#------------------------------------------------------------------------------ #$Date: 2021-08-07 07:31:41 +0300 (Sat, 07 Aug 2021) $ #$Revision: 267991 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243888.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_2243888 loop_ _publ_author_name 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Askerova, Ulviyya F.' 'Mukhtarova, Sevinc H.' 'Askerov, Rizvan K.' 'Mlowe, Sixberth' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (3Z)-7-methoxy-3-(2-phenylhydrazinylidene)-1-benzofuran-2(3H)-one ; _journal_coeditor_code WM5614 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021007891 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C15 H12 N2 O3' _chemical_formula_moiety 'C15 H12 N2 O3' _chemical_formula_sum 'C15 H12 N2 O3' _chemical_formula_weight 268.27 _chemical_name_systematic ; (3Z)-7-Methoxy-3-(2-phenylhydrazinylidene)-1-benzofuran-2(3H)-one ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90 _cell_angle_beta 99.181(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.436(2) _cell_length_b 7.2485(7) _cell_length_c 20.595(2) _cell_measurement_reflns_used 2240 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.29 _cell_measurement_theta_min 2.37 _cell_volume 2569.6(5) _computing_cell_refinement ; SAINT (Bruker, 2017) ; _computing_data_collection ; APEX3 (Bruker, 2017) ; _computing_data_reduction ; SAINT (Bruker, 2017) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_unetI/netI 0.0610 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 12800 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.986 _diffrn_reflns_theta_min 2.003 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.387 _exptl_crystal_description prism _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.491 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.059 _refine_diff_density_max 0.182 _refine_diff_density_min -0.179 _refine_ls_extinction_coef 0.0015(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2016/6 (Sheldrick 2015) ; _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 2427 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.1274 _refine_ls_R_factor_gt 0.0733 _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^)+(0.0517P)^2^+2.9831P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1347 _refine_ls_wR_factor_ref 0.1515 _reflns_number_gt 1463 _reflns_number_total 2427 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5614sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2243888 _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 0.953 _shelx_estimated_absorpt_t_max 0.994 _shelx_hkl_file ; 2 0 0 634.04 18.20 2 0 0 632.44 18.80 -2 0 0 633.34 17.60 -2 0 0 613.04 18.80 -2 0 0 621.64 18.10 -4 0 0 1171.58 34.80 -4 0 0 1156.78 36.40 4 0 0 1240.18 35.00 4 0 0 1217.58 33.70 4 0 0 1214.38 36.20 -6 0 0 234.58 12.10 -6 0 0 237.18 9.20 6 0 0 239.58 7.60 6 0 0 256.97 9.50 6 0 0 237.08 7.80 6 0 0 248.08 11.20 8 0 0 2.00 1.30 -8 0 0 4.10 5.60 8 0 0 0.50 0.90 8 0 0 5.30 2.60 10 0 0 6.30 1.70 -10 0 0 17.40 7.70 10 0 0 5.40 1.20 10 0 0 4.10 2.80 12 0 0 96.69 7.40 -12 0 0 95.29 13.90 12 0 0 102.09 4.50 -14 0 0 23.00 10.70 14 0 0 20.80 5.40 16 0 0 28.30 6.10 -16 0 0 47.70 12.30 -18 0 0 -0.40 10.00 18 0 0 18.20 6.10 -20 0 0 6.60 11.50 20 0 0 10.90 5.30 1 -1 0 99.49 3.50 1 -1 0 96.39 3.60 -1 -1 0 95.39 3.60 -1 -1 0 101.89 4.00 1 -1 0 97.49 3.90 -1 -1 0 97.69 3.80 -1 1 0 97.49 3.60 1 1 0 100.69 3.70 1 1 0 102.89 3.80 1 1 0 99.59 3.80 -1 1 0 97.69 3.80 -1 1 0 100.49 3.70 -3 -1 0 1461.75 44.40 -3 -1 0 1506.45 43.20 3 -1 0 1539.15 43.90 -3 -1 0 1547.55 42.70 3 -1 0 1547.45 43.40 -3 1 0 1457.75 43.20 -3 1 0 1473.35 44.10 -3 1 0 1552.04 42.70 3 1 0 1530.75 42.70 3 1 0 1533.95 43.20 -5 -1 0 4.30 1.20 5 -1 0 10.80 2.60 -5 -1 0 4.80 2.00 5 -1 0 3.60 1.40 -5 -1 0 8.80 4.90 5 1 0 4.70 4.10 -5 1 0 0.80 1.80 5 1 0 4.30 2.20 5 1 0 5.50 1.40 -5 1 0 10.70 4.70 -5 1 0 3.70 1.50 -7 -1 0 12.30 1.70 7 -1 0 10.30 1.70 -7 -1 0 8.00 5.10 7 -1 0 5.80 2.70 -7 -1 0 12.50 3.20 -7 1 0 11.20 2.10 7 1 0 11.90 1.80 -7 1 0 14.70 5.80 7 1 0 13.80 3.00 -9 -1 0 2.20 1.00 -9 -1 0 2.80 6.50 9 -1 0 1.90 1.40 9 -1 0 -0.50 2.20 9 1 0 -0.40 1.20 9 1 0 1.40 2.50 -9 1 0 -1.10 6.00 -11 -1 0 24.50 9.30 11 -1 0 16.50 4.40 11 -1 0 17.90 2.40 11 -1 0 19.50 2.90 11 1 0 16.20 4.40 11 1 0 21.50 2.50 -11 1 0 24.80 9.30 13 -1 0 4.30 1.50 13 -1 0 1.90 3.40 -13 -1 0 10.50 9.90 -13 1 0 14.60 10.70 13 1 0 7.80 4.10 13 1 0 4.60 1.80 -15 -1 0 4.30 10.00 15 -1 0 -0.40 4.00 15 1 0 3.40 3.30 -15 1 0 0.90 10.60 17 -1 0 12.70 5.10 -17 -1 0 7.60 9.70 17 1 0 10.70 4.70 -17 1 0 14.00 11.90 19 -1 0 -1.80 3.40 -19 -1 0 3.10 9.90 -19 1 0 5.30 11.00 19 1 0 -2.70 3.60 21 -1 0 -2.90 4.20 -21 -1 0 3.50 10.50 -21 1 0 5.50 11.50 21 1 0 -0.80 3.70 0 -2 0 1129.59 32.00 0 -2 0 1010.90 32.40 0 2 0 1124.19 31.80 -2 -2 0 2743.83 73.59 2 -2 0 2652.93 72.69 2 -2 0 2476.35 71.69 2 -2 0 2485.45 72.59 -2 -2 0 2412.46 72.29 2 2 0 2586.04 72.29 2 2 0 2548.74 72.39 2 2 0 2494.85 71.99 -2 2 0 2592.74 72.69 -2 2 0 2606.74 72.19 4 -2 0 57.39 4.30 -4 -2 0 70.99 6.90 -4 -2 0 55.39 4.00 4 -2 0 60.49 4.40 -4 -2 0 47.90 3.60 4 -2 0 52.49 5.10 4 2 0 58.99 4.20 -4 2 0 50.79 4.10 -4 2 0 66.79 6.10 4 2 0 62.89 3.70 4 2 0 58.19 4.90 -4 2 0 57.49 3.70 6 -2 0 33.70 3.60 -6 -2 0 53.79 7.60 6 -2 0 41.90 4.80 6 -2 0 44.20 4.30 -6 -2 0 46.50 2.90 6 2 0 45.70 3.30 -6 2 0 46.20 6.80 -6 2 0 46.00 3.30 6 2 0 38.90 5.20 6 2 0 44.10 4.00 -8 -2 0 114.49 5.20 8 -2 0 127.29 7.20 8 -2 0 118.39 5.40 8 2 0 123.89 5.60 -8 2 0 119.89 10.60 -8 2 0 123.79 5.70 8 2 0 128.09 6.90 -10 -2 0 71.49 11.80 10 -2 0 50.69 6.20 10 -2 0 43.80 3.50 -10 -2 0 42.50 3.10 -10 2 0 54.49 3.90 10 2 0 49.50 3.60 -10 2 0 52.79 10.40 10 2 0 47.40 5.30 12 -2 0 20.20 3.00 -12 -2 0 30.00 10.70 12 -2 0 17.80 5.00 -12 -2 0 19.50 2.70 12 2 0 21.30 5.10 -12 2 0 16.00 3.20 12 2 0 20.80 3.10 -12 2 0 26.60 10.20 14 -2 0 98.89 5.40 14 -2 0 107.09 8.80 14 -2 0 103.49 5.50 -14 -2 0 121.89 6.90 -14 -2 0 112.49 16.00 14 2 0 104.79 5.50 14 2 0 102.99 8.30 -14 2 0 114.99 16.60 -16 -2 0 8.20 11.00 16 -2 0 15.90 4.80 16 -2 0 9.40 2.10 16 -2 0 6.10 2.30 -16 2 0 2.00 10.30 16 2 0 14.60 4.70 16 2 0 12.50 2.50 -18 -2 0 6.80 11.60 18 -2 0 3.10 4.20 -18 2 0 5.50 11.20 18 2 0 8.30 4.40 -20 -2 0 -18.40 10.80 20 -2 0 0.70 3.80 20 2 0 -3.00 3.90 -20 2 0 2.60 11.10 1 -3 0 153.28 7.30 -1 -3 0 146.19 7.00 1 3 0 144.29 6.70 -1 3 0 143.09 6.70 -3 -3 0 20.20 3.60 -3 -3 0 18.80 4.00 3 -3 0 16.50 3.50 3 3 0 14.10 2.70 -3 3 0 17.10 2.90 3 3 0 16.60 2.90 -5 -3 0 11.30 5.20 5 -3 0 3.80 3.00 5 -3 0 4.10 2.70 5 3 0 7.80 3.50 -5 3 0 3.50 2.20 5 3 0 3.40 2.20 5 3 0 4.20 3.10 -5 3 0 6.80 5.00 -7 -3 0 78.39 9.50 7 -3 0 68.99 5.70 -7 3 0 76.19 4.80 7 3 0 79.99 5.80 -7 3 0 68.59 8.90 7 3 0 75.19 5.00 -9 -3 0 49.80 10.20 9 -3 0 48.90 6.50 -9 3 0 42.60 4.70 9 3 0 36.80 4.30 9 3 0 50.39 6.10 -9 3 0 50.29 10.40 -11 -3 0 62.19 12.90 11 -3 0 55.59 7.40 -11 3 0 59.39 12.00 11 3 0 53.49 4.90 11 3 0 55.09 5.90 -11 3 0 52.09 5.20 13 -3 0 5.80 4.30 -13 -3 0 14.00 10.90 -13 3 0 9.00 10.00 13 3 0 10.90 4.70 13 3 0 6.50 2.80 -13 3 0 6.70 2.70 -15 -3 0 9.30 11.70 15 -3 0 14.90 5.80 15 3 0 7.40 2.70 15 3 0 5.40 4.10 -15 3 0 5.00 9.70 17 -3 0 1.50 1.80 17 -3 0 -0.10 3.90 -17 -3 0 5.60 11.80 17 3 0 -1.40 3.70 17 3 0 2.50 2.30 -17 3 0 -1.90 10.70 -19 -3 0 1.30 12.20 19 -3 0 0.60 5.00 -19 3 0 -0.50 11.10 19 3 0 2.50 3.70 0 -4 0 149.39 8.00 0 4 0 148.69 7.70 -2 -4 0 8.70 3.40 2 -4 0 3.00 3.10 -2 4 0 1.90 2.30 2 4 0 0.90 2.40 -4 -4 0 58.59 5.70 4 -4 0 59.79 5.80 4 4 0 64.69 5.30 -4 4 0 55.19 4.90 6 -4 0 63.29 6.30 -6 -4 0 60.99 8.40 6 -4 0 76.89 5.10 -6 4 0 66.99 8.50 -6 4 0 55.99 5.00 6 4 0 64.89 5.90 6 4 0 64.89 5.50 6 4 0 57.29 5.70 8 -4 0 49.30 7.10 -8 -4 0 47.70 10.80 8 4 0 50.59 5.90 8 4 0 43.30 5.00 -8 4 0 41.00 9.00 -8 4 0 48.00 5.40 10 -4 0 70.29 7.40 -10 -4 0 96.89 14.30 10 4 0 56.29 6.60 10 4 0 73.19 5.90 -10 4 0 87.49 12.60 -10 4 0 71.19 5.80 -12 -4 0 14.90 10.50 12 -4 0 34.10 6.50 12 4 0 33.40 4.90 12 4 0 30.70 6.20 -12 4 0 36.00 5.10 -12 4 0 25.30 10.70 -14 -4 0 11.20 10.80 -14 4 0 2.70 9.60 14 4 0 -5.70 3.10 -14 4 0 2.40 2.80 14 4 0 0.50 2.70 16 -4 0 11.60 5.40 -16 -4 0 8.70 12.80 16 4 0 19.00 3.80 -16 4 0 14.20 3.30 16 4 0 12.40 5.30 -18 -4 0 -3.20 10.70 18 -4 0 -1.20 2.10 18 -4 0 4.60 4.30 18 4 0 4.50 4.30 -18 4 0 3.40 10.80 18 4 0 -3.20 2.30 1 -5 0 2.00 4.40 -1 -5 0 2.20 4.40 -1 5 0 -2.20 2.90 1 5 0 3.80 3.10 3 -5 0 -3.10 3.90 -3 -5 0 3.50 4.30 -3 5 0 3.00 3.20 3 5 0 -1.10 2.70 -5 -5 0 2.20 4.50 5 -5 0 2.40 4.10 5 5 0 6.70 3.80 -5 5 0 -1.10 3.20 -7 -5 0 64.89 7.70 -7 -5 0 44.60 8.40 7 -5 0 62.09 8.10 -7 5 0 54.29 5.70 7 5 0 50.69 6.10 -7 5 0 45.20 8.00 -9 -5 0 0.40 8.00 9 -5 0 10.90 5.30 9 5 0 1.50 3.80 -9 5 0 2.10 8.00 9 5 0 8.60 4.10 -9 5 0 3.90 3.50 -11 -5 0 -1.40 8.80 11 -5 0 -2.20 3.70 -11 5 0 1.50 2.90 11 5 0 -3.10 2.70 -11 5 0 -4.40 8.20 11 5 0 -1.40 4.10 -13 -5 0 9.90 11.50 13 -5 0 18.00 5.60 -13 5 0 18.60 4.30 -13 5 0 9.80 10.00 13 5 0 22.60 4.50 13 5 0 23.90 6.20 -15 -5 0 -2.60 12.20 15 -5 0 7.00 4.80 15 5 0 0.50 3.20 -15 5 0 -9.70 9.20 -15 5 0 4.60 2.80 15 5 0 -0.90 4.20 -17 -5 0 16.50 14.20 17 -5 0 5.30 5.50 -17 5 0 0.20 10.50 17 5 0 11.20 5.80 -17 5 0 9.40 3.50 17 5 0 6.10 3.60 0 -6 0 -1.40 4.80 0 6 0 3.30 3.70 -2 -6 0 7.20 5.40 2 -6 0 6.20 4.90 -2 6 0 10.50 4.10 2 6 0 5.40 4.60 -4 -6 0 -2.50 4.80 4 -6 0 -3.20 4.40 4 6 0 2.00 4.00 -4 6 0 0.50 3.10 6 -6 0 0.00 4.80 -6 -6 0 4.40 5.10 -6 6 0 5.20 3.50 6 6 0 0.30 3.70 -8 -6 0 17.10 5.00 8 -6 0 2.90 4.80 -8 -6 0 7.30 4.80 -8 6 0 -4.70 2.90 8 6 0 -0.20 3.40 10 -6 0 29.30 7.00 -10 -6 0 41.80 8.90 -10 -6 0 23.70 6.30 -10 6 0 36.60 5.90 -10 6 0 30.10 7.40 10 6 0 30.10 5.50 -12 -6 0 39.40 10.80 12 -6 0 22.60 6.60 -12 6 0 18.10 4.70 12 6 0 16.50 5.60 -12 6 0 16.60 8.00 12 6 0 18.20 4.80 14 -6 0 5.80 5.50 -14 -6 0 32.90 11.70 14 6 0 4.30 5.00 -14 6 0 1.30 7.60 14 6 0 3.30 3.60 -14 6 0 4.50 3.80 16 -6 0 4.30 5.40 -16 -6 0 32.70 13.60 16 6 0 3.80 5.10 -16 6 0 11.10 9.60 -16 6 0 9.70 6.60 16 6 0 8.60 5.10 1 -7 0 -2.20 4.40 -1 -7 0 5.70 6.20 1 7 0 -0.50 3.60 -1 7 0 5.20 3.70 -3 -7 0 11.50 6.00 3 -7 0 10.30 5.90 3 7 0 3.10 3.70 -3 7 0 1.90 3.30 5 -7 0 -7.10 4.50 -5 -7 0 4.70 5.40 -5 7 0 0.30 3.40 5 7 0 3.30 4.00 7 -7 0 3.90 4.80 -7 -7 0 -1.70 4.90 7 7 0 4.60 4.20 -7 7 0 -2.50 3.50 9 -7 0 -2.70 4.40 -9 -7 0 5.60 5.30 9 7 0 4.20 3.90 -9 7 0 4.40 3.80 -13 7 0 62.49 7.90 0 -8 0 4.00 5.20 0 8 0 11.40 4.20 2 -8 0 3.40 4.90 -2 -8 0 0.40 5.10 -2 8 0 4.70 4.20 2 8 0 5.80 3.90 4 -8 0 -0.70 4.70 -4 -8 0 3.30 5.60 4 8 0 5.10 4.20 -4 8 0 3.70 4.10 6 -8 0 -2.40 4.40 -6 -8 0 -5.80 4.70 6 8 0 -0.40 4.60 -6 8 0 -0.40 3.60 8 -8 0 11.80 6.20 -8 -8 0 2.60 5.90 8 8 0 9.20 4.80 -8 8 0 9.40 4.80 10 -8 0 2.90 5.80 -10 -8 0 4.40 6.20 -10 8 0 8.50 4.60 10 8 0 7.30 4.90 -1 -9 0 1.10 5.50 1 -9 0 4.10 5.50 1 9 0 4.00 4.80 -1 9 0 -0.70 4.10 -20 0 1 -1.60 11.00 20 0 -1 -1.40 3.10 18 0 -1 -3.40 5.90 -18 0 1 -9.80 7.80 -16 0 1 13.90 10.80 -14 0 1 11.30 10.40 14 0 -1 5.20 3.50 14 0 -1 -0.70 1.80 14 0 -1 2.10 1.50 12 0 -1 -0.30 1.10 -12 0 1 14.50 8.60 12 0 -1 2.30 2.80 12 0 -1 4.90 3.00 -10 0 1 6.20 7.30 10 0 -1 0.70 2.60 10 0 -1 0.30 1.40 10 0 -1 -0.10 0.90 8 0 -1 1.30 2.10 8 0 -1 0.20 1.20 8 0 -1 0.30 0.90 -8 0 1 4.60 6.40 6 0 -1 1.20 2.00 -6 0 1 4.80 5.60 6 0 -1 -0.30 1.00 6 0 -1 -1.20 1.10 -6 0 1 2.00 2.10 6 0 -1 0.20 4.10 4 0 -1 8.40 4.40 -4 0 1 6.40 4.80 -2 0 1 0.70 0.40 2 0 -1 0.20 1.80 2 0 -1 0.60 0.50 2 0 -1 0.20 0.60 -2 0 1 2.30 2.10 2 0 1 -0.50 1.10 -2 0 -1 0.20 0.90 2 0 1 -0.10 0.80 -2 0 -1 0.30 1.10 -4 0 -1 3.30 3.50 4 0 1 3.30 2.90 -4 0 -1 1.40 1.60 4 0 1 0.10 1.60 -6 0 -1 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9 2.90 4.50 -4 8 -9 -0.90 4.20 20 0 -10 -0.70 2.30 -20 0 10 3.70 8.50 20 0 -10 1.90 3.10 -18 0 10 3.40 8.10 18 0 -10 1.30 2.30 18 0 -10 6.70 3.30 -16 0 10 25.80 10.50 16 0 -10 22.40 4.30 16 0 -10 22.40 4.00 -14 0 10 27.20 10.10 14 0 -10 20.70 4.00 12 0 -10 51.59 4.00 -12 0 10 59.49 10.70 12 0 -10 54.89 5.10 -12 0 10 66.99 4.00 10 0 -10 48.40 3.10 -10 0 10 53.89 10.20 10 0 -10 47.80 4.80 -10 0 10 49.99 3.20 8 0 -10 9.40 2.70 -8 0 10 5.20 5.80 6 0 -10 140.09 7.20 -6 0 10 129.69 9.80 4 0 -10 1044.80 32.70 -4 0 10 1053.09 35.40 2 0 -10 843.42 25.80 -2 0 10 926.21 31.70 2 0 -10 914.01 28.30 -2 0 10 922.41 25.80 0 0 -10 10.10 2.20 0 0 10 12.90 2.50 0 0 10 13.30 4.40 0 0 -10 10.30 2.30 -2 0 -10 237.98 9.00 2 0 10 260.87 9.70 2 0 10 222.38 12.20 -2 0 -10 225.08 9.10 -2 0 -10 240.18 9.30 -4 0 -10 17.40 2.30 -4 0 -10 17.80 2.60 4 0 10 16.60 4.90 -6 0 -10 64.89 7.60 -6 0 -10 59.59 3.80 6 0 10 58.89 5.80 -6 0 -10 67.19 3.40 -8 0 -10 55.29 9.50 8 0 10 48.00 6.80 -10 0 -10 94.49 10.50 10 0 10 97.09 8.20 -12 0 -10 -2.00 5.30 12 0 10 1.20 4.20 14 0 10 23.60 6.20 -14 0 -10 24.90 8.70 16 0 10 4.40 4.80 -16 0 -10 4.80 7.60 18 0 10 5.20 5.90 -18 0 -10 -3.00 10.20 21 -1 -10 4.80 3.60 21 1 -10 -4.50 3.00 21 1 -10 0.60 3.30 -19 -1 10 15.30 9.30 19 -1 -10 4.90 3.00 19 -1 -10 -0.10 1.70 -19 1 10 17.50 9.40 19 1 -10 -0.50 2.40 19 1 -10 7.60 2.80 -17 -1 10 -1.70 7.30 17 -1 -10 1.80 2.80 17 -1 -10 2.00 2.30 -17 1 10 4.40 7.80 17 1 -10 2.60 2.50 17 1 -10 1.60 2.70 -15 -1 10 8.50 8.00 15 -1 -10 3.40 2.70 15 -1 -10 3.70 2.90 15 1 -10 6.90 2.90 -15 1 10 1.10 8.10 15 1 -10 5.60 3.10 13 -1 -10 15.30 4.10 13 -1 -10 20.40 4.00 -13 -1 10 8.00 8.90 13 1 -10 13.60 3.70 -13 1 10 2.10 8.10 13 1 -10 9.90 3.00 -11 -1 10 6.20 2.10 11 -1 -10 3.20 2.20 -11 -1 10 0.80 7.10 11 -1 -10 -0.50 2.40 11 1 -10 2.30 2.00 -11 1 10 9.30 2.60 -11 1 10 -12.70 6.20 11 1 -10 5.10 2.80 9 -1 -10 2.40 2.20 9 -1 -10 1.90 1.80 -9 -1 10 9.00 1.70 -9 -1 10 -3.90 5.90 -9 1 10 -2.10 6.20 -9 1 10 0.70 2.20 9 1 -10 2.50 2.20 9 1 -10 2.60 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3 -3 10 27.40 6.20 3 -3 10 31.30 5.20 -3 3 -10 28.60 3.90 3 3 10 30.10 5.10 3 3 10 26.40 5.70 3 3 10 31.30 4.60 5 -3 10 -6.40 3.00 -5 -3 -10 1.80 4.60 5 3 10 2.20 2.80 -5 3 -10 0.80 2.30 5 3 10 -2.20 3.60 -7 -3 -10 45.40 8.60 7 -3 10 34.50 6.20 7 3 10 37.50 4.50 -7 3 -10 39.20 4.60 7 3 10 26.50 5.10 -7 3 -10 38.70 7.40 9 -3 10 45.30 7.50 -9 -3 -10 54.19 9.90 9 3 10 39.30 6.50 -9 3 -10 34.50 8.10 9 3 10 37.90 3.80 -9 3 -10 31.20 3.70 11 -3 10 -1.20 1.30 11 -3 10 3.20 5.10 -11 -3 -10 5.20 6.40 -11 -3 -10 -5.60 2.30 11 3 10 7.20 2.20 -11 3 -10 3.70 5.90 -11 3 -10 1.20 1.70 13 -3 10 -0.20 4.30 -13 -3 -10 1.90 6.70 -13 3 -10 3.70 6.50 13 3 10 0.70 4.00 -15 -3 -10 1.00 8.40 15 -3 10 9.40 5.00 -15 3 -10 -0.50 7.50 15 3 10 -0.10 4.10 -17 -3 -10 -4.60 12.90 17 -3 10 13.40 5.80 17 3 10 1.70 4.10 -17 3 -10 -6.80 10.00 18 -4 -10 5.20 4.10 -18 -4 10 12.30 8.10 18 -4 -10 -2.00 2.60 -18 4 10 28.90 9.30 18 4 -10 -0.40 3.60 18 4 -10 0.50 3.00 16 -4 -10 4.30 3.90 -16 -4 10 12.00 7.60 16 -4 -10 3.60 2.90 16 4 -10 3.60 3.50 -16 4 10 12.60 7.40 -14 -4 10 5.30 8.00 14 -4 -10 5.40 3.10 -14 -4 10 -2.30 3.40 -14 4 10 6.50 3.90 14 4 -10 11.60 4.60 -14 4 10 24.60 8.90 -12 -4 10 1.20 7.80 -12 -4 10 1.80 3.80 12 -4 -10 -0.10 2.90 -12 4 10 2.90 3.50 -12 4 10 -0.90 7.30 12 4 -10 3.00 3.30 -10 -4 10 55.49 10.90 -10 -4 10 52.39 6.20 10 -4 -10 55.49 6.90 10 4 -10 41.90 5.90 -10 4 10 52.89 10.10 -10 4 10 32.00 6.40 8 -4 -10 3.30 3.30 -8 -4 10 6.50 4.30 -8 -4 10 -7.10 6.40 -8 4 10 -1.20 6.50 8 4 -10 -1.20 3.10 -8 4 10 1.80 3.60 -6 -4 10 -0.30 4.00 -6 -4 10 -9.10 5.30 6 -4 -10 0.50 3.10 -6 4 10 4.20 3.30 -6 4 10 1.90 4.90 6 4 -10 1.10 3.30 -4 -4 10 8.60 6.10 4 -4 -10 5.90 3.90 -4 -4 10 7.00 4.50 4 4 -10 6.30 3.30 -4 4 10 7.90 4.00 2 -4 -10 -4.00 3.20 -2 -4 10 1.40 3.90 -2 -4 10 2.40 5.00 -2 4 10 -1.60 4.20 -2 4 10 4.70 3.70 2 4 -10 3.10 3.20 0 -4 10 22.20 4.80 0 -4 10 24.80 7.30 0 -4 -10 20.10 4.70 0 4 10 16.60 4.70 0 4 -10 16.80 4.00 0 4 10 26.40 6.60 2 -4 10 -0.50 5.20 2 -4 10 9.50 4.50 2 4 10 2.30 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2.40 -7 1 24 -5.60 4.20 7 1 -24 1.00 2.90 -5 -1 24 9.50 7.60 5 -1 -24 -0.50 2.70 5 1 -24 -3.00 2.90 -5 1 24 0.40 5.80 3 -1 -24 2.90 3.10 -3 -1 24 12.30 6.80 -3 1 24 -0.10 6.10 3 1 -24 0.00 3.00 1 -1 -24 1.30 2.70 -1 -1 24 6.90 7.40 -1 -1 24 -2.20 3.00 1 1 -24 2.50 2.80 -1 1 24 11.10 6.90 -1 1 24 -2.90 3.10 -1 -1 -24 -1.30 2.50 1 -1 24 -6.10 3.50 1 -1 24 0.40 6.30 1 1 24 -0.80 5.30 1 1 24 0.70 3.60 -1 1 -24 0.40 3.00 -3 -1 -24 2.80 2.60 3 -1 24 1.00 3.80 3 -1 24 1.90 7.10 -3 1 -24 -2.50 2.40 3 1 24 2.70 4.20 3 1 24 3.00 5.90 -8 -2 24 4.40 6.70 8 -2 -24 1.70 4.30 -8 2 24 10.10 7.20 8 2 -24 1.20 3.60 6 -2 -24 5.80 4.10 -6 -2 24 15.40 6.70 -6 2 24 6.50 5.90 6 2 -24 -0.20 3.60 4 -2 -24 3.20 2.90 -4 -2 24 3.30 6.20 -4 2 24 12.90 6.40 4 2 -24 -2.90 2.40 -2 -2 24 4.00 6.70 2 -2 -24 7.30 3.50 2 2 -24 -2.10 2.90 -2 2 24 13.90 6.30 0 -2 24 6.70 7.10 0 -2 -24 0.90 2.70 0 -2 24 4.60 3.60 0 2 -24 5.60 3.20 0 2 24 0.80 6.00 2 -2 24 8.00 8.10 -2 -2 -24 6.70 3.30 2 -2 24 4.40 4.10 2 2 24 6.00 7.20 -2 2 -24 1.60 3.00 -5 -3 24 6.30 7.00 5 -3 -24 -1.00 3.50 5 3 -24 -1.10 3.50 -5 3 24 14.10 7.20 3 -3 -24 -1.50 3.30 3 -3 -24 -1.50 1.70 -3 -3 24 -1.20 7.00 3 3 -24 7.30 4.00 -3 3 24 5.60 7.50 -1 -3 24 -0.30 3.40 -1 -3 24 -3.20 6.10 1 -3 -24 1.60 2.40 1 -3 -24 0.10 2.60 -1 3 24 9.70 7.50 1 3 -24 7.10 3.80 -8 0 25 -0.10 6.00 8 0 -25 -5.20 2.60 6 0 -25 0.10 2.70 -6 0 25 9.20 8.50 -4 0 25 6.80 6.70 4 0 -25 -2.90 2.80 2 0 -25 -2.50 2.70 -2 0 25 1.70 6.40 0 0 25 -6.00 3.30 0 0 -25 1.00 2.90 0 0 25 -2.60 6.50 -7 -1 25 1.00 5.50 7 -1 -25 -3.70 2.70 -7 1 25 7.80 6.50 7 1 -25 -1.50 3.00 -5 -1 25 2.40 5.10 5 -1 -25 3.40 3.50 -5 1 25 8.40 6.90 5 1 -25 -3.20 2.70 3 -1 -25 -0.90 2.70 -3 -1 25 3.80 6.90 -3 1 25 -3.60 5.90 3 1 -25 -5.20 2.40 1 -1 -25 12.00 4.00 -1 -1 25 7.00 7.00 -1 -1 25 -3.40 3.40 1 1 -25 5.70 3.40 -1 1 25 13.70 7.30 -1 -1 -25 2.60 3.30 1 -1 25 -10.30 3.40 1 1 25 -3.10 3.90 -1 1 -25 -0.90 3.20 4 -2 -25 0.80 3.00 -4 -2 25 5.40 7.20 4 2 -25 -0.40 3.20 -4 2 25 -2.20 6.60 2 -2 -25 -3.50 1.60 -2 -2 25 2.00 7.30 2 -2 -25 2.90 3.20 -2 2 25 8.30 8.00 2 2 -25 -4.90 3.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 42451 _shelx_res_file ; TITL AUF66_a.res in C2/c AUF66_A.res created by SHELXL-2017/1 at 12:45:40 on 18-Feb-2020 REM Old TITL AUF66 in C2/c REM SHELXT solution in C2/c REM R1 0.195, Rweak 0.077, Alpha 0.053, Orientation as input REM Formula found by SHELXT: C15 N3 O2 CELL 0.71073 17.4362 7.2485 20.5951 90.000 99.181 90.000 ZERR 8.000 0.0020 0.0007 0.0022 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O UNIT 120 96 16 24 TEMP 23.000 SIZE 0.491 0.153 0.059 L.S. 49 BOND $H HTAB ACTA CONF OMIT 0 52 OMIT -13 7 1 OMIT -8 6 13 OMIT 13 7 0 OMIT -9 5 19 OMIT -7 5 20 OMIT -15 5 12 OMIT 0 6 16 HTAB N2 O2 EQIV $1 -x+1/2, -y+1/2, -z+1 HTAB N2 O2_$1 FMAP 2 PLAN 20 WGHT 0.051700 2.983100 EXTI 0.001472 FVAR 0.26930 O1 4 0.420006 0.238196 0.418311 11.00000 0.04841 0.07497 = 0.04057 -0.00308 0.00717 -0.00362 O2 4 0.311754 0.307667 0.459970 11.00000 0.04837 0.09172 = 0.05334 -0.00588 0.00489 -0.00608 O3 4 0.533816 0.135915 0.344259 11.00000 0.06588 0.10317 = 0.05270 -0.00736 0.02002 0.00415 N1 3 0.423890 0.339626 0.588112 11.00000 0.04883 0.05048 = 0.04408 0.00100 0.00820 -0.00676 N2 3 0.351836 0.369906 0.597502 11.00000 0.04712 0.05987 = 0.04269 -0.00439 0.00617 -0.00165 C1 1 0.381067 0.284150 0.469325 11.00000 0.04949 0.05409 = 0.04281 0.00096 0.01182 -0.01119 C2 1 0.437420 0.295505 0.529592 11.00000 0.04761 0.04448 = 0.03746 0.00197 0.00499 -0.00768 C3 1 0.512079 0.253641 0.511983 11.00000 0.04981 0.04225 = 0.04308 0.00515 0.00816 -0.00850 C4 1 0.587177 0.241901 0.546000 11.00000 0.05285 0.07332 = 0.04892 0.00375 0.00138 -0.00905 AFIX 43 H4A 2 0.598100 0.265759 0.590895 11.00000 -1.20000 AFIX 0 C5 1 0.644926 0.193704 0.510958 11.00000 0.04374 0.08320 = 0.06830 0.01242 0.00701 -0.00211 AFIX 43 H5A 2 0.695811 0.185900 0.532762 11.00000 -1.20000 AFIX 0 C6 1 0.629731 0.156436 0.444266 11.00000 0.05375 0.06661 = 0.06722 0.00996 0.01939 -0.00144 AFIX 43 H6A 2 0.670362 0.122386 0.422508 11.00000 -1.20000 AFIX 0 C7 1 0.555740 0.168755 0.409529 11.00000 0.05793 0.05079 = 0.04993 0.00251 0.01593 -0.00487 C8 1 0.498474 0.218344 0.445375 11.00000 0.04809 0.04698 = 0.04467 0.00634 0.00697 -0.00733 C9 1 0.593585 0.080390 0.308183 11.00000 0.09235 0.08395 = 0.06551 -0.00568 0.03807 0.01069 AFIX 137 H9A 2 0.571774 0.063916 0.262729 11.00000 -1.50000 H9B 2 0.615969 -0.033713 0.325700 11.00000 -1.50000 H9C 2 0.633113 0.173711 0.311913 11.00000 -1.50000 AFIX 0 C10 1 0.337734 0.427013 0.659655 11.00000 0.05241 0.04750 = 0.04039 -0.00104 0.00796 -0.00682 C11 1 0.395679 0.432630 0.713543 11.00000 0.05485 0.07562 = 0.04560 -0.01011 0.00160 0.00310 AFIX 43 H11A 2 0.445790 0.395598 0.709579 11.00000 -1.20000 AFIX 0 C12 1 0.379624 0.492571 0.772850 11.00000 0.07399 0.08030 = 0.04458 -0.01065 0.00195 0.00294 AFIX 43 H12A 2 0.419310 0.497293 0.808808 11.00000 -1.20000 AFIX 0 C13 1 0.306185 0.545791 0.780293 11.00000 0.07776 0.06933 = 0.04720 -0.00811 0.01739 -0.00158 AFIX 43 H13A 2 0.295701 0.585028 0.820967 11.00000 -1.20000 AFIX 0 C14 1 0.248219 0.540210 0.726588 11.00000 0.06011 0.06150 = 0.06453 0.00213 0.02478 0.00409 AFIX 43 H14A 2 0.198194 0.577300 0.730814 11.00000 -1.20000 AFIX 0 C15 1 0.263728 0.479926 0.666404 11.00000 0.04997 0.05950 = 0.05113 0.00369 0.00608 -0.00281 AFIX 43 H15A 2 0.224071 0.475136 0.630425 11.00000 -1.20000 AFIX 0 H1 2 0.312694 0.352445 0.562654 11.00000 0.08184 HKLF 4 REM AUF66_a.res in C2/c REM R1 = 0.0733 for 1463 Fo > 4sig(Fo) and 0.1274 for all 2427 data REM 187 parameters refined using 0 restraints END WGHT 0.0454 2.5552 REM Instructions for potential hydrogen bonds HTAB N2 O2 HTAB N2 O2_$1 REM Highest difference peak 0.182, deepest hole -0.179, 1-sigma level 0.040 Q1 1 0.5211 0.1280 0.4260 11.00000 0.05 0.18 Q2 1 0.5160 0.3247 0.4812 11.00000 0.05 0.18 Q3 1 0.4931 0.3454 0.5287 11.00000 0.05 0.17 Q4 1 0.5591 0.0632 0.3797 11.00000 0.05 0.16 Q5 1 0.6223 0.2633 0.4692 11.00000 0.05 0.16 Q6 1 0.6380 -0.0061 0.3524 11.00000 0.05 0.16 Q7 1 0.5309 0.2698 0.4292 11.00000 0.05 0.15 Q8 1 0.5158 0.1680 0.4817 11.00000 0.05 0.15 Q9 1 0.4181 0.2272 0.5475 11.00000 0.05 0.14 Q10 1 0.3134 0.2156 0.4223 11.00000 0.05 0.14 Q11 1 0.2602 0.5881 0.6973 11.00000 0.05 0.14 Q12 1 0.5534 0.0009 0.3248 11.00000 0.05 0.13 Q13 1 0.4780 0.2202 0.5316 11.00000 0.05 0.13 Q14 1 0.4805 0.1396 0.4697 11.00000 0.05 0.13 Q15 1 0.5036 0.4778 0.7208 11.00000 0.05 0.13 Q16 1 0.4529 0.5095 0.6886 11.00000 0.05 0.13 Q17 1 0.5396 -0.0010 0.3117 11.00000 0.05 0.13 Q18 1 0.6006 0.1649 0.5185 11.00000 0.05 0.12 Q19 1 0.3031 0.5105 0.6536 11.00000 0.05 0.12 Q20 1 0.5972 0.3149 0.5159 11.00000 0.05 0.12 ; _shelx_res_checksum 89171 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_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 0.42001(12) 0.2382(3) 0.41831(10) 0.0546(6) Uani d 1 . . O O2 0.31175(13) 0.3077(4) 0.45997(10) 0.0648(7) Uani d 1 . . O O3 0.53382(14) 0.1359(4) 0.34426(11) 0.0728(8) Uani d 1 . . N N1 0.42389(15) 0.3396(4) 0.58811(12) 0.0477(7) Uani d 1 . . N N2 0.35184(16) 0.3699(4) 0.59750(13) 0.0500(7) Uani d 1 . . C C1 0.38107(19) 0.2841(5) 0.46932(14) 0.0483(8) Uani d 1 . . C C2 0.43742(17) 0.2955(4) 0.52959(13) 0.0434(8) Uani d 1 . . C C3 0.51208(17) 0.2536(4) 0.51198(14) 0.0450(8) Uani d 1 . . C C4 0.58718(18) 0.2419(5) 0.54600(16) 0.0591(10) Uani d 1 . . H H4A 0.598100 0.265759 0.590895 0.071 Uiso calc 1 . . C C5 0.64493(19) 0.1937(5) 0.51096(18) 0.0653(10) Uani d 1 . . H H5A 0.695811 0.185900 0.532762 0.078 Uiso calc 1 . . C C6 0.6297(2) 0.1564(5) 0.44427(17) 0.0615(10) Uani d 1 . . H H6A 0.670362 0.122386 0.422508 0.074 Uiso calc 1 . . C C7 0.55574(19) 0.1688(5) 0.40953(15) 0.0521(9) Uani d 1 . . C C8 0.49847(17) 0.2183(4) 0.44538(14) 0.0466(8) Uani d 1 . . C C9 0.5936(2) 0.0804(6) 0.30818(17) 0.0778(12) Uani d 1 . . H H9A 0.571774 0.063916 0.262729 0.117 Uiso calc 1 . . H H9B 0.615969 -0.033713 0.325700 0.117 Uiso calc 1 . . H H9C 0.633113 0.173711 0.311913 0.117 Uiso calc 1 . . C C10 0.33773(18) 0.4270(4) 0.65966(14) 0.0467(8) Uani d 1 . . C C11 0.3957(2) 0.4326(5) 0.71354(14) 0.0594(10) Uani d 1 . . H H11A 0.445790 0.395598 0.709579 0.071 Uiso calc 1 . . C C12 0.3796(2) 0.4926(5) 0.77285(16) 0.0671(11) Uani d 1 . . H H12A 0.419310 0.497293 0.808808 0.081 Uiso calc 1 . . C C13 0.3062(2) 0.5458(5) 0.78029(16) 0.0640(10) Uani d 1 . . H H13A 0.295701 0.585028 0.820967 0.077 Uiso calc 1 . . C C14 0.2482(2) 0.5402(5) 0.72659(16) 0.0604(10) Uani d 1 . . H H14A 0.198194 0.577300 0.730814 0.073 Uiso calc 1 . . C C15 0.26373(19) 0.4799(5) 0.66640(15) 0.0538(9) Uani d 1 . . H H15A 0.224071 0.475136 0.630425 0.065 Uiso calc 1 . . H H1 0.313(2) 0.352(5) 0.5627(17) 0.082(13) 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 0.0484(13) 0.0750(18) 0.0406(11) -0.0036(12) 0.0072(10) -0.0031(11) O2 0.0484(15) 0.092(2) 0.0533(14) -0.0061(13) 0.0049(11) -0.0059(12) O3 0.0659(16) 0.103(2) 0.0527(14) 0.0041(14) 0.0200(12) -0.0074(14) N1 0.0488(16) 0.0505(18) 0.0441(14) -0.0068(13) 0.0082(12) 0.0010(12) N2 0.0471(17) 0.060(2) 0.0427(15) -0.0017(14) 0.0062(13) -0.0044(13) C1 0.049(2) 0.054(2) 0.0428(17) -0.0112(17) 0.0118(15) 0.0010(15) C2 0.0476(18) 0.044(2) 0.0375(16) -0.0077(15) 0.0050(14) 0.0020(14) C3 0.0498(19) 0.042(2) 0.0431(16) -0.0085(15) 0.0082(14) 0.0052(14) C4 0.053(2) 0.073(3) 0.0489(18) -0.0091(18) 0.0014(16) 0.0038(17) C5 0.044(2) 0.083(3) 0.068(2) -0.0021(18) 0.0070(18) 0.012(2) C6 0.054(2) 0.067(3) 0.067(2) -0.0014(18) 0.0194(18) 0.0100(19) C7 0.058(2) 0.051(2) 0.0499(19) -0.0049(17) 0.0159(17) 0.0025(16) C8 0.0481(19) 0.047(2) 0.0447(17) -0.0073(15) 0.0070(15) 0.0063(15) C9 0.092(3) 0.084(3) 0.066(2) 0.011(2) 0.038(2) -0.006(2) C10 0.052(2) 0.047(2) 0.0404(16) -0.0068(15) 0.0080(15) -0.0010(15) C11 0.055(2) 0.076(3) 0.0456(18) 0.0031(18) 0.0016(16) -0.0101(17) C12 0.074(3) 0.080(3) 0.0446(19) 0.003(2) 0.0019(18) -0.0106(18) C13 0.078(3) 0.069(3) 0.047(2) -0.002(2) 0.0174(19) -0.0081(17) C14 0.060(2) 0.061(3) 0.065(2) 0.0041(18) 0.0248(19) 0.0021(18) C15 0.050(2) 0.060(2) 0.0511(19) -0.0028(17) 0.0061(16) 0.0037(16) 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 C1 O1 C8 . . 106.9(2) ? C7 O3 C9 . . 116.7(3) ? C2 N1 N2 . . 119.5(3) ? N1 N2 C10 . . 119.5(3) ? N1 N2 H1 . . 118(2) ? C10 N2 H1 . . 123(2) ? O2 C1 O1 . . 121.0(3) ? O2 C1 C2 . . 130.6(3) ? O1 C1 C2 . . 108.4(3) ? N1 C2 C3 . . 126.1(3) ? N1 C2 C1 . . 127.2(3) ? C3 C2 C1 . . 106.7(2) ? C8 C3 C4 . . 119.4(3) ? C8 C3 C2 . . 105.7(3) ? C4 C3 C2 . . 134.9(3) ? C5 C4 C3 . . 117.6(3) ? C5 C4 H4A . . 121.2 ? C3 C4 H4A . . 121.2 ? C4 C5 C6 . . 122.1(3) ? C4 C5 H5A . . 119.0 ? C6 C5 H5A . . 119.0 ? C7 C6 C5 . . 121.3(3) ? C7 C6 H6A . . 119.4 ? C5 C6 H6A . . 119.4 ? O3 C7 C6 . . 126.6(3) ? O3 C7 C8 . . 117.5(3) ? C6 C7 C8 . . 115.9(3) ? C3 C8 C7 . . 123.8(3) ? C3 C8 O1 . . 112.3(3) ? C7 C8 O1 . . 123.9(3) ? O3 C9 H9A . . 109.5 ? O3 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? O3 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C15 C10 C11 . . 119.4(3) ? C15 C10 N2 . . 118.6(3) ? C11 C10 N2 . . 122.1(3) ? C12 C11 C10 . . 120.1(3) ? C12 C11 H11A . . 120.0 ? C10 C11 H11A . . 120.0 ? C11 C12 C13 . . 121.2(3) ? C11 C12 H12A . . 119.4 ? C13 C12 H12A . . 119.4 ? C12 C13 C14 . . 118.8(3) ? C12 C13 H13A . . 120.6 ? C14 C13 H13A . . 120.6 ? C13 C14 C15 . . 120.5(3) ? C13 C14 H14A . . 119.8 ? C15 C14 H14A . . 119.8 ? C10 C15 C14 . . 120.0(3) ? C10 C15 H15A . . 120.0 ? C14 C15 H15A . . 120.0 ? 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 C1 . 1.380(3) ? O1 C8 . 1.400(3) ? O2 C1 . 1.205(3) ? O3 C7 . 1.359(4) ? O3 C9 . 1.431(4) ? N1 C2 . 1.304(3) ? N1 N2 . 1.320(3) ? N2 C10 . 1.404(4) ? N2 H1 . 0.92(4) ? C1 C2 . 1.457(4) ? C2 C3 . 1.438(4) ? C3 C8 . 1.378(4) ? C3 C4 . 1.386(4) ? C4 C5 . 1.374(4) ? C4 H4A . 0.9300 ? C5 C6 . 1.383(5) ? C5 H5A . 0.9300 ? C6 C7 . 1.375(5) ? C6 H6A . 0.9300 ? C7 C8 . 1.381(4) ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 C15 . 1.374(4) ? C10 C11 . 1.377(4) ? C11 C12 . 1.367(4) ? C11 H11A . 0.9300 ? C12 C13 . 1.369(5) ? C12 H12A . 0.9300 ? C13 C14 . 1.375(5) ? C13 H13A . 0.9300 ? C14 C15 . 1.381(4) ? C14 H14A . 0.9300 ? C15 H15A . 0.9300 ? 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 N2 H1 O2 . 0.92(4) 2.14(3) 2.843(3) 133(3) yes N2 H1 O2 7_556 0.92(4) 2.44(4) 3.181(4) 138(3) yes C9 H9C Cg3 5_666 0.96 2.70 3.555(4) 149 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 C2 N1 N2 C10 . . . . -176.6(3) ? C8 O1 C1 O2 . . . . -179.2(3) ? C8 O1 C1 C2 . . . . 0.8(3) ? N2 N1 C2 C3 . . . . -178.2(3) ? N2 N1 C2 C1 . . . . 3.7(5) ? O2 C1 C2 N1 . . . . -1.8(6) ? O1 C1 C2 N1 . . . . 178.3(3) ? O2 C1 C2 C3 . . . . 179.9(4) ? O1 C1 C2 C3 . . . . -0.1(3) ? N1 C2 C3 C8 . . . . -179.0(3) ? C1 C2 C3 C8 . . . . -0.7(3) ? N1 C2 C3 C4 . . . . 1.5(6) ? C1 C2 C3 C4 . . . . 179.9(4) ? C8 C3 C4 C5 . . . . -0.4(5) ? C2 C3 C4 C5 . . . . 178.9(4) ? C3 C4 C5 C6 . . . . -0.5(6) ? C4 C5 C6 C7 . . . . 1.0(6) ? C9 O3 C7 C6 . . . . 0.9(5) ? C9 O3 C7 C8 . . . . -178.5(3) ? C5 C6 C7 O3 . . . . 179.9(3) ? C5 C6 C7 C8 . . . . -0.6(5) ? C4 C3 C8 C7 . . . . 0.8(5) ? C2 C3 C8 C7 . . . . -178.7(3) ? C4 C3 C8 O1 . . . . -179.3(3) ? C2 C3 C8 O1 . . . . 1.2(4) ? O3 C7 C8 C3 . . . . 179.2(3) ? C6 C7 C8 C3 . . . . -0.3(5) ? O3 C7 C8 O1 . . . . -0.6(5) ? C6 C7 C8 O1 . . . . 179.8(3) ? C1 O1 C8 C3 . . . . -1.3(3) ? C1 O1 C8 C7 . . . . 178.6(3) ? N1 N2 C10 C15 . . . . 172.0(3) ? N1 N2 C10 C11 . . . . -7.6(5) ? C15 C10 C11 C12 . . . . -0.8(5) ? N2 C10 C11 C12 . . . . 178.7(3) ? C10 C11 C12 C13 . . . . 0.8(6) ? C11 C12 C13 C14 . . . . -0.7(6) ? C12 C13 C14 C15 . . . . 0.7(5) ? C11 C10 C15 C14 . . . . 0.8(5) ? N2 C10 C15 C14 . . . . -178.8(3) ? C13 C14 C15 C10 . . . . -0.8(5) ? _cod_database_fobs_code 2243888