#------------------------------------------------------------------------------ #$Date: 2021-10-14 05:45:34 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269943 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564915.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_1564915 loop_ _publ_author_name 'Hajjar, Christelle' 'Ovens, Jeffrey S.' 'Bryce, David L.' _publ_section_title ; 1,3,5-Trifluoro-2,4,6-triiodobenzene--piperazine (2/1) ; _journal_coeditor_code BV4042 _journal_issue 10 _journal_name_full IUCrData _journal_page_first x211044 _journal_paper_doi 10.1107/S2414314621010440 _journal_volume 6 _journal_year 2021 _chemical_formula_iupac 'C4 H10 N2, 2C6 F3 I3' _chemical_formula_moiety 'C4 H10 N2, 2(C6 F3 I3)' _chemical_formula_sum 'C16 H10 F6 I6 N2' _chemical_formula_weight 1105.66 _chemical_name_systematic ; 1,3,5-Trifluoro-2,4,6-triiodobenzene--piperazine (2/1) ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _cell_angle_alpha 67.4330(10) _cell_angle_beta 72.8870(10) _cell_angle_gamma 63.0620(10) _cell_formula_units_Z 1 _cell_length_a 8.6450(5) _cell_length_b 9.1660(5) _cell_length_c 9.3403(5) _cell_measurement_reflns_used 6804 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 30.67 _cell_measurement_theta_min 2.39 _cell_volume 602.75(6) _computing_cell_refinement ; SAINT (Bruker, 2010) ; _computing_data_collection ; APEX3 (Bruker, 2010) ; _computing_data_reduction ; SAINT (Bruker, 2010) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) and ShelXle (H\"ubschle et al., 2011) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\w and \phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13748 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.821 _diffrn_reflns_theta_min 2.387 _exptl_absorpt_coefficient_mu 7.784 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Krause et al., 2015\\bbr00)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.046 _exptl_crystal_description block _exptl_crystal_F_000 492 _exptl_crystal_size_max 0.236 _exptl_crystal_size_mid 0.131 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.560 _refine_diff_density_min -0.644 _refine_ls_abs_structure_details none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 3761 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+0.1043P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0475 _reflns_number_gt 3193 _reflns_number_total 3761 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bv4042sup1.cif _cod_data_source_block I _cod_database_code 1564915 _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_hkl_file ; -1 0 0 2.70 0.80 -1 0 0 3.10 0.90 -1 0 0 3.10 0.60 -1 0 0 1.80 0.60 1 0 0 4.60 0.70 1 0 0 1.90 0.60 1 0 0 2.50 0.70 1 0 0 2.20 0.70 -2 0 0 3004.40 54.59 -2 0 0 3066.29 54.79 -2 0 0 3168.18 53.09 2 0 0 3121.59 53.09 2 0 0 3009.10 54.59 -3 0 0 484.15 13.60 -3 0 0 490.85 13.50 3 0 0 469.05 13.40 3 0 0 464.45 11.60 3 0 0 489.55 13.60 -4 0 0 354.26 12.70 -4 0 0 352.46 12.30 4 0 0 354.46 12.40 4 0 0 359.26 10.70 4 0 0 381.56 12.80 -5 0 0 15.10 3.50 5 0 0 20.30 3.80 5 0 0 14.00 3.30 5 0 0 20.30 2.70 -6 0 0 118.29 8.60 6 0 0 101.29 8.00 6 0 0 88.69 7.60 6 0 0 110.69 6.40 -7 0 0 12.60 4.50 7 0 0 8.60 2.50 7 0 0 6.40 3.20 7 0 0 3.20 2.50 -8 0 0 50.09 8.70 8 0 0 36.50 7.30 8 0 0 55.39 5.60 8 0 0 47.40 8.10 -9 0 0 3.40 4.10 9 0 0 5.70 3.70 9 0 0 1.70 3.70 -10 0 0 8.30 4.90 10 0 0 4.20 4.40 10 0 0 1.20 3.00 10 -1 0 1.20 3.80 10 -1 0 6.80 5.40 -10 1 0 12.20 6.30 9 -1 0 141.29 12.60 9 -1 0 154.98 12.90 -9 1 0 167.28 14.00 8 -1 0 50.39 7.60 8 -1 0 84.09 9.00 -8 1 0 62.59 8.60 7 -1 0 458.65 14.70 7 -1 0 454.75 19.60 7 -1 0 479.75 19.70 -7 1 0 434.96 19.50 6 -1 0 797.72 24.50 6 -1 0 746.33 24.50 6 -1 0 729.93 19.00 -6 1 0 767.82 24.90 5 -1 0 836.52 24.40 5 -1 0 806.62 23.30 5 -1 0 832.52 19.50 -5 1 0 811.22 24.10 4 -1 0 1851.11 32.50 4 -1 0 1891.11 39.70 4 -1 0 1834.42 40.20 4 -1 0 1822.52 35.40 -4 1 0 1855.81 32.20 -4 1 0 1859.21 40.40 3 -1 0 596.64 16.30 3 -1 0 575.84 11.80 3 -1 0 569.44 12.90 3 -1 0 561.44 15.30 -3 1 0 576.34 11.60 -3 1 0 554.24 15.80 2 -1 0 220.08 5.70 2 -1 0 212.08 7.70 2 -1 0 232.48 7.40 2 -1 0 221.78 5.70 2 -1 0 221.98 5.80 -2 1 0 222.08 5.60 -2 1 0 213.88 7.70 1 -1 0 115.49 4.40 1 -1 0 119.09 3.70 1 -1 0 120.39 3.10 1 -1 0 120.49 4.40 1 -1 0 109.69 3.80 -1 1 0 120.99 3.20 -1 1 0 117.29 3.70 -1 1 0 114.99 3.90 -1 1 0 120.59 4.50 0 -1 0 233.48 5.00 0 -1 0 235.28 5.10 0 -1 0 235.48 5.80 0 -1 0 229.38 5.70 0 1 0 226.38 5.00 0 1 0 228.68 5.80 0 1 0 235.78 5.10 -1 -1 0 27.10 1.50 -1 -1 0 22.20 1.40 -1 -1 0 25.00 1.20 -1 -1 0 24.80 1.60 1 1 0 22.60 1.50 1 1 0 20.70 1.10 1 1 0 22.10 1.40 -2 -1 0 1717.93 31.80 -2 -1 0 1728.13 33.70 -2 -1 0 1751.02 30.40 2 1 0 1766.02 33.40 2 1 0 1756.22 32.60 2 1 0 1811.12 32.50 2 1 0 1720.73 30.30 -3 -1 0 93.29 5.40 -3 -1 0 108.19 5.10 -3 -1 0 110.59 3.10 3 1 0 104.09 5.30 3 1 0 109.39 2.90 3 1 0 97.19 4.70 -4 -1 0 82.09 5.70 -4 -1 0 71.19 4.90 4 1 0 69.49 4.90 4 1 0 82.69 5.40 4 1 0 65.99 4.30 -5 -1 0 59.59 5.60 -5 -1 0 55.29 4.90 5 1 0 58.79 4.50 5 1 0 57.39 5.20 5 1 0 55.99 5.10 -6 -1 0 469.05 17.70 6 1 0 450.05 14.60 6 1 0 447.36 17.00 6 1 0 428.06 16.20 -7 -1 0 147.19 10.70 7 1 0 168.28 11.00 7 1 0 170.68 8.90 7 1 0 152.58 10.20 -8 -1 0 317.57 17.30 8 1 0 334.17 13.70 8 1 0 337.87 16.50 8 1 0 285.77 15.90 -9 -1 0 234.58 16.20 9 1 0 169.28 13.10 9 1 0 207.88 11.40 9 1 0 186.18 13.40 -10 -1 0 72.89 10.70 10 1 0 73.29 9.30 10 1 0 78.39 10.30 -11 -1 0 131.89 15.00 11 1 0 117.79 12.60 11 1 0 96.89 12.30 10 -2 0 2.90 4.50 10 -2 0 0.00 4.50 -10 2 0 -1.10 4.90 9 -2 0 71.59 9.90 9 -2 0 60.79 9.00 -9 2 0 71.39 12.00 8 -2 0 -0.90 2.30 8 -2 0 3.20 3.60 -8 2 0 2.20 3.70 7 -2 0 8.50 4.00 7 -2 0 6.00 3.50 -7 2 0 -0.20 2.80 6 -2 0 90.39 5.30 6 -2 0 76.59 7.30 6 -2 0 91.39 8.40 -6 2 0 90.19 8.30 5 -2 0 2.40 1.30 5 -2 0 -1.70 1.20 5 -2 0 4.80 2.60 -5 2 0 5.20 2.60 -5 2 0 2.30 1.00 4 -2 0 766.72 21.10 4 -2 0 765.82 22.20 4 -2 0 739.73 16.90 -4 2 0 769.02 16.40 -4 2 0 758.22 22.20 3 -2 0 37.20 3.50 3 -2 0 33.10 3.80 3 -2 0 37.90 2.60 -3 2 0 39.50 2.80 -3 2 0 36.00 4.00 2 -2 0 135.59 4.30 2 -2 0 143.99 6.70 2 -2 0 128.89 4.40 2 -2 0 125.19 5.50 -2 2 0 146.89 6.80 -2 2 0 130.19 5.20 -2 2 0 133.49 4.40 1 -2 0 423.76 9.90 1 -2 0 431.56 9.30 1 -2 0 432.86 11.10 -1 2 0 436.46 10.90 -1 2 0 426.06 9.30 -1 2 0 441.86 11.90 0 -2 0 1065.99 20.10 0 -2 0 1059.99 20.10 0 2 0 1054.59 20.10 0 2 0 1072.09 21.60 0 2 0 1090.29 20.10 0 2 0 1060.09 21.90 -1 -2 0 27.60 2.70 -1 -2 0 22.80 1.40 -1 -2 0 23.50 1.40 1 2 0 21.50 2.00 1 2 0 28.40 1.60 1 2 0 24.90 1.30 1 2 0 27.20 2.30 -2 -2 0 8308.97 166.38 -2 -2 0 9432.66 158.38 -2 -2 0 9288.97 158.38 2 2 0 9313.77 160.08 2 2 0 9656.13 161.08 2 2 0 9775.22 161.28 2 2 0 9999.00 159.58 -3 -2 0 24.40 2.30 -3 -2 0 31.10 3.60 -3 -2 0 26.00 2.20 3 2 0 26.70 2.80 3 2 0 27.50 2.20 3 2 0 23.90 2.70 -4 -2 0 2990.20 59.09 -4 -2 0 2933.81 51.79 -4 -2 0 2935.81 54.89 4 2 0 2901.01 55.59 4 2 0 2935.01 56.59 4 2 0 2989.60 51.49 -5 -2 0 375.26 13.00 -5 -2 0 395.86 15.30 -5 -2 0 390.86 9.40 5 2 0 390.66 13.30 5 2 0 383.16 13.00 5 2 0 397.56 8.90 5 2 0 408.66 14.40 -6 -2 0 978.70 25.90 -6 -2 0 1001.00 29.10 6 2 0 977.10 25.30 6 2 0 967.80 26.00 6 2 0 1007.30 27.70 -7 -2 0 41.60 6.30 7 2 0 43.60 5.40 7 2 0 23.10 5.10 7 2 0 32.20 5.30 -8 -2 0 7.90 4.20 8 2 0 7.60 3.20 8 2 0 10.20 3.90 8 2 0 6.10 3.30 -9 -2 0 -2.20 2.70 9 2 0 2.40 2.70 9 2 0 3.30 3.80 9 2 0 -2.20 2.40 -10 -2 0 -3.00 3.90 10 2 0 1.60 4.60 10 2 0 2.20 3.40 10 2 0 3.80 3.50 -11 -2 0 4.40 5.70 11 2 0 3.80 4.00 11 2 0 1.90 4.60 9 -3 0 -2.30 3.90 9 -3 0 -0.40 4.00 -9 3 0 4.10 4.10 8 -3 0 59.59 9.20 8 -3 0 61.39 9.90 -8 3 0 61.69 9.10 7 -3 0 62.79 8.00 7 -3 0 67.39 8.70 -7 3 0 63.29 8.50 6 -3 0 -0.90 2.10 6 -3 0 -0.60 1.80 -6 3 0 2.80 2.60 5 -3 0 457.15 18.60 5 -3 0 484.75 12.80 5 -3 0 467.15 17.20 -5 3 0 474.35 12.80 -5 3 0 492.95 19.30 4 -3 0 582.74 14.10 4 -3 0 588.84 18.00 4 -3 0 579.34 19.60 -4 3 0 582.64 19.80 -4 3 0 582.34 15.20 3 -3 0 1456.35 31.70 3 -3 0 1468.95 33.90 3 -3 0 1470.65 28.30 -3 3 0 1422.86 30.10 -3 3 0 1470.25 34.30 2 -3 0 2840.42 52.69 2 -3 0 2849.31 55.09 -2 3 0 2877.71 53.39 -2 3 0 2819.72 56.09 -2 3 0 2906.11 50.39 1 -3 0 552.04 14.10 1 -3 0 548.15 12.40 -1 3 0 541.25 12.20 -1 3 0 532.85 14.40 -1 3 0 535.05 15.30 0 -3 0 1875.11 34.90 0 -3 0 1864.31 37.90 0 3 0 1849.02 37.10 0 3 0 1945.21 38.00 0 3 0 1902.11 35.00 -1 -3 0 253.57 5.90 -1 -3 0 247.98 9.20 -1 -3 0 256.17 6.30 1 3 0 265.97 8.10 1 3 0 252.97 8.70 1 3 0 251.37 6.20 1 3 0 253.17 6.00 -2 -3 0 78.49 5.50 -2 -3 0 78.99 2.80 -2 -3 0 76.59 3.50 2 3 0 67.39 4.30 2 3 0 70.49 4.30 2 3 0 68.49 3.50 2 3 0 76.99 3.20 -3 -3 0 292.87 7.70 -3 -3 0 291.17 12.30 3 3 0 293.97 9.40 3 3 0 279.37 7.90 3 3 0 307.07 9.40 3 3 0 286.77 10.10 -4 -3 0 587.84 14.50 -4 -3 0 581.24 19.40 4 3 0 561.64 16.50 4 3 0 585.84 16.30 4 3 0 590.14 14.50 -5 -3 0 185.28 8.10 -5 -3 0 205.58 11.40 5 3 0 196.88 9.50 5 3 0 199.98 7.00 5 3 0 193.98 9.30 -6 -3 0 160.28 8.40 -6 -3 0 143.39 10.40 6 3 0 147.79 5.60 6 3 0 140.49 8.90 6 3 0 154.08 8.30 6 3 0 150.48 8.60 -7 -3 0 46.10 6.80 7 3 0 44.70 5.70 7 3 0 44.30 5.10 7 3 0 50.79 5.60 7 3 0 39.80 3.60 -8 -3 0 34.60 7.50 8 3 0 30.90 5.80 8 3 0 31.70 6.30 8 3 0 33.80 5.20 -9 -3 0 2.30 3.90 9 3 0 -0.50 2.20 9 3 0 -2.60 2.00 9 3 0 -0.40 2.40 -10 -3 0 110.09 12.70 10 3 0 105.39 11.20 10 3 0 99.59 10.00 10 3 0 108.79 9.70 -11 -3 0 44.20 10.70 11 3 0 47.50 9.40 11 3 0 33.10 7.80 8 -4 0 2.80 3.90 8 -4 0 2.20 4.00 -8 4 0 12.40 5.80 7 -4 0 188.18 12.80 7 -4 0 187.68 14.40 -7 4 0 175.48 13.80 6 -4 0 19.00 5.60 6 -4 0 16.80 4.90 -6 4 0 14.80 4.70 5 -4 0 75.39 6.90 5 -4 0 85.99 8.30 -5 4 0 73.29 5.30 -5 4 0 76.39 7.90 4 -4 0 33.30 3.00 4 -4 0 26.40 4.00 4 -4 0 33.60 5.80 -4 4 0 34.20 3.80 -4 4 0 30.50 5.70 3 -4 0 113.49 6.50 3 -4 0 107.69 7.50 3 -4 0 110.89 5.10 -3 4 0 108.49 6.40 -3 4 0 118.29 8.10 2 -4 0 761.32 20.90 2 -4 0 768.22 18.60 -2 4 0 800.42 17.30 -2 4 0 781.02 22.50 -2 4 0 814.72 20.80 1 -4 0 46.40 2.90 1 -4 0 42.70 3.70 -1 4 0 47.40 3.10 -1 4 0 43.60 4.50 -1 4 0 49.80 4.40 0 -4 0 1216.88 28.60 0 -4 0 1204.28 24.80 0 -4 0 1186.58 22.00 0 -4 0 1177.48 21.90 0 4 0 1204.78 24.90 0 4 0 1203.08 28.30 0 4 0 1196.28 27.60 -1 -4 0 478.85 9.80 -1 -4 0 487.65 11.30 -1 -4 0 489.25 15.40 1 4 0 487.15 14.60 1 4 0 474.75 10.90 1 4 0 475.35 13.20 -2 -4 0 14.40 1.40 -2 -4 0 11.10 2.90 -2 -4 0 14.20 1.60 2 4 0 13.10 2.70 2 4 0 14.30 1.70 2 4 0 15.20 2.70 2 4 0 15.70 1.40 -3 -4 0 97.99 7.50 3 4 0 92.29 4.30 3 4 0 99.29 5.80 3 4 0 99.39 6.10 3 4 0 106.19 5.20 -4 -4 0 1413.76 27.30 -4 -4 0 1395.96 36.20 4 4 0 1411.86 30.30 4 4 0 1340.17 31.80 4 4 0 1367.86 30.20 -5 -4 0 14.40 4.50 -5 -4 0 16.70 2.50 5 4 0 12.00 2.50 5 4 0 11.30 3.00 5 4 0 10.80 3.00 -6 -4 0 1026.10 32.40 -6 -4 0 1065.19 25.80 6 4 0 1118.89 26.20 6 4 0 1034.20 28.60 6 4 0 1093.09 24.40 6 4 0 1109.89 29.10 -7 -4 0 86.29 9.30 -7 -4 0 93.69 6.80 7 4 0 94.39 5.20 7 4 0 99.49 6.90 7 4 0 110.19 8.60 7 4 0 91.69 7.80 -8 -4 0 693.23 28.10 8 4 0 642.14 24.30 8 4 0 727.53 22.80 8 4 0 686.63 23.50 -9 -4 0 40.70 8.80 9 4 0 40.50 5.90 9 4 0 29.00 6.60 9 4 0 36.70 6.70 -10 -4 0 59.99 11.60 10 4 0 56.99 7.70 10 4 0 46.30 7.80 10 4 0 68.49 9.40 -11 -4 0 15.50 7.20 11 4 0 16.40 6.40 11 4 0 11.90 4.80 11 4 0 12.30 5.30 8 -5 0 81.89 11.60 -8 5 0 60.09 11.10 7 -5 0 17.40 7.90 7 -5 0 17.20 6.40 -7 5 0 8.60 4.80 6 -5 0 248.48 15.90 6 -5 0 262.37 14.20 -6 5 0 245.48 16.20 5 -5 0 6.30 3.10 5 -5 0 11.40 4.30 -5 5 0 8.80 4.00 4 -5 0 225.08 10.70 4 -5 0 188.08 11.90 -4 5 0 206.18 12.70 -4 5 0 212.68 10.20 3 -5 0 301.17 13.90 3 -5 0 335.57 10.20 3 -5 0 341.17 12.00 -3 5 0 331.67 13.10 -3 5 0 332.47 15.50 -3 5 0 317.97 9.90 2 -5 0 83.49 6.30 2 -5 0 76.59 4.80 -2 5 0 85.19 7.40 -2 5 0 79.99 6.10 -2 5 0 71.99 4.30 1 -5 0 753.72 16.70 1 -5 0 800.02 20.40 -1 5 0 753.72 21.60 -1 5 0 732.03 22.80 -1 5 0 750.82 18.00 0 -5 0 1234.48 31.70 0 -5 0 1264.17 23.20 0 -5 0 1259.87 23.30 0 -5 0 1292.57 27.20 0 5 0 1265.27 30.70 0 5 0 1232.68 27.10 -1 -5 0 268.07 12.10 -1 -5 0 265.87 6.30 -1 -5 0 289.97 8.50 1 5 0 260.57 11.30 1 5 0 278.57 10.10 -2 -5 0 2198.28 47.80 -2 -5 0 2105.09 38.30 -2 -5 0 2127.79 38.80 2 5 0 2101.39 38.90 2 5 0 2178.18 38.20 2 5 0 2187.28 44.10 2 5 0 2200.08 45.70 -3 -5 0 111.39 3.70 -3 -5 0 109.89 8.40 3 5 0 106.99 6.80 3 5 0 107.59 5.30 3 5 0 109.99 7.00 3 5 0 112.89 3.90 -4 -5 0 397.86 17.40 -4 -5 0 408.86 9.90 4 5 0 396.76 11.30 4 5 0 425.86 15.00 4 5 0 407.06 13.00 4 5 0 407.26 14.20 -5 -5 0 72.69 4.20 -5 -5 0 61.99 7.50 5 5 0 61.49 6.10 5 5 0 71.99 5.60 5 5 0 78.99 5.90 -6 -5 0 46.40 6.90 -6 -5 0 44.80 4.10 6 5 0 47.30 5.20 6 5 0 41.80 3.90 6 5 0 47.60 4.60 6 5 0 48.20 5.80 -7 -5 0 133.49 11.70 7 5 0 118.39 6.90 7 5 0 116.99 8.80 7 5 0 118.79 9.10 7 5 0 122.79 7.30 -8 -5 0 27.20 7.50 8 5 0 27.10 5.10 8 5 0 19.80 5.20 8 5 0 26.40 5.70 -9 -5 0 83.09 11.10 9 5 0 72.49 7.20 9 5 0 75.09 8.70 9 5 0 85.29 9.10 -10 -5 0 -1.50 4.00 10 5 0 -0.10 3.40 10 5 0 -0.60 3.10 10 5 0 -2.40 2.40 -11 -5 0 21.20 8.10 11 5 0 26.70 6.30 11 5 0 30.40 8.20 11 5 0 25.60 7.00 7 -6 0 68.29 10.20 -7 6 0 58.49 10.90 6 -6 0 2.30 3.80 -6 6 0 -0.80 3.00 5 -6 0 207.98 14.10 -5 6 0 174.58 13.80 4 -6 0 81.39 8.40 -4 6 0 90.29 7.30 -4 6 0 86.49 9.20 3 -6 0 182.48 8.70 3 -6 0 194.88 11.50 -3 6 0 173.48 10.30 -3 6 0 184.08 12.40 2 -6 0 18.70 2.70 2 -6 0 15.20 3.80 -2 6 0 11.00 3.70 -2 6 0 27.90 5.00 -2 6 0 16.90 2.90 1 -6 0 120.09 5.10 1 -6 0 122.79 7.40 1 -6 0 129.49 9.60 -1 6 0 126.19 9.30 -1 6 0 104.59 7.90 -1 6 0 122.79 6.40 0 -6 0 259.07 13.20 0 -6 0 261.17 9.80 0 -6 0 242.98 6.20 0 -6 0 252.67 6.40 0 6 0 225.98 9.40 0 6 0 219.88 11.50 -1 -6 0 86.09 4.80 -1 -6 0 87.69 7.50 1 6 0 79.99 6.80 1 6 0 84.99 5.80 -2 -6 0 782.22 17.20 -2 -6 0 823.72 25.50 2 6 0 764.42 23.30 2 6 0 767.32 21.60 -3 -6 0 327.67 15.60 3 6 0 341.07 10.30 3 6 0 338.07 13.50 3 6 0 336.47 14.10 -4 -6 0 357.16 17.20 4 6 0 357.06 14.50 4 6 0 370.76 12.20 4 6 0 351.36 14.40 -5 -6 0 239.28 7.30 -5 -6 0 250.07 14.90 5 6 0 239.68 11.40 5 6 0 225.08 10.30 5 6 0 251.17 12.40 -6 -6 0 6.60 2.10 -6 -6 0 6.50 4.00 6 6 0 5.70 3.00 6 6 0 7.00 2.90 6 6 0 1.60 2.30 6 6 0 3.40 1.70 -7 -6 0 88.99 10.30 7 6 0 81.79 6.60 7 6 0 92.19 8.00 7 6 0 90.39 8.50 7 6 0 84.09 5.70 -8 -6 0 260.27 17.50 8 6 0 248.68 14.10 8 6 0 235.68 11.00 8 6 0 221.48 13.70 8 6 0 241.98 11.00 -9 -6 0 3.40 4.70 9 6 0 5.40 3.20 9 6 0 4.50 3.50 9 6 0 5.10 4.10 -10 -6 0 184.68 16.90 10 6 0 184.58 14.30 10 6 0 182.88 13.60 -11 -6 0 8.50 7.10 11 6 0 6.20 4.90 11 6 0 14.80 6.00 6 -7 0 78.69 10.80 -6 7 0 52.29 10.20 5 -7 0 7.40 4.80 -5 7 0 10.30 4.80 4 -7 0 247.58 15.00 -4 7 0 237.48 16.30 -4 7 0 252.77 13.40 3 -7 0 0.40 2.30 -3 7 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21.70 7.60 7 11 -1 19.70 7.10 7 11 -1 36.50 8.80 -7 -11 1 20.20 8.00 6 11 -1 35.50 8.30 6 11 -1 41.50 9.50 -6 -11 1 56.49 11.70 5 11 -1 2.90 4.90 5 11 -1 -4.00 3.70 -5 -11 1 -3.20 4.70 4 11 -1 -0.70 4.00 4 11 -1 0.80 3.60 -4 -11 1 3.90 5.90 3 11 -1 51.09 9.40 3 11 -1 66.09 11.60 -3 -11 1 84.69 12.40 2 11 -1 8.20 5.40 -2 -11 1 10.10 6.70 1 11 -1 29.20 8.00 -1 -11 1 39.70 10.10 9 10 -1 2.50 5.00 -9 -10 1 6.40 7.40 8 10 -1 0.20 4.10 8 10 -1 2.50 4.40 -8 -10 1 2.40 5.70 7 10 -1 44.70 8.60 7 10 -1 44.80 8.90 -7 -10 1 45.90 10.80 6 10 -1 7.50 4.40 6 10 -1 0.40 3.70 -6 -10 1 2.10 5.20 5 10 -1 0.50 3.60 5 10 -1 -3.90 3.20 -5 -10 1 8.70 6.60 4 10 -1 -2.00 3.10 4 10 -1 1.10 3.70 -4 -10 1 7.90 5.80 3 10 -1 6.90 4.20 3 10 -1 6.30 4.70 -3 -10 1 25.40 8.00 2 10 -1 150.08 11.50 2 10 -1 153.98 13.30 -2 -10 1 151.68 14.60 1 10 -1 71.89 9.70 -1 -10 1 73.29 11.10 0 10 -1 199.48 15.50 0 -10 1 227.48 17.80 -1 10 -1 15.80 6.20 1 -10 1 22.30 7.40 2 -10 1 140.29 15.60 10 9 -1 2.50 5.00 -10 -9 1 3.70 6.50 9 9 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5.90 -4 -8 1 32.80 7.50 3 8 -1 24.70 6.20 3 8 -1 18.80 4.80 -3 -8 1 18.30 5.50 2 8 -1 16.80 4.10 2 8 -1 28.20 6.00 -2 -8 1 14.70 5.10 1 8 -1 21.80 4.40 1 8 -1 28.50 6.50 -1 -8 1 15.20 5.00 0 8 -1 116.59 10.30 0 8 -1 95.69 7.00 0 -8 1 91.59 7.40 0 -8 1 90.49 9.90 -1 8 -1 65.89 8.10 1 -8 1 67.99 8.70 1 -8 1 68.59 7.00 -2 8 -1 237.28 14.60 2 -8 1 197.58 15.40 2 -8 1 235.28 13.40 -3 8 -1 47.00 9.20 -3 8 -1 62.59 8.10 3 -8 1 66.09 10.10 3 -8 1 56.99 7.90 -4 8 -1 232.98 17.50 4 -8 1 277.57 16.80 4 -8 1 255.07 19.00 5 -8 1 0.20 4.10 5 -8 1 -2.50 5.00 11 7 -1 14.40 6.40 11 7 -1 28.20 7.60 -11 -7 1 10.30 7.20 10 7 -1 -1.60 3.80 10 7 -1 7.80 5.00 -10 -7 1 6.70 6.00 9 7 -1 21.10 6.00 9 7 -1 38.80 8.00 -9 -7 1 26.00 8.20 8 7 -1 43.10 8.10 8 7 -1 37.50 6.30 8 7 -1 32.00 6.40 -8 -7 1 41.40 9.30 7 7 -1 8.10 4.00 7 7 -1 5.60 3.20 7 7 -1 1.60 2.60 -7 -7 1 5.00 4.40 6 7 -1 0.60 2.40 6 7 -1 4.30 3.00 6 7 -1 7.30 3.10 -6 -7 1 1.60 3.50 5 7 -1 360.06 16.30 5 7 -1 358.46 16.60 5 7 -1 360.96 13.20 -5 -7 1 368.06 19.60 4 7 -1 119.09 6.20 4 7 -1 110.39 9.00 4 7 -1 105.79 8.70 -4 -7 1 101.79 10.00 3 7 -1 900.91 26.80 3 7 -1 901.21 28.20 -3 -7 1 901.41 20.30 -3 -7 1 939.91 30.90 2 7 -1 515.05 18.30 2 7 -1 530.55 20.60 -2 -7 1 508.45 21.50 -2 -7 1 548.95 15.40 1 7 -1 792.22 26.10 1 7 -1 764.42 22.20 -1 -7 1 791.72 27.20 -1 -7 1 752.92 20.60 0 7 -1 266.57 11.10 0 7 -1 253.67 14.00 0 -7 1 261.57 15.00 0 -7 1 265.07 11.40 -1 7 -1 54.39 4.70 -1 7 -1 55.09 6.80 1 -7 1 79.29 6.80 1 -7 1 58.79 7.70 -2 7 -1 90.79 9.40 -2 7 -1 110.59 9.40 2 -7 1 83.89 9.40 2 -7 1 74.29 7.40 -3 7 -1 3.30 3.20 -3 7 -1 2.90 3.20 3 -7 1 3.20 2.80 -4 7 -1 10.90 5.30 -4 7 -1 12.70 4.20 4 -7 1 11.00 4.70 -5 7 -1 24.70 7.20 5 -7 1 34.40 7.70 -6 7 -1 8.40 4.80 6 -7 1 9.70 5.60 11 6 -1 10.00 5.80 11 6 -1 29.20 8.10 -11 -6 1 33.30 9.70 10 6 -1 23.40 7.00 10 6 -1 36.90 8.10 -10 -6 1 30.40 8.90 9 6 -1 267.67 15.90 9 6 -1 236.98 15.70 -9 -6 1 257.27 19.00 8 6 -1 4.60 2.90 8 6 -1 6.60 4.20 8 6 -1 2.30 2.40 8 6 -1 6.00 3.60 -8 -6 1 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-12 59.09 10.50 0 -5 -12 68.79 11.70 0 5 12 64.29 12.70 -1 -5 -12 182.28 14.20 -1 -5 -12 182.08 15.90 1 5 12 158.08 16.40 -2 -5 -12 150.58 14.50 -2 -5 -12 140.29 12.70 2 5 12 139.69 15.30 -3 -5 -12 52.69 8.90 -3 -5 -12 66.09 11.10 3 5 12 50.89 10.60 -4 -5 -12 30.30 8.30 -4 -5 -12 15.10 5.30 4 5 12 21.00 7.80 -5 -5 -12 43.00 8.90 -5 -5 -12 54.39 8.70 5 5 12 42.40 9.70 -6 -5 -12 -0.50 3.60 6 5 12 8.60 5.80 -7 -5 -12 76.59 11.30 7 5 12 57.49 11.80 -8 -5 -12 33.20 8.70 8 5 12 53.99 11.40 8 5 12 36.50 8.50 0 -6 -12 0.50 5.00 0 -6 -12 -0.40 3.40 0 6 12 -4.70 4.90 -1 -6 -12 37.90 8.40 -1 -6 -12 52.19 10.60 1 6 12 61.89 12.10 -2 -6 -12 -2.90 2.80 -2 -6 -12 3.70 5.20 2 6 12 2.80 5.20 -3 -6 -12 57.59 9.70 -3 -6 -12 57.69 10.90 3 6 12 41.10 9.30 -4 -6 -12 -0.20 2.90 -4 -6 -12 0.40 4.10 4 6 12 -2.10 4.30 -5 -6 -12 10.70 5.50 -5 -6 -12 8.00 4.40 5 6 12 7.80 5.30 -6 -6 -12 13.80 5.00 -6 -6 -12 13.90 6.00 6 6 12 37.90 9.20 -7 -6 -12 13.20 6.20 7 6 12 17.00 7.40 -8 -6 -12 128.89 13.60 8 6 12 140.59 15.30 0 -7 -12 11.60 6.40 0 -7 -12 15.30 7.00 0 7 12 13.10 7.80 -1 -7 -12 83.49 10.40 -1 -7 -12 71.69 12.20 1 7 12 54.49 12.20 -2 -7 -12 105.39 11.20 -2 -7 -12 75.59 12.80 2 7 12 87.09 13.00 -3 -7 -12 206.58 14.80 -3 -7 -12 199.98 16.90 3 7 12 221.18 18.00 -4 -7 -12 200.38 14.60 -4 -7 -12 214.28 17.10 4 7 12 185.08 16.70 -5 -7 -12 71.79 9.00 -5 -7 -12 71.99 10.80 5 7 12 67.89 8.80 5 7 12 89.59 12.30 -6 -7 -12 88.49 11.70 -6 -7 -12 84.09 9.60 6 7 12 99.49 10.00 6 7 12 86.19 12.30 -7 -7 -12 -0.10 3.20 -7 -7 -12 2.10 4.50 7 7 12 -1.10 4.70 7 7 12 0.10 3.50 -8 -7 -12 14.70 6.40 8 7 12 35.00 9.60 -1 -8 -12 50.39 10.10 -1 -8 -12 60.69 11.80 1 8 12 43.80 10.80 -2 -8 -12 0.60 3.60 -2 -8 -12 6.40 5.70 2 8 12 -1.20 5.70 -3 -8 -12 -0.10 4.70 -3 -8 -12 0.40 3.20 3 8 12 5.20 5.80 -4 -8 -12 13.10 5.80 -4 -8 -12 14.90 6.50 4 8 12 15.50 6.30 4 8 12 1.40 4.50 -5 -8 -12 40.40 9.80 -5 -8 -12 24.10 6.50 5 8 12 51.69 10.50 5 8 12 32.80 7.30 -6 -8 -12 29.30 8.40 6 8 12 28.50 7.00 -7 -8 -12 20.10 7.40 7 8 12 6.40 5.00 -8 -8 -12 6.70 5.80 8 8 12 -3.80 3.50 -3 -9 -12 -0.50 4.10 -3 -9 -12 10.10 6.20 3 9 12 4.80 4.60 -4 -9 -12 12.60 7.30 -4 -9 -12 22.30 6.70 4 9 12 20.10 6.70 -5 -9 -12 99.59 12.50 5 9 12 78.29 10.50 -6 -9 -12 101.29 12.60 6 9 12 81.19 10.00 -7 -9 -12 54.19 11.00 7 9 12 46.00 8.70 -2 -2 -13 20.90 8.00 -3 -2 -13 130.79 14.70 -1 -3 -13 88.49 13.40 -1 -3 -13 91.89 11.00 1 3 13 86.39 13.10 -2 -3 -13 20.50 6.60 -2 -3 -13 8.70 6.00 2 3 13 32.50 10.00 -3 -3 -13 19.50 6.00 -3 -3 -13 15.10 7.30 3 3 13 18.00 8.00 -4 -3 -13 9.90 6.20 4 3 13 2.30 5.70 -1 -4 -13 104.09 13.80 -1 -4 -13 54.09 9.60 1 4 13 91.29 13.80 -2 -4 -13 9.10 4.80 -2 -4 -13 -4.00 5.20 2 4 13 5.90 6.80 -3 -4 -13 46.70 8.60 -3 -4 -13 54.89 10.70 3 4 13 44.70 10.40 -4 -4 -13 -0.10 5.30 -4 -4 -13 2.90 4.10 4 4 13 -4.10 4.80 -5 -4 -13 11.90 6.30 5 4 13 20.50 7.90 -1 -5 -13 163.48 16.70 1 5 13 144.79 16.90 -2 -5 -13 76.69 9.90 -2 -5 -13 62.69 11.70 2 5 13 33.00 9.60 -3 -5 -13 152.98 13.30 -3 -5 -13 151.18 15.30 3 5 13 145.69 16.30 -4 -5 -13 21.10 7.10 -4 -5 -13 16.60 6.20 4 5 13 9.00 6.00 -5 -5 -13 98.19 10.70 -5 -5 -13 99.49 13.00 5 5 13 103.49 14.00 -6 -5 -13 19.60 7.30 6 5 13 15.10 7.40 -2 -6 -13 27.70 7.80 -2 -6 -13 16.70 7.20 2 6 13 19.00 8.40 -3 -6 -13 102.59 13.40 -3 -6 -13 136.89 13.00 3 6 13 109.69 14.70 -4 -6 -13 13.00 6.20 -4 -6 -13 11.10 5.30 4 6 13 19.80 8.30 -5 -6 -13 173.28 13.80 -5 -6 -13 178.98 16.40 5 6 13 178.08 17.20 -6 -6 -13 9.20 5.60 -6 -6 -13 24.60 6.90 6 6 13 17.40 7.70 -3 -7 -13 17.00 6.30 -3 -7 -13 19.10 7.70 3 7 13 19.70 7.90 -4 -7 -13 18.40 6.30 -4 -7 -13 15.00 6.90 4 7 13 21.90 8.40 -5 -7 -13 78.89 10.20 -5 -7 -13 63.39 11.60 5 7 13 81.69 14.30 -6 -7 -13 4.30 4.20 -6 -7 -13 20.20 7.20 6 7 13 13.30 7.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 26619 _shelx_res_file ; TITL S0854 S0854_0m_a.res created by SHELXL-2018/3 at 14:02:22 on 22-Feb-2021 CELL 0.71073 8.6450 9.1660 9.3403 67.433 72.887 63.062 ZERR 1.000 0.0005 0.0005 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N I F UNIT 16 10 2 6 6 TEMP -70.000 SIZE 0.08 0.131 0.236 L.S. 10 BOND $H LIST 4 ACTA CONF EQIV $2 -x+2, -y+1, -z+1 HTAB N1 I2_$2 EQIV $3 x+1, y-1, z+1 HTAB C7 F2_$3 EQIV $4 x+1, y-1, z HTAB C7 I3_$4 EQIV $5 x, y, z+1 HTAB C8 I2_$5 EQIV $1 -x+2, -y, -z+2 HTAB C8 I1_$1 DFIX 0.83 N1 H1 FMAP 2 PLAN 20 WGHT 0.017600 0.104300 FVAR 0.32676 I1 4 0.826829 0.382763 0.699965 11.00000 0.02951 0.02437 = 0.02130 -0.00148 -0.00948 -0.00916 N1 3 1.023130 0.157180 0.947253 11.00000 0.04154 0.02892 = 0.02273 -0.00196 -0.01117 -0.01765 H1 2 1.079356 0.212084 0.952405 11.00000 -1.20000 C1 1 0.681786 0.558854 0.514102 11.00000 0.02530 0.02607 = 0.01987 -0.00277 -0.00777 -0.01088 F1 5 0.861921 0.392880 0.343791 11.00000 0.03669 0.02707 = 0.02996 -0.01149 -0.00890 0.00205 I2 4 0.700103 0.609601 0.023896 11.00000 0.04118 0.03267 = 0.02151 -0.01114 -0.00498 -0.01026 C2 1 0.726482 0.535583 0.366327 11.00000 0.02406 0.02228 = 0.02549 -0.00818 -0.00173 -0.00740 F2 5 0.412725 0.915453 0.149330 11.00000 0.03803 0.02667 = 0.02112 -0.00164 -0.01408 -0.00632 I3 4 0.228665 1.045309 0.445949 11.00000 0.02595 0.02909 = 0.02966 -0.01089 -0.00403 -0.00356 C3 1 0.637626 0.652188 0.241930 11.00000 0.02758 0.02273 = 0.01907 -0.00741 -0.00486 -0.00908 F3 5 0.486658 0.729172 0.676360 11.00000 0.03576 0.03988 = 0.01749 -0.01042 -0.00386 -0.00720 C7 1 1.157963 0.006828 0.898807 11.00000 0.02801 0.03805 = 0.02491 -0.00358 -0.00765 -0.01192 AFIX 23 H7A 2 1.243223 -0.060464 0.972668 11.00000 -1.20000 H7AB 2 1.220520 0.044203 0.794519 11.00000 -1.20000 AFIX 0 C6 1 0.538121 0.704137 0.533587 11.00000 0.02719 0.02871 = 0.01620 -0.00577 -0.00175 -0.01367 C5 1 0.444434 0.827522 0.413084 11.00000 0.02034 0.02066 = 0.02386 -0.00614 -0.00394 -0.00729 C4 1 0.499125 0.797154 0.268939 11.00000 0.02423 0.02213 = 0.02157 0.00024 -0.01033 -0.01062 C8 1 0.930132 0.101552 1.104281 11.00000 0.04250 0.02933 = 0.02195 -0.00916 -0.00686 -0.01066 AFIX 23 H8A 2 0.841947 0.201779 1.136757 11.00000 -1.20000 H8AB 2 1.013321 0.034933 1.180012 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM S0854 REM wR2 = 0.0475, GooF = S = 1.023, Restrained GooF = 1.023 for all data REM R1 = 0.0250 for 3193 Fo > 4sig(Fo) and 0.0324 for all 3761 data REM 139 parameters refined using 1 restraints END WGHT 0.0176 0.1043 REM Highest difference peak 0.560, deepest hole -0.644, 1-sigma level 0.134 Q1 1 0.6033 0.6145 0.1393 11.00000 0.05 0.56 Q2 1 0.9611 0.5439 0.2592 11.00000 0.05 0.56 Q3 1 0.7565 0.6806 -0.0425 11.00000 0.05 0.56 Q4 1 0.2075 0.9787 0.4441 11.00000 0.05 0.54 Q5 1 0.7373 0.6757 0.6218 11.00000 0.05 0.54 Q6 1 0.7877 0.2975 0.7797 11.00000 0.05 0.54 Q7 1 0.1566 0.9761 0.5366 11.00000 0.05 0.53 Q8 1 0.6406 0.4987 0.4953 11.00000 0.05 0.52 Q9 1 0.8866 0.0657 1.0820 11.00000 0.05 0.48 Q10 1 0.6567 0.7640 -0.1282 11.00000 0.05 0.48 Q11 1 0.9350 0.4991 0.4430 11.00000 0.05 0.46 Q12 1 0.3090 1.1420 0.1713 11.00000 0.05 0.45 Q13 1 0.7423 0.5866 0.4704 11.00000 0.05 0.44 Q14 1 1.0527 -0.1055 1.2788 11.00000 0.05 0.44 Q15 1 0.5041 0.7070 0.5975 11.00000 0.05 0.44 Q16 1 1.1427 -0.0372 1.1115 11.00000 0.05 0.44 Q17 1 0.2833 0.8617 0.2029 11.00000 0.05 0.44 Q18 1 0.9230 0.3849 0.6267 11.00000 0.05 0.44 Q19 1 0.7220 0.8056 -0.0738 11.00000 0.05 0.44 Q20 1 0.1200 1.3136 0.3808 11.00000 0.05 0.44 ; _shelx_res_checksum 48743 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 I I1 0.82683(3) 0.38276(3) 0.69997(2) 0.02587(5) Uani d 1 . . N N1 1.0231(4) 0.1572(3) 0.9473(3) 0.0297(6) Uani d 1 . . H H1 1.079(4) 0.212(4) 0.952(4) 0.036 Uiso d 1 . . C C1 0.6818(4) 0.5589(4) 0.5141(3) 0.0236(6) Uani d 1 . . F F1 0.8619(2) 0.3929(2) 0.3438(2) 0.0350(5) Uani d 1 . . I I2 0.70010(3) 0.60960(3) 0.02390(2) 0.03224(6) Uani d 1 . . C C2 0.7265(4) 0.5356(4) 0.3663(4) 0.0246(6) Uani d 1 . . F F2 0.4127(2) 0.9155(2) 0.1493(2) 0.0305(4) Uani d 1 . . I I3 0.22867(3) 1.04531(3) 0.44595(3) 0.03033(6) Uani d 1 . . C C3 0.6376(4) 0.6522(4) 0.2419(3) 0.0226(6) Uani d 1 . . F F3 0.4867(2) 0.7292(2) 0.6764(2) 0.0334(4) Uani d 1 . . C C7 1.1580(4) 0.0068(4) 0.8988(4) 0.0316(7) Uani d 1 . . H H7A 1.243223 -0.060464 0.972668 0.038 Uiso calc 1 . . H H7AB 1.220520 0.044203 0.794519 0.038 Uiso calc 1 . . C C6 0.5381(4) 0.7041(4) 0.5336(3) 0.0235(6) Uani d 1 . . C C5 0.4444(4) 0.8275(4) 0.4131(3) 0.0218(6) Uani d 1 . . C C4 0.4991(4) 0.7972(4) 0.2689(3) 0.0225(6) Uani d 1 . . C C8 0.9301(4) 0.1016(4) 1.1043(4) 0.0315(7) Uani d 1 . . H H8A 0.841947 0.201779 1.136757 0.038 Uiso calc 1 . . H H8AB 1.013321 0.034933 1.180012 0.038 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.02951(11) 0.02437(10) 0.02130(10) -0.00916(8) -0.00948(8) -0.00148(8) N1 0.0415(17) 0.0289(15) 0.0227(14) -0.0176(13) -0.0112(12) -0.0020(12) C1 0.0253(15) 0.0261(16) 0.0199(15) -0.0109(12) -0.0078(12) -0.0028(12) F1 0.0367(11) 0.0271(10) 0.0300(11) 0.0021(8) -0.0089(8) -0.0115(8) I2 0.04118(13) 0.03267(12) 0.02151(11) -0.01026(9) -0.00498(9) -0.01114(9) C2 0.0241(15) 0.0223(15) 0.0255(16) -0.0074(12) -0.0017(12) -0.0082(13) F2 0.0380(11) 0.0267(10) 0.0211(9) -0.0063(8) -0.0141(8) -0.0016(8) I3 0.02595(11) 0.02909(11) 0.02966(12) -0.00356(8) -0.00403(8) -0.01089(9) C3 0.0276(15) 0.0227(15) 0.0191(15) -0.0091(12) -0.0049(12) -0.0074(12) F3 0.0358(11) 0.0399(11) 0.0175(9) -0.0072(9) -0.0039(8) -0.0104(8) C7 0.0280(17) 0.0381(19) 0.0249(17) -0.0119(14) -0.0076(13) -0.0036(14) C6 0.0272(16) 0.0287(16) 0.0162(14) -0.0137(13) -0.0017(11) -0.0058(12) C5 0.0203(14) 0.0207(14) 0.0239(15) -0.0073(11) -0.0039(11) -0.0061(12) C4 0.0242(15) 0.0221(15) 0.0216(15) -0.0106(12) -0.0103(12) 0.0002(12) C8 0.042(2) 0.0293(18) 0.0219(16) -0.0107(15) -0.0069(14) -0.0092(14) 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' I I -0.4742 1.8119 '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 C8 N1 C7 . . 110.0(2) ? C8 N1 H1 . . 108(2) ? C7 N1 H1 . . 106(2) ? C6 C1 C2 . . 116.5(3) ? C6 C1 I1 . . 121.3(2) ? C2 C1 I1 . . 122.2(2) ? F1 C2 C3 . . 118.5(3) ? F1 C2 C1 . . 118.4(3) ? C3 C2 C1 . . 123.0(3) ? C4 C3 C2 . . 117.1(3) ? C4 C3 I2 . . 120.5(2) ? C2 C3 I2 . . 122.4(2) ? N1 C7 C8 . 2_757 109.0(3) ? N1 C7 H7A . . 109.9 ? C8 C7 H7A 2_757 . 109.9 ? N1 C7 H7AB . . 109.9 ? C8 C7 H7AB 2_757 . 109.9 ? H7A C7 H7AB . . 108.3 ? F3 C6 C1 . . 118.5(3) ? F3 C6 C5 . . 118.1(3) ? C1 C6 C5 . . 123.3(3) ? C4 C5 C6 . . 116.7(3) ? C4 C5 I3 . . 120.8(2) ? C6 C5 I3 . . 122.5(2) ? F2 C4 C3 . . 118.6(3) ? F2 C4 C5 . . 118.1(3) ? C3 C4 C5 . . 123.3(3) ? N1 C8 C7 . 2_757 109.4(3) ? N1 C8 H8A . . 109.8 ? C7 C8 H8A 2_757 . 109.8 ? N1 C8 H8AB . . 109.8 ? C7 C8 H8AB 2_757 . 109.8 ? H8A C8 H8AB . . 108.2 ? 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 C1 . 2.118(3) ? N1 C8 . 1.470(4) ? N1 C7 . 1.475(4) ? N1 H1 . 0.864(18) ? C1 C6 . 1.380(4) ? C1 C2 . 1.392(4) ? F1 C2 . 1.343(3) ? I2 C3 . 2.089(3) ? C2 C3 . 1.382(4) ? F2 C4 . 1.345(3) ? I3 C5 . 2.078(3) ? C3 C4 . 1.379(4) ? F3 C6 . 1.350(3) ? C7 C8 2_757 1.513(5) ? C7 H7A . 0.9800 ? C7 H7AB . 0.9800 ? C6 C5 . 1.390(4) ? C5 C4 . 1.381(4) ? C8 H8A . 0.9800 ? C8 H8AB . 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 N1 H1 I2 2_766 0.864(18) 3.115(18) 3.978(3) 177(3) yes C7 H7A F2 1_646 0.98 2.40 3.299(4) 152.0 yes C7 H7AB I3 1_645 0.98 3.23 3.990(3) 135.4 yes C8 H8A I2 1_556 0.98 3.19 4.001(3) 141.3 yes C8 H8AB I1 2_757 0.98 3.26 3.879(3) 122.5 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 C6 C1 C2 F1 . . . . -177.8(3) ? I1 C1 C2 F1 . . . . 2.8(4) ? C6 C1 C2 C3 . . . . 2.0(5) ? I1 C1 C2 C3 . . . . -177.5(2) ? F1 C2 C3 C4 . . . . 179.9(3) ? C1 C2 C3 C4 . . . . 0.1(5) ? F1 C2 C3 I2 . . . . 2.5(4) ? C1 C2 C3 I2 . . . . -177.3(2) ? C8 N1 C7 C8 . . . 2_757 60.1(3) ? C2 C1 C6 F3 . . . . 177.9(3) ? I1 C1 C6 F3 . . . . -2.6(4) ? C2 C1 C6 C5 . . . . -2.8(5) ? I1 C1 C6 C5 . . . . 176.6(2) ? F3 C6 C5 C4 . . . . -179.3(3) ? C1 C6 C5 C4 . . . . 1.5(5) ? F3 C6 C5 I3 . . . . -0.7(4) ? C1 C6 C5 I3 . . . . -179.9(2) ? C2 C3 C4 F2 . . . . 178.3(3) ? I2 C3 C4 F2 . . . . -4.3(4) ? C2 C3 C4 C5 . . . . -1.6(5) ? I2 C3 C4 C5 . . . . 175.8(2) ? C6 C5 C4 F2 . . . . -179.0(3) ? I3 C5 C4 F2 . . . . 2.4(4) ? C6 C5 C4 C3 . . . . 0.8(4) ? I3 C5 C4 C3 . . . . -177.8(2) ? C7 N1 C8 C7 . . . 2_757 -60.3(4) ? _cod_database_fobs_code 1564915