#------------------------------------------------------------------------------ #$Date: 2021-11-03 00:56:17 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270210 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/91/7129180.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7129180 loop_ _publ_author_name 'Zhou, Yibin' 'Tang, Hao' 'Li, Zhao-Hui' 'Xu, Linxian' 'Wang, Lingyun' 'Cao, Derong' _publ_section_title ; Bio-inspired AIE pillar[5]arene probe with multiple binding sites to discriminate alkanediamines ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D1CC05153A _journal_year 2021 _chemical_formula_sum 'C69 H67 N3 O13 S' _chemical_formula_weight 1178.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2021-08-31 deposited with the CCDC. 2021-11-01 downloaded from the CCDC. ; _cell_angle_alpha 75.891(2) _cell_angle_beta 82.879(2) _cell_angle_gamma 68.192(2) _cell_formula_units_Z 2 _cell_length_a 12.7652(9) _cell_length_b 16.0114(13) _cell_length_c 16.5435(12) _cell_measurement_reflns_used 6168 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 51.896 _cell_measurement_theta_min 5.082 _cell_volume 3042.5(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_unetI/netI 0.0869 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 56680 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.085 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.286 _exptl_crystal_description prismatic _exptl_crystal_F_000 1244 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.070 _refine_diff_density_max 0.339 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 804 _refine_ls_number_reflns 10699 _refine_ls_number_restraints 598 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0932 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+5.8170P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1741 _refine_ls_wR_factor_ref 0.2271 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5107 _reflns_number_total 10699 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc05153a2.cif _cod_data_source_block mo_dd20011_0m _cod_database_code 7129180 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.982 _shelx_estimated_absorpt_t_max 0.992 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_dd20011_0m_a.res in P-1 CELL 0.71073 12.7652 16.0114 16.5435 75.891 82.879 68.192 ZERR 2 0.0009 0.0013 0.0012 0.002 0.002 0.002 LATT 1 SFAC C H N O S UNIT 138 134 6 26 2 OMIT -1 0 1 OMIT 1 1 1 OMIT 1 0 0 OMIT 1 0 1 OMIT 1 1 0 OMIT 0 4 1 OMIT -1 1 0 OMIT -4 -11 2 OMIT 0 1 1 OMIT -3.00 50.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 HTAB C68 N2_$1 HTAB C53 O12 HTAB C47 N2_$1 HTAB C21 O3 HTAB C6 O4 HTAB C68 N2_$1 HTAB C53 O12 HTAB C47 N2_$1 HTAB C21 O3 HTAB C6 O4 simu 0.004 o7 o7' c46 c46' dfix 1.42 0.04 c24 o7 c24 o7' dfix 1.46 0.02 o7 c46 o7' c46' simu size 0.15 0.12 0.07 wpdb -1 mpla htab conf HTAB C6 O4 HTAB C21 O3 HTAB C43 O10 EQIV $1 x+1, y, z HTAB C47 N2_$1 HTAB C53 O12 HTAB C68 N2_$1 TEMP -80.16 WGHT 0.044300 5.817000 FVAR 0.10080 S1 5 0.294962 0.905500 0.339769 11.00000 0.05396 0.08135 = 0.05403 0.00052 0.00300 -0.01413 N1 3 0.184921 0.849065 0.664150 11.00000 0.06082 0.11974 = 0.06688 -0.04156 0.01532 -0.05263 N2 3 -0.241916 0.874157 0.565895 11.00000 0.09476 0.27119 = 0.08010 -0.04564 -0.01030 -0.08427 N3 3 -0.253020 0.776399 0.828725 11.00000 0.08270 0.16646 = 0.07936 -0.03378 0.02238 -0.07047 O1 4 0.458760 0.732618 -0.020803 11.00000 0.08569 0.14089 = 0.05240 0.00529 -0.00708 -0.05016 O2 4 0.494477 0.540096 0.306136 11.00000 0.06952 0.16409 = 0.05836 0.01817 0.00553 -0.01350 O3 4 0.886701 0.374133 0.409800 11.00000 0.10868 0.14462 = 0.09647 -0.06694 -0.05426 0.04278 O4 4 0.789691 0.469922 0.077147 11.00000 0.07883 0.18139 = 0.06282 -0.04697 0.01573 -0.07949 O5 4 1.174554 0.518570 0.192410 11.00000 0.05499 0.21621 = 0.25597 -0.19278 -0.01138 -0.00612 O6 4 0.895384 0.670120 0.442488 11.00000 0.16397 0.15726 = 0.13184 -0.11080 -0.07186 0.06950 O8 4 0.602868 0.967945 0.329653 11.00000 0.08597 0.09873 = 0.05783 -0.01468 0.00003 0.00400 O9 4 0.671894 0.935561 0.040893 11.00000 0.06200 0.13585 = 0.05414 -0.01062 0.00618 -0.04422 O10 4 0.868265 0.715290 0.026229 11.00000 0.12022 0.20399 = 0.11653 -0.00990 0.04435 -0.00299 O11 4 0.752796 0.765777 0.127953 11.00000 0.08434 0.13967 = 0.05740 -0.00219 -0.00521 -0.02993 O12 4 0.393229 0.736417 0.603870 11.00000 0.06939 0.22758 = 0.12754 -0.07724 -0.01585 -0.01070 O13 4 0.478317 0.805101 0.656254 11.00000 0.08462 0.29201 = 0.25796 -0.09618 -0.00449 -0.10359 C1 1 0.343857 0.833671 0.100929 11.00000 0.05142 0.14461 = 0.05407 0.00437 -0.00831 -0.03161 AFIX 23 H1A 2 0.272286 0.846888 0.134764 11.00000 -1.20000 H1B 2 0.324710 0.852376 0.041422 11.00000 -1.20000 AFIX 0 C2 1 0.410268 0.731313 0.121844 11.00000 0.04402 0.14117 = 0.05328 0.01006 -0.00522 -0.04369 C3 1 0.417473 0.683320 0.203533 11.00000 0.04325 0.13771 = 0.05687 0.00537 -0.00130 -0.02841 AFIX 43 H3 2 0.375996 0.714272 0.246018 11.00000 -1.20000 AFIX 0 C4 1 0.483846 0.590914 0.225164 11.00000 0.04898 0.14679 = 0.04962 0.01152 -0.00281 -0.03889 C5 1 0.544206 0.542522 0.164667 11.00000 0.03719 0.13288 = 0.06562 0.00113 -0.00249 -0.04335 C6 1 0.534787 0.590859 0.082319 11.00000 0.05188 0.14032 = 0.05186 0.00024 -0.00393 -0.04967 AFIX 43 H6 2 0.574699 0.559651 0.039599 11.00000 -1.20000 AFIX 0 C7 1 0.468890 0.683237 0.060695 11.00000 0.05811 0.14894 = 0.04759 0.01350 -0.01351 -0.05559 C8 1 0.620064 0.442639 0.187791 11.00000 0.04819 0.13224 = 0.07135 0.00214 -0.00618 -0.04076 AFIX 23 H8A 2 0.631993 0.414508 0.138775 11.00000 -1.20000 H8B 2 0.582096 0.409426 0.232744 11.00000 -1.20000 AFIX 0 C9 1 0.734134 0.430919 0.216953 11.00000 0.04330 0.12396 = 0.06327 -0.02859 0.00014 -0.02069 C10 1 0.757304 0.406715 0.300705 11.00000 0.05126 0.11687 = 0.06703 -0.02765 -0.00417 0.00591 AFIX 43 H10 2 0.701991 0.394854 0.341130 11.00000 -1.20000 AFIX 0 C11 1 0.860013 0.399539 0.326423 11.00000 0.05899 0.11782 = 0.08497 -0.05737 -0.02994 0.02553 C12 1 0.942316 0.415976 0.269570 11.00000 0.03966 0.14566 = 0.13014 -0.10359 -0.01799 0.01117 C13 1 0.920028 0.438972 0.186136 11.00000 0.04432 0.16024 = 0.11197 -0.09259 0.01059 -0.03567 AFIX 43 H13 2 0.976345 0.449399 0.145991 11.00000 -1.20000 AFIX 0 C14 1 0.816705 0.447308 0.159210 11.00000 0.05192 0.14899 = 0.07040 -0.05413 0.00824 -0.04262 C15 1 1.053923 0.412748 0.296712 11.00000 0.05004 0.16248 = 0.19516 -0.13865 -0.03741 0.01277 AFIX 23 H15A 2 1.114466 0.390570 0.255125 11.00000 -1.20000 H15B 2 1.073511 0.368564 0.350841 11.00000 -1.20000 AFIX 0 C16 1 1.047476 0.508565 0.305517 11.00000 0.05085 0.15420 = 0.18452 -0.13523 -0.05773 0.03413 C17 1 1.108123 0.555661 0.257078 11.00000 0.04705 0.19912 = 0.24525 -0.17784 -0.04621 0.01308 C18 1 1.098708 0.642078 0.268221 11.00000 0.05673 0.18207 = 0.22184 -0.15535 -0.04407 0.00277 AFIX 43 H18 2 1.141008 0.675453 0.232901 11.00000 -1.20000 AFIX 0 C19 1 1.027515 0.678601 0.330909 11.00000 0.08069 0.16459 = 0.20135 -0.13955 -0.06989 0.03276 C20 1 0.966507 0.632967 0.379898 11.00000 0.08983 0.14475 = 0.14062 -0.10624 -0.07687 0.05471 C21 1 0.975465 0.543600 0.371440 11.00000 0.07864 0.13388 = 0.14718 -0.09794 -0.06274 0.03639 AFIX 43 H21 2 0.935170 0.509434 0.408164 11.00000 -1.20000 AFIX 0 C22 1 1.011023 0.776283 0.340021 11.00000 0.09823 0.13835 = 0.17609 -0.10868 -0.06887 0.02108 AFIX 23 H22A 2 1.002115 0.778402 0.399873 11.00000 -1.20000 H22B 2 1.078745 0.791312 0.316782 11.00000 -1.20000 AFIX 0 C23 1 0.907442 0.847301 0.294678 11.00000 0.07684 0.13862 = 0.12823 -0.09369 -0.04175 0.01024 C24 1 0.915135 0.884758 0.209804 11.00000 0.05993 0.20452 = 0.12376 -0.11232 -0.00962 -0.02750 C25 1 0.820767 0.947240 0.168372 11.00000 0.06526 0.19867 = 0.09400 -0.07914 -0.00091 -0.04070 AFIX 43 H25 2 0.827889 0.972812 0.110679 11.00000 -1.20000 AFIX 0 C26 1 0.716082 0.973601 0.208663 11.00000 0.06236 0.12010 = 0.06386 -0.03644 -0.00774 -0.02197 C27 1 0.708121 0.936637 0.293149 11.00000 0.07133 0.09463 = 0.06496 -0.03536 -0.01179 0.00011 C28 1 0.803412 0.875266 0.336122 11.00000 0.09642 0.10254 = 0.07971 -0.05174 -0.03087 0.00157 AFIX 43 H28 2 0.797014 0.852346 0.394448 11.00000 -1.20000 AFIX 0 C29 1 0.611257 1.039014 0.161736 11.00000 0.06927 0.12122 = 0.05969 -0.00863 -0.00725 -0.03407 AFIX 23 H29A 2 0.565482 1.084899 0.194892 11.00000 -1.20000 H29B 2 0.634051 1.072524 0.108086 11.00000 -1.20000 AFIX 0 C30 1 0.540597 0.987589 0.145089 11.00000 0.05994 0.11223 = 0.04141 0.00365 -0.00767 -0.02840 C31 1 0.442448 0.989446 0.190760 11.00000 0.06094 0.11332 = 0.05028 0.00636 -0.00509 -0.02480 AFIX 43 H31 2 0.419422 1.024497 0.232815 11.00000 -1.20000 AFIX 0 C32 1 0.374655 0.942369 0.178522 11.00000 0.05627 0.11143 = 0.04225 0.01139 -0.00469 -0.01868 C33 1 0.408868 0.890204 0.117194 11.00000 0.04943 0.12184 = 0.04999 0.01559 -0.01305 -0.03296 C34 1 0.508931 0.886238 0.070601 11.00000 0.05740 0.12220 = 0.04346 -0.00118 -0.00632 -0.03634 AFIX 43 H34 2 0.533118 0.850665 0.028949 11.00000 -1.20000 AFIX 0 C35 1 0.572905 0.934150 0.085105 11.00000 0.05628 0.12488 = 0.03826 0.00521 -0.00604 -0.03384 C36 1 0.731246 0.865928 -0.004287 11.00000 0.05800 0.16313 = 0.05170 -0.01678 0.00918 -0.04447 AFIX 23 H36A 2 0.787168 0.885587 -0.043375 11.00000 -1.20000 H36B 2 0.677284 0.858675 -0.037765 11.00000 -1.20000 AFIX 0 C37 1 0.791254 0.774598 0.051167 11.00000 0.05470 0.16402 = 0.06733 -0.01394 0.00907 -0.03014 C38 1 0.795862 0.679713 0.186806 11.00000 0.09575 0.14308 = 0.08089 0.01380 -0.01628 -0.02120 AFIX 23 H38A 2 0.868635 0.673315 0.207387 11.00000 -1.20000 H38B 2 0.809054 0.627950 0.159463 11.00000 -1.20000 AFIX 0 C39 1 0.714452 0.677257 0.256118 11.00000 0.10088 0.17165 = 0.08392 0.02845 -0.01678 -0.04951 AFIX 137 H39A 2 0.709743 0.723058 0.287689 11.00000 -1.50000 H39B 2 0.738473 0.615793 0.292714 11.00000 -1.50000 H39C 2 0.640207 0.691262 0.234720 11.00000 -1.50000 AFIX 0 C40 1 0.532786 0.690761 -0.082938 11.00000 0.09684 0.17491 = 0.05142 -0.00219 0.01165 -0.06116 AFIX 137 H40A 2 0.611182 0.671807 -0.067337 11.00000 -1.50000 H40B 2 0.520924 0.734985 -0.136631 11.00000 -1.50000 H40C 2 0.517253 0.636652 -0.087653 11.00000 -1.50000 AFIX 0 C41 1 0.432189 0.586473 0.369368 11.00000 0.15721 0.22217 = 0.04766 0.01877 0.01910 0.00543 AFIX 137 H41A 2 0.462169 0.633202 0.374031 11.00000 -1.50000 H41B 2 0.438765 0.542007 0.422714 11.00000 -1.50000 H41C 2 0.352597 0.616253 0.355051 11.00000 -1.50000 AFIX 0 C42 1 0.797688 0.372857 0.470215 11.00000 0.17253 0.10117 = 0.07185 -0.03099 -0.03525 0.02840 AFIX 137 H42A 2 0.735960 0.432666 0.459637 11.00000 -1.50000 H42B 2 0.825625 0.360610 0.526054 11.00000 -1.50000 H42C 2 0.770044 0.324416 0.466650 11.00000 -1.50000 AFIX 0 C43 1 0.869957 0.493536 0.016030 11.00000 0.14594 0.28689 = 0.09120 -0.09594 0.06223 -0.16497 AFIX 137 H43A 2 0.887342 0.543390 0.029069 11.00000 -1.50000 H43B 2 0.838060 0.513820 -0.039370 11.00000 -1.50000 H43C 2 0.939278 0.439521 0.016657 11.00000 -1.50000 AFIX 0 C44 1 1.244183 0.564644 0.144626 11.00000 0.07408 0.32735 = 0.34507 -0.26956 0.03241 -0.05972 AFIX 137 H44A 2 1.197239 0.626828 0.117173 11.00000 -1.50000 H44B 2 1.287502 0.530496 0.102326 11.00000 -1.50000 H44C 2 1.296207 0.568635 0.181165 11.00000 -1.50000 AFIX 0 C45 1 0.821888 0.631695 0.487226 11.00000 0.24319 0.13528 = 0.08421 -0.06010 -0.04567 0.10314 AFIX 137 H45A 2 0.770682 0.628728 0.449387 11.00000 -1.50000 H45B 2 0.778009 0.669245 0.527039 11.00000 -1.50000 H45C 2 0.863891 0.569361 0.517564 11.00000 -1.50000 AFIX 0 C47 1 0.578822 0.919380 0.408734 11.00000 0.12284 0.11289 = 0.06946 -0.00401 -0.00831 -0.02480 AFIX 137 H47A 2 0.601385 0.854001 0.407977 11.00000 -1.50000 H47B 2 0.497667 0.944207 0.422131 11.00000 -1.50000 H47C 2 0.620717 0.926212 0.451001 11.00000 -1.50000 AFIX 0 C48 1 0.275143 0.944650 0.234022 11.00000 0.05570 0.09132 = 0.05628 0.01185 -0.00239 -0.01847 C49 1 0.163092 0.974443 0.218388 11.00000 0.05777 0.13278 = 0.06210 0.02481 -0.00430 -0.02617 AFIX 43 H49 2 0.134721 0.998511 0.163815 11.00000 -1.20000 AFIX 0 C50 1 0.093188 0.966145 0.290984 11.00000 0.05035 0.09599 = 0.07516 0.01968 0.00023 -0.02048 AFIX 43 H50 2 0.013483 0.983990 0.290197 11.00000 -1.20000 AFIX 0 C51 1 0.152487 0.929772 0.362247 11.00000 0.05770 0.05760 = 0.06453 -0.00004 0.00742 -0.01650 C52 1 0.107141 0.913011 0.446568 11.00000 0.06156 0.04026 = 0.07188 -0.00938 0.01215 -0.01461 AFIX 43 H52 2 0.027699 0.928626 0.454394 11.00000 -1.20000 AFIX 0 C53 1 0.168928 0.877287 0.513814 11.00000 0.05769 0.06117 = 0.06468 -0.01742 0.01067 -0.02676 AFIX 43 H53 2 0.247869 0.864840 0.506263 11.00000 -1.20000 AFIX 0 C54 1 0.123668 0.855725 0.598952 11.00000 0.06324 0.07855 = 0.05591 -0.02664 0.00856 -0.03423 C55 1 0.023619 0.841669 0.613662 11.00000 0.05652 0.08137 = 0.05618 -0.02451 0.00489 -0.03483 AFIX 43 H55 2 -0.016140 0.845418 0.567240 11.00000 -1.20000 AFIX 0 C56 1 -0.023970 0.821843 0.694238 11.00000 0.05566 0.09058 = 0.05883 -0.02746 0.00752 -0.03868 C57 1 0.047221 0.804587 0.763331 11.00000 0.05269 0.11335 = 0.05548 -0.03269 0.01090 -0.03579 C58 1 0.017746 0.776358 0.847189 11.00000 0.06272 0.13934 = 0.05635 -0.03140 0.00977 -0.03981 AFIX 43 H58 2 -0.052693 0.767882 0.860530 11.00000 -1.20000 AFIX 0 C59 1 0.086636 0.760540 0.910600 11.00000 0.07666 0.16370 = 0.05596 -0.03592 0.00066 -0.04096 AFIX 43 H59 2 0.063993 0.741233 0.966775 11.00000 -1.20000 AFIX 0 C60 1 0.189492 0.772785 0.892566 11.00000 0.07164 0.19024 = 0.07044 -0.05593 -0.00071 -0.04715 AFIX 43 H60 2 0.237314 0.762249 0.936476 11.00000 -1.20000 AFIX 0 C61 1 0.222154 0.799849 0.812161 11.00000 0.06523 0.16398 = 0.08061 -0.06013 0.00730 -0.04860 AFIX 43 H61 2 0.293605 0.806754 0.800358 11.00000 -1.20000 AFIX 0 C62 1 0.152111 0.817751 0.746320 11.00000 0.06119 0.12075 = 0.06070 -0.04042 0.01171 -0.04536 C63 1 -0.133147 0.821016 0.701066 11.00000 0.06304 0.11659 = 0.05548 -0.02847 0.00445 -0.04716 C64 1 -0.193935 0.848338 0.626870 11.00000 0.06579 0.17268 = 0.06951 -0.03671 0.01327 -0.06389 C65 1 -0.196314 0.796229 0.773749 11.00000 0.05998 0.13336 = 0.07252 -0.03413 0.01052 -0.04921 C66 1 0.285127 0.875986 0.647676 11.00000 0.07851 0.17606 = 0.09965 -0.06969 0.02399 -0.08241 AFIX 23 H66A 2 0.294467 0.899605 0.695302 11.00000 -1.20000 H66B 2 0.273576 0.926408 0.597391 11.00000 -1.20000 AFIX 0 C67 1 0.390400 0.797176 0.634705 11.00000 0.07082 0.23535 = 0.09105 -0.05757 0.01641 -0.07787 C68 1 0.589156 0.741355 0.630198 11.00000 0.06937 0.32261 = 0.25711 0.01674 0.00770 -0.08301 AFIX 23 H68A 2 0.582251 0.726156 0.577032 11.00000 -1.20000 H68B 2 0.646355 0.771116 0.621580 11.00000 -1.20000 AFIX 0 C69 1 0.623415 0.658789 0.694364 11.00000 0.10339 0.39089 = 0.11985 0.06257 -0.02642 -0.08658 AFIX 137 H69A 2 0.623183 0.674910 0.747872 11.00000 -1.50000 H69B 2 0.699650 0.618949 0.680603 11.00000 -1.50000 H69C 2 0.570765 0.626230 0.698353 11.00000 -1.50000 PART 1 AFIX 0 O7 4 1.020298 0.827734 0.190789 10.50000 0.06410 0.15136 = 0.06735 -0.03697 -0.00110 -0.04185 C46 1 1.034271 0.839417 0.102014 10.50000 0.06402 0.15936 = 0.07525 -0.02684 -0.00018 -0.03994 AFIX 137 H46A 2 1.010335 0.905252 0.076207 10.50000 -1.50000 H46B 2 0.988159 0.811873 0.082156 10.50000 -1.50000 H46C 2 1.113885 0.809125 0.086911 10.50000 -1.50000 PART 2 AFIX 0 O7' 4 1.020299 0.879717 0.154950 10.50000 0.05916 0.15027 = 0.06620 -0.03301 0.00451 -0.04199 C46' 1 1.023386 0.921851 0.069836 10.50000 0.05767 0.16126 = 0.07322 -0.02690 0.00279 -0.03959 AFIX 137 H46D 2 0.974950 0.905650 0.039529 10.50000 -1.50000 H46E 2 1.101115 0.900369 0.047177 10.50000 -1.50000 H46F 2 0.996243 0.988861 0.063557 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM mo_dd20011_0m_a.res in P-1 REM R1 = 0.0932 for 5107 Fo > 4sig(Fo) and 0.1954 for all 10699 data REM 804 parameters refined using 598 restraints END WGHT 0.0438 6.0552 REM Instructions for potential hydrogen bonds HTAB C6 O4 HTAB C21 O3 HTAB C47 N2_$1 HTAB C53 O12 HTAB C68 N2_$1 REM Highest difference peak 0.339, deepest hole -0.316, 1-sigma level 0.047 Q1 1 1.2418 0.5958 0.1189 11.00000 0.05 0.34 Q2 1 1.1938 0.5433 0.1709 11.00000 0.05 0.33 Q3 1 1.0766 0.5147 0.2836 11.00000 0.05 0.29 Q4 1 0.8607 0.6436 0.4765 11.00000 0.05 0.28 Q5 1 0.9171 0.6980 0.4317 11.00000 0.05 0.26 Q6 1 1.1010 0.5861 0.2278 11.00000 0.05 0.24 Q7 1 1.1889 0.4880 0.2417 11.00000 0.05 0.24 Q8 1 0.8984 0.4121 0.4103 11.00000 0.05 0.23 Q9 1 0.9767 0.6555 0.3535 11.00000 0.05 0.23 Q10 1 0.7679 0.6940 0.0144 11.00000 0.05 0.22 Q11 1 0.8598 0.3452 0.4380 11.00000 0.05 0.21 Q12 1 1.1174 0.6772 0.2506 11.00000 0.05 0.21 Q13 1 1.0389 0.4641 0.3382 11.00000 0.05 0.20 Q14 1 0.4246 0.8028 0.5555 11.00000 0.05 0.20 Q15 1 1.0396 0.7052 0.3082 11.00000 0.05 0.20 Q16 1 1.0589 0.4317 0.2635 11.00000 0.05 0.19 Q17 1 0.5068 0.6788 0.6060 11.00000 0.05 0.19 Q18 1 0.9177 0.9265 0.2034 11.00000 0.05 0.19 Q19 1 0.8015 0.5742 0.5036 11.00000 0.05 0.19 Q20 1 0.5366 0.6583 0.5243 11.00000 0.05 0.18 ; _shelx_res_checksum 37093 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.29496(11) 0.90550(11) 0.33977(8) 0.0693(4) Uani 1 1 d . U . . . N1 N 0.1849(4) 0.8491(4) 0.6641(3) 0.0741(14) Uani 1 1 d . U . . . N2 N -0.2419(5) 0.8742(6) 0.5659(4) 0.141(3) Uani 1 1 d . U . . . N3 N -0.2530(4) 0.7764(4) 0.8287(3) 0.1027(19) Uani 1 1 d . U . . . O1 O 0.4588(3) 0.7326(3) -0.0208(2) 0.0945(14) Uani 1 1 d . U . . . O2 O 0.4945(3) 0.5401(4) 0.3061(2) 0.1140(18) Uani 1 1 d . U . . . O3 O 0.8867(4) 0.3741(4) 0.4098(3) 0.130(2) Uani 1 1 d . U . . . O4 O 0.7897(3) 0.4699(3) 0.0771(2) 0.0957(14) Uani 1 1 d . U . . . O5 O 1.1746(4) 0.5186(5) 0.1924(5) 0.161(3) Uani 1 1 d . U . . . O6 O 0.8954(6) 0.6701(5) 0.4425(4) 0.167(4) Uani 1 1 d . U . . . O8 O 0.6029(3) 0.9679(3) 0.3297(2) 0.0923(14) Uani 1 1 d . U . . . O9 O 0.6719(3) 0.9356(3) 0.0409(2) 0.0839(13) Uani 1 1 d . U . . . O10 O 0.8683(5) 0.7153(5) 0.0262(4) 0.172(3) Uani 1 1 d . U . . . O11 O 0.7528(3) 0.7658(3) 0.1280(2) 0.1000(15) Uani 1 1 d . U . . . O12 O 0.3932(4) 0.7364(5) 0.6039(4) 0.145(3) Uani 1 1 d . U . . . O13 O 0.4783(5) 0.8051(6) 0.6563(5) 0.194(3) Uani 1 1 d . U . . . C1 C 0.3439(5) 0.8337(5) 0.1009(3) 0.088(2) Uani 1 1 d . U . . . H1A H 0.2723 0.8469 0.1348 0.106 Uiso 1 1 calc R U . . . H1B H 0.3247 0.8524 0.0414 0.106 Uiso 1 1 calc R U . . . C2 C 0.4103(4) 0.7313(5) 0.1218(3) 0.082(2) Uani 1 1 d . U . . . C3 C 0.4175(4) 0.6833(5) 0.2035(3) 0.085(2) Uani 1 1 d . U . . . H3 H 0.3760 0.7143 0.2460 0.102 Uiso 1 1 calc R U . . . C4 C 0.4838(5) 0.5909(5) 0.2252(3) 0.087(2) Uani 1 1 d . U . . . C5 C 0.5442(4) 0.5425(5) 0.1647(4) 0.0788(19) Uani 1 1 d . U . . . C6 C 0.5348(5) 0.5909(5) 0.0823(3) 0.0804(19) Uani 1 1 d . U . . . H6 H 0.5747 0.5597 0.0396 0.097 Uiso 1 1 calc R U . . . C7 C 0.4689(5) 0.6832(6) 0.0607(3) 0.085(2) Uani 1 1 d . U . . . C8 C 0.6201(4) 0.4426(5) 0.1878(4) 0.085(2) Uani 1 1 d . U . . . H8A H 0.6320 0.4145 0.1388 0.103 Uiso 1 1 calc R U . . . H8B H 0.5821 0.4094 0.2327 0.103 Uiso 1 1 calc R U . . . C9 C 0.7341(4) 0.4309(5) 0.2170(3) 0.0781(18) Uani 1 1 d . U . . . C10 C 0.7573(5) 0.4067(4) 0.3007(4) 0.087(2) Uani 1 1 d . U . . . H10 H 0.7020 0.3949 0.3411 0.105 Uiso 1 1 calc R U . . . C11 C 0.8600(5) 0.3995(5) 0.3264(4) 0.095(2) Uani 1 1 d . U . . . C12 C 0.9423(5) 0.4160(5) 0.2696(5) 0.103(3) Uani 1 1 d . U . . . C13 C 0.9200(4) 0.4390(5) 0.1861(4) 0.095(2) Uani 1 1 d . U . . . H13 H 0.9763 0.4494 0.1460 0.114 Uiso 1 1 calc R U . . . C14 C 0.8167(4) 0.4473(5) 0.1592(4) 0.0837(19) Uani 1 1 d . U . . . C15 C 1.0539(5) 0.4127(5) 0.2967(5) 0.129(3) Uani 1 1 d . U . . . H15A H 1.1145 0.3906 0.2551 0.155 Uiso 1 1 calc R U . . . H15B H 1.0735 0.3686 0.3508 0.155 Uiso 1 1 calc R U . . . C16 C 1.0475(6) 0.5086(7) 0.3055(6) 0.127(4) Uani 1 1 d . U . . . C17 C 1.1081(6) 0.5557(8) 0.2571(8) 0.153(4) Uani 1 1 d . U . . . C18 C 1.0987(5) 0.6421(6) 0.2682(6) 0.143(4) Uani 1 1 d . U . . . H18 H 1.1410 0.6755 0.2329 0.171 Uiso 1 1 calc R U . . . C19 C 1.0275(8) 0.6786(8) 0.3309(8) 0.147(5) Uani 1 1 d . U . . . C20 C 0.9665(8) 0.6330(8) 0.3799(6) 0.133(4) Uani 1 1 d . U . . . C21 C 0.9755(5) 0.5436(6) 0.3714(5) 0.124(3) Uani 1 1 d . U . . . H21 H 0.9352 0.5094 0.4082 0.149 Uiso 1 1 calc R U . . . C22 C 1.0110(6) 0.7763(5) 0.3400(5) 0.136(3) Uani 1 1 d . U . . . H22A H 1.0021 0.7784 0.3999 0.164 Uiso 1 1 calc R U . . . H22B H 1.0787 0.7913 0.3168 0.164 Uiso 1 1 calc R U . . . C23 C 0.9074(6) 0.8473(6) 0.2947(5) 0.113(3) Uani 1 1 d . U . . . C24 C 0.9151(6) 0.8848(6) 0.2098(5) 0.120(3) Uani 1 1 d D U . . . C25 C 0.8208(5) 0.9472(6) 0.1684(4) 0.112(3) Uani 1 1 d . U . . . H25 H 0.8279 0.9728 0.1107 0.135 Uiso 1 1 calc R U . . . C26 C 0.7161(5) 0.9736(5) 0.2087(4) 0.0816(18) Uani 1 1 d . U . . . C27 C 0.7081(5) 0.9366(4) 0.2931(4) 0.0814(18) Uani 1 1 d . U . . . C28 C 0.8034(6) 0.8753(5) 0.3361(4) 0.095(2) Uani 1 1 d . U . . . H28 H 0.7970 0.8523 0.3944 0.114 Uiso 1 1 calc R U . . . C29 C 0.6113(5) 1.0390(5) 0.1617(3) 0.0849(19) Uani 1 1 d . U . . . H29A H 0.5655 1.0849 0.1949 0.102 Uiso 1 1 calc R U . . . H29B H 0.6341 1.0725 0.1081 0.102 Uiso 1 1 calc R U . . . C30 C 0.5406(5) 0.9876(4) 0.1451(3) 0.0750(17) Uani 1 1 d . U . . . C31 C 0.4424(5) 0.9894(5) 0.1908(3) 0.0808(19) Uani 1 1 d . U . . . H31 H 0.4194 1.0245 0.2328 0.097 Uiso 1 1 calc R U . . . C32 C 0.3747(5) 0.9424(5) 0.1785(3) 0.0781(19) Uani 1 1 d . U . . . C33 C 0.4089(4) 0.8902(5) 0.1172(3) 0.0783(19) Uani 1 1 d . U . . . C34 C 0.5089(4) 0.8862(4) 0.0706(3) 0.0757(18) Uani 1 1 d . U . . . H34 H 0.5331 0.8507 0.0289 0.091 Uiso 1 1 calc R U . . . C35 C 0.5729(5) 0.9342(5) 0.0851(3) 0.0764(18) Uani 1 1 d . U . . . C36 C 0.7312(5) 0.8659(5) -0.0043(3) 0.092(2) Uani 1 1 d . U . . . H36A H 0.7872 0.8856 -0.0434 0.110 Uiso 1 1 calc R U . . . H36B H 0.6773 0.8587 -0.0378 0.110 Uiso 1 1 calc R U . . . C37 C 0.7913(5) 0.7746(6) 0.0512(4) 0.101(2) Uani 1 1 d . U . . . C38 C 0.7959(6) 0.6797(6) 0.1868(4) 0.119(3) Uani 1 1 d . U . . . H38A H 0.8686 0.6733 0.2074 0.142 Uiso 1 1 calc R U . . . H38B H 0.8091 0.6279 0.1595 0.142 Uiso 1 1 calc R U . . . C39 C 0.7145(6) 0.6773(6) 0.2561(4) 0.128(3) Uani 1 1 d . U . . . H39A H 0.7097 0.7231 0.2877 0.191 Uiso 1 1 calc R U . . . H39B H 0.7385 0.6158 0.2927 0.191 Uiso 1 1 calc R U . . . H39C H 0.6402 0.6913 0.2347 0.191 Uiso 1 1 calc R U . . . C40 C 0.5328(5) 0.6908(5) -0.0829(4) 0.109(3) Uani 1 1 d . U . . . H40A H 0.6112 0.6718 -0.0673 0.164 Uiso 1 1 calc R U . . . H40B H 0.5209 0.7350 -0.1366 0.164 Uiso 1 1 calc R U . . . H40C H 0.5173 0.6367 -0.0877 0.164 Uiso 1 1 calc R U . . . C41 C 0.4322(7) 0.5865(7) 0.3694(4) 0.175(5) Uani 1 1 d . U . . . H41A H 0.4622 0.6332 0.3740 0.262 Uiso 1 1 calc R U . . . H41B H 0.4388 0.5420 0.4227 0.262 Uiso 1 1 calc R U . . . H41C H 0.3526 0.6163 0.3551 0.262 Uiso 1 1 calc R U . . . C42 C 0.7977(7) 0.3729(5) 0.4702(4) 0.133(3) Uani 1 1 d . U . . . H42A H 0.7360 0.4327 0.4596 0.199 Uiso 1 1 calc R U . . . H42B H 0.8256 0.3606 0.5261 0.199 Uiso 1 1 calc R U . . . H42C H 0.7700 0.3244 0.4666 0.199 Uiso 1 1 calc R U . . . C43 C 0.8700(6) 0.4935(7) 0.0160(4) 0.145(4) Uani 1 1 d . U . . . H43A H 0.8873 0.5434 0.0291 0.217 Uiso 1 1 calc R U . . . H43B H 0.8381 0.5138 -0.0394 0.217 Uiso 1 1 calc R U . . . H43C H 0.9393 0.4395 0.0167 0.217 Uiso 1 1 calc R U . . . C44 C 1.2442(7) 0.5646(8) 0.1446(8) 0.219(7) Uani 1 1 d . U . . . H44A H 1.1972 0.6268 0.1172 0.329 Uiso 1 1 calc R U . . . H44B H 1.2875 0.5305 0.1023 0.329 Uiso 1 1 calc R U . . . H44C H 1.2962 0.5686 0.1812 0.329 Uiso 1 1 calc R U . . . C45 C 0.8219(11) 0.6317(8) 0.4872(6) 0.194(8) Uani 1 1 d . U . . . H45A H 0.7707 0.6287 0.4494 0.291 Uiso 1 1 calc R U . . . H45B H 0.7780 0.6692 0.5270 0.291 Uiso 1 1 calc R U . . . H45C H 0.8639 0.5694 0.5176 0.291 Uiso 1 1 calc R U . . . C47 C 0.5788(6) 0.9194(5) 0.4087(4) 0.109(2) Uani 1 1 d . U . . . H47A H 0.6014 0.8540 0.4080 0.164 Uiso 1 1 calc R U . . . H47B H 0.4977 0.9442 0.4221 0.164 Uiso 1 1 calc R U . . . H47C H 0.6207 0.9262 0.4510 0.164 Uiso 1 1 calc R U . . . C48 C 0.2751(4) 0.9446(4) 0.2340(3) 0.0751(17) Uani 1 1 d . U . . . C49 C 0.1631(5) 0.9744(5) 0.2184(4) 0.095(2) Uani 1 1 d . U . . . H49 H 0.1347 0.9985 0.1638 0.114 Uiso 1 1 calc R U . . . C50 C 0.0932(5) 0.9661(4) 0.2910(4) 0.0827(19) Uani 1 1 d . U . . . H50 H 0.0135 0.9840 0.2902 0.099 Uiso 1 1 calc R U . . . C51 C 0.1525(4) 0.9298(4) 0.3622(3) 0.0644(15) Uani 1 1 d . U . . . C52 C 0.1071(4) 0.9130(3) 0.4466(3) 0.0607(14) Uani 1 1 d . U . . . H52 H 0.0277 0.9286 0.4544 0.073 Uiso 1 1 calc R U . . . C53 C 0.1689(4) 0.8773(4) 0.5138(3) 0.0600(14) Uani 1 1 d . U . . . H53 H 0.2479 0.8648 0.5063 0.072 Uiso 1 1 calc R U . . . C54 C 0.1237(4) 0.8557(4) 0.5990(3) 0.0620(14) Uani 1 1 d . U . . . C55 C 0.0236(4) 0.8417(4) 0.6137(3) 0.0605(14) Uani 1 1 d . U . . . H55 H -0.0161 0.8454 0.5672 0.073 Uiso 1 1 calc R U . . . C56 C -0.0240(4) 0.8218(4) 0.6942(3) 0.0634(15) Uani 1 1 d . U . . . C57 C 0.0472(4) 0.8046(4) 0.7633(3) 0.0705(16) Uani 1 1 d . U . . . C58 C 0.0177(5) 0.7764(5) 0.8472(3) 0.0841(19) Uani 1 1 d . U . . . H58 H -0.0527 0.7679 0.8605 0.101 Uiso 1 1 calc R U . . . C59 C 0.0866(5) 0.7605(5) 0.9106(4) 0.097(2) Uani 1 1 d . U . . . H59 H 0.0640 0.7412 0.9668 0.117 Uiso 1 1 calc R U . . . C60 C 0.1895(5) 0.7728(6) 0.8926(4) 0.106(2) Uani 1 1 d . U . . . H60 H 0.2373 0.7622 0.9365 0.127 Uiso 1 1 calc R U . . . C61 C 0.2222(5) 0.7998(5) 0.8122(4) 0.096(2) Uani 1 1 d . U . . . H61 H 0.2936 0.8068 0.8004 0.115 Uiso 1 1 calc R U . . . C62 C 0.1521(4) 0.8178(4) 0.7463(3) 0.0744(17) Uani 1 1 d . U . . . C63 C -0.1331(5) 0.8210(4) 0.7011(3) 0.0726(16) Uani 1 1 d . U . . . C64 C -0.1939(5) 0.8483(6) 0.6269(4) 0.096(2) Uani 1 1 d . U . . . C65 C -0.1963(5) 0.7962(5) 0.7737(4) 0.0832(19) Uani 1 1 d . U . . . C66 C 0.2851(5) 0.8760(5) 0.6477(4) 0.102(2) Uani 1 1 d . U . . . H66A H 0.2945 0.8996 0.6953 0.123 Uiso 1 1 calc R U . . . H66B H 0.2736 0.9264 0.5974 0.123 Uiso 1 1 calc R U . . . C67 C 0.3904(7) 0.7972(8) 0.6347(5) 0.123(3) Uani 1 1 d . U . . . C68 C 0.5892(8) 0.7414(10) 0.6302(9) 0.228(6) Uani 1 1 d . U . . . H68A H 0.5823 0.7262 0.5770 0.274 Uiso 1 1 calc R U . . . H68B H 0.6464 0.7711 0.6216 0.274 Uiso 1 1 calc R U . . . C69 C 0.6234(8) 0.6588(10) 0.6944(6) 0.225(7) Uani 1 1 d . U . . . H69A H 0.6232 0.6749 0.7479 0.337 Uiso 1 1 calc R U . . . H69B H 0.6997 0.6189 0.6806 0.337 Uiso 1 1 calc R U . . . H69C H 0.5708 0.6262 0.6984 0.337 Uiso 1 1 calc R U . . . O7 O 1.0203(9) 0.8277(8) 0.1908(6) 0.091(3) Uani 0.5 1 d D U P A 1 C46 C 1.0343(11) 0.8394(12) 0.1020(7) 0.099(3) Uani 0.5 1 d D U P A 1 H46A H 1.0103 0.9053 0.0762 0.149 Uiso 0.5 1 calc R U P A 1 H46B H 0.9882 0.8119 0.0822 0.149 Uiso 0.5 1 calc R U P A 1 H46C H 1.1139 0.8091 0.0869 0.149 Uiso 0.5 1 calc R U P A 1 O7' O 1.0203(9) 0.8797(8) 0.1550(6) 0.089(3) Uani 0.5 1 d D U P A 2 C46' C 1.0234(11) 0.9219(11) 0.0698(7) 0.097(4) Uani 0.5 1 d D U P A 2 H46D H 0.9750 0.9056 0.0395 0.146 Uiso 0.5 1 calc R U P A 2 H46E H 1.1011 0.9004 0.0472 0.146 Uiso 0.5 1 calc R U P A 2 H46F H 0.9962 0.9889 0.0636 0.146 Uiso 0.5 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0540(8) 0.0813(11) 0.0540(8) 0.0005(7) 0.0030(6) -0.0141(7) N1 0.061(3) 0.120(4) 0.067(3) -0.042(3) 0.015(2) -0.053(3) N2 0.095(4) 0.271(9) 0.080(4) -0.046(5) -0.010(3) -0.084(5) N3 0.083(4) 0.166(6) 0.079(4) -0.034(4) 0.022(3) -0.070(4) O1 0.086(3) 0.141(4) 0.052(2) 0.005(2) -0.007(2) -0.050(3) O2 0.070(3) 0.164(5) 0.058(3) 0.018(3) 0.006(2) -0.013(3) O3 0.109(4) 0.145(5) 0.096(4) -0.067(3) -0.054(3) 0.043(3) O4 0.079(3) 0.181(5) 0.063(3) -0.047(3) 0.016(2) -0.079(3) O5 0.055(3) 0.216(6) 0.256(7) -0.193(6) -0.011(4) -0.006(4) O6 0.164(7) 0.157(7) 0.132(6) -0.111(6) -0.072(5) 0.069(5) O8 0.086(3) 0.099(3) 0.058(2) -0.015(2) 0.000(2) 0.004(2) O9 0.062(2) 0.136(4) 0.054(2) -0.011(2) 0.0062(19) -0.044(2) O10 0.120(5) 0.204(7) 0.117(4) -0.010(4) 0.044(4) -0.003(4) O11 0.084(3) 0.140(4) 0.057(3) -0.002(3) -0.005(2) -0.030(3) O12 0.069(3) 0.228(8) 0.128(5) -0.077(5) -0.016(3) -0.011(4) O13 0.085(4) 0.292(9) 0.258(8) -0.096(7) -0.004(4) -0.104(5) C1 0.051(3) 0.145(6) 0.054(3) 0.004(4) -0.008(3) -0.032(4) C2 0.044(3) 0.141(6) 0.053(4) 0.010(4) -0.005(3) -0.044(4) C3 0.043(3) 0.138(6) 0.057(4) 0.005(4) -0.001(3) -0.028(4) C4 0.049(3) 0.147(6) 0.050(3) 0.012(4) -0.003(3) -0.039(4) C5 0.037(3) 0.133(6) 0.066(4) 0.001(4) -0.002(3) -0.043(3) C6 0.052(3) 0.140(6) 0.052(3) 0.000(4) -0.004(3) -0.050(4) C7 0.058(4) 0.149(7) 0.048(3) 0.013(4) -0.014(3) -0.056(4) C8 0.048(3) 0.132(6) 0.071(4) 0.002(4) -0.006(3) -0.041(4) C9 0.043(3) 0.124(5) 0.063(4) -0.029(3) 0.000(3) -0.021(3) C10 0.051(3) 0.117(5) 0.067(4) -0.028(4) -0.004(3) 0.006(3) C11 0.059(4) 0.118(6) 0.085(5) -0.057(4) -0.030(3) 0.026(4) C12 0.040(3) 0.146(6) 0.130(6) -0.104(5) -0.018(4) 0.011(4) C13 0.044(3) 0.160(7) 0.112(5) -0.093(5) 0.011(3) -0.036(4) C14 0.052(3) 0.149(6) 0.070(4) -0.054(4) 0.008(3) -0.043(4) C15 0.050(4) 0.162(7) 0.195(8) -0.139(6) -0.037(4) 0.013(4) C16 0.051(4) 0.154(8) 0.185(8) -0.135(7) -0.058(5) 0.034(5) C17 0.047(5) 0.199(10) 0.245(11) -0.178(9) -0.046(5) 0.013(5) C18 0.057(4) 0.182(8) 0.222(9) -0.155(8) -0.044(5) 0.003(5) C19 0.081(6) 0.165(10) 0.201(11) -0.140(8) -0.070(6) 0.033(6) C20 0.090(6) 0.145(9) 0.141(8) -0.106(7) -0.077(5) 0.055(6) C21 0.079(5) 0.134(7) 0.147(6) -0.098(6) -0.063(4) 0.036(4) C22 0.098(5) 0.138(7) 0.176(8) -0.109(6) -0.069(5) 0.021(5) C23 0.077(5) 0.139(6) 0.128(6) -0.094(5) -0.042(4) 0.010(4) C24 0.060(4) 0.205(8) 0.124(6) -0.112(6) -0.010(4) -0.027(5) C25 0.065(4) 0.199(8) 0.094(5) -0.079(5) -0.001(4) -0.041(5) C26 0.062(4) 0.120(5) 0.064(4) -0.036(4) -0.008(3) -0.022(4) C27 0.071(4) 0.095(5) 0.065(4) -0.035(3) -0.012(3) 0.000(3) C28 0.096(5) 0.103(5) 0.080(4) -0.052(4) -0.031(4) 0.002(4) C29 0.069(4) 0.121(6) 0.060(4) -0.009(4) -0.007(3) -0.034(4) C30 0.060(3) 0.112(5) 0.041(3) 0.004(3) -0.008(3) -0.028(3) C31 0.061(4) 0.113(5) 0.050(3) 0.006(3) -0.005(3) -0.025(4) C32 0.056(3) 0.111(5) 0.042(3) 0.011(3) -0.005(3) -0.019(3) C33 0.049(3) 0.122(5) 0.050(3) 0.016(3) -0.013(3) -0.033(3) C34 0.057(3) 0.122(5) 0.043(3) -0.001(3) -0.006(3) -0.036(3) C35 0.056(3) 0.125(5) 0.038(3) 0.005(3) -0.006(3) -0.034(4) C36 0.058(4) 0.163(7) 0.052(4) -0.017(4) 0.009(3) -0.044(4) C37 0.055(4) 0.164(8) 0.067(4) -0.014(5) 0.009(3) -0.030(4) C38 0.096(5) 0.143(7) 0.081(5) 0.014(5) -0.016(4) -0.021(5) C39 0.101(5) 0.172(8) 0.084(5) 0.028(5) -0.017(4) -0.050(5) C40 0.097(5) 0.175(8) 0.051(4) -0.002(4) 0.012(3) -0.061(5) C41 0.157(8) 0.222(10) 0.048(4) 0.019(5) 0.019(5) 0.005(7) C42 0.173(8) 0.101(6) 0.072(5) -0.031(4) -0.035(5) 0.028(5) C43 0.146(7) 0.287(11) 0.091(5) -0.096(6) 0.062(5) -0.165(8) C44 0.074(6) 0.327(16) 0.345(16) -0.270(14) 0.032(8) -0.060(8) C45 0.243(15) 0.135(10) 0.084(7) -0.060(7) -0.046(7) 0.103(10) C47 0.123(6) 0.113(6) 0.069(4) -0.004(4) -0.008(4) -0.025(5) C48 0.056(3) 0.091(5) 0.056(3) 0.012(3) -0.002(3) -0.018(3) C49 0.058(4) 0.133(6) 0.062(4) 0.025(4) -0.004(3) -0.026(4) C50 0.050(3) 0.096(5) 0.075(4) 0.020(3) 0.000(3) -0.020(3) C51 0.058(3) 0.058(4) 0.065(4) 0.000(3) 0.007(3) -0.016(3) C52 0.062(3) 0.040(3) 0.072(4) -0.009(3) 0.012(3) -0.015(3) C53 0.058(3) 0.061(4) 0.065(3) -0.017(3) 0.011(3) -0.027(3) C54 0.063(3) 0.079(4) 0.056(3) -0.027(3) 0.009(3) -0.034(3) C55 0.057(3) 0.081(4) 0.056(3) -0.025(3) 0.005(2) -0.035(3) C56 0.056(3) 0.091(4) 0.059(3) -0.027(3) 0.008(3) -0.039(3) C57 0.053(3) 0.113(5) 0.055(3) -0.033(3) 0.011(3) -0.036(3) C58 0.063(4) 0.139(6) 0.056(4) -0.031(4) 0.010(3) -0.040(4) C59 0.077(4) 0.164(7) 0.056(4) -0.036(4) 0.001(3) -0.041(4) C60 0.072(4) 0.190(8) 0.070(4) -0.056(5) -0.001(3) -0.047(5) C61 0.065(4) 0.164(7) 0.081(4) -0.060(4) 0.007(3) -0.049(4) C62 0.061(3) 0.121(5) 0.061(4) -0.040(3) 0.012(3) -0.045(3) C63 0.063(4) 0.117(5) 0.055(3) -0.028(3) 0.004(3) -0.047(3) C64 0.066(4) 0.173(7) 0.070(4) -0.037(4) 0.013(3) -0.064(4) C65 0.060(4) 0.133(6) 0.073(4) -0.034(4) 0.011(3) -0.049(4) C66 0.079(4) 0.176(7) 0.100(5) -0.070(5) 0.024(4) -0.082(5) C67 0.071(5) 0.235(11) 0.091(6) -0.058(6) 0.016(4) -0.078(6) C68 0.069(6) 0.323(16) 0.257(14) 0.017(12) 0.008(7) -0.083(8) C69 0.103(7) 0.39(2) 0.120(8) 0.063(10) -0.026(6) -0.087(10) O7 0.064(3) 0.151(9) 0.067(6) -0.037(5) -0.001(4) -0.042(5) C46 0.064(4) 0.159(9) 0.075(6) -0.027(6) 0.000(5) -0.040(6) O7' 0.059(3) 0.150(9) 0.066(6) -0.033(5) 0.005(4) -0.042(5) C46' 0.058(5) 0.161(9) 0.073(6) -0.027(6) 0.003(5) -0.040(6) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C51 S1 C48 92.6(3) . . ? C54 N1 C62 120.5(4) . . ? C54 N1 C66 119.8(5) . . ? C62 N1 C66 119.8(5) . . ? C7 O1 C40 118.1(5) . . ? C4 O2 C41 116.9(6) . . ? C11 O3 C42 117.5(5) . . ? C14 O4 C43 117.3(5) . . ? C17 O5 C44 118.0(8) . . ? C45 O6 C20 122.2(10) . . ? C27 O8 C47 119.4(5) . . ? C35 O9 C36 119.6(5) . . ? C37 O11 C38 120.7(6) . . ? C67 O13 C68 116.4(9) . . ? C2 C1 C33 112.3(5) . . ? C2 C1 H1A 109.1 . . ? C33 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? C33 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C7 117.9(7) . . ? C3 C2 C1 120.2(6) . . ? C7 C2 C1 121.9(5) . . ? C2 C3 C4 121.5(6) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? O2 C4 C3 123.6(6) . . ? O2 C4 C5 115.3(6) . . ? C3 C4 C5 121.1(5) . . ? C6 C5 C4 117.1(6) . . ? C6 C5 C8 121.3(6) . . ? C4 C5 C8 121.5(5) . . ? C7 C6 C5 121.9(6) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O1 C7 C6 122.7(6) . . ? O1 C7 C2 116.7(7) . . ? C6 C7 C2 120.5(5) . . ? C5 C8 C9 112.6(5) . . ? C5 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C5 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 118.4(5) . . ? C10 C9 C8 121.5(5) . . ? C14 C9 C8 120.1(5) . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 121.2(6) . . ? C12 C11 O3 116.4(6) . . ? C10 C11 O3 122.4(7) . . ? C13 C12 C11 118.1(5) . . ? C13 C12 C15 119.9(7) . . ? C11 C12 C15 122.0(6) . . ? C12 C13 C14 121.5(6) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? O4 C14 C9 115.8(5) . . ? O4 C14 C13 124.1(5) . . ? C9 C14 C13 120.0(6) . . ? C12 C15 C16 111.6(5) . . ? C12 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C12 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C21 120.7(9) . . ? C17 C16 C15 123.5(8) . . ? C21 C16 C15 115.7(10) . . ? C16 C17 O5 117.7(9) . . ? C16 C17 C18 120.8(9) . . ? O5 C17 C18 121.4(11) . . ? C19 C18 C17 119.6(11) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 120.6(11) . . ? C20 C19 C22 119.3(10) . . ? C18 C19 C22 119.9(12) . . ? C19 C20 O6 120.2(11) . . ? C19 C20 C21 121.4(9) . . ? O6 C20 C21 118.4(11) . . ? C16 C21 C20 116.8(10) . . ? C16 C21 H21 121.6 . . ? C20 C21 H21 121.6 . . ? C23 C22 C19 110.9(6) . . ? C23 C22 H22A 109.5 . . ? C19 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 118.4(6) . . ? C28 C23 C22 121.1(8) . . ? C24 C23 C22 120.5(7) . . ? O7 C24 C25 138.1(8) . . ? O7 C24 C23 99.7(8) . . ? C25 C24 C23 120.4(6) . . ? C25 C24 O7' 110.4(8) . . ? C23 C24 O7' 128.3(7) . . ? C24 C25 C26 121.6(7) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C27 118.2(6) . . ? C25 C26 C29 121.3(6) . . ? C27 C26 C29 120.5(5) . . ? O8 C27 C26 115.1(5) . . ? O8 C27 C28 124.1(6) . . ? C26 C27 C28 120.7(6) . . ? C23 C28 C27 120.6(6) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C26 111.3(5) . . ? C30 C29 H29A 109.4 . . ? C26 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C26 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C35 116.7(6) . . ? C31 C30 C29 121.1(6) . . ? C35 C30 C29 122.1(5) . . ? C30 C31 C32 123.4(6) . . ? C30 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C33 C32 C31 118.4(5) . . ? C33 C32 C48 122.6(6) . . ? C31 C32 C48 118.9(6) . . ? C32 C33 C34 119.4(6) . . ? C32 C33 C1 122.6(5) . . ? C34 C33 C1 117.9(6) . . ? C35 C34 C33 120.0(6) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? O9 C35 C34 123.9(6) . . ? O9 C35 C30 114.0(6) . . ? C34 C35 C30 122.1(5) . . ? O9 C36 C37 112.9(5) . . ? O9 C36 H36A 109.0 . . ? C37 C36 H36A 109.0 . . ? O9 C36 H36B 109.0 . . ? C37 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? O10 C37 O11 123.2(8) . . ? O10 C37 C36 122.5(6) . . ? O11 C37 C36 114.3(6) . . ? O11 C38 C39 109.1(6) . . ? O11 C38 H38A 109.9 . . ? C39 C38 H38A 109.9 . . ? O11 C38 H38B 109.9 . . ? C39 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O1 C40 H40A 109.5 . . ? O1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C41 H41A 109.5 . . ? O2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O5 C44 H44A 109.5 . . ? O5 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O5 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O6 C45 H45A 109.5 . . ? O6 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O6 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O8 C47 H47A 109.5 . . ? O8 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O8 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C32 131.8(5) . . ? C49 C48 S1 110.1(4) . . ? C32 C48 S1 118.1(4) . . ? C48 C49 C50 113.8(5) . . ? C48 C49 H49 123.1 . . ? C50 C49 H49 123.1 . . ? C51 C50 C49 112.8(5) . . ? C51 C50 H50 123.6 . . ? C49 C50 H50 123.6 . . ? C50 C51 C52 126.9(5) . . ? C50 C51 S1 110.8(4) . . ? C52 C51 S1 122.3(4) . . ? C53 C52 C51 124.4(5) . . ? C53 C52 H52 117.8 . . ? C51 C52 H52 117.8 . . ? C52 C53 C54 124.4(5) . . ? C52 C53 H53 117.8 . . ? C54 C53 H53 117.8 . . ? C55 C54 N1 120.3(5) . . ? C55 C54 C53 121.2(5) . . ? N1 C54 C53 118.5(5) . . ? C54 C55 C56 123.3(5) . . ? C54 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C63 C56 C55 118.0(5) . . ? C63 C56 C57 126.0(5) . . ? C55 C56 C57 116.0(4) . . ? C58 C57 C62 116.9(5) . . ? C58 C57 C56 123.9(5) . . ? C62 C57 C56 119.2(5) . . ? C59 C58 C57 122.4(5) . . ? C59 C58 H58 118.8 . . ? C57 C58 H58 118.8 . . ? C58 C59 C60 119.7(6) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C61 C60 C59 120.1(6) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C62 121.1(6) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? N1 C62 C61 120.4(5) . . ? N1 C62 C57 119.9(5) . . ? C61 C62 C57 119.7(5) . . ? C56 C63 C65 129.0(5) . . ? C56 C63 C64 118.1(5) . . ? C65 C63 C64 112.9(5) . . ? N2 C64 C63 176.8(9) . . ? N3 C65 C63 175.0(6) . . ? N1 C66 C67 112.2(6) . . ? N1 C66 H66A 109.2 . . ? C67 C66 H66A 109.2 . . ? N1 C66 H66B 109.2 . . ? C67 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? O12 C67 O13 123.5(10) . . ? O12 C67 C66 124.3(7) . . ? O13 C67 C66 112.2(9) . . ? C69 C68 O13 108.7(10) . . ? C69 C68 H68A 109.9 . . ? O13 C68 H68A 109.9 . . ? C69 C68 H68B 109.9 . . ? O13 C68 H68B 109.9 . . ? H68A C68 H68B 108.3 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C24 O7 C46 108.7(9) . . ? O7 C46 H46A 109.5 . . ? O7 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O7 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C46' O7' C24 126.0(9) . . ? O7' C46' H46D 109.5 . . ? O7' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? O7' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? 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 S1 C51 1.725(5) . ? S1 C48 1.725(5) . ? N1 C54 1.370(6) . ? N1 C62 1.399(6) . ? N1 C66 1.470(6) . ? N2 C64 1.151(7) . ? N3 C65 1.148(6) . ? O1 C7 1.381(6) . ? O1 C40 1.422(7) . ? O2 C4 1.381(6) . ? O2 C41 1.418(8) . ? O3 C11 1.387(7) . ? O3 C42 1.420(9) . ? O4 C14 1.370(6) . ? O4 C43 1.435(6) . ? O5 C17 1.388(10) . ? O5 C44 1.410(12) . ? O6 C45 1.357(14) . ? O6 C20 1.384(10) . ? O8 C27 1.366(6) . ? O8 C47 1.411(7) . ? O9 C35 1.384(6) . ? O9 C36 1.419(7) . ? O10 C37 1.198(8) . ? O11 C37 1.298(7) . ? O11 C38 1.437(7) . ? O12 C67 1.191(10) . ? O13 C67 1.277(9) . ? O13 C68 1.490(12) . ? C1 C2 1.513(9) . ? C1 C33 1.521(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.377(7) . ? C2 C7 1.393(9) . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.392(8) . ? C5 C6 1.388(7) . ? C5 C8 1.511(8) . ? C6 C7 1.384(9) . ? C6 H6 0.9500 . ? C8 C9 1.522(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.383(7) . ? C9 C14 1.388(7) . ? C10 C11 1.384(8) . ? C10 H10 0.9500 . ? C11 C12 1.377(9) . ? C12 C13 1.376(9) . ? C12 C15 1.525(8) . ? C13 C14 1.393(7) . ? C13 H13 0.9500 . ? C15 C16 1.547(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.340(14) . ? C16 C21 1.420(10) . ? C17 C18 1.399(12) . ? C18 C19 1.382(12) . ? C18 H18 0.9500 . ? C19 C20 1.332(14) . ? C19 C22 1.541(12) . ? C20 C21 1.433(12) . ? C21 H21 0.9500 . ? C22 C23 1.522(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.384(9) . ? C23 C24 1.393(11) . ? C24 O7 1.364(12) . ? C24 C25 1.377(10) . ? C24 O7' 1.512(11) . ? C25 C26 1.380(8) . ? C25 H25 0.9500 . ? C26 C27 1.386(8) . ? C26 C29 1.520(7) . ? C27 C28 1.392(8) . ? C28 H28 0.9500 . ? C29 C30 1.514(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.375(7) . ? C30 C35 1.392(8) . ? C31 C32 1.400(8) . ? C31 H31 0.9500 . ? C32 C33 1.396(8) . ? C32 C48 1.467(7) . ? C33 C34 1.396(7) . ? C34 C35 1.384(8) . ? C34 H34 0.9500 . ? C36 C37 1.502(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C38 C39 1.452(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.366(7) . ? C49 C50 1.415(7) . ? C49 H49 0.9500 . ? C50 C51 1.364(7) . ? C50 H50 0.9500 . ? C51 C52 1.444(7) . ? C52 C53 1.326(7) . ? C52 H52 0.9500 . ? C53 C54 1.465(7) . ? C53 H53 0.9500 . ? C54 C55 1.360(6) . ? C55 C56 1.408(6) . ? C55 H55 0.9500 . ? C56 C63 1.389(7) . ? C56 C57 1.458(7) . ? C57 C58 1.401(7) . ? C57 C62 1.416(7) . ? C58 C59 1.368(7) . ? C58 H58 0.9500 . ? C59 C60 1.385(8) . ? C59 H59 0.9500 . ? C60 C61 1.359(8) . ? C60 H60 0.9500 . ? C61 C62 1.402(7) . ? C61 H61 0.9500 . ? C63 C65 1.421(8) . ? C63 C64 1.422(8) . ? C66 C67 1.498(11) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 C69 1.438(13) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? O7 C46 1.432(12) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O7' C46' 1.408(12) . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? 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 C68 H68B N2 0.99 2.51 3.470(13) 164.0 1_655 C53 H53 O12 0.95 2.56 3.182(8) 123.1 . C47 H47C N2 0.98 2.52 3.442(9) 156.7 1_655 C21 H21 O3 0.95 2.46 3.212(12) 136.3 . C6 H6 O4 0.95 2.65 3.110(7) 110.1 . C68 H68B N2 0.99 2.51 3.470(13) 164.0 1_655 C53 H53 O12 0.95 2.56 3.182(8) 123.1 . C47 H47C N2 0.98 2.52 3.442(9) 156.7 1_655 C21 H21 O3 0.95 2.46 3.212(12) 136.3 . C6 H6 O4 0.95 2.65 3.110(7) 110.1 . C6 H6 O4 0.95 2.65 3.110(7) 110.1 . C21 H21 O3 0.95 2.46 3.212(12) 136.3 . C43 H43A O10 0.98 2.66 3.587(11) 157.9 . C47 H47C N2 0.98 2.52 3.442(9) 156.7 1_655 C53 H53 O12 0.95 2.56 3.182(8) 123.1 . C68 H68B N2 0.99 2.51 3.470(13) 164.0 1_655 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 C1 C2 C3 78.7(6) . . . . ? C33 C1 C2 C7 -99.0(6) . . . . ? C7 C2 C3 C4 2.2(8) . . . . ? C1 C2 C3 C4 -175.6(6) . . . . ? C41 O2 C4 C3 0.7(9) . . . . ? C41 O2 C4 C5 -178.6(6) . . . . ? C2 C3 C4 O2 179.5(5) . . . . ? C2 C3 C4 C5 -1.3(9) . . . . ? O2 C4 C5 C6 179.3(5) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? O2 C4 C5 C8 -2.9(8) . . . . ? C3 C4 C5 C8 177.8(5) . . . . ? C4 C5 C6 C7 0.3(8) . . . . ? C8 C5 C6 C7 -177.5(5) . . . . ? C40 O1 C7 C6 -10.3(8) . . . . ? C40 O1 C7 C2 168.8(5) . . . . ? C5 C6 C7 O1 179.7(5) . . . . ? C5 C6 C7 C2 0.7(8) . . . . ? C3 C2 C7 O1 179.0(5) . . . . ? C1 C2 C7 O1 -3.3(8) . . . . ? C3 C2 C7 C6 -1.9(8) . . . . ? C1 C2 C7 C6 175.8(5) . . . . ? C6 C5 C8 C9 97.9(6) . . . . ? C4 C5 C8 C9 -79.9(6) . . . . ? C5 C8 C9 C10 100.7(7) . . . . ? C5 C8 C9 C14 -77.3(7) . . . . ? C14 C9 C10 C11 0.4(10) . . . . ? C8 C9 C10 C11 -177.7(6) . . . . ? C9 C10 C11 C12 -0.2(10) . . . . ? C9 C10 C11 O3 -179.0(6) . . . . ? C42 O3 C11 C12 169.0(6) . . . . ? C42 O3 C11 C10 -12.1(10) . . . . ? C10 C11 C12 C13 -0.6(10) . . . . ? O3 C11 C12 C13 178.3(6) . . . . ? C10 C11 C12 C15 177.1(6) . . . . ? O3 C11 C12 C15 -3.9(10) . . . . ? C11 C12 C13 C14 1.2(11) . . . . ? C15 C12 C13 C14 -176.6(6) . . . . ? C43 O4 C14 C9 175.8(6) . . . . ? C43 O4 C14 C13 -5.2(10) . . . . ? C10 C9 C14 O4 179.2(6) . . . . ? C8 C9 C14 O4 -2.7(9) . . . . ? C10 C9 C14 C13 0.2(10) . . . . ? C8 C9 C14 C13 178.3(6) . . . . ? C12 C13 C14 O4 -180.0(6) . . . . ? C12 C13 C14 C9 -1.0(11) . . . . ? C13 C12 C15 C16 86.3(9) . . . . ? C11 C12 C15 C16 -91.4(10) . . . . ? C12 C15 C16 C17 -114.9(9) . . . . ? C12 C15 C16 C21 67.6(9) . . . . ? C21 C16 C17 O5 -178.4(6) . . . . ? C15 C16 C17 O5 4.2(13) . . . . ? C21 C16 C17 C18 -2.5(13) . . . . ? C15 C16 C17 C18 -179.9(6) . . . . ? C44 O5 C17 C16 -175.9(9) . . . . ? C44 O5 C17 C18 8.2(12) . . . . ? C16 C17 C18 C19 1.2(13) . . . . ? O5 C17 C18 C19 176.9(7) . . . . ? C17 C18 C19 C20 -1.1(14) . . . . ? C17 C18 C19 C22 -176.2(7) . . . . ? C18 C19 C20 O6 -180.0(6) . . . . ? C22 C19 C20 O6 -4.9(14) . . . . ? C18 C19 C20 C21 2.3(15) . . . . ? C22 C19 C20 C21 177.4(5) . . . . ? C45 O6 C20 C19 171.9(10) . . . . ? C45 O6 C20 C21 -10.2(13) . . . . ? C17 C16 C21 C20 3.5(11) . . . . ? C15 C16 C21 C20 -178.9(6) . . . . ? C19 C20 C21 C16 -3.4(12) . . . . ? O6 C20 C21 C16 178.8(6) . . . . ? C20 C19 C22 C23 -80.5(12) . . . . ? C18 C19 C22 C23 94.7(9) . . . . ? C19 C22 C23 C28 94.0(10) . . . . ? C19 C22 C23 C24 -85.1(11) . . . . ? C28 C23 C24 O7 -168.4(8) . . . . ? C22 C23 C24 O7 10.7(10) . . . . ? C28 C23 C24 C25 -0.8(12) . . . . ? C22 C23 C24 C25 178.3(7) . . . . ? C28 C23 C24 O7' 167.4(9) . . . . ? C22 C23 C24 O7' -13.5(13) . . . . ? O7 C24 C25 C26 160.5(11) . . . . ? C23 C24 C25 C26 -1.0(12) . . . . ? O7' C24 C25 C26 -171.1(8) . . . . ? C24 C25 C26 C27 1.1(11) . . . . ? C24 C25 C26 C29 -177.0(7) . . . . ? C47 O8 C27 C26 164.4(6) . . . . ? C47 O8 C27 C28 -18.3(10) . . . . ? C25 C26 C27 O8 177.9(6) . . . . ? C29 C26 C27 O8 -3.9(9) . . . . ? C25 C26 C27 C28 0.5(10) . . . . ? C29 C26 C27 C28 178.7(6) . . . . ? C24 C23 C28 C27 2.4(11) . . . . ? C22 C23 C28 C27 -176.7(6) . . . . ? O8 C27 C28 C23 -179.5(6) . . . . ? C26 C27 C28 C23 -2.4(10) . . . . ? C25 C26 C29 C30 102.4(7) . . . . ? C27 C26 C29 C30 -75.7(7) . . . . ? C26 C29 C30 C31 104.2(6) . . . . ? C26 C29 C30 C35 -73.8(7) . . . . ? C35 C30 C31 C32 -1.2(8) . . . . ? C29 C30 C31 C32 -179.3(5) . . . . ? C30 C31 C32 C33 0.5(8) . . . . ? C30 C31 C32 C48 176.5(5) . . . . ? C31 C32 C33 C34 0.3(8) . . . . ? C48 C32 C33 C34 -175.5(5) . . . . ? C31 C32 C33 C1 177.7(5) . . . . ? C48 C32 C33 C1 1.9(8) . . . . ? C2 C1 C33 C32 -114.1(6) . . . . ? C2 C1 C33 C34 63.3(6) . . . . ? C32 C33 C34 C35 -0.3(8) . . . . ? C1 C33 C34 C35 -177.9(5) . . . . ? C36 O9 C35 C34 -19.3(8) . . . . ? C36 O9 C35 C30 162.2(5) . . . . ? C33 C34 C35 O9 -178.7(5) . . . . ? C33 C34 C35 C30 -0.4(8) . . . . ? C31 C30 C35 O9 179.6(5) . . . . ? C29 C30 C35 O9 -2.3(8) . . . . ? C31 C30 C35 C34 1.1(8) . . . . ? C29 C30 C35 C34 179.2(5) . . . . ? C35 O9 C36 C37 -73.4(6) . . . . ? C38 O11 C37 O10 -5.1(12) . . . . ? C38 O11 C37 C36 175.1(6) . . . . ? O9 C36 C37 O10 -159.5(7) . . . . ? O9 C36 C37 O11 20.3(8) . . . . ? C37 O11 C38 C39 -159.5(7) . . . . ? C33 C32 C48 C49 -62.9(10) . . . . ? C31 C32 C48 C49 121.4(8) . . . . ? C33 C32 C48 S1 118.3(6) . . . . ? C31 C32 C48 S1 -57.5(7) . . . . ? C51 S1 C48 C49 -0.2(5) . . . . ? C51 S1 C48 C32 178.9(6) . . . . ? C32 C48 C49 C50 -178.7(7) . . . . ? S1 C48 C49 C50 0.1(8) . . . . ? C48 C49 C50 C51 0.0(9) . . . . ? C49 C50 C51 C52 179.4(6) . . . . ? C49 C50 C51 S1 -0.1(7) . . . . ? C48 S1 C51 C50 0.2(5) . . . . ? C48 S1 C51 C52 -179.4(5) . . . . ? C50 C51 C52 C53 179.9(6) . . . . ? S1 C51 C52 C53 -0.6(8) . . . . ? C51 C52 C53 C54 -176.6(5) . . . . ? C62 N1 C54 C55 7.2(8) . . . . ? C66 N1 C54 C55 -172.1(6) . . . . ? C62 N1 C54 C53 -172.2(5) . . . . ? C66 N1 C54 C53 8.5(8) . . . . ? C52 C53 C54 C55 22.3(8) . . . . ? C52 C53 C54 N1 -158.3(5) . . . . ? N1 C54 C55 C56 1.4(9) . . . . ? C53 C54 C55 C56 -179.2(5) . . . . ? C54 C55 C56 C63 171.6(6) . . . . ? C54 C55 C56 C57 -8.0(8) . . . . ? C63 C56 C57 C58 6.0(10) . . . . ? C55 C56 C57 C58 -174.5(6) . . . . ? C63 C56 C57 C62 -173.2(6) . . . . ? C55 C56 C57 C62 6.4(8) . . . . ? C62 C57 C58 C59 -0.9(10) . . . . ? C56 C57 C58 C59 179.9(6) . . . . ? C57 C58 C59 C60 0.2(11) . . . . ? C58 C59 C60 C61 -0.4(12) . . . . ? C59 C60 C61 C62 1.4(12) . . . . ? C54 N1 C62 C61 171.9(6) . . . . ? C66 N1 C62 C61 -8.8(9) . . . . ? C54 N1 C62 C57 -8.5(9) . . . . ? C66 N1 C62 C57 170.8(6) . . . . ? C60 C61 C62 N1 177.5(6) . . . . ? C60 C61 C62 C57 -2.1(10) . . . . ? C58 C57 C62 N1 -177.7(6) . . . . ? C56 C57 C62 N1 1.5(9) . . . . ? C58 C57 C62 C61 1.8(9) . . . . ? C56 C57 C62 C61 -178.9(6) . . . . ? C55 C56 C63 C65 174.5(6) . . . . ? C57 C56 C63 C65 -6.0(11) . . . . ? C55 C56 C63 C64 -5.6(9) . . . . ? C57 C56 C63 C64 173.9(6) . . . . ? C54 N1 C66 C67 -89.4(7) . . . . ? C62 N1 C66 C67 91.3(7) . . . . ? C68 O13 C67 O12 8.4(15) . . . . ? C68 O13 C67 C66 -168.0(8) . . . . ? N1 C66 C67 O12 32.3(12) . . . . ? N1 C66 C67 O13 -151.4(7) . . . . ? C67 O13 C68 C69 -89.8(13) . . . . ? C25 C24 O7 C46 1.6(18) . . . . ? C23 C24 O7 C46 165.5(10) . . . . ? O7' C24 O7 C46 -47.8(12) . . . . ? O7 C24 O7' C46' 139(2) . . . . ? C25 C24 O7' C46' -8.3(16) . . . . ? C23 C24 O7' C46' -177.5(12) . . . . ?