#------------------------------------------------------------------------------ #$Date: 2018-02-14 10:12:20 +0200 (Wed, 14 Feb 2018) $ #$Revision: 206435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242386.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_2242386 loop_ _publ_author_name 'Noland, Wayland E.' 'Herzig, Ryan J.' 'Engwall, Abigail J.' 'Jensen, Renee C.' 'Tritch, Kenneth J.' _publ_section_title ; Crystal structures of methyl 3,5-dibromo-4-cyanobenzoate and methyl 3,5-dibromo-4-isocyanobenzoate ; _journal_coeditor_code LH5870 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 345 _journal_page_last 348 _journal_paper_doi 10.1107/S2056989018002256 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C9 H5 Br2 N O2' _chemical_formula_moiety 'C9 H5 Br2 N O2' _chemical_formula_sum 'C9 H5 Br2 N O2' _chemical_formula_weight 318.96 _chemical_melting_point 410 _chemical_name_common RCN _chemical_name_systematic 'Methyl 3,5-dibromo-4-cyanobenzoate' _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 geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 93.757(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.9273(18) _cell_length_b 17.881(8) _cell_length_c 14.739(7) _cell_measurement_reflns_used 2977 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.59 _cell_measurement_theta_min 2.67 _cell_volume 1032.8(8) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick 2015a) ; _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _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 0.0430 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11889 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.814 _diffrn_reflns_theta_min 1.793 _exptl_absorpt_coefficient_mu 7.820 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 1996) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.051 _exptl_crystal_description Block _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.250 _refine_diff_density_max 0.371 _refine_diff_density_min -0.518 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2426 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0263 _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^)+(0.0274P)^2^+0.0295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.0593 _reflns_number_gt 2013 _reflns_number_total 2426 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lh5870sup1.cif _cod_data_source_block RCN _cod_original_cell_volume 1032.9(8) _cod_database_code 2242386 _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 0.189 _shelx_estimated_absorpt_t_max 0.245 _shelx_hkl_file ; 1 0 0 101.17 3.55 -1 0 0 96.25 3.66 -1 0 0 102.18 3.72 1 0 0 89.54 3.94 -2 0 0 0.78 0.24 -2 0 0 1.26 0.24 2 0 0 1.07 0.36 2 0 0 1.30 0.21 -3 0 0 31.27 1.50 -3 0 0 29.30 1.42 3 0 0 27.82 1.72 4 0 0 66.57 3.44 -4 0 0 66.52 2.97 -4 0 0 69.65 3.10 5 0 0 11.95 1.88 0 -1 0 -0.08 0.01 0 -1 0 -0.12 0.01 0 1 0 -0.10 0.01 -1 -1 0 146.32 5.39 1 -1 0 148.33 5.20 1 -1 0 139.20 5.71 -1 -1 0 139.94 5.34 1 1 0 146.97 5.14 1 1 0 133.35 5.72 -1 1 0 143.70 5.41 -1 1 0 142.99 5.31 -2 -1 0 0.39 0.20 -2 -1 0 0.29 0.20 2 -1 0 0.15 0.27 2 -1 0 0.25 0.18 2 1 0 0.18 0.31 -2 1 0 0.47 0.22 2 1 0 0.14 0.13 -2 1 0 0.41 0.20 -3 -1 0 18.66 1.15 -3 -1 0 20.26 1.08 3 -1 0 19.22 1.00 3 -1 0 20.00 1.33 -3 1 0 21.32 1.14 3 1 0 20.17 1.41 -3 1 0 20.49 1.10 -4 -1 0 3.80 0.77 -4 -1 0 3.14 0.60 4 -1 0 3.53 0.96 4 1 0 3.42 1.01 -4 1 0 2.36 0.60 -4 1 0 1.72 0.67 5 -1 0 0.42 0.98 5 1 0 0.34 1.09 0 -2 0 75.67 2.66 0 2 0 75.54 2.84 0 2 0 61.48 2.73 1 -2 0 30.99 1.21 -1 -2 0 28.65 1.20 1 -2 0 31.10 1.31 1 2 0 28.76 1.34 -1 2 0 29.27 1.17 -1 2 0 26.20 1.22 1 2 0 31.91 1.10 -2 -2 0 78.13 3.19 2 -2 0 80.52 3.45 -2 -2 0 76.17 3.16 2 -2 0 79.44 3.07 2 2 0 84.19 2.97 2 2 0 81.98 3.51 -2 2 0 81.00 3.21 -2 2 0 81.86 3.15 -3 -2 0 17.77 1.11 3 -2 0 17.79 0.96 -3 -2 0 18.76 1.01 3 -2 0 18.79 1.32 -3 2 0 17.85 1.04 -3 2 0 18.89 1.07 3 2 0 18.38 1.32 4 -2 0 1.73 0.90 -4 -2 0 2.54 0.71 -4 -2 0 2.13 0.57 -4 2 0 3.13 0.62 4 2 0 3.69 0.92 5 -2 0 3.85 1.22 5 2 0 2.14 1.13 0 -3 0 0.11 0.07 0 -3 0 0.07 0.07 0 3 0 0.10 0.07 0 3 0 -0.10 0.07 -1 -3 0 7.29 0.41 1 -3 0 6.41 0.41 1 -3 0 6.56 0.41 -1 -3 0 6.50 0.37 -1 3 0 6.44 0.33 -1 3 0 5.93 0.38 1 3 0 6.24 0.46 -2 -3 0 9.77 0.61 -2 -3 0 10.51 0.70 2 -3 0 12.44 0.67 2 3 0 10.83 0.82 -2 3 0 11.99 0.68 2 3 0 11.28 0.49 -2 3 0 11.12 0.61 -3 -3 0 42.79 2.07 -3 -3 0 47.56 2.01 3 -3 0 46.78 1.94 3 -3 0 44.77 2.27 3 3 0 45.67 2.41 -3 3 0 44.67 2.00 -3 3 0 43.65 2.03 4 -3 0 -0.54 0.71 -4 -3 0 1.40 0.51 -4 -3 0 1.52 0.62 -4 3 0 0.65 0.51 4 3 0 -0.33 0.71 5 -3 0 3.21 1.22 5 3 0 0.66 1.06 0 -4 0 139.23 5.34 0 -4 0 140.04 5.22 0 4 0 142.25 5.69 0 4 0 150.56 5.50 1 -4 0 9.47 0.55 -1 -4 0 10.58 0.44 1 -4 0 10.42 0.59 -1 -4 0 9.67 0.53 -1 -4 0 10.02 0.57 -1 4 0 9.79 0.56 -1 4 0 10.35 0.46 1 4 0 9.86 0.63 2 -4 0 42.37 2.03 -2 -4 0 44.37 1.91 2 -4 0 44.51 1.85 -2 -4 0 43.16 1.85 -2 4 0 43.49 1.79 2 4 0 47.26 1.65 -2 4 0 40.78 1.88 2 4 0 45.42 2.13 -3 -4 0 -0.10 0.40 3 -4 0 0.33 0.45 3 -4 0 0.18 0.33 -3 -4 0 0.11 0.31 3 4 0 0.54 0.60 -3 4 0 -0.13 0.31 -3 4 0 -0.65 0.23 -4 -4 0 11.02 1.25 4 -4 0 14.46 1.47 -4 -4 0 12.73 1.06 4 4 0 13.05 1.56 -4 4 0 13.18 1.07 5 -4 0 0.72 1.11 -5 -4 0 0.35 0.97 0 -5 0 -0.12 0.14 0 -5 0 0.04 0.14 0 5 0 0.03 0.14 0 5 0 -0.24 0.14 -1 -5 0 3.14 0.23 1 -5 0 2.74 0.37 -1 -5 0 3.18 0.33 1 5 0 3.12 0.39 -1 5 0 2.21 0.29 -1 5 0 3.43 0.23 1 5 0 2.89 0.31 2 -5 0 9.03 0.68 -2 -5 0 9.59 0.42 -2 -5 0 9.43 0.68 2 -5 0 9.86 0.69 -2 -5 0 8.94 0.60 -2 5 0 9.21 0.54 -2 5 0 8.54 0.62 2 5 0 10.05 0.85 3 -5 0 2.94 0.62 3 -5 0 3.13 0.50 -3 -5 0 2.81 0.61 -3 -5 0 3.29 0.48 -3 5 0 2.59 0.42 3 5 0 2.71 0.69 -3 5 0 2.51 0.50 -4 -5 0 -0.32 0.65 4 -5 0 0.18 0.66 -4 5 0 0.22 0.53 4 5 0 -0.25 0.87 -5 -5 0 0.90 0.97 -5 5 0 0.16 0.69 0 -6 0 0.39 0.18 0 -6 0 0.24 0.15 0 6 0 0.32 0.16 0 6 0 0.11 0.18 -1 -6 0 135.19 5.09 -1 -6 0 134.69 4.84 1 -6 0 126.24 4.99 1 6 0 127.52 5.42 -1 6 0 130.82 5.30 1 6 0 139.07 5.16 -1 6 0 132.91 5.17 -2 -6 0 83.12 3.47 -2 -6 0 86.63 3.45 2 -6 0 80.49 3.64 2 -6 0 88.04 3.41 -2 -6 0 86.47 3.13 -2 6 0 83.66 3.48 2 6 0 87.23 3.80 -2 6 0 87.77 3.30 3 -6 0 26.00 1.56 -3 -6 0 24.46 1.28 3 -6 0 25.14 1.35 -3 -6 0 21.37 1.38 -3 6 0 23.25 1.34 3 6 0 27.62 1.70 4 -6 0 -0.20 0.76 -4 -6 0 0.52 0.71 4 6 0 0.61 0.81 -4 6 0 0.89 0.57 0 -7 0 -0.17 0.17 0 -7 0 0.02 0.18 0 7 0 -0.27 0.14 0 7 0 -0.03 0.19 -1 -7 0 65.82 2.67 -1 -7 0 67.75 2.50 1 -7 0 63.05 2.65 1 -7 0 66.57 2.54 -1 7 0 61.63 2.71 -1 7 0 69.14 2.73 1 7 0 66.11 2.71 1 7 0 62.89 2.85 2 -7 0 4.46 0.57 -2 -7 0 3.07 0.49 2 -7 0 3.00 0.48 2 7 0 3.77 0.63 -2 7 0 3.55 0.36 -2 7 0 4.20 0.53 -3 -7 0 18.72 1.08 3 -7 0 16.93 1.25 3 -7 0 17.59 1.14 -3 -7 0 16.74 1.26 -3 7 0 16.38 1.08 3 7 0 18.79 1.43 -4 -7 0 0.05 0.70 4 -7 0 -0.01 0.78 4 7 0 -1.92 0.68 -4 7 0 -0.01 0.54 0 -8 0 9.78 0.63 0 -8 0 10.44 0.65 0 8 0 9.86 0.63 0 8 0 9.56 0.68 -1 -8 0 106.93 4.18 1 -8 0 101.37 4.11 1 -8 0 106.93 4.04 -1 -8 0 103.98 3.97 1 8 0 109.72 4.26 -1 8 0 107.33 4.31 1 8 0 104.25 4.47 -1 8 0 106.27 4.27 -2 -8 0 155.04 6.31 2 -8 0 156.70 6.62 2 -8 0 156.67 6.18 2 8 0 167.31 6.33 -2 8 0 158.07 6.38 -2 8 0 169.88 6.10 2 8 0 166.06 6.79 3 -8 0 31.52 1.70 -3 -8 0 33.32 1.84 -3 -8 0 31.51 1.64 3 -8 0 34.47 1.89 3 8 0 31.48 2.03 -3 8 0 35.04 1.75 4 -8 0 5.82 1.14 -4 -8 0 8.16 1.17 4 8 0 10.23 1.42 -4 8 0 6.84 0.99 0 -9 0 0.19 0.22 0 -9 0 0.30 0.25 0 9 0 -0.07 0.19 0 9 0 0.18 0.23 -1 -9 0 31.34 1.48 1 -9 0 32.51 1.35 1 -9 0 30.17 1.49 -1 -9 0 30.79 1.35 -1 9 0 31.56 1.41 1 9 0 31.15 1.50 -1 9 0 31.35 1.52 1 9 0 28.11 1.55 2 -9 0 0.37 0.35 2 -9 0 0.38 0.36 -2 -9 0 0.53 0.41 2 9 0 0.56 0.42 -2 9 0 0.33 0.32 2 9 0 0.33 0.35 3 -9 0 16.54 1.21 3 -9 0 15.21 1.27 -3 -9 0 17.11 1.31 -3 9 0 16.56 1.17 3 9 0 15.11 1.36 -4 -9 0 1.19 0.76 4 9 0 0.73 0.87 -4 9 0 0.98 0.64 0 -10 0 248.06 9.87 0 -10 0 259.10 9.68 0 10 0 265.49 10.47 0 10 0 275.96 10.14 -1 -10 0 19.59 1.10 1 -10 0 18.58 1.13 1 -10 0 18.58 0.95 1 10 0 18.86 1.15 -1 10 0 19.75 1.14 -1 10 0 18.77 0.98 1 10 0 19.66 1.13 2 -10 0 9.51 0.93 2 -10 0 9.43 0.81 -2 -10 0 9.86 0.90 2 10 0 9.22 0.79 2 10 0 8.59 0.95 -2 10 0 9.65 0.87 -3 -10 0 7.20 0.96 3 -10 0 8.20 1.02 3 10 0 7.11 0.84 3 10 0 9.69 1.15 -3 10 0 8.37 0.88 4 -10 0 29.49 1.81 -4 -10 0 28.70 2.03 4 10 0 25.97 2.25 -4 10 0 28.71 1.75 0 -11 0 0.35 0.31 0 -11 0 0.11 0.28 0 11 0 -0.08 0.31 0 11 0 0.46 0.30 -1 -11 0 13.60 0.83 1 -11 0 12.41 0.79 -1 -11 0 13.48 0.93 1 -11 0 13.45 0.99 1 11 0 14.60 0.98 1 11 0 12.79 0.94 -1 11 0 13.25 0.92 -1 11 0 13.86 0.80 -2 -11 0 0.12 0.42 2 -11 0 0.44 0.44 2 -11 0 -0.08 0.39 2 11 0 0.15 0.37 2 11 0 0.11 0.44 -2 11 0 0.36 0.41 3 -11 0 8.20 1.08 -3 -11 0 7.31 0.97 3 11 0 7.43 0.86 -3 11 0 7.54 0.99 3 11 0 8.61 1.24 -4 -11 0 0.55 0.84 4 -11 0 -0.13 0.62 -4 11 0 1.26 0.67 4 11 0 0.94 0.92 0 -12 0 9.18 0.75 0 -12 0 8.35 0.75 0 12 0 9.69 0.73 0 12 0 8.35 0.75 -1 -12 0 3.04 0.55 1 -12 0 1.70 0.37 -1 -12 0 3.71 0.49 1 -12 0 1.58 0.49 1 12 0 2.13 0.48 1 12 0 3.75 0.56 -1 12 0 2.51 0.39 -1 12 0 2.45 0.49 2 -12 0 8.12 0.93 -2 -12 0 7.29 0.85 2 12 0 8.60 0.84 2 12 0 8.90 1.02 -2 12 0 8.50 0.87 3 -12 0 8.41 1.14 -3 -12 0 3.75 0.82 -3 12 0 7.91 0.96 3 12 0 7.89 1.17 -4 -12 0 2.08 0.90 4 -12 0 3.14 0.90 4 12 0 3.94 1.23 -4 12 0 2.69 0.81 0 -13 0 -0.11 0.37 0 -13 0 -0.01 0.36 0 13 0 0.29 0.33 0 13 0 0.13 0.33 -1 -13 0 20.90 1.17 1 -13 0 20.10 1.29 -1 -13 0 20.96 1.28 -1 13 0 21.01 1.29 1 13 0 19.69 1.28 1 13 0 21.53 1.31 -1 13 0 20.42 1.11 2 -13 0 2.07 0.67 -2 -13 0 0.76 0.60 -2 13 0 1.59 0.60 2 13 0 1.60 0.60 2 13 0 1.22 0.49 -3 -13 0 11.49 1.25 3 -13 0 12.44 1.24 -3 13 0 15.00 1.25 3 13 0 12.49 1.39 -4 -13 0 1.54 0.98 4 -13 0 -0.04 0.77 4 13 0 0.43 0.92 -4 13 0 -1.08 0.66 0 -14 0 129.59 5.27 0 -14 0 129.57 5.36 0 14 0 138.24 5.57 0 14 0 136.67 5.50 -1 -14 0 43.64 2.01 -1 -14 0 44.48 2.15 1 -14 0 41.84 2.17 1 14 0 43.91 2.21 1 14 0 42.10 2.16 -1 14 0 44.60 2.21 -2 -14 0 -0.36 0.49 2 -14 0 0.57 0.57 2 14 0 0.81 0.62 2 14 0 0.16 0.44 -2 14 0 0.68 0.57 -3 -14 0 7.91 1.14 3 -14 0 7.30 1.05 -3 14 0 9.04 1.21 3 14 0 9.60 1.39 -4 -14 0 23.99 2.07 4 -14 0 24.49 1.95 -4 14 0 25.59 1.95 4 14 0 24.37 2.29 0 -15 0 -0.08 0.41 0 -15 0 0.53 0.46 0 15 0 0.00 0.38 1 -15 0 1.12 0.61 -1 -15 0 0.14 0.49 -1 -15 0 0.86 0.41 1 15 0 0.88 0.51 1 15 0 1.11 0.51 -1 15 0 1.92 0.56 -2 -15 0 0.87 0.67 2 -15 0 0.00 0.61 -2 15 0 0.78 0.54 2 15 0 0.66 0.54 2 15 0 1.51 0.65 3 -15 0 0.60 0.70 -3 -15 0 2.90 0.85 -3 15 0 -0.13 0.62 3 15 0 1.37 0.86 0 -16 0 2.98 0.64 0 -16 0 1.89 0.61 0 16 0 3.97 0.68 1 -16 0 13.57 1.21 -1 -16 0 13.35 1.20 1 16 0 16.20 1.20 1 16 0 15.31 1.16 -1 16 0 13.56 1.14 2 -16 0 38.80 2.33 -2 -16 0 40.67 2.31 2 16 0 46.45 2.27 -2 16 0 38.42 2.30 2 16 0 42.27 2.36 -3 -16 0 13.79 1.44 3 -16 0 12.71 1.56 3 16 0 12.12 1.42 -3 16 0 13.57 1.36 0 -17 0 -0.24 0.53 0 17 0 0.46 0.46 -1 -17 0 40.90 2.28 1 -17 0 44.78 2.36 -1 17 0 46.34 2.32 1 17 0 42.67 2.24 -2 -17 0 1.29 0.75 2 -17 0 0.40 0.71 2 17 0 0.43 0.56 2 17 0 0.91 0.64 -2 17 0 0.07 0.61 -3 -17 0 4.15 1.07 3 -17 0 7.05 1.17 -3 17 0 6.35 1.07 3 17 0 4.70 1.07 0 -18 0 1.01 0.58 0 18 0 1.09 0.62 -1 -18 0 0.88 0.69 1 -18 0 2.12 0.69 -1 18 0 1.06 0.58 1 18 0 -0.33 0.48 2 -18 0 32.48 2.16 -2 -18 0 31.07 2.03 -2 18 0 35.39 2.17 -3 -18 0 0.74 0.96 3 -18 0 0.21 0.91 3 18 0 1.61 0.92 -3 18 0 1.22 0.92 0 -19 0 0.72 0.61 0 19 0 1.00 0.60 1 -19 0 1.10 0.68 -1 -19 0 0.48 0.69 1 19 0 0.63 0.59 -1 19 0 0.39 0.65 -2 -19 0 -1.21 0.76 2 -19 0 0.80 0.87 -2 19 0 -0.05 0.65 0 -20 0 0.15 0.66 0 20 0 0.26 0.54 -1 -20 0 2.07 0.83 1 -20 0 3.23 0.97 1 20 0 3.10 0.71 -1 20 0 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0.76 -1 8 -17 -0.87 0.90 1 8 17 0.25 0.73 1 -9 -17 1.98 0.79 -1 -9 17 0.86 0.76 -1 9 17 2.42 0.76 1 9 -17 1.27 0.97 0 -9 17 5.56 0.96 0 9 -17 3.88 1.13 -1 -9 -17 30.46 2.13 1 -9 17 25.09 1.94 1 9 17 31.91 2.08 1 -10 -17 2.09 0.83 1 10 -17 -0.05 0.93 0 -10 -17 -0.08 0.83 0 -10 17 0.12 0.79 0 10 -17 0.41 0.91 -2 0 18 -0.61 0.60 1 0 -18 0.84 0.62 -1 0 18 -0.11 0.56 0 0 -18 11.35 1.16 -2 -1 18 20.45 1.60 -2 1 18 21.07 1.64 -1 -1 18 3.99 0.75 1 -1 -18 4.50 0.83 1 1 -18 5.19 0.88 -1 1 18 4.74 0.81 0 -1 18 3.08 0.68 0 -1 -18 2.56 0.72 -2 -2 18 0.71 0.62 -2 2 18 1.60 0.79 1 -2 -18 7.84 1.01 -1 2 18 7.00 0.98 1 2 -18 6.79 0.91 0 -2 -18 0.09 0.62 0 -2 18 0.59 0.60 -1 2 -18 0.56 0.68 -2 -3 18 4.76 0.83 1 -3 -18 6.47 0.92 -1 3 18 5.06 0.90 1 3 -18 5.19 0.87 0 -3 -18 17.46 1.47 0 -3 18 20.62 1.45 0 3 18 20.53 1.45 0 3 -18 19.29 1.66 -1 3 -18 0.08 0.70 -1 -4 18 6.01 0.88 1 -4 -18 7.99 1.00 -1 4 18 5.65 0.94 0 -4 -18 2.13 0.72 0 -4 18 2.69 0.78 0 4 -18 0.87 0.85 0 4 18 3.96 0.80 1 -4 18 5.06 0.91 -1 4 -18 8.06 1.20 -1 -5 18 -0.04 0.61 1 -5 -18 -0.35 0.62 -1 5 18 0.14 0.67 1 5 -18 -1.12 0.82 0 -5 18 0.74 0.64 0 5 18 0.75 0.62 0 5 -18 -0.28 0.80 1 -5 18 5.36 0.95 -1 5 -18 6.87 1.23 1 -6 -18 11.91 1.32 -1 -6 18 10.85 1.30 1 6 -18 10.97 1.51 -1 6 18 9.83 1.15 0 -6 18 2.33 0.81 0 6 -18 1.67 0.87 0 6 18 2.81 0.80 1 -6 18 1.86 0.82 -1 6 -18 2.64 0.97 1 -7 -18 12.93 1.37 -1 7 18 13.26 1.39 1 7 -18 12.38 1.75 0 -7 18 34.84 2.19 0 7 18 38.08 2.15 0 7 -18 39.45 2.58 1 -8 -18 5.15 0.99 0 8 -18 5.00 1.16 0 8 18 3.45 0.86 -1 0 19 0.47 0.69 1 0 -19 0.24 0.66 1 -1 -19 0.54 0.73 -1 1 19 0.37 0.62 0 -1 -19 6.34 0.93 0 -1 19 6.04 0.85 1 -2 -19 16.28 1.47 -1 2 19 15.66 1.43 0 -2 -19 23.09 1.65 0 -2 19 18.38 1.50 1 -3 -19 0.59 0.70 0 -3 -19 5.45 0.93 0 -3 19 5.99 0.94 0 -4 19 1.00 0.71 0 4 -19 2.02 0.93 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 70008 _shelx_res_file ; TITL 16081a in P2(1)/c CELL 0.71073 3.9273 17.8815 14.7394 90.000 93.757 90.000 ZERR 4.00 0.0018 0.0081 0.0068 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O BR UNIT 36 20 4 8 8 TEMP -100 SIZE 0.25 0.27 0.32 L.S. 12 ACTA BOND $H CONF FMAP 2 PLAN 5 EQIV $1 x+1, -y+3/2, z+1/2 HTAB C3 Br6_$1 WGHT 0.027400 0.029500 FVAR 0.11376 C1 1 0.637005 0.655902 0.863207 11.00000 0.01829 0.01792 = 0.02261 -0.00097 0.00181 0.00082 C2 1 0.773073 0.673985 0.950785 11.00000 0.01875 0.02365 = 0.01739 0.00386 0.00216 0.00183 BR2 5 0.744076 0.603836 1.045339 11.00000 0.03760 0.02881 = 0.02189 0.00724 -0.00044 -0.00681 C3 1 0.924520 0.743038 0.968069 11.00000 0.02248 0.02203 = 0.01641 -0.00126 -0.00009 0.00235 AFIX 43 H3A 2 1.016901 0.754817 1.027533 11.00000 -1.20000 AFIX 0 C4 1 0.941154 0.795163 0.898154 11.00000 0.01743 0.01984 = 0.02193 -0.00016 0.00207 0.00363 C5 1 0.809967 0.778252 0.810494 11.00000 0.02126 0.01887 = 0.01773 0.00113 0.00112 0.00093 AFIX 43 H5A 2 0.821573 0.813843 0.762944 11.00000 -1.20000 AFIX 0 C6 1 0.662362 0.708892 0.793507 11.00000 0.01641 0.02559 = 0.01584 -0.00292 0.00021 0.00283 BR6 5 0.491489 0.683828 0.674506 11.00000 0.02657 0.02717 = 0.01735 -0.00197 -0.00436 -0.00102 C7 1 0.469486 0.584814 0.845292 11.00000 0.02732 0.02889 = 0.01888 0.00228 0.00085 -0.00058 N1 3 0.333274 0.529664 0.829913 11.00000 0.04857 0.03029 = 0.02816 0.00243 -0.00207 -0.01323 C8 1 1.106608 0.869165 0.920644 11.00000 0.02140 0.02072 = 0.01874 0.00065 0.00137 0.00203 O1 4 1.263235 0.882200 0.991591 11.00000 0.04870 0.02829 = 0.02832 0.00076 -0.01121 -0.00605 O2 4 1.058984 0.917598 0.853082 11.00000 0.04031 0.01949 = 0.02696 0.00251 -0.00361 -0.00743 C9 1 1.207833 0.991504 0.866680 11.00000 0.03874 0.01960 = 0.03875 0.00532 -0.00183 -0.00768 AFIX 137 H9A 2 1.162772 1.021456 0.811517 11.00000 -1.50000 H9B 2 1.454764 0.986818 0.879827 11.00000 -1.50000 H9C 2 1.106312 1.016064 0.917864 11.00000 -1.50000 AFIX 0 HKLF 4 REM 16081a in P2(1)/c REM R1 = 0.0263 for 2013 Fo > 4sig(Fo) and 0.0373 for all 2426 data REM 128 parameters refined using 0 restraints END WGHT 0.0260 0.1151 REM Highest difference peak 0.371, deepest hole -0.518, 1-sigma level 0.099 Q1 1 0.3686 0.6099 1.1398 11.00000 0.05 0.37 Q2 1 1.5051 0.9798 0.8419 11.00000 0.05 0.36 Q3 1 0.5595 0.7322 0.6552 11.00000 0.05 0.34 Q4 1 1.0573 1.0287 0.8461 11.00000 0.05 0.33 Q5 1 0.6816 0.4389 0.8583 11.00000 0.05 0.33 ; _shelx_res_checksum 82408 _shelxl_version_number 2014/6 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 C C1 0.6370(6) 0.65590(14) 0.86321(17) 0.0196(5) Uani d 1 C C2 0.7731(6) 0.67398(14) 0.95078(16) 0.0199(5) Uani d 1 Br Br2 0.74408(8) 0.60384(2) 1.04534(2) 0.02954(9) Uani d 1 C C3 0.9245(6) 0.74304(14) 0.96807(17) 0.0204(5) Uani d 1 H H3A 1.0169 0.7548 1.0275 0.024 Uiso calc 1 C C4 0.9412(6) 0.79516(14) 0.89815(17) 0.0197(5) Uani d 1 C C5 0.8100(6) 0.77825(14) 0.81049(16) 0.0193(5) Uani d 1 H H5A 0.8216 0.8138 0.7629 0.023 Uiso calc 1 C C6 0.6624(6) 0.70889(15) 0.79351(16) 0.0193(5) Uani d 1 Br Br6 0.49149(7) 0.68383(2) 0.67451(2) 0.02395(9) Uani d 1 C C7 0.4695(7) 0.58481(16) 0.84529(18) 0.0251(6) Uani d 1 N N1 0.3333(6) 0.52966(14) 0.82991(16) 0.0359(6) Uani d 1 C C8 1.1066(6) 0.86917(14) 0.92064(17) 0.0203(5) Uani d 1 O O1 1.2632(5) 0.88220(11) 0.99159(14) 0.0357(5) Uani d 1 O O2 1.0590(5) 0.91760(10) 0.85308(13) 0.0292(5) Uani d 1 C C9 1.2078(8) 0.99150(15) 0.8667(2) 0.0326(7) Uani d 1 H H9A 1.1628 1.0215 0.8115 0.049 Uiso calc 1 H H9B 1.4548 0.9868 0.8798 0.049 Uiso calc 1 H H9C 1.1063 1.0161 0.9179 0.049 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 C1 0.0183(13) 0.0179(13) 0.0226(13) 0.0008(11) 0.0018(10) -0.0010(11) C2 0.0187(13) 0.0237(14) 0.0174(12) 0.0018(11) 0.0022(10) 0.0039(10) Br2 0.03760(18) 0.02881(17) 0.02189(15) -0.00681(12) -0.00044(12) 0.00724(11) C3 0.0225(13) 0.0220(14) 0.0164(12) 0.0024(11) -0.0001(10) -0.0013(10) C4 0.0174(13) 0.0198(13) 0.0219(13) 0.0036(10) 0.0021(10) -0.0002(10) C5 0.0213(14) 0.0189(14) 0.0177(13) 0.0009(10) 0.0011(10) 0.0011(10) C6 0.0164(13) 0.0256(14) 0.0158(12) 0.0028(10) 0.0002(10) -0.0029(10) Br6 0.02657(15) 0.02717(16) 0.01735(14) -0.00102(11) -0.00436(10) -0.00197(10) C7 0.0273(15) 0.0289(16) 0.0189(13) -0.0006(12) 0.0009(11) 0.0023(11) N1 0.0486(17) 0.0303(15) 0.0282(13) -0.0132(12) -0.0021(11) 0.0024(11) C8 0.0214(13) 0.0207(14) 0.0187(13) 0.0020(11) 0.0014(10) 0.0007(10) O1 0.0487(13) 0.0283(11) 0.0283(11) -0.0060(10) -0.0112(10) 0.0008(9) O2 0.0403(12) 0.0195(10) 0.0270(10) -0.0074(9) -0.0036(9) 0.0025(8) C9 0.0387(17) 0.0196(15) 0.0388(17) -0.0077(12) -0.0018(13) 0.0053(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C6 118.4(2) C2 C1 C7 120.8(2) C6 C1 C7 120.8(2) C3 C2 C1 120.5(2) C3 C2 Br2 120.19(19) C1 C2 Br2 119.32(19) C2 C3 C4 120.0(2) C2 C3 H3A 120.0 C4 C3 H3A 120.0 C5 C4 C3 120.5(2) C5 C4 C8 121.6(2) C3 C4 C8 117.8(2) C6 C5 C4 119.2(2) C6 C5 H5A 120.4 C4 C5 H5A 120.4 C5 C6 C1 121.4(2) C5 C6 Br6 119.93(19) C1 C6 Br6 118.71(19) N1 C7 C1 178.6(3) O1 C8 O2 124.6(2) O1 C8 C4 123.6(2) O2 C8 C4 111.9(2) C8 O2 C9 117.1(2) O2 C9 H9A 109.5 O2 C9 H9B 109.5 H9A C9 H9B 109.5 O2 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.402(4) C1 C6 1.406(4) C1 C7 1.448(4) C2 C3 1.387(3) C2 Br2 1.884(3) C3 C4 1.394(3) C3 H3A 0.9500 C4 C5 1.393(3) C4 C8 1.502(4) C5 C6 1.385(4) C5 H5A 0.9500 C6 Br6 1.890(2) C7 N1 1.138(3) C8 O1 1.201(3) C8 O2 1.324(3) O2 C9 1.454(3) C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 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 C3 H3A Br6 4_676 0.95 2.97 3.878(3) 159.6 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 C1 C2 C3 0.9(4) C7 C1 C2 C3 -178.1(2) C6 C1 C2 Br2 -179.76(18) C7 C1 C2 Br2 1.2(3) C1 C2 C3 C4 0.2(4) Br2 C2 C3 C4 -179.11(18) C2 C3 C4 C5 -0.7(4) C2 C3 C4 C8 179.8(2) C3 C4 C5 C6 0.0(4) C8 C4 C5 C6 179.5(2) C4 C5 C6 C1 1.2(4) C4 C5 C6 Br6 -178.62(18) C2 C1 C6 C5 -1.6(4) C7 C1 C6 C5 177.4(2) C2 C1 C6 Br6 178.18(18) C7 C1 C6 Br6 -2.8(3) C5 C4 C8 O1 -169.5(3) C3 C4 C8 O1 10.1(4) C5 C4 C8 O2 10.4(3) C3 C4 C8 O2 -170.0(2) O1 C8 O2 C9 0.0(4) C4 C8 O2 C9 -179.9(2) _cod_database_fobs_code 2242386