#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:28:21 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227269 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035857.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_4035857 loop_ _publ_author_name 'Ohta, Reiya' 'Matsumoto, Nao' 'Ueyama, Yoshifumi' 'Kuboki, Yuichi' 'Aoyama, Hiroshi' 'Murai, Kenichi' 'Arisawa, Mitsuhiro' 'Maegawa, Tomohiro' 'Fujioka, Hiromichi' _publ_section_title ; Highly Discriminative and Chemoselective Deprotection/Transformations of Acetals with the Combination of Trialkylsilyl Triflate/2,4,6-Collidine. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6432 _journal_page_last 6443 _journal_paper_doi 10.1021/acs.joc.8b00675 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C9 H12 F3 N O3 S' _chemical_formula_sum 'C9 H12 F3 N O3 S' _chemical_formula_weight 271.25 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 95.622(7) _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 17.1050(13) _cell_length_b 8.9423(6) _cell_length_c 16.1115(15) _cell_measurement_reflns_used 3319 _cell_measurement_temperature 100 _cell_measurement_theta_max 74.71 _cell_measurement_theta_min 5.52 _cell_volume 2452.5(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_molecular_graphics 'CrystalStructure 4.2.4' _computing_publication_material 'CrystalStructure 4.2.4 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SHELXT Version 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 5.811 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1573 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9519 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.245 _diffrn_reflns_theta_min 5.197 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.730 _exptl_absorpt_correction_T_max 0.479 _exptl_absorpt_correction_T_min 0.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1120.00 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.270 _refine_diff_density_max 1.26 _refine_diff_density_min -1.94 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.407 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 157 _refine_ls_number_reflns 2219 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1708 _refine_ls_R_factor_gt 0.1461 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3290 _refine_ls_wR_factor_ref 0.3500 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1687 _reflns_number_total 2219 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file jo8b00675_si_002.cif _cod_data_source_block SX16121R _cod_database_code 4035857 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL SX16121R CELL 1.54184 17.10500 8.94230 16.11150 90.000 95.622 90.000 ZERR 8 0.00130 0.00060 0.00150 0.000 0.007 0.000 LATT 7 SYMM -X, +Y, 1/2-Z SFAC C H N S F O UNIT 72 96 8 8 24 24 L.S. 10 FMAP 2 PLAN -25 WPDB -2 LIST 4 TEMP 23.0 ACTA SIZE 0.320 0.280 0.270 ISOR 0.003 BOND $H CONF REM HTAB HTAB WGHT 0.200000 FVAR 0.19207 S1 4 0.637739 0.814920 0.387563 11.00000 0.00668 0.00643 = 0.02190 0.00218 0.00637 0.00058 F6 5 0.504206 0.677764 0.351524 11.00000 0.03219 0.06674 = 0.06240 -0.02202 0.01073 -0.03148 F7 5 0.498206 0.920653 0.341319 11.00000 0.02800 0.07146 = 0.05606 0.00256 0.00191 0.03088 F18 5 0.508683 0.815601 0.462854 11.00000 0.02285 0.06035 = 0.04696 -0.00464 0.02146 0.00131 O2 6 0.651669 0.789466 0.302174 11.00000 0.01456 0.01707 = 0.02074 -0.00092 0.00999 -0.00007 O3 6 0.656484 0.962369 0.418959 11.00000 0.03497 0.00690 = 0.03081 -0.00391 0.00441 -0.01082 O4 6 0.664133 0.695934 0.444293 11.00000 0.02927 0.01165 = 0.03014 0.00962 0.00945 0.00880 N5 3 0.662540 0.711286 0.618674 11.00000 0.00945 0.00367 = 0.01611 -0.00010 0.00526 0.00094 AFIX 43 H5 2 0.673021 0.718599 0.567706 11.00000 -1.20000 AFIX 0 C9 1 0.649620 0.573580 0.649098 11.00000 0.01209 0.00812 = 0.01927 0.00173 0.00463 -0.00185 C10 1 0.659866 0.839768 0.664508 11.00000 0.01105 0.00755 = 0.02130 -0.00116 0.00636 0.00219 C11 1 0.532458 0.807819 0.385711 11.00000 0.02256 0.03020 = 0.02758 -0.00426 0.00356 -0.00035 C12 1 0.640675 0.826634 0.744835 11.00000 0.02142 0.01330 = 0.02094 -0.00161 0.00653 0.00159 AFIX 43 H12 2 0.638865 0.911809 0.777714 11.00000 -1.20000 AFIX 0 C13 1 0.631092 0.560839 0.730374 11.00000 0.02160 0.01331 = 0.02297 0.00246 0.00682 -0.00203 AFIX 43 H13 2 0.623522 0.466862 0.752981 11.00000 -1.20000 AFIX 0 C14 1 0.623804 0.687457 0.778072 11.00000 0.02749 0.01461 = 0.02500 0.00030 0.00474 -0.00039 C15 1 0.678526 0.982269 0.623877 11.00000 0.02094 0.00671 = 0.02731 -0.00119 0.01098 0.00221 AFIX 137 H15A 2 0.730725 0.977393 0.606916 11.00000 -1.20000 H15B 2 0.675283 1.063222 0.662525 11.00000 -1.20000 H15C 2 0.641660 0.998525 0.575864 11.00000 -1.20000 AFIX 0 C16 1 0.657845 0.443034 0.592549 11.00000 0.02043 0.00521 = 0.02884 -0.00259 0.01131 -0.00812 AFIX 137 H16A 2 0.706004 0.451872 0.566945 11.00000 -1.20000 H16B 2 0.614337 0.441343 0.550125 11.00000 -1.20000 H16C 2 0.658471 0.352111 0.624287 11.00000 -1.20000 AFIX 0 C17 1 0.600102 0.674972 0.865786 11.00000 0.06185 0.03355 = 0.03272 -0.00012 0.01652 -0.00264 AFIX 137 H17A 2 0.618401 0.761254 0.897408 11.00000 -1.20000 H17B 2 0.622944 0.586505 0.891761 11.00000 -1.20000 H17C 2 0.543911 0.669230 0.863880 11.00000 -1.20000 AFIX 0 HKLF 4 REM SX16121R REM R1 = 0.1461 for 1687 Fo > 4sig(Fo) and 0.1708 for all 2219 data REM 157 parameters refined using 102 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB N5 O4 EQIV $1 x, -y+2, z+1/2 HTAB C12 S1_$1 HTAB C12 O3_$1 EQIV $2 x, -y+1, z+1/2 HTAB C13 O2_$2 EQIV $3 -x+3/2, -y+3/2, -z+1 HTAB C15 O4_$3 HTAB C15 O3 HTAB C16 O3_$3 REM Highest difference peak 1.264, deepest hole -1.945, 1-sigma level 0.271 Q1 1 0.6626 0.6612 0.3721 11.00000 0.05 1.26 Q2 1 0.5825 0.8887 0.3227 11.00000 0.05 1.12 Q3 1 0.5842 0.9357 0.3600 11.00000 0.05 1.12 Q4 1 0.5806 0.7396 0.4434 11.00000 0.05 1.11 Q5 1 0.6606 0.9599 0.3657 11.00000 0.05 1.09 Q6 1 0.8601 0.7989 0.3026 11.00000 0.05 1.06 Q7 1 0.5802 0.8873 0.4395 11.00000 0.05 1.05 Q8 1 0.5684 0.8112 0.3351 11.00000 0.05 1.01 Q9 1 0.7178 0.8157 0.3649 11.00000 0.05 0.97 Q10 1 0.7115 0.8646 0.3543 11.00000 0.05 0.94 Q11 1 0.6048 0.6755 0.3588 11.00000 0.05 0.92 Q12 1 0.7083 0.7226 0.3827 11.00000 0.05 0.92 Q13 1 0.6065 0.6608 0.4061 11.00000 0.05 0.91 Q14 1 0.7189 0.7519 0.3930 11.00000 0.05 0.89 Q15 1 0.6394 0.8251 0.4803 11.00000 0.05 0.85 Q16 1 0.8509 0.8048 0.2032 11.00000 0.05 0.82 Q17 1 0.7092 0.8256 0.4226 11.00000 0.05 0.80 Q18 1 0.7867 0.9771 0.3009 11.00000 0.05 0.77 Q19 1 0.8689 0.8150 0.1146 11.00000 0.05 0.76 Q20 1 0.5000 0.8789 0.2500 10.50000 0.05 0.75 Q21 1 0.8195 0.7970 0.3555 11.00000 0.05 0.75 Q22 1 0.9166 0.7130 0.3397 11.00000 0.05 0.70 Q23 1 0.4919 0.7869 0.2570 11.00000 0.05 0.66 Q24 1 0.8046 0.6656 0.4121 11.00000 0.05 0.64 Q25 1 0.6458 0.5950 0.5363 11.00000 0.05 0.62 ; _shelx_res_checksum 89564 _shelx_hkl_file ; 0 0 1 0.57 1.74 0 0 -1 0.26 0.47 0 0 -1 -0.24 2.79 0 0 -2 236.49 17.09 0 0 2 206.62 17.08 0 0 2 157.86 18.15 0 0 -2 154.63 21.09 0 0 2 139.79 19.26 0 0 3 5.65 13.46 0 0 -3 -2.15 15.61 0 0 3 -3.54 16.51 0 0 -3 -15.80 21.40 0 0 3 -1.09 2.25 0 0 -4 2883.59 233.39 0 0 4 2137.20 230.56 0 0 -4 2985.61 232.24 0 0 4 2881.50 230.40 0 0 4 3283.47 232.98 0 0 4 1981.86 230.30 0 0 4 2534.76 231.70 0 0 4 3187.89 228.15 0 0 5 -6.18 14.46 0 0 -5 -1.67 14.90 0 0 5 -6.04 9.19 0 0 5 -0.95 11.52 0 0 -5 0.25 15.23 0 0 5 0.19 2.34 0 0 5 0.60 14.58 0 0 -5 -15.10 21.05 0 0 6 100.10 20.52 0 0 -6 150.01 21.98 0 0 6 149.64 17.75 0 0 -6 126.57 27.68 0 0 6 191.99 23.36 0 0 7 1.08 10.45 0 0 -7 -4.12 17.01 0 0 7 -2.20 13.03 0 0 8 168.06 26.17 0 0 -8 250.95 29.41 0 0 -9 9.94 15.55 0 0 9 2.20 13.98 0 0 10 6.12 12.94 0 0 -14 47.01 7.41 0 0 -16 -3.39 6.62 0 0 -17 3.14 5.69 0 0 -18 33.84 5.60 0 0 -18 24.99 4.92 0 0 -18 26.16 4.65 0 0 -19 0.10 3.20 0 0 -19 0.80 2.75 0 2 0 804.82 98.39 0 2 0 1417.81 97.18 0 -2 0 1556.41 99.45 0 -2 0 819.24 97.76 0 -2 0 1320.68 97.35 0 2 1 920.10 53.51 0 2 1 499.88 54.06 0 2 -1 548.26 54.33 0 -2 1 781.59 53.99 0 -2 1 439.02 55.14 0 -2 1 524.35 55.67 0 -2 -1 562.15 54.13 0 2 2 -0.16 4.03 0 2 -2 -11.06 10.33 0 2 -2 3.18 5.40 0 2 -2 3.06 13.64 0 -2 2 12.75 10.04 0 -2 -2 -14.72 18.89 0 -2 2 10.35 11.29 0 2 -3 127.52 19.94 0 2 3 266.12 23.31 0 2 -3 157.00 18.05 0 -2 3 230.86 19.98 0 -2 3 120.27 20.42 0 -2 -3 236.46 16.88 0 -2 -3 169.43 22.96 0 -2 -3 149.54 25.78 0 2 -4 9.96 18.08 0 2 -4 7.71 8.66 0 -2 4 0.51 10.05 0 -2 -4 15.54 3.58 0 -2 -4 4.43 12.98 0 -2 4 -5.41 14.43 0 -2 4 3.86 11.99 0 2 -5 37.38 13.16 0 -2 5 68.07 16.80 0 -2 -5 64.25 15.70 0 2 -6 5.78 14.10 0 -2 6 9.10 2.65 0 -2 -6 27.91 16.24 0 -2 6 4.97 16.26 0 -2 6 13.37 16.04 0 -2 -6 14.02 3.75 0 -2 -8 17.52 26.62 0 -2 8 252.48 24.31 0 2 -9 1.22 25.39 0 -2 9 1.78 13.12 0 2 -10 4.43 3.46 0 -2 -10 9.08 4.83 0 2 -11 166.61 15.78 0 2 -11 204.59 15.89 0 -2 -11 190.30 16.43 0 2 -12 261.17 19.89 0 2 -12 233.18 19.78 0 2 -12 207.15 22.21 0 -2 -12 189.48 20.87 0 -2 -12 254.40 20.65 0 2 -13 2.95 3.98 0 2 -13 0.35 3.51 0 -2 -13 1.86 6.36 0 2 -14 86.05 7.17 0 2 -14 78.51 7.47 0 -2 -14 51.93 8.99 0 -2 -14 44.17 10.92 0 2 -15 8.15 2.60 0 2 -15 8.65 3.35 0 -2 -15 -2.30 8.63 0 -2 -15 -2.75 5.94 0 -2 -15 -13.16 8.36 0 2 -16 33.30 3.93 0 -2 -16 24.30 7.69 0 -2 -16 28.01 5.37 0 2 -17 12.27 2.39 0 2 -17 13.66 5.11 0 2 -17 9.51 4.61 0 -2 -17 7.47 3.62 0 -2 -17 10.13 5.91 0 2 -18 12.47 5.09 0 2 -18 33.29 4.17 0 2 -18 13.88 4.80 0 -2 -18 16.90 4.53 0 -2 -18 44.00 4.97 0 -2 -18 30.79 5.11 0 4 0 13.17 8.41 0 -4 0 31.75 10.28 0 -4 0 16.90 17.61 0 -4 0 14.69 5.14 0 4 1 5.46 6.55 0 -4 -1 7.42 18.93 0 -4 1 10.39 10.43 0 -4 1 -1.54 6.56 0 4 2 2.80 5.95 0 -4 2 -10.00 14.27 0 -4 2 -0.18 8.26 0 -4 -2 11.58 15.35 0 -4 -2 37.53 5.25 0 -4 -2 -6.67 21.41 0 4 -3 157.53 21.16 0 4 -3 144.11 27.32 0 -4 -3 176.63 29.17 0 4 -4 3.01 7.90 0 -4 -4 6.83 4.59 0 -4 -4 6.05 23.19 0 -4 4 9.04 7.65 0 4 -5 5.09 9.84 0 -4 5 -2.93 8.26 0 -4 -5 -3.14 23.10 0 -4 -5 0.47 15.14 0 4 -6 22.64 13.67 0 -4 6 77.68 13.65 0 -4 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3.88 -17 -3 2 29.33 4.56 17 -3 -2 17.98 4.64 17 3 -1 24.66 3.97 17 -3 -1 24.87 6.63 -17 -3 1 27.50 4.32 17 3 0 209.19 18.57 17 -3 0 224.94 19.42 -17 -3 0 238.13 18.63 -17 -3 -1 35.79 4.33 17 -3 1 28.30 6.23 -17 -3 -2 180.88 14.33 17 -3 2 150.42 14.96 17 3 3 1.26 2.85 17 -3 3 1.05 3.21 17 -3 3 2.13 4.27 -17 -3 -3 0.02 2.44 17 3 4 197.83 15.60 17 -3 4 160.55 15.83 -17 -3 -4 201.89 15.43 17 -3 4 175.12 15.62 17 3 5 28.31 3.49 17 -3 5 30.27 3.61 17 3 6 2.04 1.98 -17 3 -6 2.87 2.58 17 -3 6 3.64 1.98 17 3 7 0.46 1.55 -17 3 -7 2.37 2.29 -17 3 -7 3.77 1.11 -17 -3 -7 1.54 2.44 17 5 -7 0.60 3.01 -17 -5 7 3.99 2.04 17 -5 -7 2.00 4.46 17 5 -6 6.25 3.13 -17 -5 6 10.99 2.49 17 -5 -6 5.16 5.33 17 5 -5 3.23 2.88 17 -5 -5 0.67 2.15 -17 -5 5 2.01 2.54 17 -5 -5 3.93 5.45 17 -5 -4 1.81 2.54 -17 -5 4 1.28 2.80 17 5 -3 3.64 1.98 17 -5 -3 3.32 2.78 17 -5 -3 1.80 6.05 -17 -5 3 5.79 2.88 17 5 -2 7.17 2.26 -17 -5 2 13.10 3.03 17 -5 -2 12.82 3.32 17 5 -1 5.46 2.30 17 -5 -1 6.25 5.65 17 -5 -1 5.88 3.16 17 5 0 136.14 11.97 17 -5 0 135.06 13.06 -17 -5 0 162.36 12.09 17 -5 0 133.55 12.20 17 5 1 10.36 2.58 17 -5 1 12.11 4.78 -17 -5 -1 15.85 2.77 17 5 2 83.22 7.02 17 -5 2 64.58 7.77 -17 -5 -2 86.84 7.00 17 -5 2 72.76 7.20 17 -5 3 -0.27 2.44 -17 -5 -3 2.04 1.95 17 5 4 69.31 5.85 -17 -5 -4 67.71 5.74 17 -5 4 61.52 5.92 18 0 -11 -2.48 3.34 18 0 -11 2.19 2.72 18 0 -10 96.30 9.17 18 0 -10 97.19 8.71 18 0 -9 -2.17 3.42 18 0 -8 233.17 18.17 18 0 -8 205.34 22.16 18 0 -8 198.84 17.53 18 0 -7 3.34 5.24 18 0 -7 13.61 13.22 18 0 -7 1.84 3.39 18 0 -6 87.60 9.16 18 0 -6 95.42 15.78 18 0 -6 86.27 8.26 18 0 -5 5.02 5.16 18 0 -5 18.71 4.33 18 0 -4 -0.59 4.46 18 0 -4 2.19 4.04 18 0 -3 3.23 4.01 18 0 -3 1.96 4.36 18 0 -2 -0.45 3.40 18 0 -2 -0.08 4.33 18 0 1 0.72 4.04 18 0 2 18.41 4.27 18 0 3 -0.90 3.45 18 0 4 11.32 3.29 18 0 5 1.47 2.60 18 2 -10 34.90 12.69 18 -2 -10 57.93 11.68 18 -2 -10 116.84 9.13 18 -2 -10 107.64 8.99 18 2 -9 -1.61 4.30 18 -2 -9 0.78 3.95 18 -2 -9 3.04 3.29 18 2 -8 28.40 5.31 18 -2 -8 32.55 4.24 18 -2 -8 22.50 4.41 18 2 -7 27.49 5.72 18 -2 -7 43.34 5.65 18 -2 -7 35.59 4.58 18 -2 -7 31.92 5.28 18 2 -6 15.22 3.09 18 2 -6 18.91 5.00 -18 -2 6 26.45 4.36 18 -2 -6 16.15 5.00 18 -2 -6 24.47 5.10 18 2 -5 11.01 4.68 18 2 -5 14.07 3.08 18 -2 -5 19.65 4.77 18 -2 -5 12.16 5.26 18 2 -4 8.90 4.17 18 2 -4 9.09 3.19 18 -2 -4 7.43 4.29 18 -2 -4 13.49 5.35 18 2 -3 16.84 3.72 18 -2 -3 17.12 4.36 18 -2 -3 25.26 5.74 -18 -2 3 20.81 4.38 18 2 -2 0.32 3.32 -18 -2 2 1.66 3.65 18 -2 -2 2.61 3.36 18 2 -1 32.66 4.32 18 -2 -1 18.01 3.83 -18 -2 1 35.49 4.47 18 -2 -1 35.30 5.97 18 2 0 20.25 3.89 18 -2 0 16.04 5.49 -18 -2 0 20.09 3.70 -18 -2 -1 32.99 4.04 18 -2 1 27.72 5.50 18 2 2 1.71 3.18 18 -2 2 0.75 4.17 -18 -2 -2 2.20 2.56 18 2 3 104.34 8.78 18 -2 3 88.04 9.10 -18 -2 -3 99.58 8.44 18 2 4 60.68 5.42 18 -2 4 47.16 5.72 18 2 5 13.19 2.40 18 -2 5 13.52 2.35 18 2 6 5.25 1.87 -18 2 -6 4.83 2.44 18 -2 6 3.52 1.66 -18 2 -7 6.76 2.19 18 4 -7 3.02 3.21 18 -4 -7 2.40 4.10 18 4 -6 4.58 3.20 -18 -4 6 5.30 2.70 18 -4 -6 5.71 4.76 18 4 -5 11.78 3.52 18 -4 -5 16.71 2.76 18 -4 -5 20.19 5.58 18 4 -4 2.77 2.00 18 -4 -4 1.48 2.51 18 -4 -4 1.83 5.46 -18 -4 4 4.41 2.93 18 4 -3 20.34 2.90 18 -4 -3 21.74 3.41 18 4 -2 13.46 2.71 18 -4 -2 17.19 5.79 18 -4 -2 17.23 3.27 18 4 -1 26.34 3.42 -18 -4 1 29.56 3.87 18 -4 -1 28.62 5.97 18 -4 -1 25.70 3.96 18 4 0 2.71 2.39 18 -4 0 -0.64 2.98 18 -4 0 3.43 4.78 -18 -4 0 0.16 2.77 18 4 1 76.41 6.87 18 -4 1 63.19 7.82 -18 -4 -1 82.68 6.93 18 -4 2 3.60 2.68 -18 -4 -2 2.78 2.21 18 -4 2 1.58 3.72 18 4 3 161.32 13.21 -18 -4 -3 166.51 13.13 18 -4 3 147.51 13.25 18 4 4 1.24 1.82 -18 -4 -4 0.04 1.41 18 -4 4 -0.79 1.93 19 1 -9 53.13 5.41 19 -1 -9 32.17 8.25 19 1 -8 23.97 4.42 19 -1 -8 30.68 4.44 19 1 -7 67.46 7.25 19 1 -7 49.00 12.07 19 -1 -7 64.36 6.95 19 1 -6 5.66 3.96 19 1 -6 4.18 2.87 19 -1 -6 2.70 3.93 19 -1 -6 3.34 3.93 19 1 -5 93.00 8.24 19 1 -5 67.17 8.42 19 1 -5 96.78 13.27 19 -1 -5 103.19 8.79 19 -1 -5 101.18 8.57 19 1 -4 16.88 3.84 19 1 -4 24.04 3.81 19 -1 -4 16.69 3.95 19 -1 -4 18.90 4.69 19 1 -3 3.25 3.50 19 -1 -3 1.06 4.34 19 -1 -3 1.64 3.07 19 1 -2 13.39 3.79 19 -1 -2 13.64 4.82 19 1 -1 15.42 4.02 -19 -1 1 16.96 3.62 19 -1 0 4.70 4.32 19 1 1 -0.65 3.24 19 -1 1 -1.18 3.96 19 1 2 61.68 6.00 19 -1 2 57.10 6.30 19 1 3 132.57 11.27 19 -1 3 130.65 11.38 19 1 4 25.87 3.27 19 -1 4 22.41 3.47 19 1 5 5.66 2.01 -19 1 -5 0.22 2.18 19 -1 5 4.13 1.70 19 3 -6 2.73 2.83 19 -3 -6 -0.23 4.01 19 3 -5 0.15 2.71 19 -3 -5 3.80 1.99 -19 -3 5 0.71 2.91 19 -3 -5 2.74 4.64 19 3 -4 26.07 3.38 19 -3 -4 31.05 5.58 19 -3 -4 30.05 3.43 19 3 -3 7.70 2.57 -19 -3 3 9.40 3.13 19 -3 -3 8.99 2.76 19 3 -2 16.98 3.06 -19 -3 2 22.11 3.45 19 -3 -2 18.35 3.29 19 3 -1 9.51 2.77 19 -3 -1 9.08 2.93 19 -3 -1 10.57 4.83 -19 -3 1 10.90 2.98 19 3 0 57.75 5.37 19 -3 0 50.48 6.56 -19 -3 0 59.31 5.40 19 -3 0 51.37 5.51 -19 -3 -1 15.11 2.67 19 -3 1 14.33 4.15 19 3 2 54.53 4.93 19 -3 2 44.99 5.60 -19 -3 -2 52.89 4.72 19 -3 2 48.76 4.96 19 3 3 23.10 2.75 19 -3 3 16.83 3.24 19 -3 3 20.51 2.77 20 0 -6 55.06 5.21 20 0 -6 48.07 5.16 20 0 -5 1.95 2.57 20 0 -5 -0.89 3.08 20 0 -4 4.98 2.38 20 0 -4 7.75 3.49 20 0 -3 1.65 3.46 20 0 -2 71.62 7.04 20 0 0 27.47 4.18 20 0 1 -0.79 3.05 20 0 2 82.86 7.48 20 2 -4 -0.95 2.37 20 -2 -4 2.67 3.91 20 -2 -4 3.21 1.90 20 2 -3 24.43 3.37 20 -2 -3 32.42 4.76 20 -2 -3 25.52 3.18 20 2 -2 35.25 3.99 20 -2 -2 31.84 3.71 20 2 -1 22.00 3.13 20 -2 -1 14.80 4.22 20 -2 -1 15.34 2.80 20 2 0 -0.81 2.51 20 -2 0 1.36 3.66 20 -2 0 -0.74 2.22 20 -2 1 20.24 3.71 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46683 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_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 S1 S 0.63774(7) 0.81492(14) 0.38756(8) 0.0113(6) Uani 1 1 d . U F6 F 0.5042(3) 0.6778(7) 0.3515(4) 0.0534(15) Uani 1 1 d . U F7 F 0.4982(3) 0.9207(7) 0.3413(4) 0.0520(14) Uani 1 1 d . U F18 F 0.5087(3) 0.8156(6) 0.4629(3) 0.0422(13) Uani 1 1 d . U O2 O 0.6517(2) 0.7895(5) 0.3022(3) 0.0169(10) Uani 1 1 d . U O3 O 0.6565(3) 0.9624(5) 0.4190(3) 0.0242(11) Uani 1 1 d . U O4 O 0.6641(3) 0.6959(5) 0.4443(3) 0.0233(11) Uani 1 1 d . U N5 N 0.6625(3) 0.7113(5) 0.6187(3) 0.0095(10) Uani 1 1 d . U H5 H 0.6730 0.7186 0.5677 0.011 Uiso 1 1 calc R U C9 C 0.6496(3) 0.5736(6) 0.6491(4) 0.0130(11) Uani 1 1 d . U C10 C 0.6599(3) 0.8398(6) 0.6645(4) 0.0130(11) Uani 1 1 d . U C11 C 0.5325(4) 0.8078(8) 0.3857(5) 0.0267(15) Uani 1 1 d . U C12 C 0.6407(4) 0.8266(7) 0.7448(4) 0.0183(13) Uani 1 1 d . U H12 H 0.6389 0.9118 0.7777 0.022 Uiso 1 1 calc R U C13 C 0.6311(4) 0.5608(7) 0.7304(4) 0.0190(13) Uani 1 1 d . U H13 H 0.6235 0.4669 0.7530 0.023 Uiso 1 1 calc R U C14 C 0.6238(4) 0.6875(7) 0.7781(4) 0.0222(14) Uani 1 1 d . U C15 C 0.6785(4) 0.9823(6) 0.6239(4) 0.0178(12) Uani 1 1 d . U H15A H 0.7307 0.9774 0.6069 0.021 Uiso 1 1 calc R U H15B H 0.6753 1.0632 0.6625 0.021 Uiso 1 1 calc R U H15C H 0.6417 0.9985 0.5759 0.021 Uiso 1 1 calc R U C16 C 0.6578(3) 0.4430(6) 0.5925(4) 0.0176(13) Uani 1 1 d . U H16A H 0.7060 0.4519 0.5669 0.021 Uiso 1 1 calc R U H16B H 0.6143 0.4413 0.5501 0.021 Uiso 1 1 calc R U H16C H 0.6585 0.3521 0.6243 0.021 Uiso 1 1 calc R U C17 C 0.6001(6) 0.6750(10) 0.8658(5) 0.0419(19) Uani 1 1 d . U H17A H 0.6184 0.7613 0.8974 0.050 Uiso 1 1 calc R U H17B H 0.6229 0.5865 0.8918 0.050 Uiso 1 1 calc R U H17C H 0.5439 0.6692 0.8639 0.050 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 S1 0.0067(7) 0.0064(8) 0.0219(8) 0.0022(5) 0.0064(5) 0.0006(4) F6 0.032(2) 0.067(3) 0.062(3) -0.022(2) 0.011(2) -0.031(2) F7 0.028(2) 0.071(3) 0.056(3) 0.003(2) 0.002(2) 0.031(2) F18 0.023(2) 0.060(3) 0.047(3) -0.005(2) 0.0215(19) 0.0013(18) O2 0.0146(19) 0.017(2) 0.021(2) -0.0009(16) 0.0100(15) -0.0001(15) O3 0.035(2) 0.007(2) 0.031(2) -0.0039(16) 0.0044(18) -0.0108(16) O4 0.029(2) 0.012(2) 0.030(2) 0.0096(16) 0.0094(18) 0.0088(16) N5 0.0095(18) 0.0037(18) 0.0161(19) -0.0001(14) 0.0053(15) 0.0009(14) C9 0.012(2) 0.008(2) 0.019(2) 0.0017(17) 0.0046(16) -0.0019(16) C10 0.011(2) 0.008(2) 0.021(2) -0.0012(17) 0.0064(17) 0.0022(16) C11 0.023(2) 0.030(3) 0.028(2) -0.004(2) 0.004(2) 0.000(2) C12 0.021(2) 0.013(2) 0.021(2) -0.0016(18) 0.0065(18) 0.0016(17) C13 0.022(2) 0.013(2) 0.023(2) 0.0025(18) 0.0068(18) -0.0020(18) C14 0.027(2) 0.015(2) 0.025(2) 0.0003(18) 0.005(2) -0.0004(18) C15 0.021(3) 0.007(2) 0.027(3) -0.001(2) 0.011(2) 0.002(2) C16 0.020(3) 0.005(2) 0.029(3) -0.003(2) 0.011(2) -0.008(2) C17 0.062(4) 0.034(4) 0.033(3) 0.000(3) 0.017(3) -0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.3331 0.5567 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0727 0.0534 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (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 O3 S1 O2 115.5(3) O3 S1 O4 114.1(3) O2 S1 O4 114.7(3) O3 S1 C11 103.1(3) O2 S1 C11 103.8(3) O4 S1 C11 103.6(3) C9 N5 C10 123.6(5) C9 N5 H5 118.2 C10 N5 H5 118.2 N5 C9 C13 118.7(5) N5 C9 C16 117.5(5) C13 C9 C16 123.8(5) N5 C10 C12 117.5(5) N5 C10 C15 117.6(5) C12 C10 C15 124.9(5) F7 C11 F18 107.4(6) F7 C11 F6 108.0(6) F18 C11 F6 106.9(6) F7 C11 S1 111.6(5) F18 C11 S1 112.0(5) F6 C11 S1 110.7(5) C10 C12 C14 121.1(6) C10 C12 H12 119.5 C14 C12 H12 119.5 C9 C13 C14 120.1(6) C9 C13 H13 120.0 C14 C13 H13 120.0 C13 C14 C12 119.0(6) C13 C14 C17 120.4(6) C12 C14 C17 120.6(6) C10 C15 H15A 109.5 C10 C15 H15B 109.5 H15A C15 H15B 109.5 C10 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C9 C16 H16A 109.5 C9 C16 H16B 109.5 H16A C16 H16B 109.5 C9 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C14 C17 H17A 109.5 C14 C17 H17B 109.5 H17A C17 H17B 109.5 C14 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O3 1.437(4) S1 O2 1.437(4) S1 O4 1.446(4) S1 C11 1.799(8) F6 C11 1.355(9) F7 C11 1.338(9) F18 C11 1.347(9) N5 C9 1.352(7) N5 C10 1.369(7) N5 H5 0.8600 C9 C13 1.382(8) C9 C16 1.496(8) C10 C12 1.371(9) C10 C15 1.482(8) C12 C14 1.396(9) C12 H12 0.9300 C13 C14 1.381(9) C13 H13 0.9300 C14 C17 1.512(10) C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N5 H5 O4 2.816(7) 0.860 1.990 160.7 no 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 C10 N5 C9 C13 1.4(8) C10 N5 C9 C16 -177.5(5) C9 N5 C10 C12 -2.0(8) C9 N5 C10 C15 177.5(5) O3 S1 C11 F7 55.3(6) O2 S1 C11 F7 -65.5(5) O4 S1 C11 F7 174.4(5) O3 S1 C11 F18 -65.1(5) O2 S1 C11 F18 174.1(5) O4 S1 C11 F18 54.0(5) O3 S1 C11 F6 175.6(5) O2 S1 C11 F6 54.9(6) O4 S1 C11 F6 -65.3(6) N5 C10 C12 C14 -0.6(9) C15 C10 C12 C14 179.9(6) N5 C9 C13 C14 1.9(9) C16 C9 C13 C14 -179.3(6) C9 C13 C14 C12 -4.3(10) C9 C13 C14 C17 177.3(7) C10 C12 C14 C13 3.7(10) C10 C12 C14 C17 -178.0(7)