#------------------------------------------------------------------------------ #$Date: 2020-04-30 01:08:11 +0300 (Thu, 30 Apr 2020) $ #$Revision: 251293 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126457.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_7126457 loop_ _publ_author_name 'Zeng, Hao' 'Zhu, Chuanle' 'Liu, Chi' 'Cai, Yingying' 'Chen, Fulin' 'Jiang, Huanfeng' _publ_section_title ; Three Component hydroxyletherification and hydroxylazidation of (Trifluoromethyl)alkenes: Access to \a-Trifluoromethyl \b-Heteroatom Substituted Tertiary Alcohols ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC02550J _journal_year 2020 _chemical_formula_moiety 'C15 H14 F3 N O2 S' _chemical_formula_sum 'C15 H14 F3 N O2 S' _chemical_formula_weight 329.33 _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 dual _atom_sites_solution_secondary difmap _audit_creation_date 2018-12-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-09-27 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 110.176(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 25.516(3) _cell_length_b 5.6738(5) _cell_length_c 21.937(2) _cell_measurement_reflns_used 1197 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.012 _cell_measurement_theta_min 3.022 _cell_volume 2981.0(5) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_unetI/netI 0.1074 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 10820 _diffrn_reflns_theta_full 25.93 _diffrn_reflns_theta_max 25.93 _diffrn_reflns_theta_min 3.02 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0944 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8634. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.337 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 201 _refine_ls_number_reflns 2829 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0621 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+7.0399P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1020 _refine_ls_wR_factor_ref 0.1313 _reflns_number_gt 1630 _reflns_number_total 2829 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL zz_a.res in C2/c REM Old TITL ZZ in C2/c REM SHELXT solution in C2/c REM R1 0.197, Rweak 0.014, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C15 N O5 S CELL 0.71073 25.5162 5.6738 21.9365 90 110.176 90 ZERR 8 0.0026 0.0005 0.0024 0 0.006 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O S UNIT 120 112 24 8 16 8 L.S. 4 PLAN 20 SIZE 0.12 0.06 0.03 TEMP -173.15 HTAB O2 N1 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.026800 7.039900 FVAR 0.33577 S1 6 0.394578 0.872492 0.229763 11.00000 0.02323 0.02930 = 0.02824 -0.00374 0.00692 -0.00436 F1 3 0.293969 0.690299 0.399690 11.00000 0.02256 0.04511 = 0.02722 0.00242 -0.00196 0.00850 O1 5 0.368181 0.390679 0.370980 11.00000 0.03652 0.02239 = 0.01673 0.00163 0.00238 0.00105 F2 3 0.315961 0.453526 0.481515 11.00000 0.02902 0.07536 = 0.04572 0.02257 0.00411 -0.01683 F3 3 0.318199 0.827789 0.496294 11.00000 0.03462 0.09300 = 0.03722 -0.02242 0.00703 0.02444 O2 5 0.396817 0.874208 0.431885 11.00000 0.05152 0.01970 = 0.02090 0.00550 0.00679 -0.00345 AFIX 147 H2 2 0.388329 0.845812 0.392059 11.00000 -1.50000 AFIX 0 N1 4 0.373362 0.557672 0.325432 11.00000 0.02587 0.02502 = 0.02279 0.00287 0.00999 0.00429 C5 1 0.338749 0.511518 0.267697 11.00000 0.01927 0.02642 = 0.01800 -0.00370 0.00644 0.00236 C13 1 0.503001 0.710488 0.663684 11.00000 0.01918 0.02625 = 0.01615 -0.00067 0.00162 0.00105 AFIX 43 H13 2 0.528087 0.720475 0.707194 11.00000 -1.20000 AFIX 0 C4 1 0.341354 0.667436 0.216005 11.00000 0.01595 0.02116 = 0.02429 -0.00296 0.00878 -0.00008 C11 1 0.464233 0.875153 0.556641 11.00000 0.02265 0.01812 = 0.01866 -0.00026 0.00718 0.00280 AFIX 43 H11 2 0.463138 0.998755 0.527012 11.00000 -1.20000 AFIX 0 C10 1 0.429406 0.681926 0.535743 11.00000 0.02147 0.02131 = 0.02209 -0.00394 0.01036 0.00231 C12 1 0.500756 0.890470 0.620408 11.00000 0.02077 0.01600 = 0.03115 -0.00581 0.01136 -0.00329 AFIX 43 H12 2 0.524154 1.024588 0.634217 11.00000 -1.20000 AFIX 0 C8 1 0.390643 0.664848 0.464846 11.00000 0.02383 0.02033 = 0.01817 0.00186 0.00572 0.00071 C15 1 0.431731 0.501114 0.579975 11.00000 0.02362 0.01915 = 0.02477 -0.00251 0.00727 -0.00475 AFIX 43 H15 2 0.407977 0.367898 0.566489 11.00000 -1.20000 AFIX 0 C14 1 0.468658 0.515442 0.643609 11.00000 0.02621 0.01804 = 0.02428 0.00415 0.00971 0.00194 AFIX 43 H14 2 0.470329 0.391425 0.673318 11.00000 -1.20000 AFIX 0 C3 1 0.304972 0.681225 0.153502 11.00000 0.02315 0.03350 = 0.02135 -0.00119 0.00817 -0.00345 AFIX 43 H3 2 0.273150 0.582572 0.136571 11.00000 -1.20000 AFIX 0 C6 1 0.297195 0.313534 0.252929 11.00000 0.03103 0.03009 = 0.02004 -0.00351 0.00843 -0.00565 AFIX 137 H6A 2 0.315875 0.168628 0.273659 11.00000 -1.50000 H6B 2 0.281322 0.290094 0.205834 11.00000 -1.50000 H6C 2 0.267265 0.352646 0.269656 11.00000 -1.50000 AFIX 0 C2 1 0.319599 0.857603 0.116623 11.00000 0.02390 0.04144 = 0.02228 0.00097 0.00956 -0.00067 AFIX 43 H2A 2 0.298652 0.890406 0.072435 11.00000 -1.20000 AFIX 0 C7 1 0.406159 0.446429 0.434178 11.00000 0.03483 0.02174 = 0.01751 -0.00154 0.00471 0.00440 AFIX 23 H7A 2 0.443726 0.470292 0.431465 11.00000 -1.20000 H7B 2 0.408416 0.309960 0.463097 11.00000 -1.20000 AFIX 0 C9 1 0.329856 0.660766 0.460258 11.00000 0.02860 0.04415 = 0.02510 0.00031 0.00397 0.00496 C1 1 0.366776 0.974491 0.151304 11.00000 0.02685 0.03085 = 0.03021 0.00327 0.01527 -0.00271 AFIX 43 H1 2 0.382652 1.098389 0.134262 11.00000 -1.20000 HKLF 4 REM zz_a.res in C2/c REM R1 = 0.0621 for 1630 Fo > 4sig(Fo) and 0.1356 for all 2829 data REM 201 parameters refined using 0 restraints END WGHT 0.0263 7.0980 REM Highest difference peak 0.337, deepest hole -0.344, 1-sigma level 0.079 Q1 1 0.3560 0.2983 0.4888 11.00000 0.05 0.34 Q2 1 0.3465 0.5578 0.2283 11.00000 0.05 0.29 Q3 1 0.5000 0.9118 0.7500 10.50000 0.05 0.29 Q4 1 0.3608 0.4164 0.4584 11.00000 0.05 0.28 Q5 1 0.5619 0.7670 0.7172 11.00000 0.05 0.28 Q6 1 0.3185 0.2751 0.3115 11.00000 0.05 0.27 Q7 1 0.3735 0.6668 0.3213 11.00000 0.05 0.27 Q8 1 0.3470 0.8562 0.4398 11.00000 0.05 0.27 Q9 1 0.3609 0.9372 0.3661 11.00000 0.05 0.26 Q10 1 0.4738 0.4476 0.5205 11.00000 0.05 0.26 Q11 1 0.3162 1.0083 0.3710 11.00000 0.05 0.26 Q12 1 0.3490 1.3507 0.1609 11.00000 0.05 0.26 Q13 1 0.3522 0.5111 0.1268 11.00000 0.05 0.26 Q14 1 0.5590 0.6308 0.7486 11.00000 0.05 0.26 Q15 1 0.3014 0.6822 0.3617 11.00000 0.05 0.25 Q16 1 0.4016 1.1525 0.1381 11.00000 0.05 0.25 Q17 1 0.2521 0.6524 0.1687 11.00000 0.05 0.24 Q18 1 0.2874 0.6925 0.5304 11.00000 0.05 0.24 Q19 1 0.3526 0.2614 0.4401 11.00000 0.05 0.24 Q20 1 0.2879 0.2847 0.2875 11.00000 0.05 0.24 REM The information below was added by Olex2. REM REM R1 = 0.0621 for 1630 Fo > 4sig(Fo) and 0.1356 for all 11471 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.34 REM Mean Shift 0, Max Shift -0.005. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1356 REM R1_gt = 0.0621 REM wR_ref = 0.1313 REM GOOF = 1.026 REM Shift_max = -0.005 REM Shift_mean = 0 REM Reflections_all = 11471 REM Reflections_gt = 1630 REM Parameters = n/a REM Hole = -0.34 REM Peak = 0.34 REM Flack = n/a ; _cod_data_source_file d0cc02550j2.cif _cod_data_source_block zz _cod_database_code 7126457 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 2.b Aromatic/amide H refined with riding coordinates: C13(H13), C11(H11), C12(H12), C15(H15), C14(H14), C3(H3), C2(H2A), C1(H1) 2.c Idealised Me refined as rotating group: C6(H6A,H6B,H6C) 2.d Idealised tetrahedral OH refined as rotating group: O2(H2) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 '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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn S1 S 0.39458(5) 0.87249(19) 0.22976(5) 0.0274(3) Uani 1 d . . . F1 F 0.29397(10) 0.6903(4) 0.39969(10) 0.0344(6) Uani 1 d . . . O1 O 0.36818(12) 0.3907(5) 0.37098(11) 0.0270(7) Uani 1 d . . . F2 F 0.31596(11) 0.4535(5) 0.48151(12) 0.0523(8) Uani 1 d . . . F3 F 0.31820(11) 0.8278(5) 0.49629(12) 0.0563(9) Uani 1 d . . . O2 O 0.39682(13) 0.8742(5) 0.43189(12) 0.0322(8) Uani 1 d . . . H2 H 0.3883 0.8458 0.3921 0.048 Uiso 1 calc . . GR N1 N 0.37336(14) 0.5577(6) 0.32543(15) 0.0241(8) Uani 1 d . . . C5 C 0.33875(17) 0.5115(7) 0.26770(17) 0.0212(9) Uani 1 d . . . C13 C 0.50300(17) 0.7105(7) 0.66368(18) 0.0217(9) Uani 1 d . . . H13 H 0.5281 0.7205 0.7072 0.026 Uiso 1 calc . . R C4 C 0.34135(16) 0.6674(7) 0.21601(17) 0.0200(9) Uani 1 d . . . C11 C 0.46423(16) 0.8752(7) 0.55664(17) 0.0198(9) Uani 1 d . . . H11 H 0.4631 0.9988 0.5270 0.024 Uiso 1 calc . . R C10 C 0.42941(17) 0.6819(7) 0.53574(17) 0.0209(9) Uani 1 d . . . C12 C 0.50076(16) 0.8905(7) 0.62041(18) 0.0220(9) Uani 1 d . . . H12 H 0.5242 1.0246 0.6342 0.026 Uiso 1 calc . . R C8 C 0.39064(17) 0.6648(7) 0.46485(17) 0.0212(9) Uani 1 d . . . C15 C 0.43173(17) 0.5011(7) 0.57998(17) 0.0228(9) Uani 1 d . . . H15 H 0.4080 0.3679 0.5665 0.027 Uiso 1 calc . . R C14 C 0.46866(17) 0.5154(7) 0.64361(18) 0.0226(9) Uani 1 d . . . H14 H 0.4703 0.3914 0.6733 0.027 Uiso 1 calc . . R C3 C 0.30497(17) 0.6812(7) 0.15350(18) 0.0259(10) Uani 1 d . . . H3 H 0.2732 0.5826 0.1366 0.031 Uiso 1 calc . . R C6 C 0.29720(17) 0.3135(7) 0.25293(18) 0.0271(10) Uani 1 d . . . H6A H 0.3159 0.1686 0.2737 0.041 Uiso 1 calc . . GR H6B H 0.2813 0.2901 0.2058 0.041 Uiso 1 calc . . GR H6C H 0.2673 0.3526 0.2697 0.041 Uiso 1 calc . . GR C2 C 0.31960(18) 0.8576(8) 0.11662(19) 0.0288(10) Uani 1 d . . . H2A H 0.2987 0.8904 0.0724 0.035 Uiso 1 calc . . R C7 C 0.40616(18) 0.4464(7) 0.43418(17) 0.0258(10) Uani 1 d . . . H7A H 0.4437 0.4703 0.4315 0.031 Uiso 1 calc . . R H7B H 0.4084 0.3100 0.4631 0.031 Uiso 1 calc . . R C9 C 0.32986(19) 0.6608(8) 0.4603(2) 0.0340(11) Uani 1 d . . . C1 C 0.36678(18) 0.9745(7) 0.15130(19) 0.0279(10) Uani 1 d . . . H1 H 0.3827 1.0984 0.1343 0.033 Uiso 1 calc . . R 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 0.0232(6) 0.0293(6) 0.0282(6) -0.0037(5) 0.0069(5) -0.0044(5) F1 0.0226(15) 0.0451(17) 0.0272(13) 0.0024(11) -0.0020(11) 0.0085(12) O1 0.0365(19) 0.0224(16) 0.0167(14) 0.0016(12) 0.0024(13) 0.0010(13) F2 0.0290(17) 0.075(2) 0.0457(16) 0.0226(15) 0.0041(14) -0.0168(15) F3 0.0346(18) 0.093(2) 0.0372(15) -0.0224(15) 0.0070(13) 0.0244(16) O2 0.052(2) 0.0197(16) 0.0209(15) 0.0055(12) 0.0068(15) -0.0034(15) N1 0.026(2) 0.025(2) 0.0228(19) 0.0029(14) 0.0100(17) 0.0043(15) C5 0.019(2) 0.026(2) 0.018(2) -0.0037(17) 0.0064(19) 0.0024(19) C13 0.019(2) 0.026(2) 0.016(2) -0.0007(17) 0.0016(18) 0.0011(19) C4 0.016(2) 0.021(2) 0.024(2) -0.0030(17) 0.0088(18) -0.0001(18) C11 0.023(2) 0.018(2) 0.019(2) -0.0003(17) 0.0072(18) 0.0028(18) C10 0.021(2) 0.021(2) 0.022(2) -0.0039(17) 0.0104(19) 0.0023(18) C12 0.021(2) 0.016(2) 0.031(2) -0.0058(18) 0.011(2) -0.0033(18) C8 0.024(3) 0.020(2) 0.018(2) 0.0019(16) 0.0057(18) 0.0007(18) C15 0.024(3) 0.019(2) 0.025(2) -0.0025(17) 0.0073(19) -0.0047(18) C14 0.026(3) 0.018(2) 0.024(2) 0.0041(17) 0.010(2) 0.0019(19) C3 0.023(3) 0.034(3) 0.021(2) -0.0012(18) 0.0082(19) -0.003(2) C6 0.031(3) 0.030(3) 0.020(2) -0.0035(18) 0.008(2) -0.006(2) C2 0.024(3) 0.041(3) 0.022(2) 0.001(2) 0.010(2) -0.001(2) C7 0.035(3) 0.022(2) 0.018(2) -0.0015(17) 0.005(2) 0.0044(19) C9 0.029(3) 0.044(3) 0.025(2) 0.000(2) 0.004(2) 0.005(2) C1 0.027(3) 0.031(3) 0.030(2) 0.003(2) 0.015(2) -0.003(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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 C1 S1 C4 91.4(2) . . ? N1 O1 C7 109.9(3) . . ? C8 O2 H2 109.5 . . ? C5 N1 O1 110.9(3) . . ? N1 C5 C4 116.0(4) . . ? N1 C5 C6 123.7(3) . . ? C4 C5 C6 120.3(3) . . ? C12 C13 H13 120.0 . . ? C12 C13 C14 120.0(4) . . ? C14 C13 H13 120.0 . . ? C5 C4 S1 121.0(3) . . ? C3 C4 S1 110.9(3) . . ? C3 C4 C5 128.1(4) . . ? C10 C11 H11 119.6 . . ? C10 C11 C12 120.9(4) . . ? C12 C11 H11 119.6 . . ? C11 C10 C8 120.1(3) . . ? C11 C10 C15 118.8(4) . . ? C15 C10 C8 121.1(3) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O2 C8 C10 108.4(3) . . ? O2 C8 C7 111.2(3) . . ? O2 C8 C9 105.5(3) . . ? C7 C8 C10 108.9(3) . . ? C9 C8 C10 110.8(3) . . ? C9 C8 C7 111.9(3) . . ? C10 C15 H15 119.8 . . ? C14 C15 C10 120.3(4) . . ? C14 C15 H15 119.8 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C4 C3 H3 123.5 . . ? C4 C3 C2 113.1(4) . . ? C2 C3 H3 123.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C2 H2A 123.7 . . ? C1 C2 C3 112.5(4) . . ? C1 C2 H2A 123.7 . . ? O1 C7 C8 114.6(3) . . ? O1 C7 H7A 108.6 . . ? O1 C7 H7B 108.6 . . ? C8 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? F1 C9 F2 106.2(4) . . ? F1 C9 C8 113.4(3) . . ? F2 C9 C8 111.9(4) . . ? F3 C9 F1 106.5(3) . . ? F3 C9 F2 105.9(3) . . ? F3 C9 C8 112.4(4) . . ? S1 C1 H1 123.9 . . ? C2 C1 S1 112.2(3) . . ? C2 C1 H1 123.9 . . ? 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 S1 C4 1.734(4) . ? S1 C1 1.720(4) . ? F1 C9 1.339(5) . ? O1 N1 1.416(4) . ? O1 C7 1.426(4) . ? F2 C9 1.356(5) . ? F3 C9 1.332(5) . ? O2 H2 0.8400 . ? O2 C8 1.427(4) . ? N1 C5 1.297(5) . ? C5 C4 1.458(5) . ? C5 C6 1.501(5) . ? C13 H13 0.9500 . ? C13 C12 1.382(5) . ? C13 C14 1.386(5) . ? C4 C3 1.367(5) . ? C11 H11 0.9500 . ? C11 C10 1.386(5) . ? C11 C12 1.391(5) . ? C10 C8 1.531(5) . ? C10 C15 1.399(5) . ? C12 H12 0.9500 . ? C8 C7 1.526(5) . ? C8 C9 1.519(6) . ? C15 H15 0.9500 . ? C15 C14 1.391(5) . ? C14 H14 0.9500 . ? C3 H3 0.9500 . ? C3 C2 1.415(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C2 H2A 0.9500 . ? C2 C1 1.355(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C1 H1 0.9500 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 N1 0.84 2.14 2.841(4) 141.2 . loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 -1 0 934.41 29.5 -2 -2 0 784.42 38.6 3 3 0 62.49 16.7 -3 -3 0 97.79 19.5 -4 -4 0 617.04 43.4 -5 -5 0 42.5 17.5 -5 -5 0 65.29 17.2 6 6 0 0 16.6 8 6 -1 23.9 21.8 -7 -5 1 11.7 15 7 5 -1 19.3 14.9 -6 -4 1 6.3 10 6 4 -1 11.9 10.2 -5 -3 1 639.14 44.4 5 3 -1 658.23 45.4 -4 -2 1 1324.37 55.79 4 2 -1 1386.66 57.09 -3 -1 1 5640.04 92.29 3 1 -1 5716.53 94.79 -1 1 1 272.77 15.4 1 -1 -1 281.87 14.5 1 -1 -1 288.47 15.1 0 -2 -1 806.02 33.9 0 -2 -1 831.62 34.3 -1 -3 -1 7.4 7.1 -1 -3 -1 3.2 5.3 -2 -4 -1 42.2 13.9 -2 -4 -1 32 11.9 3 5 1 28 15.3 -10 -6 2 -38.2 16.2 -9 -5 2 64.69 20.9 9 5 -2 61.29 22.4 -8 -4 2 9 13.8 8 4 -2 3.5 14.5 -7 -3 2 349.47 36.4 7 3 -2 364.26 38.2 -6 -2 2 342.87 32.5 6 2 -2 390.86 35.3 -5 -1 2 7826.22 131.19 5 1 -2 7741.33 132.69 -4 0 2 111.99 14 4 0 -2 115.19 15.9 4 0 -2 116.99 14.3 -3 1 2 13.6 7.3 -3 1 2 15.6 6.2 3 -1 -2 18.4 7.5 3 -1 -2 16.2 6.2 2 -2 -2 -0.8 3 2 -2 -2 3.9 4.7 1 -3 -2 126.49 20.5 1 -3 -2 136.39 16.1 0 4 2 13.4 7 0 -4 -2 2.5 7.2 1 5 2 -4 10.6 -12 -6 3 117.09 34.5 12 6 -3 1.6 29.9 -11 -5 3 -18.1 14.3 11 5 -3 -37.2 15.4 -10 -4 3 197.28 38.3 10 4 -3 151.38 35.5 -9 -3 3 554.74 47.9 9 3 -3 548.15 51.99 -8 -2 3 9.6 11.4 8 2 -3 41.2 15.1 -7 -1 3 3299.87 98.19 7 1 -3 3093.59 96.79 -6 0 3 0 4.5 6 0 -3 0.5 4.9 6 0 -3 -5.4 4 -5 1 3 4476.95 90.89 -5 1 3 4515.05 104.99 5 -1 -3 4494.45 100.59 5 -1 -3 4360.76 91.79 -4 2 3 354.46 27.3 -4 2 3 400.26 30.1 4 -2 -3 346.37 25.9 4 -2 -3 359.76 25.6 3 -3 -3 6.7 5.1 3 -3 -3 -3 7 -2 4 3 898.41 49.99 2 -4 -3 837.92 42 2 -4 -3 934.01 47.8 -14 -6 4 15.3 24.7 14 6 -4 18.2 27.4 -13 -5 4 6.1 18.6 13 5 -4 -16.3 19.9 -12 -4 4 1.1 15.9 12 4 -4 28.6 19.9 -11 -3 4 211.28 39.7 11 3 -4 203.78 41.2 -10 -2 4 102.29 25.1 10 2 -4 111.09 27.9 -9 -1 4 934.31 58.59 9 1 -4 1042.3 62.89 -8 0 4 7919.21 152.88 8 0 -4 8104.09 175.18 8 0 -4 8228.18 161.28 -7 1 4 3721.63 96.59 -7 1 4 3942.21 116.49 7 -1 -4 3829.12 109.29 7 -1 -4 3853.41 101.39 -6 2 4 246.18 26.5 -6 2 4 272.97 30.5 6 -2 -4 228.78 24.1 6 -2 -4 250.07 26.4 -5 3 4 322.77 32.4 -5 3 4 257.27 29.8 5 -3 -4 259.17 30.8 5 -3 -4 298.07 28.6 4 -4 -4 31 12.9 4 -4 -4 18.3 6.7 -3 5 4 264.87 35.3 -15 -5 5 46.1 27.9 15 5 -5 0.6 26.1 -14 -4 5 96.79 25.7 14 4 -5 116.39 26.4 -13 -3 5 90.19 26.8 13 3 -5 91.69 30.5 -12 -2 5 14.8 15.7 12 2 -5 12 10.4 -11 -1 5 1406.26 79.39 11 1 -5 1348.37 87.49 11 1 -5 1476.95 82.79 -10 0 5 19 8.6 10 0 -5 9.1 9.9 10 0 -5 5.3 6.5 -9 1 5 1076.59 69.49 -9 1 5 1044.9 58.69 9 -1 -5 1100.39 62.89 9 -1 -5 1051.09 65.89 -8 2 5 719.73 54.99 8 -2 -5 658.93 47.8 -7 3 5 28.4 14.6 -7 3 5 24.5 12 7 -3 -5 16.7 10.6 7 -3 -5 20 8 -6 4 5 59.59 20.6 6 -4 -5 50.99 14.8 6 -4 -5 47.8 14.3 -5 5 5 442.66 44 -17 -5 6 59.09 26.6 17 5 -6 -15.2 29.9 -16 -4 6 -5.5 19.2 16 4 -6 31.3 27.4 -15 -3 6 392.16 53.59 15 3 -6 432.56 56.59 -14 -2 6 3.3 10 14 2 -6 34.8 13.1 -13 -1 6 7.9 12.4 13 1 -6 12.5 9.8 13 1 -6 18.4 14.9 -12 0 6 753.02 69.09 12 0 -6 651.33 85.29 12 0 -6 654.13 61.29 -11 1 6 718.73 54.09 11 -1 -6 755.22 60.69 11 -1 -6 818.32 60.19 -10 2 6 20.4 10.4 -10 2 6 4.9 10.9 10 -2 -6 16.7 10.1 10 -2 -6 -10.8 6.9 -9 3 6 125.19 27.7 -9 3 6 114.09 32 9 -3 -6 170.08 31.4 9 -3 -6 130.09 29.1 -8 4 6 483.85 47.5 -8 4 6 416.66 47.8 8 -4 -6 447.16 41.3 8 -4 -6 427.56 39.8 7 -5 -6 54.69 13.9 7 -5 -6 43.3 17.4 -19 -5 7 -24.1 30.6 19 5 -7 2.6 37.6 -18 -4 7 -14.7 22.8 18 4 -7 44.7 21.3 -17 -3 7 254.57 49.8 17 3 -7 97.79 43.8 17 3 -7 225.58 50.79 -16 -2 7 147.09 39.7 16 2 -7 69.29 27.4 16 2 -7 73.19 36.3 -15 -1 7 49.99 20.1 15 1 -7 44.1 15.3 15 1 -7 46.6 11.1 -14 0 7 7.7 10.3 -13 1 7 491.65 49.7 13 -1 -7 535.45 53.79 13 -1 -7 503.75 53.89 -12 2 7 42.1 17.7 -12 2 7 68.49 22.5 12 -2 -7 59.09 21.2 12 -2 -7 67.99 24.1 -11 3 7 234.98 42.6 -11 3 7 232.98 46.8 11 -3 -7 228.88 42.9 11 -3 -7 284.17 37.9 -10 4 7 27 18.6 -10 4 7 75.99 27.9 10 -4 -7 54.79 20.5 10 -4 -7 57.59 21.6 -9 5 7 0.9 14.3 9 -5 -7 33.1 12.9 9 -5 -7 18.5 13.2 -21 -5 8 13 34.6 21 5 -8 -33.5 33.8 -20 -4 8 17 25.7 20 4 -8 9.3 26.6 -19 -3 8 15.9 21.7 19 3 -8 -14.7 15.4 -18 -2 8 159.38 41 18 2 -8 159.98 41.6 18 2 -8 98.89 41.7 -17 -1 8 11.7 10 17 1 -8 2.8 15 17 1 -8 -10.1 9.5 -16 0 8 331.77 55.59 16 0 -8 279.77 51.39 16 0 -8 388.06 65.69 -15 1 8 138.29 37.2 15 -1 -8 132.49 34.9 15 -1 -8 98.79 35.6 -14 2 8 583.94 56.99 14 -2 -8 620.54 60.49 14 -2 -8 698.03 66.29 -13 3 8 242.78 46.5 -13 3 8 353.56 63.99 13 -3 -8 295.57 49.7 13 -3 -8 292.97 48.5 -12 4 8 392.26 65.09 12 -4 -8 314.97 51.59 12 -4 -8 365.26 40.9 -11 5 8 19.6 22.9 11 -5 -8 68.09 22 11 -5 -8 38.5 17.7 -22 -4 9 -3.7 41.8 22 4 -9 -39.1 30.4 -21 -3 9 -19.8 26.4 21 3 -9 8 22.3 -20 -2 9 -45.8 18.4 20 2 -9 15.3 15.9 20 2 -9 -36.1 26 -19 -1 9 78.79 31.1 19 1 -9 101.89 43.2 19 1 -9 62.39 29 -18 0 9 0.2 15.1 18 0 -9 -7 14.8 18 0 -9 7.3 19.6 -17 1 9 173.38 37.8 17 -1 -9 209.48 47.2 17 -1 -9 168.58 41.1 -16 2 9 14.2 13.5 16 -2 -9 16.2 18.1 16 -2 -9 43.6 22.8 -15 3 9 273.87 62.49 15 -3 -9 286.87 50.39 15 -3 -9 402.56 49.9 -14 4 9 -18.6 19 14 -4 -9 23.5 19.2 14 -4 -9 12.1 13 13 -5 -9 14.2 21.4 13 -5 -9 54.09 19.9 12 -6 -9 130.59 33.6 -24 -4 10 80.49 57.69 24 4 -10 71.49 48.6 -23 -3 10 39.2 41.2 23 3 -10 42.4 35.8 -22 -2 10 -7.2 29.6 22 2 -10 -26.3 24.9 -21 -1 10 178.78 47.3 21 1 -10 228.48 54.69 21 1 -10 66.49 42.9 -20 0 10 351.56 66.29 20 0 -10 230.28 55.79 20 0 -10 374.66 69.79 19 -1 -10 29.5 24.6 19 -1 -10 57.49 27.4 -18 2 10 234.78 50.59 18 -2 -10 169.58 40.4 18 -2 -10 201.38 46.4 -17 3 10 827.92 78.39 17 -3 -10 981.7 87.59 17 -3 -10 672.53 108.89 16 -4 -10 204.38 45.7 16 -4 -10 243.48 49.7 15 -5 -10 118.69 28.7 15 -5 -10 94.89 31.4 14 -6 -10 6.3 24.1 -25 -3 11 -12.6 46.9 -24 -2 11 51.29 39.8 24 2 -11 0.9 17.3 -23 -1 11 7.4 28.6 23 1 -11 5.1 20.8 -22 0 11 36.4 28.8 22 0 -11 38.4 22.8 22 0 -11 2.4 25.4 -21 1 11 121.19 41 21 -1 -11 71.59 57.79 21 -1 -11 135.39 43.1 20 -2 -11 1199.38 105.19 20 -2 -11 1160.08 101.09 19 -3 -11 132.89 35.4 19 -3 -11 146.99 42.8 18 -4 -11 324.07 63.39 18 -4 -11 257.77 58.49 17 -5 -11 150.98 41.2 17 -5 -11 120.99 36.3 27 3 -12 11.7 36.1 26 2 -12 95.79 51.19 25 1 -12 8.3 19.9 24 0 -12 180.08 55.99 24 0 -12 71.49 31.3 23 -1 -12 5.2 13.3 22 -2 -12 124.59 41.1 22 -2 -12 119.79 45.8 21 -3 -12 256.07 59.79 21 -3 -12 173.98 42.4 20 -4 -12 151.38 45.5 20 -4 -12 170.38 34.5 19 -5 -12 -12.1 32.1 19 -5 -12 0.5 28.2 28 2 -13 23 35.5 27 1 -13 81.99 38.1 26 0 -13 19.2 24.7 25 -1 -13 107.59 44.5 25 -1 -13 36.8 30.6 24 -2 -13 19.5 17.9 24 -2 -13 -47.2 31.2 23 -3 -13 175.68 45.9 22 -4 -13 -44.6 25.9 22 -4 -13 -6.4 23.3 29 1 -14 111.69 48.3 28 0 -14 69.09 39.6 27 -1 -14 -0.1 25.7 26 -2 -14 5.2 19.9 26 -2 -14 25.7 41.9 25 -3 -14 -76.19 61.19 25 -3 -14 -41.9 22.9 24 -4 -14 -18 24.1 24 -4 -14 -65.59 35.8 29 -1 -15 29.6 53.19 28 -2 -15 346.07 74.49 28 -2 -16 -26.5 41.5 29 -1 -16 14.6 35.6 30 0 -16 28.1 34.9 25 -3 -15 122.99 51.59 25 -3 -15 117.19 54.89 26 -2 -15 157.28 52.99 27 -1 -15 3.8 30.2 28 0 -15 -13.5 33.3 29 1 -15 -13.1 31.2 22 -4 -14 272.17 61.69 22 -4 -14 110.09 49.6 23 -3 -14 17 33.1 23 -3 -14 87.99 36.7 24 -2 -14 -20.7 23.9 24 -2 -14 -1.8 31.6 25 -1 -14 47.4 32.1 26 0 -14 74.49 39.7 27 1 -14 -30.6 22 28 2 -14 180.38 59.89 19 -5 -13 10.5 28.3 19 -5 -13 -52.89 21.4 20 -4 -13 -16.1 21.5 20 -4 -13 -23.6 27.3 21 -3 -13 17.4 25.4 21 -3 -13 -5 19.8 22 -2 -13 31.7 30.7 22 -2 -13 43.2 24.7 23 -1 -13 -24.1 15.6 23 -1 -13 27.7 33.1 24 0 -13 4.5 14.2 25 1 -13 101.59 45.5 26 2 -13 -42.8 27.2 27 3 -13 110.79 52.59 17 -5 -12 57.99 30.7 17 -5 -12 -0.7 23.7 18 -4 -12 285.97 55.89 19 -3 -12 -22.5 17.2 19 -3 -12 30.9 22 20 -2 -12 452.25 73.59 20 -2 -12 541.35 86.19 21 -1 -12 34.7 33.2 21 -1 -12 64.69 32.4 -21 1 12 67.19 36 22 0 -12 17.4 22 22 0 -12 51.59 32.4 -22 0 12 33.3 28.7 23 1 -12 7.3 23 -23 -1 12 57.69 36.2 24 2 -12 -7.4 25.9 -24 -2 12 85.99 39.6 -25 -3 12 302.57 67.49 15 -5 -11 12.3 18.1 16 -4 -11 -13.3 17.1 16 -4 -11 26.7 18.1 17 -3 -11 42.5 20.6 17 -3 -11 78.09 28.5 -17 3 11 50.39 31.7 18 -2 -11 465.95 61.99 18 -2 -11 339.37 64.79 -18 2 11 411.56 63.89 19 -1 -11 192.78 49 19 -1 -11 172.68 49.7 -19 1 11 199.68 48.3 20 0 -11 -3.3 23.8 20 0 -11 4.3 10.4 -20 0 11 -30.7 17.4 21 1 -11 108.29 43.9 21 1 -11 123.39 42.9 -21 -1 11 153.38 39.9 22 2 -11 24.7 21.2 -22 -2 11 -50.89 26.5 23 3 -11 19.9 36.6 24 4 -11 50.19 46.4 -24 -4 11 15.5 51.29 12 -6 -10 -15.3 21.4 12 -6 -10 13.9 25.5 13 -5 -10 -1.9 17.3 13 -5 -10 36.6 23.9 -13 5 10 -7 21.4 14 -4 -10 0.8 16.6 -14 4 10 -8.7 20.2 -14 4 10 17.8 22.5 15 -3 -10 1040.6 82.79 15 -3 -10 1174.18 86.99 -15 3 10 964.9 83.69 -15 3 10 1029.2 96.99 16 -2 -10 210.28 45.8 16 -2 -10 172.28 43.2 -16 2 10 192.28 43.4 17 -1 -10 225.58 49.7 17 -1 -10 189.68 49.8 -17 1 10 158.98 40.4 18 0 -10 441.26 70.69 18 0 -10 405.16 69.89 -18 0 10 511.55 59.99 19 1 -10 103.29 34.6 19 1 -10 8.4 22.5 -19 -1 10 75.89 32.8 20 2 -10 169.28 48.2 20 2 -10 103.59 45.5 -20 -2 10 87.19 32.6 21 3 -10 1.8 20.6 -21 -3 10 12.6 29.6 22 4 -10 129.99 54.89 -22 -4 10 4.7 42.2 10 -6 -9 31.3 21.1 11 -5 -9 46.6 22 11 -5 -9 50.99 23.8 -11 5 9 67.79 31.7 12 -4 -9 20.8 16.9 12 -4 -9 72.29 24.7 -12 4 9 54.39 28.4 -12 4 9 45.5 24.3 13 -3 -9 45.8 18.5 13 -3 -9 69.79 24.6 -13 3 9 80.39 28 -13 3 9 73.89 28.5 14 -2 -9 113.19 32.7 14 -2 -9 118.09 31.4 -14 2 9 140.29 26.2 -14 2 9 100.09 33.1 15 -1 -9 937.01 75.99 15 -1 -9 1017.9 84.39 -15 1 9 1025.3 75.99 16 0 -9 -1.8 14.1 16 0 -9 -19 7 -16 0 9 -0.7 10.4 17 1 -9 170.58 39.9 17 1 -9 201.98 50.09 -17 -1 9 180.88 44.7 18 2 -9 1134.29 96.19 18 2 -9 1201.98 107.19 -18 -2 9 1125.39 90.59 19 3 -9 62.29 30.6 -19 -3 9 25.1 26.1 20 4 -9 3.2 25.7 -20 -4 9 84.49 36.2 21 5 -9 24.1 39.8 -21 -5 9 -25.4 38.7 -8 6 8 4.9 26.6 9 -5 -8 33.3 18.4 9 -5 -8 48.4 16.1 -9 5 8 81.59 20.8 10 -4 -8 226.38 39.4 10 -4 -8 187.88 37.7 -10 4 8 179.78 39.2 -10 4 8 219.18 48.1 11 -3 -8 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