#------------------------------------------------------------------------------ #$Date: 2019-11-17 07:52:07 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228749 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/91/1549133.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_1549133 loop_ _publ_author_name 'Serra, Jordi' 'Font, Pau' 'Sosa Carrizo, E. Daiann' 'Mallet-Ladeira, Sonia' 'Massou, St\'ephane' 'Parella, Teodor' 'Miqueu, Karinne' 'Amgoune, Abderrahmane' 'Ribas, Xavi' 'Bourissou, Didier' _publ_section_title ; Cyclometalated gold(iii) complexes: noticeable differences between (N,C) and (P,C) ligands in migratory insertion. ; _journal_issue 16 _journal_name_full 'Chemical science' _journal_page_first 3932 _journal_page_last 3940 _journal_paper_doi 10.1039/c7sc04899h _journal_volume 9 _journal_year 2018 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C23 H23 Au N O, F6 Sb' _chemical_formula_sum 'C23 H23 Au F6 N O Sb' _chemical_formula_weight 762.15 _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_update_record ; 2017-09-13 deposited with the CCDC. 2018-03-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.6287(3) _cell_length_b 16.4246(8) _cell_length_c 21.5858(11) _cell_measurement_reflns_used 9977 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 27.36 _cell_measurement_theta_min 3.45 _cell_volume 2350.1(2) _computing_cell_refinement 'APEX2 and SAINT' _computing_data_collection APEX2 _computing_data_reduction SAINT _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 22815 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.572 _diffrn_reflns_theta_min 3.607 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.448 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1440 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.681 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.108 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.018(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 6582 _refine_ls_number_restraints 65 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0262 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0466 _reflns_Friedel_coverage 0.766 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 1 _reflns_number_gt 6022 _reflns_number_total 6582 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7sc04899h3.cif _cod_data_source_block 5A-H2O _cod_depositor_comments 'Adding full bibliography for 1549133--1549134.cif.' _cod_database_code 1549133 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL JS24_a.res in P2(1)2(1)2(1) CELL 0.71073 6.6287 16.4246 21.5858 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0008 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N F SB AU O UNIT 92 92 4 24 4 4 4 MERG 2 OMIT 1 2 0 OMIT 1 1 1 OMIT -1 1 1 OMIT 0 2 3 TWIN SHEL 6 0.72 DELU F1 > F6' SIMU 0.01 F1 > F6' DFIX 0.850 0.020 O1 H1A DFIX 0.850 0.020 O1 H1B FMAP 2 PLAN 20 SIZE 0.020 0.040 0.180 ACTA BOND $H L.S. 4 TEMP -80.14 WGHT 0.015300 BASF 0.01797 FVAR 0.15877 0.64754 0.07196 C1 1 0.481414 0.390937 0.482379 11.00000 0.01873 0.02976 = 0.03311 0.00673 -0.00078 0.00206 AFIX 43 H1 2 0.481811 0.444659 0.498688 11.00000 -1.20000 AFIX 0 C2 1 0.483022 0.379679 0.418135 11.00000 0.01773 0.04680 = 0.03538 0.01315 -0.00160 -0.00074 AFIX 43 H2 2 0.485266 0.425407 0.391194 11.00000 -1.20000 AFIX 0 C3 1 0.481356 0.302860 0.394408 11.00000 0.02186 0.04942 = 0.02221 0.00060 -0.00018 0.00049 AFIX 43 H3 2 0.482230 0.294926 0.350814 11.00000 -1.20000 AFIX 0 C4 1 0.478354 0.235511 0.434240 11.00000 0.01262 0.04783 = 0.02384 -0.00307 -0.00399 0.00112 C5 1 0.479280 0.251168 0.497689 11.00000 0.01154 0.02821 = 0.02424 -0.00070 -0.00008 0.00056 C6 1 0.476485 0.152353 0.415171 11.00000 0.01904 0.04584 = 0.02945 -0.01962 -0.00301 -0.00264 AFIX 43 H6 2 0.474548 0.139924 0.372193 11.00000 -1.20000 AFIX 0 C7 1 0.477400 0.090926 0.456663 11.00000 0.02334 0.03113 = 0.04505 -0.01664 0.00012 0.00361 AFIX 43 H7 2 0.477916 0.036287 0.442226 11.00000 -1.20000 AFIX 0 C8 1 0.477608 0.106126 0.521536 11.00000 0.01771 0.02864 = 0.03959 -0.00686 0.00019 -0.00013 C9 1 0.478852 0.043373 0.567273 11.00000 0.02986 0.03220 = 0.05280 0.00009 0.00085 0.00231 AFIX 43 H9 2 0.476161 -0.012148 0.554962 11.00000 -1.20000 AFIX 0 C10 1 0.483873 0.062945 0.628316 11.00000 0.03798 0.03002 = 0.05253 0.01258 0.00416 0.00009 AFIX 43 H10 2 0.488665 0.020419 0.658110 11.00000 -1.20000 AFIX 0 C11 1 0.482219 0.143678 0.648759 11.00000 0.02729 0.04018 = 0.02795 0.00685 0.00267 -0.00161 AFIX 43 H11 2 0.484112 0.155270 0.691873 11.00000 -1.20000 AFIX 0 C12 1 0.477890 0.205854 0.606885 11.00000 0.01470 0.03186 = 0.02793 -0.00029 -0.00087 -0.00087 C13 1 0.479072 0.187020 0.542823 11.00000 0.01170 0.02634 = 0.02627 -0.00265 -0.00261 -0.00062 C14 1 0.463076 0.319076 0.715330 11.00000 0.04025 0.04083 = 0.02265 -0.00501 0.00476 0.00171 AFIX 23 H14A 2 0.371889 0.361693 0.731694 11.00000 -1.20000 H14B 2 0.408282 0.265416 0.727711 11.00000 -1.20000 AFIX 0 C15 1 0.671117 0.329902 0.743072 11.00000 0.03535 0.04155 = 0.02351 -0.00267 -0.00549 -0.00055 AFIX 23 H15A 2 0.729367 0.381799 0.728100 11.00000 -1.20000 H15B 2 0.759439 0.285130 0.728676 11.00000 -1.20000 AFIX 0 C16 1 0.667586 0.330453 0.813954 11.00000 0.04392 0.03026 = 0.02910 -0.00157 0.00052 0.00466 AFIX 23 H16A 2 0.570448 0.372081 0.828457 11.00000 -1.20000 H16B 2 0.621073 0.276756 0.829123 11.00000 -1.20000 AFIX 0 C17 1 0.872010 0.348457 0.840539 11.00000 0.05450 0.05340 = 0.03136 0.00367 -0.00351 -0.00884 AFIX 23 H17A 2 0.918009 0.401163 0.823347 11.00000 -1.20000 H17B 2 0.966451 0.306174 0.825464 11.00000 -1.20000 AFIX 0 C18 1 0.891054 0.352730 0.910412 11.00000 0.06104 0.02596 = 0.03416 0.00035 -0.01247 0.00859 C19 1 0.739393 0.329391 0.949447 11.00000 0.07557 0.04712 = 0.02961 0.00473 -0.00362 0.00230 AFIX 43 H19 2 0.615357 0.310413 0.932787 11.00000 -1.20000 AFIX 0 C20 1 0.765280 0.333212 1.014209 11.00000 0.10878 0.04574 = 0.03403 0.00232 0.00880 0.01011 AFIX 43 H20 2 0.658873 0.317142 1.041035 11.00000 -1.20000 AFIX 0 C21 1 0.945658 0.360368 1.038495 11.00000 0.11208 0.04073 = 0.04101 -0.01102 -0.02041 0.00775 AFIX 43 H21 2 0.965083 0.362507 1.082069 11.00000 -1.20000 AFIX 0 C22 1 1.093551 0.383758 0.999824 11.00000 0.09148 0.04720 = 0.04936 -0.00615 -0.03385 -0.00370 AFIX 43 H22 2 1.217139 0.402963 1.016646 11.00000 -1.20000 AFIX 0 C23 1 1.070633 0.380617 0.936102 11.00000 0.06646 0.04047 = 0.04582 0.00113 -0.02015 -0.00414 AFIX 43 H23 2 1.177811 0.397549 0.909878 11.00000 -1.20000 AFIX 0 N1 3 0.479340 0.327921 0.521080 11.00000 0.01482 0.02886 = 0.02239 -0.00013 -0.00210 0.00101 SAME SB1 F1' > F6' SB1 5 0.991916 0.582447 0.704155 11.00000 0.03958 0.03503 = 0.03088 -0.01185 0.00638 -0.00323 PART 1 F1 4 0.799080 0.524220 0.656841 21.00000 0.04870 0.08232 = 0.08231 -0.03953 -0.00716 -0.01964 F2 4 0.860263 0.547005 0.774471 21.00000 0.10307 0.10047 = 0.06228 0.01183 0.05128 0.01685 F3 4 1.179343 0.637008 0.748701 21.00000 0.12251 0.12060 = 0.09435 -0.04344 -0.04665 -0.04614 F4 4 1.111354 0.613063 0.631200 21.00000 0.06809 0.12893 = 0.06089 0.02967 0.03332 -0.01232 F5 4 1.147881 0.488828 0.703122 21.00000 0.06254 0.07410 = 0.08060 0.00382 0.01510 0.03684 F6 4 0.814984 0.672302 0.699606 21.00000 0.09955 0.05443 = 0.10796 -0.01209 0.00171 0.03185 PART 2 F1' 4 0.746611 0.539115 0.691049 -21.00000 0.03620 0.08512 = 0.12880 -0.03262 0.01105 -0.02010 F2' 4 0.986870 0.544325 0.785340 -21.00000 0.18060 0.07333 = 0.03061 -0.00654 0.03640 -0.01117 F3' 4 1.259899 0.618574 0.717901 -21.00000 0.08764 0.09483 = 0.09960 -0.01565 -0.03096 -0.04882 F4' 4 1.022068 0.614656 0.625146 -21.00000 0.10517 0.11985 = 0.03823 0.01637 -0.02729 -0.00272 F5' 4 1.111047 0.481923 0.684148 -21.00000 0.06155 0.05395 = 0.08707 -0.02563 0.00816 0.01328 F6' 4 0.892035 0.680009 0.732096 -21.00000 0.08629 0.03550 = 0.11147 -0.03380 0.02963 0.00749 PART 0 AU1 6 0.471908 0.326413 0.620255 11.00000 0.01943 0.02958 = 0.02076 -0.00296 0.00093 -0.00062 O1 7 0.459389 0.457145 0.623224 11.00000 0.04075 0.02893 = 0.04444 -0.00855 0.00348 0.00137 H1A 2 0.362292 0.472306 0.645807 11.00000 0.07495 H1B 2 0.565776 0.482345 0.631099 11.00000 0.05347 HKLF 4 REM JS24_a.res in P2(1)2(1)2(1) REM R1 = 0.0262 for 6022 Fo > 4sig(Fo) and 0.0315 for all 6582 data REM 363 parameters refined using 65 restraints END WGHT 0.0153 0.0000 REM Highest difference peak 0.681, deepest hole -0.598, 1-sigma level 0.108 Q1 1 0.5314 0.3619 0.6387 11.00000 0.05 0.68 Q2 1 0.5047 0.2636 0.4072 11.00000 0.05 0.51 Q3 1 0.4851 0.3349 0.4080 11.00000 0.05 0.50 Q4 1 0.5535 0.0769 0.5563 11.00000 0.05 0.45 Q5 1 0.4457 0.3221 0.3666 11.00000 0.05 0.45 Q6 1 0.5173 0.1980 0.4278 11.00000 0.05 0.43 Q7 1 0.5356 0.2246 0.3009 11.00000 0.05 0.43 Q8 1 0.5290 0.3040 0.3785 11.00000 0.05 0.43 Q9 1 0.4689 0.2405 0.6229 11.00000 0.05 0.42 Q10 1 0.2665 0.3214 0.6233 11.00000 0.05 0.42 Q11 1 1.1504 0.4623 0.8625 11.00000 0.05 0.39 Q12 1 0.4776 0.2572 0.3516 11.00000 0.05 0.39 Q13 1 0.4709 0.1812 0.3235 11.00000 0.05 0.39 Q14 1 0.5321 0.0783 0.4058 11.00000 0.05 0.38 Q15 1 1.0237 0.5373 0.7145 11.00000 0.05 0.38 Q16 1 0.4834 0.2803 0.4501 11.00000 0.05 0.38 Q17 1 0.4961 0.3568 0.4982 11.00000 0.05 0.37 Q18 1 0.4307 0.2102 0.3576 11.00000 0.05 0.37 Q19 1 1.0190 0.3210 0.7152 11.00000 0.05 0.37 Q20 1 0.7178 0.3266 0.6234 11.00000 0.05 0.37 ; _shelx_res_checksum 96102 _shelx_hkl_file ; 0 -1 0 0.00 0.10 0 -1 0 0.00 0.10 0 1 0 0.00 0.10 0 1 0 0.00 0.10 0 2 0 -4.30 0.20 0 -2 0 -4.50 0.20 0 -2 0 -4.40 0.10 0 2 0 -4.30 0.20 0 3 0 -1.80 0.30 0 3 0 -1.30 0.60 0 -3 0 -1.90 0.20 0 4 0 2825.52 78.29 0 -4 0 2899.71 77.79 0 5 0 -0.10 0.80 0 -5 0 0.90 0.70 0 -6 0 1186.98 33.30 0 6 0 1157.38 34.10 0 -7 0 -0.50 0.80 0 7 0 -0.20 1.10 0 -8 0 1353.56 38.90 0 8 0 1384.36 40.30 0 -9 0 2.30 1.20 0 9 0 -0.60 1.30 0 10 0 1.80 1.80 0 -10 0 1.70 1.30 0 -11 0 2.60 1.50 0 11 0 4.50 2.00 0 -12 0 1234.68 36.70 0 12 0 1265.97 38.90 0 -13 0 4.70 1.80 0 13 0 -1.30 2.10 0 -14 0 378.06 13.60 0 14 0 361.76 15.50 0 15 0 4.10 2.80 0 -15 0 2.20 1.70 0 16 0 6.10 3.00 0 17 0 -1.40 2.60 0 18 0 17.40 4.60 0 19 0 -1.00 2.80 0 20 0 176.88 11.60 0 21 0 -0.90 3.50 0 22 0 33.30 6.90 0 23 0 1.50 4.20 1 0 0 -14.60 0.40 -1 0 0 -14.80 0.40 1 -1 0 -0.40 0.30 1 -1 0 -0.70 0.40 -1 -1 0 -0.30 0.30 1 1 0 4.50 0.90 -1 1 0 3.80 0.80 1 -2 0 1066.79 32.00 -1 -2 0 1224.08 31.70 -1 2 0 1105.09 31.50 1 -3 0 28.50 2.00 -1 -3 0 26.40 1.80 1 3 0 29.80 2.10 -1 3 0 26.80 2.00 1 -3 0 29.50 2.20 -1 3 0 31.80 2.10 -1 -4 0 387.36 11.80 1 -4 0 373.86 12.40 1 4 0 364.56 12.10 -1 4 0 400.36 12.30 1 -4 0 376.06 12.20 -1 4 0 398.16 12.40 -1 5 0 44.70 3.10 -1 5 0 45.30 3.00 -1 -5 0 45.90 2.70 1 -5 0 45.30 3.00 1 -5 0 46.00 3.10 1 5 0 42.90 2.80 1 6 0 322.57 11.10 -1 -6 0 330.47 10.80 -1 6 0 328.67 11.50 -1 6 0 326.57 11.70 -1 -7 0 1.10 1.10 -1 7 0 0.50 1.30 -1 7 0 3.80 1.60 1 7 0 3.80 1.50 -1 8 0 64.39 4.50 -1 -8 0 47.20 3.30 1 8 0 57.79 3.90 -1 -9 0 44.90 3.30 1 9 0 50.09 4.60 -1 9 0 38.20 4.40 -1 10 0 2039.00 62.79 1 10 0 2216.28 62.09 -1 -10 0 2223.28 60.79 1 11 0 4.60 2.10 -1 -11 0 6.00 1.70 -1 11 0 4.50 2.40 1 -12 0 244.18 10.60 -1 -12 0 251.17 9.60 1 12 0 241.58 11.00 -1 12 0 233.48 11.70 1 -13 0 6.30 2.50 1 13 0 5.70 2.60 -1 -13 0 8.00 2.10 -1 13 0 7.80 3.00 -1 14 0 273.97 13.40 -1 -14 0 278.57 10.70 1 -14 0 269.37 11.70 1 14 0 257.77 12.40 -1 15 0 3.00 2.80 1 -15 0 0.40 2.10 1 15 0 3.10 2.50 -1 -15 0 1.00 1.80 1 16 0 138.99 9.00 -1 16 0 143.39 9.70 -1 17 0 8.30 4.10 1 17 0 12.50 4.00 1 18 0 138.89 9.60 -1 18 0 129.49 10.20 -1 19 0 0.90 3.40 1 19 0 -1.10 2.90 -1 20 0 2.20 4.00 1 20 0 4.80 3.80 -1 21 0 1.30 3.80 1 21 0 4.60 3.70 1 22 0 168.78 12.00 -1 22 0 176.18 13.00 -1 23 0 -1.10 4.10 1 23 0 -1.00 3.50 2 0 0 9959.40 269.67 -2 0 0 9999.00 269.27 -2 -1 0 339.67 11.60 -2 1 0 329.67 11.70 2 -1 0 346.17 12.10 2 1 0 352.26 12.00 2 -2 0 212.28 7.50 -2 2 0 219.88 8.30 2 2 0 201.18 8.30 2 -2 0 216.08 8.50 -2 -2 0 204.28 7.90 2 -3 0 4.50 1.60 -2 3 0 6.20 1.60 2 3 0 2.80 1.50 -2 -3 0 6.10 1.50 2 -3 0 7.00 1.50 2 4 0 828.32 25.70 2 -4 0 850.91 26.10 -2 -4 0 852.41 25.10 -2 4 0 822.72 25.60 2 -4 0 838.02 25.00 -2 4 0 866.61 25.20 2 5 0 220.78 8.60 -2 -5 0 196.18 7.80 -2 5 0 210.18 8.20 2 -5 0 198.98 8.00 -2 5 0 204.38 8.50 2 -5 0 206.78 8.80 2 6 0 32.90 3.60 -2 -6 0 40.20 3.10 -2 6 0 35.00 3.70 -2 6 0 39.10 4.00 2 -6 0 38.60 4.10 2 -6 0 36.80 3.60 2 -7 0 60.19 4.60 2 -7 0 63.89 4.40 -2 -7 0 60.99 3.90 2 7 0 61.39 4.40 -2 7 0 56.99 5.50 -2 7 0 48.50 4.70 2 8 0 1006.50 31.10 -2 -8 0 995.20 30.10 -2 8 0 1027.90 31.60 2 -8 0 1034.00 31.60 2 -8 0 1013.20 31.10 2 9 0 0.90 1.50 2 -9 0 1.60 1.70 -2 9 0 0.00 1.50 -2 -9 0 0.50 1.20 -2 10 0 26.50 4.10 2 -10 0 19.20 3.40 2 10 0 21.50 3.50 -2 -10 0 21.30 2.90 -2 -11 0 45.80 4.30 -2 11 0 46.60 5.70 2 -11 0 46.00 5.20 2 11 0 47.20 5.10 2 -12 0 752.52 25.00 -2 12 0 733.33 26.10 -2 -12 0 719.33 23.10 2 12 0 730.53 24.80 -2 -13 0 14.00 2.60 2 -13 0 9.90 2.90 -2 13 0 8.80 3.40 2 13 0 10.70 3.10 2 -14 0 170.48 9.30 -2 14 0 156.28 10.20 -2 -14 0 166.58 7.80 2 14 0 173.28 9.50 2 15 0 8.20 3.30 2 -15 0 15.50 3.60 -2 15 0 17.70 4.50 2 16 0 3.40 3.00 -2 16 0 1.20 3.00 -2 17 0 2.70 3.50 2 17 0 3.90 3.10 2 18 0 2.40 3.20 -2 18 0 1.30 3.40 -2 19 0 0.90 3.60 2 19 0 4.60 3.50 2 20 0 95.59 9.90 -2 20 0 113.49 11.70 -2 21 0 4.90 4.50 2 21 0 4.70 4.10 -2 22 0 22.80 6.40 2 22 0 21.90 5.90 3 0 0 0.10 1.60 -3 0 0 -1.20 1.40 3 -1 0 104.59 6.30 -3 1 0 104.49 5.90 3 1 0 105.99 6.20 -3 -1 0 90.79 5.60 3 -2 0 1260.27 38.00 3 2 0 1243.68 37.70 -3 -2 0 1202.48 36.90 -3 2 0 1256.27 37.50 -3 3 0 238.18 10.20 -3 -3 0 243.68 9.80 3 -3 0 242.08 9.10 3 3 0 225.78 10.10 3 -3 0 224.18 10.30 -3 -4 0 92.89 5.30 -3 4 0 80.49 5.60 3 -4 0 86.59 4.80 3 4 0 92.59 5.80 3 -4 0 89.59 5.90 -3 -5 0 258.77 10.10 3 5 0 244.98 10.70 3 -5 0 239.78 9.60 -3 5 0 240.18 10.70 3 -5 0 257.77 11.10 -3 6 0 31.50 4.00 3 -6 0 32.90 4.40 3 -6 0 53.29 4.00 -3 6 0 39.20 4.20 3 6 0 42.00 4.60 -3 -6 0 39.60 3.90 3 -7 0 42.40 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3 -3 26 26.80 7.20 3 3 -26 23.00 5.60 -3 -3 -26 17.60 5.70 3 4 26 70.99 10.90 -3 4 -26 56.89 7.50 3 -4 -26 56.09 10.10 3 4 -26 74.69 9.90 -3 -4 -26 57.09 8.70 3 -4 26 57.29 10.00 3 -5 -26 14.60 6.50 3 5 26 6.60 6.50 -3 5 -26 13.70 4.30 3 -5 26 8.50 5.80 -3 -5 -26 6.00 4.20 3 -6 -26 22.00 7.40 3 -6 26 6.60 5.60 -3 -6 -26 16.60 6.10 3 -7 -26 26.10 8.30 3 -7 26 18.10 8.00 -3 -7 -26 24.00 6.70 3 -8 -26 19.00 7.10 -3 -8 -26 17.70 6.40 3 -9 -26 65.19 11.40 -3 -9 -26 53.09 9.20 3 -10 -26 9.80 6.00 3 10 26 27.90 10.60 -3 -10 -26 14.60 6.20 4 0 -26 29.30 7.00 -4 0 -26 9.90 4.80 4 0 26 8.60 6.60 -4 1 -26 65.09 8.70 4 -1 -26 57.59 9.50 4 1 26 51.49 9.90 -4 -1 -26 78.59 9.70 4 -1 26 73.29 11.70 4 -2 -26 32.70 7.80 -4 2 -26 30.30 6.50 4 2 26 20.70 7.00 4 -2 26 49.10 11.20 4 2 -26 31.00 7.60 -4 -2 -26 37.90 7.60 4 -3 -26 39.80 8.80 4 3 26 43.90 9.60 -4 3 -26 45.70 7.40 4 3 -26 35.60 8.00 -4 -3 -26 56.69 8.70 4 -4 -26 30.90 8.60 -4 4 -26 35.60 6.60 4 4 26 46.20 10.90 -4 -4 -26 31.90 7.30 4 4 -26 42.80 7.90 -4 5 -26 13.10 4.70 4 -5 -26 -1.80 4.90 -4 -5 -26 13.10 5.50 4 -6 -26 23.70 8.50 -4 -6 -26 50.79 9.00 4 -7 -26 24.00 8.60 -4 -7 -26 27.80 7.10 5 0 -26 25.80 7.40 -5 0 -26 24.50 6.90 5 -1 -26 29.30 8.80 -5 1 -26 35.50 7.30 -5 -1 -26 49.99 8.40 5 1 -26 32.30 8.20 -5 2 -26 22.60 6.40 5 -2 -26 9.90 6.60 5 2 -26 10.60 6.00 -5 -2 -26 26.70 7.10 0 0 27 2.40 4.60 0 0 -27 -0.40 3.10 0 -1 -27 9.30 4.50 0 1 -27 14.80 4.60 0 -1 27 15.80 5.30 0 -2 -27 132.09 12.40 0 2 -27 115.29 9.20 0 -2 27 107.19 11.30 0 -3 27 18.70 5.90 0 3 -27 13.70 4.40 0 -3 -27 14.80 5.20 0 -4 -27 122.89 12.60 0 -4 27 109.89 11.60 0 -5 -27 10.80 5.10 0 -5 27 5.70 4.60 0 -6 27 16.90 6.20 0 -6 -27 23.10 6.50 0 -7 -27 8.10 5.30 0 -7 27 11.40 5.80 0 -8 -27 71.49 10.30 0 -8 27 64.39 9.70 0 -9 27 12.90 6.30 0 -9 -27 21.10 7.30 0 -10 -27 134.59 14.30 0 -10 27 104.19 12.70 0 -11 27 11.50 6.70 0 -11 -27 16.40 6.60 -1 0 -27 155.28 10.90 1 0 27 159.38 12.60 1 0 -27 167.48 11.50 1 -1 -27 23.20 5.70 1 1 27 29.60 6.90 -1 1 -27 27.10 5.70 1 1 -27 23.50 5.30 1 -1 27 17.60 6.10 -1 -1 -27 24.90 5.50 1 -2 -27 49.90 8.00 1 2 27 40.80 7.70 -1 2 -27 35.20 6.10 1 2 -27 51.39 7.20 1 -2 27 49.50 8.90 -1 -2 -27 49.50 7.70 1 3 27 -2.80 3.80 1 -3 -27 -1.80 3.40 -1 3 -27 -1.00 3.00 1 -3 27 -2.50 3.90 1 3 -27 1.10 3.10 -1 -3 -27 0.50 3.80 1 -4 -27 2.70 4.20 1 4 27 6.90 4.90 -1 -4 -27 4.90 4.50 1 -4 27 10.60 5.50 1 -5 -27 31.00 7.00 1 5 27 30.60 7.30 -1 -5 -27 9.70 4.80 1 -5 27 29.70 7.10 1 6 27 128.19 18.60 1 -6 -27 133.39 13.70 1 -6 27 111.69 12.80 -1 -6 -27 121.29 12.50 1 -7 -27 9.90 5.90 1 -7 27 17.20 6.70 -1 -7 -27 15.30 5.80 1 -8 -27 99.19 12.50 -1 -8 -27 108.79 12.70 1 -8 27 93.19 12.10 1 -9 -27 4.60 5.00 1 -9 27 2.50 5.30 -1 -9 -27 2.60 5.30 1 -10 -27 6.10 5.20 -1 -10 -27 2.20 4.90 1 -11 -27 12.60 6.40 -1 -11 -27 18.80 6.60 2 0 -27 2.00 3.90 -2 0 -27 4.50 3.60 2 0 27 5.10 4.80 2 1 27 10.70 6.00 2 -1 -27 19.40 5.80 -2 1 -27 19.90 5.00 -2 -1 -27 19.50 5.50 2 -1 27 19.10 6.90 2 1 -27 12.80 4.90 2 -2 -27 80.79 10.40 2 2 27 78.39 10.50 -2 2 -27 91.09 9.20 -2 -2 -27 81.29 9.60 2 2 -27 78.19 9.10 2 -2 27 69.49 10.60 2 -3 -27 35.80 7.70 2 3 27 32.20 7.70 -2 3 -27 43.30 6.50 2 -3 27 29.90 7.40 -2 -3 -27 42.40 7.60 2 3 -27 31.20 6.00 2 4 27 74.89 10.70 -2 4 -27 73.39 8.30 2 -4 -27 84.59 10.90 -2 -4 -27 84.99 10.20 2 -4 27 86.49 11.60 2 5 27 7.60 6.10 2 -5 -27 3.20 5.10 2 -5 27 15.20 6.60 -2 -5 -27 12.00 5.70 2 -6 -27 17.30 7.00 2 6 27 23.10 7.10 2 -6 27 25.10 7.10 -2 -6 -27 18.50 6.10 2 7 27 1.80 5.80 2 -7 -27 6.20 5.40 -2 -7 -27 9.60 5.30 2 -7 27 -2.90 5.60 2 -8 -27 53.29 10.20 -2 -8 -27 50.59 8.90 2 -8 27 46.90 10.60 2 -9 -27 9.20 6.40 -2 -9 -27 28.10 7.10 2 -10 -27 88.79 12.50 -2 -10 -27 91.89 11.70 -3 0 -27 122.99 11.70 3 0 -27 131.99 12.70 3 0 27 106.59 13.00 3 -1 -27 53.39 9.00 3 1 27 27.80 7.50 -3 1 -27 39.50 6.90 -3 -1 -27 34.00 7.00 3 1 -27 44.80 7.90 3 -1 27 47.00 9.10 3 -2 -27 25.90 7.00 -3 2 -27 38.20 6.70 3 2 27 28.00 7.70 3 2 -27 25.20 6.00 3 -2 27 14.30 6.70 -3 -2 -27 26.30 6.30 3 3 27 14.30 7.00 3 -3 -27 -4.00 3.90 -3 3 -27 -0.10 3.40 -3 -3 -27 -0.40 3.70 3 -3 27 1.30 5.30 3 3 -27 -1.80 3.30 3 -4 -27 0.10 5.00 3 4 27 2.50 6.10 -3 4 -27 1.40 3.50 -3 -4 -27 4.10 4.40 3 -4 27 1.50 5.70 3 -5 -27 23.20 7.50 3 5 27 26.50 8.30 -3 -5 -27 19.00 6.10 3 -5 27 16.70 7.60 3 -6 -27 74.09 11.50 3 6 27 67.69 11.00 -3 -6 -27 84.69 11.00 3 -7 -27 6.70 6.50 -3 -7 -27 35.70 7.70 3 -8 -27 65.29 11.70 -3 -8 -27 65.59 9.90 4 0 -27 2.20 4.50 -4 0 -27 0.90 3.90 4 -1 -27 18.10 6.40 -4 1 -27 16.80 5.50 -4 -1 -27 33.70 7.10 -4 2 -27 57.79 8.40 4 -2 -27 43.90 8.70 -4 -2 -27 58.89 9.20 4 2 -27 46.00 9.20 4 -3 -27 64.79 10.90 -4 3 -27 57.79 8.10 -4 -3 -27 59.39 9.40 4 3 -27 50.59 9.00 -4 4 -27 38.60 6.80 4 -4 -27 42.30 9.30 -4 -4 -27 37.90 7.80 4 -5 -27 8.20 6.90 -4 5 -27 7.40 5.10 -4 -5 -27 30.50 7.40 0 0 -28 79.39 9.70 0 1 -28 5.50 4.00 0 -1 -28 -0.70 3.70 0 2 -28 10.80 4.50 0 -2 -28 19.90 6.00 0 -3 28 72.59 9.60 0 -3 -28 70.19 9.80 0 -4 28 34.70 7.40 0 -4 -28 35.10 7.60 0 -5 -28 59.69 9.30 0 -5 28 68.39 9.60 0 -6 28 50.09 8.60 0 -6 -28 71.19 10.10 0 -7 28 45.60 8.30 0 -7 -28 31.90 7.70 0 -8 28 25.40 7.00 0 -8 -28 40.20 8.60 0 -9 -28 45.00 9.00 0 -9 28 32.30 7.90 1 0 28 2.70 4.30 1 0 -28 7.70 4.00 -1 0 -28 9.10 4.20 -1 1 -28 27.10 5.70 1 1 28 27.10 6.70 1 -1 -28 31.20 6.70 1 -1 28 24.70 6.90 -1 -1 -28 31.50 6.50 1 1 -28 23.80 5.40 -1 2 -28 53.89 7.20 1 -2 -28 48.10 7.80 1 2 28 60.19 9.30 1 -2 28 79.89 10.60 1 2 -28 65.69 8.20 -1 -2 -28 71.39 9.30 1 -3 -28 42.20 7.70 -1 3 -28 55.59 7.20 1 3 28 47.70 8.60 -1 -3 -28 56.39 8.70 1 -3 28 64.29 9.80 1 -4 -28 37.40 7.60 -1 -4 -28 42.80 7.80 1 -4 28 42.20 8.40 1 -5 -28 68.39 9.90 1 -5 28 67.79 10.10 -1 -5 -28 65.19 9.50 1 -6 -28 1.80 4.80 -1 -6 -28 -2.20 4.00 1 -6 28 1.50 4.90 1 -7 -28 92.99 12.00 1 -7 28 92.59 12.10 -1 -7 -28 92.19 11.40 1 -8 -28 16.90 6.40 1 -8 28 2.70 5.50 -1 -8 -28 7.90 5.80 1 -9 -28 8.80 5.80 -1 -9 -28 -3.90 4.90 2 0 -28 50.19 8.20 -2 0 -28 58.69 8.10 2 0 28 63.69 10.10 -2 1 -28 2.30 3.70 2 -1 -28 -0.10 4.10 2 1 28 2.90 5.20 2 -1 28 8.00 5.40 2 1 -28 6.50 4.50 -2 -1 -28 5.80 4.30 2 -2 -28 14.20 5.70 -2 2 -28 12.80 4.50 2 2 28 21.20 7.30 -2 -2 -28 17.80 5.80 2 -2 28 17.30 6.50 2 2 -28 30.50 6.20 -2 3 -28 67.79 8.20 2 -3 -28 71.29 10.40 2 3 28 57.49 9.80 2 -3 28 80.29 11.40 -2 -3 -28 55.59 8.80 2 -4 -28 27.00 7.40 2 4 28 18.50 7.00 -2 -4 -28 26.70 6.70 2 -4 28 39.30 8.60 2 -5 -28 73.29 11.00 2 5 28 65.29 10.40 2 -5 28 73.99 11.50 -2 -5 -28 88.69 11.10 2 6 28 31.20 8.10 2 -6 -28 17.10 6.70 2 -6 28 26.90 7.60 -2 -6 -28 19.70 6.30 2 -7 -28 42.20 9.10 2 7 28 33.70 8.60 -2 -7 -28 28.70 7.10 2 -8 -28 18.00 7.50 2 8 28 15.30 7.50 -2 -8 -28 11.30 5.70 3 0 28 25.00 7.70 -3 0 -28 23.70 6.00 3 0 -28 30.50 6.90 3 1 28 26.20 7.50 -3 1 -28 23.50 6.00 3 -1 -28 25.70 7.00 3 1 -28 25.20 6.30 3 -1 28 19.30 7.60 -3 -1 -28 28.00 6.60 3 -2 -28 34.00 7.80 3 2 28 63.09 10.70 -3 2 -28 61.19 8.30 -3 -2 -28 40.80 7.50 3 2 -28 51.29 7.90 3 -2 28 59.49 11.90 3 -3 -28 34.80 8.00 3 3 28 51.39 10.20 -3 3 -28 28.40 6.00 -3 -3 -28 48.20 8.30 3 -4 -28 41.30 9.10 3 4 28 35.90 8.80 -3 -4 -28 41.10 8.00 3 5 28 71.29 13.00 3 -5 -28 51.29 9.90 -3 -5 -28 68.39 10.20 3 -6 -28 13.80 6.80 -3 -6 -28 11.00 5.90 0 0 -29 -1.30 3.40 0 -1 -29 134.49 12.70 0 1 -29 118.39 11.30 0 2 -29 7.80 4.10 0 -2 -29 11.70 5.30 0 -3 -29 24.50 6.80 0 -4 -29 2.30 4.50 0 -5 -29 20.40 6.50 0 -6 -29 -6.40 4.20 0 -7 -29 63.69 9.90 0 -7 29 48.30 10.50 -1 0 -29 23.30 5.90 1 0 29 19.50 6.50 1 0 -29 19.20 5.70 1 1 29 85.59 11.30 -1 1 -29 75.69 9.00 1 -1 -29 71.19 9.50 -1 -1 -29 63.49 8.60 1 -1 29 81.69 11.10 1 1 -29 69.29 8.70 -1 2 -29 8.70 4.10 1 -2 -29 7.70 5.10 1 2 -29 10.00 4.40 -1 -2 -29 10.10 4.80 1 -2 29 11.20 6.10 1 -3 -29 94.29 11.10 1 -3 29 88.69 11.60 -1 -3 -29 98.19 11.20 1 -4 -29 18.10 6.30 1 -4 29 9.10 5.80 -1 -4 -29 10.00 5.20 1 -5 -29 18.60 6.50 1 -5 29 19.90 6.90 -1 -5 -29 28.50 7.10 1 -6 -29 0.30 4.40 1 -6 29 1.20 5.00 -1 -6 -29 2.30 4.70 1 -7 -29 3.70 5.00 1 -7 29 -3.60 4.40 -1 -7 -29 4.00 5.60 2 0 29 3.20 5.50 -2 0 -29 13.00 5.40 2 0 -29 14.20 5.40 -2 1 -29 130.19 10.40 2 1 29 108.49 12.90 2 -1 -29 168.08 14.90 2 1 -29 116.19 11.80 2 -1 29 121.69 13.90 -2 -1 -29 120.09 12.00 -2 2 -29 7.30 4.20 2 2 29 8.80 6.10 2 -2 -29 9.10 5.30 2 -2 29 3.20 5.70 -2 -2 -29 13.10 5.60 2 2 -29 11.50 4.70 2 3 29 22.50 7.50 2 -3 -29 8.50 5.70 2 -3 29 10.60 6.90 -2 -3 -29 10.60 5.30 2 -4 -29 -1.40 4.60 2 4 29 5.10 5.60 2 -4 29 -3.60 4.80 -2 -4 -29 -0.90 4.50 2 5 29 59.29 10.20 2 -5 -29 62.89 10.40 -2 -5 -29 59.09 9.40 2 6 29 19.90 7.60 2 -6 -29 22.10 7.80 -2 -6 -29 7.70 5.40 -3 0 -29 9.90 4.90 3 0 -29 2.70 5.10 -3 1 -29 70.19 9.20 3 -1 -29 57.99 9.40 -3 -1 -29 46.90 8.00 3 1 -29 61.89 9.00 3 -2 -29 19.60 6.70 -3 2 -29 22.50 5.80 -3 -2 -29 16.90 5.90 3 2 -29 6.70 4.70 0 0 -30 52.69 8.20 0 -1 -30 -0.60 4.10 0 1 -30 0.20 3.80 0 -2 -30 50.79 8.50 0 -3 -30 29.00 7.20 0 -4 -30 1.20 4.90 0 -5 -30 43.70 8.20 1 0 -30 9.40 4.70 -1 0 -30 5.00 4.20 1 -1 -30 22.20 6.30 -1 1 -30 36.80 6.80 -1 -1 -30 19.70 5.70 1 1 -30 21.40 5.60 1 -2 -30 37.10 7.50 -1 2 -30 24.90 6.50 -1 -2 -30 16.90 5.80 1 -2 30 22.00 7.80 1 -3 -30 10.00 5.50 1 -3 30 11.80 6.20 -1 -3 -30 7.20 4.80 1 -4 -30 91.19 11.20 1 -4 30 77.09 11.40 -1 -4 -30 99.29 11.50 -2 0 -30 14.40 5.70 2 0 -30 16.10 5.90 2 0 30 29.10 8.20 2 1 30 10.90 6.50 2 -1 -30 11.90 5.40 -2 1 -30 9.30 4.80 2 1 -30 7.70 4.60 2 -1 30 0.40 6.20 -2 -1 -30 4.00 4.50 2 2 30 17.20 7.30 -2 2 -30 29.80 6.50 2 -2 -30 31.10 7.70 -2 -2 -30 30.90 7.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 97269 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4814(8) 0.3909(3) 0.4824(2) 0.0272(11) Uani 1 1 d . . . . . H1 H 0.4818 0.4447 0.4987 0.033 Uiso 1 1 calc R U . . . C2 C 0.4830(9) 0.3797(4) 0.4181(2) 0.0333(13) Uani 1 1 d . . . . . H2 H 0.4853 0.4254 0.3912 0.04 Uiso 1 1 calc R U . . . C3 C 0.4814(8) 0.3029(3) 0.3944(2) 0.0312(12) Uani 1 1 d . . . . . H3 H 0.4822 0.2949 0.3508 0.037 Uiso 1 1 calc R U . . . C4 C 0.4784(8) 0.2355(3) 0.4342(2) 0.0281(11) Uani 1 1 d . . . . . C5 C 0.4793(8) 0.2512(3) 0.4977(2) 0.0213(10) Uani 1 1 d . . . . . C6 C 0.4765(8) 0.1524(3) 0.4152(2) 0.0314(13) Uani 1 1 d . . . . . H6 H 0.4745 0.1399 0.3722 0.038 Uiso 1 1 calc R U . . . C7 C 0.4774(9) 0.0909(3) 0.4567(3) 0.0332(13) Uani 1 1 d . . . . . H7 H 0.4779 0.0363 0.4422 0.04 Uiso 1 1 calc R U . . . C8 C 0.4776(9) 0.1061(3) 0.5215(2) 0.0286(12) Uani 1 1 d . . . . . C9 C 0.4789(10) 0.0434(3) 0.5673(3) 0.0383(14) Uani 1 1 d . . . . . H9 H 0.4762 -0.0121 0.555 0.046 Uiso 1 1 calc R U . . . C10 C 0.4839(10) 0.0629(3) 0.6283(3) 0.0402(14) Uani 1 1 d . . . . . H10 H 0.4887 0.0204 0.6581 0.048 Uiso 1 1 calc R U . . . C11 C 0.4822(10) 0.1437(3) 0.6488(2) 0.0318(12) Uani 1 1 d . . . . . H11 H 0.4841 0.1553 0.6919 0.038 Uiso 1 1 calc R U . . . C12 C 0.4779(8) 0.2059(3) 0.6069(2) 0.0248(11) Uani 1 1 d . . . . . C13 C 0.4791(7) 0.1870(3) 0.5428(2) 0.0214(10) Uani 1 1 d . . . . . C14 C 0.4631(9) 0.3191(4) 0.7153(2) 0.0346(13) Uani 1 1 d . . . . . H14A H 0.3719 0.3617 0.7317 0.041 Uiso 1 1 calc R U . . . H14B H 0.4083 0.2654 0.7277 0.041 Uiso 1 1 calc R U . . . C15 C 0.6711(9) 0.3299(4) 0.7431(2) 0.0335(13) Uani 1 1 d . . . . . H15A H 0.7294 0.3818 0.7281 0.04 Uiso 1 1 calc R U . . . H15B H 0.7594 0.2851 0.7287 0.04 Uiso 1 1 calc R U . . . C16 C 0.6676(9) 0.3305(4) 0.8140(2) 0.0344(13) Uani 1 1 d . . . . . H16A H 0.5704 0.3721 0.8285 0.041 Uiso 1 1 calc R U . . . H16B H 0.6211 0.2768 0.8291 0.041 Uiso 1 1 calc R U . . . C17 C 0.8720(11) 0.3485(5) 0.8405(3) 0.0464(18) Uani 1 1 d . . . . . H17A H 0.918 0.4012 0.8233 0.056 Uiso 1 1 calc R U . . . H17B H 0.9665 0.3062 0.8255 0.056 Uiso 1 1 calc R U . . . C18 C 0.8911(11) 0.3527(4) 0.9104(3) 0.0404(17) Uani 1 1 d . . . . . C19 C 0.7394(12) 0.3294(5) 0.9494(3) 0.0508(18) Uani 1 1 d . . . . . H19 H 0.6154 0.3104 0.9328 0.061 Uiso 1 1 calc R U . . . C20 C 0.7653(15) 0.3332(5) 1.0142(3) 0.063(2) Uani 1 1 d . . . . . H20 H 0.6589 0.3171 1.041 0.075 Uiso 1 1 calc R U . . . C21 C 0.9457(16) 0.3604(4) 1.0385(3) 0.065(3) Uani 1 1 d . . . . . H21 H 0.9651 0.3625 1.0821 0.078 Uiso 1 1 calc R U . . . C22 C 1.0936(14) 0.3838(5) 0.9998(4) 0.063(2) Uani 1 1 d . . . . . H22 H 1.2171 0.403 1.0166 0.075 Uiso 1 1 calc R U . . . C23 C 1.0706(12) 0.3806(4) 0.9361(3) 0.051(2) Uani 1 1 d . . . . . H23 H 1.1778 0.3975 0.9099 0.061 Uiso 1 1 calc R U . . . N1 N 0.4793(6) 0.3279(3) 0.52108(16) 0.0220(8) Uani 1 1 d . . . . . Sb1 Sb 0.99192(7) 0.58245(2) 0.70415(2) 0.03516(10) Uani 1 1 d D . . . . F1 F 0.7991(14) 0.5242(6) 0.6568(5) 0.071(3) Uani 0.648(17) 1 d D U P A 1 F2 F 0.860(2) 0.5470(8) 0.7745(5) 0.089(4) Uani 0.648(17) 1 d D U P A 1 F3 F 1.179(2) 0.6370(9) 0.7487(6) 0.112(5) Uani 0.648(17) 1 d D U P A 1 F4 F 1.1114(19) 0.6131(10) 0.6312(5) 0.086(4) Uani 0.648(17) 1 d D U P A 1 F5 F 1.148(2) 0.4888(8) 0.7031(8) 0.072(5) Uani 0.648(17) 1 d D U P A 1 F6 F 0.8150(18) 0.6723(6) 0.6996(6) 0.087(3) Uani 0.648(17) 1 d D U P A 1 F1' F 0.747(2) 0.5391(11) 0.6910(13) 0.083(5) Uani 0.352(17) 1 d D U P A 2 F2' F 0.987(5) 0.5443(12) 0.7853(6) 0.095(7) Uani 0.352(17) 1 d D U P A 2 F3' F 1.260(3) 0.6186(14) 0.7179(12) 0.094(7) Uani 0.352(17) 1 d D U P A 2 F4' F 1.022(4) 0.6147(18) 0.6251(7) 0.088(7) Uani 0.352(17) 1 d D U P A 2 F5' F 1.111(5) 0.4819(13) 0.6841(15) 0.068(7) Uani 0.352(17) 1 d D U P A 2 F6' F 0.892(3) 0.6800(9) 0.7321(11) 0.078(6) Uani 0.352(17) 1 d D U P A 2 Au1 Au 0.47191(3) 0.32641(2) 0.62025(2) 0.02325(5) Uani 1 1 d . . . . . O1 O 0.4594(7) 0.4571(2) 0.6232(2) 0.0380(9) Uani 1 1 d D . . . . H1A H 0.362(9) 0.472(5) 0.646(3) 0.07(3) Uiso 1 1 d D . . . . H1B H 0.566(7) 0.482(4) 0.631(3) 0.05(2) Uiso 1 1 d 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 C1 0.019(3) 0.030(3) 0.033(3) 0.007(2) -0.001(2) 0.002(2) C2 0.018(3) 0.047(4) 0.035(3) 0.013(3) -0.002(2) -0.001(3) C3 0.022(3) 0.049(3) 0.022(2) 0.001(2) 0.000(2) 0.000(2) C4 0.013(2) 0.048(3) 0.024(2) -0.003(2) -0.004(2) 0.001(3) C5 0.012(2) 0.028(3) 0.024(2) -0.001(2) 0.000(2) 0.001(2) C6 0.019(2) 0.046(4) 0.029(3) -0.020(2) -0.003(2) -0.003(3) C7 0.023(3) 0.031(3) 0.045(3) -0.017(3) 0.000(3) 0.004(3) C8 0.018(2) 0.029(3) 0.040(3) -0.007(2) 0.000(2) 0.000(2) C9 0.030(3) 0.032(3) 0.053(4) 0.000(3) 0.001(3) 0.002(3) C10 0.038(3) 0.030(3) 0.053(4) 0.013(3) 0.004(3) 0.000(3) C11 0.027(3) 0.040(3) 0.028(3) 0.007(2) 0.003(3) -0.002(3) C12 0.015(2) 0.032(3) 0.028(3) 0.000(2) -0.001(2) -0.001(2) C13 0.012(2) 0.026(3) 0.026(2) -0.003(2) -0.0026(19) -0.001(2) C14 0.040(3) 0.041(3) 0.023(2) -0.005(2) 0.005(2) 0.002(4) C15 0.035(3) 0.042(4) 0.024(3) -0.003(3) -0.005(2) -0.001(3) C16 0.044(3) 0.030(3) 0.029(3) -0.002(3) 0.001(2) 0.005(3) C17 0.054(4) 0.053(5) 0.031(3) 0.004(3) -0.004(3) -0.009(3) C18 0.061(5) 0.026(4) 0.034(3) 0.000(3) -0.012(3) 0.009(3) C19 0.076(5) 0.047(4) 0.030(3) 0.005(4) -0.004(3) 0.002(4) C20 0.109(7) 0.046(5) 0.034(4) 0.002(4) 0.009(4) 0.010(5) C21 0.112(8) 0.041(4) 0.041(4) -0.011(3) -0.020(5) 0.008(5) C22 0.091(7) 0.047(5) 0.049(5) -0.006(4) -0.034(5) -0.004(4) C23 0.066(5) 0.040(4) 0.046(4) 0.001(3) -0.020(4) -0.004(4) N1 0.0148(18) 0.029(2) 0.0224(19) -0.0001(18) -0.0021(16) 0.001(3) Sb1 0.0396(2) 0.0350(2) 0.03088(18) -0.01185(16) 0.00638(19) -0.00323(19) F1 0.049(5) 0.082(6) 0.082(7) -0.040(5) -0.007(4) -0.020(4) F2 0.103(9) 0.100(7) 0.062(6) 0.012(5) 0.051(6) 0.017(7) F3 0.123(11) 0.121(10) 0.094(9) -0.043(7) -0.047(7) -0.046(8) F4 0.068(8) 0.129(8) 0.061(7) 0.030(6) 0.033(6) -0.012(7) F5 0.063(7) 0.074(8) 0.081(10) 0.004(6) 0.015(7) 0.037(6) F6 0.100(8) 0.054(6) 0.108(9) -0.012(6) 0.002(6) 0.032(6) F1' 0.036(7) 0.085(11) 0.129(14) -0.033(11) 0.011(9) -0.020(7) F2' 0.18(2) 0.073(10) 0.031(7) -0.007(6) 0.036(12) -0.011(16) F3' 0.088(13) 0.095(14) 0.100(16) -0.016(12) -0.031(11) -0.049(11) F4' 0.105(18) 0.120(12) 0.038(8) 0.016(8) -0.027(10) -0.003(14) F5' 0.062(12) 0.054(10) 0.087(18) -0.026(9) 0.008(11) 0.013(8) F6' 0.086(13) 0.036(8) 0.111(15) -0.034(9) 0.030(10) 0.007(8) Au1 0.01943(8) 0.02958(10) 0.02076(8) -0.00296(9) 0.00093(8) -0.00062(9) O1 0.041(2) 0.029(2) 0.044(2) -0.009(2) 0.003(3) 0.001(2) 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' O O 0.0106 0.006 '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 N1 C1 C2 121.3(5) N1 C1 H1 119.3 C2 C1 H1 119.3 C3 C2 C1 119.7(5) C3 C2 H2 120.2 C1 C2 H2 120.2 C2 C3 C4 120.1(5) C2 C3 H3 120 C4 C3 H3 120 C5 C4 C3 117.2(5) C5 C4 C6 117.4(5) C3 C4 C6 125.4(4) N1 C5 C4 122.5(4) N1 C5 C13 115.4(4) C4 C5 C13 122.1(4) C7 C6 C4 121.6(5) C7 C6 H6 119.2 C4 C6 H6 119.2 C6 C7 C8 121.5(5) C6 C7 H7 119.3 C8 C7 H7 119.3 C13 C8 C7 119.2(5) C13 C8 C9 117.2(5) C7 C8 C9 123.7(5) C10 C9 C8 120.1(5) C10 C9 H9 120 C8 C9 H9 120 C9 C10 C11 122.1(5) C9 C10 H10 119 C11 C10 H10 119 C12 C11 C10 120.1(5) C12 C11 H11 120 C10 C11 H11 120 C11 C12 C13 118.9(5) C11 C12 Au1 130.2(4) C13 C12 Au1 110.9(3) C8 C13 C12 121.7(4) C8 C13 C5 118.2(4) C12 C13 C5 120.2(4) C15 C14 Au1 111.2(4) C15 C14 H14A 109.4 Au1 C14 H14A 109.4 C15 C14 H14B 109.4 Au1 C14 H14B 109.4 H14A C14 H14B 108 C14 C15 C16 112.5(5) C14 C15 H15A 109.1 C16 C15 H15A 109.1 C14 C15 H15B 109.1 C16 C15 H15B 109.1 H15A C15 H15B 107.8 C17 C16 C15 111.7(5) C17 C16 H16A 109.3 C15 C16 H16A 109.3 C17 C16 H16B 109.3 C15 C16 H16B 109.3 H16A C16 H16B 107.9 C16 C17 C18 117.7(6) C16 C17 H17A 107.9 C18 C17 H17A 107.9 C16 C17 H17B 107.9 C18 C17 H17B 107.9 H17A C17 H17B 107.2 C19 C18 C23 118.4(6) C19 C18 C17 122.6(7) C23 C18 C17 118.9(7) C18 C19 C20 120.6(8) C18 C19 H19 119.7 C20 C19 H19 119.7 C21 C20 C19 119.8(8) C21 C20 H20 120.1 C19 C20 H20 120.1 C22 C21 C20 119.3(7) C22 C21 H21 120.4 C20 C21 H21 120.4 C21 C22 C23 121.8(8) C21 C22 H22 119.1 C23 C22 H22 119.1 C22 C23 C18 120.1(8) C22 C23 H23 119.9 C18 C23 H23 119.9 C1 N1 C5 119.3(4) C1 N1 Au1 129.6(3) C5 N1 Au1 111.2(3) F4' Sb1 F1' 93.9(9) F3 Sb1 F4 91.4(6) F4' Sb1 F6' 95.4(11) F1' Sb1 F6' 94.1(8) F3 Sb1 F2 92.5(6) F4 Sb1 F2 176.1(6) F3 Sb1 F5 92.0(7) F4 Sb1 F5 88.6(7) F2 Sb1 F5 90.7(6) F4' Sb1 F2' 174.1(11) F1' Sb1 F2' 89.9(10) F6' Sb1 F2' 88.7(8) F4' Sb1 F5' 89.6(12) F1' Sb1 F5' 89.8(11) F6' Sb1 F5' 173.4(11) F2' Sb1 F5' 85.9(11) F3 Sb1 F6 93.8(6) F4 Sb1 F6 90.5(6) F2 Sb1 F6 89.7(5) F5 Sb1 F6 174.1(6) F3 Sb1 F1 179.0(6) F4 Sb1 F1 88.1(5) F2 Sb1 F1 88.0(5) F5 Sb1 F1 87.2(6) F6 Sb1 F1 87.0(5) F4' Sb1 F3' 87.3(9) F1' Sb1 F3' 174.9(9) F6' Sb1 F3' 90.8(9) F2' Sb1 F3' 88.6(10) F5' Sb1 F3' 85.3(11) C12 Au1 C14 95.0(2) C12 Au1 N1 82.35(18) C14 Au1 N1 177.3(2) C12 Au1 O1 173.33(19) C14 Au1 O1 91.6(2) N1 Au1 O1 91.10(17) Au1 O1 H1A 110(6) Au1 O1 H1B 118(5) H1A O1 H1B 112(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.330(6) C1 C2 1.399(7) C1 H1 0.95 C2 C3 1.362(7) C2 H2 0.95 C3 C4 1.401(7) C3 H3 0.95 C4 C5 1.394(6) C4 C6 1.427(7) C5 N1 1.358(6) C5 C13 1.435(6) C6 C7 1.349(7) C6 H6 0.95 C7 C8 1.422(7) C7 H7 0.95 C8 C13 1.406(6) C8 C9 1.427(7) C9 C10 1.357(8) C9 H9 0.95 C10 C11 1.398(7) C10 H10 0.95 C11 C12 1.364(7) C11 H11 0.95 C12 C13 1.417(6) C12 Au1 2.001(5) C14 C15 1.514(8) C14 Au1 2.057(5) C14 H14A 0.99 C14 H14B 0.99 C15 C16 1.530(7) C15 H15A 0.99 C15 H15B 0.99 C16 C17 1.501(9) C16 H16A 0.99 C16 H16B 0.99 C17 C18 1.515(8) C17 H17A 0.99 C17 H17B 0.99 C18 C19 1.367(10) C18 C23 1.391(10) C19 C20 1.410(9) C19 H19 0.95 C20 C21 1.380(12) C20 H20 0.95 C21 C22 1.344(12) C21 H21 0.95 C22 C23 1.385(9) C22 H22 0.95 C23 H23 0.95 N1 Au1 2.141(4) Sb1 F4' 1.797(14) Sb1 F1' 1.797(12) Sb1 F3 1.809(9) Sb1 F4 1.833(8) Sb1 F6' 1.836(12) Sb1 F2 1.845(8) Sb1 F5 1.853(9) Sb1 F2' 1.861(13) Sb1 F5' 1.880(15) Sb1 F6 1.888(8) Sb1 F1 1.895(7) Sb1 F3' 1.896(14) Au1 O1 2.150(4) O1 H1A 0.84(3) O1 H1B 0.84(3)