . C12 C 0.71600(18) 0.20061(7) 0.76904(9) 0.0225(5) Uani 1 1 d . . . C13 C 0.77458(18) 0.16688(7) 0.74626(9) 0.0238(5) Uani 1 1 d . . . H5 H 0.7545 0.1361 0.7514 0.029 Uiso 1 1 calc R . . C14 C 0.86447(17) 0.17662(7) 0.71512(9) 0.0209(4) Uani 1 1 d . . . C15 C 0.92945(18) 0.14209(7) 0.69357(9) 0.0233(5) Uani 1 1 d . . . H6 H 0.9127 0.1111 0.7002 0.028 Uiso 1 1 calc R . . C16 C 1.01555(18) 0.15216(7) 0.66353(9) 0.0218(5) Uani 1 1 d . . . C17 C 1.03790(17) 0.19857(7) 0.65239(9) 0.0224(5) Uani 1 1 d . . . C18 C 0.97815(18) 0.23315(7) 0.67327(9) 0.0229(5) Uani 1 1 d . . . H7 H 0.9952 0.2639 0.6658 0.027 Uiso 1 1 calc R . . C19 C 0.89127(18) 0.22293(7) 0.70591(9) 0.0216(5) Uani 1 1 d . . . C20 C 0.83043(18) 0.25765(7) 0.72959(9) 0.0236(5) Uani 1 1 d . . . H8 H 0.8473 0.2887 0.7234 0.028 Uiso 1 1 calc R . . C21 C 0.74742(18) 0.24675(7) 0.76139(9) 0.0231(5) Uani 1 1 d . . . O5 O 0.68676(13) 0.27727(5) 0.78809(7) 0.0280(4) Uani 1 1 d . . . C22 C 0.7137(2) 0.32487(7) 0.78408(10) 0.0286(5) Uani 1 1 d . . . H9 H 0.7047 0.3346 0.7434 0.034 Uiso 1 1 calc R . . H10 H 0.7919 0.3305 0.8013 0.034 Uiso 1 1 calc R . . C23 C 0.6341(2) 0.35078(7) 0.81630(10) 0.0317(5) Uani 1 1 d . . . H11 H 0.6405 0.3837 0.8083 0.038 Uiso 1 1 calc R . . H12 H 0.5566 0.3413 0.8021 0.038 Uiso 1 1 calc R . . C24 C 0.6566(2) 0.34314(9) 0.88018(11) 0.0389(6) Uani 1 1 d . . . H13 H 0.7331 0.3539 0.8945 0.047 Uiso 1 1 calc R . . H14 H 0.6539 0.3101 0.8879 0.047 Uiso 1 1 calc R . . C25 C 0.5734(2) 0.36747(9) 0.91352(12) 0.0443(7) Uani 1 1 d . . . H15 H 0.5984 0.3634 0.9551 0.053 Uiso 1 1 calc R . . H16 H 0.5755 0.4004 0.9051 0.053 Uiso 1 1 calc R . . C26 C 0.4547(2) 0.35140(10) 0.90042(14) 0.0516(8) Uani 1 1 d . . . H17 H 0.4281 0.3569 0.8593 0.062 Uiso 1 1 calc R . . H18 H 0.4076 0.3697 0.9230 0.062 Uiso 1 1 calc R . . C27 C 0.4397(3) 0.30178(12) 0.9134(2) 0.1061(18) Uani 1 1 d . . . H19 H 0.4838 0.2833 0.8901 0.159 Uiso 1 1 calc R . . H20 H 0.3605 0.2937 0.9043 0.159 Uiso 1 1 calc R . . H21 H 0.4649 0.2961 0.9541 0.159 Uiso 1 1 calc R . . O6 O 1.12204(12) 0.20463(5) 0.61970(7) 0.0255(3) Uani 1 1 d . . . C28 C 1.14487(19) 0.25024(7) 0.60287(10) 0.0251(5) Uani 1 1 d . . . H22 H 1.1718 0.2688 0.6370 0.030 Uiso 1 1 calc R . . H23 H 1.0761 0.2644 0.5827 0.030 Uiso 1 1 calc R . . C29 C 1.23315(19) 0.24759(7) 0.56369(10) 0.0268(5) Uani 1 1 d . . . H24 H 1.2044 0.2294 0.5294 0.032 Uiso 1 1 calc R . . H25 H 1.2997 0.2319 0.5838 0.032 Uiso 1 1 calc R . . C30 C 1.26733(19) 0.29466(7) 0.54466(10) 0.0271(5) Uani 1 1 d . . . H26 H 1.2001 0.3107 0.5258 0.032 Uiso 1 1 calc R . . H27 H 1.2982 0.3124 0.5789 0.032 Uiso 1 1 calc R . . C31 C 1.35368(19) 0.29266(7) 0.50346(10) 0.0285(5) Uani 1 1 d . . . H28 H 1.4220 0.2778 0.5230 0.034 Uiso 1 1 calc R . . H29 H 1.3241 0.2735 0.4702 0.034 Uiso 1 1 calc R . . C32 C 1.3848(2) 0.33892(8) 0.48179(11) 0.0339(6) Uani 1 1 d . . . H30 H 1.3166 0.3539 0.4624 0.041 Uiso 1 1 calc R . . H31 H 1.4153 0.3580 0.5149 0.041 Uiso 1 1 calc R . . C33 C 1.4705(2) 0.33606(10) 0.44034(13) 0.0504(7) Uani 1 1 d . . . H32 H 1.5392 0.3221 0.4597 0.076 Uiso 1 1 calc R . . H33 H 1.4870 0.3667 0.4275 0.076 Uiso 1 1 calc R . . H34 H 1.4406 0.3175 0.4072 0.076 Uiso 1 1 calc R . . C34 C 1.09097(19) 0.11667(6) 0.64178(10) 0.0246(5) Uani 1 1 d . . . H35 H 1.0899 0.1209 0.6000 0.029 Uiso 1 1 calc R . . H36 H 1.1686 0.1217 0.6604 0.029 Uiso 1 1 calc R . . N3 N 1.05876(15) 0.07005(6) 0.65257(8) 0.0231(4) Uani 1 1 d . . . C35 C 0.98275(19) 0.04539(7) 0.61453(10) 0.0255(5) Uani 1 1 d . . . O7 O 0.93499(15) 0.05907(5) 0.56970(7) 0.0368(4) Uani 1 1 d . . . C36 C 0.97644(18) -0.00060(7) 0.64050(9) 0.0228(5) Uani 1 1 d . . . C37 C 0.91270(18) -0.03745(7) 0.61939(10) 0.0241(5) Uani 1 1 d . . . H37 H 0.8618 -0.0362 0.5849 0.029 Uiso 1 1 calc R . . C38 C 0.92894(18) -0.07632(7) 0.65260(9) 0.0229(5) Uani 1 1 d . . . C39 C 0.87813(19) -0.12225(7) 0.64214(10) 0.0256(5) Uani 1 1 d . . . O8 O 0.81155(14) -0.13494(5) 0.60252(7) 0.0325(4) Uani 1 1 d . . . N4 N 0.92503(15) -0.14935(6) 0.68797(8) 0.0248(4) Uani 1 1 d . . . C40 C 0.99814(18) -0.12492(7) 0.72762(10) 0.0239(5) Uani 1 1 d . . . O9 O 1.04543(13) -0.13968(5) 0.77252(7) 0.0305(4) Uani 1 1 d . . . C41 C 1.00277(17) -0.07804(7) 0.70345(9) 0.0215(5) Uani 1 1 d . . . C42 C 1.06712(18) -0.04086(7) 0.72466(9) 0.0228(5) Uani 1 1 d . . . H38 H 1.1181 -0.0420 0.7592 0.027 Uiso 1 1 calc R . . C43 C 1.05044(18) -0.00197(7) 0.69102(9) 0.0223(5) Uani 1 1 d . . . C44 C 1.10408(18) 0.04404(7) 0.69922(9) 0.0230(5) Uani 1 1 d . . . O10 O 1.17283(13) 0.05710(5) 0.73807(7) 0.0291(4) Uani 1 1 d . . . C45 C 0.89830(19) -0.19722(7) 0.69324(11) 0.0275(5) Uani 1 1 d . . . H39 H 0.9650 -0.2132 0.7128 0.033 Uiso 1 1 calc R . . H40 H 0.8805 -0.2104 0.6544 0.033 Uiso 1 1 calc R . . C46 C 0.80138(18) -0.20565(7) 0.72601(10) 0.0249(5) Uani 1 1 d . . . C47 C 0.74348(18) -0.17182(7) 0.74932(10) 0.0244(5) Uani 1 1 d . . . H41 H 0.7646 -0.1411 0.7447 0.029 Uiso 1 1 calc R . . C48 C 0.65371(18) -0.18137(7) 0.77990(9) 0.0233(5) Uani 1 1 d . . . C49 C 0.59181(18) -0.14696(7) 0.80365(9) 0.0243(5) Uani 1 1 d . . . H42 H 0.6102 -0.1160 0.7982 0.029 Uiso 1 1 calc R . . C50 C 0.50661(18) -0.15696(7) 0.83411(9) 0.0232(5) Uani 1 1 d . . . C51 C 0.48059(17) -0.20366(7) 0.84290(9) 0.0234(5) Uani 1 1 d . . . C52 C 0.53629(18) -0.23797(7) 0.81955(10) 0.0247(5) Uani 1 1 d . . . H43 H 0.5166 -0.2687 0.8254 0.030 Uiso 1 1 calc R . . C53 C 0.62283(18) -0.22789(7) 0.78690(9) 0.0237(5) Uani 1 1 d . . . C54 C 0.68212(18) -0.26264(7) 0.76210(10) 0.0250(5) Uani 1 1 d . . . H44 H 0.6621 -0.2936 0.7663 0.030 Uiso 1 1 calc R . . C55 C 0.76803(18) -0.25183(7) 0.73217(10) 0.0239(5) Uani 1 1 d . . . O11 O 0.83014(13) -0.28255(5) 0.70643(7) 0.0271(4) Uani 1 1 d . . . C56 C 0.79153(19) -0.32890(7) 0.70198(10) 0.0278(5) Uani 1 1 d . . . H45 H 0.7161 -0.3302 0.6794 0.033 Uiso 1 1 calc R . . H46 H 0.7869 -0.3413 0.7407 0.033 Uiso 1 1 calc R . . C57 C 0.8724(2) -0.35656(7) 0.67292(11) 0.0315(5) Uani 1 1 d . . . H47 H 0.8404 -0.3873 0.6650 0.038 Uiso 1 1 calc R . . H48 H 0.9424 -0.3601 0.6998 0.038 Uiso 1 1 calc R . . C58 C 0.9014(2) -0.33669(8) 0.61672(11) 0.0357(6) Uani 1 1 d . . . H49 H 0.9059 -0.3617 0.5890 0.043 Uiso 1 1 calc R . . H50 H 0.8406 -0.3160 0.6003 0.043 Uiso 1 1 calc R . . C59 C 1.0111(2) -0.31073(8) 0.62432(11) 0.0389(6) Uani 1 1 d . . . H51 H 1.0722 -0.3321 0.6382 0.047 Uiso 1 1 calc R . . H52 H 1.0084 -0.2874 0.6544 0.047 Uiso 1 1 calc R . . C60 C 1.0397(3) -0.28726(10) 0.56994(13) 0.0541(8) Uani 1 1 d . . . H53 H 0.9771 -0.2669 0.5549 0.065 Uiso 1 1 calc R . . H54 H 1.1068 -0.2681 0.5803 0.065 Uiso 1 1 calc R . . C61 C 1.0614(3) -0.31997(10) 0.52298(13) 0.0523(8) Uani 1 1 d . . . H55 H 1.1206 -0.3413 0.5380 0.079 Uiso 1 1 calc R . . H56 H 1.0848 -0.3029 0.4909 0.079 Uiso 1 1 calc R . . H57 H 0.9929 -0.3369 0.5096 0.079 Uiso 1 1 calc R . . O12 O 0.39815(13) -0.20964(5) 0.87634(7) 0.0275(4) Uani 1 1 d . . . C62 C 0.37259(19) -0.25554(7) 0.89125(10) 0.0260(5) Uani 1 1 d . . . H58 H 0.4407 -0.2709 0.9103 0.031 Uiso 1 1 calc R . . H59 H 0.3436 -0.2729 0.8563 0.031 Uiso 1 1 calc R . . C63 C 0.28576(19) -0.25331(7) 0.93119(10) 0.0266(5) Uani 1 1 d . . . H60 H 0.2207 -0.2355 0.9130 0.032 Uiso 1 1 calc R . . H61 H 0.3172 -0.2376 0.9670 0.032 Uiso 1 1 calc R . . C64 C 0.2477(2) -0.30082(7) 0.94541(10) 0.0278(5) Uani 1 1 d . . . H62 H 0.3137 -0.3186 0.9624 0.033 Uiso 1 1 calc R . . H63 H 0.2157 -0.3161 0.9094 0.033 Uiso 1 1 calc R . . C65 C 0.1611(2) -0.30117(7) 0.98677(10) 0.0283(5) Uani 1 1 d . . . H64 H 0.1947 -0.2880 1.0239 0.034 Uiso 1 1 calc R . . H65 H 0.0971 -0.2818 0.9711 0.034 Uiso 1 1 calc R . . C66 C 0.1192(2) -0.34853(8) 0.99678(11) 0.0341(6) Uani 1 1 d . . . H66 H 0.1832 -0.3676 1.0133 0.041 Uiso 1 1 calc R . . H67 H 0.0882 -0.3619 0.9594 0.041 Uiso 1 1 calc R . . C67 C 0.0303(2) -0.35025(10) 1.03641(13) 0.0515(8) Uani 1 1 d . . . H68 H 0.0614 -0.3387 1.0743 0.077 Uiso 1 1 calc R . . H69 H 0.0056 -0.3817 1.0400 0.077 Uiso 1 1 calc R . . H70 H -0.0336 -0.3314 1.0206 0.077 Uiso 1 1 calc R . . C68 C 0.43593(19) -0.12202(7) 0.85969(10) 0.0252(5) Uani 1 1 d . . . H71 H 0.3565 -0.1271 0.8441 0.030 Uiso 1 1 calc R . . H72 H 0.4436 -0.1267 0.9017 0.030 Uiso 1 1 calc R . . C69 C 0.6940(4) -0.04670(12) 1.07650(17) 0.0897(13) Uani 1 1 d . . . H73 H 0.6186 -0.0527 1.0567 0.135 Uiso 1 1 calc R . . H74 H 0.6980 -0.0553 1.1169 0.135 Uiso 1 1 calc R . . H75 H 0.7484 -0.0645 1.0586 0.135 Uiso 1 1 calc R . . C70 C 0.7197(3) 0.00243(11) 1.07234(13) 0.0584(9) Uani 1 1 d . . . C71 C 0.8028(3) 0.02276(15) 1.11012(14) 0.0699(11) Uani 1 1 d . . . H76 H 0.8436 0.0050 1.1396 0.084 Uiso 1 1 calc R . . C72 C 0.8268(3) 0.06683(17) 1.1061(2) 0.0851(13) Uani 1 1 d . . . H77 H 0.8827 0.0797 1.1337 0.102 Uiso 1 1 calc R . . C73 C 0.7746(4) 0.09390(14) 1.06415(17) 0.0760(11) Uani 1 1 d . . . H78 H 0.7954 0.1248 1.0609 0.091 Uiso 1 1 calc R . . C74 C 0.6875(4) 0.07419(13) 1.02531(15) 0.0721(11) Uani 1 1 d . . . H79 H 0.6474 0.0922 0.9959 0.087 Uiso 1 1 calc R . . C75 C 0.6610(3) 0.02870(12) 1.03040(12) 0.0561(8) Uani 1 1 d . . . H80 H 0.6020 0.0156 1.0047 0.067 Uiso 1 1 calc R . . C76 C 0.8660(4) -0.09104(15) 0.9091(3) 0.178(3) Uani 1 1 d . . . H81 H 0.8087 -0.1045 0.8805 0.267 Uiso 1 1 calc R . . H82 H 0.8426 -0.0933 0.9472 0.267 Uiso 1 1 calc R . . H83 H 0.9368 -0.1073 0.9089 0.267 Uiso 1 1 calc R . . C77 C 0.8814(3) -0.04194(12) 0.8947(2) 0.0652(10) Uani 1 1 d . . . C78 C 0.8903(3) -0.0099(2) 0.93698(17) 0.0936(16) Uani 1 1 d . . . H84 H 0.8840 -0.0187 0.9752 0.112 Uiso 1 1 calc R . . C79 C 0.9088(3) 0.0360(2) 0.9245(3) 0.122(3) Uani 1 1 d . . . H85 H 0.9171 0.0585 0.9536 0.147 Uiso 1 1 calc R . . C80 C 0.9143(3) 0.04671(15) 0.8678(4) 0.122(3) Uani 1 1 d . . . H86 H 0.9264 0.0773 0.8573 0.146 Uiso 1 1 calc R . . C81 C 0.9026(4) 0.0142(2) 0.8278(2) 0.114(2) Uani 1 1 d . . . H87 H 0.9059 0.0220 0.7889 0.137 Uiso 1 1 calc R . . C82 C 0.8865(3) -0.02853(15) 0.84160(18) 0.0794(12) Uani 1 1 d . . . H88 H 0.8782 -0.0507 0.8119 0.095 Uiso 1 1 calc R . . C83 C 0.3568(3) 0.12063(10) 0.57109(16) 0.0682(10) Uani 1 1 d . . . H89 H 0.4084 0.1283 0.6056 0.102 Uiso 1 1 calc R . . H90 H 0.2939 0.1420 0.5668 0.102 Uiso 1 1 calc R . . H91 H 0.3962 0.1227 0.5375 0.102 Uiso 1 1 calc R . . C84 C 0.3139(2) 0.07302(9) 0.57628(12) 0.0426(7) Uani 1 1 d . . . C85 C 0.3591(2) 0.04451(10) 0.61996(12) 0.0439(7) Uani 1 1 d . . . H92 H 0.4192 0.0551 0.6470 0.053 Uiso 1 1 calc R . . C86 C 0.3190(2) 0.00099(10) 0.62528(12) 0.0477(7) Uani 1 1 d . . . H93 H 0.3518 -0.0179 0.6558 0.057 Uiso 1 1 calc R . . C87 C 0.2324(2) -0.01529(10) 0.58682(12) 0.0469(7) Uani 1 1 d . . . H94 H 0.2046 -0.0452 0.5904 0.056 Uiso 1 1 calc R . . C88 C 0.1867(3) 0.01277(11) 0.54294(12) 0.0511(8) Uani 1 1 d . . . H95 H 0.1272 0.0020 0.5156 0.061 Uiso 1 1 calc R . . C89 C 0.2265(3) 0.05633(10) 0.53826(12) 0.0504(8) Uani 1 1 d . . . H96 H 0.1928 0.0753 0.5081 0.061 Uiso 1 1 calc R . . C90 C 0.6264(6) 0.0474(3) 0.5433(3) 0.0694(19) Uani 0.67 1 d P A 1 H97 H 0.6491 0.0794 0.5452 0.104 Uiso 0.67 1 calc PR A 1 H98 H 0.5467 0.0453 0.5285 0.104 Uiso 0.67 1 calc PR A 1 H99 H 0.6699 0.0309 0.5178 0.104 Uiso 0.67 1 calc PR A 1 C91 C 0.6474(3) 0.02664(16) 0.6032(2) 0.0427(10) Uani 0.67 1 d P A 1 C92 C 0.6909(6) 0.0522(2) 0.6498(3) 0.0477(17) Uani 0.67 1 d P A 1 H100 H 0.7100 0.0831 0.6444 0.057 Uiso 0.67 1 calc PR A 1 C93 C 0.7071(4) 0.03404(18) 0.7038(2) 0.0491(13) Uani 0.67 1 d P A 1 H101 H 0.7375 0.0522 0.7355 0.059 Uiso 0.67 1 calc PR A 1 C94 C 0.6794(4) -0.01078(16) 0.7122(2) 0.0466(11) Uani 0.67 1 d P A 1 H102 H 0.6905 -0.0237 0.7496 0.056 Uiso 0.67 1 calc PR A 1 C95 C 0.6352(5) -0.0367(2) 0.6655(3) 0.0528(15) Uani 0.67 1 d P A 1 H103 H 0.6139 -0.0673 0.6707 0.063 Uiso 0.67 1 calc PR A 1 C96 C 0.6214(2) -0.01674(11) 0.60837(16) 0.0581(9) Uani 1 1 d . . . H111 H 0.5945 -0.0344 0.5756 0.070 Uiso 0.67 1 calc PR A 1 H112 H 0.6018 -0.0475 0.5999 0.070 Uiso 0.33 1 calc PR A 2 C97 C 0.6370(12) -0.0402(4) 0.6980(5) 0.054(3) Uani 0.33 1 d P A 2 H104 H 0.6576 -0.0283 0.7370 0.082 Uiso 0.33 1 calc PR A 2 H105 H 0.6888 -0.0646 0.6910 0.082 Uiso 0.33 1 calc PR A 2 H106 H 0.5607 -0.0523 0.6940 0.082 Uiso 0.33 1 calc PR A 2 C98 C 0.6430(8) -0.0033(3) 0.6561(5) 0.050(2) Uani 0.33 1 d P A 2 C99 C 0.6732(11) 0.0399(4) 0.6725(6) 0.041(3) Uani 0.33 1 d P A 2 H107 H 0.6912 0.0469 0.7121 0.049 Uiso 0.33 1 calc PR A 2 C100 C 0.6782(11) 0.0744(4) 0.6314(6) 0.062(4) Uani 0.33 1 d P A 2 H108 H 0.6962 0.1048 0.6427 0.074 Uiso 0.33 1 calc PR A 2 C101 C 0.6558(10) 0.0624(4) 0.5741(5) 0.059(3) Uani 0.33 1 d P A 2 H109 H 0.6608 0.0846 0.5453 0.071 Uiso 0.33 1 calc PR A 2 C102 C 0.6276(9) 0.0202(4) 0.5594(7) 0.058(3) Uani 0.33 1 d P A 2 H110 H 0.6111 0.0120 0.5201 0.070 Uiso 0.33 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0229(11) 0.0186(10) 0.0272(11) -0.0014(9) 0.0120(9) 0.0019(9) C2 0.0257(11) 0.0201(10) 0.0275(12) -0.0025(9) 0.0114(10) 0.0021(10) O1 0.0289(8) 0.0246(8) 0.0362(9) -0.0044(7) 0.0010(8) -0.0028(7) N1 0.0277(10) 0.0174(8) 0.0276(10) -0.0008(8) 0.0085(8) -0.0029(8) C3 0.0256(11) 0.0230(11) 0.0266(12) 0.0004(9) 0.0075(10) -0.0006(10) O2 0.0405(10) 0.0281(8) 0.0328(9) 0.0081(7) -0.0006(8) -0.0041(8) C4 0.0259(11) 0.0181(10) 0.0247(11) 0.0014(9) 0.0092(9) 0.0008(10) C5 0.0245(11) 0.0215(10) 0.0251(11) 0.0002(9) 0.0047(9) -0.0011(10) C6 0.0227(11) 0.0191(10) 0.0258(11) -0.0018(9) 0.0107(9) 0.0005(9) C7 0.0261(11) 0.0213(10) 0.0282(12) 0.0002(9) 0.0132(10) -0.0009(10) O3 0.0343(9) 0.0280(8) 0.0351(10) -0.0009(7) 0.0029(8) -0.0070(8) N2 0.0249(9) 0.0179(8) 0.0283(10) 0.0019(8) 0.0088(8) -0.0002(8) C8 0.0253(11) 0.0190(10) 0.0275(12) -0.0006(9) 0.0098(10) 0.0027(10) O4 0.0373(9) 0.0222(8) 0.0352(10) 0.0034(7) 0.0022(8) 0.0058(7) C9 0.0241(11) 0.0158(9) 0.0266(12) 0.0009(9) 0.0111(9) 0.0024(9) C10 0.0237(11) 0.0189(10) 0.0279(12) -0.0014(9) 0.0061(9) 0.0017(9) C11 0.0312(12) 0.0155(10) 0.0362(13) -0.0010(9) 0.0160(10) -0.0024(10) C12 0.0250(11) 0.0193(10) 0.0241(11) -0.0004(9) 0.0070(9) -0.0016(9) C13 0.0279(11) 0.0149(9) 0.0295(12) 0.0016(9) 0.0074(10) 0.0000(9) C14 0.0228(11) 0.0176(10) 0.0228(11) 0.0011(8) 0.0043(9) 0.0001(9) C15 0.0283(11) 0.0157(9) 0.0269(11) 0.0017(9) 0.0076(10) -0.0013(9) C16 0.0260(11) 0.0172(10) 0.0226(11) -0.0010(8) 0.0048(9) -0.0004(9) C17 0.0230(10) 0.0210(10) 0.0241(11) 0.0004(9) 0.0067(9) -0.0037(9) C18 0.0287(11) 0.0160(9) 0.0248(11) 0.0011(9) 0.0068(9) -0.0018(9) C19 0.0233(11) 0.0180(10) 0.0239(11) 0.0010(9) 0.0046(9) -0.0006(9) C20 0.0294(12) 0.0145(9) 0.0272(12) 0.0019(9) 0.0055(10) -0.0007(9) C21 0.0245(11) 0.0190(10) 0.0263(11) -0.0028(9) 0.0047(9) 0.0010(9) O5 0.0317(8) 0.0167(7) 0.0385(9) -0.0031(7) 0.0155(7) -0.0015(7) C22 0.0363(13) 0.0157(10) 0.0361(13) -0.0008(9) 0.0130(11) -0.0018(10) C23 0.0416(14) 0.0196(10) 0.0360(14) 0.0003(10) 0.0129(11) 0.0022(11) C24 0.0405(14) 0.0401(14) 0.0363(14) -0.0047(12) 0.0060(12) 0.0015(13) C25 0.0487(16) 0.0461(15) 0.0404(15) -0.0045(13) 0.0140(13) 0.0069(14) C26 0.0492(17) 0.0495(17) 0.0601(19) 0.0097(15) 0.0215(15) 0.0055(15) C27 0.065(2) 0.073(3) 0.183(5) 0.070(3) 0.023(3) -0.010(2) O6 0.0302(8) 0.0159(7) 0.0335(9) 0.0021(6) 0.0158(7) -0.0020(7) C28 0.0274(11) 0.0177(10) 0.0318(12) 0.0011(9) 0.0103(10) -0.0039(10) C29 0.0297(12) 0.0197(10) 0.0330(13) 0.0004(9) 0.0118(10) -0.0016(10) C30 0.0311(12) 0.0219(10) 0.0304(12) 0.0014(9) 0.0121(10) -0.0014(10) C31 0.0300(12) 0.0278(11) 0.0294(12) 0.0010(10) 0.0103(10) -0.0010(10) C32 0.0367(13) 0.0345(13) 0.0327(13) 0.0030(11) 0.0124(11) -0.0084(12) C33 0.0527(17) 0.0514(17) 0.0530(18) 0.0096(14) 0.0282(15) -0.0096(15) C34 0.0292(12) 0.0158(10) 0.0304(12) 0.0017(9) 0.0099(10) 0.0004(9) N3 0.0272(10) 0.0165(8) 0.0268(10) 0.0001(7) 0.0083(8) -0.0008(8) C35 0.0288(12) 0.0188(10) 0.0301(12) 0.0015(9) 0.0088(10) 0.0017(10) O7 0.0455(10) 0.0264(8) 0.0359(10) 0.0085(8) -0.0036(8) -0.0041(8) C36 0.0256(11) 0.0179(10) 0.0267(11) 0.0017(9) 0.0096(10) 0.0002(9) C37 0.0258(11) 0.0205(10) 0.0269(12) -0.0004(9) 0.0072(9) -0.0013(10) C38 0.0231(11) 0.0183(10) 0.0301(12) -0.0006(9) 0.0128(10) -0.0002(9) C39 0.0261(11) 0.0243(11) 0.0293(12) -0.0002(10) 0.0143(10) -0.0017(10) O8 0.0335(9) 0.0273(8) 0.0364(10) -0.0022(7) 0.0038(8) -0.0060(8) N4 0.0268(10) 0.0180(8) 0.0312(10) 0.0016(8) 0.0099(8) -0.0021(8) C40 0.0231(11) 0.0190(10) 0.0317(13) -0.0023(9) 0.0117(10) 0.0018(10) O9 0.0357(9) 0.0217(8) 0.0343(9) 0.0036(7) 0.0061(8) 0.0032(7) C41 0.0223(11) 0.0158(9) 0.0288(12) 0.0002(9) 0.0115(9) 0.0015(9) C42 0.0238(11) 0.0192(10) 0.0265(11) 0.0006(9) 0.0070(9) 0.0038(9) C43 0.0229(11) 0.0174(10) 0.0286(12) -0.0026(9) 0.0108(9) -0.0004(9) C44 0.0251(11) 0.0183(10) 0.0276(12) -0.0019(9) 0.0108(10) 0.0032(10) O10 0.0302(8) 0.0236(8) 0.0332(9) -0.0022(7) 0.0032(7) -0.0021(7) C45 0.0301(12) 0.0162(10) 0.0384(13) 0.0016(9) 0.0127(11) -0.0003(10) C46 0.0269(11) 0.0194(10) 0.0296(12) 0.0030(9) 0.0086(10) -0.0020(10) C47 0.0281(11) 0.0142(9) 0.0322(12) 0.0033(9) 0.0087(10) -0.0015(9) C48 0.0248(11) 0.0170(10) 0.0284(12) 0.0034(9) 0.0052(10) 0.0001(9) C49 0.0260(11) 0.0163(10) 0.0313(12) 0.0021(9) 0.0056(10) -0.0009(9) C50 0.0264(11) 0.0185(10) 0.0250(11) 0.0010(9) 0.0043(9) 0.0005(9) C51 0.0224(11) 0.0219(10) 0.0271(12) 0.0012(9) 0.0078(9) -0.0035(9) C52 0.0261(11) 0.0161(10) 0.0325(12) 0.0030(9) 0.0061(10) -0.0024(9) C53 0.0252(11) 0.0179(10) 0.0277(12) 0.0020(9) 0.0030(10) -0.0011(9) C54 0.0265(11) 0.0153(10) 0.0338(13) 0.0002(9) 0.0060(10) -0.0032(9) C55 0.0263(11) 0.0172(10) 0.0287(12) -0.0006(9) 0.0051(10) 0.0006(9) O11 0.0296(8) 0.0160(7) 0.0382(9) -0.0018(6) 0.0135(7) -0.0022(7) C56 0.0336(12) 0.0180(10) 0.0326(13) -0.0021(9) 0.0074(11) -0.0057(10) C57 0.0382(13) 0.0207(11) 0.0373(14) -0.0034(10) 0.0112(11) -0.0004(11) C58 0.0400(14) 0.0345(13) 0.0329(13) -0.0011(11) 0.0064(11) 0.0032(12) C59 0.0453(15) 0.0322(13) 0.0412(15) -0.0002(11) 0.0128(13) -0.0040(12) C60 0.067(2) 0.0433(16) 0.0568(19) 0.0117(14) 0.0262(16) -0.0012(15) C61 0.0561(18) 0.0564(18) 0.0456(17) 0.0143(15) 0.0108(15) 0.0057(16) O12 0.0318(9) 0.0188(7) 0.0350(9) 0.0010(7) 0.0159(7) -0.0044(7) C62 0.0296(12) 0.0188(10) 0.0312(12) 0.0019(9) 0.0094(10) -0.0043(10) C63 0.0309(12) 0.0215(10) 0.0290(12) -0.0010(9) 0.0096(10) -0.0059(10) C64 0.0335(12) 0.0246(11) 0.0270(12) 0.0007(9) 0.0102(10) -0.0041(10) C65 0.0333(12) 0.0271(11) 0.0257(12) -0.0018(10) 0.0086(10) -0.0055(11) C66 0.0397(14) 0.0321(12) 0.0318(13) 0.0008(10) 0.0095(11) -0.0085(12) C67 0.0488(17) 0.0506(16) 0.0603(19) 0.0112(15) 0.0260(15) -0.0143(14) C68 0.0291(12) 0.0162(10) 0.0323(12) 0.0001(9) 0.0120(10) -0.0034(10) C69 0.132(4) 0.070(2) 0.077(3) 0.004(2) 0.050(3) 0.020(3) C70 0.072(2) 0.064(2) 0.0442(18) -0.0040(16) 0.0287(17) 0.0198(18) C71 0.053(2) 0.105(3) 0.048(2) -0.023(2) -0.0065(16) 0.031(2) C72 0.059(2) 0.108(3) 0.094(3) -0.034(3) 0.032(2) -0.007(2) C73 0.090(3) 0.084(3) 0.065(2) -0.015(2) 0.048(2) 0.001(2) C74 0.099(3) 0.081(3) 0.0406(19) 0.0019(18) 0.024(2) 0.026(2) C75 0.0573(19) 0.078(2) 0.0331(16) -0.0070(16) 0.0068(14) 0.0144(18) C76 0.056(3) 0.088(3) 0.390(10) 0.101(5) 0.029(4) 0.009(2) C77 0.0333(16) 0.061(2) 0.102(3) 0.020(2) 0.0132(19) 0.0078(16) C78 0.0323(18) 0.194(5) 0.053(2) 0.007(3) 0.0032(17) 0.025(3) C79 0.032(2) 0.134(5) 0.198(6) -0.109(5) 0.006(3) 0.003(3) C80 0.046(2) 0.047(2) 0.285(9) 0.031(4) 0.069(4) 0.0095(19) C81 0.093(3) 0.127(4) 0.139(5) 0.072(4) 0.079(3) 0.068(3) C82 0.073(3) 0.090(3) 0.075(3) -0.010(2) 0.013(2) 0.042(2) C83 0.086(3) 0.0502(18) 0.076(2) -0.0004(17) 0.038(2) 0.0014(18) C84 0.0487(16) 0.0447(15) 0.0388(15) -0.0032(13) 0.0217(13) 0.0103(14) C85 0.0380(14) 0.0524(17) 0.0426(16) -0.0014(14) 0.0103(13) 0.0055(14) C86 0.0496(17) 0.0538(17) 0.0418(16) 0.0046(14) 0.0140(14) 0.0131(15) C87 0.0509(17) 0.0460(16) 0.0482(17) -0.0091(14) 0.0224(15) 0.0034(14) C88 0.0492(17) 0.066(2) 0.0376(16) -0.0167(15) 0.0063(14) 0.0045(16) C89 0.0628(19) 0.0561(18) 0.0331(15) -0.0031(14) 0.0091(14) 0.0241(16) C90 0.059(4) 0.089(6) 0.062(5) 0.011(4) 0.014(3) 0.010(4) C91 0.028(2) 0.054(3) 0.048(3) -0.001(2) 0.011(2) 0.005(2) C92 0.048(3) 0.034(4) 0.065(6) -0.003(3) 0.022(4) -0.003(3) C93 0.051(3) 0.045(3) 0.055(3) -0.017(3) 0.019(3) -0.007(3) C94 0.046(3) 0.049(3) 0.049(3) -0.007(2) 0.022(2) 0.001(2) C95 0.046(3) 0.044(3) 0.066(4) -0.001(3) 0.003(3) -0.005(3) C96 0.0391(16) 0.056(2) 0.077(3) -0.0268(19) 0.0017(17) 0.0013(16) C97 0.059(7) 0.037(6) 0.064(8) -0.001(7) -0.007(8) 0.017(5) C98 0.047(6) 0.041(6) 0.069(8) 0.006(5) 0.031(5) 0.004(5) C99 0.041(7) 0.045(8) 0.034(7) 0.001(6) -0.002(6) -0.001(5) C100 0.053(7) 0.054(8) 0.080(10) 0.005(7) 0.015(7) -0.009(7) C101 0.055(7) 0.072(8) 0.051(7) 0.024(6) 0.008(6) -0.003(6) C102 0.028(5) 0.084(9) 0.065(9) 0.009(7) 0.012(5) 0.001(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 C1 C4 1.387(3) . ? C1 C10 1.387(3) . ? C1 C2 1.499(3) . ? C2 O1 1.201(3) . ? C2 N1 1.395(3) . ? N1 C3 1.392(3) . ? N1 C68 1.458(3) . ? C3 O2 1.199(3) . ? C3 C4 1.498(3) . ? C4 C5 1.386(3) . ? C5 C6 1.385(3) . ? C5 H1 0.9500 . ? C6 C9 1.386(3) . ? C6 C7 1.494(3) . ? C7 O3 1.203(3) . ? C7 N2 1.394(3) . ? N2 C8 1.398(3) . ? N2 C11 1.457(2) . ? C8 O4 1.201(3) . ? C8 C9 1.504(3) . ? C9 C10 1.394(3) . ? C10 H2 0.9500 . ? C11 C12 1.512(3) . ? C11 H3 0.9900 . ? C11 H4 0.9900 . ? C12 C13 1.370(3) . ? C12 C21 1.427(3) . ? C13 C14 1.421(3) . ? C13 H5 0.9500 . ? C14 C15 1.419(3) . ? C14 C19 1.423(3) . ? C15 C16 1.368(3) . ? C15 H6 0.9500 . ? C16 C17 1.423(3) . ? C16 C34 1.520(3) . ? C17 O6 1.368(2) . ? C17 C18 1.376(3) . ? C18 C19 1.416(3) . ? C18 H7 0.9500 . ? C19 C20 1.417(3) . ? C20 C21 1.370(3) . ? C20 H8 0.9500 . ? C21 O5 1.366(2) . ? O5 C22 1.443(2) . ? C22 C23 1.510(3) . ? C22 H9 0.9900 . ? C22 H10 0.9900 . ? C23 C24 1.508(3) . ? C23 H11 0.9900 . ? C23 H12 0.9900 . ? C24 C25 1.535(4) . ? C24 H13 0.9900 . ? C24 H14 0.9900 . ? C25 C26 1.501(4) . ? C25 H15 0.9900 . ? C25 H16 0.9900 . ? C26 C27 1.507(4) . ? C26 H17 0.9900 . ? C26 H18 0.9900 . ? C27 H19 0.9800 . ? C27 H20 0.9800 . ? C27 H21 0.9800 . ? O6 C28 1.436(2) . ? C28 C29 1.505(3) . ? C28 H22 0.9900 . ? C28 H23 0.9900 . ? C29 C30 1.529(3) . ? C29 H24 0.9900 . ? C29 H25 0.9900 . ? C30 C31 1.520(3) . ? C30 H26 0.9900 . ? C30 H27 0.9900 . ? C31 C32 1.519(3) . ? C31 H28 0.9900 . ? C31 H29 0.9900 . ? C32 C33 1.519(3) . ? C32 H30 0.9900 . ? C32 H31 0.9900 . ? C33 H32 0.9800 . ? C33 H33 0.9800 . ? C33 H34 0.9800 . ? C34 N3 1.457(2) . ? C34 H35 0.9900 . ? C34 H36 0.9900 . ? N3 C44 1.388(3) . ? N3 C35 1.394(3) . ? C35 O7 1.200(3) . ? C35 C36 1.491(3) . ? C36 C37 1.381(3) . ? C36 C43 1.386(3) . ? C37 C38 1.384(3) . ? C37 H37 0.9500 . ? C38 C41 1.392(3) . ? C38 C39 1.490(3) . ? C39 O8 1.204(3) . ? C39 N4 1.397(3) . ? N4 C40 1.393(3) . ? N4 C45 1.454(3) . ? C40 O9 1.211(3) . ? C40 C41 1.496(3) . ? C41 C42 1.394(3) . ? C42 C43 1.390(3) . ? C42 H38 0.9500 . ? C43 C44 1.501(3) . ? C44 O10 1.210(3) . ? C45 C46 1.509(3) . ? C45 H39 0.9900 . ? C45 H40 0.9900 . ? C46 C47 1.373(3) . ? C46 C55 1.430(3) . ? C47 C48 1.410(3) . ? C47 H41 0.9500 . ? C48 C49 1.418(3) . ? C48 C53 1.434(3) . ? C49 C50 1.365(3) . ? C49 H42 0.9500 . ? C50 C51 1.430(3) . ? C50 C68 1.513(3) . ? C51 O12 1.363(2) . ? C51 C52 1.369(3) . ? C52 C53 1.412(3) . ? C52 H43 0.9500 . ? C53 C54 1.419(3) . ? C54 C55 1.370(3) . ? C54 H44 0.9500 . ? C55 O11 1.368(3) . ? O11 C56 1.440(2) . ? C56 C57 1.506(3) . ? C56 H45 0.9900 . ? C56 H46 0.9900 . ? C57 C58 1.531(3) . ? C57 H47 0.9900 . ? C57 H48 0.9900 . ? C58 C59 1.518(3) . ? C58 H49 0.9900 . ? C58 H50 0.9900 . ? C59 C60 1.535(4) . ? C59 H51 0.9900 . ? C59 H52 0.9900 . ? C60 C61 1.515(4) . ? C60 H53 0.9900 . ? C60 H54 0.9900 . ? C61 H55 0.9800 . ? C61 H56 0.9800 . ? C61 H57 0.9800 . ? O12 C62 1.439(2) . ? C62 C63 1.503(3) . ? C62 H58 0.9900 . ? C62 H59 0.9900 . ? C63 C64 1.523(3) . ? C63 H60 0.9900 . ? C63 H61 0.9900 . ? C64 C65 1.524(3) . ? C64 H62 0.9900 . ? C64 H63 0.9900 . ? C65 C66 1.512(3) . ? C65 H64 0.9900 . ? C65 H65 0.9900 . ? C66 C67 1.517(4) . ? C66 H66 0.9900 . ? C66 H67 0.9900 . ? C67 H68 0.9800 . ? C67 H69 0.9800 . ? C67 H70 0.9800 . ? C68 H71 0.9900 . ? C68 H72 0.9900 . ? C69 C70 1.484(5) . ? C69 H73 0.9800 . ? C69 H74 0.9800 . ? C69 H75 0.9800 . ? C70 C75 1.371(4) . ? C70 C71 1.382(5) . ? C71 C72 1.335(5) . ? C71 H76 0.9500 . ? C72 C73 1.355(5) . ? C72 H77 0.9500 . ? C73 C74 1.419(5) . ? C73 H78 0.9500 . ? C74 C75 1.384(5) . ? C74 H79 0.9500 . ? C75 H80 0.9500 . ? C76 C77 1.500(5) . ? C76 H81 0.9800 . ? C76 H82 0.9800 . ? C76 H83 0.9800 . ? C77 C82 1.321(5) . ? C77 C78 1.363(6) . ? C78 C79 1.405(7) . ? C78 H84 0.9500 . ? C79 C80 1.381(8) . ? C79 H85 0.9500 . ? C80 C81 1.336(8) . ? C80 H86 0.9500 . ? C81 C82 1.320(6) . ? C81 H87 0.9500 . ? C82 H88 0.9500 . ? C83 C84 1.504(4) . ? C83 H89 0.9800 . ? C83 H90 0.9800 . ? C83 H91 0.9800 . ? C84 C89 1.377(4) . ? C84 C85 1.380(4) . ? C85 C86 1.380(4) . ? C85 H92 0.9500 . ? C86 C87 1.372(4) . ? C86 H93 0.9500 . ? C87 C88 1.377(4) . ? C87 H94 0.9500 . ? C88 C89 1.378(4) . ? C88 H95 0.9500 . ? C89 H96 0.9500 . ? C90 C91 1.526(8) . ? C90 H97 0.9800 . ? C90 H98 0.9800 . ? C90 H99 0.9800 . ? C91 C96 1.323(6) . ? C91 C92 1.373(8) . ? C92 C93 1.370(8) . ? C92 H100 0.9500 . ? C93 C94 1.381(7) . ? C93 H101 0.9500 . ? C94 C95 1.383(7) . ? C94 H102 0.9500 . ? C95 C96 1.455(7) . ? C95 H103 0.9500 . ? C96 C98 1.186(11) . ? C96 C102 1.593(14) . ? C96 H111 0.9500 . ? C96 H112 0.9500 . ? C97 C98 1.475(15) . ? C97 H104 0.9800 . ? C97 H105 0.9800 . ? C97 H106 0.9800 . ? C98 C99 1.364(17) . ? C99 C100 1.407(15) . ? C99 H107 0.9500 . ? C100 C101 1.385(18) . ? C100 H108 0.9500 . ? C101 C102 1.320(19) . ? C101 H109 0.9500 . ? C102 H110 0.9500 . ? 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 C4 C1 C10 122.74(19) . . ? C4 C1 C2 107.94(18) . . ? C10 C1 C2 129.3(2) . . ? O1 C2 N1 125.48(19) . . ? O1 C2 C1 128.8(2) . . ? N1 C2 C1 105.72(18) . . ? C3 N1 C2 112.40(17) . . ? C3 N1 C68 122.80(18) . . ? C2 N1 C68 124.63(18) . . ? O2 C3 N1 125.7(2) . . ? O2 C3 C4 128.6(2) . . ? N1 C3 C4 105.70(18) . . ? C5 C4 C1 122.80(19) . . ? C5 C4 C3 129.0(2) . . ? C1 C4 C3 108.20(18) . . ? C6 C5 C4 114.6(2) . . ? C6 C5 H1 122.7 . . ? C4 C5 H1 122.7 . . ? C5 C6 C9 122.90(19) . . ? C5 C6 C7 129.1(2) . . ? C9 C6 C7 107.98(18) . . ? O3 C7 N2 124.89(19) . . ? O3 C7 C6 129.0(2) . . ? N2 C7 C6 106.14(18) . . ? C7 N2 C8 112.17(17) . . ? C7 N2 C11 123.01(19) . . ? C8 N2 C11 124.75(18) . . ? O4 C8 N2 125.5(2) . . ? O4 C8 C9 129.0(2) . . ? N2 C8 C9 105.48(18) . . ? C6 C9 C10 122.49(19) . . ? C6 C9 C8 108.17(18) . . ? C10 C9 C8 129.3(2) . . ? C1 C10 C9 114.5(2) . . ? C1 C10 H2 122.8 . . ? C9 C10 H2 122.8 . . ? N2 C11 C12 113.18(17) . . ? N2 C11 H3 108.9 . . ? C12 C11 H3 108.9 . . ? N2 C11 H4 108.9 . . ? C12 C11 H4 108.9 . . ? H3 C11 H4 107.8 . . ? C13 C12 C21 118.58(19) . . ? C13 C12 C11 124.51(18) . . ? C21 C12 C11 116.90(18) . . ? C12 C13 C14 121.92(19) . . ? C12 C13 H5 119.0 . . ? C14 C13 H5 119.0 . . ? C15 C14 C13 122.68(18) . . ? C15 C14 C19 118.78(19) . . ? C13 C14 C19 118.53(19) . . ? C16 C15 C14 121.81(19) . . ? C16 C15 H6 119.1 . . ? C14 C15 H6 119.1 . . ? C15 C16 C17 118.69(19) . . ? C15 C16 C34 123.98(18) . . ? C17 C16 C34 117.32(18) . . ? O6 C17 C18 124.84(18) . . ? O6 C17 C16 113.77(18) . . ? C18 C17 C16 121.39(19) . . ? C17 C18 C19 120.09(19) . . ? C17 C18 H7 120.0 . . ? C19 C18 H7 120.0 . . ? C18 C19 C20 121.61(18) . . ? C18 C19 C14 119.14(19) . . ? C20 C19 C14 119.25(19) . . ? C21 C20 C19 120.33(19) . . ? C21 C20 H8 119.8 . . ? C19 C20 H8 119.8 . . ? O5 C21 C20 125.26(19) . . ? O5 C21 C12 113.47(18) . . ? C20 C21 C12 121.27(19) . . ? C21 O5 C22 117.89(17) . . ? O5 C22 C23 106.98(18) . . ? O5 C22 H9 110.3 . . ? C23 C22 H9 110.3 . . ? O5 C22 H10 110.3 . . ? C23 C22 H10 110.3 . . ? H9 C22 H10 108.6 . . ? C24 C23 C22 112.7(2) . . ? C24 C23 H11 109.0 . . ? C22 C23 H11 109.0 . . ? C24 C23 H12 109.0 . . ? C22 C23 H12 109.0 . . ? H11 C23 H12 107.8 . . ? C23 C24 C25 113.6(2) . . ? C23 C24 H13 108.9 . . ? C25 C24 H13 108.9 . . ? C23 C24 H14 108.9 . . ? C25 C24 H14 108.9 . . ? H13 C24 H14 107.7 . . ? C26 C25 C24 115.0(2) . . ? C26 C25 H15 108.5 . . ? C24 C25 H15 108.5 . . ? C26 C25 H16 108.5 . . ? C24 C25 H16 108.5 . . ? H15 C25 H16 107.5 . . ? C25 C26 C27 113.7(3) . . ? C25 C26 H17 108.8 . . ? C27 C26 H17 108.8 . . ? C25 C26 H18 108.8 . . ? C27 C26 H18 108.8 . . ? H17 C26 H18 107.7 . . ? C26 C27 H19 109.5 . . ? C26 C27 H20 109.5 . . ? H19 C27 H20 109.5 . . ? C26 C27 H21 109.5 . . ? H19 C27 H21 109.5 . . ? H20 C27 H21 109.5 . . ? C17 O6 C28 117.55(16) . . ? O6 C28 C29 107.45(17) . . ? O6 C28 H22 110.2 . . ? C29 C28 H22 110.2 . . ? O6 C28 H23 110.2 . . ? C29 C28 H23 110.2 . . ? H22 C28 H23 108.5 . . ? C28 C29 C30 112.05(18) . . ? C28 C29 H24 109.2 . . ? C30 C29 H24 109.2 . . ? C28 C29 H25 109.2 . . ? C30 C29 H25 109.2 . . ? H24 C29 H25 107.9 . . ? C31 C30 C29 112.88(18) . . ? C31 C30 H26 109.0 . . ? C29 C30 H26 109.0 . . ? C31 C30 H27 109.0 . . ? C29 C30 H27 109.0 . . ? H26 C30 H27 107.8 . . ? C32 C31 C30 113.80(19) . . ? C32 C31 H28 108.8 . . ? C30 C31 H28 108.8 . . ? C32 C31 H29 108.8 . . ? C30 C31 H29 108.8 . . ? H28 C31 H29 107.7 . . ? C33 C32 C31 112.9(2) . . ? C33 C32 H30 109.0 . . ? C31 C32 H30 109.0 . . ? C33 C32 H31 109.0 . . ? C31 C32 H31 109.0 . . ? H30 C32 H31 107.8 . . ? C32 C33 H32 109.5 . . ? C32 C33 H33 109.5 . . ? H32 C33 H33 109.5 . . ? C32 C33 H34 109.5 . . ? H32 C33 H34 109.5 . . ? H33 C33 H34 109.5 . . ? N3 C34 C16 113.62(17) . . ? N3 C34 H35 108.8 . . ? C16 C34 H35 108.8 . . ? N3 C34 H36 108.8 . . ? C16 C34 H36 108.8 . . ? H35 C34 H36 107.7 . . ? C44 N3 C35 111.98(17) . . ? C44 N3 C34 124.83(18) . . ? C35 N3 C34 123.07(18) . . ? O7 C35 N3 125.8(2) . . ? O7 C35 C36 128.3(2) . . ? N3 C35 C36 105.97(18) . . ? C37 C36 C43 123.19(19) . . ? C37 C36 C35 128.4(2) . . ? C43 C36 C35 108.35(18) . . ? C36 C37 C38 114.6(2) . . ? C36 C37 H37 122.7 . . ? C38 C37 H37 122.7 . . ? C37 C38 C41 122.69(19) . . ? C37 C38 C39 129.2(2) . . ? C41 C38 C39 108.05(18) . . ? O8 C39 N4 125.3(2) . . ? O8 C39 C38 128.7(2) . . ? N4 C39 C38 106.00(19) . . ? C40 N4 C39 112.05(18) . . ? C40 N4 C45 124.76(19) . . ? C39 N4 C45 123.18(19) . . ? O9 C40 N4 125.4(2) . . ? O9 C40 C41 128.7(2) . . ? N4 C40 C41 105.90(18) . . ? C38 C41 C42 122.64(19) . . ? C38 C41 C40 107.91(18) . . ? C42 C41 C40 129.4(2) . . ? C43 C42 C41 114.31(19) . . ? C43 C42 H38 122.8 . . ? C41 C42 H38 122.8 . . ? C36 C43 C42 122.56(19) . . ? C36 C43 C44 107.46(18) . . ? C42 C43 C44 130.0(2) . . ? O10 C44 N3 125.30(19) . . ? O10 C44 C43 128.5(2) . . ? N3 C44 C43 106.21(18) . . ? N4 C45 C46 113.58(18) . . ? N4 C45 H39 108.8 . . ? C46 C45 H39 108.8 . . ? N4 C45 H40 108.8 . . ? C46 C45 H40 108.8 . . ? H39 C45 H40 107.7 . . ? C47 C46 C55 118.8(2) . . ? C47 C46 C45 123.98(19) . . ? C55 C46 C45 117.22(19) . . ? C46 C47 C48 121.98(19) . . ? C46 C47 H41 119.0 . . ? C48 C47 H41 119.0 . . ? C47 C48 C49 122.93(19) . . ? C47 C48 C53 118.64(19) . . ? C49 C48 C53 118.43(19) . . ? C50 C49 C48 122.00(19) . . ? C50 C49 H42 119.0 . . ? C48 C49 H42 119.0 . . ? C49 C50 C51 118.67(19) . . ? C49 C50 C68 124.77(18) . . ? C51 C50 C68 116.56(18) . . ? O12 C51 C52 125.10(19) . . ? O12 C51 C50 113.59(18) . . ? C52 C51 C50 121.31(19) . . ? C51 C52 C53 120.36(19) . . ? C51 C52 H43 119.8 . . ? C53 C52 H43 119.8 . . ? C52 C53 C54 121.77(19) . . ? C52 C53 C48 119.1(2) . . ? C54 C53 C48 119.1(2) . . ? C55 C54 C53 120.38(19) . . ? C55 C54 H44 119.8 . . ? C53 C54 H44 119.8 . . ? O11 C55 C54 125.11(18) . . ? O11 C55 C46 113.77(19) . . ? C54 C55 C46 121.1(2) . . ? C55 O11 C56 117.75(16) . . ? O11 C56 C57 108.69(18) . . ? O11 C56 H45 110.0 . . ? C57 C56 H45 110.0 . . ? O11 C56 H46 110.0 . . ? C57 C56 H46 110.0 . . ? H45 C56 H46 108.3 . . ? C56 C57 C58 115.2(2) . . ? C56 C57 H47 108.5 . . ? C58 C57 H47 108.5 . . ? C56 C57 H48 108.5 . . ? C58 C57 H48 108.5 . . ? H47 C57 H48 107.5 . . ? C59 C58 C57 113.0(2) . . ? C59 C58 H49 109.0 . . ? C57 C58 H49 109.0 . . ? C59 C58 H50 109.0 . . ? C57 C58 H50 109.0 . . ? H49 C58 H50 107.8 . . ? C58 C59 C60 114.9(2) . . ? C58 C59 H51 108.5 . . ? C60 C59 H51 108.5 . . ? C58 C59 H52 108.5 . . ? C60 C59 H52 108.5 . . ? H51 C59 H52 107.5 . . ? C61 C60 C59 113.9(2) . . ? C61 C60 H53 108.8 . . ? C59 C60 H53 108.8 . . ? C61 C60 H54 108.8 . . ? C59 C60 H54 108.8 . . ? H53 C60 H54 107.7 . . ? C60 C61 H55 109.5 . . ? C60 C61 H56 109.5 . . ? H55 C61 H56 109.5 . . ? C60 C61 H57 109.5 . . ? H55 C61 H57 109.5 . . ? H56 C61 H57 109.5 . . ? C51 O12 C62 117.42(16) . . ? O12 C62 C63 107.66(17) . . ? O12 C62 H58 110.2 . . ? C63 C62 H58 110.2 . . ? O12 C62 H59 110.2 . . ? C63 C62 H59 110.2 . . ? H58 C62 H59 108.5 . . ? C62 C63 C64 110.80(18) . . ? C62 C63 H60 109.5 . . ? C64 C63 H60 109.5 . . ? C62 C63 H61 109.5 . . ? C64 C63 H61 109.5 . . ? H60 C63 H61 108.1 . . ? C63 C64 C65 113.66(18) . . ? C63 C64 H62 108.8 . . ? C65 C64 H62 108.8 . . ? C63 C64 H63 108.8 . . ? C65 C64 H63 108.8 . . ? H62 C64 H63 107.7 . . ? C66 C65 C64 112.35(19) . . ? C66 C65 H64 109.1 . . ? C64 C65 H64 109.1 . . ? C66 C65 H65 109.1 . . ? C64 C65 H65 109.1 . . ? H64 C65 H65 107.9 . . ? C65 C66 C67 114.0(2) . . ? C65 C66 H66 108.7 . . ? C67 C66 H66 108.7 . . ? C65 C66 H67 108.7 . . ? C67 C66 H67 108.7 . . ? H66 C66 H67 107.6 . . ? C66 C67 H68 109.5 . . ? C66 C67 H69 109.5 . . ? H68 C67 H69 109.5 . . ? C66 C67 H70 109.5 . . ? H68 C67 H70 109.5 . . ? H69 C67 H70 109.5 . . ? N1 C68 C50 114.00(18) . . ? N1 C68 H71 108.8 . . ? C50 C68 H71 108.8 . . ? N1 C68 H72 108.8 . . ? C50 C68 H72 108.8 . . ? H71 C68 H72 107.6 . . ? C70 C69 H73 109.5 . . ? C70 C69 H74 109.5 . . ? H73 C69 H74 109.5 . . ? C70 C69 H75 109.5 . . ? H73 C69 H75 109.5 . . ? H74 C69 H75 109.5 . . ? C75 C70 C71 118.5(3) . . ? C75 C70 C69 120.3(3) . . ? C71 C70 C69 121.3(4) . . ? C72 C71 C70 121.4(4) . . ? C72 C71 H76 119.3 . . ? C70 C71 H76 119.3 . . ? C71 C72 C73 122.6(4) . . ? C71 C72 H77 118.7 . . ? C73 C72 H77 118.7 . . ? C72 C73 C74 117.3(4) . . ? C72 C73 H78 121.3 . . ? C74 C73 H78 121.3 . . ? C75 C74 C73 119.9(4) . . ? C75 C74 H79 120.1 . . ? C73 C74 H79 120.1 . . ? C70 C75 C74 120.3(3) . . ? C70 C75 H80 119.9 . . ? C74 C75 H80 119.9 . . ? C77 C76 H81 109.5 . . ? C77 C76 H82 109.5 . . ? H81 C76 H82 109.5 . . ? C77 C76 H83 109.5 . . ? H81 C76 H83 109.5 . . ? H82 C76 H83 109.5 . . ? C82 C77 C78 118.4(4) . . ? C82 C77 C76 121.6(5) . . ? C78 C77 C76 120.0(5) . . ? C77 C78 C79 120.6(4) . . ? C77 C78 H84 119.7 . . ? C79 C78 H84 119.7 . . ? C80 C79 C78 116.9(4) . . ? C80 C79 H85 121.6 . . ? C78 C79 H85 121.6 . . ? C81 C80 C79 120.2(5) . . ? C81 C80 H86 119.9 . . ? C79 C80 H86 119.9 . . ? C82 C81 C80 120.8(5) . . ? C82 C81 H87 119.6 . . ? C80 C81 H87 119.6 . . ? C77 C82 C81 123.0(4) . . ? C77 C82 H88 118.5 . . ? C81 C82 H88 118.5 . . ? C84 C83 H89 109.5 . . ? C84 C83 H90 109.5 . . ? H89 C83 H90 109.5 . . ? C84 C83 H91 109.5 . . ? H89 C83 H91 109.5 . . ? H90 C83 H91 109.5 . . ? C89 C84 C85 117.2(3) . . ? C89 C84 C83 121.4(3) . . ? C85 C84 C83 121.4(3) . . ? C86 C85 C84 121.6(3) . . ? C86 C85 H92 119.2 . . ? C84 C85 H92 119.2 . . ? C87 C86 C85 120.6(3) . . ? C87 C86 H93 119.7 . . ? C85 C86 H93 119.7 . . ? C86 C87 C88 118.4(3) . . ? C86 C87 H94 120.8 . . ? C88 C87 H94 120.8 . . ? C87 C88 C89 120.6(3) . . ? C87 C88 H95 119.7 . . ? C89 C88 H95 119.7 . . ? C84 C89 C88 121.6(3) . . ? C84 C89 H96 119.2 . . ? C88 C89 H96 119.2 . . ? C91 C90 H97 109.5 . . ? C91 C90 H98 109.5 . . ? H97 C90 H98 109.5 . . ? C91 C90 H99 109.5 . . ? H97 C90 H99 109.5 . . ? H98 C90 H99 109.5 . . ? C96 C91 C92 121.7(5) . . ? C96 C91 C90 117.3(5) . . ? C92 C91 C90 121.0(5) . . ? C93 C92 C91 121.1(6) . . ? C93 C92 H100 119.4 . . ? C91 C92 H100 119.4 . . ? C92 C93 C94 120.0(5) . . ? C92 C93 H101 120.0 . . ? C94 C93 H101 120.0 . . ? C93 C94 C95 119.1(5) . . ? C93 C94 H102 120.5 . . ? C95 C94 H102 120.5 . . ? C94 C95 C96 119.7(6) . . ? C94 C95 H103 120.1 . . ? C96 C95 H103 120.1 . . ? C98 C96 C91 75.1(6) . . ? C98 C96 C95 43.6(5) . . ? C91 C96 C95 118.3(4) . . ? C98 C96 C102 115.7(8) . . ? C91 C96 C102 40.6(5) . . ? C95 C96 C102 158.8(6) . . ? C98 C96 H111 163.3 . . ? C91 C96 H111 120.8 . . ? C95 C96 H111 120.8 . . ? C102 C96 H111 80.3 . . ? C98 C96 H112 122.2 . . ? C91 C96 H112 162.7 . . ? C95 C96 H112 78.8 . . ? C102 C96 H112 122.2 . . ? H111 C96 H112 42.2 . . ? C98 C97 H104 109.5 . . ? C98 C97 H105 109.5 . . ? H104 C97 H105 109.5 . . ? C98 C97 H106 109.5 . . ? H104 C97 H106 109.5 . . ? H105 C97 H106 109.5 . . ? C96 C98 C99 126.3(10) . . ? C96 C98 C97 111.4(10) . . ? C99 C98 C97 122.2(11) . . ? C98 C99 C100 120.9(13) . . ? C98 C99 H107 119.6 . . ? C100 C99 H107 119.6 . . ? C101 C100 C99 117.7(13) . . ? C101 C100 H108 121.2 . . ? C99 C100 H108 121.2 . . ? C102 C101 C100 120.2(13) . . ? C102 C101 H109 119.9 . . ? C100 C101 H109 119.9 . . ? C101 C102 C96 119.2(13) . . ? C101 C102 H110 120.4 . . ? C96 C102 H110 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C1 C2 O1 -179.7(2) . . . . ? C10 C1 C2 O1 0.2(4) . . . . ? C4 C1 C2 N1 -0.3(2) . . . . ? C10 C1 C2 N1 179.6(2) . . . . ? O1 C2 N1 C3 -179.0(2) . . . . ? C1 C2 N1 C3 1.6(2) . . . . ? O1 C2 N1 C68 -3.6(3) . . . . ? C1 C2 N1 C68 176.89(18) . . . . ? C2 N1 C3 O2 176.5(2) . . . . ? C68 N1 C3 O2 1.1(3) . . . . ? C2 N1 C3 C4 -2.2(2) . . . . ? C68 N1 C3 C4 -177.56(18) . . . . ? C10 C1 C4 C5 -0.5(3) . . . . ? C2 C1 C4 C5 179.40(19) . . . . ? C10 C1 C4 C3 179.10(19) . . . . ? C2 C1 C4 C3 -1.0(2) . . . . ? O2 C3 C4 C5 2.9(4) . . . . ? N1 C3 C4 C5 -178.5(2) . . . . ? O2 C3 C4 C1 -176.7(2) . . . . ? N1 C3 C4 C1 1.9(2) . . . . ? C1 C4 C5 C6 0.2(3) . . . . ? C3 C4 C5 C6 -179.3(2) . . . . ? C4 C5 C6 C9 -0.3(3) . . . . ? C4 C5 C6 C7 177.8(2) . . . . ? C5 C6 C7 O3 -0.8(4) . . . . ? C9 C6 C7 O3 177.5(2) . . . . ? C5 C6 C7 N2 179.8(2) . . . . ? C9 C6 C7 N2 -1.9(2) . . . . ? O3 C7 N2 C8 -178.6(2) . . . . ? C6 C7 N2 C8 0.8(2) . . . . ? O3 C7 N2 C11 -1.6(3) . . . . ? C6 C7 N2 C11 177.82(18) . . . . ? C7 N2 C8 O4 -179.0(2) . . . . ? C11 N2 C8 O4 4.0(3) . . . . ? C7 N2 C8 C9 0.6(2) . . . . ? C11 N2 C8 C9 -176.44(18) . . . . ? C5 C6 C9 C10 0.6(3) . . . . ? C7 C6 C9 C10 -177.81(19) . . . . ? C5 C6 C9 C8 -179.36(19) . . . . ? C7 C6 C9 C8 2.2(2) . . . . ? O4 C8 C9 C6 177.8(2) . . . . ? N2 C8 C9 C6 -1.8(2) . . . . ? O4 C8 C9 C10 -2.1(4) . . . . ? N2 C8 C9 C10 178.3(2) . . . . ? C4 C1 C10 C9 0.8(3) . . . . ? C2 C1 C10 C9 -179.1(2) . . . . ? C6 C9 C10 C1 -0.8(3) . . . . ? C8 C9 C10 C1 179.1(2) . . . . ? C7 N2 C11 C12 86.1(3) . . . . ? C8 N2 C11 C12 -97.2(2) . . . . ? N2 C11 C12 C13 -0.6(3) . . . . ? N2 C11 C12 C21 -179.86(19) . . . . ? C21 C12 C13 C14 -0.5(3) . . . . ? C11 C12 C13 C14 -179.7(2) . . . . ? C12 C13 C14 C15 176.9(2) . . . . ? C12 C13 C14 C19 -2.2(3) . . . . ? C13 C14 C15 C16 179.8(2) . . . . ? C19 C14 C15 C16 -1.1(3) . . . . ? C14 C15 C16 C17 -1.8(3) . . . . ? C14 C15 C16 C34 177.2(2) . . . . ? C15 C16 C17 O6 -176.97(19) . . . . ? C34 C16 C17 O6 4.0(3) . . . . ? C15 C16 C17 C18 2.9(3) . . . . ? C34 C16 C17 C18 -176.2(2) . . . . ? O6 C17 C18 C19 178.9(2) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C17 C18 C19 C20 178.0(2) . . . . ? C17 C18 C19 C14 -2.0(3) . . . . ? C15 C14 C19 C18 3.0(3) . . . . ? C13 C14 C19 C18 -177.9(2) . . . . ? C15 C14 C19 C20 -177.0(2) . . . . ? C13 C14 C19 C20 2.1(3) . . . . ? C18 C19 C20 C21 -179.5(2) . . . . ? C14 C19 C20 C21 0.6(3) . . . . ? C19 C20 C21 O5 177.2(2) . . . . ? C19 C20 C21 C12 -3.3(3) . . . . ? C13 C12 C21 O5 -177.16(19) . . . . ? C11 C12 C21 O5 2.1(3) . . . . ? C13 C12 C21 C20 3.3(3) . . . . ? C11 C12 C21 C20 -177.4(2) . . . . ? C20 C21 O5 C22 -1.8(3) . . . . ? C12 C21 O5 C22 178.64(19) . . . . ? C21 O5 C22 C23 179.32(19) . . . . ? O5 C22 C23 C24 69.3(3) . . . . ? C22 C23 C24 C25 -177.4(2) . . . . ? C23 C24 C25 C26 64.1(3) . . . . ? C24 C25 C26 C27 60.2(4) . . . . ? C18 C17 O6 C28 -4.2(3) . . . . ? C16 C17 O6 C28 175.62(18) . . . . ? C17 O6 C28 C29 -175.42(18) . . . . ? O6 C28 C29 C30 -177.94(18) . . . . ? C28 C29 C30 C31 -178.1(2) . . . . ? C29 C30 C31 C32 177.3(2) . . . . ? C30 C31 C32 C33 -179.5(2) . . . . ? C15 C16 C34 N3 3.8(3) . . . . ? C17 C16 C34 N3 -177.14(19) . . . . ? C16 C34 N3 C44 -95.5(2) . . . . ? C16 C34 N3 C35 88.7(2) . . . . ? C44 N3 C35 O7 -176.8(2) . . . . ? C34 N3 C35 O7 -0.6(4) . . . . ? C44 N3 C35 C36 1.9(2) . . . . ? C34 N3 C35 C36 178.09(18) . . . . ? O7 C35 C36 C37 -1.4(4) . . . . ? N3 C35 C36 C37 179.9(2) . . . . ? O7 C35 C36 C43 176.7(2) . . . . ? N3 C35 C36 C43 -2.0(2) . . . . ? C43 C36 C37 C38 -0.4(3) . . . . ? C35 C36 C37 C38 177.4(2) . . . . ? C36 C37 C38 C41 0.6(3) . . . . ? C36 C37 C38 C39 -177.7(2) . . . . ? C37 C38 C39 O8 -0.5(4) . . . . ? C41 C38 C39 O8 -178.9(2) . . . . ? C37 C38 C39 N4 178.4(2) . . . . ? C41 C38 C39 N4 0.0(2) . . . . ? O8 C39 N4 C40 -179.1(2) . . . . ? C38 C39 N4 C40 1.9(2) . . . . ? O8 C39 N4 C45 0.1(3) . . . . ? C38 C39 N4 C45 -178.92(18) . . . . ? C39 N4 C40 O9 176.1(2) . . . . ? C45 N4 C40 O9 -3.1(3) . . . . ? C39 N4 C40 C41 -2.9(2) . . . . ? C45 N4 C40 C41 177.93(18) . . . . ? C37 C38 C41 C42 -0.7(3) . . . . ? C39 C38 C41 C42 177.89(19) . . . . ? C37 C38 C41 C40 179.72(19) . . . . ? C39 C38 C41 C40 -1.7(2) . . . . ? O9 C40 C41 C38 -176.1(2) . . . . ? N4 C40 C41 C38 2.8(2) . . . . ? O9 C40 C41 C42 4.3(4) . . . . ? N4 C40 C41 C42 -176.7(2) . . . . ? C38 C41 C42 C43 0.6(3) . . . . ? C40 C41 C42 C43 -180.0(2) . . . . ? C37 C36 C43 C42 0.4(3) . . . . ? C35 C36 C43 C42 -177.82(19) . . . . ? C37 C36 C43 C44 179.6(2) . . . . ? C35 C36 C43 C44 1.4(2) . . . . ? C41 C42 C43 C36 -0.4(3) . . . . ? C41 C42 C43 C44 -179.4(2) . . . . ? C35 N3 C44 O10 179.2(2) . . . . ? C34 N3 C44 O10 3.0(3) . . . . ? C35 N3 C44 C43 -1.0(2) . . . . ? C34 N3 C44 C43 -177.18(18) . . . . ? C36 C43 C44 O10 179.5(2) . . . . ? C42 C43 C44 O10 -1.4(4) . . . . ? C36 C43 C44 N3 -0.3(2) . . . . ? C42 C43 C44 N3 178.8(2) . . . . ? C40 N4 C45 C46 88.4(3) . . . . ? C39 N4 C45 C46 -90.7(3) . . . . ? N4 C45 C46 C47 -0.5(3) . . . . ? N4 C45 C46 C55 178.74(19) . . . . ? C55 C46 C47 C48 1.1(3) . . . . ? C45 C46 C47 C48 -179.7(2) . . . . ? C46 C47 C48 C49 -179.1(2) . . . . ? C46 C47 C48 C53 0.3(3) . . . . ? C47 C48 C49 C50 -178.7(2) . . . . ? C53 C48 C49 C50 1.9(3) . . . . ? C48 C49 C50 C51 1.0(3) . . . . ? C48 C49 C50 C68 -178.9(2) . . . . ? C49 C50 C51 O12 176.76(19) . . . . ? C68 C50 C51 O12 -3.4(3) . . . . ? C49 C50 C51 C52 -2.6(3) . . . . ? C68 C50 C51 C52 177.3(2) . . . . ? O12 C51 C52 C53 -178.1(2) . . . . ? C50 C51 C52 C53 1.2(3) . . . . ? C51 C52 C53 C54 -180.0(2) . . . . ? C51 C52 C53 C48 1.8(3) . . . . ? C47 C48 C53 C52 177.3(2) . . . . ? C49 C48 C53 C52 -3.3(3) . . . . ? C47 C48 C53 C54 -1.1(3) . . . . ? C49 C48 C53 C54 178.4(2) . . . . ? C52 C53 C54 C55 -177.9(2) . . . . ? C48 C53 C54 C55 0.3(3) . . . . ? C53 C54 C55 O11 -179.7(2) . . . . ? C53 C54 C55 C46 1.1(3) . . . . ? C47 C46 C55 O11 178.88(19) . . . . ? C45 C46 C55 O11 -0.4(3) . . . . ? C47 C46 C55 C54 -1.9(3) . . . . ? C45 C46 C55 C54 178.9(2) . . . . ? C54 C55 O11 C56 10.9(3) . . . . ? C46 C55 O11 C56 -169.87(18) . . . . ? C55 O11 C56 C57 -179.53(19) . . . . ? O11 C56 C57 C58 -50.4(3) . . . . ? C56 C57 C58 C59 98.2(3) . . . . ? C57 C58 C59 C60 -175.8(2) . . . . ? C58 C59 C60 C61 -65.9(3) . . . . ? C52 C51 O12 C62 4.2(3) . . . . ? C50 C51 O12 C62 -175.17(18) . . . . ? C51 O12 C62 C63 176.13(18) . . . . ? O12 C62 C63 C64 175.70(18) . . . . ? C62 C63 C64 C65 178.86(19) . . . . ? C63 C64 C65 C66 176.0(2) . . . . ? C64 C65 C66 C67 -178.3(2) . . . . ? C3 N1 C68 C50 -85.9(3) . . . . ? C2 N1 C68 C50 99.3(2) . . . . ? C49 C50 C68 N1 0.8(3) . . . . ? C51 C50 C68 N1 -179.05(19) . . . . ? C75 C70 C71 C72 -0.5(5) . . . . ? C69 C70 C71 C72 179.3(3) . . . . ? C70 C71 C72 C73 -2.2(6) . . . . ? C71 C72 C73 C74 3.2(6) . . . . ? C72 C73 C74 C75 -1.6(5) . . . . ? C71 C70 C75 C74 2.0(5) . . . . ? C69 C70 C75 C74 -177.8(3) . . . . ? C73 C74 C75 C70 -0.9(5) . . . . ? C82 C77 C78 C79 -2.4(5) . . . . ? C76 C77 C78 C79 177.7(4) . . . . ? C77 C78 C79 C80 1.7(6) . . . . ? C78 C79 C80 C81 -0.2(7) . . . . ? C79 C80 C81 C82 -0.5(7) . . . . ? C78 C77 C82 C81 1.8(6) . . . . ? C76 C77 C82 C81 -178.4(4) . . . . ? C80 C81 C82 C77 -0.3(7) . . . . ? C89 C84 C85 C86 0.4(4) . . . . ? C83 C84 C85 C86 179.2(3) . . . . ? C84 C85 C86 C87 0.1(4) . . . . ? C85 C86 C87 C88 0.1(4) . . . . ? C86 C87 C88 C89 -0.7(4) . . . . ? C85 C84 C89 C88 -1.0(4) . . . . ? C83 C84 C89 C88 -179.8(3) . . . . ? C87 C88 C89 C84 1.2(4) . . . . ? C96 C91 C92 C93 -1.3(8) . . . . ? C90 C91 C92 C93 178.3(6) . . . . ? C91 C92 C93 C94 -0.2(9) . . . . ? C92 C93 C94 C95 0.0(8) . . . . ? C93 C94 C95 C96 1.6(7) . . . . ? C92 C91 C96 C98 8.4(7) . . . . ? C90 C91 C96 C98 -171.2(6) . . . . ? C92 C91 C96 C95 2.8(6) . . . . ? C90 C91 C96 C95 -176.8(5) . . . . ? C92 C91 C96 C102 -174.1(9) . . . . ? C90 C91 C96 C102 6.3(8) . . . . ? C94 C95 C96 C98 -10.8(7) . . . . ? C94 C95 C96 C91 -3.0(7) . . . . ? C94 C95 C96 C102 2.7(17) . . . . ? C91 C96 C98 C99 0.9(10) . . . . ? C95 C96 C98 C99 173.7(15) . . . . ? C102 C96 C98 C99 -0.9(14) . . . . ? C91 C96 C98 C97 -177.1(9) . . . . ? C95 C96 C98 C97 -4.3(8) . . . . ? C102 C96 C98 C97 -178.9(8) . . . . ? C96 C98 C99 C100 2.1(19) . . . . ? C97 C98 C99 C100 180.0(12) . . . . ? C98 C99 C100 C101 -3(2) . . . . ? C99 C100 C101 C102 2.1(19) . . . . ? C100 C101 C102 C96 -0.9(16) . . . . ? C98 C96 C102 C101 0.3(12) . . . . ? C91 C96 C102 C101 -2.4(7) . . . . ? C95 C96 C102 C101 -10(2) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.453 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.061 # Attachment 'CCDC658508.cif' data_aniline _database_code_depnum_ccdc_archive 'CCDC 658508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H120 N11 O12' _chemical_formula_weight 1788.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.817(2) _cell_length_b 14.977(3) _cell_length_c 15.724(2) _cell_angle_alpha 100.720(6) _cell_angle_beta 91.127(8) _cell_angle_gamma 102.965(8) _cell_volume 2434.1(7) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 953 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9611 _exptl_absorpt_correction_T_max 0.9944 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-HR' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37658 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11172 _reflns_number_gt 8638 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.0228P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11125 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.27745(13) 1.09710(10) 0.54486(10) 0.0266(3) Uani 1 1 d . . . C2 C -0.34081(14) 1.04523(11) 0.61034(10) 0.0282(3) Uani 1 1 d . . . O1 O -0.41491(11) 0.96969(8) 0.59888(8) 0.0363(3) Uani 1 1 d . . . N1 N -0.29418(12) 1.10048(9) 0.69146(8) 0.0284(3) Uani 1 1 d . . . C3 C -0.34240(15) 1.08328(12) 0.77413(10) 0.0316(3) Uani 1 1 d . . . H1 H -0.4314 1.0464 0.7640 0.038 Uiso 1 1 calc R . . H2 H -0.3427 1.1439 0.8121 0.038 Uiso 1 1 calc R . . C4 C -0.20052(14) 1.17857(11) 0.68398(10) 0.0274(3) Uani 1 1 d . . . O2 O -0.14097(11) 1.23505(8) 0.74465(7) 0.0352(3) Uani 1 1 d . . . C5 C -0.19077(14) 1.17645(10) 0.58929(9) 0.0263(3) Uani 1 1 d . . . C6 C -0.11517(14) 1.24006(10) 0.54743(10) 0.0270(3) Uani 1 1 d . . . H3 H -0.0547 1.2932 0.5777 0.032 Uiso 1 1 calc R . . C7 C -0.13451(14) 1.22020(10) 0.45798(9) 0.0263(3) Uani 1 1 d . . . C8 C -0.06976(15) 1.27122(10) 0.39219(9) 0.0280(3) Uani 1 1 d . . . O3 O 0.01749(11) 1.33968(8) 0.40331(7) 0.0361(3) Uani 1 1 d . . . N2 N -0.12783(13) 1.22293(9) 0.31204(8) 0.0296(3) Uani 1 1 d . . . C9 C -0.22190(15) 1.14394(11) 0.31945(10) 0.0290(3) Uani 1 1 d . . . O4 O -0.28513(11) 1.09010(8) 0.25899(7) 0.0367(3) Uani 1 1 d . . . C10 C -0.22414(14) 1.14234(10) 0.41380(10) 0.0270(3) Uani 1 1 d . . . C11 C -0.29748(14) 1.07744(10) 0.45534(10) 0.0281(3) Uani 1 1 d . . . H4 H -0.3569 1.0237 0.4249 0.034 Uiso 1 1 calc R . . C12 C -0.08960(16) 1.24532(11) 0.22884(10) 0.0323(3) Uani 1 1 d . . . H5 H -0.0400 1.3109 0.2382 0.039 Uiso 1 1 calc R . . H6 H -0.1666 1.2401 0.1915 0.039 Uiso 1 1 calc R . . C13 C -0.01069(14) 1.18219(10) 0.18256(9) 0.0269(3) Uani 1 1 d . A . C14 C 0.00913(14) 1.18369(10) 0.09363(9) 0.0275(3) Uani 1 1 d . . . C15 C 0.07957(14) 1.12824(10) 0.04710(9) 0.0264(3) Uani 1 1 d . A . H7 H 0.0892 1.1284 -0.0128 0.032 Uiso 1 1 calc R . . C16 C 0.13807(13) 1.07061(10) 0.08902(9) 0.0245(3) Uani 1 1 d . . . C17 C 0.21644(13) 1.01502(10) 0.04467(9) 0.0262(3) Uani 1 1 d . A . H8 H 0.2249 1.0115 -0.0158 0.031 Uiso 1 1 calc R . . C18 C 0.27988(13) 0.96639(10) 0.08925(10) 0.0260(3) Uani 1 1 d . . . C19 C 0.26600(14) 0.96822(10) 0.17937(10) 0.0267(3) Uani 1 1 d . . . C20 C 0.18759(14) 1.01896(10) 0.22150(10) 0.0279(3) Uani 1 1 d . . . H9 H 0.1764 1.0192 0.2813 0.034 Uiso 1 1 calc R A . C21 C 0.12250(14) 1.07133(10) 0.17820(9) 0.0257(3) Uani 1 1 d . A . C22 C 0.04531(14) 1.12710(10) 0.22287(10) 0.0281(3) Uani 1 1 d . . . H10 H 0.0323 1.1260 0.2823 0.034 Uiso 1 1 calc R A . O5 O -0.0412(3) 1.2488(2) 0.0635(2) 0.0301(6) Uani 0.753(4) 1 d P A 1 C23 C -0.0182(4) 1.2648(3) -0.0229(2) 0.0316(7) Uani 0.753(4) 1 d P A 1 H11 H -0.0641 1.2101 -0.0664 0.038 Uiso 0.753(4) 1 calc PR A 1 H12 H 0.0738 1.2753 -0.0322 0.038 Uiso 0.753(4) 1 calc PR A 1 C24 C -0.0656(2) 1.34991(16) -0.03136(15) 0.0387(6) Uani 0.753(4) 1 d P A 1 H13 H -0.0460 1.3650 -0.0890 0.046 Uiso 0.753(4) 1 calc PR A 1 H14 H -0.0188 1.4033 0.0130 0.046 Uiso 0.753(4) 1 calc PR A 1 C25 C -0.2064(3) 1.33917(19) -0.0212(2) 0.0515(7) Uani 0.753(4) 1 d P A 1 H15 H -0.2293 1.3089 0.0290 0.062 Uiso 0.753(4) 1 calc PR A 1 H16 H -0.2530 1.2968 -0.0735 0.062 Uiso 0.753(4) 1 calc PR A 1 C26 C -0.2524(5) 1.4326(3) -0.0076(3) 0.0817(13) Uani 0.753(4) 1 d P A 1 H17 H -0.3389 1.4223 0.0138 0.098 Uiso 0.753(4) 1 calc PR A 1 H18 H -0.1947 1.4807 0.0362 0.098 Uiso 0.753(4) 1 calc PR A 1 C27 C -0.2534(4) 1.4648(2) -0.0903(2) 0.0719(10) Uani 0.753(4) 1 d P A 1 H19 H -0.2986 1.4127 -0.1366 0.086 Uiso 0.753(4) 1 calc PR A 1 H20 H -0.1651 1.4856 -0.1066 0.086 Uiso 0.753(4) 1 calc PR A 1 C28 C -0.3209(6) 1.5467(4) -0.0811(4) 0.117(2) Uani 0.753(4) 1 d P A 1 H21 H -0.3199 1.5691 -0.1359 0.176 Uiso 0.753(4) 1 calc PR A 1 H22 H -0.2764 1.5977 -0.0347 0.176 Uiso 0.753(4) 1 calc PR A 1 H23 H -0.4090 1.5252 -0.0669 0.176 Uiso 0.753(4) 1 calc PR A 1 O6 O -0.0675(10) 1.2319(8) 0.0603(9) 0.026(2) Uiso 0.247(4) 1 d P A 2 C29 C -0.0505(10) 1.2465(8) -0.0264(8) 0.029(3) Uiso 0.247(4) 1 d P A 2 H24 H -0.0668 1.1859 -0.0677 0.034 Uiso 0.247(4) 1 calc PR A 2 H25 H 0.0375 1.2812 -0.0316 0.034 Uiso 0.247(4) 1 calc PR A 2 C30 C -0.1443(7) 1.3023(5) -0.0458(4) 0.0340(17) Uiso 0.247(4) 1 d P A 2 H26 H -0.2313 1.2667 -0.0392 0.041 Uiso 0.247(4) 1 calc PR A 2 H27 H -0.1391 1.3100 -0.1069 0.041 Uiso 0.247(4) 1 calc PR A 2 C31 C -0.1219(8) 1.3990(6) 0.0129(6) 0.050(2) Uiso 0.247(4) 1 d P A 2 H28 H -0.0335 1.4358 0.0137 0.060 Uiso 0.247(4) 1 calc PR A 2 H29 H -0.1464 1.3961 0.0729 0.060 Uiso 0.247(4) 1 calc PR A 2 C32 C -0.2253(11) 1.4368(8) -0.0442(8) 0.055(3) Uiso 0.247(4) 1 d P A 2 H30 H -0.1787 1.5010 -0.0470 0.066 Uiso 0.247(4) 1 calc PR A 2 H31 H -0.2253 1.4000 -0.1035 0.066 Uiso 0.247(4) 1 calc PR A 2 C33 C -0.3566(10) 1.4453(7) -0.0386(7) 0.067(3) Uiso 0.247(4) 1 d P A 2 H32 H -0.3847 1.4332 0.0185 0.081 Uiso 0.247(4) 1 calc PR A 2 H33 H -0.4096 1.3954 -0.0835 0.081 Uiso 0.247(4) 1 calc PR A 2 C34 C -0.3832(14) 1.5379(10) -0.0495(10) 0.081(4) Uiso 0.247(4) 1 d P A 2 H34 H -0.4750 1.5334 -0.0499 0.121 Uiso 0.247(4) 1 calc PR A 2 H35 H -0.3517 1.5529 -0.1044 0.121 Uiso 0.247(4) 1 calc PR A 2 H36 H -0.3402 1.5871 -0.0013 0.121 Uiso 0.247(4) 1 calc PR A 2 O7 O 0.36150(10) 0.91403(8) 0.05413(7) 0.0303(2) Uani 1 1 d . A . C35 C 0.37109(15) 0.89870(11) -0.03844(10) 0.0295(3) Uani 1 1 d . . . H37 H 0.4042 0.9588 -0.0570 0.035 Uiso 1 1 calc R A . H38 H 0.2865 0.8693 -0.0686 0.035 Uiso 1 1 calc R . . C36 C 0.46109(15) 0.83491(11) -0.06016(10) 0.0300(3) Uani 1 1 d . A . H39 H 0.4274 0.7758 -0.0400 0.036 Uiso 1 1 calc R . . H40 H 0.5446 0.8649 -0.0286 0.036 Uiso 1 1 calc R . . C37 C 0.47954(15) 0.81285(11) -0.15708(10) 0.0322(3) Uani 1 1 d . . . H41 H 0.3963 0.7818 -0.1885 0.039 Uiso 1 1 calc R A . H42 H 0.5116 0.8720 -0.1774 0.039 Uiso 1 1 calc R . . C38 C 0.57181(16) 0.75028(12) -0.17901(12) 0.0375(4) Uani 1 1 d . A . H43 H 0.5395 0.6910 -0.1589 0.045 Uiso 1 1 calc R . . H44 H 0.6548 0.7812 -0.1473 0.045 Uiso 1 1 calc R . . C39 C 0.5914(2) 0.72838(16) -0.27538(14) 0.0589(6) Uani 1 1 d . . . H45 H 0.6262 0.7874 -0.2953 0.071 Uiso 1 1 calc R A . H46 H 0.5082 0.6989 -0.3074 0.071 Uiso 1 1 calc R . . C40 C 0.6814(3) 0.6634(2) -0.2965(2) 0.0938(11) Uani 1 1 d . A . H47 H 0.7628 0.6911 -0.2632 0.141 Uiso 1 1 calc R . . H48 H 0.6951 0.6544 -0.3587 0.141 Uiso 1 1 calc R . . H49 H 0.6440 0.6029 -0.2814 0.141 Uiso 1 1 calc R . . N3 N -0.1650(3) 0.8519(3) 0.4140(2) 0.0397(7) Uani 0.50 1 d P B 1 H50 H -0.164(4) 0.848(3) 0.372(3) 0.030(12) Uiso 0.50 1 d P . . H51 H -0.182(4) 0.806(3) 0.431(3) 0.038(12) Uiso 0.50 1 d P . . C41 C -0.08551(18) 0.92126(14) 0.45242(14) 0.0454(5) Uani 1 1 d . . . C42 C -0.01851(19) 0.99046(14) 0.41112(13) 0.0466(5) Uani 1 1 d . . . H52 H -0.0310 0.9841 0.3501 0.056 Uiso 1 1 calc R . . C43 C -0.06566(19) 0.93205(14) 0.54186(14) 0.0476(5) Uani 1 1 d . . . H53 H -0.1105 0.8856 0.5708 0.057 Uiso 1 1 calc R . . N4 N -0.13825(18) 0.67241(13) 0.20456(14) 0.0570(5) Uani 1 1 d . . . H54 H -0.053(3) 0.6975(18) 0.2312(17) 0.077(8) Uiso 1 1 d . . . H55 H -0.185(3) 0.617(2) 0.2219(19) 0.087(9) Uiso 1 1 d . . . C44 C -0.20599(17) 0.73751(13) 0.19148(12) 0.0391(4) Uani 1 1 d . . . C45 C -0.14434(17) 0.83071(12) 0.19536(11) 0.0361(4) Uani 1 1 d . . . H56 H -0.0553 0.8503 0.2092 0.043 Uiso 1 1 calc R . . C46 C -0.21156(18) 0.89484(13) 0.17919(11) 0.0389(4) Uani 1 1 d . . . H57 H -0.1683 0.9582 0.1826 0.047 Uiso 1 1 calc R . . C47 C -0.34092(18) 0.86776(14) 0.15809(12) 0.0433(4) Uani 1 1 d . . . H58 H -0.3869 0.9121 0.1473 0.052 Uiso 1 1 calc R . . C48 C -0.40216(18) 0.77569(15) 0.15291(14) 0.0489(5) Uani 1 1 d . . . H59 H -0.4908 0.7563 0.1374 0.059 Uiso 1 1 calc R . . C49 C -0.33670(18) 0.71084(14) 0.16990(14) 0.0488(5) Uani 1 1 d . . . H60 H -0.3809 0.6478 0.1669 0.059 Uiso 1 1 calc R . . N5 N -0.46653(18) 0.82679(12) 0.38994(17) 0.0555(5) Uani 1 1 d . . . H61 H -0.401(3) 0.857(2) 0.437(2) 0.098(10) Uiso 1 1 d . . . H62 H -0.433(3) 0.826(2) 0.335(2) 0.083(9) Uiso 1 1 d . . . C50 C -0.54545(17) 0.74351(12) 0.40265(13) 0.0425(4) Uani 1 1 d . . . C51 C -0.5588(2) 0.72376(14) 0.48597(14) 0.0499(5) Uani 1 1 d . . . H63 H -0.5107 0.7659 0.5341 0.060 Uiso 1 1 calc R . . C52 C -0.6419(2) 0.64308(14) 0.49850(14) 0.0530(5) Uani 1 1 d . . . H64 H -0.6500 0.6301 0.5553 0.064 Uiso 1 1 calc R . . C53 C -0.7135(2) 0.58096(14) 0.42908(15) 0.0526(5) Uani 1 1 d . . . H65 H -0.7705 0.5257 0.4379 0.063 Uiso 1 1 calc R . . C54 C -0.70045(19) 0.60070(13) 0.34662(14) 0.0483(5) Uani 1 1 d . . . H66 H -0.7491 0.5585 0.2987 0.058 Uiso 1 1 calc R . . C55 C -0.61760(18) 0.68090(13) 0.33323(13) 0.0426(4) Uani 1 1 d . . . H67 H -0.6098 0.6934 0.2763 0.051 Uiso 1 1 calc R . . N6 N -0.2568(3) 0.64995(17) 0.47170(16) 0.0526(7) Uani 0.787(5) 1 d P C 1 H68 H -0.337(3) 0.652(2) 0.487(2) 0.071(10) Uiso 0.787(5) 1 d P . . H69 H -0.191(4) 0.650(3) 0.520(3) 0.097(12) Uiso 0.787(5) 1 d P C 1 C56 C -0.2562(5) 0.5800(4) 0.3993(3) 0.0387(10) Uani 0.787(5) 1 d P C 1 C57 C -0.3574(4) 0.5500(3) 0.3393(4) 0.0522(9) Uani 0.787(5) 1 d P C 1 H70 H -0.4318 0.5732 0.3488 0.063 Uiso 0.787(5) 1 calc PR C 1 C58 C -0.3513(6) 0.4851(3) 0.2640(3) 0.0581(13) Uani 0.787(5) 1 d P C 1 H71 H -0.4208 0.4660 0.2216 0.070 Uiso 0.787(5) 1 calc PR C 1 C59 C -0.2448(7) 0.4484(2) 0.2503(3) 0.0588(10) Uani 0.787(5) 1 d P C 1 H72 H -0.2409 0.4042 0.1992 0.071 Uiso 0.787(5) 1 calc PR C 1 C60 C -0.1434(4) 0.4775(3) 0.3132(3) 0.0473(9) Uani 0.787(5) 1 d P C 1 H73 H -0.0698 0.4530 0.3050 0.057 Uiso 0.787(5) 1 calc PR C 1 C61 C -0.1502(4) 0.5420(4) 0.3871(3) 0.0351(9) Uani 0.787(5) 1 d P C 1 H74 H -0.0817 0.5605 0.4302 0.042 Uiso 0.787(5) 1 calc PR C 1 N7 N -0.0428(7) 0.5335(5) 0.4168(5) 0.047(2) Uani 0.213(5) 1 d P C 2 H75 H -0.0269 0.5720 0.4674 0.057 Uiso 0.213(5) 1 calc PR C 2 H76 H 0.0152 0.5045 0.3950 0.057 Uiso 0.213(5) 1 calc PR C 2 C62 C -0.1601(14) 0.5183(10) 0.3711(9) 0.041(5) Uani 0.213(5) 1 d PG C 2 C63 C -0.244(2) 0.5678(13) 0.4117(8) 0.051(7) Uani 0.213(5) 1 d PG C 2 H77 H -0.2217 0.6053 0.4680 0.061 Uiso 0.213(5) 1 calc PR C 2 C64 C -0.3607(19) 0.5625(14) 0.3700(13) 0.146(17) Uani 0.213(5) 1 d PG C 2 H78 H -0.4181 0.5964 0.3978 0.176 Uiso 0.213(5) 1 calc PR C 2 C65 C -0.3934(11) 0.5078(12) 0.2876(13) 0.073(6) Uani 0.213(5) 1 d PG C 2 H79 H -0.4732 0.5041 0.2591 0.087 Uiso 0.213(5) 1 calc PR C 2 C66 C -0.3094(15) 0.4583(7) 0.2470(7) 0.054(4) Uani 0.213(5) 1 d PG C 2 H80 H -0.3318 0.4208 0.1907 0.065 Uiso 0.213(5) 1 calc PR C 2 C67 C -0.1928(13) 0.4635(7) 0.2887(8) 0.040(3) Uani 0.213(5) 1 d PG C 2 H81 H -0.1354 0.4297 0.2609 0.048 Uiso 0.213(5) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0222(7) 0.0285(7) 0.0324(7) 0.0079(6) 0.0025(6) 0.0111(6) C2 0.0239(7) 0.0310(7) 0.0333(8) 0.0092(6) 0.0024(6) 0.0113(6) O1 0.0308(6) 0.0334(6) 0.0460(7) 0.0126(5) 0.0028(5) 0.0058(5) N1 0.0256(6) 0.0343(7) 0.0295(6) 0.0121(5) 0.0044(5) 0.0106(5) C3 0.0287(7) 0.0402(8) 0.0331(8) 0.0159(7) 0.0102(6) 0.0152(6) C4 0.0258(7) 0.0328(7) 0.0277(7) 0.0096(6) 0.0023(6) 0.0123(6) O2 0.0351(6) 0.0420(6) 0.0286(6) 0.0084(5) 0.0000(5) 0.0078(5) C5 0.0255(7) 0.0304(7) 0.0265(7) 0.0068(6) 0.0023(6) 0.0124(6) C6 0.0259(7) 0.0291(7) 0.0275(7) 0.0057(6) 0.0027(6) 0.0090(6) C7 0.0275(7) 0.0285(7) 0.0270(7) 0.0066(6) 0.0048(6) 0.0138(6) C8 0.0333(8) 0.0298(7) 0.0252(7) 0.0059(6) 0.0058(6) 0.0154(6) O3 0.0414(6) 0.0350(6) 0.0318(6) 0.0087(5) 0.0063(5) 0.0065(5) N2 0.0375(7) 0.0322(7) 0.0229(6) 0.0049(5) 0.0053(5) 0.0161(6) C9 0.0315(8) 0.0315(7) 0.0286(7) 0.0047(6) 0.0030(6) 0.0174(6) O4 0.0425(7) 0.0390(6) 0.0285(6) 0.0003(5) -0.0027(5) 0.0149(5) C10 0.0271(7) 0.0296(7) 0.0279(7) 0.0044(6) 0.0028(6) 0.0149(6) C11 0.0262(7) 0.0283(7) 0.0312(7) 0.0033(6) 0.0003(6) 0.0114(6) C12 0.0437(9) 0.0359(8) 0.0244(7) 0.0088(6) 0.0076(6) 0.0208(7) C13 0.0299(7) 0.0276(7) 0.0252(7) 0.0053(6) 0.0047(6) 0.0102(6) C14 0.0311(7) 0.0280(7) 0.0256(7) 0.0069(6) 0.0016(6) 0.0102(6) C15 0.0287(7) 0.0297(7) 0.0218(7) 0.0060(6) 0.0032(5) 0.0079(6) C16 0.0227(7) 0.0256(7) 0.0250(7) 0.0057(6) 0.0029(5) 0.0047(5) C17 0.0254(7) 0.0291(7) 0.0253(7) 0.0076(6) 0.0058(6) 0.0069(6) C18 0.0229(7) 0.0265(7) 0.0301(7) 0.0071(6) 0.0073(6) 0.0072(5) C19 0.0234(7) 0.0297(7) 0.0297(7) 0.0107(6) 0.0051(6) 0.0074(6) C20 0.0288(7) 0.0321(7) 0.0265(7) 0.0110(6) 0.0065(6) 0.0100(6) C21 0.0250(7) 0.0261(7) 0.0272(7) 0.0071(6) 0.0041(6) 0.0066(6) C22 0.0317(8) 0.0315(7) 0.0240(7) 0.0077(6) 0.0058(6) 0.0113(6) O5 0.0371(17) 0.0345(15) 0.0253(10) 0.0122(11) 0.0066(12) 0.0168(13) C23 0.0349(17) 0.0392(17) 0.0252(13) 0.0135(12) 0.0061(13) 0.0117(15) C24 0.0483(14) 0.0357(12) 0.0369(12) 0.0166(10) 0.0027(10) 0.0119(11) C25 0.0495(16) 0.0503(15) 0.0615(17) 0.0118(13) -0.0054(13) 0.0258(13) C26 0.094(3) 0.101(3) 0.079(3) 0.032(2) 0.016(2) 0.072(3) C27 0.089(3) 0.065(2) 0.069(2) 0.0203(17) -0.0174(18) 0.0286(18) C28 0.144(5) 0.110(4) 0.138(5) 0.063(3) -0.006(4) 0.080(4) O7 0.0303(5) 0.0370(6) 0.0292(5) 0.0100(5) 0.0095(4) 0.0160(5) C35 0.0303(8) 0.0331(8) 0.0281(7) 0.0074(6) 0.0079(6) 0.0120(6) C36 0.0284(7) 0.0315(7) 0.0333(8) 0.0089(6) 0.0076(6) 0.0109(6) C37 0.0316(8) 0.0327(8) 0.0337(8) 0.0065(7) 0.0080(6) 0.0099(6) C38 0.0281(8) 0.0340(8) 0.0461(10) -0.0031(7) 0.0064(7) 0.0071(6) C39 0.0585(13) 0.0534(12) 0.0544(12) -0.0090(10) 0.0254(10) 0.0052(10) C40 0.0697(17) 0.0808(18) 0.111(2) -0.0340(17) 0.0439(16) 0.0170(14) N3 0.0400(17) 0.048(2) 0.0299(17) 0.0091(16) 0.0009(14) 0.0064(14) C41 0.0439(10) 0.0467(10) 0.0586(12) 0.0204(9) 0.0200(9) 0.0275(9) C42 0.0500(11) 0.0516(11) 0.0512(11) 0.0209(9) 0.0199(9) 0.0282(9) C43 0.0503(11) 0.0499(11) 0.0582(12) 0.0268(10) 0.0244(9) 0.0288(9) N4 0.0390(9) 0.0477(10) 0.0916(15) 0.0293(10) -0.0015(9) 0.0127(8) C44 0.0363(9) 0.0424(9) 0.0428(9) 0.0136(8) 0.0034(7) 0.0132(7) C45 0.0366(9) 0.0416(9) 0.0308(8) 0.0068(7) 0.0032(7) 0.0106(7) C46 0.0493(10) 0.0388(9) 0.0317(8) 0.0065(7) 0.0088(7) 0.0161(8) C47 0.0473(10) 0.0526(11) 0.0399(9) 0.0170(8) 0.0095(8) 0.0253(9) C48 0.0356(9) 0.0612(12) 0.0559(12) 0.0204(10) 0.0019(8) 0.0164(9) C49 0.0390(10) 0.0466(10) 0.0635(13) 0.0191(10) 0.0010(9) 0.0088(8) N5 0.0448(10) 0.0408(9) 0.0822(14) 0.0141(9) -0.0078(10) 0.0118(7) C50 0.0371(9) 0.0334(8) 0.0608(12) 0.0069(8) -0.0034(8) 0.0180(7) C51 0.0555(12) 0.0421(10) 0.0551(12) 0.0012(9) -0.0111(9) 0.0259(9) C52 0.0700(14) 0.0446(10) 0.0526(12) 0.0115(9) 0.0052(10) 0.0281(10) C53 0.0612(13) 0.0366(9) 0.0636(13) 0.0105(9) 0.0097(10) 0.0180(9) C54 0.0503(11) 0.0377(9) 0.0563(12) -0.0001(9) 0.0002(9) 0.0168(8) C55 0.0433(10) 0.0398(9) 0.0490(10) 0.0065(8) 0.0045(8) 0.0200(8) N6 0.0545(15) 0.0551(14) 0.0535(14) 0.0098(11) 0.0070(11) 0.0239(11) C56 0.038(2) 0.0338(16) 0.0503(18) 0.0176(17) 0.0046(15) 0.0128(13) C57 0.0362(19) 0.041(2) 0.082(2) 0.0244(17) -0.0085(15) 0.0044(15) C58 0.061(3) 0.032(2) 0.076(3) 0.0149(19) -0.030(2) 0.0004(19) C59 0.089(4) 0.0286(14) 0.055(2) 0.0011(15) -0.024(2) 0.015(2) C60 0.064(3) 0.0304(16) 0.051(2) 0.0038(16) -0.0076(18) 0.0212(17) C61 0.0389(17) 0.026(2) 0.0426(15) 0.0086(16) -0.0001(12) 0.0099(14) N7 0.041(4) 0.037(4) 0.061(5) 0.004(3) -0.004(3) 0.007(3) C62 0.046(7) 0.016(8) 0.060(12) 0.002(7) -0.010(6) 0.008(5) C63 0.060(11) 0.041(9) 0.057(9) 0.022(6) -0.011(7) 0.014(6) C64 0.067(16) 0.067(13) 0.32(5) 0.03(2) 0.005(19) 0.039(11) C65 0.070(11) 0.046(9) 0.109(16) 0.030(10) 0.002(10) 0.017(8) C66 0.050(9) 0.024(6) 0.084(10) 0.004(6) -0.043(9) 0.013(5) C67 0.049(9) 0.036(6) 0.035(8) -0.004(6) -0.011(5) 0.021(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 C1 C11 1.386(2) . ? C1 C5 1.395(2) . ? C1 C2 1.490(2) . ? C2 O1 1.2110(19) . ? C2 N1 1.400(2) . ? N1 C4 1.390(2) . ? N1 C3 1.4557(19) . ? C3 C19 1.511(2) 2_576 ? C3 H1 0.9900 . ? C3 H2 0.9900 . ? C4 O2 1.2132(19) . ? C4 C5 1.490(2) . ? C5 C6 1.384(2) . ? C6 C7 1.384(2) . ? C6 H3 0.9500 . ? C7 C10 1.395(2) . ? C7 C8 1.492(2) . ? C8 O3 1.2105(19) . ? C8 N2 1.390(2) . ? N2 C9 1.402(2) . ? N2 C12 1.4551(19) . ? C9 O4 1.2099(19) . ? C9 C10 1.489(2) . ? C10 C11 1.383(2) . ? C11 H4 0.9500 . ? C12 C13 1.511(2) . ? C12 H5 0.9900 . ? C12 H6 0.9900 . ? C13 C22 1.361(2) . ? C13 C14 1.422(2) . ? C14 O5 1.368(4) . ? C14 O6 1.369(13) . ? C14 C15 1.373(2) . ? C15 C16 1.421(2) . ? C15 H7 0.9500 . ? C16 C21 1.414(2) . ? C16 C17 1.4220(19) . ? C17 C18 1.374(2) . ? C17 H8 0.9500 . ? C18 O7 1.3668(17) . ? C18 C19 1.424(2) . ? C19 C20 1.364(2) . ? C19 C3 1.511(2) 2_576 ? C20 C21 1.415(2) . ? C20 H9 0.9500 . ? C21 C22 1.416(2) . ? C22 H10 0.9500 . ? O5 C23 1.440(5) . ? C23 C24 1.503(4) . ? C23 H11 0.9900 . ? C23 H12 0.9900 . ? C24 C25 1.510(4) . ? C24 H13 0.9900 . ? C24 H14 0.9900 . ? C25 C26 1.567(4) . ? C25 H15 0.9900 . ? C25 H16 0.9900 . ? C26 C27 1.469(6) . ? C26 H17 0.9900 . ? C26 H18 0.9900 . ? C27 C28 1.550(5) . ? C27 H19 0.9900 . ? C27 H20 0.9900 . ? C28 H21 0.9800 . ? C28 H22 0.9800 . ? C28 H23 0.9800 . ? O6 C29 1.430(19) . ? C29 C30 1.512(14) . ? C29 H24 0.9900 . ? C29 H25 0.9900 . ? C30 C31 1.530(11) . ? C30 H26 0.9900 . ? C30 H27 0.9900 . ? C31 C32 1.678(15) . ? C31 H28 0.9900 . ? C31 H29 0.9900 . ? C32 C33 1.456(15) . ? C32 H30 0.9900 . ? C32 H31 0.9900 . ? C33 C34 1.517(17) . ? C33 H32 0.9900 . ? C33 H33 0.9900 . ? C34 H34 0.9800 . ? C34 H35 0.9800 . ? C34 H36 0.9800 . ? O7 C35 1.4404(18) . ? C35 C36 1.512(2) . ? C35 H37 0.9900 . ? C35 H38 0.9900 . ? C36 C37 1.525(2) . ? C36 H39 0.9900 . ? C36 H40 0.9900 . ? C37 C38 1.519(2) . ? C37 H41 0.9900 . ? C37 H42 0.9900 . ? C38 C39 1.519(3) . ? C38 H43 0.9900 . ? C38 H44 0.9900 . ? C39 C40 1.524(3) . ? C39 H45 0.9900 . ? C39 H46 0.9900 . ? C40 H47 0.9800 . ? C40 H48 0.9800 . ? C40 H49 0.9800 . ? N3 C41 1.237(4) . ? N3 H50 0.65(4) . ? N3 H51 0.77(4) . ? C41 C43 1.392(3) . ? C41 C42 1.397(3) . ? C42 C43 1.379(3) 2_576 ? C42 H52 0.9500 . ? C43 C42 1.379(3) 2_576 ? C43 H53 0.9500 . ? N4 C44 1.385(2) . ? N4 H54 0.97(3) . ? N4 H55 0.96(3) . ? C44 C45 1.395(2) . ? C44 C49 1.397(3) . ? C45 C46 1.383(2) . ? C45 H56 0.9500 . ? C46 C47 1.382(3) . ? C46 H57 0.9500 . ? C47 C48 1.376(3) . ? C47 H58 0.9500 . ? C48 C49 1.383(3) . ? C48 H59 0.9500 . ? C49 H60 0.9500 . ? N5 C50 1.395(3) . ? N5 H61 0.98(3) . ? N5 H62 0.93(3) . ? C50 C55 1.392(3) . ? C50 C51 1.399(3) . ? C51 C52 1.384(3) . ? C51 H63 0.9500 . ? C52 C53 1.386(3) . ? C52 H64 0.9500 . ? C53 C54 1.385(3) . ? C53 H65 0.9500 . ? C54 C55 1.382(3) . ? C54 H66 0.9500 . ? C55 H67 0.9500 . ? N6 C56 1.398(4) . ? N6 H68 0.91(4) . ? N6 H69 1.03(4) . ? C56 C57 1.368(7) . ? C56 C61 1.392(5) . ? C57 C58 1.398(7) . ? C57 H70 0.9500 . ? C58 C59 1.388(6) . ? C58 H71 0.9500 . ? C59 C60 1.397(5) . ? C59 H72 0.9500 . ? C60 C61 1.381(6) . ? C60 H73 0.9500 . ? C61 H74 0.9500 . ? N7 C62 1.397(13) . ? N7 H75 0.8800 . ? N7 H76 0.8800 . ? C62 C63 1.3900 . ? C62 C67 1.3900 . ? C63 C64 1.3900 . ? C63 H77 0.9500 . ? C64 C65 1.3900 . ? C64 H78 0.9500 . ? C65 C66 1.3900 . ? C65 H79 0.9500 . ? C66 C67 1.3900 . ? C66 H80 0.9500 . ? C67 H81 0.9500 . ? 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 C11 C1 C5 122.50(14) . . ? C11 C1 C2 129.63(14) . . ? C5 C1 C2 107.84(13) . . ? O1 C2 N1 125.12(14) . . ? O1 C2 C1 128.92(15) . . ? N1 C2 C1 105.93(13) . . ? C4 N1 C2 111.85(12) . . ? C4 N1 C3 123.03(13) . . ? C2 N1 C3 124.99(13) . . ? N1 C3 C19 113.68(12) . 2_576 ? N1 C3 H1 108.8 . . ? C19 C3 H1 108.8 2_576 . ? N1 C3 H2 108.8 . . ? C19 C3 H2 108.8 2_576 . ? H1 C3 H2 107.7 . . ? O2 C4 N1 124.77(14) . . ? O2 C4 C5 129.04(14) . . ? N1 C4 C5 106.19(12) . . ? C6 C5 C1 122.73(14) . . ? C6 C5 C4 129.27(14) . . ? C1 C5 C4 107.98(13) . . ? C5 C6 C7 114.81(14) . . ? C5 C6 H3 122.6 . . ? C7 C6 H3 122.6 . . ? C6 C7 C10 122.38(14) . . ? C6 C7 C8 129.79(14) . . ? C10 C7 C8 107.83(13) . . ? O3 C8 N2 125.11(14) . . ? O3 C8 C7 128.72(14) . . ? N2 C8 C7 106.15(13) . . ? C8 N2 C9 112.03(12) . . ? C8 N2 C12 124.92(14) . . ? C9 N2 C12 122.84(13) . . ? O4 C9 N2 124.66(14) . . ? O4 C9 C10 129.46(15) . . ? N2 C9 C10 105.88(13) . . ? C11 C10 C7 122.88(14) . . ? C11 C10 C9 129.05(14) . . ? C7 C10 C9 108.06(13) . . ? C10 C11 C1 114.66(14) . . ? C10 C11 H4 122.7 . . ? C1 C11 H4 122.7 . . ? N2 C12 C13 112.87(12) . . ? N2 C12 H5 109.0 . . ? C13 C12 H5 109.0 . . ? N2 C12 H6 109.0 . . ? C13 C12 H6 109.0 . . ? H5 C12 H6 107.8 . . ? C22 C13 C14 119.10(13) . . ? C22 C13 C12 123.00(13) . . ? C14 C13 C12 117.85(13) . . ? O5 C14 O6 14.0(5) . . ? O5 C14 C15 125.38(19) . . ? O6 C14 C15 126.3(6) . . ? O5 C14 C13 113.18(19) . . ? O6 C14 C13 111.4(6) . . ? C15 C14 C13 121.31(13) . . ? C14 C15 C16 119.66(13) . . ? C14 C15 H7 120.2 . . ? C16 C15 H7 120.2 . . ? C21 C16 C15 119.27(13) . . ? C21 C16 C17 118.85(13) . . ? C15 C16 C17 121.82(13) . . ? C18 C17 C16 120.03(13) . . ? C18 C17 H8 120.0 . . ? C16 C17 H8 120.0 . . ? O7 C18 C17 125.02(13) . . ? O7 C18 C19 113.79(12) . . ? C17 C18 C19 121.19(13) . . ? C20 C19 C18 118.94(13) . . ? C20 C19 C3 122.16(13) . 2_576 ? C18 C19 C3 118.86(13) . 2_576 ? C19 C20 C21 121.53(14) . . ? C19 C20 H9 119.2 . . ? C21 C20 H9 119.2 . . ? C16 C21 C20 119.41(13) . . ? C16 C21 C22 119.11(13) . . ? C20 C21 C22 121.45(13) . . ? C13 C22 C21 121.47(13) . . ? C13 C22 H10 119.3 . . ? C21 C22 H10 119.3 . . ? C14 O5 C23 119.6(3) . . ? O5 C23 C24 106.9(3) . . ? O5 C23 H11 110.3 . . ? C24 C23 H11 110.3 . . ? O5 C23 H12 110.3 . . ? C24 C23 H12 110.3 . . ? H11 C23 H12 108.6 . . ? C23 C24 C25 114.1(2) . . ? C23 C24 H13 108.7 . . ? C25 C24 H13 108.7 . . ? C23 C24 H14 108.7 . . ? C25 C24 H14 108.7 . . ? H13 C24 H14 107.6 . . ? C24 C25 C26 115.0(3) . . ? C24 C25 H15 108.5 . . ? C26 C25 H15 108.5 . . ? C24 C25 H16 108.5 . . ? C26 C25 H16 108.5 . . ? H15 C25 H16 107.5 . . ? C27 C26 C25 109.4(3) . . ? C27 C26 H17 109.8 . . ? C25 C26 H17 109.8 . . ? C27 C26 H18 109.8 . . ? C25 C26 H18 109.8 . . ? H17 C26 H18 108.2 . . ? C26 C27 C28 109.4(4) . . ? C26 C27 H19 109.8 . . ? C28 C27 H19 109.8 . . ? C26 C27 H20 109.8 . . ? C28 C27 H20 109.8 . . ? H19 C27 H20 108.2 . . ? C27 C28 H21 109.5 . . ? C27 C28 H22 109.5 . . ? H21 C28 H22 109.5 . . ? C27 C28 H23 109.5 . . ? H21 C28 H23 109.5 . . ? H22 C28 H23 109.5 . . ? C14 O6 C29 117.8(10) . . ? O6 C29 C30 106.8(10) . . ? O6 C29 H24 110.4 . . ? C30 C29 H24 110.4 . . ? O6 C29 H25 110.4 . . ? C30 C29 H25 110.4 . . ? H24 C29 H25 108.6 . . ? C29 C30 C31 113.6(7) . . ? C29 C30 H26 108.8 . . ? C31 C30 H26 108.8 . . ? C29 C30 H27 108.8 . . ? C31 C30 H27 108.8 . . ? H26 C30 H27 107.7 . . ? C30 C31 C32 94.9(7) . . ? C30 C31 H28 112.7 . . ? C32 C31 H28 112.7 . . ? C30 C31 H29 112.7 . . ? C32 C31 H29 112.7 . . ? H28 C31 H29 110.2 . . ? C33 C32 C31 136.8(10) . . ? C33 C32 H30 102.9 . . ? C31 C32 H30 102.9 . . ? C33 C32 H31 102.9 . . ? C31 C32 H31 102.9 . . ? H30 C32 H31 105.1 . . ? C32 C33 C34 116.8(10) . . ? C32 C33 H32 108.1 . . ? C34 C33 H32 108.1 . . ? C32 C33 H33 108.1 . . ? C34 C33 H33 108.1 . . ? H32 C33 H33 107.3 . . ? C33 C34 H34 109.5 . . ? C33 C34 H35 109.5 . . ? H34 C34 H35 109.5 . . ? C33 C34 H36 109.5 . . ? H34 C34 H36 109.5 . . ? H35 C34 H36 109.5 . . ? C18 O7 C35 118.18(11) . . ? O7 C35 C36 107.24(12) . . ? O7 C35 H37 110.3 . . ? C36 C35 H37 110.3 . . ? O7 C35 H38 110.3 . . ? C36 C35 H38 110.3 . . ? H37 C35 H38 108.5 . . ? C35 C36 C37 112.55(13) . . ? C35 C36 H39 109.1 . . ? C37 C36 H39 109.1 . . ? C35 C36 H40 109.1 . . ? C37 C36 H40 109.1 . . ? H39 C36 H40 107.8 . . ? C38 C37 C36 112.72(14) . . ? C38 C37 H41 109.0 . . ? C36 C37 H41 109.0 . . ? C38 C37 H42 109.0 . . ? C36 C37 H42 109.0 . . ? H41 C37 H42 107.8 . . ? C37 C38 C39 113.10(16) . . ? C37 C38 H43 109.0 . . ? C39 C38 H43 109.0 . . ? C37 C38 H44 109.0 . . ? C39 C38 H44 109.0 . . ? H43 C38 H44 107.8 . . ? C38 C39 C40 112.4(2) . . ? C38 C39 H45 109.1 . . ? C40 C39 H45 109.1 . . ? C38 C39 H46 109.1 . . ? C40 C39 H46 109.1 . . ? H45 C39 H46 107.9 . . ? C39 C40 H47 109.5 . . ? C39 C40 H48 109.5 . . ? H47 C40 H48 109.5 . . ? C39 C40 H49 109.5 . . ? H47 C40 H49 109.5 . . ? H48 C40 H49 109.5 . . ? C41 N3 H50 111(4) . . ? C41 N3 H51 122(3) . . ? H50 N3 H51 117(5) . . ? N3 C41 C43 117.9(3) . . ? N3 C41 C42 123.4(3) . . ? C43 C41 C42 118.7(2) . . ? C43 C42 C41 120.58(19) 2_576 . ? C43 C42 H52 119.7 2_576 . ? C41 C42 H52 119.7 . . ? C42 C43 C41 120.68(18) 2_576 . ? C42 C43 H53 119.7 2_576 . ? C41 C43 H53 119.7 . . ? C44 N4 H54 116.0(16) . . ? C44 N4 H55 117.1(17) . . ? H54 N4 H55 116(2) . . ? N4 C44 C45 120.79(17) . . ? N4 C44 C49 120.97(17) . . ? C45 C44 C49 118.17(16) . . ? C46 C45 C44 120.65(17) . . ? C46 C45 H56 119.7 . . ? C44 C45 H56 119.7 . . ? C47 C46 C45 120.71(17) . . ? C47 C46 H57 119.6 . . ? C45 C46 H57 119.6 . . ? C48 C47 C46 119.02(17) . . ? C48 C47 H58 120.5 . . ? C46 C47 H58 120.5 . . ? C47 C48 C49 121.04(18) . . ? C47 C48 H59 119.5 . . ? C49 C48 H59 119.5 . . ? C48 C49 C44 120.40(18) . . ? C48 C49 H60 119.8 . . ? C44 C49 H60 119.8 . . ? C50 N5 H61 114.6(18) . . ? C50 N5 H62 116.1(18) . . ? H61 N5 H62 112(3) . . ? C55 C50 N5 120.5(2) . . ? C55 C50 C51 118.76(18) . . ? N5 C50 C51 120.64(19) . . ? C52 C51 C50 120.27(19) . . ? C52 C51 H63 119.9 . . ? C50 C51 H63 119.9 . . ? C51 C52 C53 120.7(2) . . ? C51 C52 H64 119.6 . . ? C53 C52 H64 119.6 . . ? C54 C53 C52 119.0(2) . . ? C54 C53 H65 120.5 . . ? C52 C53 H65 120.5 . . ? C55 C54 C53 120.8(2) . . ? C55 C54 H66 119.6 . . ? C53 C54 H66 119.6 . . ? C54 C55 C50 120.42(19) . . ? C54 C55 H67 119.8 . . ? C50 C55 H67 119.8 . . ? C56 N6 H68 112(2) . . ? C56 N6 H69 112(2) . . ? H68 N6 H69 117(3) . . ? C57 C56 C61 119.6(4) . . ? C57 C56 N6 120.8(4) . . ? C61 C56 N6 119.6(4) . . ? C56 C57 C58 120.0(4) . . ? C56 C57 H70 120.0 . . ? C58 C57 H70 120.0 . . ? C59 C58 C57 120.7(4) . . ? C59 C58 H71 119.7 . . ? C57 C58 H71 119.7 . . ? C58 C59 C60 118.8(4) . . ? C58 C59 H72 120.6 . . ? C60 C59 H72 120.6 . . ? C61 C60 C59 120.0(4) . . ? C61 C60 H73 120.0 . . ? C59 C60 H73 120.0 . . ? C60 C61 C56 120.8(4) . . ? C60 C61 H74 119.6 . . ? C56 C61 H74 119.6 . . ? C62 N7 H75 120.0 . . ? C62 N7 H76 120.0 . . ? H75 N7 H76 120.0 . . ? C63 C62 C67 120.0 . . ? C63 C62 N7 114.9(13) . . ? C67 C62 N7 125.0(13) . . ? C64 C63 C62 120.0 . . ? C64 C63 H77 120.0 . . ? C62 C63 H77 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 H78 120.0 . . ? C65 C64 H78 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H79 120.0 . . ? C66 C65 H79 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 H80 120.0 . . ? C67 C66 H80 120.0 . . ? C66 C67 C62 120.0 . . ? C66 C67 H81 120.0 . . ? C62 C67 H81 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 C2 O1 8.0(3) . . . . ? C5 C1 C2 O1 -174.04(15) . . . . ? C11 C1 C2 N1 -173.96(14) . . . . ? C5 C1 C2 N1 4.00(15) . . . . ? O1 C2 N1 C4 173.54(14) . . . . ? C1 C2 N1 C4 -4.59(15) . . . . ? O1 C2 N1 C3 -10.5(2) . . . . ? C1 C2 N1 C3 171.41(12) . . . . ? C4 N1 C3 C19 -87.19(17) . . . 2_576 ? C2 N1 C3 C19 97.24(17) . . . 2_576 ? C2 N1 C4 O2 -176.43(14) . . . . ? C3 N1 C4 O2 7.5(2) . . . . ? C2 N1 C4 C5 3.38(15) . . . . ? C3 N1 C4 C5 -172.71(12) . . . . ? C11 C1 C5 C6 -2.1(2) . . . . ? C2 C1 C5 C6 179.71(13) . . . . ? C11 C1 C5 C4 176.10(13) . . . . ? C2 C1 C5 C4 -2.03(15) . . . . ? O2 C4 C5 C6 -2.8(3) . . . . ? N1 C4 C5 C6 177.41(14) . . . . ? O2 C4 C5 C1 179.11(15) . . . . ? N1 C4 C5 C1 -0.69(15) . . . . ? C1 C5 C6 C7 1.6(2) . . . . ? C4 C5 C6 C7 -176.24(13) . . . . ? C5 C6 C7 C10 0.5(2) . . . . ? C5 C6 C7 C8 -178.73(14) . . . . ? C6 C7 C8 O3 3.0(3) . . . . ? C10 C7 C8 O3 -176.33(15) . . . . ? C6 C7 C8 N2 -178.44(14) . . . . ? C10 C7 C8 N2 2.28(15) . . . . ? O3 C8 N2 C9 177.08(14) . . . . ? C7 C8 N2 C9 -1.59(15) . . . . ? O3 C8 N2 C12 2.3(2) . . . . ? C7 C8 N2 C12 -176.34(12) . . . . ? C8 N2 C9 O4 -179.31(14) . . . . ? C12 N2 C9 O4 -4.4(2) . . . . ? C8 N2 C9 C10 0.35(15) . . . . ? C12 N2 C9 C10 175.22(12) . . . . ? C6 C7 C10 C11 -2.2(2) . . . . ? C8 C7 C10 C11 177.16(13) . . . . ? C6 C7 C10 C9 178.57(13) . . . . ? C8 C7 C10 C9 -2.08(15) . . . . ? O4 C9 C10 C11 1.6(3) . . . . ? N2 C9 C10 C11 -178.04(14) . . . . ? O4 C9 C10 C7 -179.23(15) . . . . ? N2 C9 C10 C7 1.14(15) . . . . ? C7 C10 C11 C1 1.6(2) . . . . ? C9 C10 C11 C1 -179.27(13) . . . . ? C5 C1 C11 C10 0.4(2) . . . . ? C2 C1 C11 C10 178.13(13) . . . . ? C8 N2 C12 C13 100.72(17) . . . . ? C9 N2 C12 C13 -73.48(18) . . . . ? N2 C12 C13 C22 -15.7(2) . . . . ? N2 C12 C13 C14 166.75(14) . . . . ? C22 C13 C14 O5 -173.6(2) . . . . ? C12 C13 C14 O5 4.1(3) . . . . ? C22 C13 C14 O6 171.4(4) . . . . ? C12 C13 C14 O6 -10.9(5) . . . . ? C22 C13 C14 C15 2.4(2) . . . . ? C12 C13 C14 C15 -179.90(14) . . . . ? O5 C14 C15 C16 173.1(2) . . . . ? O6 C14 C15 C16 -169.7(5) . . . . ? C13 C14 C15 C16 -2.4(2) . . . . ? C14 C15 C16 C21 0.1(2) . . . . ? C14 C15 C16 C17 -177.23(14) . . . . ? C21 C16 C17 C18 -2.8(2) . . . . ? C15 C16 C17 C18 174.50(14) . . . . ? C16 C17 C18 O7 -177.20(13) . . . . ? C16 C17 C18 C19 1.8(2) . . . . ? O7 C18 C19 C20 179.48(13) . . . . ? C17 C18 C19 C20 0.3(2) . . . . ? O7 C18 C19 C3 1.7(2) . . . 2_576 ? C17 C18 C19 C3 -177.43(14) . . . 2_576 ? C18 C19 C20 C21 -1.5(2) . . . . ? C3 C19 C20 C21 176.17(14) 2_576 . . . ? C15 C16 C21 C20 -175.73(13) . . . . ? C17 C16 C21 C20 1.7(2) . . . . ? C15 C16 C21 C22 2.2(2) . . . . ? C17 C16 C21 C22 179.54(13) . . . . ? C19 C20 C21 C16 0.5(2) . . . . ? C19 C20 C21 C22 -177.31(14) . . . . ? C14 C13 C22 C21 -0.1(2) . . . . ? C12 C13 C22 C21 -177.65(14) . . . . ? C16 C21 C22 C13 -2.2(2) . . . . ? C20 C21 C22 C13 175.68(14) . . . . ? O6 C14 O5 C23 -100(3) . . . . ? C15 C14 O5 C23 -1.7(5) . . . . ? C13 C14 O5 C23 174.1(3) . . . . ? C14 O5 C23 C24 -170.6(3) . . . . ? O5 C23 C24 C25 -62.0(4) . . . . ? C23 C24 C25 C26 166.1(3) . . . . ? C24 C25 C26 C27 74.4(4) . . . . ? C25 C26 C27 C28 170.0(4) . . . . ? O5 C14 O6 C29 74(3) . . . . ? C15 C14 O6 C29 -17.0(10) . . . . ? C13 C14 O6 C29 174.6(7) . . . . ? C14 O6 C29 C30 -178.9(7) . . . . ? O6 C29 C30 C31 62.4(9) . . . . ? C29 C30 C31 C32 170.1(8) . . . . ? C30 C31 C32 C33 98.1(14) . . . . ? C31 C32 C33 C34 132.5(13) . . . . ? C17 C18 O7 C35 -8.0(2) . . . . ? C19 C18 O7 C35 172.94(13) . . . . ? C18 O7 C35 C36 -176.86(12) . . . . ? O7 C35 C36 C37 179.91(12) . . . . ? C35 C36 C37 C38 178.92(13) . . . . ? C36 C37 C38 C39 -179.67(15) . . . . ? C37 C38 C39 C40 -178.42(17) . . . . ? N3 C41 C42 C43 177.6(2) . . . 2_576 ? C43 C41 C42 C43 0.0(3) . . . 2_576 ? N3 C41 C43 C42 -177.8(2) . . . 2_576 ? C42 C41 C43 C42 0.0(3) . . . 2_576 ? N4 C44 C45 C46 177.66(18) . . . . ? C49 C44 C45 C46 0.7(3) . . . . ? C44 C45 C46 C47 -0.6(3) . . . . ? C45 C46 C47 C48 -0.3(3) . . . . ? C46 C47 C48 C49 1.1(3) . . . . ? C47 C48 C49 C44 -1.0(3) . . . . ? N4 C44 C49 C48 -176.9(2) . . . . ? C45 C44 C49 C48 0.1(3) . . . . ? C55 C50 C51 C52 0.4(3) . . . . ? N5 C50 C51 C52 176.92(17) . . . . ? C50 C51 C52 C53 -0.3(3) . . . . ? C51 C52 C53 C54 0.1(3) . . . . ? C52 C53 C54 C55 0.0(3) . . . . ? C53 C54 C55 C50 0.0(3) . . . . ? N5 C50 C55 C54 -176.76(17) . . . . ? C51 C50 C55 C54 -0.2(3) . . . . ? C61 C56 C57 C58 -3.4(6) . . . . ? N6 C56 C57 C58 175.1(5) . . . . ? C56 C57 C58 C59 2.0(6) . . . . ? C57 C58 C59 C60 -0.2(6) . . . . ? C58 C59 C60 C61 -0.1(6) . . . . ? C59 C60 C61 C56 -1.3(5) . . . . ? C57 C56 C61 C60 3.1(6) . . . . ? N6 C56 C61 C60 -175.5(5) . . . . ? C67 C62 C63 C64 0.0 . . . . ? N7 C62 C63 C64 176.2(13) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C62 0.0 . . . . ? C63 C62 C67 C66 0.0 . . . . ? N7 C62 C67 C66 -175.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.545 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.052