# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Kyu-Sung Jeong' _publ_contact_author_address ; Department of Chemistry Yonsei University 134 Shinchon-dong, Seodaemoon-gu Seoul 120-749 SOUTH KOREA ; _publ_contact_author_email KSJEONG@YONSEI.AC.KR _publ_section_title ; Two distinct anion-binding modes and their relative stabilities ; loop_ _publ_author_name 'Kyu-Sung Jeong' 'Kyoung-Jin Chang' 'Nam-Kyun Kim' 'Myoung Soo Lah' 'Dohyun Moon' data_p6_55tr _database_code_depnum_ccdc_archive 'CCDC 643421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C230 H299 N24 O3.50' _chemical_formula_weight 3455.93 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 22.506(5) _cell_length_b 22.564(5) _cell_length_c 22.614(5) _cell_angle_alpha 65.145(5) _cell_angle_beta 85.503(5) _cell_angle_gamma 80.707(5) _cell_volume 10283(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 35508 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3750 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multiple wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal monochromator' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35508 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 35508 _reflns_number_gt 23553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.1267P)^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 35508 _refine_ls_number_parameters 2476 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1967 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1A C -0.04453(10) 0.28480(11) 0.62850(12) 0.0371(5) Uani 1 1 d . . . C2A C -0.05073(10) 0.34368(11) 0.57242(11) 0.0355(5) Uani 1 1 d . . . N3A N -0.00652(10) 0.38006(9) 0.53580(9) 0.0366(4) Uani 1 1 d . . . H3A H 0.0338(14) 0.3694(14) 0.5438(14) 0.064(9) Uiso 1 1 d . . . C4A C -0.03344(11) 0.43326(11) 0.48343(11) 0.0361(5) Uani 1 1 d . . . C5A C -0.00780(10) 0.48252(11) 0.43197(11) 0.0355(5) Uani 1 1 d . . . N6A N 0.05199(9) 0.49238(10) 0.41897(10) 0.0371(4) Uani 1 1 d . . . H6A H 0.0826(13) 0.4627(14) 0.4420(13) 0.054(8) Uiso 1 1 d . . . C7A C 0.05492(10) 0.54694(11) 0.36156(11) 0.0357(5) Uani 1 1 d . . . C8A C 0.10563(11) 0.57569(11) 0.32891(12) 0.0379(5) Uani 1 1 d . . . C9A C 0.09593(11) 0.62965(11) 0.26963(11) 0.0379(5) Uani 1 1 d . . . H9A H 0.1296 0.6503 0.2473 0.045 Uiso 1 1 calc R . . C10A C 0.03945(11) 0.65540(11) 0.24083(12) 0.0404(6) Uani 1 1 d . . . C11A C -0.01099(11) 0.62717(11) 0.27536(12) 0.0399(6) Uani 1 1 d . . . H11A' H -0.0501 0.6447 0.2575 0.048 Uiso 1 1 calc R . . C12A C -0.00346(11) 0.57325(11) 0.33591(12) 0.0387(5) Uani 1 1 d . . . C13A C -0.04448(10) 0.53194(11) 0.38274(12) 0.0370(5) Uani 1 1 d . . . C14A C -0.10758(11) 0.53284(11) 0.38657(12) 0.0394(5) Uani 1 1 d . . . H14A' H -0.1325 0.5671 0.3539 0.047 Uiso 1 1 calc R . . C15A C -0.13307(11) 0.48426(11) 0.43755(12) 0.0393(5) Uani 1 1 d . . . H15A' H -0.1755 0.4851 0.4401 0.047 Uiso 1 1 calc R . . C16A C -0.09614(10) 0.43309(11) 0.48611(11) 0.0366(5) Uani 1 1 d . . . C17A C -0.10700(10) 0.37493(11) 0.54363(11) 0.0368(5) Uani 1 1 d . . . C18A C -0.15866(11) 0.34605(11) 0.57238(12) 0.0374(5) Uani 1 1 d . . . H18A H -0.1970 0.3671 0.5539 0.045 Uiso 1 1 calc R . . C19A C -0.15414(10) 0.28679(11) 0.62778(12) 0.0370(5) Uani 1 1 d . . . C20A C -0.09735(11) 0.25708(11) 0.65490(12) 0.0390(5) Uani 1 1 d . . . H20A H -0.0944 0.2166 0.6927 0.047 Uiso 1 1 calc R . . C21A C 0.27032(10) 0.49800(11) 0.41160(12) 0.0380(5) Uani 1 1 d . . . C22A C 0.27326(10) 0.45009(11) 0.47529(12) 0.0383(5) Uani 1 1 d . . . N23A N 0.22786(10) 0.41747(9) 0.51362(10) 0.0385(5) Uani 1 1 d . . . H23A H 0.1951(13) 0.4176(14) 0.4959(14) 0.057(9) Uiso 1 1 d . . . C24A C 0.25101(11) 0.37499(11) 0.57359(12) 0.0387(5) Uani 1 1 d . . . C25A C 0.22413(10) 0.32884(11) 0.62726(12) 0.0382(5) Uani 1 1 d . . . N26A N 0.16769(9) 0.30975(9) 0.63315(10) 0.0385(5) Uani 1 1 d . . . H26A H 0.1383(14) 0.3290(14) 0.5983(15) 0.069(9) Uiso 1 1 d . . . C27A C 0.16546(11) 0.25578(11) 0.69136(12) 0.0377(5) Uani 1 1 d . . . C28A C 0.11809(11) 0.21705(11) 0.71638(12) 0.0387(5) Uani 1 1 d . . . C29A C 0.12961(11) 0.16095(11) 0.77399(12) 0.0410(6) Uani 1 1 d . . . H29A H 0.0993 0.1331 0.7911 0.049 Uiso 1 1 calc R . . C30A C 0.18376(11) 0.14322(11) 0.80840(12) 0.0407(6) Uani 1 1 d . . . C31A C 0.22787(11) 0.18477(11) 0.78378(12) 0.0409(6) Uani 1 1 d . . . H31A H 0.2641 0.1747 0.8071 0.049 Uiso 1 1 calc R . . C32A C 0.21935(11) 0.24078(11) 0.72546(12) 0.0385(5) Uani 1 1 d . . . C33A C 0.25763(11) 0.28911(11) 0.68391(12) 0.0399(6) Uani 1 1 d . . . C34A C 0.31765(11) 0.29839(12) 0.68726(13) 0.0434(6) Uani 1 1 d . . . H34A H 0.3396 0.2733 0.7263 0.052 Uiso 1 1 calc R . . C35A C 0.34455(11) 0.34338(11) 0.63446(13) 0.0430(6) Uani 1 1 d . . . H35A H 0.3850 0.3492 0.6371 0.052 Uiso 1 1 calc R . . C36A C 0.31191(10) 0.38121(11) 0.57599(12) 0.0391(5) Uani 1 1 d . . . C37A C 0.32659(11) 0.42847(11) 0.51133(13) 0.0408(6) Uani 1 1 d . . . C38A C 0.37989(11) 0.45241(12) 0.48021(13) 0.0454(6) Uani 1 1 d . . . H38A H 0.4164 0.4380 0.5038 0.055 Uiso 1 1 calc R . . C39A C 0.37917(11) 0.49683(12) 0.41539(14) 0.0467(6) Uani 1 1 d . A . C40A C 0.32437(11) 0.52010(12) 0.38229(13) 0.0449(6) Uani 1 1 d . . . H40A H 0.3239 0.5520 0.3384 0.054 Uiso 1 1 calc R . . C41A C 0.01339(11) 0.25648(11) 0.65812(12) 0.0385(5) Uani 1 1 d . . . C42A C 0.06166(11) 0.23670(11) 0.68336(12) 0.0400(6) Uani 1 1 d . . . C43A C 0.21359(12) 0.52385(11) 0.37923(12) 0.0404(6) Uani 1 1 d . . . C44A C 0.16434(11) 0.54786(11) 0.35584(12) 0.0384(5) Uani 1 1 d . . . C45A C -0.21090(11) 0.25382(11) 0.65641(12) 0.0402(6) Uani 1 1 d . . . C46A C -0.26240(11) 0.30498(13) 0.66237(13) 0.0478(6) Uani 1 1 d . . . H46A H -0.2979 0.2833 0.6820 0.072 Uiso 1 1 calc R . . H46B H -0.2724 0.3398 0.6190 0.072 Uiso 1 1 calc R . . H46C H -0.2497 0.3244 0.6899 0.072 Uiso 1 1 calc R . . C47A C -0.20016(12) 0.19715(13) 0.72327(13) 0.0501(6) Uani 1 1 d . . . H47A H -0.2377 0.1789 0.7401 0.075 Uiso 1 1 calc R . . H47B H -0.1865 0.2134 0.7531 0.075 Uiso 1 1 calc R . . H47C H -0.1694 0.1627 0.7197 0.075 Uiso 1 1 calc R . . C48A C -0.22978(12) 0.22633(13) 0.60978(14) 0.0509(7) Uani 1 1 d . . . H48A H -0.1973 0.1933 0.6063 0.076 Uiso 1 1 calc R . . H48B H -0.2378 0.2624 0.5666 0.076 Uiso 1 1 calc R . . H48C H -0.2663 0.2058 0.6268 0.076 Uiso 1 1 calc R . . C49A C 0.03458(12) 0.71215(12) 0.17268(12) 0.0440(6) Uani 1 1 d . . . C50A C 0.08250(13) 0.69608(13) 0.12703(13) 0.0531(7) Uani 1 1 d . . . H50A H 0.1227 0.6961 0.1409 0.080 Uiso 1 1 calc R . . H50B H 0.0758 0.7294 0.0823 0.080 Uiso 1 1 calc R . . H50C H 0.0795 0.6525 0.1289 0.080 Uiso 1 1 calc R . . C51A C 0.04597(13) 0.77613(12) 0.17586(13) 0.0507(7) Uani 1 1 d . . . H51A H 0.0160 0.7872 0.2048 0.076 Uiso 1 1 calc R . . H51B H 0.0428 0.8121 0.1321 0.076 Uiso 1 1 calc R . . H51C H 0.0864 0.7698 0.1927 0.076 Uiso 1 1 calc R . . C52A C -0.02730(13) 0.72473(14) 0.14283(14) 0.0574(7) Uani 1 1 d . . . H52A H -0.0362 0.6840 0.1419 0.086 Uiso 1 1 calc R . . H52B H -0.0274 0.7592 0.0983 0.086 Uiso 1 1 calc R . . H52C H -0.0580 0.7391 0.1691 0.086 Uiso 1 1 calc R . . C53A C 0.43673(12) 0.52365(14) 0.37874(15) 0.0580(8) Uani 1 1 d . . . C54A C 0.4227(3) 0.6039(3) 0.3538(5) 0.066(2) Uani 0.525(6) 1 d P A 2 H54A' H 0.4093 0.6147 0.3908 0.098 Uiso 0.525(6) 1 calc PR A 2 H54B' H 0.3911 0.6217 0.3209 0.098 Uiso 0.525(6) 1 calc PR A 2 H54C' H 0.4594 0.6232 0.3347 0.098 Uiso 0.525(6) 1 calc PR A 2 C55A C 0.4552(4) 0.5059(4) 0.3289(4) 0.068(2) Uani 0.525(6) 1 d P A 2 H55A' H 0.4879 0.5302 0.3045 0.102 Uiso 0.525(6) 1 calc PR A 2 H55B' H 0.4214 0.5162 0.2997 0.102 Uiso 0.525(6) 1 calc PR A 2 H55C' H 0.4696 0.4584 0.3465 0.102 Uiso 0.525(6) 1 calc PR A 2 C56A C 0.4897(2) 0.5100(3) 0.4299(3) 0.070(2) Uani 0.525(6) 1 d P A 2 H56A' H 0.5237 0.5324 0.4063 0.104 Uiso 0.525(6) 1 calc PR A 2 H56B' H 0.5031 0.4624 0.4519 0.104 Uiso 0.525(6) 1 calc PR A 2 H56C' H 0.4741 0.5270 0.4623 0.104 Uiso 0.525(6) 1 calc PR A 2 C74A C 0.4498(4) 0.5751(3) 0.3873(4) 0.0534(18) Uani 0.475(6) 1 d P A 3 H74A H 0.4890 0.5861 0.3670 0.080 Uiso 0.475(6) 1 calc PR A 3 H74B H 0.4514 0.5639 0.4340 0.080 Uiso 0.475(6) 1 calc PR A 3 H74C H 0.4187 0.6131 0.3672 0.080 Uiso 0.475(6) 1 calc PR A 3 C75A C 0.4313(4) 0.5399(5) 0.2996(4) 0.061(2) Uani 0.475(6) 1 d P A 3 H75A H 0.3995 0.5772 0.2796 0.092 Uiso 0.475(6) 1 calc PR A 3 H75B H 0.4215 0.5010 0.2956 0.092 Uiso 0.475(6) 1 calc PR A 3 H75C H 0.4698 0.5511 0.2774 0.092 Uiso 0.475(6) 1 calc PR A 3 C76A C 0.4909(3) 0.4628(3) 0.3983(3) 0.0541(19) Uani 0.475(6) 1 d P A 3 H76A H 0.5261 0.4769 0.3703 0.081 Uiso 0.475(6) 1 calc PR A 3 H76B H 0.4781 0.4261 0.3925 0.081 Uiso 0.475(6) 1 calc PR A 3 H76C H 0.5015 0.4485 0.4440 0.081 Uiso 0.475(6) 1 calc PR A 3 C57A C 0.19292(12) 0.07807(12) 0.86932(13) 0.0460(6) Uani 1 1 d . . . C58A C 0.19557(13) 0.02041(12) 0.84918(14) 0.0550(7) Uani 1 1 d . . . H58A H 0.1579 0.0244 0.8280 0.083 Uiso 1 1 calc R . . H58B H 0.2012 -0.0215 0.8880 0.083 Uiso 1 1 calc R . . H58C H 0.2293 0.0216 0.8188 0.083 Uiso 1 1 calc R . . C59A C 0.25147(13) 0.06915(14) 0.90435(14) 0.0570(7) Uani 1 1 d . . . H59A H 0.2549 0.0276 0.9436 0.086 Uiso 1 1 calc R . . H59B H 0.2511 0.1060 0.9167 0.086 Uiso 1 1 calc R . . H59C H 0.2859 0.0682 0.8752 0.086 Uiso 1 1 calc R . . C60A C 0.14013(13) 0.07471(14) 0.91762(13) 0.0558(7) Uani 1 1 d . . . H60A H 0.1029 0.0748 0.8978 0.084 Uiso 1 1 calc R . . H60B H 0.1360 0.1130 0.9283 0.084 Uiso 1 1 calc R . . H60C H 0.1479 0.0342 0.9575 0.084 Uiso 1 1 calc R . . N30A N 0.12135(9) 0.36443(9) 0.50263(10) 0.0405(5) Uani 1 1 d . . . N31A N 0.11009(9) 0.33135(9) 0.47684(10) 0.0390(5) Uani 1 1 d . . . N32A N 0.09844(10) 0.29873(11) 0.45190(11) 0.0529(6) Uani 1 1 d . . . C1B C 0.49629(11) 0.11639(12) 0.20127(12) 0.0407(6) Uani 1 1 d . . . C2B C 0.50846(11) 0.16968(12) 0.21262(12) 0.0410(6) Uani 1 1 d . . . N3B N 0.53231(9) 0.16769(10) 0.26820(10) 0.0405(5) Uani 1 1 d . . . H3B H 0.5498(13) 0.1256(15) 0.3064(14) 0.064(8) Uiso 1 1 d . . . C4B C 0.53650(11) 0.23203(11) 0.25764(12) 0.0412(6) Uani 1 1 d . . . C5B C 0.56057(11) 0.25508(11) 0.29786(12) 0.0405(6) Uani 1 1 d . . . N6B N 0.58771(9) 0.22089(10) 0.35727(10) 0.0404(5) Uani 1 1 d . . . H6B H 0.5971(14) 0.1771(16) 0.3740(15) 0.071(10) Uiso 1 1 d . . . C7B C 0.61011(11) 0.26507(11) 0.37371(12) 0.0383(5) Uani 1 1 d . . . C8B C 0.64405(11) 0.25236(11) 0.42808(12) 0.0393(5) Uani 1 1 d . . . C9B C 0.66540(11) 0.30608(11) 0.43050(12) 0.0415(6) Uani 1 1 d . . . H9B H 0.6897 0.2985 0.4662 0.050 Uiso 1 1 calc R . . C10B C 0.65258(11) 0.37076(11) 0.38269(12) 0.0411(6) Uani 1 1 d . . . C11B C 0.61639(11) 0.38225(12) 0.33068(12) 0.0416(6) Uani 1 1 d . . . H11B' H 0.6061 0.4259 0.2986 0.050 Uiso 1 1 calc R . . C12B C 0.59506(11) 0.32941(11) 0.32548(12) 0.0402(5) Uani 1 1 d . . . C13B C 0.56148(11) 0.32341(11) 0.27626(12) 0.0420(6) Uani 1 1 d . . . C14B C 0.53679(12) 0.36776(12) 0.21549(13) 0.0472(6) Uani 1 1 d . . . H14B' H 0.5362 0.4139 0.2016 0.057 Uiso 1 1 calc R . . C15B C 0.51345(12) 0.34457(12) 0.17608(13) 0.0467(6) Uani 1 1 d . . . H15B' H 0.4967 0.3748 0.1352 0.056 Uiso 1 1 calc R . . C16B C 0.51426(11) 0.27619(12) 0.19617(13) 0.0432(6) Uani 1 1 d . . . C17B C 0.49746(11) 0.23551(12) 0.16599(12) 0.0427(6) Uani 1 1 d . . . C18B C 0.47689(11) 0.24821(13) 0.10433(13) 0.0453(6) Uani 1 1 d . . . H18B H 0.4693 0.2924 0.0724 0.054 Uiso 1 1 calc R . . C19B C 0.46744(11) 0.19624(12) 0.08958(12) 0.0441(6) Uani 1 1 d . . . C20B C 0.47648(11) 0.13162(12) 0.13862(12) 0.0439(6) Uani 1 1 d . . . H20B H 0.4688 0.0966 0.1288 0.053 Uiso 1 1 calc R . . C21B C 0.65748(11) 0.07149(11) 0.57855(12) 0.0391(5) Uani 1 1 d . . . C22B C 0.63086(10) 0.02248(11) 0.57231(12) 0.0380(5) Uani 1 1 d . . . N23B N 0.60568(9) 0.02414(10) 0.51823(11) 0.0376(5) Uani 1 1 d . . . H23B H 0.6057(10) 0.0551(11) 0.4800(11) 0.027(6) Uiso 1 1 d . . . C24B C 0.58656(10) -0.03580(11) 0.53456(12) 0.0378(5) Uani 1 1 d . . . C25B C 0.55954(10) -0.05852(11) 0.49555(12) 0.0371(5) Uani 1 1 d . . . N26B N 0.54487(9) -0.02797(10) 0.43069(10) 0.0380(5) Uani 1 1 d . . . H26B H 0.5501(11) 0.0110(13) 0.4023(13) 0.045(7) Uiso 1 1 d . . . C27B C 0.52133(10) -0.07189(11) 0.41463(12) 0.0380(5) Uani 1 1 d . . . C28B C 0.50064(11) -0.06268(11) 0.35406(12) 0.0395(5) Uani 1 1 d . . . C29B C 0.48105(11) -0.11726(11) 0.35092(13) 0.0411(6) Uani 1 1 d . . . H29B H 0.4658 -0.1124 0.3109 0.049 Uiso 1 1 calc R . . C30B C 0.48296(10) -0.17871(11) 0.40436(13) 0.0410(6) Uani 1 1 d . . . C31B C 0.50184(11) -0.18526(12) 0.46415(13) 0.0413(6) Uani 1 1 d . . . H31B H 0.5020 -0.2262 0.5012 0.050 Uiso 1 1 calc R . . C32B C 0.52065(10) -0.13164(11) 0.46997(12) 0.0391(5) Uani 1 1 d . . . C33B C 0.54458(10) -0.12295(11) 0.52325(12) 0.0389(5) Uani 1 1 d . . . C34B C 0.55462(11) -0.16355(11) 0.58981(13) 0.0421(6) Uani 1 1 d . . . H34B H 0.5432 -0.2065 0.6084 0.051 Uiso 1 1 calc R . . C35B C 0.58099(10) -0.14106(11) 0.62807(12) 0.0400(5) Uani 1 1 d . . . H35B H 0.5883 -0.1686 0.6728 0.048 Uiso 1 1 calc R . . C36B C 0.59712(10) -0.07666(11) 0.60019(12) 0.0379(5) Uani 1 1 d . . . C37B C 0.62623(10) -0.03872(11) 0.62520(12) 0.0373(5) Uani 1 1 d . . . C38B C 0.64905(10) -0.05101(11) 0.68573(12) 0.0388(5) Uani 1 1 d . . . H38B H 0.6459 -0.0920 0.7217 0.047 Uiso 1 1 calc R . . C39B C 0.67640(11) -0.00358(11) 0.69375(12) 0.0392(5) Uani 1 1 d . . . C40B C 0.68042(11) 0.05670(11) 0.63990(12) 0.0397(5) Uani 1 1 d . . . H40B H 0.6994 0.0888 0.6452 0.048 Uiso 1 1 calc R . . C41B C 0.50139(11) 0.05160(12) 0.25221(12) 0.0398(6) Uani 1 1 d . . . C42B C 0.50114(11) -0.00099(12) 0.29845(13) 0.0406(6) Uani 1 1 d . . . C43B C 0.65803(11) 0.13451(12) 0.52445(12) 0.0393(5) Uani 1 1 d . . . C44B C 0.65428(11) 0.18734(12) 0.47940(12) 0.0392(5) Uani 1 1 d . . . C45B C 0.44864(12) 0.20781(13) 0.02141(13) 0.0478(6) Uani 1 1 d . . . C46B C 0.42205(18) 0.27883(16) -0.01756(16) 0.0769(10) Uani 1 1 d . . . H46D H 0.3877 0.2912 0.0064 0.115 Uiso 1 1 calc R . . H46E H 0.4085 0.2838 -0.0598 0.115 Uiso 1 1 calc R . . H46F H 0.4527 0.3075 -0.0246 0.115 Uiso 1 1 calc R . . C47B C 0.40069(15) 0.16481(18) 0.02579(16) 0.0762(10) Uani 1 1 d . . . H47D H 0.3658 0.1746 0.0506 0.114 Uiso 1 1 calc R . . H47E H 0.4175 0.1181 0.0478 0.114 Uiso 1 1 calc R . . H47F H 0.3882 0.1743 -0.0182 0.114 Uiso 1 1 calc R . . C48B C 0.50320(14) 0.19008(18) -0.01533(16) 0.0709(9) Uani 1 1 d . . . H48D H 0.4913 0.1986 -0.0593 0.106 Uiso 1 1 calc R . . H48E H 0.5190 0.1433 0.0080 0.106 Uiso 1 1 calc R . . H48F H 0.5344 0.2170 -0.0183 0.106 Uiso 1 1 calc R . . C49B C 0.68217(12) 0.42485(12) 0.38856(13) 0.0454(6) Uani 1 1 d . . . C50B C 0.66258(15) 0.49286(13) 0.33542(15) 0.0615(8) Uani 1 1 d . . . H50D H 0.6738 0.4927 0.2927 0.092 Uiso 1 1 calc R . . H50E H 0.6825 0.5255 0.3414 0.092 Uiso 1 1 calc R . . H50F H 0.6188 0.5042 0.3379 0.092 Uiso 1 1 calc R . . C51B C 0.75023(13) 0.40848(15) 0.38244(16) 0.0602(8) Uani 1 1 d . . . H51D H 0.7642 0.3653 0.4171 0.090 Uiso 1 1 calc R . . H51E H 0.7700 0.4422 0.3864 0.090 Uiso 1 1 calc R . . H51F H 0.7602 0.4074 0.3399 0.090 Uiso 1 1 calc R . . C52B C 0.66645(14) 0.42667(13) 0.45523(14) 0.0565(7) Uani 1 1 d . . . H52D H 0.6226 0.4355 0.4598 0.085 Uiso 1 1 calc R . . H52E H 0.6850 0.4616 0.4585 0.085 Uiso 1 1 calc R . . H52F H 0.6817 0.3840 0.4899 0.085 Uiso 1 1 calc R . . C53B C 0.70189(12) -0.01823(12) 0.76017(12) 0.0448(6) Uani 1 1 d . . . C54B C 0.71879(14) 0.04272(13) 0.76412(14) 0.0578(7) Uani 1 1 d . . . H54A H 0.7523 0.0582 0.7339 0.087 Uiso 1 1 calc R . . H54B H 0.7310 0.0316 0.8087 0.087 Uiso 1 1 calc R . . H54C H 0.6840 0.0776 0.7524 0.087 Uiso 1 1 calc R . . C55B C 0.75884(15) -0.06990(14) 0.77281(16) 0.0663(8) Uani 1 1 d . . . H55A H 0.7490 -0.1093 0.7697 0.099 Uiso 1 1 calc R . . H55B H 0.7739 -0.0820 0.8165 0.099 Uiso 1 1 calc R . . H55C H 0.7899 -0.0513 0.7402 0.099 Uiso 1 1 calc R . . C56B C 0.65589(15) -0.04605(17) 0.81468(15) 0.0693(9) Uani 1 1 d . . . H56A H 0.6186 -0.0147 0.8059 0.104 Uiso 1 1 calc R . . H56B H 0.6723 -0.0533 0.8564 0.104 Uiso 1 1 calc R . . H56C H 0.6473 -0.0880 0.8166 0.104 Uiso 1 1 calc R . . C57B C 0.46629(11) -0.23723(12) 0.39405(13) 0.0447(6) Uani 1 1 d . . . C58B C 0.50431(13) -0.24342(13) 0.33620(15) 0.0563(7) Uani 1 1 d . . . H58D H 0.5471 -0.2469 0.3444 0.084 Uiso 1 1 calc R . . H58E H 0.4928 -0.2043 0.2960 0.084 Uiso 1 1 calc R . . H58F H 0.4970 -0.2829 0.3316 0.084 Uiso 1 1 calc R . . C59B C 0.47976(14) -0.30211(12) 0.45434(15) 0.0574(7) Uani 1 1 d . . . H59D H 0.4542 -0.3002 0.4908 0.086 Uiso 1 1 calc R . . H59E H 0.5222 -0.3091 0.4659 0.086 Uiso 1 1 calc R . . H59F H 0.4715 -0.3387 0.4450 0.086 Uiso 1 1 calc R . . C60B C 0.39945(11) -0.22557(13) 0.37769(14) 0.0478(6) Uani 1 1 d . . . H60D H 0.3899 -0.2624 0.3696 0.072 Uiso 1 1 calc R . . H60E H 0.3907 -0.1844 0.3387 0.072 Uiso 1 1 calc R . . H60F H 0.3749 -0.2225 0.4144 0.072 Uiso 1 1 calc R . . N30B N 0.61367(9) 0.08419(10) 0.37458(10) 0.0424(5) Uani 1 1 d . . . N31B N 0.65849(10) 0.04613(10) 0.37862(10) 0.0404(5) Uani 1 1 d . . . N32B N 0.70231(10) 0.00863(10) 0.38288(12) 0.0522(6) Uani 1 1 d . . . C1C C 0.74309(11) 0.43155(11) 0.00668(11) 0.0380(5) Uani 1 1 d . . . C2C C 0.77529(11) 0.36938(11) 0.01567(11) 0.0379(5) Uani 1 1 d . . . N3C N 0.83244(9) 0.34287(9) 0.03854(10) 0.0362(4) Uani 1 1 d . . . H3C H 0.8529(10) 0.3601(11) 0.0568(11) 0.035(6) Uiso 1 1 d . . . C4C C 0.84583(11) 0.28136(11) 0.03768(11) 0.0368(5) Uani 1 1 d . . . C5C C 0.89777(11) 0.23557(11) 0.05546(11) 0.0368(5) Uani 1 1 d . . . N6C N 0.95175(9) 0.23846(9) 0.07871(10) 0.0383(5) Uani 1 1 d . . . H6C H 0.9593(11) 0.2695(13) 0.0905(12) 0.046(7) Uiso 1 1 d . . . C7C C 0.98861(11) 0.18003(11) 0.09112(11) 0.0371(5) Uani 1 1 d . . . C8C C 1.04638(11) 0.15958(11) 0.11805(12) 0.0396(5) Uani 1 1 d . . . C9C C 1.07367(11) 0.09597(11) 0.12688(12) 0.0407(6) Uani 1 1 d . . . H9C H 1.1127 0.0805 0.1453 0.049 Uiso 1 1 calc R . . C10C C 1.04565(11) 0.05412(11) 0.10966(12) 0.0403(6) Uani 1 1 d . . . C11C C 0.98859(11) 0.07672(11) 0.08222(12) 0.0397(5) Uani 1 1 d . . . H11C' H 0.9693 0.0493 0.0698 0.048 Uiso 1 1 calc R . . C12C C 0.95981(10) 0.13951(11) 0.07293(11) 0.0370(5) Uani 1 1 d . . . C13C C 0.90087(11) 0.17534(11) 0.04963(11) 0.0373(5) Uani 1 1 d . . . C14C C 0.85090(11) 0.16188(11) 0.02518(12) 0.0407(6) Uani 1 1 d . . . H14C' H 0.8530 0.1214 0.0210 0.049 Uiso 1 1 calc R . . C15C C 0.79961(11) 0.20685(11) 0.00754(12) 0.0407(6) Uani 1 1 d . . . H15C' H 0.7664 0.1977 -0.0090 0.049 Uiso 1 1 calc R . . C16C C 0.79612(11) 0.26745(11) 0.01405(11) 0.0376(5) Uani 1 1 d . . . C17C C 0.75034(11) 0.32433(11) 0.00011(12) 0.0397(5) Uani 1 1 d . . . C18C C 0.69174(11) 0.34069(12) -0.02388(12) 0.0439(6) Uani 1 1 d . . . H18C H 0.6746 0.3102 -0.0339 0.053 Uiso 1 1 calc R . . C19C C 0.65837(11) 0.40160(12) -0.03311(13) 0.0453(6) Uani 1 1 d . . . C20C C 0.68501(11) 0.44553(12) -0.01763(12) 0.0421(6) Uani 1 1 d . . . H20C H 0.6622 0.4870 -0.0241 0.051 Uiso 1 1 calc R . . C21C C 1.13165(11) 0.29286(11) 0.14310(11) 0.0375(5) Uani 1 1 d . . . C22C C 1.10255(11) 0.35787(11) 0.12309(11) 0.0360(5) Uani 1 1 d . . . N23C N 1.04324(9) 0.38216(9) 0.10706(9) 0.0369(4) Uani 1 1 d . . . H23C H 1.0102(13) 0.3612(14) 0.1110(13) 0.060(8) Uiso 1 1 d . . . C24C C 1.03508(11) 0.44947(11) 0.09015(11) 0.0363(5) Uani 1 1 d . . . C25C C 0.98271(10) 0.49538(11) 0.07279(11) 0.0357(5) Uani 1 1 d . . . N26C N 0.92466(9) 0.48707(10) 0.06561(10) 0.0371(4) Uani 1 1 d . . . H26C H 0.9146(13) 0.4475(15) 0.0739(14) 0.062(9) Uiso 1 1 d . . . C27C C 0.88848(11) 0.54707(11) 0.04974(11) 0.0363(5) Uani 1 1 d . . . C28C C 0.82653(11) 0.56292(11) 0.03741(11) 0.0384(5) Uani 1 1 d . . . C29C C 0.79992(11) 0.62681(11) 0.02814(12) 0.0402(5) Uani 1 1 d . . . H29C H 0.7579 0.6388 0.0204 0.048 Uiso 1 1 calc R . . C30C C 0.83307(11) 0.67397(11) 0.02988(12) 0.0403(6) Uani 1 1 d . . . C31C C 0.89494(11) 0.65803(11) 0.03711(11) 0.0398(6) Uani 1 1 d . . . H31C H 0.9183 0.6903 0.0353 0.048 Uiso 1 1 calc R . . C32C C 0.92324(11) 0.59452(11) 0.04711(11) 0.0387(5) Uani 1 1 d . . . C33C C 0.98511(11) 0.56139(11) 0.06031(11) 0.0369(5) Uani 1 1 d . . . C34C C 1.04068(11) 0.58190(11) 0.06211(11) 0.0388(5) Uani 1 1 d . . . H34C H 1.0424 0.6270 0.0518 0.047 Uiso 1 1 calc R . . C35C C 1.09257(11) 0.53665(11) 0.07878(11) 0.0391(5) Uani 1 1 d . . . H35C H 1.1300 0.5506 0.0797 0.047 Uiso 1 1 calc R . . C36C C 1.08995(10) 0.46960(11) 0.09445(11) 0.0359(5) Uani 1 1 d . . . C37C C 1.13387(11) 0.40996(11) 0.11661(11) 0.0369(5) Uani 1 1 d . . . C38C C 1.19460(11) 0.39626(11) 0.13229(11) 0.0378(5) Uani 1 1 d . . . H38C H 1.2158 0.4310 0.1280 0.045 Uiso 1 1 calc R . . C39C C 1.22473(11) 0.33144(11) 0.15431(11) 0.0381(5) Uani 1 1 d . . . C40C C 1.19220(11) 0.28120(11) 0.15974(11) 0.0381(5) Uani 1 1 d . . . H40C H 1.2124 0.2372 0.1755 0.046 Uiso 1 1 calc R . . C41C C 0.76975(10) 0.47703(11) 0.02148(11) 0.0381(5) Uani 1 1 d . . . C42C C 0.79365(10) 0.51593(11) 0.03143(11) 0.0380(5) Uani 1 1 d . . . C43C C 1.10086(11) 0.24279(11) 0.14094(11) 0.0385(5) Uani 1 1 d . . . C44C C 1.07597(11) 0.20327(11) 0.13328(12) 0.0397(5) Uani 1 1 d . . . C45C C 0.59366(12) 0.42123(13) -0.05833(16) 0.0580(8) Uani 1 1 d . . . C46C C 0.5877(2) 0.48849(18) -0.1160(3) 0.146(3) Uani 1 1 d . . . H46G H 0.5471 0.4994 -0.1339 0.219 Uiso 1 1 calc R . . H46H H 0.6174 0.4873 -0.1497 0.219 Uiso 1 1 calc R . . H46I H 0.5948 0.5220 -0.1016 0.219 Uiso 1 1 calc R . . C47C C 0.57535(14) 0.37378(16) -0.0832(2) 0.0762(10) Uani 1 1 d . . . H47G H 0.5768 0.3298 -0.0473 0.114 Uiso 1 1 calc R . . H47H H 0.6031 0.3716 -0.1180 0.114 Uiso 1 1 calc R . . H47I H 0.5343 0.3894 -0.1001 0.114 Uiso 1 1 calc R . . C48C C 0.55110(16) 0.4230(3) -0.0034(3) 0.148(3) Uani 1 1 d . . . H48G H 0.5095 0.4350 -0.0188 0.221 Uiso 1 1 calc R . . H48H H 0.5608 0.4557 0.0109 0.221 Uiso 1 1 calc R . . H48I H 0.5555 0.3793 0.0333 0.221 Uiso 1 1 calc R . . C49C C 1.07550(11) -0.01693(11) 0.12433(13) 0.0433(6) Uani 1 1 d . . . C50C C 1.05241(16) -0.06264(13) 0.19077(14) 0.0642(8) Uani 1 1 d . . . H50G H 1.0083 -0.0568 0.1907 0.096 Uiso 1 1 calc R . . H50H H 1.0659 -0.0518 0.2247 0.096 Uiso 1 1 calc R . . H50I H 1.0683 -0.1086 0.1994 0.096 Uiso 1 1 calc R . . C51C C 1.14443(13) -0.02342(14) 0.12578(19) 0.0690(9) Uani 1 1 d . . . H51G H 1.1621 -0.0679 0.1310 0.104 Uiso 1 1 calc R . . H51H H 1.1562 -0.0155 0.1624 0.104 Uiso 1 1 calc R . . H51I H 1.1590 0.0091 0.0849 0.104 Uiso 1 1 calc R . . C52C C 1.05934(12) -0.03920(12) 0.07358(13) 0.0466(6) Uani 1 1 d . . . H52G H 1.0165 -0.0440 0.0778 0.070 Uiso 1 1 calc R . . H52H H 1.0835 -0.0817 0.0804 0.070 Uiso 1 1 calc R . . H52I H 1.0676 -0.0063 0.0299 0.070 Uiso 1 1 calc R . . C53C C 1.29221(11) 0.31768(12) 0.16941(12) 0.0415(6) Uani 1 1 d . . . C54C C 1.30337(14) 0.33784(17) 0.22388(17) 0.0705(9) Uani 1 1 d . . . H54D H 1.2893 0.3851 0.2102 0.106 Uiso 1 1 calc R . . H54E H 1.3466 0.3289 0.2330 0.106 Uiso 1 1 calc R . . H54F H 1.2814 0.3125 0.2633 0.106 Uiso 1 1 calc R . . C55C C 1.31871(12) 0.24486(12) 0.19085(14) 0.0507(6) Uani 1 1 d . . . H55D H 1.2984 0.2180 0.2309 0.076 Uiso 1 1 calc R . . H55E H 1.3619 0.2392 0.1989 0.076 Uiso 1 1 calc R . . H55F H 1.3128 0.2308 0.1565 0.076 Uiso 1 1 calc R . . C56C C 1.32707(13) 0.35739(13) 0.10800(15) 0.0587(7) Uani 1 1 d . . . H56D H 1.3206 0.3443 0.0731 0.088 Uiso 1 1 calc R . . H56E H 1.3701 0.3486 0.1176 0.088 Uiso 1 1 calc R . . H56F H 1.3128 0.4046 0.0941 0.088 Uiso 1 1 calc R . . C57C C 0.79909(12) 0.74138(11) 0.02402(12) 0.0434(6) Uani 1 1 d . . . C58C C 0.76709(12) 0.77791(12) -0.04176(13) 0.0497(6) Uani 1 1 d . . . H58G H 0.7403 0.7501 -0.0465 0.075 Uiso 1 1 calc R . . H58H H 0.7971 0.7879 -0.0771 0.075 Uiso 1 1 calc R . . H58I H 0.7435 0.8191 -0.0436 0.075 Uiso 1 1 calc R . . C59C C 0.75233(12) 0.73011(13) 0.07939(14) 0.0517(7) Uani 1 1 d . . . H59G H 0.7728 0.7079 0.1214 0.078 Uiso 1 1 calc R . . H59H H 0.7241 0.7025 0.0766 0.078 Uiso 1 1 calc R . . H59I H 0.7302 0.7727 0.0755 0.078 Uiso 1 1 calc R . . C60C C 0.84141(12) 0.78537(12) 0.02911(15) 0.0534(7) Uani 1 1 d . . . H60G H 0.8184 0.8279 0.0242 0.080 Uiso 1 1 calc R . . H60H H 0.8722 0.7925 -0.0054 0.080 Uiso 1 1 calc R . . H60I H 0.8608 0.7640 0.0718 0.080 Uiso 1 1 calc R . . N30C N 0.92412(9) 0.34383(9) 0.12336(10) 0.0412(5) Uani 1 1 d . . . N31C N 0.90881(9) 0.30816(10) 0.17659(11) 0.0383(5) Uani 1 1 d . . . N32C N 0.89417(10) 0.27233(12) 0.22883(12) 0.0538(6) Uani 1 1 d . . . N1X N 0.26363(9) 0.19020(9) 0.51863(10) 0.0436(5) Uani 1 1 d . . . C1X C 0.27122(13) 0.26232(12) 0.47984(14) 0.0505(7) Uani 1 1 d . . . H1X1 H 0.2678 0.2841 0.5101 0.061 Uiso 1 1 calc R . . H1X2 H 0.2378 0.2839 0.4484 0.061 Uiso 1 1 calc R . . C2X C 0.33078(13) 0.27338(12) 0.44247(14) 0.0536(7) Uani 1 1 d . . . H2X1 H 0.3636 0.2617 0.4738 0.064 Uiso 1 1 calc R . . H2X2 H 0.3390 0.2437 0.4198 0.064 Uiso 1 1 calc R . . C3X C 0.33090(15) 0.34387(13) 0.39299(15) 0.0609(8) Uani 1 1 d . . . H3X1 H 0.2973 0.3560 0.3624 0.073 Uiso 1 1 calc R . . H3X2 H 0.3239 0.3735 0.4158 0.073 Uiso 1 1 calc R . . C4X C 0.38911(15) 0.35435(14) 0.35471(15) 0.0669(8) Uani 1 1 d . . . H4X1 H 0.4224 0.3441 0.3845 0.100 Uiso 1 1 calc R . . H4X2 H 0.3866 0.4004 0.3229 0.100 Uiso 1 1 calc R . . H4X3 H 0.3962 0.3253 0.3319 0.100 Uiso 1 1 calc R . . C5X C 0.20084(12) 0.18831(13) 0.54999(13) 0.0495(6) Uani 1 1 d . . . H5X1 H 0.1952 0.2191 0.5714 0.059 Uiso 1 1 calc R . . H5X2 H 0.1707 0.2050 0.5149 0.059 Uiso 1 1 calc R . . C6X C 0.18764(13) 0.12220(15) 0.59910(15) 0.0633(8) Uani 1 1 d . . . H6X1 H 0.2061 0.1122 0.6412 0.076 Uiso 1 1 calc R . . H6X2 H 0.2057 0.0878 0.5841 0.076 Uiso 1 1 calc R . . C7X C 0.11946(13) 0.12071(15) 0.60904(15) 0.0604(8) Uani 1 1 d . . . H7X1 H 0.1120 0.0823 0.6498 0.073 Uiso 1 1 calc R . . H7X2 H 0.1002 0.1612 0.6138 0.073 Uiso 1 1 calc R . . C8X C 0.09073(18) 0.11620(19) 0.5521(2) 0.0908(11) Uani 1 1 d . . . H8X1 H 0.0993 0.1532 0.5114 0.136 Uiso 1 1 calc R . . H8X2 H 0.0471 0.1180 0.5591 0.136 Uiso 1 1 calc R . . H8X3 H 0.1075 0.0745 0.5493 0.136 Uiso 1 1 calc R . . C9X C 0.26943(12) 0.15399(12) 0.47415(12) 0.0441(6) Uani 1 1 d . . . H9X1 H 0.3120 0.1498 0.4597 0.053 Uiso 1 1 calc R . . H9X2 H 0.2596 0.1088 0.5000 0.053 Uiso 1 1 calc R . . C10X C 0.22980(12) 0.18633(13) 0.41405(13) 0.0492(6) Uani 1 1 d . . . H10A H 0.2403 0.2309 0.3866 0.059 Uiso 1 1 calc R . . H10B H 0.1871 0.1913 0.4277 0.059 Uiso 1 1 calc R . . C11X C 0.23825(12) 0.14493(12) 0.37442(13) 0.0479(6) Uani 1 1 d . . . H11A H 0.2149 0.1692 0.3338 0.057 Uiso 1 1 calc R . . H11B H 0.2813 0.1396 0.3619 0.057 Uiso 1 1 calc R . . C12X C 0.21894(13) 0.07703(14) 0.41002(15) 0.0567(7) Uani 1 1 d . . . H12A H 0.2451 0.0506 0.4475 0.085 Uiso 1 1 calc R . . H12B H 0.2221 0.0551 0.3803 0.085 Uiso 1 1 calc R . . H12C H 0.1772 0.0816 0.4252 0.085 Uiso 1 1 calc R . . C13X C 0.31194(12) 0.15501(12) 0.56975(12) 0.0442(6) Uani 1 1 d . . . H13A H 0.3518 0.1567 0.5476 0.053 Uiso 1 1 calc R . . H13B H 0.3063 0.1080 0.5929 0.053 Uiso 1 1 calc R . . C14X C 0.31207(13) 0.18377(13) 0.61978(13) 0.0506(7) Uani 1 1 d . . . H14A H 0.3227 0.2290 0.5979 0.061 Uiso 1 1 calc R . . H14B H 0.2712 0.1866 0.6389 0.061 Uiso 1 1 calc R . . C15X C 0.35673(12) 0.14166(13) 0.67377(13) 0.0491(6) Uani 1 1 d . . . H15A H 0.3969 0.1367 0.6538 0.059 Uiso 1 1 calc R . . H15B H 0.3596 0.1653 0.7015 0.059 Uiso 1 1 calc R . . C16X C 0.34111(14) 0.07377(14) 0.71667(15) 0.0615(8) Uani 1 1 d . . . H16A H 0.3016 0.0779 0.7372 0.092 Uiso 1 1 calc R . . H16B H 0.3716 0.0503 0.7505 0.092 Uiso 1 1 calc R . . H16C H 0.3400 0.0490 0.6902 0.092 Uiso 1 1 calc R . . N1Y N 0.76138(10) 0.17122(10) 0.24140(10) 0.0460(5) Uani 1 1 d . . . C1Y C 0.70989(12) 0.14314(13) 0.22724(13) 0.0491(6) Uani 1 1 d . . . H1Y1 H 0.6716 0.1633 0.2402 0.059 Uiso 1 1 calc R . . H1Y2 H 0.7145 0.0952 0.2551 0.059 Uiso 1 1 calc R . . C2Y C 0.70484(13) 0.15345(14) 0.15670(14) 0.0545(7) Uani 1 1 d . . . H2Y1 H 0.6969 0.2013 0.1285 0.065 Uiso 1 1 calc R . . H2Y2 H 0.7433 0.1352 0.1423 0.065 Uiso 1 1 calc R . . C3Y C 0.65428(14) 0.11962(16) 0.15008(15) 0.0640(8) Uani 1 1 d . . . H3Y1 H 0.6613 0.0724 0.1806 0.077 Uiso 1 1 calc R . . H3Y2 H 0.6157 0.1396 0.1627 0.077 Uiso 1 1 calc R . . C4Y C 0.64904(16) 0.12483(18) 0.08198(17) 0.0757(9) Uani 1 1 d . . . H4Y1 H 0.6398 0.1714 0.0518 0.114 Uiso 1 1 calc R . . H4Y2 H 0.6168 0.1009 0.0809 0.114 Uiso 1 1 calc R . . H4Y3 H 0.6872 0.1056 0.0689 0.114 Uiso 1 1 calc R . . C5Y C 0.75880(12) 0.15304(13) 0.31408(12) 0.0473(6) Uani 1 1 d . . . H5Y1 H 0.7586 0.1048 0.3372 0.057 Uiso 1 1 calc R . . H5Y2 H 0.7202 0.1750 0.3244 0.057 Uiso 1 1 calc R . . C6Y C 0.80997(13) 0.17123(15) 0.34070(13) 0.0568(7) Uani 1 1 d . . . H6Y1 H 0.8488 0.1479 0.3327 0.068 Uiso 1 1 calc R . . H6Y2 H 0.8112 0.2193 0.3175 0.068 Uiso 1 1 calc R . . C7Y C 0.80163(14) 0.15272(14) 0.41358(13) 0.0546(7) Uani 1 1 d . . . H7Y1 H 0.8356 0.1654 0.4288 0.066 Uiso 1 1 calc R . . H7Y2 H 0.7643 0.1792 0.4203 0.066 Uiso 1 1 calc R . . C8Y C 0.79787(18) 0.08095(16) 0.45576(16) 0.0799(10) Uani 1 1 d . . . H8Y1 H 0.7600 0.0697 0.4474 0.120 Uiso 1 1 calc R . . H8Y2 H 0.7993 0.0729 0.5018 0.120 Uiso 1 1 calc R . . H8Y3 H 0.8319 0.0536 0.4456 0.120 Uiso 1 1 calc R . . C9Y C 0.82154(12) 0.14262(13) 0.22177(13) 0.0481(6) Uani 1 1 d . . . H9Y1 H 0.8215 0.1557 0.1741 0.058 Uiso 1 1 calc R . . H9Y2 H 0.8536 0.1630 0.2307 0.058 Uiso 1 1 calc R . . C10Y C 0.83774(12) 0.06819(12) 0.25525(14) 0.0503(6) Uani 1 1 d . . . H10C H 0.8361 0.0538 0.3031 0.060 Uiso 1 1 calc R . . H10D H 0.8082 0.0469 0.2436 0.060 Uiso 1 1 calc R . . C11Y C 0.90048(13) 0.04709(14) 0.23476(14) 0.0578(7) Uani 1 1 d . . . H11C H 0.9034 0.0673 0.1866 0.069 Uiso 1 1 calc R . . H11D H 0.9068 -0.0014 0.2495 0.069 Uiso 1 1 calc R . . C12Y C 0.95038(14) 0.06634(17) 0.26197(18) 0.0739(9) Uani 1 1 d . . . H12D H 0.9464 0.1145 0.2449 0.111 Uiso 1 1 calc R . . H12E H 0.9896 0.0492 0.2489 0.111 Uiso 1 1 calc R . . H12F H 0.9472 0.0476 0.3096 0.111 Uiso 1 1 calc R . . C13Y C 0.75591(12) 0.24526(12) 0.20259(13) 0.0477(6) Uani 1 1 d . . . H13C H 0.7594 0.2546 0.1557 0.057 Uiso 1 1 calc R . . H13D H 0.7903 0.2611 0.2135 0.057 Uiso 1 1 calc R . . C14Y C 0.69780(13) 0.28493(13) 0.21352(14) 0.0537(7) Uani 1 1 d . . . H14C H 0.6634 0.2745 0.1967 0.064 Uiso 1 1 calc R . . H14D H 0.6912 0.2722 0.2608 0.064 Uiso 1 1 calc R . . C15Y C 0.70042(14) 0.35868(13) 0.17946(14) 0.0563(7) Uani 1 1 d . . . H15C H 0.7101 0.3703 0.1328 0.068 Uiso 1 1 calc R . . H15D H 0.6601 0.3826 0.1822 0.068 Uiso 1 1 calc R . . C16Y C 0.74614(15) 0.38216(17) 0.2073(2) 0.0798(10) Uani 1 1 d . . . H16D H 0.7366 0.3716 0.2534 0.120 Uiso 1 1 calc R . . H16E H 0.7449 0.4300 0.1833 0.120 Uiso 1 1 calc R . . H16F H 0.7865 0.3601 0.2034 0.120 Uiso 1 1 calc R . . N1Z N 0.98058(9) 0.36561(10) 0.30929(10) 0.0443(5) Uani 1 1 d . . . C1Z C 0.93353(12) 0.40896(13) 0.25848(12) 0.0466(6) Uani 1 1 d . . . H1Z1 H 0.9534 0.4242 0.2150 0.056 Uiso 1 1 calc R . . H1Z2 H 0.9033 0.3816 0.2586 0.056 Uiso 1 1 calc R . . C2Z C 0.90084(12) 0.46902(13) 0.26751(13) 0.0487(6) Uani 1 1 d . . . H2Z1 H 0.8829 0.4550 0.3118 0.058 Uiso 1 1 calc R . . H2Z2 H 0.9299 0.4993 0.2630 0.058 Uiso 1 1 calc R . . C3Z C 0.85208(13) 0.50455(14) 0.21767(14) 0.0567(7) Uani 1 1 d . . . H3Z1 H 0.8234 0.4737 0.2225 0.068 Uiso 1 1 calc R . . H3Z2 H 0.8705 0.5175 0.1736 0.068 Uiso 1 1 calc R . . C4Z C 0.81741(14) 0.56581(14) 0.22302(16) 0.0635(8) Uani 1 1 d . . . H4Z1 H 0.7971 0.5532 0.2656 0.095 Uiso 1 1 calc R . . H4Z2 H 0.7874 0.5871 0.1885 0.095 Uiso 1 1 calc R . . H4Z3 H 0.8454 0.5966 0.2184 0.095 Uiso 1 1 calc R . . C5Z C 1.00645(12) 0.30876(12) 0.29078(13) 0.0460(6) Uani 1 1 d . . . H5Z1 H 0.9733 0.2845 0.2914 0.055 Uiso 1 1 calc R . . H5Z2 H 1.0221 0.3275 0.2455 0.055 Uiso 1 1 calc R . . C6Z C 1.05611(13) 0.25998(14) 0.33389(15) 0.0599(8) Uani 1 1 d . . . H6Z1 H 1.0434 0.2461 0.3801 0.072 Uiso 1 1 calc R . . H6Z2 H 1.0926 0.2815 0.3273 0.072 Uiso 1 1 calc R . . C7Z C 1.07107(13) 0.19919(13) 0.31868(14) 0.0542(7) Uani 1 1 d . . . H7Z1 H 1.0777 0.2136 0.2711 0.065 Uiso 1 1 calc R . . H7Z2 H 1.1089 0.1729 0.3407 0.065 Uiso 1 1 calc R . . C8Z C 1.02153(18) 0.15645(18) 0.3406(3) 0.1196(18) Uani 1 1 d . . . H8Z1 H 1.0170 0.1392 0.3881 0.179 Uiso 1 1 calc R . . H8Z2 H 1.0318 0.1196 0.3276 0.179 Uiso 1 1 calc R . . H8Z3 H 0.9836 0.1828 0.3201 0.179 Uiso 1 1 calc R . . C9Z C 0.95313(11) 0.33944(13) 0.37751(12) 0.0453(6) Uani 1 1 d . . . H9Z1 H 0.9374 0.3774 0.3881 0.054 Uiso 1 1 calc R . . H9Z2 H 0.9856 0.3122 0.4087 0.054 Uiso 1 1 calc R . . C10Z C 0.90229(12) 0.29805(14) 0.38823(14) 0.0527(7) Uani 1 1 d . . . H10E H 0.8674 0.3259 0.3610 0.063 Uiso 1 1 calc R . . H10F H 0.9163 0.2615 0.3749 0.063 Uiso 1 1 calc R . . C11Z C 0.88319(13) 0.27004(15) 0.45953(14) 0.0586(8) Uani 1 1 d . . . H11E H 0.8738 0.3066 0.4736 0.070 Uiso 1 1 calc R . . H11F H 0.8458 0.2505 0.4640 0.070 Uiso 1 1 calc R . . C12Z C 0.93009(16) 0.21829(17) 0.50411(16) 0.0722(9) Uani 1 1 d . . . H12G H 0.9401 0.1822 0.4902 0.108 Uiso 1 1 calc R . . H12H H 0.9143 0.2011 0.5489 0.108 Uiso 1 1 calc R . . H12I H 0.9664 0.2379 0.5022 0.108 Uiso 1 1 calc R . . C13Z C 1.02961(11) 0.40383(13) 0.31096(13) 0.0451(6) Uani 1 1 d . . . H13E H 1.0111 0.4397 0.3238 0.054 Uiso 1 1 calc R . . H13F H 1.0587 0.3738 0.3451 0.054 Uiso 1 1 calc R . . C14Z C 1.06372(12) 0.43386(13) 0.24728(13) 0.0494(6) Uani 1 1 d . . . H14E H 1.0360 0.4685 0.2144 0.059 Uiso 1 1 calc R . . H14F H 1.0783 0.3993 0.2313 0.059 Uiso 1 1 calc R . . C15Z C 1.11706(12) 0.46390(14) 0.25437(14) 0.0515(7) Uani 1 1 d . . . H15E H 1.1351 0.4864 0.2107 0.062 Uiso 1 1 calc R . . H15F H 1.1023 0.4978 0.2711 0.062 Uiso 1 1 calc R . . C16Z C 1.16550(14) 0.41478(17) 0.29911(16) 0.0692(9) Uani 1 1 d . . . H16G H 1.1492 0.3953 0.3435 0.104 Uiso 1 1 calc R . . H16H H 1.1994 0.4373 0.2987 0.104 Uiso 1 1 calc R . . H16I H 1.1793 0.3799 0.2841 0.104 Uiso 1 1 calc R . . O1S O 0.60277(16) 0.59811(13) 0.17072(16) 0.0752(10) Uani 0.789(4) 1 d PD B 1 C1S C 0.6265(2) 0.53670(18) 0.0987(3) 0.0752(14) Uani 0.789(4) 1 d PD B 1 C2S C 0.6494(2) 0.5795(3) 0.1446(3) 0.093(2) Uani 0.789(4) 1 d PD B 1 C3S C 0.6165(3) 0.6427(2) 0.1963(2) 0.0873(15) Uani 0.789(4) 1 d PD B 1 C4S C 0.5640(3) 0.6678(3) 0.2196(3) 0.0918(16) Uani 0.789(4) 1 d PD B 1 O12S O 0.5644(12) 0.5423(13) 0.1832(14) 0.190(12) Uiso 0.211(4) 1 d PD B 2 C12S C 0.6627(7) 0.5341(8) 0.1413(7) 0.056(4) Uiso 0.211(4) 1 d PD B 2 C22S C 0.6115(12) 0.5559(12) 0.1394(12) 0.103(7) Uiso 0.211(4) 1 d PD B 2 C32S C 0.5642(5) 0.5501(5) 0.2086(5) 0.030(3) Uiso 0.211(4) 1 d PD B 2 C42S C 0.5696(15) 0.6289(15) 0.1947(14) 0.126(9) Uiso 0.211(4) 1 d PD B 2 O2S O 0.31321(15) 0.6659(2) 0.18938(15) 0.1228(11) Uani 1 1 d D . . C5S C 0.3882(2) 0.7363(3) 0.1850(3) 0.1320(18) Uani 1 1 d D . . C6S C 0.3213(2) 0.7365(2) 0.1616(2) 0.1107(15) Uani 1 1 d D C . C7S C 0.2552(2) 0.6641(4) 0.1756(2) 0.088(3) Uani 0.840(13) 1 d PD C 1 C8S C 0.2528(2) 0.5896(3) 0.1941(2) 0.0785(17) Uani 0.840(13) 1 d PD C 1 C72S C 0.2836(9) 0.6214(8) 0.1909(7) 0.028(6) Uiso 0.160(13) 1 d PD C 2 C82S C 0.2322(13) 0.5737(13) 0.1808(13) 0.069(7) Uiso 0.160(13) 1 d PD C 2 O3S O 0.0398(2) 0.9772(2) 0.4278(2) 0.0843(14) Uani 0.50 1 d PD . . C9S C 0.0980(4) 0.9512(4) 0.3471(4) 0.097(2) Uani 0.50 1 d PD . . C10S C 0.1003(3) 0.9584(4) 0.4088(4) 0.089(2) Uani 0.50 1 d PD . . C11S C 0.0337(2) 0.9878(3) 0.4930(3) 0.1342(18) Uani 1 1 d D . . O4S O 0.4778(5) 0.9491(5) 0.1030(5) 0.327(5) Uiso 1 1 d D . . C121 C 0.5738(6) 0.8800(7) 0.1505(6) 0.287(5) Uiso 1 1 d D . . C131 C 0.5358(5) 0.9399(5) 0.1488(5) 0.229(4) Uiso 1 1 d D E . C141 C 0.3916(8) 0.9466(7) 0.0707(8) 0.176(5) Uiso 0.60 1 d PD D 1 C151 C 0.3996(9) 0.9899(11) 0.0213(11) 0.143(7) Uiso 0.30 1 d PD D 1 C152 C 0.3517(19) 0.9339(19) 0.0648(18) 0.246(16) Uiso 0.30 1 d PD D 1 C142 C 0.4362(11) 0.9300(10) 0.1098(10) 0.166(6) Uiso 0.40 1 d PD E 2 C153 C 0.4407(7) 0.8855(8) 0.1784(8) 0.152(5) Uiso 0.40 1 d PD E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0338(14) 0.0333(12) 0.0492(14) -0.0217(11) -0.0002(10) -0.0054(10) C2A 0.0323(13) 0.0344(12) 0.0468(14) -0.0235(11) 0.0010(10) -0.0060(10) N3A 0.0322(12) 0.0344(10) 0.0456(12) -0.0186(9) 0.0001(9) -0.0062(9) C4A 0.0369(14) 0.0315(12) 0.0445(13) -0.0208(11) -0.0021(10) -0.0027(10) C5A 0.0327(14) 0.0325(12) 0.0460(13) -0.0213(11) 0.0000(10) -0.0033(10) N6A 0.0324(12) 0.0345(11) 0.0469(12) -0.0193(10) -0.0030(9) -0.0037(9) C7A 0.0363(14) 0.0307(12) 0.0437(13) -0.0188(11) -0.0028(10) -0.0041(10) C8A 0.0379(14) 0.0319(12) 0.0503(14) -0.0230(11) -0.0014(11) -0.0051(10) C9A 0.0391(14) 0.0332(12) 0.0470(14) -0.0211(11) 0.0003(11) -0.0082(10) C10A 0.0448(15) 0.0337(12) 0.0489(14) -0.0217(11) -0.0020(11) -0.0090(11) C11A 0.0423(15) 0.0322(12) 0.0499(14) -0.0209(11) -0.0060(11) -0.0047(10) C12A 0.0447(15) 0.0317(12) 0.0463(14) -0.0221(11) -0.0003(11) -0.0066(11) C13A 0.0348(14) 0.0332(12) 0.0498(14) -0.0239(11) -0.0014(10) -0.0042(10) C14A 0.0413(15) 0.0341(12) 0.0480(14) -0.0221(11) -0.0047(11) -0.0030(11) C15A 0.0355(14) 0.0381(13) 0.0519(15) -0.0259(12) 0.0002(11) -0.0062(11) C16A 0.0346(14) 0.0344(12) 0.0474(14) -0.0235(11) 0.0005(10) -0.0049(10) C17A 0.0349(14) 0.0334(12) 0.0485(14) -0.0234(11) -0.0009(10) -0.0044(10) C18A 0.0299(13) 0.0379(12) 0.0511(14) -0.0256(11) -0.0005(10) -0.0031(10) C19A 0.0338(14) 0.0361(12) 0.0485(14) -0.0240(11) 0.0014(10) -0.0076(10) C20A 0.0380(14) 0.0337(12) 0.0488(14) -0.0203(11) 0.0009(11) -0.0072(10) C21A 0.0312(14) 0.0312(12) 0.0563(15) -0.0233(11) 0.0001(11) -0.0031(10) C22A 0.0344(14) 0.0313(12) 0.0562(15) -0.0254(12) 0.0027(11) -0.0053(10) N23A 0.0331(12) 0.0333(10) 0.0510(13) -0.0194(10) -0.0003(10) -0.0052(9) C24A 0.0373(14) 0.0321(12) 0.0508(15) -0.0220(11) -0.0035(11) -0.0015(10) C25A 0.0334(14) 0.0336(12) 0.0523(15) -0.0229(11) -0.0004(11) -0.0032(10) N26A 0.0347(12) 0.0334(10) 0.0491(12) -0.0184(10) -0.0032(9) -0.0044(9) C27A 0.0367(14) 0.0308(12) 0.0482(14) -0.0197(11) 0.0004(10) -0.0027(10) C28A 0.0341(14) 0.0361(12) 0.0500(14) -0.0218(11) -0.0016(10) -0.0047(10) C29A 0.0360(14) 0.0358(13) 0.0550(15) -0.0227(12) 0.0014(11) -0.0056(10) C30A 0.0397(15) 0.0368(13) 0.0499(14) -0.0224(11) -0.0018(11) -0.0041(11) C31A 0.0386(15) 0.0386(13) 0.0507(15) -0.0239(12) -0.0070(11) -0.0011(11) C32A 0.0366(14) 0.0329(12) 0.0507(14) -0.0223(11) -0.0018(11) -0.0033(10) C33A 0.0380(14) 0.0319(12) 0.0546(15) -0.0227(11) -0.0028(11) -0.0041(10) C34A 0.0431(15) 0.0352(13) 0.0552(15) -0.0217(12) -0.0075(12) -0.0034(11) C35A 0.0352(14) 0.0368(13) 0.0617(16) -0.0252(12) -0.0035(11) -0.0034(11) C36A 0.0319(14) 0.0327(12) 0.0580(15) -0.0240(12) -0.0020(11) -0.0037(10) C37A 0.0340(14) 0.0350(12) 0.0603(16) -0.0274(12) -0.0001(11) -0.0024(10) C38A 0.0346(15) 0.0368(13) 0.0657(17) -0.0220(13) -0.0008(12) -0.0050(11) C39A 0.0303(15) 0.0391(13) 0.0691(18) -0.0213(13) 0.0032(12) -0.0052(11) C40A 0.0421(16) 0.0348(13) 0.0595(16) -0.0220(12) 0.0051(12) -0.0063(11) C41A 0.0382(15) 0.0333(12) 0.0465(14) -0.0186(11) 0.0018(11) -0.0071(11) C42A 0.0380(15) 0.0339(12) 0.0496(14) -0.0181(11) 0.0006(11) -0.0074(11) C43A 0.0417(16) 0.0315(12) 0.0509(15) -0.0200(11) 0.0044(12) -0.0073(11) C44A 0.0408(16) 0.0313(12) 0.0466(14) -0.0187(11) 0.0035(11) -0.0099(11) C45A 0.0325(14) 0.0384(13) 0.0532(15) -0.0216(12) 0.0012(11) -0.0078(11) C46A 0.0387(15) 0.0472(14) 0.0599(16) -0.0247(13) 0.0073(12) -0.0090(12) C47A 0.0424(16) 0.0470(15) 0.0589(17) -0.0178(13) 0.0019(12) -0.0139(12) C48A 0.0423(16) 0.0518(15) 0.0700(18) -0.0337(14) 0.0021(13) -0.0152(12) C49A 0.0512(16) 0.0361(13) 0.0468(14) -0.0168(11) -0.0058(11) -0.0103(11) C50A 0.069(2) 0.0457(15) 0.0476(15) -0.0206(13) -0.0018(13) -0.0126(14) C51A 0.0652(19) 0.0360(13) 0.0506(15) -0.0167(12) -0.0034(13) -0.0085(12) C52A 0.0649(19) 0.0482(16) 0.0515(16) -0.0083(13) -0.0126(14) -0.0164(14) C53A 0.0347(16) 0.0557(17) 0.0685(19) -0.0099(15) -0.0005(13) -0.0096(13) C54A 0.043(4) 0.043(4) 0.113(7) -0.034(4) 0.004(4) -0.011(3) C55A 0.061(6) 0.078(5) 0.093(7) -0.058(5) 0.034(4) -0.039(4) C56A 0.036(3) 0.082(5) 0.083(4) -0.025(4) 0.003(3) -0.016(3) C74A 0.048(5) 0.041(4) 0.075(5) -0.026(4) 0.009(3) -0.015(3) C75A 0.049(5) 0.080(6) 0.062(5) -0.033(4) 0.013(3) -0.025(4) C76A 0.040(4) 0.046(3) 0.073(4) -0.022(3) 0.008(3) -0.007(3) C57A 0.0457(16) 0.0392(13) 0.0529(15) -0.0178(12) -0.0024(12) -0.0081(12) C58A 0.0626(19) 0.0360(14) 0.0627(18) -0.0176(13) -0.0027(14) -0.0036(13) C59A 0.0577(19) 0.0459(15) 0.0563(17) -0.0089(13) -0.0100(13) -0.0071(13) C60A 0.0580(19) 0.0550(17) 0.0517(16) -0.0192(14) 0.0028(13) -0.0106(14) N30A 0.0362(12) 0.0356(11) 0.0526(12) -0.0205(10) -0.0015(9) -0.0062(9) N31A 0.0342(12) 0.0342(10) 0.0459(12) -0.0153(10) -0.0034(9) 0.0007(9) N32A 0.0578(15) 0.0463(13) 0.0626(14) -0.0312(12) -0.0129(11) 0.0013(11) C1B 0.0329(14) 0.0408(13) 0.0504(15) -0.0215(12) -0.0028(11) -0.0024(11) C2B 0.0347(14) 0.0410(13) 0.0499(14) -0.0218(12) -0.0028(11) -0.0024(11) N3B 0.0403(12) 0.0337(11) 0.0495(12) -0.0192(10) -0.0051(9) -0.0031(9) C4B 0.0392(15) 0.0324(12) 0.0536(15) -0.0200(11) -0.0006(11) -0.0029(10) C5B 0.0377(14) 0.0322(12) 0.0509(15) -0.0176(11) -0.0034(11) -0.0006(10) N6B 0.0417(13) 0.0305(11) 0.0485(12) -0.0165(10) -0.0047(9) -0.0016(9) C7B 0.0345(14) 0.0308(12) 0.0502(14) -0.0184(11) 0.0004(10) -0.0022(10) C8B 0.0371(14) 0.0324(12) 0.0500(14) -0.0193(11) -0.0023(11) -0.0022(10) C9B 0.0403(15) 0.0380(13) 0.0496(14) -0.0214(12) -0.0029(11) -0.0046(11) C10B 0.0394(15) 0.0364(13) 0.0511(15) -0.0220(11) 0.0020(11) -0.0056(11) C11B 0.0417(15) 0.0319(12) 0.0502(15) -0.0172(11) 0.0004(11) -0.0022(11) C12B 0.0378(15) 0.0344(12) 0.0498(14) -0.0201(11) -0.0006(11) -0.0019(10) C13B 0.0410(15) 0.0334(12) 0.0532(15) -0.0205(11) -0.0024(11) -0.0020(11) C14B 0.0466(16) 0.0305(12) 0.0610(17) -0.0167(12) -0.0071(12) 0.0008(11) C15B 0.0479(16) 0.0340(13) 0.0560(16) -0.0182(12) -0.0105(12) 0.0034(11) C16B 0.0391(15) 0.0359(13) 0.0545(15) -0.0198(12) -0.0055(11) -0.0002(11) C17B 0.0392(15) 0.0379(13) 0.0506(15) -0.0193(12) -0.0036(11) -0.0003(11) C18B 0.0403(15) 0.0410(14) 0.0523(15) -0.0175(12) -0.0082(11) -0.0007(11) C19B 0.0368(15) 0.0465(14) 0.0503(15) -0.0213(12) -0.0049(11) -0.0036(11) C20B 0.0387(15) 0.0421(14) 0.0549(16) -0.0246(12) -0.0025(11) -0.0035(11) C21B 0.0349(14) 0.0325(12) 0.0510(14) -0.0194(11) -0.0011(11) -0.0014(10) C22B 0.0324(14) 0.0350(12) 0.0483(14) -0.0203(11) -0.0006(10) -0.0009(10) N23B 0.0399(12) 0.0297(10) 0.0448(12) -0.0164(10) -0.0031(9) -0.0051(9) C24B 0.0313(14) 0.0314(12) 0.0527(15) -0.0204(11) 0.0013(10) -0.0025(10) C25B 0.0304(13) 0.0317(12) 0.0506(15) -0.0191(11) -0.0006(10) -0.0018(10) N26B 0.0367(12) 0.0300(10) 0.0481(12) -0.0172(10) 0.0000(9) -0.0050(9) C27B 0.0290(13) 0.0352(12) 0.0544(15) -0.0237(11) -0.0014(10) -0.0024(10) C28B 0.0322(14) 0.0350(12) 0.0546(15) -0.0232(11) -0.0007(11) -0.0010(10) C29B 0.0318(14) 0.0378(13) 0.0584(16) -0.0258(12) -0.0024(11) -0.0001(10) C30B 0.0301(14) 0.0348(13) 0.0620(16) -0.0249(12) -0.0028(11) -0.0011(10) C31B 0.0338(14) 0.0349(12) 0.0573(16) -0.0213(12) -0.0018(11) -0.0033(10) C32B 0.0294(13) 0.0354(12) 0.0562(15) -0.0234(12) -0.0009(10) -0.0023(10) C33B 0.0332(14) 0.0322(12) 0.0536(15) -0.0204(11) 0.0005(11) -0.0040(10) C34B 0.0369(14) 0.0308(12) 0.0598(16) -0.0201(12) 0.0023(11) -0.0055(10) C35B 0.0342(14) 0.0341(12) 0.0512(14) -0.0176(11) 0.0002(11) -0.0043(10) C36B 0.0332(14) 0.0318(12) 0.0499(14) -0.0191(11) 0.0007(10) -0.0018(10) C37B 0.0302(13) 0.0328(12) 0.0495(14) -0.0193(11) 0.0000(10) -0.0002(10) C38B 0.0362(14) 0.0322(12) 0.0460(14) -0.0153(11) -0.0021(10) -0.0013(10) C39B 0.0327(14) 0.0367(13) 0.0497(14) -0.0202(11) -0.0025(10) -0.0013(10) C40B 0.0362(14) 0.0343(12) 0.0515(15) -0.0209(11) -0.0042(11) -0.0023(10) C41B 0.0342(14) 0.0398(14) 0.0515(15) -0.0250(13) -0.0028(11) -0.0033(11) C42B 0.0345(14) 0.0424(14) 0.0536(15) -0.0281(13) -0.0035(11) -0.0048(11) C43B 0.0346(14) 0.0372(13) 0.0505(15) -0.0232(12) -0.0044(11) -0.0013(10) C44B 0.0369(14) 0.0352(13) 0.0484(15) -0.0200(12) -0.0038(11) -0.0038(10) C45B 0.0453(16) 0.0475(15) 0.0516(15) -0.0213(13) -0.0076(12) -0.0039(12) C46B 0.105(3) 0.0609(19) 0.063(2) -0.0264(16) -0.0275(18) 0.0085(18) C47B 0.071(2) 0.093(2) 0.064(2) -0.0222(18) -0.0183(16) -0.0311(19) C48B 0.060(2) 0.097(2) 0.064(2) -0.0429(19) -0.0038(15) -0.0052(18) C49B 0.0476(16) 0.0350(13) 0.0560(16) -0.0206(12) -0.0014(12) -0.0070(11) C50B 0.079(2) 0.0395(15) 0.0704(19) -0.0224(14) -0.0102(16) -0.0165(14) C51B 0.0542(18) 0.0628(18) 0.080(2) -0.0411(16) 0.0057(15) -0.0230(15) C52B 0.070(2) 0.0469(15) 0.0641(18) -0.0325(14) 0.0039(14) -0.0137(14) C53B 0.0450(16) 0.0395(13) 0.0506(15) -0.0179(12) -0.0076(11) -0.0066(11) C54B 0.074(2) 0.0438(15) 0.0581(17) -0.0214(13) -0.0157(15) -0.0083(14) C55B 0.074(2) 0.0508(17) 0.071(2) -0.0231(15) -0.0249(16) 0.0029(15) C56B 0.076(2) 0.082(2) 0.0564(18) -0.0274(17) 0.0003(15) -0.0329(18) C57B 0.0370(15) 0.0381(13) 0.0667(17) -0.0285(13) -0.0052(12) -0.0046(11) C58B 0.0495(17) 0.0473(15) 0.087(2) -0.0429(15) 0.0046(14) -0.0076(13) C59B 0.0641(19) 0.0361(14) 0.079(2) -0.0282(14) -0.0135(15) -0.0093(13) C60B 0.0390(15) 0.0444(14) 0.0716(18) -0.0346(14) -0.0016(12) -0.0073(12) N30B 0.0398(13) 0.0335(10) 0.0547(13) -0.0201(10) -0.0041(9) -0.0010(10) N31B 0.0435(14) 0.0306(10) 0.0497(12) -0.0180(9) 0.0007(9) -0.0087(11) N32B 0.0450(14) 0.0384(12) 0.0728(16) -0.0248(11) 0.0018(11) -0.0006(11) C1C 0.0364(14) 0.0324(12) 0.0444(13) -0.0158(11) 0.0009(10) -0.0035(10) C2C 0.0357(14) 0.0351(12) 0.0416(13) -0.0148(11) 0.0012(10) -0.0052(10) N3C 0.0346(12) 0.0297(10) 0.0455(12) -0.0169(9) -0.0054(9) -0.0020(8) C4C 0.0397(14) 0.0287(11) 0.0418(13) -0.0145(10) 0.0011(10) -0.0056(10) C5C 0.0363(14) 0.0322(12) 0.0415(13) -0.0149(10) -0.0004(10) -0.0049(10) N6C 0.0377(12) 0.0295(10) 0.0501(12) -0.0189(9) -0.0053(9) -0.0026(9) C7C 0.0385(14) 0.0293(11) 0.0418(13) -0.0140(10) -0.0002(10) -0.0025(10) C8C 0.0401(15) 0.0316(12) 0.0477(14) -0.0164(11) -0.0032(11) -0.0055(10) C9C 0.0374(14) 0.0317(12) 0.0510(15) -0.0150(11) -0.0054(11) -0.0029(10) C10C 0.0437(15) 0.0302(12) 0.0448(14) -0.0142(11) -0.0015(11) -0.0032(10) C11C 0.0399(15) 0.0323(12) 0.0485(14) -0.0176(11) -0.0025(11) -0.0061(10) C12C 0.0357(14) 0.0321(12) 0.0421(13) -0.0147(10) -0.0005(10) -0.0036(10) C13C 0.0408(15) 0.0286(11) 0.0416(13) -0.0140(10) -0.0005(10) -0.0044(10) C14C 0.0449(15) 0.0299(12) 0.0507(14) -0.0190(11) -0.0008(11) -0.0076(11) C15C 0.0381(15) 0.0337(12) 0.0529(15) -0.0191(11) -0.0036(11) -0.0079(11) C16C 0.0362(14) 0.0318(12) 0.0439(13) -0.0150(10) 0.0014(10) -0.0056(10) C17C 0.0363(14) 0.0333(12) 0.0485(14) -0.0157(11) -0.0010(11) -0.0058(10) C18C 0.0417(15) 0.0351(13) 0.0574(16) -0.0201(12) -0.0023(12) -0.0085(11) C19C 0.0392(15) 0.0368(13) 0.0592(16) -0.0186(12) -0.0048(12) -0.0050(11) C20C 0.0378(15) 0.0332(12) 0.0558(15) -0.0192(11) -0.0032(11) -0.0026(10) C21C 0.0394(14) 0.0327(12) 0.0427(13) -0.0178(10) -0.0024(10) -0.0041(10) C22C 0.0351(14) 0.0326(12) 0.0408(13) -0.0164(10) -0.0036(10) -0.0019(10) N23C 0.0357(12) 0.0304(10) 0.0467(12) -0.0181(9) -0.0050(9) -0.0019(9) C24C 0.0406(14) 0.0289(11) 0.0424(13) -0.0180(10) -0.0006(10) -0.0042(10) C25C 0.0369(14) 0.0320(12) 0.0407(13) -0.0175(10) -0.0032(10) -0.0035(10) N26C 0.0380(12) 0.0309(10) 0.0457(12) -0.0192(9) -0.0023(9) -0.0037(9) C27C 0.0376(14) 0.0316(12) 0.0420(13) -0.0186(10) -0.0028(10) -0.0006(10) C28C 0.0425(15) 0.0349(12) 0.0405(13) -0.0186(11) -0.0025(10) -0.0038(11) C29C 0.0385(14) 0.0389(13) 0.0459(14) -0.0221(11) -0.0008(11) 0.0000(11) C30C 0.0449(16) 0.0334(12) 0.0442(14) -0.0192(11) -0.0078(11) 0.0025(11) C31C 0.0443(16) 0.0324(12) 0.0450(14) -0.0181(11) -0.0070(11) -0.0029(11) C32C 0.0440(15) 0.0339(12) 0.0416(13) -0.0192(11) -0.0037(10) -0.0033(11) C33C 0.0392(14) 0.0318(12) 0.0417(13) -0.0186(10) -0.0046(10) 0.0007(10) C34C 0.0443(15) 0.0304(12) 0.0447(13) -0.0181(11) -0.0045(11) -0.0047(11) C35C 0.0425(15) 0.0343(12) 0.0454(14) -0.0202(11) -0.0021(11) -0.0082(11) C36C 0.0375(14) 0.0330(12) 0.0386(12) -0.0168(10) -0.0010(10) -0.0036(10) C37C 0.0407(15) 0.0320(12) 0.0390(13) -0.0156(10) -0.0021(10) -0.0048(10) C38C 0.0376(14) 0.0354(12) 0.0446(13) -0.0201(11) -0.0018(10) -0.0063(10) C39C 0.0369(14) 0.0380(13) 0.0423(13) -0.0196(11) -0.0031(10) -0.0036(10) C40C 0.0379(14) 0.0325(12) 0.0430(13) -0.0152(10) -0.0053(10) -0.0012(10) C41C 0.0340(14) 0.0331(12) 0.0444(14) -0.0151(11) -0.0003(10) 0.0001(10) C42C 0.0352(14) 0.0356(12) 0.0423(13) -0.0167(11) -0.0008(10) -0.0012(10) C43C 0.0379(14) 0.0313(12) 0.0450(14) -0.0154(11) -0.0053(10) 0.0000(10) C44C 0.0375(14) 0.0308(12) 0.0483(14) -0.0151(11) -0.0065(11) 0.0008(10) C45C 0.0380(17) 0.0447(15) 0.097(2) -0.0342(16) -0.0172(14) 0.0016(12) C46C 0.116(4) 0.054(2) 0.229(6) -0.002(3) -0.124(4) -0.008(2) C47C 0.051(2) 0.063(2) 0.128(3) -0.053(2) -0.0252(19) 0.0018(15) C48C 0.033(2) 0.283(7) 0.222(6) -0.203(6) 0.007(3) -0.009(3) C49C 0.0408(15) 0.0300(12) 0.0599(16) -0.0198(12) -0.0073(12) -0.0003(10) C50C 0.100(3) 0.0314(14) 0.0554(17) -0.0156(13) -0.0060(16) 0.0034(14) C51C 0.0510(19) 0.0469(16) 0.121(3) -0.0474(18) -0.0259(17) 0.0085(13) C52C 0.0493(16) 0.0350(13) 0.0557(16) -0.0200(12) -0.0015(12) -0.0025(11) C53C 0.0378(15) 0.0389(13) 0.0504(15) -0.0211(12) -0.0060(11) -0.0029(11) C54C 0.051(2) 0.090(2) 0.092(2) -0.063(2) -0.0223(16) 0.0088(17) C55C 0.0413(16) 0.0421(14) 0.0621(17) -0.0150(13) -0.0065(12) -0.0038(12) C56C 0.0447(17) 0.0425(15) 0.077(2) -0.0140(14) -0.0010(14) -0.0026(13) C57C 0.0462(16) 0.0331(12) 0.0543(15) -0.0230(12) -0.0080(12) 0.0023(11) C58C 0.0509(17) 0.0375(13) 0.0602(17) -0.0231(13) -0.0108(13) 0.0082(12) C59C 0.0517(18) 0.0433(14) 0.0647(18) -0.0306(13) -0.0047(13) 0.0057(12) C60C 0.0526(18) 0.0379(14) 0.0756(19) -0.0313(14) -0.0100(14) 0.0034(12) N30C 0.0430(13) 0.0338(11) 0.0483(13) -0.0182(10) -0.0016(10) -0.0056(9) N31C 0.0340(12) 0.0371(11) 0.0516(14) -0.0251(11) -0.0047(10) -0.0053(9) N32C 0.0538(15) 0.0566(14) 0.0522(14) -0.0208(12) 0.0043(11) -0.0189(12) N1X 0.0422(13) 0.0349(11) 0.0536(13) -0.0215(10) 0.0007(10) 0.0036(9) C1X 0.0613(19) 0.0299(12) 0.0594(17) -0.0201(12) -0.0052(13) 0.0023(12) C2X 0.0548(18) 0.0386(14) 0.0662(18) -0.0203(13) -0.0037(14) -0.0056(13) C3X 0.083(2) 0.0381(14) 0.0635(18) -0.0243(14) -0.0058(16) -0.0020(14) C4X 0.087(2) 0.0475(16) 0.0658(19) -0.0169(15) -0.0053(17) -0.0257(16) C5X 0.0421(16) 0.0461(15) 0.0582(16) -0.0244(13) 0.0000(12) 0.0077(12) C6X 0.0478(19) 0.0568(17) 0.0661(19) -0.0125(15) 0.0110(14) 0.0029(14) C7X 0.0485(18) 0.0618(18) 0.070(2) -0.0297(16) 0.0057(14) -0.0013(14) C8X 0.088(3) 0.086(3) 0.109(3) -0.043(2) 0.004(2) -0.036(2) C9X 0.0429(15) 0.0339(12) 0.0573(16) -0.0227(12) 0.0008(12) -0.0005(11) C10X 0.0464(17) 0.0418(14) 0.0579(16) -0.0228(13) -0.0018(12) 0.0041(12) C11X 0.0434(16) 0.0466(14) 0.0550(16) -0.0250(13) -0.0020(12) 0.0018(12) C12X 0.0541(18) 0.0559(17) 0.0667(18) -0.0329(15) 0.0011(14) -0.0052(14) C13X 0.0415(15) 0.0361(13) 0.0546(15) -0.0216(12) -0.0014(11) 0.0038(11) C14X 0.0520(17) 0.0418(14) 0.0611(17) -0.0272(13) -0.0027(13) 0.0026(12) C15X 0.0439(16) 0.0478(15) 0.0593(17) -0.0277(13) -0.0022(12) -0.0003(12) C16X 0.068(2) 0.0525(17) 0.0629(19) -0.0221(15) -0.0106(15) -0.0064(15) N1Y 0.0469(13) 0.0427(12) 0.0512(13) -0.0214(10) 0.0070(10) -0.0123(10) C1Y 0.0474(16) 0.0465(15) 0.0591(16) -0.0256(13) 0.0064(12) -0.0150(12) C2Y 0.0517(18) 0.0520(16) 0.0628(18) -0.0256(14) -0.0020(13) -0.0092(13) C3Y 0.0573(19) 0.075(2) 0.073(2) -0.0415(17) 0.0042(15) -0.0175(16) C4Y 0.068(2) 0.086(2) 0.082(2) -0.039(2) -0.0163(17) -0.0165(18) C5Y 0.0492(16) 0.0432(14) 0.0509(15) -0.0209(12) 0.0098(12) -0.0112(12) C6Y 0.0642(19) 0.0600(17) 0.0544(17) -0.0274(14) 0.0106(14) -0.0265(15) C7Y 0.0591(19) 0.0542(16) 0.0565(17) -0.0275(14) 0.0070(13) -0.0151(14) C8Y 0.114(3) 0.060(2) 0.065(2) -0.0187(17) -0.0150(19) -0.0229(19) C9Y 0.0464(16) 0.0493(15) 0.0520(15) -0.0238(13) 0.0100(12) -0.0135(12) C10Y 0.0535(17) 0.0448(14) 0.0565(16) -0.0246(13) 0.0103(13) -0.0128(13) C11Y 0.065(2) 0.0476(16) 0.0602(18) -0.0239(14) 0.0137(14) -0.0089(14) C12Y 0.054(2) 0.073(2) 0.100(3) -0.043(2) 0.0124(17) -0.0056(17) C13Y 0.0519(17) 0.0434(14) 0.0500(15) -0.0204(12) 0.0062(12) -0.0125(12) C14Y 0.0528(18) 0.0454(15) 0.0608(17) -0.0197(13) 0.0048(13) -0.0106(13) C15Y 0.0622(19) 0.0479(15) 0.0570(17) -0.0213(13) 0.0072(14) -0.0080(14) C16Y 0.067(2) 0.067(2) 0.125(3) -0.059(2) 0.000(2) -0.0096(17) N1Z 0.0418(13) 0.0485(12) 0.0519(13) -0.0299(10) 0.0016(9) -0.0067(10) C1Z 0.0438(16) 0.0546(15) 0.0477(15) -0.0274(13) -0.0024(11) -0.0064(12) C2Z 0.0472(16) 0.0483(15) 0.0555(16) -0.0264(13) -0.0022(12) -0.0060(12) C3Z 0.0579(19) 0.0595(17) 0.0550(17) -0.0271(14) -0.0057(13) -0.0028(14) C4Z 0.064(2) 0.0507(17) 0.070(2) -0.0200(15) -0.0148(15) -0.0012(15) C5Z 0.0439(16) 0.0506(15) 0.0558(16) -0.0346(13) 0.0049(12) -0.0074(12) C6Z 0.0542(19) 0.0632(18) 0.077(2) -0.0459(17) -0.0138(15) 0.0055(14) C7Z 0.0565(18) 0.0504(16) 0.0628(18) -0.0320(14) -0.0031(13) -0.0016(13) C8Z 0.074(3) 0.054(2) 0.224(6) -0.047(3) -0.037(3) -0.0017(19) C9Z 0.0451(16) 0.0493(15) 0.0501(15) -0.0292(13) 0.0021(11) -0.0077(12) C10Z 0.0477(17) 0.0639(17) 0.0628(17) -0.0410(15) 0.0062(13) -0.0138(14) C11Z 0.0585(19) 0.0696(19) 0.0692(19) -0.0466(17) 0.0169(15) -0.0256(16) C12Z 0.083(2) 0.075(2) 0.062(2) -0.0287(17) 0.0126(17) -0.0262(19) C13Z 0.0433(15) 0.0481(14) 0.0546(15) -0.0313(13) -0.0004(12) -0.0073(12) C14Z 0.0499(17) 0.0524(15) 0.0549(16) -0.0306(13) 0.0012(12) -0.0093(13) C15Z 0.0514(17) 0.0559(16) 0.0594(17) -0.0349(14) 0.0049(13) -0.0128(13) C16Z 0.052(2) 0.086(2) 0.072(2) -0.0332(18) 0.0054(15) -0.0187(17) O1S 0.088(3) 0.0472(16) 0.097(2) -0.0366(16) -0.0194(18) -0.0011(15) C1S 0.075(3) 0.041(2) 0.113(4) -0.039(2) 0.003(3) -0.0015(19) C2S 0.033(3) 0.098(4) 0.084(3) 0.024(3) -0.002(2) -0.008(3) C3S 0.108(4) 0.079(3) 0.078(3) -0.030(3) -0.008(3) -0.028(3) C4S 0.096(4) 0.091(4) 0.094(4) -0.043(3) 0.001(3) -0.019(3) O2S 0.104(2) 0.170(3) 0.094(2) -0.058(2) 0.0112(17) -0.016(2) C5S 0.106(4) 0.171(5) 0.140(4) -0.081(4) 0.011(3) -0.038(4) C6S 0.128(4) 0.095(3) 0.131(4) -0.061(3) 0.035(3) -0.051(3) C7S 0.043(3) 0.159(7) 0.078(3) -0.062(4) 0.001(2) -0.019(4) C8S 0.070(3) 0.101(4) 0.061(3) -0.028(3) 0.007(2) -0.022(3) O3S 0.087(4) 0.078(3) 0.093(4) -0.037(3) -0.003(3) -0.019(3) C9S 0.120(7) 0.088(5) 0.081(5) -0.038(4) -0.008(5) 0.004(5) C10S 0.068(5) 0.079(5) 0.124(7) -0.048(5) 0.011(4) -0.016(4) C11S 0.134(4) 0.116(4) 0.166(5) -0.067(4) 0.012(4) -0.036(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 C1A C2A 1.394(3) . ? C1A C20A 1.406(3) . ? C1A C41A 1.437(3) . ? C2A N3A 1.383(3) . ? C2A C17A 1.407(3) . ? N3A C4A 1.376(3) . ? C4A C5A 1.392(3) . ? C4A C16A 1.408(3) . ? C5A N6A 1.388(3) . ? C5A C13A 1.403(3) . ? N6A C7A 1.369(3) . ? C7A C8A 1.405(3) . ? C7A C12A 1.412(3) . ? C8A C9A 1.384(3) . ? C8A C44A 1.431(4) . ? C9A C10A 1.397(3) . ? C10A C11A 1.407(3) . ? C10A C49A 1.533(3) . ? C11A C12A 1.397(3) . ? C12A C13A 1.462(3) . ? C13A C14A 1.413(3) . ? C14A C15A 1.377(3) . ? C15A C16A 1.413(3) . ? C16A C17A 1.447(3) . ? C17A C18A 1.403(3) . ? C18A C19A 1.391(3) . ? C19A C20A 1.400(3) . ? C19A C45A 1.542(3) . ? C21A C22A 1.389(3) . ? C21A C40A 1.400(3) . ? C21A C43A 1.433(3) . ? C22A N23A 1.380(3) . ? C22A C37A 1.405(3) . ? N23A C24A 1.373(3) . ? C24A C25A 1.396(3) . ? C24A C36A 1.408(3) . ? C25A N26A 1.385(3) . ? C25A C33A 1.408(3) . ? N26A C27A 1.371(3) . ? C27A C32A 1.405(3) . ? C27A C28A 1.418(3) . ? C28A C29A 1.388(3) . ? C28A C42A 1.434(3) . ? C29A C30A 1.407(3) . ? C30A C31A 1.396(3) . ? C30A C57A 1.532(3) . ? C31A C32A 1.391(3) . ? C32A C33A 1.459(3) . ? C33A C34A 1.412(3) . ? C34A C35A 1.374(4) . ? C35A C36A 1.420(4) . ? C36A C37A 1.453(3) . ? C37A C38A 1.408(3) . ? C38A C39A 1.385(4) . ? C39A C40A 1.401(4) . ? C39A C53A 1.547(4) . ? C41A C42A 1.197(3) . ? C43A C44A 1.208(3) . ? C45A C47A 1.521(4) . ? C45A C46A 1.539(3) . ? C45A C48A 1.544(3) . ? C49A C52A 1.528(4) . ? C49A C51A 1.538(3) . ? C49A C50A 1.541(4) . ? C53A C74A 1.334(6) . ? C53A C55A 1.363(8) . ? C53A C76A 1.612(6) . ? C53A C56A 1.629(6) . ? C53A C54A 1.636(7) . ? C53A C75A 1.680(9) . ? C57A C59A 1.532(4) . ? C57A C60A 1.538(4) . ? C57A C58A 1.540(3) . ? N30A N31A 1.188(3) . ? N31A N32A 1.168(3) . ? C1B C2B 1.401(3) . ? C1B C20B 1.402(3) . ? C1B C41B 1.424(3) . ? C2B N3B 1.386(3) . ? C2B C17B 1.409(3) . ? N3B C4B 1.387(3) . ? C4B C5B 1.399(3) . ? C4B C16B 1.400(4) . ? C5B N6B 1.371(3) . ? C5B C13B 1.411(3) . ? N6B C7B 1.375(3) . ? C7B C8B 1.399(3) . ? C7B C12B 1.407(3) . ? C8B C9B 1.397(3) . ? C8B C44B 1.433(3) . ? C9B C10B 1.403(3) . ? C10B C11B 1.393(3) . ? C10B C49B 1.537(3) . ? C11B C12B 1.406(3) . ? C12B C13B 1.456(3) . ? C13B C14B 1.408(4) . ? C14B C15B 1.378(3) . ? C15B C16B 1.411(3) . ? C16B C17B 1.459(3) . ? C17B C18B 1.401(3) . ? C18B C19B 1.397(3) . ? C19B C20B 1.406(3) . ? C19B C45B 1.534(4) . ? C21B C22B 1.400(3) . ? C21B C40B 1.404(3) . ? C21B C43B 1.435(3) . ? C22B N23B 1.372(3) . ? C22B C37B 1.410(3) . ? N23B C24B 1.376(3) . ? C24B C36B 1.394(3) . ? C24B C25B 1.406(3) . ? C25B N26B 1.374(3) . ? C25B C33B 1.407(3) . ? N26B C27B 1.377(3) . ? C27B C28B 1.402(3) . ? C27B C32B 1.403(3) . ? C28B C29B 1.404(3) . ? C28B C42B 1.432(4) . ? C29B C30B 1.402(3) . ? C30B C31B 1.390(3) . ? C30B C57B 1.540(3) . ? C31B C32B 1.403(3) . ? C32B C33B 1.454(3) . ? C33B C34B 1.408(3) . ? C34B C35B 1.380(3) . ? C35B C36B 1.416(3) . ? C36B C37B 1.459(3) . ? C37B C38B 1.400(3) . ? C38B C39B 1.396(3) . ? C39B C40B 1.404(3) . ? C39B C53B 1.533(3) . ? C41B C42B 1.208(3) . ? C43B C44B 1.194(3) . ? C45B C46B 1.513(4) . ? C45B C48B 1.523(4) . ? C45B C47B 1.535(4) . ? C49B C50B 1.519(4) . ? C49B C51B 1.526(4) . ? C49B C52B 1.537(4) . ? C53B C54B 1.524(3) . ? C53B C56B 1.531(4) . ? C53B C55B 1.542(4) . ? C57B C59B 1.529(4) . ? C57B C60B 1.532(3) . ? C57B C58B 1.550(4) . ? N30B N31B 1.197(3) . ? N31B N32B 1.173(3) . ? C1C C20C 1.394(3) . ? C1C C2C 1.410(3) . ? C1C C41C 1.430(3) . ? C2C N3C 1.369(3) . ? C2C C17C 1.410(3) . ? N3C C4C 1.380(3) . ? C4C C5C 1.389(3) . ? C4C C16C 1.409(3) . ? C5C N6C 1.383(3) . ? C5C C13C 1.410(3) . ? N6C C7C 1.370(3) . ? C7C C8C 1.403(3) . ? C7C C12C 1.405(3) . ? C8C C9C 1.404(3) . ? C8C C44C 1.438(3) . ? C9C C10C 1.407(3) . ? C10C C11C 1.393(3) . ? C10C C49C 1.540(3) . ? C11C C12C 1.395(3) . ? C12C C13C 1.448(3) . ? C13C C14C 1.418(3) . ? C14C C15C 1.369(3) . ? C15C C16C 1.425(3) . ? C16C C17C 1.446(3) . ? C17C C18C 1.399(3) . ? C18C C19C 1.395(3) . ? C19C C20C 1.407(3) . ? C19C C45C 1.534(4) . ? C21C C40C 1.396(3) . ? C21C C22C 1.401(3) . ? C21C C43C 1.436(3) . ? C22C N23C 1.373(3) . ? C22C C37C 1.416(3) . ? N23C C24C 1.386(3) . ? C24C C25C 1.397(3) . ? C24C C36C 1.406(3) . ? C25C N26C 1.381(3) . ? C25C C33C 1.404(3) . ? N26C C27C 1.381(3) . ? C27C C28C 1.402(3) . ? C27C C32C 1.404(3) . ? C28C C29C 1.403(3) . ? C28C C42C 1.442(3) . ? C29C C30C 1.410(3) . ? C30C C31C 1.386(3) . ? C30C C57C 1.545(3) . ? C31C C32C 1.402(3) . ? C32C C33C 1.459(3) . ? C33C C34C 1.411(3) . ? C34C C35C 1.382(3) . ? C35C C36C 1.412(3) . ? C36C C37C 1.456(3) . ? C37C C38C 1.392(3) . ? C38C C39C 1.403(3) . ? C39C C40C 1.405(3) . ? C39C C53C 1.536(3) . ? C41C C42C 1.203(3) . ? C43C C44C 1.202(3) . ? C45C C48C 1.519(5) . ? C45C C47C 1.522(4) . ? C45C C46C 1.523(5) . ? C49C C52C 1.520(3) . ? C49C C50C 1.529(4) . ? C49C C51C 1.536(4) . ? C53C C54C 1.531(4) . ? C53C C55C 1.533(3) . ? C53C C56C 1.535(4) . ? C57C C60C 1.525(3) . ? C57C C59C 1.534(4) . ? C57C C58C 1.535(4) . ? N30C N31C 1.194(3) . ? N31C N32C 1.175(3) . ? N1X C13X 1.515(3) . ? N1X C1X 1.521(3) . ? N1X C9X 1.527(3) . ? N1X C5X 1.529(3) . ? C1X C2X 1.525(4) . ? C2X C3X 1.512(4) . ? C3X C4X 1.507(4) . ? C5X C6X 1.499(4) . ? C6X C7X 1.537(4) . ? C7X C8X 1.533(5) . ? C9X C10X 1.524(4) . ? C10X C11X 1.527(3) . ? C11X C12X 1.519(4) . ? C13X C14X 1.523(3) . ? C14X C15X 1.521(4) . ? C15X C16X 1.511(4) . ? N1Y C13Y 1.515(3) . ? N1Y C5Y 1.516(3) . ? N1Y C9Y 1.520(3) . ? N1Y C1Y 1.521(3) . ? C1Y C2Y 1.523(4) . ? C2Y C3Y 1.518(4) . ? C3Y C4Y 1.507(4) . ? C5Y C6Y 1.525(4) . ? C6Y C7Y 1.525(4) . ? C7Y C8Y 1.507(4) . ? C9Y C10Y 1.518(4) . ? C10Y C11Y 1.517(4) . ? C11Y C12Y 1.523(4) . ? C13Y C14Y 1.526(4) . ? C14Y C15Y 1.521(4) . ? C15Y C16Y 1.515(4) . ? N1Z C13Z 1.518(3) . ? N1Z C1Z 1.520(3) . ? N1Z C9Z 1.521(3) . ? N1Z C5Z 1.527(3) . ? C1Z C2Z 1.519(3) . ? C2Z C3Z 1.506(4) . ? C3Z C4Z 1.520(4) . ? C5Z C6Z 1.511(4) . ? C6Z C7Z 1.530(4) . ? C7Z C8Z 1.509(5) . ? C9Z C10Z 1.533(3) . ? C10Z C11Z 1.519(4) . ? C11Z C12Z 1.508(4) . ? C13Z C14Z 1.516(4) . ? C14Z C15Z 1.520(3) . ? C15Z C16Z 1.510(4) . ? O1S C2S 1.262(6) . ? O1S C3S 1.434(5) . ? C1S C2S 1.833(9) . ? C3S C4S 1.391(7) . ? O12S C32S 0.67(3) . ? O12S C22S 1.37(3) . ? C12S C22S 1.17(3) . ? C22S C32S 1.79(3) . ? C32S C42S 1.70(3) . ? O2S C72S 1.278(16) . ? O2S C7S 1.377(5) . ? O2S C6S 1.483(5) . ? C5S C6S 1.632(7) . ? C7S C8S 1.562(8) . ? C72S C82S 1.79(4) . ? O3S C10S 1.446(9) . ? O3S C11S 1.581(7) . ? C9S C10S 1.477(11) . ? C11S C11S 1.582(11) 2_576 ? O4S C142 1.07(2) . ? O4S C131 1.663(11) . ? C121 C131 1.466(13) . ? C141 C152 1.02(4) . ? C141 C151 1.16(2) . ? C151 C152 1.72(4) . ? C142 C153 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A C20A 116.8(2) . . ? C2A C1A C41A 120.2(2) . . ? C20A C1A C41A 122.9(2) . . ? N3A C2A C1A 128.8(2) . . ? N3A C2A C17A 109.1(2) . . ? C1A C2A C17A 122.2(2) . . ? C4A N3A C2A 108.3(2) . . ? N3A C4A C5A 129.9(2) . . ? N3A C4A C16A 110.1(2) . . ? C5A C4A C16A 120.0(2) . . ? N6A C5A C4A 130.2(2) . . ? N6A C5A C13A 109.9(2) . . ? C4A C5A C13A 119.9(2) . . ? C7A N6A C5A 108.5(2) . . ? N6A C7A C8A 129.0(2) . . ? N6A C7A C12A 109.6(2) . . ? C8A C7A C12A 121.4(2) . . ? C9A C8A C7A 117.0(2) . . ? C9A C8A C44A 122.8(2) . . ? C7A C8A C44A 120.2(2) . . ? C8A C9A C10A 123.7(2) . . ? C9A C10A C11A 118.4(2) . . ? C9A C10A C49A 119.3(2) . . ? C11A C10A C49A 122.4(2) . . ? C12A C11A C10A 119.9(2) . . ? C11A C12A C7A 119.6(2) . . ? C11A C12A C13A 134.0(2) . . ? C7A C12A C13A 106.3(2) . . ? C5A C13A C14A 119.9(2) . . ? C5A C13A C12A 105.7(2) . . ? C14A C13A C12A 134.4(2) . . ? C15A C14A C13A 120.2(2) . . ? C14A C15A C16A 120.1(2) . . ? C4A C16A C15A 119.8(2) . . ? C4A C16A C17A 105.6(2) . . ? C15A C16A C17A 134.6(2) . . ? C18A C17A C2A 119.0(2) . . ? C18A C17A C16A 134.0(2) . . ? C2A C17A C16A 106.96(19) . . ? C19A C18A C17A 120.5(2) . . ? C18A C19A C20A 118.9(2) . . ? C18A C19A C45A 119.7(2) . . ? C20A C19A C45A 121.3(2) . . ? C19A C20A C1A 122.6(2) . . ? C22A C21A C40A 117.0(2) . . ? C22A C21A C43A 120.2(2) . . ? C40A C21A C43A 122.7(2) . . ? N23A C22A C21A 128.6(2) . . ? N23A C22A C37A 109.2(2) . . ? C21A C22A C37A 122.2(2) . . ? C24A N23A C22A 108.6(2) . . ? N23A C24A C25A 130.2(2) . . ? N23A C24A C36A 109.9(2) . . ? C25A C24A C36A 119.9(2) . . ? N26A C25A C24A 129.5(2) . . ? N26A C25A C33A 110.1(2) . . ? C24A C25A C33A 120.1(2) . . ? C27A N26A C25A 107.7(2) . . ? N26A C27A C32A 110.4(2) . . ? N26A C27A C28A 127.9(2) . . ? C32A C27A C28A 121.7(2) . . ? C29A C28A C27A 116.3(2) . . ? C29A C28A C42A 123.2(2) . . ? C27A C28A C42A 120.5(2) . . ? C28A C29A C30A 123.5(2) . . ? C31A C30A C29A 118.2(2) . . ? C31A C30A C57A 122.8(2) . . ? C29A C30A C57A 118.9(2) . . ? C32A C31A C30A 120.7(2) . . ? C31A C32A C27A 119.4(2) . . ? C31A C32A C33A 134.2(2) . . ? C27A C32A C33A 106.1(2) . . ? C25A C33A C34A 119.6(2) . . ? C25A C33A C32A 105.6(2) . . ? C34A C33A C32A 134.5(2) . . ? C35A C34A C33A 120.5(2) . . ? C34A C35A C36A 120.0(2) . . ? C24A C36A C35A 119.7(2) . . ? C24A C36A C37A 105.6(2) . . ? C35A C36A C37A 134.7(2) . . ? C22A C37A C38A 118.8(2) . . ? C22A C37A C36A 106.7(2) . . ? C38A C37A C36A 134.5(2) . . ? C39A C38A C37A 120.2(2) . . ? C38A C39A C40A 119.2(2) . . ? C38A C39A C53A 122.1(2) . . ? C40A C39A C53A 118.7(2) . . ? C21A C40A C39A 122.3(2) . . ? C42A C41A C1A 175.6(2) . . ? C41A C42A C28A 174.8(2) . . ? C44A C43A C21A 174.4(2) . . ? C43A C44A C8A 179.2(3) . . ? C47A C45A C46A 108.5(2) . . ? C47A C45A C19A 112.5(2) . . ? C46A C45A C19A 109.97(19) . . ? C47A C45A C48A 108.3(2) . . ? C46A C45A C48A 109.3(2) . . ? C19A C45A C48A 108.25(19) . . ? C52A C49A C10A 112.3(2) . . ? C52A C49A C51A 108.1(2) . . ? C10A C49A C51A 110.1(2) . . ? C52A C49A C50A 108.4(2) . . ? C10A C49A C50A 109.7(2) . . ? C51A C49A C50A 108.1(2) . . ? C74A C53A C55A 127.4(5) . . ? C74A C53A C39A 114.0(4) . . ? C55A C53A C39A 115.2(4) . . ? C74A C53A C76A 113.3(5) . . ? C55A C53A C76A 66.7(5) . . ? C39A C53A C76A 108.0(3) . . ? C74A C53A C56A 62.3(4) . . ? C55A C53A C56A 113.9(5) . . ? C39A C53A C56A 110.8(3) . . ? C76A C53A C56A 55.4(3) . . ? C74A C53A C54A 35.4(4) . . ? C55A C53A C54A 111.9(5) . . ? C39A C53A C54A 105.8(3) . . ? C76A C53A C54A 142.6(4) . . ? C56A C53A C54A 97.6(4) . . ? C74A C53A C75A 112.2(5) . . ? C55A C53A C75A 32.4(4) . . ? C39A C53A C75A 109.2(3) . . ? C76A C53A C75A 98.9(4) . . ? C56A C53A C75A 137.6(4) . . ? C54A C53A C75A 84.6(4) . . ? C30A C57A C59A 112.2(2) . . ? C30A C57A C60A 110.4(2) . . ? C59A C57A C60A 108.3(2) . . ? C30A C57A C58A 109.0(2) . . ? C59A C57A C58A 108.2(2) . . ? C60A C57A C58A 108.6(2) . . ? N32A N31A N30A 179.3(3) . . ? C2B C1B C20B 116.0(2) . . ? C2B C1B C41B 120.8(2) . . ? C20B C1B C41B 123.1(2) . . ? N3B C2B C1B 127.6(2) . . ? N3B C2B C17B 109.7(2) . . ? C1B C2B C17B 122.6(2) . . ? C2B N3B C4B 107.6(2) . . ? N3B C4B C5B 129.1(2) . . ? N3B C4B C16B 110.5(2) . . ? C5B C4B C16B 120.4(2) . . ? N6B C5B C4B 130.1(2) . . ? N6B C5B C13B 110.4(2) . . ? C4B C5B C13B 119.4(2) . . ? C5B N6B C7B 108.2(2) . . ? N6B C7B C8B 128.5(2) . . ? N6B C7B C12B 109.7(2) . . ? C8B C7B C12B 121.8(2) . . ? C9B C8B C7B 116.9(2) . . ? C9B C8B C44B 122.3(2) . . ? C7B C8B C44B 120.8(2) . . ? C8B C9B C10B 123.1(2) . . ? C11B C10B C9B 118.6(2) . . ? C11B C10B C49B 123.2(2) . . ? C9B C10B C49B 118.0(2) . . ? C10B C11B C12B 120.2(2) . . ? C11B C12B C7B 119.3(2) . . ? C11B C12B C13B 134.1(2) . . ? C7B C12B C13B 106.5(2) . . ? C14B C13B C5B 119.9(2) . . ? C14B C13B C12B 134.8(2) . . ? C5B C13B C12B 105.1(2) . . ? C15B C14B C13B 120.3(2) . . ? C14B C15B C16B 120.3(2) . . ? C4B C16B C15B 119.7(2) . . ? C4B C16B C17B 105.8(2) . . ? C15B C16B C17B 134.5(2) . . ? C18B C17B C2B 119.0(2) . . ? C18B C17B C16B 134.6(2) . . ? C2B C17B C16B 106.4(2) . . ? C19B C18B C17B 120.3(2) . . ? C18B C19B C20B 118.6(2) . . ? C18B C19B C45B 121.8(2) . . ? C20B C19B C45B 119.5(2) . . ? C1B C20B C19B 123.2(2) . . ? C22B C21B C40B 117.0(2) . . ? C22B C21B C43B 120.0(2) . . ? C40B C21B C43B 122.9(2) . . ? N23B C22B C21B 128.6(2) . . ? N23B C22B C37B 109.5(2) . . ? C21B C22B C37B 121.9(2) . . ? C22B N23B C24B 108.2(2) . . ? N23B C24B C36B 110.6(2) . . ? N23B C24B C25B 129.6(2) . . ? C36B C24B C25B 119.9(2) . . ? N26B C25B C24B 130.5(2) . . ? N26B C25B C33B 110.3(2) . . ? C24B C25B C33B 119.2(2) . . ? C25B N26B C27B 108.3(2) . . ? N26B C27B C28B 128.6(2) . . ? N26B C27B C32B 109.3(2) . . ? C28B C27B C32B 122.1(2) . . ? C27B C28B C29B 116.5(2) . . ? C27B C28B C42B 121.1(2) . . ? C29B C28B C42B 122.5(2) . . ? C30B C29B C28B 122.8(2) . . ? C31B C30B C29B 118.9(2) . . ? C31B C30B C57B 122.3(2) . . ? C29B C30B C57B 118.7(2) . . ? C30B C31B C32B 120.2(2) . . ? C31B C32B C27B 119.3(2) . . ? C31B C32B C33B 133.8(2) . . ? C27B C32B C33B 106.78(19) . . ? C25B C33B C34B 120.5(2) . . ? C25B C33B C32B 105.3(2) . . ? C34B C33B C32B 134.2(2) . . ? C35B C34B C33B 120.1(2) . . ? C34B C35B C36B 119.6(2) . . ? C24B C36B C35B 120.6(2) . . ? C24B C36B C37B 105.48(19) . . ? C35B C36B C37B 133.9(2) . . ? C38B C37B C22B 119.1(2) . . ? C38B C37B C36B 134.6(2) . . ? C22B C37B C36B 106.3(2) . . ? C39B C38B C37B 120.7(2) . . ? C38B C39B C40B 118.6(2) . . ? C38B C39B C53B 120.0(2) . . ? C40B C39B C53B 121.4(2) . . ? C21B C40B C39B 122.7(2) . . ? C42B C41B C1B 173.6(3) . . ? C41B C42B C28B 178.9(3) . . ? C44B C43B C21B 175.5(3) . . ? C43B C44B C8B 174.2(3) . . ? C46B C45B C48B 108.9(3) . . ? C46B C45B C19B 111.8(2) . . ? C48B C45B C19B 109.6(2) . . ? C46B C45B C47B 107.2(3) . . ? C48B C45B C47B 108.5(3) . . ? C19B C45B C47B 110.9(2) . . ? C50B C49B C51B 107.9(2) . . ? C50B C49B C10B 112.7(2) . . ? C51B C49B C10B 108.1(2) . . ? C50B C49B C52B 108.8(2) . . ? C51B C49B C52B 109.6(2) . . ? C10B C49B C52B 109.8(2) . . ? C54B C53B C56B 107.4(2) . . ? C54B C53B C39B 112.9(2) . . ? C56B C53B C39B 110.6(2) . . ? C54B C53B C55B 108.3(2) . . ? C56B C53B C55B 108.7(2) . . ? C39B C53B C55B 108.8(2) . . ? C59B C57B C60B 109.2(2) . . ? C59B C57B C30B 111.6(2) . . ? C60B C57B C30B 110.50(19) . . ? C59B C57B C58B 108.3(2) . . ? C60B C57B C58B 108.7(2) . . ? C30B C57B C58B 108.5(2) . . ? N32B N31B N30B 179.7(3) . . ? C20C C1C C2C 116.2(2) . . ? C20C C1C C41C 122.9(2) . . ? C2C C1C C41C 120.8(2) . . ? N3C C2C C17C 109.5(2) . . ? N3C C2C C1C 128.8(2) . . ? C17C C2C C1C 121.8(2) . . ? C2C N3C C4C 108.6(2) . . ? N3C C4C C5C 130.6(2) . . ? N3C C4C C16C 109.5(2) . . ? C5C C4C C16C 119.9(2) . . ? N6C C5C C4C 130.3(2) . . ? N6C C5C C13C 109.6(2) . . ? C4C C5C C13C 120.1(2) . . ? C7C N6C C5C 108.36(19) . . ? N6C C7C C8C 128.5(2) . . ? N6C C7C C12C 109.6(2) . . ? C8C C7C C12C 121.9(2) . . ? C7C C8C C9C 116.5(2) . . ? C7C C8C C44C 120.7(2) . . ? C9C C8C C44C 122.7(2) . . ? C8C C9C C10C 122.8(2) . . ? C11C C10C C9C 118.9(2) . . ? C11C C10C C49C 120.1(2) . . ? C9C C10C C49C 121.0(2) . . ? C10C C11C C12C 120.1(2) . . ? C11C C12C C7C 119.8(2) . . ? C11C C12C C13C 133.5(2) . . ? C7C C12C C13C 106.59(19) . . ? C5C C13C C14C 119.7(2) . . ? C5C C13C C12C 105.8(2) . . ? C14C C13C C12C 134.5(2) . . ? C15C C14C C13C 120.4(2) . . ? C14C C15C C16C 120.0(2) . . ? C4C C16C C15C 119.9(2) . . ? C4C C16C C17C 106.03(19) . . ? C15C C16C C17C 134.1(2) . . ? C18C C17C C2C 119.7(2) . . ? C18C C17C C16C 133.9(2) . . ? C2C C17C C16C 106.4(2) . . ? C19C C18C C17C 120.2(2) . . ? C18C C19C C20C 118.5(2) . . ? C18C C19C C45C 122.0(2) . . ? C20C C19C C45C 119.5(2) . . ? C1C C20C C19C 123.6(2) . . ? C40C C21C C22C 116.8(2) . . ? C40C C21C C43C 122.7(2) . . ? C22C C21C C43C 120.3(2) . . ? N23C C22C C21C 128.8(2) . . ? N23C C22C C37C 109.59(19) . . ? C21C C22C C37C 121.6(2) . . ? C22C N23C C24C 108.33(19) . . ? N23C C24C C25C 130.0(2) . . ? N23C C24C C36C 110.0(2) . . ? C25C C24C C36C 120.0(2) . . ? N26C C25C C24C 130.1(2) . . ? N26C C25C C33C 110.3(2) . . ? C24C C25C C33C 119.7(2) . . ? C27C N26C C25C 108.03(19) . . ? N26C C27C C28C 128.8(2) . . ? N26C C27C C32C 109.6(2) . . ? C28C C27C C32C 121.6(2) . . ? C27C C28C C29C 116.8(2) . . ? C27C C28C C42C 120.3(2) . . ? C29C C28C C42C 122.8(2) . . ? C28C C29C C30C 122.6(2) . . ? C31C C30C C29C 118.7(2) . . ? C31C C30C C57C 122.4(2) . . ? C29C C30C C57C 118.8(2) . . ? C30C C31C C32C 120.3(2) . . ? C31C C32C C27C 119.6(2) . . ? C31C C32C C33C 133.8(2) . . ? C27C C32C C33C 106.52(19) . . ? C25C C33C C34C 120.1(2) . . ? C25C C33C C32C 105.5(2) . . ? C34C C33C C32C 134.4(2) . . ? C35C C34C C33C 120.2(2) . . ? C34C C35C C36C 119.9(2) . . ? C24C C36C C35C 120.0(2) . . ? C24C C36C C37C 105.84(19) . . ? C35C C36C C37C 134.2(2) . . ? C38C C37C C22C 119.5(2) . . ? C38C C37C C36C 134.2(2) . . ? C22C C37C C36C 106.3(2) . . ? C37C C38C C39C 120.4(2) . . ? C38C C39C C40C 118.4(2) . . ? C38C C39C C53C 119.6(2) . . ? C40C C39C C53C 122.0(2) . . ? C21C C40C C39C 123.2(2) . . ? C42C C41C C1C 177.1(3) . . ? C41C C42C C28C 173.8(2) . . ? C44C C43C C21C 174.2(3) . . ? C43C C44C C8C 174.9(3) . . ? C48C C45C C47C 108.9(3) . . ? C48C C45C C46C 110.6(4) . . ? C47C C45C C46C 106.0(3) . . ? C48C C45C C19C 108.8(3) . . ? C47C C45C C19C 112.8(2) . . ? C46C C45C C19C 109.8(3) . . ? C52C C49C C50C 108.3(2) . . ? C52C C49C C51C 108.0(2) . . ? C50C C49C C51C 109.3(2) . . ? C52C C49C C10C 111.4(2) . . ? C50C C49C C10C 108.2(2) . . ? C51C C49C C10C 111.6(2) . . ? C54C C53C C55C 107.7(2) . . ? C54C C53C C56C 109.0(2) . . ? C55C C53C C56C 107.1(2) . . ? C54C C53C C39C 110.4(2) . . ? C55C C53C C39C 113.1(2) . . ? C56C C53C C39C 109.4(2) . . ? C60C C57C C59C 108.0(2) . . ? C60C C57C C58C 108.1(2) . . ? C59C C57C C58C 109.4(2) . . ? C60C C57C C30C 111.9(2) . . ? C59C C57C C30C 109.1(2) . . ? C58C C57C C30C 110.30(19) . . ? N32C N31C N30C 179.1(3) . . ? C13X N1X C1X 111.18(19) . . ? C13X N1X C9X 106.77(17) . . ? C1X N1X C9X 110.74(19) . . ? C13X N1X C5X 111.1(2) . . ? C1X N1X C5X 107.47(18) . . ? C9X N1X C5X 109.62(19) . . ? N1X C1X C2X 114.5(2) . . ? C3X C2X C1X 112.7(2) . . ? C4X C3X C2X 112.7(2) . . ? C6X C5X N1X 116.1(2) . . ? C5X C6X C7X 111.2(2) . . ? C8X C7X C6X 112.1(3) . . ? C10X C9X N1X 115.5(2) . . ? C9X C10X C11X 110.8(2) . . ? C12X C11X C10X 114.2(2) . . ? N1X C13X C14X 114.14(19) . . ? C15X C14X C13X 111.3(2) . . ? C16X C15X C14X 114.7(2) . . ? C13Y N1Y C5Y 111.30(19) . . ? C13Y N1Y C9Y 106.12(19) . . ? C5Y N1Y C9Y 110.8(2) . . ? C13Y N1Y C1Y 111.5(2) . . ? C5Y N1Y C1Y 106.29(18) . . ? C9Y N1Y C1Y 110.90(19) . . ? N1Y C1Y C2Y 115.7(2) . . ? C3Y C2Y C1Y 110.3(2) . . ? C4Y C3Y C2Y 113.0(3) . . ? N1Y C5Y C6Y 115.6(2) . . ? C7Y C6Y C5Y 111.0(2) . . ? C8Y C7Y C6Y 115.9(2) . . ? C10Y C9Y N1Y 116.0(2) . . ? C11Y C10Y C9Y 110.3(2) . . ? C10Y C11Y C12Y 113.6(2) . . ? N1Y C13Y C14Y 115.6(2) . . ? C15Y C14Y C13Y 111.3(2) . . ? C16Y C15Y C14Y 114.3(3) . . ? C13Z N1Z C1Z 111.49(19) . . ? C13Z N1Z C9Z 106.17(18) . . ? C1Z N1Z C9Z 111.46(19) . . ? C13Z N1Z C5Z 111.08(19) . . ? C1Z N1Z C5Z 106.24(18) . . ? C9Z N1Z C5Z 110.48(19) . . ? C2Z C1Z N1Z 115.7(2) . . ? C3Z C2Z C1Z 110.5(2) . . ? C2Z C3Z C4Z 113.9(2) . . ? C6Z C5Z N1Z 115.6(2) . . ? C5Z C6Z C7Z 111.2(2) . . ? C8Z C7Z C6Z 112.1(3) . . ? N1Z C9Z C10Z 115.9(2) . . ? C11Z C10Z C9Z 110.2(2) . . ? C12Z C11Z C10Z 113.8(2) . . ? C14Z C13Z N1Z 115.0(2) . . ? C13Z C14Z C15Z 112.3(2) . . ? C16Z C15Z C14Z 114.4(2) . . ? C2S O1S C3S 109.6(5) . . ? O1S C2S C1S 107.9(4) . . ? C4S C3S O1S 109.5(4) . . ? C32S O12S C22S 119(4) . . ? C12S C22S O12S 134(2) . . ? C12S C22S C32S 125.5(19) . . ? O12S C22S C32S 19.0(12) . . ? O12S C32S C42S 119(3) . . ? O12S C32S C22S 42(3) . . ? C42S C32S C22S 91.3(14) . . ? C72S O2S C7S 44.3(8) . . ? C72S O2S C6S 148.8(9) . . ? C7S O2S C6S 106.6(4) . . ? O2S C6S C5S 104.7(4) . . ? O2S C7S C8S 104.4(6) . . ? O2S C72S C82S 167.7(17) . . ? C10S O3S C11S 116.1(5) . . ? O3S C10S C9S 109.1(7) . . ? O3S C11S C11S 112.0(6) . 2_576 ? C142 O4S C131 136.9(17) . . ? C121 C131 O4S 104.3(9) . . ? C152 C141 C151 104(3) . . ? C141 C151 C152 35.1(16) . . ? C141 C152 C151 41(2) . . ? O4S C142 C153 100(2) . . ? 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 N3A H3A N30A 0.91(3) 2.12(3) 2.920(3) 146(2) . N3A H3A N31A 0.91(3) 2.49(3) 3.102(3) 125(2) . N6A H6A N30A 0.90(3) 2.14(3) 2.961(3) 152(2) . N6A H6A N31A 0.90(3) 2.70(3) 3.370(3) 132(2) . N23A H23A N30A 0.86(3) 2.16(3) 2.917(3) 146(3) . N26A H26A N30A 0.97(3) 2.01(3) 2.886(3) 148(3) . N3B H3B N30B 1.02(3) 2.01(3) 2.908(3) 146(2) . N6B H6B N30B 0.89(3) 2.06(3) 2.906(3) 157(3) . N23B H23B N30B 0.85(2) 2.19(2) 2.951(3) 148(2) . N23B H23B N31B 0.85(2) 2.57(2) 3.148(3) 126.2(18) . N26B H26B N30B 0.86(3) 2.22(3) 2.945(3) 142(2) . N26B H26B N31B 0.86(3) 2.63(3) 3.158(3) 120(2) . N3C H3C N30C 0.87(2) 2.17(2) 2.934(3) 147(2) . N6C H6C N30C 0.89(3) 2.13(3) 2.916(3) 147(2) . N6C H6C N31C 0.89(3) 2.57(3) 3.226(3) 131(2) . N23C H23C N30C 0.92(3) 2.01(3) 2.898(3) 160(3) . N26C H26C N30C 0.90(3) 2.11(3) 2.935(3) 153(3) . _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.696 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.053 # Attachment 'CIF_2+N3_revised.CIF' data_p6_13mo _database_code_depnum_ccdc_archive 'CCDC 643422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H102 N8' _chemical_formula_weight 1199.72 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.459(4) _cell_length_b 17.029(3) _cell_length_c 12.014(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.43(3) _cell_angle_gamma 90.00 _cell_volume 3673.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 10687 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 24.30 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9874 _exptl_absorpt_correction_T_max 0.9968 _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.70000 _diffrn_radiation_type synchrotron _diffrn_radiation_source PAL _diffrn_radiation_monochromator 'Silicon double crystal monochromator' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10687 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.30 _reflns_number_total 5867 _reflns_number_gt 4505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.1746P)^2^+3.5962P] 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 0.037(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5867 _refine_ls_number_parameters 429 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2885 _refine_ls_wR_factor_gt 0.2671 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.72074(16) 0.38343(19) 0.8361(2) 0.0319(7) Uani 1 1 d . . . C2 C 0.65284(15) 0.34691(18) 0.7872(2) 0.0294(7) Uani 1 1 d . . . N3 N 0.58446(13) 0.35788(16) 0.8128(2) 0.0296(6) Uani 1 1 d . . . H3 H 0.5747(17) 0.387(2) 0.861(3) 0.028(9) Uiso 1 1 d . . . C4 C 0.53294(16) 0.31193(19) 0.7385(2) 0.0315(7) Uani 1 1 d . . . C5 C 0.45554(16) 0.30837(19) 0.7223(2) 0.0330(8) Uani 1 1 d . . . N6 N 0.40909(13) 0.35039(17) 0.7756(2) 0.0316(6) Uani 1 1 d . . . H6 H 0.423(2) 0.390(2) 0.823(3) 0.051(11) Uiso 1 1 d . . . C7 C 0.33661(16) 0.3317(2) 0.7221(3) 0.0336(7) Uani 1 1 d . . . C8 C 0.27046(16) 0.3617(2) 0.7435(3) 0.0363(8) Uani 1 1 d . . . C9 C 0.20365(17) 0.3351(2) 0.6724(3) 0.0446(9) Uani 1 1 d . . . H9 H 0.1581 0.3551 0.6847 0.054 Uiso 1 1 calc R . . C10 C 0.20078(18) 0.2810(3) 0.5849(3) 0.0506(10) Uani 1 1 d . . . C11 C 0.26800(18) 0.2508(3) 0.5674(3) 0.0498(10) Uani 1 1 d . . . H11 H 0.2672 0.2129 0.5090 0.060 Uiso 1 1 calc R . . C12 C 0.33629(17) 0.2761(2) 0.6354(3) 0.0396(8) Uani 1 1 d . . . C13 C 0.41369(17) 0.2608(2) 0.6361(3) 0.0394(8) Uani 1 1 d . . . C14 C 0.45011(18) 0.2134(2) 0.5680(3) 0.0464(9) Uani 1 1 d . . . H14 H 0.4219 0.1788 0.5124 0.056 Uiso 1 1 calc R . . C15 C 0.52589(18) 0.2179(2) 0.5826(3) 0.0453(9) Uani 1 1 d . . . H15 H 0.5501 0.1871 0.5361 0.054 Uiso 1 1 calc R . . C16 C 0.56819(17) 0.2684(2) 0.6669(3) 0.0370(8) Uani 1 1 d . . . C17 C 0.64602(16) 0.2921(2) 0.6974(3) 0.0340(8) Uani 1 1 d . . . C18 C 0.70847(17) 0.2736(2) 0.6555(3) 0.0396(8) Uani 1 1 d . . . H18 H 0.7044 0.2366 0.5951 0.047 Uiso 1 1 calc R . . C19 C 0.77701(17) 0.3094(2) 0.7019(3) 0.0381(8) Uani 1 1 d . A . C20 C 0.78177(16) 0.3628(2) 0.7916(3) 0.0358(8) Uani 1 1 d . . . H20 H 0.8286 0.3863 0.8238 0.043 Uiso 1 1 calc R . . C21 C 0.84757(18) 0.2909(3) 0.6590(3) 0.0520(10) Uani 1 1 d D . . C22 C 0.8762(3) 0.3706(3) 0.6141(5) 0.0567(16) Uani 0.788(8) 1 d P A 1 H22A H 0.9196 0.3596 0.5826 0.085 Uiso 0.788(8) 1 calc PR A 1 H22B H 0.8903 0.4077 0.6778 0.085 Uiso 0.788(8) 1 calc PR A 1 H22C H 0.8364 0.3934 0.5544 0.085 Uiso 0.788(8) 1 calc PR A 1 C23 C 0.9073(2) 0.2609(4) 0.7538(4) 0.0583(19) Uani 0.788(8) 1 d P A 1 H23A H 0.8899 0.2135 0.7859 0.087 Uiso 0.788(8) 1 calc PR A 1 H23B H 0.9202 0.3011 0.8135 0.087 Uiso 0.788(8) 1 calc PR A 1 H23C H 0.9513 0.2482 0.7248 0.087 Uiso 0.788(8) 1 calc PR A 1 C24 C 0.8327(2) 0.2377(4) 0.5562(4) 0.0424(14) Uani 0.788(8) 1 d P A 1 H24A H 0.7945 0.2612 0.4949 0.064 Uiso 0.788(8) 1 calc PR A 1 H24B H 0.8153 0.1866 0.5770 0.064 Uiso 0.788(8) 1 calc PR A 1 H24C H 0.8787 0.2306 0.5298 0.064 Uiso 0.788(8) 1 calc PR A 1 C52 C 0.8607(18) 0.1980(11) 0.705(3) 0.098(9) Uiso 0.212(8) 1 d PD A 2 H52A H 0.8162 0.1669 0.6729 0.147 Uiso 0.212(8) 1 calc PR A 2 H52B H 0.8701 0.1971 0.7892 0.147 Uiso 0.212(8) 1 calc PR A 2 H52C H 0.9036 0.1757 0.6815 0.147 Uiso 0.212(8) 1 calc PR A 2 C53 C 0.9177(11) 0.3223(15) 0.7291(18) 0.059(6) Uiso 0.212(8) 1 d P A 2 H53A H 0.9598 0.3004 0.7024 0.089 Uiso 0.212(8) 1 calc PR A 2 H53B H 0.9222 0.3078 0.8093 0.089 Uiso 0.212(8) 1 calc PR A 2 H53C H 0.9179 0.3796 0.7221 0.089 Uiso 0.212(8) 1 calc PR A 2 C54 C 0.8359(14) 0.2850(19) 0.546(2) 0.068(7) Uiso 0.212(8) 1 d P A 2 H54A H 0.8804 0.2634 0.5261 0.102 Uiso 0.212(8) 1 calc PR A 2 H54B H 0.8253 0.3372 0.5116 0.102 Uiso 0.212(8) 1 calc PR A 2 H54C H 0.7934 0.2502 0.5173 0.102 Uiso 0.212(8) 1 calc PR A 2 C25 C 0.1239(2) 0.2571(3) 0.5112(4) 0.0681(14) Uani 1 1 d . . . C26 C 0.0838(3) 0.3334(4) 0.4505(5) 0.109(2) Uani 1 1 d . . . H26A H 0.1123 0.3544 0.3978 0.163 Uiso 1 1 calc R . . H26B H 0.0809 0.3730 0.5084 0.163 Uiso 1 1 calc R . . H26C H 0.0335 0.3198 0.4076 0.163 Uiso 1 1 calc R . . C27 C 0.0744(2) 0.2298(4) 0.5832(4) 0.096(2) Uani 1 1 d . . . H27A H 0.0259 0.2155 0.5345 0.144 Uiso 1 1 calc R . . H27B H 0.0678 0.2719 0.6356 0.144 Uiso 1 1 calc R . . H27C H 0.0965 0.1839 0.6274 0.144 Uiso 1 1 calc R . . C28 C 0.1288(2) 0.2041(3) 0.4173(4) 0.0754(15) Uani 1 1 d . . . H28A H 0.1497 0.1537 0.4487 0.113 Uiso 1 1 calc R . . H28B H 0.1611 0.2274 0.3719 0.113 Uiso 1 1 calc R . . H28C H 0.0789 0.1958 0.3685 0.113 Uiso 1 1 calc R . . C29 C 0.72503(15) 0.4384(2) 0.9267(3) 0.0328(7) Uani 1 1 d . . . C30 C 0.72451(15) 0.48434(19) 1.0035(3) 0.0328(8) Uani 1 1 d . . . C31 C 0.27181(15) 0.4168(2) 0.8329(3) 0.0348(8) Uani 1 1 d . . . C32 C 0.27431(16) 0.4631(2) 0.9100(3) 0.0337(8) Uani 1 1 d . . . N1A N 0.5000 0.5000 1.0000 0.0462(11) Uani 1 2 d S . . N2A N 0.50063(15) 0.4653(2) 0.9145(3) 0.0549(9) Uani 1 1 d . . . N1T N 0.5000 0.5000 0.5000 0.0700(15) Uani 1 2 d S . . C1T C 0.4473(5) 0.5072(5) 0.3777(7) 0.060(2) Uiso 0.50 1 d P B 1 H1T1 H 0.4196 0.5572 0.3753 0.072 Uiso 0.50 1 calc PR B 1 H1T2 H 0.4793 0.5123 0.3224 0.072 Uiso 0.50 1 calc PR B 1 C2T C 0.3913(6) 0.4439(6) 0.3339(10) 0.058(3) Uiso 0.50 1 d P B 1 H2T1 H 0.4138 0.3931 0.3633 0.070 Uiso 0.50 1 calc PR B 1 H2T2 H 0.3832 0.4424 0.2495 0.070 Uiso 0.50 1 calc PR B 1 C3T C 0.3122(5) 0.4492(6) 0.3633(8) 0.070(2) Uiso 0.50 1 d P B 1 H3T1 H 0.3178 0.4346 0.4446 0.084 Uiso 0.50 1 calc PR B 1 H3T2 H 0.2954 0.5045 0.3548 0.084 Uiso 0.50 1 calc PR B 1 C4T C 0.2517(8) 0.3980(8) 0.2909(12) 0.086(4) Uiso 0.50 1 d P B 1 C5T C 0.4545(5) 0.4862(5) 0.5861(8) 0.061(2) Uiso 0.50 1 d P B 2 H5T1 H 0.4209 0.4410 0.5611 0.073 Uiso 0.50 1 calc PR B 2 H5T2 H 0.4881 0.4724 0.6604 0.073 Uiso 0.50 1 calc PR B 2 C6T C 0.4093(4) 0.5556(5) 0.6021(6) 0.0454(17) Uiso 0.50 1 d P B 2 H6T1 H 0.4431 0.5987 0.6366 0.055 Uiso 0.50 1 calc PR B 2 H6T2 H 0.3805 0.5736 0.5264 0.055 Uiso 0.50 1 calc PR B 2 C7T C 0.3577(5) 0.5391(5) 0.6752(8) 0.061(2) Uiso 0.50 1 d P B 2 H7T1 H 0.3865 0.5332 0.7552 0.074 Uiso 0.50 1 calc PR B 2 H7T2 H 0.3322 0.4886 0.6513 0.074 Uiso 0.50 1 calc PR B 2 C8T C 0.2992(8) 0.6031(8) 0.6704(12) 0.058(4) Uiso 0.50 1 d P B 2 C9T C 0.5511(5) 0.5660(6) 0.5196(8) 0.069(2) Uiso 0.50 1 d P B 3 H9T1 H 0.5216 0.6149 0.5161 0.083 Uiso 0.50 1 calc PR B 3 H9T2 H 0.5772 0.5679 0.4564 0.083 Uiso 0.50 1 calc PR B 3 C10T C 0.6069(10) 0.5649(11) 0.6280(15) 0.112(6) Uiso 0.50 1 d P B 3 H10A H 0.5816 0.5740 0.6910 0.134 Uiso 0.50 1 calc PR B 3 H10B H 0.6296 0.5120 0.6389 0.134 Uiso 0.50 1 calc PR B 3 C11T C 0.6644(6) 0.6210(7) 0.6367(10) 0.083(3) Uiso 0.50 1 d P B 3 H11A H 0.6417 0.6736 0.6373 0.100 Uiso 0.50 1 calc PR B 3 H11B H 0.6830 0.6175 0.5660 0.100 Uiso 0.50 1 calc PR B 3 C12T C 0.7306(9) 0.6174(9) 0.7360(14) 0.103(5) Uiso 0.50 1 d P B 3 C13T C 0.5400(5) 0.4158(6) 0.4937(8) 0.070(2) Uiso 0.50 1 d P B 4 H13A H 0.5768 0.4080 0.5672 0.084 Uiso 0.50 1 calc PR B 4 H13B H 0.5016 0.3746 0.4886 0.084 Uiso 0.50 1 calc PR B 4 C14T C 0.5797(6) 0.4012(8) 0.3979(10) 0.083(3) Uiso 0.50 1 d P B 4 H14A H 0.5789 0.3440 0.3836 0.099 Uiso 0.50 1 calc PR B 4 H14B H 0.5497 0.4263 0.3278 0.099 Uiso 0.50 1 calc PR B 4 C15T C 0.6524(10) 0.4265(10) 0.4117(16) 0.134(5) Uiso 0.50 1 d P B 4 H15A H 0.6827 0.4075 0.4859 0.161 Uiso 0.50 1 calc PR B 4 H15B H 0.6538 0.4846 0.4123 0.161 Uiso 0.50 1 calc PR B 4 C16T C 0.6889(9) 0.3925(10) 0.3043(14) 0.082(6) Uiso 0.50 1 d P B 4 C1H C 0.9124(10) 0.0224(10) 0.8559(14) 0.138(5) Uiso 0.50 1 d PD C -1 C2H C 0.9453(7) 0.0027(8) 0.7637(10) 0.099(4) Uiso 0.50 1 d PD C -1 H2H1 H 0.9992 0.0059 0.7999 0.119 Uiso 0.50 1 calc PR C -1 H2H2 H 0.9347 -0.0542 0.7542 0.119 Uiso 0.50 1 calc PR C -1 C3H C 0.9431(8) 0.0248(9) 0.6592(11) 0.115(4) Uiso 0.50 1 d PD C -1 H3H1 H 0.9438 0.0830 0.6588 0.138 Uiso 0.50 1 calc PR C -1 H3H2 H 0.8943 0.0084 0.6115 0.138 Uiso 0.50 1 calc PR C -1 C4H C 1.0006(6) -0.0020(7) 0.6008(8) 0.084(3) Uiso 0.50 1 d PD C -1 H4H1 H 1.0067 -0.0593 0.6139 0.101 Uiso 0.50 1 calc PR C -1 H4H2 H 1.0482 0.0229 0.6400 0.101 Uiso 0.50 1 calc PR C -1 C5H C 0.9905(10) 0.0123(12) 0.4716(11) 0.124(5) Uiso 0.50 1 d PD C -1 H5H1 H 0.9858 0.0693 0.4555 0.149 Uiso 0.50 1 calc PR C -1 H5H2 H 0.9444 -0.0137 0.4292 0.149 Uiso 0.50 1 calc PR C -1 C6H C 1.0585(10) -0.0210(11) 0.4312(16) 0.139(6) Uiso 0.50 1 d PD C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0242(15) 0.0428(19) 0.0281(15) 0.0003(13) 0.0046(12) 0.0035(13) C2 0.0217(14) 0.0399(18) 0.0272(15) 0.0025(13) 0.0066(11) 0.0027(12) N3 0.0238(13) 0.0403(16) 0.0258(13) -0.0038(12) 0.0083(10) 0.0006(11) C4 0.0241(15) 0.0443(19) 0.0265(15) -0.0033(13) 0.0065(12) -0.0012(13) C5 0.0257(15) 0.049(2) 0.0263(15) -0.0027(13) 0.0093(12) -0.0032(13) N6 0.0208(12) 0.0472(17) 0.0274(13) -0.0064(12) 0.0066(10) -0.0032(11) C7 0.0250(15) 0.049(2) 0.0272(15) -0.0033(14) 0.0077(12) -0.0063(13) C8 0.0257(15) 0.057(2) 0.0283(16) -0.0052(14) 0.0099(12) -0.0055(14) C9 0.0241(16) 0.074(3) 0.0375(18) -0.0141(17) 0.0108(13) -0.0053(15) C10 0.0271(17) 0.087(3) 0.0385(19) -0.0229(19) 0.0096(14) -0.0113(17) C11 0.0291(17) 0.082(3) 0.0410(19) -0.0262(18) 0.0133(15) -0.0124(17) C12 0.0275(16) 0.061(2) 0.0329(17) -0.0111(15) 0.0116(13) -0.0074(15) C13 0.0266(16) 0.057(2) 0.0351(17) -0.0097(15) 0.0087(13) -0.0053(14) C14 0.0311(17) 0.069(2) 0.0401(18) -0.0217(17) 0.0102(14) -0.0070(16) C15 0.0328(17) 0.063(2) 0.0409(19) -0.0192(17) 0.0114(14) -0.0007(16) C16 0.0256(16) 0.053(2) 0.0333(17) -0.0052(15) 0.0077(13) 0.0007(14) C17 0.0246(15) 0.047(2) 0.0301(15) -0.0030(14) 0.0062(12) 0.0016(13) C18 0.0268(16) 0.056(2) 0.0362(17) -0.0100(15) 0.0072(13) 0.0043(14) C19 0.0245(16) 0.054(2) 0.0360(17) -0.0055(15) 0.0076(13) 0.0033(14) C20 0.0199(15) 0.053(2) 0.0340(17) -0.0029(14) 0.0060(12) 0.0005(13) C21 0.0269(17) 0.083(3) 0.048(2) -0.023(2) 0.0132(15) 0.0016(17) C22 0.045(3) 0.072(4) 0.063(3) -0.013(3) 0.031(2) -0.012(2) C23 0.024(2) 0.109(5) 0.041(3) -0.012(3) 0.0053(19) 0.023(3) C24 0.025(2) 0.066(4) 0.039(2) -0.014(2) 0.0117(17) 0.005(2) C25 0.0282(19) 0.123(4) 0.053(2) -0.039(2) 0.0089(17) -0.011(2) C26 0.072(4) 0.122(5) 0.106(4) -0.016(4) -0.034(3) 0.012(3) C27 0.042(2) 0.186(6) 0.064(3) -0.056(3) 0.021(2) -0.053(3) C28 0.032(2) 0.130(4) 0.060(3) -0.044(3) 0.0029(18) -0.008(2) C29 0.0182(14) 0.047(2) 0.0326(16) -0.0005(15) 0.0052(11) 0.0003(12) C30 0.0184(14) 0.047(2) 0.0331(17) -0.0003(16) 0.0054(12) -0.0010(12) C31 0.0215(15) 0.052(2) 0.0314(16) -0.0023(15) 0.0079(12) -0.0042(13) C32 0.0224(15) 0.047(2) 0.0318(17) -0.0015(16) 0.0074(12) -0.0024(13) N1A 0.026(2) 0.047(3) 0.063(3) 0.000(2) 0.0043(18) -0.0006(17) N2A 0.0295(15) 0.077(2) 0.058(2) -0.0413(19) 0.0091(13) -0.0012(14) N1T 0.058(3) 0.092(4) 0.061(3) 0.028(3) 0.017(2) 0.015(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 C1 C20 1.400(4) . ? C1 C2 1.400(4) . ? C1 C29 1.423(4) . ? C2 N3 1.380(4) . ? C2 C17 1.410(4) . ? N3 C4 1.385(4) . ? C4 C5 1.398(4) . ? C4 C16 1.405(4) . ? C5 N6 1.383(4) . ? C5 C13 1.398(4) . ? N6 C7 1.380(4) . ? C7 C8 1.401(4) . ? C7 C12 1.408(5) . ? C8 C9 1.402(4) . ? C8 C31 1.423(5) . ? C9 C10 1.391(5) . ? C10 C11 1.403(5) . ? C10 C25 1.542(5) . ? C11 C12 1.401(5) . ? C12 C13 1.450(4) . ? C13 C14 1.424(5) . ? C14 C15 1.371(5) . ? C15 C16 1.416(5) . ? C16 C17 1.455(4) . ? C17 C18 1.397(4) . ? C18 C19 1.399(5) . ? C19 C20 1.397(5) . ? C19 C21 1.541(4) . ? C21 C54 1.33(2) . ? C21 C53 1.47(2) . ? C21 C23 1.480(6) . ? C21 C24 1.505(6) . ? C21 C22 1.596(7) . ? C21 C52 1.676(17) . ? C25 C28 1.464(6) . ? C25 C27 1.472(6) . ? C25 C26 1.586(8) . ? C29 C30 1.212(4) . ? C30 C32 1.367(5) 3_667 ? C31 C32 1.209(4) . ? C32 C30 1.367(5) 3_667 ? N1A N2A 1.187(3) 3_667 ? N1A N2A 1.187(3) . ? N1T C9T 1.450(10) . ? N1T C9T 1.450(10) 3_666 ? N1T C5T 1.495(9) 3_666 ? N1T C5T 1.495(9) . ? N1T C1T 1.568(8) . ? N1T C1T 1.568(8) 3_666 ? N1T C13T 1.623(9) . ? N1T C13T 1.623(9) 3_666 ? C1T C2T 1.502(14) . ? C2T C3T 1.582(14) . ? C3T C4T 1.521(16) . ? C5T C6T 1.484(12) . ? C6T C7T 1.464(12) . ? C7T C8T 1.527(16) . ? C9T C10T 1.462(19) . ? C10T C11T 1.41(2) . ? C11T C12T 1.497(18) . ? C13T C14T 1.521(14) . ? C14T C15T 1.383(19) . ? C15T C16T 1.69(2) . ? C1H C2H 1.422(14) . ? C2H C3H 1.302(13) . ? C3H C4H 1.475(13) . ? C4H C5H 1.540(14) . ? C5H C6H 1.553(16) . ? 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 C20 C1 C2 116.7(3) . . ? C20 C1 C29 123.4(3) . . ? C2 C1 C29 119.9(3) . . ? N3 C2 C1 128.5(3) . . ? N3 C2 C17 109.7(3) . . ? C1 C2 C17 121.8(3) . . ? C2 N3 C4 107.9(3) . . ? N3 C4 C5 129.9(3) . . ? N3 C4 C16 110.3(3) . . ? C5 C4 C16 119.7(3) . . ? N6 C5 C4 129.6(3) . . ? N6 C5 C13 110.3(3) . . ? C4 C5 C13 120.0(3) . . ? C7 N6 C5 107.7(3) . . ? N6 C7 C8 128.5(3) . . ? N6 C7 C12 109.7(3) . . ? C8 C7 C12 121.8(3) . . ? C7 C8 C9 116.9(3) . . ? C7 C8 C31 121.0(3) . . ? C9 C8 C31 122.1(3) . . ? C10 C9 C8 123.2(3) . . ? C9 C10 C11 118.4(3) . . ? C9 C10 C25 118.5(3) . . ? C11 C10 C25 123.1(3) . . ? C12 C11 C10 120.5(3) . . ? C11 C12 C7 119.1(3) . . ? C11 C12 C13 134.4(3) . . ? C7 C12 C13 106.4(3) . . ? C5 C13 C14 120.1(3) . . ? C5 C13 C12 105.9(3) . . ? C14 C13 C12 134.0(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 120.2(3) . . ? C4 C16 C15 120.1(3) . . ? C4 C16 C17 105.7(3) . . ? C15 C16 C17 134.1(3) . . ? C18 C17 C2 119.4(3) . . ? C18 C17 C16 134.1(3) . . ? C2 C17 C16 106.5(3) . . ? C17 C18 C19 120.2(3) . . ? C20 C19 C18 118.7(3) . . ? C20 C19 C21 119.0(3) . . ? C18 C19 C21 122.2(3) . . ? C19 C20 C1 123.1(3) . . ? C54 C21 C53 121.6(15) . . ? C54 C21 C23 132.5(12) . . ? C53 C21 C23 44.4(9) . . ? C54 C21 C24 32.9(12) . . ? C53 C21 C24 131.1(9) . . ? C23 C21 C24 112.7(4) . . ? C54 C21 C19 114.1(11) . . ? C53 C21 C19 115.7(9) . . ? C23 C21 C19 110.5(3) . . ? C24 C21 C19 113.0(3) . . ? C54 C21 C22 72.9(14) . . ? C53 C21 C22 64.3(10) . . ? C23 C21 C22 107.9(4) . . ? C24 C21 C22 104.3(4) . . ? C19 C21 C22 108.1(3) . . ? C54 C21 C52 104.3(17) . . ? C53 C21 C52 96.4(15) . . ? C23 C21 C52 52.7(11) . . ? C24 C21 C52 71.9(11) . . ? C19 C21 C52 98.7(11) . . ? C22 C21 C52 151.8(11) . . ? C28 C25 C27 114.6(4) . . ? C28 C25 C10 113.0(3) . . ? C27 C25 C10 111.1(3) . . ? C28 C25 C26 104.8(4) . . ? C27 C25 C26 104.0(5) . . ? C10 C25 C26 108.5(4) . . ? C30 C29 C1 176.3(3) . . ? C29 C30 C32 178.5(3) . 3_667 ? C32 C31 C8 178.7(3) . . ? C31 C32 C30 178.7(3) . 3_667 ? N2A N1A N2A 180.000(1) 3_667 . ? C9T N1T C9T 180.000(2) . 3_666 ? C9T N1T C5T 62.7(5) . 3_666 ? C9T N1T C5T 117.3(5) 3_666 3_666 ? C9T N1T C5T 117.3(5) . . ? C9T N1T C5T 62.7(5) 3_666 . ? C5T N1T C5T 180.0(7) 3_666 . ? C9T N1T C1T 109.3(5) . . ? C9T N1T C1T 70.7(5) 3_666 . ? C5T N1T C1T 70.4(5) 3_666 . ? C5T N1T C1T 109.6(5) . . ? C9T N1T C1T 70.7(5) . 3_666 ? C9T N1T C1T 109.3(5) 3_666 3_666 ? C5T N1T C1T 109.6(5) 3_666 3_666 ? C5T N1T C1T 70.4(5) . 3_666 ? C1T N1T C1T 180.000(2) . 3_666 ? C9T N1T C13T 114.0(5) . . ? C9T N1T C13T 66.0(5) 3_666 . ? C5T N1T C13T 76.8(5) 3_666 . ? C5T N1T C13T 103.2(5) . . ? C1T N1T C13T 102.4(5) . . ? C1T N1T C13T 77.6(5) 3_666 . ? C9T N1T C13T 66.0(5) . 3_666 ? C9T N1T C13T 114.0(5) 3_666 3_666 ? C5T N1T C13T 103.2(5) 3_666 3_666 ? C5T N1T C13T 76.8(5) . 3_666 ? C1T N1T C13T 77.6(5) . 3_666 ? C1T N1T C13T 102.4(5) 3_666 3_666 ? C13T N1T C13T 180.0(7) . 3_666 ? C2T C1T N1T 119.9(7) . . ? C1T C2T C3T 118.5(8) . . ? C4T C3T C2T 115.6(9) . . ? C6T C5T N1T 112.8(6) . . ? C7T C6T C5T 112.9(7) . . ? C6T C7T C8T 113.1(8) . . ? N1T C9T C10T 115.6(10) . . ? C11T C10T C9T 114.8(14) . . ? C10T C11T C12T 119.4(12) . . ? C14T C13T N1T 118.9(8) . . ? C15T C14T C13T 118.9(12) . . ? C14T C15T C16T 110.5(13) . . ? C3H C2H C1H 139.4(14) . . ? C2H C3H C4H 120.3(12) . . ? C3H C4H C5H 119.9(11) . . ? C4H C5H C6H 109.9(11) . . ? 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 N6 H6 N2A 0.87(4) 2.05(4) 2.856(4) 153(3) . N3 H3 N2A 0.82(4) 2.11(4) 2.848(4) 150(3) . _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 24.30 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.905 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.087