# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_kr677f _database_code_depnum_ccdc_archive 'CCDC 901365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H54 N2 O6' _chemical_formula_sum 'C72 H54 N2 O6' _chemical_formula_weight 1043.17 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' N N 0.0061 0.0033 '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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3452(15) _cell_length_b 17.876(2) _cell_length_c 12.6550(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.209(5) _cell_angle_gamma 90.00 _cell_volume 2707.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8044 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 26.81 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9756 _exptl_absorpt_correction_T_max 0.9932 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotating_anode _diffrn_radiation_monochromator MONTEL_multi_layer_optics _diffrn_measurement_device_type Bruker-Kappa_Apex2_CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44420 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.82 _reflns_number_total 5769 _reflns_number_gt 4560 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT _computing_data_reduction Bruker-SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL KR677f in P2(1)/c CELL 0.71073 12.3452 17.8764 12.655 90 104.209 90 ZERR 2 0.0015 0.0022 0.0015 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 144 108 4 12 EADP C33 C33B ISOR .003 C34B C35B C36B C37B EXYZ C38 C38B EADP C38 C38B L.S. 22 CONF HTAB 2.5 PLAN 20 SIZE 0.084 0.286 0.307 TEMP -172.95 BOND LIST 4 fmap 2 ACTA WGHT 0.048900 1.742400 FVAR 0.15317 0.84044 0.76980 PART 0 O1 4 0.366364 0.364878 0.391990 11.00000 0.03988 0.05758 = 0.02553 0.00919 0.00862 -0.01385 O3 4 0.738411 0.412374 0.464069 11.00000 0.03464 0.06746 = 0.02393 0.01502 0.00085 0.00108 N42 3 0.551296 0.391885 0.433825 11.00000 0.03626 0.02361 = 0.01745 0.00339 0.00582 -0.00052 C1 1 0.907118 0.390127 -0.018284 11.00000 0.04939 0.05269 = 0.04143 0.00073 0.01867 -0.00369 AFIX 43 H1 2 0.915203 0.441042 -0.036451 11.00000 -1.20000 AFIX 0 C2 1 0.873244 0.337601 -0.100711 11.00000 0.06254 0.06708 = 0.04498 -0.00780 0.01974 -0.00520 AFIX 43 H2 2 0.859636 0.352617 -0.174820 11.00000 -1.20000 AFIX 0 C3 1 0.859249 0.263521 -0.075316 11.00000 0.05588 0.06246 = 0.06301 -0.01892 0.01675 -0.00610 AFIX 43 H3 2 0.834691 0.227803 -0.131696 11.00000 -1.20000 AFIX 0 C4 1 0.881175 0.241987 0.032230 11.00000 0.04687 0.04353 = 0.07847 -0.00409 0.01032 -0.00400 AFIX 43 H4 2 0.871943 0.191110 0.049869 11.00000 -1.20000 AFIX 0 C5 1 0.916619 0.293752 0.115198 11.00000 0.03682 0.04949 = 0.05625 0.00699 0.00987 -0.00157 AFIX 43 H5 2 0.932324 0.277986 0.189092 11.00000 -1.20000 AFIX 0 C6 1 0.929308 0.368750 0.090722 11.00000 0.02643 0.04537 = 0.04354 0.00245 0.01235 0.00005 C21 1 0.715618 0.484343 0.148076 11.00000 0.02457 0.02776 = 0.02223 0.00193 0.00506 -0.00108 C22 1 0.611481 0.493290 0.073017 11.00000 0.02537 0.02132 = 0.01832 0.00125 0.00482 0.00019 C23 1 0.513811 0.473367 0.108504 11.00000 0.02681 0.01954 = 0.01714 0.00028 0.00470 0.00013 C24 1 0.403507 0.478741 0.038604 11.00000 0.02532 0.02679 = 0.01910 0.00152 0.00428 -0.00119 C25 1 0.314158 0.456498 0.080119 11.00000 0.02616 0.05635 = 0.02448 0.00911 0.00324 -0.00465 AFIX 43 H25 2 0.240576 0.460185 0.034820 11.00000 -1.20000 AFIX 0 C26 1 0.328600 0.429060 0.185507 11.00000 0.03003 0.05623 = 0.02601 0.00954 0.00950 -0.00592 AFIX 43 H26 2 0.265276 0.413740 0.210105 11.00000 -1.20000 AFIX 0 C28 1 0.432296 0.423884 0.253819 11.00000 0.03042 0.02906 = 0.01911 0.00272 0.00576 -0.00238 C29 1 0.525407 0.446524 0.216873 11.00000 0.02836 0.01828 = 0.01814 0.00060 0.00518 -0.00028 C30 1 0.631392 0.441127 0.288264 11.00000 0.03064 0.02183 = 0.01802 0.00092 0.00449 0.00084 C31 1 0.724610 0.458985 0.254239 11.00000 0.02453 0.03166 = 0.02117 0.00277 0.00048 0.00108 AFIX 43 H31 2 0.796219 0.454156 0.303057 11.00000 -1.20000 AFIX 0 C32 1 0.646496 0.414634 0.401727 11.00000 0.03258 0.02812 = 0.02025 0.00303 0.00388 0.00239 C43 1 0.445450 0.391540 0.364017 11.00000 0.03530 0.02803 = 0.02253 0.00162 0.00889 -0.00490 PART 1 C33 1 0.574449 0.358860 0.545637 21.00000 0.02403 AFIX 13 H33 2 0.651773 0.374763 0.583966 21.00000 -1.20000 AFIX 0 C34 1 0.497279 0.387838 0.613488 21.00000 0.05487 0.02957 = 0.02186 0.00018 0.01289 0.00540 AFIX 23 H34A 2 0.419723 0.371071 0.581504 21.00000 -1.20000 H34B 2 0.498222 0.443210 0.614737 21.00000 -1.20000 AFIX 0 C35 1 0.538611 0.356973 0.730151 21.00000 0.05908 0.04431 = 0.01808 0.00018 0.01329 -0.00203 AFIX 23 H35A 2 0.613305 0.377962 0.763894 21.00000 -1.20000 H35B 2 0.486845 0.372900 0.774476 21.00000 -1.20000 AFIX 0 C36 1 0.545575 0.271979 0.730085 21.00000 0.05308 0.04423 = 0.02430 0.01491 0.00930 -0.00342 AFIX 23 H36A 2 0.577711 0.254259 0.805380 21.00000 -1.20000 H36B 2 0.469288 0.251033 0.705501 21.00000 -1.20000 AFIX 0 C37 1 0.616301 0.243512 0.656724 21.00000 0.05118 0.03167 = 0.03131 0.01309 0.00921 0.00436 AFIX 23 H37A 2 0.613629 0.188166 0.654985 21.00000 -1.20000 H37B 2 0.694910 0.258741 0.686985 21.00000 -1.20000 AFIX 0 C38 1 0.576100 0.273814 0.539799 21.00000 0.03320 AFIX 23 H38A 2 0.627230 0.257296 0.495142 21.00000 -1.20000 H38B 2 0.500297 0.254684 0.505805 21.00000 -1.20000 AFIX 0 PART 2 C33B 1 0.536274 0.354042 0.538721 -21.00000 0.02403 AFIX 13 H33B 2 0.455737 0.355142 0.540440 -21.00000 -1.20000 AFIX 0 C34B 1 0.603211 0.394015 0.632588 -21.00000 0.04452 0.03719 = 0.03676 -0.00135 0.01178 -0.00216 AFIX 23 H34C 2 0.573411 0.445294 0.634321 -21.00000 -1.20000 H34D 2 0.681166 0.398018 0.625698 -21.00000 -1.20000 AFIX 0 C35B 1 0.601778 0.353699 0.738712 -21.00000 0.05245 0.05273 = 0.04898 0.00239 0.01378 -0.00146 AFIX 23 H35C 2 0.525993 0.356867 0.751607 -21.00000 -1.20000 H35D 2 0.654509 0.378566 0.800322 -21.00000 -1.20000 AFIX 0 C36B 1 0.634946 0.270995 0.733777 -21.00000 0.05143 0.04882 = 0.04463 0.00548 0.01280 0.00145 AFIX 23 H36C 2 0.714736 0.268162 0.732624 -21.00000 -1.20000 H36D 2 0.626267 0.245310 0.800518 -21.00000 -1.20000 AFIX 0 C37B 1 0.567186 0.231341 0.637070 -21.00000 0.05983 0.05726 = 0.05897 0.00502 0.01252 -0.00168 AFIX 23 H37C 2 0.595540 0.179801 0.633844 -21.00000 -1.20000 H37D 2 0.488202 0.228515 0.641067 -21.00000 -1.20000 AFIX 0 C38B 1 0.576100 0.273814 0.539799 -21.00000 0.03320 AFIX 23 H38C 2 0.531725 0.248014 0.474121 -21.00000 -1.20000 H38D 2 0.655106 0.273780 0.535528 -21.00000 -1.20000 AFIX 0 PART 0 SADI .005 O2 C18 O2 C18B O2 4 0.811362 0.501417 0.116506 11.00000 0.02152 0.04888 = 0.02289 0.00887 0.00276 -0.00011 PART 1 SAME C7B > C18B EADP C7 C7B EADP C8 C8B EADP C9 C9B EADP C10 C10B EADP C11 C11B EADP C12 C12B EADP C13 C13B EADP C14 C14B EADP C15 C15B EADP C16 C16B EADP C17 C17B EADP C18 C18B C7 1 0.971274 0.422815 0.176033 31.00000 0.02571 0.04448 = 0.02499 0.00747 0.00980 -0.00167 C8 1 1.070577 0.406820 0.253182 31.00000 0.02591 0.04015 = 0.03076 0.00364 0.00833 0.00122 AFIX 43 H8 2 1.108069 0.360857 0.249406 31.00000 -1.20000 AFIX 0 C9 1 1.114786 0.457589 0.335238 31.00000 0.02369 0.04904 = 0.02803 0.00580 0.00523 0.00427 AFIX 43 H9 2 1.184347 0.447625 0.385212 31.00000 -1.20000 AFIX 0 C10 1 1.057536 0.522591 0.344139 31.00000 0.03068 0.04239 = 0.02675 0.00022 0.00320 -0.00330 AFIX 43 H10 2 1.088752 0.556924 0.400723 31.00000 -1.20000 AFIX 0 C11 1 0.954982 0.539500 0.272449 31.00000 0.02778 0.03966 = 0.02669 0.00892 0.00475 -0.00163 C12 1 0.891621 0.608096 0.285137 31.00000 0.02740 0.04278 = 0.03699 0.00257 0.01016 -0.00539 C13 1 0.843748 0.654766 0.197934 31.00000 0.03184 0.04106 = 0.04752 0.00272 0.00787 -0.00150 AFIX 43 H13 2 0.853286 0.643755 0.127333 31.00000 -1.20000 AFIX 0 C14 1 0.782247 0.717196 0.213076 31.00000 0.04066 0.04245 = 0.07570 0.00928 0.01759 0.00329 AFIX 43 H14 2 0.750878 0.749246 0.153547 31.00000 -1.20000 AFIX 0 C15 1 0.767082 0.732285 0.316351 31.00000 0.05926 0.05123 = 0.10350 -0.00725 0.04616 0.00527 AFIX 43 H15 2 0.725352 0.774890 0.327710 31.00000 -1.20000 AFIX 0 C16 1 0.812534 0.685491 0.401899 31.00000 0.07837 0.06255 = 0.07122 -0.00675 0.04378 -0.00084 AFIX 43 H16 2 0.802289 0.696216 0.472329 31.00000 -1.20000 AFIX 0 C17 1 0.872452 0.623552 0.386907 31.00000 0.05454 0.05539 = 0.04449 -0.00306 0.02041 -0.00281 AFIX 43 H17 2 0.901153 0.590886 0.446406 31.00000 -1.20000 AFIX 0 C18 1 0.915689 0.488593 0.188712 31.00000 0.02165 0.04582 = 0.02170 0.00901 0.00479 -0.00096 PART 2 C7B 1 0.971137 0.425006 0.194012 -31.00000 0.02571 0.04448 = 0.02499 0.00747 0.00980 -0.00167 C8B 1 1.072063 0.418124 0.275064 -31.00000 0.02591 0.04015 = 0.03076 0.00364 0.00833 0.00122 AFIX 43 H8B 2 1.117593 0.375476 0.273640 -31.00000 -1.20000 AFIX 0 C9B 1 1.107124 0.469741 0.355106 -31.00000 0.02369 0.04904 = 0.02803 0.00580 0.00523 0.00427 AFIX 43 H9B 2 1.171710 0.459813 0.411901 -31.00000 -1.20000 AFIX 0 C10B 1 1.051378 0.535270 0.355253 -31.00000 0.03068 0.04239 = 0.02675 0.00022 0.00320 -0.00330 AFIX 43 H10B 2 1.078401 0.571991 0.409594 -31.00000 -1.20000 AFIX 0 C11B 1 0.952473 0.547848 0.273136 -31.00000 0.02778 0.03966 = 0.02669 0.00892 0.00475 -0.00163 C12B 1 0.880632 0.609235 0.296229 -31.00000 0.02740 0.04278 = 0.03699 0.00257 0.01016 -0.00539 C13B 1 0.835811 0.662193 0.215127 -31.00000 0.03184 0.04106 = 0.04752 0.00272 0.00787 -0.00150 AFIX 43 H13B 2 0.845588 0.658298 0.143174 -31.00000 -1.20000 AFIX 0 C14B 1 0.776673 0.720247 0.246462 -31.00000 0.04066 0.04245 = 0.07570 0.00928 0.01759 0.00329 AFIX 43 H14B 2 0.738901 0.754506 0.192501 -31.00000 -1.20000 AFIX 0 C15B 1 0.770201 0.730482 0.351646 -31.00000 0.05926 0.05123 = 0.10350 -0.00725 0.04616 0.00527 AFIX 43 H15B 2 0.729611 0.771794 0.369431 -31.00000 -1.20000 AFIX 0 C16B 1 0.821356 0.682051 0.431180 -31.00000 0.07837 0.06255 = 0.07122 -0.00675 0.04378 -0.00084 AFIX 43 H16B 2 0.816066 0.688789 0.504209 -31.00000 -1.20000 AFIX 0 C17B 1 0.880884 0.623142 0.403999 -31.00000 0.05454 0.05539 = 0.04449 -0.00306 0.02041 -0.00281 AFIX 43 H17B 2 0.922652 0.591626 0.459752 -31.00000 -1.20000 AFIX 0 C18B 1 0.910291 0.491163 0.198218 -31.00000 0.02165 0.04582 = 0.02170 0.00901 0.00479 -0.00096 PART 0 HKLF 4 REM test in P2(1)/c REM R1 = 0.0485 for 4560 Fo > 4sig(Fo) and 0.0637 for all 5769 data REM 428 parameters refined using 54 restraints END WGHT 0.0489 1.7421 REM Highest difference peak 0.391, deepest hole -0.378, 1-sigma level 0.041 Q1 1 0.5271 0.2714 0.5337 11.00000 0.05 0.39 Q2 1 0.3360 0.4106 0.4082 11.00000 0.05 0.38 Q3 1 0.6209 0.2748 0.5387 11.00000 0.05 0.33 Q4 1 0.5452 0.3806 0.5644 11.00000 0.05 0.30 Q5 1 0.5222 0.4654 0.1648 11.00000 0.05 0.29 Q6 1 0.5818 0.4486 0.2582 11.00000 0.05 0.28 Q7 1 0.4629 0.4771 0.0737 11.00000 0.05 0.27 Q8 1 0.4422 0.4100 0.3027 11.00000 0.05 0.27 Q9 1 0.3985 0.4844 -0.0204 11.00000 0.05 0.26 Q10 1 0.6386 0.4270 0.3383 11.00000 0.05 0.26 Q11 1 0.6604 0.4832 0.1048 11.00000 0.05 0.25 Q12 1 0.4785 0.4438 0.2405 11.00000 0.05 0.25 Q13 1 0.7043 0.3753 0.4471 11.00000 0.05 0.24 Q14 1 0.5614 0.4910 0.0920 11.00000 0.05 0.23 Q15 1 0.5993 0.3875 0.4017 11.00000 0.05 0.23 Q16 1 0.5725 0.3297 0.5363 11.00000 0.05 0.23 Q17 1 0.9119 0.2584 -0.0193 11.00000 0.05 0.22 Q18 1 0.6732 0.4323 0.2678 11.00000 0.05 0.21 Q19 1 0.3802 0.4334 0.2253 11.00000 0.05 0.21 Q20 1 0.3575 0.4832 0.0650 11.00000 0.05 0.21 ; _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^)+(0.0489P)^2^+1.7424P] 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 5769 _refine_ls_number_parameters 428 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _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 0.36636(10) 0.36488(8) 0.39199(9) 0.0409(3) Uani 1 1 d . . . O3 O 0.73841(10) 0.41237(8) 0.46407(9) 0.0431(3) Uani 1 1 d . . . N42 N 0.55130(11) 0.39188(7) 0.43383(10) 0.0259(3) Uani 1 1 d . . . C1 C 0.90712(17) 0.39013(12) -0.01828(16) 0.0465(5) Uani 1 1 d . B . H1 H 0.9152 0.4410 -0.0365 0.056 Uiso 1 1 calc R . . C2 C 0.87324(19) 0.33760(14) -0.10071(18) 0.0571(6) Uani 1 1 d . . . H2 H 0.8596 0.3526 -0.1748 0.068 Uiso 1 1 calc R . . C3 C 0.85925(19) 0.26352(14) -0.0753(2) 0.0601(6) Uani 1 1 d . . . H3 H 0.8347 0.2278 -0.1317 0.072 Uiso 1 1 calc R . . C4 C 0.88118(18) 0.24199(13) 0.0322(2) 0.0572(6) Uani 1 1 d . . . H4 H 0.8719 0.1911 0.0499 0.069 Uiso 1 1 calc R . . C5 C 0.91662(16) 0.29375(12) 0.11520(18) 0.0478(5) Uani 1 1 d . B . H5 H 0.9323 0.2780 0.1891 0.057 Uiso 1 1 calc R . . C6 C 0.92931(14) 0.36875(11) 0.09072(15) 0.0378(4) Uani 1 1 d . . . C21 C 0.71562(12) 0.48434(9) 0.14808(12) 0.0250(3) Uani 1 1 d . A . C22 C 0.61148(12) 0.49329(8) 0.07302(11) 0.0218(3) Uani 1 1 d . . . C23 C 0.51381(12) 0.47337(8) 0.10850(11) 0.0213(3) Uani 1 1 d . . . C24 C 0.40351(12) 0.47874(8) 0.03860(11) 0.0239(3) Uani 1 1 d . . . C25 C 0.31416(14) 0.45650(11) 0.08012(13) 0.0362(4) Uani 1 1 d . . . H25 H 0.2406 0.4602 0.0348 0.043 Uiso 1 1 calc R . . C26 C 0.32860(14) 0.42906(11) 0.18551(13) 0.0370(4) Uani 1 1 d . A . H26 H 0.2653 0.4137 0.2101 0.044 Uiso 1 1 calc R . . C28 C 0.43230(13) 0.42388(9) 0.25382(12) 0.0263(3) Uani 1 1 d . . . C29 C 0.52541(12) 0.44652(8) 0.21687(11) 0.0217(3) Uani 1 1 d . A . C30 C 0.63139(13) 0.44113(8) 0.28826(11) 0.0238(3) Uani 1 1 d . . . C31 C 0.72461(13) 0.45898(9) 0.25424(12) 0.0267(3) Uani 1 1 d . A . H31 H 0.7962 0.4542 0.3031 0.032 Uiso 1 1 calc R . . C32 C 0.64650(13) 0.41463(9) 0.40173(12) 0.0274(3) Uani 1 1 d . A . C43 C 0.44545(14) 0.39154(9) 0.36402(12) 0.0283(3) Uani 1 1 d . A . C33 C 0.57445(19) 0.35886(11) 0.54564(16) 0.0240(4) Uiso 0.840(4) 1 d P A 1 H33 H 0.6518 0.3748 0.5840 0.029 Uiso 0.840(4) 1 calc PR A 1 C34 C 0.49728(19) 0.38784(12) 0.61349(15) 0.0348(5) Uani 0.840(4) 1 d P A 1 H34A H 0.4197 0.3711 0.5815 0.042 Uiso 0.840(4) 1 calc PR A 1 H34B H 0.4982 0.4432 0.6147 0.042 Uiso 0.840(4) 1 calc PR A 1 C35 C 0.5386(3) 0.35697(14) 0.73015(16) 0.0398(6) Uani 0.840(4) 1 d P A 1 H35A H 0.6133 0.3780 0.7639 0.048 Uiso 0.840(4) 1 calc PR A 1 H35B H 0.4868 0.3729 0.7745 0.048 Uiso 0.840(4) 1 calc PR A 1 C36 C 0.5456(2) 0.27198(13) 0.73008(16) 0.0406(6) Uani 0.840(4) 1 d P A 1 H36A H 0.5777 0.2543 0.8054 0.049 Uiso 0.840(4) 1 calc PR A 1 H36B H 0.4693 0.2510 0.7055 0.049 Uiso 0.840(4) 1 calc PR A 1 C37 C 0.6163(3) 0.24351(14) 0.6567(2) 0.0382(6) Uani 0.840(4) 1 d P A 1 H37A H 0.6136 0.1882 0.6550 0.046 Uiso 0.840(4) 1 calc PR A 1 H37B H 0.6949 0.2587 0.6870 0.046 Uiso 0.840(4) 1 calc PR A 1 C38 C 0.57610(14) 0.27381(10) 0.53980(14) 0.0332(4) Uiso 0.840(4) 1 d P A 1 H38A H 0.6272 0.2573 0.4951 0.040 Uiso 0.840(4) 1 calc PR A 1 H38B H 0.5003 0.2547 0.5058 0.040 Uiso 0.840(4) 1 calc PR A 1 C33B C 0.5363(11) 0.3540(6) 0.5387(8) 0.0240(4) Uiso 0.160(4) 1 d P A 2 H33B H 0.4557 0.3551 0.5404 0.029 Uiso 0.160(4) 1 calc PR A 2 C34B C 0.6032(10) 0.3940(7) 0.6326(9) 0.039(3) Uani 0.160(4) 1 d PU A 2 H34C H 0.5734 0.4453 0.6343 0.047 Uiso 0.160(4) 1 calc PR A 2 H34D H 0.6812 0.3980 0.6257 0.047 Uiso 0.160(4) 1 calc PR A 2 C35B C 0.6018(15) 0.3537(9) 0.7387(12) 0.051(4) Uani 0.160(4) 1 d PU A 2 H35C H 0.5260 0.3569 0.7516 0.061 Uiso 0.160(4) 1 calc PR A 2 H35D H 0.6545 0.3786 0.8003 0.061 Uiso 0.160(4) 1 calc PR A 2 C36B C 0.6349(12) 0.2710(8) 0.7338(11) 0.048(3) Uani 0.160(4) 1 d PU A 2 H36C H 0.7147 0.2682 0.7326 0.058 Uiso 0.160(4) 1 calc PR A 2 H36D H 0.6263 0.2453 0.8005 0.058 Uiso 0.160(4) 1 calc PR A 2 C37B C 0.5672(17) 0.2313(11) 0.6371(15) 0.059(5) Uani 0.160(4) 1 d PU A 2 H37C H 0.5955 0.1798 0.6338 0.071 Uiso 0.160(4) 1 calc PR A 2 H37D H 0.4882 0.2285 0.6411 0.071 Uiso 0.160(4) 1 calc PR A 2 C38B C 0.57610(14) 0.27381(10) 0.53980(14) 0.0332(4) Uiso 0.160(4) 1 d P A 2 H38C H 0.5317 0.2480 0.4741 0.040 Uiso 0.160(4) 1 calc PR A 2 H38D H 0.6551 0.2738 0.5355 0.040 Uiso 0.160(4) 1 calc PR A 2 O2 O 0.81136(9) 0.50142(7) 0.11651(9) 0.0316(3) Uani 1 1 d D . . C7 C 0.9713(7) 0.4228(5) 0.1760(7) 0.0311(10) Uani 0.77(3) 1 d PD B 1 C8 C 1.0706(5) 0.4068(4) 0.2532(7) 0.0320(10) Uani 0.77(3) 1 d PD B 1 H8 H 1.1081 0.3609 0.2494 0.038 Uiso 0.77(3) 1 calc PR B 1 C9 C 1.1148(5) 0.4576(5) 0.3352(7) 0.0338(11) Uani 0.77(3) 1 d PD B 1 H9 H 1.1843 0.4476 0.3852 0.041 Uiso 0.77(3) 1 calc PR B 1 C10 C 1.0575(6) 0.5226(5) 0.3441(7) 0.0339(10) Uani 0.77(3) 1 d PD B 1 H10 H 1.0888 0.5569 0.4007 0.041 Uiso 0.77(3) 1 calc PR B 1 C11 C 0.9550(9) 0.5395(6) 0.2724(10) 0.0317(8) Uani 0.77(3) 1 d PD B 1 C12 C 0.8916(9) 0.6081(5) 0.2851(7) 0.0353(11) Uani 0.77(3) 1 d PD B 1 C13 C 0.8437(9) 0.6548(5) 0.1979(7) 0.0405(9) Uani 0.77(3) 1 d PD B 1 H13 H 0.8533 0.6438 0.1273 0.049 Uiso 0.77(3) 1 calc PR B 1 C14 C 0.7822(5) 0.7172(3) 0.2131(10) 0.0524(15) Uani 0.77(3) 1 d PD B 1 H14 H 0.7509 0.7492 0.1535 0.063 Uiso 0.77(3) 1 calc PR B 1 C15 C 0.7671(7) 0.7323(4) 0.3164(11) 0.0668(18) Uani 0.77(3) 1 d PD B 1 H15 H 0.7254 0.7749 0.3277 0.080 Uiso 0.77(3) 1 calc PR B 1 C16 C 0.8125(10) 0.6855(5) 0.4019(9) 0.0663(14) Uani 0.77(3) 1 d PD B 1 H16 H 0.8023 0.6962 0.4723 0.080 Uiso 0.77(3) 1 calc PR B 1 C17 C 0.8725(15) 0.6236(8) 0.3869(8) 0.0500(12) Uani 0.77(3) 1 d PD B 1 H17 H 0.9012 0.5909 0.4464 0.060 Uiso 0.77(3) 1 calc PR B 1 C18 C 0.9157(9) 0.4886(8) 0.1887(10) 0.0298(14) Uani 0.77(3) 1 d PD B 1 C7B C 0.971(2) 0.4250(18) 0.194(2) 0.0311(10) Uani 0.23(3) 1 d PD B 2 C8B C 1.072(2) 0.4181(14) 0.2751(19) 0.0320(10) Uani 0.23(3) 1 d PD B 2 H8B H 1.1176 0.3755 0.2736 0.038 Uiso 0.23(3) 1 calc PR B 2 C9B C 1.1071(18) 0.4697(14) 0.3551(17) 0.0338(11) Uani 0.23(3) 1 d PD B 2 H9B H 1.1717 0.4598 0.4119 0.041 Uiso 0.23(3) 1 calc PR B 2 C10B C 1.051(2) 0.5353(16) 0.355(2) 0.0339(10) Uani 0.23(3) 1 d PD B 2 H10B H 1.0784 0.5720 0.4096 0.041 Uiso 0.23(3) 1 calc PR B 2 C11B C 0.952(3) 0.548(2) 0.273(4) 0.0317(8) Uani 0.23(3) 1 d PD B 2 C12B C 0.881(3) 0.6092(18) 0.296(3) 0.0353(11) Uani 0.23(3) 1 d PD B 2 C13B C 0.836(3) 0.6622(17) 0.215(2) 0.0405(9) Uani 0.23(3) 1 d PD B 2 H13B H 0.8456 0.6583 0.1432 0.049 Uiso 0.23(3) 1 calc PR B 2 C14B C 0.777(2) 0.7202(13) 0.246(2) 0.0524(15) Uani 0.23(3) 1 d PD B 2 H14B H 0.7389 0.7545 0.1925 0.063 Uiso 0.23(3) 1 calc PR B 2 C15B C 0.770(3) 0.7305(17) 0.352(3) 0.0668(18) Uani 0.23(3) 1 d PD B 2 H15B H 0.7296 0.7718 0.3694 0.080 Uiso 0.23(3) 1 calc PR B 2 C16B C 0.821(4) 0.682(2) 0.431(2) 0.0663(14) Uani 0.23(3) 1 d PD B 2 H16B H 0.8161 0.6888 0.5042 0.080 Uiso 0.23(3) 1 calc PR B 2 C17B C 0.881(6) 0.623(3) 0.404(3) 0.0500(12) Uani 0.23(3) 1 d PD B 2 H17B H 0.9227 0.5916 0.4598 0.060 Uiso 0.23(3) 1 calc PR B 2 C18B C 0.910(3) 0.491(3) 0.198(4) 0.0298(14) Uani 0.23(3) 1 d PD B 2 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 0.0399(7) 0.0576(8) 0.0255(6) 0.0092(5) 0.0086(5) -0.0138(6) O3 0.0346(7) 0.0675(9) 0.0239(6) 0.0150(6) 0.0009(5) 0.0011(6) N42 0.0363(7) 0.0236(7) 0.0175(6) 0.0034(5) 0.0058(5) -0.0005(5) C1 0.0494(11) 0.0527(12) 0.0414(10) 0.0007(9) 0.0187(9) -0.0037(9) C2 0.0625(14) 0.0671(15) 0.0450(12) -0.0078(10) 0.0197(10) -0.0052(11) C3 0.0559(13) 0.0625(15) 0.0630(15) -0.0189(12) 0.0167(11) -0.0061(11) C4 0.0469(12) 0.0435(12) 0.0785(16) -0.0041(11) 0.0103(11) -0.0040(9) C5 0.0368(10) 0.0495(12) 0.0562(12) 0.0070(10) 0.0099(9) -0.0016(9) C6 0.0264(8) 0.0454(11) 0.0435(10) 0.0025(8) 0.0124(7) 0.0001(7) C21 0.0246(7) 0.0278(8) 0.0222(7) 0.0019(6) 0.0051(6) -0.0011(6) C22 0.0254(7) 0.0213(7) 0.0183(7) 0.0013(5) 0.0048(5) 0.0002(6) C23 0.0268(7) 0.0195(7) 0.0171(6) 0.0003(5) 0.0047(5) 0.0001(6) C24 0.0253(7) 0.0268(8) 0.0191(7) 0.0015(6) 0.0043(6) -0.0012(6) C25 0.0262(8) 0.0564(11) 0.0245(8) 0.0091(7) 0.0032(6) -0.0047(8) C26 0.0300(8) 0.0562(12) 0.0260(8) 0.0095(8) 0.0095(7) -0.0059(8) C28 0.0304(8) 0.0291(8) 0.0191(7) 0.0027(6) 0.0058(6) -0.0024(6) C29 0.0284(7) 0.0183(7) 0.0181(7) 0.0006(5) 0.0052(6) -0.0003(6) C30 0.0306(8) 0.0218(7) 0.0180(7) 0.0009(6) 0.0045(6) 0.0008(6) C31 0.0245(7) 0.0317(8) 0.0212(7) 0.0028(6) 0.0005(6) 0.0011(6) C32 0.0326(8) 0.0281(8) 0.0202(7) 0.0030(6) 0.0039(6) 0.0024(6) C43 0.0353(9) 0.0280(8) 0.0225(7) 0.0016(6) 0.0089(6) -0.0049(7) C34 0.0549(14) 0.0296(11) 0.0219(9) 0.0002(8) 0.0129(9) 0.0054(9) C35 0.0591(17) 0.0443(13) 0.0181(10) 0.0002(9) 0.0133(10) -0.0020(12) C36 0.0531(14) 0.0442(13) 0.0243(10) 0.0149(9) 0.0093(9) -0.0034(10) C37 0.0512(16) 0.0317(12) 0.0313(12) 0.0131(10) 0.0092(11) 0.0044(12) C34B 0.045(4) 0.037(4) 0.037(4) -0.001(3) 0.012(3) -0.002(3) C35B 0.052(5) 0.053(5) 0.049(5) 0.002(3) 0.014(3) -0.001(3) C36B 0.051(4) 0.049(4) 0.045(4) 0.005(3) 0.013(3) 0.001(3) C37B 0.060(6) 0.057(6) 0.059(6) 0.005(3) 0.013(3) -0.002(3) O2 0.0215(5) 0.0489(7) 0.0229(5) 0.0089(5) 0.0028(4) -0.0001(5) C7 0.0257(8) 0.0445(12) 0.025(3) 0.0075(17) 0.0098(16) -0.0017(8) C8 0.0259(8) 0.040(2) 0.031(3) 0.0036(16) 0.0083(16) 0.0012(13) C9 0.0237(12) 0.049(3) 0.028(2) 0.0058(18) 0.0052(14) 0.0043(13) C10 0.0307(13) 0.042(3) 0.027(2) 0.0002(16) 0.0032(13) -0.0033(16) C11 0.0278(10) 0.040(3) 0.0267(8) 0.0089(16) 0.0048(7) -0.0016(13) C12 0.027(2) 0.0428(11) 0.037(2) 0.0026(13) 0.0102(14) -0.0054(11) C13 0.0318(18) 0.041(2) 0.048(3) 0.0027(18) 0.0079(17) -0.0015(12) C14 0.0407(14) 0.0425(14) 0.076(4) 0.009(2) 0.018(2) 0.0033(10) C15 0.0593(17) 0.0512(16) 0.103(6) -0.007(3) 0.046(4) 0.0053(12) C16 0.078(3) 0.063(2) 0.071(4) -0.007(3) 0.044(4) -0.0008(17) C17 0.055(3) 0.0554(13) 0.044(3) -0.003(3) 0.020(3) -0.0028(15) C18 0.0217(14) 0.0458(14) 0.022(3) 0.0090(12) 0.0048(18) -0.0010(8) C7B 0.0257(8) 0.0445(12) 0.025(3) 0.0075(17) 0.0098(16) -0.0017(8) C8B 0.0259(8) 0.040(2) 0.031(3) 0.0036(16) 0.0083(16) 0.0012(13) C9B 0.0237(12) 0.049(3) 0.028(2) 0.0058(18) 0.0052(14) 0.0043(13) C10B 0.0307(13) 0.042(3) 0.027(2) 0.0002(16) 0.0032(13) -0.0033(16) C11B 0.0278(10) 0.040(3) 0.0267(8) 0.0089(16) 0.0048(7) -0.0016(13) C12B 0.027(2) 0.0428(11) 0.037(2) 0.0026(13) 0.0102(14) -0.0054(11) C13B 0.0318(18) 0.041(2) 0.048(3) 0.0027(18) 0.0079(17) -0.0015(12) C14B 0.0407(14) 0.0425(14) 0.076(4) 0.009(2) 0.018(2) 0.0033(10) C15B 0.0593(17) 0.0512(16) 0.103(6) -0.007(3) 0.046(4) 0.0053(12) C16B 0.078(3) 0.063(2) 0.071(4) -0.007(3) 0.044(4) -0.0008(17) C17B 0.055(3) 0.0554(13) 0.044(3) -0.003(3) 0.020(3) -0.0028(15) C18B 0.0217(14) 0.0458(14) 0.022(3) 0.0090(12) 0.0048(18) -0.0010(8) _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 C43 1.2147(19) . ? O3 C32 1.2133(19) . ? N42 C43 1.386(2) . ? N42 C32 1.395(2) . ? N42 C33 1.495(2) . ? N42 C33B 1.541(11) . ? C1 C2 1.389(3) . ? C1 C6 1.392(3) . ? C2 C3 1.384(3) . ? C3 C4 1.376(3) . ? C4 C5 1.387(3) . ? C5 C6 1.393(3) . ? C6 C7 1.447(8) . ? C6 C7B 1.63(2) . ? C21 O2 1.3717(18) . ? C21 C31 1.396(2) . ? C21 C22 1.408(2) . ? C22 C23 1.431(2) . ? C22 C24 1.4667(19) 3_665 ? C23 C29 1.4266(19) . ? C23 C24 1.433(2) . ? C24 C25 1.391(2) . ? C24 C22 1.4667(19) 3_665 ? C25 C26 1.391(2) . ? C26 C28 1.361(2) . ? C28 C29 1.403(2) . ? C28 C43 1.481(2) . ? C29 C30 1.399(2) . ? C30 C31 1.362(2) . ? C30 C32 1.480(2) . ? C33 C34 1.521(3) . ? C33 C38 1.522(3) . ? C34 C35 1.541(3) . ? C35 C36 1.522(3) . ? C36 C37 1.510(3) . ? C37 C38 1.539(3) . ? C33B C34B 1.457(16) . ? C34B C35B 1.528(18) . ? C35B C36B 1.54(2) . ? C36B C37B 1.48(2) . ? O2 C18 1.403(3) . ? O2 C18B 1.405(5) . ? C7 C18 1.390(5) . ? C7 C8 1.397(5) . ? C8 C9 1.386(4) . ? C9 C10 1.379(4) . ? C10 C11 1.398(5) . ? C11 C18 1.391(5) . ? C11 C12 1.484(5) . ? C12 C17 1.393(5) . ? C12 C13 1.394(5) . ? C13 C14 1.389(5) . ? C14 C15 1.391(5) . ? C15 C16 1.374(6) . ? C16 C17 1.370(5) . ? C7B C18B 1.409(15) . ? C7B C8B 1.411(15) . ? C8B C9B 1.360(14) . ? C9B C10B 1.359(15) . ? C10B C11B 1.414(15) . ? C11B C18B 1.398(15) . ? C11B C12B 1.484(15) . ? C12B C17B 1.386(15) . ? C12B C13B 1.406(15) . ? C13B C14B 1.382(15) . ? C14B C15B 1.365(15) . ? C15B C16B 1.360(16) . ? C16B C17B 1.375(15) . ? 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 C43 N42 C32 123.06(12) . . ? C43 N42 C33 122.20(14) . . ? C32 N42 C33 114.32(14) . . ? C43 N42 C33B 104.7(5) . . ? C32 N42 C33B 131.8(5) . . ? C33 N42 C33B 17.6(5) . . ? C2 C1 C6 120.5(2) . . ? C3 C2 C1 120.3(2) . . ? C4 C3 C2 119.5(2) . . ? C3 C4 C5 120.7(2) . . ? C4 C5 C6 120.4(2) . . ? C1 C6 C5 118.61(19) . . ? C1 C6 C7 120.2(4) . . ? C5 C6 C7 121.1(4) . . ? C1 C6 C7B 124.9(13) . . ? C5 C6 C7B 116.5(13) . . ? C7 C6 C7B 5.3(18) . . ? O2 C21 C31 118.80(13) . . ? O2 C21 C22 119.19(13) . . ? C31 C21 C22 122.00(14) . . ? C21 C22 C23 117.40(13) . . ? C21 C22 C24 124.55(13) . 3_665 ? C23 C22 C24 118.05(13) . 3_665 ? C29 C23 C22 119.47(13) . . ? C29 C23 C24 118.15(13) . . ? C22 C23 C24 122.38(13) . . ? C25 C24 C23 117.97(13) . . ? C25 C24 C22 122.47(14) . 3_665 ? C23 C24 C22 119.56(13) . 3_665 ? C26 C25 C24 122.42(15) . . ? C28 C26 C25 120.82(15) . . ? C26 C28 C29 119.26(14) . . ? C26 C28 C43 119.56(14) . . ? C29 C28 C43 121.13(14) . . ? C30 C29 C28 118.55(13) . . ? C30 C29 C23 120.08(13) . . ? C28 C29 C23 121.36(13) . . ? C31 C30 C29 120.57(13) . . ? C31 C30 C32 117.83(13) . . ? C29 C30 C32 121.59(13) . . ? C30 C31 C21 120.43(14) . . ? O3 C32 N42 121.42(14) . . ? O3 C32 C30 121.11(14) . . ? N42 C32 C30 117.48(13) . . ? O1 C43 N42 121.03(14) . . ? O1 C43 C28 121.15(14) . . ? N42 C43 C28 117.82(13) . . ? N42 C33 C34 113.52(16) . . ? N42 C33 C38 110.50(15) . . ? C34 C33 C38 112.65(17) . . ? C33 C34 C35 108.23(18) . . ? C36 C35 C34 111.25(17) . . ? C37 C36 C35 112.21(19) . . ? C36 C37 C38 111.95(19) . . ? C33 C38 C37 108.05(16) . . ? C34B C33B N42 108.8(9) . . ? C33B C34B C35B 111.0(10) . . ? C34B C35B C36B 110.9(12) . . ? C37B C36B C35B 113.0(13) . . ? C21 O2 C18 119.5(9) . . ? C21 O2 C18B 114(3) . . ? C18 O2 C18B 6(3) . . ? C18 C7 C8 117.8(4) . . ? C18 C7 C6 123.7(5) . . ? C8 C7 C6 118.5(6) . . ? C9 C8 C7 120.4(4) . . ? C10 C9 C8 119.8(4) . . ? C9 C10 C11 122.0(4) . . ? C18 C11 C10 116.4(4) . . ? C18 C11 C12 121.9(6) . . ? C10 C11 C12 121.7(5) . . ? C17 C12 C13 118.6(4) . . ? C17 C12 C11 118.5(6) . . ? C13 C12 C11 122.8(5) . . ? C14 C13 C12 120.8(4) . . ? C13 C14 C15 119.3(4) . . ? C16 C15 C14 119.9(4) . . ? C17 C16 C15 120.8(4) . . ? C16 C17 C12 120.5(5) . . ? C7 C18 C11 123.5(4) . . ? C7 C18 O2 117.6(6) . . ? C11 C18 O2 118.8(6) . . ? C18B C7B C8B 115.4(15) . . ? C18B C7B C6 118.8(18) . . ? C8B C7B C6 125.3(18) . . ? C9B C8B C7B 123.0(16) . . ? C10B C9B C8B 121.1(16) . . ? C9B C10B C11B 118.8(16) . . ? C18B C11B C10B 119.6(15) . . ? C18B C11B C12B 122(2) . . ? C10B C11B C12B 115.0(18) . . ? C17B C12B C13B 120.2(17) . . ? C17B C12B C11B 118.0(19) . . ? C13B C12B C11B 120(2) . . ? C14B C13B C12B 115.9(16) . . ? C15B C14B C13B 122.8(18) . . ? C16B C15B C14B 120.6(18) . . ? C15B C16B C17B 118.8(18) . . ? C16B C17B C12B 120.8(19) . . ? C11B C18B O2 121(2) . . ? C11B C18B C7B 121.4(13) . . ? O2 C18B C7B 117.2(19) . . ? 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 C6 C1 C2 C3 1.1(3) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 0.8(3) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? C2 C1 C6 C7 176.1(4) . . . . ? C2 C1 C6 C7B 179.1(13) . . . . ? C4 C5 C6 C1 -0.8(3) . . . . ? C4 C5 C6 C7 -177.0(4) . . . . ? C4 C5 C6 C7B 179.9(12) . . . . ? O2 C21 C22 C23 178.73(13) . . . . ? C31 C21 C22 C23 -1.7(2) . . . . ? O2 C21 C22 C24 -1.0(2) . . . 3_665 ? C31 C21 C22 C24 178.55(15) . . . 3_665 ? C21 C22 C23 C29 0.7(2) . . . . ? C24 C22 C23 C29 -179.52(13) 3_665 . . . ? C21 C22 C23 C24 -178.79(14) . . . . ? C24 C22 C23 C24 1.0(2) 3_665 . . . ? C29 C23 C24 C25 -0.8(2) . . . . ? C22 C23 C24 C25 178.65(15) . . . . ? C29 C23 C24 C22 179.49(13) . . . 3_665 ? C22 C23 C24 C22 -1.0(2) . . . 3_665 ? C23 C24 C25 C26 -0.5(3) . . . . ? C22 C24 C25 C26 179.14(17) 3_665 . . . ? C24 C25 C26 C28 1.0(3) . . . . ? C25 C26 C28 C29 -0.1(3) . . . . ? C25 C26 C28 C43 -177.50(17) . . . . ? C26 C28 C29 C30 179.75(15) . . . . ? C43 C28 C29 C30 -2.9(2) . . . . ? C26 C28 C29 C23 -1.3(2) . . . . ? C43 C28 C29 C23 176.05(14) . . . . ? C22 C23 C29 C30 1.2(2) . . . . ? C24 C23 C29 C30 -179.31(13) . . . . ? C22 C23 C29 C28 -177.73(14) . . . . ? C24 C23 C29 C28 1.8(2) . . . . ? C28 C29 C30 C31 176.76(15) . . . . ? C23 C29 C30 C31 -2.2(2) . . . . ? C28 C29 C30 C32 -2.0(2) . . . . ? C23 C29 C30 C32 179.06(14) . . . . ? C29 C30 C31 C21 1.2(2) . . . . ? C32 C30 C31 C21 -179.96(14) . . . . ? O2 C21 C31 C30 -179.65(14) . . . . ? C22 C21 C31 C30 0.7(2) . . . . ? C43 N42 C32 O3 -178.00(16) . . . . ? C33 N42 C32 O3 -5.3(2) . . . . ? C33B N42 C32 O3 -6.9(6) . . . . ? C43 N42 C32 C30 1.5(2) . . . . ? C33 N42 C32 C30 174.25(14) . . . . ? C33B N42 C32 C30 172.6(5) . . . . ? C31 C30 C32 O3 3.6(2) . . . . ? C29 C30 C32 O3 -177.66(15) . . . . ? C31 C30 C32 N42 -175.97(14) . . . . ? C29 C30 C32 N42 2.8(2) . . . . ? C32 N42 C43 O1 173.10(16) . . . . ? C33 N42 C43 O1 0.9(2) . . . . ? C33B N42 C43 O1 0.0(4) . . . . ? C32 N42 C43 C28 -6.2(2) . . . . ? C33 N42 C43 C28 -178.33(14) . . . . ? C33B N42 C43 C28 -179.3(4) . . . . ? C26 C28 C43 O1 5.0(3) . . . . ? C29 C28 C43 O1 -172.33(16) . . . . ? C26 C28 C43 N42 -175.70(15) . . . . ? C29 C28 C43 N42 6.9(2) . . . . ? C43 N42 C33 C34 -52.3(2) . . . . ? C32 N42 C33 C34 134.90(17) . . . . ? C33B N42 C33 C34 -49.3(14) . . . . ? C43 N42 C33 C38 75.4(2) . . . . ? C32 N42 C33 C38 -97.44(18) . . . . ? C33B N42 C33 C38 78.4(14) . . . . ? N42 C33 C34 C35 -173.34(18) . . . . ? C38 C33 C34 C35 60.1(2) . . . . ? C33 C34 C35 C36 -55.9(3) . . . . ? C34 C35 C36 C37 54.6(3) . . . . ? C35 C36 C37 C38 -54.6(3) . . . . ? N42 C33 C38 C37 172.19(16) . . . . ? C34 C33 C38 C37 -59.7(2) . . . . ? C36 C37 C38 C33 55.6(3) . . . . ? C43 N42 C33B C34B -139.6(8) . . . . ? C32 N42 C33B C34B 48.1(10) . . . . ? C33 N42 C33B C34B 43.1(12) . . . . ? N42 C33B C34B C35B -173.7(10) . . . . ? C33B C34B C35B C36B 52.7(15) . . . . ? C34B C35B C36B C37B -53.3(17) . . . . ? C31 C21 O2 C18 4.0(5) . . . . ? C22 C21 O2 C18 -176.4(5) . . . . ? C31 C21 O2 C18B -0.3(15) . . . . ? C22 C21 O2 C18B 179.3(15) . . . . ? C1 C6 C7 C18 58.1(14) . . . . ? C5 C6 C7 C18 -125.7(12) . . . . ? C7B C6 C7 C18 -94(13) . . . . ? C1 C6 C7 C8 -124.9(7) . . . . ? C5 C6 C7 C8 51.2(9) . . . . ? C7B C6 C7 C8 83(13) . . . . ? C18 C7 C8 C9 -3.9(16) . . . . ? C6 C7 C8 C9 178.9(6) . . . . ? C7 C8 C9 C10 3.3(11) . . . . ? C8 C9 C10 C11 0.0(15) . . . . ? C9 C10 C11 C18 -2(2) . . . . ? C9 C10 C11 C12 177.5(11) . . . . ? C18 C11 C12 C17 129.6(18) . . . . ? C10 C11 C12 C17 -50(2) . . . . ? C18 C11 C12 C13 -46(2) . . . . ? C10 C11 C12 C13 134.3(14) . . . . ? C17 C12 C13 C14 3(2) . . . . ? C11 C12 C13 C14 178.0(11) . . . . ? C12 C13 C14 C15 -1.0(16) . . . . ? C13 C14 C15 C16 -0.2(15) . . . . ? C14 C15 C16 C17 -0.4(19) . . . . ? C15 C16 C17 C12 2(3) . . . . ? C13 C12 C17 C16 -3(3) . . . . ? C11 C12 C17 C16 -178.8(14) . . . . ? C8 C7 C18 C11 1(2) . . . . ? C6 C7 C18 C11 178.3(15) . . . . ? C8 C7 C18 O2 -174.8(12) . . . . ? C6 C7 C18 O2 2(2) . . . . ? C10 C11 C18 C7 2(3) . . . . ? C12 C11 C18 C7 -178.2(16) . . . . ? C10 C11 C18 O2 177.9(15) . . . . ? C12 C11 C18 O2 -2(3) . . . . ? C21 O2 C18 C7 97.6(14) . . . . ? C18B O2 C18 C7 135(31) . . . . ? C21 O2 C18 C11 -78.7(18) . . . . ? C18B O2 C18 C11 -41(28) . . . . ? C1 C6 C7B C18B 52(5) . . . . ? C5 C6 C7B C18B -129(4) . . . . ? C7 C6 C7B C18B 81(13) . . . . ? C1 C6 C7B C8B -120(3) . . . . ? C5 C6 C7B C8B 59(4) . . . . ? C7 C6 C7B C8B -91(13) . . . . ? C18B C7B C8B C9B 3(6) . . . . ? C6 C7B C8B C9B 175(3) . . . . ? C7B C8B C9B C10B -7(5) . . . . ? C8B C9B C10B C11B 3(6) . . . . ? C9B C10B C11B C18B 4(8) . . . . ? C9B C10B C11B C12B 163(4) . . . . ? C18B C11B C12B C17B 128(6) . . . . ? C10B C11B C12B C17B -31(7) . . . . ? C18B C11B C12B C13B -67(7) . . . . ? C10B C11B C12B C13B 134(5) . . . . ? C17B C12B C13B C14B -11(7) . . . . ? C11B C12B C13B C14B -176(4) . . . . ? C12B C13B C14B C15B 6(6) . . . . ? C13B C14B C15B C16B -1(7) . . . . ? C14B C15B C16B C17B 1(8) . . . . ? C15B C16B C17B C12B -6(9) . . . . ? C13B C12B C17B C16B 11(9) . . . . ? C11B C12B C17B C16B 176(5) . . . . ? C10B C11B C18B O2 179(5) . . . . ? C12B C11B C18B O2 21(9) . . . . ? C10B C11B C18B C7B -8(10) . . . . ? C12B C11B C18B C7B -166(5) . . . . ? C21 O2 C18B C11B -87(6) . . . . ? C18 O2 C18B C11B 129(34) . . . . ? C21 O2 C18B C7B 100(5) . . . . ? C18 O2 C18B C7B -44(24) . . . . ? C8B C7B C18B C11B 5(9) . . . . ? C6 C7B C18B C11B -168(5) . . . . ? C8B C7B C18B O2 178(4) . . . . ? C6 C7B C18B O2 5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.82 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.391 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.041