#------------------------------------------------------------------------------ #$Date: 2019-04-26 05:34:48 +0300 (Fri, 26 Apr 2019) $ #$Revision: 214790 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/29/2242913.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_2242913 loop_ _publ_author_name 'Matsulevich, Zhanna V.' 'Lukiyanova, Julia M.' 'Naumov, Vladimir I.' 'Borisova, Galina N.' 'Osmanov, Vladimir K.' 'Borisov, Alexander V.' 'Grishina, Maria M.' 'Khrustalev, Victor N.' _publ_section_title ; Bromination of bis(pyridin-2-yl) diselenide in methylene chloride: the reaction mechanism and crystal structures of 1H-pyridine-2-selenenyl dibromide and its cycloadduct with cyclopentene (3aSR,9aRS)-2,3,3a,9a-tetrahydro-1H-cyclopenta[4,5][1,3]selenazolo[3,2-a]pyridinium bromide ; _journal_coeditor_code YK2121 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 675 _journal_page_last 679 _journal_paper_doi 10.1107/S2056989019004997 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C5 H5 Br2 N Se' _chemical_formula_moiety 'C5 H5 Br2 N Se' _chemical_formula_sum 'C5 H5 Br2 N Se' _chemical_formula_weight 317.86 _chemical_name_common ; 1H-Pyridine-2-selenenyl dibromide ; _chemical_name_systematic ; Dibromo(pyridin-1-ium-2-yl)selanide ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2015 _cell_angle_alpha 90 _cell_angle_beta 114.9750(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.0971(6) _cell_length_b 12.6116(10) _cell_length_c 8.7325(7) _cell_measurement_reflns_used 4271 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 32.61 _cell_measurement_theta_min 2.78 _cell_volume 808.36(11) _computing_cell_refinement ; SAINT (Bruker, 2002) ; _computing_data_collection ; APEX2 (Bruker, 2005) ; _computing_data_reduction ; SAINT (Bruker, 2002) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXTL (Sheldrick, 2008) ; _computing_structure_solution ; SHELXTL (Sheldrick, 2008) ; _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _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 0.0510 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 12425 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.624 _diffrn_reflns_theta_min 2.775 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 14.444 _exptl_absorpt_correction_T_max 0.104 _exptl_absorpt_correction_T_min 0.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 2003) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.612 _exptl_crystal_description prism _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.365 _refine_diff_density_min -1.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 85 _refine_ls_number_reflns 2959 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0317 _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^)+(0.0302P)^2^+0.5977P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.0740 _reflns_number_gt 2426 _reflns_number_total 2959 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yk2121sup1.cif _cod_data_source_block 1 _cod_database_code 2242913 _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 0.160 _shelx_estimated_absorpt_t_max 0.221 _shelx_hkl_file ; -1 0 0 369.88 20.54 -1 0 0 340.35 19.93 -1 0 0 358.92 21.94 -2 0 0 65.41 3.78 -2 0 0 63.36 4.02 -3 0 0 42.96 2.51 -3 0 0 40.80 2.65 -3 0 0 39.56 2.60 -4 0 0 0.44 0.64 -4 0 0 0.87 0.40 -4 0 0 0.82 0.34 5 0 0 60.23 3.85 -5 0 0 55.02 3.78 -5 0 0 62.98 3.67 -6 0 0 40.75 2.79 6 0 0 38.01 2.53 -6 0 0 36.42 2.45 -7 0 0 20.78 1.64 7 0 0 18.73 1.79 7 0 0 20.93 1.51 -8 0 0 1.83 0.75 8 0 0 1.77 1.01 9 0 0 100.08 6.16 -9 0 0 100.36 6.13 10 0 0 45.05 3.22 -10 0 0 45.11 3.11 -11 0 0 2.89 1.02 11 0 0 2.66 1.01 0 -1 0 -0.01 0.02 0 -1 0 0.05 0.04 0 1 0 0.10 0.04 0 1 0 0.02 0.06 0 1 0 0.00 0.03 1 -1 0 8.28 0.67 -1 -1 0 9.61 0.65 -1 -1 0 9.96 0.63 1 1 0 9.29 0.68 -1 1 0 10.73 0.72 2 -1 0 42.71 2.99 -2 -1 0 54.43 2.99 -2 -1 0 52.84 2.98 -2 1 0 49.40 3.17 2 1 0 49.92 3.18 -2 1 0 49.98 2.98 -3 -1 0 24.30 1.44 -3 -1 0 25.54 1.61 -3 1 0 17.36 1.57 -3 1 0 21.50 1.50 3 1 0 21.88 1.52 -3 1 0 22.68 1.44 -4 -1 0 180.54 9.83 -4 -1 0 164.56 9.69 -4 1 0 177.90 9.84 4 1 0 168.54 10.47 -4 1 0 169.19 10.46 -4 1 0 146.07 9.69 -5 -1 0 298.63 18.14 -5 -1 0 332.07 18.56 5 -1 0 291.12 18.13 -5 1 0 334.89 19.78 5 1 0 323.17 19.79 -5 1 0 334.41 18.57 6 -1 0 111.80 6.63 -6 -1 0 102.40 6.34 -6 -1 0 109.91 6.29 6 -1 0 97.83 6.30 6 1 0 103.59 6.64 -6 1 0 103.74 6.29 -7 -1 0 1.42 0.65 7 -1 0 0.23 0.43 7 -1 0 -1.22 0.71 -7 -1 0 -0.13 0.80 7 1 0 0.98 0.48 -7 1 0 1.56 0.69 -8 -1 0 11.14 1.13 8 -1 0 9.16 1.34 -8 1 0 11.29 1.18 8 1 0 9.93 1.32 9 -1 0 23.82 1.94 -9 -1 0 21.56 1.83 -9 1 0 19.17 1.88 9 1 0 21.76 2.12 10 -1 0 16.60 1.63 -10 -1 0 13.65 1.46 10 1 0 13.51 1.65 -10 1 0 15.25 1.54 11 -1 0 -0.04 0.93 11 1 0 -0.40 0.95 -11 1 0 -0.37 0.94 0 -2 0 28.14 1.60 0 2 0 26.90 1.81 0 2 0 28.26 1.64 -1 -2 0 209.14 10.87 -1 -2 0 167.83 11.20 1 -2 0 184.76 10.85 1 2 0 197.41 11.99 -1 2 0 208.44 11.20 2 -2 0 214.97 14.08 -2 -2 0 265.80 14.49 -2 -2 0 248.36 14.08 -2 2 0 249.81 14.50 -2 2 0 279.71 15.53 2 2 0 244.73 15.49 3 -2 0 103.88 6.62 -3 -2 0 120.04 6.70 -3 -2 0 119.06 6.61 -3 2 0 116.06 7.16 3 2 0 112.07 7.16 -3 2 0 115.86 6.72 -4 -2 0 284.28 15.48 4 -2 0 244.06 15.14 -4 -2 0 264.35 15.12 4 2 0 266.74 16.53 -4 2 0 263.27 16.50 -4 2 0 275.52 15.50 -5 -2 0 4.79 0.64 5 -2 0 4.91 0.94 -5 -2 0 7.08 0.99 5 2 0 5.13 0.64 -5 2 0 5.81 0.72 -5 2 0 6.40 0.63 -6 -2 0 65.99 4.16 6 -2 0 62.57 4.17 -6 -2 0 67.42 4.05 -6 2 0 65.79 4.08 -6 2 0 68.59 4.24 6 2 0 65.33 4.26 -7 -2 0 2.22 0.96 -7 -2 0 4.08 0.73 7 -2 0 2.73 0.94 7 -2 0 3.27 0.53 7 2 0 2.37 0.59 -7 2 0 2.95 0.68 8 -2 0 8.64 1.27 -8 -2 0 10.68 1.43 -8 -2 0 11.36 1.09 -8 2 0 9.54 1.11 9 -2 0 0.95 0.86 -9 -2 0 0.07 0.73 9 2 0 -0.44 1.01 -9 2 0 0.24 0.86 -10 -2 0 9.01 1.15 10 -2 0 7.69 1.20 10 2 0 9.48 1.44 -10 2 0 8.19 1.25 11 -2 0 30.37 2.22 -11 2 0 25.63 2.39 11 2 0 23.70 2.42 0 -3 0 0.77 0.21 0 3 0 0.30 0.19 0 3 0 0.90 0.36 1 -3 0 490.92 28.72 -1 -3 0 568.11 28.75 -1 -3 0 448.08 29.68 1 3 0 566.25 31.76 -1 3 0 474.45 31.80 -1 3 0 541.68 29.68 -2 -3 0 106.41 6.24 -2 -3 0 109.00 6.09 2 -3 0 105.06 6.07 2 3 0 103.55 6.69 -2 3 0 108.89 6.77 -2 3 0 107.79 6.24 3 -3 0 1.35 0.49 -3 -3 0 0.89 0.31 -3 -3 0 1.66 0.47 -3 3 0 0.84 0.34 3 3 0 1.53 0.41 -3 3 0 0.99 0.37 4 -3 0 6.55 0.85 -4 -3 0 4.91 0.76 -4 -3 0 5.91 0.59 4 3 0 5.64 0.65 -4 3 0 5.74 0.63 -4 3 0 4.82 0.61 5 -3 0 1.18 0.70 -5 -3 0 1.91 0.68 -5 -3 0 2.35 0.52 5 3 0 1.84 0.52 -5 3 0 3.52 0.63 -5 3 0 2.72 0.47 -6 -3 0 29.81 2.40 6 -3 0 38.27 2.50 -6 -3 0 34.77 2.29 6 3 0 34.46 2.40 -6 3 0 35.79 2.35 -6 3 0 34.77 2.35 -7 -3 0 3.19 1.02 7 -3 0 4.56 0.99 -7 -3 0 5.60 0.79 -7 3 0 5.49 0.93 -7 3 0 6.69 0.76 7 3 0 4.31 0.72 8 -3 0 31.99 2.29 -8 -3 0 30.92 2.41 -8 -3 0 29.55 2.12 8 3 0 27.76 2.12 -8 3 0 28.23 2.15 -9 -3 0 17.29 1.75 9 -3 0 17.81 1.64 -9 -3 0 13.89 1.34 -9 3 0 13.14 1.46 10 -3 0 0.47 0.86 -10 3 0 -0.95 0.91 10 3 0 1.12 1.09 0 -4 0 0.88 0.20 0 -4 0 1.32 0.26 0 4 0 1.51 0.46 -1 -4 0 6.69 0.58 -1 -4 0 5.36 0.52 1 -4 0 6.02 0.51 -1 4 0 6.37 0.53 1 4 0 5.75 0.63 -1 4 0 4.96 0.69 -2 -4 0 222.16 14.42 2 -4 0 249.63 13.97 -2 -4 0 268.39 14.01 2 4 0 263.94 15.46 -2 4 0 261.03 14.43 -2 4 0 227.76 15.56 3 -4 0 10.35 0.99 -3 -4 0 13.08 1.02 -3 -4 0 12.90 0.92 -3 4 0 11.15 0.95 3 4 0 14.20 1.10 -3 4 0 12.75 1.13 4 -4 0 3.38 0.67 -4 -4 0 6.44 0.58 -4 -4 0 5.29 0.71 -4 4 0 4.64 0.64 4 4 0 4.79 0.65 -4 4 0 4.39 0.61 5 -4 0 7.81 0.98 -5 -4 0 8.47 0.76 -5 -4 0 7.19 1.00 -5 4 0 7.08 0.81 5 4 0 8.27 0.85 -5 4 0 7.02 0.78 -6 -4 0 1.73 0.56 6 -4 0 2.80 0.80 -6 -4 0 1.41 0.81 -6 4 0 2.31 0.66 -6 4 0 2.63 0.56 6 4 0 2.32 0.62 -7 -4 0 92.46 5.88 7 -4 0 110.01 5.87 -7 -4 0 96.19 5.83 -7 4 0 96.25 5.93 7 4 0 93.86 6.22 -8 -4 0 34.22 2.39 -8 -4 0 34.12 2.67 8 -4 0 36.70 2.51 8 4 0 33.98 2.49 -8 4 0 36.83 2.56 -9 -4 0 0.18 1.02 9 -4 0 -0.26 0.76 -9 4 0 0.34 0.78 10 -4 0 5.62 1.01 -10 4 0 2.97 1.02 0 -5 0 0.31 0.21 0 -5 0 0.53 0.27 0 5 0 0.83 0.51 1 -5 0 10.30 0.74 -1 -5 0 9.25 0.74 -1 -5 0 9.01 0.75 -1 5 0 10.78 1.08 1 5 0 9.55 0.96 -1 5 0 9.44 0.75 2 -5 0 129.85 7.02 -2 -5 0 102.37 7.24 -2 -5 0 131.66 7.06 2 5 0 126.12 7.80 -2 5 0 128.24 7.24 -3 -5 0 363.00 20.03 -3 -5 0 352.04 20.60 3 -5 0 354.04 19.98 -3 5 0 348.28 20.62 -3 5 0 374.84 22.18 3 5 0 345.54 22.07 -4 -5 0 8.67 0.79 -4 -5 0 6.70 0.87 4 -5 0 7.62 0.86 -4 5 0 8.85 0.89 4 5 0 8.44 0.90 -4 5 0 9.27 0.90 -5 -5 0 0.34 0.63 5 -5 0 -0.39 0.60 -5 -5 0 0.06 0.40 -5 5 0 -0.53 0.46 5 5 0 0.50 0.56 -5 5 0 -0.21 0.53 6 -5 0 66.07 4.07 -6 -5 0 63.61 4.14 -6 -5 0 65.34 4.02 -6 5 0 66.33 4.29 -6 5 0 67.45 4.15 6 5 0 68.28 4.35 -7 -5 0 42.09 3.05 -7 -5 0 43.62 2.82 7 -5 0 48.72 2.95 7 5 0 43.61 3.04 -7 5 0 44.25 2.99 -8 -5 0 4.42 1.05 8 -5 0 2.72 0.85 -8 5 0 2.90 0.92 8 5 0 3.50 0.76 9 -5 0 3.61 0.88 -9 -5 0 3.24 1.11 -9 5 0 3.21 0.92 -10 -5 0 -0.05 1.08 10 -5 0 0.17 0.78 -10 5 0 0.62 0.99 0 -6 0 210.88 12.75 0 -6 0 219.58 12.38 0 6 0 231.10 13.81 -1 -6 0 66.09 3.81 1 -6 0 65.22 3.77 -1 -6 0 63.64 3.88 -1 6 0 67.30 4.40 -1 6 0 64.43 3.88 1 6 0 63.79 4.29 2 -6 0 29.96 1.81 -2 -6 0 32.32 1.87 -2 -6 0 23.85 1.85 2 6 0 30.11 2.15 -2 6 0 32.19 1.88 -2 6 0 24.72 2.29 -3 -6 0 36.10 2.30 -3 -6 0 33.59 2.28 3 -6 0 35.78 2.25 -3 6 0 34.90 2.68 3 6 0 39.03 2.58 -3 6 0 37.79 2.30 4 -6 0 16.52 1.33 -4 -6 0 17.40 1.44 -4 -6 0 17.26 1.21 -4 6 0 15.40 1.30 4 6 0 16.87 1.49 -4 6 0 17.92 1.51 5 -6 0 14.55 1.40 -5 -6 0 16.92 1.20 -5 -6 0 16.05 1.51 -5 6 0 16.12 1.42 -5 6 0 16.78 1.42 5 6 0 16.17 1.48 -6 -6 0 37.20 2.37 -6 -6 0 38.81 2.57 6 -6 0 36.70 2.51 -6 6 0 38.06 2.51 6 6 0 37.58 2.64 -6 6 0 35.37 2.55 -7 -6 0 19.12 1.79 7 -6 0 19.46 1.63 7 6 0 17.61 1.61 -7 6 0 18.22 1.71 8 -6 0 11.77 1.26 -8 -6 0 12.16 1.49 8 6 0 12.99 1.26 -8 6 0 11.62 1.34 -9 -6 0 30.30 2.37 9 -6 0 28.83 2.19 -9 6 0 29.38 2.28 10 -6 0 10.83 1.26 -10 -6 0 11.49 1.50 -10 6 0 9.93 1.42 0 -7 0 0.40 0.31 0 -7 0 1.23 0.41 0 7 0 0.72 0.65 -1 -7 0 108.28 6.19 1 -7 0 104.74 6.16 -1 -7 0 107.47 6.35 -1 7 0 106.37 6.35 1 7 0 105.50 6.94 -1 7 0 117.05 7.11 -2 -7 0 0.68 0.52 2 -7 0 0.72 0.42 -2 -7 0 1.13 0.40 2 7 0 0.94 0.66 -2 7 0 0.37 0.44 -2 7 0 0.34 0.70 -3 -7 0 17.12 1.29 -3 -7 0 10.65 1.10 3 -7 0 15.75 1.12 -3 7 0 14.27 1.19 3 7 0 17.13 1.47 -3 7 0 9.91 1.45 -4 -7 0 112.62 6.94 -4 -7 0 118.08 7.03 4 -7 0 124.01 6.90 -4 7 0 120.18 7.11 -4 7 0 129.67 7.75 4 7 0 115.29 7.65 5 -7 0 184.22 9.88 -5 -7 0 164.95 9.90 -5 -7 0 161.01 10.04 -5 7 0 182.88 10.86 -5 7 0 173.20 10.17 5 7 0 169.02 10.87 -6 -7 0 5.49 0.91 6 -7 0 1.90 0.76 6 7 0 4.48 0.85 -6 7 0 3.23 0.69 -6 7 0 2.40 0.73 -7 -7 0 1.89 0.94 7 -7 0 0.62 0.75 -7 7 0 1.08 0.83 7 7 0 1.23 0.73 -8 -7 0 9.60 1.38 8 -7 0 9.09 1.13 8 7 0 10.37 1.15 -8 7 0 8.23 1.13 9 -7 0 0.44 0.78 -9 -7 0 -0.35 0.86 -9 7 0 0.27 0.94 -10 -7 0 29.66 2.51 10 -7 0 28.61 2.19 -10 7 0 28.69 2.48 0 -8 0 73.95 4.53 0 -8 0 76.02 4.43 0 8 0 78.99 5.13 1 -8 0 36.80 2.26 -1 -8 0 37.98 2.34 -1 -8 0 35.18 2.28 -1 8 0 34.95 2.33 -1 8 0 41.62 2.98 1 8 0 37.18 2.78 -2 -8 0 0.74 0.41 -2 -8 0 0.24 0.54 2 -8 0 0.55 0.47 2 8 0 0.82 0.67 -2 8 0 1.23 0.97 -2 8 0 0.56 0.49 -3 -8 0 5.50 0.80 3 -8 0 3.55 0.59 -3 -8 0 2.28 0.55 3 8 0 2.20 0.84 -3 8 0 3.42 1.06 -3 8 0 2.90 0.64 -4 -8 0 11.91 0.97 -4 -8 0 13.54 1.23 4 -8 0 12.25 1.17 4 8 0 11.11 1.27 -4 8 0 12.21 1.38 -4 8 0 13.11 1.16 5 -8 0 2.50 0.70 -5 -8 0 5.32 0.92 -5 8 0 1.85 0.71 5 8 0 2.22 0.80 -5 8 0 1.99 0.68 -6 -8 0 0.19 0.72 6 -8 0 0.58 0.69 -6 8 0 -0.26 0.59 -6 8 0 -0.66 0.72 6 8 0 -0.80 0.67 -7 -8 0 1.53 0.94 7 -8 0 1.23 0.78 -7 8 0 1.71 0.77 7 8 0 2.20 0.81 -8 -8 0 -1.29 0.80 8 -8 0 -0.47 0.74 -8 8 0 0.24 0.79 8 8 0 0.58 0.76 9 -8 0 2.16 0.83 -9 -8 0 1.12 1.07 -9 8 0 2.42 0.93 -10 -8 0 5.46 1.16 -10 8 0 4.58 1.21 0 -9 0 0.53 0.48 0 -9 0 0.30 0.38 0 9 0 1.06 0.85 1 -9 0 175.63 9.85 -1 -9 0 173.98 9.88 1 -9 0 161.65 10.14 -1 -9 0 179.37 10.18 1 9 0 167.93 11.07 -1 9 0 186.89 11.28 2 -9 0 27.03 1.80 -2 -9 0 27.40 1.85 -2 -9 0 28.95 1.85 2 9 0 27.15 2.23 -2 9 0 26.43 1.89 -2 9 0 27.26 2.53 3 -9 0 13.72 1.10 -3 -9 0 13.07 1.17 -3 -9 0 10.77 1.02 -3 9 0 12.68 1.14 3 9 0 11.03 1.27 -3 9 0 11.22 1.68 4 -9 0 4.97 0.74 -4 -9 0 5.39 0.92 -4 9 0 5.63 1.10 4 9 0 5.36 0.91 -4 9 0 4.49 0.75 -5 -9 0 8.10 1.11 5 -9 0 8.40 0.95 -5 9 0 8.25 1.09 5 9 0 7.43 1.05 -5 9 0 8.37 1.00 -6 -9 0 24.18 1.91 6 -9 0 24.07 1.82 -6 9 0 24.10 1.95 -6 9 0 25.41 1.93 6 9 0 19.45 2.02 -7 -9 0 3.28 1.06 7 -9 0 1.83 0.82 -7 9 0 1.94 0.83 7 9 0 2.90 0.90 8 -9 0 19.47 1.68 -8 -9 0 18.00 1.81 -8 9 0 19.65 1.78 8 9 0 18.60 1.83 -9 -9 0 13.94 1.65 -9 9 0 12.36 1.56 0 -10 0 6.53 0.78 0 -10 0 7.83 0.78 0 10 0 7.41 1.27 -1 -10 0 1.57 0.56 1 -10 0 0.65 0.45 1 -10 0 1.03 0.52 -1 -10 0 0.37 0.54 -1 10 0 1.16 1.13 1 10 0 -0.30 0.83 -2 -10 0 7.02 0.87 2 -10 0 5.76 0.74 -2 -10 0 7.68 0.76 2 10 0 4.67 1.01 -2 10 0 4.92 0.77 -2 10 0 6.17 1.47 -3 -10 0 65.01 4.20 3 -10 0 77.85 4.15 3 10 0 65.57 4.70 -3 10 0 69.00 4.27 -3 10 0 68.04 5.16 4 -10 0 77.34 4.46 -4 -10 0 75.76 4.57 -4 10 0 72.04 5.24 4 10 0 71.87 5.07 -4 10 0 77.15 4.67 5 -10 0 2.93 0.70 -5 -10 0 1.91 0.79 5 10 0 2.41 0.91 -5 10 0 3.61 0.87 -5 10 0 1.03 0.87 -6 -10 0 35.68 2.63 6 -10 0 35.12 2.44 6 10 0 34.87 2.79 -6 10 0 38.75 2.64 7 -10 0 38.33 2.44 -7 -10 0 34.15 2.59 7 10 0 34.00 2.77 -7 10 0 36.16 2.68 -8 -10 0 15.77 1.63 8 10 0 14.79 1.62 -8 10 0 19.96 1.76 -9 -10 0 7.61 1.29 -9 10 0 8.83 1.38 0 -11 0 0.44 0.56 0 -11 0 1.08 0.55 0 11 0 0.99 1.15 1 -11 0 10.87 1.09 1 -11 0 11.91 1.08 -1 -11 0 12.00 1.16 -1 -11 0 13.92 1.23 -1 11 0 16.50 1.98 1 11 0 11.73 1.53 2 -11 0 137.40 8.74 -2 -11 0 150.65 8.54 -2 -11 0 158.66 8.79 2 -11 0 153.54 8.50 2 11 0 147.43 9.63 -2 11 0 142.43 9.93 3 -11 0 162.34 9.05 -3 -11 0 155.20 9.12 -3 11 0 167.76 10.60 -3 11 0 157.07 9.38 3 11 0 152.02 10.16 4 -11 0 1.32 0.67 -4 -11 0 1.58 0.73 -4 11 0 0.48 1.10 -4 11 0 1.25 0.77 4 11 0 1.23 0.94 -5 -11 0 9.28 1.09 5 -11 0 8.20 0.95 5 11 0 6.94 1.19 -5 11 0 7.93 1.28 -5 11 0 6.70 1.01 -6 -11 0 8.32 1.24 6 -11 0 9.64 1.04 6 11 0 9.25 1.33 -6 11 0 9.78 1.25 -7 -11 0 19.35 1.81 7 11 0 18.11 1.84 -7 11 0 20.22 1.95 -8 -11 0 0.43 0.91 8 11 0 0.92 0.95 -8 11 0 1.06 1.05 -9 -11 0 -1.74 1.03 -9 11 0 0.72 1.10 0 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15.51 1.79 1 1 11 16.03 1.56 -10 -2 11 18.56 2.68 -10 2 11 27.07 2.79 -9 -2 11 -3.09 1.66 9 -2 -11 0.20 0.90 -9 2 11 3.60 1.60 8 -2 -11 10.06 1.35 -8 -2 11 8.22 1.99 -8 2 11 14.86 1.98 7 -2 -11 6.39 1.13 -7 -2 11 5.80 1.74 -7 2 11 6.88 1.45 6 -2 -11 1.12 0.87 -6 -2 11 0.42 1.34 6 2 -11 -0.35 0.79 -6 2 11 0.17 1.15 5 -2 -11 3.61 0.97 -5 -2 11 4.98 1.39 -5 2 11 4.00 1.22 5 2 -11 5.03 1.02 -4 -2 11 9.27 1.44 4 -2 -11 7.22 1.22 -4 -2 11 8.46 1.42 4 2 -11 8.44 1.27 -4 2 11 9.96 1.43 -3 -2 11 -0.11 1.08 3 -2 -11 0.59 0.80 -3 2 11 0.53 0.99 3 2 -11 0.59 0.95 -2 -2 11 22.18 2.10 2 -2 -11 23.49 2.06 2 2 -11 16.38 1.84 -1 -2 11 41.25 2.88 1 -2 -11 36.15 2.78 1 2 -11 33.50 2.87 0 -2 11 15.60 1.55 0 -2 -11 14.39 1.71 0 2 -11 14.58 1.68 1 -2 11 30.27 2.24 -1 -2 -11 25.88 2.35 -1 2 -11 26.91 2.53 1 2 11 27.46 2.05 10 -3 -11 31.75 2.64 10 3 -11 31.48 2.93 -10 3 11 40.50 3.56 9 -3 -11 0.55 0.94 -9 3 11 1.31 1.37 -8 -3 11 -1.44 1.58 8 -3 -11 1.26 0.95 -8 3 11 4.39 1.49 7 -3 -11 -0.72 0.84 -7 -3 11 -1.33 1.45 -7 3 11 1.71 1.29 -6 -3 11 11.40 1.90 6 -3 -11 13.71 1.50 -6 3 11 13.47 1.76 5 -3 -11 119.85 7.88 -5 -3 11 130.55 8.61 -5 -3 11 133.13 7.84 5 3 -11 135.54 7.95 -5 3 11 131.86 8.55 -4 -3 11 69.01 4.33 4 -3 -11 57.44 4.18 4 3 -11 64.07 4.21 -4 3 11 66.32 4.56 3 -3 -11 2.11 0.87 -3 -3 11 2.08 1.17 3 3 -11 3.43 1.04 -3 3 11 3.65 1.05 2 -3 -11 1.12 0.96 -2 -3 11 0.72 1.13 2 3 -11 1.32 1.00 1 -3 -11 15.63 1.65 -1 -3 11 15.39 1.65 1 3 -11 12.91 1.57 0 -3 -11 0.50 0.92 0 -3 11 1.39 1.02 0 3 -11 1.22 1.01 1 -3 11 3.84 1.05 -1 -3 -11 4.17 1.18 -1 3 -11 4.69 1.22 10 -4 -11 34.38 2.83 -10 4 11 43.91 3.65 10 4 -11 34.57 3.09 9 -4 -11 29.02 2.59 -9 4 11 42.57 3.41 9 4 -11 32.37 2.91 8 -4 -11 -0.62 0.89 8 4 -11 0.48 1.07 -8 4 11 0.73 1.23 7 -4 -11 4.27 0.99 7 4 -11 5.41 1.24 -7 4 11 5.33 1.49 -6 -4 11 14.78 1.65 6 -4 -11 9.88 1.38 -6 4 11 11.45 1.60 6 4 -11 10.75 1.46 -5 -4 11 23.23 2.03 5 -4 -11 16.34 1.75 -5 4 11 20.20 2.10 5 4 -11 16.84 1.88 4 -4 -11 -0.36 0.83 -4 -4 11 1.11 1.19 4 4 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0 5 -11 2.81 1.08 1 -5 11 23.47 2.13 -1 -5 -11 18.71 1.93 -1 5 -11 16.96 1.92 9 -6 -11 6.10 1.19 -9 6 11 9.65 1.78 9 6 -11 6.67 1.39 8 -6 -11 0.92 0.97 -8 -6 11 -0.56 1.22 8 6 -11 -0.27 1.06 -8 6 11 2.63 1.26 7 -6 -11 0.51 0.95 -7 -6 11 1.02 1.24 7 6 -11 0.75 1.02 -7 6 11 1.14 1.06 -6 -6 11 27.64 2.70 6 -6 -11 28.21 2.42 6 6 -11 28.75 2.47 -6 6 11 29.69 2.61 5 -6 -11 0.32 0.94 -5 -6 11 1.36 1.24 5 6 -11 0.37 0.89 -5 6 11 2.45 1.01 4 -6 -11 58.51 3.87 -4 -6 11 60.55 4.09 -4 6 11 55.19 4.05 3 -6 -11 21.00 2.03 -3 -6 11 20.88 2.12 -3 6 11 19.38 2.00 3 6 -11 22.24 2.05 -2 -6 11 12.32 1.73 2 -6 -11 9.32 1.35 2 6 -11 14.52 1.45 -1 -6 11 6.13 1.47 1 -6 -11 3.56 1.04 1 6 -11 4.60 1.08 0 -6 11 2.50 1.25 0 -6 -11 1.50 0.94 0 6 -11 2.08 1.03 8 -7 -11 2.63 1.10 -8 -7 11 2.00 1.31 -8 7 11 3.44 1.31 8 7 -11 3.39 1.20 7 -7 -11 0.22 0.98 -7 -7 11 1.38 1.28 -7 7 11 2.83 1.22 7 7 -11 1.97 1.08 -6 -7 11 0.70 1.26 6 -7 -11 0.57 0.97 6 7 -11 1.67 1.00 -6 7 11 2.73 1.10 5 -7 -11 -1.31 0.93 -5 -7 11 -0.42 1.17 -5 7 11 2.01 1.03 5 7 -11 0.39 0.88 4 -7 -11 3.80 1.10 -4 -7 11 6.25 1.54 -4 7 11 6.81 1.13 3 -7 -11 31.81 2.52 -3 -7 11 29.33 2.85 -3 7 11 30.36 2.45 -2 -7 11 17.00 1.94 2 -7 -11 15.39 1.63 1 -7 -11 1.27 0.89 -1 -7 11 1.69 1.30 1 7 -11 1.53 0.94 0 -7 -11 5.95 1.19 0 -7 11 3.97 1.28 0 7 -11 3.75 1.08 8 -8 -11 50.55 4.05 -8 -8 11 52.15 4.09 -8 8 11 70.70 4.56 8 8 -11 65.26 4.35 -7 -8 11 66.60 4.46 7 -8 -11 62.74 4.40 7 8 -11 60.65 4.58 -7 8 11 71.77 4.68 6 -8 -11 0.83 1.03 -6 -8 11 1.65 1.29 -6 8 11 1.75 1.11 6 8 -11 1.08 1.03 5 -8 -11 6.35 1.27 -5 -8 11 7.30 1.45 5 8 -11 8.70 1.31 -5 8 11 8.20 1.29 -4 -8 11 0.99 1.31 4 -8 -11 -0.02 0.94 -4 8 11 0.35 0.88 3 -8 -11 14.62 1.58 -3 -8 11 16.50 1.98 -3 8 11 13.23 1.46 2 -8 -11 38.21 2.96 -2 -8 11 38.54 3.30 1 -8 -11 2.26 1.05 -1 -8 11 1.15 1.43 -7 -9 11 2.16 1.38 7 -9 -11 3.01 1.02 -7 9 11 3.93 1.27 7 9 -11 2.50 1.09 6 -9 -11 1.95 1.09 -6 -9 11 3.12 1.43 -6 9 11 2.83 1.01 6 9 -11 3.21 1.12 5 -9 -11 0.64 1.03 -5 -9 11 2.13 1.29 -5 9 11 2.04 0.98 5 9 -11 1.82 1.05 4 -9 -11 11.72 1.53 -4 -9 11 16.58 1.98 -4 9 11 13.30 1.50 3 -9 -11 29.10 2.54 -3 -9 11 34.86 3.01 -3 9 11 31.24 2.50 2 -9 -11 12.66 1.55 -2 -9 11 13.90 1.82 6 -10 -11 13.97 1.63 -6 -10 11 14.01 1.83 6 10 -11 14.35 1.64 -6 10 11 11.02 1.49 5 -10 -11 0.54 1.03 -5 -10 11 1.32 1.42 -5 10 11 2.08 0.98 4 -10 -11 20.45 1.95 -4 -10 11 22.90 2.26 -4 10 11 18.47 1.99 3 -10 -11 4.47 1.05 -3 -10 11 4.73 1.54 -3 10 11 5.61 1.11 -9 0 12 22.09 2.53 -8 0 12 36.36 3.34 7 0 -12 5.71 1.09 -7 0 12 4.78 1.57 6 0 -12 20.09 1.89 -6 0 12 18.76 2.20 5 0 -12 12.07 1.37 -5 0 12 8.16 1.59 4 0 -12 106.55 6.64 3 0 -12 9.49 1.37 2 0 -12 7.78 1.23 1 0 -12 0.97 1.04 0 0 -12 3.42 1.04 -9 -1 12 22.39 2.89 -9 1 12 30.04 3.14 8 -1 -12 25.80 2.29 -8 -1 12 25.84 2.83 -8 1 12 28.63 3.03 -7 -1 12 3.54 1.58 7 -1 -12 3.91 0.99 -7 1 12 3.08 1.51 -6 -1 12 3.25 1.45 6 -1 -12 3.59 0.98 -6 1 12 3.55 1.39 6 1 -12 4.76 1.06 5 -1 -12 15.33 1.56 -5 -1 12 13.24 1.82 5 1 -12 15.16 1.58 -5 1 12 13.74 1.82 4 -1 -12 41.39 3.06 4 1 -12 42.33 3.07 3 -1 -12 29.34 2.52 3 1 -12 32.32 2.56 2 -1 -12 1.01 1.04 2 1 -12 -0.24 0.99 -1 -1 12 2.96 1.04 1 -1 -12 1.14 1.09 1 1 -12 1.53 0.95 9 -2 -12 14.11 1.55 -9 -2 12 8.05 2.26 -9 2 12 16.19 2.18 -8 -2 12 3.55 1.89 8 -2 -12 7.76 1.20 -8 2 12 8.39 1.77 7 -2 -12 0.69 0.88 -7 -2 12 -0.74 1.44 -7 2 12 1.59 1.39 6 -2 -12 8.89 1.24 -6 -2 12 7.75 1.73 -6 2 12 9.09 1.61 6 2 -12 10.92 1.32 5 -2 -12 2.28 0.97 -5 -2 12 -1.18 1.20 5 2 -12 1.82 0.98 -5 2 12 1.40 1.17 4 -2 -12 1.28 0.94 4 2 -12 0.31 0.92 -4 2 12 2.39 1.13 3 -2 -12 24.40 2.03 3 2 -12 20.27 2.13 2 -2 -12 33.58 2.67 -2 -2 12 36.22 2.70 2 2 -12 29.01 2.60 1 -2 -12 9.99 1.45 -1 -2 12 10.49 1.39 1 2 -12 8.48 1.36 9 -3 -12 -0.24 0.91 -9 3 12 -0.29 1.48 9 3 -12 0.86 1.20 8 -3 -12 5.25 1.14 -8 3 12 9.19 1.67 7 -3 -12 10.93 1.37 -7 3 12 13.24 1.75 6 -3 -12 -0.32 0.74 -6 3 12 1.22 1.23 5 -3 -12 26.11 2.26 5 3 -12 25.81 2.42 5 3 -12 27.15 2.25 -5 3 12 28.61 2.65 4 -3 -12 0.98 0.92 4 3 -12 2.62 1.02 -4 3 12 1.16 1.09 -3 -3 12 10.31 1.60 3 -3 -12 9.19 1.35 3 3 -12 10.08 1.37 -2 -3 12 3.46 1.24 2 -3 -12 1.59 1.02 2 3 -12 0.41 0.99 1 -3 -12 0.89 1.05 -1 -3 12 2.69 1.18 1 3 -12 2.30 1.02 8 -4 -12 -0.56 0.91 -8 4 12 1.88 1.36 8 4 -12 -0.69 1.05 7 -4 -12 10.31 1.41 -7 4 12 14.46 1.85 7 4 -12 13.67 1.69 6 -4 -12 33.47 2.69 6 4 -12 35.18 2.90 -6 4 12 37.38 3.01 5 -4 -12 4.35 1.10 -5 -4 12 8.30 1.65 5 4 -12 7.10 1.20 -5 4 12 8.39 1.36 -4 -4 12 5.25 1.42 4 -4 -12 4.54 1.12 -4 4 12 6.40 1.20 4 4 -12 5.08 1.08 -3 -4 12 0.71 1.22 3 -4 -12 1.18 0.95 3 4 -12 1.08 0.95 2 -4 -12 1.51 0.99 -2 -4 12 1.81 1.21 2 4 -12 0.87 0.94 1 -4 -12 4.16 1.16 -1 -4 12 4.66 1.28 1 4 -12 3.51 1.09 8 -5 -12 0.48 0.89 8 5 -12 0.15 1.10 -8 5 12 3.58 1.42 7 -5 -12 13.32 1.57 -7 5 12 17.37 1.95 7 5 -12 16.00 1.78 6 -5 -12 0.24 0.80 -6 -5 12 0.11 1.40 6 5 -12 1.27 1.00 -6 5 12 1.58 1.14 5 -5 -12 15.99 1.69 -5 -5 12 17.47 2.00 -5 5 12 17.91 1.84 4 -5 -12 5.46 1.11 -4 -5 12 7.09 1.55 -4 5 12 5.54 1.17 3 -5 -12 1.52 1.01 -3 -5 12 1.18 1.32 3 5 -12 1.47 0.91 2 -5 -12 30.94 2.56 -2 -5 12 34.55 2.79 2 5 -12 27.72 2.44 1 5 -12 40.48 3.11 7 -6 -12 18.14 1.90 -7 6 12 23.41 2.39 7 6 -12 21.85 2.31 6 -6 -12 5.14 1.14 -6 -6 12 5.42 1.51 6 6 -12 5.82 1.26 -6 6 12 6.19 1.23 -5 -6 12 17.11 1.96 5 -6 -12 12.63 1.54 -5 6 12 15.70 1.67 4 -6 -12 12.49 1.48 -4 -6 12 11.21 1.79 -4 6 12 11.20 1.40 3 -6 -12 3.26 1.02 -3 -6 12 2.44 1.38 2 -6 -12 2.19 1.01 -2 -6 12 2.43 1.34 2 6 -12 2.31 0.97 7 -7 -12 1.51 1.03 7 7 -12 3.96 1.16 -7 7 12 4.44 1.26 6 -7 -12 0.29 0.84 -6 -7 12 0.97 1.43 -6 7 12 0.45 1.03 6 7 -12 0.27 0.96 -5 -7 12 3.85 1.44 5 -7 -12 2.42 1.04 -5 7 12 3.83 1.04 4 -7 -12 13.80 1.56 -4 -7 12 14.05 1.94 -4 7 12 12.32 1.47 3 -7 -12 42.17 3.21 -3 -7 12 47.20 3.55 5 -8 -12 -0.54 0.83 -5 -8 12 -1.11 1.30 -5 8 12 0.98 0.95 7 0 -13 0.38 0.89 -7 0 13 -1.66 1.31 -6 0 13 -0.16 1.28 6 0 -13 1.29 0.94 5 0 -13 0.65 0.97 4 0 -13 0.54 0.98 3 0 -13 1.30 0.98 -7 -1 13 -2.90 1.32 7 -1 -13 0.46 0.88 -7 1 13 0.96 1.36 6 -1 -13 13.95 1.50 -6 -1 13 10.19 1.83 -6 1 13 12.13 1.79 6 1 -13 14.00 1.54 5 -1 -13 9.80 1.39 5 1 -13 15.07 1.55 4 -1 -13 12.22 1.49 4 1 -13 14.11 1.58 6 -2 -13 0.50 0.92 -6 -2 13 -3.31 1.31 -6 2 13 1.01 1.21 5 -2 -13 8.26 1.27 5 2 -13 8.29 1.31 4 -2 -13 15.86 1.63 4 2 -13 14.70 1.64 6 -3 -13 3.08 1.01 6 3 -13 4.76 1.24 -6 3 13 4.00 1.31 5 -3 -13 0.61 0.88 -5 3 13 1.87 1.22 4 -3 -13 1.10 0.95 4 3 -13 0.26 0.96 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 28136 _shelx_res_file ; TITL 1 in P2(1)/c CELL 0.71073 8.0971 12.6116 8.7325 90.000 114.975 90.000 ZERR 4.00 0.0006 0.0010 0.0007 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N SE BR UNIT 20 20 4 4 8 TEMP -153.0 SIZE 0.15 0.20 0.20 L.S. 12 BOND $H ACTA CONF EQIV $1 -x, -y, -z+1 HTAB N1 Br1_$1 EQIV $2 x+1, -y+1/2, z+1/2 HTAB C3 Br2_$2 EQIV $3 -x+1, -y, -z+1 HTAB C5 Br1_$3 EQIV $4 x, y, z-1 HTAB C6 Br1_$4 WGHT 0.030200 0.597700 FVAR 0.12716 BR1 5 0.268379 0.032119 0.841656 11.00000 0.01837 0.02401 = 0.01174 0.00250 0.00598 0.00296 BR2 5 -0.144965 0.291629 0.381466 11.00000 0.01919 0.02324 = 0.01808 0.00614 0.00869 0.00366 SE1 4 0.060266 0.162272 0.614936 11.00000 0.01580 0.01724 = 0.01117 -0.00082 0.00690 -0.00047 N1 3 0.126331 0.092809 0.337744 11.00000 0.01857 0.01732 = 0.01148 -0.00112 0.00558 -0.00099 H1 2 0.012043 0.078783 0.298418 11.00000 -1.20000 C2 1 0.205296 0.138896 0.490897 11.00000 0.01595 0.01645 = 0.01122 0.00115 0.00651 0.00065 C3 1 0.387684 0.166672 0.552391 11.00000 0.02018 0.02540 = 0.01571 -0.00514 0.00745 -0.00408 AFIX 43 H3 2 0.446708 0.199700 0.659753 11.00000 -1.20000 AFIX 0 C4 1 0.483668 0.145936 0.456120 11.00000 0.01936 0.02830 = 0.01865 0.00284 0.01019 0.00051 AFIX 43 H4 2 0.608903 0.164322 0.498127 11.00000 -1.20000 AFIX 0 C5 1 0.397065 0.098478 0.298914 11.00000 0.02701 0.02572 = 0.01871 0.00368 0.01551 0.00695 AFIX 43 H5 2 0.461648 0.083909 0.232299 11.00000 -1.20000 AFIX 0 C6 1 0.215659 0.072947 0.241487 11.00000 0.02763 0.02037 = 0.01228 -0.00040 0.00869 0.00382 AFIX 43 H6 2 0.153323 0.041190 0.133499 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0317 for 2426 Fo > 4sig(Fo) and 0.0433 for all 2959 data REM 85 parameters refined using 0 restraints END WGHT 0.0302 0.5977 REM Highest difference peak 1.365, deepest hole -1.056, 1-sigma level 0.166 Q1 1 -0.0255 0.1605 0.6268 11.00000 0.05 1.37 Q2 1 0.3604 0.0333 0.8371 11.00000 0.05 1.28 Q3 1 -0.2361 0.2946 0.3824 11.00000 0.05 1.26 Q4 1 0.1740 0.0299 0.8493 11.00000 0.05 1.25 Q5 1 0.1565 0.1644 0.6174 11.00000 0.05 1.23 Q6 1 -0.0575 0.2930 0.3631 11.00000 0.05 1.09 Q7 1 0.3044 0.1635 0.5337 11.00000 0.05 0.64 Q8 1 0.2197 0.0646 0.7230 11.00000 0.05 0.59 Q9 1 -0.0828 0.2488 0.5007 11.00000 0.05 0.56 Q10 1 0.1196 0.1321 0.5262 11.00000 0.05 0.56 Q11 1 0.2130 0.0272 0.7531 11.00000 0.05 0.54 Q12 1 0.1516 0.1316 0.4073 11.00000 0.05 0.53 Q13 1 -0.0571 0.0720 0.6632 11.00000 0.05 0.52 Q14 1 0.1348 0.1596 0.7234 11.00000 0.05 0.52 Q15 1 -0.3574 0.3985 0.4343 11.00000 0.05 0.51 Q16 1 0.0308 0.0923 0.6036 11.00000 0.05 0.51 Q17 1 0.0207 0.2059 0.7090 11.00000 0.05 0.51 Q18 1 -0.1404 0.3545 0.3778 11.00000 0.05 0.51 Q19 1 0.0754 0.0518 0.8483 11.00000 0.05 0.50 Q20 1 -0.2068 0.2836 0.2941 11.00000 0.05 0.48 ; _shelx_res_checksum 97935 _shelxl_version_number .2013 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Br Br1 0.26838(4) 0.03212(2) 0.84166(3) 0.01817(8) Uani d 1 Br Br2 -0.14496(4) 0.29163(3) 0.38147(4) 0.01989(8) Uani d 1 Se Se1 0.06027(4) 0.16227(2) 0.61494(3) 0.01433(7) Uani d 1 N N1 0.1263(4) 0.0928(2) 0.3377(3) 0.0161(5) Uani d 1 H H1 0.012(6) 0.079(3) 0.298(5) 0.019 Uiso d 1 C C2 0.2053(4) 0.1389(2) 0.4909(4) 0.0143(5) Uani d 1 C C3 0.3877(4) 0.1667(3) 0.5524(4) 0.0205(6) Uani d 1 H H3 0.4467 0.1997 0.6598 0.025 Uiso calc 1 C C4 0.4837(4) 0.1459(3) 0.4561(4) 0.0214(6) Uani d 1 H H4 0.6089 0.1643 0.4981 0.026 Uiso calc 1 C C5 0.3971(5) 0.0985(3) 0.2989(4) 0.0218(6) Uani d 1 H H5 0.4616 0.0839 0.2323 0.026 Uiso calc 1 C C6 0.2157(4) 0.0729(3) 0.2415(4) 0.0200(6) Uani d 1 H H6 0.1533 0.0412 0.1335 0.024 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 Br1 0.01837(14) 0.02401(16) 0.01174(12) 0.00296(10) 0.00598(10) 0.00250(10) Br2 0.01919(14) 0.02324(16) 0.01808(14) 0.00366(11) 0.00869(11) 0.00614(11) Se1 0.01580(13) 0.01724(14) 0.01117(12) -0.00047(10) 0.00690(10) -0.00082(9) N1 0.0186(11) 0.0173(12) 0.0115(10) -0.0010(9) 0.0056(9) -0.0011(9) C2 0.0159(12) 0.0165(13) 0.0112(11) 0.0006(10) 0.0065(10) 0.0012(10) C3 0.0202(14) 0.0254(16) 0.0157(13) -0.0041(11) 0.0075(11) -0.0051(11) C4 0.0194(14) 0.0283(17) 0.0186(14) 0.0005(12) 0.0102(12) 0.0028(12) C5 0.0270(15) 0.0257(16) 0.0187(14) 0.0070(12) 0.0155(12) 0.0037(12) C6 0.0276(14) 0.0204(15) 0.0123(12) 0.0038(12) 0.0087(11) -0.0004(10) 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' Se Se -0.0929 2.2259 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 Se1 Br1 88.76(9) C2 Se1 Br2 89.69(8) Br1 Se1 Br2 178.428(15) C6 N1 C2 123.1(3) C6 N1 H1 119(3) C2 N1 H1 118(3) N1 C2 C3 118.4(3) N1 C2 Se1 118.5(2) C3 C2 Se1 123.1(2) C2 C3 C4 119.6(3) C2 C3 H3 120.2 C4 C3 H3 120.2 C5 C4 C3 120.1(3) C5 C4 H4 119.9 C3 C4 H4 119.9 C6 C5 C4 118.6(3) C6 C5 H5 120.7 C4 C5 H5 120.7 N1 C6 C5 120.2(3) N1 C6 H6 119.9 C5 C6 H6 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Se1 2.5761(4) Br2 Se1 2.5920(4) Se1 C2 1.927(3) N1 C6 1.344(4) N1 C2 1.347(4) N1 H1 0.86(4) C2 C3 1.387(4) C3 C4 1.390(4) C3 H3 0.9500 C4 C5 1.386(5) C4 H4 0.9500 C5 C6 1.375(5) C5 H5 0.9500 C6 H6 0.9500 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 N1 H1 Br1 3_556 0.86(4) 2.50(4) 3.305(3) 156(3) C5 H5 Br1 3_656 0.95 2.92 3.790(3) 152.8 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 C6 N1 C2 C3 -0.3(4) C6 N1 C2 Se1 -179.9(2) N1 C2 C3 C4 -0.4(5) Se1 C2 C3 C4 179.2(2) C2 C3 C4 C5 0.5(5) C3 C4 C5 C6 0.1(5) C2 N1 C6 C5 0.9(5) C4 C5 C6 N1 -0.8(5) _cod_database_fobs_code 2242913