#------------------------------------------------------------------------------ #$Date: 2019-10-30 08:06:10 +0200 (Wed, 30 Oct 2019) $ #$Revision: 220536 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/18/2021802.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_2021802 loop_ _publ_author_name 'Shishkina, Svitlana V.' 'Konovalova, Irina S.' 'Trostianko, Pavlo V.' 'Geleverya, Anna O.' 'Kovalenko, Sergiy M.' 'Bunyatyan, Natalya D.' _publ_section_title ; Polymorphism of 3-(5-phenyl-1,3,4-oxadiazol-2-yl)- and 3-[5-(pyridin-4-yl)-1,3,4-oxadiazol-2-yl]-2H-chromen-2-ones ; _journal_coeditor_code FN3326 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619014256 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C17 H10 N2 O3' _chemical_formula_moiety 'C17 H10 N2 O3' _chemical_formula_sum 'C17 H10 N2 O3' _chemical_formula_weight 290.27 _chemical_name_systematic ; 3-(5-Phenyl-1,3,4-oxadiazol-2-yl)-2H-chromen-2-one ; _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 90.74(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.611(5) _cell_length_b 3.8414(9) _cell_length_c 21.974(7) _cell_measurement_reflns_used 366 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.300 _cell_measurement_theta_min 5.390 _cell_volume 1317.6(7) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_publication_material ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku Xcalibur Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1169 _diffrn_reflns_av_unetI/netI 0.1211 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 7763 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.221 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.13483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2018) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.463 _exptl_crystal_description stick _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.175 _refine_diff_density_min -0.238 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 2322 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.904 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0667 _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^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.1501 _reflns_number_gt 1081 _reflns_number_total 2322 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file fn3326sup1.cif _cod_data_source_block 1B _cod_original_cell_volume 1317.6(6) _cod_database_code 2021802 _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 0.970 _shelx_estimated_absorpt_t_max 0.996 _shelx_hkl_file ; 0 0 4 9999.00 104.06 0 0 4 9892.40 104.00 0 0 5 6.25 4.28 0 0 5 -5.08 2.66 0 0 -5 2.37 5.19 0 0 6 229.14 19.44 0 0 6 219.98 18.67 0 0 7 -5.23 1.54 0 0 7 3.46 3.25 0 0 8 1716.58 61.00 0 0 8 1836.86 65.45 0 0 9 6.17 6.39 0 0 9 11.76 6.20 0 0 10 632.84 42.67 0 0 10 577.92 39.05 0 0 11 -1.96 1.22 0 0 11 2.71 3.46 0 0 12 18.58 6.43 0 0 12 20.15 9.58 0 0 13 6.55 8.74 0 0 13 -2.92 1.80 0 0 14 135.48 24.39 0 0 14 118.74 20.78 0 0 15 0.78 3.60 0 0 15 12.24 7.52 0 0 16 -0.28 5.04 0 0 16 6.54 6.94 0 0 17 -1.66 4.17 0 0 17 -2.73 2.61 0 0 18 9.25 33.67 0 0 18 9.96 9.03 0 0 19 -6.01 5.50 0 0 19 5.00 5.05 0 0 20 19.04 10.19 0 0 20 24.12 12.00 0 0 21 -1.83 4.23 0 0 21 0.18 1.22 0 0 22 47.71 20.40 0 0 22 18.74 15.00 0 0 23 12.72 11.03 0 0 23 4.41 2.83 0 0 24 3.49 7.12 0 0 24 1.02 5.50 0 0 25 -1.79 4.18 0 0 25 -11.62 9.02 0 0 26 3.00 7.24 0 0 26 10.89 9.13 0 0 27 6.72 2.68 0 0 27 7.85 9.00 0 0 28 4.69 10.84 0 0 28 0.36 5.60 0 0 29 -13.87 11.42 0 0 30 -0.19 7.10 0 0 31 -12.55 12.08 0 0 32 -4.54 8.73 0 -1 0 1.20 3.33 0 1 0 -2.60 1.90 0 -1 0 1.17 1.56 0 1 0 -2.50 2.27 0 -1 0 -1.29 2.20 0 1 0 -3.58 2.33 0 1 0 -11.22 4.49 0 -1 -1 4764.08 103.01 0 -1 1 4799.76 99.03 0 1 -1 4610.10 97.67 0 1 -1 4889.03 89.46 0 -1 1 4716.92 62.87 0 1 -1 4241.83 70.86 0 -1 1 4579.82 77.40 0 -1 -1 4185.27 67.45 0 -1 -1 4444.87 61.58 0 1 1 4628.02 72.35 0 1 -2 276.72 19.68 0 1 2 242.25 13.92 0 -1 -2 300.56 19.96 0 -1 2 367.97 24.24 0 1 2 348.13 22.55 0 -1 -2 370.13 29.47 0 -1 -2 376.20 15.11 0 -1 2 374.05 26.58 0 1 -2 395.86 28.56 0 -1 -3 4502.77 103.74 0 -1 3 4172.15 88.46 0 1 3 4325.64 86.58 0 -1 3 4320.51 87.45 0 1 -3 4763.17 90.74 0 1 -3 4669.17 98.97 0 -1 4 6842.10 107.08 0 -1 4 6996.16 121.20 0 1 4 7315.80 121.32 0 -1 -4 7460.69 137.08 0 1 -4 7279.76 122.19 0 -1 5 564.09 18.85 0 -1 -5 525.05 37.28 0 1 -5 468.04 30.22 0 1 -5 386.72 17.55 0 -1 5 536.88 35.65 0 1 5 512.28 35.28 0 -1 5 481.24 27.34 0 -1 6 100.93 15.95 0 -1 6 92.42 9.49 0 1 6 88.59 15.38 0 -1 -6 79.35 15.13 0 -1 6 77.70 10.89 0 1 -6 56.01 8.10 0 -1 7 92.57 16.59 0 1 7 97.30 8.53 0 -1 -7 92.21 16.00 0 1 -7 61.37 9.90 0 1 7 93.66 16.68 0 -1 7 74.40 9.87 0 -1 7 81.95 9.97 0 -1 8 13.33 3.91 0 1 8 22.64 4.46 0 1 8 23.44 10.33 0 -1 8 21.85 7.95 0 -1 -8 14.27 7.08 0 -1 8 18.55 4.97 0 1 9 193.57 26.43 0 -1 -9 183.84 24.05 0 1 9 176.01 15.09 0 -1 9 147.53 22.96 0 -1 9 184.34 18.24 0 1 10 51.42 8.85 0 1 10 50.72 15.17 0 -1 10 59.90 15.01 0 -1 10 52.77 10.80 0 1 11 97.94 13.65 0 -1 11 117.06 17.05 0 1 11 127.50 23.17 0 -1 11 77.97 17.25 0 1 12 172.19 19.64 0 -1 12 203.06 23.60 0 1 12 208.12 31.63 0 -1 12 179.03 26.34 0 1 13 196.36 32.66 0 -1 13 181.66 23.85 0 1 13 151.94 19.45 0 -1 13 170.47 27.10 0 1 14 50.01 17.74 0 1 14 45.02 11.30 0 -1 14 39.03 13.27 0 -1 14 38.25 11.17 0 1 15 15.22 9.40 0 1 15 25.29 9.05 0 -1 15 18.29 6.31 0 -1 15 29.12 10.97 0 1 16 26.23 13.73 0 1 16 16.96 8.95 0 -1 16 27.24 12.17 0 -1 16 19.58 9.11 0 1 17 3.50 5.62 0 -1 17 12.92 7.38 0 -1 17 9.28 6.35 0 1 17 16.83 13.38 0 1 18 36.50 12.51 0 -1 18 28.67 13.10 0 -1 18 35.19 12.18 0 1 18 34.57 13.71 0 1 19 8.59 11.62 0 1 19 6.16 4.64 0 -1 19 5.79 8.79 0 -1 19 0.82 2.94 0 1 20 18.13 10.71 0 1 20 8.76 8.19 0 -1 20 10.10 10.43 0 -1 20 -0.99 1.82 0 1 21 18.52 14.94 0 1 21 8.55 5.99 0 -1 21 17.46 13.63 0 -1 21 9.42 4.80 0 -1 22 35.21 14.96 0 1 22 37.30 19.56 0 -1 22 19.50 12.50 0 -1 23 6.53 7.07 0 -1 23 14.03 13.13 0 1 23 10.29 17.43 0 -1 24 4.76 1.38 0 1 24 17.48 15.59 0 -1 24 10.10 8.60 0 -1 25 -3.19 7.59 0 1 25 -4.08 9.13 0 -1 25 7.87 8.16 0 -1 26 3.58 5.50 0 -1 26 -5.60 8.74 0 1 26 -9.36 9.74 0 -1 27 18.01 14.30 0 -1 27 10.82 10.54 0 1 27 -5.93 8.46 0 -1 28 -0.53 2.20 0 1 28 21.59 17.05 0 1 29 -0.78 9.70 0 -1 29 8.05 11.05 0 -1 30 -8.91 9.47 0 1 30 -4.09 5.51 0 -1 31 10.55 14.51 0 -1 32 -0.27 8.09 0 2 0 57.20 8.70 0 2 0 87.45 19.64 0 -2 0 84.17 13.35 0 2 0 86.31 13.58 0 -2 0 74.53 17.09 0 -2 1 17.40 9.56 0 2 1 3.01 0.48 0 2 1 6.53 5.32 0 2 1 8.21 4.52 0 2 -1 17.28 7.45 0 -2 -1 9.88 5.40 0 -2 -1 21.27 7.72 0 -2 -1 7.23 2.04 0 2 -1 10.61 4.67 0 -2 1 10.56 6.29 0 2 -1 6.62 3.52 0 -2 -2 9.07 2.64 0 -2 -2 8.30 4.12 0 -2 -2 16.82 11.06 0 2 -2 6.49 1.96 0 -2 2 2.18 5.71 0 -2 2 13.87 6.07 0 2 -2 9.71 1.43 0 2 2 10.66 4.48 0 -2 3 0.76 3.42 0 -2 -3 -1.96 2.60 0 -2 -3 0.31 1.04 0 -2 -3 2.58 1.52 0 2 -3 0.54 3.69 0 2 3 0.46 6.45 0 -2 3 0.34 2.29 0 -2 -4 199.48 30.48 0 -2 4 183.97 25.43 0 -2 4 213.54 25.56 0 -2 -4 202.41 12.30 0 2 -4 208.10 28.00 0 2 4 243.14 29.70 0 -2 -4 212.62 13.95 0 -2 5 4.70 5.84 0 -2 5 2.63 4.05 0 -2 -5 1.54 1.56 0 2 -5 2.72 3.02 0 2 5 -9.70 5.98 0 -2 -5 -1.93 3.20 0 2 -6 5.79 3.41 0 -2 -6 -3.45 1.65 0 2 6 -2.66 6.14 0 -2 6 4.58 3.25 0 -2 -6 0.27 0.86 0 -2 6 -1.42 1.77 0 -2 7 -0.06 1.79 0 2 7 6.98 9.25 0 -2 7 -3.82 3.44 0 -2 -7 -0.85 1.49 0 -2 -7 -3.90 6.02 0 2 -7 3.58 3.04 0 2 -8 289.34 33.18 0 -2 8 189.43 24.72 0 -2 8 328.17 36.74 0 2 8 396.67 45.14 0 -2 -8 335.88 40.56 0 -2 -9 24.95 12.95 0 2 -9 15.12 5.89 0 2 9 30.48 14.57 0 -2 9 13.64 8.13 0 2 10 71.87 21.44 0 -2 -10 64.08 17.00 0 -2 10 54.74 15.66 0 -2 11 -0.64 6.05 0 2 11 5.13 8.08 0 -2 12 1.74 1.22 0 -2 12 3.28 8.44 0 2 12 -1.77 2.93 0 2 13 27.71 14.17 0 -2 13 19.81 12.34 0 -2 13 9.35 3.47 0 2 14 27.50 14.49 0 -2 14 15.08 4.72 0 -2 14 49.52 18.11 0 2 15 -3.02 11.54 0 -2 15 0.30 0.12 0 -2 15 4.34 6.42 0 2 16 21.37 12.41 0 -2 16 14.47 11.86 0 -2 17 78.31 22.64 0 2 17 60.53 24.58 0 -2 18 13.26 11.32 0 2 18 9.99 8.93 0 2 19 21.90 15.24 0 -2 19 12.66 15.96 0 -2 20 8.87 9.89 0 2 20 -0.59 12.99 0 2 21 6.72 6.94 0 -2 21 7.58 6.60 0 -2 22 -0.79 5.87 0 2 22 32.64 20.73 0 -2 23 2.07 6.05 0 2 23 -11.04 10.45 0 2 24 24.22 20.12 0 -2 24 6.67 5.22 0 2 25 50.01 21.03 0 -2 25 8.38 13.06 0 -2 26 5.69 7.34 0 2 26 -9.71 14.41 0 2 27 13.32 15.80 0 -2 27 0.16 4.83 0 -2 28 8.85 9.55 0 2 28 -0.79 11.55 0 -2 29 7.67 15.61 0 -3 0 -1.49 1.91 0 3 0 -2.31 10.32 0 -3 0 4.65 7.44 0 3 0 -0.40 3.55 0 -3 -1 7.60 8.54 0 3 -1 11.15 5.44 0 3 1 16.52 7.12 0 -3 -1 16.81 8.34 0 3 1 19.19 12.95 0 3 -1 12.78 8.82 0 -3 1 16.41 7.43 0 -3 1 7.72 6.17 0 3 2 16.89 10.47 0 -3 2 12.99 7.49 0 3 -2 10.31 3.86 0 -3 -2 12.56 8.71 0 3 2 16.85 8.38 0 -3 2 12.43 10.78 0 3 -2 18.30 9.46 0 -3 -2 14.87 7.84 0 3 3 27.93 20.20 0 3 3 16.49 9.90 0 3 -3 15.48 12.00 0 -3 3 10.61 8.70 0 -3 -3 15.14 8.30 0 -3 3 21.48 10.40 0 -3 -3 9.59 4.78 0 3 4 114.07 25.70 0 -3 -4 65.58 20.52 0 -3 4 73.45 18.24 0 -3 -4 40.92 8.50 0 3 4 182.45 45.25 0 -3 4 67.56 19.44 0 3 -4 59.71 18.28 0 3 -5 1.38 3.43 0 -3 -5 6.56 6.56 0 -3 5 1.76 5.12 0 -3 5 7.88 8.11 0 3 5 -0.69 9.97 0 -3 6 -2.00 1.31 0 -3 -6 1.68 5.22 0 3 -6 14.39 10.31 0 3 6 13.82 12.26 0 3 7 5.84 1.24 0 -3 7 4.25 5.73 0 3 -7 12.04 8.50 0 -3 8 0.66 4.75 0 3 8 4.59 8.91 0 3 -8 1.59 7.86 0 3 -9 9.64 8.66 0 3 9 -1.62 4.05 0 -3 9 0.95 3.92 0 3 -10 -1.46 4.40 0 3 10 3.46 1.59 0 -3 10 6.24 10.24 0 3 -11 15.14 11.56 0 3 11 13.55 12.01 0 -3 11 9.22 8.30 0 -3 12 6.85 10.72 0 3 12 -6.63 9.56 0 -3 13 -6.46 6.48 0 3 13 15.97 6.58 0 -3 14 46.34 17.74 0 3 14 35.46 19.54 0 -3 15 11.01 9.42 0 3 15 11.44 12.97 0 3 16 -5.27 10.04 0 -3 16 7.47 5.64 0 3 17 8.27 11.78 0 -3 17 0.12 8.67 0 3 18 -2.84 12.47 0 -3 18 0.75 3.67 0 -3 19 -2.30 1.77 0 3 19 6.20 8.29 0 -3 20 13.64 20.22 0 3 20 5.41 10.81 0 3 21 1.44 11.01 0 -3 21 10.72 12.14 0 -3 22 1.41 5.66 0 3 22 -5.02 12.58 0 3 23 -4.47 6.27 0 -3 23 -17.66 13.21 0 -3 24 25.16 17.69 0 3 24 0.53 11.54 0 -3 25 -25.68 16.47 0 3 25 21.69 20.95 0 4 0 11.85 14.75 0 4 1 16.39 20.64 0 4 -1 3.03 1.12 0 4 2 -0.02 11.59 0 4 -2 -5.36 10.87 0 -4 2 0.22 4.87 0 4 3 0.64 9.02 0 -4 3 -0.70 1.36 0 4 -3 3.55 7.04 0 4 4 5.28 14.60 0 4 -4 4.63 3.73 0 -4 4 1.80 2.48 0 4 5 -2.88 10.60 0 4 -5 2.60 6.80 0 -4 5 0.82 5.15 0 4 -6 2.03 5.18 0 -4 6 1.25 7.19 0 4 6 4.09 26.85 0 4 -7 5.31 9.16 0 -4 7 -1.54 4.15 0 4 7 -13.23 1.50 0 4 8 22.31 23.11 0 -4 8 15.19 12.80 0 4 8 12.10 13.52 0 4 -8 -2.50 3.02 0 4 9 4.76 19.25 0 4 -9 5.00 5.14 0 4 9 1.44 9.37 0 -4 9 -10.12 11.65 0 -4 10 0.77 7.82 0 4 -10 1.89 1.73 0 4 10 28.79 25.39 0 -4 11 -3.16 7.27 0 4 -11 4.36 3.33 0 4 11 0.68 9.80 0 4 -12 3.08 6.25 0 -4 12 6.43 7.77 0 4 12 9.96 18.46 0 -4 13 11.49 11.18 0 4 13 12.84 16.01 0 -4 14 8.99 8.09 0 4 14 11.23 12.63 0 4 15 -7.17 16.07 0 -4 15 5.12 12.02 0 4 16 12.90 15.33 0 -4 16 0.30 7.48 0 -4 17 3.70 6.30 0 4 17 10.17 15.80 0 4 18 -18.16 25.81 0 -4 18 5.82 8.23 0 -4 19 9.95 15.58 0 4 19 -8.86 16.85 0 4 20 -8.38 18.53 0 -4 20 11.05 15.18 0 4 21 -38.61 23.18 0 4 22 -4.61 12.83 0 5 0 1.22 14.78 0 5 -1 0.47 10.29 0 5 1 -4.00 8.07 0 5 -2 12.74 18.61 0 5 2 -0.18 21.80 0 5 3 -7.30 15.53 0 5 -3 -4.95 11.18 0 5 4 3.74 16.68 0 5 -4 9.33 14.02 0 5 5 14.28 12.46 0 5 -5 -6.09 1.54 0 5 -6 6.66 13.18 0 5 6 0.02 10.22 0 5 7 15.81 18.22 0 5 -7 6.68 9.57 0 5 8 14.80 4.80 0 5 -8 -4.37 4.79 0 5 -9 9.56 12.43 0 5 9 1.87 20.54 0 5 -10 -1.49 11.54 0 5 10 -11.74 21.01 0 5 -11 0.27 6.36 0 5 11 3.38 34.42 0 -5 12 8.82 10.08 0 -5 13 -0.78 9.31 0 -5 14 4.03 15.93 -1 0 32 -11.14 10.83 -1 0 31 -3.73 7.94 -1 0 30 -2.88 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-1.80 3.89 -20 -2 2 105.73 40.71 20 -2 -2 -2.94 5.49 -20 -2 1 6.16 8.18 20 -2 -1 -4.95 6.32 -20 -2 0 4.51 8.51 20 -2 0 -1.08 3.86 -20 -2 -1 2.80 4.10 20 -2 1 0.82 4.48 -20 -2 -2 -1.04 5.30 20 -2 2 -13.41 12.12 -20 -2 -3 16.62 15.43 20 -2 3 -3.56 5.97 -20 -2 -4 13.24 22.19 20 -2 4 8.14 8.55 -20 -2 -5 0.20 7.72 20 -2 5 10.86 12.72 -20 -2 -6 -4.79 7.75 -20 -2 -7 -8.94 21.61 -20 -2 -8 31.86 25.25 -20 -2 -9 -1.05 12.81 21 0 -10 -5.02 2.98 21 0 -9 20.95 37.24 21 0 -8 132.86 34.86 21 0 -7 35.79 18.83 21 0 -6 -5.73 9.42 21 0 -5 10.05 6.64 21 0 -4 2.51 6.36 21 0 -3 1.91 3.63 21 0 -2 3.62 7.86 21 0 -1 2.70 3.48 21 0 0 -1.06 7.01 21 0 1 20.80 15.46 21 0 2 -10.46 10.93 21 0 3 -1.48 5.22 21 0 4 -3.31 1.52 21 0 5 -11.23 10.16 21 0 6 -0.07 7.67 21 0 7 -3.40 6.93 21 0 8 -4.71 7.12 21 0 9 2.24 3.42 21 0 10 4.16 7.41 21 0 11 25.27 14.33 21 1 -11 -3.14 4.72 21 1 -10 10.24 11.62 21 1 -9 12.63 15.08 21 1 -8 1.95 5.28 21 -1 -7 10.16 17.28 21 1 -7 3.53 2.95 21 -1 -6 -7.97 10.43 21 1 -6 -3.65 5.40 21 -1 -5 -2.76 9.69 21 1 -5 3.31 11.21 21 -1 -4 -6.06 5.61 21 1 -4 -7.43 6.07 21 -1 -3 16.03 12.97 21 1 -3 6.67 8.16 21 -1 -2 3.02 4.05 21 1 -2 8.31 10.57 21 -1 -1 -5.60 6.60 21 1 -1 -5.51 7.33 21 -1 0 23.18 14.19 21 1 0 -12.34 10.48 21 -1 1 -1.95 2.56 21 1 1 7.03 11.57 21 -1 2 8.14 7.78 21 1 2 4.50 8.30 21 -1 3 0.96 1.89 21 1 3 7.10 2.66 21 -1 4 -1.80 8.80 21 1 4 2.37 6.77 21 1 5 -4.13 2.93 21 -1 5 -10.30 13.00 21 1 6 4.69 3.33 21 -1 6 11.80 10.07 21 1 7 8.21 14.95 21 -1 7 6.58 9.01 21 1 8 -0.69 6.98 21 1 9 6.86 10.73 21 1 10 -1.19 4.14 21 1 11 -3.47 7.53 21 1 12 16.41 11.43 21 1 13 -3.37 8.09 22 0 -5 18.62 16.48 22 0 -4 23.79 18.66 22 0 -3 9.26 11.49 22 0 -2 -7.49 7.82 22 0 -1 -11.31 11.88 22 0 0 8.22 8.80 22 0 1 -0.34 6.53 22 0 2 -1.54 9.53 22 0 3 -1.81 8.18 22 0 4 12.79 12.00 22 0 5 10.04 10.50 22 0 6 -1.03 6.07 22 1 -7 -0.02 4.17 22 1 -6 21.68 16.17 22 1 -5 9.20 9.53 22 1 -4 -7.30 12.25 22 1 -3 9.32 9.58 22 1 -2 -1.74 7.21 22 1 -1 -7.97 9.54 22 1 0 8.68 9.63 22 1 1 2.21 7.96 22 1 2 7.91 6.15 22 1 3 -12.35 13.48 22 1 4 0.73 4.29 22 1 5 4.74 8.03 22 1 6 4.49 1.98 22 1 7 3.48 2.78 22 1 8 -6.62 5.65 22 1 9 0.32 6.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78622 _shelx_res_file ; TITL is226_a.res in P2(1)/n IS226.res created by SHELXL-2016/6 at 15:45:47 on 16-Oct-2019 CELL 0.71073 15.6109 3.8414 21.9738 90 90.739 90 ZERR 4 0.0045 0.0009 0.0069 0 0.025 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 68 40 8 12 L.S. 4 0 0 PLAN 20 BOND $H list 4 fmap 2 53 acta OMIT 0 50 conf size 0.3 0.05 0.04 temp 20 WGHT 0.025500 FVAR 0.60103 O1 4 0.357247 0.570915 0.693524 11.00000 0.06070 0.07644 = 0.04517 -0.00899 0.00523 0.00580 O2 4 0.490151 0.731178 0.710816 11.00000 0.07076 0.09785 = 0.05224 -0.01863 -0.00818 -0.00096 O3 4 0.616183 0.552419 0.632310 11.00000 0.05240 0.05976 = 0.04449 -0.00360 -0.00604 -0.00090 N1 3 0.578492 0.257563 0.550233 11.00000 0.05427 0.07218 = 0.05300 -0.00991 -0.00056 -0.00132 N2 3 0.667432 0.303169 0.550503 11.00000 0.05427 0.07044 = 0.05776 -0.01095 -0.00254 0.00151 C1 1 0.293073 0.429708 0.657013 11.00000 0.05951 0.04839 = 0.04477 0.00180 -0.00287 0.00570 C2 1 0.211709 0.435261 0.679855 11.00000 0.05742 0.06519 = 0.04632 0.00622 0.01011 0.00921 H2 2 0.199868 0.514728 0.722368 11.00000 0.06563 C3 1 0.146274 0.296224 0.643917 11.00000 0.06134 0.06169 = 0.06843 0.00363 0.01119 0.00359 H3 2 0.090733 0.297440 0.662050 11.00000 0.06564 C4 1 0.163439 0.161384 0.587235 11.00000 0.05480 0.06351 = 0.06168 -0.00607 -0.00298 -0.00597 H4 2 0.114385 0.060618 0.560000 11.00000 0.05538 C5 1 0.245016 0.156297 0.565144 11.00000 0.05931 0.06005 = 0.04930 0.00117 -0.00020 -0.00512 H5 2 0.253939 0.076490 0.525898 11.00000 0.06440 C6 1 0.312938 0.290739 0.600695 11.00000 0.05223 0.04636 = 0.04385 0.00529 -0.00061 0.00448 C7 1 0.399901 0.291540 0.582761 11.00000 0.05641 0.04820 = 0.04219 0.00212 0.00374 0.00021 H7 2 0.414436 0.205504 0.542279 11.00000 0.05824 C8 1 0.462616 0.426880 0.618633 11.00000 0.05143 0.04746 = 0.04030 0.00395 0.00138 -0.00026 C9 1 0.440777 0.584457 0.676275 11.00000 0.06523 0.06030 = 0.04048 0.00010 -0.00504 0.00563 C10 1 0.549817 0.409772 0.598750 11.00000 0.05241 0.04877 = 0.04074 0.00015 -0.00380 -0.00189 C11 1 0.686383 0.477418 0.598574 11.00000 0.05228 0.04804 = 0.04814 -0.00237 -0.00023 -0.00132 C12 1 0.770707 0.581760 0.621245 11.00000 0.05361 0.04482 = 0.06191 0.00194 -0.00426 -0.00149 C13 1 0.841499 0.526371 0.584945 11.00000 0.06514 0.06705 = 0.05648 -0.00132 0.00260 0.00027 H13 2 0.839050 0.437148 0.545218 11.00000 0.05190 C14 1 0.922738 0.609819 0.606355 11.00000 0.06042 0.07101 = 0.08097 0.00464 0.00267 0.00204 H14 2 0.966957 0.580989 0.575110 11.00000 0.10310 C15 1 0.931598 0.752434 0.663448 11.00000 0.05838 0.06443 = 0.08968 -0.00323 -0.01964 -0.00925 H15 2 0.987282 0.799318 0.676059 11.00000 0.06934 C16 1 0.863453 0.813088 0.699431 11.00000 0.06344 0.06919 = 0.06769 -0.00520 -0.00846 -0.00507 H16 2 0.869309 0.906560 0.743114 11.00000 0.10409 C17 1 0.781784 0.733260 0.677804 11.00000 0.06135 0.06365 = 0.06082 -0.00545 -0.00175 0.00079 H17 2 0.737584 0.768861 0.702199 11.00000 0.04994 HKLF 4 REM is226_a.res in P2(1)/n REM R1 = 0.0667 for 1081 Fo > 4sig(Fo) and 0.1488 for all 2322 data REM 239 parameters refined using 0 restraints END WGHT 0.0255 0.0000 REM Highest difference peak 0.175, deepest hole -0.238, 1-sigma level 0.053 Q1 1 0.5005 0.4484 0.7192 11.00000 0.05 0.18 Q2 1 0.4334 0.5474 0.7570 11.00000 0.05 0.17 Q3 1 0.2421 0.0371 0.4609 11.00000 0.05 0.17 Q4 1 0.2439 0.4154 0.7855 11.00000 0.05 0.17 Q5 1 0.3764 0.2996 0.7017 11.00000 0.05 0.16 Q6 1 0.6758 0.1277 0.4977 11.00000 0.05 0.16 Q7 1 0.2588 -0.1775 0.4871 11.00000 0.05 0.16 Q8 1 0.3626 0.8851 0.6851 11.00000 0.05 0.16 Q9 1 0.4814 0.2413 0.4841 11.00000 0.05 0.16 Q10 1 0.6725 0.2171 0.4810 11.00000 0.05 0.16 Q11 1 0.5000 0.5000 0.5000 10.50000 0.05 0.15 Q12 1 0.7720 0.8016 0.7572 11.00000 0.05 0.15 Q13 1 0.4058 0.5616 0.5802 11.00000 0.05 0.15 Q14 1 0.4472 0.8675 0.7624 11.00000 0.05 0.15 Q15 1 0.2348 0.4299 0.5321 11.00000 0.05 0.14 Q16 1 0.5009 -0.0645 0.5613 11.00000 0.05 0.14 Q17 1 0.7274 0.5737 0.7056 11.00000 0.05 0.14 Q18 1 0.2477 -0.2388 0.5017 11.00000 0.05 0.14 Q19 1 0.3202 0.4653 0.5213 11.00000 0.05 0.14 Q20 1 0.9352 0.7888 0.7714 11.00000 0.05 0.14 ; _shelx_res_checksum 9715 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 0.3572(2) 0.5709(6) 0.69352(11) 0.0607(8) Uani d 1 O O2 0.4902(2) 0.7312(7) 0.71082(12) 0.0737(9) Uani d 1 O O3 0.61618(18) 0.5524(6) 0.63231(11) 0.0523(7) Uani d 1 N N1 0.5785(2) 0.2576(8) 0.55023(14) 0.0598(9) Uani d 1 N N2 0.6674(2) 0.3032(8) 0.55050(15) 0.0608(9) Uani d 1 C C1 0.2931(3) 0.4297(8) 0.65701(17) 0.0509(10) Uani d 1 C C2 0.2117(3) 0.4353(10) 0.6799(2) 0.0562(11) Uani d 1 H H2 0.200(2) 0.515(8) 0.7224(17) 0.066(11) Uiso d 1 C C3 0.1463(3) 0.2962(10) 0.6439(2) 0.0637(12) Uani d 1 H H3 0.091(3) 0.297(8) 0.6621(16) 0.066(12) Uiso d 1 C C4 0.1634(3) 0.1614(10) 0.5872(2) 0.0600(11) Uani d 1 H H4 0.114(2) 0.061(8) 0.5600(16) 0.055(10) Uiso d 1 C C5 0.2450(3) 0.1563(10) 0.5651(2) 0.0562(11) Uani d 1 H H5 0.254(3) 0.076(8) 0.5259(17) 0.064(12) Uiso d 1 C C6 0.3129(3) 0.2907(8) 0.60069(16) 0.0475(10) Uani d 1 C C7 0.3999(3) 0.2915(9) 0.58276(18) 0.0489(10) Uani d 1 H H7 0.414(2) 0.206(8) 0.5423(16) 0.058(10) Uiso d 1 C C8 0.4626(3) 0.4269(8) 0.61863(16) 0.0464(9) Uani d 1 C C9 0.4408(3) 0.5845(9) 0.67627(18) 0.0554(11) Uani d 1 C C10 0.5498(3) 0.4098(8) 0.59875(17) 0.0473(10) Uani d 1 C C11 0.6864(3) 0.4774(8) 0.59857(18) 0.0495(10) Uani d 1 C C12 0.7707(3) 0.5818(8) 0.62124(19) 0.0535(10) Uani d 1 C C13 0.8415(3) 0.5264(10) 0.5849(2) 0.0629(12) Uani d 1 H H13 0.839(2) 0.437(8) 0.5452(16) 0.052(11) Uiso d 1 C C14 0.9227(3) 0.6098(11) 0.6064(3) 0.0708(13) Uani d 1 H H14 0.967(3) 0.581(10) 0.575(2) 0.103(17) Uiso d 1 C C15 0.9316(4) 0.7524(11) 0.6634(3) 0.0710(14) Uani d 1 H H15 0.987(3) 0.799(9) 0.6761(18) 0.069(13) Uiso d 1 C C16 0.8635(3) 0.8131(10) 0.6994(2) 0.0669(12) Uani d 1 H H16 0.869(3) 0.907(10) 0.743(2) 0.104(16) Uiso d 1 C C17 0.7818(3) 0.7333(10) 0.6778(2) 0.0620(12) Uani d 1 H H17 0.738(2) 0.769(8) 0.7022(15) 0.050(11) 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 0.061(2) 0.0764(17) 0.0452(16) 0.0058(14) 0.0052(15) -0.0090(13) O2 0.071(2) 0.098(2) 0.0522(17) -0.0010(16) -0.0082(17) -0.0186(16) O3 0.0524(19) 0.0598(15) 0.0445(15) -0.0009(12) -0.0060(14) -0.0036(12) N1 0.054(2) 0.072(2) 0.053(2) -0.0013(17) -0.0006(19) -0.0099(17) N2 0.054(3) 0.070(2) 0.058(2) 0.0015(17) -0.003(2) -0.0109(18) C1 0.060(3) 0.048(2) 0.045(2) 0.0057(19) -0.003(2) 0.0018(18) C2 0.057(3) 0.065(2) 0.046(2) 0.009(2) 0.010(2) 0.006(2) C3 0.061(3) 0.062(2) 0.068(3) 0.004(2) 0.011(3) 0.004(2) C4 0.055(3) 0.064(2) 0.062(3) -0.006(2) -0.003(3) -0.006(2) C5 0.059(3) 0.060(2) 0.049(3) -0.005(2) 0.000(2) 0.001(2) C6 0.052(3) 0.046(2) 0.044(2) 0.0045(17) -0.001(2) 0.0053(18) C7 0.056(3) 0.048(2) 0.042(2) 0.0002(18) 0.004(2) 0.0021(19) C8 0.051(3) 0.047(2) 0.040(2) -0.0003(17) 0.001(2) 0.0040(17) C9 0.065(3) 0.060(2) 0.040(2) 0.006(2) -0.005(2) 0.000(2) C10 0.052(3) 0.049(2) 0.041(2) -0.0019(17) -0.004(2) 0.0001(18) C11 0.052(3) 0.048(2) 0.048(2) -0.0013(18) 0.000(2) -0.0024(19) C12 0.054(3) 0.045(2) 0.062(3) -0.0015(17) -0.004(2) 0.0019(19) C13 0.065(3) 0.067(3) 0.056(3) 0.000(2) 0.003(3) -0.001(2) C14 0.060(4) 0.071(3) 0.081(4) 0.002(2) 0.003(3) 0.005(3) C15 0.058(4) 0.064(3) 0.090(4) -0.009(2) -0.020(3) -0.003(3) C16 0.063(4) 0.069(3) 0.068(3) -0.005(2) -0.008(3) -0.005(2) C17 0.061(3) 0.064(3) 0.061(3) 0.001(2) -0.002(3) -0.005(2) 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 C9 O1 C1 122.7(3) C11 O3 C10 103.3(3) C10 N1 N2 107.0(3) C11 N2 N1 106.7(3) C2 C1 O1 116.6(4) C2 C1 C6 123.5(4) O1 C1 C6 119.9(4) C1 C2 C3 117.6(4) C1 C2 H2 122(2) C3 C2 H2 120(2) C4 C3 C2 120.5(5) C4 C3 H3 124(2) C2 C3 H3 115(2) C5 C4 C3 121.2(5) C5 C4 H4 118.2(19) C3 C4 H4 121(2) C4 C5 C6 119.7(4) C4 C5 H5 119(3) C6 C5 H5 121(3) C1 C6 C5 117.5(4) C1 C6 C7 118.2(4) C5 C6 C7 124.3(4) C8 C7 C6 121.8(4) C8 C7 H7 119(2) C6 C7 H7 119(2) C7 C8 C10 119.1(3) C7 C8 C9 119.6(4) C10 C8 C9 121.3(4) O2 C9 O1 116.5(4) O2 C9 C8 125.9(4) O1 C9 C8 117.6(4) N1 C10 O3 110.7(4) N1 C10 C8 127.4(4) O3 C10 C8 121.9(3) N2 C11 O3 112.3(4) N2 C11 C12 128.5(4) O3 C11 C12 119.0(3) C17 C12 C13 119.4(4) C17 C12 C11 121.7(4) C13 C12 C11 118.9(4) C14 C13 C12 120.1(5) C14 C13 H13 115(2) C12 C13 H13 125(2) C15 C14 C13 118.9(5) C15 C14 H14 128(3) C13 C14 H14 113(3) C16 C15 C14 122.1(5) C16 C15 H15 122(3) C14 C15 H15 116(3) C15 C16 C17 119.1(5) C15 C16 H16 123(3) C17 C16 H16 118(3) C12 C17 C16 120.3(5) C12 C17 H17 121(2) C16 C17 H17 118(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C9 1.364(5) O1 C1 1.386(5) O2 C9 1.214(5) O3 C11 1.362(4) O3 C10 1.378(4) N1 C10 1.300(4) N1 N2 1.399(4) N2 C11 1.282(4) C1 C2 1.372(6) C1 C6 1.387(5) C2 C3 1.390(6) C2 H2 1.00(3) C3 C4 1.378(6) C3 H3 0.96(4) C4 C5 1.369(6) C4 H4 1.04(4) C5 C6 1.407(5) C5 H5 0.93(3) C6 C7 1.418(5) C7 C8 1.353(5) C7 H7 0.98(3) C8 C10 1.437(5) C8 C9 1.448(5) C11 C12 1.458(5) C12 C17 1.381(5) C12 C13 1.388(6) C13 C14 1.385(6) C13 H13 0.94(3) C14 C15 1.374(7) C14 H14 0.99(5) C15 C16 1.354(6) C15 H15 0.93(4) C16 C17 1.389(6) C16 H16 1.03(4) C17 H17 0.89(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C10 N1 N2 C11 0.1(4) C9 O1 C1 C2 -179.5(3) C9 O1 C1 C6 0.8(5) O1 C1 C2 C3 179.8(3) C6 C1 C2 C3 -0.6(6) C1 C2 C3 C4 -0.6(6) C2 C3 C4 C5 0.9(6) C3 C4 C5 C6 0.0(6) C2 C1 C6 C5 1.4(5) O1 C1 C6 C5 -179.0(3) C2 C1 C6 C7 -178.3(3) O1 C1 C6 C7 1.3(5) C4 C5 C6 C1 -1.1(5) C4 C5 C6 C7 178.6(3) C1 C6 C7 C8 -0.8(5) C5 C6 C7 C8 179.5(3) C6 C7 C8 C10 178.0(3) C6 C7 C8 C9 -1.7(5) C1 O1 C9 O2 176.2(3) C1 O1 C9 C8 -3.3(5) C7 C8 C9 O2 -175.7(4) C10 C8 C9 O2 4.6(6) C7 C8 C9 O1 3.7(5) C10 C8 C9 O1 -176.0(3) N2 N1 C10 O3 -0.9(4) N2 N1 C10 C8 -178.8(3) C11 O3 C10 N1 1.3(4) C11 O3 C10 C8 179.3(3) C7 C8 C10 N1 -4.3(6) C9 C8 C10 N1 175.4(3) C7 C8 C10 O3 177.9(3) C9 C8 C10 O3 -2.3(5) N1 N2 C11 O3 0.8(4) N1 N2 C11 C12 177.4(3) C10 O3 C11 N2 -1.3(4) C10 O3 C11 C12 -178.2(3) N2 C11 C12 C17 -172.0(4) O3 C11 C12 C17 4.4(5) N2 C11 C12 C13 7.9(6) O3 C11 C12 C13 -175.7(3) C17 C12 C13 C14 2.5(6) C11 C12 C13 C14 -177.3(4) C12 C13 C14 C15 -1.0(6) C13 C14 C15 C16 0.2(7) C14 C15 C16 C17 -0.9(7) C13 C12 C17 C16 -3.3(6) C11 C12 C17 C16 176.6(4) C15 C16 C17 C12 2.4(6) _cod_database_fobs_code 2021802