#------------------------------------------------------------------------------ #$Date: 2019-11-30 07:36:12 +0200 (Sat, 30 Nov 2019) $ #$Revision: 244830 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243211.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_2243211 loop_ _publ_author_name 'Ben Ali, Abdelkader' 'El Bakri, Youness' 'Lai, Chin-Hung' 'Sebhaoui, Jihad' 'El Ghayati, Lhoussaine' 'Essassi, El Mokhtar' 'Mague, Joel T.' _publ_section_title ; Crystal structure, computational study and Hirshfeld surface analysis of ethyl (2S,3R)-3-(3-amino-1H-1,2,4-triazol-1-yl)-2-hydroxy-3-phenylpropanoate ; _journal_coeditor_code TX2015 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1919 _journal_page_last 1924 _journal_paper_doi 10.1107/S2056989019015743 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C13 H16 N4 O3' _chemical_formula_moiety 'C13 H16 N4 O3' _chemical_formula_sum 'C13 H16 N4 O3' _chemical_formula_weight 276.30 _chemical_name_systematic 'Ethyl (2S,3R)-3-(3-amino-1H-1,2,4-triazol-1-yl)-2-hydroxy-3-phenylpropanoate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 94.3080(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4766(2) _cell_length_b 9.4841(2) _cell_length_c 16.9904(3) _cell_measurement_reflns_used 8615 _cell_measurement_temperature 150.(2) _cell_measurement_theta_max 74.5052 _cell_measurement_theta_min 2.6080 _cell_volume 1362.05(5) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0235 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10203 _diffrn_reflns_theta_full 70.000 _diffrn_reflns_theta_max 74.497 _diffrn_reflns_theta_min 5.221 _diffrn_source 'INCOATEC I\mS micro--focus source' _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thick plate' _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.344 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.085 _refine_diff_density_max 0.219 _refine_diff_density_min -0.156 _refine_ls_extinction_coef 0.0057(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 246 _refine_ls_number_reflns 2718 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0325 _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^)+(0.0378P)^2^+0.3844P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.0840 _reflns_number_gt 2485 _reflns_number_total 2718 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tx2015sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2243211 _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 0.766 _shelx_estimated_absorpt_t_max 0.934 _shelx_hkl_file ; 1 0 0 0.90 0.10 2 0 0 11.40 0.60 -2 0 0 10.60 0.60 -3 0 0 0.20 0.30 3 0 0 0.90 0.30 4 0 0 4686.23 154.08 -4 0 0 5286.37 155.78 -5 0 0 0.30 0.60 -5 0 0 0.20 0.70 -6 0 0 141.09 5.70 6 0 0 152.18 5.20 7 0 0 0.00 0.60 8 0 0 3.20 1.10 9 0 0 0.00 0.60 10 0 0 31.70 1.90 0 -1 0 0.20 0.10 0 1 0 0.30 0.10 1 -1 0 1761.62 51.79 -1 -1 0 1605.64 50.59 1 1 0 1632.24 50.59 -1 1 0 1535.15 50.79 -2 -1 0 2976.10 95.19 2 -1 0 3158.08 95.49 2 1 0 3154.88 95.29 -2 1 0 2985.90 95.89 3 -1 0 923.31 28.20 -3 -1 0 866.51 28.00 -3 1 0 916.31 28.10 3 1 0 907.41 28.10 -4 -1 0 999.90 31.40 4 -1 0 963.90 31.70 -4 -1 0 1039.00 31.50 4 1 0 981.40 31.60 -4 1 0 1055.49 31.60 -5 -1 0 144.19 5.10 -5 -1 0 137.09 5.30 6 -1 0 81.09 3.20 6 -1 0 68.29 3.40 6 -1 0 70.69 3.50 -6 -1 0 78.69 3.20 6 1 0 75.09 3.00 7 -1 0 5.50 1.30 -7 -1 0 5.20 1.60 7 -1 0 3.80 0.90 7 1 0 7.10 1.10 8 -1 0 19.50 2.40 8 1 0 16.20 1.40 8 1 0 14.40 2.10 9 -1 0 9.30 1.20 9 1 0 10.70 1.10 10 -1 0 22.70 1.30 10 1 0 21.40 1.30 1 -2 0 4661.43 141.19 -1 2 0 4468.95 140.89 -2 -2 0 1483.75 45.70 2 -2 0 1486.75 46.10 2 2 0 1452.55 45.90 -2 2 0 1463.65 46.00 -3 -2 0 3.40 0.80 3 -2 0 2.90 0.80 -3 -2 0 3.60 0.50 -3 2 0 3.50 0.50 3 2 0 3.20 0.60 -4 -2 0 3.60 0.80 -4 -2 0 1.90 0.80 4 2 0 5.70 1.10 -4 2 0 3.70 0.80 -5 -2 0 662.63 21.20 5 -2 0 653.43 21.00 -5 -2 0 661.53 21.00 6 -2 0 8.10 1.50 -6 -2 0 7.40 1.20 -6 -2 0 5.70 1.40 6 -2 0 8.20 1.30 6 -2 0 9.00 2.00 7 -2 0 0.30 1.30 -7 -2 0 0.40 0.70 7 -2 0 1.50 0.90 7 -2 0 0.30 0.80 7 2 0 1.80 0.60 -8 -2 0 21.60 2.20 8 -2 0 23.80 1.80 8 2 0 22.40 1.50 9 -2 0 17.70 1.40 9 2 0 16.50 1.30 10 -2 0 8.50 1.00 10 2 0 9.10 0.90 1 -3 0 206.38 6.50 -1 3 0 197.98 6.40 2 -3 0 123.39 4.30 -2 -3 0 119.39 4.00 2 3 0 129.39 4.00 -2 3 0 121.09 4.20 -3 -3 0 897.01 28.00 -3 -3 0 879.11 28.20 3 -3 0 924.71 28.40 3 3 0 914.31 28.00 -3 3 0 897.51 28.20 -4 -3 0 6.10 1.00 -4 -3 0 5.20 1.40 -4 3 0 6.70 1.10 5 -3 0 141.59 5.50 -5 -3 0 153.18 5.20 -5 -3 0 146.19 5.20 -5 -3 0 159.28 5.50 5 -3 0 139.49 5.70 5 -3 0 149.19 5.60 5 -3 0 148.09 5.30 6 -3 0 87.59 4.10 -6 -3 0 97.89 3.90 6 -3 0 96.39 3.70 6 -3 0 81.09 3.90 -6 -3 0 91.99 3.60 -7 -3 0 1.50 0.80 -7 -3 0 2.70 1.20 7 -3 0 3.60 1.30 7 -3 0 1.50 0.80 7 -3 0 1.40 0.70 -8 -3 0 4.30 1.40 8 -3 0 2.00 0.80 8 3 0 3.40 0.90 9 -3 0 36.30 1.90 9 3 0 37.00 1.80 10 -3 0 51.69 2.20 10 3 0 53.09 2.10 -1 4 0 470.55 14.70 2 -4 0 70.29 2.80 -2 -4 0 67.39 2.70 -2 4 0 68.39 2.60 -3 -4 0 20.40 1.40 -3 -4 0 19.70 1.00 3 -4 0 17.20 2.00 -3 4 0 19.80 1.30 3 4 0 19.00 1.00 -4 -4 0 87.09 3.30 -4 -4 0 87.99 3.50 -4 -4 0 90.29 3.30 4 -4 0 81.89 3.80 4 -4 0 85.29 3.50 4 -4 0 83.79 3.60 -4 4 0 81.79 3.70 5 -4 0 -1.00 0.80 -5 -4 0 1.90 0.70 5 -4 0 1.70 1.30 -5 -4 0 -0.30 0.70 5 -4 0 0.40 1.00 5 -4 0 0.40 0.70 -5 -4 0 -0.70 0.50 6 -4 0 70.59 3.70 6 -4 0 73.59 3.30 -6 -4 0 76.89 3.10 -6 -4 0 75.89 3.40 6 -4 0 73.79 3.50 6 -4 0 77.39 3.20 7 -4 0 38.10 2.00 7 -4 0 33.20 2.30 7 -4 0 37.10 2.70 -7 -4 0 38.20 2.30 -7 -4 0 37.50 2.00 8 -4 0 15.80 2.20 -8 -4 0 17.80 1.70 8 4 0 19.10 1.70 -9 -4 0 84.09 3.80 9 -4 0 82.29 3.30 -9 4 0 78.69 3.20 9 4 0 85.49 3.10 -1 -5 0 846.92 27.00 -1 5 0 875.01 26.70 -2 -5 0 16.90 1.40 -2 5 0 18.20 1.30 3 -5 0 14.90 1.70 -3 -5 0 17.30 1.40 3 -5 0 13.40 2.00 3 -5 0 14.50 1.60 -3 -5 0 15.20 1.30 -3 -5 0 16.80 1.50 3 -5 0 13.00 2.30 -3 5 0 15.60 1.70 -4 -5 0 156.38 5.80 4 -5 0 154.88 6.00 -4 -5 0 155.28 5.50 -4 -5 0 156.28 5.50 4 -5 0 157.68 6.00 4 -5 0 153.68 5.60 4 -5 0 158.68 5.60 5 -5 0 66.49 3.60 5 -5 0 67.09 3.40 -5 -5 0 71.09 3.20 -5 -5 0 68.69 2.90 5 -5 0 68.49 3.00 6 -5 0 -1.60 1.20 6 -5 0 0.80 0.60 6 -5 0 1.30 1.10 -6 -5 0 2.40 0.70 6 -5 0 0.80 0.80 7 -5 0 0.80 1.30 -7 -5 0 0.10 0.60 7 -5 0 -1.50 0.80 -7 -5 0 0.10 0.50 7 -5 0 0.10 0.80 8 -5 0 12.50 1.40 -8 -5 0 12.10 1.40 8 5 0 14.30 1.00 9 -5 0 51.39 2.20 9 5 0 49.40 2.10 -9 5 0 50.99 2.10 0 -6 0 364.56 12.10 0 -6 0 375.16 12.20 1 -6 0 218.78 7.60 -1 -6 0 221.28 7.50 -1 -6 0 214.98 7.60 1 -6 0 223.68 7.70 -1 -6 0 215.48 7.50 1 -6 0 220.48 7.50 -2 -6 0 109.09 4.10 2 -6 0 106.99 4.30 2 -6 0 102.69 4.30 2 -6 0 99.29 4.10 -2 -6 0 103.69 4.00 2 -6 0 104.39 4.10 -2 -6 0 100.59 4.00 -3 -6 0 143.29 5.30 3 -6 0 138.59 5.10 3 -6 0 139.39 5.20 -3 -6 0 138.69 5.00 -3 -6 0 135.99 5.00 3 -6 0 140.79 5.40 3 -6 0 133.19 5.40 4 -6 0 239.88 9.70 -4 -6 0 234.88 8.00 -4 -6 0 245.78 8.40 4 -6 0 234.08 8.10 4 -6 0 242.78 8.30 4 -6 0 231.18 8.50 -5 -6 0 116.49 4.30 -5 -6 0 120.99 4.70 5 -6 0 111.59 4.40 5 -6 0 109.39 4.70 5 -6 0 115.99 4.80 5 -6 0 108.99 5.70 -5 -6 0 115.99 4.20 6 -6 0 29.20 1.80 -6 -6 0 27.60 1.60 6 -6 0 27.90 1.70 6 -6 0 28.30 2.30 -6 -6 0 24.50 1.90 6 -6 0 27.50 2.10 7 -6 0 19.50 1.80 7 -6 0 21.80 2.10 -7 -6 0 21.50 1.40 7 -6 0 23.10 1.60 -8 -6 0 47.20 2.50 8 -6 0 48.30 2.60 8 6 0 50.69 2.50 9 -6 0 34.70 1.60 9 6 0 34.60 1.40 0 -7 0 -0.20 0.70 0 -7 0 -0.10 0.80 0 -7 0 0.10 0.70 1 -7 0 66.49 2.90 -1 -7 0 64.79 2.90 -1 -7 0 64.99 3.00 1 -7 0 65.89 3.10 -1 -7 0 60.19 2.90 1 -7 0 64.09 3.00 2 -7 0 82.19 4.50 2 -7 0 97.29 4.10 2 -7 0 94.99 4.10 -2 -7 0 90.09 4.20 -2 -7 0 103.59 4.00 -2 -7 0 98.99 3.90 2 -7 0 98.29 3.90 -3 -7 0 605.14 19.30 3 -7 0 609.34 19.80 3 -7 0 595.34 19.50 -3 -7 0 601.94 19.40 -3 -7 0 595.94 19.60 3 -7 0 615.04 19.40 3 -7 0 618.54 19.70 4 -7 0 5.80 1.20 -4 -7 0 4.50 1.30 4 -7 0 8.00 1.80 -4 -7 0 4.90 1.10 4 -7 0 5.30 1.60 -5 -7 0 8.30 1.10 5 -7 0 9.00 1.20 5 -7 0 6.70 1.10 -5 -7 0 4.70 1.00 -5 -7 0 6.10 1.20 5 -7 0 6.70 1.70 5 -7 0 6.50 1.60 -6 -7 0 17.50 1.80 6 -7 0 19.60 1.80 -6 -7 0 17.70 1.60 6 -7 0 16.40 1.80 -7 -7 0 45.80 1.90 7 -7 0 43.40 2.00 7 -7 0 43.70 2.50 8 -7 0 2.10 0.50 8 7 0 3.00 0.60 -8 7 0 2.20 0.60 0 -8 0 11.40 1.50 0 -8 0 11.40 1.50 0 -8 0 11.50 1.40 1 -8 0 24.60 1.90 1 -8 0 26.80 1.80 -1 -8 0 26.70 1.80 1 -8 0 25.80 1.90 2 -8 0 207.38 7.30 -2 -8 0 199.28 7.30 -2 -8 0 205.78 7.10 2 -8 0 198.68 7.10 2 -8 0 197.68 7.30 -2 -8 0 201.98 7.30 -3 -8 0 28.30 2.10 3 -8 0 30.80 2.20 3 -8 0 28.30 2.10 -3 -8 0 27.80 1.90 -3 -8 0 28.50 1.70 3 -8 0 28.40 2.00 -4 -8 0 19.70 1.90 4 -8 0 27.00 2.80 4 -8 0 16.60 1.80 -4 -8 0 22.50 1.40 4 -8 0 22.00 1.60 -4 -8 0 21.40 1.40 -5 -8 0 26.80 2.00 5 -8 0 25.20 2.50 -5 -8 0 26.10 1.90 5 -8 0 26.40 1.90 -5 -8 0 23.90 2.00 6 -8 0 197.28 7.00 -6 -8 0 191.88 7.50 -6 -8 0 203.58 6.60 6 -8 0 201.28 6.70 6 -8 0 195.58 6.70 -7 -8 0 27.50 1.80 -7 -8 0 26.80 1.30 7 -8 0 24.60 1.30 7 -8 0 28.30 1.50 0 -9 0 0.40 0.70 0 -9 0 -0.30 0.60 0 -9 0 -0.20 0.70 1 -9 0 4.70 1.20 -1 -9 0 5.00 1.10 -1 -9 0 5.90 1.10 1 -9 0 5.00 1.30 2 -9 0 218.88 7.70 2 -9 0 224.88 7.90 -2 -9 0 222.28 7.60 -2 -9 0 226.08 7.70 2 -9 0 224.48 7.80 3 -9 0 392.66 13.00 -3 -9 0 391.86 12.70 -3 -9 0 384.86 12.70 3 -9 0 397.96 12.80 3 -9 0 390.06 13.50 4 -9 0 4.90 1.20 4 -9 0 5.60 1.00 -4 -9 0 12.70 2.90 -4 -9 0 7.80 0.90 -4 -9 0 7.70 0.90 4 -9 0 9.00 1.30 5 -9 0 7.60 1.20 5 -9 0 6.80 1.10 -5 -9 0 7.30 0.80 -5 -9 0 6.90 0.80 -5 -9 0 10.30 1.60 5 -9 0 7.90 0.90 6 -9 0 7.00 0.90 -6 -9 0 7.10 0.80 6 -9 0 6.60 0.70 -6 9 0 7.40 1.00 0 -10 0 0.70 0.50 0 -10 0 0.20 0.50 1 -10 0 42.90 2.20 1 -10 0 43.70 2.10 -1 -10 0 42.90 2.10 -1 -10 0 45.40 2.10 2 -10 0 0.00 0.50 -2 -10 0 0.30 0.50 2 -10 0 0.70 0.60 -2 -10 0 0.00 0.70 2 -10 0 0.40 0.50 3 -10 0 8.30 1.10 -3 -10 0 8.90 0.80 3 -10 0 9.80 1.10 3 -10 0 9.20 1.10 -3 -10 0 8.90 0.90 -4 -10 0 0.20 0.40 4 -10 0 -0.50 0.50 -4 -10 0 0.30 0.40 4 -10 0 0.90 0.60 4 -10 0 -0.40 0.50 -4 10 0 -1.10 0.90 -5 -10 0 0.40 0.40 5 -10 0 0.40 0.50 -5 10 0 -1.00 0.70 0 -11 0 0.00 0.40 -1 -11 0 8.70 0.80 -1 -11 0 8.90 0.80 1 -11 0 9.70 0.90 1 -11 0 8.60 0.90 -2 -11 0 14.30 0.90 -2 -11 0 12.60 0.90 2 -11 0 14.70 1.00 2 -11 0 13.00 1.00 -3 -11 0 0.30 0.30 -3 -11 0 2.30 0.60 3 -11 0 1.10 0.50 10 0 -1 0.20 0.50 9 0 -1 11.30 1.20 8 0 -1 0.80 0.70 8 0 -1 -0.60 0.90 7 0 -1 34.90 2.00 6 0 -1 -0.40 0.60 -5 0 1 275.67 9.30 -5 0 1 288.07 9.60 -4 0 1 -0.50 0.30 4 0 -1 -0.50 0.50 -3 0 1 3.10 0.40 3 0 -1 3.40 0.50 2 0 -1 0.00 0.10 -2 0 1 0.20 0.10 0 0 -1 0.00 0.10 -3 0 -1 7980.30 251.27 3 0 1 8261.17 251.47 4 0 1 -0.10 0.50 -4 0 -1 -0.10 0.30 -5 0 -1 66.59 3.10 -5 0 -1 68.39 2.90 6 0 1 4.10 1.10 7 0 1 15.10 1.40 8 0 1 -0.90 0.60 9 0 1 109.49 4.20 10 0 1 -0.50 0.50 10 -1 -1 3.70 0.90 10 1 -1 3.60 0.80 9 -1 -1 38.20 2.00 9 1 -1 37.40 2.00 8 -1 -1 25.50 2.00 8 -1 -1 22.10 2.20 8 1 -1 26.10 1.70 7 -1 -1 38.50 2.50 7 -1 -1 39.50 2.20 -7 -1 1 37.90 2.40 7 1 -1 36.10 2.00 6 -1 -1 33.90 1.90 -6 -1 1 33.80 2.00 -6 -1 1 32.80 1.90 6 -1 -1 27.50 2.30 6 1 -1 34.80 1.80 -5 -1 1 232.18 8.10 -5 -1 1 235.78 7.80 -5 1 1 227.28 8.40 4 -1 -1 659.53 22.50 -4 -1 1 706.33 22.30 -4 -1 1 749.62 22.40 -4 1 1 729.83 22.40 4 1 -1 702.53 22.40 -3 -1 1 464.55 14.60 3 -1 -1 468.25 14.80 -3 1 1 459.05 14.70 3 1 -1 468.55 14.70 2 -1 -1 2376.26 72.09 -2 -1 1 2283.07 72.29 -2 1 1 2343.27 73.09 2 1 -1 2275.57 72.09 1 -1 -1 117.79 3.70 -1 -1 1 116.49 3.70 -1 1 1 110.79 3.70 1 1 -1 118.79 3.70 0 -1 -1 501.05 15.50 0 1 1 503.85 15.50 1 -1 1 772.82 23.90 -1 -1 -1 756.92 23.50 1 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-18 25.00 1.90 3 1 18 25.40 1.50 3 1 18 27.40 1.90 4 -1 18 10.60 0.90 4 -1 18 8.30 0.90 4 1 18 11.30 0.90 -5 2 18 26.10 1.40 -4 2 18 0.50 0.50 3 -2 -18 19.40 2.20 -3 -2 18 20.20 1.50 -3 2 18 20.30 1.40 2 -2 -18 30.90 2.10 -2 -2 18 30.90 1.80 -2 2 18 27.70 1.70 1 -2 -18 0.30 0.70 -1 -2 18 -0.80 0.60 -1 2 18 0.10 0.60 -1 2 18 0.20 0.70 0 -2 18 72.89 3.10 0 -2 -18 73.39 3.30 0 2 18 69.49 3.00 0 2 18 73.99 2.90 -1 -2 -18 16.80 1.60 1 -2 18 15.60 1.50 1 -2 18 15.40 1.20 -1 2 -18 15.00 2.40 1 2 18 15.40 1.30 1 2 18 17.40 1.20 2 -2 18 31.50 1.70 2 -2 18 31.70 1.70 -2 -2 -18 30.70 1.90 2 2 18 31.40 1.60 2 2 18 30.70 1.70 -2 2 -18 32.00 2.10 3 -2 18 20.50 1.30 -3 -2 -18 22.80 1.60 3 -2 18 21.70 1.30 3 2 18 20.70 1.30 3 2 18 23.40 1.50 4 -2 18 28.20 1.40 4 -2 18 29.10 1.40 4 2 18 27.40 1.30 -5 3 18 1.10 0.50 -4 3 18 0.30 0.60 -3 3 18 38.20 1.90 2 -3 -18 8.70 2.00 -2 -3 18 5.50 1.20 -2 3 18 4.90 0.90 1 -3 -18 4.60 1.10 -1 -3 18 5.00 1.10 -1 3 18 5.50 1.10 -1 3 18 6.40 1.00 0 -3 -18 50.29 2.60 0 -3 18 48.60 2.30 0 3 18 50.19 2.20 0 3 18 49.00 2.30 -1 -3 -18 16.50 1.50 1 -3 18 12.90 2.40 1 -3 18 17.20 1.20 -1 3 -18 14.70 1.70 1 3 18 16.00 1.30 1 3 18 15.20 1.10 2 -3 18 123.39 4.40 2 -3 18 124.79 4.40 -2 -3 -18 124.59 4.70 3 -3 18 12.40 0.90 3 -3 18 14.40 1.10 -3 -3 -18 14.20 1.40 3 3 18 12.50 0.90 4 -3 18 78.69 2.80 4 -3 18 78.49 2.70 4 3 18 75.79 2.70 -5 4 18 22.70 1.20 -3 4 18 37.80 1.90 -2 4 18 18.60 1.40 -1 -4 18 4.50 1.10 1 -4 -18 7.20 1.90 -1 4 18 5.60 1.00 -1 4 18 4.10 0.90 0 -4 -18 3.50 1.40 0 -4 18 2.10 0.60 0 4 18 2.10 0.50 0 4 18 4.00 0.90 1 -4 18 122.99 4.30 -1 -4 -18 127.39 4.60 1 4 18 109.49 4.20 1 4 18 117.59 4.20 2 -4 18 118.89 4.10 -2 -4 -18 118.09 4.50 2 -4 18 115.69 4.10 2 4 18 116.59 4.10 3 -4 18 37.10 1.60 3 -4 18 33.80 1.50 3 4 18 34.80 1.50 -4 5 18 5.40 0.80 -3 5 18 -0.40 0.40 -2 5 18 6.40 1.10 -1 5 18 2.60 0.90 0 -5 18 0.10 0.60 0 5 18 -0.90 0.70 0 5 18 -0.10 0.50 1 -5 18 34.80 1.60 2 -5 18 9.10 0.80 2 5 18 9.20 0.80 -1 6 18 2.20 0.60 0 6 18 6.70 0.80 1 6 18 26.00 1.20 -4 0 19 0.50 0.60 -3 0 19 235.88 8.00 -2 0 19 -0.20 0.50 1 0 -19 0.80 0.60 -1 0 19 0.30 0.50 0 0 -19 0.40 0.60 0 0 19 0.20 0.50 0 0 19 -1.10 0.80 1 0 19 44.00 2.10 1 0 19 43.00 2.00 -1 0 -19 46.50 2.30 2 0 19 -0.40 0.50 -2 0 -19 0.10 0.70 2 0 19 0.10 0.50 3 0 19 14.80 1.10 3 0 19 13.70 1.00 4 0 19 0.20 0.40 -4 -1 19 5.60 1.20 3 -1 -19 5.50 1.60 -3 -1 19 5.20 1.00 -3 1 19 5.40 0.90 2 -1 -19 1.10 0.80 -2 -1 19 0.00 0.50 -2 1 19 1.10 0.50 -1 -1 19 2.20 0.60 1 -1 -19 1.40 0.70 -1 1 19 2.50 0.80 0 -1 -19 3.60 1.30 0 -1 19 3.70 0.90 0 1 19 5.00 1.10 0 1 19 3.90 0.80 1 -1 19 3.30 1.10 -1 -1 -19 2.80 1.20 1 -1 19 4.50 0.80 1 1 19 3.20 0.90 -1 1 -19 5.10 1.30 1 1 19 3.80 0.90 2 -1 19 13.20 1.10 -2 -1 -19 14.00 1.40 2 -1 19 12.10 1.00 2 1 19 13.10 1.00 2 1 19 11.70 1.10 -2 1 -19 13.60 1.60 3 -1 19 2.50 0.80 3 -1 19 1.40 0.50 3 1 19 0.90 0.40 3 1 19 3.80 1.00 -4 2 19 24.90 1.50 -3 -2 19 6.00 1.20 -3 2 19 8.60 1.50 -2 -2 19 30.90 1.60 2 -2 -19 29.90 2.20 -2 2 19 31.60 1.70 -1 -2 19 1.10 0.60 1 -2 -19 0.10 0.80 -1 2 19 0.30 0.50 0 -2 -19 43.80 2.40 0 -2 19 44.10 2.10 0 2 19 45.50 2.00 0 2 -19 45.80 2.40 0 2 19 43.50 2.10 1 -2 19 64.79 2.60 -1 -2 -19 66.09 2.90 1 2 19 64.69 2.60 -1 2 -19 64.49 3.00 1 2 19 65.29 2.50 2 -2 19 0.70 0.60 -2 -2 -19 3.00 1.10 2 -2 19 1.00 0.50 2 2 19 1.70 0.60 2 2 19 1.70 0.50 3 -2 19 12.80 1.00 3 -2 19 11.70 0.90 3 2 19 13.00 0.90 -4 3 19 24.90 1.30 -3 3 19 1.00 0.50 -2 -3 19 15.40 1.30 -2 3 19 15.10 1.10 -1 -3 19 49.40 2.10 1 -3 -19 46.30 2.60 -1 3 19 47.20 2.10 -1 3 19 49.10 2.20 0 -3 -19 21.10 1.70 0 -3 19 21.90 1.30 0 3 19 21.20 1.70 0 3 19 22.30 1.30 0 3 -19 18.30 1.70 1 -3 19 0.30 0.50 -1 -3 -19 -0.10 0.70 1 3 19 0.40 0.50 1 3 19 1.20 0.60 2 3 19 42.10 1.80 3 -3 19 6.50 0.70 3 3 19 6.70 0.70 -3 4 19 30.60 1.50 -2 4 19 2.60 0.80 -1 -4 19 5.40 1.20 -1 4 19 3.00 0.70 -1 4 19 2.90 0.80 0 -4 19 2.70 0.90 0 4 19 0.90 0.50 0 4 19 0.20 0.60 1 -4 19 12.70 1.00 1 4 19 10.30 0.90 2 -4 19 84.89 3.00 2 4 19 83.69 2.90 0 5 19 -0.30 0.50 -3 0 20 0.30 0.50 2 0 -20 103.09 4.20 -2 0 20 110.69 3.90 1 0 -20 0.80 0.70 0 0 20 129.19 4.60 0 0 -20 134.69 4.90 1 0 20 0.20 0.50 -1 0 -20 0.70 0.70 1 0 20 1.20 0.70 2 0 20 44.20 1.80 2 0 20 43.00 1.80 -4 1 20 0.90 0.50 -3 -1 20 30.30 1.50 -3 1 20 29.70 1.40 2 1 -20 11.00 1.40 -2 1 20 13.40 1.00 -1 -1 20 8.60 0.90 1 -1 -20 9.30 1.50 -1 1 20 9.90 0.90 1 1 -20 10.80 1.40 0 -1 -20 14.90 1.60 0 -1 20 19.00 1.20 0 1 20 18.00 1.20 0 1 -20 18.90 1.60 1 -1 20 1.90 0.70 -1 -1 -20 0.00 0.90 1 1 20 1.10 0.80 1 1 20 0.60 0.60 2 -1 20 10.50 0.80 2 1 20 7.80 0.90 2 1 20 7.80 0.90 -3 2 20 98.19 3.50 -2 -2 20 53.09 2.20 -1 -2 20 17.60 1.20 -1 2 20 18.10 1.10 0 2 20 17.80 2.00 0 2 20 13.40 1.20 1 -2 20 0.40 0.40 1 2 20 0.70 0.50 1 2 20 0.50 0.50 2 -2 20 0.70 0.40 2 2 20 -0.20 0.40 -3 3 20 35.70 1.50 -2 3 20 7.90 0.80 -1 -3 20 2.00 0.60 -1 3 20 2.90 0.70 0 -3 20 78.29 2.80 0 3 20 78.99 2.90 1 -3 20 13.30 1.00 1 3 20 16.50 1.00 -2 0 21 0.40 0.50 -1 0 21 91.99 3.20 0 0 21 0.20 0.40 -2 1 21 41.30 1.70 -1 -1 21 79.09 2.80 -1 1 21 75.99 2.80 0 -1 21 157.28 5.20 0 1 21 156.48 5.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35355 _shelx_res_file ; TITL JTM1126_0m_a.res in P2(1)/n JTM1126_0m_a.res created by SHELXL-2018/3 at 15:32:27 on 06-Sep-2019 REM Old TITL JTM1126_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.128, Rweak 0.004, Alpha 0.016, Orientation as input REM Formula found by SHELXT: C14 N3 O3 CELL 1.54178 8.4766 9.4841 16.9904 90.000 94.308 90.000 ZERR 4.000 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 52 64 16 12 TEMP -123 SIZE 0.085 0.22 0.344 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 EQIV $1 -x+3/2, y-1/2, -z+1/2 HTAB O1 N3_$1 EQIV $2 -x+3/2, y+1/2, -z+1/2 HTAB N4 O2_$2 EQIV $3 -x+2, -y+1, -z HTAB N4 N1_$3 HTAB C2 O1 EQIV $4 -x+2, -y+1, -z+1 HTAB C12 O1_$4 CONF MPLA C4 > C9 MPLA C1 N1 N2 C2 N3 ACTA 140 WGHT 0.037800 0.384400 EXTI 0.005696 FVAR 0.83176 O1 4 0.916992 0.367856 0.329156 11.00000 0.02770 0.02589 = 0.02853 0.00164 0.00702 0.00193 H1 2 0.834909 0.319145 0.342917 11.00000 0.05106 O2 4 0.818076 0.452508 0.471359 11.00000 0.03813 0.03537 = 0.02584 0.00334 0.00644 -0.00437 O3 4 0.855017 0.680093 0.440128 11.00000 0.03873 0.03074 = 0.02324 -0.00160 0.00489 0.00094 N1 3 0.973547 0.505806 0.099650 11.00000 0.04129 0.04724 = 0.02469 0.00409 0.01134 0.01747 N2 3 0.851829 0.574349 0.202474 11.00000 0.02745 0.03074 = 0.02141 0.00278 0.00733 0.00487 N3 3 0.811677 0.672585 0.144527 11.00000 0.03083 0.02791 = 0.02173 0.00304 0.00768 0.00187 N4 3 0.889703 0.695052 0.014036 11.00000 0.05151 0.03974 = 0.02504 0.00521 0.01413 0.01248 H4A 2 0.819292 0.763932 0.006587 11.00000 0.03895 H4B 2 0.917358 0.640437 -0.025843 11.00000 0.04933 C1 1 0.889461 0.626752 0.084479 11.00000 0.02964 0.03347 = 0.02350 0.00050 0.00717 0.00246 C2 1 0.945260 0.477287 0.173578 11.00000 0.03764 0.04138 = 0.02572 0.00352 0.00867 0.01586 H2 2 0.980238 0.396533 0.203463 11.00000 0.04329 C3 1 0.783169 0.584362 0.278611 11.00000 0.02788 0.02721 = 0.01963 0.00093 0.00787 0.00338 H3 2 0.779977 0.685244 0.291429 11.00000 0.02735 C4 1 0.616772 0.524840 0.276373 11.00000 0.02489 0.03075 = 0.02441 0.00500 0.00392 0.00520 C5 1 0.556668 0.434460 0.217320 11.00000 0.02976 0.03571 = 0.02889 0.00227 0.00126 0.00529 H5 2 0.618500 0.414096 0.172018 11.00000 0.03036 C6 1 0.408161 0.373246 0.221963 11.00000 0.03333 0.04619 = 0.04187 0.00031 -0.00652 -0.00080 H6 2 0.371850 0.312155 0.181123 11.00000 0.05060 C7 1 0.319940 0.401861 0.285399 11.00000 0.02533 0.06255 = 0.05008 0.01030 0.00263 -0.00276 H7 2 0.220494 0.354035 0.288849 11.00000 0.05599 C8 1 0.375913 0.496368 0.342597 11.00000 0.02785 0.06579 = 0.03823 0.00521 0.00990 0.00272 H8 2 0.310967 0.519841 0.388789 11.00000 0.05586 C9 1 0.522844 0.558812 0.337958 11.00000 0.02857 0.04795 = 0.02899 0.00072 0.00739 0.00468 H9 2 0.561432 0.630606 0.380498 11.00000 0.04494 C10 1 0.897944 0.512192 0.341754 11.00000 0.02458 0.02704 = 0.02375 0.00046 0.00420 0.00009 H10 2 1.002392 0.558049 0.337749 11.00000 0.02538 C11 1 0.851200 0.542680 0.425180 11.00000 0.02513 0.02982 = 0.02375 0.00054 0.00130 -0.00039 C12 1 0.813498 0.722298 0.519084 11.00000 0.03756 0.04228 = 0.02362 -0.00589 0.00430 0.00477 H12A 2 0.698013 0.713108 0.519464 11.00000 0.04146 H12B 2 0.865379 0.654291 0.557852 11.00000 0.03920 C13 1 0.872096 0.868527 0.533083 11.00000 0.07120 0.04100 = 0.04138 -0.00994 -0.00128 0.00270 H13A 2 0.839439 0.905364 0.588395 11.00000 0.07705 H13B 2 0.821122 0.931617 0.491776 11.00000 0.07561 H13C 2 1.000019 0.870446 0.533977 11.00000 0.07113 HKLF 4 REM JTM1126_0m_a.res in P2(1)/n REM wR2 = 0.083978, GooF = S = 1.05187, Restrained GooF = 1.05187 for all data REM R1 = 0.032459 for 2485 Fo > 4sig(Fo) and 0.035592 for all 2718 data REM 246 parameters refined using 0 restraints END WGHT 0.0378 0.3844 REM Highest difference peak 0.219, deepest hole -0.156, 1-sigma level 0.034 Q1 1 0.8364 0.5469 0.3116 11.00000 0.05 0.22 Q2 1 0.6980 0.5536 0.2769 11.00000 0.05 0.20 Q3 1 0.3781 0.4255 0.3233 11.00000 0.05 0.18 Q4 1 0.8647 0.5276 0.3802 11.00000 0.05 0.18 Q5 1 0.8200 0.5710 0.2387 11.00000 0.05 0.16 ; _shelx_res_checksum 42629 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 O O1 0.91699(9) 0.36786(8) 0.32916(5) 0.02713(19) Uani d 1 H H1 0.835(2) 0.3191(18) 0.3429(10) 0.051(5) Uiso d 1 O O2 0.81808(10) 0.45251(9) 0.47136(5) 0.0329(2) Uani d 1 O O3 0.85502(10) 0.68009(8) 0.44013(4) 0.0308(2) Uani d 1 N N1 0.97355(13) 0.50581(12) 0.09965(6) 0.0373(3) Uani d 1 N N2 0.85183(11) 0.57435(10) 0.20247(5) 0.0263(2) Uani d 1 N N3 0.81168(11) 0.67258(10) 0.14453(5) 0.0265(2) Uani d 1 N N4 0.88970(15) 0.69505(13) 0.01404(6) 0.0382(3) Uani d 1 H H4A 0.8193(19) 0.7639(17) 0.0066(9) 0.039(4) Uiso d 1 H H4B 0.917(2) 0.6404(18) -0.0258(10) 0.049(4) Uiso d 1 C C1 0.88946(13) 0.62675(12) 0.08448(6) 0.0286(3) Uani d 1 C C2 0.94526(15) 0.47729(14) 0.17358(7) 0.0346(3) Uani d 1 H H2 0.9802(18) 0.3965(17) 0.2035(9) 0.043(4) Uiso d 1 C C3 0.78317(13) 0.58436(12) 0.27861(6) 0.0246(2) Uani d 1 H H3 0.7800(16) 0.6852(14) 0.2914(8) 0.027(3) Uiso d 1 C C4 0.61677(13) 0.52484(12) 0.27637(6) 0.0266(2) Uani d 1 C C5 0.55667(14) 0.43446(13) 0.21732(7) 0.0315(3) Uani d 1 H H5 0.6185(16) 0.4141(14) 0.1720(8) 0.030(3) Uiso d 1 C C6 0.40816(16) 0.37325(15) 0.22196(8) 0.0409(3) Uani d 1 H H6 0.372(2) 0.3122(18) 0.1811(10) 0.051(4) Uiso d 1 C C7 0.31994(16) 0.40186(17) 0.28540(9) 0.0460(3) Uani d 1 H H7 0.220(2) 0.3540(19) 0.2888(10) 0.056(5) Uiso d 1 C C8 0.37591(15) 0.49637(17) 0.34260(8) 0.0436(3) Uani d 1 H H8 0.311(2) 0.5198(18) 0.3888(10) 0.056(5) Uiso d 1 C C9 0.52284(14) 0.55881(15) 0.33796(7) 0.0349(3) Uani d 1 H H9 0.5614(19) 0.6306(17) 0.3805(9) 0.045(4) Uiso d 1 C C10 0.89794(13) 0.51219(11) 0.34175(6) 0.0250(2) Uani d 1 H H10 1.0024(15) 0.5580(13) 0.3377(7) 0.025(3) Uiso d 1 C C11 0.85120(13) 0.54268(12) 0.42518(6) 0.0263(2) Uani d 1 C C12 0.81350(16) 0.72230(14) 0.51908(7) 0.0344(3) Uani d 1 H H12A 0.6980(19) 0.7131(16) 0.5195(9) 0.041(4) Uiso d 1 H H12B 0.8654(17) 0.6543(16) 0.5579(9) 0.039(4) Uiso d 1 C C13 0.8721(2) 0.86853(16) 0.53308(10) 0.0515(4) Uani d 1 H H13A 0.839(2) 0.905(2) 0.5884(13) 0.077(6) Uiso d 1 H H13B 0.821(2) 0.932(2) 0.4918(12) 0.076(6) Uiso d 1 H H13C 1.000(3) 0.870(2) 0.5340(11) 0.071(6) Uiso d 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 0.0277(4) 0.0259(4) 0.0285(4) 0.0019(3) 0.0070(3) 0.0016(3) O2 0.0381(5) 0.0354(4) 0.0258(4) -0.0044(3) 0.0064(3) 0.0033(3) O3 0.0387(5) 0.0307(4) 0.0232(4) 0.0009(3) 0.0049(3) -0.0016(3) N1 0.0413(6) 0.0472(6) 0.0247(5) 0.0175(5) 0.0113(4) 0.0041(4) N2 0.0274(5) 0.0307(5) 0.0214(4) 0.0049(4) 0.0073(4) 0.0028(4) N3 0.0308(5) 0.0279(5) 0.0217(4) 0.0019(4) 0.0077(4) 0.0030(4) N4 0.0515(7) 0.0397(6) 0.0250(5) 0.0125(5) 0.0141(5) 0.0052(4) C1 0.0296(6) 0.0335(6) 0.0235(5) 0.0025(4) 0.0072(4) 0.0005(4) C2 0.0376(7) 0.0414(7) 0.0257(6) 0.0159(5) 0.0087(5) 0.0035(5) C3 0.0279(5) 0.0272(5) 0.0196(5) 0.0034(4) 0.0079(4) 0.0009(4) C4 0.0249(5) 0.0307(6) 0.0244(5) 0.0052(4) 0.0039(4) 0.0050(4) C5 0.0298(6) 0.0357(6) 0.0289(6) 0.0053(5) 0.0013(5) 0.0023(5) C6 0.0333(7) 0.0462(8) 0.0419(7) -0.0008(5) -0.0065(5) 0.0003(6) C7 0.0253(6) 0.0625(9) 0.0501(8) -0.0028(6) 0.0026(6) 0.0103(7) C8 0.0279(6) 0.0658(9) 0.0382(7) 0.0027(6) 0.0099(5) 0.0052(6) C9 0.0286(6) 0.0480(7) 0.0290(6) 0.0047(5) 0.0074(5) 0.0007(5) C10 0.0246(5) 0.0270(5) 0.0237(5) 0.0001(4) 0.0042(4) 0.0005(4) C11 0.0251(5) 0.0298(6) 0.0237(5) -0.0004(4) 0.0013(4) 0.0005(4) C12 0.0376(7) 0.0423(7) 0.0236(6) 0.0048(5) 0.0043(5) -0.0059(5) C13 0.0712(11) 0.0410(8) 0.0414(8) 0.0027(7) -0.0013(7) -0.0099(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C10 O1 H1 111.7(11) C11 O3 C12 116.00(9) C2 N1 C1 102.80(10) C2 N2 N3 108.99(9) C2 N2 C3 131.21(10) N3 N2 C3 119.65(8) C1 N3 N2 102.53(9) C1 N4 H4A 115.5(10) C1 N4 H4B 114.0(11) H4A N4 H4B 121.9(14) N3 C1 N4 123.58(11) N3 C1 N1 114.34(10) N4 C1 N1 122.06(10) N1 C2 N2 111.32(11) N1 C2 H2 126.7(9) N2 C2 H2 121.9(9) N2 C3 C4 112.65(9) N2 C3 C10 108.22(8) C4 C3 C10 112.74(9) N2 C3 H3 106.2(8) C4 C3 H3 109.1(8) C10 C3 H3 107.6(8) C5 C4 C9 118.98(11) C5 C4 C3 122.57(10) C9 C4 C3 118.41(10) C4 C5 C6 120.04(12) C4 C5 H5 120.0(8) C6 C5 H5 120.0(8) C7 C6 C5 120.36(13) C7 C6 H6 122.1(10) C5 C6 H6 117.6(10) C8 C7 C6 119.90(13) C8 C7 H7 121.3(10) C6 C7 H7 118.8(10) C7 C8 C9 120.01(13) C7 C8 H8 120.6(10) C9 C8 H8 119.4(10) C8 C9 C4 120.54(12) C8 C9 H9 118.8(9) C4 C9 H9 120.6(9) O1 C10 C11 111.63(9) O1 C10 C3 113.57(9) C11 C10 C3 111.41(9) O1 C10 H10 107.7(7) C11 C10 H10 106.0(7) C3 C10 H10 106.0(7) O2 C11 O3 125.05(10) O2 C11 C10 123.90(10) O3 C11 C10 111.04(9) O3 C12 C13 107.49(11) O3 C12 H12A 106.8(9) C13 C12 H12A 113.7(9) O3 C12 H12B 107.6(9) C13 C12 H12B 111.8(9) H12A C12 H12B 109.1(12) C12 C13 H13A 110.1(12) C12 C13 H13B 109.0(12) H13A C13 H13B 107.4(17) C12 C13 H13C 109.9(11) H13A C13 H13C 108.1(15) H13B C13 H13C 112.4(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C10 1.3968(13) O1 H1 0.881(18) O2 C11 1.2079(14) O3 C11 1.3277(14) O3 C12 1.4679(13) N1 C2 1.3242(15) N1 C1 1.3648(15) N2 C2 1.3319(15) N2 N3 1.3794(13) N2 C3 1.4609(13) N3 C1 1.3288(14) N4 C1 1.3610(15) N4 H4A 0.887(16) N4 H4B 0.898(18) C2 H2 0.954(16) C3 C4 1.5171(15) C3 C10 1.5522(15) C3 H3 0.982(14) C4 C5 1.3871(17) C4 C9 1.3992(16) C5 C6 1.3939(18) C5 H5 0.982(14) C6 C7 1.384(2) C6 H6 0.938(17) C7 C8 1.380(2) C7 H7 0.963(18) C8 C9 1.3867(18) C8 H8 1.017(18) C9 H9 1.028(16) C10 C11 1.5278(15) C10 H10 0.993(13) C12 C13 1.486(2) C12 H12A 0.983(16) C12 H12B 1.000(15) C13 H13A 1.06(2) C13 H13B 1.00(2) C13 H13C 1.08(2) 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 O1 H1 N3 2_645 0.881(18) 1.887(18) 2.7417(12) 162.9(16) yes N4 H4A O2 2_655 0.887(16) 2.182(17) 3.0317(14) 160.2(13) yes N4 H4B N1 3_765 0.898(18) 2.127(18) 3.0066(15) 166.1(15) yes C2 H2 O1 . 0.954(16) 2.257(16) 2.8665(14) 120.9(12) yes C12 H12B O1 3_766 1.000(15) 2.569(15) 3.4225(15) 143.2(11) yes C5 H5 Cg1 . 0.982(14) 2.856(14) 3.4816(13) 122.3(10) 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 C2 N2 N3 C1 -1.38(12) C3 N2 N3 C1 -177.37(10) N2 N3 C1 N4 -177.46(11) N2 N3 C1 N1 1.03(13) C2 N1 C1 N3 -0.29(15) C2 N1 C1 N4 178.23(12) C1 N1 C2 N2 -0.65(15) N3 N2 C2 N1 1.33(15) C3 N2 C2 N1 176.70(11) C2 N2 C3 C4 -94.74(14) N3 N2 C3 C4 80.22(12) C2 N2 C3 C10 30.59(16) N3 N2 C3 C10 -154.44(9) N2 C3 C4 C5 18.19(15) C10 C3 C4 C5 -104.64(12) N2 C3 C4 C9 -164.15(10) C10 C3 C4 C9 73.02(13) C9 C4 C5 C6 -3.29(17) C3 C4 C5 C6 174.36(11) C4 C5 C6 C7 -0.12(19) C5 C6 C7 C8 2.9(2) C6 C7 C8 C9 -2.3(2) C7 C8 C9 C4 -1.2(2) C5 C4 C9 C8 3.98(18) C3 C4 C9 C8 -173.77(11) N2 C3 C10 O1 -63.92(11) C4 C3 C10 O1 61.36(12) N2 C3 C10 C11 168.99(9) C4 C3 C10 C11 -65.74(12) C12 O3 C11 O2 -0.70(16) C12 O3 C11 C10 -179.49(9) O1 C10 C11 O2 -7.54(15) C3 C10 C11 O2 120.60(12) O1 C10 C11 O3 171.26(9) C3 C10 C11 O3 -60.59(12) C11 O3 C12 C13 162.57(11) _cod_database_fobs_code 2243211