#------------------------------------------------------------------------------ #$Date: 2018-10-20 05:43:40 +0300 (Sat, 20 Oct 2018) $ #$Revision: 211563 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/26/2242679.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_2242679 loop_ _publ_author_name 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Toze, Flavien A. A.' 'Dorovatovskii, Pavel V.' 'Guliyeva, Narmina A.' 'Panahova, Humay M.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of dimethyl (3aS,6R,6aS,7S)-2-(2,2,2-trifluoroacetyl)-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a^1^,6a-dicarboxylate ; _journal_coeditor_code WM5463 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1599 _journal_page_last 1604 _journal_paper_doi 10.1107/S2056989018014305 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C18 H16 F3 N O7' _chemical_formula_moiety 'C18 H16 F3 N O7' _chemical_formula_sum 'C18 H16 F3 N O7' _chemical_formula_weight 415.32 _chemical_name_systematic ;Crystal structure and Hirshfeld surface analysis of dimethyl (3aS,6R,6aS,7S)-2-(2,2,2-trifluoroacetyl)-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a^1^,6a-dicarboxylate, dimethyl (3aS,6R,6aS,7S)-2-(2,2,2-trifluoroacetyl)-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a^1^,6a-dicarboxylate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 96.0210(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7661(2) _cell_length_b 11.2908(3) _cell_length_c 17.5089(4) _cell_measurement_reflns_used 3572 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.87 _cell_measurement_theta_min 2.95 _cell_volume 1723.41(7) _computing_cell_refinement ; SAINT (Bruker, 2007) ; _computing_data_collection ; APEX2 (Bruker, 2007) ; _computing_data_reduction ; SAINT (Bruker, 2007) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.992 _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 0.0281 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11170 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.410 _diffrn_reflns_theta_min 3.084 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.601 _exptl_crystal_description block _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.298 _refine_diff_density_min -0.254 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 3496 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0364 _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^)+(0.0391P)^2^+0.8462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.0908 _reflns_number_gt 2739 _reflns_number_total 3496 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5463sup1.cif _cod_data_source_block I _cod_database_code 2242679 _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 0.951 _shelx_estimated_absorpt_t_max 0.958 _shelx_hkl_file ; -1 0 0 0.20 0.40 -1 0 0 0.40 0.50 -1 0 0 0.40 0.50 1 0 0 0.40 0.40 1 0 0 0.50 0.50 1 0 0 0.10 0.50 2 0 0 8.70 1.50 2 0 0 8.80 1.60 -2 0 0 10.50 1.60 -2 0 0 8.70 1.50 2 0 0 7.80 1.20 -2 0 0 10.80 1.30 -3 0 0 -1.50 1.40 3 0 0 1.70 1.20 -3 0 0 -0.90 1.40 3 0 0 0.50 1.40 3 0 0 -0.50 1.50 4 0 0 129.49 4.70 4 0 0 125.99 5.50 -4 0 0 122.99 5.50 4 0 0 128.39 5.40 -4 0 0 126.29 5.60 5 0 0 -1.90 1.20 5 0 0 -2.50 1.90 -5 0 0 1.90 2.20 -5 0 0 1.50 2.20 -6 0 0 22.10 3.60 6 0 0 33.10 3.30 6 0 0 22.50 3.70 7 0 0 -0.40 2.60 -7 0 0 -2.50 2.50 -8 0 0 126.69 7.90 8 0 0 142.19 8.10 -9 0 0 2.30 3.40 9 0 0 -4.90 2.90 10 0 0 2.00 3.80 -10 0 0 0.30 4.10 0 1 0 -1.20 0.30 -1 -1 0 445.56 10.20 -1 1 0 537.05 10.10 2 -1 0 0.30 1.30 2 -1 0 -0.10 1.00 -2 -1 0 -0.30 1.30 -2 -1 0 -0.40 0.90 -2 -1 0 0.40 1.30 2 1 0 -0.40 0.80 2 1 0 1.10 1.40 -2 1 0 1.00 1.20 -2 1 0 -0.50 1.10 -3 -1 0 49.60 3.40 -3 -1 0 51.19 2.70 -3 -1 0 53.19 3.30 3 -1 0 51.09 3.10 3 -1 0 48.60 3.30 3 -1 0 47.50 2.90 3 1 0 48.80 2.60 -3 1 0 53.39 3.50 3 1 0 50.49 3.60 3 1 0 50.69 3.50 -3 1 0 44.30 3.00 -4 -1 0 50.19 4.00 -4 -1 0 56.19 3.10 4 -1 0 49.99 3.20 4 -1 0 60.69 4.30 4 -1 0 55.89 3.70 -4 -1 0 67.09 4.50 -4 1 0 54.39 3.80 -4 1 0 56.39 3.80 4 1 0 60.39 3.90 4 1 0 57.19 3.10 4 1 0 57.89 4.30 -5 -1 0 345.87 11.50 5 -1 0 302.77 10.10 5 -1 0 331.27 9.30 -5 -1 0 301.97 10.20 -5 -1 0 307.37 8.70 5 1 0 323.07 8.80 -5 1 0 317.07 10.00 5 1 0 316.47 10.10 -5 1 0 311.57 10.10 6 -1 0 378.96 11.80 -6 -1 0 343.17 11.80 6 -1 0 356.66 10.50 -6 1 0 368.06 11.70 6 1 0 354.26 11.70 6 1 0 346.97 10.00 7 -1 0 56.39 5.50 -7 -1 0 61.59 5.80 7 1 0 53.89 5.40 -7 1 0 74.19 6.10 7 1 0 74.19 5.00 8 -1 0 0.00 3.00 -8 -1 0 -2.40 2.70 8 1 0 -2.40 2.60 -8 1 0 1.00 2.70 -9 -1 0 384.76 14.90 9 -1 0 361.16 14.20 -9 1 0 373.56 14.50 -10 -1 0 26.10 5.50 10 -1 0 12.20 4.40 -10 1 0 9.30 4.30 0 2 0 946.31 18.50 -1 -2 0 313.47 7.00 1 -2 0 318.77 7.60 -1 -2 0 314.37 7.40 1 2 0 294.07 7.20 -1 2 0 315.07 7.60 -2 -2 0 4.30 1.20 -2 -2 0 8.10 1.80 2 -2 0 5.80 1.70 -2 2 0 6.30 1.70 -2 2 0 3.80 1.30 2 2 0 5.00 1.10 2 2 0 5.20 1.60 3 -2 0 101.09 4.60 -3 -2 0 104.29 3.70 -3 -2 0 98.29 4.80 3 2 0 98.99 3.60 3 2 0 105.19 4.80 -3 2 0 99.19 4.30 -3 2 0 105.79 4.50 4 -2 0 384.36 11.00 -4 -2 0 396.36 9.80 -4 -2 0 384.66 11.20 4 -2 0 383.86 10.50 -4 -2 0 402.96 11.30 -4 2 0 415.26 11.20 4 2 0 389.26 11.00 -4 2 0 391.06 10.60 4 2 0 384.46 9.60 -5 -2 0 802.52 18.00 5 -2 0 803.52 18.90 5 -2 0 857.21 20.80 -5 -2 0 801.62 20.00 5 -2 0 801.72 19.80 -5 2 0 804.92 19.40 5 2 0 780.32 17.90 -6 -2 0 172.98 8.00 6 -2 0 179.08 8.10 -6 -2 0 170.78 6.40 6 2 0 182.48 6.40 -6 2 0 179.58 7.60 -7 -2 0 213.58 9.90 7 -2 0 234.18 9.90 7 2 0 219.98 7.80 -7 2 0 218.58 9.20 -8 -2 0 2.30 3.40 8 -2 0 4.00 3.20 -8 2 0 2.30 3.20 -9 -2 0 22.60 5.00 9 -2 0 20.30 4.80 -9 2 0 28.40 5.30 -10 -2 0 5.00 4.40 10 -2 0 1.10 3.80 -10 2 0 -0.30 3.70 0 3 0 -0.50 0.90 1 -3 0 1339.07 27.40 -1 -3 0 1356.26 26.70 -1 -3 0 1314.57 26.70 1 3 0 1326.57 26.70 -2 -3 0 857.31 19.00 2 -3 0 866.61 19.30 -2 -3 0 872.01 18.30 -2 3 0 897.01 19.40 2 3 0 904.11 19.10 2 3 0 894.91 18.30 -3 -3 0 143.79 5.60 -3 -3 0 124.99 4.40 3 -3 0 131.69 5.70 -3 3 0 125.69 4.80 -3 3 0 117.39 5.30 3 3 0 123.99 4.30 3 3 0 127.39 5.40 -4 -3 0 193.98 7.40 -4 -3 0 195.98 7.30 4 -3 0 203.58 7.60 -4 -3 0 191.98 6.00 4 3 0 190.28 7.20 -4 3 0 187.88 7.20 4 3 0 188.98 5.90 -4 3 0 188.88 6.70 5 -3 0 3.70 2.20 -5 -3 0 2.30 2.30 -5 -3 0 3.20 1.50 5 3 0 0.30 1.20 -5 3 0 -1.10 1.80 -6 -3 0 112.69 5.10 6 -3 0 104.79 6.60 -6 -3 0 113.89 6.70 6 3 0 110.99 4.90 -6 3 0 112.79 6.00 7 -3 0 232.68 10.30 -7 -3 0 238.48 8.20 -7 -3 0 238.68 10.60 -7 3 0 238.18 9.60 7 3 0 247.88 8.10 8 -3 0 17.30 4.20 -8 -3 0 25.30 4.90 -8 3 0 12.60 3.60 9 -3 0 52.39 6.30 -9 -3 0 41.70 6.30 -9 3 0 50.49 6.20 -10 -3 0 6.30 4.70 10 -3 0 4.00 3.80 -10 3 0 4.20 3.90 0 4 0 407.16 9.40 1 -4 0 39.40 3.40 -1 -4 0 43.20 2.90 1 4 0 38.00 2.80 -2 -4 0 0.30 1.70 -2 -4 0 1.30 1.30 2 -4 0 2.10 1.90 2 4 0 0.20 1.50 -3 -4 0 69.19 4.60 3 -4 0 64.29 4.30 -3 -4 0 70.99 3.50 -3 4 0 68.49 4.20 3 4 0 67.09 3.30 3 4 0 65.99 4.10 -3 4 0 68.09 3.70 -4 -4 0 350.76 9.30 4 -4 0 355.76 11.10 -4 -4 0 354.86 10.90 -4 4 0 358.16 9.90 4 4 0 353.26 9.30 -5 -4 0 59.19 3.70 -5 -4 0 54.99 5.20 5 -4 0 57.09 5.00 5 4 0 70.09 3.80 -5 4 0 59.79 4.60 -6 -4 0 393.06 11.00 -6 -4 0 398.06 13.30 6 -4 0 390.06 13.20 6 4 0 398.46 10.90 -6 4 0 419.26 12.50 -7 -4 0 393.76 11.40 -7 -4 0 409.46 14.50 7 -4 0 398.76 13.90 -7 4 0 401.66 13.10 7 4 0 404.96 11.40 8 -4 0 57.99 6.30 -8 -4 0 43.60 6.00 -8 -4 0 55.89 4.60 -8 4 0 51.79 5.70 9 -4 0 22.50 5.00 -9 -4 0 34.10 5.80 -9 4 0 28.10 5.10 10 -4 0 -1.30 4.10 -10 -4 0 4.00 4.20 -10 4 0 -2.50 3.70 0 5 0 -0.80 1.30 1 -5 0 1852.21 38.50 -1 -5 0 1821.42 37.20 1 5 0 1889.51 37.30 -2 -5 0 1991.40 40.20 2 -5 0 1946.61 41.00 -2 -5 0 1975.40 39.70 2 5 0 1971.70 40.10 -3 -5 0 367.36 10.90 3 -5 0 394.96 11.60 -3 -5 0 380.26 10.00 -3 5 0 391.96 12.20 3 5 0 366.46 10.80 4 -5 0 0.30 2.30 -4 -5 0 3.00 2.10 -4 -5 0 -2.30 1.40 -4 5 0 0.80 1.70 4 5 0 -0.60 1.30 -5 -5 0 298.37 8.90 5 -5 0 301.97 11.00 -5 -5 0 299.87 10.90 -5 5 0 305.37 9.70 5 5 0 307.27 8.90 -6 -5 0 31.10 3.30 6 -5 0 29.90 4.50 -6 -5 0 27.00 4.40 6 5 0 38.20 3.50 -6 5 0 38.50 4.20 -7 -5 0 28.10 4.70 7 -5 0 19.30 4.40 -7 -5 0 24.10 3.20 -7 5 0 19.20 3.80 8 -5 0 34.30 5.40 -8 -5 0 23.20 3.40 -8 -5 0 31.70 5.40 -8 5 0 22.00 4.20 9 -5 0 21.00 5.00 -9 -5 0 22.40 5.60 -9 5 0 21.20 4.60 10 -5 0 5.60 4.30 -10 -5 0 3.30 4.70 -10 5 0 -4.30 3.50 0 6 0 6.20 1.70 -1 -6 0 338.07 9.30 1 -6 0 333.47 10.50 1 6 0 333.97 9.20 -1 6 0 327.67 8.60 -2 -6 0 987.40 22.00 2 -6 0 964.60 23.10 -2 -6 0 990.20 21.70 2 6 0 949.01 21.70 -3 -6 0 118.09 5.30 3 -6 0 139.29 7.00 -3 -6 0 129.49 6.00 -4 -6 0 320.27 10.70 4 -6 0 320.67 11.20 -4 -6 0 327.47 9.60 -4 6 0 329.87 9.60 -5 -6 0 1253.17 29.50 -5 -6 0 1221.38 27.10 5 -6 0 1229.68 29.70 -5 6 0 1245.58 27.70 6 -6 0 93.69 7.10 -6 -6 0 106.49 5.40 -6 -6 0 88.69 7.20 -6 6 0 92.19 5.70 6 6 0 98.39 5.10 -7 -6 0 19.80 3.10 -7 -6 0 14.60 4.20 7 -6 0 20.70 4.40 -7 6 0 12.90 3.40 -8 -6 0 -1.20 2.10 -8 -6 0 -0.90 3.30 8 -6 0 -3.40 2.90 -8 6 0 -1.30 2.70 -9 -6 0 8.90 4.90 9 -6 0 9.90 4.70 -9 6 0 24.60 4.60 0 7 0 -0.80 1.50 1 -7 0 59.69 5.30 1 7 0 51.69 3.80 -1 7 0 56.09 3.50 2 -7 0 1.30 2.50 -2 -7 0 5.20 2.20 -2 -7 0 2.50 1.90 2 7 0 3.60 2.00 3 -7 0 328.17 11.50 -3 -7 0 304.67 9.60 -3 -7 0 308.17 10.20 -4 -7 0 19.70 3.80 4 -7 0 10.90 3.20 -4 -7 0 15.10 2.70 -4 7 0 14.50 2.50 -5 -7 0 37.30 4.50 5 -7 0 30.80 4.60 -5 -7 0 39.40 3.80 -5 7 0 36.40 3.80 -6 -7 0 83.99 7.00 -6 -7 0 75.39 5.00 6 -7 0 76.49 7.20 -6 7 0 78.49 5.40 -7 -7 0 7.10 3.80 7 -7 0 11.40 3.90 -7 -7 0 8.70 2.70 -7 7 0 2.60 2.80 -8 -7 0 10.90 4.60 8 -7 0 11.40 4.50 -8 -7 0 9.90 4.50 -8 7 0 6.20 3.40 9 -7 0 43.50 7.00 -9 -7 0 45.30 6.80 -9 7 0 34.10 5.40 0 8 0 569.84 14.10 1 -8 0 42.90 4.90 -1 8 0 40.80 3.30 1 8 0 41.50 3.80 -2 -8 0 321.47 10.20 -2 -8 0 335.97 10.60 2 -8 0 327.27 11.80 -3 -8 0 12.00 2.90 3 -8 0 9.00 3.10 -3 -8 0 7.70 2.60 -4 -8 0 -2.50 2.30 -4 -8 0 -0.20 2.00 4 -8 0 -0.60 2.50 -4 8 0 0.20 1.70 -5 -8 0 109.29 7.30 -5 -8 0 98.09 5.60 5 -8 0 109.29 7.80 -5 8 0 107.29 5.80 6 -8 0 21.50 4.80 -6 -8 0 13.50 2.90 -6 -8 0 12.10 4.00 -6 8 0 17.60 3.40 -7 -8 0 32.90 5.80 7 -8 0 41.60 6.10 -7 -8 0 46.10 4.80 -7 8 0 48.30 5.30 -8 -8 0 -2.70 3.40 8 -8 0 -1.10 3.80 -8 8 0 -1.30 2.80 0 9 0 1.40 1.80 1 -9 0 297.47 11.70 -1 9 0 313.57 9.30 2 -9 0 260.17 10.70 -2 -9 0 245.88 9.30 -2 9 0 231.28 7.80 3 -9 0 4.40 3.30 -3 -9 0 -1.00 2.10 -3 -9 0 -0.40 2.10 4 -9 0 -0.40 3.00 -4 -9 0 1.60 2.70 -4 -9 0 -0.90 2.10 -4 9 0 2.70 2.00 -5 -9 0 0.70 2.20 -5 -9 0 1.10 3.00 5 -9 0 -0.20 2.70 -5 9 0 -2.10 2.00 6 -9 0 20.70 4.80 -6 -9 0 19.90 4.60 -6 -9 0 23.20 3.70 -6 9 0 16.20 3.40 7 -9 0 41.70 6.40 -7 -9 0 44.20 5.90 -7 -9 0 34.80 5.60 -7 9 0 38.70 4.90 -8 -9 0 46.80 6.90 8 -9 0 37.40 6.40 1 -10 0 143.79 8.50 -1 10 0 162.18 6.60 -2 -10 0 194.18 8.50 2 -10 0 181.68 9.90 -2 10 0 184.38 7.20 -3 -10 0 5.70 3.00 -3 -10 0 8.00 2.90 3 -10 0 13.00 4.00 4 -10 0 7.40 3.70 -4 -10 0 14.50 3.30 -4 -10 0 14.20 3.60 -4 10 0 9.50 2.50 -5 -10 0 5.90 2.70 -5 -10 0 6.40 3.50 5 -10 0 4.50 3.60 -5 10 0 9.00 2.80 6 -10 0 6.60 4.00 -6 -10 0 0.40 3.30 -6 -10 0 4.90 2.90 -6 10 0 4.10 3.10 7 -10 0 -2.30 3.90 -7 -10 0 6.80 4.40 -1 -11 0 16.00 3.90 1 -11 0 20.60 4.80 2 -11 0 -0.30 3.10 -2 -11 0 -1.80 2.70 -3 -11 0 1.10 2.80 3 -11 0 0.50 3.30 -4 -11 0 1.20 2.80 4 -11 0 -1.00 3.60 -4 -11 0 -1.10 2.70 -4 11 0 2.60 3.50 -5 -11 0 9.10 3.60 -5 -11 0 4.30 3.00 5 -11 0 2.90 4.10 6 -11 0 25.30 5.60 -6 -11 0 36.70 5.60 -1 -12 0 14.90 4.10 1 -12 0 8.90 4.10 -2 -12 0 81.59 7.10 2 -12 0 53.89 7.10 -3 -12 0 0.00 2.80 3 -12 0 4.00 3.80 -4 -12 0 9.60 3.70 4 -12 0 14.00 4.90 -5 -12 0 48.60 6.10 -5 -12 0 58.39 6.10 5 -12 0 44.10 7.10 0 -13 0 -3.20 3.20 1 -13 0 1.30 3.50 -1 -13 0 3.80 3.70 2 -13 0 7.40 4.60 -2 -13 0 14.70 3.90 -3 -13 0 1.80 3.50 3 -13 0 1.40 4.10 -4 -13 0 1.00 3.50 4 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18 37.00 6.00 4 -7 -18 12.40 4.80 3 -7 -18 3.30 4.10 2 -7 -18 5.40 4.60 1 -7 -18 52.59 7.40 0 -7 -18 31.00 6.30 -1 -7 -18 -3.70 3.60 1 -7 18 2.90 3.50 2 -7 18 24.30 5.20 -2 -7 -18 28.70 6.10 1 -8 -18 27.00 5.90 -6 0 19 2.00 3.20 3 0 -19 19.20 3.70 2 0 -19 2.30 2.70 1 0 -19 226.08 10.10 0 0 -19 -1.10 3.00 -1 0 -19 17.90 4.30 -2 0 -19 -2.80 3.10 -3 0 -19 7.90 4.60 3 0 19 10.30 3.70 -4 0 -19 -0.70 3.90 4 0 19 1.80 3.30 -6 -1 19 72.39 7.70 -6 1 19 83.79 8.50 -5 -1 19 5.00 3.50 3 -1 -19 5.50 3.00 3 1 -19 3.30 3.90 2 -1 -19 122.89 7.50 2 1 -19 117.09 7.00 1 -1 -19 3.10 3.10 1 1 -19 2.10 3.00 0 -1 -19 15.90 4.40 0 1 -19 15.00 4.00 -1 -1 -19 35.90 5.60 -1 1 -19 33.30 5.40 2 -1 19 123.79 7.30 -2 -1 -19 97.99 8.70 -2 1 -19 88.39 8.10 -3 -1 -19 50.19 7.10 3 -1 19 58.49 6.10 -3 1 -19 52.89 7.20 4 -1 19 12.50 4.30 -4 -1 -19 19.60 5.50 -4 1 -19 23.60 5.50 -6 -2 19 1.40 3.40 -5 -2 19 16.40 4.40 4 -2 -19 15.40 3.70 -4 -2 19 19.80 4.10 3 -2 -19 0.90 2.90 2 -2 -19 66.99 6.50 2 2 -19 60.79 5.40 1 -2 -19 15.70 4.20 1 2 -19 21.20 4.10 0 -2 -19 -4.80 3.20 0 2 -19 1.10 3.00 -1 -2 -19 37.00 5.80 -1 2 -19 44.20 5.70 -2 -2 -19 75.89 8.10 2 -2 19 95.69 6.90 -2 2 -19 88.19 8.20 -3 -2 -19 22.70 5.70 3 -2 19 10.20 3.90 -3 2 -19 21.00 5.20 4 -2 19 14.80 4.50 -4 -2 -19 23.70 5.50 -4 2 -19 10.40 4.50 -5 -3 19 6.50 3.50 4 -3 -19 39.90 5.20 -4 -3 19 42.30 5.40 3 -3 -19 103.59 7.30 -3 -3 19 89.29 6.50 2 -3 -19 3.20 3.20 1 -3 -19 3.10 3.50 0 -3 -19 72.89 7.40 -1 -3 -19 33.00 5.50 2 -3 19 43.80 5.30 -2 -3 -19 42.70 6.60 -3 -3 -19 2.50 4.30 3 -3 19 -2.60 2.70 -5 -4 19 1.90 3.10 4 -4 -19 70.19 6.70 -4 -4 19 67.89 6.30 -3 -4 19 0.00 2.50 3 -4 -19 1.20 3.30 2 -4 -19 15.40 4.60 1 -4 -19 53.39 6.60 0 -4 -19 3.10 4.10 -1 -4 -19 48.00 6.90 2 -4 19 7.30 3.50 -2 -4 -19 8.30 4.70 3 -4 19 14.20 4.40 -3 -4 -19 28.00 6.20 4 -5 -19 7.60 4.00 3 -5 -19 -2.90 3.20 2 -5 -19 71.79 7.40 1 -5 -19 100.09 8.90 0 -5 -19 18.80 5.10 -1 -5 -19 49.20 7.10 -2 -5 -19 16.10 5.20 2 -5 19 24.90 4.80 3 -6 -19 8.20 4.10 2 -6 -19 6.60 4.30 1 -6 -19 -0.60 4.00 0 -6 -19 2.70 4.20 -1 -6 -19 18.80 5.40 1 -7 -19 4.30 4.10 -5 0 20 1.80 3.30 2 0 -20 94.19 7.30 1 0 -20 -0.70 3.00 0 0 -20 -0.10 3.20 -1 0 -20 -1.90 3.50 -2 0 -20 22.30 5.40 -3 0 -20 -1.30 3.80 -5 -1 20 20.00 4.80 3 -1 -20 3.10 3.10 2 -1 -20 3.90 3.20 2 1 -20 4.00 3.10 1 -1 -20 185.78 9.70 1 1 -20 201.38 9.70 0 -1 -20 -0.50 3.50 0 1 -20 1.80 3.30 -1 -1 -20 15.40 4.70 -1 1 -20 12.90 4.40 -2 -1 -20 8.00 4.20 -2 1 -20 5.40 4.20 -3 -1 -20 69.99 8.00 -3 1 -20 65.49 8.00 -5 -2 20 -0.50 3.50 -4 -2 20 0.70 3.20 3 -2 -20 -0.90 3.00 2 -2 -20 58.39 6.20 2 2 -20 60.29 8.90 1 -2 -20 63.59 6.70 1 2 -20 60.19 6.10 0 -2 -20 23.90 4.80 0 2 -20 23.80 4.70 -1 -2 -20 3.60 4.20 -1 2 -20 14.80 4.40 -2 -2 -20 13.00 5.00 -2 2 -20 11.30 4.20 -3 -2 -20 46.70 7.10 -3 2 -20 39.10 6.30 -4 -3 20 48.70 5.90 -3 -3 20 -0.80 2.50 3 -3 -20 -3.20 2.90 2 -3 -20 56.19 6.50 1 -3 -20 -7.30 3.20 0 -3 -20 -1.80 3.70 -1 -3 -20 4.90 4.50 -2 -3 -20 147.19 10.10 4 -4 -20 1.90 3.50 3 -4 -20 -1.40 3.40 2 -4 -20 0.70 3.70 1 -4 -20 23.90 5.30 0 -4 -20 -2.50 3.80 -1 -4 -20 13.70 4.70 -2 -4 -20 54.69 7.80 3 -5 -20 17.50 4.80 2 -5 -20 5.00 4.30 1 -5 -20 3.80 4.10 0 -5 -20 37.50 6.50 -1 -5 -20 2.20 4.60 2 0 -21 -1.80 3.20 1 0 -21 100.29 8.10 0 0 -21 -1.90 3.30 -1 0 -21 143.39 9.70 2 -1 -21 5.60 3.60 1 -1 -21 24.00 4.80 1 1 -21 24.60 4.70 0 -1 -21 121.69 8.60 0 1 -21 130.89 8.90 -1 -1 -21 9.10 4.60 -1 1 -21 18.30 4.70 3 -2 -21 63.09 7.60 2 -2 -21 5.40 3.70 1 -2 -21 34.00 5.50 1 2 -21 34.10 5.20 0 -2 -21 45.60 6.70 0 2 -21 38.10 5.90 -1 -2 -21 19.70 5.10 -1 2 -21 21.10 5.10 3 -3 -21 8.10 4.00 2 -3 -21 23.90 5.00 1 -3 -21 9.90 4.40 0 -3 -21 10.10 4.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_res_file ; TITL AB-135 in P2(1)/n shelx.res created by SHELXL-2018/3 at 09:59:31 on 25-May-2018 CELL 0.71073 8.7661 11.2908 17.5089 90.000 96.021 90.000 ZERR 4.00 0.0002 0.0003 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 72 64 4 28 12 MERG 2 EQIV $1 x-1, y, z HTAB C4 O3_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C5 O2_$2 HTAB C7 O1_$2 HTAB C11 O4 EQIV $3 -x+1/2, y-1/2, -z+3/2 HTAB C12 O7_$3 HTAB C12 O5_$3 HTAB C12 F1 HTAB C12 F2 EQIV $4 -x+3/2, y+1/2, -z+3/2 HTAB C16 F3_$4 OMIT 1 0 1 OMIT 0 1 1 OMIT -1 0 1 OMIT 0 0 2 OMIT 1 1 0 OMIT 3 6 3 OMIT -3 0 3 OMIT 1 1 1 FMAP 2 PLAN 3 SIZE 0.300 0.320 0.350 ACTA BOND $H CONF L.S. 13 TEMP -123.00 WGHT 0.039100 0.846200 FVAR 0.54322 C1 1 0.394734 0.496106 0.677775 11.00000 0.01687 0.01548 = 0.01300 -0.00056 0.00230 -0.00093 C2 1 0.346358 0.364537 0.655120 11.00000 0.01811 0.01630 = 0.01388 -0.00016 0.00513 -0.00179 C3 1 0.175165 0.353922 0.660612 11.00000 0.01724 0.01488 = 0.02541 -0.00197 0.00820 -0.00422 AFIX 43 H3 2 0.125910 0.313775 0.698918 11.00000 -1.20000 AFIX 0 C4 1 0.109261 0.412747 0.600437 11.00000 0.01626 0.01667 = 0.02436 -0.00483 0.00328 -0.00252 AFIX 43 H4 2 0.002414 0.423058 0.586488 11.00000 -1.20000 AFIX 0 C5 1 0.239475 0.460402 0.558240 11.00000 0.01727 0.01691 = 0.01532 -0.00108 0.00019 0.00083 AFIX 13 H5 2 0.211134 0.478143 0.502604 11.00000 -1.20000 AFIX 0 C6 1 0.316823 0.565801 0.606534 11.00000 0.01855 0.01500 = 0.01338 -0.00049 0.00217 -0.00119 C7 1 0.465803 0.618374 0.575445 11.00000 0.01993 0.01684 = 0.01790 0.00273 0.00386 -0.00092 AFIX 13 H7 2 0.450625 0.648514 0.521478 11.00000 -1.20000 AFIX 0 C8 1 0.537853 0.706975 0.634299 11.00000 0.02256 0.01840 = 0.02678 -0.00069 0.00598 -0.00684 AFIX 43 H8 2 0.534938 0.790901 0.630565 11.00000 -1.20000 AFIX 0 C9 1 0.605370 0.643101 0.691720 11.00000 0.02126 0.02219 = 0.02045 -0.00380 -0.00016 -0.00710 AFIX 43 H9 2 0.663054 0.671359 0.737022 11.00000 -1.20000 AFIX 0 C10 1 0.570770 0.514908 0.669592 11.00000 0.01911 0.01842 = 0.01437 -0.00186 0.00238 -0.00484 C11 1 0.674127 0.414883 0.700145 11.00000 0.01725 0.02303 = 0.01796 -0.00139 -0.00028 -0.00290 AFIX 23 H11A 2 0.777907 0.426465 0.683886 11.00000 -1.20000 H11B 2 0.683028 0.415179 0.756980 11.00000 -1.20000 AFIX 0 C12 1 0.457394 0.273646 0.691213 11.00000 0.01806 0.01976 = 0.01926 0.00266 0.00641 -0.00108 AFIX 23 H12A 2 0.456518 0.274715 0.747704 11.00000 -1.20000 H12B 2 0.426248 0.193647 0.672394 11.00000 -1.20000 AFIX 0 C13 1 0.682106 0.243661 0.616962 11.00000 0.01713 0.02414 = 0.02248 -0.00083 0.00195 0.00075 C14 1 0.615621 0.123607 0.587859 11.00000 0.02256 0.02676 = 0.03150 -0.00479 0.00482 0.00189 C15 1 0.343240 0.528404 0.754876 11.00000 0.02538 0.01495 = 0.01607 0.00056 0.00423 -0.00046 C16 1 0.413216 0.544406 0.887821 11.00000 0.04698 0.03037 = 0.01138 -0.00250 0.00568 0.00370 AFIX 137 H16A 2 0.502378 0.535376 0.926090 11.00000 -1.50000 H16B 2 0.332265 0.489567 0.899623 11.00000 -1.50000 H16C 2 0.375106 0.625921 0.888922 11.00000 -1.50000 AFIX 0 C17 1 0.206097 0.666540 0.617492 11.00000 0.02109 0.01719 = 0.01314 0.00162 0.00303 -0.00121 C18 1 -0.037253 0.744266 0.571522 11.00000 0.02990 0.02634 = 0.04088 -0.00804 -0.00739 0.01154 AFIX 137 H18A 2 -0.136339 0.716249 0.547019 11.00000 -1.50000 H18B 2 -0.001422 0.810491 0.541928 11.00000 -1.50000 H18C 2 -0.048909 0.770680 0.623910 11.00000 -1.50000 AFIX 0 N1 3 0.612263 0.300342 0.671373 11.00000 0.01576 0.01800 = 0.01837 0.00140 0.00163 -0.00100 O1 4 0.350514 0.367558 0.573482 11.00000 0.01763 0.01573 = 0.01414 -0.00155 0.00341 -0.00008 O2 4 0.570828 0.521591 0.587564 11.00000 0.01697 0.02012 = 0.01481 0.00054 0.00387 -0.00207 O3 4 0.798978 0.276226 0.591888 11.00000 0.02592 0.04241 = 0.05092 -0.01560 0.02054 -0.01051 O4 4 0.457602 0.518210 0.811855 11.00000 0.02974 0.02870 = 0.01165 -0.00201 0.00195 0.00040 O5 4 0.214953 0.555468 0.764980 11.00000 0.02961 0.03221 = 0.02151 -0.00146 0.00855 0.00954 O6 4 0.072919 0.649222 0.574035 11.00000 0.02123 0.01941 = 0.02611 -0.00388 -0.00233 0.00440 O7 4 0.234897 0.754103 0.655171 11.00000 0.02961 0.02098 = 0.02716 -0.00692 -0.00195 0.00351 F1 5 0.608955 0.045885 0.644973 11.00000 0.05149 0.02178 = 0.05230 0.00556 0.00017 0.00287 F2 5 0.475664 0.130744 0.550608 11.00000 0.02789 0.03200 = 0.04271 -0.01025 -0.00726 -0.00238 F3 5 0.704762 0.076212 0.539227 11.00000 0.04047 0.04963 = 0.06622 -0.03406 0.02253 -0.00478 HKLF 4 REM AB-135 in P2(1)/n REM wR2 = 0.0908, GooF = S = 1.011, Restrained GooF = 1.011 for all data REM R1 = 0.0364 for 2739 Fo > 4sig(Fo) and 0.0518 for all 3496 data REM 264 parameters refined using 0 restraints END WGHT 0.0391 0.8462 REM Highest difference peak 0.298, deepest hole -0.254, 1-sigma level 0.048 Q1 1 0.2631 0.6051 0.6190 11.00000 0.05 0.30 Q2 1 0.2806 0.5162 0.5809 11.00000 0.05 0.28 Q3 1 0.3471 0.5338 0.6466 11.00000 0.05 0.27 ; _shelx_res_checksum 59927 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy C C1 0.39473(17) 0.49611(14) 0.67777(9) 0.0151(3) Uani d 1 C C2 0.34636(17) 0.36454(14) 0.65512(9) 0.0159(3) Uani d 1 C C3 0.17517(18) 0.35392(15) 0.66061(10) 0.0188(4) Uani d 1 H H3 0.125910 0.313775 0.698918 0.023 Uiso calc 1 C C4 0.10926(18) 0.41275(15) 0.60044(9) 0.0190(4) Uani d 1 H H4 0.002414 0.423058 0.586488 0.023 Uiso calc 1 C C5 0.23948(17) 0.46040(14) 0.55824(9) 0.0166(3) Uani d 1 H H5 0.211134 0.478143 0.502604 0.020 Uiso calc 1 C C6 0.31682(17) 0.56580(14) 0.60653(9) 0.0156(3) Uani d 1 C C7 0.46580(18) 0.61837(14) 0.57545(9) 0.0181(3) Uani d 1 H H7 0.450625 0.648514 0.521478 0.022 Uiso calc 1 C C8 0.53785(19) 0.70697(16) 0.63430(10) 0.0223(4) Uani d 1 H H8 0.534938 0.790901 0.630565 0.027 Uiso calc 1 C C9 0.60537(19) 0.64310(16) 0.69172(10) 0.0215(4) Uani d 1 H H9 0.663054 0.671359 0.737022 0.026 Uiso calc 1 C C10 0.57077(18) 0.51491(15) 0.66959(9) 0.0173(3) Uani d 1 C C11 0.67413(18) 0.41488(15) 0.70014(9) 0.0196(4) Uani d 1 H H11A 0.777907 0.426465 0.683886 0.023 Uiso calc 1 H H11B 0.683028 0.415179 0.756980 0.023 Uiso calc 1 C C12 0.45739(18) 0.27365(15) 0.69121(9) 0.0187(3) Uani d 1 H H12A 0.456518 0.274715 0.747704 0.022 Uiso calc 1 H H12B 0.426248 0.193647 0.672394 0.022 Uiso calc 1 C C13 0.68211(18) 0.24366(16) 0.61696(10) 0.0213(4) Uani d 1 C C14 0.61562(19) 0.12361(17) 0.58786(11) 0.0268(4) Uani d 1 C C15 0.34324(19) 0.52840(15) 0.75488(9) 0.0187(4) Uani d 1 C C16 0.4132(2) 0.54441(18) 0.88782(9) 0.0294(4) Uani d 1 H H16A 0.502378 0.535376 0.926090 0.044 Uiso calc 1 H H16B 0.332265 0.489567 0.899623 0.044 Uiso calc 1 H H16C 0.375106 0.625921 0.888922 0.044 Uiso calc 1 C C17 0.20610(18) 0.66654(15) 0.61749(9) 0.0171(3) Uani d 1 C C18 -0.0373(2) 0.74427(17) 0.57152(12) 0.0332(5) Uani d 1 H H18A -0.136339 0.716249 0.547019 0.050 Uiso calc 1 H H18B -0.001422 0.810491 0.541928 0.050 Uiso calc 1 H H18C -0.048909 0.770680 0.623910 0.050 Uiso calc 1 N N1 0.61226(15) 0.30034(12) 0.67137(8) 0.0174(3) Uani d 1 O O1 0.35051(12) 0.36756(10) 0.57348(6) 0.0157(2) Uani d 1 O O2 0.57083(12) 0.52159(10) 0.58756(6) 0.0171(3) Uani d 1 O O3 0.79898(15) 0.27623(13) 0.59189(8) 0.0386(4) Uani d 1 O O4 0.45760(13) 0.51821(11) 0.81186(6) 0.0234(3) Uani d 1 O O5 0.21495(14) 0.55547(12) 0.76498(7) 0.0274(3) Uani d 1 O O6 0.07292(13) 0.64922(10) 0.57403(7) 0.0226(3) Uani d 1 O O7 0.23490(14) 0.75410(11) 0.65517(7) 0.0263(3) Uani d 1 F F1 0.60895(14) 0.04589(10) 0.64497(7) 0.0422(3) Uani d 1 F F2 0.47566(12) 0.13074(10) 0.55061(6) 0.0350(3) Uani d 1 F F3 0.70476(14) 0.07621(12) 0.53923(8) 0.0509(4) Uani 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 C1 0.0169(8) 0.0155(8) 0.0130(8) -0.0009(6) 0.0023(6) -0.0006(6) C2 0.0181(8) 0.0163(8) 0.0139(8) -0.0018(6) 0.0051(6) -0.0002(6) C3 0.0172(8) 0.0149(8) 0.0254(9) -0.0042(6) 0.0082(7) -0.0020(7) C4 0.0163(8) 0.0167(9) 0.0244(9) -0.0025(6) 0.0033(6) -0.0048(7) C5 0.0173(8) 0.0169(8) 0.0153(8) 0.0008(6) 0.0002(6) -0.0011(7) C6 0.0185(8) 0.0150(8) 0.0134(8) -0.0012(6) 0.0022(6) -0.0005(6) C7 0.0199(8) 0.0168(9) 0.0179(8) -0.0009(6) 0.0039(6) 0.0027(7) C8 0.0226(9) 0.0184(9) 0.0268(9) -0.0068(7) 0.0060(7) -0.0007(7) C9 0.0213(8) 0.0222(9) 0.0205(9) -0.0071(7) -0.0002(7) -0.0038(7) C10 0.0191(8) 0.0184(9) 0.0144(8) -0.0048(6) 0.0024(6) -0.0019(7) C11 0.0173(8) 0.0230(9) 0.0180(8) -0.0029(7) -0.0003(6) -0.0014(7) C12 0.0181(8) 0.0198(9) 0.0193(8) -0.0011(7) 0.0064(6) 0.0027(7) C13 0.0171(8) 0.0241(10) 0.0225(9) 0.0007(7) 0.0020(7) -0.0008(7) C14 0.0226(9) 0.0268(10) 0.0315(10) 0.0019(7) 0.0048(7) -0.0048(8) C15 0.0254(9) 0.0149(8) 0.0161(8) -0.0005(7) 0.0042(7) 0.0006(7) C16 0.0470(11) 0.0304(11) 0.0114(8) 0.0037(9) 0.0057(8) -0.0025(8) C17 0.0211(8) 0.0172(9) 0.0131(8) -0.0012(6) 0.0030(6) 0.0016(7) C18 0.0299(10) 0.0263(11) 0.0409(11) 0.0115(8) -0.0074(8) -0.0080(9) N1 0.0158(7) 0.0180(7) 0.0184(7) -0.0010(5) 0.0016(5) 0.0014(6) O1 0.0176(5) 0.0157(6) 0.0141(6) -0.0001(4) 0.0034(4) -0.0016(4) O2 0.0170(6) 0.0201(6) 0.0148(6) -0.0021(5) 0.0039(4) 0.0005(5) O3 0.0259(7) 0.0424(9) 0.0509(9) -0.0105(6) 0.0205(6) -0.0156(7) O4 0.0297(7) 0.0287(7) 0.0116(6) 0.0004(5) 0.0019(5) -0.0020(5) O5 0.0296(7) 0.0322(8) 0.0215(6) 0.0095(6) 0.0086(5) -0.0015(5) O6 0.0212(6) 0.0194(6) 0.0261(6) 0.0044(5) -0.0023(5) -0.0039(5) O7 0.0296(7) 0.0210(7) 0.0272(7) 0.0035(5) -0.0020(5) -0.0069(5) F1 0.0515(7) 0.0218(6) 0.0523(8) 0.0029(5) 0.0002(6) 0.0056(5) F2 0.0279(6) 0.0320(6) 0.0427(7) -0.0024(5) -0.0073(5) -0.0102(5) F3 0.0405(7) 0.0496(8) 0.0662(9) -0.0048(6) 0.0225(6) -0.0341(7) 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 C15 C1 C6 116.28(13) C15 C1 C10 115.76(13) C6 C1 C10 102.03(12) C15 C1 C2 110.64(13) C6 C1 C2 100.86(12) C10 C1 C2 109.99(12) O1 C2 C12 110.57(12) O1 C2 C3 101.16(12) C12 C2 C3 121.25(13) O1 C2 C1 101.14(11) C12 C2 C1 112.92(13) C3 C2 C1 107.37(13) C4 C3 C2 105.15(14) C4 C3 H3 127.4 C2 C3 H3 127.4 C3 C4 C5 106.05(14) C3 C4 H4 127.0 C5 C4 H4 127.0 O1 C5 C4 100.37(12) O1 C5 C6 101.94(12) C4 C5 C6 108.05(13) O1 C5 H5 114.9 C4 C5 H5 114.9 C6 C5 H5 114.9 C17 C6 C1 120.34(13) C17 C6 C5 112.90(13) C1 C6 C5 100.09(12) C17 C6 C7 108.88(13) C1 C6 C7 98.94(12) C5 C6 C7 115.09(13) O2 C7 C8 100.74(12) O2 C7 C6 101.77(12) C8 C7 C6 108.18(13) O2 C7 H7 114.8 C8 C7 H7 114.8 C6 C7 H7 114.8 C9 C8 C7 106.02(15) C9 C8 H8 127.0 C7 C8 H8 127.0 C8 C9 C10 105.27(14) C8 C9 H9 127.4 C10 C9 H9 127.4 O2 C10 C11 109.26(13) O2 C10 C9 100.58(13) C11 C10 C9 121.69(14) O2 C10 C1 101.56(11) C11 C10 C1 115.03(13) C9 C10 C1 106.00(13) N1 C11 C10 110.50(12) N1 C11 H11A 109.5 C10 C11 H11A 109.5 N1 C11 H11B 109.5 C10 C11 H11B 109.5 H11A C11 H11B 108.1 N1 C12 C2 109.50(13) N1 C12 H12A 109.8 C2 C12 H12A 109.8 N1 C12 H12B 109.8 C2 C12 H12B 109.8 H12A C12 H12B 108.2 O3 C13 N1 125.15(16) O3 C13 C14 116.83(15) N1 C13 C14 117.88(14) F3 C14 F2 106.54(15) F3 C14 F1 106.87(16) F2 C14 F1 107.23(14) F3 C14 C13 109.82(14) F2 C14 C13 113.97(15) F1 C14 C13 112.02(15) O5 C15 O4 123.51(15) O5 C15 C1 124.53(15) O4 C15 C1 111.90(14) O4 C16 H16A 109.5 O4 C16 H16B 109.5 H16A C16 H16B 109.5 O4 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 O7 C17 O6 123.57(15) O7 C17 C6 125.81(15) O6 C17 C6 110.43(13) O6 C18 H18A 109.5 O6 C18 H18B 109.5 H18A C18 H18B 109.5 O6 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C13 N1 C12 124.77(14) C13 N1 C11 118.78(13) C12 N1 C11 114.62(13) C2 O1 C5 96.60(11) C7 O2 C10 96.93(11) C15 O4 C16 114.29(13) C17 O6 C18 116.74(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C15 1.512(2) C1 C6 1.569(2) C1 C10 1.579(2) C1 C2 1.584(2) C2 O1 1.4341(19) C2 C12 1.507(2) C2 C3 1.519(2) C3 C4 1.326(2) C3 H3 0.9500 C4 C5 1.522(2) C4 H4 0.9500 C5 O1 1.4363(19) C5 C6 1.572(2) C5 H5 1.0000 C6 C17 1.520(2) C6 C7 1.582(2) C7 O2 1.4303(19) C7 C8 1.525(2) C7 H7 1.0000 C8 C9 1.325(2) C8 H8 0.9500 C9 C10 1.521(2) C9 H9 0.9500 C10 O2 1.4382(19) C10 C11 1.510(2) C11 N1 1.471(2) C11 H11A 0.9900 C11 H11B 0.9900 C12 N1 1.467(2) C12 H12A 0.9900 C12 H12B 0.9900 C13 O3 1.213(2) C13 N1 1.347(2) C13 C14 1.541(3) C14 F3 1.327(2) C14 F2 1.330(2) C14 F1 1.336(2) C15 O5 1.196(2) C15 O4 1.343(2) C16 O4 1.455(2) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 O7 1.2006(19) C17 O6 1.3393(19) C18 O6 1.441(2) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 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 C4 H4 O3 1_455 0.95 2.44 3.116(2) 127.6 yes C5 H5 O2 3_666 1.00 2.60 3.1960(19) 117.9 yes C7 H7 O1 3_666 1.00 2.54 3.2091(19) 124.2 yes C11 H11B O4 . 0.99 2.57 3.093(2) 113.3 yes C12 H12A O7 2_546 0.99 2.52 3.328(2) 138.4 yes C12 H12B O5 2_546 0.99 2.34 3.030(2) 126.5 yes C12 H12B F1 . 0.99 2.40 3.043(2) 122.4 yes C12 H12B F2 . 0.99 2.33 2.962(2) 120.7 yes C16 H16A F3 2_656 0.98 2.62 3.475(2) 146.4 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 C15 C1 C2 O1 158.98(12) C6 C1 C2 O1 35.33(13) C10 C1 C2 O1 -71.87(14) C15 C1 C2 C12 -82.85(16) C6 C1 C2 C12 153.50(12) C10 C1 C2 C12 46.30(16) C15 C1 C2 C3 53.42(16) C6 C1 C2 C3 -70.24(14) C10 C1 C2 C3 -177.43(13) O1 C2 C3 C4 -32.33(16) C12 C2 C3 C4 -154.93(15) C1 C2 C3 C4 73.22(16) C2 C3 C4 C5 -0.44(17) C3 C4 C5 O1 32.93(16) C3 C4 C5 C6 -73.38(16) C15 C1 C6 C17 4.8(2) C10 C1 C6 C17 -122.10(14) C2 C1 C6 C17 124.52(14) C15 C1 C6 C5 -119.37(14) C10 C1 C6 C5 113.70(12) C2 C1 C6 C5 0.31(13) C15 C1 C6 C7 122.99(14) C10 C1 C6 C7 -3.95(14) C2 C1 C6 C7 -117.33(12) O1 C5 C6 C17 -165.16(12) C4 C5 C6 C17 -59.95(17) O1 C5 C6 C1 -35.94(13) C4 C5 C6 C1 69.27(14) O1 C5 C6 C7 68.99(15) C4 C5 C6 C7 174.20(13) C17 C6 C7 O2 165.38(12) C1 C6 C7 O2 38.92(14) C5 C6 C7 O2 -66.71(16) C17 C6 C7 C8 59.79(16) C1 C6 C7 C8 -66.68(15) C5 C6 C7 C8 -172.31(13) O2 C7 C8 C9 -31.04(16) C6 C7 C8 C9 75.27(16) C7 C8 C9 C10 -1.76(17) C8 C9 C10 O2 33.85(16) C8 C9 C10 C11 154.49(15) C8 C9 C10 C1 -71.55(16) C15 C1 C10 O2 -158.88(13) C6 C1 C10 O2 -31.61(14) C2 C1 C10 O2 74.81(14) C15 C1 C10 C11 83.27(17) C6 C1 C10 C11 -149.45(13) C2 C1 C10 C11 -43.04(17) C15 C1 C10 C9 -54.19(17) C6 C1 C10 C9 73.08(14) C2 C1 C10 C9 179.49(12) O2 C10 C11 N1 -65.07(16) C9 C10 C11 N1 178.56(14) C1 C10 C11 N1 48.35(17) O1 C2 C12 N1 57.13(17) C3 C2 C12 N1 175.15(14) C1 C2 C12 N1 -55.37(17) O3 C13 C14 F3 0.8(2) N1 C13 C14 F3 -175.17(15) O3 C13 C14 F2 -118.68(18) N1 C13 C14 F2 65.4(2) O3 C13 C14 F1 119.35(18) N1 C13 C14 F1 -56.6(2) C6 C1 C15 O5 35.8(2) C10 C1 C15 O5 155.57(16) C2 C1 C15 O5 -78.4(2) C6 C1 C15 O4 -146.90(14) C10 C1 C15 O4 -27.14(19) C2 C1 C15 O4 98.85(15) C1 C6 C17 O7 58.2(2) C5 C6 C17 O7 176.13(15) C7 C6 C17 O7 -54.7(2) C1 C6 C17 O6 -126.65(15) C5 C6 C17 O6 -8.77(18) C7 C6 C17 O6 120.36(14) O3 C13 N1 C12 167.96(17) C14 C13 N1 C12 -16.5(2) O3 C13 N1 C11 4.3(3) C14 C13 N1 C11 179.81(14) C2 C12 N1 C13 -101.78(18) C2 C12 N1 C11 62.52(17) C10 C11 N1 C13 106.74(16) C10 C11 N1 C12 -58.57(17) C12 C2 O1 C5 -178.88(12) C3 C2 O1 C5 51.41(13) C1 C2 O1 C5 -59.02(12) C4 C5 O1 C2 -51.23(13) C6 C5 O1 C2 59.90(13) C8 C7 O2 C10 50.57(13) C6 C7 O2 C10 -60.77(13) C11 C10 O2 C7 179.05(12) C9 C10 O2 C7 -51.80(13) C1 C10 O2 C7 57.12(13) O5 C15 O4 C16 -0.7(2) C1 C15 O4 C16 -178.05(14) O7 C17 O6 C18 2.2(2) C6 C17 O6 C18 -173.02(14) _cod_database_fobs_code 2242679