#------------------------------------------------------------------------------ #$Date: 2020-06-09 06:48:25 +0300 (Tue, 09 Jun 2020) $ #$Revision: 253031 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157534.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_7157534 loop_ _publ_author_name 'Sheppard, Daniel' 'Cameron, Scott A.' 'Tyler, Peter' 'Schw\"orer, Ralf' _publ_section_title ; Comparison of Disaccharide Donors for Heparan Sulfate Synthesis: Uronic Acids vs. their Pyranose Equivalents ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB00671H _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C59 H56 Cl N3 O14 S' _chemical_formula_sum 'C59 H56 Cl N3 O14 S' _chemical_formula_weight 1098.57 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-03-03 deposited with the CCDC. 2020-06-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.5220(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.23660(10) _cell_length_b 35.3229(3) _cell_length_c 14.56840(10) _cell_measurement_reflns_used 26240 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 73.2940 _cell_measurement_theta_min 3.9400 _cell_volume 2682.24(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0856 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 48369 _diffrn_reflns_point_group_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.534 _diffrn_reflns_theta_min 3.944 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.54132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.360 _exptl_crystal_description rod _exptl_crystal_F_000 1152 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.484 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.055 _refine_diff_density_max 0.388 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.047 _refine_ls_abs_structure_details ; Flack x determined using 4408 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.005(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 914 _refine_ls_number_reflns 10328 _refine_ls_number_restraints 68 _refine_ls_restrained_S_all 1.114 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0396 _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^)+(0.0400P)^2^+1.3455P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.1051 _reflns_Friedel_coverage 0.906 _reflns_Friedel_fraction_full 0.954 _reflns_Friedel_fraction_max 0.922 _reflns_number_gt 9914 _reflns_number_total 10328 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00671h2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7157534 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.513 _shelx_estimated_absorpt_t_max 0.918 _shelx_res_file ; TITL DJS-HS17-051b in P2(1) shelx.res created by SHELXL-2016/6 at 14:36:48 on 18-Jul-2017 CELL 1.54184 5.2366 35.3229 14.5684 90.000 95.522 90.000 ZERR 2.00 0.0001 0.0003 0.0001 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S Cl UNIT 118 112 6 28 2 2 MERG 2 ISOR 0.005 O4 O104 SIZE 0.055 0.098 0.484 FMAP 2 PLAN 10 ACTA L.S. 10 TEMP -153.00 WGHT 0.040000 1.345500 FVAR 4.69757 0.50723 C1 1 0.720107 0.708750 0.664403 11.00000 0.02247 0.03641 = 0.02212 0.00042 -0.00036 -0.00140 AFIX 13 H1 2 0.895743 0.711931 0.697000 11.00000 -1.20000 AFIX 0 C2 1 0.550473 0.686210 0.724158 11.00000 0.02309 0.03830 = 0.02045 0.00069 -0.00306 0.00032 AFIX 13 H2 2 0.365920 0.690915 0.702888 11.00000 -1.20000 AFIX 0 C3 1 0.602624 0.643838 0.725616 11.00000 0.02312 0.03743 = 0.02366 0.00442 0.00074 -0.00007 AFIX 13 H3 2 0.771462 0.639120 0.761981 11.00000 -1.20000 AFIX 0 C4 1 0.616715 0.629292 0.627571 11.00000 0.02314 0.02968 = 0.02781 0.00342 0.00086 0.00065 AFIX 13 H4 2 0.448308 0.631175 0.589182 11.00000 -1.20000 AFIX 0 C5 1 0.827148 0.652309 0.587726 11.00000 0.02277 0.03305 = 0.02554 0.00221 -0.00088 -0.00006 AFIX 13 H5 2 0.984489 0.652017 0.632439 11.00000 -1.20000 AFIX 0 C6 1 0.897463 0.639753 0.494616 11.00000 0.02534 0.03680 = 0.02987 -0.00073 0.00537 -0.00516 AFIX 23 H6A 2 0.952924 0.612948 0.496980 11.00000 -1.20000 H6B 2 0.747938 0.642217 0.447968 11.00000 -1.20000 AFIX 0 C7 1 0.823181 0.782101 0.608093 11.00000 0.03355 0.02611 = 0.03698 -0.00400 0.00492 0.00102 C8 1 0.866638 0.784806 0.516726 11.00000 0.06892 0.04306 = 0.04073 -0.00920 0.02016 -0.01578 AFIX 43 H8 2 0.769893 0.769679 0.472041 11.00000 -1.20000 AFIX 0 C9 1 1.049818 0.809348 0.489610 11.00000 0.07646 0.04292 = 0.06986 -0.00500 0.04647 -0.00699 AFIX 43 H9 2 1.074700 0.811233 0.426034 11.00000 -1.20000 AFIX 0 C10 1 1.197933 0.831247 0.552602 11.00000 0.04004 0.02557 = 0.10240 0.01099 0.01369 0.00363 C11 1 1.400875 0.857693 0.521949 11.00000 0.05217 0.03899 = 0.16579 0.03228 0.02169 -0.00223 AFIX 137 H11A 2 1.334970 0.883677 0.519592 11.00000 -1.20000 H11B 2 1.444342 0.850187 0.460587 11.00000 -1.20000 H11C 2 1.554658 0.856331 0.565829 11.00000 -1.20000 AFIX 0 C12 1 1.155607 0.827646 0.644156 11.00000 0.05895 0.03342 = 0.08162 0.00560 -0.02176 -0.01183 AFIX 43 H12 2 1.257072 0.842027 0.689122 11.00000 -1.20000 AFIX 0 C13 1 0.968607 0.803558 0.672435 11.00000 0.05734 0.02984 = 0.04569 -0.00180 -0.01030 -0.00105 AFIX 43 H13 2 0.941227 0.801901 0.735832 11.00000 -1.20000 AFIX 0 C14 1 0.425496 0.720664 0.855352 11.00000 0.03059 0.03857 = 0.02415 0.00095 0.00593 -0.00534 C15 1 0.517806 0.731827 0.951631 11.00000 0.02647 0.04171 = 0.02605 0.00222 0.00394 -0.00775 C16 1 0.741041 0.717451 0.997138 11.00000 0.03424 0.06160 = 0.02868 -0.00365 -0.00105 -0.00039 AFIX 43 H16 2 0.847004 0.700857 0.966218 11.00000 -1.20000 AFIX 0 C17 1 0.809066 0.727522 1.088690 11.00000 0.03774 0.07784 = 0.02799 -0.00213 -0.00417 -0.00617 AFIX 43 H17 2 0.959641 0.717152 1.120689 11.00000 -1.20000 AFIX 0 C18 1 0.661151 0.752204 1.132982 11.00000 0.04420 0.07271 = 0.02502 -0.00832 0.00792 -0.01856 AFIX 43 H18 2 0.709375 0.758947 1.195373 11.00000 -1.20000 AFIX 0 C19 1 0.440997 0.767350 1.086747 11.00000 0.04890 0.05986 = 0.03444 -0.01140 0.00998 -0.00550 AFIX 43 H19 2 0.339229 0.784744 1.117108 11.00000 -1.20000 AFIX 0 C20 1 0.369870 0.757105 0.996450 11.00000 0.03549 0.05047 = 0.03087 -0.00107 0.00588 -0.00468 AFIX 43 H20 2 0.218619 0.767442 0.964844 11.00000 -1.20000 AFIX 0 C21 1 0.504229 0.609836 0.858346 11.00000 0.03838 0.07258 = 0.03890 0.02889 0.00931 0.01213 AFIX 23 H21A 2 0.621596 0.628266 0.891695 11.00000 -1.20000 H21B 2 0.603661 0.586652 0.847915 11.00000 -1.20000 AFIX 0 C22 1 0.292396 0.600337 0.916128 11.00000 0.03330 0.04885 = 0.03184 0.01791 0.00448 0.00649 C23 1 0.196357 0.627650 0.971732 11.00000 0.03504 0.06302 = 0.04354 -0.00389 -0.00068 -0.00784 AFIX 43 H23 2 0.255791 0.652974 0.968328 11.00000 -1.20000 AFIX 0 C24 1 0.018416 0.619176 1.031373 11.00000 0.03955 0.09869 = 0.03126 -0.00585 0.00017 0.01153 AFIX 43 H24 2 -0.044357 0.638492 1.068626 11.00000 -1.20000 AFIX 0 C25 1 -0.069897 0.582571 1.037425 11.00000 0.03981 0.09881 = 0.05605 0.04822 0.01585 0.01966 AFIX 43 H25 2 -0.192119 0.576479 1.079261 11.00000 -1.20000 AFIX 0 C26 1 0.019723 0.555179 0.982828 11.00000 0.06089 0.05414 = 0.12936 0.05129 0.04566 0.01848 AFIX 43 H26 2 -0.040801 0.529929 0.986677 11.00000 -1.20000 AFIX 0 C27 1 0.198361 0.563894 0.921795 11.00000 0.06003 0.04084 = 0.08992 0.01598 0.03174 0.01323 AFIX 43 H27 2 0.256901 0.544631 0.883420 11.00000 -1.20000 AFIX 0 C28 1 1.045552 0.691340 0.407804 11.00000 0.02956 0.03836 = 0.02204 -0.00149 0.00316 0.00090 C29 1 1.272350 0.717568 0.409221 11.00000 0.03037 0.04619 = 0.02679 0.00477 0.00126 -0.00408 AFIX 23 H29A 2 1.431756 0.702460 0.409895 11.00000 -1.20000 H29B 2 1.283065 0.733017 0.466161 11.00000 -1.20000 AFIX 0 PART 1 SAME N101 > C159 N1 3 0.774233 0.534027 0.755916 21.00000 0.09949 0.03404 = 0.03861 0.00431 -0.00637 -0.02002 N2 3 0.816829 0.505258 0.801327 21.00000 0.07088 0.05111 = 0.05269 0.00118 -0.00029 0.00002 N3 3 0.883071 0.481454 0.850511 21.00000 0.10523 0.05895 = 0.06539 0.01687 -0.00386 0.00328 O4 4 0.711174 0.591355 0.634263 21.00000 0.02829 0.03389 = 0.04002 -0.00059 -0.00143 -0.00301 O8 4 0.375098 0.561284 0.540952 21.00000 0.01397 0.03305 = 0.05326 -0.00628 -0.00139 -0.00289 O11 4 0.322459 0.585259 0.345648 21.00000 0.03835 0.06241 = 0.04014 -0.00358 -0.00407 0.01134 O14 4 0.643960 0.581487 0.255876 21.00000 0.05289 0.09934 = 0.09479 -0.03400 0.04503 -0.00937 C30 1 0.506316 0.565437 0.631082 21.00000 0.02156 0.03917 = 0.03834 -0.00220 0.00141 0.00125 AFIX 13 H30 2 0.380910 0.574278 0.674063 21.00000 -1.20000 AFIX 0 C31 1 0.618114 0.527305 0.665775 21.00000 0.03541 0.03700 = 0.05218 0.00960 0.00405 -0.00681 AFIX 13 H31 2 0.478112 0.508616 0.673157 21.00000 -1.20000 AFIX 0 C32 1 0.794114 0.513225 0.596615 21.00000 0.04807 0.03875 = 0.05178 0.00095 0.00390 0.00390 AFIX 13 H32 2 0.925790 0.533439 0.591682 21.00000 -1.20000 AFIX 0 C33 1 0.647955 0.509720 0.501243 21.00000 0.02311 0.02834 = 0.07255 0.00154 0.01621 -0.00368 AFIX 13 H33 2 0.510762 0.490053 0.501832 21.00000 -1.20000 AFIX 0 C34 1 0.531584 0.547624 0.472330 21.00000 0.01932 0.03815 = 0.04391 -0.00059 -0.00085 -0.00025 AFIX 13 H34 2 0.675340 0.566007 0.468372 21.00000 -1.20000 AFIX 0 C35 1 0.374625 0.547564 0.381842 21.00000 0.02946 0.04767 = 0.05781 -0.01296 -0.02031 -0.00032 AFIX 23 H35A 2 0.465757 0.532952 0.337041 21.00000 -1.20000 H35B 2 0.209819 0.534620 0.388638 21.00000 -1.20000 AFIX 0 O9 4 0.930771 0.479937 0.625612 21.00000 0.04144 0.03808 = 0.07671 0.00661 0.00644 -0.00252 C36 1 0.784412 0.446598 0.636727 21.00000 0.06157 0.04992 = 0.06317 0.00177 0.00702 -0.00695 AFIX 23 H36A 2 0.700397 0.438152 0.576419 21.00000 -1.20000 H36B 2 0.649990 0.451546 0.678565 21.00000 -1.20000 AFIX 0 C37 1 0.969194 0.416413 0.677473 21.00000 0.05397 0.04557 = 0.05662 -0.00070 0.00972 0.00241 C38 1 1.217488 0.413237 0.653961 21.00000 0.06769 0.04938 = 0.07340 0.00681 0.02039 0.00183 AFIX 43 H38 2 1.276419 0.430060 0.609697 21.00000 -1.20000 AFIX 0 C39 1 1.381131 0.386006 0.693785 21.00000 0.06490 0.05518 = 0.10305 -0.00199 0.00969 0.00735 AFIX 43 H39 2 1.554405 0.384960 0.679714 21.00000 -1.20000 AFIX 0 C40 1 1.291371 0.360357 0.754082 21.00000 0.09672 0.06975 = 0.06431 0.00325 0.00202 0.02589 AFIX 43 H40 2 1.403974 0.341812 0.782624 21.00000 -1.20000 AFIX 0 C41 1 1.036275 0.361455 0.773459 21.00000 0.13713 0.06702 = 0.07194 0.03042 0.03216 0.02080 AFIX 43 H41 2 0.971436 0.342499 0.811238 21.00000 -1.20000 AFIX 0 C42 1 0.876282 0.390429 0.737300 21.00000 0.08212 0.06589 = 0.08514 0.01625 0.03789 0.01330 AFIX 43 H42 2 0.705308 0.392348 0.753494 21.00000 -1.20000 AFIX 0 C58 1 0.453361 0.597773 0.276292 21.00000 0.04665 0.04928 = 0.05968 -0.03104 0.01872 -0.00719 C59 1 0.387450 0.636753 0.242689 21.00000 0.07922 0.06866 = 0.03861 -0.02380 -0.00741 0.00091 AFIX 137 H59A 2 0.526679 0.654131 0.263888 21.00000 -1.20000 H59B 2 0.228320 0.644975 0.266955 21.00000 -1.20000 H59C 2 0.364018 0.636779 0.175135 21.00000 -1.20000 AFIX 0 PART 2 N101 3 0.623822 0.523735 0.734364 -21.00000 0.06034 0.03275 = 0.04355 0.01279 0.01593 0.00328 N102 3 0.544796 0.495119 0.771468 -21.00000 0.07748 0.06798 = 0.05688 0.00676 0.01134 0.01046 N103 3 0.486979 0.470423 0.817492 -21.00000 0.13510 0.07754 = 0.07121 0.02735 0.02867 0.00210 O104 4 0.661958 0.588656 0.622573 -21.00000 0.01681 0.02322 = 0.02583 0.00217 -0.00288 -0.00156 O108 4 0.327842 0.566738 0.516444 -21.00000 0.01937 0.03268 = 0.03915 -0.00401 -0.00626 0.00620 O111 4 0.310205 0.592159 0.323228 -21.00000 0.03993 0.04246 = 0.03554 -0.00258 0.00182 -0.00101 O114 4 0.605020 0.577442 0.227862 -21.00000 0.18308 0.06918 = 0.10049 -0.02985 0.07859 0.00722 C130 1 0.438830 0.565962 0.609593 -21.00000 0.00719 0.02391 = 0.04333 0.00444 -0.00301 -0.00444 AFIX 13 H130 2 0.310163 0.575408 0.650617 -21.00000 -1.20000 AFIX 0 C131 1 0.511393 0.525264 0.636401 -21.00000 0.02512 0.03143 = 0.04555 0.00916 0.00549 0.00397 AFIX 13 H131 2 0.352773 0.509346 0.629730 -21.00000 -1.20000 AFIX 0 C132 1 0.704012 0.509174 0.573166 -21.00000 0.03685 0.02089 = 0.04830 0.00139 0.00486 0.00087 AFIX 13 H132 2 0.867793 0.523897 0.580773 -21.00000 -1.20000 AFIX 0 C133 1 0.580393 0.512565 0.474667 -21.00000 0.03285 0.02618 = 0.04950 -0.00241 0.00722 0.00118 AFIX 13 H133 2 0.438737 0.493752 0.461876 -21.00000 -1.20000 AFIX 0 C134 1 0.489888 0.552581 0.449875 -21.00000 0.01845 0.01750 = 0.04635 0.00409 0.00231 0.00116 AFIX 13 H134 2 0.641876 0.569591 0.447803 -21.00000 -1.20000 AFIX 0 C135 1 0.329393 0.553591 0.357668 -21.00000 0.01970 0.04087 = 0.04401 -0.00936 -0.01217 0.00277 AFIX 23 H13A 2 0.409142 0.537340 0.312979 -21.00000 -1.20000 H13B 2 0.155709 0.543609 0.364726 -21.00000 -1.20000 AFIX 0 O109 4 0.749739 0.470643 0.599356 -21.00000 0.02891 0.02094 = 0.07056 0.00530 0.00453 0.00114 C136 1 1.006012 0.456698 0.594704 -21.00000 0.05820 0.04673 = 0.05299 0.00855 0.01102 0.01313 AFIX 23 H13C 2 1.130058 0.477773 0.605100 -21.00000 -1.20000 H13D 2 1.022465 0.446041 0.532699 -21.00000 -1.20000 AFIX 0 C137 1 1.065783 0.426242 0.667511 -21.00000 0.02923 0.05006 = 0.05026 -0.00038 0.00264 0.00552 C138 1 1.120757 0.390047 0.640528 -21.00000 0.05583 0.05242 = 0.04616 -0.00320 0.01436 0.00749 AFIX 43 H138 2 1.126920 0.384433 0.577006 -21.00000 -1.20000 AFIX 0 C139 1 1.167276 0.361694 0.706197 -21.00000 0.07346 0.04793 = 0.06601 -0.00070 0.01001 0.01266 AFIX 43 H139 2 1.206671 0.336714 0.687928 -21.00000 -1.20000 AFIX 0 C140 1 1.155429 0.370368 0.800239 -21.00000 0.04922 0.07631 = 0.04884 0.01272 -0.00139 0.01480 AFIX 43 H140 2 1.189286 0.351347 0.845893 -21.00000 -1.20000 AFIX 0 C141 1 1.094637 0.406483 0.825292 -21.00000 0.04849 0.07413 = 0.04227 -0.00712 0.00009 0.00606 AFIX 43 H141 2 1.083830 0.412421 0.888401 -21.00000 -1.20000 AFIX 0 C142 1 1.049112 0.434230 0.758771 -21.00000 0.04954 0.05192 = 0.04495 -0.00835 0.00412 0.00497 AFIX 43 H142 2 1.005783 0.459114 0.776551 -21.00000 -1.20000 AFIX 0 C158 1 0.477321 0.601096 0.261515 -21.00000 0.04715 0.11784 = 0.04879 -0.01913 0.02313 -0.03688 C159 1 0.431041 0.641173 0.231621 -21.00000 0.05584 0.08853 = 0.04812 0.00851 -0.00931 -0.03025 AFIX 137 H15A 2 0.509265 0.658295 0.279253 -21.00000 -1.20000 H15B 2 0.245986 0.645923 0.222249 -21.00000 -1.20000 H15C 2 0.507514 0.645589 0.173753 -21.00000 -1.20000 AFIX 0 PART 0 C43 1 0.798433 0.468087 0.386140 11.00000 0.02990 0.03375 = 0.07175 -0.01153 0.01085 -0.00559 C44 1 1.052624 0.428281 0.302315 11.00000 0.04257 0.03164 = 0.04610 -0.00953 0.00078 0.00023 AFIX 23 H44A 2 0.895963 0.412585 0.302192 11.00000 -1.20000 H44B 2 1.197540 0.414029 0.334451 11.00000 -1.20000 AFIX 0 C45 1 1.107472 0.436627 0.203965 11.00000 0.03290 0.03192 = 0.05073 -0.00243 0.00425 -0.00279 AFIX 13 H45 2 1.261349 0.453330 0.202924 11.00000 -1.20000 AFIX 0 C46 1 1.147660 0.399457 0.155135 11.00000 0.03161 0.03777 = 0.04302 -0.00060 0.00946 -0.00242 C47 1 1.335199 0.372557 0.175019 11.00000 0.04460 0.04633 = 0.05342 -0.00254 0.00052 0.00632 AFIX 43 H47 2 1.463575 0.376131 0.224930 11.00000 -1.20000 AFIX 0 C48 1 1.333988 0.340005 0.120862 11.00000 0.05084 0.04398 = 0.05897 -0.00193 0.01520 0.00725 AFIX 43 H48 2 1.464400 0.321491 0.133139 11.00000 -1.20000 AFIX 0 C49 1 1.144599 0.334527 0.049586 11.00000 0.05180 0.04340 = 0.05388 -0.01114 0.01773 -0.00123 AFIX 43 H49 2 1.144270 0.312023 0.013868 11.00000 -1.20000 AFIX 0 C50 1 0.954313 0.361460 0.029299 11.00000 0.04115 0.05686 = 0.04759 -0.01081 0.00603 -0.00484 AFIX 43 H50 2 0.824770 0.357639 -0.020107 11.00000 -1.20000 AFIX 0 C51 1 0.956948 0.394288 0.082919 11.00000 0.03102 0.04127 = 0.04281 -0.00075 0.01109 -0.00296 C52 1 0.790624 0.427890 0.076694 11.00000 0.02994 0.04690 = 0.04525 0.00649 0.00589 -0.00163 C53 1 0.579055 0.436757 0.016577 11.00000 0.04430 0.06208 = 0.05240 0.00045 -0.00265 0.00162 AFIX 43 H53 2 0.518123 0.419509 -0.030567 11.00000 -1.20000 AFIX 0 C54 1 0.456930 0.471071 0.025861 11.00000 0.05026 0.06266 = 0.06064 0.01495 -0.00606 0.00980 AFIX 43 H54 2 0.309449 0.477188 -0.014568 11.00000 -1.20000 AFIX 0 C55 1 0.547705 0.496705 0.093728 11.00000 0.04712 0.04264 = 0.06950 0.01830 0.00983 0.00626 AFIX 43 H55 2 0.463483 0.520337 0.098632 11.00000 -1.20000 AFIX 0 C56 1 0.760490 0.488023 0.154375 11.00000 0.04510 0.03279 = 0.05736 0.00736 0.01220 -0.00164 AFIX 43 H56 2 0.823086 0.505552 0.200635 11.00000 -1.20000 AFIX 0 C57 1 0.880314 0.453268 0.146261 11.00000 0.03559 0.03451 = 0.04765 0.00613 0.00927 -0.00331 O1 4 0.734484 0.690503 0.577501 11.00000 0.03191 0.03088 = 0.02184 0.00159 0.00004 -0.00172 O2 4 0.604345 0.699353 0.817747 11.00000 0.02632 0.04380 = 0.02027 -0.00008 -0.00151 0.00033 O3 4 0.406736 0.625619 0.770700 11.00000 0.02688 0.04104 = 0.02700 0.00970 0.00431 -0.00089 O5 4 1.104951 0.663874 0.470923 11.00000 0.02192 0.04075 = 0.02697 0.00382 0.00135 -0.00209 O6 4 0.220437 0.728897 0.816571 11.00000 0.02773 0.05654 = 0.03086 -0.00456 -0.00424 0.00492 O7 4 0.848641 0.694047 0.360857 11.00000 0.02765 0.05605 = 0.03223 0.00566 -0.00539 -0.00444 O10 4 0.806709 0.502542 0.425651 11.00000 0.04669 0.03240 = 0.08579 -0.01750 0.03381 -0.01323 O12 4 0.624562 0.446428 0.384823 11.00000 0.03728 0.03634 = 0.14171 -0.02443 0.02754 -0.01228 O13 4 1.017042 0.463817 0.350191 11.00000 0.03369 0.03241 = 0.05369 -0.01201 0.00701 -0.00472 S1 5 0.568983 0.754195 0.644216 11.00000 0.03052 0.03497 = 0.03146 0.00229 0.00145 0.00180 CL1 6 1.246876 0.747898 0.311723 11.00000 0.04606 0.05519 = 0.03181 0.01256 0.00133 -0.00774 HKLF 4 REM DJS-HS17-051b in P2(1) REM R1 = 0.0396 for 9914 Fo > 4sig(Fo) and 0.0415 for all 10328 data REM 914 parameters refined using 68 restraints END WGHT 0.0400 1.3474 REM Highest difference peak 0.388, deepest hole -0.269, 1-sigma level 0.047 Q1 1 1.0763 0.5316 0.7762 11.00000 0.05 0.39 Q2 1 0.7240 0.7303 0.4141 11.00000 0.05 0.17 Q3 1 1.3733 0.3704 0.3216 11.00000 0.05 0.17 Q4 1 1.3466 0.4781 0.2898 11.00000 0.05 0.17 Q5 1 0.6409 0.7539 1.3199 11.00000 0.05 0.17 Q6 1 0.3070 0.5787 0.9415 11.00000 0.05 0.17 Q7 1 0.4051 0.5881 0.7224 11.00000 0.05 0.16 Q8 1 0.2601 0.6696 0.8257 11.00000 0.05 0.16 Q9 1 0.5397 0.6692 0.9646 11.00000 0.05 0.16 Q10 1 0.8594 0.6896 0.2635 11.00000 0.05 0.16 ; _shelx_res_checksum 54420 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7201(7) 0.70875(10) 0.6644(2) 0.0272(7) Uani 1 1 d . . . . . H1 H 0.895743 0.711931 0.697000 0.033 Uiso 1 1 calc R U . . . C2 C 0.5505(7) 0.68621(10) 0.7242(2) 0.0276(7) Uani 1 1 d . . . . . H2 H 0.365920 0.690915 0.702888 0.033 Uiso 1 1 calc R U . . . C3 C 0.6026(7) 0.64384(10) 0.7256(2) 0.0282(7) Uani 1 1 d . . . . . H3 H 0.771462 0.639120 0.761981 0.034 Uiso 1 1 calc R U . . . C4 C 0.6167(7) 0.62929(9) 0.6276(2) 0.0270(7) Uani 1 1 d . . . . . H4 H 0.448308 0.631175 0.589182 0.032 Uiso 1 1 calc R U . A 1 C5 C 0.8271(7) 0.65231(10) 0.5877(2) 0.0273(7) Uani 1 1 d . . . . . H5 H 0.984489 0.652017 0.632439 0.033 Uiso 1 1 calc R U . . . C6 C 0.8975(7) 0.63975(11) 0.4946(2) 0.0305(7) Uani 1 1 d . . . . . H6A H 0.952924 0.612948 0.496980 0.037 Uiso 1 1 calc R U . . . H6B H 0.747938 0.642217 0.447968 0.037 Uiso 1 1 calc R U . . . C7 C 0.8232(8) 0.78210(10) 0.6081(3) 0.0321(8) Uani 1 1 d . . . . . C8 C 0.8666(10) 0.78481(13) 0.5167(3) 0.0499(11) Uani 1 1 d . . . . . H8 H 0.769893 0.769679 0.472041 0.060 Uiso 1 1 calc R U . . . C9 C 1.0498(12) 0.80935(13) 0.4896(4) 0.0605(14) Uani 1 1 d . . . . . H9 H 1.074700 0.811233 0.426034 0.073 Uiso 1 1 calc R U . . . C10 C 1.1979(9) 0.83125(11) 0.5526(4) 0.0556(13) Uani 1 1 d . . . . . C11 C 1.4009(11) 0.85769(15) 0.5219(6) 0.085(2) Uani 1 1 d . . . . . H11A H 1.334970 0.883677 0.519592 0.102 Uiso 1 1 calc R U . . . H11B H 1.444342 0.850187 0.460587 0.102 Uiso 1 1 calc R U . . . H11C H 1.554658 0.856331 0.565829 0.102 Uiso 1 1 calc R U . . . C12 C 1.1556(11) 0.82765(12) 0.6442(4) 0.0598(14) Uani 1 1 d . . . . . H12 H 1.257072 0.842027 0.689122 0.072 Uiso 1 1 calc R U . . . C13 C 0.9686(9) 0.80356(11) 0.6724(3) 0.0453(10) Uani 1 1 d . . . . . H13 H 0.941227 0.801901 0.735832 0.054 Uiso 1 1 calc R U . . . C14 C 0.4255(7) 0.72066(11) 0.8554(2) 0.0309(7) Uani 1 1 d . . . . . C15 C 0.5178(7) 0.73183(11) 0.9516(2) 0.0313(7) Uani 1 1 d . . . . . C16 C 0.7410(8) 0.71745(13) 0.9971(3) 0.0418(9) Uani 1 1 d . . . . . H16 H 0.847004 0.700857 0.966218 0.050 Uiso 1 1 calc R U . . . C17 C 0.8091(9) 0.72752(15) 1.0887(3) 0.0483(11) Uani 1 1 d . . . . . H17 H 0.959641 0.717152 1.120689 0.058 Uiso 1 1 calc R U . . . C18 C 0.6612(8) 0.75220(15) 1.1330(2) 0.0470(10) Uani 1 1 d . . . . . H18 H 0.709375 0.758947 1.195373 0.056 Uiso 1 1 calc R U . . . C19 C 0.4410(9) 0.76735(14) 1.0867(3) 0.0473(10) Uani 1 1 d . . . . . H19 H 0.339229 0.784744 1.117108 0.057 Uiso 1 1 calc R U . . . C20 C 0.3699(8) 0.75710(12) 0.9965(2) 0.0388(8) Uani 1 1 d . . . . . H20 H 0.218619 0.767442 0.964844 0.047 Uiso 1 1 calc R U . . . C21 C 0.5042(9) 0.60984(15) 0.8583(3) 0.0496(11) Uani 1 1 d . . . . . H21A H 0.621596 0.628266 0.891695 0.060 Uiso 1 1 calc R U . . . H21B H 0.603661 0.586652 0.847915 0.060 Uiso 1 1 calc R U . . . C22 C 0.2924(8) 0.60034(12) 0.9161(3) 0.0379(9) Uani 1 1 d . . . . . C23 C 0.1964(9) 0.62765(15) 0.9717(3) 0.0475(10) Uani 1 1 d . . . . . H23 H 0.255791 0.652974 0.968328 0.057 Uiso 1 1 calc R U . . . C24 C 0.0184(9) 0.61918(17) 1.0314(3) 0.0567(13) Uani 1 1 d . . . . . H24 H -0.044357 0.638492 1.068626 0.068 Uiso 1 1 calc R U . . . C25 C -0.0699(10) 0.58257(18) 1.0374(4) 0.0642(16) Uani 1 1 d . . . . . H25 H -0.192119 0.576479 1.079261 0.077 Uiso 1 1 calc R U . . . C26 C 0.0197(11) 0.55518(16) 0.9828(5) 0.079(2) Uani 1 1 d . . . . . H26 H -0.040801 0.529929 0.986677 0.095 Uiso 1 1 calc R U . . . C27 C 0.1984(11) 0.56389(14) 0.9218(4) 0.0620(14) Uani 1 1 d . . . . . H27 H 0.256901 0.544631 0.883420 0.074 Uiso 1 1 calc R U . . . C28 C 1.0456(7) 0.69134(11) 0.4078(2) 0.0299(7) Uani 1 1 d . . . . . C29 C 1.2724(7) 0.71757(11) 0.4092(2) 0.0345(8) Uani 1 1 d . . . . . H29A H 1.431756 0.702460 0.409895 0.041 Uiso 1 1 calc R U . . . H29B H 1.283065 0.733017 0.466161 0.041 Uiso 1 1 calc R U . . . N1 N 0.774(3) 0.5340(2) 0.7559(5) 0.058(3) Uani 0.507(5) 1 d D . P B 1 N2 N 0.8168(19) 0.5053(2) 0.8013(6) 0.059(2) Uani 0.507(5) 1 d D . P B 1 N3 N 0.883(2) 0.4815(3) 0.8505(7) 0.077(3) Uani 0.507(5) 1 d D . P B 1 O4 O 0.711(3) 0.5914(5) 0.6343(14) 0.034(3) Uani 0.507(5) 1 d D U P B 1 O8 O 0.375(3) 0.5613(4) 0.5410(10) 0.034(3) Uani 0.507(5) 1 d D . P B 1 O11 O 0.322(5) 0.5853(7) 0.3456(13) 0.047(4) Uani 0.507(5) 1 d D . P B 1 O14 O 0.644(3) 0.5815(6) 0.2559(15) 0.080(5) Uani 0.507(5) 1 d D . P B 1 C30 C 0.506(3) 0.5654(4) 0.6311(13) 0.033(4) Uani 0.507(5) 1 d D . P B 1 H30 H 0.380910 0.574278 0.674063 0.040 Uiso 0.507(5) 1 calc R U P B 1 C31 C 0.618(2) 0.5273(3) 0.6658(8) 0.042(2) Uani 0.507(5) 1 d D . P B 1 H31 H 0.478112 0.508616 0.673157 0.050 Uiso 0.507(5) 1 calc R U P B 1 C32 C 0.794(3) 0.5132(3) 0.5966(10) 0.046(4) Uani 0.507(5) 1 d D . P B 1 H32 H 0.925790 0.533439 0.591682 0.056 Uiso 0.507(5) 1 calc R U P B 1 C33 C 0.648(3) 0.5097(5) 0.5012(12) 0.041(5) Uani 0.507(5) 1 d D . P B 1 H33 H 0.510762 0.490053 0.501832 0.049 Uiso 0.507(5) 1 calc R U P B 1 C34 C 0.532(5) 0.5476(6) 0.4723(12) 0.034(4) Uani 0.507(5) 1 d D . P B 1 H34 H 0.675340 0.566007 0.468372 0.041 Uiso 0.507(5) 1 calc R U P B 1 C35 C 0.375(4) 0.5476(6) 0.3818(13) 0.047(5) Uani 0.507(5) 1 d D . P B 1 H35A H 0.465757 0.532952 0.337041 0.056 Uiso 0.507(5) 1 calc R U P B 1 H35B H 0.209819 0.534620 0.388638 0.056 Uiso 0.507(5) 1 calc R U P B 1 O9 O 0.9308(14) 0.47994(18) 0.6256(5) 0.0520(17) Uani 0.507(5) 1 d D . P B 1 C36 C 0.784(2) 0.4466(3) 0.6367(8) 0.058(3) Uani 0.507(5) 1 d D . P B 1 H36A H 0.700397 0.438152 0.576419 0.070 Uiso 0.507(5) 1 calc R U P B 1 H36B H 0.649990 0.451546 0.678565 0.070 Uiso 0.507(5) 1 calc R U P B 1 C37 C 0.969(3) 0.4164(4) 0.6775(9) 0.052(3) Uani 0.507(5) 1 d D . P B 1 C38 C 1.217(2) 0.4132(3) 0.6540(9) 0.063(3) Uani 0.507(5) 1 d D . P B 1 H38 H 1.276419 0.430060 0.609697 0.075 Uiso 0.507(5) 1 calc R U P B 1 C39 C 1.381(2) 0.3860(3) 0.6938(10) 0.074(3) Uani 0.507(5) 1 d D . P B 1 H39 H 1.554405 0.384960 0.679714 0.089 Uiso 0.507(5) 1 calc R U P B 1 C40 C 1.291(3) 0.3604(4) 0.7541(11) 0.077(4) Uani 0.507(5) 1 d D . P B 1 H40 H 1.403974 0.341812 0.782624 0.093 Uiso 0.507(5) 1 calc R U P B 1 C41 C 1.036(4) 0.3615(5) 0.7735(13) 0.091(6) Uani 0.507(5) 1 d D . P B 1 H41 H 0.971436 0.342499 0.811238 0.109 Uiso 0.507(5) 1 calc R U P B 1 C42 C 0.876(3) 0.3904(3) 0.7373(9) 0.076(4) Uani 0.507(5) 1 d D . P B 1 H42 H 0.705308 0.392348 0.753494 0.091 Uiso 0.507(5) 1 calc R U P B 1 C58 C 0.453(5) 0.5978(5) 0.276(2) 0.051(6) Uani 0.507(5) 1 d D . P B 1 C59 C 0.387(6) 0.6368(5) 0.2427(18) 0.063(7) Uani 0.507(5) 1 d D . P B 1 H59A H 0.526679 0.654131 0.263888 0.076 Uiso 0.507(5) 1 calc R U P B 1 H59B H 0.228320 0.644975 0.266955 0.076 Uiso 0.507(5) 1 calc R U P B 1 H59C H 0.364018 0.636779 0.175135 0.076 Uiso 0.507(5) 1 calc R U P B 1 N101 N 0.624(2) 0.5237(2) 0.7344(7) 0.0448(19) Uani 0.493(5) 1 d D . P B 2 N102 N 0.545(2) 0.4951(3) 0.7715(6) 0.067(3) Uani 0.493(5) 1 d D . P B 2 N103 N 0.487(3) 0.4704(3) 0.8175(8) 0.093(4) Uani 0.493(5) 1 d D . P B 2 O104 O 0.662(3) 0.5887(5) 0.6226(12) 0.022(2) Uani 0.493(5) 1 d D U P B 2 O108 O 0.328(3) 0.5667(5) 0.5164(10) 0.031(3) Uani 0.493(5) 1 d D . P B 2 O111 O 0.310(4) 0.5922(6) 0.3232(12) 0.039(3) Uani 0.493(5) 1 d D . P B 2 O114 O 0.605(5) 0.5774(7) 0.2279(16) 0.113(10) Uani 0.493(5) 1 d D . P B 2 C130 C 0.439(3) 0.5660(4) 0.6096(12) 0.025(3) Uani 0.493(5) 1 d D . P B 2 H130 H 0.310163 0.575408 0.650617 0.030 Uiso 0.493(5) 1 calc R U P B 2 C131 C 0.511(2) 0.5253(3) 0.6364(8) 0.034(2) Uani 0.493(5) 1 d D . P B 2 H131 H 0.352773 0.509346 0.629730 0.041 Uiso 0.493(5) 1 calc R U P B 2 C132 C 0.704(3) 0.5092(3) 0.5732(10) 0.035(3) Uani 0.493(5) 1 d D . P B 2 H132 H 0.867793 0.523897 0.580773 0.042 Uiso 0.493(5) 1 calc R U P B 2 C133 C 0.580(4) 0.5126(5) 0.4747(13) 0.036(3) Uani 0.493(5) 1 d D . P B 2 H133 H 0.438737 0.493752 0.461876 0.043 Uiso 0.493(5) 1 calc R U P B 2 C134 C 0.490(4) 0.5526(6) 0.4499(11) 0.027(4) Uani 0.493(5) 1 d D . P B 2 H134 H 0.641876 0.569591 0.447803 0.033 Uiso 0.493(5) 1 calc R U P B 2 C135 C 0.329(4) 0.5536(6) 0.3577(12) 0.036(3) Uani 0.493(5) 1 d D . P B 2 H13A H 0.409142 0.537340 0.312979 0.043 Uiso 0.493(5) 1 calc R U P B 2 H13B H 0.155709 0.543609 0.364726 0.043 Uiso 0.493(5) 1 calc R U P B 2 O109 O 0.7497(11) 0.47064(15) 0.5994(5) 0.0402(15) Uani 0.493(5) 1 d D . P B 2 C136 C 1.006(2) 0.4567(3) 0.5947(7) 0.052(2) Uani 0.493(5) 1 d D . P B 2 H13C H 1.130058 0.477773 0.605100 0.063 Uiso 0.493(5) 1 calc R U P B 2 H13D H 1.022465 0.446041 0.532699 0.063 Uiso 0.493(5) 1 calc R U P B 2 C137 C 1.066(3) 0.4262(3) 0.6675(9) 0.043(3) Uani 0.493(5) 1 d D . P B 2 C138 C 1.121(2) 0.3900(3) 0.6405(7) 0.051(2) Uani 0.493(5) 1 d D . P B 2 H138 H 1.126920 0.384433 0.577006 0.061 Uiso 0.493(5) 1 calc R U P B 2 C139 C 1.167(3) 0.3617(3) 0.7062(9) 0.062(3) Uani 0.493(5) 1 d D . P B 2 H139 H 1.206671 0.336714 0.687928 0.075 Uiso 0.493(5) 1 calc R U P B 2 C140 C 1.155(3) 0.3704(4) 0.8002(10) 0.059(4) Uani 0.493(5) 1 d D . P B 2 H140 H 1.189286 0.351347 0.845893 0.070 Uiso 0.493(5) 1 calc R U P B 2 C141 C 1.095(2) 0.4065(3) 0.8253(7) 0.055(3) Uani 0.493(5) 1 d D . P B 2 H141 H 1.083830 0.412421 0.888401 0.066 Uiso 0.493(5) 1 calc R U P B 2 C142 C 1.0491(19) 0.4342(3) 0.7588(6) 0.049(2) Uani 0.493(5) 1 d D . P B 2 H142 H 1.005783 0.459114 0.776551 0.059 Uiso 0.493(5) 1 calc R U P B 2 C158 C 0.477(7) 0.6011(8) 0.262(3) 0.070(9) Uani 0.493(5) 1 d D . P B 2 C159 C 0.431(7) 0.6412(7) 0.232(2) 0.065(7) Uani 0.493(5) 1 d D . P B 2 H15A H 0.509265 0.658295 0.279253 0.078 Uiso 0.493(5) 1 calc R U P B 2 H15B H 0.245986 0.645923 0.222249 0.078 Uiso 0.493(5) 1 calc R U P B 2 H15C H 0.507514 0.645589 0.173753 0.078 Uiso 0.493(5) 1 calc R U P B 2 C43 C 0.7984(8) 0.46809(12) 0.3861(3) 0.0447(10) Uani 1 1 d . . . . . C44 C 1.0526(9) 0.42828(11) 0.3023(3) 0.0403(9) Uani 1 1 d . . . . . H44A H 0.895963 0.412585 0.302192 0.048 Uiso 1 1 calc R U . . . H44B H 1.197540 0.414029 0.334451 0.048 Uiso 1 1 calc R U . . . C45 C 1.1075(8) 0.43663(11) 0.2040(3) 0.0385(9) Uani 1 1 d . . . . . H45 H 1.261349 0.453330 0.202924 0.046 Uiso 1 1 calc R U . . . C46 C 1.1477(8) 0.39946(11) 0.1551(3) 0.0371(8) Uani 1 1 d . . . . . C47 C 1.3352(9) 0.37256(13) 0.1750(3) 0.0484(11) Uani 1 1 d . . . . . H47 H 1.463575 0.376131 0.224930 0.058 Uiso 1 1 calc R U . . . C48 C 1.3340(10) 0.34000(13) 0.1209(3) 0.0506(11) Uani 1 1 d . . . . . H48 H 1.464400 0.321491 0.133139 0.061 Uiso 1 1 calc R U . . . C49 C 1.1446(10) 0.33453(13) 0.0496(3) 0.0489(11) Uani 1 1 d . . . . . H49 H 1.144270 0.312023 0.013868 0.059 Uiso 1 1 calc R U . . . C50 C 0.9543(9) 0.36146(14) 0.0293(3) 0.0484(10) Uani 1 1 d . . . . . H50 H 0.824770 0.357639 -0.020107 0.058 Uiso 1 1 calc R U . . . C51 C 0.9569(8) 0.39429(12) 0.0829(3) 0.0379(8) Uani 1 1 d . . . . . C52 C 0.7906(8) 0.42789(12) 0.0767(3) 0.0405(9) Uani 1 1 d . . . . . C53 C 0.5791(10) 0.43676(15) 0.0166(3) 0.0534(11) Uani 1 1 d . . . . . H53 H 0.518123 0.419509 -0.030567 0.064 Uiso 1 1 calc R U . . . C54 C 0.4569(10) 0.47107(15) 0.0259(4) 0.0586(13) Uani 1 1 d . . . . . H54 H 0.309449 0.477188 -0.014568 0.070 Uiso 1 1 calc R U . . . C55 C 0.5477(10) 0.49671(13) 0.0937(4) 0.0528(11) Uani 1 1 d . . . . . H55 H 0.463483 0.520337 0.098632 0.063 Uiso 1 1 calc R U . . . C56 C 0.7605(9) 0.48802(11) 0.1544(3) 0.0446(10) Uani 1 1 d . . . . . H56 H 0.823086 0.505552 0.200635 0.054 Uiso 1 1 calc R U . . . C57 C 0.8803(8) 0.45327(11) 0.1463(3) 0.0389(9) Uani 1 1 d . . . . . O1 O 0.7345(5) 0.69050(7) 0.57750(15) 0.0284(5) Uani 1 1 d . . . . . O2 O 0.6043(5) 0.69935(7) 0.81775(15) 0.0304(5) Uani 1 1 d . . . . . O3 O 0.4067(5) 0.62562(7) 0.77070(16) 0.0315(5) Uani 1 1 d . . . . . O5 O 1.1050(5) 0.66387(7) 0.47092(16) 0.0299(5) Uani 1 1 d . . . . . O6 O 0.2204(5) 0.72890(8) 0.81657(18) 0.0388(6) Uani 1 1 d . . . . . O7 O 0.8486(5) 0.69405(9) 0.36086(18) 0.0392(6) Uani 1 1 d . . . . . O10 O 0.8067(6) 0.50254(8) 0.4257(3) 0.0532(9) Uani 1 1 d . . . . . O12 O 0.6246(6) 0.44643(9) 0.3848(3) 0.0705(12) Uani 1 1 d . . . . . O13 O 1.0170(5) 0.46382(7) 0.3502(2) 0.0397(6) Uani 1 1 d . . . . . S1 S 0.56898(17) 0.75420(2) 0.64422(6) 0.03241(19) Uani 1 1 d . . . . . Cl1 Cl 1.2469(2) 0.74790(3) 0.31172(6) 0.0445(2) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0225(17) 0.0364(17) 0.0221(15) 0.0004(12) -0.0004(13) -0.0014(13) C2 0.0231(17) 0.0383(18) 0.0205(15) 0.0007(13) -0.0031(13) 0.0003(14) C3 0.0231(17) 0.0374(17) 0.0237(15) 0.0044(13) 0.0007(13) -0.0001(14) C4 0.0231(17) 0.0297(16) 0.0278(16) 0.0034(13) 0.0009(13) 0.0007(13) C5 0.0228(17) 0.0330(17) 0.0255(16) 0.0022(13) -0.0009(13) -0.0001(13) C6 0.0253(17) 0.0368(17) 0.0299(17) -0.0007(14) 0.0054(14) -0.0052(14) C7 0.034(2) 0.0261(16) 0.0370(18) -0.0040(14) 0.0049(16) 0.0010(14) C8 0.069(3) 0.043(2) 0.041(2) -0.0092(18) 0.020(2) -0.016(2) C9 0.076(4) 0.043(2) 0.070(3) -0.005(2) 0.046(3) -0.007(2) C10 0.040(3) 0.0256(18) 0.102(4) 0.011(2) 0.014(3) 0.0036(17) C11 0.052(3) 0.039(2) 0.166(7) 0.032(3) 0.022(4) -0.002(2) C12 0.059(3) 0.033(2) 0.082(4) 0.006(2) -0.022(3) -0.012(2) C13 0.057(3) 0.0298(19) 0.046(2) -0.0018(16) -0.010(2) -0.0010(18) C14 0.0306(19) 0.0386(18) 0.0242(15) 0.0009(13) 0.0059(14) -0.0053(15) C15 0.0265(18) 0.0417(19) 0.0260(16) 0.0022(14) 0.0039(14) -0.0077(14) C16 0.034(2) 0.062(3) 0.0287(18) -0.0037(17) -0.0011(16) -0.0004(18) C17 0.038(2) 0.078(3) 0.0280(19) -0.0021(19) -0.0042(17) -0.006(2) C18 0.044(2) 0.073(3) 0.0250(16) -0.008(2) 0.0079(16) -0.019(2) C19 0.049(3) 0.060(3) 0.034(2) -0.0114(18) 0.0100(19) -0.005(2) C20 0.035(2) 0.050(2) 0.0309(17) -0.0011(16) 0.0059(15) -0.0047(18) C21 0.038(2) 0.073(3) 0.039(2) 0.029(2) 0.0093(18) 0.012(2) C22 0.033(2) 0.049(2) 0.0318(18) 0.0179(16) 0.0045(16) 0.0065(17) C23 0.035(2) 0.063(3) 0.044(2) -0.0039(19) -0.0007(18) -0.008(2) C24 0.040(3) 0.099(4) 0.031(2) -0.006(2) 0.0002(19) 0.012(3) C25 0.040(3) 0.099(4) 0.056(3) 0.048(3) 0.016(2) 0.020(3) C26 0.061(3) 0.054(3) 0.129(6) 0.051(3) 0.046(4) 0.018(3) C27 0.060(3) 0.041(2) 0.090(4) 0.016(2) 0.032(3) 0.013(2) C28 0.0296(18) 0.0384(18) 0.0220(15) -0.0015(13) 0.0032(14) 0.0009(15) C29 0.030(2) 0.046(2) 0.0268(16) 0.0048(15) 0.0013(15) -0.0041(16) N1 0.099(8) 0.034(4) 0.039(4) 0.004(3) -0.006(5) -0.020(5) N2 0.071(6) 0.051(5) 0.053(5) 0.001(4) 0.000(4) 0.000(4) N3 0.105(9) 0.059(5) 0.065(6) 0.017(5) -0.004(6) 0.003(5) O4 0.028(6) 0.034(4) 0.040(6) -0.001(3) -0.001(4) -0.003(4) O8 0.014(5) 0.033(5) 0.053(9) -0.006(5) -0.001(5) -0.003(4) O11 0.038(5) 0.062(11) 0.040(8) -0.004(6) -0.004(5) 0.011(5) O14 0.053(6) 0.099(10) 0.095(12) -0.034(7) 0.045(6) -0.009(6) C30 0.022(8) 0.039(5) 0.038(7) -0.002(4) 0.001(6) 0.001(5) C31 0.035(6) 0.037(4) 0.052(8) 0.010(4) 0.004(5) -0.007(4) C32 0.048(8) 0.039(6) 0.052(7) 0.001(5) 0.004(6) 0.004(5) C33 0.023(8) 0.028(5) 0.073(14) 0.002(7) 0.016(8) -0.004(5) C34 0.019(7) 0.038(9) 0.044(8) -0.001(6) -0.001(6) 0.000(5) C35 0.029(9) 0.048(8) 0.058(11) -0.013(7) -0.020(7) 0.000(6) O9 0.041(4) 0.038(3) 0.077(5) 0.007(3) 0.006(3) -0.003(3) C36 0.062(7) 0.050(6) 0.063(6) 0.002(5) 0.007(5) -0.007(5) C37 0.054(8) 0.046(6) 0.057(6) -0.001(5) 0.010(6) 0.002(6) C38 0.068(8) 0.049(6) 0.073(7) 0.007(5) 0.020(6) 0.002(6) C39 0.065(8) 0.055(6) 0.103(10) -0.002(6) 0.010(7) 0.007(5) C40 0.097(12) 0.070(8) 0.064(8) 0.003(6) 0.002(8) 0.026(8) C41 0.137(18) 0.067(9) 0.072(11) 0.030(8) 0.032(11) 0.021(11) C42 0.082(9) 0.066(7) 0.085(8) 0.016(6) 0.038(7) 0.013(6) C58 0.047(12) 0.049(7) 0.060(13) -0.031(7) 0.019(8) -0.007(7) C59 0.079(18) 0.069(12) 0.039(9) -0.024(8) -0.007(8) 0.001(11) N101 0.060(6) 0.033(4) 0.044(5) 0.013(4) 0.016(4) 0.003(4) N102 0.077(7) 0.068(6) 0.057(5) 0.007(5) 0.011(5) 0.010(5) N103 0.135(12) 0.078(7) 0.071(7) 0.027(6) 0.029(7) 0.002(7) O104 0.017(5) 0.023(4) 0.026(4) 0.002(3) -0.003(3) -0.002(3) O108 0.019(5) 0.033(5) 0.039(6) -0.004(4) -0.006(4) 0.006(3) O111 0.040(6) 0.042(7) 0.036(8) -0.003(5) 0.002(6) -0.001(4) O114 0.18(2) 0.069(8) 0.100(15) -0.030(9) 0.079(14) 0.007(10) C130 0.007(6) 0.024(4) 0.043(10) 0.004(4) -0.003(5) -0.004(4) C131 0.025(5) 0.031(4) 0.046(6) 0.009(4) 0.005(4) 0.004(4) C132 0.037(7) 0.021(4) 0.048(9) 0.001(4) 0.005(6) 0.001(4) C133 0.033(10) 0.026(5) 0.050(7) -0.002(5) 0.007(6) 0.001(5) C134 0.018(8) 0.018(5) 0.046(8) 0.004(5) 0.002(7) 0.001(4) C135 0.020(7) 0.041(8) 0.044(8) -0.009(6) -0.012(6) 0.003(5) O109 0.029(3) 0.021(3) 0.071(4) 0.005(3) 0.005(3) 0.001(2) C136 0.058(6) 0.047(5) 0.053(5) 0.009(4) 0.011(5) 0.013(5) C137 0.029(6) 0.050(7) 0.050(6) 0.000(5) 0.003(5) 0.006(5) C138 0.056(6) 0.052(6) 0.046(5) -0.003(4) 0.014(5) 0.007(5) C139 0.073(8) 0.048(6) 0.066(8) -0.001(5) 0.010(7) 0.013(5) C140 0.049(7) 0.076(9) 0.049(7) 0.013(6) -0.001(6) 0.015(6) C141 0.048(6) 0.074(7) 0.042(5) -0.007(4) 0.000(4) 0.006(5) C142 0.050(6) 0.052(5) 0.045(5) -0.008(4) 0.004(4) 0.005(4) C158 0.047(13) 0.12(2) 0.049(9) -0.019(9) 0.023(8) -0.037(13) C159 0.056(11) 0.089(13) 0.048(11) 0.009(8) -0.009(8) -0.030(9) C43 0.030(2) 0.0337(19) 0.072(3) -0.0115(19) 0.011(2) -0.0056(16) C44 0.043(2) 0.0316(18) 0.046(2) -0.0095(16) 0.0008(18) 0.0002(16) C45 0.033(2) 0.0319(18) 0.051(2) -0.0024(16) 0.0043(18) -0.0028(15) C46 0.032(2) 0.0378(19) 0.043(2) -0.0006(16) 0.0095(17) -0.0024(16) C47 0.045(3) 0.046(2) 0.053(3) -0.0025(19) 0.001(2) 0.0063(19) C48 0.051(3) 0.044(2) 0.059(3) -0.002(2) 0.015(2) 0.007(2) C49 0.052(3) 0.043(2) 0.054(3) -0.0111(19) 0.018(2) -0.001(2) C50 0.041(2) 0.057(3) 0.048(2) -0.011(2) 0.006(2) -0.005(2) C51 0.031(2) 0.041(2) 0.043(2) -0.0007(16) 0.0111(17) -0.0030(16) C52 0.030(2) 0.047(2) 0.045(2) 0.0065(18) 0.0059(18) -0.0016(17) C53 0.044(3) 0.062(3) 0.052(3) 0.000(2) -0.003(2) 0.002(2) C54 0.050(3) 0.063(3) 0.061(3) 0.015(2) -0.006(2) 0.010(2) C55 0.047(3) 0.043(2) 0.069(3) 0.018(2) 0.010(2) 0.006(2) C56 0.045(3) 0.0328(19) 0.057(3) 0.0074(18) 0.012(2) -0.0016(17) C57 0.036(2) 0.0345(19) 0.048(2) 0.0061(16) 0.0093(18) -0.0033(16) O1 0.0319(13) 0.0309(12) 0.0218(11) 0.0016(9) 0.0000(9) -0.0017(10) O2 0.0263(13) 0.0438(14) 0.0203(11) -0.0001(10) -0.0015(9) 0.0003(10) O3 0.0269(13) 0.0410(13) 0.0270(12) 0.0097(10) 0.0043(10) -0.0009(11) O5 0.0219(12) 0.0407(14) 0.0270(12) 0.0038(10) 0.0013(10) -0.0021(10) O6 0.0277(14) 0.0565(17) 0.0309(13) -0.0046(12) -0.0042(11) 0.0049(12) O7 0.0277(14) 0.0561(16) 0.0322(13) 0.0057(12) -0.0054(11) -0.0044(12) O10 0.0467(18) 0.0324(14) 0.086(2) -0.0175(14) 0.0338(17) -0.0132(12) O12 0.0373(19) 0.0363(16) 0.142(4) -0.024(2) 0.028(2) -0.0123(14) O13 0.0337(15) 0.0324(13) 0.0537(17) -0.0120(12) 0.0070(13) -0.0047(11) S1 0.0305(4) 0.0350(4) 0.0315(4) 0.0023(3) 0.0015(3) 0.0018(4) Cl1 0.0461(5) 0.0552(6) 0.0318(4) 0.0126(4) 0.0013(4) -0.0077(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 O1 C1 C2 110.7(3) . . ? O1 C1 S1 108.5(2) . . ? C2 C1 S1 106.7(2) . . ? O2 C2 C3 106.6(3) . . ? O2 C2 C1 107.4(3) . . ? C3 C2 C1 114.1(3) . . ? O3 C3 C2 108.3(3) . . ? O3 C3 C4 112.4(3) . . ? C2 C3 C4 110.1(3) . . ? O4 C4 C3 107.4(8) . . ? O104 C4 C3 113.6(7) . . ? O4 C4 C5 105.5(8) . . ? O104 C4 C5 112.2(7) . . ? C3 C4 C5 106.1(3) . . ? O1 C5 C6 107.0(3) . . ? O1 C5 C4 106.9(3) . . ? C6 C5 C4 115.7(3) . . ? O5 C6 C5 107.2(3) . . ? C8 C7 C13 119.2(4) . . ? C8 C7 S1 121.6(3) . . ? C13 C7 S1 119.0(3) . . ? C7 C8 C9 120.4(4) . . ? C8 C9 C10 121.6(5) . . ? C12 C10 C9 117.3(4) . . ? C12 C10 C11 121.7(6) . . ? C9 C10 C11 121.0(6) . . ? C10 C12 C13 121.8(4) . . ? C7 C13 C12 119.7(4) . . ? O6 C14 O2 124.4(3) . . ? O6 C14 C15 124.9(4) . . ? O2 C14 C15 110.6(3) . . ? C16 C15 C20 119.7(3) . . ? C16 C15 C14 122.4(4) . . ? C20 C15 C14 117.9(3) . . ? C15 C16 C17 119.4(4) . . ? C18 C17 C16 120.7(4) . . ? C17 C18 C19 119.9(4) . . ? C20 C19 C18 119.8(4) . . ? C19 C20 C15 120.4(4) . . ? O3 C21 C22 111.5(3) . . ? C27 C22 C23 117.5(4) . . ? C27 C22 C21 122.0(4) . . ? C23 C22 C21 120.3(4) . . ? C24 C23 C22 121.8(5) . . ? C23 C24 C25 120.0(5) . . ? C26 C25 C24 119.4(5) . . ? C25 C26 C27 120.5(5) . . ? C22 C27 C26 120.7(5) . . ? O7 C28 O5 125.5(3) . . ? O7 C28 C29 126.9(3) . . ? O5 C28 C29 107.6(3) . . ? C28 C29 Cl1 111.2(2) . . ? N2 N1 C31 113.5(8) . . ? N3 N2 N1 170.2(12) . . ? C30 O4 C4 110.5(13) . . ? C30 O8 C34 114.7(13) . . ? C58 O11 C35 118.8(18) . . ? O4 C30 O8 113.2(15) . . ? O4 C30 C31 107.1(13) . . ? O8 C30 C31 110.3(12) . . ? N1 C31 C32 108.7(10) . . ? N1 C31 C30 108.0(9) . . ? C32 C31 C30 107.9(10) . . ? O9 C32 C31 113.3(11) . . ? O9 C32 C33 113.5(11) . . ? C31 C32 C33 110.4(11) . . ? O10 C33 C34 100.7(12) . . ? O10 C33 C32 115.3(13) . . ? C34 C33 C32 109.6(12) . . ? O8 C34 C35 108.3(16) . . ? O8 C34 C33 110.2(14) . . ? C35 C34 C33 114.8(16) . . ? O11 C35 C34 113.0(15) . . ? C32 O9 C36 117.2(9) . . ? O9 C36 C37 107.2(9) . . ? C38 C37 C42 119.9(11) . . ? C38 C37 C36 122.6(11) . . ? C42 C37 C36 117.4(11) . . ? C39 C38 C37 121.0(11) . . ? C40 C39 C38 119.4(12) . . ? C39 C40 C41 120.3(13) . . ? C40 C41 C42 119.8(14) . . ? C37 C42 C41 119.3(12) . . ? O14 C58 O11 121(2) . . ? O14 C58 C59 122(2) . . ? O11 C58 C59 115.5(15) . . ? N102 N101 C131 109.3(10) . . ? N103 N102 N101 170.5(13) . . ? C130 O104 C4 115.4(13) . . ? C130 O108 C134 115.0(12) . . ? C158 O111 C135 114.9(18) . . ? O104 C130 O108 111.9(14) . . ? O104 C130 C131 108.5(12) . . ? O108 C130 C131 109.3(10) . . ? N101 C131 C130 110.1(9) . . ? N101 C131 C132 109.8(9) . . ? C130 C131 C132 110.8(10) . . ? O109 C132 C133 111.9(11) . . ? O109 C132 C131 107.2(9) . . ? C133 C132 C131 107.0(12) . . ? O10 C133 C132 98.5(11) . . ? O10 C133 C134 110.6(15) . . ? C132 C133 C134 113.0(12) . . ? O108 C134 C135 106.1(14) . . ? O108 C134 C133 110.7(15) . . ? C135 C134 C133 111.4(14) . . ? O111 C135 C134 110.0(14) . . ? C132 O109 C136 116.6(8) . . ? O109 C136 C137 109.9(9) . . ? C142 C137 C138 120.2(10) . . ? C142 C137 C136 120.2(10) . . ? C138 C137 C136 119.5(11) . . ? C137 C138 C139 120.0(10) . . ? C138 C139 C140 119.4(10) . . ? C141 C140 C139 119.5(12) . . ? C140 C141 C142 120.1(10) . . ? C137 C142 C141 120.8(9) . . ? O114 C158 O111 122(2) . . ? O114 C158 C159 128(2) . . ? O111 C158 C159 109(2) . . ? O12 C43 O13 128.0(4) . . ? O12 C43 O10 125.6(4) . . ? O13 C43 O10 106.3(3) . . ? O13 C44 C45 109.2(3) . . ? C57 C45 C44 113.0(4) . . ? C57 C45 C46 102.3(3) . . ? C44 C45 C46 108.8(3) . . ? C47 C46 C51 120.9(4) . . ? C47 C46 C45 128.8(4) . . ? C51 C46 C45 110.3(4) . . ? C46 C47 C48 119.1(5) . . ? C49 C48 C47 120.4(4) . . ? C48 C49 C50 120.9(4) . . ? C49 C50 C51 118.8(4) . . ? C46 C51 C50 120.0(4) . . ? C46 C51 C52 108.6(4) . . ? C50 C51 C52 131.4(4) . . ? C53 C52 C57 120.5(4) . . ? C53 C52 C51 131.1(4) . . ? C57 C52 C51 108.5(4) . . ? C52 C53 C54 119.2(5) . . ? C53 C54 C55 120.7(5) . . ? C56 C55 C54 120.5(4) . . ? C55 C56 C57 118.9(5) . . ? C56 C57 C52 120.3(4) . . ? C56 C57 C45 129.5(4) . . ? C52 C57 C45 110.2(3) . . ? C1 O1 C5 112.2(2) . . ? C14 O2 C2 118.7(3) . . ? C3 O3 C21 112.0(3) . . ? C28 O5 C6 117.1(3) . . ? C43 O10 C33 118.8(7) . . ? C43 O10 C133 115.3(8) . . ? C43 O13 C44 116.5(3) . . ? C7 S1 C1 102.29(17) . . ? 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 O1 1.429(4) . ? C1 C2 1.526(5) . ? C1 S1 1.801(4) . ? C2 O2 1.442(4) . ? C2 C3 1.521(5) . ? C3 O3 1.424(4) . ? C3 C4 1.526(5) . ? C4 O4 1.43(2) . ? C4 O104 1.458(17) . ? C4 C5 1.528(5) . ? C5 O1 1.437(4) . ? C5 C6 1.506(5) . ? C6 O5 1.448(4) . ? C7 C8 1.375(6) . ? C7 C13 1.377(5) . ? C7 S1 1.776(4) . ? C8 C9 1.379(7) . ? C9 C10 1.380(8) . ? C10 C12 1.379(8) . ? C10 C11 1.514(7) . ? C12 C13 1.389(7) . ? C14 O6 1.200(5) . ? C14 O2 1.357(5) . ? C14 C15 1.492(5) . ? C15 C16 1.384(6) . ? C15 C20 1.386(6) . ? C16 C17 1.393(5) . ? C17 C18 1.368(7) . ? C18 C19 1.385(7) . ? C19 C20 1.381(5) . ? C21 O3 1.441(4) . ? C21 C22 1.494(6) . ? C22 C27 1.384(7) . ? C22 C23 1.385(6) . ? C23 C24 1.367(7) . ? C24 C25 1.379(8) . ? C25 C26 1.364(9) . ? C26 C27 1.386(8) . ? C28 O7 1.185(4) . ? C28 O5 1.352(4) . ? C28 C29 1.505(5) . ? C29 Cl1 1.774(4) . ? N1 N2 1.221(10) . ? N1 C31 1.498(14) . ? N2 N3 1.137(11) . ? O4 C30 1.408(15) . ? O8 C30 1.430(14) . ? O8 C34 1.436(15) . ? O11 C58 1.349(18) . ? O11 C35 1.448(16) . ? O14 C58 1.214(18) . ? C30 C31 1.535(15) . ? C31 C32 1.513(15) . ? C32 O9 1.419(13) . ? C32 C33 1.525(16) . ? C33 O10 1.464(18) . ? C33 C34 1.514(16) . ? C34 C35 1.485(16) . ? O9 C36 1.423(11) . ? C36 C37 1.521(14) . ? C37 C38 1.381(14) . ? C37 C42 1.386(15) . ? C38 C39 1.379(15) . ? C39 C40 1.376(17) . ? C40 C41 1.39(2) . ? C41 C42 1.394(17) . ? C58 C59 1.491(18) . ? N101 N102 1.236(12) . ? N101 C131 1.492(13) . ? N102 N103 1.158(12) . ? O104 C130 1.415(15) . ? O108 C130 1.424(13) . ? O108 C134 1.438(15) . ? O111 C158 1.35(2) . ? O111 C135 1.452(15) . ? O114 C158 1.20(2) . ? C130 C131 1.528(14) . ? C131 C132 1.539(13) . ? C132 O109 1.428(11) . ? C132 C133 1.521(15) . ? C133 O10 1.484(19) . ? C133 C134 1.523(17) . ? C134 C135 1.515(16) . ? O109 C136 1.437(11) . ? C136 C137 1.522(13) . ? C137 C142 1.370(15) . ? C137 C138 1.376(14) . ? C138 C139 1.390(14) . ? C139 C140 1.411(17) . ? C140 C141 1.373(18) . ? C141 C142 1.383(13) . ? C158 C159 1.49(2) . ? C43 O12 1.188(5) . ? C43 O13 1.313(5) . ? C43 O10 1.345(5) . ? C44 O13 1.457(4) . ? C44 C45 1.517(6) . ? C45 C57 1.508(6) . ? C45 C46 1.518(5) . ? C46 C47 1.377(6) . ? C46 C51 1.391(6) . ? C47 C48 1.394(6) . ? C48 C49 1.379(7) . ? C49 C50 1.389(7) . ? C50 C51 1.397(6) . ? C51 C52 1.470(6) . ? C52 C53 1.381(6) . ? C52 C57 1.400(6) . ? C53 C54 1.383(7) . ? C54 C55 1.390(8) . ? C55 C56 1.388(7) . ? C56 C57 1.389(6) . ?