#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:56:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294486 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572125.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_1572125 loop_ _publ_author_name 'Seki, Tomohiro' 'Kobayashi, Shiori' 'Ishikawa, Rintaro' 'Yano, Keigo' 'Matsuo, Takumi' 'Hayashi, Shotaro' _publ_section_title ; Preparation of intrinsically fragile bent crystals. ; _journal_issue 31 _journal_name_full 'Chemical science' _journal_page_first 12258 _journal_page_last 12263 _journal_paper_doi 10.1039/d4sc02918f _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C15 H12 F3 N O2' _chemical_formula_sum 'C15 H12 F3 N O2' _chemical_formula_weight 295.26 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-11-20 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-04-24 deposited with the CCDC. 2024-07-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.674(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.9586(2) _cell_length_b 11.2709(4) _cell_length_c 24.1190(8) _cell_measurement_reflns_used 4251 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 76.0810 _cell_measurement_theta_min 3.6870 _cell_volume 1341.36(8) _computing_cell_refinement 'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -66.00 -6.00 0.50 1.07 -- -47.48 103.00 -73.00 120 2 \w 16.00 67.00 0.50 1.07 -- 47.48-103.00-174.00 102 3 \w -176.00-114.00 0.50 4.30 -- -106.00-103.00-174.00 124 4 \w -98.00 -72.00 0.50 4.30 -- -106.00 103.00 -73.00 52 5 \w 51.00 107.00 0.50 4.30 -- 108.21-103.00-174.00 112 6 \w 90.00 155.00 0.50 4.30 -- 108.21 103.00 -73.00 130 7 \w -113.00 -74.00 0.50 1.07 -- -47.48-125.00 60.00 78 8 \w -104.00 -73.00 0.50 1.07 -- -47.48-125.00-120.00 62 9 \w -117.00 -78.00 0.50 1.07 -- -47.48-125.00 -90.00 78 10 \w 82.00 116.00 0.50 1.07 -- 47.48 125.00-150.00 68 11 \w 82.00 107.00 0.50 1.07 -- 47.48 125.00 120.00 50 12 \w -60.00 -34.00 0.50 4.30 -- -106.00 57.00 150.00 52 13 \w -164.00-138.00 0.50 4.30 -- -106.00 -99.00 120.00 52 14 \w -67.00 -42.00 0.50 4.30 -- -106.00 57.00 60.00 50 15 \w -67.00 -42.00 0.50 4.30 -- -106.00 57.00 30.00 50 16 \w -61.00 -35.00 0.50 4.30 -- -106.00 57.00-120.00 52 17 \w -67.00 -41.00 0.50 4.30 -- -106.00 57.00 120.00 52 18 \w -125.00 -97.00 0.50 4.30 -- -106.00 -38.00 90.00 56 19 \w -133.00 -91.00 0.50 4.30 -- -106.00 -99.00 120.00 84 20 \w -168.00-142.00 0.50 4.30 -- -106.00 -38.00 90.00 52 21 \w -63.00 -38.00 0.50 4.30 -- -106.00 57.00 90.00 50 22 \w 35.00 60.00 0.50 4.30 -- 108.21 -57.00-180.00 50 23 \w 56.00 81.00 0.50 4.30 -- 108.21 -77.00-150.00 50 24 \w 72.00 98.00 0.50 4.30 -- 108.21 -77.00-180.00 52 25 \w 37.00 62.00 0.50 4.30 -- 108.21 -77.00-180.00 50 26 \w 37.00 64.00 0.50 4.30 -- 108.21 -57.00-120.00 54 27 \w 35.00 60.00 0.50 4.30 -- 108.21 -57.00 -30.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.2388669000 _diffrn_orient_matrix_UB_12 0.0725405000 _diffrn_orient_matrix_UB_13 0.0183552000 _diffrn_orient_matrix_UB_21 0.1860072000 _diffrn_orient_matrix_UB_22 0.1091910000 _diffrn_orient_matrix_UB_23 0.0094477000 _diffrn_orient_matrix_UB_31 -0.0760454000 _diffrn_orient_matrix_UB_32 0.0388272000 _diffrn_orient_matrix_UB_33 -0.0607787000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_unetI/netI 0.0419 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 8206 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.294 _diffrn_reflns_theta_min 3.683 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.29927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.462 _exptl_crystal_description needle _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.343 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 2708 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0482 _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^)+(0.0715P)^2^+0.4718P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1306 _refine_ls_wR_factor_ref 0.1359 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2343 _reflns_number_total 2708 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02918f3.cif _cod_data_source_block ffa4ch3-8_auto _cod_depositor_comments 'Adding full bibliography for 1572123--1572125.cif.' _cod_database_code 1572125 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHONF _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: N006(H006), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00L(H00L) 2.b Idealised Me refined as rotating group: C00K(H00A,H00B,H00C) 2.c Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL ffa4ch3-8_auto_a.res in P2(1)/n ffa4ch3-8_auto.res created by SHELXL-2018/3 at 18:28:55 on 20-Nov-2023 REM Old TITL FFA4CH3-8_auto in P21/n #14 REM SHELXT solution in P2(1)/n: R1 0.175, Rweak 0.017, Alpha 0.025 REM 0.589 for 151 systematic absences, Orientation as input REM Formula found by SHELXT: C15 F5 N CELL 1.54184 4.9586 11.2709 24.119 90 95.674 90 ZERR 4 0.0002 0.0004 0.0008 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O UNIT 60 48 12 4 8 L.S. 10 PLAN 5 TEMP -100 CONF BOND list 4 fmap 2 MORE -1 ACTA BOND $H REM REM REM WGHT 0.071500 0.471800 FVAR 0.65400 O2 5 -0.272733 0.513457 0.455078 11.00000 0.03368 0.03366 = 0.03142 0.00296 0.01687 0.00509 O1 5 -0.380120 0.348060 0.498745 11.00000 0.03723 0.03686 = 0.03176 0.00330 0.01863 0.00432 AFIX 147 H1 2 -0.492183 0.394166 0.511405 11.00000 -1.50000 AFIX 0 F003 3 0.548602 0.940775 0.322199 11.00000 0.08231 0.03339 = 0.05583 0.00536 0.00707 0.00983 F004 3 0.562334 0.873274 0.404497 11.00000 0.11224 0.05385 = 0.03972 -0.01074 0.01530 -0.01369 F005 3 0.904446 0.854417 0.357161 11.00000 0.04155 0.05515 = 0.13413 -0.02447 -0.00514 -0.00054 N006 4 0.084908 0.497239 0.379329 11.00000 0.03802 0.03648 = 0.03674 0.00512 0.02308 0.00838 AFIX 43 H006 2 -0.044649 0.538284 0.392845 11.00000 -1.20000 AFIX 0 C007 1 -0.057085 0.331580 0.434138 11.00000 0.02680 0.03288 = 0.02676 -0.00223 0.00724 0.00142 C008 1 0.103607 0.379598 0.394009 11.00000 0.02786 0.03591 = 0.02349 -0.00271 0.00660 0.00241 C009 1 -0.243921 0.405747 0.462838 11.00000 0.02578 0.03663 = 0.02217 0.00089 0.00748 -0.00012 C00A 1 0.250750 0.559537 0.344933 11.00000 0.02958 0.03765 = 0.02681 0.00467 0.01255 0.00706 C00B 1 0.525482 0.732375 0.331333 11.00000 0.03126 0.03332 = 0.03049 0.00457 0.00635 0.00766 C00C 1 0.585632 0.691368 0.279017 11.00000 0.02887 0.03795 = 0.03181 0.00725 0.01236 0.00783 C00D 1 0.285996 0.301743 0.370817 11.00000 0.03342 0.04106 = 0.03062 -0.00377 0.01291 0.00377 AFIX 43 H00D 2 0.400441 0.331545 0.344695 11.00000 -1.20000 AFIX 0 C00E 1 0.360389 0.666952 0.363400 11.00000 0.03702 0.03682 = 0.02396 0.00265 0.00981 0.01086 AFIX 43 H00E 2 0.322305 0.696670 0.398651 11.00000 -1.20000 AFIX 0 C00F 1 0.299910 0.520075 0.291950 11.00000 0.03492 0.03991 = 0.02794 -0.00037 0.01067 0.00015 AFIX 43 H00F 2 0.218856 0.448734 0.277456 11.00000 -1.20000 AFIX 0 C00G 1 0.467257 0.585170 0.260502 11.00000 0.03918 0.04164 = 0.02567 0.00041 0.01471 0.00582 AFIX 43 H00G 2 0.502044 0.555904 0.224964 11.00000 -1.20000 AFIX 0 C00H 1 -0.036678 0.210514 0.447654 11.00000 0.03920 0.03518 = 0.04178 0.00152 0.01619 -0.00027 AFIX 43 H00H 2 -0.146230 0.179041 0.474286 11.00000 -1.20000 AFIX 0 C00I 1 0.300887 0.184048 0.385300 11.00000 0.03980 0.03927 = 0.04026 -0.00974 0.01286 0.00827 AFIX 43 H00I 2 0.425497 0.134086 0.368953 11.00000 -1.20000 AFIX 0 C00J 1 0.635065 0.847920 0.354051 11.00000 0.04331 0.03779 = 0.04003 0.00105 0.00549 0.00577 C00K 1 0.772512 0.755387 0.242866 11.00000 0.03803 0.04614 = 0.04486 0.00911 0.02037 0.00465 AFIX 137 H00A 2 0.720621 0.839191 0.239664 11.00000 -1.50000 H00B 2 0.757834 0.719251 0.205733 11.00000 -1.50000 H00C 2 0.959859 0.749095 0.259838 11.00000 -1.50000 AFIX 0 C00L 1 0.137976 0.136215 0.423317 11.00000 0.04951 0.03203 = 0.05396 -0.00200 0.01673 0.00494 AFIX 43 H00L 2 0.146867 0.054157 0.432312 11.00000 -1.20000 AFIX 0 HKLF 4 REM ffa4ch3-8_auto_a.res in P2(1)/n REM wR2 = 0.1359, GooF = S = 1.067, Restrained GooF = 1.067 for all data REM R1 = 0.0482 for 2343 Fo > 4sig(Fo) and 0.0547 for all 2708 data REM 192 parameters refined using 0 restraints END WGHT 0.0715 0.4719 REM Highest difference peak 0.343, deepest hole -0.310, 1-sigma level 0.058 Q1 1 0.7364 0.8393 0.4019 11.00000 0.05 0.34 Q2 1 0.8602 0.8087 0.3871 11.00000 0.05 0.28 Q3 1 0.0304 0.5490 0.4085 11.00000 0.05 0.27 Q4 1 0.9536 0.7032 0.2415 11.00000 0.05 0.25 Q5 1 0.4521 0.6970 0.3480 11.00000 0.05 0.20 ; _shelx_res_checksum 35127 _shelx_hkl_file ; 0 0 -2 14.20 0.82 0 0 -2 15.17 0.81 0 0 -3 0.09 0.28 0 0 -3 0.19 0.36 0 0 -4 2356.15 111.45 0 0 -4 2327.97 111.46 0 0 -5 9.12 0.94 0 0 -5 12.08 0.89 0 0 -6 47.13 2.71 0 0 -6 54.26 2.81 0 0 -7 0.71 0.86 0 0 -7 0.04 0.55 0 0 -8 1286.67 59.88 0 0 -8 1218.94 59.77 0 0 -9 0.46 0.77 0 0 -9 1.71 1.00 0 0 -10 610.48 29.62 0 0 -11 -0.08 0.80 0 0 -12 11.08 1.37 0 0 -13 0.11 0.90 0 0 -14 4.13 1.10 0 0 -15 0.42 1.02 0 0 -16 14.66 1.09 0 0 -16 17.42 1.30 0 0 -16 14.45 1.86 0 0 -16 13.09 1.07 0 0 -17 -0.25 0.85 0 0 -17 0.28 0.56 0 0 -17 -0.17 0.57 0 0 -17 0.40 0.66 0 0 -17 -0.09 0.94 0 0 -17 0.92 1.19 0 0 -18 168.20 8.53 0 0 -18 155.41 8.47 0 0 -18 163.36 9.70 0 0 -18 174.78 8.92 0 0 -18 170.31 8.72 0 0 -19 -0.34 0.71 0 0 -19 -0.08 0.90 0 0 -19 0.20 1.05 0 0 -19 -0.10 1.06 0 0 -19 0.37 0.74 0 0 -20 78.42 4.40 0 0 -20 81.28 4.43 0 0 -20 84.90 4.75 0 0 -20 81.07 4.77 0 0 -20 78.27 4.60 0 0 -21 0.70 1.03 0 0 -21 -0.44 1.18 0 0 -21 1.06 0.89 0 0 -21 -0.35 0.89 0 0 -21 -0.24 1.21 0 0 -22 65.17 3.82 0 0 -22 63.15 3.75 0 0 -22 64.07 4.09 0 0 -23 0.25 1.12 0 0 -23 0.46 1.07 0 0 -23 -0.46 1.16 0 0 -24 62.95 4.05 0 0 -24 69.89 3.99 0 0 -25 -0.16 1.10 0 0 -25 -0.76 1.10 0 0 -25 1.49 1.18 0 0 -26 0.88 1.13 0 0 -26 -0.17 1.06 0 0 -27 0.19 0.94 0 0 -27 1.13 0.95 0 0 -28 52.97 3.07 0 0 -29 -0.48 0.68 0 0 -30 10.13 0.82 0 1 0 0.16 0.24 0 1 -1 1587.88 72.82 0 -1 -1 1467.11 72.81 0 1 -1 1567.79 72.81 0 -1 -1 1515.69 72.82 0 -1 -2 196.00 9.64 0 1 -2 201.03 9.64 0 1 -2 209.06 9.64 0 -1 -2 196.76 9.63 0 -1 -3 524.51 24.93 0 -1 -3 504.77 25.12 0 1 -3 534.58 24.94 0 1 -3 530.19 24.92 0 -1 -3 506.10 24.91 0 -1 -4 5153.11 249.85 0 -1 -4 5430.37 249.89 0 1 -4 5302.71 249.89 0 1 -4 5170.25 249.86 0 -1 -4 5262.43 250.08 0 -1 -5 565.78 26.74 0 -1 -5 538.87 26.45 0 1 -5 541.73 26.46 0 -1 -5 570.48 26.50 0 -1 -6 405.67 20.09 0 -1 -6 397.24 19.75 0 1 -6 403.74 19.77 0 -1 -6 434.31 19.84 0 -1 -7 2.13 0.85 0 -1 -7 2.23 1.16 0 -1 -7 2.25 0.65 0 -1 -8 234.28 11.26 0 -1 -8 215.93 11.12 0 -1 -9 604.82 28.58 0 -1 -9 573.65 28.46 0 -1 -10 51.63 3.10 0 -1 -11 1448.51 69.50 0 -1 -12 24.30 1.95 0 -1 -13 75.87 4.50 0 -1 -14 627.74 30.85 0 -1 -15 7.99 1.45 0 -1 -16 26.78 1.65 0 -1 -16 29.22 2.49 0 -1 -16 29.07 2.11 0 1 -16 29.02 1.68 0 1 -16 24.52 1.63 0 -1 -16 30.04 1.84 0 -1 -16 23.55 1.61 0 -1 -17 31.16 2.10 0 -1 -17 33.14 2.88 0 -1 -17 31.93 2.36 0 -1 -17 33.47 1.94 0 1 -17 33.65 2.40 0 -1 -17 29.20 1.88 0 1 -17 26.41 1.87 0 -1 -17 36.02 2.36 0 1 -17 33.04 2.10 0 1 -17 30.71 1.94 0 -1 -17 31.90 2.45 0 -1 -18 176.32 8.39 0 1 -18 167.96 7.95 0 1 -18 162.08 8.09 0 1 -18 175.31 8.35 0 -1 -18 144.99 7.85 0 -1 -18 164.57 8.13 0 -1 -18 146.02 8.24 0 -1 -18 153.74 8.31 0 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0.12 1.13 -2 -5 -15 77.31 4.78 -2 -5 -15 75.78 4.79 -2 5 -15 82.76 4.73 -2 5 -15 81.15 4.83 -2 5 -15 77.01 4.52 -2 5 -15 78.11 4.10 -2 -5 -15 83.49 4.14 -2 -5 -16 90.95 5.69 -2 -5 -16 99.40 5.80 -2 5 -16 106.09 5.66 -2 5 -16 108.09 5.82 -2 5 -16 93.87 5.06 -2 -5 -16 100.70 5.11 -2 5 -16 99.63 5.48 -2 -5 -17 16.52 1.84 -2 -5 -17 18.46 2.02 -2 5 -17 17.47 1.25 -2 5 -17 17.53 1.69 -2 -5 -17 18.28 2.11 -2 -5 -17 17.58 1.30 -2 -5 -18 59.50 3.80 -2 -5 -18 52.82 3.81 -2 -5 -18 57.45 3.19 -2 5 -18 59.49 3.16 -2 -5 -18 64.31 3.89 -2 -5 -19 5.17 1.36 -2 -5 -19 6.40 1.53 -2 5 -19 6.19 0.78 -2 -5 -19 7.30 0.87 -2 -5 -19 3.83 1.74 -2 -5 -19 6.41 1.47 -2 -5 -20 1.08 1.46 -2 -5 -20 0.38 1.16 -2 -5 -20 0.11 1.30 -2 -5 -20 0.67 0.64 -2 -5 -20 0.46 1.19 -2 -5 -21 61.45 3.75 -2 -5 -21 64.31 3.94 -2 -5 -21 59.74 3.27 -2 -5 -21 61.92 3.73 -2 -5 -21 60.68 3.92 -2 -5 -22 22.33 2.09 -2 -5 -22 23.43 2.02 -2 -5 -22 23.90 1.93 2 -6 -26 2.13 0.73 2 -6 -25 1.49 0.91 2 -6 -24 2.55 0.80 2 -6 -24 3.28 1.07 2 -6 -24 3.53 1.38 2 -6 -23 36.30 2.35 2 -6 -23 39.96 2.92 2 -6 -22 13.12 1.32 2 -6 -22 13.78 1.97 2 -6 -21 13.82 1.34 2 -6 -21 15.97 2.09 2 6 -21 12.96 1.11 2 -6 -20 0.68 0.80 2 6 -20 0.62 0.62 2 -6 -20 0.13 1.48 2 6 -20 0.42 0.61 2 -6 -19 49.16 2.92 2 -6 -19 50.25 3.55 2 6 -19 46.45 2.77 2 -6 -18 2.72 1.60 2 6 -18 3.68 0.76 2 -6 -18 3.45 0.89 2 -6 -17 2.32 0.81 2 -6 -17 3.82 2.14 2 -6 -17 3.05 1.45 2 6 -17 2.78 0.74 2 -6 -16 2.31 1.96 2 -6 -16 2.35 1.36 2 6 -16 2.59 0.72 2 -6 -15 7.67 2.31 2 6 -15 8.65 1.00 2 -6 -14 14.81 2.96 2 -6 -13 2.62 2.05 2 -6 -12 3.77 2.16 2 6 -12 2.82 0.74 2 -6 -11 3.03 2.23 2 6 -11 3.57 0.76 2 -6 -10 52.28 5.36 2 6 -10 61.40 3.34 2 -6 -9 177.42 11.02 2 6 -9 167.49 8.58 2 6 -9 196.83 11.09 2 -6 -8 80.50 6.73 2 6 -8 103.20 6.99 2 6 -7 105.13 7.45 2 6 -6 55.42 4.90 2 6 -5 2.06 1.88 -2 6 5 1.35 1.69 -2 6 5 0.79 1.85 2 6 -5 0.74 0.47 -2 6 5 0.20 1.46 2 6 -4 21.73 3.02 -2 6 4 19.09 2.87 -2 6 4 22.11 2.85 2 6 -4 23.45 1.45 -2 6 4 23.01 2.60 2 6 -3 128.76 7.92 -2 6 3 111.99 7.58 -2 6 3 112.59 7.48 -2 6 3 112.02 7.01 2 6 -3 115.92 5.82 2 6 -2 129.67 8.18 -2 6 2 125.93 8.03 -2 6 2 118.31 7.82 -2 6 2 123.75 7.47 -2 6 1 14.48 2.53 -2 6 1 9.65 1.55 -2 6 1 13.45 2.05 -2 6 0 35.47 3.73 -2 6 0 41.45 3.72 -2 6 0 40.18 3.35 -2 6 0 36.95 2.90 -2 6 -1 4.33 1.85 -2 6 -1 3.40 1.36 -2 6 -1 3.60 1.79 -2 6 -1 2.16 1.39 -2 6 -2 2.95 1.91 -2 6 -2 3.51 1.35 -2 6 -2 7.04 1.97 -2 -6 -2 5.12 1.00 -2 6 -2 4.31 1.49 -2 6 -3 3.04 2.05 -2 6 -3 0.53 1.29 -2 6 -3 0.53 1.77 -2 -6 -3 0.76 0.84 -2 6 -4 32.90 3.77 -2 6 -4 28.80 2.70 -2 -6 -4 36.96 2.60 -2 -6 -4 36.60 2.37 -2 -6 -5 11.79 1.57 -2 6 -5 15.39 2.60 -2 6 -5 11.84 1.87 -2 -6 -5 13.08 1.40 -2 6 -6 -0.29 1.39 -2 -6 -6 -0.91 1.20 -2 -6 -6 -0.17 0.92 -2 -6 -7 154.78 8.24 -2 -6 -7 146.67 7.88 -2 -6 -8 -0.14 1.35 -2 -6 -8 1.06 1.01 -2 6 -8 0.09 1.03 -2 6 -9 167.31 10.09 -2 -6 -9 191.43 10.12 -2 -6 -9 170.42 9.59 -2 6 -9 178.41 9.54 -2 -6 -10 0.75 1.09 -2 -6 -10 1.32 1.03 -2 6 -10 -0.50 1.56 -2 -6 -10 1.45 1.74 -2 6 -10 1.38 1.36 -2 6 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3.59 1.04 -2 -6 -22 4.67 1.03 2 -7 -24 0.64 0.96 2 -7 -23 1.87 1.01 2 -7 -23 2.24 1.18 2 -7 -22 42.16 2.66 2 -7 -22 51.20 3.03 2 -7 -22 48.42 3.19 2 -7 -21 7.77 1.00 2 -7 -21 5.75 1.24 2 -7 -21 7.61 1.57 2 -7 -20 -0.06 0.73 2 -7 -20 0.45 1.09 2 -7 -20 1.25 1.46 2 -7 -19 19.83 1.49 2 7 -19 16.29 1.46 2 -7 -19 18.62 2.07 2 7 -19 18.51 1.38 2 -7 -18 91.25 4.67 2 -7 -18 84.65 5.17 2 7 -18 82.06 4.57 2 -7 -17 10.07 1.09 2 -7 -17 7.37 1.64 2 7 -17 8.72 1.04 2 -7 -16 9.09 1.06 2 -7 -16 9.41 1.72 2 7 -16 10.12 1.08 2 -7 -15 185.31 9.34 2 -7 -15 185.97 11.79 2 -7 -14 61.09 5.54 2 -7 -13 22.47 3.46 2 7 -13 25.70 1.79 2 -7 -12 35.59 4.23 2 7 -12 33.46 2.15 2 -7 -11 24.50 3.61 2 7 -11 23.68 1.67 2 -7 -10 4.72 2.42 2 7 -10 3.45 0.74 2 -7 -9 192.01 11.68 -2 7 9 162.31 10.29 2 7 -9 179.89 9.06 2 -7 -8 62.86 5.73 2 7 -8 69.68 5.78 2 7 -8 62.69 3.37 -2 7 8 50.95 4.47 2 7 -7 36.17 4.15 -2 7 7 30.76 3.75 -2 7 7 33.79 3.71 2 -7 -7 40.80 4.52 -2 7 7 34.15 3.29 2 7 -7 35.24 2.11 -2 7 6 368.28 19.98 -2 7 6 374.50 19.89 2 7 -6 361.30 17.85 -2 7 6 350.75 19.13 -2 7 5 40.82 4.20 -2 7 5 46.78 4.22 2 7 -5 45.72 4.60 2 7 -5 44.06 2.45 -2 7 5 37.39 3.55 2 7 -4 45.25 4.39 -2 7 4 38.03 4.07 -2 7 4 48.23 4.18 2 7 -4 44.64 2.39 -2 7 4 36.84 3.42 -2 7 4 38.90 2.52 2 7 -3 5.92 1.97 -2 7 3 4.10 2.09 -2 7 3 4.69 1.30 -2 7 3 5.63 1.91 2 7 -3 5.05 0.69 -2 7 3 6.84 1.68 -2 7 3 5.37 1.02 2 7 -2 86.31 6.34 -2 7 2 75.40 6.07 -2 7 2 64.36 4.72 -2 7 2 86.47 6.06 -2 7 2 84.78 4.53 2 7 -2 82.68 4.18 -2 7 2 81.00 5.38 2 7 -1 7.37 2.30 -2 7 1 5.53 2.36 -2 7 1 3.00 1.39 -2 7 1 5.35 1.97 -2 7 1 7.53 1.22 -2 7 1 6.09 1.63 -2 7 0 53.44 4.93 -2 7 0 43.51 3.51 -2 7 0 57.11 4.64 -2 -7 0 54.47 3.29 -2 7 0 55.48 3.38 -2 7 0 52.17 4.00 -2 7 -1 31.14 3.77 -2 7 -1 24.08 2.45 -2 7 -1 30.05 3.38 -2 7 -1 33.49 2.40 -2 7 -2 10.42 2.65 -2 7 -2 10.71 1.82 -2 7 -2 13.09 2.56 -2 7 -2 11.85 1.59 -2 7 -3 6.39 2.44 -2 7 -3 6.40 1.65 -2 -7 -3 8.19 1.34 -2 7 -3 8.59 1.45 -2 7 -4 27.72 3.49 -2 7 -4 21.49 2.51 -2 -7 -4 26.25 2.14 -2 7 -4 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2 -8 -19 -0.40 0.65 2 -8 -19 1.26 1.07 2 8 -19 0.12 0.69 2 -8 -19 0.29 1.21 2 -8 -18 2.68 0.72 2 -8 -18 4.25 1.18 2 8 -18 2.19 0.82 2 -8 -18 1.33 1.32 2 -8 -17 14.58 1.19 2 8 -17 14.89 1.37 2 -8 -17 12.82 1.75 2 8 -17 11.67 1.19 2 -8 -16 2.05 0.71 2 -8 -16 0.21 1.25 2 -8 -15 0.65 1.19 2 8 -14 22.14 1.65 -2 8 13 1.00 1.75 2 -8 -13 0.36 1.88 2 8 -13 0.13 0.71 -2 8 12 6.76 2.09 2 -8 -12 10.43 2.61 2 8 -12 8.85 1.05 -2 8 11 0.34 1.82 2 -8 -11 -0.77 1.87 2 8 -11 1.07 0.77 -2 8 10 6.95 2.22 -2 8 10 7.05 2.33 2 -8 -10 8.45 2.54 2 8 -10 7.09 0.96 -2 8 9 190.01 12.27 -2 8 9 217.13 12.44 2 -8 -9 232.09 13.20 2 8 -9 202.02 10.24 -2 8 8 236.10 14.84 -2 8 8 237.64 14.74 2 -8 -8 274.48 15.65 2 8 -8 259.51 12.84 -2 8 7 280.99 16.71 -2 8 7 290.58 16.57 2 -8 -7 286.36 17.17 2 8 -7 294.43 14.56 -2 8 6 227.76 13.70 -2 8 6 225.32 13.41 2 -8 -6 234.70 14.26 2 8 -6 271.21 14.72 2 8 -6 228.46 11.45 -2 8 5 280.18 15.89 -2 8 5 269.49 15.47 -2 -8 5 272.77 13.76 2 8 -5 269.88 13.50 -2 8 4 1034.28 55.74 -2 8 4 1110.62 55.50 -2 -8 4 1121.67 53.73 2 8 -4 1106.81 53.44 2 8 -3 30.70 3.91 -2 8 3 23.97 3.60 -2 8 3 23.35 2.42 -2 -8 3 29.28 2.18 -2 8 3 36.51 3.47 2 8 -3 28.67 1.81 -2 8 3 30.05 2.91 -2 8 3 26.31 1.98 -2 8 2 114.85 8.08 -2 8 2 100.08 6.45 -2 8 2 127.79 7.84 -2 -8 2 118.74 6.17 2 8 -2 121.62 8.21 -2 8 2 104.01 6.01 2 8 -2 115.44 5.79 2 8 -1 276.66 15.95 -2 8 1 283.68 16.15 -2 8 1 248.11 14.27 -2 8 1 294.60 15.66 -2 -8 1 289.95 14.01 -2 8 1 275.83 13.90 2 8 0 1.07 1.74 -2 8 0 -0.77 1.95 -2 8 0 3.75 1.57 -2 -8 0 2.90 1.27 -2 8 0 0.89 1.18 2 8 1 136.94 8.89 -2 8 -1 152.04 9.43 -2 -8 -1 133.64 7.11 -2 8 -1 136.95 7.15 -2 8 -2 273.92 15.61 -2 8 -2 233.48 13.74 -2 8 -2 281.03 13.50 -2 8 -3 63.86 5.95 -2 8 -3 54.97 4.43 -2 -8 -3 65.67 4.22 -2 8 -4 15.49 3.14 -2 8 -4 15.68 2.41 -2 -8 -4 17.26 2.07 -2 8 -4 21.02 2.10 -2 8 -5 0.36 1.66 -2 -8 -5 0.54 1.34 -2 -8 -5 0.89 1.34 -2 8 -5 0.24 1.45 -2 8 -6 46.40 3.86 -2 -8 -6 46.49 3.58 -2 -8 -6 47.55 3.48 -2 8 -6 55.05 3.54 -2 8 -7 -0.73 1.62 -2 -8 -7 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18.95 1.18 5 3 -15 20.70 1.20 5 -3 -14 27.86 1.63 5 3 -14 30.81 1.67 5 -3 -13 39.35 2.16 5 3 -13 40.63 2.17 5 -3 -12 85.14 4.40 5 3 -12 89.35 4.42 5 -3 -11 7.07 0.71 5 3 -11 7.01 0.74 5 -3 -10 26.09 1.58 5 3 -10 26.42 1.60 5 -3 -9 59.57 3.17 5 3 -9 60.22 3.18 5 -3 -8 22.24 1.45 5 3 -8 23.22 1.48 5 -3 -7 24.59 1.60 5 3 -7 26.73 1.63 5 -3 -6 4.12 0.73 5 3 -6 3.71 0.74 5 -3 -5 2.27 0.68 5 3 -5 1.84 0.70 5 3 -4 9.41 0.97 5 -3 -4 7.55 0.89 5 -3 -3 1.82 0.67 5 3 -3 2.15 0.74 -5 -3 3 1.16 0.78 -5 3 2 17.66 1.41 -5 -3 2 19.83 1.41 5 -3 -2 17.08 1.31 5 3 -2 17.97 1.35 -5 3 1 2.53 1.06 5 -3 -1 1.10 0.69 5 3 -1 1.67 0.73 -5 3 1 3.58 0.85 -5 -3 1 2.04 0.77 -5 3 0 85.81 4.15 -5 -3 0 82.13 4.11 -5 3 0 77.64 4.46 5 -3 0 69.56 4.08 5 3 0 76.82 4.15 -5 3 -1 33.82 1.90 -5 -3 -1 32.26 1.85 -5 3 -1 29.07 2.25 5 -3 1 26.84 1.85 5 3 1 28.20 1.89 -5 3 -2 18.94 1.30 -5 -3 -2 17.47 1.24 -5 3 -3 39.91 2.13 -5 -3 -3 34.61 2.06 -5 3 -3 33.01 2.51 -5 3 -4 44.03 2.37 -5 -3 -4 43.86 2.33 -5 3 -5 5.16 1.18 -5 3 -5 6.79 0.77 -5 -3 -5 6.49 0.73 -5 3 -6 21.71 1.36 -5 -3 -6 21.02 1.33 -5 3 -7 1.03 0.55 -5 -3 -7 0.97 0.50 -5 3 -8 2.06 0.55 -5 -3 -8 1.74 0.51 -5 3 -9 3.51 0.56 -5 -3 -9 3.79 0.54 -5 3 -10 1.58 0.72 -5 3 -10 2.61 0.50 -5 -3 -10 1.13 0.44 -5 3 -11 3.33 0.50 -5 -3 -11 3.64 0.47 -5 3 -12 0.31 0.36 -5 -3 -12 0.11 0.33 -5 3 -13 0.22 0.32 -5 -3 -13 0.38 0.29 5 4 -18 0.59 0.26 5 4 -17 34.02 1.83 5 -4 -16 18.14 1.03 5 4 -16 22.82 1.22 5 -4 -15 52.62 2.63 5 4 -15 51.83 2.78 5 -4 -14 4.24 0.45 5 4 -14 3.68 0.56 5 -4 -13 15.95 0.98 5 -4 -12 44.62 2.33 5 -4 -11 2.81 0.48 5 4 -11 3.91 0.53 5 -4 -10 78.98 4.07 5 4 -10 83.16 4.09 5 -4 -9 6.95 0.66 5 4 -9 6.60 0.68 5 -4 -8 24.86 1.50 5 4 -8 26.51 1.54 5 -4 -7 1.65 0.51 5 4 -7 1.60 0.53 5 -4 -6 2.28 0.55 5 4 -6 2.09 0.56 5 -4 -5 15.92 1.05 5 4 -5 14.83 1.07 5 -4 -4 0.13 0.50 5 4 -4 0.32 0.54 -5 4 4 -0.04 0.67 -5 -4 4 -0.56 0.63 -5 4 3 43.58 2.52 -5 -4 3 45.62 2.51 5 -4 -3 44.78 2.49 5 4 -3 49.58 2.55 -5 4 2 26.91 1.67 -5 -4 2 27.61 1.65 5 -4 -2 25.26 1.62 5 4 -2 29.25 1.70 -5 4 2 26.87 1.97 -5 4 1 0.30 0.90 5 -4 -1 0.24 0.54 5 4 -1 0.49 0.61 -5 4 1 1.01 0.61 -5 -4 1 0.75 0.56 -5 4 0 109.22 5.25 -5 -4 0 106.13 5.21 5 -4 0 96.60 5.24 5 4 0 106.43 5.30 -5 4 0 99.29 5.60 -5 4 -1 11.96 0.94 -5 -4 -1 11.34 0.88 5 -4 1 10.00 0.93 5 4 1 10.42 0.97 -5 4 -1 10.42 1.35 -5 4 -2 0.95 0.99 5 -4 2 -0.45 0.57 5 4 2 0.56 0.58 -5 4 -2 -0.35 0.53 -5 -4 -2 -0.32 0.49 -5 4 -3 11.35 0.89 -5 -4 -3 12.41 0.86 5 -4 3 9.42 0.90 5 4 3 11.66 0.96 -5 4 -3 8.93 1.32 -5 4 -4 3.59 1.10 5 -4 4 3.74 0.65 5 4 4 3.44 0.67 -5 4 -4 5.03 0.62 -5 -4 -4 5.08 0.59 -5 4 -5 28.92 1.53 -5 -4 -5 26.25 1.48 -5 4 -5 23.25 1.95 5 -4 5 23.64 1.54 5 4 5 25.93 1.59 -5 4 -6 47.79 2.42 -5 -4 -6 45.38 2.38 -5 4 -6 41.30 2.84 -5 4 -7 5.00 1.06 -5 4 -7 4.54 0.54 -5 -4 -7 3.42 0.49 -5 4 -8 3.35 0.86 -5 -4 -8 3.89 0.48 -5 -4 -9 2.90 0.41 -5 4 -9 4.31 0.82 -5 -4 -10 0.81 0.32 -5 4 -10 1.11 0.60 5 5 -17 8.75 0.59 5 5 -16 7.43 0.59 5 5 -15 0.66 0.35 5 5 -14 16.31 1.05 5 5 -13 17.61 1.12 5 5 -12 0.68 0.43 5 5 -11 28.38 1.65 5 5 -10 1.37 0.47 5 5 -9 81.59 4.15 5 5 -8 3.15 0.49 5 5 -7 15.77 1.02 5 -5 -6 1.89 0.40 5 -5 -5 2.21 0.42 -5 -5 4 -0.16 0.65 5 -5 -4 -0.23 0.38 -5 -5 3 3.82 0.78 5 -5 -3 4.05 0.50 -5 5 2 0.06 0.79 5 -5 -2 0.39 0.40 5 -5 -1 11.69 0.83 -5 5 1 11.95 1.29 5 -5 0 8.34 0.70 -5 5 0 8.97 1.18 -5 5 -1 2.06 0.92 5 -5 1 2.72 0.47 -5 5 -2 8.31 1.18 -5 5 -3 5.03 1.04 -5 5 -4 6.52 1.10 -5 5 -5 6.35 1.06 -5 5 -6 8.89 1.12 -5 5 -7 10.37 1.21 -5 5 -7 12.33 1.16 -5 5 -8 23.61 1.60 -5 5 -9 4.56 0.75 -5 5 -10 25.06 1.55 -5 -6 15 0.24 0.44 -5 -6 14 22.76 1.33 5 6 -14 17.75 1.07 5 6 -13 16.07 0.97 5 6 -12 4.49 0.46 5 6 -11 -0.09 0.31 5 6 -10 5.07 0.49 -5 -6 9 0.59 0.60 5 6 -9 -0.21 0.30 -5 -6 8 0.44 0.60 -5 -6 7 0.35 0.62 -5 -6 6 23.95 1.51 -5 6 6 18.20 1.40 -5 -6 5 55.32 3.02 -5 6 5 52.55 3.00 -5 -6 4 0.81 0.64 -5 6 4 -0.05 0.70 -5 -6 3 7.45 0.88 -5 6 3 6.98 1.00 -5 6 2 13.49 1.23 -5 6 2 17.05 1.38 -5 6 1 1.46 0.75 -5 6 1 2.23 0.84 -5 6 0 1.70 0.78 -5 6 0 1.60 0.84 -5 6 -1 7.81 1.04 -5 6 -1 10.23 1.15 -5 6 -2 -0.06 0.76 -5 6 -2 -0.23 0.80 -5 6 -3 1.04 0.78 -5 6 -3 1.01 0.81 -5 6 -4 1.59 0.80 -5 6 -4 1.34 0.81 -5 6 -5 3.37 0.84 -5 6 -5 4.70 0.86 -5 6 -6 -0.26 0.71 -5 6 -7 3.60 0.79 -5 6 -7 4.57 0.78 -5 6 -8 -0.19 0.54 -5 6 -9 0.70 0.54 -5 -7 10 2.74 0.60 -5 -7 9 0.96 0.55 -5 -7 8 31.77 1.91 -5 -7 7 0.30 0.55 -5 -7 6 12.83 1.08 -5 -7 5 22.16 1.49 -5 -7 4 -0.31 0.56 -5 7 4 0.35 0.51 -5 -7 3 0.75 0.56 -5 7 3 -0.31 0.55 -5 7 2 12.07 1.05 -5 7 2 14.99 1.12 -5 7 1 0.04 0.58 -5 7 1 0.52 0.62 -5 7 0 -0.80 0.63 -5 7 0 0.44 0.64 -5 7 -1 9.93 1.02 -5 7 -1 12.76 1.07 -5 7 -2 7.41 0.91 -5 7 -2 9.30 0.94 -5 7 -3 2.38 0.70 -5 7 -3 2.18 0.71 -5 7 -4 1.33 0.64 -5 7 -4 1.23 0.64 -5 7 -5 0.17 0.59 -5 7 -5 0.54 0.57 -5 7 -6 7.72 0.82 -5 7 -6 8.16 0.82 -5 7 -8 0.50 0.39 -5 -8 8 6.33 0.66 -5 -8 7 5.66 0.64 -5 -8 6 4.69 0.61 -5 -8 5 0.38 0.44 -5 -8 4 7.39 0.71 -5 8 0 9.93 0.79 -5 8 -1 17.03 1.12 -5 8 -2 0.50 0.45 -5 8 -3 3.47 0.53 6 0 -11 0.22 0.20 -6 0 11 -0.35 0.27 -6 0 10 27.79 1.65 6 0 -10 36.05 1.65 6 0 -9 0.01 0.24 -6 0 9 -0.10 0.34 -6 0 8 52.33 2.91 6 0 -8 64.21 2.92 6 0 -7 0.11 0.30 -6 0 7 -0.16 0.38 6 0 -6 1.31 0.33 -6 0 6 0.80 0.39 6 0 -5 0.14 0.31 -6 0 5 0.15 0.38 -6 0 4 13.54 0.88 6 0 -4 13.86 0.85 6 0 -3 0.29 0.35 -6 0 3 -0.09 0.37 -6 0 2 7.84 0.62 6 0 -2 7.26 0.58 6 0 -1 -0.09 0.33 -6 0 1 0.21 0.35 -6 0 0 90.41 4.20 6 0 0 79.89 4.18 6 0 1 0.24 0.32 -6 0 -1 0.40 0.35 -6 0 -2 28.45 1.39 6 0 2 23.23 1.37 6 0 3 -0.14 0.28 -6 0 -3 0.24 0.30 6 0 4 6.32 0.51 -6 0 -4 8.63 0.54 6 0 5 -0.24 0.23 -6 0 -5 -0.03 0.24 6 0 6 0.13 0.19 -6 1 11 21.82 1.26 6 -1 -11 25.21 1.26 6 1 -11 25.61 1.26 6 -1 -10 1.12 0.25 6 1 -10 0.74 0.25 -6 -1 10 0.86 0.30 6 -1 -9 1.00 0.26 6 1 -9 1.47 0.28 -6 -1 9 0.87 0.35 6 -1 -8 1.29 0.28 -6 -1 8 0.54 0.34 -6 -1 7 5.54 0.52 6 -1 -7 6.18 0.48 6 -1 -6 3.10 0.36 -6 -1 6 1.61 0.40 6 -1 -5 3.64 0.39 -6 -1 5 1.98 0.42 -6 -1 4 9.54 0.69 6 -1 -4 9.46 0.66 -6 -1 3 8.92 0.67 6 -1 -3 9.38 0.65 -6 -1 2 37.47 1.96 6 -1 -2 37.61 1.95 -6 -1 1 9.71 0.67 6 -1 -1 9.16 0.65 -6 -1 0 70.09 3.28 6 -1 0 61.81 3.27 -6 -1 -1 60.30 2.81 6 -1 1 51.69 2.80 -6 -1 -2 16.42 0.91 6 -1 2 14.60 0.90 6 -1 3 1.41 0.30 6 1 3 1.02 0.31 -6 -1 -3 1.19 0.32 6 -1 4 28.68 1.56 6 1 4 28.51 1.56 6 -1 5 0.20 0.21 6 1 5 0.34 0.22 -6 1 -5 0.33 0.24 -6 -1 -5 0.29 0.23 6 -2 -9 3.81 0.32 6 2 -9 3.97 0.33 -6 2 9 3.34 0.37 6 -2 -8 2.42 0.28 6 2 -8 2.53 0.30 -6 2 8 1.96 0.32 -6 -2 8 1.69 0.33 -6 2 7 15.03 0.90 -6 -2 7 13.76 0.88 6 -2 -7 17.06 0.88 6 2 -7 16.23 0.89 -6 2 6 11.40 0.74 -6 -2 6 10.61 0.74 6 -2 -6 11.84 0.72 6 2 -6 13.57 0.74 6 -2 -5 1.58 0.31 6 2 -5 1.50 0.31 -6 2 5 1.39 0.36 -6 -2 5 1.30 0.35 6 -2 -4 1.33 0.29 6 2 -4 1.13 0.31 -6 2 4 0.34 0.32 -6 -2 4 0.41 0.32 -6 2 3 36.10 1.83 -6 -2 3 34.22 1.81 6 -2 -3 35.89 1.82 6 2 -3 34.37 1.82 -6 2 2 25.10 1.40 -6 -2 2 26.08 1.39 6 -2 -2 27.47 1.40 6 2 -2 26.49 1.41 -6 2 1 29.60 1.44 -6 -2 1 26.69 1.42 6 -2 -1 25.71 1.43 6 2 -1 25.89 1.43 -6 2 0 5.35 0.45 -6 -2 0 5.15 0.45 6 -2 0 4.49 0.43 6 2 0 5.24 0.45 6 -2 1 0.76 0.28 6 2 1 0.95 0.28 -6 2 -1 1.07 0.32 -6 -2 -1 0.50 0.28 6 -2 2 1.50 0.29 6 2 2 0.97 0.27 -6 2 -2 1.09 0.29 -6 -2 -2 1.18 0.28 6 -2 3 10.48 0.69 6 2 3 12.15 0.70 -6 2 -3 13.09 0.71 -6 -2 -3 11.78 0.68 0 0 0 0.00 0.00 TITL FFA4CH3-8_auto in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 4.958606 11.270866 24.119000 90.0000 95.6740 90.0000 ZERR 19.00 0.000169 0.000428 0.000757 0.0000 0.0031 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O F UNIT 19.00 19.00 19.00 19.00 19.00 REM CrysAlisPro recorded range (K): Min=173.0; max=173.0; aver:173.0 TEMP -100 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 3109 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.263 _oxdiff_exptl_absorpt_empirical_full_min 0.393 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O -0.2727(2) 0.51346(11) 0.45508(5) 0.0320(3) Uani 1 1 d . . . . . O1 O -0.3801(2) 0.34806(11) 0.49874(5) 0.0343(3) Uani 1 1 d . . . . . H1 H -0.492183 0.394166 0.511405 0.051 Uiso 1 1 calc R U . . . F003 F 0.5486(3) 0.94078(11) 0.32220(5) 0.0572(4) Uani 1 1 d . . . . . F004 F 0.5623(4) 0.87327(13) 0.40450(5) 0.0681(4) Uani 1 1 d . . . . . F005 F 0.9044(3) 0.85442(13) 0.35716(8) 0.0779(5) Uani 1 1 d . . . . . N006 N 0.0849(3) 0.49724(14) 0.37933(6) 0.0358(4) Uani 1 1 d . . . . . H006 H -0.044649 0.538284 0.392845 0.043 Uiso 1 1 calc R U . . . C007 C -0.0571(3) 0.33158(15) 0.43414(6) 0.0285(4) Uani 1 1 d . . . . . C008 C 0.1036(3) 0.37960(16) 0.39401(6) 0.0288(4) Uani 1 1 d . . . . . C009 C -0.2439(3) 0.40575(15) 0.46284(6) 0.0279(4) Uani 1 1 d . . . . . C00A C 0.2508(3) 0.55954(16) 0.34493(7) 0.0307(4) Uani 1 1 d . . . . . C00B C 0.5255(3) 0.73237(16) 0.33133(7) 0.0315(4) Uani 1 1 d . . . . . C00C C 0.5856(3) 0.69137(16) 0.27902(7) 0.0323(4) Uani 1 1 d . . . . . C00D C 0.2860(3) 0.30174(17) 0.37082(7) 0.0344(4) Uani 1 1 d . . . . . H00D H 0.400441 0.331545 0.344695 0.041 Uiso 1 1 calc R U . . . C00E C 0.3604(3) 0.66695(16) 0.36340(7) 0.0321(4) Uani 1 1 d . . . . . H00E H 0.322305 0.696670 0.398651 0.039 Uiso 1 1 calc R U . . . C00F C 0.2999(3) 0.52007(17) 0.29195(7) 0.0338(4) Uani 1 1 d . . . . . H00F H 0.218856 0.448734 0.277456 0.041 Uiso 1 1 calc R U . . . C00G C 0.4673(3) 0.58517(17) 0.26050(7) 0.0347(4) Uani 1 1 d . . . . . H00G H 0.502044 0.555904 0.224964 0.042 Uiso 1 1 calc R U . . . C00H C -0.0367(4) 0.21051(17) 0.44765(8) 0.0379(4) Uani 1 1 d . . . . . H00H H -0.146230 0.179041 0.474286 0.045 Uiso 1 1 calc R U . . . C00I C 0.3009(4) 0.18405(18) 0.38530(8) 0.0392(4) Uani 1 1 d . . . . . H00I H 0.425497 0.134086 0.368953 0.047 Uiso 1 1 calc R U . . . C00J C 0.6351(4) 0.84792(18) 0.35405(8) 0.0403(4) Uani 1 1 d . . . . . C00K C 0.7725(4) 0.75539(19) 0.24287(8) 0.0419(5) Uani 1 1 d . . . . . H00A H 0.720621 0.839191 0.239664 0.063 Uiso 1 1 calc R U . . . H00B H 0.757834 0.719251 0.205733 0.063 Uiso 1 1 calc R U . . . H00C H 0.959859 0.749095 0.259838 0.063 Uiso 1 1 calc R U . . . C00L C 0.1380(4) 0.13621(18) 0.42332(9) 0.0444(5) Uani 1 1 d . . . . . H00L H 0.146867 0.054157 0.432312 0.053 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 O2 0.0337(6) 0.0337(7) 0.0314(6) 0.0030(5) 0.0169(5) 0.0051(5) O1 0.0372(6) 0.0369(7) 0.0318(6) 0.0033(5) 0.0186(5) 0.0043(5) F003 0.0823(9) 0.0334(6) 0.0558(7) 0.0054(5) 0.0071(6) 0.0098(6) F004 0.1122(12) 0.0539(8) 0.0397(7) -0.0107(6) 0.0153(7) -0.0137(8) F005 0.0416(7) 0.0552(9) 0.1341(15) -0.0245(9) -0.0051(8) -0.0005(6) N006 0.0380(7) 0.0365(8) 0.0367(8) 0.0051(6) 0.0231(6) 0.0084(6) C007 0.0268(7) 0.0329(9) 0.0268(7) -0.0022(6) 0.0072(6) 0.0014(6) C008 0.0279(7) 0.0359(9) 0.0235(7) -0.0027(6) 0.0066(6) 0.0024(6) C009 0.0258(7) 0.0366(9) 0.0222(7) 0.0009(6) 0.0075(5) -0.0001(6) C00A 0.0296(8) 0.0376(9) 0.0268(7) 0.0047(7) 0.0126(6) 0.0071(7) C00B 0.0313(8) 0.0333(9) 0.0305(8) 0.0046(7) 0.0064(6) 0.0077(7) C00C 0.0289(8) 0.0380(9) 0.0318(8) 0.0073(7) 0.0124(6) 0.0078(7) C00D 0.0334(8) 0.0411(10) 0.0306(8) -0.0038(7) 0.0129(6) 0.0038(7) C00E 0.0370(8) 0.0368(10) 0.0240(7) 0.0026(6) 0.0098(6) 0.0109(7) C00F 0.0349(8) 0.0399(10) 0.0279(8) -0.0004(7) 0.0107(6) 0.0001(7) C00G 0.0392(9) 0.0416(10) 0.0257(8) 0.0004(7) 0.0147(6) 0.0058(7) C00H 0.0392(9) 0.0352(10) 0.0418(9) 0.0015(8) 0.0162(7) -0.0003(8) C00I 0.0398(9) 0.0393(10) 0.0403(9) -0.0097(8) 0.0129(7) 0.0083(8) C00J 0.0433(10) 0.0378(10) 0.0400(9) 0.0011(8) 0.0055(7) 0.0058(8) C00K 0.0380(9) 0.0461(11) 0.0449(10) 0.0091(8) 0.0204(8) 0.0046(8) C00L 0.0495(11) 0.0320(10) 0.0540(11) -0.0020(8) 0.0167(9) 0.0049(8) 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' F F 0.0727 0.0534 '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' O O 0.0492 0.0322 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C009 O1 H1 109.5 . . ? C008 N006 H006 116.4 . . ? C008 N006 C00A 127.12(13) . . ? C00A N006 H006 116.4 . . ? C008 C007 C009 121.74(15) . . ? C00H C007 C008 119.74(15) . . ? C00H C007 C009 118.51(14) . . ? N006 C008 C007 121.03(14) . . ? N006 C008 C00D 121.77(15) . . ? C00D C008 C007 117.18(16) . . ? O2 C009 O1 121.63(14) . . ? O2 C009 C007 123.81(14) . . ? O1 C009 C007 114.55(15) . . ? C00E C00A N006 118.66(14) . . ? C00E C00A C00F 118.35(15) . . ? C00F C00A N006 122.94(17) . . ? C00C C00B C00J 120.99(16) . . ? C00E C00B C00C 120.94(17) . . ? C00E C00B C00J 118.07(15) . . ? C00B C00C C00K 123.82(17) . . ? C00G C00C C00B 116.92(15) . . ? C00G C00C C00K 119.25(15) . . ? C008 C00D H00D 119.3 . . ? C00I C00D C008 121.30(16) . . ? C00I C00D H00D 119.3 . . ? C00A C00E C00B 121.27(15) . . ? C00A C00E H00E 119.4 . . ? C00B C00E H00E 119.4 . . ? C00A C00F H00F 120.0 . . ? C00G C00F C00A 119.96(17) . . ? C00G C00F H00F 120.0 . . ? C00C C00G C00F 122.47(15) . . ? C00C C00G H00G 118.8 . . ? C00F C00G H00G 118.8 . . ? C007 C00H H00H 119.1 . . ? C00L C00H C007 121.73(16) . . ? C00L C00H H00H 119.1 . . ? C00D C00I H00I 119.2 . . ? C00D C00I C00L 121.54(16) . . ? C00L C00I H00I 119.2 . . ? F003 C00J C00B 112.67(16) . . ? F004 C00J F003 104.77(16) . . ? F004 C00J C00B 113.57(16) . . ? F005 C00J F003 104.53(17) . . ? F005 C00J F004 107.27(18) . . ? F005 C00J C00B 113.25(16) . . ? C00C C00K H00A 109.5 . . ? C00C C00K H00B 109.5 . . ? C00C C00K H00C 109.5 . . ? H00A C00K H00B 109.5 . . ? H00A C00K H00C 109.5 . . ? H00B C00K H00C 109.5 . . ? C00H C00L C00I 118.46(18) . . ? C00H C00L H00L 120.8 . . ? C00I C00L H00L 120.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C009 1.234(2) . ? O1 H1 0.8400 . ? O1 C009 1.3208(19) . ? F003 C00J 1.343(2) . ? F004 C00J 1.334(2) . ? F005 C00J 1.332(2) . ? N006 H006 0.8800 . ? N006 C008 1.373(2) . ? N006 C00A 1.412(2) . ? C007 C008 1.420(2) . ? C007 C009 1.471(2) . ? C007 C00H 1.404(3) . ? C008 C00D 1.415(2) . ? C00A C00E 1.383(3) . ? C00A C00F 1.397(2) . ? C00B C00C 1.403(2) . ? C00B C00E 1.392(2) . ? C00B C00J 1.494(3) . ? C00C C00G 1.387(3) . ? C00C C00K 1.516(2) . ? C00D H00D 0.9500 . ? C00D C00I 1.372(3) . ? C00E H00E 0.9500 . ? C00F H00F 0.9500 . ? C00F C00G 1.388(2) . ? C00G H00G 0.9500 . ? C00H H00H 0.9500 . ? C00H C00L 1.377(3) . ? C00I H00I 0.9500 . ? C00I C00L 1.389(3) . ? C00K H00A 0.9800 . ? C00K H00B 0.9800 . ? C00K H00C 0.9800 . ? C00L H00L 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N006 C008 C00D C00I -179.25(17) . . . . ? N006 C00A C00E C00B 179.98(15) . . . . ? N006 C00A C00F C00G -179.40(16) . . . . ? C007 C008 C00D C00I 1.9(3) . . . . ? C007 C00H C00L C00I 1.3(3) . . . . ? C008 N006 C00A C00E -130.95(18) . . . . ? C008 N006 C00A C00F 51.9(3) . . . . ? C008 C007 C009 O2 -1.0(2) . . . . ? C008 C007 C009 O1 179.66(14) . . . . ? C008 C007 C00H C00L 0.6(3) . . . . ? C008 C00D C00I C00L 0.0(3) . . . . ? C009 C007 C008 N006 -1.8(2) . . . . ? C009 C007 C008 C00D 177.07(15) . . . . ? C009 C007 C00H C00L -178.66(17) . . . . ? C00A N006 C008 C007 172.68(16) . . . . ? C00A N006 C008 C00D -6.1(3) . . . . ? C00A C00F C00G C00C -1.6(3) . . . . ? C00B C00C C00G C00F -1.0(3) . . . . ? C00C C00B C00E C00A 0.1(3) . . . . ? C00C C00B C00J F003 62.0(2) . . . . ? C00C C00B C00J F004 -179.11(16) . . . . ? C00C C00B C00J F005 -56.4(2) . . . . ? C00D C00I C00L C00H -1.6(3) . . . . ? C00E C00A C00F C00G 3.4(2) . . . . ? C00E C00B C00C C00G 1.7(2) . . . . ? C00E C00B C00C C00K -177.49(16) . . . . ? C00E C00B C00J F003 -117.60(18) . . . . ? C00E C00B C00J F004 1.3(2) . . . . ? C00E C00B C00J F005 124.01(19) . . . . ? C00F C00A C00E C00B -2.7(2) . . . . ? C00H C007 C008 N006 178.99(16) . . . . ? C00H C007 C008 C00D -2.2(2) . . . . ? C00H C007 C009 O2 178.25(16) . . . . ? C00H C007 C009 O1 -1.1(2) . . . . ? C00J C00B C00C C00G -177.81(16) . . . . ? C00J C00B C00C C00K 3.0(3) . . . . ? C00J C00B C00E C00A 179.69(15) . . . . ? C00K C00C C00G C00F 178.26(16) . . . . ?