#------------------------------------------------------------------------------ #$Date: 2022-07-30 02:56:58 +0100 (Sat, 30 Jul 2022) $ #$Revision: 277011 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244138.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_2244138 loop_ _publ_author_name 'Missioui, Mohcine' 'Guerrab, Walid' 'Alsubari, Abdulsalam' 'Mague, Joel T.' 'Ramli, Youssef' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 2-azido-N-(4-fluorophenyl)acetamide ; _journal_coeditor_code VM2266 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 855 _journal_page_last 859 _journal_paper_doi 10.1107/S2056989022006764 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C8 H7 F N4 O' _chemical_formula_moiety 'C8 H7 F N4 O' _chemical_formula_sum 'C8 H7 F N4 O' _chemical_formula_weight 194.18 _chemical_name_systematic ; 2-Azido-N-(4-fluorophenyl)acetamide ; _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 geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 112.378(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.8398(7) _cell_length_b 19.0207(11) _cell_length_c 9.3307(5) _cell_measurement_reflns_used 8481 _cell_measurement_temperature 296.(2) _cell_measurement_theta_max 68.2848 _cell_measurement_theta_min 2.3229 _cell_volume 1778.93(18) _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 ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.985 _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 0.0340 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 12623 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 68.495 _diffrn_reflns_theta_min 4.411 _diffrn_source 'INCOATEC I\mS micro--focus source' _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thick plate' _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.466 _exptl_crystal_size_mid 0.246 _exptl_crystal_size_min 0.146 _refine_diff_density_max 0.446 _refine_diff_density_min -0.237 _refine_ls_extinction_coef 0.0033(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL 2018/3 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 3224 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0533 _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^)+(0.0828P)^2^+0.4718P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1485 _refine_ls_wR_factor_ref 0.1622 _reflns_number_gt 2545 _reflns_number_total 3224 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2266sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244138 _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 0.654 _shelx_estimated_absorpt_t_max 0.868 _shelx_hkl_file ; 0 0 -4 60.59 2.70 0 0 -5 0.00 0.20 0 0 -6 35.50 1.60 0 0 6 32.70 2.00 0 0 -7 2.10 0.40 0 0 7 0.10 0.60 0 0 -8 43.00 2.10 0 0 8 49.30 2.40 0 0 9 -0.10 0.40 0 0 -9 0.40 0.30 0 0 10 -0.20 0.30 0 -1 0 0.00 0.10 0 1 1 32.40 1.40 0 1 -1 33.80 1.50 0 -1 1 33.90 1.50 0 -1 -1 33.90 1.40 0 1 2 164.08 6.70 0 1 -2 154.58 6.70 0 -1 -2 157.38 6.70 0 1 -4 10.90 0.60 0 -1 -4 10.50 0.60 0 1 -5 126.59 5.40 0 -1 -5 124.29 5.40 0 1 -6 2.60 0.40 0 1 6 2.10 0.70 0 -1 6 2.60 1.10 0 -1 -6 2.10 0.40 0 1 7 0.10 0.50 0 1 -7 -0.30 0.20 0 -1 7 0.00 0.70 0 1 -8 4.50 0.50 0 -1 -8 4.10 0.50 0 1 -9 6.70 0.60 0 1 9 8.60 0.90 0 -1 -9 8.40 0.70 0 -1 9 8.70 0.90 0 1 10 0.20 0.40 0 -1 10 0.20 0.30 0 2 0 935.01 39.10 0 2 1 341.47 15.10 0 2 -1 352.96 15.10 0 -2 -1 374.56 15.10 0 -2 1 367.66 15.10 0 2 2 1442.66 59.89 0 2 -2 1398.36 59.89 0 -2 -2 1456.75 59.89 0 2 3 0.60 0.20 0 2 -3 0.00 0.20 0 2 -3 0.00 0.20 0 -2 -3 0.30 0.20 0 2 -4 363.66 15.20 0 -2 -4 358.56 15.20 0 2 -5 320.87 13.90 0 -2 -5 334.47 13.90 0 2 6 15.70 1.90 0 2 -6 19.70 1.00 0 -2 6 17.00 1.40 0 -2 -6 19.30 1.00 0 -2 -6 11.60 3.50 0 2 7 17.10 1.30 0 2 -7 17.60 1.00 0 -2 7 16.70 1.30 0 -2 -7 17.20 1.00 0 2 8 24.80 1.60 0 2 -8 22.80 1.20 0 -2 -8 21.40 1.20 0 -2 8 26.90 1.60 0 2 -9 0.10 0.20 0 2 9 0.40 0.40 0 -2 9 0.40 0.40 0 2 10 2.10 0.70 0 -2 10 2.00 0.60 0 3 0 0.10 0.10 0 -3 0 0.10 0.10 0 3 1 35.50 1.70 0 3 -1 38.10 1.70 0 -3 -1 37.50 1.70 0 -3 1 38.50 1.70 0 3 2 1700.23 75.99 0 3 -2 1835.22 75.99 0 -3 2 1863.01 75.99 0 -3 -2 1865.51 75.99 0 3 3 10.40 0.80 0 3 -3 10.90 0.80 0 -3 -3 12.10 0.80 0 3 -4 14.20 0.80 0 -3 -4 15.60 0.90 0 3 -5 264.07 11.10 0 -3 -5 258.97 11.10 0 3 -6 13.80 0.80 0 3 6 10.60 1.50 0 -3 6 13.70 1.20 0 -3 -6 12.20 0.80 0 3 7 3.00 1.00 0 3 -7 3.10 0.40 0 3 7 2.60 0.90 0 -3 7 3.90 0.90 0 -3 -7 2.10 0.50 0 3 8 0.60 0.50 0 -3 8 0.70 0.50 0 3 -9 1.90 0.40 0 3 9 1.90 0.80 0 -3 9 1.90 0.80 0 3 10 0.00 0.30 0 -3 10 -0.50 0.30 0 4 0 1.10 0.30 0 -4 0 1.30 0.30 0 4 1 29.20 1.40 0 4 -1 29.70 1.40 0 -4 1 30.60 1.40 0 -4 -1 30.20 1.40 0 4 -2 195.58 8.30 0 4 2 185.98 8.30 0 -4 -2 200.58 8.30 0 -4 2 195.98 8.30 0 4 3 77.09 3.40 0 4 -3 68.59 3.30 0 4 -3 78.29 3.40 0 -4 -3 78.39 3.40 0 4 -4 31.60 2.40 0 4 -4 29.40 1.40 0 4 4 29.90 1.70 0 4 -4 29.10 1.70 0 4 -5 130.59 5.60 0 -4 -5 128.39 5.60 0 4 -6 4.40 0.40 0 4 6 5.30 1.40 0 -4 6 4.30 1.10 0 -4 -6 4.40 0.50 0 -4 -6 7.10 2.20 0 4 -7 160.28 6.60 0 4 7 146.79 6.70 0 -4 -7 147.49 7.00 0 4 8 0.10 0.50 0 4 -8 0.10 0.20 0 -4 8 0.30 0.50 0 4 -9 7.10 0.50 0 4 9 6.80 0.90 0 -4 9 8.10 0.90 0 4 10 8.70 0.70 0 -4 10 9.50 0.80 0 -5 0 1.70 0.40 0 5 1 99.49 4.50 0 5 -1 102.59 4.50 0 -5 1 102.39 4.50 0 -5 -1 105.99 4.50 0 5 -2 1049.70 41.80 0 5 2 1003.40 41.80 0 -5 -2 1013.60 41.80 0 -5 2 916.11 41.90 0 5 -3 376.26 16.70 0 5 3 401.56 16.80 0 5 -3 401.26 16.80 0 -5 3 396.86 16.80 0 -5 -3 408.06 16.80 0 5 4 0.10 0.50 0 5 -4 0.40 0.50 0 5 -4 0.30 0.10 0 -5 -4 0.20 0.60 0 5 5 24.00 1.80 0 5 -5 26.10 1.20 0 -5 -5 23.00 3.10 0 5 6 -0.10 0.70 0 5 -6 0.40 0.20 0 -5 6 0.70 0.60 0 -5 -6 -0.50 0.90 0 5 -7 15.70 0.90 0 5 7 18.70 1.50 0 -5 7 16.10 1.30 0 -5 -7 18.30 2.20 0 5 -8 9.80 0.70 0 5 8 10.40 1.10 0 5 8 7.80 1.40 0 -5 8 10.40 1.10 0 -5 -8 10.90 2.60 0 5 -9 25.00 1.30 0 5 9 26.60 1.50 0 -5 9 25.60 1.50 0 5 10 10.50 0.70 0 -5 10 10.90 0.90 0 6 0 426.66 18.20 0 -6 0 433.36 18.20 0 6 -1 60.39 2.80 0 6 1 58.59 2.70 0 -6 -1 58.99 2.70 0 -6 1 56.09 2.70 0 6 2 1455.65 64.99 0 6 -2 1581.44 64.99 0 -6 -2 1594.94 64.99 0 -6 2 1567.34 64.99 0 6 -3 593.04 24.20 0 6 3 580.84 24.20 0 6 -3 518.05 24.00 0 -6 -3 591.44 24.20 0 -6 3 573.74 24.20 0 6 -4 17.70 2.10 0 6 4 25.60 2.00 0 6 -4 23.10 1.10 0 -6 -4 21.30 2.10 0 6 -5 87.99 3.70 0 6 5 84.59 4.00 0 -6 5 80.89 4.00 0 -6 -5 85.49 4.30 0 6 6 108.79 5.00 0 6 -6 109.69 4.80 0 -6 -6 113.99 5.30 0 -6 6 109.59 5.00 0 6 -7 0.80 0.20 0 6 7 0.30 0.60 0 -6 -7 2.20 1.00 0 -6 7 1.40 0.60 0 6 -8 23.40 1.20 0 6 8 24.10 1.60 0 6 8 24.50 1.60 0 -6 8 24.80 1.50 0 -6 -8 26.20 2.40 0 6 9 25.00 1.50 0 6 -9 23.80 1.20 0 -6 9 24.70 1.40 0 6 10 2.90 0.50 0 7 0 0.50 0.20 0 -7 0 0.00 0.30 0 7 1 93.99 4.20 0 7 -1 96.49 4.20 0 -7 -1 93.09 4.20 0 -7 1 90.99 4.20 0 7 -2 742.13 30.20 0 7 2 726.93 30.20 0 -7 2 687.73 30.20 0 -7 -2 707.93 30.20 0 7 -3 34.10 1.90 0 7 -3 33.30 1.50 0 7 3 30.70 2.00 0 -7 -3 31.90 2.10 0 -7 3 30.70 2.10 0 7 -4 40.20 2.50 0 7 4 35.90 2.60 0 7 -4 37.80 1.80 0 7 -5 106.89 4.40 0 7 5 98.99 4.50 0 -7 -5 100.39 4.80 0 -7 5 92.19 4.60 0 7 6 18.90 1.40 0 7 -6 18.60 1.00 0 -7 -6 23.60 2.10 0 -7 6 16.20 1.50 0 7 7 3.70 1.10 0 7 -7 3.50 0.40 0 -7 -7 3.40 0.90 0 7 -8 6.70 0.60 0 7 8 7.00 1.00 0 7 8 6.60 1.20 0 -7 8 6.80 1.00 0 7 -9 14.60 1.00 0 7 9 16.30 1.10 0 -7 9 17.90 1.20 0 8 0 100.99 4.40 0 -8 0 94.49 4.50 0 8 1 0.70 0.30 0 8 -1 0.30 0.30 0 -8 1 -0.10 0.40 0 -8 -1 1.20 0.40 0 8 2 304.57 12.70 0 8 -2 316.67 12.80 0 8 -2 281.47 12.50 0 -8 -2 295.67 12.80 0 -8 2 283.17 12.80 0 8 -3 41.90 2.30 0 8 -3 41.10 1.80 0 8 3 37.80 2.40 0 -8 -3 39.60 2.70 0 -8 3 39.40 2.80 0 8 -4 6.50 2.30 0 8 -4 10.90 0.60 0 -8 -4 11.50 1.90 0 8 5 103.19 4.60 0 8 -5 104.49 4.40 0 -8 -5 104.29 4.80 0 -8 5 88.49 4.60 0 8 -6 11.70 0.70 0 8 6 11.50 1.20 0 -8 6 7.30 2.00 0 -8 -6 13.90 1.90 0 8 -7 1.60 0.30 0 8 7 1.20 0.60 0 -8 -7 1.80 0.90 0 -8 7 1.20 0.60 0 8 8 2.80 0.90 0 8 8 3.60 1.30 0 8 -8 3.00 0.50 0 -8 8 2.70 1.10 0 8 9 2.00 0.70 0 8 -9 0.90 0.30 0 -8 9 1.20 0.70 0 9 0 0.50 0.40 0 -9 0 1.00 0.50 0 9 -1 44.30 2.30 0 9 1 44.00 2.30 0 -9 -1 40.70 2.50 0 -9 1 43.90 2.50 0 9 2 97.89 4.60 0 9 -2 93.29 4.20 0 9 -2 97.69 4.60 0 -9 -2 108.69 6.00 0 9 3 40.30 2.90 0 9 -3 44.50 2.70 0 9 -3 44.70 2.00 0 9 4 105.89 7.00 0 9 -4 124.69 5.20 0 -9 -4 128.19 5.60 0 -9 -4 120.79 5.60 0 9 5 68.59 3.20 0 -9 5 58.59 3.30 0 -9 -5 67.89 3.40 0 9 6 1.30 0.60 0 9 -6 1.30 0.30 0 -9 -6 1.50 0.80 0 -9 6 1.20 0.80 0 9 -7 70.09 3.30 0 9 7 77.39 3.60 0 -9 -7 81.39 3.80 0 -9 7 69.29 3.50 0 9 8 1.40 0.50 0 9 -8 1.70 0.30 0 9 8 0.80 0.50 0 -9 8 3.40 1.20 0 -9 -8 1.20 0.80 0 9 9 20.00 1.20 0 9 9 16.60 1.40 0 9 -9 22.40 1.00 0 10 0 6.50 1.20 0 10 1 4.10 1.30 0 10 -1 4.60 1.30 0 10 -2 133.89 5.70 0 10 2 135.59 6.20 0 10 -2 132.79 6.20 0 10 3 2.50 1.20 0 10 -3 2.10 1.00 0 -10 -3 3.50 0.90 0 10 -4 37.60 1.70 0 -10 -4 38.00 2.30 0 -10 -4 36.00 2.50 0 -10 -4 38.80 2.40 0 10 -5 23.70 1.20 0 10 6 7.90 1.10 0 10 -6 8.40 0.60 0 -10 6 6.20 1.80 0 -10 6 7.70 0.70 0 10 7 98.59 4.30 0 10 -7 86.79 4.00 0 -10 -7 96.59 4.50 0 -10 7 82.79 4.70 0 10 -8 3.50 0.40 0 10 8 3.90 0.90 0 10 8 4.90 0.90 0 -10 -8 4.30 1.40 0 10 9 0.60 0.40 0 10 -9 1.50 0.30 0 10 9 -0.80 0.60 0 11 0 -1.00 0.70 0 11 -1 41.50 2.70 0 11 1 39.80 2.70 0 11 2 120.29 6.90 0 11 -2 106.59 4.70 0 -11 -2 109.39 5.20 0 -11 2 105.99 4.80 0 11 -3 61.79 2.60 0 -11 -3 58.69 2.80 0 -11 3 59.99 2.70 0 -11 -3 59.69 3.10 0 -11 -3 52.09 3.60 0 11 -4 5.30 0.40 0 -11 4 4.50 0.60 0 -11 -4 5.40 1.20 0 -11 -4 5.20 1.50 0 11 -5 10.90 0.70 0 11 5 10.90 1.10 0 -11 -5 13.40 1.60 0 -11 5 9.30 0.70 0 11 6 1.00 0.60 0 11 -6 1.40 0.30 0 -11 -6 3.60 1.50 0 -11 6 1.70 0.60 0 11 7 1.10 0.60 0 11 -7 0.70 0.40 0 11 7 1.00 0.50 0 -11 -7 1.50 0.70 0 11 -8 7.90 0.50 0 11 8 7.10 0.90 0 11 8 6.20 0.80 0 -11 -8 8.50 1.30 0 11 -9 3.90 0.40 0 11 9 4.90 0.70 0 -12 0 420.66 17.80 0 -12 -1 5.30 1.40 0 -12 -1 4.30 1.00 0 -12 -1 5.90 0.70 0 -12 1 5.10 0.60 0 12 -2 1.50 0.40 0 -12 2 1.60 0.50 0 -12 -2 1.30 0.80 0 -12 -2 1.20 0.40 0 12 -3 37.50 1.60 0 -12 -3 33.00 1.90 0 -12 -3 35.80 2.30 0 -12 3 36.00 1.70 0 -12 -3 30.70 2.80 0 12 -4 -0.10 0.20 0 -12 4 0.00 0.30 0 -12 -4 0.10 0.70 0 -12 -4 -1.00 1.00 0 -12 -4 -1.30 1.10 0 12 -5 11.90 0.70 0 12 5 11.00 1.10 0 -12 5 9.50 0.70 0 -12 -5 13.80 2.20 0 -12 -5 10.70 1.60 0 12 6 0.30 0.50 0 12 -6 1.00 0.30 0 -12 -6 1.60 0.90 0 -12 6 1.90 0.50 0 12 7 30.70 2.50 0 12 7 30.00 1.80 0 12 -7 32.30 1.50 0 12 8 0.10 0.40 0 12 8 0.10 0.40 0 12 -8 -0.10 0.20 0 -12 -8 0.00 0.60 0 -13 0 5.30 2.00 0 -13 0 1.80 0.90 0 -13 -1 27.20 2.20 0 -13 1 20.80 3.90 0 -13 -1 28.00 1.80 0 -13 -1 28.50 1.40 0 -13 1 28.50 1.40 0 13 -2 7.40 0.60 0 -13 -2 7.10 0.90 0 -13 -2 5.40 1.60 0 -13 2 8.60 0.60 0 13 -3 0.50 0.20 0 -13 -3 -2.10 1.50 0 -13 -3 0.40 0.80 0 -13 -3 0.00 0.50 0 -13 3 -0.10 0.20 0 13 -4 28.70 1.40 0 -13 -4 29.00 2.00 0 -13 4 26.30 1.40 0 -13 -4 27.60 2.20 0 -13 -4 28.10 1.80 0 13 -5 0.00 0.30 0 13 5 -0.10 0.50 0 -13 -5 0.20 0.70 0 -13 -5 0.60 0.80 0 -13 5 0.60 0.20 0 13 -6 2.50 0.40 0 13 6 1.50 0.60 0 -13 -6 4.90 1.50 0 -13 6 2.30 0.50 0 13 7 0.10 0.50 0 13 -7 0.30 0.20 0 13 7 0.10 0.60 0 13 8 -0.60 0.50 0 13 -8 0.20 0.20 0 13 8 -0.20 0.40 0 -13 -8 -0.80 0.50 0 -14 0 88.99 4.20 0 -14 0 86.59 4.40 0 -14 0 87.29 3.90 0 -14 -1 9.50 0.70 0 -14 -1 8.90 1.80 0 -14 1 8.40 0.70 0 -14 1 4.60 1.80 0 -14 1 5.80 1.40 0 -14 -2 12.00 1.60 0 -14 2 10.80 0.70 0 -14 -2 11.80 1.00 0 14 -3 14.80 0.90 0 -14 -3 13.20 1.70 0 -14 -3 15.20 1.20 0 -14 3 15.40 0.90 0 14 4 45.50 2.30 0 14 -4 45.60 2.10 0 -14 -4 43.70 2.30 0 -14 4 42.50 2.10 0 -14 -4 48.40 2.60 0 14 5 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1 0.30 0.20 -10 -10 1 0.20 0.40 -10 -10 1 0.10 0.70 -10 -10 1 0.20 0.60 -10 10 0 2.90 0.80 -10 10 0 2.70 0.40 -10 -10 0 1.50 0.70 -10 -10 0 2.10 0.60 -10 10 -1 0.30 0.20 -10 10 -1 0.20 0.30 -10 -10 -1 -0.20 0.70 -10 -10 -1 -0.10 0.30 -10 -11 7 0.70 0.50 -10 -11 7 1.50 0.50 -10 11 6 0.20 0.30 -10 -11 6 0.10 0.50 -10 -11 6 -0.20 0.30 -10 11 5 3.40 0.50 -10 -11 5 4.70 0.60 -10 -11 5 4.70 0.80 -10 11 4 1.60 0.50 -10 -11 4 2.70 0.80 -10 -11 4 1.00 0.40 -10 11 3 0.50 0.20 -10 -11 3 -0.20 0.40 -10 -11 3 0.00 0.60 -10 11 2 -0.10 0.20 -10 -11 2 -0.30 0.40 -10 -11 2 -0.70 0.50 -10 11 1 0.00 0.40 -10 11 1 -0.30 0.20 -10 -11 1 -0.10 0.40 -10 -11 1 -0.60 0.60 -10 -11 1 -0.60 0.60 -10 11 0 4.40 0.40 -10 11 0 4.20 0.80 -10 -11 0 4.70 0.60 -10 -11 0 3.90 0.90 -10 11 -1 0.60 0.30 10 -11 1 1.30 0.40 -10 -11 -1 0.20 0.60 -10 -11 -1 1.50 0.40 -10 -12 7 12.60 0.80 -10 -12 7 11.60 0.90 -10 12 6 8.80 0.70 -10 -12 6 8.50 0.80 -10 -12 6 9.20 0.70 -10 12 5 0.50 0.30 10 -12 -5 -0.20 0.80 -10 -12 5 0.90 0.50 -10 -12 5 0.50 0.30 -10 12 4 15.80 0.90 -10 -12 4 16.40 1.10 -10 -12 4 16.00 1.00 -10 12 3 0.30 0.30 -10 -12 3 -0.50 0.40 -10 -12 3 0.10 0.50 -10 12 2 1.30 0.40 -10 -12 2 2.00 0.80 -10 -12 2 1.10 0.50 -10 12 1 0.50 0.20 -10 -12 1 0.10 0.60 -10 12 0 0.00 0.20 -10 -12 0 0.70 0.50 -10 -12 0 0.30 0.30 -10 -13 6 6.50 0.60 -10 13 5 0.70 0.30 10 -13 -5 1.00 0.80 -10 -13 5 1.10 0.60 -10 -13 5 2.10 0.50 -10 13 4 7.90 0.60 -10 -13 4 7.90 0.70 -10 -13 4 7.50 0.90 -10 13 3 0.20 0.30 -10 -13 3 0.40 0.50 -10 -13 3 0.30 0.40 -10 13 2 1.90 0.40 -10 -13 2 1.20 0.50 -10 -13 2 0.70 0.40 -10 13 1 0.10 0.20 -10 -13 1 -0.50 0.40 -10 -13 1 0.00 0.50 10 -14 -5 6.70 1.50 -10 -14 5 7.30 0.60 -10 -14 4 0.10 0.40 -10 -14 4 0.60 0.30 10 -14 -4 0.30 0.60 -10 14 3 0.80 0.30 -10 -14 3 1.60 0.70 -10 -14 3 0.50 0.40 -10 -14 2 10.60 0.80 -10 -14 2 11.00 0.90 -11 0 9 0.00 0.30 -11 0 8 19.10 1.10 -11 0 7 -0.60 0.30 -11 0 6 1.70 0.40 -11 0 6 2.80 0.50 -11 0 5 -0.10 0.30 -11 0 5 0.60 0.50 -11 0 4 14.10 0.90 -11 0 3 -0.40 0.40 -11 0 1 0.50 0.60 -11 0 0 18.20 1.10 -11 0 0 19.90 1.30 -11 0 -1 0.20 0.40 -11 0 -1 0.00 0.30 -11 1 9 0.30 0.30 -11 -1 9 0.70 0.20 11 -1 -9 0.80 0.30 -11 1 8 -0.30 0.30 -11 -1 8 -0.20 0.30 -11 1 7 0.80 0.40 -11 -1 7 0.30 0.40 -11 1 6 3.80 0.50 -11 1 6 3.20 0.80 -11 -1 6 3.40 0.70 -11 1 5 1.70 0.50 -11 -1 5 1.00 0.50 -11 -1 5 1.30 0.40 -11 1 4 3.90 0.60 -11 -1 4 3.70 0.70 -11 1 3 2.30 0.60 -11 1 2 1.00 0.80 -11 1 2 -0.40 0.40 -11 1 1 0.30 0.50 -11 -1 1 -0.20 0.60 -11 1 0 0.70 0.50 -11 1 0 0.70 0.40 -11 -1 0 0.60 0.50 -11 1 -1 4.70 0.80 -11 1 -1 3.90 0.60 -11 -1 -1 5.80 0.90 -11 -1 -1 5.20 0.60 -11 2 9 -0.20 0.30 -11 -2 9 -0.10 0.20 11 -2 -9 -0.10 0.30 11 2 -8 3.70 0.50 -11 2 8 3.20 0.60 -11 -2 8 3.00 0.60 -11 2 7 1.50 0.40 -11 -2 7 1.50 0.60 -11 2 6 -0.20 0.50 -11 2 6 0.00 0.30 -11 -2 6 -0.40 0.40 -11 2 5 9.60 0.70 -11 -2 5 10.90 1.00 -11 2 4 10.80 0.80 -11 2 3 0.80 0.30 -11 2 2 0.60 0.60 -11 2 2 0.90 0.40 -11 2 1 1.10 0.50 -11 -2 1 0.60 0.70 -11 2 0 0.40 0.40 -11 2 0 -0.10 0.40 -11 -2 0 -0.60 0.40 -11 -2 0 0.10 0.50 -11 2 -1 1.90 0.80 -11 2 -1 -0.10 0.30 -11 -2 -1 0.50 0.40 -11 -2 -1 0.00 0.30 -11 3 9 0.60 0.30 -11 -3 9 1.50 0.40 11 3 -8 0.50 0.30 -11 3 8 0.10 0.30 -11 -3 8 0.40 0.30 -11 3 7 1.20 0.40 -11 -3 7 1.90 0.60 -11 3 6 21.80 1.50 -11 3 6 21.60 1.20 -11 -3 6 23.40 1.20 -11 3 5 30.80 1.60 -11 -3 5 31.30 1.60 -11 3 4 0.30 0.30 -11 -3 4 -0.20 0.70 -11 3 3 4.20 0.50 -11 3 2 0.60 0.60 -11 3 2 0.50 0.30 -11 3 1 5.90 0.80 -11 3 1 7.30 1.10 -11 3 0 -0.10 0.40 -11 3 0 -0.40 0.40 -11 -3 0 0.20 0.40 -11 -3 0 -0.40 0.60 -11 3 -1 3.80 0.80 -11 3 -1 4.80 0.80 -11 -3 -1 5.10 0.60 -11 -3 -1 4.90 0.90 -11 4 8 2.80 0.60 -11 -4 8 3.30 0.50 -11 4 7 0.00 0.30 -11 4 7 -0.30 0.40 -11 -4 7 0.00 0.30 -11 4 6 3.80 0.50 -11 -4 6 2.80 0.60 -11 4 5 0.50 0.30 -11 -4 5 0.10 0.40 -11 4 4 -0.40 0.30 -11 -4 4 0.70 0.60 -11 4 3 10.70 2.10 -11 4 3 12.00 0.80 -11 4 2 1.10 0.60 -11 4 2 1.00 0.30 -11 4 1 14.10 0.90 -11 4 1 13.90 1.10 -11 -4 1 15.80 1.60 -11 4 0 3.20 0.70 -11 4 0 3.00 0.80 -11 4 0 2.10 0.80 -11 -4 0 2.10 0.60 -11 -4 0 1.50 0.60 -11 4 -1 10.30 0.90 -11 -4 -1 9.60 0.80 -11 -4 -1 7.80 1.10 -11 5 8 -0.30 0.40 -11 -5 8 0.30 0.30 -11 -5 8 0.90 0.90 -11 5 7 0.10 0.50 -11 5 7 -0.10 0.20 -11 -5 7 0.20 0.30 -11 -5 7 0.60 0.80 -11 5 6 54.49 2.60 -11 -5 6 57.19 2.50 -11 -5 6 53.79 2.80 -11 5 5 14.50 0.90 -11 -5 5 15.70 1.70 -11 -5 5 16.90 1.10 -11 5 4 0.00 0.30 -11 -5 4 -0.80 0.50 -11 5 3 -0.50 0.70 -11 5 3 0.10 0.30 -11 5 2 0.10 0.30 -11 5 2 -0.80 0.50 -11 5 1 10.90 0.70 -11 5 1 10.50 1.10 -11 -5 1 10.90 1.20 -11 5 0 0.90 0.40 -11 5 0 2.50 0.60 -11 -5 0 1.10 0.40 -11 5 -1 1.60 0.70 -11 -5 -1 1.90 0.50 -11 -6 8 10.90 0.70 -11 -6 8 9.50 1.20 -11 6 7 0.10 0.20 -11 -6 7 1.30 0.50 -11 -6 7 0.60 0.70 -11 6 6 0.50 0.20 -11 -6 6 0.60 0.30 -11 -6 6 0.20 0.70 -11 6 5 38.40 1.80 -11 -6 5 39.30 1.90 -11 -6 5 36.40 2.10 -11 6 4 0.80 0.30 -11 -6 4 0.90 0.50 -11 -6 4 -0.20 0.90 -11 6 3 0.30 0.30 -11 6 3 -0.60 0.70 -11 -6 3 -0.40 0.70 -11 6 2 2.80 1.00 -11 6 2 5.20 0.50 -11 6 1 3.40 0.50 -11 6 1 2.40 0.90 -11 -6 1 4.60 1.10 -11 6 0 10.00 0.90 -11 6 0 9.70 0.70 -11 -6 0 8.70 0.70 -11 6 -1 0.20 0.30 -11 -6 -1 0.10 0.30 -11 -7 8 0.50 0.20 -11 -7 8 0.10 0.60 -11 7 7 0.10 0.20 -11 -7 7 -0.10 0.30 -11 -7 7 -0.20 0.60 -11 7 6 0.90 0.30 -11 -7 6 0.50 0.70 -11 -7 6 0.80 0.30 -11 7 5 7.90 0.60 -11 -7 5 7.40 0.80 -11 -7 5 8.10 1.20 -11 7 4 2.20 0.40 -11 -7 4 1.10 0.40 -11 -7 4 1.30 0.80 -11 7 3 0.30 0.20 -11 7 3 1.30 0.60 -11 -7 3 0.00 0.80 -11 -7 3 -0.40 0.60 -11 7 2 -0.40 0.50 -11 7 2 0.00 0.40 -11 -7 2 -1.00 1.00 -11 7 1 -0.30 0.30 -11 7 1 -0.10 0.40 -11 7 0 -0.10 0.30 -11 7 0 -0.30 0.40 -11 -7 0 0.20 0.40 -11 7 -1 -0.10 0.40 -11 8 7 0.90 0.30 -11 -8 7 0.20 0.90 -11 -8 7 0.80 0.30 -11 8 6 2.00 0.40 -11 -8 6 3.00 0.60 -11 8 5 0.20 0.30 -11 -8 5 0.00 0.40 -11 -8 5 0.40 0.60 -11 8 4 0.60 0.30 -11 -8 4 -0.40 0.40 -11 -8 4 0.30 0.70 -11 8 3 0.10 0.30 -11 -8 3 0.30 0.70 -11 -8 3 0.50 0.60 -11 8 2 0.40 0.50 -11 8 2 0.70 0.30 -11 -8 2 -1.40 0.80 -11 8 1 -0.20 0.40 -11 8 1 0.10 0.20 -11 -8 1 2.20 0.90 -11 8 0 0.10 0.30 -11 8 0 -0.40 0.30 -11 -8 0 -0.20 0.40 -11 -9 7 0.00 0.50 -11 -9 7 0.90 0.30 -11 9 6 1.10 0.40 -11 -9 6 0.20 0.60 -11 -9 6 1.60 0.60 -11 -9 5 0.60 0.30 -11 -9 5 3.10 1.00 -11 9 4 0.00 0.30 -11 -9 4 -0.40 0.60 -11 -9 4 -0.20 0.40 -11 9 3 0.00 0.20 -11 -9 3 0.00 0.60 -11 -9 3 -0.30 0.50 -11 9 2 0.70 0.50 -11 9 2 -0.20 0.30 -11 -9 2 -1.10 0.80 -11 9 1 0.60 0.30 -11 -9 1 3.30 1.20 -11 9 0 -0.40 0.30 -11 -9 0 0.00 0.40 -11 10 6 5.20 0.50 -11 -10 6 5.40 0.80 -11 -10 6 5.70 0.60 -11 10 5 0.90 0.30 -11 -10 5 0.90 0.30 -11 -10 5 2.80 0.90 -11 10 4 0.20 0.20 -11 -10 4 0.30 0.60 -11 -10 4 0.40 0.40 -11 10 3 0.50 0.20 -11 -10 3 -0.10 0.60 -11 -10 3 0.10 0.50 -11 -10 2 1.20 0.70 -11 10 1 1.40 0.40 -11 -10 1 3.20 1.10 -11 -11 6 0.90 0.40 -11 -11 6 0.70 0.50 -11 11 5 0.20 0.30 -11 -11 5 -0.30 0.50 -11 -11 5 0.00 0.30 -11 11 4 0.20 0.30 -11 -11 4 -0.10 0.40 -11 -11 4 0.90 0.50 -11 11 3 0.30 0.20 -11 -11 3 -0.10 0.50 -11 -11 3 -0.40 0.50 -11 11 2 -0.30 0.30 -11 -11 2 -0.50 0.60 -11 12 4 0.30 0.50 -11 -12 4 -0.60 0.50 -11 -12 4 0.40 0.40 11 -12 -4 -1.10 0.80 -11 12 3 1.70 0.60 -11 -12 3 1.10 0.50 -11 -12 3 0.80 0.40 -12 0 8 1.10 0.40 -12 0 0 1.50 0.60 -12 1 8 1.50 0.40 -12 -1 8 1.30 0.30 -12 -1 7 0.80 0.40 -12 1 5 0.40 0.40 -12 1 4 62.39 2.90 -12 1 1 0.30 1.20 -12 1 0 6.80 1.10 -12 -2 7 1.40 0.40 -12 -2 6 0.00 0.80 -12 2 5 0.10 0.30 -12 2 4 0.70 0.40 -12 2 1 4.50 1.20 -12 2 0 1.20 0.50 -12 -3 7 0.40 0.40 -12 3 6 33.80 1.70 -12 -3 6 36.00 1.80 -12 3 5 0.30 0.30 -12 3 4 3.70 0.60 -12 3 3 2.60 0.70 -12 3 1 -0.90 0.50 -12 -4 7 0.20 0.40 -12 4 6 18.60 1.00 -12 -4 6 21.30 1.30 -12 4 5 0.20 0.30 -12 4 4 3.30 0.50 -12 4 3 -0.60 0.30 -12 4 2 -1.00 1.30 -12 4 1 0.30 0.50 -12 -5 7 -0.20 0.30 -12 5 6 3.80 0.50 -12 -5 6 5.30 1.10 -12 5 5 3.90 0.50 -12 5 4 2.80 0.50 -12 5 3 -0.20 0.30 -12 5 2 3.30 0.80 -12 5 1 3.20 1.00 -12 6 6 1.60 0.40 -12 -6 6 2.90 0.70 -12 6 5 0.30 0.30 -12 -6 5 -0.20 0.50 -12 6 4 0.90 0.30 -12 6 3 0.90 0.30 -12 6 1 0.70 0.50 -12 7 6 0.30 0.30 -12 -7 6 0.10 0.40 -12 7 5 0.10 0.30 -12 -7 5 0.50 0.50 -12 7 4 0.60 0.30 -12 7 3 0.40 0.30 -12 8 5 1.40 0.40 -12 -8 5 0.40 0.50 -12 8 4 0.00 0.30 -12 8 3 0.70 0.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65949 _shelx_res_file ; TITL JTM1248_0ma_a.res in P2(1)/c JTM1248_0ma_a.res created by SHELXL-2018/3 at 10:46:21 on 25-Apr-2020 REM Old TITL JTM1248_0ma in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.217, Rweak 0.006, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C21 N4 O3 CELL 1.54178 10.8398 19.0207 9.3307 90.000 112.378 90.000 ZERR 8.000 0.0007 0.0011 0.0005 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H F N O UNIT 64 56 8 32 8 TEMP 23 SIZE 0.146 0.246 0.466 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 MPLA C1 > C6 MPLA N1 C7 C8 O1 MPLA C8 N2 N3 N4 MPLA C9 > C14 MPLA N5 C15 C16 O2 MPLA C16 N6 N7 N8 EQIV $1 x, -y+1/2, z+1/2 HTAB N1 O1_$1 EQIV $2 x, -y+1/2, z-1/2 HTAB N5 O2_$1 CONF ACTA 136 WGHT 0.082800 0.471800 EXTI 0.003314 FVAR 0.57554 F1 3 0.754496 0.519341 0.550634 11.00000 0.09035 0.07057 = 0.13341 0.01032 0.01853 -0.02640 O1 5 0.376278 0.278653 0.118566 11.00000 0.09942 0.07501 = 0.04954 -0.00793 0.04277 -0.00528 N1 4 0.388537 0.304472 0.361107 11.00000 0.05956 0.06526 = 0.04109 -0.00501 0.02751 -0.00575 AFIX 43 H1 2 0.357573 0.292390 0.429765 11.00000 -1.20000 AFIX 0 N2 4 0.237919 0.157681 0.111846 11.00000 0.06940 0.08487 = 0.07388 -0.02726 0.02084 0.00081 N3 4 0.140606 0.157964 -0.009735 11.00000 0.07806 0.07767 = 0.05169 -0.00566 0.03095 0.00524 N4 4 0.058694 0.150580 -0.123812 11.00000 0.11177 0.15983 = 0.06149 -0.02810 0.00552 0.04378 C1 1 0.481070 0.360203 0.401968 11.00000 0.05072 0.05417 = 0.04837 -0.00032 0.02466 0.00433 C2 1 0.506483 0.402012 0.294286 11.00000 0.06844 0.06635 = 0.05345 0.00793 0.02762 0.00301 AFIX 43 H2 2 0.461604 0.394037 0.188729 11.00000 -1.20000 AFIX 0 C3 1 0.599376 0.455730 0.345679 11.00000 0.07628 0.06144 = 0.08731 0.01976 0.03959 0.00250 AFIX 43 H3 2 0.617810 0.483972 0.274916 11.00000 -1.20000 AFIX 0 C4 1 0.663737 0.466853 0.501459 11.00000 0.05888 0.05354 = 0.08966 0.00518 0.01858 -0.00224 C5 1 0.638298 0.427869 0.609226 11.00000 0.06462 0.06367 = 0.06520 -0.00361 0.01464 -0.00301 AFIX 43 H5 2 0.681609 0.437309 0.714400 11.00000 -1.20000 AFIX 0 C6 1 0.547067 0.374192 0.559001 11.00000 0.06212 0.06205 = 0.04836 -0.00082 0.02306 -0.00261 AFIX 43 H6 2 0.529166 0.346752 0.631306 11.00000 -1.20000 AFIX 0 C7 1 0.342773 0.267900 0.227966 11.00000 0.05679 0.05935 = 0.04289 -0.00326 0.02340 0.00795 C8 1 0.241705 0.212213 0.222793 11.00000 0.06508 0.07393 = 0.06200 -0.01867 0.02915 -0.00805 AFIX 23 H8A 2 0.265262 0.191575 0.324847 11.00000 -1.20000 H8AB 2 0.154166 0.233482 0.193244 11.00000 -1.20000 AFIX 0 F2 3 1.234436 0.518177 0.984495 11.00000 0.13017 0.12543 = 0.17381 -0.04894 0.05572 -0.07110 O2 5 0.862297 0.277974 0.551423 11.00000 0.10834 0.07838 = 0.06232 -0.01355 0.05607 -0.02010 N5 4 0.871049 0.302196 0.792964 11.00000 0.06327 0.06318 = 0.04366 0.00178 0.02756 -0.00137 AFIX 43 H5A 2 0.839332 0.289670 0.860681 11.00000 -1.20000 AFIX 0 N6 4 0.670440 0.183850 0.491839 11.00000 0.11681 0.10214 = 0.06105 -0.02252 0.04529 -0.03853 N7 4 0.584678 0.140009 0.465387 11.00000 0.07648 0.07879 = 0.05015 -0.01031 0.02915 -0.00184 N8 4 0.501927 0.100610 0.421475 11.00000 0.09057 0.12309 = 0.07123 -0.03071 0.03002 -0.02314 C9 1 0.963408 0.358141 0.835438 11.00000 0.05299 0.05706 = 0.05377 -0.00168 0.02385 0.00494 C10 1 0.988134 0.400315 0.728293 11.00000 0.06907 0.06548 = 0.06545 0.00067 0.03338 -0.00184 AFIX 43 H10 2 0.943298 0.392439 0.622692 11.00000 -1.20000 AFIX 0 C11 1 1.080061 0.454206 0.779804 11.00000 0.08707 0.07081 = 0.10558 -0.00032 0.05381 -0.01010 AFIX 43 H11 2 1.098105 0.482845 0.709361 11.00000 -1.20000 AFIX 0 C12 1 1.144454 0.464927 0.936441 11.00000 0.07793 0.08065 = 0.11244 -0.02508 0.03512 -0.02165 C13 1 1.119524 0.425281 1.043462 11.00000 0.08634 0.09584 = 0.07740 -0.01998 0.01809 -0.01338 AFIX 43 H13 2 1.162906 0.434404 1.148769 11.00000 -1.20000 AFIX 0 C14 1 1.029184 0.371630 0.992915 11.00000 0.07504 0.07624 = 0.05783 -0.00456 0.02005 -0.00355 AFIX 43 H14 2 1.011492 0.343792 1.064795 11.00000 -1.20000 AFIX 0 C15 1 0.826969 0.266277 0.659219 11.00000 0.06152 0.05797 = 0.04718 0.00040 0.02620 0.00294 C16 1 0.731255 0.207747 0.652973 11.00000 0.07174 0.07216 = 0.05025 -0.00078 0.02702 -0.00771 AFIX 23 H16A 2 0.778421 0.169287 0.719587 11.00000 -1.20000 H16B 2 0.662987 0.224593 0.687969 11.00000 -1.20000 AFIX 0 HKLF 4 REM JTM1248_0ma_a.res in P2(1)/c REM wR2 = 0.162191, GooF = S = 1.05842, Restrained GooF = 1.05842 for all data REM R1 = 0.053288 for 2545 Fo > 4sig(Fo) and 0.064986 for all 3224 data REM 254 parameters refined using 0 restraints END WGHT 0.0827 0.4717 REM Highest difference peak 0.446, deepest hole -0.237, 1-sigma level 0.038 Q1 1 0.7360 0.1539 0.5833 11.00000 0.05 0.45 Q2 1 0.1932 0.2028 0.0279 11.00000 0.05 0.30 Q3 1 0.0394 0.1134 -0.0662 11.00000 0.05 0.19 Q4 1 0.6952 0.5286 0.4453 11.00000 0.05 0.15 Q5 1 0.7286 0.1975 0.7402 11.00000 0.05 0.15 ; _shelx_res_checksum 94882 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 F F1 0.75450(16) 0.51934(8) 0.5506(2) 0.1053(6) Uani d 1 . . O O1 0.37628(16) 0.27865(8) 0.11857(16) 0.0704(5) Uani d 1 . . N N1 0.38854(15) 0.30447(8) 0.36111(17) 0.0528(4) Uani d 1 . . H H1 0.357573 0.292390 0.429765 0.063 Uiso calc 1 . . N N2 0.23792(19) 0.15768(11) 0.1118(2) 0.0780(6) Uani d 1 . . N N3 0.1406(2) 0.15796(10) -0.0097(2) 0.0673(5) Uani d 1 . . N N4 0.0587(3) 0.15058(17) -0.1238(3) 0.1192(11) Uani d 1 . . C C1 0.48107(18) 0.36020(10) 0.4020(2) 0.0494(4) Uani d 1 . . C C2 0.5065(2) 0.40201(11) 0.2943(2) 0.0614(5) Uani d 1 . . H H2 0.461604 0.394037 0.188729 0.074 Uiso calc 1 . . C C3 0.5994(2) 0.45573(12) 0.3457(3) 0.0725(6) Uani d 1 . . H H3 0.617810 0.483972 0.274916 0.087 Uiso calc 1 . . C C4 0.6637(2) 0.46685(11) 0.5015(3) 0.0702(6) Uani d 1 . . C C5 0.6383(2) 0.42787(12) 0.6092(3) 0.0675(6) Uani d 1 . . H H5 0.681609 0.437309 0.714400 0.081 Uiso calc 1 . . C C6 0.54707(19) 0.37419(11) 0.5590(2) 0.0569(5) Uani d 1 . . H H6 0.529166 0.346752 0.631306 0.068 Uiso calc 1 . . C C7 0.34277(18) 0.26790(10) 0.2280(2) 0.0517(5) Uani d 1 . . C C8 0.2417(2) 0.21221(12) 0.2228(3) 0.0655(6) Uani d 1 . . H H8A 0.265262 0.191575 0.324847 0.079 Uiso calc 1 . . H H8B 0.154166 0.233482 0.193244 0.079 Uiso calc 1 . . F F2 1.2344(2) 0.51818(12) 0.9845(3) 0.1438(9) Uani d 1 . . O O2 0.86230(17) 0.27797(9) 0.55142(18) 0.0760(5) Uani d 1 . . N N5 0.87105(16) 0.30220(9) 0.79296(17) 0.0546(4) Uani d 1 . . H H5A 0.839332 0.289670 0.860681 0.065 Uiso calc 1 . . N N6 0.6704(2) 0.18385(13) 0.4918(2) 0.0899(7) Uani d 1 . . N N7 0.5847(2) 0.14001(11) 0.4654(2) 0.0670(5) Uani d 1 . . N N8 0.5019(2) 0.10061(15) 0.4215(3) 0.0952(8) Uani d 1 . . C C9 0.96341(19) 0.35814(10) 0.8354(2) 0.0536(5) Uani d 1 . . C C10 0.9881(2) 0.40031(12) 0.7283(3) 0.0644(5) Uani d 1 . . H H10 0.943298 0.392439 0.622692 0.077 Uiso calc 1 . . C C11 1.0801(3) 0.45421(14) 0.7798(4) 0.0827(7) Uani d 1 . . H H11 1.098105 0.482845 0.709361 0.099 Uiso calc 1 . . C C12 1.1445(3) 0.46493(15) 0.9364(4) 0.0907(8) Uani d 1 . . C C13 1.1195(3) 0.42528(16) 1.0435(3) 0.0904(8) Uani d 1 . . H H13 1.162906 0.434404 1.148769 0.108 Uiso calc 1 . . C C14 1.0292(2) 0.37163(13) 0.9929(3) 0.0713(6) Uani d 1 . . H H14 1.011492 0.343792 1.064795 0.086 Uiso calc 1 . . C C15 0.82697(19) 0.26628(10) 0.6592(2) 0.0539(5) Uani d 1 . . C C16 0.7313(2) 0.20775(12) 0.6530(2) 0.0636(5) Uani d 1 . . H H16A 0.778421 0.169287 0.719587 0.076 Uiso calc 1 . . H H16B 0.662987 0.224593 0.687969 0.076 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 F1 0.0904(10) 0.0706(9) 0.1334(15) -0.0264(8) 0.0185(10) 0.0103(9) O1 0.0994(11) 0.0750(10) 0.0495(8) -0.0053(8) 0.0428(8) -0.0079(7) N1 0.0596(9) 0.0653(10) 0.0411(8) -0.0057(7) 0.0275(7) -0.0050(7) N2 0.0694(11) 0.0849(14) 0.0739(13) 0.0008(10) 0.0208(10) -0.0273(10) N3 0.0781(12) 0.0777(12) 0.0517(11) 0.0052(9) 0.0310(10) -0.0057(8) N4 0.1118(19) 0.160(3) 0.0615(14) 0.0438(19) 0.0055(14) -0.0281(15) C1 0.0507(10) 0.0542(10) 0.0484(9) 0.0043(8) 0.0247(8) -0.0003(8) C2 0.0684(12) 0.0663(13) 0.0534(11) 0.0030(10) 0.0276(9) 0.0079(9) C3 0.0763(14) 0.0614(13) 0.0873(16) 0.0025(11) 0.0396(13) 0.0198(11) C4 0.0589(12) 0.0535(12) 0.0897(17) -0.0022(9) 0.0186(11) 0.0052(11) C5 0.0646(12) 0.0637(13) 0.0652(13) -0.0030(10) 0.0146(10) -0.0036(10) C6 0.0621(11) 0.0621(12) 0.0484(10) -0.0026(9) 0.0231(9) -0.0008(8) C7 0.0568(10) 0.0593(11) 0.0429(9) 0.0079(8) 0.0234(8) -0.0033(8) C8 0.0651(12) 0.0739(13) 0.0620(12) -0.0080(10) 0.0292(10) -0.0187(10) F2 0.1302(15) 0.1254(16) 0.174(2) -0.0711(13) 0.0557(15) -0.0489(15) O2 0.1083(13) 0.0784(10) 0.0623(9) -0.0201(9) 0.0561(9) -0.0135(7) N5 0.0633(10) 0.0632(10) 0.0437(8) -0.0014(7) 0.0276(7) 0.0018(7) N6 0.1168(17) 0.1021(17) 0.0610(12) -0.0385(14) 0.0453(12) -0.0225(11) N7 0.0765(12) 0.0788(12) 0.0501(9) -0.0018(11) 0.0292(9) -0.0103(9) N8 0.0906(15) 0.123(2) 0.0712(13) -0.0231(15) 0.0300(12) -0.0307(13) C9 0.0530(10) 0.0571(11) 0.0538(10) 0.0049(8) 0.0239(8) -0.0017(8) C10 0.0691(13) 0.0655(13) 0.0654(13) -0.0018(10) 0.0334(10) 0.0007(10) C11 0.0871(17) 0.0708(15) 0.106(2) -0.0101(13) 0.0538(16) -0.0003(14) C12 0.0779(16) 0.0806(18) 0.112(2) -0.0217(13) 0.0351(16) -0.0251(16) C13 0.0863(17) 0.096(2) 0.0774(17) -0.0134(15) 0.0181(14) -0.0200(15) C14 0.0750(14) 0.0762(15) 0.0578(12) -0.0036(11) 0.0201(10) -0.0046(11) C15 0.0615(11) 0.0580(11) 0.0472(10) 0.0029(8) 0.0262(9) 0.0004(8) C16 0.0717(13) 0.0722(13) 0.0502(11) -0.0077(10) 0.0270(9) -0.0008(9) 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' F F 0.0727 0.0534 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 N1 C1 . . 127.90(16) ? C7 N1 H1 . . 116.0 ? C1 N1 H1 . . 116.0 ? N3 N2 C8 . . 116.02(19) ? N4 N3 N2 . . 171.2(3) ? C2 C1 C6 . . 119.27(18) ? C2 C1 N1 . . 123.51(17) ? C6 C1 N1 . . 117.20(17) ? C3 C2 C1 . . 119.3(2) ? C3 C2 H2 . . 120.3 ? C1 C2 H2 . . 120.3 ? C4 C3 C2 . . 119.4(2) ? C4 C3 H3 . . 120.3 ? C2 C3 H3 . . 120.3 ? F1 C4 C5 . . 118.5(2) ? F1 C4 C3 . . 119.0(2) ? C5 C4 C3 . . 122.4(2) ? C4 C5 C6 . . 118.4(2) ? C4 C5 H5 . . 120.8 ? C6 C5 H5 . . 120.8 ? C5 C6 C1 . . 121.11(19) ? C5 C6 H6 . . 119.4 ? C1 C6 H6 . . 119.4 ? O1 C7 N1 . . 124.23(19) ? O1 C7 C8 . . 122.15(17) ? N1 C7 C8 . . 113.61(16) ? N2 C8 C7 . . 110.25(17) ? N2 C8 H8A . . 109.6 ? C7 C8 H8A . . 109.6 ? N2 C8 H8B . . 109.6 ? C7 C8 H8B . . 109.6 ? H8A C8 H8B . . 108.1 ? C15 N5 C9 . . 127.53(16) ? C15 N5 H5A . . 116.2 ? C9 N5 H5A . . 116.2 ? N7 N6 C16 . . 115.87(19) ? N8 N7 N6 . . 171.2(2) ? C10 C9 C14 . . 119.6(2) ? C10 C9 N5 . . 123.08(18) ? C14 C9 N5 . . 117.35(18) ? C11 C10 C9 . . 119.4(2) ? C11 C10 H10 . . 120.3 ? C9 C10 H10 . . 120.3 ? C12 C11 C10 . . 119.1(3) ? C12 C11 H11 . . 120.4 ? C10 C11 H11 . . 120.4 ? C13 C12 F2 . . 119.4(3) ? C13 C12 C11 . . 122.5(2) ? F2 C12 C11 . . 118.2(3) ? C12 C13 C14 . . 118.5(3) ? C12 C13 H13 . . 120.7 ? C14 C13 H13 . . 120.7 ? C13 C14 C9 . . 120.9(2) ? C13 C14 H14 . . 119.6 ? C9 C14 H14 . . 119.6 ? O2 C15 N5 . . 124.02(19) ? O2 C15 C16 . . 121.86(18) ? N5 C15 C16 . . 114.10(16) ? N6 C16 C15 . . 107.63(17) ? N6 C16 H16A . . 110.2 ? C15 C16 H16A . . 110.2 ? N6 C16 H16B . . 110.2 ? C15 C16 H16B . . 110.2 ? H16A C16 H16B . . 108.5 ? 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 F1 C4 . 1.353(3) ? O1 C7 . 1.224(2) ? N1 C7 . 1.343(2) ? N1 C1 . 1.409(2) ? N1 H1 . 0.8600 ? N2 N3 . 1.220(3) ? N2 C8 . 1.455(3) ? N3 N4 . 1.105(3) ? C1 C2 . 1.389(3) ? C1 C6 . 1.390(3) ? C2 C3 . 1.386(3) ? C2 H2 . 0.9300 ? C3 C4 . 1.368(4) ? C3 H3 . 0.9300 ? C4 C5 . 1.359(3) ? C5 C6 . 1.374(3) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? C7 C8 . 1.511(3) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? F2 C12 . 1.358(3) ? O2 C15 . 1.225(2) ? N5 C15 . 1.341(2) ? N5 C9 . 1.411(3) ? N5 H5A . 0.8600 ? N6 N7 . 1.202(3) ? N6 C16 . 1.465(3) ? N7 N8 . 1.120(3) ? C9 C10 . 1.385(3) ? C9 C14 . 1.391(3) ? C10 C11 . 1.382(3) ? C10 H10 . 0.9300 ? C11 C12 . 1.374(4) ? C11 H11 . 0.9300 ? C12 C13 . 1.358(4) ? C13 C14 . 1.368(4) ? C13 H13 . 0.9300 ? C14 H14 . 0.9300 ? C15 C16 . 1.508(3) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? 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 O1 4_566 0.86 2.17 2.921(2) 146 yes N5 H5A O2 4_566 0.86 2.13 2.885(2) 146 yes C4 F1 Cg1 3_666 1.353(3) 3.755(3) 3.563(2) 71.45(2) y C12 F2 Cg2 3_767 1.358(3) 3.983(3) 3.942(2) 78.45(18) y 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 C7 N1 C1 C2 . . . . 22.8(3) ? C7 N1 C1 C6 . . . . -158.76(19) ? C6 C1 C2 C3 . . . . 1.5(3) ? N1 C1 C2 C3 . . . . 179.95(18) ? C1 C2 C3 C4 . . . . -0.4(3) ? C2 C3 C4 F1 . . . . 179.9(2) ? C2 C3 C4 C5 . . . . -1.3(4) ? F1 C4 C5 C6 . . . . -179.38(19) ? C3 C4 C5 C6 . . . . 1.8(4) ? C4 C5 C6 C1 . . . . -0.6(3) ? C2 C1 C6 C5 . . . . -1.0(3) ? N1 C1 C6 C5 . . . . -179.57(18) ? C1 N1 C7 O1 . . . . -0.3(3) ? C1 N1 C7 C8 . . . . -178.95(18) ? N3 N2 C8 C7 . . . . -106.1(2) ? O1 C7 C8 N2 . . . . 24.7(3) ? N1 C7 C8 N2 . . . . -156.63(18) ? C15 N5 C9 C10 . . . . 23.2(3) ? C15 N5 C9 C14 . . . . -158.3(2) ? C14 C9 C10 C11 . . . . 1.4(3) ? N5 C9 C10 C11 . . . . 179.8(2) ? C9 C10 C11 C12 . . . . -0.3(4) ? C10 C11 C12 C13 . . . . -1.2(5) ? C10 C11 C12 F2 . . . . 180.0(2) ? F2 C12 C13 C14 . . . . -179.6(3) ? C11 C12 C13 C14 . . . . 1.6(5) ? C12 C13 C14 C9 . . . . -0.5(4) ? C10 C9 C14 C13 . . . . -1.0(4) ? N5 C9 C14 C13 . . . . -179.5(2) ? C9 N5 C15 O2 . . . . -0.3(3) ? C9 N5 C15 C16 . . . . 178.13(18) ? N7 N6 C16 C15 . . . . -175.4(2) ? O2 C15 C16 N6 . . . . -13.6(3) ? N5 C15 C16 N6 . . . . 168.00(19) ? _cod_database_fobs_code 2244138