#------------------------------------------------------------------------------ #$Date: 2025-04-05 13:40:53 +0200 (Sat, 05 Apr 2025) $ #$Revision: 299190 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023407.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_2023407 loop_ _publ_author_name 'Mewis, Ryan E.' 'Hulme, Matthew C.' 'Marron, Jack' 'Langley, Stuart K.' 'Sutcliffe, Oliver B.' 'Benjamin, Sophie L.' _publ_section_title ; Synthesis and crystal structures of five fluorinated diphenidine derivatives. ; _journal_coeditor_code EE2011 _journal_issue 'Pt 3' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 229 _journal_page_last 234 _journal_paper_doi 10.1107/S2056989025001288 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C18 H20 F2 N +, Cl -' _chemical_formula_moiety 'C18 H20 F2 N +, Cl -' _chemical_formula_sum 'C18 H20 Cl F2 N' _chemical_formula_weight 323.80 _chemical_name_systematic ; 1-[1-(2,6-Difluorophenyl)-2-phenylethyl]pyrrolidin-1-ium chloride ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 88.059(5) _cell_angle_beta 82.349(4) _cell_angle_gamma 86.140(5) _cell_formula_units_Z 4 _cell_length_a 8.1365(4) _cell_length_b 12.7421(10) _cell_length_c 16.0451(8) _cell_measurement_reflns_used 9872 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 25.43 _cell_measurement_theta_min 2.99 _cell_volume 1644.42(17) _computing_cell_refinement 'CrysAlisPro (Agilent, 2014)' _computing_data_collection 'CrysAlisPro (Agilent, 2014)' _computing_data_reduction 'CrysAlisPro (Agilent, 2014)' _computing_molecular_graphics ; X-SEED (Barbour, 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method 'scans in phi and omega' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 13277 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.988 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.308 _exptl_crystal_description block _exptl_crystal_F_000 680 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.585 _refine_diff_density_min -0.338 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 5775 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.185 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0896 _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^)+(0.0143P)^2^+10.4102P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2001 _refine_ls_wR_factor_ref 0.2059 _reflns_number_gt 4892 _reflns_number_total 5775 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ee2011.cif _cod_data_source_block IV _cod_depositor_comments 'Adding full bibliography for 2023405--2023409.cif.' _cod_database_code 2023407 _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 -3 56.45 3.12 0 0 -3 56.36 3.59 0 0 -4 1964.24 22.98 0 0 -4 1795.26 19.56 0 0 -5 23.41 2.87 0 0 -5 29.23 3.60 0 0 -6 739.32 15.56 0 0 -6 817.51 18.61 0 0 -7 146.04 8.63 0 0 -7 132.03 7.09 0 0 8 526.59 17.14 0 0 -8 492.43 14.43 0 0 -8 510.56 17.08 0 0 -9 154.12 8.76 0 0 -10 331.90 13.47 0 0 10 340.15 15.44 0 0 11 72.87 8.14 0 0 -11 80.40 7.24 0 0 12 9.76 4.06 0 0 -12 8.27 4.00 0 0 -13 101.44 8.71 0 0 -13 93.33 4.60 0 0 13 103.50 10.44 0 0 14 47.22 7.61 0 0 -14 49.91 7.11 0 0 -15 115.29 10.42 0 0 -16 145.88 12.71 0 0 -17 23.02 5.89 0 0 17 26.98 7.02 0 0 -18 121.62 11.36 0 0 18 118.89 13.18 0 0 19 127.13 14.29 0 0 -19 103.07 11.30 0 0 20 22.87 7.51 0 -1 20 67.54 10.93 0 1 -19 18.23 6.96 0 -1 19 23.10 7.48 0 1 -18 201.23 15.31 0 1 -17 27.60 9.37 0 -1 16 160.68 14.61 0 1 -16 169.74 13.13 0 1 -15 35.89 6.37 0 -1 15 33.27 6.98 0 -1 14 287.06 17.55 0 1 -14 319.18 16.24 0 1 -13 41.88 6.51 0 -1 13 28.33 6.28 0 1 -12 2.03 3.08 0 -1 12 1.86 4.38 0 -1 11 8.86 4.57 0 1 -11 5.58 3.38 0 1 -10 316.54 13.53 0 1 -10 256.86 5.72 0 1 -10 251.05 5.66 0 1 -9 48.99 5.42 0 -1 9 55.50 5.66 0 -1 8 1245.61 26.42 0 1 -8 1194.39 23.36 0 -1 8 1280.28 23.82 0 1 -7 334.05 13.37 0 -1 7 326.65 12.66 0 1 -7 330.67 11.78 0 -1 7 375.22 12.24 0 1 -6 722.67 17.63 0 -1 6 746.74 17.66 0 1 -6 714.19 15.83 0 -1 6 754.97 16.01 0 -1 5 1233.15 20.81 0 1 -5 1197.26 18.94 0 1 -5 1253.76 21.66 0 -1 5 1265.46 19.57 0 1 -4 1343.21 18.08 0 -1 4 1313.69 19.29 0 1 -4 1324.88 19.76 0 -1 3 915.61 14.80 0 1 -3 881.95 14.03 0 -1 2 550.78 8.39 0 1 2 346.89 5.83 0 1 3 2003.05 14.16 0 -1 -3 1998.99 19.43 0 -1 -4 708.32 7.86 0 -1 -4 817.49 14.77 0 -1 -4 838.45 9.35 0 -1 -5 1564.79 22.88 0 -1 -5 1566.07 12.83 0 -1 -5 1514.47 12.27 0 1 5 1475.04 12.58 0 -1 -6 167.94 4.51 0 -1 -6 194.31 4.85 0 -1 -6 215.67 10.14 0 -1 -6 159.44 7.68 0 -1 -7 628.60 8.68 0 -1 -7 695.67 18.05 0 -1 -7 673.51 15.80 0 -1 -7 661.32 9.39 0 1 7 709.48 18.03 0 1 8 113.84 8.53 0 -1 -8 114.98 9.79 0 -1 -8 85.56 3.74 0 -1 -8 97.53 3.58 0 -1 -8 108.81 7.68 0 -1 -9 15.25 1.75 0 -1 -9 13.91 2.90 0 1 9 17.33 4.08 0 -1 -10 125.64 4.62 0 -1 -10 131.41 8.63 0 1 10 136.97 9.91 0 -1 -11 202.41 5.80 0 1 11 245.13 13.66 0 -1 -11 233.49 11.75 0 -1 -12 2.70 1.08 0 -1 -12 2.58 2.70 0 1 12 2.63 3.11 0 1 12 -2.05 3.76 0 1 13 31.79 5.80 0 -1 -13 40.72 5.88 0 1 14 164.47 13.03 0 -1 -14 171.95 11.82 0 -1 -15 80.26 8.68 0 1 15 76.49 9.90 0 -1 -16 256.08 15.60 0 1 16 272.34 18.22 0 1 17 9.09 6.44 0 -1 -17 2.60 3.66 0 1 18 30.69 8.06 0 -1 -18 24.09 7.47 0 1 19 35.09 9.25 0 -1 -19 13.25 5.59 0 1 20 1.92 5.33 0 2 -20 16.21 6.34 0 2 -19 78.98 11.14 0 2 -18 -0.39 4.73 0 -2 18 24.33 8.40 0 2 -17 30.04 6.78 0 -2 17 47.82 9.84 0 2 -16 60.32 10.16 0 -2 16 54.48 9.49 0 -2 15 7.34 5.50 0 2 -15 9.39 6.05 0 -2 14 3.85 5.01 0 2 -14 10.38 4.98 0 -2 13 246.56 15.84 0 2 -13 264.66 14.63 0 2 -12 10.91 1.63 0 -2 12 21.45 5.90 0 2 -12 14.55 4.41 0 2 -11 255.08 13.42 0 -2 11 272.22 15.37 0 2 -11 243.60 7.07 0 2 -10 1218.69 16.37 0 2 -10 1190.40 27.36 0 -2 9 398.31 14.92 0 2 -9 385.06 14.92 0 2 -8 0.65 1.99 0 -2 8 2.11 2.77 0 -2 7 7.58 2.41 0 -2 7 4.58 2.43 0 2 -7 4.58 2.19 0 2 -7 5.62 2.75 0 -2 6 104.72 7.14 0 2 -6 106.92 6.72 0 -2 6 117.77 6.93 0 2 -6 112.42 7.45 0 -2 5 505.99 13.93 0 -2 5 511.68 12.91 0 -2 5 502.42 14.44 0 2 -5 497.80 13.37 0 2 -5 498.38 14.61 0 2 -4 128.29 6.37 0 2 -4 125.73 6.50 0 -2 4 124.00 6.51 0 -2 4 135.06 5.96 0 -2 3 36.77 3.08 0 2 -3 43.98 3.96 0 2 -3 41.84 3.84 0 2 -2 4666.31 30.82 0 -2 2 4576.12 27.79 0 2 -2 4716.54 33.01 0 2 -1 659.00 11.58 0 -2 0 519.96 9.18 0 2 1 732.06 11.92 0 -2 -1 764.90 11.47 0 2 2 4849.05 30.40 0 -2 -2 4846.79 32.02 0 -2 -2 4893.90 32.16 0 2 3 92.86 4.42 0 -2 -3 101.67 5.31 0 -2 -4 2.34 2.45 0 2 4 2.06 2.26 0 2 4 1.91 1.96 0 -2 -4 4.40 2.60 0 -2 -4 7.92 2.33 0 2 5 843.88 12.77 0 -2 -5 852.23 16.59 0 2 5 817.82 10.90 0 -2 -5 851.07 12.72 0 -2 -6 77.58 3.97 0 -2 -6 81.14 5.90 0 2 6 76.68 3.94 0 2 7 1.10 1.37 0 -2 -7 0.06 2.54 0 -2 -7 1.93 1.27 0 -2 -8 11.75 3.87 0 2 8 5.45 1.32 0 -2 -9 416.20 14.31 0 -2 -10 108.83 8.48 0 2 10 102.28 9.12 0 2 11 4.10 3.55 0 -2 -11 9.79 3.46 0 -2 -12 298.24 13.89 0 2 12 307.56 16.27 0 -2 -13 484.78 18.54 0 2 13 502.85 21.76 0 2 14 75.43 9.92 0 -2 -14 60.30 7.70 0 -2 -15 24.63 5.25 0 2 15 22.33 5.86 0 2 16 3.68 5.59 0 -2 -16 9.13 6.01 0 2 17 300.98 19.95 0 -2 -17 303.29 17.28 0 -2 -18 21.33 7.58 0 2 18 20.91 8.93 0 -2 -19 25.39 6.33 0 2 19 40.60 9.09 0 2 20 26.77 8.60 0 3 -20 15.97 6.17 0 3 -19 50.34 9.24 0 -3 19 42.78 9.14 0 -3 18 13.21 7.02 0 3 -18 10.58 6.21 0 3 -17 8.48 6.21 0 -3 17 12.63 6.78 0 -3 16 38.69 7.52 0 3 -16 32.04 6.44 0 3 -15 -0.70 3.16 0 -3 15 3.27 4.24 0 3 -14 49.09 7.41 0 -3 14 38.84 7.54 0 -3 13 305.78 17.72 0 3 -13 256.37 8.09 0 3 -13 313.17 16.40 0 3 -12 85.94 5.15 0 3 -12 106.07 9.80 0 -3 12 97.36 9.92 0 3 -11 261.16 14.10 0 3 -11 259.33 9.00 0 -3 11 264.83 15.13 0 3 -10 28.41 3.39 0 3 -10 21.08 4.59 0 3 -9 7.54 3.36 0 3 -9 5.92 3.10 0 -3 9 11.45 3.94 0 -3 8 454.43 15.97 0 -3 8 463.15 15.55 0 3 -8 445.85 16.85 0 3 -8 445.12 16.14 0 -3 7 364.43 13.61 0 3 -7 345.33 13.34 0 -3 7 359.78 12.74 0 -3 7 347.72 14.28 0 3 -7 360.94 14.57 0 3 -6 1436.61 26.08 0 3 -6 1420.25 26.89 0 -3 6 1472.41 27.40 0 -3 6 1483.77 24.01 0 -3 6 1481.74 26.10 0 3 -5 170.25 8.93 0 3 -5 166.25 8.52 0 -3 5 165.27 7.47 0 -3 5 168.06 8.61 0 3 -4 223.04 9.20 0 -3 4 221.10 8.07 0 3 -4 209.19 8.02 0 3 -4 223.03 9.36 0 3 -3 2778.28 30.00 0 -3 3 2841.90 26.92 0 3 -3 2816.01 27.06 0 3 -3 2838.48 32.63 0 3 -2 69.53 5.20 0 3 -1 1006.60 17.33 0 -3 0 61.85 4.11 0 -3 0 62.37 4.27 0 3 0 61.44 4.58 0 3 1 467.56 11.82 0 -3 -1 472.85 11.15 0 -3 -1 495.02 11.28 0 3 2 84.32 5.30 0 -3 -2 87.63 5.15 0 -3 -2 98.21 5.57 0 -3 -3 4671.28 38.45 0 -3 -3 4597.28 38.23 0 3 3 4533.69 36.33 0 -3 -4 59.48 4.90 0 3 4 54.96 4.70 0 -3 -4 55.97 5.32 0 3 5 144.54 5.82 0 -3 -5 147.70 7.17 0 -3 -5 151.66 8.32 0 -3 -5 150.11 6.81 0 3 5 143.41 6.71 0 3 6 600.43 13.49 0 -3 -6 684.85 16.65 0 3 6 598.11 11.62 0 -3 -6 627.69 13.94 0 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0 4 -10 1.23 2.75 0 4 -9 416.17 13.41 0 -4 9 414.50 15.69 0 4 -9 389.81 17.34 0 4 -9 393.97 16.77 0 -4 8 0.08 2.58 0 4 -8 3.56 2.70 0 4 -8 -1.21 2.45 0 4 -8 2.78 2.72 0 4 -7 843.59 22.88 0 4 -7 887.68 19.37 0 -4 7 870.96 20.27 0 4 -7 836.53 22.58 0 -4 6 343.66 13.79 0 4 -6 326.08 13.60 0 -4 6 329.34 11.78 0 4 -6 320.64 13.60 0 4 -5 60.37 6.28 0 -4 5 66.92 5.38 0 4 -5 59.06 5.42 0 4 -5 68.69 6.27 0 -4 4 71.67 5.53 0 4 -4 68.98 5.80 0 4 -4 55.82 7.28 0 -4 3 315.37 10.06 0 4 -3 351.79 11.91 0 4 -3 335.34 10.21 0 4 -3 331.67 12.09 0 -4 3 321.36 10.48 0 -4 2 2985.69 29.77 0 4 -2 3129.25 30.22 0 4 -2 3066.85 35.90 0 4 -2 3065.47 35.32 0 4 -1 101.28 6.60 0 -4 0 305.63 10.19 0 -4 0 308.05 10.17 0 4 0 320.23 11.28 0 -4 -1 167.62 7.66 0 -4 -1 169.72 7.71 0 4 1 156.99 8.04 0 -4 -2 3749.08 36.33 0 4 2 3744.87 38.13 0 -4 -2 3802.29 36.77 0 4 3 39.41 5.30 0 -4 -3 48.04 5.30 0 -4 -3 36.66 5.15 0 -4 -4 677.00 16.83 0 -4 -4 646.77 16.77 0 4 4 623.66 15.58 0 4 5 193.94 8.87 0 -4 -5 203.53 9.97 0 -4 -6 36.22 5.38 0 4 6 32.30 4.39 0 4 6 36.92 3.98 0 -4 -6 47.10 5.12 0 4 7 31.10 4.37 0 4 7 30.69 3.76 0 -4 -7 52.21 6.28 0 4 8 278.89 8.81 0 4 8 285.06 10.41 0 -4 -8 289.40 12.32 0 4 9 104.33 6.47 0 4 10 241.33 9.30 0 4 10 229.06 13.51 0 4 11 2.98 2.48 0 4 11 1.06 3.09 0 4 12 10.87 2.39 0 4 12 8.44 4.08 0 4 13 0.45 3.34 0 -4 -13 -4.39 2.64 0 -4 -14 28.83 5.56 0 4 14 25.50 5.83 0 -4 -15 23.17 5.08 0 4 15 46.76 8.08 0 -4 -16 2.74 3.73 0 4 16 1.88 4.64 0 4 17 139.56 13.99 0 -4 -17 131.58 11.40 0 4 18 52.77 9.66 0 -4 -18 57.56 8.70 0 4 19 10.20 6.93 0 5 -20 79.35 11.83 0 5 -19 7.36 6.07 0 -5 18 65.85 11.46 0 5 -18 79.30 11.21 0 5 -17 8.18 5.73 0 -5 17 -3.61 4.83 0 -5 16 3.81 5.00 0 5 -16 18.35 6.33 0 -5 15 24.26 7.10 0 5 -15 13.72 5.07 0 5 -14 175.89 13.93 0 -5 14 156.08 14.02 0 -5 13 19.00 5.41 0 5 -13 21.50 6.02 0 -5 12 49.90 8.06 0 5 -12 43.46 5.05 0 5 -12 53.80 7.74 0 5 -11 17.01 3.71 0 -5 11 14.83 5.27 0 5 -11 15.29 4.65 0 5 -11 19.77 4.77 0 5 -10 41.99 5.26 0 5 -10 46.88 7.04 0 -5 10 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3 159.04 10.02 0 -5 -4 175.39 9.62 0 -5 -4 159.61 9.42 0 5 4 153.01 9.12 0 5 5 2610.64 35.35 0 -5 -5 2751.25 38.57 0 -5 -5 2751.17 38.62 0 5 6 309.55 12.29 0 5 7 3.00 2.34 0 5 7 1.25 2.62 0 -5 -7 1.27 2.32 0 5 8 11.06 2.87 0 5 8 11.94 3.02 0 -5 -8 11.28 3.43 0 5 9 448.25 14.72 0 5 9 456.17 18.60 0 5 9 455.27 12.70 0 5 10 388.71 18.02 0 5 10 384.77 13.41 0 5 11 53.89 5.21 0 5 11 55.23 7.47 0 5 12 7.84 4.41 0 5 12 9.48 2.69 0 5 13 62.53 8.69 0 5 14 47.71 7.81 0 -5 -14 47.21 6.58 0 5 15 17.04 6.61 0 -5 -15 11.68 4.46 0 -5 -16 49.54 7.03 0 5 16 53.84 8.92 0 5 17 13.26 6.47 0 -5 -17 5.61 3.93 0 5 18 5.82 4.73 0 -5 -18 10.49 5.70 0 5 19 38.83 10.18 0 6 -20 9.33 5.52 0 6 -19 6.21 6.40 0 6 -18 0.72 5.95 0 -6 18 5.45 5.60 0 6 -17 7.10 5.71 0 -6 17 19.97 7.21 0 6 -16 2.39 4.84 0 -6 16 9.87 6.16 0 6 -15 10.52 4.63 0 -6 15 8.42 6.10 0 6 -14 4.64 4.78 0 -6 14 4.83 4.33 0 6 -13 108.94 11.26 0 -6 13 86.21 10.74 0 -6 12 127.02 11.87 0 6 -12 121.81 11.56 0 6 -12 113.79 11.26 0 6 -11 84.31 9.59 0 6 -11 64.87 8.67 0 -6 11 80.98 9.45 0 -6 10 12.08 4.85 0 6 -10 9.35 4.38 0 6 -10 0.52 3.18 0 -6 9 17.41 4.84 0 6 -9 18.38 4.90 0 6 -9 22.53 5.03 0 -6 8 290.54 14.70 0 6 -8 294.18 15.81 0 -6 8 287.63 13.35 0 6 -8 297.54 15.70 0 -6 7 367.88 14.72 0 6 -7 367.84 17.26 0 -6 7 373.80 15.92 0 6 -7 371.58 17.20 0 6 -6 4.15 3.23 0 -6 6 5.08 2.93 0 6 -6 3.94 2.72 0 -6 6 2.86 3.09 0 6 -6 0.22 2.69 0 -6 5 85.56 7.34 0 6 -5 69.67 7.02 0 6 -5 83.48 7.85 0 6 -5 88.70 7.76 0 6 -5 85.57 6.74 0 6 -4 678.98 21.36 0 6 -4 666.94 17.52 0 6 -4 695.91 20.68 0 -6 4 667.75 18.01 0 -6 3 453.96 14.25 0 6 -3 497.21 14.98 0 6 -3 445.61 16.84 0 6 -2 51.14 6.01 0 6 -2 55.96 5.14 0 -6 2 44.76 4.41 0 -6 1 40.07 5.18 0 6 -1 43.75 5.64 0 -6 1 40.81 5.24 0 -6 0 1.25 2.35 0 6 0 2.04 2.62 0 -6 0 0.57 2.11 0 -6 -1 54.46 5.77 0 6 1 49.69 5.77 0 -6 -1 42.31 5.15 0 6 2 12.09 3.90 0 -6 -2 13.79 3.21 0 -6 -2 9.69 3.39 0 -6 -3 839.61 21.34 0 6 3 821.44 22.24 0 -6 -3 823.79 21.63 0 6 4 45.01 7.21 0 -6 -4 98.71 9.05 0 -6 -5 26.33 4.61 0 6 5 22.27 4.27 0 6 6 0.22 2.36 0 -6 -7 8.10 3.33 0 6 7 5.10 3.33 0 6 8 36.42 5.18 0 -6 -8 37.27 5.18 0 6 8 39.29 5.02 0 6 9 6.09 3.66 0 6 9 6.70 2.99 0 6 9 6.13 3.76 0 6 10 6.50 4.42 0 6 10 4.34 2.49 0 6 10 4.69 3.15 0 6 11 147.14 9.49 0 6 11 150.66 12.31 0 6 12 101.13 10.79 0 6 13 42.36 7.49 0 6 14 23.32 7.13 0 -6 -15 -2.81 3.63 0 6 15 4.66 5.24 0 -6 -16 -5.34 3.35 0 6 16 6.03 4.38 0 6 17 28.84 7.34 0 -6 -17 10.47 4.04 0 6 18 19.32 6.28 0 6 19 95.39 13.32 0 7 -19 2.50 4.89 0 7 -18 -7.65 4.81 0 7 -17 21.61 7.76 0 -7 17 35.18 8.66 0 7 -16 11.21 6.07 0 -7 16 2.67 5.11 0 7 -15 6.33 5.03 0 -7 15 15.03 6.00 0 7 -14 -2.64 4.45 0 -7 14 -3.84 4.41 0 -7 13 11.46 5.89 0 7 -13 3.90 3.54 0 7 -13 10.03 5.80 0 -7 12 16.64 5.37 0 7 -12 23.88 6.39 0 7 -12 9.43 3.78 0 7 -11 134.09 12.20 0 -7 11 156.58 12.76 0 7 -11 148.60 13.14 0 -7 10 2.72 4.49 0 7 -10 8.23 4.62 0 7 -10 4.91 3.30 0 -7 9 519.48 21.09 0 7 -9 487.17 21.94 0 7 -9 499.35 21.90 0 -7 8 5.73 3.96 0 7 -8 -5.11 4.14 0 7 -8 -0.77 3.61 0 7 -7 1.63 2.62 0 7 -7 2.34 3.07 0 7 -7 -0.28 3.02 0 -7 7 -0.62 3.15 0 -7 6 146.65 10.21 0 7 -6 139.68 10.90 0 7 -6 146.64 11.54 0 7 -6 148.97 9.49 0 7 -5 29.71 4.55 0 -7 5 31.57 4.86 0 7 -5 28.80 5.94 0 -7 4 215.27 10.83 0 7 -4 232.28 11.14 0 -7 3 951.38 21.92 0 7 -3 1013.95 23.16 0 7 -2 0.95 2.23 0 -7 2 0.42 2.41 0 -7 1 490.49 17.24 0 -7 0 0.55 2.42 0 -7 -1 576.26 18.81 0 -7 -2 11.01 3.81 0 -7 -3 2054.62 35.71 0 -7 -4 47.51 6.50 0 -7 -5 84.02 8.06 0 -7 -6 37.33 6.13 0 7 7 26.56 5.44 0 7 8 17.17 4.15 0 7 8 25.54 5.82 0 7 9 21.34 5.68 0 7 9 20.51 4.51 0 7 10 217.49 14.59 0 7 10 216.17 11.09 0 7 11 257.00 16.51 0 7 11 258.55 11.47 0 7 12 4.54 4.64 0 7 13 2.37 4.90 0 7 14 59.04 9.15 0 7 15 6.22 5.00 0 7 16 -4.90 4.30 0 -7 -16 2.34 3.92 0 -7 -17 3.99 4.35 0 7 17 14.96 6.83 0 7 18 131.00 15.14 0 8 -18 5.42 6.80 0 8 -17 104.14 13.58 0 -8 17 103.66 14.00 0 8 -16 1.68 4.20 0 -8 16 5.49 5.64 0 -8 15 15.23 5.98 0 8 -15 17.40 7.15 0 8 -14 0.40 3.81 0 8 -14 3.72 4.25 0 -8 14 3.79 4.32 0 8 -13 1.13 3.72 0 -8 13 7.66 5.49 0 8 -13 6.89 5.11 0 8 -12 50.28 8.79 0 8 -12 44.75 7.85 0 -8 12 46.41 8.21 0 8 -11 131.05 13.25 0 8 -11 120.56 11.95 0 -8 11 124.25 11.99 0 8 -10 9.00 4.84 0 -8 10 13.70 4.69 0 8 -10 1.53 3.32 0 8 -9 144.06 12.93 0 -8 9 153.50 12.20 0 8 -9 136.93 11.99 0 8 -8 242.92 15.88 0 8 -8 241.45 16.21 0 -8 8 228.99 14.09 0 8 -7 38.03 7.25 0 8 -7 35.49 6.05 0 -8 7 48.04 6.75 0 8 -7 44.78 6.07 0 -8 6 124.67 9.71 0 8 -6 134.94 9.59 0 8 -6 113.25 10.39 0 8 -5 646.35 20.05 0 -8 5 611.85 19.76 0 -8 4 497.42 17.22 0 8 -4 507.06 17.57 0 8 -3 46.51 5.73 0 -8 3 55.59 6.01 0 -8 2 298.29 12.65 0 8 -2 308.02 13.86 0 -8 1 2.97 3.03 0 -8 0 329.73 15.34 0 -8 -1 5.29 3.59 0 -8 -2 451.62 17.71 0 8 2 448.28 18.02 0 8 3 44.43 6.42 0 -8 -3 36.85 5.97 0 -8 -4 679.75 22.62 0 8 4 696.92 23.26 0 8 5 21.10 6.33 0 -8 -5 45.79 8.58 0 8 6 14.22 4.20 0 -8 -6 15.30 4.82 0 8 7 17.66 4.87 0 8 8 860.65 28.32 0 8 9 12.15 5.30 0 8 9 5.93 3.38 0 8 10 25.63 4.85 0 8 10 10.77 4.58 0 8 11 25.85 6.37 0 8 11 24.33 4.58 0 8 12 63.14 9.44 0 8 12 59.95 6.14 0 8 13 14.98 6.33 0 8 14 32.61 7.87 0 8 15 16.25 6.85 0 8 16 -4.02 4.19 0 8 17 131.89 14.98 0 9 -17 12.49 7.98 0 9 -16 63.13 11.80 0 -9 16 54.86 9.73 0 -9 15 14.62 6.36 0 9 -15 20.54 6.59 0 9 -15 28.24 8.46 0 -9 14 65.95 10.48 0 9 -14 66.95 10.99 0 9 -14 52.34 8.96 0 9 -13 -2.03 4.41 0 -9 13 0.46 5.39 0 9 -13 -2.88 4.32 0 9 -12 12.63 4.80 0 -9 12 16.30 5.97 0 9 -12 5.84 4.79 0 9 -11 11.21 6.25 0 -9 11 7.04 3.44 0 9 -11 4.59 4.01 0 -9 10 281.32 17.19 0 9 -10 290.28 19.40 0 9 -10 270.43 18.20 0 9 -9 79.18 10.22 0 -9 9 58.73 8.25 0 9 -9 64.62 9.28 0 9 -8 40.20 6.28 0 9 -8 25.01 6.01 0 -9 8 27.75 6.16 0 -9 7 21.49 4.74 0 9 -7 17.92 4.95 0 9 -7 30.05 5.25 0 9 -6 332.12 18.42 0 9 -6 348.51 15.92 0 -9 6 320.95 15.56 0 9 -5 123.33 9.76 0 -9 5 99.41 8.89 0 -9 4 10.42 4.30 0 9 -4 2.42 3.04 0 -9 3 326.43 14.34 0 9 -3 379.47 16.57 0 9 -2 16.34 4.49 0 -9 2 10.71 3.80 0 -9 2 10.46 4.84 0 -9 1 54.66 7.55 0 -9 0 -2.31 3.47 0 -9 -1 11.92 4.04 0 -9 -2 70.82 8.30 0 -9 -3 1415.68 33.98 0 9 3 1459.17 35.25 0 9 4 3.91 4.02 0 -9 -4 -6.69 3.35 0 9 5 192.78 13.43 0 -9 -5 214.92 13.99 0 9 6 52.88 7.98 0 -9 -6 61.22 8.42 0 -9 -7 0.03 3.72 0 9 7 0.78 3.18 0 9 8 169.96 13.34 0 9 9 214.63 15.30 0 9 9 218.84 12.79 0 9 10 12.24 3.93 0 9 10 5.68 4.39 0 9 11 42.90 5.97 0 9 11 60.72 9.30 0 9 12 46.44 8.43 0 9 13 -0.93 5.49 0 9 14 19.67 6.97 0 9 15 2.81 5.23 0 9 16 26.94 8.80 0 -10 16 46.65 10.02 0 10 -16 55.73 11.30 0 10 -15 -0.79 5.21 0 10 -15 2.16 5.40 0 -10 15 0.88 5.97 0 -10 14 44.55 8.94 0 10 -14 43.70 9.43 0 10 -14 25.87 6.64 0 10 -13 5.35 5.06 0 10 -13 18.15 7.55 0 -10 13 3.18 4.77 0 -10 12 35.72 7.70 0 10 -12 56.78 10.37 0 10 -12 54.11 9.51 0 10 -11 9.62 5.52 0 -10 11 6.91 5.40 0 10 -10 110.25 12.51 0 -10 10 115.33 11.78 0 -10 9 26.64 6.36 0 10 -9 28.26 6.64 0 -10 8 94.25 9.85 0 10 -8 87.67 10.54 0 10 -8 100.06 9.69 0 10 -7 1.28 3.87 0 -10 7 7.69 3.93 0 10 -7 12.49 4.64 0 10 -6 45.60 6.54 0 -10 6 49.89 7.18 0 -10 5 64.18 7.28 0 10 -5 72.76 8.09 0 -10 4 7.41 3.87 0 10 -4 8.29 3.96 0 10 -3 128.82 10.38 0 -10 3 138.55 12.00 0 -10 3 119.18 9.06 0 -10 2 103.71 10.22 0 -10 2 105.81 8.42 0 10 -2 105.40 9.29 0 -10 1 57.58 6.14 0 -10 1 62.94 8.30 0 -10 0 142.83 11.39 0 -10 -1 56.84 8.08 0 -10 -2 41.34 7.16 0 -10 -3 172.35 12.96 0 -10 -4 22.26 5.75 0 10 4 12.33 4.74 0 -10 -5 81.79 9.60 0 10 5 88.94 10.05 0 10 6 8.30 4.27 0 -10 -6 8.08 4.49 0 -10 -7 3.56 3.87 0 10 7 2.17 3.66 0 10 8 -1.72 3.98 0 10 9 503.02 20.96 0 10 9 507.38 24.55 0 10 10 7.88 4.48 0 10 10 0.23 4.28 0 10 11 7.06 5.15 0 10 11 6.83 4.03 0 10 12 16.82 5.98 0 10 13 53.52 9.88 0 10 14 13.47 7.08 0 10 15 31.78 8.82 0 -11 15 1.82 4.76 0 -11 14 -2.52 5.06 0 11 -14 12.10 6.26 0 11 -13 8.78 6.53 0 -11 13 11.43 6.31 0 -11 12 2.88 4.44 0 11 -12 6.37 5.09 0 11 -11 73.59 10.63 0 -11 11 70.76 10.07 0 11 -10 1.78 3.76 0 -11 10 16.04 6.36 0 -11 9 28.11 6.57 0 11 -9 32.48 7.42 0 -11 8 79.16 9.46 0 11 -8 69.21 8.54 0 11 -8 67.73 9.93 0 -11 7 240.80 14.84 0 11 -7 245.96 17.99 0 11 -7 241.46 15.00 0 11 -6 75.83 8.63 0 -11 6 62.02 7.91 0 11 -5 26.22 5.58 0 -11 5 26.03 5.27 0 -11 4 38.22 6.91 0 -11 4 32.37 5.78 0 11 -4 42.07 6.35 0 11 -3 90.99 9.43 0 -11 3 74.30 7.57 0 -11 3 87.11 10.11 0 -11 2 7.30 3.51 0 -11 2 5.63 3.07 0 11 -2 11.64 4.68 0 -11 1 447.12 16.81 0 11 -1 515.86 21.58 0 -11 1 466.47 21.92 0 -11 0 160.64 12.96 0 -11 -1 464.00 21.58 0 -11 -2 5.69 4.46 0 -11 -3 162.75 13.47 0 -11 -4 15.85 5.18 0 -11 -5 2.34 3.79 0 11 5 8.82 4.29 0 -11 -6 29.22 6.76 0 11 6 23.63 6.64 0 11 7 107.51 11.84 0 -11 -7 84.90 10.61 0 11 8 12.68 5.40 0 11 9 9.23 5.36 0 11 9 5.00 4.32 0 11 10 31.22 7.52 0 11 10 20.91 6.02 0 11 11 58.75 9.91 0 11 12 27.71 7.32 0 11 13 7.65 4.94 0 11 14 19.89 7.47 0 -12 14 6.20 5.36 0 -12 13 49.54 9.87 0 12 -13 51.71 9.85 0 12 -12 4.86 4.79 0 -12 12 14.35 6.47 0 -12 11 45.05 8.29 0 12 -11 42.36 8.81 0 -12 10 18.64 6.20 0 12 -10 6.56 5.38 0 12 -9 48.33 9.04 0 -12 9 44.97 8.14 0 12 -9 51.98 8.54 0 -12 8 14.24 4.72 0 12 -8 18.51 5.46 0 12 -8 14.58 5.92 0 12 -7 19.30 6.93 0 12 -7 14.74 4.28 0 -12 7 16.80 5.40 0 -12 6 12.84 5.13 0 12 -6 13.59 4.94 0 -12 5 13.04 4.98 0 12 -5 17.22 5.07 0 -12 5 7.86 3.76 0 -12 4 143.52 11.05 0 12 -4 169.00 12.99 0 -12 4 157.18 14.27 0 -12 3 244.61 13.70 0 12 -3 274.77 16.31 0 -12 3 265.89 17.67 0 -12 2 170.12 11.04 0 12 -2 206.65 14.36 0 -12 2 203.93 15.80 0 12 -1 157.30 12.96 0 -12 1 148.69 13.15 0 -12 1 147.92 10.17 0 -12 0 82.80 10.08 0 -12 0 66.03 6.71 0 -12 -1 57.46 8.78 0 -12 -2 131.06 12.44 0 -12 -3 43.80 8.23 0 -12 -4 136.69 13.04 0 -12 -5 4.03 4.43 0 -12 -6 458.63 23.90 0 12 6 474.68 24.57 0 -12 -7 44.64 8.60 0 12 7 46.90 8.73 0 12 8 4.81 4.10 0 12 9 83.10 11.49 0 12 9 53.76 8.34 0 12 10 43.08 7.52 0 12 10 65.64 10.94 0 12 11 11.86 6.12 0 12 12 79.83 12.14 0 12 13 9.17 6.19 0 -13 13 0.69 4.74 0 -13 12 3.41 5.16 0 13 -11 17.23 7.44 0 -13 11 6.32 4.81 0 -13 10 157.10 15.16 0 13 -10 150.89 16.59 0 -13 9 11.08 5.98 0 13 -9 0.86 4.27 0 13 -8 14.18 6.40 0 13 -8 13.18 5.22 0 -13 8 11.61 5.51 0 -13 7 10.23 4.67 0 13 -7 11.71 6.29 0 13 -7 13.05 5.04 0 -13 6 5.66 4.64 0 13 -6 8.33 4.28 0 -13 6 -6.46 3.64 0 13 -5 33.90 6.96 0 -13 5 31.31 6.27 0 -13 5 28.16 7.35 0 13 -4 29.82 6.64 0 -13 4 26.32 6.23 0 -13 4 20.22 6.94 0 -13 3 13.61 5.90 0 -13 3 14.37 4.52 0 13 -3 25.41 6.13 0 13 -2 73.05 9.40 0 -13 2 68.71 10.03 0 -13 2 66.02 7.51 0 -13 1 78.71 7.89 0 13 -1 109.19 11.16 0 -13 1 88.10 11.11 0 -13 0 11.57 4.95 0 -13 0 21.40 4.62 0 -13 -1 71.90 9.90 0 -13 -1 60.03 6.66 0 -13 -2 76.82 10.67 0 -13 -3 33.43 7.35 0 -13 -4 29.15 7.27 0 -13 -5 15.14 6.10 0 -13 -6 9.08 5.86 0 13 7 40.05 8.61 0 -13 -7 38.84 8.68 0 13 8 17.67 6.17 0 13 9 9.05 4.27 0 13 9 21.83 7.47 0 13 10 88.59 12.98 0 13 10 64.05 10.33 0 13 11 12.58 6.40 0 -14 12 20.36 7.59 0 -14 11 9.90 6.16 0 14 -10 89.04 13.81 0 -14 10 64.53 10.31 0 14 -9 19.43 7.68 0 -14 9 9.19 5.55 0 -14 8 7.97 5.54 0 14 -8 14.37 7.37 0 -14 7 -4.28 4.60 0 14 -7 0.86 5.43 0 -14 7 9.63 5.47 0 -14 6 23.47 7.25 0 14 -6 30.34 6.89 0 -14 5 25.16 7.40 0 14 -5 36.36 7.97 0 14 -4 335.59 19.72 0 -14 4 348.22 22.43 0 -14 3 -0.83 4.02 0 14 -3 -3.47 4.66 0 14 -2 88.80 10.52 0 -14 2 91.94 11.85 0 -14 1 9.35 5.47 0 14 -1 6.73 3.75 0 14 0 466.52 24.17 0 -14 0 410.76 23.74 0 -14 -1 17.67 6.80 0 -14 -2 28.84 7.69 0 -14 -3 13.92 5.82 0 -14 -4 38.89 9.47 0 -14 -5 -2.84 4.73 0 -14 -6 32.72 8.40 0 -14 -7 2.90 5.49 0 14 8 2.34 4.65 0 14 9 73.04 11.07 0 14 9 93.06 12.95 0 14 10 7.84 7.19 0 -15 8 17.43 7.67 0 -15 7 20.72 6.96 0 15 -7 21.63 6.83 0 -15 6 14.38 6.89 0 -15 5 69.22 11.28 0 15 -4 14.44 5.34 0 -15 4 20.87 7.00 0 15 -3 9.90 5.99 0 -15 3 8.01 5.30 0 15 -2 14.92 5.79 0 -15 2 21.41 6.74 0 -15 1 297.72 21.34 0 15 -1 321.85 20.88 0 15 0 79.40 11.09 0 -15 0 61.22 10.38 0 15 1 87.83 11.37 0 -15 -1 80.44 12.07 0 -15 -2 69.29 10.81 0 -15 -3 17.86 7.46 0 -15 -4 4.01 4.96 0 -15 -5 54.95 10.62 0 -15 -6 8.42 6.35 0 -15 -7 4.83 6.41 0 15 8 1.67 5.04 0 -16 4 29.07 8.93 0 -16 3 5.53 5.64 0 -16 2 3.23 5.42 0 16 -2 4.59 4.55 0 -16 1 39.96 10.73 0 16 -1 20.82 6.11 0 16 0 323.18 22.09 0 -16 0 288.74 22.27 0 -16 -1 19.20 8.05 0 16 1 17.72 6.91 0 -16 -2 21.63 8.05 0 -16 -3 7.02 5.84 0 16 8 34.53 8.54 0 17 0 4.63 5.57 0 17 1 11.82 6.50 0 17 2 11.37 5.11 -1 17 1 5.48 6.09 -1 17 0 29.52 8.27 -1 17 -1 -6.26 5.11 -1 17 -2 15.52 6.85 -1 16 2 50.19 10.02 -1 16 1 111.89 14.29 -1 16 0 3.28 5.12 -1 16 -1 1.72 4.54 -1 16 -2 49.31 9.30 -1 16 -3 -0.77 4.23 -1 16 -4 8.01 5.24 -1 16 -5 14.48 6.72 1 -15 -6 64.55 11.68 1 -15 -5 7.82 5.75 1 -15 -4 38.71 8.87 1 -15 -3 19.49 6.55 1 -15 -2 145.17 15.65 -1 15 1 34.28 7.93 1 -15 -1 40.31 9.23 1 -15 0 43.67 9.64 -1 15 0 31.03 7.82 -1 15 -1 18.04 6.81 1 -15 1 8.28 6.41 1 -15 2 1.70 6.12 -1 15 -2 9.76 5.41 1 -15 3 9.40 6.00 -1 15 -3 -3.74 4.45 -1 15 -4 23.40 7.09 1 -15 4 15.80 7.12 -1 15 -5 5.64 4.82 1 -15 5 8.31 6.69 1 -15 6 34.55 9.92 -1 15 -6 14.41 5.93 -1 15 -7 7.45 4.85 -1 15 -7 6.33 5.12 -1 14 9 7.18 6.23 1 -14 -8 37.46 9.15 -1 14 8 44.63 10.22 1 -14 -7 9.34 7.56 -1 14 7 28.26 8.30 1 -14 -6 11.88 6.66 1 -14 -5 34.99 8.56 1 -14 -4 3.53 4.31 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6.53 -2 14 -2 6.18 4.80 -2 14 -3 43.20 8.84 2 -14 3 54.24 10.62 2 -14 4 15.83 7.91 -2 14 -4 18.58 7.24 2 -14 5 20.66 7.31 -2 14 -5 25.76 6.83 -2 14 -6 10.66 6.02 2 -14 6 8.99 6.51 -2 14 -7 0.80 4.09 -2 14 -7 -4.57 4.10 2 -14 7 -0.27 4.81 -2 14 -8 58.86 10.53 -2 14 -8 52.29 9.69 -2 14 -9 18.82 6.08 -2 14 -9 10.39 5.68 -2 14 -10 0.73 4.81 -2 14 -10 -0.15 4.84 -2 14 -11 27.85 7.24 -2 13 10 47.25 10.00 -2 13 9 20.02 7.86 -2 13 8 11.74 5.62 2 -13 -8 23.28 8.38 -2 13 7 8.90 4.58 2 -13 -7 8.90 5.10 2 -13 -6 5.04 6.49 -2 13 6 10.82 6.00 -2 13 5 0.05 4.61 2 -13 -5 -6.21 4.84 2 -13 -4 120.65 13.88 2 -13 -3 14.42 5.52 2 -13 -2 111.97 12.72 2 -13 -1 -5.49 4.58 -2 13 1 2.20 4.21 2 -13 0 19.98 6.71 -2 13 0 25.76 6.27 2 -13 1 11.44 5.53 -2 13 -1 11.43 5.94 -2 13 -2 207.56 16.94 2 -13 2 201.83 17.02 -2 13 -3 7.72 5.57 2 -13 3 1.50 4.47 -2 13 -4 125.07 13.49 2 -13 4 120.14 13.54 2 -13 5 79.77 11.89 -2 13 -5 88.73 11.29 -2 13 -6 112.79 12.48 2 -13 6 96.90 12.59 -2 13 -7 21.28 6.06 -2 13 -7 38.61 8.78 -2 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7 78.76 8.11 -2 11 -7 97.73 10.99 -2 11 -7 76.08 10.19 2 -11 8 15.98 4.31 -2 11 -8 9.88 5.02 -2 11 -8 12.74 5.71 -2 11 -8 10.41 5.19 2 -11 9 7.89 5.06 -2 11 -9 2.08 3.41 -2 11 -9 6.54 4.77 -2 11 -9 6.42 5.32 2 -11 10 24.98 6.76 -2 11 -10 20.75 6.99 -2 11 -10 23.54 8.38 -2 11 -10 26.98 7.41 -2 11 -11 62.74 10.27 2 -11 11 66.59 9.13 -2 11 -11 53.82 9.17 2 -11 12 9.20 4.99 -2 11 -12 8.21 5.02 -2 11 -12 3.04 4.26 -2 11 -13 24.47 7.39 2 -11 13 36.83 8.61 -2 11 -13 29.81 9.87 -2 11 -14 42.59 8.66 2 -11 14 34.51 7.95 2 -11 15 40.78 9.51 -2 11 -15 53.37 10.36 -2 10 14 7.98 4.92 -2 10 13 6.19 5.80 -2 10 12 40.49 8.65 -2 10 11 14.74 6.33 -2 10 10 -2.47 3.92 -2 10 9 119.17 12.72 -2 10 8 15.60 5.11 2 -10 -8 19.03 6.48 2 -10 -7 219.28 16.18 -2 10 7 224.59 16.06 -2 10 6 55.90 8.45 2 -10 -6 48.05 8.19 2 -10 -5 378.80 20.34 -2 10 5 371.18 19.44 2 -10 -4 260.67 16.69 -2 10 4 263.60 16.22 2 -10 -3 40.19 7.47 -2 10 3 28.46 5.94 -2 10 2 7.86 4.08 2 -10 -2 10.35 4.02 2 -10 -1 385.11 19.87 2 -10 0 16.26 5.22 2 -10 0 8.52 1.48 2 -10 1 57.06 4.00 2 -10 1 84.67 9.85 -2 10 -1 100.44 10.43 -2 10 -2 2.05 3.80 2 -10 2 3.52 2.33 2 -10 2 -0.02 3.80 2 -10 3 144.38 12.59 2 -10 3 144.94 7.87 -2 10 -3 157.29 12.67 -2 10 -4 41.21 7.22 2 -10 4 39.38 4.97 -2 10 -5 388.10 20.30 2 -10 5 378.47 14.90 2 -10 6 17.87 4.08 -2 10 -6 18.68 5.31 -2 10 -6 18.55 6.12 -2 10 -7 19.08 5.63 -2 10 -7 21.74 6.38 -2 10 -7 15.52 5.26 2 -10 7 25.90 5.14 -2 10 -8 109.04 11.62 -2 10 -8 96.08 11.85 2 -10 8 95.31 9.54 -2 10 -8 93.97 10.65 -2 10 -9 1.36 4.51 -2 10 -9 8.31 4.50 2 -10 9 12.32 5.15 -2 10 -9 6.14 4.90 -2 10 -10 -1.09 4.39 2 -10 10 -0.11 3.53 -2 10 -10 3.18 4.66 -2 10 -10 -0.55 4.09 -2 10 -11 16.24 5.25 2 -10 11 15.90 5.82 -2 10 -11 16.42 6.81 2 -10 12 163.23 14.42 -2 10 -12 155.63 16.30 -2 10 -12 159.02 14.77 -2 10 -13 26.40 6.75 2 -10 13 32.96 7.88 -2 10 -13 41.40 9.71 -2 10 -14 193.11 18.62 2 -10 14 206.89 16.89 -2 10 -14 171.92 16.04 -2 10 -15 7.15 6.16 -2 10 -15 3.01 4.12 2 -10 15 5.79 5.17 2 -10 16 1.42 6.28 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9 -7 77.54 10.53 4 9 -6 54.32 8.66 -4 -9 6 57.38 9.44 -4 -9 6 58.24 8.34 4 9 -6 45.86 8.11 4 9 -5 5.09 4.25 -4 -9 5 8.99 4.68 4 9 -5 -2.29 3.86 -4 -9 5 -2.31 3.33 4 9 -4 11.00 5.18 -4 -9 4 13.96 5.51 -4 -9 4 16.11 4.33 4 9 -4 5.02 4.18 4 9 -3 39.69 7.37 -4 -9 3 47.48 7.93 -4 -9 3 39.19 5.40 4 9 -3 29.05 6.04 -4 -9 2 158.69 13.58 -4 -9 2 135.20 9.03 4 9 -2 141.92 13.15 4 9 -1 26.17 6.45 -4 -9 1 33.43 6.97 -4 -9 1 40.24 5.26 4 9 0 27.16 7.34 -4 -9 0 29.01 8.66 -4 -9 0 23.76 4.86 4 9 1 8.74 5.16 -4 -9 -1 14.04 3.72 -4 -9 -1 15.74 6.16 -4 -9 -2 165.52 13.91 -4 -9 -2 167.16 10.42 4 9 2 170.45 14.34 -4 -9 -3 99.23 8.36 -4 -9 -3 103.53 11.32 4 9 3 84.36 10.12 -4 -9 -4 306.93 18.79 4 9 4 314.73 19.01 -4 -9 -5 121.24 12.11 4 9 5 113.34 11.73 -4 -9 -6 104.51 11.36 4 9 6 86.47 10.45 -4 -9 -7 16.18 6.00 4 9 7 18.74 6.67 -4 -9 -8 204.50 15.82 4 9 8 206.51 15.99 -4 -9 -9 531.55 25.43 4 9 9 552.58 25.19 4 9 9 546.68 24.48 -4 -9 -10 45.65 7.85 4 9 10 33.84 7.07 4 9 10 29.00 6.60 -4 -9 -11 111.53 12.32 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19.94 6.47 4 11 -7 16.99 6.84 -4 -11 7 11.61 5.75 -4 -11 7 15.61 5.16 4 11 -7 16.74 6.33 -4 -11 6 7.46 4.64 4 11 -6 8.88 5.73 4 11 -6 1.81 3.87 -4 -11 6 9.02 4.53 -4 -11 5 27.93 5.45 4 11 -5 29.25 8.00 -4 -11 5 26.29 7.45 4 11 -5 25.82 6.31 4 11 -4 10.33 5.00 -4 -11 4 5.02 4.14 -4 -11 4 2.27 3.17 4 11 -4 9.83 5.45 4 11 -3 58.45 9.38 -4 -11 3 54.57 6.97 -4 -11 3 60.58 9.99 4 11 -2 6.66 5.39 -4 -11 2 9.52 5.92 -4 -11 2 10.18 4.31 -4 -11 1 273.21 19.19 -4 -11 1 250.28 13.97 4 11 -1 242.96 18.42 4 11 0 -5.25 4.51 -4 -11 0 -1.52 2.82 -4 -11 0 -0.91 4.38 -4 -11 -1 168.10 15.66 -4 -11 -1 172.91 11.94 4 11 1 146.63 14.56 -4 -11 -2 14.65 4.42 4 11 2 20.25 6.22 -4 -11 -2 13.92 5.48 4 11 3 85.75 11.29 -4 -11 -3 100.74 9.65 -4 -11 -3 107.09 12.81 -4 -11 -4 50.88 9.05 4 11 4 35.40 7.88 -4 -11 -5 18.40 6.24 4 11 5 21.86 6.10 -4 -11 -6 23.12 7.24 4 11 6 10.97 5.42 -4 -11 -7 155.45 15.30 4 11 7 159.33 14.98 -4 -11 -8 88.95 11.66 4 11 8 101.17 12.24 -4 -11 -9 63.54 10.56 4 11 9 56.97 9.88 -4 -11 -10 5.10 5.05 4 11 10 4.23 3.92 -4 -11 -11 290.52 20.87 4 11 11 269.28 19.56 4 11 11 272.50 19.65 -4 -11 -12 15.95 6.62 4 11 12 4.11 5.63 -4 -11 -13 5.39 5.89 4 11 13 9.06 5.55 -4 -11 -14 5.87 5.37 4 11 14 12.08 5.72 -4 -11 -15 2.93 4.40 4 11 15 11.17 6.55 4 12 -12 5.36 4.96 4 12 -11 134.57 15.27 4 12 -10 -0.10 5.46 -4 -12 10 1.96 5.09 4 12 -10 -4.01 4.81 4 12 -9 3.35 5.84 -4 -12 9 1.57 5.28 4 12 -9 1.18 4.09 4 12 -8 14.28 6.40 -4 -12 8 -0.44 4.81 4 12 -8 14.50 6.33 -4 -12 7 29.59 7.65 4 12 -7 27.89 7.82 4 12 -7 21.87 7.37 4 12 -6 7.09 5.57 -4 -12 6 17.84 6.50 4 12 -6 1.19 4.98 4 12 -5 127.18 14.20 -4 -12 5 126.23 14.28 -4 -12 5 128.10 11.46 4 12 -5 117.64 13.61 4 12 -4 76.23 11.64 -4 -12 4 88.59 9.40 4 12 -4 96.10 12.43 -4 -12 3 5.35 4.51 4 12 -3 14.21 6.97 -4 -12 2 6.81 5.10 -4 -12 2 17.42 5.01 -4 -12 1 116.13 13.78 4 12 -1 111.32 12.84 -4 -12 1 110.46 10.23 4 12 0 37.03 8.90 -4 -12 0 40.34 9.38 -4 -12 0 31.75 6.07 4 12 1 13.98 6.53 -4 -12 -1 12.16 4.30 -4 -12 -1 18.07 6.68 -4 -12 -2 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5.95 -10 -3 -3 27.62 8.36 -10 -3 -4 20.68 7.49 -10 -3 -5 3.96 5.31 -10 -3 -6 19.29 6.96 -10 -3 -7 -0.97 4.80 -10 -3 -8 49.34 10.15 -10 -3 -9 24.85 8.20 -10 -3 -10 25.83 8.98 -10 -4 4 29.83 8.33 -10 -4 3 1.77 5.53 -10 -4 2 5.36 5.44 -10 -4 1 119.41 15.37 -10 -4 0 69.71 12.22 -10 -4 -1 114.66 15.63 -10 -4 -2 38.91 9.36 -10 -4 -3 44.68 10.11 -10 -4 -4 -2.41 6.16 -10 -4 -6 -2.05 4.71 -10 -4 -7 12.78 5.58 -10 -4 -8 12.77 6.23 -10 -4 -9 -1.26 4.57 -10 -5 4 17.89 7.67 -10 -5 3 21.03 8.26 -10 -5 2 36.41 9.33 -10 -5 1 58.00 11.42 -10 -5 0 18.70 8.04 -10 -5 -1 25.56 8.40 -10 -5 -2 60.71 11.49 -10 -5 -5 23.61 7.17 -10 -5 -6 9.55 4.31 -10 -5 -7 5.45 5.68 -10 -5 -8 6.32 4.53 -10 -5 -9 -3.44 5.34 -10 -6 4 18.72 6.87 -10 -6 3 9.19 6.68 -10 -6 -8 12.16 7.01 0 0 0 0.00 0.00 TITL OS-DFDP-pyrrol in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.136505 12.742063 16.045061 88.0587 82.3489 86.1404 ZERR 6.00 0.000441 0.001018 0.000773 0.0054 0.0043 0.0055 LATT 1 SFAC C H N F UNIT 72.00 72.00 6.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 49389 _shelx_res_file ; REM REM wR2 = 0.2059, GooF = S = 1.185, Restrained GooF = 1.185 for all data REM R1 = 0.0896 for 4892 Fo > 4sig(Fo) and 0.1033 for all 5775 data REM 403 parameters refined using 2 restraints REM Highest difference peak 0.584, deepest hole -0.338, 1-sigma level 0.087 REM REM wR2 = 0.2043, GooF = S = 1.185, Restrained GooF = 1.185 for all data REM R1 = 0.0896 for 4892 Fo > 4sig(Fo) and 0.1033 for all 5775 data REM 403 parameters refined using 0 restraints REM Highest difference peak 0.576, deepest hole -0.338, 1-sigma level 0.086 TITL C:\Users\stula\Desktop\OS3-IV~1\OS3.res created by SHELXL-2018/3 at 10:39:14 on 29-Jan-2025 CELL 0.71073 8.1365 12.7421 16.0451 88.059 82.349 86.140 ZERR 4.0000 0.0004 0.0010 0.0008 0.005 0.004 0.005 LATT 1 SFAC C H N F CL UNIT 72 80 4 8 4 MERG 2 OMIT -2 50 SHEL 7.00 0.77 FMAP 2 GRID PLAN 4 TEMP -100 OMIT -5 2 4 OMIT -2 -1 10 OMIT 3 -4 12 OMIT 3 1 7 OMIT 3 -1 7 OMIT -5 -2 2 OMIT 3 8 10 OMIT -5 -1 3 OMIT -1 -4 4 OMIT 5 0 1 OMIT 4 -7 8 OMIT 0 -5 1 OMIT 5 1 3 OMIT 5 1 2 OMIT -1 3 6 OMIT 2 4 15 OMIT 4 -3 4 OMIT 3 0 10 OMIT 2 1 15 OMIT 3 -6 10 HTAB N1 CL1 HTAB N2 CL2 DFIX 0.98 0.01 N1 H1' DFIX 0.98 0.01 N2 H2 L.S. 16 ACTA WGHT 0.014300 10.410200 FVAR 0.64733 CL2 5 1.114244 0.866111 0.521286 11.00000 0.03899 0.02792 = 0.02196 -0.00624 -0.00989 0.00352 CL1 5 0.609712 0.634202 1.005790 11.00000 0.05526 0.03071 = 0.02900 0.00752 -0.02031 -0.01626 F1 4 0.339327 0.701415 0.693278 11.00000 0.04128 0.03380 = 0.02849 0.00937 -0.00756 -0.01342 F2 4 0.075161 0.432897 0.856778 11.00000 0.03330 0.03094 = 0.03600 0.00765 -0.00167 -0.01003 F3 4 0.918242 0.771972 0.216823 11.00000 0.03818 0.03036 = 0.03210 -0.01108 -0.00132 0.00336 F4 4 0.587777 1.074014 0.308655 11.00000 0.03412 0.02809 = 0.05686 -0.01285 -0.00829 0.00639 N2 3 0.830647 0.873098 0.413969 11.00000 0.02834 0.02741 = 0.01642 0.00118 -0.00146 -0.00332 N1 3 0.319010 0.638382 0.906294 11.00000 0.03140 0.02665 = 0.01601 -0.00383 -0.00522 -0.00277 C27 1 0.759892 0.923371 0.268335 11.00000 0.02286 0.02101 = 0.01654 0.00002 -0.00184 -0.00427 C9 1 0.216362 0.565714 0.779003 11.00000 0.02186 0.02052 = 0.01839 -0.00475 -0.00217 0.00456 C28 1 0.627118 0.993362 0.254587 11.00000 0.02254 0.02545 = 0.02750 -0.00070 -0.00157 -0.00552 C1 1 0.347072 0.556885 0.838596 11.00000 0.02622 0.01988 = 0.01835 -0.00178 -0.00637 -0.00105 AFIX 13 H1 2 0.335348 0.487106 0.868486 11.00000 -1.20000 AFIX 0 C21 1 1.094432 1.016945 0.235129 11.00000 0.01548 0.02857 = 0.02352 -0.00098 -0.00095 -0.00103 C19 1 0.866653 0.942954 0.335850 11.00000 0.02620 0.02138 = 0.01827 0.00201 -0.00319 -0.00490 AFIX 13 H19 2 0.836336 1.016817 0.354039 11.00000 -1.20000 AFIX 0 C3 1 0.558488 0.469575 0.731978 11.00000 0.01969 0.03099 = 0.02256 -0.00490 -0.00084 -0.00310 C20 1 1.052920 0.937368 0.305622 11.00000 0.02580 0.02866 = 0.02216 -0.00142 -0.00584 -0.00391 AFIX 23 H20A 2 1.113949 0.951212 0.353117 11.00000 -1.20000 H20B 2 1.088997 0.865768 0.285632 11.00000 -1.20000 AFIX 0 C14 1 0.090688 0.496533 0.787407 11.00000 0.02326 0.02254 = 0.02951 -0.00219 -0.00294 0.00030 C32 1 0.790695 0.843983 0.209400 11.00000 0.02734 0.02710 = 0.02209 -0.00148 0.00248 -0.00573 C11 1 0.114537 0.627173 0.647467 11.00000 0.04266 0.03266 = 0.02382 0.00108 -0.01469 0.00477 AFIX 43 H11 2 0.122464 0.673672 0.599757 11.00000 -1.20000 AFIX 0 C22 1 1.100744 1.122531 0.253336 11.00000 0.03100 0.03370 = 0.02844 -0.00644 -0.00178 -0.00566 AFIX 43 H22 2 1.075832 1.144702 0.309803 11.00000 -1.20000 AFIX 0 C2 1 0.526329 0.555733 0.795571 11.00000 0.02338 0.02803 = 0.02228 -0.00262 -0.00460 -0.00586 AFIX 23 H2A 2 0.546795 0.624627 0.767039 11.00000 -1.20000 H2B 2 0.603436 0.544026 0.838268 11.00000 -1.20000 AFIX 0 C25 1 1.166180 1.060235 0.088214 11.00000 0.03164 0.04424 = 0.02103 0.00057 0.00195 -0.00468 AFIX 43 H25 2 1.187292 1.039035 0.031390 11.00000 -1.20000 AFIX 0 C10 1 0.220812 0.630470 0.706558 11.00000 0.02444 0.02269 = 0.02464 -0.00080 -0.00231 -0.00405 C8 1 0.564740 0.364428 0.758534 11.00000 0.01954 0.03946 = 0.03656 -0.00205 -0.00282 0.00169 AFIX 43 H8 2 0.546327 0.346785 0.816886 11.00000 -1.20000 AFIX 0 C36 1 0.665769 0.897737 0.464390 11.00000 0.02663 0.05290 = 0.02410 -0.00354 0.00356 -0.00829 AFIX 23 H36A 2 0.575698 0.900454 0.428380 11.00000 -1.20000 H36B 2 0.663620 0.965988 0.492346 11.00000 -1.20000 AFIX 0 C15 1 0.164894 0.628648 0.967751 11.00000 0.03765 0.03535 = 0.02878 -0.00419 0.00843 0.00068 AFIX 23 H15A 2 0.174375 0.564876 1.004224 11.00000 -1.20000 H15B 2 0.065945 0.625638 0.938275 11.00000 -1.20000 AFIX 0 C33 1 0.836572 0.756313 0.403714 11.00000 0.04472 0.03166 = 0.02847 0.00507 -0.00730 -0.00711 AFIX 23 H33A 2 0.952397 0.726924 0.389866 11.00000 -1.20000 H33B 2 0.771135 0.738088 0.359065 11.00000 -1.20000 AFIX 0 C26 1 1.126230 0.986607 0.151773 11.00000 0.02266 0.03075 = 0.02411 -0.00121 -0.00347 -0.00533 AFIX 43 H26 2 1.120489 0.914988 0.138423 11.00000 -1.20000 AFIX 0 C31 1 0.699050 0.832264 0.144736 11.00000 0.03605 0.04433 = 0.02483 -0.01088 0.00286 -0.02042 AFIX 43 H31 2 0.722886 0.774732 0.107981 11.00000 -1.20000 AFIX 0 C13 1 -0.019723 0.488234 0.729992 11.00000 0.02522 0.02868 = 0.04940 -0.00031 -0.01002 -0.00667 AFIX 43 H13 2 -0.103175 0.438879 0.738846 11.00000 -1.20000 AFIX 0 C5 1 0.620488 0.414365 0.587978 11.00000 0.03797 0.06289 = 0.02579 -0.01508 0.00361 0.00177 AFIX 43 H5 2 0.638539 0.431937 0.529606 11.00000 -1.20000 AFIX 0 C29 1 0.532987 0.988660 0.189618 11.00000 0.03049 0.03842 = 0.04186 0.01134 -0.01593 -0.00782 AFIX 43 H29 2 0.445057 1.039810 0.182690 11.00000 -1.20000 AFIX 0 C17 1 0.248397 0.809687 0.960253 11.00000 0.04359 0.03221 = 0.04304 -0.01580 -0.00724 0.00455 AFIX 23 H17A 2 0.172625 0.871072 0.948940 11.00000 -1.20000 H17B 2 0.342017 0.834403 0.986302 11.00000 -1.20000 AFIX 0 C30 1 0.571946 0.906209 0.134817 11.00000 0.03455 0.06158 = 0.02625 0.00317 -0.01326 -0.02223 AFIX 43 H30 2 0.509337 0.900738 0.089399 11.00000 -1.20000 AFIX 0 C7 1 0.597869 0.284853 0.699991 11.00000 0.02741 0.03530 = 0.04974 -0.01073 0.00197 0.00004 AFIX 43 H7 2 0.599135 0.213208 0.718453 11.00000 -1.20000 AFIX 0 C24 1 1.175478 1.164408 0.107063 11.00000 0.03662 0.04681 = 0.03129 0.01505 -0.00241 -0.00654 AFIX 43 H24 2 1.204076 1.214593 0.063287 11.00000 -1.20000 AFIX 0 C23 1 1.143371 1.195579 0.189160 11.00000 0.03370 0.02629 = 0.04762 -0.00074 -0.00240 -0.00282 AFIX 43 H23 2 1.150355 1.267240 0.202027 11.00000 -1.20000 AFIX 0 C18 1 0.311612 0.752611 0.879715 11.00000 0.04619 0.02151 = 0.03115 -0.00524 -0.00471 -0.00095 AFIX 23 H18A 2 0.234606 0.766623 0.837207 11.00000 -1.20000 H18B 2 0.423028 0.774539 0.855950 11.00000 -1.20000 AFIX 0 C12 1 -0.005574 0.553332 0.659688 11.00000 0.03272 0.04056 = 0.04877 -0.00502 -0.02438 0.00005 AFIX 43 H12 2 -0.078813 0.547876 0.618826 11.00000 -1.20000 AFIX 0 C4 1 0.585815 0.492762 0.645947 11.00000 0.02902 0.03766 = 0.02632 -0.00303 0.00020 -0.00382 AFIX 43 H4 2 0.580421 0.564153 0.626864 11.00000 -1.20000 AFIX 0 C6 1 0.629007 0.310134 0.614767 11.00000 0.03145 0.05715 = 0.05568 -0.03428 0.00802 0.00014 AFIX 43 H6 2 0.656059 0.256025 0.575020 11.00000 -1.20000 AFIX 0 C35 1 0.647471 0.808063 0.528571 11.00000 0.04451 0.07476 = 0.02323 0.00341 0.00081 -0.02038 AFIX 23 H35A 2 0.530490 0.788934 0.539572 11.00000 -1.20000 H35B 2 0.683247 0.827842 0.582205 11.00000 -1.20000 AFIX 0 C16 1 0.154667 0.727553 1.018531 11.00000 0.04637 0.04708 = 0.03079 -0.01179 0.00059 0.00366 AFIX 23 H16A 2 0.207772 0.713990 1.070222 11.00000 -1.20000 H16B 2 0.037391 0.752837 1.034725 11.00000 -1.20000 AFIX 0 C34 1 0.759727 0.716145 0.489499 11.00000 0.04662 0.05567 = 0.03374 0.01802 -0.00937 -0.01507 AFIX 23 H34A 2 0.847256 0.694674 0.525112 11.00000 -1.20000 H34B 2 0.693919 0.654893 0.483513 11.00000 -1.20000 AFIX 0 H1' 2 0.397329 0.632087 0.948299 11.00000 -1.20000 H2 2 0.911297 0.874911 0.454434 11.00000 -1.20000 HKLF 4 REM REM wR2 = 0.2059, GooF = S = 1.185, Restrained GooF = 1.185 for all data REM R1 = 0.0896 for 4892 Fo > 4sig(Fo) and 0.1033 for all 5775 data REM 403 parameters refined using 2 restraints END WGHT 0.0143 10.4118 REM Highest difference peak 0.585, deepest hole -0.338, 1-sigma level 0.087 Q1 1 1.0340 0.8627 0.4773 11.00000 0.05 0.59 Q2 1 0.8021 0.6383 1.0535 11.00000 0.05 0.58 Q3 1 0.3315 0.8649 0.5570 11.00000 0.05 0.54 Q4 1 0.9158 0.8777 0.4770 11.00000 0.05 0.44 ; _shelx_res_checksum 76721 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Cl Cl2 1.11424(18) 0.86611(11) 0.52129(8) 0.0292(3) Uani d 1 . . Cl Cl1 0.6097(2) 0.63420(11) 1.00579(9) 0.0366(4) Uani d 1 . . F F1 0.3393(4) 0.7014(3) 0.6933(2) 0.0340(8) Uani d 1 . . F F2 0.0752(4) 0.4329(3) 0.8568(2) 0.0335(8) Uani d 1 . . F F3 0.9182(4) 0.7720(3) 0.2168(2) 0.0339(8) Uani d 1 . . F F4 0.5878(4) 1.0740(3) 0.3087(2) 0.0396(9) Uani d 1 . . N N2 0.8306(6) 0.8731(4) 0.4140(3) 0.0242(10) Uani d 1 . . N N1 0.3190(6) 0.6384(4) 0.9063(3) 0.0244(10) Uani d 1 . . C C27 0.7599(6) 0.9234(4) 0.2683(3) 0.0201(11) Uani d 1 . . C C9 0.2164(6) 0.5657(4) 0.7790(3) 0.0205(11) Uani d 1 . . C C28 0.6271(7) 0.9934(4) 0.2546(3) 0.0251(12) Uani d 1 . . C C1 0.3471(6) 0.5569(4) 0.8386(3) 0.0212(11) Uani d 1 . . H H1 0.335348 0.487106 0.868486 0.025 Uiso calc 1 . . C C21 1.0944(6) 1.0169(4) 0.2351(3) 0.0227(11) Uani d 1 . . C C19 0.8667(6) 0.9430(4) 0.3359(3) 0.0218(11) Uani d 1 . . H H19 0.836336 1.016817 0.354039 0.026 Uiso calc 1 . . C C3 0.5585(6) 0.4696(4) 0.7320(3) 0.0244(12) Uani d 1 . . C C20 1.0529(7) 0.9374(4) 0.3056(3) 0.0252(12) Uani d 1 . . H H20A 1.113949 0.951212 0.353117 0.030 Uiso calc 1 . . H H20B 1.088997 0.865768 0.285632 0.030 Uiso calc 1 . . C C14 0.0907(7) 0.4965(4) 0.7874(3) 0.0252(12) Uani d 1 . . C C32 0.7907(7) 0.8440(4) 0.2094(3) 0.0258(12) Uani d 1 . . C C11 0.1145(8) 0.6272(5) 0.6475(4) 0.0325(14) Uani d 1 . . H H11 0.122464 0.673672 0.599757 0.039 Uiso calc 1 . . C C22 1.1007(7) 1.1225(5) 0.2533(4) 0.0309(13) Uani d 1 . . H H22 1.075832 1.144702 0.309803 0.037 Uiso calc 1 . . C C2 0.5263(7) 0.5557(4) 0.7956(3) 0.0242(12) Uani d 1 . . H H2A 0.546795 0.624627 0.767039 0.029 Uiso calc 1 . . H H2B 0.603436 0.544026 0.838268 0.029 Uiso calc 1 . . C C25 1.1662(7) 1.0602(5) 0.0882(4) 0.0327(14) Uani d 1 . . H H25 1.187292 1.039035 0.031390 0.039 Uiso calc 1 . . C C10 0.2208(7) 0.6305(4) 0.7066(3) 0.0239(12) Uani d 1 . . C C8 0.5647(7) 0.3644(5) 0.7585(4) 0.0321(13) Uani d 1 . . H H8 0.546327 0.346785 0.816886 0.038 Uiso calc 1 . . C C36 0.6658(7) 0.8977(5) 0.4644(4) 0.0348(14) Uani d 1 . . H H36A 0.575698 0.900454 0.428380 0.042 Uiso calc 1 . . H H36B 0.663620 0.965988 0.492346 0.042 Uiso calc 1 . . C C15 0.1649(8) 0.6286(5) 0.9678(4) 0.0351(14) Uani d 1 . . H H15A 0.174375 0.564876 1.004224 0.042 Uiso calc 1 . . H H15B 0.065945 0.625638 0.938275 0.042 Uiso calc 1 . . C C33 0.8366(8) 0.7563(5) 0.4037(4) 0.0346(14) Uani d 1 . . H H33A 0.952397 0.726924 0.389866 0.042 Uiso calc 1 . . H H33B 0.771135 0.738088 0.359065 0.042 Uiso calc 1 . . C C26 1.1262(7) 0.9866(4) 0.1518(3) 0.0256(12) Uani d 1 . . H H26 1.120489 0.914988 0.138423 0.031 Uiso calc 1 . . C C31 0.6991(8) 0.8323(5) 0.1447(4) 0.0346(14) Uani d 1 . . H H31 0.722886 0.774732 0.107981 0.042 Uiso calc 1 . . C C13 -0.0197(7) 0.4882(5) 0.7300(4) 0.0338(14) Uani d 1 . . H H13 -0.103175 0.438879 0.738846 0.041 Uiso calc 1 . . C C5 0.6205(8) 0.4144(6) 0.5880(4) 0.0428(16) Uani d 1 . . H H5 0.638539 0.431937 0.529606 0.051 Uiso calc 1 . . C C29 0.5330(8) 0.9887(5) 0.1896(4) 0.0359(15) Uani d 1 . . H H29 0.445057 1.039810 0.182690 0.043 Uiso calc 1 . . C C17 0.2484(8) 0.8097(5) 0.9603(4) 0.0394(15) Uani d 1 . . H H17A 0.172625 0.871072 0.948940 0.047 Uiso calc 1 . . H H17B 0.342017 0.834403 0.986302 0.047 Uiso calc 1 . . C C30 0.5719(8) 0.9062(6) 0.1348(4) 0.0392(16) Uani d 1 . . H H30 0.509337 0.900738 0.089399 0.047 Uiso calc 1 . . C C7 0.5979(7) 0.2849(5) 0.7000(4) 0.0380(15) Uani d 1 . . H H7 0.599135 0.213208 0.718453 0.046 Uiso calc 1 . . C C24 1.1755(8) 1.1644(5) 0.1071(4) 0.0386(15) Uani d 1 . . H H24 1.204076 1.214593 0.063287 0.046 Uiso calc 1 . . C C23 1.1434(8) 1.1956(5) 0.1892(4) 0.0361(14) Uani d 1 . . H H23 1.150355 1.267240 0.202027 0.043 Uiso calc 1 . . C C18 0.3116(8) 0.7526(4) 0.8797(4) 0.0329(14) Uani d 1 . . H H18A 0.234606 0.766623 0.837207 0.040 Uiso calc 1 . . H H18B 0.423028 0.774539 0.855950 0.040 Uiso calc 1 . . C C12 -0.0056(8) 0.5533(5) 0.6597(4) 0.0390(15) Uani d 1 . . H H12 -0.078813 0.547876 0.618826 0.047 Uiso calc 1 . . C C4 0.5858(7) 0.4928(5) 0.6459(4) 0.0312(13) Uani d 1 . . H H4 0.580421 0.564153 0.626864 0.037 Uiso calc 1 . . C C6 0.6290(8) 0.3101(6) 0.6148(5) 0.0487(19) Uani d 1 . . H H6 0.656059 0.256025 0.575020 0.058 Uiso calc 1 . . C C35 0.6475(9) 0.8081(6) 0.5286(4) 0.0473(18) Uani d 1 . . H H35A 0.530490 0.788934 0.539572 0.057 Uiso calc 1 . . H H35B 0.683247 0.827842 0.582205 0.057 Uiso calc 1 . . C C16 0.1547(9) 0.7276(5) 1.0185(4) 0.0420(16) Uani d 1 . . H H16A 0.207772 0.713990 1.070222 0.050 Uiso calc 1 . . H H16B 0.037391 0.752837 1.034725 0.050 Uiso calc 1 . . C C34 0.7597(9) 0.7161(6) 0.4895(4) 0.0449(17) Uani d 1 . . H H34A 0.847256 0.694674 0.525112 0.054 Uiso calc 1 . . H H34B 0.693919 0.654893 0.483513 0.054 Uiso calc 1 . . H H1' 0.397(7) 0.632(5) 0.948(3) 0.054 Uiso d 1 . . H H2 0.911(6) 0.875(5) 0.454(3) 0.054 Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl2 0.0390(8) 0.0279(7) 0.0220(7) 0.0035(6) -0.0099(6) -0.0062(5) Cl1 0.0553(10) 0.0307(8) 0.0290(8) -0.0163(7) -0.0203(7) 0.0075(6) F1 0.041(2) 0.0338(19) 0.0285(18) -0.0134(15) -0.0076(15) 0.0094(14) F2 0.0333(19) 0.0309(18) 0.0360(19) -0.0100(14) -0.0017(15) 0.0077(15) F3 0.038(2) 0.0304(18) 0.0321(19) 0.0034(15) -0.0013(15) -0.0111(14) F4 0.034(2) 0.0281(18) 0.057(2) 0.0064(15) -0.0083(17) -0.0129(16) N2 0.028(3) 0.027(2) 0.016(2) -0.003(2) -0.0015(19) 0.0012(19) N1 0.031(3) 0.027(2) 0.016(2) -0.003(2) -0.0052(19) -0.0038(19) C27 0.023(3) 0.021(3) 0.017(3) -0.004(2) -0.002(2) 0.000(2) C9 0.022(3) 0.021(3) 0.018(3) 0.005(2) -0.002(2) -0.005(2) C28 0.023(3) 0.025(3) 0.027(3) -0.006(2) -0.002(2) -0.001(2) C1 0.026(3) 0.020(3) 0.018(3) -0.001(2) -0.006(2) -0.002(2) C21 0.015(3) 0.029(3) 0.024(3) -0.001(2) -0.001(2) -0.001(2) C19 0.026(3) 0.021(3) 0.018(3) -0.005(2) -0.003(2) 0.002(2) C3 0.020(3) 0.031(3) 0.023(3) -0.003(2) -0.001(2) -0.005(2) C20 0.026(3) 0.029(3) 0.022(3) -0.004(2) -0.006(2) -0.001(2) C14 0.023(3) 0.023(3) 0.030(3) 0.000(2) -0.003(2) -0.002(2) C32 0.027(3) 0.027(3) 0.022(3) -0.006(2) 0.002(2) -0.001(2) C11 0.043(4) 0.033(3) 0.024(3) 0.005(3) -0.015(3) 0.001(2) C22 0.031(3) 0.034(3) 0.028(3) -0.006(3) -0.002(3) -0.006(3) C2 0.023(3) 0.028(3) 0.022(3) -0.006(2) -0.005(2) -0.003(2) C25 0.032(3) 0.044(4) 0.021(3) -0.005(3) 0.002(2) 0.001(3) C10 0.024(3) 0.023(3) 0.025(3) -0.004(2) -0.002(2) -0.001(2) C8 0.020(3) 0.039(3) 0.037(3) 0.002(2) -0.003(2) -0.002(3) C36 0.027(3) 0.053(4) 0.024(3) -0.008(3) 0.004(2) -0.004(3) C15 0.038(4) 0.035(3) 0.029(3) 0.001(3) 0.008(3) -0.004(3) C33 0.045(4) 0.032(3) 0.028(3) -0.007(3) -0.007(3) 0.005(3) C26 0.023(3) 0.031(3) 0.024(3) -0.005(2) -0.003(2) -0.001(2) C31 0.036(3) 0.044(4) 0.025(3) -0.020(3) 0.003(3) -0.011(3) C13 0.025(3) 0.029(3) 0.049(4) -0.007(2) -0.010(3) 0.000(3) C5 0.038(4) 0.063(5) 0.026(3) 0.002(3) 0.004(3) -0.015(3) C29 0.030(3) 0.038(4) 0.042(4) -0.008(3) -0.016(3) 0.011(3) C17 0.044(4) 0.032(3) 0.043(4) 0.005(3) -0.007(3) -0.016(3) C30 0.035(4) 0.062(4) 0.026(3) -0.022(3) -0.013(3) 0.003(3) C7 0.027(3) 0.035(3) 0.050(4) 0.000(3) 0.002(3) -0.011(3) C24 0.037(4) 0.047(4) 0.031(3) -0.007(3) -0.002(3) 0.015(3) C23 0.034(3) 0.026(3) 0.048(4) -0.003(3) -0.002(3) -0.001(3) C18 0.046(4) 0.022(3) 0.031(3) -0.001(3) -0.005(3) -0.005(2) C12 0.033(3) 0.041(4) 0.049(4) 0.000(3) -0.024(3) -0.005(3) C4 0.029(3) 0.038(3) 0.026(3) -0.004(3) 0.000(2) -0.003(3) C6 0.031(4) 0.057(5) 0.056(5) 0.000(3) 0.008(3) -0.034(4) C35 0.045(4) 0.075(5) 0.023(3) -0.020(4) 0.001(3) 0.003(3) C16 0.046(4) 0.047(4) 0.031(3) 0.004(3) 0.001(3) -0.012(3) C34 0.047(4) 0.056(4) 0.034(4) -0.015(3) -0.009(3) 0.018(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C36 N2 C33 . . 103.9(4) ? C36 N2 C19 . . 114.4(4) ? C33 N2 C19 . . 118.5(4) ? C15 N1 C18 . . 103.7(4) ? C15 N1 C1 . . 115.1(4) ? C18 N1 C1 . . 118.3(4) ? C28 C27 C32 . . 113.3(5) ? C28 C27 C19 . . 120.6(5) ? C32 C27 C19 . . 125.7(5) ? C14 C9 C10 . . 113.8(5) ? C14 C9 C1 . . 120.1(5) ? C10 C9 C1 . . 125.5(5) ? F4 C28 C29 . . 117.1(5) ? F4 C28 C27 . . 117.7(5) ? C29 C28 C27 . . 125.2(5) ? N1 C1 C9 . . 113.3(4) ? N1 C1 C2 . . 110.0(4) ? C9 C1 C2 . . 114.7(4) ? C26 C21 C22 . . 119.0(5) ? C26 C21 C20 . . 121.1(5) ? C22 C21 C20 . . 119.9(5) ? C27 C19 N2 . . 113.2(4) ? C27 C19 C20 . . 114.3(4) ? N2 C19 C20 . . 110.0(4) ? C8 C3 C4 . . 118.4(5) ? C8 C3 C2 . . 120.3(5) ? C4 C3 C2 . . 121.3(5) ? C21 C20 C19 . . 111.0(4) ? F2 C14 C13 . . 117.9(5) ? F2 C14 C9 . . 117.6(5) ? C13 C14 C9 . . 124.6(5) ? F3 C32 C31 . . 117.2(5) ? F3 C32 C27 . . 118.1(5) ? C31 C32 C27 . . 124.8(5) ? C10 C11 C12 . . 117.7(5) ? C23 C22 C21 . . 120.2(5) ? C3 C2 C1 . . 110.2(4) ? C24 C25 C26 . . 120.2(6) ? F1 C10 C11 . . 117.3(5) ? F1 C10 C9 . . 118.0(5) ? C11 C10 C9 . . 124.7(5) ? C3 C8 C7 . . 120.4(6) ? N2 C36 C35 . . 104.2(5) ? N1 C15 C16 . . 103.7(5) ? N2 C33 C34 . . 103.2(5) ? C25 C26 C21 . . 120.3(5) ? C30 C31 C32 . . 118.0(6) ? C12 C13 C14 . . 118.2(5) ? C4 C5 C6 . . 120.0(6) ? C28 C29 C30 . . 117.2(6) ? C18 C17 C16 . . 105.3(5) ? C31 C30 C29 . . 121.4(5) ? C6 C7 C8 . . 120.1(6) ? C23 C24 C25 . . 120.0(6) ? C24 C23 C22 . . 120.2(6) ? N1 C18 C17 . . 104.2(5) ? C13 C12 C11 . . 121.0(5) ? C5 C4 C3 . . 121.4(6) ? C5 C6 C7 . . 119.7(6) ? C36 C35 C34 . . 105.5(5) ? C15 C16 C17 . . 105.7(5) ? C33 C34 C35 . . 105.9(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 F1 C10 . 1.357(6) ? F2 C14 . 1.352(6) ? F3 C32 . 1.353(6) ? F4 C28 . 1.361(6) ? N2 C36 . 1.491(7) ? N2 C33 . 1.500(7) ? N2 C19 . 1.520(6) ? N1 C15 . 1.498(7) ? N1 C18 . 1.502(7) ? N1 C1 . 1.513(6) ? C27 C28 . 1.390(7) ? C27 C32 . 1.396(7) ? C27 C19 . 1.513(7) ? C9 C14 . 1.385(7) ? C9 C10 . 1.400(7) ? C9 C1 . 1.518(7) ? C28 C29 . 1.378(8) ? C1 C2 . 1.528(7) ? C21 C26 . 1.391(7) ? C21 C22 . 1.392(8) ? C21 C20 . 1.513(7) ? C19 C20 . 1.526(7) ? C3 C8 . 1.392(8) ? C3 C4 . 1.393(8) ? C3 C2 . 1.510(7) ? C14 C13 . 1.381(8) ? C32 C31 . 1.373(8) ? C11 C10 . 1.369(8) ? C11 C12 . 1.393(9) ? C22 C23 . 1.389(8) ? C25 C24 . 1.381(9) ? C25 C26 . 1.383(8) ? C8 C7 . 1.394(8) ? C36 C35 . 1.513(9) ? C15 C16 . 1.515(8) ? C33 C34 . 1.521(8) ? C31 C30 . 1.373(9) ? C13 C12 . 1.374(9) ? C5 C4 . 1.378(9) ? C5 C6 . 1.382(10) ? C29 C30 . 1.386(9) ? C17 C18 . 1.516(8) ? C17 C16 . 1.550(9) ? C7 C6 . 1.388(10) ? C24 C23 . 1.375(9) ? C35 C34 . 1.534(10) ? 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 N1 H1' Cl1 . 0.985(10) 2.07(2) 3.021(5) 163(6) yes N2 H2 Cl2 . 0.984(10) 2.080(17) 3.052(5) 169(6) yes