#------------------------------------------------------------------------------ #$Date: 2024-10-12 01:12:32 +0300 (Sat, 12 Oct 2024) $ #$Revision: 295438 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572861.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_1572861 loop_ _publ_author_name 'Kumar, Rakesh' 'Chmielewski, Piotr J.' 'Lis, Tadeusz' 'Czarnecki, Miros\/law' 'St\;epie\'n, Marcin' _publ_section_title ; Pentacosacyclenes: Cruciform Molecular Nanocarbons Based on Cyclooctatetraene ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05938G _journal_year 2024 _chemical_formula_moiety 'C120 H104, 6(C6 H14)' _chemical_formula_sum 'C156 H188' _chemical_formula_weight 2063.05 _space_group_crystal_system tetragonal _space_group_IT_number 142 _space_group_name_Hall '-I 4bd 2c' _space_group_name_H-M_alt 'I 41/a c d :2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2023-10-11 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-09-01 deposited with the CCDC. 2024-10-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 21.398(3) _cell_length_b 21.398(3) _cell_length_c 53.967(14) _cell_measurement_reflns_used 25909 _cell_measurement_temperature 80(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 1.9 _cell_volume 24710(8) _computing_cell_refinement 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008' _diffrn_ambient_temperature 80(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix-Arc 150' _diffrn_measurement_method 'omega scan' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1481 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 71 _diffrn_reflns_limit_l_min -71 _diffrn_reflns_number 194560 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 27.998 _diffrn_reflns_theta_min 1.903 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.109 _exptl_crystal_description plate _exptl_crystal_F_000 8992 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.459 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.614 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 404 _refine_ls_number_reflns 7461 _refine_ls_number_restraints 53 _refine_ls_restrained_S_all 1.682 _refine_ls_R_factor_all 0.1883 _refine_ls_R_factor_gt 0.1132 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2734 _refine_ls_wR_factor_ref 0.2976 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3702 _reflns_number_total 7461 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05938g3.cif _cod_data_source_block rk275ba _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_primary' value 'direct methods' was changed to 'direct'. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 24710(9) _cod_original_sg_symbol_H-M 'I 41/a c d' _cod_database_code 1572861 _shelxl_version_number 2013-2 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.998 _shelx_estimated_absorpt_t_min 0.991 _olex2_refinement_description ; 1. Restrained distances C27-C28 = C27-C29 = C27-C29 = C27-C31 = C27-C32 = C27-C33 1.52 with sigma of 0.01 C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C46 1.52 with sigma of 0.015 C41-C43 = C42-C44 = C43-C45 = C44-C46 2.5 with sigma of 0.02 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56 1.52 with sigma of 0.015 C51-C53 = C52-C54 = C53-C55 = C54-C56 2.5 with sigma of 0.02 C81-C82 = C82-C83 = C83-C84 = C84-C85 = C85-C86 1.52 with sigma of 0.015 C81-C83 = C82-C84 = C83-C85 = C84-C86 2.5 with sigma of 0.02 C94-C95 = C95-C96 = C96-C96_$1 1.52 with sigma of 0.015 C94-C96 = C95-C96_$1 2.5 with sigma of 0.02 2. Uiso/Uaniso restraints and constraints Uiso(C41) = Uiso(C42) = Uiso(C43) = Uiso(C44) = Uiso(C45) = Uiso(C46) Uiso(C71) = Uiso(C72) = Uiso(C73) Uiso(C61) = Uiso(C62) = Uiso(C63) Uiso(C51) = Uiso(C52) = Uiso(C53) = Uiso(C54) = Uiso(C55) = Uiso(C56) Uiso(C81) = Uiso(C82) = Uiso(C83) = Uiso(C84) = Uiso(C85) = Uiso(C86) Uiso(C91) = Uiso(C92) = Uiso(C93) Uiso(C94) = Uiso(C95) = Uiso(C96) 3. Others Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C71(0.25) H71A(0.25) H71B(0.25) H71C(0.25) C72(0.25) H72A(0.25) H72B(0.25) C73(0.25) H73A(0.25) H73B(0.25) C61(0.25) H61A(0.25) H61B(0.25) H61C(0.25) C62(0.25) H62A(0.25) H62B(0.25) C63(0.25) H63A(0.25) H63B(0.25) C51(0.25) H51A(0.25) H51B(0.25) H51C(0.25) C52(0.25) H52A(0.25) H52B(0.25) C53(0.25) H53A(0.25) H53B(0.25) C54(0.25) H54A(0.25) H54B(0.25) C55(0.25) H55A(0.25) H55B(0.25) C56(0.25) H56A(0.25) H56B(0.25) H56C(0.25) C81(0.25) H81A(0.25) H81B(0.25) H81C(0.25) C82(0.25) H82A(0.25) H82B(0.25) C83(0.25) H83A(0.25) H83B(0.25) C84(0.25) H84A(0.25) H84B(0.25) C85(0.25) H85A(0.25) H85B(0.25) C86(0.25) H86A(0.25) H86B(0.25) H86C(0.25) C91(0.25) H91A(0.25) H91B(0.25) H91C(0.25) C92(0.25) H92A(0.25) H92B(0.25) C93(0.25) H93A(0.25) H93B(0.25) C94(0.25) H94A(0.25) H94B(0.25) H94C(0.25) C95(0.25) H95A(0.25) H95B(0.25) C96(0.25) H96A(0.25) H96B(0.25) 4.a Riding coordinates: C73(H73A,H73B), C93(H93A,H93B) 4.b Secondary CH2 refined with riding coordinates: C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C72(H72A, H72B), C62(H62A,H62B), C63(H63A,H63B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C92(H92A,H92B), C95(H95A,H95B), C96(H96A,H96B) 4.c Me refined with riding coordinates: C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C71(H71A,H71B,H71C), C61(H61A,H61B, H61C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C81(H81A,H81B,H81C), C86(H86A, H86B,H86C), C91(H91A,H91B,H91C), C94(H94A,H94B,H94C) 4.d Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C8(H8), C9(H9), C14(H14), C16(H16), C17(H17), C19(H19) 4.e Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B, H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C), C33(H33A,H33B,H33C) ; _shelx_res_file ; tITL rk275b in I41/acd #142 CELL 0.71073 21.398 21.398 53.967 90 90 90 ZERR 8 0.003 0.003 0.014 0 0 0 LATT 2 SYMM 0.25-Y,0.75+X,0.25+Z SYMM -X,0.5-Y,+Z SYMM 0.25+Y,0.25-X,0.75+Z SYMM +X,-Y,0.5-Z SYMM 0.5-X,+Y,-Z SYMM 0.75+Y,0.25+X,0.25-Z SYMM 0.25-Y,0.25-X,0.25-Z SFAC C H UNIT 1248 1504 acta 51 omit -1 56 size 0.04 0.12 0.15 L.S. 10 PLAN 20 TEMP -193 fmap 2 bond $h WGHT 0.100000 FVAR 0.07746 C1 1 0.522399 0.328640 0.618793 11.00000 0.06092 0.05675 = 0.06040 -0.00706 0.00567 -0.00002 C2 1 0.571624 0.287037 0.617881 11.00000 0.05540 0.05328 = 0.06833 0.00032 0.00522 -0.00056 C3 1 0.622174 0.314698 0.602522 11.00000 0.06173 0.04969 = 0.06620 0.00527 0.00567 0.00182 C4 1 0.679967 0.296904 0.593863 11.00000 0.06374 0.04852 = 0.07371 0.01014 0.00911 0.01018 AFIX 43 H4 2 0.696509 0.257007 0.597940 11.00000 -1.20000 AFIX 0 C5 1 0.714343 0.338399 0.578905 11.00000 0.05980 0.05135 = 0.07140 0.01022 0.01043 0.00961 AFIX 43 H5 2 0.754222 0.325281 0.573177 11.00000 -1.20000 AFIX 0 C6 1 0.693558 0.397194 0.572030 11.00000 0.06287 0.04779 = 0.06107 0.00021 0.00062 0.00388 C7 1 0.605282 0.474978 0.575632 11.00000 0.06143 0.04867 = 0.06310 0.00129 -0.00317 0.00632 C8 1 0.544825 0.485162 0.584765 11.00000 0.06649 0.04851 = 0.07387 -0.00067 -0.00233 0.01134 AFIX 43 H8 2 0.525227 0.523932 0.581133 11.00000 -1.20000 AFIX 0 C9 1 0.511553 0.441461 0.598955 11.00000 0.05928 0.05821 = 0.07157 -0.00608 0.00205 0.00859 AFIX 43 H9 2 0.470222 0.450291 0.604346 11.00000 -1.20000 AFIX 0 C10 1 0.539960 0.384966 0.605026 11.00000 0.06097 0.05354 = 0.06110 -0.00409 0.00132 0.00330 C11 1 0.600110 0.374347 0.595476 11.00000 0.05575 0.04997 = 0.06350 0.00024 0.00312 0.00492 C12 1 0.633173 0.416162 0.580733 11.00000 0.05897 0.04677 = 0.06185 0.00134 0.00181 0.00216 C13 1 0.728427 0.441526 0.556466 11.00000 0.05875 0.04768 = 0.06520 0.00479 -0.00119 0.00196 C14 1 0.784907 0.427428 0.545808 11.00000 0.06494 0.05098 = 0.07258 0.01301 0.00135 0.00331 AFIX 43 H14 2 0.801896 0.386990 0.548530 11.00000 -1.20000 AFIX 0 C15 1 0.819216 0.469773 0.530995 11.00000 0.05962 0.05736 = 0.07422 0.01492 -0.00306 -0.00200 C16 1 0.794504 0.528024 0.527707 11.00000 0.06583 0.05207 = 0.07520 0.01194 -0.00166 -0.00502 AFIX 43 H16 2 0.817230 0.557577 0.518148 11.00000 -1.20000 AFIX 0 C17 1 0.712691 0.606508 0.533969 11.00000 0.08327 0.04570 = 0.08031 0.01088 -0.00999 -0.00252 AFIX 43 H17 2 0.736402 0.635542 0.524536 11.00000 -1.20000 AFIX 0 C18 1 0.655343 0.624952 0.543468 11.00000 0.08842 0.03990 = 0.09169 0.00709 -0.01123 0.00604 C19 1 0.620560 0.581152 0.556891 11.00000 0.07105 0.04772 = 0.08400 -0.00257 -0.00607 0.00625 AFIX 43 H19 2 0.580790 0.593083 0.563123 11.00000 -1.20000 AFIX 0 C20 1 0.641836 0.520908 0.561473 11.00000 0.06910 0.04827 = 0.06487 -0.00186 -0.00855 0.00474 C21 1 0.701759 0.502319 0.552171 11.00000 0.06355 0.04428 = 0.06395 0.00456 -0.00417 0.00380 C22 1 0.736903 0.545975 0.537878 11.00000 0.06827 0.04620 = 0.06895 0.00416 -0.00719 -0.00334 C23 1 0.880871 0.448187 0.518997 11.00000 0.06317 0.06829 = 0.09393 0.02590 0.01155 0.00486 C24 1 0.910938 0.501237 0.503701 11.00000 0.07766 0.09591 = 0.13184 0.04322 0.02293 0.00419 AFIX 137 H24A 2 0.879682 0.519154 0.492489 11.00000 -1.50000 H24B 2 0.945817 0.484439 0.493998 11.00000 -1.50000 H24C 2 0.926400 0.533790 0.514907 11.00000 -1.50000 AFIX 0 C25 1 0.866922 0.394933 0.501109 11.00000 0.10443 0.08206 = 0.10590 0.01616 0.04018 0.01713 AFIX 137 H25A 2 0.844353 0.361748 0.509858 11.00000 -1.50000 H25B 2 0.906232 0.378259 0.494544 11.00000 -1.50000 H25C 2 0.841203 0.410527 0.487414 11.00000 -1.50000 AFIX 0 C26 1 0.925880 0.426771 0.539116 11.00000 0.06548 0.12752 = 0.12758 0.03850 0.00338 0.01515 AFIX 137 H26A 2 0.935010 0.461782 0.550249 11.00000 -1.50000 H26B 2 0.964757 0.412117 0.531475 11.00000 -1.50000 H26C 2 0.906854 0.392624 0.548578 11.00000 -1.50000 AFIX 0 C27 1 0.630649 0.691829 0.539855 11.00000 0.10560 0.04509 = 0.12840 0.00803 -0.00016 0.01274 part 1 dfix 1.52 0.01 c27 c28 c27 c29 c27 c29 c27 c31 c27 c32 c27 c33 C28 1 0.569026 0.688722 0.527018 10.50000 0.13333 0.06250 = 0.16217 0.02952 -0.03403 0.04334 AFIX 137 H28A 2 0.548641 0.729685 0.527816 10.50000 -1.50000 H28B 2 0.542561 0.657476 0.535152 10.50000 -1.50000 H28C 2 0.575371 0.676964 0.509649 10.50000 -1.50000 AFIX 0 C29 1 0.631542 0.722230 0.565620 10.50000 0.13872 0.04974 = 0.19823 -0.03722 0.02391 0.00050 AFIX 137 H29A 2 0.673639 0.719066 0.572661 10.50000 -1.50000 H29B 2 0.601779 0.700688 0.576461 10.50000 -1.50000 H29C 2 0.619777 0.766343 0.564184 10.50000 -1.50000 AFIX 0 C30 1 0.683009 0.733301 0.526245 10.50000 0.11011 0.04401 = 0.20591 0.04405 0.00686 0.00187 AFIX 137 H30A 2 0.724082 0.723981 0.533378 10.50000 -1.50000 H30B 2 0.673524 0.777729 0.528548 10.50000 -1.50000 H30C 2 0.683353 0.723486 0.508508 10.50000 -1.50000 AFIX 0 part 2 C31 1 0.565590 0.702773 0.552302 10.50000 0.07968 0.04723 = 0.35079 0.01950 -0.04362 0.00759 AFIX 137 H31A 2 0.534296 0.675958 0.544380 10.50000 -1.50000 H31B 2 0.553460 0.746662 0.550354 10.50000 -1.50000 H31C 2 0.568233 0.692560 0.569973 10.50000 -1.50000 AFIX 0 C32 1 0.672093 0.737740 0.550175 10.50000 0.11579 0.04179 = 0.09340 0.00992 -0.00460 -0.00189 AFIX 137 H32A 2 0.680363 0.727695 0.567586 10.50000 -1.50000 H32B 2 0.652709 0.779139 0.549064 10.50000 -1.50000 H32C 2 0.711494 0.737721 0.540918 10.50000 -1.50000 AFIX 0 C33 1 0.622798 0.703333 0.511567 10.50000 0.39755 0.04813 = 0.18868 -0.01532 -0.20976 0.03966 AFIX 137 H33A 2 0.591377 0.674525 0.504929 10.50000 -1.50000 H33B 2 0.662817 0.696220 0.503199 10.50000 -1.50000 H33C 2 0.609255 0.746503 0.508751 10.50000 -1.50000 AFIX 0 part -3 dfix 1.52 0.015 c41 c42 c42 c43 c43 c44 c44 c45 c45 c46 dfix 2.5 c41 c43 c42 c44 c43 c45 c44 c46 eadp c41 > c46 C41 1 0.852971 0.617085 0.579369 10.50000 0.14350 AFIX 33 H41A 2 0.893409 0.600469 0.573958 10.50000 -1.50000 H41B 2 0.859535 0.655858 0.588677 10.50000 -1.50000 H41C 2 0.826840 0.625650 0.564847 10.50000 -1.50000 AFIX 0 C42 1 0.821075 0.570132 0.595606 10.50000 0.14350 AFIX 23 H42A 2 0.813629 0.531615 0.585882 10.50000 -1.20000 H42B 2 0.849340 0.559252 0.609474 10.50000 -1.20000 AFIX 0 C43 1 0.760182 0.592148 0.606042 10.50000 0.14350 AFIX 23 H43A 2 0.733710 0.606784 0.592161 10.50000 -1.20000 H43B 2 0.768503 0.628623 0.616834 10.50000 -1.20000 AFIX 0 C44 1 0.723106 0.544335 0.620915 10.50000 0.14350 AFIX 23 H44A 2 0.745309 0.535044 0.636582 10.50000 -1.20000 H44B 2 0.719635 0.505017 0.611345 10.50000 -1.20000 AFIX 0 C45 1 0.654037 0.570749 0.627021 10.50000 0.14350 AFIX 23 H45A 2 0.657200 0.609499 0.636965 10.50000 -1.50000 H45B 2 0.631807 0.580660 0.611421 10.50000 -1.50000 AFIX 0 C46 1 0.618170 0.521252 0.641412 10.50000 0.14350 AFIX 33 H46A 2 0.576294 0.536931 0.645338 10.50000 -1.50000 H46B 2 0.640458 0.511657 0.656813 10.50000 -1.50000 H46C 2 0.614652 0.483279 0.631356 10.50000 -1.50000 AFIX 0 part -4 eadp c71 c72 c73 C71 1 0.642891 0.887906 0.630319 10.25000 0.25955 AFIX 33 H71A 2 0.663222 0.927950 0.633880 10.25000 -1.50000 H71B 2 0.671176 0.861605 0.620561 10.25000 -1.50000 H71C 2 0.632751 0.866770 0.645919 10.25000 -1.50000 AFIX 0 C72 1 0.582763 0.899461 0.615626 10.25000 0.25955 AFIX 23 H72A 2 0.592546 0.910517 0.598240 10.25000 -1.20000 H72B 2 0.558358 0.933915 0.623127 10.25000 -1.20000 AFIX 0 C73 1 0.545201 0.836633 0.616800 10.25000 0.25955 AFIX 3 H73A 2 0.506090 0.844304 0.626115 10.25000 -1.50000 H73B 2 0.534746 0.819254 0.600313 10.25000 -1.50000 AFIX 0 dfix 1.52 0.015 c71 c72 c72 c73 c73 c73_$2 dfix 2.5 c71 c73 c72 c73_$2 eqiv $2 y-1/4, x+1/4, -z+5/4 part 5 eadp c61 > c63 C61 1 0.628342 0.803232 0.628621 10.25000 0.21147 AFIX 33 H61A 2 0.603815 0.841909 0.628654 10.25000 -1.50000 H61B 2 0.650948 0.799575 0.612895 10.25000 -1.50000 H61C 2 0.658305 0.804081 0.642351 10.25000 -1.50000 AFIX 0 C62 1 0.584664 0.747360 0.631680 10.25000 0.21147 AFIX 23 H62A 2 0.548829 0.752406 0.620250 10.25000 -1.20000 H62B 2 0.568036 0.747333 0.648799 10.25000 -1.20000 AFIX 0 C63 1 0.615653 0.684251 0.626639 10.25000 0.21147 AFIX 23 H63A 2 0.641519 0.686972 0.611468 10.25000 -1.20000 H63B 2 0.643286 0.673007 0.640661 10.25000 -1.20000 AFIX 0 dfix 1.52 c61 c62 c62 c63 c63 c63_$1 dfix 2.5 c61 c63 c62 c63_$1 eqiv $1 -y+5/4, -x+5/4, -z+5/4 part -6 eadp c51 > c56 C51 1 0.860682 0.626271 0.602968 10.25000 0.19579 AFIX 33 H51A 2 0.866763 0.663432 0.592631 10.25000 -1.50000 H51B 2 0.891977 0.594668 0.598634 10.25000 -1.50000 H51C 2 0.865254 0.637662 0.620463 10.25000 -1.50000 AFIX 0 C52 1 0.795967 0.600121 0.598610 10.25000 0.19579 AFIX 23 H52A 2 0.788011 0.597040 0.580580 10.25000 -1.20000 H52B 2 0.764423 0.628643 0.605835 10.25000 -1.20000 AFIX 0 C53 1 0.789735 0.534386 0.610627 10.25000 0.19579 AFIX 23 H53A 2 0.795072 0.537233 0.628814 10.25000 -1.20000 H53B 2 0.748035 0.516435 0.607093 10.25000 -1.20000 AFIX 0 C54 1 0.841609 0.493077 0.599184 10.25000 0.19579 AFIX 23 H54A 2 0.824796 0.471436 0.584404 10.25000 -1.20000 H54B 2 0.876567 0.520055 0.593709 10.25000 -1.20000 AFIX 0 C55 1 0.865067 0.446971 0.616540 10.25000 0.19579 AFIX 23 H55A 2 0.830360 0.439418 0.628295 10.25000 -1.20000 H55B 2 0.898017 0.468652 0.626128 10.25000 -1.20000 AFIX 0 C56 1 0.890784 0.384800 0.610910 10.25000 0.19579 AFIX 33 H56A 2 0.927731 0.377261 0.621216 10.25000 -1.50000 H56B 2 0.902575 0.382891 0.593379 10.25000 -1.50000 H56C 2 0.859174 0.352838 0.614385 10.25000 -1.50000 AFIX 0 dfix 1.52 0.015 c51 c52 c52 c53 c53 c54 c54 c55 c55 c56 dfix 2.5 c51 c53 c52 c54 c53 c55 c54 c56 part -7 eadp c81 > c86 C81 1 1.084636 0.734647 0.545914 10.25000 0.15622 AFIX 33 H81A 2 1.127042 0.735256 0.552769 10.25000 -1.50000 H81B 2 1.086810 0.733430 0.527782 10.25000 -1.50000 H81C 2 1.062475 0.697571 0.551950 10.25000 -1.50000 AFIX 0 C82 1 1.048941 0.794651 0.554261 10.25000 0.15622 AFIX 23 H82A 2 1.050226 0.799815 0.572483 10.25000 -1.20000 H82B 2 1.066277 0.832541 0.546288 10.25000 -1.20000 AFIX 0 C83 1 0.982472 0.780973 0.545171 10.25000 0.15622 AFIX 23 H83A 2 0.977419 0.793528 0.527629 10.25000 -1.20000 H83B 2 0.951260 0.803546 0.555333 10.25000 -1.20000 AFIX 0 C84 1 0.974835 0.708217 0.548174 10.25000 0.15622 AFIX 23 H84A 2 0.999727 0.686280 0.535389 10.25000 -1.20000 H84B 2 0.990049 0.694986 0.564685 10.25000 -1.20000 AFIX 0 C85 1 0.904435 0.691354 0.545305 10.25000 0.15622 AFIX 23 H85A 2 0.879134 0.729619 0.547691 10.25000 -1.20000 H85B 2 0.896987 0.676143 0.528234 10.25000 -1.20000 AFIX 0 C86 1 0.882940 0.642502 0.563314 10.25000 0.15622 AFIX 33 H86A 2 0.837333 0.638824 0.562527 10.25000 -1.50000 H86B 2 0.895459 0.654502 0.580121 10.25000 -1.50000 H86C 2 0.901983 0.602253 0.559062 10.25000 -1.50000 AFIX 0 dfix 1.52 0.015 c81 c82 c82 c83 c83 c84 c84 c85 c85 c86 dfix 2.5 c81 c83 c82 c84 c83 c85 c84 c86 part 8 eadp c91 > c93 C91 1 1.030240 0.853658 0.545186 10.25000 0.13900 AFIX 33 H91A 2 1.045848 0.892958 0.552161 10.25000 -1.50000 H91B 2 0.985276 0.850157 0.548347 10.25000 -1.50000 H91C 2 1.037828 0.853069 0.527279 10.25000 -1.50000 AFIX 0 C92 1 1.064109 0.798873 0.557278 10.25000 0.13900 AFIX 23 H92A 2 1.056454 0.797842 0.575365 10.25000 -1.20000 H92B 2 1.109686 0.801108 0.554249 10.25000 -1.20000 AFIX 0 C93 1 1.034161 0.739582 0.543966 10.25000 0.13900 AFIX 3 H93A 2 1.048780 0.726123 0.527562 10.25000 -1.20000 H93B 2 1.046212 0.708055 0.556465 10.25000 -1.20000 dfix 1.52 0.015 c91 c92 c92 c93 c93 c93_$5 dfix 2.5 c91 c93 c92 c93_$5 eqiv $5 -x+2, -y+3/2, z AFIX 0 part 9 eadp c94 > c96 C94 1 1.075019 0.863658 0.552519 10.25000 0.11309 AFIX 33 H94A 2 1.095400 0.887292 0.539228 10.25000 -1.50000 H94B 2 1.102335 0.829390 0.557795 10.25000 -1.50000 H94C 2 1.066944 0.891417 0.566603 10.25000 -1.50000 AFIX 0 C95 1 1.009471 0.835326 0.542478 10.25000 0.11309 AFIX 23 H95A 2 0.972266 0.853901 0.550519 10.25000 -1.20000 H95B 2 1.005401 0.836546 0.524211 10.25000 -1.20000 AFIX 0 C96 1 1.026413 0.771312 0.552471 10.25000 0.11309 AFIX 23 H96A 2 1.060364 0.753366 0.542240 10.25000 -1.20000 H96B 2 1.042292 0.775763 0.569611 10.25000 -1.20000 dfix 1.52 0.015 c94 c95 c95 c96 c96 c96_$5 dfix 2.5 c94 c96 c95 c96_$5 AFIX 0 hklf 4 REM rk275b in I41/acd #142 REM R1 = 0.1132 for 3702 Fo > 4sig(Fo) and 0.1883 for all 7461 data REM 404 parameters refined using 53 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.459, deepest hole -0.519, 1-sigma level 0.069 Q1 1 0.8330 0.4171 0.6250 10.50000 0.05 0.46 Q2 1 0.7980 0.4866 0.6196 11.00000 0.05 0.35 Q3 1 1.1428 0.8187 0.5479 11.00000 0.05 0.33 Q4 1 1.0618 0.8425 0.5525 11.00000 0.05 0.31 Q5 1 0.8353 0.6073 0.5849 11.00000 0.05 0.30 Q6 1 0.8792 0.4432 0.6072 11.00000 0.05 0.30 Q7 1 1.0727 0.8458 0.5567 11.00000 0.05 0.30 Q8 1 0.6102 0.6947 0.6247 11.00000 0.05 0.29 Q9 1 0.6056 0.6841 0.5091 11.00000 0.05 0.27 Q10 1 0.8809 0.3609 0.6207 11.00000 0.05 0.27 Q11 1 0.5051 0.8870 0.6304 11.00000 0.05 0.26 Q12 1 0.5045 0.3228 0.6262 11.00000 0.05 0.26 Q13 1 0.5384 0.2944 0.6177 11.00000 0.05 0.26 Q14 1 0.5380 0.7880 0.6250 10.50000 0.05 0.25 Q15 1 0.6330 0.6903 0.5277 11.00000 0.05 0.23 Q16 1 1.0085 0.6702 0.5386 11.00000 0.05 0.23 Q17 1 0.6644 0.4107 0.5780 11.00000 0.05 0.23 Q18 1 0.6149 0.3404 0.5979 11.00000 0.05 0.22 Q19 1 0.6016 0.7499 0.6340 11.00000 0.05 0.21 Q20 1 0.5000 0.7500 0.6250 10.25000 0.05 0.21 ; _shelx_res_checksum 76568 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.276 _oxdiff_exptl_absorpt_empirical_full_min 0.456 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/4, x+3/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+3/4' 'x, -y, -z+1/2' '-x+1/2, y, -z' 'y+3/4, x+1/4, -z+1/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+5/4' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' 'y+5/4, x+3/4, -z+3/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'y-1/4, -x-3/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-3/4' '-x, y, z-1/2' 'x-1/2, -y, z' '-y-3/4, -x-1/4, z-1/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z-1/4' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-y-1/4, -x+1/4, z+1/4' 'y+1/4, x+1/4, z+1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.52240(14) 0.32864(13) 0.61879(5) 0.0594(7) Uani 1 1 d . . . . . C2 C 0.57162(13) 0.28704(13) 0.61788(5) 0.0590(8) Uani 1 1 d . . . . . C3 C 0.62217(14) 0.31470(13) 0.60252(5) 0.0592(7) Uani 1 1 d . . . . . C4 C 0.67997(14) 0.29690(13) 0.59386(5) 0.0620(8) Uani 1 1 d . . . . . H4 H 0.6965 0.2570 0.5979 0.074 Uiso 1 1 calc R U . . . C5 C 0.71434(14) 0.33840(13) 0.57891(5) 0.0609(8) Uani 1 1 d . . . . . H5 H 0.7542 0.3253 0.5732 0.073 Uiso 1 1 calc R U . . . C6 C 0.69356(13) 0.39719(13) 0.57203(5) 0.0572(7) Uani 1 1 d . . . . . C7 C 0.60528(14) 0.47498(13) 0.57563(5) 0.0577(7) Uani 1 1 d . . . . . C8 C 0.54483(14) 0.48516(13) 0.58476(5) 0.0630(8) Uani 1 1 d . . . . . H8 H 0.5252 0.5239 0.5811 0.076 Uiso 1 1 calc R U . . . C9 C 0.51155(14) 0.44146(14) 0.59895(5) 0.0630(8) Uani 1 1 d . . . . . H9 H 0.4702 0.4503 0.6043 0.076 Uiso 1 1 calc R U . . . C10 C 0.53996(14) 0.38497(13) 0.60503(5) 0.0585(7) Uani 1 1 d . . . . . C11 C 0.60011(13) 0.37435(13) 0.59548(5) 0.0564(7) Uani 1 1 d . . . . . C12 C 0.63317(13) 0.41616(12) 0.58073(5) 0.0559(7) Uani 1 1 d . . . . . C13 C 0.72843(13) 0.44153(13) 0.55647(5) 0.0572(7) Uani 1 1 d . . . . . C14 C 0.78491(14) 0.42743(14) 0.54581(6) 0.0628(8) Uani 1 1 d . . . . . H14 H 0.8019 0.3870 0.5485 0.075 Uiso 1 1 calc R U . . . C15 C 0.81922(14) 0.46977(14) 0.53099(6) 0.0637(8) Uani 1 1 d . . . . . C16 C 0.79450(14) 0.52802(14) 0.52771(6) 0.0644(8) Uani 1 1 d . . . . . H16 H 0.8172 0.5576 0.5181 0.077 Uiso 1 1 calc R U . . . C17 C 0.71269(16) 0.60651(14) 0.53397(6) 0.0698(9) Uani 1 1 d . . . . . H17 H 0.7364 0.6355 0.5245 0.084 Uiso 1 1 calc R U . . . C18 C 0.65534(17) 0.62495(13) 0.54347(7) 0.0733(9) Uani 1 1 d . . . . . C19 C 0.62056(15) 0.58115(13) 0.55689(6) 0.0676(8) Uani 1 1 d . . . . . H19 H 0.5808 0.5931 0.5631 0.081 Uiso 1 1 calc R U . . . C20 C 0.64184(14) 0.52091(13) 0.56147(5) 0.0607(8) Uani 1 1 d . . . . . C21 C 0.70176(13) 0.50232(13) 0.55217(5) 0.0573(7) Uani 1 1 d . . . . . C22 C 0.73690(14) 0.54598(13) 0.53788(5) 0.0611(8) Uani 1 1 d . . . . . C23 C 0.88087(15) 0.44819(16) 0.51900(7) 0.0751(10) Uani 1 1 d . . . . . C24 C 0.91094(17) 0.50124(19) 0.50370(8) 0.1018(13) Uani 1 1 d . . . . . H24A H 0.8797 0.5192 0.4925 0.153 Uiso 1 1 calc R U . . . H24B H 0.9458 0.4844 0.4940 0.153 Uiso 1 1 calc R U . . . H24C H 0.9264 0.5338 0.5149 0.153 Uiso 1 1 calc R U . . . C25 C 0.86692(19) 0.39493(18) 0.50111(8) 0.0975(13) Uani 1 1 d . . . . . H25A H 0.8444 0.3617 0.5099 0.146 Uiso 1 1 calc R U . . . H25B H 0.9062 0.3783 0.4945 0.146 Uiso 1 1 calc R U . . . H25C H 0.8412 0.4105 0.4874 0.146 Uiso 1 1 calc R U . . . C26 C 0.92588(17) 0.4268(2) 0.53912(8) 0.1069(14) Uani 1 1 d . . . . . H26A H 0.9350 0.4618 0.5502 0.160 Uiso 1 1 calc R U . . . H26B H 0.9648 0.4121 0.5315 0.160 Uiso 1 1 calc R U . . . H26C H 0.9069 0.3926 0.5486 0.160 Uiso 1 1 calc R U . . . C27 C 0.63065(19) 0.69183(15) 0.53985(8) 0.0930(12) Uani 1 1 d D . . . . C28 C 0.5690(5) 0.6887(5) 0.5270(3) 0.119(4) Uani 0.5 1 d D . P A 1 H28A H 0.5486 0.7297 0.5278 0.179 Uiso 0.5 1 calc R U P A 1 H28B H 0.5426 0.6575 0.5352 0.179 Uiso 0.5 1 calc R U P A 1 H28C H 0.5754 0.6770 0.5096 0.179 Uiso 0.5 1 calc R U P A 1 C29 C 0.6315(5) 0.7222(4) 0.56562(16) 0.129(4) Uani 0.5 1 d D . P A 1 H29A H 0.6736 0.7191 0.5727 0.193 Uiso 0.5 1 calc R U P A 1 H29B H 0.6018 0.7007 0.5765 0.193 Uiso 0.5 1 calc R U P A 1 H29C H 0.6198 0.7663 0.5642 0.193 Uiso 0.5 1 calc R U P A 1 C30 C 0.6830(4) 0.7333(3) 0.5262(3) 0.120(4) Uani 0.5 1 d . . P A 1 H30A H 0.7241 0.7240 0.5334 0.180 Uiso 0.5 1 calc R U P A 1 H30B H 0.6735 0.7777 0.5285 0.180 Uiso 0.5 1 calc R U P A 1 H30C H 0.6834 0.7235 0.5085 0.180 Uiso 0.5 1 calc R U P A 1 C31 C 0.5656(4) 0.7028(4) 0.5523(3) 0.159(6) Uani 0.5 1 d D . P A 2 H31A H 0.5343 0.6760 0.5444 0.239 Uiso 0.5 1 calc R U P A 2 H31B H 0.5535 0.7467 0.5504 0.239 Uiso 0.5 1 calc R U P A 2 H31C H 0.5682 0.6926 0.5700 0.239 Uiso 0.5 1 calc R U P A 2 C32 C 0.6721(4) 0.7377(3) 0.55017(17) 0.084(2) Uani 0.5 1 d D . P A 2 H32A H 0.6804 0.7277 0.5676 0.125 Uiso 0.5 1 calc R U P A 2 H32B H 0.6527 0.7791 0.5491 0.125 Uiso 0.5 1 calc R U P A 2 H32C H 0.7115 0.7377 0.5409 0.125 Uiso 0.5 1 calc R U P A 2 C33 C 0.6228(9) 0.7033(4) 0.51157(18) 0.211(9) Uani 0.5 1 d D . P A 2 H33A H 0.5914 0.6745 0.5049 0.317 Uiso 0.5 1 calc R U P A 2 H33B H 0.6628 0.6962 0.5032 0.317 Uiso 0.5 1 calc R U P A 2 H33C H 0.6093 0.7465 0.5088 0.317 Uiso 0.5 1 calc R U P A 2 C41 C 0.8530(5) 0.6171(5) 0.5794(2) 0.1435(17) Uiso 0.5 1 d D . P B -3 H41A H 0.8934 0.6005 0.5740 0.215 Uiso 0.5 1 calc R U P B -3 H41B H 0.8595 0.6559 0.5887 0.215 Uiso 0.5 1 calc R U P B -3 H41C H 0.8268 0.6256 0.5648 0.215 Uiso 0.5 1 calc R U P B -3 C42 C 0.8211(5) 0.5701(5) 0.5956(2) 0.1435(17) Uiso 0.5 1 d D . P B -3 H42A H 0.8136 0.5316 0.5859 0.172 Uiso 0.5 1 calc R U P B -3 H42B H 0.8493 0.5593 0.6095 0.172 Uiso 0.5 1 calc R U P B -3 C43 C 0.7602(5) 0.5921(5) 0.6060(2) 0.1435(17) Uiso 0.5 1 d D . P B -3 H43A H 0.7337 0.6068 0.5922 0.172 Uiso 0.5 1 calc R U P B -3 H43B H 0.7685 0.6286 0.6168 0.172 Uiso 0.5 1 calc R U P B -3 C44 C 0.7231(5) 0.5443(5) 0.6209(3) 0.1435(17) Uiso 0.5 1 d D . P B -3 H44A H 0.7453 0.5350 0.6366 0.172 Uiso 0.5 1 calc R U P B -3 H44B H 0.7196 0.5050 0.6113 0.172 Uiso 0.5 1 calc R U P B -3 C45 C 0.6540(4) 0.5707(5) 0.6270(3) 0.1435(17) Uiso 0.5 1 d D . P B -3 H45A H 0.6572 0.6095 0.6370 0.215 Uiso 0.5 1 calc R U P B -3 H45B H 0.6318 0.5807 0.6114 0.215 Uiso 0.5 1 calc R U P B -3 C46 C 0.6182(5) 0.5213(5) 0.6414(2) 0.1435(17) Uiso 0.5 1 d D . P B -3 H46A H 0.5763 0.5369 0.6453 0.215 Uiso 0.5 1 calc R U P B -3 H46B H 0.6405 0.5117 0.6568 0.215 Uiso 0.5 1 calc R U P B -3 H46C H 0.6147 0.4833 0.6314 0.215 Uiso 0.5 1 calc R U P B -3 C71 C 0.643(2) 0.888(3) 0.6303(13) 0.260(13) Uiso 0.25 1 d D . P C -4 H71A H 0.6632 0.9280 0.6339 0.389 Uiso 0.25 1 calc R U P C -4 H71B H 0.6712 0.8616 0.6206 0.389 Uiso 0.25 1 calc R U P C -4 H71C H 0.6328 0.8668 0.6459 0.389 Uiso 0.25 1 calc R U P C -4 C72 C 0.5828(19) 0.8995(14) 0.6156(9) 0.260(13) Uiso 0.25 1 d D . P C -4 H72A H 0.5925 0.9105 0.5982 0.311 Uiso 0.25 1 calc R U P C -4 H72B H 0.5584 0.9339 0.6231 0.311 Uiso 0.25 1 calc R U P C -4 C73 C 0.5452(15) 0.8366(15) 0.6168(8) 0.260(13) Uiso 0.25 1 d D . P C -4 H73A H 0.5061 0.8443 0.6261 0.389 Uiso 0.25 1 d R U P C -4 H73B H 0.5347 0.8193 0.6003 0.389 Uiso 0.25 1 d R U P C -4 C61 C 0.6283(16) 0.8032(10) 0.6286(7) 0.211(8) Uiso 0.25 1 d D . P D 5 H61A H 0.6038 0.8419 0.6287 0.317 Uiso 0.25 1 calc R U P D 5 H61B H 0.6509 0.7996 0.6129 0.317 Uiso 0.25 1 calc R U P D 5 H61C H 0.6583 0.8041 0.6424 0.317 Uiso 0.25 1 calc R U P D 5 C62 C 0.5847(13) 0.7474(12) 0.6317(6) 0.211(8) Uiso 0.25 1 d D . P D 5 H62A H 0.5488 0.7524 0.6203 0.254 Uiso 0.25 1 calc R U P D 5 H62B H 0.5680 0.7473 0.6488 0.254 Uiso 0.25 1 calc R U P D 5 C63 C 0.6157(11) 0.6843(10) 0.6266(7) 0.211(8) Uiso 0.25 1 d D . P D 5 H63A H 0.6415 0.6870 0.6115 0.254 Uiso 0.25 1 calc R U P D 5 H63B H 0.6433 0.6730 0.6407 0.254 Uiso 0.25 1 calc R U P D 5 C51 C 0.8607(13) 0.6263(12) 0.6030(6) 0.196(5) Uiso 0.25 1 d D . P E -6 H51A H 0.8668 0.6634 0.5926 0.294 Uiso 0.25 1 calc R U P E -6 H51B H 0.8920 0.5947 0.5986 0.294 Uiso 0.25 1 calc R U P E -6 H51C H 0.8653 0.6377 0.6205 0.294 Uiso 0.25 1 calc R U P E -6 C52 C 0.7960(12) 0.6001(10) 0.5986(6) 0.196(5) Uiso 0.25 1 d D . P E -6 H52A H 0.7880 0.5970 0.5806 0.235 Uiso 0.25 1 calc R U P E -6 H52B H 0.7644 0.6286 0.6058 0.235 Uiso 0.25 1 calc R U P E -6 C53 C 0.7897(11) 0.5344(10) 0.6106(6) 0.196(5) Uiso 0.25 1 d D . P E -6 H53A H 0.7951 0.5372 0.6288 0.235 Uiso 0.25 1 calc R U P E -6 H53B H 0.7480 0.5164 0.6071 0.235 Uiso 0.25 1 calc R U P E -6 C54 C 0.8416(14) 0.4931(11) 0.5992(5) 0.196(5) Uiso 0.25 1 d D . P E -6 H54A H 0.8248 0.4714 0.5844 0.235 Uiso 0.25 1 calc R U P E -6 H54B H 0.8766 0.5201 0.5937 0.235 Uiso 0.25 1 calc R U P E -6 C55 C 0.8651(13) 0.4470(11) 0.6165(5) 0.196(5) Uiso 0.25 1 d D . P E -6 H55A H 0.8304 0.4394 0.6283 0.235 Uiso 0.25 1 calc R U P E -6 H55B H 0.8980 0.4687 0.6261 0.235 Uiso 0.25 1 calc R U P E -6 C56 C 0.8908(15) 0.3848(11) 0.6109(7) 0.196(5) Uiso 0.25 1 d D . P E -6 H56A H 0.9277 0.3773 0.6212 0.294 Uiso 0.25 1 calc R U P E -6 H56B H 0.9026 0.3829 0.5934 0.294 Uiso 0.25 1 calc R U P E -6 H56C H 0.8592 0.3528 0.6144 0.294 Uiso 0.25 1 calc R U P E -6 C81 C 1.0846(9) 0.7346(11) 0.5459(5) 0.156(4) Uiso 0.25 1 d D . P F -7 H81A H 1.1270 0.7353 0.5528 0.234 Uiso 0.25 1 calc R U P F -7 H81B H 1.0868 0.7334 0.5278 0.234 Uiso 0.25 1 calc R U P F -7 H81C H 1.0625 0.6976 0.5520 0.234 Uiso 0.25 1 calc R U P F -7 C82 C 1.0489(11) 0.7947(12) 0.5543(9) 0.156(4) Uiso 0.25 1 d D . P F -7 H82A H 1.0502 0.7998 0.5725 0.187 Uiso 0.25 1 calc R U P F -7 H82B H 1.0663 0.8325 0.5463 0.187 Uiso 0.25 1 calc R U P F -7 C83 C 0.9825(8) 0.7810(10) 0.5452(6) 0.156(4) Uiso 0.25 1 d D . P F -7 H83A H 0.9774 0.7935 0.5276 0.187 Uiso 0.25 1 calc R U P F -7 H83B H 0.9513 0.8035 0.5553 0.187 Uiso 0.25 1 calc R U P F -7 C84 C 0.9748(9) 0.7082(11) 0.5482(7) 0.156(4) Uiso 0.25 1 d D . P F -7 H84A H 0.9997 0.6863 0.5354 0.187 Uiso 0.25 1 calc R U P F -7 H84B H 0.9900 0.6950 0.5647 0.187 Uiso 0.25 1 calc R U P F -7 C85 C 0.9044(9) 0.6914(11) 0.5453(5) 0.156(4) Uiso 0.25 1 d D . P F -7 H85A H 0.8791 0.7296 0.5477 0.187 Uiso 0.25 1 calc R U P F -7 H85B H 0.8970 0.6761 0.5282 0.187 Uiso 0.25 1 calc R U P F -7 C86 C 0.8829(11) 0.6425(11) 0.5633(5) 0.156(4) Uiso 0.25 1 d D . P F -7 H86A H 0.8373 0.6388 0.5625 0.234 Uiso 0.25 1 calc R U P F -7 H86B H 0.8955 0.6545 0.5801 0.234 Uiso 0.25 1 calc R U P F -7 H86C H 0.9020 0.6023 0.5591 0.234 Uiso 0.25 1 calc R U P F -7 C91 C 1.0302(12) 0.8537(8) 0.5452(5) 0.139(5) Uiso 0.25 1 d D . P G 8 H91A H 1.0458 0.8930 0.5522 0.208 Uiso 0.25 1 calc R U P G 8 H91B H 0.9853 0.8502 0.5483 0.208 Uiso 0.25 1 calc R U P G 8 H91C H 1.0378 0.8531 0.5273 0.208 Uiso 0.25 1 calc R U P G 8 C92 C 1.0641(11) 0.7989(9) 0.5573(6) 0.139(5) Uiso 0.25 1 d D . P G 8 H92A H 1.0565 0.7978 0.5754 0.167 Uiso 0.25 1 calc R U P G 8 H92B H 1.1097 0.8011 0.5542 0.167 Uiso 0.25 1 calc R U P G 8 C93 C 1.0342(4) 0.7396(7) 0.5440(5) 0.139(5) Uiso 0.25 1 d D . P G 8 H93A H 1.0488 0.7261 0.5276 0.167 Uiso 0.25 1 d R U P G 8 H93B H 1.0462 0.7081 0.5565 0.167 Uiso 0.25 1 d R U P G 8 C94 C 1.0750(8) 0.8637(7) 0.5525(4) 0.113(3) Uiso 0.25 1 d D . P H 9 H94A H 1.0954 0.8873 0.5392 0.170 Uiso 0.25 1 calc R U P H 9 H94B H 1.1023 0.8294 0.5578 0.170 Uiso 0.25 1 calc R U P H 9 H94C H 1.0669 0.8914 0.5666 0.170 Uiso 0.25 1 calc R U P H 9 C95 C 1.0095(8) 0.8353(6) 0.5425(4) 0.113(3) Uiso 0.25 1 d D . P H 9 H95A H 0.9723 0.8539 0.5505 0.136 Uiso 0.25 1 calc R U P H 9 H95B H 1.0054 0.8365 0.5242 0.136 Uiso 0.25 1 calc R U P H 9 C96 C 1.0264(6) 0.7713(6) 0.5525(5) 0.113(3) Uiso 0.25 1 d D . P H 9 H96A H 1.0604 0.7534 0.5422 0.136 Uiso 0.25 1 calc R U P H 9 H96B H 1.0423 0.7758 0.5696 0.136 Uiso 0.25 1 calc R U P H 9 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 0.0609(19) 0.0567(18) 0.0604(17) -0.0071(14) 0.0057(14) 0.0000(14) C2 0.0554(17) 0.0533(17) 0.0683(18) 0.0003(14) 0.0052(14) -0.0006(14) C3 0.0617(19) 0.0497(17) 0.0662(18) 0.0053(13) 0.0057(14) 0.0018(14) C4 0.0637(19) 0.0485(16) 0.0737(18) 0.0101(14) 0.0091(15) 0.0102(14) C5 0.0598(18) 0.0514(17) 0.0714(18) 0.0102(14) 0.0104(14) 0.0096(14) C6 0.0629(18) 0.0478(16) 0.0611(17) 0.0002(13) 0.0006(14) 0.0039(13) C7 0.0614(18) 0.0487(16) 0.0631(17) 0.0013(13) -0.0032(14) 0.0063(13) C8 0.066(2) 0.0485(17) 0.0739(19) -0.0007(14) -0.0023(15) 0.0113(14) C9 0.0593(18) 0.0582(18) 0.0716(19) -0.0061(15) 0.0021(14) 0.0086(15) C10 0.0610(19) 0.0535(18) 0.0611(17) -0.0041(13) 0.0013(14) 0.0033(14) C11 0.0557(17) 0.0500(17) 0.0635(17) 0.0002(13) 0.0031(14) 0.0049(13) C12 0.0590(18) 0.0468(16) 0.0618(17) 0.0013(13) 0.0018(13) 0.0022(13) C13 0.0588(18) 0.0477(16) 0.0652(17) 0.0048(13) -0.0012(14) 0.0020(13) C14 0.0649(19) 0.0510(17) 0.0726(19) 0.0130(14) 0.0014(15) 0.0033(14) C15 0.0596(19) 0.0574(18) 0.0742(19) 0.0149(15) -0.0031(14) -0.0020(14) C16 0.066(2) 0.0521(18) 0.0752(19) 0.0119(14) -0.0017(15) -0.0050(15) C17 0.083(2) 0.0457(17) 0.080(2) 0.0109(15) -0.0100(17) -0.0025(16) C18 0.088(2) 0.0399(16) 0.092(2) 0.0071(15) -0.0112(19) 0.0060(16) C19 0.071(2) 0.0477(17) 0.084(2) -0.0026(15) -0.0061(16) 0.0063(15) C20 0.069(2) 0.0483(17) 0.0649(18) -0.0019(13) -0.0086(15) 0.0047(14) C21 0.0635(19) 0.0443(15) 0.0640(17) 0.0046(13) -0.0042(14) 0.0038(13) C22 0.068(2) 0.0462(17) 0.0689(18) 0.0042(13) -0.0072(15) -0.0033(14) C23 0.063(2) 0.068(2) 0.094(2) 0.0259(19) 0.0116(17) 0.0049(16) C24 0.078(2) 0.096(3) 0.132(3) 0.043(3) 0.023(2) 0.004(2) C25 0.104(3) 0.082(3) 0.106(3) 0.016(2) 0.040(2) 0.017(2) C26 0.065(2) 0.128(4) 0.128(3) 0.039(3) 0.003(2) 0.015(2) C27 0.106(3) 0.0451(19) 0.128(3) 0.008(2) 0.000(3) 0.0127(19) C28 0.133(9) 0.062(6) 0.162(10) 0.030(6) -0.034(8) 0.043(6) C29 0.139(9) 0.050(5) 0.198(11) -0.037(6) 0.024(8) 0.001(5) C30 0.110(7) 0.044(4) 0.206(11) 0.044(6) 0.007(7) 0.002(4) C31 0.080(6) 0.047(5) 0.35(2) 0.020(8) -0.044(10) 0.008(4) C32 0.116(7) 0.042(4) 0.093(5) 0.010(4) -0.005(5) -0.002(4) C33 0.40(2) 0.048(5) 0.189(12) -0.015(7) -0.210(15) 0.040(10) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C2 127.8(3) . 20_657 ? C2 C1 C10 108.5(2) . . ? C10 C1 C2 123.7(3) . 20_657 ? C1 C2 C1 128.3(3) . 26_566 ? C1 C2 C3 108.6(2) . . ? C1 C2 C3 122.9(3) 26_566 . ? C4 C3 C2 137.2(3) . . ? C4 C3 C11 117.3(3) . . ? C11 C3 C2 105.5(2) . . ? C3 C4 H4 120.3 . . ? C3 C4 C5 119.3(3) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 118.0 . . ? C6 C5 C4 124.0(3) . . ? C6 C5 H5 118.0 . . ? C5 C6 C12 117.3(3) . . ? C5 C6 C13 125.2(3) . . ? C12 C6 C13 117.5(2) . . ? C8 C7 C12 117.2(3) . . ? C8 C7 C20 124.7(3) . . ? C12 C7 C20 118.0(3) . . ? C7 C8 H8 118.1 . . ? C7 C8 C9 123.8(3) . . ? C9 C8 H8 118.1 . . ? C8 C9 H9 120.5 . . ? C10 C9 C8 119.1(3) . . ? C10 C9 H9 120.5 . . ? C9 C10 C1 136.2(3) . . ? C9 C10 C11 117.0(3) . . ? C11 C10 C1 106.7(2) . . ? C10 C11 C3 110.7(3) . . ? C12 C11 C3 124.4(3) . . ? C12 C11 C10 124.9(3) . . ? C7 C12 C6 124.5(3) . . ? C11 C12 C6 117.6(2) . . ? C11 C12 C7 117.9(3) . . ? C14 C13 C6 123.0(2) . . ? C14 C13 C21 118.7(3) . . ? C21 C13 C6 118.3(2) . . ? C13 C14 H14 118.2 . . ? C13 C14 C15 123.6(3) . . ? C15 C14 H14 118.2 . . ? C14 C15 C23 119.4(3) . . ? C16 C15 C14 117.2(3) . . ? C16 C15 C23 123.4(3) . . ? C15 C16 H16 118.7 . . ? C15 C16 C22 122.6(3) . . ? C22 C16 H16 118.7 . . ? C18 C17 H17 119.0 . . ? C18 C17 C22 122.1(3) . . ? C22 C17 H17 119.0 . . ? C17 C18 C19 118.1(3) . . ? C17 C18 C27 121.5(3) . . ? C19 C18 C27 120.4(3) . . ? C18 C19 H19 118.7 . . ? C20 C19 C18 122.6(3) . . ? C20 C19 H19 118.7 . . ? C19 C20 C7 122.6(3) . . ? C19 C20 C21 119.2(3) . . ? C21 C20 C7 118.2(2) . . ? C20 C21 C13 123.3(3) . . ? C22 C21 C13 118.0(3) . . ? C22 C21 C20 118.7(2) . . ? C16 C22 C17 121.0(3) . . ? C16 C22 C21 119.7(3) . . ? C17 C22 C21 119.3(3) . . ? C15 C23 C24 111.2(3) . . ? C25 C23 C15 108.8(3) . . ? C25 C23 C24 107.0(3) . . ? C26 C23 C15 109.4(3) . . ? C26 C23 C24 109.8(3) . . ? C26 C23 C25 110.5(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C18 C27 C30 109.4(4) . . ? C18 C27 C31 113.0(4) . . ? C18 C27 C33 108.0(5) . . ? C28 C27 C18 108.7(5) . . ? C28 C27 C29 116.8(7) . . ? C28 C27 C30 115.4(7) . . ? C29 C27 C18 106.0(4) . . ? C29 C27 C30 99.9(7) . . ? C32 C27 C18 112.0(4) . . ? C32 C27 C31 106.3(6) . . ? C32 C27 C33 109.8(7) . . ? C33 C27 C31 107.6(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? C41 C42 H42A 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C43 C42 C41 114.0(9) . . ? C43 C42 H42A 108.8 . . ? C43 C42 H42B 108.8 . . ? C42 C43 H43A 108.3 . . ? C42 C43 H43B 108.3 . . ? C42 C43 C44 116.1(9) . . ? H43A C43 H43B 107.4 . . ? C44 C43 H43A 108.3 . . ? C44 C43 H43B 108.3 . . ? C43 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C43 C44 C45 110.4(7) . . ? H44A C44 H44B 108.1 . . ? C45 C44 H44A 109.6 . . ? C45 C44 H44B 109.6 . . ? C44 C45 H45A 109.9 . . ? C44 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C46 C45 C44 108.8(8) . . ? C46 C45 H45A 109.9 . . ? C46 C45 H45B 109.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? C71 C72 H72A 110.6 . . ? C71 C72 H72B 110.6 . . ? C71 C72 C73 105.7(14) . . ? H72A C72 H72B 108.7 . . ? C73 C72 H72A 110.6 . . ? C73 C72 H72B 110.6 . . ? C72 C73 H73A 108.2 . . ? C72 C73 H73B 113.7 . . ? H73A C73 H73B 109.1 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? C61 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C61 C62 C63 114.0(17) . . ? H62A C62 H62B 107.6 . . ? C63 C62 H62A 108.7 . . ? C63 C62 H62B 108.7 . . ? C62 C63 H63A 109.7 . . ? C62 C63 H63B 109.7 . . ? C63 C63 C62 109.7(12) 8_666 . ? C63 C63 H63A 109.7 8_666 . ? C63 C63 H63B 109.7 8_666 . ? H63A C63 H63B 108.2 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? C51 C52 H52A 109.6 . . ? C51 C52 H52B 109.6 . . ? C51 C52 C53 110.4(14) . . ? H52A C52 H52B 108.1 . . ? C53 C52 H52A 109.6 . . ? C53 C52 H52B 109.6 . . ? C52 C53 H53A 110.4 . . ? C52 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? C54 C53 C52 106.8(14) . . ? C54 C53 H53A 110.4 . . ? C54 C53 H53B 110.4 . . ? C53 C54 H54A 109.1 . . ? C53 C54 H54B 109.1 . . ? H54A C54 H54B 107.9 . . ? C55 C54 C53 112.3(15) . . ? C55 C54 H54A 109.1 . . ? C55 C54 H54B 109.1 . . ? C54 C55 H55A 105.4 . . ? C54 C55 H55B 105.4 . . ? C54 C55 C56 127.7(19) . . ? H55A C55 H55B 106.0 . . ? C56 C55 H55A 105.4 . . ? C56 C55 H55B 105.4 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? H81A C81 H81B 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? C81 C82 H82A 111.4 . . ? C81 C82 H82B 111.4 . . ? H82A C82 H82B 109.3 . . ? C83 C82 C81 101.8(12) . . ? C83 C82 H82A 111.4 . . ? C83 C82 H82B 111.4 . . ? C82 C83 H83A 110.8 . . ? C82 C83 H83B 110.8 . . ? C82 C83 C84 104.6(12) . . ? H83A C83 H83B 108.9 . . ? C84 C83 H83A 110.8 . . ? C84 C83 H83B 110.8 . . ? C83 C84 H84A 110.0 . . ? C83 C84 H84B 110.0 . . ? H84A C84 H84B 108.3 . . ? C85 C84 C83 108.6(14) . . ? C85 C84 H84A 110.0 . . ? C85 C84 H84B 110.0 . . ? C84 C85 H85A 108.9 . . ? C84 C85 H85B 108.9 . . ? H85A C85 H85B 107.8 . . ? C86 C85 C84 113.2(15) . . ? C86 C85 H85A 108.9 . . ? C86 C85 H85B 108.9 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86B 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? H91A C91 H91B 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C92 C91 H91A 109.5 . . ? C92 C91 H91B 109.5 . . ? C92 C91 H91C 109.5 . . ? C91 C92 H92A 111.1 . . ? C91 C92 H92B 111.1 . . ? C91 C92 C93 103.2(12) . . ? H92A C92 H92B 109.1 . . ? C93 C92 H92A 111.1 . . ? C93 C92 H92B 111.1 . . ? C92 C93 H93A 120.8 . . ? C92 C93 H93B 97.5 . . ? C93 C93 C92 98.8(12) 3_765 . ? C93 C93 H93A 113.0 3_765 . ? C93 C93 H93B 116.7 3_765 . ? H93A C93 H93B 109.4 . . ? H94A C94 H94B 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C95 C94 H94A 109.5 . . ? C95 C94 H94B 109.5 . . ? C95 C94 H94C 109.5 . . ? C94 C95 H95A 113.5 . . ? C94 C95 H95B 113.5 . . ? H95A C95 H95B 110.8 . . ? C96 C95 C94 90.7(9) . . ? C96 C95 H95A 113.5 . . ? C96 C95 H95B 113.5 . . ? C95 C96 H96A 109.1 . . ? C95 C96 H96B 109.1 . . ? C96 C96 C95 112.4(14) 3_765 . ? C96 C96 H96A 109.1 3_765 . ? C96 C96 H96B 109.1 3_765 . ? H96A C96 H96B 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(4) . ? C1 C2 1.469(4) 20_657 ? C1 C10 1.465(4) . ? C2 C1 1.469(4) 26_566 ? C2 C3 1.486(4) . ? C3 C4 1.376(4) . ? C3 C11 1.413(4) . ? C4 H4 0.9500 . ? C4 C5 1.408(4) . ? C5 H5 0.9500 . ? C5 C6 1.385(4) . ? C6 C12 1.433(4) . ? C6 C13 1.470(4) . ? C7 C8 1.401(4) . ? C7 C12 1.420(4) . ? C7 C20 1.470(4) . ? C8 H8 0.9500 . ? C8 C9 1.403(4) . ? C9 H9 0.9500 . ? C9 C10 1.392(4) . ? C10 C11 1.405(4) . ? C11 C12 1.391(4) . ? C13 C14 1.372(4) . ? C13 C21 1.439(4) . ? C14 H14 0.9500 . ? C14 C15 1.414(4) . ? C15 C16 1.366(4) . ? C15 C23 1.540(4) . ? C16 H16 0.9500 . ? C16 C22 1.403(4) . ? C17 H17 0.9500 . ? C17 C18 1.387(5) . ? C17 C22 1.411(4) . ? C18 C19 1.399(4) . ? C18 C27 1.538(4) . ? C19 H19 0.9500 . ? C19 C20 1.389(4) . ? C20 C21 1.433(4) . ? C21 C22 1.426(4) . ? C23 C24 1.544(5) . ? C23 C25 1.523(5) . ? C23 C26 1.522(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.491(8) . ? C27 C29 1.535(6) . ? C27 C30 1.607(9) . ? C27 C31 1.563(8) . ? C27 C32 1.436(6) . ? C27 C33 1.555(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 C42 1.498(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C43 1.496(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.523(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.616(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.521(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C71 C72 1.531(15) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72 C73 1.568(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9899 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C61 C62 1.526(18) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C62 C63 1.529(17) . ? C63 C63 1.521(18) 8_666 ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 C52 1.512(14) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 C53 1.555(14) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 C54 1.548(14) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.450(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C55 C56 1.471(14) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C81 C82 1.560(14) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C82 C83 1.533(14) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C83 C84 1.574(14) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C84 C85 1.557(14) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C85 C86 1.500(14) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C91 C92 1.525(14) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C92 C93 1.593(14) . ? C93 C93 1.528(15) 3_765 ? C93 H93A 0.9821 . ? C93 H93B 0.9882 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C94 C95 1.621(13) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C95 C96 1.516(14) . ? C96 C96 1.452(14) 3_765 ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ?