#------------------------------------------------------------------------------ #$Date: 2023-06-29 17:54:38 +0200 (Thu, 29 Jun 2023) $ #$Revision: 284700 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022800.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_2022800 loop_ _publ_author_name 'Siddiqui, Shaziyaparveen K.' 'Ramana, C. V.' 'Gonnade, Rajesh G.' _publ_section_title ; Crystal structure of 1-(4-bromophenyl)but-3-yn-1-one ; _journal_coeditor_code DX2053 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S205698902300508X _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C10 H7 Br O' _chemical_formula_moiety 'C10 H7 Br O' _chemical_formula_sum 'C10 H7 Br O' _chemical_formula_weight 223.07 _chemical_name_systematic ; 1-(4-Bromophenyl)but-3-yn-1-one ; _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 92.252(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.471(2) _cell_length_b 9.032(4) _cell_length_c 21.652(11) _cell_measurement_reflns_used 1876 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 24.9185 _cell_measurement_theta_min 2.4415 _cell_volume 873.7(7) _computing_cell_refinement ; SAINT-Plus (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT-Plus (Bruker, 2016) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012), Mercury (Macrae et al., 2020) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008), PLATON (Spek, 2020) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014/7 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.923 _diffrn_measurement_device 'Bruker SMART APEX' _diffrn_measurement_method 'Phi and Omega Scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 4994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.165 _diffrn_reflns_theta_min 2.444 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.648 _exptl_absorpt_correction_T_max 0.583 _exptl_absorpt_correction_T_min 0.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker 2016) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.696 _exptl_crystal_description block _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.404 _refine_diff_density_min -0.620 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 1965 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0482 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.1069P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1281 _refine_ls_wR_factor_ref 0.1401 _reflns_number_gt 1397 _reflns_number_total 1965 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dx2053sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2022800 _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 0.293 _shelx_estimated_absorpt_t_max 0.583 _shelx_hkl_file ; 1 0 0 0.26 0.18 2 0 0 97.63 6.55 3 0 0 0.17 0.58 3 0 0 -0.44 0.43 4 0 0 123.00 9.15 5 0 0 0.42 1.05 0 -1 0 -4.18 0.25 0 1 0 -4.03 0.28 -1 -1 0 15.77 1.39 1 -1 0 17.46 1.22 2 -1 0 975.28 65.90 -2 -1 0 1028.74 65.97 3 -1 0 33.04 2.38 3 1 0 31.28 2.65 3 1 0 31.33 2.35 4 -1 0 0.00 0.88 4 1 0 -0.40 0.78 5 -1 0 -0.19 1.09 5 1 0 -0.09 0.98 0 -2 0 4846.81 302.99 0 2 0 4371.62 342.31 -1 -2 0 26.12 1.82 1 -2 0 24.90 1.78 1 2 0 25.04 2.28 2 2 0 80.60 5.73 2 -2 0 81.37 5.30 -2 -2 0 68.96 5.54 3 -2 0 48.65 3.48 3 2 0 47.36 3.80 3 -2 0 51.99 3.93 4 2 0 67.92 5.28 4 -2 0 68.31 5.38 4 -2 0 68.59 4.81 5 2 0 0.35 1.02 5 -2 0 1.25 1.16 0 3 0 1.19 0.35 0 -3 0 0.22 0.29 1 3 0 464.87 31.58 -1 -3 0 432.00 29.24 1 3 0 431.44 33.13 1 -3 0 443.93 29.24 2 3 0 1026.54 71.24 2 -3 0 1050.10 65.86 -2 -3 0 921.38 66.00 3 3 0 38.37 3.08 3 -3 0 38.31 3.23 -3 -3 0 40.84 3.14 3 -3 0 37.38 2.85 4 3 0 7.31 1.18 4 -3 0 4.74 1.30 4 -3 0 6.99 1.11 5 -3 0 0.21 1.28 5 3 0 0.62 1.04 0 -4 0 825.14 54.04 0 4 0 816.58 61.06 1 4 0 142.80 10.20 1 -4 0 145.92 9.56 -1 -4 0 140.48 9.55 1 4 0 142.55 10.86 2 -4 0 4.07 0.77 -2 -4 0 5.70 0.94 2 4 0 5.15 0.67 2 4 0 5.05 1.32 3 4 0 59.43 4.11 3 4 0 43.29 4.80 3 -4 0 53.63 3.83 -3 -4 0 41.84 4.09 3 -4 0 57.91 4.25 4 -4 0 19.76 2.07 4 -4 0 15.24 1.70 5 -4 0 1.69 1.39 0 5 0 0.27 0.58 0 -5 0 0.27 0.53 1 -5 0 93.78 6.31 1 -5 0 88.67 6.71 -1 -5 0 94.05 6.30 1 5 0 94.22 7.17 2 -5 0 216.53 15.47 2 -5 0 205.24 14.31 -2 -5 0 213.58 14.40 2 5 0 223.35 16.45 -3 -5 0 35.09 3.69 3 -5 0 50.27 3.70 3 5 0 40.77 4.24 3 -5 0 45.68 3.32 4 -5 0 21.46 2.18 4 5 0 11.86 2.27 4 -5 0 19.56 1.87 5 5 0 0.79 1.29 5 -5 0 2.54 1.52 0 -6 0 5.86 0.86 0 6 0 5.55 0.95 -1 -6 0 114.37 7.97 1 -6 0 119.69 7.98 1 6 0 117.83 9.03 -2 -6 0 1.40 0.85 2 6 0 1.37 1.16 2 -6 0 0.48 0.75 2 -6 0 1.43 0.87 3 -6 0 64.01 4.86 3 6 0 68.16 5.53 3 -6 0 54.14 4.42 4 -6 0 8.52 1.63 4 -6 0 9.88 1.46 4 6 0 9.43 1.98 5 6 0 0.34 1.27 5 -6 0 1.31 1.52 0 7 0 -0.21 0.86 0 -7 0 0.96 0.78 -1 -7 0 419.05 28.49 1 7 0 442.26 32.22 1 -7 0 427.45 28.50 2 7 0 5.48 1.41 -2 -7 0 4.73 1.16 2 -7 0 4.24 1.09 3 -7 0 9.82 1.44 3 7 0 9.65 2.16 4 7 0 5.14 1.80 4 -7 0 4.23 1.32 4 -7 0 4.03 1.44 0 -8 0 6.07 1.15 0 8 0 7.83 1.36 1 8 0 25.25 2.50 1 -8 0 23.55 2.15 -1 -8 0 23.51 2.14 -2 -8 0 16.14 1.82 2 -8 0 14.74 1.77 2 8 0 14.41 2.05 3 -8 0 17.02 2.00 3 8 0 19.59 2.66 4 8 0 -1.31 1.57 4 -8 0 1.03 1.39 0 -9 0 0.64 1.08 0 9 0 0.60 1.25 1 -9 0 16.55 1.90 1 9 0 17.57 2.10 -1 -9 0 16.70 1.85 -2 -9 0 12.95 1.81 2 -9 0 10.04 1.65 2 9 0 10.51 1.96 3 9 0 14.94 2.36 3 -9 0 7.45 1.71 0 10 0 -0.86 1.29 0 -10 0 0.00 1.20 1 -10 0 16.61 2.01 1 10 0 13.65 2.10 -1 -10 0 16.61 1.95 2 -10 0 2.22 1.43 -2 -10 0 2.59 1.44 2 10 0 2.15 1.82 3 10 0 11.82 2.57 0 -11 0 -0.09 1.45 -1 -11 0 7.13 1.73 1 11 0 10.29 2.00 1 -11 0 9.37 1.88 2 11 0 -0.13 1.78 5 0 -1 7.29 1.33 4 0 -1 -1.05 0.76 3 0 -1 203.10 13.54 2 0 -1 -0.14 0.35 1 0 -1 78.84 5.30 1 0 1 773.92 50.40 1 0 1 759.16 54.56 2 0 1 -0.16 0.27 2 0 1 -0.41 0.35 3 0 1 17.21 1.63 3 0 1 15.37 1.32 4 0 1 -1.73 0.87 5 0 1 28.61 2.79 5 1 -1 5.95 1.17 5 -1 -1 3.23 1.19 4 1 -1 1.11 0.79 4 -1 -1 0.17 0.65 4 -1 -1 1.28 0.87 3 1 -1 119.88 7.52 3 -1 -1 101.96 7.44 -2 -1 1 73.54 4.68 2 -1 -1 61.66 4.52 -1 -1 1 1564.70 112.01 1 -1 -1 1837.68 111.88 0 1 1 0.46 0.29 0 -1 -1 0.31 0.30 0 1 1 0.79 0.36 0 -1 1 -0.15 0.31 1 -1 1 586.88 36.12 1 1 1 559.13 39.10 1 -1 1 543.48 39.11 -1 -1 -1 504.19 36.21 2 1 1 61.74 4.15 2 -1 1 60.05 4.53 2 1 1 57.93 4.49 2 -1 1 62.18 4.12 3 1 1 562.89 39.44 3 1 1 485.41 36.33 3 -1 1 570.17 36.37 3 -1 1 590.39 39.49 4 -1 1 4.05 1.15 4 1 1 5.57 1.11 5 1 1 10.32 1.55 5 -1 1 7.31 1.54 5 2 -1 1.74 1.00 5 -2 -1 2.59 1.17 4 -2 -1 1.90 0.76 4 -2 -1 1.19 0.96 4 2 -1 0.96 0.81 3 -2 -1 34.35 2.74 -3 -2 1 43.90 3.02 2 -2 -1 142.62 8.66 -2 -2 1 110.95 8.89 -1 -2 1 1267.98 84.61 1 -2 -1 1298.62 84.59 1 2 -1 1292.94 95.71 0 -2 -1 843.49 55.94 0 2 -1 831.87 63.21 0 2 1 836.12 63.22 0 2 1 896.88 60.60 0 -2 1 843.74 55.95 1 -2 1 860.47 53.99 1 2 1 740.03 61.19 1 -2 1 793.22 58.43 1 2 1 872.13 58.41 -1 -2 -1 834.22 53.99 2 -2 1 269.97 18.66 2 2 1 259.18 18.60 -2 -2 -1 239.04 17.37 2 -2 1 267.04 17.19 3 2 1 104.66 7.31 3 -2 1 109.58 7.31 3 -2 1 111.14 8.03 3 2 1 106.65 7.94 4 -2 1 0.04 1.06 4 2 1 1.56 0.93 5 2 1 39.90 3.53 5 -2 1 40.71 3.67 5 3 -1 4.12 1.15 5 -3 -1 4.92 1.38 4 -3 -1 10.25 1.25 4 3 -1 12.21 1.38 4 -3 -1 10.53 1.53 3 3 -1 49.59 3.82 -3 -3 1 51.04 3.87 3 -3 -1 47.94 3.53 2 -3 -1 57.91 3.93 -2 -3 1 54.24 4.14 1 -3 -1 448.15 29.60 1 3 -1 446.56 33.50 -1 -3 1 451.50 29.61 0 3 -1 1609.35 123.00 0 -3 -1 1689.30 108.86 0 3 1 1648.51 123.02 0 -3 1 1676.57 108.86 -1 -3 -1 1013.94 66.39 1 -3 1 1037.95 66.40 1 3 1 1065.00 71.80 1 3 1 960.39 75.15 1 -3 1 967.68 71.83 2 -3 1 18.07 1.60 2 3 1 15.27 1.50 -2 -3 -1 17.99 1.60 2 -3 1 17.94 1.45 3 3 1 278.46 20.06 3 -3 1 289.74 20.17 3 -3 1 270.65 18.52 -3 -3 -1 276.57 18.69 4 3 1 16.66 1.91 4 -3 1 20.77 2.18 4 -3 1 20.67 1.85 5 3 1 2.03 1.17 5 -3 1 2.14 1.47 5 -4 -1 1.45 1.31 4 -4 -1 1.87 1.10 4 -4 -1 2.45 1.03 3 4 -1 45.65 3.26 3 -4 -1 44.75 3.07 3 4 -1 37.13 3.97 -3 -4 1 28.82 3.29 2 4 -1 115.35 8.55 -2 -4 1 117.08 8.12 2 -4 -1 114.78 7.99 2 4 -1 129.41 9.36 -1 -4 1 399.41 26.87 1 4 -1 421.62 28.96 1 -4 -1 402.85 26.86 1 4 -1 400.96 30.38 0 -4 1 27.18 2.02 0 -4 -1 27.86 2.01 0 4 1 28.03 2.30 0 4 -1 27.31 2.24 1 -4 1 445.09 28.83 1 -4 1 417.27 31.13 1 4 1 440.78 32.66 1 4 1 449.07 31.08 -1 -4 -1 430.49 28.81 2 -4 1 616.75 44.64 2 -4 1 616.51 41.25 2 4 1 625.98 46.98 -2 -4 -1 614.38 41.33 2 4 1 651.67 44.58 3 4 1 4.95 1.76 3 -4 1 7.60 1.07 3 -4 1 6.85 1.20 3 4 1 7.65 1.03 4 -4 1 0.68 1.19 4 -4 1 0.18 0.90 5 -4 1 3.00 1.56 5 -5 -1 6.75 1.60 5 5 -1 6.35 1.57 4 -5 -1 21.06 2.15 4 5 -1 12.64 2.36 4 -5 -1 21.08 1.96 3 -5 -1 11.91 1.35 -3 -5 1 13.14 1.88 3 -5 -1 8.80 1.39 3 5 -1 14.68 2.07 -2 -5 1 0.19 0.73 2 -5 -1 -0.22 0.68 2 5 -1 0.12 0.98 -1 -5 1 215.96 14.46 1 5 -1 217.15 16.34 1 -5 -1 217.65 14.46 0 5 -1 816.96 60.97 0 -5 -1 816.38 53.97 0 -5 1 821.23 53.97 0 5 1 822.58 60.99 1 -5 1 427.01 28.61 1 -5 1 426.52 30.86 -1 -5 -1 431.24 28.60 1 5 1 446.53 32.40 2 -5 1 9.90 1.18 2 -5 1 11.13 1.21 -2 -5 -1 11.91 1.28 2 5 1 12.05 1.80 3 5 1 38.21 4.18 3 -5 1 44.22 3.57 3 -5 1 43.01 3.21 4 5 1 29.80 3.75 4 -5 1 39.08 3.13 4 -5 1 45.23 3.54 5 5 1 0.20 1.21 5 -5 1 -0.81 1.44 5 6 -1 -0.54 1.27 5 -6 -1 -0.40 1.36 4 -6 -1 2.54 1.18 4 -6 -1 3.39 1.28 4 6 -1 1.79 1.64 3 -6 -1 0.90 0.95 -3 -6 1 2.12 1.35 3 6 -1 0.71 1.40 3 -6 -1 -0.64 0.93 2 -6 -1 156.27 11.17 -2 -6 1 160.84 11.27 2 6 -1 182.49 12.82 1 6 -1 49.62 4.19 -1 -6 1 53.90 3.74 1 -6 -1 51.94 3.71 0 -6 -1 11.34 1.14 0 6 1 11.55 1.30 0 -6 1 12.33 1.21 0 6 -1 12.18 1.32 1 6 1 2.29 0.91 -1 -6 -1 0.78 0.61 1 -6 1 -0.30 0.69 2 6 1 281.32 19.83 2 -6 1 251.81 17.30 -2 -6 -1 257.99 17.37 2 -6 1 249.51 18.65 3 6 1 18.11 2.58 3 -6 1 18.41 1.98 3 -6 1 18.98 1.83 4 -6 1 1.69 1.14 4 6 1 -1.07 1.47 4 -6 1 -0.30 1.24 5 6 1 0.22 1.33 4 -7 -1 20.46 2.31 4 7 -1 18.53 2.66 4 -7 -1 23.03 2.19 3 -7 -1 1.59 1.07 3 7 -1 2.64 1.58 2 7 -1 53.70 4.46 2 -7 -1 49.11 3.83 -2 -7 1 52.29 3.95 -1 -7 1 21.20 1.99 1 -7 -1 23.62 2.02 1 7 -1 21.60 2.19 0 -7 -1 151.26 10.55 0 -7 1 155.61 10.56 0 7 1 158.84 11.94 0 7 -1 159.05 11.92 1 7 1 127.78 9.73 1 -7 1 123.21 8.58 -1 -7 -1 125.31 8.57 -2 -7 -1 13.70 1.59 2 -7 1 13.46 1.58 2 7 1 17.81 2.14 3 7 1 3.07 1.82 3 -7 1 1.49 1.14 4 -7 1 5.69 1.39 4 -7 1 4.96 1.51 4 7 1 2.10 1.72 4 8 -1 0.72 1.68 4 -8 -1 -0.81 1.28 3 -8 -1 0.89 1.21 3 8 -1 0.66 1.69 2 8 -1 108.58 8.49 2 -8 -1 101.14 7.47 -2 -8 1 111.97 7.62 -1 -8 1 9.81 1.25 1 -8 -1 5.01 1.21 1 8 -1 7.74 1.31 0 -8 -1 0.61 0.90 0 8 -1 0.97 1.05 0 -8 1 0.61 0.91 0 8 1 1.99 1.11 1 8 1 4.46 1.25 1 -8 1 3.78 1.11 -1 -8 -1 4.34 1.06 2 8 1 138.00 9.74 2 -8 1 118.72 8.40 -2 -8 -1 109.37 8.43 3 -8 1 1.80 1.24 3 8 1 0.57 1.80 4 -8 1 1.06 1.50 4 8 1 1.51 1.81 3 -9 -1 -0.15 1.32 3 9 -1 -0.42 1.62 -2 -9 1 1.06 1.32 2 -9 -1 1.86 1.25 2 9 -1 2.77 1.43 -1 -9 1 4.25 1.24 1 -9 -1 6.71 1.35 1 9 -1 6.13 1.39 0 9 1 55.81 4.64 0 9 -1 53.06 4.61 0 -9 -1 52.03 4.09 0 -9 1 54.48 4.12 1 9 1 12.07 1.85 -1 -9 -1 11.77 1.56 1 -9 1 12.15 1.66 2 9 1 2.33 1.60 -2 -9 -1 2.70 1.23 2 -9 1 0.16 1.21 3 -9 1 1.83 1.43 3 9 1 3.35 1.97 3 10 -1 0.40 1.86 2 10 -1 21.35 2.51 2 -10 -1 15.40 2.12 -2 -10 1 19.10 2.36 -1 -10 1 6.76 1.49 1 10 -1 8.22 1.64 1 -10 -1 6.80 1.57 0 10 1 2.08 1.47 0 10 -1 2.07 1.29 0 -10 -1 0.16 1.11 0 -10 1 3.02 1.35 -1 -10 -1 5.44 1.49 1 -10 1 6.35 1.52 1 10 1 6.03 1.68 2 10 1 15.57 2.56 2 -10 1 15.26 2.04 3 10 1 1.42 2.04 -2 -11 1 0.22 1.55 2 11 -1 -1.66 1.75 1 11 -1 1.46 1.54 1 -11 -1 0.57 1.50 -1 -11 1 0.75 1.46 0 -11 1 16.92 2.15 0 -11 -1 12.34 2.02 0 11 1 16.13 2.24 1 -11 1 5.29 1.71 -1 -11 -1 4.12 1.56 1 11 1 6.54 1.87 5 0 -2 -0.88 0.85 4 0 -2 144.61 9.76 3 0 -2 0.58 0.52 2 0 -2 118.45 7.98 1 0 -2 -0.35 0.29 1 0 2 -1.56 0.16 1 0 2 -1.86 0.22 2 0 2 29.72 2.37 2 0 2 30.19 2.10 3 0 2 -0.49 0.63 3 0 2 -0.70 0.41 4 0 2 95.15 7.24 5 0 2 -1.30 1.11 5 1 -2 -0.08 0.83 5 -1 -2 -0.03 0.94 4 1 -2 -0.42 0.67 4 -1 -2 -0.75 0.67 3 -1 -2 0.22 0.54 3 1 -2 -0.25 0.61 -2 -1 2 935.19 58.02 2 -1 -2 825.32 57.85 1 -1 -2 635.92 40.69 -1 -1 2 598.31 40.86 0 1 -2 191.17 13.36 0 1 2 171.96 12.80 0 -1 -2 174.96 11.82 0 -1 2 171.49 11.83 0 1 2 172.98 13.38 1 -1 2 199.63 12.42 -1 -1 -2 162.46 12.47 1 -1 2 186.51 13.47 1 1 2 197.49 13.46 2 -1 2 872.18 56.83 2 1 2 847.55 61.55 2 1 2 892.47 56.84 2 -1 2 842.82 61.56 3 -1 2 19.34 1.93 3 1 2 18.05 1.85 3 -1 2 22.73 1.59 3 1 2 17.88 1.51 4 -1 2 17.58 1.95 4 1 2 17.16 1.86 5 -1 2 7.37 1.57 5 1 2 8.10 1.52 5 2 -2 0.13 0.86 5 -2 -2 0.73 1.00 4 -2 -2 98.72 6.19 4 2 -2 80.22 6.64 3 -2 -2 6.31 0.88 -3 -2 2 10.50 1.30 2 -2 -2 4.46 0.61 1 2 -2 528.69 37.78 1 -2 -2 492.71 33.35 -1 -2 2 498.24 33.39 0 2 -2 2161.25 163.28 0 2 2 2099.41 156.48 0 2 2 2205.11 163.31 0 -2 2 2241.59 144.51 0 -2 -2 2277.89 144.51 1 -2 2 7.73 0.69 1 -2 2 7.49 0.75 -1 -2 -2 7.87 0.69 1 2 2 7.34 0.72 1 2 2 5.50 1.02 2 -2 2 148.32 9.61 -2 -2 -2 146.13 9.76 2 -2 2 138.91 10.44 2 2 2 143.07 10.41 3 2 2 11.19 1.31 3 -2 2 13.15 1.47 3 -2 2 13.44 1.16 4 -2 2 78.86 5.91 4 2 2 71.14 5.74 5 -2 2 2.35 1.40 5 2 2 1.42 1.21 5 -3 -2 0.98 1.14 5 3 -2 2.38 0.99 4 3 -2 2.14 0.78 4 -3 -2 2.43 0.91 -3 -3 2 129.01 9.57 3 -3 -2 142.67 9.28 2 -3 -2 479.19 32.04 -2 -3 2 492.29 32.28 1 3 -2 31.32 2.47 1 -3 -2 28.48 2.16 -1 -3 2 30.38 2.18 0 3 -2 516.61 40.16 0 3 2 536.29 38.43 0 3 2 555.97 40.21 0 -3 -2 537.17 35.55 0 -3 2 553.71 35.57 1 3 2 20.20 1.53 1 -3 2 19.32 1.59 1 -3 2 20.31 1.51 -1 -3 -2 21.00 1.49 1 3 2 18.27 1.91 2 -3 2 202.12 13.47 2 -3 2 198.78 14.60 2 3 2 206.41 14.56 3 -3 2 15.83 1.69 3 3 2 14.66 1.53 3 -3 2 16.02 1.45 4 -3 2 4.87 1.34 4 3 2 4.76 1.15 5 3 2 12.13 1.77 5 -3 2 11.45 1.98 5 -4 -2 3.17 1.29 4 -4 -2 35.57 3.18 4 -4 -2 36.05 2.85 3 4 -2 33.06 2.64 3 4 -2 32.45 3.33 -3 -4 2 22.76 2.80 3 -4 -2 36.03 2.54 -2 -4 2 177.68 12.37 2 4 -2 200.52 14.08 2 -4 -2 173.70 12.22 1 -4 -2 1280.72 82.59 -1 -4 2 1229.97 82.59 1 4 -2 1255.09 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43.63 2.97 0 3 3 40.73 3.12 1 3 3 186.26 15.21 1 -3 3 203.27 14.37 1 -3 3 202.91 13.30 1 3 3 196.90 14.33 -1 -3 -3 210.76 13.28 -2 -3 -3 6.23 0.85 2 -3 3 6.03 0.85 2 -3 3 6.66 0.75 2 3 3 6.74 0.77 3 3 3 144.04 10.54 3 -3 3 144.01 9.70 3 -3 3 144.56 10.62 4 3 3 9.11 1.40 4 -3 3 8.29 1.56 5 3 3 2.86 1.35 5 -3 3 3.98 1.66 5 -4 -3 7.42 1.43 4 -4 -3 4.21 1.03 -3 -4 3 100.70 8.34 3 4 -3 129.42 9.32 2 4 -3 178.16 12.46 -2 -4 3 162.91 11.04 2 -4 -3 148.08 10.86 -1 -4 3 62.94 4.35 1 4 -3 62.19 4.85 1 -4 -3 63.23 4.32 0 4 -3 2.67 0.53 0 -4 -3 2.02 0.50 0 -4 3 2.12 0.48 0 4 3 2.77 0.66 0 -4 3 4.44 0.53 1 -4 3 642.86 46.78 1 -4 3 650.99 43.27 -1 -4 -3 643.10 43.25 1 4 3 707.92 46.78 1 4 3 636.61 49.06 2 -4 3 205.89 14.67 2 -4 3 204.71 13.55 -2 -4 -3 205.42 13.62 2 4 3 185.35 15.73 2 4 3 209.70 14.60 3 -4 3 0.96 0.74 3 -4 3 0.10 0.89 3 4 3 -0.98 1.41 3 4 3 1.49 0.75 4 -4 3 7.70 1.58 5 -4 3 4.85 1.80 5 -5 -3 2.47 1.25 4 -5 -3 19.94 2.06 4 5 -3 16.74 2.36 4 -5 -3 22.09 2.06 3 -5 -3 6.10 1.11 3 5 -3 6.78 1.59 -3 -5 3 6.75 1.67 -2 -5 3 34.35 2.66 2 -5 -3 30.06 2.49 2 5 -3 33.03 2.94 1 5 -3 128.63 10.37 -1 -5 3 142.92 9.27 1 -5 -3 140.99 9.24 0 -5 -3 454.12 29.72 0 -5 3 434.99 29.73 0 5 -3 448.98 33.56 0 5 3 461.81 33.64 1 -5 3 7.54 0.88 1 -5 3 6.99 0.81 -1 -5 -3 7.98 0.85 1 5 3 9.28 1.23 2 5 3 153.84 11.65 2 -5 3 141.34 10.68 2 -5 3 145.15 9.91 -2 -5 -3 150.48 9.97 3 -5 3 38.93 2.90 3 -5 3 37.76 3.22 3 5 3 33.60 3.88 4 5 3 4.38 1.78 4 -5 3 8.03 1.61 5 -5 3 -0.29 1.66 5 5 3 -0.07 1.28 4 -6 -3 0.58 1.03 4 6 -3 2.05 1.44 4 -6 -3 1.27 1.17 3 -6 -3 9.23 1.38 -3 -6 3 10.66 1.88 3 6 -3 11.47 1.76 2 6 -3 294.33 21.57 -2 -6 3 291.85 19.18 2 -6 -3 271.89 19.05 -1 -6 3 46.92 3.35 1 6 -3 45.39 3.72 1 -6 -3 45.03 3.32 0 6 -3 182.38 13.49 0 -6 -3 172.10 11.95 0 -6 3 175.71 11.97 0 6 3 183.69 13.57 -1 -6 -3 62.94 4.41 1 -6 3 62.82 4.45 1 6 3 62.65 5.20 2 6 3 88.88 7.10 -2 -6 -3 86.72 5.94 2 -6 3 80.92 6.27 2 -6 3 82.70 5.87 3 6 3 19.38 2.81 3 -6 3 19.16 1.91 3 -6 3 20.52 2.07 4 -6 3 16.13 2.08 4 6 3 11.05 2.34 4 -6 3 15.57 1.85 4 -7 -3 6.84 1.40 4 -7 -3 7.38 1.49 3 7 -3 3.18 1.39 3 -7 -3 2.65 1.13 -3 -7 3 3.30 1.57 2 -7 -3 -0.51 0.88 -2 -7 3 0.86 0.93 2 7 -3 0.72 0.98 1 -7 -3 2.94 0.93 1 7 -3 2.07 0.83 -1 -7 3 3.14 0.90 0 -7 -3 139.64 9.68 0 -7 3 135.87 9.69 0 7 3 148.35 11.02 0 7 -3 147.47 10.93 1 7 3 11.08 1.63 -1 -7 -3 9.84 1.22 1 -7 3 9.23 1.19 2 -7 3 15.38 1.71 2 7 3 17.86 2.32 -2 -7 -3 17.40 1.78 3 -7 3 7.43 1.39 3 7 3 8.86 2.35 4 7 3 11.00 2.37 4 -7 3 11.70 1.69 4 -8 -3 1.67 1.42 3 -8 -3 3.06 1.30 3 8 -3 5.15 1.60 -3 -8 3 6.88 1.72 -2 -8 3 102.18 7.22 2 8 -3 100.72 7.94 2 -8 -3 99.33 7.08 -1 -8 3 1.20 0.95 1 -8 -3 1.32 1.01 1 8 -3 1.31 0.94 0 -8 -3 121.04 8.23 0 8 -3 119.60 9.25 0 -8 3 115.98 8.25 0 8 3 121.17 9.35 1 -8 3 85.38 5.97 1 8 3 87.79 6.90 -1 -8 -3 80.72 5.94 2 -8 3 31.74 2.89 2 8 3 37.83 3.74 3 8 3 -0.18 2.14 3 -8 3 -0.94 1.22 4 8 3 7.82 2.32 4 -8 3 6.10 1.57 3 -9 -3 4.15 1.45 3 9 -3 2.39 1.54 -2 -9 3 2.30 1.25 2 9 -3 1.84 1.32 2 -9 -3 0.57 1.08 1 9 -3 0.92 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-1 -4 3.08 0.84 4 1 -4 4.13 0.90 3 1 -4 70.90 4.87 3 -1 -4 63.45 4.69 2 -1 -4 496.70 33.39 -2 -1 4 515.35 33.61 1 -1 -4 889.03 57.25 -1 -1 4 848.22 57.43 0 -1 4 173.57 10.62 0 1 4 163.57 12.01 0 1 4 133.86 11.51 0 -1 4 153.59 11.57 0 -1 -4 175.75 10.60 1 -1 4 122.97 8.95 1 -1 4 124.78 8.22 1 1 4 121.27 8.93 2 1 4 555.32 38.76 2 -1 4 560.82 35.74 2 -1 4 526.68 38.76 2 1 4 529.15 35.71 3 -1 4 4.72 1.00 3 -1 4 6.85 0.76 3 1 4 5.93 1.01 4 -1 4 105.40 7.99 4 1 4 104.74 7.93 5 -1 4 -1.45 1.28 5 1 4 0.50 1.30 5 -2 -4 0.20 0.85 5 2 -4 0.53 0.75 4 2 -4 47.64 3.62 4 -2 -4 39.77 3.26 3 -2 -4 45.88 3.49 -3 -2 4 52.51 3.94 -2 -2 4 369.39 25.12 2 -2 -4 379.27 24.80 1 2 -4 69.78 5.31 1 -2 -4 67.47 4.72 -1 -2 4 71.75 4.80 0 2 4 2011.67 135.81 0 -2 4 1852.61 125.47 0 -2 4 1881.29 135.85 0 2 4 1913.80 141.82 0 -2 -4 1886.38 125.46 1 2 4 126.93 11.63 1 2 4 152.28 10.90 1 -2 4 154.13 10.93 -1 -2 -4 158.50 10.05 1 -2 4 158.35 10.09 -2 -2 -4 895.53 58.51 2 2 4 906.51 63.33 2 -2 4 857.62 63.35 2 -2 4 895.50 58.48 3 2 4 37.07 3.08 3 -2 4 38.87 2.75 3 -2 4 37.36 3.14 4 2 4 40.40 3.52 4 -2 4 41.91 3.63 5 -2 4 6.27 1.77 5 2 4 8.25 1.62 5 -3 -4 0.88 0.97 5 3 -4 1.09 0.78 4 -3 -4 0.25 0.81 -3 -3 4 17.90 2.18 3 -3 -4 23.79 1.87 2 -3 -4 617.68 43.65 -2 -3 4 675.59 43.94 2 3 -4 696.46 49.51 1 -3 -4 4.45 0.60 1 3 -4 4.68 0.60 -1 -3 4 5.69 0.65 0 3 4 629.77 45.52 0 -3 -4 608.07 40.22 0 3 4 628.11 43.50 0 3 -4 606.87 45.43 0 -3 4 605.58 40.25 0 -3 4 587.54 43.56 1 -3 4 2007.54 138.16 -1 -3 -4 2014.02 127.65 1 3 4 2011.44 138.15 1 -3 4 1994.49 127.68 1 3 4 1678.06 144.45 2 -3 4 276.75 18.19 2 -3 4 269.81 19.72 2 3 4 277.13 19.68 3 3 4 0.61 0.71 3 -3 4 0.92 0.70 3 -3 4 0.44 0.84 4 3 4 65.13 5.19 4 -3 4 66.68 5.35 5 3 4 6.86 1.57 5 -3 4 4.87 1.79 5 -4 -4 0.42 1.03 4 -4 -4 5.51 1.10 -3 -4 4 29.64 3.09 3 4 -4 29.52 3.13 3 -4 -4 34.74 2.55 2 -4 -4 15.57 1.49 2 4 -4 20.80 1.95 -2 -4 4 18.15 1.75 1 -4 -4 616.53 39.77 -1 -4 4 598.22 39.79 1 4 -4 594.40 44.88 0 4 4 1509.99 114.58 0 4 -4 1683.70 119.70 0 -4 -4 1572.08 105.93 0 -4 4 1636.49 105.97 0 4 4 1656.54 119.78 1 -4 4 0.64 0.44 1 4 4 0.75 0.82 1 -4 4 0.11 0.39 1 4 4 0.88 0.47 -1 -4 -4 0.56 0.40 -2 -4 -4 175.46 11.59 2 -4 4 177.85 11.54 2 4 4 177.00 12.42 2 -4 4 175.01 12.49 2 4 4 150.18 13.43 3 -4 4 187.97 12.45 3 -4 4 176.06 13.53 3 4 4 191.72 13.46 4 -4 4 21.49 2.40 5 -4 4 -1.85 1.58 5 -5 -4 2.80 1.19 5 -5 -4 4.45 1.30 4 -5 -4 0.51 1.02 4 5 -4 -0.46 1.22 -3 -5 4 48.99 4.44 3 -5 -4 47.55 3.80 3 5 -4 59.10 4.59 2 5 -4 180.66 13.91 2 -5 -4 182.96 12.31 -2 -5 4 186.65 12.45 1 -5 -4 0.33 0.61 1 5 -4 0.29 0.54 -1 -5 4 0.50 0.63 0 -5 -4 55.07 3.91 0 5 -4 58.05 4.40 0 5 4 58.97 4.55 0 -5 4 52.53 3.94 1 5 4 686.69 50.21 -1 -5 -4 653.62 44.23 1 -5 4 674.83 44.27 1 -5 4 670.56 47.82 2 -5 4 48.87 3.93 2 5 4 56.95 4.77 -2 -5 -4 54.73 3.73 2 -5 4 47.37 3.65 3 -5 4 11.98 1.46 3 -5 4 11.13 1.34 3 5 4 4.39 1.92 4 -5 4 1.03 1.32 4 5 4 0.63 1.58 5 5 4 1.59 1.47 5 -5 4 2.57 1.79 5 -6 -4 4.38 1.49 4 -6 -4 4.68 1.27 4 -6 -4 3.38 1.11 -3 -6 4 -0.98 1.25 3 6 -4 0.12 1.24 3 -6 -4 -0.32 0.90 2 6 -4 66.68 5.24 2 -6 -4 61.44 4.64 -2 -6 4 67.45 4.80 -1 -6 4 276.12 17.99 1 6 -4 261.49 20.20 1 -6 -4 271.38 17.94 0 6 -4 126.68 9.34 0 -6 4 119.45 8.31 0 6 4 126.22 9.46 0 -6 -4 117.05 8.26 -1 -6 -4 2.18 0.70 1 -6 4 2.61 0.79 1 6 4 2.66 1.11 -2 -6 -4 20.08 1.76 2 -6 4 16.42 1.68 2 -6 4 17.76 1.71 2 6 4 20.02 2.53 3 -6 4 99.43 6.85 3 6 4 87.94 8.30 3 -6 4 102.73 7.44 4 6 4 2.22 1.83 4 -6 4 2.49 1.44 4 -7 -4 0.01 1.21 4 -7 -4 -0.52 1.00 -3 -7 4 34.33 3.16 3 -7 -4 27.34 2.61 3 7 -4 30.43 3.09 2 -7 -4 38.33 3.12 2 7 -4 40.77 3.43 -2 -7 4 40.86 3.28 1 7 -4 13.09 1.47 1 -7 -4 15.37 1.51 -1 -7 4 13.39 1.49 0 -7 -4 -0.63 0.77 0 7 -4 0.48 0.83 0 -7 4 1.01 0.83 0 7 4 -0.16 1.02 1 7 4 254.34 18.86 -1 -7 -4 242.53 16.51 1 -7 4 245.29 16.55 2 7 4 22.32 2.80 2 -7 4 21.19 2.00 3 7 4 6.08 2.26 3 -7 4 4.31 1.26 4 7 4 -1.30 1.73 4 -8 -4 0.61 1.32 3 8 -4 1.64 1.24 -3 -8 4 4.14 1.64 3 -8 -4 2.08 1.24 2 8 -4 8.66 1.40 2 -8 -4 8.53 1.40 -2 -8 4 9.25 1.51 1 -8 -4 80.16 5.62 1 8 -4 79.33 6.24 -1 -8 4 76.22 5.64 0 8 4 80.18 6.16 0 8 -4 71.85 5.96 0 -8 -4 76.39 5.37 0 -8 4 73.39 5.39 1 8 4 5.32 1.49 1 -8 4 3.88 1.16 -1 -8 -4 4.63 1.05 2 -8 4 0.65 0.99 2 8 4 2.04 1.74 3 -8 4 23.00 2.32 3 8 4 24.50 3.40 4 8 4 -0.65 1.94 -3 -9 4 23.52 2.84 3 -9 -4 21.90 2.38 2 9 -4 0.24 1.23 -2 -9 4 -0.16 1.20 2 -9 -4 -0.76 1.18 1 -9 -4 0.37 1.14 1 9 -4 0.22 1.05 -1 -9 4 -0.85 1.05 0 9 4 -0.59 1.37 0 -9 4 -0.70 1.08 0 -9 -4 -0.21 1.04 -1 -9 -4 69.88 5.25 1 9 4 74.73 6.18 1 -9 4 72.22 5.31 2 -9 4 0.55 1.23 2 9 4 1.21 1.87 3 -9 4 1.33 1.43 3 9 4 2.66 2.30 -2 -10 4 0.85 1.37 2 10 -4 0.41 1.36 2 -10 -4 -0.44 1.36 -1 -10 4 24.71 2.43 1 10 -4 22.38 2.51 1 -10 -4 21.09 2.36 0 10 4 5.74 1.75 0 -10 -4 9.61 1.57 0 -10 4 7.60 1.55 1 10 4 5.87 1.87 -1 -10 -4 2.42 1.44 1 -10 4 4.31 1.49 2 -10 4 2.10 1.50 2 10 4 4.65 2.13 -2 -11 4 6.17 1.78 1 11 -4 0.52 1.57 1 -11 -4 2.20 1.52 -1 -11 4 0.52 1.48 0 11 4 4.38 1.97 0 -11 4 4.74 1.63 0 -11 -4 4.96 1.59 1 11 4 8.98 2.30 -1 -11 -4 9.51 1.96 1 -11 4 8.78 1.69 4 0 -5 -0.60 0.78 3 0 -5 280.70 18.77 2 0 -5 0.51 0.64 -1 0 5 3225.35 229.75 -1 0 5 3764.55 248.56 0 0 5 -0.08 0.37 0 0 5 0.21 0.29 1 0 5 4064.37 277.45 1 0 5 4368.83 299.97 2 0 5 -0.49 0.46 2 0 5 -0.05 0.24 3 0 5 14.62 1.52 4 0 5 -0.51 1.00 5 0 5 28.19 2.89 4 1 -5 -0.65 0.91 4 -1 -5 0.92 0.80 3 1 -5 1.40 0.93 3 -1 -5 1.30 0.73 2 -1 -5 11.60 1.12 -2 -1 5 12.90 1.47 -1 -1 5 747.94 55.13 1 -1 -5 798.40 51.00 -1 1 5 768.57 55.14 -1 -1 5 781.63 51.20 0 -1 -5 4.12 0.38 0 -1 5 3.29 0.59 0 1 5 2.35 0.49 0 -1 5 4.13 0.42 0 1 5 2.88 0.46 1 -1 5 1.77 0.40 1 1 5 1.72 0.38 1 -1 5 2.22 0.32 2 1 5 19.52 1.68 2 -1 5 18.05 1.71 2 -1 5 18.98 1.39 3 -1 5 388.13 27.40 3 1 5 374.40 27.37 4 1 5 3.19 1.13 4 -1 5 2.49 1.18 5 -1 5 -1.71 1.30 5 1 5 -0.93 1.27 5 2 -5 1.00 0.73 4 -2 -5 2.33 1.00 4 2 -5 5.16 1.43 -3 -2 5 261.52 17.13 3 -2 -5 243.43 16.77 -2 -2 5 55.31 4.02 2 -2 -5 49.11 3.59 -1 -2 5 12.92 1.18 1 -2 -5 11.30 1.02 -1 -2 5 11.52 1.02 1 2 -5 11.46 1.03 0 -2 -5 64.85 4.32 0 2 5 64.82 4.97 0 2 5 64.59 4.72 0 -2 5 63.89 4.81 0 -2 5 63.88 4.36 1 2 5 508.01 42.05 1 2 5 576.19 40.05 1 -2 5 576.03 37.01 -1 -2 -5 569.64 36.97 1 -2 5 574.90 40.07 2 -2 5 127.41 9.16 2 2 5 130.29 9.13 -2 -2 -5 118.70 8.34 2 -2 5 127.33 8.38 3 -2 5 -0.27 0.75 3 -2 5 0.54 0.58 3 2 5 -0.07 0.68 4 2 5 42.32 3.53 4 -2 5 40.00 3.63 5 -2 5 16.03 2.29 5 2 5 15.82 2.10 5 -3 -5 8.05 1.25 5 3 -5 5.54 0.99 4 3 -5 18.21 2.49 4 -3 -5 12.14 1.44 -3 -3 5 2.34 1.19 3 -3 -5 2.48 0.82 2 -3 -5 232.60 16.89 2 3 -5 267.34 19.20 -2 -3 5 266.53 17.22 -1 -3 5 847.17 61.55 -1 -3 5 874.68 56.99 1 3 -5 861.06 64.28 1 -3 -5 877.45 56.94 0 -3 5 329.16 21.47 0 3 5 350.33 23.19 0 3 5 331.13 24.30 0 -3 5 283.81 23.25 0 -3 -5 328.10 21.43 1 3 5 22.97 2.26 1 3 5 23.67 1.86 1 -3 5 23.01 1.72 1 -3 5 22.27 1.85 -1 -3 -5 23.93 1.66 2 -3 5 197.46 14.45 2 3 5 203.85 14.42 2 -3 5 199.59 13.31 3 -3 5 364.57 24.28 3 3 5 375.85 26.34 3 -3 5 359.73 26.39 4 3 5 -0.85 0.95 4 -3 5 0.06 1.18 5 3 5 -1.34 1.28 5 -3 5 -0.46 1.58 5 -4 -5 -0.64 0.90 5 -4 -5 -0.30 1.10 4 -4 -5 10.81 1.30 4 4 -5 4.83 1.36 -4 -4 5 9.11 1.76 3 4 -5 41.49 3.76 -3 -4 5 40.74 3.66 3 -4 -5 40.97 3.12 2 4 -5 107.74 8.17 -2 -4 5 112.85 7.45 2 -4 -5 99.71 7.20 -1 -4 5 3.14 0.66 1 4 -5 2.38 0.50 1 -4 -5 2.28 0.59 0 -4 5 165.59 10.65 0 4 5 168.58 12.10 0 4 -5 153.57 11.94 0 -4 -5 161.75 10.61 0 4 5 149.99 11.40 1 -4 5 323.36 21.46 1 -4 5 323.42 23.17 1 4 5 311.57 24.47 1 4 5 340.65 23.26 -1 -4 -5 321.12 21.42 2 -4 5 72.09 4.88 2 4 5 69.55 5.21 2 4 5 61.20 5.97 2 -4 5 73.03 5.30 -2 -4 -5 73.48 4.93 3 -4 5 0.19 0.89 3 4 5 1.35 1.56 3 -4 5 0.12 0.81 3 4 5 0.56 0.76 4 -4 5 22.94 2.55 4 4 5 25.93 2.56 5 -4 5 4.23 1.87 5 -5 -5 0.44 1.02 5 -5 -5 0.06 1.10 4 -5 -5 6.28 1.24 -3 -5 5 5.01 1.68 3 5 -5 5.55 1.29 3 -5 -5 3.15 0.98 -2 -5 5 200.34 12.98 2 5 -5 185.95 14.44 2 -5 -5 188.10 12.80 1 5 -5 305.74 23.86 -1 5 5 332.21 24.00 1 -5 -5 315.26 21.19 -1 -5 5 325.97 21.24 0 -5 5 130.42 8.66 0 5 5 135.36 9.84 0 5 -5 127.79 9.68 0 5 5 119.00 9.19 0 -5 -5 131.33 8.61 -1 -5 -5 11.79 1.05 1 -5 5 10.68 1.06 1 5 5 9.11 1.09 1 -5 5 9.81 1.02 1 5 5 12.85 1.61 2 -5 5 73.56 5.72 2 -5 5 78.33 5.31 -2 -5 -5 81.66 5.38 2 5 5 70.44 6.44 3 5 5 182.31 17.19 3 -5 5 238.65 14.81 3 -5 5 230.56 16.06 4 5 5 2.23 1.73 4 -5 5 3.67 1.44 5 -5 5 -0.31 1.77 5 -6 -5 -1.60 1.16 4 -6 -5 7.57 1.45 3 6 -5 0.36 1.04 3 -6 -5 0.67 0.89 -3 -6 5 1.40 1.52 -2 -6 5 75.72 5.32 2 6 -5 77.00 5.78 2 -6 -5 66.56 5.15 -1 6 5 6.26 1.10 -1 -6 5 7.38 0.99 1 -6 -5 6.84 1.02 1 6 -5 6.09 0.91 0 6 -5 244.14 19.34 0 -6 5 259.60 17.21 0 6 5 273.73 19.53 0 -6 -5 256.59 17.17 1 6 5 10.45 1.55 -1 -6 -5 11.35 1.10 1 -6 5 10.32 1.22 2 -6 5 69.42 5.23 2 6 5 69.32 6.14 2 -6 5 69.25 4.92 3 -6 5 21.24 2.03 3 6 5 21.06 3.02 3 -6 5 23.14 2.30 4 6 5 9.99 2.40 4 -6 5 13.22 1.95 4 -7 -5 3.33 1.10 4 -7 -5 3.90 1.35 3 -7 -5 31.65 2.78 -3 -7 5 33.86 3.32 2 7 -5 5.19 1.04 -2 -7 5 6.32 1.26 2 -7 -5 5.43 1.14 1 7 -5 24.86 2.25 -1 -7 5 24.51 2.23 1 -7 -5 24.24 2.14 0 7 5 448.06 32.07 0 -7 5 413.14 28.29 0 -7 -5 418.55 28.26 1 -7 5 3.05 1.01 -1 -7 -5 3.55 0.89 1 7 5 3.71 1.26 2 -7 5 86.08 6.30 2 7 5 95.96 7.68 3 -7 5 19.73 2.01 3 7 5 18.48 3.09 4 7 5 2.92 1.98 4 -8 -5 4.01 1.47 -3 -8 5 -0.11 1.43 3 -8 -5 0.29 1.18 -2 -8 5 15.91 1.85 2 8 -5 14.79 1.72 2 -8 -5 14.22 1.63 -1 -8 5 -0.38 0.98 1 -8 -5 -0.60 0.96 1 8 -5 -0.59 0.87 0 -8 5 141.16 10.06 0 -8 -5 146.92 10.04 0 8 5 154.02 11.51 1 -8 5 24.96 2.31 1 8 5 26.35 2.80 -1 -8 -5 24.14 2.21 2 -8 5 26.44 2.47 2 8 5 28.08 3.30 3 -8 5 -0.55 1.23 3 8 5 -0.11 2.08 3 -9 -5 6.86 1.57 -3 -9 5 9.39 2.07 2 -9 -5 11.97 1.76 -2 -9 5 14.27 1.92 2 9 -5 14.27 1.73 -1 -9 5 4.19 1.31 1 9 -5 4.37 1.24 1 -9 -5 3.50 1.25 0 -9 -5 17.38 1.92 0 9 5 20.65 2.44 0 -9 5 18.34 1.99 -1 -9 -5 2.53 1.21 1 9 5 2.54 1.63 1 -9 5 2.08 1.26 2 9 5 1.09 1.93 2 -9 5 2.10 1.19 3 -9 5 1.08 1.37 3 9 5 0.42 2.28 2 -10 -5 8.13 1.75 -2 -10 5 11.66 1.90 1 10 -5 1.51 1.31 -1 -10 5 1.49 1.35 1 -10 -5 1.35 1.36 0 -10 -5 18.54 2.06 0 10 5 21.68 2.66 0 -10 5 13.82 1.89 1 10 5 1.93 1.77 -1 -10 -5 0.81 1.23 1 -10 5 0.93 1.35 2 10 5 21.37 3.26 2 -10 5 21.70 2.43 1 -11 -5 1.65 1.54 -1 -11 5 1.75 1.57 0 -11 -5 4.84 1.56 0 11 5 4.88 2.11 0 -11 5 3.29 1.58 1 11 5 6.19 2.22 4 0 -6 39.36 3.17 3 0 -6 0.33 0.80 2 0 -6 3749.39 246.50 -1 0 6 0.70 0.48 -1 0 6 -0.24 0.25 0 0 6 350.73 22.93 0 0 6 341.11 24.83 1 0 6 -0.46 0.19 1 0 6 -0.14 0.33 2 0 6 1424.31 91.67 2 0 6 1365.27 99.31 3 0 6 0.63 0.74 4 0 6 28.77 2.74 5 0 6 -0.66 1.34 4 1 -6 34.39 2.86 4 -1 -6 30.73 2.67 3 1 -6 -0.70 0.95 3 -1 -6 0.09 0.74 2 -1 -6 208.66 13.17 -2 -1 6 181.50 13.36 -1 -1 6 65.76 4.43 -1 1 6 57.50 4.46 1 -1 -6 64.75 4.21 -1 -1 6 58.25 4.45 0 -1 -6 1927.11 118.66 0 -1 6 1819.66 128.53 0 1 6 1669.36 134.10 1 -1 6 163.59 10.55 1 -1 6 155.58 11.47 1 1 6 155.73 11.46 2 -1 6 579.28 37.90 2 -1 6 556.49 41.12 2 1 6 592.23 41.13 3 -1 6 2.13 0.83 3 1 6 1.82 0.81 4 -1 6 17.83 2.01 4 1 6 17.39 1.95 5 1 6 -0.25 1.32 5 -1 6 0.35 1.43 5 -2 -6 3.73 1.18 4 -2 -6 4.28 1.05 4 2 -6 6.99 1.81 -3 -2 6 4.77 1.30 3 -2 -6 0.00 0.75 -2 -2 6 527.28 35.74 2 -2 -6 544.66 35.46 1 2 -6 384.21 29.33 -1 -2 6 415.48 26.16 -1 -2 6 386.00 28.12 1 -2 -6 396.02 26.04 -1 2 6 391.93 28.15 0 -2 6 903.48 57.06 0 2 6 897.82 64.52 0 2 6 865.97 61.78 0 -2 6 752.57 61.82 0 -2 -6 913.02 57.03 1 -2 6 76.82 5.49 1 2 6 75.77 5.49 1 2 6 71.09 6.00 -1 -2 -6 72.80 4.98 1 -2 6 77.44 5.06 2 -2 6 466.98 33.92 2 2 6 478.25 33.90 2 -2 6 478.06 31.27 3 2 6 4.08 0.86 3 -2 6 2.67 0.88 4 -2 6 75.51 5.76 4 2 6 69.03 5.63 5 -2 6 -0.32 1.54 5 2 6 0.32 1.30 5 -3 -6 0.07 1.03 5 3 -6 0.57 0.66 4 -3 -6 32.86 2.72 3 -3 -6 47.82 3.31 -3 -3 6 36.12 3.62 -2 -3 6 78.58 5.51 2 -3 -6 71.52 5.16 2 3 -6 74.93 5.85 1 3 -6 46.71 3.52 -1 -3 6 44.57 3.38 1 -3 -6 45.17 3.21 -1 -3 6 46.93 3.30 0 -3 6 851.45 57.58 0 3 6 849.47 65.12 0 -3 -6 860.88 57.55 0 3 6 936.97 62.31 1 -3 6 285.28 20.04 1 -3 6 291.16 18.54 1 3 6 230.88 21.13 -1 -3 -6 284.20 18.48 1 3 6 302.88 20.08 2 3 6 171.64 12.29 2 -3 6 174.45 11.35 2 -3 6 164.61 12.33 3 3 6 9.19 1.24 3 -3 6 8.41 1.30 3 -3 6 11.21 1.09 4 3 6 22.80 2.41 4 -3 6 27.67 2.61 5 -3 6 1.99 1.68 5 3 6 2.90 1.47 5 -4 -6 3.58 1.25 4 -4 -6 6.55 1.23 -4 -4 6 3.86 1.60 -3 -4 6 6.52 1.57 3 -4 -6 6.87 1.08 3 4 -6 5.50 1.27 2 -4 -6 152.66 10.46 -2 -4 6 163.01 10.70 2 4 -6 152.52 11.77 1 4 -6 235.15 18.15 -1 -4 6 248.61 16.21 -1 -4 6 232.32 17.36 -1 4 6 261.25 18.30 1 -4 -6 240.85 16.15 0 4 6 36.48 3.04 0 4 6 36.55 2.68 0 -4 6 29.49 2.80 0 -4 -6 37.41 2.55 0 -4 6 37.17 2.60 1 4 6 1.59 0.86 1 -4 6 0.67 0.51 1 4 6 0.95 0.59 -1 -4 -6 0.52 0.40 1 -4 6 -0.22 0.43 2 4 6 169.24 13.66 2 -4 6 178.05 12.65 2 -4 6 176.45 11.67 2 4 6 172.91 12.58 3 -4 6 42.45 3.40 3 -4 6 41.38 3.05 3 4 6 41.71 3.33 3 4 6 33.71 4.05 4 -4 6 10.54 1.77 4 4 6 10.60 1.58 5 -4 6 0.62 1.76 5 -5 -6 -1.72 1.08 -4 -5 6 3.79 1.62 4 -5 -6 6.32 1.24 -3 -5 6 57.38 5.13 3 5 -6 66.57 5.22 2 5 -6 71.91 5.66 -2 -5 6 72.99 5.28 2 -5 -6 72.88 5.11 1 5 -6 16.66 1.61 -1 -5 6 18.58 1.60 1 -5 -6 17.07 1.58 -1 5 6 18.37 1.90 0 -5 -6 92.56 5.91 0 -5 6 75.30 6.34 0 5 6 84.47 6.26 0 -5 6 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2.95 1 1 -25 19.83 2.15 -1 -1 25 28.40 3.05 0 -1 25 1.20 1.48 0 1 25 0.67 1.48 1 1 25 -1.43 1.28 1 -1 25 -0.64 1.37 2 1 25 1.82 1.54 2 -2 -25 0.36 1.73 2 2 -25 1.07 1.14 -2 -2 25 -3.88 1.71 -2 2 25 -1.87 1.83 -1 -2 25 4.45 1.93 -1 2 25 3.80 1.86 0 -2 25 5.72 1.69 0 2 25 4.03 1.68 1 2 25 22.69 2.55 1 -2 25 22.31 2.59 -2 -3 25 0.44 1.92 2 -3 -25 7.25 2.20 -2 3 25 -0.59 1.95 -2 -3 25 6.80 1.59 -1 -3 25 1.85 1.82 -1 3 25 3.23 1.97 -1 -3 25 4.13 1.59 0 3 25 1.90 1.61 0 -3 25 2.19 1.55 1 -3 25 -0.39 1.44 1 3 25 -0.41 1.32 -2 -4 25 -4.86 1.74 2 -4 -25 -1.80 2.53 -1 -4 25 0.70 1.76 -1 4 25 -0.03 1.79 -1 -4 25 -0.34 1.44 0 -4 25 5.70 1.70 0 4 25 3.75 1.85 1 4 25 15.06 2.12 1 -4 25 13.37 2.14 -1 -5 25 2.66 1.64 -1 5 25 1.37 1.94 0 5 25 2.35 1.74 1 5 25 -0.72 1.39 1 -5 25 0.56 1.55 2 0 -26 2.43 1.31 -1 0 26 -0.76 1.77 0 0 26 7.55 1.90 1 0 26 1.96 1.46 -2 -1 26 0.26 2.09 2 1 -26 3.71 1.37 2 -1 -26 0.83 1.35 -1 -1 26 1.21 1.85 -1 1 26 -1.60 1.64 0 -1 26 21.87 2.67 0 1 26 21.37 2.65 1 -1 26 0.56 1.54 1 1 26 1.85 1.48 2 2 -26 0.74 1.18 2 -2 -26 -0.46 1.60 -2 -2 26 -1.93 1.94 -1 2 26 1.07 1.75 -1 -2 26 0.97 1.82 0 2 26 11.32 2.06 0 -2 26 10.60 2.04 1 2 26 2.60 1.48 1 -2 26 2.08 1.55 2 -3 -26 1.17 2.05 -1 3 26 -1.96 1.76 -1 -3 26 0.58 1.79 0 3 26 8.71 2.02 0 -3 26 10.48 1.99 1 3 26 5.25 1.61 1 -3 26 4.73 1.71 -1 -4 26 1.95 1.87 0 -4 26 3.90 1.77 0 4 26 4.68 1.83 2 0 -27 -0.04 1.32 -1 0 27 -1.34 1.80 0 0 27 1.55 1.69 2 -1 -27 -1.69 1.32 2 1 -27 0.35 1.32 -1 -1 27 5.86 2.08 0 1 27 -0.61 1.51 0 -1 27 2.73 1.72 2 -2 -27 0.55 1.56 -1 -2 27 2.61 1.91 0 -2 27 1.35 1.67 0 -3 27 -0.88 1.60 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 33873 _shelx_res_file ; 4bracid.res created by SHELXL-2014/7 TITL 4BRACID in P2(1)/n CELL 0.71073 4.4711 9.0316 21.6519 90.000 92.252 90.000 ZERR 4.00 0.0022 0.0044 0.0105 0.000 0.008 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O Br UNIT 40 28 4 4 LIST 4 L.S. 30 ACTA BOND $H FMAP 2 ACTA CONF SIZE 0.35 0.28 0.13 EQIV $1 -x+3/2, y-1/2, -z+3/2 HTAB C8 O1B_$1 PLAN 20 TEMP 24 WGHT 0.081200 0.106900 FVAR 0.49025 C1 1 0.599008 0.366573 0.793818 11.00000 0.05530 0.03535 = 0.06219 -0.00178 0.00968 -0.00252 BR1 4 1.379590 0.220060 1.025487 11.00000 0.08273 0.07025 = 0.06883 -0.00504 -0.01157 -0.00322 C2 1 0.797188 0.326138 0.847661 11.00000 0.05424 0.03678 = 0.05632 -0.00514 0.01247 -0.00314 C3 1 0.938422 0.439143 0.881811 11.00000 0.07576 0.03821 = 0.06058 -0.00330 0.00572 -0.00703 H3 2 0.886958 0.545239 0.867913 11.00000 0.08019 C4 1 1.118618 0.407923 0.933235 11.00000 0.07410 0.04836 = 0.06238 -0.01103 0.00719 -0.01523 H4 2 1.217248 0.493738 0.955518 11.00000 0.07698 C5 1 1.157771 0.262792 0.951222 11.00000 0.06015 0.05469 = 0.05245 -0.00654 0.00681 -0.00423 C6 1 1.023299 0.147531 0.918078 11.00000 0.07709 0.04150 = 0.06389 -0.00029 0.00161 -0.00305 H6 2 1.065424 0.051403 0.931881 11.00000 0.06975 C7 1 0.843909 0.178297 0.866186 11.00000 0.06936 0.03860 = 0.05981 -0.00533 0.00093 -0.00302 H7 2 0.751692 0.095584 0.836363 11.00000 0.05367 C8 1 0.454440 0.243870 0.755148 11.00000 0.05702 0.03956 = 0.06933 -0.00285 -0.00335 0.00161 H8B 2 0.342147 0.183549 0.782371 11.00000 0.05601 C9 1 0.256449 0.304772 0.706426 11.00000 0.06657 0.04635 = 0.08691 -0.00187 0.00214 -0.00477 H8A 2 0.617423 0.187071 0.733943 11.00000 0.06832 C10 1 0.101111 0.351560 0.669792 11.00000 0.08439 0.06010 = 0.08756 0.01683 -0.03221 0.00513 AFIX 163 H10 2 -0.028268 0.390528 0.639280 11.00000 -1.20000 AFIX 0 O1B 3 0.551436 0.495367 0.779852 11.00000 0.08751 0.03765 = 0.08951 0.00235 -0.00658 0.00020 HKLF 4 REM 4BRACID in P2(1)/n REM R1 = 0.0482 for 1397 Fo > 4sig(Fo) and 0.0656 for all 1965 data REM 133 parameters refined using 0 restraints END WGHT 0.0835 0.0786 REM Highest difference peak 0.404, deepest hole -0.620, 1-sigma level 0.105 Q1 1 1.4224 0.2858 1.0106 11.00000 0.05 0.40 Q2 1 0.2461 0.3357 0.6525 11.00000 0.05 0.40 Q3 1 0.1000 0.3873 0.6568 11.00000 0.05 0.40 Q4 1 0.0472 0.3793 0.6665 11.00000 0.05 0.38 Q5 1 0.1441 0.3840 0.6872 11.00000 0.05 0.35 Q6 1 0.7377 0.1914 0.9605 11.00000 0.05 0.32 Q7 1 1.3496 0.1623 1.0117 11.00000 0.05 0.32 Q8 1 1.6900 0.2262 1.0219 11.00000 0.05 0.32 Q9 1 0.7112 0.2302 0.9653 11.00000 0.05 0.31 Q10 1 1.8463 0.2286 1.0243 11.00000 0.05 0.31 Q11 1 1.5038 0.2063 0.9797 11.00000 0.05 0.29 Q12 1 0.9303 0.2183 1.0850 11.00000 0.05 0.28 Q13 1 1.1303 0.2186 1.0292 11.00000 0.05 0.27 Q14 1 0.6532 0.4630 0.7725 11.00000 0.05 0.27 Q15 1 0.9766 0.7069 0.9157 11.00000 0.05 0.26 Q16 1 1.3113 0.2200 1.0611 11.00000 0.05 0.26 Q17 1 1.5034 0.2480 0.9384 11.00000 0.05 0.25 Q18 1 1.6180 0.3155 0.9455 11.00000 0.05 0.25 Q19 1 0.1609 0.2409 0.7999 11.00000 0.05 0.24 Q20 1 0.5956 0.1587 0.9389 11.00000 0.05 0.22 ; _shelx_res_checksum 41374 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 _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.5990(7) 0.3666(3) 0.79382(16) 0.0508(8) Uani d 1 . . Br Br1 1.37959(10) 0.22006(5) 1.02549(2) 0.0743(2) Uani d 1 . . C C2 0.7972(7) 0.3261(3) 0.84766(16) 0.0488(7) Uani d 1 . . C C3 0.9384(9) 0.4391(4) 0.88181(17) 0.0581(9) Uani d 1 . . H H3 0.887(9) 0.545(5) 0.8679(19) 0.080(12) Uiso d 1 . . C C4 1.1186(9) 0.4079(4) 0.93323(18) 0.0615(9) Uani d 1 . . H H4 1.217(9) 0.494(5) 0.9555(19) 0.077(11) Uiso d 1 . . C C5 1.1578(9) 0.2628(4) 0.95122(18) 0.0556(8) Uani d 1 . . C C6 1.0233(9) 0.1475(4) 0.91808(18) 0.0609(9) Uani d 1 . . H H6 1.065(9) 0.051(5) 0.9319(19) 0.070(11) Uiso d 1 . . C C7 0.8439(9) 0.1783(4) 0.86619(17) 0.0560(8) Uani d 1 . . H H7 0.752(8) 0.096(4) 0.8364(15) 0.054(9) Uiso d 1 . . C C8 0.4544(9) 0.2439(4) 0.7551(2) 0.0555(9) Uani d 1 . . H H8B 0.342(9) 0.184(4) 0.7824(18) 0.056(10) Uiso d 1 . . C C9 0.2564(10) 0.3048(4) 0.7064(2) 0.0666(11) Uani d 1 . . H H8A 0.617(10) 0.187(5) 0.734(2) 0.068(12) Uiso d 1 . . C C10 0.1011(10) 0.3516(5) 0.6698(2) 0.0783(12) Uani d 1 . . H H10 -0.0283 0.3905 0.6393 0.094 Uiso calc 1 . . O O1 0.5514(7) 0.4954(2) 0.77985(13) 0.0718(8) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0553(18) 0.0353(15) 0.0622(19) -0.0025(13) 0.0097(15) -0.0018(14) Br1 0.0827(4) 0.0702(3) 0.0688(3) -0.00322(18) -0.0116(2) -0.00504(18) C2 0.0542(18) 0.0368(14) 0.0563(18) -0.0031(13) 0.0125(15) -0.0051(14) C3 0.076(2) 0.0382(16) 0.061(2) -0.0070(15) 0.0057(18) -0.0033(15) C4 0.074(2) 0.0484(19) 0.062(2) -0.0152(17) 0.0072(18) -0.0110(17) C5 0.060(2) 0.0547(19) 0.0524(19) -0.0042(15) 0.0068(15) -0.0065(16) C6 0.077(2) 0.0415(18) 0.064(2) -0.0030(17) 0.0016(18) -0.0003(16) C7 0.069(2) 0.0386(15) 0.060(2) -0.0030(15) 0.0009(17) -0.0053(15) C8 0.057(2) 0.0396(15) 0.069(2) 0.0016(15) -0.0034(19) -0.0029(16) C9 0.067(2) 0.0464(18) 0.087(3) -0.0048(17) 0.002(2) -0.0019(19) C10 0.084(3) 0.060(2) 0.088(3) 0.005(2) -0.032(2) 0.017(2) O1 0.0875(18) 0.0377(12) 0.0895(19) 0.0002(12) -0.0066(16) 0.0024(13) 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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 C1 C2 . . 121.6(3) ? O1 C1 C8 . . 119.6(3) ? C2 C1 C8 . . 118.8(3) ? C3 C2 C7 . . 118.9(3) ? C3 C2 C1 . . 118.7(3) ? C7 C2 C1 . . 122.4(3) ? C4 C3 C2 . . 121.1(3) ? C4 C3 H3 . . 123(2) ? C2 C3 H3 . . 116(2) ? C5 C4 C3 . . 119.2(3) ? C5 C4 H4 . . 123(2) ? C3 C4 H4 . . 117(3) ? C4 C5 C6 . . 121.3(4) ? C4 C5 Br1 . . 119.4(3) ? C6 C5 Br1 . . 119.2(3) ? C7 C6 C5 . . 119.7(3) ? C7 C6 H6 . . 123(3) ? C5 C6 H6 . . 117(3) ? C6 C7 C2 . . 119.8(3) ? C6 C7 H7 . . 123.5(18) ? C2 C7 H7 . . 116.4(18) ? C9 C8 C1 . . 110.9(3) ? C9 C8 H8B . . 110(2) ? C1 C8 H8B . . 107(2) ? C9 C8 H8A . . 107(2) ? C1 C8 H8A . . 109(2) ? H8B C8 H8A . . 113(3) ? C10 C9 C8 . . 178.8(6) ? C9 C10 H10 . . 180.0 ? 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 C1 O1 . 1.218(4) ? C1 C2 . 1.482(5) ? C1 C8 . 1.518(5) ? Br1 C5 . 1.895(4) ? C2 C3 . 1.397(5) ? C2 C7 . 1.407(5) ? C3 C4 . 1.378(6) ? C3 H3 . 1.03(5) ? C4 C5 . 1.377(5) ? C4 H4 . 1.01(5) ? C5 C6 . 1.388(5) ? C6 C7 . 1.383(5) ? C6 H6 . 0.93(4) ? C7 H7 . 1.06(3) ? C8 C9 . 1.458(7) ? C8 H8B . 0.96(4) ? C8 H8A . 1.02(4) ? C9 C10 . 1.117(6) ? C10 H10 . 0.9300 ? 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 C1 O1 C9 2_556 . 3.134(5) . 154.2(3) C8 H8A O1 2_646 1.02(4) 2.31(4) 3.259(5) 156(3) C7 H7 C10 2_546 1.06(3) 2.71(4) 3.626(5) 144(3) C10 H10 Br1 4_465 0.93 2.68 3.305(5) 126 . . . . . . . . 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 O1 C1 C2 C3 . . . . -1.9(5) ? C8 C1 C2 C3 . . . . 177.7(3) ? O1 C1 C2 C7 . . . . 177.0(3) ? C8 C1 C2 C7 . . . . -3.4(5) ? C7 C2 C3 C4 . . . . -0.7(5) ? C1 C2 C3 C4 . . . . 178.3(3) ? C2 C3 C4 C5 . . . . -0.4(6) ? C3 C4 C5 C6 . . . . 1.0(6) ? C3 C4 C5 Br1 . . . . -175.1(3) ? C4 C5 C6 C7 . . . . -0.6(6) ? Br1 C5 C6 C7 . . . . 175.5(3) ? C5 C6 C7 C2 . . . . -0.5(6) ? C3 C2 C7 C6 . . . . 1.1(6) ? C1 C2 C7 C6 . . . . -177.8(3) ? O1 C1 C8 C9 . . . . -3.3(6) ? C2 C1 C8 C9 . . . . 177.1(3) ? _cod_database_fobs_code 2022800