#------------------------------------------------------------------------------ #$Date: 2014-12-26 09:57:27 +0200 (Fri, 26 Dec 2014) $ #$Revision: 129084 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/61/7116128.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_7116128 loop_ _publ_author_name 'L. Turunen' 'N. K. Beyeh' 'F. Pan' 'A. Valkonen' 'K. Rissanen' _publ_section_title ; Tetraiodoethynyl resorcinarene cavitands as multivalent halogen bond donors ; _journal_name_full Chem.Commun. _journal_page_first 15920 _journal_paper_doi 10.1039/C4cc07771G _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C64 H68 I4 O8, 3.7(C4 H8 O2), 0.3(O)' _chemical_formula_sum 'C78.8 H97.6 I4 O15.7' _chemical_formula_weight 1803.56 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 96.532(2) _cell_angle_beta 101.5835(19) _cell_angle_gamma 113.200(3) _cell_formula_units_Z 2 _cell_length_a 14.9822(4) _cell_length_b 16.9494(5) _cell_length_c 17.6201(4) _cell_measurement_reflns_used 11732 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 71.0410 _cell_measurement_theta_min 3.4420 _cell_volume 3935.3(2) _computing_cell_refinement CrysAlisPro _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2013)' _computing_data_reduction CrysAlisPro _computing_molecular_graphics 'SHELXL-2013 (Sheldrick, 2013)' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SIR2011 (Burla, et. al., 2012)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 5.1977 _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_laue_measured_fraction_full 0.980 _diffrn_reflns_laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22925 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.498 _diffrn_reflns_theta_min 3.332 _exptl_absorpt_coefficient_mu 12.945 _exptl_absorpt_correction_T_max 0.454 _exptl_absorpt_correction_T_min 0.104 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31. Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.522 _exptl_crystal_description plate _exptl_crystal_F_000 1816 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.040 _refine_diff_density_max 4.521 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.177 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1036 _refine_ls_number_reflns 13955 _refine_ls_number_restraints 433 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0728 _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^)+(0.1399P)^2^+7.2423P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1951 _refine_ls_wR_factor_ref 0.2091 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11795 _reflns_number_total 13955 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc07771g2.cif _[local]_cod_data_source_block 4b.dioxane _[local]_cod_chemical_formula_sum_orig 'C78.80 H97.60 I4 O15.70' _cod_original_cell_volume 3935.34(19) _cod_database_code 7116128 _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 0.112 _shelx_estimated_absorpt_t_max 0.625 _shelxl_version_number 2013-4 _shelx_res_file ; TITL l1+k3 in P -1 CELL 1.54184 14.982179 16.949358 17.62005 96.5315 101.5835 113.1996 ZERR 2 0.000369 0.000486 0.000368 0.002 0.0019 0.0025 LATT 1 SFAC C H I O UNIT 157.6 195.2 8 31.4 DFIX 1.4 O13 C73 O13 C76 O14 C74 O14 C75 O13B C73B O13B C76B O14B C74B O14B = C75B DFIX 1.45 C73 C74 C75 C76 C73B C74B C75B C76B DFIX 2.8 O13 O14 O13B O14B DFIX 1.4 O15 C77 O15 C80 O16 C78 O16 C79 O15B C77B O15B C80B O16B C78B O16B = C79B DFIX 1.45 C77 C78 C79 C80 C77B C78B C79B C80B DFIX 2.8 O15 O16 O15B O16B SADI C43 C44 C43 C44B SADI C44 C45 C44B C45B SADI C77B C80B C78B C79B SIMU 0.01 0.02 1.7 C44 C45 C44B C45B SIMU 0.01 0.02 1.7 O11 C69 C70 O12 C71 C72 SIMU 0.01 0.02 1.7 O13 C73 C74 O14 C75 C76 O13B C73B C74B O14B C75B C76B SIMU 0.01 0.02 1.7 O15 C77 C78 O16 C79 C80 O15B C77B C78B O16B C79B C80B L.S. 20 PLAN 25 SIZE 0.04 0.18 0.3 TEMP -150 CONF HTAB BOND $H MORE -1 FMAP 2 ACTA MERG 2 OMIT -3 135 WGHT 0.139900 7.242300 FVAR 1.81226 I1 3 0.479295 0.487889 0.301550 11.00000 0.04332 0.05341 = 0.02616 0.00444 0.00766 0.02018 I2 3 0.440913 0.086042 0.546584 11.00000 0.06702 0.04303 = 0.05387 0.00042 -0.00159 0.01573 I3 3 0.098870 0.246027 0.769394 11.00000 0.03327 0.06492 = 0.05070 0.00539 0.00814 0.01327 I4 3 0.170827 0.693034 0.556787 11.00000 0.04428 0.08242 = 0.04720 0.01945 0.01185 0.03254 O1 4 0.642010 0.734520 0.554622 11.00000 0.03857 0.04674 = 0.02939 0.00995 0.00781 0.01774 O2 4 0.751203 0.506166 0.549585 11.00000 0.04010 0.04769 = 0.02558 0.00565 0.01251 0.02093 O3 4 0.742582 0.394714 0.620417 11.00000 0.03573 0.05089 = 0.02518 0.00528 0.01180 0.02178 O4 4 0.584676 0.296618 0.822782 11.00000 0.04088 0.04032 = 0.04357 0.01049 0.01764 0.01743 O5 4 0.483286 0.340990 0.887680 11.00000 0.03830 0.04137 = 0.04358 0.01158 0.01995 0.01332 O6 4 0.370093 0.566841 0.891426 11.00000 0.03523 0.04960 = 0.03719 0.01148 0.01564 0.01962 O7 4 0.388589 0.684433 0.825360 11.00000 0.03207 0.05134 = 0.04031 0.01197 0.01343 0.02065 O8 4 0.553509 0.787123 0.628076 11.00000 0.04378 0.04370 = 0.03346 0.01123 0.01131 0.01913 C1 1 0.749874 0.729909 0.675268 11.00000 0.03011 0.03988 = 0.03014 0.01138 0.01264 0.01036 C2 1 0.692772 0.693182 0.597083 11.00000 0.03464 0.04214 = 0.02902 0.00930 0.00994 0.01430 C3 1 0.690223 0.616582 0.555137 11.00000 0.03376 0.04667 = 0.02590 0.00849 0.00856 0.01213 C4 1 0.748877 0.577600 0.593945 11.00000 0.03621 0.04439 = 0.02653 0.00673 0.01477 0.01508 C5 1 0.807206 0.613375 0.672143 11.00000 0.02684 0.04845 = 0.02869 0.00687 0.01166 0.01382 C6 1 0.804662 0.689013 0.711386 11.00000 0.02683 0.04592 = 0.02717 0.00749 0.01104 0.00969 AFIX 43 H6 2 0.842423 0.713088 0.765278 11.00000 -1.20000 AFIX 0 C7 1 0.865615 0.567402 0.714327 11.00000 0.03154 0.05148 = 0.02466 0.00439 0.00944 0.01694 AFIX 13 H7 2 0.885116 0.537263 0.672805 11.00000 -1.20000 AFIX 0 C8 1 0.963707 0.629598 0.777120 11.00000 0.02849 0.04753 = 0.03565 0.00588 0.00865 0.01654 AFIX 23 H8A 2 0.992127 0.594106 0.805624 11.00000 -1.20000 H8B 2 0.947939 0.665286 0.816246 11.00000 -1.20000 AFIX 0 C9 1 1.043902 0.691774 0.742295 11.00000 0.03599 0.06625 = 0.04764 0.01779 0.01390 0.01506 AFIX 23 H9A 2 1.069242 0.656887 0.711230 11.00000 -1.20000 H9B 2 1.011829 0.718913 0.705482 11.00000 -1.20000 AFIX 0 C10 1 1.133137 0.764594 0.805409 11.00000 0.03522 0.06206 = 0.06538 0.01846 0.01768 0.01002 AFIX 23 H10A 2 1.181317 0.800961 0.778462 11.00000 -1.20000 H10B 2 1.108155 0.802832 0.832477 11.00000 -1.20000 AFIX 0 C11 1 1.189480 0.734018 0.867654 11.00000 0.03531 0.07115 = 0.05013 -0.00245 0.00599 0.01867 AFIX 23 H11A 2 1.142262 0.700048 0.896490 11.00000 -1.20000 H11B 2 1.212080 0.693741 0.840643 11.00000 -1.20000 AFIX 0 C12 1 1.279991 0.806798 0.927264 11.00000 0.04632 0.06619 = 0.08002 0.00695 -0.00123 0.00303 AFIX 23 H12A 2 1.326014 0.842154 0.898310 11.00000 -1.20000 H12B 2 1.257038 0.845808 0.955738 11.00000 -1.20000 AFIX 0 C13 1 1.338354 0.775974 0.987538 11.00000 0.05145 0.10086 = 0.05441 -0.01159 0.00513 0.03109 AFIX 33 H13A 2 1.395590 0.826974 1.023746 11.00000 -1.50000 H13B 2 1.363181 0.738572 0.960207 11.00000 -1.50000 H13C 2 1.294180 0.742365 1.017792 11.00000 -1.50000 AFIX 0 C14 1 0.627052 0.576851 0.476081 11.00000 0.03661 0.04851 = 0.02311 0.00454 0.00760 0.01860 C15 1 0.571469 0.543708 0.410267 11.00000 0.04170 0.04107 = 0.04083 0.00539 0.01271 0.01963 C16 1 0.690707 0.421605 0.560637 11.00000 0.04021 0.04899 = 0.02676 0.00224 0.01145 0.01800 AFIX 23 H16A 2 0.630312 0.422568 0.574627 11.00000 -1.20000 H16B 2 0.667547 0.378195 0.510112 11.00000 -1.20000 AFIX 0 C17 1 0.793519 0.496043 0.745261 11.00000 0.02963 0.04610 = 0.02849 0.00694 0.01128 0.01673 C18 1 0.732486 0.413921 0.696789 11.00000 0.03765 0.04685 = 0.02948 0.00382 0.00976 0.02316 C19 1 0.660956 0.346869 0.720564 11.00000 0.03752 0.03938 = 0.03707 0.00264 0.00881 0.01796 C20 1 0.651973 0.364580 0.798274 11.00000 0.03309 0.04020 = 0.03393 0.01007 0.01049 0.01442 C21 1 0.710752 0.446165 0.849259 11.00000 0.03314 0.04206 = 0.02958 0.00756 0.01030 0.01956 C22 1 0.780832 0.510994 0.822192 11.00000 0.02849 0.04508 = 0.02843 0.00613 0.00653 0.01678 AFIX 43 H22 2 0.821306 0.566954 0.856540 11.00000 -1.20000 AFIX 0 C23 1 0.692130 0.462604 0.930231 11.00000 0.03068 0.04248 = 0.02968 0.00883 0.01336 0.01239 AFIX 13 H23 2 0.665913 0.404447 0.945743 11.00000 -1.20000 AFIX 0 C24 1 0.786882 0.524400 0.996741 11.00000 0.03539 0.04735 = 0.02849 0.00842 0.00980 0.01787 AFIX 23 H24A 2 0.821116 0.579943 0.979986 11.00000 -1.20000 H24B 2 0.766751 0.538645 1.044812 11.00000 -1.20000 AFIX 0 C25 1 0.859428 0.483323 1.016423 11.00000 0.04349 0.05293 = 0.04619 0.00986 0.00135 0.02445 AFIX 23 H25A 2 0.890281 0.480808 0.972042 11.00000 -1.20000 H25B 2 0.821249 0.422237 1.021314 11.00000 -1.20000 AFIX 0 C26 1 0.943055 0.532970 1.092804 11.00000 0.04365 0.06393 = 0.04193 0.01872 0.00468 0.02623 AFIX 23 H26A 2 0.911741 0.536191 1.136782 11.00000 -1.20000 H26B 2 0.982729 0.498798 1.104435 11.00000 -1.20000 AFIX 0 C27 1 1.014341 0.625031 1.091467 11.00000 0.04219 0.06210 = 0.03518 0.00707 0.00664 0.02929 AFIX 23 H27A 2 0.978071 0.662867 1.090448 11.00000 -1.20000 H27B 2 1.036923 0.623852 1.042433 11.00000 -1.20000 AFIX 0 C28 1 1.106542 0.664556 1.163396 11.00000 0.04707 0.05541 = 0.04654 0.00942 0.00617 0.02602 AFIX 23 H28A 2 1.083584 0.667980 1.212070 11.00000 -1.20000 H28B 2 1.140127 0.624599 1.165825 11.00000 -1.20000 AFIX 0 C29 1 1.182787 0.755031 1.162660 11.00000 0.06438 0.06097 = 0.07645 0.01030 0.01179 0.02195 AFIX 33 H29A 2 1.239396 0.776001 1.210365 11.00000 -1.50000 H29B 2 1.150836 0.795580 1.161677 11.00000 -1.50000 H29C 2 1.207539 0.752141 1.115463 11.00000 -1.50000 AFIX 0 C30 1 0.595980 0.264410 0.667804 11.00000 0.04484 0.04049 = 0.04092 0.00762 0.01517 0.02011 C31 1 0.539974 0.197641 0.624355 11.00000 0.05755 0.04599 = 0.04791 0.00656 0.01171 0.02262 C32 1 0.488256 0.296182 0.816947 11.00000 0.04014 0.04475 = 0.04192 0.00904 0.01789 0.01405 AFIX 23 H32A 2 0.472531 0.324150 0.772925 11.00000 -1.20000 H32B 2 0.436505 0.234597 0.804099 11.00000 -1.20000 AFIX 0 C33 1 0.607596 0.491967 0.919989 11.00000 0.03931 0.04934 = 0.02249 0.01086 0.01582 0.02112 C34 1 0.507734 0.430407 0.895997 11.00000 0.03651 0.03621 = 0.02924 0.00616 0.01230 0.01429 C35 1 0.427870 0.454370 0.882907 11.00000 0.03215 0.04902 = 0.03152 0.00922 0.01400 0.01270 C36 1 0.449413 0.543637 0.897827 11.00000 0.03311 0.04957 = 0.02967 0.01180 0.01474 0.01808 C37 1 0.549460 0.607939 0.922602 11.00000 0.03548 0.04222 = 0.02488 0.00520 0.01304 0.01338 C38 1 0.626383 0.580654 0.932337 11.00000 0.03433 0.04571 = 0.02369 0.01096 0.01337 0.01381 AFIX 43 H38 2 0.694305 0.623898 0.947975 11.00000 -1.20000 AFIX 0 C39 1 0.569729 0.704881 0.933382 11.00000 0.03400 0.04755 = 0.02932 0.00441 0.00914 0.01726 AFIX 13 H39 2 0.510741 0.709408 0.948421 11.00000 -1.20000 AFIX 0 C40 1 0.663573 0.767556 0.999251 11.00000 0.04482 0.04498 = 0.03047 0.00195 0.01047 0.01312 AFIX 23 H40A 2 0.660780 0.746335 1.049183 11.00000 -1.20000 H40B 2 0.724340 0.767681 0.985148 11.00000 -1.20000 AFIX 0 C41 1 0.672005 0.860848 1.012297 11.00000 0.05813 0.05314 = 0.05416 -0.00488 0.01397 0.01788 AFIX 23 H41A 2 0.684472 0.883973 0.964447 11.00000 -1.20000 H41B 2 0.606062 0.858093 1.016757 11.00000 -1.20000 AFIX 0 C42 1 0.752761 0.926210 1.084003 11.00000 0.06160 0.05739 = 0.05565 -0.01293 0.01365 0.01588 AFIX 23 H42A 2 0.817640 0.923225 1.084951 11.00000 -1.20000 H42B 2 0.761450 0.986370 1.079611 11.00000 -1.20000 AFIX 0 C43 1 0.726365 0.908261 1.159733 11.00000 0.09097 0.07346 = 0.05485 0.00718 0.01625 0.04317 PART 1 AFIX 23 H43A 2 0.723181 0.849766 1.165107 10.75000 -1.20000 H43B 2 0.657931 0.904809 1.155260 10.75000 -1.20000 AFIX 23 PART 0 PART 2 H43C 2 0.719327 0.849410 1.167636 10.25000 -1.20000 H43D 2 0.664351 0.914745 1.163120 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C44 1 0.798562 0.975782 1.237201 10.75000 0.11404 0.11334 = 0.04608 0.00069 0.03074 0.04334 AFIX 23 H44A 2 0.799596 1.034193 1.234759 10.75000 -1.20000 H44B 2 0.867884 0.981109 1.242658 10.75000 -1.20000 AFIX 0 C45 1 0.761897 0.944710 1.311015 10.75000 0.12093 0.12436 = 0.06772 0.00569 0.04306 0.03013 AFIX 33 H45A 2 0.807243 0.987755 1.359595 10.75000 -1.50000 H45B 2 0.762340 0.887457 1.313885 10.75000 -1.50000 H45C 2 0.693315 0.939605 1.305450 10.75000 -1.50000 AFIX 0 PART 0 PART 2 C44B 1 0.823494 0.984091 1.218817 10.25000 0.11701 0.11592 = 0.04628 -0.00277 0.03155 0.04940 AFIX 23 H44C 2 0.830758 1.043010 1.210967 10.25000 -1.20000 H44D 2 0.885556 0.977481 1.215853 10.25000 -1.20000 AFIX 0 C45B 1 0.793913 0.964335 1.298282 10.25000 0.11885 0.11415 = 0.05119 0.00029 0.04317 0.04562 AFIX 33 H45D 2 0.848305 1.005890 1.343810 10.25000 -1.50000 H45E 2 0.783480 0.904222 1.301967 10.25000 -1.50000 H45F 2 0.731648 0.970667 1.298244 10.25000 -1.50000 AFIX 0 PART 0 C46 1 0.325300 0.388322 0.851856 11.00000 0.03849 0.05117 = 0.03490 0.01321 0.01791 0.01838 C47 1 0.241942 0.335518 0.822886 11.00000 0.04085 0.05720 = 0.04239 0.01252 0.01806 0.02096 C48 1 0.339210 0.592136 0.820230 11.00000 0.03181 0.05064 = 0.04007 0.01283 0.01115 0.01886 AFIX 23 H48A 2 0.265480 0.573602 0.807330 11.00000 -1.20000 H48B 2 0.353395 0.561101 0.776392 11.00000 -1.20000 AFIX 0 C49 1 0.567565 0.727701 0.852776 11.00000 0.04137 0.03622 = 0.02957 0.00315 0.01013 0.01628 C50 1 0.475168 0.713054 0.800882 11.00000 0.03762 0.03990 = 0.03986 0.00857 0.01479 0.02104 C51 1 0.471213 0.732913 0.726225 11.00000 0.03857 0.04218 = 0.03501 0.00989 0.00993 0.01941 C52 1 0.559961 0.765469 0.701578 11.00000 0.03780 0.03784 = 0.03156 0.00864 0.00887 0.01770 C53 1 0.652552 0.779210 0.750164 11.00000 0.03541 0.03070 = 0.03051 0.00502 0.00865 0.01093 C54 1 0.653340 0.759149 0.825873 11.00000 0.03338 0.03724 = 0.02599 0.00280 0.00686 0.01272 AFIX 43 H54 2 0.715625 0.767610 0.859996 11.00000 -1.20000 AFIX 0 C55 1 0.745545 0.810241 0.720022 11.00000 0.03368 0.03728 = 0.02815 0.00670 0.01037 0.01229 AFIX 13 H55 2 0.735396 0.845651 0.680220 11.00000 -1.20000 AFIX 0 C56 1 0.843973 0.870201 0.783841 11.00000 0.03097 0.04078 = 0.03207 0.00858 0.00999 0.01239 AFIX 23 H56A 2 0.859520 0.835336 0.821531 11.00000 -1.20000 H56B 2 0.899547 0.890657 0.758061 11.00000 -1.20000 AFIX 0 C57 1 0.840524 0.950120 0.830197 11.00000 0.04722 0.03859 = 0.03925 -0.00016 0.01034 0.01457 AFIX 23 H57A 2 0.811354 0.978404 0.792628 11.00000 -1.20000 H57B 2 0.795996 0.930705 0.865484 11.00000 -1.20000 AFIX 0 C58 1 0.944503 1.016825 0.879712 11.00000 0.03739 0.04154 = 0.04278 0.00554 0.00725 0.00989 AFIX 23 H58A 2 0.979270 0.985504 0.908294 11.00000 -1.20000 H58B 2 0.984164 1.045055 0.843737 11.00000 -1.20000 AFIX 0 C59 1 0.943097 1.087716 0.939535 11.00000 0.04154 0.04170 = 0.03767 0.00188 0.00350 0.01222 AFIX 23 H59A 2 0.907118 1.060001 0.977656 11.00000 -1.20000 H59B 2 0.905095 1.117001 0.911495 11.00000 -1.20000 AFIX 0 C60 1 1.049000 1.157252 0.985511 11.00000 0.04594 0.05101 = 0.03801 0.00548 0.00857 0.01001 AFIX 23 H60A 2 1.088293 1.127791 1.011437 11.00000 -1.20000 H60B 2 1.083789 1.187329 0.947792 11.00000 -1.20000 AFIX 0 C61 1 1.046394 1.224893 1.047851 11.00000 0.06206 0.04682 = 0.03527 0.00481 0.00887 0.01655 AFIX 33 H61A 2 1.115426 1.267770 1.075547 11.00000 -1.50000 H61B 2 1.013314 1.195608 1.086023 11.00000 -1.50000 H61C 2 1.008755 1.255121 1.022368 11.00000 -1.50000 AFIX 0 C62 1 0.377090 0.720998 0.674888 11.00000 0.04659 0.05055 = 0.04445 0.01586 0.01786 0.02567 C63 1 0.300654 0.712256 0.632459 11.00000 0.03793 0.06807 = 0.04446 0.01185 0.01079 0.02975 C64 1 0.546757 0.722421 0.565449 11.00000 0.03351 0.04023 = 0.03319 0.00352 0.00501 0.01391 AFIX 23 H64A 2 0.513515 0.663559 0.576990 11.00000 -1.20000 H64B 2 0.504042 0.724318 0.515557 11.00000 -1.20000 AFIX 0 O9 4 -0.157105 0.481059 0.328097 11.00000 0.07715 0.08095 = 0.04516 0.00654 0.00854 0.02744 O10 4 -0.007427 0.636020 0.429688 11.00000 0.04778 0.07896 = 0.04975 0.00504 0.01770 0.01754 C65 1 -0.071616 0.532320 0.306290 11.00000 0.09204 0.09885 = 0.05599 0.00972 0.02866 0.04958 AFIX 23 H65A 2 -0.085014 0.575612 0.278325 11.00000 -1.20000 H65B 2 -0.055716 0.494367 0.269433 11.00000 -1.20000 AFIX 0 C66 1 0.011719 0.576980 0.373752 11.00000 0.06700 0.12808 = 0.08376 0.02664 0.04634 0.04978 AFIX 23 H66A 2 0.071924 0.611680 0.356740 11.00000 -1.20000 H66B 2 0.025975 0.533489 0.400848 11.00000 -1.20000 AFIX 0 C67 1 -0.096241 0.585033 0.452019 11.00000 0.05916 0.08709 = 0.05859 -0.00175 0.02580 0.02113 AFIX 23 H67A 2 -0.113863 0.624672 0.485443 11.00000 -1.20000 H67B 2 -0.082588 0.544483 0.483799 11.00000 -1.20000 AFIX 0 C68 1 -0.180086 0.534985 0.383257 11.00000 0.06787 0.13144 = 0.05329 0.00243 0.02763 0.03673 AFIX 23 H68A 2 -0.238293 0.496917 0.400669 11.00000 -1.20000 H68B 2 -0.199807 0.575900 0.355943 11.00000 -1.20000 AFIX 0 O11 4 0.611535 0.980610 0.783972 11.00000 0.10665 0.13609 = 0.10766 0.00812 0.02361 0.07170 O12 4 0.455626 0.989980 0.845830 11.00000 0.10201 0.12677 = 0.14805 0.00993 0.03890 0.05947 C69 1 0.624297 1.015895 0.861487 11.00000 0.09800 0.12396 = 0.10206 0.01805 0.02850 0.05675 AFIX 23 H69A 2 0.645676 1.079974 0.867308 11.00000 -1.20000 H69B 2 0.679925 1.007437 0.895031 11.00000 -1.20000 AFIX 0 C70 1 0.535772 0.979835 0.892157 11.00000 0.09905 0.11965 = 0.12451 0.02398 0.03444 0.04768 AFIX 23 H70A 2 0.516684 0.916718 0.891317 11.00000 -1.20000 H70B 2 0.552004 1.010741 0.947743 11.00000 -1.20000 AFIX 0 C71 1 0.435862 0.945828 0.769857 11.00000 0.11023 0.14071 = 0.14466 0.01193 0.01174 0.07270 AFIX 23 H71A 2 0.377238 0.949665 0.735663 11.00000 -1.20000 H71B 2 0.418643 0.883020 0.769291 11.00000 -1.20000 AFIX 0 C72 1 0.528312 0.985245 0.736762 11.00000 0.11475 0.14260 = 0.12441 0.01556 0.01218 0.07524 AFIX 23 H72A 2 0.512790 0.952548 0.681962 11.00000 -1.20000 H72B 2 0.543716 1.047336 0.735091 11.00000 -1.20000 AFIX 0 PART 1 O13 4 0.269613 -0.047491 0.439369 10.50000 0.06830 0.06089 = 0.09803 0.01216 -0.01861 0.01506 O14 4 0.098592 -0.152002 0.317287 10.50000 0.06411 0.06511 = 0.11100 0.00688 -0.00263 0.00686 C73 1 0.229059 -0.007310 0.384609 10.50000 0.06516 0.06004 = 0.10204 0.01463 -0.01230 0.01749 AFIX 23 H73A 2 0.267844 0.004703 0.344598 10.50000 -1.20000 H73B 2 0.236049 0.049580 0.412955 10.50000 -1.20000 AFIX 0 C74 1 0.118840 -0.064832 0.342996 10.50000 0.06088 0.05986 = 0.10720 0.01293 -0.00448 0.00863 AFIX 23 H74A 2 0.077793 -0.061554 0.379778 10.50000 -1.20000 H74B 2 0.098282 -0.041634 0.296781 10.50000 -1.20000 AFIX 0 C75 1 0.147816 -0.169467 0.386119 10.50000 0.06679 0.06686 = 0.11310 0.01106 -0.00395 0.00621 AFIX 23 H75A 2 0.124564 -0.233684 0.380891 10.50000 -1.20000 H75B 2 0.131357 -0.146460 0.433021 10.50000 -1.20000 AFIX 0 C76 1 0.256667 -0.127398 0.396501 10.50000 0.06708 0.06208 = 0.10521 0.00579 -0.00656 0.00761 AFIX 23 H76A 2 0.292785 -0.156092 0.427691 10.50000 -1.20000 H76B 2 0.274762 -0.122425 0.345651 10.50000 -1.20000 AFIX 0 PART 0 PART 2 O13B 4 0.303710 -0.053102 0.420715 10.50000 0.06791 0.06046 = 0.10028 0.01724 -0.01989 0.00750 O14B 4 0.108556 -0.132171 0.317942 10.50000 0.06320 0.06591 = 0.11183 0.00782 -0.00335 0.00703 C73B 1 0.255354 -0.024523 0.359653 10.50000 0.07261 0.06909 = 0.10609 0.01782 -0.01769 0.00708 AFIX 23 H73C 2 0.260604 -0.050857 0.308575 10.50000 -1.20000 H73D 2 0.293186 0.039991 0.368031 10.50000 -1.20000 AFIX 0 C74B 1 0.148332 -0.044851 0.352034 10.50000 0.06942 0.06431 = 0.10614 0.01453 -0.00990 0.01169 AFIX 23 H74C 2 0.134833 -0.034732 0.404164 10.50000 -1.20000 H74D 2 0.124207 -0.011531 0.317050 10.50000 -1.20000 AFIX 0 C75B 1 0.143555 -0.187357 0.356201 10.50000 0.06388 0.06066 = 0.10642 0.00336 -0.00258 0.00938 AFIX 23 H75C 2 0.134060 -0.237365 0.315434 10.50000 -1.20000 H75D 2 0.100949 -0.211622 0.391707 10.50000 -1.20000 AFIX 0 C76B 1 0.251178 -0.145014 0.403776 10.50000 0.06580 0.06137 = 0.10543 0.00715 -0.00645 0.00831 AFIX 23 H76C 2 0.254030 -0.163948 0.454983 10.50000 -1.20000 H76D 2 0.288738 -0.169313 0.375647 10.50000 -1.20000 AFIX 0 PART 0 PART 1 O15 4 0.867186 0.866610 0.574585 10.35000 0.08562 0.08144 = 0.08843 0.03179 0.03227 0.03435 O16 4 0.958100 0.822209 0.464579 10.35000 0.08015 0.07930 = 0.07874 0.03064 0.04470 0.03591 C77 1 0.834764 0.872821 0.494946 10.35000 0.08477 0.08156 = 0.08604 0.03653 0.03348 0.03259 AFIX 23 H77A 2 0.872855 0.932699 0.487253 10.35000 -1.20000 H77B 2 0.761899 0.858347 0.480062 10.35000 -1.20000 AFIX 0 C78 1 0.855481 0.808844 0.448499 10.35000 0.08433 0.08005 = 0.07982 0.03551 0.03891 0.03633 AFIX 23 H78A 2 0.815045 0.750014 0.457139 10.35000 -1.20000 H78B 2 0.831674 0.808193 0.391696 10.35000 -1.20000 AFIX 0 C79 1 0.992268 0.831614 0.548947 10.35000 0.08120 0.07922 = 0.08610 0.02308 0.03058 0.04283 AFIX 23 H79A 2 1.065322 0.847075 0.565486 10.35000 -1.20000 H79B 2 0.955180 0.776545 0.565315 10.35000 -1.20000 AFIX 0 C80 1 0.970979 0.902930 0.583525 10.35000 0.08193 0.08123 = 0.08471 0.02980 0.03496 0.03686 AFIX 23 H80A 2 1.008251 0.925552 0.640327 10.35000 -1.20000 H80B 2 0.991090 0.951908 0.555483 10.35000 -1.20000 AFIX 0 PART 0 PART 2 O15B 4 0.874157 0.889588 0.577640 10.35000 0.08696 0.08318 = 0.08787 0.03257 0.03167 0.03326 O16B 4 0.916566 0.790622 0.470619 10.35000 0.09095 0.08341 = 0.08319 0.03157 0.03298 0.03531 C77B 1 0.826320 0.850687 0.493064 10.35000 0.08599 0.08346 = 0.08364 0.03753 0.03769 0.03059 AFIX 23 H77C 2 0.758507 0.849659 0.484933 10.35000 -1.20000 H77D 2 0.863214 0.896700 0.466503 10.35000 -1.20000 AFIX 0 C78B 1 0.808264 0.768869 0.442019 10.35000 0.07711 0.07579 = 0.06654 0.04605 0.05042 0.04082 AFIX 23 H78C 2 0.785702 0.766689 0.384704 10.35000 -1.20000 H78D 2 0.763520 0.715445 0.456653 10.35000 -1.20000 AFIX 0 C79B 1 0.948130 0.799717 0.559227 10.35000 0.07710 0.07188 = 0.07721 0.02999 0.04001 0.04374 AFIX 23 H79C 2 0.894536 0.752770 0.574373 10.35000 -1.20000 H79D 2 1.009936 0.790112 0.572891 10.35000 -1.20000 AFIX 0 C80B 1 0.967584 0.883929 0.606165 10.35000 0.08275 0.08237 = 0.08337 0.03160 0.03363 0.03661 AFIX 23 H80C 2 0.981912 0.884232 0.663574 10.35000 -1.20000 H80D 2 1.024566 0.932632 0.596130 10.35000 -1.20000 AFIX 0 PART 0 PART 3 O17 4 0.969489 0.917485 0.461098 10.30000 0.08641 0.03077 = 0.07875 0.00564 0.04311 0.01344 HKLF 4 REM l1+k3 in P -1 REM R1 = 0.0728 for 11795 Fo > 4sig(Fo) and 0.0818 for all 13955 data REM 1036 parameters refined using 433 restraints END WGHT 0.1398 7.2361 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y+1, -z+1 HTAB C48 O9_$1 HTAB C65 I3_$1 EQIV $2 x-1, y, z HTAB C68 O2_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C73 O15_$3 EQIV $4 x-1, y-1, z HTAB C75 O16_$4 EQIV $5 x, y-1, z HTAB C76B I4_$5 REM Highest difference peak 4.521, deepest hole -1.678, 1-sigma level 0.177 Q1 1 0.3810 0.0879 0.5508 11.00000 0.05 4.52 Q2 1 0.5242 0.4620 0.3013 11.00000 0.05 2.66 Q3 1 0.1344 0.2169 0.7702 11.00000 0.05 2.43 Q4 1 0.4335 0.5127 0.3000 11.00000 0.05 2.26 Q5 1 0.1229 0.7189 0.5597 11.00000 0.05 2.04 Q6 1 0.0418 0.2659 0.7706 11.00000 0.05 2.03 Q7 1 0.2241 0.6696 0.5590 11.00000 0.05 1.90 Q8 1 0.4967 0.0583 0.5404 11.00000 0.05 1.85 Q9 1 0.5243 0.5125 0.2839 11.00000 0.05 1.51 Q10 1 0.7280 0.7455 0.3708 11.00000 0.05 1.29 Q11 1 0.8817 0.8403 0.5163 11.00000 0.05 1.29 Q12 1 0.5328 1.0886 0.7838 11.00000 0.05 1.08 Q13 1 0.8093 0.9292 0.4118 11.00000 0.05 0.99 Q14 1 -0.1181 0.6150 0.4100 11.00000 0.05 0.91 Q15 1 0.4338 0.5128 0.2400 11.00000 0.05 0.90 Q16 1 0.1134 0.6661 0.5895 11.00000 0.05 0.88 Q17 1 0.3978 0.1065 0.4897 11.00000 0.05 0.85 Q18 1 0.4360 0.4602 0.3269 11.00000 0.05 0.81 Q19 1 0.1964 -0.0778 0.3166 11.00000 0.05 0.81 Q20 1 0.5283 0.4685 0.3691 11.00000 0.05 0.79 Q21 1 0.8965 0.8550 0.4458 11.00000 0.05 0.77 Q22 1 0.2213 0.6733 0.6068 11.00000 0.05 0.75 Q23 1 0.7553 0.8853 1.1178 11.00000 0.05 0.72 Q24 1 0.2212 0.7182 0.5234 11.00000 0.05 0.71 Q25 1 0.4931 0.0659 0.5990 11.00000 0.05 0.71 ; _shelx_res_checksum 28465 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.47930(3) 0.48789(3) 0.30155(2) 0.04176(14) Uani 1 1 d . . . . . I2 I 0.44091(5) 0.08604(3) 0.54658(3) 0.06093(18) Uani 1 1 d . . . . . I3 I 0.09887(3) 0.24603(4) 0.76939(3) 0.05331(16) Uani 1 1 d . . . . . I4 I 0.17083(4) 0.69303(4) 0.55679(3) 0.05576(17) Uani 1 1 d . . . . . O1 O 0.6420(3) 0.7345(3) 0.5546(3) 0.0385(10) Uani 1 1 d . . . . . O2 O 0.7512(3) 0.5062(3) 0.5496(2) 0.0367(9) Uani 1 1 d . . . . . O3 O 0.7426(3) 0.3947(3) 0.6204(2) 0.0359(9) Uani 1 1 d . . . . . O4 O 0.5847(4) 0.2966(3) 0.8228(3) 0.0405(10) Uani 1 1 d . . . . . O5 O 0.4833(4) 0.3410(3) 0.8877(3) 0.0407(10) Uani 1 1 d . . . . . O6 O 0.3701(3) 0.5668(3) 0.8914(3) 0.0391(10) Uani 1 1 d . . . . . O7 O 0.3886(3) 0.6844(3) 0.8254(3) 0.0395(10) Uani 1 1 d . . . . . O8 O 0.5535(4) 0.7871(3) 0.6281(3) 0.0398(10) Uani 1 1 d . . . . . C1 C 0.7499(5) 0.7299(4) 0.6753(4) 0.0338(13) Uani 1 1 d . . . . . C2 C 0.6928(5) 0.6932(4) 0.5971(4) 0.0356(13) Uani 1 1 d . . . . . C3 C 0.6902(5) 0.6166(5) 0.5551(4) 0.0370(13) Uani 1 1 d . . . . . C4 C 0.7489(5) 0.5776(4) 0.5939(4) 0.0355(13) Uani 1 1 d . . . . . C5 C 0.8072(4) 0.6134(5) 0.6721(4) 0.0349(13) Uani 1 1 d . . . . . C6 C 0.8047(4) 0.6890(4) 0.7114(4) 0.0347(13) Uani 1 1 d . . . . . H6 H 0.8424 0.7131 0.7653 0.042 Uiso 1 1 calc R U . . . C7 C 0.8656(5) 0.5674(5) 0.7143(4) 0.0362(13) Uani 1 1 d . . . . . H7 H 0.8851 0.5373 0.6728 0.043 Uiso 1 1 calc R U . . . C8 C 0.9637(5) 0.6296(5) 0.7771(4) 0.0374(13) Uani 1 1 d . . . . . H8A H 0.9921 0.5941 0.8056 0.045 Uiso 1 1 calc R U . . . H8B H 0.9479 0.6653 0.8162 0.045 Uiso 1 1 calc R U . . . C9 C 1.0439(6) 0.6918(6) 0.7423(5) 0.0513(18) Uani 1 1 d . . . . . H9A H 1.0692 0.6569 0.7112 0.062 Uiso 1 1 calc R U . . . H9B H 1.0118 0.7189 0.7055 0.062 Uiso 1 1 calc R U . . . C10 C 1.1331(6) 0.7646(6) 0.8054(6) 0.057(2) Uani 1 1 d . . . . . H10A H 1.1813 0.8010 0.7785 0.068 Uiso 1 1 calc R U . . . H10B H 1.1082 0.8028 0.8325 0.068 Uiso 1 1 calc R U . . . C11 C 1.1895(6) 0.7340(6) 0.8677(5) 0.056(2) Uani 1 1 d . . . . . H11A H 1.1423 0.7000 0.8965 0.067 Uiso 1 1 calc R U . . . H11B H 1.2121 0.6937 0.8406 0.067 Uiso 1 1 calc R U . . . C12 C 1.2800(7) 0.8068(7) 0.9273(7) 0.075(3) Uani 1 1 d . . . . . H12A H 1.3260 0.8422 0.8983 0.090 Uiso 1 1 calc R U . . . H12B H 1.2570 0.8458 0.9557 0.090 Uiso 1 1 calc R U . . . C13 C 1.3384(7) 0.7760(8) 0.9875(6) 0.073(3) Uani 1 1 d . . . . . H13A H 1.3956 0.8270 1.0237 0.110 Uiso 1 1 calc R U . . . H13B H 1.3632 0.7386 0.9602 0.110 Uiso 1 1 calc R U . . . H13C H 1.2942 0.7424 1.0178 0.110 Uiso 1 1 calc R U . . . C14 C 0.6271(5) 0.5769(5) 0.4761(4) 0.0363(13) Uani 1 1 d . . . . . C15 C 0.5715(5) 0.5437(5) 0.4103(4) 0.0406(14) Uani 1 1 d . . . . . C16 C 0.6907(5) 0.4216(5) 0.5606(4) 0.0391(14) Uani 1 1 d . . . . . H16A H 0.6303 0.4226 0.5746 0.047 Uiso 1 1 calc R U . . . H16B H 0.6675 0.3782 0.5101 0.047 Uiso 1 1 calc R U . . . C17 C 0.7935(5) 0.4960(5) 0.7453(4) 0.0341(13) Uani 1 1 d . . . . . C18 C 0.7325(5) 0.4139(5) 0.6968(4) 0.0366(13) Uani 1 1 d . . . . . C19 C 0.6610(5) 0.3469(5) 0.7206(4) 0.0382(13) Uani 1 1 d . . . . . C20 C 0.6520(5) 0.3646(4) 0.7983(4) 0.0357(13) Uani 1 1 d . . . . . C21 C 0.7108(5) 0.4462(4) 0.8493(4) 0.0335(12) Uani 1 1 d . . . . . C22 C 0.7808(5) 0.5110(5) 0.8222(4) 0.0340(13) Uani 1 1 d . . . . . H22 H 0.8213 0.5670 0.8565 0.041 Uiso 1 1 calc R U . . . C23 C 0.6921(5) 0.4626(4) 0.9302(4) 0.0344(13) Uani 1 1 d . . . . . H23 H 0.6659 0.4044 0.9457 0.041 Uiso 1 1 calc R U . . . C24 C 0.7869(5) 0.5244(5) 0.9967(4) 0.0368(13) Uani 1 1 d . . . . . H24A H 0.8211 0.5799 0.9800 0.044 Uiso 1 1 calc R U . . . H24B H 0.7668 0.5386 1.0448 0.044 Uiso 1 1 calc R U . . . C25 C 0.8594(6) 0.4833(5) 1.0164(5) 0.0480(17) Uani 1 1 d . . . . . H25A H 0.8903 0.4808 0.9720 0.058 Uiso 1 1 calc R U . . . H25B H 0.8212 0.4222 1.0213 0.058 Uiso 1 1 calc R U . . . C26 C 0.9431(6) 0.5330(6) 1.0928(5) 0.0492(17) Uani 1 1 d . . . . . H26A H 0.9117 0.5362 1.1368 0.059 Uiso 1 1 calc R U . . . H26B H 0.9827 0.4988 1.1044 0.059 Uiso 1 1 calc R U . . . C27 C 1.0143(5) 0.6250(5) 1.0915(4) 0.0451(16) Uani 1 1 d . . . . . H27A H 0.9781 0.6629 1.0904 0.054 Uiso 1 1 calc R U . . . H27B H 1.0369 0.6239 1.0424 0.054 Uiso 1 1 calc R U . . . C28 C 1.1065(6) 0.6646(5) 1.1634(5) 0.0495(17) Uani 1 1 d . . . . . H28A H 1.0836 0.6680 1.2121 0.059 Uiso 1 1 calc R U . . . H28B H 1.1401 0.6246 1.1658 0.059 Uiso 1 1 calc R U . . . C29 C 1.1828(8) 0.7550(7) 1.1627(7) 0.070(2) Uani 1 1 d . . . . . H29A H 1.2394 0.7760 1.2104 0.106 Uiso 1 1 calc R U . . . H29B H 1.1508 0.7956 1.1617 0.106 Uiso 1 1 calc R U . . . H29C H 1.2075 0.7521 1.1155 0.106 Uiso 1 1 calc R U . . . C30 C 0.5960(5) 0.2644(5) 0.6678(4) 0.0410(14) Uani 1 1 d . . . . . C31 C 0.5400(6) 0.1976(5) 0.6244(5) 0.0510(17) Uani 1 1 d . . . . . C32 C 0.4883(5) 0.2962(5) 0.8169(4) 0.0426(15) Uani 1 1 d . . . . . H32A H 0.4725 0.3241 0.7729 0.051 Uiso 1 1 calc R U . . . H32B H 0.4365 0.2346 0.8041 0.051 Uiso 1 1 calc R U . . . C33 C 0.6076(5) 0.4920(5) 0.9200(3) 0.0349(13) Uani 1 1 d . . . . . C34 C 0.5077(5) 0.4304(4) 0.8960(4) 0.0339(12) Uani 1 1 d . . . . . C35 C 0.4279(5) 0.4544(5) 0.8829(4) 0.0382(14) Uani 1 1 d . . . . . C36 C 0.4494(5) 0.5436(5) 0.8978(4) 0.0360(13) Uani 1 1 d . . . . . C37 C 0.5495(5) 0.6079(4) 0.9226(3) 0.0347(13) Uani 1 1 d . . . . . C38 C 0.6264(5) 0.5807(4) 0.9323(3) 0.0345(13) Uani 1 1 d . . . . . H38 H 0.6943 0.6239 0.9480 0.041 Uiso 1 1 calc R U . . . C39 C 0.5697(5) 0.7049(5) 0.9334(4) 0.0373(13) Uani 1 1 d . . . . . H39 H 0.5107 0.7094 0.9484 0.045 Uiso 1 1 calc R U . . . C40 C 0.6636(5) 0.7676(5) 0.9993(4) 0.0426(15) Uani 1 1 d . . . . . H40A H 0.6608 0.7463 1.0492 0.051 Uiso 1 1 calc R U . . . H40B H 0.7243 0.7677 0.9851 0.051 Uiso 1 1 calc R U . . . C41 C 0.6720(7) 0.8608(6) 1.0123(5) 0.059(2) Uani 1 1 d . . . . . H41A H 0.6845 0.8840 0.9644 0.070 Uiso 1 1 calc R U . . . H41B H 0.6061 0.8581 1.0168 0.070 Uiso 1 1 calc R U . . . C42 C 0.7528(7) 0.9262(6) 1.0840(5) 0.064(2) Uani 1 1 d . . . . . H42A H 0.8176 0.9232 1.0850 0.077 Uiso 1 1 calc R U . . . H42B H 0.7614 0.9864 1.0796 0.077 Uiso 1 1 calc R U . . . C43 C 0.7264(9) 0.9083(7) 1.1597(6) 0.072(3) Uani 1 1 d D . . . . H43A H 0.7232 0.8498 1.1651 0.086 Uiso 0.75 1 calc R U P A 1 H43B H 0.6579 0.9048 1.1553 0.086 Uiso 0.75 1 calc R U P A 1 H43C H 0.7193 0.8494 1.1676 0.086 Uiso 0.25 1 calc R U P B 2 H43D H 0.6644 0.9147 1.1631 0.086 Uiso 0.25 1 calc R U P B 2 C44 C 0.7986(16) 0.9758(15) 1.2372(9) 0.093(5) Uani 0.75 1 d D U P C 1 H44A H 0.7996 1.0342 1.2348 0.111 Uiso 0.75 1 calc R U P C 1 H44B H 0.8679 0.9811 1.2427 0.111 Uiso 0.75 1 calc R U P C 1 C45 C 0.762(2) 0.9447(19) 1.3110(14) 0.110(6) Uani 0.75 1 d D U P C 1 H45A H 0.8072 0.9878 1.3596 0.165 Uiso 0.75 1 calc R U P C 1 H45B H 0.7623 0.8875 1.3139 0.165 Uiso 0.75 1 calc R U P C 1 H45C H 0.6933 0.9396 1.3054 0.165 Uiso 0.75 1 calc R U P C 1 C44B C 0.823(4) 0.984(5) 1.219(3) 0.093(8) Uani 0.25 1 d D U P C 2 H44C H 0.8308 1.0430 1.2110 0.112 Uiso 0.25 1 calc R U P C 2 H44D H 0.8856 0.9775 1.2159 0.112 Uiso 0.25 1 calc R U P C 2 C45B C 0.794(6) 0.964(5) 1.298(4) 0.094(9) Uani 0.25 1 d D U P C 2 H45D H 0.8483 1.0059 1.3438 0.142 Uiso 0.25 1 calc R U P C 2 H45E H 0.7835 0.9042 1.3020 0.142 Uiso 0.25 1 calc R U P C 2 H45F H 0.7316 0.9707 1.2982 0.142 Uiso 0.25 1 calc R U P C 2 C46 C 0.3253(5) 0.3883(5) 0.8519(4) 0.0402(15) Uani 1 1 d . . . . . C47 C 0.2419(6) 0.3355(5) 0.8229(4) 0.0456(16) Uani 1 1 d . . . . . C48 C 0.3392(5) 0.5921(5) 0.8202(4) 0.0399(14) Uani 1 1 d . . . . . H48A H 0.2655 0.5736 0.8073 0.048 Uiso 1 1 calc R U . . . H48B H 0.3534 0.5611 0.7764 0.048 Uiso 1 1 calc R U . . . C49 C 0.5676(5) 0.7277(4) 0.8528(4) 0.0361(13) Uani 1 1 d . . . . . C50 C 0.4752(5) 0.7131(4) 0.8009(4) 0.0370(13) Uani 1 1 d . . . . . C51 C 0.4712(5) 0.7329(5) 0.7262(4) 0.0377(13) Uani 1 1 d . . . . . C52 C 0.5600(5) 0.7655(4) 0.7016(4) 0.0352(13) Uani 1 1 d . . . . . C53 C 0.6526(5) 0.7792(4) 0.7502(4) 0.0334(12) Uani 1 1 d . . . . . C54 C 0.6533(5) 0.7591(4) 0.8259(4) 0.0335(12) Uani 1 1 d . . . . . H54 H 0.7156 0.7676 0.8600 0.040 Uiso 1 1 calc R U . . . C55 C 0.7455(5) 0.8102(4) 0.7200(4) 0.0337(12) Uani 1 1 d . . . . . H55 H 0.7354 0.8457 0.6802 0.040 Uiso 1 1 calc R U . . . C56 C 0.8440(5) 0.8702(4) 0.7838(4) 0.0353(13) Uani 1 1 d . . . . . H56A H 0.8595 0.8353 0.8215 0.042 Uiso 1 1 calc R U . . . H56B H 0.8995 0.8907 0.7581 0.042 Uiso 1 1 calc R U . . . C57 C 0.8405(6) 0.9501(5) 0.8302(4) 0.0439(15) Uani 1 1 d . . . . . H57A H 0.8114 0.9784 0.7926 0.053 Uiso 1 1 calc R U . . . H57B H 0.7960 0.9307 0.8655 0.053 Uiso 1 1 calc R U . . . C58 C 0.9445(5) 1.0168(5) 0.8797(4) 0.0438(15) Uani 1 1 d . . . . . H58A H 0.9793 0.9855 0.9083 0.053 Uiso 1 1 calc R U . . . H58B H 0.9842 1.0451 0.8437 0.053 Uiso 1 1 calc R U . . . C59 C 0.9431(5) 1.0877(5) 0.9395(4) 0.0439(15) Uani 1 1 d . . . . . H59A H 0.9071 1.0600 0.9777 0.053 Uiso 1 1 calc R U . . . H59B H 0.9051 1.1170 0.9115 0.053 Uiso 1 1 calc R U . . . C60 C 1.0490(6) 1.1573(5) 0.9855(4) 0.0493(17) Uani 1 1 d . . . . . H60A H 1.0883 1.1278 1.0114 0.059 Uiso 1 1 calc R U . . . H60B H 1.0838 1.1873 0.9478 0.059 Uiso 1 1 calc R U . . . C61 C 1.0464(7) 1.2249(5) 1.0479(4) 0.0513(18) Uani 1 1 d . . . . . H61A H 1.1154 1.2678 1.0755 0.077 Uiso 1 1 calc R U . . . H61B H 1.0133 1.1956 1.0860 0.077 Uiso 1 1 calc R U . . . H61C H 1.0088 1.2551 1.0224 0.077 Uiso 1 1 calc R U . . . C62 C 0.3771(6) 0.7210(5) 0.6749(4) 0.0442(15) Uani 1 1 d . . . . . C63 C 0.3007(5) 0.7123(6) 0.6325(5) 0.0479(17) Uani 1 1 d . . . . . C64 C 0.5468(5) 0.7224(4) 0.5654(4) 0.0373(13) Uani 1 1 d . . . . . H64A H 0.5135 0.6636 0.5770 0.045 Uiso 1 1 calc R U . . . H64B H 0.5040 0.7243 0.5156 0.045 Uiso 1 1 calc R U . . . O9 O -0.1571(6) 0.4811(5) 0.3281(4) 0.0717(17) Uani 1 1 d . . . . . O10 O -0.0074(4) 0.6360(5) 0.4297(4) 0.0620(15) Uani 1 1 d . . . . . C65 C -0.0716(9) 0.5323(9) 0.3063(6) 0.079(3) Uani 1 1 d . . . . . H65A H -0.0850 0.5756 0.2783 0.094 Uiso 1 1 calc R U . . . H65B H -0.0557 0.4944 0.2694 0.094 Uiso 1 1 calc R U . . . C66 C 0.0117(9) 0.5770(10) 0.3738(7) 0.086(3) Uani 1 1 d . . . . . H66A H 0.0719 0.6117 0.3567 0.103 Uiso 1 1 calc R U . . . H66B H 0.0260 0.5335 0.4008 0.103 Uiso 1 1 calc R U . . . C67 C -0.0962(7) 0.5850(8) 0.4520(6) 0.072(3) Uani 1 1 d . . . . . H67A H -0.1139 0.6247 0.4854 0.086 Uiso 1 1 calc R U . . . H67B H -0.0826 0.5445 0.4838 0.086 Uiso 1 1 calc R U . . . C68 C -0.1801(9) 0.5350(10) 0.3833(6) 0.086(4) Uani 1 1 d . . . . . H68A H -0.2383 0.4969 0.4007 0.103 Uiso 1 1 calc R U . . . H68B H -0.1998 0.5759 0.3559 0.103 Uiso 1 1 calc R U . . . O11 O 0.6115(8) 0.9806(8) 0.7840(7) 0.113(3) Uani 1 1 d . U . . . O12 O 0.4556(9) 0.9900(8) 0.8458(8) 0.123(3) Uani 1 1 d . U . . . C69 C 0.6243(12) 1.0159(12) 0.8615(9) 0.105(3) Uani 1 1 d . U . . . H69A H 0.6457 1.0800 0.8673 0.126 Uiso 1 1 calc R U . . . H69B H 0.6799 1.0074 0.8950 0.126 Uiso 1 1 calc R U . . . C70 C 0.5358(12) 0.9798(12) 0.8922(11) 0.114(4) Uani 1 1 d . U . . . H70A H 0.5167 0.9167 0.8913 0.136 Uiso 1 1 calc R U . . . H70B H 0.5520 1.0107 0.9477 0.136 Uiso 1 1 calc R U . . . C71 C 0.4359(14) 0.9458(14) 0.7699(12) 0.131(4) Uani 1 1 d . U . . . H71A H 0.3772 0.9497 0.7357 0.157 Uiso 1 1 calc R U . . . H71B H 0.4186 0.8830 0.7693 0.157 Uiso 1 1 calc R U . . . C72 C 0.5283(13) 0.9852(14) 0.7368(11) 0.125(4) Uani 1 1 d . U . . . H72A H 0.5128 0.9525 0.6820 0.150 Uiso 1 1 calc R U . . . H72B H 0.5437 1.0473 0.7351 0.150 Uiso 1 1 calc R U . . . O13 O 0.2696(13) -0.0475(12) 0.4394(11) 0.087(4) Uani 0.5 1 d D U P D 1 O14 O 0.099(2) -0.1520(12) 0.3173(18) 0.092(3) Uani 0.5 1 d D U P D 1 C73 C 0.2291(16) -0.0073(15) 0.3846(16) 0.085(4) Uani 0.5 1 d D U P D 1 H73A H 0.2678 0.0047 0.3446 0.101 Uiso 0.5 1 calc R U P D 1 H73B H 0.2360 0.0496 0.4130 0.101 Uiso 0.5 1 calc R U P D 1 C74 C 0.1188(16) -0.0648(14) 0.343(2) 0.086(4) Uani 0.5 1 d D U P D 1 H74A H 0.0778 -0.0616 0.3798 0.104 Uiso 0.5 1 calc R U P D 1 H74B H 0.0983 -0.0416 0.2968 0.104 Uiso 0.5 1 calc R U P D 1 C75 C 0.1478(19) -0.1695(18) 0.3861(17) 0.095(4) Uani 0.5 1 d D U P D 1 H75A H 0.1246 -0.2337 0.3809 0.114 Uiso 0.5 1 calc R U P D 1 H75B H 0.1314 -0.1465 0.4330 0.114 Uiso 0.5 1 calc R U P D 1 C76 C 0.257(2) -0.1274(14) 0.397(2) 0.091(4) Uani 0.5 1 d D U P D 1 H76A H 0.2928 -0.1561 0.4277 0.109 Uiso 0.5 1 calc R U P D 1 H76B H 0.2748 -0.1224 0.3457 0.109 Uiso 0.5 1 calc R U P D 1 O13B O 0.3037(12) -0.0531(12) 0.4207(12) 0.090(4) Uani 0.5 1 d D U P E 2 O14B O 0.1086(19) -0.1322(12) 0.318(2) 0.092(3) Uani 0.5 1 d D U P E 2 C73B C 0.2554(17) -0.0245(18) 0.3597(17) 0.097(4) Uani 0.5 1 d D U P E 2 H73C H 0.2606 -0.0509 0.3086 0.116 Uiso 0.5 1 calc R U P E 2 H73D H 0.2932 0.0400 0.3680 0.116 Uiso 0.5 1 calc R U P E 2 C74B C 0.1483(16) -0.0449(15) 0.352(2) 0.091(4) Uani 0.5 1 d D U P E 2 H74C H 0.1348 -0.0347 0.4042 0.109 Uiso 0.5 1 calc R U P E 2 H74D H 0.1242 -0.0115 0.3171 0.109 Uiso 0.5 1 calc R U P E 2 C75B C 0.1436(19) -0.1874(15) 0.3562(17) 0.088(4) Uani 0.5 1 d D U P E 2 H75C H 0.1341 -0.2374 0.3154 0.106 Uiso 0.5 1 calc R U P E 2 H75D H 0.1009 -0.2116 0.3917 0.106 Uiso 0.5 1 calc R U P E 2 C76B C 0.251(2) -0.1450(14) 0.404(2) 0.089(4) Uani 0.5 1 d D U P E 2 H76C H 0.2540 -0.1639 0.4550 0.107 Uiso 0.5 1 calc R U P E 2 H76D H 0.2887 -0.1693 0.3756 0.107 Uiso 0.5 1 calc R U P E 2 O15 O 0.867(2) 0.8666(19) 0.5746(15) 0.083(4) Uani 0.35 1 d D U P F 1 O16 O 0.9581(16) 0.8222(15) 0.4646(12) 0.074(4) Uani 0.35 1 d D U P F 1 C77 C 0.835(4) 0.873(2) 0.4949(17) 0.082(4) Uani 0.35 1 d D U P F 1 H77A H 0.8729 0.9327 0.4873 0.098 Uiso 0.35 1 calc R U P F 1 H77B H 0.7619 0.8583 0.4801 0.098 Uiso 0.35 1 calc R U P F 1 C78 C 0.8555(19) 0.809(2) 0.448(2) 0.077(4) Uani 0.35 1 d D U P F 1 H78A H 0.8150 0.7500 0.4571 0.092 Uiso 0.35 1 calc R U P F 1 H78B H 0.8317 0.8082 0.3917 0.092 Uiso 0.35 1 calc R U P F 1 C79 C 0.992(3) 0.832(2) 0.5489(14) 0.078(4) Uani 0.35 1 d D U P F 1 H79A H 1.0653 0.8471 0.5655 0.093 Uiso 0.35 1 calc R U P F 1 H79B H 0.9552 0.7765 0.5653 0.093 Uiso 0.35 1 calc R U P F 1 C80 C 0.971(2) 0.9029(19) 0.584(2) 0.079(4) Uani 0.35 1 d D U P F 1 H80A H 1.0083 0.9256 0.6403 0.095 Uiso 0.35 1 calc R U P F 1 H80B H 0.9911 0.9519 0.5555 0.095 Uiso 0.35 1 calc R U P F 1 O15B O 0.874(2) 0.8896(18) 0.5776(15) 0.085(4) Uani 0.35 1 d D U P G 2 O16B O 0.9166(16) 0.7906(16) 0.4706(12) 0.084(4) Uani 0.35 1 d D U P G 2 C77B C 0.826(3) 0.851(2) 0.4931(16) 0.082(4) Uani 0.35 1 d D U P G 2 H77C H 0.7585 0.8497 0.4849 0.099 Uiso 0.35 1 calc R U P G 2 H77D H 0.8632 0.8967 0.4665 0.099 Uiso 0.35 1 calc R U P G 2 C78B C 0.8083(16) 0.7689(16) 0.4420(14) 0.063(4) Uani 0.35 1 d D U P G 2 H78C H 0.7857 0.7667 0.3847 0.075 Uiso 0.35 1 calc R U P G 2 H78D H 0.7635 0.7154 0.4567 0.075 Uiso 0.35 1 calc R U P G 2 C79B C 0.948(2) 0.7997(19) 0.5592(13) 0.067(4) Uani 0.35 1 d D U P G 2 H79C H 0.8945 0.7528 0.5744 0.081 Uiso 0.35 1 calc R U P G 2 H79D H 1.0099 0.7901 0.5729 0.081 Uiso 0.35 1 calc R U P G 2 C80B C 0.968(2) 0.8839(19) 0.6062(18) 0.079(4) Uani 0.35 1 d D U P G 2 H80C H 0.9819 0.8842 0.6636 0.095 Uiso 0.35 1 calc R U P G 2 H80D H 1.0246 0.9326 0.5961 0.095 Uiso 0.35 1 calc R U P G 2 O17 O 0.9695(18) 0.9175(12) 0.4611(14) 0.066(6) Uani 0.3 1 d . . P H 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 I1 0.0433(2) 0.0534(3) 0.0262(2) 0.00444(17) 0.00766(17) 0.0202(2) I2 0.0670(3) 0.0430(3) 0.0539(3) 0.0004(2) -0.0016(2) 0.0157(2) I3 0.0333(2) 0.0649(3) 0.0507(3) 0.0054(2) 0.0081(2) 0.0133(2) I4 0.0443(3) 0.0824(4) 0.0472(3) 0.0195(2) 0.0118(2) 0.0325(3) O1 0.039(2) 0.047(3) 0.029(2) 0.0099(19) 0.0078(18) 0.018(2) O2 0.040(2) 0.048(3) 0.026(2) 0.0057(18) 0.0125(18) 0.021(2) O3 0.036(2) 0.051(3) 0.025(2) 0.0053(18) 0.0118(17) 0.022(2) O4 0.041(2) 0.040(2) 0.044(3) 0.010(2) 0.018(2) 0.017(2) O5 0.038(2) 0.041(2) 0.044(3) 0.012(2) 0.020(2) 0.013(2) O6 0.035(2) 0.050(3) 0.037(2) 0.011(2) 0.0156(19) 0.020(2) O7 0.032(2) 0.051(3) 0.040(2) 0.012(2) 0.0134(19) 0.021(2) O8 0.044(2) 0.044(2) 0.033(2) 0.0112(19) 0.0113(19) 0.019(2) C1 0.030(3) 0.040(3) 0.030(3) 0.011(3) 0.013(2) 0.010(3) C2 0.035(3) 0.042(3) 0.029(3) 0.009(3) 0.010(2) 0.014(3) C3 0.034(3) 0.047(4) 0.026(3) 0.008(3) 0.009(2) 0.012(3) C4 0.036(3) 0.044(3) 0.027(3) 0.007(3) 0.015(2) 0.015(3) C5 0.027(3) 0.048(4) 0.029(3) 0.007(3) 0.012(2) 0.014(3) C6 0.027(3) 0.046(3) 0.027(3) 0.007(3) 0.011(2) 0.010(3) C7 0.032(3) 0.051(4) 0.025(3) 0.004(3) 0.009(2) 0.017(3) C8 0.028(3) 0.048(4) 0.036(3) 0.006(3) 0.009(3) 0.017(3) C9 0.036(4) 0.066(5) 0.048(4) 0.018(4) 0.014(3) 0.015(3) C10 0.035(4) 0.062(5) 0.065(5) 0.018(4) 0.018(4) 0.010(4) C11 0.035(4) 0.071(5) 0.050(4) -0.002(4) 0.006(3) 0.019(4) C12 0.046(5) 0.066(6) 0.080(7) 0.007(5) -0.001(5) 0.003(4) C13 0.051(5) 0.101(8) 0.054(5) -0.012(5) 0.005(4) 0.031(5) C14 0.037(3) 0.049(4) 0.023(3) 0.005(3) 0.008(3) 0.019(3) C15 0.042(3) 0.041(3) 0.041(4) 0.005(3) 0.013(3) 0.020(3) C16 0.040(3) 0.049(4) 0.027(3) 0.002(3) 0.011(3) 0.018(3) C17 0.030(3) 0.046(3) 0.028(3) 0.007(3) 0.011(2) 0.017(3) C18 0.038(3) 0.047(4) 0.029(3) 0.004(3) 0.010(3) 0.023(3) C19 0.038(3) 0.039(3) 0.037(3) 0.003(3) 0.009(3) 0.018(3) C20 0.033(3) 0.040(3) 0.034(3) 0.010(3) 0.010(3) 0.014(3) C21 0.033(3) 0.042(3) 0.030(3) 0.008(3) 0.010(2) 0.020(3) C22 0.028(3) 0.045(3) 0.028(3) 0.006(3) 0.007(2) 0.017(3) C23 0.031(3) 0.042(3) 0.030(3) 0.009(3) 0.013(2) 0.012(3) C24 0.035(3) 0.047(4) 0.028(3) 0.008(3) 0.010(3) 0.018(3) C25 0.043(4) 0.053(4) 0.046(4) 0.010(3) 0.001(3) 0.024(3) C26 0.044(4) 0.064(5) 0.042(4) 0.019(4) 0.005(3) 0.026(4) C27 0.042(4) 0.062(4) 0.035(3) 0.007(3) 0.007(3) 0.029(3) C28 0.047(4) 0.055(4) 0.047(4) 0.009(3) 0.006(3) 0.026(4) C29 0.064(6) 0.061(5) 0.076(6) 0.010(5) 0.012(5) 0.022(5) C30 0.045(4) 0.040(4) 0.041(4) 0.008(3) 0.015(3) 0.020(3) C31 0.058(4) 0.046(4) 0.048(4) 0.007(4) 0.012(4) 0.023(4) C32 0.040(4) 0.045(4) 0.042(4) 0.009(3) 0.018(3) 0.014(3) C33 0.039(3) 0.049(4) 0.022(3) 0.011(3) 0.016(2) 0.021(3) C34 0.037(3) 0.036(3) 0.029(3) 0.006(2) 0.012(2) 0.014(3) C35 0.032(3) 0.049(4) 0.032(3) 0.009(3) 0.014(3) 0.013(3) C36 0.033(3) 0.050(4) 0.030(3) 0.012(3) 0.015(3) 0.018(3) C37 0.035(3) 0.042(3) 0.025(3) 0.005(2) 0.013(2) 0.013(3) C38 0.034(3) 0.046(3) 0.024(3) 0.011(2) 0.013(2) 0.014(3) C39 0.034(3) 0.048(4) 0.029(3) 0.004(3) 0.009(3) 0.017(3) C40 0.045(4) 0.045(4) 0.030(3) 0.002(3) 0.010(3) 0.013(3) C41 0.058(5) 0.053(5) 0.054(5) -0.005(4) 0.014(4) 0.018(4) C42 0.062(5) 0.057(5) 0.056(5) -0.013(4) 0.014(4) 0.016(4) C43 0.091(7) 0.073(6) 0.055(5) 0.007(5) 0.016(5) 0.043(6) C44 0.114(12) 0.113(11) 0.046(8) 0.001(8) 0.031(7) 0.043(10) C45 0.121(15) 0.124(14) 0.068(10) 0.006(9) 0.043(9) 0.030(11) C44B 0.117(15) 0.116(13) 0.046(12) -0.003(12) 0.032(12) 0.049(13) C45B 0.119(17) 0.114(16) 0.051(13) 0.000(13) 0.043(13) 0.046(14) C46 0.038(4) 0.051(4) 0.035(3) 0.013(3) 0.018(3) 0.018(3) C47 0.041(4) 0.057(4) 0.042(4) 0.013(3) 0.018(3) 0.021(4) C48 0.032(3) 0.051(4) 0.040(3) 0.013(3) 0.011(3) 0.019(3) C49 0.041(3) 0.036(3) 0.030(3) 0.003(2) 0.010(3) 0.016(3) C50 0.038(3) 0.040(3) 0.040(3) 0.009(3) 0.015(3) 0.021(3) C51 0.039(3) 0.042(3) 0.035(3) 0.010(3) 0.010(3) 0.019(3) C52 0.038(3) 0.038(3) 0.032(3) 0.009(3) 0.009(3) 0.018(3) C53 0.035(3) 0.031(3) 0.031(3) 0.005(2) 0.009(3) 0.011(3) C54 0.033(3) 0.037(3) 0.026(3) 0.003(2) 0.007(2) 0.013(3) C55 0.034(3) 0.037(3) 0.028(3) 0.007(2) 0.010(2) 0.012(3) C56 0.031(3) 0.041(3) 0.032(3) 0.009(3) 0.010(3) 0.012(3) C57 0.047(4) 0.039(3) 0.039(3) 0.000(3) 0.010(3) 0.015(3) C58 0.037(3) 0.042(4) 0.043(4) 0.006(3) 0.007(3) 0.010(3) C59 0.042(4) 0.042(4) 0.038(3) 0.002(3) 0.004(3) 0.012(3) C60 0.046(4) 0.051(4) 0.038(4) 0.005(3) 0.009(3) 0.010(3) C61 0.062(5) 0.047(4) 0.035(4) 0.005(3) 0.009(3) 0.017(4) C62 0.047(4) 0.051(4) 0.044(4) 0.016(3) 0.018(3) 0.026(3) C63 0.038(4) 0.068(5) 0.044(4) 0.012(3) 0.011(3) 0.030(4) C64 0.034(3) 0.040(3) 0.033(3) 0.004(3) 0.005(3) 0.014(3) O9 0.077(4) 0.081(5) 0.045(3) 0.007(3) 0.009(3) 0.027(4) O10 0.048(3) 0.079(4) 0.050(3) 0.005(3) 0.018(3) 0.018(3) C65 0.092(8) 0.099(8) 0.056(5) 0.010(5) 0.029(5) 0.050(7) C66 0.067(6) 0.128(10) 0.084(7) 0.027(7) 0.046(6) 0.050(7) C67 0.059(5) 0.087(7) 0.059(5) -0.002(5) 0.026(4) 0.021(5) C68 0.068(6) 0.131(11) 0.053(5) 0.002(6) 0.028(5) 0.037(7) O11 0.107(5) 0.136(7) 0.108(6) 0.008(5) 0.024(5) 0.072(5) O12 0.102(5) 0.127(6) 0.148(7) 0.010(6) 0.039(5) 0.059(5) C69 0.098(6) 0.124(7) 0.102(7) 0.018(6) 0.029(6) 0.057(6) C70 0.099(6) 0.120(7) 0.125(7) 0.024(6) 0.034(6) 0.048(6) C71 0.110(7) 0.141(8) 0.145(8) 0.012(7) 0.012(7) 0.073(6) C72 0.115(7) 0.143(8) 0.124(8) 0.016(7) 0.012(6) 0.075(6) O13 0.068(6) 0.061(5) 0.098(6) 0.012(5) -0.019(5) 0.015(5) O14 0.064(5) 0.065(6) 0.111(6) 0.007(6) -0.003(5) 0.007(5) C73 0.065(6) 0.060(6) 0.102(7) 0.015(5) -0.012(5) 0.017(5) C74 0.061(6) 0.060(6) 0.107(6) 0.013(6) -0.004(6) 0.009(6) C75 0.067(5) 0.067(6) 0.113(6) 0.011(6) -0.004(5) 0.006(5) C76 0.067(5) 0.062(6) 0.105(6) 0.006(6) -0.007(5) 0.008(5) O13B 0.068(6) 0.060(5) 0.100(6) 0.017(5) -0.020(5) 0.008(5) O14B 0.063(5) 0.066(6) 0.112(6) 0.008(6) -0.003(5) 0.007(5) C73B 0.073(7) 0.069(6) 0.106(7) 0.018(6) -0.018(6) 0.007(6) C74B 0.069(6) 0.064(6) 0.106(6) 0.015(6) -0.010(6) 0.012(5) C75B 0.064(5) 0.061(6) 0.106(6) 0.003(6) -0.003(5) 0.009(5) C76B 0.066(5) 0.061(6) 0.105(6) 0.007(6) -0.006(5) 0.008(5) O15 0.086(6) 0.081(9) 0.088(6) 0.032(6) 0.032(5) 0.034(6) O16 0.080(8) 0.079(9) 0.079(7) 0.031(6) 0.045(6) 0.036(7) C77 0.085(7) 0.082(9) 0.086(6) 0.037(6) 0.033(6) 0.033(7) C78 0.084(7) 0.080(9) 0.080(6) 0.036(6) 0.039(6) 0.036(7) C79 0.081(7) 0.079(8) 0.086(6) 0.023(6) 0.031(6) 0.043(7) C80 0.082(7) 0.081(9) 0.085(7) 0.030(6) 0.035(6) 0.037(7) O15B 0.087(6) 0.083(9) 0.088(6) 0.033(6) 0.032(6) 0.033(6) O16B 0.091(7) 0.083(8) 0.083(6) 0.032(6) 0.033(6) 0.035(7) C77B 0.086(7) 0.083(9) 0.084(6) 0.038(6) 0.038(6) 0.031(7) C78B 0.077(8) 0.076(9) 0.067(7) 0.046(6) 0.050(6) 0.041(7) C79B 0.077(7) 0.072(9) 0.077(7) 0.030(6) 0.040(6) 0.044(7) C80B 0.083(7) 0.082(9) 0.083(7) 0.032(6) 0.034(6) 0.037(6) O17 0.086(15) 0.031(8) 0.079(14) 0.006(9) 0.043(12) 0.013(9) 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' I I -0.3257 6.8362 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 O1 C64 117.6(5) C4 O2 C16 117.1(5) C18 O3 C16 116.4(5) C20 O4 C32 115.7(5) C34 O5 C32 117.9(5) C36 O6 C48 116.8(5) C50 O7 C48 115.8(5) C52 O8 C64 115.5(5) C6 C1 C2 118.3(6) C6 C1 C55 121.9(6) C2 C1 C55 119.7(6) C1 C2 O1 121.6(6) C1 C2 C3 121.6(6) O1 C2 C3 116.7(6) C2 C3 C4 118.3(6) C2 C3 C14 121.0(6) C4 C3 C14 120.6(6) O2 C4 C5 121.4(6) O2 C4 C3 117.2(6) C5 C4 C3 121.2(6) C4 C5 C6 117.6(6) C4 C5 C7 120.3(6) C6 C5 C7 122.0(6) C1 C6 C5 123.0(6) C1 C6 H6 118.5 C5 C6 H6 118.5 C17 C7 C5 107.7(5) C17 C7 C8 114.0(5) C5 C7 C8 114.4(6) C17 C7 H7 106.7 C5 C7 H7 106.7 C8 C7 H7 106.7 C7 C8 C9 113.5(6) C7 C8 H8A 108.9 C9 C8 H8A 108.9 C7 C8 H8B 108.9 C9 C8 H8B 108.9 H8A C8 H8B 107.7 C10 C9 C8 113.4(6) C10 C9 H9A 108.9 C8 C9 H9A 108.9 C10 C9 H9B 108.9 C8 C9 H9B 108.9 H9A C9 H9B 107.7 C11 C10 C9 115.6(8) C11 C10 H10A 108.4 C9 C10 H10A 108.4 C11 C10 H10B 108.4 C9 C10 H10B 108.4 H10A C10 H10B 107.4 C12 C11 C10 114.7(8) C12 C11 H11A 108.6 C10 C11 H11A 108.6 C12 C11 H11B 108.6 C10 C11 H11B 108.6 H11A C11 H11B 107.6 C13 C12 C11 114.7(9) C13 C12 H12A 108.6 C11 C12 H12A 108.6 C13 C12 H12B 108.6 C11 C12 H12B 108.6 H12A C12 H12B 107.6 C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C15 C14 C3 178.0(7) C14 C15 I1 179.5(6) O3 C16 O2 112.7(5) O3 C16 H16A 109.0 O2 C16 H16A 109.0 O3 C16 H16B 109.0 O2 C16 H16B 109.0 H16A C16 H16B 107.8 C18 C17 C22 117.2(6) C18 C17 C7 120.5(6) C22 C17 C7 122.2(6) C17 C18 C19 123.2(6) C17 C18 O3 119.8(6) C19 C18 O3 117.0(6) C18 C19 C20 117.6(6) C18 C19 C30 121.7(6) C20 C19 C30 120.7(6) O4 C20 C21 121.0(6) O4 C20 C19 117.3(6) C21 C20 C19 121.7(6) C20 C21 C22 118.3(6) C20 C21 C23 118.8(6) C22 C21 C23 122.8(6) C21 C22 C17 122.1(6) C21 C22 H22 118.9 C17 C22 H22 118.9 C33 C23 C21 107.7(5) C33 C23 C24 113.7(6) C21 C23 C24 114.7(5) C33 C23 H23 106.7 C21 C23 H23 106.7 C24 C23 H23 106.7 C25 C24 C23 111.6(6) C25 C24 H24A 109.3 C23 C24 H24A 109.3 C25 C24 H24B 109.3 C23 C24 H24B 109.3 H24A C24 H24B 108.0 C24 C25 C26 113.5(7) C24 C25 H25A 108.9 C26 C25 H25A 108.9 C24 C25 H25B 108.9 C26 C25 H25B 108.9 H25A C25 H25B 107.7 C27 C26 C25 115.1(6) C27 C26 H26A 108.5 C25 C26 H26A 108.5 C27 C26 H26B 108.5 C25 C26 H26B 108.5 H26A C26 H26B 107.5 C26 C27 C28 112.2(6) C26 C27 H27A 109.2 C28 C27 H27A 109.2 C26 C27 H27B 109.2 C28 C27 H27B 109.2 H27A C27 H27B 107.9 C29 C28 C27 114.1(7) C29 C28 H28A 108.7 C27 C28 H28A 108.7 C29 C28 H28B 108.7 C27 C28 H28B 108.7 H28A C28 H28B 107.6 C28 C29 H29A 109.5 C28 C29 H29B 109.5 H29A C29 H29B 109.5 C28 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C31 C30 C19 177.6(8) C30 C31 I2 177.3(7) O5 C32 O4 112.6(6) O5 C32 H32A 109.1 O4 C32 H32A 109.1 O5 C32 H32B 109.1 O4 C32 H32B 109.1 H32A C32 H32B 107.8 C34 C33 C38 117.4(6) C34 C33 C23 120.4(6) C38 C33 C23 122.2(6) C33 C34 O5 120.5(6) C33 C34 C35 122.3(6) O5 C34 C35 117.1(6) C34 C35 C36 118.7(6) C34 C35 C46 120.5(7) C36 C35 C46 120.8(6) O6 C36 C35 118.4(6) O6 C36 C37 120.8(6) C35 C36 C37 120.7(6) C38 C37 C36 118.4(6) C38 C37 C39 122.6(6) C36 C37 C39 119.0(6) C37 C38 C33 122.5(6) C37 C38 H38 118.8 C33 C38 H38 118.8 C49 C39 C40 114.4(6) C49 C39 C37 107.0(5) C40 C39 C37 115.1(6) C49 C39 H39 106.6 C40 C39 H39 106.6 C37 C39 H39 106.6 C41 C40 C39 111.8(6) C41 C40 H40A 109.3 C39 C40 H40A 109.3 C41 C40 H40B 109.3 C39 C40 H40B 109.3 H40A C40 H40B 107.9 C42 C41 C40 116.8(8) C42 C41 H41A 108.1 C40 C41 H41A 108.1 C42 C41 H41B 108.1 C40 C41 H41B 108.1 H41A C41 H41B 107.3 C43 C42 C41 111.7(9) C43 C42 H42A 109.3 C41 C42 H42A 109.3 C43 C42 H42B 109.3 C41 C42 H42B 109.3 H42A C42 H42B 107.9 C42 C43 C44 116.7(11) C42 C43 C44B 98(2) C42 C43 H43A 108.1 C44 C43 H43A 108.1 C42 C43 H43B 108.1 C44 C43 H43B 108.1 H43A C43 H43B 107.3 C42 C43 H43C 112.1 C44B C43 H43C 112.1 C42 C43 H43D 112.1 C44B C43 H43D 112.1 H43C C43 H43D 109.8 C43 C44 C45 109.8(16) C43 C44 H44A 109.7 C45 C44 H44A 109.7 C43 C44 H44B 109.7 C45 C44 H44B 109.7 H44A C44 H44B 108.2 C44 C45 H45A 109.5 C44 C45 H45B 109.5 H45A C45 H45B 109.5 C44 C45 H45C 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C43 C44B C45B 97(4) C43 C44B H44C 112.3 C45B C44B H44C 112.3 C43 C44B H44D 112.3 C45B C44B H44D 112.3 H44C C44B H44D 109.9 C44B C45B H45D 109.5 C44B C45B H45E 109.5 H45D C45B H45E 109.5 C44B C45B H45F 109.5 H45D C45B H45F 109.5 H45E C45B H45F 109.5 C47 C46 C35 176.6(7) C46 C47 I3 178.0(7) O6 C48 O7 112.9(6) O6 C48 H48A 109.0 O7 C48 H48A 109.0 O6 C48 H48B 109.0 O7 C48 H48B 109.0 H48A C48 H48B 107.8 C54 C49 C50 117.9(6) C54 C49 C39 122.3(6) C50 C49 C39 119.7(6) O7 C50 C51 118.8(6) O7 C50 C49 120.3(6) C51 C50 C49 120.7(6) C50 C51 C52 119.5(6) C50 C51 C62 120.3(6) C52 C51 C62 120.2(6) O8 C52 C53 120.4(6) O8 C52 C51 117.7(6) C53 C52 C51 121.8(6) C52 C53 C54 116.9(6) C52 C53 C55 120.2(6) C54 C53 C55 122.9(6) C49 C54 C53 123.2(6) C49 C54 H54 118.4 C53 C54 H54 118.4 C53 C55 C1 108.2(5) C53 C55 C56 114.5(5) C1 C55 C56 113.2(5) C53 C55 H55 106.8 C1 C55 H55 106.8 C56 C55 H55 106.8 C57 C56 C55 114.0(5) C57 C56 H56A 108.7 C55 C56 H56A 108.7 C57 C56 H56B 108.7 C55 C56 H56B 108.7 H56A C56 H56B 107.6 C58 C57 C56 112.0(6) C58 C57 H57A 109.2 C56 C57 H57A 109.2 C58 C57 H57B 109.2 C56 C57 H57B 109.2 H57A C57 H57B 107.9 C59 C58 C57 114.0(6) C59 C58 H58A 108.8 C57 C58 H58A 108.8 C59 C58 H58B 108.8 C57 C58 H58B 108.8 H58A C58 H58B 107.6 C58 C59 C60 113.1(6) C58 C59 H59A 109.0 C60 C59 H59A 109.0 C58 C59 H59B 109.0 C60 C59 H59B 109.0 H59A C59 H59B 107.8 C61 C60 C59 112.4(7) C61 C60 H60A 109.1 C59 C60 H60A 109.1 C61 C60 H60B 109.1 C59 C60 H60B 109.1 H60A C60 H60B 107.9 C60 C61 H61A 109.5 C60 C61 H61B 109.5 H61A C61 H61B 109.5 C60 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C63 C62 C51 179.1(9) C62 C63 I4 177.4(7) O1 C64 O8 112.8(5) O1 C64 H64A 109.0 O8 C64 H64A 109.0 O1 C64 H64B 109.0 O8 C64 H64B 109.0 H64A C64 H64B 107.8 C65 O9 C68 110.3(9) C67 O10 C66 108.5(8) O9 C65 C66 110.7(9) O9 C65 H65A 109.5 C66 C65 H65A 109.5 O9 C65 H65B 109.5 C66 C65 H65B 109.5 H65A C65 H65B 108.1 C65 C66 O10 111.6(9) C65 C66 H66A 109.3 O10 C66 H66A 109.3 C65 C66 H66B 109.3 O10 C66 H66B 109.3 H66A C66 H66B 108.0 O10 C67 C68 111.3(8) O10 C67 H67A 109.4 C68 C67 H67A 109.4 O10 C67 H67B 109.4 C68 C67 H67B 109.4 H67A C67 H67B 108.0 O9 C68 C67 112.7(9) O9 C68 H68A 109.1 C67 C68 H68A 109.1 O9 C68 H68B 109.1 C67 C68 H68B 109.1 H68A C68 H68B 107.8 C69 O11 C72 109.1(12) C71 O12 C70 107.4(13) O11 C69 C70 115.9(15) O11 C69 H69A 108.3 C70 C69 H69A 108.3 O11 C69 H69B 108.3 C70 C69 H69B 108.3 H69A C69 H69B 107.4 O12 C70 C69 109.8(14) O12 C70 H70A 109.7 C69 C70 H70A 109.7 O12 C70 H70B 109.7 C69 C70 H70B 109.7 H70A C70 H70B 108.2 O12 C71 C72 110.6(16) O12 C71 H71A 109.5 C72 C71 H71A 109.5 O12 C71 H71B 109.5 C72 C71 H71B 109.5 H71A C71 H71B 108.1 O11 C72 C71 110.5(15) O11 C72 H72A 109.6 C71 C72 H72A 109.6 O11 C72 H72B 109.6 C71 C72 H72B 109.6 H72A C72 H72B 108.1 C76 O13 C73 107(2) C74 O14 C75 101(2) O13 C73 C74 112(2) O13 C73 H73A 109.3 C74 C73 H73A 109.3 O13 C73 H73B 109.3 C74 C73 H73B 109.3 H73A C73 H73B 107.9 O14 C74 C73 113(2) O14 C74 H74A 108.9 C73 C74 H74A 108.9 O14 C74 H74B 108.9 C73 C74 H74B 108.9 H74A C74 H74B 107.7 O14 C75 C76 109(3) O14 C75 H75A 109.8 C76 C75 H75A 109.8 O14 C75 H75B 109.8 C76 C75 H75B 109.8 H75A C75 H75B 108.3 O13 C76 C75 94(2) O13 C76 H76A 112.9 C75 C76 H76A 112.9 O13 C76 H76B 112.9 C75 C76 H76B 112.9 H76A C76 H76B 110.3 C76B O13B C73B 106(2) C74B O14B C75B 119(2) O13B C73B C74B 117(2) O13B C73B H73C 108.1 C74B C73B H73C 108.1 O13B C73B H73D 108.1 C74B C73B H73D 108.1 H73C C73B H73D 107.3 O14B C74B C73B 98(2) O14B C74B H74C 112.2 C73B C74B H74C 112.2 O14B C74B H74D 112.2 C73B C74B H74D 112.2 H74C C74B H74D 109.8 O14B C75B C76B 116(2) O14B C75B H75C 108.4 C76B C75B H75C 108.4 O14B C75B H75D 108.4 C76B C75B H75D 108.4 H75C C75B H75D 107.4 O13B C76B C75B 119(2) O13B C76B H76C 107.5 C75B C76B H76C 107.5 O13B C76B H76D 107.5 C75B C76B H76D 107.5 H76C C76B H76D 107.0 C80 O15 C77 99(3) C78 O16 C79 106(2) O15 C77 C78 104(3) O15 C77 H77A 110.9 C78 C77 H77A 110.9 O15 C77 H77B 110.9 C78 C77 H77B 110.9 H77A C77 H77B 108.9 O16 C78 C77 116(3) O16 C78 H78A 108.2 C77 C78 H78A 108.2 O16 C78 H78B 108.2 C77 C78 H78B 108.2 H78A C78 H78B 107.3 O16 C79 C80 105(2) O16 C79 H79A 110.9 C80 C79 H79A 110.9 O16 C79 H79B 110.9 C80 C79 H79B 110.9 H79A C79 H79B 108.9 O15 C80 C79 106(3) O15 C80 H80A 110.5 C79 C80 H80A 110.5 O15 C80 H80B 110.5 C79 C80 H80B 110.5 H80A C80 H80B 108.7 C80B O15B C77B 114(2) C78B O16B C79B 111.4(17) C78B C77B O15B 134(2) C78B C77B H77C 103.8 O15B C77B H77C 103.8 C78B C77B H77D 103.8 O15B C77B H77D 103.8 H77C C77B H77D 105.4 C77B C78B O16B 89(2) C77B C78B H78C 113.8 O16B C78B H78C 113.8 C77B C78B H78D 113.8 O16B C78B H78D 113.8 H78C C78B H78D 111.1 C80B C79B O16B 115(2) C80B C79B H79C 108.5 O16B C79B H79C 108.5 C80B C79B H79D 108.5 O16B C79B H79D 108.5 H79C C79B H79D 107.5 O15B C80B C79B 102(2) O15B C80B H80C 111.4 C79B C80B H80C 111.4 O15B C80B H80D 111.4 C79B C80B H80D 111.4 H80C C80B H80D 109.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C15 1.992(7) I2 C31 2.010(8) I3 C47 2.021(8) I4 C63 2.007(7) O1 C2 1.393(8) O1 C64 1.415(8) O2 C4 1.381(8) O2 C16 1.423(9) O3 C18 1.400(7) O3 C16 1.407(8) O4 C20 1.379(8) O4 C32 1.425(8) O5 C34 1.394(8) O5 C32 1.415(9) O6 C36 1.380(8) O6 C48 1.420(8) O7 C50 1.371(8) O7 C48 1.425(9) O8 C52 1.381(8) O8 C64 1.422(8) C1 C6 1.378(9) C1 C2 1.389(9) C1 C55 1.525(9) C2 C3 1.402(10) C3 C4 1.413(9) C3 C14 1.430(9) C4 C5 1.392(9) C5 C6 1.404(10) C5 C7 1.527(9) C6 H6 0.9500 C7 C17 1.511(9) C7 C8 1.535(9) C7 H7 1.0000 C8 C9 1.542(10) C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.529(12) C9 H9A 0.9900 C9 H9B 0.9900 C10 C11 1.512(12) C10 H10A 0.9900 C10 H10B 0.9900 C11 C12 1.510(12) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.510(15) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 C15 1.204(10) C16 H16A 0.9900 C16 H16B 0.9900 C17 C18 1.384(10) C17 C22 1.415(9) C18 C19 1.394(10) C19 C20 1.413(9) C19 C30 1.426(10) C20 C21 1.391(10) C21 C22 1.396(9) C21 C23 1.524(8) C22 H22 0.9500 C23 C33 1.520(9) C23 C24 1.538(9) C23 H23 1.0000 C24 C25 1.512(9) C24 H24A 0.9900 C24 H24B 0.9900 C25 C26 1.524(11) C25 H25A 0.9900 C25 H25B 0.9900 C26 C27 1.510(12) C26 H26A 0.9900 C26 H26B 0.9900 C27 C28 1.529(10) C27 H27A 0.9900 C27 H27B 0.9900 C28 C29 1.512(13) C28 H28A 0.9900 C28 H28B 0.9900 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 C31 1.169(11) C32 H32A 0.9900 C32 H32B 0.9900 C33 C34 1.386(10) C33 C38 1.398(10) C34 C35 1.394(9) C35 C36 1.398(10) C35 C46 1.443(10) C36 C37 1.403(10) C37 C38 1.389(9) C37 C39 1.530(10) C38 H38 0.9500 C39 C49 1.511(9) C39 C40 1.530(10) C39 H39 1.0000 C40 C41 1.522(11) C40 H40A 0.9900 C40 H40B 0.9900 C41 C42 1.516(12) C41 H41A 0.9900 C41 H41B 0.9900 C42 C43 1.496(14) C42 H42A 0.9900 C42 H42B 0.9900 C43 C44 1.555(18) C43 C44B 1.57(2) C43 H43A 0.9900 C43 H43B 0.9900 C43 H43C 0.9900 C43 H43D 0.9900 C44 C45 1.58(2) C44 H44A 0.9900 C44 H44B 0.9900 C45 H45A 0.9800 C45 H45B 0.9800 C45 H45C 0.9800 C44B C45B 1.58(3) C44B H44C 0.9900 C44B H44D 0.9900 C45B H45D 0.9800 C45B H45E 0.9800 C45B H45F 0.9800 C46 C47 1.175(11) C48 H48A 0.9900 C48 H48B 0.9900 C49 C54 1.387(9) C49 C50 1.408(10) C50 C51 1.390(9) C51 C52 1.403(9) C51 C62 1.439(10) C52 C53 1.391(9) C53 C54 1.413(9) C53 C55 1.511(9) C54 H54 0.9500 C55 C56 1.538(9) C55 H55 1.0000 C56 C57 1.525(9) C56 H56A 0.9900 C56 H56B 0.9900 C57 C58 1.519(10) C57 H57A 0.9900 C57 H57B 0.9900 C58 C59 1.515(10) C58 H58A 0.9900 C58 H58B 0.9900 C59 C60 1.535(10) C59 H59A 0.9900 C59 H59B 0.9900 C60 C61 1.513(11) C60 H60A 0.9900 C60 H60B 0.9900 C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C62 C63 1.179(11) C64 H64A 0.9900 C64 H64B 0.9900 O9 C65 1.393(14) O9 C68 1.442(14) O10 C67 1.433(11) O10 C66 1.473(14) C65 C66 1.414(17) C65 H65A 0.9900 C65 H65B 0.9900 C66 H66A 0.9900 C66 H66B 0.9900 C67 C68 1.443(15) C67 H67A 0.9900 C67 H67B 0.9900 C68 H68A 0.9900 C68 H68B 0.9900 O11 C69 1.371(18) O11 C72 1.389(18) O12 C71 1.37(2) O12 C70 1.392(19) C69 C70 1.47(2) C69 H69A 0.9900 C69 H69B 0.9900 C70 H70A 0.9900 C70 H70B 0.9900 C71 C72 1.55(3) C71 H71A 0.9900 C71 H71B 0.9900 C72 H72A 0.9900 C72 H72B 0.9900 O13 C76 1.394(19) O13 C73 1.416(17) O14 C74 1.385(18) O14 C75 1.413(18) C73 C74 1.516(17) C73 H73A 0.9900 C73 H73B 0.9900 C74 H74A 0.9900 C74 H74B 0.9900 C75 C76 1.461(19) C75 H75A 0.9900 C75 H75B 0.9900 C76 H76A 0.9900 C76 H76B 0.9900 O13B C76B 1.403(17) O13B C73B 1.414(17) O14B C74B 1.366(18) O14B C75B 1.411(18) C73B C74B 1.475(18) C73B H73C 0.9900 C73B H73D 0.9900 C74B H74C 0.9900 C74B H74D 0.9900 C75B C76B 1.492(18) C75B H75C 0.9900 C75B H75D 0.9900 C76B H76C 0.9900 C76B H76D 0.9900 O15 C80 1.395(19) O15 C77 1.420(19) O16 C78 1.425(19) O16 C79 1.440(19) C77 C78 1.452(19) C77 H77A 0.9900 C77 H77B 0.9900 C78 H78A 0.9900 C78 H78B 0.9900 C79 C80 1.466(19) C79 H79A 0.9900 C79 H79B 0.9900 C80 H80A 0.9900 C80 H80B 0.9900 O15B C80B 1.434(19) O15B C77B 1.464(18) O16B C78B 1.477(18) O16B C79B 1.509(18) C77B C78B 1.459(19) C77B H77C 0.9900 C77B H77D 0.9900 C78B H78C 0.9900 C78B H78D 0.9900 C79B C80B 1.454(19) C79B H79C 0.9900 C79B H79D 0.9900 C80B H80C 0.9900 C80B H80D 0.9900 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 C6 C1 C2 O1 -174.7(5) C55 C1 C2 O1 8.9(9) C6 C1 C2 C3 -0.1(9) C55 C1 C2 C3 -176.5(6) C64 O1 C2 C1 -82.6(7) C64 O1 C2 C3 102.5(7) C1 C2 C3 C4 -1.0(9) O1 C2 C3 C4 173.9(5) C1 C2 C3 C14 176.7(6) O1 C2 C3 C14 -8.4(9) C16 O2 C4 C5 81.8(7) C16 O2 C4 C3 -102.4(6) C2 C3 C4 O2 -175.2(5) C14 C3 C4 O2 7.1(9) C2 C3 C4 C5 0.6(9) C14 C3 C4 C5 -177.1(6) O2 C4 C5 C6 176.4(5) C3 C4 C5 C6 0.8(9) O2 C4 C5 C7 -7.6(9) C3 C4 C5 C7 176.7(6) C2 C1 C6 C5 1.6(9) C55 C1 C6 C5 177.9(6) C4 C5 C6 C1 -1.9(9) C7 C5 C6 C1 -177.8(6) C4 C5 C7 C17 -82.7(7) C6 C5 C7 C17 93.1(7) C4 C5 C7 C8 149.4(6) C6 C5 C7 C8 -34.8(8) C17 C7 C8 C9 170.1(6) C5 C7 C8 C9 -65.2(7) C7 C8 C9 C10 169.3(7) C8 C9 C10 C11 57.5(10) C9 C10 C11 C12 177.5(8) C10 C11 C12 C13 -177.9(8) C18 O3 C16 O2 92.9(6) C4 O2 C16 O3 -90.4(6) C5 C7 C17 C18 85.0(7) C8 C7 C17 C18 -146.8(6) C5 C7 C17 C22 -91.2(7) C8 C7 C17 C22 37.0(8) C22 C17 C18 C19 -0.3(9) C7 C17 C18 C19 -176.7(6) C22 C17 C18 O3 -179.0(5) C7 C17 C18 O3 4.6(9) C16 O3 C18 C17 -83.7(7) C16 O3 C18 C19 97.5(7) C17 C18 C19 C20 -0.5(10) O3 C18 C19 C20 178.3(5) C17 C18 C19 C30 177.0(6) O3 C18 C19 C30 -4.3(9) C32 O4 C20 C21 84.2(7) C32 O4 C20 C19 -97.9(7) C18 C19 C20 O4 -176.8(5) C30 C19 C20 O4 5.7(9) C18 C19 C20 C21 1.1(9) C30 C19 C20 C21 -176.4(6) O4 C20 C21 C22 177.0(5) C19 C20 C21 C22 -0.8(9) O4 C20 C21 C23 -6.3(9) C19 C20 C21 C23 175.9(6) C20 C21 C22 C17 -0.1(9) C23 C21 C22 C17 -176.6(6) C18 C17 C22 C21 0.6(9) C7 C17 C22 C21 176.9(6) C20 C21 C23 C33 -85.3(7) C22 C21 C23 C33 91.3(7) C20 C21 C23 C24 147.0(6) C22 C21 C23 C24 -36.4(8) C33 C23 C24 C25 167.8(6) C21 C23 C24 C25 -67.6(7) C23 C24 C25 C26 -167.8(6) C24 C25 C26 C27 -64.1(9) C25 C26 C27 C28 -169.6(6) C26 C27 C28 C29 177.1(7) C34 O5 C32 O4 90.6(7) C20 O4 C32 O5 -92.3(7) C21 C23 C33 C34 84.5(7) C24 C23 C33 C34 -147.2(6) C21 C23 C33 C38 -94.0(7) C24 C23 C33 C38 34.3(8) C38 C33 C34 O5 -175.7(5) C23 C33 C34 O5 5.7(8) C38 C33 C34 C35 1.1(9) C23 C33 C34 C35 -177.5(6) C32 O5 C34 C33 -81.2(7) C32 O5 C34 C35 101.8(7) C33 C34 C35 C36 -2.8(9) O5 C34 C35 C36 174.1(5) C33 C34 C35 C46 175.0(6) O5 C34 C35 C46 -8.1(9) C48 O6 C36 C35 -100.1(7) C48 O6 C36 C37 83.1(7) C34 C35 C36 O6 -174.4(5) C46 C35 C36 O6 7.8(9) C34 C35 C36 C37 2.4(9) C46 C35 C36 C37 -175.4(6) O6 C36 C37 C38 176.4(5) C35 C36 C37 C38 -0.4(9) O6 C36 C37 C39 -7.0(8) C35 C36 C37 C39 176.3(5) C36 C37 C38 C33 -1.4(9) C39 C37 C38 C33 -177.9(5) C34 C33 C38 C37 1.0(8) C23 C33 C38 C37 179.6(5) C38 C37 C39 C49 92.2(7) C36 C37 C39 C49 -84.4(7) C38 C37 C39 C40 -36.1(8) C36 C37 C39 C40 147.4(6) C49 C39 C40 C41 61.9(8) C37 C39 C40 C41 -173.7(6) C39 C40 C41 C42 171.0(7) C40 C41 C42 C43 -71.8(10) C41 C42 C43 C44 -174.7(14) C41 C42 C43 C44B 179(4) C42 C43 C44 C45 -177.7(15) C44B C43 C44 C45 -159(14) C42 C43 C44B C45B 180(4) C44 C43 C44B C45B 17(10) C36 O6 C48 O7 -91.9(7) C50 O7 C48 O6 92.3(7) C40 C39 C49 C54 38.5(9) C37 C39 C49 C54 -90.2(7) C40 C39 C49 C50 -144.6(6) C37 C39 C49 C50 86.7(7) C48 O7 C50 C51 101.6(7) C48 O7 C50 C49 -82.7(8) C54 C49 C50 O7 -178.1(6) C39 C49 C50 O7 4.9(9) C54 C49 C50 C51 -2.5(10) C39 C49 C50 C51 -179.5(6) O7 C50 C51 C52 177.6(6) C49 C50 C51 C52 1.9(10) O7 C50 C51 C62 -1.8(10) C49 C50 C51 C62 -177.5(6) C64 O8 C52 C53 84.0(7) C64 O8 C52 C51 -98.5(7) C50 C51 C52 O8 -177.9(6) C62 C51 C52 O8 1.5(10) C50 C51 C52 C53 -0.5(10) C62 C51 C52 C53 178.9(6) O8 C52 C53 C54 177.1(6) C51 C52 C53 C54 -0.2(9) O8 C52 C53 C55 -5.6(9) C51 C52 C53 C55 177.1(6) C50 C49 C54 C53 1.8(10) C39 C49 C54 C53 178.7(6) C52 C53 C54 C49 -0.4(9) C55 C53 C54 C49 -177.7(6) C52 C53 C55 C1 -85.6(7) C54 C53 C55 C1 91.6(7) C52 C53 C55 C56 147.1(6) C54 C53 C55 C56 -35.8(8) C6 C1 C55 C53 -94.7(7) C2 C1 C55 C53 81.6(7) C6 C1 C55 C56 33.4(8) C2 C1 C55 C56 -150.3(6) C53 C55 C56 C57 -54.3(7) C1 C55 C56 C57 -179.0(5) C55 C56 C57 C58 -167.9(6) C56 C57 C58 C59 -167.9(6) C57 C58 C59 C60 -176.7(6) C58 C59 C60 C61 -177.1(6) C2 O1 C64 O8 90.0(7) C52 O8 C64 O1 -92.3(7) C68 O9 C65 C66 57.8(13) O9 C65 C66 O10 -60.5(14) C67 O10 C66 C65 57.5(13) C66 O10 C67 C68 -53.5(13) C65 O9 C68 C67 -55.1(13) O10 C67 C68 O9 54.0(15) C72 O11 C69 C70 53(2) C71 O12 C70 C69 60(2) O11 C69 C70 O12 -58(2) C70 O12 C71 C72 -61.5(19) C69 O11 C72 C71 -51(2) O12 C71 C72 O11 59(2) C76 O13 C73 C74 58(3) C75 O14 C74 C73 49(4) O13 C73 C74 O14 -45(4) C74 O14 C75 C76 -74(3) C73 O13 C76 C75 -73(3) O14 C75 C76 O13 87(3) C76B O13B C73B C74B 61(4) C75B O14B C74B C73B 55(4) O13B C73B C74B O14B -75(3) C74B O14B C75B C76B -31(5) C73B O13B C76B C75B -26(4) O14B C75B C76B O13B 13(5) C80 O15 C77 C78 70(4) C79 O16 C78 C77 52(3) O15 C77 C78 O16 -60(4) C78 O16 C79 C80 -55(3) C77 O15 C80 C79 -82(3) O16 C79 C80 O15 76(3) C80B O15B C77B C78B 45(6) O15B C77B C78B O16B -53(5) C79B O16B C78B C77B 60(2) C78B O16B C79B C80B -81(3) C77B O15B C80B C79B -35(4) O16B C79B C80B O15B 56(3)