#------------------------------------------------------------------------------ #$Date: 2021-07-28 08:40:35 +0300 (Wed, 28 Jul 2021) $ #$Revision: 267785 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243880.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243880 loop_ _publ_author_name 'El Hafi, Mohamed' 'Lahmidi, Sanae' 'El Ghayati, Lhoussaine' 'H\"okelek, Tuncer' 'Mague, Joel T.' 'Amer, Bushra' 'Sebbar, Nada Kheira' 'Essassi, El Mokhtar' _publ_section_title ; Crystal structure, Hirshfeld surface analysis and interaction energy calculation of 4-(furan-2-yl)-2-(6-methyl-2,4-dioxopyran-3-ylidene)-2,3,4,5-tetrahydro-1H-1,5-benzodiazepine ; _journal_coeditor_code WM5612 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 834 _journal_page_last 838 _journal_paper_doi 10.1107/S2056989021007441 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C19 H16 N2 O4' _chemical_formula_moiety 'C19 H16 N2 O4' _chemical_formula_sum 'C19 H16 N2 O4' _chemical_formula_weight 336.34 _chemical_name_systematic (S,E)-3-[4-(Furan-2-yl)-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-2-ylidene]-6-methyl-2H-pyran-2,4(3H)-dione _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 96.202(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.0111(8) _cell_length_b 11.0123(13) _cell_length_c 20.493(2) _cell_measurement_reflns_used 9980 _cell_measurement_temperature 150.(2) _cell_measurement_theta_max 28.4053 _cell_measurement_theta_min 2.7240 _cell_volume 1573.0(3) _computing_cell_refinement ; SAINT (Bruker, 2020) ; _computing_data_collection ; APEX3 (Bruker, 2020) ; _computing_data_reduction ; SAINT (Bruker, 2020) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/1 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.950 _diffrn_measurement_device 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_unetI/netI 0.0590 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5201 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.512 _diffrn_reflns_theta_min 2.724 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.50 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Sheldrick, 2009) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.336 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.114 _refine_diff_density_max 0.540 _refine_diff_density_min -0.298 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 5201 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.136 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0786 _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^)+(0.0648P)^2^+2.9838P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1999 _refine_ls_wR_factor_ref 0.2138 _reflns_number_gt 4007 _reflns_number_total 5201 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5612sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2243880 _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 0.967 _shelx_estimated_absorpt_t_max 0.989 _shelx_hkl_file ; 1 0 0 424.826 11.6202 2 1 0 0 1604.63 48.5088 1 2 0 0 2336.30 107.783 2 -3 0 2 1467.74 35.8374 -2 3 0 0 1467.74 35.8374 1 4 0 0 0.10077 0.92712 2 -4 0 3 -4.9147 3.94596 -2 4 0 0 -4.9147 3.94596 1 4 0 0 0.20632 1.05861 1 -5 0 3 3.31553 1.38210 -2 5 0 0 3.31553 1.38210 1 5 0 0 5.90392 2.92042 2 -6 0 4 150.825 6.19144 -2 6 0 0 150.825 6.19144 1 -7 0 4 67.3857 11.3909 -2 7 0 0 67.3857 11.3909 1 -8 0 5 6.58082 3.30531 -2 8 0 0 6.58082 3.30531 1 -9 0 6 -7.7736 7.67868 -2 9 0 0 -7.7736 7.67868 1 0 1 0 0.19241 0.13558 -2 0 1 0 0.19241 0.13558 1 1 1 0 470.554 8.57569 2 1 1 0 1897.70 37.6179 1 -1 1 1 2010.41 135.951 -2 1 1 0 2010.41 135.951 1 2 1 0 2215.00 52.1950 1 -2 1 1 4495.67 144.240 -2 2 1 0 4495.67 144.240 1 2 1 0 1845.10 85.6077 2 -3 1 2 1787.97 31.3339 -2 3 1 0 1787.97 31.3339 1 4 1 0 686.322 19.3171 2 -4 1 2 2289.93 129.314 -2 4 1 0 2289.93 129.314 1 -4 1 3 2431.43 61.6223 -2 4 1 0 2431.43 61.6223 1 4 1 0 2179.79 75.7379 1 -5 1 3 0.26018 0.87354 -2 5 1 0 0.26018 0.87354 1 -6 1 4 585.153 14.1298 -2 6 1 0 585.153 14.1298 1 -7 1 4 4.66205 8.52954 -2 7 1 0 4.66205 8.52954 1 -8 1 5 9.19259 2.34010 -2 8 1 0 9.19259 2.34010 1 -9 1 6 20.8038 9.61754 -2 9 1 0 20.8038 9.61754 1 0 2 0 5819.07 530.755 -2 0 2 0 5819.07 530.755 1 1 2 0 234.222 4.64000 2 1 2 0 969.947 20.1097 1 -1 2 1 907.634 45.9160 -2 1 2 0 907.634 45.9160 1 2 2 0 155.558 8.66203 2 -2 2 1 267.988 6.13484 -2 2 2 0 267.988 6.13484 1 2 2 0 16.3043 0.72608 1 -3 2 2 31.9452 0.87119 -2 3 2 0 31.9452 0.87119 1 4 2 0 373.156 10.1394 2 -4 2 3 1287.79 36.0167 -2 4 2 0 1287.79 36.0167 1 4 2 0 1125.69 32.9847 1 -4 2 2 1115.15 109.672 -2 4 2 0 1115.15 109.672 1 -5 2 3 98.0419 2.03863 -2 5 2 0 98.0419 2.03863 1 -6 2 4 50.9075 2.19026 -2 6 2 0 50.9075 2.19026 1 -7 2 4 29.4580 6.10666 -2 7 2 0 29.4580 6.10666 1 -8 2 5 66.3161 4.37447 -2 8 2 0 66.3161 4.37447 1 -9 2 6 2.55361 5.54793 -2 9 2 0 2.55361 5.54793 1 0 3 0 4.84665 0.44396 -2 0 3 0 4.84665 0.44396 1 1 3 0 126.185 2.96055 1 1 3 0 29.7891 0.94901 2 -1 3 1 114.115 7.60171 -2 1 3 0 114.115 7.60171 1 2 3 0 59.1924 1.63618 1 2 3 0 44.3850 1.85466 2 -2 3 1 194.816 5.05896 -2 2 3 0 194.816 5.05896 1 -3 3 2 58.9964 1.20676 -2 3 3 0 58.9964 1.20676 1 -4 3 3 568.128 19.6816 -2 4 3 0 568.128 19.6816 1 4 3 0 156.399 5.94687 2 -4 3 2 557.909 32.3630 -2 4 3 0 557.909 32.3630 1 4 3 0 573.494 17.7299 1 -5 3 3 41.4935 1.34526 -2 5 3 0 41.4935 1.34526 1 -6 3 4 385.632 10.2541 -2 6 3 0 385.632 10.2541 1 -7 3 4 21.5175 5.77843 -2 7 3 0 21.5175 5.77843 1 -8 3 5 37.7935 4.43609 -2 8 3 0 37.7935 4.43609 1 -9 3 6 27.0647 7.06804 -2 9 3 0 27.0647 7.06804 1 0 4 0 1269.25 32.2989 -2 0 4 0 1269.25 32.2989 1 1 4 0 39.0240 1.27355 1 -1 4 1 139.945 5.32621 -2 1 4 0 139.945 5.32621 1 1 4 0 13.6849 0.76637 2 -2 4 1 2982.80 65.4788 -2 2 4 0 2982.80 65.4788 1 2 4 0 751.572 31.2892 2 2 4 0 2565.64 173.756 1 -3 4 2 128.872 2.61202 -2 3 4 0 128.872 2.61202 1 4 4 0 258.387 7.95941 1 -4 4 3 285.750 11.3838 -2 4 4 0 285.750 11.3838 1 -4 4 2 334.610 19.6065 -2 4 4 0 334.610 19.6065 1 4 4 0 86.7278 3.16717 2 -5 4 3 146.840 3.35254 -2 5 4 0 146.840 3.35254 1 -6 4 4 99.7931 3.67091 -2 6 4 0 99.7931 3.67091 1 -8 4 5 104.945 6.13897 -2 8 4 0 104.945 6.13897 1 0 5 0 0.18129 0.50701 -2 0 5 0 0.18129 0.50701 1 1 5 0 1686.59 49.6024 1 -1 5 1 1626.36 41.0069 -2 1 5 0 1626.36 41.0069 1 1 5 0 447.487 12.7552 2 -2 5 1 2585.96 59.0709 -2 2 5 0 2585.96 59.0709 1 2 5 0 2062.73 198.025 1 -3 5 2 38.4926 1.06692 -2 3 5 0 38.4926 1.06692 1 -4 5 3 993.472 40.6050 -2 4 5 0 993.472 40.6050 1 4 5 0 274.968 11.0880 2 4 5 0 816.115 25.3529 1 -4 5 2 896.333 33.5371 -2 4 5 0 896.333 33.5371 1 -5 5 3 149.240 3.89711 -2 5 5 0 149.240 3.89711 1 -6 5 4 55.6673 3.83554 -2 6 5 0 55.6673 3.83554 1 -7 5 4 -17.098 9.52917 -2 7 5 0 -17.098 9.52917 1 -8 5 5 9.76247 4.19605 -2 8 5 0 9.76247 4.19605 1 0 6 0 2785.49 71.6906 -2 0 6 0 2785.49 71.6906 1 -1 6 1 218.746 5.26477 -2 1 6 0 218.746 5.26477 1 1 6 0 57.3717 2.35826 2 1 6 0 196.066 8.72340 1 2 6 0 0.01646 0.62418 1 -2 6 1 422.621 9.22091 -2 2 6 0 422.621 9.22091 1 -3 6 2 39.4835 1.31522 -2 3 6 0 39.4835 1.31522 1 -4 6 3 136.665 6.18424 -2 4 6 0 136.665 6.18424 1 4 6 0 129.620 7.13865 1 4 6 0 36.1505 3.42967 2 -4 6 2 121.896 8.00549 -2 4 6 0 121.896 8.00549 1 -5 6 3 3.15622 1.50915 -2 5 6 0 3.15622 1.50915 1 -6 6 4 4.48916 2.84548 -2 6 6 0 4.48916 2.84548 1 -7 6 4 1.98728 8.71296 -2 7 6 0 1.98728 8.71296 1 -8 6 5 15.7383 5.08412 -2 8 6 0 15.7383 5.08412 1 0 7 0 -0.2161 0.69446 -2 0 7 0 -0.2161 0.69446 1 1 7 0 32.6634 2.27761 1 -1 7 1 34.1802 1.50956 -2 1 7 0 34.1802 1.50956 1 1 7 0 10.8076 1.59772 2 -2 7 1 234.262 5.57160 -2 2 7 0 234.262 5.57160 1 -3 7 2 67.6287 1.90903 -2 3 7 0 67.6287 1.90903 1 -4 7 3 427.183 16.7481 -2 4 7 0 427.183 16.7481 1 -4 7 2 410.595 23.9444 -2 4 7 0 410.595 23.9444 1 4 7 0 110.781 8.92252 2 4 7 0 394.950 39.7608 1 -5 7 3 16.9827 2.12431 -2 5 7 0 16.9827 2.12431 1 -6 7 4 23.4390 3.27954 -2 6 7 0 23.4390 3.27954 1 -7 7 4 -10.810 9.21637 -2 7 7 0 -10.810 9.21637 1 -8 7 5 21.1134 5.02854 -2 8 7 0 21.1134 5.02854 1 0 8 0 552.346 14.3058 -2 0 8 0 552.346 14.3058 1 1 8 0 -0.6867 1.25233 2 -1 8 1 1.47512 1.15730 -2 1 8 0 1.47512 1.15730 1 1 8 0 1.39307 0.99465 1 -2 8 1 211.254 5.40326 -2 2 8 0 211.254 5.40326 1 -3 8 2 -0.3205 1.23997 -2 3 8 0 -0.3205 1.23997 1 -4 8 2 7.95401 3.85056 -2 4 8 0 7.95401 3.85056 1 -4 8 3 -2.2316 4.79872 -2 4 8 0 -2.2316 4.79872 1 -5 8 3 1.50457 2.49781 -2 5 8 0 1.50457 2.49781 1 -6 8 4 37.2873 3.47643 -2 6 8 0 37.2873 3.47643 1 -7 8 4 -0.5677 10.3639 -2 7 8 0 -0.5677 10.3639 1 -7 8 5 14.6765 10.6596 -2 7 8 0 14.6765 10.6596 1 0 9 0 -0.3518 0.78030 -2 0 9 0 -0.3518 0.78030 1 -1 9 1 9.59070 1.52476 -2 1 9 0 9.59070 1.52476 1 -1 9 1 31.8361 9.12192 -2 1 9 0 31.8361 9.12192 -1 1 9 1 31.8361 9.12192 1 1 9 0 -1.2742 2.59689 2 -2 9 1 35.9584 1.85168 -2 2 9 0 35.9584 1.85168 1 -3 9 2 37.4444 1.94208 -2 3 9 0 37.4444 1.94208 1 -4 9 3 53.5999 7.26015 -2 4 9 0 53.5999 7.26015 1 -5 9 3 11.6305 3.50107 -2 5 9 0 11.6305 3.50107 1 -6 9 4 41.3176 4.48486 -2 6 9 0 41.3176 4.48486 1 0 10 0 2.87433 1.23828 -2 0 10 0 2.87433 1.23828 1 -1 10 1 5.81199 2.27917 -2 1 10 0 5.81199 2.27917 1 1 10 0 -0.8434 3.28939 1 -2 10 1 52.6786 3.62294 -2 2 10 0 52.6786 3.62294 1 -3 10 2 21.9409 2.20318 -2 3 10 0 21.9409 2.20318 1 -4 10 3 193.763 15.6138 -2 4 10 0 193.763 15.6138 1 -4 10 2 175.995 21.6386 -2 4 10 0 175.995 21.6386 1 -5 10 3 35.8569 3.54222 -2 5 10 0 35.8569 3.54222 1 -6 10 4 1.28581 4.04749 -2 6 10 0 1.28581 4.04749 1 0 11 0 -1.4733 2.35114 -2 0 11 0 -1.4733 2.35114 1 -1 11 1 38.5753 3.62404 -2 1 11 0 38.5753 3.62404 1 1 11 0 37.6291 8.05929 1 1 11 0 9.83479 4.45520 2 -2 11 1 6.96184 2.39787 -2 2 11 0 6.96184 2.39787 1 -3 11 2 22.4346 2.46248 -2 3 11 0 22.4346 2.46248 1 -4 11 2 13.1310 11.0546 -2 4 11 0 13.1310 11.0546 1 -5 11 3 26.5076 3.44141 -2 5 11 0 26.5076 3.44141 1 -6 11 4 22.5579 6.31053 -2 6 11 0 22.5579 6.31053 1 0 12 0 14.5483 3.00664 -2 0 12 0 14.5483 3.00664 1 -1 12 1 1.39280 4.23038 -2 1 12 0 1.39280 4.23038 1 1 12 0 4.01770 3.94860 1 -2 12 1 0.89901 3.08445 -2 2 12 0 0.89901 3.08445 1 -3 12 2 11.2757 2.73198 -2 3 12 0 11.2757 2.73198 1 -4 12 2 64.1488 14.6272 -2 4 12 0 64.1488 14.6272 1 -4 12 3 45.0985 13.4839 -2 4 12 0 45.0985 13.4839 1 -5 12 3 9.25142 4.56192 -2 5 12 0 9.25142 4.56192 1 0 13 0 -3.2713 3.60084 -2 0 13 0 -3.2713 3.60084 1 -1 13 1 13.5609 7.44490 -2 1 13 0 13.5609 7.44490 1 -2 13 1 24.6207 4.44511 -2 2 13 0 24.6207 4.44511 1 -3 13 2 13.9933 5.58263 -2 3 13 0 13.9933 5.58263 1 -4 13 3 -14.610 12.4007 -2 4 13 0 -14.610 12.4007 1 0 14 0 -2.5025 4.13240 -2 0 14 0 -2.5025 4.13240 1 1 14 0 0.48408 5.41686 2 -1 14 1 2.96924 9.63869 -2 1 14 0 2.96924 9.63869 1 -2 14 1 4.32506 4.61668 -2 2 14 0 4.32506 4.61668 1 -9 0 5 -7.6420 7.68431 -2 -9 0 1 -7.6420 7.68431 1 -8 0 4 1.43512 2.96861 -2 -8 0 1 1.43512 2.96861 1 -7 0 3 5.81133 5.44252 -2 -7 0 1 5.81133 5.44252 1 -6 0 3 1.94026 1.84513 -2 -6 0 1 1.94026 1.84513 1 -5 0 2 1.67502 1.33481 -2 -5 0 1 1.67502 1.33481 1 -4 0 1 0.09412 1.07375 1 -4 0 2 5.71878 3.34349 -2 -4 0 1 5.71878 3.34349 1 -4 0 1 0.45360 0.91151 2 -3 0 1 -1.6918 0.76799 -2 -3 0 1 -1.6918 0.76799 1 -2 0 1 56.2443 2.56343 1 -2 0 1 2856.28 257.411 2 -1 0 1 7.58659 0.39253 1 -1 0 1 3.87681 0.30363 2 0 0 1 -0.0363 0.03302 -2 0 0 1 -0.0363 0.03302 1 1 0 1 2.88654 0.36932 2 1 0 1 6.33262 0.36543 1 -2 0 2 1727.34 69.6199 -2 2 0 1 1727.34 69.6199 1 2 0 1 66.0495 3.12427 1 -3 0 3 -1.7144 0.80304 -2 3 0 1 -1.7144 0.80304 1 -4 0 4 172.424 10.0629 -2 4 0 1 172.424 10.0629 1 4 0 1 5.24501 1.10712 2 4 0 1 6.88778 1.57216 1 -5 0 4 113.877 3.55373 -2 5 0 1 113.877 3.55373 1 -6 0 5 -1.1996 3.98834 -2 6 0 1 -1.1996 3.98834 1 -7 0 5 16.9825 8.68265 -2 7 0 1 16.9825 8.68265 1 -8 0 6 18.7693 3.70350 -2 8 0 1 18.7693 3.70350 1 -9 0 7 7.69761 8.40838 -2 9 0 1 7.69761 8.40838 1 -9 1 5 0.42068 9.41687 -2 -9 1 1 0.42068 9.41687 1 -8 1 4 1.19729 2.10773 -2 -8 1 1 1.19729 2.10773 1 -7 1 3 21.8963 5.99900 -2 -7 1 1 21.8963 5.99900 1 -6 1 3 13.1196 1.63632 -2 -6 1 1 13.1196 1.63632 1 -5 1 2 48.1133 1.49736 -2 -5 1 1 48.1133 1.49736 1 -4 1 1 2454.55 68.1881 1 -4 1 1 826.969 25.3904 2 -4 1 2 2690.53 70.0270 -2 -4 1 1 2690.53 70.0270 1 -4 1 1 3187.12 220.033 -2 -4 1 1 3187.12 220.033 1 -3 1 1 99.4588 1.99563 -2 -3 1 1 99.4588 1.99563 1 -2 1 1 2536.72 60.1838 2 -2 1 1 6664.80 414.075 1 -1 1 1 907.493 18.7620 1 -1 1 1 231.433 4.30222 2 1 1 0 1277.65 125.398 -2 -1 1 1 1277.65 125.398 1 0 1 1 6.89533 0.49424 -2 0 1 1 6.89533 0.49424 1 1 1 1 1631.10 39.0017 2 2 1 1 4755.67 302.739 2 2 1 1 9999.99 858.479 1 -3 1 3 270.111 4.75729 -2 3 1 1 270.111 4.75729 1 4 1 1 72.6428 3.47094 1 -4 1 4 149.553 7.59229 -2 4 1 1 149.553 7.59229 1 -4 1 3 282.240 16.8054 -2 4 1 1 282.240 16.8054 1 4 1 1 49.4206 2.32966 2 -5 1 4 115.432 2.43337 -2 5 1 1 115.432 2.43337 1 -6 1 5 175.999 4.68746 -2 6 1 1 175.999 4.68746 1 -7 1 5 42.2331 6.94797 -2 7 1 1 42.2331 6.94797 1 -8 1 6 5.33291 2.40518 -2 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-2 2 3 25 28.7465 18.7858 1 3 4 23 10.6580 4.64091 -2 -3 4 25 10.6580 4.64091 1 2 4 24 -3.0320 10.2133 -2 -2 4 25 -3.0320 10.2133 1 1 4 24 13.8350 7.21866 -2 -1 4 25 13.8350 7.21866 1 0 4 25 1.98712 3.56132 -2 0 4 25 1.98712 3.56132 1 -1 4 26 11.9983 8.70959 -2 1 4 25 11.9983 8.70959 1 3 5 23 16.3490 5.47809 -2 -3 5 25 16.3490 5.47809 1 2 5 24 3.88599 7.10993 -2 -2 5 25 3.88599 7.10993 1 2 5 24 -3.9163 14.3041 -2 2 5 23 -3.9163 14.3041 -2 -2 5 25 -3.9163 14.3041 1 1 5 24 1.27523 7.20851 -2 -1 5 25 1.27523 7.20851 1 0 5 25 48.7299 5.39382 -2 0 5 25 48.7299 5.39382 1 1 5 25 7.26507 2.80505 2 1 6 24 8.55789 10.9162 -2 -1 6 25 8.55789 10.9162 1 3 0 24 15.8635 7.06752 -2 -3 0 26 15.8635 7.06752 1 2 0 25 23.0108 8.91714 -2 -2 0 26 23.0108 8.91714 1 1 0 25 6.41194 7.65008 -2 -1 0 26 6.41194 7.65008 1 0 0 26 31.6829 7.03356 -2 0 0 26 31.6829 7.03356 1 -1 0 27 -10.239 11.3551 -2 1 0 26 -10.239 11.3551 1 3 1 24 13.3930 4.50775 -2 -3 1 26 13.3930 4.50775 1 2 1 25 15.6998 7.58988 -2 -2 1 26 15.6998 7.58988 1 1 1 25 10.8779 7.10765 -2 -1 1 26 10.8779 7.10765 1 0 1 26 -1.3501 4.56874 -2 0 1 26 -1.3501 4.56874 1 -1 1 27 7.88369 7.81873 -2 1 1 26 7.88369 7.81873 1 3 2 24 3.19057 5.30002 -2 -3 2 26 3.19057 5.30002 1 2 2 25 38.5933 8.53347 -2 -2 2 26 38.5933 8.53347 1 1 2 25 7.50684 5.79663 -2 -1 2 26 7.50684 5.79663 1 0 2 26 155.110 12.7734 -2 0 2 26 155.110 12.7734 1 -1 2 27 27.6308 6.57304 -2 1 2 26 27.6308 6.57304 1 1 2 26 6.80484 9.65583 2 3 3 24 11.9403 5.35823 -2 -3 3 26 11.9403 5.35823 1 2 3 25 23.6112 6.23450 -2 -2 3 26 23.6112 6.23450 1 1 3 25 29.4934 8.14698 -2 -1 3 26 29.4934 8.14698 1 0 3 26 29.1121 5.02644 -2 0 3 26 29.1121 5.02644 1 1 3 26 12.6811 3.06076 2 1 3 26 15.8588 4.33466 1 -2 4 26 20.1152 3.41258 1 -2 4 26 9.34668 3.03744 2 1 4 25 35.0443 6.56986 -2 -1 4 26 35.0443 6.56986 1 0 4 26 3.20778 3.27596 -2 0 4 26 3.20778 3.27596 1 -2 0 27 3.79110 3.37754 1 -2 0 27 0.79204 3.28128 2 1 0 26 2.82741 10.4270 -2 -1 0 27 2.82741 10.4270 1 0 0 27 4.02577 6.76184 -2 0 0 27 4.02577 6.76184 1 -2 1 27 24.6922 3.36471 1 -2 1 27 10.0723 3.00226 2 1 1 26 22.5727 8.60998 -2 -1 1 27 22.5727 8.60998 1 0 1 27 12.9213 5.01773 -2 0 1 27 12.9213 5.01773 1 -2 2 27 7.16416 6.95261 2 -2 2 27 2.89178 6.65015 1 1 2 26 16.5763 6.86778 -2 -1 2 27 16.5763 6.86778 1 0 2 27 14.0740 11.5174 -2 0 2 27 14.0740 11.5174 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 97433 _shelx_res_file ; TITL jtm1424_4_a.res in P2(1)/c jtm1424_5.res created by SHELXL-2018/3 at 16:26:01 on 17-Feb-2021 REM Old TITL jtm1424_4 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.167, Rweak 0.014, Alpha 0.029 REM 2.188 for 172 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N3 O3 CELL 0.71073 7.0111 11.0123 20.4930 90.000 96.202 90.000 ZERR 4.000 0.0008 0.0013 0.0023 0.000 0.005 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 76 64 8 16 TEMP -123 SIZE 0.114 0.223 0.336 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 HTAB N1 O2 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB N2 O3_$1 CONF ACTA 50 MPLA O1 C10 > C14 MPLA 6 C1 > C6 N1 N2 MPLA O4 C16 > C19 OMIT 2 6 0 OMIT 0 1 1 OMIT 2 6 1 OMIT 0 0 2 OMIT -2 6 1 DFIX 0.91 0.01 N1 H1 N2 H2A WGHT 0.064800 2.983800 BASF 0.22364 FVAR 0.83411 O1 4 0.874878 0.520856 0.310784 11.00000 0.03717 0.03197 = 0.02332 0.00102 0.00519 -0.00227 O2 4 0.777880 0.354728 0.481399 11.00000 0.05556 0.04002 = 0.02012 -0.00051 0.00364 -0.01644 O3 4 0.804159 0.359189 0.250761 11.00000 0.04338 0.03926 = 0.02130 -0.00263 0.00172 0.00278 O4 4 0.684521 -0.115771 0.231600 11.00000 0.06283 0.04249 = 0.05219 0.00245 0.01820 0.00524 N1 3 0.741318 0.152820 0.421684 11.00000 0.03931 0.03030 = 0.02298 -0.00179 0.00234 -0.00775 H1 2 0.749615 0.206478 0.455743 11.00000 0.05153 N2 3 0.486125 0.034088 0.323109 11.00000 0.03345 0.03899 = 0.02535 0.00062 0.00382 -0.00785 H2A 2 0.380871 -0.006262 0.304933 11.00000 0.06588 C1 1 0.564834 -0.028315 0.379908 11.00000 0.03172 0.03166 = 0.02628 -0.00331 0.01060 -0.00007 C2 1 0.502176 -0.144760 0.393514 11.00000 0.04043 0.03073 = 0.03426 -0.00495 0.01117 -0.00416 AFIX 43 H2 2 0.417357 -0.185984 0.361639 11.00000 -1.20000 AFIX 0 C3 1 0.560846 -0.201507 0.452399 11.00000 0.05657 0.02796 = 0.04194 0.00286 0.02158 -0.00515 AFIX 43 H3 2 0.515597 -0.280802 0.460548 11.00000 -1.20000 AFIX 0 C4 1 0.684680 -0.143954 0.499503 11.00000 0.05480 0.04253 = 0.03109 0.01194 0.01292 0.00667 AFIX 43 H4 2 0.726016 -0.183596 0.539729 11.00000 -1.20000 AFIX 0 C5 1 0.747863 -0.027966 0.487472 11.00000 0.03883 0.04172 = 0.02498 0.00198 0.00622 0.00078 AFIX 43 H5 2 0.831745 0.012667 0.519869 11.00000 -1.20000 AFIX 0 C6 1 0.689458 0.029620 0.428270 11.00000 0.03401 0.02568 = 0.02516 -0.00014 0.00927 -0.00270 C7 1 0.780224 0.206969 0.366884 11.00000 0.02467 0.03235 = 0.02377 -0.00087 0.00197 -0.00494 C8 1 0.800126 0.124645 0.309832 11.00000 0.04061 0.03376 = 0.02955 -0.00252 0.00929 -0.00444 AFIX 23 H8A 2 0.873700 0.051597 0.325464 11.00000 -1.20000 H8B 2 0.873351 0.167001 0.277963 11.00000 -1.20000 AFIX 0 C9 1 0.607560 0.085957 0.275729 11.00000 0.03819 0.03414 = 0.02508 -0.00033 0.00728 -0.00178 AFIX 13 H9 2 0.541795 0.160745 0.256997 11.00000 -1.20000 AFIX 0 C10 1 0.810842 0.334339 0.367100 11.00000 0.02921 0.02811 = 0.02130 0.00079 0.00368 -0.00437 C11 1 0.812199 0.402495 0.427654 11.00000 0.02972 0.03441 = 0.02184 -0.00005 0.00088 -0.00794 C12 1 0.857979 0.529398 0.425000 11.00000 0.03568 0.02885 = 0.02273 -0.00313 0.00210 -0.00553 AFIX 43 H12 2 0.864632 0.576254 0.464103 11.00000 -1.20000 AFIX 0 C13 1 0.891325 0.583023 0.369126 11.00000 0.02957 0.02989 = 0.02770 -0.00110 0.00401 -0.00110 C14 1 0.827741 0.398363 0.306732 11.00000 0.02536 0.02853 = 0.02533 0.00053 0.00273 -0.00055 C15 1 0.948966 0.710795 0.361366 11.00000 0.04917 0.03444 = 0.03540 0.00226 0.01380 -0.00448 AFIX 137 H15A 2 0.967050 0.750057 0.404507 11.00000 -1.50000 H15B 2 0.848667 0.753521 0.333246 11.00000 -1.50000 H15C 2 1.069420 0.713570 0.341196 11.00000 -1.50000 AFIX 0 C16 1 0.632491 0.002204 0.219285 11.00000 0.03449 0.02890 = 0.02818 -0.00044 0.00436 -0.00537 C17 1 0.623633 0.026849 0.155105 11.00000 0.03643 0.05642 = 0.02191 0.01016 0.00417 0.00836 AFIX 43 H17 2 0.594168 0.102485 0.134101 11.00000 -1.20000 AFIX 0 C18 1 0.668749 -0.086892 0.124513 11.00000 0.03345 0.09038 = 0.03525 -0.02649 0.00342 -0.00261 AFIX 43 H18 2 0.671856 -0.100553 0.078868 11.00000 -1.20000 AFIX 0 C19 1 0.704396 -0.167262 0.171316 11.00000 0.04792 0.04707 = 0.07806 -0.02331 0.02530 -0.00302 AFIX 43 H19 2 0.739039 -0.249397 0.164714 11.00000 -1.20000 AFIX 0 HKLF 5 REM jtm1424_4_a.res in P2(1)/c REM wR2 = 0.213757, GooF = S = 1.13637, Restrained GooF = 1.13616 for all data REM R1 = 0.078640 for 4007 Fo > 4sig(Fo) and 0.103851 for all 5201 data REM 236 parameters refined using 2 restraints END WGHT 0.0648 2.9838 REM Highest difference peak 0.540, deepest hole -0.298, 1-sigma level 0.079 Q1 1 0.6696 -0.0010 0.1204 11.00000 0.05 0.54 Q2 1 0.6507 0.0846 0.1631 11.00000 0.05 0.39 Q3 1 1.0035 0.8533 0.4275 11.00000 0.05 0.33 Q4 1 0.5689 0.0285 0.1501 11.00000 0.05 0.33 Q5 1 1.0615 0.8436 0.4671 11.00000 0.05 0.31 ; _shelx_res_checksum 24709 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.8749(4) 0.5209(2) 0.31078(12) 0.0307(6) Uani d 1 . . O O2 0.7779(4) 0.3547(3) 0.48140(13) 0.0386(7) Uani d 1 . . O O3 0.8042(4) 0.3592(3) 0.25076(12) 0.0348(7) Uani d 1 . . O O4 0.6845(5) -0.1158(3) 0.23160(17) 0.0516(9) Uani d 1 . . N N1 0.7413(5) 0.1528(3) 0.42168(15) 0.0309(7) Uani d 1 . . H H1 0.750(7) 0.206(3) 0.4557(16) 0.052(14) Uiso d 1 . . N N2 0.4861(5) 0.0341(3) 0.32311(16) 0.0325(8) Uani d 1 . . H H2A 0.381(5) -0.006(4) 0.305(2) 0.066(17) Uiso d 1 . . C C1 0.5648(5) -0.0283(3) 0.37991(18) 0.0293(8) Uani d 1 . . C C2 0.5022(6) -0.1448(4) 0.3935(2) 0.0346(9) Uani d 1 . . H H2 0.417357 -0.185984 0.361639 0.042 Uiso calc 1 . . C C3 0.5608(7) -0.2015(4) 0.4524(2) 0.0410(11) Uani d 1 . . H H3 0.515597 -0.280802 0.460548 0.049 Uiso calc 1 . . C C4 0.6847(7) -0.1440(4) 0.4995(2) 0.0422(11) Uani d 1 . . H H4 0.726016 -0.183596 0.539729 0.051 Uiso calc 1 . . C C5 0.7479(6) -0.0280(4) 0.48747(19) 0.0350(9) Uani d 1 . . H H5 0.831745 0.012667 0.519869 0.042 Uiso calc 1 . . C C6 0.6895(6) 0.0296(3) 0.42827(18) 0.0278(8) Uani d 1 . . C C7 0.7802(5) 0.2070(3) 0.36688(18) 0.0270(8) Uani d 1 . . C C8 0.8001(6) 0.1246(4) 0.30983(19) 0.0342(9) Uani d 1 . . H H8A 0.873700 0.051597 0.325464 0.041 Uiso calc 1 . . H H8B 0.873351 0.167001 0.277963 0.041 Uiso calc 1 . . C C9 0.6076(6) 0.0860(4) 0.27573(19) 0.0322(9) Uani d 1 . . H H9 0.541795 0.160745 0.256997 0.039 Uiso calc 1 . . C C10 0.8108(5) 0.3343(3) 0.36710(17) 0.0261(8) Uani d 1 . . C C11 0.8122(5) 0.4025(3) 0.42765(18) 0.0288(8) Uani d 1 . . C C12 0.8580(5) 0.5294(3) 0.42500(18) 0.0292(8) Uani d 1 . . H H12 0.864632 0.576254 0.464103 0.035 Uiso calc 1 . . C C13 0.8913(6) 0.5830(3) 0.36913(19) 0.0290(8) Uani d 1 . . C C14 0.8277(5) 0.3984(3) 0.30673(18) 0.0264(8) Uani d 1 . . C C15 0.9490(7) 0.7108(4) 0.3614(2) 0.0390(10) Uani d 1 . . H H15A 0.967050 0.750057 0.404507 0.058 Uiso calc 1 . . H H15B 0.848667 0.753521 0.333246 0.058 Uiso calc 1 . . H H15C 1.069420 0.713570 0.341196 0.058 Uiso calc 1 . . C C16 0.6325(6) 0.0022(3) 0.21928(19) 0.0305(8) Uani d 1 . . C C17 0.6236(6) 0.0268(4) 0.15511(18) 0.0382(10) Uani d 1 . . H H17 0.594168 0.102485 0.134101 0.046 Uiso calc 1 . . C C18 0.6687(7) -0.0869(5) 0.1245(2) 0.0530(14) Uani d 1 . . H H18 0.671856 -0.100553 0.078868 0.064 Uiso calc 1 . . C C19 0.7044(7) -0.1673(5) 0.1713(3) 0.0563(14) Uani d 1 . . H H19 0.739039 -0.249397 0.164714 0.068 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0372(16) 0.0320(14) 0.0233(13) -0.0023(12) 0.0052(11) 0.0010(11) O2 0.0556(18) 0.0400(16) 0.0201(13) -0.0164(14) 0.0036(12) -0.0005(12) O3 0.0434(17) 0.0393(16) 0.0213(13) 0.0028(13) 0.0017(12) -0.0026(11) O4 0.063(2) 0.0425(18) 0.052(2) 0.0052(16) 0.0182(17) 0.0024(16) N1 0.0393(19) 0.0303(17) 0.0230(16) -0.0078(15) 0.0023(14) -0.0018(13) N2 0.0335(19) 0.0390(19) 0.0253(16) -0.0079(15) 0.0038(14) 0.0006(14) C1 0.032(2) 0.032(2) 0.0263(19) -0.0001(17) 0.0106(16) -0.0033(16) C2 0.040(2) 0.031(2) 0.034(2) -0.0042(18) 0.0112(18) -0.0050(17) C3 0.057(3) 0.028(2) 0.042(2) -0.005(2) 0.022(2) 0.0029(18) C4 0.055(3) 0.043(2) 0.031(2) 0.007(2) 0.013(2) 0.0119(19) C5 0.039(2) 0.042(2) 0.0250(19) 0.0008(19) 0.0062(17) 0.0020(17) C6 0.034(2) 0.0257(18) 0.0252(18) -0.0027(16) 0.0093(15) -0.0001(15) C7 0.0247(19) 0.0323(19) 0.0238(18) -0.0049(16) 0.0020(15) -0.0009(15) C8 0.041(2) 0.034(2) 0.030(2) -0.0044(18) 0.0093(17) -0.0025(17) C9 0.038(2) 0.034(2) 0.0251(19) -0.0018(18) 0.0073(16) -0.0003(16) C10 0.029(2) 0.0281(18) 0.0213(17) -0.0044(15) 0.0037(15) 0.0008(14) C11 0.030(2) 0.034(2) 0.0218(18) -0.0079(16) 0.0009(15) -0.0001(15) C12 0.036(2) 0.0288(19) 0.0227(18) -0.0055(16) 0.0021(15) -0.0031(15) C13 0.030(2) 0.0299(19) 0.0277(19) -0.0011(16) 0.0040(16) -0.0011(15) C14 0.0254(19) 0.0285(19) 0.0253(18) -0.0006(15) 0.0027(15) 0.0005(15) C15 0.049(3) 0.034(2) 0.035(2) -0.004(2) 0.014(2) 0.0023(18) C16 0.034(2) 0.0289(19) 0.0282(19) -0.0054(17) 0.0044(16) -0.0004(16) C17 0.036(2) 0.056(3) 0.0219(19) 0.008(2) 0.0042(17) 0.0102(18) C18 0.033(3) 0.090(4) 0.035(2) -0.003(3) 0.003(2) -0.026(3) C19 0.048(3) 0.047(3) 0.078(4) -0.003(2) 0.025(3) -0.023(3) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C13 O1 C14 . . 122.3(3) ? C16 O4 C19 . . 106.0(4) ? C7 N1 C6 . . 126.2(3) ? C7 N1 H1 . . 111(3) ? C6 N1 H1 . . 123(3) ? C1 N2 C9 . . 122.0(3) ? C1 N2 H2A . . 109(3) ? C9 N2 H2A . . 115(3) ? C2 C1 C6 . . 117.6(4) ? C2 C1 N2 . . 120.6(4) ? C6 C1 N2 . . 121.3(3) ? C3 C2 C1 . . 121.4(4) ? C3 C2 H2 . . 119.3 ? C1 C2 H2 . . 119.3 ? C4 C3 C2 . . 120.6(4) ? C4 C3 H3 . . 119.7 ? C2 C3 H3 . . 119.7 ? C3 C4 C5 . . 119.3(4) ? C3 C4 H4 . . 120.4 ? C5 C4 H4 . . 120.4 ? C4 C5 C6 . . 120.5(4) ? C4 C5 H5 . . 119.8 ? C6 C5 H5 . . 119.8 ? C5 C6 C1 . . 120.8(4) ? C5 C6 N1 . . 117.8(3) ? C1 C6 N1 . . 121.1(3) ? N1 C7 C10 . . 119.1(3) ? N1 C7 C8 . . 115.7(3) ? C10 C7 C8 . . 125.0(3) ? C7 C8 C9 . . 112.2(3) ? C7 C8 H8A . . 109.2 ? C9 C8 H8A . . 109.2 ? C7 C8 H8B . . 109.2 ? C9 C8 H8B . . 109.2 ? H8A C8 H8B . . 107.9 ? N2 C9 C16 . . 113.1(3) ? N2 C9 C8 . . 110.8(3) ? C16 C9 C8 . . 110.8(3) ? N2 C9 H9 . . 107.3 ? C16 C9 H9 . . 107.3 ? C8 C9 H9 . . 107.3 ? C7 C10 C14 . . 120.5(3) ? C7 C10 C11 . . 120.1(3) ? C14 C10 C11 . . 119.2(3) ? O2 C11 C12 . . 120.1(3) ? O2 C11 C10 . . 123.0(3) ? C12 C11 C10 . . 116.9(3) ? C13 C12 C11 . . 121.7(3) ? C13 C12 H12 . . 119.2 ? C11 C12 H12 . . 119.2 ? C12 C13 O1 . . 121.5(3) ? C12 C13 C15 . . 126.2(4) ? O1 C13 C15 . . 112.3(3) ? O3 C14 O1 . . 114.0(3) ? O3 C14 C10 . . 128.3(3) ? O1 C14 C10 . . 117.7(3) ? C13 C15 H15A . . 109.5 ? C13 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C13 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C17 C16 O4 . . 111.0(4) ? C17 C16 C9 . . 129.4(4) ? O4 C16 C9 . . 119.5(3) ? C16 C17 C18 . . 105.1(4) ? C16 C17 H17 . . 127.4 ? C18 C17 H17 . . 127.4 ? C19 C18 C17 . . 107.5(4) ? C19 C18 H18 . . 126.3 ? C17 C18 H18 . . 126.3 ? C18 C19 O4 . . 110.4(4) ? C18 C19 H19 . . 124.8 ? O4 C19 H19 . . 124.8 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C13 . 1.372(4) ? O1 C14 . 1.389(4) ? O2 C11 . 1.267(4) ? O3 C14 . 1.220(4) ? O4 C16 . 1.366(5) ? O4 C19 . 1.380(6) ? N1 C7 . 1.326(5) ? N1 C6 . 1.415(5) ? N1 H1 . 0.912(12) ? N2 C1 . 1.412(5) ? N2 C9 . 1.474(5) ? N2 H2A . 0.906(12) ? C1 C2 . 1.393(5) ? C1 C6 . 1.402(5) ? C2 C3 . 1.382(6) ? C2 H2 . 0.9500 ? C3 C4 . 1.381(6) ? C3 H3 . 0.9500 ? C4 C5 . 1.383(6) ? C4 H4 . 0.9500 ? C5 C6 . 1.391(5) ? C5 H5 . 0.9500 ? C7 C10 . 1.419(5) ? C7 C8 . 1.498(5) ? C8 C9 . 1.513(6) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 C16 . 1.504(5) ? C9 H9 . 1.0000 ? C10 C14 . 1.440(5) ? C10 C11 . 1.449(5) ? C11 C12 . 1.436(5) ? C12 C13 . 1.331(5) ? C12 H12 . 0.9500 ? C13 C15 . 1.477(5) ? C15 H15A . 0.9800 ? C15 H15B . 0.9800 ? C15 H15C . 0.9800 ? C16 C17 . 1.338(5) ? C17 C18 . 1.451(7) ? C17 H17 . 0.9500 ? C18 C19 . 1.309(7) ? C18 H18 . 0.9500 ? C19 H19 . 0.9500 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O2 C3 3.322(5) . 3_656 no O2 N1 2.537(4) . . yes O2 C12 3.282(4) . 3_766 no O3 C9 3.372(4) . . no O3 C8 2.856(4) . . yes O3 N2 3.079(4) . 2_655 yes O4 N2 2.955(5) . . yes O4 C1 3.376(5) . . no O1 H2A 2.84(4) . 2_655 no O2 H12 2.74 . 3_766 yes O2 H3 2.62 . 3_656 yes O2 H1 1.72(3) . . yes O3 H9 2.87 . . no O3 H2A 2.20(4) . 2_655 yes H15C O3 2.70 . 2_755 yes O3 H2 2.68 . 2_655 yes O3 H8B 2.23 . . yes O4 H8A 2.88 . . no O4 H15B 2.70 . 1_545 yes N1 N2 2.865(4) . . yes N2 H19 2.89 . 2_655 no C3 C15 3.591(6) . 1_545 no C4 C6 3.387(5) . 3_656 yes C10 C18 3.497(6) . 2_655 no C11 C17 3.600(5) . 2_655 no C11 C18 3.428(5) . 2_655 no C12 C12 3.541(5) . 3_766 no C12 C17 3.589(5) . 2_655 no C14 C16 3.407(5) . 2_655 yes C1 H8A 2.68 . . yes C2 H17 2.91 . 2_645 no C3 H17 2.93 . 2_645 no C6 H8A 2.59 . . yes C11 H1 2.28(3) . . yes C14 H2A 2.79(4) . 2_655 yes C14 H8B 2.64 . . yes H2 H2A 2.29 . . yes H2 H17 2.33 . 2_645 yes H3 H17 2.38 . 2_645 yes H5 H1 2.55 . . no H12 H15A 2.42 . . yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O2 . 0.912(12) 1.72(3) 2.538(4) 148(4) yes N2 H2A O3 2_645 0.906(12) 2.20(2) 3.079(4) 162(5) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C9 N2 C1 C2 . . . . -126.6(4) ? C9 N2 C1 C6 . . . . 61.5(5) ? C6 C1 C2 C3 . . . . -0.2(6) ? N2 C1 C2 C3 . . . . -172.4(4) ? C1 C2 C3 C4 . . . . -0.3(6) ? C2 C3 C4 C5 . . . . 0.8(7) ? C3 C4 C5 C6 . . . . -0.8(6) ? C4 C5 C6 C1 . . . . 0.4(6) ? C4 C5 C6 N1 . . . . 173.1(4) ? C2 C1 C6 C5 . . . . 0.1(5) ? N2 C1 C6 C5 . . . . 172.2(4) ? C2 C1 C6 N1 . . . . -172.3(3) ? N2 C1 C6 N1 . . . . -0.2(5) ? C7 N1 C6 C5 . . . . 147.3(4) ? C7 N1 C6 C1 . . . . -40.0(6) ? C6 N1 C7 C10 . . . . 173.6(4) ? C6 N1 C7 C8 . . . . -10.1(6) ? N1 C7 C8 C9 . . . . 79.4(4) ? C10 C7 C8 C9 . . . . -104.5(4) ? C1 N2 C9 C16 . . . . 94.4(4) ? C1 N2 C9 C8 . . . . -30.7(5) ? C7 C8 C9 N2 . . . . -52.9(4) ? C7 C8 C9 C16 . . . . -179.3(3) ? N1 C7 C10 C14 . . . . -171.6(4) ? C8 C7 C10 C14 . . . . 12.4(6) ? N1 C7 C10 C11 . . . . 4.1(6) ? C8 C7 C10 C11 . . . . -171.9(4) ? C7 C10 C11 O2 . . . . -3.5(6) ? C14 C10 C11 O2 . . . . 172.3(4) ? C7 C10 C11 C12 . . . . 175.6(3) ? C14 C10 C11 C12 . . . . -8.6(5) ? O2 C11 C12 C13 . . . . -178.7(4) ? C10 C11 C12 C13 . . . . 2.2(6) ? C11 C12 C13 O1 . . . . 3.1(6) ? C11 C12 C13 C15 . . . . -176.7(4) ? C14 O1 C13 C12 . . . . -1.7(6) ? C14 O1 C13 C15 . . . . 178.1(3) ? C13 O1 C14 O3 . . . . 174.5(3) ? C13 O1 C14 C10 . . . . -4.9(5) ? C7 C10 C14 O3 . . . . 6.4(6) ? C11 C10 C14 O3 . . . . -169.4(4) ? C7 C10 C14 O1 . . . . -174.3(3) ? C11 C10 C14 O1 . . . . 9.9(5) ? C19 O4 C16 C17 . . . . -1.4(5) ? C19 O4 C16 C9 . . . . -177.3(4) ? N2 C9 C16 C17 . . . . 135.7(4) ? C8 C9 C16 C17 . . . . -99.2(5) ? N2 C9 C16 O4 . . . . -49.3(5) ? C8 C9 C16 O4 . . . . 75.8(5) ? O4 C16 C17 C18 . . . . 1.8(5) ? C9 C16 C17 C18 . . . . 177.1(4) ? C16 C17 C18 C19 . . . . -1.4(5) ? C17 C18 C19 O4 . . . . 0.6(6) ? C16 O4 C19 C18 . . . . 0.5(5) ? _cod_database_fobs_code 2243880