#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:07:34 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293766 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571967.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_1571967 loop_ _publ_author_name 'Chen, Jia-Wei' 'Ji, Wen-Jun' 'Huang, Xue-Ying' 'Ge, Danhua' 'Shen, Zhi-Liang' 'Guo, Kai' 'Chu, Xue-Qiang' _publ_section_title ; Chemo-, regio-, and stereoselective tetrafunctionalization of fluoroalkynes enables divergent synthesis of 5-7-membered azacycles. ; _journal_issue 30 _journal_name_full 'Chemical science' _journal_page_first 12026 _journal_page_last 12035 _journal_paper_doi 10.1039/d4sc03230f _journal_volume 15 _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_moiety 'C29 H25 F7 N2 O4 S2' _chemical_formula_sum 'C29 H25 F7 N2 O4 S2' _chemical_formula_weight 662.63 _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yac' _space_group_name_H-M_alt 'P 1 n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-02-01 _audit_creation_method ; Olex2 1.5-beta (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2024-02-01 deposited with the CCDC. 2024-06-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.953(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.8892(5) _cell_length_b 5.71600(10) _cell_length_c 27.6517(7) _cell_measurement_reflns_used 3688 _cell_measurement_temperature 169.99(10) _cell_measurement_theta_max 73.2950 _cell_measurement_theta_min 2.4820 _cell_volume 2840.20(12) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 169.99(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -95.00 -44.00 1.00 1.50 -- -41.11 125.00 90.00 51 2 \w -108.00 -32.00 1.00 1.50 -- -41.11 -38.00 90.00 76 3 \w -113.00 -13.00 1.00 1.50 -- -41.11 -57.00 0.00 100 4 \w 80.00 105.00 1.00 2.00 -- 106.95 30.00 -60.00 25 5 \w 132.00 169.00 1.00 2.00 -- 106.95 30.00 -60.00 37 6 \w 125.00 171.00 1.00 2.00 -- 106.95 125.00 0.00 46 7 \w 57.00 178.00 1.00 2.00 -- 106.95 15.00-120.00 121 8 \w 38.00 105.00 1.00 2.00 -- 106.95 -94.00 0.00 67 9 \w 34.00 103.00 1.00 2.00 -- 106.95 -45.00 60.00 69 10 \w 30.00 88.00 1.00 2.00 -- 106.95 -94.00 -60.00 58 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0038061000 _diffrn_orient_matrix_UB_12 0.0170033000 _diffrn_orient_matrix_UB_13 0.0547569000 _diffrn_orient_matrix_UB_21 -0.0831387000 _diffrn_orient_matrix_UB_22 0.0641448000 _diffrn_orient_matrix_UB_23 -0.0207803000 _diffrn_orient_matrix_UB_31 -0.0206171000 _diffrn_orient_matrix_UB_32 -0.2611022000 _diffrn_orient_matrix_UB_33 -0.0014301000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_unetI/netI 0.0676 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 10438 _diffrn_reflns_point_group_measured_fraction_full 0.684 _diffrn_reflns_point_group_measured_fraction_max 0.653 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.534 _diffrn_reflns_theta_min 2.514 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.480 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.60188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description block _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.396 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.077 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.05(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 791 _refine_ls_number_reflns 7478 _refine_ls_number_restraints 740 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0538 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1347 _refine_ls_wR_factor_ref 0.1506 _reflns_Friedel_coverage 0.349 _reflns_Friedel_fraction_full 0.368 _reflns_Friedel_fraction_max 0.339 _reflns_number_gt 5937 _reflns_number_total 7478 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03230f2.cif _cod_data_source_block 3022-5 _cod_depositor_comments 'Adding full bibliography for 1571965--1571967.cif.' _cod_database_code 1571967 _shelx_shelxl_version_number 2018/3 _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. ; _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. Rigid bond restraints S2, C16 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0008 S3, C30 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0008 3. Uiso/Uaniso restraints and constraints S1 \\sim N1: within 2A with sigma of 0.0006 and sigma for terminal atoms of 0.0012 within 2A N2 \\sim S2: within 2A with sigma of 0.0006 and sigma for terminal atoms of 0.0012 within 2A N4 \\sim S4: within 2A with sigma of 0.0006 and sigma for terminal atoms of 0.0012 within 2A S3 \\sim N3: within 2A with sigma of 0.0006 and sigma for terminal atoms of 0.0012 within 2A S2 \\sim C16: within 2A with sigma of 0.000008 and sigma for terminal atoms of 0.000016 within 2A C30 \\sim S3: within 2A with sigma of 0.0008 and sigma for terminal atoms of 0.0016 within 2A Uanis(C13) \\sim Ueq: with sigma of 0.0007 and sigma for terminal atoms of 0.0014 Uanis(C51) \\sim Ueq: with sigma of 0.0009 and sigma for terminal atoms of 0.0018 Uanis(S2) = Uanis(C16) 4. Rigid body (RIGU) restrains C49, S3, O6, O5, N3, C30, C40, C37, C35, C31, C41, C45, H37A, H37B, C38, H35, C34, H31, C32, F8, C42, C46, N4, H38A, H38B, C39, H34, C33, H32, F9, C43, C47, C51, S4, H39A, H39B, C36, F10, F11, C44, C48, H47, H51, C50, O7, O8, C52, H36A, H36B, H36C, F13, F12, F14, H48, H50, C53, C56, H49, H53, C54, C57, H56, H54, C55, H57, C58, H58A, H58B, H58C with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.006 C9, S1, O2, O1, N1, C23, C1, C8, C24, C27, C2, C11, H8A, H8B, H24, C25, C28, H27, C3, C7, N2, C12, C10, H9A, H9B, H25, C26, H28, H3, C4, H7, C19, S2, F2, C13, H10A, H10B, C29, C22, H4, H19, O3, O4, C16, C14, F1, H29A, H29B, H29C, H22, C20, C17, F4, C15, F3, H20, C21, C18, H17, F7, F6, F5, H21, C6, H18, C5, H5A, H5B, H5C with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.006 5.a Secondary CH2 refined with riding coordinates: C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C8(H8A,H8B), C10(H10A,H10B), C9(H9A,H9B) 5.b Aromatic/amide H refined with riding coordinates: C24(H24), C50(H50), C35(H35), C53(H53), C3(H3), C7(H7), C34(H34), C54(H54), C20(H20), C22(H22), C48(H48), C31(H31), C25(H25), C47(H47), C51(H51), C21(H21), C32(H32), C4(H4), C57(H57), C28(H28), C49(H49), C27(H27), C18(H18), C19(H19), C17(H17), C56(H56) 5.c Idealised Me refined as rotating group: C36(H36A,H36B,H36C), C58(H58A,H58B,H58C), C5(H5A,H5B,H5C), C29(H29A,H29B,H29C) ; _shelx_res_file ; TITL 3022-5_a.res in Pn 3022-5.res created by SHELXL-2018/3 at 17:20:20 on 01-Feb-2024 REM Old TITL 3022-5 in P2(1)/n REM SHELXT solution in Pn: R1 0.137, Rweak 0.006, Alpha 0.009 REM 0.468 for 573 systematic absences, Orientation as input REM Flack x = 0.485 ( 0.033 ) from 1363 Parsons' quotients REM Formula found by SHELXT: C59 N7 O12 F6 Cl4 CELL 1.54184 18.8892 5.716 27.6517 90 107.953 90 ZERR 4 0.0005 0.0001 0.0007 0 0.003 0 LATT -1 SYMM 0.5+X,-Y,0.5+Z SFAC C H F N O S UNIT 116 100 28 8 16 8 ISOR 0.0007 0.0014 C13 ISOR 0.0009 0.0018 C51 RIGU 0.001 0.006 C49 S3 O6 O5 N3 C30 C40 C37 C35 C31 C41 C45 H37a H37b C38 = H35 C34 H31 C32 F8 C42 C46 N4 H38A H38B C39 H34 C33 H32 F9 C43 C47 C51 S4 = H39A H39B C36 F10 F11 C44 C48 H47 H51 C50 O7 O8 C52 H36A H36B H36C F13 F12 = F14 H48 H50 C53 C56 H49 H53 C54 C57 H56 H54 C55 H57 C58 H58A H58B H58C RIGU 0.001 0.006 C9 S1 O2 O1 N1 C23 C1 C8 C24 C27 C2 C11 H8a H8b H24 C25 = C28 H27 C3 C7 N2 C12 C10 H9A H9B H25 C26 H28 H3 C4 H7 C19 S2 F2 C13 H10A = H10B C29 C22 H4 H19 O3 O4 C16 C14 F1 H29A H29B H29C H22 C20 C17 F4 C15 F3 = H20 C21 C18 H17 F7 F6 F5 H21 C6 H18 C5 H5A H5B H5C SIMU 0.0006 0.0012 2 S1 N1 SIMU 0.0006 0.0012 2 N2 S2 SIMU 0.0006 0.0012 2 N4 S4 SIMU 0.0006 0.0012 2 S3 N3 DELU 0.0008 0.0008 S2 C16 SIMU 0.000008 0.000016 2 S2 C16 SIMU 0.0008 0.0016 2 C30 S3 DELU 0.0008 0.0008 S3 C30 EADP S2 C16 L.S. 10 PLAN 8 CONF temp -120 BOND list 4 fmap 2 53 MORE -1 ACTA BOND $H REM REM REM WGHT 0.076200 FVAR 0.27381 S3 6 0.914532 1.016796 0.595681 11.00000 0.02045 0.01414 = 0.02264 0.00219 0.00209 -0.00055 S4 6 0.747579 0.714620 0.399832 11.00000 0.02474 0.01588 = 0.01949 -0.00201 0.00496 0.00161 S1 6 0.244491 0.214342 0.598099 11.00000 0.02499 0.01937 = 0.02158 0.00048 0.00919 -0.00583 S2 6 0.077127 0.517253 0.401936 11.00000 0.02549 0.01713 = 0.02124 0.00275 0.00544 -0.00029 F9 3 0.680379 1.163565 0.566629 11.00000 0.05170 0.02356 = 0.03543 0.00679 0.01769 0.01320 F2 3 0.217735 0.131406 0.391122 11.00000 0.04362 0.03320 = 0.03876 -0.01657 0.02214 -0.01340 F11 3 0.597704 1.013237 0.618198 11.00000 0.03302 0.08094 = 0.04219 0.01508 0.01680 0.01254 F3 3 0.335597 0.187640 0.358936 11.00000 0.06025 0.03575 = 0.05821 0.00229 0.03454 0.01050 O7 5 0.740518 0.487444 0.418699 11.00000 0.03450 0.01625 = 0.03177 -0.00472 0.00383 0.00063 O3 5 0.043387 0.689188 0.426501 11.00000 0.03575 0.01471 = 0.02647 -0.00169 0.00597 0.00455 F8 3 0.772714 0.629375 0.607412 11.00000 0.03749 0.02424 = 0.03288 0.01163 0.00904 0.00708 F6 3 0.217377 0.407119 0.295892 11.00000 0.04111 0.10041 = 0.03813 -0.00003 -0.00137 0.00362 O2 5 0.191640 0.248130 0.625677 11.00000 0.03406 0.03166 = 0.03260 0.01086 0.01841 -0.00513 O6 5 0.868292 1.099519 0.625855 11.00000 0.02690 0.03251 = 0.03262 -0.00988 0.00648 -0.00071 O4 5 0.120912 0.600126 0.372812 11.00000 0.02644 0.02581 = 0.02715 0.01122 0.00558 -0.00521 F1 3 0.309500 0.661183 0.431440 11.00000 0.05658 0.02812 = 0.03004 -0.00657 0.02023 -0.01529 O5 5 0.946949 1.183916 0.570942 11.00000 0.02714 0.01965 = 0.03577 0.00891 0.00386 -0.00656 O1 5 0.251461 -0.012728 0.577780 11.00000 0.03634 0.01539 = 0.02775 -0.00610 0.00423 -0.00878 F14 3 0.672049 0.983618 0.716732 11.00000 0.07451 0.09669 = 0.02092 -0.00448 0.02149 -0.00224 F10 3 0.655394 0.686816 0.637178 11.00000 0.05506 0.04434 = 0.05211 -0.00384 0.03105 -0.01607 N2 4 0.129399 0.326218 0.443544 11.00000 0.02467 0.01688 = 0.02105 0.00242 0.00586 -0.00078 O8 5 0.799022 0.755015 0.372493 11.00000 0.02384 0.05986 = 0.01873 0.00407 0.00739 0.00421 N4 4 0.771061 0.907515 0.448121 11.00000 0.02332 0.01516 = 0.01964 -0.00105 0.00558 0.00055 F7 3 0.320693 0.486900 0.281102 11.00000 0.08120 0.07757 = 0.04358 0.00147 0.04185 -0.00052 N1 4 0.219639 0.401496 0.550295 11.00000 0.02385 0.01874 = 0.02158 -0.00067 0.00994 -0.00475 C13 1 0.289214 0.459934 0.408027 11.00000 0.02371 0.02294 = 0.02289 -0.00012 0.00670 -0.00014 C24 1 0.389990 0.149800 0.643206 11.00000 0.02692 0.01629 = 0.01575 -0.00003 0.00438 -0.00222 AFIX 43 H24 2 0.382400 0.009855 0.625178 11.00000 -1.20000 AFIX 0 N3 4 0.863037 0.830113 0.553914 11.00000 0.01982 0.01384 = 0.02206 0.00243 0.00285 -0.00064 C30 1 0.986379 0.835093 0.633311 11.00000 0.02003 0.01491 = 0.02137 0.00223 0.00267 -0.00064 C40 1 0.782766 0.855009 0.537832 11.00000 0.02102 0.01539 = 0.02624 0.00033 0.00528 -0.00301 C1 1 0.250335 0.371882 0.510304 11.00000 0.02292 0.01518 = 0.02129 0.00163 0.00868 -0.00194 C37 1 0.899692 0.711439 0.520720 11.00000 0.02097 0.01759 = 0.02375 -0.00282 0.00337 -0.00253 AFIX 23 H37A 2 0.870358 0.576045 0.505387 11.00000 -1.20000 H37B 2 0.948167 0.656101 0.541288 11.00000 -1.20000 AFIX 0 F12 3 0.720700 1.234982 0.680858 11.00000 0.15006 0.04571 = 0.05806 -0.01670 0.03723 -0.02612 F5 3 0.265939 0.736330 0.317537 11.00000 0.14800 0.06035 = 0.04876 0.02686 0.04547 0.03969 C50 1 0.545158 1.073561 0.429530 11.00000 0.02468 0.02414 = 0.02673 -0.00245 0.00866 0.00477 AFIX 43 H50 2 0.520564 1.202798 0.411623 11.00000 -1.20000 AFIX 0 C35 1 0.968084 0.634315 0.654557 11.00000 0.03408 0.02053 = 0.02744 0.00588 0.00626 -0.00400 AFIX 43 H35 2 0.918948 0.586684 0.648038 11.00000 -1.20000 AFIX 0 C38 1 0.909583 0.870103 0.478341 11.00000 0.02145 0.03123 = 0.02095 0.00030 0.00355 -0.00466 AFIX 23 H38A 2 0.954524 0.962219 0.491684 11.00000 -1.20000 H38B 2 0.915582 0.773432 0.451038 11.00000 -1.20000 AFIX 0 C46 1 0.658640 0.873121 0.473188 11.00000 0.02166 0.01303 = 0.01894 -0.00475 0.00624 -0.00268 C14 1 0.324685 0.414394 0.365431 11.00000 0.02107 0.03304 = 0.02670 -0.00051 0.00935 -0.00221 C53 1 0.651232 1.007234 0.334204 11.00000 0.03146 0.02487 = 0.02390 0.00475 0.01023 0.00019 AFIX 43 H53 2 0.692028 1.104583 0.337961 11.00000 -1.20000 AFIX 0 C39 1 0.845002 1.030795 0.457523 11.00000 0.02497 0.02145 = 0.02746 0.00161 0.00569 -0.00680 AFIX 23 H39A 2 0.847547 1.097420 0.425838 11.00000 -1.20000 H39B 2 0.848212 1.158208 0.481275 11.00000 -1.20000 AFIX 0 C3 1 0.372910 0.186404 0.515481 11.00000 0.02040 0.03053 = 0.01501 0.00074 0.00485 0.00242 AFIX 43 H3 2 0.347941 0.057408 0.497700 11.00000 -1.20000 AFIX 0 F4 3 0.391711 0.521035 0.378486 11.00000 0.03902 0.11315 = 0.04266 -0.02348 0.02036 -0.04112 C7 1 0.368813 0.564709 0.550833 11.00000 0.02560 0.01835 = 0.02234 0.00472 0.00867 0.00078 AFIX 43 H7 2 0.341210 0.690443 0.556591 11.00000 -1.20000 AFIX 0 C34 1 1.028930 0.503016 0.687239 11.00000 0.04235 0.02440 = 0.02013 0.00500 0.00751 0.00544 AFIX 43 H34 2 1.019161 0.367954 0.702828 11.00000 -1.20000 AFIX 0 C54 1 0.580777 1.068169 0.302472 11.00000 0.03561 0.01768 = 0.03322 0.00571 0.00789 0.00536 AFIX 43 H54 2 0.574754 1.208933 0.284798 11.00000 -1.20000 AFIX 0 C52 1 0.658275 0.796030 0.359980 11.00000 0.02785 0.02079 = 0.01529 0.00004 0.00778 0.00162 C23 1 0.332203 0.299217 0.638411 11.00000 0.02516 0.01896 = 0.01746 0.00262 0.00563 -0.00154 C20 1 -0.068664 0.410528 0.354965 11.00000 0.02747 0.02659 = 0.03075 -0.00678 0.00675 0.00242 AFIX 43 H20 2 -0.079436 0.550725 0.368262 11.00000 -1.20000 AFIX 0 C6 1 -0.110043 0.070604 0.301487 11.00000 0.02572 0.02018 = 0.01662 -0.00049 0.00007 -0.00534 C41 1 0.750263 0.826350 0.578938 11.00000 0.02630 0.02095 = 0.02663 0.00540 0.00644 0.00098 C36 1 1.162634 0.431352 0.731110 11.00000 0.04728 0.04359 = 0.02159 -0.00172 0.01240 0.01363 AFIX 137 H36A 2 1.161245 0.448189 0.765348 11.00000 -1.50000 H36B 2 1.209641 0.486220 0.729028 11.00000 -1.50000 H36C 2 1.156458 0.269515 0.721441 11.00000 -1.50000 AFIX 0 C2 1 0.333242 0.367821 0.525672 11.00000 0.02245 0.02283 = 0.01267 0.00495 0.00919 -0.00109 C55 1 0.517893 0.921506 0.296341 11.00000 0.03661 0.03278 = 0.02452 -0.00092 0.00808 -0.00102 C22 1 0.487307 0.390190 0.558954 11.00000 0.01978 0.04026 = 0.02515 0.00599 -0.00057 0.00370 AFIX 43 H22 2 0.539014 0.394165 0.571036 11.00000 -1.20000 AFIX 0 C48 1 0.540191 0.694879 0.464586 11.00000 0.03377 0.02617 = 0.02693 -0.01127 0.01476 -0.01029 AFIX 43 H48 2 0.512585 0.569197 0.470364 11.00000 -1.20000 AFIX 0 C31 1 1.058530 0.907354 0.640590 11.00000 0.02208 0.02039 = 0.02258 -0.00172 0.00482 -0.00280 AFIX 43 H31 2 1.068963 1.039666 0.624426 11.00000 -1.20000 AFIX 0 C8 1 0.148783 0.526471 0.541300 11.00000 0.02467 0.01892 = 0.02475 -0.00309 0.01297 -0.00226 AFIX 23 H8A 2 0.147322 0.656858 0.518560 11.00000 -1.20000 H8B 2 0.146201 0.589616 0.573273 11.00000 -1.20000 AFIX 0 C25 1 0.463502 0.209328 0.676522 11.00000 0.02335 0.03735 = 0.02193 -0.00055 0.00432 -0.00065 AFIX 43 H25 2 0.503816 0.109639 0.680520 11.00000 -1.20000 AFIX 0 C15 1 0.281359 0.512619 0.314777 11.00000 0.04370 0.05612 = 0.02418 0.00679 0.01224 0.00911 C47 1 0.616434 0.681155 0.481457 11.00000 0.03382 0.01384 = 0.02723 -0.00476 0.01502 -0.00548 AFIX 43 H47 2 0.640018 0.547745 0.498073 11.00000 -1.20000 AFIX 0 C45 1 0.741369 0.870651 0.488952 11.00000 0.02191 0.00595 = 0.02463 0.00038 0.00737 -0.00120 C51 1 0.620140 1.066208 0.445636 11.00000 0.02298 0.02119 = 0.02236 0.00026 0.00721 0.00071 AFIX 43 H51 2 0.646936 1.190772 0.438436 11.00000 -1.20000 AFIX 0 C11 1 0.206669 0.352927 0.460449 11.00000 0.02454 0.01294 = 0.02155 0.00178 0.00817 0.00078 C21 1 -0.125520 0.274349 0.324873 11.00000 0.02454 0.02562 = 0.02576 -0.00102 0.00232 0.00455 AFIX 43 H21 2 -0.174683 0.317773 0.319988 11.00000 -1.20000 AFIX 0 F13 3 0.773512 0.894615 0.701909 11.00000 0.04388 0.12694 = 0.03288 0.02148 -0.00256 0.00868 C32 1 1.115740 0.773010 0.673437 11.00000 0.02507 0.04029 = 0.02693 0.00266 0.00465 0.00700 AFIX 43 H32 2 1.164869 0.821031 0.680133 11.00000 -1.20000 AFIX 0 C4 1 0.451091 0.190777 0.531406 11.00000 0.02024 0.03654 = 0.02439 0.00333 0.00769 0.00980 AFIX 43 H4 2 0.478296 0.067366 0.524181 11.00000 -1.20000 AFIX 0 C12 1 0.242084 0.324241 0.419321 11.00000 0.02381 0.02238 = 0.01959 -0.00063 0.00567 0.00068 C57 1 0.531005 0.716605 0.321978 11.00000 0.03121 0.02680 = 0.02398 -0.00577 0.00980 -0.00706 AFIX 43 H57 2 0.490975 0.615236 0.317468 11.00000 -1.20000 AFIX 0 C33 1 1.100757 0.572750 0.695831 11.00000 0.04126 0.03434 = 0.01908 -0.00460 0.00872 0.00633 C28 1 0.410540 0.569142 0.696184 11.00000 0.03968 0.03359 = 0.01552 -0.00503 0.01108 -0.00566 AFIX 43 H28 2 0.416494 0.710192 0.713749 11.00000 -1.20000 AFIX 0 C49 1 0.504024 0.883717 0.439993 11.00000 0.03130 0.03043 = 0.03063 -0.01072 0.01822 -0.00293 AFIX 43 H49 2 0.452318 0.889561 0.429923 11.00000 -1.20000 AFIX 0 C58 1 0.443926 0.999827 0.263386 11.00000 0.03958 0.04792 = 0.04001 0.00609 0.00429 0.00432 AFIX 137 H58A 2 0.438589 1.164694 0.267902 11.00000 -1.50000 H58B 2 0.405655 0.916858 0.272434 11.00000 -1.50000 H58C 2 0.439639 0.968645 0.228483 11.00000 -1.50000 AFIX 0 C27 1 0.341459 0.509455 0.664455 11.00000 0.03448 0.01914 = 0.02161 0.00301 0.00954 0.00206 AFIX 43 H27 2 0.301213 0.609397 0.660485 11.00000 -1.20000 AFIX 0 C26 1 0.471388 0.425109 0.702678 11.00000 0.02826 0.03866 = 0.01419 -0.00100 0.00728 -0.01030 C18 1 -0.034740 0.004114 0.312577 11.00000 0.02962 0.01979 = 0.02339 -0.00103 0.00461 0.00288 AFIX 43 H18 2 -0.023169 -0.133628 0.298768 11.00000 -1.20000 AFIX 0 C16 1 0.005051 0.337819 0.365452 11.00000 0.02549 0.01713 = 0.02124 0.00275 0.00544 -0.00029 C19 1 0.448136 0.573425 0.567879 11.00000 0.02632 0.02807 = 0.02510 0.00569 0.00507 -0.00472 AFIX 43 H19 2 0.472650 0.704483 0.585017 11.00000 -1.20000 AFIX 0 C17 1 0.020613 0.134718 0.342561 11.00000 0.02109 0.02322 = 0.02649 0.00187 0.00496 0.00475 AFIX 43 H17 2 0.069777 0.089453 0.348131 11.00000 -1.20000 AFIX 0 C10 1 0.094459 0.210241 0.478225 11.00000 0.02486 0.02418 = 0.02708 -0.00101 0.00767 -0.01180 AFIX 23 H10A 2 0.126224 0.082442 0.495236 11.00000 -1.20000 H10B 2 0.047374 0.143396 0.458143 11.00000 -1.20000 AFIX 0 C43 1 0.666047 0.914832 0.631551 11.00000 0.02979 0.04039 = 0.02701 -0.00036 0.00954 -0.00171 C56 1 0.596185 0.648589 0.352972 11.00000 0.03477 0.02436 = 0.02377 -0.00414 0.00862 -0.00574 AFIX 43 H56 2 0.600909 0.505901 0.369833 11.00000 -1.20000 AFIX 0 C9 1 0.080542 0.369235 0.518121 11.00000 0.02600 0.03203 = 0.02870 -0.00004 0.01388 -0.00912 AFIX 23 H9A 2 0.070814 0.275712 0.544653 11.00000 -1.20000 H9B 2 0.037152 0.465666 0.502811 11.00000 -1.20000 AFIX 0 C5 1 -0.172475 -0.070416 0.266860 11.00000 0.03694 0.03721 = 0.03036 -0.01008 -0.00149 -0.01281 AFIX 137 H5A 2 -0.207022 -0.112788 0.284577 11.00000 -1.50000 H5B 2 -0.152666 -0.209512 0.256441 11.00000 -1.50000 H5C 2 -0.197594 0.021022 0.237455 11.00000 -1.50000 AFIX 0 C29 1 0.549108 0.493195 0.735957 11.00000 0.03020 0.06612 = 0.03187 -0.00320 0.00301 -0.01779 AFIX 137 H29A 2 0.545999 0.628639 0.755731 11.00000 -1.50000 H29B 2 0.579652 0.527987 0.714828 11.00000 -1.50000 H29C 2 0.570651 0.365865 0.758285 11.00000 -1.50000 AFIX 0 C42 1 0.701205 0.960339 0.591847 11.00000 0.03163 0.02360 = 0.01688 0.00132 0.00240 0.00432 C44 1 0.709492 1.012303 0.685505 11.00000 0.05301 0.04516 = 0.02414 -0.00274 0.01164 -0.00458 HKLF 4 REM 3022-5_a.res in Pn REM wR2 = 0.1506, GooF = S = 1.037, Restrained GooF = 1.012 for all data REM R1 = 0.0538 for 5937 Fo > 4sig(Fo) and 0.0679 for all 7478 data REM 791 parameters refined using 740 restraints END WGHT 0.0762 0.0000 REM Highest difference peak 0.396, deepest hole -0.445, 1-sigma level 0.077 Q1 1 0.2579 0.0288 0.5975 11.00000 0.05 0.40 Q2 1 0.8872 0.8499 0.5821 11.00000 0.05 0.38 Q3 1 0.1025 0.3445 0.4157 11.00000 0.05 0.37 Q4 1 0.7360 0.5204 0.4014 11.00000 0.05 0.35 Q5 1 0.2209 0.3605 0.5651 11.00000 0.05 0.34 Q6 1 0.4600 0.4813 0.7010 11.00000 0.05 0.33 Q7 1 0.5355 0.9945 0.2984 11.00000 0.05 0.32 Q8 1 0.1604 0.4401 0.3605 11.00000 0.05 0.30 ; _shelx_res_checksum 63716 _shelx_hkl_file ; 0 0 -2 842.93 16.32 0 0 -3 0.21 0.20 0 0 -4 2440.42 45.81 0 0 -5 1.19 0.59 0 0 -6 82.11 4.34 0 0 -7 0.48 0.60 0 0 -8 297.13 10.59 0 0 -9 0.38 0.68 0 0 -10 164.40 8.38 0 0 -11 0.23 0.83 0 0 -12 315.42 13.37 0 0 -13 0.05 0.90 0 0 -14 2.95 1.23 0 0 -15 -0.12 1.56 0 0 -16 26.65 4.65 0 0 -17 0.81 1.04 0 0 18 112.21 9.83 0 0 -18 108.21 9.95 0 0 -19 0.65 1.82 0 0 -19 0.56 1.59 0 0 19 2.22 1.56 0 0 20 4.25 1.82 0 0 -20 6.26 3.06 0 0 -20 7.06 2.79 0 0 -21 -1.15 2.18 0 0 21 0.86 1.40 0 0 -21 -0.83 1.93 0 0 -22 65.11 7.96 0 0 -23 -0.82 1.29 0 0 -24 125.05 11.26 0 0 -25 -1.49 2.01 0 0 -26 193.37 13.78 0 0 -27 1.23 1.05 0 0 -28 11.94 3.16 0 0 29 -0.21 1.29 0 0 -29 2.00 1.57 0 0 30 103.37 8.68 0 0 31 -2.15 1.34 0 0 32 -0.84 0.98 0 -1 0 0.00 0.45 0 1 -1 103.84 3.27 0 -1 -1 96.06 4.65 0 -1 1 99.62 4.61 0 -1 2 982.43 21.20 0 1 -2 922.61 18.54 0 -1 3 316.86 6.96 0 1 -3 315.89 8.02 0 -1 4 205.23 5.15 0 1 -4 208.79 6.45 0 -1 -5 137.58 5.94 0 1 -5 137.83 5.43 0 -1 5 136.22 4.25 0 -1 6 1789.07 34.47 0 1 -6 1795.99 36.35 0 -1 -6 1770.25 37.32 0 1 -7 14.36 1.88 0 -1 7 14.83 1.62 0 -1 -7 13.81 2.05 0 -1 8 1094.51 24.12 0 -1 -8 1066.00 26.80 0 1 -8 1131.88 26.00 0 1 -9 6.73 1.56 0 -1 9 5.42 1.25 0 -1 -9 6.91 1.70 0 1 -10 0.08 0.76 0 -1 10 0.77 0.55 0 -1 -10 -0.23 0.78 0 -1 -11 45.81 4.82 0 1 -11 42.03 4.27 0 -1 11 37.99 3.48 0 1 -12 32.22 4.11 0 -1 -12 31.27 4.26 0 -1 12 28.58 3.25 0 -1 -13 226.65 12.39 0 -1 13 201.63 9.51 0 1 -13 214.92 11.29 0 1 -14 16.00 3.10 0 -1 -14 15.13 3.38 0 -1 14 9.87 2.02 0 -1 -15 0.62 1.12 0 -1 15 1.91 1.18 0 1 -15 2.60 1.75 0 1 -16 94.28 8.34 0 -1 -16 86.46 8.61 0 -1 -17 26.30 5.00 0 1 -17 19.70 3.96 0 1 -18 22.32 4.36 0 -1 -18 16.93 3.87 0 1 -19 38.77 5.60 0 -1 -19 44.52 6.01 0 1 -19 49.78 6.89 0 -1 -19 48.93 6.84 0 -1 -20 61.39 7.28 0 1 -20 59.19 7.29 0 -1 -20 59.76 7.63 0 1 -20 55.58 7.83 0 -1 -21 1.15 1.02 0 -1 -21 1.52 2.10 0 1 -21 -0.94 1.43 0 1 -21 1.13 2.34 0 1 21 -1.54 1.58 0 -1 -22 111.17 10.68 0 1 -22 89.63 10.63 0 1 -22 112.55 10.42 0 -1 -22 111.81 10.03 0 1 22 92.34 10.86 0 -1 -23 59.17 7.78 0 -1 -23 61.56 7.32 0 1 -23 52.56 7.04 0 -1 -24 143.47 11.34 0 1 -24 139.26 11.72 0 -1 -24 116.23 10.96 0 -1 -25 -0.31 1.29 0 1 -25 0.33 1.28 0 -1 -25 -2.57 1.99 0 1 -26 25.80 5.01 0 -1 -26 33.95 5.27 0 -1 -26 32.85 5.64 0 -1 -27 56.64 6.44 0 1 -27 57.05 7.00 0 -1 -27 56.15 7.01 0 1 -28 13.84 3.54 0 1 28 14.47 3.56 0 -1 28 10.52 3.15 0 1 -29 8.07 2.26 0 1 29 12.40 3.02 0 -1 29 14.26 3.37 0 1 30 -1.85 1.46 0 -1 30 1.86 1.11 0 1 31 0.33 0.91 0 1 32 0.71 1.12 0 -2 0 162.90 8.31 0 2 0 141.22 5.06 0 -2 -1 115.22 7.00 0 -2 1 124.33 7.18 0 2 -1 113.39 4.44 0 2 -2 374.41 9.94 0 -2 2 402.43 13.98 0 -2 -2 380.07 14.27 0 -2 -3 326.16 13.16 0 2 -3 306.29 8.92 0 -2 3 340.71 12.54 0 -2 -4 116.35 7.64 0 2 -4 118.12 5.14 0 -2 -5 508.25 18.09 0 2 -5 501.95 13.59 0 2 -6 404.38 12.27 0 2 -7 15.47 2.17 0 2 -8 45.83 3.97 0 2 -9 0.63 0.65 0 2 -10 177.28 9.17 0 2 -11 185.02 9.96 0 2 -12 23.05 3.57 0 2 -13 4.34 2.00 0 2 -14 5.12 1.83 0 2 -15 11.61 3.12 0 -2 -16 21.20 4.26 0 2 -16 29.27 4.97 0 -2 -17 6.93 2.44 0 -2 -17 8.97 3.00 0 2 -17 10.91 2.94 0 -2 -18 5.05 2.13 0 2 -18 6.47 2.44 0 -2 -19 3.45 2.04 0 2 -19 9.75 2.75 0 -2 -19 5.77 2.66 0 -2 -20 70.65 7.94 0 2 -20 62.31 8.41 0 -2 -20 81.17 9.12 0 -2 -21 1.68 2.09 0 -2 -21 1.94 1.08 0 -2 -22 1.29 1.82 0 -2 -22 2.33 2.25 0 -2 -23 74.81 8.17 0 -2 -23 58.38 7.77 0 -2 -24 25.33 4.74 0 -2 -25 -0.41 1.43 0 -2 -26 41.08 5.51 0 2 26 31.41 5.26 0 2 27 30.84 4.96 0 -2 -27 33.31 4.84 0 2 28 65.07 6.76 0 2 29 2.52 1.57 0 2 30 0.47 0.86 0 2 31 24.67 3.04 0 -3 0 -0.81 1.11 0 -3 -1 369.74 17.18 0 -3 1 375.75 16.98 0 -3 2 2.52 1.90 0 -3 -2 1.16 1.35 0 -3 3 113.93 8.72 0 -3 -3 108.98 9.10 0 -3 -4 1.62 1.41 0 -3 -5 82.72 7.84 0 -3 -6 360.82 17.58 0 -3 -7 5.28 2.33 0 -3 -8 83.47 8.51 0 -3 -9 178.96 12.98 0 -3 -10 172.95 13.14 0 -3 -11 6.27 2.61 0 -3 -12 84.55 9.62 0 -3 13 1.55 1.05 0 -3 -13 1.52 1.91 0 -3 -13 1.43 1.51 0 -3 -14 95.04 8.88 0 -3 -14 88.81 10.59 0 -3 14 98.11 7.80 0 -3 15 2.47 0.83 0 -3 -15 0.79 1.07 0 -3 -16 14.83 4.72 0 -3 -16 11.34 3.23 0 -3 16 18.58 3.56 0 -3 -17 5.21 2.54 0 -3 17 4.87 1.74 0 -3 -17 2.00 1.89 0 -3 18 26.26 3.96 0 -3 -18 35.82 5.68 0 3 19 102.34 10.90 0 -3 -19 83.52 8.77 0 -3 -20 11.04 3.19 0 3 20 7.99 2.62 0 -3 -21 0.23 1.05 0 3 21 -0.33 1.75 0 -3 -22 4.74 1.74 0 3 22 -6.86 2.86 0 3 23 1.50 1.40 0 -3 -23 0.73 1.47 0 3 24 24.69 4.75 0 -3 -24 30.27 4.77 0 3 25 6.79 2.18 0 -3 -25 5.62 2.10 0 3 26 1.11 1.19 0 3 27 3.33 1.49 0 3 28 0.75 0.88 0 -3 29 2.07 0.76 0 -4 0 47.06 6.82 0 -4 0 36.19 4.67 0 -4 1 57.36 7.69 0 -4 -1 57.32 6.01 0 -4 -1 60.57 7.91 0 -4 1 58.84 6.05 0 -4 2 107.56 8.19 0 -4 -2 111.36 10.99 0 -4 -2 112.71 8.61 0 -4 -3 -0.91 1.41 0 -4 3 2.43 1.57 0 -4 3 0.76 1.12 0 -4 -3 1.53 1.17 0 -4 4 112.32 8.44 0 -4 4 96.84 7.72 0 -4 -4 96.59 10.32 0 -4 -4 108.28 8.52 0 -4 5 7.20 2.22 0 -4 5 3.61 1.25 0 -4 -5 5.02 2.47 0 -4 -5 10.02 2.69 0 -4 -6 82.83 7.48 0 -4 -6 73.96 8.95 0 -4 6 78.39 6.90 0 -4 6 88.26 7.53 0 -4 -7 4.32 2.13 0 -4 7 2.92 2.05 0 -4 7 2.29 1.07 0 -4 -7 2.15 1.20 0 -4 7 2.83 1.60 0 -4 8 9.71 2.30 0 -4 8 10.16 2.72 0 -4 -8 8.73 2.98 0 -4 -8 10.94 2.71 0 -4 8 8.67 2.89 0 -4 9 32.16 4.46 0 -4 -9 21.88 4.97 0 -4 9 34.92 6.06 0 -4 -9 29.57 4.41 0 -4 9 28.69 4.48 0 -4 10 270.30 17.46 0 -4 -10 264.32 13.70 0 -4 10 311.83 15.02 0 -4 -11 4.23 2.62 0 -4 11 7.77 2.53 0 -4 -11 4.29 1.77 0 -4 11 5.70 2.65 0 -4 -12 108.01 9.09 0 -4 -12 82.66 10.29 0 -4 -13 44.27 5.81 0 -4 13 48.03 5.70 0 -4 14 216.00 12.39 0 -4 -14 189.85 12.77 0 -4 15 25.76 4.23 0 -4 -15 19.54 4.21 0 -4 -16 55.22 6.84 0 -4 16 57.70 6.13 0 -4 -17 13.58 3.39 0 -4 17 20.72 3.71 0 -4 -18 0.40 1.31 0 -4 18 -0.44 1.31 0 -4 -19 1.46 1.18 0 -4 19 0.45 1.03 0 -4 -20 0.72 1.05 0 -4 20 1.36 1.38 0 -4 -21 5.47 1.86 0 -4 22 110.06 9.88 0 -4 -22 121.89 9.26 0 -4 23 32.30 5.01 0 -4 24 1.32 1.54 0 -4 25 33.18 4.44 0 -4 26 17.06 2.93 0 -5 0 -5.40 1.93 0 -5 0 -0.70 1.57 0 -5 -1 16.78 3.52 0 -5 -1 20.17 3.60 0 -5 1 18.53 3.37 0 -5 1 18.15 3.62 0 -5 2 354.22 16.44 0 -5 2 375.76 17.02 0 -5 -2 385.55 17.56 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21.58 3.40 -18 -2 -2 24.92 5.19 -18 2 -3 3.91 1.92 -18 2 -3 5.60 1.80 -18 -2 -3 3.03 1.94 -18 2 -4 9.94 2.69 -18 -2 -4 13.94 3.90 -18 -2 -5 -0.33 1.30 -18 -2 -6 2.40 1.58 -18 -2 -7 1.42 1.23 -18 -2 -8 0.34 0.89 -18 -2 -9 21.69 3.42 -18 -2 -10 6.84 1.71 -18 3 23 4.43 1.07 18 -3 -23 6.19 1.38 -18 3 22 1.53 0.79 -18 3 21 0.25 0.61 -18 3 20 1.25 1.02 -18 3 19 0.94 0.82 -18 3 18 -0.66 1.15 -18 3 17 34.08 4.24 -18 3 16 14.87 2.89 -18 3 15 3.05 1.68 -18 3 14 59.26 5.95 -18 3 13 9.71 2.50 -18 3 12 14.60 3.10 -18 3 11 3.92 1.28 -18 3 10 1.37 1.36 -18 3 9 -2.21 1.66 -18 3 8 5.92 2.12 -18 3 7 1.41 1.15 -18 3 6 2.26 1.37 -18 -3 6 -0.07 1.42 -18 3 5 1.36 1.47 -18 3 5 4.38 1.91 -18 -3 5 2.28 1.91 -18 3 4 23.07 4.08 -18 3 4 28.57 4.05 -18 -3 4 19.16 3.90 -18 3 3 2.05 1.70 -18 3 3 -0.97 0.90 -18 -3 3 2.94 1.45 -18 3 2 2.41 1.81 -18 3 2 1.93 1.03 -18 -3 2 1.09 1.30 -18 3 1 6.44 1.74 -18 3 1 3.95 1.48 -18 -3 1 3.57 1.65 -18 3 0 16.31 3.14 -18 3 0 19.91 3.13 -18 -3 0 19.55 3.87 -18 3 -1 -1.52 0.91 -18 3 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63.46 6.65 -19 0 14 0.08 1.04 -19 0 13 12.32 3.03 -19 0 12 0.42 1.07 -19 0 11 124.49 9.62 -19 0 10 1.16 1.63 -19 0 9 5.73 2.22 -19 0 8 -0.73 1.70 -19 0 7 -4.13 1.92 -19 0 6 0.96 1.54 -19 0 5 275.33 15.08 -19 0 4 0.80 1.43 -19 0 3 13.89 3.26 -19 0 2 -0.72 1.10 -19 0 1 172.92 11.66 -19 0 0 -1.14 1.28 -19 0 -1 3.15 1.55 -19 0 -2 0.36 0.90 -19 0 -3 57.57 6.31 -19 0 -4 0.52 1.09 -19 0 -5 16.66 3.49 -19 0 -6 -1.54 1.15 -19 0 -7 48.42 5.19 -19 0 -8 -0.75 0.86 -19 1 26 6.20 1.51 -19 1 25 34.94 3.73 -19 1 24 -0.08 0.72 -19 1 23 1.47 0.90 -19 1 22 10.99 2.52 -19 1 21 0.38 0.90 -19 1 20 11.28 2.84 -19 1 19 44.96 5.42 -19 1 18 18.08 3.65 -19 1 17 29.17 4.61 -19 1 16 15.31 3.39 -19 1 15 47.08 5.93 -19 1 14 36.08 5.19 -19 1 13 9.82 2.93 -19 -1 12 0.93 1.15 -19 1 12 0.32 1.21 -19 -1 11 189.24 11.41 -19 1 11 247.33 13.91 -19 -1 10 4.81 1.90 -19 1 10 6.81 2.51 -19 -1 9 7.97 2.28 -19 1 9 10.37 3.06 -19 1 9 14.51 2.75 -19 -1 8 -1.08 1.11 -19 1 8 0.34 1.08 -19 1 8 0.81 1.10 -19 -1 7 9.21 2.62 -19 1 7 10.87 2.99 -19 1 7 13.11 2.67 -19 -1 6 -0.26 1.18 -19 1 6 1.97 1.39 -19 1 6 1.43 1.17 -19 -1 5 3.37 1.53 -19 1 5 3.34 2.16 -19 1 5 2.60 1.23 -19 -1 4 13.61 3.13 -19 1 4 17.46 3.82 -19 1 4 17.36 3.03 -19 -1 3 32.48 4.71 -19 1 3 26.17 3.65 -19 1 3 36.85 5.17 -19 -1 2 0.22 1.33 -19 1 2 2.21 1.18 -19 1 2 2.57 1.76 -19 -1 1 9.12 2.41 -19 1 1 10.12 2.36 -19 1 1 14.16 3.51 -19 -1 0 22.55 3.94 -19 1 0 20.59 3.12 -19 1 0 20.26 3.85 -19 -1 -1 6.45 2.19 -19 1 -1 10.01 2.80 -19 1 -2 12.56 2.98 -19 1 -3 14.69 3.09 -19 -1 -3 11.00 3.27 -19 1 -3 11.47 3.17 -19 1 -4 5.08 2.00 -19 -1 -4 3.91 2.40 -19 1 -4 4.49 2.05 -19 -1 -5 -0.50 1.41 -19 -1 -6 2.33 1.23 -19 -1 -7 42.32 5.04 -19 -1 -8 7.43 1.91 -19 -1 -9 24.75 3.23 -19 2 25 13.79 2.18 -19 2 24 3.46 1.29 -19 2 23 32.74 3.70 -19 2 22 23.50 3.26 -19 2 21 4.43 1.69 -19 2 20 0.39 0.91 -19 2 19 9.88 2.52 -19 2 18 32.91 4.40 -19 2 17 107.25 8.16 -19 2 16 80.06 7.17 -19 2 15 6.34 2.26 -19 2 14 1.95 1.82 -19 2 13 8.04 2.51 -19 2 12 1.15 1.37 -19 2 11 16.41 3.43 -19 2 10 7.28 2.39 -19 2 9 17.13 3.74 -19 2 8 12.23 3.24 -19 2 7 54.79 6.49 -19 2 7 50.16 5.33 -19 2 6 1.33 1.98 -19 2 6 0.16 0.93 -19 2 5 12.67 3.13 -19 2 5 10.30 2.34 -19 2 4 2.57 2.18 -19 2 4 0.88 0.74 -19 2 3 52.14 6.28 -19 2 3 54.29 5.36 -19 2 2 7.07 2.50 -19 2 2 4.77 1.73 -19 2 1 2.75 1.45 -19 2 1 4.20 1.47 -19 2 0 0.76 0.96 -19 2 0 -1.31 0.86 -19 2 -1 31.27 4.62 -19 2 -1 24.85 3.38 -19 -2 -1 28.41 4.87 -19 2 -2 78.61 7.07 -19 -2 -2 76.09 7.90 -19 2 -3 5.83 1.88 -19 -2 -3 9.55 2.70 -19 -2 -4 41.22 5.34 -19 -2 -5 21.06 3.57 -19 -2 -6 4.07 1.53 -19 -2 -7 56.20 5.21 -19 -2 -8 33.84 3.67 -19 3 21 16.15 2.23 -19 3 20 -0.05 0.80 -19 3 19 4.51 1.31 -19 3 18 1.13 1.07 -19 3 17 6.95 1.85 -19 3 16 2.90 1.30 -19 3 15 9.48 2.17 -19 3 14 63.76 5.64 -19 3 13 15.08 2.89 -19 3 12 -0.73 0.99 -19 3 11 2.69 1.54 -19 3 10 13.26 2.71 -19 3 9 -0.20 0.74 -19 3 9 0.32 0.67 -19 3 8 0.74 0.87 -19 3 8 0.16 0.97 -19 3 7 2.89 1.41 -19 3 7 3.20 1.24 -19 3 6 4.15 1.87 -19 3 6 2.11 1.13 -19 -3 6 0.32 1.01 -19 3 5 10.92 2.51 -19 3 5 8.08 1.92 -19 -3 5 6.58 2.17 -19 3 4 2.06 1.36 -19 3 4 3.72 1.42 -19 -3 4 3.51 1.90 -19 3 3 13.64 2.82 -19 3 3 17.89 2.92 -19 -3 3 8.60 2.28 -19 3 2 12.92 2.73 -19 3 2 10.82 2.26 -19 -3 2 10.78 2.62 -19 3 1 36.88 4.29 -19 3 1 41.20 4.19 -19 -3 1 36.80 4.68 -19 3 0 60.70 5.38 -19 3 0 72.49 5.44 -19 -3 0 69.69 6.28 -19 -3 -1 0.42 1.00 -19 -3 -2 4.78 1.67 -19 -3 -3 77.62 5.85 -19 4 14 1.36 0.61 -19 4 13 6.89 1.52 -19 4 12 -0.34 0.58 -19 4 11 8.98 1.63 -19 4 10 11.23 1.85 -19 4 9 1.94 0.89 -19 4 8 7.84 1.54 -19 4 7 1.80 0.73 -19 4 6 -0.89 0.82 -19 4 5 -0.46 0.69 -19 4 4 4.80 1.11 -19 4 3 2.25 0.85 -20 0 23 -0.16 0.55 -20 0 22 1.02 1.02 -20 0 21 -0.06 0.88 -20 0 20 53.43 5.11 -20 0 19 -1.28 1.36 -20 0 18 47.49 5.12 -20 0 17 1.12 1.33 -20 0 16 8.43 2.34 -20 0 15 1.43 1.38 -20 0 14 7.43 2.24 -20 0 13 0.47 0.83 -20 0 12 29.35 4.52 -20 0 11 -0.22 1.18 -20 0 10 10.93 2.94 -20 0 9 -0.92 1.10 -20 0 8 3.85 1.86 -20 0 7 -0.47 1.08 -20 0 6 31.33 4.71 -20 0 5 0.13 1.11 -20 0 4 6.18 2.42 -20 0 3 1.33 0.83 -20 0 2 79.80 7.26 -20 0 1 1.82 1.41 -20 0 0 2.96 1.71 -20 0 -1 -1.25 1.22 -20 0 -2 1.96 1.18 -20 0 -2 1.52 1.50 -20 0 -3 1.83 1.40 -20 0 -4 3.28 1.58 -20 0 -5 0.32 0.92 -20 0 -6 11.01 2.27 -20 1 25 24.07 2.68 -20 1 24 2.37 1.00 -20 1 23 0.50 0.71 -20 1 22 3.48 1.27 -20 1 21 12.52 2.55 -20 1 20 0.72 0.79 -20 1 19 15.63 3.10 -20 1 18 2.57 1.49 -20 1 17 73.93 6.73 -20 1 16 1.28 1.41 -20 1 15 7.65 3.02 -20 1 14 2.98 1.90 -20 1 13 23.46 4.00 -20 1 12 16.67 3.52 -20 1 11 -1.36 1.37 -20 -1 10 22.04 3.63 -20 1 10 27.61 4.39 -20 -1 9 9.98 2.41 -20 1 9 6.45 2.49 -20 -1 8 -1.35 1.36 -20 1 8 -0.56 1.44 -20 -1 7 10.38 2.70 -20 1 7 12.98 3.13 -20 -1 6 2.32 1.43 -20 1 6 -0.30 1.45 -20 -1 5 7.34 2.10 -20 1 5 11.17 2.77 -20 1 4 39.54 5.28 -20 -1 4 26.14 3.92 -20 -1 3 16.49 3.23 -20 1 3 12.59 2.24 -20 1 3 21.73 4.02 -20 -1 2 8.46 2.34 -20 1 2 10.53 2.54 -20 -1 1 62.18 5.92 -20 1 1 78.60 7.13 -20 1 0 36.83 4.89 -20 1 -1 -0.14 1.00 -20 -1 -1 -1.91 1.69 -20 1 -2 6.08 1.84 -20 -1 -2 6.04 2.17 -20 1 -2 5.36 2.07 -20 -1 -3 18.64 3.52 -20 -1 -4 14.52 3.00 -20 -1 -5 1.86 1.32 -20 -1 -6 4.64 1.58 -20 -1 -7 8.98 1.85 -20 2 23 3.93 1.34 -20 2 22 -0.21 0.69 -20 2 21 0.50 0.78 -20 2 20 75.54 5.86 -20 2 19 9.45 2.27 -20 2 18 0.76 1.13 -20 2 17 2.01 1.32 -20 2 16 44.04 4.88 -20 2 15 0.38 1.08 -20 2 14 2.51 0.82 -20 2 13 5.88 1.84 -20 2 12 10.68 2.64 -20 2 11 6.94 2.35 -20 2 11 8.60 2.02 -20 2 10 22.61 3.73 -20 2 10 17.86 2.91 -20 2 9 -0.56 0.91 -20 2 9 0.04 0.85 -20 2 8 88.54 7.57 -20 2 8 78.56 6.11 -20 2 7 1.41 1.44 -20 2 7 1.48 0.87 -20 2 6 1.96 0.96 -20 2 6 1.73 0.76 -20 2 5 3.06 1.51 -20 2 5 7.09 1.83 -20 2 4 65.14 6.56 -20 2 4 62.85 5.31 -20 2 3 1.24 1.54 -20 2 3 0.10 0.61 -20 2 2 10.45 2.48 -20 2 2 12.01 2.24 -20 -2 2 14.56 3.43 -20 2 1 9.97 2.01 -20 2 1 8.97 2.29 -20 -2 1 8.27 2.51 -20 2 0 42.09 4.85 -20 -2 0 43.01 5.46 -20 2 -1 1.74 1.15 -20 -2 -1 0.32 1.18 -20 -2 -2 57.69 5.88 -20 -2 -3 3.13 1.38 -20 -2 -4 2.20 1.14 -20 -2 -5 -0.84 0.90 -20 3 18 81.20 5.04 -20 3 17 3.17 1.23 -20 3 16 23.08 2.84 -20 3 15 13.83 2.36 -20 3 14 17.08 2.59 -20 3 13 7.81 1.90 -20 3 13 7.96 1.73 -20 3 12 13.43 2.49 -20 3 12 9.26 1.89 -20 3 11 2.77 1.37 -20 3 11 1.88 1.06 -20 3 10 5.04 1.54 -20 3 10 2.98 1.22 -20 3 9 1.05 0.67 -20 3 9 2.71 1.11 -20 3 8 6.89 1.88 -20 3 8 11.09 2.11 -20 3 7 8.05 1.89 -20 3 7 9.53 2.03 -20 3 6 24.14 3.01 -20 3 6 16.90 2.76 -20 3 5 0.76 0.87 -20 3 5 0.45 0.74 -20 3 4 -0.87 0.70 -20 3 4 2.78 1.13 -20 3 3 10.53 2.05 -20 3 3 14.53 2.25 -20 -3 3 8.40 1.89 -20 3 2 26.97 2.93 -21 0 21 16.46 2.36 -21 0 20 0.57 0.71 -21 0 19 44.99 4.31 -21 0 18 0.29 0.79 -21 0 17 123.63 7.80 -21 0 16 -0.01 0.69 -21 0 15 41.92 4.66 -21 0 14 0.45 1.05 -21 0 13 3.55 1.58 -21 0 12 0.36 0.82 -21 0 11 5.86 1.95 -21 0 10 -1.30 1.00 -21 0 9 5.63 2.05 -21 0 8 1.23 1.15 -21 0 7 33.12 4.45 -21 0 6 1.00 1.42 -21 0 5 1.04 0.95 -21 0 4 -1.90 1.24 -21 0 3 114.07 8.03 -21 0 2 -0.17 1.09 -21 0 1 34.32 4.22 -21 0 0 -0.24 1.21 -21 0 -1 34.52 4.49 -21 0 -2 -1.10 1.21 -21 0 -3 39.63 4.23 -21 1 22 16.38 2.37 -21 1 21 30.23 3.51 -21 1 20 0.02 0.57 -21 1 19 2.66 1.03 -21 1 18 3.57 1.43 -21 1 17 16.23 2.97 -21 1 16 5.50 1.97 -21 1 15 -0.91 1.23 -21 1 14 -0.38 1.12 -21 1 13 -0.64 0.98 -21 1 12 0.97 1.05 -21 1 11 22.47 3.74 -21 1 10 16.46 3.32 -21 1 9 20.40 3.59 -21 1 8 16.87 3.30 -21 1 7 5.92 1.86 -21 1 6 13.92 3.03 -21 -1 5 14.59 2.69 -21 1 5 14.35 3.11 -21 -1 4 13.66 2.51 -21 1 4 20.41 3.48 -21 1 3 0.27 0.77 -21 1 2 1.90 1.29 -21 1 1 15.00 2.80 -21 -1 1 16.22 3.31 -21 1 0 23.96 3.46 -21 -1 0 25.75 4.01 -21 1 0 23.55 3.43 -21 1 -1 12.41 2.41 -21 -1 -1 7.56 2.25 -21 -1 -2 18.11 3.16 -21 -1 -3 15.53 2.71 -21 -1 -4 37.91 3.88 -21 2 20 -0.83 0.95 -21 2 19 2.53 1.05 -21 2 18 1.12 1.13 -21 2 17 1.64 1.15 -21 2 16 1.33 1.07 -21 2 15 7.86 1.97 -21 2 14 2.51 0.96 -21 2 14 2.90 0.96 -21 2 13 0.37 0.78 -21 2 13 1.42 0.82 -21 2 12 11.89 2.53 -21 2 12 10.52 1.93 -21 2 11 3.16 1.50 -21 2 11 3.17 1.08 -21 2 10 0.94 0.94 -21 2 10 0.83 0.68 -21 2 9 15.51 2.90 -21 2 9 8.72 1.76 -21 2 8 22.04 2.77 -21 2 8 25.92 3.77 -21 2 7 4.71 1.75 -21 2 7 5.77 1.43 -21 2 6 11.59 2.00 -21 2 6 11.59 2.54 -21 2 5 10.68 1.89 -21 2 5 9.04 2.32 -21 -2 5 12.06 2.82 -21 2 4 37.19 4.39 -21 2 4 37.18 3.42 -21 -2 4 32.65 4.42 -21 2 3 1.75 1.12 -21 -2 3 3.22 1.48 -21 2 2 19.36 3.16 -21 -2 2 19.68 3.25 -21 2 1 9.87 2.09 -21 -2 1 11.43 2.47 -21 -2 0 0.25 1.01 -21 -2 -1 18.68 2.86 -21 3 10 -0.37 0.52 -21 3 9 1.53 0.74 -21 3 8 7.71 1.49 -21 3 7 17.05 2.09 -22 0 18 2.73 0.96 -22 0 17 0.03 0.51 -22 0 16 1.50 0.92 -22 0 15 -0.07 0.65 -22 0 14 0.13 0.58 -22 0 13 -1.19 1.03 -22 0 12 3.66 1.30 -22 0 11 -0.98 1.25 -22 0 10 0.45 0.70 -22 0 9 1.46 1.20 -22 0 8 70.39 5.81 -22 0 7 -0.91 0.97 -22 0 6 25.60 3.52 -22 0 5 0.17 0.64 -22 0 4 66.67 5.36 -22 0 3 0.84 0.82 -22 0 2 57.62 5.49 -22 0 1 1.21 1.11 -22 0 0 17.71 2.76 -22 1 19 35.96 3.50 -22 1 18 9.41 1.90 -22 1 17 4.50 1.27 -22 1 16 3.47 1.24 -22 1 15 0.49 0.67 -22 1 14 2.76 1.34 -22 1 13 8.53 2.12 -22 1 12 3.78 1.52 -22 1 11 68.68 5.95 -22 1 10 5.23 1.89 -22 1 9 3.05 1.49 -22 1 8 -0.75 0.95 -22 1 7 3.74 1.60 -22 1 6 13.00 2.55 -22 1 5 7.35 2.06 -22 1 4 -0.54 1.07 -22 1 3 0.58 0.70 -22 -1 3 0.79 0.61 -22 1 2 6.67 1.68 -22 -1 2 6.75 2.02 -22 -1 1 10.35 2.28 -22 -1 0 7.66 1.82 -22 2 16 3.84 1.17 -22 2 15 -0.07 0.66 -22 2 14 0.84 0.89 -22 2 13 1.47 0.85 -22 2 12 7.58 1.78 -22 2 11 8.55 1.92 -22 2 10 12.35 2.24 -22 2 9 0.17 0.61 -22 -2 9 1.97 0.96 -22 2 8 0.35 0.77 -22 -2 8 -1.67 0.85 -22 2 7 1.82 1.04 -22 -2 7 2.37 1.18 -22 2 6 14.74 2.44 -22 -2 6 11.51 2.24 -22 2 5 0.21 0.72 -22 -2 5 1.55 0.95 -22 2 4 0.01 0.86 -23 1 14 0.50 0.77 -23 1 13 0.76 0.74 -23 1 12 0.38 0.81 -23 1 11 7.15 1.67 -23 1 10 4.64 1.43 -23 1 9 44.24 3.99 -23 1 8 2.09 0.95 -23 1 7 4.86 1.26 -23 -1 7 4.79 1.44 -23 1 6 1.30 0.74 -23 -1 6 3.57 1.32 0 0 0 0.00 0.00 TITL 3022-5 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 18.889226 5.716017 27.651688 90.0000 107.9535 90.0000 ZERR 12.00 0.000505 0.000119 0.000676 0.0000 0.0028 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 132.00 120.00 12.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 43738 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.525 _oxdiff_exptl_absorpt_empirical_full_min 0.662 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.91453(4) 1.01680(13) 0.59568(3) 0.02011(14) Uani 1 1 d . U . . . S4 S 0.74758(4) 0.71462(13) 0.39983(3) 0.02046(16) Uani 1 1 d . U . . . S1 S 0.24449(4) 0.21434(14) 0.59810(3) 0.02152(16) Uani 1 1 d . U . . . S2 S 0.07713(4) 0.51725(14) 0.40194(3) 0.02169(5) Uani 1 1 d . U . . . F9 F 0.68038(12) 1.1636(3) 0.56663(8) 0.0359(6) Uani 1 1 d . . . . . F2 F 0.21773(12) 0.1314(4) 0.39112(8) 0.0364(6) Uani 1 1 d . . . . . F11 F 0.59770(12) 1.0132(5) 0.61820(9) 0.0509(7) Uani 1 1 d . . . . . F3 F 0.33560(13) 0.1876(4) 0.35894(10) 0.0477(7) Uani 1 1 d . . . . . O7 O 0.74052(14) 0.4874(4) 0.41870(10) 0.0290(7) Uani 1 1 d . . . . . O3 O 0.04339(13) 0.6892(4) 0.42650(9) 0.0265(7) Uani 1 1 d . . . . . F8 F 0.77271(12) 0.6294(4) 0.60741(8) 0.0319(6) Uani 1 1 d . . . . . F6 F 0.21738(15) 0.4071(6) 0.29589(10) 0.0630(9) Uani 1 1 d . . . . . O2 O 0.19164(13) 0.2481(4) 0.62568(9) 0.0309(7) Uani 1 1 d . . . . . O6 O 0.86829(13) 1.0995(4) 0.62585(10) 0.0313(7) Uani 1 1 d . . . . . O4 O 0.12091(13) 0.6001(4) 0.37281(9) 0.0271(6) Uani 1 1 d . . . . . F1 F 0.30950(13) 0.6612(4) 0.43144(8) 0.0367(6) Uani 1 1 d . . . . . O5 O 0.94695(13) 1.1839(4) 0.57094(10) 0.0288(7) Uani 1 1 d . . . . . O1 O 0.25146(14) -0.0127(4) 0.57778(10) 0.0278(7) Uani 1 1 d . . . . . F14 F 0.67205(16) 0.9836(6) 0.71673(9) 0.0625(8) Uani 1 1 d . . . . . F10 F 0.65539(13) 0.6868(4) 0.63718(9) 0.0472(7) Uani 1 1 d . . . . . N2 N 0.12940(15) 0.3262(5) 0.44354(10) 0.0211(3) Uani 1 1 d . U . . . O8 O 0.79902(13) 0.7550(5) 0.37249(9) 0.0340(7) Uani 1 1 d . . . . . N4 N 0.77106(15) 0.9075(4) 0.44812(10) 0.0196(3) Uani 1 1 d . U . . . F7 F 0.32069(16) 0.4869(6) 0.28110(10) 0.0623(8) Uani 1 1 d . . . . . N1 N 0.21964(14) 0.4015(5) 0.55029(10) 0.0207(3) Uani 1 1 d . U . . . C13 C 0.28921(18) 0.4599(6) 0.40803(13) 0.0233(4) Uani 1 1 d . U . . . C24 C 0.38999(18) 0.1498(5) 0.64321(12) 0.0201(7) Uani 1 1 d . . . . . H24 H 0.382400 0.009855 0.625178 0.024 Uiso 1 1 calc R U . . . N3 N 0.86304(14) 0.8301(4) 0.55391(10) 0.0194(3) Uani 1 1 d . U . . . C30 C 0.98638(17) 0.8351(5) 0.63331(12) 0.0196(3) Uani 1 1 d . U . . . C40 C 0.78277(18) 0.8550(5) 0.53783(13) 0.0213(6) Uani 1 1 d . . . . . C1 C 0.25033(17) 0.3719(5) 0.51030(12) 0.0194(6) Uani 1 1 d . . . . . C37 C 0.89969(17) 0.7114(6) 0.52072(12) 0.0216(6) Uani 1 1 d . . . . . H37A H 0.870358 0.576045 0.505387 0.026 Uiso 1 1 calc R U . . . H37B H 0.948167 0.656101 0.541288 0.026 Uiso 1 1 calc R U . . . F12 F 0.7207(2) 1.2350(5) 0.68086(12) 0.0834(12) Uani 1 1 d . . . . . F5 F 0.2659(2) 0.7363(5) 0.31754(11) 0.0823(11) Uani 1 1 d . . . . . C50 C 0.54516(18) 1.0736(6) 0.42953(13) 0.0250(7) Uani 1 1 d . . . . . H50 H 0.520564 1.202798 0.411623 0.030 Uiso 1 1 calc R U . . . C35 C 0.9681(2) 0.6343(6) 0.65456(14) 0.0281(7) Uani 1 1 d . . . . . H35 H 0.918948 0.586684 0.648038 0.034 Uiso 1 1 calc R U . . . C38 C 0.90958(18) 0.8701(6) 0.47834(13) 0.0252(7) Uani 1 1 d . . . . . H38A H 0.954524 0.962219 0.491684 0.030 Uiso 1 1 calc R U . . . H38B H 0.915582 0.773432 0.451038 0.030 Uiso 1 1 calc R U . . . C46 C 0.65864(17) 0.8731(5) 0.47319(12) 0.0179(6) Uani 1 1 d . . . . . C14 C 0.32469(18) 0.4144(6) 0.36543(13) 0.0265(5) Uani 1 1 d . . . . . C53 C 0.6512(2) 1.0072(6) 0.33420(13) 0.0264(7) Uani 1 1 d . . . . . H53 H 0.692028 1.104583 0.337961 0.032 Uiso 1 1 calc R U . . . C39 C 0.84500(18) 1.0308(6) 0.45752(14) 0.0252(8) Uani 1 1 d . . . . . H39A H 0.847547 1.097420 0.425838 0.030 Uiso 1 1 calc R U . . . H39B H 0.848212 1.158208 0.481275 0.030 Uiso 1 1 calc R U . . . C3 C 0.37291(17) 0.1864(6) 0.51548(12) 0.0221(7) Uani 1 1 d . . . . . H3 H 0.347941 0.057408 0.497700 0.027 Uiso 1 1 calc R U . . . F4 F 0.39171(13) 0.5210(6) 0.37849(10) 0.0632(8) Uani 1 1 d . . . . . C7 C 0.36881(18) 0.5647(6) 0.55083(12) 0.0218(7) Uani 1 1 d . . . . . H7 H 0.341210 0.690443 0.556591 0.026 Uiso 1 1 calc R U . . . C34 C 1.0289(2) 0.5030(6) 0.68724(13) 0.0294(8) Uani 1 1 d . . . . . H34 H 1.019161 0.367954 0.702828 0.035 Uiso 1 1 calc R U . . . C54 C 0.5808(2) 1.0682(6) 0.30247(14) 0.0295(8) Uani 1 1 d . . . . . H54 H 0.574754 1.208933 0.284798 0.035 Uiso 1 1 calc R U . . . C52 C 0.65828(18) 0.7960(6) 0.35998(12) 0.0211(7) Uani 1 1 d . . . . . C23 C 0.33220(18) 0.2992(6) 0.63841(12) 0.0207(6) Uani 1 1 d . . . . . C20 C -0.06866(19) 0.4105(6) 0.35497(14) 0.0288(8) Uani 1 1 d . . . . . H20 H -0.079436 0.550725 0.368262 0.035 Uiso 1 1 calc R U . . . C6 C -0.11004(18) 0.0706(6) 0.30149(12) 0.0223(6) Uani 1 1 d . . . . . C41 C 0.75026(19) 0.8264(6) 0.57894(13) 0.0250(6) Uani 1 1 d . . . . . C36 C 1.1626(2) 0.4314(7) 0.73111(14) 0.0371(10) Uani 1 1 d . . . . . H36A H 1.161245 0.448189 0.765348 0.056 Uiso 1 1 calc R U . . . H36B H 1.209641 0.486220 0.729028 0.056 Uiso 1 1 calc R U . . . H36C H 1.156458 0.269515 0.721441 0.056 Uiso 1 1 calc R U . . . C2 C 0.33324(17) 0.3678(6) 0.52567(11) 0.0185(6) Uani 1 1 d . . . . . C55 C 0.5179(2) 0.9215(7) 0.29634(14) 0.0316(7) Uani 1 1 d . . . . . C22 C 0.48731(19) 0.3902(7) 0.55895(14) 0.0301(8) Uani 1 1 d . . . . . H22 H 0.539014 0.394165 0.571036 0.036 Uiso 1 1 calc R U . . . C48 C 0.54019(19) 0.6949(6) 0.46459(13) 0.0277(7) Uani 1 1 d . . . . . H48 H 0.512585 0.569197 0.470364 0.033 Uiso 1 1 calc R U . . . C31 C 1.05853(17) 0.9074(6) 0.64059(13) 0.0222(7) Uani 1 1 d . . . . . H31 H 1.068963 1.039666 0.624426 0.027 Uiso 1 1 calc R U . . . C8 C 0.14878(17) 0.5265(6) 0.54130(13) 0.0216(7) Uani 1 1 d . . . . . H8A H 0.147322 0.656858 0.518560 0.026 Uiso 1 1 calc R U . . . H8B H 0.146201 0.589616 0.573273 0.026 Uiso 1 1 calc R U . . . C25 C 0.46350(19) 0.2093(7) 0.67652(13) 0.0281(7) Uani 1 1 d . . . . . H25 H 0.503816 0.109639 0.680520 0.034 Uiso 1 1 calc R U . . . C15 C 0.2814(2) 0.5126(8) 0.31478(15) 0.0409(6) Uani 1 1 d . . . . . C47 C 0.61643(19) 0.6812(5) 0.48146(13) 0.0237(7) Uani 1 1 d . . . . . H47 H 0.640018 0.547745 0.498073 0.028 Uiso 1 1 calc R U . . . C45 C 0.74137(17) 0.8707(5) 0.48895(12) 0.0175(5) Uani 1 1 d . . . . . C51 C 0.62014(18) 1.0662(6) 0.44564(12) 0.0221(4) Uani 1 1 d . U . . . H51 H 0.646936 1.190772 0.438436 0.027 Uiso 1 1 calc R U . . . C11 C 0.20667(17) 0.3529(5) 0.46045(12) 0.0194(6) Uani 1 1 d . . . . . C21 C -0.1255(2) 0.2743(6) 0.32487(13) 0.0265(7) Uani 1 1 d . . . . . H21 H -0.174683 0.317773 0.319988 0.032 Uiso 1 1 calc R U . . . F13 F 0.77351(15) 0.8946(7) 0.70191(10) 0.0712(9) Uani 1 1 d . . . . . C32 C 1.1157(2) 0.7730(7) 0.67344(14) 0.0315(8) Uani 1 1 d . . . . . H32 H 1.164869 0.821031 0.680133 0.038 Uiso 1 1 calc R U . . . C4 C 0.45109(18) 0.1908(7) 0.53141(13) 0.0269(7) Uani 1 1 d . . . . . H4 H 0.478296 0.067366 0.524181 0.032 Uiso 1 1 calc R U . . . C12 C 0.24208(18) 0.3242(6) 0.41932(12) 0.0222(5) Uani 1 1 d . . . . . C57 C 0.5310(2) 0.7166(6) 0.32198(13) 0.0270(7) Uani 1 1 d . . . . . H57 H 0.490975 0.615236 0.317468 0.032 Uiso 1 1 calc R U . . . C33 C 1.1008(2) 0.5728(7) 0.69583(13) 0.0317(7) Uani 1 1 d . . . . . C28 C 0.4105(2) 0.5691(7) 0.69618(13) 0.0290(8) Uani 1 1 d . . . . . H28 H 0.416494 0.710192 0.713749 0.035 Uiso 1 1 calc R U . . . C49 C 0.50402(19) 0.8837(6) 0.43999(13) 0.0288(7) Uani 1 1 d . . . . . H49 H 0.452318 0.889561 0.429923 0.035 Uiso 1 1 calc R U . . . C58 C 0.4439(2) 0.9998(8) 0.26339(17) 0.0443(12) Uani 1 1 d . . . . . H58A H 0.438589 1.164694 0.267902 0.066 Uiso 1 1 calc R U . . . H58B H 0.405655 0.916858 0.272434 0.066 Uiso 1 1 calc R U . . . H58C H 0.439639 0.968645 0.228483 0.066 Uiso 1 1 calc R U . . . C27 C 0.3415(2) 0.5095(6) 0.66445(13) 0.0249(7) Uani 1 1 d . . . . . H27 H 0.301213 0.609397 0.660485 0.030 Uiso 1 1 calc R U . . . C26 C 0.47139(19) 0.4251(7) 0.70268(12) 0.0269(7) Uani 1 1 d . . . . . C18 C -0.03474(19) 0.0041(6) 0.31258(13) 0.0251(7) Uani 1 1 d . . . . . H18 H -0.023169 -0.133628 0.298768 0.030 Uiso 1 1 calc R U . . . C16 C 0.00505(18) 0.3378(6) 0.36545(12) 0.02169(5) Uani 1 1 d . U . . . C19 C 0.44814(19) 0.5734(6) 0.56788(13) 0.0271(7) Uani 1 1 d . . . . . H19 H 0.472650 0.704483 0.585017 0.033 Uiso 1 1 calc R U . . . C17 C 0.02061(18) 0.1347(6) 0.34256(13) 0.0241(7) Uani 1 1 d . . . . . H17 H 0.069777 0.089453 0.348131 0.029 Uiso 1 1 calc R U . . . C10 C 0.09446(18) 0.2102(6) 0.47823(13) 0.0254(6) Uani 1 1 d . . . . . H10A H 0.126224 0.082442 0.495236 0.031 Uiso 1 1 calc R U . . . H10B H 0.047374 0.143396 0.458143 0.031 Uiso 1 1 calc R U . . . C43 C 0.6660(2) 0.9148(7) 0.63155(14) 0.0322(6) Uani 1 1 d . . . . . C56 C 0.5962(2) 0.6486(6) 0.35297(13) 0.0277(8) Uani 1 1 d . . . . . H56 H 0.600909 0.505901 0.369833 0.033 Uiso 1 1 calc R U . . . C9 C 0.08054(18) 0.3692(6) 0.51812(14) 0.0277(7) Uani 1 1 d . . . . . H9A H 0.070814 0.275712 0.544653 0.033 Uiso 1 1 calc R U . . . H9B H 0.037152 0.465666 0.502811 0.033 Uiso 1 1 calc R U . . . C5 C -0.1725(2) -0.0704(7) 0.26686(15) 0.0375(10) Uani 1 1 d . . . . . H5A H -0.207022 -0.112788 0.284577 0.056 Uiso 1 1 calc R U . . . H5B H -0.152666 -0.209512 0.256441 0.056 Uiso 1 1 calc R U . . . H5C H -0.197594 0.021022 0.237455 0.056 Uiso 1 1 calc R U . . . C29 C 0.5491(2) 0.4932(9) 0.73596(16) 0.0442(12) Uani 1 1 d . . . . . H29A H 0.545999 0.628639 0.755731 0.066 Uiso 1 1 calc R U . . . H29B H 0.579652 0.527987 0.714828 0.066 Uiso 1 1 calc R U . . . H29C H 0.570651 0.365865 0.758285 0.066 Uiso 1 1 calc R U . . . C42 C 0.7012(2) 0.9603(6) 0.59185(13) 0.0252(6) Uani 1 1 d . . . . . C44 C 0.7095(3) 1.0123(8) 0.68551(15) 0.0408(6) Uani 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 S3 0.0204(2) 0.0141(2) 0.0226(2) 0.0022(2) 0.0021(2) -0.0005(2) S4 0.0247(3) 0.0159(3) 0.0195(3) -0.0020(2) 0.0050(2) 0.0016(2) S1 0.0250(3) 0.0194(3) 0.0216(3) 0.0005(2) 0.0092(2) -0.0058(2) S2 0.02549(7) 0.01713(7) 0.02124(7) 0.00275(7) 0.00544(7) -0.00029(7) F9 0.0517(12) 0.0236(8) 0.0354(10) 0.0068(7) 0.0177(9) 0.0132(8) F2 0.0436(10) 0.0332(9) 0.0388(10) -0.0166(7) 0.0221(8) -0.0134(8) F11 0.0330(9) 0.0809(17) 0.0422(12) 0.0151(12) 0.0168(8) 0.0125(10) F3 0.0603(13) 0.0358(9) 0.0582(13) 0.0023(9) 0.0345(10) 0.0105(9) O7 0.0345(12) 0.0163(10) 0.0318(12) -0.0047(9) 0.0038(10) 0.0006(9) O3 0.0357(12) 0.0147(10) 0.0265(11) -0.0017(9) 0.0060(9) 0.0046(9) F8 0.0375(10) 0.0242(8) 0.0329(10) 0.0116(7) 0.0090(8) 0.0071(8) F6 0.0411(11) 0.1004(19) 0.0381(13) 0.0000(15) -0.0014(11) 0.0036(11) O2 0.0341(11) 0.0317(12) 0.0326(11) 0.0109(10) 0.0184(9) -0.0051(9) O6 0.0269(11) 0.0325(12) 0.0326(12) -0.0099(10) 0.0065(10) -0.0007(10) O4 0.0264(10) 0.0258(11) 0.0271(11) 0.0112(9) 0.0056(9) -0.0052(9) F1 0.0566(12) 0.0281(8) 0.0300(9) -0.0066(7) 0.0202(8) -0.0153(8) O5 0.0271(10) 0.0196(10) 0.0358(12) 0.0089(10) 0.0039(9) -0.0066(9) O1 0.0363(12) 0.0154(10) 0.0277(11) -0.0061(9) 0.0042(10) -0.0088(9) F14 0.0745(12) 0.097(2) 0.0209(8) -0.0045(11) 0.0215(7) -0.0022(14) F10 0.0551(12) 0.0443(9) 0.0521(12) -0.0038(10) 0.0310(9) -0.0161(9) N2 0.0247(4) 0.0169(4) 0.0210(4) 0.0024(4) 0.0059(4) -0.0008(4) O8 0.0238(10) 0.0599(16) 0.0187(10) 0.0041(11) 0.0074(9) 0.0042(11) N4 0.0233(4) 0.0152(4) 0.0196(4) -0.0011(4) 0.0056(4) 0.0005(4) F7 0.0812(13) 0.0776(19) 0.0436(10) 0.0015(12) 0.0418(7) -0.0005(14) N1 0.0238(4) 0.0187(4) 0.0216(4) -0.0007(4) 0.0099(4) -0.0047(4) C13 0.0237(5) 0.0229(5) 0.0229(5) -0.0001(4) 0.0067(4) -0.0001(4) C24 0.0269(9) 0.0163(12) 0.0158(13) 0.0000(11) 0.0044(9) -0.0022(8) N3 0.0198(4) 0.0138(4) 0.0221(4) 0.0024(4) 0.0029(4) -0.0006(4) C30 0.0200(5) 0.0149(5) 0.0214(5) 0.0022(5) 0.0027(5) -0.0006(4) C40 0.0210(8) 0.0154(13) 0.0262(8) 0.0003(10) 0.0053(6) -0.0030(10) C1 0.0229(8) 0.0152(13) 0.0213(8) 0.0016(10) 0.0087(6) -0.0019(10) C37 0.0210(12) 0.0176(12) 0.0237(10) -0.0028(8) 0.0034(7) -0.0025(9) F12 0.150(3) 0.0457(10) 0.0581(16) -0.0167(12) 0.0372(17) -0.0261(13) F5 0.148(3) 0.0603(11) 0.0488(14) 0.0269(11) 0.0455(14) 0.0397(13) C50 0.0247(8) 0.0241(12) 0.0267(15) -0.0024(11) 0.0087(9) 0.0048(8) C35 0.0341(13) 0.0205(11) 0.0274(14) 0.0059(9) 0.0063(10) -0.0040(9) C38 0.0214(12) 0.0312(13) 0.0209(11) 0.0003(9) 0.0035(9) -0.0047(9) C46 0.0217(8) 0.0130(9) 0.0189(13) -0.0048(8) 0.0062(9) -0.0027(7) C14 0.0211(9) 0.0330(10) 0.0267(9) -0.0005(9) 0.0093(7) -0.0022(8) C53 0.0315(12) 0.0249(11) 0.0239(13) 0.0047(9) 0.0102(10) 0.0002(10) C39 0.0250(9) 0.0215(13) 0.0275(16) 0.0016(12) 0.0057(11) -0.0068(8) C3 0.0204(8) 0.0305(12) 0.0150(13) 0.0007(10) 0.0049(8) 0.0024(8) F4 0.0390(9) 0.1131(19) 0.0427(12) -0.0235(14) 0.0204(9) -0.0411(10) C7 0.0256(9) 0.0184(11) 0.0223(13) 0.0047(10) 0.0087(10) 0.0008(9) C34 0.0424(10) 0.0244(14) 0.0201(14) 0.0050(11) 0.0075(10) 0.0054(9) C54 0.0356(10) 0.0177(13) 0.0332(16) 0.0057(13) 0.0079(11) 0.0054(9) C52 0.0279(11) 0.0208(10) 0.0153(12) 0.0000(9) 0.0078(10) 0.0016(8) C23 0.0252(10) 0.0190(10) 0.0175(12) 0.0026(8) 0.0056(9) -0.0015(8) C20 0.0275(9) 0.0266(14) 0.0307(16) -0.0068(12) 0.0067(10) 0.0024(9) C6 0.0257(9) 0.0202(10) 0.0166(12) -0.0005(9) 0.0001(9) -0.0053(8) C41 0.0263(10) 0.0209(10) 0.0266(9) 0.0054(8) 0.0064(6) 0.0010(8) C36 0.0473(16) 0.0436(18) 0.0216(15) -0.0017(13) 0.0124(12) 0.0136(13) C2 0.0224(8) 0.0228(9) 0.0127(11) 0.0050(8) 0.0092(8) -0.0011(7) C55 0.0366(11) 0.0328(11) 0.0245(14) -0.0009(10) 0.0081(11) -0.0010(9) C22 0.0198(12) 0.0403(11) 0.0252(15) 0.0060(10) -0.0006(10) 0.0037(8) C48 0.0338(9) 0.0262(12) 0.0269(14) -0.0113(10) 0.0148(10) -0.0103(9) C31 0.0221(9) 0.0204(13) 0.0226(13) -0.0017(11) 0.0048(9) -0.0028(8) C8 0.0247(9) 0.0189(12) 0.0247(14) -0.0031(11) 0.0130(9) -0.0023(8) C25 0.0234(11) 0.0373(12) 0.0219(13) -0.0006(10) 0.0043(10) -0.0007(11) C15 0.0437(11) 0.0561(12) 0.0242(10) 0.0068(11) 0.0122(7) 0.0091(10) C47 0.0338(9) 0.0138(11) 0.0272(14) -0.0048(10) 0.0150(9) -0.0055(8) C45 0.0219(8) 0.0060(11) 0.0246(8) 0.0004(9) 0.0074(6) -0.0012(9) C51 0.0230(6) 0.0212(7) 0.0224(7) 0.0003(5) 0.0072(5) 0.0007(5) C11 0.0245(8) 0.0129(13) 0.0216(8) 0.0018(10) 0.0082(6) 0.0008(9) C21 0.0245(13) 0.0256(11) 0.0258(14) -0.0010(9) 0.0023(10) 0.0046(9) F13 0.0439(11) 0.127(2) 0.0329(13) 0.0215(15) -0.0026(11) 0.0087(12) C32 0.0251(13) 0.0403(12) 0.0269(14) 0.0027(9) 0.0047(10) 0.0070(10) C4 0.0202(9) 0.0365(13) 0.0244(15) 0.0033(11) 0.0077(10) 0.0098(10) C12 0.0238(9) 0.0224(10) 0.0196(9) -0.0006(8) 0.0057(6) 0.0007(8) C57 0.0312(11) 0.0268(11) 0.0240(13) -0.0058(9) 0.0098(10) -0.0071(10) C33 0.0413(10) 0.0343(12) 0.0191(13) -0.0046(9) 0.0087(9) 0.0063(9) C28 0.0397(10) 0.0336(15) 0.0155(13) -0.0050(12) 0.0111(9) -0.0057(9) C49 0.0313(12) 0.0304(10) 0.0306(14) -0.0107(9) 0.0182(10) -0.0029(8) C58 0.0396(14) 0.048(2) 0.040(2) 0.0061(18) 0.0043(14) 0.0043(15) C27 0.0345(12) 0.0191(10) 0.0216(13) 0.0030(9) 0.0095(10) 0.0021(10) C26 0.0283(10) 0.0387(11) 0.0142(12) -0.0010(9) 0.0073(9) -0.0103(8) C18 0.0296(9) 0.0198(13) 0.0234(14) -0.0010(11) 0.0046(10) 0.0029(9) C16 0.02549(7) 0.01713(7) 0.02124(7) 0.00275(7) 0.00544(7) -0.00029(7) C19 0.0263(9) 0.0281(12) 0.0251(15) 0.0057(11) 0.0051(10) -0.0047(9) C17 0.0211(12) 0.0232(10) 0.0265(13) 0.0019(9) 0.0050(9) 0.0047(9) C10 0.0249(12) 0.0242(13) 0.0271(10) -0.0010(8) 0.0077(8) -0.0118(10) C43 0.0298(10) 0.0404(10) 0.0270(10) -0.0004(10) 0.0095(7) -0.0017(9) C56 0.0348(10) 0.0244(13) 0.0238(15) -0.0041(12) 0.0086(10) -0.0057(9) C9 0.0260(12) 0.0320(13) 0.0287(12) 0.0000(10) 0.0139(9) -0.0091(9) C5 0.0369(16) 0.0372(17) 0.0304(17) -0.0101(14) -0.0015(13) -0.0128(12) C29 0.0302(13) 0.066(3) 0.0319(19) -0.0032(19) 0.0030(13) -0.0178(15) C42 0.0316(10) 0.0236(10) 0.0169(9) 0.0013(8) 0.0024(7) 0.0043(8) C44 0.0530(11) 0.0452(11) 0.0241(10) -0.0027(10) 0.0116(7) -0.0046(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 S3 N3 106.37(15) . . ? O6 S3 C30 109.84(16) . . ? O5 S3 O6 118.72(16) . . ? O5 S3 N3 110.28(15) . . ? O5 S3 C30 108.17(15) . . ? N3 S3 C30 102.22(14) . . ? O7 S4 O8 120.03(18) . . ? O7 S4 N4 109.83(15) . . ? O7 S4 C52 106.84(15) . . ? O8 S4 N4 105.03(16) . . ? O8 S4 C52 107.62(15) . . ? N4 S4 C52 106.83(14) . . ? O2 S1 N1 105.29(15) . . ? O2 S1 C23 107.36(16) . . ? O1 S1 O2 119.28(16) . . ? O1 S1 N1 108.05(15) . . ? O1 S1 C23 108.40(15) . . ? N1 S1 C23 107.98(15) . . ? O3 S2 N2 111.86(14) . . ? O3 S2 C16 106.89(16) . . ? O4 S2 O3 117.54(15) . . ? O4 S2 N2 106.75(15) . . ? O4 S2 C16 110.96(16) . . ? N2 S2 C16 101.72(14) . . ? C11 N2 S2 119.6(2) . . ? C11 N2 C10 117.5(2) . . ? C10 N2 S2 116.9(2) . . ? C39 N4 S4 116.4(2) . . ? C45 N4 S4 117.4(2) . . ? C45 N4 C39 120.1(3) . . ? C1 N1 S1 117.8(2) . . ? C1 N1 C8 120.0(3) . . ? C8 N1 S1 118.0(2) . . ? F1 C13 C14 113.1(3) . . ? C12 C13 F1 121.6(4) . . ? C12 C13 C14 125.2(3) . . ? C23 C24 H24 120.1 . . ? C23 C24 C25 119.8(3) . . ? C25 C24 H24 120.1 . . ? C40 N3 S3 119.1(2) . . ? C40 N3 C37 120.1(2) . . ? C37 N3 S3 116.4(2) . . ? C35 C30 S3 119.4(3) . . ? C31 C30 S3 117.0(2) . . ? C31 C30 C35 123.6(3) . . ? N3 C40 C41 113.7(3) . . ? C45 C40 N3 123.1(3) . . ? C45 C40 C41 122.6(3) . . ? N1 C1 C2 115.4(3) . . ? C11 C1 N1 122.1(3) . . ? C11 C1 C2 122.5(3) . . ? N3 C37 H37A 108.9 . . ? N3 C37 H37B 108.9 . . ? N3 C37 C38 113.2(3) . . ? H37A C37 H37B 107.8 . . ? C38 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C51 C50 H50 120.1 . . ? C51 C50 C49 119.7(3) . . ? C49 C50 H50 120.1 . . ? C30 C35 H35 121.8 . . ? C30 C35 C34 116.5(3) . . ? C34 C35 H35 121.8 . . ? C37 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? C39 C38 C37 112.3(3) . . ? C39 C38 H38A 109.1 . . ? C39 C38 H38B 109.1 . . ? C47 C46 C45 122.6(3) . . ? C51 C46 C47 118.2(3) . . ? C51 C46 C45 119.1(3) . . ? F3 C14 C13 112.8(3) . . ? F3 C14 F4 107.7(3) . . ? F3 C14 C15 107.5(3) . . ? F4 C14 C13 108.1(3) . . ? F4 C14 C15 106.1(3) . . ? C15 C14 C13 114.2(3) . . ? C54 C53 H53 121.2 . . ? C52 C53 H53 121.2 . . ? C52 C53 C54 117.6(3) . . ? N4 C39 H39A 109.1 . . ? N4 C39 H39B 109.1 . . ? C38 C39 N4 112.4(3) . . ? C38 C39 H39A 109.1 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.9 . . ? C2 C3 H3 119.5 . . ? C2 C3 C4 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C7 H7 120.2 . . ? C2 C7 C19 119.5(3) . . ? C19 C7 H7 120.3 . . ? C35 C34 H34 119.4 . . ? C33 C34 C35 121.2(3) . . ? C33 C34 H34 119.4 . . ? C53 C54 H54 119.0 . . ? C53 C54 C55 121.9(3) . . ? C55 C54 H54 119.1 . . ? C53 C52 S4 118.1(3) . . ? C53 C52 C56 120.4(3) . . ? C56 C52 S4 121.5(2) . . ? C24 C23 S1 117.4(2) . . ? C24 C23 C27 121.7(3) . . ? C27 C23 S1 120.9(3) . . ? C21 C20 H20 120.0 . . ? C21 C20 C16 119.9(3) . . ? C16 C20 H20 120.0 . . ? C21 C6 C18 117.5(3) . . ? C21 C6 C5 120.2(3) . . ? C18 C6 C5 122.3(3) . . ? F8 C41 C40 114.3(3) . . ? C42 C41 F8 116.0(3) . . ? C42 C41 C40 129.7(3) . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? C3 C2 C1 123.4(3) . . ? C3 C2 C7 120.8(3) . . ? C7 C2 C1 115.8(3) . . ? C54 C55 C58 119.3(3) . . ? C57 C55 C54 115.9(3) . . ? C57 C55 C58 124.7(4) . . ? C4 C22 H22 119.3 . . ? C19 C22 H22 119.3 . . ? C19 C22 C4 121.3(3) . . ? C47 C48 H48 118.9 . . ? C49 C48 H48 118.9 . . ? C49 C48 C47 122.3(3) . . ? C30 C31 H31 121.3 . . ? C30 C31 C32 117.3(3) . . ? C32 C31 H31 121.3 . . ? N1 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? N1 C8 C9 112.9(3) . . ? H8A C8 H8B 107.8 . . ? C9 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C24 C25 H25 121.4 . . ? C26 C25 C24 117.3(3) . . ? C26 C25 H25 121.3 . . ? F6 C15 F7 108.0(3) . . ? F6 C15 F5 106.1(4) . . ? F6 C15 C14 111.9(4) . . ? F7 C15 C14 110.0(3) . . ? F5 C15 F7 108.7(4) . . ? F5 C15 C14 112.1(3) . . ? C46 C47 H47 120.5 . . ? C48 C47 C46 119.0(3) . . ? C48 C47 H47 120.5 . . ? N4 C45 C46 113.7(3) . . ? C40 C45 N4 124.1(3) . . ? C40 C45 C46 122.0(3) . . ? C50 C51 C46 121.2(3) . . ? C50 C51 H51 119.4 . . ? C46 C51 H51 119.4 . . ? N2 C11 C12 113.6(3) . . ? C1 C11 N2 125.9(3) . . ? C1 C11 C12 120.0(3) . . ? C20 C21 C6 120.8(3) . . ? C20 C21 H21 119.6 . . ? C6 C21 H21 119.6 . . ? C31 C32 H32 119.2 . . ? C33 C32 C31 121.5(3) . . ? C33 C32 H32 119.2 . . ? C3 C4 C22 117.9(3) . . ? C3 C4 H4 121.1 . . ? C22 C4 H4 121.1 . . ? F2 C12 C11 112.2(3) . . ? C13 C12 F2 119.3(3) . . ? C13 C12 C11 128.5(3) . . ? C55 C57 H57 117.4 . . ? C56 C57 C55 125.3(4) . . ? C56 C57 H57 117.4 . . ? C34 C33 C36 119.2(4) . . ? C34 C33 C32 119.9(3) . . ? C32 C33 C36 120.9(4) . . ? C27 C28 H28 119.2 . . ? C27 C28 C26 121.6(3) . . ? C26 C28 H28 119.2 . . ? C50 C49 H49 120.2 . . ? C48 C49 C50 119.6(3) . . ? C48 C49 H49 120.2 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C23 C27 H27 120.3 . . ? C28 C27 C23 119.4(3) . . ? C28 C27 H27 120.3 . . ? C25 C26 C29 117.5(3) . . ? C28 C26 C25 120.1(3) . . ? C28 C26 C29 122.4(4) . . ? C6 C18 H18 119.2 . . ? C17 C18 C6 121.7(3) . . ? C17 C18 H18 119.2 . . ? C20 C16 S2 119.6(3) . . ? C20 C16 C17 119.3(3) . . ? C17 C16 S2 120.8(3) . . ? C7 C19 H19 120.3 . . ? C22 C19 C7 119.5(3) . . ? C22 C19 H19 120.3 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? N2 C10 H10A 108.6 . . ? N2 C10 H10B 108.6 . . ? N2 C10 C9 114.6(3) . . ? H10A C10 H10B 107.6 . . ? C9 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? F11 C43 C42 109.6(3) . . ? F11 C43 C44 106.7(3) . . ? F10 C43 F11 105.8(3) . . ? F10 C43 C42 112.2(3) . . ? F10 C43 C44 106.8(3) . . ? C42 C43 C44 115.0(3) . . ? C52 C56 H56 120.6 . . ? C57 C56 C52 118.8(3) . . ? C57 C56 H56 120.6 . . ? C8 C9 H9A 109.7 . . ? C8 C9 H9B 109.6 . . ? C10 C9 C8 110.0(3) . . ? C10 C9 H9A 109.6 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F9 C42 C43 114.3(3) . . ? C41 C42 F9 118.2(3) . . ? C41 C42 C43 127.5(3) . . ? F14 C44 F12 109.3(4) . . ? F14 C44 F13 109.6(3) . . ? F14 C44 C43 111.1(4) . . ? F12 C44 F13 111.6(4) . . ? F12 C44 C43 107.9(3) . . ? F13 C44 C43 107.3(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S3 O6 1.460(3) . ? S3 O5 1.419(3) . ? S3 N3 1.651(3) . ? S3 C30 1.770(3) . ? S4 O7 1.421(3) . ? S4 O8 1.422(3) . ? S4 N4 1.682(3) . ? S4 C52 1.769(3) . ? S1 O2 1.444(3) . ? S1 O1 1.436(2) . ? S1 N1 1.652(3) . ? S1 C23 1.756(3) . ? S2 O3 1.449(3) . ? S2 O4 1.403(3) . ? S2 N2 1.671(3) . ? S2 C16 1.754(3) . ? F9 C42 1.350(4) . ? F2 C12 1.347(4) . ? F11 C43 1.351(4) . ? F3 C14 1.333(4) . ? F8 C41 1.364(4) . ? F6 C15 1.307(5) . ? F1 C13 1.318(4) . ? F14 C44 1.284(6) . ? F10 C43 1.335(5) . ? N2 C11 1.397(4) . ? N2 C10 1.478(5) . ? N4 C39 1.514(4) . ? N4 C45 1.423(5) . ? F7 C15 1.366(6) . ? N1 C1 1.408(5) . ? N1 C8 1.469(4) . ? C13 C14 1.546(6) . ? C13 C12 1.290(5) . ? C24 H24 0.9300 . ? C24 C23 1.360(5) . ? C24 C25 1.451(4) . ? N3 C40 1.450(4) . ? N3 C37 1.474(5) . ? C30 C35 1.381(5) . ? C30 C31 1.378(5) . ? C40 C41 1.458(6) . ? C40 C45 1.340(4) . ? C1 C2 1.491(4) . ? C1 C11 1.375(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.538(5) . ? F12 C44 1.303(5) . ? F5 C15 1.319(6) . ? C50 H50 0.9300 . ? C50 C51 1.348(5) . ? C50 C49 1.415(5) . ? C35 H35 0.9300 . ? C35 C34 1.435(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 C39 1.493(5) . ? C46 C47 1.416(5) . ? C46 C45 1.487(4) . ? C46 C51 1.409(4) . ? C14 F4 1.350(4) . ? C14 C15 1.497(5) . ? C53 H53 0.9300 . ? C53 C54 1.394(5) . ? C53 C52 1.387(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C3 H3 0.9300 . ? C3 C2 1.359(5) . ? C3 C4 1.405(4) . ? C7 H7 0.9300 . ? C7 C2 1.383(4) . ? C7 C19 1.426(5) . ? C34 H34 0.9300 . ? C34 C33 1.363(6) . ? C54 H54 0.9300 . ? C54 C55 1.421(5) . ? C52 C56 1.408(5) . ? C23 C27 1.384(5) . ? C20 H20 0.9300 . ? C20 C21 1.379(5) . ? C20 C16 1.395(5) . ? C6 C21 1.406(5) . ? C6 C18 1.412(5) . ? C6 C5 1.504(5) . ? C41 C42 1.333(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C36 C33 1.506(5) . ? C55 C57 1.352(5) . ? C55 C58 1.483(5) . ? C22 H22 0.9300 . ? C22 C4 1.423(5) . ? C22 C19 1.348(5) . ? C48 H48 0.9300 . ? C48 C47 1.372(5) . ? C48 C49 1.345(5) . ? C31 H31 0.9300 . ? C31 C32 1.406(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.540(4) . ? C25 H25 0.9300 . ? C25 C26 1.414(5) . ? C47 H47 0.9300 . ? C51 H51 0.9300 . ? C11 C12 1.496(5) . ? C21 H21 0.9300 . ? F13 C44 1.335(5) . ? C32 H32 0.9300 . ? C32 C33 1.372(6) . ? C4 H4 0.9300 . ? C57 H57 0.9300 . ? C57 C56 1.323(5) . ? C28 H28 0.9300 . ? C28 C27 1.372(5) . ? C28 C26 1.380(5) . ? C49 H49 0.9300 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C27 H27 0.9300 . ? C26 C29 1.523(5) . ? C18 H18 0.9300 . ? C18 C17 1.343(4) . ? C16 C17 1.396(5) . ? C19 H19 0.9300 . ? C17 H17 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C9 1.514(5) . ? C43 C42 1.471(6) . ? C43 C44 1.567(5) . ? C56 H56 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 N3 C40 C41 -62.5(3) . . . . ? S3 N3 C40 C45 126.2(3) . . . . ? S3 N3 C37 C38 -75.5(3) . . . . ? S3 C30 C35 C34 -176.2(3) . . . . ? S3 C30 C31 C32 175.5(3) . . . . ? S4 N4 C39 C38 -70.1(3) . . . . ? S4 N4 C45 C40 125.6(3) . . . . ? S4 N4 C45 C46 -59.9(3) . . . . ? S4 C52 C56 C57 -178.8(3) . . . . ? S1 N1 C1 C2 -55.5(3) . . . . ? S1 N1 C1 C11 125.8(3) . . . . ? S1 N1 C8 C9 -73.4(3) . . . . ? S1 C23 C27 C28 179.1(3) . . . . ? S2 N2 C11 C1 124.0(3) . . . . ? S2 N2 C11 C12 -64.6(3) . . . . ? S2 N2 C10 C9 -70.0(3) . . . . ? S2 C16 C17 C18 -176.6(3) . . . . ? F11 C43 C42 F9 30.6(4) . . . . ? F11 C43 C42 C41 -149.9(3) . . . . ? F11 C43 C44 F14 52.5(5) . . . . ? F11 C43 C44 F12 -67.3(5) . . . . ? F11 C43 C44 F13 172.3(3) . . . . ? F3 C14 C15 F6 59.3(5) . . . . ? F3 C14 C15 F7 -60.7(4) . . . . ? F3 C14 C15 F5 178.3(4) . . . . ? O7 S4 N4 C39 118.2(2) . . . . ? O7 S4 N4 C45 -34.6(3) . . . . ? O7 S4 C52 C53 -176.2(3) . . . . ? O7 S4 C52 C56 1.7(4) . . . . ? O3 S2 N2 C11 -100.7(3) . . . . ? O3 S2 N2 C10 51.3(3) . . . . ? O3 S2 C16 C20 15.3(3) . . . . ? O3 S2 C16 C17 -171.1(3) . . . . ? F8 C41 C42 F9 176.4(3) . . . . ? F8 C41 C42 C43 -3.1(5) . . . . ? O2 S1 N1 C1 -165.7(2) . . . . ? O2 S1 N1 C8 -8.8(3) . . . . ? O2 S1 C23 C24 131.4(3) . . . . ? O2 S1 C23 C27 -48.1(3) . . . . ? O6 S3 N3 C40 27.0(3) . . . . ? O6 S3 N3 C37 -176.5(2) . . . . ? O6 S3 C30 C35 59.8(3) . . . . ? O6 S3 C30 C31 -118.8(3) . . . . ? O4 S2 N2 C11 29.1(3) . . . . ? O4 S2 N2 C10 -178.8(2) . . . . ? O4 S2 C16 C20 -114.0(3) . . . . ? O4 S2 C16 C17 59.5(3) . . . . ? F1 C13 C14 F3 149.3(3) . . . . ? F1 C13 C14 F4 30.3(4) . . . . ? F1 C13 C14 C15 -87.5(4) . . . . ? F1 C13 C12 F2 173.7(3) . . . . ? F1 C13 C12 C11 -4.4(5) . . . . ? O5 S3 N3 C40 -102.9(3) . . . . ? O5 S3 N3 C37 53.5(2) . . . . ? O5 S3 C30 C35 -169.2(3) . . . . ? O5 S3 C30 C31 12.2(3) . . . . ? O1 S1 N1 C1 -37.2(3) . . . . ? O1 S1 N1 C8 119.7(2) . . . . ? O1 S1 C23 C24 1.3(3) . . . . ? O1 S1 C23 C27 -178.2(3) . . . . ? F10 C43 C42 F9 147.9(3) . . . . ? F10 C43 C42 C41 -32.6(5) . . . . ? F10 C43 C44 F14 -60.4(5) . . . . ? F10 C43 C44 F12 179.8(4) . . . . ? F10 C43 C44 F13 59.4(4) . . . . ? N2 S2 C16 C20 132.7(3) . . . . ? N2 S2 C16 C17 -53.7(3) . . . . ? N2 C11 C12 F2 -47.9(4) . . . . ? N2 C11 C12 C13 130.3(3) . . . . ? N2 C10 C9 C8 -43.6(4) . . . . ? O8 S4 N4 C39 -12.2(2) . . . . ? O8 S4 N4 C45 -164.9(2) . . . . ? O8 S4 C52 C53 -46.0(3) . . . . ? O8 S4 C52 C56 131.9(3) . . . . ? N4 S4 C52 C53 66.3(3) . . . . ? N4 S4 C52 C56 -115.8(3) . . . . ? N1 S1 C23 C24 -115.5(3) . . . . ? N1 S1 C23 C27 65.0(3) . . . . ? N1 C1 C2 C3 122.5(3) . . . . ? N1 C1 C2 C7 -58.5(4) . . . . ? N1 C1 C11 N2 -9.8(5) . . . . ? N1 C1 C11 C12 179.3(3) . . . . ? N1 C8 C9 C10 -40.8(4) . . . . ? C13 C14 C15 F6 -66.7(5) . . . . ? C13 C14 C15 F7 173.3(3) . . . . ? C13 C14 C15 F5 52.3(5) . . . . ? C24 C23 C27 C28 -0.3(6) . . . . ? C24 C25 C26 C28 0.3(5) . . . . ? C24 C25 C26 C29 -177.5(3) . . . . ? N3 S3 C30 C35 -52.9(3) . . . . ? N3 S3 C30 C31 128.5(3) . . . . ? N3 C40 C41 F8 -50.3(4) . . . . ? N3 C40 C41 C42 131.3(4) . . . . ? N3 C40 C45 N4 -11.9(5) . . . . ? N3 C40 C45 C46 174.0(3) . . . . ? N3 C37 C38 C39 -37.2(4) . . . . ? C30 S3 N3 C40 142.2(3) . . . . ? C30 S3 N3 C37 -61.3(3) . . . . ? C30 C35 C34 C33 -1.1(6) . . . . ? C30 C31 C32 C33 2.5(6) . . . . ? C40 N3 C37 C38 80.7(3) . . . . ? C40 C41 C42 F9 -5.2(5) . . . . ? C40 C41 C42 C43 175.3(3) . . . . ? C1 N1 C8 C9 83.0(4) . . . . ? C1 C11 C12 F2 124.0(3) . . . . ? C1 C11 C12 C13 -57.8(5) . . . . ? C37 N3 C40 C41 141.9(3) . . . . ? C37 N3 C40 C45 -29.4(4) . . . . ? C37 C38 C39 N4 -44.5(4) . . . . ? C35 C30 C31 C32 -3.1(5) . . . . ? C35 C34 C33 C36 179.0(3) . . . . ? C35 C34 C33 C32 0.7(6) . . . . ? C14 C13 C12 F2 -3.4(5) . . . . ? C14 C13 C12 C11 178.5(3) . . . . ? C53 C54 C55 C57 -1.8(6) . . . . ? C53 C54 C55 C58 177.9(4) . . . . ? C53 C52 C56 C57 -0.9(6) . . . . ? C39 N4 C45 C40 -26.1(4) . . . . ? C39 N4 C45 C46 148.4(3) . . . . ? F4 C14 C15 F6 174.3(4) . . . . ? F4 C14 C15 F7 54.3(4) . . . . ? F4 C14 C15 F5 -66.7(5) . . . . ? C54 C53 C52 S4 179.3(3) . . . . ? C54 C53 C52 C56 1.4(5) . . . . ? C54 C55 C57 C56 2.4(6) . . . . ? C52 S4 N4 C39 -126.3(2) . . . . ? C52 S4 N4 C45 81.0(2) . . . . ? C52 C53 C54 C55 0.0(6) . . . . ? C23 S1 N1 C1 79.8(3) . . . . ? C23 S1 N1 C8 -123.2(2) . . . . ? C23 C24 C25 C26 -0.3(5) . . . . ? C20 C16 C17 C18 -3.0(5) . . . . ? C6 C18 C17 C16 2.4(6) . . . . ? C41 C40 C45 N4 177.5(3) . . . . ? C41 C40 C45 C46 3.5(5) . . . . ? C2 C1 C11 N2 171.6(3) . . . . ? C2 C1 C11 C12 0.7(5) . . . . ? C2 C3 C4 C22 0.6(5) . . . . ? C2 C7 C19 C22 0.4(5) . . . . ? C55 C57 C56 C52 -1.1(6) . . . . ? C31 C30 C35 C34 2.3(5) . . . . ? C31 C32 C33 C34 -1.4(6) . . . . ? C31 C32 C33 C36 -179.7(4) . . . . ? C8 N1 C1 C2 148.0(3) . . . . ? C8 N1 C1 C11 -30.7(4) . . . . ? C25 C24 C23 S1 -179.2(3) . . . . ? C25 C24 C23 C27 0.3(5) . . . . ? C47 C46 C45 N4 121.8(3) . . . . ? C47 C46 C45 C40 -63.6(4) . . . . ? C47 C46 C51 C50 3.0(5) . . . . ? C47 C48 C49 C50 1.9(6) . . . . ? C45 N4 C39 C38 81.9(4) . . . . ? C45 C40 C41 F8 121.1(3) . . . . ? C45 C40 C41 C42 -57.3(5) . . . . ? C45 C46 C47 C48 -178.3(3) . . . . ? C45 C46 C51 C50 178.4(3) . . . . ? C51 C50 C49 C48 -2.0(5) . . . . ? C51 C46 C47 C48 -3.1(5) . . . . ? C51 C46 C45 N4 -53.5(4) . . . . ? C51 C46 C45 C40 121.2(4) . . . . ? C11 N2 C10 C9 82.6(3) . . . . ? C11 C1 C2 C3 -58.8(5) . . . . ? C11 C1 C2 C7 120.3(3) . . . . ? C21 C20 C16 S2 177.8(3) . . . . ? C21 C20 C16 C17 4.1(6) . . . . ? C21 C6 C18 C17 -2.8(5) . . . . ? C4 C3 C2 C1 -179.2(3) . . . . ? C4 C3 C2 C7 1.8(5) . . . . ? C4 C22 C19 C7 2.0(6) . . . . ? C12 C13 C14 F3 -33.4(4) . . . . ? C12 C13 C14 F4 -152.4(3) . . . . ? C12 C13 C14 C15 89.8(4) . . . . ? C49 C50 C51 C46 -0.5(5) . . . . ? C49 C48 C47 C46 0.6(6) . . . . ? C58 C55 C57 C56 -177.3(4) . . . . ? C27 C28 C26 C25 -0.3(6) . . . . ? C27 C28 C26 C29 177.3(4) . . . . ? C26 C28 C27 C23 0.3(6) . . . . ? C18 C6 C21 C20 3.9(5) . . . . ? C16 S2 N2 C11 145.5(3) . . . . ? C16 S2 N2 C10 -62.5(3) . . . . ? C16 C20 C21 C6 -4.6(6) . . . . ? C19 C7 C2 C1 178.6(3) . . . . ? C19 C7 C2 C3 -2.3(5) . . . . ? C19 C22 C4 C3 -2.5(6) . . . . ? C10 N2 C11 C1 -27.9(5) . . . . ? C10 N2 C11 C12 143.5(3) . . . . ? C5 C6 C21 C20 -177.2(4) . . . . ? C5 C6 C18 C17 178.3(4) . . . . ? C42 C43 C44 F14 174.3(3) . . . . ? C42 C43 C44 F12 54.5(5) . . . . ? C42 C43 C44 F13 -65.9(5) . . . . ? C44 C43 C42 F9 -89.7(4) . . . . ? C44 C43 C42 C41 89.8(5) . . . . ?