# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'A. N. Cammidge' _publ_contact_author_email A.CAMMIDGE@UEA.AC.UK _publ_section_title ; Probing the Structural Factors Influencing Columnar Mesophase Formation and Stability in Triphenylene Discotics ; loop_ _publ_author_name 'A. N. Cammidge' 'Celine Chausson' 'Hemant Gopee' 'David L. Hughes' 'Juanjuan Li.' # Attachment 'H2.CIF' data_hemg2 _database_code_depnum_ccdc_archive 'CCDC 725154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 23' _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 N2 O4, ca 0.7(O H2)' _chemical_formula_structural 2,11-bis(C6H4CN-4)-3,6,7,10-tetrakis(O-n-C6H13)-triphenylene _chemical_formula_sum 'C56 H67.4 N2 O4.7' _chemical_formula_weight 843.7 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.215(1) _cell_length_b 12.998(2) _cell_length_c 17.424(4) _cell_angle_alpha 77.29(3) _cell_angle_beta 80.52(1) _cell_angle_gamma 80.53(1) _cell_volume 2422.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour 'very pale yellow' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13816 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.36 _reflns_number_total 8194 _reflns_number_gt 5686 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0989P)^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 8194 _refine_ls_number_parameters 612 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1650 _refine_ls_wR_factor_gt 0.1537 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.24406(15) 0.54465(15) 0.38507(10) 0.0285(4) Uani 1 1 d . . . C11 C 0.18030(15) 0.60867(15) 0.32403(10) 0.0309(4) Uani 1 1 d . . . H11 H 0.2131 0.6066 0.2717 0.037 Uiso 1 1 calc R . . C12 C 0.07172(15) 0.67428(15) 0.33781(10) 0.0294(4) Uani 1 1 d . . . C13 C 0.01456(15) 0.74832(15) 0.27149(10) 0.0306(4) Uani 1 1 d . . . C14 C -0.11175(15) 0.77049(15) 0.27272(10) 0.0305(4) Uani 1 1 d . . . H14 H -0.1623 0.7354 0.3146 0.037 Uiso 1 1 calc R . . C15 C -0.16294(16) 0.84375(15) 0.21263(10) 0.0333(4) Uani 1 1 d . . . H15 H -0.2473 0.8570 0.2141 0.040 Uiso 1 1 calc R . . C16 C -0.08856(16) 0.89756(16) 0.15001(10) 0.0345(4) Uani 1 1 d . . . C17 C 0.03780(16) 0.87428(16) 0.14605(10) 0.0369(5) Uani 1 1 d . . . H17 H 0.0880 0.9083 0.1034 0.044 Uiso 1 1 calc R . . C18 C 0.08794(16) 0.80035(16) 0.20592(10) 0.0359(4) Uani 1 1 d . . . H18 H 0.1723 0.7846 0.2028 0.043 Uiso 1 1 calc R . . C19 C -0.14451(17) 0.97779(17) 0.09015(11) 0.0404(5) Uani 1 1 d . . . N20 N -0.19142(16) 1.04207(16) 0.04398(11) 0.0531(5) Uani 1 1 d . . . C2 C 0.19366(15) 0.54779(14) 0.46455(10) 0.0287(4) Uani 1 1 d . . . C21 C 0.08083(15) 0.61176(15) 0.47895(10) 0.0307(4) Uani 1 1 d . . . H21 H 0.0457 0.6121 0.5311 0.037 Uiso 1 1 calc R . . C22 C 0.02135(15) 0.67352(15) 0.41821(10) 0.0293(4) Uani 1 1 d . . . O23 O -0.08513(10) 0.73936(10) 0.43110(7) 0.0342(3) Uani 1 1 d . . . C24 C -0.13896(16) 0.74018(16) 0.51155(10) 0.0319(4) Uani 1 1 d . . . H24A H -0.0822 0.7600 0.5404 0.038 Uiso 1 1 calc R . . H24B H -0.1587 0.6699 0.5377 0.038 Uiso 1 1 calc R . . C25 C -0.25309(16) 0.81956(16) 0.51034(11) 0.0351(4) Uani 1 1 d . . . H25A H -0.3104 0.7978 0.4830 0.042 Uiso 1 1 calc R . . H25B H -0.2332 0.8888 0.4816 0.042 Uiso 1 1 calc R . . C26 C -0.31157(17) 0.82759(17) 0.59445(12) 0.0403(5) Uani 1 1 d . . . H26A H -0.3307 0.7579 0.6225 0.048 Uiso 1 1 calc R . . H26B H -0.2526 0.8476 0.6215 0.048 Uiso 1 1 calc R . . C27 C -0.42636(18) 0.90646(18) 0.59915(14) 0.0511(6) Uani 1 1 d . B . H27A H -0.4858 0.8867 0.5723 0.061 Uiso 1 1 calc R . . H27B H -0.4076 0.9765 0.5716 0.061 Uiso 1 1 calc R . . C28 C -0.4819(2) 0.9115(2) 0.68423(18) 0.0766(9) Uani 1 1 d . . . H28A H -0.4913 0.8390 0.7112 0.092 Uiso 0.60 1 calc PR A 1 H28B H -0.4211 0.9338 0.7085 0.092 Uiso 0.60 1 calc PR A 1 H28C H -0.4276 0.9367 0.7118 0.092 Uiso 0.40 1 calc PR A 2 H28D H -0.5024 0.8428 0.7137 0.092 Uiso 0.40 1 calc PR A 2 C29 C -0.5935(6) 0.9747(5) 0.7037(4) 0.0552(15) Uani 0.60 1 d P B 1 H29A H -0.6117 0.9665 0.7604 0.083 Uiso 0.60 1 calc PR B 1 H29B H -0.6576 0.9525 0.6835 0.083 Uiso 0.60 1 calc PR B 1 H29C H -0.5869 1.0480 0.6805 0.083 Uiso 0.60 1 calc PR B 1 C29A C -0.6117(10) 1.0027(9) 0.6693(5) 0.062(3) Uani 0.40 1 d P B 2 H29D H -0.6558 1.0132 0.7197 0.093 Uiso 0.40 1 calc PR B 2 H29E H -0.6626 0.9762 0.6409 0.093 Uiso 0.40 1 calc PR B 2 H29F H -0.5885 1.0692 0.6390 0.093 Uiso 0.40 1 calc PR B 2 C3 C 0.25658(15) 0.48720(15) 0.53040(10) 0.0280(4) Uani 1 1 d . . . C31 C 0.20750(15) 0.49302(15) 0.60993(10) 0.0302(4) Uani 1 1 d . . . H31 H 0.1325 0.5339 0.6198 0.036 Uiso 1 1 calc R . . C32 C 0.26747(15) 0.44015(15) 0.67264(10) 0.0298(4) Uani 1 1 d . . . O33 O 0.22800(10) 0.44175(11) 0.75046(7) 0.0340(3) Uani 1 1 d . . . C34 C 0.10974(16) 0.49908(16) 0.76990(10) 0.0343(4) Uani 1 1 d . . . H34A H 0.0483 0.4729 0.7489 0.041 Uiso 1 1 calc R . . H34B H 0.1092 0.5743 0.7472 0.041 Uiso 1 1 calc R . . C35 C 0.08322(16) 0.48209(16) 0.85919(10) 0.0352(4) Uani 1 1 d . . . H35A H 0.0061 0.5239 0.8736 0.042 Uiso 1 1 calc R . . H35B H 0.1462 0.5079 0.8790 0.042 Uiso 1 1 calc R . . C36 C 0.07705(17) 0.36620(16) 0.89925(10) 0.0362(4) Uani 1 1 d . . . H36A H 0.1548 0.3246 0.8857 0.043 Uiso 1 1 calc R . . H36B H 0.0152 0.3400 0.8786 0.043 Uiso 1 1 calc R . . C37 C 0.04773(18) 0.34905(16) 0.98925(11) 0.0393(5) Uani 1 1 d . . . H37A H 0.1128 0.3701 1.0103 0.047 Uiso 1 1 calc R . . H37B H -0.0269 0.3946 1.0029 0.047 Uiso 1 1 calc R . . C38 C 0.0324(2) 0.23430(18) 1.02832(11) 0.0463(5) Uani 1 1 d . . . H38A H 0.1047 0.1882 1.0116 0.056 Uiso 1 1 calc R . . H38B H -0.0364 0.2149 1.0100 0.056 Uiso 1 1 calc R . . C39 C 0.0118(2) 0.2152(2) 1.11892(12) 0.0601(7) Uani 1 1 d . . . H39A H 0.0025 0.1418 1.1400 0.090 Uiso 1 1 calc R . . H39B H -0.0606 0.2595 1.1361 0.090 Uiso 1 1 calc R . . H39C H 0.0806 0.2323 1.1376 0.090 Uiso 1 1 calc R . . C4 C 0.36860(15) 0.42379(15) 0.51548(10) 0.0298(4) Uani 1 1 d . . . C41 C 0.42806(15) 0.36754(15) 0.58137(10) 0.0318(4) Uani 1 1 d . . . H41 H 0.5014 0.3240 0.5724 0.038 Uiso 1 1 calc R . . C42 C 0.38035(16) 0.37575(15) 0.65763(10) 0.0320(4) Uani 1 1 d . . . O43 O 0.43021(11) 0.32731(11) 0.72510(7) 0.0394(3) Uani 1 1 d . . . C44 C 0.53368(16) 0.24699(17) 0.72076(12) 0.0421(5) Uani 1 1 d . . . H44A H 0.6008 0.2753 0.6840 0.051 Uiso 1 1 calc R . . H44B H 0.5132 0.1870 0.7032 0.051 Uiso 1 1 calc R . . C45 C 0.56747(18) 0.21337(19) 0.80426(12) 0.0475(5) Uani 1 1 d . . . H45A H 0.6302 0.1522 0.8057 0.057 Uiso 1 1 calc R . . H45B H 0.6026 0.2707 0.8159 0.057 Uiso 1 1 calc R . . C46 C 0.4637(2) 0.1853(2) 0.86918(13) 0.0539(6) Uani 1 1 d . . . H46A H 0.4376 0.1204 0.8630 0.065 Uiso 1 1 calc R . . H46B H 0.3954 0.2414 0.8625 0.065 Uiso 1 1 calc R . . C47 C 0.4951(2) 0.1697(2) 0.95281(14) 0.0595(6) Uani 1 1 d . . . H47A H 0.5588 0.1097 0.9611 0.071 Uiso 1 1 calc R . . H47B H 0.5274 0.2324 0.9578 0.071 Uiso 1 1 calc R . . C48 C 0.3890(2) 0.1506(3) 1.01650(15) 0.0716(8) Uani 1 1 d . . . H48A H 0.3570 0.0877 1.0116 0.086 Uiso 1 1 calc R . . H48B H 0.3251 0.2104 1.0079 0.086 Uiso 1 1 calc R . . C49 C 0.4192(3) 0.1355(3) 1.10032(16) 0.0990(11) Uani 1 1 d . . . H49A H 0.3471 0.1237 1.1375 0.149 Uiso 1 1 calc R . . H49B H 0.4488 0.1981 1.1064 0.149 Uiso 1 1 calc R . . H49C H 0.4807 0.0753 1.1101 0.149 Uiso 1 1 calc R . . C5 C 0.42062(15) 0.41807(15) 0.43350(10) 0.0305(4) Uani 1 1 d . . . C51 C 0.53354(15) 0.35542(16) 0.41670(11) 0.0335(4) Uani 1 1 d . . . H51 H 0.5737 0.3159 0.4585 0.040 Uiso 1 1 calc R . . C52 C 0.58557(15) 0.35138(16) 0.33993(11) 0.0346(4) Uani 1 1 d . . . O53 O 0.69740(11) 0.29443(12) 0.32141(8) 0.0443(4) Uani 1 1 d . D . C54 C 0.75951(18) 0.23362(18) 0.38545(14) 0.0515(6) Uani 1 1 d . . . H54A H 0.7092 0.1858 0.4225 0.062 Uiso 0.50 1 calc PR C 1 H54B H 0.7899 0.2783 0.4137 0.062 Uiso 0.50 1 calc PR C 1 H54C H 0.7139 0.1754 0.4117 0.062 Uiso 0.50 1 calc PR C 2 H54D H 0.7568 0.2786 0.4235 0.062 Uiso 0.50 1 calc PR C 2 C55 C 0.8676(4) 0.1711(5) 0.3331(3) 0.0378(11) Uani 0.50 1 d P D 1 H55A H 0.8345 0.1380 0.2980 0.045 Uiso 0.50 1 calc PR D 1 H55B H 0.9224 0.2195 0.3014 0.045 Uiso 0.50 1 calc PR D 1 C56 C 0.9339(3) 0.0878(3) 0.3921(2) 0.0336(8) Uani 0.50 1 d P D 1 H56A H 0.8785 0.0386 0.4215 0.040 Uiso 0.50 1 calc PR D 1 H56B H 0.9596 0.1221 0.4296 0.040 Uiso 0.50 1 calc PR D 1 C57 C 1.0447(4) 0.0264(4) 0.3518(3) 0.0361(11) Uani 0.50 1 d P D 1 H57A H 1.0989 0.0758 0.3209 0.043 Uiso 0.50 1 calc PR D 1 H57B H 1.0188 -0.0100 0.3157 0.043 Uiso 0.50 1 calc PR D 1 C58 C 1.1140(5) -0.0553(5) 0.4124(3) 0.0383(12) Uani 0.50 1 d P D 1 H58A H 1.1377 -0.0198 0.4498 0.046 Uiso 0.50 1 calc PR D 1 H58B H 1.0614 -0.1071 0.4418 0.046 Uiso 0.50 1 calc PR D 1 C55A C 0.8894(4) 0.1877(4) 0.3660(3) 0.0334(10) Uani 0.50 1 d P D 2 H55C H 0.9271 0.1649 0.4143 0.040 Uiso 0.50 1 calc PR D 2 H55D H 0.9337 0.2418 0.3309 0.040 Uiso 0.50 1 calc PR D 2 C56A C 0.8971(3) 0.0931(4) 0.3260(2) 0.0351(9) Uani 0.50 1 d P D 2 H56C H 0.8455 0.0430 0.3590 0.042 Uiso 0.50 1 calc PR D 2 H56D H 0.8655 0.1179 0.2756 0.042 Uiso 0.50 1 calc PR D 2 C57A C 1.0252(4) 0.0357(4) 0.3113(3) 0.0373(11) Uani 0.50 1 d P D 2 H57C H 1.0262 -0.0127 0.2760 0.045 Uiso 0.50 1 calc PR D 2 H57D H 1.0799 0.0872 0.2852 0.045 Uiso 0.50 1 calc PR D 2 C58A C 1.0710(5) -0.0265(5) 0.3874(4) 0.0380(13) Uani 0.50 1 d P D 2 H58C H 1.0114 -0.0724 0.4157 0.046 Uiso 0.50 1 calc PR D 2 H58D H 1.0763 0.0233 0.4204 0.046 Uiso 0.50 1 calc PR D 2 C59 C 1.2126(2) -0.1044(2) 0.37506(15) 0.0639(7) Uani 1 1 d . . . H59A H 1.2556 -0.1555 0.4132 0.096 Uiso 0.50 1 calc PR D 1 H59B H 1.2648 -0.0530 0.3466 0.096 Uiso 0.50 1 calc PR D 1 H59C H 1.1886 -0.1400 0.3384 0.096 Uiso 0.50 1 calc PR D 1 H59D H 1.2341 -0.1410 0.4261 0.096 Uiso 0.50 1 calc PR D 2 H59E H 1.2732 -0.0596 0.3488 0.096 Uiso 0.50 1 calc PR D 2 H59F H 1.2082 -0.1553 0.3436 0.096 Uiso 0.50 1 calc PR D 2 C6 C 0.36006(15) 0.47737(15) 0.36955(10) 0.0309(4) Uani 1 1 d . . . C61 C 0.41546(16) 0.47015(16) 0.29177(11) 0.0337(4) Uani 1 1 d . . . H61 H 0.3751 0.5080 0.2496 0.040 Uiso 1 1 calc R . . C62 C 0.52702(16) 0.40952(16) 0.27493(11) 0.0354(4) Uani 1 1 d . . . C63 C 0.58094(16) 0.40899(17) 0.19082(11) 0.0369(5) Uani 1 1 d . . . C64 C 0.63515(18) 0.31641(18) 0.16439(12) 0.0439(5) Uani 1 1 d . . . H64 H 0.6421 0.2524 0.2008 0.053 Uiso 1 1 calc R . . C65 C 0.67904(17) 0.31743(19) 0.08512(12) 0.0462(5) Uani 1 1 d . . . H65 H 0.7145 0.2545 0.0688 0.055 Uiso 1 1 calc R . . C66 C 0.66996(16) 0.41267(19) 0.02997(11) 0.0436(5) Uani 1 1 d . . . C67 C 0.61787(16) 0.50697(19) 0.05510(11) 0.0433(5) Uani 1 1 d . . . H67 H 0.6123 0.5710 0.0186 0.052 Uiso 1 1 calc R . . C68 C 0.57452(16) 0.50478(18) 0.13448(11) 0.0398(5) Uani 1 1 d . . . H68 H 0.5405 0.5679 0.1509 0.048 Uiso 1 1 calc R . . C69 C 0.71339(18) 0.4147(2) -0.05306(13) 0.0525(6) Uani 1 1 d . . . N70 N 0.74652(17) 0.4147(2) -0.11924(11) 0.0680(6) Uani 1 1 d . . . O81 O 0.1331(8) 0.3337(8) 0.2798(6) 0.173(3) Uiso 0.40 1 d P . . O82 O 0.2887(12) 0.3301(12) 0.1484(8) 0.187(5) Uiso 0.30 1 d P . . 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 0.0294(9) 0.0322(11) 0.0231(9) -0.0077(7) 0.0016(7) -0.0044(7) C11 0.0334(9) 0.0357(11) 0.0230(9) -0.0087(8) 0.0019(7) -0.0053(8) C12 0.0316(9) 0.0343(11) 0.0220(9) -0.0071(8) -0.0001(7) -0.0052(7) C13 0.0334(9) 0.0345(11) 0.0245(9) -0.0105(8) -0.0001(7) -0.0038(7) C14 0.0331(9) 0.0345(11) 0.0235(9) -0.0081(8) 0.0006(7) -0.0047(7) C15 0.0341(9) 0.0381(12) 0.0280(9) -0.0108(8) -0.0023(7) -0.0014(8) C16 0.0415(10) 0.0365(12) 0.0249(9) -0.0077(8) -0.0043(7) -0.0014(8) C17 0.0403(10) 0.0438(13) 0.0232(9) -0.0036(8) 0.0019(7) -0.0059(8) C18 0.0333(9) 0.0461(13) 0.0269(9) -0.0085(8) -0.0003(7) -0.0037(8) C19 0.0453(11) 0.0428(13) 0.0303(10) -0.0039(9) -0.0038(8) -0.0041(9) N20 0.0579(11) 0.0539(13) 0.0400(10) 0.0018(9) -0.0060(8) -0.0010(9) C2 0.0304(9) 0.0293(11) 0.0256(9) -0.0075(8) 0.0013(7) -0.0042(7) C21 0.0323(9) 0.0385(11) 0.0194(8) -0.0078(8) 0.0026(7) -0.0027(8) C22 0.0280(9) 0.0322(11) 0.0263(9) -0.0082(8) 0.0012(7) -0.0020(7) O23 0.0336(7) 0.0418(8) 0.0226(6) -0.0083(6) 0.0021(5) 0.0050(5) C24 0.0349(9) 0.0384(12) 0.0215(9) -0.0095(8) 0.0025(7) -0.0041(8) C25 0.0335(9) 0.0355(12) 0.0347(10) -0.0108(8) 0.0029(8) -0.0021(8) C26 0.0400(10) 0.0418(13) 0.0373(11) -0.0139(9) 0.0091(8) -0.0061(9) C27 0.0396(10) 0.0463(14) 0.0686(15) -0.0282(12) 0.0137(10) -0.0076(9) C28 0.0753(16) 0.0551(17) 0.091(2) -0.0358(15) 0.0516(15) -0.0175(13) C29 0.052(3) 0.048(4) 0.063(4) -0.023(3) 0.012(3) -0.005(2) C29A 0.050(4) 0.069(7) 0.061(6) -0.029(5) 0.009(4) 0.014(4) C3 0.0279(9) 0.0301(11) 0.0255(9) -0.0068(7) 0.0000(7) -0.0048(7) C31 0.0310(9) 0.0310(11) 0.0267(9) -0.0063(8) -0.0004(7) -0.0014(7) C32 0.0335(9) 0.0332(11) 0.0214(9) -0.0059(8) 0.0010(7) -0.0048(7) O33 0.0354(7) 0.0427(8) 0.0201(6) -0.0058(5) 0.0010(5) 0.0004(6) C34 0.0366(10) 0.0372(12) 0.0259(9) -0.0075(8) 0.0001(7) 0.0023(8) C35 0.0390(10) 0.0402(12) 0.0250(9) -0.0099(8) 0.0015(7) -0.0022(8) C36 0.0423(10) 0.0411(12) 0.0238(9) -0.0088(8) 0.0011(7) -0.0036(8) C37 0.0461(11) 0.0443(13) 0.0267(10) -0.0103(9) 0.0011(8) -0.0056(9) C38 0.0589(13) 0.0483(14) 0.0292(10) -0.0068(9) 0.0015(9) -0.0085(10) C39 0.0904(18) 0.0542(16) 0.0308(12) 0.0011(11) -0.0033(11) -0.0130(13) C4 0.0328(9) 0.0302(11) 0.0269(9) -0.0081(8) -0.0005(7) -0.0061(7) C41 0.0292(9) 0.0326(11) 0.0318(10) -0.0080(8) -0.0018(7) 0.0009(7) C42 0.0332(9) 0.0336(11) 0.0274(9) -0.0022(8) -0.0053(7) -0.0033(8) O43 0.0376(7) 0.0459(9) 0.0295(7) -0.0044(6) -0.0068(5) 0.0078(6) C44 0.0363(10) 0.0412(13) 0.0461(12) -0.0075(10) -0.0084(9) 0.0042(8) C45 0.0413(11) 0.0495(14) 0.0495(13) -0.0057(10) -0.0133(9) 0.0017(9) C46 0.0544(13) 0.0570(16) 0.0468(13) 0.0015(11) -0.0147(10) -0.0054(11) C47 0.0614(15) 0.0618(17) 0.0528(14) 0.0030(12) -0.0189(11) -0.0090(12) C48 0.0784(17) 0.083(2) 0.0532(15) -0.0019(14) -0.0134(13) -0.0207(15) C49 0.122(3) 0.127(3) 0.0503(17) -0.0052(18) -0.0193(17) -0.033(2) C5 0.0320(9) 0.0322(11) 0.0271(9) -0.0094(8) 0.0019(7) -0.0049(7) C51 0.0314(9) 0.0359(11) 0.0327(10) -0.0112(8) 0.0000(7) -0.0013(8) C52 0.0281(9) 0.0376(12) 0.0386(11) -0.0161(9) 0.0033(7) -0.0022(8) O53 0.0325(7) 0.0520(10) 0.0464(8) -0.0221(7) 0.0062(6) 0.0052(6) C54 0.0389(11) 0.0354(13) 0.0670(15) 0.0016(11) 0.0067(10) 0.0037(9) C55 0.038(3) 0.044(3) 0.028(3) -0.009(2) 0.005(2) 0.000(2) C56 0.0359(19) 0.034(2) 0.029(2) -0.0065(16) -0.0019(15) -0.0019(16) C57 0.044(3) 0.031(3) 0.027(3) -0.001(3) -0.002(2) 0.005(2) C58 0.038(3) 0.039(3) 0.037(3) -0.014(3) 0.000(2) 0.001(2) C55A 0.036(2) 0.032(3) 0.030(3) -0.009(2) 0.0022(19) -0.0016(17) C56A 0.038(2) 0.037(3) 0.029(2) -0.0080(18) -0.0039(15) 0.0000(18) C57A 0.042(2) 0.043(3) 0.026(3) -0.011(2) -0.005(2) 0.0028(18) C58A 0.034(3) 0.039(4) 0.038(4) -0.011(3) 0.000(2) 0.003(3) C59 0.0818(17) 0.0672(18) 0.0491(14) -0.0160(13) -0.0054(12) -0.0255(14) C6 0.0312(9) 0.0333(11) 0.0278(9) -0.0100(8) 0.0021(7) -0.0041(7) C61 0.0355(9) 0.0389(12) 0.0260(9) -0.0105(8) 0.0036(7) -0.0051(8) C62 0.0352(10) 0.0397(12) 0.0325(10) -0.0163(9) 0.0061(8) -0.0065(8) C63 0.0315(9) 0.0480(13) 0.0323(10) -0.0167(9) 0.0061(8) -0.0069(8) C64 0.0446(11) 0.0470(13) 0.0408(11) -0.0207(10) 0.0107(9) -0.0082(9) C65 0.0415(11) 0.0584(15) 0.0419(12) -0.0286(11) 0.0084(9) -0.0044(10) C66 0.0321(10) 0.0696(16) 0.0314(11) -0.0227(11) 0.0023(8) -0.0024(9) C67 0.0366(10) 0.0596(15) 0.0323(11) -0.0143(10) 0.0002(8) -0.0004(9) C68 0.0360(10) 0.0506(14) 0.0321(10) -0.0179(9) 0.0038(8) 0.0012(8) C69 0.0410(11) 0.0811(18) 0.0366(12) -0.0263(12) -0.0013(9) 0.0047(10) N70 0.0575(12) 0.1086(19) 0.0338(11) -0.0275(11) -0.0005(9) 0.0131(11) _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 C2 1.414(2) . ? C1 C11 1.414(2) . ? C1 C6 1.464(2) . ? C11 C12 1.386(2) . ? C11 H11 0.9300 . ? C12 C22 1.420(2) . ? C12 C13 1.491(2) . ? C13 C14 1.396(2) . ? C13 C18 1.405(2) . ? C14 C15 1.383(3) . ? C14 H14 0.9300 . ? C15 C16 1.390(3) . ? C15 H15 0.9300 . ? C16 C17 1.393(3) . ? C16 C19 1.446(3) . ? C17 C18 1.379(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 N20 1.149(2) . ? C2 C21 1.413(2) . ? C2 C3 1.456(2) . ? C21 C22 1.376(2) . ? C21 H21 0.9300 . ? C22 O23 1.367(2) . ? O23 C24 1.434(2) . ? C24 C25 1.506(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.522(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.511(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.522(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.414(7) . ? C28 C29A 1.736(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C28 H28D 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C29A H29D 0.9600 . ? C29A H29E 0.9600 . ? C29A H29F 0.9600 . ? C3 C4 1.404(2) . ? C3 C31 1.418(2) . ? C31 C32 1.370(2) . ? C31 H31 0.9300 . ? C32 O33 1.359(2) . ? C32 C42 1.418(2) . ? O33 C34 1.438(2) . ? C34 C35 1.509(2) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.522(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.522(2) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.522(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.528(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C4 C41 1.421(2) . ? C4 C5 1.464(2) . ? C41 C42 1.368(2) . ? C41 H41 0.9300 . ? C42 O43 1.366(2) . ? O43 C44 1.432(2) . ? C44 C45 1.516(3) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.514(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.518(3) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.500(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.517(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C5 C6 1.413(2) . ? C5 C51 1.413(2) . ? C51 C52 1.377(3) . ? C51 H51 0.9300 . ? C52 O53 1.375(2) . ? C52 C62 1.411(3) . ? O53 C54 1.429(3) . ? C54 C55A 1.495(5) . ? C54 C55 1.612(6) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? C54 H54D 0.9700 . ? C55 C56 1.509(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.520(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.533(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.329(6) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C55A C56A 1.526(6) . ? C55A H55C 0.9700 . ? C55A H55D 0.9700 . ? C56A C57A 1.516(6) . ? C56A H56C 0.9700 . ? C56A H56D 0.9700 . ? C57A C58A 1.513(7) . ? C57A H57C 0.9700 . ? C57A H57D 0.9700 . ? C58A C59 1.745(6) . ? C58A H58C 0.9700 . ? C58A H58D 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C59 H59D 0.9600 . ? C59 H59E 0.9600 . ? C59 H59F 0.9600 . ? C6 C61 1.411(2) . ? C61 C62 1.389(3) . ? C61 H61 0.9300 . ? C62 C63 1.491(2) . ? C63 C64 1.393(3) . ? C63 C68 1.405(3) . ? C64 C65 1.386(3) . ? C64 H64 0.9300 . ? C65 C66 1.391(3) . ? C65 H65 0.9300 . ? C66 C67 1.397(3) . ? C66 C69 1.444(3) . ? C67 C68 1.384(3) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 N70 1.152(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C11 117.95(15) . . ? C2 C1 C6 118.97(15) . . ? C11 C1 C6 123.08(15) . . ? C12 C11 C1 123.70(16) . . ? C12 C11 H11 118.1 . . ? C1 C11 H11 118.1 . . ? C11 C12 C22 117.15(15) . . ? C11 C12 C13 121.56(15) . . ? C22 C12 C13 121.15(15) . . ? C14 C13 C18 117.78(17) . . ? C14 C13 C12 122.05(15) . . ? C18 C13 C12 120.16(16) . . ? C15 C14 C13 121.08(17) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.09(17) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 119.90(17) . . ? C15 C16 C19 118.97(17) . . ? C17 C16 C19 121.12(17) . . ? C18 C17 C16 119.49(17) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C13 121.56(17) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? N20 C19 C16 178.3(2) . . ? C21 C2 C1 118.55(15) . . ? C21 C2 C3 120.45(15) . . ? C1 C2 C3 121.00(15) . . ? C22 C21 C2 122.05(16) . . ? C22 C21 H21 119.0 . . ? C2 C21 H21 119.0 . . ? O23 C22 C21 122.78(15) . . ? O23 C22 C12 116.63(15) . . ? C21 C22 C12 120.55(15) . . ? C22 O23 C24 118.14(13) . . ? O23 C24 C25 108.20(14) . . ? O23 C24 H24A 110.1 . . ? C25 C24 H24A 110.1 . . ? O23 C24 H24B 110.1 . . ? C25 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C24 C25 C26 110.65(16) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 114.43(17) . . ? C27 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 112.6(2) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C27 123.0(3) . . ? C29 C28 C29A 21.8(4) . . ? C27 C28 C29A 101.3(4) . . ? C29 C28 H28A 106.6 . . ? C27 C28 H28A 106.6 . . ? C29A C28 H28A 118.9 . . ? C29 C28 H28B 106.6 . . ? C27 C28 H28B 106.6 . . ? C29A C28 H28B 115.8 . . ? H28A C28 H28B 106.5 . . ? C29 C28 H28C 101.3 . . ? C27 C28 H28C 111.5 . . ? C29A C28 H28C 111.5 . . ? H28A C28 H28C 106.9 . . ? H28B C28 H28C 5.6 . . ? C29 C28 H28D 98.9 . . ? C27 C28 H28D 111.5 . . ? C29A C28 H28D 111.5 . . ? H28A C28 H28D 7.7 . . ? H28B C28 H28D 109.7 . . ? H28C C28 H28D 109.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29A H29D 109.5 . . ? C28 C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C28 C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C4 C3 C31 119.13(15) . . ? C4 C3 C2 120.02(15) . . ? C31 C3 C2 120.83(15) . . ? C32 C31 C3 121.87(16) . . ? C32 C31 H31 119.1 . . ? C3 C31 H31 119.1 . . ? O33 C32 C31 125.92(16) . . ? O33 C32 C42 115.07(15) . . ? C31 C32 C42 119.01(15) . . ? C32 O33 C34 117.63(13) . . ? O33 C34 C35 107.47(14) . . ? O33 C34 H34A 110.2 . . ? C35 C34 H34A 110.2 . . ? O33 C34 H34B 110.2 . . ? C35 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C34 C35 C36 113.45(16) . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 113.60(16) . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 113.24(17) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 113.39(18) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C3 C4 C41 118.21(16) . . ? C3 C4 C5 119.55(15) . . ? C41 C4 C5 122.25(16) . . ? C42 C41 C4 121.80(16) . . ? C42 C41 H41 119.1 . . ? C4 C41 H41 119.1 . . ? O43 C42 C41 126.94(16) . . ? O43 C42 C32 113.10(15) . . ? C41 C42 C32 119.97(15) . . ? C42 O43 C44 119.37(15) . . ? O43 C44 C45 105.61(16) . . ? O43 C44 H44A 110.6 . . ? C45 C44 H44A 110.6 . . ? O43 C44 H44B 110.6 . . ? C45 C44 H44B 110.6 . . ? H44A C44 H44B 108.7 . . ? C46 C45 C44 115.59(17) . . ? C46 C45 H45A 108.4 . . ? C44 C45 H45A 108.4 . . ? C46 C45 H45B 108.4 . . ? C44 C45 H45B 108.4 . . ? H45A C45 H45B 107.4 . . ? C45 C46 C47 114.38(18) . . ? C45 C46 H46A 108.7 . . ? C47 C46 H46A 108.7 . . ? C45 C46 H46B 108.7 . . ? C47 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C48 C47 C46 113.9(2) . . ? C48 C47 H47A 108.8 . . ? C46 C47 H47A 108.8 . . ? C48 C47 H47B 108.8 . . ? C46 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? C47 C48 C49 114.4(2) . . ? C47 C48 H48A 108.7 . . ? C49 C48 H48A 108.7 . . ? C47 C48 H48B 108.7 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C6 C5 C51 118.73(16) . . ? C6 C5 C4 120.47(15) . . ? C51 C5 C4 120.78(16) . . ? C52 C51 C5 121.63(17) . . ? C52 C51 H51 119.2 . . ? C5 C51 H51 119.2 . . ? O53 C52 C51 123.11(17) . . ? O53 C52 C62 115.98(16) . . ? C51 C52 C62 120.88(16) . . ? C52 O53 C54 117.87(15) . . ? O53 C54 C55A 117.7(2) . . ? O53 C54 C55 97.4(2) . . ? C55A C54 C55 27.35(18) . . ? O53 C54 H54A 112.3 . . ? C55A C54 H54A 115.1 . . ? C55 C54 H54A 112.3 . . ? O53 C54 H54B 112.3 . . ? C55A C54 H54B 86.8 . . ? C55 C54 H54B 112.3 . . ? H54A C54 H54B 109.9 . . ? O53 C54 H54C 107.9 . . ? C55A C54 H54C 107.9 . . ? C55 C54 H54C 99.9 . . ? H54A C54 H54C 14.7 . . ? H54B C54 H54C 123.5 . . ? O53 C54 H54D 107.9 . . ? C55A C54 H54D 107.9 . . ? C55 C54 H54D 134.5 . . ? H54A C54 H54D 92.6 . . ? H54B C54 H54D 22.8 . . ? H54C C54 H54D 107.2 . . ? C56 C55 C54 105.6(3) . . ? C56 C55 H55A 110.6 . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55B 110.6 . . ? C54 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? C55 C56 C57 112.0(4) . . ? C55 C56 H56A 109.2 . . ? C57 C56 H56A 109.2 . . ? C55 C56 H56B 109.2 . . ? C57 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C56 C57 C58 111.6(4) . . ? C56 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? C56 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? C59 C58 C57 109.7(5) . . ? C59 C58 H58A 109.7 . . ? C57 C58 H58A 109.7 . . ? C59 C58 H58B 109.7 . . ? C57 C58 H58B 109.7 . . ? H58A C58 H58B 108.2 . . ? C54 C55A C56A 110.6(4) . . ? C54 C55A H55C 109.5 . . ? C56A C55A H55C 109.5 . . ? C54 C55A H55D 109.5 . . ? C56A C55A H55D 109.5 . . ? H55C C55A H55D 108.1 . . ? C57A C56A C55A 113.8(3) . . ? C57A C56A H56C 108.8 . . ? C55A C56A H56C 108.8 . . ? C57A C56A H56D 108.8 . . ? C55A C56A H56D 108.8 . . ? H56C C56A H56D 107.7 . . ? C58A C57A C56A 112.2(4) . . ? C58A C57A H57C 109.2 . . ? C56A C57A H57C 109.2 . . ? C58A C57A H57D 109.2 . . ? C56A C57A H57D 109.2 . . ? H57C C57A H57D 107.9 . . ? C57A C58A C59 115.1(4) . . ? C57A C58A H58C 108.5 . . ? C59 C58A H58C 108.5 . . ? C57A C58A H58D 108.5 . . ? C59 C58A H58D 108.5 . . ? H58C C58A H58D 107.5 . . ? C58 C59 C58A 21.6(3) . . ? C58 C59 H59A 109.5 . . ? C58A C59 H59A 130.2 . . ? C58 C59 H59B 109.5 . . ? C58A C59 H59B 102.6 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? C58A C59 H59C 93.8 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C59 H59D 88.2 . . ? C58A C59 H59D 109.5 . . ? H59A C59 H59D 21.6 . . ? H59B C59 H59D 114.9 . . ? H59C C59 H59D 122.7 . . ? C58 C59 H59E 115.0 . . ? C58A C59 H59E 109.5 . . ? H59A C59 H59E 102.6 . . ? H59B C59 H59E 7.3 . . ? H59C C59 H59E 110.6 . . ? H59D C59 H59E 109.5 . . ? C58 C59 H59F 122.6 . . ? C58A C59 H59F 109.5 . . ? H59A C59 H59F 93.7 . . ? H59B C59 H59F 110.7 . . ? H59C C59 H59F 17.0 . . ? H59D C59 H59F 109.5 . . ? H59E C59 H59F 109.5 . . ? C61 C6 C5 118.00(16) . . ? C61 C6 C1 122.02(16) . . ? C5 C6 C1 119.97(15) . . ? C62 C61 C6 123.48(17) . . ? C62 C61 H61 118.3 . . ? C6 C61 H61 118.3 . . ? C61 C62 C52 117.28(16) . . ? C61 C62 C63 120.00(17) . . ? C52 C62 C63 122.71(16) . . ? C64 C63 C68 117.70(18) . . ? C64 C63 C62 122.83(19) . . ? C68 C63 C62 119.43(17) . . ? C65 C64 C63 121.6(2) . . ? C65 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? C64 C65 C66 119.9(2) . . ? C64 C65 H65 120.1 . . ? C66 C65 H65 120.1 . . ? C65 C66 C67 119.67(18) . . ? C65 C66 C69 120.5(2) . . ? C67 C66 C69 119.8(2) . . ? C68 C67 C66 119.8(2) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C67 C68 C63 121.29(19) . . ? C67 C68 H68 119.4 . . ? C63 C68 H68 119.4 . . ? N70 C69 C66 178.6(3) . . ? 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 C2 C1 C11 C12 0.2(3) . . . . ? C6 C1 C11 C12 -178.69(16) . . . . ? C1 C11 C12 C22 -2.0(3) . . . . ? C1 C11 C12 C13 173.77(16) . . . . ? C11 C12 C13 C14 144.78(18) . . . . ? C22 C12 C13 C14 -39.7(3) . . . . ? C11 C12 C13 C18 -36.8(3) . . . . ? C22 C12 C13 C18 138.80(18) . . . . ? C18 C13 C14 C15 -2.0(3) . . . . ? C12 C13 C14 C15 176.47(17) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C17 2.8(3) . . . . ? C14 C15 C16 C19 -176.77(17) . . . . ? C15 C16 C17 C18 -2.2(3) . . . . ? C19 C16 C17 C18 177.37(18) . . . . ? C16 C17 C18 C13 -0.6(3) . . . . ? C14 C13 C18 C17 2.6(3) . . . . ? C12 C13 C18 C17 -175.88(17) . . . . ? C15 C16 C19 N20 30(8) . . . . ? C17 C16 C19 N20 -150(8) . . . . ? C11 C1 C2 C21 2.0(2) . . . . ? C6 C1 C2 C21 -179.11(15) . . . . ? C11 C1 C2 C3 -177.60(16) . . . . ? C6 C1 C2 C3 1.3(2) . . . . ? C1 C2 C21 C22 -2.4(3) . . . . ? C3 C2 C21 C22 177.20(16) . . . . ? C2 C21 C22 O23 -177.07(16) . . . . ? C2 C21 C22 C12 0.5(3) . . . . ? C11 C12 C22 O23 179.35(15) . . . . ? C13 C12 C22 O23 3.6(2) . . . . ? C11 C12 C22 C21 1.6(3) . . . . ? C13 C12 C22 C21 -174.17(17) . . . . ? C21 C22 O23 C24 -2.7(2) . . . . ? C12 C22 O23 C24 179.64(15) . . . . ? C22 O23 C24 C25 179.03(14) . . . . ? O23 C24 C25 C26 -177.51(14) . . . . ? C24 C25 C26 C27 179.41(16) . . . . ? C25 C26 C27 C28 179.76(18) . . . . ? C26 C27 C28 C29 -176.1(4) . . . . ? C26 C27 C28 C29A -177.8(4) . . . . ? C21 C2 C3 C4 179.94(16) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C21 C2 C3 C31 -1.4(3) . . . . ? C1 C2 C3 C31 178.12(16) . . . . ? C4 C3 C31 C32 1.3(3) . . . . ? C2 C3 C31 C32 -177.31(16) . . . . ? C3 C31 C32 O33 179.46(17) . . . . ? C3 C31 C32 C42 -1.6(3) . . . . ? C31 C32 O33 C34 3.6(3) . . . . ? C42 C32 O33 C34 -175.36(15) . . . . ? C32 O33 C34 C35 175.78(15) . . . . ? O33 C34 C35 C36 -62.32(19) . . . . ? C34 C35 C36 C37 -178.82(15) . . . . ? C35 C36 C37 C38 175.71(16) . . . . ? C36 C37 C38 C39 175.97(18) . . . . ? C31 C3 C4 C41 0.2(3) . . . . ? C2 C3 C4 C41 178.84(15) . . . . ? C31 C3 C4 C5 -179.42(15) . . . . ? C2 C3 C4 C5 -0.8(2) . . . . ? C3 C4 C41 C42 -1.5(3) . . . . ? C5 C4 C41 C42 178.15(17) . . . . ? C4 C41 C42 O43 -178.69(17) . . . . ? C4 C41 C42 C32 1.2(3) . . . . ? O33 C32 C42 O43 -0.7(2) . . . . ? C31 C32 C42 O43 -179.78(15) . . . . ? O33 C32 C42 C41 179.38(16) . . . . ? C31 C32 C42 C41 0.3(3) . . . . ? C41 C42 O43 C44 -9.9(3) . . . . ? C32 C42 O43 C44 170.16(16) . . . . ? C42 O43 C44 C45 178.20(16) . . . . ? O43 C44 C45 C46 50.4(3) . . . . ? C44 C45 C46 C47 -170.4(2) . . . . ? C45 C46 C47 C48 175.4(2) . . . . ? C46 C47 C48 C49 -179.7(3) . . . . ? C3 C4 C5 C6 1.2(3) . . . . ? C41 C4 C5 C6 -178.39(17) . . . . ? C3 C4 C5 C51 179.62(16) . . . . ? C41 C4 C5 C51 0.0(3) . . . . ? C6 C5 C51 C52 0.3(3) . . . . ? C4 C5 C51 C52 -178.15(16) . . . . ? C5 C51 C52 O53 177.49(16) . . . . ? C5 C51 C52 C62 -0.5(3) . . . . ? C51 C52 O53 C54 2.5(3) . . . . ? C62 C52 O53 C54 -179.47(17) . . . . ? C52 O53 C54 C55A -169.4(3) . . . . ? C52 O53 C54 C55 171.3(3) . . . . ? O53 C54 C55 C56 -171.1(3) . . . . ? C55A C54 C55 C56 48.6(5) . . . . ? C54 C55 C56 C57 -176.2(3) . . . . ? C55 C56 C57 C58 178.0(4) . . . . ? C56 C57 C58 C59 -177.6(4) . . . . ? O53 C54 C55A C56A -73.9(4) . . . . ? C55 C54 C55A C56A -28.2(5) . . . . ? C54 C55A C56A C57A -174.6(3) . . . . ? C55A C56A C57A C58A 71.2(5) . . . . ? C56A C57A C58A C59 174.6(4) . . . . ? C57 C58 C59 C58A -14.6(8) . . . . ? C57A C58A C59 C58 169.1(14) . . . . ? C51 C5 C6 C61 0.5(3) . . . . ? C4 C5 C6 C61 178.95(16) . . . . ? C51 C5 C6 C1 -178.82(16) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? C2 C1 C6 C61 179.82(16) . . . . ? C11 C1 C6 C61 -1.3(3) . . . . ? C2 C1 C6 C5 -0.9(3) . . . . ? C11 C1 C6 C5 177.97(16) . . . . ? C5 C6 C61 C62 -1.2(3) . . . . ? C1 C6 C61 C62 178.11(16) . . . . ? C6 C61 C62 C52 1.0(3) . . . . ? C6 C61 C62 C63 -178.10(17) . . . . ? O53 C52 C62 C61 -178.27(16) . . . . ? C51 C52 C62 C61 -0.2(3) . . . . ? O53 C52 C62 C63 0.8(3) . . . . ? C51 C52 C62 C63 178.93(18) . . . . ? C61 C62 C63 C64 -136.8(2) . . . . ? C52 C62 C63 C64 44.1(3) . . . . ? C61 C62 C63 C68 41.3(2) . . . . ? C52 C62 C63 C68 -137.8(2) . . . . ? C68 C63 C64 C65 -1.4(3) . . . . ? C62 C63 C64 C65 176.69(17) . . . . ? C63 C64 C65 C66 0.3(3) . . . . ? C64 C65 C66 C67 0.8(3) . . . . ? C64 C65 C66 C69 -178.93(18) . . . . ? C65 C66 C67 C68 -0.7(3) . . . . ? C69 C66 C67 C68 179.00(17) . . . . ? C66 C67 C68 C63 -0.5(3) . . . . ? C64 C63 C68 C67 1.5(3) . . . . ? C62 C63 C68 C67 -176.70(16) . . . . ? C65 C66 C69 N70 55(11) . . . . ? C67 C66 C69 N70 -125(11) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.471 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.045