#------------------------------------------------------------------------------ #$Date: 2019-12-18 04:13:26 +0200 (Wed, 18 Dec 2019) $ #$Revision: 245292 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125667.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_7125667 loop_ _publ_author_name 'Phukon, Jyotshna' 'Gogoi, Sanjib' _publ_section_title ; Palladium(II)-Catalyzed Vinylic Geminal Double C-H Activation and Alkyne Annulation Reaction: Synthesis of Pentafulvenes ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09564K _journal_year 2020 _chemical_formula_sum 'C96 H86 N2 O4' _chemical_formula_weight 1331.66 _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 mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-09-11 deposited with the CCDC. 2019-12-13 downloaded from the CCDC. ; _cell_angle_alpha 100.456(2) _cell_angle_beta 103.9830(10) _cell_angle_gamma 94.9720(10) _cell_formula_units_Z 2 _cell_length_a 12.8892(4) _cell_length_b 14.4794(4) _cell_length_c 21.3927(6) _cell_measurement_temperature 296(2) _cell_volume 3774.03(19) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 56834 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.436 _diffrn_reflns_theta_min 1.003 _exptl_absorpt_coefficient_mu 0.070 _exptl_crystal_density_diffrn 1.172 _exptl_crystal_F_000 1416 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.382 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 941 _refine_ls_number_reflns 15452 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0686 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1192P)^2^+0.3835P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1869 _refine_ls_wR_factor_ref 0.2257 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8797 _reflns_number_total 15452 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09564k2.cif _cod_data_source_block PP_DH_JP_81_0m_a _cod_database_code 7125667 _shelx_shelxl_version_number 2016/6 _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_min 0.987 _shelx_estimated_absorpt_t_max 0.992 _shelx_res_file ; TITL PP_DH_JP_81_0m_a.res in P-1 PP_DH_JP_81_0m_a.res created by SHELXL-2016/6 at 13:15:10 on 05-Feb-2019 CELL 0.71073 12.8892 14.4794 21.3927 100.456 103.983 94.972 ZERR 2.000 0.0004 0.0004 0.0006 0.002 0.001 0.001 LATT 1 SFAC C H N O UNIT 192 172 4 8 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 LIST 6 SIZE 0.12 0.15 0.18 TEMP 23.000 WGHT 0.119200 0.383500 FVAR 0.43317 O1 4 0.608650 0.496468 0.423298 11.00000 0.10280 0.11218 = 0.12308 -0.04888 -0.03062 0.02682 O2 4 0.820596 0.586389 0.734358 11.00000 0.06749 0.16174 = 0.09159 0.01874 0.03535 0.02359 O3 4 0.891568 0.625436 0.628242 11.00000 0.07386 0.11939 = 0.06959 0.02133 0.00401 0.00638 O4 4 0.567724 0.391098 0.298930 11.00000 0.07528 0.15504 = 0.07889 -0.01947 0.01521 -0.01689 N1 3 0.705756 0.613763 0.505024 11.00000 0.05242 0.05813 = 0.06046 0.00611 0.00662 0.00057 N2 3 0.672355 0.618320 0.767766 11.00000 0.05195 0.07209 = 0.06114 0.01612 0.02334 0.00643 C1 1 0.892581 0.848751 0.566585 11.00000 0.03879 0.04399 = 0.04039 0.01145 0.00928 0.00900 C2 1 0.860033 0.891474 0.626673 11.00000 0.04125 0.04499 = 0.04270 0.00924 0.01344 0.00819 C3 1 0.949616 0.939238 0.672203 11.00000 0.04176 0.04865 = 0.04157 0.00937 0.01245 0.00579 C4 1 1.043086 0.932512 0.643813 11.00000 0.03834 0.04774 = 0.04007 0.01207 0.00936 0.00598 C5 1 1.010285 0.879886 0.581594 11.00000 0.03716 0.04638 = 0.04079 0.01235 0.01048 0.00875 C6 1 0.749834 0.882078 0.636412 11.00000 0.04338 0.05386 = 0.03757 0.00787 0.01201 0.00785 C7 1 0.700911 0.798019 0.644298 11.00000 0.05267 0.05975 = 0.06660 0.01772 0.02095 0.00716 AFIX 43 H7 2 0.737499 0.745389 0.643608 11.00000 -1.20000 AFIX 0 C8 1 0.597569 0.791109 0.653259 11.00000 0.06148 0.08091 = 0.08127 0.01562 0.03166 -0.00465 AFIX 43 H8 2 0.565384 0.733873 0.658293 11.00000 -1.20000 AFIX 0 C9 1 0.542937 0.867754 0.654728 11.00000 0.04651 0.09300 = 0.06918 0.00951 0.02435 0.00641 AFIX 43 H9 2 0.473280 0.862745 0.660017 11.00000 -1.20000 AFIX 0 C10 1 0.591244 0.951321 0.648398 11.00000 0.05901 0.08172 = 0.07811 0.01282 0.03140 0.02484 AFIX 43 H10 2 0.554727 1.003993 0.650026 11.00000 -1.20000 AFIX 0 C11 1 0.693626 0.959027 0.639599 11.00000 0.05895 0.06035 = 0.07500 0.01471 0.03315 0.01210 AFIX 43 H11 2 0.725573 1.017087 0.635727 11.00000 -1.20000 AFIX 0 C12 1 0.956177 0.993016 0.739007 11.00000 0.03976 0.06980 = 0.04311 0.00060 0.01094 0.00729 C13 1 0.906793 0.953984 0.781192 11.00000 0.06326 0.09396 = 0.04837 0.01053 0.01868 0.01440 AFIX 43 H13 2 0.868232 0.893334 0.767166 11.00000 -1.20000 AFIX 0 C14 1 0.914851 1.005207 0.844125 11.00000 0.07265 0.15028 = 0.05076 0.00780 0.02614 0.02226 AFIX 43 H14 2 0.880499 0.978987 0.871650 11.00000 -1.20000 AFIX 0 C15 1 0.972163 1.092824 0.865743 11.00000 0.06733 0.16231 = 0.06302 -0.03456 0.02252 0.00788 AFIX 43 H15 2 0.978617 1.126024 0.908313 11.00000 -1.20000 AFIX 0 C16 1 1.020569 1.132436 0.824852 11.00000 0.06358 0.11817 = 0.10216 -0.05390 0.02805 -0.01204 AFIX 43 H16 2 1.059263 1.192995 0.839614 11.00000 -1.20000 AFIX 0 C17 1 1.012471 1.082907 0.761243 11.00000 0.06036 0.08261 = 0.07090 -0.01715 0.02585 -0.00210 AFIX 43 H17 2 1.045261 1.110739 0.733709 11.00000 -1.20000 AFIX 0 C18 1 1.156200 0.973800 0.679335 11.00000 0.04055 0.04679 = 0.04405 0.00423 0.01186 0.00507 C19 1 1.205623 0.949333 0.737885 11.00000 0.05441 0.07075 = 0.04738 0.01602 0.00449 -0.00287 AFIX 43 H19 2 1.166187 0.910102 0.756327 11.00000 -1.20000 AFIX 0 C20 1 1.312988 0.982479 0.769367 11.00000 0.05388 0.08546 = 0.05908 0.01993 -0.00406 0.00272 AFIX 43 H20 2 1.344972 0.965734 0.808831 11.00000 -1.20000 AFIX 0 C21 1 1.371547 1.039133 0.742940 11.00000 0.04058 0.07963 = 0.07627 0.00814 0.00152 0.00099 AFIX 43 H21 2 1.444098 1.060206 0.763618 11.00000 -1.20000 AFIX 0 C22 1 1.323362 1.065365 0.685456 11.00000 0.04765 0.07336 = 0.08210 0.02379 0.01362 -0.00434 AFIX 43 H22 2 1.362913 1.105793 0.667872 11.00000 -1.20000 AFIX 0 C23 1 1.217230 1.032297 0.653804 11.00000 0.04560 0.06218 = 0.06294 0.02096 0.00902 0.00323 AFIX 43 H23 2 1.185977 1.049673 0.614450 11.00000 -1.20000 AFIX 0 C24 1 1.081795 0.865767 0.536885 11.00000 0.04054 0.04516 = 0.04103 0.00621 0.01114 0.00756 C25 1 1.178178 0.829115 0.555305 11.00000 0.04895 0.06554 = 0.05186 0.01744 0.01401 0.01966 AFIX 43 H25 2 1.195992 0.809641 0.595211 11.00000 -1.20000 AFIX 0 C26 1 1.247336 0.821240 0.515569 11.00000 0.05164 0.08421 = 0.07959 0.01906 0.02602 0.02921 AFIX 43 H26 2 1.311725 0.797026 0.528825 11.00000 -1.20000 AFIX 0 C27 1 1.221832 0.849024 0.456162 11.00000 0.07140 0.09366 = 0.07843 0.03014 0.04635 0.03109 AFIX 43 H27 2 1.268710 0.843395 0.429180 11.00000 -1.20000 AFIX 0 C28 1 1.127551 0.884858 0.436962 11.00000 0.06886 0.07442 = 0.05736 0.02532 0.02939 0.02178 AFIX 43 H28 2 1.109998 0.903335 0.396691 11.00000 -1.20000 AFIX 0 C29 1 1.058348 0.893778 0.476901 11.00000 0.04744 0.05117 = 0.05009 0.01380 0.01675 0.01506 AFIX 43 H29 2 0.994722 0.919024 0.463477 11.00000 -1.20000 AFIX 0 C30 1 0.827796 0.790820 0.511045 11.00000 0.04137 0.04550 = 0.04062 0.01172 0.00728 0.00879 C31 1 0.707429 0.778233 0.495227 11.00000 0.04423 0.06231 = 0.04012 0.00470 0.00659 0.01762 C32 1 0.648778 0.688652 0.487797 11.00000 0.04181 0.06857 = 0.04804 -0.00144 0.00698 0.00177 C33 1 0.537240 0.675624 0.465789 11.00000 0.04556 0.09003 = 0.07953 -0.00617 0.01130 0.00469 AFIX 43 H33 2 0.498244 0.616636 0.461435 11.00000 -1.20000 AFIX 0 C34 1 0.484959 0.749614 0.450558 11.00000 0.04821 0.10764 = 0.09085 -0.01020 0.00321 0.02120 AFIX 43 H34 2 0.410291 0.739682 0.434065 11.00000 -1.20000 AFIX 0 C35 1 0.539374 0.837969 0.458885 11.00000 0.06582 0.10574 = 0.07026 0.00848 0.01178 0.04900 AFIX 43 H35 2 0.501678 0.887889 0.449539 11.00000 -1.20000 AFIX 0 C36 1 0.652213 0.853298 0.481558 11.00000 0.06440 0.07720 = 0.05482 0.00932 0.01164 0.02980 AFIX 43 H36 2 0.689775 0.913368 0.487391 11.00000 -1.20000 AFIX 0 C37 1 0.867604 0.736142 0.458073 11.00000 0.03949 0.04451 = 0.04375 0.00513 0.00726 0.00815 C38 1 0.948559 0.679496 0.469526 11.00000 0.05922 0.05675 = 0.04760 0.01069 0.00626 0.01577 AFIX 43 H38 2 0.978643 0.672767 0.512308 11.00000 -1.20000 AFIX 0 C39 1 0.985365 0.632914 0.418706 11.00000 0.07116 0.06909 = 0.06732 0.00688 0.01550 0.03381 AFIX 43 H39 2 1.038862 0.594444 0.427843 11.00000 -1.20000 AFIX 0 C40 1 0.944730 0.642037 0.354706 11.00000 0.07946 0.07735 = 0.05369 -0.00688 0.01795 0.02080 C41 1 0.862114 0.696150 0.342837 11.00000 0.08617 0.08411 = 0.04035 0.00305 0.00706 0.02737 AFIX 43 H41 2 0.832768 0.702998 0.299994 11.00000 -1.20000 AFIX 0 C42 1 0.821810 0.740412 0.392813 11.00000 0.05857 0.06162 = 0.04484 0.00552 0.00352 0.01936 AFIX 43 H42 2 0.763356 0.773511 0.382837 11.00000 -1.20000 AFIX 0 C43 1 0.685473 0.523004 0.470840 11.00000 0.07167 0.07237 = 0.07465 -0.00797 -0.00248 0.00428 C44 1 0.762989 0.458939 0.493717 11.00000 0.11980 0.06787 = 0.12054 0.00870 0.00430 0.02349 AFIX 137 H44A 2 0.724673 0.397396 0.489797 11.00000 -1.50000 H44B 2 0.801091 0.484088 0.538950 11.00000 -1.50000 H44C 2 0.813521 0.453749 0.467252 11.00000 -1.50000 AFIX 0 C45 1 0.991880 0.596407 0.299928 11.00000 0.12234 0.11946 = 0.07744 -0.01078 0.04005 0.04604 AFIX 23 H45A 2 1.011747 0.535748 0.308121 11.00000 -1.20000 H45B 2 0.936484 0.584271 0.258539 11.00000 -1.20000 AFIX 0 C46 1 1.085867 0.652991 0.293251 11.00000 0.24770 0.16186 = 0.19608 -0.01606 0.17493 0.01312 AFIX 137 H46A 2 1.063995 0.706860 0.275726 11.00000 -1.50000 H46B 2 1.119140 0.615227 0.263964 11.00000 -1.50000 H46C 2 1.136533 0.674251 0.335654 11.00000 -1.50000 AFIX 0 C47 1 0.479280 0.599906 0.882296 11.00000 0.04079 0.04399 = 0.03343 0.00474 0.00731 0.00361 C48 1 0.443768 0.694553 0.896009 11.00000 0.04571 0.04518 = 0.03591 0.00428 0.00978 0.00978 C49 1 0.344291 0.681936 0.907185 11.00000 0.04394 0.05086 = 0.03430 0.00429 0.00998 0.01073 C50 1 0.311987 0.580438 0.902495 11.00000 0.03822 0.05398 = 0.03450 0.00951 0.00557 0.00651 C51 1 0.391271 0.531080 0.887802 11.00000 0.03978 0.04808 = 0.03375 0.00661 0.00568 0.00705 C52 1 0.500984 0.786826 0.894154 11.00000 0.04647 0.04385 = 0.04493 0.00735 0.01176 0.01105 C53 1 0.529721 0.803700 0.838044 11.00000 0.05711 0.05500 = 0.04293 0.00891 0.01054 0.00665 AFIX 43 H53 2 0.512015 0.756134 0.800127 11.00000 -1.20000 AFIX 0 C54 1 0.583994 0.889915 0.838062 11.00000 0.07757 0.06381 = 0.06399 0.02302 0.02257 0.00120 AFIX 43 H54 2 0.603412 0.899499 0.800351 11.00000 -1.20000 AFIX 0 C55 1 0.609613 0.961310 0.892532 11.00000 0.08790 0.05212 = 0.08185 0.01345 0.02655 -0.00475 AFIX 43 H55 2 0.645902 1.019431 0.892003 11.00000 -1.20000 AFIX 0 C56 1 0.581451 0.946778 0.948161 11.00000 0.08842 0.04942 = 0.07172 -0.00347 0.02361 -0.00160 AFIX 43 H56 2 0.599220 0.995104 0.985645 11.00000 -1.20000 AFIX 0 C57 1 0.526821 0.860736 0.948832 11.00000 0.07284 0.05255 = 0.05074 0.00063 0.02054 0.00843 AFIX 43 H57 2 0.507029 0.852254 0.986645 11.00000 -1.20000 AFIX 0 C58 1 0.279334 0.757045 0.924944 11.00000 0.04431 0.05458 = 0.04375 0.00216 0.00915 0.01220 C59 1 0.253560 0.824129 0.887234 11.00000 0.06693 0.06684 = 0.05541 0.01026 0.01550 0.02421 AFIX 43 H59 2 0.277148 0.822295 0.849290 11.00000 -1.20000 AFIX 0 C60 1 0.193008 0.894070 0.905282 11.00000 0.08075 0.06984 = 0.07928 0.01267 0.01690 0.03422 AFIX 43 H60 2 0.175367 0.938125 0.879127 11.00000 -1.20000 AFIX 0 C61 1 0.159493 0.898271 0.961051 11.00000 0.07307 0.08589 = 0.09249 -0.00772 0.01894 0.03524 AFIX 43 H61 2 0.120036 0.945905 0.973504 11.00000 -1.20000 AFIX 0 C62 1 0.183721 0.832387 0.999065 11.00000 0.07411 0.09903 = 0.07024 -0.00283 0.03431 0.02040 AFIX 43 H62 2 0.160218 0.835241 1.037107 11.00000 -1.20000 AFIX 0 C63 1 0.242771 0.761914 0.981157 11.00000 0.06172 0.07598 = 0.05252 0.00644 0.02107 0.02118 AFIX 43 H63 2 0.258231 0.717195 1.007046 11.00000 -1.20000 AFIX 0 C64 1 0.207491 0.539752 0.910249 11.00000 0.04012 0.05845 = 0.04189 0.00569 0.00881 0.00715 C65 1 0.110546 0.563546 0.875256 11.00000 0.05036 0.07682 = 0.05427 0.01372 0.00454 0.01522 AFIX 43 H65 2 0.112207 0.607451 0.848600 11.00000 -1.20000 AFIX 0 C66 1 0.013120 0.523077 0.879689 11.00000 0.03697 0.10177 = 0.07620 0.00966 0.00294 0.01461 AFIX 43 H66 2 -0.050644 0.539043 0.855670 11.00000 -1.20000 AFIX 0 C67 1 0.009421 0.459410 0.919257 11.00000 0.04720 0.09665 = 0.09442 0.01082 0.02240 -0.00330 AFIX 43 H67 2 -0.056867 0.432087 0.922061 11.00000 -1.20000 AFIX 0 C68 1 0.104125 0.435346 0.955268 11.00000 0.05338 0.08906 = 0.08007 0.02614 0.02400 0.00134 AFIX 43 H68 2 0.101522 0.392552 0.982619 11.00000 -1.20000 AFIX 0 C69 1 0.201737 0.474958 0.950374 11.00000 0.04200 0.07562 = 0.05416 0.01851 0.01319 0.00872 AFIX 43 H69 2 0.265084 0.458191 0.974288 11.00000 -1.20000 AFIX 0 C70 1 0.391982 0.428048 0.885154 11.00000 0.03628 0.04835 = 0.03842 0.00687 0.00990 0.00125 C71 1 0.308869 0.362472 0.842612 11.00000 0.04764 0.05571 = 0.05298 0.00436 0.00408 0.00098 AFIX 43 H71 2 0.252340 0.383231 0.814983 11.00000 -1.20000 AFIX 0 C72 1 0.308837 0.266666 0.840681 11.00000 0.06645 0.05639 = 0.06683 -0.00057 0.00842 -0.01430 AFIX 43 H72 2 0.253025 0.223453 0.811293 11.00000 -1.20000 AFIX 0 C73 1 0.390416 0.234829 0.881741 11.00000 0.09205 0.04687 = 0.07050 0.01336 0.01773 0.00144 AFIX 43 H73 2 0.389849 0.170274 0.880616 11.00000 -1.20000 AFIX 0 C74 1 0.473075 0.298958 0.924592 11.00000 0.06888 0.05626 = 0.05556 0.01659 0.01077 0.01472 AFIX 43 H74 2 0.528928 0.277707 0.952410 11.00000 -1.20000 AFIX 0 C75 1 0.473653 0.394287 0.926562 11.00000 0.04894 0.05194 = 0.04011 0.00724 0.00975 0.00297 AFIX 43 H75 2 0.529727 0.437004 0.956148 11.00000 -1.20000 AFIX 0 C76 1 0.573034 0.579735 0.867329 11.00000 0.04275 0.04643 = 0.03547 0.00806 0.00935 0.00603 C77 1 0.669112 0.653377 0.881920 11.00000 0.03821 0.04705 = 0.05197 0.00942 0.00756 0.00771 C78 1 0.722073 0.666350 0.834210 11.00000 0.04260 0.05376 = 0.06897 0.01407 0.01636 0.00454 C79 1 0.816669 0.727920 0.850698 11.00000 0.05710 0.06879 = 0.10825 0.01776 0.02798 -0.00250 AFIX 43 H79 2 0.852239 0.736012 0.818674 11.00000 -1.20000 AFIX 0 C80 1 0.858171 0.776990 0.913916 11.00000 0.05401 0.07319 = 0.13100 0.00888 0.00561 -0.01608 AFIX 43 H80 2 0.923180 0.817071 0.924989 11.00000 -1.20000 AFIX 0 C81 1 0.805379 0.768076 0.961435 11.00000 0.06344 0.06859 = 0.09082 -0.00142 -0.01562 -0.00998 AFIX 43 H81 2 0.833026 0.803783 1.004035 11.00000 -1.20000 AFIX 0 C82 1 0.710968 0.705857 0.945796 11.00000 0.05860 0.05789 = 0.05854 0.00462 0.00429 0.00562 AFIX 43 H82 2 0.675395 0.699082 0.978029 11.00000 -1.20000 AFIX 0 C83 1 0.591366 0.483910 0.837380 11.00000 0.03983 0.04854 = 0.04473 0.00741 0.01474 0.00434 C84 1 0.516336 0.426230 0.784110 11.00000 0.04743 0.05140 = 0.05384 0.00582 0.01434 0.00570 AFIX 43 H84 2 0.451093 0.446922 0.767079 11.00000 -1.20000 AFIX 0 C85 1 0.536537 0.339110 0.756014 11.00000 0.05951 0.05571 = 0.05903 -0.00393 0.01297 -0.00164 AFIX 43 H85 2 0.484620 0.301798 0.720250 11.00000 -1.20000 AFIX 0 C86 1 0.631714 0.305681 0.779486 11.00000 0.06862 0.04671 = 0.08833 0.00207 0.02628 0.00669 C87 1 0.707360 0.363467 0.832487 11.00000 0.05515 0.05707 = 0.09568 0.00577 0.01389 0.01781 AFIX 43 H87 2 0.772293 0.342166 0.849345 11.00000 -1.20000 AFIX 0 C88 1 0.689156 0.450930 0.860674 11.00000 0.04483 0.05418 = 0.06478 0.00247 0.01076 0.00799 AFIX 43 H88 2 0.742174 0.488769 0.895586 11.00000 -1.20000 AFIX 0 C89 1 0.722592 0.577794 0.723379 11.00000 0.06643 0.08743 = 0.07262 0.02360 0.02992 0.01417 C90 1 0.651520 0.521948 0.660524 11.00000 0.09188 0.11255 = 0.07201 0.00531 0.03454 0.01216 AFIX 137 H90A 2 0.637001 0.561955 0.629108 11.00000 -1.50000 H90B 2 0.584894 0.497002 0.667702 11.00000 -1.50000 H90C 2 0.686483 0.470600 0.643921 11.00000 -1.50000 AFIX 0 C91 1 0.653941 0.208763 0.748552 11.00000 0.10179 0.05950 = 0.13521 -0.00900 0.02758 0.01815 AFIX 23 H91A 2 0.587167 0.174107 0.718885 11.00000 -1.20000 H91B 2 0.704422 0.217557 0.722372 11.00000 -1.20000 AFIX 0 C92 1 0.696180 0.153136 0.793936 11.00000 0.24750 0.08270 = 0.18291 -0.00945 -0.06525 0.05809 AFIX 137 H92A 2 0.769921 0.178456 0.816135 11.00000 -1.50000 H92B 2 0.692762 0.089083 0.770893 11.00000 -1.50000 H92C 2 0.654586 0.154035 0.825648 11.00000 -1.50000 AFIX 0 C94 1 0.677280 0.354589 0.296258 11.00000 0.13229 0.36592 = 0.14432 -0.12324 0.07357 -0.14395 AFIX 23 H94A 2 0.713222 0.336558 0.336710 11.00000 -1.20000 H94B 2 0.670354 0.303251 0.258781 11.00000 -1.20000 AFIX 0 C95 1 0.999082 0.663015 0.653240 11.00000 0.08912 0.12209 = 0.09241 0.04100 0.00968 -0.00583 AFIX 23 H95A 2 1.015807 0.709303 0.628293 11.00000 -1.20000 H95B 2 1.042648 0.612603 0.646497 11.00000 -1.20000 AFIX 0 C96 1 1.030483 0.708830 0.723745 11.00000 0.11805 0.11754 = 0.10506 0.01501 -0.00023 -0.01251 AFIX 137 H96A 2 0.988305 0.759237 0.731126 11.00000 -1.50000 H96B 2 1.105653 0.734137 0.736738 11.00000 -1.50000 H96C 2 1.017937 0.662947 0.749276 11.00000 -1.50000 AFIX 0 C98 1 0.721003 0.432170 0.289506 11.00000 0.25407 0.41731 = 0.17960 0.12936 0.04056 0.21912 AFIX 137 H98A 2 0.761405 0.420163 0.257302 11.00000 -1.50000 H98B 2 0.768631 0.465096 0.330898 11.00000 -1.50000 H98C 2 0.666273 0.470338 0.275173 11.00000 -1.50000 AFIX 0 H1 2 0.776041 0.631578 0.539787 11.00000 0.08554 H2 2 0.589202 0.616177 0.753316 11.00000 0.11883 H4 2 0.581909 0.426665 0.341915 11.00000 0.14474 H3 2 0.867620 0.606949 0.669261 11.00000 0.16615 HKLF 4 REM PP_DH_JP_81_0m_a.res in P-1 REM R1 = 0.0686 for 8797 Fo > 4sig(Fo) and 0.1256 for all 15452 data REM 941 parameters refined using 0 restraints END WGHT 0.1192 0.3890 REM Highest difference peak 0.382, deepest hole -0.340, 1-sigma level 0.056 Q1 1 0.6769 0.2778 0.3123 11.00000 0.05 0.38 Q2 1 0.7630 0.3338 0.3024 11.00000 0.05 0.34 Q3 1 0.6634 0.3757 0.2835 11.00000 0.05 0.33 Q4 1 0.7534 0.2131 0.7415 11.00000 0.05 0.27 Q5 1 0.8521 0.6686 0.7518 11.00000 0.05 0.25 ; _shelx_res_checksum 76124 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 O1 O 0.6087(2) 0.4965(2) 0.42330(16) 0.1322(12) Uani 1 1 d . . O2 O 0.8206(2) 0.5864(2) 0.73436(13) 0.1049(9) Uani 1 1 d . . O3 O 0.8916(2) 0.6254(2) 0.62824(12) 0.0905(7) Uani 1 1 d . . O4 O 0.5677(2) 0.3911(2) 0.29893(15) 0.1117(10) Uani 1 1 d . . N1 N 0.7058(2) 0.61376(17) 0.50502(12) 0.0597(6) Uani 1 1 d . . N2 N 0.6724(2) 0.61832(18) 0.76777(12) 0.0601(6) Uani 1 1 d . . C1 C 0.89258(18) 0.84875(17) 0.56659(11) 0.0407(5) Uani 1 1 d . . C2 C 0.86003(19) 0.89147(17) 0.62667(11) 0.0424(6) Uani 1 1 d . . C3 C 0.94962(19) 0.93924(17) 0.67220(12) 0.0438(6) Uani 1 1 d . . C4 C 1.04309(18) 0.93251(17) 0.64381(11) 0.0418(6) Uani 1 1 d . . C5 C 1.01029(18) 0.87989(17) 0.58159(11) 0.0408(5) Uani 1 1 d . . C6 C 0.7498(2) 0.88208(18) 0.63641(11) 0.0448(6) Uani 1 1 d . . C7 C 0.7009(2) 0.7980(2) 0.64430(14) 0.0582(7) Uani 1 1 d . . H7 H 0.737499 0.745389 0.643608 0.070 Uiso 1 1 calc R U C8 C 0.5976(3) 0.7911(3) 0.65326(16) 0.0733(9) Uani 1 1 d . . H8 H 0.565384 0.733873 0.658293 0.088 Uiso 1 1 calc R U C9 C 0.5429(2) 0.8678(3) 0.65473(15) 0.0691(8) Uani 1 1 d . . H9 H 0.473280 0.862745 0.660017 0.083 Uiso 1 1 calc R U C10 C 0.5912(2) 0.9513(3) 0.64840(16) 0.0702(9) Uani 1 1 d . . H10 H 0.554727 1.003993 0.650026 0.084 Uiso 1 1 calc R U C11 C 0.6936(2) 0.9590(2) 0.63960(15) 0.0617(8) Uani 1 1 d . . H11 H 0.725573 1.017087 0.635727 0.074 Uiso 1 1 calc R U C12 C 0.9562(2) 0.9930(2) 0.73901(12) 0.0524(7) Uani 1 1 d . . C13 C 0.9068(2) 0.9540(3) 0.78119(14) 0.0682(8) Uani 1 1 d . . H13 H 0.868232 0.893334 0.767166 0.082 Uiso 1 1 calc R U C14 C 0.9149(3) 1.0052(3) 0.84413(16) 0.0908(12) Uani 1 1 d . . H14 H 0.880499 0.978987 0.871650 0.109 Uiso 1 1 calc R U C15 C 0.9722(3) 1.0928(4) 0.86574(19) 0.1047(15) Uani 1 1 d . . H15 H 0.978617 1.126024 0.908313 0.126 Uiso 1 1 calc R U C16 C 1.0206(3) 1.1324(3) 0.8249(2) 0.1051(15) Uani 1 1 d . . H16 H 1.059263 1.192995 0.839614 0.126 Uiso 1 1 calc R U C17 C 1.0125(2) 1.0829(2) 0.76124(16) 0.0749(9) Uani 1 1 d . . H17 H 1.045261 1.110739 0.733709 0.090 Uiso 1 1 calc R U C18 C 1.15620(19) 0.97380(17) 0.67934(12) 0.0444(6) Uani 1 1 d . . C19 C 1.2056(2) 0.9493(2) 0.73788(13) 0.0593(7) Uani 1 1 d . . H19 H 1.166187 0.910102 0.756327 0.071 Uiso 1 1 calc R U C20 C 1.3130(2) 0.9825(2) 0.76937(15) 0.0693(8) Uani 1 1 d . . H20 H 1.344972 0.965734 0.808831 0.083 Uiso 1 1 calc R U C21 C 1.3715(2) 1.0391(2) 0.74294(16) 0.0695(8) Uani 1 1 d . . H21 H 1.444098 1.060206 0.763618 0.083 Uiso 1 1 calc R U C22 C 1.3234(2) 1.0654(2) 0.68546(16) 0.0681(8) Uani 1 1 d . . H22 H 1.362913 1.105793 0.667872 0.082 Uiso 1 1 calc R U C23 C 1.2172(2) 1.0323(2) 0.65380(14) 0.0571(7) Uani 1 1 d . . H23 H 1.185977 1.049673 0.614450 0.068 Uiso 1 1 calc R U C24 C 1.08180(19) 0.86577(17) 0.53688(11) 0.0424(6) Uani 1 1 d . . C25 C 1.1782(2) 0.8291(2) 0.55530(13) 0.0539(7) Uani 1 1 d . . H25 H 1.195992 0.809641 0.595211 0.065 Uiso 1 1 calc R U C26 C 1.2473(2) 0.8212(2) 0.51557(16) 0.0688(8) Uani 1 1 d . . H26 H 1.311725 0.797026 0.528825 0.083 Uiso 1 1 calc R U C27 C 1.2218(3) 0.8490(2) 0.45616(17) 0.0736(9) Uani 1 1 d . . H27 H 1.268710 0.843395 0.429180 0.088 Uiso 1 1 calc R U C28 C 1.1276(2) 0.8849(2) 0.43696(14) 0.0624(8) Uani 1 1 d . . H28 H 1.109998 0.903335 0.396691 0.075 Uiso 1 1 calc R U C29 C 1.0583(2) 0.89378(18) 0.47690(12) 0.0479(6) Uani 1 1 d . . H29 H 0.994722 0.919024 0.463477 0.058 Uiso 1 1 calc R U C30 C 0.82780(19) 0.79082(17) 0.51104(11) 0.0426(6) Uani 1 1 d . . C31 C 0.7074(2) 0.7782(2) 0.49523(12) 0.0498(6) Uani 1 1 d . . C32 C 0.6488(2) 0.6887(2) 0.48780(13) 0.0558(7) Uani 1 1 d . . C33 C 0.5372(2) 0.6756(3) 0.46579(16) 0.0760(9) Uani 1 1 d . . H33 H 0.498244 0.616636 0.461435 0.091 Uiso 1 1 calc R U C34 C 0.4850(3) 0.7496(3) 0.45056(18) 0.0883(11) Uani 1 1 d . . H34 H 0.410291 0.739682 0.434065 0.106 Uiso 1 1 calc R U C35 C 0.5394(3) 0.8380(3) 0.45889(16) 0.0807(10) Uani 1 1 d . . H35 H 0.501678 0.887889 0.449539 0.097 Uiso 1 1 calc R U C36 C 0.6522(2) 0.8533(2) 0.48156(14) 0.0655(8) Uani 1 1 d . . H36 H 0.689775 0.913368 0.487391 0.079 Uiso 1 1 calc R U C37 C 0.86760(19) 0.73614(17) 0.45807(12) 0.0436(6) Uani 1 1 d . . C38 C 0.9486(2) 0.67950(19) 0.46953(13) 0.0554(7) Uani 1 1 d . . H38 H 0.978643 0.672767 0.512308 0.067 Uiso 1 1 calc R U C39 C 0.9854(3) 0.6329(2) 0.41871(15) 0.0691(8) Uani 1 1 d . . H39 H 1.038862 0.594444 0.427843 0.083 Uiso 1 1 calc R U C40 C 0.9447(3) 0.6420(2) 0.35471(15) 0.0722(9) Uani 1 1 d . . C41 C 0.8621(3) 0.6961(2) 0.34284(14) 0.0722(9) Uani 1 1 d . . H41 H 0.832768 0.702998 0.299994 0.087 Uiso 1 1 calc R U C42 C 0.8218(2) 0.7404(2) 0.39281(13) 0.0568(7) Uani 1 1 d . . H42 H 0.763356 0.773511 0.382837 0.068 Uiso 1 1 calc R U C43 C 0.6855(3) 0.5230(3) 0.47084(17) 0.0801(10) Uani 1 1 d . . C44 C 0.7630(4) 0.4589(3) 0.4937(2) 0.1083(14) Uani 1 1 d . . H44A H 0.724673 0.397396 0.489797 0.163 Uiso 1 1 calc R U H44B H 0.801091 0.484088 0.538950 0.163 Uiso 1 1 calc R U H44C H 0.813521 0.453749 0.467252 0.163 Uiso 1 1 calc R U C45 C 0.9919(4) 0.5964(3) 0.29993(19) 0.1063(14) Uani 1 1 d . . H45A H 1.011747 0.535748 0.308121 0.128 Uiso 1 1 calc R U H45B H 0.936484 0.584271 0.258539 0.128 Uiso 1 1 calc R U C46 C 1.0859(6) 0.6530(4) 0.2933(3) 0.189(3) Uani 1 1 d . . H46A H 1.063995 0.706860 0.275726 0.284 Uiso 1 1 calc R U H46B H 1.119140 0.615227 0.263964 0.284 Uiso 1 1 calc R U H46C H 1.136533 0.674251 0.335654 0.284 Uiso 1 1 calc R U C47 C 0.47928(19) 0.59991(17) 0.88230(11) 0.0404(5) Uani 1 1 d . . C48 C 0.44377(19) 0.69455(17) 0.89601(11) 0.0428(6) Uani 1 1 d . . C49 C 0.34429(19) 0.68194(17) 0.90718(11) 0.0434(6) Uani 1 1 d . . C50 C 0.31199(19) 0.58044(18) 0.90249(11) 0.0429(6) Uani 1 1 d . . C51 C 0.39127(18) 0.53108(17) 0.88780(11) 0.0414(6) Uani 1 1 d . . C52 C 0.5010(2) 0.78683(17) 0.89415(12) 0.0451(6) Uani 1 1 d . . C53 C 0.5297(2) 0.80370(19) 0.83804(13) 0.0524(7) Uani 1 1 d . . H53 H 0.512015 0.756134 0.800127 0.063 Uiso 1 1 calc R U C54 C 0.5840(3) 0.8899(2) 0.83806(15) 0.0670(8) Uani 1 1 d . . H54 H 0.603412 0.899499 0.800351 0.080 Uiso 1 1 calc R U C55 C 0.6096(3) 0.9613(2) 0.89253(17) 0.0742(9) Uani 1 1 d . . H55 H 0.645902 1.019431 0.892003 0.089 Uiso 1 1 calc R U C56 C 0.5815(3) 0.9468(2) 0.94816(16) 0.0722(9) Uani 1 1 d . . H56 H 0.599220 0.995104 0.985645 0.087 Uiso 1 1 calc R U C57 C 0.5268(2) 0.8607(2) 0.94883(14) 0.0593(7) Uani 1 1 d . . H57 H 0.507029 0.852254 0.986645 0.071 Uiso 1 1 calc R U C58 C 0.2793(2) 0.75705(18) 0.92494(12) 0.0487(6) Uani 1 1 d . . C59 C 0.2536(2) 0.8241(2) 0.88723(14) 0.0626(8) Uani 1 1 d . . H59 H 0.277148 0.822295 0.849290 0.075 Uiso 1 1 calc R U C60 C 0.1930(3) 0.8941(2) 0.90528(18) 0.0763(9) Uani 1 1 d . . H60 H 0.175367 0.938125 0.879127 0.092 Uiso 1 1 calc R U C61 C 0.1595(3) 0.8983(3) 0.9611(2) 0.0863(11) Uani 1 1 d . . H61 H 0.120036 0.945905 0.973504 0.104 Uiso 1 1 calc R U C62 C 0.1837(3) 0.8324(3) 0.99906(18) 0.0806(10) Uani 1 1 d . . H62 H 0.160218 0.835241 1.037107 0.097 Uiso 1 1 calc R U C63 C 0.2428(2) 0.7619(2) 0.98116(14) 0.0625(8) Uani 1 1 d . . H63 H 0.258231 0.717195 1.007046 0.075 Uiso 1 1 calc R U C64 C 0.20749(19) 0.53975(19) 0.91025(12) 0.0478(6) Uani 1 1 d . . C65 C 0.1105(2) 0.5635(2) 0.87526(14) 0.0617(8) Uani 1 1 d . . H65 H 0.112207 0.607451 0.848600 0.074 Uiso 1 1 calc R U C66 C 0.0131(2) 0.5231(3) 0.87969(17) 0.0746(9) Uani 1 1 d . . H66 H -0.050644 0.539043 0.855670 0.090 Uiso 1 1 calc R U C67 C 0.0094(3) 0.4594(3) 0.91926(19) 0.0808(10) Uani 1 1 d . . H67 H -0.056867 0.432087 0.922061 0.097 Uiso 1 1 calc R U C68 C 0.1041(2) 0.4353(2) 0.95527(17) 0.0724(9) Uani 1 1 d . . H68 H 0.101522 0.392552 0.982619 0.087 Uiso 1 1 calc R U C69 C 0.2017(2) 0.4750(2) 0.95037(13) 0.0565(7) Uani 1 1 d . . H69 H 0.265084 0.458191 0.974288 0.068 Uiso 1 1 calc R U C70 C 0.39198(18) 0.42805(17) 0.88515(11) 0.0416(6) Uani 1 1 d . . C71 C 0.3089(2) 0.3625(2) 0.84261(13) 0.0550(7) Uani 1 1 d . . H71 H 0.252340 0.383231 0.814983 0.066 Uiso 1 1 calc R U C72 C 0.3088(3) 0.2667(2) 0.84068(15) 0.0680(8) Uani 1 1 d . . H72 H 0.253025 0.223453 0.811293 0.082 Uiso 1 1 calc R U C73 C 0.3904(3) 0.2348(2) 0.88174(16) 0.0708(9) Uani 1 1 d . . H73 H 0.389849 0.170274 0.880616 0.085 Uiso 1 1 calc R U C74 C 0.4731(2) 0.2990(2) 0.92459(14) 0.0602(7) Uani 1 1 d . . H74 H 0.528928 0.277707 0.952410 0.072 Uiso 1 1 calc R U C75 C 0.4737(2) 0.39429(19) 0.92656(12) 0.0479(6) Uani 1 1 d . . H75 H 0.529727 0.437004 0.956148 0.057 Uiso 1 1 calc R U C76 C 0.57303(19) 0.57973(17) 0.86733(11) 0.0418(6) Uani 1 1 d . . C77 C 0.66911(19) 0.65338(18) 0.88192(12) 0.0465(6) Uani 1 1 d . . C78 C 0.7221(2) 0.66635(19) 0.83421(14) 0.0548(7) Uani 1 1 d . . C79 C 0.8167(3) 0.7279(2) 0.8507(2) 0.0777(9) Uani 1 1 d . . H79 H 0.852239 0.736012 0.818674 0.093 Uiso 1 1 calc R U C80 C 0.8582(3) 0.7770(3) 0.9139(2) 0.0925(12) Uani 1 1 d . . H80 H 0.923180 0.817071 0.924989 0.111 Uiso 1 1 calc R U C81 C 0.8054(3) 0.7681(2) 0.9614(2) 0.0842(11) Uani 1 1 d . . H81 H 0.833026 0.803783 1.004035 0.101 Uiso 1 1 calc R U C82 C 0.7110(2) 0.7059(2) 0.94580(14) 0.0614(7) Uani 1 1 d . . H82 H 0.675395 0.699082 0.978029 0.074 Uiso 1 1 calc R U C83 C 0.59137(19) 0.48391(17) 0.83738(12) 0.0441(6) Uani 1 1 d . . C84 C 0.5163(2) 0.42623(19) 0.78411(13) 0.0515(6) Uani 1 1 d . . H84 H 0.451093 0.446922 0.767079 0.062 Uiso 1 1 calc R U C85 C 0.5365(2) 0.3391(2) 0.75601(14) 0.0612(7) Uani 1 1 d . . H85 H 0.484620 0.301798 0.720250 0.073 Uiso 1 1 calc R U C86 C 0.6317(3) 0.3057(2) 0.77949(17) 0.0685(8) Uani 1 1 d . . C87 C 0.7074(2) 0.3635(2) 0.83249(17) 0.0711(9) Uani 1 1 d . . H87 H 0.772293 0.342166 0.849345 0.085 Uiso 1 1 calc R U C88 C 0.6892(2) 0.4509(2) 0.86067(14) 0.0565(7) Uani 1 1 d . . H88 H 0.742174 0.488769 0.895586 0.068 Uiso 1 1 calc R U C89 C 0.7226(3) 0.5778(2) 0.72338(17) 0.0723(9) Uani 1 1 d . . C90 C 0.6515(3) 0.5219(3) 0.66052(17) 0.0918(11) Uani 1 1 d . . H90A H 0.637001 0.561955 0.629108 0.138 Uiso 1 1 calc R U H90B H 0.584894 0.497002 0.667702 0.138 Uiso 1 1 calc R U H90C H 0.686483 0.470600 0.643921 0.138 Uiso 1 1 calc R U C91 C 0.6539(3) 0.2088(3) 0.7486(2) 0.1029(13) Uani 1 1 d . . H91A H 0.587167 0.174107 0.718885 0.123 Uiso 1 1 calc R U H91B H 0.704422 0.217557 0.722372 0.123 Uiso 1 1 calc R U C92 C 0.6962(6) 0.1531(4) 0.7939(3) 0.195(3) Uani 1 1 d . . H92A H 0.769921 0.178456 0.816135 0.293 Uiso 1 1 calc R U H92B H 0.692762 0.089083 0.770893 0.293 Uiso 1 1 calc R U H92C H 0.654586 0.154035 0.825648 0.293 Uiso 1 1 calc R U C94 C 0.6773(6) 0.3546(7) 0.2963(4) 0.242(6) Uani 1 1 d . . H94A H 0.713222 0.336558 0.336710 0.290 Uiso 1 1 calc R U H94B H 0.670354 0.303251 0.258781 0.290 Uiso 1 1 calc R U C95 C 0.9991(3) 0.6630(3) 0.6532(2) 0.1025(13) Uani 1 1 d . . H95A H 1.015807 0.709303 0.628293 0.123 Uiso 1 1 calc R U H95B H 1.042648 0.612603 0.646497 0.123 Uiso 1 1 calc R U C96 C 1.0305(4) 0.7088(3) 0.7237(2) 0.1216(15) Uani 1 1 d . . H96A H 0.988305 0.759237 0.731126 0.182 Uiso 1 1 calc R U H96B H 1.105653 0.734137 0.736738 0.182 Uiso 1 1 calc R U H96C H 1.017937 0.662947 0.749276 0.182 Uiso 1 1 calc R U C98 C 0.7210(8) 0.4322(9) 0.2895(4) 0.267(6) Uani 1 1 d . . H98A H 0.761405 0.420163 0.257302 0.401 Uiso 1 1 calc R U H98B H 0.768631 0.465096 0.330898 0.401 Uiso 1 1 calc R U H98C H 0.666273 0.470338 0.275173 0.401 Uiso 1 1 calc R U H1 H 0.776(3) 0.632(2) 0.5398(17) 0.086(10) Uiso 1 1 d . . H2 H 0.589(3) 0.616(3) 0.753(2) 0.119(13) Uiso 1 1 d . . H4 H 0.582(4) 0.427(4) 0.342(3) 0.145(18) Uiso 1 1 d . . H3 H 0.868(4) 0.607(4) 0.669(3) 0.17(2) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.103(2) 0.112(2) 0.123(2) -0.0489(18) -0.0306(18) 0.0268(17) O2 0.0675(16) 0.162(3) 0.0916(18) 0.0187(17) 0.0354(14) 0.0236(16) O3 0.0739(16) 0.119(2) 0.0696(15) 0.0213(14) 0.0040(13) 0.0064(14) O4 0.0753(18) 0.155(3) 0.0789(18) -0.0195(18) 0.0152(14) -0.0169(17) N1 0.0524(14) 0.0581(16) 0.0605(15) 0.0061(12) 0.0066(12) 0.0006(12) N2 0.0520(15) 0.0721(16) 0.0611(15) 0.0161(12) 0.0233(12) 0.0064(12) C1 0.0388(13) 0.0440(14) 0.0404(13) 0.0115(10) 0.0093(10) 0.0090(11) C2 0.0412(13) 0.0450(14) 0.0427(13) 0.0092(11) 0.0134(11) 0.0082(11) C3 0.0418(14) 0.0486(15) 0.0416(13) 0.0094(11) 0.0124(11) 0.0058(11) C4 0.0383(13) 0.0477(14) 0.0401(13) 0.0121(11) 0.0094(10) 0.0060(11) C5 0.0372(13) 0.0464(14) 0.0408(13) 0.0124(11) 0.0105(10) 0.0087(10) C6 0.0434(14) 0.0539(16) 0.0376(13) 0.0079(11) 0.0120(11) 0.0079(12) C7 0.0527(17) 0.0598(18) 0.0666(18) 0.0177(14) 0.0209(14) 0.0072(14) C8 0.061(2) 0.081(2) 0.081(2) 0.0156(18) 0.0317(17) -0.0046(17) C9 0.0465(17) 0.093(3) 0.069(2) 0.0095(17) 0.0243(15) 0.0064(17) C10 0.0590(19) 0.082(2) 0.078(2) 0.0128(17) 0.0314(17) 0.0248(17) C11 0.0589(18) 0.0603(18) 0.075(2) 0.0147(15) 0.0331(16) 0.0121(14) C12 0.0398(14) 0.0698(19) 0.0431(14) 0.0006(13) 0.0109(12) 0.0073(13) C13 0.0633(19) 0.094(2) 0.0484(16) 0.0105(16) 0.0187(14) 0.0144(16) C14 0.073(2) 0.150(4) 0.0508(19) 0.008(2) 0.0261(17) 0.022(2) C15 0.067(2) 0.162(4) 0.063(2) -0.035(2) 0.0225(19) 0.008(3) C16 0.064(2) 0.118(3) 0.102(3) -0.054(2) 0.028(2) -0.012(2) C17 0.0604(19) 0.083(2) 0.071(2) -0.0172(17) 0.0258(16) -0.0021(17) C18 0.0406(13) 0.0468(15) 0.0440(13) 0.0042(11) 0.0119(11) 0.0051(11) C19 0.0544(17) 0.0707(19) 0.0474(15) 0.0160(13) 0.0045(13) -0.0029(14) C20 0.0539(18) 0.085(2) 0.0591(18) 0.0199(16) -0.0041(14) 0.0027(16) C21 0.0406(15) 0.080(2) 0.076(2) 0.0081(17) 0.0015(15) 0.0010(15) C22 0.0476(17) 0.073(2) 0.082(2) 0.0238(17) 0.0136(16) -0.0043(14) C23 0.0456(15) 0.0622(18) 0.0629(17) 0.0210(14) 0.0090(13) 0.0032(13) C24 0.0405(13) 0.0452(14) 0.0410(13) 0.0062(11) 0.0111(11) 0.0076(11) C25 0.0490(15) 0.0655(18) 0.0519(15) 0.0174(13) 0.0140(13) 0.0197(13) C26 0.0516(17) 0.084(2) 0.080(2) 0.0191(17) 0.0260(16) 0.0292(16) C27 0.071(2) 0.094(2) 0.078(2) 0.0301(19) 0.0463(18) 0.0311(18) C28 0.0689(19) 0.074(2) 0.0574(17) 0.0253(15) 0.0294(15) 0.0218(16) C29 0.0474(15) 0.0512(15) 0.0501(15) 0.0138(12) 0.0167(12) 0.0151(12) C30 0.0414(13) 0.0455(14) 0.0406(13) 0.0117(11) 0.0073(11) 0.0088(11) C31 0.0442(14) 0.0623(18) 0.0401(13) 0.0047(12) 0.0066(11) 0.0176(13) C32 0.0418(15) 0.0686(19) 0.0480(15) -0.0014(13) 0.0070(12) 0.0018(14) C33 0.0456(17) 0.090(2) 0.080(2) -0.0062(18) 0.0113(15) 0.0047(17) C34 0.0482(18) 0.108(3) 0.091(3) -0.010(2) 0.0032(17) 0.021(2) C35 0.066(2) 0.106(3) 0.070(2) 0.0085(19) 0.0118(17) 0.049(2) C36 0.0644(19) 0.077(2) 0.0548(17) 0.0093(15) 0.0116(14) 0.0298(16) C37 0.0395(13) 0.0445(14) 0.0438(13) 0.0051(11) 0.0073(11) 0.0082(11) C38 0.0592(17) 0.0567(17) 0.0476(15) 0.0107(13) 0.0063(13) 0.0158(14) C39 0.071(2) 0.069(2) 0.067(2) 0.0069(15) 0.0155(16) 0.0338(16) C40 0.079(2) 0.077(2) 0.0537(18) -0.0069(15) 0.0179(16) 0.0208(18) C41 0.086(2) 0.084(2) 0.0403(15) 0.0030(14) 0.0071(15) 0.0274(18) C42 0.0586(17) 0.0616(18) 0.0448(15) 0.0055(13) 0.0035(13) 0.0194(14) C43 0.072(2) 0.072(2) 0.075(2) -0.0080(18) -0.0025(18) 0.0043(18) C44 0.120(3) 0.068(2) 0.121(3) 0.009(2) 0.004(3) 0.023(2) C45 0.122(3) 0.119(3) 0.077(2) -0.011(2) 0.040(2) 0.046(3) C46 0.248(8) 0.162(5) 0.196(6) -0.016(4) 0.175(6) 0.013(5) C47 0.0408(13) 0.0440(14) 0.0334(12) 0.0047(10) 0.0073(10) 0.0036(11) C48 0.0457(14) 0.0452(15) 0.0359(12) 0.0043(10) 0.0098(11) 0.0098(11) C49 0.0439(14) 0.0509(15) 0.0343(12) 0.0043(10) 0.0100(10) 0.0107(11) C50 0.0382(13) 0.0540(16) 0.0345(12) 0.0095(11) 0.0056(10) 0.0065(11) C51 0.0398(13) 0.0481(15) 0.0337(12) 0.0066(10) 0.0057(10) 0.0070(11) C52 0.0465(14) 0.0438(15) 0.0449(14) 0.0073(11) 0.0118(11) 0.0110(11) C53 0.0571(16) 0.0550(17) 0.0429(14) 0.0089(12) 0.0105(12) 0.0066(13) C54 0.078(2) 0.064(2) 0.0640(19) 0.0230(16) 0.0226(16) 0.0012(16) C55 0.088(2) 0.0521(19) 0.082(2) 0.0134(17) 0.0266(19) -0.0047(16) C56 0.088(2) 0.0494(18) 0.072(2) -0.0035(15) 0.0236(18) -0.0016(16) C57 0.0728(19) 0.0526(17) 0.0507(16) 0.0006(13) 0.0205(14) 0.0084(14) C58 0.0443(14) 0.0546(16) 0.0437(14) 0.0022(12) 0.0092(11) 0.0122(12) C59 0.0669(19) 0.0668(19) 0.0554(16) 0.0103(14) 0.0155(14) 0.0242(15) C60 0.081(2) 0.070(2) 0.079(2) 0.0127(17) 0.0169(19) 0.0342(18) C61 0.073(2) 0.086(3) 0.092(3) -0.008(2) 0.019(2) 0.0352(19) C62 0.074(2) 0.099(3) 0.070(2) -0.003(2) 0.0343(18) 0.020(2) C63 0.0617(18) 0.076(2) 0.0525(16) 0.0064(14) 0.0211(14) 0.0212(15) C64 0.0401(14) 0.0584(16) 0.0419(13) 0.0057(12) 0.0088(11) 0.0071(12) C65 0.0504(17) 0.077(2) 0.0543(16) 0.0137(14) 0.0045(13) 0.0152(15) C66 0.0370(16) 0.102(3) 0.076(2) 0.0097(19) 0.0029(15) 0.0146(16) C67 0.0472(18) 0.097(3) 0.094(3) 0.011(2) 0.0224(18) -0.0033(17) C68 0.0534(19) 0.089(2) 0.080(2) 0.0261(18) 0.0240(16) 0.0013(16) C69 0.0420(15) 0.076(2) 0.0542(16) 0.0185(14) 0.0132(12) 0.0087(13) C70 0.0363(13) 0.0484(15) 0.0384(12) 0.0069(10) 0.0099(10) 0.0013(11) C71 0.0476(15) 0.0557(18) 0.0530(16) 0.0044(13) 0.0041(12) 0.0010(13) C72 0.0664(19) 0.0564(19) 0.0668(19) -0.0006(15) 0.0084(16) -0.0143(15) C73 0.092(2) 0.0469(17) 0.070(2) 0.0134(15) 0.0177(18) 0.0014(16) C74 0.0689(19) 0.0563(18) 0.0556(16) 0.0166(14) 0.0108(14) 0.0147(15) C75 0.0489(15) 0.0519(16) 0.0401(13) 0.0072(11) 0.0097(11) 0.0030(12) C76 0.0427(14) 0.0464(14) 0.0355(12) 0.0081(10) 0.0094(10) 0.0060(11) C77 0.0382(13) 0.0471(15) 0.0520(15) 0.0094(12) 0.0076(12) 0.0077(11) C78 0.0426(15) 0.0538(17) 0.0690(18) 0.0141(14) 0.0164(14) 0.0045(12) C79 0.0571(19) 0.069(2) 0.108(3) 0.018(2) 0.0280(19) -0.0025(16) C80 0.054(2) 0.073(2) 0.131(4) 0.009(2) 0.006(2) -0.0161(17) C81 0.063(2) 0.069(2) 0.091(3) -0.0014(18) -0.0156(19) -0.0100(17) C82 0.0586(17) 0.0579(18) 0.0585(17) 0.0046(14) 0.0043(14) 0.0056(14) C83 0.0398(13) 0.0485(15) 0.0447(14) 0.0074(11) 0.0147(11) 0.0043(11) C84 0.0474(15) 0.0514(16) 0.0538(15) 0.0058(12) 0.0143(12) 0.0057(12) C85 0.0595(18) 0.0557(18) 0.0590(17) -0.0039(13) 0.0130(14) -0.0016(14) C86 0.069(2) 0.0467(17) 0.088(2) 0.0021(15) 0.0263(18) 0.0067(15) C87 0.0551(18) 0.0571(19) 0.096(2) 0.0058(17) 0.0139(17) 0.0178(15) C88 0.0448(15) 0.0542(17) 0.0648(17) 0.0025(13) 0.0108(13) 0.0080(13) C89 0.066(2) 0.087(2) 0.073(2) 0.0236(18) 0.0299(18) 0.0142(18) C90 0.092(3) 0.113(3) 0.072(2) 0.005(2) 0.035(2) 0.012(2) C91 0.102(3) 0.059(2) 0.135(4) -0.009(2) 0.028(3) 0.018(2) C92 0.248(8) 0.083(3) 0.183(6) -0.009(4) -0.065(5) 0.058(4) C94 0.132(5) 0.366(13) 0.144(6) -0.123(7) 0.074(4) -0.144(7) C95 0.089(3) 0.122(3) 0.092(3) 0.041(3) 0.010(2) -0.006(2) C96 0.118(4) 0.118(4) 0.105(3) 0.015(3) 0.000(3) -0.013(3) C98 0.254(11) 0.417(17) 0.180(8) 0.129(10) 0.041(8) 0.219(12) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C95 O3 H3 105(3) C94 O4 H4 103(3) C43 N1 C32 125.8(3) C43 N1 H1 115.9(19) C32 N1 H1 117.0(19) C89 N2 C78 126.7(3) C89 N2 H2 119(2) C78 N2 H2 115(2) C30 C1 C5 127.8(2) C30 C1 C2 126.7(2) C5 C1 C2 105.44(19) C3 C2 C6 125.2(2) C3 C2 C1 108.1(2) C6 C2 C1 126.7(2) C2 C3 C12 127.2(2) C2 C3 C4 108.9(2) C12 C3 C4 123.8(2) C5 C4 C3 109.5(2) C5 C4 C18 125.5(2) C3 C4 C18 125.0(2) C4 C5 C24 123.6(2) C4 C5 C1 108.0(2) C24 C5 C1 128.2(2) C7 C6 C11 117.6(2) C7 C6 C2 121.9(2) C11 C6 C2 120.5(2) C6 C7 C8 120.7(3) C6 C7 H7 119.7 C8 C7 H7 119.7 C9 C8 C7 120.4(3) C9 C8 H8 119.8 C7 C8 H8 119.8 C10 C9 C8 119.3(3) C10 C9 H9 120.3 C8 C9 H9 120.3 C9 C10 C11 120.7(3) C9 C10 H10 119.6 C11 C10 H10 119.6 C10 C11 C6 121.2(3) C10 C11 H11 119.4 C6 C11 H11 119.4 C17 C12 C13 118.4(3) C17 C12 C3 120.5(3) C13 C12 C3 121.1(3) C14 C13 C12 120.3(3) C14 C13 H13 119.8 C12 C13 H13 119.8 C15 C14 C13 120.6(4) C15 C14 H14 119.7 C13 C14 H14 119.7 C14 C15 C16 119.8(3) C14 C15 H15 120.1 C16 C15 H15 120.1 C15 C16 C17 120.6(4) C15 C16 H16 119.7 C17 C16 H16 119.7 C12 C17 C16 120.3(3) C12 C17 H17 119.9 C16 C17 H17 119.9 C23 C18 C19 117.8(2) C23 C18 C4 121.9(2) C19 C18 C4 120.2(2) C18 C19 C20 120.9(3) C18 C19 H19 119.6 C20 C19 H19 119.6 C21 C20 C19 120.2(3) C21 C20 H20 119.9 C19 C20 H20 119.9 C20 C21 C22 119.7(3) C20 C21 H21 120.2 C22 C21 H21 120.2 C23 C22 C21 120.4(3) C23 C22 H22 119.8 C21 C22 H22 119.8 C22 C23 C18 121.1(3) C22 C23 H23 119.5 C18 C23 H23 119.5 C29 C24 C25 117.6(2) C29 C24 C5 121.3(2) C25 C24 C5 121.1(2) C26 C25 C24 121.0(3) C26 C25 H25 119.5 C24 C25 H25 119.5 C25 C26 C27 120.2(3) C25 C26 H26 119.9 C27 C26 H26 119.9 C28 C27 C26 119.8(3) C28 C27 H27 120.1 C26 C27 H27 120.1 C27 C28 C29 120.3(3) C27 C28 H28 119.9 C29 C28 H28 119.9 C28 C29 C24 121.1(2) C28 C29 H29 119.4 C24 C29 H29 119.4 C1 C30 C37 124.3(2) C1 C30 C31 123.5(2) C37 C30 C31 112.2(2) C36 C31 C32 119.2(3) C36 C31 C30 119.8(3) C32 C31 C30 120.7(2) C33 C32 C31 120.0(3) C33 C32 N1 121.2(3) C31 C32 N1 118.7(2) C34 C33 C32 119.7(3) C34 C33 H33 120.2 C32 C33 H33 120.2 C33 C34 C35 121.6(3) C33 C34 H34 119.2 C35 C34 H34 119.2 C34 C35 C36 119.8(3) C34 C35 H35 120.1 C36 C35 H35 120.1 C31 C36 C35 119.5(3) C31 C36 H36 120.3 C35 C36 H36 120.3 C38 C37 C42 117.1(2) C38 C37 C30 123.6(2) C42 C37 C30 119.3(2) C39 C38 C37 121.2(3) C39 C38 H38 119.4 C37 C38 H38 119.4 C40 C39 C38 121.5(3) C40 C39 H39 119.2 C38 C39 H39 119.2 C39 C40 C41 117.4(3) C39 C40 C45 121.0(3) C41 C40 C45 121.6(3) C40 C41 C42 121.7(3) C40 C41 H41 119.1 C42 C41 H41 119.1 C41 C42 C37 120.8(3) C41 C42 H42 119.6 C37 C42 H42 119.6 O1 C43 N1 121.4(3) O1 C43 C44 122.1(3) N1 C43 C44 116.5(3) C43 C44 H44A 109.5 C43 C44 H44B 109.5 H44A C44 H44B 109.5 C43 C44 H44C 109.5 H44A C44 H44C 109.5 H44B C44 H44C 109.5 C46 C45 C40 114.3(4) C46 C45 H45A 108.7 C40 C45 H45A 108.7 C46 C45 H45B 108.7 C40 C45 H45B 108.7 H45A C45 H45B 107.6 C45 C46 H46A 109.5 C45 C46 H46B 109.5 H46A C46 H46B 109.5 C45 C46 H46C 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 C76 C47 C48 127.3(2) C76 C47 C51 126.9(2) C48 C47 C51 105.79(19) C49 C48 C52 124.8(2) C49 C48 C47 107.8(2) C52 C48 C47 127.2(2) C48 C49 C50 109.3(2) C48 C49 C58 126.7(2) C50 C49 C58 124.0(2) C51 C50 C49 109.2(2) C51 C50 C64 126.3(2) C49 C50 C64 124.5(2) C50 C51 C70 124.6(2) C50 C51 C47 107.9(2) C70 C51 C47 127.1(2) C57 C52 C53 117.4(2) C57 C52 C48 120.5(2) C53 C52 C48 122.2(2) C54 C53 C52 120.8(3) C54 C53 H53 119.6 C52 C53 H53 119.6 C55 C54 C53 120.9(3) C55 C54 H54 119.6 C53 C54 H54 119.6 C54 C55 C56 119.4(3) C54 C55 H55 120.3 C56 C55 H55 120.3 C55 C56 C57 120.3(3) C55 C56 H56 119.8 C57 C56 H56 119.8 C56 C57 C52 121.2(3) C56 C57 H57 119.4 C52 C57 H57 119.4 C59 C58 C63 118.0(3) C59 C58 C49 122.1(2) C63 C58 C49 119.9(2) C58 C59 C60 120.9(3) C58 C59 H59 119.6 C60 C59 H59 119.6 C61 C60 C59 120.1(3) C61 C60 H60 120.0 C59 C60 H60 120.0 C60 C61 C62 120.1(3) C60 C61 H61 120.0 C62 C61 H61 120.0 C61 C62 C63 120.3(3) C61 C62 H62 119.8 C63 C62 H62 119.8 C62 C63 C58 120.7(3) C62 C63 H63 119.7 C58 C63 H63 119.7 C69 C64 C65 117.8(2) C69 C64 C50 121.8(2) C65 C64 C50 120.4(2) C66 C65 C64 121.0(3) C66 C65 H65 119.5 C64 C65 H65 119.5 C67 C66 C65 120.2(3) C67 C66 H66 119.9 C65 C66 H66 119.9 C66 C67 C68 120.2(3) C66 C67 H67 119.9 C68 C67 H67 119.9 C69 C68 C67 119.7(3) C69 C68 H68 120.2 C67 C68 H68 120.2 C68 C69 C64 121.1(3) C68 C69 H69 119.5 C64 C69 H69 119.5 C71 C70 C75 117.8(2) C71 C70 C51 120.8(2) C75 C70 C51 121.4(2) C72 C71 C70 120.8(3) C72 C71 H71 119.6 C70 C71 H71 119.6 C73 C72 C71 120.4(3) C73 C72 H72 119.8 C71 C72 H72 119.8 C72 C73 C74 119.5(3) C72 C73 H73 120.3 C74 C73 H73 120.3 C75 C74 C73 120.3(3) C75 C74 H74 119.8 C73 C74 H74 119.8 C74 C75 C70 121.1(2) C74 C75 H75 119.4 C70 C75 H75 119.4 C47 C76 C83 124.2(2) C47 C76 C77 122.3(2) C83 C76 C77 113.5(2) C78 C77 C82 119.0(3) C78 C77 C76 121.5(2) C82 C77 C76 119.3(2) C79 C78 C77 120.2(3) C79 C78 N2 121.7(3) C77 C78 N2 118.0(2) C80 C79 C78 120.0(3) C80 C79 H79 120.0 C78 C79 H79 120.0 C79 C80 C81 120.9(3) C79 C80 H80 119.6 C81 C80 H80 119.6 C80 C81 C82 119.7(3) C80 C81 H81 120.1 C82 C81 H81 120.1 C81 C82 C77 120.0(3) C81 C82 H82 120.0 C77 C82 H82 120.0 C84 C83 C88 117.6(2) C84 C83 C76 122.2(2) C88 C83 C76 120.1(2) C85 C84 C83 121.1(3) C85 C84 H84 119.4 C83 C84 H84 119.5 C84 C85 C86 121.5(3) C84 C85 H85 119.3 C86 C85 H85 119.3 C85 C86 C87 117.6(3) C85 C86 C91 121.5(3) C87 C86 C91 120.9(3) C88 C87 C86 121.7(3) C88 C87 H87 119.1 C86 C87 H87 119.1 C87 C88 C83 120.4(3) C87 C88 H88 119.8 C83 C88 H88 119.8 O2 C89 N2 122.2(3) O2 C89 C90 121.8(3) N2 C89 C90 116.0(3) C89 C90 H90A 109.5 C89 C90 H90B 109.5 H90A C90 H90B 109.5 C89 C90 H90C 109.5 H90A C90 H90C 109.5 H90B C90 H90C 109.5 C92 C91 C86 114.8(4) C92 C91 H91A 108.6 C86 C91 H91A 108.6 C92 C91 H91B 108.6 C86 C91 H91B 108.6 H91A C91 H91B 107.5 C91 C92 H92A 109.5 C91 C92 H92B 109.5 H92A C92 H92B 109.5 C91 C92 H92C 109.5 H92A C92 H92C 109.5 H92B C92 H92C 109.5 C98 C94 O4 94.5(10) C98 C94 H94A 112.8 O4 C94 H94A 112.8 C98 C94 H94B 112.8 O4 C94 H94B 112.8 H94A C94 H94B 110.3 O3 C95 C96 114.9(4) O3 C95 H95A 108.5 C96 C95 H95A 108.5 O3 C95 H95B 108.5 C96 C95 H95B 108.5 H95A C95 H95B 107.5 C95 C96 H96A 109.5 C95 C96 H96B 109.5 H96A C96 H96B 109.5 C95 C96 H96C 109.5 H96A C96 H96C 109.5 H96B C96 H96C 109.5 C94 C98 H98A 109.5 C94 C98 H98B 109.5 H98A C98 H98B 109.5 C94 C98 H98C 109.5 H98A C98 H98C 109.5 H98B C98 H98C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C43 1.212(4) O2 C89 1.219(4) O3 C95 1.381(4) O3 H3 1.07(6) O4 C94 1.560(10) O4 H4 0.94(5) N1 C43 1.353(4) N1 C32 1.415(4) N1 H1 1.00(3) N2 C89 1.351(4) N2 C78 1.428(4) N2 H2 1.04(4) C1 C30 1.360(3) C1 C5 1.484(3) C1 C2 1.493(3) C2 C3 1.354(3) C2 C6 1.483(3) C3 C12 1.477(3) C3 C4 1.477(3) C4 C5 1.355(3) C4 C18 1.486(3) C5 C24 1.481(3) C6 C7 1.379(4) C6 C11 1.381(4) C7 C8 1.389(4) C7 H7 0.9300 C8 C9 1.365(5) C8 H8 0.9300 C9 C10 1.356(5) C9 H9 0.9300 C10 C11 1.375(4) C10 H10 0.9300 C11 H11 0.9300 C12 C17 1.375(4) C12 C13 1.393(4) C13 C14 1.389(4) C13 H13 0.9300 C14 C15 1.352(6) C14 H14 0.9300 C15 C16 1.366(6) C15 H15 0.9300 C16 C17 1.393(5) C16 H16 0.9300 C17 H17 0.9300 C18 C23 1.376(4) C18 C19 1.384(4) C19 C20 1.384(4) C19 H19 0.9300 C20 C21 1.353(4) C20 H20 0.9300 C21 C22 1.372(4) C21 H21 0.9300 C22 C23 1.371(4) C22 H22 0.9300 C23 H23 0.9300 C24 C29 1.388(3) C24 C25 1.391(3) C25 C26 1.371(4) C25 H25 0.9300 C26 C27 1.375(4) C26 H26 0.9300 C27 C28 1.364(4) C27 H27 0.9300 C28 C29 1.375(4) C28 H28 0.9300 C29 H29 0.9300 C30 C37 1.483(3) C30 C31 1.493(3) C31 C36 1.386(4) C31 C32 1.406(4) C32 C33 1.385(4) C33 C34 1.362(5) C33 H33 0.9300 C34 C35 1.364(5) C34 H34 0.9300 C35 C36 1.401(4) C35 H35 0.9300 C36 H36 0.9300 C37 C38 1.385(3) C37 C42 1.393(3) C38 C39 1.379(4) C38 H38 0.9300 C39 C40 1.377(4) C39 H39 0.9300 C40 C41 1.378(4) C40 C45 1.520(4) C41 C42 1.379(4) C41 H41 0.9300 C42 H42 0.9300 C43 C44 1.479(5) C44 H44A 0.9600 C44 H44B 0.9600 C44 H44C 0.9600 C45 C46 1.454(7) C45 H45A 0.9700 C45 H45B 0.9700 C46 H46A 0.9600 C46 H46B 0.9600 C46 H46C 0.9600 C47 C76 1.365(3) C47 C48 1.484(3) C47 C51 1.485(3) C48 C49 1.363(3) C48 C52 1.481(4) C49 C50 1.471(4) C49 C58 1.480(3) C50 C51 1.362(3) C50 C64 1.481(3) C51 C70 1.484(3) C52 C57 1.386(4) C52 C53 1.394(4) C53 C54 1.377(4) C53 H53 0.9300 C54 C55 1.361(4) C54 H54 0.9300 C55 C56 1.371(4) C55 H55 0.9300 C56 C57 1.381(4) C56 H56 0.9300 C57 H57 0.9300 C58 C59 1.384(4) C58 C63 1.386(4) C59 C60 1.387(4) C59 H59 0.9300 C60 C61 1.357(5) C60 H60 0.9300 C61 C62 1.371(5) C61 H61 0.9300 C62 C63 1.379(4) C62 H62 0.9300 C63 H63 0.9300 C64 C69 1.390(4) C64 C65 1.399(4) C65 C66 1.371(4) C65 H65 0.9300 C66 C67 1.365(5) C66 H66 0.9300 C67 C68 1.386(5) C67 H67 0.9300 C68 C69 1.372(4) C68 H68 0.9300 C69 H69 0.9300 C70 C71 1.384(3) C70 C75 1.388(3) C71 C72 1.380(4) C71 H71 0.9300 C72 C73 1.369(4) C72 H72 0.9300 C73 C74 1.373(4) C73 H73 0.9300 C74 C75 1.373(4) C74 H74 0.9300 C75 H75 0.9300 C76 C83 1.483(3) C76 C77 1.494(3) C77 C78 1.388(4) C77 C82 1.390(4) C78 C79 1.377(4) C79 C80 1.362(5) C79 H79 0.9300 C80 C81 1.371(5) C80 H80 0.9300 C81 C82 1.381(4) C81 H81 0.9300 C82 H82 0.9300 C83 C84 1.383(3) C83 C88 1.397(3) C84 C85 1.370(4) C84 H84 0.9300 C85 C86 1.373(4) C85 H85 0.9300 C86 C87 1.384(4) C86 C91 1.521(4) C87 C88 1.366(4) C87 H87 0.9300 C88 H88 0.9300 C89 C90 1.477(5) C90 H90A 0.9600 C90 H90B 0.9600 C90 H90C 0.9600 C91 C92 1.411(6) C91 H91A 0.9700 C91 H91B 0.9700 C92 H92A 0.9600 C92 H92B 0.9600 C92 H92C 0.9600 C94 C98 1.260(13) C94 H94A 0.9700 C94 H94B 0.9700 C95 C96 1.474(6) C95 H95A 0.9700 C95 H95B 0.9700 C96 H96A 0.9600 C96 H96B 0.9600 C96 H96C 0.9600 C98 H98A 0.9600 C98 H98B 0.9600 C98 H98C 0.9600