# 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 'Janusz Jurczak' _publ_contact_author_email JURCZAK@ICHO.EDU.PL _publ_section_title ; Anion receptors based on 7,7'-diamido-2,2'-diindolylmethane ; loop_ _publ_author_name 'Janusz Jurczak' 'Pawel Dydio' 'Tomasz Zielinski' # Attachment '1c_TBACL.CIF' data_p243cl _database_code_depnum_ccdc_archive 'CCDC 707057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H66 Cl N7 O2' _chemical_formula_weight 796.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.7982(7) _cell_length_b 20.0727(13) _cell_length_c 22.7848(14) _cell_angle_alpha 65.331(6) _cell_angle_beta 80.937(5) _cell_angle_gamma 86.475(5) _cell_volume 4431.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84109 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.74 _reflns_number_total 21476 _reflns_number_gt 12427 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0560P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21476 _refine_ls_number_parameters 1085 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 Cl1A Cl 0.27367(3) 0.29610(2) 0.269132(17) 0.02152(9) Uani 1 1 d . . . N1A N 0.52703(12) 0.12902(8) 0.16858(6) 0.0217(3) Uani 1 1 d . . . N2A N 0.23195(12) 0.12900(8) 0.27042(6) 0.0202(3) Uani 1 1 d . . . N3A N 0.09562(12) 0.17395(7) 0.37269(6) 0.0201(3) Uani 1 1 d . . . N4A N -0.00544(13) 0.33473(7) 0.32647(6) 0.0200(3) Uani 1 1 d . . . N5A N 0.03742(13) 0.42816(7) 0.18437(6) 0.0207(3) Uani 1 1 d . . . N6A N 0.17764(14) 0.46048(8) 0.01858(7) 0.0283(3) Uani 1 1 d . . . C7A C 0.59257(15) 0.18547(9) 0.11908(7) 0.0242(4) Uani 1 1 d . . . H7A H 0.6736 0.1823 0.0971 0.029 Uiso 1 1 calc R . . C8A C 0.52189(15) 0.24794(9) 0.10610(8) 0.0255(4) Uani 1 1 d . . . H8A H 0.5447 0.2954 0.0734 0.031 Uiso 1 1 calc R . . C9A C 0.40960(15) 0.22858(8) 0.15008(7) 0.0231(3) Uani 1 1 d . . . H9A H 0.3426 0.2606 0.1527 0.028 Uiso 1 1 calc R . . C10A C 0.41463(14) 0.15437(8) 0.18872(7) 0.0197(3) Uani 1 1 d . . . C11A C 0.32617(14) 0.10134(8) 0.24038(7) 0.0208(3) Uani 1 1 d . . . O12A O 0.33901(10) 0.03505(6) 0.25507(5) 0.0280(3) Uani 1 1 d . . . C13A C 0.07187(14) 0.11310(8) 0.36379(7) 0.0193(3) Uani 1 1 d . . . C14A C 0.00910(14) 0.17808(8) 0.42276(7) 0.0196(3) Uani 1 1 d . . . C15A C -0.06994(14) 0.11853(8) 0.44792(7) 0.0213(3) Uani 1 1 d . . . C16A C -0.03176(14) 0.07610(8) 0.41067(7) 0.0209(3) Uani 1 1 d . . . C17A C -0.07697(15) 0.01195(8) 0.41077(8) 0.0257(4) Uani 1 1 d . . . H17A H -0.1455 -0.0144 0.4421 0.031 Uiso 1 1 calc R . . C18A C -0.02037(15) -0.01207(9) 0.36487(8) 0.0279(4) Uani 1 1 d . . . H18A H -0.0518 -0.0550 0.3644 0.034 Uiso 1 1 calc R . . C19A C 0.08267(15) 0.02471(8) 0.31851(8) 0.0247(4) Uani 1 1 d . . . H19A H 0.1192 0.0064 0.2875 0.030 Uiso 1 1 calc R . . C20A C 0.13161(14) 0.08777(8) 0.31765(7) 0.0202(3) Uani 1 1 d . . . C21A C -0.17516(15) 0.09949(9) 0.50358(7) 0.0282(4) Uani 1 1 d . . . H21A H -0.2151 0.0537 0.5105 0.042 Uiso 0.50 1 calc PR . . H21B H -0.2371 0.1390 0.4935 0.042 Uiso 0.50 1 calc PR . . H21C H -0.1422 0.0933 0.5432 0.042 Uiso 0.50 1 calc PR . . H21D H -0.1812 0.1369 0.5210 0.042 Uiso 0.50 1 calc PR . . H21E H -0.1592 0.0517 0.5380 0.042 Uiso 0.50 1 calc PR . . H21F H -0.2540 0.0974 0.4882 0.042 Uiso 0.50 1 calc PR . . C22A C 0.01230(14) 0.24211(8) 0.44099(7) 0.0203(3) Uani 1 1 d . . . H22A H -0.0420 0.2284 0.4842 0.024 Uiso 1 1 calc R . . C23A C 0.14524(14) 0.25663(8) 0.45046(7) 0.0240(4) Uani 1 1 d . . . H23A H 0.1988 0.2770 0.4074 0.029 Uiso 1 1 calc R . . H23B H 0.1399 0.2938 0.4687 0.029 Uiso 1 1 calc R . . C24A C 0.20673(15) 0.18778(9) 0.49570(8) 0.0300(4) Uani 1 1 d . . . H24A H 0.2304 0.1554 0.4734 0.045 Uiso 1 1 calc R . . H24B H 0.1475 0.1622 0.5354 0.045 Uiso 1 1 calc R . . H24C H 0.2818 0.2015 0.5074 0.045 Uiso 1 1 calc R . . C25A C -0.04290(14) 0.31070(8) 0.39351(7) 0.0200(3) Uani 1 1 d . . . C26A C -0.06640(13) 0.39882(8) 0.29464(7) 0.0189(3) Uani 1 1 d . . . C27A C -0.05470(14) 0.44491(8) 0.22779(7) 0.0192(3) Uani 1 1 d . . . C28A C -0.13122(14) 0.50588(8) 0.20903(8) 0.0226(3) Uani 1 1 d . . . H28A H -0.1266 0.5380 0.1641 0.027 Uiso 1 1 calc R . . C29A C -0.21555(15) 0.52104(8) 0.25535(8) 0.0245(4) Uani 1 1 d . . . H29A H -0.2680 0.5628 0.2409 0.029 Uiso 1 1 calc R . . C30A C -0.22445(14) 0.47695(8) 0.32128(8) 0.0227(3) Uani 1 1 d . . . H30A H -0.2810 0.4885 0.3521 0.027 Uiso 1 1 calc R . . C31A C -0.14827(14) 0.41475(8) 0.34180(7) 0.0203(3) Uani 1 1 d . . . C32A C -0.13061(14) 0.35787(8) 0.40480(7) 0.0210(3) Uani 1 1 d . . . C33A C -0.19068(15) 0.35600(9) 0.46970(7) 0.0278(4) Uani 1 1 d . . . H33A H -0.2500 0.3966 0.4627 0.042 Uiso 0.50 1 calc PR . . H33B H -0.1258 0.3607 0.4933 0.042 Uiso 0.50 1 calc PR . . H33C H -0.2354 0.3094 0.4953 0.042 Uiso 0.50 1 calc PR . . H33D H -0.1575 0.3145 0.5049 0.042 Uiso 0.50 1 calc PR . . H33E H -0.2817 0.3504 0.4743 0.042 Uiso 0.50 1 calc PR . . H33F H -0.1720 0.4018 0.4723 0.042 Uiso 0.50 1 calc PR . . C34A C 0.04455(15) 0.45383(8) 0.11839(7) 0.0226(3) Uani 1 1 d . . . O35A O -0.04470(10) 0.48438(7) 0.08935(5) 0.0333(3) Uani 1 1 d . . . C36A C 0.16505(15) 0.44361(8) 0.08418(7) 0.0225(3) Uani 1 1 d . . . C37A C 0.28144(15) 0.42300(8) 0.10341(8) 0.0255(4) Uani 1 1 d . . . H37A H 0.3012 0.4083 0.1462 0.031 Uiso 1 1 calc R . . C38A C 0.36546(16) 0.42779(9) 0.04801(8) 0.0310(4) Uani 1 1 d . . . H38A H 0.4526 0.4172 0.0463 0.037 Uiso 1 1 calc R . . C39A C 0.29810(17) 0.45056(9) -0.00299(8) 0.0341(4) Uani 1 1 d . . . H39A H 0.3308 0.4582 -0.0465 0.041 Uiso 1 1 calc R . . H1A H 0.5530(15) 0.0833(9) 0.1898(8) 0.026(5) Uiso 1 1 d . . . H2A H 0.2357(16) 0.1709(9) 0.2645(8) 0.028(5) Uiso 1 1 d . . . H3A H 0.1476(15) 0.2066(9) 0.3507(8) 0.023(5) Uiso 1 1 d . . . H4A H 0.0597(16) 0.3224(9) 0.3105(8) 0.025(5) Uiso 1 1 d . . . H5A H 0.1019(16) 0.4060(9) 0.1996(8) 0.030(5) Uiso 1 1 d . . . H6A H 0.1186(18) 0.4755(10) -0.0050(9) 0.040(6) Uiso 1 1 d . . . N7A N 0.66710(11) 0.21841(7) 0.29783(6) 0.0205(3) Uani 1 1 d . . . C40A C 0.80202(14) 0.20217(9) 0.27551(8) 0.0248(4) Uani 1 1 d . . . H40A H 0.8564 0.2434 0.2690 0.030 Uiso 1 1 calc R . . H40B H 0.8305 0.1576 0.3105 0.030 Uiso 1 1 calc R . . C41A C 0.81851(15) 0.19081(9) 0.21265(8) 0.0296(4) Uani 1 1 d . . . H41A H 0.7765 0.2312 0.1798 0.036 Uiso 1 1 calc R . . H41B H 0.7768 0.1444 0.2213 0.036 Uiso 1 1 calc R . . C42A C 0.95614(16) 0.18810(9) 0.18452(9) 0.0316(4) Uani 1 1 d . . . H42A H 0.9979 0.1477 0.2176 0.038 Uiso 1 1 calc R . . H42B H 0.9599 0.1765 0.1461 0.038 Uiso 1 1 calc R . . C43A C 1.02841(17) 0.25835(10) 0.16419(9) 0.0375(4) Uani 1 1 d . . . H43A H 0.9857 0.2992 0.1330 0.056 Uiso 1 1 calc R . . H43B H 1.1134 0.2537 0.1437 0.056 Uiso 1 1 calc R . . H43C H 1.0329 0.2677 0.2027 0.056 Uiso 1 1 calc R . . C44A C 0.61727(14) 0.28543(8) 0.24479(7) 0.0215(3) Uani 1 1 d . . . H44A H 0.6015 0.2719 0.2095 0.026 Uiso 1 1 calc R . . H44B H 0.5358 0.2991 0.2634 0.026 Uiso 1 1 calc R . . C45A C 0.70325(15) 0.35195(8) 0.21517(8) 0.0258(4) Uani 1 1 d . . . H45A H 0.7185 0.3666 0.2499 0.031 Uiso 1 1 calc R . . H45B H 0.7850 0.3391 0.1960 0.031 Uiso 1 1 calc R . . C46A C 0.64659(16) 0.41573(9) 0.16270(8) 0.0340(4) Uani 1 1 d . . . H46A H 0.7125 0.4533 0.1374 0.041 Uiso 1 1 calc R . . H46B H 0.6181 0.3982 0.1324 0.041 Uiso 1 1 calc R . . C47A C 0.53771(17) 0.45093(10) 0.18895(10) 0.0474(5) Uani 1 1 d . . . H47A H 0.4693 0.4152 0.2112 0.071 Uiso 1 1 calc R . . H47B H 0.5086 0.4931 0.1528 0.071 Uiso 1 1 calc R . . H47C H 0.5644 0.4674 0.2199 0.071 Uiso 1 1 calc R . . C48A C 0.66627(15) 0.23318(9) 0.35811(7) 0.0235(4) Uani 1 1 d . . . H48A H 0.7042 0.2820 0.3444 0.028 Uiso 1 1 calc R . . H48B H 0.7200 0.1964 0.3871 0.028 Uiso 1 1 calc R . . C49A C 0.53689(15) 0.23114(9) 0.39718(8) 0.0280(4) Uani 1 1 d . . . H49A H 0.5156 0.1801 0.4285 0.034 Uiso 1 1 calc R . . H49B H 0.4732 0.2485 0.3672 0.034 Uiso 1 1 calc R . . C50A C 0.53465(18) 0.27981(10) 0.43433(9) 0.0390(5) Uani 1 1 d . . . H50A H 0.4667 0.2631 0.4720 0.047 Uiso 1 1 calc R . . H50B H 0.6151 0.2749 0.4514 0.047 Uiso 1 1 calc R . . C51A C 0.51411(18) 0.35968(10) 0.39080(10) 0.0435(5) Uani 1 1 d . . . H51A H 0.5810 0.3763 0.3533 0.065 Uiso 1 1 calc R . . H51B H 0.5152 0.3894 0.4156 0.065 Uiso 1 1 calc R . . H51C H 0.4328 0.3650 0.3753 0.065 Uiso 1 1 calc R . . C52A C 0.58184(14) 0.15473(8) 0.31204(7) 0.0224(3) Uani 1 1 d . . . H52A H 0.5817 0.1487 0.2711 0.027 Uiso 1 1 calc R . . H52B H 0.4953 0.1670 0.3261 0.027 Uiso 1 1 calc R . . C53A C 0.61743(15) 0.08222(9) 0.36378(8) 0.0283(4) Uani 1 1 d . . . H53A H 0.6387 0.0901 0.4011 0.034 Uiso 1 1 calc R . . H53B H 0.6925 0.0624 0.3455 0.034 Uiso 1 1 calc R . . C54A C 0.51028(16) 0.02716(9) 0.38742(8) 0.0302(4) Uani 1 1 d . . . H54A H 0.4836 0.0232 0.3494 0.036 Uiso 1 1 calc R . . H54B H 0.4380 0.0451 0.4093 0.036 Uiso 1 1 calc R . . C55A C 0.54754(17) -0.04830(9) 0.43462(9) 0.0355(4) Uani 1 1 d . . . H55A H 0.6167 -0.0672 0.4125 0.053 Uiso 1 1 calc R . . H55B H 0.4755 -0.0817 0.4494 0.053 Uiso 1 1 calc R . . H55C H 0.5744 -0.0446 0.4723 0.053 Uiso 1 1 calc R . . Cl1B Cl 0.25277(3) 0.27135(2) 0.766907(17) 0.02179(9) Uani 1 1 d . . . N1B N 0.15470(14) 0.43160(8) 0.51451(7) 0.0298(3) Uani 1 1 d . . . N2B N 0.03294(12) 0.40264(7) 0.68193(6) 0.0205(3) Uani 1 1 d . . . N3B N -0.01282(13) 0.31403(7) 0.82591(6) 0.0184(3) Uani 1 1 d . . . N4B N 0.08143(12) 0.15013(7) 0.87805(6) 0.0204(3) Uani 1 1 d . . . N5B N 0.21710(12) 0.09681(8) 0.78046(6) 0.0221(3) Uani 1 1 d . . . N6B N 0.52270(12) 0.08887(8) 0.69081(6) 0.0226(3) Uani 1 1 d . . . C7B C 0.26376(16) 0.41064(9) 0.48980(8) 0.0299(4) Uani 1 1 d . . . H7B H 0.2891 0.4193 0.4453 0.036 Uiso 1 1 calc R . . C8B C 0.33187(18) 0.37469(10) 0.53966(8) 0.0377(5) Uani 1 1 d . . . H8B H 0.4126 0.3538 0.5362 0.045 Uiso 1 1 calc R . . C9B C 0.26041(16) 0.37425(9) 0.59714(8) 0.0307(4) Uani 1 1 d . . . H9B H 0.2841 0.3532 0.6396 0.037 Uiso 1 1 calc R . . C10B C 0.15019(15) 0.40990(8) 0.58041(7) 0.0229(3) Uani 1 1 d . . . C11B C 0.03920(15) 0.42801(9) 0.61619(7) 0.0261(4) Uani 1 1 d . . . O12B O -0.04637(12) 0.46389(8) 0.58724(6) 0.0529(4) Uani 1 1 d . . . C13B C -0.07382(13) 0.37728(8) 0.79141(7) 0.0182(3) Uani 1 1 d . . . C14B C -0.05722(14) 0.29091(8) 0.89214(7) 0.0193(3) Uani 1 1 d . . . C15B C -0.14755(14) 0.33828(8) 0.90055(7) 0.0205(3) Uani 1 1 d . . . C16B C -0.16069(14) 0.39378(8) 0.83637(7) 0.0198(3) Uani 1 1 d . . . C17B C -0.23649(14) 0.45572(8) 0.81386(8) 0.0238(4) Uani 1 1 d . . . H17B H -0.2968 0.4672 0.8434 0.029 Uiso 1 1 calc R . . C18B C -0.22175(15) 0.49976(8) 0.74776(8) 0.0245(4) Uani 1 1 d . . . H18B H -0.2726 0.5421 0.7319 0.029 Uiso 1 1 calc R . . C19B C -0.13387(14) 0.48366(8) 0.70348(8) 0.0229(3) Uani 1 1 d . . . H19B H -0.1254 0.5156 0.6584 0.027 Uiso 1 1 calc R . . C20B C -0.05882(13) 0.42186(8) 0.72416(7) 0.0187(3) Uani 1 1 d . . . C21B C -0.21650(16) 0.33693(9) 0.96371(8) 0.0288(4) Uani 1 1 d . . . H21G H -0.2758 0.3778 0.9545 0.043 Uiso 0.50 1 calc PR . . H21H H -0.1563 0.3417 0.9898 0.043 Uiso 0.50 1 calc PR . . H21I H -0.2624 0.2905 0.9880 0.043 Uiso 0.50 1 calc PR . . H21J H -0.1872 0.2955 1.0004 0.043 Uiso 0.50 1 calc PR . . H21K H -0.3067 0.3316 0.9651 0.043 Uiso 0.50 1 calc PR . . H21L H -0.2006 0.3828 0.9669 0.043 Uiso 0.50 1 calc PR . . C22B C -0.00454(14) 0.22337(8) 0.94203(7) 0.0208(3) Uani 1 1 d . . . H22B H -0.0616 0.2114 0.9842 0.025 Uiso 1 1 calc R . . C23B C 0.12673(15) 0.23746(9) 0.95377(8) 0.0246(4) Uani 1 1 d . . . H23C H 0.1599 0.1910 0.9844 0.030 Uiso 1 1 calc R . . H23D H 0.1845 0.2544 0.9120 0.030 Uiso 1 1 calc R . . C24B C 0.12277(17) 0.29468(10) 0.98172(8) 0.0334(4) Uani 1 1 d . . . H24D H 0.0977 0.3420 0.9497 0.050 Uiso 1 1 calc R . . H24E H 0.2061 0.2993 0.9916 0.050 Uiso 1 1 calc R . . H24F H 0.0620 0.2795 1.0218 0.050 Uiso 1 1 calc R . . C25B C -0.00692(14) 0.15807(8) 0.92591(7) 0.0205(3) Uani 1 1 d . . . C26B C 0.05477(14) 0.08787(8) 0.87114(7) 0.0202(3) Uani 1 1 d . . . C27B C 0.11375(14) 0.05884(8) 0.82764(7) 0.0211(3) Uani 1 1 d . . . C28B C 0.06326(15) -0.00476(9) 0.83129(8) 0.0261(4) Uani 1 1 d . . . H28B H 0.0988 -0.0250 0.8015 0.031 Uiso 1 1 calc R . . C29B C -0.03970(15) -0.03972(9) 0.87841(8) 0.0299(4) Uani 1 1 d . . . H29B H -0.0710 -0.0840 0.8804 0.036 Uiso 1 1 calc R . . C30B C -0.09645(15) -0.01185(8) 0.92161(8) 0.0258(4) Uani 1 1 d . . . H30B H -0.1652 -0.0367 0.9536 0.031 Uiso 1 1 calc R . . C31B C -0.05098(14) 0.05384(8) 0.91759(7) 0.0205(3) Uani 1 1 d . . . C32B C -0.08973(14) 0.09978(8) 0.95169(7) 0.0207(3) Uani 1 1 d . . . C33B C -0.19679(15) 0.08424(9) 1.00615(7) 0.0258(4) Uani 1 1 d . . . H33G H -0.2392 0.0389 1.0139 0.039 Uiso 0.50 1 calc PR . . H33H H -0.2563 0.1250 0.9943 0.039 Uiso 0.50 1 calc PR . . H33I H -0.1649 0.0786 1.0459 0.039 Uiso 0.50 1 calc PR . . H33J H -0.2011 0.1228 1.0222 0.039 Uiso 0.50 1 calc PR . . H33K H -0.1840 0.0367 1.0418 0.039 Uiso 0.50 1 calc PR . . H33L H -0.2753 0.0831 0.9901 0.039 Uiso 0.50 1 calc PR . . C34B C 0.31542(14) 0.06493(9) 0.75649(7) 0.0214(3) Uani 1 1 d . . . O35B O 0.32868(10) -0.00219(6) 0.77689(5) 0.0273(3) Uani 1 1 d . . . C36B C 0.40681(14) 0.11529(8) 0.70478(7) 0.0210(3) Uani 1 1 d . . . C37B C 0.40340(15) 0.18820(9) 0.66194(7) 0.0249(4) Uani 1 1 d . . . H37B H 0.3348 0.2207 0.6599 0.030 Uiso 1 1 calc R . . C38B C 0.52066(15) 0.20529(9) 0.62174(8) 0.0273(4) Uani 1 1 d . . . H38B H 0.5456 0.2515 0.5875 0.033 Uiso 1 1 calc R . . C39B C 0.59224(16) 0.14307(9) 0.64110(8) 0.0262(4) Uani 1 1 d . . . H39B H 0.6761 0.1387 0.6228 0.031 Uiso 1 1 calc R . . H1B H 0.1053(19) 0.4596(11) 0.4905(10) 0.054(7) Uiso 1 1 d . . . H2B H 0.0970(16) 0.3765(9) 0.6986(8) 0.030(5) Uiso 1 1 d . . . H3B H 0.0531(17) 0.3004(10) 0.8116(8) 0.035(5) Uiso 1 1 d . . . H4B H 0.1370(16) 0.1829(10) 0.8524(8) 0.034(5) Uiso 1 1 d . . . H5B H 0.2215(16) 0.1403(10) 0.7696(8) 0.029(5) Uiso 1 1 d . . . H6B H 0.5490(16) 0.0455(9) 0.7119(8) 0.029(5) Uiso 1 1 d . . . N7B N 0.64616(12) 0.22070(7) 0.79631(6) 0.0208(3) Uani 1 1 d . . . C40B C 0.62586(15) 0.23217(9) 0.85907(7) 0.0237(4) Uani 1 1 d . . . H40C H 0.6538 0.2824 0.8489 0.028 Uiso 1 1 calc R . . H40D H 0.6797 0.1974 0.8895 0.028 Uiso 1 1 calc R . . C41B C 0.49122(15) 0.22210(9) 0.89358(8) 0.0270(4) Uani 1 1 d . . . H41C H 0.4695 0.1693 0.9150 0.032 Uiso 1 1 calc R . . H41D H 0.4335 0.2471 0.8613 0.032 Uiso 1 1 calc R . . C42B C 0.47569(17) 0.25404(9) 0.94477(8) 0.0303(4) Uani 1 1 d . . . H42C H 0.3988 0.2333 0.9761 0.036 Uiso 1 1 calc R . . H42D H 0.5480 0.2391 0.9693 0.036 Uiso 1 1 calc R . . C43B C 0.46695(18) 0.33713(9) 0.91469(9) 0.0372(4) Uani 1 1 d . . . H43D H 0.5432 0.3580 0.8839 0.056 Uiso 1 1 calc R . . H43E H 0.4581 0.3549 0.9492 0.056 Uiso 1 1 calc R . . H43F H 0.3939 0.3522 0.8915 0.056 Uiso 1 1 calc R . . C44B C 0.58602(15) 0.28202(8) 0.74303(7) 0.0224(3) Uani 1 1 d . . . H44C H 0.6000 0.2721 0.7034 0.027 Uiso 1 1 calc R . . H44D H 0.4944 0.2803 0.7574 0.027 Uiso 1 1 calc R . . C45B C 0.63222(18) 0.35913(9) 0.72438(8) 0.0338(4) Uani 1 1 d . . . H45C H 0.7246 0.3611 0.7126 0.041 Uiso 1 1 calc R . . H45D H 0.6111 0.3720 0.7622 0.041 Uiso 1 1 calc R . . C46B C 0.57260(18) 0.41447(9) 0.66688(8) 0.0367(4) Uani 1 1 d . . . H46C H 0.4806 0.4069 0.6765 0.044 Uiso 1 1 calc R . . H46D H 0.5894 0.4646 0.6621 0.044 Uiso 1 1 calc R . . C47B C 0.6207(2) 0.40880(11) 0.60278(9) 0.0572(6) Uani 1 1 d . . . H47D H 0.7118 0.4161 0.5929 0.086 Uiso 1 1 calc R . . H47E H 0.5808 0.4464 0.5677 0.086 Uiso 1 1 calc R . . H47F H 0.6006 0.3602 0.6064 0.086 Uiso 1 1 calc R . . C48B C 0.78713(14) 0.21808(9) 0.77702(8) 0.0237(4) Uani 1 1 d . . . H48C H 0.8260 0.2601 0.7794 0.028 Uiso 1 1 calc R . . H48D H 0.8197 0.1727 0.8095 0.028 Uiso 1 1 calc R . . C49B C 0.82888(15) 0.22001(10) 0.70950(8) 0.0286(4) Uani 1 1 d . . . H49C H 0.8064 0.2678 0.6761 0.034 Uiso 1 1 calc R . . H49D H 0.7848 0.1810 0.7049 0.034 Uiso 1 1 calc R . . C50B C 0.96965(15) 0.20878(10) 0.69852(8) 0.0309(4) Uani 1 1 d . . . H50C H 1.0127 0.2435 0.7093 0.037 Uiso 1 1 calc R . . H50D H 0.9901 0.1584 0.7284 0.037 Uiso 1 1 calc R . . C51B C 1.01810(17) 0.22015(11) 0.62905(9) 0.0416(5) Uani 1 1 d . . . H51D H 0.9746 0.1866 0.6178 0.062 Uiso 1 1 calc R . . H51E H 1.1083 0.2104 0.6249 0.062 Uiso 1 1 calc R . . H51F H 1.0028 0.2709 0.5994 0.062 Uiso 1 1 calc R . . C52B C 0.58325(15) 0.15021(8) 0.80659(8) 0.0225(3) Uani 1 1 d . . . H52C H 0.4916 0.1553 0.8171 0.027 Uiso 1 1 calc R . . H52D H 0.5985 0.1447 0.7648 0.027 Uiso 1 1 calc R . . C53B C 0.62473(15) 0.08035(8) 0.85950(8) 0.0267(4) Uani 1 1 d . . . H53C H 0.6330 0.0893 0.8983 0.032 Uiso 1 1 calc R . . H53D H 0.7077 0.0654 0.8435 0.032 Uiso 1 1 calc R . . C54B C 0.52961(16) 0.01934(9) 0.87838(8) 0.0303(4) Uani 1 1 d . . . H54C H 0.5210 0.0114 0.8391 0.036 Uiso 1 1 calc R . . H54D H 0.4470 0.0350 0.8940 0.036 Uiso 1 1 calc R . . C55B C 0.56544(17) -0.05273(9) 0.93121(9) 0.0362(4) Uani 1 1 d . . . H55D H 0.6438 -0.0707 0.9148 0.054 Uiso 1 1 calc R . . H55E H 0.4987 -0.0890 0.9431 0.054 Uiso 1 1 calc R . . H55F H 0.5769 -0.0450 0.9697 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1A 0.0194(2) 0.02008(19) 0.02124(19) -0.00638(15) 0.00190(15) -0.00090(15) N1A 0.0216(7) 0.0221(8) 0.0235(7) -0.0123(6) -0.0024(6) 0.0038(6) N2A 0.0204(7) 0.0155(7) 0.0234(7) -0.0077(6) -0.0009(6) 0.0008(6) N3A 0.0165(7) 0.0198(7) 0.0201(7) -0.0058(6) 0.0023(6) -0.0028(6) N4A 0.0182(7) 0.0222(7) 0.0184(7) -0.0088(6) 0.0004(6) 0.0040(6) N5A 0.0212(7) 0.0227(7) 0.0173(7) -0.0073(6) -0.0028(6) 0.0007(6) N6A 0.0318(9) 0.0318(8) 0.0177(7) -0.0073(6) -0.0050(6) 0.0082(7) C7A 0.0216(9) 0.0315(9) 0.0232(8) -0.0167(7) 0.0022(7) -0.0015(7) C8A 0.0288(9) 0.0261(9) 0.0207(8) -0.0098(7) -0.0010(7) 0.0003(7) C9A 0.0239(9) 0.0243(9) 0.0219(8) -0.0111(7) -0.0033(7) 0.0050(7) C10A 0.0178(8) 0.0249(8) 0.0197(8) -0.0127(7) -0.0032(6) 0.0031(6) C11A 0.0191(8) 0.0225(9) 0.0238(8) -0.0115(7) -0.0084(7) 0.0049(7) O12A 0.0237(6) 0.0200(6) 0.0390(7) -0.0119(5) -0.0031(5) 0.0046(5) C13A 0.0170(8) 0.0163(8) 0.0209(8) -0.0031(6) -0.0052(6) 0.0007(6) C14A 0.0177(8) 0.0214(8) 0.0154(8) -0.0038(6) -0.0019(6) 0.0025(6) C15A 0.0154(8) 0.0228(8) 0.0186(8) -0.0016(7) -0.0030(6) 0.0020(6) C16A 0.0168(8) 0.0192(8) 0.0201(8) -0.0009(6) -0.0048(6) 0.0015(6) C17A 0.0187(8) 0.0211(8) 0.0295(9) -0.0019(7) -0.0047(7) -0.0028(7) C18A 0.0259(9) 0.0191(8) 0.0364(10) -0.0078(7) -0.0076(8) -0.0016(7) C19A 0.0229(9) 0.0223(9) 0.0282(9) -0.0098(7) -0.0044(7) 0.0012(7) C20A 0.0174(8) 0.0186(8) 0.0213(8) -0.0048(6) -0.0048(6) 0.0029(6) C21A 0.0228(9) 0.0316(10) 0.0216(9) -0.0036(7) 0.0000(7) -0.0012(7) C22A 0.0194(8) 0.0233(8) 0.0148(7) -0.0060(6) 0.0015(6) 0.0002(7) C23A 0.0236(9) 0.0272(9) 0.0197(8) -0.0083(7) -0.0024(7) -0.0009(7) C24A 0.0254(9) 0.0343(10) 0.0267(9) -0.0083(8) -0.0056(7) -0.0001(8) C25A 0.0194(8) 0.0238(8) 0.0164(8) -0.0081(7) -0.0006(6) -0.0021(7) C26A 0.0155(8) 0.0203(8) 0.0229(8) -0.0104(7) -0.0038(6) -0.0010(6) C27A 0.0182(8) 0.0213(8) 0.0197(8) -0.0097(7) -0.0013(6) -0.0047(6) C28A 0.0247(9) 0.0198(8) 0.0222(8) -0.0068(7) -0.0051(7) -0.0022(7) C29A 0.0214(9) 0.0200(8) 0.0329(9) -0.0110(7) -0.0065(7) 0.0020(7) C30A 0.0191(8) 0.0235(9) 0.0276(9) -0.0136(7) -0.0003(7) 0.0004(7) C31A 0.0181(8) 0.0228(8) 0.0230(8) -0.0125(7) -0.0016(6) -0.0025(6) C32A 0.0202(8) 0.0240(8) 0.0203(8) -0.0108(7) -0.0016(6) -0.0015(7) C33A 0.0273(9) 0.0327(10) 0.0228(9) -0.0129(7) 0.0011(7) 0.0020(7) C34A 0.0253(9) 0.0232(8) 0.0191(8) -0.0080(7) -0.0040(7) -0.0031(7) O35A 0.0267(7) 0.0524(8) 0.0209(6) -0.0148(6) -0.0067(5) 0.0056(6) C36A 0.0290(9) 0.0201(8) 0.0156(8) -0.0048(6) -0.0022(7) 0.0000(7) C37A 0.0312(9) 0.0228(9) 0.0187(8) -0.0053(7) -0.0033(7) 0.0022(7) C38A 0.0299(10) 0.0286(9) 0.0248(9) -0.0041(7) -0.0008(7) 0.0107(8) C39A 0.0398(11) 0.0339(10) 0.0191(9) -0.0060(7) 0.0033(8) 0.0122(8) N7A 0.0188(7) 0.0220(7) 0.0205(7) -0.0077(6) -0.0062(5) 0.0012(5) C40A 0.0177(8) 0.0265(9) 0.0282(9) -0.0084(7) -0.0065(7) 0.0019(7) C41A 0.0257(9) 0.0312(10) 0.0352(10) -0.0166(8) -0.0064(8) 0.0030(7) C42A 0.0295(10) 0.0333(10) 0.0343(10) -0.0164(8) -0.0076(8) 0.0076(8) C43A 0.0317(10) 0.0451(12) 0.0407(11) -0.0241(9) -0.0008(8) -0.0003(9) C44A 0.0191(8) 0.0219(8) 0.0210(8) -0.0056(7) -0.0067(6) 0.0029(6) C45A 0.0207(9) 0.0243(9) 0.0264(9) -0.0041(7) -0.0049(7) -0.0004(7) C46A 0.0298(10) 0.0282(10) 0.0321(10) 0.0015(8) -0.0097(8) -0.0042(8) C47A 0.0299(11) 0.0262(10) 0.0733(15) -0.0062(10) -0.0139(10) 0.0026(8) C48A 0.0269(9) 0.0244(8) 0.0190(8) -0.0069(7) -0.0074(7) -0.0033(7) C49A 0.0306(10) 0.0305(9) 0.0217(8) -0.0095(7) -0.0002(7) -0.0090(8) C50A 0.0383(11) 0.0524(12) 0.0304(10) -0.0232(9) 0.0066(8) -0.0142(9) C51A 0.0334(11) 0.0462(12) 0.0579(13) -0.0329(11) 0.0085(9) -0.0057(9) C52A 0.0212(8) 0.0220(8) 0.0247(8) -0.0092(7) -0.0055(7) -0.0029(7) C53A 0.0272(9) 0.0233(9) 0.0325(9) -0.0085(7) -0.0080(7) 0.0003(7) C54A 0.0353(10) 0.0244(9) 0.0318(10) -0.0098(8) -0.0111(8) -0.0029(8) C55A 0.0443(11) 0.0237(9) 0.0356(10) -0.0068(8) -0.0119(9) -0.0038(8) Cl1B 0.0196(2) 0.0221(2) 0.02083(19) -0.00661(16) -0.00231(15) 0.00143(15) N1B 0.0272(8) 0.0401(9) 0.0178(7) -0.0085(7) -0.0043(6) 0.0081(7) N2B 0.0195(7) 0.0233(7) 0.0176(7) -0.0069(6) -0.0054(6) 0.0034(6) N3B 0.0186(7) 0.0190(7) 0.0174(7) -0.0080(6) -0.0019(6) 0.0031(6) N4B 0.0211(7) 0.0183(7) 0.0196(7) -0.0065(6) 0.0000(6) -0.0015(6) N5B 0.0240(8) 0.0168(7) 0.0243(7) -0.0078(6) -0.0035(6) 0.0035(6) N6B 0.0244(8) 0.0208(7) 0.0246(7) -0.0117(6) -0.0048(6) 0.0052(6) C7B 0.0347(10) 0.0301(9) 0.0213(9) -0.0095(7) 0.0005(7) 0.0072(8) C8B 0.0409(11) 0.0380(11) 0.0271(10) -0.0086(8) -0.0057(8) 0.0190(9) C9B 0.0365(10) 0.0309(10) 0.0193(8) -0.0058(7) -0.0062(7) 0.0105(8) C10B 0.0264(9) 0.0230(8) 0.0170(8) -0.0061(7) -0.0032(7) -0.0004(7) C11B 0.0247(9) 0.0306(9) 0.0202(8) -0.0070(7) -0.0052(7) 0.0006(7) O12B 0.0343(8) 0.0929(11) 0.0220(7) -0.0162(7) -0.0107(6) 0.0299(7) C13B 0.0162(8) 0.0169(8) 0.0231(8) -0.0090(6) -0.0051(6) -0.0006(6) C14B 0.0205(8) 0.0211(8) 0.0176(8) -0.0091(6) -0.0023(6) -0.0032(6) C15B 0.0192(8) 0.0220(8) 0.0211(8) -0.0099(7) -0.0018(6) -0.0017(6) C16B 0.0175(8) 0.0207(8) 0.0230(8) -0.0109(7) -0.0007(6) -0.0035(6) C17B 0.0181(8) 0.0237(9) 0.0321(9) -0.0147(7) -0.0020(7) 0.0007(7) C18B 0.0213(8) 0.0187(8) 0.0341(9) -0.0103(7) -0.0091(7) 0.0038(7) C19B 0.0223(8) 0.0202(8) 0.0249(8) -0.0066(7) -0.0068(7) -0.0010(7) C20B 0.0165(8) 0.0205(8) 0.0201(8) -0.0091(7) -0.0029(6) -0.0018(6) C21B 0.0274(9) 0.0328(10) 0.0250(9) -0.0132(8) 0.0021(7) 0.0025(8) C22B 0.0242(9) 0.0204(8) 0.0157(8) -0.0059(6) -0.0017(6) -0.0012(7) C23B 0.0254(9) 0.0268(9) 0.0216(8) -0.0086(7) -0.0073(7) 0.0004(7) C24B 0.0345(10) 0.0392(11) 0.0323(10) -0.0190(8) -0.0083(8) -0.0013(8) C25B 0.0214(8) 0.0217(8) 0.0163(8) -0.0054(6) -0.0052(6) 0.0038(7) C26B 0.0205(8) 0.0171(8) 0.0211(8) -0.0052(6) -0.0070(6) 0.0046(6) C27B 0.0184(8) 0.0204(8) 0.0226(8) -0.0066(7) -0.0058(7) 0.0050(6) C28B 0.0237(9) 0.0249(9) 0.0338(9) -0.0159(7) -0.0068(7) 0.0056(7) C29B 0.0245(9) 0.0213(9) 0.0449(11) -0.0146(8) -0.0053(8) 0.0000(7) C30B 0.0190(8) 0.0209(8) 0.0331(9) -0.0069(7) -0.0040(7) 0.0013(7) C31B 0.0181(8) 0.0191(8) 0.0208(8) -0.0042(6) -0.0059(6) 0.0040(6) C32B 0.0207(8) 0.0195(8) 0.0181(8) -0.0038(6) -0.0053(6) 0.0041(7) C33B 0.0246(9) 0.0253(9) 0.0227(8) -0.0059(7) -0.0008(7) -0.0007(7) C34B 0.0218(8) 0.0249(9) 0.0212(8) -0.0118(7) -0.0083(7) 0.0042(7) O35B 0.0229(6) 0.0213(6) 0.0377(7) -0.0126(5) -0.0056(5) 0.0059(5) C36B 0.0232(9) 0.0234(8) 0.0206(8) -0.0131(7) -0.0060(7) 0.0064(7) C37B 0.0281(9) 0.0264(9) 0.0222(8) -0.0120(7) -0.0062(7) 0.0061(7) C38B 0.0336(10) 0.0263(9) 0.0211(8) -0.0091(7) -0.0035(7) -0.0005(8) C39B 0.0258(9) 0.0325(9) 0.0245(9) -0.0167(8) -0.0009(7) -0.0002(7) N7B 0.0203(7) 0.0218(7) 0.0235(7) -0.0114(6) -0.0071(5) 0.0013(6) C40B 0.0289(9) 0.0230(8) 0.0230(8) -0.0114(7) -0.0089(7) 0.0003(7) C41B 0.0309(10) 0.0279(9) 0.0227(8) -0.0105(7) -0.0045(7) -0.0025(7) C42B 0.0341(10) 0.0333(10) 0.0257(9) -0.0140(8) -0.0069(8) 0.0048(8) C43B 0.0396(11) 0.0358(11) 0.0405(11) -0.0209(9) -0.0047(9) 0.0045(9) C44B 0.0219(8) 0.0237(8) 0.0226(8) -0.0091(7) -0.0086(7) 0.0034(7) C45B 0.0470(12) 0.0226(9) 0.0350(10) -0.0114(8) -0.0177(9) 0.0023(8) C46B 0.0413(11) 0.0249(9) 0.0403(11) -0.0069(8) -0.0145(9) 0.0012(8) C47B 0.0961(19) 0.0332(11) 0.0380(12) -0.0058(9) -0.0189(12) -0.0109(12) C48B 0.0181(8) 0.0244(9) 0.0296(9) -0.0104(7) -0.0085(7) -0.0002(7) C49B 0.0228(9) 0.0354(10) 0.0302(9) -0.0161(8) -0.0048(7) 0.0015(7) C50B 0.0217(9) 0.0347(10) 0.0362(10) -0.0142(8) -0.0065(7) 0.0030(7) C51B 0.0301(10) 0.0544(13) 0.0484(12) -0.0309(10) -0.0008(9) -0.0005(9) C52B 0.0216(8) 0.0223(8) 0.0272(9) -0.0125(7) -0.0062(7) -0.0024(7) C53B 0.0250(9) 0.0237(9) 0.0326(9) -0.0115(7) -0.0075(7) -0.0004(7) C54B 0.0315(10) 0.0281(9) 0.0313(9) -0.0101(8) -0.0086(8) -0.0049(8) C55B 0.0401(11) 0.0277(10) 0.0366(10) -0.0071(8) -0.0082(8) -0.0089(8) _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 N1A C7A 1.355(2) . ? N1A C10A 1.3733(19) . ? N1A H1A 0.892(17) . ? N2A C11A 1.3566(19) . ? N2A C20A 1.4200(19) . ? N2A H2A 0.796(17) . ? N3A C13A 1.364(2) . ? N3A C14A 1.3838(19) . ? N3A H3A 0.824(16) . ? N4A C26A 1.3717(19) . ? N4A C25A 1.3943(19) . ? N4A H4A 0.814(17) . ? N5A C34A 1.3612(19) . ? N5A C27A 1.4170(19) . ? N5A H5A 0.844(17) . ? N6A C39A 1.350(2) . ? N6A C36A 1.3733(19) . ? N6A H6A 0.857(19) . ? C7A C8A 1.373(2) . ? C7A H7A 0.9500 . ? C8A C9A 1.405(2) . ? C8A H8A 0.9500 . ? C9A C10A 1.381(2) . ? C9A H9A 0.9500 . ? C10A C11A 1.468(2) . ? C11A O12A 1.2336(17) . ? C13A C20A 1.404(2) . ? C13A C16A 1.417(2) . ? C14A C15A 1.373(2) . ? C14A C22A 1.510(2) . ? C15A C16A 1.437(2) . ? C15A C21A 1.497(2) . ? C16A C17A 1.404(2) . ? C17A C18A 1.372(2) . ? C17A H17A 0.9500 . ? C18A C19A 1.407(2) . ? C18A H18A 0.9500 . ? C19A C20A 1.393(2) . ? C19A H19A 0.9500 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C25A 1.510(2) . ? C22A C23A 1.547(2) . ? C22A H22A 1.0000 . ? C23A C24A 1.525(2) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C25A C32A 1.370(2) . ? C26A C27A 1.403(2) . ? C26A C31A 1.411(2) . ? C27A C28A 1.383(2) . ? C28A C29A 1.403(2) . ? C28A H28A 0.9500 . ? C29A C30A 1.380(2) . ? C29A H29A 0.9500 . ? C30A C31A 1.401(2) . ? C30A H30A 0.9500 . ? C31A C32A 1.446(2) . ? C32A C33A 1.505(2) . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A O35A 1.2378(18) . ? C34A C36A 1.457(2) . ? C36A C37A 1.379(2) . ? C37A C38A 1.405(2) . ? C37A H37A 0.9500 . ? C38A C39A 1.368(2) . ? C38A H38A 0.9500 . ? C39A H39A 0.9500 . ? N7A C52A 1.5139(19) . ? N7A C48A 1.5199(19) . ? N7A C44A 1.5226(18) . ? N7A C40A 1.5277(19) . ? C40A C41A 1.524(2) . ? C40A H40A 0.9900 . ? C40A H40B 0.9900 . ? C41A C42A 1.530(2) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A C43A 1.513(2) . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A C45A 1.518(2) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.516(2) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A C47A 1.506(3) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A C49A 1.527(2) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C50A 1.534(2) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A C51A 1.517(3) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C51A H51A 0.9800 . ? C51A H51B 0.9800 . ? C51A H51C 0.9800 . ? C52A C53A 1.516(2) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A C54A 1.521(2) . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C54A C55A 1.521(2) . ? C54A H54A 0.9900 . ? C54A H54B 0.9900 . ? C55A H55A 0.9800 . ? C55A H55B 0.9800 . ? C55A H55C 0.9800 . ? N1B C7B 1.345(2) . ? N1B C10B 1.371(2) . ? N1B H1B 0.84(2) . ? N2B C11B 1.3577(19) . ? N2B C20B 1.4208(19) . ? N2B H2B 0.878(17) . ? N3B C13B 1.3751(18) . ? N3B C14B 1.3918(19) . ? N3B H3B 0.816(18) . ? N4B C26B 1.3756(19) . ? N4B C25B 1.3869(19) . ? N4B H4B 0.867(18) . ? N5B C34B 1.3639(19) . ? N5B C27B 1.423(2) . ? N5B H5B 0.805(17) . ? N6B C39B 1.354(2) . ? N6B C36B 1.3720(19) . ? N6B H6B 0.855(17) . ? C7B C8B 1.366(2) . ? C7B H7B 0.9500 . ? C8B C9B 1.408(2) . ? C8B H8B 0.9500 . ? C9B C10B 1.373(2) . ? C9B H9B 0.9500 . ? C10B C11B 1.456(2) . ? C11B O12B 1.2333(19) . ? C13B C20B 1.404(2) . ? C13B C16B 1.408(2) . ? C14B C15B 1.368(2) . ? C14B C22B 1.509(2) . ? C15B C16B 1.444(2) . ? C15B C21B 1.503(2) . ? C16B C17B 1.398(2) . ? C17B C18B 1.380(2) . ? C17B H17B 0.9500 . ? C18B C19B 1.399(2) . ? C18B H18B 0.9500 . ? C19B C20B 1.388(2) . ? C19B H19B 0.9500 . ? C21B H21G 0.9800 . ? C21B H21H 0.9800 . ? C21B H21I 0.9800 . ? C21B H21J 0.9800 . ? C21B H21K 0.9800 . ? C21B H21L 0.9800 . ? C22B C25B 1.504(2) . ? C22B C23B 1.547(2) . ? C22B H22B 1.0000 . ? C23B C24B 1.524(2) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25B C32B 1.380(2) . ? C26B C27B 1.402(2) . ? C26B C31B 1.415(2) . ? C27B C28B 1.384(2) . ? C28B C29B 1.404(2) . ? C28B H28B 0.9500 . ? C29B C30B 1.373(2) . ? C29B H29B 0.9500 . ? C30B C31B 1.398(2) . ? C30B H30B 0.9500 . ? C31B C32B 1.441(2) . ? C32B C33B 1.498(2) . ? C33B H33G 0.9800 . ? C33B H33H 0.9800 . ? C33B H33I 0.9800 . ? C33B H33J 0.9800 . ? C33B H33K 0.9800 . ? C33B H33L 0.9800 . ? C34B O35B 1.2354(17) . ? C34B C36B 1.465(2) . ? C36B C37B 1.381(2) . ? C37B C38B 1.409(2) . ? C37B H37B 0.9500 . ? C38B C39B 1.371(2) . ? C38B H38B 0.9500 . ? C39B H39B 0.9500 . ? N7B C52B 1.5199(19) . ? N7B C48B 1.5205(19) . ? N7B C44B 1.5209(19) . ? N7B C40B 1.5217(19) . ? C40B C41B 1.522(2) . ? C40B H40C 0.9900 . ? C40B H40D 0.9900 . ? C41B C42B 1.532(2) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B C43B 1.519(2) . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B C45B 1.518(2) . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45B C46B 1.526(2) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B C47B 1.519(3) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B C49B 1.518(2) . ? C48B H48C 0.9900 . ? C48B H48D 0.9900 . ? C49B C50B 1.520(2) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50B C51B 1.511(2) . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? C51B H51D 0.9800 . ? C51B H51E 0.9800 . ? C51B H51F 0.9800 . ? C52B C53B 1.517(2) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? C53B C54B 1.522(2) . ? C53B H53C 0.9900 . ? C53B H53D 0.9900 . ? C54B C55B 1.522(2) . ? C54B H54C 0.9900 . ? C54B H54D 0.9900 . ? C55B H55D 0.9800 . ? C55B H55E 0.9800 . ? C55B H55F 0.9800 . ? 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 C7A N1A C10A 109.40(13) . . ? C7A N1A H1A 127.9(10) . . ? C10A N1A H1A 122.2(10) . . ? C11A N2A C20A 125.46(14) . . ? C11A N2A H2A 118.6(12) . . ? C20A N2A H2A 115.6(12) . . ? C13A N3A C14A 109.47(13) . . ? C13A N3A H3A 128.2(11) . . ? C14A N3A H3A 122.1(11) . . ? C26A N4A C25A 108.93(13) . . ? C26A N4A H4A 123.5(12) . . ? C25A N4A H4A 123.6(12) . . ? C34A N5A C27A 127.38(14) . . ? C34A N5A H5A 115.0(12) . . ? C27A N5A H5A 116.7(12) . . ? C39A N6A C36A 109.13(14) . . ? C39A N6A H6A 125.5(13) . . ? C36A N6A H6A 125.4(13) . . ? N1A C7A C8A 108.41(14) . . ? N1A C7A H7A 125.8 . . ? C8A C7A H7A 125.8 . . ? C7A C8A C9A 107.33(14) . . ? C7A C8A H8A 126.3 . . ? C9A C8A H8A 126.3 . . ? C10A C9A C8A 107.37(14) . . ? C10A C9A H9A 126.3 . . ? C8A C9A H9A 126.3 . . ? N1A C10A C9A 107.48(13) . . ? N1A C10A C11A 118.41(13) . . ? C9A C10A C11A 134.00(14) . . ? O12A C11A N2A 122.70(15) . . ? O12A C11A C10A 120.52(14) . . ? N2A C11A C10A 116.77(13) . . ? N3A C13A C20A 129.92(14) . . ? N3A C13A C16A 107.60(13) . . ? C20A C13A C16A 122.47(14) . . ? C15A C14A N3A 109.35(14) . . ? C15A C14A C22A 130.62(14) . . ? N3A C14A C22A 120.03(13) . . ? C14A C15A C16A 106.63(13) . . ? C14A C15A C21A 127.81(15) . . ? C16A C15A C21A 125.55(14) . . ? C17A C16A C13A 118.81(14) . . ? C17A C16A C15A 134.21(14) . . ? C13A C16A C15A 106.93(13) . . ? C18A C17A C16A 118.81(15) . . ? C18A C17A H17A 120.6 . . ? C16A C17A H17A 120.6 . . ? C17A C18A C19A 122.21(15) . . ? C17A C18A H18A 118.9 . . ? C19A C18A H18A 118.9 . . ? C20A C19A C18A 120.63(15) . . ? C20A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C19A C20A C13A 117.03(14) . . ? C19A C20A N2A 123.25(14) . . ? C13A C20A N2A 119.59(14) . . ? C15A C21A H21A 109.5 . . ? C15A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C15A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C15A C21A H21D 109.5 . . ? H21A C21A H21D 141.1 . . ? H21B C21A H21D 56.3 . . ? H21C C21A H21D 56.3 . . ? C15A C21A H21E 109.5 . . ? H21A C21A H21E 56.3 . . ? H21B C21A H21E 141.1 . . ? H21C C21A H21E 56.3 . . ? H21D C21A H21E 109.5 . . ? C15A C21A H21F 109.5 . . ? H21A C21A H21F 56.3 . . ? H21B C21A H21F 56.3 . . ? H21C C21A H21F 141.1 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C25A C22A C14A 112.40(12) . . ? C25A C22A C23A 111.32(12) . . ? C14A C22A C23A 112.37(12) . . ? C25A C22A H22A 106.8 . . ? C14A C22A H22A 106.8 . . ? C23A C22A H22A 106.8 . . ? C24A C23A C22A 112.92(13) . . ? C24A C23A H23A 109.0 . . ? C22A C23A H23A 109.0 . . ? C24A C23A H23B 109.0 . . ? C22A C23A H23B 109.0 . . ? H23A C23A H23B 107.8 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C32A C25A N4A 109.31(13) . . ? C32A C25A C22A 130.12(13) . . ? N4A C25A C22A 120.57(13) . . ? N4A C26A C27A 129.70(14) . . ? N4A C26A C31A 108.09(13) . . ? C27A C26A C31A 122.21(13) . . ? C28A C27A C26A 117.22(14) . . ? C28A C27A N5A 124.22(14) . . ? C26A C27A N5A 118.51(13) . . ? C27A C28A C29A 120.98(14) . . ? C27A C28A H28A 119.5 . . ? C29A C28A H28A 119.5 . . ? C30A C29A C28A 121.83(14) . . ? C30A C29A H29A 119.1 . . ? C28A C29A H29A 119.1 . . ? C29A C30A C31A 118.53(14) . . ? C29A C30A H30A 120.7 . . ? C31A C30A H30A 120.7 . . ? C30A C31A C26A 119.18(14) . . ? C30A C31A C32A 134.12(14) . . ? C26A C31A C32A 106.70(13) . . ? C25A C32A C31A 106.92(13) . . ? C25A C32A C33A 127.59(14) . . ? C31A C32A C33A 125.31(14) . . ? C32A C33A H33A 109.5 . . ? C32A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C32A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C32A C33A H33D 109.5 . . ? H33A C33A H33D 141.1 . . ? H33B C33A H33D 56.3 . . ? H33C C33A H33D 56.3 . . ? C32A C33A H33E 109.5 . . ? H33A C33A H33E 56.3 . . ? H33B C33A H33E 141.1 . . ? H33C C33A H33E 56.3 . . ? H33D C33A H33E 109.5 . . ? C32A C33A H33F 109.5 . . ? H33A C33A H33F 56.3 . . ? H33B C33A H33F 56.3 . . ? H33C C33A H33F 141.1 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? O35A C34A N5A 122.37(15) . . ? O35A C34A C36A 122.26(14) . . ? N5A C34A C36A 115.37(14) . . ? N6A C36A C37A 107.45(14) . . ? N6A C36A C34A 119.73(14) . . ? C37A C36A C34A 132.68(14) . . ? C36A C37A C38A 107.42(14) . . ? C36A C37A H37A 126.3 . . ? C38A C37A H37A 126.3 . . ? C39A C38A C37A 107.03(15) . . ? C39A C38A H38A 126.5 . . ? C37A C38A H38A 126.5 . . ? N6A C39A C38A 108.96(15) . . ? N6A C39A H39A 125.5 . . ? C38A C39A H39A 125.5 . . ? C52A N7A C48A 111.26(11) . . ? C52A N7A C44A 107.03(11) . . ? C48A N7A C44A 109.17(11) . . ? C52A N7A C40A 110.50(12) . . ? C48A N7A C40A 107.94(11) . . ? C44A N7A C40A 110.96(11) . . ? C41A C40A N7A 113.77(12) . . ? C41A C40A H40A 108.8 . . ? N7A C40A H40A 108.8 . . ? C41A C40A H40B 108.8 . . ? N7A C40A H40B 108.8 . . ? H40A C40A H40B 107.7 . . ? C40A C41A C42A 113.07(13) . . ? C40A C41A H41A 109.0 . . ? C42A C41A H41A 109.0 . . ? C40A C41A H41B 109.0 . . ? C42A C41A H41B 109.0 . . ? H41A C41A H41B 107.8 . . ? C43A C42A C41A 114.30(14) . . ? C43A C42A H42A 108.7 . . ? C41A C42A H42A 108.7 . . ? C43A C42A H42B 108.7 . . ? C41A C42A H42B 108.7 . . ? H42A C42A H42B 107.6 . . ? C42A C43A H43A 109.5 . . ? C42A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C42A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C45A C44A N7A 114.90(12) . . ? C45A C44A H44A 108.5 . . ? N7A C44A H44A 108.5 . . ? C45A C44A H44B 108.5 . . ? N7A C44A H44B 108.5 . . ? H44A C44A H44B 107.5 . . ? C46A C45A C44A 111.26(13) . . ? C46A C45A H45A 109.4 . . ? C44A C45A H45A 109.4 . . ? C46A C45A H45B 109.4 . . ? C44A C45A H45B 109.4 . . ? H45A C45A H45B 108.0 . . ? C47A C46A C45A 113.77(15) . . ? C47A C46A H46A 108.8 . . ? C45A C46A H46A 108.8 . . ? C47A C46A H46B 108.8 . . ? C45A C46A H46B 108.8 . . ? H46A C46A H46B 107.7 . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? N7A C48A C49A 115.01(12) . . ? N7A C48A H48A 108.5 . . ? C49A C48A H48A 108.5 . . ? N7A C48A H48B 108.5 . . ? C49A C48A H48B 108.5 . . ? H48A C48A H48B 107.5 . . ? C48A C49A C50A 110.56(13) . . ? C48A C49A H49A 109.5 . . ? C50A C49A H49A 109.5 . . ? C48A C49A H49B 109.5 . . ? C50A C49A H49B 109.5 . . ? H49A C49A H49B 108.1 . . ? C51A C50A C49A 111.50(15) . . ? C51A C50A H50A 109.3 . . ? C49A C50A H50A 109.3 . . ? C51A C50A H50B 109.3 . . ? C49A C50A H50B 109.3 . . ? H50A C50A H50B 108.0 . . ? C50A C51A H51A 109.5 . . ? C50A C51A H51B 109.5 . . ? H51A C51A H51B 109.5 . . ? C50A C51A H51C 109.5 . . ? H51A C51A H51C 109.5 . . ? H51B C51A H51C 109.5 . . ? N7A C52A C53A 114.83(12) . . ? N7A C52A H52A 108.6 . . ? C53A C52A H52A 108.6 . . ? N7A C52A H52B 108.6 . . ? C53A C52A H52B 108.6 . . ? H52A C52A H52B 107.5 . . ? C52A C53A C54A 110.90(13) . . ? C52A C53A H53A 109.5 . . ? C54A C53A H53A 109.5 . . ? C52A C53A H53B 109.5 . . ? C54A C53A H53B 109.5 . . ? H53A C53A H53B 108.0 . . ? C53A C54A C55A 112.07(14) . . ? C53A C54A H54A 109.2 . . ? C55A C54A H54A 109.2 . . ? C53A C54A H54B 109.2 . . ? C55A C54A H54B 109.2 . . ? H54A C54A H54B 107.9 . . ? C54A C55A H55A 109.5 . . ? C54A C55A H55B 109.5 . . ? H55A C55A H55B 109.5 . . ? C54A C55A H55C 109.5 . . ? H55A C55A H55C 109.5 . . ? H55B C55A H55C 109.5 . . ? C7B N1B C10B 109.92(14) . . ? C7B N1B H1B 121.8(14) . . ? C10B N1B H1B 127.6(14) . . ? C11B N2B C20B 126.00(13) . . ? C11B N2B H2B 115.9(11) . . ? C20B N2B H2B 117.7(11) . . ? C13B N3B C14B 109.02(13) . . ? C13B N3B H3B 124.2(13) . . ? C14B N3B H3B 124.0(12) . . ? C26B N4B C25B 109.30(13) . . ? C26B N4B H4B 125.3(12) . . ? C25B N4B H4B 124.7(12) . . ? C34B N5B C27B 125.53(14) . . ? C34B N5B H5B 116.9(12) . . ? C27B N5B H5B 117.3(12) . . ? C39B N6B C36B 109.74(14) . . ? C39B N6B H6B 124.9(11) . . ? C36B N6B H6B 125.2(11) . . ? N1B C7B C8B 108.21(15) . . ? N1B C7B H7B 125.9 . . ? C8B C7B H7B 125.9 . . ? C7B C8B C9B 107.41(15) . . ? C7B C8B H8B 126.3 . . ? C9B C8B H8B 126.3 . . ? C10B C9B C8B 107.24(14) . . ? C10B C9B H9B 126.4 . . ? C8B C9B H9B 126.4 . . ? N1B C10B C9B 107.22(14) . . ? N1B C10B C11B 118.25(14) . . ? C9B C10B C11B 134.52(14) . . ? O12B C11B N2B 121.98(15) . . ? O12B C11B C10B 120.41(14) . . ? N2B C11B C10B 117.60(14) . . ? N3B C13B C20B 130.13(14) . . ? N3B C13B C16B 107.75(13) . . ? C20B C13B C16B 122.11(13) . . ? C15B C14B N3B 109.35(13) . . ? C15B C14B C22B 129.99(14) . . ? N3B C14B C22B 120.66(13) . . ? C14B C15B C16B 106.81(13) . . ? C14B C15B C21B 127.79(14) . . ? C16B C15B C21B 125.32(14) . . ? C17B C16B C13B 119.54(14) . . ? C17B C16B C15B 133.40(14) . . ? C13B C16B C15B 107.05(13) . . ? C18B C17B C16B 118.47(14) . . ? C18B C17B H17B 120.8 . . ? C16B C17B H17B 120.8 . . ? C17B C18B C19B 121.67(14) . . ? C17B C18B H18B 119.2 . . ? C19B C18B H18B 119.2 . . ? C20B C19B C18B 121.24(14) . . ? C20B C19B H19B 119.4 . . ? C18B C19B H19B 119.4 . . ? C19B C20B C13B 116.95(14) . . ? C19B C20B N2B 124.13(13) . . ? C13B C20B N2B 118.90(13) . . ? C15B C21B H21G 109.5 . . ? C15B C21B H21H 109.5 . . ? H21G C21B H21H 109.5 . . ? C15B C21B H21I 109.5 . . ? H21G C21B H21I 109.5 . . ? H21H C21B H21I 109.5 . . ? C15B C21B H21J 109.5 . . ? H21G C21B H21J 141.1 . . ? H21H C21B H21J 56.3 . . ? H21I C21B H21J 56.3 . . ? C15B C21B H21K 109.5 . . ? H21G C21B H21K 56.3 . . ? H21H C21B H21K 141.1 . . ? H21I C21B H21K 56.3 . . ? H21J C21B H21K 109.5 . . ? C15B C21B H21L 109.5 . . ? H21G C21B H21L 56.3 . . ? H21H C21B H21L 56.3 . . ? H21I C21B H21L 141.1 . . ? H21J C21B H21L 109.5 . . ? H21K C21B H21L 109.5 . . ? C25B C22B C14B 111.98(12) . . ? C25B C22B C23B 112.57(13) . . ? C14B C22B C23B 112.13(12) . . ? C25B C22B H22B 106.6 . . ? C14B C22B H22B 106.6 . . ? C23B C22B H22B 106.6 . . ? C24B C23B C22B 111.87(13) . . ? C24B C23B H23C 109.2 . . ? C22B C23B H23C 109.2 . . ? C24B C23B H23D 109.2 . . ? C22B C23B H23D 109.2 . . ? H23C C23B H23D 107.9 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C32B C25B N4B 109.27(13) . . ? C32B C25B C22B 129.58(14) . . ? N4B C25B C22B 121.14(14) . . ? N4B C26B C27B 130.28(14) . . ? N4B C26B C31B 107.60(13) . . ? C27B C26B C31B 122.12(14) . . ? C28B C27B C26B 117.13(14) . . ? C28B C27B N5B 123.17(14) . . ? C26B C27B N5B 119.63(14) . . ? C27B C28B C29B 120.92(15) . . ? C27B C28B H28B 119.5 . . ? C29B C28B H28B 119.5 . . ? C30B C29B C28B 121.94(15) . . ? C30B C29B H29B 119.0 . . ? C28B C29B H29B 119.0 . . ? C29B C30B C31B 118.63(15) . . ? C29B C30B H30B 120.7 . . ? C31B C30B H30B 120.7 . . ? C30B C31B C26B 119.19(14) . . ? C30B C31B C32B 133.71(14) . . ? C26B C31B C32B 107.10(13) . . ? C25B C32B C31B 106.68(13) . . ? C25B C32B C33B 127.70(14) . . ? C31B C32B C33B 125.58(14) . . ? C32B C33B H33G 109.5 . . ? C32B C33B H33H 109.5 . . ? H33G C33B H33H 109.5 . . ? C32B C33B H33I 109.5 . . ? H33G C33B H33I 109.5 . . ? H33H C33B H33I 109.5 . . ? C32B C33B H33J 109.5 . . ? H33G C33B H33J 141.1 . . ? H33H C33B H33J 56.3 . . ? H33I C33B H33J 56.3 . . ? C32B C33B H33K 109.5 . . ? H33G C33B H33K 56.3 . . ? H33H C33B H33K 141.1 . . ? H33I C33B H33K 56.3 . . ? H33J C33B H33K 109.5 . . ? C32B C33B H33L 109.5 . . ? H33G C33B H33L 56.3 . . ? H33H C33B H33L 56.3 . . ? H33I C33B H33L 141.1 . . ? H33J C33B H33L 109.5 . . ? H33K C33B H33L 109.5 . . ? O35B C34B N5B 122.89(15) . . ? O35B C34B C36B 121.18(14) . . ? N5B C34B C36B 115.93(14) . . ? N6B C36B C37B 107.40(14) . . ? N6B C36B C34B 118.66(14) . . ? C37B C36B C34B 133.91(14) . . ? C36B C37B C38B 107.15(14) . . ? C36B C37B H37B 126.4 . . ? C38B C37B H37B 126.4 . . ? C39B C38B C37B 107.54(15) . . ? C39B C38B H38B 126.2 . . ? C37B C38B H38B 126.2 . . ? N6B C39B C38B 108.16(15) . . ? N6B C39B H39B 125.9 . . ? C38B C39B H39B 125.9 . . ? C52B N7B C48B 111.18(11) . . ? C52B N7B C44B 105.98(11) . . ? C48B N7B C44B 111.50(11) . . ? C52B N7B C40B 110.65(12) . . ? C48B N7B C40B 106.77(11) . . ? C44B N7B C40B 110.82(11) . . ? N7B C40B C41B 115.01(12) . . ? N7B C40B H40C 108.5 . . ? C41B C40B H40C 108.5 . . ? N7B C40B H40D 108.5 . . ? C41B C40B H40D 108.5 . . ? H40C C40B H40D 107.5 . . ? C40B C41B C42B 110.07(13) . . ? C40B C41B H41C 109.6 . . ? C42B C41B H41C 109.6 . . ? C40B C41B H41D 109.6 . . ? C42B C41B H41D 109.6 . . ? H41C C41B H41D 108.2 . . ? C43B C42B C41B 112.58(14) . . ? C43B C42B H42C 109.1 . . ? C41B C42B H42C 109.1 . . ? C43B C42B H42D 109.1 . . ? C41B C42B H42D 109.1 . . ? H42C C42B H42D 107.8 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C45B C44B N7B 116.17(12) . . ? C45B C44B H44C 108.2 . . ? N7B C44B H44C 108.2 . . ? C45B C44B H44D 108.2 . . ? N7B C44B H44D 108.2 . . ? H44C C44B H44D 107.4 . . ? C44B C45B C46B 110.85(14) . . ? C44B C45B H45C 109.5 . . ? C46B C45B H45C 109.5 . . ? C44B C45B H45D 109.5 . . ? C46B C45B H45D 109.5 . . ? H45C C45B H45D 108.1 . . ? C47B C46B C45B 113.34(16) . . ? C47B C46B H46C 108.9 . . ? C45B C46B H46C 108.9 . . ? C47B C46B H46D 108.9 . . ? C45B C46B H46D 108.9 . . ? H46C C46B H46D 107.7 . . ? C46B C47B H47D 109.5 . . ? C46B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C49B C48B N7B 115.37(12) . . ? C49B C48B H48C 108.4 . . ? N7B C48B H48C 108.4 . . ? C49B C48B H48D 108.4 . . ? N7B C48B H48D 108.4 . . ? H48C C48B H48D 107.5 . . ? C48B C49B C50B 110.64(13) . . ? C48B C49B H49C 109.5 . . ? C50B C49B H49C 109.5 . . ? C48B C49B H49D 109.5 . . ? C50B C49B H49D 109.5 . . ? H49C C49B H49D 108.1 . . ? C51B C50B C49B 112.51(14) . . ? C51B C50B H50C 109.1 . . ? C49B C50B H50C 109.1 . . ? C51B C50B H50D 109.1 . . ? C49B C50B H50D 109.1 . . ? H50C C50B H50D 107.8 . . ? C50B C51B H51D 109.5 . . ? C50B C51B H51E 109.5 . . ? H51D C51B H51E 109.5 . . ? C50B C51B H51F 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? C53B C52B N7B 116.27(12) . . ? C53B C52B H52C 108.2 . . ? N7B C52B H52C 108.2 . . ? C53B C52B H52D 108.2 . . ? N7B C52B H52D 108.2 . . ? H52C C52B H52D 107.4 . . ? C52B C53B C54B 110.22(13) . . ? C52B C53B H53C 109.6 . . ? C54B C53B H53C 109.6 . . ? C52B C53B H53D 109.6 . . ? C54B C53B H53D 109.6 . . ? H53C C53B H53D 108.1 . . ? C53B C54B C55B 113.16(14) . . ? C53B C54B H54C 108.9 . . ? C55B C54B H54C 108.9 . . ? C53B C54B H54D 108.9 . . ? C55B C54B H54D 108.9 . . ? H54C C54B H54D 107.8 . . ? C54B C55B H55D 109.5 . . ? C54B C55B H55E 109.5 . . ? H55D C55B H55E 109.5 . . ? C54B C55B H55F 109.5 . . ? H55D C55B H55F 109.5 . . ? H55E C55B H55F 109.5 . . ? 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 C10A N1A C7A C8A -0.85(17) . . . . ? N1A C7A C8A C9A 0.67(18) . . . . ? C7A C8A C9A C10A -0.24(18) . . . . ? C7A N1A C10A C9A 0.69(17) . . . . ? C7A N1A C10A C11A 177.41(13) . . . . ? C8A C9A C10A N1A -0.27(17) . . . . ? C8A C9A C10A C11A -176.25(16) . . . . ? C20A N2A C11A O12A -5.5(2) . . . . ? C20A N2A C11A C10A 174.70(13) . . . . ? N1A C10A C11A O12A -15.8(2) . . . . ? C9A C10A C11A O12A 159.85(16) . . . . ? N1A C10A C11A N2A 163.97(13) . . . . ? C9A C10A C11A N2A -20.4(3) . . . . ? C14A N3A C13A C20A 177.61(15) . . . . ? C14A N3A C13A C16A -1.26(16) . . . . ? C13A N3A C14A C15A 1.51(17) . . . . ? C13A N3A C14A C22A -178.03(13) . . . . ? N3A C14A C15A C16A -1.11(17) . . . . ? C22A C14A C15A C16A 178.37(14) . . . . ? N3A C14A C15A C21A 178.31(14) . . . . ? C22A C14A C15A C21A -2.2(3) . . . . ? N3A C13A C16A C17A 178.58(13) . . . . ? C20A C13A C16A C17A -0.4(2) . . . . ? N3A C13A C16A C15A 0.56(16) . . . . ? C20A C13A C16A C15A -178.41(13) . . . . ? C14A C15A C16A C17A -177.23(16) . . . . ? C21A C15A C16A C17A 3.3(3) . . . . ? C14A C15A C16A C13A 0.34(16) . . . . ? C21A C15A C16A C13A -179.10(14) . . . . ? C13A C16A C17A C18A -0.9(2) . . . . ? C15A C16A C17A C18A 176.41(16) . . . . ? C16A C17A C18A C19A 1.1(2) . . . . ? C17A C18A C19A C20A 0.1(2) . . . . ? C18A C19A C20A C13A -1.3(2) . . . . ? C18A C19A C20A N2A -177.26(14) . . . . ? N3A C13A C20A C19A -177.20(14) . . . . ? C16A C13A C20A C19A 1.5(2) . . . . ? N3A C13A C20A N2A -1.1(2) . . . . ? C16A C13A C20A N2A 177.60(13) . . . . ? C11A N2A C20A C19A -30.5(2) . . . . ? C11A N2A C20A C13A 153.69(14) . . . . ? C15A C14A C22A C25A -102.33(18) . . . . ? N3A C14A C22A C25A 77.10(17) . . . . ? C15A C14A C22A C23A 131.17(16) . . . . ? N3A C14A C22A C23A -49.40(18) . . . . ? C25A C22A C23A C24A -177.33(13) . . . . ? C14A C22A C23A C24A -50.25(17) . . . . ? C26A N4A C25A C32A 1.85(17) . . . . ? C26A N4A C25A C22A -178.24(13) . . . . ? C14A C22A C25A C32A 130.60(17) . . . . ? C23A C22A C25A C32A -102.33(18) . . . . ? C14A C22A C25A N4A -49.29(19) . . . . ? C23A C22A C25A N4A 77.77(17) . . . . ? C25A N4A C26A C27A 176.60(15) . . . . ? C25A N4A C26A C31A -2.38(17) . . . . ? N4A C26A C27A C28A 178.45(15) . . . . ? C31A C26A C27A C28A -2.7(2) . . . . ? N4A C26A C27A N5A -4.2(2) . . . . ? C31A C26A C27A N5A 174.65(13) . . . . ? C34A N5A C27A C28A -20.0(2) . . . . ? C34A N5A C27A C26A 162.86(14) . . . . ? C26A C27A C28A C29A 0.8(2) . . . . ? N5A C27A C28A C29A -176.39(14) . . . . ? C27A C28A C29A C30A 1.1(2) . . . . ? C28A C29A C30A C31A -1.2(2) . . . . ? C29A C30A C31A C26A -0.7(2) . . . . ? C29A C30A C31A C32A 179.00(16) . . . . ? N4A C26A C31A C30A -178.24(13) . . . . ? C27A C26A C31A C30A 2.7(2) . . . . ? N4A C26A C31A C32A 2.00(17) . . . . ? C27A C26A C31A C32A -177.07(13) . . . . ? N4A C25A C32A C31A -0.57(17) . . . . ? C22A C25A C32A C31A 179.53(15) . . . . ? N4A C25A C32A C33A -175.86(15) . . . . ? C22A C25A C32A C33A 4.2(3) . . . . ? C30A C31A C32A C25A 179.41(17) . . . . ? C26A C31A C32A C25A -0.87(17) . . . . ? C30A C31A C32A C33A -5.2(3) . . . . ? C26A C31A C32A C33A 174.56(14) . . . . ? C27A N5A C34A O35A -15.1(2) . . . . ? C27A N5A C34A C36A 164.26(14) . . . . ? C39A N6A C36A C37A 0.26(19) . . . . ? C39A N6A C36A C34A 176.62(14) . . . . ? O35A C34A C36A N6A -7.6(2) . . . . ? N5A C34A C36A N6A 173.08(14) . . . . ? O35A C34A C36A C37A 167.69(17) . . . . ? N5A C34A C36A C37A -11.6(3) . . . . ? N6A C36A C37A C38A 0.10(18) . . . . ? C34A C36A C37A C38A -175.60(16) . . . . ? C36A C37A C38A C39A -0.41(19) . . . . ? C36A N6A C39A C38A -0.5(2) . . . . ? C37A C38A C39A N6A 0.6(2) . . . . ? C52A N7A C40A C41A 61.68(16) . . . . ? C48A N7A C40A C41A -176.46(13) . . . . ? C44A N7A C40A C41A -56.88(17) . . . . ? N7A C40A C41A C42A 169.85(13) . . . . ? C40A C41A C42A C43A -63.12(19) . . . . ? C52A N7A C44A C45A -169.58(13) . . . . ? C48A N7A C44A C45A 69.90(16) . . . . ? C40A N7A C44A C45A -48.94(17) . . . . ? N7A C44A C45A C46A 179.68(13) . . . . ? C44A C45A C46A C47A 72.21(19) . . . . ? C52A N7A C48A C49A -43.65(17) . . . . ? C44A N7A C48A C49A 74.25(16) . . . . ? C40A N7A C48A C49A -165.05(13) . . . . ? N7A C48A C49A C50A -153.07(14) . . . . ? C48A C49A C50A C51A 82.19(18) . . . . ? C48A N7A C52A C53A -61.30(17) . . . . ? C44A N7A C52A C53A 179.52(13) . . . . ? C40A N7A C52A C53A 58.59(17) . . . . ? N7A C52A C53A C54A 165.11(13) . . . . ? C52A C53A C54A C55A 174.56(14) . . . . ? C10B N1B C7B C8B 0.1(2) . . . . ? N1B C7B C8B C9B -0.2(2) . . . . ? C7B C8B C9B C10B 0.2(2) . . . . ? C7B N1B C10B C9B 0.05(19) . . . . ? C7B N1B C10B C11B 179.62(14) . . . . ? C8B C9B C10B N1B -0.18(19) . . . . ? C8B C9B C10B C11B -179.64(18) . . . . ? C20B N2B C11B O12B -9.9(3) . . . . ? C20B N2B C11B C10B 171.51(14) . . . . ? N1B C10B C11B O12B -2.2(2) . . . . ? C9B C10B C11B O12B 177.25(19) . . . . ? N1B C10B C11B N2B 176.40(14) . . . . ? C9B C10B C11B N2B -4.2(3) . . . . ? C14B N3B C13B C20B 177.96(15) . . . . ? C14B N3B C13B C16B -1.36(16) . . . . ? C13B N3B C14B C15B 0.75(17) . . . . ? C13B N3B C14B C22B -178.62(13) . . . . ? N3B C14B C15B C16B 0.15(17) . . . . ? C22B C14B C15B C16B 179.44(14) . . . . ? N3B C14B C15B C21B -176.73(15) . . . . ? C22B C14B C15B C21B 2.6(3) . . . . ? N3B C13B C16B C17B -179.52(13) . . . . ? C20B C13B C16B C17B 1.1(2) . . . . ? N3B C13B C16B C15B 1.42(16) . . . . ? C20B C13B C16B C15B -177.96(13) . . . . ? C14B C15B C16B C17B -179.84(16) . . . . ? C21B C15B C16B C17B -2.9(3) . . . . ? C14B C15B C16B C13B -0.97(17) . . . . ? C21B C15B C16B C13B 176.01(14) . . . . ? C13B C16B C17B C18B -1.2(2) . . . . ? C15B C16B C17B C18B 177.56(16) . . . . ? C16B C17B C18B C19B 0.2(2) . . . . ? C17B C18B C19B C20B 1.0(2) . . . . ? C18B C19B C20B C13B -1.1(2) . . . . ? C18B C19B C20B N2B -179.41(14) . . . . ? N3B C13B C20B C19B -179.19(15) . . . . ? C16B C13B C20B C19B 0.0(2) . . . . ? N3B C13B C20B N2B -0.8(2) . . . . ? C16B C13B C20B N2B 178.48(13) . . . . ? C11B N2B C20B C19B -18.8(2) . . . . ? C11B N2B C20B C13B 162.86(15) . . . . ? C15B C14B C22B C25B 128.72(17) . . . . ? N3B C14B C22B C25B -52.06(19) . . . . ? C15B C14B C22B C23B -103.62(18) . . . . ? N3B C14B C22B C23B 75.60(17) . . . . ? C25B C22B C23B C24B -169.82(13) . . . . ? C14B C22B C23B C24B 62.84(17) . . . . ? C26B N4B C25B C32B 1.63(16) . . . . ? C26B N4B C25B C22B -177.36(13) . . . . ? C14B C22B C25B C32B -101.16(18) . . . . ? C23B C22B C25B C32B 131.42(16) . . . . ? C14B C22B C25B N4B 77.61(17) . . . . ? C23B C22B C25B N4B -49.81(18) . . . . ? C25B N4B C26B C27B 177.20(15) . . . . ? C25B N4B C26B C31B -2.12(16) . . . . ? N4B C26B C27B C28B -178.50(15) . . . . ? C31B C26B C27B C28B 0.7(2) . . . . ? N4B C26B C27B N5B -1.4(2) . . . . ? C31B C26B C27B N5B 177.83(13) . . . . ? C34B N5B C27B C28B -34.5(2) . . . . ? C34B N5B C27B C26B 148.63(15) . . . . ? C26B C27B C28B C29B -2.4(2) . . . . ? N5B C27B C28B C29B -179.33(14) . . . . ? C27B C28B C29B C30B 1.6(2) . . . . ? C28B C29B C30B C31B 1.0(2) . . . . ? C29B C30B C31B C26B -2.5(2) . . . . ? C29B C30B C31B C32B 176.56(16) . . . . ? N4B C26B C31B C30B -178.88(13) . . . . ? C27B C26B C31B C30B 1.7(2) . . . . ? N4B C26B C31B C32B 1.80(16) . . . . ? C27B C26B C31B C32B -177.59(13) . . . . ? N4B C25B C32B C31B -0.47(16) . . . . ? C22B C25B C32B C31B 178.41(14) . . . . ? N4B C25B C32B C33B 177.40(14) . . . . ? C22B C25B C32B C33B -3.7(3) . . . . ? C30B C31B C32B C25B 180.00(16) . . . . ? C26B C31B C32B C25B -0.81(16) . . . . ? C30B C31B C32B C33B 2.1(3) . . . . ? C26B C31B C32B C33B -178.74(14) . . . . ? C27B N5B C34B O35B -4.7(2) . . . . ? C27B N5B C34B C36B 175.86(14) . . . . ? C39B N6B C36B C37B 0.63(17) . . . . ? C39B N6B C36B C34B 178.80(13) . . . . ? O35B C34B C36B N6B -16.7(2) . . . . ? N5B C34B C36B N6B 162.78(13) . . . . ? O35B C34B C36B C37B 160.89(16) . . . . ? N5B C34B C36B C37B -19.6(3) . . . . ? N6B C36B C37B C38B -0.20(17) . . . . ? C34B C36B C37B C38B -177.97(16) . . . . ? C36B C37B C38B C39B -0.30(18) . . . . ? C36B N6B C39B C38B -0.82(18) . . . . ? C37B C38B C39B N6B 0.68(18) . . . . ? C52B N7B C40B C41B -47.89(16) . . . . ? C48B N7B C40B C41B -169.01(13) . . . . ? C44B N7B C40B C41B 69.37(16) . . . . ? N7B C40B C41B C42B -165.21(13) . . . . ? C40B C41B C42B C43B 77.30(17) . . . . ? C52B N7B C44B C45B 179.10(14) . . . . ? C48B N7B C44B C45B -59.78(17) . . . . ? C40B N7B C44B C45B 59.01(17) . . . . ? N7B C44B C45B C46B 175.32(14) . . . . ? C44B C45B C46B C47B -70.9(2) . . . . ? C52B N7B C48B C49B 69.26(16) . . . . ? C44B N7B C48B C49B -48.78(17) . . . . ? C40B N7B C48B C49B -169.97(13) . . . . ? N7B C48B C49B C50B -173.84(13) . . . . ? C48B C49B C50B C51B -172.47(15) . . . . ? C48B N7B C52B C53B 60.47(17) . . . . ? C44B N7B C52B C53B -178.20(13) . . . . ? C40B N7B C52B C53B -58.00(17) . . . . ? N7B C52B C53B C54B 162.92(13) . . . . ? C52B C53B C54B C55B 179.76(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A O35B 0.892(17) 1.969(17) 2.8168(17) 158.2(15) 2_656 N2A H2A Cl1A 0.796(17) 2.619(17) 3.3990(15) 166.7(16) . N3A H3A Cl1A 0.824(16) 2.292(17) 3.0979(14) 166.3(15) . N4A H4A Cl1A 0.814(17) 2.466(17) 3.2724(14) 170.9(15) . N5A H5A Cl1A 0.844(17) 2.884(18) 3.7029(15) 163.9(15) . N6A H6A O35A 0.857(19) 2.024(19) 2.8246(18) 155.3(17) 2_565 N1B H1B O12B 0.84(2) 1.97(2) 2.7636(19) 159(2) 2_566 N2B H2B Cl1B 0.878(17) 2.711(17) 3.5704(14) 166.5(14) . N3B H3B Cl1B 0.816(18) 2.382(18) 3.1955(14) 174.8(17) . N4B H4B Cl1B 0.867(18) 2.264(18) 3.1128(14) 166.0(16) . N5B H5B Cl1B 0.805(17) 2.646(18) 3.4269(15) 163.9(16) . N6B H6B O12A 0.855(17) 1.917(17) 2.7387(17) 160.5(16) 2_656 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.319 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.044 # Attachment '1b_H2O.CIF' data_p257 _database_code_depnum_ccdc_archive 'CCDC 707058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H34 N4 O3' _chemical_formula_weight 558.66 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5822(6) _cell_length_b 13.6329(5) _cell_length_c 15.4897(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.956(4) _cell_angle_gamma 90.00 _cell_volume 2835.45(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26227 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 28.71 _reflns_number_total 6833 _reflns_number_gt 4567 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material SHELXTL-97 _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^)+(0.0533P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6833 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.03415(7) 0.60486(7) 0.35718(7) 0.0201(2) Uani 1 1 d . . . N2 N -0.23384(7) 0.69997(7) 0.29611(7) 0.0200(2) Uani 1 1 d . . . N3 N -0.28126(7) 0.95138(7) 0.32507(6) 0.0206(2) Uani 1 1 d . . . N4 N -0.12772(8) 1.10533(7) 0.41979(7) 0.0242(2) Uani 1 1 d . . . C5 C 0.07773(9) 0.71656(8) 0.27314(8) 0.0234(3) Uani 1 1 d . . . H5 H 0.0117 0.7393 0.2584 0.028 Uiso 1 1 calc R . . C6 C 0.14488(9) 0.77517(9) 0.25377(8) 0.0276(3) Uani 1 1 d . . . H6 H 0.1250 0.8379 0.2260 0.033 Uiso 1 1 calc R . . C7 C 0.24029(10) 0.74243(10) 0.27488(9) 0.0318(3) Uani 1 1 d . . . H7 H 0.2863 0.7826 0.2615 0.038 Uiso 1 1 calc R . . C8 C 0.26982(9) 0.65127(10) 0.31552(9) 0.0306(3) Uani 1 1 d . . . H8 H 0.3360 0.6293 0.3302 0.037 Uiso 1 1 calc R . . C9 C 0.20285(9) 0.59191(9) 0.33487(8) 0.0253(3) Uani 1 1 d . . . H9 H 0.2230 0.5291 0.3623 0.030 Uiso 1 1 calc R . . C10 C 0.10617(9) 0.62453(8) 0.31404(8) 0.0209(3) Uani 1 1 d . . . O11 O 0.03431(6) 0.46834(6) 0.32174(6) 0.0256(2) Uani 1 1 d . . . C12 C 0.03348(8) 0.55850(9) 0.33178(8) 0.0201(3) Uani 1 1 d . . . C13 C -0.20590(8) 0.61196(8) 0.34266(8) 0.0195(3) Uani 1 1 d . . . C14 C -0.33183(8) 0.71953(8) 0.28242(8) 0.0203(3) Uani 1 1 d . . . C15 C -0.36736(9) 0.64541(9) 0.32021(8) 0.0228(3) Uani 1 1 d . . . C16 C -0.28847(9) 0.57537(8) 0.35903(8) 0.0220(3) Uani 1 1 d . . . C17 C -0.28005(9) 0.48414(9) 0.40338(8) 0.0256(3) Uani 1 1 d . . . H17 H -0.3343 0.4581 0.4155 0.031 Uiso 1 1 calc R . . C18 C -0.19214(9) 0.43293(9) 0.42901(8) 0.0268(3) Uani 1 1 d . . . H18 H -0.1869 0.3704 0.4577 0.032 Uiso 1 1 calc R . . C19 C -0.11010(9) 0.47051(8) 0.41400(8) 0.0235(3) Uani 1 1 d . . . H19 H -0.0500 0.4338 0.4334 0.028 Uiso 1 1 calc R . . C20 C -0.11588(8) 0.56076(8) 0.37109(8) 0.0197(3) Uani 1 1 d . . . C21 C -0.46947(9) 0.63848(9) 0.32187(9) 0.0296(3) Uani 1 1 d . . . H21A H -0.5179 0.6701 0.2658 0.044 Uiso 1 1 calc R . . H21B H -0.4698 0.6715 0.3780 0.044 Uiso 1 1 calc R . . H21C H -0.4874 0.5693 0.3229 0.044 Uiso 1 1 calc R . . C22 C -0.38497(9) 0.80996(8) 0.23109(8) 0.0217(3) Uani 1 1 d . . . H22 H -0.4576 0.7944 0.2079 0.026 Uiso 1 1 calc R . . C23 C -0.36385(9) 0.83080(9) 0.14327(8) 0.0256(3) Uani 1 1 d . . . H23A H -0.2932 0.8502 0.1627 0.031 Uiso 1 1 calc R . . H23B H -0.3742 0.7698 0.1059 0.031 Uiso 1 1 calc R . . C24 C -0.42922(10) 0.91072(10) 0.08229(9) 0.0369(3) Uani 1 1 d . . . H24A H -0.4109 0.9224 0.0286 0.055 Uiso 1 1 calc R . . H24B H -0.4200 0.9712 0.1190 0.055 Uiso 1 1 calc R . . H24C H -0.4991 0.8904 0.0597 0.055 Uiso 1 1 calc R . . C25 C -0.36927(8) 0.89729(8) 0.29511(8) 0.0202(3) Uani 1 1 d . . . C26 C -0.28817(9) 1.02616(8) 0.38242(8) 0.0214(3) Uani 1 1 d . . . C27 C -0.22069(9) 1.10085(9) 0.42942(8) 0.0227(3) Uani 1 1 d . . . C28 C -0.24969(10) 1.16658(9) 0.48246(8) 0.0286(3) Uani 1 1 d . . . H28 H -0.2054 1.2174 0.5157 0.034 Uiso 1 1 calc R . . C29 C -0.34299(10) 1.15926(10) 0.48779(9) 0.0338(3) Uani 1 1 d . . . H29 H -0.3608 1.2055 0.5244 0.041 Uiso 1 1 calc R . . C30 C -0.40969(10) 1.08680(9) 0.44138(9) 0.0310(3) Uani 1 1 d . . . H30 H -0.4730 1.0830 0.4453 0.037 Uiso 1 1 calc R . . C31 C -0.38198(9) 1.01878(9) 0.38825(8) 0.0239(3) Uani 1 1 d . . . C32 C -0.43214(9) 0.93629(9) 0.33222(8) 0.0237(3) Uani 1 1 d . . . C33 C -0.53500(9) 0.90311(10) 0.31902(9) 0.0311(3) Uani 1 1 d . . . H33A H -0.5325 0.8694 0.3758 0.047 Uiso 1 1 calc R . . H33B H -0.5605 0.8581 0.2656 0.047 Uiso 1 1 calc R . . H33C H -0.5791 0.9602 0.3071 0.047 Uiso 1 1 calc R . . C34 C -0.04294(9) 1.15062(8) 0.47640(8) 0.0242(3) Uani 1 1 d . . . C36 C 0.04495(9) 1.14113(9) 0.45091(8) 0.0246(3) Uani 1 1 d . . . O35 O -0.03682(6) 1.19663(6) 0.54778(6) 0.0293(2) Uani 1 1 d . . . C37 C 0.06195(9) 1.05945(9) 0.40526(8) 0.0267(3) Uani 1 1 d . . . H37 H 0.0144 1.0079 0.3865 0.032 Uiso 1 1 calc R . . C38 C 0.14730(10) 1.05229(10) 0.38676(9) 0.0311(3) Uani 1 1 d . . . H38 H 0.1580 0.9961 0.3556 0.037 Uiso 1 1 calc R . . C39 C 0.21686(10) 1.12712(10) 0.41366(9) 0.0352(3) Uani 1 1 d . . . H39 H 0.2756 1.1223 0.4014 0.042 Uiso 1 1 calc R . . C40 C 0.20059(11) 1.20936(11) 0.45866(9) 0.0396(4) Uani 1 1 d . . . H40 H 0.2483 1.2609 0.4770 0.048 Uiso 1 1 calc R . . C41 C 0.11530(10) 1.21661(10) 0.47695(9) 0.0335(3) Uani 1 1 d . . . H41 H 0.1045 1.2733 0.5074 0.040 Uiso 1 1 calc R . . H1 H -0.0228(9) 0.6646(9) 0.3725(8) 0.025(4) Uiso 1 1 d . . . H2 H -0.1935(10) 0.7390(10) 0.2793(9) 0.038(4) Uiso 1 1 d . . . H3 H -0.2242(10) 0.9340(10) 0.3155(9) 0.035(4) Uiso 1 1 d . . . H4 H -0.1243(9) 1.0798(10) 0.3711(9) 0.030(4) Uiso 1 1 d . . . O1S O -0.11410(6) 0.87228(6) 0.28810(7) 0.0250(2) Uani 1 1 d . . . H1SA H -0.0656(11) 0.8574(10) 0.3372(11) 0.037 Uiso 1 1 d . . . H1SB H -0.0911(10) 0.9020(10) 0.2514(10) 0.037 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0208(5) 0.0160(5) 0.0258(5) -0.0012(4) 0.0115(4) -0.0018(4) N2 0.0186(5) 0.0192(5) 0.0247(5) 0.0002(4) 0.0112(4) -0.0028(4) N3 0.0196(5) 0.0205(5) 0.0230(5) -0.0014(4) 0.0099(4) -0.0007(4) N4 0.0283(6) 0.0249(6) 0.0196(5) -0.0029(4) 0.0096(5) -0.0061(5) C5 0.0258(7) 0.0237(6) 0.0231(6) -0.0035(5) 0.0123(5) 0.0001(5) C6 0.0366(8) 0.0228(6) 0.0278(7) -0.0025(5) 0.0172(6) -0.0044(6) C7 0.0340(8) 0.0345(8) 0.0332(7) -0.0087(6) 0.0198(6) -0.0158(6) C8 0.0197(6) 0.0407(8) 0.0336(7) -0.0085(6) 0.0129(6) -0.0044(6) C9 0.0236(7) 0.0257(6) 0.0280(6) -0.0046(5) 0.0114(5) 0.0002(5) C10 0.0224(6) 0.0215(6) 0.0199(6) -0.0043(5) 0.0095(5) -0.0017(5) O11 0.0302(5) 0.0189(4) 0.0326(5) -0.0017(4) 0.0176(4) 0.0007(4) C12 0.0199(6) 0.0213(6) 0.0182(6) -0.0003(5) 0.0064(5) 0.0005(5) C13 0.0228(6) 0.0178(6) 0.0186(6) -0.0029(5) 0.0088(5) -0.0044(5) C14 0.0187(6) 0.0214(6) 0.0219(6) -0.0036(5) 0.0090(5) -0.0018(5) C15 0.0225(6) 0.0233(6) 0.0246(6) -0.0031(5) 0.0113(5) -0.0038(5) C16 0.0224(6) 0.0227(6) 0.0231(6) -0.0035(5) 0.0113(5) -0.0051(5) C17 0.0277(7) 0.0241(6) 0.0296(7) 0.0003(5) 0.0162(6) -0.0063(5) C18 0.0353(8) 0.0196(6) 0.0275(6) 0.0025(5) 0.0146(6) -0.0049(6) C19 0.0255(7) 0.0221(6) 0.0232(6) -0.0007(5) 0.0098(5) 0.0003(5) C20 0.0211(6) 0.0191(6) 0.0210(6) -0.0038(5) 0.0107(5) -0.0041(5) C21 0.0243(7) 0.0301(7) 0.0392(7) 0.0002(6) 0.0175(6) -0.0045(6) C22 0.0191(6) 0.0225(6) 0.0235(6) -0.0016(5) 0.0082(5) -0.0019(5) C23 0.0264(7) 0.0260(7) 0.0247(6) -0.0017(5) 0.0104(5) 0.0015(5) C24 0.0424(9) 0.0383(8) 0.0304(7) 0.0036(6) 0.0147(6) 0.0095(7) C25 0.0189(6) 0.0202(6) 0.0216(6) 0.0029(5) 0.0079(5) -0.0005(5) C26 0.0256(7) 0.0207(6) 0.0182(6) 0.0017(5) 0.0090(5) 0.0004(5) C27 0.0258(7) 0.0217(6) 0.0205(6) 0.0022(5) 0.0088(5) -0.0017(5) C28 0.0370(8) 0.0218(7) 0.0269(7) -0.0027(5) 0.0124(6) -0.0043(6) C29 0.0412(8) 0.0306(7) 0.0343(7) -0.0075(6) 0.0200(6) 0.0019(6) C30 0.0318(7) 0.0336(7) 0.0326(7) -0.0037(6) 0.0180(6) 0.0006(6) C31 0.0254(7) 0.0246(6) 0.0233(6) 0.0018(5) 0.0112(5) 0.0013(5) C32 0.0228(6) 0.0248(6) 0.0245(6) 0.0004(5) 0.0105(5) 0.0008(5) C33 0.0242(7) 0.0353(7) 0.0376(7) -0.0048(6) 0.0163(6) -0.0012(6) C34 0.0319(7) 0.0173(6) 0.0206(6) 0.0031(5) 0.0072(5) -0.0053(5) C36 0.0278(7) 0.0256(6) 0.0165(6) 0.0030(5) 0.0043(5) -0.0071(5) O35 0.0358(5) 0.0256(5) 0.0241(4) -0.0048(4) 0.0093(4) -0.0063(4) C37 0.0273(7) 0.0223(6) 0.0254(6) 0.0039(5) 0.0045(5) -0.0052(5) C38 0.0343(8) 0.0288(7) 0.0278(7) 0.0042(6) 0.0094(6) 0.0007(6) C39 0.0321(8) 0.0459(9) 0.0284(7) 0.0045(6) 0.0128(6) -0.0072(7) C40 0.0411(9) 0.0479(9) 0.0324(7) -0.0094(7) 0.0172(7) -0.0254(7) C41 0.0417(8) 0.0341(8) 0.0271(7) -0.0071(6) 0.0161(6) -0.0158(6) O1S 0.0225(5) 0.0273(5) 0.0271(5) 0.0036(4) 0.0117(4) -0.0022(4) _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 N1 C12 1.3526(14) . ? N1 C20 1.4243(14) . ? N1 H1 0.846(13) . ? N2 C13 1.3771(14) . ? N2 C14 1.3861(14) . ? N2 H2 0.903(14) . ? N3 C26 1.3814(15) . ? N3 C25 1.3934(15) . ? N3 H3 0.931(13) . ? N4 C34 1.3540(15) . ? N4 C27 1.4218(15) . ? N4 H4 0.849(13) . ? C5 C6 1.3844(16) . ? C5 C10 1.3938(16) . ? C5 H5 0.9500 . ? C6 C7 1.3737(18) . ? C6 H6 0.9500 . ? C7 C8 1.3837(18) . ? C7 H7 0.9500 . ? C8 C9 1.3882(17) . ? C8 H8 0.9500 . ? C9 C10 1.3909(16) . ? C9 H9 0.9500 . ? C10 C12 1.4955(16) . ? O11 C12 1.2395(13) . ? C13 C20 1.3976(16) . ? C13 C16 1.4145(15) . ? C14 C15 1.3670(16) . ? C14 C22 1.5074(16) . ? C15 C16 1.4342(17) . ? C15 C21 1.5021(16) . ? C16 C17 1.4030(16) . ? C17 C18 1.3752(17) . ? C17 H17 0.9500 . ? C18 C19 1.4018(16) . ? C18 H18 0.9500 . ? C19 C20 1.3853(16) . ? C19 H19 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C25 1.5087(16) . ? C22 C23 1.5339(15) . ? C22 H22 1.0000 . ? C23 C24 1.5118(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C32 1.3656(16) . ? C26 C27 1.4058(16) . ? C26 C31 1.4092(16) . ? C27 C28 1.3885(17) . ? C28 C29 1.3984(18) . ? C28 H28 0.9500 . ? C29 C30 1.3759(18) . ? C29 H29 0.9500 . ? C30 C31 1.4000(17) . ? C30 H30 0.9500 . ? C31 C32 1.4344(16) . ? C32 C33 1.5024(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O35 1.2437(14) . ? C34 C36 1.4865(17) . ? C36 C37 1.3921(17) . ? C36 C41 1.3969(17) . ? C37 C38 1.3853(18) . ? C37 H37 0.9500 . ? C38 C39 1.3833(18) . ? C38 H38 0.9500 . ? C39 C40 1.389(2) . ? C39 H39 0.9500 . ? C40 C41 1.3827(19) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? O1S H1SA 0.837(15) . ? O1S H1SB 0.865(14) . ? 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 C12 N1 C20 126.51(10) . . ? C12 N1 H1 116.4(9) . . ? C20 N1 H1 116.6(8) . . ? C13 N2 C14 108.93(9) . . ? C13 N2 H2 124.8(9) . . ? C14 N2 H2 126.2(9) . . ? C26 N3 C25 108.42(10) . . ? C26 N3 H3 125.7(8) . . ? C25 N3 H3 125.2(8) . . ? C34 N4 C27 128.23(11) . . ? C34 N4 H4 114.0(9) . . ? C27 N4 H4 117.6(9) . . ? C6 C5 C10 120.52(11) . . ? C6 C5 H5 119.7 . . ? C10 C5 H5 119.7 . . ? C7 C6 C5 119.82(12) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.44(12) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 120.10(12) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 119.89(12) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C5 119.23(11) . . ? C9 C10 C12 119.46(11) . . ? C5 C10 C12 121.25(10) . . ? O11 C12 N1 122.93(11) . . ? O11 C12 C10 122.11(10) . . ? N1 C12 C10 114.94(10) . . ? N2 C13 C20 130.53(10) . . ? N2 C13 C16 107.60(10) . . ? C20 C13 C16 121.87(10) . . ? C15 C14 N2 109.43(10) . . ? C15 C14 C22 128.88(11) . . ? N2 C14 C22 121.68(10) . . ? C14 C15 C16 107.19(10) . . ? C14 C15 C21 126.70(11) . . ? C16 C15 C21 126.11(10) . . ? C17 C16 C13 118.84(11) . . ? C17 C16 C15 134.28(11) . . ? C13 C16 C15 106.84(10) . . ? C18 C17 C16 119.02(11) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 121.76(11) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 120.54(11) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C13 117.95(10) . . ? C19 C20 N1 123.33(10) . . ? C13 C20 N1 118.69(10) . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C25 112.57(9) . . ? C14 C22 C23 112.31(9) . . ? C25 C22 C23 113.91(10) . . ? C14 C22 H22 105.7 . . ? C25 C22 H22 105.7 . . ? C23 C22 H22 105.7 . . ? C24 C23 C22 113.07(10) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C32 C25 N3 109.64(10) . . ? C32 C25 C22 129.00(11) . . ? N3 C25 C22 121.36(10) . . ? N3 C26 C27 130.96(11) . . ? N3 C26 C31 107.74(10) . . ? C27 C26 C31 121.30(11) . . ? C28 C27 C26 117.43(11) . . ? C28 C27 N4 123.86(11) . . ? C26 C27 N4 118.70(10) . . ? C27 C28 C29 121.11(11) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 121.75(12) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 118.39(12) . . ? C29 C30 H30 120.8 . . ? C31 C30 H30 120.8 . . ? C30 C31 C26 120.02(11) . . ? C30 C31 C32 132.77(11) . . ? C26 C31 C32 107.21(10) . . ? C25 C32 C31 107.00(10) . . ? C25 C32 C33 128.61(11) . . ? C31 C32 C33 124.39(11) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O35 C34 N4 122.45(12) . . ? O35 C34 C36 120.64(11) . . ? N4 C34 C36 116.89(10) . . ? C37 C36 C41 118.67(12) . . ? C37 C36 C34 123.19(11) . . ? C41 C36 C34 118.11(11) . . ? C38 C37 C36 120.92(12) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C39 C38 C37 119.88(13) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 119.86(13) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 120.26(12) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C36 120.41(13) . . ? C40 C41 H41 119.8 . . ? C36 C41 H41 119.8 . . ? H1SA O1S H1SB 107.7(13) . . ? 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 C10 C5 C6 C7 0.08(17) . . . . ? C5 C6 C7 C8 -0.09(18) . . . . ? C6 C7 C8 C9 0.31(18) . . . . ? C7 C8 C9 C10 -0.52(18) . . . . ? C8 C9 C10 C5 0.50(17) . . . . ? C8 C9 C10 C12 177.67(11) . . . . ? C6 C5 C10 C9 -0.29(16) . . . . ? C6 C5 C10 C12 -177.40(11) . . . . ? C20 N1 C12 O11 -3.62(18) . . . . ? C20 N1 C12 C10 174.83(10) . . . . ? C9 C10 C12 O11 -34.47(16) . . . . ? C5 C10 C12 O11 142.64(11) . . . . ? C9 C10 C12 N1 147.06(11) . . . . ? C5 C10 C12 N1 -35.82(15) . . . . ? C14 N2 C13 C20 179.09(11) . . . . ? C14 N2 C13 C16 -0.24(12) . . . . ? C13 N2 C14 C15 0.42(13) . . . . ? C13 N2 C14 C22 -178.52(10) . . . . ? N2 C14 C15 C16 -0.41(13) . . . . ? C22 C14 C15 C16 178.43(11) . . . . ? N2 C14 C15 C21 179.07(11) . . . . ? C22 C14 C15 C21 -2.1(2) . . . . ? N2 C13 C16 C17 178.08(10) . . . . ? C20 C13 C16 C17 -1.33(16) . . . . ? N2 C13 C16 C15 -0.01(12) . . . . ? C20 C13 C16 C15 -179.41(10) . . . . ? C14 C15 C16 C17 -177.40(12) . . . . ? C21 C15 C16 C17 3.1(2) . . . . ? C14 C15 C16 C13 0.26(13) . . . . ? C21 C15 C16 C13 -179.23(11) . . . . ? C13 C16 C17 C18 -0.38(16) . . . . ? C15 C16 C17 C18 177.06(12) . . . . ? C16 C17 C18 C19 1.53(18) . . . . ? C17 C18 C19 C20 -0.99(18) . . . . ? C18 C19 C20 C13 -0.70(16) . . . . ? C18 C19 C20 N1 177.39(11) . . . . ? N2 C13 C20 C19 -177.40(11) . . . . ? C16 C13 C20 C19 1.85(16) . . . . ? N2 C13 C20 N1 4.42(18) . . . . ? C16 C13 C20 N1 -176.33(10) . . . . ? C12 N1 C20 C19 39.64(17) . . . . ? C12 N1 C20 C13 -142.29(11) . . . . ? C15 C14 C22 C25 93.72(14) . . . . ? N2 C14 C22 C25 -87.57(13) . . . . ? C15 C14 C22 C23 -136.13(12) . . . . ? N2 C14 C22 C23 42.59(14) . . . . ? C14 C22 C23 C24 170.47(10) . . . . ? C25 C22 C23 C24 -60.06(14) . . . . ? C26 N3 C25 C32 0.07(13) . . . . ? C26 N3 C25 C22 -179.99(10) . . . . ? C14 C22 C25 C32 -101.76(14) . . . . ? C23 C22 C25 C32 128.90(13) . . . . ? C14 C22 C25 N3 78.31(13) . . . . ? C23 C22 C25 N3 -51.03(14) . . . . ? C25 N3 C26 C27 -179.37(11) . . . . ? C25 N3 C26 C31 -0.10(12) . . . . ? N3 C26 C27 C28 179.73(11) . . . . ? C31 C26 C27 C28 0.54(17) . . . . ? N3 C26 C27 N4 0.07(18) . . . . ? C31 C26 C27 N4 -179.11(10) . . . . ? C34 N4 C27 C28 20.61(19) . . . . ? C34 N4 C27 C26 -159.76(11) . . . . ? C26 C27 C28 C29 -0.79(17) . . . . ? N4 C27 C28 C29 178.85(11) . . . . ? C27 C28 C29 C30 0.3(2) . . . . ? C28 C29 C30 C31 0.45(19) . . . . ? C29 C30 C31 C26 -0.69(18) . . . . ? C29 C30 C31 C32 -179.72(12) . . . . ? N3 C26 C31 C30 -179.16(10) . . . . ? C27 C26 C31 C30 0.20(17) . . . . ? N3 C26 C31 C32 0.10(13) . . . . ? C27 C26 C31 C32 179.45(10) . . . . ? N3 C25 C32 C31 0.00(13) . . . . ? C22 C25 C32 C31 -179.94(11) . . . . ? N3 C25 C32 C33 179.57(11) . . . . ? C22 C25 C32 C33 -0.4(2) . . . . ? C30 C31 C32 C25 179.07(13) . . . . ? C26 C31 C32 C25 -0.06(13) . . . . ? C30 C31 C32 C33 -0.5(2) . . . . ? C26 C31 C32 C33 -179.66(11) . . . . ? C27 N4 C34 O35 -0.21(19) . . . . ? C27 N4 C34 C36 178.33(10) . . . . ? O35 C34 C36 C37 148.00(11) . . . . ? N4 C34 C36 C37 -30.56(16) . . . . ? O35 C34 C36 C41 -29.81(16) . . . . ? N4 C34 C36 C41 151.63(11) . . . . ? C41 C36 C37 C38 0.69(18) . . . . ? C34 C36 C37 C38 -177.12(11) . . . . ? C36 C37 C38 C39 -0.10(18) . . . . ? C37 C38 C39 C40 -0.35(19) . . . . ? C38 C39 C40 C41 0.2(2) . . . . ? C39 C40 C41 C36 0.4(2) . . . . ? C37 C36 C41 C40 -0.83(19) . . . . ? C34 C36 C41 C40 177.09(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O35 0.846(13) 2.241(13) 3.0616(13) 163.3(11) 3_576 N2 H2 O1S 0.903(14) 2.131(14) 2.9582(13) 152.0(12) . N3 H3 O1S 0.931(13) 1.999(14) 2.9191(13) 169.2(12) . O1S H1SA O35 0.837(15) 1.967(15) 2.7972(13) 171.0(14) 3_576 O1S H1SB O11 0.865(14) 1.876(15) 2.7401(12) 176.5(14) 2 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.244 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.037 # Attachment '1a_TBAB_Revised.CIF' data_p156tbab _database_code_depnum_ccdc_archive 'CCDC 725837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H77 N5 O4' _chemical_formula_weight 836.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4563(10) _cell_length_b 13.7844(11) _cell_length_c 27.517(2) _cell_angle_alpha 101.614(7) _cell_angle_beta 100.781(7) _cell_angle_gamma 94.217(6) _cell_volume 4878.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.6479 _diffrn_standards_number '1 frame' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88056 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.00 _reflns_number_total 21275 _reflns_number_gt 10525 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET) (compiled Nov 11 2005,15:50:43) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material SHELXTL-97 _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^)+(0.0571P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21275 _refine_ls_number_parameters 1318 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.16884(10) -0.00002(10) 0.16694(5) 0.0505(4) Uani 1 1 d . . . N1A N 0.20899(12) 0.08041(12) 0.10764(7) 0.0396(4) Uani 1 1 d . . . N2A N 0.34677(11) 0.18720(10) 0.05956(6) 0.0293(4) Uani 1 1 d . . . N3A N 0.36495(11) 0.43865(10) 0.06721(5) 0.0239(3) Uani 1 1 d . A . N4A N 0.24815(11) 0.57719(12) 0.12421(6) 0.0323(4) Uani 1 1 d . . . C1A C 0.42760(12) 0.21298(12) 0.03823(6) 0.0262(4) Uani 1 1 d . . . C2A C 0.50141(12) 0.15139(12) 0.04641(6) 0.0281(4) Uani 1 1 d . . . C3A C 0.60165(12) 0.15125(13) 0.02980(7) 0.0349(4) Uani 1 1 d . . . H3A1 H 0.6015 0.1915 0.0042 0.052 Uiso 1 1 calc R . . H3A2 H 0.6120 0.0827 0.0153 0.052 Uiso 1 1 calc R . . H3A3 H 0.6569 0.1795 0.0591 0.052 Uiso 1 1 calc R . . C4A C 0.46379(12) 0.08274(12) 0.07322(7) 0.0302(4) Uani 1 1 d . . . C5A C 0.50226(14) 0.00198(13) 0.09104(7) 0.0377(5) Uani 1 1 d . . . H5A H 0.5678 -0.0154 0.0871 0.045 Uiso 1 1 calc R . . C6A C 0.44337(15) -0.05144(14) 0.11432(7) 0.0419(5) Uani 1 1 d . . . H6A H 0.4689 -0.1067 0.1263 0.050 Uiso 1 1 calc R . . C7A C 0.34666(14) -0.02746(13) 0.12111(7) 0.0401(5) Uani 1 1 d . . . H7A H 0.3081 -0.0665 0.1374 0.048 Uiso 1 1 calc R . . C8A C 0.30698(13) 0.05233(13) 0.10431(7) 0.0344(4) Uani 1 1 d . . . C9A C 0.36691(13) 0.10674(12) 0.08034(7) 0.0295(4) Uani 1 1 d . . . C10A C 0.14593(14) 0.05252(13) 0.13659(7) 0.0380(5) Uani 1 1 d . . . C11A C 0.04228(14) 0.08864(14) 0.12723(8) 0.0453(5) Uani 1 1 d . . . H11A H 0.0487 0.1544 0.1182 0.054 Uiso 1 1 calc R . . H11B H 0.0152 0.0970 0.1587 0.054 Uiso 1 1 calc R . . C12A C -0.03171(15) 0.01563(15) 0.08474(9) 0.0531(6) Uani 1 1 d . . . H12A H -0.0339 -0.0513 0.0927 0.064 Uiso 1 1 calc R . . H12B H -0.0067 0.0110 0.0528 0.064 Uiso 1 1 calc R . . C13A C -0.13942(16) 0.04665(17) 0.07694(11) 0.0727(8) Uani 1 1 d . . . H13A H -0.1670 0.0455 0.1074 0.109 Uiso 1 1 calc R . . H13B H -0.1831 0.0002 0.0478 0.109 Uiso 1 1 calc R . . H13C H -0.1372 0.1142 0.0706 0.109 Uiso 1 1 calc R . . C14A C 0.42256(12) 0.29694(11) 0.01085(6) 0.0243(4) Uani 1 1 d . . . H14A H 0.4785 0.2926 -0.0086 0.029 Uiso 1 1 calc R . . C15A C 0.32190(12) 0.28461(12) -0.02836(6) 0.0265(4) Uani 1 1 d . . . H15A H 0.2644 0.2861 -0.0106 0.032 Uiso 1 1 calc R . . H15B H 0.3210 0.3416 -0.0453 0.032 Uiso 1 1 calc R . . C16A C 0.30716(13) 0.18847(12) -0.06810(7) 0.0349(4) Uani 1 1 d . . . H16A H 0.3625 0.1877 -0.0868 0.052 Uiso 1 1 calc R . . H16B H 0.2418 0.1837 -0.0917 0.052 Uiso 1 1 calc R . . H16C H 0.3076 0.1318 -0.0516 0.052 Uiso 1 1 calc R . . C17A C 0.44218(12) 0.39724(12) 0.04632(6) 0.0225(4) Uani 1 1 d . . . C18A C 0.52932(12) 0.46160(12) 0.06279(6) 0.0234(4) Uani 1 1 d . . . C19A C 0.63023(12) 0.44661(12) 0.04810(7) 0.0288(4) Uani 1 1 d . . . H19A H 0.6415 0.3764 0.0450 0.043 Uiso 1 1 calc R . . H19B H 0.6848 0.4884 0.0742 0.043 Uiso 1 1 calc R . . H19C H 0.6301 0.4653 0.0156 0.043 Uiso 1 1 calc R . . C20A C 0.50608(12) 0.54797(12) 0.09528(6) 0.0243(4) Uani 1 1 d . A . C21A C 0.56222(13) 0.63864(12) 0.12326(6) 0.0281(4) Uani 1 1 d . . . H21A H 0.6323 0.6523 0.1230 0.034 Uiso 1 1 calc R . . C22A C 0.51339(13) 0.70680(13) 0.15083(6) 0.0320(4) Uani 1 1 d . A . H22A H 0.5510 0.7680 0.1698 0.038 Uiso 1 1 calc R . . C23A C 0.41040(13) 0.68951(13) 0.15198(6) 0.0317(4) Uani 1 1 d . . . H23A H 0.3795 0.7392 0.1713 0.038 Uiso 1 1 calc R A . C24A C 0.35247(12) 0.60082(13) 0.12533(6) 0.0280(4) Uani 1 1 d . A . C25A C 0.40239(12) 0.53078(12) 0.09722(6) 0.0234(4) Uani 1 1 d . . . C26A C 0.1868(5) 0.6448(7) 0.1474(3) 0.0344(16) Uani 0.503(11) 1 d PD A 1 O2A O 0.2152(3) 0.7258(5) 0.1746(2) 0.0565(19) Uani 0.503(11) 1 d PU A 1 C27A C 0.0797(6) 0.5967(10) 0.1382(6) 0.054(3) Uani 0.503(11) 1 d PD A 1 H27A H 0.0714 0.5316 0.1139 0.064 Uiso 0.503(11) 1 calc PR A 1 H27B H 0.0636 0.5850 0.1704 0.064 Uiso 0.503(11) 1 calc PR A 1 C28A C 0.0107(6) 0.6620(6) 0.1176(2) 0.0329(15) Uani 0.503(11) 1 d PD A 1 H28A H 0.0220 0.6657 0.0835 0.040 Uiso 0.503(11) 1 calc PR A 1 H28B H 0.0282 0.7299 0.1394 0.040 Uiso 0.503(11) 1 calc PR A 1 C29A C -0.1019(8) 0.6296(12) 0.1134(7) 0.053(2) Uani 0.503(11) 1 d PD A 1 H29A H -0.1195 0.5611 0.0935 0.079 Uiso 0.503(11) 1 calc PR A 1 H29B H -0.1430 0.6741 0.0967 0.079 Uiso 0.503(11) 1 calc PR A 1 H29C H -0.1157 0.6329 0.1474 0.079 Uiso 0.503(11) 1 calc PR A 1 C26C C 0.1930(5) 0.6092(6) 0.1585(3) 0.0356(17) Uani 0.497(11) 1 d PD A 2 O2C O 0.2296(4) 0.6735(6) 0.1965(2) 0.064(3) Uani 0.497(11) 1 d P A 2 C27C C 0.0808(6) 0.5755(9) 0.1462(5) 0.043(2) Uani 0.497(11) 1 d PD A 2 H27E H 0.0687 0.5114 0.1209 0.051 Uiso 0.497(11) 1 calc PR A 2 H27F H 0.0612 0.5620 0.1773 0.051 Uiso 0.497(11) 1 calc PR A 2 C28C C 0.0123(9) 0.6424(7) 0.1266(4) 0.083(3) Uani 0.497(11) 1 d PDU A 2 H28E H 0.0247 0.6490 0.0930 0.099 Uiso 0.497(11) 1 calc PR A 2 H28F H 0.0292 0.7093 0.1495 0.099 Uiso 0.497(11) 1 calc PR A 2 C29C C -0.1005(9) 0.6090(14) 0.1212(8) 0.067(3) Uani 0.497(11) 1 d PD A 2 H29G H -0.1181 0.5424 0.0989 0.100 Uiso 0.497(11) 1 calc PR A 2 H29H H -0.1412 0.6561 0.1064 0.100 Uiso 0.497(11) 1 calc PR A 2 H29I H -0.1148 0.6070 0.1546 0.100 Uiso 0.497(11) 1 calc PR A 2 H1NA H 0.1856(14) 0.1202(14) 0.0873(7) 0.054(6) Uiso 1 1 d . . . H2NA H 0.2894(14) 0.2116(13) 0.0563(7) 0.047(6) Uiso 1 1 d . . . H3NA H 0.3046(13) 0.4131(12) 0.0629(6) 0.032(5) Uiso 1 1 d . . . H4NA H 0.2152(13) 0.5228(13) 0.1019(7) 0.042(6) Uiso 1 1 d . . . O3A O 0.14408(9) 0.22805(10) 0.05011(6) 0.0499(4) Uani 1 1 d . . . O4A O 0.15825(8) 0.39198(9) 0.05700(5) 0.0380(3) Uani 1 1 d . . . C30A C 0.10752(13) 0.30700(14) 0.04466(7) 0.0319(4) Uani 1 1 d . . . C31A C -0.00322(12) 0.30131(12) 0.02098(6) 0.0271(4) Uani 1 1 d . . . C32A C -0.04974(12) 0.38677(13) 0.01836(6) 0.0276(4) Uani 1 1 d . . . H32A H -0.0116 0.4501 0.0329 0.033 Uiso 1 1 calc R . . C33A C -0.15076(13) 0.38169(14) -0.00499(7) 0.0348(4) Uani 1 1 d . . . H33A H -0.1819 0.4410 -0.0062 0.042 Uiso 1 1 calc R . . C34A C -0.20605(14) 0.29004(16) -0.02650(7) 0.0447(5) Uani 1 1 d . . . H34A H -0.2754 0.2861 -0.0429 0.054 Uiso 1 1 calc R . . C35A C -0.16099(15) 0.20423(16) -0.02431(8) 0.0503(6) Uani 1 1 d . . . H35A H -0.1992 0.1411 -0.0392 0.060 Uiso 1 1 calc R . . C36A C -0.06009(14) 0.20979(14) -0.00049(8) 0.0423(5) Uani 1 1 d . . . H36A H -0.0295 0.1503 0.0012 0.051 Uiso 1 1 calc R . . N5A N 0.58381(10) 0.35421(12) 0.20950(5) 0.0381(4) Uani 1 1 d . . . C37A C 0.64828(13) 0.33702(15) 0.16960(7) 0.0417(5) Uani 1 1 d . B . H37A H 0.6349 0.3858 0.1479 0.050 Uiso 1 1 calc R . . H37B H 0.6260 0.2696 0.1478 0.050 Uiso 1 1 calc R . . C38A C 0.76268(14) 0.34566(17) 0.18995(8) 0.0508(6) Uani 1 1 d . . . H38A H 0.7772 0.2989 0.2127 0.061 Uiso 1 1 calc R B . H38B H 0.7870 0.4142 0.2100 0.061 Uiso 1 1 calc R . . C39A C 0.81948(15) 0.32194(18) 0.14668(8) 0.0581(6) Uani 1 1 d . B . H39A H 0.7994 0.2515 0.1286 0.070 Uiso 1 1 calc R . . H39B H 0.7995 0.3644 0.1222 0.070 Uiso 1 1 calc R . . C40A C 0.93258(16) 0.33886(18) 0.16511(9) 0.0669(7) Uani 1 1 d . . . H40A H 0.9530 0.4089 0.1824 0.100 Uiso 1 1 calc R B . H40B H 0.9659 0.3228 0.1362 0.100 Uiso 1 1 calc R . . H40C H 0.9529 0.2960 0.1888 0.100 Uiso 1 1 calc R . . C41A C 0.62255(14) 0.45078(15) 0.24814(7) 0.0448(7) Uani 0.810(4) 1 d P B 3 H41A H 0.6942 0.4475 0.2641 0.054 Uiso 0.810(4) 1 calc PR B 3 H41B H 0.5825 0.4559 0.2751 0.054 Uiso 0.810(4) 1 calc PR B 3 C42A C 0.6177(2) 0.5472(2) 0.22715(9) 0.0427(7) Uani 0.810(4) 1 d P B 3 H42A H 0.6490 0.5389 0.1970 0.051 Uiso 0.810(4) 1 calc PR B 3 H42B H 0.5455 0.5572 0.2162 0.051 Uiso 0.810(4) 1 calc PR B 3 C43A C 0.6723(2) 0.6396(2) 0.26619(11) 0.0586(9) Uani 0.810(4) 1 d P B 3 H43A H 0.6466 0.6997 0.2561 0.070 Uiso 0.810(4) 1 calc PR B 3 H43B H 0.6556 0.6371 0.2995 0.070 Uiso 0.810(4) 1 calc PR B 3 C44A C 0.7873(2) 0.6491(3) 0.27174(12) 0.0690(10) Uani 0.810(4) 1 d P B 3 H44A H 0.8130 0.5887 0.2804 0.104 Uiso 0.810(4) 1 calc PR B 3 H44B H 0.8182 0.7071 0.2987 0.104 Uiso 0.810(4) 1 calc PR B 3 H44C H 0.8047 0.6574 0.2397 0.104 Uiso 0.810(4) 1 calc PR B 3 C41C C 0.62255(14) 0.45078(15) 0.24814(7) 0.0448(7) Uani 0.19 1 d PD B 4 H41E H 0.5664 0.4752 0.2641 0.054 Uiso 0.190(4) 1 calc PR B 4 H41F H 0.6770 0.4385 0.2751 0.054 Uiso 0.190(4) 1 calc PR B 4 C42C C 0.6616(12) 0.5251(10) 0.2248(6) 0.072(6) Uiso 0.190(4) 1 d PD B 4 H42E H 0.6063 0.5497 0.2030 0.086 Uiso 0.190(4) 1 calc PR B 4 H42F H 0.7116 0.4999 0.2046 0.086 Uiso 0.190(4) 1 calc PR B 4 C43C C 0.7144(12) 0.6089(9) 0.2736(5) 0.049(4) Uiso 0.190(4) 1 d PD B 4 H43E H 0.6675 0.6205 0.2974 0.059 Uiso 0.190(4) 1 calc PR B 4 H43F H 0.7769 0.5869 0.2912 0.059 Uiso 0.190(4) 1 calc PR B 4 C44C C 0.7409(13) 0.7050(10) 0.2571(6) 0.087(5) Uiso 0.190(4) 1 d PD B 4 H44G H 0.7698 0.6895 0.2266 0.130 Uiso 0.190(4) 1 calc PR B 4 H44H H 0.7908 0.7498 0.2844 0.130 Uiso 0.190(4) 1 calc PR B 4 H44I H 0.6792 0.7375 0.2496 0.130 Uiso 0.190(4) 1 calc PR B 4 C45A C 0.47586(13) 0.35715(15) 0.18144(7) 0.0428(7) Uani 0.347(5) 1 d P B 5 H45A H 0.4752 0.4195 0.1688 0.051 Uiso 0.347(5) 1 calc PR B 5 H45B H 0.4611 0.3012 0.1513 0.051 Uiso 0.347(5) 1 calc PR B 5 C46A C 0.3910(9) 0.3520(10) 0.2076(4) 0.062(4) Uani 0.347(5) 1 d P B 5 H46A H 0.3988 0.4134 0.2344 0.074 Uiso 0.347(5) 1 calc PR B 5 H46B H 0.3962 0.2951 0.2245 0.074 Uiso 0.347(5) 1 calc PR B 5 C47A C 0.2882(15) 0.3408(9) 0.1756(7) 0.045(3) Uani 0.347(5) 1 d P B 5 H47A H 0.2862 0.3915 0.1546 0.054 Uiso 0.347(5) 1 calc PR B 5 H47B H 0.2762 0.2744 0.1522 0.054 Uiso 0.347(5) 1 calc PR B 5 C48A C 0.2049(5) 0.3507(8) 0.2030(3) 0.065(3) Uani 0.347(5) 1 d P B 5 H48A H 0.1964 0.2927 0.2180 0.097 Uiso 0.347(5) 1 calc PR B 5 H48B H 0.1417 0.3546 0.1794 0.097 Uiso 0.347(5) 1 calc PR B 5 H48C H 0.2207 0.4115 0.2299 0.097 Uiso 0.347(5) 1 calc PR B 5 C45C C 0.47586(13) 0.35715(15) 0.18144(7) 0.0428(7) Uani 0.65 1 d P B 6 H45E H 0.4461 0.2886 0.1635 0.051 Uiso 0.653(5) 1 calc PR B 6 H45F H 0.4781 0.3975 0.1556 0.051 Uiso 0.653(5) 1 calc PR B 6 C46C C 0.4059(5) 0.4018(4) 0.2171(3) 0.0414(13) Uani 0.653(5) 1 d P B 6 H46E H 0.4134 0.3712 0.2470 0.050 Uiso 0.653(5) 1 calc PR B 6 H46F H 0.4250 0.4746 0.2290 0.050 Uiso 0.653(5) 1 calc PR B 6 C47C C 0.2952(7) 0.3799(4) 0.1871(3) 0.0414(16) Uani 0.653(5) 1 d P B 6 H47E H 0.2922 0.3971 0.1536 0.050 Uiso 0.653(5) 1 calc PR B 6 H47F H 0.2731 0.3076 0.1811 0.050 Uiso 0.653(5) 1 calc PR B 6 C48C C 0.2224(2) 0.4372(4) 0.21390(13) 0.0538(12) Uani 0.653(5) 1 d P B 6 H48G H 0.2264 0.4221 0.2475 0.081 Uiso 0.653(5) 1 calc PR B 6 H48H H 0.1528 0.4178 0.1940 0.081 Uiso 0.653(5) 1 calc PR B 6 H48I H 0.2406 0.5088 0.2177 0.081 Uiso 0.653(5) 1 calc PR B 6 C49A C 0.58806(15) 0.27382(15) 0.23956(7) 0.0463(5) Uani 1 1 d . B . H49A H 0.6568 0.2819 0.2614 0.056 Uiso 1 1 calc R . . H49B H 0.5387 0.2844 0.2621 0.056 Uiso 1 1 calc R . . C50A C 0.56602(16) 0.16869(17) 0.20902(8) 0.0577(6) Uani 1 1 d . . . H50A H 0.6256 0.1497 0.1945 0.069 Uiso 1 1 calc R B . H50B H 0.5071 0.1636 0.1807 0.069 Uiso 1 1 calc R . . C51A C 0.54222(18) 0.09710(19) 0.24301(9) 0.0733(8) Uani 1 1 d . B . H51A H 0.5449 0.0276 0.2253 0.088 Uiso 1 1 calc R . . H51B H 0.5948 0.1121 0.2747 0.088 Uiso 1 1 calc R . . C52A C 0.43896(18) 0.1063(2) 0.25581(9) 0.0803(8) Uani 1 1 d U . . H52A H 0.4351 0.1756 0.2722 0.120 Uiso 1 1 calc R B . H52B H 0.4281 0.0628 0.2789 0.120 Uiso 1 1 calc R . . H52C H 0.3863 0.0866 0.2247 0.120 Uiso 1 1 calc R . . O1B O 0.50867(10) 0.37774(10) 0.34010(5) 0.0519(4) Uani 1 1 d . C . O2B O -0.19154(10) 0.25774(10) 0.30241(5) 0.0523(4) Uani 1 1 d . . . N1B N 0.42244(11) 0.32803(11) 0.39657(6) 0.0334(4) Uani 1 1 d . C . N2B N 0.32348(10) 0.18266(11) 0.44411(5) 0.0238(3) Uani 1 1 d . . . N3B N 0.06742(9) 0.14593(11) 0.43377(5) 0.0209(3) Uani 1 1 d . . . N4B N -0.08240(11) 0.24816(11) 0.37446(5) 0.0261(3) Uani 1 1 d . . . C1B C 0.30080(11) 0.09915(12) 0.46218(6) 0.0214(4) Uani 1 1 d . . . C2B C 0.36757(11) 0.03110(12) 0.45138(6) 0.0234(4) Uani 1 1 d . . . C3B C 0.36955(13) -0.07097(12) 0.46202(6) 0.0305(4) Uani 1 1 d . . . H3B1 H 0.3311 -0.0765 0.4885 0.046 Uiso 1 1 calc R . . H3B2 H 0.4402 -0.0826 0.4735 0.046 Uiso 1 1 calc R . . H3B3 H 0.3386 -0.1207 0.4310 0.046 Uiso 1 1 calc R . . C4B C 0.43693(12) 0.07655(12) 0.42648(6) 0.0249(4) Uani 1 1 d . . . C5B C 0.52411(12) 0.04696(14) 0.40901(6) 0.0324(4) Uani 1 1 d . . . H5B H 0.5465 -0.0159 0.4117 0.039 Uiso 1 1 calc R . . C6B C 0.57610(13) 0.11180(15) 0.38785(7) 0.0390(5) Uani 1 1 d . . . H6B H 0.6358 0.0931 0.3764 0.047 Uiso 1 1 calc R . . C7B C 0.54445(13) 0.20351(15) 0.38262(6) 0.0370(5) Uani 1 1 d . . . H7B H 0.5821 0.2453 0.3673 0.044 Uiso 1 1 calc R . . C8B C 0.45882(12) 0.23503(13) 0.39939(6) 0.0296(4) Uani 1 1 d . . . C9B C 0.40696(11) 0.17022(12) 0.42219(6) 0.0241(4) Uani 1 1 d . . . C10B C 0.44663(14) 0.39157(15) 0.36759(7) 0.0409(5) Uani 1 1 d D . . C11B C 0.3806(9) 0.4754(7) 0.3668(7) 0.053(3) Uani 0.479(4) 1 d PD C 7 H11C H 0.3383 0.4787 0.3928 0.064 Uiso 0.479(4) 1 calc PR C 7 H11D H 0.3357 0.4680 0.3330 0.064 Uiso 0.479(4) 1 calc PR C 7 C12B C 0.4584(10) 0.5666(8) 0.3788(4) 0.060(3) Uani 0.479(4) 1 d PD C 7 H12C H 0.5071 0.5574 0.3558 0.072 Uiso 0.479(4) 1 calc PR C 7 H12D H 0.4970 0.5779 0.4142 0.072 Uiso 0.479(4) 1 calc PR C 7 C13B C 0.3998(3) 0.6552(3) 0.3713(2) 0.0664(17) Uani 0.479(4) 1 d PD C 7 H13D H 0.3662 0.6455 0.3356 0.100 Uiso 0.479(4) 1 calc PR C 7 H13E H 0.4472 0.7167 0.3812 0.100 Uiso 0.479(4) 1 calc PR C 7 H13F H 0.3484 0.6604 0.3924 0.100 Uiso 0.479(4) 1 calc PR C 7 C11D C 0.4012(7) 0.4898(5) 0.3754(6) 0.038(2) Uani 0.521(4) 1 d PD C 8 H11G H 0.3505 0.4846 0.3969 0.046 Uiso 0.521(4) 1 calc PR C 8 H11H H 0.3631 0.4960 0.3419 0.046 Uiso 0.521(4) 1 calc PR C 8 C12D C 0.4702(9) 0.5872(8) 0.3987(3) 0.0419(19) Uani 0.521(4) 1 d PD C 8 H12G H 0.4278 0.6427 0.4038 0.050 Uiso 0.521(4) 1 calc PR C 8 H12H H 0.5139 0.6005 0.3750 0.050 Uiso 0.521(4) 1 calc PR C 8 C13D C 0.5374(3) 0.5837(3) 0.44937(13) 0.0401(12) Uani 0.521(4) 1 d PD C 8 H13J H 0.4945 0.5754 0.4737 0.060 Uiso 0.521(4) 1 calc PR C 8 H13K H 0.5831 0.6460 0.4623 0.060 Uiso 0.521(4) 1 calc PR C 8 H13L H 0.5777 0.5275 0.4447 0.060 Uiso 0.521(4) 1 calc PR C 8 C14B C 0.21545(11) 0.09558(11) 0.49049(6) 0.0214(4) Uani 1 1 d . . . H14B H 0.2237 0.0385 0.5078 0.026 Uiso 1 1 calc R . . C15B C 0.22441(11) 0.18968(12) 0.53250(6) 0.0235(4) Uani 1 1 d . . . H15C H 0.2257 0.2491 0.5174 0.028 Uiso 1 1 calc R . . H15D H 0.1638 0.1877 0.5480 0.028 Uiso 1 1 calc R . . C16B C 0.32007(12) 0.19912(13) 0.57357(6) 0.0325(4) Uani 1 1 d . . . H16D H 0.3178 0.1417 0.5895 0.049 Uiso 1 1 calc R . . H16E H 0.3236 0.2606 0.5992 0.049 Uiso 1 1 calc R . . H16F H 0.3803 0.2010 0.5584 0.049 Uiso 1 1 calc R . . C17B C 0.11259(11) 0.07349(11) 0.45566(6) 0.0206(4) Uani 1 1 d . . . C18B C 0.05047(11) -0.01458(11) 0.43964(6) 0.0216(4) Uani 1 1 d . . . C19B C 0.06912(12) -0.11078(11) 0.45529(6) 0.0273(4) Uani 1 1 d . . . H19D H 0.1387 -0.1248 0.4532 0.041 Uiso 1 1 calc R . . H19E H 0.0206 -0.1650 0.4327 0.041 Uiso 1 1 calc R . . H19F H 0.0603 -0.1055 0.4902 0.041 Uiso 1 1 calc R . . C20B C -0.03794(11) 0.00249(11) 0.40603(6) 0.0216(4) Uani 1 1 d . . . C21B C -0.12616(12) -0.05853(13) 0.37763(6) 0.0273(4) Uani 1 1 d . . . H21B H -0.1366 -0.1268 0.3790 0.033 Uiso 1 1 calc R . . C22B C -0.19697(12) -0.01712(13) 0.34784(6) 0.0300(4) Uani 1 1 d . . . H22B H -0.2570 -0.0577 0.3285 0.036 Uiso 1 1 calc R . . C23B C -0.18340(12) 0.08289(13) 0.34517(6) 0.0277(4) Uani 1 1 d . . . H23B H -0.2339 0.1085 0.3237 0.033 Uiso 1 1 calc R . . C24B C -0.09792(12) 0.14557(12) 0.37306(6) 0.0229(4) Uani 1 1 d . . . C25B C -0.02485(11) 0.10305(12) 0.40332(6) 0.0208(4) Uani 1 1 d . . . C26B C -0.13264(13) 0.29889(14) 0.34205(7) 0.0345(4) Uani 1 1 d . . . C27B C -0.11647(14) 0.40984(13) 0.35955(7) 0.0375(5) Uani 1 1 d . . . H27C H -0.1144 0.4408 0.3302 0.045 Uiso 1 1 calc R . . H27D H -0.0504 0.4301 0.3838 0.045 Uiso 1 1 calc R . . C28B C -0.20256(15) 0.44621(14) 0.38512(7) 0.0426(5) Uani 1 1 d . . . H28C H -0.2682 0.4250 0.3606 0.051 Uiso 1 1 calc R . . H28D H -0.2045 0.4141 0.4141 0.051 Uiso 1 1 calc R . . C29B C -0.19152(17) 0.55828(15) 0.40407(8) 0.0576(6) Uani 1 1 d . . . H29D H -0.1284 0.5796 0.4297 0.086 Uiso 1 1 calc R . . H29E H -0.2497 0.5771 0.4192 0.086 Uiso 1 1 calc R . . H29F H -0.1893 0.5907 0.3756 0.086 Uiso 1 1 calc R . . H1NB H 0.3732(14) 0.3450(13) 0.4147(7) 0.048(6) Uiso 1 1 d . . . H2NB H 0.2918(13) 0.2395(13) 0.4481(6) 0.040(5) Uiso 1 1 d . . . H3NB H 0.0894(13) 0.2117(13) 0.4396(6) 0.038(5) Uiso 1 1 d . . . H4NB H -0.0353(13) 0.2834(12) 0.3984(6) 0.031(5) Uiso 1 1 d . . . O3B O 0.26006(9) 0.36689(8) 0.44942(5) 0.0383(3) Uani 1 1 d . . . O4B O 0.09390(9) 0.35513(8) 0.44807(4) 0.0330(3) Uani 1 1 d . . . C30B C 0.17932(14) 0.40457(12) 0.45510(6) 0.0278(4) Uani 1 1 d . . . C31B C 0.18821(13) 0.51596(12) 0.47301(6) 0.0277(4) Uani 1 1 d . . . C32B C 0.10221(14) 0.56409(12) 0.47755(6) 0.0302(4) Uani 1 1 d . . . H32B H 0.0367 0.5268 0.4677 0.036 Uiso 1 1 calc R . . C33B C 0.11142(15) 0.66649(13) 0.49650(7) 0.0370(5) Uani 1 1 d . . . H33B H 0.0524 0.6992 0.4996 0.044 Uiso 1 1 calc R . . C34B C 0.20644(16) 0.72020(14) 0.51082(7) 0.0431(5) Uani 1 1 d . . . H34B H 0.2128 0.7900 0.5242 0.052 Uiso 1 1 calc R . . C35B C 0.29223(15) 0.67387(14) 0.50592(7) 0.0435(5) Uani 1 1 d . . . H35B H 0.3575 0.7116 0.5153 0.052 Uiso 1 1 calc R . . C36B C 0.28294(14) 0.57202(13) 0.48728(7) 0.0373(5) Uani 1 1 d . . . H36B H 0.3423 0.5400 0.4842 0.045 Uiso 1 1 calc R . . N5B N 0.14228(10) 0.91250(10) 0.29057(5) 0.0263(3) Uani 1 1 d . . . C37B C 0.11847(13) 0.84505(12) 0.32503(6) 0.0312(4) Uani 1 1 d . D . H37C H 0.0541 0.8613 0.3355 0.037 Uiso 1 1 calc R . . H37D H 0.1729 0.8606 0.3560 0.037 Uiso 1 1 calc R . . C38B C 0.10818(16) 0.73370(13) 0.30284(7) 0.0460(5) Uani 1 1 d . . . H38C H 0.1693 0.7170 0.2891 0.055 Uiso 1 1 calc R D . H38D H 0.0481 0.7152 0.2745 0.055 Uiso 1 1 calc R . . C39B C 0.09639(18) 0.67410(14) 0.34305(8) 0.0568(6) Uani 1 1 d . D . H39C H 0.1527 0.6983 0.3729 0.068 Uiso 1 1 calc R . . H39D H 0.0316 0.6860 0.3541 0.068 Uiso 1 1 calc R . . C40B C 0.0969(2) 0.56397(17) 0.32404(10) 0.0808(8) Uani 1 1 d . . . H40D H 0.0396 0.5390 0.2954 0.121 Uiso 1 1 calc R D . H40E H 0.0906 0.5294 0.3513 0.121 Uiso 1 1 calc R . . H40F H 0.1609 0.5517 0.3131 0.121 Uiso 1 1 calc R . . C41B C 0.05685(13) 0.89802(13) 0.24428(6) 0.0338(4) Uani 1 1 d . D . H41C H 0.0782 0.9384 0.2213 0.041 Uiso 1 1 calc R . . H41D H 0.0486 0.8272 0.2263 0.041 Uiso 1 1 calc R . . C42B C -0.04577(13) 0.92463(15) 0.25346(7) 0.0445(5) Uani 1 1 d . . . H42C H -0.0392 0.9950 0.2720 0.053 Uiso 1 1 calc R D . H42D H -0.0708 0.8820 0.2746 0.053 Uiso 1 1 calc R . . C43B C -0.12138(15) 0.91016(16) 0.20357(7) 0.0526(6) Uani 1 1 d . D . H43C H -0.0925 0.9483 0.1815 0.063 Uiso 1 1 calc R . . H43D H -0.1307 0.8387 0.1864 0.063 Uiso 1 1 calc R . . C44B C -0.22459(16) 0.9427(2) 0.20900(9) 0.0794(8) Uani 1 1 d U . . H44D H -0.2556 0.9029 0.2292 0.119 Uiso 1 1 calc R D . H44E H -0.2687 0.9330 0.1753 0.119 Uiso 1 1 calc R . . H44F H -0.2163 1.0134 0.2260 0.119 Uiso 1 1 calc R . . C45B C 0.15711(13) 1.01860(12) 0.32185(6) 0.0287(5) Uani 0.625(3) 1 d P D 9 H45C H 0.0984 1.0285 0.3386 0.034 Uiso 0.625(3) 1 calc PR D 9 H45D H 0.2189 1.0263 0.3489 0.034 Uiso 0.625(3) 1 calc PR D 9 C46B C 0.1677(5) 1.1005(5) 0.2931(3) 0.0384(14) Uani 0.625(3) 1 d P D 9 H46C H 0.2344 1.1019 0.2829 0.046 Uiso 0.625(3) 1 calc PR D 9 H46D H 0.1136 1.0868 0.2619 0.046 Uiso 0.625(3) 1 calc PR D 9 C47B C 0.1595(8) 1.1974(7) 0.3249(4) 0.038(2) Uani 0.625(3) 1 d P D 9 H47C H 0.2113 1.2090 0.3568 0.046 Uiso 0.625(3) 1 calc PR D 9 H47D H 0.0915 1.1964 0.3338 0.046 Uiso 0.625(3) 1 calc PR D 9 C48B C 0.1745(3) 1.2817(2) 0.29871(12) 0.0435(10) Uani 0.625(3) 1 d P D 9 H48D H 0.2440 1.2869 0.2927 0.065 Uiso 0.625(3) 1 calc PR D 9 H48E H 0.1635 1.3443 0.3201 0.065 Uiso 0.625(3) 1 calc PR D 9 H48F H 0.1257 1.2687 0.2662 0.065 Uiso 0.625(3) 1 calc PR D 9 C45D C 0.15711(13) 1.01860(12) 0.32185(6) 0.0287(5) Uani 0.37 1 d PD D 10 H45G H 0.0901 1.0383 0.3273 0.034 Uiso 0.375(3) 1 calc PR D 10 H45H H 0.2003 1.0208 0.3555 0.034 Uiso 0.375(3) 1 calc PR D 10 C46D C 0.2058(7) 1.0929(9) 0.2973(5) 0.045(3) Uani 0.375(3) 1 d PD D 10 H46G H 0.1824 1.0719 0.2601 0.054 Uiso 0.375(3) 1 calc PR D 10 H46H H 0.2806 1.0922 0.3052 0.054 Uiso 0.375(3) 1 calc PR D 10 C47D C 0.1803(13) 1.2049(14) 0.3156(7) 0.047(4) Uani 0.375(3) 1 d P D 10 H47G H 0.1850 1.2195 0.3528 0.056 Uiso 0.375(3) 1 calc PR D 10 H47H H 0.2314 1.2522 0.3082 0.056 Uiso 0.375(3) 1 calc PR D 10 C48D C 0.0751(4) 1.2199(5) 0.2896(2) 0.062(2) Uani 0.375(3) 1 d P D 10 H48J H 0.0685 1.2003 0.2528 0.093 Uiso 0.375(3) 1 calc PR D 10 H48K H 0.0647 1.2902 0.2991 0.093 Uiso 0.375(3) 1 calc PR D 10 H48L H 0.0239 1.1788 0.3000 0.093 Uiso 0.375(3) 1 calc PR D 10 C49B C 0.23685(12) 0.88737(13) 0.27012(6) 0.0306(4) Uani 1 1 d . D . H49C H 0.2223 0.8192 0.2484 0.037 Uiso 1 1 calc R E 11 H49D H 0.2492 0.9337 0.2481 0.037 Uiso 1 1 calc R E 11 C50B C 0.33397(13) 0.89184(14) 0.30890(7) 0.0410(6) Uani 0.491(3) 1 d PD D 11 H50C H 0.3259 0.8472 0.3323 0.049 Uiso 0.491(3) 1 calc PR D 11 H50D H 0.3575 0.9606 0.3287 0.049 Uiso 0.491(3) 1 calc PR D 11 C51B C 0.4075(4) 0.8537(5) 0.2728(2) 0.0317(14) Uani 0.491(3) 1 d PD D 11 H51C H 0.3854 0.7827 0.2565 0.038 Uiso 0.491(3) 1 calc PR D 11 H51D H 0.4029 0.8920 0.2458 0.038 Uiso 0.491(3) 1 calc PR D 11 C52B C 0.5172(3) 0.8648(3) 0.30127(15) 0.0451(13) Uani 0.491(3) 1 d P D 11 H52D H 0.5400 0.9354 0.3166 0.068 Uiso 0.491(3) 1 calc PR D 11 H52E H 0.5603 0.8395 0.2777 0.068 Uiso 0.491(3) 1 calc PR D 11 H52F H 0.5221 0.8268 0.3279 0.068 Uiso 0.491(3) 1 calc PR D 11 C50D C 0.33397(13) 0.89184(14) 0.30890(7) 0.0410(6) Uani 0.51 1 d P D 12 H50G H 0.3157 0.8642 0.3370 0.049 Uiso 0.509(3) 1 calc PR D 12 H50H H 0.3596 0.9631 0.3230 0.049 Uiso 0.509(3) 1 calc PR D 12 C51D C 0.4226(5) 0.8391(6) 0.2927(2) 0.0502(18) Uani 0.509(3) 1 d P D 12 H51G H 0.4340 0.8559 0.2607 0.060 Uiso 0.509(3) 1 calc PR D 12 H51H H 0.4853 0.8639 0.3189 0.060 Uiso 0.509(3) 1 calc PR D 12 C52D C 0.4037(4) 0.7290(3) 0.28512(17) 0.0670(16) Uani 0.509(3) 1 d P D 12 H52J H 0.4003 0.7115 0.3176 0.101 Uiso 0.509(3) 1 calc PR D 12 H52K H 0.4592 0.6982 0.2717 0.101 Uiso 0.509(3) 1 calc PR D 12 H52L H 0.3390 0.7045 0.2611 0.101 Uiso 0.509(3) 1 calc PR D 12 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 O1A 0.0595(9) 0.0602(10) 0.0407(8) 0.0219(7) 0.0202(7) 0.0094(7) N1A 0.0346(9) 0.0364(10) 0.0598(12) 0.0276(9) 0.0193(8) 0.0085(8) N2A 0.0218(8) 0.0277(9) 0.0450(10) 0.0176(7) 0.0104(7) 0.0100(7) N3A 0.0196(8) 0.0281(9) 0.0247(8) 0.0076(6) 0.0046(7) 0.0025(7) N4A 0.0262(9) 0.0431(10) 0.0249(9) -0.0007(8) 0.0061(7) 0.0078(8) C1A 0.0225(9) 0.0248(10) 0.0330(10) 0.0088(8) 0.0066(8) 0.0038(7) C2A 0.0227(9) 0.0269(10) 0.0343(10) 0.0061(8) 0.0045(8) 0.0064(8) C3A 0.0260(10) 0.0331(11) 0.0453(12) 0.0064(9) 0.0069(9) 0.0091(8) C4A 0.0264(10) 0.0265(10) 0.0397(11) 0.0107(8) 0.0056(8) 0.0090(8) C5A 0.0345(11) 0.0334(11) 0.0485(12) 0.0150(9) 0.0060(9) 0.0147(9) C6A 0.0465(12) 0.0307(11) 0.0553(13) 0.0225(10) 0.0087(10) 0.0157(9) C7A 0.0467(12) 0.0285(11) 0.0510(13) 0.0198(9) 0.0129(10) 0.0054(9) C8A 0.0299(10) 0.0303(11) 0.0473(12) 0.0157(9) 0.0100(9) 0.0062(8) C9A 0.0286(10) 0.0247(10) 0.0396(11) 0.0152(8) 0.0067(8) 0.0094(8) C10A 0.0439(12) 0.0279(11) 0.0434(12) 0.0040(9) 0.0177(10) 0.0011(9) C11A 0.0453(12) 0.0362(12) 0.0651(14) 0.0169(10) 0.0315(11) 0.0070(10) C12A 0.0423(13) 0.0405(13) 0.0834(17) 0.0241(12) 0.0180(12) 0.0062(10) C13A 0.0447(14) 0.0652(16) 0.123(2) 0.0467(16) 0.0248(14) 0.0093(12) C14A 0.0208(9) 0.0241(9) 0.0311(10) 0.0094(8) 0.0080(7) 0.0057(7) C15A 0.0251(9) 0.0241(9) 0.0315(10) 0.0081(8) 0.0059(8) 0.0048(7) C16A 0.0340(11) 0.0277(10) 0.0409(11) 0.0059(9) 0.0035(9) 0.0052(8) C17A 0.0225(9) 0.0259(9) 0.0230(9) 0.0111(7) 0.0066(7) 0.0068(7) C18A 0.0225(9) 0.0255(9) 0.0265(9) 0.0127(7) 0.0065(7) 0.0068(7) C19A 0.0237(9) 0.0291(10) 0.0360(10) 0.0118(8) 0.0064(8) 0.0041(8) C20A 0.0253(9) 0.0279(10) 0.0222(9) 0.0123(8) 0.0031(7) 0.0061(8) C21A 0.0261(9) 0.0311(10) 0.0278(10) 0.0114(8) 0.0017(8) 0.0033(8) C22A 0.0360(11) 0.0290(10) 0.0280(10) 0.0072(8) -0.0012(8) 0.0035(8) C23A 0.0389(11) 0.0336(11) 0.0222(10) 0.0048(8) 0.0037(8) 0.0129(9) C24A 0.0273(10) 0.0378(11) 0.0194(9) 0.0078(8) 0.0026(8) 0.0083(8) C25A 0.0266(9) 0.0270(10) 0.0171(9) 0.0074(7) 0.0015(7) 0.0061(8) C26A 0.037(3) 0.036(5) 0.029(3) 0.004(3) 0.004(2) 0.016(3) O2A 0.0455(18) 0.052(3) 0.055(3) -0.027(2) 0.0043(16) 0.0165(16) C27A 0.046(5) 0.059(5) 0.058(6) 0.000(3) 0.023(4) 0.022(3) C28A 0.033(3) 0.046(4) 0.019(2) -0.005(2) 0.011(2) 0.012(2) C29A 0.045(5) 0.045(5) 0.058(6) -0.007(3) -0.004(3) 0.019(3) C26C 0.035(3) 0.031(4) 0.034(4) -0.010(3) 0.011(3) -0.001(3) O2C 0.050(2) 0.071(4) 0.051(3) -0.035(3) 0.028(2) -0.021(2) C27C 0.021(4) 0.065(6) 0.032(4) -0.014(3) 0.012(3) -0.005(3) C28C 0.079(5) 0.069(4) 0.089(5) 0.013(3) -0.001(4) -0.006(3) C29C 0.048(5) 0.074(9) 0.078(7) 0.010(5) 0.010(4) 0.029(4) O3A 0.0280(7) 0.0469(9) 0.0915(11) 0.0413(8) 0.0208(7) 0.0183(6) O4A 0.0238(7) 0.0384(8) 0.0506(8) 0.0069(6) 0.0077(6) 0.0036(6) C30A 0.0249(10) 0.0367(12) 0.0406(11) 0.0157(9) 0.0132(8) 0.0083(9) C31A 0.0221(9) 0.0289(10) 0.0336(10) 0.0093(8) 0.0107(8) 0.0045(8) C32A 0.0264(10) 0.0318(10) 0.0283(10) 0.0102(8) 0.0096(8) 0.0066(8) C33A 0.0298(10) 0.0473(12) 0.0341(11) 0.0176(9) 0.0103(9) 0.0140(9) C34A 0.0228(10) 0.0702(16) 0.0430(12) 0.0215(11) 0.0028(9) 0.0028(10) C35A 0.0369(12) 0.0454(13) 0.0606(15) 0.0056(11) 0.0026(11) -0.0116(10) C36A 0.0359(12) 0.0304(11) 0.0630(14) 0.0115(10) 0.0141(10) 0.0051(9) N5A 0.0283(9) 0.0613(11) 0.0295(9) 0.0235(8) 0.0024(7) 0.0082(8) C37A 0.0346(11) 0.0637(14) 0.0294(11) 0.0152(10) 0.0067(9) 0.0078(10) C38A 0.0353(12) 0.0736(16) 0.0457(13) 0.0169(11) 0.0079(10) 0.0110(11) C39A 0.0422(13) 0.0773(17) 0.0522(14) 0.0081(12) 0.0071(11) 0.0135(12) C40A 0.0498(15) 0.0858(18) 0.0717(17) 0.0197(14) 0.0220(13) 0.0198(13) C41A 0.0355(12) 0.0725(16) 0.0260(11) 0.0123(10) 0.0045(9) 0.0045(10) C42A 0.0510(18) 0.0511(18) 0.0310(15) 0.0130(13) 0.0120(13) 0.0174(15) C43A 0.084(2) 0.054(2) 0.0397(17) 0.0103(14) 0.0093(16) 0.0289(19) C44A 0.073(2) 0.068(2) 0.060(2) 0.0073(16) 0.0119(17) -0.0040(19) C41C 0.0355(12) 0.0725(16) 0.0260(11) 0.0123(10) 0.0045(9) 0.0045(10) C45A 0.0288(11) 0.0698(16) 0.0357(12) 0.0308(11) 0.0000(9) 0.0067(10) C46A 0.025(5) 0.135(11) 0.030(5) 0.034(7) 0.003(4) 0.001(7) C47A 0.033(5) 0.050(8) 0.055(8) 0.014(6) 0.007(5) 0.009(6) C48A 0.047(4) 0.100(7) 0.060(5) 0.035(5) 0.018(4) 0.027(5) C45C 0.0288(11) 0.0698(16) 0.0357(12) 0.0308(11) 0.0000(9) 0.0067(10) C46C 0.026(3) 0.058(3) 0.039(3) 0.017(3) -0.0029(19) 0.000(2) C47C 0.031(2) 0.055(4) 0.041(4) 0.024(3) 0.000(3) 0.001(4) C48C 0.038(2) 0.081(3) 0.055(2) 0.035(2) 0.0153(17) 0.016(2) C49A 0.0418(12) 0.0643(15) 0.0381(12) 0.0303(11) 0.0001(9) 0.0086(10) C50A 0.0515(14) 0.0721(17) 0.0566(15) 0.0387(13) 0.0020(11) 0.0076(12) C51A 0.0644(17) 0.0913(19) 0.0629(16) 0.0476(14) -0.0128(13) -0.0184(14) C52A 0.0648(16) 0.107(2) 0.0608(16) 0.0460(14) -0.0166(13) -0.0408(14) O1B 0.0448(8) 0.0752(10) 0.0469(9) 0.0329(8) 0.0186(7) 0.0016(7) O2B 0.0523(9) 0.0562(9) 0.0404(8) 0.0179(7) -0.0179(7) 0.0048(7) N1B 0.0242(8) 0.0465(10) 0.0352(9) 0.0195(8) 0.0095(7) 0.0028(7) N2B 0.0195(8) 0.0283(9) 0.0265(8) 0.0095(7) 0.0068(6) 0.0076(6) N3B 0.0184(7) 0.0205(8) 0.0233(8) 0.0055(6) 0.0017(6) 0.0036(6) N4B 0.0243(8) 0.0302(9) 0.0225(8) 0.0066(7) -0.0011(7) 0.0077(7) C1B 0.0187(9) 0.0258(9) 0.0190(9) 0.0064(7) 0.0005(7) 0.0026(7) C2B 0.0198(9) 0.0281(10) 0.0204(9) 0.0036(7) -0.0003(7) 0.0069(7) C3B 0.0287(10) 0.0300(10) 0.0308(10) 0.0037(8) 0.0013(8) 0.0112(8) C4B 0.0186(9) 0.0347(10) 0.0183(9) 0.0010(7) -0.0003(7) 0.0062(7) C5B 0.0251(10) 0.0485(12) 0.0225(10) 0.0032(8) 0.0027(8) 0.0162(9) C6B 0.0199(10) 0.0725(15) 0.0276(10) 0.0112(10) 0.0082(8) 0.0151(10) C7B 0.0221(10) 0.0640(14) 0.0293(10) 0.0186(9) 0.0074(8) 0.0054(9) C8B 0.0211(9) 0.0447(12) 0.0232(9) 0.0105(8) 0.0024(8) 0.0025(8) C9B 0.0156(8) 0.0370(10) 0.0194(9) 0.0068(8) 0.0019(7) 0.0048(7) C10B 0.0276(11) 0.0598(14) 0.0388(12) 0.0258(10) 0.0033(9) -0.0039(10) C11B 0.015(4) 0.066(5) 0.083(8) 0.050(5) -0.009(4) -0.007(3) C12B 0.040(5) 0.047(6) 0.100(9) 0.027(5) 0.020(6) 0.010(4) C13B 0.055(3) 0.042(3) 0.109(5) 0.035(3) 0.016(3) 0.006(2) C11D 0.017(4) 0.059(5) 0.046(4) 0.034(3) 0.004(4) -0.006(3) C12D 0.040(3) 0.037(4) 0.049(4) 0.019(3) 0.004(3) -0.006(3) C13D 0.038(2) 0.041(2) 0.040(2) 0.0126(18) 0.0027(18) -0.0049(17) C14B 0.0202(9) 0.0240(9) 0.0218(9) 0.0082(7) 0.0036(7) 0.0075(7) C15B 0.0223(9) 0.0267(9) 0.0229(9) 0.0056(7) 0.0065(7) 0.0059(7) C16B 0.0281(10) 0.0362(11) 0.0300(10) 0.0037(8) 0.0009(8) 0.0053(8) C17B 0.0197(9) 0.0249(9) 0.0203(9) 0.0065(7) 0.0082(7) 0.0075(7) C18B 0.0206(9) 0.0238(9) 0.0230(9) 0.0060(7) 0.0089(7) 0.0059(7) C19B 0.0295(10) 0.0251(10) 0.0292(10) 0.0065(8) 0.0096(8) 0.0061(8) C20B 0.0198(9) 0.0243(9) 0.0223(9) 0.0032(7) 0.0097(7) 0.0042(7) C21B 0.0234(9) 0.0296(10) 0.0289(10) 0.0019(8) 0.0112(8) 0.0014(8) C22B 0.0186(9) 0.0384(11) 0.0290(10) -0.0003(8) 0.0052(8) -0.0010(8) C23B 0.0189(9) 0.0399(11) 0.0240(9) 0.0054(8) 0.0041(7) 0.0076(8) C24B 0.0208(9) 0.0275(10) 0.0215(9) 0.0031(7) 0.0078(7) 0.0071(7) C25B 0.0171(8) 0.0270(9) 0.0187(9) 0.0033(7) 0.0057(7) 0.0052(7) C26B 0.0288(10) 0.0435(12) 0.0320(11) 0.0126(9) 0.0010(9) 0.0115(9) C27B 0.0370(11) 0.0408(12) 0.0389(11) 0.0208(9) 0.0014(9) 0.0148(9) C28B 0.0483(12) 0.0475(13) 0.0346(11) 0.0142(9) 0.0041(9) 0.0185(10) C29B 0.0727(16) 0.0527(14) 0.0548(14) 0.0203(11) 0.0120(12) 0.0345(12) O3B 0.0381(8) 0.0294(7) 0.0545(9) 0.0148(6) 0.0186(6) 0.0106(6) O4B 0.0300(7) 0.0252(7) 0.0412(8) 0.0081(6) -0.0002(6) 0.0024(5) C30B 0.0341(11) 0.0265(10) 0.0251(10) 0.0112(8) 0.0049(8) 0.0066(9) C31B 0.0330(10) 0.0255(10) 0.0254(9) 0.0098(8) 0.0032(8) 0.0037(8) C32B 0.0378(11) 0.0271(10) 0.0272(10) 0.0105(8) 0.0050(8) 0.0053(8) C33B 0.0525(13) 0.0305(11) 0.0323(11) 0.0128(9) 0.0096(9) 0.0140(10) C34B 0.0670(15) 0.0226(10) 0.0360(12) 0.0077(9) 0.0013(10) 0.0021(10) C35B 0.0456(13) 0.0311(12) 0.0464(13) 0.0101(9) -0.0063(10) -0.0070(10) C36B 0.0362(11) 0.0302(11) 0.0432(12) 0.0116(9) -0.0002(9) 0.0017(9) N5B 0.0294(8) 0.0284(8) 0.0210(8) 0.0025(6) 0.0078(6) 0.0049(6) C37B 0.0372(11) 0.0349(11) 0.0250(10) 0.0075(8) 0.0137(8) 0.0044(8) C38B 0.0630(14) 0.0334(12) 0.0463(13) 0.0059(9) 0.0283(11) 0.0006(10) C39B 0.0853(17) 0.0339(12) 0.0599(15) 0.0063(10) 0.0445(13) -0.0018(11) C40B 0.105(2) 0.0554(16) 0.092(2) 0.0212(14) 0.0446(17) 0.0008(14) C41B 0.0394(11) 0.0363(11) 0.0207(9) -0.0006(8) 0.0013(8) 0.0039(9) C42B 0.0331(11) 0.0592(14) 0.0342(11) 0.0005(10) -0.0002(9) 0.0053(10) C43B 0.0422(13) 0.0677(15) 0.0374(12) -0.0005(11) -0.0059(10) 0.0095(11) C44B 0.0460(14) 0.125(2) 0.0513(15) -0.0017(14) -0.0111(12) 0.0201(14) C45B 0.0339(11) 0.0291(11) 0.0213(10) -0.0002(8) 0.0057(8) 0.0078(8) C46B 0.067(4) 0.025(3) 0.028(2) 0.0118(17) 0.011(3) 0.018(3) C47B 0.058(5) 0.022(3) 0.038(4) 0.011(2) 0.010(3) 0.011(3) C48B 0.060(2) 0.0297(19) 0.043(2) 0.0162(16) 0.0070(17) 0.0018(16) C45D 0.0339(11) 0.0291(11) 0.0213(10) -0.0002(8) 0.0057(8) 0.0078(8) C46D 0.072(7) 0.035(4) 0.027(4) 0.004(3) 0.002(5) 0.034(5) C47D 0.056(7) 0.046(7) 0.026(7) -0.004(5) -0.003(5) -0.013(5) C48D 0.057(4) 0.077(5) 0.065(4) 0.024(4) 0.031(3) 0.029(4) C49B 0.0349(10) 0.0304(10) 0.0287(10) 0.0018(8) 0.0167(8) 0.0047(8) C50B 0.0333(11) 0.0441(13) 0.0461(13) 0.0065(10) 0.0113(10) 0.0091(9) C51B 0.016(3) 0.032(3) 0.043(4) 0.001(3) 0.000(3) 0.0089(19) C52B 0.026(2) 0.063(3) 0.039(2) -0.008(2) 0.0077(19) 0.005(2) C50D 0.0333(11) 0.0441(13) 0.0461(13) 0.0065(10) 0.0113(10) 0.0091(9) C51D 0.042(4) 0.063(4) 0.043(4) 0.007(3) 0.002(3) 0.025(3) C52D 0.095(4) 0.078(4) 0.055(3) 0.036(3) 0.039(3) 0.058(3) _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 O1A C10A 1.224(2) . ? N1A C10A 1.353(2) . ? N1A C8A 1.415(2) . ? N1A H1NA 0.89(2) . ? N2A C9A 1.368(2) . ? N2A C1A 1.386(2) . ? N2A H2NA 0.861(18) . ? N3A C25A 1.370(2) . ? N3A C17A 1.384(2) . ? N3A H3NA 0.838(17) . ? N4A C26C 1.334(7) . ? N4A C24A 1.411(2) . ? N4A C26A 1.425(8) . ? N4A H4NA 0.895(18) . ? C1A C2A 1.369(2) . ? C1A C14A 1.502(2) . ? C2A C4A 1.431(2) . ? C2A C3A 1.503(2) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A C5A 1.399(2) . ? C4A C9A 1.407(2) . ? C5A C6A 1.369(2) . ? C5A H5A 0.9500 . ? C6A C7A 1.402(2) . ? C6A H6A 0.9500 . ? C7A C8A 1.381(2) . ? C7A H7A 0.9500 . ? C8A C9A 1.399(2) . ? C10A C11A 1.510(3) . ? C11A C12A 1.521(3) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.530(3) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A C17A 1.497(2) . ? C14A C15A 1.541(2) . ? C14A H14A 1.0000 . ? C15A C16A 1.513(2) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A C18A 1.362(2) . ? C18A C20A 1.430(2) . ? C18A C19A 1.504(2) . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A C21A 1.408(2) . ? C20A C25A 1.411(2) . ? C21A C22A 1.371(2) . ? C21A H21A 0.9500 . ? C22A C23A 1.396(2) . ? C22A H22A 0.9500 . ? C23A C24A 1.388(2) . ? C23A H23A 0.9500 . ? C24A C25A 1.404(2) . ? C26A O2A 1.203(8) . ? C26A C27A 1.496(6) . ? C27A C28A 1.457(6) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A C29A 1.524(6) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C26C O2C 1.221(8) . ? C26C C27C 1.501(6) . ? C27C C28C 1.460(7) . ? C27C H27E 0.9900 . ? C27C H27F 0.9900 . ? C28C C29C 1.524(7) . ? C28C H28E 0.9900 . ? C28C H28F 0.9900 . ? C29C H29G 0.9800 . ? C29C H29H 0.9800 . ? C29C H29I 0.9800 . ? O3A C30A 1.2512(19) . ? O4A C30A 1.261(2) . ? C30A C31A 1.500(2) . ? C31A C32A 1.382(2) . ? C31A C36A 1.384(2) . ? C32A C33A 1.381(2) . ? C32A H32A 0.9500 . ? C33A C34A 1.377(3) . ? C33A H33A 0.9500 . ? C34A C35A 1.375(3) . ? C34A H34A 0.9500 . ? C35A C36A 1.382(3) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? N5A C49A 1.509(2) . ? N5A C41A 1.515(2) . ? N5A C37A 1.516(2) . ? N5A C45A 1.520(2) . ? C37A C38A 1.523(2) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A C39A 1.526(3) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A C40A 1.496(3) . ? C39A H39A 0.9900 . ? C39A H39B 0.9900 . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? C41A C42A 1.553(3) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A C43A 1.527(4) . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? C43A C44A 1.520(4) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C42C C43C 1.59(2) . ? C42C H42E 0.9900 . ? C42C H42F 0.9900 . ? C43C C44C 1.523(10) . ? C43C H43E 0.9900 . ? C43C H43F 0.9900 . ? C44C H44G 0.9800 . ? C44C H44H 0.9800 . ? C44C H44I 0.9800 . ? C45A C46A 1.464(12) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A C47A 1.47(2) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A C48A 1.46(2) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C46C C47C 1.538(11) . ? C46C H46E 0.9900 . ? C46C H46F 0.9900 . ? C47C C48C 1.510(9) . ? C47C H47E 0.9900 . ? C47C H47F 0.9900 . ? C48C H48G 0.9800 . ? C48C H48H 0.9800 . ? C48C H48I 0.9800 . ? C49A C50A 1.499(3) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A C51A 1.545(3) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C51A C52A 1.504(3) . ? C51A H51A 0.9900 . ? C51A H51B 0.9900 . ? C52A H52A 0.9800 . ? C52A H52B 0.9800 . ? C52A H52C 0.9800 . ? O1B C10B 1.228(2) . ? O2B C26B 1.225(2) . ? N1B C10B 1.358(2) . ? N1B C8B 1.417(2) . ? N1B H1NB 0.917(19) . ? N2B C9B 1.3767(19) . ? N2B C1B 1.379(2) . ? N2B H2NB 0.916(17) . ? N3B C25B 1.3771(19) . ? N3B C17B 1.3871(19) . ? N3B H3NB 0.905(17) . ? N4B C26B 1.355(2) . ? N4B C24B 1.406(2) . ? N4B H4NB 0.862(17) . ? C1B C2B 1.374(2) . ? C1B C14B 1.507(2) . ? C2B C4B 1.435(2) . ? C2B C3B 1.495(2) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4B C9B 1.401(2) . ? C4B C5B 1.406(2) . ? C5B C6B 1.377(2) . ? C5B H5B 0.9500 . ? C6B C7B 1.389(2) . ? C6B H6B 0.9500 . ? C7B C8B 1.386(2) . ? C7B H7B 0.9500 . ? C8B C9B 1.406(2) . ? C10B C11B 1.510(6) . ? C10B C11D 1.519(6) . ? C11B C12B 1.515(7) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.530(12) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C11D C12D 1.524(6) . ? C11D H11G 0.9900 . ? C11D H11H 0.9900 . ? C12D C13D 1.525(10) . ? C12D H12G 0.9900 . ? C12D H12H 0.9900 . ? C13D H13J 0.9800 . ? C13D H13K 0.9800 . ? C13D H13L 0.9800 . ? C14B C17B 1.500(2) . ? C14B C15B 1.534(2) . ? C14B H14B 1.0000 . ? C15B C16B 1.524(2) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B C18B 1.365(2) . ? C18B C20B 1.429(2) . ? C18B C19B 1.499(2) . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B C21B 1.403(2) . ? C20B C25B 1.403(2) . ? C21B C22B 1.372(2) . ? C21B H21B 0.9500 . ? C22B C23B 1.396(2) . ? C22B H22B 0.9500 . ? C23B C24B 1.384(2) . ? C23B H23B 0.9500 . ? C24B C25B 1.407(2) . ? C26B C27B 1.495(2) . ? C27B C28B 1.529(2) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B C29B 1.514(3) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? O3B C30B 1.2604(19) . ? O4B C30B 1.2537(19) . ? C30B C31B 1.504(2) . ? C31B C36B 1.386(2) . ? C31B C32B 1.389(2) . ? C32B C33B 1.390(2) . ? C32B H32B 0.9500 . ? C33B C34B 1.376(3) . ? C33B H33B 0.9500 . ? C34B C35B 1.375(3) . ? C34B H34B 0.9500 . ? C35B C36B 1.382(2) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? N5B C37B 1.514(2) . ? N5B C41B 1.517(2) . ? N5B C45B 1.518(2) . ? N5B C49B 1.520(2) . ? C37B C38B 1.519(2) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38B C39B 1.529(3) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B C40B 1.504(3) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C41B C42B 1.508(2) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B C43B 1.515(2) . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? C43B C44B 1.515(3) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C45B C46B 1.517(6) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B C47B 1.468(14) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B C48B 1.506(10) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C46D C47D 1.61(2) . ? C46D H46G 0.9900 . ? C46D H46H 0.9900 . ? C47D C48D 1.511(19) . ? C47D H47G 0.9900 . ? C47D H47H 0.9900 . ? C48D H48J 0.9800 . ? C48D H48K 0.9800 . ? C48D H48L 0.9800 . ? C49B C50B 1.513(2) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50B C51B 1.573(6) . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? C51B C52B 1.517(7) . ? C51B H51C 0.9900 . ? C51B H51D 0.9900 . ? C52B H52D 0.9800 . ? C52B H52E 0.9800 . ? C52B H52F 0.9800 . ? C51D C52D 1.487(9) . ? C51D H51G 0.9900 . ? C51D H51H 0.9900 . ? C52D H52J 0.9800 . ? C52D H52K 0.9800 . ? C52D H52L 0.9800 . ? 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 C10A N1A C8A 128.28(17) . . ? C10A N1A H1NA 116.4(12) . . ? C8A N1A H1NA 115.3(12) . . ? C9A N2A C1A 108.83(14) . . ? C9A N2A H2NA 125.0(12) . . ? C1A N2A H2NA 125.5(13) . . ? C25A N3A C17A 108.98(14) . . ? C25A N3A H3NA 123.8(12) . . ? C17A N3A H3NA 127.2(12) . . ? C26C N4A C24A 129.8(3) . . ? C26C N4A C26A 26.2(3) . . ? C24A N4A C26A 124.0(4) . . ? C26C N4A H4NA 110.5(12) . . ? C24A N4A H4NA 117.9(11) . . ? C26A N4A H4NA 116.6(12) . . ? C2A C1A N2A 109.55(14) . . ? C2A C1A C14A 130.91(15) . . ? N2A C1A C14A 119.53(14) . . ? C1A C2A C4A 106.54(14) . . ? C1A C2A C3A 128.19(15) . . ? C4A C2A C3A 125.25(14) . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C5A C4A C9A 119.01(16) . . ? C5A C4A C2A 133.65(16) . . ? C9A C4A C2A 107.33(14) . . ? C6A C5A C4A 118.49(17) . . ? C6A C5A H5A 120.8 . . ? C4A C5A H5A 120.8 . . ? C5A C6A C7A 122.27(17) . . ? C5A C6A H6A 118.9 . . ? C7A C6A H6A 118.9 . . ? C8A C7A C6A 120.59(17) . . ? C8A C7A H7A 119.7 . . ? C6A C7A H7A 119.7 . . ? C7A C8A C9A 117.20(16) . . ? C7A C8A N1A 124.97(16) . . ? C9A C8A N1A 117.78(15) . . ? N2A C9A C8A 129.82(15) . . ? N2A C9A C4A 107.73(15) . . ? C8A C9A C4A 122.44(15) . . ? O1A C10A N1A 123.46(18) . . ? O1A C10A C11A 122.04(17) . . ? N1A C10A C11A 114.46(17) . . ? C10A C11A C12A 111.29(16) . . ? C10A C11A H11A 109.4 . . ? C12A C11A H11A 109.4 . . ? C10A C11A H11B 109.4 . . ? C12A C11A H11B 109.4 . . ? H11A C11A H11B 108.0 . . ? C11A C12A C13A 112.42(18) . . ? C11A C12A H12A 109.1 . . ? C13A C12A H12A 109.1 . . ? C11A C12A H12B 109.1 . . ? C13A C12A H12B 109.1 . . ? H12A C12A H12B 107.9 . . ? C12A C13A H13A 109.5 . . ? C12A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C12A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C17A C14A C1A 112.58(13) . . ? C17A C14A C15A 112.17(12) . . ? C1A C14A C15A 111.38(13) . . ? C17A C14A H14A 106.8 . . ? C1A C14A H14A 106.8 . . ? C15A C14A H14A 106.8 . . ? C16A C15A C14A 112.63(13) . . ? C16A C15A H15A 109.1 . . ? C14A C15A H15A 109.1 . . ? C16A C15A H15B 109.1 . . ? C14A C15A H15B 109.1 . . ? H15A C15A H15B 107.8 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C18A C17A N3A 109.41(14) . . ? C18A C17A C14A 129.82(14) . . ? N3A C17A C14A 120.77(14) . . ? C17A C18A C20A 107.15(14) . . ? C17A C18A C19A 126.55(15) . . ? C20A C18A C19A 126.26(14) . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C21A C20A C25A 118.61(15) . . ? C21A C20A C18A 134.53(15) . . ? C25A C20A C18A 106.86(14) . . ? C22A C21A C20A 118.50(16) . . ? C22A C21A H21A 120.7 . . ? C20A C21A H21A 120.7 . . ? C21A C22A C23A 122.40(16) . . ? C21A C22A H22A 118.8 . . ? C23A C22A H22A 118.8 . . ? C24A C23A C22A 120.98(16) . . ? C24A C23A H23A 119.5 . . ? C22A C23A H23A 119.5 . . ? C23A C24A C25A 116.71(15) . . ? C23A C24A N4A 124.81(16) . . ? C25A C24A N4A 118.48(15) . . ? N3A C25A C24A 129.61(15) . . ? N3A C25A C20A 107.60(14) . . ? C24A C25A C20A 122.78(15) . . ? O2A C26A N4A 126.9(6) . . ? O2A C26A C27A 122.6(9) . . ? N4A C26A C27A 110.2(8) . . ? C28A C27A C26A 109.0(6) . . ? C28A C27A H27A 109.9 . . ? C26A C27A H27A 109.9 . . ? C28A C27A H27B 109.9 . . ? C26A C27A H27B 109.9 . . ? H27A C27A H27B 108.3 . . ? C27A C28A C29A 114.7(6) . . ? C27A C28A H28A 108.6 . . ? C29A C28A H28A 108.6 . . ? C27A C28A H28B 108.6 . . ? C29A C28A H28B 108.6 . . ? H28A C28A H28B 107.6 . . ? O2C C26C N4A 121.1(6) . . ? O2C C26C C27C 119.8(9) . . ? N4A C26C C27C 118.5(8) . . ? C28C C27C C26C 117.8(8) . . ? C28C C27C H27E 107.9 . . ? C26C C27C H27E 107.9 . . ? C28C C27C H27F 107.9 . . ? C26C C27C H27F 107.9 . . ? H27E C27C H27F 107.2 . . ? C27C C28C C29C 114.6(7) . . ? C27C C28C H28E 108.6 . . ? C29C C28C H28E 108.6 . . ? C27C C28C H28F 108.6 . . ? C29C C28C H28F 108.6 . . ? H28E C28C H28F 107.6 . . ? C28C C29C H29G 109.5 . . ? C28C C29C H29H 109.5 . . ? H29G C29C H29H 109.5 . . ? C28C C29C H29I 109.5 . . ? H29G C29C H29I 109.5 . . ? H29H C29C H29I 109.5 . . ? O3A C30A O4A 124.22(16) . . ? O3A C30A C31A 118.67(16) . . ? O4A C30A C31A 117.09(15) . . ? C32A C31A C36A 118.54(16) . . ? C32A C31A C30A 121.07(15) . . ? C36A C31A C30A 120.35(16) . . ? C33A C32A C31A 121.15(16) . . ? C33A C32A H32A 119.4 . . ? C31A C32A H32A 119.4 . . ? C34A C33A C32A 119.57(17) . . ? C34A C33A H33A 120.2 . . ? C32A C33A H33A 120.2 . . ? C35A C34A C33A 120.08(18) . . ? C35A C34A H34A 120.0 . . ? C33A C34A H34A 120.0 . . ? C34A C35A C36A 120.07(18) . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C35A C36A C31A 120.59(18) . . ? C35A C36A H36A 119.7 . . ? C31A C36A H36A 119.7 . . ? C49A N5A C41A 105.37(14) . . ? C49A N5A C37A 111.88(15) . . ? C41A N5A C37A 111.11(14) . . ? C49A N5A C45A 111.26(14) . . ? C41A N5A C45A 110.90(14) . . ? C37A N5A C45A 106.41(13) . . ? N5A C37A C38A 115.39(15) . . ? N5A C37A H37A 108.4 . . ? C38A C37A H37A 108.4 . . ? N5A C37A H37B 108.4 . . ? C38A C37A H37B 108.4 . . ? H37A C37A H37B 107.5 . . ? C37A C38A C39A 110.90(16) . . ? C37A C38A H38A 109.5 . . ? C39A C38A H38A 109.5 . . ? C37A C38A H38B 109.5 . . ? C39A C38A H38B 109.5 . . ? H38A C38A H38B 108.0 . . ? C40A C39A C38A 112.18(18) . . ? C40A C39A H39A 109.2 . . ? C38A C39A H39A 109.2 . . ? C40A C39A H39B 109.2 . . ? C38A C39A H39B 109.2 . . ? H39A C39A H39B 107.9 . . ? C39A C40A H40A 109.5 . . ? C39A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C39A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N5A C41A C42A 115.59(16) . . ? N5A C41A H41A 108.4 . . ? C42A C41A H41A 108.4 . . ? N5A C41A H41B 108.4 . . ? C42A C41A H41B 108.4 . . ? H41A C41A H41B 107.4 . . ? C43A C42A C41A 112.6(2) . . ? C43A C42A H42A 109.1 . . ? C41A C42A H42A 109.1 . . ? C43A C42A H42B 109.1 . . ? C41A C42A H42B 109.1 . . ? H42A C42A H42B 107.8 . . ? C44A C43A C42A 113.2(3) . . ? C44A C43A H43A 108.9 . . ? C42A C43A H43A 108.9 . . ? C44A C43A H43B 108.9 . . ? C42A C43A H43B 108.9 . . ? H43A C43A H43B 107.7 . . ? C43C C42C H42E 111.6 . . ? C43C C42C H42F 111.6 . . ? H42E C42C H42F 109.4 . . ? C44C C43C C42C 109.1(10) . . ? C44C C43C H43E 109.9 . . ? C42C C43C H43E 109.9 . . ? C44C C43C H43F 109.9 . . ? C42C C43C H43F 109.9 . . ? H43E C43C H43F 108.3 . . ? C46A C45A N5A 119.9(5) . . ? C46A C45A H45A 107.3 . . ? N5A C45A H45A 107.3 . . ? C46A C45A H45B 107.3 . . ? N5A C45A H45B 107.3 . . ? H45A C45A H45B 106.9 . . ? C45A C46A C47A 116.0(11) . . ? C45A C46A H46A 108.3 . . ? C47A C46A H46A 108.3 . . ? C45A C46A H46B 108.3 . . ? C47A C46A H46B 108.3 . . ? H46A C46A H46B 107.4 . . ? C48A C47A C46A 115.4(13) . . ? C48A C47A H47A 108.4 . . ? C46A C47A H47A 108.4 . . ? C48A C47A H47B 108.4 . . ? C46A C47A H47B 108.4 . . ? H47A C47A H47B 107.5 . . ? C47C C46C H46E 110.1 . . ? C47C C46C H46F 110.1 . . ? H46E C46C H46F 108.4 . . ? C48C C47C C46C 113.0(5) . . ? C48C C47C H47E 109.0 . . ? C46C C47C H47E 109.0 . . ? C48C C47C H47F 109.0 . . ? C46C C47C H47F 109.0 . . ? H47E C47C H47F 107.8 . . ? C50A C49A N5A 115.81(16) . . ? C50A C49A H49A 108.3 . . ? N5A C49A H49A 108.3 . . ? C50A C49A H49B 108.3 . . ? N5A C49A H49B 108.3 . . ? H49A C49A H49B 107.4 . . ? C49A C50A C51A 109.96(19) . . ? C49A C50A H50A 109.7 . . ? C51A C50A H50A 109.7 . . ? C49A C50A H50B 109.7 . . ? C51A C50A H50B 109.7 . . ? H50A C50A H50B 108.2 . . ? C52A C51A C50A 111.75(19) . . ? C52A C51A H51A 109.3 . . ? C50A C51A H51A 109.3 . . ? C52A C51A H51B 109.3 . . ? C50A C51A H51B 109.3 . . ? H51A C51A H51B 107.9 . . ? C51A C52A H52A 109.5 . . ? C51A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C10B N1B C8B 127.71(17) . . ? C10B N1B H1NB 116.2(11) . . ? C8B N1B H1NB 115.9(11) . . ? C9B N2B C1B 108.93(13) . . ? C9B N2B H2NB 124.9(11) . . ? C1B N2B H2NB 126.0(11) . . ? C25B N3B C17B 108.17(13) . . ? C25B N3B H3NB 123.4(11) . . ? C17B N3B H3NB 128.2(11) . . ? C26B N4B C24B 127.54(16) . . ? C26B N4B H4NB 115.4(11) . . ? C24B N4B H4NB 117.0(11) . . ? C2B C1B N2B 109.66(14) . . ? C2B C1B C14B 130.49(14) . . ? N2B C1B C14B 119.82(13) . . ? C1B C2B C4B 106.29(14) . . ? C1B C2B C3B 128.37(15) . . ? C4B C2B C3B 125.33(14) . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C9B C4B C5B 119.21(15) . . ? C9B C4B C2B 107.51(13) . . ? C5B C4B C2B 133.23(16) . . ? C6B C5B C4B 118.02(16) . . ? C6B C5B H5B 121.0 . . ? C4B C5B H5B 121.0 . . ? C5B C6B C7B 122.39(16) . . ? C5B C6B H6B 118.8 . . ? C7B C6B H6B 118.8 . . ? C8B C7B C6B 121.12(17) . . ? C8B C7B H7B 119.4 . . ? C6B C7B H7B 119.4 . . ? C7B C8B C9B 116.70(16) . . ? C7B C8B N1B 124.88(16) . . ? C9B C8B N1B 118.39(15) . . ? N2B C9B C4B 107.59(14) . . ? N2B C9B C8B 129.90(15) . . ? C4B C9B C8B 122.50(15) . . ? O1B C10B N1B 123.98(19) . . ? O1B C10B C11B 121.8(7) . . ? N1B C10B C11B 113.8(7) . . ? O1B C10B C11D 119.8(5) . . ? N1B C10B C11D 115.8(5) . . ? C11B C10B C11D 13.2(9) . . ? C10B C11B C12B 102.5(8) . . ? C10B C11B H11C 111.3 . . ? C12B C11B H11C 111.3 . . ? C10B C11B H11D 111.3 . . ? C12B C11B H11D 111.3 . . ? H11C C11B H11D 109.2 . . ? C11B C12B C13B 107.0(8) . . ? C11B C12B H12C 110.3 . . ? C13B C12B H12C 110.3 . . ? C11B C12B H12D 110.3 . . ? C13B C12B H12D 110.3 . . ? H12C C12B H12D 108.6 . . ? C10B C11D C12D 120.0(7) . . ? C10B C11D H11G 107.3 . . ? C12D C11D H11G 107.3 . . ? C10B C11D H11H 107.3 . . ? C12D C11D H11H 107.3 . . ? H11G C11D H11H 106.9 . . ? C11D C12D C13D 111.8(9) . . ? C11D C12D H12G 109.3 . . ? C13D C12D H12G 109.3 . . ? C11D C12D H12H 109.3 . . ? C13D C12D H12H 109.3 . . ? H12G C12D H12H 107.9 . . ? C17B C14B C1B 112.39(13) . . ? C17B C14B C15B 112.82(12) . . ? C1B C14B C15B 111.49(13) . . ? C17B C14B H14B 106.5 . . ? C1B C14B H14B 106.5 . . ? C15B C14B H14B 106.5 . . ? C16B C15B C14B 112.03(13) . . ? C16B C15B H15C 109.2 . . ? C14B C15B H15C 109.2 . . ? C16B C15B H15D 109.2 . . ? C14B C15B H15D 109.2 . . ? H15C C15B H15D 107.9 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C18B C17B N3B 109.57(14) . . ? C18B C17B C14B 128.73(14) . . ? N3B C17B C14B 121.69(14) . . ? C17B C18B C20B 107.20(13) . . ? C17B C18B C19B 126.84(14) . . ? C20B C18B C19B 125.94(14) . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C21B C20B C25B 119.52(14) . . ? C21B C20B C18B 133.68(15) . . ? C25B C20B C18B 106.79(13) . . ? C22B C21B C20B 118.29(16) . . ? C22B C21B H21B 120.9 . . ? C20B C21B H21B 120.9 . . ? C21B C22B C23B 121.94(16) . . ? C21B C22B H22B 119.0 . . ? C23B C22B H22B 119.0 . . ? C24B C23B C22B 121.39(15) . . ? C24B C23B H23B 119.3 . . ? C22B C23B H23B 119.3 . . ? C23B C24B N4B 124.26(15) . . ? C23B C24B C25B 116.75(15) . . ? N4B C24B C25B 118.94(14) . . ? N3B C25B C20B 108.27(13) . . ? N3B C25B C24B 129.61(14) . . ? C20B C25B C24B 122.11(14) . . ? O2B C26B N4B 123.08(17) . . ? O2B C26B C27B 121.63(16) . . ? N4B C26B C27B 115.18(16) . . ? C26B C27B C28B 110.13(15) . . ? C26B C27B H27C 109.6 . . ? C28B C27B H27C 109.6 . . ? C26B C27B H27D 109.6 . . ? C28B C27B H27D 109.6 . . ? H27C C27B H27D 108.1 . . ? C29B C28B C27B 113.34(16) . . ? C29B C28B H28C 108.9 . . ? C27B C28B H28C 108.9 . . ? C29B C28B H28D 108.9 . . ? C27B C28B H28D 108.9 . . ? H28C C28B H28D 107.7 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O4B C30B O3B 124.28(16) . . ? O4B C30B C31B 118.72(15) . . ? O3B C30B C31B 116.97(16) . . ? C36B C31B C32B 118.77(16) . . ? C36B C31B C30B 120.48(15) . . ? C32B C31B C30B 120.70(15) . . ? C31B C32B C33B 120.40(17) . . ? C31B C32B H32B 119.8 . . ? C33B C32B H32B 119.8 . . ? C34B C33B C32B 119.64(17) . . ? C34B C33B H33B 120.2 . . ? C32B C33B H33B 120.2 . . ? C35B C34B C33B 120.67(18) . . ? C35B C34B H34B 119.7 . . ? C33B C34B H34B 119.7 . . ? C34B C35B C36B 119.60(18) . . ? C34B C35B H35B 120.2 . . ? C36B C35B H35B 120.2 . . ? C35B C36B C31B 120.92(17) . . ? C35B C36B H36B 119.5 . . ? C31B C36B H36B 119.5 . . ? C37B N5B C41B 110.66(13) . . ? C37B N5B C45B 106.72(12) . . ? C41B N5B C45B 111.63(12) . . ? C37B N5B C49B 111.39(12) . . ? C41B N5B C49B 105.52(12) . . ? C45B N5B C49B 111.00(12) . . ? N5B C37B C38B 116.16(13) . . ? N5B C37B H37C 108.2 . . ? C38B C37B H37C 108.2 . . ? N5B C37B H37D 108.2 . . ? C38B C37B H37D 108.2 . . ? H37C C37B H37D 107.4 . . ? C37B C38B C39B 111.01(15) . . ? C37B C38B H38C 109.4 . . ? C39B C38B H38C 109.4 . . ? C37B C38B H38D 109.4 . . ? C39B C38B H38D 109.4 . . ? H38C C38B H38D 108.0 . . ? C40B C39B C38B 112.63(18) . . ? C40B C39B H39C 109.1 . . ? C38B C39B H39C 109.1 . . ? C40B C39B H39D 109.1 . . ? C38B C39B H39D 109.1 . . ? H39C C39B H39D 107.8 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C42B C41B N5B 116.84(14) . . ? C42B C41B H41C 108.1 . . ? N5B C41B H41C 108.1 . . ? C42B C41B H41D 108.1 . . ? N5B C41B H41D 108.1 . . ? H41C C41B H41D 107.3 . . ? C41B C42B C43B 110.42(15) . . ? C41B C42B H42C 109.6 . . ? C43B C42B H42C 109.6 . . ? C41B C42B H42D 109.6 . . ? C43B C42B H42D 109.6 . . ? H42C C42B H42D 108.1 . . ? C44B C43B C42B 113.99(17) . . ? C44B C43B H43C 108.8 . . ? C42B C43B H43C 108.8 . . ? C44B C43B H43D 108.8 . . ? C42B C43B H43D 108.8 . . ? H43C C43B H43D 107.6 . . ? C43B C44B H44D 109.5 . . ? C43B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C43B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C46B C45B N5B 116.0(3) . . ? C46B C45B H45C 108.3 . . ? N5B C45B H45C 108.3 . . ? C46B C45B H45D 108.3 . . ? N5B C45B H45D 108.3 . . ? H45C C45B H45D 107.4 . . ? C47B C46B C45B 110.2(6) . . ? C47B C46B H46C 109.6 . . ? C45B C46B H46C 109.6 . . ? C47B C46B H46D 109.6 . . ? C45B C46B H46D 109.6 . . ? H46C C46B H46D 108.1 . . ? C46B C47B C48B 112.0(7) . . ? C46B C47B H47C 109.2 . . ? C48B C47B H47C 109.2 . . ? C46B C47B H47D 109.2 . . ? C48B C47B H47D 109.2 . . ? H47C C47B H47D 107.9 . . ? C47D C46D H46G 108.9 . . ? C47D C46D H46H 108.9 . . ? H46G C46D H46H 107.7 . . ? C48D C47D C46D 111.7(13) . . ? C48D C47D H47G 109.3 . . ? C46D C47D H47G 109.3 . . ? C48D C47D H47H 109.3 . . ? C46D C47D H47H 109.3 . . ? H47G C47D H47H 107.9 . . ? C50B C49B N5B 116.70(14) . . ? C50B C49B H49C 108.1 . . ? N5B C49B H49C 108.1 . . ? C50B C49B H49D 108.1 . . ? N5B C49B H49D 108.1 . . ? H49C C49B H49D 107.3 . . ? C49B C50B C51B 100.1(2) . . ? C49B C50B H50C 111.8 . . ? C51B C50B H50C 111.8 . . ? C49B C50B H50D 111.8 . . ? C51B C50B H50D 111.8 . . ? H50C C50B H50D 109.5 . . ? C52B C51B C50B 111.9(4) . . ? C52B C51B H51C 109.2 . . ? C50B C51B H51C 109.2 . . ? C52B C51B H51D 109.2 . . ? C50B C51B H51D 109.2 . . ? H51C C51B H51D 107.9 . . ? C52D C51D H51G 109.1 . . ? C52D C51D H51H 109.1 . . ? H51G C51D H51H 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9A N2A C1A C2A -1.8(2) . . . . ? C9A N2A C1A C14A 177.48(15) . . . . ? N2A C1A C2A C4A 1.20(19) . . . . ? C14A C1A C2A C4A -177.95(17) . . . . ? N2A C1A C2A C3A 179.46(16) . . . . ? C14A C1A C2A C3A 0.3(3) . . . . ? C1A C2A C4A C5A 178.35(19) . . . . ? C3A C2A C4A C5A 0.0(3) . . . . ? C1A C2A C4A C9A -0.2(2) . . . . ? C3A C2A C4A C9A -178.54(16) . . . . ? C9A C4A C5A C6A 0.7(3) . . . . ? C2A C4A C5A C6A -177.72(19) . . . . ? C4A C5A C6A C7A -0.4(3) . . . . ? C5A C6A C7A C8A -0.1(3) . . . . ? C6A C7A C8A C9A 0.3(3) . . . . ? C6A C7A C8A N1A 177.57(18) . . . . ? C10A N1A C8A C7A 16.3(3) . . . . ? C10A N1A C8A C9A -166.47(18) . . . . ? C1A N2A C9A C8A -177.50(18) . . . . ? C1A N2A C9A C4A 1.6(2) . . . . ? C7A C8A C9A N2A 178.95(18) . . . . ? N1A C8A C9A N2A 1.5(3) . . . . ? C7A C8A C9A C4A 0.0(3) . . . . ? N1A C8A C9A C4A -177.48(17) . . . . ? C5A C4A C9A N2A -179.67(16) . . . . ? C2A C4A C9A N2A -0.9(2) . . . . ? C5A C4A C9A C8A -0.5(3) . . . . ? C2A C4A C9A C8A 178.33(16) . . . . ? C8A N1A C10A O1A 3.5(3) . . . . ? C8A N1A C10A C11A -174.42(17) . . . . ? O1A C10A C11A C12A -90.2(2) . . . . ? N1A C10A C11A C12A 87.8(2) . . . . ? C10A C11A C12A C13A 175.94(17) . . . . ? C2A C1A C14A C17A -104.1(2) . . . . ? N2A C1A C14A C17A 76.80(18) . . . . ? C2A C1A C14A C15A 128.87(19) . . . . ? N2A C1A C14A C15A -50.2(2) . . . . ? C17A C14A C15A C16A 173.35(14) . . . . ? C1A C14A C15A C16A -59.43(18) . . . . ? C25A N3A C17A C18A 0.32(17) . . . . ? C25A N3A C17A C14A -178.81(13) . . . . ? C1A C14A C17A C18A 98.23(19) . . . . ? C15A C14A C17A C18A -135.19(17) . . . . ? C1A C14A C17A N3A -82.84(17) . . . . ? C15A C14A C17A N3A 43.74(19) . . . . ? N3A C17A C18A C20A -0.44(17) . . . . ? C14A C17A C18A C20A 178.59(15) . . . . ? N3A C17A C18A C19A -178.32(14) . . . . ? C14A C17A C18A C19A 0.7(3) . . . . ? C17A C18A C20A C21A -179.79(17) . . . . ? C19A C18A C20A C21A -1.9(3) . . . . ? C17A C18A C20A C25A 0.39(17) . . . . ? C19A C18A C20A C25A 178.29(14) . . . . ? C25A C20A C21A C22A -0.6(2) . . . . ? C18A C20A C21A C22A 179.58(17) . . . . ? C20A C21A C22A C23A -0.2(2) . . . . ? C21A C22A C23A C24A 0.7(3) . . . . ? C22A C23A C24A C25A -0.5(2) . . . . ? C22A C23A C24A N4A -179.80(15) . . . . ? C26C N4A C24A C23A -27.2(6) . . . . ? C26A N4A C24A C23A 4.9(5) . . . . ? C26C N4A C24A C25A 153.5(6) . . . . ? C26A N4A C24A C25A -174.4(4) . . . . ? C17A N3A C25A C24A 178.91(15) . . . . ? C17A N3A C25A C20A -0.06(17) . . . . ? C23A C24A C25A N3A -179.16(15) . . . . ? N4A C24A C25A N3A 0.2(3) . . . . ? C23A C24A C25A C20A -0.3(2) . . . . ? N4A C24A C25A C20A 179.04(14) . . . . ? C21A C20A C25A N3A 179.95(14) . . . . ? C18A C20A C25A N3A -0.20(17) . . . . ? C21A C20A C25A C24A 0.9(2) . . . . ? C18A C20A C25A C24A -179.26(14) . . . . ? C26C N4A C26A O2A 104.8(15) . . . . ? C24A N4A C26A O2A -7.5(8) . . . . ? C26C N4A C26A C27A -68.9(13) . . . . ? C24A N4A C26A C27A 178.9(5) . . . . ? O2A C26A C27A C28A 57.7(14) . . . . ? N4A C26A C27A C28A -128.3(10) . . . . ? C26A C27A C28A C29A -171.6(12) . . . . ? C24A N4A C26C O2C 5.5(9) . . . . ? C26A N4A C26C O2C -81.9(13) . . . . ? C24A N4A C26C C27C 176.8(4) . . . . ? C26A N4A C26C C27C 89.4(14) . . . . ? O2C C26C C27C C28C 74.3(13) . . . . ? N4A C26C C27C C28C -97.2(13) . . . . ? C26C C27C C28C C29C -172.7(14) . . . . ? O3A C30A C31A C32A 173.88(16) . . . . ? O4A C30A C31A C32A -7.3(2) . . . . ? O3A C30A C31A C36A -8.6(3) . . . . ? O4A C30A C31A C36A 170.19(16) . . . . ? C36A C31A C32A C33A 0.1(2) . . . . ? C30A C31A C32A C33A 177.72(15) . . . . ? C31A C32A C33A C34A -0.6(3) . . . . ? C32A C33A C34A C35A 0.5(3) . . . . ? C33A C34A C35A C36A 0.0(3) . . . . ? C34A C35A C36A C31A -0.5(3) . . . . ? C32A C31A C36A C35A 0.4(3) . . . . ? C30A C31A C36A C35A -177.16(18) . . . . ? C49A N5A C37A C38A -66.4(2) . . . . ? C41A N5A C37A C38A 51.1(2) . . . . ? C45A N5A C37A C38A 171.92(17) . . . . ? N5A C37A C38A C39A 177.19(17) . . . . ? C37A C38A C39A C40A 174.74(18) . . . . ? C49A N5A C41A C42A -175.32(19) . . . . ? C37A N5A C41A C42A 63.3(2) . . . . ? C45A N5A C41A C42A -54.8(2) . . . . ? N5A C41A C42A C43A -171.4(2) . . . . ? C41A C42A C43A C44A 79.0(3) . . . . ? C49A N5A C45A C46A 45.2(6) . . . . ? C41A N5A C45A C46A -71.7(6) . . . . ? C37A N5A C45A C46A 167.3(6) . . . . ? N5A C45A C46A C47A -171.5(7) . . . . ? C45A C46A C47A C48A -171.2(9) . . . . ? C41A N5A C49A C50A -172.43(16) . . . . ? C37A N5A C49A C50A -51.6(2) . . . . ? C45A N5A C49A C50A 67.3(2) . . . . ? N5A C49A C50A C51A -163.62(16) . . . . ? C49A C50A C51A C52A 73.1(2) . . . . ? C9B N2B C1B C2B -1.21(18) . . . . ? C9B N2B C1B C14B 176.86(13) . . . . ? N2B C1B C2B C4B 1.63(17) . . . . ? C14B C1B C2B C4B -176.16(15) . . . . ? N2B C1B C2B C3B -177.57(15) . . . . ? C14B C1B C2B C3B 4.6(3) . . . . ? C1B C2B C4B C9B -1.46(17) . . . . ? C3B C2B C4B C9B 177.77(14) . . . . ? C1B C2B C4B C5B 175.96(17) . . . . ? C3B C2B C4B C5B -4.8(3) . . . . ? C9B C4B C5B C6B -0.5(2) . . . . ? C2B C4B C5B C6B -177.73(17) . . . . ? C4B C5B C6B C7B -1.0(3) . . . . ? C5B C6B C7B C8B 1.0(3) . . . . ? C6B C7B C8B C9B 0.6(2) . . . . ? C6B C7B C8B N1B 178.58(16) . . . . ? C10B N1B C8B C7B 17.0(3) . . . . ? C10B N1B C8B C9B -165.10(16) . . . . ? C1B N2B C9B C4B 0.24(17) . . . . ? C1B N2B C9B C8B -179.03(16) . . . . ? C5B C4B C9B N2B -177.09(14) . . . . ? C2B C4B C9B N2B 0.76(17) . . . . ? C5B C4B C9B C8B 2.2(2) . . . . ? C2B C4B C9B C8B -179.91(14) . . . . ? C7B C8B C9B N2B 176.93(16) . . . . ? N1B C8B C9B N2B -1.2(3) . . . . ? C7B C8B C9B C4B -2.2(2) . . . . ? N1B C8B C9B C4B 179.66(14) . . . . ? C8B N1B C10B O1B -2.7(3) . . . . ? C8B N1B C10B C11B 169.9(7) . . . . ? C8B N1B C10B C11D -175.8(5) . . . . ? O1B C10B C11B C12B -57.2(13) . . . . ? N1B C10B C11B C12B 130.0(9) . . . . ? C11D C10B C11B C12B 28(5) . . . . ? C10B C11B C12B C13B 171.9(9) . . . . ? O1B C10B C11D C12D -60.5(13) . . . . ? N1B C10B C11D C12D 112.8(9) . . . . ? C11B C10B C11D C12D -163(6) . . . . ? C10B C11D C12D C13D -53.9(13) . . . . ? C2B C1B C14B C17B -104.12(19) . . . . ? N2B C1B C14B C17B 78.27(17) . . . . ? C2B C1B C14B C15B 128.07(17) . . . . ? N2B C1B C14B C15B -49.54(18) . . . . ? C17B C14B C15B C16B 168.10(14) . . . . ? C1B C14B C15B C16B -64.33(17) . . . . ? C25B N3B C17B C18B -0.06(17) . . . . ? C25B N3B C17B C14B 178.92(13) . . . . ? C1B C14B C17B C18B 101.42(18) . . . . ? C15B C14B C17B C18B -131.48(16) . . . . ? C1B C14B C17B N3B -77.36(17) . . . . ? C15B C14B C17B N3B 49.74(19) . . . . ? N3B C17B C18B C20B 0.12(17) . . . . ? C14B C17B C18B C20B -178.77(14) . . . . ? N3B C17B C18B C19B -178.18(14) . . . . ? C14B C17B C18B C19B 2.9(3) . . . . ? C17B C18B C20B C21B 178.98(16) . . . . ? C19B C18B C20B C21B -2.7(3) . . . . ? C17B C18B C20B C25B -0.14(17) . . . . ? C19B C18B C20B C25B 178.18(14) . . . . ? C25B C20B C21B C22B 0.2(2) . . . . ? C18B C20B C21B C22B -178.85(16) . . . . ? C20B C21B C22B C23B 0.0(2) . . . . ? C21B C22B C23B C24B -0.8(2) . . . . ? C22B C23B C24B N4B -176.03(15) . . . . ? C22B C23B C24B C25B 1.2(2) . . . . ? C26B N4B C24B C23B -16.0(2) . . . . ? C26B N4B C24B C25B 166.84(15) . . . . ? C17B N3B C25B C20B -0.03(16) . . . . ? C17B N3B C25B C24B -179.47(15) . . . . ? C21B C20B C25B N3B -179.16(13) . . . . ? C18B C20B C25B N3B 0.10(16) . . . . ? C21B C20B C25B C24B 0.3(2) . . . . ? C18B C20B C25B C24B 179.59(14) . . . . ? C23B C24B C25B N3B 178.37(15) . . . . ? N4B C24B C25B N3B -4.2(2) . . . . ? C23B C24B C25B C20B -1.0(2) . . . . ? N4B C24B C25B C20B 176.38(14) . . . . ? C24B N4B C26B O2B -9.6(3) . . . . ? C24B N4B C26B C27B 166.60(15) . . . . ? O2B C26B C27B C28B 80.6(2) . . . . ? N4B C26B C27B C28B -95.67(18) . . . . ? C26B C27B C28B C29B 179.88(15) . . . . ? O4B C30B C31B C36B 171.92(16) . . . . ? O3B C30B C31B C36B -6.3(2) . . . . ? O4B C30B C31B C32B -5.4(2) . . . . ? O3B C30B C31B C32B 176.39(15) . . . . ? C36B C31B C32B C33B -0.6(2) . . . . ? C30B C31B C32B C33B 176.81(15) . . . . ? C31B C32B C33B C34B 0.0(3) . . . . ? C32B C33B C34B C35B 0.9(3) . . . . ? C33B C34B C35B C36B -1.2(3) . . . . ? C34B C35B C36B C31B 0.6(3) . . . . ? C32B C31B C36B C35B 0.3(3) . . . . ? C30B C31B C36B C35B -177.09(16) . . . . ? C41B N5B C37B C38B 62.70(19) . . . . ? C45B N5B C37B C38B -175.65(15) . . . . ? C49B N5B C37B C38B -54.35(19) . . . . ? N5B C37B C38B C39B 173.49(16) . . . . ? C37B C38B C39B C40B -174.03(19) . . . . ? C37B N5B C41B C42B 63.30(19) . . . . ? C45B N5B C41B C42B -55.4(2) . . . . ? C49B N5B C41B C42B -176.09(15) . . . . ? N5B C41B C42B C43B 177.65(16) . . . . ? C41B C42B C43B C44B -175.56(19) . . . . ? C37B N5B C45B C46B -172.0(3) . . . . ? C41B N5B C45B C46B -50.9(3) . . . . ? C49B N5B C45B C46B 66.5(3) . . . . ? N5B C45B C46B C47B 167.9(5) . . . . ? C45B C46B C47B C48B 177.3(6) . . . . ? C37B N5B C49B C50B -57.56(19) . . . . ? C41B N5B C49B C50B -177.69(15) . . . . ? C45B N5B C49B C50B 61.21(18) . . . . ? N5B C49B C50B C51B 175.9(3) . . . . ? C49B C50B C51B C52B 171.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1NA O3A 0.89(2) 2.02(2) 2.907(2) 171.1(18) . N2A H2NA O3A 0.861(18) 1.965(19) 2.8005(19) 163.2(17) . N3A H3NA O4A 0.838(17) 1.940(17) 2.7569(18) 164.3(16) . N4A H4NA O4A 0.895(18) 1.977(18) 2.865(2) 171.6(17) . N1B H1NB O3B 0.917(19) 1.954(19) 2.868(2) 173.6(17) . N2B H2NB O3B 0.916(17) 1.833(18) 2.7229(18) 163.3(16) . N3B H3NB O4B 0.905(17) 1.939(17) 2.8172(18) 163.1(15) . N4B H4NB O4B 0.862(17) 2.044(17) 2.8965(19) 169.8(16) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.455 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.037