#------------------------------------------------------------------------------ #$Date: 2020-06-09 06:48:25 +0300 (Tue, 09 Jun 2020) $ #$Revision: 253031 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157535.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_7157535 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 syn _chemical_formula_moiety 'C44 H46 Cl N3 O14' _chemical_formula_sum 'C44 H46 Cl N3 O14' _chemical_formula_weight 876.29 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-03 deposited with the CCDC. 2020-06-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.1104(2) _cell_length_b 19.5548(6) _cell_length_c 27.2321(19) _cell_measurement_reflns_used 17308 _cell_measurement_temperature 164(2) _cell_measurement_theta_max 72.7 _cell_measurement_theta_min 6.7 _cell_volume 4318.9(3) _computing_cell_refinement 'FSProcess (Rigaku, 1998)' _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_data_reduction 'FSProcess (Rigaku, 1998)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 164(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details '551 images in steps of 1\%' _diffrn_measurement_device_details 'Curved image plate' _diffrn_measurement_device_type ; Rigaku Spider ; _diffrn_measurement_method \w-scans _diffrn_radiation_monochromator ; Rigaku VariMax-HF Confocal Optical System ; _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 34329 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 58.931 _diffrn_reflns_theta_max 58.931 _diffrn_reflns_theta_min 6.654 _diffrn_source ; Rigaku MM007 rotating anode ; _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR, Higashi (1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.348 _exptl_crystal_description needle _exptl_crystal_F_000 1840 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Toluene / Petroleum ether' _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.429 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details ; Flack x determined using 1487 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.101(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 528 _refine_ls_number_reflns 6132 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0625 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1173P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1705 _refine_ls_wR_factor_ref 0.1892 _reflns_Friedel_coverage 0.754 _reflns_Friedel_fraction_full 0.987 _reflns_Friedel_fraction_max 0.987 _reflns_number_gt 4550 _reflns_number_total 6132 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00671h2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 4318.9(4) _cod_database_code 7157535 _shelx_shelxl_version_number 2018/3 _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_res_file ; TITL rs71 in P21 21 21 created/ mASSEY PROC. into cell opt 5 shelx.res created by SHELXL-2018/3 at 09:11:30 on 03-Mar-2020 cell 1.54178 8.11035 19.55478 27.23212 90.0000 90.0000 90.0000 ZERR 4.0 0.00023 0.00060 0.00191 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O CL UNIT 176 184 12 56 4 temp -109 L.S. 10 BOND $H FMAP 2 PLAN 20 ACTA CONF HTAB EQIV $1 x-1/2, -y+1/2, -z+1 HTAB O12 O14_$1 REM RESTRAINTS FOR DISORDERED Cl'S SUMP 1.0 0.001 1.0 5 1.0 6 1.0 7 REM PHENYL RINGS EADP C38a C39a C40a C41a C42a EADP C38b C39b c40b c41b c42b EADP C16 C17 C18 REM LINKS TO CL'S EADP o9a o6a o6b o9b EADP c29a c29b SADI c29A CL1A C29B CL1B C29C CL1C SADI c28A c29a c28b c29b c28b c29C SADI C28A o6a C28B o6b SADI O9a c28a o9b c28b REM SADI c36a c42a c36a c38a FREE o9b c29B DELU 0.005 O6a C28a O9a SHEL 12 0.90 OMIT 8 4 9 OMIT 8 4 6 OMIT 8 3 6 OMIT 0 3 13 OMIT 1 4 0 OMIT 4 0 3 OMIT -8 4 6 WGHT 0.117300 FVAR 0.13823 0.42909 0.06396 0.07036 0.58278 0.21074 0.20581 FVAR 0.11634 0.08227 O1 4 0.638723 0.686260 0.499578 11.00000 0.04166 0.06035 = 0.05536 0.00273 -0.00589 -0.00227 O2 4 0.605578 0.800819 0.488336 11.00000 0.05619 0.05400 = 0.06535 0.00023 -0.00193 -0.00662 O3 4 0.456042 0.775784 0.395990 11.00000 0.05252 0.05494 = 0.06043 0.00890 0.00472 0.00057 O4 4 0.565125 0.648432 0.353694 11.00000 0.03395 0.07128 = 0.04849 0.00351 0.00181 0.00170 O5 4 0.524973 0.537582 0.425952 11.00000 0.04332 0.05419 = 0.05559 -0.00405 0.00344 -0.00187 O7 4 0.504342 0.928246 0.667242 11.00000 0.06246 0.08415 = 0.09406 -0.03520 0.01185 -0.01519 O8 4 0.671014 0.830921 0.362674 11.00000 0.06740 0.08984 = 0.09804 0.02912 -0.00206 -0.02133 O10 4 0.710004 0.445780 0.423765 11.00000 0.04461 0.06431 = 0.05777 0.00251 0.00300 0.00464 O11 4 0.263252 0.364019 0.378821 11.00000 0.04734 0.06707 = 0.08892 -0.01995 0.01757 -0.01060 O12 4 0.394348 0.329140 0.473638 11.00000 0.08593 0.08664 = 0.09853 0.01444 0.03475 -0.00753 AFIX 87 H12X 2 0.411561 0.286785 0.473243 11.00000 -1.20000 AFIX 0 O13 4 0.870674 0.400285 0.506254 11.00000 0.09088 0.06423 = 0.08307 0.00319 -0.02654 0.00277 O14 4 0.981689 0.305869 0.537892 11.00000 0.12853 0.07892 = 0.12356 0.04588 -0.03419 0.00759 N1 3 0.376372 0.491474 0.339669 11.00000 0.07899 0.07884 = 0.07156 0.00242 -0.02118 -0.01697 N2 3 0.295913 0.463087 0.307490 11.00000 0.06641 0.08892 = 0.07609 -0.00006 -0.00984 -0.00595 N3 3 0.214037 0.445669 0.275703 11.00000 0.09593 0.14496 = 0.08351 -0.02333 -0.02827 -0.01756 C1 1 0.539602 0.737150 0.475761 11.00000 0.04374 0.04691 = 0.05510 0.00018 -0.01095 -0.00398 AFIX 13 H1 2 0.421004 0.733397 0.485436 11.00000 -1.20000 AFIX 0 C2 1 0.562503 0.728554 0.420574 11.00000 0.04347 0.05678 = 0.05122 0.00500 0.00441 -0.00818 AFIX 13 H2 2 0.679703 0.738380 0.411612 11.00000 -1.20000 AFIX 0 C3 1 0.516794 0.656698 0.403806 11.00000 0.04009 0.06254 = 0.04524 0.00589 0.00232 -0.00027 AFIX 13 H3 2 0.394668 0.650707 0.406460 11.00000 -1.20000 AFIX 0 C4 1 0.601745 0.602104 0.434342 11.00000 0.03503 0.05403 = 0.04586 0.00334 -0.00089 -0.00039 AFIX 13 H4 2 0.721349 0.599661 0.425593 11.00000 -1.20000 AFIX 0 C5 1 0.581882 0.617647 0.489391 11.00000 0.05059 0.05358 = 0.04682 -0.00019 0.00257 -0.01099 AFIX 13 H5 2 0.463500 0.612982 0.499096 11.00000 -1.20000 AFIX 0 C6 1 0.689053 0.570939 0.521356 11.00000 0.09011 0.06422 = 0.04472 -0.00152 -0.00817 0.00395 AFIX 23 H6A 2 0.733711 0.533396 0.500912 11.00000 -1.20000 H6B 2 0.783321 0.597456 0.534426 11.00000 -1.20000 AFIX 0 C7 1 0.570848 0.827213 0.534514 11.00000 0.03971 0.05527 = 0.06602 -0.00896 -0.00821 0.00351 C8 1 0.520500 0.789673 0.574485 11.00000 0.03989 0.05245 = 0.05843 0.00203 -0.00271 -0.00037 AFIX 43 H8 2 0.502439 0.741873 0.571342 11.00000 -1.20000 AFIX 0 C9 1 0.495649 0.822112 0.620165 11.00000 0.03484 0.05880 = 0.07188 -0.00144 -0.00556 -0.00504 AFIX 43 H9 2 0.461622 0.796144 0.647852 11.00000 -1.20000 AFIX 0 C10 1 0.520787 0.891422 0.624536 11.00000 0.03499 0.06808 = 0.07460 -0.01675 -0.00461 -0.00361 C11 1 0.568398 0.928584 0.583999 11.00000 0.04743 0.05464 = 0.10189 -0.01247 -0.00159 -0.00398 AFIX 43 H11 2 0.583347 0.976601 0.586881 11.00000 -1.20000 AFIX 0 C12 1 0.594724 0.897378 0.539358 11.00000 0.04854 0.05538 = 0.07224 0.00238 -0.00928 -0.00570 AFIX 43 H12 2 0.629148 0.923709 0.511892 11.00000 -1.20000 AFIX 0 C13 1 0.458925 0.890456 0.710570 11.00000 0.07783 0.11624 = 0.08983 -0.03967 0.01933 -0.01175 AFIX 137 H13A 2 0.347883 0.871570 0.706393 11.00000 -1.20000 H13B 2 0.460452 0.921008 0.739093 11.00000 -1.20000 H13C 2 0.537536 0.853075 0.715708 11.00000 -1.20000 AFIX 0 C14 1 0.524709 0.821821 0.365067 11.00000 0.06334 0.05978 = 0.07181 0.00095 0.00419 -0.00741 AFIX 66 C15 1 0.397879 0.856196 0.334303 11.00000 0.06953 0.06832 = 0.06031 0.01104 -0.00041 0.00388 C16 1 0.233330 0.836433 0.335821 11.00000 0.08484 0.09391 = 0.15914 0.04057 -0.03597 0.00040 AFIX 43 H16 2 0.198485 0.802335 0.358398 11.00000 -1.20000 AFIX 65 C17 1 0.119764 0.866562 0.304304 11.00000 0.08484 0.09391 = 0.15914 0.04057 -0.03597 0.00040 AFIX 43 H17 2 0.007302 0.853055 0.305341 11.00000 -1.20000 AFIX 65 C18 1 0.170746 0.916453 0.271269 11.00000 0.08484 0.09391 = 0.15914 0.04057 -0.03597 0.00040 AFIX 43 H18 2 0.093128 0.937045 0.249729 11.00000 -1.20000 AFIX 65 C19 1 0.335294 0.936217 0.269751 11.00000 0.10325 0.08940 = 0.08347 0.02479 -0.00352 0.01279 AFIX 43 H19 2 0.370138 0.970315 0.247173 11.00000 -1.20000 AFIX 65 C20 1 0.448862 0.906089 0.301268 11.00000 0.09119 0.07540 = 0.07849 0.01622 0.00582 0.00532 AFIX 43 H20 2 0.561324 0.919596 0.300230 11.00000 -1.20000 AFIX 0 C21 1 0.430705 0.655902 0.318782 11.00000 0.04546 0.07151 = 0.05370 0.00757 -0.00167 0.00260 AFIX 23 H21A 2 0.366992 0.697945 0.325861 11.00000 -1.20000 H21B 2 0.355345 0.616176 0.320817 11.00000 -1.20000 AFIX 0 C22 1 0.507257 0.660046 0.268449 11.00000 0.05745 0.06899 = 0.04674 0.00688 0.00051 0.00570 C23 1 0.486097 0.606475 0.235006 11.00000 0.07857 0.08862 = 0.06367 -0.00837 0.00715 -0.00687 AFIX 43 H23 2 0.424208 0.567320 0.244319 11.00000 -1.20000 AFIX 0 C24 1 0.555192 0.609940 0.187923 11.00000 0.11152 0.14781 = 0.06485 -0.01442 0.01580 -0.00845 AFIX 43 H24 2 0.538824 0.573573 0.165312 11.00000 -1.20000 AFIX 0 C25 1 0.645205 0.665144 0.174738 11.00000 0.10309 0.16198 = 0.05088 0.01290 0.01581 0.00475 AFIX 43 H25 2 0.694985 0.666568 0.143176 11.00000 -1.20000 AFIX 0 C26 1 0.666200 0.720624 0.207186 11.00000 0.09118 0.12313 = 0.06914 0.02618 0.02248 -0.00650 AFIX 43 H26 2 0.724931 0.760379 0.197383 11.00000 -1.20000 AFIX 0 C27 1 0.598217 0.715489 0.254151 11.00000 0.06729 0.08300 = 0.06885 0.00589 0.00992 0.00316 AFIX 43 H27 2 0.615678 0.751623 0.276881 11.00000 -1.20000 AFIX 0 C30 1 0.608283 0.490136 0.396130 11.00000 0.05226 0.06926 = 0.04358 -0.00610 0.00859 0.00770 AFIX 13 H30 2 0.677084 0.515201 0.371541 11.00000 -1.20000 AFIX 0 C31 1 0.479294 0.446406 0.369103 11.00000 0.05776 0.06550 = 0.05198 -0.00368 0.00721 0.00110 AFIX 13 H31 2 0.537867 0.413948 0.346722 11.00000 -1.20000 AFIX 0 C32 1 0.376630 0.405083 0.405826 11.00000 0.04900 0.06529 = 0.06724 -0.00588 0.00545 -0.00639 AFIX 13 H32 2 0.314348 0.437049 0.427678 11.00000 -1.20000 AFIX 0 C33 1 0.489144 0.360857 0.436563 11.00000 0.06729 0.06130 = 0.06518 0.00286 0.01650 -0.00233 AFIX 13 H33 2 0.540281 0.324965 0.415296 11.00000 -1.20000 AFIX 0 C34 1 0.623754 0.403598 0.459924 11.00000 0.06652 0.06319 = 0.05059 0.00866 0.00966 0.00367 AFIX 13 H34 2 0.573899 0.433906 0.485504 11.00000 -1.20000 AFIX 0 C35 1 0.745611 0.358324 0.483213 11.00000 0.07403 0.06873 = 0.06209 0.00307 0.00225 0.00264 AFIX 23 H35A 2 0.691130 0.329178 0.508119 11.00000 -1.20000 H35B 2 0.796597 0.328237 0.458227 11.00000 -1.20000 AFIX 0 PART 1 C36A 1 0.110401 0.358795 0.404493 21.00000 31.00000 AFIX 23 H36A 2 0.058018 0.404429 0.406599 21.00000 -1.20000 H36B 2 0.130441 0.342206 0.438318 21.00000 -1.20000 AFIX 66 C37A 1 -0.000151 0.311174 0.378713 21.00000 41.00000 C38A 1 -0.000081 0.242827 0.392736 21.00000 0.13258 0.09047 = 0.13955 -0.00570 -0.01733 -0.04817 AFIX 43 H38A 2 0.065033 0.228348 0.419807 21.00000 -1.20000 AFIX 65 C39A 1 -0.095284 0.195666 0.367152 21.00000 0.13258 0.09047 = 0.13955 -0.00570 -0.01733 -0.04817 AFIX 43 H39A 2 -0.095235 0.148954 0.376736 21.00000 -1.20000 AFIX 65 C40A 1 -0.190556 0.216852 0.327544 21.00000 0.13258 0.09047 = 0.13955 -0.00570 -0.01733 -0.04817 AFIX 43 H40A 2 -0.255623 0.184619 0.310058 21.00000 -1.20000 AFIX 65 C41A 1 -0.190628 0.285198 0.313520 21.00000 0.13258 0.09047 = 0.13955 -0.00570 -0.01733 -0.04817 AFIX 43 H41A 2 -0.255743 0.299677 0.286450 21.00000 -1.20000 AFIX 65 C42A 1 -0.095426 0.332360 0.339104 21.00000 0.13258 0.09047 = 0.13955 -0.00570 -0.01733 -0.04817 AFIX 43 H42A 2 -0.095475 0.379072 0.329519 21.00000 -1.20000 AFIX 0 PART 2 C36B 1 0.096603 0.377870 0.385876 -21.00000 31.00000 AFIX 23 H36C 2 0.061261 0.415624 0.364062 -21.00000 -1.20000 H36D 2 0.076593 0.391787 0.420318 -21.00000 -1.20000 AFIX 66 C37B 1 0.000989 0.314012 0.374235 -21.00000 41.00000 C38B 1 0.028776 0.255736 0.402265 -21.00000 0.09197 0.09425 = 0.11735 0.00038 -0.00973 -0.03399 AFIX 43 H38B 2 0.107111 0.256717 0.428192 -21.00000 -1.20000 AFIX 65 C39B 1 -0.058052 0.196024 0.392361 -21.00000 0.09197 0.09425 = 0.11735 0.00038 -0.00973 -0.03399 AFIX 43 H39B 2 -0.039061 0.156195 0.411519 -21.00000 -1.20000 AFIX 65 C40B 1 -0.172668 0.194587 0.354426 -21.00000 0.09197 0.09425 = 0.11735 0.00038 -0.00973 -0.03399 AFIX 43 H40B 2 -0.232011 0.153776 0.347657 -21.00000 -1.20000 AFIX 65 C41B 1 -0.200457 0.252863 0.326395 -21.00000 0.09197 0.09425 = 0.11735 0.00038 -0.00973 -0.03399 AFIX 43 H41B 2 -0.278792 0.251880 0.300469 -21.00000 -1.20000 AFIX 65 C42B 1 -0.113630 0.312575 0.336299 -21.00000 0.09197 0.09425 = 0.11735 0.00038 -0.00973 -0.03399 AFIX 43 H42B 2 -0.132622 0.352404 0.317142 -21.00000 -1.20000 AFIX 0 PART 0 C43 1 0.984963 0.367358 0.532859 11.00000 0.09731 0.08911 = 0.05981 0.00702 -0.01272 0.01205 C44 1 1.114543 0.414298 0.551991 11.00000 0.10923 0.10951 = 0.08804 -0.00221 -0.04358 -0.00004 AFIX 137 H44A 2 1.198443 0.387724 0.569500 11.00000 -1.20000 H44B 2 1.064437 0.447386 0.574526 11.00000 -1.20000 H44C 2 1.166008 0.438668 0.524534 11.00000 -1.20000 AFIX 0 part 1 O6A 4 0.601882 0.543868 0.559483 51.00000 0.11236 0.11537 = 0.06704 0.01638 0.01032 -0.00450 O9A 4 0.826907 0.498264 0.593931 51.00000 0.11236 0.11537 = 0.06704 0.01638 0.01032 -0.00450 C28A 1 0.671874 0.503464 0.592709 51.00000 0.10881 0.10149 = 0.03382 -0.00523 0.01922 0.02662 C29A 1 0.576865 0.471219 0.630323 51.00000 81.00000 AFIX 23 H29A 2 0.633599 0.477318 0.662213 51.00000 -1.20000 H29B 2 0.570892 0.421550 0.623514 51.00000 -1.20000 AFIX 0 CL1A 5 0.371855 0.504557 0.635017 51.00000 0.10439 0.12418 = 0.09912 0.00534 0.00506 -0.01331 part 2 O6B 4 0.596766 0.572076 0.570847 -51.00000 0.11236 0.11537 = 0.06704 0.01638 0.01032 -0.00450 O9B 4 0.450153 0.487673 0.558475 -51.00000 0.11236 0.11537 = 0.06704 0.01638 0.01032 -0.00450 C28B 1 0.503519 0.527883 0.588247 -51.00000 0.07119 0.10782 = 0.03851 -0.03628 0.01454 -0.03208 C29B 1 0.469094 0.542593 0.639778 61.00000 81.00000 AFIX 23 H29C 2 0.397052 0.583349 0.641962 61.00000 -1.20000 H29D 2 0.573723 0.553286 0.656856 61.00000 -1.20000 AFIX 0 CL1B 5 0.369268 0.471023 0.670320 61.00000 91.00000 PART 3 C29C 1 0.407746 0.557078 0.634079 71.00000 81.00000 AFIX 1 H29E 2 0.337386 0.589563 0.620405 71.00000 -1.20000 H29F 2 0.492749 0.572641 0.654737 71.00000 -1.20000 AFIX 0 CL1C 5 0.298377 0.483836 0.659247 71.00000 91.00000 HKLF 4 REM rs71 in P21 21 21 created/ mASSEY PROC. into cell opt 5 REM wR2 = 0.1892, GooF = S = 1.095, Restrained GooF = 1.098 for all data REM R1 = 0.0625 for 4550 Fo > 4sig(Fo) and 0.0813 for all 6132 data REM 528 parameters refined using 10 restraints END WGHT 0.1173 0.0000 REM Instructions for potential hydrogen bonds HTAB O12 O14_$1 HTAB C8 O1 HTAB C21 O3 HTAB C21 N1 HTAB C34 O9B HTAB C36A O12 HTAB C36B N2 HTAB C44 O9A EQIV $2 x-1/2, -y+3/2, -z+1 HTAB C29B O8_$2 HTAB C29C O8_$2 REM Highest difference peak 0.429, deepest hole -0.339, 1-sigma level 0.052 Q1 1 0.5454 0.4625 0.5798 11.00000 0.05 0.43 Q2 1 0.5004 0.4230 0.6601 11.00000 0.05 0.31 Q3 1 0.6598 0.5777 0.5775 11.00000 0.05 0.25 Q4 1 0.3961 0.9854 0.3066 11.00000 0.05 0.22 Q5 1 0.6350 0.5031 0.5062 11.00000 0.05 0.22 Q6 1 0.3967 0.5133 0.5419 11.00000 0.05 0.20 Q7 1 0.2120 0.4973 0.6419 11.00000 0.05 0.20 Q8 1 0.5829 0.8151 0.4899 11.00000 0.05 0.20 Q9 1 -0.0020 0.2592 0.3934 11.00000 0.05 0.20 Q10 1 0.4964 0.4277 0.5994 11.00000 0.05 0.19 Q11 1 -0.0711 0.8082 0.2807 11.00000 0.05 0.18 Q12 1 0.5583 0.4835 0.3494 11.00000 0.05 0.17 Q13 1 0.5446 0.5220 0.4258 11.00000 0.05 0.17 Q14 1 0.3490 0.6434 0.4076 11.00000 0.05 0.17 Q15 1 0.5879 0.8935 0.3518 11.00000 0.05 0.17 Q16 1 0.5748 0.8335 0.6038 11.00000 0.05 0.17 Q17 1 0.7761 0.4586 0.5681 11.00000 0.05 0.17 Q18 1 -0.3789 0.2025 0.3171 11.00000 0.05 0.16 Q19 1 0.5717 0.4019 0.3519 11.00000 0.05 0.16 Q20 1 0.5328 0.5921 0.5739 11.00000 0.05 0.16 ; _shelx_res_checksum 7460 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 O1 O 0.6387(5) 0.68626(19) 0.49958(12) 0.0525(10) Uani 1 1 d . . . . . O2 O 0.6056(5) 0.80082(19) 0.48834(13) 0.0585(11) Uani 1 1 d . . . . . O3 O 0.4560(5) 0.77578(19) 0.39599(13) 0.0560(10) Uani 1 1 d . . . . . O4 O 0.5651(4) 0.64843(19) 0.35369(12) 0.0512(10) Uani 1 1 d . . . . . O5 O 0.5250(5) 0.53758(18) 0.42595(12) 0.0510(9) Uani 1 1 d . . . . . O7 O 0.5043(6) 0.9282(2) 0.66724(18) 0.0802(13) Uani 1 1 d . . . . . O8 O 0.6710(7) 0.8309(3) 0.36267(17) 0.0851(15) Uani 1 1 d . . . . . O10 O 0.7100(5) 0.4458(2) 0.42376(13) 0.0556(10) Uani 1 1 d . . . . . O11 O 0.2633(5) 0.3640(2) 0.37882(15) 0.0678(12) Uani 1 1 d . . . . . O12 O 0.3943(7) 0.3291(3) 0.47364(18) 0.0904(16) Uani 1 1 d . . . . . H12X H 0.411561 0.286785 0.473243 0.108 Uiso 1 1 calc R U . . . O13 O 0.8707(6) 0.4003(2) 0.50625(16) 0.0794(14) Uani 1 1 d . . . . . O14 O 0.9817(9) 0.3059(3) 0.53789(19) 0.110(2) Uani 1 1 d . . . . . N1 N 0.3764(8) 0.4915(3) 0.3397(2) 0.0765(16) Uani 1 1 d . . . . . N2 N 0.2959(8) 0.4631(3) 0.3075(2) 0.0771(16) Uani 1 1 d . . . . . N3 N 0.2140(10) 0.4457(4) 0.2757(2) 0.108(2) Uani 1 1 d . . . . . C1 C 0.5396(8) 0.7372(3) 0.47576(18) 0.0486(14) Uani 1 1 d . . . . . H1 H 0.421004 0.733397 0.485436 0.058 Uiso 1 1 calc R U . . . C2 C 0.5625(7) 0.7286(3) 0.42057(19) 0.0505(14) Uani 1 1 d . . . . . H2 H 0.679703 0.738380 0.411612 0.061 Uiso 1 1 calc R U . . . C3 C 0.5168(8) 0.6567(3) 0.40381(17) 0.0493(13) Uani 1 1 d . . . . . H3 H 0.394668 0.650707 0.406460 0.059 Uiso 1 1 calc R U . . . C4 C 0.6017(7) 0.6021(3) 0.43434(18) 0.0450(13) Uani 1 1 d . . . . . H4 H 0.721349 0.599661 0.425593 0.054 Uiso 1 1 calc R U . . . C5 C 0.5819(8) 0.6176(3) 0.48939(18) 0.0503(14) Uani 1 1 d . . . . . H5 H 0.463500 0.612982 0.499096 0.060 Uiso 1 1 calc R U . . . C6 C 0.6891(9) 0.5709(3) 0.5214(2) 0.0663(18) Uani 1 1 d . . . . . H6A H 0.733711 0.533396 0.500912 0.080 Uiso 1 1 calc R U . A 1 H6B H 0.783321 0.597456 0.534426 0.080 Uiso 1 1 calc R U . A 1 C7 C 0.5708(7) 0.8272(3) 0.5345(2) 0.0537(15) Uani 1 1 d . . . . . C8 C 0.5205(7) 0.7897(3) 0.5745(2) 0.0503(13) Uani 1 1 d . . . . . H8 H 0.502439 0.741873 0.571342 0.060 Uiso 1 1 calc R U . . . C9 C 0.4956(7) 0.8221(3) 0.6202(2) 0.0552(14) Uani 1 1 d . . . . . H9 H 0.461622 0.796144 0.647852 0.066 Uiso 1 1 calc R U . . . C10 C 0.5208(7) 0.8914(3) 0.6245(2) 0.0592(15) Uani 1 1 d . . . . . C11 C 0.5684(8) 0.9286(3) 0.5840(3) 0.0680(18) Uani 1 1 d . . . . . H11 H 0.583347 0.976601 0.586881 0.082 Uiso 1 1 calc R U . . . C12 C 0.5947(8) 0.8974(3) 0.5394(2) 0.0587(15) Uani 1 1 d . . . . . H12 H 0.629148 0.923709 0.511892 0.070 Uiso 1 1 calc R U . . . C13 C 0.4589(11) 0.8905(4) 0.7106(3) 0.095(2) Uani 1 1 d . . . . . H13A H 0.347883 0.871570 0.706393 0.114 Uiso 1 1 calc R U . . . H13B H 0.460452 0.921008 0.739093 0.114 Uiso 1 1 calc R U . . . H13C H 0.537536 0.853075 0.715708 0.114 Uiso 1 1 calc R U . . . C14 C 0.5247(10) 0.8218(3) 0.3651(2) 0.0650(17) Uani 1 1 d . . . . . C15 C 0.3979(5) 0.8562(2) 0.33430(15) 0.0661(17) Uani 1 1 d G . . . . C16 C 0.2333(6) 0.8364(2) 0.33582(19) 0.1126(19) Uani 1 1 d G . . . . H16 H 0.198485 0.802335 0.358398 0.135 Uiso 1 1 calc R U . . . C17 C 0.1198(5) 0.8666(3) 0.3043(2) 0.1126(19) Uani 1 1 d G . . . . H17 H 0.007302 0.853055 0.305341 0.135 Uiso 1 1 calc R U . . . C18 C 0.1707(6) 0.9165(3) 0.2713(2) 0.1126(19) Uani 1 1 d G . . . . H18 H 0.093128 0.937045 0.249729 0.135 Uiso 1 1 calc R U . . . C19 C 0.3353(7) 0.9362(2) 0.26975(17) 0.092(2) Uani 1 1 d G . . . . H19 H 0.370138 0.970315 0.247173 0.110 Uiso 1 1 calc R U . . . C20 C 0.4489(5) 0.9061(2) 0.30127(18) 0.082(2) Uani 1 1 d G . . . . H20 H 0.561324 0.919596 0.300230 0.098 Uiso 1 1 calc R U . . . C21 C 0.4307(8) 0.6559(3) 0.31878(18) 0.0569(15) Uani 1 1 d . . . . . H21A H 0.366992 0.697945 0.325861 0.068 Uiso 1 1 calc R U . . . H21B H 0.355345 0.616176 0.320817 0.068 Uiso 1 1 calc R U . . . C22 C 0.5073(8) 0.6600(3) 0.26845(18) 0.0577(15) Uani 1 1 d . . . . . C23 C 0.4861(10) 0.6065(4) 0.2350(2) 0.077(2) Uani 1 1 d . . . . . H23 H 0.424208 0.567320 0.244319 0.092 Uiso 1 1 calc R U . . . C24 C 0.5552(12) 0.6099(6) 0.1879(3) 0.108(3) Uani 1 1 d . . . . . H24 H 0.538824 0.573573 0.165312 0.130 Uiso 1 1 calc R U . . . C25 C 0.6452(12) 0.6651(6) 0.1747(3) 0.105(3) Uani 1 1 d . . . . . H25 H 0.694985 0.666568 0.143176 0.126 Uiso 1 1 calc R U . . . C26 C 0.6662(10) 0.7206(5) 0.2072(3) 0.094(2) Uani 1 1 d . . . . . H26 H 0.724931 0.760379 0.197383 0.113 Uiso 1 1 calc R U . . . C27 C 0.5982(9) 0.7155(4) 0.2542(2) 0.0730(19) Uani 1 1 d . . . . . H27 H 0.615678 0.751623 0.276881 0.088 Uiso 1 1 calc R U . . . C30 C 0.6083(8) 0.4901(3) 0.39613(19) 0.0550(15) Uani 1 1 d . . . . . H30 H 0.677084 0.515201 0.371541 0.066 Uiso 1 1 calc R U . . . C31 C 0.4793(8) 0.4464(3) 0.3691(2) 0.0584(15) Uani 1 1 d . . . . . H31 H 0.537867 0.413948 0.346722 0.070 Uiso 1 1 calc R U . . . C32 C 0.3766(8) 0.4051(3) 0.4058(2) 0.0605(16) Uani 1 1 d . . . . . H32 H 0.314348 0.437049 0.427678 0.073 Uiso 1 1 calc R U . . . C33 C 0.4891(9) 0.3609(3) 0.4366(2) 0.0646(17) Uani 1 1 d . . . . . H33 H 0.540281 0.324965 0.415296 0.078 Uiso 1 1 calc R U . . . C34 C 0.6238(8) 0.4036(3) 0.4599(2) 0.0601(16) Uani 1 1 d . . . . . H34 H 0.573899 0.433906 0.485504 0.072 Uiso 1 1 calc R U . . . C35 C 0.7456(9) 0.3583(3) 0.4832(2) 0.0683(18) Uani 1 1 d . . . . . H35A H 0.691130 0.329178 0.508119 0.082 Uiso 1 1 calc R U . . . H35B H 0.796597 0.328237 0.458227 0.082 Uiso 1 1 calc R U . . . C36A C 0.110(2) 0.3588(10) 0.4045(8) 0.064(3) Uiso 0.429(17) 1 d . U P B 1 H36A H 0.058018 0.404429 0.406599 0.077 Uiso 0.429(17) 1 calc R U P B 1 H36B H 0.130441 0.342206 0.438318 0.077 Uiso 0.429(17) 1 calc R U P B 1 C37A C 0.000(3) 0.3112(7) 0.3787(7) 0.0704(19) Uiso 0.429(17) 1 d G U P B 1 C38A C 0.000(3) 0.2428(8) 0.3927(6) 0.121(5) Uani 0.429(17) 1 d G . P B 1 H38A H 0.065033 0.228348 0.419807 0.145 Uiso 0.429(17) 1 calc R U P B 1 C39A C -0.095(3) 0.1957(6) 0.3672(8) 0.121(5) Uani 0.429(17) 1 d G . P B 1 H39A H -0.095235 0.148954 0.376736 0.145 Uiso 0.429(17) 1 calc R U P B 1 C40A C -0.191(2) 0.2169(8) 0.3275(8) 0.121(5) Uani 0.429(17) 1 d G . P B 1 H40A H -0.255623 0.184619 0.310058 0.145 Uiso 0.429(17) 1 calc R U P B 1 C41A C -0.191(2) 0.2852(9) 0.3135(6) 0.121(5) Uani 0.429(17) 1 d G . P B 1 H41A H -0.255743 0.299677 0.286450 0.145 Uiso 0.429(17) 1 calc R U P B 1 C42A C -0.095(3) 0.3324(6) 0.3391(7) 0.121(5) Uani 0.429(17) 1 d G . P B 1 H42A H -0.095475 0.379072 0.329519 0.145 Uiso 0.429(17) 1 calc R U P B 1 C36B C 0.0966(16) 0.3779(7) 0.3859(6) 0.064(3) Uiso 0.571(17) 1 d . U P B 2 H36C H 0.061261 0.415624 0.364062 0.077 Uiso 0.571(17) 1 calc R U P B 2 H36D H 0.076593 0.391787 0.420318 0.077 Uiso 0.571(17) 1 calc R U P B 2 C37B C 0.0010(19) 0.3140(5) 0.3742(5) 0.0704(19) Uiso 0.571(17) 1 d G U P B 2 C38B C 0.0288(17) 0.2557(6) 0.4023(5) 0.101(3) Uani 0.571(17) 1 d G . P B 2 H38B H 0.107111 0.256717 0.428192 0.121 Uiso 0.571(17) 1 calc R U P B 2 C39B C -0.0581(16) 0.1960(5) 0.3924(5) 0.101(3) Uani 0.571(17) 1 d G . P B 2 H39B H -0.039061 0.156195 0.411519 0.121 Uiso 0.571(17) 1 calc R U P B 2 C40B C -0.1727(15) 0.1946(5) 0.3544(5) 0.101(3) Uani 0.571(17) 1 d G . P B 2 H40B H -0.232011 0.153776 0.347657 0.121 Uiso 0.571(17) 1 calc R U P B 2 C41B C -0.2005(14) 0.2529(7) 0.3264(4) 0.101(3) Uani 0.571(17) 1 d G . P B 2 H41B H -0.278792 0.251880 0.300469 0.121 Uiso 0.571(17) 1 calc R U P B 2 C42B C -0.1136(18) 0.3126(5) 0.3363(5) 0.101(3) Uani 0.571(17) 1 d G . P B 2 H42B H -0.132622 0.352404 0.317142 0.121 Uiso 0.571(17) 1 calc R U P B 2 C43 C 0.9850(11) 0.3674(4) 0.5329(2) 0.082(2) Uani 1 1 d . . . . . C44 C 1.1145(12) 0.4143(4) 0.5520(3) 0.102(3) Uani 1 1 d . . . . . H44A H 1.198443 0.387724 0.569500 0.123 Uiso 1 1 calc R U . . . H44B H 1.064437 0.447386 0.574526 0.123 Uiso 1 1 calc R U . . . H44C H 1.166008 0.438668 0.524534 0.123 Uiso 1 1 calc R U . . . O6A O 0.602(2) 0.5439(6) 0.5595(4) 0.0983(19) Uani 0.583(5) 1 d D U P C 1 O9A O 0.8269(14) 0.4983(5) 0.5939(3) 0.0983(19) Uani 0.583(5) 1 d D U P C 1 C28A C 0.672(2) 0.5035(7) 0.5927(4) 0.081(3) Uani 0.583(5) 1 d D U P C 1 C29A C 0.577(2) 0.4712(8) 0.6303(6) 0.116(5) Uiso 0.583(5) 1 d D U P C 1 H29A H 0.633599 0.477318 0.662213 0.140 Uiso 0.583(5) 1 calc R U P C 1 H29B H 0.570892 0.421550 0.623514 0.140 Uiso 0.583(5) 1 calc R U P C 1 Cl1A Cl 0.3719(6) 0.5046(3) 0.63502(16) 0.1092(16) Uani 0.583(5) 1 d D . P C 1 O6B O 0.597(3) 0.5721(8) 0.5708(5) 0.0983(19) Uani 0.417(5) 1 d D . P C 2 O9B O 0.4502(19) 0.4877(7) 0.5585(4) 0.0983(19) Uani 0.417(5) 1 d D . P C 2 C28B C 0.504(2) 0.5279(9) 0.5882(5) 0.073(5) Uani 0.417(5) 1 d D . P C 2 C29B C 0.469(7) 0.5426(18) 0.6398(12) 0.116(5) Uiso 0.211(7) 1 d D U P C 2 H29C H 0.397052 0.583349 0.641962 0.140 Uiso 0.211(7) 1 calc R U P C 2 H29D H 0.573723 0.553286 0.656856 0.140 Uiso 0.211(7) 1 calc R U P C 2 Cl1B Cl 0.3693(19) 0.4710(5) 0.6703(4) 0.082(2) Uiso 0.211(7) 1 d D U P C 2 C29C C 0.408(6) 0.557(2) 0.6341(18) 0.116(5) Uiso 0.206(7) 1 d D U P D 3 H29E H 0.337386 0.589563 0.620405 0.140 Uiso 0.2058 1 d . U P D 3 H29F H 0.492749 0.572641 0.654737 0.140 Uiso 0.2058 1 d . U P D 3 Cl1C Cl 0.298(2) 0.4838(6) 0.6592(5) 0.082(2) Uiso 0.206(7) 1 d D U P D 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.042(2) 0.060(2) 0.055(2) 0.0027(17) -0.0059(18) -0.0023(18) O2 0.056(3) 0.054(2) 0.065(2) 0.0002(18) -0.002(2) -0.007(2) O3 0.053(3) 0.055(2) 0.060(2) 0.0089(17) 0.0047(19) 0.001(2) O4 0.034(2) 0.071(3) 0.048(2) 0.0035(17) 0.0018(16) 0.0017(18) O5 0.043(2) 0.054(2) 0.056(2) -0.0040(17) 0.0034(17) -0.0019(19) O7 0.062(3) 0.084(3) 0.094(3) -0.035(3) 0.012(3) -0.015(3) O8 0.067(4) 0.090(3) 0.098(3) 0.029(3) -0.002(3) -0.021(3) O10 0.045(3) 0.064(2) 0.058(2) 0.0025(18) 0.0030(18) 0.0046(19) O11 0.047(3) 0.067(3) 0.089(3) -0.020(2) 0.018(2) -0.011(2) O12 0.086(4) 0.087(3) 0.099(3) 0.014(3) 0.035(3) -0.008(3) O13 0.091(4) 0.064(3) 0.083(3) 0.003(2) -0.027(3) 0.003(3) O14 0.129(5) 0.079(4) 0.124(4) 0.046(3) -0.034(4) 0.008(3) N1 0.079(4) 0.079(4) 0.072(3) 0.002(3) -0.021(3) -0.017(3) N2 0.066(4) 0.089(4) 0.076(4) 0.000(3) -0.010(3) -0.006(3) N3 0.096(5) 0.145(6) 0.084(4) -0.023(4) -0.028(4) -0.018(5) C1 0.044(4) 0.047(3) 0.055(3) 0.000(2) -0.011(3) -0.004(3) C2 0.043(4) 0.057(3) 0.051(3) 0.005(2) 0.004(3) -0.008(3) C3 0.040(3) 0.063(3) 0.045(3) 0.006(2) 0.002(2) 0.000(3) C4 0.035(3) 0.054(3) 0.046(3) 0.003(2) -0.001(2) 0.000(3) C5 0.051(4) 0.054(3) 0.047(3) 0.000(2) 0.003(3) -0.011(3) C6 0.090(5) 0.064(4) 0.045(3) -0.002(3) -0.008(3) 0.004(4) C7 0.040(4) 0.055(4) 0.066(4) -0.009(3) -0.008(3) 0.004(3) C8 0.040(4) 0.052(3) 0.058(3) 0.002(3) -0.003(3) 0.000(3) C9 0.035(3) 0.059(4) 0.072(4) -0.001(3) -0.006(3) -0.005(3) C10 0.035(4) 0.068(4) 0.075(4) -0.017(3) -0.005(3) -0.004(3) C11 0.047(4) 0.055(4) 0.102(5) -0.012(4) -0.002(4) -0.004(3) C12 0.049(4) 0.055(4) 0.072(4) 0.002(3) -0.009(3) -0.006(3) C13 0.078(5) 0.116(6) 0.090(5) -0.040(5) 0.019(5) -0.012(5) C14 0.063(5) 0.060(4) 0.072(4) 0.001(3) 0.004(4) -0.007(4) C15 0.070(5) 0.068(4) 0.060(4) 0.011(3) 0.000(3) 0.004(3) C16 0.085(4) 0.094(4) 0.159(5) 0.041(3) -0.036(3) 0.000(3) C17 0.085(4) 0.094(4) 0.159(5) 0.041(3) -0.036(3) 0.000(3) C18 0.085(4) 0.094(4) 0.159(5) 0.041(3) -0.036(3) 0.000(3) C19 0.103(7) 0.089(5) 0.083(5) 0.025(4) -0.004(5) 0.013(5) C20 0.091(6) 0.075(5) 0.078(4) 0.016(4) 0.006(4) 0.005(4) C21 0.045(4) 0.072(4) 0.054(3) 0.008(3) -0.002(3) 0.003(3) C22 0.057(4) 0.069(4) 0.047(3) 0.007(3) 0.001(3) 0.006(3) C23 0.079(5) 0.089(5) 0.064(4) -0.008(3) 0.007(4) -0.007(4) C24 0.112(8) 0.148(8) 0.065(5) -0.014(5) 0.016(5) -0.008(7) C25 0.103(7) 0.162(9) 0.051(4) 0.013(5) 0.016(4) 0.005(7) C26 0.091(6) 0.123(6) 0.069(5) 0.026(5) 0.022(4) -0.006(5) C27 0.067(5) 0.083(5) 0.069(4) 0.006(3) 0.010(3) 0.003(4) C30 0.052(4) 0.069(4) 0.044(3) -0.006(3) 0.009(3) 0.008(3) C31 0.058(4) 0.065(4) 0.052(3) -0.004(3) 0.007(3) 0.001(3) C32 0.049(4) 0.065(4) 0.067(4) -0.006(3) 0.005(3) -0.006(3) C33 0.067(5) 0.061(4) 0.065(4) 0.003(3) 0.017(3) -0.002(4) C34 0.067(4) 0.063(4) 0.051(3) 0.009(3) 0.010(3) 0.004(3) C35 0.074(5) 0.069(4) 0.062(4) 0.003(3) 0.002(3) 0.003(4) C38A 0.133(11) 0.090(7) 0.140(10) -0.006(6) -0.017(8) -0.048(7) C39A 0.133(11) 0.090(7) 0.140(10) -0.006(6) -0.017(8) -0.048(7) C40A 0.133(11) 0.090(7) 0.140(10) -0.006(6) -0.017(8) -0.048(7) C41A 0.133(11) 0.090(7) 0.140(10) -0.006(6) -0.017(8) -0.048(7) C42A 0.133(11) 0.090(7) 0.140(10) -0.006(6) -0.017(8) -0.048(7) C38B 0.092(6) 0.094(5) 0.117(6) 0.000(4) -0.010(5) -0.034(4) C39B 0.092(6) 0.094(5) 0.117(6) 0.000(4) -0.010(5) -0.034(4) C40B 0.092(6) 0.094(5) 0.117(6) 0.000(4) -0.010(5) -0.034(4) C41B 0.092(6) 0.094(5) 0.117(6) 0.000(4) -0.010(5) -0.034(4) C42B 0.092(6) 0.094(5) 0.117(6) 0.000(4) -0.010(5) -0.034(4) C43 0.097(6) 0.089(5) 0.060(4) 0.007(4) -0.013(4) 0.012(5) C44 0.109(7) 0.110(6) 0.088(5) -0.002(4) -0.044(5) 0.000(5) O6A 0.112(4) 0.115(5) 0.067(3) 0.016(3) 0.010(3) -0.005(4) O9A 0.112(4) 0.115(5) 0.067(3) 0.016(3) 0.010(3) -0.005(4) C28A 0.109(7) 0.101(9) 0.034(5) -0.005(5) 0.019(6) 0.027(8) Cl1A 0.104(3) 0.124(3) 0.099(3) 0.005(2) 0.005(2) -0.013(3) O6B 0.112(4) 0.115(5) 0.067(3) 0.016(3) 0.010(3) -0.005(4) O9B 0.112(4) 0.115(5) 0.067(3) 0.016(3) 0.010(3) -0.005(4) C28B 0.071(12) 0.108(13) 0.039(8) -0.036(8) 0.015(8) -0.032(11) 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' 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 C1 O1 C5 112.2(4) . . ? C7 O2 C1 118.4(4) . . ? C14 O3 C2 118.2(5) . . ? C3 O4 C21 114.0(4) . . ? C30 O5 C4 117.8(4) . . ? C10 O7 C13 116.7(5) . . ? C30 O10 C34 115.2(4) . . ? C36B O11 C32 116.5(6) . . ? C32 O11 C36A 110.4(7) . . ? C33 O12 H12X 109.5 . . ? C43 O13 C35 116.5(5) . . ? N2 N1 C31 115.2(5) . . ? N3 N2 N1 170.4(8) . . ? O2 C1 O1 107.0(4) . . ? O2 C1 C2 107.1(4) . . ? O1 C1 C2 107.5(5) . . ? O2 C1 H1 111.7 . . ? O1 C1 H1 111.7 . . ? C2 C1 H1 111.7 . . ? O3 C2 C3 108.0(4) . . ? O3 C2 C1 108.5(5) . . ? C3 C2 C1 111.6(4) . . ? O3 C2 H2 109.6 . . ? C3 C2 H2 109.6 . . ? C1 C2 H2 109.6 . . ? O4 C3 C4 108.6(4) . . ? O4 C3 C2 108.9(4) . . ? C4 C3 C2 112.0(4) . . ? O4 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? C2 C3 H3 109.1 . . ? O5 C4 C3 109.7(4) . . ? O5 C4 C5 106.6(4) . . ? C3 C4 C5 110.3(4) . . ? O5 C4 H4 110.1 . . ? C3 C4 H4 110.1 . . ? C5 C4 H4 110.1 . . ? O1 C5 C6 105.3(4) . . ? O1 C5 C4 109.7(4) . . ? C6 C5 C4 112.1(5) . . ? O1 C5 H5 109.9 . . ? C6 C5 H5 109.9 . . ? C4 C5 H5 109.9 . . ? O6A C6 C5 111.7(8) . . ? C5 C6 O6B 102.3(9) . . ? O6A C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? O6A C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C8 C7 O2 125.4(5) . . ? C8 C7 C12 119.5(5) . . ? O2 C7 C12 115.1(5) . . ? C7 C8 C9 120.0(5) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.9(6) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? O7 C10 C9 125.1(6) . . ? O7 C10 C11 115.4(6) . . ? C9 C10 C11 119.5(6) . . ? C10 C11 C12 121.2(6) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.9(6) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O7 C13 H13A 109.5 . . ? O7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O8 C14 O3 122.6(6) . . ? O8 C14 C15 125.8(6) . . ? O3 C14 C15 111.5(6) . . ? C16 C15 C20 120.0 . . ? C16 C15 C14 121.4(4) . . ? C20 C15 C14 118.4(4) . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? O4 C21 C22 106.9(5) . . ? O4 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? O4 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.6 . . ? C27 C22 C23 118.3(6) . . ? C27 C22 C21 121.6(6) . . ? C23 C22 C21 120.1(6) . . ? C22 C23 C24 120.7(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.9(8) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 118.1(8) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C22 C27 C26 122.0(7) . . ? C22 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? O5 C30 O10 112.2(4) . . ? O5 C30 C31 108.4(5) . . ? O10 C30 C31 108.1(5) . . ? O5 C30 H30 109.4 . . ? O10 C30 H30 109.4 . . ? C31 C30 H30 109.4 . . ? N1 C31 C32 111.6(5) . . ? N1 C31 C30 108.5(5) . . ? C32 C31 C30 110.5(5) . . ? N1 C31 H31 108.7 . . ? C32 C31 H31 108.7 . . ? C30 C31 H31 108.7 . . ? O11 C32 C33 110.7(5) . . ? O11 C32 C31 108.1(5) . . ? C33 C32 C31 109.6(5) . . ? O11 C32 H32 109.5 . . ? C33 C32 H32 109.5 . . ? C31 C32 H32 109.5 . . ? O12 C33 C32 108.6(6) . . ? O12 C33 C34 109.5(5) . . ? C32 C33 C34 110.6(5) . . ? O12 C33 H33 109.4 . . ? C32 C33 H33 109.4 . . ? C34 C33 H33 109.4 . . ? O10 C34 C35 108.0(5) . . ? O10 C34 C33 111.9(4) . . ? C35 C34 C33 109.5(5) . . ? O10 C34 H34 109.2 . . ? C35 C34 H34 109.2 . . ? C33 C34 H34 109.2 . . ? O13 C35 C34 108.5(5) . . ? O13 C35 H35A 110.0 . . ? C34 C35 H35A 110.0 . . ? O13 C35 H35B 110.0 . . ? C34 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? O11 C36A C37A 109.9(15) . . ? O11 C36A H36A 109.7 . . ? C37A C36A H36A 109.7 . . ? O11 C36A H36B 109.7 . . ? C37A C36A H36B 109.7 . . ? H36A C36A H36B 108.2 . . ? C38A C37A C42A 120.0 . . ? C38A C37A C36A 118.5(13) . . ? C42A C37A C36A 121.4(13) . . ? C37A C38A C39A 120.0 . . ? C37A C38A H38A 120.0 . . ? C39A C38A H38A 120.0 . . ? C40A C39A C38A 120.0 . . ? C40A C39A H39A 120.0 . . ? C38A C39A H39A 120.0 . . ? C39A C40A C41A 120.0 . . ? C39A C40A H40A 120.0 . . ? C41A C40A H40A 120.0 . . ? C40A C41A C42A 120.0 . . ? C40A C41A H41A 120.0 . . ? C42A C41A H41A 120.0 . . ? C41A C42A C37A 120.0 . . ? C41A C42A H42A 120.0 . . ? C37A C42A H42A 120.0 . . ? O11 C36B C37B 108.1(11) . . ? O11 C36B H36C 110.1 . . ? C37B C36B H36C 110.1 . . ? O11 C36B H36D 110.1 . . ? C37B C36B H36D 110.1 . . ? H36C C36B H36D 108.4 . . ? C38B C37B C42B 120.0 . . ? C38B C37B C36B 118.8(9) . . ? C42B C37B C36B 121.2(9) . . ? C37B C38B C39B 120.0 . . ? C37B C38B H38B 120.0 . . ? C39B C38B H38B 120.0 . . ? C40B C39B C38B 120.0 . . ? C40B C39B H39B 120.0 . . ? C38B C39B H39B 120.0 . . ? C39B C40B C41B 120.0 . . ? C39B C40B H40B 120.0 . . ? C41B C40B H40B 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? C42B C41B H41B 120.0 . . ? C41B C42B C37B 120.0 . . ? C41B C42B H42B 120.0 . . ? C37B C42B H42B 120.0 . . ? O14 C43 O13 121.5(8) . . ? O14 C43 C44 126.0(8) . . ? O13 C43 C44 112.4(7) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C28A O6A C6 121.9(14) . . ? O9A C28A O6A 119.4(13) . . ? O9A C28A C29A 118.9(12) . . ? O6A C28A C29A 121.4(15) . . ? C28A C29A Cl1A 113.0(11) . . ? C28A C29A H29A 109.0 . . ? Cl1A C29A H29A 109.0 . . ? C28A C29A H29B 109.0 . . ? Cl1A C29A H29B 109.0 . . ? H29A C29A H29B 107.8 . . ? C28B O6B C6 128.2(13) . . ? O9B C28B O6B 114.5(14) . . ? O9B C28B C29B 135(2) . . ? O6B C28B C29B 110.2(18) . . ? C28B C29B Cl1B 112(2) . . ? C28B C29B H29C 109.2 . . ? Cl1B C29B H29C 109.2 . . ? C28B C29B H29D 109.2 . . ? Cl1B C29B H29D 109.2 . . ? H29C C29B H29D 107.9 . . ? Cl1C C29C H29E 112.9 . . ? Cl1C C29C H29F 112.8 . . ? H29E C29C H29F 117.9 . . ? 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 O1 C1 1.434(6) . ? O1 C5 1.446(6) . ? O2 C7 1.388(7) . ? O2 C1 1.398(6) . ? O3 C14 1.353(7) . ? O3 C2 1.431(6) . ? O4 C3 1.429(6) . ? O4 C21 1.454(6) . ? O5 C30 1.406(6) . ? O5 C4 1.425(6) . ? O7 C10 1.374(7) . ? O7 C13 1.440(9) . ? O8 C14 1.202(8) . ? O10 C30 1.414(7) . ? O10 C34 1.463(6) . ? O11 C36B 1.392(13) . ? O11 C32 1.425(7) . ? O11 C36A 1.427(18) . ? O12 C33 1.412(7) . ? O12 H12X 0.8400 . ? O13 C43 1.341(9) . ? O13 C35 1.448(8) . ? O14 C43 1.210(8) . ? N1 N2 1.226(8) . ? N1 C31 1.455(8) . ? N2 N3 1.143(8) . ? C1 C2 1.524(8) . ? C1 H1 1.0000 . ? C2 C3 1.523(8) . ? C2 H2 1.0000 . ? C3 C4 1.519(7) . ? C3 H3 1.0000 . ? C4 C5 1.538(7) . ? C4 H4 1.0000 . ? C5 C6 1.532(8) . ? C5 H5 1.0000 . ? C6 O6A 1.363(13) . ? C6 O6B 1.542(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.375(8) . ? C7 C12 1.392(8) . ? C8 C9 1.411(8) . ? C8 H8 0.9500 . ? C9 C10 1.376(8) . ? C9 H9 0.9500 . ? C10 C11 1.377(9) . ? C11 C12 1.377(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.487(8) . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.507(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.368(9) . ? C22 C23 1.399(8) . ? C23 C24 1.401(10) . ? C23 H23 0.9500 . ? C24 C25 1.352(12) . ? C24 H24 0.9500 . ? C25 C26 1.410(12) . ? C25 H25 0.9500 . ? C26 C27 1.396(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C30 C31 1.539(8) . ? C30 H30 1.0000 . ? C31 C32 1.532(8) . ? C31 H31 1.0000 . ? C32 C33 1.510(9) . ? C32 H32 1.0000 . ? C33 C34 1.515(9) . ? C33 H33 1.0000 . ? C34 C35 1.471(9) . ? C34 H34 1.0000 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36A C37A 1.471(18) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38A 1.3900 . ? C37A C42A 1.3900 . ? C38A C39A 1.3900 . ? C38A H38A 0.9500 . ? C39A C40A 1.3900 . ? C39A H39A 0.9500 . ? C40A C41A 1.3900 . ? C40A H40A 0.9500 . ? C41A C42A 1.3900 . ? C41A H41A 0.9500 . ? C42A H42A 0.9500 . ? C36B C37B 1.504(13) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B C38B 1.3900 . ? C37B C42B 1.3900 . ? C38B C39B 1.3900 . ? C38B H38B 0.9500 . ? C39B C40B 1.3900 . ? C39B H39B 0.9500 . ? C40B C41B 1.3900 . ? C40B H40B 0.9500 . ? C41B C42B 1.3900 . ? C41B H41B 0.9500 . ? C42B H42B 0.9500 . ? C43 C44 1.489(11) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O6A C28A 1.329(15) . ? O9A C28A 1.262(14) . ? C28A C29A 1.428(19) . ? C29A Cl1A 1.791(17) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? O6B C28B 1.242(18) . ? O9B C28B 1.210(15) . ? C28B C29B 1.46(3) . ? C29B Cl1B 1.82(3) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C29C Cl1C 1.82(3) . ? C29C H29E 0.9316 . ? C29C H29F 0.9404 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O12 H12X O14 0.84 1.92 2.751(8) 168.6 4_456 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O2 C1 O1 -77.8(6) . . . . ? C7 O2 C1 C2 167.1(5) . . . . ? C5 O1 C1 O2 179.8(4) . . . . ? C5 O1 C1 C2 -65.4(5) . . . . ? C14 O3 C2 C3 -117.1(5) . . . . ? C14 O3 C2 C1 121.9(5) . . . . ? O2 C1 C2 O3 -69.2(6) . . . . ? O1 C1 C2 O3 176.1(4) . . . . ? O2 C1 C2 C3 172.0(5) . . . . ? O1 C1 C2 C3 57.3(6) . . . . ? C21 O4 C3 C4 137.6(5) . . . . ? C21 O4 C3 C2 -100.3(5) . . . . ? O3 C2 C3 O4 70.0(5) . . . . ? C1 C2 C3 O4 -170.9(4) . . . . ? O3 C2 C3 C4 -169.9(4) . . . . ? C1 C2 C3 C4 -50.8(6) . . . . ? C30 O5 C4 C3 104.5(5) . . . . ? C30 O5 C4 C5 -136.1(5) . . . . ? O4 C3 C4 O5 -74.4(5) . . . . ? C2 C3 C4 O5 165.4(4) . . . . ? O4 C3 C4 C5 168.5(5) . . . . ? C2 C3 C4 C5 48.3(6) . . . . ? C1 O1 C5 C6 -174.5(4) . . . . ? C1 O1 C5 C4 64.7(6) . . . . ? O5 C4 C5 O1 -172.9(4) . . . . ? C3 C4 C5 O1 -53.9(6) . . . . ? O5 C4 C5 C6 70.5(6) . . . . ? C3 C4 C5 C6 -170.5(5) . . . . ? O1 C5 C6 O6A 108.4(7) . . . . ? C4 C5 C6 O6A -132.4(7) . . . . ? O1 C5 C6 O6B 85.0(8) . . . . ? C4 C5 C6 O6B -155.8(8) . . . . ? C1 O2 C7 C8 20.8(8) . . . . ? C1 O2 C7 C12 -160.9(5) . . . . ? O2 C7 C8 C9 177.3(5) . . . . ? C12 C7 C8 C9 -0.9(9) . . . . ? C7 C8 C9 C10 0.4(9) . . . . ? C13 O7 C10 C9 0.7(9) . . . . ? C13 O7 C10 C11 -178.4(6) . . . . ? C8 C9 C10 O7 -178.4(6) . . . . ? C8 C9 C10 C11 0.7(9) . . . . ? O7 C10 C11 C12 177.8(6) . . . . ? C9 C10 C11 C12 -1.4(10) . . . . ? C10 C11 C12 C7 0.9(10) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? O2 C7 C12 C11 -178.2(5) . . . . ? C2 O3 C14 O8 -10.7(8) . . . . ? C2 O3 C14 C15 167.2(4) . . . . ? O8 C14 C15 C16 172.3(6) . . . . ? O3 C14 C15 C16 -5.4(6) . . . . ? O8 C14 C15 C20 -3.5(8) . . . . ? O3 C14 C15 C20 178.7(4) . . . . ? C20 C15 C16 C17 0.0 . . . . ? C14 C15 C16 C17 -175.8(5) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C15 0.0 . . . . ? C16 C15 C20 C19 0.0 . . . . ? C14 C15 C20 C19 175.9(5) . . . . ? C3 O4 C21 C22 168.8(4) . . . . ? O4 C21 C22 C27 -69.1(7) . . . . ? O4 C21 C22 C23 111.0(7) . . . . ? C27 C22 C23 C24 -0.6(11) . . . . ? C21 C22 C23 C24 179.4(7) . . . . ? C22 C23 C24 C25 0.9(13) . . . . ? C23 C24 C25 C26 -2.2(14) . . . . ? C24 C25 C26 C27 3.1(13) . . . . ? C23 C22 C27 C26 1.6(11) . . . . ? C21 C22 C27 C26 -178.4(7) . . . . ? C25 C26 C27 C22 -2.8(12) . . . . ? C4 O5 C30 O10 91.9(5) . . . . ? C4 O5 C30 C31 -148.8(4) . . . . ? C34 O10 C30 O5 60.9(6) . . . . ? C34 O10 C30 C31 -58.6(5) . . . . ? N2 N1 C31 C32 -75.0(7) . . . . ? N2 N1 C31 C30 163.0(6) . . . . ? O5 C30 C31 N1 59.4(6) . . . . ? O10 C30 C31 N1 -178.7(4) . . . . ? O5 C30 C31 C32 -63.2(6) . . . . ? O10 C30 C31 C32 58.7(6) . . . . ? C36B O11 C32 C33 123.7(9) . . . . ? C36A O11 C32 C33 95.9(11) . . . . ? C36B O11 C32 C31 -116.3(10) . . . . ? C36A O11 C32 C31 -144.1(11) . . . . ? N1 C31 C32 O11 61.1(6) . . . . ? C30 C31 C32 O11 -178.1(5) . . . . ? N1 C31 C32 C33 -178.2(5) . . . . ? C30 C31 C32 C33 -57.4(6) . . . . ? O11 C32 C33 O12 -67.3(6) . . . . ? C31 C32 C33 O12 173.5(5) . . . . ? O11 C32 C33 C34 172.5(5) . . . . ? C31 C32 C33 C34 53.3(6) . . . . ? C30 O10 C34 C35 177.0(5) . . . . ? C30 O10 C34 C33 56.4(6) . . . . ? O12 C33 C34 O10 -171.3(5) . . . . ? C32 C33 C34 O10 -51.7(6) . . . . ? O12 C33 C34 C35 69.0(7) . . . . ? C32 C33 C34 C35 -171.3(5) . . . . ? C43 O13 C35 C34 174.7(5) . . . . ? O10 C34 C35 O13 59.3(6) . . . . ? C33 C34 C35 O13 -178.6(5) . . . . ? C32 O11 C36A C37A -174.7(12) . . . . ? O11 C36A C37A C38A 92.8(18) . . . . ? O11 C36A C37A C42A -83.1(19) . . . . ? C42A C37A C38A C39A 0.0 . . . . ? C36A C37A C38A C39A -176(2) . . . . ? C37A C38A C39A C40A 0.0 . . . . ? C38A C39A C40A C41A 0.0 . . . . ? C39A C40A C41A C42A 0.0 . . . . ? C40A C41A C42A C37A 0.0 . . . . ? C38A C37A C42A C41A 0.0 . . . . ? C36A C37A C42A C41A 176(2) . . . . ? C32 O11 C36B C37B -155.0(9) . . . . ? O11 C36B C37B C38B 62.1(14) . . . . ? O11 C36B C37B C42B -118.0(12) . . . . ? C42B C37B C38B C39B 0.0 . . . . ? C36B C37B C38B C39B 179.9(15) . . . . ? C37B C38B C39B C40B 0.0 . . . . ? C38B C39B C40B C41B 0.0 . . . . ? C39B C40B C41B C42B 0.0 . . . . ? C40B C41B C42B C37B 0.0 . . . . ? C38B C37B C42B C41B 0.0 . . . . ? C36B C37B C42B C41B -179.9(15) . . . . ? C35 O13 C43 O14 -1.1(10) . . . . ? C35 O13 C43 C44 175.9(6) . . . . ? C5 C6 O6A C28A -178.0(10) . . . . ? C6 O6A C28A O9A 11.4(18) . . . . ? C6 O6A C28A C29A -175.2(11) . . . . ? O9A C28A C29A Cl1A 161.4(11) . . . . ? O6A C28A C29A Cl1A -12.1(18) . . . . ? C5 C6 O6B C28B 102(2) . . . . ? C6 O6B C28B O9B -18(3) . . . . ? C6 O6B C28B C29B 168(3) . . . . ? O9B C28B C29B Cl1B 21(6) . . . . ? O6B C28B C29B Cl1B -168(3) . . . . ?