#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:09:53 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247618 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125671.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_7125671 loop_ _publ_author_name 'Qiu, Yi-Feng' 'Niu, Yue-Jie' 'Song, Xian-Rong' 'Wei, Xi' 'Chen, Hui' 'Li, Shun-Xi' 'Wang, Xi-Cun' 'Huo, Congde' 'Quan, Zheng-Jun' 'Liang, Yong-Min' _publ_section_title ; Iodine promoted cascade cycloisomerization of 1-en-6,11-diynes. ; _journal_issue 9 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1421 _journal_page_last 1424 _journal_paper_doi 10.1039/c9cc08286g _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C28 H23 Br I N O3 S' _chemical_formula_sum 'C28 H23 Br I N O3 S' _chemical_formula_weight 660.34 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2018-07-27 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2019-05-05 deposited with the CCDC. 2019-12-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 14.8474(5) _cell_length_b 30.0430(15) _cell_length_c 26.3798(6) _cell_measurement_reflns_used 3035 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 23.1560 _cell_measurement_theta_min 3.6500 _cell_volume 11767.0(8) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 173.00(10) _diffrn_detector_area_resol_mean 16.0733 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 21.00 61.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.6305 -99.0000 60.0000 40 #__ type_ start__ end____ width___ exp.time_ 2 omega -47.00 66.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 22.6305 -19.0000 -90.0000 113 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0168200000 _diffrn_orient_matrix_UB_12 -0.0217318000 _diffrn_orient_matrix_UB_13 0.0045512000 _diffrn_orient_matrix_UB_21 0.0438818000 _diffrn_orient_matrix_UB_22 -0.0088600000 _diffrn_orient_matrix_UB_23 -0.0033912000 _diffrn_orient_matrix_UB_31 0.0085988000 _diffrn_orient_matrix_UB_32 0.0026290000 _diffrn_orient_matrix_UB_33 0.0262738000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_unetI/netI 0.1276 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 29148 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 3.374 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.545 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.491 _exptl_crystal_description block _exptl_crystal_F_000 5216 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.914 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 633 _refine_ls_number_reflns 11570 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.978 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0609 _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^)+(0.0126P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.1049 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6211 _reflns_number_total 11570 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08286g2.cif _cod_data_source_block qiuyf_0725 _cod_depositor_comments 'Adding full bibliography for 7125671--7125672.cif.' _cod_database_code 7125671 _shelx_shelxl_version_number 2014/7 _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. ; _reflns_odcompleteness_completeness 99.63 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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: C2(H2), C30(H30) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B), C29(H29A,H29B), C33(H33A,H33B), C56(H56A,H56B) 2.c Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54) 2.d Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C55(H55A,H55B,H55C) ; _shelx_res_file ; qiuyf_0725.res created by SHELXL-2014/7 TITL qiuyf_0725 in Pbcn #60 REM reset to Pbcn #60 CELL 0.71073 14.847449 30.043006 26.379807 90 90 90 ZERR 16 0.000544 0.001479 0.000629 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,+Y,0.5-Z SFAC C H Br I N O S UNIT 448 368 16 16 16 48 16 L.S. 10 PLAN 20 BOND $H HTAB CONF fmap 2 acta ABIN SHEL 999 0.81 OMIT 1 5 4 OMIT 2 3 1 OMIT 2 1 3 OMIT 1 5 1 OMIT 1 1 4 OMIT 3 1 2 OMIT 2 3 3 OMIT 2 4 1 REM REM REM WGHT 0.012600 FVAR 0.71643 I1 4 0.553529 0.582996 0.682879 11.00000 0.05880 0.09022 = 0.03043 0.01205 0.00382 0.01411 BR1 3 0.270349 0.545696 0.205429 11.00000 0.13954 0.05378 = 0.06356 0.01632 -0.05476 -0.05797 S1 7 0.426852 0.702728 0.568838 11.00000 0.03394 0.03710 = 0.03723 -0.00732 0.00845 -0.00263 O1 6 0.472232 0.660983 0.393109 11.00000 0.07558 0.02305 = 0.03635 0.00131 -0.01174 -0.00432 O2 6 0.338213 0.701009 0.546681 11.00000 0.02216 0.04994 = 0.06548 -0.01257 0.00491 -0.00418 O3 6 0.437197 0.705654 0.622933 11.00000 0.05345 0.04537 = 0.02583 -0.01083 0.01510 -0.00445 N1 5 0.478616 0.657280 0.550993 11.00000 0.03139 0.03307 = 0.02191 -0.00452 -0.00076 0.00032 C1 1 0.569175 0.649427 0.572361 11.00000 0.03174 0.04765 = 0.02463 -0.00367 -0.00177 0.00051 AFIX 23 H1A 2 0.571268 0.659195 0.607388 11.00000 -1.20000 H1B 2 0.613945 0.665957 0.553315 11.00000 -1.20000 AFIX 0 C2 1 0.588331 0.599900 0.569118 11.00000 0.03192 0.03006 = 0.02992 0.00092 0.00243 0.00262 AFIX 13 H2 2 0.650789 0.594579 0.579491 11.00000 -1.20000 AFIX 0 C3 1 0.576034 0.583308 0.514500 11.00000 0.02748 0.03166 = 0.02178 0.00048 -0.00064 -0.00984 C4 1 0.525646 0.607178 0.481278 11.00000 0.02607 0.02855 = 0.02103 0.00132 -0.00159 -0.00879 C5 1 0.479044 0.650342 0.495450 11.00000 0.03884 0.02819 = 0.02757 -0.00668 -0.00431 -0.00343 AFIX 23 H5A 2 0.509727 0.675035 0.479233 11.00000 -1.20000 H5B 2 0.417517 0.649739 0.483106 11.00000 -1.20000 AFIX 0 C6 1 0.525997 0.573196 0.603627 11.00000 0.04366 0.05117 = 0.03445 0.00492 -0.00299 -0.00038 AFIX 23 H6A 2 0.532177 0.541817 0.595694 11.00000 -1.20000 H6B 2 0.464150 0.581688 0.596785 11.00000 -1.20000 AFIX 0 C7 1 0.620028 0.542740 0.498967 11.00000 0.03013 0.02187 = 0.02919 0.00430 -0.00458 -0.00649 C8 1 0.674241 0.516412 0.531180 11.00000 0.04773 0.03185 = 0.04475 0.00096 -0.01309 -0.00466 AFIX 43 H8 2 0.681853 0.525130 0.564735 11.00000 -1.20000 AFIX 0 C9 1 0.715356 0.478994 0.514803 11.00000 0.06117 0.03956 = 0.05900 0.00984 -0.02099 0.01245 AFIX 43 H9 2 0.749054 0.462029 0.537382 11.00000 -1.20000 AFIX 0 C10 1 0.707858 0.465545 0.464518 11.00000 0.05039 0.03116 = 0.07647 0.00807 -0.01075 0.01118 AFIX 43 H10 2 0.736924 0.439894 0.453477 11.00000 -1.20000 AFIX 0 C11 1 0.657761 0.490105 0.431523 11.00000 0.04613 0.02654 = 0.05129 -0.00347 0.00384 -0.00034 AFIX 43 H11 2 0.652770 0.480977 0.397954 11.00000 -1.20000 AFIX 0 C12 1 0.613717 0.528836 0.447342 11.00000 0.02731 0.02417 = 0.03741 0.00457 -0.00515 -0.00366 C13 1 0.559304 0.553940 0.414398 11.00000 0.03751 0.03828 = 0.02955 -0.00488 -0.00183 -0.00595 AFIX 43 H13 2 0.551750 0.544161 0.381220 11.00000 -1.20000 AFIX 0 C14 1 0.516604 0.592636 0.429507 11.00000 0.02992 0.02592 = 0.02634 0.00426 -0.00309 -0.00448 C15 1 0.470130 0.620912 0.390928 11.00000 0.04168 0.02803 = 0.03186 0.00034 0.00222 -0.01159 C16 1 0.424238 0.598966 0.346519 11.00000 0.02984 0.02809 = 0.02958 0.00539 0.00067 -0.00090 C17 1 0.422459 0.623707 0.301561 11.00000 0.04413 0.01397 = 0.03114 0.00199 -0.01039 -0.01057 AFIX 43 H17 2 0.451064 0.651202 0.299786 11.00000 -1.20000 AFIX 0 C18 1 0.377402 0.606694 0.259553 11.00000 0.06333 0.02634 = 0.03770 0.00719 -0.00811 -0.02011 AFIX 43 H18 2 0.376590 0.622485 0.229234 11.00000 -1.20000 AFIX 0 C19 1 0.334416 0.566664 0.263178 11.00000 0.04903 0.03775 = 0.04121 0.00422 -0.01906 -0.01468 C20 1 0.335095 0.541615 0.307210 11.00000 0.06195 0.03641 = 0.06164 0.02002 -0.02291 -0.02703 AFIX 43 H20 2 0.305514 0.514374 0.308986 11.00000 -1.20000 AFIX 0 C21 1 0.381318 0.558512 0.348503 11.00000 0.04958 0.03062 = 0.03689 0.01538 -0.01156 -0.00522 AFIX 43 H21 2 0.383366 0.542059 0.378343 11.00000 -1.20000 AFIX 0 C22 1 0.486316 0.746904 0.540756 11.00000 0.02430 0.02925 = 0.03124 -0.00369 0.00601 0.00784 C23 1 0.561819 0.764732 0.564514 11.00000 0.04008 0.02894 = 0.03401 0.00168 -0.00729 0.00475 AFIX 43 H23 2 0.579147 0.754439 0.596300 11.00000 -1.20000 AFIX 0 C24 1 0.611019 0.797773 0.540779 11.00000 0.03048 0.02732 = 0.05029 0.00488 -0.00307 -0.00336 AFIX 43 H24 2 0.663014 0.808471 0.556207 11.00000 -1.20000 AFIX 0 C25 1 0.584676 0.815286 0.494601 11.00000 0.03567 0.03269 = 0.04282 0.00400 0.01365 0.01787 C26 1 0.509280 0.797334 0.471431 11.00000 0.04204 0.03994 = 0.02981 0.00287 -0.00136 0.01294 AFIX 43 H26 2 0.491567 0.808263 0.439990 11.00000 -1.20000 AFIX 0 C27 1 0.459389 0.763561 0.493676 11.00000 0.03554 0.04435 = 0.02913 -0.00704 -0.00536 0.01244 AFIX 43 H27 2 0.408742 0.752161 0.477499 11.00000 -1.20000 AFIX 0 C28 1 0.636361 0.851874 0.469722 11.00000 0.06574 0.04511 = 0.05555 0.01205 0.01891 -0.00107 AFIX 137 H28A 2 0.697290 0.842378 0.464120 11.00000 -1.50000 H28B 2 0.636182 0.877663 0.491209 11.00000 -1.50000 H28C 2 0.608852 0.859111 0.437837 11.00000 -1.50000 AFIX 0 I2 4 0.335745 0.941051 0.351062 11.00000 0.06417 0.05058 = 0.07233 0.01124 0.01945 0.03405 BR2 3 0.826586 0.617589 0.508329 11.00000 0.05703 0.04387 = 0.04150 0.01292 -0.01838 -0.00432 S2 7 0.281358 0.770080 0.363977 11.00000 0.02481 0.04780 = 0.03107 0.00586 0.00416 -0.00650 O4 6 0.593266 0.697002 0.305444 11.00000 0.03814 0.02810 = 0.03735 -0.00846 -0.01477 0.00592 O5 6 0.306547 0.734933 0.398418 11.00000 0.03849 0.06755 = 0.03338 0.02489 -0.00494 -0.01198 O6 6 0.230655 0.807164 0.381622 11.00000 0.03022 0.06104 = 0.04323 -0.00622 0.01254 0.00297 N2 5 0.374947 0.790605 0.342142 11.00000 0.01714 0.02775 = 0.03262 0.00674 0.00360 0.00118 C29 1 0.369498 0.827571 0.305379 11.00000 0.02115 0.03164 = 0.02762 0.00956 -0.00123 0.00057 AFIX 23 H29A 2 0.312091 0.842719 0.308617 11.00000 -1.20000 H29B 2 0.374579 0.816192 0.271087 11.00000 -1.20000 AFIX 0 C30 1 0.445230 0.859317 0.316220 11.00000 0.02727 0.01712 = 0.02249 0.00263 0.00256 -0.00390 AFIX 13 H30 2 0.450737 0.880198 0.287848 11.00000 -1.20000 AFIX 0 C31 1 0.534037 0.835232 0.323013 11.00000 0.02376 0.02281 = 0.01851 0.00108 -0.00024 0.00266 C32 1 0.537172 0.790075 0.329658 11.00000 0.02692 0.02393 = 0.01385 -0.00210 0.00319 -0.00382 C33 1 0.452358 0.761681 0.331087 11.00000 0.02433 0.03452 = 0.02904 0.01138 0.00131 0.00267 AFIX 23 H33A 2 0.443816 0.747007 0.298688 11.00000 -1.20000 H33B 2 0.457893 0.739004 0.357075 11.00000 -1.20000 AFIX 0 C34 1 0.614104 0.860905 0.321968 11.00000 0.02615 0.02462 = 0.02090 -0.00120 -0.00337 0.00016 C35 1 0.615445 0.907600 0.312453 11.00000 0.03257 0.02135 = 0.03595 0.00029 0.00095 -0.00173 AFIX 43 H35 2 0.561527 0.922937 0.308348 11.00000 -1.20000 AFIX 0 C36 1 0.694333 0.929725 0.309356 11.00000 0.04827 0.02553 = 0.05921 0.00448 -0.00830 -0.01151 AFIX 43 H36 2 0.693237 0.960082 0.302480 11.00000 -1.20000 AFIX 0 C37 1 0.777301 0.908955 0.316034 11.00000 0.03916 0.03854 = 0.06013 0.01209 0.00120 -0.01041 AFIX 43 H37 2 0.830283 0.925314 0.313481 11.00000 -1.20000 AFIX 0 C38 1 0.780500 0.864546 0.326328 11.00000 0.02674 0.03604 = 0.04285 0.00837 -0.00254 -0.01097 AFIX 43 H38 2 0.835617 0.850504 0.331308 11.00000 -1.20000 AFIX 0 C39 1 0.698685 0.839684 0.329426 11.00000 0.03393 0.03059 = 0.01731 -0.00218 0.00341 -0.00257 C40 1 0.699572 0.793100 0.338333 11.00000 0.02078 0.03004 = 0.02667 -0.00550 -0.00321 0.00430 AFIX 43 H40 2 0.754146 0.779015 0.344820 11.00000 -1.20000 AFIX 0 C41 1 0.622198 0.768387 0.337620 11.00000 0.02325 0.02782 = 0.01879 -0.00173 -0.00341 0.00173 C42 1 0.628684 0.718880 0.338728 11.00000 0.02077 0.01742 = 0.03909 0.00669 0.00588 -0.00066 C43 1 0.681700 0.696732 0.380210 11.00000 0.01857 0.01910 = 0.03088 -0.00258 0.00271 0.00094 C44 1 0.699101 0.716883 0.426608 11.00000 0.03426 0.02109 = 0.03507 0.00143 0.00146 0.00628 AFIX 43 H44 2 0.681676 0.746212 0.432176 11.00000 -1.20000 AFIX 0 C45 1 0.742632 0.693149 0.464758 11.00000 0.02631 0.05277 = 0.02558 0.00559 -0.00032 -0.01446 AFIX 43 H45 2 0.754136 0.706551 0.495871 11.00000 -1.20000 AFIX 0 C46 1 0.768367 0.650168 0.456366 11.00000 0.03362 0.02666 = 0.03909 -0.00268 -0.00969 -0.00539 C47 1 0.751881 0.629234 0.410922 11.00000 0.03947 0.03554 = 0.03617 -0.00528 -0.00725 0.00861 AFIX 43 H47 2 0.769548 0.599878 0.405802 11.00000 -1.20000 AFIX 0 C48 1 0.708602 0.652664 0.373078 11.00000 0.04295 0.03010 = 0.03360 -0.00754 -0.01229 0.00460 AFIX 43 H48 2 0.697140 0.638811 0.342218 11.00000 -1.20000 AFIX 0 C49 1 0.220801 0.746939 0.312700 11.00000 0.02091 0.04078 = 0.03550 0.00599 -0.00197 -0.00496 C50 1 0.163584 0.772999 0.284477 11.00000 0.02920 0.04090 = 0.04916 0.00279 0.00063 -0.00094 AFIX 43 H50 2 0.154816 0.802738 0.292932 11.00000 -1.20000 AFIX 0 C51 1 0.119230 0.754693 0.243485 11.00000 0.03037 0.04325 = 0.04433 0.00476 -0.00148 -0.01207 AFIX 43 H51 2 0.081303 0.772648 0.224276 11.00000 -1.20000 AFIX 0 C52 1 0.129407 0.710693 0.230169 11.00000 0.03191 0.06708 = 0.03635 0.00162 0.00211 -0.01472 C53 1 0.188019 0.684512 0.259227 11.00000 0.05555 0.04069 = 0.06400 -0.00408 -0.00599 -0.00691 AFIX 43 H53 2 0.196533 0.654728 0.250900 11.00000 -1.20000 AFIX 0 C54 1 0.233715 0.702702 0.300523 11.00000 0.02700 0.03810 = 0.05587 0.00564 -0.00481 0.00043 AFIX 43 H54 2 0.272543 0.685185 0.319687 11.00000 -1.20000 AFIX 0 C55 1 0.078578 0.690736 0.186570 11.00000 0.05093 0.07358 = 0.05875 -0.01803 -0.01423 -0.00762 AFIX 137 H55A 2 0.088910 0.708129 0.156601 11.00000 -1.50000 H55B 2 0.015368 0.690506 0.194224 11.00000 -1.50000 H55C 2 0.098937 0.660805 0.180994 11.00000 -1.50000 AFIX 0 C56 1 0.424675 0.885567 0.364598 11.00000 0.02915 0.02412 = 0.05096 0.00187 0.00926 0.01636 AFIX 23 H56A 2 0.480667 0.896503 0.378875 11.00000 -1.20000 H56B 2 0.397272 0.865808 0.389252 11.00000 -1.20000 AFIX 0 HKLF 4 REM qiuyf_0725 in Pbcn #60 REM R1 = 0.0609 for 6211 Fo > 4sig(Fo) and 0.1245 for all 11570 data REM 633 parameters refined using 0 restraints END WGHT 0.0124 0.0000 REM Instructions for potential hydrogen bonds HTAB C1 I1 EQIV $1 -x+1, y, -z+1/2 HTAB C18 O4_$1 EQIV $2 -x+1/2, y-1/2, z HTAB C20 I2_$2 HTAB C27 O5 HTAB C29 I2 HTAB C33 O1 EQIV $3 x-1/2, -y+3/2, -z+1 HTAB C56 Br2_$3 REM Highest difference peak 0.914, deepest hole -0.932, 1-sigma level 0.110 Q1 1 0.2250 0.5525 0.2310 11.00000 0.05 0.91 Q2 1 0.2612 0.5468 0.1934 11.00000 0.05 0.65 Q3 1 0.2833 0.9173 0.3219 11.00000 0.05 0.59 Q4 1 0.5162 0.5592 0.6510 11.00000 0.05 0.52 Q5 1 0.2372 0.9520 0.3564 11.00000 0.05 0.51 Q6 1 0.6228 0.6182 0.6705 11.00000 0.05 0.48 Q7 1 0.3203 0.5322 0.2116 11.00000 0.05 0.47 Q8 1 0.6448 0.4929 0.5693 11.00000 0.05 0.46 Q9 1 0.4827 0.5560 0.6805 11.00000 0.05 0.46 Q10 1 0.3763 0.9602 0.3256 11.00000 0.05 0.43 Q11 1 0.6116 0.5853 0.6871 11.00000 0.05 0.43 Q12 1 0.8770 0.6213 0.4910 11.00000 0.05 0.42 Q13 1 0.6439 0.4600 0.3891 11.00000 0.05 0.42 Q14 1 0.6241 0.5481 0.6916 11.00000 0.05 0.41 Q15 1 0.5977 0.5141 0.6394 11.00000 0.05 0.40 Q16 1 0.6856 0.8421 0.3086 11.00000 0.05 0.40 Q17 1 0.5638 0.5802 0.7251 11.00000 0.05 0.40 Q18 1 0.3542 0.9011 0.3169 11.00000 0.05 0.39 Q19 1 0.5411 0.7336 0.5264 11.00000 0.05 0.39 Q20 1 0.5365 0.5058 0.6596 11.00000 0.05 0.38 ; _shelx_res_checksum 6446 _shelx_fab_file ; 0 0 6 -75.8390 -7.5240 0 0 8 19.3562 0.1024 0 0 10 -1.3611 -3.3472 0 0 12 6.8971 -0.7320 0 0 14 -0.2570 -3.2969 0 0 16 15.4887 -1.5838 0 0 18 -5.5461 0.6305 0 0 20 -6.0541 -2.0196 0 0 22 -3.3576 -0.6282 0 0 24 -4.0606 0.5016 0 0 26 5.0340 -0.0321 0 0 28 -8.4095 -1.2363 0 0 30 -6.3463 1.0651 0 0 32 11.5460 0.1496 0 2 4 -27.7215 -0.7957 0 2 5 30.6920 1.9140 0 2 6 -56.7932 -3.6258 0 2 7 49.4266 0.0743 0 2 8 3.2753 4.3487 0 2 9 -0.6362 -5.1092 0 2 10 -5.6884 -4.1081 0 2 11 -8.4834 3.4195 0 2 12 6.6017 3.5622 0 2 13 -10.3444 -3.9034 0 2 14 1.2227 -2.4878 0 2 15 0.4461 -0.2453 0 2 16 14.4534 0.3138 0 2 17 -8.0351 -1.5684 0 2 18 -2.7373 1.8543 0 2 19 2.7354 -1.7518 0 2 20 -6.2399 -2.1933 0 2 21 -2.4314 0.4923 0 2 22 2.1102 1.6611 0 2 23 0.7631 -3.7209 0 2 24 -3.2813 -0.5196 0 2 25 7.3753 0.5943 0 2 26 -7.6874 0.7051 0 2 27 -12.0293 -1.3739 0 2 28 -0.7077 -0.4937 0 2 29 2.7089 -1.6764 0 2 30 -2.4509 0.4885 0 2 31 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-2.5054 0.5265 16 12 10 2.1868 -0.6761 16 12 11 -9.4564 -0.6925 16 13 1 -5.6837 0.4080 16 13 2 -7.2781 0.2544 16 13 3 -1.3898 -0.1613 16 13 4 -5.5625 0.3238 16 13 5 -0.3610 -0.5487 16 13 6 -0.8548 0.4235 16 13 7 2.6210 0.5561 16 13 8 2.1765 0.0316 16 13 9 -6.1567 -1.5053 16 13 10 -22.9535 0.0970 16 13 11 -1.8906 0.7225 16 14 0 4.6854 0.2033 16 14 1 -0.8304 -0.7104 16 14 2 0.7929 0.5712 16 14 3 -1.8193 0.0046 16 14 4 -5.2489 -0.5759 16 14 5 -6.8990 0.6742 16 14 6 11.9653 0.8249 16 14 7 10.4199 -0.6119 16 14 8 0.2716 0.7690 16 14 9 2.4761 0.5070 16 14 10 -0.0031 -0.4473 16 15 1 -5.3887 0.3673 16 15 2 -0.7030 0.0389 16 15 3 6.0775 -0.0543 16 15 4 -0.1419 0.3579 16 15 5 0.0407 -0.1871 16 15 6 1.9285 -0.0705 16 15 7 1.3762 0.0553 16 15 8 -6.1740 -0.2910 16 16 0 -2.2833 1.2568 16 16 1 0.7024 -0.1698 16 16 2 -3.7480 0.6868 16 16 3 0.1222 -0.0628 16 16 4 -1.9622 -0.7507 16 16 5 4.3500 0.9146 16 16 6 22.9707 0.2175 16 16 7 4.8650 -0.1053 16 17 1 4.7476 0.1402 16 17 2 5.9122 -0.3100 16 17 3 7.9822 0.4601 16 17 4 -6.0932 0.2684 16 17 5 -3.0617 0.1925 16 18 0 -0.2868 1.8013 16 18 1 3.1384 -0.0807 17 0 2 11.7582 0.5853 17 0 4 2.2382 -0.7826 17 0 6 -7.1289 -0.2357 17 0 8 -7.9384 0.4705 17 0 10 -8.4501 -0.3533 17 0 12 -17.2767 -0.1518 17 1 0 -2.6547 0.2691 17 1 1 1.9423 -1.2810 17 1 2 -1.5258 0.2623 17 1 3 -2.0913 0.1108 17 1 4 12.7031 -0.0164 17 1 5 -6.9801 0.0920 17 1 6 -3.4359 0.5029 17 1 7 -2.9522 0.7332 17 1 8 2.9102 -0.9759 17 1 9 -3.2335 0.8440 17 1 10 -8.5330 -0.1412 17 1 11 2.5131 1.1591 17 1 12 -5.4590 0.4197 17 2 1 8.7697 -0.4540 17 2 2 6.7034 0.4998 17 2 3 0.6177 -1.3341 17 2 4 -3.8404 -0.1432 17 2 5 -10.1201 -1.3569 17 2 6 -4.6659 -0.6108 17 2 7 -8.5514 -0.5173 17 2 8 -0.7194 0.9855 17 2 9 5.1530 -1.6648 17 2 10 -10.7444 -0.1893 17 2 11 0.6426 -0.3114 17 2 12 -14.4953 -0.2885 17 3 0 -0.2546 -0.9282 17 3 1 2.3779 -0.2399 17 3 2 -7.9448 0.6362 17 3 3 -3.2262 0.0799 17 3 4 6.1320 -0.0490 17 3 5 -13.2836 -0.0217 17 3 6 -2.9070 0.4117 17 3 7 -3.5624 0.0970 17 3 8 2.2441 -0.8272 17 3 9 -7.4960 0.2819 17 3 10 -3.7887 -0.2403 17 3 11 1.3196 1.0732 17 4 1 4.1986 0.6549 17 4 2 5.9200 0.1480 17 4 3 -1.1348 -0.5498 17 4 4 -6.1730 0.2330 17 4 5 -3.0429 -1.4121 17 4 6 -4.5731 -0.5118 17 4 7 -4.7048 0.1724 17 4 8 2.4443 0.7986 17 4 9 0.5125 -1.4383 17 4 10 -13.3655 -0.1032 17 4 11 -3.1620 -0.0281 17 5 0 2.6816 -1.0740 17 5 1 -0.8615 0.4656 17 5 2 -9.4826 0.0492 17 5 3 -0.0990 -0.0834 17 5 4 0.9025 -0.6755 17 5 5 -10.5470 0.1689 17 5 6 -0.6880 0.1147 17 5 7 1.6126 0.1510 17 5 8 -3.5947 -1.1272 17 5 9 -3.8299 0.0283 17 5 10 -3.9833 0.2243 17 5 11 -2.8211 0.5720 17 6 1 2.3983 0.9448 17 6 2 7.5767 0.0018 17 6 3 -4.8224 0.1035 17 6 4 -0.1104 -0.1752 17 6 5 1.2353 -0.9117 17 6 6 -6.7088 -0.7780 17 6 7 1.9596 0.6869 17 6 8 -2.1095 0.5048 17 6 9 1.0563 -1.1103 17 6 10 -15.1027 -0.4380 17 7 0 4.8964 0.2314 17 7 1 -4.9201 0.1270 17 7 2 -3.8898 -0.1044 17 7 3 0.6952 -0.3120 17 7 4 -1.5911 -0.5743 17 7 5 -2.4563 0.5061 17 7 6 6.3149 0.3028 17 7 7 2.7408 0.1616 17 7 8 -7.8413 -1.1027 17 7 9 3.2159 0.5545 17 7 10 -10.2608 0.3850 17 8 1 0.4690 0.2633 17 8 2 0.6392 -0.0199 17 8 3 -3.1059 0.1263 17 8 4 0.6926 0.0712 17 8 5 4.2785 -0.3450 17 8 6 -4.9429 -0.9945 17 8 7 8.8704 1.2092 17 8 8 0.9048 0.0971 17 8 9 0.2369 -1.1505 17 9 0 1.3447 1.0520 17 9 1 -6.7489 -0.2541 17 9 2 3.1643 0.1269 17 9 3 -3.2291 -0.0480 17 9 4 4.1438 -0.2445 17 9 5 9.1627 0.6725 17 9 6 10.4168 0.4192 17 9 7 -3.7024 -0.0522 17 9 8 -5.8815 -0.6566 17 9 9 7.2989 0.6509 17 10 1 -3.2716 -0.3383 17 10 2 1.9949 0.2714 17 10 3 1.3572 0.3900 17 10 4 1.7668 0.6562 17 10 5 8.1669 -0.4630 17 10 6 -2.7762 -0.7574 17 10 7 14.1760 1.1545 17 10 8 -2.1678 -0.0325 17 11 0 -3.7240 0.7286 17 11 1 -2.2076 -0.1215 17 11 2 5.3646 0.4778 17 11 3 -4.0727 0.2049 17 11 4 15.2770 -0.4346 17 11 5 11.9818 0.5447 17 11 6 5.1109 0.2575 17 11 7 -11.7675 -0.2392 17 12 1 2.2447 -0.2184 17 12 2 8.6812 0.4057 17 12 3 -1.1112 0.3923 17 12 4 3.1433 0.3641 17 12 5 1.3558 -0.6813 17 12 6 1.7581 -0.3965 17 13 0 -2.6797 0.4060 17 13 1 1.1420 0.5480 17 13 2 1.3050 0.5159 17 13 3 0.4875 0.0607 17 13 4 15.5868 -0.5988 18 0 0 -7.4721 -1.4315 18 0 2 -6.1674 0.3018 18 0 4 -10.9330 0.0135 18 0 6 16.5870 -1.0441 18 1 1 -4.6053 1.6232 18 1 2 -10.4343 -0.1054 18 1 3 3.4262 -2.1575 18 1 4 5.9227 -0.2295 18 1 5 3.4161 -0.6752 18 1 6 6.6702 0.2448 18 2 0 -0.1989 -0.6804 18 2 1 -0.7169 -0.5052 18 2 2 4.2397 0.2639 18 2 3 12.7163 -0.5714 18 2 4 -14.7762 -0.2249 18 2 5 12.8660 -0.1464 18 3 1 -8.3955 1.4414 18 3 2 -4.1288 -1.0478 18 3 3 3.8535 -1.7287 18 3 4 1.7435 0.0528 18 3 5 3.7353 0.2229 18 4 0 5.1317 0.5747 18 4 1 -2.0680 -0.2060 18 4 2 15.6955 0.0771 18 4 3 1.6977 -0.2763 18 4 4 -14.9020 -0.3380 18 4 5 14.1416 0.4466 18 5 1 -5.6657 0.9152 18 5 2 -0.3738 -1.1446 18 5 3 0.7077 -0.5962 18 5 4 -0.5336 0.8661 18 6 0 -1.3463 0.8182 18 6 1 1.1818 -0.4205 18 6 2 9.0765 0.4604 18 6 3 -7.2861 -0.0521 0 0 0 0.0 0.0 ; _shelx_fab_checksum 13895 _olex2_date_sample_data_collection 2018-07-27 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn I1 I 0.55353(3) 0.58300(2) 0.68288(2) 0.05982(19) Uani 1 1 d . Br1 Br 0.27035(7) 0.54570(3) 0.20543(3) 0.0856(4) Uani 1 1 d . S1 S 0.42685(11) 0.70273(6) 0.56884(6) 0.0361(4) Uani 1 1 d . O1 O 0.4722(3) 0.66098(16) 0.39311(14) 0.0450(13) Uani 1 1 d . O2 O 0.3382(3) 0.70101(16) 0.54668(15) 0.0459(13) Uani 1 1 d . O3 O 0.4372(3) 0.70565(15) 0.62293(12) 0.0416(13) Uani 1 1 d . N1 N 0.4786(3) 0.65728(18) 0.55099(15) 0.0288(13) Uani 1 1 d . C1 C 0.5692(4) 0.6494(2) 0.5724(2) 0.0347(17) Uani 1 1 d . H1A H 0.5713 0.6592 0.6074 0.042 Uiso 1 1 calc R H1B H 0.6139 0.6660 0.5533 0.042 Uiso 1 1 calc R C2 C 0.5883(4) 0.5999(2) 0.56912(19) 0.0306(16) Uani 1 1 d . H2 H 0.6508 0.5946 0.5795 0.037 Uiso 1 1 calc R C3 C 0.5760(4) 0.5833(2) 0.51450(19) 0.0270(15) Uani 1 1 d . C4 C 0.5256(4) 0.6072(2) 0.48128(19) 0.0252(15) Uani 1 1 d . C5 C 0.4790(4) 0.6503(2) 0.49545(18) 0.0315(16) Uani 1 1 d . H5A H 0.5097 0.6750 0.4792 0.038 Uiso 1 1 calc R H5B H 0.4175 0.6497 0.4831 0.038 Uiso 1 1 calc R C6 C 0.5260(4) 0.5732(2) 0.60363(19) 0.0431(19) Uani 1 1 d . H6A H 0.5322 0.5418 0.5957 0.052 Uiso 1 1 calc R H6B H 0.4641 0.5817 0.5968 0.052 Uiso 1 1 calc R C7 C 0.6200(4) 0.5427(2) 0.4990(2) 0.0271(15) Uani 1 1 d . C8 C 0.6742(5) 0.5164(2) 0.5312(2) 0.0414(18) Uani 1 1 d . H8 H 0.6819 0.5251 0.5647 0.050 Uiso 1 1 calc R C9 C 0.7154(5) 0.4790(3) 0.5148(3) 0.053(2) Uani 1 1 d . H9 H 0.7491 0.4620 0.5374 0.064 Uiso 1 1 calc R C10 C 0.7079(5) 0.4655(3) 0.4645(3) 0.053(2) Uani 1 1 d . H10 H 0.7369 0.4399 0.4535 0.063 Uiso 1 1 calc R C11 C 0.6578(5) 0.4901(2) 0.4315(2) 0.0413(18) Uani 1 1 d . H11 H 0.6528 0.4810 0.3980 0.050 Uiso 1 1 calc R C12 C 0.6137(4) 0.5288(2) 0.4473(2) 0.0296(16) Uani 1 1 d . C13 C 0.5593(4) 0.5539(2) 0.4144(2) 0.0351(17) Uani 1 1 d . H13 H 0.5518 0.5442 0.3812 0.042 Uiso 1 1 calc R C14 C 0.5166(4) 0.5926(2) 0.4295(2) 0.0274(15) Uani 1 1 d . C15 C 0.4701(5) 0.6209(2) 0.3909(2) 0.0339(17) Uani 1 1 d . C16 C 0.4242(4) 0.5990(2) 0.3465(2) 0.0292(16) Uani 1 1 d . C17 C 0.4225(4) 0.6237(2) 0.30156(19) 0.0297(16) Uani 1 1 d . H17 H 0.4511 0.6512 0.2998 0.036 Uiso 1 1 calc R C18 C 0.3774(5) 0.6067(2) 0.2596(2) 0.0425(19) Uani 1 1 d . H18 H 0.3766 0.6225 0.2292 0.051 Uiso 1 1 calc R C19 C 0.3344(5) 0.5667(2) 0.2632(2) 0.0427(19) Uani 1 1 d . C20 C 0.3351(5) 0.5416(2) 0.3072(2) 0.053(2) Uani 1 1 d . H20 H 0.3055 0.5144 0.3090 0.064 Uiso 1 1 calc R C21 C 0.3813(4) 0.5585(2) 0.3485(2) 0.0390(18) Uani 1 1 d . H21 H 0.3834 0.5421 0.3783 0.047 Uiso 1 1 calc R C22 C 0.4863(4) 0.7469(2) 0.5408(2) 0.0283(15) Uani 1 1 d . C23 C 0.5618(4) 0.7647(2) 0.5645(2) 0.0343(17) Uani 1 1 d . H23 H 0.5791 0.7544 0.5963 0.041 Uiso 1 1 calc R C24 C 0.6110(4) 0.7978(2) 0.5408(2) 0.0360(17) Uani 1 1 d . H24 H 0.6630 0.8085 0.5562 0.043 Uiso 1 1 calc R C25 C 0.5847(4) 0.8153(2) 0.4946(2) 0.0371(18) Uani 1 1 d . C26 C 0.5093(5) 0.7973(2) 0.4714(2) 0.0373(18) Uani 1 1 d . H26 H 0.4916 0.8083 0.4400 0.045 Uiso 1 1 calc R C27 C 0.4594(4) 0.7636(2) 0.4937(2) 0.0363(18) Uani 1 1 d . H27 H 0.4087 0.7522 0.4775 0.044 Uiso 1 1 calc R C28 C 0.6364(5) 0.8519(2) 0.4697(2) 0.055(2) Uani 1 1 d . H28A H 0.6973 0.8424 0.4641 0.083 Uiso 1 1 calc GR H28B H 0.6362 0.8777 0.4912 0.083 Uiso 1 1 calc GR H28C H 0.6089 0.8591 0.4378 0.083 Uiso 1 1 calc GR I2 I 0.33575(4) 0.94105(2) 0.35106(2) 0.06236(18) Uani 1 1 d . Br2 Br 0.82659(5) 0.61759(3) 0.50833(2) 0.0475(2) Uani 1 1 d . S2 S 0.28136(11) 0.77008(7) 0.36398(6) 0.0346(4) Uani 1 1 d . O4 O 0.5933(3) 0.69700(15) 0.30544(13) 0.0345(11) Uani 1 1 d . O5 O 0.3065(3) 0.73493(17) 0.39842(13) 0.0465(14) Uani 1 1 d . O6 O 0.2307(3) 0.80716(17) 0.38162(14) 0.0448(13) Uani 1 1 d . N2 N 0.3749(3) 0.79060(17) 0.34214(16) 0.0258(12) Uani 1 1 d . C29 C 0.3695(4) 0.8276(2) 0.30538(19) 0.0268(15) Uani 1 1 d . H29A H 0.3121 0.8427 0.3086 0.032 Uiso 1 1 calc R H29B H 0.3746 0.8162 0.2711 0.032 Uiso 1 1 calc R C30 C 0.4452(4) 0.8593(2) 0.31622(19) 0.0223(14) Uani 1 1 d . H30 H 0.4507 0.8802 0.2878 0.027 Uiso 1 1 calc R C31 C 0.5340(4) 0.8352(2) 0.32301(18) 0.0217(14) Uani 1 1 d . C32 C 0.5372(4) 0.7901(2) 0.32966(18) 0.0216(14) Uani 1 1 d . C33 C 0.4524(4) 0.7617(2) 0.3311(2) 0.0293(16) Uani 1 1 d . H33A H 0.4438 0.7470 0.2987 0.035 Uiso 1 1 calc R H33B H 0.4579 0.7390 0.3571 0.035 Uiso 1 1 calc R C34 C 0.6141(4) 0.8609(2) 0.32197(19) 0.0239(14) Uani 1 1 d . C35 C 0.6154(4) 0.9076(2) 0.31245(19) 0.0300(16) Uani 1 1 d . H35 H 0.5615 0.9229 0.3083 0.036 Uiso 1 1 calc R C36 C 0.6943(5) 0.9297(2) 0.3094(2) 0.0443(19) Uani 1 1 d . H36 H 0.6932 0.9601 0.3025 0.053 Uiso 1 1 calc R C37 C 0.7773(5) 0.9090(3) 0.3160(2) 0.0459(19) Uani 1 1 d . H37 H 0.8303 0.9253 0.3135 0.055 Uiso 1 1 calc R C38 C 0.7805(4) 0.8645(2) 0.3263(2) 0.0352(17) Uani 1 1 d . H38 H 0.8356 0.8505 0.3313 0.042 Uiso 1 1 calc R C39 C 0.6987(4) 0.8397(2) 0.32943(19) 0.0273(16) Uani 1 1 d . C40 C 0.6996(4) 0.7931(2) 0.33833(18) 0.0258(15) Uani 1 1 d . H40 H 0.7541 0.7790 0.3448 0.031 Uiso 1 1 calc R C41 C 0.6222(4) 0.7684(2) 0.33762(18) 0.0233(14) Uani 1 1 d . C42 C 0.6287(4) 0.7189(2) 0.3387(2) 0.0258(15) Uani 1 1 d . C43 C 0.6817(4) 0.6967(2) 0.3802(2) 0.0229(14) Uani 1 1 d . C44 C 0.6991(4) 0.7169(2) 0.4266(2) 0.0301(16) Uani 1 1 d . H44 H 0.6817 0.7462 0.4322 0.036 Uiso 1 1 calc R C45 C 0.7426(4) 0.6931(3) 0.4648(2) 0.0349(18) Uani 1 1 d . H45 H 0.7541 0.7066 0.4959 0.042 Uiso 1 1 calc R C46 C 0.7684(4) 0.6502(2) 0.4564(2) 0.0331(17) Uani 1 1 d . C47 C 0.7519(4) 0.6292(2) 0.4109(2) 0.0371(18) Uani 1 1 d . H47 H 0.7695 0.5999 0.4058 0.044 Uiso 1 1 calc R C48 C 0.7086(4) 0.6527(2) 0.3731(2) 0.0356(17) Uani 1 1 d . H48 H 0.6971 0.6388 0.3422 0.043 Uiso 1 1 calc R C49 C 0.2208(4) 0.7469(2) 0.3127(2) 0.0324(16) Uani 1 1 d . C50 C 0.1636(4) 0.7730(2) 0.2845(2) 0.0398(18) Uani 1 1 d . H50 H 0.1548 0.8027 0.2929 0.048 Uiso 1 1 calc R C51 C 0.1192(4) 0.7547(3) 0.2435(2) 0.0393(18) Uani 1 1 d . H51 H 0.0813 0.7726 0.2243 0.047 Uiso 1 1 calc R C52 C 0.1294(5) 0.7107(3) 0.2302(2) 0.045(2) Uani 1 1 d . C53 C 0.1880(5) 0.6845(3) 0.2592(2) 0.053(2) Uani 1 1 d . H53 H 0.1965 0.6547 0.2509 0.064 Uiso 1 1 calc R C54 C 0.2337(4) 0.7027(2) 0.3005(2) 0.0403(18) Uani 1 1 d . H54 H 0.2725 0.6852 0.3197 0.048 Uiso 1 1 calc R C55 C 0.0786(5) 0.6907(3) 0.1866(2) 0.061(2) Uani 1 1 d . H55A H 0.0889 0.7081 0.1566 0.092 Uiso 1 1 calc GR H55B H 0.0154 0.6905 0.1942 0.092 Uiso 1 1 calc GR H55C H 0.0989 0.6608 0.1810 0.092 Uiso 1 1 calc GR C56 C 0.4247(4) 0.8856(2) 0.3646(2) 0.0347(17) Uani 1 1 d . H56A H 0.4807 0.8965 0.3789 0.042 Uiso 1 1 calc R H56B H 0.3973 0.8658 0.3893 0.042 Uiso 1 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 I1 0.0588(3) 0.0902(5) 0.0304(2) 0.0120(3) 0.0038(2) 0.0141(4) Br1 0.1395(9) 0.0538(6) 0.0636(5) 0.0163(5) -0.0548(5) -0.0580(7) S1 0.0339(10) 0.0371(12) 0.0372(9) -0.0073(9) 0.0084(8) -0.0026(10) O1 0.076(4) 0.023(3) 0.036(2) 0.001(2) -0.012(2) -0.004(3) O2 0.022(2) 0.050(3) 0.065(3) -0.013(3) 0.005(2) -0.004(3) O3 0.053(3) 0.045(3) 0.026(2) -0.011(2) 0.015(2) -0.004(3) N1 0.031(3) 0.033(4) 0.022(2) -0.005(3) -0.001(2) 0.000(3) C1 0.032(4) 0.048(5) 0.025(3) -0.004(3) -0.002(3) 0.001(4) C2 0.032(4) 0.030(4) 0.030(3) 0.001(3) 0.002(3) 0.003(4) C3 0.027(4) 0.032(4) 0.022(3) 0.000(3) -0.001(3) -0.010(3) C4 0.026(3) 0.029(4) 0.021(3) 0.001(3) -0.002(3) -0.009(3) C5 0.039(4) 0.028(4) 0.028(3) -0.007(3) -0.004(3) -0.003(4) C6 0.044(4) 0.051(5) 0.034(3) 0.005(4) -0.003(3) 0.000(4) C7 0.030(4) 0.022(4) 0.029(3) 0.004(3) -0.005(3) -0.006(3) C8 0.048(5) 0.032(5) 0.045(4) 0.001(4) -0.013(3) -0.005(4) C9 0.061(5) 0.040(5) 0.059(5) 0.010(4) -0.021(4) 0.012(5) C10 0.050(5) 0.031(5) 0.076(5) 0.008(4) -0.011(4) 0.011(4) C11 0.046(4) 0.027(4) 0.051(4) -0.003(4) 0.004(4) 0.000(4) C12 0.027(4) 0.024(4) 0.037(4) 0.005(3) -0.005(3) -0.004(3) C13 0.038(4) 0.038(5) 0.030(3) -0.005(3) -0.002(3) -0.006(4) C14 0.030(4) 0.026(4) 0.026(3) 0.004(3) -0.003(3) -0.004(3) C15 0.042(4) 0.028(4) 0.032(4) 0.000(4) 0.002(3) -0.012(4) C16 0.030(4) 0.028(4) 0.030(3) 0.005(3) 0.001(3) -0.001(3) C17 0.044(4) 0.014(4) 0.031(3) 0.002(3) -0.010(3) -0.011(3) C18 0.063(5) 0.026(4) 0.038(4) 0.007(4) -0.008(3) -0.020(4) C19 0.049(5) 0.038(5) 0.041(4) 0.004(4) -0.019(3) -0.015(4) C20 0.062(5) 0.036(5) 0.062(4) 0.020(4) -0.023(4) -0.027(5) C21 0.050(4) 0.031(4) 0.037(4) 0.015(4) -0.012(3) -0.005(4) C22 0.024(3) 0.029(4) 0.031(3) -0.004(3) 0.006(3) 0.008(3) C23 0.040(4) 0.029(4) 0.034(3) 0.002(3) -0.007(3) 0.005(4) C24 0.030(4) 0.027(4) 0.050(4) 0.005(4) -0.003(3) -0.003(4) C25 0.036(4) 0.033(4) 0.043(4) 0.004(4) 0.014(3) 0.018(4) C26 0.042(4) 0.040(5) 0.030(3) 0.003(4) -0.001(3) 0.013(4) C27 0.036(4) 0.044(5) 0.029(3) -0.007(4) -0.005(3) 0.012(4) C28 0.066(5) 0.045(5) 0.056(4) 0.012(4) 0.019(4) -0.001(5) I2 0.0642(4) 0.0506(4) 0.0723(3) 0.0112(3) 0.0195(3) 0.0341(3) Br2 0.0570(5) 0.0439(5) 0.0415(4) 0.0129(4) -0.0184(3) -0.0043(5) S2 0.0248(9) 0.0478(12) 0.0311(9) 0.0059(9) 0.0042(7) -0.0065(10) O4 0.038(3) 0.028(3) 0.037(2) -0.008(2) -0.015(2) 0.006(2) O5 0.038(3) 0.068(4) 0.033(2) 0.025(3) -0.005(2) -0.012(3) O6 0.030(3) 0.061(4) 0.043(2) -0.006(3) 0.013(2) 0.003(3) N2 0.017(3) 0.028(3) 0.033(3) 0.007(3) 0.004(2) 0.001(3) C29 0.021(3) 0.032(4) 0.028(3) 0.010(3) -0.001(3) 0.001(3) C30 0.027(3) 0.017(3) 0.022(3) 0.003(3) 0.003(3) -0.004(3) C31 0.024(3) 0.023(4) 0.019(3) 0.001(3) 0.000(2) 0.003(3) C32 0.027(3) 0.024(4) 0.014(3) -0.002(3) 0.003(2) -0.004(3) C33 0.024(3) 0.035(4) 0.029(3) 0.011(3) 0.001(3) 0.003(3) C34 0.026(3) 0.025(4) 0.021(3) -0.001(3) -0.003(3) 0.000(3) C35 0.033(4) 0.021(4) 0.036(3) 0.000(3) 0.001(3) -0.002(3) C36 0.048(5) 0.026(4) 0.059(4) 0.004(4) -0.008(4) -0.012(4) C37 0.039(4) 0.039(5) 0.060(4) 0.012(4) 0.001(4) -0.010(4) C38 0.027(4) 0.036(5) 0.043(4) 0.008(4) -0.003(3) -0.011(4) C39 0.034(4) 0.031(4) 0.017(3) -0.002(3) 0.003(3) -0.003(4) C40 0.021(3) 0.030(4) 0.027(3) -0.006(3) -0.003(3) 0.004(3) C41 0.023(3) 0.028(4) 0.019(3) -0.002(3) -0.003(2) 0.002(3) C42 0.021(3) 0.017(4) 0.039(4) 0.007(3) 0.006(3) -0.001(3) C43 0.019(3) 0.019(4) 0.031(3) -0.003(3) 0.003(3) 0.001(3) C44 0.034(4) 0.021(4) 0.035(3) 0.001(3) 0.001(3) 0.006(3) C45 0.026(4) 0.053(5) 0.026(3) 0.006(4) 0.000(3) -0.014(4) C46 0.034(4) 0.027(4) 0.039(4) -0.003(4) -0.010(3) -0.005(4) C47 0.039(4) 0.036(5) 0.036(3) -0.005(4) -0.007(3) 0.009(4) C48 0.043(4) 0.030(4) 0.034(3) -0.008(3) -0.012(3) 0.005(4) C49 0.021(3) 0.041(5) 0.036(3) 0.006(4) -0.002(3) -0.005(4) C50 0.029(4) 0.041(5) 0.049(4) 0.003(4) 0.001(3) -0.001(4) C51 0.030(4) 0.043(5) 0.044(4) 0.005(4) -0.001(3) -0.012(4) C52 0.032(4) 0.067(6) 0.036(4) 0.002(4) 0.002(3) -0.015(5) C53 0.056(5) 0.041(5) 0.064(5) -0.004(4) -0.006(4) -0.007(5) C54 0.027(4) 0.038(5) 0.056(4) 0.006(4) -0.005(3) 0.000(4) C55 0.051(5) 0.074(7) 0.059(4) -0.018(5) -0.014(4) -0.008(5) C56 0.029(4) 0.024(4) 0.051(4) 0.002(3) 0.009(3) 0.016(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 O2 S1 N1 106.4(3) O2 S1 C22 108.4(3) O3 S1 O2 120.2(3) O3 S1 N1 106.6(3) O3 S1 C22 108.6(3) N1 S1 C22 105.8(3) C1 N1 S1 116.8(4) C1 N1 C5 110.6(5) C5 N1 S1 113.9(4) N1 C1 H1A 110.1 N1 C1 H1B 110.1 N1 C1 C2 107.8(5) H1A C1 H1B 108.5 C2 C1 H1A 110.1 C2 C1 H1B 110.1 C1 C2 H2 108.8 C1 C2 C3 110.4(5) C1 C2 C6 111.6(5) C3 C2 H2 108.8 C6 C2 H2 108.8 C6 C2 C3 108.5(5) C4 C3 C2 120.0(6) C4 C3 C7 120.8(5) C7 C3 C2 119.1(5) C3 C4 C5 123.0(5) C3 C4 C14 120.2(6) C14 C4 C5 116.8(5) N1 C5 C4 111.5(5) N1 C5 H5A 109.3 N1 C5 H5B 109.3 C4 C5 H5A 109.3 C4 C5 H5B 109.3 H5A C5 H5B 108.0 I1 C6 H6A 109.0 I1 C6 H6B 109.0 C2 C6 I1 113.1(4) C2 C6 H6A 109.0 C2 C6 H6B 109.0 H6A C6 H6B 107.8 C8 C7 C3 124.1(5) C8 C7 C12 116.6(6) C12 C7 C3 119.2(5) C7 C8 H8 119.0 C9 C8 C7 122.1(6) C9 C8 H8 119.0 C8 C9 H9 119.6 C8 C9 C10 120.7(7) C10 C9 H9 119.6 C9 C10 H10 120.1 C11 C10 C9 119.7(7) C11 C10 H10 120.1 C10 C11 H11 119.5 C10 C11 C12 121.0(6) C12 C11 H11 119.5 C11 C12 C7 119.8(6) C11 C12 C13 122.0(6) C13 C12 C7 118.1(6) C12 C13 H13 118.8 C14 C13 C12 122.4(5) C14 C13 H13 118.8 C4 C14 C15 121.1(6) C13 C14 C4 119.1(6) C13 C14 C15 119.6(5) O1 C15 C14 121.5(6) O1 C15 C16 119.1(6) C14 C15 C16 119.3(6) C17 C16 C15 115.8(6) C21 C16 C15 124.6(6) C21 C16 C17 119.6(6) C16 C17 H17 120.4 C18 C17 C16 119.3(6) C18 C17 H17 120.4 C17 C18 H18 120.2 C19 C18 C17 119.5(6) C19 C18 H18 120.2 C18 C19 Br1 118.0(5) C18 C19 C20 122.3(6) C20 C19 Br1 119.7(5) C19 C20 H20 121.2 C21 C20 C19 117.7(6) C21 C20 H20 121.2 C16 C21 C20 121.6(6) C16 C21 H21 119.2 C20 C21 H21 119.2 C23 C22 S1 120.4(5) C23 C22 C27 119.5(6) C27 C22 S1 120.1(5) C22 C23 H23 120.1 C24 C23 C22 119.9(6) C24 C23 H23 120.1 C23 C24 H24 119.2 C23 C24 C25 121.5(6) C25 C24 H24 119.2 C24 C25 C26 118.0(6) C24 C25 C28 121.5(6) C26 C25 C28 120.6(6) C25 C26 H26 119.0 C25 C26 C27 122.0(6) C27 C26 H26 119.0 C22 C27 H27 120.5 C26 C27 C22 119.0(6) C26 C27 H27 120.5 C25 C28 H28A 109.5 C25 C28 H28B 109.5 C25 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 O5 S2 N2 106.2(3) O5 S2 C49 109.0(3) O6 S2 O5 120.3(2) O6 S2 N2 105.7(3) O6 S2 C49 106.8(3) N2 S2 C49 108.2(3) C29 N2 S2 118.1(4) C33 N2 S2 121.0(4) C33 N2 C29 110.9(4) N2 C29 H29A 110.1 N2 C29 H29B 110.1 N2 C29 C30 108.2(4) H29A C29 H29B 108.4 C30 C29 H29A 110.1 C30 C29 H29B 110.1 C29 C30 H30 108.9 C29 C30 C31 111.8(5) C29 C30 C56 109.7(5) C31 C30 H30 108.9 C31 C30 C56 108.7(4) C56 C30 H30 108.9 C32 C31 C30 121.2(6) C32 C31 C34 120.9(6) C34 C31 C30 117.9(5) C31 C32 C33 122.1(6) C31 C32 C41 119.9(6) C41 C32 C33 118.0(5) N2 C33 C32 108.7(5) N2 C33 H33A 109.9 N2 C33 H33B 109.9 C32 C33 H33A 109.9 C32 C33 H33B 109.9 H33A C33 H33B 108.3 C31 C34 C35 123.4(6) C31 C34 C39 119.6(6) C39 C34 C35 117.0(6) C34 C35 H35 119.7 C36 C35 C34 120.5(6) C36 C35 H35 119.7 C35 C36 H36 118.7 C35 C36 C37 122.7(7) C37 C36 H36 118.7 C36 C37 H37 120.2 C38 C37 C36 119.7(7) C38 C37 H37 120.2 C37 C38 H38 120.2 C37 C38 C39 119.6(7) C39 C38 H38 120.2 C34 C39 C38 120.6(6) C40 C39 C34 118.2(6) C40 C39 C38 121.1(6) C39 C40 H40 119.2 C41 C40 C39 121.7(6) C41 C40 H40 119.2 C32 C41 C42 120.8(6) C40 C41 C32 119.6(6) C40 C41 C42 119.1(6) O4 C42 C41 119.8(5) O4 C42 C43 120.8(6) C41 C42 C43 119.3(5) C44 C43 C42 123.1(6) C44 C43 C48 118.6(6) C48 C43 C42 118.1(5) C43 C44 H44 120.0 C43 C44 C45 120.0(6) C45 C44 H44 120.0 C44 C45 H45 120.1 C46 C45 C44 119.8(6) C46 C45 H45 120.1 C45 C46 Br2 120.0(5) C45 C46 C47 121.6(6) C47 C46 Br2 118.4(5) C46 C47 H47 120.7 C46 C47 C48 118.7(6) C48 C47 H47 120.7 C43 C48 H48 119.3 C47 C48 C43 121.3(6) C47 C48 H48 119.3 C50 C49 S2 120.3(6) C50 C49 C54 120.5(6) C54 C49 S2 119.1(5) C49 C50 H50 120.3 C49 C50 C51 119.5(7) C51 C50 H50 120.3 C50 C51 H51 119.0 C52 C51 C50 122.0(7) C52 C51 H51 119.0 C51 C52 C53 117.9(7) C51 C52 C55 121.6(7) C53 C52 C55 120.5(8) C52 C53 H53 119.7 C54 C53 C52 120.6(7) C54 C53 H53 119.7 C49 C54 C53 119.4(7) C49 C54 H54 120.3 C53 C54 H54 120.3 C52 C55 H55A 109.5 C52 C55 H55B 109.5 C52 C55 H55C 109.5 H55A C55 H55B 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 I2 C56 H56A 109.1 I2 C56 H56B 109.1 C30 C56 I2 112.5(4) C30 C56 H56A 109.1 C30 C56 H56B 109.1 H56A C56 H56B 107.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C6 2.150(5) Br1 C19 1.903(6) S1 O2 1.441(4) S1 O3 1.438(4) S1 N1 1.636(5) S1 C22 1.758(6) O1 C15 1.206(7) N1 C1 1.477(7) N1 C5 1.480(6) C1 H1A 0.9700 C1 H1B 0.9700 C1 C2 1.517(8) C2 H2 0.9800 C2 C3 1.535(7) C2 C6 1.526(8) C3 C4 1.357(7) C3 C7 1.442(8) C4 C5 1.517(8) C4 C14 1.440(7) C5 H5A 0.9700 C5 H5B 0.9700 C6 H6A 0.9700 C6 H6B 0.9700 C7 C8 1.413(8) C7 C12 1.428(7) C8 H8 0.9300 C8 C9 1.350(9) C9 H9 0.9300 C9 C10 1.391(8) C10 H10 0.9300 C10 C11 1.362(8) C11 H11 0.9300 C11 C12 1.398(8) C12 C13 1.406(8) C13 H13 0.9300 C13 C14 1.383(8) C14 C15 1.495(8) C15 C16 1.507(8) C16 C17 1.400(7) C16 C21 1.373(8) C17 H17 0.9300 C17 C18 1.392(7) C18 H18 0.9300 C18 C19 1.365(9) C19 C20 1.384(8) C20 H20 0.9300 C20 C21 1.384(8) C21 H21 0.9300 C22 C23 1.392(8) C22 C27 1.397(7) C23 H23 0.9300 C23 C24 1.382(8) C24 H24 0.9300 C24 C25 1.383(8) C25 C26 1.385(8) C25 C28 1.493(9) C26 H26 0.9300 C26 C27 1.387(9) C27 H27 0.9300 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 I2 C56 2.156(6) Br2 C46 1.893(6) S2 O5 1.442(4) S2 O6 1.423(5) S2 N2 1.626(5) S2 C49 1.767(6) O4 C42 1.216(6) N2 C29 1.477(7) N2 C33 1.470(7) C29 H29A 0.9700 C29 H29B 0.9700 C29 C30 1.502(7) C30 H30 0.9800 C30 C31 1.515(7) C30 C56 1.531(7) C31 C32 1.369(8) C31 C34 1.417(8) C32 C33 1.521(8) C32 C41 1.436(8) C33 H33A 0.9700 C33 H33B 0.9700 C34 C35 1.425(8) C34 C39 1.422(8) C35 H35 0.9300 C35 C36 1.349(8) C36 H36 0.9300 C36 C37 1.392(9) C37 H37 0.9300 C37 C38 1.362(9) C38 H38 0.9300 C38 C39 1.428(8) C39 C40 1.419(8) C40 H40 0.9300 C40 C41 1.368(8) C41 C42 1.491(8) C42 C43 1.503(8) C43 C44 1.390(7) C43 C48 1.396(8) C44 H44 0.9300 C44 C45 1.392(8) C45 H45 0.9300 C45 C46 1.365(9) C46 C47 1.376(7) C47 H47 0.9300 C47 C48 1.380(8) C48 H48 0.9300 C49 C50 1.374(8) C49 C54 1.381(9) C50 H50 0.9300 C50 C51 1.380(8) C51 H51 0.9300 C51 C52 1.376(10) C52 C53 1.401(9) C52 C55 1.501(8) C53 H53 0.9300 C53 C54 1.395(8) C54 H54 0.9300 C55 H55A 0.9600 C55 H55B 0.9600 C55 H55C 0.9600 C56 H56A 0.9700 C56 H56B 0.9700 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 Br1 C19 C20 C21 -179.0(5) S1 N1 C1 C2 157.5(4) S1 N1 C5 C4 -178.5(4) S1 C22 C23 C24 176.4(5) S1 C22 C27 C26 -177.7(5) O1 C15 C16 C17 27.2(9) O1 C15 C16 C21 -149.2(7) O2 S1 N1 C1 -175.2(4) O2 S1 N1 C5 53.9(5) O2 S1 C22 C23 160.7(5) O2 S1 C22 C27 -21.0(6) O3 S1 N1 C1 -45.9(5) O3 S1 N1 C5 -176.7(4) O3 S1 C22 C23 28.7(6) O3 S1 C22 C27 -153.0(5) N1 S1 C22 C23 -85.5(5) N1 S1 C22 C27 92.8(5) N1 C1 C2 C3 54.3(6) N1 C1 C2 C6 -66.5(6) C1 N1 C5 C4 47.7(7) C1 C2 C3 C4 -20.6(8) C1 C2 C3 C7 158.2(5) C1 C2 C6 I1 -69.6(6) C2 C3 C4 C5 -0.4(9) C2 C3 C4 C14 177.7(5) C2 C3 C7 C8 0.5(9) C2 C3 C7 C12 -175.8(5) C3 C2 C6 I1 168.5(4) C3 C4 C5 N1 -12.6(8) C3 C4 C14 C13 0.5(9) C3 C4 C14 C15 -173.1(6) C3 C7 C8 C9 -178.9(6) C3 C7 C12 C11 178.5(6) C3 C7 C12 C13 -4.3(9) C4 C3 C7 C8 179.3(6) C4 C3 C7 C12 3.0(9) C4 C14 C15 O1 31.7(10) C4 C14 C15 C16 -152.0(5) C5 N1 C1 C2 -70.2(6) C5 C4 C14 C13 178.7(6) C5 C4 C14 C15 5.1(8) C6 C2 C3 C4 102.0(7) C6 C2 C3 C7 -79.2(7) C7 C3 C4 C5 -179.1(5) C7 C3 C4 C14 -1.1(9) C7 C8 C9 C10 1.9(11) C7 C12 C13 C14 3.9(9) C8 C7 C12 C11 2.0(9) C8 C7 C12 C13 179.1(6) C8 C9 C10 C11 -0.7(11) C9 C10 C11 C12 0.2(11) C10 C11 C12 C7 -0.9(10) C10 C11 C12 C13 -177.9(6) C11 C12 C13 C14 -179.0(6) C12 C7 C8 C9 -2.5(10) C12 C13 C14 C4 -2.0(9) C12 C13 C14 C15 171.7(6) C13 C14 C15 O1 -141.9(7) C13 C14 C15 C16 34.4(9) C14 C4 C5 N1 169.2(5) C14 C15 C16 C17 -149.2(6) C14 C15 C16 C21 34.4(9) C15 C16 C17 C18 -176.8(6) C15 C16 C21 C20 175.4(6) C16 C17 C18 C19 1.2(10) C17 C16 C21 C20 -0.8(10) C17 C18 C19 Br1 177.9(5) C17 C18 C19 C20 -1.1(12) C18 C19 C20 C21 0.1(11) C19 C20 C21 C16 0.9(11) C21 C16 C17 C18 -0.3(10) C22 S1 N1 C1 69.6(5) C22 S1 N1 C5 -61.2(5) C22 C23 C24 C25 3.1(9) C23 C22 C27 C26 0.6(9) C23 C24 C25 C26 -2.9(9) C23 C24 C25 C28 178.2(6) C24 C25 C26 C27 1.5(10) C25 C26 C27 C22 -0.4(9) C27 C22 C23 C24 -1.9(9) C28 C25 C26 C27 -179.5(6) Br2 C46 C47 C48 179.3(5) S2 N2 C29 C30 142.7(4) S2 N2 C33 C32 -160.1(3) S2 C49 C50 C51 177.8(5) S2 C49 C54 C53 -178.2(5) O4 C42 C43 C44 -159.0(6) O4 C42 C43 C48 15.9(9) O5 S2 N2 C29 179.8(4) O5 S2 N2 C33 37.4(5) O5 S2 C49 C50 157.5(5) O5 S2 C49 C54 -24.3(6) O6 S2 N2 C29 -51.3(4) O6 S2 N2 C33 166.3(4) O6 S2 C49 C50 26.1(6) O6 S2 C49 C54 -155.7(5) N2 S2 C49 C50 -87.4(5) N2 S2 C49 C54 90.8(6) N2 C29 C30 C31 47.1(6) N2 C29 C30 C56 -73.5(6) C29 N2 C33 C32 55.0(6) C29 C30 C31 C32 -13.7(7) C29 C30 C31 C34 166.0(5) C29 C30 C56 I2 -81.6(5) C30 C31 C32 C33 -0.6(8) C30 C31 C32 C41 -178.0(4) C30 C31 C34 C35 -3.1(8) C30 C31 C34 C39 178.5(5) C31 C30 C56 I2 156.0(4) C31 C32 C33 N2 -19.4(7) C31 C32 C41 C40 -0.2(8) C31 C32 C41 C42 -172.6(5) C31 C34 C35 C36 -176.5(5) C31 C34 C39 C38 177.2(5) C31 C34 C39 C40 -0.7(8) C32 C31 C34 C35 176.5(5) C32 C31 C34 C39 -1.9(8) C32 C41 C42 O4 48.4(8) C32 C41 C42 C43 -133.6(5) C33 N2 C29 C30 -71.4(6) C33 C32 C41 C40 -177.8(5) C33 C32 C41 C42 9.9(8) C34 C31 C32 C33 179.8(5) C34 C31 C32 C41 2.4(8) C34 C35 C36 C37 -1.2(10) C34 C39 C40 C41 2.9(8) C35 C34 C39 C38 -1.2(8) C35 C34 C39 C40 -179.2(5) C35 C36 C37 C38 -0.2(10) C36 C37 C38 C39 0.9(10) C37 C38 C39 C34 -0.1(9) C37 C38 C39 C40 177.8(6) C38 C39 C40 C41 -175.0(5) C39 C34 C35 C36 1.9(8) C39 C40 C41 C32 -2.5(8) C39 C40 C41 C42 170.0(5) C40 C41 C42 O4 -124.0(6) C40 C41 C42 C43 54.0(7) C41 C32 C33 N2 158.1(4) C41 C42 C43 C44 23.0(8) C41 C42 C43 C48 -162.0(6) C42 C43 C44 C45 175.0(5) C42 C43 C48 C47 -175.4(5) C43 C44 C45 C46 0.2(9) C44 C43 C48 C47 -0.2(9) C44 C45 C46 Br2 -179.4(4) C44 C45 C46 C47 -0.4(10) C45 C46 C47 C48 0.3(10) C46 C47 C48 C43 0.0(10) C48 C43 C44 C45 0.1(9) C49 S2 N2 C29 62.9(5) C49 S2 N2 C33 -79.6(5) C49 C50 C51 C52 0.9(10) C50 C49 C54 C53 -0.1(10) C50 C51 C52 C53 -1.0(10) C50 C51 C52 C55 178.0(6) C51 C52 C53 C54 0.5(10) C52 C53 C54 C49 0.0(10) C54 C49 C50 C51 -0.4(9) C55 C52 C53 C54 -178.5(6) C56 C30 C31 C32 107.6(6) C56 C30 C31 C34 -72.8(6)