#------------------------------------------------------------------------------ #$Date: 2024-12-18 04:09:02 +0100 (Wed, 18 Dec 2024) $ #$Revision: 296913 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023337.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_2023337 loop_ _publ_author_name 'Gurbanov, Atash V.' 'H\"okelek, Tuncer' 'Mammadova, Gunay Z.' 'Hasanov, Khudayar I.' 'Javadzade, Tahir A.' 'Belay, Alebel N.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of supramolecular aggregate of 2,2,6,6-tetramethylpiperidin-1-ium bromide with 1,2,3,4-tetrafluoro-5,6-diiodobenzene ; _journal_coeditor_code YZ2062 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024011502 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C9 H20 N +, Br -, C6 F4 I2' _chemical_formula_moiety 'C9 H20 N +, Br -, C6 F4 I2' _chemical_formula_sum 'C15 H20 Br F4 I2 N' _chemical_formula_weight 624.03 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 108.5330(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 29.0324(8) _cell_length_b 9.1477(2) _cell_length_c 15.0296(4) _cell_measurement_reflns_used 8061 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.42 _cell_measurement_theta_min 2.35 _cell_volume 3784.56(17) _computing_cell_refinement ; SAINT (Bruker, 2014) ; _computing_data_collection ; APEX4 (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2014) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2019/1 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2019/1 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.994 _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 0.0217 _diffrn_reflns_av_unetI/netI 0.0213 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 14152 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.456 _diffrn_reflns_theta_min 2.622 _exptl_absorpt_coefficient_mu 5.469 _exptl_absorpt_correction_T_max 0.4230 _exptl_absorpt_correction_T_min 0.3418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.190 _exptl_crystal_description prism _exptl_crystal_F_000 2352 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.190 _refine_diff_density_max 1.503 _refine_diff_density_min -0.694 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 3877 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0262 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+23.4044P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.0692 _reflns_number_gt 3480 _reflns_number_total 3877 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yz2062.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2023337 _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 0.342 _shelx_estimated_absorpt_t_max 0.423 _shelx_hkl_file ; 2 0 0 -0.50 0.10 2 0 0 -0.60 0.10 2 0 0 -0.60 0.10 -2 0 0 -0.60 0.10 -2 0 0 -0.60 0.10 -2 0 0 -0.60 0.10 -4 0 0 401.26 7.50 4 0 0 311.77 7.50 4 0 0 339.17 7.40 4 0 0 388.06 7.50 -4 0 0 399.46 7.60 6 0 0 25.90 0.90 -6 0 0 25.90 0.90 -6 0 0 30.20 1.10 -6 0 0 25.90 0.90 6 0 0 26.70 1.10 8 0 0 162.88 3.80 -8 0 0 163.18 3.80 8 0 0 158.98 3.50 -8 0 0 153.48 3.50 -8 0 0 154.78 3.50 -10 0 0 2834.62 55.89 10 0 0 2831.32 55.39 -10 0 0 2687.13 55.99 -10 0 0 2757.32 55.99 10 0 0 2817.72 56.19 -10 0 0 2707.53 55.79 -12 0 0 727.13 16.00 -12 0 0 743.53 15.70 -12 0 0 775.32 15.70 12 0 0 781.42 15.70 -12 0 0 775.72 16.00 12 0 0 789.72 16.10 -14 0 0 1209.28 24.70 -14 0 0 1232.28 25.10 14 0 0 1245.08 24.70 14 0 0 1229.58 25.10 -14 0 0 1225.08 24.70 -14 0 0 1143.69 25.00 -16 0 0 7.50 0.80 -16 0 0 7.20 1.10 16 0 0 7.50 1.10 -16 0 0 5.20 0.90 -18 0 0 104.59 3.00 18 0 0 107.89 3.60 -18 0 0 105.59 3.10 -20 0 0 433.86 9.60 -20 0 0 434.86 9.70 20 0 0 439.66 10.30 -22 0 0 166.28 4.40 22 0 0 158.78 5.00 -22 0 0 162.68 4.50 -24 0 0 612.64 13.20 24 0 0 592.54 14.00 -24 0 0 615.94 13.30 -26 0 0 22.40 1.80 -26 0 0 19.10 1.90 -28 0 0 74.79 3.30 -28 0 0 74.79 3.20 -30 0 0 33.10 2.60 -30 0 0 31.80 2.80 -32 0 0 5.20 1.80 -32 0 0 1.30 1.60 -34 0 0 219.88 6.30 -1 1 0 -1.70 0.20 -1 1 0 -1.70 0.20 3 -1 0 13.00 0.60 -3 -1 0 12.00 0.50 3 -1 0 12.20 0.70 -3 -1 0 14.30 0.70 3 -1 0 15.20 0.60 3 -1 0 12.10 0.60 -3 1 0 12.50 0.70 3 1 0 12.70 0.50 -3 1 0 11.00 0.70 -3 1 0 15.20 0.70 3 1 0 13.70 0.70 -3 1 0 13.70 0.60 5 -1 0 547.65 11.00 -5 -1 0 520.65 10.80 5 -1 0 524.05 11.00 5 -1 0 533.15 11.00 5 -1 0 548.25 10.90 -5 -1 0 536.35 11.00 5 1 0 517.55 10.80 -5 1 0 546.65 11.00 -5 1 0 531.35 11.00 -5 1 0 559.64 10.90 -5 1 0 536.85 10.90 5 1 0 531.15 11.00 7 -1 0 1983.70 38.60 7 -1 0 1981.50 39.10 7 -1 0 1897.01 39.00 7 -1 0 1899.31 38.90 -7 -1 0 1940.51 38.90 -7 -1 0 1843.72 38.40 7 1 0 1922.81 38.90 -7 1 0 1850.11 38.40 -7 1 0 1923.81 38.80 7 1 0 1900.41 38.40 -7 1 0 1958.90 38.90 -7 1 0 1897.81 38.70 9 -1 0 208.28 4.80 -9 -1 0 209.68 4.90 -9 -1 0 206.88 4.50 9 -1 0 210.18 4.80 9 -1 0 206.18 4.70 9 -1 0 207.88 4.60 -9 1 0 216.58 4.60 -9 1 0 212.08 4.80 9 1 0 205.28 4.90 -9 1 0 199.18 4.80 -9 1 0 206.58 4.70 9 1 0 210.78 4.50 11 -1 0 639.34 13.40 -11 -1 0 645.54 13.30 11 -1 0 656.83 13.60 -11 -1 0 636.04 13.40 11 -1 0 665.93 13.40 -11 -1 0 648.34 13.70 -11 1 0 654.33 13.40 -11 1 0 622.94 13.60 -11 1 0 651.63 13.60 -11 1 0 650.03 13.50 11 1 0 643.94 13.30 11 1 0 665.43 13.70 13 -1 0 2.00 0.60 -13 -1 0 3.30 0.70 -13 -1 0 2.00 0.70 -13 -1 0 1.70 0.80 13 -1 0 2.40 0.60 13 -1 0 2.20 0.90 -13 1 0 2.50 0.70 -13 1 0 2.50 0.80 -13 1 0 2.00 0.80 -13 1 0 3.30 0.80 13 1 0 2.30 0.60 13 1 0 4.30 1.00 15 -1 0 2.80 0.90 -15 -1 0 2.80 0.70 -15 -1 0 2.40 0.90 -15 1 0 3.20 0.70 15 1 0 2.90 0.60 15 1 0 4.20 1.00 -17 -1 0 962.50 19.70 17 -1 0 959.90 20.30 -17 -1 0 961.00 19.80 17 -1 0 964.30 19.90 -17 1 0 955.10 19.90 -17 1 0 964.60 19.80 17 1 0 951.10 20.40 -19 -1 0 85.99 2.60 19 -1 0 80.39 3.10 -19 -1 0 82.69 2.70 19 1 0 80.79 3.20 -19 1 0 81.19 2.70 -19 1 0 80.39 2.80 -21 -1 0 23.80 1.80 -21 -1 0 25.30 1.70 21 -1 0 28.70 2.20 -21 1 0 25.80 1.90 21 1 0 24.50 2.30 -21 1 0 22.90 1.80 -23 -1 0 76.89 2.90 -23 -1 0 72.09 2.70 23 1 0 72.69 3.50 -23 1 0 77.59 2.90 -23 1 0 79.29 3.00 -25 -1 0 69.89 2.90 -25 -1 0 67.99 2.80 -25 1 0 71.09 2.90 25 1 0 67.19 3.70 -25 1 0 69.79 3.10 -27 -1 0 265.77 6.70 -27 -1 0 260.97 6.50 -27 1 0 250.47 6.80 -27 1 0 263.07 6.60 -29 -1 0 65.49 3.00 -29 -1 0 63.09 3.20 -29 1 0 60.69 3.30 -29 1 0 67.59 3.10 -31 -1 0 31.50 2.60 -31 -1 0 32.30 2.80 -31 1 0 30.90 2.90 -31 1 0 34.70 2.80 -33 -1 0 3.50 1.70 -33 1 0 1.30 1.80 -33 1 0 3.50 1.80 0 -2 0 877.41 18.30 0 -2 0 868.71 18.00 0 2 0 888.01 17.80 0 2 0 885.21 17.80 2 -2 0 1101.59 23.00 2 -2 0 1173.18 23.10 -2 -2 0 1174.08 23.00 -2 2 0 1097.09 22.80 -2 2 0 1087.59 22.90 4 -2 0 1529.55 30.10 4 -2 0 1458.85 30.10 -4 -2 0 1472.75 29.70 4 -2 0 1477.35 30.00 -4 -2 0 1465.95 30.00 -4 2 0 1467.85 30.00 -4 2 0 1462.55 29.90 4 2 0 1479.65 29.90 6 -2 0 1897.01 37.30 6 -2 0 1867.01 37.50 6 -2 0 1810.52 37.40 6 -2 0 1884.81 37.70 -6 -2 0 1857.91 37.20 -6 -2 0 1815.22 37.40 -6 2 0 1856.01 37.40 -6 2 0 1829.42 37.60 6 2 0 1811.62 37.60 -6 2 0 1889.31 37.30 -6 2 0 1869.21 37.20 6 2 0 1826.92 36.90 8 -2 0 1326.77 26.40 -8 -2 0 1267.07 26.50 -8 -2 0 1312.07 26.10 8 -2 0 1323.47 26.30 8 -2 0 1304.37 26.50 8 -2 0 1295.17 26.40 8 2 0 1282.37 26.50 8 2 0 1310.47 26.10 -8 2 0 1284.27 26.50 -8 2 0 1323.27 26.50 -8 2 0 1310.37 26.40 -8 2 0 1323.87 26.30 10 -2 0 127.19 3.30 10 -2 0 132.39 3.40 -10 -2 0 129.79 3.00 10 -2 0 134.39 3.20 10 -2 0 133.49 3.30 -10 -2 0 132.09 3.40 -10 2 0 133.79 3.30 -10 2 0 126.79 3.40 -10 2 0 130.99 3.40 10 2 0 132.59 3.00 10 2 0 128.89 3.50 -12 -2 0 26.30 1.50 12 -2 0 24.50 1.30 12 -2 0 24.30 1.50 12 -2 0 23.20 1.30 12 -2 0 23.20 1.60 -12 -2 0 24.10 1.10 -12 2 0 23.60 1.50 12 2 0 24.40 1.10 -12 2 0 26.20 1.40 -12 2 0 23.20 1.50 -12 2 0 24.70 1.40 12 2 0 23.00 1.60 14 -2 0 3.20 0.80 14 -2 0 2.50 0.90 -14 -2 0 3.70 0.90 -14 -2 0 2.50 0.60 -14 2 0 3.00 0.80 -14 2 0 3.00 0.90 14 2 0 2.20 0.60 -14 2 0 1.70 0.90 14 2 0 1.60 1.00 -14 2 0 2.30 0.90 16 -2 0 722.73 15.40 -16 -2 0 721.23 15.00 16 -2 0 741.83 15.60 -16 -2 0 737.73 15.30 -16 2 0 734.83 15.50 -16 2 0 715.03 15.40 16 2 0 735.53 15.80 -16 2 0 725.43 15.20 16 2 0 714.13 15.00 -18 -2 0 1141.59 23.10 18 -2 0 1126.79 23.50 -18 -2 0 1123.59 22.90 18 2 0 1118.29 23.70 -18 2 0 1114.29 23.30 -18 2 0 1102.29 23.10 -20 -2 0 16.90 1.50 -20 -2 0 15.90 1.70 20 2 0 16.90 1.80 -20 2 0 18.20 1.50 -20 2 0 17.50 1.90 -22 -2 0 21.50 1.70 -22 -2 0 23.10 1.90 22 2 0 24.80 2.50 -22 2 0 24.00 2.00 -22 2 0 22.10 2.10 -24 -2 0 50.49 2.30 -24 -2 0 52.69 2.50 24 2 0 48.10 3.20 -24 2 0 45.50 2.70 -24 2 0 48.00 2.50 -26 -2 0 59.29 2.80 -26 -2 0 55.59 2.60 -26 2 0 53.79 3.00 -26 2 0 57.69 2.90 -28 -2 0 436.26 10.00 -28 -2 0 451.75 10.20 -28 2 0 439.66 10.50 -28 2 0 423.46 10.20 -30 -2 0 64.89 3.10 -30 -2 0 66.99 3.80 -30 2 0 65.79 3.30 -30 2 0 61.69 3.40 -32 -2 0 44.70 2.80 -32 2 0 46.80 3.30 -32 2 0 48.10 3.20 -1 -3 0 1730.33 35.00 -1 -3 0 1708.13 35.40 1 -3 0 1710.13 35.20 1 -3 0 1713.13 35.60 -1 3 0 1683.63 35.00 -1 3 0 1747.63 34.90 1 3 0 1729.43 35.00 -3 -3 0 492.75 10.20 -3 -3 0 491.75 10.50 3 -3 0 482.25 10.30 3 -3 0 501.85 10.10 3 -3 0 497.05 10.30 -3 3 0 496.65 10.30 -3 3 0 470.65 10.30 -5 -3 0 32.10 1.20 -5 -3 0 34.00 1.20 -5 -3 0 31.70 0.90 5 -3 0 34.30 1.20 5 -3 0 31.00 1.40 5 -3 0 32.10 1.30 5 3 0 31.70 1.30 -5 3 0 31.20 1.40 -5 3 0 31.00 1.40 7 -3 0 95.09 2.60 7 -3 0 92.69 2.60 7 -3 0 94.39 2.40 -7 -3 0 91.59 2.10 -7 -3 0 90.89 2.50 -7 3 0 90.99 2.60 7 3 0 95.39 2.20 7 3 0 92.09 2.60 -7 3 0 93.99 2.70 9 -3 0 134.09 3.50 -9 -3 0 134.29 3.00 9 -3 0 130.49 3.40 -9 -3 0 133.09 3.50 9 -3 0 140.59 3.30 -9 3 0 133.49 3.50 -9 3 0 136.39 3.60 9 3 0 133.99 3.00 9 3 0 134.79 3.50 11 -3 0 1418.26 27.70 11 -3 0 1341.57 27.90 -11 -3 0 1309.17 27.90 -11 -3 0 1343.37 27.40 11 -3 0 1378.76 27.90 -11 3 0 1346.67 27.90 -11 3 0 1384.16 27.90 -11 3 0 1398.26 27.80 11 3 0 1361.96 27.40 11 3 0 1349.77 28.00 -11 3 0 1369.66 27.70 -13 -3 0 445.96 9.50 13 -3 0 457.75 10.10 -13 -3 0 443.66 10.10 13 -3 0 452.05 10.00 13 3 0 463.75 9.60 -13 3 0 474.65 9.90 -13 3 0 464.65 9.90 -13 3 0 460.15 10.10 13 3 0 457.05 10.20 -13 3 0 447.86 10.10 -15 -3 0 143.19 3.40 15 -3 0 139.79 4.00 -15 3 0 140.59 3.80 15 3 0 137.49 4.10 15 3 0 141.99 3.40 -15 3 0 139.49 3.80 -15 3 0 142.99 4.00 -17 -3 0 203.38 4.70 17 -3 0 200.68 5.40 17 3 0 203.98 4.80 -17 3 0 206.68 5.10 -17 3 0 205.98 5.30 17 3 0 207.48 5.60 -17 3 0 208.48 5.20 -19 -3 0 2.80 0.80 -19 3 0 4.40 1.20 -19 3 0 3.80 1.10 19 3 0 4.30 1.40 -21 -3 0 95.09 2.80 -21 -3 0 97.19 3.20 -21 3 0 90.19 3.20 -21 3 0 92.39 3.40 21 3 0 87.69 3.80 -23 -3 0 204.28 5.10 -23 -3 0 214.48 5.40 -23 3 0 204.28 5.50 -23 3 0 206.28 5.80 23 3 0 206.68 6.30 -25 -3 0 156.38 4.50 -25 -3 0 149.49 4.20 -25 3 0 150.88 4.60 -25 3 0 146.39 4.80 25 3 0 148.39 5.40 -27 -3 0 20.40 1.90 -27 -3 0 24.50 2.10 -27 3 0 25.00 2.60 -27 3 0 24.10 2.20 -29 -3 0 4.00 1.40 -29 3 0 3.50 1.70 -29 3 0 4.80 1.80 -31 -3 0 0.30 1.50 -31 3 0 0.50 1.80 -33 -3 0 60.39 3.10 -33 3 0 61.89 3.90 0 -4 0 712.33 14.70 0 -4 0 691.03 14.60 0 4 0 715.93 14.70 0 4 0 705.33 14.80 -2 -4 0 429.76 9.10 2 -4 0 429.66 9.20 2 -4 0 420.56 9.10 -2 -4 0 424.26 9.20 -2 4 0 420.66 9.20 -2 4 0 420.06 9.10 4 -4 0 38.10 1.60 -4 -4 0 40.80 1.50 4 -4 0 40.70 1.70 4 -4 0 41.70 1.40 -4 -4 0 39.40 2.00 -4 4 0 36.60 1.70 -4 4 0 39.30 1.60 -6 -4 0 35.00 1.10 6 -4 0 37.00 1.70 -6 -4 0 36.80 1.40 6 -4 0 37.90 1.40 6 -4 0 35.00 1.60 -6 4 0 34.80 1.70 -8 -4 0 3.10 0.60 -8 -4 0 2.30 0.40 8 -4 0 2.80 0.90 8 -4 0 3.30 0.60 -8 -4 0 4.00 0.80 8 -4 0 2.30 0.70 -8 4 0 3.00 0.80 -8 4 0 3.50 0.90 8 4 0 4.50 0.90 10 -4 0 567.64 12.30 -10 -4 0 568.24 12.30 -10 -4 0 571.04 11.70 10 -4 0 571.84 12.30 10 -4 0 579.74 12.10 -10 4 0 576.54 12.40 -10 4 0 578.94 12.30 10 4 0 573.24 12.30 -12 -4 0 459.85 9.60 12 -4 0 468.75 10.30 -12 -4 0 450.05 10.20 12 4 0 468.65 10.30 -12 4 0 467.25 10.40 12 4 0 479.25 9.70 14 -4 0 104.59 3.30 -14 -4 0 101.39 2.60 -14 -4 0 109.19 3.50 -14 4 0 106.39 3.40 -14 4 0 105.39 3.00 14 4 0 104.99 2.70 14 4 0 103.89 3.40 -16 -4 0 49.20 1.70 16 -4 0 47.10 2.40 16 4 0 48.00 2.60 -16 4 0 48.80 2.10 -16 4 0 49.50 2.50 16 4 0 44.90 1.70 -18 -4 0 81.79 2.40 18 -4 0 80.69 3.20 -18 4 0 79.39 3.20 -18 4 0 84.49 3.20 18 4 0 83.89 3.40 -20 -4 0 36.80 1.80 -20 4 0 33.30 2.50 20 4 0 35.90 2.70 -22 -4 0 169.78 4.30 22 4 0 168.58 5.50 -22 4 0 167.48 5.10 -24 -4 0 209.58 5.20 -24 -4 0 206.98 5.60 -24 4 0 209.28 6.00 -26 -4 0 26.60 2.00 -26 -4 0 24.60 2.40 -26 4 0 21.40 2.20 -28 -4 0 91.29 3.30 -28 4 0 90.89 4.10 -30 -4 0 11.50 1.70 -30 4 0 11.50 2.10 -32 -4 0 10.90 1.70 -32 4 0 7.40 2.10 1 -5 0 55.09 2.00 1 -5 0 57.09 2.00 -1 -5 0 54.49 2.10 -1 -5 0 55.09 2.00 -1 5 0 52.99 2.10 -1 5 0 55.09 2.20 1 5 0 54.89 2.10 -3 -5 0 265.37 6.20 3 -5 0 259.07 6.10 3 -5 0 261.27 5.70 -3 -5 0 261.87 6.00 3 -5 0 268.07 6.10 -3 5 0 255.87 6.10 -3 5 0 259.57 6.20 5 -5 0 1343.77 27.80 -5 -5 0 1392.56 28.40 -5 -5 0 1397.16 27.60 5 -5 0 1403.36 28.30 5 -5 0 1373.06 28.10 -5 -5 0 1394.26 28.10 -5 5 0 1351.06 28.10 -5 5 0 1344.57 28.30 7 -5 0 851.81 18.00 7 -5 0 861.21 17.60 -7 -5 0 868.11 17.30 -7 -5 0 860.61 17.80 -7 5 0 851.51 18.10 -7 5 0 857.71 18.00 -9 -5 0 263.27 5.90 -9 -5 0 257.57 6.00 -9 -5 0 257.37 5.50 9 -5 0 255.17 6.20 -9 5 0 252.97 6.20 -9 5 0 261.77 6.40 9 5 0 261.27 6.10 -11 -5 0 5.40 1.00 11 -5 0 5.60 1.10 -11 -5 0 5.70 0.60 -11 -5 0 5.60 0.70 11 5 0 5.10 1.10 -11 5 0 5.10 1.10 -13 -5 0 3.90 1.00 -13 -5 0 3.50 0.60 13 -5 0 4.40 1.10 -13 5 0 3.20 1.10 13 5 0 3.30 1.20 -15 -5 0 223.88 5.00 15 -5 0 229.68 5.90 15 5 0 225.88 6.00 -15 5 0 224.98 6.00 15 5 0 227.98 5.10 17 -5 0 466.25 10.80 -17 -5 0 468.25 9.90 17 5 0 473.95 11.00 -17 5 0 461.75 10.40 -17 5 0 474.35 10.90 17 5 0 475.45 10.00 -19 -5 0 139.29 3.50 19 -5 0 139.69 4.50 19 5 0 142.49 4.70 -19 5 0 136.89 4.50 -21 -5 0 2.10 0.90 21 -5 0 2.30 1.40 -21 5 0 3.10 1.40 -23 -5 0 23.20 1.70 -23 5 0 26.40 2.60 -25 -5 0 14.10 1.40 -25 5 0 13.00 2.00 -27 -5 0 90.59 3.20 -27 5 0 90.99 4.10 -29 -5 0 136.59 4.10 -29 5 0 127.69 5.00 -31 -5 0 60.49 4.50 0 -6 0 252.87 6.00 0 6 0 257.27 6.20 2 -6 0 179.78 4.50 -2 -6 0 176.48 4.60 -2 -6 0 160.58 4.70 2 -6 0 175.18 4.10 -2 6 0 179.88 4.70 -2 6 0 178.38 4.70 4 -6 0 160.58 4.30 4 -6 0 156.78 3.80 -4 -6 0 162.18 4.10 -4 -6 0 161.78 4.40 -4 6 0 157.68 4.40 -4 6 0 152.48 4.30 -6 -6 0 277.47 6.50 6 -6 0 274.87 6.60 -6 -6 0 281.97 6.90 6 -6 0 278.47 6.20 -6 6 0 278.27 6.80 -10 -6 0 26.90 1.50 10 -6 0 28.40 1.90 -10 -6 0 27.60 1.70 -10 -6 0 24.20 1.00 -10 6 0 26.20 2.10 -12 -6 0 379.06 8.00 -12 -6 0 378.66 8.60 12 -6 0 398.36 9.00 -12 -6 0 375.56 8.80 -12 6 0 392.76 9.20 -14 -6 0 1.00 0.70 14 -6 0 0.60 1.10 -14 -6 0 0.80 0.60 -14 6 0 1.00 1.30 16 -6 0 53.79 2.70 -16 -6 0 50.09 2.00 -16 -6 0 50.89 1.70 -16 6 0 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24.30 18 0 -10 1165.48 24.50 -16 0 10 147.49 3.90 16 0 -10 139.49 3.60 16 0 -10 143.39 4.10 14 0 -10 98.99 3.20 -14 0 10 101.39 3.00 -12 0 10 1.70 0.90 12 0 -10 0.90 1.00 -12 0 10 2.40 0.90 -10 0 10 5.20 1.00 -10 0 10 5.30 1.00 -8 0 10 460.55 9.90 -8 0 10 448.26 9.90 8 0 -10 447.96 9.90 6 0 -10 178.98 4.60 -4 0 10 340.97 8.60 4 0 -10 367.36 8.10 -2 0 10 56.89 3.10 2 0 -10 62.09 2.60 0 0 -10 145.69 4.40 0 0 10 141.19 4.80 2 0 10 310.67 8.30 -2 0 -10 321.87 7.90 4 0 10 142.49 4.90 6 0 10 591.24 13.80 8 0 10 69.29 3.70 -10 0 -10 131.89 5.10 10 0 10 141.89 5.20 12 0 10 19.20 2.60 -12 0 -10 19.70 2.50 14 0 10 8.00 2.30 -14 0 -10 8.00 2.20 -16 0 -10 288.27 8.80 16 0 10 325.37 9.20 -18 0 -10 94.69 4.90 18 0 10 96.29 5.10 -20 0 -10 3.70 2.30 20 0 10 2.40 2.30 -22 0 -10 2.90 2.40 22 0 10 -0.50 2.50 -35 -1 10 244.38 6.70 -35 1 10 236.08 6.60 -33 -1 10 3.10 1.50 -33 1 10 1.70 1.60 -31 -1 10 2.70 1.50 -31 1 10 4.70 1.50 29 -1 -10 47.10 3.50 -29 -1 10 48.40 2.70 -29 1 10 46.50 2.70 27 -1 -10 47.80 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14 613.24 15.20 -4 2 14 612.94 13.40 4 2 -14 619.84 14.40 -2 -2 14 22.30 2.80 2 -2 -14 16.20 2.60 2 2 -14 18.40 2.30 -2 2 14 19.40 1.70 -2 2 14 22.60 3.00 0 -2 -14 6.70 2.40 0 -2 14 5.50 2.10 0 2 14 6.50 2.30 0 2 -14 7.80 2.00 2 -2 14 16.60 2.60 -2 -2 -14 10.70 2.80 -2 2 -14 11.80 2.30 2 2 14 16.40 2.70 4 -2 14 3.60 2.10 -4 -2 -14 0.00 2.60 -4 2 -14 1.30 1.80 4 2 14 3.90 2.20 6 -2 14 244.48 7.70 -6 -2 -14 269.27 8.20 -6 2 -14 230.68 7.70 6 2 14 258.47 8.00 8 -2 14 90.59 4.70 -8 -2 -14 94.79 5.40 8 2 14 90.39 4.90 -8 2 -14 82.49 4.80 -10 -2 -14 51.29 4.70 10 -2 14 50.39 4.00 10 2 14 51.19 4.30 -10 2 -14 42.80 4.10 12 -2 14 27.40 3.20 -12 -2 -14 28.80 3.60 12 2 14 27.00 3.40 -12 2 -14 18.00 2.90 -29 -3 14 3.50 1.70 29 -3 -14 4.10 2.30 -29 3 14 4.30 1.80 27 -3 -14 5.40 2.30 -27 -3 14 3.90 1.60 -27 3 14 6.00 1.70 -25 -3 14 3.90 1.40 25 -3 -14 4.00 2.10 -25 3 14 1.90 1.60 23 -3 -14 62.19 4.10 -23 -3 14 62.49 3.10 -23 3 14 66.89 3.20 -21 -3 14 312.87 8.00 21 -3 -14 317.77 8.70 -21 3 14 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4 14 179.28 4.70 8 -4 -14 62.09 4.10 -8 -4 14 60.79 3.80 8 4 -14 60.19 3.00 -8 4 14 64.59 4.40 -8 4 14 60.79 2.50 6 -4 -14 0.80 2.20 -6 -4 14 2.70 1.90 -6 4 14 -1.50 1.00 6 4 -14 0.70 1.40 -6 4 14 0.00 2.20 -4 -4 14 85.29 4.40 4 -4 -14 76.29 4.70 -4 4 14 79.99 4.90 4 4 -14 88.99 3.80 -4 4 14 86.89 2.90 -2 -4 14 15.60 2.50 2 -4 -14 4.70 2.70 -2 4 14 15.90 2.70 -2 4 14 10.70 1.30 2 4 -14 13.90 2.00 0 -4 14 96.09 4.60 0 -4 -14 89.59 5.30 0 4 -14 97.99 4.40 0 4 14 96.99 5.00 -2 -4 -14 176.28 7.00 2 -4 14 175.18 6.20 2 4 14 186.38 6.60 -2 4 -14 180.18 6.10 -4 -4 -14 51.59 4.90 4 -4 14 52.79 3.70 -4 4 -14 47.60 3.70 4 4 14 62.59 4.40 -6 -4 -14 28.20 3.90 6 -4 14 29.40 3.30 6 4 14 34.20 3.90 -6 4 -14 25.10 2.80 -8 -4 -14 27.70 3.90 8 -4 14 33.70 3.50 -8 4 -14 22.80 2.80 8 4 14 28.80 3.30 -10 -4 -14 1.70 3.20 10 -4 14 6.20 2.20 10 4 14 5.90 2.70 -10 4 -14 3.10 2.20 25 -5 -14 79.49 4.70 -25 -5 14 70.99 3.40 -25 5 14 75.89 3.60 23 -5 -14 3.50 2.30 -23 -5 14 2.60 1.60 -23 5 14 5.20 1.70 -21 -5 14 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-4 0 18 24.70 3.70 2 0 -18 113.99 5.40 -2 0 18 121.49 6.30 19 -1 -18 61.49 4.00 -19 -1 18 58.79 3.50 -19 1 18 54.99 3.40 -17 -1 18 36.80 3.10 17 -1 -18 39.20 3.60 -17 1 18 34.90 3.00 15 -1 -18 50.59 3.80 -15 -1 18 47.70 3.30 15 1 -18 41.70 4.40 -15 1 18 47.80 3.20 -13 -1 18 -2.10 2.40 13 -1 -18 -1.40 2.10 -13 -1 18 -0.30 1.60 13 1 -18 1.40 1.80 -13 1 18 0.70 1.60 -13 1 18 0.60 2.50 -11 -1 18 15.50 2.20 11 -1 -18 12.00 2.50 -11 -1 18 13.60 3.10 11 1 -18 10.80 2.20 -11 1 18 14.30 3.30 -11 1 18 12.50 2.10 -9 -1 18 71.49 3.70 -9 -1 18 82.89 5.50 9 -1 -18 76.39 4.60 -9 1 18 73.49 3.60 9 1 -18 72.79 4.30 -9 1 18 76.89 5.60 7 -1 -18 86.69 5.70 -7 -1 18 90.39 5.70 -7 -1 18 97.09 4.10 -7 1 18 93.79 5.90 -7 1 18 86.79 3.80 7 1 -18 86.79 4.60 -5 -1 18 6.60 1.70 -5 -1 18 6.40 2.90 5 -1 -18 -0.20 4.40 -5 1 18 7.30 3.00 5 1 -18 5.60 2.10 -5 1 18 3.80 1.70 -3 -1 18 0.90 2.60 -3 1 18 0.60 1.40 -3 1 18 1.30 2.60 3 1 -18 4.70 2.20 18 -2 -18 143.99 5.70 -18 -2 18 138.49 5.10 -18 2 18 129.59 4.80 -16 -2 18 2.80 1.70 16 -2 -18 2.50 2.30 -16 2 18 1.20 1.70 14 -2 -18 4.30 2.50 -14 -2 18 3.00 1.90 -14 2 18 6.70 1.80 -14 2 18 8.10 3.00 -12 -2 18 -2.60 2.40 -12 -2 18 0.00 1.50 12 -2 -18 -3.00 2.20 -12 2 18 -2.20 1.50 12 2 -18 0.30 1.70 -12 2 18 -0.40 2.70 -10 -2 18 13.50 3.10 10 -2 -18 7.10 2.50 -10 -2 18 7.50 2.00 -10 2 18 8.00 3.10 10 2 -18 10.10 2.10 -10 2 18 7.50 1.80 -8 -2 18 225.18 8.30 8 -2 -18 224.98 7.50 -8 -2 18 234.68 6.80 -8 2 18 230.78 8.70 -8 2 18 222.48 6.30 6 -2 -18 19.50 3.10 -6 -2 18 21.90 3.50 -6 2 18 23.30 2.20 6 2 -18 21.90 2.70 -6 2 18 27.00 3.90 4 -2 -18 0.90 2.60 -4 -2 18 1.60 2.60 -4 2 18 3.10 2.90 -4 2 18 3.40 1.60 4 2 -18 2.30 2.10 15 -3 -18 112.49 5.40 -15 -3 18 91.79 4.30 -15 3 18 97.89 4.00 -15 3 18 103.99 6.10 13 -3 -18 76.49 4.90 -13 -3 18 72.39 5.10 -13 -3 18 68.89 3.80 -13 3 18 68.49 3.40 -13 3 18 75.59 5.70 -11 -3 18 26.80 2.60 -11 -3 18 31.90 3.70 11 -3 -18 26.10 3.40 -11 3 18 28.10 2.30 11 3 -18 20.80 2.60 -11 3 18 32.20 4.10 -9 -3 18 3.00 2.70 -9 -3 18 5.70 1.90 9 -3 -18 -0.60 2.80 9 3 -18 2.80 1.80 -9 3 18 4.80 3.10 -7 -3 18 14.90 3.20 7 -3 -18 7.90 3.00 7 3 -18 12.40 2.30 -7 3 18 19.20 3.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 10537 _shelx_res_file ; TITL LM7_a.res in C2/c shelx.res created by SHELXL-2018/3 at 10:44:06 on 28-Nov-2024 CELL 0.71073 29.0324 9.1477 15.0296 90.000 108.533 90.000 ZERR 8.00 0.0008 0.0002 0.0004 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H F BR I N UNIT 120 160 32 8 16 8 MERG 2 OMIT 2 0 0 OMIT 1 1 0 EQIV $1 x-1/2, -y+1/2, z-1/2 HTAB N1 Br1_$1 EQIV $2 -x+1, y, -z+3/2 HTAB N1 Br1_$2 HTAB C13 Br1_$1 DFIX 0.850 0.020 H1A N1 DFIX 0.850 0.020 H1B N1 FMAP 2 PLAN 10 SIZE 0.190 0.210 0.250 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 WGHT 0.029700 23.404400 FVAR 0.07400 I1 5 0.587237 0.506663 0.954155 11.00000 0.01724 0.02663 = 0.02143 -0.00051 0.00575 -0.00053 I2 5 0.495978 0.208284 0.888780 11.00000 0.03171 0.02433 = 0.03802 0.00187 0.01060 -0.00134 BR1 4 0.702289 0.446444 1.062385 11.00000 0.01935 0.01805 = 0.02299 -0.00154 0.00620 0.00066 F1 3 0.396597 0.355932 0.787404 11.00000 0.02487 0.03783 = 0.04143 0.00239 0.00576 -0.01142 F2 3 0.368816 0.633649 0.748295 11.00000 0.01875 0.05242 = 0.04062 0.00718 0.00404 0.00860 F3 3 0.435152 0.851967 0.795334 11.00000 0.03978 0.02857 = 0.05075 0.00634 0.01213 0.01298 F4 3 0.528278 0.794339 0.881125 11.00000 0.03615 0.02347 = 0.04285 -0.00037 0.00906 -0.00820 N1 6 0.209024 0.422837 0.538712 11.00000 0.02004 0.01185 = 0.01993 0.00110 0.00835 -0.00126 C1 1 0.415593 0.604273 0.791498 11.00000 0.01983 0.04103 = 0.02176 0.00348 0.00767 0.00358 C2 1 0.430632 0.461617 0.812561 11.00000 0.01985 0.03524 = 0.02112 0.00003 0.00775 -0.00693 C3 1 0.478652 0.427240 0.858693 11.00000 0.02534 0.02348 = 0.01934 0.00116 0.00872 0.00042 C4 1 0.512955 0.539874 0.883904 11.00000 0.01741 0.02551 = 0.01995 -0.00178 0.00673 -0.00061 C5 1 0.496979 0.681297 0.860682 11.00000 0.02483 0.02861 = 0.02170 -0.00220 0.00871 -0.00120 C6 1 0.448958 0.713385 0.815472 11.00000 0.02939 0.03193 = 0.02611 0.00370 0.01147 0.00658 C7 1 0.125862 0.478960 0.536676 11.00000 0.02038 0.02636 = 0.03023 0.00097 0.00724 0.00168 AFIX 23 H7A 2 0.095235 0.529016 0.501617 11.00000 -1.20000 H7B 2 0.117866 0.376129 0.546160 11.00000 -1.20000 AFIX 0 C8 1 0.160114 0.481432 0.477433 11.00000 0.01856 0.01743 = 0.02503 0.00209 0.00693 0.00285 C9 1 0.232267 0.480905 0.638092 11.00000 0.02106 0.02003 = 0.01855 -0.00309 0.00565 -0.00336 C10 1 0.193999 0.474928 0.686872 11.00000 0.02565 0.02562 = 0.02430 -0.00270 0.01268 -0.00242 AFIX 23 H10A 2 0.207115 0.520952 0.749488 11.00000 -1.20000 H10B 2 0.186794 0.371383 0.696339 11.00000 -1.20000 AFIX 0 C11 1 0.146949 0.551836 0.632066 11.00000 0.02473 0.02940 = 0.02987 -0.00416 0.01276 0.00129 AFIX 23 H11A 2 0.123373 0.545906 0.667202 11.00000 -1.20000 H11B 2 0.153481 0.656302 0.623706 11.00000 -1.20000 AFIX 0 C12 1 0.252346 0.633917 0.635434 11.00000 0.02154 0.02419 = 0.03418 -0.00862 0.01119 -0.00554 AFIX 137 H12A 2 0.273188 0.661239 0.698410 11.00000 -1.50000 H12B 2 0.225401 0.703502 0.614153 11.00000 -1.50000 H12C 2 0.271380 0.635554 0.592027 11.00000 -1.50000 AFIX 0 C13 1 0.274483 0.379663 0.684142 11.00000 0.02079 0.02925 = 0.02318 -0.00217 0.00485 0.00066 AFIX 137 H13A 2 0.289234 0.407421 0.750087 11.00000 -1.50000 H13B 2 0.298770 0.387430 0.651613 11.00000 -1.50000 H13C 2 0.262726 0.278711 0.680484 11.00000 -1.50000 AFIX 0 C14 1 0.165473 0.632498 0.440266 11.00000 0.03128 0.01998 = 0.03444 0.00771 0.00875 0.00402 AFIX 137 H14A 2 0.191404 0.631076 0.411518 11.00000 -1.50000 H14B 2 0.173643 0.702913 0.492089 11.00000 -1.50000 H14C 2 0.134833 0.661096 0.393177 11.00000 -1.50000 AFIX 0 C15 1 0.142723 0.377281 0.395043 11.00000 0.02384 0.02346 = 0.02295 0.00223 0.00296 -0.00020 AFIX 137 H15A 2 0.165817 0.377765 0.359601 11.00000 -1.50000 H15B 2 0.110710 0.408459 0.354083 11.00000 -1.50000 H15C 2 0.140398 0.278296 0.418190 11.00000 -1.50000 AFIX 0 H1A 2 0.207412 0.329544 0.544099 11.00000 0.00968 H1B 2 0.230881 0.451386 0.516600 11.00000 0.04041 HKLF 4 REM LM7_a.res in C2/c REM wR2 = 0.0692, GooF = S = 1.100, Restrained GooF = 1.100 for all data REM R1 = 0.0262 for 3480 Fo > 4sig(Fo) and 0.0312 for all 3877 data REM 220 parameters refined using 2 restraints END WGHT 0.0297 23.4053 REM Highest difference peak 1.503, deepest hole -0.694, 1-sigma level 0.125 Q1 1 0.4937 0.8175 0.8671 11.00000 0.05 1.50 Q2 1 0.4899 0.1903 0.8233 11.00000 0.05 0.87 Q3 1 0.7069 0.5847 1.0679 11.00000 0.05 0.82 Q4 1 0.5779 0.4931 0.9017 11.00000 0.05 0.75 Q5 1 0.5991 0.4428 0.9539 11.00000 0.05 0.74 Q6 1 0.6073 0.4611 0.9770 11.00000 0.05 0.72 Q7 1 0.4718 0.1682 0.8368 11.00000 0.05 0.69 Q8 1 0.5104 0.1273 0.8899 11.00000 0.05 0.61 Q9 1 0.7338 0.4108 1.1065 11.00000 0.05 0.57 Q10 1 0.5330 0.2165 0.9208 11.00000 0.05 0.47 ; _shelx_res_checksum 72231 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 0.58724(2) 0.50666(3) 0.95416(2) 0.02186(8) Uani d 1 . . I I2 0.49598(2) 0.20828(3) 0.88878(2) 0.03147(9) Uani d 1 . . Br Br1 0.70229(2) 0.44644(4) 1.06238(3) 0.02025(10) Uani d 1 . . F F1 0.39660(9) 0.3559(3) 0.7874(2) 0.0358(6) Uani d 1 . . F F2 0.36882(9) 0.6336(3) 0.7483(2) 0.0385(7) Uani d 1 . . F F3 0.43515(10) 0.8520(3) 0.7953(2) 0.0402(7) Uani d 1 . . F F4 0.52828(10) 0.7943(3) 0.8811(2) 0.0350(6) Uani d 1 . . N N1 0.20902(12) 0.4228(4) 0.5387(2) 0.0168(7) Uani d 1 . . C C1 0.41559(15) 0.6043(5) 0.7915(3) 0.0273(10) Uani d 1 . . C C2 0.43063(15) 0.4616(5) 0.8126(3) 0.0251(9) Uani d 1 . . C C3 0.47865(15) 0.4272(5) 0.8587(3) 0.0223(8) Uani d 1 . . C C4 0.51296(14) 0.5399(5) 0.8839(3) 0.0208(8) Uani d 1 . . C C5 0.49698(15) 0.6813(5) 0.8607(3) 0.0247(9) Uani d 1 . . C C6 0.44896(16) 0.7134(5) 0.8155(3) 0.0285(10) Uani d 1 . . C C7 0.12586(15) 0.4790(5) 0.5367(3) 0.0258(9) Uani d 1 . . H H7A 0.095235 0.529016 0.501617 0.031 Uiso calc 1 . . H H7B 0.117866 0.376129 0.546160 0.031 Uiso calc 1 . . C C8 0.16011(14) 0.4814(4) 0.4774(3) 0.0203(8) Uani d 1 . . C C9 0.23227(14) 0.4809(4) 0.6381(3) 0.0200(8) Uani d 1 . . C C10 0.19400(15) 0.4749(5) 0.6869(3) 0.0241(9) Uani d 1 . . H H10A 0.207115 0.520952 0.749488 0.029 Uiso calc 1 . . H H10B 0.186794 0.371383 0.696339 0.029 Uiso calc 1 . . C C11 0.14695(15) 0.5518(5) 0.6321(3) 0.0270(9) Uani d 1 . . H H11A 0.123373 0.545906 0.667202 0.032 Uiso calc 1 . . H H11B 0.153481 0.656302 0.623706 0.032 Uiso calc 1 . . C C12 0.25235(15) 0.6339(5) 0.6354(3) 0.0261(9) Uani d 1 . . H H12A 0.273188 0.661239 0.698410 0.039 Uiso calc 1 . . H H12B 0.225401 0.703502 0.614153 0.039 Uiso calc 1 . . H H12C 0.271380 0.635554 0.592027 0.039 Uiso calc 1 . . C C13 0.27448(14) 0.3797(5) 0.6841(3) 0.0249(9) Uani d 1 . . H H13A 0.289234 0.407421 0.750087 0.037 Uiso calc 1 . . H H13B 0.298770 0.387430 0.651613 0.037 Uiso calc 1 . . H H13C 0.262726 0.278711 0.680484 0.037 Uiso calc 1 . . C C14 0.16547(16) 0.6325(5) 0.4403(3) 0.0290(10) Uani d 1 . . H H14A 0.191404 0.631076 0.411518 0.043 Uiso calc 1 . . H H14B 0.173643 0.702913 0.492089 0.043 Uiso calc 1 . . H H14C 0.134833 0.661096 0.393177 0.043 Uiso calc 1 . . C C15 0.14272(15) 0.3773(5) 0.3950(3) 0.0245(9) Uani d 1 . . H H15A 0.165817 0.377765 0.359601 0.037 Uiso calc 1 . . H H15B 0.110710 0.408459 0.354083 0.037 Uiso calc 1 . . H H15C 0.140398 0.278296 0.418190 0.037 Uiso calc 1 . . H H1A 0.2074(14) 0.330(2) 0.544(3) 0.010(10) Uiso d 1 . . H H1B 0.2309(15) 0.451(6) 0.517(4) 0.040(15) 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 I1 0.01724(13) 0.02663(16) 0.02143(14) -0.00053(10) 0.00575(10) -0.00051(11) I2 0.03171(16) 0.02433(16) 0.03802(18) -0.00134(12) 0.01060(13) 0.00187(12) Br1 0.01935(19) 0.0180(2) 0.0230(2) 0.00066(15) 0.00620(16) -0.00154(16) F1 0.0249(13) 0.0378(16) 0.0414(16) -0.0114(12) 0.0058(12) 0.0024(13) F2 0.0188(12) 0.0524(18) 0.0406(16) 0.0086(12) 0.0040(11) 0.0072(14) F3 0.0398(15) 0.0286(15) 0.0507(18) 0.0130(12) 0.0121(14) 0.0063(14) F4 0.0361(14) 0.0235(14) 0.0428(16) -0.0082(11) 0.0091(12) -0.0004(12) N1 0.0200(17) 0.0119(17) 0.0199(17) -0.0013(13) 0.0083(14) 0.0011(13) C1 0.020(2) 0.041(3) 0.022(2) 0.0036(18) 0.0077(17) 0.0035(19) C2 0.020(2) 0.035(2) 0.021(2) -0.0069(18) 0.0077(17) 0.0000(18) C3 0.025(2) 0.023(2) 0.019(2) 0.0004(17) 0.0087(17) 0.0012(17) C4 0.0174(19) 0.026(2) 0.020(2) -0.0006(16) 0.0067(16) -0.0018(17) C5 0.025(2) 0.029(2) 0.022(2) -0.0012(18) 0.0087(17) -0.0022(18) C6 0.029(2) 0.032(3) 0.026(2) 0.0066(19) 0.0115(19) 0.0037(19) C7 0.020(2) 0.026(2) 0.030(2) 0.0017(17) 0.0072(18) 0.0010(19) C8 0.0186(19) 0.017(2) 0.025(2) 0.0028(15) 0.0069(16) 0.0021(17) C9 0.0211(19) 0.020(2) 0.0185(19) -0.0034(16) 0.0057(16) -0.0031(16) C10 0.026(2) 0.026(2) 0.024(2) -0.0024(17) 0.0127(18) -0.0027(18) C11 0.025(2) 0.029(2) 0.030(2) 0.0013(18) 0.0128(18) -0.0042(19) C12 0.022(2) 0.024(2) 0.034(2) -0.0055(17) 0.0112(18) -0.0086(19) C13 0.021(2) 0.029(2) 0.023(2) 0.0007(17) 0.0048(17) -0.0022(18) C14 0.031(2) 0.020(2) 0.034(2) 0.0040(18) 0.0088(19) 0.0077(19) C15 0.024(2) 0.023(2) 0.023(2) -0.0002(17) 0.0030(17) 0.0022(17) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' 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 C8 N1 C9 . . 120.4(3) ? C8 N1 H1A . . 110(3) ? C9 N1 H1A . . 106(3) ? C8 N1 H1B . . 109(4) ? C9 N1 H1B . . 97(4) ? H1A N1 H1B . . 114(5) ? F2 C1 C6 . . 120.8(4) ? F2 C1 C2 . . 120.1(4) ? C6 C1 C2 . . 119.2(4) ? F1 C2 C1 . . 117.6(4) ? F1 C2 C3 . . 120.7(4) ? C1 C2 C3 . . 121.7(4) ? C2 C3 C4 . . 119.1(4) ? C2 C3 I2 . . 117.7(3) ? C4 C3 I2 . . 123.3(3) ? C5 C4 C3 . . 117.9(4) ? C5 C4 I1 . . 118.1(3) ? C3 C4 I1 . . 124.0(3) ? F4 C5 C6 . . 117.0(4) ? F4 C5 C4 . . 120.9(4) ? C6 C5 C4 . . 122.1(4) ? F3 C6 C1 . . 120.0(4) ? F3 C6 C5 . . 119.9(4) ? C1 C6 C5 . . 120.0(4) ? C11 C7 C8 . . 113.6(4) ? C11 C7 H7A . . 108.8 ? C8 C7 H7A . . 108.8 ? C11 C7 H7B . . 108.8 ? C8 C7 H7B . . 108.8 ? H7A C7 H7B . . 107.7 ? C15 C8 C14 . . 108.6(4) ? C15 C8 N1 . . 106.1(3) ? C14 C8 N1 . . 111.0(3) ? C15 C8 C7 . . 110.9(3) ? C14 C8 C7 . . 112.9(3) ? N1 C8 C7 . . 107.2(3) ? C10 C9 C13 . . 111.6(3) ? C10 C9 C12 . . 113.1(3) ? C13 C9 C12 . . 108.2(3) ? C10 C9 N1 . . 107.3(3) ? C13 C9 N1 . . 106.0(3) ? C12 C9 N1 . . 110.4(3) ? C9 C10 C11 . . 113.0(4) ? C9 C10 H10A . . 109.0 ? C11 C10 H10A . . 109.0 ? C9 C10 H10B . . 109.0 ? C11 C10 H10B . . 109.0 ? H10A C10 H10B . . 107.8 ? C7 C11 C10 . . 109.3(3) ? C7 C11 H11A . . 109.8 ? C10 C11 H11A . . 109.8 ? C7 C11 H11B . . 109.8 ? C10 C11 H11B . . 109.8 ? H11A C11 H11B . . 108.3 ? C9 C12 H12A . . 109.5 ? C9 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C9 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C9 C13 H13A . . 109.5 ? C9 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C9 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? C8 C14 H14A . . 109.5 ? C8 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C8 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? C8 C15 H15A . . 109.5 ? C8 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C8 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? 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 I1 C4 . 2.100(4) ? I2 C3 . 2.080(4) ? F1 C2 . 1.348(5) ? F2 C1 . 1.333(5) ? F3 C6 . 1.335(5) ? F4 C5 . 1.346(5) ? N1 C8 . 1.523(5) ? N1 C9 . 1.526(5) ? N1 H1A . 0.860(19) ? N1 H1B . 0.846(19) ? C1 C6 . 1.357(7) ? C1 C2 . 1.381(7) ? C2 C3 . 1.382(6) ? C3 C4 . 1.399(6) ? C4 C5 . 1.381(6) ? C5 C6 . 1.375(6) ? C7 C11 . 1.522(6) ? C7 C8 . 1.531(6) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C8 C15 . 1.516(6) ? C8 C14 . 1.517(6) ? C9 C10 . 1.514(5) ? C9 C13 . 1.516(6) ? C9 C12 . 1.522(6) ? C10 C11 . 1.525(6) ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 H11A . 0.9900 ? C11 H11B . 0.9900 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C13 H13C . 0.9800 ? C14 H14A . 0.9800 ? C14 H14B . 0.9800 ? C14 H14C . 0.9800 ? C15 H15A . 0.9800 ? C15 H15B . 0.9800 ? C15 H15C . 0.9800 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 F4 3.138(3) . . yes I1 I2 3.7118(4) . . yes I2 F1 3.111(3) . . yes H1A Br1 2.56 . 8_455 yes H13C Br1 2.91 . 8_455 yes H1B Br1 2.58(5) . 2_656 yes F1 F2 2.670(4) . . yes F2 F3 2.709(4) . . yes F3 F4 2.654(4) . . yes F2 H12A 2.65 . . yes H11A F3 2.63 . 4_546 yes C12 C14 3.203(6) . . yes C11 H12B 2.76 . . yes C11 H14B 2.83 . . yes C12 H11B 2.83 . . yes C12 H14B 2.67 . . yes C14 H12B 2.72 . . yes C14 H11B 2.90 . . yes H1A H13C 2.22 . . yes H1A H15C 2.30 . . yes H1B H12C 2.16 . . yes H1B H14A 2.32 . . yes H7B H15C 2.40 . . yes H11B H12B 2.19 . . yes H11B H14B 2.27 . . yes H12B H14B 1.97 . . yes 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 H1A Br1 8_455 0.860(19) 2.55(2) 3.409(3) 179(4) yes N1 H1B Br1 2_656 0.846(19) 2.58(3) 3.387(3) 161(5) yes C13 H13C Br1 8_455 0.98 2.91 3.769(4) 146.3 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 F2 C1 C2 F1 . . . . 0.4(6) ? C6 C1 C2 F1 . . . . -179.7(4) ? F2 C1 C2 C3 . . . . -178.9(4) ? C6 C1 C2 C3 . . . . 1.0(6) ? F1 C2 C3 C4 . . . . -179.9(4) ? C1 C2 C3 C4 . . . . -0.6(6) ? F1 C2 C3 I2 . . . . -0.7(5) ? C1 C2 C3 I2 . . . . 178.6(3) ? C2 C3 C4 C5 . . . . -0.4(6) ? I2 C3 C4 C5 . . . . -179.5(3) ? C2 C3 C4 I1 . . . . 180.0(3) ? I2 C3 C4 I1 . . . . 0.9(5) ? C3 C4 C5 F4 . . . . -178.6(4) ? I1 C4 C5 F4 . . . . 1.1(5) ? C3 C4 C5 C6 . . . . 1.0(6) ? I1 C4 C5 C6 . . . . -179.4(3) ? F2 C1 C6 F3 . . . . -0.4(6) ? C2 C1 C6 F3 . . . . 179.7(4) ? F2 C1 C6 C5 . . . . 179.5(4) ? C2 C1 C6 C5 . . . . -0.4(6) ? F4 C5 C6 F3 . . . . -1.2(6) ? C4 C5 C6 F3 . . . . 179.3(4) ? F4 C5 C6 C1 . . . . 179.0(4) ? C4 C5 C6 C1 . . . . -0.6(7) ? C9 N1 C8 C15 . . . . -166.9(3) ? C9 N1 C8 C14 . . . . 75.4(4) ? C9 N1 C8 C7 . . . . -48.4(4) ? C11 C7 C8 C15 . . . . 166.3(4) ? C11 C7 C8 C14 . . . . -71.7(5) ? C11 C7 C8 N1 . . . . 50.9(5) ? C8 N1 C9 C10 . . . . 49.8(4) ? C8 N1 C9 C13 . . . . 169.1(3) ? C8 N1 C9 C12 . . . . -73.8(4) ? C13 C9 C10 C11 . . . . -169.0(4) ? C12 C9 C10 C11 . . . . 68.7(5) ? N1 C9 C10 C11 . . . . -53.2(4) ? C8 C7 C11 C10 . . . . -58.9(5) ? C9 C10 C11 C7 . . . . 60.2(5) ?