#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:17:22 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242492 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132522.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_4132522 loop_ _publ_author_name 'Gr\'elaud, Simon' 'Cooper, Phillippa' 'Feron, Lyman J.' 'Bower, John F.' _publ_section_title ; Branch-Selective and Enantioselective Iridium-Catalyzed Alkene Hydroarylation via Anilide-Directed C-H Oxidative Addition. ; _journal_issue 30 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 9351 _journal_page_last 9356 _journal_paper_doi 10.1021/jacs.8b04627 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C10 H15 O4 S, C15 H18 N' _chemical_formula_sum 'C25 H33 N O4 S' _chemical_formula_weight 443.58 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-04-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486) ; _cell_angle_alpha 90 _cell_angle_beta 91.738(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.8224(3) _cell_length_b 6.6868(2) _cell_length_c 17.4224(6) _cell_measurement_reflns_used 6322 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.12 _cell_measurement_theta_min 2.34 _cell_volume 1143.78(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'Bruker Apex suite' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker area detector' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'Bruker Apex II kappa CCD area detector' _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 0.0426 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 19403 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.298 _diffrn_reflns_theta_min 2.074 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0743 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.8174. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.288 _exptl_crystal_description plate _exptl_crystal_F_000 476 _exptl_crystal_size_max 0.431 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.174 _refine_diff_density_max 0.677 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Flack x determined using 1938 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 296 _refine_ls_number_reflns 5131 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.2312P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.1021 _reflns_Friedel_coverage 0.833 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.986 _reflns_number_gt 4672 _reflns_number_total 5131 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04627_si_002.cif _cod_data_source_block testm1 _cod_database_code 4132522 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.971 _shelx_estimated_absorpt_t_min 0.929 _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 2.a Ternary CH refined with riding coordinates: C20(H20), C8(H8) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B) 2.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C) ; _shelx_res_file ; TITL testm1_a.res in P2(1) testm1.res created by SHELXL-2017/1 at 14:32:22 on 16-Apr-2018 REM Old TITL testm1 in P2(1) REM SHELXT solution in P2(1) REM R1 0.096, Rweak 0.030, Alpha 0.002, Orientation as input REM Flack x = 0.006 ( 0.034 ) from Parsons' quotients REM Formula found by SHELXT: C24 N2 O4 S CELL 0.71073 9.8224 6.6868 17.4224 90 91.738 90 ZERR 2 0.0003 0.0002 0.0006 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 50 66 2 8 2 EQIV $1 1-X,-0.5+Y,1-Z EQIV $2 1-X,0.5+Y,1-Z L.S. 4 0 0 PLAN 5 SIZE 0.174 0.3 0.431 TEMP -173(2) HTAB N1 O1_$1 HTAB N1 O2 HTAB N1 O3_$2 BOND $H list 4 fmap 2 53 ACTA REM REM REM WGHT 0.058700 0.231200 FVAR 0.87614 S1 5 0.483138 0.549921 0.644583 11.00000 0.02306 0.01822 = 0.01717 0.00093 0.00573 0.00282 O1 4 0.580019 0.686207 0.681238 11.00000 0.03580 0.02607 = 0.02905 -0.00179 0.00977 -0.01141 O2 4 0.419175 0.641021 0.575589 11.00000 0.04477 0.03140 = 0.01963 0.00573 0.00724 0.01443 O3 4 0.538249 0.352771 0.628956 11.00000 0.02189 0.02366 = 0.02285 -0.00266 0.00120 0.00559 O4 4 0.224143 0.150376 0.762714 11.00000 0.02504 0.02774 = 0.03815 -0.00529 -0.00438 -0.00674 C16 1 0.346950 0.515656 0.708068 11.00000 0.01577 0.02972 = 0.01772 0.00233 0.00250 0.00601 AFIX 23 H16A 2 0.302053 0.646846 0.714618 11.00000 -1.20000 H16B 2 0.279454 0.426022 0.682446 11.00000 -1.20000 AFIX 0 C17 1 0.379087 0.431155 0.787838 11.00000 0.01101 0.01794 = 0.01798 0.00200 0.00197 0.00079 C18 1 0.522912 0.338266 0.806914 11.00000 0.01083 0.02154 = 0.02385 0.00269 0.00115 0.00347 AFIX 23 H18A 2 0.530684 0.202770 0.784567 11.00000 -1.20000 H18B 2 0.596340 0.423692 0.787152 11.00000 -1.20000 AFIX 0 C19 1 0.529770 0.329876 0.895989 11.00000 0.01535 0.03095 = 0.02230 0.00420 -0.00119 0.00196 AFIX 23 H19A 2 0.545368 0.191517 0.914468 11.00000 -1.20000 H19B 2 0.603061 0.417292 0.917179 11.00000 -1.20000 AFIX 0 C20 1 0.388267 0.406543 0.918290 11.00000 0.01811 0.02330 = 0.01688 0.00108 0.00255 0.00362 AFIX 13 H20 2 0.382827 0.451449 0.972860 11.00000 -1.20000 AFIX 0 C21 1 0.286566 0.240706 0.895024 11.00000 0.01979 0.02057 = 0.02663 0.00390 0.00540 0.00071 AFIX 23 H21A 2 0.318916 0.107753 0.912686 11.00000 -1.20000 H21B 2 0.195378 0.266661 0.915581 11.00000 -1.20000 AFIX 0 C22 1 0.284741 0.256312 0.807730 11.00000 0.01377 0.01619 = 0.02828 -0.00112 0.00022 0.00290 C23 1 0.358100 0.572890 0.857956 11.00000 0.01698 0.01713 = 0.01973 0.00123 0.00044 0.00004 C24 1 0.459985 0.745388 0.862524 11.00000 0.02515 0.02374 = 0.03033 -0.00301 -0.00042 -0.00478 AFIX 137 H24A 2 0.551906 0.694120 0.854420 11.00000 -1.50000 H24B 2 0.456959 0.808292 0.913248 11.00000 -1.50000 H24C 2 0.436453 0.844417 0.822833 11.00000 -1.50000 AFIX 0 C25 1 0.213692 0.658697 0.860332 11.00000 0.01992 0.02463 = 0.02551 0.00007 0.00432 0.00527 AFIX 137 H25A 2 0.201217 0.759304 0.819825 11.00000 -1.50000 H25B 2 0.200201 0.720867 0.910469 11.00000 -1.50000 H25C 2 0.147271 0.550817 0.852222 11.00000 -1.50000 AFIX 0 N1 3 0.359711 0.487042 0.429928 11.00000 0.01175 0.01408 = 0.02500 0.00156 0.00539 -0.00018 C1 1 0.217751 0.414850 0.418733 11.00000 0.01157 0.01247 = 0.02032 -0.00303 0.00360 -0.00106 C2 1 0.174021 0.266341 0.469095 11.00000 0.01440 0.01365 = 0.01960 -0.00307 0.00209 0.00166 C3 1 0.039480 0.202056 0.460972 11.00000 0.01644 0.01317 = 0.02155 -0.00048 0.00547 0.00002 AFIX 43 H3 2 0.005522 0.106003 0.495718 11.00000 -1.20000 AFIX 0 C4 1 -0.045574 0.276752 0.402672 11.00000 0.01189 0.01749 = 0.02501 -0.00454 0.00059 -0.00074 AFIX 43 H4 2 -0.137151 0.231754 0.397667 11.00000 -1.20000 AFIX 0 C5 1 0.003283 0.417243 0.351694 11.00000 0.01623 0.01902 = 0.01965 -0.00087 -0.00192 0.00162 AFIX 43 H5 2 -0.055036 0.465588 0.311340 11.00000 -1.20000 AFIX 0 C6 1 0.136439 0.488600 0.358695 11.00000 0.01920 0.01337 = 0.01608 -0.00379 0.00418 0.00038 C7 1 0.266808 0.167502 0.528600 11.00000 0.01645 0.02160 = 0.03128 0.00635 -0.00142 -0.00122 AFIX 137 H7A 2 0.301416 0.041589 0.508021 11.00000 -1.50000 H7B 2 0.215777 0.140253 0.574926 11.00000 -1.50000 H7C 2 0.343386 0.256586 0.541433 11.00000 -1.50000 AFIX 0 C8 1 0.182620 0.652183 0.304298 11.00000 0.01998 0.01586 = 0.02282 0.00041 0.00209 -0.00244 AFIX 13 H8 2 0.283903 0.661231 0.311012 11.00000 -1.20000 AFIX 0 C9 1 0.125958 0.851185 0.330526 11.00000 0.04391 0.01894 = 0.03148 -0.00174 0.00996 -0.00074 AFIX 137 H9A 2 0.027420 0.854674 0.319962 11.00000 -1.50000 H9B 2 0.169541 0.960120 0.302763 11.00000 -1.50000 H9C 2 0.144335 0.867223 0.385784 11.00000 -1.50000 AFIX 0 C10 1 0.153388 0.601060 0.220366 11.00000 0.01023 0.02443 = 0.01888 0.00166 0.00239 -0.00228 C11 1 0.175234 0.408384 0.193468 11.00000 0.02193 0.02760 = 0.02459 0.00115 0.00227 -0.00101 AFIX 43 H11 2 0.202994 0.306053 0.228381 11.00000 -1.20000 AFIX 0 C12 1 0.156868 0.364434 0.116236 11.00000 0.02864 0.04418 = 0.02796 -0.00983 0.00541 -0.00758 AFIX 43 H12 2 0.170582 0.231718 0.098612 11.00000 -1.20000 AFIX 0 C13 1 0.118553 0.513021 0.064411 11.00000 0.02071 0.07130 = 0.01604 -0.00353 0.00065 -0.00956 AFIX 43 H13 2 0.105868 0.482476 0.011423 11.00000 -1.20000 AFIX 0 C14 1 0.098978 0.705668 0.090387 11.00000 0.01722 0.05899 = 0.02477 0.01785 -0.00031 0.00354 AFIX 43 H14 2 0.074871 0.808636 0.054947 11.00000 -1.20000 AFIX 0 C15 1 0.114244 0.749307 0.167489 11.00000 0.01450 0.03441 = 0.03068 0.00813 0.00443 0.00329 AFIX 43 H15 2 0.098004 0.881539 0.184926 11.00000 -1.20000 AFIX 0 H1A 2 0.379119 0.509502 0.484228 11.00000 0.01097 H1B 2 0.372961 0.595427 0.406223 11.00000 0.01630 H1C 2 0.418316 0.387058 0.408945 11.00000 0.05929 HKLF 4 REM testm1_a.res in P2(1) REM R1 = 0.0414 for 4672 Fo > 4sig(Fo) and 0.0474 for all 5131 data REM 296 parameters refined using 1 restraints END WGHT 0.0587 0.2312 REM Highest difference peak 0.677, deepest hole -0.314, 1-sigma level 0.056 Q1 1 0.4791 0.5552 0.5942 11.00000 0.05 0.68 Q2 1 0.4906 0.5543 0.6989 11.00000 0.05 0.46 Q3 1 0.1682 0.6395 0.2592 11.00000 0.05 0.40 Q4 1 0.2824 0.2442 0.8540 11.00000 0.05 0.37 Q5 1 0.5394 0.3433 0.5771 11.00000 0.05 0.31 ; _shelx_res_checksum 33371 _shelx_hkl_file ; -1 0 0 1637.84 49.60 1 0 0 1689.03 49.70 1 0 0 1616.54 49.60 -1 0 0 1558.04 49.40 -1 0 0 1678.23 49.70 2 0 0 396.76 13.80 -2 0 0 424.86 13.90 -2 0 0 384.36 13.50 -2 0 0 404.06 12.80 -2 0 0 394.46 13.70 3 0 0 4626.84 141.39 -3 0 0 4545.65 141.29 -3 0 0 4729.93 141.39 -3 0 0 4685.93 140.19 4 0 0 66.09 5.80 -4 0 0 54.99 5.00 -4 0 0 49.00 3.50 -4 0 0 66.49 5.70 -5 0 0 46.90 5.50 5 0 0 31.30 4.90 -5 0 0 36.80 5.30 -5 0 0 33.00 3.30 6 0 0 406.16 17.50 -6 0 0 403.76 17.10 -6 0 0 399.36 14.20 -6 0 0 398.96 17.30 -7 0 0 13.90 2.50 -7 0 0 9.80 4.80 -7 0 0 11.00 5.20 7 0 0 9.10 5.10 8 0 0 240.88 15.00 -8 0 0 239.48 14.50 -8 0 0 243.98 14.20 9 0 0 33.10 7.70 -9 0 0 39.30 7.30 -9 0 0 33.20 7.20 -10 0 0 9.40 5.90 -10 0 0 3.90 5.50 10 0 0 -2.50 5.90 -11 0 0 39.30 9.00 -11 0 0 35.10 7.70 11 0 0 27.40 8.70 12 0 0 130.89 14.40 -12 0 0 145.99 13.60 -12 0 0 106.19 13.80 0 -1 0 2.90 0.80 0 -1 0 0.20 0.80 0 1 0 4.20 0.90 0 1 0 2.00 0.70 0 1 0 0.10 0.70 0 1 0 1.40 0.90 -1 -1 0 4872.81 143.59 -1 -1 0 4638.44 143.69 -1 1 0 4933.11 145.39 1 1 0 4648.73 144.49 -1 1 0 4466.55 144.39 -1 1 0 4920.21 144.89 -1 1 0 5016.20 144.29 1 1 0 4769.32 144.59 2 -1 0 295.87 10.60 2 -1 0 339.77 10.80 -2 -1 0 301.67 12.00 -2 -1 0 314.87 11.90 -2 1 0 336.07 11.70 -2 1 0 348.17 11.80 -2 1 0 330.07 11.40 2 1 0 319.87 12.40 -3 -1 0 4137.69 130.29 3 -1 0 4355.96 129.39 -3 -1 0 4316.77 130.39 3 -1 0 4234.78 128.89 -3 1 0 4482.85 134.89 -3 1 0 4309.87 134.69 -3 1 0 4538.75 135.29 3 1 0 4449.15 135.99 -4 -1 0 397.86 16.00 4 -1 0 390.76 15.10 -4 -1 0 413.86 17.30 -4 -1 0 412.76 15.30 4 -1 0 397.56 14.10 -4 -1 0 419.66 16.10 -4 1 0 439.96 15.50 -4 1 0 442.46 16.00 -4 1 0 397.26 15.40 4 1 0 435.16 16.90 5 -1 0 1716.83 54.19 -5 -1 0 1675.23 56.09 5 -1 0 1761.72 55.49 -5 -1 0 1750.02 55.19 -5 -1 0 1773.62 56.59 -5 -1 0 1702.13 56.99 -5 1 0 1830.52 57.99 -5 1 0 1787.22 58.09 -5 1 0 1845.42 58.59 5 1 0 1846.22 59.69 -6 -1 0 587.34 23.40 6 -1 0 598.04 22.50 -6 -1 0 582.44 21.50 -6 -1 0 589.04 24.30 -6 1 0 593.84 21.90 -6 1 0 587.84 22.00 6 1 0 607.84 23.60 -6 1 0 581.04 22.40 7 -1 0 117.19 10.10 -7 -1 0 116.69 11.20 -7 -1 0 115.49 10.60 -7 -1 0 100.99 7.60 -7 1 0 126.59 9.00 -7 1 0 132.59 9.60 -7 1 0 117.89 9.30 7 1 0 113.49 10.60 8 -1 0 706.53 27.60 -8 -1 0 663.63 24.90 -8 -1 0 692.43 28.20 -8 -1 0 678.73 28.50 -8 1 0 697.63 26.50 8 1 0 668.53 28.10 -8 1 0 680.53 26.90 -8 1 0 697.33 26.80 9 -1 0 240.58 15.40 -9 -1 0 241.18 16.00 -9 -1 0 265.17 16.00 9 1 0 241.88 15.90 -9 1 0 260.27 14.60 -9 1 0 243.98 13.80 10 -1 0 77.79 10.20 -10 -1 0 69.09 9.90 -10 -1 0 78.29 10.50 -10 1 0 78.19 9.30 -10 1 0 55.39 9.10 10 1 0 62.09 9.60 -11 -1 0 79.49 11.20 -11 -1 0 57.59 9.70 11 -1 0 54.19 10.10 -11 1 0 63.99 9.00 -11 1 0 56.59 9.90 11 1 0 63.39 10.20 -12 -1 0 34.20 9.30 12 -1 0 25.80 9.00 -12 1 0 31.40 9.20 12 1 0 27.70 8.80 -12 1 0 36.20 7.90 0 -2 0 569.74 19.20 0 2 0 571.14 20.10 0 2 0 625.64 20.10 0 2 0 568.64 20.20 0 2 0 651.03 19.50 1 -2 0 318.27 11.80 -1 -2 0 360.46 12.60 -1 -2 0 334.47 13.00 -1 2 0 337.57 13.50 1 2 0 371.06 13.70 -1 2 0 406.96 13.50 1 2 0 385.06 13.50 -1 2 0 414.96 12.70 1 2 0 382.36 13.30 -1 2 0 349.87 13.20 -2 -2 0 512.45 19.10 -2 -2 0 535.35 18.80 -2 2 0 477.15 18.10 2 2 0 512.65 18.30 -2 2 0 518.65 17.70 2 2 0 529.25 18.70 -2 2 0 540.15 18.10 -2 2 0 526.95 17.30 2 2 0 543.45 17.80 -3 -2 0 196.18 10.00 3 -2 0 222.98 8.60 -3 -2 0 197.88 10.30 3 2 0 210.08 10.40 -3 2 0 223.68 9.30 -3 2 0 232.08 9.20 -3 2 0 234.38 9.60 3 2 0 211.48 10.50 -4 -2 0 726.93 26.80 4 -2 0 744.03 24.40 -4 -2 0 753.42 26.80 4 -2 0 724.63 24.30 4 2 0 753.42 27.80 -4 2 0 803.42 26.70 -4 2 0 733.63 25.00 -4 2 0 800.12 26.10 5 -2 0 4.10 3.60 -5 -2 0 15.10 4.80 5 -2 0 15.70 3.10 -5 -2 0 10.40 5.00 -5 -2 0 12.50 4.20 -5 2 0 26.90 4.50 -5 2 0 13.30 3.10 5 2 0 11.00 4.70 -5 2 0 13.90 3.10 6 -2 0 549.15 20.70 -6 -2 0 558.44 23.10 -6 -2 0 515.75 22.50 -6 -2 0 528.55 25.40 -6 -2 0 557.74 21.70 6 -2 0 538.15 19.60 -6 2 0 537.15 20.20 -6 2 0 558.54 20.70 -6 2 0 533.65 21.50 6 2 0 579.14 23.30 7 -2 0 301.97 13.60 7 -2 0 300.17 15.00 -7 -2 0 315.07 17.00 -7 -2 0 323.47 15.20 -7 -2 0 314.97 19.70 -7 -2 0 308.87 17.00 7 2 0 318.47 17.20 -7 2 0 319.37 14.50 -7 2 0 320.87 15.50 -8 -2 0 505.95 21.30 8 -2 0 480.15 19.60 -8 -2 0 524.05 23.60 -8 -2 0 521.65 25.60 8 -2 0 516.15 21.80 -8 2 0 507.85 22.20 8 2 0 554.84 24.20 -8 2 0 497.05 20.90 -9 -2 0 7.70 7.90 -9 -2 0 -1.20 4.20 9 -2 0 -3.70 5.80 -9 -2 0 0.70 6.00 -9 2 0 7.40 5.40 -9 2 0 14.50 4.80 9 2 0 10.70 6.40 -10 -2 0 9.20 6.60 -10 -2 0 11.50 8.30 10 -2 0 -4.90 6.00 10 2 0 2.60 6.10 -10 2 0 10.60 5.00 -10 2 0 8.90 6.10 -11 -2 0 42.20 9.20 11 -2 0 26.00 8.10 -11 -2 0 53.89 11.00 -11 2 0 54.89 8.40 -11 2 0 31.80 8.60 11 2 0 42.50 9.50 -12 -2 0 84.19 13.00 -12 -2 0 60.29 10.70 12 -2 0 45.30 9.40 12 2 0 59.69 10.80 -12 2 0 55.09 10.80 0 -3 0 -1.90 2.60 0 -3 0 -1.70 2.00 0 3 0 0.10 2.10 0 3 0 -0.60 1.90 0 3 0 -0.10 1.80 0 3 0 0.40 2.50 0 3 0 0.70 1.80 -1 -3 0 454.75 17.40 -1 -3 0 467.25 16.60 1 -3 0 428.56 16.00 -1 3 0 497.85 17.50 -1 3 0 472.15 17.40 -1 3 0 495.55 16.20 1 3 0 480.55 16.70 1 3 0 481.85 17.50 1 3 0 469.75 17.20 -1 3 0 443.36 17.60 -2 -3 0 447.36 17.70 -2 -3 0 468.75 18.40 -2 3 0 491.45 16.30 2 3 0 463.05 18.00 2 3 0 472.55 17.30 -2 3 0 462.45 17.10 -2 3 0 488.05 17.50 -2 3 0 434.46 17.70 2 3 0 491.45 17.40 3 -3 0 542.25 19.10 -3 -3 0 548.25 20.90 -3 -3 0 524.05 21.10 3 3 0 530.25 19.50 -3 3 0 566.04 20.00 -3 3 0 556.34 18.90 3 3 0 548.95 21.00 3 3 0 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187.28 15.90 -2 0 21 167.58 15.80 1 0 -21 50.79 9.20 1 0 -21 37.40 8.70 -1 0 21 56.39 10.30 0 0 -21 11.40 7.10 0 0 21 -4.30 5.70 0 0 -21 8.30 5.70 -1 0 -21 8.10 6.70 -1 0 -21 -3.60 6.50 1 0 21 13.00 7.20 2 0 21 116.69 12.30 2 0 21 102.29 13.80 -2 0 -21 98.89 12.10 -2 0 -21 107.09 11.80 -3 0 -21 23.50 8.70 3 0 21 43.80 9.10 3 0 21 40.80 10.60 -3 0 -21 52.39 9.90 -4 0 -21 9.50 8.90 4 0 21 3.70 6.50 4 -1 -21 102.79 12.70 -4 -1 21 120.09 14.70 4 1 -21 92.59 12.50 -4 1 21 125.39 15.10 4 1 -21 105.29 11.30 3 -1 -21 89.19 11.50 3 -1 -21 78.19 11.40 -3 -1 21 95.19 12.90 3 1 -21 77.49 10.00 3 1 -21 74.29 11.50 -3 1 21 80.89 12.50 2 -1 -21 82.19 10.50 2 -1 -21 65.59 10.90 -2 -1 21 56.59 10.10 2 1 -21 64.79 10.30 2 1 -21 61.29 9.10 -2 1 21 68.49 11.30 -1 -1 21 18.60 7.60 1 -1 -21 5.30 6.90 1 1 -21 11.60 7.60 1 1 -21 8.10 6.40 -1 1 21 2.10 6.60 0 -1 21 22.70 8.20 0 -1 -21 21.90 8.40 0 1 -21 12.30 7.40 0 1 21 21.10 8.20 0 1 -21 30.80 7.50 -1 -1 -21 30.70 8.70 1 -1 21 14.40 7.80 1 1 21 27.00 9.20 -1 1 -21 24.50 8.20 1 1 21 33.70 7.40 -1 1 -21 33.30 7.90 -2 -1 -21 50.59 10.00 2 -1 21 45.90 10.00 2 1 21 30.30 7.60 -2 1 -21 39.00 8.80 2 1 21 55.39 11.60 -2 1 -21 44.10 8.60 -3 -1 -21 33.80 9.30 3 -1 21 37.60 9.90 3 -1 21 28.40 8.00 -3 1 -21 34.20 8.30 3 1 21 38.20 8.60 -3 1 -21 26.10 8.70 3 1 21 16.60 9.10 -3 1 -21 33.30 9.10 -3 -2 21 224.98 17.20 3 -2 -21 160.68 15.50 3 -2 -21 204.18 17.10 -3 2 21 210.88 18.60 3 2 -21 228.58 16.80 3 2 -21 226.28 17.50 2 -2 -21 24.70 8.20 2 -2 -21 22.60 8.10 -2 -2 21 33.60 8.40 -2 2 21 8.70 8.10 2 2 -21 39.10 8.20 2 2 -21 25.60 8.30 1 -2 -21 78.89 10.80 -1 -2 21 88.19 12.60 1 -2 -21 81.09 11.70 1 2 -21 87.79 11.70 1 2 -21 62.29 10.00 -1 2 21 70.19 12.20 0 -2 21 106.29 14.10 0 -2 -21 76.89 11.70 0 2 -21 90.89 12.00 0 2 -21 77.69 10.50 0 2 21 84.59 13.30 -1 -2 -21 7.50 7.40 1 -2 21 27.70 8.10 -1 2 -21 18.60 7.90 1 2 21 14.70 6.30 -1 2 -21 24.70 8.20 1 2 21 15.80 9.10 -2 -2 -21 78.29 11.90 2 -2 21 65.39 11.20 -2 2 -21 82.39 10.90 2 2 21 63.39 13.00 -2 2 -21 69.69 10.50 2 2 21 88.29 11.70 1 3 -21 3.90 7.00 0 3 -21 68.39 10.50 2 0 -22 11.00 8.20 -2 0 22 35.80 9.50 1 0 -22 23.10 8.40 -1 0 22 11.00 7.50 0 0 22 22.80 9.00 0 0 -22 15.20 8.20 -1 0 -22 -5.30 6.80 1 0 22 2.90 7.50 -1 0 -22 10.00 6.90 -2 0 -22 70.59 10.70 2 -1 -22 18.20 11.80 -2 -1 22 12.80 7.50 2 -1 -22 6.80 7.90 -2 1 22 4.90 7.30 2 1 -22 10.70 6.70 2 1 -22 13.90 7.90 -1 -1 22 105.09 13.90 1 -1 -22 96.19 12.90 1 1 -22 113.59 13.60 1 1 -22 93.29 10.80 -1 1 22 105.19 14.90 0 -1 22 2.00 6.50 0 -1 -22 14.70 8.30 0 1 -22 10.60 7.00 0 1 22 12.60 8.60 0 1 -22 5.20 7.50 1 -1 22 63.19 11.80 -1 -1 -22 41.30 10.00 1 1 22 70.69 10.30 -1 1 -22 67.89 10.20 1 1 22 71.69 13.10 -1 1 -22 36.50 9.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 56140 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 S1 S 0.48314(7) 0.54992(11) 0.64458(4) 0.01938(17) Uani 1 1 d . O1 O 0.5800(2) 0.6862(4) 0.68124(12) 0.0301(5) Uani 1 1 d . O2 O 0.4192(3) 0.6410(4) 0.57559(12) 0.0318(6) Uani 1 1 d . O3 O 0.5382(2) 0.3528(3) 0.62896(11) 0.0228(5) Uani 1 1 d . O4 O 0.2241(2) 0.1504(4) 0.76271(13) 0.0304(5) Uani 1 1 d . C16 C 0.3470(3) 0.5157(5) 0.70807(15) 0.0210(6) Uani 1 1 d . H16A H 0.302053 0.646846 0.714618 0.025 Uiso 1 1 calc R H16B H 0.279454 0.426022 0.682446 0.025 Uiso 1 1 calc R C17 C 0.3791(3) 0.4312(4) 0.78784(15) 0.0156(5) Uani 1 1 d . C18 C 0.5229(3) 0.3383(5) 0.80691(16) 0.0187(6) Uani 1 1 d . H18A H 0.530684 0.202770 0.784567 0.022 Uiso 1 1 calc R H18B H 0.596340 0.423692 0.787152 0.022 Uiso 1 1 calc R C19 C 0.5298(3) 0.3299(5) 0.89599(17) 0.0229(6) Uani 1 1 d . H19A H 0.545368 0.191517 0.914468 0.027 Uiso 1 1 calc R H19B H 0.603061 0.417292 0.917179 0.027 Uiso 1 1 calc R C20 C 0.3883(3) 0.4065(5) 0.91829(16) 0.0194(6) Uani 1 1 d . H20 H 0.382827 0.451449 0.972860 0.023 Uiso 1 1 calc R C21 C 0.2866(3) 0.2407(5) 0.89502(17) 0.0222(6) Uani 1 1 d . H21A H 0.318916 0.107753 0.912686 0.027 Uiso 1 1 calc R H21B H 0.195378 0.266661 0.915581 0.027 Uiso 1 1 calc R C22 C 0.2847(3) 0.2563(4) 0.80773(17) 0.0194(6) Uani 1 1 d . C23 C 0.3581(3) 0.5729(5) 0.85796(15) 0.0179(6) Uani 1 1 d . C24 C 0.4600(3) 0.7454(5) 0.86252(18) 0.0264(7) Uani 1 1 d . H24A H 0.551906 0.694120 0.854420 0.040 Uiso 1 1 calc GR H24B H 0.456959 0.808292 0.913248 0.040 Uiso 1 1 calc GR H24C H 0.436453 0.844417 0.822833 0.040 Uiso 1 1 calc GR C25 C 0.2137(3) 0.6587(5) 0.86033(17) 0.0233(6) Uani 1 1 d . H25A H 0.201217 0.759304 0.819825 0.035 Uiso 1 1 calc GR H25B H 0.200201 0.720867 0.910469 0.035 Uiso 1 1 calc GR H25C H 0.147271 0.550817 0.852222 0.035 Uiso 1 1 calc GR N1 N 0.3597(2) 0.4870(4) 0.42993(15) 0.0168(5) Uani 1 1 d . C1 C 0.2178(3) 0.4149(4) 0.41873(15) 0.0147(5) Uani 1 1 d . C2 C 0.1740(3) 0.2663(4) 0.46910(15) 0.0159(5) Uani 1 1 d . C3 C 0.0395(3) 0.2021(4) 0.46097(16) 0.0170(6) Uani 1 1 d . H3 H 0.005522 0.106003 0.495718 0.020 Uiso 1 1 calc R C4 C -0.0456(3) 0.2768(4) 0.40267(16) 0.0181(6) Uani 1 1 d . H4 H -0.137151 0.231754 0.397667 0.022 Uiso 1 1 calc R C5 C 0.0033(3) 0.4172(4) 0.35169(15) 0.0184(6) Uani 1 1 d . H5 H -0.055036 0.465588 0.311340 0.022 Uiso 1 1 calc R C6 C 0.1364(3) 0.4886(4) 0.35869(15) 0.0161(6) Uani 1 1 d . C7 C 0.2668(3) 0.1675(5) 0.52860(17) 0.0232(6) Uani 1 1 d . H7A H 0.301416 0.041589 0.508021 0.035 Uiso 1 1 calc GR H7B H 0.215777 0.140253 0.574926 0.035 Uiso 1 1 calc GR H7C H 0.343386 0.256586 0.541433 0.035 Uiso 1 1 calc GR C8 C 0.1826(3) 0.6522(4) 0.30430(16) 0.0195(6) Uani 1 1 d . H8 H 0.283903 0.661231 0.311012 0.023 Uiso 1 1 calc R C9 C 0.1260(4) 0.8512(5) 0.33053(19) 0.0313(8) Uani 1 1 d . H9A H 0.027420 0.854674 0.319962 0.047 Uiso 1 1 calc GR H9B H 0.169541 0.960120 0.302763 0.047 Uiso 1 1 calc GR H9C H 0.144335 0.867223 0.385784 0.047 Uiso 1 1 calc GR C10 C 0.1534(3) 0.6011(4) 0.22037(15) 0.0178(6) Uani 1 1 d . C11 C 0.1752(3) 0.4084(5) 0.19347(17) 0.0247(7) Uani 1 1 d . H11 H 0.202994 0.306053 0.228381 0.030 Uiso 1 1 calc R C12 C 0.1569(3) 0.3644(6) 0.11624(19) 0.0335(8) Uani 1 1 d . H12 H 0.170582 0.231718 0.098612 0.040 Uiso 1 1 calc R C13 C 0.1186(3) 0.5130(7) 0.06441(17) 0.0360(10) Uani 1 1 d . H13 H 0.105868 0.482476 0.011423 0.043 Uiso 1 1 calc R C14 C 0.0990(3) 0.7057(6) 0.09039(19) 0.0337(8) Uani 1 1 d . H14 H 0.074871 0.808636 0.054947 0.040 Uiso 1 1 calc R C15 C 0.1142(3) 0.7493(5) 0.16749(18) 0.0265(7) Uani 1 1 d . H15 H 0.098004 0.881539 0.184926 0.032 Uiso 1 1 calc R H1A H 0.379(3) 0.510(5) 0.4842(17) 0.011(7) Uiso 1 1 d . H1B H 0.373(3) 0.595(6) 0.4062(18) 0.016(8) Uiso 1 1 d . H1C H 0.418(5) 0.387(7) 0.409(3) 0.059(14) Uiso 1 1 d . 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 0.0231(3) 0.0182(3) 0.0172(3) 0.0009(3) 0.0057(2) 0.0028(3) O1 0.0358(13) 0.0261(12) 0.0290(11) -0.0018(10) 0.0098(10) -0.0114(10) O2 0.0448(14) 0.0314(13) 0.0196(11) 0.0057(9) 0.0072(9) 0.0144(11) O3 0.0219(11) 0.0237(11) 0.0229(10) -0.0027(8) 0.0012(8) 0.0056(9) O4 0.0250(12) 0.0277(13) 0.0381(13) -0.0053(11) -0.0044(9) -0.0067(10) C16 0.0158(13) 0.0297(18) 0.0177(13) 0.0023(12) 0.0025(10) 0.0060(12) C17 0.0110(12) 0.0179(14) 0.0180(13) 0.0020(11) 0.0020(10) 0.0008(10) C18 0.0108(12) 0.0215(14) 0.0239(14) 0.0027(11) 0.0012(10) 0.0035(11) C19 0.0153(14) 0.0309(17) 0.0223(15) 0.0042(12) -0.0012(11) 0.0020(12) C20 0.0181(14) 0.0233(15) 0.0169(13) 0.0011(11) 0.0026(10) 0.0036(12) C21 0.0198(14) 0.0206(16) 0.0266(15) 0.0039(12) 0.0054(11) 0.0007(12) C22 0.0138(13) 0.0162(14) 0.0283(15) -0.0011(12) 0.0002(11) 0.0029(11) C23 0.0170(12) 0.0171(15) 0.0197(12) 0.0012(11) 0.0004(10) 0.0000(11) C24 0.0252(16) 0.0237(16) 0.0303(16) -0.0030(13) -0.0004(12) -0.0048(13) C25 0.0199(15) 0.0246(16) 0.0255(15) 0.0001(13) 0.0043(11) 0.0053(13) N1 0.0117(11) 0.0141(12) 0.0250(13) 0.0016(10) 0.0054(9) -0.0002(9) C1 0.0116(12) 0.0125(12) 0.0203(13) -0.0030(10) 0.0036(10) -0.0011(10) C2 0.0144(13) 0.0137(13) 0.0196(13) -0.0031(11) 0.0021(10) 0.0017(11) C3 0.0164(13) 0.0132(13) 0.0215(13) -0.0005(11) 0.0055(10) 0.0000(11) C4 0.0119(12) 0.0175(14) 0.0250(14) -0.0045(11) 0.0006(10) -0.0007(10) C5 0.0162(13) 0.0190(14) 0.0197(14) -0.0009(11) -0.0019(10) 0.0016(11) C6 0.0192(14) 0.0134(13) 0.0161(13) -0.0038(10) 0.0042(10) 0.0004(11) C7 0.0165(14) 0.0216(16) 0.0313(16) 0.0063(13) -0.0014(11) -0.0012(12) C8 0.0200(14) 0.0159(15) 0.0228(15) 0.0004(12) 0.0021(11) -0.0024(12) C9 0.044(2) 0.0189(16) 0.0315(18) -0.0017(13) 0.0100(14) -0.0007(15) C10 0.0102(12) 0.0244(17) 0.0189(13) 0.0017(11) 0.0024(10) -0.0023(10) C11 0.0219(15) 0.0276(17) 0.0246(16) 0.0011(13) 0.0023(12) -0.0010(13) C12 0.0286(17) 0.044(2) 0.0280(17) -0.0098(15) 0.0054(13) -0.0076(15) C13 0.0207(15) 0.071(3) 0.0160(14) -0.0035(16) 0.0007(11) -0.0096(17) C14 0.0172(15) 0.059(2) 0.0248(16) 0.0179(16) -0.0003(12) 0.0035(15) C15 0.0145(14) 0.0344(18) 0.0307(16) 0.0081(14) 0.0044(12) 0.0033(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 S1 O2 110.95(15) O1 S1 O3 114.13(14) O1 S1 C16 107.64(14) O2 S1 C16 104.55(13) O3 S1 O2 112.00(13) O3 S1 C16 106.94(14) S1 C16 H16A 107.7 S1 C16 H16B 107.7 H16A C16 H16B 107.1 C17 C16 S1 118.46(19) C17 C16 H16A 107.7 C17 C16 H16B 107.7 C16 C17 C18 120.0(2) C16 C17 C22 112.2(2) C16 C17 C23 117.3(2) C22 C17 C18 101.3(2) C22 C17 C23 101.0(2) C23 C17 C18 102.3(2) C17 C18 H18A 111.0 C17 C18 H18B 111.0 H18A C18 H18B 109.0 C19 C18 C17 103.7(2) C19 C18 H18A 111.0 C19 C18 H18B 111.0 C18 C19 H19A 111.1 C18 C19 H19B 111.1 H19A C19 H19B 109.1 C20 C19 C18 103.2(2) C20 C19 H19A 111.1 C20 C19 H19B 111.1 C19 C20 H20 114.5 C19 C20 C23 102.9(2) C21 C20 C19 106.1(2) C21 C20 H20 114.5 C21 C20 C23 103.2(2) C23 C20 H20 114.5 C20 C21 H21A 111.4 C20 C21 H21B 111.4 H21A C21 H21B 109.3 C22 C21 C20 101.6(2) C22 C21 H21A 111.4 C22 C21 H21B 111.4 O4 C22 C17 126.2(3) O4 C22 C21 127.0(3) C21 C22 C17 106.7(2) C20 C23 C17 93.9(2) C24 C23 C17 113.4(2) C24 C23 C20 113.2(2) C24 C23 C25 108.8(3) C25 C23 C17 113.1(2) C25 C23 C20 114.1(2) C23 C24 H24A 109.5 C23 C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C1 N1 H1A 109.5(18) C1 N1 H1B 112(2) C1 N1 H1C 107(3) H1A N1 H1B 108(3) H1A N1 H1C 112(3) H1B N1 H1C 108(3) C2 C1 N1 117.0(2) C6 C1 N1 120.1(2) C6 C1 C2 122.9(2) C1 C2 C7 123.3(2) C3 C2 C1 117.6(2) C3 C2 C7 119.0(3) C2 C3 H3 119.6 C4 C3 C2 120.8(3) C4 C3 H3 119.6 C3 C4 H4 120.0 C5 C4 C3 120.0(3) C5 C4 H4 120.0 C4 C5 H5 119.4 C4 C5 C6 121.1(3) C6 C5 H5 119.4 C1 C6 C5 117.5(2) C1 C6 C8 123.2(2) C5 C6 C8 119.1(2) C2 C7 H7A 109.5 C2 C7 H7B 109.5 C2 C7 H7C 109.5 H7A C7 H7B 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C6 C8 H8 106.5 C9 C8 C6 108.8(2) C9 C8 H8 106.5 C9 C8 C10 115.2(3) C10 C8 C6 112.7(2) C10 C8 H8 106.5 C8 C9 H9A 109.5 C8 C9 H9B 109.5 C8 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C11 C10 C8 120.4(3) C11 C10 C15 118.5(3) C15 C10 C8 120.9(3) C10 C11 H11 119.7 C12 C11 C10 120.5(3) C12 C11 H11 119.7 C11 C12 H12 119.8 C11 C12 C13 120.4(4) C13 C12 H12 119.8 C12 C13 H13 120.2 C14 C13 C12 119.5(3) C14 C13 H13 120.2 C13 C14 H14 119.8 C15 C14 C13 120.3(3) C15 C14 H14 119.8 C10 C15 H15 119.6 C14 C15 C10 120.7(3) C14 C15 H15 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O1 1.452(2) S1 O2 1.471(2) S1 O3 1.454(2) S1 C16 1.776(3) O4 C22 1.201(4) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.524(4) C17 C18 1.570(4) C17 C22 1.538(4) C17 C23 1.565(4) C18 H18A 0.9900 C18 H18B 0.9900 C18 C19 1.552(4) C19 H19A 0.9900 C19 H19B 0.9900 C19 C20 1.542(4) C20 H20 1.0000 C20 C21 1.539(4) C20 C23 1.553(4) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.524(4) C23 C24 1.528(4) C23 C25 1.532(4) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 N1 C1 1.483(3) N1 H1A 0.97(3) N1 H1B 0.85(4) N1 H1C 0.96(5) C1 C2 1.401(4) C1 C6 1.387(4) C2 C3 1.393(4) C2 C7 1.512(4) C3 H3 0.9500 C3 C4 1.388(4) C4 H4 0.9500 C4 C5 1.388(4) C5 H5 0.9500 C5 C6 1.394(4) C6 C8 1.525(4) C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8 1.0000 C8 C9 1.518(4) C8 C10 1.521(4) C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 C11 1.390(4) C10 C15 1.399(4) C11 H11 0.9500 C11 C12 1.384(4) C12 H12 0.9500 C12 C13 1.387(5) C13 H13 0.9500 C13 C14 1.381(6) C14 H14 0.9500 C14 C15 1.378(5) C15 H15 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 _geom_hbond_publ_flag N1 H1A O2 0.97(3) 1.85(3) 2.784(3) 160(3) . yes N1 H1B O3 0.85(4) 2.03(4) 2.846(3) 161(3) 2_656 yes N1 H1C O1 0.96(5) 2.07(5) 2.867(3) 139(4) 2_646 yes