#------------------------------------------------------------------------------ #$Date: 2024-12-06 18:41:39 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296393 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572739.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_1572739 loop_ _publ_author_name 'Valdés, Hugo' 'Alpuente, Nora' 'Salvador, Pedro' 'Hashmi, A Stephen K' 'Ribas, Xavi' _publ_section_title ; CCC-NHC Au(iii) pincer complexes as a reliable platform for isolating elusive species. ; _journal_issue 42 _journal_name_full 'Chemical science' _journal_page_first 17618 _journal_page_last 17628 _journal_paper_doi 10.1039/d4sc02999b _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C36 H34 Au N4, B F4, C H2 Cl2' _chemical_formula_sum 'C37 H36 Au B Cl2 F4 N4' _chemical_formula_weight 891.37 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_update_record ; 2024-02-20 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 77.893(3) _cell_angle_beta 80.575(3) _cell_angle_gamma 80.828(3) _cell_formula_units_Z 2 _cell_length_a 9.5527(12) _cell_length_b 13.7464(17) _cell_length_c 14.2095(15) _cell_measurement_reflns_used 5770 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 26.2460 _cell_measurement_theta_min 3.0571 _cell_volume 1784.6(4) _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_collection 'Bruker Instrument Service vV6.2.16' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1365)' _computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)' _computing_structure_solution 'XT, VERSION 2018/2' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'D8 QUEST ECO' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'doubly curved silicon crystal Bruker Triumph' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1530 _diffrn_reflns_av_unetI/netI 0.0879 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 54188 _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 26.48 _diffrn_reflns_theta_min 3.06 _diffrn_source_current 20.0 _diffrn_source_power 1.00 _diffrn_source_type 'Ceramic x-ray tube' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 4.325 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.721 _refine_diff_density_min -3.241 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 491 _refine_ls_number_reflns 7338 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0631 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+18.9888P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1186 _refine_ls_wR_factor_ref 0.1277 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5967 _reflns_number_total 7338 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02999b3.cif _cod_data_source_block HV2_129 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1572736--1572746.cif. ; _cod_database_code 1572739 _shelx_res_file ; TITL HV2_129_0m_a.res in P-1 HV2_129_0m_a.res created by SHELXL-2019/1 at 15:49:14 on 16-Jan-2024 REM Old TITL HV2_129_0m in P-1 REM SHELXT solution in P-1: R1 0.127, Rweak 0.049, Alpha 0.039 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C40 Au N9 CELL 0.71073 9.5527 13.7464 14.2095 77.893 80.575 80.828 ZERR 2.000 0.0012 0.0017 0.0015 0.003 0.003 0.003 LATT 1 SFAC C H AU N B F Cl UNIT 74 72 2 8 2 8 4 OMIT 0 -1 1 OMIT 1 1 0 OMIT 1 0 1 OMIT 1 0 0 OMIT 1 1 1 OMIT -1 1 0 TEMP -173.150 SIZE 0.05 0.13 0.30 L.S. 10 BOND $h conf acta LIST 6 FMAP 2 PLAN 40 isor 0.01 $f $b c3m eadp f2r f3r eadp f2' f3' eadp c3" c3m WGHT 0.035900 18.988798 FVAR 0.35140 0.69367 0.62707 AU1 3 0.351841 0.239067 0.671442 11.00000 0.01811 0.02255 = 0.02086 -0.00006 -0.00791 -0.00390 N3 4 0.399009 0.025707 0.798365 11.00000 0.02252 0.02471 = 0.02905 -0.00454 -0.00951 0.00015 N10 4 0.546544 0.128139 0.809579 11.00000 0.02620 0.02540 = 0.03440 -0.00441 -0.01489 -0.00436 N19 4 0.188911 0.438848 0.623834 11.00000 0.01903 0.01941 = 0.02826 -0.00522 -0.00869 0.00036 N21 4 0.304236 0.402609 0.487566 11.00000 0.02702 0.01771 = 0.01627 -0.00581 -0.00521 -0.00697 C2 1 0.432362 0.119908 0.768365 11.00000 0.03264 0.02765 = 0.02481 -0.00337 -0.01534 -0.00282 C4 1 0.499058 -0.028494 0.858589 11.00000 0.02417 0.03011 = 0.02785 -0.00218 -0.00148 0.00650 C5 1 0.514039 -0.127427 0.909023 11.00000 0.02854 0.03384 = 0.03200 -0.00156 -0.00025 -0.00496 AFIX 43 H5 2 0.447217 -0.171697 0.908893 11.00000 -1.20000 AFIX 0 C6 1 0.631151 -0.158169 0.959412 11.00000 0.04096 0.04480 = 0.03014 0.00355 -0.00058 0.01205 AFIX 43 H6 2 0.646454 -0.225672 0.992825 11.00000 -1.20000 AFIX 0 C7 1 0.726390 -0.092771 0.962186 11.00000 0.02628 0.04898 = 0.02713 -0.00889 -0.00754 0.00483 AFIX 43 H7 2 0.805336 -0.116669 0.997388 11.00000 -1.20000 AFIX 0 C8 1 0.709652 0.004720 0.915790 11.00000 0.03093 0.03766 = 0.02119 -0.00436 -0.00573 0.00603 AFIX 43 H8 2 0.773917 0.049794 0.918659 11.00000 -1.20000 AFIX 0 C9 1 0.594063 0.034936 0.864123 11.00000 0.02574 0.02328 = 0.02862 0.00185 -0.00267 0.00252 C11 1 0.610124 0.220176 0.799712 11.00000 0.01664 0.03671 = 0.03045 -0.00065 -0.00731 -0.01053 AFIX 23 H11A 2 0.664988 0.235078 0.734093 11.00000 -1.20000 H11B 2 0.677755 0.210028 0.847822 11.00000 -1.20000 AFIX 0 C12 1 0.497303 0.309337 0.815026 11.00000 0.03250 0.02896 = 0.02032 -0.00193 -0.00164 -0.00362 C13 1 0.513377 0.370208 0.877188 11.00000 0.01827 0.03835 = 0.03055 -0.00726 -0.00611 -0.00924 AFIX 43 H13 2 0.597453 0.358556 0.907694 11.00000 -1.20000 AFIX 0 C14 1 0.408169 0.448121 0.895552 11.00000 0.03041 0.05048 = 0.02674 -0.01617 -0.00183 -0.01575 AFIX 43 H14 2 0.417467 0.488654 0.940161 11.00000 -1.20000 AFIX 0 C15 1 0.289107 0.465755 0.847558 11.00000 0.03346 0.03892 = 0.02246 -0.00922 -0.00535 0.00382 AFIX 43 H15 2 0.216621 0.519288 0.859707 11.00000 -1.20000 AFIX 0 C16 1 0.272340 0.407898 0.782474 11.00000 0.01711 0.02946 = 0.02111 0.00183 -0.00143 -0.00615 C17 1 0.376574 0.328145 0.766277 11.00000 0.02293 0.03667 = 0.01450 0.00080 0.00103 -0.01218 C18 1 0.143792 0.432052 0.728402 11.00000 0.02481 0.03238 = 0.02680 -0.00507 -0.00558 0.00372 AFIX 23 H18A 2 0.080494 0.379090 0.752199 11.00000 -1.20000 H18B 2 0.088943 0.496588 0.740846 11.00000 -1.20000 AFIX 0 C20 1 0.280401 0.370144 0.584315 11.00000 0.01629 0.02336 = 0.02522 0.00158 -0.00547 -0.01084 C22 1 0.226957 0.496098 0.463705 11.00000 0.02081 0.02127 = 0.03142 -0.00458 -0.00953 -0.00614 C23 1 0.211953 0.563029 0.375667 11.00000 0.02041 0.02353 = 0.02712 -0.00054 -0.00703 -0.00584 AFIX 43 H23 2 0.263337 0.549043 0.315835 11.00000 -1.20000 AFIX 0 C24 1 0.118951 0.650165 0.380165 11.00000 0.02265 0.02278 = 0.03732 0.00292 -0.01380 -0.00816 AFIX 43 H24 2 0.105608 0.696684 0.321635 11.00000 -1.20000 AFIX 0 C25 1 0.043629 0.672598 0.467553 11.00000 0.02771 0.02358 = 0.04069 -0.00441 -0.01273 0.00188 AFIX 43 H25 2 -0.019341 0.733599 0.466716 11.00000 -1.20000 AFIX 0 C26 1 0.058550 0.608031 0.555398 11.00000 0.02153 0.01926 = 0.03534 -0.00474 -0.01228 0.00100 AFIX 43 H26 2 0.008632 0.623151 0.615202 11.00000 -1.20000 AFIX 0 C27 1 0.151296 0.519568 0.550572 11.00000 0.01891 0.02660 = 0.02972 -0.00615 -0.00802 -0.00651 C28 1 0.277998 -0.014182 0.771312 11.00000 0.03200 0.02610 = 0.03766 0.00079 -0.00951 -0.00816 AFIX 13 H28 2 0.232066 0.040829 0.723636 11.00000 -1.20000 AFIX 0 C29 1 0.165906 -0.036645 0.856899 11.00000 0.03151 0.03286 = 0.04934 -0.00007 -0.01517 -0.00616 AFIX 137 H29A 2 0.085454 -0.059069 0.836153 11.00000 -1.50000 H29B 2 0.132126 0.024054 0.884243 11.00000 -1.50000 H29C 2 0.206779 -0.089620 0.906311 11.00000 -1.50000 AFIX 0 C30 1 0.336895 -0.099867 0.717767 11.00000 0.04903 0.03484 = 0.04968 -0.01103 -0.02049 -0.00349 AFIX 137 H30A 2 0.261778 -0.114864 0.685602 11.00000 -1.50000 H30B 2 0.369143 -0.159488 0.764149 11.00000 -1.50000 H30C 2 0.417761 -0.080530 0.669005 11.00000 -1.50000 AFIX 0 C31 1 0.412316 0.350095 0.420324 11.00000 0.01932 0.03273 = 0.02832 -0.00829 -0.00176 -0.00187 AFIX 13 H31 2 0.449654 0.284179 0.458783 11.00000 -1.20000 AFIX 0 C32 1 0.537919 0.409704 0.384086 11.00000 0.02481 0.04509 = 0.04532 -0.00917 -0.00243 -0.00768 AFIX 137 H32A 2 0.607458 0.375443 0.339031 11.00000 -1.50000 H32B 2 0.583681 0.415094 0.439349 11.00000 -1.50000 H32C 2 0.503600 0.477007 0.350512 11.00000 -1.50000 AFIX 0 C33 1 0.345816 0.328136 0.338515 11.00000 0.03179 0.03920 = 0.02782 -0.01061 -0.00626 0.00266 AFIX 137 H33A 2 0.417831 0.289126 0.298868 11.00000 -1.50000 H33B 2 0.310828 0.391424 0.297988 11.00000 -1.50000 H33C 2 0.265780 0.289656 0.365782 11.00000 -1.50000 AFIX 0 C34 1 0.316756 0.153702 0.575832 11.00000 0.02129 0.02506 = 0.02968 0.00021 -0.00811 -0.00173 C35 1 0.282344 0.108900 0.522898 11.00000 0.01706 0.03217 = 0.03377 -0.00781 -0.00704 -0.00140 C36 1 0.236672 0.049041 0.463431 11.00000 0.01850 0.03264 = 0.03244 -0.01679 -0.00308 0.00193 C37 1 0.124443 0.087911 0.409042 11.00000 0.04022 0.03329 = 0.04711 -0.01221 -0.02171 0.00596 AFIX 43 H37 2 0.079857 0.154970 0.407983 11.00000 -1.20000 AFIX 0 C38 1 0.078672 0.026878 0.356250 11.00000 0.03995 0.03485 = 0.05234 -0.01805 -0.02006 0.00614 AFIX 43 H38 2 0.001404 0.053105 0.319962 11.00000 -1.20000 AFIX 0 C39 1 0.140745 -0.068224 0.355144 11.00000 0.04499 0.03541 = 0.04095 -0.01225 -0.01358 -0.00963 AFIX 43 H39 2 0.106871 -0.108422 0.319093 11.00000 -1.20000 AFIX 0 C40 1 0.256693 -0.107471 0.408160 11.00000 0.04634 0.03043 = 0.04724 -0.01704 -0.01444 -0.00322 AFIX 43 H40 2 0.302515 -0.173979 0.407416 11.00000 -1.20000 AFIX 0 C41 1 0.302180 -0.048364 0.460655 11.00000 0.03247 0.02701 = 0.03576 -0.01097 -0.01394 0.01043 AFIX 43 H41 2 0.380426 -0.074605 0.496029 11.00000 -1.20000 AFIX 0 part 1 21 B1R 5 0.903174 0.272735 0.909448 21.00000 0.02590 0.04087 = 0.04285 0.00416 -0.00556 -0.00929 F2R 6 0.857315 0.357253 0.850388 21.00000 0.02265 0.07158 = 0.04859 0.00336 -0.01395 -0.01282 F3R 6 1.034118 0.283850 0.938718 21.00000 0.02265 0.07158 = 0.04859 0.00336 -0.01395 -0.01282 F4R 6 0.809817 0.247320 0.983391 21.00000 0.04890 0.12711 = 0.08338 0.07123 -0.02825 -0.03145 F5R 6 0.940778 0.198910 0.849857 21.00000 0.08225 0.07090 = 0.11371 -0.01910 -0.04486 0.00967 part 2 -21 B1' 5 0.966799 0.241070 0.887429 -21.00000 0.04482 0.04003 = 0.04274 -0.01157 -0.01128 -0.00860 F2' 6 0.864686 0.320016 0.842140 -21.00000 0.04392 0.05972 = 0.03803 -0.00771 -0.00700 -0.00935 F3' 6 1.079531 0.267065 0.912527 -21.00000 0.04392 0.05972 = 0.03803 -0.00771 -0.00700 -0.00935 F4' 6 0.911815 0.162294 0.935280 -21.00000 0.06306 0.06795 = 0.05415 0.01999 -0.00356 -0.03108 F5' 6 1.038331 0.201397 0.792126 -21.00000 0.05633 0.06145 = 0.05645 -0.00993 -0.01204 0.02127 part 0 AFIX 9 part 1 31 CL1" 7 0.874289 0.588322 0.872505 31.00000 0.03959 0.08256 = 0.05963 -0.02632 0.00666 -0.01144 C3" 1 0.931720 0.708008 0.853157 31.00000 0.11364 0.10128 = 0.11305 -0.03122 -0.00428 -0.01047 AFIX 23 H3"A 2 0.853595 0.760169 0.831219 31.00000 -1.20000 H3"B 2 0.953401 0.720168 0.915177 31.00000 -1.20000 AFIX 5 CL2" 7 1.083768 0.717567 0.766351 31.00000 0.05996 0.02989 = 0.07779 -0.01373 -0.01909 0.00261 part 2 -31 CL1M 7 0.851184 0.531169 0.884605 -31.00000 0.07252 0.13536 = 0.08131 -0.07054 0.01168 -0.00598 C3M 1 0.880237 0.648222 0.884205 -31.00000 0.11364 0.10128 = 0.11305 -0.03122 -0.00428 -0.01047 AFIX 23 H3MA 2 0.784780 0.688746 0.888999 -31.00000 -1.20000 H3MB 2 0.917750 0.645529 0.945777 -31.00000 -1.20000 AFIX 5 CL2M 7 0.981315 0.713544 0.800175 -31.00000 0.18415 0.05896 = 0.12404 -0.01781 -0.07128 0.02214 AFIX 0 HKLF 4 REM HV2_129_0m_a.res in P-1 REM wR2 = 0.1277, GooF = S = 1.066, Restrained GooF = 1.065 for all data REM R1 = 0.0631 for 5967 Fo > 4sig(Fo) and 0.0878 for all 7338 data REM 491 parameters refined using 66 restraints END WGHT 0.0359 18.9889 REM Highest difference peak 1.721, deepest hole -3.241, 1-sigma level 0.204 Q1 1 0.3246 0.2775 0.7264 11.00000 0.05 1.72 Q2 1 0.4136 0.2570 0.5989 11.00000 0.05 1.66 Q3 1 0.3020 0.2202 0.7446 11.00000 0.05 1.58 Q4 1 0.4324 0.2246 0.6185 11.00000 0.05 1.54 Q5 1 0.3831 0.2009 0.6146 11.00000 0.05 1.41 Q6 1 0.2358 0.5836 0.4878 11.00000 0.05 1.06 Q7 1 0.4364 -0.0971 0.8579 11.00000 0.05 0.99 Q8 1 0.3110 0.1957 0.7069 11.00000 0.05 0.95 Q9 1 0.3393 0.2973 0.5804 11.00000 0.05 0.88 Q10 1 1.0851 0.6985 0.9502 11.00000 0.05 0.84 Q11 1 0.2661 0.1762 0.6760 11.00000 0.05 0.81 Q12 1 0.8433 0.2172 0.9642 11.00000 0.05 0.78 Q13 1 0.1838 -0.0822 0.5364 11.00000 0.05 0.77 Q14 1 0.2418 -0.1807 0.6579 11.00000 0.05 0.75 Q15 1 0.3533 0.4400 0.7746 11.00000 0.05 0.74 Q16 1 0.9803 0.6626 0.9957 11.00000 0.05 0.74 Q17 1 0.4334 0.1416 0.6756 11.00000 0.05 0.73 Q18 1 0.8631 0.2883 1.0053 11.00000 0.05 0.71 Q19 1 0.8088 0.4287 0.9239 11.00000 0.05 0.70 Q20 1 0.8693 0.2926 0.9721 11.00000 0.05 0.69 Q21 1 0.9564 0.3393 0.9469 11.00000 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289.17 62.49 -1 7 0 409.66 70.99 -1 7 0 306.47 70.49 0 -7 0 62.49 57.79 0 -7 0 72.59 63.29 0 -7 0 28.60 52.19 0 -7 0 31.90 52.39 0 -7 0 -14.70 20.80 0 7 0 91.09 58.99 0 7 0 14.20 51.49 0 7 0 33.40 50.29 0 7 0 35.60 52.19 -1 -7 0 1477.85 102.69 -1 -7 0 1324.97 100.19 -1 -7 0 1722.13 110.99 -1 -7 0 1481.95 98.59 1 7 0 1586.14 99.09 1 7 0 1296.87 100.79 1 7 0 1491.55 96.99 1 7 0 1452.15 106.59 1 7 0 1521.95 112.59 -2 -7 0 169.98 55.19 -2 -7 0 208.08 57.19 -2 -7 0 159.38 55.99 -2 -7 0 338.27 72.29 2 7 0 264.27 65.59 2 7 0 167.28 57.89 2 7 0 137.39 49.30 2 7 0 203.58 68.99 2 7 0 155.08 55.59 2 7 0 128.09 50.89 -3 -7 0 80.09 50.29 -3 -7 0 103.99 59.39 -3 -7 0 127.49 48.70 -3 -7 0 173.18 61.39 3 7 0 64.79 47.70 3 7 0 170.58 61.79 3 7 0 51.89 51.39 3 7 0 103.39 62.49 3 7 0 170.88 57.69 3 7 0 16.50 58.09 -4 -7 0 1439.06 89.29 -4 -7 0 1462.95 108.69 -4 -7 0 1556.84 102.29 -4 -7 0 1507.85 93.09 4 7 0 1578.84 94.69 4 7 0 1589.44 99.79 4 7 0 1451.85 108.89 4 7 0 1433.16 98.89 4 7 0 1497.05 91.49 4 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10 16 166.28 121.59 0 1 -17 91.39 83.39 0 1 -17 95.59 105.19 -1 1 -17 109.09 75.99 -2 1 -17 100.29 91.19 3 -1 17 -15.80 47.70 3 -1 17 -28.80 46.90 0 0 -17 116.09 72.29 0 0 -17 221.48 85.49 -1 0 -17 108.89 78.79 -2 0 -17 111.39 81.09 2 0 17 196.88 33.70 2 0 17 131.49 38.00 -3 0 -17 286.87 46.20 -3 0 -17 265.67 58.49 3 0 17 242.58 49.00 3 0 17 181.88 60.19 4 0 17 114.29 64.39 1 -1 -17 -22.10 59.39 1 -1 -17 -26.10 100.79 0 -1 -17 145.19 93.09 0 -1 -17 143.19 72.29 -1 -1 -17 481.75 88.49 1 1 17 339.47 40.00 1 1 17 466.15 39.70 -2 -1 -17 143.69 77.19 -2 -1 -17 147.79 35.80 -2 -1 -17 110.09 45.30 2 1 17 120.69 48.40 2 1 17 208.28 42.30 -3 -1 -17 40.60 55.99 -3 -1 -17 102.29 42.80 3 1 17 132.59 46.90 3 1 17 -3.20 52.39 -4 -1 -17 314.57 73.79 4 1 17 295.17 74.09 4 1 17 448.16 105.49 1 -2 -17 469.25 119.49 -1 2 17 174.28 25.90 -1 2 17 306.47 32.00 0 -2 -17 148.29 86.49 0 -2 -17 144.19 62.69 0 2 17 124.89 35.00 0 2 17 200.48 34.90 -1 -2 -17 22.80 30.40 -1 -2 -17 30.20 37.00 -1 -2 -17 93.79 67.69 1 2 17 49.50 43.20 1 2 17 23.00 34.90 -2 -2 -17 229.28 46.20 -2 -2 -17 243.58 64.09 2 2 17 284.37 52.19 2 2 17 224.48 59.19 -3 -2 -17 254.57 50.19 -3 -2 -17 326.37 71.99 3 2 17 317.27 89.19 3 2 17 244.78 59.49 3 2 17 280.47 69.59 -4 -2 -17 95.29 66.79 4 2 17 67.09 81.09 4 2 17 70.99 71.19 4 2 17 -71.29 67.39 -5 -2 -17 98.49 53.79 -5 -2 -17 164.08 72.29 5 2 17 22.90 82.49 5 2 17 150.68 86.49 5 2 17 124.69 76.69 1 -3 -17 69.39 32.20 1 -3 -17 72.19 36.60 1 -3 -17 291.97 106.99 -1 3 17 99.39 42.90 -1 3 17 59.99 40.50 0 -3 -17 98.39 85.29 0 -3 -17 93.49 45.40 0 -3 -17 179.58 43.20 0 3 17 141.49 46.00 0 3 17 165.58 49.60 -1 -3 -17 426.86 69.89 -1 -3 -17 245.18 56.99 -1 -3 -17 279.57 51.09 1 3 17 273.87 57.59 1 3 17 200.78 50.39 -2 -3 -17 133.49 56.59 -2 -3 -17 62.69 44.80 -2 -3 -17 50.59 57.69 2 3 17 134.59 52.99 2 3 17 116.19 75.19 2 3 17 12.10 56.69 -3 -3 -17 13.50 63.79 -3 -3 -17 -25.20 45.30 -3 -3 -17 -15.00 73.39 -3 -3 -17 7.70 66.39 3 3 17 48.30 53.89 3 3 17 218.98 84.09 3 3 17 -8.90 60.79 3 3 17 49.70 64.79 -4 -3 -17 249.58 63.49 -4 -3 -17 163.68 76.99 4 3 17 133.09 85.79 4 3 17 86.19 72.49 -5 -3 -17 110.29 61.99 -5 -3 -17 206.68 77.39 5 3 17 211.08 96.29 5 3 17 63.59 78.49 5 3 17 119.09 93.99 1 -4 -17 333.87 109.39 1 -4 -17 227.98 53.79 -1 4 17 234.68 57.39 0 -4 -17 152.58 49.00 0 -4 -17 77.09 53.99 0 -4 -17 154.98 88.49 0 4 17 86.59 55.69 0 4 17 85.29 51.89 -1 -4 -17 98.49 61.29 -1 -4 -17 55.39 42.70 1 4 17 35.40 49.20 1 4 17 48.60 57.89 -2 -4 -17 290.77 61.69 -2 -4 -17 249.18 74.09 -2 -4 -17 214.38 68.19 -2 -4 -17 215.48 49.60 2 4 17 219.58 64.59 2 4 17 260.87 87.79 2 4 17 341.57 73.19 2 4 17 150.68 54.89 -3 -4 -17 153.98 51.19 -3 -4 -17 35.60 54.29 -3 -4 -17 196.98 69.89 -3 -4 -17 170.08 74.09 3 4 17 122.09 77.19 3 4 17 190.18 76.79 3 4 17 276.77 93.69 3 4 17 166.78 73.29 -4 -4 -17 -47.90 56.49 -4 -4 -17 174.78 78.39 4 4 17 76.69 75.59 4 4 17 170.48 80.09 4 4 17 1.50 78.39 -5 -4 -17 30.60 67.69 -5 -4 -17 70.59 63.09 5 4 17 120.29 89.09 5 4 17 2.40 86.99 5 4 17 -34.90 88.49 1 -5 -17 101.99 99.09 1 -5 -17 -67.39 55.59 -1 5 17 11.00 62.99 0 -5 -17 463.35 100.59 0 5 17 225.18 89.99 0 5 17 213.38 70.49 -1 -5 -17 202.88 50.99 -1 -5 -17 261.37 82.69 -1 -5 -17 334.07 75.39 1 5 17 312.47 79.79 1 5 17 441.56 80.49 1 5 17 192.98 71.19 1 5 17 140.29 78.89 -2 -5 -17 113.49 63.09 -2 -5 -17 34.80 48.90 -2 -5 -17 126.59 72.09 2 5 17 198.68 80.39 2 5 17 164.08 74.09 2 5 17 65.29 68.39 2 5 17 45.50 79.19 -3 -5 -17 63.09 57.99 -3 -5 -17 -58.19 72.69 -3 -5 -17 55.79 40.40 -3 -5 -17 175.68 89.39 3 5 17 74.79 82.29 3 5 17 99.29 82.19 3 5 17 91.79 77.09 3 5 17 32.90 71.39 -4 -5 -17 369.86 70.19 4 5 17 120.09 83.19 4 5 17 338.97 100.99 4 5 17 284.57 97.49 -5 -5 -17 139.39 72.19 -5 -5 -17 -30.80 75.29 5 5 17 140.79 90.39 5 5 17 142.59 95.29 5 5 17 -2.20 83.29 0 -6 -17 154.88 58.49 0 -6 -17 93.59 70.79 0 -6 -17 303.47 89.99 0 6 17 95.49 64.69 0 6 17 152.58 76.29 -1 -6 -17 201.28 81.19 -1 -6 -17 75.79 59.69 1 6 17 13.50 62.19 1 6 17 125.49 74.59 1 6 17 -63.19 76.49 -2 -6 -17 289.97 84.89 -2 -6 -17 243.78 72.69 2 6 17 270.17 79.69 2 6 17 379.96 92.99 2 6 17 147.19 80.99 -3 -6 -17 292.27 84.19 -3 -6 -17 262.37 71.79 3 6 17 387.66 98.59 3 6 17 229.28 97.69 -4 -6 -17 50.79 74.89 -4 -6 -17 123.09 71.69 4 6 17 8.00 87.29 4 6 17 -24.20 65.59 4 6 17 53.49 83.99 -5 -6 -17 25.10 83.09 -5 -6 -17 224.28 72.29 5 6 17 134.79 98.49 5 6 17 103.69 83.39 5 6 17 8.30 78.39 0 -7 -17 167.68 66.49 0 -7 -17 185.38 80.09 0 7 17 202.98 93.89 0 7 17 35.00 80.19 -1 -7 -17 281.87 68.39 -1 -7 -17 154.18 77.49 1 7 17 217.88 80.79 1 7 17 255.37 93.89 1 7 17 202.38 83.09 -2 -7 -17 33.10 64.29 -2 -7 -17 23.00 67.59 2 7 17 111.59 78.99 2 7 17 -86.89 81.69 2 7 17 -37.80 75.39 -3 -7 -17 234.28 74.69 -3 -7 -17 96.29 76.09 3 7 17 30.20 77.89 3 7 17 138.69 72.69 3 7 17 198.08 94.29 -4 -7 -17 492.95 102.29 -4 -7 -17 202.48 81.79 4 7 17 240.48 93.19 4 7 17 172.18 97.29 4 7 17 211.28 101.29 -1 -8 -17 105.39 82.99 -1 -8 -17 -53.19 66.09 1 8 17 82.69 84.69 1 8 17 -20.50 92.09 1 8 17 99.89 78.79 -2 -8 -17 255.57 90.49 -2 -8 -17 287.77 74.89 2 8 17 225.78 100.59 2 8 17 99.89 78.59 2 8 17 152.98 88.19 -3 -8 -17 -159.38 80.29 -3 -8 -17 134.09 74.79 3 8 17 -46.40 76.49 3 8 17 142.29 84.29 3 8 17 -50.29 91.59 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 29170 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au Au1 0.35184(4) 0.23907(3) 0.67144(3) 0.02036(11) Uani d . . . 1.000000 . . N N3 0.3990(8) 0.0257(6) 0.7984(5) 0.0252(17) Uani d . . . 1.000000 . . N N10 0.5465(8) 0.1281(6) 0.8096(5) 0.0275(17) Uani d . . . 1.000000 . . N N19 0.1889(7) 0.4388(5) 0.6238(5) 0.0218(15) Uani d . . . 1.000000 . . N N21 0.3042(7) 0.4026(5) 0.4876(5) 0.0192(15) Uani d . . . 1.000000 . . C C2 0.4324(10) 0.1199(7) 0.7684(6) 0.027(2) Uani d . . . 1.000000 . . C C4 0.4991(10) -0.0285(7) 0.8586(7) 0.029(2) Uani d . . . 1.000000 . . C C5 0.5140(10) -0.1274(7) 0.9090(7) 0.032(2) Uani d . . . 1.000000 . . H H5 0.447217 -0.171697 0.908893 0.039000 Uiso calc U . R 1.000000 . . C C6 0.6312(12) -0.1582(9) 0.9594(7) 0.043(3) Uani d . . . 1.000000 . . H H6 0.646454 -0.225672 0.992825 0.051000 Uiso calc U . R 1.000000 . . C C7 0.7264(10) -0.0928(8) 0.9622(7) 0.035(2) Uani d . . . 1.000000 . . H H7 0.805336 -0.116669 0.997388 0.041000 Uiso calc U . R 1.000000 . . C C8 0.7097(10) 0.0047(8) 0.9158(6) 0.031(2) Uani d . . . 1.000000 . . H H8 0.773917 0.049794 0.918659 0.037000 Uiso calc U . R 1.000000 . . C C9 0.5941(10) 0.0349(7) 0.8641(6) 0.028(2) Uani d . . . 1.000000 . . C C11 0.6101(9) 0.2202(7) 0.7997(7) 0.028(2) Uani d . . . 1.000000 . . H H11A 0.664988 0.235078 0.734093 0.033000 Uiso calc U . R 1.000000 . . H H11B 0.677755 0.210028 0.847822 0.033000 Uiso calc U . R 1.000000 . . C C12 0.4973(10) 0.3093(7) 0.8150(6) 0.028(2) Uani d . . . 1.000000 . . C C13 0.5134(9) 0.3702(7) 0.8772(6) 0.028(2) Uani d . . . 1.000000 . . H H13 0.597453 0.358556 0.907694 0.034000 Uiso calc U . R 1.000000 . . C C14 0.4082(10) 0.4481(8) 0.8956(7) 0.034(2) Uani d . . . 1.000000 . . H H14 0.417467 0.488654 0.940161 0.040000 Uiso calc U . R 1.000000 . . C C15 0.2891(10) 0.4658(8) 0.8476(6) 0.032(2) Uani d . . . 1.000000 . . H H15 0.216621 0.519288 0.859707 0.038000 Uiso calc U . R 1.000000 . . C C16 0.2723(9) 0.4079(7) 0.7825(6) 0.0233(19) Uani d . . . 1.000000 . . C C17 0.3766(10) 0.3281(7) 0.7663(6) 0.025(2) Uani d . . . 1.000000 . . C C18 0.1438(10) 0.4321(7) 0.7284(6) 0.029(2) Uani d . . . 1.000000 . . H H18A 0.080494 0.379090 0.752199 0.034000 Uiso calc U . R 1.000000 . . H H18B 0.088943 0.496588 0.740846 0.034000 Uiso calc U . R 1.000000 . . C C20 0.2804(9) 0.3701(7) 0.5843(6) 0.0213(19) Uani d . . . 1.000000 . . C C22 0.2270(9) 0.4961(7) 0.4637(6) 0.0235(19) Uani d . . . 1.000000 . . C C23 0.2120(9) 0.5630(6) 0.3757(6) 0.0235(19) Uani d . . . 1.000000 . . H H23 0.263337 0.549043 0.315835 0.028000 Uiso calc U . R 1.000000 . . C C24 0.1190(9) 0.6502(7) 0.3802(7) 0.027(2) Uani d . . . 1.000000 . . H H24 0.105608 0.696684 0.321635 0.033000 Uiso calc U . R 1.000000 . . C C25 0.0436(10) 0.6726(7) 0.4676(7) 0.031(2) Uani d . . . 1.000000 . . H H25 -0.019341 0.733599 0.466716 0.037000 Uiso calc U . R 1.000000 . . C C26 0.0585(9) 0.6080(6) 0.5554(7) 0.0249(19) Uani d . . . 1.000000 . . H H26 0.008632 0.623151 0.615202 0.030000 Uiso calc U . R 1.000000 . . C C27 0.1513(9) 0.5196(7) 0.5506(6) 0.0240(19) Uani d . . . 1.000000 . . C C28 0.2780(10) -0.0142(7) 0.7713(7) 0.032(2) Uani d . . . 1.000000 . . H H28 0.232066 0.040829 0.723636 0.038000 Uiso calc U . R 1.000000 . . C C29 0.1659(11) -0.0366(8) 0.8569(8) 0.038(2) Uani d . . . 1.000000 . . H H29A 0.085454 -0.059069 0.836153 0.057000 Uiso calc U . R 1.000000 . . H H29B 0.132126 0.024054 0.884243 0.057000 Uiso calc U . R 1.000000 . . H H29C 0.206779 -0.089620 0.906311 0.057000 Uiso calc U . R 1.000000 . . C C30 0.3369(12) -0.0999(8) 0.7178(8) 0.043(3) Uani d . . . 1.000000 . . H H30A 0.261778 -0.114864 0.685602 0.064000 Uiso calc U . R 1.000000 . . H H30B 0.369143 -0.159488 0.764149 0.064000 Uiso calc U . R 1.000000 . . H H30C 0.417761 -0.080530 0.669005 0.064000 Uiso calc U . R 1.000000 . . C C31 0.4123(9) 0.3501(7) 0.4203(6) 0.027(2) Uani d . . . 1.000000 . . H H31 0.449654 0.284179 0.458783 0.032000 Uiso calc U . R 1.000000 . . C C32 0.5379(10) 0.4097(8) 0.3841(8) 0.038(2) Uani d . . . 1.000000 . . H H32A 0.607458 0.375443 0.339031 0.057000 Uiso calc U . R 1.000000 . . H H32B 0.583681 0.415094 0.439349 0.057000 Uiso calc U . R 1.000000 . . H H32C 0.503600 0.477007 0.350512 0.057000 Uiso calc U . R 1.000000 . . C C33 0.3458(10) 0.3281(8) 0.3385(7) 0.033(2) Uani d . . . 1.000000 . . H H33A 0.417831 0.289126 0.298868 0.049000 Uiso calc U . R 1.000000 . . H H33B 0.310828 0.391424 0.297988 0.049000 Uiso calc U . R 1.000000 . . H H33C 0.265780 0.289656 0.365782 0.049000 Uiso calc U . R 1.000000 . . C C34 0.3168(10) 0.1537(7) 0.5758(7) 0.026(2) Uani d . . . 1.000000 . . C C35 0.2823(9) 0.1089(7) 0.5229(7) 0.027(2) Uani d . . . 1.000000 . . C C36 0.2367(9) 0.0490(7) 0.4634(7) 0.027(2) Uani d . . . 1.000000 . . C C37 0.1244(11) 0.0879(8) 0.4090(8) 0.039(2) Uani d . . . 1.000000 . . H H37 0.079857 0.154970 0.407983 0.047000 Uiso calc U . R 1.000000 . . C C38 0.0787(11) 0.0269(8) 0.3563(8) 0.041(3) Uani d . . . 1.000000 . . H H38 0.001404 0.053105 0.319962 0.049000 Uiso calc U . R 1.000000 . . C C39 0.1407(11) -0.0682(8) 0.3551(7) 0.038(2) Uani d . . . 1.000000 . . H H39 0.106871 -0.108422 0.319093 0.046000 Uiso calc U . R 1.000000 . . C C40 0.2567(12) -0.1075(8) 0.4082(8) 0.039(2) Uani d . . . 1.000000 . . H H40 0.302515 -0.173979 0.407416 0.047000 Uiso calc U . R 1.000000 . . C C41 0.3022(10) -0.0484(7) 0.4607(7) 0.032(2) Uani d . . . 1.000000 . . H H41 0.380426 -0.074605 0.496029 0.038000 Uiso calc U . R 1.000000 . . B B1R 0.903(2) 0.2727(16) 0.9094(15) 0.038(4) Uani d U P . 0.694(17) A 1 F F2R 0.8573(14) 0.3573(10) 0.8504(10) 0.048(3) Uani d U P . 0.694(17) A 1 F F3R 1.0341(11) 0.2838(11) 0.9387(9) 0.048(3) Uani d U P . 0.694(17) A 1 F F4R 0.8098(12) 0.2473(11) 0.9834(9) 0.096(6) Uani d U P . 0.694(17) A 1 F F5R 0.9408(17) 0.1989(10) 0.8499(12) 0.087(5) Uani d U P . 0.694(17) A 1 B B1' 0.967(6) 0.241(4) 0.887(4) 0.041(11) Uani d U P . 0.306(17) A 2 F F2' 0.865(4) 0.320(2) 0.842(2) 0.047(6) Uani d U P . 0.306(17) A 2 F F3' 1.080(3) 0.267(2) 0.9125(19) 0.047(6) Uani d U P . 0.306(17) A 2 F F4' 0.912(3) 0.162(2) 0.9353(18) 0.064(9) Uani d U P . 0.306(17) A 2 F F5' 1.038(3) 0.2014(18) 0.7921(18) 0.061(8) Uani d U P . 0.306(17) A 2 Cl Cl1" 0.8743(5) 0.5883(6) 0.8725(3) 0.060(2) Uani d . P G 0.627(13) B 1 C C3" 0.9317(14) 0.7080(5) 0.8532(10) 0.109(12) Uani d . P G 0.627(13) B 1 H H3"A 0.853595 0.760169 0.831219 0.131000 Uiso calc U P R 0.627(13) B 1 H H3"B 0.953401 0.720168 0.915177 0.131000 Uiso calc U P R 0.627(13) B 1 Cl Cl2" 1.0838(7) 0.7176(3) 0.7664(5) 0.0552(19) Uani d . P G 0.627(13) B 1 Cl Cl1M 0.8512(7) 0.5312(8) 0.8846(5) 0.092(5) Uani d . P G 0.373(13) B 2 C C3M 0.8802(12) 0.6482(6) 0.8842(8) 0.109(12) Uani d U P G 0.373(13) B 2 H H3MA 0.784780 0.688746 0.888999 0.131000 Uiso calc U P R 0.373(13) B 2 H H3MB 0.917750 0.645529 0.945777 0.131000 Uiso calc U P R 0.373(13) B 2 Cl Cl2M 0.9813(7) 0.7135(3) 0.8002(6) 0.121(8) Uani d . P G 0.373(13) B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 0.01811(16) 0.02255(18) 0.02086(17) -0.00390(12) -0.00791(11) -0.00006(12) N3 0.023(4) 0.025(4) 0.029(4) 0.000(3) -0.010(3) -0.005(3) N10 0.026(4) 0.025(4) 0.034(4) -0.004(3) -0.015(3) -0.004(3) N19 0.019(4) 0.019(4) 0.028(4) 0.000(3) -0.009(3) -0.005(3) N21 0.027(4) 0.018(4) 0.016(3) -0.007(3) -0.005(3) -0.006(3) C2 0.033(5) 0.028(5) 0.025(5) -0.003(4) -0.015(4) -0.003(4) C4 0.024(5) 0.030(5) 0.028(5) 0.007(4) -0.001(4) -0.002(4) C5 0.029(5) 0.034(6) 0.032(5) -0.005(4) 0.000(4) -0.002(4) C6 0.041(6) 0.045(7) 0.030(6) 0.012(5) -0.001(5) 0.004(5) C7 0.026(5) 0.049(7) 0.027(5) 0.005(5) -0.008(4) -0.009(5) C8 0.031(5) 0.038(6) 0.021(5) 0.006(4) -0.006(4) -0.004(4) C9 0.026(5) 0.023(5) 0.029(5) 0.003(4) -0.003(4) 0.002(4) C11 0.017(4) 0.037(5) 0.030(5) -0.011(4) -0.007(4) -0.001(4) C12 0.032(5) 0.029(5) 0.020(5) -0.004(4) -0.002(4) -0.002(4) C13 0.018(5) 0.038(6) 0.031(5) -0.009(4) -0.006(4) -0.007(4) C14 0.030(5) 0.050(7) 0.027(5) -0.016(5) -0.002(4) -0.016(5) C15 0.033(5) 0.039(6) 0.022(5) 0.004(4) -0.005(4) -0.009(4) C16 0.017(4) 0.029(5) 0.021(4) -0.006(4) -0.001(3) 0.002(4) C17 0.023(5) 0.037(6) 0.014(4) -0.012(4) 0.001(4) 0.001(4) C18 0.025(5) 0.032(5) 0.027(5) 0.004(4) -0.006(4) -0.005(4) C20 0.016(4) 0.023(5) 0.025(5) -0.011(4) -0.005(3) 0.002(4) C22 0.021(4) 0.021(5) 0.031(5) -0.006(4) -0.010(4) -0.005(4) C23 0.020(4) 0.024(5) 0.027(5) -0.006(4) -0.007(4) -0.001(4) C24 0.023(5) 0.023(5) 0.037(5) -0.008(4) -0.014(4) 0.003(4) C25 0.028(5) 0.024(5) 0.041(6) 0.002(4) -0.013(4) -0.004(4) C26 0.022(5) 0.019(5) 0.035(5) 0.001(4) -0.012(4) -0.005(4) C27 0.019(4) 0.027(5) 0.030(5) -0.007(4) -0.008(4) -0.006(4) C28 0.032(5) 0.026(5) 0.038(5) -0.008(4) -0.010(4) 0.001(4) C29 0.032(5) 0.033(6) 0.049(6) -0.006(4) -0.015(5) 0.000(5) C30 0.049(7) 0.035(6) 0.050(7) -0.003(5) -0.020(5) -0.011(5) C31 0.019(4) 0.033(5) 0.028(5) -0.002(4) -0.002(4) -0.008(4) C32 0.025(5) 0.045(6) 0.045(6) -0.008(5) -0.002(4) -0.009(5) C33 0.032(5) 0.039(6) 0.028(5) 0.003(4) -0.006(4) -0.011(4) C34 0.021(5) 0.025(5) 0.030(5) -0.002(4) -0.008(4) 0.000(4) C35 0.017(4) 0.032(5) 0.034(5) -0.001(4) -0.007(4) -0.008(4) C36 0.019(5) 0.033(5) 0.032(5) 0.002(4) -0.003(4) -0.017(4) C37 0.040(6) 0.033(6) 0.047(6) 0.006(5) -0.022(5) -0.012(5) C38 0.040(6) 0.035(6) 0.052(7) 0.006(5) -0.020(5) -0.018(5) C39 0.045(6) 0.035(6) 0.041(6) -0.010(5) -0.014(5) -0.012(5) C40 0.046(6) 0.030(6) 0.047(6) -0.003(5) -0.014(5) -0.017(5) C41 0.032(5) 0.027(5) 0.036(5) 0.010(4) -0.014(4) -0.011(4) B1R 0.026(7) 0.041(8) 0.043(8) -0.009(7) -0.006(6) 0.004(7) F2R 0.023(4) 0.072(6) 0.049(5) -0.013(4) -0.014(3) 0.003(5) F3R 0.023(4) 0.072(6) 0.049(5) -0.013(4) -0.014(3) 0.003(5) F4R 0.049(7) 0.127(11) 0.083(8) -0.031(7) -0.028(6) 0.071(8) F5R 0.082(10) 0.071(8) 0.114(12) 0.010(7) -0.045(9) -0.019(8) B1' 0.045(14) 0.040(14) 0.043(14) -0.009(10) -0.011(9) -0.012(9) F2' 0.044(9) 0.060(11) 0.038(9) -0.009(9) -0.007(7) -0.008(8) F3' 0.044(9) 0.060(11) 0.038(9) -0.009(9) -0.007(7) -0.008(8) F4' 0.063(14) 0.068(15) 0.054(14) -0.031(11) -0.004(10) 0.020(11) F5' 0.056(14) 0.061(13) 0.056(13) 0.021(11) -0.012(11) -0.010(10) Cl1" 0.040(3) 0.083(5) 0.060(3) -0.011(3) 0.007(2) -0.026(3) C3" 0.114(15) 0.101(15) 0.113(15) -0.010(9) -0.004(9) -0.031(9) Cl2" 0.060(4) 0.030(3) 0.078(4) 0.003(2) -0.019(3) -0.014(2) Cl1M 0.073(8) 0.135(14) 0.081(9) -0.006(8) 0.012(6) -0.071(9) C3M 0.114(15) 0.101(15) 0.113(15) -0.010(9) -0.004(9) -0.031(9) Cl2M 0.18(2) 0.059(8) 0.124(17) 0.022(10) -0.071(17) -0.018(8) 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' Au Au -2.0133 8.8022 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Au1 C20 . . 172.5(4) ? C2 Au1 C17 . . 86.8(4) ? C20 Au1 C17 . . 85.9(4) ? C2 Au1 C34 . . 95.2(4) ? C20 Au1 C34 . . 92.2(3) ? C17 Au1 C34 . . 177.1(4) ? C2 N3 C4 . . 108.1(7) ? C2 N3 C28 . . 125.8(7) ? C4 N3 C28 . . 126.0(8) ? C2 N10 C9 . . 109.5(8) ? C2 N10 C11 . . 125.3(8) ? C9 N10 C11 . . 125.1(7) ? C20 N19 C27 . . 109.1(7) ? C20 N19 C18 . . 124.4(7) ? C27 N19 C18 . . 126.3(7) ? C20 N21 C22 . . 109.4(7) ? C20 N21 C31 . . 124.0(7) ? C22 N21 C31 . . 126.2(7) ? N3 C2 N10 . . 108.6(8) ? N3 C2 Au1 . . 132.2(6) ? N10 C2 Au1 . . 119.1(7) ? C9 C4 C5 . . 120.0(9) ? C9 C4 N3 . . 107.9(8) ? C5 C4 N3 . . 132.1(9) ? C6 C5 C4 . . 116.9(10) ? C6 C5 H5 . . 121.600000 ? C4 C5 H5 . . 121.600000 ? C7 C6 C5 . . 121.6(10) ? C7 C6 H6 . . 119.200000 ? C5 C6 H6 . . 119.200000 ? C8 C7 C6 . . 121.7(9) ? C8 C7 H7 . . 119.100000 ? C6 C7 H7 . . 119.100000 ? C7 C8 C9 . . 116.6(10) ? C7 C8 H8 . . 121.700000 ? C9 C8 H8 . . 121.700000 ? C4 C9 C8 . . 123.1(9) ? C4 C9 N10 . . 105.8(8) ? C8 C9 N10 . . 131.1(9) ? N10 C11 C12 . . 112.0(7) ? N10 C11 H11A . . 109.200000 ? C12 C11 H11A . . 109.200000 ? N10 C11 H11B . . 109.200000 ? C12 C11 H11B . . 109.200000 ? H11A C11 H11B . . 107.900000 ? C13 C12 C17 . . 120.4(9) ? C13 C12 C11 . . 120.1(8) ? C17 C12 C11 . . 119.5(8) ? C12 C13 C14 . . 120.6(8) ? C12 C13 H13 . . 119.700000 ? C14 C13 H13 . . 119.700000 ? C13 C14 C15 . . 118.6(9) ? C13 C14 H14 . . 120.700000 ? C15 C14 H14 . . 120.700000 ? C16 C15 C14 . . 122.0(9) ? C16 C15 H15 . . 119.000000 ? C14 C15 H15 . . 119.000000 ? C15 C16 C17 . . 119.1(8) ? C15 C16 C18 . . 120.5(8) ? C17 C16 C18 . . 120.4(8) ? C16 C17 C12 . . 119.3(9) ? C16 C17 Au1 . . 119.7(6) ? C12 C17 Au1 . . 121.0(7) ? N19 C18 C16 . . 110.5(7) ? N19 C18 H18A . . 109.600000 ? C16 C18 H18A . . 109.600000 ? N19 C18 H18B . . 109.600000 ? C16 C18 H18B . . 109.600000 ? H18A C18 H18B . . 108.100000 ? N19 C20 N21 . . 108.9(7) ? N19 C20 Au1 . . 119.2(6) ? N21 C20 Au1 . . 131.8(7) ? N21 C22 C27 . . 106.4(7) ? N21 C22 C23 . . 133.4(8) ? C27 C22 C23 . . 120.2(8) ? C24 C23 C22 . . 116.7(8) ? C24 C23 H23 . . 121.600000 ? C22 C23 H23 . . 121.600000 ? C23 C24 C25 . . 122.5(8) ? C23 C24 H24 . . 118.800000 ? C25 C24 H24 . . 118.800000 ? C26 C25 C24 . . 121.6(9) ? C26 C25 H25 . . 119.200000 ? C24 C25 H25 . . 119.200000 ? C25 C26 C27 . . 115.8(9) ? C25 C26 H26 . . 122.100000 ? C27 C26 H26 . . 122.100000 ? C26 C27 C22 . . 123.2(8) ? C26 C27 N19 . . 130.6(8) ? C22 C27 N19 . . 106.2(8) ? N3 C28 C29 . . 111.3(8) ? N3 C28 C30 . . 109.3(8) ? C29 C28 C30 . . 116.0(9) ? N3 C28 H28 . . 106.600000 ? C29 C28 H28 . . 106.600000 ? C30 C28 H28 . . 106.600000 ? C28 C29 H29A . . 109.500000 ? C28 C29 H29B . . 109.500000 ? H29A C29 H29B . . 109.500000 ? C28 C29 H29C . . 109.500000 ? H29A C29 H29C . . 109.500000 ? H29B C29 H29C . . 109.500000 ? C28 C30 H30A . . 109.500000 ? C28 C30 H30B . . 109.500000 ? H30A C30 H30B . . 109.500000 ? C28 C30 H30C . . 109.500000 ? H30A C30 H30C . . 109.500000 ? H30B C30 H30C . . 109.500000 ? N21 C31 C33 . . 111.7(7) ? N21 C31 C32 . . 110.0(8) ? C33 C31 C32 . . 112.8(8) ? N21 C31 H31 . . 107.400000 ? C33 C31 H31 . . 107.400000 ? C32 C31 H31 . . 107.400000 ? C31 C32 H32A . . 109.500000 ? C31 C32 H32B . . 109.500000 ? H32A C32 H32B . . 109.500000 ? C31 C32 H32C . . 109.500000 ? H32A C32 H32C . . 109.500000 ? H32B C32 H32C . . 109.500000 ? C31 C33 H33A . . 109.500000 ? C31 C33 H33B . . 109.500000 ? H33A C33 H33B . . 109.500000 ? C31 C33 H33C . . 109.500000 ? H33A C33 H33C . . 109.500000 ? H33B C33 H33C . . 109.500000 ? C35 C34 Au1 . . 173.2(8) ? C34 C35 C36 . . 176.2(10) ? C41 C36 C37 . . 118.8(9) ? C41 C36 C35 . . 120.8(8) ? C37 C36 C35 . . 120.4(9) ? C38 C37 C36 . . 119.0(9) ? C38 C37 H37 . . 120.500000 ? C36 C37 H37 . . 120.500000 ? C39 C38 C37 . . 122.0(10) ? C39 C38 H38 . . 119.000000 ? C37 C38 H38 . . 119.000000 ? C38 C39 C40 . . 119.3(9) ? C38 C39 H39 . . 120.300000 ? C40 C39 H39 . . 120.300000 ? C41 C40 C39 . . 119.2(10) ? C41 C40 H40 . . 120.400000 ? C39 C40 H40 . . 120.400000 ? C40 C41 C36 . . 121.6(9) ? C40 C41 H41 . . 119.200000 ? C36 C41 H41 . . 119.200000 ? F4R B1R F2R . . 112.9(18) ? F4R B1R F3R . . 111.3(15) ? F2R B1R F3R . . 109.2(14) ? F4R B1R F5R . . 112.7(17) ? F2R B1R F5R . . 105.4(16) ? F3R B1R F5R . . 104.8(17) ? F4' B1' F3' . . 121.(4) ? F4' B1' F2' . . 114.(4) ? F3' B1' F2' . . 118.(4) ? F4' B1' F5' . . 100.(4) ? F3' B1' F5' . . 99.(4) ? F2' B1' F5' . . 97.(3) ? Cl2" C3" Cl1" . . 111.500000 ? Cl2" C3" H3"A . . 109.300000 ? Cl1" C3" H3"A . . 109.300000 ? Cl2" C3" H3"B . . 109.300000 ? Cl1" C3" H3"B . . 109.300000 ? H3"A C3" H3"B . . 108.000000 ? Cl2M C3M Cl1M . . 124.900000 ? Cl2M C3M H3MA . . 106.100000 ? Cl1M C3M H3MA . . 106.100000 ? Cl2M C3M H3MB . . 106.100000 ? Cl1M C3M H3MB . . 106.100000 ? H3MA C3M H3MB . . 106.300000 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 C2 . 2.042(9) ? Au1 C20 . 2.048(8) ? Au1 C17 . 2.064(9) ? Au1 C34 . 2.068(10) ? N3 C2 . 1.347(12) ? N3 C4 . 1.405(11) ? N3 C28 . 1.490(11) ? N10 C2 . 1.350(11) ? N10 C9 . 1.401(11) ? N10 C11 . 1.460(11) ? N19 C20 . 1.330(11) ? N19 C27 . 1.398(11) ? N19 C18 . 1.465(11) ? N21 C20 . 1.347(10) ? N21 C22 . 1.381(11) ? N21 C31 . 1.493(11) ? C4 C9 . 1.376(13) ? C4 C5 . 1.395(13) ? C5 C6 . 1.388(14) ? C5 H5 . 0.950000 ? C6 C7 . 1.387(15) ? C6 H6 . 0.950000 ? C7 C8 . 1.361(14) ? C7 H7 . 0.950000 ? C8 C9 . 1.386(12) ? C8 H8 . 0.950000 ? C11 C12 . 1.525(13) ? C11 H11A . 0.990000 ? C11 H11B . 0.990000 ? C12 C13 . 1.378(13) ? C12 C17 . 1.403(12) ? C13 C14 . 1.383(14) ? C13 H13 . 0.950000 ? C14 C15 . 1.384(13) ? C14 H14 . 0.950000 ? C15 C16 . 1.382(13) ? C15 H15 . 0.950000 ? C16 C17 . 1.389(13) ? C16 C18 . 1.510(12) ? C18 H18A . 0.990000 ? C18 H18B . 0.990000 ? C22 C27 . 1.397(12) ? C22 C23 . 1.402(12) ? C23 C24 . 1.379(13) ? C23 H23 . 0.950000 ? C24 C25 . 1.397(13) ? C24 H24 . 0.950000 ? C25 C26 . 1.385(12) ? C25 H25 . 0.950000 ? C26 C27 . 1.393(12) ? C26 H26 . 0.950000 ? C28 C29 . 1.497(13) ? C28 C30 . 1.519(14) ? C28 H28 . 1.000000 ? C29 H29A . 0.980000 ? C29 H29B . 0.980000 ? C29 H29C . 0.980000 ? C30 H30A . 0.980000 ? C30 H30B . 0.980000 ? C30 H30C . 0.980000 ? C31 C33 . 1.515(12) ? C31 C32 . 1.520(13) ? C31 H31 . 1.000000 ? C32 H32A . 0.980000 ? C32 H32B . 0.980000 ? C32 H32C . 0.980000 ? C33 H33A . 0.980000 ? C33 H33B . 0.980000 ? C33 H33C . 0.980000 ? C34 C35 . 1.180(13) ? C35 C36 . 1.452(13) ? C36 C41 . 1.390(13) ? C36 C37 . 1.396(13) ? C37 C38 . 1.395(14) ? C37 H37 . 0.950000 ? C38 C39 . 1.349(14) ? C38 H38 . 0.950000 ? C39 C40 . 1.413(14) ? C39 H39 . 0.950000 ? C40 C41 . 1.371(13) ? C40 H40 . 0.950000 ? C41 H41 . 0.950000 ? B1R F4R . 1.29(2) ? B1R F2R . 1.34(2) ? B1R F3R . 1.42(2) ? B1R F5R . 1.42(3) ? B1' F4' . 1.29(5) ? B1' F3' . 1.31(6) ? B1' F2' . 1.46(6) ? B1' F5' . 1.58(6) ? Cl1" C3" . 1.770(5) ? C3" Cl2" . 1.748(5) ? C3" H3"A . 0.990000 ? C3" H3"B . 0.990000 ? Cl1M C3M . 1.675(5) ? C3M Cl2M . 1.617(5) ? C3M H3MA . 0.990000 ? C3M H3MB . 0.990000 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C4 N3 C2 N10 . . . . -1.9(11) ? C28 N3 C2 N10 . . . . 178.8(8) ? C4 N3 C2 Au1 . . . . 173.8(7) ? C28 N3 C2 Au1 . . . . -5.6(15) ? C9 N10 C2 N3 . . . . 3.2(11) ? C11 N10 C2 N3 . . . . -176.2(8) ? C9 N10 C2 Au1 . . . . -173.1(6) ? C11 N10 C2 Au1 . . . . 7.5(13) ? C2 N3 C4 C9 . . . . -0.2(11) ? C28 N3 C4 C9 . . . . 179.1(8) ? C2 N3 C4 C5 . . . . 179.4(10) ? C28 N3 C4 C5 . . . . -1.2(16) ? C9 C4 C5 C6 . . . . -3.1(14) ? N3 C4 C5 C6 . . . . 177.3(10) ? C4 C5 C6 C7 . . . . 2.0(15) ? C5 C6 C7 C8 . . . . 0.1(16) ? C6 C7 C8 C9 . . . . -1.1(14) ? C5 C4 C9 C8 . . . . 2.1(15) ? N3 C4 C9 C8 . . . . -178.2(8) ? C5 C4 C9 N10 . . . . -177.6(8) ? N3 C4 C9 N10 . . . . 2.1(10) ? C7 C8 C9 C4 . . . . 0.0(14) ? C7 C8 C9 N10 . . . . 179.7(9) ? C2 N10 C9 C4 . . . . -3.3(11) ? C11 N10 C9 C4 . . . . 176.2(8) ? C2 N10 C9 C8 . . . . 177.0(10) ? C11 N10 C9 C8 . . . . -3.6(16) ? C2 N10 C11 C12 . . . . 46.5(12) ? C9 N10 C11 C12 . . . . -132.8(9) ? N10 C11 C12 C13 . . . . 130.9(9) ? N10 C11 C12 C17 . . . . -48.4(11) ? C17 C12 C13 C14 . . . . 2.7(14) ? C11 C12 C13 C14 . . . . -176.6(8) ? C12 C13 C14 C15 . . . . -2.3(14) ? C13 C14 C15 C16 . . . . 0.2(15) ? C14 C15 C16 C17 . . . . 1.5(14) ? C14 C15 C16 C18 . . . . -177.5(9) ? C15 C16 C17 C12 . . . . -1.1(13) ? C18 C16 C17 C12 . . . . 177.9(8) ? C15 C16 C17 Au1 . . . . 178.8(7) ? C18 C16 C17 Au1 . . . . -2.2(11) ? C13 C12 C17 C16 . . . . -1.0(13) ? C11 C12 C17 C16 . . . . 178.3(8) ? C13 C12 C17 Au1 . . . . 179.1(7) ? C11 C12 C17 Au1 . . . . -1.6(11) ? C20 N19 C18 C16 . . . . 49.6(11) ? C27 N19 C18 C16 . . . . -126.1(9) ? C15 C16 C18 N19 . . . . 128.5(9) ? C17 C16 C18 N19 . . . . -50.5(11) ? C27 N19 C20 N21 . . . . -0.1(9) ? C18 N19 C20 N21 . . . . -176.5(7) ? C27 N19 C20 Au1 . . . . -177.8(5) ? C18 N19 C20 Au1 . . . . 5.8(11) ? C22 N21 C20 N19 . . . . 0.8(9) ? C31 N21 C20 N19 . . . . 173.6(7) ? C22 N21 C20 Au1 . . . . 178.1(6) ? C31 N21 C20 Au1 . . . . -9.2(12) ? C20 N21 C22 C27 . . . . -1.1(9) ? C31 N21 C22 C27 . . . . -173.7(7) ? C20 N21 C22 C23 . . . . -179.8(9) ? C31 N21 C22 C23 . . . . 7.6(14) ? N21 C22 C23 C24 . . . . 177.7(9) ? C27 C22 C23 C24 . . . . -0.9(12) ? C22 C23 C24 C25 . . . . 0.7(13) ? C23 C24 C25 C26 . . . . 0.1(14) ? C24 C25 C26 C27 . . . . -0.8(13) ? C25 C26 C27 C22 . . . . 0.7(13) ? C25 C26 C27 N19 . . . . -179.0(8) ? N21 C22 C27 C26 . . . . -178.8(8) ? C23 C22 C27 C26 . . . . 0.2(13) ? N21 C22 C27 N19 . . . . 1.0(9) ? C23 C22 C27 N19 . . . . 179.9(7) ? C20 N19 C27 C26 . . . . 179.2(9) ? C18 N19 C27 C26 . . . . -4.5(14) ? C20 N19 C27 C22 . . . . -0.6(9) ? C18 N19 C27 C22 . . . . 175.7(8) ? C2 N3 C28 C29 . . . . -112.0(10) ? C4 N3 C28 C29 . . . . 68.8(12) ? C2 N3 C28 C30 . . . . 118.6(10) ? C4 N3 C28 C30 . . . . -60.6(12) ? C20 N21 C31 C33 . . . . 125.8(9) ? C22 N21 C31 C33 . . . . -62.7(11) ? C20 N21 C31 C32 . . . . -108.2(9) ? C22 N21 C31 C32 . . . . 63.4(11) ? C41 C36 C37 C38 . . . . 2.0(15) ? C35 C36 C37 C38 . . . . -177.0(9) ? C36 C37 C38 C39 . . . . -0.9(17) ? C37 C38 C39 C40 . . . . -0.6(17) ? C38 C39 C40 C41 . . . . 0.9(16) ? C39 C40 C41 C36 . . . . 0.3(16) ? C37 C36 C41 C40 . . . . -1.8(15) ? C35 C36 C41 C40 . . . . 177.3(9) ?