#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:17:35 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242493 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132523.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_4132523 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 'C16 H19 N O S' _chemical_formula_sum 'C16 H19 N O S' _chemical_formula_weight 273.38 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-03-12 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.0523(2) _cell_length_b 16.4230(5) _cell_length_c 17.2698(5) _cell_measurement_reflns_used 4855 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.86 _cell_measurement_theta_min 2.36 _cell_volume 1432.94(8) _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 0.999 _diffrn_measured_fraction_theta_max 1.000 _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 0.0296 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 13524 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.926 _diffrn_reflns_theta_min 2.359 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0623 before and 0.0399 after correction. The Ratio of minimum to maximum transmission is 0.8163. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.267 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.441 _exptl_crystal_size_mid 0.304 _exptl_crystal_size_min 0.235 _refine_diff_density_max 0.232 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 1261 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 3442 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.2205P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.0782 _reflns_Friedel_coverage 0.704 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 3220 _reflns_number_total 3442 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04627_si_004.cif _cod_data_source_block testo1 _cod_database_code 4132523 _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 0.951 _shelx_estimated_absorpt_t_min 0.910 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C7(H7), C14(H14) 2.b Aromatic/amide H refined with riding coordinates: C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12) 2.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C) ; _shelx_res_file ; TITL testo1_a.res in P2(1)2(1)2(1) testo1.res created by SHELXL-2017/1 at 14:18:27 on 12-Mar-2018 REM Old TITL testo1 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.087, Rweak 0.022, Alpha 0.002, Orientation as input REM Flack x = 0.141 ( 0.022 ) from Parsons' quotients REM Formula found by SHELXT: C16 N O Cl CELL 0.71073 5.0523 16.423 17.2698 90 90 90 ZERR 4 0.0002 0.0005 0.0005 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S UNIT 64 76 4 4 4 L.S. 4 PLAN 5 SIZE 0.235 0.304 0.441 TEMP -173(2) BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.043000 0.220500 FVAR 0.56063 S1 5 0.348394 0.604924 0.494924 11.00000 0.02480 0.02397 = 0.01647 -0.00145 0.00163 0.00145 O1 4 -0.026482 0.678362 0.235766 11.00000 0.01295 0.03074 = 0.02481 0.00286 -0.00057 -0.00083 N1 3 0.398189 0.665732 0.276280 11.00000 0.01196 0.02153 = 0.01849 0.00026 0.00214 0.00011 H1 2 0.550189 0.664392 0.262071 11.00000 0.03759 C1 1 0.737499 0.481183 0.243472 11.00000 0.03560 0.02805 = 0.02420 0.00162 0.00762 -0.00299 AFIX 43 H1A 2 0.881946 0.517640 0.237282 11.00000 -1.20000 AFIX 0 C2 1 0.676099 0.426638 0.184351 11.00000 0.05036 0.03851 = 0.02017 -0.00196 0.00806 0.00594 AFIX 43 H2 2 0.778764 0.426141 0.138267 11.00000 -1.20000 AFIX 0 C3 1 0.466023 0.373140 0.192481 11.00000 0.04433 0.02666 = 0.02342 -0.00711 -0.00781 0.00838 AFIX 43 H3 2 0.424240 0.335797 0.152288 11.00000 -1.20000 AFIX 0 C4 1 0.317858 0.374705 0.259746 11.00000 0.02974 0.03414 = 0.03766 -0.01013 -0.00209 -0.00539 AFIX 43 H4 2 0.172897 0.338453 0.265993 11.00000 -1.20000 AFIX 0 C5 1 0.381344 0.429316 0.318071 11.00000 0.02411 0.03826 = 0.02780 -0.00964 0.00553 -0.00569 AFIX 43 H5 2 0.278389 0.429989 0.364097 11.00000 -1.20000 AFIX 0 C6 1 0.591450 0.482904 0.310748 11.00000 0.02055 0.01924 = 0.01852 0.00076 -0.00057 0.00424 C7 1 0.674932 0.537433 0.378202 11.00000 0.01764 0.01902 = 0.02179 -0.00060 0.00123 -0.00097 AFIX 13 H7 2 0.833921 0.568966 0.361162 11.00000 -1.20000 AFIX 0 C8 1 0.758480 0.484550 0.447121 11.00000 0.02531 0.02675 = 0.02325 -0.00123 -0.00428 0.00286 AFIX 137 H8A 2 0.606029 0.453108 0.465478 11.00000 -1.50000 H8B 2 0.823474 0.519509 0.488995 11.00000 -1.50000 H8C 2 0.899360 0.447219 0.430958 11.00000 -1.50000 AFIX 0 C9 1 0.463961 0.598198 0.400887 11.00000 0.01639 0.02079 = 0.01504 -0.00235 0.00051 -0.00194 C10 1 0.338382 0.655137 0.355665 11.00000 0.01428 0.02053 = 0.01660 -0.00144 -0.00076 -0.00281 C11 1 0.148439 0.702646 0.396452 11.00000 0.01726 0.01882 = 0.02168 -0.00348 -0.00019 0.00024 AFIX 43 H11 2 0.045006 0.744293 0.373174 11.00000 -1.20000 AFIX 0 C12 1 0.131616 0.681692 0.472616 11.00000 0.02071 0.02129 = 0.02353 -0.00635 0.00173 0.00125 AFIX 43 H12 2 0.014768 0.706446 0.508718 11.00000 -1.20000 AFIX 0 C13 1 0.211730 0.676971 0.221278 11.00000 0.01592 0.01489 = 0.01953 0.00030 -0.00027 -0.00091 C14 1 0.314700 0.685423 0.139037 11.00000 0.01664 0.03047 = 0.01974 0.00175 0.00065 0.00060 AFIX 13 H14 2 0.511413 0.692021 0.140348 11.00000 -1.20000 AFIX 0 C15 1 0.191257 0.760045 0.100812 11.00000 0.04237 0.04286 = 0.02708 0.01428 0.00389 0.00612 AFIX 137 H15A 2 -0.001772 0.754210 0.100155 11.00000 -1.50000 H15B 2 0.256787 0.764923 0.047604 11.00000 -1.50000 H15C 2 0.239445 0.808946 0.130119 11.00000 -1.50000 AFIX 0 C16 1 0.245701 0.607791 0.095012 11.00000 0.05815 0.04482 = 0.02877 -0.01483 0.00870 -0.00039 AFIX 137 H16A 2 0.320840 0.560711 0.122075 11.00000 -1.50000 H16B 2 0.319029 0.610731 0.042551 11.00000 -1.50000 H16C 2 0.052888 0.602037 0.092115 11.00000 -1.50000 AFIX 0 HKLF 4 REM testo1_a.res in P2(1)2(1)2(1) REM R1 = 0.0322 for 3220 Fo > 4sig(Fo) and 0.0356 for all 3442 data REM 179 parameters refined using 0 restraints END WGHT 0.0430 0.2205 REM Highest difference peak 0.232, deepest hole -0.157, 1-sigma level 0.041 Q1 1 0.3441 0.3956 0.2165 11.00000 0.05 0.23 Q2 1 0.4063 0.6001 0.4438 11.00000 0.05 0.22 Q3 1 0.2058 0.6464 0.4799 11.00000 0.05 0.22 Q4 1 0.2534 0.6763 0.1785 11.00000 0.05 0.21 Q5 1 0.3389 0.6446 0.1195 11.00000 0.05 0.20 ; _shelx_res_checksum 28205 _shelx_hkl_file ; 1 0 0 1.10 0.60 -1 0 0 0.90 0.50 -2 0 0 1191.68 17.90 2 0 0 1199.28 18.00 3 0 0 0.30 1.40 -3 0 0 0.60 1.40 4 0 0 125.89 5.60 -4 0 0 130.69 5.50 5 0 0 -0.90 2.20 -5 0 0 1.00 2.10 -6 0 0 129.29 7.00 0 -1 0 0.30 0.10 1 -1 0 396.96 6.50 1 1 0 389.76 6.20 -1 -1 0 391.46 6.20 -1 1 0 384.46 6.50 -2 -1 0 62.09 2.50 2 -1 0 72.29 2.90 -2 1 0 70.09 2.80 2 1 0 60.69 2.70 3 1 0 160.88 5.30 3 -1 0 151.18 5.20 -3 1 0 162.58 5.30 -3 -1 0 169.18 5.20 -4 -1 0 10.60 2.40 4 1 0 13.20 2.60 -4 1 0 9.10 2.30 4 -1 0 7.70 2.30 5 -1 0 148.39 6.50 -5 1 0 144.29 6.50 5 1 0 132.39 6.50 -5 -1 0 138.09 6.20 -6 -1 0 1.90 2.30 -6 1 0 -2.60 2.10 0 -2 0 49.10 1.10 0 -2 0 46.40 1.20 -1 -2 0 13.30 0.90 -1 2 0 16.60 1.40 1 2 0 11.20 0.90 2 2 0 203.48 4.80 -2 2 0 204.88 5.30 2 -2 0 214.78 5.30 -2 -2 0 208.28 4.80 3 2 0 251.57 6.60 3 -2 0 243.48 6.80 -3 2 0 242.58 6.90 -3 -2 0 250.47 6.40 -4 2 0 0.20 1.70 4 -2 0 -0.30 1.70 -4 -2 0 -1.70 1.60 4 2 0 -2.10 1.80 -5 2 0 5.70 2.60 -5 -2 0 5.50 2.30 5 -2 0 5.40 2.60 -6 -2 0 24.10 3.90 -6 -2 0 21.00 3.30 -6 2 0 25.30 4.30 0 3 0 0.20 0.30 0 -3 0 0.70 0.30 0 -3 0 1.00 0.30 1 -3 0 9780.32 133.89 -1 3 0 9621.94 132.59 1 3 0 9999.00 131.39 -1 -3 0 9990.60 133.49 -1 -3 0 9710.83 131.29 -2 -3 0 657.63 10.80 2 -3 0 665.63 11.60 -2 3 0 656.23 11.80 2 3 0 674.33 10.90 3 3 0 1.90 1.40 -3 -3 0 0.60 1.20 -3 3 0 1.40 1.80 3 -3 0 0.10 1.50 4 -3 0 62.79 4.20 4 3 0 64.29 4.30 -4 3 0 69.29 4.60 -4 -3 0 60.59 3.90 -5 -3 0 88.99 5.20 -5 3 0 91.89 5.60 -6 -3 0 5.90 2.40 -6 -3 0 8.30 2.90 -6 3 0 5.60 3.00 0 -4 0 1717.53 23.00 0 -4 0 1695.23 22.60 0 4 0 1717.53 23.10 1 -4 0 143.49 3.70 -1 -4 0 162.98 3.60 -1 -4 0 157.28 3.30 -1 4 0 149.99 4.00 1 4 0 158.18 3.40 2 -4 0 100.29 3.60 2 4 0 88.79 3.00 -2 4 0 86.29 3.70 -2 -4 0 87.49 2.90 3 4 0 14.80 2.00 3 -4 0 17.30 2.40 -3 4 0 16.70 2.60 -3 -4 0 20.40 2.10 4 4 0 75.99 4.50 -4 4 0 85.29 5.30 -4 -4 0 79.29 4.20 4 -4 0 92.09 5.10 -5 -4 0 41.80 4.00 5 -4 0 41.40 4.50 -5 4 0 50.39 5.10 -5 -4 0 43.90 4.10 -6 -4 0 85.99 5.70 -6 4 0 82.99 7.00 -6 -4 0 78.69 5.40 0 5 0 0.90 0.40 0 5 0 -0.20 0.70 0 -5 0 0.30 0.50 0 -5 0 1.00 0.60 -1 -5 0 1118.19 16.10 1 5 0 1111.09 15.90 -1 5 0 1109.19 16.90 -1 -5 0 1114.29 15.90 1 -5 0 1090.09 16.60 2 5 0 220.28 5.00 -2 -5 0 206.38 4.80 2 -5 0 212.58 5.60 -2 5 0 185.38 5.70 -2 -5 0 204.18 5.10 3 -5 0 9.90 2.00 -3 -5 0 16.80 2.10 -3 5 0 11.40 2.40 -3 -5 0 14.00 1.80 3 5 0 16.90 2.10 -4 5 0 8.00 2.60 -4 -5 0 8.60 2.00 -4 -5 0 8.10 2.00 4 5 0 6.80 2.20 4 -5 0 10.30 2.40 -5 5 0 13.70 3.20 -5 -5 0 21.30 3.00 5 -5 0 20.80 3.40 -5 -5 0 16.40 2.80 -6 -5 0 6.50 2.30 6 -5 0 3.10 2.50 -6 5 0 5.80 2.90 -6 -5 0 5.60 2.50 0 6 0 457.25 8.00 0 6 0 451.25 6.70 0 -6 0 470.15 7.90 0 -6 0 469.95 7.40 1 -6 0 417.76 8.00 1 6 0 437.26 7.40 -1 -6 0 424.26 7.60 -1 6 0 427.46 8.30 -1 -6 0 429.66 7.40 2 -6 0 1.70 1.10 -2 6 0 6.60 1.70 2 6 0 2.00 1.00 -2 -6 0 2.10 1.00 -2 -6 0 3.00 0.90 3 -6 0 98.49 4.60 -3 -6 0 99.69 3.90 -3 6 0 103.59 5.10 3 6 0 95.49 4.10 -3 -6 0 95.89 4.10 -4 6 0 23.60 3.70 -4 -6 0 26.60 2.90 4 -6 0 26.70 3.50 -4 -6 0 21.50 2.70 -5 -6 0 29.70 3.80 5 -6 0 29.30 3.90 -5 -6 0 29.70 3.40 -5 6 0 30.10 4.30 -6 6 0 32.60 5.20 6 -6 0 24.40 4.10 -6 -6 0 26.40 3.80 -6 -6 0 28.30 4.00 0 -7 0 7.20 1.00 0 7 0 0.40 0.40 0 -7 0 0.00 0.60 0 7 0 1.40 0.90 -1 -7 0 7.80 1.10 -1 -7 0 7.70 1.10 -1 7 0 7.30 1.40 1 -7 0 6.60 1.20 1 7 0 6.90 1.10 -2 -7 0 75.59 3.10 2 -7 0 73.89 3.60 -2 -7 0 73.19 2.80 -2 7 0 66.19 3.90 2 7 0 72.09 2.90 3 -7 0 1.20 1.50 3 7 0 2.30 1.50 -3 -7 0 -0.10 1.10 -3 -7 0 1.20 1.20 -3 7 0 -1.00 1.80 -4 7 0 92.39 6.00 4 -7 0 104.69 5.50 -4 -7 0 93.19 4.80 -4 -7 0 100.09 4.50 -5 7 0 0.00 2.70 5 -7 0 -0.50 2.10 -5 -7 0 4.50 1.90 -5 -7 0 0.60 1.70 -6 7 0 18.80 4.20 -6 -7 0 21.90 3.60 6 -7 0 20.10 3.80 0 -8 0 24.80 1.70 0 8 0 27.10 1.20 0 8 0 28.30 2.00 0 -8 0 26.00 1.60 -1 -8 0 79.59 2.80 1 -8 0 81.79 3.20 -1 -8 0 77.49 2.90 1 8 0 80.19 2.90 -1 8 0 79.59 3.50 2 -8 0 28.20 2.60 -2 8 0 16.80 2.40 -2 -8 0 25.30 2.30 -2 -8 0 24.60 1.90 2 8 0 28.70 2.20 -3 8 0 11.70 2.70 3 -8 0 10.10 2.20 -3 -8 0 9.90 1.90 3 8 0 12.00 2.10 -3 -8 0 11.20 1.80 -4 -8 0 9.00 2.00 -4 8 0 9.90 3.20 -4 -8 0 9.00 2.20 4 -8 0 13.00 2.70 -5 8 0 9.70 3.50 -5 -8 0 1.70 1.90 -5 -8 0 7.10 2.20 5 -8 0 5.20 2.60 6 -8 0 1.40 2.80 -6 -8 0 2.70 2.10 -6 8 0 1.10 3.40 -6 -8 0 5.30 2.40 0 9 0 1.00 1.00 0 -9 0 0.70 0.80 0 -9 0 1.10 0.80 0 9 0 0.60 0.50 1 -9 0 0.90 1.00 -1 9 0 3.70 1.50 -1 -9 0 1.00 0.80 1 9 0 1.60 1.00 -1 -9 0 3.40 1.00 -2 -9 0 9.60 1.50 -2 -9 0 9.00 1.70 2 -9 0 9.60 1.90 -2 9 0 10.90 2.30 2 9 0 10.10 1.60 -3 -9 0 11.90 1.90 3 -9 0 12.80 2.60 -3 -9 0 14.50 2.30 -3 9 0 12.10 3.00 4 -9 0 19.60 3.30 -4 -9 0 19.30 2.80 -4 9 0 16.70 3.70 -4 -9 0 20.20 2.60 -5 -9 0 13.70 2.60 -5 -9 0 13.30 2.80 5 -9 0 11.00 2.90 -5 9 0 17.60 3.70 6 -9 0 50.79 5.70 -6 -9 0 71.29 5.20 -6 9 0 51.09 6.10 -6 -9 0 56.29 5.60 0 -10 0 591.44 11.00 0 10 0 606.24 11.10 0 -10 0 585.34 10.10 0 10 0 594.34 8.80 1 10 0 10.10 1.60 -1 -10 0 8.20 1.40 -1 -10 0 7.80 1.30 -1 10 0 9.80 1.90 1 -10 0 9.00 1.70 -2 -10 0 14.60 2.00 2 10 0 16.60 2.00 -2 -10 0 14.30 1.80 2 -10 0 16.90 2.40 -2 10 0 17.10 3.00 -3 -10 0 28.00 2.70 -3 10 0 20.40 3.50 -3 -10 0 20.80 2.60 3 -10 0 31.90 3.40 -4 -10 0 3.80 2.00 -4 10 0 6.60 2.80 4 -10 0 3.40 2.20 -4 -10 0 5.20 1.80 -5 10 0 18.00 4.00 -5 -10 0 19.50 3.50 5 -10 0 13.20 3.10 -5 -10 0 18.60 2.90 0 11 0 -0.60 1.20 0 -11 0 -0.50 0.90 0 -11 0 0.00 0.90 0 11 0 0.60 0.60 -1 -11 0 278.07 6.60 1 11 0 269.97 6.70 -1 -11 0 283.77 6.70 1 -11 0 273.37 7.30 -1 11 0 279.47 7.70 -2 -11 0 18.40 2.00 -2 -11 0 18.80 2.30 -2 11 0 18.90 2.90 2 -11 0 16.50 2.50 2 11 0 18.80 2.20 3 -11 0 0.60 1.60 -3 11 0 -0.90 2.00 -3 -11 0 0.80 1.40 -3 -11 0 -1.00 1.00 -4 11 0 -0.60 2.50 -4 -11 0 0.50 1.60 -4 -11 0 0.10 1.30 4 -11 0 0.70 1.80 5 -11 0 54.69 5.40 -5 11 0 45.90 5.60 -5 -11 0 56.09 4.10 -5 -11 0 60.29 5.50 0 -12 0 149.88 5.00 0 -12 0 141.39 4.40 0 12 0 138.59 5.10 -1 -12 0 5.50 1.40 -1 -12 0 6.30 1.50 1 -12 0 3.90 1.40 -1 12 0 8.90 2.30 1 12 0 6.30 1.60 1 12 0 6.30 1.10 -2 -12 0 1.20 1.10 -2 -12 0 1.00 1.30 2 -12 0 -0.30 1.30 -2 12 0 -1.60 2.00 3 -12 0 65.89 4.60 -3 -12 0 64.79 4.00 -3 -12 0 66.99 3.60 -3 12 0 61.69 5.60 -4 -12 0 0.20 1.70 -4 -12 0 1.20 1.50 4 -12 0 1.80 2.00 -4 12 0 -3.50 2.10 -5 -12 0 6.10 2.70 5 -12 0 0.00 2.20 -5 12 0 -0.40 2.70 -5 -12 0 4.30 1.90 0 -13 0 -0.10 1.10 0 -13 0 -1.20 1.00 0 13 0 0.60 1.50 1 13 0 195.58 6.00 -1 -13 0 194.68 5.90 1 -13 0 192.68 6.40 -1 13 0 204.08 6.90 -1 -13 0 194.48 5.70 -2 -13 0 337.87 8.50 -2 -13 0 335.27 8.10 2 -13 0 334.47 9.30 -2 13 0 309.37 9.60 -3 13 0 11.70 3.00 3 -13 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6.10 2.70 0 11 18 4.90 2.80 -1 11 18 51.19 5.70 -1 -11 -18 49.50 5.30 -1 11 18 38.90 4.60 1 11 18 46.30 5.20 1 11 18 45.00 5.20 2 -11 18 9.90 2.60 -2 11 18 8.40 3.30 -2 -11 -18 12.20 3.20 -2 11 18 16.20 3.50 2 11 18 16.80 3.70 2 11 18 13.80 3.50 -2 -11 18 8.10 3.50 0 12 18 5.80 2.90 0 12 18 2.90 2.80 -1 12 18 38.80 4.70 -1 -12 -18 36.70 4.60 -1 12 18 32.80 4.60 1 12 18 36.40 4.70 1 12 18 32.90 4.50 0 13 18 33.10 4.80 0 13 18 29.60 4.60 0 -13 -18 21.30 3.80 0 0 19 -0.30 1.80 0 0 19 2.00 1.70 -1 0 19 0.20 1.30 -1 0 19 1.20 2.10 1 0 19 3.70 2.10 1 0 19 1.60 2.00 -2 0 19 75.69 5.60 2 0 19 80.29 5.20 2 0 19 82.89 5.60 3 0 19 23.20 3.60 3 0 19 16.80 3.80 0 -1 19 56.69 4.90 0 1 19 47.20 3.90 0 1 19 51.99 4.80 0 -1 19 46.50 3.60 1 -1 19 6.60 2.20 -1 1 19 8.40 2.70 -1 1 19 8.00 2.00 1 -1 19 8.70 2.40 1 1 19 5.30 2.30 -1 -1 19 9.80 1.80 1 1 19 6.10 2.40 -1 -1 19 7.20 2.60 2 -1 19 6.10 2.20 2 -1 19 6.90 2.70 -2 1 19 9.80 2.40 -2 1 19 13.30 3.30 -2 -1 19 9.60 3.10 2 1 19 10.10 2.50 2 1 19 12.60 3.10 3 -1 19 19.60 3.30 3 -1 19 15.50 3.70 3 1 19 17.80 4.00 3 1 19 17.60 3.30 0 -2 19 34.80 3.90 0 -2 19 43.10 3.30 0 2 19 32.30 3.80 0 2 19 41.90 3.80 1 -2 19 114.39 5.60 1 -2 19 105.69 5.60 -1 2 19 112.49 4.90 -1 2 19 101.09 6.00 -1 -2 19 105.69 6.00 1 2 19 104.29 5.60 1 2 19 94.99 5.70 -2 2 19 -0.20 1.30 -2 2 19 0.00 2.20 2 -2 19 3.50 2.40 2 -2 19 2.00 1.80 2 2 19 -1.70 1.80 -2 -2 19 -2.60 2.20 -2 -2 19 -0.80 2.00 2 2 19 3.70 2.40 3 -2 19 23.50 4.20 3 -2 19 17.40 3.10 3 2 19 14.70 3.70 3 2 19 20.30 3.60 0 3 19 52.89 4.90 0 3 19 48.80 4.20 0 -3 19 48.70 4.40 0 -3 19 48.90 3.50 -1 3 19 12.00 2.30 1 -3 19 10.60 2.50 1 -3 19 12.50 2.70 -1 3 19 12.10 3.10 1 3 19 10.00 2.80 1 3 19 8.10 2.50 -1 -3 19 8.30 2.60 -2 3 19 0.00 1.40 2 -3 19 1.00 1.70 -2 3 19 -1.40 2.20 2 -3 19 0.70 2.30 2 3 19 -3.10 1.70 -2 -3 19 -0.90 2.00 2 3 19 -1.50 2.00 3 -3 19 20.00 4.10 3 -3 19 15.50 2.90 -3 -3 19 22.10 3.60 3 3 19 17.90 3.40 3 3 19 16.90 3.80 0 4 19 5.50 2.30 0 4 19 7.30 2.20 0 -4 19 7.30 2.00 0 -4 19 5.00 2.10 -1 4 19 42.50 4.90 1 -4 19 44.80 4.00 1 -4 19 42.90 4.00 -1 4 19 45.90 4.00 -1 -4 19 34.10 3.80 1 4 19 43.10 4.40 1 4 19 37.80 4.30 -2 4 19 26.90 3.20 2 -4 19 38.40 4.10 -2 4 19 26.80 4.10 2 -4 19 27.60 3.90 -2 -4 19 25.50 3.90 2 4 19 31.00 4.30 2 4 19 34.60 4.40 3 -4 19 12.80 2.70 -3 4 19 10.80 2.40 3 -4 19 5.30 3.20 3 4 19 7.30 2.80 -3 -4 19 16.10 3.30 3 4 19 14.70 3.70 0 5 19 28.50 3.90 0 5 19 31.60 3.80 0 -5 19 24.80 3.30 -1 5 19 107.69 5.50 1 -5 19 120.49 5.60 -1 5 19 108.89 6.50 1 -5 19 109.49 5.40 1 5 19 95.59 6.00 1 5 19 104.59 5.90 -1 -5 19 106.89 5.50 -2 5 19 28.90 4.30 -2 5 19 26.80 3.30 2 -5 19 34.10 3.70 2 -5 19 27.80 3.90 2 5 19 36.80 4.60 2 5 19 25.10 3.80 -2 -5 19 36.70 4.70 3 -5 19 4.60 3.10 -3 5 19 9.10 2.40 -3 -5 19 5.60 2.70 3 5 19 8.70 3.40 3 5 19 8.80 3.00 0 6 19 0.20 2.20 0 6 19 -0.10 1.70 0 -6 19 1.70 1.80 1 -6 19 9.60 2.40 -1 6 19 12.10 2.50 -1 6 19 10.30 3.10 -1 -6 19 6.50 2.40 1 6 19 6.40 2.50 1 6 19 6.60 2.30 2 -6 19 2.40 2.30 -2 6 19 7.10 3.10 -2 6 19 4.00 2.00 -2 -6 19 2.50 2.80 2 6 19 5.00 2.50 2 6 19 5.20 2.80 3 -6 19 61.79 6.00 -3 6 19 64.19 4.70 -3 -6 -19 65.79 6.00 3 6 19 62.59 5.90 -3 -6 19 62.69 5.70 3 6 19 65.29 6.30 0 7 19 46.00 5.10 0 7 19 31.70 3.90 1 -7 19 20.90 2.90 -1 7 19 20.00 3.20 -1 7 19 19.90 3.80 1 7 19 19.50 3.70 1 7 19 17.80 3.30 -2 7 19 29.00 3.70 2 -7 19 29.50 3.90 -2 7 19 22.00 4.20 -2 -7 19 21.70 3.90 2 7 19 19.90 3.70 2 7 19 24.60 4.10 0 8 19 11.60 2.90 0 8 19 13.30 3.20 -1 8 19 32.10 4.50 -1 8 19 42.00 4.50 1 8 19 38.10 4.50 1 8 19 36.00 4.50 2 -8 19 16.00 3.30 -2 -8 -19 20.60 4.10 -2 8 19 25.70 3.60 -2 8 19 25.80 4.30 -2 -8 19 17.40 3.70 2 8 19 21.10 4.00 2 8 19 24.40 4.30 0 9 19 50.09 4.90 0 9 19 46.30 5.30 -1 9 19 30.80 4.60 -1 9 19 26.60 3.80 1 9 19 31.70 4.30 1 9 19 29.80 4.20 2 -9 19 23.60 3.50 -2 9 19 24.10 4.50 -2 9 19 20.80 3.50 -2 -9 -19 22.40 3.80 2 9 19 21.80 4.20 -2 -9 19 27.90 4.50 2 9 19 32.80 4.70 0 10 19 26.50 4.30 0 10 19 23.50 3.80 -1 10 19 22.90 4.20 -1 10 19 19.60 3.70 1 10 19 15.90 3.60 1 10 19 23.10 4.00 0 11 19 45.30 5.10 0 11 19 51.19 5.70 -1 11 19 12.10 3.70 -1 11 19 8.20 2.90 1 11 19 9.70 3.20 1 11 19 13.30 3.70 0 0 20 128.59 5.60 0 0 20 116.19 6.20 -1 0 20 0.10 2.20 1 0 20 1.70 2.10 -1 0 20 1.00 1.50 1 0 20 0.30 2.00 2 0 20 15.30 3.40 -2 0 20 21.20 3.90 2 0 20 22.20 3.50 3 0 20 15.80 3.30 3 0 20 18.10 4.10 0 1 20 54.29 4.90 0 -1 20 55.59 4.00 0 -1 20 50.99 4.70 0 1 20 49.80 4.00 -1 1 20 19.40 2.60 -1 1 20 18.70 3.60 1 -1 20 14.30 3.10 1 -1 20 17.50 3.00 -1 -1 20 17.00 3.40 1 1 20 23.40 3.40 1 1 20 13.10 3.10 -2 1 20 30.80 4.50 2 -1 20 25.40 3.90 2 -1 20 28.00 3.80 2 1 20 22.20 3.70 -2 -1 20 36.40 4.50 2 1 20 27.30 4.00 3 -1 20 48.40 4.90 3 -1 20 37.90 5.10 3 1 20 43.40 4.80 3 1 20 38.70 5.10 0 2 20 11.10 3.00 0 -2 20 12.40 2.80 0 2 20 9.70 2.40 0 -2 20 13.20 2.40 -1 2 20 51.69 5.10 1 -2 20 45.30 4.40 1 -2 20 44.40 4.20 -1 2 20 46.00 3.60 1 2 20 43.70 4.30 -1 -2 20 49.30 5.00 1 2 20 42.40 4.50 2 -2 20 38.80 4.20 -2 2 20 43.40 3.30 2 -2 20 43.20 4.70 -2 2 20 48.40 5.30 -2 -2 20 41.00 4.60 2 2 20 40.10 4.70 2 2 20 51.39 5.20 3 -2 20 56.69 6.00 3 -2 20 59.29 5.40 3 2 20 55.39 5.40 3 2 20 56.79 6.00 0 3 20 20.40 3.10 0 -3 20 26.80 3.60 0 -3 20 25.70 2.90 0 3 20 23.80 3.70 1 -3 20 14.90 2.90 1 -3 20 12.70 2.70 -1 3 20 16.90 2.70 -1 3 20 15.80 3.50 1 3 20 22.00 3.50 1 3 20 17.70 3.40 -1 -3 20 20.90 3.40 2 -3 20 100.79 5.60 2 -3 20 94.69 6.20 -2 3 20 111.49 6.80 -2 3 20 106.89 4.90 2 3 20 95.99 6.30 2 3 20 112.99 6.60 3 -3 20 18.50 4.20 3 -3 20 21.80 3.50 3 3 20 15.80 3.40 3 3 20 20.90 4.20 0 4 20 27.70 3.60 0 -4 20 26.60 3.60 0 4 20 28.90 4.10 1 -4 20 27.30 3.50 1 -4 20 23.10 3.30 -1 4 20 23.30 4.00 -1 4 20 22.00 3.00 1 4 20 22.50 3.50 1 4 20 28.90 4.20 -1 -4 20 21.30 3.50 -2 4 20 5.20 2.00 -2 4 20 9.70 3.20 2 -4 20 4.50 2.20 2 -4 20 5.00 2.80 -2 -4 20 1.40 2.80 2 4 20 4.70 2.70 2 4 20 6.30 2.60 0 5 20 8.70 2.90 0 5 20 5.60 2.40 0 -5 20 5.30 2.30 -1 5 20 135.79 7.40 -1 5 20 130.49 6.10 1 -5 20 146.89 6.30 1 -5 20 132.99 6.00 1 5 20 140.59 7.40 1 5 20 122.09 6.50 -1 -5 20 117.39 6.00 -2 5 20 2.80 1.90 2 -5 20 0.70 2.40 -2 5 20 0.70 2.70 -2 -5 20 -3.60 2.30 2 5 20 -0.20 2.30 2 5 20 1.30 2.20 0 6 20 76.69 5.80 0 6 20 79.79 5.30 1 -6 20 18.50 3.00 -1 6 20 18.70 3.80 -1 6 20 22.60 3.30 1 6 20 14.00 3.20 -1 -6 20 21.00 3.40 1 6 20 20.50 4.10 -2 6 20 8.80 2.50 -2 6 20 4.60 3.00 2 -6 20 13.20 3.30 -2 -6 20 4.10 3.10 2 6 20 5.10 2.80 2 6 20 6.80 3.00 0 7 20 13.60 3.10 0 7 20 16.10 3.50 -1 7 20 15.00 3.10 -1 7 20 8.80 3.00 1 7 20 9.70 3.10 1 7 20 12.70 3.10 -2 7 20 16.60 3.90 -2 7 20 15.20 3.00 2 -7 20 15.80 3.30 -2 -7 20 10.60 3.30 2 7 20 12.20 3.40 2 7 20 12.30 3.30 0 8 20 194.08 8.20 0 8 20 198.78 8.90 -1 8 20 43.60 4.50 -1 8 20 39.40 5.10 1 8 20 55.49 6.00 1 8 20 46.00 5.10 -2 -8 20 31.80 5.00 0 9 20 34.10 4.50 0 9 20 24.20 4.10 -1 9 20 35.50 4.50 -1 9 20 39.10 5.30 1 9 20 44.00 5.30 1 9 20 38.60 4.90 0 10 20 130.19 7.10 0 10 20 123.29 7.30 0 0 21 -0.20 2.00 0 0 21 0.10 1.70 -1 0 21 0.90 2.40 1 0 21 2.30 2.40 1 0 21 -2.10 2.00 -2 0 21 80.69 6.80 2 0 21 73.89 5.50 2 0 21 76.49 6.00 0 1 21 4.10 2.20 0 -1 21 2.20 2.20 0 -1 21 2.30 1.80 0 1 21 3.20 1.90 1 -1 21 35.50 4.30 -1 1 21 31.70 4.40 1 -1 21 34.10 3.90 -1 1 21 32.60 3.30 -1 -1 21 38.30 4.70 1 1 21 33.60 4.30 1 1 21 36.90 4.10 -2 1 21 24.10 4.30 2 -1 21 16.00 3.60 2 -1 21 18.60 3.50 -2 -1 21 16.10 3.60 2 1 21 17.30 3.40 2 1 21 16.80 3.60 0 2 21 17.40 3.50 0 -2 21 10.90 2.80 0 2 21 8.60 2.40 0 -2 21 10.70 2.40 1 -2 21 15.40 3.00 -1 2 21 18.00 2.70 1 -2 21 18.80 3.30 -1 2 21 15.30 3.50 1 2 21 17.50 3.30 1 2 21 21.60 3.80 -1 -2 21 17.70 3.40 -2 2 21 8.00 3.20 2 -2 21 11.90 3.00 2 -2 21 6.00 3.00 2 2 21 8.50 3.10 2 2 21 7.40 2.80 -2 -2 21 10.20 3.30 0 3 21 69.49 4.80 0 3 21 72.69 6.20 0 -3 21 68.09 5.60 -1 3 21 24.90 3.20 -1 3 21 20.10 3.90 1 -3 21 15.60 3.00 1 -3 21 16.90 3.20 1 3 21 18.50 3.60 1 3 21 17.30 3.20 -1 -3 21 15.90 3.30 -2 3 21 3.50 1.80 -2 3 21 4.00 3.00 2 -3 21 4.30 2.30 2 -3 21 3.30 2.80 2 3 21 -1.00 2.40 2 3 21 2.00 2.40 0 4 21 78.79 5.90 0 -4 21 80.89 5.50 0 4 21 82.29 5.30 1 -4 21 23.10 3.40 -1 4 21 25.70 4.30 -1 4 21 24.80 3.30 1 -4 21 21.60 3.40 -1 -4 21 25.30 3.90 1 4 21 20.70 3.60 1 4 21 31.40 4.50 -2 4 21 49.99 5.60 -2 4 21 41.00 3.80 2 -4 21 43.40 4.90 2 -4 21 46.50 4.70 2 4 21 45.60 5.10 2 4 21 47.40 5.40 0 5 21 10.40 2.80 0 -5 21 12.40 2.90 0 5 21 13.20 3.30 1 -5 21 26.80 3.50 -1 5 21 25.70 4.40 -1 5 21 21.40 3.30 1 5 21 27.50 4.30 -1 -5 21 27.80 3.80 1 5 21 17.40 3.40 -2 5 21 34.70 4.90 2 -5 21 34.90 4.50 -2 5 21 29.40 3.70 2 5 21 32.40 4.60 2 5 21 28.10 4.20 0 6 21 23.10 3.60 0 6 21 26.80 4.20 -1 6 21 2.10 2.70 -1 6 21 8.40 2.60 1 6 21 5.80 2.80 1 6 21 5.60 3.00 0 7 21 149.49 7.80 0 7 21 142.79 7.10 -1 7 21 35.40 4.20 -1 7 21 20.70 4.00 1 7 21 31.00 4.30 1 7 21 34.40 4.80 0 8 21 106.69 6.60 0 8 21 115.79 7.20 0 0 22 283.27 8.70 0 0 22 274.77 10.10 1 0 22 52.59 4.90 -1 0 22 48.40 5.30 1 0 22 41.90 4.70 0 1 22 25.60 3.30 0 1 22 19.30 3.60 0 -1 22 23.30 3.10 0 -1 22 16.00 3.50 1 -1 22 64.49 5.60 1 -1 22 54.79 5.00 -1 1 22 44.40 5.20 1 1 22 58.19 5.30 1 1 22 68.29 6.10 -1 -1 22 56.79 5.70 0 2 22 -1.30 2.30 0 2 22 2.00 2.10 0 -2 22 3.40 2.30 1 -2 22 23.20 3.70 -1 2 22 15.70 3.90 -1 2 22 24.70 3.10 1 -2 22 23.90 3.50 1 2 22 21.00 3.70 1 2 22 30.30 4.50 -1 -2 22 21.60 3.80 0 3 22 3.20 2.10 0 -3 22 7.00 2.60 0 3 22 1.50 2.70 1 -3 22 53.39 4.80 -1 3 22 57.29 6.00 -1 3 22 47.90 4.40 1 -3 22 54.39 5.00 -1 -3 22 44.90 5.00 1 3 22 46.80 4.80 1 3 22 58.79 5.90 0 4 22 80.39 6.20 0 -4 22 76.59 5.40 0 4 22 78.99 5.30 -1 4 22 38.00 4.00 1 -4 22 41.90 4.30 -1 4 22 37.40 5.10 1 -4 22 46.10 4.60 1 4 22 37.50 4.50 -1 -4 22 45.20 4.90 1 4 22 42.70 5.00 0 5 22 10.20 3.10 0 5 22 22.00 3.60 0 -5 22 17.20 4.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 29374 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+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 S1 S 0.34839(10) 0.60492(3) 0.49492(3) 0.02175(13) Uani 1 1 d . O1 O -0.0265(3) 0.67836(10) 0.23577(8) 0.0228(3) Uani 1 1 d . N1 N 0.3982(3) 0.66573(10) 0.27628(10) 0.0173(3) Uani 1 1 d . H1 H 0.550(7) 0.6644(17) 0.2621(16) 0.038(8) Uiso 1 1 d . C1 C 0.7375(5) 0.48118(14) 0.24347(12) 0.0293(5) Uani 1 1 d . H1A H 0.881946 0.517640 0.237282 0.035 Uiso 1 1 calc R C2 C 0.6761(6) 0.42664(15) 0.18435(13) 0.0363(6) Uani 1 1 d . H2 H 0.778764 0.426141 0.138267 0.044 Uiso 1 1 calc R C3 C 0.4660(5) 0.37314(14) 0.19248(13) 0.0315(5) Uani 1 1 d . H3 H 0.424240 0.335797 0.152288 0.038 Uiso 1 1 calc R C4 C 0.3179(5) 0.37471(15) 0.25975(14) 0.0338(5) Uani 1 1 d . H4 H 0.172897 0.338453 0.265993 0.041 Uiso 1 1 calc R C5 C 0.3813(5) 0.42932(14) 0.31807(13) 0.0301(5) Uani 1 1 d . H5 H 0.278389 0.429989 0.364097 0.036 Uiso 1 1 calc R C6 C 0.5914(4) 0.48290(12) 0.31075(11) 0.0194(4) Uani 1 1 d . C7 C 0.6749(4) 0.53743(11) 0.37820(11) 0.0195(4) Uani 1 1 d . H7 H 0.833921 0.568966 0.361162 0.023 Uiso 1 1 calc R C8 C 0.7585(5) 0.48455(13) 0.44712(12) 0.0251(5) Uani 1 1 d . H8A H 0.606029 0.453108 0.465478 0.038 Uiso 1 1 calc GR H8B H 0.823474 0.519509 0.488995 0.038 Uiso 1 1 calc GR H8C H 0.899360 0.447219 0.430958 0.038 Uiso 1 1 calc GR C9 C 0.4640(4) 0.59820(12) 0.40089(10) 0.0174(4) Uani 1 1 d . C10 C 0.3384(4) 0.65514(11) 0.35566(10) 0.0171(4) Uani 1 1 d . C11 C 0.1484(4) 0.70265(11) 0.39645(11) 0.0193(4) Uani 1 1 d . H11 H 0.045006 0.744293 0.373174 0.023 Uiso 1 1 calc R C12 C 0.1316(4) 0.68169(12) 0.47262(12) 0.0218(4) Uani 1 1 d . H12 H 0.014768 0.706446 0.508718 0.026 Uiso 1 1 calc R C13 C 0.2117(4) 0.67697(11) 0.22128(11) 0.0168(4) Uani 1 1 d . C14 C 0.3147(4) 0.68542(12) 0.13904(11) 0.0223(4) Uani 1 1 d . H14 H 0.511413 0.692021 0.140348 0.027 Uiso 1 1 calc R C15 C 0.1913(6) 0.76005(15) 0.10081(14) 0.0374(6) Uani 1 1 d . H15A H -0.001772 0.754210 0.100155 0.056 Uiso 1 1 calc GR H15B H 0.256787 0.764923 0.047604 0.056 Uiso 1 1 calc GR H15C H 0.239445 0.808946 0.130119 0.056 Uiso 1 1 calc GR C16 C 0.2457(6) 0.60779(17) 0.09501(14) 0.0439(6) Uani 1 1 d . H16A H 0.320840 0.560711 0.122075 0.066 Uiso 1 1 calc GR H16B H 0.319029 0.610731 0.042551 0.066 Uiso 1 1 calc GR H16C H 0.052888 0.602037 0.092115 0.066 Uiso 1 1 calc GR 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 0.0248(2) 0.0240(2) 0.0165(2) -0.00145(19) 0.0016(2) 0.0014(2) O1 0.0129(7) 0.0307(8) 0.0248(8) 0.0029(6) -0.0006(6) -0.0008(6) N1 0.0120(8) 0.0215(8) 0.0185(8) 0.0003(6) 0.0021(6) 0.0001(6) C1 0.0356(12) 0.0280(12) 0.0242(10) 0.0016(9) 0.0076(9) -0.0030(10) C2 0.0504(16) 0.0385(12) 0.0202(10) -0.0020(9) 0.0081(11) 0.0059(12) C3 0.0443(14) 0.0267(11) 0.0234(11) -0.0071(9) -0.0078(10) 0.0084(10) C4 0.0297(12) 0.0341(12) 0.0377(12) -0.0101(10) -0.0021(10) -0.0054(10) C5 0.0241(11) 0.0383(12) 0.0278(11) -0.0096(9) 0.0055(9) -0.0057(10) C6 0.0206(10) 0.0192(9) 0.0185(9) 0.0008(7) -0.0006(7) 0.0042(8) C7 0.0176(9) 0.0190(9) 0.0218(9) -0.0006(7) 0.0012(8) -0.0010(8) C8 0.0253(11) 0.0267(10) 0.0232(10) -0.0012(8) -0.0043(8) 0.0029(9) C9 0.0164(9) 0.0208(9) 0.0150(8) -0.0024(8) 0.0005(7) -0.0019(8) C10 0.0143(8) 0.0205(8) 0.0166(8) -0.0014(7) -0.0008(8) -0.0028(8) C11 0.0173(9) 0.0188(8) 0.0217(9) -0.0035(7) -0.0002(9) 0.0002(8) C12 0.0207(10) 0.0213(9) 0.0235(9) -0.0064(8) 0.0017(9) 0.0013(8) C13 0.0159(9) 0.0149(8) 0.0195(9) 0.0003(7) -0.0003(7) -0.0009(7) C14 0.0166(10) 0.0305(10) 0.0197(9) 0.0018(8) 0.0007(8) 0.0006(9) C15 0.0424(15) 0.0429(13) 0.0271(11) 0.0143(10) 0.0039(11) 0.0061(12) C16 0.0582(17) 0.0448(14) 0.0288(12) -0.0148(11) 0.0087(12) -0.0004(14) 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 C12 S1 C9 92.96(10) C10 N1 H1 120(2) C13 N1 H1 117(2) C13 N1 C10 123.33(17) C2 C1 H1A 119.6 C6 C1 H1A 119.6 C6 C1 C2 120.8(2) C1 C2 H2 119.9 C3 C2 C1 120.3(2) C3 C2 H2 119.9 C2 C3 H3 120.4 C4 C3 C2 119.2(2) C4 C3 H3 120.4 C3 C4 H4 120.1 C3 C4 C5 119.8(2) C5 C4 H4 120.1 C4 C5 H5 119.3 C6 C5 C4 121.5(2) C6 C5 H5 119.3 C1 C6 C5 118.36(19) C1 C6 C7 120.48(19) C5 C6 C7 120.95(18) C6 C7 H7 107.5 C6 C7 C8 109.62(16) C8 C7 H7 107.5 C9 C7 C6 112.93(17) C9 C7 H7 107.5 C9 C7 C8 111.53(16) C7 C8 H8A 109.5 C7 C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C7 C9 S1 121.57(14) C10 C9 S1 109.54(14) C10 C9 C7 128.88(17) N1 C10 C11 123.79(17) C9 C10 N1 122.42(18) C9 C10 C11 113.78(17) C10 C11 H11 123.8 C12 C11 C10 112.42(18) C12 C11 H11 123.8 S1 C12 H12 124.4 C11 C12 S1 111.28(15) C11 C12 H12 124.4 O1 C13 N1 122.84(18) O1 C13 C14 121.59(17) N1 C13 C14 115.55(17) C13 C14 H14 109.2 C13 C14 C15 109.76(18) C13 C14 C16 108.15(18) C15 C14 H14 109.2 C16 C14 H14 109.2 C16 C14 C15 111.3(2) C14 C15 H15A 109.5 C14 C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C14 C16 H16A 109.5 C14 C16 H16B 109.5 C14 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C9 1.7293(19) S1 C12 1.714(2) O1 C13 1.229(2) N1 H1 0.81(3) N1 C10 1.415(2) N1 C13 1.350(3) C1 H1A 0.9500 C1 C2 1.393(3) C1 C6 1.377(3) C2 H2 0.9500 C2 C3 1.385(4) C3 H3 0.9500 C3 C4 1.382(3) C4 H4 0.9500 C4 C5 1.386(3) C5 H5 0.9500 C5 C6 1.385(3) C6 C7 1.529(3) C7 H7 1.0000 C7 C8 1.533(3) C7 C9 1.512(3) C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 C10 1.374(3) C10 C11 1.423(3) C11 H11 0.9500 C11 C12 1.362(3) C12 H12 0.9500 C13 C14 1.519(3) C14 H14 1.0000 C14 C15 1.525(3) C14 C16 1.525(3) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800