#------------------------------------------------------------------------------ #$Date: 2020-05-04 05:49:44 +0300 (Mon, 04 May 2020) $ #$Revision: 251489 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557804.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_1557804 loop_ _publ_author_name 'Cobos, Katherine' 'Rodr\'iguez, Rafael' 'Domarco, Olaya' 'Fern\'andez, Berta' 'Qui\~no\'a, Emilio' 'Riguera, Ricardo' 'Freire, F\'elix' _publ_section_title ; Polymeric Helical Structures \`a la Carte by Rational Design of Monomers ; _journal_issue 8 _journal_name_full Macromolecules _journal_page_first 3182 _journal_paper_doi 10.1021/acs.macromol.0c00085 _journal_volume 53 _journal_year 2020 _chemical_absolute_configuration syn _chemical_formula_moiety 'C16 H13 N O2' _chemical_formula_sum 'C16 H13 N O2' _chemical_formula_weight 251.27 _chemical_name_common R-o-MA _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2016-05-04T18:21:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 99.117(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.191(2) _cell_length_b 9.5150(11) _cell_length_c 7.2721(10) _cell_measurement_reflns_used 1872 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.93 _cell_measurement_theta_min 2.4 _cell_measurement_wavelength 0.71073 _cell_volume 1311.1(3) _computing_cell_refinement 'SAINT V8.37A integration software' _computing_data_collection 'Bruker APEX2 software' _computing_data_reduction 'SORTAV (Blessing, 1995)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'APEX-II CCD' _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method '\f or \w oscillation scans' _diffrn_orient_matrix_UB_11 0.035243 _diffrn_orient_matrix_UB_12 -0.078219 _diffrn_orient_matrix_UB_13 0.013265 _diffrn_orient_matrix_UB_21 0.011692 _diffrn_orient_matrix_UB_22 0.019444 _diffrn_orient_matrix_UB_23 0.136548 _diffrn_orient_matrix_UB_31 -0.037501 _diffrn_orient_matrix_UB_32 -0.067447 _diffrn_orient_matrix_UB_33 0.023982 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_unetI/netI 0.0924 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 13501 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.615 _diffrn_reflns_theta_min 2.15 _diffrn_source 'sealed x-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.196 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details ; Flack x determined using 845 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.7(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 178 _refine_ls_number_reflns 3979 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.963 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0511 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.1038 _reflns_Friedel_coverage 0.868 _reflns_Friedel_fraction_full 1 _reflns_Friedel_fraction_max 0.965 _reflns_number_gt 2673 _reflns_number_total 3979 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ma0c00085_si_005.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 1557803--1557808.cif.' _cod_original_sg_symbol_H-M 'C 2' _cod_database_code 1557804 _shelx_estimated_absorpt_t_min 0.973 _shelx_estimated_absorpt_t_max 0.992 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in C2 CELL 0.71073 19.1911 9.5150 7.2721 90.000 99.117 90.000 ZERR 4.00 0.0021 0.0011 0.0010 0.000 0.008 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H N O UNIT 64 52 4 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.090 0.120 0.320 ACTA BOND $H REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y+1/2, -z HTAB O1 O3_$1 HTAB N4 O1 CONF LIST 4 WPDB -2 L.S. 12 TEMP -173.00 WGHT 0.041900 FVAR 0.41071 O1 4 0.283474 0.569183 -0.020197 11.00000 0.02069 0.01966 = 0.02593 0.00790 0.00379 0.00168 AFIX 148 H1A 2 0.246252 0.619818 -0.043706 11.00000 -1.50000 AFIX 0 C1 1 0.266054 0.437310 0.051465 11.00000 0.01894 0.01646 = 0.01997 0.00198 0.00153 -0.00158 AFIX 13 H1 2 0.234712 0.384360 -0.047896 11.00000 -1.20000 AFIX 0 C2 1 0.334255 0.354862 0.108764 11.00000 0.01903 0.01986 = 0.01621 0.00088 0.00365 -0.00143 O3 4 0.334051 0.225746 0.124375 11.00000 0.02262 0.01529 = 0.02606 -0.00001 0.00251 -0.00031 N4 3 0.391643 0.437173 0.148069 11.00000 0.01711 0.01441 = 0.02418 0.00232 0.00011 -0.00043 H4 2 0.384568 0.522379 0.123373 11.00000 0.02598 C5 1 0.462774 0.401392 0.211591 11.00000 0.01649 0.02095 = 0.01965 0.00140 0.00242 -0.00014 C6 1 0.487243 0.264498 0.230745 11.00000 0.02273 0.01858 = 0.03943 0.00538 0.00002 -0.00111 AFIX 43 H6 2 0.455318 0.188189 0.204093 11.00000 -1.20000 AFIX 0 C7 1 0.558695 0.238915 0.289114 11.00000 0.02799 0.02495 = 0.04746 0.00662 0.00010 0.00185 AFIX 43 H7 2 0.575388 0.144848 0.301123 11.00000 -1.20000 AFIX 0 C8 1 0.605752 0.349113 0.329903 11.00000 0.02013 0.03423 = 0.03371 0.00371 0.00008 0.00377 AFIX 43 H8 2 0.654444 0.330658 0.369895 11.00000 -1.20000 AFIX 0 C9 1 0.581711 0.485342 0.312282 11.00000 0.01924 0.03034 = 0.02525 -0.00253 0.00352 -0.00186 AFIX 43 H9 2 0.614013 0.560842 0.340714 11.00000 -1.20000 AFIX 0 C10 1 0.510406 0.513820 0.253110 11.00000 0.01893 0.02267 = 0.01719 -0.00086 0.00273 -0.00010 C11 1 0.484697 0.656184 0.233720 11.00000 0.01744 0.02666 = 0.02792 -0.00625 0.00453 -0.00455 C12 1 0.461944 0.771777 0.212747 11.00000 0.03008 0.02429 = 0.05586 -0.00403 0.00658 0.00073 AFIX 163 H12 2 0.443693 0.864502 0.195924 11.00000 -1.20000 AFIX 0 C13 1 0.229372 0.452065 0.221108 11.00000 0.01516 0.01625 = 0.02018 0.00337 -0.00015 0.00394 C14 1 0.252803 0.554461 0.354559 11.00000 0.01894 0.01793 = 0.02440 0.00041 -0.00021 -0.00369 AFIX 43 H14 2 0.289655 0.616600 0.334827 11.00000 -1.20000 AFIX 0 C15 1 0.223112 0.566296 0.514158 11.00000 0.02157 0.02383 = 0.02286 -0.00317 -0.00114 -0.00034 AFIX 43 H15 2 0.239499 0.636216 0.603915 11.00000 -1.20000 AFIX 0 C16 1 0.169114 0.475820 0.543894 11.00000 0.02324 0.02303 = 0.02241 0.00002 0.00501 0.00394 AFIX 43 H16 2 0.148779 0.483481 0.654379 11.00000 -1.20000 AFIX 0 C17 1 0.145090 0.374979 0.412971 11.00000 0.01861 0.01932 = 0.02829 0.00018 0.00415 -0.00168 AFIX 43 H17 2 0.108071 0.313393 0.433105 11.00000 -1.20000 AFIX 0 C18 1 0.175015 0.363263 0.251231 11.00000 0.01688 0.01568 = 0.02491 -0.00153 -0.00042 0.00018 AFIX 43 H18 2 0.158084 0.294022 0.161014 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM shelxt_a.res in C2 REM R1 = 0.0511 for 2673 Fo > 4sig(Fo) and 0.0904 for all 3979 data REM 178 parameters refined using 1 restraints END WGHT 0.0419 0.0000 REM Highest difference peak 0.196, deepest hole -0.229, 1-sigma level 0.053 Q1 1 0.4544 0.9815 0.2681 11.00000 0.05 0.20 Q2 1 0.5441 0.0779 0.0403 11.00000 0.05 0.19 Q3 1 0.4579 0.9615 0.4365 11.00000 0.05 0.19 Q4 1 0.0715 0.3973 0.5245 11.00000 0.05 0.18 Q5 1 0.2242 0.6782 0.5621 11.00000 0.05 0.18 Q6 1 0.1192 0.4614 0.6157 11.00000 0.05 0.18 Q7 1 0.1907 0.4442 0.2112 11.00000 0.05 0.18 Q8 1 0.2104 0.2434 0.0590 11.00000 0.05 0.17 Q9 1 0.3413 0.1622 -0.1163 11.00000 0.05 0.17 Q10 1 0.5519 0.4767 0.0529 11.00000 0.05 0.17 Q11 1 0.0902 0.2602 0.1626 11.00000 0.05 0.17 Q12 1 0.5369 0.7957 0.1398 11.00000 0.05 0.17 Q13 1 0.4686 0.0535 0.1982 11.00000 0.05 0.17 Q14 1 0.1196 0.4438 0.7192 11.00000 0.05 0.16 Q15 1 0.3434 0.7000 0.3285 11.00000 0.05 0.16 Q16 1 0.6113 0.5967 0.4672 11.00000 0.05 0.16 Q17 1 0.2636 0.5581 0.7376 11.00000 0.05 0.16 Q18 1 0.7078 0.2555 0.3339 11.00000 0.05 0.16 Q19 1 0.3445 0.5382 0.2374 11.00000 0.05 0.16 Q20 1 0.1912 0.5529 0.6928 11.00000 0.05 0.16 ; _shelx_res_checksum 82484 _shelx_hkl_file ; -27 1 1 19.1341 8.22991 1 -27 -1 1 15.9194 6.7403 1 -27 1 2 11.9078 7.01715 1 -27 -1 2 11.2803 5.76387 1 -27 -1 3 8.42864 5.44701 1 -27 1 3 7.10456 6.35842 1 -26 0 1 1.75288 4.55448 1 -26 0 2 0.73247 4.38717 1 -26 0 3 35.6011 8.84915 1 -26 0 4-0.43196 3.91648 1 -26 -2 1 34.2373 7.83015 1 -26 -2 2 4.23974 4.67557 1 -26 -2 2-1.75829 3.79804 1 -26 -2 3 4.98062 5.1839 1 -26 2 3 4.42893 7.26032 1 -26 -2 3 4.85375 4.2691 1 -26 -2 4 1.80493 4.50257 1 -26 -2 4 1.34808 3.62881 1 -26 -4 1 23.7247 6.12431 1 26 -4 -1 16.6946 8.62054 1 -26 -4 1 24.4249 6.48394 1 26 -4 -2 2.07835 6.6432 1 -26 -4 2 8.8053 4.16932 1 26 -4 -2 5.03085 6.23238 1 -26 -4 2 15.3373 4.49829 1 -25 -1 1-0.69461 3.88826 1 -25 1 1 2.06116 5.01064 1 -25 1 2 4.57577 5.41221 1 -25 -1 2 2.26365 4.0957 1 -25 1 3-5.11687 4.17918 1 -25 -1 3 0.60531 3.65622 1 -25 -1 3 3.16649 5.53287 1 -25 -1 4 8.34949 5.11584 1 -25 1 4 12.3766 6.59912 1 -25 1 5 7.1033 6.69839 1 -25 -1 5 9.26157 5.13482 1 -25 -3 1 81.0603 10.6158 1 25 -3 -1 77.742 13.6757 1 -25 -3 1 75.8552 9.65484 1 -25 -3 2-0.20597 2.7799 1 -25 -3 2 4.48304 3.87994 1 25 -3 -2 2.8001 5.76126 1 -25 -3 3 9.85332 4.66447 1 25 -3 -3 17.2667 7.36795 1 -25 -3 3 10.7725 4.40636 1 25 -3 -4 7.39652 6.40979 1 -25 -3 4 0.43877 2.93865 1 -25 -3 4-0.77111 3.69682 1 -25 -3 5 21.0481 5.78201 1 25 -5 -1 40.1221 11.2625 1 -25 -5 1 21.2583 5.00777 1 -25 -5 1 40.1257 6.44907 1 25 -5 -2-1.91151 5.75943 1 -25 -5 2 5.76311 2.9335 1 -25 -5 2 12.0406 3.67884 1 25 -5 -2 11.7239 8.04465 1 -25 -5 3 24.6433 4.06129 1 -25 -5 3 22.8932 4.00686 1 25 -5 -3 9.45067 7.21792 1 -24 0 1 32.2466 8.3143 1 -24 0 2 10.2991 5.08459 1 -24 0 3 2.4507 3.8638 1 -24 0 4 -0.306 3.45356 1 -24 0 5 0.68456 4.97011 1 -24 0 6 2.09594 4.33012 1 -24 -2 1 8.82872 3.99875 1 24 -2 -1 20.1449 7.36092 1 -24 2 1 22.3158 7.87979 1 -24 -2 1 11.7604 4.85253 1 24 -2 -2-0.72601 3.71232 1 -24 2 2 3.8999 5.63082 1 -24 -2 2 5.47331 3.83543 1 -24 -2 2-0.52689 3.14801 1 -24 -2 3 28.5587 6.61025 1 -24 -2 3 36.3751 7.37812 1 -24 2 3 48.0006 9.91462 1 24 -2 -3 50.8008 10.4044 1 -24 -2 4 5.43913 3.85906 1 -24 2 4-3.56435 4.79425 1 -24 -2 4 8.93135 5.24153 1 -24 -2 5-2.63383 3.71782 1 -24 2 5 3.41031 5.82239 1 -24 -2 5 0.51377 3.6033 1 -24 -2 6 13.7499 5.51549 1 -24 4 1 27.4089 13.6322 1 24 -4 -1 23.5131 7.33073 1 -24 -4 1 22.6688 5.42754 1 -24 -4 1 18.6461 5.05368 1 -24 -4 2 4.86545 3.28173 1 24 -4 -2 -0.0469 5.4368 1 -24 -4 2 10.0826 3.99026 1 24 -4 -2 8.66316 6.87089 1 -24 -4 3 0.64509 2.54029 1 24 -4 -3-0.56636 4.69823 1 -24 -4 3-0.05587 2.45183 1 -24 -4 4 2.72126 3.01566 1 -24 -4 4-0.87134 2.11169 1 24 -4 -4-4.37191 5.66065 1 -24 -4 5 11.3842 4.08278 1 -24 -4 5 16.183 5.03251 1 24 -4 -5 8.75583 6.32748 1 -24 -6 1 79.9443 7.39558 1 -24 6 1 69.8797 14.0904 1 -24 -6 1 66.6554 6.41757 1 24 -6 -1 77.175 15.5648 1 24 -6 -2 4.82945 7.67591 1 -24 6 2 5.19417 6.63403 1 -24 -6 2 9.47181 1.7509 1 -24 -6 2 11.4152 1.65941 1 -24 6 3 25.2325 9.57008 1 24 -6 -3 33.6006 11.8951 1 23 -1 -1 1.69307 3.24314 1 -23 -1 1 2.33642 3.94845 1 -23 1 1 0.9469 3.38774 1 -23 -1 1 2.69559 3.68665 1 -23 1 2 23.3354 7.48318 1 -23 -1 2 36.5866 7.51793 1 -23 -1 2 12.8157 4.97724 1 23 -1 -2 25.4815 7.48445 1 -23 1 3 9.01455 5.00972 1 -23 -1 3 10.5472 4.84412 1 -23 -1 3 10.6644 4.54198 1 -23 -1 4 0.55138 4.00544 1 -23 1 4 4.0918 4.90214 1 -23 -1 4 0.59804 3.20842 1 -23 1 5-0.47382 4.71116 1 -23 -1 5 8.61852 4.78228 1 -23 -1 6 6.89445 5.25312 1 -23 1 6 16.7505 7.01712 1 -23 -3 1 42.0605 7.02422 1 23 -3 -1 36.863 9.44126 1 -23 -3 1 43.7389 7.36372 1 -23 3 1 38.357 9.08262 1 -23 -3 2 47.6805 7.29666 1 -23 -3 2 28.4063 5.74394 1 23 -3 -2 33.0974 8.26685 1 -23 3 2 35.1225 8.71723 1 -23 -3 3 20.4872 4.98222 1 23 -3 -3 23.1468 7.52549 1 -23 -3 3 13.1852 4.10341 1 -23 -3 4-0.20377 2.92036 1 23 -3 -4-5.00961 3.45835 1 -23 -3 4-0.06939 2.40916 1 23 -3 -5-0.21303 4.80615 1 -23 -3 5-1.57025 2.62857 1 -23 -3 5-1.08622 3.35999 1 23 -3 -6-2.20746 5.21087 1 -23 -3 6 3.95386 4.70219 1 -23 -3 6-3.93022 3.11394 1 23 -5 -1 100.059 15.3538 1 -23 -5 1 107.655 8.40238 1 -23 -5 1 100.318 8.22354 1 -23 5 1 81.2436 12.973 1 -23 -5 2 18.5211 3.81068 1 23 -5 -2 15.28 7.80737 1 -23 -5 2 13.8042 3.25981 1 23 -5 -2 11.0049 7.08906 1 -23 5 2 10.0538 6.90865 1 -23 -5 3 14.5197 3.10567 1 -23 5 3 14.3402 7.22198 1 23 -5 -3 22.081 8.68151 1 -23 -5 4 0.90936 1.80924 1 -23 5 4 3.54553 6.18203 1 23 -5 -4 5.98483 6.23588 1 -23 -5 4-0.95605 2.09195 1 -23 -5 5 22.6728 4.32851 1 23 -5 -5 15.968 8.39115 1 -23 -5 5 28.4394 5.05583 1 -23 7 1 10.4612 6.86514 1 23 -7 -1 14.1024 7.59611 1 23 -7 -1 19.7307 8.82366 1 23 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10.5183 1 -2 8 5 4.95949 5.42922 1 -2 -8 5 8.69445 4.41047 1 2 8 -5 5.23828 4.47731 1 2 -8 -5 5.00622 4.29652 1 -2 -8 5 1.9345 3.70509 1 -2 -8 6 80.2554 13.7983 1 -2 -8 6 69.8594 11.4103 1 -2 8 6 69.963 12.9758 1 2 -8 -6 55.4894 10.6416 1 2 8 -6 77.8112 12.2281 1 2 8 -7 27.557 8.17394 1 2 -8 -7 52.7843 11.8077 1 -2 -8 7 32.1154 10.1788 1 -2 -8 7 22.3737 8.32758 1 -2 8 7 24.3764 9.1822 1 -2 -8 8 16.3344 8.90847 1 2 -8 -8 13.31 7.29073 1 -2 8 8 9.89456 7.50057 1 2 8 -8 18.1667 8.20458 1 -2 -10 1 46.4357 8.43664 1 -2 -10 1 49.878 6.76207 1 -2 -10 1 46.5885 8.17009 1 2 -10 -1 49.1318 8.06513 1 -2 -10 1 33.7627 6.90385 1 2 -10 -1 37.3404 8.34861 1 -2 10 1 36.9879 8.07849 1 2 10 -1 38.7911 7.42203 1 2 -10 -2 22.4268 5.94405 1 2 -10 -2 8.40514 5.21173 1 -2 -10 2 14.3885 5.09976 1 -2 -10 2 11.3341 5.03618 1 -2 -10 2 19.2872 5.68912 1 -2 -10 2 20.4588 5.25115 1 2 10 -2 23.3867 6.08263 1 -2 10 2 10.9249 5.49172 1 -2 -10 3 11.1499 4.71009 1 2 -10 -3 16.4707 6.26882 1 -2 -10 3 11.4771 6.53037 1 -2 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114.284 5.26115 1 1 1 -1 115.351 4.50858 1 -1 1 1 120.605 5.40383 1 -1 1 1 111.531 5.28273 1 -1 -1 1 111.177 4.46885 1 -1 1 1 118.733 5.2999 1 -1 -1 1 105.219 4.57203 1 -1 -1 1 113.289 4.7263 1 1 1 -1 116.511 4.89579 1 -1 1 1 112.098 3.46097 1 1 1 -1 115.227 4.62697 1 1 -1 -1 116.14 5.28604 1 -1 -1 2 1736.04 49.7221 1 -1 -1 2 1799.73 50.3134 1 1 -1 -2 1817.27 50.9488 1 -1 -1 2 1834.34 50.7289 1 1 -1 -2 1779.64 51.6356 1 -1 -1 2 1779.48 50.2316 1 -1 -1 2 1803.79 49.711 1 -1 -1 2 1884.68 50.0391 1 1 -1 -2 1791.66 50.8014 1 1 -1 -2 1847.65 51.0993 1 -1 1 2 1914.90 52.4975 1 -1 1 2 1830.63 52.2011 1 -1 1 2 1939.24 53.8777 1 1 1 -2 1819.57 51.3587 1 -1 1 2 1873.57 52.2105 1 -1 1 2 1888.92 53.1261 1 1 1 -2 1909.77 51.7086 1 1 1 -2 1830.05 51.186 1 1 1 -2 1757.10 51.1979 1 1 1 -2 1835.25 52.1851 1 -1 -1 3 140.569 7.87191 1 -1 -1 3 141.624 8.36062 1 -1 -1 3 145.196 8.73262 1 1 -1 -3 144.12 8.76619 1 -1 -1 3 166.409 9.11218 1 1 -1 -3 130.269 8.4658 1 1 -1 -3 151.582 9.36513 1 1 -1 -3 140.08 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-6 3 58.3327 13.3427 1 -20 6 -3 61.0322 13.7722 1 20 -6 4 12.2462 7.62778 1 -20 -6 -4 2.87895 6.05838 1 -20 6 -4 10.243 6.79354 1 -20 -8 0 6.5826 2.6691 1 20 -8 0-1.38386 4.87469 1 -20 -8 0 12.0779 3.06332 1 -20 8 0 -0.8679 6.30011 1 -20 -8 -1 9.47948 3.9884 1 -20 -8 -1 7.40435 3.61397 1 20 -8 1 9.07209 7.76225 1 -20 8 -1 4.05176 5.8436 1 -20 -8 -2 9.9063 4.86698 1 -20 -8 -2 15.0568 5.48745 1 20 -8 2 7.851 6.79686 1 -20 8 -2 12.3408 7.34352 1 -21 -1 0 2.21233 3.36666 1 21 -1 0 11.3758 5.47423 1 -21 -1 0 7.94491 4.28332 1 21 1 0 6.46163 4.1456 1 -21 1 0 2.40783 3.73272 1 -21 1 0 9.2487 5.11907 1 -21 -1 -1 29.4117 6.82955 1 -21 -1 -1 12.9644 7.1888 1 21 -1 1 15.9007 5.65725 1 -21 1 -1 17.2397 5.10977 1 -21 1 -1 10.9789 5.09127 1 -21 1 -1 28.4129 7.64564 1 21 1 1 26.2495 7.26548 1 -21 -1 -2 14.6973 5.99831 1 21 -1 2 2.37986 4.94464 1 -21 1 -2 2.49545 4.12658 1 21 1 2 7.95193 5.2417 1 -21 1 -2 7.77332 5.91695 1 -21 1 -2 11.3496 4.89784 1 21 -1 3 42.9846 11.0292 1 -21 -1 -3 32.0734 8.49135 1 -21 1 -3 53.2228 10.4775 1 21 1 3 39.2503 9.37365 1 -21 1 -3 42.1067 8.67575 1 21 -1 4 4.26321 5.06206 1 -21 1 -4-2.93885 4.25409 1 21 1 4 1.1358 5.5301 1 21 -1 5 41.5212 11.3809 1 -21 1 -5 42.0238 10.788 1 21 1 5 12.8043 8.47452 1 -21 -3 0 7.87454 3.61363 1 -21 -3 0 11.6826 3.83002 1 21 -3 0 9.67533 5.64385 1 -21 3 0 17.1726 5.69018 1 -21 3 0 19.0361 6.46719 1 -21 -3 -1 1.28336 3.74763 1 -21 -3 -1-1.83699 2.64207 1 21 -3 1 5.01866 5.33231 1 -21 3 -1 6.78095 6.3206 1 -21 3 -1 1.42532 3.97638 1 21 -3 2 3.13335 4.08392 1 -21 -3 -2 0.80339 3.91069 1 -21 3 -2 2.05047 4.72338 1 21 -3 3 15.4729 7.32345 1 -21 -3 -3 15.9041 6.50289 1 -21 3 -3 16.3546 6.67855 1 -21 -3 -4 13.8411 7.48026 1 21 -3 4 21.6376 8.20555 1 -21 3 -4 5.06102 6.81692 1 -21 -5 0 3.601 2.9643 1 -21 -5 0 5.62586 3.20177 1 21 -5 0 3.78497 5.12309 1 -21 5 0 12.1649 6.35371 1 -21 -5 -1 31.4514 6.69236 1 21 -5 1 43.3762 11.0515 1 -21 -5 -1 33.1852 6.50125 1 -21 5 -1 33.6213 9.72106 1 21 -5 2 62.068 12.9186 1 -21 -5 -2 60.245 9.66144 1 -21 -5 -2 65.2017 10.0325 1 -21 5 -2 57.2151 11.8229 1 -21 -5 -3-0.41965 4.28539 1 21 -5 3 5.65998 6.1974 1 -21 5 -3 4.02946 6.19351 1 -21 -5 -4 0.14912 5.95069 1 21 -5 4 5.21673 6.01103 1 -21 5 -4 6.74334 6.26721 1 21 -7 0 9.80134 6.85565 1 -21 -7 0 10.6258 3.42995 1 -21 -7 0 4.89247 2.8233 1 -21 7 0 12.4106 6.41886 1 -21 -7 -1 17.0363 4.96944 1 21 -7 1 7.58071 7.05345 1 -21 -7 -1 19.867 4.96887 1 -21 7 -1 7.82326 6.32551 1 21 -7 2 0.84852 5.05739 1 -21 -7 -2 4.33697 4.53665 1 -21 -7 -2 6.05878 4.54085 1 -21 7 -2-6.99016 3.77312 1 22 0 0 2.28007 3.34266 1 -22 0 0 1.4789 3.58205 1 -22 0 -1 13.9542 6.1882 1 22 0 1 10.0264 5.23788 1 -22 0 -2-0.35636 4.37652 1 22 0 2 2.35018 5.12882 1 22 0 3 6.70402 4.56781 1 22 0 4 71.4705 13.4546 1 22 -2 0 16.0466 6.69105 1 -22 -2 0 15.2726 4.98613 1 -22 -2 0 19.4458 5.44417 1 -22 2 0 16.5427 5.78728 1 -22 2 0 9.23092 5.5741 1 -22 2 0 9.59808 6.41269 1 -22 -2 -1 2.50519 4.2235 1 -22 -2 -1 14.9051 5.32078 1 22 -2 1 12.4941 6.17371 1 -22 2 -1 10.9115 5.25562 1 -22 2 -1 9.21102 5.25677 1 -22 -2 -2 2.24856 4.44528 1 22 -2 2 3.65837 4.13471 1 -22 2 -2 7.97691 5.17076 1 -22 2 -2 7.45094 7.15653 1 22 -2 3 7.1583 5.53545 1 -22 -2 -3 9.01516 5.92023 1 -22 2 -3 8.83204 5.80692 1 22 -2 4 85.5414 15.6349 1 -22 2 -4 52.3485 11.2643 1 -22 -4 0 2.62567 3.09654 1 -22 4 0 2.26508 4.8904 1 -22 -4 0 0.68358 2.83247 1 22 -4 0 -3.3716 2.88696 1 -22 -4 -1-0.65105 3.0585 1 -22 -4 -1 4.50996 3.87024 1 22 -4 1 2.86101 5.04884 1 -22 4 -1-1.71673 4.59565 1 -22 -4 -2 0.53005 4.50089 1 22 -4 2 4.78063 5.93638 1 -22 4 -2 3.93862 5.58832 1 22 -4 3 22.298 8.95786 1 -22 -4 -3 20.0995 7.51161 1 -22 4 -3 18.0672 7.15182 1 22 -4 4-1.70466 5.28307 1 -22 4 -4 0.57229 5.73706 1 -22 -6 0 1.12673 2.92287 1 -22 -6 0 2.65829 2.83896 1 22 -6 0 2.34209 5.72533 1 -22 6 0-2.47577 4.10831 1 -22 -6 -1 19.2521 5.49379 1 22 -6 1 34.8407 10.5043 1 -22 -6 -1 22.3828 5.90711 1 -22 6 -1 16.6402 7.38441 1 -22 -6 -2 4.0124 4.87905 1 -22 -6 -2 1.8531 5.10741 1 22 -6 2 4.56998 7.52612 1 -22 6 -2 2.82342 6.92044 1 23 -1 0 14.416 6.09142 1 -23 -1 0 6.40675 4.54974 1 -23 1 0 3.09681 4.80297 1 23 -1 1 6.53772 5.12919 1 -23 -1 -1 5.74984 5.07424 1 -23 1 -1 8.91339 7.40201 1 -23 1 -1 10.2997 5.95048 1 -23 -1 -2-1.18284 3.82408 1 23 -1 2-0.08152 3.49593 1 -23 1 -2 0.6355 5.72849 1 23 -1 3 24.8731 8.75711 1 23 -1 4 16.7131 8.60082 1 23 1 4 14.4064 8.52364 1 -23 -3 0 11.7775 4.51187 1 -23 -3 0 3.67002 3.41995 1 23 -3 0 0.25186 4.33588 1 -23 3 0-2.35234 3.86837 1 -23 3 0 5.33043 6.6807 1 -23 -3 -1 0.49681 4.55442 1 23 -3 1 2.78882 4.35026 1 -23 -3 -1-0.40102 3.63994 1 -23 3 -1 10.4705 6.26132 1 -23 -3 -2 31.0541 8.18284 1 23 -3 2 28.0226 9.088 1 -23 3 -2 30.8777 9.0637 1 -23 -3 -3 11.3661 6.87118 1 23 -3 3 21.8953 8.7581 1 -23 3 -3 18.0263 8.09149 1 -23 -5 0 12.3634 4.51743 1 23 -5 0 11.7341 6.63101 1 -23 -5 0 5.57928 3.54034 1 -23 5 0 13.8942 7.09817 1 -23 -5 -1 6.6326 4.12631 1 23 -5 1 0.88876 3.86265 1 -23 -5 -1 5.91654 4.16817 1 -23 5 -1-2.76184 4.85681 1 -23 -5 -2-0.66256 4.21126 1 23 -5 2 0.55019 6.24249 1 -23 5 -2 0.21919 5.67889 1 -23 -7 0 0.30367 2.53725 1 23 -7 0-2.44224 3.82543 1 -23 -7 0 1.24623 2.3721 1 -23 7 0 6.12004 6.03134 1 -24 0 0-0.27496 4.09325 1 -24 0 -1-2.40133 3.92914 1 -24 0 -1 1.29948 4.54699 1 -24 0 -2 3.08291 7.38362 1 24 0 2 7.13651 6.8095 1 24 0 3 3.11199 5.79672 1 -24 -2 0 1.98614 4.75488 1 24 -2 0-0.46907 4.0937 1 -24 -2 0 6.81154 4.84851 1 -24 2 0 1.30353 9.58186 1 -24 -2 -1 66.008 11.0178 1 24 -2 1 62.8189 12.5435 1 -24 -2 -2 11.577 6.4132 1 24 -2 2 27.5251 8.79447 1 -24 -2 -3 32.0502 9.2595 1 24 -2 3 14.1106 7.69616 1 -24 -4 0 14.7097 5.18634 1 24 -4 0 21.0037 8.55827 1 -24 -4 0 18.4369 5.56499 1 -24 4 0 14.1961 6.77313 1 -24 -4 -1 16.254 5.73743 1 24 -4 1 20.394 9.04969 1 -24 -4 -1 16.2393 6.14818 1 -24 4 -1 16.8472 8.02398 1 -24 -4 -2-1.97688 4.5836 1 24 -4 2 2.44474 6.81683 1 -24 4 -2-0.84425 5.88818 1 -24 -6 0 8.74117 3.88614 1 -24 -6 0 8.2914 3.86066 1 24 -6 0 9.25149 5.81504 1 -24 6 0 5.25336 6.37271 1 -25 -1 0 12.9352 6.1914 1 -25 1 0 6.78694 5.5503 1 -25 -1 -1 52.2487 10.8616 1 25 -1 1 34.4676 10.22 1 25 -1 2 29.5005 9.88492 1 -25 -1 -2 19.766 7.98144 1 -25 -3 0 19.9952 6.32908 1 25 -3 0 19.7503 7.08847 1 -25 -3 0 25.2162 6.91705 1 -25 -3 -1 35.9346 8.36953 1 25 -3 1 41.9354 11.7833 1 25 -3 2 30.3977 10.4867 1 25 -5 0 11.5048 8.21178 1 -25 -5 0 17.1468 5.58609 1 -25 -5 0 14.4887 5.44203 1 -25 5 0 14.8351 8.51439 1 -26 0 0-1.01933 4.1556 1 -26 0 -1 15.3732 8.21805 1 26 -2 0 28.7151 8.70453 1 -26 -2 0 31.5323 8.37099 1 26 -2 1 21.9944 8.57689 1 -26 -2 -1 12.0623 6.38217 1 0 0 0 0.00 0.00 1 ; _shelx_hkl_checksum 75816 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.28347(9) 0.56918(19) -0.0202(2) 0.0221(4) Uani 1 1 d . . . . . H1A H 0.2463(14) 0.620(2) -0.044(4) 0.033 Uiso 1 1 calc R U . . . C1 C 0.26605(13) 0.4373(3) 0.0515(4) 0.0186(5) Uani 1 1 d . . . . . H1 H 0.2347 0.3844 -0.0479 0.022 Uiso 1 1 calc R U . . . C2 C 0.33426(13) 0.3549(3) 0.1088(3) 0.0183(5) Uani 1 1 d . . . . . O3 O 0.33405(9) 0.22575(17) 0.1244(2) 0.0215(4) Uani 1 1 d . . . . . N4 N 0.39164(10) 0.4372(2) 0.1481(3) 0.0189(5) Uani 1 1 d . . . . . H4 H 0.3846(15) 0.522(3) 0.123(4) 0.026(8) Uiso 1 1 d . . . . . C5 C 0.46277(13) 0.4014(3) 0.2116(4) 0.0191(6) Uani 1 1 d . . . . . C6 C 0.48724(14) 0.2645(3) 0.2307(4) 0.0274(7) Uani 1 1 d . . . . . H6 H 0.4553 0.1882 0.2041 0.033 Uiso 1 1 calc R U . . . C7 C 0.55869(15) 0.2389(3) 0.2891(4) 0.0341(7) Uani 1 1 d . . . . . H7 H 0.5754 0.1448 0.3011 0.041 Uiso 1 1 calc R U . . . C8 C 0.60575(15) 0.3491(3) 0.3299(4) 0.0298(7) Uani 1 1 d . . . . . H8 H 0.6544 0.3307 0.3699 0.036 Uiso 1 1 calc R U . . . C9 C 0.58171(14) 0.4853(3) 0.3123(4) 0.0249(6) Uani 1 1 d . . . . . H9 H 0.614 0.5608 0.3407 0.03 Uiso 1 1 calc R U . . . C10 C 0.51041(14) 0.5138(3) 0.2531(3) 0.0196(6) Uani 1 1 d . . . . . C11 C 0.48470(14) 0.6562(3) 0.2337(4) 0.0239(6) Uani 1 1 d . . . . . C12 C 0.46194(15) 0.7718(3) 0.2127(5) 0.0368(8) Uani 1 1 d . . . . . H12 H 0.4437 0.8645 0.1959 0.044 Uiso 1 1 calc R U . . . C13 C 0.22937(12) 0.4521(3) 0.2211(3) 0.0175(5) Uani 1 1 d . . . . . C14 C 0.25280(13) 0.5545(3) 0.3546(4) 0.0208(6) Uani 1 1 d . . . . . H14 H 0.2897 0.6166 0.3348 0.025 Uiso 1 1 calc R U . . . C15 C 0.22311(13) 0.5663(3) 0.5142(4) 0.0233(6) Uani 1 1 d . . . . . H15 H 0.2395 0.6362 0.6039 0.028 Uiso 1 1 calc R U . . . C16 C 0.16911(13) 0.4758(3) 0.5439(4) 0.0227(6) Uani 1 1 d . . . . . H16 H 0.1488 0.4835 0.6544 0.027 Uiso 1 1 calc R U . . . C17 C 0.14509(13) 0.3750(3) 0.4130(4) 0.0220(6) Uani 1 1 d . . . . . H17 H 0.1081 0.3134 0.4331 0.026 Uiso 1 1 calc R U . . . C18 C 0.17501(13) 0.3633(3) 0.2512(4) 0.0196(6) Uani 1 1 d . . . . . H18 H 0.1581 0.294 0.161 0.023 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0207(9) 0.0197(10) 0.0259(11) 0.0079(8) 0.0038(8) 0.0017(8) C1 0.0189(13) 0.0165(13) 0.0200(14) 0.0020(11) 0.0015(10) -0.0016(10) C2 0.0190(13) 0.0199(14) 0.0162(13) 0.0009(11) 0.0036(10) -0.0014(10) O3 0.0226(10) 0.0153(9) 0.0261(11) 0.0000(8) 0.0025(8) -0.0003(8) N4 0.0171(11) 0.0144(12) 0.0242(13) 0.0023(10) 0.0001(9) -0.0004(9) C5 0.0165(12) 0.0210(14) 0.0196(14) 0.0014(11) 0.0024(10) -0.0001(10) C6 0.0227(14) 0.0186(15) 0.0394(18) 0.0054(13) 0.0000(13) -0.0011(11) C7 0.0280(16) 0.0250(16) 0.047(2) 0.0066(14) 0.0001(14) 0.0019(13) C8 0.0201(14) 0.0342(17) 0.0337(18) 0.0037(14) 0.0001(13) 0.0038(12) C9 0.0192(14) 0.0303(16) 0.0252(16) -0.0025(12) 0.0035(11) -0.0019(11) C10 0.0189(14) 0.0227(13) 0.0172(14) -0.0009(11) 0.0027(11) -0.0001(11) C11 0.0174(13) 0.0267(15) 0.0279(16) -0.0063(12) 0.0045(12) -0.0045(11) C12 0.0301(16) 0.0243(16) 0.056(2) -0.0040(15) 0.0066(15) 0.0007(13) C13 0.0152(11) 0.0162(12) 0.0202(14) 0.0034(11) -0.0002(10) 0.0039(10) C14 0.0189(13) 0.0179(13) 0.0244(15) 0.0004(11) -0.0002(11) -0.0037(11) C15 0.0216(13) 0.0238(14) 0.0229(14) -0.0032(12) -0.0011(11) -0.0003(12) C16 0.0232(14) 0.0230(14) 0.0224(15) 0.0000(11) 0.0050(11) 0.0039(11) C17 0.0186(13) 0.0193(13) 0.0283(16) 0.0002(11) 0.0042(11) -0.0017(11) C18 0.0169(12) 0.0157(13) 0.0249(15) -0.0015(11) -0.0004(10) 0.0002(10) 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 0 '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 0.006 '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 C1 O1 H1A 109.5 . . ? O1 C1 C13 112.5(2) . . ? O1 C1 C2 108.2(2) . . ? C13 C1 C2 108.3(2) . . ? O1 C1 H1 109.3 . . ? C13 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? O3 C2 N4 125.1(2) . . ? O3 C2 C1 121.5(2) . . ? N4 C2 C1 113.4(2) . . ? C2 N4 C5 130.2(2) . . ? C2 N4 H4 115(2) . . ? C5 N4 H4 115(2) . . ? C6 C5 C10 119.7(2) . . ? C6 C5 N4 123.7(2) . . ? C10 C5 N4 116.6(2) . . ? C5 C6 C7 119.8(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C7 119.7(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.7(2) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 119.4(2) . . ? C9 C10 C11 121.1(2) . . ? C5 C10 C11 119.5(2) . . ? C12 C11 C10 177.8(3) . . ? C11 C12 H12 180 . . ? C18 C13 C14 118.8(2) . . ? C18 C13 C1 121.9(2) . . ? C14 C13 C1 119.2(2) . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120 . . ? C16 C15 H15 120 . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? C13 C18 C17 120.4(2) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? 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 O1 C1 1.419(3) . ? O1 H1A 0.86(3) . ? C1 C13 1.521(3) . ? C1 C2 1.526(4) . ? C1 H1 1 . ? C2 O3 1.234(3) . ? C2 N4 1.345(3) . ? N4 C5 1.412(3) . ? N4 H4 0.84(3) . ? C5 C6 1.384(4) . ? C5 C10 1.408(3) . ? C6 C7 1.391(4) . ? C6 H6 0.95 . ? C7 C8 1.385(4) . ? C7 H7 0.95 . ? C8 C9 1.375(4) . ? C8 H8 0.95 . ? C9 C10 1.394(4) . ? C9 H9 0.95 . ? C10 C11 1.441(4) . ? C11 C12 1.184(4) . ? C12 H12 0.95 . ? C13 C18 1.387(3) . ? C13 C14 1.398(3) . ? C14 C15 1.376(3) . ? C14 H14 0.95 . ? C15 C16 1.390(4) . ? C15 H15 0.95 . ? C16 C17 1.379(4) . ? C16 H16 0.95 . ? C17 C18 1.393(4) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? 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 O1 H1A O3 0.86 1.86 2.709(2) 173.2 4 N4 H4 O1 0.84(3) 2.10(3) 2.565(3) 115(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 O1 C1 C2 O3 -158.8(2) . . . . ? C13 C1 C2 O3 79.0(3) . . . . ? O1 C1 C2 N4 24.4(3) . . . . ? C13 C1 C2 N4 -97.8(2) . . . . ? O3 C2 N4 C5 0.8(4) . . . . ? C1 C2 N4 C5 177.4(2) . . . . ? C2 N4 C5 C6 5.7(4) . . . . ? C2 N4 C5 C10 -175.6(2) . . . . ? C10 C5 C6 C7 -0.6(4) . . . . ? N4 C5 C6 C7 178.1(2) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 -0.2(4) . . . . ? C8 C9 C10 C5 0.1(4) . . . . ? C8 C9 C10 C11 -179.8(3) . . . . ? C6 C5 C10 C9 0.3(4) . . . . ? N4 C5 C10 C9 -178.5(2) . . . . ? C6 C5 C10 C11 -179.8(3) . . . . ? N4 C5 C10 C11 1.5(3) . . . . ? O1 C1 C13 C18 142.4(2) . . . . ? C2 C1 C13 C18 -98.0(3) . . . . ? O1 C1 C13 C14 -40.1(3) . . . . ? C2 C1 C13 C14 79.5(3) . . . . ? C18 C13 C14 C15 0.7(4) . . . . ? C1 C13 C14 C15 -176.8(2) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C14 C13 C18 C17 -0.9(3) . . . . ? C1 C13 C18 C17 176.6(2) . . . . ? C16 C17 C18 C13 0.4(4) . . . . ?