#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:28:07 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227268 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035856.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_4035856 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 H14 F3 N O3 S Si' _chemical_formula_sum 'C9 H14 F3 N O3 S Si' _chemical_formula_weight 301.36 _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 direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 95.2270(6) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 8.71268(6) _cell_length_b 16.91650(12) _cell_length_c 9.27210(7) _cell_measurement_reflns_used 7806 _cell_measurement_temperature 93 _cell_measurement_theta_max 68.17 _cell_measurement_theta_min 4.77 _cell_volume 1360.914(17) _computing_cell_refinement 'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28c (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 93 _diffrn_detector_area_resol_mean 5.811 _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _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 0.0279 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10893 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.234 _diffrn_reflns_theta_min 5.229 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.333 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_correction_T_min 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 624.00 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.91 _refine_diff_density_min -0.46 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 166 _refine_ls_number_reflns 2435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0446 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.9171P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1201 _refine_ls_wR_factor_ref 0.1211 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2314 _reflns_number_total 2435 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file jo8b00675_si_001.cif _cod_data_source_block SX17024R _cod_database_code 4035856 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL SX17024R CELL 1.54184 8.71268 16.91650 9.27210 90.00000 95.22700 90.00000 ZERR 4 0.00006 0.00012 0.00007 0.00000 0.00060 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H N O F S SI UNIT 36 56 4 12 12 4 4 L.S. 10 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -180.0 ACTA SIZE 0.210 0.130 0.110 WGHT 0.064500 1.917100 FVAR 0.53524 S1 6 0.350941 0.385529 0.765589 11.00000 0.02373 0.02950 = 0.02566 -0.00005 0.00213 -0.00509 SI2 7 0.613834 0.729203 0.814913 11.00000 0.02147 0.01913 = 0.02389 0.00024 0.00348 0.00149 F3 5 0.413286 0.431594 0.506935 11.00000 0.06172 0.04990 = 0.03830 0.00456 0.02022 -0.01084 F4 5 0.184519 0.390060 0.517594 11.00000 0.04269 0.08831 = 0.03624 0.00801 -0.00940 -0.00950 F5 5 0.253622 0.504922 0.605203 11.00000 0.12578 0.03824 = 0.05699 0.01845 0.03146 0.03547 O6 4 0.207199 0.376162 0.827296 11.00000 0.02900 0.03696 = 0.03661 0.00713 0.01203 0.00733 O7 4 0.417436 0.311341 0.726011 11.00000 0.05058 0.05080 = 0.04947 0.01185 0.01884 0.02767 O8 4 0.456963 0.439197 0.837254 11.00000 0.08531 0.08148 = 0.04251 -0.00370 -0.00431 -0.05602 N9 3 0.748082 0.643634 0.822642 11.00000 0.01979 0.02239 = 0.02036 -0.00060 0.00202 0.00026 C10 1 0.698968 0.568842 0.837162 11.00000 0.02434 0.02386 = 0.02750 -0.00002 0.00321 -0.00037 AFIX 43 H10 2 0.593103 0.559391 0.847759 11.00000 -1.20000 AFIX 0 C11 1 0.899176 0.657338 0.809110 11.00000 0.02138 0.02926 = 0.02650 -0.00213 0.00229 -0.00308 AFIX 43 H11 2 0.933967 0.710121 0.799280 11.00000 -1.20000 AFIX 0 C12 1 0.799025 0.505591 0.836994 11.00000 0.03638 0.02247 = 0.03557 0.00180 0.00449 0.00457 AFIX 43 H12 2 0.762260 0.453166 0.846733 11.00000 -1.20000 AFIX 0 C13 1 1.002914 0.596335 0.809346 11.00000 0.01930 0.04328 = 0.03220 -0.00167 0.00135 0.00384 AFIX 43 H13 2 1.108702 0.606976 0.800478 11.00000 -1.20000 AFIX 0 C14 1 0.296214 0.430369 0.590099 11.00000 0.04542 0.02827 = 0.03051 0.00206 0.00911 0.00363 C15 1 0.627659 0.772684 0.633767 11.00000 0.03378 0.02421 = 0.02986 0.00269 0.00472 0.00448 AFIX 137 H15A 2 0.602850 0.732326 0.559458 11.00000 -1.20000 H15B 2 0.732680 0.792086 0.626629 11.00000 -1.20000 H15C 2 0.554780 0.816702 0.619128 11.00000 -1.20000 AFIX 0 C16 1 0.423240 0.686332 0.840333 11.00000 0.02219 0.02871 = 0.03734 0.00358 0.00542 0.00409 AFIX 137 H16A 2 0.395955 0.647420 0.763975 11.00000 -1.20000 H16B 2 0.345640 0.728416 0.835404 11.00000 -1.20000 H16C 2 0.426982 0.660409 0.935110 11.00000 -1.20000 AFIX 0 C17 1 0.952992 0.519278 0.822536 11.00000 0.03054 0.03383 = 0.03310 -0.00087 0.00232 0.01337 AFIX 43 H17 2 1.023526 0.476492 0.821656 11.00000 -1.20000 AFIX 0 C18 1 0.689241 0.797005 0.960471 11.00000 0.03705 0.02445 = 0.03216 -0.00407 0.00264 0.00122 AFIX 137 H18A 2 0.689998 0.770144 1.054178 11.00000 -1.20000 H18B 2 0.623338 0.843955 0.960359 11.00000 -1.20000 H18C 2 0.794424 0.812913 0.944156 11.00000 -1.20000 AFIX 0 HKLF 4 REM SX17024R REM R1 = 0.0446 for 2314 Fo > 4sig(Fo) and 0.0460 for all 2435 data REM 166 parameters refined using 0 restraints END WGHT 0.0640 1.9342 REM Instructions for potential hydrogen bonds HTAB C10 O8 EQIV $1 -x+3/2, y+1/2, -z+3/2 HTAB C11 O7_$1 REM Highest difference peak 0.905, deepest hole -0.457, 1-sigma level 0.068 Q1 1 0.3694 0.4798 0.8201 11.00000 0.05 0.91 Q2 1 0.1471 0.4771 0.5790 11.00000 0.05 0.83 Q3 1 0.4685 0.3590 0.7484 11.00000 0.05 0.75 Q4 1 0.3225 0.4030 0.6650 11.00000 0.05 0.44 Q5 1 0.6099 0.7448 0.7129 11.00000 0.05 0.43 Q6 1 0.6485 0.7580 0.9036 11.00000 0.05 0.39 Q7 1 0.2042 0.3405 0.5392 11.00000 0.05 0.33 Q8 1 0.3618 0.4778 0.5142 11.00000 0.05 0.29 Q9 1 0.6809 0.6780 0.8216 11.00000 0.05 0.28 Q10 1 0.5173 0.7007 0.8407 11.00000 0.05 0.25 Q11 1 0.3583 0.3172 0.7205 11.00000 0.05 0.23 Q12 1 0.1233 0.4225 0.5769 11.00000 0.05 0.21 Q13 1 0.2713 0.4015 0.8711 11.00000 0.05 0.21 Q14 1 0.4242 0.4400 0.7227 11.00000 0.05 0.20 Q15 1 0.1946 0.3888 0.7406 11.00000 0.05 0.20 Q16 1 0.6078 0.7619 0.5346 11.00000 0.05 0.18 Q17 1 0.3694 0.3160 0.7926 11.00000 0.05 0.18 Q18 1 0.7451 0.5341 0.8281 11.00000 0.05 0.18 Q19 1 0.8741 0.5196 0.8131 11.00000 0.05 0.18 Q20 1 0.7379 0.6219 0.8615 11.00000 0.05 0.17 Q21 1 0.7321 0.6175 0.8070 11.00000 0.05 0.17 Q22 1 0.7248 0.8407 0.9299 11.00000 0.05 0.17 Q23 1 0.2954 0.5069 0.7305 11.00000 0.05 0.17 Q24 1 0.4058 0.4176 0.6551 11.00000 0.05 0.16 Q25 1 0.7655 0.6412 0.9037 11.00000 0.05 0.16 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286.45 9.98 -7 7 5 264.78 9.35 -7 7 5 279.04 9.85 -7 -7 5 287.24 10.08 -7 -7 5 284.91 9.74 -7 7 4 25.54 2.34 -7 7 4 23.76 2.34 -7 7 4 23.87 2.19 -7 7 4 22.81 1.90 -7 -7 4 27.19 2.45 -7 -7 4 23.03 2.07 -7 -7 4 27.18 2.28 -7 7 3 265.55 9.69 -7 7 3 251.02 9.58 -7 7 3 255.08 9.04 -7 7 3 262.12 9.44 -7 -7 3 254.31 9.25 -7 -7 3 268.95 9.51 -7 -7 3 249.97 8.75 -7 7 2 85.16 4.49 -7 7 2 81.13 4.38 -7 7 2 81.64 4.30 -7 7 2 85.39 4.09 -7 -7 2 86.44 4.36 -7 -7 2 79.41 3.86 -7 7 1 397.56 13.23 -7 7 1 384.02 13.00 -7 7 1 384.91 12.68 -7 -7 1 385.97 13.00 -7 -7 1 375.99 12.59 -7 7 0 270.84 9.43 -7 7 0 257.31 9.52 -7 7 0 250.57 9.00 -7 7 0 262.43 9.33 -7 -7 0 242.52 9.21 -7 -7 0 237.50 8.95 -7 7 -1 42.33 2.75 -7 7 -1 45.46 3.11 -7 7 -1 46.41 3.00 -7 -7 -1 42.91 2.92 -7 -7 -1 44.73 3.03 -7 -7 -1 44.30 2.86 -7 7 -2 2.94 1.04 -7 7 -2 2.75 1.13 -7 7 -2 2.81 1.12 -7 -7 -2 3.47 1.18 -7 -7 -2 3.31 1.02 -7 7 -3 92.45 4.23 -7 7 -3 95.87 4.45 -7 7 -3 101.54 4.57 -7 -7 -3 98.75 4.76 -7 -7 -3 94.47 4.53 -7 -7 -3 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1.22 -8 8 -3 10.66 1.34 -8 -8 -3 9.56 1.16 -8 -8 -3 9.77 1.32 -8 8 -4 16.56 1.42 -8 8 -4 16.50 1.39 -8 8 -4 17.99 1.51 -8 -8 -4 15.84 1.48 -8 -8 -4 17.15 1.42 -8 9 6 0.28 0.54 -8 9 6 -0.08 0.45 -8 9 6 -0.24 0.44 -8 -9 6 0.26 0.49 -8 -9 6 -0.04 0.47 -8 -9 6 -0.13 0.46 -8 9 5 134.10 4.99 -8 9 5 132.94 5.08 -8 -9 5 129.99 5.07 -8 -9 5 129.73 5.02 -8 9 4 0.72 0.81 -8 9 4 0.30 0.52 -8 -9 4 0.19 0.72 -8 -9 4 0.46 0.85 -8 9 3 214.45 7.87 -8 9 3 202.43 7.26 -8 9 3 202.67 7.75 -8 9 3 211.81 7.67 -8 -9 3 224.84 7.77 -8 -9 3 217.65 7.62 -8 9 2 37.34 2.63 -8 9 2 39.00 2.34 -8 9 2 41.03 2.65 -8 -9 2 36.64 2.47 -8 -9 2 39.78 2.62 -8 -9 2 41.72 2.85 -8 9 1 348.28 11.46 -8 9 1 351.20 11.50 -8 9 1 327.24 11.06 -8 -9 1 351.07 11.75 -8 -9 1 336.78 11.38 -8 -9 1 335.76 11.08 -8 -9 1 334.25 11.33 -8 9 0 13.53 1.62 -8 9 0 12.10 1.56 -8 9 0 11.48 1.38 -8 9 0 11.80 1.35 -8 -9 0 10.54 1.43 -8 -9 0 11.78 1.56 -8 -9 0 11.16 1.35 -8 9 -1 61.25 3.17 -8 9 -1 71.73 3.67 -8 -9 -1 58.89 3.26 -8 -9 -1 61.72 3.31 -8 -9 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2.47 -9 -4 6 45.66 2.31 -9 4 5 30.78 2.09 -9 -4 5 26.57 1.87 -9 4 4 21.06 1.85 -9 4 4 19.67 1.82 -9 4 4 21.31 1.51 -9 -4 4 19.67 1.66 -9 -4 4 21.52 1.92 -9 4 3 3.72 0.87 -9 4 3 5.52 1.15 -9 4 3 4.90 1.13 -9 -4 3 5.85 1.18 -9 -4 3 2.99 0.91 -9 4 2 41.26 2.64 -9 4 2 37.77 2.49 -9 4 2 41.04 2.56 -9 4 2 42.13 2.39 -9 -4 2 40.24 2.69 -9 -4 2 43.81 2.57 -9 4 1 1.06 0.73 -9 4 1 0.86 0.72 -9 4 1 0.81 0.76 -9 -4 1 1.52 0.85 -9 -4 1 1.52 0.90 -9 4 0 20.91 1.64 -9 4 0 18.95 1.67 -9 -4 0 19.02 1.72 -9 -4 0 17.37 1.52 -9 4 -1 107.13 4.29 -9 -4 -1 104.32 4.45 -9 -4 -1 97.71 4.27 -9 4 -2 16.28 1.45 -9 4 -2 16.23 1.47 -9 -4 -2 16.75 1.52 -9 -4 -2 14.59 1.46 -9 4 -3 258.71 8.16 -9 4 -3 253.49 8.30 -9 -4 -3 233.08 8.12 -9 -4 -3 256.12 8.41 -9 4 -4 0.75 0.54 -9 4 -4 -0.14 0.50 -9 -4 -4 0.69 0.57 -9 5 5 41.20 2.00 -9 -5 5 42.90 2.44 -9 -5 5 41.00 2.28 -9 -5 5 38.84 2.04 -9 5 4 17.21 1.60 -9 5 4 15.00 1.32 -9 -5 4 14.30 1.29 -9 -5 4 15.55 1.46 -9 5 3 7.47 1.07 -9 5 3 6.04 1.14 -9 5 3 6.08 1.15 -9 -5 3 6.76 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-1 37.23 2.12 -9 -9 -1 35.84 2.01 -9 9 -2 3.38 0.73 -9 -9 -2 2.86 0.69 -9 -9 -2 2.39 0.60 -9 10 2 8.16 0.94 -9 10 2 9.19 0.96 -9 -10 2 7.92 1.01 -9 -10 2 7.87 0.95 -9 10 1 4.63 0.83 -9 10 1 5.53 0.89 -9 -10 1 5.34 0.87 -9 -10 1 5.41 0.85 -9 -10 1 4.98 0.75 -9 10 0 43.71 2.14 -9 -10 0 39.19 1.98 -10 0 4 0.36 0.49 -10 0 4 0.05 0.59 -10 0 3 0.29 0.51 -10 0 3 0.41 0.56 -10 1 4 80.00 3.29 -10 1 4 77.56 3.31 -10 -1 4 80.26 3.27 -10 -1 4 83.58 3.41 -10 1 3 7.80 0.94 -10 1 3 8.96 1.04 -10 -1 3 8.22 0.95 -10 -1 3 7.96 1.05 -10 -1 2 2.59 0.72 -10 2 4 68.06 2.98 -10 2 4 72.28 3.04 -10 -2 4 74.40 3.15 -10 2 3 166.49 5.64 -10 2 3 147.83 5.50 -10 -2 3 164.86 5.74 -10 2 2 55.51 2.57 -10 -2 2 57.26 2.69 -10 3 3 2.14 0.64 -10 3 3 1.43 0.47 -10 -3 3 1.62 0.64 -10 3 2 12.77 1.11 -10 -3 2 15.41 1.28 -10 -3 2 12.93 1.09 -10 -3 1 27.12 1.58 -10 4 3 11.32 1.04 -10 4 3 11.29 0.96 -10 -4 3 10.94 1.12 -10 4 2 79.07 3.19 -10 4 2 82.57 3.21 -10 -4 2 79.92 3.22 -10 -4 2 84.54 3.41 -10 -4 1 1.16 0.54 -10 -4 0 48.00 2.21 -10 -4 -1 19.10 1.19 -10 5 2 4.17 0.66 -10 5 2 4.71 0.69 -10 -5 2 4.92 0.74 -10 -5 2 5.14 0.77 -10 5 1 6.45 0.77 -10 -5 1 6.53 0.83 -10 5 0 8.22 0.77 -10 -5 0 7.17 0.84 -10 -5 -1 15.55 1.08 -10 -5 -1 16.78 1.07 -10 6 1 5.98 0.68 -10 -6 1 4.17 0.72 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 70463 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+X,-1/2-Y,-1/2+Z 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 0.35094(7) 0.38553(4) 0.76559(6) 0.02630(19) Uani 1 1 d . . Si2 Si 0.61383(7) 0.72920(4) 0.81491(7) 0.02141(19) Uani 1 1 d . . F3 F 0.4133(2) 0.43159(11) 0.50693(19) 0.0490(5) Uani 1 1 d . . F4 F 0.1845(2) 0.39006(13) 0.5176(2) 0.0565(5) Uani 1 1 d . . F5 F 0.2536(3) 0.50492(11) 0.6052(2) 0.0723(7) Uani 1 1 d . . O6 O 0.2072(2) 0.37616(11) 0.8273(2) 0.0336(4) Uani 1 1 d . . O7 O 0.4174(3) 0.31134(13) 0.7260(2) 0.0494(6) Uani 1 1 d . . O8 O 0.4570(3) 0.43920(17) 0.8373(3) 0.0704(9) Uani 1 1 d . . N9 N 0.7481(2) 0.64363(11) 0.8226(2) 0.0208(4) Uani 1 1 d . . C10 C 0.6990(3) 0.56884(14) 0.8372(3) 0.0252(5) Uani 1 1 d . . H10 H 0.5931 0.5594 0.8478 0.030 Uiso 1 1 calc R U C11 C 0.8992(3) 0.65734(15) 0.8091(3) 0.0257(5) Uani 1 1 d . . H11 H 0.9340 0.7101 0.7993 0.031 Uiso 1 1 calc R U C12 C 0.7990(3) 0.50559(15) 0.8370(3) 0.0314(6) Uani 1 1 d . . H12 H 0.7623 0.4532 0.8467 0.038 Uiso 1 1 calc R U C13 C 1.0029(3) 0.59633(17) 0.8093(3) 0.0317(6) Uani 1 1 d . . H13 H 1.1087 0.6070 0.8005 0.038 Uiso 1 1 calc R U C14 C 0.2962(3) 0.43037(16) 0.5901(3) 0.0344(6) Uani 1 1 d . . C15 C 0.6277(3) 0.77268(14) 0.6338(3) 0.0292(5) Uani 1 1 d . . H15A H 0.6029 0.7323 0.5595 0.035 Uiso 1 1 calc R U H15B H 0.7327 0.7921 0.6266 0.035 Uiso 1 1 calc R U H15C H 0.5548 0.8167 0.6191 0.035 Uiso 1 1 calc R U C16 C 0.4232(3) 0.68633(15) 0.8403(3) 0.0292(5) Uani 1 1 d . . H16A H 0.3960 0.6474 0.7640 0.035 Uiso 1 1 calc R U H16B H 0.3456 0.7284 0.8354 0.035 Uiso 1 1 calc R U H16C H 0.4270 0.6604 0.9351 0.035 Uiso 1 1 calc R U C17 C 0.9530(3) 0.51928(16) 0.8225(3) 0.0325(6) Uani 1 1 d . . H17 H 1.0235 0.4765 0.8217 0.039 Uiso 1 1 calc R U C18 C 0.6892(3) 0.79700(15) 0.9605(3) 0.0313(6) Uani 1 1 d . . H18A H 0.6900 0.7701 1.0542 0.038 Uiso 1 1 calc R U H18B H 0.6233 0.8440 0.9604 0.038 Uiso 1 1 calc R U H18C H 0.7944 0.8129 0.9442 0.038 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 0.0237(3) 0.0295(3) 0.0257(3) 0.0000(2) 0.0021(2) -0.0051(2) Si2 0.0215(3) 0.0191(3) 0.0239(3) 0.0002(2) 0.0035(2) 0.0015(2) F3 0.0617(11) 0.0499(11) 0.0383(9) 0.0046(8) 0.0202(8) -0.0108(9) F4 0.0427(10) 0.0883(15) 0.0362(10) 0.0080(9) -0.0094(8) -0.0095(10) F5 0.126(2) 0.0382(10) 0.0570(12) 0.0184(9) 0.0315(13) 0.0355(12) O6 0.0290(10) 0.0370(10) 0.0366(10) 0.0071(8) 0.0120(8) 0.0073(8) O7 0.0506(13) 0.0508(13) 0.0495(13) 0.0119(10) 0.0188(10) 0.0277(11) O8 0.0853(19) 0.0815(19) 0.0425(13) -0.0037(12) -0.0043(12) -0.0560(16) N9 0.0198(9) 0.0224(10) 0.0204(9) -0.0006(7) 0.0020(7) 0.0003(7) C10 0.0243(12) 0.0239(12) 0.0275(12) 0.0000(9) 0.0032(9) -0.0004(9) C11 0.0214(12) 0.0293(12) 0.0265(12) -0.0021(10) 0.0023(9) -0.0031(9) C12 0.0364(14) 0.0225(12) 0.0356(14) 0.0018(10) 0.0045(11) 0.0046(10) C13 0.0193(12) 0.0433(15) 0.0322(13) -0.0017(11) 0.0013(10) 0.0038(11) C14 0.0454(16) 0.0283(13) 0.0305(13) 0.0021(10) 0.0091(12) 0.0036(11) C15 0.0338(14) 0.0242(12) 0.0299(13) 0.0027(10) 0.0047(10) 0.0045(10) C16 0.0222(12) 0.0287(13) 0.0373(14) 0.0036(10) 0.0054(10) 0.0041(10) C17 0.0305(13) 0.0338(14) 0.0331(14) -0.0009(11) 0.0023(10) 0.0134(11) C18 0.0371(14) 0.0245(12) 0.0322(13) -0.0041(10) 0.0026(11) 0.0012(11) 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) ; O O 0.0492 0.0322 ; 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) ; S S 0.3331 0.5567 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.2541 0.3302 ; 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 O8 S1 O6 116.10(15) O8 S1 O7 114.63(18) O6 S1 O7 113.02(13) O8 S1 C14 105.00(15) O6 S1 C14 103.65(12) O7 S1 C14 102.34(13) C18 Si2 C16 114.52(12) C18 Si2 C15 111.65(12) C16 Si2 C15 113.97(12) C18 Si2 N9 105.96(10) C16 Si2 N9 105.03(10) C15 Si2 N9 104.61(10) C10 N9 C11 119.4(2) C10 N9 Si2 122.09(16) C11 N9 Si2 118.49(16) N9 C10 C12 121.5(2) N9 C10 H10 119.3 C12 C10 H10 119.3 N9 C11 C13 121.1(2) N9 C11 H11 119.4 C13 C11 H11 119.4 C17 C12 C10 119.3(2) C17 C12 H12 120.3 C10 C12 H12 120.3 C11 C13 C17 119.8(2) C11 C13 H13 120.1 C17 C13 H13 120.1 F4 C14 F5 110.2(3) F4 C14 F3 106.3(2) F5 C14 F3 106.4(2) F4 C14 S1 111.16(19) F5 C14 S1 110.8(2) F3 C14 S1 111.8(2) Si2 C15 H15A 109.5 Si2 C15 H15B 109.5 H15A C15 H15B 109.5 Si2 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 Si2 C16 H16A 109.5 Si2 C16 H16B 109.5 H16A C16 H16B 109.5 Si2 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C12 C17 C13 118.9(2) C12 C17 H17 120.6 C13 C17 H17 120.6 Si2 C18 H18A 109.5 Si2 C18 H18B 109.5 H18A C18 H18B 109.5 Si2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O8 1.417(2) S1 O6 1.4323(19) S1 O7 1.444(2) S1 C14 1.819(3) Si2 C18 1.846(3) Si2 C16 1.847(3) Si2 C15 1.848(3) Si2 N9 1.858(2) F3 C14 1.334(3) F4 C14 1.321(3) F5 C14 1.326(3) N9 C10 1.346(3) N9 C11 1.354(3) C10 C12 1.380(4) C10 H10 0.9500 C11 C13 1.372(4) C11 H11 0.9500 C12 C17 1.380(4) C12 H12 0.9500 C13 C17 1.383(4) C13 H13 0.9500 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17 0.9500 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 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 C18 Si2 N9 C10 124.38(19) C16 Si2 N9 C10 2.8(2) C15 Si2 N9 C10 -117.5(2) C18 Si2 N9 C11 -57.5(2) C16 Si2 N9 C11 -179.07(18) C15 Si2 N9 C11 60.62(19) C11 N9 C10 C12 -0.7(4) Si2 N9 C10 C12 177.40(19) C10 N9 C11 C13 0.3(3) Si2 N9 C11 C13 -177.91(19) N9 C10 C12 C17 0.4(4) N9 C11 C13 C17 0.5(4) O8 S1 C14 F4 -173.3(2) O6 S1 C14 F4 -51.1(2) O7 S1 C14 F4 66.6(2) O8 S1 C14 F5 -50.5(3) O6 S1 C14 F5 71.8(2) O7 S1 C14 F5 -170.5(2) O8 S1 C14 F3 68.0(2) O6 S1 C14 F3 -169.69(19) O7 S1 C14 F3 -52.0(2) C10 C12 C17 C13 0.3(4) C11 C13 C17 C12 -0.8(4)