#------------------------------------------------------------------------------ #$Date: 2019-05-18 06:53:50 +0300 (Sat, 18 May 2019) $ #$Revision: 215297 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/68/7156869.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_7156869 loop_ _publ_author_name 'Kraevaya, Olga' 'Peregudov, Alexander S.' 'Troyanov, Sergey I.' 'Godovikov, Ivan' 'Fedorova, Natalia E.' 'Klimova, Regina R.' 'Sergeeva, Vasilina' 'Kameneva, Larisa V.' 'Ershova, Elizaveta' 'Martynenko, Vyacheslav M.' 'Claes, Sandra' 'Kushch, Alla A.' 'Kostyuk, Svetlana' 'Schols, Dominique' 'Shestakov, Alexander F.' 'Troshin, Pavel' _publ_section_title ; Diversion of the Arbuzov Reaction: Alkylation of C-Cl Instead of Phosphonic Ester Formation on the Fullerene Cage ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/C9OB00593E _journal_year 2019 _chemical_formula_sum 'C100 H35 O20' _chemical_formula_weight 1556.28 _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-01-24 deposited with the CCDC. 2019-05-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.293(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.893(2) _cell_length_b 16.1500(10) _cell_length_c 20.4330(10) _cell_measurement_reflns_used 33000 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32 _cell_measurement_theta_min 4 _cell_volume 7193.7(9) _computing_cell_refinement XDS _computing_data_collection XDS _computing_data_reduction XDS _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXD _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.915 _diffrn_measured_fraction_theta_max 0.800 _diffrn_measurement_device_type MAR225 _diffrn_measurement_method CCD _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.895 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_Laue_measured_fraction_full 0.915 _diffrn_reflns_Laue_measured_fraction_max 0.800 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 85973 _diffrn_reflns_point_group_measured_fraction_full 0.915 _diffrn_reflns_point_group_measured_fraction_max 0.800 _diffrn_reflns_theta_full 32.450 _diffrn_reflns_theta_max 36.172 _diffrn_reflns_theta_min 2.027 _diffrn_source 'BL 14.3 PSF, BESSY, Berlin, Germany' _exptl_absorpt_coefficient_mu 0.153 _exptl_absorpt_correction_type none _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.437 _exptl_crystal_description plate _exptl_crystal_F_000 3180 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.697 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef 0.027(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1020 _refine_ls_number_reflns 13833 _refine_ls_number_restraints 278 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.2316 _refine_ls_R_factor_gt 0.1818 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3751 _refine_ls_wR_factor_ref 0.3908 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7916 _reflns_number_total 13833 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ob00593e2.cif _cod_data_source_block 232 _cod_database_code 7156869 _shelx_shelxl_version_number 2014/7 _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 0.995 _shelx_estimated_absorpt_t_max 0.998 _shelx_res_file ; 232.res created by SHELXL-2014/7 TITL in P2(1)/c CELL 0.8950 21.8930 16.1500 20.4330 90.000 95.293 90.000 ZERR 4.00 0.002 0.001 0.001 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 400 140 80 omit 0 OMIT 0 0 4 OMIT 3 2 1 OMIT 3 2 3 OMIT -1 5 1 omit 0 5 2 OMIT -3 3 2 OMIT -6 6 2 OMIT 2 2 4 OMIT 7 0 0 OMIT 3 3 0 OMIT -2 1 5 OMIT -5 0 6 OMIT 0 4 0 OMIT 3 3 2 OMIT 2 1 3 OMIT -1 1 3 OMIT 1 4 4 OMIT 2 3 2 ACTA 64.9 l.s. 6 bond fmap 2 plan 20 TEMP -173 SIZE 0.05 0.04 0.015 isor 0.03 C25 C34 C35 C36 C50 C67 C67A C65C C68A C69A C69B C70 C70B C71B ISOR 0.03 C50 C69C ISOR 0.02 C52 C54 C64 C66A C68 C69 C70A C70C ISOR 0.014 C56 C63 C66 C65A ISOR 0.01 C65 DFIX 1.55 0.02 C68D C69D C69D C70D WGHT 0.090000 20.000000 EXTI 0.026036 FVAR 7.29922 C1 1 0.690657 0.581847 0.647528 11.00000 0.17097 0.04287 = 0.09400 0.00467 0.03202 -0.00646 C2 1 0.705545 0.637996 0.590033 11.00000 0.13500 0.07654 = 0.06938 0.00741 0.04194 0.00666 C3 1 0.731030 0.707935 0.619421 11.00000 0.11407 0.07562 = 0.07765 0.00612 0.02270 -0.00421 C4 1 0.727207 0.707431 0.691399 11.00000 0.12370 0.09073 = 0.07949 0.01765 0.01266 -0.01464 C5 1 0.698909 0.634418 0.705567 11.00000 0.13901 0.07302 = 0.06098 0.01724 0.01781 0.02028 C6 1 0.666357 0.622663 0.767366 11.00000 0.12047 0.09663 = 0.07256 0.03395 0.01828 0.00662 C7 1 0.601865 0.589556 0.744116 11.00000 0.14270 0.06132 = 0.06790 0.02378 0.02657 0.01550 C8 1 0.588167 0.549098 0.686996 11.00000 0.11095 0.05153 = 0.09490 0.01556 0.01182 0.00445 C9 1 0.633342 0.526027 0.636523 11.00000 0.13957 0.04858 = 0.10341 0.00050 0.04503 0.00979 C10 1 0.594611 0.551674 0.571855 11.00000 0.13215 0.05590 = 0.09635 -0.03102 0.03342 -0.00432 C11 1 0.616502 0.597733 0.521303 11.00000 0.15926 0.06074 = 0.06766 -0.01627 0.02804 0.00056 C12 1 0.679999 0.630855 0.520461 11.00000 0.14268 0.07349 = 0.07044 -0.01476 0.03736 -0.00703 C13 1 0.667464 0.721098 0.496049 11.00000 0.13675 0.07183 = 0.06118 -0.00268 0.02571 0.00182 C14 1 0.694899 0.788994 0.523898 11.00000 0.15225 0.06982 = 0.05894 0.00605 0.03013 -0.00781 C15 1 0.742822 0.786609 0.583131 11.00000 0.13751 0.07807 = 0.06776 0.01300 0.02247 -0.01439 C16 1 0.718959 0.858746 0.624110 11.00000 0.16066 0.06744 = 0.08111 -0.00355 0.02568 -0.03012 C17 1 0.714559 0.858043 0.690422 11.00000 0.17217 0.08318 = 0.07814 -0.00303 0.00278 -0.03276 C18 1 0.732053 0.783867 0.733761 11.00000 0.14813 0.08994 = 0.07223 -0.00719 0.00770 -0.02460 C19 1 0.678377 0.783528 0.776555 11.00000 0.15194 0.11090 = 0.05251 0.00213 0.00278 -0.02909 C20 1 0.650194 0.711380 0.791931 11.00000 0.14853 0.08684 = 0.04692 0.00380 -0.00037 0.01336 C21 1 0.584728 0.713079 0.800082 11.00000 0.13528 0.09931 = 0.04597 0.00986 0.01967 0.01256 C22 1 0.555269 0.638429 0.770681 11.00000 0.12825 0.07762 = 0.06326 0.02556 0.03209 0.02092 C23 1 0.493906 0.641404 0.740567 11.00000 0.12590 0.06739 = 0.07293 0.01304 0.03697 0.01513 C24 1 0.480280 0.598915 0.681366 11.00000 0.12550 0.07232 = 0.08084 0.01225 0.01807 -0.00681 C25 1 0.528053 0.553808 0.655004 11.00000 0.16584 0.04156 = 0.09308 -0.00542 0.04664 -0.01301 C26 1 0.531850 0.556719 0.582239 11.00000 0.15683 0.05408 = 0.08823 -0.01237 0.01548 -0.01646 C27 1 0.490180 0.600974 0.544556 11.00000 0.13061 0.09310 = 0.07295 -0.02536 0.01670 -0.01056 C28 1 0.512788 0.649769 0.490504 11.00000 0.16891 0.08732 = 0.06441 -0.01734 -0.01142 0.00820 C29 1 0.574575 0.648498 0.481999 11.00000 0.13469 0.10555 = 0.06271 -0.03413 0.02287 -0.00729 C30 1 0.607344 0.724167 0.467060 11.00000 0.16206 0.08404 = 0.04740 -0.00297 0.02425 -0.00045 C31 1 0.574519 0.799626 0.461198 11.00000 0.17560 0.11858 = 0.04487 0.02065 0.01272 0.00358 C32 1 0.603876 0.872314 0.491233 11.00000 0.18240 0.07451 = 0.07414 0.03010 0.02826 0.01454 C33 1 0.662166 0.865878 0.523072 11.00000 0.17455 0.05778 = 0.07778 0.02160 0.03075 -0.00067 C34 1 0.676267 0.908404 0.583931 11.00000 0.18678 0.05887 = 0.08024 0.00528 0.02846 -0.02407 C35 1 0.631542 0.957195 0.610158 11.00000 0.21880 0.03752 = 0.11329 -0.00001 0.04380 -0.00550 C36 1 0.627623 0.955201 0.678900 11.00000 0.22732 0.05243 = 0.09523 -0.01555 0.01877 -0.00289 C37 1 0.668223 0.905472 0.718152 11.00000 0.18504 0.07813 = 0.07569 -0.02496 0.02241 -0.02300 C38 1 0.645912 0.858630 0.770029 11.00000 0.18414 0.06865 = 0.07194 -0.02148 0.00405 -0.00924 C39 1 0.582776 0.862191 0.781274 11.00000 0.16963 0.10238 = 0.06828 -0.04085 0.02297 -0.00126 C40 1 0.552727 0.786372 0.797707 11.00000 0.16838 0.09072 = 0.05252 -0.01203 0.02725 0.02424 C41 1 0.490946 0.789913 0.765877 11.00000 0.13338 0.09087 = 0.07834 -0.00685 0.03496 0.03562 C42 1 0.462168 0.719575 0.737441 11.00000 0.12749 0.09058 = 0.06731 0.00698 0.03103 0.02919 C43 1 0.426067 0.724228 0.674215 11.00000 0.12382 0.10118 = 0.08193 0.01422 0.02484 0.02307 C44 1 0.437311 0.649660 0.639564 11.00000 0.11984 0.09620 = 0.09618 -0.01002 0.02217 0.00235 C45 1 0.442338 0.650396 0.570183 11.00000 0.12900 0.09906 = 0.08741 -0.00016 0.00055 -0.00221 C46 1 0.436154 0.727788 0.537489 11.00000 0.13081 0.11338 = 0.07881 -0.00360 -0.00214 0.03012 C47 1 0.478849 0.724848 0.487490 11.00000 0.14299 0.12683 = 0.06067 0.00743 0.00040 -0.00292 C48 1 0.507879 0.800066 0.472115 11.00000 0.17528 0.11770 = 0.05553 0.01987 -0.00558 0.04216 C49 1 0.497310 0.875531 0.508037 11.00000 0.16873 0.08829 = 0.08951 0.04346 0.00596 0.02826 C50 1 0.554347 0.919747 0.519740 11.00000 0.22221 0.06228 = 0.08505 0.03313 0.02229 0.03219 C51 1 0.570840 0.961642 0.577114 11.00000 0.20448 0.04584 = 0.11891 0.02807 0.03624 0.02499 C52 1 0.524044 0.961061 0.626166 11.00000 0.21637 0.05530 = 0.09683 0.00496 0.01598 0.04683 C53 1 0.562917 0.959117 0.688399 11.00000 0.22721 0.04692 = 0.16095 -0.03103 0.07446 0.01567 C54 1 0.539390 0.910632 0.740873 11.00000 0.21241 0.06841 = 0.09128 -0.02013 0.02519 0.04616 C55 1 0.482624 0.867985 0.728968 11.00000 0.14924 0.07599 = 0.10909 -0.01988 0.04322 0.02414 C56 1 0.449173 0.872233 0.668625 11.00000 0.15531 0.09269 = 0.08120 0.00427 0.01982 0.05520 C57 1 0.420665 0.800160 0.641412 11.00000 0.14386 0.10435 = 0.09256 0.00618 0.01664 0.05061 C58 1 0.426464 0.801603 0.569976 11.00000 0.12876 0.12400 = 0.09895 0.04349 0.00749 0.03980 C59 1 0.457429 0.876531 0.556695 11.00000 0.15706 0.09806 = 0.09327 0.02167 0.01217 0.05808 C60 1 0.470398 0.919836 0.615958 11.00000 0.15168 0.07082 = 0.13868 0.00993 0.02628 0.03790 C61 1 0.759652 0.525600 0.653784 11.00000 0.18851 0.10577 = 0.16114 -0.02092 0.00933 0.02857 AFIX 137 H61A 2 0.756749 0.479489 0.684520 11.00000 -1.50000 H61B 2 0.793556 0.562045 0.669869 11.00000 -1.50000 H61C 2 0.767131 0.503896 0.610450 11.00000 -1.50000 AFIX 0 C62 1 0.646126 0.433881 0.637681 11.00000 0.11048 0.04768 = 0.15450 0.00169 0.04268 0.00324 C63 1 0.655611 0.395657 0.699956 11.00000 0.17785 0.08172 = 0.14006 0.02855 0.06617 0.02701 AFIX 43 H63 2 0.653704 0.427655 0.738727 11.00000 -1.20000 AFIX 0 C64 1 0.668114 0.308615 0.704724 11.00000 0.19915 0.08586 = 0.19107 0.03247 0.08915 0.01230 AFIX 43 H64 2 0.676738 0.282585 0.746243 11.00000 -1.20000 AFIX 0 C65 1 0.655277 0.390832 0.582526 11.00000 0.15014 0.08849 = 0.13877 -0.04130 -0.03066 0.03626 AFIX 43 H65 2 0.654628 0.418628 0.541492 11.00000 -1.20000 AFIX 0 C66 1 0.666274 0.300576 0.586242 11.00000 0.15648 0.11358 = 0.15300 -0.04980 -0.04082 0.03632 AFIX 43 H66 2 0.672351 0.268714 0.548303 11.00000 -1.20000 AFIX 0 C67 1 0.667252 0.264742 0.648318 11.00000 0.18748 0.06279 = 0.23547 -0.02882 0.06265 -0.03292 C68 1 0.680798 0.166103 0.652530 11.00000 0.20181 0.08413 = 0.38167 -0.00626 0.01947 -0.00800 AFIX 23 H68A 2 0.662747 0.143563 0.691479 11.00000 -1.20000 H68B 2 0.659783 0.139183 0.613142 11.00000 -1.20000 AFIX 0 C69 1 0.746522 0.143741 0.656970 11.00000 0.33068 0.23312 = 0.28736 -0.03441 -0.10517 0.01535 AFIX 23 H69A 2 0.760675 0.145980 0.612364 11.00000 -1.20000 H69B 2 0.751142 0.085909 0.672718 11.00000 -1.20000 AFIX 0 C70 1 0.788181 0.199799 0.702782 11.00000 0.31460 0.28191 = 0.33796 0.07846 0.02021 0.02841 C71 1 0.851716 0.305622 0.743936 11.00000 0.38492 AFIX 137 H71A 2 0.893407 0.320762 0.734690 11.00000 -1.50000 H71B 2 0.853648 0.267632 0.781468 11.00000 -1.50000 H71C 2 0.829135 0.355623 0.754278 11.00000 -1.50000 AFIX 0 O1 3 0.776802 0.196979 0.766544 11.00000 10.50000 O2 3 0.815458 0.258841 0.677371 11.00000 0.48849 C62A 1 0.717350 0.583170 0.473790 11.00000 0.15281 0.07616 = 0.09851 -0.01473 0.05491 0.00325 C63A 1 0.693535 0.527577 0.430055 11.00000 0.21120 0.11586 = 0.12813 -0.05206 0.05235 0.01448 AFIX 43 H63A 2 0.650791 0.516380 0.427764 11.00000 -1.20000 AFIX 0 C64A 1 0.729117 0.485581 0.387818 11.00000 0.24748 0.15668 = 0.16047 -0.07344 0.05982 0.03590 AFIX 43 H64A 2 0.710479 0.444369 0.359421 11.00000 -1.20000 AFIX 0 C65A 1 0.778291 0.600212 0.471730 11.00000 0.22006 0.15673 = 0.20398 -0.06136 0.11213 -0.01318 AFIX 43 H65A 2 0.796665 0.641245 0.500482 11.00000 -1.20000 AFIX 0 C66A 1 0.814700 0.559591 0.428926 11.00000 0.23812 0.18648 = 0.23957 -0.07155 0.15166 -0.03251 AFIX 43 H66A 2 0.857118 0.572415 0.429817 11.00000 -1.20000 AFIX 0 C67A 1 0.789646 0.501920 0.386125 11.00000 0.28350 0.15240 = 0.15943 -0.04985 0.11186 0.00249 C68A 1 0.840890 0.440357 0.351004 11.00000 0.38316 0.33332 = 0.19454 -0.06511 0.18792 -0.05846 AFIX 23 H68C 2 0.879718 0.436047 0.379739 11.00000 -1.20000 H68D 2 0.823918 0.384069 0.342976 11.00000 -1.20000 AFIX 0 C69A 1 0.850387 0.478001 0.293522 11.00000 10.40000 AFIX 23 H69C 2 0.864628 0.535167 0.303596 11.00000 -1.20000 H69D 2 0.810385 0.482189 0.266872 11.00000 -1.20000 AFIX 0 C70A 1 0.900017 0.433762 0.247408 11.00000 0.30733 0.29198 = 0.26765 -0.09443 0.11873 -0.05505 C71A 1 0.897489 0.437287 0.131563 11.00000 0.34596 0.53973 = 0.12828 -0.03389 0.01565 0.00163 AFIX 137 H71D 2 0.920361 0.489520 0.134541 11.00000 -1.50000 H71E 2 0.872643 0.434488 0.089198 11.00000 -1.50000 H71F 2 0.926335 0.390756 0.135226 11.00000 -1.50000 AFIX 0 O1A 3 0.918528 0.358638 0.279741 11.00000 0.39167 O2A 3 0.854933 0.432690 0.188140 11.00000 10.40000 C62B 1 0.809006 0.799682 0.568039 11.00000 0.14252 0.09027 = 0.09597 0.00575 0.02690 -0.02252 C63B 1 0.825260 0.866481 0.531177 11.00000 0.20277 0.11365 = 0.12867 0.02735 0.05559 -0.02069 AFIX 43 H63B 2 0.795108 0.903506 0.511754 11.00000 -1.20000 AFIX 0 C64B 1 0.889524 0.878312 0.523069 11.00000 0.19276 0.12814 = 0.18387 0.02247 0.09066 -0.04941 AFIX 43 H64B 2 0.900919 0.925020 0.498682 11.00000 -1.20000 AFIX 0 C65B 1 0.856648 0.751275 0.594501 11.00000 0.17318 0.10977 = 0.17544 0.04024 0.04836 -0.01264 AFIX 43 H65B 2 0.847443 0.705174 0.620748 11.00000 -1.20000 AFIX 0 C66B 1 0.918604 0.766652 0.584618 11.00000 0.13323 0.16034 = 0.17401 0.03854 0.03364 -0.03276 AFIX 43 H66B 2 0.950046 0.732231 0.604937 11.00000 -1.20000 AFIX 0 C67B 1 0.932660 0.828784 0.547190 11.00000 0.13527 0.13979 = 0.16935 0.00943 0.03795 -0.01752 C68B 1 1.001492 0.850256 0.535548 11.00000 0.15693 0.33077 = 0.20978 -0.03466 0.06803 -0.04326 AFIX 23 H68E 2 1.018669 0.806117 0.509059 11.00000 -1.20000 H68F 2 1.002923 0.903051 0.511115 11.00000 -1.20000 AFIX 0 C69B 1 1.039738 0.857820 0.602281 11.00000 0.35609 0.43513 = 0.40603 -0.06066 0.12460 -0.01135 AFIX 23 H69E 2 1.083531 0.848568 0.596069 11.00000 -1.20000 H69F 2 1.026827 0.814328 0.632247 11.00000 -1.20000 AFIX 0 C70B 1 1.032470 0.942751 0.633815 11.00000 0.18427 0.39986 = 0.31834 -0.10167 -0.06268 0.04931 C71B 1 1.057058 1.047779 0.710169 11.00000 0.21161 0.20415 = 0.53100 0.05921 0.07999 -0.04087 AFIX 137 H71G 2 1.039807 1.077625 0.670979 11.00000 -1.50000 H71H 2 1.099005 1.067062 0.722389 11.00000 -1.50000 H71I 2 1.031817 1.058143 0.746507 11.00000 -1.50000 AFIX 0 O1B 3 1.020793 1.008535 0.595369 11.00000 10.40000 O2B 3 1.057961 0.949241 0.694652 11.00000 10.40000 C62C 1 0.797111 0.788250 0.772987 11.00000 0.15221 0.10696 = 0.11046 -0.01713 0.00108 -0.03119 C63C 1 0.846730 0.822888 0.746476 11.00000 0.18792 0.23588 = 0.09171 -0.01176 0.00899 -0.07346 AFIX 43 H63C 2 0.841148 0.848415 0.704462 11.00000 -1.20000 AFIX 0 C64C 1 0.907528 0.821067 0.781684 11.00000 0.17267 0.22552 = 0.17495 -0.00906 -0.02125 -0.06970 AFIX 43 H64C 2 0.941406 0.847140 0.764282 11.00000 -1.20000 AFIX 0 C65C 1 0.808112 0.750848 0.835982 11.00000 0.17624 0.15512 = 0.10821 0.00311 0.00130 -0.00524 AFIX 43 H65C 2 0.774934 0.726487 0.855896 11.00000 -1.20000 AFIX 0 C66C 1 0.866573 0.749310 0.868935 11.00000 0.16818 0.17506 = 0.12669 0.00181 -0.03133 -0.04284 AFIX 43 H66C 2 0.871775 0.725934 0.911751 11.00000 -1.20000 AFIX 0 C67C 1 0.914643 0.778721 0.843384 11.00000 0.17021 0.15306 = 0.17769 -0.00600 -0.04829 -0.01896 C68C 1 0.979559 0.768764 0.880185 11.00000 0.17362 0.31658 = 0.24069 0.04812 -0.01492 -0.04387 AFIX 23 H68G 2 0.974551 0.767087 0.927828 11.00000 -1.20000 H68H 2 0.995436 0.713943 0.868223 11.00000 -1.20000 AFIX 0 C69C 1 1.024126 0.826118 0.870894 11.00000 10.40000 AFIX 23 H69G 2 1.033213 0.820097 0.824560 11.00000 -1.20000 H69H 2 1.061310 0.807370 0.898111 11.00000 -1.20000 AFIX 0 C70C 1 1.019533 0.916106 0.882625 11.00000 0.26957 0.22260 = 0.30047 -0.02188 -0.06873 0.07729 C71C 1 1.044529 1.051608 0.903193 11.00000 0.38089 AFIX 137 H71J 2 1.025341 1.039589 0.943616 11.00000 -1.50000 H71K 2 1.014751 1.079117 0.871644 11.00000 -1.50000 H71L 2 1.079986 1.087956 0.913326 11.00000 -1.50000 AFIX 0 O1C 3 0.986289 0.947050 0.930842 11.00000 10.40000 O2C 3 1.067589 0.963116 0.870743 11.00000 0.45291 C62D 1 0.699188 0.569287 0.821080 11.00000 0.10657 0.09944 = 0.07795 0.01933 0.01535 0.01063 C63D 1 0.761916 0.559152 0.824369 11.00000 0.15677 0.11576 = 0.09935 0.03541 -0.00317 -0.01250 AFIX 43 H63D 2 0.784774 0.589363 0.795057 11.00000 -1.20000 AFIX 0 C64D 1 0.792726 0.505311 0.869958 11.00000 0.14742 0.13823 = 0.13587 0.04690 0.00423 0.01665 AFIX 43 H64D 2 0.835615 0.496382 0.869948 11.00000 -1.20000 AFIX 0 C65D 1 0.670710 0.530636 0.866409 11.00000 0.12808 0.06580 = 0.06406 0.01281 0.01741 0.01159 AFIX 43 H65D 2 0.627858 0.539659 0.866720 11.00000 -1.20000 AFIX 0 C66D 1 0.698925 0.477398 0.914006 11.00000 0.12338 0.07551 = 0.08042 0.01932 0.02107 0.01468 AFIX 43 H66D 2 0.675462 0.450663 0.944679 11.00000 -1.20000 AFIX 0 SAME 0.03 0.03 C67 > O2 SAME 0.03 0.03 C67A > O2A SAME 0.03 0.03 C67B > O2B SAME 0.03 0.03 C67C > O2C C67D 1 0.758995 0.464751 0.915710 11.00000 0.15046 0.12052 = 0.10401 0.04196 0.01471 0.01261 C68D 1 0.794106 0.403973 0.965292 11.00000 0.17413 0.16075 = 0.12256 0.04348 0.01774 0.02702 AFIX 23 H68I 2 0.838633 0.415779 0.967780 11.00000 -1.20000 H68J 2 0.780225 0.412102 1.009602 11.00000 -1.20000 AFIX 0 C69D 1 0.782507 0.315730 0.943684 11.00000 0.28339 0.09171 = 0.15257 0.04866 0.03191 0.03915 AFIX 23 H69I 2 0.790674 0.309313 0.897101 11.00000 -1.20000 H69J 2 0.739115 0.300994 0.947687 11.00000 -1.20000 AFIX 0 C70D 1 0.825812 0.257093 0.988132 11.00000 0.36390 0.09536 = 0.27904 0.08601 0.08495 -0.03760 C71D 1 0.830506 0.129085 1.039826 11.00000 0.38129 0.21015 = 0.32295 0.18612 -0.02843 0.01308 AFIX 137 H71M 2 0.874173 0.139416 1.036189 11.00000 -1.50000 H71N 2 0.820537 0.071975 1.026607 11.00000 -1.50000 H71O 2 0.821424 0.137521 1.085426 11.00000 -1.50000 AFIX 0 O1D 3 0.877984 0.269270 1.014891 11.00000 0.32346 O2D 3 0.791069 0.190515 0.993778 11.00000 0.24083 HKLF 4 1 0 0 1 0 -1 0 1 0 0 REM in P2(1)/c REM R1 = 0.1818 for 7916 Fo > 4sig(Fo) and 0.2316 for all 13833 data REM 1020 parameters refined using 278 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.697, deepest hole -0.432, 1-sigma level 0.076 Q1 1 0.8411 0.2391 0.7881 11.00000 0.05 0.70 Q2 1 0.6066 0.3704 0.6346 11.00000 0.05 0.65 Q3 1 0.6158 0.2924 0.6319 11.00000 0.05 0.55 Q4 1 1.0008 0.8306 0.9309 11.00000 0.05 0.52 Q5 1 0.6746 0.5148 0.7938 11.00000 0.05 0.52 Q6 1 0.8634 0.2734 1.0274 11.00000 0.05 0.51 Q7 1 0.8489 0.3715 0.3632 11.00000 0.05 0.49 Q8 1 0.8154 0.4146 0.1704 11.00000 0.05 0.48 Q9 1 0.9376 0.3376 0.3022 11.00000 0.05 0.47 Q10 1 0.7914 0.4667 0.3035 11.00000 0.05 0.46 Q11 1 1.0189 0.8947 0.6770 11.00000 0.05 0.44 Q12 1 0.6980 0.4505 0.7707 11.00000 0.05 0.44 Q13 1 1.0193 0.9402 0.5630 11.00000 0.05 0.43 Q14 1 0.7182 0.3812 0.8137 11.00000 0.05 0.43 Q15 1 0.7908 0.1123 0.6550 11.00000 0.05 0.42 Q16 1 0.7212 0.1281 0.6998 11.00000 0.05 0.42 Q17 1 0.8765 0.3204 0.3118 11.00000 0.05 0.42 Q18 1 0.7174 0.3943 0.8809 11.00000 0.05 0.41 Q19 1 0.6834 0.1732 0.5851 11.00000 0.05 0.40 Q20 1 0.8000 0.6118 0.7021 11.00000 0.05 0.40 ; _shelx_res_checksum 47460 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 C1 C 0.6907(4) 0.5818(3) 0.6475(3) 0.101(2) Uani 1 1 d . . C2 C 0.7055(3) 0.6380(4) 0.5900(3) 0.092(2) Uani 1 1 d . . C3 C 0.7310(3) 0.7079(4) 0.6194(3) 0.0883(18) Uani 1 1 d . . C4 C 0.7272(3) 0.7074(4) 0.6914(3) 0.098(2) Uani 1 1 d . . C5 C 0.6989(3) 0.6344(4) 0.7056(3) 0.0905(19) Uani 1 1 d . . C6 C 0.6664(4) 0.6227(4) 0.7674(3) 0.096(2) Uani 1 1 d . . C7 C 0.6019(4) 0.5896(4) 0.7441(3) 0.090(2) Uani 1 1 d . . C8 C 0.5882(3) 0.5491(3) 0.6870(4) 0.0857(18) Uani 1 1 d . . C9 C 0.6333(4) 0.5260(3) 0.6365(4) 0.095(2) Uani 1 1 d . . C10 C 0.5946(4) 0.5517(4) 0.5719(4) 0.093(2) Uani 1 1 d . . C11 C 0.6165(4) 0.5977(4) 0.5213(3) 0.095(2) Uani 1 1 d . . C12 C 0.6800(4) 0.6309(4) 0.5205(3) 0.094(2) Uani 1 1 d . . C13 C 0.6675(4) 0.7211(4) 0.4960(3) 0.0889(19) Uani 1 1 d . . C14 C 0.6949(4) 0.7890(4) 0.5239(3) 0.092(2) Uani 1 1 d . . C15 C 0.7428(4) 0.7866(4) 0.5831(3) 0.094(2) Uani 1 1 d . . C16 C 0.7190(4) 0.8587(4) 0.6241(4) 0.102(2) Uani 1 1 d . . C17 C 0.7146(4) 0.8580(4) 0.6904(4) 0.112(2) Uani 1 1 d . . C18 C 0.7321(4) 0.7839(4) 0.7338(4) 0.104(2) Uani 1 1 d . . C19 C 0.6784(4) 0.7835(5) 0.7766(3) 0.106(2) Uani 1 1 d . . C20 C 0.6502(4) 0.7114(4) 0.7919(3) 0.095(2) Uani 1 1 d . . C21 C 0.5847(4) 0.7131(4) 0.8001(3) 0.093(2) Uani 1 1 d . . C22 C 0.5553(4) 0.6384(4) 0.7707(3) 0.0883(19) Uani 1 1 d . . C23 C 0.4939(4) 0.6414(4) 0.7406(3) 0.0870(19) Uani 1 1 d . . C24 C 0.4803(3) 0.5989(4) 0.6814(3) 0.0924(19) Uani 1 1 d . . C25 C 0.5281(4) 0.5538(3) 0.6550(4) 0.098(2) Uani 1 1 d . U C26 C 0.5319(4) 0.5567(4) 0.5822(4) 0.099(2) Uani 1 1 d . . C27 C 0.4902(4) 0.6010(5) 0.5446(4) 0.098(2) Uani 1 1 d . . C28 C 0.5128(5) 0.6498(5) 0.4905(4) 0.108(2) Uani 1 1 d . . C29 C 0.5746(4) 0.6485(5) 0.4820(3) 0.100(2) Uani 1 1 d . . C30 C 0.6073(4) 0.7242(4) 0.4671(3) 0.097(2) Uani 1 1 d . . C31 C 0.5745(5) 0.7996(5) 0.4612(3) 0.113(3) Uani 1 1 d . . C32 C 0.6039(5) 0.8723(4) 0.4912(4) 0.109(3) Uani 1 1 d . . C33 C 0.6622(4) 0.8659(4) 0.5231(4) 0.102(2) Uani 1 1 d . . C34 C 0.6763(4) 0.9084(4) 0.5839(4) 0.108(2) Uani 1 1 d . U C35 C 0.6315(6) 0.9572(4) 0.6102(5) 0.121(3) Uani 1 1 d . U C36 C 0.6276(6) 0.9552(4) 0.6789(4) 0.125(3) Uani 1 1 d . U C37 C 0.6682(5) 0.9055(5) 0.7182(4) 0.112(3) Uani 1 1 d . . C38 C 0.6459(5) 0.8586(4) 0.7700(4) 0.109(3) Uani 1 1 d . . C39 C 0.5828(5) 0.8622(5) 0.7813(4) 0.113(3) Uani 1 1 d . . C40 C 0.5527(4) 0.7864(5) 0.7977(3) 0.103(2) Uani 1 1 d . . C41 C 0.4909(4) 0.7899(4) 0.7659(4) 0.099(2) Uani 1 1 d . . C42 C 0.4622(4) 0.7196(4) 0.7374(3) 0.094(2) Uani 1 1 d . . C43 C 0.4261(4) 0.7242(5) 0.6742(4) 0.101(2) Uani 1 1 d . . C44 C 0.4373(4) 0.6497(5) 0.6396(4) 0.103(2) Uani 1 1 d . . C45 C 0.4423(4) 0.6504(5) 0.5702(4) 0.106(2) Uani 1 1 d . . C46 C 0.4362(4) 0.7278(5) 0.5375(4) 0.108(2) Uani 1 1 d . . C47 C 0.4788(4) 0.7248(6) 0.4875(4) 0.111(2) Uani 1 1 d . . C48 C 0.5079(5) 0.8001(6) 0.4721(4) 0.117(3) Uani 1 1 d . . C49 C 0.4973(5) 0.8755(5) 0.5080(4) 0.116(3) Uani 1 1 d . . C50 C 0.5543(6) 0.9197(5) 0.5197(4) 0.123(3) Uani 1 1 d . U C51 C 0.5708(6) 0.9616(4) 0.5771(5) 0.122(3) Uani 1 1 d . . C52 C 0.5240(6) 0.9611(4) 0.6262(5) 0.123(3) Uani 1 1 d . U C53 C 0.5629(6) 0.9591(4) 0.6884(6) 0.142(4) Uani 1 1 d . . C54 C 0.5394(6) 0.9106(5) 0.7409(4) 0.123(3) Uani 1 1 d . U C55 C 0.4826(5) 0.8680(5) 0.7290(4) 0.109(3) Uani 1 1 d . . C56 C 0.4492(4) 0.8722(5) 0.6686(4) 0.109(2) Uani 1 1 d . U C57 C 0.4207(4) 0.8002(5) 0.6414(4) 0.113(3) Uani 1 1 d . . C58 C 0.4265(4) 0.8016(6) 0.5700(4) 0.117(3) Uani 1 1 d . . C59 C 0.4574(4) 0.8765(5) 0.5567(4) 0.116(3) Uani 1 1 d . . C60 C 0.4704(5) 0.9198(5) 0.6160(5) 0.120(3) Uani 1 1 d . . C61 C 0.7597(5) 0.5256(6) 0.6538(5) 0.152(4) Uani 1 1 d . . H61A H 0.7567 0.4795 0.6845 0.228 Uiso 1 1 calc R U H61B H 0.7936 0.5620 0.6699 0.228 Uiso 1 1 calc R U H61C H 0.7671 0.5039 0.6105 0.228 Uiso 1 1 calc R U C62 C 0.6461(3) 0.4339(3) 0.6377(4) 0.102(2) Uani 1 1 d . . C63 C 0.6556(4) 0.3957(5) 0.7000(5) 0.130(3) Uani 1 1 d . U H63 H 0.6537 0.4277 0.7387 0.156 Uiso 1 1 calc R U C64 C 0.6681(5) 0.3086(6) 0.7047(6) 0.154(4) Uani 1 1 d . U H64 H 0.6767 0.2826 0.7462 0.185 Uiso 1 1 calc R U C65 C 0.6553(4) 0.3908(5) 0.5825(5) 0.129(3) Uani 1 1 d . U H65 H 0.6546 0.4186 0.5415 0.154 Uiso 1 1 calc R U C66 C 0.6663(5) 0.3006(6) 0.5862(6) 0.144(4) Uani 1 1 d . U H66 H 0.6724 0.2687 0.5483 0.173 Uiso 1 1 calc R U C67 C 0.6673(5) 0.2647(5) 0.6483(8) 0.159(4) Uani 1 1 d D U C68 C 0.6808(6) 0.1661(6) 0.6525(9) 0.223(6) Uani 1 1 d D U H68A H 0.6627 0.1436 0.6915 0.268 Uiso 1 1 calc R U H68B H 0.6598 0.1392 0.6131 0.268 Uiso 1 1 calc R U C69 C 0.7465(9) 0.1437(10) 0.6570(9) 0.292(10) Uani 1 1 d D U H69A H 0.7607 0.1460 0.6124 0.350 Uiso 1 1 calc R U H69B H 0.7511 0.0859 0.6727 0.350 Uiso 1 1 calc R U C70 C 0.7882(9) 0.1998(13) 0.7028(11) 0.312(11) Uani 1 1 d D U C71 C 0.8517(11) 0.3056(16) 0.7439(13) 0.385(14) Uiso 1 1 d D . H71A H 0.8934 0.3208 0.7347 0.577 Uiso 1 1 calc R U H71B H 0.8536 0.2676 0.7815 0.577 Uiso 1 1 calc R U H71C H 0.8291 0.3556 0.7543 0.577 Uiso 1 1 calc R U O1 O 0.7768(13) 0.1970(18) 0.7665(11) 0.500 Uiso 1 1 d D U O2 O 0.8155(12) 0.2588(16) 0.6774(12) 0.488(16) Uiso 1 1 d D . C62A C 0.7174(4) 0.5832(4) 0.4738(4) 0.106(2) Uani 1 1 d . . C63A C 0.6935(5) 0.5276(6) 0.4301(5) 0.149(4) Uani 1 1 d . . H63A H 0.6508 0.5164 0.4278 0.179 Uiso 1 1 calc R U C64A C 0.7291(7) 0.4856(8) 0.3878(6) 0.186(5) Uani 1 1 d . . H64A H 0.7105 0.4444 0.3594 0.223 Uiso 1 1 calc R U C65A C 0.7783(6) 0.6002(7) 0.4717(6) 0.188(5) Uani 1 1 d . U H65A H 0.7967 0.6412 0.5005 0.225 Uiso 1 1 calc R U C66A C 0.8147(7) 0.5596(8) 0.4289(7) 0.213(6) Uani 1 1 d . U H66A H 0.8571 0.5724 0.4298 0.256 Uiso 1 1 calc R U C67A C 0.7896(8) 0.5019(8) 0.3861(7) 0.193(6) Uani 1 1 d D U C68A C 0.8409(9) 0.4404(11) 0.3510(7) 0.294(10) Uani 1 1 d D U H68C H 0.8797 0.4360 0.3797 0.352 Uiso 1 1 calc R U H68D H 0.8239 0.3841 0.3430 0.352 Uiso 1 1 calc R U C69A C 0.8504(12) 0.4780(15) 0.2935(10) 0.400 Uiso 1 1 d D U H69C H 0.8646 0.5352 0.3036 0.480 Uiso 1 1 calc R U H69D H 0.8104 0.4822 0.2669 0.480 Uiso 1 1 calc R U C70A C 0.9000(9) 0.4338(13) 0.2474(8) 0.283(9) Uani 1 1 d D U C71A C 0.8975(10) 0.4373(17) 0.1316(7) 0.338(13) Uani 1 1 d D . H71D H 0.9204 0.4895 0.1345 0.508 Uiso 1 1 calc R U H71E H 0.8726 0.4345 0.0892 0.508 Uiso 1 1 calc R U H71F H 0.9263 0.3908 0.1352 0.508 Uiso 1 1 calc R U O1A O 0.9185(9) 0.3586(13) 0.2797(9) 0.392(10) Uiso 1 1 d D . O2A O 0.8549(9) 0.4327(13) 0.1881(10) 0.400 Uiso 1 1 d D U C62B C 0.8090(4) 0.7997(5) 0.5680(4) 0.109(2) Uani 1 1 d . . C63B C 0.8253(5) 0.8665(6) 0.5312(5) 0.146(4) Uani 1 1 d . . H63B H 0.7951 0.9035 0.5118 0.175 Uiso 1 1 calc R U C64B C 0.8895(6) 0.8783(7) 0.5231(6) 0.164(5) Uani 1 1 d . . H64B H 0.9009 0.9250 0.4987 0.196 Uiso 1 1 calc R U C65B C 0.8566(6) 0.7513(6) 0.5945(6) 0.151(4) Uani 1 1 d . . H65B H 0.8474 0.7052 0.6207 0.181 Uiso 1 1 calc R U C66B C 0.9186(5) 0.7667(7) 0.5846(6) 0.155(4) Uani 1 1 d . . H66B H 0.9500 0.7322 0.6049 0.186 Uiso 1 1 calc R U C67B C 0.9327(5) 0.8288(8) 0.5472(6) 0.147(4) Uani 1 1 d D . C68B C 1.0015(6) 0.8503(11) 0.5355(7) 0.229(7) Uani 1 1 d D . H68E H 1.0187 0.8061 0.5091 0.275 Uiso 1 1 calc R U H68F H 1.0029 0.9031 0.5111 0.275 Uiso 1 1 calc R U C69B C 1.0397(10) 0.8578(13) 0.6023(11) 0.394(16) Uani 1 1 d D U H69E H 1.0835 0.8486 0.5961 0.472 Uiso 1 1 calc R U H69F H 1.0268 0.8143 0.6322 0.472 Uiso 1 1 calc R U C70B C 1.0325(8) 0.9428(13) 0.6338(10) 0.306(11) Uani 1 1 d D U C71B C 1.0571(8) 1.0478(10) 0.7102(11) 0.313(11) Uani 1 1 d D U H71G H 1.0398 1.0776 0.6710 0.469 Uiso 1 1 calc R U H71H H 1.0990 1.0671 0.7224 0.469 Uiso 1 1 calc R U H71I H 1.0318 1.0581 0.7465 0.469 Uiso 1 1 calc R U O1B O 1.0208(10) 1.0085(12) 0.5954(10) 0.400 Uiso 1 1 d D U O2B O 1.0580(10) 0.9492(13) 0.6947(9) 0.400 Uiso 1 1 d D U C62C C 0.7971(5) 0.7883(5) 0.7730(5) 0.124(3) Uani 1 1 d . . C63C C 0.8467(6) 0.8229(8) 0.7465(5) 0.172(5) Uani 1 1 d . . H63C H 0.8411 0.8484 0.7045 0.206 Uiso 1 1 calc R U C64C C 0.9075(6) 0.8211(10) 0.7817(8) 0.193(5) Uani 1 1 d . . H64C H 0.9414 0.8471 0.7643 0.232 Uiso 1 1 calc R U C65C C 0.8081(6) 0.7508(6) 0.8360(6) 0.147(3) Uani 1 1 d . U H65C H 0.7749 0.7265 0.8559 0.177 Uiso 1 1 calc R U C66C C 0.8666(7) 0.7493(7) 0.8689(6) 0.159(4) Uani 1 1 d . . H66C H 0.8718 0.7259 0.9118 0.191 Uiso 1 1 calc R U C67C C 0.9146(7) 0.7787(8) 0.8434(9) 0.171(5) Uani 1 1 d D . C68C C 0.9796(6) 0.7688(10) 0.8802(9) 0.246(8) Uani 1 1 d D . H68G H 0.9746 0.7671 0.9278 0.295 Uiso 1 1 calc R U H68H H 0.9954 0.7139 0.8682 0.295 Uiso 1 1 calc R U C69C C 1.0241(10) 0.8261(13) 0.8709(14) 0.400 Uiso 1 1 d D U H69G H 1.0332 0.8201 0.8246 0.480 Uiso 1 1 calc R U H69H H 1.0613 0.8074 0.8981 0.480 Uiso 1 1 calc R U C70C C 1.0195(9) 0.9161(10) 0.8826(10) 0.270(8) Uani 1 1 d D U C71C C 1.0445(12) 1.0516(13) 0.9032(13) 0.381(13) Uiso 1 1 d D . H71J H 1.0253 1.0396 0.9436 0.571 Uiso 1 1 calc R U H71K H 1.0148 1.0791 0.8716 0.571 Uiso 1 1 calc R U H71L H 1.0800 1.0880 0.9133 0.571 Uiso 1 1 calc R U O1C O 0.9863(9) 0.9471(13) 0.9308(10) 0.400 Uiso 1 1 d D U O2C O 1.0676(10) 0.9631(15) 0.8707(11) 0.453(14) Uiso 1 1 d D . C62D C 0.6992(4) 0.5693(4) 0.8211(3) 0.0942(19) Uani 1 1 d . . C63D C 0.7619(5) 0.5592(5) 0.8244(4) 0.125(3) Uani 1 1 d . . H63D H 0.7848 0.5894 0.7951 0.150 Uiso 1 1 calc R U C64D C 0.7927(5) 0.5053(6) 0.8700(5) 0.141(3) Uani 1 1 d . . H64D H 0.8356 0.4964 0.8699 0.169 Uiso 1 1 calc R U C65D C 0.6707(3) 0.5306(3) 0.8664(3) 0.0854(18) Uani 1 1 d . . H65D H 0.6279 0.5397 0.8667 0.103 Uiso 1 1 calc R U C66D C 0.6989(4) 0.4774(4) 0.9140(3) 0.0924(19) Uani 1 1 d . . H66D H 0.6755 0.4507 0.9447 0.111 Uiso 1 1 calc R U C67D C 0.7590(5) 0.4648(5) 0.9157(4) 0.125(3) Uani 1 1 d D . C68D C 0.7941(5) 0.4040(6) 0.9653(5) 0.152(4) Uani 1 1 d D . H68I H 0.8386 0.4158 0.9678 0.183 Uiso 1 1 calc R U H68J H 0.7802 0.4121 1.0096 0.183 Uiso 1 1 calc R U C69D C 0.7825(6) 0.3157(5) 0.9437(5) 0.175(5) Uani 1 1 d D . H69I H 0.7907 0.3093 0.8971 0.210 Uiso 1 1 calc R U H69J H 0.7391 0.3010 0.9477 0.210 Uiso 1 1 calc R U C70D C 0.8258(7) 0.2571(6) 0.9881(8) 0.243(8) Uani 1 1 d D . C71D C 0.8305(9) 0.1291(10) 1.0398(9) 0.309(11) Uani 1 1 d D . H71M H 0.8742 0.1394 1.0362 0.463 Uiso 1 1 calc R U H71N H 0.8205 0.0720 1.0266 0.463 Uiso 1 1 calc R U H71O H 0.8214 0.1375 1.0854 0.463 Uiso 1 1 calc R U O1D O 0.8780(7) 0.2693(10) 1.0149(9) 0.323(9) Uiso 1 1 d D . O2D O 0.7911(5) 0.1905(7) 0.9938(6) 0.241(4) Uiso 1 1 d 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 C1 0.171(7) 0.043(3) 0.094(5) 0.005(3) 0.032(5) -0.006(3) C2 0.135(6) 0.077(4) 0.069(5) 0.007(3) 0.042(4) 0.007(4) C3 0.114(5) 0.076(4) 0.078(5) 0.006(3) 0.023(4) -0.004(3) C4 0.124(6) 0.091(4) 0.079(5) 0.018(3) 0.013(4) -0.015(4) C5 0.139(6) 0.073(4) 0.061(4) 0.017(3) 0.018(4) 0.020(4) C6 0.120(5) 0.097(5) 0.073(5) 0.034(3) 0.018(4) 0.007(4) C7 0.143(6) 0.061(3) 0.068(4) 0.024(3) 0.027(4) 0.015(4) C8 0.111(5) 0.052(3) 0.095(5) 0.016(3) 0.012(4) 0.004(3) C9 0.140(6) 0.049(3) 0.103(5) 0.000(3) 0.045(4) 0.010(3) C10 0.132(6) 0.056(3) 0.096(5) -0.031(3) 0.033(4) -0.004(3) C11 0.159(7) 0.061(3) 0.068(4) -0.016(3) 0.028(4) 0.001(4) C12 0.143(6) 0.073(4) 0.070(5) -0.015(3) 0.037(4) -0.007(4) C13 0.137(6) 0.072(4) 0.061(4) -0.003(3) 0.026(4) 0.002(4) C14 0.152(6) 0.070(4) 0.059(4) 0.006(3) 0.030(4) -0.008(4) C15 0.138(6) 0.078(4) 0.068(5) 0.013(3) 0.022(4) -0.014(4) C16 0.161(7) 0.067(4) 0.081(5) -0.004(3) 0.026(4) -0.030(4) C17 0.172(8) 0.083(5) 0.078(5) -0.003(4) 0.003(5) -0.033(5) C18 0.148(7) 0.090(5) 0.072(5) -0.007(3) 0.008(4) -0.025(4) C19 0.152(7) 0.111(6) 0.053(4) 0.002(3) 0.003(4) -0.029(5) C20 0.149(7) 0.087(4) 0.047(4) 0.004(3) 0.000(4) 0.013(4) C21 0.135(6) 0.099(5) 0.046(4) 0.010(3) 0.020(3) 0.013(4) C22 0.128(6) 0.078(4) 0.063(4) 0.026(3) 0.032(4) 0.021(4) C23 0.126(5) 0.067(3) 0.073(4) 0.013(3) 0.037(4) 0.015(3) C24 0.126(5) 0.072(4) 0.081(5) 0.012(3) 0.018(4) -0.007(4) C25 0.166(7) 0.042(3) 0.093(5) -0.005(3) 0.047(5) -0.013(3) C26 0.157(7) 0.054(3) 0.088(5) -0.012(3) 0.015(5) -0.016(4) C27 0.131(6) 0.093(5) 0.073(5) -0.025(4) 0.017(4) -0.011(4) C28 0.169(8) 0.087(5) 0.064(5) -0.017(3) -0.011(5) 0.008(5) C29 0.135(6) 0.106(5) 0.063(5) -0.034(4) 0.023(4) -0.007(5) C30 0.162(7) 0.084(4) 0.047(4) -0.003(3) 0.024(4) 0.000(5) C31 0.176(8) 0.119(6) 0.045(4) 0.021(4) 0.013(4) 0.004(6) C32 0.182(8) 0.075(4) 0.074(5) 0.030(4) 0.028(5) 0.015(5) C33 0.175(8) 0.058(3) 0.078(5) 0.022(3) 0.031(5) -0.001(4) C34 0.187(8) 0.059(4) 0.080(5) 0.005(3) 0.028(5) -0.024(4) C35 0.219(10) 0.038(3) 0.113(7) 0.000(3) 0.044(7) -0.006(4) C36 0.227(10) 0.052(4) 0.095(6) -0.016(3) 0.019(6) -0.003(5) C37 0.185(8) 0.078(4) 0.076(5) -0.025(4) 0.022(5) -0.023(5) C38 0.184(9) 0.069(4) 0.072(5) -0.021(3) 0.004(5) -0.009(5) C39 0.170(8) 0.102(6) 0.068(5) -0.041(4) 0.023(5) -0.001(6) C40 0.168(8) 0.091(5) 0.053(4) -0.012(3) 0.027(4) 0.024(5) C41 0.133(6) 0.091(5) 0.078(5) -0.007(3) 0.035(4) 0.036(4) C42 0.127(5) 0.091(4) 0.067(5) 0.007(3) 0.031(4) 0.029(4) C43 0.124(6) 0.101(5) 0.082(5) 0.014(4) 0.025(4) 0.023(4) C44 0.120(6) 0.096(5) 0.096(6) -0.010(4) 0.022(4) 0.002(4) C45 0.129(6) 0.099(5) 0.087(6) 0.000(4) 0.001(4) -0.002(4) C46 0.131(6) 0.113(6) 0.079(5) -0.004(4) -0.002(4) 0.030(5) C47 0.143(7) 0.127(7) 0.061(5) 0.007(4) 0.000(4) -0.003(5) C48 0.175(9) 0.118(6) 0.056(5) 0.020(4) -0.006(5) 0.042(6) C49 0.169(8) 0.088(5) 0.090(6) 0.043(4) 0.006(5) 0.028(5) C50 0.222(10) 0.062(4) 0.085(6) 0.033(4) 0.022(6) 0.032(5) C51 0.204(10) 0.046(3) 0.119(8) 0.028(4) 0.036(7) 0.025(5) C52 0.216(10) 0.055(4) 0.097(6) 0.005(4) 0.016(7) 0.047(5) C53 0.227(11) 0.047(4) 0.161(10) -0.031(4) 0.074(9) 0.016(5) C54 0.212(9) 0.068(4) 0.091(6) -0.020(4) 0.025(6) 0.046(5) C55 0.149(7) 0.076(4) 0.109(7) -0.020(4) 0.043(5) 0.024(5) C56 0.155(6) 0.093(5) 0.081(5) 0.004(4) 0.020(5) 0.055(4) C57 0.144(7) 0.104(6) 0.093(6) 0.006(4) 0.017(5) 0.051(5) C58 0.129(6) 0.124(7) 0.099(6) 0.043(5) 0.007(5) 0.040(5) C59 0.157(7) 0.098(5) 0.093(6) 0.022(4) 0.012(5) 0.058(5) C60 0.152(8) 0.071(5) 0.139(8) 0.010(5) 0.026(6) 0.038(5) C61 0.189(9) 0.106(6) 0.161(9) -0.021(6) 0.009(7) 0.029(6) C62 0.110(5) 0.048(3) 0.155(7) 0.002(4) 0.043(5) 0.003(3) C63 0.178(7) 0.082(4) 0.140(7) 0.029(4) 0.066(6) 0.027(5) C64 0.199(9) 0.086(5) 0.191(9) 0.032(6) 0.089(8) 0.012(6) C65 0.150(6) 0.088(4) 0.139(6) -0.041(4) -0.031(5) 0.036(4) C66 0.156(7) 0.114(6) 0.153(8) -0.050(6) -0.041(6) 0.036(5) C67 0.187(10) 0.063(5) 0.235(13) -0.029(6) 0.063(9) -0.033(5) C68 0.202(11) 0.084(6) 0.382(16) -0.006(9) 0.019(11) -0.008(7) C69 0.331(17) 0.233(15) 0.287(16) -0.034(12) -0.105(14) 0.015(14) C70 0.31(2) 0.28(2) 0.34(2) 0.078(19) 0.020(19) 0.028(18) C62A 0.153(7) 0.076(4) 0.099(5) -0.015(3) 0.055(5) 0.003(4) C63A 0.211(10) 0.116(6) 0.128(8) -0.052(6) 0.052(7) 0.014(6) C64A 0.247(14) 0.157(10) 0.160(10) -0.073(8) 0.060(10) 0.036(10) C65A 0.220(10) 0.157(8) 0.204(9) -0.061(7) 0.112(8) -0.013(7) C66A 0.238(11) 0.186(10) 0.240(12) -0.072(9) 0.152(10) -0.033(9) C67A 0.284(15) 0.152(9) 0.159(10) -0.050(8) 0.112(11) 0.002(10) C68A 0.383(19) 0.333(19) 0.195(13) -0.065(12) 0.188(14) -0.058(16) C70A 0.307(16) 0.292(16) 0.268(15) -0.094(14) 0.119(13) -0.055(14) C71A 0.35(2) 0.54(4) 0.128(14) -0.034(17) 0.016(14) 0.00(2) C62B 0.143(7) 0.090(5) 0.096(6) 0.006(4) 0.027(5) -0.023(5) C63B 0.203(10) 0.114(6) 0.129(8) 0.027(5) 0.056(7) -0.021(6) C64B 0.193(11) 0.128(8) 0.184(11) 0.022(7) 0.091(9) -0.049(8) C65B 0.173(10) 0.110(7) 0.175(10) 0.040(6) 0.048(8) -0.013(6) C66B 0.133(8) 0.160(9) 0.174(10) 0.039(8) 0.034(7) -0.033(7) C67B 0.135(9) 0.140(9) 0.169(10) 0.009(8) 0.038(7) -0.018(7) C68B 0.157(11) 0.33(2) 0.210(15) -0.035(14) 0.068(10) -0.043(12) C69B 0.36(2) 0.44(3) 0.41(3) -0.06(2) 0.12(2) -0.01(2) C70B 0.184(13) 0.40(2) 0.32(2) -0.102(19) -0.063(14) 0.049(16) C71B 0.212(15) 0.204(16) 0.53(3) 0.059(19) 0.080(18) -0.041(13) C62C 0.152(8) 0.107(6) 0.110(7) -0.017(5) 0.001(6) -0.031(5) C63C 0.188(11) 0.236(13) 0.092(8) -0.012(7) 0.009(7) -0.073(10) C64C 0.173(12) 0.226(15) 0.175(14) -0.009(11) -0.021(10) -0.070(10) C65C 0.176(10) 0.155(8) 0.108(8) 0.003(6) 0.001(7) -0.005(7) C66C 0.168(11) 0.175(11) 0.127(10) 0.002(7) -0.031(8) -0.043(9) C67C 0.170(12) 0.153(10) 0.178(14) -0.006(9) -0.048(10) -0.019(9) C68C 0.174(13) 0.32(2) 0.241(18) 0.048(14) -0.015(12) -0.044(13) C70C 0.270(15) 0.223(14) 0.300(16) -0.022(13) -0.069(13) 0.077(12) C62D 0.107(5) 0.099(5) 0.078(5) 0.019(3) 0.015(4) 0.011(4) C63D 0.157(8) 0.116(6) 0.099(6) 0.035(5) -0.003(5) -0.012(6) C64D 0.147(8) 0.138(7) 0.136(8) 0.047(6) 0.004(6) 0.017(6) C65D 0.128(5) 0.066(3) 0.064(4) 0.013(3) 0.017(3) 0.012(3) C66D 0.123(6) 0.076(4) 0.080(5) 0.019(3) 0.021(4) 0.015(4) C67D 0.150(8) 0.121(6) 0.104(7) 0.042(5) 0.015(5) 0.013(6) C68D 0.174(9) 0.161(9) 0.123(8) 0.043(7) 0.018(6) 0.027(7) C69D 0.283(14) 0.092(6) 0.153(9) 0.049(6) 0.032(9) 0.039(7) C70D 0.36(2) 0.095(7) 0.279(19) 0.086(9) 0.085(17) -0.038(11) C71D 0.38(2) 0.210(15) 0.32(2) 0.186(16) -0.028(18) 0.013(15) 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' 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 C5 C1 C9 119.8(6) C5 C1 C2 105.0(5) C9 C1 C2 117.3(6) C5 C1 C61 101.6(6) C9 C1 C61 113.0(5) C2 C1 C61 96.8(6) C3 C2 C12 125.8(6) C3 C2 C1 104.9(6) C12 C2 C1 126.6(6) C2 C3 C4 111.8(6) C2 C3 C15 124.1(6) C4 C3 C15 121.5(6) C5 C4 C3 106.4(6) C5 C4 C18 126.2(6) C3 C4 C18 124.0(6) C4 C5 C1 110.7(5) C4 C5 C6 122.5(6) C1 C5 C6 124.9(6) C5 C6 C62D 116.3(6) C5 C6 C7 105.9(6) C62D C6 C7 112.5(5) C5 C6 C20 106.8(5) C62D C6 C20 113.1(6) C7 C6 C20 100.8(6) C8 C7 C22 119.0(7) C8 C7 C6 124.0(6) C22 C7 C6 110.8(6) C7 C8 C25 119.8(6) C7 C8 C9 126.3(7) C25 C8 C9 109.3(7) C62 C9 C8 110.9(5) C62 C9 C1 115.1(6) C8 C9 C1 109.0(5) C62 C9 C10 111.1(6) C8 C9 C10 99.8(6) C1 C9 C10 109.8(5) C11 C10 C26 119.1(7) C11 C10 C9 125.0(7) C26 C10 C9 110.4(6) C10 C11 C29 118.6(8) C10 C11 C12 125.8(7) C29 C11 C12 109.9(6) C2 C12 C11 106.6(5) C2 C12 C62A 117.6(7) C11 C12 C62A 112.4(6) C2 C12 C13 105.9(5) C11 C12 C13 101.7(6) C62A C12 C13 111.2(5) C14 C13 C30 121.1(7) C14 C13 C12 124.5(7) C30 C13 C12 107.5(6) C13 C14 C33 119.7(8) C13 C14 C15 124.0(6) C33 C14 C15 109.7(6) C3 C15 C62B 115.2(6) C3 C15 C14 106.0(6) C62B C15 C14 115.6(6) C3 C15 C16 106.6(5) C62B C15 C16 112.2(6) C14 C15 C16 99.7(6) C17 C16 C34 118.1(8) C17 C16 C15 125.9(7) C34 C16 C15 110.2(6) C16 C17 C37 120.4(8) C16 C17 C18 123.2(7) C37 C17 C18 110.0(7) C4 C18 C17 108.1(6) C4 C18 C19 108.0(6) C17 C18 C19 99.8(7) C4 C18 C62C 110.1(7) C17 C18 C62C 115.5(7) C19 C18 C62C 114.7(7) C20 C19 C38 121.4(8) C20 C19 C18 121.4(7) C38 C19 C18 110.6(7) C19 C20 C21 118.6(7) C19 C20 C6 125.7(7) C21 C20 C6 107.9(6) C40 C21 C20 121.0(7) C40 C21 C22 119.3(7) C20 C21 C22 109.7(6) C23 C22 C7 122.0(7) C23 C22 C21 120.6(6) C7 C22 C21 107.8(7) C24 C23 C22 118.3(6) C24 C23 C42 109.2(6) C22 C23 C42 118.7(7) C23 C24 C25 118.3(7) C23 C24 C44 107.7(6) C25 C24 C44 121.5(7) C8 C25 C24 122.5(7) C8 C25 C26 109.0(7) C24 C25 C26 118.1(7) C27 C26 C10 124.3(7) C27 C26 C25 119.2(7) C10 C26 C25 106.9(7) C26 C27 C45 124.0(7) C26 C27 C28 117.1(8) C45 C27 C28 106.2(7) C29 C28 C47 121.5(8) C29 C28 C27 119.1(7) C47 C28 C27 106.1(8) C28 C29 C11 121.8(7) C28 C29 C30 121.3(8) C11 C29 C30 107.2(7) C13 C30 C31 121.3(7) C13 C30 C29 110.1(7) C31 C30 C29 118.8(8) C30 C31 C32 117.4(9) C30 C31 C48 119.1(8) C32 C31 C48 109.5(8) C33 C32 C31 119.6(7) C33 C32 C50 121.9(8) C31 C32 C50 105.8(9) C32 C33 C34 119.3(8) C32 C33 C14 120.7(7) C34 C33 C14 109.8(7) C35 C34 C16 122.5(8) C35 C34 C33 120.0(9) C16 C34 C33 107.9(7) C34 C35 C36 118.4(10) C34 C35 C51 119.8(8) C36 C35 C51 109.2(10) C37 C36 C35 119.3(10) C37 C36 C53 121.8(9) C35 C36 C53 106.3(10) C36 C37 C17 121.2(8) C36 C37 C38 119.3(9) C17 C37 C38 108.4(8) C19 C38 C39 120.6(8) C19 C38 C37 108.9(8) C39 C38 C37 120.2(8) C38 C39 C54 122.1(9) C38 C39 C40 118.3(8) C54 C39 C40 107.8(9) C21 C40 C39 119.8(8) C21 C40 C41 120.2(7) C39 C40 C41 106.8(7) C42 C41 C40 121.4(6) C42 C41 C55 116.9(8) C40 C41 C55 109.3(8) C41 C42 C23 119.8(7) C41 C42 C43 121.0(7) C23 C42 C43 107.8(6) C57 C43 C44 120.8(7) C57 C43 C42 119.1(8) C44 C43 C42 107.0(6) C43 C44 C45 121.0(7) C43 C44 C24 108.3(7) C45 C44 C24 118.6(7) C46 C45 C44 117.5(7) C46 C45 C27 110.8(7) C44 C45 C27 118.4(7) C58 C46 C45 122.9(8) C58 C46 C47 120.1(8) C45 C46 C47 105.3(7) C48 C47 C28 119.8(8) C48 C47 C46 117.4(8) C28 C47 C46 111.5(7) C47 C48 C49 120.7(8) C47 C48 C31 119.4(7) C49 C48 C31 106.4(9) C59 C49 C50 118.1(9) C59 C49 C48 120.9(9) C50 C49 C48 108.9(9) C51 C50 C49 122.8(9) C51 C50 C32 116.3(10) C49 C50 C32 109.4(8) C50 C51 C35 122.4(9) C50 C51 C52 115.2(10) C35 C51 C52 110.2(9) C60 C52 C53 123.5(10) C60 C52 C51 122.6(10) C53 C52 C51 101.7(10) C36 C53 C54 119.4(11) C36 C53 C52 112.4(9) C54 C53 C52 115.7(11) C55 C54 C39 110.9(8) C55 C54 C53 119.8(10) C39 C54 C53 117.1(11) C56 C55 C54 120.9(8) C56 C55 C41 122.2(8) C54 C55 C41 105.2(8) C55 C56 C57 119.4(7) C55 C56 C60 121.1(9) C57 C56 C60 108.0(8) C43 C57 C56 121.4(8) C43 C57 C58 118.5(7) C56 C57 C58 107.5(8) C46 C58 C59 122.7(8) C46 C58 C57 119.3(7) C59 C58 C57 106.7(9) C49 C59 C60 122.3(10) C49 C59 C58 118.0(8) C60 C59 C58 108.7(8) C52 C60 C59 118.9(9) C52 C60 C56 119.1(10) C59 C60 C56 109.0(9) C65 C62 C63 120.3(7) C65 C62 C9 122.2(7) C63 C62 C9 117.1(7) C62 C63 C64 120.1(9) C67 C64 C63 117.9(10) C62 C65 C66 119.9(9) C67 C66 C65 116.4(9) C64 C67 C66 123.8(8) C64 C67 C68 118.8(13) C66 C67 C68 116.4(11) C69 C68 C67 114.6(10) C68 C69 C70 114.4(14) O2 C70 O1 124(2) O2 C70 C69 118.1(19) O1 C70 C69 114.5(18) C70 O2 C71 102.2(16) C63A C62A C65A 115.8(8) C63A C62A C12 124.0(8) C65A C62A C12 120.0(8) C62A C63A C64A 122.4(11) C67A C64A C63A 121.7(12) C62A C65A C66A 122.6(12) C67A C66A C65A 120.3(13) C64A C67A C66A 117.1(10) C64A C67A C68A 125.4(13) C66A C67A C68A 115.4(15) C69A C68A C67A 105.2(14) C68A C69A C70A 117.3(15) O1A C70A O2A 120.4(17) O1A C70A C69A 106.0(14) O2A C70A C69A 92.7(14) C70A O2A C71A 101.9(14) C65B C62B C63B 115.8(9) C65B C62B C15 122.9(7) C63B C62B C15 121.1(9) C62B C63B C64B 117.9(10) C67B C64B C63B 123.8(9) C62B C65B C66B 123.2(9) C67B C66B C65B 119.8(11) C64B C67B C66B 119.3(10) C64B C67B C68B 118.4(12) C66B C67B C68B 122.1(12) C69B C68B C67B 109.4(12) C68B C69B C70B 112.0(16) O1B C70B O2B 122.3(18) O1B C70B C69B 119.2(18) O2B C70B C69B 114.6(17) C70B O2B C71B 104.5(15) C63C C62C C65C 117.1(10) C63C C62C C18 121.9(10) C65C C62C C18 120.8(9) C62C C63C C64C 121.1(12) C67C C64C C63C 117.8(12) C66C C65C C62C 121.2(11) C67C C66C C65C 122.6(13) C66C C67C C64C 120.0(12) C66C C67C C68C 120.2(15) C64C C67C C68C 119.8(15) C69C C68C C67C 119.6(16) C68C C69C C70C 125.6(18) O1C C70C O2C 113.7(16) O1C C70C C69C 121.5(19) O2C C70C C69C 117.5(17) C70C O2C C71C 98.2(14) C65D C62D C63D 116.3(7) C65D C62D C6 123.5(7) C63D C62D C6 120.3(6) C62D C63D C64D 121.5(8) C63D C64D C67D 118.8(9) C62D C65D C66D 124.9(7) C67D C66D C65D 119.0(7) C66D C67D C64D 119.4(7) C66D C67D C68D 122.7(8) C64D C67D C68D 117.9(9) C69D C68D C67D 110.2(8) C68D C69D C70D 109.0(9) O1D C70D O2D 127.1(13) O1D C70D C69D 130.1(12) O2D C70D C69D 102.6(12) C70D O2D C71D 106.0(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C5 1.456(9) C1 C9 1.545(10) C1 C2 1.543(8) C1 C61 1.757(12) C2 C3 1.373(9) C2 C12 1.483(10) C3 C4 1.481(9) C3 C15 1.505(8) C4 C5 1.375(9) C4 C18 1.506(10) C5 C6 1.518(8) C6 C62D 1.523(9) C6 C7 1.543(10) C6 C20 1.569(9) C7 C8 1.347(9) C7 C22 1.435(9) C8 C25 1.416(10) C8 C9 1.539(9) C9 C62 1.514(7) C9 C10 1.559(10) C10 C11 1.393(9) C10 C26 1.412(10) C11 C29 1.423(11) C11 C12 1.491(10) C12 C62A 1.522(8) C12 C13 1.557(9) C13 C14 1.351(9) C13 C30 1.394(10) C14 C33 1.433(9) C14 C15 1.527(10) C15 C62B 1.524(10) C15 C16 1.553(9) C16 C17 1.367(10) C16 C34 1.431(11) C17 C37 1.429(11) C17 C18 1.518(10) C18 C19 1.528(11) C18 C62C 1.570(12) C19 C20 1.369(10) C19 C38 1.406(11) C20 C21 1.458(10) C21 C40 1.374(9) C21 C22 1.469(10) C22 C23 1.426(10) C23 C24 1.399(9) C23 C42 1.440(8) C24 C25 1.421(10) C24 C44 1.462(10) C25 C26 1.498(9) C26 C27 1.344(10) C27 C45 1.452(10) C27 C28 1.479(11) C28 C29 1.380(11) C28 C47 1.420(11) C29 C30 1.463(10) C30 C31 1.414(11) C31 C32 1.447(11) C31 C48 1.496(12) C32 C33 1.382(11) C32 C50 1.489(12) C33 C34 1.429(10) C34 C35 1.401(12) C35 C36 1.415(11) C35 C51 1.436(13) C36 C37 1.395(12) C36 C53 1.449(13) C37 C38 1.425(11) C38 C39 1.423(11) C39 C54 1.432(12) C39 C40 1.444(11) C40 C41 1.447(11) C41 C42 1.399(10) C41 C55 1.472(10) C42 C43 1.453(10) C43 C57 1.397(10) C43 C44 1.430(10) C44 C45 1.432(10) C45 C46 1.418(10) C46 C58 1.390(11) C46 C47 1.448(11) C47 C48 1.420(12) C48 C49 1.452(11) C49 C59 1.382(11) C49 C50 1.439(13) C50 C51 1.373(12) C51 C52 1.498(13) C52 C60 1.349(13) C52 C53 1.464(14) C53 C54 1.459(12) C54 C55 1.422(12) C55 C56 1.376(11) C56 C57 1.411(12) C56 C60 1.434(11) C57 C58 1.477(11) C58 C59 1.425(12) C59 C60 1.405(12) C62 C65 1.355(10) C62 C63 1.412(11) C63 C64 1.434(11) C64 C67 1.352(15) C65 C66 1.478(12) C66 C67 1.393(14) C67 C68 1.621(12) C68 C69 1.478(16) C69 C70 1.540(17) C70 O2 1.262(19) C70 O1 1.35(2) C71 O2 1.69(2) C62A C63A 1.338(11) C62A C65A 1.367(14) C63A C64A 1.391(12) C64A C67A 1.355(17) C65A C66A 1.400(13) C66A C67A 1.358(17) C67A C68A 1.706(15) C68A C69A 1.355(18) C69A C70A 1.664(18) C70A O1A 1.422(19) C70A O2A 1.490(18) C71A O2A 1.552(17) C62B C65B 1.374(12) C62B C63B 1.381(10) C63B C64B 1.444(14) C64B C67B 1.299(14) C65B C66B 1.412(13) C66B C67B 1.315(13) C67B C68B 1.586(13) C68B C69B 1.538(18) C69B C70B 1.530(18) C70B O1B 1.33(2) C70B O2B 1.319(17) C71B O2B 1.623(18) C62C C63C 1.377(13) C62C C65C 1.422(13) C63C C64C 1.454(16) C64C C67C 1.430(17) C65C C66C 1.390(15) C66C C67C 1.307(16) C67C C68C 1.554(15) C68C C69C 1.371(17) C69C C70C 1.478(18) C70C O1C 1.372(18) C70C O2C 1.338(18) C71C O2C 1.67(2) C62D C65D 1.320(8) C62D C63D 1.378(10) C63D C64D 1.401(11) C64D C67D 1.406(12) C65D C66D 1.399(8) C66D C67D 1.328(10) C67D C68D 1.561(10) C68D C69D 1.507(11) C69D C70D 1.569(12) C70D O1D 1.236(16) C70D O2D 1.328(13) C71D O2D 1.570(13)