#------------------------------------------------------------------------------ #$Date: 2021-10-01 03:50:57 +0300 (Fri, 01 Oct 2021) $ #$Revision: 269419 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/83/7158329.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_7158329 loop_ _publ_author_name 'Marras, Valentina' 'Caboni, P.' 'Secci, Francesco' 'Guillot, R\'egis' 'Aitken, David J.' 'Frongia, Angelo' _publ_section_title ; A Br\/onsted acid catalyzed tandem reaction for the diastereoselective synthesis of cyclobuta-fused tetrahydroquinoline carboxylic esters ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01518D _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C22 H26 N2 O2' _chemical_formula_sum 'C22 H26 N2 O2' _chemical_formula_weight 350.45 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-31 deposited with the CCDC. 2021-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.5210(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.1401(3) _cell_length_b 28.7617(7) _cell_length_c 11.7457(3) _cell_measurement_reflns_used 9143 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 65.21 _cell_measurement_theta_min 3.07 _cell_volume 3763.26(17) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(1) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker VENTURE PHOTON100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0253 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 50526 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 65.200 _diffrn_reflns_theta_max 65.200 _diffrn_reflns_theta_min 3.073 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_correction_T_min 0.9087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker APEX3' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.237 _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.220 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Flack x determined using 5585 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.06(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 945 _refine_ls_number_reflns 12738 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0324 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.7720P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.0817 _reflns_Friedel_coverage 0.941 _reflns_Friedel_fraction_full 0.983 _reflns_Friedel_fraction_max 0.983 _reflns_number_gt 12154 _reflns_number_total 12738 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01518d2.cif _cod_data_source_block 3s _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7158329 _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 0.906 _shelx_estimated_absorpt_t_max 0.941 _shelx_res_file ; TITL cu_v1075_GuillotICMMO.res in P2(1) shelx.res created by SHELXL-2018/3 at 14:33:28 on 28-May-2021 CELL 1.54178 11.1401 28.7617 11.7457 90.000 90.521 90.000 ZERR 8.00 0.0003 0.0007 0.0003 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O DISP O 0.04946 0.03229 280.59 DISP N 0.03112 0.01806 156.90 DISP C 0.01788 0.00907 78.80 UNIT 176 208 16 16 MERG 2 EADP C70B C72B C71B C67B C69B C68B EADP C67A C68A C69A C70A C71A C72A EADP N7B N7A EADP N7B N7A EADP C73 C74A C75A C76 N7B N7A FMAP 2 PLAN 20 SIZE 0.110 0.160 0.180 ACTA 164.00 BOND $H LIST 6 WPDB -2 L.S. 10 TEMP -173.00 WGHT 0.044900 0.772000 FVAR 0.13167 0.48486 C1 1 1.388701 0.710511 0.406849 11.00000 0.02667 0.01353 = 0.07285 -0.00504 -0.02137 0.00083 AFIX 43 H1 2 1.414563 0.724760 0.475793 11.00000 -1.20000 AFIX 0 C2 1 1.456318 0.715593 0.309287 11.00000 0.01772 0.01674 = 0.10003 0.01042 0.00254 -0.00009 AFIX 43 H2 2 1.528030 0.733443 0.312237 11.00000 -1.20000 AFIX 0 C3 1 1.421650 0.695297 0.208229 11.00000 0.02828 0.01968 = 0.07165 0.01465 0.01082 0.00219 AFIX 43 H3 2 1.469529 0.698617 0.142206 11.00000 -1.20000 AFIX 0 C4 1 1.316598 0.670093 0.203992 11.00000 0.02850 0.01968 = 0.04117 0.01126 0.00639 0.00446 AFIX 43 H4 2 1.291567 0.656274 0.134256 11.00000 -1.20000 AFIX 0 C5 1 1.246831 0.664639 0.300435 11.00000 0.01796 0.01749 = 0.03347 0.00302 -0.00533 0.00005 AFIX 43 H5 2 1.174397 0.647290 0.295585 11.00000 -1.20000 AFIX 0 C6 1 1.281425 0.684251 0.404503 11.00000 0.02171 0.01218 = 0.03954 0.00040 -0.00808 0.00290 C7 1 1.119882 0.644782 0.513816 11.00000 0.02716 0.01888 = 0.01765 -0.00484 -0.00233 0.00522 C8 1 1.093433 0.635191 0.641717 11.00000 0.05170 0.03098 = 0.01700 -0.00685 -0.00169 0.01456 AFIX 23 H8A 2 1.135085 0.656850 0.694336 11.00000 -1.20000 H8B 2 1.006707 0.633559 0.658940 11.00000 -1.20000 AFIX 0 C9 1 1.154109 0.587106 0.633753 11.00000 0.04887 0.02965 = 0.01570 -0.00372 -0.00470 0.01327 AFIX 23 H9A 2 1.101125 0.561012 0.655573 11.00000 -1.20000 H9B 2 1.232106 0.585279 0.674576 11.00000 -1.20000 AFIX 0 C10 1 1.166163 0.593368 0.503434 11.00000 0.02131 0.01801 = 0.01546 -0.00306 -0.00143 0.00328 AFIX 13 H10 2 1.251759 0.592007 0.478733 11.00000 -1.20000 AFIX 0 C11 1 1.086015 0.562036 0.431842 11.00000 0.01392 0.01782 = 0.01684 0.00016 -0.00012 0.00183 AFIX 13 H11 2 1.105591 0.567232 0.349902 11.00000 -1.20000 AFIX 0 C12 1 0.929398 0.619610 0.416175 11.00000 0.01698 0.02147 = 0.02447 0.00371 0.00626 0.00454 C13 1 1.008771 0.655857 0.443431 11.00000 0.02204 0.02120 = 0.01714 -0.00177 0.00444 0.00594 C14 1 0.979902 0.700772 0.408786 11.00000 0.02738 0.02084 = 0.02743 -0.00316 0.00121 0.00457 AFIX 43 H14 2 1.034430 0.725408 0.424364 11.00000 -1.20000 AFIX 0 C15 1 0.873180 0.710250 0.352020 11.00000 0.02943 0.02078 = 0.03236 0.00196 0.00163 0.00995 AFIX 43 H15 2 0.855085 0.741092 0.328553 11.00000 -1.20000 AFIX 0 C16 1 0.792871 0.674503 0.329605 11.00000 0.01892 0.03065 = 0.03613 0.00518 0.00135 0.00826 AFIX 43 H16 2 0.718252 0.680993 0.293171 11.00000 -1.20000 AFIX 0 C17 1 0.821478 0.629355 0.360342 11.00000 0.01698 0.02486 = 0.03845 0.00504 0.00157 0.00145 AFIX 43 H17 2 0.767097 0.604836 0.343227 11.00000 -1.20000 AFIX 0 C18 1 1.103632 0.510584 0.458267 11.00000 0.01677 0.01953 = 0.01329 -0.00091 0.00161 0.00079 C19 1 1.262170 0.455756 0.519966 11.00000 0.01553 0.01729 = 0.01819 0.00338 -0.00153 0.00303 C20 1 1.193544 0.437887 0.621584 11.00000 0.02837 0.03337 = 0.02377 0.01070 0.00659 0.00670 AFIX 137 H20A 2 1.191708 0.461913 0.680703 11.00000 -1.50000 H20B 2 1.233204 0.410010 0.651709 11.00000 -1.50000 H20C 2 1.111278 0.430163 0.598152 11.00000 -1.50000 AFIX 0 C21 1 1.255710 0.423809 0.418056 11.00000 0.02188 0.02088 = 0.02386 -0.00212 -0.00102 0.00412 AFIX 137 H21A 2 1.171555 0.419022 0.396027 11.00000 -1.50000 H21B 2 1.292337 0.393836 0.437546 11.00000 -1.50000 H21C 2 1.299047 0.437840 0.354463 11.00000 -1.50000 AFIX 0 C22 1 1.391518 0.465850 0.552889 11.00000 0.02021 0.02462 = 0.03183 0.00317 -0.00683 0.00109 AFIX 137 H22A 2 1.433269 0.479374 0.487699 11.00000 -1.50000 H22B 2 1.431342 0.436873 0.575598 11.00000 -1.50000 H22C 2 1.393528 0.487824 0.616643 11.00000 -1.50000 AFIX 0 C23 1 0.880207 0.707796 0.788452 11.00000 0.01851 0.01598 = 0.04441 0.00094 0.00381 0.00135 AFIX 43 H23 2 0.899793 0.717511 0.713583 11.00000 -1.20000 AFIX 0 C24 1 0.958128 0.717189 0.877002 11.00000 0.01894 0.01658 = 0.05908 -0.00329 -0.00354 -0.00046 AFIX 43 H24 2 1.031253 0.732988 0.862297 11.00000 -1.20000 AFIX 0 C25 1 0.931516 0.703941 0.987316 11.00000 0.02840 0.01836 = 0.05361 -0.01286 -0.01682 0.00402 AFIX 43 H25 2 0.985524 0.710603 1.048213 11.00000 -1.20000 AFIX 0 C26 1 0.824359 0.680730 1.007238 11.00000 0.03329 0.01869 = 0.03088 -0.00771 -0.00841 0.00499 AFIX 43 H26 2 0.805295 0.671525 1.082617 11.00000 -1.20000 AFIX 0 C27 1 0.744547 0.670724 0.918988 11.00000 0.02127 0.01661 = 0.03122 -0.00332 -0.00255 -0.00033 AFIX 43 H27 2 0.671614 0.654917 0.934457 11.00000 -1.20000 AFIX 0 C28 1 0.771378 0.683880 0.807403 11.00000 0.01536 0.01185 = 0.03168 -0.00192 0.00040 0.00188 C29 1 0.603663 0.639625 0.716427 11.00000 0.01739 0.01415 = 0.01724 0.00160 -0.00063 -0.00086 C30 1 0.653876 0.588980 0.735784 11.00000 0.01366 0.01657 = 0.01504 0.00124 0.00036 0.00032 AFIX 13 H30 2 0.741536 0.589191 0.754882 11.00000 -1.20000 AFIX 0 C31 1 0.630793 0.577855 0.608656 11.00000 0.03499 0.02128 = 0.01606 0.00181 0.00337 0.00200 AFIX 23 H31A 2 0.705183 0.574283 0.564019 11.00000 -1.20000 H31B 2 0.576290 0.551114 0.596167 11.00000 -1.20000 AFIX 0 C32 1 0.569320 0.625416 0.592509 11.00000 0.02454 0.02409 = 0.01482 0.00218 -0.00055 0.00269 AFIX 23 H32A 2 0.481634 0.623192 0.579159 11.00000 -1.20000 H32B 2 0.607421 0.645035 0.533757 11.00000 -1.20000 AFIX 0 C33 1 0.582864 0.560440 0.820099 11.00000 0.01346 0.01658 = 0.01589 0.00161 0.00053 -0.00004 AFIX 13 H33 2 0.610217 0.569203 0.898533 11.00000 -1.20000 AFIX 0 C34 1 0.424085 0.617164 0.830697 11.00000 0.01572 0.01461 = 0.01747 0.00073 -0.00173 0.00170 C35 1 0.496841 0.652707 0.788122 11.00000 0.01479 0.01672 = 0.01498 0.00075 -0.00122 0.00079 C36 1 0.463889 0.698831 0.806197 11.00000 0.02172 0.01575 = 0.02479 0.00279 0.00342 -0.00138 AFIX 43 H36 2 0.513509 0.723078 0.778307 11.00000 -1.20000 AFIX 0 C37 1 0.359945 0.709942 0.864177 11.00000 0.02689 0.01539 = 0.02985 -0.00044 0.00201 0.00507 AFIX 43 H37 2 0.339184 0.741545 0.876857 11.00000 -1.20000 AFIX 0 C38 1 0.286634 0.674711 0.903457 11.00000 0.01908 0.02226 = 0.02816 0.00039 0.00349 0.00471 AFIX 43 H38 2 0.214189 0.682160 0.941410 11.00000 -1.20000 AFIX 0 C39 1 0.318391 0.628664 0.887694 11.00000 0.01686 0.01868 = 0.02416 0.00129 0.00160 -0.00079 AFIX 43 H39 2 0.268063 0.604676 0.915776 11.00000 -1.20000 AFIX 0 C40 1 0.600824 0.508102 0.805998 11.00000 0.01463 0.01922 = 0.01235 0.00181 -0.00094 0.00072 C41 1 0.758157 0.451066 0.756445 11.00000 0.01692 0.01918 = 0.02126 -0.00489 -0.00157 0.00563 C42 1 0.755166 0.423916 0.866380 11.00000 0.02733 0.01993 = 0.02654 -0.00088 -0.00648 0.00862 AFIX 137 H42A 2 0.800170 0.440788 0.925357 11.00000 -1.50000 H42B 2 0.791642 0.393295 0.854761 11.00000 -1.50000 H42C 2 0.671742 0.420039 0.890387 11.00000 -1.50000 AFIX 0 C43 1 0.685744 0.428163 0.661795 11.00000 0.02593 0.03542 = 0.02278 -0.01114 -0.00572 0.00603 AFIX 137 H43A 2 0.604258 0.421869 0.688505 11.00000 -1.50000 H43B 2 0.724213 0.398881 0.640019 11.00000 -1.50000 H43C 2 0.682010 0.448954 0.595756 11.00000 -1.50000 AFIX 0 C44 1 0.885731 0.459767 0.718357 11.00000 0.02013 0.03230 = 0.04040 -0.00889 0.00603 0.00509 AFIX 137 H44A 2 0.884650 0.478291 0.648327 11.00000 -1.50000 H44B 2 0.925521 0.429975 0.704028 11.00000 -1.50000 H44C 2 0.929566 0.476665 0.778071 11.00000 -1.50000 AFIX 0 C45 1 0.516359 0.335553 0.459173 11.00000 0.02195 0.01821 = 0.02935 0.00285 -0.00035 -0.00162 AFIX 43 H45 2 0.590631 0.351745 0.462623 11.00000 -1.20000 AFIX 0 C46 1 0.450686 0.328990 0.557840 11.00000 0.02933 0.02151 = 0.03347 0.00507 0.00471 0.00078 AFIX 43 H46 2 0.480769 0.340827 0.628010 11.00000 -1.20000 AFIX 0 C47 1 0.342198 0.305515 0.555798 11.00000 0.03019 0.02417 = 0.05655 0.00882 0.01228 0.00103 AFIX 43 H47 2 0.297592 0.301322 0.623580 11.00000 -1.20000 AFIX 0 C48 1 0.300037 0.288258 0.452763 11.00000 0.01951 0.01811 = 0.07608 -0.00151 0.00224 -0.00013 AFIX 43 H48 2 0.226243 0.271722 0.450132 11.00000 -1.20000 AFIX 0 C49 1 0.364236 0.294835 0.353519 11.00000 0.02687 0.01641 = 0.05486 -0.00736 -0.00818 0.00522 AFIX 43 H49 2 0.333348 0.283109 0.283545 11.00000 -1.20000 AFIX 0 C50 1 0.474094 0.318552 0.355068 11.00000 0.02293 0.01300 = 0.03617 -0.00196 -0.00485 0.00454 C51 1 0.631368 0.357926 0.240275 11.00000 0.03554 0.01664 = 0.01613 -0.00294 -0.00209 0.00457 C52 1 0.654837 0.367834 0.111180 11.00000 0.07005 0.02602 = 0.01653 -0.00147 0.00015 0.01026 AFIX 23 H52A 2 0.740788 0.366644 0.090688 11.00000 -1.20000 H52B 2 0.606188 0.348226 0.059090 11.00000 -1.20000 AFIX 0 C53 1 0.605985 0.417700 0.124146 11.00000 0.12520 0.02363 = 0.01671 -0.00283 -0.00840 0.01469 AFIX 23 H53A 2 0.666149 0.442079 0.107798 11.00000 -1.20000 H53B 2 0.530767 0.423341 0.080783 11.00000 -1.20000 AFIX 0 C54 1 0.586360 0.409676 0.251318 11.00000 0.02974 0.01499 = 0.01784 0.00011 -0.00445 0.00423 AFIX 13 H54 2 0.499049 0.410795 0.270166 11.00000 -1.20000 AFIX 0 C55 1 0.659088 0.440033 0.331622 11.00000 0.02022 0.01945 = 0.01995 0.00098 0.00000 0.00213 AFIX 13 H55 2 0.632219 0.433733 0.411146 11.00000 -1.20000 AFIX 0 C56 1 0.818492 0.382908 0.345222 11.00000 0.01815 0.02001 = 0.03852 0.00762 0.00881 0.00366 C57 1 0.744458 0.346636 0.306367 11.00000 0.02692 0.02026 = 0.01826 0.00230 0.00830 0.00481 C58 1 0.781050 0.301031 0.324022 11.00000 0.03686 0.01954 = 0.02839 0.00286 0.00379 0.00523 AFIX 43 H58 2 0.730150 0.276328 0.300080 11.00000 -1.20000 AFIX 0 C59 1 0.889891 0.290756 0.375659 11.00000 0.03362 0.02134 = 0.04421 0.00980 0.01099 0.01012 AFIX 43 H59 2 0.914709 0.259364 0.384756 11.00000 -1.20000 AFIX 0 C60 1 0.962172 0.326667 0.413892 11.00000 0.01594 0.03249 = 0.07758 0.02212 0.00417 0.00703 AFIX 43 H60 2 1.036883 0.319862 0.449798 11.00000 -1.20000 AFIX 0 C61 1 0.926656 0.372435 0.400321 11.00000 0.01410 0.02435 = 0.08238 0.01209 0.00124 0.00058 AFIX 43 H61 2 0.976085 0.396827 0.428615 11.00000 -1.20000 AFIX 0 C62 1 0.642272 0.491522 0.307379 11.00000 0.01605 0.01870 = 0.01621 -0.00201 -0.00045 0.00222 C63 1 0.484937 0.546672 0.244187 11.00000 0.01752 0.01490 = 0.01610 0.00235 -0.00218 0.00393 C64 1 0.556218 0.565632 0.145410 11.00000 0.03087 0.03206 = 0.02133 0.00731 0.00565 0.00800 AFIX 137 H64A 2 0.638355 0.572472 0.170871 11.00000 -1.50000 H64B 2 0.518286 0.594192 0.117224 11.00000 -1.50000 H64C 2 0.558169 0.542507 0.084179 11.00000 -1.50000 AFIX 0 C65 1 0.490243 0.577426 0.348867 11.00000 0.01793 0.01960 = 0.02096 -0.00202 -0.00031 0.00545 AFIX 137 H65A 2 0.446769 0.562476 0.411113 11.00000 -1.50000 H65B 2 0.453207 0.607535 0.331466 11.00000 -1.50000 H65C 2 0.574183 0.582155 0.371721 11.00000 -1.50000 AFIX 0 C66 1 0.356038 0.536994 0.208695 11.00000 0.02233 0.02429 = 0.03308 -0.00157 -0.00993 0.00272 AFIX 137 H66A 2 0.355081 0.516725 0.141626 11.00000 -1.50000 H66B 2 0.315717 0.566361 0.190244 11.00000 -1.50000 H66C 2 0.314063 0.521644 0.271293 11.00000 -1.50000 PART 1 AFIX 66 C67A 1 -0.031862 0.319949 0.959383 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 C68A 1 0.001892 0.329604 0.848226 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 AFIX 43 H68A 2 0.075025 0.345488 0.834090 21.00000 -1.20000 AFIX 65 C69A 1 -0.071357 0.316017 0.757752 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 AFIX 43 H69A 2 -0.048287 0.322616 0.681781 21.00000 -1.20000 AFIX 65 C70A 1 -0.178362 0.292776 0.778435 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 AFIX 43 H70A 2 -0.228424 0.283490 0.716600 21.00000 -1.20000 AFIX 65 C71A 1 -0.212117 0.283121 0.889592 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 AFIX 43 H71A 2 -0.285250 0.267236 0.903727 21.00000 -1.20000 AFIX 65 C72A 1 -0.138869 0.296707 0.980067 21.00000 0.02123 0.01824 = 0.04822 -0.00961 -0.00949 0.00205 AFIX 43 H72A 2 -0.161939 0.290108 1.056038 21.00000 -1.20000 PART 0 AFIX 0 C73 1 0.128239 0.363472 1.047991 11.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 PART 1 C74A 1 0.170955 0.379935 1.174702 21.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 AFIX 23 H74A 2 0.123846 0.365477 1.236383 21.00000 -1.20000 H74B 2 0.258026 0.375691 1.188756 21.00000 -1.20000 AFIX 0 C75A 1 0.140746 0.423684 1.154628 21.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 AFIX 23 H75A 2 0.210930 0.444800 1.155113 21.00000 -1.20000 H75B 2 0.079153 0.435223 1.207888 21.00000 -1.20000 PART 0 AFIX 0 C76 1 0.088568 0.415212 1.030434 11.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 AFIX 13 H76 2 -0.000552 0.419043 1.025593 11.00000 -1.20000 AFIX 0 C77 1 0.154764 0.441878 0.938313 11.00000 0.02019 0.01689 = 0.02052 -0.00025 0.00173 0.00085 AFIX 13 H77 2 0.120334 0.432599 0.862744 11.00000 -1.20000 AFIX 0 C78 1 0.313068 0.383358 0.934095 11.00000 0.01829 0.01600 = 0.01685 -0.00117 -0.00179 -0.00037 C79 1 0.240641 0.349671 0.986338 11.00000 0.01646 0.01535 = 0.01714 -0.00002 -0.00253 0.00010 C80 1 0.278838 0.303588 0.986900 11.00000 0.02290 0.01699 = 0.03816 0.00448 0.00448 0.00038 AFIX 43 H80 2 0.231203 0.280615 1.023040 11.00000 -1.20000 AFIX 0 C81 1 0.384967 0.290755 0.935699 11.00000 0.02824 0.01732 = 0.05581 0.00119 0.00948 0.00863 AFIX 43 H81 2 0.409988 0.259182 0.936980 11.00000 -1.20000 AFIX 0 C82 1 0.454922 0.324016 0.882436 11.00000 0.01967 0.02603 = 0.04363 -0.00085 0.00707 0.00785 AFIX 43 H82 2 0.527571 0.315191 0.846631 11.00000 -1.20000 AFIX 0 C83 1 0.418904 0.370088 0.881429 11.00000 0.01703 0.02128 = 0.03035 0.00266 0.00375 0.00111 AFIX 43 H83 2 0.466819 0.392765 0.844519 11.00000 -1.20000 AFIX 0 C84 1 0.140813 0.494248 0.950948 11.00000 0.01558 0.01722 = 0.01579 0.00173 0.00089 0.00096 C85 1 -0.013743 0.552750 0.999305 11.00000 0.01602 0.01234 = 0.02011 -0.00103 0.00209 0.00366 C86 1 -0.141859 0.545464 1.037336 11.00000 0.01847 0.02232 = 0.03632 0.00164 0.00502 0.00135 AFIX 137 H86A 2 -0.186526 0.528570 0.978167 11.00000 -1.50000 H86B 2 -0.179892 0.575699 1.050374 11.00000 -1.50000 H86C 2 -0.142091 0.527405 1.108086 11.00000 -1.50000 AFIX 0 C87 1 0.059738 0.576335 1.091954 11.00000 0.02277 0.02794 = 0.01917 -0.00438 -0.00108 0.00439 AFIX 137 H87A 2 0.062428 0.556431 1.159647 11.00000 -1.50000 H87B 2 0.022765 0.606190 1.111320 11.00000 -1.50000 H87C 2 0.141523 0.581632 1.064785 11.00000 -1.50000 AFIX 0 C88 1 -0.009601 0.578488 0.886562 11.00000 0.01979 0.01853 = 0.02127 0.00021 -0.00273 0.00171 AFIX 137 H88A 2 0.073981 0.581538 0.862344 11.00000 -1.50000 H88B 2 -0.044903 0.609463 0.895604 11.00000 -1.50000 H88C 2 -0.055208 0.561076 0.828962 11.00000 -1.50000 AFIX 0 N1 3 1.213360 0.679873 0.501711 11.00000 0.03328 0.01797 = 0.03109 -0.00864 -0.01414 0.00137 N2 3 0.959653 0.573775 0.448414 11.00000 0.01526 0.01971 = 0.03313 0.00549 0.00246 0.00331 N3 3 0.695440 0.675537 0.715515 11.00000 0.01790 0.01945 = 0.02040 0.00416 0.00348 -0.00372 N4 3 0.455011 0.570653 0.810595 11.00000 0.01374 0.01333 = 0.02672 0.00122 0.00370 0.00019 N5 3 0.538775 0.322998 0.253860 11.00000 0.03610 0.01931 = 0.02330 -0.00584 -0.01091 -0.00008 N6 3 0.785346 0.429188 0.324601 11.00000 0.01796 0.01665 = 0.06450 0.00427 -0.00322 0.00219 PART 2 N7B 3 0.026136 0.329264 1.016836 -21.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 AFIX 43 H7B 2 -0.002523 0.312620 1.073274 -21.00000 -1.20000 PART 0 AFIX 0 N8 3 0.280673 0.430358 0.939421 11.00000 0.01955 0.01514 = 0.03820 0.00689 0.01252 0.00092 O1 4 1.024619 0.482033 0.450512 11.00000 0.01656 0.02073 = 0.04164 0.00429 -0.00295 -0.00081 O2 4 1.217581 0.502624 0.487236 11.00000 0.01481 0.01666 = 0.01821 0.00014 -0.00085 0.00176 O3 4 0.523355 0.479833 0.823499 11.00000 0.01769 0.01706 = 0.03093 0.00264 0.00463 0.00072 O4 4 0.713626 0.499104 0.776069 11.00000 0.01544 0.01713 = 0.02158 0.00011 0.00249 0.00321 O5 4 0.720188 0.520118 0.319391 11.00000 0.01692 0.01900 = 0.04225 0.00068 -0.00375 0.00021 O6 4 0.529318 0.499490 0.274411 11.00000 0.01729 0.01521 = 0.02214 0.00018 -0.00338 0.00217 O7 4 0.219192 0.521774 0.930376 11.00000 0.01721 0.01633 = 0.03199 0.00345 0.00499 -0.00073 O8 4 0.029318 0.504188 0.982707 11.00000 0.01678 0.01496 = 0.02567 0.00282 0.00298 0.00056 PART 2 AFIX 66 C70B 1 -0.137437 0.306586 0.700598 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 AFIX 43 H70B 2 -0.175488 0.301466 0.628980 -21.00000 -1.20000 AFIX 65 C72B 1 -0.188374 0.289055 0.799294 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 AFIX 43 H72B 2 -0.261237 0.271952 0.795131 -21.00000 -1.20000 AFIX 65 C71B 1 -0.132700 0.296546 0.904082 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 AFIX 43 H71B 2 -0.167513 0.284564 0.971536 -21.00000 -1.20000 AFIX 65 C67B 1 -0.026089 0.321569 0.910174 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 C69B 1 0.024849 0.339101 0.811479 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 AFIX 43 H69B 2 0.097713 0.356203 0.815644 -21.00000 -1.20000 AFIX 65 C68B 1 -0.030824 0.331610 0.706691 -21.00000 0.02100 0.01619 = 0.05614 -0.01009 -0.00854 0.00090 AFIX 43 H68B 2 0.003990 0.343593 0.639237 -21.00000 -1.20000 PART 1 AFIX 0 N7A 3 0.040731 0.329868 1.055457 21.00000 0.02066 0.01529 = 0.01919 0.00288 0.00498 0.00077 AFIX 43 H7A 2 0.030115 0.314682 1.119624 21.00000 -1.20000 PART 2 AFIX 0 C74B 1 0.132799 0.370420 1.174874 -21.00000 0.03467 0.01810 = 0.01903 0.00756 0.00655 0.00308 AFIX 23 H74C 2 0.211600 0.362882 1.209877 -21.00000 -1.20000 H74D 2 0.066721 0.354902 1.215934 -21.00000 -1.20000 AFIX 0 C75B 1 0.110320 0.428389 1.153391 -21.00000 0.03601 0.02570 = 0.01951 0.00022 0.00164 0.01595 AFIX 23 H75C 2 0.039211 0.441232 1.192365 -21.00000 -1.20000 H75D 2 0.182346 0.447898 1.166499 -21.00000 -1.20000 AFIX 0 PART 0 H400 2 0.410188 0.550072 0.847443 11.00000 0.01940 H600 2 0.828812 0.448549 0.355511 11.00000 0.03930 H100 2 1.251622 0.688179 0.562896 11.00000 0.03603 H500 2 0.493780 0.318489 0.190337 11.00000 0.03632 H200 2 0.909538 0.550555 0.416695 11.00000 0.03631 H300 2 0.731366 0.676790 0.645472 11.00000 0.03559 H800 2 0.324259 0.448443 0.899855 11.00000 0.02591 HKLF 4 REM cu_v1075_GuillotICMMO.res in P2(1) REM wR2 = 0.0817, GooF = S = 1.025, Restrained GooF = 1.025 for all data REM R1 = 0.0324 for 12154 Fo > 4sig(Fo) and 0.0343 for all 12738 data REM 945 parameters refined using 1 restraints END WGHT 0.0448 0.7719 REM Highest difference peak 0.220, deepest hole -0.204, 1-sigma level 0.039 Q1 1 0.0199 0.4141 1.1530 11.00000 0.05 0.19 Q2 1 -0.1463 0.2899 0.8613 11.00000 0.05 0.14 Q3 1 0.1999 0.4434 1.0176 11.00000 0.05 0.14 Q4 1 0.2099 0.2685 0.3774 11.00000 0.05 0.13 Q5 1 0.5992 0.4420 0.0783 11.00000 0.05 0.13 Q6 1 1.0637 0.6497 0.4779 11.00000 0.05 0.13 Q7 1 0.6679 0.3449 0.0616 11.00000 0.05 0.12 Q8 1 0.1893 0.3575 1.0196 11.00000 0.05 0.12 Q9 1 0.1174 0.4604 1.2067 11.00000 0.05 0.12 Q10 1 0.2834 0.3675 0.9878 11.00000 0.05 0.12 Q11 1 -0.0220 0.3330 1.1155 11.00000 0.05 0.12 Q12 1 0.1006 0.4193 0.7746 11.00000 0.05 0.12 Q13 1 0.4532 0.4228 0.1155 11.00000 0.05 0.12 Q14 1 0.9294 0.3510 0.4399 11.00000 0.05 0.12 Q15 1 0.6516 0.5784 0.6727 11.00000 0.05 0.12 Q16 1 -0.3301 0.5011 0.9978 11.00000 0.05 0.12 Q17 1 0.6436 0.5825 0.1549 11.00000 0.05 0.11 Q18 1 0.0495 0.5097 1.0528 11.00000 0.05 0.11 Q19 1 0.1303 0.3984 1.1833 11.00000 0.05 0.11 Q20 1 -0.0457 0.3298 1.0848 11.00000 0.05 0.11 ; _shelx_res_checksum 58140 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3887(3) 0.71051(9) 0.4068(3) 0.0378(7) Uani 1 1 d . . . . . H1 H 1.414563 0.724760 0.475793 0.045 Uiso 1 1 calc R U . . . C2 C 1.4563(3) 0.71559(10) 0.3093(4) 0.0448(9) Uani 1 1 d . . . . . H2 H 1.528030 0.733443 0.312237 0.054 Uiso 1 1 calc R U . . . C3 C 1.4216(3) 0.69530(10) 0.2082(3) 0.0398(7) Uani 1 1 d . . . . . H3 H 1.469529 0.698617 0.142206 0.048 Uiso 1 1 calc R U . . . C4 C 1.3166(2) 0.67009(9) 0.2040(3) 0.0297(6) Uani 1 1 d . . . . . H4 H 1.291567 0.656274 0.134256 0.036 Uiso 1 1 calc R U . . . C5 C 1.2468(2) 0.66464(8) 0.3004(2) 0.0230(5) Uani 1 1 d . . . . . H5 H 1.174397 0.647290 0.295585 0.028 Uiso 1 1 calc R U . . . C6 C 1.2814(2) 0.68425(8) 0.4045(2) 0.0245(6) Uani 1 1 d . . . . . C7 C 1.1199(2) 0.64478(8) 0.5138(2) 0.0212(5) Uani 1 1 d . . . . . C8 C 1.0934(3) 0.63519(10) 0.6417(2) 0.0332(7) Uani 1 1 d . . . . . H8A H 1.135085 0.656850 0.694336 0.040 Uiso 1 1 calc R U . . . H8B H 1.006707 0.633559 0.658940 0.040 Uiso 1 1 calc R U . . . C9 C 1.1541(3) 0.58711(10) 0.6338(2) 0.0314(6) Uani 1 1 d . . . . . H9A H 1.101125 0.561012 0.655573 0.038 Uiso 1 1 calc R U . . . H9B H 1.232106 0.585279 0.674576 0.038 Uiso 1 1 calc R U . . . C10 C 1.1662(2) 0.59337(8) 0.50343(19) 0.0183(5) Uani 1 1 d . . . . . H10 H 1.251759 0.592007 0.478733 0.022 Uiso 1 1 calc R U . . . C11 C 1.0860(2) 0.56204(8) 0.43184(19) 0.0162(5) Uani 1 1 d . . . . . H11 H 1.105591 0.567232 0.349902 0.019 Uiso 1 1 calc R U . . . C12 C 0.9294(2) 0.61961(9) 0.4162(2) 0.0209(5) Uani 1 1 d . . . . . C13 C 1.0088(2) 0.65586(8) 0.4434(2) 0.0201(5) Uani 1 1 d . . . . . C14 C 0.9799(2) 0.70077(9) 0.4088(2) 0.0252(5) Uani 1 1 d . . . . . H14 H 1.034430 0.725408 0.424364 0.030 Uiso 1 1 calc R U . . . C15 C 0.8732(2) 0.71025(9) 0.3520(2) 0.0275(6) Uani 1 1 d . . . . . H15 H 0.855085 0.741092 0.328553 0.033 Uiso 1 1 calc R U . . . C16 C 0.7929(2) 0.67450(10) 0.3296(2) 0.0286(6) Uani 1 1 d . . . . . H16 H 0.718252 0.680993 0.293171 0.034 Uiso 1 1 calc R U . . . C17 C 0.8215(2) 0.62935(10) 0.3603(2) 0.0268(6) Uani 1 1 d . . . . . H17 H 0.767097 0.604836 0.343227 0.032 Uiso 1 1 calc R U . . . C18 C 1.1036(2) 0.51058(8) 0.45827(18) 0.0165(5) Uani 1 1 d . . . . . C19 C 1.2622(2) 0.45576(8) 0.5200(2) 0.0170(5) Uani 1 1 d . . . . . C20 C 1.1935(2) 0.43789(10) 0.6216(2) 0.0285(6) Uani 1 1 d . . . . . H20A H 1.191708 0.461913 0.680703 0.043 Uiso 1 1 calc R U . . . H20B H 1.233204 0.410010 0.651709 0.043 Uiso 1 1 calc R U . . . H20C H 1.111278 0.430163 0.598152 0.043 Uiso 1 1 calc R U . . . C21 C 1.2557(2) 0.42381(9) 0.4181(2) 0.0222(5) Uani 1 1 d . . . . . H21A H 1.171555 0.419022 0.396027 0.033 Uiso 1 1 calc R U . . . H21B H 1.292337 0.393836 0.437546 0.033 Uiso 1 1 calc R U . . . H21C H 1.299047 0.437840 0.354463 0.033 Uiso 1 1 calc R U . . . C22 C 1.3915(2) 0.46585(9) 0.5529(2) 0.0256(5) Uani 1 1 d . . . . . H22A H 1.433269 0.479374 0.487699 0.038 Uiso 1 1 calc R U . . . H22B H 1.431342 0.436873 0.575598 0.038 Uiso 1 1 calc R U . . . H22C H 1.393528 0.487824 0.616643 0.038 Uiso 1 1 calc R U . . . C23 C 0.8802(2) 0.70780(8) 0.7885(2) 0.0263(5) Uani 1 1 d . . . . . H23 H 0.899793 0.717511 0.713583 0.032 Uiso 1 1 calc R U . . . C24 C 0.9581(2) 0.71719(9) 0.8770(3) 0.0316(6) Uani 1 1 d . . . . . H24 H 1.031253 0.732988 0.862297 0.038 Uiso 1 1 calc R U . . . C25 C 0.9315(2) 0.70394(9) 0.9873(3) 0.0336(6) Uani 1 1 d . . . . . H25 H 0.985524 0.710603 1.048213 0.040 Uiso 1 1 calc R U . . . C26 C 0.8244(2) 0.68073(9) 1.0072(2) 0.0277(6) Uani 1 1 d . . . . . H26 H 0.805295 0.671525 1.082617 0.033 Uiso 1 1 calc R U . . . C27 C 0.7445(2) 0.67072(8) 0.9190(2) 0.0231(5) Uani 1 1 d . . . . . H27 H 0.671614 0.654917 0.934457 0.028 Uiso 1 1 calc R U . . . C28 C 0.7714(2) 0.68388(8) 0.8074(2) 0.0196(5) Uani 1 1 d . . . . . C29 C 0.6037(2) 0.63963(8) 0.71643(19) 0.0163(5) Uani 1 1 d . . . . . C30 C 0.6539(2) 0.58898(8) 0.73578(19) 0.0151(4) Uani 1 1 d . . . . . H30 H 0.741536 0.589191 0.754882 0.018 Uiso 1 1 calc R U . . . C31 C 0.6308(2) 0.57786(9) 0.6087(2) 0.0241(5) Uani 1 1 d . . . . . H31A H 0.705183 0.574283 0.564019 0.029 Uiso 1 1 calc R U . . . H31B H 0.576290 0.551114 0.596167 0.029 Uiso 1 1 calc R U . . . C32 C 0.5693(2) 0.62542(8) 0.59251(19) 0.0212(5) Uani 1 1 d . . . . . H32A H 0.481634 0.623192 0.579159 0.025 Uiso 1 1 calc R U . . . H32B H 0.607421 0.645035 0.533757 0.025 Uiso 1 1 calc R U . . . C33 C 0.5829(2) 0.56044(8) 0.82010(19) 0.0153(5) Uani 1 1 d . . . . . H33 H 0.610217 0.569203 0.898533 0.018 Uiso 1 1 calc R U . . . C34 C 0.4241(2) 0.61716(8) 0.83070(19) 0.0159(5) Uani 1 1 d . . . . . C35 C 0.4968(2) 0.65271(8) 0.78812(19) 0.0155(4) Uani 1 1 d . . . . . C36 C 0.4639(2) 0.69883(8) 0.8062(2) 0.0207(5) Uani 1 1 d . . . . . H36 H 0.513509 0.723078 0.778307 0.025 Uiso 1 1 calc R U . . . C37 C 0.3599(2) 0.70994(9) 0.8642(2) 0.0240(5) Uani 1 1 d . . . . . H37 H 0.339184 0.741545 0.876857 0.029 Uiso 1 1 calc R U . . . C38 C 0.2866(2) 0.67471(9) 0.9035(2) 0.0231(5) Uani 1 1 d . . . . . H38 H 0.214189 0.682160 0.941410 0.028 Uiso 1 1 calc R U . . . C39 C 0.3184(2) 0.62866(9) 0.8877(2) 0.0199(5) Uani 1 1 d . . . . . H39 H 0.268063 0.604676 0.915776 0.024 Uiso 1 1 calc R U . . . C40 C 0.60082(19) 0.50810(8) 0.80600(18) 0.0154(5) Uani 1 1 d . . . . . C41 C 0.7582(2) 0.45107(8) 0.7564(2) 0.0191(5) Uani 1 1 d . . . . . C42 C 0.7552(2) 0.42392(9) 0.8664(2) 0.0246(6) Uani 1 1 d . . . . . H42A H 0.800170 0.440788 0.925357 0.037 Uiso 1 1 calc R U . . . H42B H 0.791642 0.393295 0.854761 0.037 Uiso 1 1 calc R U . . . H42C H 0.671742 0.420039 0.890387 0.037 Uiso 1 1 calc R U . . . C43 C 0.6857(2) 0.42816(10) 0.6618(2) 0.0281(6) Uani 1 1 d . . . . . H43A H 0.604258 0.421869 0.688505 0.042 Uiso 1 1 calc R U . . . H43B H 0.724213 0.398881 0.640019 0.042 Uiso 1 1 calc R U . . . H43C H 0.682010 0.448954 0.595756 0.042 Uiso 1 1 calc R U . . . C44 C 0.8857(2) 0.45977(10) 0.7184(3) 0.0309(6) Uani 1 1 d . . . . . H44A H 0.884650 0.478291 0.648327 0.046 Uiso 1 1 calc R U . . . H44B H 0.925521 0.429975 0.704028 0.046 Uiso 1 1 calc R U . . . H44C H 0.929566 0.476665 0.778071 0.046 Uiso 1 1 calc R U . . . C45 C 0.5164(2) 0.33555(9) 0.4592(2) 0.0232(5) Uani 1 1 d . . . . . H45 H 0.590631 0.351745 0.462623 0.028 Uiso 1 1 calc R U . . . C46 C 0.4507(2) 0.32899(9) 0.5578(2) 0.0281(6) Uani 1 1 d . . . . . H46 H 0.480769 0.340827 0.628010 0.034 Uiso 1 1 calc R U . . . C47 C 0.3422(3) 0.30551(10) 0.5558(3) 0.0369(7) Uani 1 1 d . . . . . H47 H 0.297592 0.301322 0.623580 0.044 Uiso 1 1 calc R U . . . C48 C 0.3000(2) 0.28826(10) 0.4528(3) 0.0379(7) Uani 1 1 d . . . . . H48 H 0.226243 0.271722 0.450132 0.045 Uiso 1 1 calc R U . . . C49 C 0.3642(2) 0.29483(9) 0.3535(3) 0.0328(6) Uani 1 1 d . . . . . H49 H 0.333348 0.283109 0.283545 0.039 Uiso 1 1 calc R U . . . C50 C 0.4741(2) 0.31855(8) 0.3551(2) 0.0241(5) Uani 1 1 d . . . . . C51 C 0.6314(2) 0.35793(8) 0.2403(2) 0.0228(5) Uani 1 1 d . . . . . C52 C 0.6548(3) 0.36783(10) 0.1112(2) 0.0375(7) Uani 1 1 d . . . . . H52A H 0.740788 0.366644 0.090688 0.045 Uiso 1 1 calc R U . . . H52B H 0.606188 0.348226 0.059090 0.045 Uiso 1 1 calc R U . . . C53 C 0.6060(4) 0.41770(11) 0.1241(2) 0.0552(11) Uani 1 1 d . . . . . H53A H 0.666149 0.442079 0.107798 0.066 Uiso 1 1 calc R U . . . H53B H 0.530767 0.423341 0.080783 0.066 Uiso 1 1 calc R U . . . C54 C 0.5864(2) 0.40968(8) 0.25132(19) 0.0209(5) Uani 1 1 d . . . . . H54 H 0.499049 0.410795 0.270166 0.025 Uiso 1 1 calc R U . . . C55 C 0.6591(2) 0.44003(8) 0.3316(2) 0.0199(5) Uani 1 1 d . . . . . H55 H 0.632219 0.433733 0.411146 0.024 Uiso 1 1 calc R U . . . C56 C 0.8185(2) 0.38291(9) 0.3452(2) 0.0255(6) Uani 1 1 d . . . . . C57 C 0.7445(2) 0.34664(8) 0.3064(2) 0.0218(5) Uani 1 1 d . . . . . C58 C 0.7810(3) 0.30103(9) 0.3240(2) 0.0282(6) Uani 1 1 d . . . . . H58 H 0.730150 0.276328 0.300080 0.034 Uiso 1 1 calc R U . . . C59 C 0.8899(3) 0.29076(10) 0.3757(3) 0.0330(7) Uani 1 1 d . . . . . H59 H 0.914709 0.259364 0.384756 0.040 Uiso 1 1 calc R U . . . C60 C 0.9622(2) 0.32667(11) 0.4139(3) 0.0420(8) Uani 1 1 d . . . . . H60 H 1.036883 0.319862 0.449798 0.050 Uiso 1 1 calc R U . . . C61 C 0.9267(2) 0.37243(11) 0.4003(3) 0.0403(8) Uani 1 1 d . . . . . H61 H 0.976085 0.396827 0.428615 0.048 Uiso 1 1 calc R U . . . C62 C 0.6423(2) 0.49152(8) 0.30738(19) 0.0170(5) Uani 1 1 d . . . . . C63 C 0.4849(2) 0.54667(8) 0.24419(19) 0.0162(5) Uani 1 1 d . . . . . C64 C 0.5562(2) 0.56563(10) 0.1454(2) 0.0281(6) Uani 1 1 d . . . . . H64A H 0.638355 0.572472 0.170871 0.042 Uiso 1 1 calc R U . . . H64B H 0.518286 0.594192 0.117224 0.042 Uiso 1 1 calc R U . . . H64C H 0.558169 0.542507 0.084179 0.042 Uiso 1 1 calc R U . . . C65 C 0.4902(2) 0.57743(9) 0.3489(2) 0.0195(5) Uani 1 1 d . . . . . H65A H 0.446769 0.562476 0.411113 0.029 Uiso 1 1 calc R U . . . H65B H 0.453207 0.607535 0.331466 0.029 Uiso 1 1 calc R U . . . H65C H 0.574183 0.582155 0.371721 0.029 Uiso 1 1 calc R U . . . C66 C 0.3560(2) 0.53699(9) 0.2087(2) 0.0266(6) Uani 1 1 d . . . . . H66A H 0.355081 0.516725 0.141626 0.040 Uiso 1 1 calc R U . . . H66B H 0.315717 0.566361 0.190244 0.040 Uiso 1 1 calc R U . . . H66C H 0.314063 0.521644 0.271293 0.040 Uiso 1 1 calc R U . . . C67A C -0.0319(3) 0.31995(15) 0.9594(3) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 C68A C 0.0019(3) 0.32960(14) 0.8482(3) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 H68A H 0.075025 0.345488 0.834090 0.035 Uiso 0.485(5) 1 calc R U P A 1 C69A C -0.0714(3) 0.31602(13) 0.7578(2) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 H69A H -0.048287 0.322616 0.681781 0.035 Uiso 0.485(5) 1 calc R U P A 1 C70A C -0.1784(3) 0.29278(14) 0.7784(3) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 H70A H -0.228424 0.283490 0.716600 0.035 Uiso 0.485(5) 1 calc R U P A 1 C71A C -0.2121(3) 0.28312(13) 0.8896(3) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 H71A H -0.285250 0.267236 0.903727 0.035 Uiso 0.485(5) 1 calc R U P A 1 C72A C -0.1389(3) 0.29671(13) 0.9801(3) 0.0293(8) Uani 0.485(5) 1 d G . P A 1 H72A H -0.161939 0.290108 1.056038 0.035 Uiso 0.485(5) 1 calc R U P A 1 C73 C 0.1282(2) 0.36347(8) 1.0480(2) 0.0183(3) Uani 1 1 d . . . . . C74A C 0.1710(6) 0.3799(3) 1.1747(6) 0.0183(3) Uani 0.485(5) 1 d . . P A 1 H74A H 0.123846 0.365477 1.236383 0.022 Uiso 0.485(5) 1 calc R U P A 1 H74B H 0.258026 0.375691 1.188756 0.022 Uiso 0.485(5) 1 calc R U P A 1 C75A C 0.1407(8) 0.4237(4) 1.1546(9) 0.0183(3) Uani 0.485(5) 1 d . . P A 1 H75A H 0.210930 0.444800 1.155113 0.022 Uiso 0.485(5) 1 calc R U P A 1 H75B H 0.079153 0.435223 1.207888 0.022 Uiso 0.485(5) 1 calc R U P A 1 C76 C 0.0886(2) 0.41521(8) 1.0304(2) 0.0183(3) Uani 1 1 d . . . . . H76 H -0.000552 0.419043 1.025593 0.022 Uiso 1 1 calc R U . A 1 C77 C 0.1548(2) 0.44188(8) 0.9383(2) 0.0192(5) Uani 1 1 d . . . . . H77 H 0.120334 0.432599 0.862744 0.023 Uiso 1 1 calc R U . . . C78 C 0.3131(2) 0.38336(8) 0.93410(19) 0.0171(5) Uani 1 1 d . . . . . C79 C 0.2406(2) 0.34967(8) 0.98634(19) 0.0163(5) Uani 1 1 d . . . . . C80 C 0.2788(2) 0.30359(9) 0.9869(2) 0.0260(6) Uani 1 1 d . . . . . H80 H 0.231203 0.280615 1.023040 0.031 Uiso 1 1 calc R U . . . C81 C 0.3850(3) 0.29076(10) 0.9357(3) 0.0337(6) Uani 1 1 d . . . . . H81 H 0.409988 0.259182 0.936980 0.040 Uiso 1 1 calc R U . . . C82 C 0.4549(2) 0.32402(10) 0.8824(3) 0.0297(6) Uani 1 1 d . . . . . H82 H 0.527571 0.315191 0.846631 0.036 Uiso 1 1 calc R U . . . C83 C 0.4189(2) 0.37009(9) 0.8814(2) 0.0229(6) Uani 1 1 d . . . . . H83 H 0.466819 0.392765 0.844519 0.027 Uiso 1 1 calc R U . . . C84 C 0.1408(2) 0.49425(8) 0.95095(19) 0.0162(5) Uani 1 1 d . . . . . C85 C -0.0137(2) 0.55275(8) 0.9993(2) 0.0161(5) Uani 1 1 d . . . . . C86 C -0.1419(2) 0.54546(9) 1.0373(2) 0.0257(5) Uani 1 1 d . . . . . H86A H -0.186526 0.528570 0.978167 0.039 Uiso 1 1 calc R U . . . H86B H -0.179892 0.575699 1.050374 0.039 Uiso 1 1 calc R U . . . H86C H -0.142091 0.527405 1.108086 0.039 Uiso 1 1 calc R U . . . C87 C 0.0597(2) 0.57634(9) 1.0920(2) 0.0233(5) Uani 1 1 d . . . . . H87A H 0.062428 0.556431 1.159647 0.035 Uiso 1 1 calc R U . . . H87B H 0.022765 0.606190 1.111320 0.035 Uiso 1 1 calc R U . . . H87C H 0.141523 0.581632 1.064785 0.035 Uiso 1 1 calc R U . . . C88 C -0.0096(2) 0.57849(8) 0.8866(2) 0.0199(5) Uani 1 1 d . . . . . H88A H 0.073981 0.581538 0.862344 0.030 Uiso 1 1 calc R U . . . H88B H -0.044903 0.609463 0.895604 0.030 Uiso 1 1 calc R U . . . H88C H -0.055208 0.561076 0.828962 0.030 Uiso 1 1 calc R U . . . N1 N 1.2134(2) 0.67987(7) 0.5017(2) 0.0275(5) Uani 1 1 d . . . . . N2 N 0.95965(18) 0.57378(7) 0.44841(19) 0.0227(4) Uani 1 1 d . . . . . N3 N 0.69544(17) 0.67554(7) 0.71551(18) 0.0192(4) Uani 1 1 d . . . . . N4 N 0.45501(17) 0.57065(7) 0.81060(18) 0.0179(4) Uani 1 1 d . . . . . N5 N 0.5388(2) 0.32300(7) 0.25386(18) 0.0263(5) Uani 1 1 d . . . . . N6 N 0.7853(2) 0.42919(8) 0.3246(2) 0.0331(6) Uani 1 1 d . . . . . N7B N 0.0261(4) 0.32926(16) 1.0168(4) 0.0183(3) Uani 0.515(5) 1 d . . P A 2 H7B H -0.002523 0.312620 1.073274 0.022 Uiso 0.515(5) 1 calc R U P A 2 N8 N 0.28067(19) 0.43036(7) 0.9394(2) 0.0242(5) Uani 1 1 d . . . . . O1 O 1.02462(15) 0.48203(6) 0.45051(16) 0.0263(4) Uani 1 1 d . . . . . O2 O 1.21758(14) 0.50262(5) 0.48724(13) 0.0166(3) Uani 1 1 d . . . . . O3 O 0.52335(15) 0.47983(6) 0.82350(15) 0.0219(4) Uani 1 1 d . . . . . O4 O 0.71363(14) 0.49910(5) 0.77607(13) 0.0180(3) Uani 1 1 d . . . . . O5 O 0.72019(15) 0.52012(6) 0.31939(16) 0.0261(4) Uani 1 1 d . . . . . O6 O 0.52932(14) 0.49949(5) 0.27441(13) 0.0182(3) Uani 1 1 d . . . . . O7 O 0.21919(14) 0.52177(6) 0.93038(14) 0.0218(4) Uani 1 1 d . . . . . O8 O 0.02932(14) 0.50419(5) 0.98271(14) 0.0191(3) Uani 1 1 d . . . . . C70B C -0.1374(3) 0.30659(12) 0.7006(3) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 H70B H -0.175488 0.301466 0.628980 0.037 Uiso 0.515(5) 1 calc R U P A 2 C72B C -0.1884(2) 0.28905(12) 0.7993(3) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 H72B H -0.261237 0.271952 0.795131 0.037 Uiso 0.515(5) 1 calc R U P A 2 C71B C -0.1327(3) 0.29655(12) 0.9041(3) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 H71B H -0.167513 0.284564 0.971536 0.037 Uiso 0.515(5) 1 calc R U P A 2 C67B C -0.0261(3) 0.32157(13) 0.9102(2) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 C69B C 0.0248(3) 0.33910(13) 0.8115(3) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 H69B H 0.097713 0.356203 0.815644 0.037 Uiso 0.515(5) 1 calc R U P A 2 C68B C -0.0308(3) 0.33161(12) 0.7067(3) 0.0312(8) Uani 0.515(5) 1 d G . P A 2 H68B H 0.003990 0.343593 0.639237 0.037 Uiso 0.515(5) 1 calc R U P A 2 N7A N 0.0407(4) 0.32987(17) 1.0555(5) 0.0183(3) Uani 0.485(5) 1 d . . P A 1 H7A H 0.030115 0.314682 1.119624 0.022 Uiso 0.485(5) 1 calc R U P A 1 C74B C 0.1328(6) 0.3704(2) 1.1749(5) 0.0239(14) Uani 0.515(5) 1 d . . P A 2 H74C H 0.211600 0.362882 1.209877 0.029 Uiso 0.515(5) 1 calc R U P A 2 H74D H 0.066721 0.354902 1.215934 0.029 Uiso 0.515(5) 1 calc R U P A 2 C75B C 0.1103(7) 0.4284(3) 1.1534(7) 0.0271(17) Uani 0.515(5) 1 d . . P A 2 H75C H 0.039211 0.441232 1.192365 0.032 Uiso 0.515(5) 1 calc R U P A 2 H75D H 0.182346 0.447898 1.166499 0.032 Uiso 0.515(5) 1 calc R U P A 2 H400 H 0.410(2) 0.5501(11) 0.847(2) 0.019(7) Uiso 1 1 d . . . . . H600 H 0.829(3) 0.4485(14) 0.356(3) 0.039(10) Uiso 1 1 d . . . . . H100 H 1.252(3) 0.6882(12) 0.563(3) 0.036(9) Uiso 1 1 d . . . . . H500 H 0.494(3) 0.3185(11) 0.190(3) 0.036(9) Uiso 1 1 d . . . . . H200 H 0.910(3) 0.5506(12) 0.417(3) 0.036(9) Uiso 1 1 d . . . . . H300 H 0.731(3) 0.6768(11) 0.645(3) 0.036(8) Uiso 1 1 d . . . . . H800 H 0.324(3) 0.4484(11) 0.900(3) 0.026(8) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0267(14) 0.0135(13) 0.073(2) -0.0050(13) -0.0214(15) 0.0008(11) C2 0.0177(14) 0.0167(13) 0.100(3) 0.0104(16) 0.0025(16) -0.0001(11) C3 0.0283(15) 0.0197(14) 0.072(2) 0.0146(14) 0.0108(14) 0.0022(12) C4 0.0285(14) 0.0197(13) 0.0412(16) 0.0113(11) 0.0064(12) 0.0045(11) C5 0.0180(12) 0.0175(12) 0.0335(14) 0.0030(10) -0.0053(10) 0.0001(9) C6 0.0217(13) 0.0122(11) 0.0395(15) 0.0004(10) -0.0081(11) 0.0029(10) C7 0.0272(13) 0.0189(13) 0.0177(12) -0.0048(9) -0.0023(10) 0.0052(10) C8 0.0517(18) 0.0310(15) 0.0170(13) -0.0069(11) -0.0017(12) 0.0146(13) C9 0.0489(17) 0.0297(15) 0.0157(12) -0.0037(11) -0.0047(11) 0.0133(13) C10 0.0213(12) 0.0180(12) 0.0155(11) -0.0031(9) -0.0014(9) 0.0033(10) C11 0.0139(11) 0.0178(12) 0.0168(11) 0.0002(9) -0.0001(9) 0.0018(9) C12 0.0170(12) 0.0215(12) 0.0245(12) 0.0037(10) 0.0063(9) 0.0045(10) C13 0.0220(12) 0.0212(12) 0.0171(11) -0.0018(9) 0.0044(9) 0.0059(10) C14 0.0274(13) 0.0208(12) 0.0274(13) -0.0032(10) 0.0012(10) 0.0046(10) C15 0.0294(14) 0.0208(13) 0.0324(14) 0.0020(11) 0.0016(11) 0.0100(11) C16 0.0189(13) 0.0306(15) 0.0361(15) 0.0052(12) 0.0013(11) 0.0083(11) C17 0.0170(13) 0.0249(14) 0.0384(15) 0.0050(12) 0.0016(11) 0.0015(11) C18 0.0168(11) 0.0195(12) 0.0133(10) -0.0009(9) 0.0016(8) 0.0008(10) C19 0.0155(11) 0.0173(12) 0.0182(11) 0.0034(9) -0.0015(9) 0.0030(9) C20 0.0284(14) 0.0334(15) 0.0238(13) 0.0107(11) 0.0066(11) 0.0067(11) C21 0.0219(12) 0.0209(12) 0.0239(12) -0.0021(10) -0.0010(10) 0.0041(10) C22 0.0202(13) 0.0246(13) 0.0318(14) 0.0032(11) -0.0068(10) 0.0011(10) C23 0.0185(12) 0.0160(12) 0.0444(15) 0.0009(11) 0.0038(11) 0.0014(10) C24 0.0189(13) 0.0166(12) 0.0591(19) -0.0033(12) -0.0035(12) -0.0005(10) C25 0.0284(14) 0.0184(13) 0.0536(17) -0.0129(12) -0.0168(13) 0.0040(11) C26 0.0333(14) 0.0187(12) 0.0309(13) -0.0077(10) -0.0084(11) 0.0050(10) C27 0.0213(12) 0.0166(12) 0.0312(13) -0.0033(10) -0.0026(10) -0.0003(10) C28 0.0154(11) 0.0118(11) 0.0317(13) -0.0019(9) 0.0004(10) 0.0019(9) C29 0.0174(11) 0.0142(11) 0.0172(11) 0.0016(9) -0.0006(9) -0.0009(9) C30 0.0137(10) 0.0166(11) 0.0150(11) 0.0012(8) 0.0004(8) 0.0003(9) C31 0.0350(14) 0.0213(13) 0.0161(12) 0.0018(10) 0.0034(10) 0.0020(11) C32 0.0245(12) 0.0241(13) 0.0148(11) 0.0022(10) -0.0006(9) 0.0027(10) C33 0.0135(11) 0.0166(12) 0.0159(11) 0.0016(9) 0.0005(8) 0.0000(9) C34 0.0157(11) 0.0146(11) 0.0175(11) 0.0007(9) -0.0017(9) 0.0017(9) C35 0.0148(11) 0.0167(11) 0.0150(11) 0.0007(9) -0.0012(8) 0.0008(9) C36 0.0217(12) 0.0157(11) 0.0248(12) 0.0028(9) 0.0034(9) -0.0014(9) C37 0.0269(13) 0.0154(12) 0.0299(13) -0.0004(10) 0.0020(11) 0.0051(10) C38 0.0191(12) 0.0223(13) 0.0282(13) 0.0004(10) 0.0035(10) 0.0047(10) C39 0.0169(12) 0.0187(12) 0.0242(12) 0.0013(10) 0.0016(9) -0.0008(9) C40 0.0146(11) 0.0192(12) 0.0124(10) 0.0018(9) -0.0009(8) 0.0007(9) C41 0.0169(11) 0.0192(12) 0.0213(12) -0.0049(9) -0.0016(9) 0.0056(9) C42 0.0273(13) 0.0199(13) 0.0265(13) -0.0009(10) -0.0065(10) 0.0086(11) C43 0.0259(14) 0.0354(15) 0.0228(13) -0.0111(11) -0.0057(11) 0.0060(12) C44 0.0201(13) 0.0323(15) 0.0404(16) -0.0089(12) 0.0060(11) 0.0051(11) C45 0.0219(13) 0.0182(12) 0.0294(13) 0.0028(10) -0.0004(10) -0.0016(10) C46 0.0293(13) 0.0215(13) 0.0335(14) 0.0051(11) 0.0047(11) 0.0008(11) C47 0.0302(15) 0.0242(14) 0.0565(19) 0.0088(13) 0.0123(13) 0.0010(12) C48 0.0195(14) 0.0181(14) 0.076(2) -0.0015(14) 0.0022(14) -0.0001(11) C49 0.0269(14) 0.0164(13) 0.0549(18) -0.0074(12) -0.0082(13) 0.0052(11) C50 0.0229(13) 0.0130(12) 0.0362(14) -0.0020(10) -0.0049(11) 0.0045(10) C51 0.0355(14) 0.0166(12) 0.0161(12) -0.0029(9) -0.0021(10) 0.0046(11) C52 0.070(2) 0.0260(15) 0.0165(13) -0.0015(11) 0.0002(13) 0.0103(14) C53 0.125(3) 0.0236(16) 0.0167(14) -0.0028(11) -0.0084(17) 0.0147(18) C54 0.0297(13) 0.0150(12) 0.0178(12) 0.0001(9) -0.0044(10) 0.0042(10) C55 0.0202(12) 0.0195(12) 0.0199(12) 0.0010(10) 0.0000(9) 0.0021(10) C56 0.0182(12) 0.0200(13) 0.0385(15) 0.0076(11) 0.0088(11) 0.0037(10) C57 0.0269(13) 0.0203(12) 0.0183(11) 0.0023(10) 0.0083(10) 0.0048(10) C58 0.0369(15) 0.0195(12) 0.0284(14) 0.0029(10) 0.0038(11) 0.0052(11) C59 0.0336(15) 0.0213(14) 0.0442(17) 0.0098(12) 0.0110(13) 0.0101(12) C60 0.0159(13) 0.0325(16) 0.078(2) 0.0221(16) 0.0042(13) 0.0070(12) C61 0.0141(13) 0.0243(15) 0.082(2) 0.0121(15) 0.0012(14) 0.0006(11) C62 0.0161(11) 0.0187(12) 0.0162(11) -0.0020(9) -0.0005(9) 0.0022(10) C63 0.0175(11) 0.0149(11) 0.0161(11) 0.0023(9) -0.0022(9) 0.0039(9) C64 0.0309(14) 0.0321(15) 0.0213(12) 0.0073(11) 0.0056(10) 0.0080(11) C65 0.0179(11) 0.0196(13) 0.0210(12) -0.0020(10) -0.0003(9) 0.0054(10) C66 0.0223(13) 0.0243(13) 0.0331(14) -0.0016(11) -0.0099(11) 0.0027(10) C67A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C68A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C69A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C70A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C71A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C72A 0.0212(13) 0.0182(13) 0.0482(17) -0.0096(11) -0.0095(11) 0.0020(9) C73 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) C74A 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) C75A 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) C76 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) C77 0.0202(12) 0.0169(12) 0.0205(12) -0.0003(9) 0.0017(9) 0.0009(9) C78 0.0183(11) 0.0160(11) 0.0168(11) -0.0012(9) -0.0018(9) -0.0004(9) C79 0.0165(11) 0.0154(11) 0.0171(11) 0.0000(9) -0.0025(9) 0.0001(9) C80 0.0229(13) 0.0170(12) 0.0382(14) 0.0045(10) 0.0045(11) 0.0004(10) C81 0.0282(14) 0.0173(13) 0.0558(18) 0.0012(12) 0.0095(13) 0.0086(11) C82 0.0197(13) 0.0260(15) 0.0436(16) -0.0009(12) 0.0071(11) 0.0079(11) C83 0.0170(12) 0.0213(14) 0.0303(14) 0.0027(10) 0.0037(10) 0.0011(10) C84 0.0156(11) 0.0172(11) 0.0158(11) 0.0017(9) 0.0009(8) 0.0010(9) C85 0.0160(11) 0.0123(11) 0.0201(11) -0.0010(9) 0.0021(9) 0.0037(9) C86 0.0185(12) 0.0223(13) 0.0363(14) 0.0016(11) 0.0050(10) 0.0013(10) C87 0.0228(12) 0.0279(14) 0.0192(12) -0.0044(10) -0.0011(10) 0.0044(11) C88 0.0198(12) 0.0185(12) 0.0213(12) 0.0002(9) -0.0027(9) 0.0017(10) N1 0.0333(12) 0.0180(11) 0.0311(12) -0.0086(9) -0.0141(10) 0.0014(9) N2 0.0153(10) 0.0197(11) 0.0331(11) 0.0055(9) 0.0025(9) 0.0033(9) N3 0.0179(10) 0.0195(10) 0.0204(10) 0.0042(8) 0.0035(8) -0.0037(8) N4 0.0137(9) 0.0133(9) 0.0267(10) 0.0012(8) 0.0037(8) 0.0002(8) N5 0.0361(12) 0.0193(11) 0.0233(11) -0.0058(9) -0.0109(10) -0.0001(9) N6 0.0180(11) 0.0167(11) 0.0645(17) 0.0043(11) -0.0032(11) 0.0022(9) N7B 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) N8 0.0195(10) 0.0151(10) 0.0382(12) 0.0069(9) 0.0125(9) 0.0009(9) O1 0.0166(9) 0.0207(9) 0.0416(11) 0.0043(8) -0.0030(7) -0.0008(7) O2 0.0148(8) 0.0167(8) 0.0182(8) 0.0001(6) -0.0008(6) 0.0018(6) O3 0.0177(9) 0.0171(8) 0.0309(9) 0.0026(7) 0.0046(7) 0.0007(7) O4 0.0154(8) 0.0171(8) 0.0216(8) 0.0001(7) 0.0025(6) 0.0032(6) O5 0.0169(9) 0.0190(9) 0.0423(11) 0.0007(8) -0.0037(7) 0.0002(7) O6 0.0173(8) 0.0152(8) 0.0221(8) 0.0002(7) -0.0034(6) 0.0022(6) O7 0.0172(8) 0.0163(8) 0.0320(9) 0.0035(7) 0.0050(7) -0.0007(7) O8 0.0168(8) 0.0150(8) 0.0257(9) 0.0028(7) 0.0030(6) 0.0006(6) C70B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) C72B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) C71B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) C67B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) C69B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) C68B 0.0210(12) 0.0162(11) 0.0561(18) -0.0101(10) -0.0085(10) 0.0009(9) N7A 0.0207(7) 0.0153(7) 0.0192(7) 0.0029(6) 0.0050(6) 0.0008(6) C74B 0.035(4) 0.018(3) 0.019(2) 0.008(2) 0.007(3) 0.003(2) C75B 0.036(5) 0.026(3) 0.020(2) 0.000(2) 0.002(3) 0.016(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0179 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0181 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0495 0.0323 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.4(3) . . ? C2 C1 H1 119.8 . . ? C6 C1 H1 119.8 . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N1 C6 C5 122.5(2) . . ? N1 C6 C1 120.2(2) . . ? C5 C6 C1 117.3(3) . . ? N1 C7 C13 112.4(2) . . ? N1 C7 C8 111.0(2) . . ? C13 C7 C8 113.7(2) . . ? N1 C7 C10 114.1(2) . . ? C13 C7 C10 114.98(19) . . ? C8 C7 C10 88.47(18) . . ? C9 C8 C7 90.8(2) . . ? C9 C8 H8A 113.5 . . ? C7 C8 H8A 113.5 . . ? C9 C8 H8B 113.5 . . ? C7 C8 H8B 113.5 . . ? H8A C8 H8B 110.8 . . ? C8 C9 C10 89.9(2) . . ? C8 C9 H9A 113.7 . . ? C10 C9 H9A 113.7 . . ? C8 C9 H9B 113.7 . . ? C10 C9 H9B 113.7 . . ? H9A C9 H9B 110.9 . . ? C11 C10 C9 115.0(2) . . ? C11 C10 C7 114.21(19) . . ? C9 C10 C7 90.07(18) . . ? C11 C10 H10 111.9 . . ? C9 C10 H10 111.9 . . ? C7 C10 H10 111.9 . . ? N2 C11 C10 110.57(19) . . ? N2 C11 C18 108.62(19) . . ? C10 C11 C18 112.93(18) . . ? N2 C11 H11 108.2 . . ? C10 C11 H11 108.2 . . ? C18 C11 H11 108.2 . . ? C17 C12 C13 119.9(2) . . ? C17 C12 N2 121.1(2) . . ? C13 C12 N2 119.0(2) . . ? C14 C13 C12 118.7(2) . . ? C14 C13 C7 122.7(2) . . ? C12 C13 C7 118.6(2) . . ? C15 C14 C13 121.2(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? O1 C18 O2 126.6(2) . . ? O1 C18 C11 123.6(2) . . ? O2 C18 C11 109.86(18) . . ? O2 C19 C21 109.48(18) . . ? O2 C19 C20 110.00(18) . . ? C21 C19 C20 113.4(2) . . ? O2 C19 C22 101.94(18) . . ? C21 C19 C22 110.9(2) . . ? C20 C19 C22 110.5(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 120.9(3) . . ? C24 C23 H23 119.6 . . ? C28 C23 H23 119.6 . . ? C23 C24 C25 121.0(2) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 118.8(2) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 121.2(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C28 120.1(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? N3 C28 C27 123.3(2) . . ? N3 C28 C23 118.7(2) . . ? C27 C28 C23 118.0(2) . . ? N3 C29 C35 112.62(19) . . ? N3 C29 C32 110.29(19) . . ? C35 C29 C32 113.47(19) . . ? N3 C29 C30 114.15(18) . . ? C35 C29 C30 115.46(18) . . ? C32 C29 C30 88.63(17) . . ? C33 C30 C31 115.84(19) . . ? C33 C30 C29 114.10(18) . . ? C31 C30 C29 89.79(17) . . ? C33 C30 H30 111.8 . . ? C31 C30 H30 111.8 . . ? C29 C30 H30 111.8 . . ? C32 C31 C30 90.29(18) . . ? C32 C31 H31A 113.6 . . ? C30 C31 H31A 113.6 . . ? C32 C31 H31B 113.6 . . ? C30 C31 H31B 113.6 . . ? H31A C31 H31B 110.9 . . ? C31 C32 C29 90.73(17) . . ? C31 C32 H32A 113.5 . . ? C29 C32 H32A 113.5 . . ? C31 C32 H32B 113.5 . . ? C29 C32 H32B 113.5 . . ? H32A C32 H32B 110.8 . . ? N4 C33 C30 110.88(18) . . ? N4 C33 C40 108.61(18) . . ? C30 C33 C40 113.16(19) . . ? N4 C33 H33 108.0 . . ? C30 C33 H33 108.0 . . ? C40 C33 H33 108.0 . . ? C39 C34 C35 119.4(2) . . ? C39 C34 N4 121.0(2) . . ? C35 C34 N4 119.5(2) . . ? C36 C35 C34 119.1(2) . . ? C36 C35 C29 122.1(2) . . ? C34 C35 C29 118.6(2) . . ? C37 C36 C35 121.1(2) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C38 C37 C36 119.6(2) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 120.3(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 120.5(2) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? O3 C40 O4 126.3(2) . . ? O3 C40 C33 123.5(2) . . ? O4 C40 C33 110.15(18) . . ? O4 C41 C42 109.76(19) . . ? O4 C41 C44 101.98(19) . . ? C42 C41 C44 111.5(2) . . ? O4 C41 C43 109.94(18) . . ? C42 C41 C43 112.7(2) . . ? C44 C41 C43 110.4(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 120.5(2) . . ? C46 C45 H45 119.7 . . ? C50 C45 H45 119.7 . . ? C47 C46 C45 121.2(3) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 118.6(3) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C47 C48 C49 120.8(3) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C48 C49 C50 120.9(3) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C45 C50 C49 118.0(3) . . ? C45 C50 N5 122.7(2) . . ? C49 C50 N5 119.3(2) . . ? N5 C51 C57 112.7(2) . . ? N5 C51 C52 111.0(2) . . ? C57 C51 C52 113.0(2) . . ? N5 C51 C54 114.7(2) . . ? C57 C51 C54 115.2(2) . . ? C52 C51 C54 87.93(18) . . ? C53 C52 C51 90.7(2) . . ? C53 C52 H52A 113.5 . . ? C51 C52 H52A 113.5 . . ? C53 C52 H52B 113.5 . . ? C51 C52 H52B 113.5 . . ? H52A C52 H52B 110.8 . . ? C54 C53 C52 90.6(2) . . ? C54 C53 H53A 113.5 . . ? C52 C53 H53A 113.5 . . ? C54 C53 H53B 113.5 . . ? C52 C53 H53B 113.5 . . ? H53A C53 H53B 110.8 . . ? C55 C54 C53 116.2(2) . . ? C55 C54 C51 115.26(19) . . ? C53 C54 C51 90.79(19) . . ? C55 C54 H54 111.1 . . ? C53 C54 H54 111.1 . . ? C51 C54 H54 111.1 . . ? N6 C55 C54 110.8(2) . . ? N6 C55 C62 108.6(2) . . ? C54 C55 C62 112.38(19) . . ? N6 C55 H55 108.3 . . ? C54 C55 H55 108.3 . . ? C62 C55 H55 108.3 . . ? C61 C56 N6 120.7(3) . . ? C61 C56 C57 119.5(2) . . ? N6 C56 C57 119.8(2) . . ? C58 C57 C56 118.9(2) . . ? C58 C57 C51 121.5(2) . . ? C56 C57 C51 119.5(2) . . ? C59 C58 C57 121.5(3) . . ? C59 C58 H58 119.3 . . ? C57 C58 H58 119.3 . . ? C60 C59 C58 119.3(3) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C61 120.6(3) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C56 120.2(3) . . ? C60 C61 H61 119.9 . . ? C56 C61 H61 119.9 . . ? O5 C62 O6 126.5(2) . . ? O5 C62 C55 123.8(2) . . ? O6 C62 C55 109.66(19) . . ? O6 C63 C64 109.66(18) . . ? O6 C63 C65 109.19(18) . . ? C64 C63 C65 113.3(2) . . ? O6 C63 C66 102.12(18) . . ? C64 C63 C66 110.9(2) . . ? C65 C63 C66 111.1(2) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68A C67A C72A 120.0 . . ? C68A C67A N7A 123.6(3) . . ? C72A C67A N7A 116.3(3) . . ? C67A C68A C69A 120.0 . . ? C67A C68A H68A 120.0 . . ? C69A C68A H68A 120.0 . . ? C70A C69A C68A 120.0 . . ? C70A C69A H69A 120.0 . . ? C68A C69A H69A 120.0 . . ? C69A C70A C71A 120.0 . . ? C69A C70A H70A 120.0 . . ? C71A C70A H70A 120.0 . . ? C70A C71A C72A 120.0 . . ? C70A C71A H71A 120.0 . . ? C72A C71A H71A 120.0 . . ? C71A C72A C67A 120.0 . . ? C71A C72A H72A 120.0 . . ? C67A C72A H72A 120.0 . . ? N7A C73 C79 116.0(3) . . ? C74B C73 C79 119.4(3) . . ? C74B C73 N7B 109.7(3) . . ? C79 C73 N7B 109.4(2) . . ? N7A C73 C76 118.5(3) . . ? C74B C73 C76 90.6(3) . . ? C79 C73 C76 114.98(19) . . ? N7B C73 C76 111.6(2) . . ? N7A C73 C74A 110.3(3) . . ? C79 C73 C74A 106.2(3) . . ? C76 C73 C74A 85.6(3) . . ? C75A C74A C73 92.4(6) . . ? C75A C74A H74A 113.2 . . ? C73 C74A H74A 113.2 . . ? C75A C74A H74B 113.2 . . ? C73 C74A H74B 113.2 . . ? H74A C74A H74B 110.6 . . ? C74A C75A C76 96.2(7) . . ? C74A C75A H75A 112.5 . . ? C76 C75A H75A 112.5 . . ? C74A C75A H75B 112.5 . . ? C76 C75A H75B 112.5 . . ? H75A C75A H75B 110.0 . . ? C75B C76 C77 118.6(4) . . ? C75B C76 C73 94.0(3) . . ? C77 C76 C73 115.76(19) . . ? C77 C76 C75A 113.6(4) . . ? C73 C76 C75A 85.6(4) . . ? C77 C76 H76 113.0 . . ? C73 C76 H76 113.0 . . ? C75A C76 H76 113.0 . . ? N8 C77 C84 109.08(19) . . ? N8 C77 C76 110.82(19) . . ? C84 C77 C76 112.26(19) . . ? N8 C77 H77 108.2 . . ? C84 C77 H77 108.2 . . ? C76 C77 H77 108.2 . . ? C83 C78 N8 120.3(2) . . ? C83 C78 C79 119.8(2) . . ? N8 C78 C79 119.8(2) . . ? C80 C79 C78 118.8(2) . . ? C80 C79 C73 120.3(2) . . ? C78 C79 C73 120.8(2) . . ? C81 C80 C79 121.0(2) . . ? C81 C80 H80 119.5 . . ? C79 C80 H80 119.5 . . ? C80 C81 C82 119.9(2) . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 120.0(2) . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C82 C83 C78 120.4(2) . . ? C82 C83 H83 119.8 . . ? C78 C83 H83 119.8 . . ? O7 C84 O8 126.5(2) . . ? O7 C84 C77 123.8(2) . . ? O8 C84 C77 109.65(19) . . ? O8 C85 C86 102.37(18) . . ? O8 C85 C87 109.93(18) . . ? C86 C85 C87 110.8(2) . . ? O8 C85 C88 109.30(18) . . ? C86 C85 C88 111.2(2) . . ? C87 C85 C88 112.8(2) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C6 N1 C7 122.8(2) . . ? C6 N1 H100 113(2) . . ? C7 N1 H100 117(2) . . ? C12 N2 C11 114.06(19) . . ? C12 N2 H200 115(2) . . ? C11 N2 H200 110.5(19) . . ? C28 N3 C29 122.79(19) . . ? C28 N3 H300 115(2) . . ? C29 N3 H300 110(2) . . ? C34 N4 C33 114.89(19) . . ? C34 N4 H400 114.4(18) . . ? C33 N4 H400 112.4(18) . . ? C50 N5 C51 121.9(2) . . ? C50 N5 H500 114(2) . . ? C51 N5 H500 113(2) . . ? C56 N6 C55 116.8(2) . . ? C56 N6 H600 114(3) . . ? C55 N6 H600 114(2) . . ? C67B N7B C73 127.9(4) . . ? C67B N7B H7B 116.1 . . ? C73 N7B H7B 116.1 . . ? C78 N8 C77 118.2(2) . . ? C78 N8 H800 115(2) . . ? C77 N8 H800 114(2) . . ? C18 O2 C19 122.54(17) . . ? C40 O4 C41 122.54(17) . . ? C62 O6 C63 122.51(17) . . ? C84 O8 C85 122.70(17) . . ? C72B C70B C68B 120.0 . . ? C72B C70B H70B 120.0 . . ? C68B C70B H70B 120.0 . . ? C71B C72B C70B 120.0 . . ? C71B C72B H72B 120.0 . . ? C70B C72B H72B 120.0 . . ? C67B C71B C72B 120.0 . . ? C67B C71B H71B 120.0 . . ? C72B C71B H71B 120.0 . . ? C71B C67B C69B 120.0 . . ? C71B C67B N7B 118.5(3) . . ? C69B C67B N7B 121.4(3) . . ? C68B C69B C67B 120.0 . . ? C68B C69B H69B 120.0 . . ? C67B C69B H69B 120.0 . . ? C69B C68B C70B 120.0 . . ? C69B C68B H68B 120.0 . . ? C70B C68B H68B 120.0 . . ? C73 N7A C67A 119.5(4) . . ? C73 N7A H7A 120.3 . . ? C67A N7A H7A 120.3 . . ? C73 C74B C75B 88.8(4) . . ? C73 C74B H74C 113.8 . . ? C75B C74B H74C 113.8 . . ? C73 C74B H74D 113.8 . . ? C75B C74B H74D 113.8 . . ? H74C C74B H74D 111.1 . . ? C76 C75B C74B 85.3(5) . . ? C76 C75B H75C 114.4 . . ? C74B C75B H75C 114.4 . . ? C76 C75B H75D 114.4 . . ? C74B C75B H75D 114.4 . . ? H75C C75B H75D 111.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(5) . ? C1 C6 1.414(4) . ? C1 H1 0.9500 . ? C2 C3 1.375(5) . ? C2 H2 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.397(4) . ? C5 H5 0.9500 . ? C6 N1 1.382(4) . ? C7 N1 1.458(3) . ? C7 C13 1.516(3) . ? C7 C8 1.558(3) . ? C7 C10 1.571(3) . ? C8 C9 1.543(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.548(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.517(3) . ? C10 H10 1.0000 . ? C11 N2 1.462(3) . ? C11 C18 1.524(3) . ? C11 H11 1.0000 . ? C12 C17 1.393(4) . ? C12 C13 1.402(4) . ? C12 N2 1.412(3) . ? C13 C14 1.391(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 O1 1.207(3) . ? C18 O2 1.331(3) . ? C19 O2 1.486(3) . ? C19 C21 1.510(3) . ? C19 C20 1.513(3) . ? C19 C22 1.517(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.375(4) . ? C23 C28 1.413(3) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.389(4) . ? C25 H25 0.9500 . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.399(4) . ? C27 H27 0.9500 . ? C28 N3 1.386(3) . ? C29 N3 1.453(3) . ? C29 C35 1.512(3) . ? C29 C32 1.556(3) . ? C29 C30 1.576(3) . ? C30 C33 1.515(3) . ? C30 C31 1.546(3) . ? C30 H30 1.0000 . ? C31 C32 1.541(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N4 1.458(3) . ? C33 C40 1.528(3) . ? C33 H33 1.0000 . ? C34 C39 1.399(3) . ? C34 C35 1.400(3) . ? C34 N4 1.402(3) . ? C35 C36 1.393(3) . ? C36 C37 1.386(4) . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 C39 1.384(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O3 1.205(3) . ? C40 O4 1.333(3) . ? C41 O4 1.487(3) . ? C41 C42 1.510(4) . ? C41 C44 1.515(3) . ? C41 C43 1.518(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.389(4) . ? C45 C50 1.395(4) . ? C45 H45 0.9500 . ? C46 C47 1.384(4) . ? C46 H46 0.9500 . ? C47 C48 1.386(5) . ? C47 H47 0.9500 . ? C48 C49 1.386(4) . ? C48 H48 0.9500 . ? C49 C50 1.401(4) . ? C49 H49 0.9500 . ? C50 N5 1.402(4) . ? C51 N5 1.450(3) . ? C51 C57 1.509(3) . ? C51 C52 1.567(3) . ? C51 C54 1.576(3) . ? C52 C53 1.542(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.529(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.515(3) . ? C54 H54 1.0000 . ? C55 N6 1.444(3) . ? C55 C62 1.519(3) . ? C55 H55 1.0000 . ? C56 C61 1.395(4) . ? C56 N6 1.402(3) . ? C56 C57 1.404(4) . ? C57 C58 1.389(4) . ? C58 C59 1.383(4) . ? C58 H58 0.9500 . ? C59 C60 1.382(5) . ? C59 H59 0.9500 . ? C60 C61 1.383(4) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 O5 1.203(3) . ? C62 O6 1.333(3) . ? C63 O6 1.486(3) . ? C63 C64 1.514(3) . ? C63 C65 1.515(3) . ? C63 C66 1.517(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67A C68A 1.3900 . ? C67A C72A 1.3900 . ? C67A N7A 1.411(6) . ? C68A C69A 1.3900 . ? C68A H68A 0.9500 . ? C69A C70A 1.3900 . ? C69A H69A 0.9500 . ? C70A C71A 1.3900 . ? C70A H70A 0.9500 . ? C71A C72A 1.3900 . ? C71A H71A 0.9500 . ? C72A H72A 0.9500 . ? C73 N7A 1.376(5) . ? C73 C74B 1.504(6) . ? C73 C79 1.505(3) . ? C73 N7B 1.545(5) . ? C73 C76 1.565(3) . ? C73 C74A 1.629(8) . ? C74A C75A 1.323(13) . ? C74A H74A 0.9900 . ? C74A H74B 0.9900 . ? C75A C76 1.584(11) . ? C75A H75A 0.9900 . ? C75A H75B 0.9900 . ? C76 C75B 1.511(9) . ? C76 C77 1.522(3) . ? C76 H76 1.0000 . ? C77 N8 1.441(3) . ? C77 C84 1.522(3) . ? C77 H77 1.0000 . ? C78 C83 1.390(3) . ? C78 N8 1.401(3) . ? C78 C79 1.405(3) . ? C79 C80 1.392(3) . ? C80 C81 1.382(4) . ? C80 H80 0.9500 . ? C81 C82 1.387(4) . ? C81 H81 0.9500 . ? C82 C83 1.385(4) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? C84 O7 1.205(3) . ? C84 O8 1.331(3) . ? C85 O8 1.490(3) . ? C85 C86 1.514(3) . ? C85 C87 1.516(3) . ? C85 C88 1.518(3) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? N1 H100 0.87(3) . ? N2 H200 0.94(3) . ? N3 H300 0.92(3) . ? N4 H400 0.89(3) . ? N5 H500 0.90(3) . ? N6 H600 0.82(4) . ? N7B C67B 1.394(5) . ? N7B H7B 0.8800 . ? N8 H800 0.85(3) . ? C70B C72B 1.3900 . ? C70B C68B 1.3900 . ? C70B H70B 0.9500 . ? C72B C71B 1.3900 . ? C72B H72B 0.9500 . ? C71B C67B 1.3900 . ? C71B H71B 0.9500 . ? C67B C69B 1.3900 . ? C69B C68B 1.3900 . ? C69B H69B 0.9500 . ? C68B H68B 0.9500 . ? N7A H7A 0.8800 . ? C74B C75B 1.704(10) . ? C74B H74C 0.9900 . ? C74B H74D 0.9900 . ? C75B H75C 0.9900 . ? C75B H75D 0.9900 . ?