#------------------------------------------------------------------------------ #$Date: 2018-01-17 02:18:13 +0200 (Wed, 17 Jan 2018) $ #$Revision: 205275 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/33/4033361.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4033361 loop_ _publ_author_name 'Druzhenko, Tetiana' 'Skalenko, Yevhen' 'Samoilenko, Maryna' 'Denisenko, Aleksandr' 'Zozulya, Sergey' 'Borysko, Petro O.' 'Sokolenko, Maria I.' 'Tarasov, Alexandr' 'Mykhailiuk, Pavel K.' _publ_section_title ; Photochemical synthesis of 2-azabicyclo[3.2.0]heptanes: advanced building blocks for drug discovery. Synthesis of 2,3-ethanoproline. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.7b02910 _journal_year 2018 _chemical_formula_sum 'C16 H17 F3 I N O3' _chemical_formula_weight 455.20 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 106.832(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8527(3) _cell_length_b 13.2507(4) _cell_length_c 13.5893(5) _cell_measurement_reflns_used 3332 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.7 _cell_measurement_theta_min 3.7 _cell_volume 1698.14(10) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 17164 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.999 _diffrn_reflns_theta_min 3.383 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.780 _exptl_crystal_description plate _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.853 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef 0.0190(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 4921 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0515 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.3973P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1433 _refine_ls_wR_factor_ref 0.1559 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3609 _reflns_number_total 4921 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo7b02910_si_004.cif _cod_data_source_block tolm318 _cod_database_code 4033361 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.699 _shelx_estimated_absorpt_t_max 0.910 _shelx_hkl_file ; 0 0 -2 1042.27 41.07 0 0 3 1.73 0.80 0 0 4 9999.00 384.92 0 0 5 -1.19 1.20 0 0 6 139.03 8.97 0 0 7 0.67 1.18 0 0 8 1050.94 46.47 0 0 9 -0.34 1.17 0 0 10 8.98 2.51 0 0 11 0.30 1.87 0 0 12 313.02 20.72 0 0 13 0.20 1.39 0 0 14 11.98 4.29 0 0 15 1.33 2.09 0 0 16 138.37 14.68 0 0 17 -1.94 2.42 0 0 18 6.95 4.31 0 -1 18 26.74 7.08 0 -1 17 1.34 2.35 0 -1 16 9.20 4.32 0 -1 15 15.46 4.38 0 -1 14 147.59 13.93 0 -1 13 47.91 7.21 0 -1 12 2.84 2.24 0 -1 11 91.63 9.19 0 -1 10 489.92 26.27 0 -1 9 98.12 8.56 0 -1 8 73.45 6.86 0 -1 7 225.39 13.30 0 -1 6 2550.23 110.33 0 1 -6 3014.26 110.79 0 -1 5 30.89 3.25 0 1 -5 34.47 3.46 0 -1 4 4.42 1.11 0 1 -4 5.42 1.30 0 -1 3 18.39 2.01 0 1 -3 18.37 2.01 0 1 -2 1857.19 72.62 0 1 3 19.32 2.18 0 1 4 7.55 1.51 0 1 5 28.19 3.27 0 1 6 2588.77 103.91 0 1 7 238.96 13.81 0 1 8 71.30 6.77 0 1 9 99.09 8.45 0 1 10 589.81 30.45 0 1 11 97.76 9.46 0 1 12 4.17 3.11 0 1 13 52.10 7.59 0 1 14 168.75 15.22 0 1 15 19.56 5.04 0 1 16 0.78 2.14 0 1 17 0.89 2.22 0 1 18 28.25 6.49 0 -2 18 5.65 3.81 0 -2 17 34.95 7.76 0 -2 16 6.63 3.01 0 -2 15 51.87 8.52 0 -2 14 2.53 2.57 0 -2 13 186.29 15.62 0 -2 12 147.55 12.76 0 -2 11 177.56 13.73 0 -2 10 69.65 7.45 0 -2 9 778.70 36.87 0 2 -8 425.84 20.62 0 -2 8 327.46 19.30 0 -2 7 1947.71 79.74 0 2 -7 1931.31 79.91 0 2 -6 114.96 7.89 0 -2 6 101.15 7.50 0 2 -5 2219.76 84.99 0 -2 5 2003.79 84.40 0 -2 4 1375.64 52.00 0 2 -4 1157.70 51.83 0 -2 3 954.47 39.34 0 2 -3 952.64 39.78 0 2 -2 871.39 31.17 0 -2 2 633.05 29.82 0 2 -1 1922.33 76.43 0 -2 -1 1546.79 60.36 0 2 2 700.78 29.07 0 2 3 1042.12 42.71 0 2 4 1390.54 56.80 0 2 5 2581.34 103.16 0 2 6 123.34 8.56 0 2 7 2105.75 86.47 0 2 8 335.05 18.60 0 2 9 672.66 32.93 0 2 10 79.38 7.97 0 2 11 163.57 12.92 0 2 12 126.04 11.71 0 2 13 197.22 15.84 0 2 14 7.62 3.59 0 2 15 54.85 8.58 0 2 16 11.44 4.14 0 2 17 25.80 6.42 0 2 18 1.51 1.53 0 -3 18 -2.35 2.03 0 -3 17 34.17 7.64 0 -3 16 -3.39 3.21 0 -3 15 74.94 10.39 0 -3 14 -1.56 1.31 0 -3 13 192.47 16.09 0 -3 12 27.32 5.01 0 -3 11 185.04 14.19 0 -3 10 41.97 5.65 0 3 -9 825.92 40.53 0 -3 9 915.47 40.90 0 -3 8 39.14 4.83 0 3 -8 41.76 5.19 0 -3 7 360.22 19.80 0 3 -7 408.44 20.65 0 3 -6 55.95 5.35 0 -3 6 45.49 4.86 0 -3 5 3936.08 155.13 0 3 -5 3964.73 155.82 0 -3 4 18.70 2.68 0 3 -4 27.54 3.49 0 -3 3 1911.91 77.94 0 3 -3 1987.79 78.99 0 -3 2 24.56 2.64 0 3 -2 34.45 3.58 0 3 -1 4603.40 219.52 0 -3 1 5530.71 218.91 0 -3 0 1.02 0.61 0 -3 0 1.53 0.95 0 3 0 2.21 0.90 0 -3 -1 6090.02 221.77 0 3 1 5701.49 221.08 0 -3 -1 5384.27 222.72 0 3 2 32.14 2.04 0 -3 -2 28.74 2.41 0 -3 -2 30.55 2.97 0 3 3 2332.69 92.56 0 3 4 24.69 3.06 0 3 5 4294.99 168.91 0 3 6 56.40 5.42 0 3 7 378.29 20.04 0 3 8 48.43 5.46 0 3 9 804.20 38.12 0 3 10 51.76 6.35 0 3 11 152.11 12.44 0 3 12 22.31 4.72 0 3 13 164.64 14.06 0 3 14 -2.28 1.70 0 3 15 77.62 10.03 0 3 16 2.61 2.52 0 3 17 30.07 6.88 0 3 18 1.53 3.07 0 -4 18 4.87 3.56 0 -4 17 7.70 4.08 0 -4 16 15.99 5.09 0 -4 15 19.58 5.30 0 -4 14 2.11 2.42 0 -4 13 9.68 4.08 0 -4 12 24.80 4.96 0 -4 11 175.34 13.86 0 4 -11 174.59 13.97 0 -4 10 1.18 1.17 0 4 -10 1.67 0.93 0 4 -9 5.20 1.96 0 -4 9 4.43 2.02 0 4 -8 436.52 23.06 0 -4 8 390.05 21.88 0 -4 7 139.35 10.16 0 4 -7 140.80 10.52 0 4 -6 2.36 1.37 0 -4 6 3.78 1.83 0 -4 5 966.86 44.33 0 4 -5 1105.41 45.93 0 -4 4 819.83 35.21 0 4 -4 771.77 36.06 0 -4 3 1720.94 66.89 0 4 -3 1526.04 67.80 0 -4 2 246.64 12.82 0 4 -2 246.16 14.10 0 -4 1 2553.01 99.27 0 -4 1 2494.08 97.18 0 4 -1 2345.08 100.49 0 -4 1 2558.82 99.55 0 -4 0 16.56 2.08 0 4 0 16.26 2.69 0 -4 0 17.38 2.50 0 -4 -1 2525.13 90.51 0 4 1 2428.22 92.08 0 -4 -2 212.62 11.83 0 4 2 235.26 10.06 0 -4 -2 215.25 10.69 0 4 3 1659.57 63.01 0 -4 -3 1523.90 65.43 0 -4 -3 1570.97 64.18 0 4 4 760.40 33.57 0 4 5 965.57 41.92 0 4 6 3.02 1.12 0 4 7 131.26 9.71 0 4 8 375.31 20.72 0 4 9 4.70 1.85 0 4 10 1.26 1.21 0 4 11 155.48 12.78 0 4 12 34.16 5.89 0 4 13 3.05 1.93 0 4 14 7.01 2.91 0 4 15 17.79 4.62 0 4 16 21.75 5.85 0 4 17 7.84 4.08 0 4 18 0.71 2.68 0 -5 17 14.17 5.49 0 -5 16 4.46 3.54 0 -5 15 2.46 2.37 0 -5 14 190.56 17.01 0 -5 13 45.63 7.33 0 -5 12 10.77 3.01 0 5 -12 12.09 3.63 0 -5 11 71.64 8.70 0 5 -11 87.15 9.38 0 -5 10 655.23 32.72 0 5 -10 583.50 32.55 0 -5 9 300.08 18.81 0 5 -9 314.68 19.62 0 -5 8 -0.32 1.55 0 5 -8 -0.31 1.20 0 -5 7 6.60 2.11 0 5 -7 5.44 2.08 0 5 -6 994.59 44.41 0 -5 6 919.46 42.75 0 -5 5 427.98 21.79 0 5 -5 427.00 23.09 0 -5 4 208.21 12.87 0 5 -4 250.02 14.87 0 -5 3 150.84 9.42 0 5 -3 126.12 9.92 0 -5 2 3433.29 137.13 0 5 -2 3495.07 139.20 0 -5 1 534.37 29.20 0 -5 1 601.06 29.28 0 5 -1 598.44 30.76 0 5 0 1.28 1.22 0 -5 0 0.39 1.04 0 -5 0 0.94 0.49 0 5 1 590.49 27.51 0 -5 -1 599.44 27.16 0 -5 -1 567.81 25.60 0 5 2 3870.85 148.26 0 -5 -2 3745.88 148.47 0 5 2 3487.02 145.12 0 -5 -3 169.27 10.01 0 5 3 140.81 7.19 0 -5 -3 155.42 8.43 0 -5 -4 233.78 12.08 0 -5 -4 216.70 13.07 0 5 5 385.64 20.12 0 5 6 857.18 38.87 0 5 7 6.60 1.68 0 5 8 -0.89 1.23 0 5 9 314.59 19.08 0 5 10 556.90 29.91 0 5 11 80.86 8.89 0 5 12 8.14 2.85 0 5 13 48.80 7.64 0 5 14 207.98 17.12 0 5 15 0.72 2.60 0 5 16 -1.41 1.42 0 5 17 6.52 3.01 0 -6 17 0.79 2.41 0 -6 16 45.33 8.53 0 -6 15 0.25 1.30 0 -6 14 5.74 3.08 0 -6 13 26.53 5.86 0 6 -12 335.58 23.28 0 -6 12 363.88 23.70 0 6 -11 57.79 7.88 0 -6 11 46.08 6.90 0 6 -10 17.51 4.22 0 -6 10 19.14 4.34 0 6 -9 67.75 8.00 0 -6 9 56.87 7.27 0 6 -8 867.61 43.08 0 -6 8 890.43 41.88 0 -6 7 53.34 6.15 0 6 -7 50.43 6.70 0 6 -6 96.81 9.44 0 -6 6 101.45 8.66 0 -6 5 8.27 2.39 0 6 -5 14.36 3.40 0 -6 4 2183.92 86.79 0 6 -4 1995.60 88.42 0 6 -3 244.17 15.99 0 -6 3 255.72 14.70 0 6 -2 180.95 12.87 0 -6 2 182.24 9.80 0 -6 2 190.59 11.97 0 6 -1 2.14 1.53 0 -6 1 2.69 0.62 0 -6 1 2.78 1.42 0 -6 1 1.26 1.04 0 -6 0 2525.00 101.90 0 -6 0 2430.13 100.51 0 6 0 2629.28 103.43 0 -6 -1 2.59 1.27 0 6 1 5.14 1.98 0 -6 -1 4.17 1.25 0 6 2 144.71 8.03 0 -6 -2 160.79 9.22 0 -6 -2 168.34 10.81 0 6 2 172.76 10.88 0 -6 -3 252.18 13.70 0 -6 -3 193.57 10.99 0 6 3 213.99 12.53 0 6 3 210.28 10.03 0 -6 -4 2286.88 88.80 0 -6 -4 2069.32 85.89 0 6 4 2112.43 84.05 0 -6 -5 7.92 1.70 0 6 5 5.63 1.55 0 -6 -5 17.36 3.26 0 -6 -6 101.31 8.66 0 6 6 94.87 8.31 0 6 7 31.56 4.75 0 6 8 946.53 44.22 0 6 9 62.17 7.07 0 6 10 17.51 4.18 0 6 11 70.36 8.38 0 6 12 283.44 19.94 0 6 13 27.04 5.41 0 6 14 1.47 1.40 0 6 15 4.48 3.53 0 6 16 24.00 5.83 0 6 17 1.30 1.96 0 -7 17 -3.03 3.27 0 -7 16 -0.03 2.55 0 -7 15 42.94 8.26 0 -7 14 14.23 4.59 0 -7 13 -1.48 2.28 0 7 -13 0.31 1.02 0 7 -12 4.98 2.81 0 -7 12 10.16 2.56 0 7 -11 191.20 16.48 0 -7 11 198.49 15.83 0 -7 10 266.97 18.57 0 7 -10 274.27 19.91 0 -7 9 99.39 9.90 0 7 -9 88.15 10.22 0 -7 8 181.89 13.73 0 7 -8 165.75 14.25 0 7 -7 156.88 13.56 0 -7 7 167.69 12.48 0 -7 6 990.26 44.76 0 7 -6 920.73 46.34 0 -7 5 359.34 19.94 0 7 -5 327.14 21.07 0 -7 4 506.89 24.91 0 7 -4 420.05 25.45 0 -7 3 431.21 23.33 0 7 -3 467.90 25.36 0 7 -2 663.58 31.51 0 -7 2 559.36 25.53 0 -7 2 637.57 29.74 0 -7 1 524.49 25.07 0 -7 1 472.36 19.91 0 -7 0 7.65 1.95 0 -7 0 2.55 1.57 0 7 0 1.84 1.52 0 -7 -1 562.78 25.52 0 7 1 518.22 27.43 0 -7 -1 543.95 27.10 0 7 2 503.97 22.35 0 -7 -2 536.61 26.06 0 -7 -2 459.26 23.39 0 7 2 584.73 26.69 0 7 3 402.00 17.62 0 7 3 453.61 21.62 0 -7 -3 459.69 22.37 0 -7 -4 395.64 19.49 0 -7 -4 417.96 22.18 0 7 4 453.37 21.53 0 7 4 394.19 17.73 0 -7 -5 353.22 19.26 0 -7 -5 302.41 16.50 0 7 6 1075.24 48.66 0 -7 -6 1027.01 45.97 0 -7 -6 1099.26 48.86 0 -7 -7 178.80 13.10 0 -7 -7 148.89 10.91 0 7 7 173.35 12.64 0 7 8 163.63 13.03 0 -7 -8 206.14 14.72 0 7 9 91.78 9.41 0 7 10 248.51 17.47 0 7 11 201.82 15.85 0 7 12 10.32 3.92 0 7 13 1.32 1.62 0 7 14 19.68 4.87 0 7 15 38.73 7.63 0 7 16 -1.02 2.55 0 7 17 -1.61 3.05 0 -8 16 5.43 2.86 0 -8 15 14.18 5.10 0 8 -14 21.57 5.84 0 -8 14 29.63 6.50 0 8 -13 65.67 10.05 0 -8 13 78.99 10.33 0 8 -12 11.37 3.62 0 -8 12 10.43 3.52 0 -8 11 160.83 14.17 0 8 -11 137.08 14.22 0 8 -10 55.23 8.56 0 -8 10 72.94 8.58 0 -8 9 308.60 20.47 0 8 -9 317.52 22.30 0 -8 8 14.42 3.47 0 8 -8 22.60 5.14 0 -8 7 385.17 22.08 0 8 -7 327.52 22.90 0 -8 6 55.19 6.93 0 8 -6 55.04 7.67 0 8 -5 871.90 45.58 0 -8 5 970.21 44.15 0 -8 4 192.19 13.17 0 8 -4 144.91 13.03 0 8 -3 1006.38 48.82 0 -8 3 1048.91 43.74 0 -8 3 990.96 47.14 0 -8 2 34.00 3.03 0 -8 2 29.86 4.73 0 8 -2 43.02 5.94 0 -8 1 759.42 37.82 0 8 -1 884.62 40.50 0 8 0 193.89 14.31 0 -8 0 228.95 14.33 0 -8 -1 855.01 37.75 0 -8 -1 789.80 39.36 0 8 1 904.93 40.82 0 8 2 29.60 4.58 0 -8 -2 33.23 3.88 0 -8 -2 29.67 4.65 0 8 2 31.24 3.27 0 -8 -3 931.66 41.52 0 8 3 955.17 39.54 0 -8 -3 1063.24 45.28 0 8 3 927.84 43.86 0 -8 -4 118.77 8.58 0 -8 -4 159.52 11.74 0 8 4 136.52 7.31 0 8 4 137.89 10.35 0 8 5 762.13 35.58 0 -8 -5 717.78 33.68 0 -8 -5 816.68 37.70 0 8 6 61.00 6.16 0 -8 -6 49.04 6.61 0 8 6 55.35 6.93 0 -8 -6 50.37 5.33 0 -8 -7 304.37 17.75 0 -8 -7 333.26 20.72 0 8 7 324.89 20.35 0 -8 -8 14.81 3.65 0 8 8 29.18 5.26 0 -8 -8 18.18 3.37 0 -8 -9 301.55 20.58 0 8 9 293.88 19.80 0 -8 -9 301.50 18.52 0 8 10 87.36 9.52 0 -8 -10 65.10 8.55 0 -8 -10 55.05 6.99 0 -8 -11 190.23 15.97 0 8 11 162.91 14.62 0 -8 -12 4.33 2.34 0 8 12 13.78 3.91 0 -8 -13 73.77 9.97 0 8 13 86.68 10.60 0 8 14 27.82 6.06 0 8 15 6.74 3.37 0 -8 -16 0.75 1.65 0 8 16 4.60 2.80 0 -8 -17 28.11 7.06 0 -9 16 9.70 4.86 0 -9 15 14.09 4.80 0 -9 14 -0.42 1.65 0 9 -14 3.38 2.49 0 9 -13 61.87 10.02 0 -9 13 79.08 10.42 0 -9 12 54.06 8.30 0 9 -12 49.86 8.82 0 9 -11 46.38 8.34 0 -9 11 56.31 8.31 0 9 -10 28.53 6.56 0 -9 10 40.04 6.45 0 -9 9 97.49 10.29 0 9 -9 95.53 11.50 0 -9 8 94.47 10.05 0 9 -8 99.46 11.61 0 -9 7 358.13 22.07 0 9 -7 318.58 23.14 0 9 -6 48.72 7.19 0 -9 6 59.37 7.19 0 9 -5 351.54 24.01 0 -9 5 414.88 23.60 0 9 -4 3.26 2.16 0 -9 4 0.44 0.50 0 -9 4 0.05 1.29 0 9 -3 446.97 25.36 0 -9 3 371.54 18.91 0 -9 3 428.09 23.74 0 9 -2 40.88 6.18 0 -9 2 28.04 2.44 0 -9 1 289.65 18.00 0 9 -1 284.47 19.08 0 9 0 1.68 1.40 0 -9 0 -0.87 1.16 0 -9 -1 276.28 15.69 0 9 1 276.60 18.04 0 -9 -1 283.64 17.68 0 9 2 38.46 3.90 0 -9 -2 35.43 5.40 0 9 2 34.91 5.25 0 -9 -2 34.21 4.19 0 9 3 368.70 17.15 0 9 3 394.50 21.65 0 -9 -3 325.65 18.52 0 -9 -3 415.20 22.50 0 9 4 0.95 1.32 0 -9 -4 -0.44 0.79 0 -9 -4 -0.38 1.49 0 9 4 1.71 0.63 0 9 5 331.30 18.54 0 -9 -5 341.24 20.53 0 -9 -6 53.30 5.66 0 9 6 54.44 6.23 0 9 6 60.90 7.74 0 -9 -6 76.11 8.49 0 9 7 301.27 20.04 0 -9 -7 265.06 16.36 0 9 7 270.34 16.95 0 -9 -7 304.05 19.85 0 -9 -8 102.67 10.87 0 9 8 99.30 10.63 0 -9 -8 91.54 8.55 0 9 9 95.14 10.31 0 -9 -9 84.86 10.14 0 9 10 31.52 5.73 0 -9 -10 35.49 6.33 0 -9 -11 44.05 7.63 0 9 11 65.35 9.11 0 -9 -12 49.03 8.17 0 9 12 58.72 8.81 0 9 13 58.51 9.24 0 -9 -13 68.39 9.97 0 9 14 1.88 1.30 0 -9 -14 -1.23 1.16 0 -9 -15 11.50 4.58 0 9 15 22.62 5.99 0 9 16 13.80 4.86 0 -9 -16 7.46 3.58 0 10 -15 8.93 4.48 0 -10 15 17.36 5.79 0 10 -14 23.92 6.80 0 -10 14 19.63 5.71 0 -10 13 5.26 2.96 0 10 -13 3.90 3.42 0 10 -12 42.14 8.00 0 -10 12 47.08 8.08 0 -10 11 38.30 6.84 0 10 -11 33.73 7.38 0 -10 10 15.10 4.47 0 10 -10 12.47 4.48 0 -10 9 38.20 6.67 0 10 -9 28.15 6.30 0 -10 8 114.92 11.56 0 10 -8 104.74 12.62 0 -10 7 422.64 25.27 0 10 -7 349.93 25.72 0 -10 6 26.79 5.28 0 10 -6 16.62 4.53 0 -10 6 20.43 3.78 0 10 -5 10.46 3.36 0 -10 5 11.78 3.46 0 10 -4 596.74 34.65 0 -10 4 641.84 34.09 0 -10 3 404.71 25.03 0 10 -3 434.01 26.45 0 10 -2 3.03 2.38 0 -10 1 152.11 12.52 0 10 -1 168.75 13.82 0 -10 0 76.84 8.38 0 10 0 92.62 9.50 0 -10 -1 152.26 12.71 0 10 1 164.27 10.48 0 10 1 160.09 13.14 0 10 2 1.82 1.62 0 -10 -2 3.13 1.35 0 10 2 1.93 1.11 0 -10 -2 -2.23 1.10 0 -10 -3 462.88 25.34 0 10 3 426.65 24.16 0 -10 -3 397.78 21.30 0 -10 -4 579.52 30.81 0 10 4 562.41 29.48 0 -10 -4 531.10 26.60 0 -10 -5 9.90 2.37 0 10 5 11.82 3.12 0 -10 -5 14.84 4.09 0 10 6 18.78 4.06 0 -10 -6 21.42 4.74 0 10 6 24.37 4.82 0 10 7 400.54 24.32 0 10 7 317.39 20.13 0 -10 -7 372.98 23.91 0 -10 -8 128.77 12.72 0 10 8 110.30 12.01 0 -10 -9 23.48 5.23 0 10 9 36.87 6.61 0 10 10 10.84 4.20 0 -10 -10 7.38 3.50 0 10 11 42.60 7.63 0 -10 -11 40.15 7.31 0 -10 -12 53.19 8.95 0 10 12 51.45 8.55 0 10 13 2.04 2.22 0 -10 -13 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5.91 5 -3 8 349.91 22.92 5 -3 9 2.55 3.21 5 -3 10 18.75 4.84 5 -3 11 -2.09 1.78 5 -3 12 34.75 7.14 5 -3 13 1.02 2.99 5 -3 14 10.68 4.77 5 -3 15 -0.30 2.00 -5 2 19 1.73 4.80 -5 2 18 39.78 10.38 -5 2 17 7.27 5.08 -5 2 17 5.89 3.18 -5 2 16 7.03 3.61 -5 2 16 6.63 2.79 -5 2 15 -1.81 3.18 -5 2 15 2.28 1.87 -5 2 14 139.61 16.55 -5 2 14 136.78 12.07 -5 2 13 95.21 13.00 -5 2 13 98.79 9.44 -5 2 12 33.66 7.47 -5 2 12 34.57 4.98 -5 2 11 29.34 4.30 -5 2 11 27.47 5.94 -5 2 10 631.28 30.49 -5 2 10 689.54 38.23 -5 2 9 238.97 18.43 -5 2 9 217.71 12.91 -5 2 8 598.20 33.42 -5 2 8 571.41 26.52 -5 2 8 595.64 29.73 -5 2 7 7.95 1.54 -5 2 7 10.87 3.41 -5 2 7 9.83 2.62 -5 2 6 584.94 30.81 -5 2 6 554.56 24.03 -5 2 6 518.03 27.09 -5 2 5 169.15 10.33 -5 2 5 138.37 7.66 -5 2 5 165.73 12.81 -5 2 5 137.69 10.40 -5 2 4 466.46 23.34 -5 2 4 420.19 19.03 -5 2 4 502.77 25.97 -5 2 4 539.53 23.49 -5 2 3 150.79 9.88 5 -2 -3 125.78 8.39 -5 2 3 162.19 11.93 -5 2 3 142.77 10.16 -5 2 2 1906.69 79.70 5 -2 -2 1924.93 78.60 -5 2 2 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19.80 5.62 -12 2 10 1.77 2.57 -12 2 10 3.19 3.32 -12 2 9 1.88 2.29 -12 2 8 4.92 3.50 -12 2 7 25.34 6.38 -12 2 6 3.72 2.92 -12 2 5 23.92 6.00 -12 2 4 -0.27 2.93 -12 2 3 18.42 5.56 -12 2 3 19.96 5.30 -12 2 2 0.40 1.31 -12 2 2 0.39 1.66 -12 2 1 -1.21 1.26 -12 2 1 -0.71 1.93 -12 2 0 -1.75 2.66 -12 2 0 1.26 2.92 -12 2 -1 5.64 3.53 -12 2 -1 7.21 4.00 -12 2 -2 -0.28 2.90 -12 2 -2 -0.07 1.21 -12 2 -3 0.32 1.14 -12 2 -3 -2.87 2.59 -12 2 -4 -0.14 1.95 -12 2 -4 -0.01 1.73 -12 2 -5 1.47 2.17 -12 2 -5 0.87 1.63 -12 1 14 -0.72 2.31 -12 1 13 2.11 3.03 -12 1 12 3.45 3.66 -12 1 11 0.58 3.05 -12 1 11 4.49 2.83 -12 1 10 14.73 6.33 -12 1 10 8.06 3.76 -12 1 9 4.00 2.50 -12 1 8 3.68 3.28 -12 1 7 -2.09 2.00 -12 1 6 30.22 6.60 -12 1 5 3.25 2.88 -12 1 5 1.23 1.91 -12 1 4 2.02 2.11 -12 1 4 0.70 2.23 -12 1 3 7.30 3.61 -12 1 3 3.73 2.94 -12 1 2 21.97 5.77 -12 1 2 21.72 5.64 -12 1 1 -1.57 2.39 -12 1 1 0.40 1.76 -12 1 0 7.20 3.63 -12 1 0 4.03 2.58 -12 1 -1 1.71 1.26 -12 1 -1 -0.64 1.33 -12 1 -2 0.89 2.49 -12 1 -2 0.02 1.27 -12 1 -3 3.95 2.85 -12 1 -3 1.40 2.03 -12 1 -4 6.04 4.69 -12 1 -4 -0.20 1.98 -12 1 -5 -0.85 1.62 -12 0 14 5.18 3.77 -12 0 13 -3.38 3.86 -12 0 12 60.32 12.50 -12 0 11 -1.97 3.08 -12 0 10 6.07 4.04 -12 0 10 4.94 3.04 -12 0 9 1.28 1.11 -12 0 8 15.07 5.34 -12 0 8 17.65 4.95 -12 0 7 0.29 1.37 -12 0 7 -0.13 1.83 -12 0 6 12.02 4.41 -12 0 6 8.99 3.28 -12 0 5 0.64 1.60 -12 0 5 -0.17 1.35 -12 0 4 35.49 7.60 -12 0 4 46.45 7.91 -12 0 3 -0.58 2.47 -12 0 3 0.80 2.00 -12 0 2 10.14 4.30 -12 0 2 6.80 3.49 -12 0 1 -1.96 1.06 -12 0 1 1.86 1.52 -12 0 0 13.72 5.31 -12 0 0 16.06 4.95 -12 0 -1 -2.60 2.94 -12 0 -1 -1.09 2.20 -12 0 -2 1.95 3.28 -12 0 -2 1.61 1.95 -12 0 -3 1.22 1.95 -12 0 -3 1.22 2.00 -12 0 -4 10.52 5.95 -12 -1 14 0.56 1.58 -12 -1 13 -3.20 4.84 -12 -1 12 -1.31 2.05 -12 -1 11 1.64 2.02 -12 -1 10 7.96 3.96 -12 -1 10 13.16 4.78 -12 -1 10 7.96 4.96 -12 -1 9 3.14 1.69 -12 -1 9 5.15 3.10 -12 -1 8 4.65 3.49 -12 -1 8 3.89 2.40 -12 -1 7 0.66 1.78 -12 -1 7 2.10 2.32 -12 -1 6 30.05 7.43 -12 -1 6 30.29 6.41 -12 -1 5 4.25 2.98 -12 -1 5 0.76 1.92 -12 -1 4 0.57 1.53 -12 -1 4 2.69 2.54 -12 -1 3 5.06 3.35 -12 -1 3 1.74 2.39 -12 -1 2 16.22 5.54 -12 -1 2 24.72 6.00 -12 -1 1 0.02 2.36 -12 -1 1 3.00 2.36 -12 -1 0 4.43 2.65 -12 -1 0 6.42 3.56 -12 -1 -1 -0.14 1.53 -12 -1 -1 -1.25 2.10 -12 -1 -2 4.22 2.13 -12 -1 -3 2.17 3.05 -12 -1 -4 -4.50 4.33 -12 -2 13 4.66 4.41 -12 -2 12 0.65 1.83 -12 -2 11 14.91 5.97 -12 -2 10 -2.40 2.95 -12 -2 10 4.56 4.27 -12 -2 9 0.11 1.33 -12 -2 9 4.89 3.12 -12 -2 8 7.67 4.14 -12 -2 8 4.40 2.34 -12 -2 7 22.43 6.50 -12 -2 7 24.58 5.75 -12 -2 6 -0.41 1.62 -12 -2 6 0.16 1.44 -12 -2 5 24.44 7.09 -12 -2 5 21.37 5.20 -12 -2 4 -0.57 2.63 -12 -2 4 -0.91 2.29 -12 -2 3 27.63 7.29 -12 -2 3 23.54 5.73 -12 -2 2 3.35 2.99 -12 -2 2 1.91 2.46 -12 -2 1 0.31 1.94 -12 -2 1 2.61 1.21 -12 -2 0 3.26 2.88 -12 -2 0 6.10 3.02 -12 -2 -1 5.47 1.86 -12 -2 -2 1.01 1.69 -12 -2 -3 2.24 2.82 -12 -2 -4 3.55 3.24 -12 -3 13 25.42 8.82 -12 -3 12 1.76 1.39 -12 -3 11 6.31 4.63 -12 -3 10 3.63 2.79 -12 -3 10 0.13 1.75 -12 -3 9 13.46 5.21 -12 -3 8 1.16 2.77 -12 -3 8 3.80 2.34 -12 -3 7 11.11 4.40 -12 -3 7 9.32 3.79 -12 -3 6 17.07 5.95 -12 -3 6 21.28 5.72 -12 -3 5 9.97 4.62 -12 -3 5 17.28 4.95 -12 -3 4 -0.90 2.10 -12 -3 4 0.79 2.09 -12 -3 3 -1.27 2.19 -12 -3 3 -0.17 1.22 -12 -3 2 -1.37 2.23 -12 -3 2 3.95 2.44 -12 -3 1 29.59 8.31 -12 -3 0 9.45 4.12 -12 -3 -1 2.56 2.83 -12 -3 -2 2.50 2.95 -12 -3 -3 8.77 4.28 -12 -3 -4 2.73 2.24 -12 -4 13 -0.84 2.04 -12 -4 12 -4.61 4.64 -12 -4 11 -0.10 3.66 -12 -4 10 0.29 2.53 -12 -4 10 7.02 5.73 -12 -4 9 0.57 1.49 -12 -4 8 2.42 2.78 -12 -4 7 16.66 6.21 -12 -4 7 14.55 4.72 -12 -4 6 2.26 2.06 -12 -4 6 3.70 2.63 -12 -4 5 0.91 1.62 -12 -4 5 -0.17 1.11 -12 -4 4 6.80 3.38 -12 -4 4 5.54 2.48 -12 -4 3 8.80 4.65 -12 -4 2 3.81 3.69 -12 -4 1 6.13 3.54 -12 -4 0 0.48 2.88 -12 -4 -1 4.52 4.04 -12 -4 -2 -0.46 3.02 -12 -4 -3 -0.48 3.05 -12 -5 12 1.77 3.60 -12 -5 11 0.16 2.01 -12 -5 10 1.78 2.44 -12 -5 10 7.42 4.55 -12 -5 9 16.34 6.00 -12 -5 8 2.34 3.85 -12 -5 7 3.16 1.62 -12 -5 6 7.85 5.01 -12 -5 5 -2.22 3.13 -12 -5 5 -0.40 1.20 -12 -5 4 -0.07 1.24 -12 -5 3 -1.05 3.08 -12 -5 2 15.87 6.49 -12 -5 1 -0.13 1.87 -12 -5 0 1.27 2.30 -12 -5 -1 -0.50 1.57 -12 -5 -2 7.30 4.53 -12 -5 -3 -0.32 2.43 -12 -6 12 8.29 4.90 -12 -6 11 -0.16 1.96 -12 -6 10 7.27 4.29 -12 -6 10 15.71 6.18 -12 -6 9 0.65 3.08 -12 -6 8 23.63 7.35 -12 -6 7 1.58 3.65 -12 -6 6 5.33 3.16 -12 -6 5 2.43 2.68 -12 -6 4 14.27 5.98 -12 -6 3 -1.19 1.59 -12 -6 2 7.46 4.23 -12 -6 1 5.62 4.32 -12 -6 0 7.84 4.65 -12 -6 -1 3.33 3.43 -12 -6 -2 5.39 3.96 -12 -7 11 4.42 3.56 -12 -7 10 -2.82 2.17 -12 -7 9 10.45 5.09 -12 -7 8 9.57 5.61 -12 -7 7 0.05 1.35 -12 -7 6 -2.33 2.49 -12 -7 5 15.49 6.86 -12 -7 4 0.91 2.72 -12 -7 3 -1.41 3.48 -12 -7 2 3.50 3.68 -12 -7 1 6.50 4.00 -12 -7 0 -0.31 2.76 -12 -7 -1 -1.62 2.89 -12 -8 9 8.23 4.15 -12 -8 8 -2.72 3.12 -12 -8 7 6.98 4.04 -12 -8 6 0.59 2.49 -12 -8 5 -0.99 2.90 -12 -8 4 -2.06 2.15 -12 -8 3 11.23 5.44 -12 -8 2 -4.39 4.41 -12 -8 1 2.51 3.75 12 9 -10 6.64 4.89 -12 -9 7 1.55 1.65 -12 -9 6 -1.34 1.25 -12 -9 5 0.06 1.60 -12 -9 4 -4.99 3.76 -12 -9 3 -0.61 2.70 12 10 -9 -0.43 1.77 -13 6 7 -1.16 2.30 -13 6 6 4.62 3.92 -13 6 5 -1.32 3.13 -13 6 4 1.59 1.92 -13 6 3 7.83 4.52 -13 6 2 2.28 2.70 -13 5 9 2.62 2.15 -13 5 8 2.43 2.22 -13 5 7 5.77 3.90 -13 5 6 -2.11 2.33 -13 5 5 6.36 3.78 -13 5 4 -0.68 2.08 -13 5 3 4.22 3.65 -13 5 2 -3.09 2.29 -13 5 1 -0.78 1.52 -13 5 0 -0.27 2.31 -13 4 10 1.30 2.65 -13 4 9 -0.93 2.37 -13 4 8 6.26 3.52 -13 4 7 15.99 5.30 -13 4 6 5.05 3.73 -13 4 5 2.55 3.04 -13 4 4 10.03 4.30 -13 4 3 8.73 4.31 -13 4 2 3.30 1.86 -13 4 1 -0.94 2.77 -13 4 0 2.50 2.04 -13 4 -1 1.16 3.19 -13 3 12 1.89 1.37 -13 3 10 15.67 5.23 -13 3 9 -0.88 2.25 -13 3 8 2.38 2.43 -13 3 7 -2.49 2.71 -13 3 6 4.88 2.91 -13 3 5 1.66 1.58 -13 3 4 1.02 2.13 -13 3 3 0.91 1.58 -13 3 2 10.69 4.41 -13 3 1 0.71 2.24 -13 3 0 -0.30 1.71 -13 3 -1 2.25 2.61 -13 3 -2 2.01 2.59 -13 3 -3 -1.05 1.82 -13 2 12 2.39 2.95 -13 2 11 7.24 3.85 -13 2 10 5.07 3.38 -13 2 9 -1.59 2.40 -13 2 8 7.64 3.76 -13 2 7 4.57 3.44 -13 2 6 0.10 2.65 -13 2 5 4.78 3.24 -13 2 4 2.96 1.95 -13 2 3 8.46 3.81 -13 2 2 1.55 2.07 -13 2 1 -0.68 1.15 -13 2 0 4.33 2.50 -13 2 0 2.37 2.36 -13 2 -1 2.32 2.77 -13 2 -1 1.15 1.97 -13 2 -2 1.41 1.12 -13 2 -2 -0.59 2.36 -13 2 -3 2.40 3.06 -13 1 12 1.29 2.49 -13 1 11 -0.48 2.50 -13 1 10 -0.96 1.50 -13 1 9 3.70 3.15 -13 1 8 1.16 1.55 -13 1 7 -0.94 1.28 -13 1 6 8.88 3.87 -13 1 5 5.35 3.01 -13 1 4 1.22 1.30 -13 1 3 -0.63 2.13 -13 1 3 -2.50 2.72 -13 1 2 0.94 1.61 -13 1 2 3.49 2.95 -13 1 1 5.08 3.21 -13 1 1 5.23 3.40 -13 1 0 3.32 4.18 -13 1 0 -5.04 3.61 -13 1 -1 1.63 1.22 -13 1 -1 1.55 2.53 -13 1 -2 5.38 4.77 -13 1 -2 1.90 2.21 -13 0 12 5.21 4.71 -13 0 11 -0.63 2.94 -13 0 10 -0.68 1.37 -13 0 9 7.30 3.53 -13 0 8 0.75 2.15 -13 0 7 8.01 3.48 -13 0 6 1.21 2.50 -13 0 5 9.08 4.53 -13 0 5 8.59 3.93 -13 0 4 -1.87 2.91 -13 0 4 -0.63 2.02 -13 0 3 0.14 1.86 -13 0 3 -0.45 2.14 -13 0 2 0.45 2.52 -13 0 2 -0.41 1.92 -13 0 1 -1.14 2.30 -13 0 1 1.76 1.80 -13 0 0 1.58 2.35 -13 0 0 1.17 2.34 -13 0 -1 5.07 4.23 -13 0 -1 4.21 2.15 -13 0 -2 -2.01 3.32 -13 -1 11 -2.18 3.05 -13 -1 10 -1.03 1.82 -13 -1 9 6.01 3.71 -13 -1 8 -1.27 1.14 -13 -1 8 -0.32 1.97 -13 -1 7 1.31 2.88 -13 -1 7 0.07 2.15 -13 -1 6 8.69 4.32 -13 -1 6 3.61 3.14 -13 -1 5 9.20 4.31 -13 -1 5 6.49 4.10 -13 -1 4 1.93 3.10 -13 -1 4 5.73 3.08 -13 -1 3 1.74 3.40 -13 -1 3 1.30 1.49 -13 -1 2 1.21 2.43 -13 -1 2 -0.92 2.04 -13 -1 1 3.71 3.39 -13 -1 1 2.78 3.17 -13 -1 0 -2.13 2.69 -13 -1 -1 1.55 3.15 -13 -1 -2 4.52 3.73 -13 -2 11 7.96 4.71 -13 -2 10 0.80 1.27 -13 -2 9 -2.39 2.82 -13 -2 9 2.03 1.62 -13 -2 8 0.29 2.68 -13 -2 8 1.42 1.63 -13 -2 7 1.22 2.79 -13 -2 7 5.28 2.99 -13 -2 6 1.99 2.48 -13 -2 6 1.77 2.45 -13 -2 5 0.24 2.38 -13 -2 5 -0.99 1.78 -13 -2 4 0.66 2.16 -13 -2 4 4.81 3.45 -13 -2 3 3.90 3.05 -13 -2 3 3.78 2.83 -13 -2 2 -3.12 2.83 -13 -2 2 -0.43 1.66 -13 -2 1 0.79 1.79 -13 -2 0 -0.30 2.10 -13 -2 -1 0.10 1.53 -13 -3 10 7.17 3.91 -13 -3 9 -0.20 1.87 -13 -3 8 3.04 2.89 -13 -3 8 0.20 2.50 -13 -3 7 -0.46 2.23 -13 -3 7 2.25 1.99 -13 -3 6 4.54 3.19 -13 -3 6 4.84 2.95 -13 -3 5 -1.16 2.45 -13 -3 5 -1.23 1.26 -13 -3 4 2.07 3.16 -13 -3 4 1.26 1.79 -13 -3 3 1.30 1.62 -13 -3 2 10.40 5.78 -13 -3 1 -2.24 3.20 -13 -3 0 3.38 3.04 -13 -3 -1 0.50 2.15 -13 -4 10 -1.76 2.54 -13 -4 9 -0.59 2.32 -13 -4 8 8.83 4.58 -13 -4 7 12.86 5.22 -13 -4 7 11.07 4.34 -13 -4 6 -3.08 3.73 -13 -4 6 0.62 1.46 -13 -4 5 -0.79 1.73 -13 -4 5 0.05 0.97 -13 -4 4 7.24 4.83 -13 -4 3 6.50 5.23 -13 -4 2 1.58 2.80 -13 -4 1 3.24 4.45 -13 -4 0 -1.95 1.79 -13 -5 10 1.59 2.09 -13 -5 9 0.20 2.45 -13 -5 8 4.16 3.56 -13 -5 7 2.95 2.12 -13 -5 6 1.86 2.71 -13 -5 5 -1.06 2.49 -13 -5 4 1.50 1.88 -13 -5 3 1.09 2.10 -13 -5 2 3.27 3.48 -13 -5 1 6.10 4.79 -13 -6 9 1.53 1.82 -13 -6 8 -0.35 2.17 -13 -6 7 0.48 1.30 -13 -6 6 2.64 3.32 -13 -6 5 1.95 3.69 -13 -6 4 -1.51 2.01 -13 -6 3 5.24 3.78 -14 2 7 -0.46 1.73 -14 2 6 -0.69 2.26 -14 2 5 7.72 4.06 -14 2 4 1.18 1.63 -14 2 3 1.28 2.07 -14 2 2 2.26 3.12 -14 2 1 -0.81 2.10 -14 1 8 2.22 3.02 -14 1 7 0.39 1.47 -14 1 6 3.09 3.19 -14 1 5 -1.36 2.50 -14 1 4 -2.36 2.86 -14 1 3 -0.24 1.76 -14 1 2 7.32 5.62 -14 1 1 1.87 2.76 -14 1 0 -0.37 1.96 -14 0 8 2.32 2.29 -14 0 7 5.89 3.44 -14 0 6 -1.42 2.04 -14 0 5 0.45 1.28 -14 0 4 10.37 4.31 -14 0 3 -0.80 1.41 -14 0 3 2.12 1.86 -14 0 2 2.33 2.29 -14 0 2 -1.55 2.88 -14 0 1 -2.70 2.92 -14 0 1 -1.53 2.16 -14 -1 9 5.17 4.13 -14 -1 8 -1.52 3.02 -14 -1 7 1.08 2.02 -14 -1 6 0.38 1.61 -14 -1 5 -0.78 1.82 -14 -1 5 -0.06 1.99 -14 -1 4 -1.30 0.95 -14 -1 4 1.64 2.07 -14 -1 3 -1.18 1.57 -14 -1 3 -1.40 2.93 -14 -1 2 4.75 4.13 -14 -2 9 2.38 2.73 -14 -2 8 0.12 1.33 -14 -2 8 0.82 1.69 -14 -2 7 4.57 4.01 -14 -2 7 -1.59 2.58 -14 -2 6 1.95 2.85 -14 -2 6 1.19 2.47 -14 -2 5 -1.27 2.35 -14 -2 5 3.34 2.17 -14 -2 4 2.62 3.36 -14 -2 4 -4.09 2.92 -14 -2 3 -0.46 2.54 -14 -3 9 1.30 2.15 -14 -3 8 -1.59 3.03 -14 -3 8 0.55 1.34 -14 -3 7 -1.32 2.62 -14 -3 7 3.17 3.09 -14 -3 6 1.20 1.36 -14 -3 6 0.04 1.41 -14 -3 5 -1.80 3.45 -14 -3 4 2.19 1.88 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 66968 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp I1 I 0.71461(3) 0.66357(2) 0.62427(2) 0.06866(17) Uani 1 1 d . . F1 F 1.0408(3) 0.4421(2) 0.1278(2) 0.0824(8) Uani 1 1 d . . F2 F 0.8692(3) 0.5453(3) 0.0763(2) 0.0924(9) Uani 1 1 d . . F3 F 1.0672(3) 0.5935(2) 0.1769(3) 0.0925(9) Uani 1 1 d . . O1 O 0.9698(3) 0.54572(19) 0.3279(2) 0.0542(6) Uani 1 1 d . . O2 O 0.5276(3) 0.4661(2) 0.1923(2) 0.0678(8) Uani 1 1 d . . O3 O 0.4401(3) 0.6902(2) 0.4484(3) 0.0658(7) Uani 1 1 d . . N1 N 0.8311(3) 0.4195(2) 0.2412(2) 0.0447(6) Uani 1 1 d . . C1 C 0.7768(4) 0.3929(2) 0.3288(3) 0.0461(7) Uani 1 1 d . . C2 C 0.8936(5) 0.3420(3) 0.4167(4) 0.0592(10) Uani 1 1 d . . H2B H 0.9893 0.3605 0.4178 0.071 Uiso 1 1 calc R U H2A H 0.8799 0.3503 0.4841 0.071 Uiso 1 1 calc R U C3 C 0.8471(6) 0.2392(3) 0.3683(4) 0.0825(14) Uani 1 1 d . . H3B H 0.8288 0.1902 0.4159 0.099 Uiso 1 1 calc R U H3A H 0.9103 0.2115 0.3321 0.099 Uiso 1 1 calc R U C4 C 0.7105(5) 0.2873(3) 0.2961(4) 0.0643(11) Uani 1 1 d . . H4 H 0.6255 0.2743 0.3177 0.077 Uiso 1 1 calc R U C5 C 0.6872(5) 0.2748(3) 0.1829(4) 0.0726(12) Uani 1 1 d . . H5B H 0.5899 0.2909 0.1453 0.087 Uiso 1 1 calc R U H5A H 0.7068 0.2059 0.1671 0.087 Uiso 1 1 calc R U C6 C 0.7889(6) 0.3474(3) 0.1543(4) 0.0735(13) Uani 1 1 d . . H6B H 0.8709 0.3118 0.1461 0.088 Uiso 1 1 calc R U H6A H 0.7425 0.3823 0.0907 0.088 Uiso 1 1 calc R U C7 C 0.9247(3) 0.4950(2) 0.2516(3) 0.0420(6) Uani 1 1 d . . C8 C 0.9753(4) 0.5187(3) 0.1570(3) 0.0558(9) Uani 1 1 d . . C9 C 0.6899(3) 0.4767(2) 0.3558(3) 0.0423(6) Uani 1 1 d . . C10 C 0.5627(4) 0.5085(3) 0.2877(3) 0.0494(7) Uani 1 1 d . . C11 C 0.4759(4) 0.5789(3) 0.3162(3) 0.0537(8) Uani 1 1 d . . H11 H 0.3898 0.5973 0.2700 0.064 Uiso 1 1 calc R U C12 C 0.5184(4) 0.6214(2) 0.4136(3) 0.0484(7) Uani 1 1 d . . C13 C 0.6477(4) 0.5945(2) 0.4806(3) 0.0448(7) Uani 1 1 d . . C14 C 0.7311(3) 0.5224(2) 0.4525(3) 0.0434(7) Uani 1 1 d . . H14 H 0.8168 0.5039 0.4992 0.052 Uiso 1 1 calc R U C15 C 0.4001(5) 0.4918(5) 0.1207(4) 0.0811(14) Uani 1 1 d . . H15A H 0.3924 0.4574 0.0571 0.122 Uiso 1 1 calc R U H15B H 0.3971 0.5633 0.1094 0.122 Uiso 1 1 calc R U H15C H 0.3226 0.4723 0.1462 0.122 Uiso 1 1 calc R U C16 C 0.3049(5) 0.7142(4) 0.3887(4) 0.0779(14) Uani 1 1 d . . H16A H 0.2629 0.7613 0.4250 0.117 Uiso 1 1 calc R U H16B H 0.2483 0.6540 0.3743 0.117 Uiso 1 1 calc R U H16C H 0.3095 0.7439 0.3253 0.117 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0758(3) 0.0765(2) 0.0544(2) -0.02347(11) 0.02004(16) 0.00242(12) F1 0.0904(17) 0.0934(19) 0.0827(19) -0.0009(14) 0.0556(16) 0.0122(15) F2 0.0786(16) 0.132(2) 0.0637(17) 0.0437(17) 0.0163(14) 0.0115(17) F3 0.0974(19) 0.099(2) 0.094(2) 0.0082(16) 0.0469(18) -0.0400(16) O1 0.0544(13) 0.0520(13) 0.0555(15) -0.0088(11) 0.0148(12) -0.0085(11) O2 0.0595(15) 0.088(2) 0.0507(16) -0.0216(14) 0.0078(13) 0.0052(14) O3 0.0659(17) 0.0677(16) 0.0657(19) -0.0074(14) 0.0220(14) 0.0206(13) N1 0.0497(14) 0.0446(13) 0.0432(14) -0.0086(10) 0.0189(12) -0.0057(11) C1 0.0537(17) 0.0391(15) 0.0519(19) -0.0037(12) 0.0253(15) -0.0038(13) C2 0.077(3) 0.0490(19) 0.060(2) 0.0059(15) 0.033(2) 0.0124(16) C3 0.120(4) 0.043(2) 0.095(4) 0.005(2) 0.048(3) 0.013(2) C4 0.078(3) 0.0446(19) 0.083(3) -0.0116(18) 0.043(2) -0.0141(17) C5 0.080(3) 0.060(2) 0.082(3) -0.032(2) 0.029(2) -0.021(2) C6 0.104(4) 0.067(3) 0.058(3) -0.0300(19) 0.036(3) -0.025(2) C7 0.0432(15) 0.0410(14) 0.0438(16) -0.0009(12) 0.0159(13) 0.0019(12) C8 0.0557(19) 0.060(2) 0.055(2) 0.0128(16) 0.0207(17) 0.0026(16) C9 0.0476(15) 0.0394(14) 0.0443(17) -0.0028(11) 0.0203(14) -0.0062(12) C10 0.0524(17) 0.0540(18) 0.0431(18) -0.0064(14) 0.0157(15) -0.0076(15) C11 0.0483(18) 0.059(2) 0.054(2) -0.0006(16) 0.0148(16) 0.0044(15) C12 0.0535(18) 0.0410(16) 0.056(2) -0.0027(14) 0.0236(16) -0.0024(14) C13 0.0532(17) 0.0424(15) 0.0414(17) -0.0073(12) 0.0176(14) -0.0045(13) C14 0.0480(16) 0.0366(14) 0.0471(18) -0.0014(12) 0.0162(14) -0.0021(12) C15 0.063(2) 0.112(4) 0.057(3) -0.019(2) -0.002(2) -0.003(2) C16 0.078(3) 0.086(3) 0.078(3) 0.012(2) 0.036(3) 0.029(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 C10 O2 C15 119.6(3) C12 O3 C16 119.7(4) C7 N1 C1 119.4(3) C7 N1 C6 126.2(3) C1 N1 C6 113.8(3) N1 C1 C9 112.5(3) N1 C1 C2 111.2(3) C9 C1 C2 118.6(3) N1 C1 C4 101.8(3) C9 C1 C4 120.7(3) C2 C1 C4 89.1(3) C3 C2 C1 89.6(3) C2 C3 C4 90.2(3) C5 C4 C1 108.7(3) C5 C4 C3 116.7(4) C1 C4 C3 88.5(3) C4 C5 C6 106.0(3) N1 C6 C5 105.0(3) O1 C7 N1 125.2(3) O1 C7 C8 118.4(3) N1 C7 C8 116.4(3) F3 C8 F1 105.8(3) F3 C8 F2 107.5(3) F1 C8 F2 107.0(4) F3 C8 C7 110.6(3) F1 C8 C7 113.4(3) F2 C8 C7 112.1(3) C10 C9 C14 117.2(3) C10 C9 C1 121.7(3) C14 C9 C1 121.1(3) O2 C10 C9 116.1(3) O2 C10 C11 122.2(3) C9 C10 C11 121.6(3) C12 C11 C10 119.8(3) O3 C12 C13 116.8(3) O3 C12 C11 123.9(3) C13 C12 C11 119.3(3) C12 C13 C14 120.3(3) C12 C13 I1 119.0(2) C14 C13 I1 120.7(3) C13 C14 C9 121.7(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C13 2.083(3) F1 C8 1.323(5) F2 C8 1.325(5) F3 C8 1.316(5) O1 C7 1.208(4) O2 C10 1.362(4) O2 C15 1.391(5) O3 C12 1.364(4) O3 C16 1.381(5) N1 C7 1.340(4) N1 C1 1.481(4) N1 C6 1.482(4) C1 C9 1.511(4) C1 C2 1.553(6) C1 C4 1.554(5) C2 C3 1.524(6) C3 C4 1.555(7) C4 C5 1.498(7) C5 C6 1.518(6) C7 C8 1.540(5) C9 C10 1.391(5) C9 C14 1.395(5) C10 C11 1.394(5) C11 C12 1.387(5) C12 C13 1.381(5) C13 C14 1.384(4) 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 C7 N1 C1 C9 65.0(4) C6 N1 C1 C9 -123.4(4) C7 N1 C1 C2 -70.8(4) C6 N1 C1 C2 100.9(4) C7 N1 C1 C4 -164.4(3) C6 N1 C1 C4 7.2(4) N1 C1 C2 C3 -90.1(3) C9 C1 C2 C3 137.2(3) C4 C1 C2 C3 12.2(3) C1 C2 C3 C4 -12.2(3) N1 C1 C4 C5 -18.3(4) C9 C1 C4 C5 107.0(4) C2 C1 C4 C5 -129.8(4) N1 C1 C4 C3 99.5(3) C9 C1 C4 C3 -135.2(4) C2 C1 C4 C3 -12.0(3) C2 C3 C4 C5 122.4(4) C2 C3 C4 C1 12.2(3) C1 C4 C5 C6 22.7(5) C3 C4 C5 C6 -75.3(5) C7 N1 C6 C5 177.1(4) C1 N1 C6 C5 6.2(5) C4 C5 C6 N1 -17.5(5) C1 N1 C7 O1 -0.6(5) C6 N1 C7 O1 -171.1(4) C1 N1 C7 C8 -179.5(3) C6 N1 C7 C8 9.9(5) O1 C7 C8 F3 1.4(5) N1 C7 C8 F3 -179.6(3) O1 C7 C8 F1 120.1(4) N1 C7 C8 F1 -60.9(4) O1 C7 C8 F2 -118.6(4) N1 C7 C8 F2 60.4(4) N1 C1 C9 C10 64.2(4) C2 C1 C9 C10 -163.6(3) C4 C1 C9 C10 -56.0(5) N1 C1 C9 C14 -118.8(3) C2 C1 C9 C14 13.3(4) C4 C1 C9 C14 121.0(4) C15 O2 C10 C9 178.2(4) C15 O2 C10 C11 -1.2(6) C14 C9 C10 O2 177.3(3) C1 C9 C10 O2 -5.6(5) C14 C9 C10 C11 -3.4(5) C1 C9 C10 C11 173.7(3) O2 C10 C11 C12 -178.5(3) C9 C10 C11 C12 2.2(5) C16 O3 C12 C13 -174.7(4) C16 O3 C12 C11 5.9(6) C10 C11 C12 O3 -179.5(3) C10 C11 C12 C13 1.0(5) O3 C12 C13 C14 177.6(3) C11 C12 C13 C14 -2.9(5) O3 C12 C13 I1 -2.2(4) C11 C12 C13 I1 177.3(3) C12 C13 C14 C9 1.6(5) I1 C13 C14 C9 -178.6(2) C10 C9 C14 C13 1.5(4) C1 C9 C14 C13 -175.6(3)