#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:30:10 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253835 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557828.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_1557828 loop_ _publ_author_name 'Guo, Chenxing' 'Wang, Hu' 'Lynch, Vincent M.' 'Ji, Xiaofan' 'Page, Zachariah A.' 'Sessler, Jonathan L.' _publ_section_title ; Molecular recognition of pyrazine N,N′-dioxide using aryl extended calix[4]pyrroles ; _journal_issue 22 _journal_name_full 'Chemical Science' _journal_page_first 5650 _journal_paper_doi 10.1039/D0SC01496F _journal_volume 11 _journal_year 2020 _chemical_formula_moiety '2 C38 H38 N6 O4, C4 H4 N2 O2, 2 C H4 O' _chemical_formula_sum 'C82 H88 N14 O12' _chemical_formula_weight 1461.66 _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 _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-02-20 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 104.398(2) _cell_angle_beta 102.401(2) _cell_angle_gamma 109.792(2) _cell_formula_units_Z 1 _cell_length_a 10.5727(5) _cell_length_b 12.9980(5) _cell_length_c 15.4783(8) _cell_measurement_reflns_used 4258 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.6 _cell_measurement_theta_min 3.05 _cell_volume 1831.32(15) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material 'XP SHELXTL/PC, Siemens Analytical' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_structure_solution ; SHELXT. (2015). G. M. Sheldrick. ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Rigaku AFC12 with a Saturn 724+ CCD' _diffrn_measurement_method \w-scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 34417 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.529 _diffrn_reflns_theta_min 3.048 _diffrn_source 'sealed fine focus tube' _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_description prism _exptl_crystal_F_000 774 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.247 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 522 _refine_ls_number_reflns 8391 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0474 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.8273P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0999 _refine_ls_wR_factor_ref 0.1102 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6389 _reflns_number_total 8391 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01496f3.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 1557828--1557833.cif.' _cod_original_cell_volume 1831.31(15) _cod_database_code 1557828 _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 0.969 _shelx_estimated_absorpt_t_max 0.995 _shelx_res_file ; TITL shelxt_a.res in P-1 37 sec 0.5 deg saturn shelx.res created by SHELXL-2016/6 at 10:50:45 on 23-Feb-2018 CELL 0.71073 10.5727 12.9980 15.4783 104.398 102.401 109.792 ZERR 1.00 0.0005 0.0005 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 82 88 14 12 MERG 2 EQIV $2 -x, -y+1, -z+1 HTAB C37 O1_$2 HTAB C39 N4 HTAB N4 O6 EQIV $1 -x+1, -y+2, -z+2 HTAB C40 N3_$1 HTAB N2 O6 HTAB N1 N7 HTAB N1 O5 HTAB N3 O6 FMAP 2 PLAN 20 SIZE 0.050 0.100 0.350 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -173.00 WGHT 0.037400 0.827300 FVAR 0.29282 C1 1 0.124827 0.568844 0.750513 11.00000 0.01423 0.01643 = 0.01728 0.00514 0.00623 0.00641 C2 1 0.082868 0.520161 0.653460 11.00000 0.01789 0.01707 = 0.01641 0.00345 0.00598 0.00645 AFIX 43 H2 2 0.061621 0.441845 0.617970 11.00000 -1.20000 AFIX 0 C3 1 0.077283 0.609222 0.616226 11.00000 0.01659 0.02237 = 0.01475 0.00602 0.00465 0.00745 AFIX 43 H3 2 0.051935 0.601020 0.551381 11.00000 -1.20000 AFIX 0 C4 1 0.115280 0.709067 0.691325 11.00000 0.01458 0.01926 = 0.01815 0.00789 0.00741 0.00789 C5 1 0.135276 0.832198 0.696777 11.00000 0.01819 0.01887 = 0.02072 0.00802 0.00876 0.00885 C6 1 0.292041 0.912676 0.735319 11.00000 0.01927 0.01797 = 0.01821 0.00843 0.00844 0.00998 C7 1 0.361943 1.026789 0.793696 11.00000 0.02414 0.02005 = 0.01959 0.00704 0.00900 0.01198 AFIX 43 H7 2 0.320349 1.073065 0.823993 11.00000 -1.20000 AFIX 0 C8 1 0.507699 1.063937 0.801052 11.00000 0.02113 0.01680 = 0.02010 0.00531 0.00484 0.00516 AFIX 43 H8 2 0.580865 1.139525 0.837141 11.00000 -1.20000 AFIX 0 C9 1 0.524439 0.971456 0.746852 11.00000 0.01820 0.01902 = 0.01651 0.00817 0.00584 0.00703 C10 1 0.657731 0.961675 0.732301 11.00000 0.01696 0.02176 = 0.01920 0.00791 0.00725 0.00744 C11 1 0.719867 0.911047 0.799767 11.00000 0.01659 0.01736 = 0.01613 0.00444 0.00733 0.00594 C12 1 0.850737 0.958129 0.867269 11.00000 0.01755 0.01744 = 0.01804 0.00330 0.00536 0.00429 AFIX 43 H12 2 0.924374 1.032757 0.881799 11.00000 -1.20000 AFIX 0 C13 1 0.857468 0.876092 0.911889 11.00000 0.01654 0.02062 = 0.01566 0.00299 0.00244 0.00649 AFIX 43 H13 2 0.936463 0.886062 0.961310 11.00000 -1.20000 AFIX 0 C14 1 0.729741 0.779825 0.871054 11.00000 0.01607 0.01703 = 0.01367 0.00260 0.00449 0.00795 C15 1 0.682549 0.665488 0.889733 11.00000 0.01679 0.01663 = 0.01469 0.00430 0.00440 0.00746 C16 1 0.545263 0.637788 0.913273 11.00000 0.01757 0.01649 = 0.01475 0.00502 0.00479 0.00828 C17 1 0.523062 0.652007 0.998772 11.00000 0.02098 0.01980 = 0.01463 0.00517 0.00396 0.00831 AFIX 43 H17 2 0.594507 0.681553 1.058632 11.00000 -1.20000 AFIX 0 C18 1 0.374156 0.614706 0.982032 11.00000 0.02325 0.01945 = 0.01561 0.00672 0.00915 0.00973 AFIX 43 H18 2 0.328874 0.615816 1.028828 11.00000 -1.20000 AFIX 0 C19 1 0.307518 0.576885 0.886505 11.00000 0.01831 0.01440 = 0.01608 0.00545 0.00700 0.00726 C20 1 0.151280 0.518302 0.827182 11.00000 0.01806 0.01653 = 0.01654 0.00613 0.00680 0.00733 C21 1 0.062454 0.879026 0.764320 11.00000 0.02474 0.02093 = 0.02646 0.01034 0.01418 0.01289 AFIX 137 H21A 2 0.105936 0.881231 0.827790 11.00000 -1.50000 H21B 2 -0.039236 0.827545 0.741354 11.00000 -1.50000 H21C 2 0.074625 0.957907 0.766516 11.00000 -1.50000 AFIX 0 C22 1 0.768106 1.085140 0.751789 11.00000 0.02130 0.03006 = 0.03542 0.01895 0.01017 0.00906 AFIX 137 H22A 2 0.728931 1.119282 0.708980 11.00000 -1.50000 H22B 2 0.854714 1.080772 0.741501 11.00000 -1.50000 H22C 2 0.790965 1.133993 0.817299 11.00000 -1.50000 AFIX 0 C23 1 0.625809 0.885696 0.629549 11.00000 0.02575 0.03739 = 0.01948 0.01215 0.01138 0.01618 AFIX 137 H23A 2 0.556778 0.806333 0.616439 11.00000 -1.50000 H23B 2 0.713963 0.883320 0.620720 11.00000 -1.50000 H23C 2 0.586414 0.919184 0.586235 11.00000 -1.50000 AFIX 0 C24 1 0.800125 0.677477 0.975421 11.00000 0.02160 0.02221 = 0.01846 0.00672 0.00412 0.00988 AFIX 137 H24A 2 0.888859 0.692063 0.960730 11.00000 -1.50000 H24B 2 0.771116 0.605216 0.989577 11.00000 -1.50000 H24C 2 0.814987 0.742758 1.030313 11.00000 -1.50000 AFIX 0 C25 1 0.061070 0.535260 0.891210 11.00000 0.01979 0.02736 = 0.02145 0.01129 0.00977 0.01038 AFIX 137 H25A 2 0.090470 0.618844 0.923325 11.00000 -1.50000 H25B 2 0.075132 0.498256 0.938280 11.00000 -1.50000 H25C 2 -0.039695 0.499452 0.852700 11.00000 -1.50000 AFIX 0 C26 1 0.109283 0.386900 0.780844 11.00000 0.02451 0.01707 = 0.02261 0.00636 0.00546 0.00684 AFIX 137 H26A 2 0.008669 0.348397 0.741776 11.00000 -1.50000 H26B 2 0.124628 0.353092 0.830021 11.00000 -1.50000 H26C 2 0.167812 0.375549 0.741233 11.00000 -1.50000 AFIX 0 C27 1 0.064239 0.830765 0.598450 11.00000 0.01948 0.01768 = 0.02408 0.00957 0.01006 0.01108 C28 1 -0.083562 0.770688 0.556161 11.00000 0.01953 0.02909 = 0.03083 0.01820 0.01116 0.00971 AFIX 43 H28 2 -0.137308 0.726938 0.586813 11.00000 -1.20000 AFIX 0 C29 1 -0.153118 0.773517 0.470899 11.00000 0.01677 0.02748 = 0.03288 0.01531 0.00768 0.00913 AFIX 43 H29 2 -0.253687 0.733816 0.443558 11.00000 -1.20000 AFIX 0 C30 1 -0.072678 0.835601 0.426326 11.00000 0.02179 0.01605 = 0.02187 0.00777 0.00733 0.01039 C31 1 0.073709 0.893505 0.464261 11.00000 0.02286 0.02019 = 0.02210 0.00861 0.01096 0.00826 AFIX 43 H31 2 0.127140 0.934195 0.431822 11.00000 -1.20000 AFIX 0 C32 1 0.141109 0.891092 0.550542 11.00000 0.01770 0.02135 = 0.02198 0.00720 0.00811 0.00824 AFIX 43 H32 2 0.241668 0.931341 0.577562 11.00000 -1.20000 AFIX 0 C33 1 0.671644 0.565004 0.805902 11.00000 0.01520 0.01949 = 0.01498 0.00478 0.00273 0.00958 C34 1 0.756019 0.589514 0.748975 11.00000 0.01596 0.01922 = 0.02185 0.00601 0.00619 0.00698 AFIX 43 H34 2 0.813247 0.668505 0.759224 11.00000 -1.20000 AFIX 0 C35 1 0.758173 0.501444 0.678037 11.00000 0.01845 0.02337 = 0.01940 0.00602 0.00736 0.01056 AFIX 43 H35 2 0.815316 0.519009 0.639481 11.00000 -1.20000 AFIX 0 C36 1 0.674548 0.387083 0.665036 11.00000 0.02044 0.02065 = 0.01636 0.00239 0.00320 0.01251 C37 1 0.591265 0.358388 0.720617 11.00000 0.02149 0.01758 = 0.02229 0.00362 0.00506 0.00838 AFIX 43 H37 2 0.536692 0.279107 0.711185 11.00000 -1.20000 AFIX 0 C38 1 0.589315 0.448247 0.790556 11.00000 0.02000 0.01939 = 0.02047 0.00789 0.00782 0.00853 AFIX 43 H38 2 0.531218 0.430043 0.828444 11.00000 -1.20000 AFIX 0 C39 1 0.468394 0.886376 0.956810 11.00000 0.02922 0.01612 = 0.01769 0.00448 0.01081 0.01161 C40 1 0.397692 1.031363 1.021083 11.00000 0.02792 0.01869 = 0.01582 0.00319 0.00926 0.01207 C41 1 0.417672 0.542985 0.581197 11.00000 0.03346 0.03361 = 0.02304 0.00316 0.00987 0.01583 AFIX 137 H41A 2 0.507211 0.588467 0.573771 11.00000 -1.50000 H41B 2 0.339485 0.514978 0.522000 11.00000 -1.50000 H41C 2 0.424334 0.476161 0.597107 11.00000 -1.50000 AFIX 0 N1 3 0.144047 0.683291 0.772227 11.00000 0.01843 0.01537 = 0.01559 0.00478 0.00718 0.00724 N2 3 0.392129 0.879022 0.707510 11.00000 0.01791 0.01554 = 0.01945 0.00389 0.00770 0.00721 N3 3 0.646278 0.801904 0.802339 11.00000 0.01479 0.01630 = 0.01437 0.00273 0.00345 0.00553 N4 3 0.413256 0.592384 0.845216 11.00000 0.01788 0.01969 = 0.01132 0.00455 0.00563 0.00867 N5 3 -0.146214 0.838125 0.335410 11.00000 0.02351 0.02064 = 0.02622 0.01020 0.00812 0.01192 N6 3 0.675433 0.292543 0.589080 11.00000 0.02510 0.02518 = 0.02029 0.00336 0.00428 0.01442 N7 3 0.364767 0.916876 0.977670 11.00000 0.02409 0.01694 = 0.01541 0.00374 0.00878 0.00792 O1 4 -0.276432 0.785276 0.302980 11.00000 0.02114 0.03797 = 0.03824 0.01838 0.00266 0.00917 O2 4 -0.074127 0.891053 0.295153 11.00000 0.03057 0.03593 = 0.03135 0.02123 0.01373 0.01563 O3 4 0.730684 0.319127 0.530946 11.00000 0.03502 0.03506 = 0.02851 0.00265 0.01760 0.01450 O4 4 0.619516 0.192047 0.587168 11.00000 0.05338 0.02216 = 0.02697 0.00434 0.00994 0.01867 O5 4 0.236080 0.837907 0.956917 11.00000 0.02542 0.01973 = 0.02096 0.00237 0.01012 0.00465 O6 4 0.391413 0.614919 0.655115 11.00000 0.01770 0.03224 = 0.01696 0.00226 0.00601 0.00732 H39 2 0.442901 0.806666 0.929128 11.00000 0.02066 H4N 2 0.397673 0.578838 0.784928 11.00000 0.02763 H40 2 0.322713 1.049242 1.032467 11.00000 0.02466 H2N 2 0.373784 0.810630 0.667652 11.00000 0.03386 H1N 2 0.172622 0.734733 0.831391 11.00000 0.03854 H3N 2 0.557569 0.751232 0.763482 11.00000 0.04026 H6O 2 0.299650 0.595550 0.641546 11.00000 0.05547 HKLF 4 REM shelxt_a.res in P-1 37 sec 0.5 deg saturn REM R1 = 0.0474 for 6389 Fo > 4sig(Fo) and 0.0690 for all 8391 data REM 522 parameters refined using 0 restraints END WGHT 0.0374 0.8300 REM Highest difference peak 0.247, deepest hole -0.280, 1-sigma level 0.050 Q1 1 0.0916 0.5616 0.6346 11.00000 0.05 0.25 Q2 1 0.2042 0.8637 0.7111 11.00000 0.05 0.24 Q3 1 0.1033 0.8340 0.6533 11.00000 0.05 0.24 Q4 1 0.4996 0.5214 0.6117 11.00000 0.05 0.24 Q5 1 0.6737 0.6177 0.8510 11.00000 0.05 0.24 Q6 1 0.6565 0.9217 0.6871 11.00000 0.05 0.23 Q7 1 0.1418 0.5417 0.7868 11.00000 0.05 0.23 Q8 1 0.1355 0.5467 0.7045 11.00000 0.05 0.23 Q9 1 0.1249 0.7744 0.6922 11.00000 0.05 0.22 Q10 1 0.6056 0.6439 0.8961 11.00000 0.05 0.22 Q11 1 0.1049 0.5201 0.8523 11.00000 0.05 0.21 Q12 1 0.6794 0.7829 0.8370 11.00000 0.05 0.21 Q13 1 0.6839 0.9236 0.7586 11.00000 0.05 0.21 Q14 1 0.1044 0.8396 0.5688 11.00000 0.05 0.21 Q15 1 0.3220 0.9853 0.7419 11.00000 0.05 0.21 Q16 1 0.7839 0.8276 0.9137 11.00000 0.05 0.20 Q17 1 0.3862 0.5742 0.5195 11.00000 0.05 0.20 Q18 1 0.1383 0.4556 0.8099 11.00000 0.05 0.20 Q19 1 0.8154 0.8160 0.8792 11.00000 0.05 0.20 Q20 1 -0.1187 0.7410 0.4968 11.00000 0.05 0.20 ; _shelx_res_checksum 35893 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 C1 C 0.12483(16) 0.56884(13) 0.75051(11) 0.0159(3) Uani 1 1 d . . . . . C2 C 0.08287(17) 0.52016(14) 0.65346(11) 0.0178(3) Uani 1 1 d . . . . . H2 H 0.061621 0.441845 0.617970 0.021 Uiso 1 1 calc R U . . . C3 C 0.07728(17) 0.60922(14) 0.61623(11) 0.0183(3) Uani 1 1 d . . . . . H3 H 0.051935 0.601020 0.551381 0.022 Uiso 1 1 calc R U . . . C4 C 0.11528(16) 0.70907(14) 0.69133(11) 0.0164(3) Uani 1 1 d . . . . . C5 C 0.13528(17) 0.83220(14) 0.69678(11) 0.0183(3) Uani 1 1 d . . . . . C6 C 0.29204(17) 0.91268(14) 0.73532(11) 0.0170(3) Uani 1 1 d . . . . . C7 C 0.36194(18) 1.02679(14) 0.79370(11) 0.0201(3) Uani 1 1 d . . . . . H7 H 0.320349 1.073065 0.823993 0.024 Uiso 1 1 calc R U . . . C8 C 0.50770(18) 1.06394(14) 0.80105(11) 0.0207(3) Uani 1 1 d . . . . . H8 H 0.580865 1.139525 0.837141 0.025 Uiso 1 1 calc R U . . . C9 C 0.52444(17) 0.97146(14) 0.74685(11) 0.0177(3) Uani 1 1 d . . . . . C10 C 0.65773(17) 0.96167(14) 0.73230(11) 0.0191(3) Uani 1 1 d . . . . . C11 C 0.71987(17) 0.91105(14) 0.79977(11) 0.0170(3) Uani 1 1 d . . . . . C12 C 0.85074(17) 0.95813(14) 0.86727(11) 0.0192(3) Uani 1 1 d . . . . . H12 H 0.924374 1.032757 0.881799 0.023 Uiso 1 1 calc R U . . . C13 C 0.85747(17) 0.87609(14) 0.91189(11) 0.0191(3) Uani 1 1 d . . . . . H13 H 0.936463 0.886062 0.961310 0.023 Uiso 1 1 calc R U . . . C14 C 0.72974(16) 0.77983(13) 0.87105(11) 0.0159(3) Uani 1 1 d . . . . . C15 C 0.68255(16) 0.66549(13) 0.88973(11) 0.0163(3) Uani 1 1 d . . . . . C16 C 0.54526(17) 0.63779(13) 0.91327(11) 0.0161(3) Uani 1 1 d . . . . . C17 C 0.52306(17) 0.65201(14) 0.99877(11) 0.0190(3) Uani 1 1 d . . . . . H17 H 0.594507 0.681553 1.058632 0.023 Uiso 1 1 calc R U . . . C18 C 0.37416(17) 0.61471(14) 0.98203(11) 0.0186(3) Uani 1 1 d . . . . . H18 H 0.328874 0.615816 1.028828 0.022 Uiso 1 1 calc R U . . . C19 C 0.30752(17) 0.57689(13) 0.88650(11) 0.0159(3) Uani 1 1 d . . . . . C20 C 0.15128(17) 0.51830(14) 0.82718(11) 0.0167(3) Uani 1 1 d . . . . . C21 C 0.06245(18) 0.87903(15) 0.76432(12) 0.0216(4) Uani 1 1 d . . . . . H21A H 0.105936 0.881231 0.827790 0.032 Uiso 1 1 calc R U . . . H21B H -0.039236 0.827545 0.741354 0.032 Uiso 1 1 calc R U . . . H21C H 0.074625 0.957907 0.766516 0.032 Uiso 1 1 calc R U . . . C22 C 0.76811(19) 1.08514(16) 0.75179(14) 0.0277(4) Uani 1 1 d . . . . . H22A H 0.728931 1.119282 0.708980 0.042 Uiso 1 1 calc R U . . . H22B H 0.854714 1.080772 0.741501 0.042 Uiso 1 1 calc R U . . . H22C H 0.790965 1.133993 0.817299 0.042 Uiso 1 1 calc R U . . . C23 C 0.62581(19) 0.88570(16) 0.62955(12) 0.0255(4) Uani 1 1 d . . . . . H23A H 0.556778 0.806333 0.616439 0.038 Uiso 1 1 calc R U . . . H23B H 0.713963 0.883320 0.620720 0.038 Uiso 1 1 calc R U . . . H23C H 0.586414 0.919184 0.586235 0.038 Uiso 1 1 calc R U . . . C24 C 0.80013(18) 0.67748(15) 0.97542(11) 0.0210(3) Uani 1 1 d . . . . . H24A H 0.888859 0.692063 0.960730 0.032 Uiso 1 1 calc R U . . . H24B H 0.771116 0.605216 0.989577 0.032 Uiso 1 1 calc R U . . . H24C H 0.814987 0.742758 1.030313 0.032 Uiso 1 1 calc R U . . . C25 C 0.06107(18) 0.53526(15) 0.89121(12) 0.0216(4) Uani 1 1 d . . . . . H25A H 0.090470 0.618844 0.923325 0.032 Uiso 1 1 calc R U . . . H25B H 0.075132 0.498256 0.938280 0.032 Uiso 1 1 calc R U . . . H25C H -0.039695 0.499452 0.852700 0.032 Uiso 1 1 calc R U . . . C26 C 0.10928(18) 0.38690(14) 0.78084(12) 0.0224(4) Uani 1 1 d . . . . . H26A H 0.008669 0.348397 0.741776 0.034 Uiso 1 1 calc R U . . . H26B H 0.124628 0.353092 0.830021 0.034 Uiso 1 1 calc R U . . . H26C H 0.167812 0.375549 0.741233 0.034 Uiso 1 1 calc R U . . . C27 C 0.06424(17) 0.83076(14) 0.59845(12) 0.0185(3) Uani 1 1 d . . . . . C28 C -0.08356(18) 0.77069(16) 0.55616(13) 0.0245(4) Uani 1 1 d . . . . . H28 H -0.137308 0.726938 0.586813 0.029 Uiso 1 1 calc R U . . . C29 C -0.15312(18) 0.77352(16) 0.47090(13) 0.0248(4) Uani 1 1 d . . . . . H29 H -0.253687 0.733816 0.443558 0.030 Uiso 1 1 calc R U . . . C30 C -0.07268(17) 0.83560(14) 0.42633(11) 0.0189(3) Uani 1 1 d . . . . . C31 C 0.07371(18) 0.89350(14) 0.46426(12) 0.0210(3) Uani 1 1 d . . . . . H31 H 0.127140 0.934195 0.431822 0.025 Uiso 1 1 calc R U . . . C32 C 0.14111(18) 0.89109(14) 0.55054(12) 0.0201(3) Uani 1 1 d . . . . . H32 H 0.241668 0.931341 0.577562 0.024 Uiso 1 1 calc R U . . . C33 C 0.67164(16) 0.56500(14) 0.80590(11) 0.0165(3) Uani 1 1 d . . . . . C34 C 0.75602(17) 0.58951(14) 0.74898(11) 0.0193(3) Uani 1 1 d . . . . . H34 H 0.813247 0.668505 0.759224 0.023 Uiso 1 1 calc R U . . . C35 C 0.75817(17) 0.50144(14) 0.67804(11) 0.0200(3) Uani 1 1 d . . . . . H35 H 0.815316 0.519009 0.639481 0.024 Uiso 1 1 calc R U . . . C36 C 0.67455(17) 0.38708(14) 0.66504(11) 0.0193(3) Uani 1 1 d . . . . . C37 C 0.59127(18) 0.35839(15) 0.72062(12) 0.0214(4) Uani 1 1 d . . . . . H37 H 0.536692 0.279107 0.711185 0.026 Uiso 1 1 calc R U . . . C38 C 0.58931(17) 0.44825(14) 0.79056(11) 0.0194(3) Uani 1 1 d . . . . . H38 H 0.531218 0.430043 0.828444 0.023 Uiso 1 1 calc R U . . . C39 C 0.46839(18) 0.88638(15) 0.95681(11) 0.0201(3) Uani 1 1 d . . . . . C40 C 0.39769(19) 1.03136(14) 1.02108(11) 0.0203(3) Uani 1 1 d . . . . . C41 C 0.4177(2) 0.54299(17) 0.58120(13) 0.0308(4) Uani 1 1 d . . . . . H41A H 0.507211 0.588467 0.573771 0.046 Uiso 1 1 calc R U . . . H41B H 0.339485 0.514978 0.522000 0.046 Uiso 1 1 calc R U . . . H41C H 0.424334 0.476161 0.597107 0.046 Uiso 1 1 calc R U . . . N1 N 0.14405(14) 0.68329(12) 0.77223(10) 0.0162(3) Uani 1 1 d . . . . . N2 N 0.39213(14) 0.87902(12) 0.70751(10) 0.0177(3) Uani 1 1 d . . . . . N3 N 0.64628(14) 0.80190(12) 0.80234(9) 0.0162(3) Uani 1 1 d . . . . . N4 N 0.41326(14) 0.59238(12) 0.84522(9) 0.0161(3) Uani 1 1 d . . . . . N5 N -0.14621(15) 0.83813(12) 0.33541(10) 0.0223(3) Uani 1 1 d . . . . . N6 N 0.67543(16) 0.29254(13) 0.58908(10) 0.0239(3) Uani 1 1 d . . . . . N7 N 0.36477(15) 0.91688(12) 0.97767(9) 0.0190(3) Uani 1 1 d . . . . . O1 O -0.27643(13) 0.78528(12) 0.30298(10) 0.0335(3) Uani 1 1 d . . . . . O2 O -0.07413(14) 0.89105(11) 0.29515(9) 0.0295(3) Uani 1 1 d . . . . . O3 O 0.73068(14) 0.31913(12) 0.53095(9) 0.0333(3) Uani 1 1 d . . . . . O4 O 0.61952(16) 0.19205(11) 0.58717(9) 0.0347(3) Uani 1 1 d . . . . . O5 O 0.23608(13) 0.83791(10) 0.95692(8) 0.0239(3) Uani 1 1 d . . . . . O6 O 0.39141(13) 0.61492(11) 0.65512(8) 0.0244(3) Uani 1 1 d . . . . . H39 H 0.4429(19) 0.8067(16) 0.9291(13) 0.021(5) Uiso 1 1 d . . . . . H4N H 0.398(2) 0.5788(17) 0.7849(15) 0.028(5) Uiso 1 1 d . . . . . H40 H 0.323(2) 1.0492(16) 1.0325(13) 0.025(5) Uiso 1 1 d . . . . . H2N H 0.374(2) 0.8106(19) 0.6677(15) 0.034(6) Uiso 1 1 d . . . . . H1N H 0.173(2) 0.7347(19) 0.8314(16) 0.039(6) Uiso 1 1 d . . . . . H3N H 0.558(2) 0.7512(19) 0.7635(16) 0.040(6) Uiso 1 1 d . . . . . H6O H 0.300(3) 0.596(2) 0.6415(17) 0.055(7) 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 0.0142(7) 0.0164(8) 0.0173(7) 0.0051(6) 0.0062(6) 0.0064(6) C2 0.0179(8) 0.0171(8) 0.0164(8) 0.0035(6) 0.0060(6) 0.0064(6) C3 0.0166(8) 0.0224(8) 0.0148(7) 0.0060(6) 0.0047(6) 0.0075(7) C4 0.0146(8) 0.0193(8) 0.0182(8) 0.0079(6) 0.0074(6) 0.0079(6) C5 0.0182(8) 0.0189(8) 0.0207(8) 0.0080(7) 0.0088(7) 0.0089(7) C6 0.0193(8) 0.0180(8) 0.0182(8) 0.0084(6) 0.0084(6) 0.0100(7) C7 0.0241(9) 0.0201(8) 0.0196(8) 0.0070(7) 0.0090(7) 0.0120(7) C8 0.0211(8) 0.0168(8) 0.0201(8) 0.0053(7) 0.0048(7) 0.0052(7) C9 0.0182(8) 0.0190(8) 0.0165(7) 0.0082(6) 0.0058(6) 0.0070(6) C10 0.0170(8) 0.0218(8) 0.0192(8) 0.0079(7) 0.0073(6) 0.0074(7) C11 0.0166(8) 0.0174(8) 0.0161(7) 0.0044(6) 0.0073(6) 0.0059(6) C12 0.0176(8) 0.0174(8) 0.0180(8) 0.0033(6) 0.0054(6) 0.0043(6) C13 0.0165(8) 0.0206(8) 0.0157(8) 0.0030(6) 0.0024(6) 0.0065(7) C14 0.0161(8) 0.0170(8) 0.0137(7) 0.0026(6) 0.0045(6) 0.0079(6) C15 0.0168(8) 0.0166(8) 0.0147(7) 0.0043(6) 0.0044(6) 0.0075(6) C16 0.0176(8) 0.0165(8) 0.0147(7) 0.0050(6) 0.0048(6) 0.0083(6) C17 0.0210(8) 0.0198(8) 0.0146(7) 0.0052(6) 0.0040(6) 0.0083(7) C18 0.0233(8) 0.0194(8) 0.0156(8) 0.0067(6) 0.0092(7) 0.0097(7) C19 0.0183(8) 0.0144(8) 0.0161(7) 0.0055(6) 0.0070(6) 0.0073(6) C20 0.0181(8) 0.0165(8) 0.0165(7) 0.0061(6) 0.0068(6) 0.0073(6) C21 0.0247(9) 0.0209(9) 0.0265(9) 0.0103(7) 0.0142(7) 0.0129(7) C22 0.0213(9) 0.0301(10) 0.0354(10) 0.0189(8) 0.0102(8) 0.0091(8) C23 0.0258(9) 0.0374(11) 0.0195(8) 0.0122(8) 0.0114(7) 0.0162(8) C24 0.0216(8) 0.0222(9) 0.0185(8) 0.0067(7) 0.0041(7) 0.0099(7) C25 0.0198(8) 0.0274(9) 0.0215(8) 0.0113(7) 0.0098(7) 0.0104(7) C26 0.0245(9) 0.0171(8) 0.0226(8) 0.0064(7) 0.0055(7) 0.0068(7) C27 0.0195(8) 0.0177(8) 0.0241(8) 0.0096(7) 0.0101(7) 0.0111(7) C28 0.0195(9) 0.0291(10) 0.0308(9) 0.0182(8) 0.0112(7) 0.0097(7) C29 0.0168(8) 0.0275(9) 0.0329(10) 0.0153(8) 0.0077(7) 0.0091(7) C30 0.0218(8) 0.0160(8) 0.0219(8) 0.0078(7) 0.0073(7) 0.0104(7) C31 0.0229(9) 0.0202(8) 0.0221(8) 0.0086(7) 0.0110(7) 0.0083(7) C32 0.0177(8) 0.0214(9) 0.0220(8) 0.0072(7) 0.0081(7) 0.0082(7) C33 0.0152(8) 0.0195(8) 0.0150(7) 0.0048(6) 0.0027(6) 0.0096(6) C34 0.0160(8) 0.0192(8) 0.0219(8) 0.0060(7) 0.0062(7) 0.0070(6) C35 0.0185(8) 0.0234(9) 0.0194(8) 0.0060(7) 0.0074(7) 0.0106(7) C36 0.0204(8) 0.0206(8) 0.0164(8) 0.0024(6) 0.0032(6) 0.0125(7) C37 0.0215(9) 0.0176(8) 0.0223(8) 0.0036(7) 0.0051(7) 0.0084(7) C38 0.0200(8) 0.0194(8) 0.0205(8) 0.0079(7) 0.0078(7) 0.0085(7) C39 0.0292(9) 0.0161(8) 0.0177(8) 0.0045(6) 0.0108(7) 0.0116(7) C40 0.0279(9) 0.0187(8) 0.0158(8) 0.0032(6) 0.0093(7) 0.0121(7) C41 0.0335(10) 0.0336(11) 0.0230(9) 0.0032(8) 0.0099(8) 0.0158(9) N1 0.0184(7) 0.0154(7) 0.0156(7) 0.0048(6) 0.0072(5) 0.0072(5) N2 0.0179(7) 0.0155(7) 0.0194(7) 0.0039(6) 0.0077(6) 0.0072(6) N3 0.0148(7) 0.0163(7) 0.0144(6) 0.0027(5) 0.0035(5) 0.0055(6) N4 0.0179(7) 0.0197(7) 0.0113(6) 0.0046(5) 0.0056(5) 0.0087(6) N5 0.0235(8) 0.0206(7) 0.0262(8) 0.0102(6) 0.0081(6) 0.0119(6) N6 0.0251(8) 0.0252(8) 0.0203(7) 0.0034(6) 0.0043(6) 0.0144(6) N7 0.0241(7) 0.0169(7) 0.0154(6) 0.0037(5) 0.0088(6) 0.0079(6) O1 0.0211(7) 0.0380(8) 0.0382(8) 0.0184(6) 0.0027(6) 0.0092(6) O2 0.0306(7) 0.0359(8) 0.0313(7) 0.0212(6) 0.0137(6) 0.0156(6) O3 0.0350(8) 0.0351(8) 0.0285(7) 0.0026(6) 0.0176(6) 0.0145(6) O4 0.0534(9) 0.0222(7) 0.0270(7) 0.0043(6) 0.0099(6) 0.0187(6) O5 0.0254(6) 0.0197(6) 0.0210(6) 0.0024(5) 0.0101(5) 0.0046(5) O6 0.0177(6) 0.0322(7) 0.0170(6) 0.0023(5) 0.0060(5) 0.0073(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 C1 C2 107.29(14) . . ? N1 C1 C20 121.13(13) . . ? C2 C1 C20 131.57(14) . . ? C1 C2 C3 107.37(14) . . ? C1 C2 H2 126.3 . . ? C3 C2 H2 126.3 . . ? C4 C3 C2 107.57(14) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? N1 C4 C3 107.35(14) . . ? N1 C4 C5 120.54(14) . . ? C3 C4 C5 132.02(15) . . ? C6 C5 C4 109.98(13) . . ? C6 C5 C27 111.67(13) . . ? C4 C5 C27 109.50(13) . . ? C6 C5 C21 107.89(13) . . ? C4 C5 C21 110.14(13) . . ? C27 C5 C21 107.63(13) . . ? C7 C6 N2 107.17(14) . . ? C7 C6 C5 130.78(14) . . ? N2 C6 C5 121.88(14) . . ? C6 C7 C8 107.89(14) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? C9 C8 C7 108.03(14) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? C8 C9 N2 106.83(14) . . ? C8 C9 C10 130.11(15) . . ? N2 C9 C10 122.99(14) . . ? C11 C10 C9 111.15(13) . . ? C11 C10 C22 108.58(14) . . ? C9 C10 C22 108.03(14) . . ? C11 C10 C23 109.80(13) . . ? C9 C10 C23 110.64(13) . . ? C22 C10 C23 108.56(14) . . ? C12 C11 N3 106.97(14) . . ? C12 C11 C10 129.74(15) . . ? N3 C11 C10 123.28(14) . . ? C11 C12 C13 108.11(14) . . ? C11 C12 H12 125.9 . . ? C13 C12 H12 125.9 . . ? C14 C13 C12 107.97(14) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? C13 C14 N3 106.78(14) . . ? C13 C14 C15 129.63(15) . . ? N3 C14 C15 123.53(14) . . ? C16 C15 C14 111.93(12) . . ? C16 C15 C24 108.08(13) . . ? C14 C15 C24 108.03(13) . . ? C16 C15 C33 112.10(13) . . ? C14 C15 C33 110.58(12) . . ? C24 C15 C33 105.82(12) . . ? C17 C16 N4 106.84(14) . . ? C17 C16 C15 130.42(14) . . ? N4 C16 C15 122.73(13) . . ? C16 C17 C18 107.98(14) . . ? C16 C17 H17 126.0 . . ? C18 C17 H17 126.0 . . ? C19 C18 C17 108.02(14) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? C18 C19 N4 106.73(14) . . ? C18 C19 C20 131.69(14) . . ? N4 C19 C20 121.38(13) . . ? C1 C20 C19 110.30(13) . . ? C1 C20 C26 108.87(13) . . ? C19 C20 C26 108.87(13) . . ? C1 C20 C25 110.36(13) . . ? C19 C20 C25 109.38(13) . . ? C26 C20 C25 109.03(13) . . ? C5 C21 H21A 109.5 . . ? C5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C10 C22 H22A 109.5 . . ? C10 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C10 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C15 C24 H24A 109.5 . . ? C15 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C15 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.07(15) . . ? C32 C27 C5 122.37(15) . . ? C28 C27 C5 119.52(14) . . ? C29 C28 C27 121.57(16) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 118.36(16) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C31 C30 C29 121.98(16) . . ? C31 C30 N5 119.53(14) . . ? C29 C30 N5 118.48(15) . . ? C30 C31 C32 118.71(15) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C31 C32 C27 121.27(15) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C38 C33 C34 118.42(14) . . ? C38 C33 C15 121.53(14) . . ? C34 C33 C15 119.76(14) . . ? C35 C34 C33 121.64(15) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C36 C35 C34 118.00(15) . . ? C36 C35 H35 121.0 . . ? C34 C35 H35 121.0 . . ? C35 C36 C37 122.49(15) . . ? C35 C36 N6 118.38(15) . . ? C37 C36 N6 119.13(15) . . ? C36 C37 C38 118.49(15) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? C37 C38 C33 120.93(15) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? N7 C39 C40 120.86(16) . 2_677 ? N7 C39 H39 116.2(11) . . ? C40 C39 H39 122.9(11) 2_677 . ? N7 C40 C39 120.62(15) . 2_677 ? N7 C40 H40 116.0(12) . . ? C39 C40 H40 123.3(12) 2_677 . ? O6 C41 H41A 109.5 . . ? O6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C1 N1 C4 110.41(13) . . ? C1 N1 H1N 124.9(14) . . ? C4 N1 H1N 124.7(14) . . ? C9 N2 C6 110.08(14) . . ? C9 N2 H2N 124.5(13) . . ? C6 N2 H2N 125.2(14) . . ? C14 N3 C11 110.16(13) . . ? C14 N3 H3N 124.8(14) . . ? C11 N3 H3N 125.0(14) . . ? C16 N4 C19 110.41(13) . . ? C16 N4 H4N 125.5(13) . . ? C19 N4 H4N 123.9(13) . . ? O2 N5 O1 123.58(15) . . ? O2 N5 C30 118.22(14) . . ? O1 N5 C30 118.19(14) . . ? O4 N6 O3 123.91(14) . . ? O4 N6 C36 118.01(14) . . ? O3 N6 C36 118.07(14) . . ? O5 N7 C40 120.49(13) . . ? O5 N7 C39 121.00(14) . . ? C40 N7 C39 118.52(15) . . ? C41 O6 H6O 109.8(16) . . ? 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 N1 1.373(2) . ? C1 C2 1.380(2) . ? C1 C20 1.512(2) . ? C2 C3 1.428(2) . ? C2 H2 0.9500 . ? C3 C4 1.376(2) . ? C3 H3 0.9500 . ? C4 N1 1.374(2) . ? C4 C5 1.520(2) . ? C5 C6 1.513(2) . ? C5 C27 1.538(2) . ? C5 C21 1.550(2) . ? C6 C7 1.366(2) . ? C6 N2 1.3827(19) . ? C7 C8 1.419(2) . ? C7 H7 0.9500 . ? C8 C9 1.373(2) . ? C8 H8 0.9500 . ? C9 N2 1.380(2) . ? C9 C10 1.515(2) . ? C10 C11 1.515(2) . ? C10 C22 1.539(2) . ? C10 C23 1.543(2) . ? C11 C12 1.367(2) . ? C11 N3 1.383(2) . ? C12 C13 1.420(2) . ? C12 H12 0.9500 . ? C13 C14 1.373(2) . ? C13 H13 0.9500 . ? C14 N3 1.383(2) . ? C14 C15 1.521(2) . ? C15 C16 1.519(2) . ? C15 C24 1.545(2) . ? C15 C33 1.547(2) . ? C16 C17 1.372(2) . ? C16 N4 1.381(2) . ? C17 C18 1.423(2) . ? C17 H17 0.9500 . ? C18 C19 1.371(2) . ? C18 H18 0.9500 . ? C19 N4 1.3846(19) . ? C19 C20 1.517(2) . ? C20 C26 1.539(2) . ? C20 C25 1.543(2) . ? 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 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.393(2) . ? C27 C28 1.400(2) . ? C28 C29 1.382(2) . ? C28 H28 0.9500 . ? C29 C30 1.384(2) . ? C29 H29 0.9500 . ? C30 C31 1.381(2) . ? C30 N5 1.468(2) . ? C31 C32 1.385(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.398(2) . ? C33 C34 1.399(2) . ? C34 C35 1.386(2) . ? C34 H34 0.9500 . ? C35 C36 1.384(2) . ? C35 H35 0.9500 . ? C36 C37 1.385(2) . ? C36 N6 1.479(2) . ? C37 C38 1.391(2) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 N7 1.358(2) . ? C39 C40 1.360(2) 2_677 ? C39 H39 0.933(19) . ? C40 N7 1.356(2) . ? C40 H40 0.937(19) . ? C41 O6 1.428(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N1 H1N 0.90(2) . ? N2 H2N 0.88(2) . ? N3 H3N 0.90(2) . ? N4 H4N 0.87(2) . ? N5 O2 1.2266(18) . ? N5 O1 1.2290(18) . ? N6 O4 1.2276(19) . ? N6 O3 1.2304(19) . ? N7 O5 1.3079(17) . ? O6 H6O 0.88(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C37 H37 O1 0.95 2.53 3.103(2) 118.8 2_566 C39 H39 N4 0.933(19) 2.642(19) 3.564(2) 170.1(15) . N4 H4N O6 0.87(2) 2.17(2) 2.9966(18) 158.7(17) . C40 H40 N3 0.937(19) 2.672(19) 3.266(2) 121.9(14) 2_677 N2 H2N O6 0.88(2) 2.58(2) 3.3222(19) 143.6(17) . N1 H1N N7 0.90(2) 2.64(2) 3.4625(19) 152.0(18) . N1 H1N O5 0.90(2) 1.89(2) 2.7896(18) 177(2) . N3 H3N O6 0.90(2) 2.05(2) 2.9213(19) 162(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 N1 C1 C2 C3 0.12(17) . . . . ? C20 C1 C2 C3 -178.97(15) . . . . ? C1 C2 C3 C4 -0.24(18) . . . . ? C2 C3 C4 N1 0.26(17) . . . . ? C2 C3 C4 C5 176.82(16) . . . . ? N1 C4 C5 C6 69.79(18) . . . . ? C3 C4 C5 C6 -106.40(19) . . . . ? N1 C4 C5 C27 -167.15(13) . . . . ? C3 C4 C5 C27 16.7(2) . . . . ? N1 C4 C5 C21 -48.99(19) . . . . ? C3 C4 C5 C21 134.82(18) . . . . ? C4 C5 C6 C7 -143.72(17) . . . . ? C27 C5 C6 C7 94.5(2) . . . . ? C21 C5 C6 C7 -23.6(2) . . . . ? C4 C5 C6 N2 41.6(2) . . . . ? C27 C5 C6 N2 -80.13(18) . . . . ? C21 C5 C6 N2 161.79(14) . . . . ? N2 C6 C7 C8 0.51(18) . . . . ? C5 C6 C7 C8 -174.73(16) . . . . ? C6 C7 C8 C9 -0.04(19) . . . . ? C7 C8 C9 N2 -0.45(18) . . . . ? C7 C8 C9 C10 -177.51(16) . . . . ? C8 C9 C10 C11 94.2(2) . . . . ? N2 C9 C10 C11 -82.48(18) . . . . ? C8 C9 C10 C22 -24.9(2) . . . . ? N2 C9 C10 C22 158.49(15) . . . . ? C8 C9 C10 C23 -143.56(17) . . . . ? N2 C9 C10 C23 39.8(2) . . . . ? C9 C10 C11 C12 -120.08(18) . . . . ? C22 C10 C11 C12 -1.4(2) . . . . ? C23 C10 C11 C12 117.17(18) . . . . ? C9 C10 C11 N3 59.70(19) . . . . ? C22 C10 C11 N3 178.39(14) . . . . ? C23 C10 C11 N3 -63.06(19) . . . . ? N3 C11 C12 C13 0.12(17) . . . . ? C10 C11 C12 C13 179.92(15) . . . . ? C11 C12 C13 C14 -0.26(18) . . . . ? C12 C13 C14 N3 0.29(17) . . . . ? C12 C13 C14 C15 177.51(15) . . . . ? C13 C14 C15 C16 125.70(17) . . . . ? N3 C14 C15 C16 -57.49(19) . . . . ? C13 C14 C15 C24 6.8(2) . . . . ? N3 C14 C15 C24 -176.36(13) . . . . ? C13 C14 C15 C33 -108.54(18) . . . . ? N3 C14 C15 C33 68.27(18) . . . . ? C14 C15 C16 C17 -100.36(19) . . . . ? C24 C15 C16 C17 18.5(2) . . . . ? C33 C15 C16 C17 134.72(17) . . . . ? C14 C15 C16 N4 78.37(18) . . . . ? C24 C15 C16 N4 -162.79(14) . . . . ? C33 C15 C16 N4 -46.54(19) . . . . ? N4 C16 C17 C18 -0.21(18) . . . . ? C15 C16 C17 C18 178.67(15) . . . . ? C16 C17 C18 C19 0.76(19) . . . . ? C17 C18 C19 N4 -0.99(18) . . . . ? C17 C18 C19 C20 173.82(16) . . . . ? N1 C1 C20 C19 -65.12(18) . . . . ? C2 C1 C20 C19 113.87(19) . . . . ? N1 C1 C20 C26 175.49(14) . . . . ? C2 C1 C20 C26 -5.5(2) . . . . ? N1 C1 C20 C25 55.86(19) . . . . ? C2 C1 C20 C25 -125.15(18) . . . . ? C18 C19 C20 C1 138.52(17) . . . . ? N4 C19 C20 C1 -47.30(19) . . . . ? C18 C19 C20 C26 -102.09(19) . . . . ? N4 C19 C20 C26 72.09(18) . . . . ? C18 C19 C20 C25 17.0(2) . . . . ? N4 C19 C20 C25 -168.86(14) . . . . ? C6 C5 C27 C32 4.2(2) . . . . ? C4 C5 C27 C32 -117.82(16) . . . . ? C21 C5 C27 C32 122.46(16) . . . . ? C6 C5 C27 C28 -173.31(14) . . . . ? C4 C5 C27 C28 64.64(18) . . . . ? C21 C5 C27 C28 -55.07(19) . . . . ? C32 C27 C28 C29 -2.1(3) . . . . ? C5 C27 C28 C29 175.55(16) . . . . ? C27 C28 C29 C30 1.4(3) . . . . ? C28 C29 C30 C31 0.4(3) . . . . ? C28 C29 C30 N5 179.61(15) . . . . ? C29 C30 C31 C32 -1.4(2) . . . . ? N5 C30 C31 C32 179.38(14) . . . . ? C30 C31 C32 C27 0.7(2) . . . . ? C28 C27 C32 C31 1.0(2) . . . . ? C5 C27 C32 C31 -176.54(14) . . . . ? C16 C15 C33 C38 -33.4(2) . . . . ? C14 C15 C33 C38 -159.10(14) . . . . ? C24 C15 C33 C38 84.16(17) . . . . ? C16 C15 C33 C34 152.77(14) . . . . ? C14 C15 C33 C34 27.1(2) . . . . ? C24 C15 C33 C34 -89.63(17) . . . . ? C38 C33 C34 C35 0.7(2) . . . . ? C15 C33 C34 C35 174.70(14) . . . . ? C33 C34 C35 C36 -0.4(2) . . . . ? C34 C35 C36 C37 -0.7(2) . . . . ? C34 C35 C36 N6 179.60(14) . . . . ? C35 C36 C37 C38 1.6(2) . . . . ? N6 C36 C37 C38 -178.75(14) . . . . ? C36 C37 C38 C33 -1.3(2) . . . . ? C34 C33 C38 C37 0.2(2) . . . . ? C15 C33 C38 C37 -173.70(15) . . . . ? C2 C1 N1 C4 0.04(17) . . . . ? C20 C1 N1 C4 179.25(13) . . . . ? C3 C4 N1 C1 -0.19(17) . . . . ? C5 C4 N1 C1 -177.23(13) . . . . ? C8 C9 N2 C6 0.78(18) . . . . ? C10 C9 N2 C6 178.10(14) . . . . ? C7 C6 N2 C9 -0.80(18) . . . . ? C5 C6 N2 C9 174.95(14) . . . . ? C13 C14 N3 C11 -0.22(17) . . . . ? C15 C14 N3 C11 -177.65(13) . . . . ? C12 C11 N3 C14 0.06(17) . . . . ? C10 C11 N3 C14 -179.76(13) . . . . ? C17 C16 N4 C19 -0.41(18) . . . . ? C15 C16 N4 C19 -179.41(14) . . . . ? C18 C19 N4 C16 0.89(18) . . . . ? C20 C19 N4 C16 -174.58(14) . . . . ? C31 C30 N5 O2 0.9(2) . . . . ? C29 C30 N5 O2 -178.36(15) . . . . ? C31 C30 N5 O1 179.56(15) . . . . ? C29 C30 N5 O1 0.3(2) . . . . ? C35 C36 N6 O4 168.79(15) . . . . ? C37 C36 N6 O4 -10.9(2) . . . . ? C35 C36 N6 O3 -12.0(2) . . . . ? C37 C36 N6 O3 168.28(15) . . . . ? C39 C40 N7 O5 179.66(15) 2_677 . . . ? C39 C40 N7 C39 0.0(3) 2_677 . . . ? C40 C39 N7 O5 -179.66(15) 2_677 . . . ? C40 C39 N7 C40 0.0(3) 2_677 . . . ?