#------------------------------------------------------------------------------ #$Date: 2016-05-11 07:48:00 +0300 (Wed, 11 May 2016) $ #$Revision: 182866 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543282.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_1543282 loop_ _publ_author_name 'Rosenzweig, Michael W.' 'Scheurer, Andreas' 'Heinemann, Frank' 'Alvarez Lamsfus, Carlos' 'Maron, Laurent' 'Andrez, Julie' 'Mazzanti, M.' 'Meyer, Karsten' _publ_section_title ; Uranium(IV) Terminal Hydrosulfido and Sulfido Complexes: The Nature of the Uranium--Sulfur Bond ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C6SC00677A _journal_year 2016 _chemical_formula_moiety 'C80 H102 K N3 O9 S U, 0.62(C6 H6), 0.38(C4 H10 O)' _chemical_formula_sum 'C85.23 H109.53 K N3 O9.38 S U' _chemical_formula_weight 1635.38 _chemical_name_systematic ; ? ; _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-10-26 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2016-02-11 deposited with the CCDC. 2016-05-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.271(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.017(2) _cell_length_b 12.8557(12) _cell_length_c 28.173(3) _cell_measurement_reflns_used 9175 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 2.26 _cell_volume 7465.2(13) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 83.33 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'Quazar focussing montel optics' _diffrn_radiation_source 'ImuS micro-focus tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_unetI/netI 0.0299 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 233649 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.942 _diffrn_reflns_theta_min 0.988 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.320 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0598 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.9016. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3376 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: diethyl ether/benzene' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.302 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.096 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 949 _refine_ls_number_reflns 17883 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 1.287 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0434 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+19.9650P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0867 _reflns_Friedel_coverage 0.000 _reflns_number_gt 15242 _reflns_number_total 17883 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6sc00677a2.cif _cod_data_source_block mr1520 _cod_original_cell_volume 7465.1(12) _cod_database_code 1543282 _shelxl_version_number 2014/6 _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_max 0.836 _shelx_estimated_absorpt_t_min 0.629 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H11A,H11B,H11C} of C111, All C(H,H) groups At 1.5 times of: All C(H,H,H,H,H,H) groups, {H42A,H42B,H42C} of C42, {H24A,H24B,H24C} of C24, {H11H,H11I,H11J} of C115 2. Uiso/Uaniso restraints and constraints C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 C111 \\sim C112 \\sim O113 \\sim C114 \\sim C115: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 3. Others Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(H11C)= Sof(C112)=Sof(H11D)=Sof(H11E)=Sof(O113)=Sof(C114)=Sof(H11F)=Sof(H11G)= Sof(C115)=Sof(H11H)=Sof(H11I)=Sof(H11J)=1-FVAR(1) Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)= Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)= Sof(H106)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C15(H15), C16(H16), C17(H17), C33(H33), C34(H34), C35(H35), C51(H51), C52(H52), C53(H53) 4.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A, H43B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A, H74B), C112(H11D,H11E), C114(H11F,H11G) 4.c Aromatic/amide H refined with riding coordinates: C11(H11), C13(H13), C29(H29), C31(H31), C47(H47), C49(H49), C66(H66), C67(H67), C68(H68), C69(H69), C76(H76), C77(H77), C78(H78), C79(H79), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106) 4.d Fitted hexagon refined as free rotating group: C101(C102,C103,C104,C105,C106) 4.e Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C), C60(H60D,H60E, H60F), C111(H11A,H11B,H11C), C115(H11H,H11I,H11J) ; _shelx_res_file ; TITL MR1520,P2(1)/c,ROSENZWEIG/MEYER,[U((Ad_ArO)3tacn)S(K18bz_c6)]*solv CELL 0.71073 21.0169 12.8557 28.1726 90 101.2709 90 ZERR 4 0.002 0.0012 0.0027 0 0.0025 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S K U UNIT 340.93 438.13 12 37.53 4 4 4 SIMU 0.005 0.01 2 C101 > C106 SIMU 0.005 0.01 2 C111 > C115 L.S. 8 PLAN 20 SIZE 0.22 0.13 0.08 TEMP -173 BOND .5 $H HTAB CONF WPDB -1 LIST 4 CONF HTAB MORE -1 fmap 2 acta REM REM REM WGHT 0.013500 19.964998 FVAR 0.05563 0.61689 U1 7 0.740629 0.693990 -0.061223 11.00000 0.01310 0.02030 = 0.02694 -0.00124 0.00205 -0.00293 K1 6 0.791731 0.913025 0.102988 11.00000 0.03498 0.03230 = 0.03215 0.00571 0.00826 0.00460 S1 5 0.762460 0.849203 -0.006565 11.00000 0.02412 0.03016 = 0.03480 -0.00788 0.00449 -0.00484 O1 4 0.679801 0.635100 -0.010659 11.00000 0.02196 0.01921 = 0.02932 0.00324 0.00633 -0.00261 O2 4 0.678474 0.781336 -0.118942 11.00000 0.02142 0.01906 = 0.03256 0.00069 -0.00648 -0.00365 O3 4 0.847158 0.692968 -0.062299 11.00000 0.01489 0.02854 = 0.03373 -0.00516 0.00474 -0.00072 O4 4 0.678759 1.018579 0.101951 11.00000 0.03972 0.02929 = 0.03097 0.00977 0.01701 0.00774 O5 4 0.777649 1.121011 0.068349 11.00000 0.02771 0.03116 = 0.03646 0.00367 0.00397 0.00044 O6 4 0.896780 1.054348 0.115178 11.00000 0.03289 0.02764 = 0.05029 0.00189 -0.00640 -0.00325 O7 4 0.902006 0.917383 0.184549 11.00000 0.03910 0.04137 = 0.03378 0.00037 -0.00339 0.00627 O8 4 0.814031 0.749217 0.166604 11.00000 0.04217 0.03825 = 0.04694 0.00742 0.00675 0.00711 O9 4 0.699119 0.858218 0.159205 11.00000 0.04287 0.02822 = 0.03511 0.00999 0.01685 0.00772 N1 3 0.752994 0.486180 -0.047794 11.00000 0.01508 0.02187 = 0.03238 -0.00097 0.00138 -0.00095 N2 3 0.643476 0.563965 -0.118968 11.00000 0.01565 0.01777 = 0.02646 -0.00346 0.00452 -0.00382 N3 3 0.773603 0.576639 -0.139638 11.00000 0.01625 0.02064 = 0.03352 -0.00352 0.00523 -0.00165 C1 1 0.695046 0.419054 -0.065267 11.00000 0.02029 0.01961 = 0.03343 -0.00039 0.00548 -0.00250 AFIX 23 H1A 2 0.687110 0.375614 -0.037995 11.00000 -1.20000 H1B 2 0.704942 0.371659 -0.090558 11.00000 -1.20000 AFIX 0 C2 1 0.633062 0.479057 -0.085925 11.00000 0.01818 0.01913 = 0.03170 -0.00194 0.00568 -0.00548 AFIX 23 H2A 2 0.600502 0.430090 -0.103640 11.00000 -1.20000 H2B 2 0.615208 0.508793 -0.058862 11.00000 -1.20000 AFIX 0 C3 1 0.658406 0.520906 -0.164473 11.00000 0.01900 0.02046 = 0.03135 -0.00933 0.00477 -0.00454 AFIX 23 H3A 2 0.619939 0.528899 -0.190807 11.00000 -1.20000 H3B 2 0.667787 0.445657 -0.160158 11.00000 -1.20000 AFIX 0 C4 1 0.715812 0.574618 -0.178882 11.00000 0.02092 0.02401 = 0.02859 -0.00578 0.00524 -0.00387 AFIX 23 H4A 2 0.726793 0.538367 -0.207226 11.00000 -1.20000 H4B 2 0.703505 0.646935 -0.188729 11.00000 -1.20000 AFIX 0 C5 1 0.797077 0.470584 -0.124413 11.00000 0.01799 0.02220 = 0.04454 -0.00514 0.01119 -0.00179 AFIX 23 H5A 2 0.838235 0.457662 -0.135539 11.00000 -1.20000 H5B 2 0.764908 0.419049 -0.140415 11.00000 -1.20000 AFIX 0 C6 1 0.808279 0.454236 -0.069780 11.00000 0.01787 0.02057 = 0.04306 0.00015 0.00503 0.00014 AFIX 23 H6A 2 0.817379 0.379672 -0.062722 11.00000 -1.20000 H6B 2 0.847154 0.494141 -0.054397 11.00000 -1.20000 AFIX 0 C7 1 0.774763 0.480383 0.005988 11.00000 0.02133 0.02674 = 0.03778 0.00032 -0.00168 0.00344 AFIX 23 H7A 2 0.807055 0.536179 0.016030 11.00000 -1.20000 H7B 2 0.797304 0.413147 0.013918 11.00000 -1.20000 AFIX 0 C8 1 0.723169 0.489884 0.035941 11.00000 0.02218 0.02452 = 0.02822 -0.00265 0.00206 -0.00240 C9 1 0.677402 0.570568 0.026085 11.00000 0.02341 0.01987 = 0.02725 0.00097 0.00180 -0.00539 C10 1 0.628894 0.580259 0.055099 11.00000 0.02917 0.01972 = 0.02765 -0.00109 0.00483 -0.00134 C11 1 0.631863 0.510422 0.093224 11.00000 0.03757 0.02485 = 0.02841 -0.00234 0.00833 -0.00556 AFIX 43 H11 2 0.600193 0.516321 0.112958 11.00000 -1.20000 AFIX 0 C12 1 0.678121 0.432903 0.104156 11.00000 0.04580 0.02476 = 0.02711 0.00376 0.00404 -0.00281 C13 1 0.722843 0.422688 0.074347 11.00000 0.03479 0.02715 = 0.03513 0.00275 -0.00118 0.00349 AFIX 43 H13 2 0.754032 0.368372 0.080349 11.00000 -1.20000 AFIX 0 C14 1 0.576137 0.663484 0.044180 11.00000 0.02713 0.01766 = 0.03475 0.00322 0.01339 0.00048 C15 1 0.484996 0.731419 -0.021309 11.00000 0.02404 0.03017 = 0.03937 0.00955 0.00994 0.00117 AFIX 13 H15 2 0.461108 0.720301 -0.055267 11.00000 -1.20000 AFIX 0 C16 1 0.553287 0.856114 0.034693 11.00000 0.03497 0.02120 = 0.05081 0.00546 0.02246 0.00058 AFIX 13 H16 2 0.573754 0.926638 0.037489 11.00000 -1.20000 AFIX 0 C17 1 0.474316 0.740825 0.065217 11.00000 0.03597 0.02965 = 0.04744 0.00725 0.02416 0.00199 AFIX 13 H17 2 0.443386 0.735765 0.087956 11.00000 -1.20000 AFIX 0 C18 1 0.536913 0.648462 -0.007757 11.00000 0.02153 0.02239 = 0.03445 0.00261 0.01018 -0.00147 AFIX 23 H18A 2 0.566818 0.650926 -0.030871 11.00000 -1.20000 H18B 2 0.516130 0.579041 -0.010371 11.00000 -1.20000 AFIX 0 C19 1 0.527554 0.658810 0.078875 11.00000 0.03502 0.02302 = 0.03776 0.00370 0.01759 -0.00281 AFIX 23 H19A 2 0.507656 0.588787 0.077359 11.00000 -1.20000 H19B 2 0.550897 0.670892 0.112491 11.00000 -1.20000 AFIX 0 C20 1 0.517814 0.839671 -0.016669 11.00000 0.02772 0.02844 = 0.05467 0.01675 0.01794 0.00563 AFIX 23 H20A 2 0.548731 0.844332 -0.038969 11.00000 -1.20000 H20B 2 0.484558 0.894488 -0.025664 11.00000 -1.20000 AFIX 0 C21 1 0.504490 0.849838 0.068845 11.00000 0.04039 0.02665 = 0.05491 0.00608 0.02381 0.00765 AFIX 23 H21A 2 0.526870 0.863643 0.102556 11.00000 -1.20000 H21B 2 0.470126 0.902838 0.059608 11.00000 -1.20000 AFIX 0 C22 1 0.606048 0.774024 0.048480 11.00000 0.02985 0.01761 = 0.03452 0.00031 0.01270 -0.00179 AFIX 23 H22A 2 0.629296 0.786006 0.082130 11.00000 -1.20000 H22B 2 0.637810 0.779935 0.026889 11.00000 -1.20000 AFIX 0 C23 1 0.437829 0.722696 0.014006 11.00000 0.02348 0.02998 = 0.05924 0.02017 0.01783 0.00498 AFIX 23 H23A 2 0.402820 0.774918 0.005592 11.00000 -1.20000 H23B 2 0.417772 0.652728 0.011460 11.00000 -1.20000 AFIX 0 C24 1 0.679100 0.362989 0.147504 11.00000 0.07113 0.03405 = 0.03412 0.00723 0.01019 0.00769 AFIX 137 H24A 2 0.634971 0.338873 0.147894 11.00000 -1.50000 H24B 2 0.695801 0.401868 0.177252 11.00000 -1.50000 H24C 2 0.707162 0.302949 0.145440 11.00000 -1.50000 AFIX 0 C25 1 0.583564 0.628792 -0.129915 11.00000 0.01545 0.02194 = 0.02895 -0.00209 0.00346 -0.00315 AFIX 23 H25A 2 0.577031 0.662307 -0.099593 11.00000 -1.20000 H25B 2 0.545998 0.582509 -0.141175 11.00000 -1.20000 AFIX 0 C26 1 0.584276 0.711603 -0.167262 11.00000 0.01666 0.02201 = 0.02310 -0.00288 0.00545 0.00042 C27 1 0.632074 0.789397 -0.158449 11.00000 0.01557 0.02061 = 0.02648 -0.00564 0.00208 0.00273 C28 1 0.630521 0.874299 -0.190851 11.00000 0.01859 0.02589 = 0.02422 -0.00444 0.00790 -0.00208 C29 1 0.582157 0.872703 -0.232748 11.00000 0.03023 0.02512 = 0.02075 -0.00130 0.00801 0.00258 AFIX 43 H29 2 0.581511 0.927082 -0.255671 11.00000 -1.20000 AFIX 0 C30 1 0.534910 0.795500 -0.242584 11.00000 0.02428 0.03216 = 0.02094 -0.00652 0.00308 0.00283 C31 1 0.536301 0.716483 -0.209114 11.00000 0.01451 0.02694 = 0.02388 -0.00784 0.00483 -0.00330 AFIX 43 H31 2 0.503762 0.664183 -0.214756 11.00000 -1.20000 AFIX 0 C32 1 0.676855 0.966817 -0.177898 11.00000 0.03031 0.02579 = 0.03058 -0.00328 0.00836 -0.00865 C33 1 0.711140 1.145204 -0.201786 11.00000 0.09919 0.04657 = 0.04724 0.00588 0.01369 -0.04379 AFIX 13 H33 2 0.702805 1.199623 -0.227620 11.00000 -1.20000 AFIX 0 C34 1 0.710448 1.108571 -0.114853 11.00000 0.05280 0.02388 = 0.03529 -0.00402 -0.00005 -0.00973 AFIX 13 H34 2 0.701688 1.139067 -0.084111 11.00000 -1.20000 AFIX 0 C35 1 0.793671 1.027792 -0.154720 11.00000 0.03512 0.06488 = 0.08634 -0.01531 0.02102 -0.02816 AFIX 13 H35 2 0.840007 1.005094 -0.149821 11.00000 -1.20000 AFIX 0 C36 1 0.665281 1.052103 -0.216852 11.00000 0.06790 0.03518 = 0.03051 -0.00145 0.01187 -0.02068 AFIX 23 H36A 2 0.619673 1.075938 -0.221731 11.00000 -1.20000 H36B 2 0.672793 1.023331 -0.247886 11.00000 -1.20000 AFIX 0 C37 1 0.748695 0.932719 -0.170329 11.00000 0.02777 0.04453 = 0.06148 -0.01735 0.01959 -0.01488 AFIX 23 H37A 2 0.757752 0.903205 -0.200782 11.00000 -1.20000 H37B 2 0.757349 0.878198 -0.145071 11.00000 -1.20000 AFIX 0 C38 1 0.698447 1.190459 -0.154796 11.00000 0.07774 0.03152 = 0.04671 -0.00139 -0.00024 -0.02299 AFIX 23 H38A 2 0.653008 1.215060 -0.159501 11.00000 -1.20000 H38B 2 0.727373 1.250800 -0.145209 11.00000 -1.20000 AFIX 0 C39 1 0.779636 1.069856 -0.106967 11.00000 0.04282 0.03849 = 0.06397 -0.01014 -0.00185 -0.02694 AFIX 23 H39A 2 0.786161 1.014122 -0.082240 11.00000 -1.20000 H39B 2 0.809859 1.127459 -0.095143 11.00000 -1.20000 AFIX 0 C40 1 0.664413 1.015928 -0.130356 11.00000 0.02945 0.02232 = 0.02686 -0.00150 0.00167 -0.00327 AFIX 23 H40A 2 0.618865 1.040016 -0.135100 11.00000 -1.20000 H40B 2 0.671110 0.962776 -0.104428 11.00000 -1.20000 AFIX 0 C41 1 0.780829 1.110865 -0.194546 11.00000 0.09142 0.07164 = 0.07502 -0.01263 0.03911 -0.05714 AFIX 23 H41A 2 0.809852 1.171181 -0.185173 11.00000 -1.20000 H41B 2 0.789850 1.081965 -0.225128 11.00000 -1.20000 AFIX 0 C42 1 0.482552 0.800835 -0.287712 11.00000 0.03604 0.04429 = 0.02467 -0.00130 -0.00335 0.00007 AFIX 137 H42A 2 0.491456 0.858992 -0.307939 11.00000 -1.50000 H42B 2 0.440335 0.811289 -0.278595 11.00000 -1.50000 H42C 2 0.481923 0.735684 -0.305857 11.00000 -1.50000 AFIX 0 C43 1 0.824176 0.636346 -0.158445 11.00000 0.02188 0.03302 = 0.02991 -0.00418 0.00703 -0.00606 AFIX 23 H43A 2 0.810283 0.709956 -0.162278 11.00000 -1.20000 H43B 2 0.826420 0.609394 -0.190995 11.00000 -1.20000 AFIX 0 C44 1 0.890925 0.632736 -0.127724 11.00000 0.01766 0.02463 = 0.04171 -0.00442 0.00783 -0.00633 C45 1 0.899550 0.665323 -0.079622 11.00000 0.01649 0.02026 = 0.03769 -0.00149 0.00607 -0.00328 C46 1 0.963269 0.667565 -0.050716 11.00000 0.01738 0.01891 = 0.04436 -0.00099 0.00464 -0.00358 C47 1 1.013803 0.631538 -0.072147 11.00000 0.01672 0.02839 = 0.05561 -0.00937 0.00687 -0.00476 AFIX 43 H47 2 1.056405 0.631386 -0.053067 11.00000 -1.20000 AFIX 0 C48 1 1.005763 0.596107 -0.119336 11.00000 0.02166 0.03728 = 0.05843 -0.01052 0.01646 -0.00334 C49 1 0.943229 0.597419 -0.146996 11.00000 0.02812 0.03751 = 0.04162 -0.01007 0.01334 -0.00839 AFIX 43 H49 2 0.936048 0.573850 -0.179568 11.00000 -1.20000 AFIX 0 C50 1 0.975932 0.711687 0.000157 11.00000 0.01225 0.02495 = 0.04388 -0.00437 -0.00057 -0.00308 C51 1 1.059922 0.753185 0.075898 11.00000 0.02009 0.04766 = 0.05555 -0.00756 -0.01231 -0.00361 AFIX 13 H51 2 1.107087 0.748479 0.090812 11.00000 -1.20000 AFIX 0 C52 1 0.948379 0.700356 0.083411 11.00000 0.03628 0.07388 = 0.03653 -0.00278 -0.00305 -0.01932 AFIX 13 H52 2 0.921901 0.662230 0.103674 11.00000 -1.20000 AFIX 0 C53 1 0.967075 0.874075 0.048685 11.00000 0.02359 0.03920 = 0.05534 -0.01899 0.00041 0.00248 AFIX 13 H53 2 0.953083 0.948556 0.046530 11.00000 -1.20000 AFIX 0 C54 1 1.048648 0.705430 0.025266 11.00000 0.01869 0.02688 = 0.05517 -0.00692 -0.00284 -0.00001 AFIX 23 H54A 2 1.062595 0.631744 0.027630 11.00000 -1.20000 H54B 2 1.075292 0.742751 0.005384 11.00000 -1.20000 AFIX 0 C55 1 0.955675 0.827091 -0.001899 11.00000 0.01917 0.02509 = 0.04497 -0.00536 0.00352 0.00144 AFIX 23 H55A 2 0.981061 0.866131 -0.022126 11.00000 -1.20000 H55B 2 0.909174 0.833113 -0.017038 11.00000 -1.20000 AFIX 0 C56 1 1.020783 0.693514 0.107316 11.00000 0.04121 0.06553 = 0.04731 -0.00136 -0.01492 -0.00808 AFIX 23 H56A 2 1.027927 0.724083 0.140185 11.00000 -1.20000 H56B 2 1.034777 0.619868 0.110172 11.00000 -1.20000 AFIX 0 C57 1 0.927125 0.814260 0.078585 11.00000 0.02920 0.07301 = 0.04192 -0.02348 -0.00157 -0.00629 AFIX 23 H57A 2 0.880687 0.818216 0.063022 11.00000 -1.20000 H57B 2 0.932346 0.845951 0.111145 11.00000 -1.20000 AFIX 0 C58 1 0.937877 0.651401 0.032770 11.00000 0.02226 0.03949 = 0.04226 0.00266 -0.00514 -0.01157 AFIX 23 H58A 2 0.891067 0.652270 0.018080 11.00000 -1.20000 H58B 2 0.952494 0.578053 0.035410 11.00000 -1.20000 AFIX 0 C59 1 1.039527 0.867582 0.072284 11.00000 0.02243 0.03802 = 0.06092 -0.02148 -0.00567 -0.00301 AFIX 23 H59A 2 1.065698 0.906258 0.052504 11.00000 -1.20000 H59B 2 1.046897 0.899124 0.104959 11.00000 -1.20000 AFIX 0 C60 1 1.063375 0.558095 -0.139748 11.00000 0.02799 0.06944 = 0.07527 -0.02553 0.02370 -0.00422 PART 1 AFIX 137 H60A 2 1.084436 0.617446 -0.152140 21.00000 -1.50000 H60B 2 1.048409 0.508844 -0.166118 21.00000 -1.50000 H60C 2 1.094445 0.523473 -0.114153 21.00000 -1.50000 AFIX 137 PART 0 PART 2 H60D 2 1.054640 0.487691 -0.152730 -21.00000 -1.50000 H60E 2 1.102187 0.557187 -0.114000 -21.00000 -1.50000 H60F 2 1.070463 0.604885 -0.165682 -21.00000 -1.50000 AFIX 0 PART 0 C61 1 0.665952 1.104478 0.068583 11.00000 0.03494 0.03045 = 0.03198 0.01068 0.01010 0.00400 AFIX 23 H61A 2 0.668076 1.170948 0.086568 11.00000 -1.20000 H61B 2 0.622056 1.097663 0.048261 11.00000 -1.20000 AFIX 0 C62 1 0.716097 1.103083 0.037477 11.00000 0.02756 0.03206 = 0.03216 0.00661 0.00733 -0.00337 AFIX 23 H62A 2 0.715981 1.034943 0.021088 11.00000 -1.20000 H62B 2 0.706877 1.158060 0.012469 11.00000 -1.20000 AFIX 0 C63 1 0.829573 1.115376 0.043132 11.00000 0.03122 0.03417 = 0.04410 0.01053 0.00724 -0.00399 AFIX 23 H63A 2 0.824093 1.168452 0.017189 11.00000 -1.20000 H63B 2 0.830756 1.045875 0.028195 11.00000 -1.20000 AFIX 0 C64 1 0.891107 1.134560 0.079030 11.00000 0.03596 0.02823 = 0.05743 0.00737 0.00153 -0.00534 AFIX 23 H64A 2 0.928771 1.132425 0.062737 11.00000 -1.20000 H64B 2 0.889771 1.203821 0.094166 11.00000 -1.20000 AFIX 0 C65 1 0.953454 1.052333 0.149324 11.00000 0.03679 0.03184 = 0.04659 -0.01409 -0.00456 0.00276 C66 1 1.005237 1.119230 0.149470 11.00000 0.04517 0.03647 = 0.06021 -0.00873 -0.00732 -0.00604 AFIX 43 H66 2 1.002540 1.171713 0.125420 11.00000 -1.20000 AFIX 0 C67 1 1.060588 1.109437 0.184551 11.00000 0.04881 0.06359 = 0.05831 -0.01626 -0.01123 -0.01397 AFIX 43 H67 2 1.095976 1.155447 0.184615 11.00000 -1.20000 AFIX 0 C68 1 1.065037 1.034365 0.219153 11.00000 0.04582 0.08501 = 0.05102 -0.01555 -0.01762 -0.00472 AFIX 43 H68 2 1.103701 1.027551 0.242881 11.00000 -1.20000 AFIX 0 C69 1 1.013421 0.968021 0.219843 11.00000 0.04987 0.06145 = 0.03368 -0.01120 -0.00840 0.00698 AFIX 43 H69 2 1.016853 0.916146 0.244227 11.00000 -1.20000 AFIX 0 C70 1 0.956786 0.976329 0.185400 11.00000 0.03860 0.04006 = 0.03612 -0.01419 -0.00319 0.00680 C71 1 0.909042 0.824732 0.213363 11.00000 0.05262 0.05497 = 0.03786 0.00758 -0.00791 0.01329 AFIX 23 H71A 2 0.931156 0.840800 0.246908 11.00000 -1.20000 H71B 2 0.935330 0.772828 0.199762 11.00000 -1.20000 AFIX 0 C72 1 0.842243 0.782385 0.213049 11.00000 0.06080 0.05482 = 0.03542 0.01771 0.00561 0.01265 AFIX 23 H72A 2 0.845069 0.723314 0.235911 11.00000 -1.20000 H72B 2 0.814959 0.837048 0.223707 11.00000 -1.20000 AFIX 0 C73 1 0.753262 0.697499 0.163299 11.00000 0.04268 0.03694 = 0.05429 0.02196 0.00203 0.01558 AFIX 23 H73A 2 0.760722 0.631047 0.181285 11.00000 -1.20000 H73B 2 0.736016 0.680515 0.128916 11.00000 -1.20000 AFIX 0 C74 1 0.702633 0.758753 0.182583 11.00000 0.04597 0.03995 = 0.04337 0.02012 0.01504 0.00715 AFIX 23 H74A 2 0.660116 0.723063 0.174966 11.00000 -1.20000 H74B 2 0.715277 0.766844 0.218126 11.00000 -1.20000 AFIX 0 C75 1 0.647825 0.920597 0.164440 11.00000 0.04309 0.02981 = 0.03436 0.00885 0.01832 0.00954 C76 1 0.607506 0.903909 0.196920 11.00000 0.05283 0.04155 = 0.03620 0.01551 0.02310 0.01227 AFIX 43 H76 2 0.615072 0.846470 0.218503 11.00000 -1.20000 AFIX 0 C77 1 0.556086 0.970468 0.198202 11.00000 0.06674 0.05180 = 0.04534 0.01755 0.03870 0.01903 AFIX 43 H77 2 0.528379 0.957862 0.220488 11.00000 -1.20000 AFIX 0 C78 1 0.544667 1.054544 0.167612 11.00000 0.06521 0.04778 = 0.04890 0.01720 0.03617 0.02848 AFIX 43 H78 2 0.509116 1.099562 0.168642 11.00000 -1.20000 AFIX 0 C79 1 0.585383 1.073475 0.135121 11.00000 0.05952 0.03246 = 0.04248 0.01376 0.02735 0.01742 AFIX 43 H79 2 0.577831 1.131877 0.114112 11.00000 -1.20000 AFIX 0 C80 1 0.636760 1.007557 0.133338 11.00000 0.04229 0.02910 = 0.03174 0.00913 0.01979 0.00698 PART 1 AFIX 66 C101 1 0.789201 0.349508 0.700817 21.00000 0.07636 0.09863 = 0.08118 -0.01363 0.00751 0.00748 AFIX 43 H101 2 0.747074 0.361699 0.682176 21.00000 -1.20000 AFIX 65 C102 1 0.833150 0.288663 0.682134 21.00000 0.07814 0.10008 = 0.07283 -0.01521 0.00814 0.00799 AFIX 43 H102 2 0.821061 0.259269 0.650724 21.00000 -1.20000 AFIX 65 C103 1 0.894789 0.270825 0.709409 21.00000 0.07845 0.10226 = 0.07498 -0.01232 0.00957 0.00727 AFIX 43 H103 2 0.924826 0.229240 0.696640 21.00000 -1.20000 AFIX 65 C104 1 0.912478 0.313832 0.755366 21.00000 0.07452 0.10119 = 0.07360 -0.01196 0.01082 -0.00154 AFIX 43 H104 2 0.954605 0.301641 0.774007 21.00000 -1.20000 AFIX 65 C105 1 0.868530 0.374678 0.774049 21.00000 0.07410 0.09394 = 0.07354 -0.02275 0.01453 -0.00474 AFIX 43 H105 2 0.880620 0.404071 0.805459 21.00000 -1.20000 AFIX 65 C106 1 0.806891 0.392516 0.746775 21.00000 0.08160 0.09514 = 0.08885 -0.02932 0.01536 0.00772 AFIX 43 H106 2 0.776855 0.434101 0.759544 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C111 1 0.898798 0.294881 0.750342 -21.00000 0.06320 0.09561 = 0.04266 0.03282 0.00091 0.00055 AFIX 137 H11A 2 0.937828 0.313882 0.738160 -21.00000 -1.20000 H11B 2 0.891962 0.219582 0.747253 -21.00000 -1.20000 H11C 2 0.904215 0.314894 0.784462 -21.00000 -1.20000 AFIX 0 C112 1 0.847658 0.344217 0.724713 -21.00000 0.06182 0.06430 = 0.04890 0.01416 0.01139 -0.00382 AFIX 23 H11D 2 0.844172 0.325824 0.690177 -21.00000 -1.20000 H11E 2 0.855666 0.420032 0.727797 -21.00000 -1.20000 AFIX 0 O113 4 0.789091 0.323125 0.737708 -21.00000 0.06787 0.05592 = 0.05014 0.00734 0.01235 -0.00213 C114 1 0.738888 0.382614 0.716056 -21.00000 0.06638 0.04215 = 0.04310 -0.00131 0.01501 0.00436 AFIX 23 H11F 2 0.731287 0.371271 0.680638 -21.00000 -1.20000 H11G 2 0.749948 0.456852 0.722336 -21.00000 -1.20000 AFIX 0 C115 1 0.678691 0.358075 0.733925 -21.00000 0.07611 0.04526 = 0.05040 -0.00415 0.00940 0.01181 AFIX 137 H11H 2 0.644298 0.406538 0.719538 -21.00000 -1.50000 H11I 2 0.686895 0.364768 0.769249 -21.00000 -1.50000 H11J 2 0.665129 0.286716 0.724788 -21.00000 -1.50000 AFIX 0 HKLF 4 REM MR1520,P2(1)/c,ROSENZWEIG/MEYER,[U((Ad_ArO)3tacn)S(K18bz_c6)]*solv REM R1 = 0.0434 for 15242 Fo > 4sig(Fo) and 0.0561 for all 17883 data REM 949 parameters refined using 60 restraints END WGHT 0.0135 19.9878 REM Instructions for potential hydrogen bonds HTAB C2 O1 HTAB C6 O3 REM Highest difference peak 1.302, deepest hole -0.973, 1-sigma level 0.096 Q1 1 0.7792 0.9173 0.1852 11.00000 0.05 1.30 Q2 1 0.7781 0.8537 0.0835 11.00000 0.05 1.22 Q3 1 0.7658 0.6428 -0.0564 11.00000 0.05 1.14 Q4 1 0.7446 0.7088 -0.0355 11.00000 0.05 0.77 Q5 1 0.7892 0.4223 0.7146 11.00000 0.05 0.74 Q6 1 0.8436 0.4462 0.7562 11.00000 0.05 0.66 Q7 1 0.7202 0.5394 -0.1147 11.00000 0.05 0.64 Q8 1 0.7034 0.7525 -0.0659 11.00000 0.05 0.64 Q9 1 0.7619 0.6498 -0.0885 11.00000 0.05 0.64 Q10 1 0.8788 0.3564 0.7699 11.00000 0.05 0.64 Q11 1 0.6912 0.4763 -0.2222 11.00000 0.05 0.62 Q12 1 0.7503 0.6595 -0.0983 11.00000 0.05 0.62 Q13 1 0.7305 0.6406 -0.0983 11.00000 0.05 0.58 Q14 1 0.7778 0.7381 -0.0579 11.00000 0.05 0.56 Q15 1 0.7297 0.7463 -0.0971 11.00000 0.05 0.54 Q16 1 0.7316 0.9569 -0.0614 11.00000 0.05 0.52 Q17 1 0.8058 0.7835 0.1924 11.00000 0.05 0.51 Q18 1 0.7591 0.7239 0.1906 11.00000 0.05 0.50 Q19 1 0.8046 1.0621 -0.1813 11.00000 0.05 0.48 Q20 1 0.7548 0.7588 0.1314 11.00000 0.05 0.48 ; _shelx_res_checksum 57487 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 U1 U 0.74063(2) 0.69399(2) -0.06122(2) 0.02037(4) Uani 1 1 d . . . . . K1 K 0.79173(5) 0.91303(7) 0.10299(3) 0.0329(2) Uani 1 1 d . . . . . S1 S 0.76246(5) 0.84920(8) -0.00656(4) 0.0299(2) Uani 1 1 d . . . . . O1 O 0.67980(12) 0.6351(2) -0.01066(9) 0.0233(6) Uani 1 1 d . . . . . O2 O 0.67847(12) 0.78134(19) -0.11894(10) 0.0259(6) Uani 1 1 d . . . . . O3 O 0.84716(11) 0.6930(2) -0.06230(10) 0.0257(6) Uani 1 1 d . . . . . O4 O 0.67876(14) 1.0186(2) 0.10195(10) 0.0320(7) Uani 1 1 d . . . . . O5 O 0.77765(13) 1.1210(2) 0.06835(11) 0.0321(7) Uani 1 1 d . . . . . O6 O 0.89678(14) 1.0543(2) 0.11518(12) 0.0389(8) Uani 1 1 d . . . . . O7 O 0.90201(15) 0.9174(3) 0.18455(11) 0.0395(7) Uani 1 1 d . . . . . O8 O 0.81403(16) 0.7492(3) 0.16660(12) 0.0427(8) Uani 1 1 d . . . . . O9 O 0.69912(15) 0.8582(2) 0.15920(11) 0.0341(7) Uani 1 1 d . . . . . N1 N 0.75299(14) 0.4862(2) -0.04779(12) 0.0236(7) Uani 1 1 d . . . . . N2 N 0.64348(14) 0.5640(2) -0.11897(11) 0.0199(6) Uani 1 1 d . . . . . N3 N 0.77360(14) 0.5766(2) -0.13964(12) 0.0234(7) Uani 1 1 d . . . . . C1 C 0.69505(17) 0.4191(3) -0.06527(15) 0.0244(8) Uani 1 1 d . . . . . H1A H 0.6871 0.3756 -0.0380 0.029 Uiso 1 1 calc R . . . . H1B H 0.7049 0.3717 -0.0906 0.029 Uiso 1 1 calc R . . . . C2 C 0.63306(17) 0.4791(3) -0.08593(14) 0.0229(8) Uani 1 1 d . . . . . H2A H 0.6005 0.4301 -0.1036 0.027 Uiso 1 1 calc R . . . . H2B H 0.6152 0.5088 -0.0589 0.027 Uiso 1 1 calc R . . . . C3 C 0.65841(17) 0.5209(3) -0.16447(14) 0.0236(8) Uani 1 1 d . . . . . H3A H 0.6199 0.5289 -0.1908 0.028 Uiso 1 1 calc R . . . . H3B H 0.6678 0.4457 -0.1602 0.028 Uiso 1 1 calc R . . . . C4 C 0.71581(18) 0.5746(3) -0.17888(14) 0.0245(8) Uani 1 1 d . . . . . H4A H 0.7268 0.5384 -0.2072 0.029 Uiso 1 1 calc R . . . . H4B H 0.7035 0.6469 -0.1887 0.029 Uiso 1 1 calc R . . . . C5 C 0.79708(18) 0.4706(3) -0.12441(15) 0.0276(9) Uani 1 1 d . . . . . H5A H 0.8382 0.4577 -0.1355 0.033 Uiso 1 1 calc R . . . . H5B H 0.7649 0.4190 -0.1404 0.033 Uiso 1 1 calc R . . . . C6 C 0.80828(18) 0.4542(3) -0.06978(15) 0.0273(9) Uani 1 1 d . . . . . H6A H 0.8174 0.3797 -0.0627 0.033 Uiso 1 1 calc R . . . . H6B H 0.8472 0.4941 -0.0544 0.033 Uiso 1 1 calc R . . . . C7 C 0.77476(19) 0.4804(3) 0.00599(15) 0.0296(9) Uani 1 1 d . . . . . H7A H 0.8071 0.5362 0.0160 0.036 Uiso 1 1 calc R . . . . H7B H 0.7973 0.4131 0.0139 0.036 Uiso 1 1 calc R . . . . C8 C 0.72317(18) 0.4899(3) 0.03594(14) 0.0254(8) Uani 1 1 d . . . . . C9 C 0.67740(18) 0.5706(3) 0.02609(14) 0.0239(8) Uani 1 1 d . . . . . C10 C 0.62889(19) 0.5803(3) 0.05510(14) 0.0256(8) Uani 1 1 d . . . . . C11 C 0.6319(2) 0.5104(3) 0.09322(15) 0.0300(9) Uani 1 1 d . . . . . H11 H 0.6002 0.5163 0.1130 0.036 Uiso 1 1 calc R . . . . C12 C 0.6781(2) 0.4329(3) 0.10416(15) 0.0330(10) Uani 1 1 d . . . . . C13 C 0.7228(2) 0.4227(3) 0.07435(15) 0.0334(9) Uani 1 1 d . . . . . H13 H 0.7540 0.3684 0.0803 0.040 Uiso 1 1 calc R . . . . C14 C 0.57614(19) 0.6635(3) 0.04418(15) 0.0255(8) Uani 1 1 d . . . . . C15 C 0.48500(19) 0.7314(3) -0.02131(16) 0.0307(9) Uani 1 1 d . . . . . H15 H 0.4611 0.7203 -0.0553 0.037 Uiso 1 1 calc R . . . . C16 C 0.5533(2) 0.8561(3) 0.03469(17) 0.0338(10) Uani 1 1 d . . . . . H16 H 0.5738 0.9266 0.0375 0.041 Uiso 1 1 calc R . . . . C17 C 0.4743(2) 0.7408(3) 0.06522(17) 0.0355(10) Uani 1 1 d . . . . . H17 H 0.4434 0.7358 0.0880 0.043 Uiso 1 1 calc R . . . . C18 C 0.53691(18) 0.6485(3) -0.00776(15) 0.0255(8) Uani 1 1 d . . . . . H18A H 0.5668 0.6509 -0.0309 0.031 Uiso 1 1 calc R . . . . H18B H 0.5161 0.5790 -0.0104 0.031 Uiso 1 1 calc R . . . . C19 C 0.5276(2) 0.6588(3) 0.07887(16) 0.0305(9) Uani 1 1 d . . . . . H19A H 0.5077 0.5888 0.0774 0.037 Uiso 1 1 calc R . . . . H19B H 0.5509 0.6709 0.1125 0.037 Uiso 1 1 calc R . . . . C20 C 0.5178(2) 0.8397(3) -0.01667(17) 0.0356(10) Uani 1 1 d . . . . . H20A H 0.5487 0.8443 -0.0390 0.043 Uiso 1 1 calc R . . . . H20B H 0.4846 0.8945 -0.0257 0.043 Uiso 1 1 calc R . . . . C21 C 0.5045(2) 0.8498(3) 0.06885(19) 0.0387(11) Uani 1 1 d . . . . . H21A H 0.5269 0.8636 0.1026 0.046 Uiso 1 1 calc R . . . . H21B H 0.4701 0.9028 0.0596 0.046 Uiso 1 1 calc R . . . . C22 C 0.60605(19) 0.7740(3) 0.04848(15) 0.0265(8) Uani 1 1 d . . . . . H22A H 0.6293 0.7860 0.0821 0.032 Uiso 1 1 calc R . . . . H22B H 0.6378 0.7799 0.0269 0.032 Uiso 1 1 calc R . . . . C23 C 0.4378(2) 0.7227(3) 0.01401(17) 0.0362(11) Uani 1 1 d . . . . . H23A H 0.4028 0.7749 0.0056 0.043 Uiso 1 1 calc R . . . . H23B H 0.4178 0.6527 0.0115 0.043 Uiso 1 1 calc R . . . . C24 C 0.6791(3) 0.3630(4) 0.14750(17) 0.0464(12) Uani 1 1 d . . . . . H24A H 0.6350 0.3389 0.1479 0.070 Uiso 1 1 calc GR . . . . H24B H 0.6958 0.4019 0.1773 0.070 Uiso 1 1 calc GR . . . . H24C H 0.7072 0.3029 0.1454 0.070 Uiso 1 1 calc GR . . . . C25 C 0.58356(17) 0.6288(3) -0.12992(14) 0.0222(8) Uani 1 1 d . . . . . H25A H 0.5770 0.6623 -0.0996 0.027 Uiso 1 1 calc R . . . . H25B H 0.5460 0.5825 -0.1412 0.027 Uiso 1 1 calc R . . . . C26 C 0.58428(17) 0.7116(3) -0.16726(13) 0.0204(7) Uani 1 1 d . . . . . C27 C 0.63207(17) 0.7894(3) -0.15845(13) 0.0212(8) Uani 1 1 d . . . . . C28 C 0.63052(17) 0.8743(3) -0.19085(14) 0.0224(8) Uani 1 1 d . . . . . C29 C 0.58216(19) 0.8727(3) -0.23275(14) 0.0250(8) Uani 1 1 d . . . . . H29 H 0.5815 0.9271 -0.2557 0.030 Uiso 1 1 calc R . . . . C30 C 0.53491(18) 0.7955(3) -0.24258(13) 0.0260(8) Uani 1 1 d . . . . . C31 C 0.53630(17) 0.7165(3) -0.20911(13) 0.0216(8) Uani 1 1 d . . . . . H31 H 0.5038 0.6642 -0.2148 0.026 Uiso 1 1 calc R . . . . C32 C 0.6769(2) 0.9668(3) -0.17790(15) 0.0286(9) Uani 1 1 d . . . . . C33 C 0.7111(3) 1.1452(4) -0.2018(2) 0.0644(18) Uani 1 1 d . . . . . H33 H 0.7028 1.1996 -0.2276 0.077 Uiso 1 1 calc R . . . . C34 C 0.7104(2) 1.1086(3) -0.11485(17) 0.0385(11) Uani 1 1 d . . . . . H34 H 0.7017 1.1391 -0.0841 0.046 Uiso 1 1 calc R . . . . C35 C 0.7937(3) 1.0278(5) -0.1547(2) 0.0609(16) Uani 1 1 d . . . . . H35 H 0.8400 1.0051 -0.1498 0.073 Uiso 1 1 calc R . . . . C36 C 0.6653(3) 1.0521(4) -0.21685(17) 0.0442(12) Uani 1 1 d . . . . . H36A H 0.6197 1.0759 -0.2217 0.053 Uiso 1 1 calc R . . . . H36B H 0.6728 1.0233 -0.2479 0.053 Uiso 1 1 calc R . . . . C37 C 0.7487(2) 0.9327(4) -0.1703(2) 0.0431(12) Uani 1 1 d . . . . . H37A H 0.7578 0.9032 -0.2008 0.052 Uiso 1 1 calc R . . . . H37B H 0.7573 0.8782 -0.1451 0.052 Uiso 1 1 calc R . . . . C38 C 0.6984(3) 1.1905(4) -0.15480(18) 0.0537(14) Uani 1 1 d . . . . . H38A H 0.6530 1.2151 -0.1595 0.064 Uiso 1 1 calc R . . . . H38B H 0.7274 1.2508 -0.1452 0.064 Uiso 1 1 calc R . . . . C39 C 0.7796(2) 1.0699(4) -0.1070(2) 0.0501(13) Uani 1 1 d . . . . . H39A H 0.7862 1.0141 -0.0822 0.060 Uiso 1 1 calc R . . . . H39B H 0.8099 1.1275 -0.0951 0.060 Uiso 1 1 calc R . . . . C40 C 0.6644(2) 1.0159(3) -0.13036(14) 0.0267(8) Uani 1 1 d . . . . . H40A H 0.6189 1.0400 -0.1351 0.032 Uiso 1 1 calc R . . . . H40B H 0.6711 0.9628 -0.1044 0.032 Uiso 1 1 calc R . . . . C41 C 0.7808(3) 1.1109(5) -0.1945(2) 0.076(2) Uani 1 1 d . . . . . H41A H 0.8099 1.1712 -0.1852 0.092 Uiso 1 1 calc R . . . . H41B H 0.7898 1.0820 -0.2251 0.092 Uiso 1 1 calc R . . . . C42 C 0.4826(2) 0.8008(4) -0.28771(14) 0.0363(10) Uani 1 1 d . . . . . H42A H 0.4915 0.8590 -0.3079 0.054 Uiso 1 1 calc GR . . . . H42B H 0.4403 0.8113 -0.2786 0.054 Uiso 1 1 calc GR . . . . H42C H 0.4819 0.7357 -0.3059 0.054 Uiso 1 1 calc GR . . . . C43 C 0.82418(18) 0.6363(3) -0.15845(15) 0.0280(9) Uani 1 1 d . . . . . H43A H 0.8103 0.7100 -0.1623 0.034 Uiso 1 1 calc R . . . . H43B H 0.8264 0.6094 -0.1910 0.034 Uiso 1 1 calc R . . . . C44 C 0.89092(18) 0.6327(3) -0.12772(16) 0.0277(9) Uani 1 1 d . . . . . C45 C 0.89955(18) 0.6653(3) -0.07962(15) 0.0247(8) Uani 1 1 d . . . . . C46 C 0.96327(18) 0.6676(3) -0.05072(16) 0.0271(9) Uani 1 1 d . . . . . C47 C 1.01380(19) 0.6315(3) -0.07215(17) 0.0336(10) Uani 1 1 d . . . . . H47 H 1.0564 0.6314 -0.0531 0.040 Uiso 1 1 calc R . . . . C48 C 1.0058(2) 0.5961(4) -0.11934(18) 0.0380(11) Uani 1 1 d . . . . . C49 C 0.9432(2) 0.5974(4) -0.14700(17) 0.0349(10) Uani 1 1 d . . . . . H49 H 0.9360 0.5739 -0.1796 0.042 Uiso 1 1 calc R . . . . C50 C 0.97593(17) 0.7117(3) 0.00016(16) 0.0278(9) Uani 1 1 d . . . . . C51 C 1.0599(2) 0.7532(4) 0.07590(19) 0.0438(12) Uani 1 1 d . . . . . H51 H 1.1071 0.7485 0.0908 0.053 Uiso 1 1 calc R . . . . C52 C 0.9484(2) 0.7004(5) 0.08341(17) 0.0503(13) Uani 1 1 d . . . . . H52 H 0.9219 0.6622 0.1037 0.060 Uiso 1 1 calc R . . . . C53 C 0.9671(2) 0.8741(4) 0.04869(18) 0.0404(11) Uani 1 1 d . . . . . H53 H 0.9531 0.9486 0.0465 0.048 Uiso 1 1 calc R . . . . C54 C 1.04865(19) 0.7054(3) 0.02527(17) 0.0349(10) Uani 1 1 d . . . . . H54A H 1.0626 0.6317 0.0276 0.042 Uiso 1 1 calc R . . . . H54B H 1.0753 0.7428 0.0054 0.042 Uiso 1 1 calc R . . . . C55 C 0.95567(19) 0.8271(3) -0.00190(16) 0.0301(9) Uani 1 1 d . . . . . H55A H 0.9811 0.8661 -0.0221 0.036 Uiso 1 1 calc R . . . . H55B H 0.9092 0.8331 -0.0170 0.036 Uiso 1 1 calc R . . . . C56 C 1.0208(2) 0.6935(5) 0.10732(19) 0.0545(14) Uani 1 1 d . . . . . H56A H 1.0279 0.7241 0.1402 0.065 Uiso 1 1 calc R . . . . H56B H 1.0348 0.6199 0.1102 0.065 Uiso 1 1 calc R . . . . C57 C 0.9271(2) 0.8143(5) 0.07859(18) 0.0492(13) Uani 1 1 d . . . . . H57A H 0.8807 0.8182 0.0630 0.059 Uiso 1 1 calc R . . . . H57B H 0.9323 0.8460 0.1111 0.059 Uiso 1 1 calc R . . . . C58 C 0.9379(2) 0.6514(4) 0.03277(16) 0.0362(10) Uani 1 1 d . . . . . H58A H 0.8911 0.6523 0.0181 0.043 Uiso 1 1 calc R . . . . H58B H 0.9525 0.5781 0.0354 0.043 Uiso 1 1 calc R . . . . C59 C 1.0395(2) 0.8676(4) 0.07228(19) 0.0423(12) Uani 1 1 d . . . . . H59A H 1.0657 0.9063 0.0525 0.051 Uiso 1 1 calc R . . . . H59B H 1.0469 0.8991 0.1050 0.051 Uiso 1 1 calc R . . . . C60 C 1.0634(2) 0.5581(5) -0.1397(2) 0.0557(15) Uani 1 1 d . . . . . H60A H 1.0844 0.6174 -0.1521 0.084 Uiso 0.617(6) 1 calc GR . P A 1 H60B H 1.0484 0.5088 -0.1661 0.084 Uiso 0.617(6) 1 calc GR . P A 1 H60C H 1.0944 0.5235 -0.1142 0.084 Uiso 0.617(6) 1 calc GR . P A 1 H60D H 1.0546 0.4877 -0.1527 0.084 Uiso 0.383(6) 1 calc GR . P A 2 H60E H 1.1022 0.5572 -0.1140 0.084 Uiso 0.383(6) 1 calc GR . P A 2 H60F H 1.0705 0.6049 -0.1657 0.084 Uiso 0.383(6) 1 calc GR . P A 2 C61 C 0.6660(2) 1.1045(3) 0.06858(15) 0.0320(9) Uani 1 1 d . . . . . H61A H 0.6681 1.1709 0.0866 0.038 Uiso 1 1 calc R . . . . H61B H 0.6221 1.0977 0.0483 0.038 Uiso 1 1 calc R . . . . C62 C 0.71610(19) 1.1031(3) 0.03748(15) 0.0304(9) Uani 1 1 d . . . . . H62A H 0.7160 1.0349 0.0211 0.036 Uiso 1 1 calc R . . . . H62B H 0.7069 1.1581 0.0125 0.036 Uiso 1 1 calc R . . . . C63 C 0.8296(2) 1.1154(4) 0.04313(17) 0.0365(10) Uani 1 1 d . . . . . H63A H 0.8241 1.1685 0.0172 0.044 Uiso 1 1 calc R . . . . H63B H 0.8308 1.0459 0.0282 0.044 Uiso 1 1 calc R . . . . C64 C 0.8911(2) 1.1346(4) 0.07903(18) 0.0416(11) Uani 1 1 d . . . . . H64A H 0.9288 1.1324 0.0627 0.050 Uiso 1 1 calc R . . . . H64B H 0.8898 1.2038 0.0942 0.050 Uiso 1 1 calc R . . . . C65 C 0.9535(2) 1.0523(4) 0.14932(18) 0.0401(11) Uani 1 1 d . . . . . C66 C 1.0052(2) 1.1192(4) 0.1495(2) 0.0497(13) Uani 1 1 d . . . . . H66 H 1.0025 1.1717 0.1254 0.060 Uiso 1 1 calc R . . . . C67 C 1.0606(3) 1.1094(5) 0.1846(2) 0.0598(16) Uani 1 1 d . . . . . H67 H 1.0960 1.1554 0.1846 0.072 Uiso 1 1 calc R . . . . C68 C 1.0650(3) 1.0344(5) 0.2192(2) 0.0643(17) Uani 1 1 d . . . . . H68 H 1.1037 1.0276 0.2429 0.077 Uiso 1 1 calc R . . . . C69 C 1.0134(3) 0.9680(5) 0.21984(18) 0.0506(13) Uani 1 1 d . . . . . H69 H 1.0169 0.9161 0.2442 0.061 Uiso 1 1 calc R . . . . C70 C 0.9568(2) 0.9763(4) 0.18540(17) 0.0397(11) Uani 1 1 d . . . . . C71 C 0.9090(3) 0.8247(4) 0.21336(18) 0.0508(14) Uani 1 1 d . . . . . H71A H 0.9312 0.8408 0.2469 0.061 Uiso 1 1 calc R . . . . H71B H 0.9353 0.7728 0.1998 0.061 Uiso 1 1 calc R . . . . C72 C 0.8422(3) 0.7824(4) 0.21305(18) 0.0509(14) Uani 1 1 d . . . . . H72A H 0.8451 0.7233 0.2359 0.061 Uiso 1 1 calc R . . . . H72B H 0.8150 0.8370 0.2237 0.061 Uiso 1 1 calc R . . . . C73 C 0.7533(2) 0.6975(4) 0.16330(19) 0.0456(12) Uani 1 1 d . . . . . H73A H 0.7607 0.6310 0.1813 0.055 Uiso 1 1 calc R . . . . H73B H 0.7360 0.6805 0.1289 0.055 Uiso 1 1 calc R . . . . C74 C 0.7026(2) 0.7588(4) 0.18258(18) 0.0422(12) Uani 1 1 d . . . . . H74A H 0.6601 0.7231 0.1750 0.051 Uiso 1 1 calc R . . . . H74B H 0.7153 0.7668 0.2181 0.051 Uiso 1 1 calc R . . . . C75 C 0.6478(2) 0.9206(3) 0.16444(16) 0.0343(10) Uani 1 1 d . . . . . C76 C 0.6075(2) 0.9039(4) 0.19692(17) 0.0416(11) Uani 1 1 d . . . . . H76 H 0.6151 0.8465 0.2185 0.050 Uiso 1 1 calc R . . . . C77 C 0.5561(3) 0.9705(4) 0.19820(18) 0.0509(14) Uani 1 1 d . . . . . H77 H 0.5284 0.9579 0.2205 0.061 Uiso 1 1 calc R . . . . C78 C 0.5447(3) 1.0545(4) 0.16761(18) 0.0506(14) Uani 1 1 d . . . . . H78 H 0.5091 1.0996 0.1686 0.061 Uiso 1 1 calc R . . . . C79 C 0.5854(2) 1.0735(4) 0.13512(17) 0.0425(12) Uani 1 1 d . . . . . H79 H 0.5778 1.1319 0.1141 0.051 Uiso 1 1 calc R . . . . C80 C 0.6368(2) 1.0076(3) 0.13334(15) 0.0327(10) Uani 1 1 d . . . . . C101 C 0.7892(3) 0.3495(7) 0.7008(3) 0.086(3) Uani 0.617(6) 1 d . U P A 1 H101 H 0.7471 0.3617 0.6822 0.104 Uiso 0.617(6) 1 calc R . P A 1 C102 C 0.8332(4) 0.2887(7) 0.6821(2) 0.085(3) Uani 0.617(6) 1 d G U P A 1 H102 H 0.8211 0.2593 0.6507 0.101 Uiso 0.617(6) 1 calc R . P A 1 C103 C 0.8948(4) 0.2708(7) 0.7094(3) 0.086(3) Uani 0.617(6) 1 d G U P A 1 H103 H 0.9248 0.2292 0.6966 0.103 Uiso 0.617(6) 1 calc R . P A 1 C104 C 0.9125(3) 0.3138(8) 0.7554(3) 0.084(3) Uani 0.617(6) 1 d G U P A 1 H104 H 0.9546 0.3016 0.7740 0.100 Uiso 0.617(6) 1 calc R . P A 1 C105 C 0.8685(4) 0.3747(7) 0.7740(2) 0.081(2) Uani 0.617(6) 1 d G U P A 1 H105 H 0.8806 0.4041 0.8055 0.097 Uiso 0.617(6) 1 calc R . P A 1 C106 C 0.8069(4) 0.3925(7) 0.7468(3) 0.089(3) Uani 0.617(6) 1 d G U P A 1 H106 H 0.7769 0.4341 0.7595 0.106 Uiso 0.617(6) 1 calc R . P A 1 C111 C 0.8988(9) 0.2949(17) 0.7503(6) 0.068(4) Uani 0.383(6) 1 d . U P A 2 H11A H 0.9378 0.3139 0.7382 0.082 Uiso 0.383(6) 1 calc GR . P A 2 H11B H 0.8920 0.2196 0.7473 0.082 Uiso 0.383(6) 1 calc GR . P A 2 H11C H 0.9042 0.3149 0.7845 0.082 Uiso 0.383(6) 1 calc GR . P A 2 C112 C 0.8477(7) 0.3442(13) 0.7247(5) 0.058(3) Uani 0.383(6) 1 d . U P A 2 H11D H 0.8442 0.3258 0.6902 0.070 Uiso 0.383(6) 1 calc R . P A 2 H11E H 0.8557 0.4200 0.7278 0.070 Uiso 0.383(6) 1 calc R . P A 2 O113 O 0.7891(5) 0.3231(8) 0.7377(4) 0.058(2) Uani 0.383(6) 1 d . U P A 2 C114 C 0.7389(7) 0.3826(11) 0.7161(5) 0.050(3) Uani 0.383(6) 1 d . U P A 2 H11F H 0.7313 0.3713 0.6806 0.060 Uiso 0.383(6) 1 calc R . P A 2 H11G H 0.7499 0.4569 0.7223 0.060 Uiso 0.383(6) 1 calc R . P A 2 C115 C 0.6787(8) 0.3581(12) 0.7339(5) 0.058(4) Uani 0.383(6) 1 d . U P A 2 H11H H 0.6443 0.4065 0.7195 0.086 Uiso 0.383(6) 1 calc GR . P A 2 H11I H 0.6869 0.3648 0.7692 0.086 Uiso 0.383(6) 1 calc GR . P A 2 H11J H 0.6651 0.2867 0.7248 0.086 Uiso 0.383(6) 1 calc GR . 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 U1 0.01310(6) 0.02030(7) 0.02694(7) -0.00124(6) 0.00205(4) -0.00293(6) K1 0.0350(5) 0.0323(5) 0.0321(5) 0.0057(4) 0.0083(4) 0.0046(4) S1 0.0241(5) 0.0302(5) 0.0348(6) -0.0079(4) 0.0045(4) -0.0048(4) O1 0.0220(13) 0.0192(13) 0.0293(14) 0.0032(11) 0.0063(11) -0.0026(11) O2 0.0214(13) 0.0191(14) 0.0326(15) 0.0007(11) -0.0065(11) -0.0036(10) O3 0.0149(12) 0.0285(14) 0.0337(14) -0.0052(13) 0.0047(10) -0.0007(12) O4 0.0397(17) 0.0293(15) 0.0310(15) 0.0098(13) 0.0170(13) 0.0077(13) O5 0.0277(15) 0.0312(16) 0.0365(17) 0.0037(13) 0.0040(13) 0.0004(12) O6 0.0329(16) 0.0276(16) 0.050(2) 0.0019(14) -0.0064(14) -0.0033(13) O7 0.0391(18) 0.0414(18) 0.0338(17) 0.0004(14) -0.0034(14) 0.0063(15) O8 0.0422(19) 0.0382(19) 0.047(2) 0.0074(15) 0.0067(15) 0.0071(15) O9 0.0429(18) 0.0282(16) 0.0351(17) 0.0100(13) 0.0169(14) 0.0077(13) N1 0.0151(15) 0.0219(16) 0.0324(18) -0.0010(13) 0.0014(13) -0.0009(12) N2 0.0157(14) 0.0178(15) 0.0265(16) -0.0035(13) 0.0045(12) -0.0038(12) N3 0.0163(15) 0.0206(16) 0.0335(18) -0.0035(14) 0.0052(13) -0.0016(13) C1 0.0203(18) 0.0196(18) 0.033(2) -0.0004(16) 0.0055(16) -0.0025(15) C2 0.0182(17) 0.0191(18) 0.032(2) -0.0019(16) 0.0057(15) -0.0055(14) C3 0.0190(18) 0.0205(19) 0.031(2) -0.0093(16) 0.0048(15) -0.0045(15) C4 0.0209(18) 0.0240(19) 0.029(2) -0.0058(16) 0.0052(15) -0.0039(15) C5 0.0180(18) 0.0222(19) 0.045(2) -0.0051(18) 0.0112(17) -0.0018(15) C6 0.0179(18) 0.0206(19) 0.043(2) 0.0002(17) 0.0050(17) 0.0001(15) C7 0.0213(19) 0.027(2) 0.038(2) 0.0003(18) -0.0017(17) 0.0034(16) C8 0.0222(19) 0.025(2) 0.028(2) -0.0026(16) 0.0021(16) -0.0024(16) C9 0.0234(19) 0.0199(19) 0.027(2) 0.0010(15) 0.0018(15) -0.0054(15) C10 0.029(2) 0.0197(19) 0.028(2) -0.0011(16) 0.0048(16) -0.0013(16) C11 0.038(2) 0.025(2) 0.028(2) -0.0023(17) 0.0083(18) -0.0056(18) C12 0.046(3) 0.025(2) 0.027(2) 0.0038(17) 0.0040(19) -0.0028(19) C13 0.035(2) 0.027(2) 0.035(2) 0.0027(18) -0.0012(18) 0.0035(18) C14 0.027(2) 0.0177(18) 0.035(2) 0.0032(16) 0.0134(17) 0.0005(15) C15 0.024(2) 0.030(2) 0.039(2) 0.0095(18) 0.0099(18) 0.0012(17) C16 0.035(2) 0.021(2) 0.051(3) 0.0055(19) 0.022(2) 0.0006(18) C17 0.036(2) 0.030(2) 0.047(3) 0.007(2) 0.024(2) 0.0020(19) C18 0.0215(19) 0.0224(19) 0.034(2) 0.0026(17) 0.0102(16) -0.0015(15) C19 0.035(2) 0.023(2) 0.038(2) 0.0037(17) 0.0176(19) -0.0028(17) C20 0.028(2) 0.028(2) 0.055(3) 0.017(2) 0.018(2) 0.0056(17) C21 0.040(3) 0.027(2) 0.055(3) 0.006(2) 0.024(2) 0.008(2) C22 0.030(2) 0.0176(18) 0.035(2) 0.0003(16) 0.0127(17) -0.0018(15) C23 0.023(2) 0.030(2) 0.059(3) 0.020(2) 0.018(2) 0.0050(17) C24 0.071(4) 0.034(3) 0.034(3) 0.007(2) 0.010(2) 0.008(2) C25 0.0154(17) 0.0219(19) 0.029(2) -0.0021(15) 0.0035(15) -0.0032(14) C26 0.0167(16) 0.0220(19) 0.0231(18) -0.0029(15) 0.0055(14) 0.0004(14) C27 0.0156(16) 0.0206(19) 0.0265(19) -0.0056(15) 0.0021(14) 0.0027(14) C28 0.0186(17) 0.0259(19) 0.0242(19) -0.0044(16) 0.0079(15) -0.0021(15) C29 0.030(2) 0.025(2) 0.0208(19) -0.0013(16) 0.0080(16) 0.0026(16) C30 0.0243(18) 0.032(2) 0.0209(18) -0.0065(17) 0.0031(15) 0.0028(17) C31 0.0145(16) 0.027(2) 0.0239(18) -0.0078(15) 0.0048(14) -0.0033(14) C32 0.030(2) 0.026(2) 0.031(2) -0.0033(17) 0.0084(17) -0.0086(17) C33 0.099(5) 0.047(3) 0.047(3) 0.006(3) 0.014(3) -0.044(3) C34 0.053(3) 0.024(2) 0.035(2) -0.0040(18) 0.000(2) -0.010(2) C35 0.035(3) 0.065(4) 0.086(4) -0.015(3) 0.021(3) -0.028(3) C36 0.068(3) 0.035(3) 0.031(2) -0.001(2) 0.012(2) -0.021(2) C37 0.028(2) 0.045(3) 0.061(3) -0.017(2) 0.020(2) -0.015(2) C38 0.078(4) 0.032(3) 0.047(3) -0.001(2) 0.000(3) -0.023(3) C39 0.043(3) 0.038(3) 0.064(3) -0.010(2) -0.002(2) -0.027(2) C40 0.029(2) 0.022(2) 0.027(2) -0.0015(16) 0.0017(16) -0.0033(16) C41 0.091(5) 0.072(4) 0.075(4) -0.013(4) 0.039(4) -0.057(4) C42 0.036(2) 0.044(3) 0.025(2) -0.001(2) -0.0034(17) 0.000(2) C43 0.0219(19) 0.033(2) 0.030(2) -0.0042(18) 0.0070(16) -0.0061(17) C44 0.0177(18) 0.025(2) 0.042(2) -0.0044(18) 0.0078(17) -0.0063(15) C45 0.0165(17) 0.0203(19) 0.038(2) -0.0015(16) 0.0061(16) -0.0033(14) C46 0.0174(18) 0.0189(19) 0.044(2) -0.0010(16) 0.0046(17) -0.0036(14) C47 0.0167(18) 0.028(2) 0.056(3) -0.009(2) 0.0069(18) -0.0048(16) C48 0.022(2) 0.037(2) 0.058(3) -0.011(2) 0.016(2) -0.0033(18) C49 0.028(2) 0.038(2) 0.042(3) -0.010(2) 0.0133(19) -0.0084(19) C50 0.0122(16) 0.025(2) 0.044(2) -0.0044(17) -0.0006(16) -0.0031(15) C51 0.020(2) 0.048(3) 0.056(3) -0.008(2) -0.012(2) -0.004(2) C52 0.036(3) 0.074(4) 0.037(3) -0.003(3) -0.003(2) -0.019(3) C53 0.024(2) 0.039(3) 0.055(3) -0.019(2) 0.000(2) 0.0025(19) C54 0.0187(18) 0.027(2) 0.055(3) -0.007(2) -0.0028(18) 0.0000(17) C55 0.0192(18) 0.025(2) 0.045(2) -0.0054(18) 0.0035(17) 0.0014(15) C56 0.041(3) 0.066(4) 0.047(3) -0.001(3) -0.015(2) -0.008(3) C57 0.029(2) 0.073(4) 0.042(3) -0.023(3) -0.002(2) -0.006(3) C58 0.022(2) 0.039(2) 0.042(3) 0.003(2) -0.0051(18) -0.0116(18) C59 0.022(2) 0.038(3) 0.061(3) -0.021(2) -0.006(2) -0.0030(19) C60 0.028(2) 0.069(4) 0.075(4) -0.026(3) 0.024(3) -0.004(2) C61 0.035(2) 0.030(2) 0.032(2) 0.0107(18) 0.0101(18) 0.0040(18) C62 0.028(2) 0.032(2) 0.032(2) 0.0066(18) 0.0073(17) -0.0034(17) C63 0.031(2) 0.034(2) 0.044(3) 0.011(2) 0.007(2) -0.0040(19) C64 0.036(2) 0.028(2) 0.057(3) 0.007(2) 0.002(2) -0.0053(19) C65 0.037(2) 0.032(2) 0.047(3) -0.014(2) -0.005(2) 0.003(2) C66 0.045(3) 0.036(3) 0.060(3) -0.009(2) -0.007(2) -0.006(2) C67 0.049(3) 0.064(4) 0.058(4) -0.016(3) -0.011(3) -0.014(3) C68 0.046(3) 0.085(5) 0.051(3) -0.016(3) -0.018(3) -0.005(3) C69 0.050(3) 0.061(3) 0.034(3) -0.011(2) -0.008(2) 0.007(3) C70 0.039(3) 0.040(3) 0.036(2) -0.014(2) -0.003(2) 0.007(2) C71 0.053(3) 0.055(3) 0.038(3) 0.008(2) -0.008(2) 0.013(3) C72 0.061(3) 0.055(3) 0.035(3) 0.018(2) 0.006(2) 0.013(3) C73 0.043(3) 0.037(3) 0.054(3) 0.022(2) 0.002(2) 0.016(2) C74 0.046(3) 0.040(3) 0.043(3) 0.020(2) 0.015(2) 0.007(2) C75 0.043(2) 0.030(2) 0.034(2) 0.0088(19) 0.018(2) 0.010(2) C76 0.053(3) 0.042(3) 0.036(2) 0.016(2) 0.023(2) 0.012(2) C77 0.067(4) 0.052(3) 0.045(3) 0.018(2) 0.039(3) 0.019(3) C78 0.065(3) 0.048(3) 0.049(3) 0.017(2) 0.036(3) 0.028(3) C79 0.060(3) 0.032(2) 0.042(3) 0.014(2) 0.027(2) 0.017(2) C80 0.042(2) 0.029(2) 0.032(2) 0.0091(18) 0.0198(19) 0.0070(19) C101 0.076(5) 0.099(5) 0.081(5) -0.014(4) 0.008(4) 0.007(4) C102 0.078(5) 0.100(5) 0.073(5) -0.015(4) 0.008(4) 0.008(4) C103 0.078(5) 0.102(5) 0.075(5) -0.012(4) 0.010(4) 0.007(4) C104 0.075(5) 0.101(6) 0.074(5) -0.012(4) 0.011(4) -0.002(4) C105 0.074(5) 0.094(5) 0.074(5) -0.023(4) 0.015(4) -0.005(4) C106 0.082(5) 0.095(5) 0.089(5) -0.029(4) 0.015(4) 0.008(4) C111 0.063(8) 0.096(9) 0.043(7) 0.033(7) 0.001(6) 0.001(8) C112 0.062(6) 0.064(6) 0.049(5) 0.014(5) 0.011(5) -0.004(5) O113 0.068(5) 0.056(5) 0.050(5) 0.007(4) 0.012(4) -0.002(4) C114 0.066(6) 0.042(5) 0.043(5) -0.001(4) 0.015(4) 0.004(4) C115 0.076(8) 0.045(7) 0.050(7) -0.004(6) 0.009(6) 0.012(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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 S1 U1 N1 134.38(7) S1 U1 N2 146.34(6) S1 U1 N3 148.04(7) O1 U1 S1 86.37(7) O1 U1 O3 134.92(10) O1 U1 N1 68.02(9) O1 U1 N2 74.44(9) O1 U1 N3 124.72(9) O2 U1 S1 93.39(7) O2 U1 O1 108.45(10) O2 U1 O3 116.45(10) O2 U1 N1 129.69(9) O2 U1 N2 67.90(9) O2 U1 N3 84.06(10) O3 U1 S1 87.12(7) O3 U1 N1 85.83(10) O3 U1 N2 125.96(9) O3 U1 N3 66.11(9) N1 U1 N2 62.88(9) N1 U1 N3 63.72(10) N3 U1 N2 60.77(8) S1 K1 C57 72.92(9) S1 K1 C62 70.17(8) S1 K1 C63 73.88(9) S1 K1 C72 135.46(10) S1 K1 C73 104.86(10) O4 K1 S1 96.70(7) O4 K1 O5 59.78(8) O4 K1 O6 109.80(9) O4 K1 O7 123.52(9) O4 K1 O8 115.17(10) O4 K1 O9 55.77(8) O4 K1 C57 165.95(12) O4 K1 C62 45.48(9) O4 K1 C63 84.15(10) O4 K1 C72 111.11(11) O4 K1 C73 96.79(10) O5 K1 S1 85.47(7) O5 K1 O7 105.36(9) O5 K1 C57 109.01(12) O5 K1 C62 25.75(9) O5 K1 C63 25.46(10) O5 K1 C72 138.43(12) O5 K1 C73 155.74(11) O6 K1 S1 106.61(8) O6 K1 O5 57.57(8) O6 K1 O7 54.05(9) O6 K1 O9 134.31(10) O6 K1 C57 65.73(12) O6 K1 C62 82.57(10) O6 K1 C63 44.86(10) O6 K1 C72 96.09(12) O6 K1 C73 135.49(11) O7 K1 S1 138.61(7) O7 K1 C57 65.76(10) O7 K1 C62 130.51(10) O7 K1 C63 98.86(11) O7 K1 C72 42.11(11) O7 K1 C73 81.59(11) O8 K1 S1 114.67(8) O8 K1 O5 159.86(10) O8 K1 O6 112.57(10) O8 K1 O7 59.63(10) O8 K1 O9 59.45(9) O8 K1 C57 78.30(13) O8 K1 C62 160.20(10) O8 K1 C63 156.34(11) O8 K1 C72 21.73(12) O8 K1 C73 23.56(10) O9 K1 S1 117.51(7) O9 K1 O5 112.94(9) O9 K1 O7 95.23(9) O9 K1 C57 137.29(12) O9 K1 C62 100.94(9) O9 K1 C63 138.40(10) O9 K1 C72 60.50(11) O9 K1 C73 42.81(10) C57 K1 C72 82.87(13) C57 K1 C73 95.08(13) C62 K1 C57 120.72(13) C62 K1 C63 42.24(10) C62 K1 C72 152.23(12) C62 K1 C73 138.21(11) C63 K1 C57 83.84(13) C63 K1 C72 140.61(13) C63 K1 C73 178.53(13) C73 K1 C72 40.01(13) U1 S1 K1 142.16(5) C9 O1 U1 145.2(2) C27 O2 U1 153.4(2) C45 O3 U1 154.3(2) C61 O4 K1 116.0(2) C80 O4 K1 127.5(2) C80 O4 C61 115.9(3) C62 O5 K1 94.5(2) C63 O5 K1 94.9(2) C63 O5 C62 112.4(3) C64 O6 K1 114.8(2) C65 O6 K1 128.4(3) C65 O6 C64 116.7(4) C70 O7 K1 123.8(3) C70 O7 C71 117.1(4) C71 O7 K1 114.0(3) C72 O8 K1 111.4(3) C72 O8 C73 114.5(4) C73 O8 K1 106.2(2) C74 O9 K1 120.0(2) C75 O9 K1 123.7(2) C75 O9 C74 116.2(3) C1 N1 U1 118.3(2) C1 N1 C7 111.9(3) C6 N1 U1 106.1(2) C6 N1 C1 111.0(3) C6 N1 C7 107.5(3) C7 N1 U1 101.1(2) C2 N2 U1 104.4(2) C2 N2 C3 110.5(3) C2 N2 C25 108.7(3) C3 N2 U1 117.2(2) C3 N2 C25 110.0(3) C25 N2 U1 105.6(2) C4 N3 U1 107.4(2) C4 N3 C5 112.3(3) C4 N3 C43 106.4(3) C5 N3 U1 112.1(2) C5 N3 C43 110.9(3) C43 N3 U1 107.4(2) N1 C1 H1A 108.7 N1 C1 H1B 108.7 N1 C1 C2 114.4(3) H1A C1 H1B 107.6 C2 C1 H1A 108.7 C2 C1 H1B 108.7 N2 C2 C1 113.1(3) N2 C2 H2A 109.0 N2 C2 H2B 109.0 C1 C2 H2A 109.0 C1 C2 H2B 109.0 H2A C2 H2B 107.8 N2 C3 H3A 109.2 N2 C3 H3B 109.2 N2 C3 C4 112.1(3) H3A C3 H3B 107.9 C4 C3 H3A 109.2 C4 C3 H3B 109.2 N3 C4 C3 113.0(3) N3 C4 H4A 109.0 N3 C4 H4B 109.0 C3 C4 H4A 109.0 C3 C4 H4B 109.0 H4A C4 H4B 107.8 N3 C5 H5A 108.9 N3 C5 H5B 108.9 N3 C5 C6 113.3(3) H5A C5 H5B 107.7 C6 C5 H5A 108.9 C6 C5 H5B 108.9 N1 C6 C5 113.9(3) N1 C6 H6A 108.8 N1 C6 H6B 108.8 C5 C6 H6A 108.8 C5 C6 H6B 108.8 H6A C6 H6B 107.7 N1 C7 H7A 108.1 N1 C7 H7B 108.1 N1 C7 C8 116.9(3) H7A C7 H7B 107.3 C8 C7 H7A 108.1 C8 C7 H7B 108.1 C9 C8 C7 119.3(4) C13 C8 C7 120.1(4) C13 C8 C9 120.5(4) O1 C9 C8 118.9(3) O1 C9 C10 121.8(3) C8 C9 C10 119.2(4) C9 C10 C14 121.0(3) C11 C10 C9 117.1(4) C11 C10 C14 121.9(4) C10 C11 H11 118.0 C12 C11 C10 124.0(4) C12 C11 H11 118.0 C11 C12 C24 120.4(4) C13 C12 C11 117.7(4) C13 C12 C24 122.0(4) C8 C13 H13 119.3 C12 C13 C8 121.5(4) C12 C13 H13 119.3 C10 C14 C18 109.6(3) C10 C14 C19 112.8(3) C10 C14 C22 111.0(3) C18 C14 C19 107.3(3) C18 C14 C22 108.8(3) C19 C14 C22 107.1(3) C18 C15 H15 110.0 C18 C15 C20 108.9(3) C18 C15 C23 107.9(3) C20 C15 H15 110.0 C23 C15 H15 110.0 C23 C15 C20 110.1(4) C20 C16 H16 109.1 C20 C16 C21 109.1(4) C20 C16 C22 110.2(4) C21 C16 H16 109.1 C22 C16 H16 109.1 C22 C16 C21 110.2(3) C19 C17 H17 109.2 C19 C17 C21 109.9(4) C21 C17 H17 109.2 C23 C17 H17 109.2 C23 C17 C19 110.0(4) C23 C17 C21 109.3(4) C14 C18 H18A 109.2 C14 C18 H18B 109.2 C15 C18 C14 112.0(3) C15 C18 H18A 109.2 C15 C18 H18B 109.2 H18A C18 H18B 107.9 C14 C19 H19A 109.5 C14 C19 H19B 109.5 C17 C19 C14 110.8(3) C17 C19 H19A 109.5 C17 C19 H19B 109.5 H19A C19 H19B 108.1 C15 C20 H20A 109.7 C15 C20 H20B 109.7 C16 C20 C15 109.6(3) C16 C20 H20A 109.7 C16 C20 H20B 109.7 H20A C20 H20B 108.2 C16 C21 H21A 109.9 C16 C21 H21B 109.9 C17 C21 C16 108.9(4) C17 C21 H21A 109.9 C17 C21 H21B 109.9 H21A C21 H21B 108.3 C14 C22 H22A 109.5 C14 C22 H22B 109.5 C16 C22 C14 110.6(3) C16 C22 H22A 109.5 C16 C22 H22B 109.5 H22A C22 H22B 108.1 C15 C23 H23A 109.8 C15 C23 H23B 109.8 C17 C23 C15 109.5(3) C17 C23 H23A 109.8 C17 C23 H23B 109.8 H23A C23 H23B 108.2 C12 C24 H24A 109.5 C12 C24 H24B 109.5 C12 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 N2 C25 H25A 108.6 N2 C25 H25B 108.6 N2 C25 C26 114.7(3) H25A C25 H25B 107.6 C26 C25 H25A 108.6 C26 C25 H25B 108.6 C27 C26 C25 119.1(3) C31 C26 C25 121.4(3) C31 C26 C27 119.4(3) O2 C27 C26 118.3(3) O2 C27 C28 121.2(3) C26 C27 C28 120.5(3) C27 C28 C32 120.6(3) C29 C28 C27 116.9(3) C29 C28 C32 122.3(4) C28 C29 H29 118.3 C30 C29 C28 123.4(4) C30 C29 H29 118.3 C29 C30 C42 120.6(4) C31 C30 C29 117.9(3) C31 C30 C42 121.5(4) C26 C31 H31 119.2 C30 C31 C26 121.7(3) C30 C31 H31 119.2 C28 C32 C36 112.2(3) C28 C32 C37 111.7(3) C28 C32 C40 108.4(3) C36 C32 C37 108.3(4) C36 C32 C40 107.3(3) C37 C32 C40 108.8(3) C36 C33 H33 109.3 C38 C33 H33 109.3 C38 C33 C36 109.3(4) C41 C33 H33 109.3 C41 C33 C36 110.4(5) C41 C33 C38 109.1(5) C38 C34 H34 109.7 C38 C34 C40 108.6(4) C39 C34 H34 109.7 C39 C34 C38 110.6(4) C39 C34 C40 108.6(4) C40 C34 H34 109.7 C37 C35 H35 109.4 C39 C35 H35 109.4 C39 C35 C37 108.4(4) C39 C35 C41 111.1(5) C41 C35 H35 109.4 C41 C35 C37 109.3(5) C32 C36 C33 110.7(4) C32 C36 H36A 109.5 C32 C36 H36B 109.5 C33 C36 H36A 109.5 C33 C36 H36B 109.5 H36A C36 H36B 108.1 C32 C37 C35 109.8(4) C32 C37 H37A 109.7 C32 C37 H37B 109.7 C35 C37 H37A 109.7 C35 C37 H37B 109.7 H37A C37 H37B 108.2 C33 C38 C34 110.3(5) C33 C38 H38A 109.6 C33 C38 H38B 109.6 C34 C38 H38A 109.6 C34 C38 H38B 109.6 H38A C38 H38B 108.1 C34 C39 C35 109.4(4) C34 C39 H39A 109.8 C34 C39 H39B 109.8 C35 C39 H39A 109.8 C35 C39 H39B 109.8 H39A C39 H39B 108.2 C32 C40 H40A 109.5 C32 C40 H40B 109.5 C34 C40 C32 110.9(3) C34 C40 H40A 109.5 C34 C40 H40B 109.5 H40A C40 H40B 108.0 C33 C41 C35 109.3(5) C33 C41 H41A 109.8 C33 C41 H41B 109.8 C35 C41 H41A 109.8 C35 C41 H41B 109.8 H41A C41 H41B 108.3 C30 C42 H42A 109.5 C30 C42 H42B 109.5 C30 C42 H42C 109.5 H42A C42 H42B 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 N3 C43 H43A 108.4 N3 C43 H43B 108.4 N3 C43 C44 115.5(3) H43A C43 H43B 107.5 C44 C43 H43A 108.4 C44 C43 H43B 108.4 C45 C44 C43 118.7(3) C49 C44 C43 120.4(4) C49 C44 C45 120.9(4) O3 C45 C44 118.3(3) O3 C45 C46 122.3(4) C44 C45 C46 119.3(4) C45 C46 C50 121.3(3) C47 C46 C45 117.0(4) C47 C46 C50 121.6(4) C46 C47 H47 117.9 C48 C47 C46 124.3(4) C48 C47 H47 117.9 C47 C48 C49 117.3(4) C47 C48 C60 120.8(4) C49 C48 C60 121.8(4) C44 C49 H49 119.4 C48 C49 C44 121.1(4) C48 C49 H49 119.4 C46 C50 C54 112.7(3) C46 C50 C55 109.2(3) C46 C50 C58 111.1(3) C55 C50 C54 107.8(3) C58 C50 C54 106.3(3) C58 C50 C55 109.6(3) C54 C51 H51 109.1 C54 C51 C59 109.5(4) C56 C51 H51 109.1 C56 C51 C54 109.7(4) C56 C51 C59 110.2(5) C59 C51 H51 109.1 C56 C52 H52 109.5 C57 C52 H52 109.5 C57 C52 C56 109.9(4) C57 C52 C58 108.9(4) C58 C52 H52 109.5 C58 C52 C56 109.4(4) C55 C53 H53 109.4 C55 C53 C59 110.1(4) C57 C53 H53 109.4 C57 C53 C55 108.5(4) C57 C53 C59 110.0(4) C59 C53 H53 109.4 C50 C54 H54A 109.4 C50 C54 H54B 109.4 C51 C54 C50 111.3(4) C51 C54 H54A 109.4 C51 C54 H54B 109.4 H54A C54 H54B 108.0 C50 C55 H55A 109.5 C50 C55 H55B 109.5 C53 C55 C50 110.8(4) C53 C55 H55A 109.5 C53 C55 H55B 109.5 H55A C55 H55B 108.1 C51 C56 C52 108.4(4) C51 C56 H56A 110.0 C51 C56 H56B 110.0 C52 C56 H56A 110.0 C52 C56 H56B 110.0 H56A C56 H56B 108.4 K1 C57 H57A 42.2 K1 C57 H57B 66.0 C52 C57 K1 126.7(3) C52 C57 H57A 109.5 C52 C57 H57B 109.5 C53 C57 K1 121.0(3) C53 C57 C52 110.6(4) C53 C57 H57A 109.5 C53 C57 H57B 109.5 H57A C57 H57B 108.1 C50 C58 H58A 109.5 C50 C58 H58B 109.5 C52 C58 C50 110.5(4) C52 C58 H58A 109.5 C52 C58 H58B 109.5 H58A C58 H58B 108.1 C51 C59 C53 108.7(4) C51 C59 H59A 109.9 C51 C59 H59B 109.9 C53 C59 H59A 109.9 C53 C59 H59B 109.9 H59A C59 H59B 108.3 C48 C60 H60A 109.5 C48 C60 H60B 109.5 C48 C60 H60C 109.5 C48 C60 H60D 109.5 C48 C60 H60E 109.5 C48 C60 H60F 109.5 H60A C60 H60B 109.5 H60A C60 H60C 109.5 H60B C60 H60C 109.5 H60D C60 H60E 109.5 H60D C60 H60F 109.5 H60E C60 H60F 109.5 O4 C61 H61A 110.1 O4 C61 H61B 110.1 O4 C61 C62 108.0(3) H61A C61 H61B 108.4 C62 C61 H61A 110.1 C62 C61 H61B 110.1 K1 C62 H62A 63.9 K1 C62 H62B 159.8 O5 C62 K1 59.75(19) O5 C62 C61 107.4(3) O5 C62 H62A 110.2 O5 C62 H62B 110.2 C61 C62 K1 89.9(2) C61 C62 H62A 110.2 C61 C62 H62B 110.2 H62A C62 H62B 108.5 K1 C63 H63A 157.1 K1 C63 H63B 62.1 O5 C63 K1 59.6(2) O5 C63 H63A 110.2 O5 C63 H63B 110.2 O5 C63 C64 107.5(4) H63A C63 H63B 108.5 C64 C63 K1 92.7(3) C64 C63 H63A 110.2 C64 C63 H63B 110.2 O6 C64 C63 107.5(3) O6 C64 H64A 110.2 O6 C64 H64B 110.2 C63 C64 H64A 110.2 C63 C64 H64B 110.2 H64A C64 H64B 108.5 O6 C65 C66 124.2(5) O6 C65 C70 115.7(4) C66 C65 C70 120.2(4) C65 C66 H66 120.1 C67 C66 C65 119.9(5) C67 C66 H66 120.1 C66 C67 H67 119.7 C68 C67 C66 120.6(6) C68 C67 H67 119.7 C67 C68 H68 119.9 C67 C68 C69 120.2(5) C69 C68 H68 119.9 C68 C69 H69 119.6 C68 C69 C70 120.8(5) C70 C69 H69 119.6 O7 C70 C65 116.7(4) O7 C70 C69 124.9(5) C69 C70 C65 118.4(5) O7 C71 H71A 110.2 O7 C71 H71B 110.2 O7 C71 C72 107.7(4) H71A C71 H71B 108.5 C72 C71 H71A 110.2 C72 C71 H71B 110.2 K1 C72 H72A 155.9 K1 C72 H72B 80.5 O8 C72 K1 46.8(2) O8 C72 C71 110.0(4) O8 C72 H72A 109.7 O8 C72 H72B 109.7 C71 C72 K1 87.3(3) C71 C72 H72A 109.7 C71 C72 H72B 109.7 H72A C72 H72B 108.2 K1 C73 H73A 157.2 K1 C73 H73B 76.7 O8 C73 K1 50.3(2) O8 C73 H73A 108.6 O8 C73 H73B 108.6 O8 C73 C74 114.8(4) H73A C73 H73B 107.6 C74 C73 K1 90.5(3) C74 C73 H73A 108.6 C74 C73 H73B 108.6 O9 C74 C73 106.1(4) O9 C74 H74A 110.5 O9 C74 H74B 110.5 C73 C74 H74A 110.5 C73 C74 H74B 110.5 H74A C74 H74B 108.7 O9 C75 C76 125.2(4) O9 C75 C80 115.7(4) C76 C75 C80 119.1(4) C75 C76 H76 119.8 C75 C76 C77 120.3(4) C77 C76 H76 119.8 C76 C77 H77 119.6 C78 C77 C76 120.8(4) C78 C77 H77 119.6 C77 C78 H78 120.1 C77 C78 C79 119.7(4) C79 C78 H78 120.1 C78 C79 H79 119.9 C80 C79 C78 120.2(4) C80 C79 H79 119.9 O4 C80 C75 115.6(4) O4 C80 C79 124.4(4) C79 C80 C75 119.9(4) C102 C101 H101 120.0 C102 C101 C106 120.0 C106 C101 H101 120.0 C101 C102 H102 120.0 C103 C102 C101 120.0 C103 C102 H102 120.0 C102 C103 H103 120.0 C102 C103 C104 120.0 C104 C103 H103 120.0 C103 C104 H104 120.0 C105 C104 C103 120.0 C105 C104 H104 120.0 C104 C105 H105 120.0 C104 C105 C106 120.0 C106 C105 H105 120.0 C101 C106 H106 120.0 C105 C106 C101 120.0 C105 C106 H106 120.0 H11A C111 H11B 109.5 H11A C111 H11C 109.5 H11B C111 H11C 109.5 C112 C111 H11A 109.5 C112 C111 H11B 109.5 C112 C111 H11C 109.5 C111 C112 H11D 108.4 C111 C112 H11E 108.4 C111 C112 O113 115.5(15) H11D C112 H11E 107.5 O113 C112 H11D 108.4 O113 C112 H11E 108.4 C114 O113 C112 115.4(12) O113 C114 H11F 109.3 O113 C114 H11G 109.3 O113 C114 C115 111.7(12) H11F C114 H11G 107.9 C115 C114 H11F 109.3 C115 C114 H11G 109.3 C114 C115 H11H 109.5 C114 C115 H11I 109.5 C114 C115 H11J 109.5 H11H C115 H11I 109.5 H11H C115 H11J 109.5 H11I C115 H11J 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance U1 S1 2.5074(11) U1 O1 2.225(3) U1 O2 2.187(3) U1 O3 2.245(2) U1 N1 2.704(3) U1 N2 2.883(3) U1 N3 2.870(3) K1 S1 3.1361(14) K1 O4 2.730(3) K1 O5 2.842(3) K1 O6 2.828(3) K1 O7 2.928(3) K1 O8 2.746(3) K1 O9 2.828(3) K1 C57 3.309(5) K1 C62 3.280(4) K1 C63 3.281(4) K1 C72 3.504(5) K1 C73 3.429(5) O1 C9 1.335(4) O2 C27 1.333(4) O3 C45 1.337(4) O4 C61 1.441(5) O4 C80 1.373(5) O5 C62 1.429(5) O5 C63 1.416(5) O6 C64 1.438(5) O6 C65 1.377(5) O7 C70 1.375(6) O7 C71 1.433(6) O8 C72 1.394(6) O8 C73 1.427(6) O9 C74 1.434(5) O9 C75 1.374(5) N1 C1 1.495(5) N1 C6 1.478(5) N1 C7 1.497(5) N2 C2 1.478(5) N2 C3 1.485(5) N2 C25 1.491(5) N3 C4 1.474(5) N3 C5 1.484(5) N3 C43 1.490(5) C1 H1A 0.9900 C1 H1B 0.9900 C1 C2 1.528(5) C2 H2A 0.9900 C2 H2B 0.9900 C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.513(5) C4 H4A 0.9900 C4 H4B 0.9900 C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.525(6) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7A 0.9900 C7 H7B 0.9900 C7 C8 1.503(6) C8 C9 1.405(5) C8 C13 1.386(6) C9 C10 1.431(5) C10 C11 1.392(6) C10 C14 1.528(5) C11 H11 0.9500 C11 C12 1.384(6) C12 C13 1.384(6) C12 C24 1.513(6) C13 H13 0.9500 C14 C18 1.545(6) C14 C19 1.547(5) C14 C22 1.549(5) C15 H15 1.0000 C15 C18 1.520(5) C15 C20 1.547(6) C15 C23 1.540(6) C16 H16 1.0000 C16 C20 1.508(7) C16 C21 1.539(6) C16 C22 1.525(6) C17 H17 1.0000 C17 C19 1.531(6) C17 C21 1.533(6) C17 C23 1.514(7) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19A 0.9900 C19 H19B 0.9900 C20 H20A 0.9900 C20 H20B 0.9900 C21 H21A 0.9900 C21 H21B 0.9900 C22 H22A 0.9900 C22 H22B 0.9900 C23 H23A 0.9900 C23 H23B 0.9900 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9900 C25 H25B 0.9900 C25 C26 1.499(5) C26 C27 1.405(5) C26 C31 1.395(5) C27 C28 1.419(5) C28 C29 1.399(5) C28 C32 1.535(5) C29 H29 0.9500 C29 C30 1.393(6) C30 C31 1.382(5) C30 C42 1.512(5) C31 H31 0.9500 C32 C36 1.537(6) C32 C37 1.546(6) C32 C40 1.548(6) C33 H33 1.0000 C33 C36 1.543(7) C33 C38 1.517(8) C33 C41 1.505(10) C34 H34 1.0000 C34 C38 1.526(7) C34 C39 1.512(7) C34 C40 1.543(6) C35 H35 1.0000 C35 C37 1.555(6) C35 C39 1.531(8) C35 C41 1.534(9) C36 H36A 0.9900 C36 H36B 0.9900 C37 H37A 0.9900 C37 H37B 0.9900 C38 H38A 0.9900 C38 H38B 0.9900 C39 H39A 0.9900 C39 H39B 0.9900 C40 H40A 0.9900 C40 H40B 0.9900 C41 H41A 0.9900 C41 H41B 0.9900 C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C43 H43A 0.9900 C43 H43B 0.9900 C43 C44 1.498(5) C44 C45 1.396(6) C44 C49 1.394(6) C45 C46 1.425(5) C46 C47 1.399(6) C46 C50 1.516(6) C47 H47 0.9500 C47 C48 1.384(6) C48 C49 1.391(6) C48 C60 1.519(6) C49 H49 0.9500 C50 C54 1.556(5) C50 C55 1.541(5) C50 C58 1.540(6) C51 H51 1.0000 C51 C54 1.528(7) C51 C56 1.527(7) C51 C59 1.530(7) C52 H52 1.0000 C52 C56 1.542(6) C52 C57 1.529(8) C52 C58 1.535(7) C53 H53 1.0000 C53 C55 1.523(6) C53 C57 1.511(7) C53 C59 1.540(6) C54 H54A 0.9900 C54 H54B 0.9900 C55 H55A 0.9900 C55 H55B 0.9900 C56 H56A 0.9900 C56 H56B 0.9900 C57 H57A 0.9900 C57 H57B 0.9900 C58 H58A 0.9900 C58 H58B 0.9900 C59 H59A 0.9900 C59 H59B 0.9900 C60 H60A 0.9800 C60 H60B 0.9800 C60 H60C 0.9800 C60 H60D 0.9800 C60 H60E 0.9800 C60 H60F 0.9800 C61 H61A 0.9900 C61 H61B 0.9900 C61 C62 1.497(6) C62 H62A 0.9900 C62 H62B 0.9900 C63 H63A 0.9900 C63 H63B 0.9900 C63 C64 1.498(6) C64 H64A 0.9900 C64 H64B 0.9900 C65 C66 1.386(7) C65 C70 1.402(7) C66 H66 0.9500 C66 C67 1.377(7) C67 H67 0.9500 C67 C68 1.362(9) C68 H68 0.9500 C68 C69 1.383(8) C69 H69 0.9500 C69 C70 1.385(6) C71 H71A 0.9900 C71 H71B 0.9900 C71 C72 1.504(8) C72 H72A 0.9900 C72 H72B 0.9900 C73 H73A 0.9900 C73 H73B 0.9900 C73 C74 1.508(7) C74 H74A 0.9900 C74 H74B 0.9900 C75 C76 1.380(6) C75 C80 1.411(6) C76 H76 0.9500 C76 C77 1.384(7) C77 H77 0.9500 C77 C78 1.374(7) C78 H78 0.9500 C78 C79 1.391(6) C79 H79 0.9500 C79 C80 1.381(6) C101 H101 0.9500 C101 C102 1.3900 C101 C106 1.3900 C102 H102 0.9500 C102 C103 1.3900 C103 H103 0.9500 C103 C104 1.3900 C104 H104 0.9500 C104 C105 1.3900 C105 H105 0.9500 C105 C106 1.3900 C106 H106 0.9500 C111 H11A 0.9800 C111 H11B 0.9800 C111 H11C 0.9800 C111 C112 1.33(2) C112 H11D 0.9900 C112 H11E 0.9900 C112 O113 1.378(17) O113 C114 1.349(17) C114 H11F 0.9900 C114 H11G 0.9900 C114 C115 1.48(2) C115 H11H 0.9800 C115 H11I 0.9800 C115 H11J 0.9800 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 U1 O1 C9 C8 -17.3(6) U1 O1 C9 C10 163.8(3) U1 O2 C27 C26 25.8(7) U1 O2 C27 C28 -154.4(4) U1 O3 C45 C44 22.2(8) U1 O3 C45 C46 -157.5(4) U1 N1 C1 C2 -4.2(4) U1 N1 C6 C5 -64.2(3) U1 N1 C7 C8 80.2(3) U1 N2 C2 C1 -57.6(3) U1 N2 C3 C4 -14.2(4) U1 N2 C25 C26 74.7(3) U1 N3 C4 C3 -62.3(3) U1 N3 C5 C6 -9.0(4) U1 N3 C43 C44 75.3(4) K1 O4 C61 C62 7.9(4) K1 O4 C80 C75 -11.3(6) K1 O4 C80 C79 170.2(4) K1 O5 C62 C61 79.4(3) K1 O5 C63 C64 -82.7(3) K1 O6 C64 C63 -2.3(5) K1 O6 C65 C66 173.1(4) K1 O6 C65 C70 -6.7(6) K1 O7 C70 C65 12.6(5) K1 O7 C70 C69 -169.5(4) K1 O7 C71 C72 -32.9(5) K1 O8 C72 C71 -65.8(4) K1 O8 C73 C74 -68.2(4) K1 O9 C74 C73 -9.1(5) K1 O9 C75 C76 -169.9(4) K1 O9 C75 C80 10.5(6) K1 C63 C64 O6 1.8(4) K1 C73 C74 O9 6.5(4) O1 C9 C10 C11 -178.5(3) O1 C9 C10 C14 1.9(6) O2 C27 C28 C29 176.3(3) O2 C27 C28 C32 -8.2(5) O3 C45 C46 C47 176.7(4) O3 C45 C46 C50 -6.1(6) O4 C61 C62 K1 -5.9(3) O4 C61 C62 O5 -64.0(4) O5 C63 C64 O6 60.8(5) O6 C65 C66 C67 -178.4(5) O6 C65 C70 O7 -4.1(6) O6 C65 C70 C69 177.8(4) O7 C71 C72 K1 24.5(4) O7 C71 C72 O8 66.3(5) O8 C73 C74 O9 52.1(5) O9 C75 C76 C77 -178.3(5) O9 C75 C80 O4 -0.1(6) O9 C75 C80 C79 178.5(4) N1 C1 C2 N2 45.0(4) N1 C7 C8 C9 -47.9(5) N1 C7 C8 C13 135.2(4) N2 C3 C4 N3 52.6(4) N2 C25 C26 C27 -60.7(4) N2 C25 C26 C31 123.1(4) N3 C5 C6 N1 50.1(4) N3 C43 C44 C45 -56.9(5) N3 C43 C44 C49 123.0(4) C1 N1 C6 C5 65.6(4) C1 N1 C7 C8 -46.7(5) C2 N2 C3 C4 -133.6(3) C2 N2 C25 C26 -173.8(3) C3 N2 C2 C1 69.2(4) C3 N2 C25 C26 -52.7(4) C4 N3 C5 C6 -130.0(3) C4 N3 C43 C44 -169.9(3) C5 N3 C4 C3 61.4(4) C5 N3 C43 C44 -47.5(4) C6 N1 C1 C2 -127.2(3) C6 N1 C7 C8 -168.8(3) C7 N1 C1 C2 112.7(4) C7 N1 C6 C5 -171.8(3) C7 C8 C9 O1 1.9(5) C7 C8 C9 C10 -179.1(3) C7 C8 C13 C12 176.5(4) C8 C9 C10 C11 2.6(5) C8 C9 C10 C14 -177.0(4) C9 C8 C13 C12 -0.3(6) C9 C10 C11 C12 -0.5(6) C9 C10 C14 C18 58.9(5) C9 C10 C14 C19 178.4(4) C9 C10 C14 C22 -61.3(5) C10 C11 C12 C13 -2.0(6) C10 C11 C12 C24 177.7(4) C10 C14 C18 C15 -178.1(3) C10 C14 C19 C17 -177.8(3) C10 C14 C22 C16 176.7(3) C11 C10 C14 C18 -120.7(4) C11 C10 C14 C19 -1.2(5) C11 C10 C14 C22 119.1(4) C11 C12 C13 C8 2.4(6) C13 C8 C9 O1 178.8(4) C13 C8 C9 C10 -2.3(6) C14 C10 C11 C12 179.1(4) C18 C14 C19 C17 -57.0(4) C18 C14 C22 C16 56.1(4) C18 C15 C20 C16 -59.9(4) C18 C15 C23 C17 60.7(4) C19 C14 C18 C15 59.0(4) C19 C14 C22 C16 -59.6(4) C19 C17 C21 C16 58.8(5) C19 C17 C23 C15 -60.7(4) C20 C15 C18 C14 58.4(4) C20 C15 C23 C17 -58.1(4) C20 C16 C21 C17 62.1(5) C20 C16 C22 C14 -59.8(4) C21 C16 C20 C15 -60.0(4) C21 C16 C22 C14 60.7(5) C21 C17 C19 C14 -60.7(5) C21 C17 C23 C15 60.1(4) C22 C14 C18 C15 -56.5(4) C22 C14 C19 C17 59.7(4) C22 C16 C20 C15 61.1(4) C22 C16 C21 C17 -59.1(5) C23 C15 C18 C14 -61.1(4) C23 C15 C20 C16 58.3(4) C23 C17 C19 C14 59.6(4) C23 C17 C21 C16 -62.0(5) C24 C12 C13 C8 -177.3(4) C25 N2 C2 C1 -170.0(3) C25 N2 C3 C4 106.4(3) C25 C26 C27 O2 5.7(5) C25 C26 C27 C28 -174.0(3) C25 C26 C31 C30 176.9(3) C26 C27 C28 C29 -3.9(5) C26 C27 C28 C32 171.5(3) C27 C26 C31 C30 0.7(5) C27 C28 C29 C30 2.9(6) C27 C28 C32 C36 -177.6(4) C27 C28 C32 C37 60.5(5) C27 C28 C32 C40 -59.3(5) C28 C29 C30 C31 -0.2(6) C28 C29 C30 C42 177.7(4) C28 C32 C36 C33 178.1(4) C28 C32 C37 C35 -177.1(4) C28 C32 C40 C34 179.0(3) C29 C28 C32 C36 -2.4(5) C29 C28 C32 C37 -124.4(4) C29 C28 C32 C40 115.8(4) C29 C30 C31 C26 -1.7(5) C31 C26 C27 O2 -178.1(3) C31 C26 C27 C28 2.2(5) C32 C28 C29 C30 -172.4(4) C36 C32 C37 C35 58.8(5) C36 C32 C40 C34 -59.6(4) C36 C33 C38 C34 60.0(6) C36 C33 C41 C35 -60.0(6) C37 C32 C36 C33 -58.0(5) C37 C32 C40 C34 57.4(4) C37 C35 C39 C34 -63.3(6) C37 C35 C41 C33 60.5(6) C38 C33 C36 C32 -60.4(6) C38 C33 C41 C35 60.2(6) C38 C34 C39 C35 -56.4(5) C38 C34 C40 C32 60.2(5) C39 C34 C38 C33 59.3(5) C39 C34 C40 C32 -60.1(5) C39 C35 C37 C32 60.7(6) C39 C35 C41 C33 -59.0(6) C40 C32 C36 C33 59.2(5) C40 C32 C37 C35 -57.5(5) C40 C34 C38 C33 -59.8(6) C40 C34 C39 C35 62.7(5) C41 C33 C36 C32 59.6(6) C41 C33 C38 C34 -60.8(6) C41 C35 C37 C32 -60.5(6) C41 C35 C39 C34 56.7(5) C42 C30 C31 C26 -179.6(4) C43 N3 C4 C3 -177.1(3) C43 N3 C5 C6 111.1(4) C43 C44 C45 O3 3.6(6) C43 C44 C45 C46 -176.7(4) C43 C44 C49 C48 178.3(4) C44 C45 C46 C47 -3.0(6) C44 C45 C46 C50 174.3(4) C45 C44 C49 C48 -1.7(7) C45 C46 C47 C48 1.2(6) C45 C46 C50 C54 179.4(4) C45 C46 C50 C55 -60.7(5) C45 C46 C50 C58 60.2(5) C46 C47 C48 C49 0.4(7) C46 C47 C48 C60 -179.9(5) C46 C50 C54 C51 178.5(4) C46 C50 C55 C53 179.5(3) C46 C50 C58 C52 -177.1(4) C47 C46 C50 C54 -3.4(5) C47 C46 C50 C55 116.4(4) C47 C46 C50 C58 -122.6(4) C47 C48 C49 C44 -0.2(7) C49 C44 C45 O3 -176.4(4) C49 C44 C45 C46 3.3(6) C50 C46 C47 C48 -176.1(4) C54 C50 C55 C53 -57.8(4) C54 C50 C58 C52 59.9(5) C54 C51 C56 C52 -59.7(6) C54 C51 C59 C53 59.9(5) C55 C50 C54 C51 57.9(5) C55 C50 C58 C52 -56.4(5) C55 C53 C57 K1 -104.2(3) C55 C53 C57 C52 61.9(5) C55 C53 C59 C51 -60.4(6) C56 C51 C54 C50 61.0(5) C56 C51 C59 C53 -60.9(5) C56 C52 C57 K1 -136.1(4) C56 C52 C57 C53 58.8(5) C56 C52 C58 C50 -62.3(5) C57 C52 C56 C51 -59.1(6) C57 C52 C58 C50 57.8(5) C57 C53 C55 C50 -60.0(4) C57 C53 C59 C51 59.1(5) C58 C50 C54 C51 -59.6(5) C58 C50 C55 C53 57.6(4) C58 C52 C56 C51 60.4(6) C58 C52 C57 K1 104.0(4) C58 C52 C57 C53 -61.0(5) C59 C51 C54 C50 -60.0(5) C59 C51 C56 C52 60.9(5) C59 C53 C55 C50 60.5(5) C59 C53 C57 K1 135.3(3) C59 C53 C57 C52 -58.6(5) C60 C48 C49 C44 -179.9(5) C61 O4 C80 C75 177.3(4) C61 O4 C80 C79 -1.3(7) C62 O5 C63 K1 -96.9(3) C62 O5 C63 C64 -179.6(3) C63 O5 C62 K1 97.2(3) C63 O5 C62 C61 176.6(3) C64 O6 C65 C66 -2.8(7) C64 O6 C65 C70 177.4(4) C65 O6 C64 C63 174.2(4) C65 C66 C67 C68 0.1(9) C66 C65 C70 O7 176.0(4) C66 C65 C70 C69 -2.0(7) C66 C67 C68 C69 -1.0(10) C67 C68 C69 C70 0.4(9) C68 C69 C70 O7 -176.7(5) C68 C69 C70 C65 1.1(8) C70 O7 C71 C72 171.4(4) C70 C65 C66 C67 1.4(8) C71 O7 C70 C65 165.7(4) C71 O7 C70 C69 -16.4(7) C72 O8 C73 K1 123.4(4) C72 O8 C73 C74 55.2(5) C73 O8 C72 K1 -120.5(4) C73 O8 C72 C71 173.7(4) C74 O9 C75 C76 12.7(7) C74 O9 C75 C80 -167.0(4) C75 O9 C74 C73 168.5(4) C75 C76 C77 C78 -0.6(9) C76 C75 C80 O4 -179.7(4) C76 C75 C80 C79 -1.2(7) C76 C77 C78 C79 -0.3(9) C77 C78 C79 C80 0.5(9) C78 C79 C80 O4 178.7(5) C78 C79 C80 C75 0.2(8) C80 O4 C61 C62 -179.6(4) C80 C75 C76 C77 1.4(8) C101 C102 C103 C104 0.0 C102 C101 C106 C105 0.0 C102 C103 C104 C105 0.0 C103 C104 C105 C106 0.0 C104 C105 C106 C101 0.0 C106 C101 C102 C103 0.0 C111 C112 O113 C114 172.0(16) C112 O113 C114 C115 -177.2(13)