#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:01:57 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257293 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557830.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_1557830 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_page_last 5657 _journal_paper_doi 10.1039/D0SC01496F _journal_volume 11 _journal_year 2020 _chemical_formula_moiety '2 C36 H38 N6, C4 H4 N2 O2, 2 C H4 O, 2 H2 O' _chemical_formula_sum 'C78 H92 N14 O6' _chemical_formula_weight 1321.65 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 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 90 _cell_angle_beta 93.976(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.761(3) _cell_length_b 17.133(3) _cell_length_c 31.684(5) _cell_measurement_reflns_used 4693 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 22.6 _cell_measurement_theta_min 2.31 _cell_volume 6911(2) _computing_cell_refinement 'Apex II release 2010, Bruker AXS, Inc.' _computing_data_collection 'Apex II release 2010, Bruker AXS, Inc.' _computing_data_reduction 'Apex II release 2010, Bruker AXS, Inc.' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material 'SHELXL-2016/6, Sheldrick, G. M.' _computing_structure_refinement 'Shelxl-2016/6, Sheldrick, G. M.' _computing_structure_solution ; Sheldrick, G. M. (2015). SHELXT. Acta Cryst. A71, 3-8. ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Nonius Kappa CCD with a Bruker Apex II detector' _diffrn_measurement_method \w-scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1768 _diffrn_reflns_av_unetI/netI 0.1311 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 63040 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.493 _diffrn_reflns_theta_min 1.993 _diffrn_source 'sealed fine focus tube' _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.270 _exptl_crystal_description prism _exptl_crystal_F_000 2824 _refine_diff_density_max 0.381 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.072 _refine_ls_extinction_coef 0.0042(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 482 _refine_ls_number_reflns 6385 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0644 _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^)+(0.0670P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1483 _refine_ls_wR_factor_ref 0.1703 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3948 _reflns_number_total 6385 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01496f3.cif _cod_data_source_block shelx_CCDC2 _cod_depositor_comments ;Adding full bibliography for 1557828--1557833.cif. Adding full bibliography for 1557828--1557833.cif. ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1557830 _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_res_file ; TITL pyC4Ppyr in C2/c shelx.res created by SHELXL-2016/6 at 13:59:08 on 24-Apr-2019 CELL 0.71073 12.7608 17.1331 31.6843 90.000 93.976 90.000 ZERR 4.00 0.0029 0.0029 0.0054 0.000 0.010 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 312 368 56 24 MERG 2 OMIT 0 0 2 OMIT 1 1 1 EQIV $2 -x+3/2, y+1/2, -z+1/2 HTAB O1A N6_$2 EQIV $3 -x+3/2, y-1/2, -z+1/2 HTAB C1A N5_$3 HTAB C1A N6_$2 HTAB N3 N7 HTAB N3 O1 dfix 1.45 o1a c1a HTAB N4 O1W HTAB O1W N5_$3 HTAB N1 O1W HTAB N2 O1A FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 TEMP -173.00 WGHT 0.067000 EXTI 0.004193 FVAR 0.23788 C1 1 0.676814 0.022578 0.075031 11.00000 0.02564 0.01351 = 0.01460 -0.00190 0.00573 -0.00290 C2 1 0.586363 0.012624 0.049793 11.00000 0.02396 0.02136 = 0.01933 -0.00613 0.00239 -0.00658 AFIX 43 H2 2 0.573732 -0.027052 0.029120 11.00000 -1.20000 AFIX 0 C3 1 0.515200 0.071628 0.059876 11.00000 0.01738 0.02614 = 0.02481 0.00169 -0.00203 -0.00415 AFIX 43 H3 2 0.446564 0.079134 0.046911 11.00000 -1.20000 AFIX 0 C4 1 0.562464 0.116226 0.091659 11.00000 0.01487 0.01976 = 0.02365 0.00088 0.00457 -0.00349 C5 1 0.522814 0.184428 0.115827 11.00000 0.01737 0.01885 = 0.03273 -0.00215 0.00245 0.00016 C6 1 0.589523 0.256089 0.110015 11.00000 0.01324 0.01735 = 0.02571 -0.00286 0.00151 0.00214 C7 1 0.587599 0.308481 0.077663 11.00000 0.01977 0.02491 = 0.02395 -0.00018 -0.00472 0.00056 AFIX 43 H7 2 0.538602 0.308951 0.053680 11.00000 -1.20000 AFIX 0 C8 1 0.670349 0.361771 0.085729 11.00000 0.02509 0.01528 = 0.02366 0.00118 0.00213 0.00231 AFIX 43 H8 2 0.686790 0.404582 0.068315 11.00000 -1.20000 AFIX 0 C9 1 0.722775 0.341063 0.122987 11.00000 0.01983 0.01356 = 0.02343 -0.00275 0.00386 0.00246 C10 1 0.818450 0.376512 0.147383 11.00000 0.01751 0.01404 = 0.01898 -0.00327 0.00221 0.00163 C11 1 0.897204 0.312749 0.158903 11.00000 0.01815 0.01449 = 0.01662 -0.00400 0.00197 -0.00387 C12 1 0.931505 0.278624 0.196419 11.00000 0.02287 0.02333 = 0.01443 -0.00389 0.00235 -0.00363 AFIX 43 H12 2 0.911038 0.292580 0.223676 11.00000 -1.20000 AFIX 0 C13 1 1.002872 0.218876 0.187272 11.00000 0.02029 0.02147 = 0.01649 0.00237 -0.00009 -0.00162 AFIX 43 H13 2 1.039412 0.185707 0.207312 11.00000 -1.20000 AFIX 0 C14 1 1.009905 0.217367 0.144389 11.00000 0.01715 0.01700 = 0.02130 -0.00178 -0.00242 -0.00192 C15 1 1.071296 0.166376 0.115767 11.00000 0.02026 0.01657 = 0.02244 0.00073 0.00265 0.00213 C16 1 0.999033 0.115840 0.087431 11.00000 0.01590 0.01285 = 0.02472 -0.00080 0.00681 0.00201 C17 1 1.003628 0.094738 0.046230 11.00000 0.02698 0.02282 = 0.02236 -0.00186 0.01116 -0.00182 AFIX 43 H17 2 1.052202 0.113854 0.027307 11.00000 -1.20000 AFIX 0 C18 1 0.923752 0.039576 0.036532 11.00000 0.02529 0.02189 = 0.02178 -0.00677 0.00789 -0.00394 AFIX 43 H18 2 0.908889 0.015301 0.009829 11.00000 -1.20000 AFIX 0 C19 1 0.871326 0.026915 0.072006 11.00000 0.01728 0.01369 = 0.01880 -0.00374 0.00249 0.00407 C20 1 0.777059 -0.023924 0.078985 11.00000 0.02442 0.01319 = 0.01831 -0.00115 0.00605 -0.00280 C21 1 0.409087 0.202131 0.098979 11.00000 0.01895 0.03159 = 0.05685 -0.00605 0.00217 0.00102 AFIX 137 H21A 2 0.407763 0.214614 0.068762 11.00000 -1.50000 H21B 2 0.382305 0.246678 0.114375 11.00000 -1.50000 H21C 2 0.364882 0.156356 0.103087 11.00000 -1.50000 AFIX 0 C22 1 0.522162 0.161807 0.163130 11.00000 0.02792 0.02504 = 0.03594 -0.00477 0.01388 -0.00473 AFIX 137 H22A 2 0.474287 0.117754 0.166178 11.00000 -1.50000 H22B 2 0.498548 0.206463 0.179309 11.00000 -1.50000 H22C 2 0.593240 0.146888 0.173836 11.00000 -1.50000 AFIX 0 C23 1 0.867947 0.437399 0.118424 11.00000 0.02145 0.01793 = 0.02878 -0.00029 0.00640 0.00264 AFIX 137 H23A 2 0.932090 0.458606 0.132904 11.00000 -1.50000 H23B 2 0.817811 0.479827 0.112070 11.00000 -1.50000 H23C 2 0.885189 0.412206 0.092016 11.00000 -1.50000 AFIX 0 C24 1 1.137996 0.217282 0.087762 11.00000 0.01802 0.02127 = 0.03518 -0.00312 0.00731 -0.00144 AFIX 137 H24A 2 1.180705 0.183608 0.070771 11.00000 -1.50000 H24B 2 1.184101 0.251128 0.105740 11.00000 -1.50000 H24C 2 1.091577 0.249468 0.068975 11.00000 -1.50000 AFIX 0 C25 1 1.144658 0.113591 0.143459 11.00000 0.02471 0.02486 = 0.03853 -0.00026 -0.00072 0.00742 AFIX 137 H25A 2 1.103100 0.082125 0.162005 11.00000 -1.50000 H25B 2 1.194507 0.145852 0.160701 11.00000 -1.50000 H25C 2 1.183265 0.079054 0.125372 11.00000 -1.50000 AFIX 0 C26 1 0.771053 -0.089172 0.044989 11.00000 0.03176 0.01902 = 0.02403 -0.00593 0.00738 -0.00359 AFIX 137 H26A 2 0.710126 -0.122539 0.048937 11.00000 -1.50000 H26B 2 0.835279 -0.120653 0.047781 11.00000 -1.50000 H26C 2 0.763956 -0.065563 0.016763 11.00000 -1.50000 AFIX 0 C27 1 0.789011 0.419962 0.187060 11.00000 0.02497 0.01709 = 0.02218 -0.00166 0.00274 0.00480 C28 1 0.685234 0.433717 0.195281 11.00000 0.02232 0.02290 = 0.02249 0.00192 0.00197 0.00215 AFIX 43 H28 2 0.629608 0.411688 0.177677 11.00000 -1.20000 AFIX 0 C29 1 0.663706 0.480091 0.229566 11.00000 0.03154 0.03609 = 0.02589 0.00069 0.01020 0.01151 AFIX 43 H29 2 0.592105 0.488431 0.234712 11.00000 -1.20000 AFIX 0 C30 1 0.835724 0.498455 0.247450 11.00000 0.03717 0.04756 = 0.04165 -0.02360 -0.01258 0.01145 AFIX 43 H30 2 0.889807 0.520426 0.265862 11.00000 -1.20000 AFIX 0 C31 1 0.865205 0.453334 0.214224 11.00000 0.02930 0.03073 = 0.03803 -0.01945 -0.00100 0.00658 AFIX 43 H31 2 0.937457 0.445340 0.210110 11.00000 -1.20000 AFIX 0 C32 1 0.787860 -0.066194 0.121871 11.00000 0.02808 0.00934 = 0.02192 -0.00545 0.00177 -0.00045 C33 1 0.883810 -0.088283 0.141196 11.00000 0.03036 0.01866 = 0.03118 -0.00170 0.00551 0.00005 AFIX 43 H33 2 0.947176 -0.074468 0.129000 11.00000 -1.20000 AFIX 0 C34 1 0.886739 -0.130469 0.178261 11.00000 0.03990 0.02408 = 0.03306 0.00097 0.00102 0.00018 AFIX 43 H34 2 0.953598 -0.144085 0.191227 11.00000 -1.20000 AFIX 0 C35 1 0.709521 -0.133125 0.178154 11.00000 0.04196 0.02892 = 0.02743 0.00196 0.00558 -0.00843 AFIX 43 H35 2 0.647534 -0.149227 0.190669 11.00000 -1.20000 AFIX 0 C36 1 0.699136 -0.089897 0.141258 11.00000 0.02789 0.02158 = 0.02609 0.00201 0.00569 -0.00466 AFIX 43 H36 2 0.631285 -0.076460 0.129213 11.00000 -1.20000 AFIX 0 C37 1 0.794929 0.211542 0.033563 11.00000 0.02480 0.02111 = 0.02016 0.00441 0.00468 -0.00011 C38 1 0.792944 0.317038 -0.012634 11.00000 0.02670 0.02094 = 0.01692 0.00414 0.00371 0.00269 N1 3 0.660869 0.085671 0.100496 11.00000 0.01838 0.01952 = 0.01532 -0.00267 0.00062 -0.00291 N2 3 0.673493 0.275972 0.137730 11.00000 0.01668 0.01729 = 0.02092 0.00058 0.00057 -0.00051 N3 3 0.945246 0.274444 0.127331 11.00000 0.01743 0.01742 = 0.01456 -0.00066 0.00214 0.00065 N4 3 0.917447 0.074780 0.102910 11.00000 0.02274 0.01557 = 0.01804 -0.00197 0.00743 -0.00194 N5 3 0.735892 0.513440 0.255543 11.00000 0.04276 0.04646 = 0.02685 -0.01167 -0.00194 0.01785 N6 3 0.802033 -0.153337 0.197040 11.00000 0.05042 0.03330 = 0.02581 0.00700 0.00089 -0.00554 N7 3 0.839340 0.278766 0.021164 11.00000 0.02327 0.02073 = 0.01673 0.00018 0.00513 0.00093 O1 4 0.923817 0.306674 0.040903 11.00000 0.02467 0.02991 = 0.01891 0.00117 -0.00156 -0.00619 O1W 4 0.803831 0.108101 0.176195 11.00000 0.02879 0.02588 = 0.01576 0.00227 0.00360 -0.00579 O1A 4 0.682399 0.251805 0.232220 11.00000 0.10036 0.06984 = 0.02973 -0.00872 0.01520 -0.04998 AFIX 3 H1A 2 0.700783 0.291295 0.246601 11.00000 -1.50000 AFIX 0 C1A 1 0.678886 0.193225 0.256178 11.00000 0.18397 0.07917 = 0.08605 -0.00945 0.01331 0.00234 AFIX 137 H1A1 2 0.738680 0.158924 0.251891 11.00000 -1.50000 H1A2 2 0.613241 0.164697 0.249542 11.00000 -1.50000 H1A3 2 0.682007 0.210531 0.285719 11.00000 -1.50000 AFIX 0 H3N 2 0.937995 0.287402 0.098827 11.00000 0.02915 H37 2 0.835325 0.183860 0.057714 11.00000 0.02078 H4N 2 0.896076 0.078895 0.126238 11.00000 0.01408 H38 2 0.830959 0.364003 -0.019174 11.00000 0.02315 H1WA 2 0.795258 0.080142 0.199563 11.00000 0.05352 H1N 2 0.700896 0.099188 0.121185 11.00000 0.01627 H1WB 2 0.839155 0.153482 0.189495 11.00000 0.05800 H2N 2 0.686337 0.261533 0.167988 11.00000 0.05788 HKLF 4 REM pyC4Ppyr in C2/c REM R1 = 0.0644 for 3948 Fo > 4sig(Fo) and 0.1191 for all 6385 data REM 482 parameters refined using 1 restraints END WGHT 0.0831 0.0000 REM Highest difference peak 0.381, deepest hole -0.473, 1-sigma level 0.072 Q1 1 1.0363 0.1334 0.1014 11.00000 0.05 0.38 Q2 1 1.0345 0.1928 0.1278 11.00000 0.05 0.29 Q3 1 1.0220 0.0894 0.0740 11.00000 0.05 0.28 Q4 1 0.4789 0.1998 0.1111 11.00000 0.05 0.27 Q5 1 0.5512 0.2224 0.1181 11.00000 0.05 0.27 Q6 1 0.5645 0.2560 0.2505 11.00000 0.05 0.26 Q7 1 0.8525 0.3983 0.1297 11.00000 0.05 0.26 Q8 1 1.0921 0.1427 0.1290 11.00000 0.05 0.26 Q9 1 0.7820 -0.0554 0.0964 11.00000 0.05 0.25 Q10 1 0.5426 0.1443 0.1115 11.00000 0.05 0.25 Q11 1 0.6665 0.0428 0.0891 11.00000 0.05 0.24 Q12 1 0.4887 0.0903 0.1697 11.00000 0.05 0.24 Q13 1 0.6017 0.0771 0.0482 11.00000 0.05 0.24 Q14 1 0.3972 0.2471 0.1271 11.00000 0.05 0.23 Q15 1 0.8593 0.3484 0.1537 11.00000 0.05 0.23 Q16 1 0.5153 0.1717 0.1382 11.00000 0.05 0.23 Q17 1 0.8212 0.3428 0.1407 11.00000 0.05 0.23 Q18 1 0.8870 0.2902 0.1763 11.00000 0.05 0.23 Q19 1 0.8630 -0.2025 0.2085 11.00000 0.05 0.23 Q20 1 0.9410 0.2966 0.2173 11.00000 0.05 0.22 ; _shelx_res_checksum 95436 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6768(2) 0.02258(15) 0.07503(8) 0.0177(6) Uani 1 1 d . . . . . C2 C 0.5864(2) 0.01262(16) 0.04979(8) 0.0215(7) Uani 1 1 d . . . . . H2 H 0.573732 -0.027052 0.029120 0.026 Uiso 1 1 calc R U . . . C3 C 0.5152(2) 0.07163(16) 0.05988(8) 0.0229(7) Uani 1 1 d . . . . . H3 H 0.446564 0.079134 0.046911 0.028 Uiso 1 1 calc R U . . . C4 C 0.5625(2) 0.11623(16) 0.09166(8) 0.0193(7) Uani 1 1 d . . . . . C5 C 0.5228(2) 0.18443(16) 0.11583(9) 0.0230(7) Uani 1 1 d . . . . . C6 C 0.5895(2) 0.25609(16) 0.11002(8) 0.0188(6) Uani 1 1 d . . . . . C7 C 0.5876(2) 0.30848(16) 0.07766(9) 0.0232(7) Uani 1 1 d . . . . . H7 H 0.538602 0.308951 0.053680 0.028 Uiso 1 1 calc R U . . . C8 C 0.6703(2) 0.36177(16) 0.08573(8) 0.0213(7) Uani 1 1 d . . . . . H8 H 0.686790 0.404582 0.068315 0.026 Uiso 1 1 calc R U . . . C9 C 0.7228(2) 0.34106(16) 0.12299(8) 0.0188(7) Uani 1 1 d . . . . . C10 C 0.8184(2) 0.37651(15) 0.14738(8) 0.0168(6) Uani 1 1 d . . . . . C11 C 0.8972(2) 0.31275(15) 0.15890(8) 0.0164(6) Uani 1 1 d . . . . . C12 C 0.9315(2) 0.27862(16) 0.19642(8) 0.0202(7) Uani 1 1 d . . . . . H12 H 0.911038 0.292580 0.223676 0.024 Uiso 1 1 calc R U . . . C13 C 1.0029(2) 0.21888(16) 0.18727(8) 0.0195(7) Uani 1 1 d . . . . . H13 H 1.039412 0.185707 0.207312 0.023 Uiso 1 1 calc R U . . . C14 C 1.0099(2) 0.21737(15) 0.14439(8) 0.0187(6) Uani 1 1 d . . . . . C15 C 1.0713(2) 0.16638(15) 0.11577(8) 0.0197(7) Uani 1 1 d . . . . . C16 C 0.9990(2) 0.11584(15) 0.08743(8) 0.0176(6) Uani 1 1 d . . . . . C17 C 1.0036(2) 0.09474(16) 0.04623(9) 0.0236(7) Uani 1 1 d . . . . . H17 H 1.052202 0.113854 0.027307 0.028 Uiso 1 1 calc R U . . . C18 C 0.9238(2) 0.03958(16) 0.03653(8) 0.0227(7) Uani 1 1 d . . . . . H18 H 0.908889 0.015301 0.009829 0.027 Uiso 1 1 calc R U . . . C19 C 0.8713(2) 0.02691(15) 0.07201(8) 0.0165(6) Uani 1 1 d . . . . . C20 C 0.7771(2) -0.02392(15) 0.07899(8) 0.0184(7) Uani 1 1 d . . . . . C21 C 0.4091(2) 0.20213(19) 0.09898(11) 0.0358(8) Uani 1 1 d . . . . . H21A H 0.407763 0.214614 0.068762 0.054 Uiso 1 1 calc R U . . . H21B H 0.382305 0.246678 0.114375 0.054 Uiso 1 1 calc R U . . . H21C H 0.364882 0.156356 0.103087 0.054 Uiso 1 1 calc R U . . . C22 C 0.5222(2) 0.16181(17) 0.16313(9) 0.0291(8) Uani 1 1 d . . . . . H22A H 0.474287 0.117754 0.166178 0.044 Uiso 1 1 calc R U . . . H22B H 0.498548 0.206463 0.179309 0.044 Uiso 1 1 calc R U . . . H22C H 0.593240 0.146888 0.173836 0.044 Uiso 1 1 calc R U . . . C23 C 0.8679(2) 0.43740(15) 0.11842(9) 0.0225(7) Uani 1 1 d . . . . . H23A H 0.932090 0.458606 0.132904 0.034 Uiso 1 1 calc R U . . . H23B H 0.817811 0.479827 0.112070 0.034 Uiso 1 1 calc R U . . . H23C H 0.885189 0.412206 0.092016 0.034 Uiso 1 1 calc R U . . . C24 C 1.1380(2) 0.21728(16) 0.08776(9) 0.0246(7) Uani 1 1 d . . . . . H24A H 1.180705 0.183608 0.070771 0.037 Uiso 1 1 calc R U . . . H24B H 1.184101 0.251128 0.105740 0.037 Uiso 1 1 calc R U . . . H24C H 1.091577 0.249468 0.068975 0.037 Uiso 1 1 calc R U . . . C25 C 1.1447(2) 0.11359(17) 0.14346(9) 0.0295(8) Uani 1 1 d . . . . . H25A H 1.103100 0.082125 0.162005 0.044 Uiso 1 1 calc R U . . . H25B H 1.194507 0.145852 0.160701 0.044 Uiso 1 1 calc R U . . . H25C H 1.183265 0.079054 0.125372 0.044 Uiso 1 1 calc R U . . . C26 C 0.7711(2) -0.08917(16) 0.04499(8) 0.0247(7) Uani 1 1 d . . . . . H26A H 0.710126 -0.122539 0.048937 0.037 Uiso 1 1 calc R U . . . H26B H 0.835279 -0.120653 0.047781 0.037 Uiso 1 1 calc R U . . . H26C H 0.763956 -0.065563 0.016763 0.037 Uiso 1 1 calc R U . . . C27 C 0.7890(2) 0.41996(16) 0.18706(8) 0.0214(7) Uani 1 1 d . . . . . C28 C 0.6852(2) 0.43372(16) 0.19528(8) 0.0225(7) Uani 1 1 d . . . . . H28 H 0.629608 0.411688 0.177677 0.027 Uiso 1 1 calc R U . . . C29 C 0.6637(3) 0.48009(18) 0.22957(9) 0.0308(8) Uani 1 1 d . . . . . H29 H 0.592105 0.488431 0.234712 0.037 Uiso 1 1 calc R U . . . C30 C 0.8357(3) 0.4985(2) 0.24745(10) 0.0428(9) Uani 1 1 d . . . . . H30 H 0.889807 0.520426 0.265862 0.051 Uiso 1 1 calc R U . . . C31 C 0.8652(3) 0.45333(17) 0.21422(9) 0.0328(8) Uani 1 1 d . . . . . H31 H 0.937457 0.445340 0.210110 0.039 Uiso 1 1 calc R U . . . C32 C 0.7879(2) -0.06619(15) 0.12187(8) 0.0198(7) Uani 1 1 d . . . . . C33 C 0.8838(2) -0.08828(16) 0.14120(9) 0.0266(7) Uani 1 1 d . . . . . H33 H 0.947176 -0.074468 0.129000 0.032 Uiso 1 1 calc R U . . . C34 C 0.8867(3) -0.13047(17) 0.17826(9) 0.0324(8) Uani 1 1 d . . . . . H34 H 0.953598 -0.144085 0.191227 0.039 Uiso 1 1 calc R U . . . C35 C 0.7095(3) -0.13313(18) 0.17815(9) 0.0326(8) Uani 1 1 d . . . . . H35 H 0.647534 -0.149227 0.190669 0.039 Uiso 1 1 calc R U . . . C36 C 0.6991(2) -0.08990(16) 0.14126(9) 0.0250(7) Uani 1 1 d . . . . . H36 H 0.631285 -0.076460 0.129213 0.030 Uiso 1 1 calc R U . . . C37 C 0.7949(2) 0.21154(17) 0.03356(9) 0.0219(7) Uani 1 1 d . . . . . C38 C 0.7929(2) 0.31704(17) -0.01263(8) 0.0214(7) Uani 1 1 d . . . . . N1 N 0.66087(19) 0.08567(13) 0.10050(7) 0.0178(6) Uani 1 1 d . . . . . N2 N 0.67349(17) 0.27597(13) 0.13773(7) 0.0183(5) Uani 1 1 d . . . . . N3 N 0.94525(17) 0.27444(13) 0.12733(7) 0.0164(5) Uani 1 1 d . . . . . N4 N 0.91745(18) 0.07478(13) 0.10291(7) 0.0185(6) Uani 1 1 d . . . . . N5 N 0.7359(2) 0.51344(16) 0.25554(8) 0.0389(7) Uani 1 1 d . . . . . N6 N 0.8020(2) -0.15334(15) 0.19704(8) 0.0366(7) Uani 1 1 d . . . . . N7 N 0.83934(18) 0.27877(13) 0.02116(7) 0.0201(6) Uani 1 1 d . . . . . O1 O 0.92382(15) 0.30667(11) 0.04090(5) 0.0246(5) Uani 1 1 d . . . . . O1W O 0.80383(16) 0.10810(13) 0.17620(6) 0.0234(5) Uani 1 1 d . . . . . O1A O 0.6824(2) 0.25180(17) 0.23222(7) 0.0661(9) Uani 1 1 d D . . . . H1A H 0.700783 0.291295 0.246601 0.099 Uiso 1 1 d R U . . . C1A C 0.6789(5) 0.1932(3) 0.25618(17) 0.116(2) Uani 1 1 d D . . . . H1A1 H 0.738680 0.158924 0.251891 0.174 Uiso 1 1 calc R U . . . H1A2 H 0.613241 0.164697 0.249542 0.174 Uiso 1 1 calc R U . . . H1A3 H 0.682007 0.210531 0.285719 0.174 Uiso 1 1 calc R U . . . H3N H 0.938(2) 0.2874(16) 0.0988(9) 0.029(8) Uiso 1 1 d . . . . . H37 H 0.835(2) 0.1839(14) 0.0577(8) 0.021(7) Uiso 1 1 d . . . . . H4N H 0.896(2) 0.0789(15) 0.1262(8) 0.014(8) Uiso 1 1 d . . . . . H38 H 0.831(2) 0.3640(17) -0.0192(8) 0.023(8) Uiso 1 1 d . . . . . H1WA H 0.795(3) 0.080(2) 0.1996(11) 0.054(11) Uiso 1 1 d . . . . . H1N H 0.701(2) 0.0992(15) 0.1212(8) 0.016(8) Uiso 1 1 d . . . . . H1WB H 0.839(3) 0.153(2) 0.1895(11) 0.058(11) Uiso 1 1 d . . . . . H2N H 0.686(3) 0.2615(19) 0.1680(11) 0.058(11) 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 0.0256(17) 0.0135(15) 0.0146(14) -0.0019(12) 0.0057(12) -0.0029(13) C2 0.0240(17) 0.0214(17) 0.0193(15) -0.0061(12) 0.0024(13) -0.0066(13) C3 0.0174(16) 0.0261(17) 0.0248(16) 0.0017(13) -0.0020(13) -0.0042(14) C4 0.0149(16) 0.0198(16) 0.0237(16) 0.0009(12) 0.0046(12) -0.0035(13) C5 0.0174(16) 0.0189(17) 0.0327(17) -0.0021(13) 0.0025(13) 0.0002(13) C6 0.0132(15) 0.0174(16) 0.0257(16) -0.0029(13) 0.0015(12) 0.0021(12) C7 0.0198(17) 0.0249(17) 0.0239(16) -0.0002(13) -0.0047(13) 0.0006(14) C8 0.0251(17) 0.0153(16) 0.0237(16) 0.0012(13) 0.0021(13) 0.0023(13) C9 0.0198(16) 0.0136(16) 0.0234(16) -0.0028(12) 0.0039(12) 0.0025(13) C10 0.0175(15) 0.0140(15) 0.0190(14) -0.0033(12) 0.0022(12) 0.0016(12) C11 0.0182(15) 0.0145(15) 0.0166(15) -0.0040(12) 0.0020(12) -0.0039(12) C12 0.0229(17) 0.0233(17) 0.0144(14) -0.0039(12) 0.0024(12) -0.0036(13) C13 0.0203(16) 0.0215(16) 0.0165(15) 0.0024(12) -0.0001(12) -0.0016(13) C14 0.0171(16) 0.0170(16) 0.0213(15) -0.0018(12) -0.0024(12) -0.0019(13) C15 0.0203(16) 0.0166(16) 0.0224(15) 0.0007(12) 0.0027(12) 0.0021(13) C16 0.0159(15) 0.0129(15) 0.0247(16) -0.0008(12) 0.0068(12) 0.0020(12) C17 0.0270(18) 0.0228(17) 0.0224(16) -0.0019(13) 0.0112(13) -0.0018(14) C18 0.0253(17) 0.0219(17) 0.0218(15) -0.0068(13) 0.0079(13) -0.0039(14) C19 0.0173(16) 0.0137(15) 0.0188(14) -0.0037(12) 0.0025(12) 0.0041(12) C20 0.0244(17) 0.0132(15) 0.0183(14) -0.0011(12) 0.0061(12) -0.0028(13) C21 0.0190(18) 0.032(2) 0.057(2) -0.0060(16) 0.0022(15) 0.0010(15) C22 0.0279(18) 0.0250(18) 0.0359(18) -0.0048(14) 0.0139(14) -0.0047(14) C23 0.0214(17) 0.0179(16) 0.0288(16) -0.0003(13) 0.0064(13) 0.0026(13) C24 0.0180(16) 0.0213(17) 0.0352(17) -0.0031(13) 0.0073(13) -0.0014(13) C25 0.0247(18) 0.0249(18) 0.0385(19) -0.0003(14) -0.0007(14) 0.0074(14) C26 0.0318(18) 0.0190(17) 0.0240(16) -0.0059(13) 0.0074(13) -0.0036(14) C27 0.0250(17) 0.0171(16) 0.0222(15) -0.0017(12) 0.0027(13) 0.0048(13) C28 0.0223(17) 0.0229(17) 0.0225(15) 0.0019(13) 0.0020(13) 0.0022(14) C29 0.0315(19) 0.036(2) 0.0259(17) 0.0007(15) 0.0102(15) 0.0115(16) C30 0.037(2) 0.048(2) 0.042(2) -0.0236(17) -0.0126(16) 0.0114(18) C31 0.0293(19) 0.0307(19) 0.0380(19) -0.0194(15) -0.0010(15) 0.0066(15) C32 0.0281(18) 0.0093(15) 0.0219(15) -0.0055(12) 0.0018(13) -0.0005(13) C33 0.0304(19) 0.0187(17) 0.0312(17) -0.0017(14) 0.0055(14) 0.0000(14) C34 0.040(2) 0.0241(19) 0.0331(18) 0.0010(15) 0.0010(15) 0.0002(15) C35 0.042(2) 0.0289(19) 0.0274(18) 0.0020(14) 0.0056(15) -0.0084(16) C36 0.0279(18) 0.0216(17) 0.0261(17) 0.0020(13) 0.0057(14) -0.0047(14) C37 0.0248(18) 0.0211(17) 0.0202(16) 0.0044(13) 0.0047(13) -0.0001(14) C38 0.0267(18) 0.0209(18) 0.0169(15) 0.0041(13) 0.0037(13) 0.0027(15) N1 0.0184(14) 0.0195(14) 0.0153(13) -0.0027(11) 0.0006(11) -0.0029(11) N2 0.0167(13) 0.0173(14) 0.0209(13) 0.0006(10) 0.0006(10) -0.0005(10) N3 0.0174(13) 0.0174(13) 0.0146(13) -0.0007(10) 0.0021(10) 0.0007(10) N4 0.0227(14) 0.0156(14) 0.0180(14) -0.0020(11) 0.0074(11) -0.0019(11) N5 0.0428(19) 0.0465(18) 0.0269(15) -0.0117(13) -0.0019(13) 0.0179(15) N6 0.050(2) 0.0333(17) 0.0258(15) 0.0070(12) 0.0009(14) -0.0055(15) N7 0.0233(14) 0.0207(14) 0.0167(13) 0.0002(10) 0.0051(11) 0.0009(11) O1 0.0247(12) 0.0299(12) 0.0189(11) 0.0012(9) -0.0016(9) -0.0062(10) O1W 0.0288(13) 0.0259(13) 0.0158(11) 0.0023(10) 0.0036(9) -0.0058(10) O1A 0.100(2) 0.070(2) 0.0297(14) -0.0087(14) 0.0152(14) -0.0500(18) C1A 0.184(7) 0.079(4) 0.086(4) -0.009(3) 0.013(4) 0.002(4) 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 C2 C1 N1 106.8(2) . . ? C2 C1 C20 131.3(2) . . ? N1 C1 C20 121.9(2) . . ? C1 C2 C3 108.0(2) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? C4 C3 C2 108.0(3) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C3 C4 N1 106.7(2) . . ? C3 C4 C5 131.4(3) . . ? N1 C4 C5 121.9(2) . . ? C4 C5 C6 110.9(2) . . ? C4 C5 C21 108.6(2) . . ? C6 C5 C21 108.8(2) . . ? C4 C5 C22 108.8(2) . . ? C6 C5 C22 111.2(2) . . ? C21 C5 C22 108.4(2) . . ? C7 C6 N2 106.8(2) . . ? C7 C6 C5 130.2(3) . . ? N2 C6 C5 122.8(2) . . ? C6 C7 C8 108.5(3) . . ? C6 C7 H7 125.8 . . ? C8 C7 H7 125.8 . . ? C9 C8 C7 107.8(2) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C8 C9 N2 107.2(2) . . ? C8 C9 C10 131.5(3) . . ? N2 C9 C10 121.2(2) . . ? C11 C10 C9 109.3(2) . . ? C11 C10 C27 110.5(2) . . ? C9 C10 C27 112.1(2) . . ? C11 C10 C23 109.7(2) . . ? C9 C10 C23 108.2(2) . . ? C27 C10 C23 107.0(2) . . ? C12 C11 N3 107.2(2) . . ? C12 C11 C10 133.3(2) . . ? N3 C11 C10 119.4(2) . . ? C11 C12 C13 107.6(2) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? C14 C13 C12 107.8(2) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? N3 C14 C13 107.5(2) . . ? N3 C14 C15 119.9(2) . . ? C13 C14 C15 132.6(3) . . ? C16 C15 C14 111.4(2) . . ? C16 C15 C25 108.9(2) . . ? C14 C15 C25 108.5(2) . . ? C16 C15 C24 108.7(2) . . ? C14 C15 C24 110.3(2) . . ? C25 C15 C24 108.9(2) . . ? C17 C16 N4 106.9(2) . . ? C17 C16 C15 131.0(2) . . ? N4 C16 C15 121.8(2) . . ? C16 C17 C18 108.0(2) . . ? C16 C17 H17 126.0 . . ? C18 C17 H17 126.0 . . ? C19 C18 C17 108.4(2) . . ? C19 C18 H18 125.8 . . ? C17 C18 H18 125.8 . . ? C18 C19 N4 106.3(2) . . ? C18 C19 C20 130.7(2) . . ? N4 C19 C20 122.9(2) . . ? C1 C20 C19 111.3(2) . . ? C1 C20 C32 110.3(2) . . ? C19 C20 C32 112.1(2) . . ? C1 C20 C26 108.8(2) . . ? C19 C20 C26 108.4(2) . . ? C32 C20 C26 105.7(2) . . ? 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 . . ? C5 C22 H22A 109.5 . . ? C5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C5 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 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 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 . . ? C31 C27 C28 117.0(3) . . ? C31 C27 C10 120.8(3) . . ? C28 C27 C10 121.9(2) . . ? C27 C28 C29 119.2(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? N5 C29 C28 124.6(3) . . ? N5 C29 H29 117.7 . . ? C28 C29 H29 117.7 . . ? N5 C30 C31 124.5(3) . . ? N5 C30 H30 117.8 . . ? C31 C30 H30 117.8 . . ? C27 C31 C30 119.4(3) . . ? C27 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C36 116.7(3) . . ? C33 C32 C20 122.8(3) . . ? C36 C32 C20 120.3(3) . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? N6 C34 C33 124.2(3) . . ? N6 C34 H34 117.9 . . ? C33 C34 H34 117.9 . . ? N6 C35 C36 123.3(3) . . ? N6 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C32 119.9(3) . . ? C35 C36 H36 120.1 . . ? C32 C36 H36 120.1 . . ? N7 C37 C38 121.0(3) . 7_655 ? N7 C37 H37 114.7(15) . . ? C38 C37 H37 124.2(15) 7_655 . ? C37 C38 N7 120.9(3) 7_655 . ? C37 C38 H38 127.2(15) 7_655 . ? N7 C38 H38 111.9(15) . . ? C4 N1 C1 110.6(2) . . ? C4 N1 H1N 123.8(19) . . ? C1 N1 H1N 124.9(19) . . ? C9 N2 C6 109.7(2) . . ? C9 N2 H2N 119(2) . . ? C6 N2 H2N 128(2) . . ? C14 N3 C11 109.9(2) . . ? C14 N3 H3N 124.9(17) . . ? C11 N3 H3N 125.0(17) . . ? C16 N4 C19 110.4(2) . . ? C16 N4 H4N 126.4(19) . . ? C19 N4 H4N 123.2(19) . . ? C29 N5 C30 115.4(3) . . ? C34 N6 C35 116.5(3) . . ? O1 N7 C37 121.6(2) . . ? O1 N7 C38 120.3(2) . . ? C37 N7 C38 118.2(3) . . ? H1WA O1W H1WB 99(3) . . ? C1A O1A H1A 109.6 . . ? O1A C1A H1A1 109.5 . . ? O1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? O1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.368(4) . ? C1 N1 1.372(3) . ? C1 C20 1.505(4) . ? C2 C3 1.410(4) . ? C2 H2 0.9500 . ? C3 C4 1.370(4) . ? C3 H3 0.9500 . ? C4 N1 1.371(3) . ? C4 C5 1.504(4) . ? C5 C6 1.513(4) . ? C5 C21 1.541(4) . ? C5 C22 1.549(4) . ? C6 C7 1.361(4) . ? C6 N2 1.380(3) . ? C7 C8 1.406(4) . ? C7 H7 0.9500 . ? C8 C9 1.363(4) . ? C8 H8 0.9500 . ? C9 N2 1.378(3) . ? C9 C10 1.525(4) . ? C10 C11 1.512(4) . ? C10 C27 1.530(4) . ? C10 C23 1.552(4) . ? C11 C12 1.369(4) . ? C11 N3 1.376(3) . ? C12 C13 1.413(4) . ? C12 H12 0.9500 . ? C13 C14 1.368(4) . ? C13 H13 0.9500 . ? C14 N3 1.366(3) . ? C14 C15 1.516(4) . ? C15 C16 1.514(4) . ? C15 C25 1.533(4) . ? C15 C24 1.542(4) . ? C16 C17 1.360(4) . ? C16 N4 1.375(3) . ? C17 C18 1.408(4) . ? C17 H17 0.9500 . ? C18 C19 1.365(3) . ? C18 H18 0.9500 . ? C19 N4 1.378(3) . ? C19 C20 1.514(4) . ? C20 C32 1.537(4) . ? C20 C26 1.551(4) . ? 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 C31 1.377(4) . ? C27 C28 1.387(4) . ? C28 C29 1.389(4) . ? C28 H28 0.9500 . ? C29 N5 1.322(4) . ? C29 H29 0.9500 . ? C30 N5 1.342(4) . ? C30 C31 1.379(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.383(4) . ? C32 C36 1.386(4) . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 N6 1.329(4) . ? C34 H34 0.9500 . ? C35 N6 1.332(4) . ? C35 C36 1.382(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N7 1.354(3) . ? C37 C38 1.354(4) 7_655 ? C37 H37 1.01(3) . ? C38 N7 1.356(3) . ? C38 H38 0.97(3) . ? N1 H1N 0.84(3) . ? N2 H2N 0.99(3) . ? N3 H3N 0.93(3) . ? N4 H4N 0.81(3) . ? N7 O1 1.299(3) . ? O1W H1WA 0.89(4) . ? O1W H1WB 0.98(4) . ? O1A C1A 1.261(5) . ? O1A H1A 0.8400 . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? 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 O1A H1A N6 0.84 2.02 2.765(3) 146.6 4_655 C1A H1A1 N5 0.98 2.53 3.296(6) 135.3 4_645 C1A H1A3 N6 0.98 2.40 3.019(6) 120.6 4_655 N3 H3N N7 0.93(3) 2.69(3) 3.538(3) 152(2) . N3 H3N O1 0.93(3) 1.86(3) 2.788(3) 176(3) . N4 H4N O1W 0.81(3) 2.10(3) 2.879(3) 162(3) . O1W H1WA N5 0.89(4) 1.89(4) 2.778(3) 172(3) 4_645 N1 H1N O1W 0.84(3) 2.11(3) 2.936(3) 168(3) . N2 H2N O1A 0.99(3) 2.05(4) 3.017(3) 165(3) . 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 0.9(3) . . . . ? C20 C1 C2 C3 178.0(2) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C2 C3 C4 N1 0.6(3) . . . . ? C2 C3 C4 C5 -177.4(3) . . . . ? C3 C4 C5 C6 -120.0(3) . . . . ? N1 C4 C5 C6 62.3(3) . . . . ? C3 C4 C5 C21 -0.5(4) . . . . ? N1 C4 C5 C21 -178.2(2) . . . . ? C3 C4 C5 C22 117.4(3) . . . . ? N1 C4 C5 C22 -60.4(3) . . . . ? C4 C5 C6 C7 80.9(4) . . . . ? C21 C5 C6 C7 -38.4(4) . . . . ? C22 C5 C6 C7 -157.8(3) . . . . ? C4 C5 C6 N2 -93.6(3) . . . . ? C21 C5 C6 N2 147.1(3) . . . . ? C22 C5 C6 N2 27.7(3) . . . . ? N2 C6 C7 C8 -0.7(3) . . . . ? C5 C6 C7 C8 -175.9(3) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C7 C8 C9 N2 0.1(3) . . . . ? C7 C8 C9 C10 179.7(3) . . . . ? C8 C9 C10 C11 -130.2(3) . . . . ? N2 C9 C10 C11 49.3(3) . . . . ? C8 C9 C10 C27 106.9(3) . . . . ? N2 C9 C10 C27 -73.6(3) . . . . ? C8 C9 C10 C23 -10.8(4) . . . . ? N2 C9 C10 C23 168.7(2) . . . . ? C9 C10 C11 C12 -110.5(3) . . . . ? C27 C10 C11 C12 13.4(4) . . . . ? C23 C10 C11 C12 131.1(3) . . . . ? C9 C10 C11 N3 65.6(3) . . . . ? C27 C10 C11 N3 -170.5(2) . . . . ? C23 C10 C11 N3 -52.8(3) . . . . ? N3 C11 C12 C13 0.7(3) . . . . ? C10 C11 C12 C13 177.1(3) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C12 C13 C14 N3 0.1(3) . . . . ? C12 C13 C14 C15 -179.0(3) . . . . ? N3 C14 C15 C16 -65.6(3) . . . . ? C13 C14 C15 C16 113.5(3) . . . . ? N3 C14 C15 C25 174.5(2) . . . . ? C13 C14 C15 C25 -6.5(4) . . . . ? N3 C14 C15 C24 55.3(3) . . . . ? C13 C14 C15 C24 -125.7(3) . . . . ? C14 C15 C16 C17 141.0(3) . . . . ? C25 C15 C16 C17 -99.2(3) . . . . ? C24 C15 C16 C17 19.3(4) . . . . ? C14 C15 C16 N4 -46.3(3) . . . . ? C25 C15 C16 N4 73.4(3) . . . . ? C24 C15 C16 N4 -168.1(2) . . . . ? N4 C16 C17 C18 -0.3(3) . . . . ? C15 C16 C17 C18 173.2(3) . . . . ? C16 C17 C18 C19 -0.4(3) . . . . ? C17 C18 C19 N4 1.0(3) . . . . ? C17 C18 C19 C20 177.5(3) . . . . ? C2 C1 C20 C19 124.2(3) . . . . ? N1 C1 C20 C19 -59.0(3) . . . . ? C2 C1 C20 C32 -110.7(3) . . . . ? N1 C1 C20 C32 66.0(3) . . . . ? C2 C1 C20 C26 4.9(4) . . . . ? N1 C1 C20 C26 -178.4(2) . . . . ? C18 C19 C20 C1 -96.0(3) . . . . ? N4 C19 C20 C1 80.1(3) . . . . ? C18 C19 C20 C32 140.0(3) . . . . ? N4 C19 C20 C32 -43.9(3) . . . . ? C18 C19 C20 C26 23.7(4) . . . . ? N4 C19 C20 C26 -160.3(2) . . . . ? C11 C10 C27 C31 55.2(3) . . . . ? C9 C10 C27 C31 177.4(3) . . . . ? C23 C10 C27 C31 -64.2(3) . . . . ? C11 C10 C27 C28 -130.8(3) . . . . ? C9 C10 C27 C28 -8.6(4) . . . . ? C23 C10 C27 C28 109.8(3) . . . . ? C31 C27 C28 C29 0.6(4) . . . . ? C10 C27 C28 C29 -173.7(2) . . . . ? C27 C28 C29 N5 0.4(4) . . . . ? C28 C27 C31 C30 -0.5(4) . . . . ? C10 C27 C31 C30 173.8(3) . . . . ? N5 C30 C31 C27 -0.5(5) . . . . ? C1 C20 C32 C33 -155.1(2) . . . . ? C19 C20 C32 C33 -30.5(3) . . . . ? C26 C20 C32 C33 87.3(3) . . . . ? C1 C20 C32 C36 30.5(3) . . . . ? C19 C20 C32 C36 155.0(2) . . . . ? C26 C20 C32 C36 -87.1(3) . . . . ? C36 C32 C33 C34 -1.2(4) . . . . ? C20 C32 C33 C34 -175.8(2) . . . . ? C32 C33 C34 N6 1.2(5) . . . . ? N6 C35 C36 C32 0.7(4) . . . . ? C33 C32 C36 C35 0.3(4) . . . . ? C20 C32 C36 C35 175.0(2) . . . . ? C3 C4 N1 C1 -0.1(3) . . . . ? C5 C4 N1 C1 178.1(2) . . . . ? C2 C1 N1 C4 -0.5(3) . . . . ? C20 C1 N1 C4 -177.9(2) . . . . ? C8 C9 N2 C6 -0.6(3) . . . . ? C10 C9 N2 C6 179.8(2) . . . . ? C7 C6 N2 C9 0.8(3) . . . . ? C5 C6 N2 C9 176.4(2) . . . . ? C13 C14 N3 C11 0.3(3) . . . . ? C15 C14 N3 C11 179.5(2) . . . . ? C12 C11 N3 C14 -0.6(3) . . . . ? C10 C11 N3 C14 -177.6(2) . . . . ? C17 C16 N4 C19 0.9(3) . . . . ? C15 C16 N4 C19 -173.3(2) . . . . ? C18 C19 N4 C16 -1.2(3) . . . . ? C20 C19 N4 C16 -178.1(2) . . . . ? C28 C29 N5 C30 -1.4(5) . . . . ? C31 C30 N5 C29 1.5(5) . . . . ? C33 C34 N6 C35 -0.2(4) . . . . ? C36 C35 N6 C34 -0.8(4) . . . . ? C38 C37 N7 O1 -179.8(2) 7_655 . . . ? C38 C37 N7 C38 0.5(4) 7_655 . . . ? C37 C38 N7 O1 179.8(2) 7_655 . . . ? C37 C38 N7 C37 -0.5(4) 7_655 . . . ?