#------------------------------------------------------------------------------ #$Date: 2025-01-11 04:21:54 +0200 (Sat, 11 Jan 2025) $ #$Revision: 297283 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312738.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_2312738 loop_ _publ_author_name 'Hollenwäger, Dirk' 'Leitz, Dominik' 'Bockmair, Valentin' 'Kornath, Andreas J.' _publ_section_title ; Monoprotonated species of 2-aminomalonyl difluoride, [C3H4F2NO2][H2F3]. ; _journal_coeditor_code OJ3024 _journal_issue 2 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229624012452 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C3 H3 F2 N O2 +, H2 F3 -' _chemical_formula_moiety 'C3 H3 F2 N O2 +, H2 F3 -' _chemical_formula_sum 'C3 H6 F5 N O2' _chemical_formula_weight 183.09 _chemical_name_systematic ; 1,3-Difluoro-1,3-dioxopropan-2-aminium dihydrogen trifluoride ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.5736(2) _cell_length_b 9.2154(4) _cell_length_c 12.7952(7) _cell_measurement_reflns_used 2040 _cell_measurement_temperature 102(2) _cell_measurement_theta_max 31.1830 _cell_measurement_theta_min 2.7220 _cell_volume 657.20(5) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2020) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2020) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2020) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2019 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 102(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9809 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Rigaku Xcalibur Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7118 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.302 _diffrn_reflns_theta_min 2.724 _diffrn_source_current 40 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2020) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.338 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.072 _refine_diff_density_max 0.273 _refine_diff_density_min -0.181 _refine_ls_abs_structure_details ; Flack x determined using 683 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.3(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 2187 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0338 _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^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.0668 _reflns_number_gt 1930 _reflns_number_total 2187 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file oj3024.cif _cod_data_source_block I _cod_database_code 2312738 _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 0.926 _shelx_estimated_absorpt_t_max 0.984 _shelx_hkl_file ; 0 0 -1 0.09 0.45 0 0 -2 187.79 5.55 0 0 -3 -0.18 1.57 0 0 -4 2618.07 29.21 0 0 -5 2.45 2.40 0 0 -6 707.05 18.92 0 0 -7 3.75 2.41 0 0 -8 782.33 23.51 0 0 -9 -5.85 3.08 0 0 -10 0.92 3.00 0 0 -11 8.56 4.44 0 0 -12 50.83 8.17 0 0 -13 -0.19 3.21 0 0 -14 7.09 3.35 0 0 -14 15.10 5.56 0 0 -15 13.17 6.17 0 0 -15 13.90 4.86 0 0 -16 277.40 21.42 0 0 -17 -3.06 3.69 0 0 18 6.64 4.57 0 0 -18 -8.65 6.04 0 1 0 0.69 0.72 0 -1 0 0.10 0.66 0 -1 -1 452.22 7.87 0 1 1 418.99 7.63 0 1 -2 2003.97 14.81 0 1 -2 1961.73 12.69 0 -1 -2 2039.01 19.90 0 1 2 1982.87 19.63 0 -1 -3 37.16 2.37 0 -1 -3 40.95 3.86 0 1 -3 37.87 2.53 0 1 -3 36.82 2.58 0 -1 -4 237.39 6.37 0 1 -4 225.23 6.79 0 -1 -4 238.70 9.28 0 -1 -5 1130.59 15.06 0 -1 -5 1173.37 22.50 0 1 -5 1135.33 16.94 0 1 -6 844.38 16.01 0 -1 -6 934.32 22.04 0 1 -7 4248.02 50.56 0 -1 -7 4244.26 50.34 0 1 -8 65.16 7.22 0 -1 -8 58.90 6.79 0 -1 -9 650.13 22.71 0 1 -9 653.21 22.93 0 -1 -10 102.97 10.37 0 1 -10 123.22 10.85 0 1 -11 49.56 7.70 0 -1 -11 32.31 6.15 0 1 -11 37.50 5.38 0 -1 -12 12.63 4.84 0 1 -12 18.81 4.96 0 1 -12 13.01 3.86 0 1 -13 4.25 3.79 0 -1 -13 12.02 5.63 0 1 -13 13.06 3.91 0 1 -14 14.07 4.20 0 -1 -14 11.66 5.09 0 1 -14 14.26 5.78 0 1 -15 29.10 7.37 0 1 15 22.28 7.04 0 -1 -15 29.06 7.59 0 -1 -16 116.24 14.26 0 -1 -16 114.72 12.84 0 1 16 106.28 13.37 0 1 -16 104.19 13.65 0 1 17 85.31 12.42 0 1 -17 91.68 13.47 0 -1 -17 115.42 14.65 0 -1 -18 0.65 3.51 0 1 -18 -3.23 4.19 0 1 18 4.95 5.25 0 2 0 1640.53 19.25 0 -2 0 1632.09 19.33 0 -2 -1 1414.26 18.51 0 2 1 1426.09 18.62 0 2 -1 1396.32 17.14 0 -2 1 1416.13 18.92 0 2 -2 17.79 2.24 0 2 2 28.38 3.45 0 -2 -2 18.62 2.93 0 2 -3 158.75 4.18 0 2 3 159.27 7.53 0 -2 -3 160.18 7.66 0 2 -3 154.91 5.63 0 -2 -4 421.08 13.15 0 2 4 419.93 13.13 0 2 -4 399.92 8.06 0 2 -4 397.69 9.52 0 -2 -5 26.34 4.04 0 2 -5 27.30 2.68 0 2 -5 24.14 2.75 0 2 5 24.93 3.92 0 -2 -5 19.60 2.57 0 2 6 284.16 12.71 0 2 -6 267.51 9.02 0 -2 -6 266.02 8.72 0 2 -6 276.69 9.00 0 -2 -6 275.39 12.33 0 -2 -7 997.29 17.46 0 2 -7 995.67 19.16 0 2 7 1061.64 25.94 0 2 -7 992.84 18.64 0 -2 -7 1026.30 25.75 0 -2 -8 172.55 7.57 0 2 -8 169.52 8.67 0 -2 -8 177.76 11.69 0 2 -8 163.30 8.16 0 2 8 171.59 11.47 0 2 9 -0.87 3.08 0 2 -9 2.70 1.91 0 -2 -9 -2.56 2.57 0 2 -10 471.31 21.38 0 2 -10 445.02 16.03 0 2 10 467.67 20.98 0 -2 -10 472.22 20.91 0 2 -11 9.20 2.85 0 2 -11 0.64 2.93 0 2 11 3.87 3.34 0 -2 -11 3.87 3.42 0 2 -12 -0.42 3.67 0 -2 -12 6.36 4.36 0 2 -12 -0.10 1.75 0 2 12 -0.60 3.18 0 -2 -13 54.30 8.84 0 2 13 65.66 9.70 0 2 -13 60.54 9.45 0 2 14 76.40 10.63 0 2 -14 72.53 10.70 0 -2 -14 82.57 11.10 0 2 -15 2.16 3.25 0 -2 -15 3.85 3.80 0 2 15 4.92 3.46 0 -2 -16 30.83 8.05 0 2 -16 26.87 7.82 0 2 16 35.13 8.32 0 -2 -17 107.18 14.24 0 2 17 152.27 16.63 0 -2 -17 140.96 15.43 0 2 -17 133.32 15.94 0 -2 -18 15.82 5.79 0 2 -18 15.65 6.12 0 2 18 18.44 7.15 0 -2 -18 13.70 5.67 0 -3 0 3.96 2.43 0 3 0 -1.87 2.77 0 3 -1 2428.14 27.75 0 -3 1 2482.86 30.01 0 3 1 2459.30 30.03 0 -3 -1 2463.89 29.47 0 -3 -2 1355.53 22.97 0 3 2 1395.97 23.21 0 -3 2 1407.13 23.33 0 3 3 5.26 2.90 0 3 -3 9.05 2.21 0 -3 -3 6.32 2.28 0 3 -4 587.60 13.11 0 -3 -4 610.82 16.94 0 3 4 628.53 17.50 0 -3 -5 189.56 10.48 0 3 5 199.75 10.73 0 3 -5 185.22 5.81 0 3 -5 192.05 7.77 0 3 -6 753.36 13.31 0 -3 -6 807.87 22.11 0 -3 -6 780.16 16.67 0 3 -6 787.30 16.30 0 3 6 842.08 22.87 0 -3 -7 1778.77 25.86 0 3 7 1833.90 35.84 0 -3 -7 1853.81 35.98 0 3 -7 1768.35 25.57 0 3 -7 1749.25 22.75 0 3 -8 521.49 14.57 0 3 8 545.28 20.90 0 -3 -8 559.20 14.81 0 -3 -8 606.49 21.70 0 3 -8 532.01 13.85 0 3 9 534.21 21.75 0 -3 -9 539.96 21.94 0 -3 -9 537.59 14.80 0 3 -9 515.79 15.21 0 3 -9 503.01 14.69 0 3 10 33.35 6.12 0 3 -10 31.16 4.19 0 -3 -10 21.57 5.24 0 3 -10 23.35 3.54 0 -3 -11 116.16 11.37 0 3 11 123.13 11.99 0 3 12 370.50 20.99 0 -3 -12 368.82 20.93 0 3 -12 382.52 21.89 0 -3 -13 -1.27 3.29 0 3 13 -2.30 3.76 0 3 -13 2.22 3.65 0 3 14 195.94 16.88 0 -3 -14 190.54 16.63 0 3 -14 195.35 17.27 0 3 -15 4.06 4.93 0 3 15 14.69 5.98 0 -3 -15 10.12 5.13 0 -3 -16 2.77 3.47 0 3 16 0.38 3.69 0 3 -16 5.72 4.49 0 3 17 35.97 9.22 0 3 -17 35.12 9.02 0 -3 -17 54.18 10.13 0 3 -18 114.87 15.59 0 -3 -18 103.56 14.33 0 -3 -18 178.44 18.77 0 -4 0 2379.80 33.62 0 4 0 2392.88 33.23 0 4 0 2393.45 31.80 0 -4 1 6726.67 56.69 0 4 -1 6549.37 51.80 0 -4 -1 6685.96 56.16 0 4 1 6632.43 56.18 0 4 2 204.34 10.39 0 -4 2 221.02 10.54 0 -4 -2 203.67 10.43 0 4 3 9.52 3.37 0 -4 -3 17.80 3.70 0 4 -3 14.77 2.70 0 -4 -4 77.81 6.89 0 4 4 66.37 6.53 0 4 -4 77.34 5.61 0 4 -5 408.19 12.55 0 4 5 412.37 16.47 0 -4 -5 420.60 16.52 0 4 -6 598.19 15.49 0 -4 -6 601.13 20.73 0 4 6 577.54 20.67 0 4 -7 878.23 19.21 0 4 7 917.36 27.00 0 -4 -7 918.47 20.72 0 -4 -7 930.96 26.63 0 4 -8 1.84 1.14 0 4 -8 3.38 1.68 0 4 8 6.28 3.39 0 -4 -8 2.95 2.88 0 -4 -8 2.95 1.77 0 -4 -9 207.42 10.10 0 4 9 211.88 14.66 0 -4 -9 227.20 14.75 0 4 -9 190.12 9.50 0 4 10 1681.20 41.89 0 -4 -10 1625.90 40.76 0 4 11 89.29 10.51 0 -4 -11 90.41 10.57 0 4 12 48.55 8.57 0 -4 -12 51.68 8.35 0 4 13 0.48 3.35 0 -4 -13 -3.25 3.88 0 4 -13 6.15 5.40 0 -4 -14 9.51 4.91 0 4 -14 9.22 5.24 0 4 14 15.58 5.58 0 4 15 43.51 9.02 0 -4 -15 37.74 8.49 0 4 -15 27.95 7.56 0 -4 -16 11.77 4.99 0 4 -16 17.52 6.25 0 4 16 17.51 6.40 0 4 17 -2.77 4.91 0 -4 -17 14.49 6.20 0 4 -17 11.12 5.39 0 -5 0 4.09 3.19 0 5 0 2.36 2.40 0 5 0 -3.26 2.91 0 5 -1 10.61 2.83 0 5 1 9.87 3.36 0 -5 1 13.61 3.67 0 -5 -1 4.42 3.20 0 -5 2 1180.62 27.38 0 5 2 1162.01 27.08 0 5 -2 1102.37 24.24 0 -5 -2 1143.57 26.87 0 -5 -3 151.94 10.24 0 5 3 141.12 9.92 0 -5 3 136.80 3.47 0 5 -3 146.43 8.55 0 -5 -4 486.25 18.54 0 5 -4 456.08 14.90 0 5 4 469.43 18.50 0 -5 -5 275.57 14.50 0 5 5 267.46 14.46 0 5 -5 248.11 10.94 0 5 6 54.01 7.10 0 5 -6 63.65 5.67 0 -5 -6 62.59 7.61 0 -5 -7 22.38 4.85 0 5 7 24.33 5.66 0 5 -7 33.25 4.20 0 5 8 1142.62 33.38 0 -5 -8 1152.11 32.72 0 5 -8 1104.49 23.63 0 -5 -8 1188.43 26.38 0 -5 -9 2.91 2.32 0 5 9 3.32 3.15 0 -5 -9 3.44 3.31 0 -5 -10 60.82 8.94 0 5 10 58.32 8.68 0 5 11 -0.60 3.72 0 -5 -11 7.34 3.95 0 5 12 41.24 8.54 0 -5 -12 26.92 6.47 0 5 13 69.79 10.62 0 -5 -13 68.06 10.45 0 -5 -14 10.21 5.68 0 5 14 12.70 5.89 0 5 -14 11.30 5.98 0 -5 -15 -1.16 3.61 0 5 -15 -3.47 4.48 0 5 15 4.37 4.60 0 5 -16 10.26 6.14 0 -5 -16 12.21 6.10 0 5 16 11.07 5.79 0 5 17 131.82 16.34 0 5 -17 118.16 15.67 0 -5 -17 125.98 15.73 0 -6 0 1589.54 34.43 0 6 0 1600.38 32.42 0 -6 1 124.08 10.15 0 6 1 118.01 9.70 0 -6 -1 132.59 10.50 0 6 -1 117.78 8.93 0 -6 2 129.97 10.48 0 6 -2 121.54 9.12 0 -6 -2 137.37 10.45 0 6 2 125.33 10.23 0 6 3 34.45 6.49 0 6 -3 37.29 5.22 0 -6 -3 32.63 5.68 0 6 -4 4.68 2.38 0 -6 -4 1.73 2.66 0 6 4 -1.18 3.99 0 6 5 48.75 7.19 0 6 -5 48.99 5.51 0 -6 -5 40.32 6.45 0 6 -6 879.78 22.79 0 6 6 853.14 28.29 0 -6 -6 862.71 28.14 0 -6 -7 47.61 7.10 0 6 -7 55.58 5.75 0 6 7 73.25 9.47 0 6 -8 13.21 3.30 0 -6 -8 12.24 4.64 0 6 8 10.88 4.54 0 -6 -9 22.40 5.80 0 6 9 21.74 6.18 0 -6 -9 21.29 4.01 0 6 10 203.18 16.34 0 -6 -10 186.91 15.21 0 -6 -11 92.62 11.22 0 6 11 84.44 11.36 0 -6 -12 15.87 5.30 0 6 12 30.43 7.30 0 6 13 68.21 10.82 0 -6 -13 23.12 6.98 0 6 14 25.92 7.17 0 -6 -14 32.33 8.20 0 6 15 -3.30 3.66 0 6 -15 2.79 4.03 0 6 -16 22.54 7.84 0 6 16 42.79 10.10 0 -6 -16 17.21 6.85 0 7 0 2.18 2.53 0 -7 0 -3.59 2.96 0 7 1 2363.29 45.65 0 -7 -1 2390.32 46.19 0 7 1 2209.53 42.10 0 7 -1 2334.21 42.51 0 -7 1 2398.63 46.39 0 7 -2 496.01 19.62 0 7 2 451.12 20.41 0 -7 2 488.88 21.72 0 -7 -2 493.73 21.55 0 -7 3 471.22 21.22 0 7 3 450.07 20.73 0 7 -3 487.77 18.96 0 -7 -3 445.70 20.47 0 7 4 132.16 11.69 0 7 -4 133.95 9.95 0 -7 -4 137.10 11.82 0 7 -5 41.51 5.70 0 7 5 36.25 6.89 0 -7 -5 37.18 6.56 0 -7 -6 104.25 10.90 0 7 -6 110.54 8.85 0 7 6 108.69 11.35 0 7 7 84.68 10.21 0 -7 -7 86.35 10.13 0 7 -7 81.40 7.72 0 7 8 372.09 21.18 0 -7 -8 356.31 20.46 0 7 9 2.59 3.74 0 -7 -9 0.01 4.13 0 7 10 129.49 13.67 0 -7 -10 123.00 13.05 0 7 11 75.75 11.10 0 -7 -11 59.78 10.18 0 7 12 9.66 4.75 0 -7 -12 3.62 4.95 0 7 13 53.54 9.70 0 -7 -13 40.33 8.76 0 7 14 1.35 3.66 0 -7 -14 9.65 4.48 0 -7 -15 83.60 12.84 0 7 15 81.67 13.10 0 -7 -16 45.84 10.02 0 -8 0 -1.54 3.03 0 8 0 1.40 3.12 0 8 1 380.07 19.02 0 8 -1 362.74 18.38 0 -8 -1 381.33 20.33 0 -8 1 384.77 20.46 0 8 2 117.03 11.58 0 8 2 119.11 11.15 0 8 -2 123.89 10.82 0 -8 -2 113.61 11.59 0 -8 2 170.96 13.78 0 8 3 164.65 13.52 0 8 -3 160.28 11.73 0 -8 -3 156.08 13.26 0 -8 -4 58.15 8.44 0 8 4 54.71 8.61 0 8 -4 62.12 7.61 0 8 -5 1.15 2.33 0 -8 -5 2.25 3.87 0 8 5 2.59 3.42 0 8 -6 484.13 19.89 0 8 6 490.25 24.48 0 -8 -6 519.30 24.97 0 -8 -7 17.67 5.71 0 8 7 11.53 5.35 0 8 8 128.83 13.53 0 -8 -8 113.68 12.95 0 8 9 10.23 5.13 0 -8 -9 10.20 4.81 0 -8 -10 5.26 3.95 0 8 10 7.01 4.51 0 8 11 218.93 18.95 0 -8 -11 228.24 19.14 0 -8 -12 9.39 5.36 0 8 12 18.01 6.70 0 -8 -13 5.31 4.88 0 8 13 14.99 6.64 0 -8 -14 10.45 5.94 0 8 14 9.15 5.65 0 -8 -15 -6.17 4.40 0 -9 0 2.78 3.71 0 9 0 1.71 3.04 0 -9 -1 21.28 6.36 0 -9 1 26.73 7.02 0 9 -1 16.29 4.85 0 9 1 27.50 6.00 0 -9 -2 32.70 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-6 -3 26.80 6.72 -6 6 2 10.96 5.04 -6 -6 -2 6.94 4.99 -6 -6 -1 115.09 14.17 -6 6 1 91.13 12.67 -6 6 0 3.52 5.03 -6 -6 0 3.50 3.40 -6 6 -1 90.14 12.83 -6 -6 1 92.29 12.42 -6 6 -2 10.08 5.44 -6 -6 2 7.52 4.27 -6 6 -3 23.47 7.53 -6 -6 3 28.18 7.41 -6 -6 4 114.43 13.54 -6 6 -4 117.55 15.33 -6 -6 4 109.07 13.60 -6 6 -5 3.50 4.09 -6 -6 5 10.08 5.38 -6 6 -6 18.08 6.83 -6 -6 6 14.93 5.35 -6 6 -7 74.72 12.83 -6 -6 7 78.29 11.73 -6 6 -8 110.28 15.04 -6 -6 8 90.38 12.89 -6 -6 9 38.44 8.88 -6 -6 10 -1.16 3.32 -6 -7 -8 49.80 10.11 -6 7 7 15.92 6.51 -6 -7 -7 23.66 8.04 -6 7 7 8.12 5.24 -6 -7 -7 15.44 7.45 -6 -7 -6 3.22 4.22 -6 7 6 -0.07 3.66 -6 -7 -6 2.68 3.40 -6 7 6 10.01 4.81 -6 7 5 12.30 5.99 -6 -7 -5 4.71 4.71 -6 -7 -5 4.29 3.88 -6 7 4 17.42 6.17 -6 -7 -4 8.66 4.86 -6 7 3 49.55 9.93 -6 -7 -3 63.31 11.73 -6 7 2 33.32 8.38 -6 -7 -2 29.35 7.82 -6 7 1 24.22 7.39 -6 -7 -1 27.63 8.40 -6 7 0 -0.44 3.61 -6 -7 0 -5.55 5.07 -6 7 -1 14.01 5.74 -6 -7 1 20.17 6.16 -6 7 -2 22.89 7.38 -6 -7 2 30.91 7.90 -6 7 -3 58.23 11.16 -6 -7 3 49.12 9.66 -6 7 -4 11.02 5.22 -6 -7 4 19.56 6.25 -6 7 -5 5.37 4.94 -6 -7 5 -0.13 3.06 -6 -7 5 3.97 4.31 -6 7 -6 2.69 4.26 -6 -7 6 7.55 5.26 -6 7 -7 9.70 5.26 -6 -7 7 15.25 5.70 -6 -7 8 41.39 9.31 -6 8 7 6.36 3.87 -6 8 7 15.78 6.27 -6 -8 -7 41.43 9.70 -6 8 6 41.71 9.69 -6 8 6 47.43 9.78 -6 8 5 0.83 3.23 -6 8 4 25.35 7.46 -6 -8 -4 20.43 7.55 -6 8 3 137.10 16.65 -6 -8 -3 141.54 17.30 -6 8 2 -2.21 3.61 -6 -8 -2 1.99 5.99 -6 8 1 29.64 8.08 -6 -8 -1 23.04 7.42 -6 8 0 58.80 11.40 -6 -8 0 88.09 13.65 -6 8 -1 20.61 8.33 -6 -8 1 20.51 7.15 -6 8 -2 2.41 4.79 -6 -8 2 4.50 4.68 -6 8 -3 132.93 17.51 -6 -8 3 142.48 16.63 -6 8 -4 21.36 7.12 -6 -8 4 20.81 6.80 -6 -8 5 5.71 5.42 -6 -9 1 51.77 10.57 -6 -9 2 13.27 5.75 -6 -9 3 105.98 14.95 -6 -9 4 18.12 6.71 -7 0 0 2.40 2.98 -7 0 -1 56.06 9.71 -7 0 1 63.30 9.78 -7 0 1 55.97 10.31 -7 0 -2 225.99 18.93 -7 0 2 261.13 21.42 -7 0 -3 25.61 7.14 -7 0 3 57.21 10.78 -7 0 -4 35.29 8.44 -7 0 4 38.75 8.86 -7 0 -5 2.67 4.91 -7 0 5 1.70 5.18 -7 0 6 51.97 10.54 -7 0 -6 45.62 10.15 -7 0 7 0.72 3.51 -7 0 -7 6.07 4.67 -7 0 8 42.06 9.68 -7 0 -8 23.68 8.25 -7 1 8 2.83 4.21 -7 -1 -8 13.44 5.05 -7 -1 -7 112.91 14.97 -7 1 7 167.96 18.03 -7 1 6 13.04 4.95 -7 -1 -6 16.10 6.43 -7 -1 -5 74.75 11.54 -7 1 5 88.36 12.79 -7 -1 -4 58.63 10.47 -7 1 4 49.87 9.50 -7 -1 -3 102.71 13.01 -7 1 3 122.49 14.86 -7 -1 -2 30.40 7.30 -7 1 2 36.40 8.50 -7 -1 -1 33.17 7.43 -7 1 1 17.49 5.44 -7 1 1 31.47 8.06 -7 -1 0 5.42 3.82 -7 1 0 1.88 3.90 -7 1 -1 19.67 6.33 -7 -1 1 34.52 9.19 -7 1 -2 33.83 8.09 -7 -1 2 33.50 8.23 -7 1 -3 123.39 14.61 -7 -1 3 130.20 15.39 -7 1 -4 50.49 10.10 -7 -1 4 55.38 10.80 -7 1 -5 55.60 10.52 -7 -1 5 79.06 12.55 -7 1 -6 10.12 6.30 -7 -1 6 16.19 7.04 -7 1 -7 156.90 17.61 -7 -1 7 152.81 17.28 -7 -1 8 4.86 5.57 -7 1 -8 7.16 6.28 -7 2 8 28.00 8.22 -7 -2 -8 30.56 8.40 -7 2 7 25.86 7.61 -7 -2 -7 31.60 8.99 -7 2 6 26.67 7.48 -7 -2 -6 21.25 6.79 -7 2 5 93.58 13.56 -7 -2 -5 92.14 13.06 -7 -2 -4 54.01 9.93 -7 2 4 58.89 11.07 -7 -2 -3 31.02 7.50 -7 2 3 25.48 7.05 -7 -2 -2 53.80 9.34 -7 2 2 50.41 9.05 -7 2 2 62.45 10.54 -7 -2 -1 10.33 4.99 -7 -2 -1 12.62 5.70 -7 2 1 8.19 3.86 -7 2 1 9.58 5.94 -7 -2 0 7.81 4.54 -7 2 0 1.40 3.08 -7 -2 1 12.85 4.87 -7 2 -1 7.30 4.70 -7 -2 2 42.48 8.31 -7 2 -2 56.94 10.11 -7 -2 2 52.17 9.93 -7 2 -3 23.36 6.65 -7 -2 3 20.55 6.62 -7 2 -4 71.63 11.49 -7 -2 4 80.42 12.82 -7 2 -5 91.19 13.48 -7 -2 5 101.98 14.25 -7 2 -6 25.24 8.20 -7 -2 6 20.13 7.86 -7 -2 7 25.73 7.83 -7 2 -7 24.70 7.84 -7 -2 8 21.28 7.03 -7 2 -8 13.38 6.60 -7 3 8 77.27 13.25 -7 -3 -8 77.00 13.30 -7 3 7 45.27 9.96 -7 -3 -7 47.92 10.31 -7 3 6 18.57 7.34 -7 -3 -6 20.07 6.53 -7 3 5 28.16 7.81 -7 -3 -5 15.64 6.22 -7 -3 -4 17.01 7.21 -7 3 4 3.32 3.58 -7 -3 -3 319.93 24.22 -7 3 3 285.86 20.81 -7 3 3 291.88 22.46 -7 -3 -2 68.34 11.29 -7 3 2 79.28 11.45 -7 3 2 58.77 10.33 -7 -3 -1 0.09 3.80 -7 3 1 4.82 4.48 -7 3 1 20.25 6.66 -7 3 0 11.99 5.24 -7 -3 0 9.32 4.82 -7 3 -1 1.22 3.57 -7 -3 1 1.48 3.74 -7 3 -2 69.77 11.54 -7 -3 2 66.07 10.26 -7 -3 2 86.03 12.80 -7 3 -3 305.61 23.51 -7 -3 3 281.99 22.82 -7 3 -4 9.74 5.70 -7 -3 4 3.70 3.43 -7 3 -5 29.65 8.36 -7 -3 5 41.24 9.63 -7 3 -6 22.39 7.28 -7 -3 6 24.20 7.50 -7 3 -7 59.08 11.46 -7 -3 7 42.65 9.97 -7 4 8 48.32 10.47 -7 4 7 25.72 7.34 -7 -4 -7 21.93 7.55 -7 4 6 12.93 5.64 -7 -4 -6 20.86 7.93 -7 -4 -6 22.13 7.23 -7 -4 -5 35.63 9.17 -7 -4 -5 20.78 7.52 -7 4 5 25.43 7.78 -7 -4 -4 51.35 10.32 -7 4 4 37.80 8.38 -7 4 4 56.85 10.28 -7 -4 -3 69.54 11.88 -7 4 3 66.87 11.07 -7 4 3 71.99 11.24 -7 4 2 26.53 7.20 -7 -4 -2 28.50 8.60 -7 4 2 21.47 6.20 -7 4 1 2.42 3.17 -7 -4 -1 8.61 4.58 -7 4 1 3.34 3.03 -7 4 0 1.77 3.32 -7 -4 0 17.74 6.86 -7 4 -1 7.01 3.44 -7 -4 1 5.78 4.37 -7 4 -2 16.45 5.61 -7 -4 2 26.84 7.36 -7 4 -3 50.30 10.41 -7 -4 3 59.33 10.33 -7 4 -4 49.32 10.08 -7 -4 4 68.44 11.87 -7 4 -5 32.73 8.99 -7 -4 5 42.93 9.82 -7 4 -6 18.57 7.00 -7 -4 6 14.56 6.91 -7 -4 7 25.59 7.80 -7 5 7 28.95 8.09 -7 5 6 35.07 8.38 -7 -5 -6 26.10 8.40 -7 -5 -5 8.85 5.08 -7 -5 -5 19.84 7.66 -7 5 5 16.04 5.91 -7 -5 -4 40.71 10.20 -7 5 4 43.43 8.94 -7 -5 -4 34.91 8.55 -7 5 4 42.08 8.84 -7 -5 -3 54.98 11.13 -7 5 3 37.77 8.74 -7 5 2 45.11 9.35 -7 -5 -2 65.93 11.61 -7 5 1 15.63 6.32 -7 -5 -1 17.11 6.37 -7 5 0 1.86 3.21 -7 -5 0 16.40 5.77 -7 5 -1 11.58 6.19 -7 -5 1 12.94 5.59 -7 5 -2 73.51 12.88 -7 -5 2 56.45 10.18 -7 5 -3 35.04 8.54 -7 -5 3 35.31 7.87 -7 5 -4 32.36 9.07 -7 -5 4 39.83 9.21 -7 5 -5 28.90 7.85 -7 -5 5 22.18 7.68 -7 -5 6 19.64 6.72 -7 -6 -6 3.41 3.35 -7 6 5 14.96 6.57 -7 -6 -5 9.86 4.83 -7 6 4 83.38 12.50 -7 6 3 20.20 6.68 -7 -6 -3 37.00 9.52 -7 6 2 -0.54 4.20 -7 -6 -2 7.65 5.56 -7 6 1 15.28 6.43 -7 -6 -1 16.65 7.37 -7 6 0 2.03 5.12 -7 -6 0 1.21 3.44 -7 6 -1 17.81 5.14 -7 -6 1 13.35 6.38 -7 6 -2 8.47 6.04 -7 -6 2 71.59 13.74 -7 6 -3 53.55 11.39 -7 -6 3 30.30 8.04 -7 -6 5 18.11 7.47 -7 -7 1 73.24 12.55 -7 -7 2 78.50 13.27 -7 -7 3 7.09 4.76 -8 0 -2 19.92 6.79 -8 0 -3 7.39 4.74 -8 0 -4 68.43 11.66 -8 -1 -4 15.03 5.94 -8 -1 -3 22.46 6.97 -8 1 2 33.46 9.17 -8 1 -1 5.91 4.93 -8 1 -2 24.80 7.29 -8 1 -3 27.70 7.76 -8 1 -4 4.27 4.23 -8 2 2 108.06 15.36 -8 2 0 -0.83 3.47 -8 2 -1 15.77 6.86 -8 2 -2 91.44 13.87 -8 2 -3 3.36 4.68 -8 3 2 1.28 3.87 -8 3 1 55.99 10.82 -8 3 0 9.16 5.90 -8 3 -1 41.21 9.63 -8 4 1 5.97 5.07 0 0 0 0.00 0.00 TITL xi075 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 0.71073 5.573566 9.215351 12.795168 90.0000 90.0000 90.0000 ZERR 1.00 0.000236 0.000441 0.000666 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O F UNIT 12.00 16.00 4.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 5686 _shelx_res_file ; TITL shelxt_a.res in P2(1)2(1)2(1) shelx.res created by SHELXL-2019/3 at 09:36:01 on 07-Jan-2025 CELL 0.71073 5.5736 9.2154 12.7952 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0004 0.0007 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC H C N O F UNIT 24 12 4 8 20 MERG 2 OMIT 0 1 3 EQIV $1 x-1/2, -y+1/2, -z+1 HTAB N1 F5_$1 EQIV $2 x-1, y, z HTAB N1 F4_$2 HTAB N1 F3 HTAB F4 F3 HTAB F3 F4 HTAB F5 F3 HTAB F3 F5 HTAB N1 F5_$1 HTAB N1 F4_$2 HTAB N1 F3 HTAB F4 F3 HTAB F3 F4 HTAB F5 F3 HTAB F3 F5 FMAP 2 PLAN 20 SIZE 0.072 0.108 0.338 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -171.00 WGHT 0.029600 FVAR 1.03931 MOLE 1 F1 5 0.047598 0.320003 0.022154 11.00000 0.02362 0.02763 = 0.02166 -0.00408 -0.00475 -0.00040 F2 5 0.430640 0.504336 0.052123 11.00000 0.02338 0.02905 = 0.02090 0.00230 0.00587 -0.00263 O2 4 0.440799 0.583475 0.214023 11.00000 0.01939 0.01648 = 0.02474 0.00091 -0.00227 -0.00334 O1 4 -0.166451 0.319688 0.166603 11.00000 0.01356 0.02082 = 0.02867 -0.00080 -0.00195 -0.00120 N1 3 0.221802 0.344947 0.293014 11.00000 0.01376 0.01714 = 0.02034 0.00296 -0.00092 -0.00190 C1 2 0.021003 0.330146 0.125288 11.00000 0.01854 0.01199 = 0.02274 -0.00103 -0.00434 0.00056 C2 2 0.382937 0.494513 0.153642 11.00000 0.01101 0.01761 = 0.01952 0.00272 0.00054 0.00060 C3 2 0.260557 0.351649 0.179593 11.00000 0.01197 0.01351 = 0.01878 -0.00036 -0.00144 0.00127 H1 1 0.153579 0.256682 0.314779 11.00000 0.02503 H2 1 0.125575 0.414236 0.312142 11.00000 0.02016 H4 1 0.361958 0.275012 0.156204 11.00000 0.01181 H3 1 0.355458 0.362889 0.330818 11.00000 0.03659 MOLE 2 F4 5 0.883922 0.548340 0.346154 11.00000 0.02007 0.02049 = 0.02683 -0.00035 0.00055 -0.00179 F5 5 0.535002 0.383582 0.596448 11.00000 0.02382 0.02317 = 0.01928 0.00321 0.00099 0.00507 F3 5 0.597280 0.393213 0.415897 11.00000 0.02105 0.03006 = 0.02063 -0.00119 -0.00196 -0.00457 H5 1 0.783541 0.481551 0.377637 11.00000 0.07119 H6 1 0.562241 0.384692 0.524129 11.00000 0.06960 HKLF 4 REM shelxt_a.res in P2(1)2(1)2(1) REM wR2 = 0.0668, GooF = S = 1.019, Restrained GooF = 1.019 for all data REM R1 = 0.0338 for 1930 Fo > 4sig(Fo) and 0.0415 for all 2187 data REM 124 parameters refined using 0 restraints END WGHT 0.0296 0.0000 REM Highest difference peak 0.273, deepest hole -0.181, 1-sigma level 0.051 Q1 1 0.3108 0.4235 0.1626 11.00000 0.05 0.27 Q2 1 0.1408 0.3405 0.1549 11.00000 0.05 0.27 Q3 1 0.2436 0.3445 0.2380 11.00000 0.05 0.21 Q4 1 0.3696 0.5799 0.1631 11.00000 0.05 0.20 Q5 1 0.9462 0.5825 0.4435 11.00000 0.05 0.19 Q6 1 0.9386 0.6391 0.3441 11.00000 0.05 0.19 Q7 1 0.4984 0.2952 0.5858 11.00000 0.05 0.19 Q8 1 0.4301 0.4638 0.6071 11.00000 0.05 0.18 Q9 1 0.0496 0.3297 0.0835 11.00000 0.05 0.17 Q10 1 0.3504 0.5224 0.2380 11.00000 0.05 0.17 Q11 1 0.4632 0.5001 0.1981 11.00000 0.05 0.17 Q12 1 0.9161 0.6212 0.3747 11.00000 0.05 0.17 Q13 1 -0.0571 0.2744 0.1425 11.00000 0.05 0.17 Q14 1 0.0048 0.2209 0.0381 11.00000 0.05 0.16 Q15 1 0.5735 0.4816 0.3741 11.00000 0.05 0.16 Q16 1 0.8866 0.5401 0.2755 11.00000 0.05 0.16 Q17 1 0.5022 0.5598 0.2631 11.00000 0.05 0.16 Q18 1 0.6215 0.3825 0.4733 11.00000 0.05 0.15 Q19 1 0.5411 0.3901 0.6743 11.00000 0.05 0.15 Q20 1 0.4539 0.4996 -0.0222 11.00000 0.05 0.15 ; _shelx_res_checksum 43428 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 0.0476(2) 0.32000(12) 0.02215(9) 0.0243(3) Uani d 1 . . F F2 0.4306(2) 0.50434(12) 0.05212(8) 0.0244(3) Uani d 1 . . O O2 0.4408(2) 0.58347(13) 0.21402(10) 0.0202(3) Uani d 1 . . O O1 -0.1665(2) 0.31969(15) 0.16660(11) 0.0210(3) Uani d 1 . . N N1 0.2218(3) 0.34495(18) 0.29301(12) 0.0171(3) Uani d 1 . . C C1 0.0210(3) 0.33015(19) 0.12529(14) 0.0178(3) Uani d 1 . . C C2 0.3829(3) 0.49451(19) 0.15364(13) 0.0160(3) Uani d 1 . . C C3 0.2606(3) 0.35165(19) 0.17959(14) 0.0148(3) Uani d 1 . . H H1 0.154(4) 0.257(3) 0.3148(19) 0.025(6) Uiso d 1 . . H H2 0.126(4) 0.414(2) 0.3121(17) 0.020(5) Uiso d 1 . . H H4 0.362(4) 0.275(2) 0.1562(15) 0.012(5) Uiso d 1 . . H H3 0.355(4) 0.363(3) 0.331(2) 0.037(7) Uiso d 1 . . F F4 0.88392(19) 0.54834(12) 0.34615(9) 0.0225(2) Uani d 1 . . F F5 0.53500(19) 0.38358(12) 0.59645(9) 0.0221(2) Uani d 1 . . F F3 0.59728(18) 0.39321(12) 0.41590(9) 0.0239(3) Uani d 1 . . H H5 0.784(6) 0.482(4) 0.378(3) 0.071(11) Uiso d 1 . . H H6 0.562(5) 0.385(4) 0.524(3) 0.070(9) 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 F1 0.0236(5) 0.0276(6) 0.0217(5) -0.0004(4) -0.0047(5) -0.0041(5) F2 0.0234(5) 0.0291(6) 0.0209(6) -0.0026(5) 0.0059(4) 0.0023(4) O2 0.0194(6) 0.0165(6) 0.0247(7) -0.0033(5) -0.0023(5) 0.0009(5) O1 0.0136(6) 0.0208(7) 0.0287(7) -0.0012(5) -0.0019(5) -0.0008(6) N1 0.0138(7) 0.0171(7) 0.0203(8) -0.0019(6) -0.0009(6) 0.0030(6) C1 0.0185(8) 0.0120(8) 0.0227(8) 0.0006(6) -0.0043(6) -0.0010(7) C2 0.0110(7) 0.0176(8) 0.0195(8) 0.0006(6) 0.0005(6) 0.0027(7) C3 0.0120(7) 0.0135(8) 0.0188(8) 0.0013(6) -0.0014(6) -0.0004(6) F4 0.0201(5) 0.0205(6) 0.0268(6) -0.0018(4) 0.0006(5) -0.0004(5) F5 0.0238(5) 0.0232(6) 0.0193(5) 0.0051(4) 0.0010(4) 0.0032(4) F3 0.0210(5) 0.0301(6) 0.0206(5) -0.0046(4) -0.0020(4) -0.0012(5) 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' F F 0.0171 0.0103 '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 C3 N1 H1 . . 112.9(15) ? C3 N1 H2 . . 109.8(14) ? H1 N1 H2 . . 107.6(19) ? C3 N1 H3 . . 113.6(15) ? H1 N1 H3 . . 109(2) ? H2 N1 H3 . . 103(2) ? O1 C1 F1 . . 122.64(16) ? O1 C1 C3 . . 125.94(17) ? F1 C1 C3 . . 111.40(14) ? O2 C2 F2 . . 122.80(16) ? O2 C2 C3 . . 125.85(16) ? F2 C2 C3 . . 111.25(14) ? N1 C3 C1 . . 108.51(14) ? N1 C3 C2 . . 108.57(14) ? C1 C3 C2 . . 114.07(14) ? N1 C3 H4 . . 111.5(12) ? C1 C3 H4 . . 106.3(12) ? C2 C3 H4 . . 107.9(12) ? H5 F3 H6 . . 118.6(19) ? 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 C1 . 1.331(2) ? F2 C2 . 1.329(2) ? O2 C2 . 1.172(2) ? O1 C1 . 1.175(2) ? N1 C3 . 1.469(2) ? N1 H1 . 0.94(2) ? N1 H2 . 0.87(2) ? N1 H3 . 0.90(3) ? C1 C3 . 1.518(2) ? C2 C3 . 1.519(2) ? C3 H4 . 0.95(2) ? F4 H5 . 0.92(4) ? F5 H6 . 0.94(3) ? F3 H5 . 1.41(4) ? F3 H6 . 1.40(3) ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance C1 F4 2.676(2) C1 F5 2.682(2) C2 F5 2.688(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 F5 4_456 0.94(2) 1.84(2) 2.7422(19) 159(2) yes N1 H2 F4 1_455 0.87(2) 1.88(2) 2.7426(19) 172(2) yes N1 H3 F3 . 0.90(3) 1.75(3) 2.6551(19) 174(2) yes F4 H5 F3 . 0.92(4) 1.41(4) 2.3221(15) 170(3) yes F5 H6 F3 . 0.94(3) 1.40(3) 2.3378(16) 177(3) yes N1 H1 F5 4_456 0.94(2) 1.84(2) 2.7422(19) 159(2) yes N1 H2 F4 1_455 0.87(2) 1.88(2) 2.7426(19) 172(2) yes N1 H3 F3 . 0.90(3) 1.75(3) 2.6551(19) 174(2) yes F4 H5 F3 . 0.92(4) 1.41(4) 2.3221(15) 170(3) yes F5 H6 F3 . 0.94(3) 1.40(3) 2.3378(16) 177(3) 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 O1 C1 C3 N1 . . . . 4.7(3) ? F1 C1 C3 N1 . . . . -173.50(14) ? O1 C1 C3 C2 . . . . -116.4(2) ? F1 C1 C3 C2 . . . . 65.34(19) ? O2 C2 C3 N1 . . . . 1.3(2) ? F2 C2 C3 N1 . . . . 177.71(13) ? O2 C2 C3 C1 . . . . 122.37(19) ? F2 C2 C3 C1 . . . . -61.17(18) ?