#------------------------------------------------------------------------------ #$Date: 2025-02-08 05:10:10 +0200 (Sat, 08 Feb 2025) $ #$Revision: 297642 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573866.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_1573866 loop_ _publ_author_name 'Albert, Daniel R.' 'Gau, Michael' 'Rajaseelan, Edward' _publ_section_title ; 4-(4-tert-Butylbenzyl)-1-neopentyl-1,2,4-triazolium bromide ; _journal_coeditor_code HB4505 _journal_issue 2 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314625000926 _journal_volume 10 _journal_year 2025 _chemical_formula_iupac 'C18 H28 N3 +, Br -' _chemical_formula_moiety 'C18 H28 N3 +, Br -' _chemical_formula_sum 'C18 H28 Br N3' _chemical_formula_weight 366.34 _chemical_name_systematic ; 4-(4-tert-Butylbenzyl)-1-neopentyl-1,2,4-triazolium bromide ; _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yc' _space_group_name_H-M_alt 'P 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 90.4350(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.9741(2) _cell_length_b 6.38420(10) _cell_length_c 10.07410(10) _cell_measurement_reflns_used 11602 _cell_measurement_temperature 100 _cell_measurement_theta_max 74.3920 _cell_measurement_theta_min 2.9120 _cell_volume 963.03(2) _computing_cell_refinement ; CrysAlisPro 1.171.43.134a (Rigaku OD, 2024) ; _computing_data_collection ; CrysAlisPro 1.171.43.134a (Rigaku OD, 2024) ; _computing_data_reduction ; CrysAlisPro 1.171.43.134a (Rigaku OD, 2024) ; _computing_molecular_graphics ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_publication_material ; PublCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_unetI/netI 0.0437 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 14617 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.473 _diffrn_reflns_theta_min 2.951 _exptl_absorpt_coefficient_mu 2.898 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.67545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SCALE3 ABSPACK in CrysAlis PRO (Rigaku OD, 2024)] ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.263 _exptl_crystal_description needle _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.766 _refine_diff_density_min -0.869 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.31(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 206 _refine_ls_number_reflns 3683 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.147 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0428 _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^)+(0.0959P)^2^+0.2583P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1149 _refine_ls_wR_factor_ref 0.1354 _reflns_number_gt 3564 _reflns_number_total 3683 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb4505.cif _cod_data_source_block I _cod_database_code 1573866 _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 ; -18 0 -3 1.17 2.09 -18 0 -2 87.92 6.30 -18 0 -2 90.63 6.38 -18 0 -1 1.09 2.97 -18 0 -1 -0.14 2.79 -18 0 0 42.96 5.03 -18 0 0 31.81 4.48 -18 0 1 -0.72 3.35 -18 0 1 -1.44 3.13 -18 0 1 0.87 2.81 -18 0 2 104.70 7.19 -18 0 2 89.80 6.87 -18 0 2 102.51 7.17 -18 0 3 0.44 2.75 -18 0 3 0.45 2.23 -18 0 3 -0.92 2.54 -18 1 -2 32.25 3.07 -18 -1 -2 38.15 4.16 -18 1 -2 35.86 4.02 -18 -1 -2 32.67 3.17 -18 1 -2 28.44 3.54 -18 1 -1 15.32 3.19 -18 -1 -1 16.21 2.89 -18 1 -1 17.25 3.49 -18 1 -1 20.69 3.20 -18 -1 -1 14.17 3.55 -18 1 0 80.00 5.69 -18 -1 0 90.16 6.67 -18 1 0 84.23 6.49 -18 -1 0 72.51 5.44 -18 1 0 64.12 5.88 -18 1 1 6.47 2.76 -18 1 1 6.79 3.11 -18 -1 1 5.12 2.44 -18 1 1 2.46 2.65 -18 1 2 58.96 5.25 -18 1 2 72.62 5.64 -18 1 2 77.22 5.16 -18 1 2 72.57 5.20 -18 1 3 23.80 3.29 -18 1 3 28.48 3.10 -18 1 3 33.59 3.52 -18 1 3 29.02 3.76 -18 -2 -1 3.74 2.32 -18 2 -1 5.68 2.03 -18 -2 0 19.70 2.98 -18 2 0 16.07 2.86 -18 2 1 103.07 6.28 -18 -2 1 103.72 6.17 -17 0 -4 80.16 9.02 -17 0 -3 -0.16 3.55 -17 0 -3 -2.33 2.41 -17 0 -2 48.63 5.50 -17 0 -2 36.33 8.14 -17 0 -1 0.19 3.21 -17 0 -1 1.24 4.43 -17 0 -1 -1.47 4.47 -17 0 -1 5.33 6.03 -17 0 0 45.24 5.99 -17 0 0 62.60 7.25 -17 0 0 72.05 7.44 -17 0 0 70.64 7.17 -17 0 1 -0.19 3.39 -17 0 1 0.44 4.01 -17 0 1 5.99 4.91 -17 0 1 1.08 4.59 -17 0 2 70.53 7.48 -17 0 2 77.76 7.72 -17 0 2 83.60 7.85 -17 0 3 -2.20 4.27 -17 0 3 1.95 3.76 -17 0 3 3.03 4.17 -17 0 4 139.54 9.28 -17 0 4 146.34 9.56 -17 0 4 150.07 9.50 -17 0 5 1.22 2.85 -17 0 5 -1.93 2.58 -17 0 5 2.81 2.64 -17 -1 -4 65.99 4.99 -17 1 -4 74.84 5.71 -17 1 -4 59.00 5.28 -17 1 -3 21.16 4.25 -17 1 -3 34.15 4.15 -17 -1 -3 29.66 4.82 -17 1 -3 25.26 4.39 -17 -1 -3 33.84 4.12 -17 -1 -3 21.45 6.58 -17 1 -2 118.71 8.97 -17 -1 -2 143.08 9.41 -17 1 -2 143.50 8.61 -17 1 -2 136.24 9.22 -17 -1 -2 90.64 11.44 -17 -1 -2 151.44 8.89 -17 -1 -2 71.84 7.91 -17 1 -1 36.52 5.32 -17 1 -1 29.17 5.22 -17 -1 -1 25.14 7.31 -17 1 -1 31.85 5.38 -17 -1 -1 36.61 4.89 -17 -1 -1 42.30 6.04 -17 1 0 80.63 7.84 -17 1 0 90.71 8.22 -17 -1 0 83.50 7.30 -17 1 0 93.59 7.66 -17 1 0 97.58 8.16 -17 1 1 12.10 4.38 -17 1 1 12.60 4.53 -17 -1 1 10.96 4.04 -17 1 1 9.44 4.27 -17 1 1 13.55 4.73 -17 1 2 78.02 7.13 -17 1 2 85.60 7.41 -17 -1 2 68.01 6.67 -17 1 2 68.62 7.48 -17 1 3 157.95 9.60 -17 1 3 150.46 9.59 -17 1 3 137.20 9.92 -17 -1 3 143.93 9.17 -17 1 4 141.93 8.48 -17 -1 4 124.08 8.08 -17 1 4 140.06 9.26 -17 1 4 155.85 8.98 -17 -1 4 158.06 9.17 -17 1 5 23.67 3.62 -17 -1 5 21.95 3.46 -17 1 5 24.22 3.44 -17 -1 5 26.15 3.41 -17 2 -4 59.11 4.25 -17 2 -3 15.37 3.14 -17 -2 -3 9.36 2.71 -17 -2 -3 19.39 3.63 -17 -2 -2 55.12 4.94 -17 2 -2 77.77 6.77 -17 -2 -2 88.35 6.75 -17 2 -2 81.20 6.30 -17 -2 -2 70.03 8.49 -17 -2 -2 62.08 6.84 -17 2 -1 44.06 5.63 -17 -2 -1 29.61 4.08 -17 -2 -1 49.64 5.33 -17 2 -1 42.28 5.19 -17 -2 -1 27.77 6.36 -17 -2 0 35.95 4.66 -17 -2 0 52.32 5.52 -17 -2 0 44.61 5.45 -17 2 0 56.54 5.84 -17 2 0 45.61 5.87 -17 2 1 109.62 8.72 -17 2 1 113.86 7.01 -17 -2 1 119.66 8.25 -17 2 1 125.72 8.57 -17 -2 1 124.15 8.47 -17 -2 2 62.71 6.06 -17 2 2 60.93 6.37 -17 -2 2 75.56 6.16 -17 2 2 69.48 5.11 -17 2 2 63.69 6.30 -17 -2 3 60.05 5.41 -17 2 3 59.31 5.74 -17 2 3 56.72 4.43 -17 -2 3 63.52 5.25 -17 -2 4 10.51 2.75 -17 2 4 9.65 2.87 -17 -2 4 12.24 2.07 -17 3 -2 16.08 2.86 -17 -3 -2 13.13 2.36 -17 -3 -2 13.65 3.24 -17 -3 -1 70.43 5.39 -17 -3 -1 73.16 6.84 -17 3 -1 82.69 6.06 -17 3 0 38.93 4.46 -17 -3 0 32.90 3.82 -17 -3 1 13.32 2.87 -17 3 1 15.58 3.36 -17 -3 2 10.95 2.65 -17 3 2 11.31 2.88 -16 0 -5 -1.19 2.52 -16 0 -4 90.59 7.54 -16 0 -4 111.29 8.45 -16 0 -3 -1.15 4.50 -16 0 -3 -0.86 3.44 -16 0 -2 8.93 4.58 -16 0 -2 10.45 5.46 -16 0 -2 17.84 6.04 -16 0 -1 -1.56 4.14 -16 0 -1 -0.81 5.17 -16 0 -1 0.81 5.33 -16 0 0 464.82 21.82 -16 0 0 440.10 21.49 -16 0 1 -1.41 5.49 -16 0 1 5.83 5.72 -16 0 2 221.41 14.93 -16 0 2 232.14 15.09 -16 0 2 224.15 15.07 -16 0 3 0.52 5.03 -16 0 3 -0.51 5.27 -16 0 3 0.27 4.87 -16 0 4 317.19 17.16 -16 0 4 284.76 16.83 -16 0 4 302.77 16.85 -16 0 5 -1.77 4.13 -16 0 5 -1.13 4.07 -16 0 5 2.20 3.72 -16 0 6 205.07 11.01 -16 0 6 188.23 10.52 -16 0 6 174.69 10.60 -16 1 -6 54.13 4.51 -16 1 -6 47.14 4.17 -16 -1 -5 43.67 4.48 -16 1 -5 37.28 4.77 -16 1 -5 36.68 4.68 -16 1 -4 80.98 7.34 -16 -1 -4 93.94 7.86 -16 1 -4 96.15 6.97 -16 1 -4 81.01 7.42 -16 -1 -4 83.34 6.95 -16 1 -3 11.71 4.59 -16 -1 -3 9.43 4.87 -16 1 -3 15.09 4.50 -16 -1 -3 10.14 4.25 -16 1 -3 18.25 4.94 -16 -1 -3 12.42 8.02 -16 1 -2 137.51 10.00 -16 -1 -2 146.57 11.08 -16 1 -2 139.37 10.81 -16 -1 -2 140.75 10.20 -16 1 -2 111.03 10.20 -16 -1 -1 54.57 6.30 -16 1 -1 68.48 8.24 -16 1 -1 63.64 8.21 -16 -1 -1 66.84 7.56 -16 1 -1 74.37 8.44 -16 -1 -1 75.23 8.61 -16 1 -1 74.50 7.87 -16 1 0 61.00 7.73 -16 -1 0 59.58 7.32 -16 1 0 65.74 8.45 -16 -1 0 48.03 9.61 -16 1 0 67.08 8.15 -16 1 1 12.23 5.50 -16 -1 1 19.70 5.34 -16 1 1 13.27 5.79 -16 1 1 11.07 5.80 -16 1 2 184.62 12.54 -16 1 2 170.61 12.49 -16 1 2 183.98 13.19 -16 -1 2 165.89 12.05 -16 1 3 9.30 5.40 -16 1 3 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8.57 -16 2 1 85.58 7.50 -16 -2 1 64.78 8.95 -16 2 1 85.55 8.54 -16 2 2 44.98 5.78 -16 2 2 45.51 5.81 -16 -2 2 55.31 6.72 -16 2 2 41.30 6.34 -16 -2 2 46.36 6.31 -16 2 3 45.86 5.24 -16 -2 3 49.33 6.12 -16 2 3 48.05 5.79 -16 2 3 55.27 6.76 -16 -2 3 43.38 6.24 -16 2 4 58.88 5.73 -16 -2 4 53.18 5.78 -16 2 4 55.75 6.41 -16 -2 4 52.09 5.97 -16 -2 5 52.87 4.45 -16 2 5 67.04 5.13 -16 2 5 48.93 5.46 -16 -2 5 55.45 5.49 -16 -3 -4 31.28 4.01 -16 -3 -4 25.47 4.14 -16 3 -4 34.46 3.74 -16 3 -3 44.14 5.06 -16 -3 -3 35.18 4.45 -16 -3 -3 41.86 6.70 -16 3 -3 39.35 3.61 -16 -3 -3 45.92 5.98 -16 3 -2 33.99 5.32 -16 -3 -2 36.30 4.77 -16 -3 -2 34.85 7.20 -16 -3 -2 38.82 4.66 -16 3 -2 37.92 4.23 -16 -3 -2 48.51 6.98 -16 -3 -1 67.95 6.74 -16 -3 -1 88.73 6.61 -16 -3 -1 77.58 9.11 -16 3 -1 65.30 5.92 -16 3 -1 75.02 7.24 -16 -3 0 16.22 5.75 -16 -3 0 21.22 4.04 -16 3 0 18.65 3.79 -16 -3 0 21.33 4.45 -16 3 0 21.49 5.13 -16 3 1 136.15 8.78 -16 3 1 133.66 9.93 -16 3 2 5.18 2.95 -16 3 2 4.30 3.63 -16 3 3 133.34 8.00 -16 3 4 7.66 2.18 -16 -4 -1 35.43 5.04 -16 -4 -1 43.90 4.23 -16 4 0 19.85 2.80 -16 -4 0 32.54 3.76 -16 4 1 52.34 4.14 -16 -4 1 75.54 5.46 -15 0 -7 0.15 2.11 -15 0 -6 87.45 6.71 -15 0 -5 2.38 4.33 -15 0 -5 2.46 3.37 -15 0 -4 145.51 11.10 -15 0 -4 179.39 12.26 -15 0 -3 0.29 5.33 -15 0 -3 -2.80 4.22 -15 0 -2 281.60 17.08 -15 0 -2 255.42 16.53 -15 0 -1 -3.20 6.34 -15 0 -1 1.28 5.82 -15 0 -1 -2.53 4.52 -15 0 0 525.04 27.54 -15 0 0 540.91 27.73 -15 0 1 -2.31 6.62 -15 0 1 0.67 5.93 -15 0 2 57.92 9.03 -15 0 2 52.58 8.88 -15 0 3 -1.59 6.04 -15 0 3 -2.25 6.11 -15 0 4 127.41 11.69 -15 0 4 109.85 10.96 -15 0 4 139.56 11.87 -15 0 5 -5.77 5.67 -15 0 5 2.43 4.75 -15 0 5 -0.81 5.44 -15 0 6 227.11 13.48 -15 0 6 193.45 13.06 -15 0 6 224.58 13.78 -15 0 7 1.10 3.34 -15 0 7 6.04 3.57 -15 -1 -7 14.73 3.84 -15 1 -7 18.39 2.99 -15 1 -6 51.73 5.48 -15 1 -6 49.97 5.53 -15 -1 -6 54.14 5.11 -15 1 -5 5.16 4.02 -15 -1 -5 5.74 4.70 -15 -1 -5 8.14 3.86 -15 1 -5 5.38 4.03 -15 1 -4 87.52 8.00 -15 -1 -4 93.73 9.14 -15 -1 -4 85.52 8.27 -15 1 -4 93.69 8.88 -15 1 -4 84.26 8.73 -15 -1 -3 27.06 5.73 -15 1 -3 21.02 5.91 -15 -1 -3 25.59 6.49 -15 1 -3 27.13 5.84 -15 -1 -3 17.80 4.00 -15 1 -3 25.51 6.04 -15 -1 -3 19.69 4.47 -15 -1 -2 160.33 11.50 -15 1 -2 159.31 12.94 -15 -1 -2 131.34 10.77 -15 -1 -2 196.51 13.58 -15 1 -2 194.80 13.64 -15 1 -2 190.74 12.91 -15 -1 -2 182.85 13.51 -15 1 -2 147.14 12.72 -15 -1 -2 168.57 12.54 -15 1 -1 55.95 8.55 -15 1 -1 60.91 8.50 -15 -1 -1 55.82 8.47 -15 -1 -1 47.63 6.56 -15 -1 -1 64.59 8.87 -15 1 -1 57.00 7.88 -15 -1 -1 47.66 7.63 -15 1 -1 57.08 8.55 -15 1 0 125.48 11.06 -15 1 0 108.58 10.51 -15 -1 0 102.06 10.16 -15 1 0 100.81 10.85 -15 -1 0 83.38 8.65 -15 1 1 20.83 6.84 -15 -1 1 23.62 8.56 -15 -1 1 29.29 6.51 -15 1 1 33.22 7.56 -15 1 1 25.33 7.33 -15 1 2 277.36 17.73 -15 -1 2 271.30 17.32 -15 1 2 303.89 18.04 -15 1 2 256.55 17.87 -15 1 3 77.95 9.20 -15 1 3 82.47 9.46 -15 -1 3 79.29 9.01 -15 1 3 83.00 9.85 -15 -1 4 142.33 11.86 -15 1 4 149.84 11.98 -15 1 4 135.21 11.84 -15 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674.10 28.86 1 -2 -4 651.20 26.68 1 -2 -4 616.27 26.97 1 2 -4 605.38 26.40 1 -2 -3 428.94 17.17 1 -2 -3 427.80 17.16 1 -2 -3 485.03 18.71 1 2 -3 482.36 18.93 1 -2 -3 474.39 19.39 1 -2 -2 478.02 19.36 1 -2 -2 437.15 17.47 1 -2 -2 424.68 17.44 1 2 -2 428.96 17.58 1 -2 -2 438.74 16.97 1 -2 -2 452.60 18.06 1 -2 -1 1238.28 44.75 1 2 -1 1203.59 44.62 1 -2 -1 1101.94 46.81 1 -2 0 2268.00 84.70 1 -2 1 3162.23 117.61 1 -2 4 726.01 33.23 1 -2 4 606.32 28.64 1 -2 5 231.60 14.30 1 -2 6 692.24 37.11 1 -2 7 714.16 38.50 1 -2 7 621.69 33.26 1 -2 8 536.47 34.06 1 -2 8 519.22 29.28 1 -2 8 513.89 29.00 1 -2 9 240.54 19.12 1 -2 9 280.07 19.39 1 -2 9 283.34 19.23 1 -2 9 249.16 23.08 1 -2 10 201.34 16.07 1 -2 10 224.56 15.43 1 -2 11 71.82 8.58 1 2 11 60.17 6.76 1 -2 12 81.06 6.96 1 3 -11 137.02 8.76 1 -3 -11 136.41 12.06 1 -3 -11 115.24 13.29 1 -3 -11 91.57 10.71 1 -3 -11 117.44 12.09 1 -3 -10 99.27 14.40 1 -3 -10 101.25 13.85 1 -3 -10 90.84 9.51 1 3 -10 109.64 9.48 1 -3 -10 67.13 9.57 1 -3 -10 119.05 13.96 1 -3 -10 104.07 14.88 1 -3 -10 73.17 13.24 1 -3 -9 548.16 34.04 1 -3 -9 501.67 28.42 1 3 -9 535.46 26.76 1 -3 -9 472.52 25.55 1 -3 -9 493.61 34.38 1 -3 -9 457.94 34.31 1 -3 -8 13.45 9.10 1 -3 -8 6.03 8.99 1 -3 -8 17.99 6.78 1 -3 -8 10.31 4.98 1 3 -8 12.28 5.48 1 3 -8 12.23 5.76 1 -3 -8 9.31 8.86 1 -3 -7 669.71 40.51 1 -3 -7 793.70 40.28 1 -3 -7 673.40 33.84 1 -3 -7 542.85 31.27 1 -3 -7 619.48 35.54 1 -3 -7 661.21 31.68 1 3 -7 637.53 31.51 1 -3 -7 669.95 39.42 1 -3 -7 683.70 32.19 1 3 -7 702.81 34.76 1 -3 -6 16.74 6.08 1 -3 -6 11.19 5.93 1 3 -6 13.64 4.97 1 3 -6 13.54 5.13 1 -3 -6 19.48 4.67 1 -3 -6 23.84 9.11 1 -3 -6 10.03 4.57 1 -3 -6 12.44 6.93 1 3 -5 691.80 32.42 1 -3 -5 690.98 30.44 1 -3 -5 655.81 31.75 1 -3 -4 255.63 13.36 1 3 -4 269.13 15.09 1 -3 -4 244.22 15.35 1 -3 -3 1843.60 70.83 1 -3 -3 1771.88 74.26 1 -3 -3 1981.05 72.89 1 -3 -2 112.18 10.20 1 -3 -2 143.63 9.13 1 -3 -1 2934.30 118.66 1 -3 -1 3199.72 117.15 1 -3 0 326.03 15.50 1 -3 0 366.33 18.87 1 -3 1 104.72 10.83 1 -3 1 122.89 11.76 1 -3 2 53.94 7.00 1 -3 2 64.07 6.58 1 -3 2 53.51 8.62 1 -3 2 54.06 9.56 1 -3 3 1967.36 80.07 1 -3 3 1709.45 80.93 1 -3 4 231.24 15.02 1 -3 4 199.89 15.58 1 -3 5 983.30 41.21 1 -3 5 785.34 40.68 1 -3 6 75.92 9.01 1 -3 6 79.21 9.80 1 -3 6 75.72 10.75 1 -3 7 410.33 25.96 1 -3 7 399.43 24.44 1 -3 7 470.84 26.86 1 -3 8 7.49 8.25 1 -3 8 12.30 6.63 1 -3 8 10.25 6.47 1 -3 9 369.05 22.84 1 -3 9 335.11 21.51 1 -3 10 103.42 10.66 1 -3 10 73.94 9.17 1 -3 11 342.01 17.52 1 -4 -10 9.99 8.22 1 4 -10 15.75 3.61 1 -4 -10 17.61 7.98 1 -4 -10 20.86 8.43 1 -4 -9 156.20 19.43 1 4 -9 201.91 12.31 1 -4 -9 204.53 18.81 1 -4 -9 206.82 20.15 1 -4 -9 182.29 16.33 1 -4 -9 159.85 18.13 1 -4 -8 6.31 6.24 1 -4 -8 12.07 3.92 1 -4 -8 8.82 9.53 1 4 -8 13.83 5.04 1 -4 -8 8.69 9.71 1 -4 -8 13.00 10.31 1 -4 -7 747.77 38.38 1 -4 -7 888.20 45.19 1 -4 -7 736.06 34.91 1 4 -7 806.40 35.30 1 -4 -7 835.88 45.60 1 -4 -7 642.63 41.08 1 -4 -6 9.56 7.08 1 -4 -6 21.82 8.55 1 -4 -6 8.42 9.68 1 -4 -6 11.34 4.33 1 -4 -6 19.41 10.13 1 -4 -6 13.86 9.43 1 -4 -6 9.20 10.19 1 -4 -5 859.79 43.49 1 -4 -5 993.90 48.42 1 -4 -5 1013.00 49.46 1 -4 -5 1053.81 51.60 1 -4 -5 1028.07 49.82 1 -4 -4 90.02 9.95 1 -4 -4 89.16 10.58 1 -4 -4 85.29 11.12 1 -4 -4 83.76 12.41 1 -4 -4 68.73 11.89 1 -4 -4 84.23 12.23 1 -4 -3 785.09 34.16 1 -4 -3 736.01 36.64 1 -4 -2 92.86 8.05 1 -4 -2 93.01 10.63 1 -4 -2 63.57 7.75 1 -4 -1 1101.18 45.21 1 -4 -1 1053.73 48.49 1 -4 -1 1025.99 46.09 1 -4 0 52.21 7.45 1 -4 0 38.42 6.86 1 -4 0 42.44 8.83 1 -4 1 2033.82 81.67 1 -4 1 2043.88 84.71 1 -4 1 1941.91 77.49 1 -4 1 2092.85 83.02 1 -4 2 79.81 9.65 1 -4 2 83.92 11.32 1 -4 2 91.73 8.46 1 -4 2 91.00 11.89 1 -4 3 688.44 34.10 1 -4 3 630.79 35.74 1 -4 3 626.37 37.23 1 -4 3 742.56 33.04 1 -4 4 254.15 16.68 1 -4 4 226.60 16.83 1 -4 4 197.53 17.86 1 -4 4 209.03 19.28 1 -4 4 229.60 16.97 1 -4 4 231.85 18.83 1 -4 4 221.08 21.46 1 -4 4 221.16 20.46 1 -4 5 1301.02 53.48 1 -4 5 1241.44 53.26 1 -4 5 1034.57 53.14 1 -4 5 1056.28 54.82 1 -4 5 1141.92 58.08 1 -4 5 1076.45 58.12 1 -4 6 223.89 17.85 1 -4 6 190.03 16.77 1 -4 6 238.01 17.69 1 -4 6 199.89 21.33 1 -4 6 216.44 21.81 1 -4 7 536.01 29.21 1 -4 7 580.29 32.89 1 -4 7 657.88 33.87 1 -4 7 554.87 37.77 1 -4 8 34.99 9.73 1 -4 8 18.51 6.14 1 -4 9 481.91 20.31 1 -4 9 1.86 3.46 1 -5 -9 117.50 11.84 1 -5 -9 142.98 13.99 1 -5 -9 98.55 12.79 1 -5 -8 190.80 17.38 1 -5 -8 187.40 18.87 1 -5 -8 220.07 19.41 1 -5 -8 170.67 20.16 1 -5 -7 152.51 16.39 1 -5 -7 190.13 18.89 1 -5 -7 203.50 18.14 1 -5 -7 180.82 20.15 1 -5 -6 131.62 12.32 1 -5 -6 124.52 16.19 1 -5 -6 124.92 17.64 1 -5 -6 147.25 17.24 1 -5 -6 107.83 17.19 1 -5 -5 313.32 19.89 1 -5 -5 280.13 23.62 1 -5 -5 246.86 24.28 1 -5 -5 325.62 23.91 1 -5 -5 260.57 25.45 1 -5 -4 116.08 16.25 1 -5 -4 154.80 13.88 1 -5 -4 137.79 13.32 1 -5 -4 123.36 12.69 1 -5 -4 112.10 16.61 1 -5 -4 125.95 14.48 1 -5 -4 125.20 16.32 1 -5 -3 779.19 47.92 1 -5 -3 877.10 46.14 1 -5 -3 814.59 47.45 1 -5 -3 929.12 44.27 1 -5 -3 1048.07 45.80 1 -5 -3 931.56 41.35 1 -5 -3 966.49 43.50 1 -5 -3 810.87 45.87 1 -5 -3 908.20 44.95 1 -5 -2 57.62 7.19 1 -5 -2 48.27 11.73 1 -5 -2 62.21 10.37 1 -5 -2 55.82 13.49 1 -5 -2 60.40 9.39 1 -5 -2 63.96 11.03 1 -5 -2 58.25 11.03 1 -5 -2 48.69 8.16 1 -5 -2 35.24 9.85 1 -5 -1 297.17 23.66 1 -5 -1 294.44 19.23 1 -5 -1 308.34 21.60 1 -5 -1 277.32 24.07 1 -5 -1 325.47 22.84 1 -5 -1 314.70 19.87 1 -5 -1 295.91 19.93 1 -5 -1 293.77 22.07 1 -5 -1 286.38 21.20 1 -5 -1 338.77 18.61 1 -5 0 201.32 17.75 1 -5 0 176.93 20.12 1 -5 0 201.00 17.58 1 -5 0 174.02 15.45 1 -5 0 221.33 15.83 1 -5 0 186.73 19.02 1 -5 0 179.44 14.84 1 -5 0 200.48 16.12 1 -5 0 208.04 14.68 1 -5 0 212.05 18.72 1 -5 1 455.72 25.39 1 -5 1 442.77 26.55 1 -5 1 378.98 27.03 1 -5 1 454.08 25.55 1 -5 1 451.35 28.08 1 -5 2 295.42 24.72 1 -5 2 275.45 25.35 1 -5 2 300.73 23.23 1 -5 2 296.41 20.88 1 -5 3 396.42 23.08 1 -5 3 353.31 27.59 1 -5 3 338.94 25.08 1 -5 3 303.75 28.24 1 -5 3 345.73 25.53 1 -5 3 367.88 23.82 1 -5 3 300.05 23.87 1 -5 4 399.27 30.38 1 -5 4 496.76 27.41 1 -5 4 415.90 32.77 1 -5 4 376.93 28.37 1 -5 4 440.22 28.86 1 -5 4 439.63 27.25 1 -5 5 453.78 28.87 1 -5 5 475.22 27.87 1 -5 5 365.52 28.90 1 -5 5 392.56 30.01 1 -5 5 513.69 28.46 1 -5 5 413.74 28.95 1 -5 5 423.44 33.04 1 -5 6 26.85 11.22 1 -5 6 31.26 9.75 1 -5 6 25.62 10.46 1 -5 6 27.05 8.76 1 -5 7 248.72 19.43 1 -5 8 136.97 12.31 1 -5 9 239.68 15.37 1 -6 -8 -3.25 3.58 1 -6 -7 48.44 9.34 1 -6 -6 357.77 20.85 1 -6 -6 313.45 22.49 1 -6 -5 203.40 15.91 1 -6 -5 180.49 17.03 1 -6 -4 315.36 14.89 1 -6 -4 319.88 19.38 1 -6 -3 12.70 9.72 1 -6 -3 8.15 6.23 1 -6 -3 7.72 7.09 1 -6 -3 1.93 6.88 1 -6 -3 7.23 6.94 1 -6 -2 502.85 29.17 1 -6 -2 471.82 32.53 1 -6 -2 512.21 30.18 1 -6 -2 501.58 27.11 1 -6 -2 520.74 27.13 1 -6 -2 458.36 28.76 1 -6 -2 461.94 31.37 1 -6 -2 461.24 28.59 1 -6 -1 245.80 20.18 1 -6 -1 242.38 18.01 1 -6 -1 238.90 16.88 1 -6 -1 207.04 21.39 1 -6 -1 222.25 18.84 1 -6 -1 235.17 23.42 1 -6 -1 207.60 15.90 1 -6 -1 214.15 19.27 1 -6 0 545.73 32.01 1 -6 0 496.64 36.30 1 -6 0 484.87 26.69 1 -6 0 527.32 35.06 1 -6 0 499.30 28.34 1 -6 0 546.66 33.26 1 -6 0 486.74 28.85 1 -6 0 583.28 33.82 1 -6 0 566.31 30.82 1 -6 1 188.05 18.05 1 -6 1 146.55 12.84 1 -6 1 171.21 16.21 1 -6 1 168.58 14.92 1 -6 1 179.00 18.82 1 -6 1 165.01 16.17 1 -6 2 472.70 29.16 1 -6 2 447.78 34.69 1 -6 2 470.14 30.20 1 -6 2 430.41 32.84 1 -6 2 451.32 26.94 1 -6 2 439.03 30.35 1 -6 2 482.70 30.79 1 -6 3 190.98 23.90 1 -6 3 221.06 19.92 1 -6 3 199.56 17.78 1 -6 3 199.33 22.04 1 -6 3 191.56 16.48 1 -6 3 200.96 19.05 1 -6 4 236.05 20.92 1 -6 4 262.16 24.25 1 -6 4 237.02 25.33 1 -6 4 269.33 21.02 1 -6 4 258.06 19.91 1 -6 4 234.77 21.37 1 -6 5 56.43 13.89 1 -6 5 60.80 10.75 1 -6 5 66.93 12.90 1 -6 5 75.75 16.37 1 -6 6 282.73 20.63 1 -6 6 284.43 21.04 1 -6 6 271.70 18.12 1 -6 7 82.12 10.98 1 -6 7 73.65 9.81 1 -6 8 210.29 12.20 1 -6 8 195.41 13.10 1 -7 -2 39.95 10.82 1 -7 -2 382.21 18.18 1 -7 -1 8.22 10.36 1 -7 -1 10.58 5.89 1 -7 -1 13.93 7.23 1 -7 -1 14.81 11.37 1 -7 0 324.31 25.20 1 -7 0 344.70 26.62 1 -7 0 341.67 22.80 1 -7 0 344.67 21.17 1 -7 0 327.23 22.62 1 -7 1 24.00 7.52 1 -7 1 21.26 8.79 1 -7 1 19.74 13.77 1 -7 1 21.25 9.51 1 -7 1 24.58 11.99 1 -7 2 200.41 16.24 1 -7 2 239.47 16.10 1 -7 2 187.20 12.66 1 -7 2 225.98 17.76 1 -7 3 44.27 9.88 1 -7 3 52.82 14.60 1 -7 3 56.44 12.83 1 -7 3 45.47 7.55 1 -7 3 49.47 9.06 1 -7 4 456.57 25.18 1 -7 4 451.07 25.04 1 -7 4 442.01 26.33 1 -7 4 452.63 23.20 1 -7 4 482.70 28.61 1 -7 5 11.33 6.90 1 -7 5 9.01 6.81 1 -7 5 2.38 7.69 1 -7 5 5.24 4.41 1 -7 6 223.93 13.04 1 -7 6 205.10 12.75 1 -7 6 189.61 11.17 2 0 -12 49.09 6.56 2 0 -12 66.37 6.59 2 0 -11 -1.09 5.80 2 0 -11 -1.16 5.80 2 0 -10 537.03 30.11 2 0 -9 2.30 8.01 2 0 -9 1.44 5.87 2 0 -9 0.83 3.59 2 0 -9 -1.00 4.90 2 0 -8 625.20 40.59 2 0 -8 744.21 34.93 2 0 -8 724.38 36.29 2 0 -8 589.60 34.42 2 0 -7 5.43 4.42 2 0 -7 1.90 4.43 2 0 -7 4.87 5.94 2 0 -7 13.49 4.66 2 0 -6 1677.75 71.25 2 0 -6 1699.98 72.31 2 0 -5 1.24 3.25 2 0 -5 -2.03 3.38 2 0 -4 4490.60 167.05 2 0 -3 -0.61 2.77 2 0 0 1341.34 48.98 2 0 0 1302.86 49.73 2 0 1 -0.31 2.50 2 0 9 -2.82 4.73 2 0 11 1.03 5.40 2 0 12 73.88 7.34 2 -1 -12 207.31 13.72 2 1 -12 283.05 14.20 2 -1 -11 136.45 11.38 2 1 -11 144.76 11.57 2 -1 -11 87.27 13.14 2 -1 -11 146.49 13.67 2 1 -11 120.83 11.36 2 -1 -11 104.97 11.47 2 -1 -10 491.35 29.58 2 -1 -10 458.28 34.01 2 -1 -10 474.25 29.10 2 1 -10 555.55 29.28 2 1 -10 580.21 28.64 2 -1 -10 546.28 28.66 2 -1 -9 131.27 16.34 2 1 -9 168.05 14.66 2 -1 -9 148.28 14.66 2 1 -9 148.56 13.32 2 -1 -9 162.07 14.01 2 -1 -9 170.60 15.70 2 1 -9 151.35 12.79 2 -1 -9 135.86 13.23 2 -1 -9 156.00 19.01 2 -1 -8 505.14 34.55 2 -1 -8 647.54 33.70 2 -1 -8 626.86 38.01 2 1 -8 621.01 30.55 2 -1 -8 563.80 30.67 2 -1 -8 522.71 31.46 2 1 -8 752.62 34.67 2 -1 -8 582.38 30.16 2 1 -8 594.59 30.12 2 1 -8 581.03 32.22 2 -1 -8 588.24 31.31 2 -1 -7 283.46 18.01 2 1 -7 288.50 17.32 2 1 -7 276.35 18.58 2 -1 -7 326.62 20.28 2 1 -7 285.70 16.45 2 -1 -7 258.64 18.39 2 -1 -7 290.56 18.12 2 1 -7 279.41 17.29 2 -1 -7 280.82 17.23 2 -1 -7 262.33 21.63 2 1 -6 1010.45 42.20 2 -1 -6 949.48 42.04 2 1 -6 937.55 41.23 2 -1 -5 12.64 4.97 2 1 -5 10.27 3.41 2 1 -5 11.10 3.54 2 -1 -5 12.10 3.90 2 1 -4 755.29 31.80 2 -1 -4 776.48 32.10 2 -1 -3 1974.22 74.07 2 1 -3 1924.57 73.95 2 -1 -2 6393.64 225.69 2 -1 -2 5929.03 225.52 2 -1 -1 1340.89 50.82 2 -1 0 1749.26 67.65 2 -1 0 1804.12 66.98 2 -1 1 260.02 12.88 2 1 1 235.26 9.77 2 -1 2 1694.47 57.73 2 1 2 1385.01 54.05 2 -1 8 686.65 34.77 2 -1 9 100.14 11.25 2 -1 9 92.53 11.19 2 -1 9 91.29 14.08 2 1 11 48.38 7.42 2 -1 11 45.27 7.82 2 -1 12 257.27 14.22 2 1 12 233.98 13.10 2 2 -12 181.43 9.59 2 -2 -12 132.91 10.15 2 2 -11 231.42 14.90 2 -2 -11 208.41 15.36 2 2 -11 272.13 15.20 2 -2 -11 205.06 19.25 2 -2 -11 278.36 18.40 2 -2 -11 221.41 17.03 2 -2 -10 67.12 11.70 2 -2 -10 78.07 10.12 2 -2 -10 58.43 8.65 2 2 -10 74.61 9.02 2 -2 -10 40.48 11.61 2 2 -10 70.09 8.50 2 -2 -10 89.80 13.41 2 -2 -10 54.45 12.99 2 -2 -9 215.38 22.67 2 -2 -9 245.93 20.73 2 -2 -9 234.47 18.14 2 -2 -9 220.24 16.79 2 2 -9 244.58 16.53 2 -2 -9 231.73 16.62 2 2 -9 217.85 17.88 2 -2 -9 201.39 22.01 2 2 -9 254.94 17.55 2 -2 -8 268.74 24.30 2 -2 -8 335.13 23.69 2 -2 -8 251.97 17.37 2 -2 -8 290.79 20.86 2 2 -8 304.33 18.82 2 -2 -8 249.36 20.42 2 -2 -8 285.39 19.75 2 -2 -8 266.53 24.37 2 2 -8 295.25 18.22 2 -2 -8 330.30 19.58 2 2 -8 297.60 20.80 2 -2 -7 509.24 32.86 2 -2 -7 522.91 33.50 2 -2 -7 570.60 31.86 2 2 -7 481.23 25.12 2 -2 -7 473.71 29.18 2 -2 -7 520.83 28.13 2 2 -7 514.45 26.68 2 -2 -7 534.59 27.30 2 2 -7 585.95 29.96 2 -2 -7 529.20 26.83 2 2 -7 540.99 26.53 2 -2 -7 502.30 26.20 2 -2 -7 559.68 29.55 2 2 -6 798.05 34.91 2 -2 -6 798.11 36.90 2 -2 -6 767.57 34.52 2 -2 -6 765.11 34.86 2 2 -6 740.14 34.08 2 2 -6 778.47 36.76 2 2 -5 1853.63 76.79 2 -2 -5 1964.82 77.09 2 2 -5 1946.29 77.11 2 -2 -5 2006.76 77.78 2 2 -4 1634.46 68.24 2 -2 -4 1809.29 68.28 2 2 -4 1761.36 68.51 2 -2 -4 1749.73 68.86 2 2 -3 10.34 2.62 2 -2 -3 11.21 2.72 2 -2 -3 13.61 2.41 2 -2 -2 150.79 6.71 2 -2 -2 154.87 7.82 2 2 -2 155.48 7.86 2 -2 -1 2576.68 94.85 2 -2 0 2915.34 104.37 2 -2 0 2761.89 101.53 2 -2 1 2129.19 85.66 2 -2 1 2227.28 83.24 2 -2 2 769.76 32.14 2 -2 4 404.60 23.28 2 -2 4 368.71 19.48 2 -2 5 709.96 36.56 2 -2 6 558.67 32.22 2 -2 7 340.91 22.08 2 -2 8 258.99 20.00 2 -2 8 302.72 20.61 2 -2 8 275.27 23.39 2 -2 9 436.50 27.39 2 -2 9 412.84 31.28 2 -2 9 489.84 26.98 2 -2 9 456.58 26.57 2 -2 10 106.69 11.13 2 -2 10 117.64 11.89 2 -2 11 83.74 8.80 2 2 11 63.81 7.08 2 -2 12 35.20 4.59 2 -3 -11 110.28 11.03 2 -3 -11 93.59 11.07 2 -3 -11 98.40 11.02 2 3 -11 124.07 8.07 2 -3 -11 93.21 12.40 2 -3 -10 66.04 8.74 2 3 -10 94.43 8.45 2 -3 -10 67.40 9.26 2 -3 -10 92.71 14.34 2 -3 -10 70.27 12.76 2 -3 -10 49.08 12.63 2 -3 -10 94.11 12.81 2 -3 -10 80.83 13.76 2 -3 -9 522.95 28.90 2 3 -9 566.60 27.14 2 -3 -9 522.33 33.92 2 -3 -9 421.45 34.67 2 -3 -9 624.72 35.04 2 -3 -9 497.05 35.48 2 -3 -8 96.16 15.63 2 -3 -8 70.59 14.94 2 -3 -8 92.79 14.79 2 -3 -8 111.55 11.68 2 3 -8 104.03 10.07 2 -3 -8 88.98 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9 -6 -3 89.14 9.94 9 -6 -2 253.49 18.85 9 -6 -2 247.78 16.94 9 -6 -2 236.74 21.68 9 -6 -1 60.01 9.18 9 -6 -1 61.16 11.55 9 -6 -1 51.72 10.51 9 -6 -1 49.09 9.19 9 -6 -1 61.90 11.31 9 -6 0 261.15 21.29 9 -6 0 223.68 17.51 9 -6 0 253.11 23.36 9 -6 0 258.91 19.29 9 -6 1 119.34 16.18 9 -6 1 107.49 12.12 9 -6 1 132.08 13.68 9 -6 1 146.86 18.50 9 -6 2 120.36 12.37 9 -6 2 112.12 16.60 9 -6 2 89.30 10.80 9 -6 2 105.22 11.46 9 -6 3 14.29 5.39 9 -6 3 24.61 10.85 9 -6 3 20.35 7.94 9 -6 3 12.04 10.45 9 -6 4 213.63 15.68 9 -6 4 201.43 15.37 9 -6 4 237.23 17.76 9 -6 5 64.22 8.30 9 -6 5 67.07 8.65 10 0 -10 112.90 9.23 10 0 -9 10.15 7.51 10 0 -9 1.53 4.99 10 0 -8 456.60 32.39 10 0 -8 407.96 26.92 10 0 -7 6.25 10.90 10 0 -7 0.87 5.18 10 0 -6 410.93 26.40 10 0 -6 407.55 32.76 10 0 -5 -3.29 5.56 10 0 -5 8.07 10.75 10 0 -5 -0.35 4.11 10 0 -4 800.01 51.61 10 0 -4 1116.49 45.06 10 0 -3 -0.56 3.18 10 0 -2 132.22 9.89 10 0 -1 -0.46 3.03 10 0 3 -0.47 6.50 10 0 3 7.29 5.14 10 0 4 473.33 27.93 10 0 4 429.70 24.96 10 0 5 0.40 4.90 10 0 6 735.92 36.37 10 0 6 715.09 40.11 10 0 7 -5.93 9.55 10 0 8 315.72 21.91 10 0 9 1.23 6.11 10 -1 -10 87.37 8.38 10 -1 -10 75.26 7.19 10 1 -10 77.54 9.13 10 1 -9 33.01 10.68 10 -1 -9 57.56 7.55 10 -1 -9 53.43 9.41 10 -1 -8 185.16 16.89 10 1 -8 193.94 21.38 10 -1 -8 198.53 18.11 10 -1 -7 18.00 9.76 10 1 -7 24.90 12.81 10 -1 -7 36.23 11.07 10 -1 -7 59.96 10.29 10 1 -6 449.67 27.83 10 -1 -6 511.11 28.72 10 -1 -6 470.09 33.25 10 -1 -6 420.60 29.58 10 1 -5 155.79 14.37 10 -1 -5 174.03 14.75 10 -1 -5 163.35 19.29 10 -1 -5 146.52 16.22 10 -1 -5 208.27 14.11 10 1 -5 181.40 13.87 10 -1 -4 642.96 32.71 10 -1 -4 540.32 36.77 10 1 -4 441.30 36.14 10 -1 -4 714.20 30.21 10 1 -4 708.03 31.26 10 -1 -4 494.37 32.28 10 -1 -3 11.83 9.62 10 1 -3 10.06 9.98 10 1 -3 18.27 4.84 10 -1 -3 15.42 4.11 10 -1 -3 17.84 8.14 10 1 -2 1311.13 50.38 10 -1 -2 1202.38 48.32 10 -1 -2 1137.56 57.24 10 -1 2 466.65 27.97 10 -1 2 421.47 24.94 10 -1 3 84.44 11.78 10 1 3 92.84 11.05 10 -1 3 82.61 10.33 10 -1 4 573.73 31.18 10 -1 5 47.59 11.85 10 -1 5 44.48 8.74 10 -1 6 148.42 14.28 10 -1 6 157.95 17.54 10 1 6 155.49 16.63 10 1 7 90.84 12.99 10 -1 7 90.41 14.51 10 -1 8 171.28 16.11 10 1 8 153.76 14.34 10 -1 9 6.29 6.52 10 -1 10 99.97 7.97 10 2 -10 156.28 11.32 10 -2 -10 161.58 8.98 10 -2 -9 121.36 12.87 10 -2 -9 105.69 10.29 10 -2 -8 70.21 12.43 10 2 -8 106.56 9.78 10 -2 -8 83.62 9.69 10 -2 -7 229.03 17.48 10 -2 -7 232.17 21.18 10 2 -7 263.24 17.37 10 -2 -7 271.10 16.78 10 -2 -6 257.67 19.49 10 2 -6 164.39 21.87 10 -2 -6 223.97 17.74 10 2 -6 194.18 16.06 10 -2 -6 242.44 17.15 10 2 -6 269.40 17.26 10 -2 -6 316.72 18.13 10 -2 -6 236.37 21.58 10 -2 -6 192.05 16.84 10 -2 -5 44.42 10.89 10 2 -5 20.85 12.72 10 -2 -5 39.59 8.55 10 2 -5 45.31 7.72 10 -2 -5 39.02 7.16 10 2 -5 38.76 7.22 10 -2 -5 36.80 11.60 10 -2 -5 24.07 7.78 10 -2 -4 8.92 8.05 10 2 -4 2.37 11.06 10 -2 -4 3.55 5.99 10 2 -4 7.34 5.04 10 -2 -4 13.71 5.43 10 2 -4 11.50 5.07 10 -2 -4 7.08 10.07 10 -2 -4 6.44 6.78 10 -2 -3 566.19 31.20 10 2 -3 321.83 29.17 10 -2 -3 388.12 24.09 10 2 -3 546.72 25.27 10 -2 -3 399.65 25.66 10 -2 -3 429.05 28.99 10 -2 -3 479.11 25.54 10 2 -2 364.62 28.85 10 -2 -2 456.05 26.93 10 -2 -1 1081.53 49.05 10 -2 -1 950.83 45.24 10 -2 -1 989.27 40.41 10 -2 0 308.43 16.44 10 -2 0 356.90 23.41 10 -2 0 300.05 20.87 10 -2 0 319.32 20.60 10 -2 1 495.48 24.40 10 -2 1 510.64 27.92 10 -2 1 524.23 30.27 10 -2 2 122.88 9.69 10 -2 2 142.48 13.36 10 -2 2 100.49 13.29 10 -2 3 235.66 18.07 10 -2 3 203.28 18.61 10 -2 4 184.74 16.30 10 -2 4 193.41 18.57 10 -2 5 89.02 11.79 10 -2 5 94.88 14.57 10 -2 6 86.77 11.44 10 -2 7 223.85 19.30 10 2 7 185.08 16.17 10 -2 8 58.31 11.16 10 -2 9 293.66 18.08 10 -2 10 51.73 5.51 10 -3 -9 184.60 11.60 10 3 -9 169.93 14.58 10 -3 -9 155.15 11.61 10 -3 -8 69.46 9.15 10 -3 -8 64.41 8.37 10 3 -8 86.19 8.70 10 3 -8 59.11 11.96 10 -3 -8 83.56 12.49 10 -3 -7 372.09 23.25 10 -3 -7 382.39 23.69 10 3 -7 450.21 22.77 10 3 -7 319.82 27.50 10 -3 -7 413.38 27.82 10 -3 -6 41.28 9.15 10 -3 -6 25.98 8.57 10 3 -6 33.54 6.25 10 3 -6 30.38 12.44 10 -3 -6 22.10 11.76 10 -3 -5 262.27 19.63 10 -3 -5 269.88 20.93 10 3 -5 330.01 18.96 10 -3 -5 285.20 24.53 10 3 -4 162.82 12.93 10 -3 -4 148.23 15.54 10 -3 -4 137.01 13.92 10 -3 -3 649.44 36.50 10 -3 -3 625.60 33.90 10 -3 -2 61.20 9.65 10 -3 -2 81.50 11.97 10 3 -2 85.46 9.38 10 -3 -2 78.92 12.03 10 -3 -2 90.97 8.94 10 3 -2 59.12 12.42 10 -3 -2 102.31 12.45 10 -3 -1 163.64 15.28 10 -3 -1 134.68 12.70 10 -3 -1 144.50 11.31 10 -3 -1 139.34 15.14 10 -3 -1 120.01 14.43 10 -3 -1 151.82 15.19 10 -3 0 171.83 15.86 10 -3 0 119.60 11.82 10 -3 0 141.14 11.10 10 -3 0 141.87 15.23 10 -3 0 133.71 14.07 10 -3 0 125.13 13.98 10 -3 1 506.24 29.02 10 -3 1 492.86 26.93 10 -3 1 514.35 26.12 10 -3 1 560.48 32.09 10 -3 1 456.59 28.16 10 -3 2 157.30 13.12 10 -3 2 188.28 16.15 10 -3 2 161.76 12.78 10 -3 2 167.52 14.62 10 -3 2 151.19 14.40 10 -3 3 764.77 38.93 10 -3 3 712.74 35.32 10 -3 3 701.67 37.98 10 -3 3 719.94 40.37 10 -3 4 24.42 9.44 10 -3 5 435.82 28.17 10 -3 6 75.28 12.94 10 -3 8 48.89 8.98 10 -3 9 51.28 6.92 10 -4 -8 20.80 5.36 10 -4 -8 22.24 5.36 10 -4 -8 30.14 6.04 10 4 -8 15.08 6.77 10 -4 -7 112.74 10.63 10 -4 -7 98.36 11.09 10 4 -7 128.34 9.54 10 -4 -7 102.31 11.67 10 4 -7 78.92 12.27 10 4 -6 7.35 3.89 10 -4 -6 7.67 7.26 10 -4 -6 7.52 6.86 10 4 -6 10.74 9.54 10 -4 -6 -0.43 7.94 10 -4 -5 539.69 29.37 10 -4 -5 544.08 31.55 10 4 -5 599.10 27.41 10 -4 -5 545.44 32.50 10 -4 -4 38.73 9.12 10 -4 -4 29.45 10.04 10 4 -4 52.03 7.20 10 -4 -4 35.95 10.96 10 4 -4 28.31 10.07 10 4 -3 244.21 16.18 10 -4 -3 224.25 20.26 10 -4 -3 234.71 21.14 10 -4 -3 231.11 18.34 10 -4 -2 149.14 14.60 10 -4 -2 145.16 16.94 10 4 -2 173.37 13.08 10 -4 -2 154.67 16.34 10 -4 -2 158.66 17.55 10 -4 -1 404.41 26.69 10 -4 -1 410.74 24.94 10 -4 -1 425.19 28.47 10 -4 -1 408.53 22.86 10 -4 -1 388.90 27.18 10 -4 0 4.60 6.88 10 -4 0 6.70 8.93 10 -4 0 4.11 7.95 10 -4 0 0.70 3.97 10 -4 0 -1.64 8.07 10 -4 1 365.77 24.57 10 -4 1 380.58 30.37 10 -4 1 369.59 22.70 10 -4 1 401.96 27.70 10 -4 1 357.90 21.27 10 -4 1 340.53 23.58 10 -4 2 50.89 9.78 10 -4 2 49.10 7.72 10 -4 2 58.01 15.45 10 -4 2 66.88 10.71 10 -4 3 344.54 21.76 10 -4 3 334.88 26.40 10 -4 3 325.02 20.85 10 -4 4 29.60 9.19 10 -4 5 270.21 19.47 10 -4 6 34.85 8.86 10 -4 6 19.99 9.20 10 -4 7 179.22 13.81 10 -4 8 10.08 4.92 10 -5 -7 134.77 9.07 10 -5 -7 122.50 9.12 10 -5 -6 76.69 9.50 10 -5 -6 66.00 8.08 10 -5 -6 70.49 9.19 10 -5 -5 220.38 16.97 10 -5 -5 180.90 16.53 10 -5 -5 214.06 14.96 10 -5 -4 63.39 9.42 10 -5 -4 57.66 11.13 10 5 -4 57.93 6.38 10 -5 -4 66.57 14.17 10 -5 -4 71.45 11.64 10 -5 -3 232.92 16.98 10 -5 -3 251.72 19.96 10 5 -3 192.18 13.33 10 -5 -3 237.24 19.57 10 -5 -3 228.11 22.21 10 -5 -2 155.84 15.34 10 -5 -2 164.33 14.54 10 -5 -2 134.53 16.06 10 5 -2 146.10 11.11 10 -5 -2 148.49 16.48 10 -5 -2 164.34 16.87 10 -5 -1 228.02 24.28 10 -5 -1 228.03 17.26 10 -5 -1 250.99 20.25 10 5 -1 226.52 14.81 10 -5 -1 230.43 20.43 10 -5 -1 226.93 18.94 10 -5 0 190.97 23.00 10 -5 0 218.64 16.75 10 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0 -8 675.29 31.07 11 0 -8 303.86 25.90 11 0 -7 0.40 5.03 11 0 -7 0.71 10.08 11 0 -6 296.25 20.88 11 0 -6 231.91 24.71 11 0 -5 -0.71 4.06 11 0 -5 -1.97 4.54 11 0 -5 -0.81 10.89 11 0 -4 752.00 33.48 11 0 -4 550.06 39.73 11 0 -3 0.30 3.40 11 0 -2 550.40 25.57 11 0 -2 423.45 31.22 11 0 -1 -0.51 3.07 11 0 -1 4.39 7.89 11 0 0 1446.29 67.32 11 0 1 0.54 7.59 11 0 2 635.88 35.24 11 0 3 -3.55 7.34 11 0 5 -4.24 10.01 11 0 5 -2.79 4.78 11 0 6 165.42 17.93 11 0 7 -2.05 9.17 11 0 8 261.62 18.88 11 0 9 6.35 5.35 11 -1 -9 21.03 4.55 11 -1 -9 18.21 4.88 11 1 -9 14.66 7.86 11 -1 -8 110.51 10.59 11 -1 -8 106.93 12.45 11 -1 -8 148.85 12.03 11 1 -8 107.88 15.48 11 -1 -7 79.43 9.62 11 -1 -7 84.92 12.95 11 1 -7 66.08 14.86 11 -1 -7 80.64 12.25 11 1 -7 94.20 10.28 11 -1 -7 117.93 12.78 11 -1 -6 197.70 15.80 11 -1 -6 235.63 21.91 11 1 -6 235.97 17.83 11 -1 -6 227.62 17.60 11 -1 -6 195.38 18.54 11 1 -6 290.03 17.81 11 -1 -6 311.23 18.49 11 -1 -5 63.74 8.77 11 1 -5 80.51 10.48 11 -1 -5 81.71 10.28 11 -1 -5 87.80 14.83 11 -1 -5 56.41 11.27 11 -1 -5 84.72 8.97 11 1 -5 83.60 9.53 11 -1 -4 467.32 26.85 11 -1 -4 420.67 30.88 11 1 -4 353.82 30.49 11 -1 -4 467.49 23.59 11 1 -4 508.93 25.22 11 -1 -4 386.80 26.74 11 -1 -3 153.11 18.06 11 1 -3 137.84 18.54 11 -1 -3 173.71 11.77 11 1 -3 181.98 13.03 11 -1 -2 420.40 28.45 11 1 -2 428.30 21.69 11 -1 -2 374.73 19.35 11 1 -1 61.63 12.20 11 -1 -1 59.98 12.04 11 1 0 596.78 35.13 11 -1 1 169.96 16.45 11 1 1 147.71 15.31 11 -1 2 493.55 29.98 11 1 2 459.49 28.04 11 -1 3 172.90 16.72 11 1 3 163.79 15.07 11 -1 3 154.56 14.41 11 -1 4 449.30 26.64 11 -1 5 164.01 14.61 11 -1 6 190.96 19.10 11 1 6 203.14 18.91 11 -1 7 18.96 9.76 11 1 7 19.31 9.20 11 -1 8 56.66 10.57 11 1 8 56.53 9.21 11 -1 9 54.88 7.82 11 2 -9 157.59 11.29 11 -2 -9 89.95 8.14 11 -2 -8 75.12 11.50 11 2 -8 103.75 9.89 11 -2 -8 83.36 9.01 11 2 -7 93.81 15.90 11 -2 -7 115.19 14.85 11 2 -7 128.43 11.27 11 -2 -7 102.53 11.03 11 -2 -6 407.74 24.39 11 2 -6 303.18 28.14 11 -2 -6 338.18 21.67 11 -2 -6 350.55 25.78 11 2 -6 411.39 22.42 11 -2 -5 653.07 35.05 11 2 -5 460.55 36.01 11 2 -5 561.71 31.03 11 -2 -5 552.71 30.44 11 -2 -5 496.79 29.18 11 -2 -5 557.79 34.31 11 2 -5 686.22 31.00 11 -2 -4 112.79 12.04 11 -2 -4 181.41 17.59 11 2 -4 114.57 17.81 11 2 -4 146.84 13.52 11 -2 -4 157.78 13.45 11 -2 -3 460.88 25.35 11 -2 -3 387.71 23.14 11 -2 -3 398.35 25.22 11 2 -3 358.44 29.59 11 -2 -2 390.91 24.38 11 2 -2 308.54 26.45 11 -2 -1 110.68 12.81 11 2 -1 92.51 13.75 11 -2 0 193.16 16.76 11 -2 0 219.44 19.32 11 2 0 179.04 17.34 11 -2 1 173.17 16.74 11 -2 1 125.31 13.72 11 -2 1 144.82 14.77 11 -2 2 117.41 14.06 11 -2 3 147.20 14.03 11 -2 3 104.54 14.20 11 -2 4 252.89 19.45 11 -2 4 261.73 21.52 11 -2 5 257.89 19.46 11 -2 5 263.82 21.92 11 2 6 77.70 11.87 11 -2 7 197.68 17.44 11 2 7 158.52 14.56 11 -2 8 104.44 11.75 11 -2 9 64.72 7.94 11 3 -9 199.81 13.27 11 -3 -9 195.34 10.52 11 -3 -8 60.41 7.44 11 3 -8 84.36 8.07 11 3 -8 55.50 10.15 11 -3 -8 57.10 9.07 11 -3 -7 245.78 16.74 11 3 -7 231.22 20.82 11 -3 -7 270.38 17.08 11 3 -6 23.45 5.48 11 -3 -6 17.04 7.20 11 3 -6 18.95 11.34 11 -3 -6 19.62 7.21 11 -3 -5 177.53 16.31 11 3 -5 155.62 19.29 11 -3 -5 176.60 15.13 11 3 -4 115.06 10.66 11 -3 -4 88.53 12.15 11 3 -4 72.86 14.91 11 -3 -4 78.54 10.87 11 3 -3 214.17 15.01 11 -3 -3 191.83 17.55 11 -3 -3 230.82 17.46 11 -3 -3 192.80 15.58 11 -3 -2 82.55 10.32 11 -3 -2 86.10 12.45 11 3 -2 103.48 10.34 11 -3 -2 96.37 13.20 11 3 -2 72.01 13.13 11 -3 -2 112.28 12.65 11 -3 -1 893.51 44.97 11 -3 -1 993.52 43.97 11 -3 -1 1052.88 50.42 11 -3 -1 958.49 48.86 11 -3 0 244.39 16.89 11 -3 0 264.72 21.10 11 -3 0 263.14 19.59 11 -3 0 230.64 15.32 11 -3 1 497.33 28.28 11 -3 1 526.04 31.21 11 -3 1 457.82 24.18 11 -3 2 31.05 8.63 11 -3 3 304.41 21.63 11 -3 3 284.55 23.07 11 -3 3 287.37 21.40 11 -3 4 66.72 12.00 11 -3 5 189.54 17.62 11 3 6 47.04 9.11 11 -3 6 92.75 12.38 11 -4 -8 22.70 4.01 11 -4 -8 21.49 4.58 11 4 -8 22.32 4.94 11 -4 -7 198.30 13.47 11 -4 -7 207.34 13.20 11 4 -6 3.71 3.43 11 -4 -6 -1.77 6.33 11 -4 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117.86 11.47 15 -2 2 66.24 8.53 15 -2 3 239.06 16.74 15 -2 4 43.26 8.16 15 -2 5 52.48 7.97 15 2 5 43.34 8.34 15 -2 6 52.98 6.79 15 2 6 39.48 6.36 15 -3 -5 65.39 6.97 15 3 -5 81.36 7.81 15 -3 -4 55.84 7.33 15 3 -4 66.38 8.04 15 -3 -3 80.91 8.61 15 3 -3 95.36 9.64 15 -3 -2 10.26 4.97 15 3 -2 15.43 5.47 15 3 -1 385.91 20.03 15 3 0 59.94 6.76 15 3 1 274.93 15.60 15 -3 1 284.53 20.41 15 3 2 8.76 3.36 15 3 5 65.25 6.82 15 -4 -4 -0.85 2.64 15 -4 -4 6.20 5.62 15 -4 -3 29.48 4.54 15 -4 -2 13.46 3.81 15 4 -2 10.15 2.83 15 -4 -2 10.29 8.23 15 4 -1 130.14 8.97 15 -4 -1 157.92 14.33 15 4 0 3.46 2.52 15 -4 0 5.11 7.84 15 4 1 62.97 5.90 15 -4 1 77.06 9.93 15 -4 4 23.30 5.02 16 0 -6 228.13 13.72 16 0 -5 1.61 5.63 16 0 -3 2.19 7.28 16 0 -2 280.37 20.58 16 0 -1 0.47 7.01 16 0 0 491.35 28.43 16 0 1 -2.15 6.69 16 0 2 15.33 8.07 16 0 3 -0.77 6.87 16 0 4 101.01 11.43 16 0 6 42.39 6.31 16 -1 -5 113.80 9.38 16 1 -5 93.68 9.74 16 1 -4 81.83 7.04 16 -1 -4 114.35 10.90 16 1 -4 96.01 11.02 16 1 -3 10.43 3.47 16 -1 -3 17.69 7.55 16 1 -3 16.16 7.50 16 1 -2 142.74 10.02 16 1 -2 184.31 15.43 16 1 -1 9.96 3.30 16 1 -1 15.45 7.72 16 1 0 47.31 5.58 16 -1 0 77.57 11.13 16 1 0 66.33 10.05 16 -1 1 31.33 6.48 16 1 1 21.75 3.71 16 -1 2 119.21 11.90 16 -1 3 12.90 6.65 16 -1 4 84.62 9.82 16 -1 5 35.76 6.78 16 1 5 41.39 7.22 16 1 6 56.59 6.21 16 -2 -5 40.06 4.65 16 2 -5 61.45 7.26 16 2 -4 61.87 5.52 16 2 -4 68.81 8.38 16 2 -3 54.51 5.84 16 -2 -3 66.49 8.74 16 2 -3 63.37 8.53 16 2 -2 43.73 5.32 16 -2 -2 58.20 9.09 16 2 -2 43.99 8.08 16 2 -1 78.47 7.37 16 -2 -1 104.08 11.42 16 2 -1 106.26 10.43 16 2 0 57.19 6.35 16 2 0 91.04 9.20 16 2 1 69.30 6.67 16 2 1 83.56 8.16 16 2 2 46.05 5.34 16 2 3 145.68 9.17 16 -2 4 8.88 4.35 16 2 4 51.53 7.81 16 -2 5 13.42 4.10 16 2 5 13.46 4.85 16 3 -4 11.96 3.16 16 3 -3 149.52 9.26 16 3 -3 151.84 9.48 16 3 -2 4.44 2.44 16 3 -1 135.33 9.15 16 3 0 18.00 3.70 16 -3 0 21.20 8.31 16 3 1 53.70 5.57 16 -3 1 74.09 8.86 16 3 2 35.60 4.32 16 3 4 34.41 5.31 16 -4 -1 73.21 8.10 16 -4 0 33.06 5.90 17 0 -5 -2.27 3.78 17 0 -3 -1.58 5.60 17 0 -2 98.63 10.59 17 0 -1 3.87 5.84 17 0 0 68.82 9.42 17 0 1 3.28 5.50 17 0 1 -3.60 6.05 17 0 2 48.38 8.00 17 0 3 0.27 5.38 17 0 4 115.02 9.64 17 -1 -5 32.61 3.72 17 1 -5 30.09 4.88 17 -1 -4 194.60 12.01 17 1 -4 163.19 12.03 17 -1 -3 186.69 13.17 17 1 -3 190.33 13.54 17 1 -2 95.68 10.00 17 1 -1 15.21 6.15 17 -1 0 107.39 11.06 17 1 0 104.49 10.18 17 1 1 34.41 6.56 17 1 2 122.60 11.21 17 -1 3 32.72 5.52 17 1 3 32.41 6.83 17 -1 4 56.95 6.35 17 2 -4 13.09 3.63 17 2 -3 80.53 7.36 17 2 -2 70.83 7.33 17 2 -1 131.09 9.63 17 2 0 50.95 6.01 17 2 3 11.45 5.33 17 2 4 70.10 6.42 17 -3 -2 9.47 5.48 17 -3 -1 21.17 5.92 17 -3 0 43.48 5.85 18 0 -3 2.82 3.56 18 0 -2 119.20 9.47 18 0 -1 2.35 4.12 18 0 3 -2.42 3.05 18 -1 -3 46.26 5.15 18 1 -3 45.17 5.18 18 1 -2 91.97 7.56 18 1 -1 5.70 4.04 18 1 1 8.97 4.12 18 1 2 36.14 5.43 18 2 0 17.11 3.73 18 2 1 2.75 3.49 0 0 0 0.00 0.00 TITL 99718 in Pc REM Pc (#7 in standard setting) CELL 1.54184 14.974081 6.384199 10.074134 90.0000 90.4354 90.0000 ZERR 3.00 0.000214 0.000085 0.000136 0.0000 0.0013 0.0000 LATT -1 SYMM x,-y, z+1/2 SFAC C H N Br UNIT 54.00 84.00 9.00 3.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 28799 _shelx_res_file ; TITL 99718_a.res in Pc 99718.res created by SHELXL-2018/3 at 10:58:09 on 15-Jan-2025 REM Old TITL 99718 in Pc REM SHELXT solution in Pc: R1 0.104, Rweak 0.023, Alpha 0.007 REM 0.415 for 183 systematic absences, Orientation as input REM Flack x = 0.294 ( 0.026 ) from 1607 Parsons' quotients REM Formula found by SHELXT: C18 N3 Br CELL 1.54184 14.9741 6.3842 10.0741 90 90.435 90 ZERR 2 0.0002 0.0001 0.0001 0 0.001 0 LATT -1 SYMM +X,-Y,0.5+Z SFAC C H Br N UNIT 36 56 2 6 EQIV $1 +X,-Y,-0.5+Z EQIV $2 +X,1+Y,+Z EQIV $3 +X,1-Y,-0.5+Z L.S. 4 0 0 PLAN 7 TEMP -173 CONF HTAB C1 Br1_$1 HTAB C2 Br1_$2 HTAB C3 Br1_$3 list 4 WPDB -2 MORE -1 BOND $H fmap 2 53 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.095900 0.258300 BASF 0.30905 FVAR 0.89193 BR1 3 0.546560 0.069086 0.654930 11.00000 0.04248 0.02038 = 0.02436 0.00186 0.00457 0.00679 N1 4 0.550000 0.463690 0.378279 11.00000 0.02209 0.02107 = 0.01884 0.00243 0.00196 0.00009 N2 4 0.678294 0.371302 0.453900 11.00000 0.01950 0.02597 = 0.02144 0.00030 -0.00041 0.00453 N3 4 0.661995 0.566623 0.506179 11.00000 0.02296 0.02546 = 0.03375 -0.01127 -0.00729 0.00243 C1 1 0.610149 0.309267 0.380633 11.00000 0.02179 0.02544 = 0.02086 -0.00064 0.00112 0.00079 AFIX 43 H1 2 0.604702 0.177837 0.337098 11.00000 -1.20000 AFIX 0 C2 1 0.584896 0.617629 0.457593 11.00000 0.02567 0.01699 = 0.03690 -0.00681 0.00038 0.00216 AFIX 43 H2 2 0.555844 0.746944 0.474936 11.00000 -1.20000 AFIX 0 C3 1 0.464719 0.459030 0.307031 11.00000 0.02054 0.01599 = 0.02414 -0.00379 -0.00204 -0.00343 AFIX 23 H3A 2 0.454105 0.316252 0.271962 11.00000 -1.20000 H3B 2 0.467148 0.556569 0.230747 11.00000 -1.20000 AFIX 0 C4 1 0.388305 0.520586 0.396565 11.00000 0.02224 0.02242 = 0.01899 0.00045 -0.00285 -0.00329 C5 1 0.352828 0.374055 0.485017 11.00000 0.03162 0.01517 = 0.03087 -0.00005 0.00297 0.00267 AFIX 43 H5 2 0.378248 0.238097 0.491755 11.00000 -1.20000 AFIX 0 C6 1 0.280174 0.428440 0.563011 11.00000 0.02535 0.03089 = 0.02581 0.00636 -0.00075 -0.00184 AFIX 43 H6 2 0.256577 0.327384 0.622421 11.00000 -1.20000 AFIX 0 C7 1 0.240724 0.626363 0.557025 11.00000 0.02018 0.02385 = 0.02252 -0.00012 0.00192 -0.00098 C8 1 0.279831 0.772546 0.472192 11.00000 0.03168 0.02477 = 0.03583 0.00774 0.01002 0.00729 AFIX 43 H8 2 0.256487 0.910800 0.468385 11.00000 -1.20000 AFIX 0 C9 1 0.352695 0.719565 0.392680 11.00000 0.03156 0.01901 = 0.03596 0.01171 0.00386 0.00407 AFIX 43 H9 2 0.377835 0.821754 0.335496 11.00000 -1.20000 AFIX 0 C10 1 0.158664 0.684920 0.639538 11.00000 0.02042 0.03842 = 0.02243 -0.00110 0.00126 0.00464 C11 1 0.122790 0.500401 0.717666 11.00000 0.05454 0.05407 = 0.09379 0.01260 0.05260 0.00676 AFIX 137 H11A 2 0.171894 0.432843 0.766215 11.00000 -1.50000 H11B 2 0.095357 0.399365 0.656521 11.00000 -1.50000 H11C 2 0.077949 0.549817 0.780724 11.00000 -1.50000 AFIX 0 C12 1 0.086153 0.773436 0.550455 11.00000 0.03272 0.14050 = 0.03730 0.01715 0.00649 0.03765 AFIX 137 H12A 2 0.110278 0.890299 0.498836 11.00000 -1.50000 H12B 2 0.036538 0.823367 0.604882 11.00000 -1.50000 H12C 2 0.064673 0.663981 0.489943 11.00000 -1.50000 AFIX 0 C13 1 0.186813 0.853098 0.739684 11.00000 0.04138 0.07584 = 0.05343 -0.02478 0.01297 0.00310 AFIX 137 H13A 2 0.236811 0.801050 0.793659 11.00000 -1.50000 H13B 2 0.136364 0.886337 0.797395 11.00000 -1.50000 H13C 2 0.205292 0.979608 0.692129 11.00000 -1.50000 AFIX 0 C14 1 0.757996 0.254072 0.489958 11.00000 0.02283 0.02739 = 0.02546 0.00272 -0.00048 0.00573 AFIX 23 H14A 2 0.742071 0.103995 0.496963 11.00000 -1.20000 H14B 2 0.778492 0.300990 0.578763 11.00000 -1.20000 AFIX 0 C15 1 0.835610 0.276070 0.392720 11.00000 0.02709 0.02771 = 0.03102 0.00807 0.00092 0.00872 C16 1 0.810111 0.179065 0.260290 11.00000 0.04051 0.05794 = 0.02789 -0.00616 -0.00107 0.01450 AFIX 137 H16A 2 0.792902 0.032522 0.273682 11.00000 -1.50000 H16B 2 0.861192 0.185658 0.200193 11.00000 -1.50000 H16C 2 0.759767 0.256349 0.221446 11.00000 -1.50000 AFIX 0 C17 1 0.859014 0.508702 0.376364 11.00000 0.02741 0.04563 = 0.06540 0.01458 0.00725 0.00195 AFIX 137 H17A 2 0.807805 0.583173 0.337805 11.00000 -1.50000 H17B 2 0.910499 0.522528 0.317528 11.00000 -1.50000 H17C 2 0.873678 0.568915 0.463317 11.00000 -1.50000 AFIX 0 C18 1 0.913941 0.156130 0.453428 11.00000 0.02600 0.04580 = 0.04049 0.00558 -0.00242 0.00842 AFIX 137 H18A 2 0.928094 0.213916 0.541221 11.00000 -1.50000 H18B 2 0.966108 0.169448 0.395882 11.00000 -1.50000 H18C 2 0.897962 0.007942 0.462197 11.00000 -1.50000 AFIX 0 HKLF 4 REM 99718_a.res in Pc REM wR2 = 0.1354, GooF = S = 1.147, Restrained GooF = 1.147 for all data REM R1 = 0.0428 for 3564 Fo > 4sig(Fo) and 0.0454 for all 3683 data REM 206 parameters refined using 2 restraints END WGHT 0.0959 0.2583 REM Highest difference peak 0.766, deepest hole -0.869, 1-sigma level 0.082 Q1 1 0.4813 0.1596 0.6402 11.00000 0.05 0.77 Q2 1 0.4821 -0.0148 0.6386 11.00000 0.05 0.72 Q3 1 0.4854 0.0389 0.6569 11.00000 0.05 0.70 Q4 1 0.6123 -0.0226 0.6746 11.00000 0.05 0.69 Q5 1 0.6127 0.1400 0.6651 11.00000 0.05 0.66 Q6 1 0.6037 0.0466 0.6474 11.00000 0.05 0.65 Q7 1 0.5636 0.0629 0.7608 11.00000 0.05 0.43 ; _shelx_res_checksum 91963 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, 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 0.54656(4) 0.06909(7) 0.65493(5) 0.0291(2) Uani d 1 . . N N1 0.5500(4) 0.4637(8) 0.3783(5) 0.0207(10) Uani d 1 . . N N2 0.6783(3) 0.3713(9) 0.4539(5) 0.0223(9) Uani d 1 . . N N3 0.6620(4) 0.5666(8) 0.5062(7) 0.0274(14) Uani d 1 . . C C1 0.6101(3) 0.3093(10) 0.3806(6) 0.0227(11) Uani d 1 . . H H1 0.604702 0.177837 0.337098 0.027 Uiso calc 1 . . C C2 0.5849(4) 0.6176(10) 0.4576(7) 0.0265(12) Uani d 1 . . H H2 0.555844 0.746944 0.474936 0.032 Uiso calc 1 . . C C3 0.4647(5) 0.4590(10) 0.3070(7) 0.0202(12) Uani d 1 . . H H3A 0.454105 0.316252 0.271962 0.024 Uiso calc 1 . . H H3B 0.467148 0.556569 0.230747 0.024 Uiso calc 1 . . C C4 0.3883(4) 0.5206(10) 0.3966(6) 0.0212(11) Uani d 1 . . C C5 0.3528(4) 0.3741(10) 0.4850(7) 0.0259(11) Uani d 1 . . H H5 0.378248 0.238097 0.491755 0.031 Uiso calc 1 . . C C6 0.2802(4) 0.4284(9) 0.5630(7) 0.0274(14) Uani d 1 . . H H6 0.256577 0.327384 0.622421 0.033 Uiso calc 1 . . C C7 0.2407(4) 0.6264(10) 0.5570(6) 0.0222(10) Uani d 1 . . C C8 0.2798(4) 0.7725(11) 0.4722(8) 0.0307(13) Uani d 1 . . H H8 0.256487 0.910800 0.468385 0.037 Uiso calc 1 . . C C9 0.3527(4) 0.7196(9) 0.3927(7) 0.0288(13) Uani d 1 . . H H9 0.377835 0.821754 0.335496 0.035 Uiso calc 1 . . C C10 0.1587(4) 0.6849(11) 0.6395(6) 0.0271(12) Uani d 1 . . C C11 0.1228(7) 0.5004(18) 0.7177(13) 0.067(3) Uani d 1 . . H H11A 0.171894 0.432843 0.766215 0.101 Uiso calc 1 . . H H11B 0.095357 0.399365 0.656521 0.101 Uiso calc 1 . . H H11C 0.077949 0.549817 0.780724 0.101 Uiso calc 1 . . C C12 0.0862(5) 0.773(2) 0.5505(9) 0.070(3) Uani d 1 . . H H12A 0.110278 0.890299 0.498836 0.105 Uiso calc 1 . . H H12B 0.036538 0.823367 0.604882 0.105 Uiso calc 1 . . H H12C 0.064673 0.663981 0.489943 0.105 Uiso calc 1 . . C C13 0.1868(6) 0.8531(18) 0.7397(10) 0.057(2) Uani d 1 . . H H13A 0.236811 0.801050 0.793659 0.085 Uiso calc 1 . . H H13B 0.136364 0.886337 0.797395 0.085 Uiso calc 1 . . H H13C 0.205292 0.979608 0.692129 0.085 Uiso calc 1 . . C C14 0.7580(4) 0.2541(10) 0.4900(6) 0.0252(11) Uani d 1 . . H H14A 0.742071 0.103995 0.496963 0.030 Uiso calc 1 . . H H14B 0.778492 0.300990 0.578763 0.030 Uiso calc 1 . . C C15 0.8356(4) 0.2761(11) 0.3927(7) 0.0286(13) Uani d 1 . . C C16 0.8101(5) 0.1791(14) 0.2603(8) 0.0421(17) Uani d 1 . . H H16A 0.792902 0.032522 0.273682 0.063 Uiso calc 1 . . H H16B 0.861192 0.185658 0.200193 0.063 Uiso calc 1 . . H H16C 0.759767 0.256349 0.221446 0.063 Uiso calc 1 . . C C17 0.8590(5) 0.5087(15) 0.3764(10) 0.0461(18) Uani d 1 . . H H17A 0.807805 0.583173 0.337805 0.069 Uiso calc 1 . . H H17B 0.910499 0.522528 0.317528 0.069 Uiso calc 1 . . H H17C 0.873678 0.568915 0.463317 0.069 Uiso calc 1 . . C C18 0.9139(4) 0.1561(13) 0.4534(8) 0.0374(15) Uani d 1 . . H H18A 0.928094 0.213916 0.541221 0.056 Uiso calc 1 . . H H18B 0.966108 0.169448 0.395882 0.056 Uiso calc 1 . . H H18C 0.897962 0.007942 0.462197 0.056 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 0.0425(3) 0.0204(3) 0.0244(3) 0.0068(3) 0.0046(2) 0.0019(3) N1 0.022(2) 0.021(3) 0.019(3) 0.0001(19) 0.002(2) 0.0024(19) N2 0.019(2) 0.026(2) 0.021(2) 0.005(2) -0.0004(17) 0.000(2) N3 0.023(3) 0.025(3) 0.034(3) 0.0024(18) -0.007(3) -0.011(2) C1 0.022(2) 0.025(3) 0.021(3) 0.001(2) 0.0011(19) -0.001(2) C2 0.026(3) 0.017(2) 0.037(3) 0.002(3) 0.000(2) -0.007(3) C3 0.021(3) 0.016(2) 0.024(3) -0.003(2) -0.002(2) -0.004(2) C4 0.022(2) 0.022(3) 0.019(3) -0.003(2) -0.003(2) 0.000(2) C5 0.032(3) 0.015(2) 0.031(3) 0.003(2) 0.003(2) 0.000(2) C6 0.025(3) 0.031(4) 0.026(3) -0.002(2) -0.001(2) 0.006(2) C7 0.020(2) 0.024(3) 0.023(3) -0.001(2) 0.0019(19) 0.000(2) C8 0.032(3) 0.025(3) 0.036(4) 0.007(2) 0.010(3) 0.008(3) C9 0.032(3) 0.019(3) 0.036(3) 0.004(2) 0.004(2) 0.012(3) C10 0.020(2) 0.038(3) 0.022(3) 0.005(2) 0.001(2) -0.001(2) C11 0.055(5) 0.054(5) 0.094(8) 0.007(4) 0.053(5) 0.013(6) C12 0.033(3) 0.141(10) 0.037(4) 0.038(5) 0.006(3) 0.017(5) C13 0.041(4) 0.076(6) 0.053(5) 0.003(4) 0.013(3) -0.025(5) C14 0.023(2) 0.027(3) 0.025(3) 0.006(2) 0.000(2) 0.003(2) C15 0.027(3) 0.028(3) 0.031(3) 0.009(2) 0.001(2) 0.008(3) C16 0.041(3) 0.058(5) 0.028(4) 0.015(3) -0.001(3) -0.006(3) C17 0.027(3) 0.046(4) 0.065(5) 0.002(3) 0.007(3) 0.015(4) C18 0.026(3) 0.046(4) 0.040(4) 0.008(3) -0.002(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 C1 N1 C2 . . 105.4(5) ? C1 N1 C3 . . 125.5(5) ? C2 N1 C3 . . 129.1(5) ? N3 N2 C14 . . 121.3(5) ? C1 N2 N3 . . 110.4(5) ? C1 N2 C14 . . 128.1(6) ? C2 N3 N2 . . 104.1(5) ? N1 C1 H1 . . 126.0 ? N2 C1 N1 . . 107.9(5) ? N2 C1 H1 . . 126.0 ? N1 C2 H2 . . 123.9 ? N3 C2 N1 . . 112.1(6) ? N3 C2 H2 . . 123.9 ? N1 C3 H3A . . 109.4 ? N1 C3 H3B . . 109.4 ? N1 C3 C4 . . 111.3(5) ? H3A C3 H3B . . 108.0 ? C4 C3 H3A . . 109.4 ? C4 C3 H3B . . 109.4 ? C5 C4 C3 . . 119.9(6) ? C9 C4 C3 . . 121.1(6) ? C9 C4 C5 . . 119.1(6) ? C4 C5 H5 . . 120.2 ? C6 C5 C4 . . 119.7(6) ? C6 C5 H5 . . 120.2 ? C5 C6 H6 . . 118.9 ? C5 C6 C7 . . 122.3(6) ? C7 C6 H6 . . 118.9 ? C6 C7 C8 . . 116.9(5) ? C6 C7 C10 . . 122.5(6) ? C8 C7 C10 . . 120.6(6) ? C7 C8 H8 . . 119.3 ? C7 C8 C9 . . 121.4(6) ? C9 C8 H8 . . 119.3 ? C4 C9 C8 . . 120.6(6) ? C4 C9 H9 . . 119.7 ? C8 C9 H9 . . 119.7 ? C11 C10 C7 . . 112.3(6) ? C11 C10 C13 . . 107.4(8) ? C12 C10 C7 . . 110.1(5) ? C12 C10 C11 . . 110.0(8) ? C12 C10 C13 . . 108.8(8) ? C13 C10 C7 . . 108.1(5) ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11B . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C10 C12 H12A . . 109.5 ? C10 C12 H12B . . 109.5 ? C10 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C10 C13 H13A . . 109.5 ? C10 C13 H13B . . 109.5 ? C10 C13 H13C . . 109.5 ? H13A C13 H13B . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? N2 C14 H14A . . 108.6 ? N2 C14 H14B . . 108.6 ? N2 C14 C15 . . 114.8(5) ? H14A C14 H14B . . 107.6 ? C15 C14 H14A . . 108.6 ? C15 C14 H14B . . 108.6 ? C14 C15 C17 . . 109.4(6) ? C16 C15 C14 . . 109.7(6) ? C16 C15 C17 . . 110.9(7) ? C16 C15 C18 . . 109.6(6) ? C18 C15 C14 . . 106.4(5) ? C18 C15 C17 . . 110.7(6) ? C15 C16 H16A . . 109.5 ? C15 C16 H16B . . 109.5 ? C15 C16 H16C . . 109.5 ? H16A C16 H16B . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? C15 C17 H17A . . 109.5 ? C15 C17 H17B . . 109.5 ? C15 C17 H17C . . 109.5 ? H17A C17 H17B . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C15 C18 H18A . . 109.5 ? C15 C18 H18B . . 109.5 ? C15 C18 H18C . . 109.5 ? H18A C18 H18B . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? 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 N1 C1 . 1.335(7) ? N1 C2 . 1.368(9) ? N1 C3 . 1.460(8) ? N2 N3 . 1.376(8) ? N2 C1 . 1.316(8) ? N2 C14 . 1.453(7) ? N3 C2 . 1.292(9) ? C1 H1 . 0.9500 ? C2 H2 . 0.9500 ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C3 C4 . 1.514(9) ? C4 C5 . 1.399(9) ? C4 C9 . 1.378(8) ? C5 H5 . 0.9500 ? C5 C6 . 1.391(9) ? C6 H6 . 0.9500 ? C6 C7 . 1.396(9) ? C7 C8 . 1.397(9) ? C7 C10 . 1.535(7) ? C8 H8 . 0.9500 ? C8 C9 . 1.400(9) ? C9 H9 . 0.9500 ? C10 C11 . 1.517(12) ? C10 C12 . 1.513(10) ? C10 C13 . 1.530(11) ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C13 H13C . 0.9800 ? C14 H14A . 0.9900 ? C14 H14B . 0.9900 ? C14 C15 . 1.532(8) ? C15 C16 . 1.517(11) ? C15 C17 . 1.535(11) ? C15 C18 . 1.525(8) ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C16 H16C . 0.9800 ? C17 H17A . 0.9800 ? C17 H17B . 0.9800 ? C17 H17C . 0.9800 ? C18 H18A . 0.9800 ? C18 H18B . 0.9800 ? C18 H18C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C1 H1 Br1 2_554 0.95 2.57 3.446(6) 154 yes C2 H2 Br1 1_565 0.95 2.75 3.550(6) 143 yes C3 H3B Br1 2_564 0.99 2.78 3.599(7) 141 yes 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 N1 C3 C4 C5 . . . . -79.6(7) ? N1 C3 C4 C9 . . . . 100.4(7) ? N2 N3 C2 N1 . . . . 1.0(8) ? N2 C14 C15 C16 . . . . -65.7(7) ? N2 C14 C15 C17 . . . . 56.2(8) ? N2 C14 C15 C18 . . . . 175.8(6) ? N3 N2 C1 N1 . . . . 2.6(7) ? N3 N2 C14 C15 . . . . -96.1(7) ? C1 N1 C2 N3 . . . . 0.6(8) ? C1 N1 C3 C4 . . . . 129.5(6) ? C1 N2 N3 C2 . . . . -2.2(8) ? C1 N2 C14 C15 . . . . 89.9(8) ? C2 N1 C1 N2 . . . . -1.9(7) ? C2 N1 C3 C4 . . . . -48.7(9) ? C3 N1 C1 N2 . . . . 179.5(6) ? C3 N1 C2 N3 . . . . 179.1(7) ? C3 C4 C5 C6 . . . . -177.3(6) ? C3 C4 C9 C8 . . . . 177.5(7) ? C4 C5 C6 C7 . . . . -0.2(10) ? C5 C4 C9 C8 . . . . -2.5(10) ? C5 C6 C7 C8 . . . . -2.5(10) ? C5 C6 C7 C10 . . . . 178.0(6) ? C6 C7 C8 C9 . . . . 2.8(10) ? C6 C7 C10 C11 . . . . -4.4(10) ? C6 C7 C10 C12 . . . . -127.4(8) ? C6 C7 C10 C13 . . . . 114.0(8) ? C7 C8 C9 C4 . . . . -0.3(12) ? C8 C7 C10 C11 . . . . 176.1(8) ? C8 C7 C10 C12 . . . . 53.1(10) ? C8 C7 C10 C13 . . . . -65.6(8) ? C9 C4 C5 C6 . . . . 2.7(9) ? C10 C7 C8 C9 . . . . -177.7(6) ? C14 N2 N3 C2 . . . . -177.2(6) ? C14 N2 C1 N1 . . . . 177.2(6) ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.69(4) 2 0.31(4)