#------------------------------------------------------------------------------ #$Date: 2018-02-14 10:12:20 +0200 (Wed, 14 Feb 2018) $ #$Revision: 206435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242387.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_2242387 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_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 391 _chemical_name_common RNC _chemical_name_systematic 'Methyl 3,5-dibromo-4-isocyanobenzoate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 90.002(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.9233(9) _cell_length_b 13.554(3) _cell_length_c 18.672(4) _cell_measurement_reflns_used 2953 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.39 _cell_measurement_theta_min 2.18 _cell_volume 992.9(4) _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 0.998 _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 0.0526 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 11400 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.531 _diffrn_reflns_theta_min 1.090 _exptl_absorpt_coefficient_mu 8.134 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 1996) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.134 _exptl_crystal_description Needle _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.849 _refine_diff_density_min -0.653 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2277 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0287 _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^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0689 _reflns_number_gt 2132 _reflns_number_total 2277 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lh5870sup1.cif _cod_data_source_block RNC _cod_database_code 2242387 _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 0.106 _shelx_estimated_absorpt_t_max 0.792 _shelx_hkl_file ; -1 0 0 -0.15 0.10 -1 0 0 0.14 0.18 -1 0 0 0.04 0.13 -1 0 0 0.12 0.17 -2 0 0 122.02 7.33 -2 0 0 123.74 7.90 -2 0 0 117.24 8.79 -2 0 0 116.41 7.52 3 0 0 -0.14 0.54 -3 0 0 0.05 0.32 -3 0 0 -0.15 0.43 -3 0 0 0.10 0.59 -4 0 0 2.01 0.79 4 0 0 1.14 0.80 -4 0 0 2.50 0.99 0 -1 0 -0.04 0.03 0 -1 0 -0.06 0.03 0 1 0 -0.03 0.03 -1 -1 0 1.79 0.26 -1 -1 0 2.42 0.38 -1 -1 0 1.91 0.30 -1 -1 0 1.79 0.24 1 -1 0 2.09 0.29 -1 1 0 1.49 0.28 -1 1 0 2.15 0.20 -1 1 0 2.19 0.29 -2 -1 0 73.83 4.92 -2 -1 0 73.37 4.67 -2 -1 0 71.85 5.39 2 -1 0 73.03 4.86 -2 -1 0 70.39 4.51 -2 1 0 71.59 5.42 -2 1 0 68.71 4.67 -2 1 0 77.83 4.48 -3 -1 0 79.90 5.09 -3 -1 0 78.49 4.86 3 -1 0 79.11 5.26 -3 -1 0 79.95 5.32 -3 -1 0 74.88 5.82 -3 1 0 69.57 5.14 -3 1 0 76.97 5.86 -4 -1 0 24.38 2.27 -4 -1 0 25.33 2.34 4 -1 0 26.07 2.24 -4 1 0 21.70 2.41 -4 1 0 25.30 2.40 4 1 0 25.20 2.27 5 1 0 0.73 1.17 0 -2 0 98.56 6.04 0 -2 0 90.67 5.67 0 2 0 96.73 5.70 0 2 0 87.55 6.76 -1 -2 0 16.81 1.28 1 -2 0 17.17 1.19 -1 -2 0 16.52 1.11 -1 -2 0 17.45 1.26 1 2 0 16.56 1.13 -1 2 0 16.22 1.32 -1 2 0 17.00 1.14 -2 -2 0 70.74 4.50 -2 -2 0 70.36 4.82 2 -2 0 72.14 4.72 -2 -2 0 69.75 4.40 -2 -2 0 69.33 5.23 -2 2 0 70.30 5.29 -2 2 0 72.10 4.55 -3 -2 0 0.72 0.58 3 -2 0 1.12 0.56 -3 -2 0 0.68 0.46 -3 -2 0 0.56 0.40 -3 -2 0 0.96 0.55 -3 2 0 0.15 0.63 -3 2 0 0.15 0.49 -4 -2 0 36.07 3.02 4 -2 0 34.16 2.82 -4 -2 0 35.27 2.74 -4 2 0 37.20 3.03 -4 2 0 36.02 3.14 4 2 0 33.71 2.91 0 -3 0 -0.84 0.10 0 -3 0 -0.96 0.11 0 3 0 -0.93 0.10 1 -3 0 1.00 0.24 -1 -3 0 1.13 0.21 -1 -3 0 1.17 0.29 -1 -3 0 0.61 0.20 -1 3 0 0.68 0.22 1 3 0 0.79 0.22 -1 3 0 1.17 0.23 -2 -3 0 47.25 3.48 2 -3 0 45.92 3.17 2 -3 0 47.23 2.84 -2 -3 0 42.75 3.31 -2 -3 0 46.42 2.97 -2 3 0 45.59 3.56 -2 3 0 48.12 3.08 -3 -3 0 3.26 0.79 -3 -3 0 1.72 0.50 3 -3 0 1.69 0.59 -3 -3 0 1.78 0.57 -3 -3 0 0.76 0.43 -3 3 0 0.86 0.68 -3 3 0 0.31 0.51 4 -3 0 1.01 0.78 -4 -3 0 2.33 0.94 -4 3 0 2.07 0.86 -4 3 0 1.16 1.08 0 -4 0 306.26 19.40 0 -4 0 288.68 18.23 0 4 0 314.51 18.33 0 4 0 299.37 21.76 -1 -4 0 3.67 0.48 -1 -4 0 3.53 0.41 1 -4 0 3.63 0.41 1 4 0 2.97 0.38 -1 4 0 4.24 0.40 -1 4 0 2.96 0.43 2 -4 0 21.89 1.68 -2 -4 0 21.33 1.88 -2 -4 0 21.71 1.76 -2 -4 0 22.22 1.58 2 4 0 24.02 1.60 -2 4 0 23.25 1.66 -2 4 0 22.81 1.90 -3 -4 0 22.15 2.01 3 -4 0 21.22 1.72 -3 -4 0 20.30 1.77 -3 -4 0 19.76 1.58 3 4 0 21.00 1.67 -3 4 0 19.58 1.84 -3 4 0 20.37 1.96 -4 -4 0 19.46 1.65 4 -4 0 16.67 1.82 -4 4 0 21.11 2.15 -4 4 0 15.05 2.20 4 4 0 16.55 1.80 0 -5 0 0.07 0.17 0 -5 0 -0.31 0.12 0 5 0 -0.02 0.11 0 5 0 -0.16 0.15 -1 -5 0 27.68 1.93 -1 -5 0 26.79 1.78 1 -5 0 29.38 1.89 -1 5 0 27.99 1.80 1 5 0 25.93 1.76 -1 5 0 24.34 2.09 -2 -5 0 200.41 14.28 2 -5 0 226.93 14.13 -2 -5 0 214.97 13.30 -2 5 0 224.42 13.42 -2 5 0 221.07 15.90 2 5 0 217.05 13.34 -3 -5 0 2.31 0.60 3 -5 0 2.82 0.66 -3 -5 0 1.72 0.87 -3 5 0 2.27 0.70 3 5 0 2.92 0.63 -3 5 0 2.72 0.78 4 -5 0 30.18 2.46 -4 -5 0 29.86 2.30 -4 5 0 24.98 2.80 -4 5 0 30.61 2.86 0 -6 0 762.75 48.07 0 -6 0 787.50 51.15 0 6 0 823.17 57.42 0 6 0 818.47 48.31 1 -6 0 238.51 15.25 -1 -6 0 227.52 14.35 -1 -6 0 242.02 15.29 -1 6 0 238.22 14.43 1 6 0 243.95 14.40 -1 6 0 226.33 17.12 -2 -6 0 90.61 6.28 2 -6 0 93.42 6.10 -2 -6 0 88.05 5.76 -2 6 0 91.87 6.88 2 6 0 94.31 5.76 -2 6 0 92.20 5.83 -3 -6 0 0.80 0.86 3 -6 0 1.22 0.62 -3 -6 0 0.72 0.54 -3 6 0 1.65 0.73 3 6 0 2.22 0.61 -3 6 0 2.30 0.74 -4 -6 0 0.00 0.64 4 -6 0 0.15 0.85 -4 6 0 0.73 0.87 -4 6 0 -0.01 1.13 0 -7 0 -0.15 0.26 0 -7 0 -0.18 0.18 0 7 0 0.13 0.24 -1 -7 0 50.17 3.26 -1 -7 0 51.65 3.49 1 -7 0 49.53 3.43 -1 7 0 50.30 3.85 -1 7 0 52.66 3.28 1 7 0 51.08 3.24 -2 -7 0 3.50 0.59 2 -7 0 3.44 0.62 -2 -7 0 2.67 0.72 -2 7 0 3.00 0.64 -2 7 0 4.14 0.69 2 7 0 3.60 0.63 3 -7 0 64.53 4.42 -3 -7 0 63.40 4.19 3 7 0 61.49 4.15 -3 7 0 60.93 4.35 -3 7 0 65.82 5.03 4 -7 0 4.52 1.03 -4 -7 0 2.41 0.82 -4 7 0 3.96 1.36 -4 7 0 4.89 1.14 0 -8 0 0.85 0.27 0 -8 0 1.13 0.38 0 8 0 0.66 0.31 1 -8 0 88.07 5.82 -1 -8 0 88.39 5.88 -1 -8 0 85.06 5.51 1 8 0 88.72 5.50 -1 8 0 89.51 5.54 -1 8 0 88.21 6.53 2 -8 0 8.71 0.96 -2 -8 0 7.81 1.17 -2 -8 0 6.92 0.93 -2 8 0 8.44 1.08 2 8 0 7.67 0.88 -2 8 0 9.40 0.97 3 -8 0 12.69 1.42 -3 -8 0 7.33 1.56 -3 -8 0 12.23 1.32 -3 8 0 12.23 1.53 3 8 0 11.06 1.24 -3 8 0 13.16 1.57 4 -8 0 25.58 2.49 -4 -8 0 28.16 2.39 -4 8 0 26.94 2.95 -4 8 0 33.60 2.99 0 -9 0 0.14 0.25 0 -9 0 0.00 0.38 0 9 0 0.09 0.31 -1 -9 0 13.37 1.19 -1 -9 0 15.43 1.34 1 -9 0 13.50 1.24 -1 9 0 15.83 1.35 1 9 0 15.24 1.18 -1 9 0 14.44 1.18 -2 -9 0 7.67 0.98 2 -9 0 7.37 0.95 -2 -9 0 7.78 1.20 2 9 0 5.65 0.91 -2 9 0 6.40 1.02 -2 9 0 5.94 0.92 3 -9 0 2.13 0.85 -3 -9 0 2.05 0.72 -3 -9 0 3.36 1.23 3 9 0 2.82 0.77 -3 9 0 3.89 0.98 -3 9 0 4.42 0.95 4 -9 0 0.90 0.97 -4 -9 0 0.96 0.79 -4 9 0 -0.87 1.08 -4 9 0 0.67 0.98 0 -10 0 118.53 7.14 0 -10 0 111.86 7.61 0 10 0 115.26 7.20 -1 -10 0 -0.15 0.49 1 -10 0 -0.30 0.41 -1 -10 0 -0.30 0.34 -1 10 0 0.31 0.37 1 10 0 -0.13 0.38 -1 10 0 0.45 0.36 -2 -10 0 23.64 1.97 2 -10 0 26.31 2.04 -2 -10 0 23.99 2.26 2 10 0 26.63 1.95 -2 10 0 25.94 2.29 -2 10 0 25.35 2.01 3 -10 0 37.53 2.73 -3 -10 0 24.37 3.10 -3 -10 0 32.64 2.64 -3 10 0 34.49 2.77 3 10 0 34.39 2.54 -3 10 0 35.74 3.10 4 -10 0 3.86 1.11 -4 -10 0 2.37 0.97 -4 10 0 1.99 1.34 -4 10 0 3.39 1.19 0 -11 0 0.14 0.51 0 -11 0 -0.38 0.33 0 11 0 0.63 0.40 -1 -11 0 8.38 0.98 1 -11 0 8.27 1.03 -1 -11 0 9.22 1.15 -1 11 0 7.76 0.92 1 11 0 8.88 0.95 -2 -11 0 58.41 3.97 -2 -11 0 53.86 4.33 2 -11 0 61.65 4.16 -2 11 0 55.17 3.99 2 11 0 57.42 3.89 -2 11 0 65.11 4.69 -3 -11 0 3.12 1.36 3 -11 0 4.57 1.02 -3 -11 0 4.57 0.97 -3 11 0 4.93 1.12 -3 11 0 4.11 1.10 3 11 0 4.81 0.96 0 -12 0 24.14 2.02 0 -12 0 24.23 1.80 0 12 0 25.39 1.85 -1 -12 0 118.26 7.26 -1 -12 0 113.86 7.73 1 -12 0 115.28 7.66 -1 12 0 106.48 7.26 1 12 0 120.37 7.26 -2 -12 0 9.84 1.59 2 -12 0 8.47 1.32 -2 -12 0 9.73 1.28 2 12 0 10.17 1.22 -2 12 0 9.79 1.25 -2 12 0 11.17 1.43 -3 -12 0 4.22 0.98 3 -12 0 4.06 1.02 -3 -12 0 2.75 1.36 -3 12 0 4.33 1.17 -3 12 0 3.01 1.06 3 12 0 2.63 0.88 0 -13 0 -0.05 0.62 0 13 0 -0.03 0.48 -1 -13 0 32.88 2.44 1 -13 0 32.95 2.55 -1 -13 0 31.39 2.63 1 13 0 34.87 2.42 -1 13 0 30.71 2.39 2 -13 0 18.48 1.85 -2 -13 0 16.27 2.08 -2 -13 0 20.02 1.85 2 13 0 19.93 1.73 -2 13 0 17.13 1.75 -3 -13 0 32.96 2.64 -3 -13 0 23.03 3.19 3 -13 0 29.52 2.63 3 13 0 29.79 2.39 -3 13 0 31.03 2.72 0 -14 0 26.00 2.20 0 14 0 24.07 1.97 1 -14 0 9.82 1.44 -1 -14 0 11.49 1.56 -1 -14 0 11.46 1.29 1 14 0 12.59 1.36 -1 14 0 9.79 1.24 2 -14 0 2.31 0.92 -2 -14 0 1.23 1.14 -2 -14 0 0.35 0.71 2 14 0 2.27 0.84 -2 14 0 1.15 0.80 -3 -14 0 12.05 2.28 -3 -14 0 12.87 1.82 3 -14 0 13.78 1.85 -3 14 0 12.88 1.93 3 14 0 13.55 1.72 0 -15 0 -0.73 0.78 0 15 0 0.31 0.58 -1 -15 0 8.28 1.21 -1 -15 0 10.65 1.62 1 -15 0 7.14 1.19 -1 15 0 9.08 1.22 1 15 0 9.62 1.32 -2 -15 0 0.11 1.15 -2 -15 0 -0.57 0.64 2 -15 0 -0.51 0.86 2 15 0 1.75 0.89 -2 15 0 0.80 0.78 0 -16 0 20.56 2.13 0 16 0 19.68 1.84 1 -16 0 7.17 1.27 -1 -16 0 5.00 1.25 1 16 0 4.98 1.04 -1 16 0 5.62 1.01 2 -16 0 4.14 1.20 -2 -16 0 4.81 1.53 2 16 0 5.27 1.13 -2 16 0 5.18 1.17 0 -17 0 0.45 1.01 0 17 0 0.12 0.68 -1 -17 0 11.01 1.69 1 -17 0 8.20 1.52 1 17 0 8.02 1.31 -1 17 0 9.75 1.42 5 0 -1 13.56 2.27 -4 0 1 0.62 0.94 4 0 -1 -0.04 0.73 3 0 -1 90.27 5.96 -3 0 1 80.48 5.80 -3 0 1 94.06 5.51 -3 0 1 85.98 6.62 -2 0 1 -0.06 0.25 -2 0 1 -0.13 0.36 -2 0 1 0.02 0.20 -1 0 1 59.78 3.72 -1 0 1 51.71 3.57 -1 0 1 55.76 4.16 -1 0 1 58.10 3.47 0 0 1 -0.07 0.02 -1 0 -1 104.43 6.73 -1 0 -1 102.15 7.14 -1 0 -1 106.64 7.96 -1 0 -1 123.05 6.66 -2 0 -1 -0.17 0.20 -2 0 -1 -0.54 0.31 -2 0 -1 -0.25 0.30 -2 0 -1 0.12 0.27 3 0 1 65.63 4.55 -3 0 -1 65.26 4.39 -3 0 -1 64.19 4.99 -4 0 -1 0.08 0.69 4 0 1 0.75 0.82 5 -1 -1 17.43 2.58 5 1 -1 20.70 2.55 4 -1 -1 9.29 1.27 -4 -1 1 12.42 1.60 -4 1 1 9.84 1.45 -4 1 1 8.13 1.52 -3 -1 1 13.67 1.11 -3 -1 1 13.68 1.41 3 -1 -1 14.39 1.30 -3 -1 1 12.33 1.33 -3 1 1 13.70 1.07 -3 1 1 12.69 1.38 -3 1 1 12.97 1.49 -2 -1 1 25.77 1.66 -2 -1 1 23.42 1.82 -2 -1 1 24.31 1.97 -2 -1 1 25.42 1.85 2 -1 -1 24.53 1.80 -2 1 1 25.64 1.62 -2 1 1 26.24 1.85 -2 1 1 24.47 2.00 -1 -1 1 26.97 2.04 -1 -1 1 26.48 1.79 -1 -1 1 26.53 1.71 -1 -1 1 26.39 1.88 1 -1 -1 28.32 1.83 -1 1 1 27.22 1.78 -1 1 1 26.05 2.05 -1 1 1 27.36 1.68 0 -1 -1 128.36 9.21 0 -1 1 124.01 8.20 0 -1 -1 143.87 8.21 0 -1 1 121.08 7.71 0 1 1 126.31 7.72 0 1 -1 133.39 9.22 0 1 1 120.47 7.75 0 1 -1 125.89 7.75 -1 -1 -1 25.39 1.65 -1 -1 -1 26.80 1.63 -1 -1 -1 25.28 1.92 1 -1 1 24.95 1.77 -1 -1 -1 22.59 1.81 1 -1 1 26.63 1.59 -1 1 -1 25.61 1.65 -1 1 -1 24.95 1.95 -2 -1 -1 16.29 1.37 2 -1 1 15.85 1.31 -2 -1 -1 17.72 1.28 -2 -1 -1 16.94 1.37 -2 -1 -1 15.37 1.14 -2 1 -1 15.58 1.39 -2 1 -1 15.17 1.29 3 -1 1 6.90 0.69 -3 -1 -1 6.33 0.98 -3 -1 -1 8.26 1.08 -3 -1 -1 8.44 1.03 3 -1 1 6.57 1.07 -3 1 -1 6.29 1.02 -3 1 -1 7.67 1.20 -4 -1 -1 18.33 1.91 4 -1 1 19.60 1.92 4 1 1 16.00 1.87 -4 1 -1 14.16 2.11 -4 1 -1 18.15 1.97 -5 1 -1 9.16 1.83 5 -2 -1 0.32 1.23 -4 -2 1 22.68 2.07 4 -2 -1 22.29 1.98 -4 2 1 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2 -5 -19 10.11 2.02 -2 -5 19 10.71 1.58 -2 5 19 11.13 1.49 2 5 -19 10.77 1.65 2 5 -19 8.71 1.52 1 -5 -19 1.11 1.13 -1 -5 19 1.46 0.82 -1 5 19 3.34 0.87 1 5 -19 2.59 1.13 0 -5 19 8.26 1.32 0 -5 -19 9.61 1.79 0 5 -19 5.85 1.47 0 5 19 7.54 1.29 1 -5 19 5.65 0.95 -1 -5 -19 13.37 2.03 -1 5 -19 3.00 1.36 1 5 19 4.49 1.02 -2 -5 -19 5.94 1.42 2 -5 19 7.62 1.21 2 -5 19 5.44 1.20 -2 5 -19 5.89 1.63 2 5 19 7.17 1.24 -2 -6 19 1.32 0.97 2 -6 -19 2.81 1.35 2 6 -19 1.69 1.03 -2 6 19 1.86 0.84 2 6 -19 0.91 1.03 1 -6 -19 0.25 1.08 -1 -6 19 -0.18 0.69 -1 6 19 -0.04 0.67 1 6 -19 -0.17 1.03 0 -6 19 0.51 0.63 0 -6 -19 1.34 1.11 0 6 19 0.90 0.76 0 6 -19 -0.14 1.08 1 -6 19 0.45 0.62 -1 -6 -19 3.81 1.31 1 6 19 -0.95 0.69 -1 6 -19 0.07 1.15 -2 -6 -19 2.07 1.23 2 6 19 0.69 0.86 -2 6 -19 0.40 1.24 -2 -7 19 4.17 1.18 2 -7 -19 1.93 1.38 2 7 -19 3.57 1.17 -2 7 19 3.01 1.03 -1 -7 19 6.29 1.23 1 -7 -19 6.34 1.48 -1 7 19 10.82 1.42 1 7 -19 6.57 1.49 0 -7 19 3.32 0.89 0 -7 -19 4.59 1.27 0 7 19 3.91 0.98 0 7 -19 4.94 1.40 1 -7 19 2.75 0.79 -1 -7 -19 11.59 2.21 -1 7 -19 2.86 1.37 1 7 19 5.76 1.12 -2 -7 -19 8.14 1.69 2 7 19 5.68 1.17 -2 7 -19 4.69 1.58 -2 -8 19 1.90 1.01 2 -8 -19 1.78 1.45 2 8 -19 3.19 1.24 -1 -8 19 34.25 2.78 1 -8 -19 29.49 3.14 0 -8 -19 13.60 2.05 0 -8 19 10.14 1.50 0 8 19 9.89 1.51 0 8 -19 10.06 1.82 1 -8 19 41.95 3.12 1 8 19 45.93 3.27 -1 8 -19 36.28 4.04 -2 -8 -19 5.23 1.62 -2 8 -19 3.09 1.53 2 8 19 3.48 1.06 -1 -9 19 6.29 1.20 1 -9 -19 5.83 1.47 0 -9 19 14.38 1.71 0 9 -19 11.93 2.24 0 9 19 12.91 1.74 -1 9 -19 4.19 1.47 1 9 19 4.72 1.13 -1 -10 19 2.46 0.99 0 -10 19 44.67 3.37 0 10 19 41.29 3.35 1 10 19 0.77 0.92 -1 10 -19 1.52 1.37 -2 0 20 9.15 1.65 -2 0 20 15.12 1.40 2 0 -20 8.42 1.65 -1 0 20 0.35 0.76 1 0 -20 0.44 0.96 0 0 20 25.60 2.31 0 0 -20 30.33 3.00 -1 0 -20 3.31 1.26 1 0 20 -0.05 0.62 2 0 20 39.69 3.15 2 0 20 41.74 3.09 -2 -1 20 22.55 2.18 2 -1 -20 17.45 2.46 -2 -1 20 21.36 1.80 2 1 -20 14.52 2.37 -2 1 20 25.07 2.17 -2 1 20 20.73 1.83 1 -1 -20 16.33 2.28 -1 -1 20 27.93 2.20 1 1 -20 18.91 2.40 -1 1 20 23.56 2.06 0 -1 20 38.90 2.87 0 -1 -20 40.67 3.61 0 1 20 32.75 2.78 0 1 -20 38.81 3.62 -1 -1 -20 21.31 2.43 1 -1 20 12.97 1.59 1 1 20 11.11 1.58 -1 1 -20 19.71 2.42 -2 -1 -20 6.14 1.64 2 -1 20 9.36 1.42 2 1 20 13.46 1.55 -2 1 -20 6.76 1.76 2 -2 -20 11.27 1.99 -2 -2 20 10.73 1.75 2 2 -20 10.79 1.57 2 2 -20 9.13 1.84 -2 2 20 15.14 1.73 -2 2 20 9.81 1.34 1 -2 -20 2.83 1.17 -1 -2 20 2.81 0.95 -1 2 20 3.75 0.95 1 2 -20 3.55 1.17 0 -2 20 12.12 1.56 0 -2 -20 12.64 2.10 0 2 -20 13.36 2.23 0 2 20 12.64 1.52 -1 -2 -20 13.76 2.06 1 -2 20 9.25 1.35 -1 2 -20 6.03 1.60 1 2 20 10.50 1.43 2 -2 20 4.54 0.90 -2 -2 -20 1.70 1.37 -2 -2 -20 6.74 1.35 2 2 20 6.64 1.14 -2 2 -20 3.21 1.50 -2 -3 20 3.01 1.07 2 -3 -20 3.24 1.31 2 3 -20 3.79 1.14 2 3 -20 5.20 1.09 -2 3 20 5.97 1.16 1 -3 -20 -0.01 1.01 -1 -3 20 0.99 0.82 1 3 -20 2.97 1.11 -1 3 20 2.32 0.80 0 -3 -20 0.63 1.12 0 -3 20 -1.30 0.60 0 3 20 0.19 0.65 0 3 -20 0.71 1.19 1 -3 20 5.03 0.92 -1 -3 -20 5.92 1.41 1 3 20 3.26 0.92 -1 3 -20 3.35 1.34 2 -3 20 9.82 1.34 -2 -3 -20 7.85 1.43 2 3 20 6.36 1.21 -2 3 -20 4.36 1.62 -2 -4 20 9.65 1.51 2 -4 -20 7.32 1.66 2 4 -20 6.26 1.41 2 4 -20 12.73 1.52 1 -4 -20 3.43 1.23 -1 -4 20 4.76 1.04 1 4 -20 3.60 1.23 -1 4 20 5.57 1.01 0 -4 -20 13.54 2.06 0 -4 20 10.79 1.52 0 4 -20 11.30 1.89 0 4 20 11.52 1.54 1 -4 20 2.60 0.80 -1 -4 -20 7.04 1.50 1 4 20 3.93 1.00 -1 4 -20 4.89 1.44 -2 -4 -20 10.56 1.68 2 -4 20 11.37 1.41 2 4 20 12.12 1.67 -2 4 -20 5.74 1.67 2 -5 -20 16.90 2.42 -2 -5 20 16.83 2.05 2 5 -20 18.67 1.87 2 5 -20 13.30 2.12 -1 -5 20 1.17 0.80 1 -5 -20 -0.28 1.12 -1 5 20 0.67 0.78 1 5 -20 1.95 1.14 0 -5 20 54.44 4.18 0 -5 -20 67.57 5.04 0 5 20 58.29 4.18 0 5 -20 58.66 5.15 1 -5 20 1.04 0.67 -1 -5 -20 4.08 1.36 1 5 20 0.87 0.86 -1 5 -20 0.68 1.21 -2 -5 -20 2.82 1.43 -2 -5 -20 9.24 1.55 2 5 20 9.58 1.38 -2 5 -20 6.49 1.76 2 -6 -20 1.93 1.44 -2 -6 20 4.75 1.21 2 6 -20 6.70 1.34 2 6 -20 6.74 1.28 -1 -6 20 3.43 1.01 1 -6 -20 3.57 1.29 -1 6 20 4.31 0.97 1 6 -20 3.89 1.33 0 -6 20 32.98 2.73 0 -6 -20 41.25 3.41 0 6 20 34.31 2.72 0 6 -20 27.84 3.39 -1 -6 -20 15.19 2.31 1 -6 20 11.83 1.42 -1 6 -20 7.18 1.78 1 6 20 8.11 1.38 -2 -6 -20 18.23 2.24 2 6 20 13.68 1.90 -2 6 -20 14.37 2.63 2 -7 -20 2.32 1.46 2 7 -20 2.41 1.12 -1 -7 20 20.46 2.25 1 -7 -20 18.90 2.58 -1 7 20 27.38 2.12 1 7 -20 19.41 2.63 0 -7 20 3.56 0.90 0 -7 -20 1.95 1.19 0 7 20 1.69 0.91 0 7 -20 2.75 1.29 1 -7 20 15.25 1.76 -1 7 -20 15.90 2.63 1 7 20 19.98 2.00 -2 -7 -20 3.15 1.44 -2 7 -20 2.35 1.52 -1 -8 20 2.74 1.01 1 -8 -20 3.62 1.35 0 -8 20 0.30 0.68 0 -8 -20 0.52 1.17 0 8 20 0.44 0.80 0 8 -20 -1.24 1.15 1 -8 20 9.43 1.35 1 8 20 6.61 1.31 -1 8 -20 8.11 1.82 1 -9 -20 0.80 1.24 -1 -9 20 -0.14 0.81 0 -9 20 3.06 1.00 0 9 -20 4.60 1.47 0 9 20 4.46 1.11 1 9 20 -1.11 0.85 -1 9 -20 0.98 1.39 -2 0 21 -0.76 0.79 2 0 -21 -0.65 1.04 1 0 -21 39.64 4.08 -1 0 21 56.48 3.59 0 0 21 1.17 0.74 0 0 -21 0.83 1.20 1 0 21 24.62 2.35 -1 0 -21 35.51 3.29 2 0 21 0.05 0.73 -2 0 -21 -1.31 1.18 2 -1 -21 2.09 1.19 -2 -1 21 1.27 0.92 2 1 -21 1.72 1.13 -2 1 21 2.26 0.98 -1 -1 21 20.38 1.92 1 -1 -21 15.67 2.22 -1 1 21 17.67 1.85 1 1 -21 13.60 2.25 0 -1 21 10.80 1.58 0 -1 -21 14.78 2.29 0 1 21 12.18 1.61 0 1 -21 15.01 2.33 1 -1 21 9.72 1.50 -1 -1 -21 19.26 2.41 1 1 21 11.05 1.60 -1 1 -21 17.23 2.37 2 -1 21 3.05 0.85 -2 -1 -21 0.09 1.22 2 1 21 2.68 0.91 -2 1 -21 0.07 1.28 2 -2 -21 5.60 1.49 -2 -2 21 6.63 1.30 -2 2 21 9.33 1.50 2 2 -21 3.73 1.27 -1 -2 21 3.38 0.98 1 -2 -21 6.61 1.37 -1 2 21 5.32 1.05 1 2 -21 4.83 1.31 0 -2 21 1.26 0.80 0 -2 -21 3.62 1.36 0 2 -21 4.13 1.40 0 2 21 1.28 0.81 1 -2 21 9.74 1.41 -1 -2 -21 13.28 2.22 -1 2 -21 11.08 2.16 1 2 21 9.34 1.57 -2 -2 -21 1.79 1.33 2 -2 21 4.71 0.98 2 2 21 4.44 1.04 -2 2 -21 2.95 1.51 2 -3 -21 1.38 1.27 -2 -3 21 0.81 0.97 -2 3 21 4.03 1.05 2 3 -21 0.81 1.08 1 -3 -21 27.44 2.98 -1 -3 21 29.67 2.62 -1 3 21 33.28 2.54 1 3 -21 28.44 3.05 0 -3 21 5.40 1.06 0 -3 -21 5.50 1.50 0 3 -21 6.13 1.52 0 3 21 5.48 1.06 -1 -3 -21 43.25 3.72 -1 3 -21 33.60 3.68 1 3 21 34.65 2.90 -2 -3 -21 3.43 1.40 2 -3 21 2.03 0.78 -2 3 -21 0.70 1.40 2 3 21 4.28 1.10 -2 -4 21 5.79 1.30 2 -4 -21 3.64 1.43 2 4 -21 5.60 1.34 -1 -4 21 7.26 1.28 1 -4 -21 7.55 1.51 -1 4 21 9.98 1.46 1 4 -21 7.18 1.52 0 -4 -21 0.67 1.19 0 -4 21 0.76 0.73 0 4 -21 0.88 1.17 0 4 21 0.98 0.77 -1 -4 -21 15.77 2.29 1 -4 21 12.40 1.54 1 4 21 9.69 1.71 -1 4 -21 13.37 2.37 2 -4 21 10.02 1.35 -2 -4 -21 4.91 1.50 -2 4 -21 3.24 1.59 2 4 21 10.12 1.71 -2 -5 21 7.89 1.53 2 -5 -21 7.12 1.76 2 5 -21 7.98 1.48 1 -5 -21 0.37 1.17 -1 -5 21 -0.04 0.76 -1 5 21 1.67 0.89 1 5 -21 2.10 1.20 0 -5 -21 18.33 2.48 0 -5 21 19.11 1.88 0 5 -21 18.44 2.55 0 5 21 15.52 1.80 1 -5 21 0.88 0.70 -1 -5 -21 1.37 1.28 1 5 21 0.61 0.85 -1 5 -21 1.76 1.33 -2 -5 -21 4.63 1.48 2 5 21 9.52 1.58 -1 -6 21 26.01 2.43 1 -6 -21 23.23 2.77 1 6 -21 17.82 2.75 -1 6 21 27.52 2.24 0 -6 -21 7.25 1.49 0 -6 21 4.48 0.99 0 6 -21 6.73 1.51 0 6 21 4.38 1.07 -1 -6 -21 23.00 2.67 1 6 21 16.17 2.06 -1 6 -21 14.75 2.72 1 -7 -21 4.03 1.38 -1 -7 21 2.22 1.03 -1 7 21 3.17 0.97 1 7 -21 4.14 1.39 0 -7 -21 0.59 1.24 0 -7 21 1.43 0.79 0 7 21 0.42 0.90 0 7 -21 1.12 1.22 1 -7 21 2.18 0.83 -1 7 -21 3.41 1.54 1 7 21 3.59 1.12 1 -8 -21 0.98 1.24 -1 -8 21 0.48 0.98 0 -8 -21 3.32 1.38 0 -8 21 1.63 0.86 0 8 21 2.11 0.95 0 8 -21 2.45 1.36 1 -8 21 5.08 1.02 1 8 21 6.01 1.33 -1 8 -21 5.74 1.76 -2 0 22 1.71 1.03 2 0 -22 2.22 1.25 -1 0 22 1.01 0.86 1 0 -22 0.67 1.12 0 0 22 2.39 0.89 0 0 -22 1.95 1.32 1 0 22 0.08 0.72 -1 0 -22 2.88 1.36 2 0 22 5.28 1.10 -2 0 -22 4.35 1.57 -2 -1 22 6.11 1.26 2 -1 -22 5.11 1.53 2 1 -22 6.47 1.44 -2 1 22 3.63 1.12 -1 -1 22 0.88 0.86 1 -1 -22 2.44 1.16 -1 1 22 2.67 0.95 1 1 -22 3.39 1.24 0 -1 -22 35.34 3.41 0 -1 22 31.35 2.66 0 1 22 28.66 2.59 0 1 -22 34.34 3.40 1 -1 22 4.44 0.98 -1 -1 -22 4.18 1.45 -1 1 -22 6.12 1.58 1 1 22 4.48 1.01 2 -1 22 9.62 1.41 -2 -1 -22 6.85 1.72 -2 1 -22 5.60 1.78 2 1 22 11.18 1.60 -2 -2 22 3.18 1.16 -2 2 22 5.50 1.18 2 2 -22 2.34 1.24 -1 -2 22 5.11 1.09 1 -2 -22 2.82 1.24 1 2 -22 1.56 1.22 -1 2 22 2.64 0.94 0 -2 -22 58.21 4.75 0 -2 22 52.39 3.80 0 2 22 49.74 3.80 0 2 -22 51.82 4.77 1 -2 22 2.87 0.86 -1 -2 -22 3.92 1.43 1 2 22 2.88 0.96 -1 2 -22 2.40 1.39 -2 -2 -22 5.15 1.54 2 -2 22 2.72 0.89 2 2 22 1.99 0.99 -1 -3 22 3.25 1.02 1 -3 -22 1.63 1.22 1 3 -22 3.05 1.31 -1 3 22 1.46 0.89 0 -3 -22 6.63 1.64 0 -3 22 6.20 1.12 0 3 22 6.43 1.13 0 3 -22 7.02 1.67 -1 -3 -22 4.38 1.40 1 -3 22 1.97 0.80 1 3 22 1.61 0.91 -1 3 -22 4.07 1.44 1 -4 -22 8.49 1.65 -1 -4 22 9.68 1.65 -1 4 22 13.63 1.64 1 4 -22 10.62 2.13 0 -4 22 6.17 1.16 0 -4 -22 13.26 2.25 0 4 22 8.73 1.47 0 4 -22 9.33 1.76 1 -4 22 9.17 1.41 -1 -4 -22 10.60 2.20 1 4 22 7.75 1.34 -1 4 -22 11.48 2.33 -1 -5 22 16.59 1.92 1 -5 -22 13.08 2.30 -1 5 22 17.61 1.82 1 5 -22 12.76 2.36 0 -5 22 6.72 1.20 0 -5 -22 6.79 1.62 0 5 -22 8.10 1.68 0 5 22 6.29 1.14 1 -5 22 5.34 1.11 -1 -5 -22 13.25 2.22 -1 5 -22 9.51 1.90 1 5 22 7.88 1.33 1 -6 -22 2.52 1.38 -1 -6 22 1.60 0.98 1 6 -22 0.34 1.25 -1 6 22 1.13 0.90 0 -6 -22 -0.84 1.24 0 -6 22 0.47 0.76 0 6 22 0.04 0.82 0 6 -22 0.61 1.28 -1 -6 -22 1.71 1.34 1 -6 22 0.68 0.69 1 6 22 0.49 0.93 -1 6 -22 0.80 1.47 0 -7 -22 3.51 1.46 0 -7 22 1.86 0.88 0 7 22 4.01 1.11 0 7 -22 5.77 1.56 1 0 -23 17.30 2.54 -1 0 23 21.88 2.08 0 0 -23 1.16 1.35 0 0 23 -0.09 0.77 1 0 23 32.07 2.68 -1 0 -23 34.11 3.54 1 -1 -23 25.12 2.97 -1 -1 23 30.67 2.59 1 1 -23 24.51 2.99 -1 1 23 30.86 2.56 0 -1 23 9.14 1.50 0 -1 -23 6.96 1.72 0 1 23 10.02 1.51 0 1 -23 11.58 2.35 1 -1 23 19.91 2.09 -1 -1 -23 23.47 2.91 1 1 23 20.18 2.11 -1 1 -23 23.99 2.91 1 -2 -23 0.14 1.19 -1 -2 23 1.14 0.94 -1 2 23 0.07 0.85 1 2 -23 0.30 1.22 0 -2 -23 6.61 1.67 0 -2 23 6.38 1.20 0 2 -23 8.74 1.80 0 2 23 9.99 1.57 -1 -2 -23 2.00 1.33 1 -2 23 0.56 0.77 -1 2 -23 2.11 1.39 1 2 23 -0.80 0.75 1 -3 -23 6.39 1.55 -1 -3 23 5.47 1.19 1 3 -23 5.12 1.52 -1 3 23 5.70 1.14 0 -3 23 6.47 1.18 0 -3 -23 8.75 1.76 0 3 23 6.75 1.16 0 3 -23 7.49 1.70 -1 -3 -23 12.11 2.26 1 -3 23 8.77 1.48 -1 3 -23 8.44 1.84 1 3 23 7.68 1.32 1 -4 -23 2.62 1.37 -1 4 23 1.86 0.92 1 4 -23 5.10 1.47 0 -4 23 6.72 1.22 0 4 23 6.34 1.19 0 4 -23 7.59 1.76 -1 -4 -23 6.27 1.57 1 -4 23 4.80 1.00 0 -5 23 6.50 1.17 0 -5 -23 4.68 1.60 0 5 -23 5.73 1.61 0 5 23 4.07 1.10 0 0 -24 0.60 1.40 0 0 24 -0.21 0.81 0 -1 -24 13.67 2.78 0 1 24 13.64 1.92 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14850 _shelx_res_file ; TITL 16114z in P2(1)/n CELL 0.71073 3.9233 13.5536 18.6723 90.000 90.002 90.000 ZERR 4.00 0.0009 0.0031 0.0042 0.000 0.003 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O BR UNIT 36 20 4 8 8 TEMP -100 SIZE 0.030 0.120 0.500 L.S. 8 ACTA LIST 4 CONF BOND $H FMAP 2 PLAN 5 EQIV $2 0.5+X, 0.5-Y, 0.5+Z MPLA C11 C12 C13 C14 C15 C16 MPLA C11_$2 C12_$2 C13_$2 C14_$2 C15_$2 C16_$2 EQIV $3 1/2 + X, 3/2 - Y, 1/2 + Z RTAB N..C N11 C17 RTAB C..C C17 C19_$3 RTAB N..C N11 C19_$3 RTAB NC.C N11 C17 C19_$3 EQIV $4 1/2 + X, 3/2 - Y, -1/2 + Z RTAB C..O C18 O11 RTAB C.BR C18 BR16_$4 RTAB O.BR O11 BR16_$4 RTAB COBR C18 O11 BR16_$4 TWIN -1 0 0 0 -1 0 0 0 1 WGHT 0.038500 BASF 0.32770 FVAR 0.13345 C11 1 0.531236 0.592957 0.687973 11.00000 0.02145 0.01921 = 0.01532 -0.00012 -0.00021 -0.00497 C12 1 0.665285 0.560543 0.622819 11.00000 0.01687 0.01657 = 0.02455 -0.00218 -0.00016 -0.00212 BR12 5 0.853191 0.433062 0.615970 11.00000 0.02804 0.01584 = 0.03104 -0.00255 0.00115 0.00238 C13 1 0.660552 0.621089 0.563448 11.00000 0.02080 0.02087 = 0.02313 -0.00341 0.00310 -0.00184 AFIX 43 H13A 2 0.750409 0.598255 0.519207 11.00000 -1.20000 AFIX 0 C14 1 0.524562 0.715327 0.568350 11.00000 0.02292 0.01757 = 0.01600 -0.00072 0.00078 -0.00253 C15 1 0.390007 0.750088 0.632838 11.00000 0.01955 0.01845 = 0.01747 -0.00220 -0.00193 -0.00191 AFIX 43 H15A 2 0.297102 0.814673 0.635954 11.00000 -1.20000 AFIX 0 C16 1 0.394368 0.688744 0.692189 11.00000 0.01955 0.02099 = 0.01381 -0.00597 0.00013 -0.00486 BR16 5 0.218588 0.733124 0.780279 11.00000 0.02964 0.02670 = 0.01950 -0.00694 0.00484 -0.00182 N11 3 0.530722 0.532089 0.747416 11.00000 0.03102 0.01976 = 0.02129 -0.00136 0.00110 -0.00289 C17 1 0.528178 0.480030 0.796826 11.00000 0.06523 0.02816 = 0.02717 -0.00248 -0.00350 -0.00782 C18 1 0.525467 0.775952 0.501064 11.00000 0.02721 0.01721 = 0.01868 -0.00214 -0.00149 -0.00306 O11 4 0.671226 0.750120 0.447319 11.00000 0.04827 0.02346 = 0.02450 0.00185 0.00867 0.00222 O12 4 0.346657 0.859022 0.506812 11.00000 0.03911 0.02187 = 0.02010 0.00158 0.00008 0.00551 C19 1 0.313514 0.914989 0.440754 11.00000 0.03875 0.02694 = 0.02601 0.00706 -0.00262 0.00423 AFIX 137 H19A 2 0.179401 0.974713 0.449764 11.00000 -1.50000 H19B 2 0.198430 0.874506 0.404610 11.00000 -1.50000 H19C 2 0.540369 0.933475 0.423362 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 16114z in P2(1)/n REM R1 = 0.0287 for 2132 Fo > 4sig(Fo) and 0.0322 for all 2277 data REM 129 parameters refined using 0 restraints END WGHT 0.0385 0.0000 REM Highest difference peak 0.849, deepest hole -0.653, 1-sigma level 0.109 Q1 1 0.8447 0.4358 0.6618 11.00000 0.05 0.85 Q2 1 0.1976 0.7335 0.8250 11.00000 0.05 0.75 Q3 1 -0.0152 0.7311 0.7805 11.00000 0.05 0.72 Q4 1 0.8480 0.4312 0.5605 11.00000 0.05 0.71 Q5 1 1.0874 0.4267 0.6202 11.00000 0.05 0.70 ; _shelx_res_checksum 26906 _shelxl_version_number 2014/6 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy C C11 0.5312(10) 0.5930(3) 0.6880(2) 0.0187(7) Uani d 1 C C12 0.6653(9) 0.5605(2) 0.6228(2) 0.0193(7) Uani d 1 Br Br12 0.85319(11) 0.43306(2) 0.61597(2) 0.02497(11) Uani d 1 C C13 0.6606(10) 0.6211(2) 0.5634(2) 0.0216(8) Uani d 1 H H13A 0.7504 0.5983 0.5192 0.026 Uiso calc 1 C C14 0.5246(10) 0.7153(2) 0.56835(19) 0.0188(8) Uani d 1 C C15 0.3900(9) 0.7501(2) 0.63284(19) 0.0185(8) Uani d 1 H H15A 0.2971 0.8147 0.6360 0.022 Uiso calc 1 C C16 0.3944(9) 0.6887(3) 0.69219(18) 0.0181(7) Uani d 1 Br Br16 0.21859(11) 0.73312(2) 0.78028(2) 0.02528(11) Uani d 1 N N11 0.5307(9) 0.5321(2) 0.74742(17) 0.0240(7) Uani d 1 C C17 0.5282(15) 0.4800(3) 0.7968(2) 0.0402(11) Uani d 1 C C18 0.5255(11) 0.7760(2) 0.5011(2) 0.0210(8) Uani d 1 O O11 0.6712(9) 0.75012(19) 0.44732(15) 0.0321(7) Uani d 1 O O12 0.3467(8) 0.85902(17) 0.50681(14) 0.0270(6) Uani d 1 C C19 0.3135(13) 0.9150(3) 0.4408(2) 0.0306(9) Uani d 1 H H19A 0.1794 0.9747 0.4498 0.046 Uiso calc 1 H H19B 0.1984 0.8745 0.4046 0.046 Uiso calc 1 H H19C 0.5404 0.9335 0.4234 0.046 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 C11 0.0214(19) 0.0192(16) 0.0153(18) -0.0050(15) -0.0002(15) -0.0001(14) C12 0.0169(19) 0.0166(15) 0.0246(19) -0.0021(13) -0.0002(18) -0.0022(13) Br12 0.0280(2) 0.01584(15) 0.0310(2) 0.00238(13) 0.0011(2) -0.00255(14) C13 0.021(2) 0.0209(16) 0.0231(19) -0.0018(15) 0.0031(16) -0.0034(14) C14 0.023(2) 0.0176(16) 0.0160(18) -0.0025(14) 0.0008(15) -0.0007(14) C15 0.020(2) 0.0185(15) 0.0175(19) -0.0019(13) -0.0019(15) -0.0022(13) C16 0.0196(19) 0.0210(16) 0.0138(16) -0.0049(14) 0.0001(14) -0.0060(13) Br16 0.0296(2) 0.02670(18) 0.01950(19) -0.00182(15) 0.00484(19) -0.00694(13) N11 0.0310(19) 0.0198(15) 0.0213(17) -0.0029(13) 0.0011(14) -0.0014(13) C17 0.065(3) 0.028(2) 0.027(2) -0.008(2) -0.003(2) -0.0025(19) C18 0.027(2) 0.0172(17) 0.0187(19) -0.0031(14) -0.0015(16) -0.0021(14) O11 0.048(2) 0.0235(12) 0.0245(15) 0.0022(14) 0.0087(16) 0.0019(10) O12 0.0391(17) 0.0219(12) 0.0201(13) 0.0055(12) 0.0001(13) 0.0016(10) C19 0.039(3) 0.0269(18) 0.026(2) 0.0042(19) -0.003(2) 0.0071(15) 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 N11 C11 C12 120.8(3) N11 C11 C16 120.3(3) C12 C11 C16 118.9(3) C13 C12 C11 120.5(3) C13 C12 Br12 119.8(3) C11 C12 Br12 119.7(3) C12 C13 C14 120.0(3) C12 C13 H13A 120.0 C14 C13 H13A 120.0 C13 C14 C15 120.9(3) C13 C14 C18 116.6(3) C15 C14 C18 122.5(3) C16 C15 C14 118.8(3) C16 C15 H15A 120.6 C14 C15 H15A 120.6 C15 C16 C11 120.9(3) C15 C16 Br16 120.2(3) C11 C16 Br16 118.9(3) C17 N11 C11 179.1(4) O11 C18 O12 124.2(4) O11 C18 C14 122.6(3) O12 C18 C14 113.2(3) C18 O12 C19 114.8(3) O12 C19 H19A 109.5 O12 C19 H19B 109.5 H19A C19 H19B 109.5 O12 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C11 N11 1.383(5) C11 C12 1.396(5) C11 C16 1.407(5) C12 C13 1.379(5) C12 Br12 1.883(3) C13 C14 1.387(5) C13 H13A 0.9500 C14 C15 1.397(5) C14 C18 1.501(5) C15 C16 1.386(5) C15 H15A 0.9500 C16 Br16 1.882(3) N11 C17 1.162(5) C18 O11 1.207(5) C18 O12 1.331(4) O12 C19 1.454(4) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 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 N11 C11 C12 C13 179.1(3) C16 C11 C12 C13 -0.6(6) N11 C11 C12 Br12 -0.8(5) C16 C11 C12 Br12 179.5(3) C11 C12 C13 C14 0.6(6) Br12 C12 C13 C14 -179.5(3) C12 C13 C14 C15 -0.3(6) C12 C13 C14 C18 -179.3(4) C13 C14 C15 C16 0.0(6) C18 C14 C15 C16 179.0(3) C14 C15 C16 C11 -0.1(6) C14 C15 C16 Br16 179.5(3) N11 C11 C16 C15 -179.3(4) C12 C11 C16 C15 0.4(5) N11 C11 C16 Br16 1.1(5) C12 C11 C16 Br16 -179.2(3) C13 C14 C18 O11 -8.6(6) C15 C14 C18 O11 172.4(4) C13 C14 C18 O12 170.5(3) C15 C14 C18 O12 -8.5(6) O11 C18 O12 C19 4.8(6) C14 C18 O12 C19 -174.2(4) _cod_database_fobs_code 2242387