#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:28:56 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287241 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247657.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_7247657 loop_ _publ_author_name 'Saito, Erika' 'Yamakado, Ryohei' 'Yasuhara, Taichi' 'Yamaguchi, Hiroto' 'Okada, Shuji' 'Yoshida, Tsukasa' _publ_section_title ; Formation of charge-transfer complexes in ionic crystals composed of 1,3-bis(dicyanomethylidene)indan anion and viologens bearing alkyl chains ; _journal_issue 45 _journal_name_full 'RSC Advances' _journal_page_first 32039 _journal_page_last 32044 _journal_paper_doi 10.1039/D3RA06782C _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C20 H30 N2, 2(C15 H5 N4)' _chemical_formula_sum 'C50 H40 N10' _chemical_formula_weight 780.92 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-06-09 deposited with the CCDC. 2023-10-26 downloaded from the CCDC. ; _cell_angle_alpha 68.229(2) _cell_angle_beta 75.915(2) _cell_angle_gamma 85.545(2) _cell_formula_units_Z 2 _cell_length_a 11.2406(2) _cell_length_b 13.7520(3) _cell_length_c 14.5481(3) _cell_measurement_reflns_used 11029 _cell_measurement_temperature 150 _cell_measurement_theta_max 30.3400 _cell_measurement_theta_min 2.2020 _cell_volume 2025.47(8) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'Yadokari-XG (Wakita, Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Rigaku Saturn 70 CCD area detector' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 28031 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 1.549 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'Dark blue' _exptl_crystal_density_diffrn 1.280 _exptl_crystal_description Platelet _exptl_crystal_F_000 820 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.560 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 549 _refine_ls_number_reflns 9221 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0637 _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^)+(0.1036P)^2^+0.4669P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1632 _refine_ls_wR_factor_ref 0.1921 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6763 _reflns_number_total 9221 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra06782c2.cif _cod_data_source_block 20190317_PnV_-123 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7247657 _shelx_shelxl_version_number 2018/3 _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 0.988 _shelx_estimated_absorpt_t_max 0.997 _oxdiff_exptl_absorpt_empirical_full_min 0.908 _oxdiff_exptl_absorpt_empirical_full_max 1.078 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _shelx_res_file ; TITL 20190317_PnV_-123_a.res in P-1 20190317_PnV_-123.res created by SHELXL-2018/3 at 15:48:29 on 20-Mar-2019 REM Yadorkari-X generated CELL 0.71073 11.2406 13.7520 14.5481 68.2290 75.9150 85.5450 ZERR 2.0 0.0002 0.0003 0.0003 0.0020 0.0020 0.0020 LATT 1 REM SPGR P-1 triclinic SFAC C H N UNIT 100 80 20 SIZE 0.16 0.14 0.04 TEMP -123.0 L.S. 50 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H OMIT -10.000000 55.000000 OMIT 0 1 1 OMIT 0 2 0 OMIT 0 -1 1 OMIT 1 0 1 OMIT 1 0 0 OMIT 1 2 1 OMIT -1 0 1 OMIT 1 1 1 WGHT 0.103600 0.466900 FVAR 6.46753 N1 3 0.624117 0.443202 -0.178796 11.00000 0.06477 0.04015 = 0.04731 -0.02361 -0.02526 0.01107 N2 3 0.535419 0.694575 -0.448782 11.00000 0.05287 0.07447 = 0.03350 -0.01925 -0.01822 0.00397 N3 3 0.723078 0.587509 0.101474 11.00000 0.05845 0.02974 = 0.03566 -0.01080 -0.01978 0.00892 N4 3 0.637265 0.922577 0.041611 11.00000 0.05835 0.03205 = 0.05078 -0.02079 -0.02350 0.00873 N5 3 0.697876 0.211396 0.043452 11.00000 0.02808 0.02577 = 0.02936 -0.00975 -0.00608 0.00038 N6 3 0.784131 0.308833 0.465136 11.00000 0.03093 0.02791 = 0.02789 -0.00993 -0.00727 0.00119 N7 3 0.784917 -0.071177 0.398098 11.00000 0.06321 0.03317 = 0.03719 -0.01136 -0.02136 0.01221 N8 3 0.876325 -0.404619 0.445333 11.00000 0.05296 0.03350 = 0.04552 -0.01991 -0.01771 0.00462 N9 3 0.866751 0.059454 0.690664 11.00000 0.05684 0.03796 = 0.04857 -0.01974 -0.02217 0.00399 N10 3 0.970280 -0.202799 0.951033 11.00000 0.05094 0.05743 = 0.03785 -0.01855 -0.01632 -0.00508 C1 1 0.629283 0.677730 -0.131300 11.00000 0.03086 0.02801 = 0.02706 -0.01002 -0.00948 0.00626 H1 2 0.648976 0.604396 -0.088284 11.00000 -1.20000 C2 1 0.600483 0.706591 -0.226124 11.00000 0.02492 0.03263 = 0.02680 -0.01075 -0.00656 0.00574 C3 1 0.577858 0.820987 -0.261660 11.00000 0.02448 0.03144 = 0.02674 -0.00596 -0.00631 0.00283 C4 1 0.547663 0.889724 -0.349831 11.00000 0.03285 0.04392 = 0.02999 -0.00742 -0.00927 0.00440 AFIX 43 H4 2 0.542644 0.866761 -0.402851 11.00000 -1.20000 AFIX 0 C5 1 0.524679 0.994194 -0.358765 11.00000 0.04201 0.03728 = 0.03708 0.00366 -0.01478 0.00092 AFIX 43 H5 2 0.503179 1.042513 -0.418421 11.00000 -1.20000 AFIX 0 C6 1 0.532892 1.027785 -0.281936 11.00000 0.04335 0.02619 = 0.04870 -0.00119 -0.01627 0.00279 AFIX 43 H6 2 0.514589 1.098398 -0.288767 11.00000 -1.20000 AFIX 0 C7 1 0.567889 0.959192 -0.193814 11.00000 0.03525 0.02624 = 0.04009 -0.00563 -0.01075 0.00035 AFIX 43 H7 2 0.576147 0.983056 -0.142165 11.00000 -1.20000 AFIX 0 C8 1 0.589922 0.856027 -0.184544 11.00000 0.02524 0.02660 = 0.03058 -0.00579 -0.00657 0.00187 C9 1 0.625571 0.764488 -0.102141 11.00000 0.02464 0.02553 = 0.02610 -0.00695 -0.00645 0.00263 C10 1 0.590677 0.638374 -0.275021 11.00000 0.03034 0.03855 = 0.02888 -0.01483 -0.01024 0.00730 C11 1 0.609047 0.529545 -0.223752 11.00000 0.03796 0.04231 = 0.03434 -0.02230 -0.01467 0.00865 C12 1 0.561020 0.669128 -0.371494 11.00000 0.03213 0.04630 = 0.03365 -0.01728 -0.00933 0.00382 C13 1 0.652377 0.763464 -0.013355 11.00000 0.03109 0.02293 = 0.02963 -0.00935 -0.01001 0.00379 C14 1 0.691548 0.667446 0.052725 11.00000 0.03846 0.02808 = 0.02673 -0.01202 -0.01118 0.00377 C15 1 0.645283 0.851998 0.015900 11.00000 0.03425 0.02801 = 0.03541 -0.01153 -0.01349 0.00496 C16 1 0.700126 0.310766 0.039840 11.00000 0.04862 0.02501 = 0.03105 -0.00770 -0.01307 0.00265 AFIX 43 H16 2 0.688075 0.367227 -0.019083 11.00000 -1.20000 AFIX 0 C17 1 0.719786 0.330895 0.121049 11.00000 0.04899 0.02317 = 0.03253 -0.00934 -0.01234 0.00303 AFIX 43 H17 2 0.721176 0.401163 0.117595 11.00000 -1.20000 AFIX 0 C18 1 0.737715 0.248811 0.208520 11.00000 0.02553 0.02490 = 0.02560 -0.00863 -0.00427 0.00237 C19 1 0.738081 0.147000 0.208097 11.00000 0.02872 0.02423 = 0.02909 -0.00744 -0.00563 0.00303 AFIX 43 H19 2 0.752633 0.089074 0.264962 11.00000 -1.20000 AFIX 0 C20 1 0.717316 0.130902 0.125128 11.00000 0.02814 0.02539 = 0.03058 -0.00938 -0.00533 0.00370 AFIX 43 H20 2 0.716781 0.061564 0.125881 11.00000 -1.20000 AFIX 0 C21 1 0.770470 0.389036 0.380409 11.00000 0.03329 0.02340 = 0.03132 -0.00895 -0.00655 0.00256 AFIX 43 H21 2 0.771725 0.458844 0.378273 11.00000 -1.20000 AFIX 0 C22 1 0.754702 0.371373 0.296785 11.00000 0.03077 0.02358 = 0.02800 -0.00700 -0.00553 0.00298 AFIX 43 H22 2 0.744520 0.428817 0.237911 11.00000 -1.20000 AFIX 0 C23 1 0.753658 0.269041 0.298409 11.00000 0.02506 0.02418 = 0.02674 -0.00791 -0.00404 0.00232 C24 1 0.767907 0.187754 0.387248 11.00000 0.04213 0.02362 = 0.02969 -0.00783 -0.01071 0.00377 AFIX 43 H24 2 0.767398 0.117222 0.391312 11.00000 -1.20000 AFIX 0 C25 1 0.782732 0.209271 0.469234 11.00000 0.04158 0.02552 = 0.03018 -0.00727 -0.00976 0.00293 AFIX 43 H25 2 0.792080 0.153230 0.529376 11.00000 -1.20000 AFIX 0 C26 1 0.674144 0.192321 -0.045188 11.00000 0.03174 0.03335 = 0.03074 -0.01324 -0.01058 0.00082 AFIX 23 H26 2 0.607474 0.238337 -0.069910 11.00000 -1.20000 H26A 2 0.646863 0.118766 -0.023234 11.00000 -1.20000 AFIX 0 C27 1 0.788270 0.213470 -0.131102 11.00000 0.04008 0.03317 = 0.03354 -0.01265 -0.01063 0.00360 AFIX 23 H27 2 0.765891 0.210365 -0.191710 11.00000 -1.20000 H27A 2 0.818567 0.285355 -0.148844 11.00000 -1.20000 AFIX 0 C28 1 0.891181 0.137350 -0.106202 11.00000 0.03684 0.03208 = 0.03265 -0.01412 -0.00971 0.00531 AFIX 23 H28 2 0.865755 0.067254 -0.099519 11.00000 -1.20000 H28A 2 0.904604 0.131838 -0.039675 11.00000 -1.20000 AFIX 0 C29 1 1.011725 0.168957 -0.185838 11.00000 0.03829 0.03209 = 0.03870 -0.01423 -0.00512 0.00097 AFIX 23 H29 2 0.998012 0.178135 -0.253246 11.00000 -1.20000 H29A 2 1.040439 0.236935 -0.189722 11.00000 -1.20000 AFIX 0 C30 1 1.109621 0.087759 -0.160927 11.00000 0.04123 0.03556 = 0.04193 -0.01460 -0.00828 0.00263 AFIX 137 H30 2 1.123508 0.078589 -0.094275 11.00000 -1.50000 H30A 2 1.186045 0.111146 -0.212973 11.00000 -1.50000 H30B 2 1.082678 0.020982 -0.159407 11.00000 -1.50000 AFIX 0 C31 1 0.802299 0.332654 0.553153 11.00000 0.03632 0.03577 = 0.03022 -0.01456 -0.01209 -0.00006 AFIX 23 H31 2 0.875167 0.378986 0.530722 11.00000 -1.20000 H31A 2 0.817693 0.266797 0.607065 11.00000 -1.20000 AFIX 0 C32 1 0.689877 0.386025 0.596533 11.00000 0.04235 0.03334 = 0.03439 -0.01621 -0.00876 -0.00042 AFIX 23 H32 2 0.709433 0.408411 0.648551 11.00000 -1.20000 H32A 2 0.672570 0.449725 0.541187 11.00000 -1.20000 AFIX 0 C33 1 0.575036 0.317064 0.644331 11.00000 0.04038 0.03770 = 0.03182 -0.01384 -0.01054 -0.00068 AFIX 23 H33 2 0.583944 0.264057 0.710355 11.00000 -1.20000 H33A 2 0.568031 0.279352 0.599607 11.00000 -1.20000 AFIX 0 C34 1 0.456487 0.377531 0.662010 11.00000 0.04204 0.04540 = 0.04144 -0.01919 -0.00592 -0.00280 AFIX 23 H34 2 0.460865 0.412170 0.709855 11.00000 -1.20000 H34A 2 0.448729 0.432711 0.596765 11.00000 -1.20000 AFIX 0 C35 1 0.344406 0.306287 0.704822 11.00000 0.04320 0.05365 = 0.04078 -0.01717 -0.00929 -0.00360 AFIX 137 H35 2 0.339384 0.272346 0.657343 11.00000 -1.50000 H35A 2 0.270602 0.347635 0.714450 11.00000 -1.50000 H35B 2 0.350682 0.252767 0.770386 11.00000 -1.50000 AFIX 0 C36 1 0.882177 -0.168345 0.627859 11.00000 0.03239 0.02668 = 0.02772 -0.00979 -0.00965 0.00435 H36 2 0.862373 -0.094006 0.588103 11.00000 -1.20000 C37 1 0.886082 -0.253445 0.595919 11.00000 0.02342 0.02533 = 0.02966 -0.00893 -0.00652 0.00304 C38 1 0.919430 -0.347007 0.677480 11.00000 0.02468 0.02511 = 0.02970 -0.00650 -0.00632 0.00167 C39 1 0.938002 -0.450192 0.685133 11.00000 0.03167 0.02556 = 0.03959 -0.00846 -0.01066 0.00158 AFIX 43 H39 2 0.929989 -0.471931 0.632075 11.00000 -1.20000 AFIX 0 C40 1 0.969004 -0.521725 0.773542 11.00000 0.03811 0.02454 = 0.04857 -0.00320 -0.01253 0.00049 AFIX 43 H40 2 0.984647 -0.592377 0.779260 11.00000 -1.20000 AFIX 0 C41 1 0.977239 -0.491613 0.852297 11.00000 0.03642 0.03421 = 0.03767 0.00195 -0.01177 0.00169 AFIX 43 H41 2 0.995860 -0.542050 0.912214 11.00000 -1.20000 AFIX 0 C42 1 0.958316 -0.386953 0.844637 11.00000 0.03283 0.03862 = 0.02995 -0.00646 -0.01032 0.00308 AFIX 43 H42 2 0.964087 -0.365978 0.898717 11.00000 -1.20000 AFIX 0 C43 1 0.931095 -0.315096 0.756636 11.00000 0.02437 0.02783 = 0.02842 -0.00688 -0.00721 0.00149 C44 1 0.909442 -0.200517 0.723628 11.00000 0.02421 0.02993 = 0.03033 -0.01155 -0.00613 0.00319 C45 1 0.860096 -0.248947 0.505495 11.00000 0.03192 0.02269 = 0.02947 -0.00948 -0.00959 0.00387 C46 1 0.819575 -0.151705 0.442748 11.00000 0.04025 0.03146 = 0.02822 -0.01297 -0.01023 0.00419 C47 1 0.867858 -0.335172 0.472729 11.00000 0.03513 0.02861 = 0.03282 -0.01157 -0.01273 0.00462 C48 1 0.915637 -0.135182 0.776645 11.00000 0.03033 0.03391 = 0.02953 -0.01288 -0.00907 0.00173 C49 1 0.889864 -0.026638 0.731082 11.00000 0.03582 0.03704 = 0.03388 -0.01695 -0.01048 0.00058 C50 1 0.945128 -0.171523 0.873201 11.00000 0.03205 0.04107 = 0.03439 -0.01631 -0.00765 -0.00214 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 20190317_PnV_-123_a.res in P-1 REM wR2 = 0.1921, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0637 for 6763 Fo > 4sig(Fo) and 0.0838 for all 9221 data REM 549 parameters refined using 0 restraints END WGHT 0.1036 0.4669 REM Highest difference peak 0.560, deepest hole -0.291, 1-sigma level 0.060 Q1 1 0.7966 0.1206 -0.0913 11.00000 0.05 0.56 Q2 1 0.9162 0.1973 -0.1496 11.00000 0.05 0.40 Q3 1 1.0467 0.1148 -0.1598 11.00000 0.05 0.37 Q4 1 0.7160 0.2853 0.6331 11.00000 0.05 0.37 Q5 1 0.4936 0.3214 0.6989 11.00000 0.05 0.35 Q6 1 0.3811 0.4147 0.6590 11.00000 0.05 0.32 Q7 1 0.6164 0.3574 0.5981 11.00000 0.05 0.29 Q8 1 1.1563 0.1886 -0.1998 11.00000 0.05 0.28 Q9 1 0.9029 -0.3990 0.6892 11.00000 0.05 0.28 Q10 1 0.8994 -0.2994 0.6308 11.00000 0.05 0.26 Q11 1 0.9147 -0.3363 0.7266 11.00000 0.05 0.24 Q12 1 0.7684 0.3441 0.4356 11.00000 0.05 0.22 Q13 1 0.7971 0.2023 0.4347 11.00000 0.05 0.22 Q14 1 0.5837 0.9858 -0.2397 11.00000 0.05 0.21 Q15 1 0.9265 -0.4988 0.7535 11.00000 0.05 0.20 Q16 1 0.7552 0.2847 0.1580 11.00000 0.05 0.20 Q17 1 0.6326 0.3574 -0.1304 11.00000 0.05 0.20 Q18 1 0.6854 0.3149 0.0927 11.00000 0.05 0.20 Q19 1 0.9029 -0.1988 0.6000 11.00000 0.05 0.19 Q20 1 0.9466 -0.4354 0.8587 11.00000 0.05 0.19 ; _shelx_res_checksum 72927 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.62412(17) 0.44320(13) -0.17880(13) 0.0468(4) Uani 1 1 d . . . . . N2 N 0.53542(16) 0.69458(16) -0.44878(12) 0.0524(5) Uani 1 1 d . . . . . N3 N 0.72308(16) 0.58751(11) 0.10147(11) 0.0404(4) Uani 1 1 d . . . . . N4 N 0.63727(16) 0.92258(12) 0.04161(12) 0.0438(4) Uani 1 1 d . . . . . N5 N 0.69788(12) 0.21140(10) 0.04345(10) 0.0279(3) Uani 1 1 d . . . . . N6 N 0.78413(12) 0.30883(10) 0.46514(10) 0.0289(3) Uani 1 1 d . . . . . N7 N 0.78492(16) -0.07118(12) 0.39810(12) 0.0438(4) Uani 1 1 d . . . . . N8 N 0.87633(15) -0.40462(12) 0.44533(12) 0.0414(4) Uani 1 1 d . . . . . N9 N 0.86675(16) 0.05945(13) 0.69066(13) 0.0450(4) Uani 1 1 d . . . . . N10 N 0.97028(16) -0.20280(14) 0.95103(12) 0.0469(4) Uani 1 1 d . . . . . C1 C 0.62928(15) 0.67773(13) -0.13130(12) 0.0285(3) Uani 1 1 d . . . . . H1 H 0.6490(16) 0.6044(15) -0.0883(13) 0.034 Uiso 1 1 d . U . . . C2 C 0.60048(14) 0.70659(13) -0.22612(12) 0.0283(3) Uani 1 1 d . . . . . C3 C 0.57786(14) 0.82099(13) -0.26166(12) 0.0290(3) Uani 1 1 d . . . . . C4 C 0.54766(16) 0.88972(15) -0.34983(13) 0.0372(4) Uani 1 1 d . . . . . H4 H 0.542644 0.866761 -0.402851 0.045 Uiso 1 1 calc R U . . . C5 C 0.52468(17) 0.99419(15) -0.35877(14) 0.0428(5) Uani 1 1 d . . . . . H5 H 0.503179 1.042513 -0.418421 0.051 Uiso 1 1 calc R U . . . C6 C 0.53289(17) 1.02779(14) -0.28194(15) 0.0422(4) Uani 1 1 d . . . . . H6 H 0.514589 1.098398 -0.288767 0.051 Uiso 1 1 calc R U . . . C7 C 0.56789(16) 0.95919(13) -0.19381(14) 0.0354(4) Uani 1 1 d . . . . . H7 H 0.576147 0.983056 -0.142165 0.042 Uiso 1 1 calc R U . . . C8 C 0.58992(14) 0.85603(12) -0.18454(12) 0.0289(3) Uani 1 1 d . . . . . C9 C 0.62557(14) 0.76449(12) -0.10214(11) 0.0262(3) Uani 1 1 d . . . . . C10 C 0.59068(15) 0.63837(14) -0.27502(12) 0.0316(4) Uani 1 1 d . . . . . C11 C 0.60905(16) 0.52954(14) -0.22375(13) 0.0350(4) Uani 1 1 d . . . . . C12 C 0.56102(16) 0.66913(15) -0.37149(13) 0.0364(4) Uani 1 1 d . . . . . C13 C 0.65238(14) 0.76346(12) -0.01335(12) 0.0276(3) Uani 1 1 d . . . . . C14 C 0.69155(16) 0.66745(12) 0.05273(12) 0.0300(4) Uani 1 1 d . . . . . C15 C 0.64528(15) 0.85200(13) 0.01590(13) 0.0318(4) Uani 1 1 d . . . . . C16 C 0.70013(17) 0.31077(13) 0.03984(13) 0.0350(4) Uani 1 1 d . . . . . H16 H 0.688075 0.367227 -0.019083 0.042 Uiso 1 1 calc R U . . . C17 C 0.71979(17) 0.33089(13) 0.12105(13) 0.0347(4) Uani 1 1 d . . . . . H17 H 0.721176 0.401163 0.117595 0.042 Uiso 1 1 calc R U . . . C18 C 0.73771(14) 0.24881(12) 0.20852(11) 0.0259(3) Uani 1 1 d . . . . . C19 C 0.73808(14) 0.14700(12) 0.20810(12) 0.0284(3) Uani 1 1 d . . . . . H19 H 0.752633 0.089074 0.264962 0.034 Uiso 1 1 calc R U . . . C20 C 0.71732(14) 0.13090(12) 0.12513(12) 0.0287(3) Uani 1 1 d . . . . . H20 H 0.716781 0.061564 0.125881 0.034 Uiso 1 1 calc R U . . . C21 C 0.77047(15) 0.38904(12) 0.38041(12) 0.0299(3) Uani 1 1 d . . . . . H21 H 0.771725 0.458844 0.378273 0.036 Uiso 1 1 calc R U . . . C22 C 0.75470(14) 0.37137(12) 0.29678(12) 0.0285(3) Uani 1 1 d . . . . . H22 H 0.744520 0.428817 0.237911 0.034 Uiso 1 1 calc R U . . . C23 C 0.75366(14) 0.26904(12) 0.29841(11) 0.0262(3) Uani 1 1 d . . . . . C24 C 0.76791(16) 0.18775(12) 0.38725(12) 0.0321(4) Uani 1 1 d . . . . . H24 H 0.767398 0.117222 0.391312 0.039 Uiso 1 1 calc R U . . . C25 C 0.78273(16) 0.20927(13) 0.46923(13) 0.0331(4) Uani 1 1 d . . . . . H25 H 0.792080 0.153230 0.529376 0.040 Uiso 1 1 calc R U . . . C26 C 0.67414(15) 0.19232(13) -0.04519(12) 0.0309(4) Uani 1 1 d . . . . . H26 H 0.607474 0.238337 -0.069910 0.037 Uiso 1 1 calc R U . . . H26A H 0.646863 0.118766 -0.023234 0.037 Uiso 1 1 calc R U . . . C27 C 0.78827(16) 0.21347(13) -0.13110(12) 0.0352(4) Uani 1 1 d . . . . . H27 H 0.765891 0.210365 -0.191710 0.042 Uiso 1 1 calc R U . . . H27A H 0.818567 0.285355 -0.148844 0.042 Uiso 1 1 calc R U . . . C28 C 0.89118(15) 0.13735(13) -0.10620(12) 0.0331(4) Uani 1 1 d . . . . . H28 H 0.865755 0.067254 -0.099519 0.040 Uiso 1 1 calc R U . . . H28A H 0.904604 0.131838 -0.039675 0.040 Uiso 1 1 calc R U . . . C29 C 1.01172(16) 0.16896(13) -0.18584(13) 0.0367(4) Uani 1 1 d . . . . . H29 H 0.998012 0.178135 -0.253246 0.044 Uiso 1 1 calc R U . . . H29A H 1.040439 0.236935 -0.189722 0.044 Uiso 1 1 calc R U . . . C30 C 1.10962(17) 0.08776(14) -0.16093(14) 0.0398(4) Uani 1 1 d . . . . . H30 H 1.123508 0.078589 -0.094275 0.060 Uiso 1 1 calc R U . . . H30A H 1.186045 0.111146 -0.212973 0.060 Uiso 1 1 calc R U . . . H30B H 1.082678 0.020982 -0.159407 0.060 Uiso 1 1 calc R U . . . C31 C 0.80230(16) 0.33265(14) 0.55315(12) 0.0325(4) Uani 1 1 d . . . . . H31 H 0.875167 0.378986 0.530722 0.039 Uiso 1 1 calc R U . . . H31A H 0.817693 0.266797 0.607065 0.039 Uiso 1 1 calc R U . . . C32 C 0.68988(16) 0.38602(13) 0.59653(13) 0.0355(4) Uani 1 1 d . . . . . H32 H 0.709433 0.408411 0.648551 0.043 Uiso 1 1 calc R U . . . H32A H 0.672570 0.449725 0.541187 0.043 Uiso 1 1 calc R U . . . C33 C 0.57504(16) 0.31706(14) 0.64433(13) 0.0358(4) Uani 1 1 d . . . . . H33 H 0.583944 0.264057 0.710355 0.043 Uiso 1 1 calc R U . . . H33A H 0.568031 0.279352 0.599607 0.043 Uiso 1 1 calc R U . . . C34 C 0.45649(17) 0.37753(15) 0.66201(14) 0.0425(4) Uani 1 1 d . . . . . H34 H 0.460865 0.412170 0.709855 0.051 Uiso 1 1 calc R U . . . H34A H 0.448729 0.432711 0.596765 0.051 Uiso 1 1 calc R U . . . C35 C 0.34441(18) 0.30629(16) 0.70482(14) 0.0457(5) Uani 1 1 d . . . . . H35 H 0.339384 0.272346 0.657343 0.069 Uiso 1 1 calc R U . . . H35A H 0.270602 0.347635 0.714450 0.069 Uiso 1 1 calc R U . . . H35B H 0.350682 0.252767 0.770386 0.069 Uiso 1 1 calc R U . . . C36 C 0.88218(15) -0.16835(13) 0.62786(12) 0.0287(3) Uani 1 1 d . . . . . H36 H 0.8624(16) -0.0940(15) 0.5881(13) 0.034 Uiso 1 1 d . U . . . C37 C 0.88608(14) -0.25344(12) 0.59592(12) 0.0265(3) Uani 1 1 d . . . . . C38 C 0.91943(14) -0.34701(12) 0.67748(12) 0.0276(3) Uani 1 1 d . . . . . C39 C 0.93800(15) -0.45019(13) 0.68513(13) 0.0329(4) Uani 1 1 d . . . . . H39 H 0.929989 -0.471931 0.632075 0.039 Uiso 1 1 calc R U . . . C40 C 0.96900(17) -0.52172(13) 0.77354(14) 0.0396(4) Uani 1 1 d . . . . . H40 H 0.984647 -0.592377 0.779260 0.048 Uiso 1 1 calc R U . . . C41 C 0.97724(16) -0.49161(14) 0.85230(14) 0.0400(4) Uani 1 1 d . . . . . H41 H 0.995860 -0.542050 0.912214 0.048 Uiso 1 1 calc R U . . . C42 C 0.95832(16) -0.38695(14) 0.84464(13) 0.0352(4) Uani 1 1 d . . . . . H42 H 0.964087 -0.365978 0.898717 0.042 Uiso 1 1 calc R U . . . C43 C 0.93109(14) -0.31510(12) 0.75664(12) 0.0277(3) Uani 1 1 d . . . . . C44 C 0.90944(14) -0.20052(12) 0.72363(12) 0.0282(3) Uani 1 1 d . . . . . C45 C 0.86010(15) -0.24895(12) 0.50549(12) 0.0278(3) Uani 1 1 d . . . . . C46 C 0.81958(16) -0.15171(13) 0.44275(12) 0.0325(4) Uani 1 1 d . . . . . C47 C 0.86786(15) -0.33517(13) 0.47273(12) 0.0314(4) Uani 1 1 d . . . . . C48 C 0.91564(15) -0.13518(13) 0.77665(12) 0.0305(4) Uani 1 1 d . . . . . C49 C 0.88986(16) -0.02664(14) 0.73108(13) 0.0339(4) Uani 1 1 d . . . . . C50 C 0.94513(16) -0.17152(14) 0.87320(13) 0.0349(4) Uani 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 N1 0.0648(11) 0.0401(9) 0.0473(9) -0.0236(8) -0.0253(8) 0.0111(8) N2 0.0529(10) 0.0745(13) 0.0335(8) -0.0192(8) -0.0182(7) 0.0040(9) N3 0.0585(10) 0.0297(8) 0.0357(8) -0.0108(6) -0.0198(7) 0.0089(7) N4 0.0584(10) 0.0321(8) 0.0508(9) -0.0208(7) -0.0235(8) 0.0087(7) N5 0.0281(7) 0.0258(7) 0.0294(7) -0.0097(5) -0.0061(5) 0.0004(5) N6 0.0309(7) 0.0279(7) 0.0279(7) -0.0099(5) -0.0073(5) 0.0012(5) N7 0.0632(11) 0.0332(8) 0.0372(8) -0.0114(7) -0.0214(8) 0.0122(7) N8 0.0530(10) 0.0335(8) 0.0455(9) -0.0199(7) -0.0177(7) 0.0046(7) N9 0.0568(10) 0.0380(9) 0.0486(9) -0.0197(7) -0.0222(8) 0.0040(8) N10 0.0509(10) 0.0574(10) 0.0379(9) -0.0185(8) -0.0163(7) -0.0051(8) C1 0.0309(8) 0.0280(8) 0.0271(8) -0.0100(6) -0.0095(6) 0.0063(6) C2 0.0249(8) 0.0326(8) 0.0268(8) -0.0108(6) -0.0066(6) 0.0057(6) C3 0.0245(8) 0.0314(8) 0.0267(8) -0.0060(6) -0.0063(6) 0.0028(6) C4 0.0329(9) 0.0439(10) 0.0300(9) -0.0074(7) -0.0093(7) 0.0044(7) C5 0.0420(10) 0.0373(10) 0.0371(10) 0.0037(8) -0.0148(8) 0.0009(8) C6 0.0434(10) 0.0262(8) 0.0487(11) -0.0012(8) -0.0163(8) 0.0028(7) C7 0.0353(9) 0.0262(8) 0.0401(9) -0.0056(7) -0.0107(7) 0.0003(7) C8 0.0252(8) 0.0266(8) 0.0306(8) -0.0058(6) -0.0066(6) 0.0019(6) C9 0.0246(7) 0.0255(7) 0.0261(7) -0.0069(6) -0.0064(6) 0.0026(6) C10 0.0303(8) 0.0386(9) 0.0289(8) -0.0148(7) -0.0102(6) 0.0073(7) C11 0.0380(9) 0.0423(10) 0.0343(9) -0.0223(8) -0.0147(7) 0.0086(8) C12 0.0321(9) 0.0463(10) 0.0336(9) -0.0173(8) -0.0093(7) 0.0038(8) C13 0.0311(8) 0.0229(7) 0.0296(8) -0.0093(6) -0.0100(6) 0.0038(6) C14 0.0385(9) 0.0281(8) 0.0267(8) -0.0120(6) -0.0112(7) 0.0038(7) C15 0.0342(9) 0.0280(8) 0.0354(9) -0.0115(7) -0.0135(7) 0.0050(7) C16 0.0486(10) 0.0250(8) 0.0310(8) -0.0077(7) -0.0131(7) 0.0026(7) C17 0.0490(10) 0.0232(8) 0.0325(9) -0.0093(7) -0.0123(7) 0.0030(7) C18 0.0255(8) 0.0249(7) 0.0256(8) -0.0086(6) -0.0043(6) 0.0024(6) C19 0.0287(8) 0.0242(7) 0.0291(8) -0.0074(6) -0.0056(6) 0.0030(6) C20 0.0281(8) 0.0254(7) 0.0306(8) -0.0094(6) -0.0053(6) 0.0037(6) C21 0.0333(8) 0.0234(7) 0.0313(8) -0.0090(6) -0.0065(7) 0.0026(6) C22 0.0308(8) 0.0236(7) 0.0280(8) -0.0070(6) -0.0055(6) 0.0030(6) C23 0.0251(8) 0.0242(7) 0.0267(8) -0.0079(6) -0.0040(6) 0.0023(6) C24 0.0421(9) 0.0236(7) 0.0297(8) -0.0078(6) -0.0107(7) 0.0038(7) C25 0.0416(10) 0.0255(8) 0.0302(8) -0.0073(6) -0.0098(7) 0.0029(7) C26 0.0317(8) 0.0333(8) 0.0307(8) -0.0132(7) -0.0106(7) 0.0008(7) C27 0.0401(9) 0.0332(9) 0.0335(9) -0.0127(7) -0.0106(7) 0.0036(7) C28 0.0368(9) 0.0321(8) 0.0327(8) -0.0141(7) -0.0097(7) 0.0053(7) C29 0.0383(9) 0.0321(9) 0.0387(9) -0.0142(7) -0.0051(7) 0.0010(7) C30 0.0412(10) 0.0356(9) 0.0419(10) -0.0146(8) -0.0083(8) 0.0026(8) C31 0.0363(9) 0.0358(9) 0.0302(8) -0.0146(7) -0.0121(7) -0.0001(7) C32 0.0424(10) 0.0333(9) 0.0344(9) -0.0162(7) -0.0088(7) -0.0004(7) C33 0.0404(10) 0.0377(9) 0.0318(9) -0.0138(7) -0.0105(7) -0.0007(8) C34 0.0420(10) 0.0454(11) 0.0414(10) -0.0192(8) -0.0059(8) -0.0028(8) C35 0.0432(11) 0.0536(12) 0.0408(10) -0.0172(9) -0.0093(8) -0.0036(9) C36 0.0324(8) 0.0267(8) 0.0277(8) -0.0098(6) -0.0097(6) 0.0043(6) C37 0.0234(7) 0.0253(7) 0.0297(8) -0.0089(6) -0.0065(6) 0.0030(6) C38 0.0247(8) 0.0251(8) 0.0297(8) -0.0065(6) -0.0063(6) 0.0017(6) C39 0.0317(9) 0.0256(8) 0.0396(9) -0.0085(7) -0.0107(7) 0.0016(7) C40 0.0381(10) 0.0245(8) 0.0486(11) -0.0032(7) -0.0125(8) 0.0005(7) C41 0.0364(10) 0.0342(9) 0.0377(9) 0.0019(7) -0.0118(7) 0.0017(7) C42 0.0328(9) 0.0386(9) 0.0300(8) -0.0065(7) -0.0103(7) 0.0031(7) C43 0.0244(8) 0.0278(8) 0.0284(8) -0.0069(6) -0.0072(6) 0.0015(6) C44 0.0242(8) 0.0299(8) 0.0303(8) -0.0116(6) -0.0061(6) 0.0032(6) C45 0.0319(8) 0.0227(7) 0.0295(8) -0.0095(6) -0.0096(6) 0.0039(6) C46 0.0402(9) 0.0315(8) 0.0282(8) -0.0130(7) -0.0102(7) 0.0042(7) C47 0.0351(9) 0.0286(8) 0.0328(8) -0.0116(7) -0.0127(7) 0.0046(7) C48 0.0303(8) 0.0339(8) 0.0295(8) -0.0129(7) -0.0091(6) 0.0017(7) C49 0.0358(9) 0.0370(9) 0.0339(9) -0.0170(7) -0.0105(7) 0.0006(7) C50 0.0320(9) 0.0411(10) 0.0344(9) -0.0163(8) -0.0077(7) -0.0021(7) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 N5 C16 120.56(14) . . ? C20 N5 C26 120.39(13) . . ? C16 N5 C26 119.05(13) . . ? C21 N6 C25 120.15(14) . . ? C21 N6 C31 118.75(13) . . ? C25 N6 C31 121.10(13) . . ? C2 C1 C9 110.82(14) . . ? C2 C1 H1 125.4(10) . . ? C9 C1 H1 123.8(10) . . ? C10 C2 C1 125.49(15) . . ? C10 C2 C3 127.17(15) . . ? C1 C2 C3 107.30(14) . . ? C4 C3 C8 120.87(16) . . ? C4 C3 C2 131.74(16) . . ? C8 C3 C2 107.38(13) . . ? C3 C4 C5 118.21(17) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 120.89(16) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.13(17) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 118.08(17) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C7 C8 C3 120.76(15) . . ? C7 C8 C9 131.70(16) . . ? C3 C8 C9 107.54(13) . . ? C13 C9 C1 125.57(14) . . ? C13 C9 C8 127.51(14) . . ? C1 C9 C8 106.91(13) . . ? C2 C10 C12 124.72(16) . . ? C2 C10 C11 117.77(14) . . ? C12 C10 C11 117.50(15) . . ? N1 C11 C10 176.86(18) . . ? N2 C12 C10 178.9(2) . . ? C9 C13 C15 124.64(14) . . ? C9 C13 C14 118.04(14) . . ? C15 C13 C14 117.32(14) . . ? N3 C14 C13 175.75(17) . . ? N4 C15 C13 178.3(2) . . ? N5 C16 C17 120.47(15) . . ? N5 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.63(15) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 117.11(14) . . ? C17 C18 C23 121.21(14) . . ? C19 C18 C23 121.68(14) . . ? C20 C19 C18 120.03(14) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? N5 C20 C19 121.17(14) . . ? N5 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? N6 C21 C22 121.05(14) . . ? N6 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 120.18(14) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 117.38(14) . . ? C24 C23 C18 121.83(14) . . ? C22 C23 C18 120.79(14) . . ? C25 C24 C23 120.35(15) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? N6 C25 C24 120.89(15) . . ? N6 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? N5 C26 C27 111.27(13) . . ? N5 C26 H26 109.4 . . ? C27 C26 H26 109.4 . . ? N5 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? H26 C26 H26A 108.0 . . ? C28 C27 C26 113.96(14) . . ? C28 C27 H27 108.8 . . ? C26 C27 H27 108.8 . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? H27 C27 H27A 107.7 . . ? C27 C28 C29 113.55(14) . . ? C27 C28 H28 108.9 . . ? C29 C28 H28 108.9 . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? H28 C28 H28A 107.7 . . ? C30 C29 C28 111.70(14) . . ? C30 C29 H29 109.3 . . ? C28 C29 H29 109.3 . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? H29 C29 H29A 107.9 . . ? C29 C30 H30 109.5 . . ? C29 C30 H30A 109.5 . . ? H30 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C31 C32 111.32(13) . . ? N6 C31 H31 109.4 . . ? C32 C31 H31 109.4 . . ? N6 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? H31 C31 H31A 108.0 . . ? C33 C32 C31 114.04(14) . . ? C33 C32 H32 108.7 . . ? C31 C32 H32 108.7 . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32A 108.7 . . ? H32 C32 H32A 107.6 . . ? C32 C33 C34 113.84(15) . . ? C32 C33 H33 108.8 . . ? C34 C33 H33 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? H33 C33 H33A 107.7 . . ? C35 C34 C33 111.79(16) . . ? C35 C34 H34 109.3 . . ? C33 C34 H34 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? H34 C34 H34A 107.9 . . ? C34 C35 H35 109.5 . . ? C34 C35 H35A 109.5 . . ? H35 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C44 C36 C37 110.66(14) . . ? C44 C36 H36 124.0(10) . . ? C37 C36 H36 125.3(10) . . ? C45 C37 C36 125.32(14) . . ? C45 C37 C38 127.70(14) . . ? C36 C37 C38 106.96(13) . . ? C39 C38 C43 120.78(15) . . ? C39 C38 C37 131.57(15) . . ? C43 C38 C37 107.66(13) . . ? C38 C39 C40 118.08(17) . . ? C38 C39 H39 121.0 . . ? C40 C39 H39 121.0 . . ? C41 C40 C39 121.39(16) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C40 C41 C42 120.54(16) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 118.57(17) . . ? C43 C42 H42 120.7 . . ? C41 C42 H42 120.7 . . ? C42 C43 C38 120.59(15) . . ? C42 C43 C44 132.06(16) . . ? C38 C43 C44 107.35(13) . . ? C48 C44 C36 125.46(15) . . ? C48 C44 C43 127.20(15) . . ? C36 C44 C43 107.34(14) . . ? C37 C45 C47 124.70(14) . . ? C37 C45 C46 117.63(14) . . ? C47 C45 C46 117.65(14) . . ? N7 C46 C45 175.10(18) . . ? N8 C47 C45 178.78(19) . . ? C44 C48 C50 123.28(16) . . ? C44 C48 C49 117.97(15) . . ? C50 C48 C49 118.74(15) . . ? N9 C49 C48 176.32(19) . . ? N10 C50 C48 178.5(2) . . ? 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 N1 C11 1.146(2) . ? N2 C12 1.149(2) . ? N3 C14 1.149(2) . ? N4 C15 1.153(2) . ? N5 C20 1.3409(19) . ? N5 C16 1.350(2) . ? N5 C26 1.494(2) . ? N6 C21 1.348(2) . ? N6 C25 1.349(2) . ? N6 C31 1.496(2) . ? N7 C46 1.150(2) . ? N8 C47 1.153(2) . ? N9 C49 1.151(2) . ? N10 C50 1.150(2) . ? C1 C2 1.399(2) . ? C1 C9 1.402(2) . ? C1 H1 1.011(19) . ? C2 C10 1.396(2) . ? C2 C3 1.485(2) . ? C3 C4 1.384(2) . ? C3 C8 1.412(2) . ? C4 C5 1.403(3) . ? C4 H4 0.9500 . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 C7 1.407(2) . ? C6 H6 0.9500 . ? C7 C8 1.383(2) . ? C7 H7 0.9500 . ? C8 C9 1.489(2) . ? C9 C13 1.391(2) . ? C10 C12 1.423(2) . ? C10 C11 1.427(2) . ? C13 C15 1.422(2) . ? C13 C14 1.427(2) . ? C16 C17 1.379(2) . ? C16 H16 0.9500 . ? C17 C18 1.399(2) . ? C17 H17 0.9500 . ? C18 C19 1.402(2) . ? C18 C23 1.487(2) . ? C19 C20 1.380(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.379(2) . ? C21 H21 0.9500 . ? C22 C23 1.400(2) . ? C22 H22 0.9500 . ? C23 C24 1.395(2) . ? C24 C25 1.380(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.517(2) . ? C26 H26 0.9900 . ? C26 H26A 0.9900 . ? C27 C28 1.516(2) . ? C27 H27 0.9900 . ? C27 H27A 0.9900 . ? C28 C29 1.523(2) . ? C28 H28 0.9900 . ? C28 H28A 0.9900 . ? C29 C30 1.514(2) . ? C29 H29 0.9900 . ? C29 H29A 0.9900 . ? C30 H30 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.531(2) . ? C31 H31 0.9900 . ? C31 H31A 0.9900 . ? C32 C33 1.521(2) . ? C32 H32 0.9900 . ? C32 H32A 0.9900 . ? C33 C34 1.534(3) . ? C33 H33 0.9900 . ? C33 H33A 0.9900 . ? C34 C35 1.514(3) . ? C34 H34 0.9900 . ? C34 H34A 0.9900 . ? C35 H35 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C44 1.400(2) . ? C36 C37 1.405(2) . ? C36 H36 1.009(19) . ? C37 C45 1.394(2) . ? C37 C38 1.488(2) . ? C38 C39 1.385(2) . ? C38 C43 1.412(2) . ? C39 C40 1.403(2) . ? C39 H39 0.9500 . ? C40 C41 1.379(3) . ? C40 H40 0.9500 . ? C41 C42 1.405(3) . ? C41 H41 0.9500 . ? C42 C43 1.384(2) . ? C42 H42 0.9500 . ? C43 C44 1.486(2) . ? C44 C48 1.399(2) . ? C45 C47 1.423(2) . ? C45 C46 1.425(2) . ? C48 C50 1.419(2) . ? C48 C49 1.430(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C10 -177.03(15) . . . . ? C9 C1 C2 C3 0.72(18) . . . . ? C10 C2 C3 C4 -3.1(3) . . . . ? C1 C2 C3 C4 179.24(17) . . . . ? C10 C2 C3 C8 175.71(15) . . . . ? C1 C2 C3 C8 -1.99(17) . . . . ? C8 C3 C4 C5 -2.5(2) . . . . ? C2 C3 C4 C5 176.18(16) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C4 C5 C6 C7 1.8(3) . . . . ? C5 C6 C7 C8 -2.1(3) . . . . ? C6 C7 C8 C3 0.2(2) . . . . ? C6 C7 C8 C9 -178.81(16) . . . . ? C4 C3 C8 C7 2.1(2) . . . . ? C2 C3 C8 C7 -176.78(14) . . . . ? C4 C3 C8 C9 -178.65(14) . . . . ? C2 C3 C8 C9 2.42(17) . . . . ? C2 C1 C9 C13 -178.35(15) . . . . ? C2 C1 C9 C8 0.76(18) . . . . ? C7 C8 C9 C13 -3.8(3) . . . . ? C3 C8 C9 C13 177.07(15) . . . . ? C7 C8 C9 C1 177.07(17) . . . . ? C3 C8 C9 C1 -2.02(17) . . . . ? C1 C2 C10 C12 179.87(16) . . . . ? C3 C2 C10 C12 2.6(3) . . . . ? C1 C2 C10 C11 1.3(2) . . . . ? C3 C2 C10 C11 -176.00(15) . . . . ? C1 C9 C13 C15 -178.47(16) . . . . ? C8 C9 C13 C15 2.6(3) . . . . ? C1 C9 C13 C14 2.5(2) . . . . ? C8 C9 C13 C14 -176.44(15) . . . . ? C20 N5 C16 C17 -1.4(2) . . . . ? C26 N5 C16 C17 178.93(15) . . . . ? N5 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C19 1.7(2) . . . . ? C16 C17 C18 C23 -177.33(15) . . . . ? C17 C18 C19 C20 -2.1(2) . . . . ? C23 C18 C19 C20 176.98(14) . . . . ? C16 N5 C20 C19 1.1(2) . . . . ? C26 N5 C20 C19 -179.31(14) . . . . ? C18 C19 C20 N5 0.7(2) . . . . ? C25 N6 C21 C22 0.1(2) . . . . ? C31 N6 C21 C22 179.34(14) . . . . ? N6 C21 C22 C23 -0.5(2) . . . . ? C21 C22 C23 C24 0.6(2) . . . . ? C21 C22 C23 C18 -179.52(14) . . . . ? C17 C18 C23 C24 178.03(14) . . . . ? C19 C18 C23 C24 -1.0(2) . . . . ? C17 C18 C23 C22 -1.9(2) . . . . ? C19 C18 C23 C22 179.12(14) . . . . ? C22 C23 C24 C25 -0.2(2) . . . . ? C18 C23 C24 C25 179.88(15) . . . . ? C21 N6 C25 C24 0.3(2) . . . . ? C31 N6 C25 C24 -178.95(15) . . . . ? C23 C24 C25 N6 -0.2(3) . . . . ? C20 N5 C26 C27 -101.04(17) . . . . ? C16 N5 C26 C27 78.60(18) . . . . ? N5 C26 C27 C28 66.87(18) . . . . ? C26 C27 C28 C29 -170.91(14) . . . . ? C27 C28 C29 C30 -176.76(14) . . . . ? C21 N6 C31 C32 63.67(19) . . . . ? C25 N6 C31 C32 -117.10(17) . . . . ? N6 C31 C32 C33 65.51(18) . . . . ? C31 C32 C33 C34 -164.74(14) . . . . ? C32 C33 C34 C35 177.20(15) . . . . ? C44 C36 C37 C45 178.09(15) . . . . ? C44 C36 C37 C38 -0.47(18) . . . . ? C45 C37 C38 C39 2.8(3) . . . . ? C36 C37 C38 C39 -178.73(17) . . . . ? C45 C37 C38 C43 -176.97(15) . . . . ? C36 C37 C38 C43 1.54(17) . . . . ? C43 C38 C39 C40 -0.2(2) . . . . ? C37 C38 C39 C40 -179.88(16) . . . . ? C38 C39 C40 C41 2.0(3) . . . . ? C39 C40 C41 C42 -2.0(3) . . . . ? C40 C41 C42 C43 0.1(3) . . . . ? C41 C42 C43 C38 1.7(2) . . . . ? C41 C42 C43 C44 -178.24(16) . . . . ? C39 C38 C43 C42 -1.6(2) . . . . ? C37 C38 C43 C42 178.12(14) . . . . ? C39 C38 C43 C44 178.28(14) . . . . ? C37 C38 C43 C44 -1.96(17) . . . . ? C37 C36 C44 C48 178.79(15) . . . . ? C37 C36 C44 C43 -0.73(18) . . . . ? C42 C43 C44 C48 2.1(3) . . . . ? C38 C43 C44 C48 -177.81(15) . . . . ? C42 C43 C44 C36 -178.40(17) . . . . ? C38 C43 C44 C36 1.69(17) . . . . ? C36 C37 C45 C47 178.09(16) . . . . ? C38 C37 C45 C47 -3.7(3) . . . . ? C36 C37 C45 C46 -3.7(2) . . . . ? C38 C37 C45 C46 174.52(15) . . . . ? C36 C44 C48 C50 -179.23(16) . . . . ? C43 C44 C48 C50 0.2(3) . . . . ? C36 C44 C48 C49 1.3(2) . . . . ? C43 C44 C48 C49 -179.28(15) . . . . ?