# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_C:\lndf0m.CIF _database_code_depnum_ccdc_archive 'CCDC 910406' #TrackingRef '15341_web_deposit_cif_file_0_DJKleinhans_1352536964.lndf0m.cif' _iucr_refine_instructions_details ; REM mo_LN_DISTAL_0m in P-1 REM R1 = 0.0443 for 9456 Fo > 4sig(Fo) and 0.0531 for all 11231 data REM 591 parameters refined using 0 restraints REM Highest difference peak 0.442, deepest hole -0.233, 1-sigma level 0.044 REM mo_LN_DISTAL_0m in P-1 REM R1 = 0.0443 for 9456 Fo > 4sig(Fo) and 0.0531 for all 11231 data REM 591 parameters refined using 0 restraints REM Highest difference peak 0.442, deepest hole -0.233, 1-sigma level 0.044 TITL mo_LN_DISTAL_0m in P-1 CELL 0.71073 10.9142 14.4914 16.5792 68.963 85.539 79.574 ZERR 2.0000 0.0008 0.0011 0.0012 0.001 0.001 0.001 LATT 1 SFAC C H O UNIT 104 136 24 MERG 2 FMAP 2 GRID PLAN 5 TEMP -173 SIZE 0.166 0.251 0.341 HTAB CONF BOND $H OMIT 0 9 6 OMIT 0 0 7 OMIT 6 -6 3 OMIT 9 6 6 OMIT -3 9 3 OMIT 1 1 1 OMIT -7 0 7 OMIT 7 7 7 OMIT 6 6 0 L.S. 4 ACTA 50 WGHT 0.051300 1.136600 FVAR 0.12139 O1 3 0.277682 0.709179 0.128330 11.00000 0.02253 0.01424 = 0.01842 -0.00095 0.00245 -0.00167 O2 3 0.455074 0.356060 0.204481 11.00000 0.02130 0.01672 = 0.02109 -0.00601 0.00374 0.00119 O3 3 -0.065739 0.246602 0.102997 11.00000 0.03057 0.02217 = 0.01988 -0.01116 0.00216 -0.00307 O4 3 -0.220435 0.605537 0.005863 11.00000 0.03463 0.02105 = 0.01486 -0.00268 -0.00222 -0.00399 O5 3 -0.353138 0.813821 0.095279 11.00000 0.01836 0.02068 = 0.02003 -0.00322 -0.00352 0.00072 O6 3 0.008953 0.879017 0.196291 11.00000 0.02400 0.01622 = 0.02078 -0.00645 -0.00073 -0.00489 O7 3 0.046131 0.042600 0.262615 11.00000 0.03326 0.01771 = 0.02701 -0.01076 -0.00074 -0.00694 O8 3 0.431081 0.125325 0.318351 11.00000 0.02241 0.01664 = 0.03036 -0.00394 -0.00275 0.00265 O9 3 -0.258532 0.978530 0.187360 11.00000 0.03764 0.01572 = 0.02048 -0.00541 0.00043 0.00270 O10 3 -0.242202 1.012203 0.044594 11.00000 0.04453 0.01917 = 0.02020 -0.00166 -0.00101 0.00457 O11 3 0.365613 0.009136 0.201754 11.00000 0.03757 0.02188 = 0.03060 -0.01021 0.00412 0.00775 C12 1 0.114679 0.672322 0.267182 11.00000 0.01650 0.01399 = 0.01684 -0.00490 -0.00053 -0.00123 AFIX 13 H12 2 0.160524 0.730375 0.251201 11.00000 -1.20000 AFIX 0 C13 1 -0.004110 0.708516 0.214088 11.00000 0.01771 0.01545 = 0.01441 -0.00486 0.00029 -0.00075 C14 1 0.371907 0.534272 0.161718 11.00000 0.01736 0.01885 = 0.01493 -0.00492 0.00066 -0.00328 AFIX 43 H14 2 0.427513 0.550611 0.113572 11.00000 -1.20000 AFIX 0 C15 1 0.285783 0.609432 0.178447 11.00000 0.01739 0.01394 = 0.01556 -0.00297 -0.00226 -0.00336 C16 1 0.237489 0.083948 0.288808 11.00000 0.02913 0.01418 = 0.01949 -0.00538 -0.00021 0.00113 C17 1 0.307618 0.300601 0.349284 11.00000 0.01716 0.01344 = 0.01645 -0.00320 -0.00067 -0.00037 AFIX 13 H17 2 0.398319 0.271932 0.351289 11.00000 -1.20000 AFIX 0 C18 1 0.112868 0.261037 0.303020 11.00000 0.02188 0.01308 = 0.01635 -0.00442 0.00026 -0.00040 AFIX 43 H18 2 0.070639 0.323404 0.305372 11.00000 -1.20000 AFIX 0 C19 1 -0.213080 0.507697 0.153331 11.00000 0.01711 0.01841 = 0.01810 -0.00668 -0.00098 -0.00426 C20 1 0.240555 0.236321 0.317858 11.00000 0.02243 0.01381 = 0.01404 -0.00246 0.00096 -0.00231 C21 1 -0.278678 0.599455 0.172806 11.00000 0.01864 0.01619 = 0.01716 -0.00490 -0.00232 -0.00155 AFIX 13 H21 2 -0.344978 0.634685 0.128677 11.00000 -1.20000 AFIX 0 C22 1 0.375259 0.434940 0.216570 11.00000 0.01592 0.01720 = 0.01755 -0.00731 -0.00213 -0.00083 C23 1 0.294915 0.409261 0.288373 11.00000 0.01682 0.01469 = 0.01589 -0.00398 -0.00213 -0.00293 C24 1 -0.141224 0.426381 0.048515 11.00000 0.02147 0.02512 = 0.01485 -0.00775 0.00088 -0.00701 AFIX 43 H24 2 -0.127335 0.430454 -0.009859 11.00000 -1.20000 AFIX 0 C25 1 0.202574 0.587373 0.248742 11.00000 0.01591 0.01506 = 0.01656 -0.00565 -0.00236 -0.00087 C26 1 -0.096679 0.226124 0.274194 11.00000 0.02215 0.01579 = 0.01881 -0.00637 -0.00044 -0.00389 AFIX 13 H26 2 -0.124588 0.174378 0.256276 11.00000 -1.20000 AFIX 0 C27 1 -0.236562 0.777356 0.133020 11.00000 0.01739 0.01856 = 0.01566 -0.00434 -0.00056 -0.00004 O28 3 0.290507 -0.094884 0.323634 11.00000 0.05289 0.01827 = 0.03864 -0.00784 0.00161 0.00073 C29 1 -0.181256 0.414648 0.218154 11.00000 0.01913 0.01961 = 0.01573 -0.00699 -0.00074 -0.00419 AFIX 43 H29 2 -0.194185 0.410730 0.276546 11.00000 -1.20000 AFIX 0 C30 1 0.209721 0.486992 0.301673 11.00000 0.01633 0.01641 = 0.01501 -0.00435 0.00013 -0.00204 AFIX 43 H30 2 0.153482 0.470593 0.349442 11.00000 -1.20000 AFIX 0 C31 1 -0.159342 0.219750 0.362236 11.00000 0.02332 0.02015 = 0.01714 -0.00410 -0.00060 -0.00498 AFIX 23 H31A 2 -0.123097 0.155439 0.406205 11.00000 -1.20000 H31B 2 -0.138487 0.274359 0.378574 11.00000 -1.20000 AFIX 0 C32 1 -0.343680 0.570631 0.262550 11.00000 0.01972 0.01943 = 0.02149 -0.00642 0.00146 -0.00327 AFIX 23 H32A 2 -0.393058 0.517693 0.267910 11.00000 -1.20000 H32B 2 -0.278785 0.541589 0.307356 11.00000 -1.20000 AFIX 0 C33 1 -0.113285 0.334589 0.115598 11.00000 0.01717 0.02152 = 0.02063 -0.01047 0.00072 -0.00465 C34 1 -0.193403 0.674316 0.166904 11.00000 0.01895 0.01741 = 0.01498 -0.00581 0.00051 -0.00257 C35 1 0.043836 0.198760 0.284867 11.00000 0.02300 0.01661 = 0.01526 -0.00414 -0.00008 -0.00270 C36 1 -0.076679 0.642392 0.206018 11.00000 0.01894 0.01434 = 0.01564 -0.00434 0.00025 -0.00060 AFIX 43 H36 2 -0.045438 0.572576 0.228066 11.00000 -1.20000 AFIX 0 C37 1 -0.053304 0.811104 0.183018 11.00000 0.02038 0.01569 = 0.01576 -0.00550 0.00056 -0.00225 C38 1 -0.168936 0.845312 0.142804 11.00000 0.02108 0.01462 = 0.01482 -0.00301 0.00106 0.00035 C39 1 0.266094 0.291794 0.442561 11.00000 0.02128 0.01739 = 0.01642 -0.00388 -0.00046 -0.00137 AFIX 23 H39A 2 0.311484 0.333702 0.461358 11.00000 -1.20000 H39B 2 0.176140 0.319081 0.442724 11.00000 -1.20000 AFIX 0 C40 1 0.303444 0.147315 0.308481 11.00000 0.02142 0.01641 = 0.01825 -0.00342 0.00011 0.00009 C41 1 -0.189787 0.512383 0.067641 11.00000 0.01878 0.02050 = 0.01653 -0.00389 -0.00192 -0.00600 C42 1 -0.131608 0.327035 0.202407 11.00000 0.01807 0.01852 = 0.01751 -0.00537 -0.00049 -0.00515 C43 1 0.075280 0.647517 0.363003 11.00000 0.01954 0.01886 = 0.01732 -0.00720 -0.00024 -0.00016 AFIX 23 H43A 2 0.013457 0.704233 0.368274 11.00000 -1.20000 H43B 2 0.033428 0.587910 0.381180 11.00000 -1.20000 AFIX 0 C44 1 0.082411 0.928933 0.123085 11.00000 0.02922 0.02180 = 0.02500 -0.00620 0.00196 -0.00928 AFIX 137 H44A 2 0.144373 0.879092 0.108516 11.00000 -1.50000 H44B 2 0.124938 0.975121 0.137225 11.00000 -1.50000 H44C 2 0.027992 0.966608 0.073618 11.00000 -1.50000 AFIX 0 C45 1 0.181120 0.627075 0.424828 11.00000 0.02641 0.02693 = 0.02119 -0.00987 -0.00538 -0.00166 AFIX 23 H45A 2 0.217591 0.688781 0.411486 11.00000 -1.20000 H45B 2 0.247166 0.574525 0.416484 11.00000 -1.20000 AFIX 0 C46 1 0.108169 0.108184 0.280501 11.00000 0.02810 0.01608 = 0.01887 -0.00615 -0.00135 -0.00448 C47 1 -0.225808 0.954278 0.117159 11.00000 0.01848 0.01600 = 0.02019 -0.00388 0.00020 -0.00135 C48 1 0.361762 0.736452 0.056919 11.00000 0.02638 0.02041 = 0.02239 0.00013 0.00576 -0.00223 AFIX 137 H48A 2 0.447611 0.715038 0.077626 11.00000 -1.50000 H48B 2 0.346290 0.809347 0.027557 11.00000 -1.50000 H48C 2 0.349270 0.703747 0.016410 11.00000 -1.50000 AFIX 0 C49 1 0.534009 0.375666 0.129810 11.00000 0.02355 0.02407 = 0.02416 -0.00947 0.00596 -0.00031 AFIX 137 H49A 2 0.482997 0.406020 0.077814 11.00000 -1.50000 H49B 2 0.584567 0.312702 0.129227 11.00000 -1.50000 H49C 2 0.588815 0.421778 0.130974 11.00000 -1.50000 AFIX 0 C50 1 -0.347623 0.841052 0.002409 11.00000 0.02862 0.02704 = 0.02011 -0.00287 -0.00624 -0.00263 AFIX 137 H50A 2 -0.290916 0.889789 -0.022208 11.00000 -1.50000 H50B 2 -0.431044 0.870750 -0.021234 11.00000 -1.50000 H50C 2 -0.317170 0.781085 -0.012317 11.00000 -1.50000 AFIX 0 C51 1 -0.429368 0.656292 0.281232 11.00000 0.02308 0.02523 = 0.02992 -0.01133 0.00214 -0.00174 AFIX 23 H51A 2 -0.499280 0.681938 0.240181 11.00000 -1.20000 H51B 2 -0.382525 0.711710 0.272368 11.00000 -1.20000 AFIX 0 C52 1 -0.195071 0.616298 -0.082878 11.00000 0.02930 0.03119 = 0.01494 -0.00293 -0.00231 -0.00719 AFIX 137 H52A 2 -0.105568 0.596657 -0.091108 11.00000 -1.50000 H52B 2 -0.221121 0.686323 -0.119625 11.00000 -1.50000 H52C 2 -0.241176 0.573275 -0.098595 11.00000 -1.50000 AFIX 0 C53 1 0.299942 -0.011094 0.275657 11.00000 0.02987 0.01861 = 0.02531 -0.00909 -0.00570 0.00192 C54 1 0.288223 0.185021 0.507864 11.00000 0.02600 0.02059 = 0.02179 -0.00177 0.00057 -0.00135 AFIX 23 H54A 2 0.230524 0.145916 0.496321 11.00000 -1.20000 H54B 2 0.374456 0.152862 0.500784 11.00000 -1.20000 AFIX 0 C55 1 -0.300828 0.226935 0.365516 11.00000 0.02576 0.03731 = 0.02263 -0.00831 0.00119 -0.01126 AFIX 23 H55A 2 -0.338137 0.290213 0.320797 11.00000 -1.20000 H55B 2 -0.322763 0.170627 0.352201 11.00000 -1.20000 AFIX 0 C56 1 -0.031660 0.250054 0.017039 11.00000 0.02980 0.03259 = 0.02260 -0.01672 0.00323 -0.00289 AFIX 137 H56A 2 -0.106043 0.273864 -0.018955 11.00000 -1.50000 H56B 2 0.005773 0.182799 0.018242 11.00000 -1.50000 H56C 2 0.028644 0.295864 -0.007077 11.00000 -1.50000 AFIX 0 C57 1 -0.003462 -0.026788 0.338851 11.00000 0.04512 0.02409 = 0.03397 -0.01216 0.00655 -0.01366 AFIX 137 H57A 2 0.065008 -0.068481 0.377071 11.00000 -1.50000 H57B 2 -0.048512 -0.069628 0.322066 11.00000 -1.50000 H57C 2 -0.060582 0.010593 0.369222 11.00000 -1.50000 AFIX 0 C58 1 0.479485 0.029601 0.378676 11.00000 0.03161 0.02504 = 0.03992 -0.00082 -0.00995 0.00436 AFIX 137 H58A 2 0.417187 0.007739 0.424282 11.00000 -1.50000 H58B 2 0.555146 0.034011 0.404345 11.00000 -1.50000 H58C 2 0.499462 -0.018878 0.348949 11.00000 -1.50000 AFIX 0 C59 1 -0.309847 1.083038 0.171055 11.00000 0.04269 0.01676 = 0.02866 -0.00903 0.00133 0.00345 AFIX 137 H59A 2 -0.248288 1.125009 0.139431 11.00000 -1.50000 H59B 2 -0.330642 1.093215 0.226164 11.00000 -1.50000 H59C 2 -0.385290 1.101513 0.136553 11.00000 -1.50000 AFIX 0 C60 1 0.268462 0.183027 0.600265 11.00000 0.04335 0.03220 = 0.01988 -0.00062 0.00165 0.00055 AFIX 137 H60A 2 0.329448 0.217605 0.613214 11.00000 -1.50000 H60B 2 0.279128 0.113355 0.640160 11.00000 -1.50000 H60C 2 0.184077 0.216835 0.606958 11.00000 -1.50000 AFIX 0 C61 1 -0.481137 0.622568 0.373492 11.00000 0.04278 0.03886 = 0.04489 -0.01785 0.02158 -0.00723 AFIX 137 H61A 2 -0.527540 0.567688 0.382435 11.00000 -1.50000 H61B 2 -0.536897 0.678932 0.383031 11.00000 -1.50000 H61C 2 -0.412236 0.599415 0.414286 11.00000 -1.50000 AFIX 0 C62 1 0.136202 0.593126 0.518664 11.00000 0.05022 0.04824 = 0.02100 -0.01141 -0.00510 -0.01170 AFIX 137 H62A 2 0.067813 0.643439 0.526396 11.00000 -1.50000 H62B 2 0.205066 0.585191 0.556430 11.00000 -1.50000 H62C 2 0.106837 0.528913 0.533516 11.00000 -1.50000 AFIX 0 C63 1 0.431660 -0.078366 0.183868 11.00000 0.04634 0.02844 = 0.04021 -0.01836 0.00139 0.01263 AFIX 137 H63A 2 0.494466 -0.115331 0.228228 11.00000 -1.50000 H63B 2 0.472617 -0.056753 0.126983 11.00000 -1.50000 H63C 2 0.372338 -0.121891 0.184358 11.00000 -1.50000 AFIX 0 C64 1 -0.355172 0.223913 0.453435 11.00000 0.02923 0.08245 = 0.02715 -0.01700 0.00661 -0.02000 AFIX 137 H64A 2 -0.315839 0.162726 0.498184 11.00000 -1.50000 H64B 2 -0.445154 0.224444 0.454058 11.00000 -1.50000 H64C 2 -0.339582 0.282620 0.464783 11.00000 -1.50000 HKLF 4 REM mo_LN_DISTAL_0m in P-1 REM R1 = 0.0443 for 9456 Fo > 4sig(Fo) and 0.0531 for all 11231 data REM 591 parameters refined using 0 restraints END WGHT 0.0513 1.1366 REM Highest difference peak 0.442, deepest hole -0.233, 1-sigma level 0.044 Q1 1 0.3764 -0.0839 0.3322 11.00000 0.05 0.44 Q2 1 0.2990 0.3568 0.3197 11.00000 0.05 0.37 Q3 1 -0.1925 0.8982 0.1333 11.00000 0.05 0.36 Q4 1 0.1648 0.6277 0.2615 11.00000 0.05 0.34 Q5 1 0.2736 0.1887 0.3214 11.00000 0.05 0.32 ; _audit_update_record ; 2012-11-08 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety 'C52 H68 O12' _chemical_formula_sum 'C52 H68 O12' _chemical_formula_weight 885.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9142(8) _cell_length_b 14.4914(11) _cell_length_c 16.5792(12) _cell_angle_alpha 68.9630(10) _cell_angle_beta 85.5390(10) _cell_angle_gamma 79.5740(10) _cell_volume 2406.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9607 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9714 _exptl_absorpt_correction_T_max 0.9859 _exptl_absorpt_process_details 'SADABS (Bruker,2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 27093 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11231 _reflns_number_gt 9456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001;Atwood&Barbour,2003)' _computing_publication_material 'publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.1366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11231 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.27768(9) 0.70918(7) 0.12833(6) 0.02007(19) Uani 1 1 d . . . O2 O 0.45507(9) 0.35606(7) 0.20448(6) 0.0207(2) Uani 1 1 d . . . O3 O -0.06574(9) 0.24660(7) 0.10300(6) 0.0235(2) Uani 1 1 d . . . O4 O -0.22044(10) 0.60554(7) 0.00586(6) 0.0245(2) Uani 1 1 d . . . O5 O -0.35314(9) 0.81382(7) 0.09528(6) 0.0211(2) Uani 1 1 d . . . O6 O 0.00895(9) 0.87902(7) 0.19629(6) 0.02011(19) Uani 1 1 d . . . O7 O 0.04613(10) 0.04260(7) 0.26261(6) 0.0248(2) Uani 1 1 d . . . O8 O 0.43108(9) 0.12532(7) 0.31835(7) 0.0250(2) Uani 1 1 d . . . O9 O -0.25853(10) 0.97853(7) 0.18736(6) 0.0259(2) Uani 1 1 d . . . O10 O -0.24220(11) 1.01220(7) 0.04459(6) 0.0307(2) Uani 1 1 d . . . O11 O 0.36561(10) 0.00914(8) 0.20175(7) 0.0317(2) Uani 1 1 d . . . C12 C 0.11468(11) 0.67232(9) 0.26718(8) 0.0161(2) Uani 1 1 d . . . H12 H 0.1605 0.7304 0.2512 0.019 Uiso 1 1 calc R . . C13 C -0.00411(12) 0.70852(9) 0.21409(8) 0.0163(2) Uani 1 1 d . . . C14 C 0.37191(12) 0.53427(9) 0.16172(8) 0.0173(2) Uani 1 1 d . . . H14 H 0.4275 0.5506 0.1136 0.021 Uiso 1 1 calc R . . C15 C 0.28578(12) 0.60943(9) 0.17845(8) 0.0160(2) Uani 1 1 d . . . C16 C 0.23749(13) 0.08395(10) 0.28881(9) 0.0217(3) Uani 1 1 d . . . C17 C 0.30762(12) 0.30060(9) 0.34928(8) 0.0165(2) Uani 1 1 d . . . H17 H 0.3983 0.2719 0.3513 0.020 Uiso 1 1 calc R . . C18 C 0.11287(12) 0.26104(9) 0.30302(8) 0.0177(2) Uani 1 1 d . . . H18 H 0.0706 0.3234 0.3054 0.021 Uiso 1 1 calc R . . C19 C -0.21308(12) 0.50770(10) 0.15333(8) 0.0176(2) Uani 1 1 d . . . C20 C 0.24055(12) 0.23632(9) 0.31786(8) 0.0176(2) Uani 1 1 d . . . C21 C -0.27868(12) 0.59946(9) 0.17281(8) 0.0177(2) Uani 1 1 d . . . H21 H -0.3450 0.6347 0.1287 0.021 Uiso 1 1 calc R . . C22 C 0.37526(12) 0.43494(9) 0.21657(8) 0.0167(2) Uani 1 1 d . . . C23 C 0.29492(12) 0.40926(9) 0.28837(8) 0.0160(2) Uani 1 1 d . . . C24 C -0.14122(12) 0.42638(10) 0.04852(8) 0.0199(3) Uani 1 1 d . . . H24 H -0.1273 0.4305 -0.0099 0.024 Uiso 1 1 calc R . . C25 C 0.20257(11) 0.58737(9) 0.24874(8) 0.0159(2) Uani 1 1 d . . . C26 C -0.09668(12) 0.22612(9) 0.27419(8) 0.0187(3) Uani 1 1 d . . . H26 H -0.1246 0.1744 0.2563 0.022 Uiso 1 1 calc R . . C27 C -0.23656(12) 0.77736(10) 0.13302(8) 0.0180(2) Uani 1 1 d . . . O28 O 0.29051(12) -0.09488(8) 0.32363(8) 0.0382(3) Uani 1 1 d . . . C29 C -0.18126(12) 0.41465(10) 0.21815(8) 0.0178(2) Uani 1 1 d . . . H29 H -0.1942 0.4107 0.2765 0.021 Uiso 1 1 calc R . . C30 C 0.20972(12) 0.48699(9) 0.30167(8) 0.0164(2) Uani 1 1 d . . . H30 H 0.1535 0.4706 0.3494 0.020 Uiso 1 1 calc R . . C31 C -0.15934(12) 0.21975(10) 0.36224(8) 0.0207(3) Uani 1 1 d . . . H31A H -0.1231 0.1554 0.4062 0.025 Uiso 1 1 calc R . . H31B H -0.1385 0.2744 0.3786 0.025 Uiso 1 1 calc R . . C32 C -0.34368(12) 0.57063(10) 0.26255(9) 0.0205(3) Uani 1 1 d . . . H32A H -0.3931 0.5177 0.2679 0.025 Uiso 1 1 calc R . . H32B H -0.2788 0.5416 0.3074 0.025 Uiso 1 1 calc R . . C33 C -0.11328(12) 0.33459(10) 0.11560(8) 0.0188(3) Uani 1 1 d . . . C34 C -0.19340(12) 0.67432(9) 0.16690(8) 0.0172(2) Uani 1 1 d . . . C35 C 0.04384(12) 0.19876(10) 0.28487(8) 0.0188(3) Uani 1 1 d . . . C36 C -0.07668(12) 0.64239(9) 0.20602(8) 0.0169(2) Uani 1 1 d . . . H36 H -0.0454 0.5726 0.2281 0.020 Uiso 1 1 calc R . . C37 C -0.05330(12) 0.81110(9) 0.18302(8) 0.0174(2) Uani 1 1 d . . . C38 C -0.16894(12) 0.84531(9) 0.14280(8) 0.0180(2) Uani 1 1 d . . . C39 C 0.26609(12) 0.29179(9) 0.44256(8) 0.0192(3) Uani 1 1 d . . . H39A H 0.3115 0.3337 0.4614 0.023 Uiso 1 1 calc R . . H39B H 0.1761 0.3191 0.4427 0.023 Uiso 1 1 calc R . . C40 C 0.30344(12) 0.14732(10) 0.30848(8) 0.0199(3) Uani 1 1 d . . . C41 C -0.18979(12) 0.51238(10) 0.06764(8) 0.0189(3) Uani 1 1 d . . . C42 C -0.13161(12) 0.32704(10) 0.20241(8) 0.0180(2) Uani 1 1 d . . . C43 C 0.07528(12) 0.64752(10) 0.36300(8) 0.0187(3) Uani 1 1 d . . . H43A H 0.0135 0.7042 0.3683 0.022 Uiso 1 1 calc R . . H43B H 0.0334 0.5879 0.3812 0.022 Uiso 1 1 calc R . . C44 C 0.08241(14) 0.92893(11) 0.12309(9) 0.0254(3) Uani 1 1 d . . . H44A H 0.1444 0.8791 0.1085 0.038 Uiso 1 1 calc R . . H44B H 0.1249 0.9751 0.1372 0.038 Uiso 1 1 calc R . . H44C H 0.0280 0.9666 0.0736 0.038 Uiso 1 1 calc R . . C45 C 0.18112(13) 0.62707(11) 0.42483(9) 0.0245(3) Uani 1 1 d . . . H45A H 0.2176 0.6888 0.4115 0.029 Uiso 1 1 calc R . . H45B H 0.2472 0.5745 0.4165 0.029 Uiso 1 1 calc R . . C46 C 0.10817(13) 0.10818(10) 0.28050(8) 0.0208(3) Uani 1 1 d . . . C47 C -0.22581(12) 0.95428(10) 0.11716(8) 0.0191(3) Uani 1 1 d . . . C48 C 0.36176(14) 0.73645(11) 0.05692(9) 0.0258(3) Uani 1 1 d . . . H48A H 0.4476 0.7150 0.0776 0.039 Uiso 1 1 calc R . . H48B H 0.3463 0.8093 0.0276 0.039 Uiso 1 1 calc R . . H48C H 0.3493 0.7037 0.0164 0.039 Uiso 1 1 calc R . . C49 C 0.53401(13) 0.37567(11) 0.12981(9) 0.0245(3) Uani 1 1 d . . . H49A H 0.4830 0.4060 0.0778 0.037 Uiso 1 1 calc R . . H49B H 0.5846 0.3127 0.1292 0.037 Uiso 1 1 calc R . . H49C H 0.5888 0.4218 0.1310 0.037 Uiso 1 1 calc R . . C50 C -0.34762(14) 0.84105(11) 0.00241(9) 0.0267(3) Uani 1 1 d . . . H50A H -0.2909 0.8898 -0.0222 0.040 Uiso 1 1 calc R . . H50B H -0.4310 0.8708 -0.0212 0.040 Uiso 1 1 calc R . . H50C H -0.3172 0.7811 -0.0123 0.040 Uiso 1 1 calc R . . C51 C -0.42937(13) 0.65629(11) 0.28123(10) 0.0261(3) Uani 1 1 d . . . H51A H -0.4993 0.6819 0.2402 0.031 Uiso 1 1 calc R . . H51B H -0.3825 0.7117 0.2724 0.031 Uiso 1 1 calc R . . C52 C -0.19507(14) 0.61630(11) -0.08288(8) 0.0262(3) Uani 1 1 d . . . H52A H -0.1056 0.5967 -0.0911 0.039 Uiso 1 1 calc R . . H52B H -0.2211 0.6863 -0.1196 0.039 Uiso 1 1 calc R . . H52C H -0.2412 0.5733 -0.0986 0.039 Uiso 1 1 calc R . . C53 C 0.29994(14) -0.01109(10) 0.27566(9) 0.0247(3) Uani 1 1 d . . . C54 C 0.28822(14) 0.18502(10) 0.50786(9) 0.0248(3) Uani 1 1 d . . . H54A H 0.2305 0.1459 0.4963 0.030 Uiso 1 1 calc R . . H54B H 0.3745 0.1529 0.5008 0.030 Uiso 1 1 calc R . . C55 C -0.30083(14) 0.22693(12) 0.36552(9) 0.0285(3) Uani 1 1 d . . . H55A H -0.3381 0.2902 0.3208 0.034 Uiso 1 1 calc R . . H55B H -0.3228 0.1706 0.3522 0.034 Uiso 1 1 calc R . . C56 C -0.03166(14) 0.25005(12) 0.01704(9) 0.0269(3) Uani 1 1 d . . . H56A H -0.1060 0.2739 -0.0190 0.040 Uiso 1 1 calc R . . H56B H 0.0058 0.1828 0.0182 0.040 Uiso 1 1 calc R . . H56C H 0.0286 0.2959 -0.0071 0.040 Uiso 1 1 calc R . . C57 C -0.00346(16) -0.02679(11) 0.33885(10) 0.0332(3) Uani 1 1 d . . . H57A H 0.0650 -0.0685 0.3771 0.050 Uiso 1 1 calc R . . H57B H -0.0485 -0.0696 0.3221 0.050 Uiso 1 1 calc R . . H57C H -0.0606 0.0106 0.3692 0.050 Uiso 1 1 calc R . . C58 C 0.47949(16) 0.02960(12) 0.37868(11) 0.0358(4) Uani 1 1 d . . . H58A H 0.4172 0.0077 0.4243 0.054 Uiso 1 1 calc R . . H58B H 0.5551 0.0340 0.4043 0.054 Uiso 1 1 calc R . . H58C H 0.4995 -0.0189 0.3489 0.054 Uiso 1 1 calc R . . C59 C -0.30985(16) 1.08304(10) 0.17106(10) 0.0303(3) Uani 1 1 d . . . H59A H -0.2483 1.1250 0.1394 0.045 Uiso 1 1 calc R . . H59B H -0.3306 1.0932 0.2262 0.045 Uiso 1 1 calc R . . H59C H -0.3853 1.1015 0.1366 0.045 Uiso 1 1 calc R . . C60 C 0.26846(17) 0.18303(12) 0.60026(10) 0.0352(4) Uani 1 1 d . . . H60A H 0.3294 0.2176 0.6132 0.053 Uiso 1 1 calc R . . H60B H 0.2791 0.1134 0.6402 0.053 Uiso 1 1 calc R . . H60C H 0.1841 0.2168 0.6070 0.053 Uiso 1 1 calc R . . C61 C -0.48114(18) 0.62257(14) 0.37349(12) 0.0425(4) Uani 1 1 d . . . H61A H -0.5275 0.5677 0.3824 0.064 Uiso 1 1 calc R . . H61B H -0.5369 0.6789 0.3830 0.064 Uiso 1 1 calc R . . H61C H -0.4122 0.5994 0.4143 0.064 Uiso 1 1 calc R . . C62 C 0.13620(18) 0.59313(14) 0.51866(10) 0.0393(4) Uani 1 1 d . . . H62A H 0.0678 0.6434 0.5264 0.059 Uiso 1 1 calc R . . H62B H 0.2051 0.5852 0.5564 0.059 Uiso 1 1 calc R . . H62C H 0.1068 0.5289 0.5335 0.059 Uiso 1 1 calc R . . C63 C 0.43166(17) -0.07837(12) 0.18387(12) 0.0392(4) Uani 1 1 d . . . H63A H 0.4945 -0.1153 0.2282 0.059 Uiso 1 1 calc R . . H63B H 0.4726 -0.0568 0.1270 0.059 Uiso 1 1 calc R . . H63C H 0.3723 -0.1219 0.1844 0.059 Uiso 1 1 calc R . . C64 C -0.35517(16) 0.22391(17) 0.45343(11) 0.0459(5) Uani 1 1 d . . . H64A H -0.3158 0.1627 0.4982 0.069 Uiso 1 1 calc R . . H64B H -0.4452 0.2244 0.4541 0.069 Uiso 1 1 calc R . . H64C H -0.3396 0.2826 0.4648 0.069 Uiso 1 1 calc R . . 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 0.0225(5) 0.0142(4) 0.0184(4) -0.0009(4) 0.0025(4) -0.0017(3) O2 0.0213(5) 0.0167(4) 0.0211(5) -0.0060(4) 0.0037(4) 0.0012(4) O3 0.0306(5) 0.0222(5) 0.0199(5) -0.0112(4) 0.0022(4) -0.0031(4) O4 0.0346(6) 0.0211(5) 0.0149(4) -0.0027(4) -0.0022(4) -0.0040(4) O5 0.0184(5) 0.0207(5) 0.0200(5) -0.0032(4) -0.0035(4) 0.0007(4) O6 0.0240(5) 0.0162(4) 0.0208(4) -0.0065(4) -0.0007(4) -0.0049(4) O7 0.0333(6) 0.0177(5) 0.0270(5) -0.0108(4) -0.0007(4) -0.0069(4) O8 0.0224(5) 0.0166(5) 0.0304(5) -0.0039(4) -0.0027(4) 0.0026(4) O9 0.0376(6) 0.0157(5) 0.0205(5) -0.0054(4) 0.0004(4) 0.0027(4) O10 0.0445(6) 0.0192(5) 0.0202(5) -0.0017(4) -0.0010(4) 0.0046(4) O11 0.0376(6) 0.0219(5) 0.0306(6) -0.0102(4) 0.0041(5) 0.0077(4) C12 0.0165(6) 0.0140(6) 0.0168(6) -0.0049(5) -0.0005(4) -0.0012(5) C13 0.0177(6) 0.0155(6) 0.0144(5) -0.0049(5) 0.0003(4) -0.0007(5) C14 0.0174(6) 0.0188(6) 0.0149(6) -0.0049(5) 0.0007(4) -0.0033(5) C15 0.0174(6) 0.0139(6) 0.0156(6) -0.0030(5) -0.0023(4) -0.0034(4) C16 0.0291(7) 0.0142(6) 0.0195(6) -0.0054(5) -0.0002(5) 0.0011(5) C17 0.0172(6) 0.0134(6) 0.0164(6) -0.0032(5) -0.0007(4) -0.0004(4) C18 0.0219(6) 0.0131(6) 0.0163(6) -0.0044(5) 0.0003(5) -0.0004(5) C19 0.0171(6) 0.0184(6) 0.0181(6) -0.0067(5) -0.0010(5) -0.0043(5) C20 0.0224(6) 0.0138(6) 0.0140(6) -0.0025(5) 0.0010(5) -0.0023(5) C21 0.0186(6) 0.0162(6) 0.0172(6) -0.0049(5) -0.0023(5) -0.0015(5) C22 0.0159(6) 0.0172(6) 0.0175(6) -0.0073(5) -0.0021(5) -0.0008(5) C23 0.0168(6) 0.0147(6) 0.0159(6) -0.0040(5) -0.0021(4) -0.0029(5) C24 0.0215(6) 0.0251(7) 0.0149(6) -0.0078(5) 0.0009(5) -0.0070(5) C25 0.0159(6) 0.0151(6) 0.0166(6) -0.0057(5) -0.0024(4) -0.0009(4) C26 0.0222(6) 0.0158(6) 0.0188(6) -0.0064(5) -0.0004(5) -0.0039(5) C27 0.0174(6) 0.0186(6) 0.0157(6) -0.0043(5) -0.0006(5) 0.0000(5) O28 0.0529(7) 0.0183(5) 0.0386(6) -0.0078(5) 0.0016(5) 0.0007(5) C29 0.0191(6) 0.0196(6) 0.0157(6) -0.0070(5) -0.0007(5) -0.0042(5) C30 0.0163(6) 0.0164(6) 0.0150(6) -0.0044(5) 0.0001(4) -0.0020(5) C31 0.0233(7) 0.0201(6) 0.0171(6) -0.0041(5) -0.0006(5) -0.0050(5) C32 0.0197(6) 0.0194(6) 0.0215(6) -0.0064(5) 0.0015(5) -0.0033(5) C33 0.0172(6) 0.0215(6) 0.0206(6) -0.0105(5) 0.0007(5) -0.0046(5) C34 0.0190(6) 0.0174(6) 0.0150(6) -0.0058(5) 0.0005(5) -0.0026(5) C35 0.0230(6) 0.0166(6) 0.0153(6) -0.0041(5) -0.0001(5) -0.0027(5) C36 0.0189(6) 0.0143(6) 0.0156(6) -0.0043(5) 0.0003(5) -0.0006(5) C37 0.0204(6) 0.0157(6) 0.0158(6) -0.0055(5) 0.0006(5) -0.0023(5) C38 0.0211(6) 0.0146(6) 0.0148(6) -0.0030(5) 0.0011(5) 0.0003(5) C39 0.0213(6) 0.0174(6) 0.0164(6) -0.0039(5) -0.0005(5) -0.0014(5) C40 0.0214(6) 0.0164(6) 0.0183(6) -0.0034(5) 0.0001(5) 0.0001(5) C41 0.0188(6) 0.0205(6) 0.0165(6) -0.0039(5) -0.0019(5) -0.0060(5) C42 0.0181(6) 0.0185(6) 0.0175(6) -0.0054(5) -0.0005(5) -0.0052(5) C43 0.0195(6) 0.0189(6) 0.0173(6) -0.0072(5) -0.0002(5) -0.0002(5) C44 0.0292(7) 0.0218(7) 0.0250(7) -0.0062(6) 0.0020(6) -0.0093(6) C45 0.0264(7) 0.0269(7) 0.0212(7) -0.0099(6) -0.0054(5) -0.0017(6) C46 0.0281(7) 0.0161(6) 0.0189(6) -0.0062(5) -0.0014(5) -0.0045(5) C47 0.0185(6) 0.0160(6) 0.0202(6) -0.0039(5) 0.0002(5) -0.0013(5) C48 0.0264(7) 0.0204(7) 0.0224(7) 0.0001(5) 0.0058(5) -0.0022(5) C49 0.0235(7) 0.0241(7) 0.0242(7) -0.0095(6) 0.0060(5) -0.0003(5) C50 0.0286(7) 0.0270(7) 0.0201(7) -0.0029(6) -0.0062(5) -0.0026(6) C51 0.0231(7) 0.0252(7) 0.0299(7) -0.0113(6) 0.0021(6) -0.0017(5) C52 0.0293(7) 0.0312(8) 0.0149(6) -0.0029(6) -0.0023(5) -0.0072(6) C53 0.0299(7) 0.0186(7) 0.0253(7) -0.0091(6) -0.0057(6) 0.0019(5) C54 0.0260(7) 0.0206(7) 0.0218(7) -0.0018(5) 0.0006(5) -0.0013(5) C55 0.0258(7) 0.0373(8) 0.0226(7) -0.0083(6) 0.0012(5) -0.0113(6) C56 0.0298(8) 0.0326(8) 0.0226(7) -0.0167(6) 0.0032(6) -0.0029(6) C57 0.0451(9) 0.0241(7) 0.0340(8) -0.0122(6) 0.0066(7) -0.0137(7) C58 0.0316(8) 0.0250(8) 0.0399(9) -0.0008(7) -0.0099(7) 0.0044(6) C59 0.0427(9) 0.0168(7) 0.0287(7) -0.0090(6) 0.0013(6) 0.0034(6) C60 0.0433(9) 0.0322(8) 0.0199(7) -0.0006(6) 0.0017(6) 0.0005(7) C61 0.0428(10) 0.0389(9) 0.0449(10) -0.0178(8) 0.0216(8) -0.0072(8) C62 0.0502(10) 0.0482(10) 0.0210(7) -0.0114(7) -0.0051(7) -0.0117(8) C63 0.0463(10) 0.0284(8) 0.0402(9) -0.0184(7) 0.0014(7) 0.0126(7) C64 0.0292(9) 0.0824(14) 0.0271(8) -0.0170(9) 0.0066(6) -0.0200(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C15 1.3750(15) . ? O1 C48 1.4235(16) . ? O2 C22 1.3721(15) . ? O2 C49 1.4233(16) . ? O3 C33 1.3688(16) . ? O3 C56 1.4300(16) . ? O4 C41 1.3713(16) . ? O4 C52 1.4329(16) . ? O5 C27 1.3902(15) . ? O5 C50 1.4450(16) . ? O6 C37 1.3782(15) . ? O6 C44 1.4378(16) . ? O7 C46 1.3842(16) . ? O7 C57 1.4421(18) . ? O8 C40 1.3807(16) . ? O8 C58 1.4229(17) . ? O9 C47 1.3376(16) . ? O9 C59 1.4502(16) . ? O10 C47 1.1992(16) . ? O11 C53 1.3351(18) . ? O11 C63 1.4565(17) . ? C12 C25 1.5252(17) . ? C12 C13 1.5267(17) . ? C12 C43 1.5419(17) . ? C12 H12 1.0000 . ? C13 C36 1.3952(18) . ? C13 C37 1.4029(17) . ? C14 C22 1.3952(18) . ? C14 C15 1.3973(18) . ? C14 H14 0.9500 . ? C15 C25 1.3993(17) . ? C16 C46 1.397(2) . ? C16 C40 1.3995(19) . ? C16 C53 1.5039(18) . ? C17 C23 1.5230(16) . ? C17 C20 1.5263(17) . ? C17 C39 1.5438(17) . ? C17 H17 1.0000 . ? C18 C20 1.3930(18) . ? C18 C35 1.3961(18) . ? C18 H18 0.9500 . ? C19 C29 1.3936(18) . ? C19 C41 1.4030(17) . ? C19 C21 1.5208(17) . ? C20 C40 1.4021(18) . ? C21 C34 1.5257(18) . ? C21 C32 1.5454(18) . ? C21 H21 1.0000 . ? C22 C23 1.4008(17) . ? C23 C30 1.3962(17) . ? C24 C33 1.3940(19) . ? C24 C41 1.3976(19) . ? C24 H24 0.9500 . ? C25 C30 1.3947(17) . ? C26 C35 1.5206(18) . ? C26 C42 1.5230(17) . ? C26 C31 1.5420(18) . ? C26 H26 1.0000 . ? C27 C38 1.3919(18) . ? C27 C34 1.3970(17) . ? O28 C53 1.2070(18) . ? C29 C42 1.3931(18) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C55 1.5268(19) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C51 1.5239(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C42 1.4048(17) . ? C34 C36 1.3990(17) . ? C35 C46 1.3957(18) . ? C36 H36 0.9500 . ? C37 C38 1.3965(18) . ? C38 C47 1.5046(17) . ? C39 C54 1.5256(18) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C43 C45 1.5216(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C62 1.524(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C61 1.525(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C54 C60 1.521(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C64 1.519(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 C15 O1 C48 118.18(10) . . ? C22 O2 C49 118.46(10) . . ? C33 O3 C56 118.39(11) . . ? C41 O4 C52 118.22(11) . . ? C27 O5 C50 112.82(10) . . ? C37 O6 C44 113.79(10) . . ? C46 O7 C57 113.17(11) . . ? C40 O8 C58 116.63(11) . . ? C47 O9 C59 115.65(10) . . ? C53 O11 C63 115.05(12) . . ? C25 C12 C13 113.91(10) . . ? C25 C12 C43 113.99(10) . . ? C13 C12 C43 107.40(10) . . ? C25 C12 H12 107.0 . . ? C13 C12 H12 107.0 . . ? C43 C12 H12 107.0 . . ? C36 C13 C37 117.61(11) . . ? C36 C13 C12 122.26(11) . . ? C37 C13 C12 119.40(11) . . ? C22 C14 C15 119.21(12) . . ? C22 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? O1 C15 C14 122.83(11) . . ? O1 C15 C25 115.62(11) . . ? C14 C15 C25 121.55(11) . . ? C46 C16 C40 119.92(12) . . ? C46 C16 C53 117.30(12) . . ? C40 C16 C53 122.77(12) . . ? C23 C17 C20 113.26(10) . . ? C23 C17 C39 112.15(10) . . ? C20 C17 C39 110.49(10) . . ? C23 C17 H17 106.8 . . ? C20 C17 H17 106.8 . . ? C39 C17 H17 106.8 . . ? C20 C18 C35 123.30(12) . . ? C20 C18 H18 118.4 . . ? C35 C18 H18 118.4 . . ? C29 C19 C41 117.12(12) . . ? C29 C19 C21 122.25(11) . . ? C41 C19 C21 120.50(11) . . ? C18 C20 C40 117.87(12) . . ? C18 C20 C17 120.77(11) . . ? C40 C20 C17 121.23(11) . . ? C19 C21 C34 113.79(11) . . ? C19 C21 C32 111.92(10) . . ? C34 C21 C32 108.84(10) . . ? C19 C21 H21 107.3 . . ? C34 C21 H21 107.3 . . ? C32 C21 H21 107.3 . . ? O2 C22 C14 123.33(11) . . ? O2 C22 C23 115.31(11) . . ? C14 C22 C23 121.35(11) . . ? C30 C23 C22 117.18(11) . . ? C30 C23 C17 123.50(11) . . ? C22 C23 C17 119.28(11) . . ? C33 C24 C41 119.61(12) . . ? C33 C24 H24 120.2 . . ? C41 C24 H24 120.2 . . ? C30 C25 C15 117.04(11) . . ? C30 C25 C12 123.14(11) . . ? C15 C25 C12 119.73(11) . . ? C35 C26 C42 110.92(11) . . ? C35 C26 C31 109.42(10) . . ? C42 C26 C31 114.14(11) . . ? C35 C26 H26 107.4 . . ? C42 C26 H26 107.4 . . ? C31 C26 H26 107.4 . . ? O5 C27 C38 118.35(11) . . ? O5 C27 C34 120.57(11) . . ? C38 C27 C34 120.86(12) . . ? C42 C29 C19 123.89(12) . . ? C42 C29 H29 118.1 . . ? C19 C29 H29 118.1 . . ? C25 C30 C23 123.66(12) . . ? C25 C30 H30 118.2 . . ? C23 C30 H30 118.2 . . ? C55 C31 C26 115.49(11) . . ? C55 C31 H31A 108.4 . . ? C26 C31 H31A 108.4 . . ? C55 C31 H31B 108.4 . . ? C26 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C51 C32 C21 115.35(11) . . ? C51 C32 H32A 108.4 . . ? C21 C32 H32A 108.4 . . ? C51 C32 H32B 108.4 . . ? C21 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? O3 C33 C24 123.65(12) . . ? O3 C33 C42 115.18(11) . . ? C24 C33 C42 121.16(12) . . ? C27 C34 C36 117.75(12) . . ? C27 C34 C21 120.67(11) . . ? C36 C34 C21 120.98(11) . . ? C46 C35 C18 117.33(12) . . ? C46 C35 C26 121.15(12) . . ? C18 C35 C26 121.46(11) . . ? C13 C36 C34 122.93(11) . . ? C13 C36 H36 118.5 . . ? C34 C36 H36 118.5 . . ? O6 C37 C38 119.01(11) . . ? O6 C37 C13 120.15(11) . . ? C38 C37 C13 120.74(12) . . ? C27 C38 C37 119.98(11) . . ? C27 C38 C47 119.70(11) . . ? C37 C38 C47 120.10(12) . . ? C54 C39 C17 114.21(11) . . ? C54 C39 H39A 108.7 . . ? C17 C39 H39A 108.7 . . ? C54 C39 H39B 108.7 . . ? C17 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? O8 C40 C16 121.68(11) . . ? O8 C40 C20 118.07(12) . . ? C16 C40 C20 120.25(12) . . ? O4 C41 C24 123.56(11) . . ? O4 C41 C19 115.33(11) . . ? C24 C41 C19 121.10(12) . . ? C29 C42 C33 117.08(12) . . ? C29 C42 C26 123.10(11) . . ? C33 C42 C26 119.82(11) . . ? C45 C43 C12 115.05(11) . . ? C45 C43 H43A 108.5 . . ? C12 C43 H43A 108.5 . . ? C45 C43 H43B 108.5 . . ? C12 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? O6 C44 H44A 109.5 . . ? O6 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O6 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 C62 111.55(13) . . ? C43 C45 H45A 109.3 . . ? C62 C45 H45A 109.3 . . ? C43 C45 H45B 109.3 . . ? C62 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? O7 C46 C35 120.68(12) . . ? O7 C46 C16 118.14(12) . . ? C35 C46 C16 121.07(12) . . ? O10 C47 O9 123.73(12) . . ? O10 C47 C38 125.84(12) . . ? O9 C47 C38 110.41(11) . . ? O1 C48 H48A 109.5 . . ? O1 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O1 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O2 C49 H49A 109.5 . . ? O2 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O2 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O5 C50 H50A 109.5 . . ? O5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C32 C51 C61 111.55(12) . . ? C32 C51 H51A 109.3 . . ? C61 C51 H51A 109.3 . . ? C32 C51 H51B 109.3 . . ? C61 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O28 C53 O11 123.76(13) . . ? O28 C53 C16 125.35(14) . . ? O11 C53 C16 110.87(12) . . ? C60 C54 C39 111.72(12) . . ? C60 C54 H54A 109.3 . . ? C39 C54 H54A 109.3 . . ? C60 C54 H54B 109.3 . . ? C39 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C64 C55 C31 111.97(12) . . ? C64 C55 H55A 109.2 . . ? C31 C55 H55A 109.2 . . ? C64 C55 H55B 109.2 . . ? C31 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? O3 C56 H56A 109.5 . . ? O3 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O3 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O7 C57 H57A 109.5 . . ? O7 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O7 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O8 C58 H58A 109.5 . . ? O8 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O8 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O9 C59 H59A 109.5 . . ? O9 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O9 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C54 C60 H60A 109.5 . . ? C54 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C54 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C45 C62 H62A 109.5 . . ? C45 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C45 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O11 C63 H63A 109.5 . . ? O11 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O11 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C55 C64 H64A 109.5 . . ? C55 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C55 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? 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 C25 C12 C13 C36 47.83(16) . . . . ? C43 C12 C13 C36 -79.40(14) . . . . ? C25 C12 C13 C37 -142.14(12) . . . . ? C43 C12 C13 C37 90.63(13) . . . . ? C48 O1 C15 C14 -0.57(18) . . . . ? C48 O1 C15 C25 178.71(11) . . . . ? C22 C14 C15 O1 179.03(11) . . . . ? C22 C14 C15 C25 -0.21(19) . . . . ? C35 C18 C20 C40 4.23(19) . . . . ? C35 C18 C20 C17 -171.67(11) . . . . ? C23 C17 C20 C18 -58.64(15) . . . . ? C39 C17 C20 C18 68.14(14) . . . . ? C23 C17 C20 C40 125.60(13) . . . . ? C39 C17 C20 C40 -107.63(13) . . . . ? C29 C19 C21 C34 104.25(14) . . . . ? C41 C19 C21 C34 -80.16(15) . . . . ? C29 C19 C21 C32 -19.66(17) . . . . ? C41 C19 C21 C32 155.93(12) . . . . ? C49 O2 C22 C14 -3.40(18) . . . . ? C49 O2 C22 C23 176.10(11) . . . . ? C15 C14 C22 O2 178.89(11) . . . . ? C15 C14 C22 C23 -0.59(18) . . . . ? O2 C22 C23 C30 -178.25(11) . . . . ? C14 C22 C23 C30 1.27(18) . . . . ? O2 C22 C23 C17 4.16(16) . . . . ? C14 C22 C23 C17 -176.33(11) . . . . ? C20 C17 C23 C30 99.55(14) . . . . ? C39 C17 C23 C30 -26.35(17) . . . . ? C20 C17 C23 C22 -83.02(14) . . . . ? C39 C17 C23 C22 151.08(11) . . . . ? O1 C15 C25 C30 -179.03(11) . . . . ? C14 C15 C25 C30 0.27(18) . . . . ? O1 C15 C25 C12 -2.39(16) . . . . ? C14 C15 C25 C12 176.90(11) . . . . ? C13 C12 C25 C30 -100.07(14) . . . . ? C43 C12 C25 C30 23.66(17) . . . . ? C13 C12 C25 C15 83.51(14) . . . . ? C43 C12 C25 C15 -152.76(11) . . . . ? C50 O5 C27 C38 89.72(14) . . . . ? C50 O5 C27 C34 -95.71(14) . . . . ? C41 C19 C29 C42 -1.84(19) . . . . ? C21 C19 C29 C42 173.89(12) . . . . ? C15 C25 C30 C23 0.48(18) . . . . ? C12 C25 C30 C23 -176.03(11) . . . . ? C22 C23 C30 C25 -1.24(19) . . . . ? C17 C23 C30 C25 176.25(11) . . . . ? C35 C26 C31 C55 -169.58(11) . . . . ? C42 C26 C31 C55 65.47(15) . . . . ? C19 C21 C32 C51 -170.26(11) . . . . ? C34 C21 C32 C51 63.11(14) . . . . ? C56 O3 C33 C24 6.15(19) . . . . ? C56 O3 C33 C42 -173.21(12) . . . . ? C41 C24 C33 O3 179.87(12) . . . . ? C41 C24 C33 C42 -0.80(19) . . . . ? O5 C27 C34 C36 -178.37(11) . . . . ? C38 C27 C34 C36 -3.93(18) . . . . ? O5 C27 C34 C21 -7.19(18) . . . . ? C38 C27 C34 C21 167.25(11) . . . . ? C19 C21 C34 C27 142.24(12) . . . . ? C32 C21 C34 C27 -92.20(14) . . . . ? C19 C21 C34 C36 -46.87(16) . . . . ? C32 C21 C34 C36 78.69(14) . . . . ? C20 C18 C35 C46 -0.91(19) . . . . ? C20 C18 C35 C26 176.44(11) . . . . ? C42 C26 C35 C46 -124.90(13) . . . . ? C31 C26 C35 C46 108.31(14) . . . . ? C42 C26 C35 C18 57.86(16) . . . . ? C31 C26 C35 C18 -68.94(15) . . . . ? C37 C13 C36 C34 1.54(18) . . . . ? C12 C13 C36 C34 171.74(11) . . . . ? C27 C34 C36 C13 1.49(19) . . . . ? C21 C34 C36 C13 -169.66(11) . . . . ? C44 O6 C37 C38 -84.86(14) . . . . ? C44 O6 C37 C13 98.79(14) . . . . ? C36 C13 C37 O6 174.07(11) . . . . ? C12 C13 C37 O6 3.58(18) . . . . ? C36 C13 C37 C38 -2.21(18) . . . . ? C12 C13 C37 C38 -172.70(11) . . . . ? O5 C27 C38 C37 177.88(11) . . . . ? C34 C27 C38 C37 3.32(19) . . . . ? O5 C27 C38 C47 3.32(18) . . . . ? C34 C27 C38 C47 -171.24(12) . . . . ? O6 C37 C38 C27 -176.47(11) . . . . ? C13 C37 C38 C27 -0.15(19) . . . . ? O6 C37 C38 C47 -1.93(18) . . . . ? C13 C37 C38 C47 174.39(11) . . . . ? C23 C17 C39 C54 -174.63(11) . . . . ? C20 C17 C39 C54 57.97(14) . . . . ? C58 O8 C40 C16 -53.91(18) . . . . ? C58 O8 C40 C20 126.74(14) . . . . ? C46 C16 C40 O8 179.13(12) . . . . ? C53 C16 C40 O8 -1.0(2) . . . . ? C46 C16 C40 C20 -1.5(2) . . . . ? C53 C16 C40 C20 178.36(12) . . . . ? C18 C20 C40 O8 176.43(11) . . . . ? C17 C20 C40 O8 -7.69(18) . . . . ? C18 C20 C40 C16 -2.93(19) . . . . ? C17 C20 C40 C16 172.95(12) . . . . ? C52 O4 C41 C24 -3.49(19) . . . . ? C52 O4 C41 C19 177.89(11) . . . . ? C33 C24 C41 O4 -179.69(12) . . . . ? C33 C24 C41 C19 -1.15(19) . . . . ? C29 C19 C41 O4 -178.94(11) . . . . ? C21 C19 C41 O4 5.25(17) . . . . ? C29 C19 C41 C24 2.40(19) . . . . ? C21 C19 C41 C24 -173.41(12) . . . . ? C19 C29 C42 C33 0.00(19) . . . . ? C19 C29 C42 C26 179.62(12) . . . . ? O3 C33 C42 C29 -179.26(11) . . . . ? C24 C33 C42 C29 1.36(19) . . . . ? O3 C33 C42 C26 1.11(17) . . . . ? C24 C33 C42 C26 -178.27(12) . . . . ? C35 C26 C42 C29 -104.57(14) . . . . ? C31 C26 C42 C29 19.58(18) . . . . ? C35 C26 C42 C33 75.04(15) . . . . ? C31 C26 C42 C33 -160.81(12) . . . . ? C25 C12 C43 C45 62.78(15) . . . . ? C13 C12 C43 C45 -170.04(11) . . . . ? C12 C43 C45 C62 -174.31(12) . . . . ? C57 O7 C46 C35 -88.12(15) . . . . ? C57 O7 C46 C16 95.68(15) . . . . ? C18 C35 C46 O7 -179.87(11) . . . . ? C26 C35 C46 O7 2.78(19) . . . . ? C18 C35 C46 C16 -3.77(19) . . . . ? C26 C35 C46 C16 178.87(12) . . . . ? C40 C16 C46 O7 -178.80(11) . . . . ? C53 C16 C46 O7 1.31(18) . . . . ? C40 C16 C46 C35 5.0(2) . . . . ? C53 C16 C46 C35 -174.88(12) . . . . ? C59 O9 C47 O10 -3.6(2) . . . . ? C59 O9 C47 C38 177.49(12) . . . . ? C27 C38 C47 O10 -72.55(19) . . . . ? C37 C38 C47 O10 112.89(16) . . . . ? C27 C38 C47 O9 106.36(14) . . . . ? C37 C38 C47 O9 -68.19(15) . . . . ? C21 C32 C51 C61 -175.55(13) . . . . ? C63 O11 C53 O28 -2.7(2) . . . . ? C63 O11 C53 C16 178.94(13) . . . . ? C46 C16 C53 O28 -69.17(19) . . . . ? C40 C16 C53 O28 110.94(18) . . . . ? C46 C16 C53 O11 109.11(14) . . . . ? C40 C16 C53 O11 -70.79(17) . . . . ? C17 C39 C54 C60 169.37(12) . . . . ? C26 C31 C55 C64 -177.86(14) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.442 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.044