#------------------------------------------------------------------------------ #$Date: 2019-11-17 08:52:39 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229920.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_7229920 loop_ _publ_author_name 'Alimi, Lukman O.' 'Lama, Prem' 'Smith, Vincent J.' 'Barbour, Leonard J.' _publ_section_title ; Large volumetric thermal expansion of a novel organic cocrystal over a wide temperature range ; _journal_issue 5 _journal_name_full CrystEngComm _journal_page_first 631 _journal_paper_doi 10.1039/C7CE01848G _journal_volume 20 _journal_year 2018 _chemical_formula_sum 'C25 H26 N6' _chemical_formula_weight 410.52 _chemical_name_common ABN.2DMABN _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-06-09 deposited with the CCDC. 2018-01-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.2740(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.7661(3) _cell_length_b 25.2392(8) _cell_length_c 19.0103(6) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 140(2) _cell_measurement_theta_max 28.19 _cell_measurement_theta_min 2.66 _cell_volume 4541.2(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 140(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 209426 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.363 _diffrn_reflns_theta_min 1.368 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_T_max 0.9920 _exptl_absorpt_correction_T_min 0.9761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.201 _exptl_crystal_description Flat _exptl_crystal_F_000 1744 _exptl_crystal_size_max 0.327 _exptl_crystal_size_mid 0.234 _exptl_crystal_size_min 0.108 _refine_diff_density_max 0.390 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 567 _refine_ls_number_reflns 11237 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0888 _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^)+(0.1361P)^2^+3.4630P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2262 _refine_ls_wR_factor_ref 0.2896 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6781 _reflns_number_total 11237 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce01848g3.cif _cod_data_source_block 140K _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 7229912--7229922.cif. ; _cod_database_code 7229920 _shelx_shelxl_version_number 2016/6 _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 0.976 _shelx_estimated_absorpt_t_max 0.992 _shelx_res_file ; TITL C:\Users\lukman\Desktop\140K\140K_a.res in P2(1)/n C:\Users\lukman\Desktop\140K\140K_a.res created by SHELXL-2016/6 at 12:09:25 on 02-Mar-2017 CELL 0.71073 9.7661 25.2392 19.0103 90.000 104.274 90.000 ZERR 8.0000 0.0003 0.0008 0.0006 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N UNIT 200 208 48 BOND $H CONF OMIT -1 12 2 OMIT 2 6 6 OMIT 0 18 6 OMIT 1 6 8 OMIT 0 21 7 OMIT 1 0 1 OMIT -2 8 8 OMIT 1 4 6 OMIT -2 20 4 OMIT 2 16 0 OMIT 1 6 0 OMIT 1 12 6 OMIT 2 20 0 OMIT 0 0 14 OMIT 0 15 5 OMIT 1 2 8 OMIT 1 2 4 OMIT 1 20 6 OMIT -1 10 8 OMIT 2 14 14 OMIT -2 16 4 OMIT 0 12 0 OMIT 1 14 8 OMIT -2 10 2 OMIT -3 10 8 OMIT -2 22 2 OMIT 2 11 12 OMIT -1 9 11 OMIT 1 14 0 OMIT 2 12 0 OMIT 1 22 0 OMIT -1 4 10 OMIT -1 8 2 OMIT -1 4 6 OMIT -12 0 12 OMIT -2 14 2 OMIT 0 7 21 OMIT 2 0 8 OMIT 2 20 12 OMIT -6 1 14 OMIT -5 1 20 OMIT 0 2 1 OMIT 1 11 10 OMIT -7 0 17 OMIT 1 4 1 OMIT -6 1 18 OMIT -8 9 6 OMIT 7 2 9 OMIT -6 3 17 OMIT 2 14 2 OMIT 2 0 4 OMIT -12 13 6 OMIT 11 8 3 OMIT 1 8 2 OMIT 1 20 2 OMIT -6 3 16 OMIT 7 3 10 OMIT -6 3 18 OMIT -7 4 14 OMIT -7 1 18 OMIT -7 3 13 OMIT -6 8 18 OMIT 3 18 17 OMIT -6 3 19 OMIT -6 3 15 OMIT -4 11 16 OMIT 12 0 0 OMIT -1 8 18 OMIT 3 21 6 OMIT -6 2 17 OMIT -6 0 14 OMIT 7 1 7 OMIT -6 1 19 OMIT -5 1 19 OMIT -3 15 3 OMIT 4 11 17 OMIT -5 3 17 OMIT 7 3 8 OMIT 7 7 10 ACTA 50 PLAN 10 0 0 LIST 6 1 SIZE 0.327 0.234 0.108 TEMP -133 L.S. 10 WGHT 0.136100 3.463000 FVAR 0.30569 N1 3 0.741325 0.953480 0.511175 11.00000 0.05077 0.05398 = 0.03745 -0.00054 0.01365 -0.01049 N2 3 0.077201 0.872637 0.502403 11.00000 0.04734 0.06327 = 0.04755 0.00122 0.01019 -0.00318 N3 3 -0.028922 0.747435 0.510367 11.00000 0.03147 0.06450 = 0.05560 -0.00172 0.01246 0.00160 AFIX 93 H3D 2 0.012968 0.717102 0.506399 11.00000 -1.20000 H3E 2 0.018740 0.777277 0.513247 11.00000 -1.20000 AFIX 0 N4 3 -0.718298 0.750636 0.513469 11.00000 0.03761 0.07365 = 0.07264 -0.00649 0.01826 -0.00214 N5 3 0.740458 0.548916 0.497441 11.00000 0.04530 0.04940 = 0.03508 0.00215 0.00668 0.00788 N6 3 0.078267 0.625372 0.500154 11.00000 0.05076 0.05642 = 0.06974 0.00100 0.02228 0.00315 N7 3 0.009299 0.704879 0.760232 11.00000 0.05517 0.04983 = 0.03303 0.00189 0.00823 0.00963 N8 3 0.669704 0.627528 0.756269 11.00000 0.04990 0.06154 = 0.07172 0.00224 0.01227 0.00361 N9 3 0.779562 0.506163 0.745768 11.00000 0.03328 0.06689 = 0.05336 0.00535 0.01366 0.00178 AFIX 93 H9E 2 0.736909 0.536633 0.747805 11.00000 -1.20000 H9D 2 0.732117 0.476326 0.743723 11.00000 -1.20000 AFIX 0 N10 3 1.471551 0.501361 0.748103 11.00000 0.03452 0.07848 = 0.06487 0.00229 0.01190 0.00148 N11 3 0.011023 0.300870 0.738014 11.00000 0.04385 0.04884 = 0.03967 0.00252 0.01117 -0.00641 N12 3 0.679217 0.380049 0.753110 11.00000 0.04603 0.05752 = 0.05384 0.00376 0.01369 -0.00016 C1 1 0.606093 0.938976 0.508837 11.00000 0.04730 0.03214 = 0.03301 0.00141 0.01248 -0.00058 C2 1 0.557735 0.934391 0.573140 11.00000 0.04878 0.03579 = 0.03202 -0.00073 0.00931 -0.00162 AFIX 43 H2 2 0.619565 0.942798 0.618723 11.00000 -1.20000 AFIX 0 C3 1 0.422239 0.917894 0.570023 11.00000 0.04819 0.03752 = 0.03393 0.00085 0.01332 0.00199 AFIX 43 H3 2 0.391601 0.915269 0.613602 11.00000 -1.20000 AFIX 0 C4 1 0.328599 0.904899 0.503917 11.00000 0.04332 0.03704 = 0.03732 0.00135 0.00937 0.00100 C5 1 0.373897 0.910221 0.439879 11.00000 0.05003 0.03984 = 0.03166 0.00072 0.00597 0.00066 AFIX 43 H5 2 0.310922 0.902078 0.394520 11.00000 -1.20000 AFIX 0 C6 1 0.509000 0.927166 0.442092 11.00000 0.05361 0.03769 = 0.03496 0.00112 0.01417 0.00030 AFIX 43 H6 2 0.537512 0.930994 0.398059 11.00000 -1.20000 AFIX 0 C7 1 0.188374 0.886683 0.502367 11.00000 0.04787 0.04537 = 0.03477 0.00029 0.00626 0.00220 C8 1 0.787991 0.959510 0.444734 11.00000 0.05247 0.05709 = 0.04679 -0.00002 0.02132 -0.00445 AFIX 137 H8A 2 0.774451 0.926033 0.417788 11.00000 -1.50000 H8B 2 0.888307 0.969116 0.456741 11.00000 -1.50000 H8C 2 0.732698 0.987451 0.414847 11.00000 -1.50000 AFIX 0 C9 1 0.842181 0.964619 0.579506 11.00000 0.04666 0.06225 = 0.04717 0.00064 0.00901 -0.00622 AFIX 137 H9A 2 0.814377 0.997090 0.600629 11.00000 -1.50000 H9B 2 0.936413 0.969292 0.570998 11.00000 -1.50000 H9C 2 0.843865 0.934998 0.613040 11.00000 -1.50000 AFIX 0 C10 1 -0.167054 0.748193 0.512046 11.00000 0.03142 0.04711 = 0.02921 0.00139 0.00687 0.00227 C11 1 -0.235977 0.796152 0.519236 11.00000 0.04200 0.03656 = 0.03535 0.00008 0.00925 -0.00720 AFIX 43 H11 2 -0.185061 0.828534 0.523161 11.00000 -1.20000 AFIX 0 C12 1 -0.376357 0.796706 0.520652 11.00000 0.04013 0.03143 = 0.03622 0.00008 0.00864 0.00285 AFIX 43 H12 2 -0.421459 0.829396 0.525400 11.00000 -1.20000 AFIX 0 C13 1 -0.452745 0.749397 0.515136 11.00000 0.03238 0.03825 = 0.03257 -0.00040 0.00762 -0.00146 C14 1 -0.384867 0.701804 0.509034 11.00000 0.04120 0.03217 = 0.03268 -0.00171 0.00787 -0.00295 AFIX 43 H14 2 -0.435775 0.669459 0.505872 11.00000 -1.20000 AFIX 0 C15 1 -0.245111 0.701071 0.507531 11.00000 0.04133 0.03668 = 0.03529 -0.00039 0.00872 0.00754 AFIX 43 H15 2 -0.200504 0.668172 0.503371 11.00000 -1.20000 AFIX 0 C16 1 -0.600800 0.750237 0.514347 11.00000 0.03762 0.04340 = 0.04153 -0.00189 0.00854 0.00054 C17 1 0.604111 0.560440 0.497724 11.00000 0.04383 0.02919 = 0.03419 0.00260 0.00766 0.00007 C18 1 0.499917 0.569322 0.431868 11.00000 0.04711 0.03490 = 0.03123 0.00166 0.00900 -0.00098 AFIX 43 H18 2 0.523229 0.564315 0.386671 11.00000 -1.20000 AFIX 0 C19 1 0.366046 0.585059 0.433111 11.00000 0.04469 0.03898 = 0.03714 0.00265 0.00676 -0.00049 AFIX 43 H19 2 0.298437 0.591471 0.388606 11.00000 -1.20000 AFIX 0 C20 1 0.327015 0.591869 0.498769 11.00000 0.04409 0.03466 = 0.04568 0.00066 0.01305 -0.00137 C21 1 0.427188 0.580422 0.563680 11.00000 0.05494 0.03710 = 0.03605 -0.00094 0.01481 0.00080 AFIX 43 H21 2 0.401392 0.583164 0.608570 11.00000 -1.20000 AFIX 0 C22 1 0.561212 0.565399 0.563208 11.00000 0.05404 0.03577 = 0.03315 0.00015 0.00915 -0.00023 AFIX 43 H22 2 0.627226 0.558102 0.607947 11.00000 -1.20000 AFIX 0 C23 1 0.188171 0.610171 0.499677 11.00000 0.04773 0.04577 = 0.04666 0.00228 0.01463 -0.00061 C24 1 0.845909 0.541353 0.565458 11.00000 0.04599 0.05887 = 0.04468 0.00642 0.00399 0.00401 AFIX 137 H24A 2 0.844327 0.571676 0.597445 11.00000 -1.50000 H24B 2 0.939676 0.538426 0.555816 11.00000 -1.50000 H24C 2 0.824830 0.508855 0.588976 11.00000 -1.50000 AFIX 0 C25 1 0.783652 0.539143 0.430930 11.00000 0.04690 0.04896 = 0.04278 0.00216 0.01344 0.00542 AFIX 137 H25A 2 0.737250 0.507004 0.407642 11.00000 -1.50000 H25B 2 0.886382 0.534477 0.442140 11.00000 -1.50000 H25C 2 0.756533 0.569340 0.398035 11.00000 -1.50000 AFIX 0 C26 1 0.144003 0.692251 0.759536 11.00000 0.04647 0.03009 = 0.03211 -0.00113 0.00592 0.00253 C27 1 0.247856 0.681438 0.824351 11.00000 0.06169 0.03392 = 0.03225 -0.00144 0.00730 0.00043 AFIX 43 H27 2 0.224302 0.685224 0.869684 11.00000 -1.20000 AFIX 0 C28 1 0.381386 0.665658 0.823217 11.00000 0.05336 0.04037 = 0.03617 0.00118 0.00134 -0.00108 AFIX 43 H28 2 0.448399 0.658199 0.867567 11.00000 -1.20000 AFIX 0 C29 1 0.420321 0.660386 0.757502 11.00000 0.04657 0.03498 = 0.04545 -0.00094 0.00800 -0.00100 C30 1 0.320864 0.673420 0.692884 11.00000 0.05423 0.03559 = 0.03756 0.00010 0.00877 0.00139 AFIX 43 H30 2 0.347298 0.671644 0.648081 11.00000 -1.20000 AFIX 0 C31 1 0.186810 0.688606 0.693284 11.00000 0.05561 0.03456 = 0.03041 0.00140 0.00426 0.00269 AFIX 43 H31 2 0.121223 0.696850 0.648765 11.00000 -1.20000 AFIX 0 C32 1 0.558784 0.642300 0.756145 11.00000 0.04758 0.04955 = 0.05342 -0.00058 0.00720 -0.00497 C33 1 -0.097288 0.713088 0.693227 11.00000 0.05244 0.05579 = 0.04344 0.00330 0.00541 0.00936 AFIX 137 H33A 2 -0.078703 0.746492 0.670984 11.00000 -1.50000 H33B 2 -0.190747 0.714588 0.703491 11.00000 -1.50000 H33C 2 -0.094579 0.683741 0.659842 11.00000 -1.50000 AFIX 0 C34 1 -0.030079 0.712578 0.828470 11.00000 0.06181 0.05450 = 0.04503 0.00084 0.01998 0.00426 AFIX 137 H34A 2 -0.010371 0.680144 0.857554 11.00000 -1.50000 H34B 2 -0.131090 0.720818 0.818634 11.00000 -1.50000 H34C 2 0.024685 0.741962 0.855211 11.00000 -1.50000 AFIX 0 C35 1 0.918876 0.505183 0.745782 11.00000 0.03160 0.04931 = 0.02646 0.00240 0.00599 0.00212 C36 1 0.988445 0.457053 0.741465 11.00000 0.04206 0.03760 = 0.03671 0.00289 0.01034 -0.00711 AFIX 43 H36 2 0.937563 0.424696 0.738202 11.00000 -1.20000 AFIX 0 C37 1 1.129559 0.456254 0.741912 11.00000 0.04172 0.03126 = 0.03546 0.00199 0.00962 0.00351 AFIX 43 H37 2 1.175449 0.423337 0.739642 11.00000 -1.20000 AFIX 0 C38 1 1.205639 0.503223 0.745660 11.00000 0.03114 0.03726 = 0.03182 0.00064 0.00815 0.00218 C39 1 1.136893 0.551385 0.749055 11.00000 0.04091 0.03294 = 0.03710 -0.00145 0.00865 -0.00334 AFIX 43 H39 2 1.187750 0.583689 0.751406 11.00000 -1.20000 AFIX 0 C40 1 0.996077 0.552284 0.749012 11.00000 0.04378 0.03883 = 0.03577 -0.00175 0.01108 0.00746 AFIX 43 H40 2 0.950541 0.585288 0.751202 11.00000 -1.20000 AFIX 0 C41 1 1.353894 0.502337 0.747708 11.00000 0.03642 0.04239 = 0.04069 -0.00001 0.00770 0.00189 C42 1 0.148127 0.313958 0.742274 11.00000 0.04168 0.02982 = 0.03682 0.00220 0.01220 0.00152 C43 1 0.197961 0.320365 0.678575 11.00000 0.04870 0.03740 = 0.03278 0.00168 0.00908 -0.00136 AFIX 43 H43 2 0.136195 0.313524 0.632422 11.00000 -1.20000 AFIX 0 C44 1 0.333752 0.336258 0.682846 11.00000 0.05065 0.03707 = 0.03431 0.00051 0.01564 0.00023 AFIX 43 H44 2 0.364629 0.340109 0.639483 11.00000 -1.20000 AFIX 0 C45 1 0.427902 0.346937 0.749484 11.00000 0.04112 0.03566 = 0.03762 0.00237 0.01299 0.00139 C46 1 0.381489 0.339409 0.813336 11.00000 0.04679 0.03980 = 0.03146 -0.00032 0.00876 0.00047 AFIX 43 H46 2 0.444484 0.345789 0.859288 11.00000 -1.20000 AFIX 0 C47 1 0.245845 0.322914 0.809627 11.00000 0.04864 0.03788 = 0.03420 0.00156 0.01341 -0.00037 AFIX 43 H47 2 0.217062 0.317403 0.853292 11.00000 -1.20000 AFIX 0 C48 1 0.567972 0.365324 0.752447 11.00000 0.04350 0.04631 = 0.03731 0.00075 0.01142 0.00301 C49 1 -0.038277 0.292300 0.803144 11.00000 0.04438 0.05106 = 0.04878 0.00282 0.01724 -0.00221 AFIX 137 H49A 2 0.012462 0.262260 0.830276 11.00000 -1.50000 H49B 2 -0.139797 0.284675 0.789667 11.00000 -1.50000 H49C 2 -0.020790 0.324177 0.833476 11.00000 -1.50000 AFIX 0 C50 1 -0.089005 0.292380 0.668311 11.00000 0.04543 0.06097 = 0.04681 0.00432 0.00558 -0.00429 AFIX 137 H50A 2 -0.084986 0.322371 0.636139 11.00000 -1.50000 H50B 2 -0.184669 0.289366 0.675509 11.00000 -1.50000 H50C 2 -0.064721 0.259685 0.646346 11.00000 -1.50000 AFIX 0 HKLF 4 REM C:\Users\lukman\Desktop\140K\140K_a.res in P2(1)/n REM R1 = 0.0888 for 6781 Fo > 4sig(Fo) and 0.1366 for all 11237 data REM 567 parameters refined using 0 restraints END WGHT 0.1361 3.4631 REM Highest difference peak 0.390, deepest hole -0.421, 1-sigma level 0.074 Q1 1 1.2819 0.4984 0.7528 11.00000 0.05 0.39 Q2 1 -0.5262 0.7502 0.5167 11.00000 0.05 0.39 Q3 1 -0.2058 0.3313 0.7463 11.00000 0.05 0.34 Q4 1 0.9545 0.9244 0.5058 11.00000 0.05 0.31 Q5 1 1.5612 0.5450 0.7446 11.00000 0.05 0.28 Q6 1 0.8610 0.9081 0.5046 11.00000 0.05 0.27 Q7 1 -0.1727 0.3058 0.7238 11.00000 0.05 0.27 Q8 1 0.1784 0.7019 0.5223 11.00000 0.05 0.26 Q9 1 -0.2788 0.7505 0.5046 11.00000 0.05 0.26 Q10 1 -0.1010 0.3423 0.7557 11.00000 0.05 0.26 ; _shelx_res_checksum 65783 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 N1 N 0.7413(2) 0.95348(9) 0.51117(11) 0.0469(5) Uani 1 1 d . . N2 N 0.0772(3) 0.87264(10) 0.50240(13) 0.0530(6) Uani 1 1 d . . N3 N -0.0289(2) 0.74743(10) 0.51037(13) 0.0502(6) Uani 1 1 d . . H3D H 0.012968 0.717102 0.506399 0.060 Uiso 1 1 calc R U H3E H 0.018740 0.777277 0.513247 0.060 Uiso 1 1 calc R U N4 N -0.7183(3) 0.75064(11) 0.51347(16) 0.0605(7) Uani 1 1 d . . N5 N 0.7405(2) 0.54892(9) 0.49744(11) 0.0438(5) Uani 1 1 d . . N6 N 0.0783(3) 0.62537(10) 0.50015(15) 0.0577(6) Uani 1 1 d . . N7 N 0.0093(2) 0.70488(9) 0.76023(11) 0.0465(5) Uani 1 1 d . . N8 N 0.6697(3) 0.62753(11) 0.75627(15) 0.0615(7) Uani 1 1 d . . N9 N 0.7796(2) 0.50616(10) 0.74577(13) 0.0507(6) Uani 1 1 d . . H9E H 0.736909 0.536633 0.747805 0.061 Uiso 1 1 calc R U H9D H 0.732117 0.476326 0.743723 0.061 Uiso 1 1 calc R U N10 N 1.4716(3) 0.50136(11) 0.74810(15) 0.0594(7) Uani 1 1 d . . N11 N 0.0110(2) 0.30087(9) 0.73801(11) 0.0440(5) Uani 1 1 d . . N12 N 0.6792(2) 0.38005(10) 0.75311(13) 0.0522(6) Uani 1 1 d . . C1 C 0.6061(3) 0.93898(9) 0.50884(12) 0.0370(5) Uani 1 1 d . . C2 C 0.5577(3) 0.93439(9) 0.57314(13) 0.0390(5) Uani 1 1 d . . H2 H 0.619565 0.942798 0.618723 0.047 Uiso 1 1 calc R U C3 C 0.4222(3) 0.91789(10) 0.57002(13) 0.0393(5) Uani 1 1 d . . H3 H 0.391601 0.915269 0.613602 0.047 Uiso 1 1 calc R U C4 C 0.3286(3) 0.90490(10) 0.50392(13) 0.0393(5) Uani 1 1 d . . C5 C 0.3739(3) 0.91022(10) 0.43988(13) 0.0412(5) Uani 1 1 d . . H5 H 0.310922 0.902078 0.394520 0.049 Uiso 1 1 calc R U C6 C 0.5090(3) 0.92717(10) 0.44209(13) 0.0415(6) Uani 1 1 d . . H6 H 0.537512 0.930994 0.398059 0.050 Uiso 1 1 calc R U C7 C 0.1884(3) 0.88668(11) 0.50237(13) 0.0434(6) Uani 1 1 d . . C8 C 0.7880(3) 0.95951(12) 0.44473(15) 0.0505(7) Uani 1 1 d . . H8A H 0.774451 0.926033 0.417788 0.076 Uiso 1 1 calc R U H8B H 0.888307 0.969116 0.456741 0.076 Uiso 1 1 calc R U H8C H 0.732698 0.987451 0.414847 0.076 Uiso 1 1 calc R U C9 C 0.8422(3) 0.96462(12) 0.57951(15) 0.0525(7) Uani 1 1 d . . H9A H 0.814377 0.997090 0.600629 0.079 Uiso 1 1 calc R U H9B H 0.936413 0.969292 0.570998 0.079 Uiso 1 1 calc R U H9C H 0.843865 0.934998 0.613040 0.079 Uiso 1 1 calc R U C10 C -0.1671(2) 0.74819(9) 0.51205(12) 0.0360(5) Uani 1 1 d . . C11 C -0.2360(3) 0.79615(10) 0.51924(12) 0.0380(5) Uani 1 1 d . . H11 H -0.185061 0.828534 0.523161 0.046 Uiso 1 1 calc R U C12 C -0.3764(2) 0.79671(9) 0.52065(12) 0.0361(5) Uani 1 1 d . . H12 H -0.421459 0.829396 0.525400 0.043 Uiso 1 1 calc R U C13 C -0.4527(2) 0.74940(9) 0.51514(12) 0.0345(5) Uani 1 1 d . . C14 C -0.3849(2) 0.70180(9) 0.50903(12) 0.0356(5) Uani 1 1 d . . H14 H -0.435775 0.669459 0.505872 0.043 Uiso 1 1 calc R U C15 C -0.2451(2) 0.70107(10) 0.50753(12) 0.0379(5) Uani 1 1 d . . H15 H -0.200504 0.668172 0.503371 0.045 Uiso 1 1 calc R U C16 C -0.6008(3) 0.75024(10) 0.51435(14) 0.0411(6) Uani 1 1 d . . C17 C 0.6041(3) 0.56044(9) 0.49772(12) 0.0361(5) Uani 1 1 d . . C18 C 0.4999(3) 0.56932(9) 0.43187(12) 0.0379(5) Uani 1 1 d . . H18 H 0.523229 0.564315 0.386671 0.045 Uiso 1 1 calc R U C19 C 0.3660(3) 0.58506(10) 0.43311(13) 0.0409(5) Uani 1 1 d . . H19 H 0.298437 0.591471 0.388606 0.049 Uiso 1 1 calc R U C20 C 0.3270(3) 0.59187(10) 0.49877(14) 0.0411(5) Uani 1 1 d . . C21 C 0.4272(3) 0.58042(10) 0.56368(13) 0.0421(6) Uani 1 1 d . . H21 H 0.401392 0.583164 0.608570 0.050 Uiso 1 1 calc R U C22 C 0.5612(3) 0.56540(10) 0.56321(13) 0.0413(5) Uani 1 1 d . . H22 H 0.627226 0.558102 0.607947 0.050 Uiso 1 1 calc R U C23 C 0.1882(3) 0.61017(11) 0.49968(14) 0.0462(6) Uani 1 1 d . . C24 C 0.8459(3) 0.54135(12) 0.56546(15) 0.0511(7) Uani 1 1 d . . H24A H 0.844327 0.571676 0.597445 0.077 Uiso 1 1 calc R U H24B H 0.939676 0.538426 0.555816 0.077 Uiso 1 1 calc R U H24C H 0.824830 0.508855 0.588976 0.077 Uiso 1 1 calc R U C25 C 0.7837(3) 0.53914(11) 0.43093(14) 0.0458(6) Uani 1 1 d . . H25A H 0.737250 0.507004 0.407642 0.069 Uiso 1 1 calc R U H25B H 0.886382 0.534477 0.442140 0.069 Uiso 1 1 calc R U H25C H 0.756533 0.569340 0.398035 0.069 Uiso 1 1 calc R U C26 C 0.1440(3) 0.69225(9) 0.75954(12) 0.0369(5) Uani 1 1 d . . C27 C 0.2479(3) 0.68144(10) 0.82435(13) 0.0434(6) Uani 1 1 d . . H27 H 0.224302 0.685224 0.869684 0.052 Uiso 1 1 calc R U C28 C 0.3814(3) 0.66566(10) 0.82322(14) 0.0450(6) Uani 1 1 d . . H28 H 0.448399 0.658199 0.867567 0.054 Uiso 1 1 calc R U C29 C 0.4203(3) 0.66039(10) 0.75750(14) 0.0429(6) Uani 1 1 d . . C30 C 0.3209(3) 0.67342(10) 0.69288(14) 0.0429(6) Uani 1 1 d . . H30 H 0.347298 0.671644 0.648081 0.051 Uiso 1 1 calc R U C31 C 0.1868(3) 0.68861(9) 0.69328(13) 0.0413(6) Uani 1 1 d . . H31 H 0.121223 0.696850 0.648765 0.050 Uiso 1 1 calc R U C32 C 0.5588(3) 0.64230(12) 0.75615(16) 0.0511(7) Uani 1 1 d . . C33 C -0.0973(3) 0.71309(12) 0.69323(15) 0.0517(7) Uani 1 1 d . . H33A H -0.078703 0.746492 0.670984 0.078 Uiso 1 1 calc R U H33B H -0.190747 0.714588 0.703491 0.078 Uiso 1 1 calc R U H33C H -0.094579 0.683741 0.659842 0.078 Uiso 1 1 calc R U C34 C -0.0301(3) 0.71258(12) 0.82847(15) 0.0526(7) Uani 1 1 d . . H34A H -0.010371 0.680144 0.857554 0.079 Uiso 1 1 calc R U H34B H -0.131090 0.720818 0.818634 0.079 Uiso 1 1 calc R U H34C H 0.024685 0.741962 0.855211 0.079 Uiso 1 1 calc R U C35 C 0.9189(2) 0.50518(10) 0.74578(12) 0.0360(5) Uani 1 1 d . . C36 C 0.9884(3) 0.45705(10) 0.74147(13) 0.0387(5) Uani 1 1 d . . H36 H 0.937563 0.424696 0.738202 0.046 Uiso 1 1 calc R U C37 C 1.1296(2) 0.45625(9) 0.74191(12) 0.0361(5) Uani 1 1 d . . H37 H 1.175449 0.423337 0.739642 0.043 Uiso 1 1 calc R U C38 C 1.2056(2) 0.50322(9) 0.74566(12) 0.0333(5) Uani 1 1 d . . C39 C 1.1369(2) 0.55139(9) 0.74905(12) 0.0372(5) Uani 1 1 d . . H39 H 1.187750 0.583689 0.751406 0.045 Uiso 1 1 calc R U C40 C 0.9961(3) 0.55228(10) 0.74901(12) 0.0392(5) Uani 1 1 d . . H40 H 0.950541 0.585288 0.751202 0.047 Uiso 1 1 calc R U C41 C 1.3539(3) 0.50234(10) 0.74771(13) 0.0401(5) Uani 1 1 d . . C42 C 0.1481(2) 0.31396(9) 0.74227(13) 0.0357(5) Uani 1 1 d . . C43 C 0.1980(3) 0.32036(10) 0.67858(13) 0.0398(5) Uani 1 1 d . . H43 H 0.136195 0.313524 0.632422 0.048 Uiso 1 1 calc R U C44 C 0.3338(3) 0.33626(9) 0.68285(13) 0.0398(5) Uani 1 1 d . . H44 H 0.364629 0.340109 0.639483 0.048 Uiso 1 1 calc R U C45 C 0.4279(3) 0.34694(9) 0.74948(13) 0.0376(5) Uani 1 1 d . . C46 C 0.3815(3) 0.33941(10) 0.81334(13) 0.0395(5) Uani 1 1 d . . H46 H 0.444484 0.345789 0.859288 0.047 Uiso 1 1 calc R U C47 C 0.2458(3) 0.32291(10) 0.80963(13) 0.0397(5) Uani 1 1 d . . H47 H 0.217062 0.317403 0.853292 0.048 Uiso 1 1 calc R U C48 C 0.5680(3) 0.36532(10) 0.75245(13) 0.0421(6) Uani 1 1 d . . C49 C -0.0383(3) 0.29230(11) 0.80314(15) 0.0471(6) Uani 1 1 d . . H49A H 0.012462 0.262260 0.830276 0.071 Uiso 1 1 calc R U H49B H -0.139797 0.284675 0.789667 0.071 Uiso 1 1 calc R U H49C H -0.020790 0.324177 0.833476 0.071 Uiso 1 1 calc R U C50 C -0.0890(3) 0.29238(12) 0.66831(15) 0.0521(7) Uani 1 1 d . . H50A H -0.084986 0.322371 0.636139 0.078 Uiso 1 1 calc R U H50B H -0.184669 0.289366 0.675509 0.078 Uiso 1 1 calc R U H50C H -0.064721 0.259685 0.646346 0.078 Uiso 1 1 calc R U 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 N1 0.0508(13) 0.0540(13) 0.0374(11) -0.0005(9) 0.0136(9) -0.0105(10) N2 0.0473(14) 0.0633(15) 0.0475(13) 0.0012(11) 0.0102(10) -0.0032(11) N3 0.0315(11) 0.0645(16) 0.0556(14) -0.0017(11) 0.0125(10) 0.0016(10) N4 0.0376(13) 0.0736(19) 0.0726(17) -0.0065(13) 0.0183(12) -0.0021(11) N5 0.0453(12) 0.0494(13) 0.0351(10) 0.0022(9) 0.0067(9) 0.0079(9) N6 0.0508(14) 0.0564(15) 0.0697(16) 0.0010(12) 0.0223(12) 0.0032(11) N7 0.0552(13) 0.0498(13) 0.0330(10) 0.0019(9) 0.0082(9) 0.0096(10) N8 0.0499(15) 0.0615(16) 0.0717(17) 0.0022(13) 0.0123(12) 0.0036(12) N9 0.0333(11) 0.0669(16) 0.0534(13) 0.0053(11) 0.0137(10) 0.0018(10) N10 0.0345(13) 0.0785(19) 0.0649(16) 0.0023(13) 0.0119(11) 0.0015(11) N11 0.0439(12) 0.0488(13) 0.0397(11) 0.0025(9) 0.0112(9) -0.0064(9) N12 0.0460(13) 0.0575(15) 0.0538(14) 0.0038(11) 0.0137(10) -0.0002(11) C1 0.0473(13) 0.0321(12) 0.0330(11) 0.0014(9) 0.0125(10) -0.0006(10) C2 0.0488(14) 0.0358(12) 0.0320(11) -0.0007(9) 0.0093(10) -0.0016(10) C3 0.0482(14) 0.0375(12) 0.0339(11) 0.0008(9) 0.0133(10) 0.0020(10) C4 0.0433(13) 0.0370(12) 0.0373(12) 0.0013(10) 0.0094(10) 0.0010(10) C5 0.0500(14) 0.0398(13) 0.0317(11) 0.0007(10) 0.0060(10) 0.0007(11) C6 0.0536(15) 0.0377(13) 0.0350(12) 0.0011(10) 0.0142(10) 0.0003(11) C7 0.0479(15) 0.0454(14) 0.0348(12) 0.0003(10) 0.0063(10) 0.0022(11) C8 0.0525(16) 0.0571(17) 0.0468(15) 0.0000(12) 0.0213(12) -0.0045(13) C9 0.0467(15) 0.0623(18) 0.0472(15) 0.0006(13) 0.0090(12) -0.0062(13) C10 0.0314(12) 0.0471(14) 0.0292(11) 0.0014(9) 0.0069(9) 0.0023(9) C11 0.0420(13) 0.0366(12) 0.0354(11) 0.0001(9) 0.0092(9) -0.0072(10) C12 0.0401(12) 0.0314(11) 0.0362(11) 0.0001(9) 0.0086(9) 0.0029(9) C13 0.0324(12) 0.0382(12) 0.0326(11) -0.0004(9) 0.0076(9) -0.0015(9) C14 0.0412(12) 0.0322(11) 0.0327(11) -0.0017(9) 0.0079(9) -0.0030(9) C15 0.0413(13) 0.0367(12) 0.0353(12) -0.0004(9) 0.0087(9) 0.0075(10) C16 0.0376(14) 0.0434(14) 0.0415(13) -0.0019(10) 0.0085(10) 0.0005(10) C17 0.0438(13) 0.0292(11) 0.0342(11) 0.0026(9) 0.0077(9) 0.0001(9) C18 0.0471(13) 0.0349(12) 0.0312(11) 0.0017(9) 0.0090(10) -0.0010(10) C19 0.0447(14) 0.0390(13) 0.0371(12) 0.0027(10) 0.0068(10) -0.0005(10) C20 0.0441(14) 0.0347(12) 0.0457(13) 0.0007(10) 0.0130(11) -0.0014(10) C21 0.0549(15) 0.0371(13) 0.0361(12) -0.0009(10) 0.0148(11) 0.0008(11) C22 0.0540(15) 0.0358(12) 0.0332(12) 0.0001(9) 0.0091(10) -0.0002(10) C23 0.0477(15) 0.0458(14) 0.0467(14) 0.0023(11) 0.0146(11) -0.0006(11) C24 0.0460(15) 0.0589(17) 0.0447(14) 0.0064(12) 0.0040(11) 0.0040(12) C25 0.0469(14) 0.0490(15) 0.0428(13) 0.0022(11) 0.0134(11) 0.0054(11) C26 0.0465(13) 0.0301(11) 0.0321(11) -0.0011(9) 0.0059(9) 0.0025(9) C27 0.0617(16) 0.0339(12) 0.0322(12) -0.0014(9) 0.0073(11) 0.0004(11) C28 0.0534(15) 0.0404(13) 0.0362(12) 0.0012(10) 0.0013(11) -0.0011(11) C29 0.0466(14) 0.0350(12) 0.0454(14) -0.0009(10) 0.0080(11) -0.0010(10) C30 0.0542(15) 0.0356(13) 0.0376(12) 0.0001(10) 0.0088(11) 0.0014(11) C31 0.0556(15) 0.0346(12) 0.0304(11) 0.0014(9) 0.0043(10) 0.0027(10) C32 0.0476(16) 0.0496(16) 0.0534(16) -0.0006(12) 0.0072(12) -0.0050(12) C33 0.0524(16) 0.0558(17) 0.0434(14) 0.0033(12) 0.0054(12) 0.0094(13) C34 0.0618(17) 0.0545(16) 0.0450(14) 0.0008(12) 0.0200(13) 0.0043(13) C35 0.0316(12) 0.0493(14) 0.0265(10) 0.0024(9) 0.0060(8) 0.0021(9) C36 0.0421(13) 0.0376(12) 0.0367(12) 0.0029(9) 0.0103(10) -0.0071(10) C37 0.0417(13) 0.0313(11) 0.0355(11) 0.0020(9) 0.0096(9) 0.0035(9) C38 0.0311(12) 0.0373(12) 0.0318(11) 0.0006(9) 0.0081(9) 0.0022(8) C39 0.0409(13) 0.0329(12) 0.0371(12) -0.0015(9) 0.0087(9) -0.0033(9) C40 0.0438(13) 0.0388(13) 0.0358(12) -0.0017(9) 0.0111(10) 0.0075(10) C41 0.0364(13) 0.0424(14) 0.0407(13) 0.0000(10) 0.0077(10) 0.0019(9) C42 0.0417(13) 0.0298(11) 0.0368(12) 0.0022(9) 0.0122(9) 0.0015(9) C43 0.0487(14) 0.0374(12) 0.0328(11) 0.0017(9) 0.0091(10) -0.0014(10) C44 0.0506(14) 0.0371(12) 0.0343(12) 0.0005(9) 0.0156(10) 0.0002(10) C45 0.0411(13) 0.0357(12) 0.0376(12) 0.0024(9) 0.0130(10) 0.0014(9) C46 0.0468(14) 0.0398(13) 0.0315(11) -0.0003(9) 0.0088(10) 0.0005(10) C47 0.0486(14) 0.0379(13) 0.0342(12) 0.0016(9) 0.0134(10) -0.0004(10) C48 0.0435(14) 0.0463(14) 0.0373(12) 0.0007(10) 0.0114(10) 0.0030(11) C49 0.0444(14) 0.0511(15) 0.0488(14) 0.0028(12) 0.0172(11) -0.0022(11) C50 0.0454(15) 0.0610(18) 0.0468(15) 0.0043(13) 0.0056(11) -0.0043(12) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 N1 C9 121.4(2) C1 N1 C8 120.7(2) C9 N1 C8 118.0(2) C10 N3 H3D 120.0 C10 N3 H3E 120.0 H3D N3 H3E 120.0 C17 N5 C25 122.3(2) C17 N5 C24 120.2(2) C25 N5 C24 117.3(2) C26 N7 C33 120.9(2) C26 N7 C34 120.7(2) C33 N7 C34 118.4(2) C35 N9 H9E 120.0 C35 N9 H9D 120.0 H9E N9 H9D 120.0 C42 N11 C49 120.9(2) C42 N11 C50 121.3(2) C49 N11 C50 117.7(2) N1 C1 C6 121.1(2) N1 C1 C2 121.3(2) C6 C1 C2 117.6(2) C3 C2 C1 120.6(2) C3 C2 H2 119.7 C1 C2 H2 119.7 C2 C3 C4 121.3(2) C2 C3 H3 119.4 C4 C3 H3 119.4 C3 C4 C5 118.8(2) C3 C4 C7 120.1(2) C5 C4 C7 121.1(2) C6 C5 C4 120.6(2) C6 C5 H5 119.7 C4 C5 H5 119.7 C5 C6 C1 121.2(2) C5 C6 H6 119.4 C1 C6 H6 119.4 N2 C7 C4 178.7(3) N1 C8 H8A 109.5 N1 C8 H8B 109.5 H8A C8 H8B 109.5 N1 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 N1 C9 H9A 109.5 N1 C9 H9B 109.5 H9A C9 H9B 109.5 N1 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 N3 C10 C15 121.0(2) N3 C10 C11 121.1(2) C15 C10 C11 118.0(2) C12 C11 C10 120.8(2) C12 C11 H11 119.6 C10 C11 H11 119.6 C11 C12 C13 120.3(2) C11 C12 H12 119.8 C13 C12 H12 119.8 C14 C13 C12 119.2(2) C14 C13 C16 120.6(2) C12 C13 C16 120.2(2) C15 C14 C13 120.7(2) C15 C14 H14 119.7 C13 C14 H14 119.7 C14 C15 C10 121.0(2) C14 C15 H15 119.5 C10 C15 H15 119.5 N4 C16 C13 179.6(3) N5 C17 C22 121.6(2) N5 C17 C18 121.1(2) C22 C17 C18 117.3(2) C19 C18 C17 120.5(2) C19 C18 H18 119.7 C17 C18 H18 119.7 C18 C19 C20 121.3(2) C18 C19 H19 119.3 C20 C19 H19 119.3 C19 C20 C21 118.3(2) C19 C20 C23 121.0(2) C21 C20 C23 120.7(2) C22 C21 C20 120.9(2) C22 C21 H21 119.6 C20 C21 H21 119.6 C21 C22 C17 121.6(2) C21 C22 H22 119.2 C17 C22 H22 119.2 N6 C23 C20 179.1(3) N5 C24 H24A 109.5 N5 C24 H24B 109.5 H24A C24 H24B 109.5 N5 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 N5 C25 H25A 109.5 N5 C25 H25B 109.5 H25A C25 H25B 109.5 N5 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 N7 C26 C27 121.7(2) N7 C26 C31 121.4(2) C27 C26 C31 117.0(2) C28 C27 C26 121.5(2) C28 C27 H27 119.2 C26 C27 H27 119.2 C27 C28 C29 120.8(2) C27 C28 H28 119.6 C29 C28 H28 119.6 C28 C29 C30 118.5(2) C28 C29 C32 120.8(2) C30 C29 C32 120.7(2) C31 C30 C29 121.2(2) C31 C30 H30 119.4 C29 C30 H30 119.4 C30 C31 C26 120.9(2) C30 C31 H31 119.5 C26 C31 H31 119.5 N8 C32 C29 178.8(3) N7 C33 H33A 109.5 N7 C33 H33B 109.5 H33A C33 H33B 109.5 N7 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 N7 C34 H34A 109.5 N7 C34 H34B 109.5 H34A C34 H34B 109.5 N7 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 N9 C35 C40 120.8(2) N9 C35 C36 120.9(2) C40 C35 C36 118.3(2) C37 C36 C35 120.7(2) C37 C36 H36 119.6 C35 C36 H36 119.6 C36 C37 C38 120.6(2) C36 C37 H37 119.7 C38 C37 H37 119.7 C37 C38 C39 119.1(2) C37 C38 C41 120.6(2) C39 C38 C41 120.3(2) C40 C39 C38 120.4(2) C40 C39 H39 119.8 C38 C39 H39 119.8 C39 C40 C35 120.9(2) C39 C40 H40 119.6 C35 C40 H40 119.6 N10 C41 C38 178.8(3) N11 C42 C47 121.8(2) N11 C42 C43 121.0(2) C47 C42 C43 117.2(2) C44 C43 C42 120.9(2) C44 C43 H43 119.6 C42 C43 H43 119.6 C43 C44 C45 121.5(2) C43 C44 H44 119.3 C45 C44 H44 119.3 C44 C45 C46 118.4(2) C44 C45 C48 120.5(2) C46 C45 C48 121.1(2) C47 C46 C45 120.5(2) C47 C46 H46 119.8 C45 C46 H46 119.8 C46 C47 C42 121.5(2) C46 C47 H47 119.3 C42 C47 H47 119.3 N12 C48 C45 178.4(3) N11 C49 H49A 109.5 N11 C49 H49B 109.5 H49A C49 H49B 109.5 N11 C49 H49C 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 N11 C50 H50A 109.5 N11 C50 H50B 109.5 H50A C50 H50B 109.5 N11 C50 H50C 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1 1.361(3) N1 C9 1.451(3) N1 C8 1.453(3) N2 C7 1.142(3) N3 C10 1.357(3) N3 H3D 0.8800 N3 H3E 0.8800 N4 C16 1.144(3) N5 C17 1.364(3) N5 C25 1.449(3) N5 C24 1.453(3) N6 C23 1.142(3) N7 C26 1.357(3) N7 C33 1.447(3) N7 C34 1.454(3) N8 C32 1.145(4) N9 C35 1.361(3) N9 H9E 0.8800 N9 H9D 0.8800 N10 C41 1.147(3) N11 C42 1.362(3) N11 C49 1.451(3) N11 C50 1.455(3) N12 C48 1.145(3) C1 C6 1.416(3) C1 C2 1.420(3) C2 C3 1.374(3) C2 H2 0.9500 C3 C4 1.399(3) C3 H3 0.9500 C4 C5 1.400(3) C4 C7 1.438(4) C5 C6 1.378(4) C5 H5 0.9500 C6 H6 0.9500 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 C15 1.404(3) C10 C11 1.408(3) C11 C12 1.378(3) C11 H11 0.9500 C12 C13 1.398(3) C12 H12 0.9500 C13 C14 1.391(3) C13 C16 1.442(3) C14 C15 1.372(3) C14 H14 0.9500 C15 H15 0.9500 C17 C22 1.414(3) C17 C18 1.423(3) C18 C19 1.372(3) C18 H18 0.9500 C19 C20 1.403(3) C19 H19 0.9500 C20 C21 1.403(4) C20 C23 1.437(4) C21 C22 1.365(4) C21 H21 0.9500 C22 H22 0.9500 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 C27 1.416(3) C26 C31 1.424(3) C27 C28 1.369(4) C27 H27 0.9500 C28 C29 1.399(4) C28 H28 0.9500 C29 C30 1.404(4) C29 C32 1.433(4) C30 C31 1.366(4) C30 H30 0.9500 C31 H31 0.9500 C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 C40 1.401(3) C35 C36 1.404(3) C36 C37 1.376(3) C36 H36 0.9500 C37 C38 1.392(3) C37 H37 0.9500 C38 C39 1.398(3) C38 C41 1.439(3) C39 C40 1.375(3) C39 H39 0.9500 C40 H40 0.9500 C42 C47 1.414(3) C42 C43 1.421(3) C43 C44 1.369(3) C43 H43 0.9500 C44 C45 1.396(3) C44 H44 0.9500 C45 C46 1.409(3) C45 C48 1.432(3) C46 C47 1.374(3) C46 H46 0.9500 C47 H47 0.9500 C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 0.9800 C50 H50A 0.9800 C50 H50B 0.9800 C50 H50C 0.9800 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 C9 N1 C1 C6 -178.8(2) C8 N1 C1 C6 2.7(4) C9 N1 C1 C2 0.3(4) C8 N1 C1 C2 -178.2(2) N1 C1 C2 C3 -177.7(2) C6 C1 C2 C3 1.4(3) C1 C2 C3 C4 0.4(4) C2 C3 C4 C5 -1.6(4) C2 C3 C4 C7 178.7(2) C3 C4 C5 C6 1.0(4) C7 C4 C5 C6 -179.3(2) C4 C5 C6 C1 0.8(4) N1 C1 C6 C5 177.1(2) C2 C1 C6 C5 -2.0(4) N3 C10 C11 C12 179.8(2) C15 C10 C11 C12 -1.0(3) C10 C11 C12 C13 0.2(3) C11 C12 C13 C14 0.7(3) C11 C12 C13 C16 -178.1(2) C12 C13 C14 C15 -0.8(3) C16 C13 C14 C15 178.0(2) C13 C14 C15 C10 0.0(4) N3 C10 C15 C14 -179.8(2) C11 C10 C15 C14 0.9(3) C25 N5 C17 C22 174.5(2) C24 N5 C17 C22 0.0(4) C25 N5 C17 C18 -7.2(4) C24 N5 C17 C18 178.4(2) N5 C17 C18 C19 -174.7(2) C22 C17 C18 C19 3.7(3) C17 C18 C19 C20 -1.2(4) C18 C19 C20 C21 -2.1(4) C18 C19 C20 C23 177.8(2) C19 C20 C21 C22 3.0(4) C23 C20 C21 C22 -176.9(2) C20 C21 C22 C17 -0.4(4) N5 C17 C22 C21 175.5(2) C18 C17 C22 C21 -2.9(4) C33 N7 C26 C27 -176.7(2) C34 N7 C26 C27 5.8(4) C33 N7 C26 C31 2.4(4) C34 N7 C26 C31 -175.1(2) N7 C26 C27 C28 176.1(2) C31 C26 C27 C28 -3.1(4) C26 C27 C28 C29 0.9(4) C27 C28 C29 C30 2.2(4) C27 C28 C29 C32 -178.1(2) C28 C29 C30 C31 -3.0(4) C32 C29 C30 C31 177.3(2) C29 C30 C31 C26 0.7(4) N7 C26 C31 C30 -176.9(2) C27 C26 C31 C30 2.3(4) N9 C35 C36 C37 -179.6(2) C40 C35 C36 C37 1.3(3) C35 C36 C37 C38 -0.9(4) C36 C37 C38 C39 0.1(3) C36 C37 C38 C41 178.7(2) C37 C38 C39 C40 0.3(3) C41 C38 C39 C40 -178.3(2) C38 C39 C40 C35 0.2(4) N9 C35 C40 C39 180.0(2) C36 C35 C40 C39 -1.0(3) C49 N11 C42 C47 -3.9(4) C50 N11 C42 C47 179.2(2) C49 N11 C42 C43 177.5(2) C50 N11 C42 C43 0.7(4) N11 C42 C43 C44 176.5(2) C47 C42 C43 C44 -2.1(3) C42 C43 C44 C45 -0.3(4) C43 C44 C45 C46 1.9(4) C43 C44 C45 C48 -177.8(2) C44 C45 C46 C47 -1.2(4) C48 C45 C46 C47 178.5(2) C45 C46 C47 C42 -1.2(4) N11 C42 C47 C46 -175.8(2) C43 C42 C47 C46 2.8(4)