#------------------------------------------------------------------------------ #$Date: 2025-01-15 04:30:19 +0200 (Wed, 15 Jan 2025) $ #$Revision: 297321 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023352.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_2023352 loop_ _publ_author_name 'Groneck, Erin N.' 'Peek, Nathan' 'Lynch, Will E.' 'Padgett, Clifford W.' _publ_section_title ; Crystal structures of zinc(II) coordination complexes with isoquinoline N-oxide ; _journal_coeditor_code HB8119 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025000180 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Zn Br2 (C9 H7 N1 O1)2]' _chemical_formula_moiety 'C18 H14 Br2 N2 O2 Zn' _chemical_formula_sum 'C18 H14 Br2 N2 O2 Zn' _chemical_formula_weight 515.50 _chemical_name_systematic ; Dibromidobis(isoquinoline N-oxide-\kO)zinc(II) ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 96.472(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.1095(10) _cell_length_b 7.2020(6) _cell_length_c 14.9534(11) _cell_measurement_reflns_used 2412 _cell_measurement_temperature 170 _cell_measurement_theta_max 33.1270 _cell_measurement_theta_min 2.4460 _cell_volume 1830.9(2) _computing_cell_refinement ; CrysAlisPro 1.171.39.46b (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlisPro 1.171.39.46b (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlisPro 1.171.39.46b (Rigaku OD, 2018) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL 2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 170 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_unetI/netI 0.0508 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 2980 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.345 _diffrn_reflns_theta_min 2.396 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 5.720 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.35745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2019) ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.870 _exptl_crystal_description block _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.830 _refine_diff_density_min -0.960 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 114 _refine_ls_number_reflns 1671 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0519 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1335 _refine_ls_wR_factor_ref 0.1407 _reflns_number_gt 1402 _reflns_number_total 1671 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8119.cif _cod_data_source_block II _cod_database_code 2023352 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_hkl_file ; 0 0 2 888.14 13.15 0 0 -2 991.19 13.61 0 0 -3 3.90 1.75 0 0 -4 2142.28 30.09 0 0 -5 2.58 1.87 0 0 -6 716.46 21.29 0 0 -7 2.59 2.63 0 0 -8 230.07 15.67 0 0 -9 -3.26 4.23 0 0 -10 174.63 16.68 0 0 -11 1.18 4.90 0 0 -12 135.14 20.35 0 0 -13 12.17 11.23 0 0 -14 571.29 46.72 0 0 -15 -3.59 8.89 0 0 -16 30.48 13.45 0 0 -17 7.98 12.13 0 -2 0 448.11 10.47 0 -2 -1 2181.58 26.01 0 -2 1 2187.21 18.82 0 -2 -2 271.69 10.07 0 -2 -2 271.18 10.65 0 -2 -3 1069.76 18.38 0 -2 -3 964.46 22.23 0 -2 -4 611.17 19.45 0 -2 -5 22.27 4.26 0 -2 -6 949.92 27.89 0 2 -6 981.59 19.29 0 2 -7 30.43 5.13 0 -2 -7 22.00 4.90 0 2 -8 27.79 5.64 0 -2 -8 52.36 7.88 0 -2 -9 1055.45 35.07 0 2 -9 777.62 32.25 0 2 -10 118.85 11.75 0 -2 -10 175.51 16.04 0 -2 -11 1456.90 50.51 0 2 -11 1260.03 34.54 0 -2 -12 104.59 15.12 0 2 -12 88.54 10.62 0 2 -13 986.69 38.17 0 -2 -13 953.99 45.54 0 -2 -14 59.65 13.88 0 2 -14 62.36 13.88 0 -2 -15 699.47 45.80 0 -2 -16 217.09 33.21 0 -2 -17 143.27 26.14 0 -4 0 138.87 8.62 0 -4 -1 167.58 9.32 0 -4 1 150.44 8.41 0 -4 2 604.49 16.45 0 -4 -2 722.97 20.17 0 -4 -3 189.89 11.43 0 -4 -3 136.04 9.44 0 -4 -4 124.53 9.55 0 -4 -4 136.04 8.89 0 -4 -5 265.12 14.90 0 -4 -5 296.48 13.46 0 -4 -6 21.98 5.07 0 -4 -7 267.37 17.05 0 -4 -8 371.18 21.52 0 -4 -9 66.52 10.01 0 -4 -10 649.30 33.85 0 -4 -11 105.61 15.18 0 -4 -12 588.62 33.60 0 -4 -13 49.96 12.15 0 -4 -14 541.65 37.19 0 -4 -15 61.94 14.78 0 -6 0 10.33 4.76 0 -6 -1 1234.95 32.37 0 -6 1 1143.40 27.79 0 -6 -2 14.79 6.13 0 -6 2 6.68 2.05 0 -6 -2 14.22 5.01 0 -6 -3 479.24 21.77 0 -6 -3 469.58 20.33 0 -6 -4 2.24 3.24 0 -6 -4 3.56 3.96 0 -6 -5 269.08 18.95 0 -6 -5 287.92 15.36 0 -6 -6 0.28 3.71 0 -6 -7 3.85 4.29 0 -6 -8 1.38 4.48 0 -6 -9 0.09 5.22 0 -6 -10 39.87 8.94 0 -6 -11 11.19 7.99 0 -6 -12 57.08 13.19 0 -8 0 132.83 14.22 0 -8 -1 19.77 5.74 0 -8 -2 22.38 6.62 0 -8 -2 34.62 7.52 0 -8 -3 5.35 3.88 0 -8 -3 13.01 6.19 0 -8 -4 12.46 7.91 0 -8 -4 21.03 5.48 0 -8 -5 67.01 12.10 0 -8 -6 30.40 8.56 1 -1 -17 5.27 13.72 1 1 -17 5.21 9.67 1 1 -16 23.20 13.16 1 -1 -16 64.63 17.57 1 1 -15 24.57 12.12 1 -1 -15 17.92 9.11 1 1 -14 0.37 10.35 1 -1 -14 13.68 7.96 1 1 -13 482.50 38.20 1 -1 -13 450.05 32.20 1 -1 -12 18.86 8.33 1 1 -12 0.37 5.19 1 1 -11 959.25 40.07 1 -1 -11 775.96 32.83 1 -1 -10 103.17 12.56 1 1 -10 116.21 14.75 1 1 -9 1107.92 33.74 1 -1 -9 1041.70 34.88 1 1 -8 10.48 3.88 1 -1 -8 4.34 3.55 1 1 -7 1748.30 34.73 1 -1 -7 1622.84 37.55 1 -1 -6 267.93 14.30 1 1 -6 289.02 12.38 1 1 -5 6.10 2.16 1 -1 -5 4.34 2.73 1 -1 -4 784.31 18.60 1 1 -4 937.94 14.97 1 -1 -3 103.59 6.79 -1 -1 3 105.31 3.60 1 -1 -2 6162.67 43.14 1 -1 -1 212.51 7.55 1 -1 0 1263.47 11.03 -1 -1 0 1359.67 15.13 -1 -1 -1 55.35 4.49 -1 -1 -1 43.68 3.26 -1 -1 -2 4721.33 42.74 -1 1 -2 4561.76 23.38 1 -1 3 3401.20 26.90 -1 -1 -3 3412.88 42.82 -1 -1 -4 4792.43 56.10 -1 1 -4 5303.47 47.01 -1 1 -5 2714.42 33.99 -1 -1 -5 2951.36 48.43 -1 1 -6 4549.63 62.52 -1 -1 -6 4580.12 65.94 -1 -1 -7 1.42 3.16 -1 1 -7 11.94 5.37 -1 1 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9.37 -1 -3 -3 134.12 8.53 1 -3 3 118.01 3.87 -1 -3 -4 130.99 10.12 -1 -3 -5 73.47 8.28 -1 -3 -6 8.06 3.88 -1 -3 -7 16.63 5.21 -1 -3 -8 8.70 5.42 -1 -3 -9 55.78 8.88 -1 -3 -10 184.27 17.56 -1 -3 -11 330.33 24.51 -1 -3 -12 313.71 26.13 -1 -3 -13 439.07 33.37 -1 -3 -14 742.09 51.56 -1 -3 -15 546.57 42.89 -1 -3 -16 292.56 33.88 1 -5 -14 9.19 9.96 1 -5 -13 34.39 11.36 1 -5 -12 334.78 25.54 1 -5 -11 28.35 8.27 1 -5 -10 310.31 22.76 1 -5 -9 14.28 6.10 1 -5 -8 322.46 20.24 1 -5 -7 4.91 4.00 1 -5 -6 37.97 7.18 1 -5 -5 115.47 8.63 1 -5 -5 105.47 10.04 1 -5 -4 88.95 7.73 1 -5 -4 68.18 7.91 1 -5 -3 128.58 10.34 1 -5 -3 129.84 10.87 1 -5 -2 4.99 3.14 -1 -5 2 0.58 1.45 1 -5 -1 683.15 20.67 -1 -5 1 632.11 18.97 1 -5 0 41.48 5.31 -1 -5 0 80.31 7.95 -1 -5 -1 1065.38 29.82 1 -5 1 837.92 19.82 1 -5 2 225.74 10.85 -1 -5 -2 249.77 15.38 1 -5 3 891.95 18.02 -1 -5 -3 892.72 28.97 -1 -5 -4 257.83 15.45 -1 -5 -4 245.82 13.85 -1 -5 -5 690.64 23.32 -1 -5 -5 665.12 27.33 -1 -5 -6 60.66 9.49 -1 -5 -7 498.38 26.07 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2.87 2 0 -6 987.67 25.88 2 0 -5 2.41 1.84 2 0 -4 1263.13 25.28 2 0 -3 6.50 1.86 2 0 -2 182.66 6.41 2 0 -1 2.81 1.02 -2 0 1 4.52 1.15 2 0 0 1654.95 17.06 2 0 1 1.57 1.01 2 0 2 9999.00 60.87 -2 0 -3 3.76 2.33 -2 0 -4 7299.35 63.06 -2 0 -5 5.30 2.94 -2 0 -6 2881.78 51.92 -2 0 -7 1.11 4.52 -2 0 -8 7665.47 104.69 -2 0 -9 -6.27 6.40 -2 0 -10 1626.13 52.90 -2 0 -11 -1.62 6.84 -2 0 -12 246.74 22.69 -2 0 -13 0.04 6.80 -2 0 -14 -1.88 6.13 -2 0 -15 8.83 7.83 -2 0 -16 178.92 24.14 -2 0 -17 0.81 10.98 2 -2 -17 96.15 21.45 2 -2 -16 67.59 15.39 2 -2 -15 24.51 9.78 2 2 -14 207.05 24.43 2 -2 -14 146.30 18.43 2 -2 -13 144.26 16.52 2 2 -13 228.16 24.58 2 2 -12 157.31 17.60 2 -2 -12 135.02 15.14 2 2 -11 841.79 33.35 2 -2 -11 596.46 30.37 2 -2 -10 183.42 16.37 2 2 -10 190.34 14.93 2 2 -9 2356.94 45.06 2 -2 -9 2216.90 51.62 2 -2 -8 198.06 14.65 2 2 -8 185.52 13.43 2 2 -7 2416.05 37.59 2 -2 -7 2352.41 47.65 2 2 -6 461.39 11.65 2 -2 -6 475.04 18.89 2 2 -5 2669.44 24.66 2 -2 -5 2319.09 38.92 2 2 -4 1214.27 16.32 2 -2 -4 825.24 23.41 2 2 -3 1724.94 16.28 2 -2 -3 1701.84 19.07 2 2 -2 2162.58 20.05 2 -2 -2 2177.95 30.19 2 -2 -1 2525.89 30.60 2 2 -1 2372.65 28.34 2 -2 0 2241.36 24.74 -2 -2 0 2319.94 35.98 2 -2 1 2308.15 23.39 -2 -2 -1 2272.84 31.41 -2 -2 -1 2292.36 33.59 2 -2 2 3349.35 25.63 -2 -2 -2 3321.82 40.15 2 -2 3 815.16 12.74 -2 -2 -3 1020.87 31.61 -2 -2 -4 1263.20 34.00 2 -2 4 1094.06 16.50 2 -2 5 1402.59 19.29 -2 -2 -5 1441.99 37.74 2 -2 6 486.74 12.22 -2 -2 -6 481.58 23.65 2 -2 7 1024.96 19.97 -2 -2 -7 1115.99 37.70 -2 -2 -8 59.69 8.79 2 -2 8 46.47 5.59 -2 -2 -9 217.22 19.37 2 -2 9 163.91 10.65 2 -2 10 177.48 11.85 -2 -2 -10 296.25 27.34 2 -2 11 5.36 3.54 -2 -2 -11 3.30 7.20 -2 -2 -12 133.77 19.41 2 -2 12 68.15 8.81 2 -2 13 48.33 8.57 -2 -2 -13 79.89 15.71 2 -2 14 67.03 10.33 -2 -2 -14 169.47 22.59 -2 -2 -15 463.62 37.58 -2 -2 -16 59.12 17.50 -2 -2 -17 301.52 30.92 2 -4 -15 21.20 11.36 2 -4 -14 10.96 6.82 2 -4 -13 142.30 18.15 2 -4 -12 396.37 26.64 2 -4 -11 1.41 5.10 2 -4 -10 302.03 22.38 2 -4 -9 87.56 11.18 2 -4 -8 1298.21 40.02 2 -4 -7 539.85 23.78 2 -4 -6 1290.71 35.69 2 -4 -5 51.22 5.03 2 -4 -5 55.82 7.51 2 -4 -4 1096.42 23.19 2 4 -4 1150.43 13.40 2 -4 -4 1169.44 30.63 2 4 -3 234.63 8.82 2 -4 -3 257.74 14.13 2 4 -2 509.84 17.25 2 -4 -2 659.68 20.82 2 -4 -1 248.34 11.96 -2 -4 1 198.71 10.81 2 -4 0 10.56 2.29 -2 -4 0 6.56 2.90 -2 -4 -1 100.60 9.30 -2 -4 -1 75.56 8.84 2 -4 1 81.77 6.11 -2 -4 -2 362.97 16.89 -2 -4 -2 377.59 17.46 -2 -4 -3 475.22 18.58 2 -4 3 482.44 10.99 -2 -4 -4 546.84 19.91 -2 -4 -4 604.78 25.32 -2 -4 -5 123.88 13.11 -2 -4 -6 545.99 26.57 -2 -4 -7 152.89 15.18 -2 -4 -8 224.06 18.85 -2 -4 -9 109.99 15.15 -2 -4 -10 36.17 10.47 -2 -4 -11 123.45 19.36 -2 -4 -12 72.66 15.94 -2 -4 -13 123.54 18.93 -2 -4 -14 187.12 23.41 -2 -4 -15 60.52 13.41 2 -6 -13 6.24 8.05 2 -6 -12 23.49 9.83 2 -6 -11 3.47 6.90 2 -6 -10 -5.19 5.78 2 -6 -9 15.83 6.87 2 -6 -8 2.81 4.35 2 -6 -7 52.85 8.40 2 -6 -6 31.63 5.15 2 -6 -6 17.49 6.17 2 -6 -5 154.47 10.29 2 -6 -5 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376.79 28.77 11 5 6 73.04 12.93 11 -5 6 47.92 7.55 11 5 7 316.43 28.21 11 5 8 47.42 13.35 11 5 9 154.34 22.19 11 -7 -5 4.31 6.83 -11 -7 5 3.77 6.26 11 -7 -4 21.63 9.67 -11 -7 4 49.58 11.15 11 -7 -3 9.45 6.98 -11 -7 3 10.51 7.18 11 -7 -2 1.10 5.34 -11 -7 2 -1.96 6.78 -11 -7 1 17.80 9.57 11 7 -1 36.58 9.21 11 -7 -1 14.44 7.36 11 7 0 2.13 6.18 -11 -7 0 17.64 8.56 11 -7 0 9.07 6.19 11 7 1 51.82 11.87 11 7 2 69.31 13.02 11 7 3 215.59 21.84 12 0 -15 -5.78 8.99 12 0 -14 510.24 30.98 12 0 -13 2.74 6.72 12 0 -12 309.82 21.21 12 0 -11 3.36 4.92 12 0 -10 1.83 3.74 12 0 -9 -0.82 4.22 12 0 -8 85.69 12.69 12 0 -7 1.34 3.24 12 0 -6 293.37 18.61 12 0 -5 -6.25 3.50 12 0 -4 88.90 10.27 12 0 -3 6.88 4.30 12 0 -2 145.82 12.97 12 0 -1 -0.09 4.32 12 0 0 8.99 5.89 12 0 1 -3.51 4.61 12 0 2 321.11 20.94 12 0 3 -4.23 6.08 12 0 4 1261.71 43.62 12 0 5 -4.64 5.03 12 0 6 1887.02 56.34 12 0 7 -6.58 6.68 12 0 8 1644.80 54.61 12 0 9 -1.27 7.76 12 0 10 705.72 38.18 12 0 11 0.89 6.57 12 0 12 273.73 25.25 12 0 13 -2.77 7.77 12 -2 -15 44.24 11.74 -12 -2 14 75.69 12.14 12 -2 -14 83.11 15.08 12 2 -14 108.50 14.77 -12 -2 13 9.90 6.52 12 -2 -13 3.99 5.59 12 2 -13 18.69 7.67 12 2 -12 53.92 10.30 -12 -2 12 70.48 11.76 12 -2 -12 55.42 11.22 12 -2 -11 65.59 11.46 12 2 -11 51.79 8.61 -12 -2 11 57.11 10.13 12 -2 -10 392.76 24.14 12 2 -10 389.41 22.64 -12 -2 10 360.31 24.11 12 -2 -9 179.07 16.37 12 2 -9 200.66 16.16 -12 -2 9 196.85 17.42 12 -2 -8 116.43 11.47 -12 -2 8 151.00 15.92 12 2 -8 143.97 13.53 12 -2 -7 990.97 34.84 -12 -2 7 1067.72 40.43 12 2 -7 978.00 32.64 -12 -2 6 153.24 16.00 12 2 -6 126.29 12.33 12 -2 -5 1733.20 46.03 12 2 -5 1799.27 43.80 12 2 -4 48.18 7.36 12 -2 -4 45.12 8.05 12 -2 -3 1878.69 46.20 12 2 -3 1837.89 46.68 12 -2 -2 382.51 21.16 12 2 -2 398.05 21.68 12 2 -1 460.09 24.32 12 -2 -1 424.12 22.32 12 2 0 133.40 13.72 12 -2 0 146.14 13.55 12 2 1 151.28 15.37 12 -2 1 137.35 13.74 12 2 2 56.31 9.94 12 -2 2 45.89 8.22 12 -2 3 21.73 6.63 12 2 3 24.60 8.84 12 2 4 300.95 22.96 12 -2 4 247.12 18.40 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4 0 267.10 20.28 12 -4 0 270.97 19.02 12 -4 1 376.03 21.65 12 4 1 400.70 25.66 12 -4 2 2.23 4.88 12 4 2 -0.68 5.33 12 -4 3 130.46 12.81 12 4 3 139.83 16.31 12 -4 4 -1.68 4.39 12 4 4 4.20 5.83 12 -4 5 12.78 5.88 12 4 5 23.40 9.61 12 -4 6 139.61 14.65 12 4 6 143.88 17.21 12 -4 7 63.09 9.66 12 4 7 68.20 14.32 12 -4 8 35.08 8.02 12 4 8 80.18 16.78 12 4 9 119.68 19.28 12 4 10 276.93 29.44 12 -6 -8 17.90 8.90 -12 -6 8 11.29 6.79 12 -6 -7 23.96 9.20 -12 -6 7 13.09 8.22 -12 -6 6 5.08 5.74 12 -6 -6 4.29 6.77 -12 -6 5 100.38 15.62 12 -6 -5 58.34 11.50 -12 -6 4 11.10 7.95 12 -6 -4 3.54 6.55 12 6 -4 4.73 5.63 -12 -6 3 11.50 7.16 12 -6 -3 11.81 7.50 12 6 -3 26.66 8.47 12 6 -2 10.91 6.55 -12 -6 2 6.14 6.87 12 -6 -2 0.03 5.26 -12 -6 1 -2.59 8.14 12 -6 -1 2.57 6.02 12 6 0 18.39 7.08 12 -6 0 22.94 6.64 12 6 1 28.34 8.51 12 -6 1 8.07 5.08 12 6 2 26.18 8.90 12 -6 2 18.48 7.20 12 -6 3 79.84 8.57 12 6 3 139.51 18.09 12 6 4 -8.68 8.26 12 6 5 289.15 24.57 12 6 6 -1.10 8.35 13 -1 -15 91.39 16.08 13 1 -15 117.40 16.93 13 1 -14 473.23 31.76 13 -1 -14 408.35 28.36 13 -1 -13 92.32 16.19 13 1 -13 76.30 11.95 13 -1 -12 561.18 30.23 13 1 -12 561.98 28.32 -13 -1 12 583.39 28.57 -13 -1 11 49.00 9.89 13 -1 -11 41.82 8.65 13 1 -11 33.52 6.94 13 1 -10 333.50 22.04 -13 -1 10 365.80 22.64 13 1 -9 11.49 6.27 13 -1 -9 13.59 5.80 13 -1 -8 55.42 9.52 13 1 -8 43.90 7.91 13 -1 -7 149.82 15.81 13 1 -7 123.14 12.92 13 -1 -6 20.80 6.17 13 1 -6 24.97 6.35 13 -1 -5 884.07 33.44 13 1 -5 933.22 32.33 13 -1 -4 11.79 5.11 13 1 -4 23.31 6.68 13 -1 -3 361.81 21.27 13 1 -3 371.60 21.72 13 -1 -2 315.51 20.43 13 1 -2 367.28 22.12 13 -1 -1 706.48 30.17 13 1 -1 756.05 32.03 13 1 0 32.21 8.62 13 -1 0 14.48 5.54 13 1 1 382.20 24.30 13 -1 1 382.83 23.00 13 1 2 1.92 5.41 13 -1 2 -1.95 4.50 13 1 3 154.58 16.91 13 -1 3 137.84 15.13 13 -1 4 207.11 18.13 13 1 4 179.80 18.21 13 1 5 4.91 7.07 13 -1 5 3.81 6.67 13 -1 6 409.72 26.05 13 1 6 391.37 28.29 13 -1 7 47.96 9.80 13 1 7 45.13 11.18 13 -1 8 453.16 28.46 13 1 8 436.38 31.42 13 -1 9 67.18 12.32 13 1 9 66.15 13.28 13 -1 10 456.01 30.16 13 1 10 450.92 34.42 13 -1 11 195.58 20.61 13 1 11 212.02 24.54 13 -1 12 318.39 25.94 13 1 12 345.68 30.30 13 -3 -13 36.98 10.01 -13 -3 13 40.53 9.59 -13 -3 12 6.24 8.32 13 -3 -12 -4.02 5.96 13 3 -12 -4.03 5.77 -13 -3 11 19.84 8.00 13 -3 -11 13.28 8.27 13 3 -11 20.74 8.25 13 3 -10 2.18 6.25 -13 -3 10 19.03 7.98 13 -3 -10 1.62 5.59 13 3 -9 34.18 8.02 -13 -3 9 42.83 10.04 13 -3 -9 39.77 8.66 13 -3 -8 187.57 17.36 -13 -3 8 208.63 19.98 13 3 -8 191.82 15.58 13 -3 -7 53.63 7.71 13 3 -7 71.62 11.09 13 -3 -6 429.29 23.81 -13 -3 6 409.69 27.81 13 3 -6 421.98 22.53 13 -3 -5 304.22 20.94 -13 -3 5 354.61 25.10 13 3 -5 283.82 19.14 13 -3 -4 1014.52 43.42 13 3 -4 648.16 30.37 13 -3 -3 375.10 22.84 13 3 -3 366.79 22.54 13 3 -2 429.90 24.36 13 -3 -2 398.28 22.69 13 3 -1 1621.22 49.03 13 -3 -1 1622.31 45.39 13 3 0 1103.45 41.24 13 -3 0 1075.99 37.35 13 3 1 590.10 31.36 13 -3 1 576.40 28.14 13 3 2 579.02 32.12 13 -3 2 512.79 27.13 13 3 3 174.47 17.87 13 -3 3 161.91 15.74 13 3 4 5.61 6.09 13 -3 4 22.18 7.13 13 3 5 47.42 11.66 13 -3 5 45.94 9.99 13 3 6 0.69 6.96 13 -3 6 -3.39 5.17 13 -3 7 -0.93 4.54 13 3 7 2.58 8.33 13 3 8 45.98 12.84 13 -3 8 60.60 9.96 13 -3 9 100.02 13.37 13 3 9 89.36 15.88 13 -3 10 -2.20 5.77 13 3 10 -14.13 9.33 13 3 11 22.74 11.46 -13 -5 10 82.75 13.77 13 -5 -10 87.69 14.20 -13 -5 9 -4.03 7.55 13 -5 -9 20.63 14.16 -13 -5 8 6.75 6.79 13 -5 -8 16.67 8.77 -13 -5 7 3.96 6.93 13 5 -7 3.97 4.86 13 -5 -7 5.72 6.74 13 -5 -6 94.01 14.47 -13 -5 6 100.34 15.49 13 5 -6 94.26 11.47 13 5 -5 11.97 5.89 -13 -5 5 16.56 10.69 13 -5 -5 8.20 4.78 13 -5 -4 142.35 15.81 -13 -5 4 130.57 16.93 13 5 -4 145.95 15.28 -13 -5 3 28.05 10.04 13 -5 -3 17.93 6.10 13 5 -3 31.72 8.22 13 5 -2 247.27 21.96 13 -5 -2 226.09 16.43 13 5 -1 25.90 9.02 13 -5 -1 19.75 6.88 13 -5 0 233.77 18.57 13 5 0 240.82 20.26 13 5 1 2.47 6.70 13 -5 1 2.11 6.10 13 -5 2 97.96 15.41 13 5 2 69.60 12.63 13 -5 3 0.59 4.83 13 5 3 -12.39 8.32 13 -5 4 92.97 11.50 13 5 4 78.59 14.20 13 -5 5 192.38 16.43 13 5 5 225.02 22.94 13 5 6 17.75 7.75 13 5 7 225.48 23.82 13 5 8 48.39 11.94 14 0 -14 509.02 35.79 14 0 -13 -6.79 6.74 14 0 -12 994.59 40.30 14 0 -11 -1.43 3.63 14 0 -10 421.41 24.89 14 0 -9 -2.83 5.73 14 0 -8 1053.79 38.33 14 0 -7 -3.99 5.02 14 0 -6 402.17 22.51 14 0 -5 2.69 4.57 14 0 -4 58.53 10.09 14 0 -3 3.89 5.16 14 0 -2 464.85 25.13 14 0 -1 3.55 5.65 14 0 0 173.42 16.46 14 0 1 4.02 5.78 14 0 2 139.15 15.60 14 0 3 18.18 6.55 14 0 4 80.35 12.67 14 0 5 -4.07 6.56 14 0 6 25.05 9.54 14 0 7 -3.90 6.93 14 0 8 185.19 20.01 14 0 9 9.35 9.27 14 0 10 365.49 29.65 14 0 11 -7.99 8.95 14 2 -13 99.01 14.35 -14 -2 13 117.87 15.46 14 -2 -13 121.28 17.56 14 2 -12 34.38 7.40 14 -2 -12 50.51 10.24 14 -2 -11 225.93 19.35 14 2 -11 263.02 20.17 -14 -2 11 290.07 24.02 14 -2 -10 114.71 13.91 -14 -2 10 141.62 16.25 -14 -2 9 120.41 15.60 14 2 -9 105.61 12.43 14 -2 -8 221.22 18.26 14 2 -8 217.71 16.93 14 2 -7 31.06 7.41 14 -2 -7 32.30 8.41 14 -2 -6 197.35 20.62 14 2 -6 137.96 13.88 14 -2 -5 64.62 10.39 14 2 -5 65.03 10.34 14 -2 -4 5.87 5.15 14 2 -4 4.91 5.00 14 -2 -3 1074.24 38.56 14 2 -3 1076.28 38.50 14 -2 -2 569.29 27.96 14 2 -2 598.88 30.39 14 2 -1 738.59 33.89 14 -2 -1 741.99 32.15 14 2 0 239.64 19.66 14 -2 0 201.93 17.50 14 2 1 1042.85 42.37 14 -2 1 1015.95 39.85 14 2 2 142.93 16.73 14 -2 2 91.77 12.65 14 2 3 784.03 38.86 14 -2 3 746.04 34.18 14 -2 4 14.04 5.75 14 2 4 9.17 8.22 14 2 5 518.67 33.11 14 -2 5 521.74 29.70 14 2 6 114.55 18.07 14 -2 6 86.73 13.96 14 2 7 36.62 11.77 14 -2 7 16.70 8.24 14 2 8 26.48 12.04 14 -2 8 21.62 8.21 14 2 9 9.46 7.50 14 -2 9 8.20 6.11 14 2 10 46.53 13.64 14 -2 10 72.09 11.69 14 -2 11 119.16 15.15 14 2 11 111.72 18.43 -14 -4 11 38.56 10.99 14 -4 -11 33.89 9.88 14 -4 -10 179.93 22.50 -14 -4 10 126.90 17.20 14 4 -9 39.10 9.37 -14 -4 9 29.36 9.54 14 -4 -9 50.43 10.97 14 4 -8 26.86 6.89 -14 -4 8 15.08 9.25 14 -4 -8 18.92 9.39 -14 -4 7 12.11 6.49 14 4 -7 10.70 5.82 14 -4 -7 17.77 7.79 -14 -4 6 19.74 10.43 14 -4 -6 14.68 5.89 14 4 -6 6.91 4.92 14 4 -5 8.99 6.05 -14 -4 5 9.35 7.60 14 -4 -5 8.83 4.72 14 -4 -4 197.37 18.12 14 4 -4 249.21 19.54 14 4 -3 25.67 8.34 14 -4 -3 38.10 9.69 14 4 -2 505.85 28.77 14 -4 -2 633.81 36.51 14 -4 -1 55.29 10.83 14 4 -1 55.79 11.53 14 4 0 627.65 33.22 14 -4 0 563.70 27.88 14 4 1 58.29 11.41 14 -4 1 70.67 11.44 14 4 2 643.16 35.64 14 -4 2 560.98 29.32 14 4 3 178.57 20.21 14 -4 3 184.85 16.31 14 4 4 331.79 27.31 14 -4 4 305.47 21.12 14 -4 5 21.26 7.20 14 4 5 34.60 11.82 14 -4 6 84.19 11.87 14 4 6 73.80 15.12 14 -4 7 30.36 7.82 14 4 7 31.00 11.99 14 -4 8 0.25 4.98 14 4 8 26.00 11.41 14 -6 -5 80.83 13.39 -14 -6 5 57.78 12.21 -14 -6 4 67.16 14.21 14 -6 -4 66.46 11.74 14 6 -4 74.93 13.80 14 -6 -3 9.60 6.80 14 6 -3 5.77 5.78 14 -6 -2 7.11 6.01 14 6 -2 0.14 7.17 14 6 -1 34.68 11.05 14 -6 -1 9.83 5.95 14 6 0 4.72 8.45 14 -6 0 -8.76 6.87 14 -6 1 45.56 7.55 14 6 1 73.12 14.33 14 6 2 16.71 8.25 14 -6 2 8.19 5.69 14 6 3 8.39 8.02 15 -1 -13 29.55 9.14 15 1 -13 25.04 8.53 15 -1 -12 243.42 20.04 15 1 -12 211.94 16.18 15 -1 -11 107.07 13.66 15 1 -11 95.98 12.95 15 -1 -10 571.83 29.10 15 1 -10 826.12 41.02 15 -1 -9 357.19 23.83 15 1 -9 367.49 23.81 15 -1 -8 1233.91 59.44 15 1 -8 733.72 32.32 15 -1 -7 48.45 9.76 15 1 -7 47.45 9.61 15 -1 -6 587.04 29.43 15 1 -6 582.16 29.38 15 -1 -5 -0.33 4.47 15 1 -5 10.65 6.60 15 -1 -4 148.65 15.39 15 1 -4 179.28 16.50 15 -1 -3 -6.92 6.20 15 1 -3 5.39 5.89 15 -1 -2 659.41 31.47 15 1 -2 657.86 32.62 15 1 -1 17.13 6.08 15 -1 -1 10.89 6.12 15 -1 0 48.17 9.68 15 1 0 68.23 11.73 15 1 1 413.82 27.60 15 -1 1 358.79 24.74 15 -1 2 58.85 11.00 15 1 2 56.59 10.71 15 1 3 859.16 42.58 15 -1 3 857.15 39.44 15 1 4 18.10 9.68 15 -1 4 0.28 6.83 15 -1 5 319.77 24.29 15 1 5 281.41 25.43 15 1 6 55.71 16.10 15 -1 6 -7.09 9.07 15 -1 7 140.28 17.73 15 1 7 129.71 18.91 15 1 8 28.41 10.99 15 -1 8 3.28 7.98 15 1 9 52.12 12.57 15 -1 9 37.64 11.28 15 -1 10 49.42 12.81 15 1 10 34.32 12.78 -15 -3 12 26.79 9.49 15 -3 -12 34.40 11.17 15 3 -12 12.95 6.27 -15 -3 11 8.59 7.01 15 -3 -11 10.43 5.92 15 3 -11 26.00 8.98 15 3 -10 32.73 9.44 -15 -3 10 34.33 10.33 15 -3 -10 19.91 7.67 15 3 -9 57.13 10.54 -15 -3 9 52.23 12.15 15 -3 -9 46.95 10.20 15 3 -8 19.95 7.03 -15 -3 8 30.85 10.79 15 -3 -8 21.67 5.96 15 3 -7 24.54 7.90 15 -3 -7 34.64 8.73 15 3 -6 15.70 7.00 15 -3 -6 11.11 7.30 15 -3 -5 59.44 17.39 15 3 -5 54.53 9.40 15 3 -4 8.75 6.20 15 -3 -4 21.31 7.53 15 -3 -3 7.53 5.37 15 3 -3 6.10 5.64 15 -3 -2 195.52 17.90 15 3 -2 167.45 17.70 15 3 -1 282.11 22.33 15 -3 -1 248.80 19.93 15 3 0 416.33 28.10 15 -3 0 367.97 24.09 15 3 1 373.45 27.19 15 -3 1 337.09 24.22 15 3 2 564.54 34.04 15 -3 2 545.26 28.74 15 3 3 481.85 32.40 15 -3 3 431.31 26.90 15 3 4 429.30 30.99 15 -3 4 408.46 26.33 15 3 5 280.80 25.88 15 -3 5 288.79 22.02 15 3 6 183.37 22.94 15 -3 6 172.17 16.67 15 3 7 213.53 23.64 15 -3 7 216.78 19.89 15 3 8 130.91 20.35 15 -3 8 115.94 14.88 15 -3 9 32.98 9.92 15 3 9 51.85 15.11 15 -5 -8 61.67 14.47 -15 -5 8 78.29 14.74 15 -5 -7 253.01 21.59 -15 -5 7 238.18 24.37 15 5 -7 203.34 18.53 -15 -5 6 26.67 11.31 15 -5 -6 41.43 9.87 15 5 -6 39.82 9.19 15 -5 -5 86.92 14.37 -15 -5 5 118.09 16.87 15 5 -5 102.17 14.41 15 5 -4 7.13 7.46 15 -5 -4 24.07 7.56 15 -5 -3 53.27 9.36 15 5 -3 45.61 11.38 15 5 -2 12.56 7.99 15 -5 -2 15.06 7.07 15 -5 -1 -1.84 5.40 15 5 -1 7.32 7.52 15 5 0 53.07 11.75 15 -5 0 29.95 8.78 15 -5 1 15.33 8.44 15 5 1 10.07 7.58 15 -5 2 82.19 12.63 15 5 2 100.63 15.75 15 -5 3 7.73 5.61 15 5 3 -0.04 6.80 15 -5 4 152.56 16.07 15 5 4 235.96 24.31 15 -5 5 1.10 4.90 15 5 5 4.32 8.61 16 0 -12 78.66 12.23 16 0 -11 1.27 6.21 16 0 -10 445.11 28.20 16 0 -9 8.24 7.83 16 0 -8 634.76 30.99 16 0 -7 1.17 5.17 16 0 -6 1418.51 46.67 16 0 -5 12.01 7.73 16 0 -4 2452.97 61.71 16 0 -3 -4.49 5.74 16 0 -2 9.51 6.54 16 0 -1 1.87 5.33 16 0 0 146.90 17.26 16 0 1 -6.13 6.86 16 0 2 19.54 7.91 16 0 3 -0.82 6.32 16 0 4 15.19 9.63 16 0 5 0.99 6.78 16 0 6 298.41 27.25 16 0 7 -7.69 8.08 16 0 8 44.48 13.40 16 0 9 3.89 8.44 16 -2 -12 5.35 6.45 16 2 -12 7.94 5.79 16 -2 -11 29.47 9.14 16 2 -11 22.68 7.90 16 -2 -10 88.00 12.11 16 2 -10 119.70 15.57 16 2 -9 50.51 9.78 16 -2 -9 58.52 11.39 16 2 -8 16.67 6.66 16 -2 -8 24.94 9.04 16 -2 -7 352.11 28.97 16 2 -7 254.37 20.10 16 -2 -6 53.00 10.90 16 2 -6 67.57 10.60 16 -2 -5 235.41 19.83 16 2 -5 263.90 20.42 16 -2 -4 100.16 13.85 16 2 -4 91.97 12.88 16 -2 -3 163.61 17.26 16 2 -3 183.25 17.97 16 -2 -2 257.74 21.31 16 2 -2 263.80 22.94 16 2 -1 2.76 7.87 16 -2 -1 14.43 7.47 16 2 0 125.46 16.54 16 -2 0 128.58 15.56 16 2 1 88.70 14.19 16 -2 1 85.16 13.26 16 2 2 117.12 16.84 16 -2 2 121.09 15.75 16 2 3 252.06 24.16 16 -2 3 231.27 21.17 16 -2 4 56.46 12.17 16 2 4 70.61 14.38 16 2 5 683.94 41.50 16 -2 5 626.54 35.60 16 2 6 40.15 11.28 16 -2 6 42.09 9.79 16 2 7 491.45 37.18 16 -2 7 445.72 29.93 16 2 8 49.89 13.47 16 -2 8 46.42 11.64 16 4 -9 41.91 9.97 -16 -4 9 56.88 13.39 16 -4 -9 37.22 9.98 16 -4 -8 126.79 16.98 -16 -4 8 160.93 20.67 16 4 -8 113.17 14.90 16 4 -7 62.01 11.46 16 -4 -7 38.81 9.47 16 -4 -6 119.83 13.92 16 4 -6 166.13 17.30 16 -4 -5 19.31 9.43 16 4 -5 16.79 7.27 16 4 -4 55.70 11.67 16 -4 -4 38.13 9.96 16 -4 -3 21.29 11.34 16 4 -3 18.03 8.49 16 -4 -2 46.17 10.35 16 4 -2 47.80 11.29 16 -4 -1 29.01 8.87 16 4 -1 24.87 9.49 16 -4 0 14.64 7.45 16 4 0 6.83 7.67 16 4 1 44.73 12.51 16 -4 1 20.44 7.75 16 4 2 126.13 18.36 16 -4 2 117.56 15.28 16 4 3 25.98 10.72 16 -4 3 18.82 6.31 16 4 4 335.59 29.67 16 -4 4 277.84 22.68 16 4 5 21.36 11.88 16 -4 5 6.83 6.12 16 4 6 273.40 28.47 16 -4 6 244.74 20.50 17 -1 -11 13.26 5.28 17 1 -11 22.88 7.69 17 1 -10 31.78 13.18 17 -1 -10 19.12 8.02 17 1 -9 19.53 7.70 17 -1 -9 11.59 6.62 17 -1 -8 406.62 32.33 17 1 -8 291.62 23.12 17 -1 -7 23.92 9.14 17 1 -7 26.08 9.15 17 -1 -6 436.79 28.39 17 1 -6 434.86 27.22 17 -1 -5 62.95 11.18 17 1 -5 57.19 10.29 17 -1 -4 642.24 33.59 17 1 -4 662.13 34.61 17 -1 -3 92.67 13.42 17 1 -3 103.23 14.02 17 -1 -2 405.41 26.95 17 1 -2 417.94 28.33 17 -1 -1 531.06 31.17 17 1 -1 496.96 31.23 17 -1 0 799.84 38.83 17 1 0 784.82 40.01 17 1 1 4.03 6.62 17 -1 1 4.92 6.17 17 1 2 289.73 25.69 17 -1 2 299.93 24.10 17 1 3 68.90 13.86 17 -1 3 80.01 14.17 17 -1 4 5.02 7.74 17 1 4 7.07 8.23 17 -1 5 86.83 15.97 17 1 5 81.54 16.45 17 1 6 20.86 10.22 17 -1 6 25.80 10.58 17 -1 7 86.96 16.02 17 1 7 104.82 19.22 17 1 8 -3.58 9.53 17 -1 8 14.64 9.76 17 3 -9 41.72 11.74 17 -3 -9 21.60 7.91 17 3 -8 5.73 6.70 17 -3 -8 4.98 4.57 17 3 -7 14.66 7.08 17 -3 -7 19.24 7.93 17 3 -6 23.82 9.17 17 -3 -6 34.14 10.41 17 -3 -5 62.59 14.98 17 3 -5 69.48 12.28 17 -3 -4 1.19 6.36 17 3 -4 4.81 5.36 17 -3 -3 8.42 7.51 17 3 -3 3.38 5.74 17 -3 -2 138.23 17.23 17 3 -2 152.07 16.92 17 -3 -1 29.93 9.40 17 3 -1 41.88 11.50 17 -3 0 6.49 5.71 17 3 0 6.11 8.23 17 -3 1 -1.86 6.31 17 3 1 -0.88 6.99 17 -3 2 28.45 9.16 17 3 2 29.37 10.47 17 3 3 1.69 8.19 17 -3 3 1.91 6.08 17 3 4 91.83 17.15 17 -3 4 75.95 13.71 17 3 5 108.51 18.04 17 -3 5 75.98 12.75 17 3 6 135.87 21.03 17 -3 6 129.63 16.56 18 0 -10 14.88 7.46 18 0 -9 -2.58 8.72 18 0 -8 44.41 10.27 18 0 -7 -8.65 6.56 18 0 -6 252.03 22.04 18 0 -5 6.31 6.70 18 0 -4 620.66 34.37 18 0 -3 -0.97 6.16 18 0 -2 975.76 45.09 18 0 -1 -2.40 8.49 18 0 0 786.88 40.78 18 0 1 -1.47 6.93 18 0 2 649.29 38.86 18 0 3 5.89 8.71 18 0 4 585.51 37.51 18 0 5 5.76 9.92 18 0 6 25.17 11.59 18 -2 -9 121.37 16.25 18 2 -9 118.24 15.60 18 2 -8 44.45 12.09 18 -2 -8 52.53 10.73 18 -2 -7 67.68 19.83 18 2 -7 23.41 8.59 18 -2 -6 4.38 7.26 18 2 -6 27.56 9.27 18 -2 -5 8.99 6.22 18 2 -5 21.29 8.76 18 -2 -4 10.24 6.53 18 2 -4 1.77 6.40 18 -2 -3 311.00 25.14 18 2 -3 304.34 25.77 18 -2 -2 364.34 26.38 18 2 -2 312.17 26.36 18 -2 -1 124.13 17.31 18 2 -1 138.64 18.80 18 2 0 54.68 12.95 18 -2 0 105.16 15.43 18 -2 1 153.55 18.35 18 2 1 152.67 20.24 18 -2 2 40.38 11.18 18 2 2 32.53 10.59 18 -2 3 55.74 12.15 18 2 3 65.42 15.94 18 -2 4 11.36 7.18 18 2 4 20.11 11.40 18 2 5 0.11 9.76 18 -2 5 -5.04 7.20 18 4 -4 46.69 11.89 18 -4 -4 34.36 10.96 18 -4 -3 123.66 23.13 18 4 -3 51.25 12.01 18 -4 -2 194.03 22.94 18 4 -2 197.85 23.01 18 -4 -1 19.46 9.69 18 4 -1 49.05 13.65 18 -4 0 26.90 9.60 18 4 0 31.01 11.01 18 -4 1 13.39 8.61 18 4 1 14.71 10.59 19 -1 -8 0.57 9.07 19 1 -8 2.07 5.92 19 -1 -7 91.76 14.74 19 1 -7 92.20 14.03 19 -1 -6 15.60 7.78 19 1 -6 18.76 8.97 19 -1 -5 15.21 7.58 19 1 -5 33.45 10.05 19 -1 -4 58.97 12.77 19 1 -4 54.10 12.58 19 -1 -3 -13.70 9.73 19 1 -3 12.69 8.44 19 -1 -2 224.44 22.33 19 1 -2 241.29 23.41 19 -1 -1 130.64 18.27 19 1 -1 184.57 20.72 19 -1 0 349.52 28.81 19 1 0 345.56 29.30 19 1 1 104.17 16.19 19 -1 1 110.78 16.98 19 -1 2 390.59 32.22 19 1 2 456.72 34.91 19 -1 3 51.16 14.21 19 1 3 42.57 11.71 19 1 4 469.69 37.14 19 -1 4 406.77 32.74 19 -3 -5 41.18 14.64 19 3 -5 37.09 9.17 19 -3 -4 2.41 6.73 19 3 -4 1.53 7.43 19 3 -3 3.88 7.09 19 -3 -3 12.44 7.99 19 3 -2 32.25 11.86 19 -3 -2 15.60 8.93 19 -3 -1 37.17 11.20 19 3 -1 22.38 10.01 19 -3 0 58.48 12.53 19 3 0 55.93 13.88 19 -3 1 68.92 14.18 19 3 1 85.67 17.07 20 0 -6 7.14 7.70 20 0 -5 -4.72 6.58 20 0 -4 -4.85 6.92 20 0 -3 -10.38 8.57 20 0 -2 1.19 7.27 20 0 -1 17.02 10.93 20 0 0 166.72 21.30 20 0 1 -0.94 8.06 20 0 2 470.92 36.43 20 -2 -3 96.21 16.45 20 2 -3 83.59 15.02 20 -2 -2 54.05 14.08 20 2 -2 62.38 14.55 20 2 -1 7.13 8.54 20 -2 -1 14.05 10.47 0 0 0 0.00 0.00 TITL x208b WL in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 17.109513 7.201971 14.953356 90.0000 96.4721 90.0000 ZERR 8.00 0.001039 0.000572 0.001140 0.0000 0.0062 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 11987 _shelx_res_file ; TITL x208b_a.res in C2/c x208b.res created by SHELXL-2018/3 at 13:39:28 on 01-Nov-2024 REM Old TITL x208b WL in C2/c REM SHELXT solution in C2/c REM R1 0.138, Rweak 0.078, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C18 N2 O2 Br3 CELL 0.71073 17.1095 7.202 14.9534 90 96.472 90 ZERR 4 0.001 0.0006 0.0011 0 0.006 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Br N O Zn UNIT 72 56 8 8 8 4 L.S. 10 PLAN 1 TEMP -103.15 CONF BOND $H list 4 fmap 2 acta MORE -1 REM REM REM WGHT 0.092700 FVAR 0.27747 BR1 3 0.609545 0.375048 0.210970 11.00000 0.02764 0.05359 = 0.03007 -0.00431 0.00414 0.00966 ZN1 6 0.500000 0.539983 0.250000 10.50000 0.02000 0.03926 = 0.02372 0.00000 0.00321 0.00000 O1 5 0.536908 0.714992 0.349304 11.00000 0.01890 0.05332 = 0.03708 -0.01347 0.00596 0.00358 N1 4 0.480999 0.774066 0.399901 11.00000 0.02079 0.03714 = 0.02991 -0.00771 0.00324 -0.00152 C2 1 0.355953 0.908811 0.414823 11.00000 0.02306 0.03065 = 0.02783 0.00327 -0.00014 -0.00239 C7 1 0.370370 0.884557 0.508859 11.00000 0.02632 0.03459 = 0.03108 -0.00418 0.00365 -0.00550 C1 1 0.415743 0.851676 0.362147 11.00000 0.02507 0.03778 = 0.02425 0.00031 -0.00086 -0.00387 AFIX 43 H1 2 0.408573 0.869682 0.298816 11.00000 -1.20000 AFIX 0 C3 1 0.284792 0.982920 0.374984 11.00000 0.02640 0.03809 = 0.04240 0.00187 0.00329 -0.00434 AFIX 43 H3 2 0.275439 0.998479 0.311593 11.00000 -1.20000 AFIX 0 C9 1 0.496039 0.750304 0.491855 11.00000 0.02721 0.04199 = 0.03165 0.00250 -0.00382 -0.00254 AFIX 43 H9 2 0.544037 0.695474 0.517045 11.00000 -1.20000 AFIX 0 C4 1 0.228944 1.032525 0.429244 11.00000 0.02311 0.03885 = 0.05554 0.00246 0.00294 -0.00017 AFIX 43 H4 2 0.180142 1.081746 0.403055 11.00000 -1.20000 AFIX 0 C8 1 0.442636 0.804920 0.545426 11.00000 0.03824 0.03321 = 0.02425 0.00413 -0.00492 -0.00095 AFIX 43 H8 2 0.453412 0.790004 0.608739 11.00000 -1.20000 AFIX 0 C6 1 0.310805 0.941289 0.562677 11.00000 0.04193 0.03682 = 0.03863 -0.00769 0.01501 -0.00681 AFIX 43 H6 2 0.319011 0.929530 0.626322 11.00000 -1.20000 AFIX 0 C5 1 0.242632 1.011886 0.522194 11.00000 0.02840 0.04284 = 0.06541 -0.01052 0.02201 -0.00202 AFIX 43 H5 2 0.202956 1.048433 0.558206 11.00000 -1.20000 AFIX 0 HKLF 4 REM x208b_a.res in C2/c REM wR2 = 0.1407, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0519 for 1402 Fo > 4sig(Fo) and 0.0604 for all 1671 data REM 114 parameters refined using 0 restraints END WGHT 0.0926 0.0000 REM Highest difference peak 0.830, deepest hole -0.960, 1-sigma level 0.168 Q1 1 0.6509 0.4902 0.2208 11.00000 0.05 0.80 ; _shelx_res_checksum 81828 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Br Br1 0.60954(3) 0.37505(9) 0.21097(4) 0.0370(3) Uani d 1 . . Zn Zn1 0.500000 0.53998(12) 0.250000 0.0276(3) Uani d 1 . . O O1 0.5369(2) 0.7150(6) 0.3493(3) 0.0362(9) Uani d 1 . . N N1 0.4810(2) 0.7741(6) 0.3999(3) 0.0293(10) Uani d 1 . . C C2 0.3560(3) 0.9088(7) 0.4148(4) 0.0274(12) Uani d 1 . . C C7 0.3704(3) 0.8846(7) 0.5089(4) 0.0306(13) Uani d 1 . . C C1 0.4157(3) 0.8517(7) 0.3621(4) 0.0293(12) Uani d 1 . . H H1 0.408573 0.869682 0.298816 0.035 Uiso calc 1 . . C C3 0.2848(3) 0.9829(8) 0.3750(5) 0.0357(13) Uani d 1 . . H H3 0.275439 0.998479 0.311593 0.043 Uiso calc 1 . . C C9 0.4960(3) 0.7503(8) 0.4919(4) 0.0342(13) Uani d 1 . . H H9 0.544037 0.695474 0.517045 0.041 Uiso calc 1 . . C C4 0.2289(3) 1.0325(8) 0.4292(5) 0.0393(15) Uani d 1 . . H H4 0.180142 1.081746 0.403055 0.047 Uiso calc 1 . . C C8 0.4426(3) 0.8049(7) 0.5454(4) 0.0325(12) Uani d 1 . . H H8 0.453412 0.790004 0.608739 0.039 Uiso calc 1 . . C C6 0.3108(4) 0.9413(8) 0.5627(5) 0.0383(14) Uani d 1 . . H H6 0.319011 0.929530 0.626322 0.046 Uiso calc 1 . . C C5 0.2426(4) 1.0119(8) 0.5222(5) 0.0443(17) Uani d 1 . . H H5 0.202956 1.048433 0.558206 0.053 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0276(4) 0.0536(4) 0.0301(4) 0.0097(2) 0.0041(2) -0.0043(3) Zn1 0.0200(5) 0.0393(5) 0.0237(5) 0.000 0.0032(3) 0.000 O1 0.0189(18) 0.053(2) 0.037(2) 0.0036(17) 0.0060(15) -0.013(2) N1 0.021(2) 0.037(2) 0.030(3) -0.0015(18) 0.0032(17) -0.008(2) C2 0.023(3) 0.031(3) 0.028(3) -0.002(2) 0.000(2) 0.003(2) C7 0.026(3) 0.035(3) 0.031(3) -0.006(2) 0.004(2) -0.004(2) C1 0.025(3) 0.038(3) 0.024(3) -0.004(2) -0.001(2) 0.000(2) C3 0.026(3) 0.038(3) 0.042(4) -0.004(2) 0.003(2) 0.002(3) C9 0.027(3) 0.042(3) 0.032(3) -0.003(2) -0.004(2) 0.003(3) C4 0.023(3) 0.039(3) 0.056(4) 0.000(2) 0.003(3) 0.002(3) C8 0.038(3) 0.033(3) 0.024(3) -0.001(2) -0.005(2) 0.004(3) C6 0.042(4) 0.037(3) 0.039(4) -0.007(3) 0.015(3) -0.008(3) C5 0.028(3) 0.043(3) 0.065(5) -0.002(2) 0.022(3) -0.011(3) 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' Br Br -0.2901 2.4595 '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' Zn Zn 0.2839 1.4301 '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 Br1 Zn1 Br1 . 2_655 119.21(5) ? O1 Zn1 Br1 . . 108.06(10) ? O1 Zn1 Br1 2_655 2_655 108.06(10) ? O1 Zn1 Br1 . 2_655 109.22(11) ? O1 Zn1 Br1 2_655 . 109.22(11) ? O1 Zn1 O1 . 2_655 101.6(3) ? N1 O1 Zn1 . . 115.5(3) ? O1 N1 C9 . . 117.0(4) ? C1 N1 O1 . . 120.8(5) ? C1 N1 C9 . . 122.2(5) ? C7 C2 C1 . . 117.4(5) ? C3 C2 C7 . . 121.2(5) ? C3 C2 C1 . . 121.4(5) ? C2 C7 C8 . . 118.8(5) ? C2 C7 C6 . . 118.1(5) ? C8 C7 C6 . . 123.1(6) ? N1 C1 C2 . . 120.9(5) ? N1 C1 H1 . . 119.5 ? C2 C1 H1 . . 119.5 ? C2 C3 H3 . . 120.7 ? C4 C3 C2 . . 118.6(6) ? C4 C3 H3 . . 120.7 ? N1 C9 H9 . . 120.1 ? C8 C9 N1 . . 119.7(5) ? C8 C9 H9 . . 120.1 ? C3 C4 H4 . . 119.5 ? C3 C4 C5 . . 120.9(6) ? C5 C4 H4 . . 119.5 ? C7 C8 H8 . . 119.6 ? C9 C8 C7 . . 120.8(6) ? C9 C8 H8 . . 119.6 ? C7 C6 H6 . . 120.3 ? C5 C6 C7 . . 119.3(6) ? C5 C6 H6 . . 120.3 ? C4 C5 H5 . . 119.1 ? C6 C5 C4 . . 121.8(6) ? C6 C5 H5 . . 119.1 ? 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 Zn1 Br1 . 2.3476(7) ? Zn1 Br1 2_655 2.3476(7) ? Zn1 O1 . 1.995(4) ? Zn1 O1 2_655 1.995(4) ? O1 N1 . 1.353(5) ? N1 C1 . 1.317(7) ? N1 C9 . 1.381(8) ? C2 C7 . 1.411(8) ? C2 C1 . 1.421(8) ? C2 C3 . 1.400(8) ? C7 C8 . 1.416(8) ? C7 C6 . 1.428(8) ? C1 H1 . 0.9500 ? C3 H3 . 0.9500 ? C3 C4 . 1.369(8) ? C9 H9 . 0.9500 ? C9 C8 . 1.340(8) ? C4 H4 . 0.9500 ? C4 C5 . 1.391(10) ? C8 H8 . 0.9500 ? C6 H6 . 0.9500 ? C6 C5 . 1.351(9) ? C5 H5 . 0.9500 ? 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 Zn1 O1 N1 C1 . . . . -54.2(6) ? Zn1 O1 N1 C9 . . . . 126.2(4) ? O1 N1 C1 C2 . . . . 178.1(4) ? O1 N1 C9 C8 . . . . -179.5(5) ? N1 C9 C8 C7 . . . . 0.9(8) ? C2 C7 C8 C9 . . . . -1.2(8) ? C2 C7 C6 C5 . . . . 1.4(8) ? C2 C3 C4 C5 . . . . 0.7(9) ? C7 C2 C1 N1 . . . . 2.0(8) ? C7 C2 C3 C4 . . . . 0.2(8) ? C7 C6 C5 C4 . . . . -0.6(9) ? C1 N1 C9 C8 . . . . 0.9(8) ? C1 C2 C7 C8 . . . . -0.2(7) ? C1 C2 C7 C6 . . . . -180.0(5) ? C1 C2 C3 C4 . . . . 178.9(5) ? C3 C2 C7 C8 . . . . 178.5(5) ? C3 C2 C7 C6 . . . . -1.2(8) ? C3 C2 C1 N1 . . . . -176.8(5) ? C3 C4 C5 C6 . . . . -0.5(10) ? C9 N1 C1 C2 . . . . -2.4(8) ? C8 C7 C6 C5 . . . . -178.4(6) ? C6 C7 C8 C9 . . . . 178.6(5) ?