#------------------------------------------------------------------------------ #$Date: 2024-08-01 04:19:28 +0200 (Thu, 01 Aug 2024) $ #$Revision: 293619 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023219.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023219 loop_ _publ_author_name 'D\"oring, Cindy' 'Jones, Peter G.' _publ_section_title ; Crystal structures of seven gold(III) complexes of the form LAuX 3 (L = substituted pyridine, X = Cl or Br) ; _journal_coeditor_code WM5729 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 894 _journal_page_last 909 _journal_paper_doi 10.1107/S2056989024007266 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Au Cl3 (C7 H9 N)]' _chemical_formula_moiety 'C7 H9 Au Cl3 N' _chemical_formula_sum 'C7 H9 Au Cl3 N' _chemical_formula_weight 410.47 _chemical_name_systematic ; Trichlorido(3,5-dimethylpyridine-\kN)gold(III) ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 112.333(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6240(3) _cell_length_b 15.9360(6) _cell_length_c 9.2538(4) _cell_measurement_reflns_used 6320 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.3340 _cell_measurement_theta_min 3.1490 _cell_volume 1039.97(8) _computing_cell_refinement ; CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2020) ; _computing_data_collection ; CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2020) ; _computing_data_reduction ; CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2020) ; _computing_molecular_graphics ; Bruker XP, Version 5.1 (Bruker, 1998) ; _computing_publication_material ; SHELXL-2019/3 (Sheldrick, 2015) ; _computing_structure_refinement ; SHELXL-2019/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.954 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13810 _diffrn_reflns_theta_full 30.000 _diffrn_reflns_theta_max 30.879 _diffrn_reflns_theta_min 2.556 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 14.862 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.26976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2020) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.261 _refine_diff_density_min -0.880 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 1563 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0161 _refine_ls_R_factor_gt 0.0144 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+1.5857P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0322 _reflns_number_gt 1496 _reflns_number_total 1563 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5729.cif _cod_data_source_block 5 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2023219 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.155 _shelx_estimated_absorpt_t_max 0.588 _shelx_hkl_file ; -10 0 2 24793.3 2305.30 12 -10 0 3-45.8032 395.580 12 -10 0 3 623.287 591.516 4 -10 0 4 42723.3 2901.17 12 -10 0 4 44101.8 3126.66 4 -10 0 5 216.285 420.462 4 -10 0 5 295.595 319.493 12 -10 0 6 68356.1 3881.30 4 -10 0 7 280.801 462.125 4 -10 0 8 69964.2 3874.33 4 -10 -2 2 21901.7 2115.03 12 -10 2 2 18875.0 1974.02 12 -10 2 3-1097.91 651.664 12 -10 2 3 146.068 421.798 4 -10 -2 3-467.390 551.208 4 -10 -2 3 276.178 485.551 12 -10 -2 4 36417.6 2635.58 12 -10 2 4 39693.9 2794.19 12 -10 -2 4 41614.2 2981.91 4 -10 2 4 39441.9 2949.10 4 -10 -2 5 934.710 551.685 12 -10 -2 5 446.215 430.062 4 -10 2 5 1034.63 488.497 12 -10 2 5 758.391 611.433 4 -10 2 6 46002.4 3220.46 4 -10 -2 6 51700.6 3263.02 4 -10 2 7-236.927 562.821 4 -10 -2 7 228.939 486.921 4 -10 2 8 30823.1 2514.91 4 -10 -4 2 13430.1 1660.84 12 -10 4 2 13323.9 1631.03 12 -10 -4 3 4325.45 895.471 12 -10 4 3 4276.00 961.047 12 -10 -4 4 17982.1 1899.44 4 -10 4 4 21125.7 2138.88 4 -10 4 4 25617.6 2182.89 12 -10 -4 4 19702.4 1909.03 12 -10 4 5 6864.42 1111.26 12 -10 4 5 7088.95 1292.15 4 -10 -4 5 6026.56 982.467 12 -10 4 6 33206.7 2723.83 4 -10 4 7 7826.30 1205.08 10 -10 4 7 7040.70 1230.84 4 -10 4 8 30920.7 2573.43 10 -10 4 8 28358.8 2519.28 4 -10 -6 3 8907.04 1338.73 12 -10 6 3 6774.25 1213.71 12 -10 6 4 33871.2 2555.64 12 -10 -6 4 28678.0 2322.74 12 -10 6 5 16494.5 1940.59 6 -10 -6 5 13207.0 1510.53 12 -10 6 7 12723.6 1574.33 10 -10 -8 4 20784.3 1967.04 12 -10 8 4 19502.6 1945.65 12 -10 -8 5 17353.7 1712.91 12 -10 8 7 24064.8 2199.85 10 -9 -1 -2 47045.4 3115.26 4 -9 1 -1 531.441 604.050 6 -9 1 -1 337.675 439.819 12 -9 -1 -1 1328.28 736.263 12 -9 -1 -1 919.804 518.971 4 -9 1 0 45320.1 3113.53 12 -9 1 0 40752.9 2991.28 6 -9 -1 0 43524.1 2970.49 4 -9 -1 0 40888.5 2975.27 12 -9 -1 1 1844.71 657.017 4 -9 1 1 598.358 573.747 12 -9 1 1 621.346 446.711 6 -9 -1 1 1272.09 624.760 12 -9 -1 2 28155.0 2385.57 4 -9 1 2 33158.5 2576.99 4 -9 -1 2 28432.4 2339.04 12 -9 1 2 32439.0 2515.25 12 -9 1 2 34897.8 2671.70 6 -9 1 3 126.944 437.681 12 -9 1 3-653.480 561.106 4 -9 -1 3 665.748 507.033 4 -9 -1 3 90.0552 356.014 12 -9 -1 4 26055.0 2026.51 12 -9 -1 4 22327.4 2036.50 4 -9 1 4 21693.4 2055.69 4 -9 1 4 25411.2 2047.07 12 -9 -1 5-149.735 394.509 4 -9 1 5 551.473 532.958 4 -9 1 5-7.06543 359.153 12 -9 -1 5 602.865 465.809 12 -9 1 6 42104.6 2809.76 4 -9 -1 6 43201.4 2774.06 4 -9 1 7 1508.48 444.062 4 -9 -1 7 2434.81 689.868 4 -9 1 8 65311.1 3469.01 4 -9 -1 8 66621.9 3467.57 4 -9 1 9 276.081 338.345 4 -9 -1 9 91.3741 365.804 4 -9 -1 10 57623.9 3170.93 4 -9 1 10 58988.9 3193.40 4 -9 1 11-469.277 698.605 7 -9 -1 11 1433.09 774.954 7 -9 -3 -2 27579.4 2339.57 4 -9 3 -2 30256.7 2398.37 1 -9 3 -1 1662.38 640.612 6 -9 -3 -1 1600.37 620.735 4 -9 3 0 27179.0 2379.96 6 -9 -3 0 30709.2 2443.85 4 -9 3 0 29878.9 2506.91 12 -9 -3 0 30852.8 2531.33 12 -9 3 1 26.9674 419.987 6 -9 -3 1 1319.92 601.355 4 -9 -3 1 812.881 459.117 12 -9 3 1 621.391 552.779 12 -9 3 2 13882.7 1608.24 12 -9 -3 2 14519.3 1608.35 4 -9 3 2 16103.6 1791.13 6 -9 -3 2 13341.4 1556.98 12 -9 -3 3 805.326 512.232 12 -9 3 3 1349.39 608.411 12 -9 -3 3 817.183 454.754 4 -9 3 3 1217.39 541.472 6 -9 -3 4 19042.6 1690.48 12 -9 3 4 17328.8 1707.68 12 -9 3 4 20677.2 2033.17 4 -9 -3 4 20858.6 1892.67 4 -9 3 5 1807.65 571.111 12 -9 -3 5 3733.65 743.563 12 -9 3 5 1453.11 620.616 4 -9 -3 5 1888.76 687.331 4 -9 3 6 25722.8 2105.92 10 -9 -3 6 26847.5 2122.16 4 -9 3 6 24028.0 2135.97 4 -9 3 7 524.219 480.288 10 -9 -3 7 342.900 352.844 4 -9 3 7 1065.06 538.234 4 -9 3 8 48132.1 3269.51 10 -9 3 8 42525.2 2814.76 4 -9 -3 8 44802.7 2784.40 4 -9 -3 9 2828.58 749.020 4 -9 3 9 1111.37 399.627 4 -9 3 9 1503.37 729.819 10 -9 -3 10 42076.3 2677.41 4 -9 3 11 3376.10 1019.85 7 -9 -5 -1 7755.44 1240.91 4 -9 -5 0 20859.6 1941.22 4 -9 5 0 18862.8 1974.53 12 -9 -5 0 20761.4 2047.96 12 -9 5 0 22904.9 2167.26 6 -9 5 1 6324.04 1147.44 12 -9 5 1 6490.11 1107.14 6 -9 -5 1 5943.20 1068.33 12 -9 -5 1 5321.24 1033.27 4 -9 -5 2 15055.6 1605.67 4 -9 5 2 15376.2 1755.05 6 -9 -5 2 13736.3 1541.63 12 -9 5 2 13376.9 1593.64 12 -9 -5 3 3060.16 722.581 12 -9 -5 3 1763.72 569.635 4 -9 5 3 4057.90 932.969 6 -9 5 3 4299.69 879.461 12 -9 5 4 9680.00 1286.63 12 -9 5 4 9531.54 1379.14 6 -9 -5 4 7884.66 1159.07 4 -9 -5 4 9945.17 1214.47 12 -9 5 5 6443.15 1125.44 6 -9 -5 5 6236.71 917.776 12 -9 -5 5 6603.66 1078.02 4 -9 5 5 5300.39 906.610 10 -9 5 5 6751.64 1052.67 12 -9 5 6 23821.3 2025.68 10 -9 -5 6 22011.0 1914.28 4 -9 5 6 22735.1 2137.29 4 -9 -5 7 8933.63 1214.95 4 -9 5 7 10278.5 1431.99 4 -9 5 7 11427.2 1529.75 10 -9 5 8 38768.9 2871.04 10 -9 -5 8 36347.2 2483.37 4 -9 5 8 32963.8 2528.94 4 -9 5 9 9497.16 1304.63 4 -9 -5 9 11844.3 1381.63 4 -9 -7 -1 11903.8 1467.65 4 -9 -7 0 30398.2 2329.82 4 -9 7 1 13433.4 1608.99 12 -9 7 1 14954.7 1742.76 6 -9 -7 1 11146.6 1462.50 12 -9 -7 1 11548.8 1423.63 4 -9 -7 2 17682.7 1743.86 4 -9 7 2 19597.3 1997.31 6 -9 -7 2 20105.0 1863.09 12 -9 7 2 17652.2 1816.93 12 -9 -7 3 8921.98 1227.71 4 -9 7 3 10654.5 1379.79 12 -9 -7 3 10027.8 1284.85 12 -9 7 3 11778.0 1509.78 6 -9 -7 4 18579.0 1673.46 12 -9 7 4 18700.0 1943.89 6 -9 7 4 18446.1 1760.96 12 -9 -7 4 19390.2 1811.50 4 -9 -7 5 10176.5 1308.40 4 -9 7 5 11292.1 1502.42 6 -9 7 5 9964.91 1274.13 10 -9 -7 5 12710.5 1307.16 12 -9 7 5 10865.8 1329.09 12 -9 7 6 27552.4 2256.92 10 -9 -7 6 31892.1 2302.43 4 -9 7 6 26144.2 2328.10 6 -9 -7 7 24460.5 2038.52 4 -9 7 7 23753.9 2214.64 4 -9 7 7 27024.0 2292.57 10 -9 7 8 42321.9 2979.21 4 -9 -7 8 46870.5 2860.84 4 -9 7 8 44074.5 3108.54 10 -9 -9 0 12139.7 1452.77 4 -9 -9 1 7204.66 1130.47 4 -9 9 2 11457.0 1467.74 12 -9 -9 2 11714.6 1445.62 12 -9 -9 2 10011.2 1307.18 4 -9 9 2 10839.8 1510.72 6 -9 9 3 6220.80 1109.90 12 -9 -9 3 6040.40 1017.81 4 -9 9 3 6932.18 1235.09 6 -9 -9 3 6392.02 1014.32 12 -9 -9 4 16680.3 1703.39 4 -9 9 4 14329.7 1594.71 12 -9 9 4 16803.5 1851.97 6 -9 -9 4 17985.9 1650.99 12 -9 -9 5 10619.0 1331.33 4 -9 9 5 12516.4 1616.56 6 -9 -9 5 12392.1 1301.62 12 -9 9 5 10128.2 1308.89 12 -9 9 6 14549.6 1634.41 10 -9 9 6 15635.1 1790.14 6 -9 -9 6 14957.9 1606.97 4 -9 9 7 16546.8 1856.41 10 -9 9 7 16045.0 1871.82 4 -9 9 8 20017.9 2107.80 10 -9 9 8 17677.8 1936.24 4 -9 -11 1 12039.4 1479.89 4 -9 -11 2 3252.56 799.197 4 -9 -11 3 9229.89 1263.68 12 -9 11 3 8338.85 1319.45 12 -9 -11 4 841.792 493.937 12 -9 11 4 365.521 466.587 6 -9 11 4-23.8645 381.478 12 -9 11 5 13084.3 1655.84 6 -9 11 6 1602.04 662.778 6 -9 11 6 4228.31 1016.90 10 -9 11 7 24025.2 2247.57 10 -8 0 -4 24273.0 2255.59 1 -8 0 -4 27411.5 2325.41 6 -8 0 -3-643.914 499.321 1 -8 0 -3 510.262 757.489 12 -8 0 -3 607.089 500.455 6 -8 0 -2 53183.8 3132.12 1 -8 0 -2 60109.6 3503.33 6 -8 0 -2 56846.8 3502.97 12 -8 0 -1 104.264 378.427 12 -8 0 -1 438.939 409.641 1 -8 0 -1 382.865 513.804 6 -8 0 0 133993. 4971.54 1 -8 0 0 129166. 5516.30 12 -8 0 0 139939. 5717.66 6 -8 0 1 490.660 429.826 12 -8 0 1 100.351 457.620 6 -8 0 2 99540.7 4413.86 4 -8 0 2 89201.1 4200.42 12 -8 0 3 31.8082 408.450 4 -8 0 3 286.703 433.152 12 -8 0 4 54565.7 2880.45 12 -8 0 4 57050.6 3106.74 4 -8 0 5 385.948 380.351 12 -8 0 5-293.841 343.046 4 -8 0 6 36195.3 2009.82 12 -8 0 6 40706.2 2462.19 4 -8 0 7-521.717 396.384 7 -8 0 7 103.879 303.396 4 -8 0 8 74610.8 3709.57 7 -8 0 8 75186.4 4174.10 10 -8 0 9 9.57858 571.673 10 -8 0 9-94.4013 299.988 4 -8 0 9 224.384 654.036 7 -8 0 10 72927.0 4483.73 10 -8 0 10 62901.8 3096.25 4 -8 0 10 70258.7 4139.83 7 -8 0 11-796.513 826.562 7 -8 -2 -4 20625.6 2073.68 1 -8 2 -4 21505.2 2096.56 1 -8 2 -4 21704.4 2069.68 6 -8 -2 -3-431.288 381.642 4 -8 -2 -3-26.4364 375.148 1 -8 2 -3 590.587 420.650 12 -8 2 -3-208.876 439.354 1 -8 2 -3-38.8700 453.326 6 -8 2 -2 50930.4 3212.48 6 -8 -2 -2 43930.2 2862.40 4 -8 -2 -2 48735.2 3227.10 12 -8 -2 -2 49840.3 2940.34 1 -8 2 -2 51603.4 3297.20 12 -8 2 -1 1536.69 636.675 6 -8 -2 -1 667.272 372.159 1 -8 2 -1 1141.95 628.104 12 -8 -2 -1 1447.35 558.625 4 -8 -2 -1 843.038 461.368 12 -8 -2 0 57708.8 3236.41 4 -8 2 0 59447.7 3423.77 12 -8 2 0 57298.3 3376.43 6 -8 -2 0 49744.4 3157.91 12 -8 2 1 853.837 466.162 12 -8 2 1 2327.27 847.331 6 -8 -2 1 1050.80 480.447 12 -8 -2 1 2253.94 746.641 4 -8 -2 2 74521.6 3661.68 12 -8 -2 2 74820.8 3697.80 4 -8 2 2 75286.2 3794.25 12 -8 2 2 77616.5 3955.56 6 -8 -2 3-224.790 427.657 12 -8 -2 3 357.813 346.064 4 -8 2 3 362.414 402.625 6 -8 2 3 3.11083 347.289 12 -8 -2 4 47636.2 2548.77 12 -8 2 4 46695.0 2701.13 12 -8 -2 4 45100.8 2663.91 4 -8 2 4 44967.2 2836.37 4 -8 2 5-126.137 346.179 4 -8 2 5-20.5824 364.839 10 -8 2 5-311.017 356.772 12 -8 -2 5 173.352 347.250 4 -8 -2 5-72.8627 263.109 12 -8 2 6 25631.8 2101.15 10 -8 -2 6 26485.1 1621.46 12 -8 2 6 25867.5 1722.28 12 -8 2 6 26739.6 2052.27 4 -8 -2 6 24563.2 1876.79 4 -8 2 7 460.734 382.082 4 -8 2 7-272.377 363.063 7 -8 2 7-468.567 580.429 10 -8 -2 7 152.654 304.244 4 -8 -2 8 21526.7 1960.40 7 -8 2 8 17093.5 1896.77 10 -8 2 8 17699.8 1569.35 4 -8 2 8 22352.0 1921.50 7 -8 -2 8 19974.2 1653.89 4 -8 2 9 1471.82 733.086 10 -8 -2 9 1302.35 628.265 7 -8 2 9 1614.70 624.125 7 -8 2 9 491.420 366.901 4 -8 -2 9 443.794 281.803 4 -8 2 10 47556.7 3333.22 7 -8 -2 10 45568.1 2593.25 4 -8 -2 10 48367.5 3430.57 7 -8 2 11-428.346 653.374 7 -8 -2 11 787.731 823.046 7 -8 -4 -4 11021.5 1558.15 1 -8 4 -3 7530.44 1265.37 12 -8 -4 -3 4730.44 1038.21 12 -8 -4 -3 4599.81 960.190 1 -8 4 -3 5499.23 1066.31 6 -8 -4 -2 31798.3 2282.90 1 -8 -4 -2 29904.5 2221.90 4 -8 4 -2 32998.3 2558.56 6 -8 -4 -2 27165.9 2357.02 12 -8 4 -2 31861.2 2541.26 12 -8 -4 -1 6419.59 1013.37 4 -8 -4 -1 7189.86 1195.44 12 -8 4 -1 8303.04 1279.29 12 -8 4 -1 7680.85 1233.11 6 -8 -4 0 56795.8 3277.90 12 -8 -4 0 55041.3 3083.26 4 -8 4 0 55630.1 3313.57 6 -8 4 0 57083.9 3333.43 12 -8 -4 1 9285.77 1219.02 12 -8 -4 1 9032.60 1164.32 4 -8 4 1 9177.98 1282.39 6 -8 4 1 9751.34 1313.99 12 -8 4 2 49488.2 2970.85 12 -8 -4 2 48786.4 2800.81 12 -8 4 2 53514.4 3200.48 6 -8 -4 2 46048.9 2742.79 4 -8 -4 3 10985.4 1211.06 12 -8 4 3 10240.8 1356.28 6 -8 -4 3 9923.09 1211.31 4 -8 4 3 9135.13 1194.57 12 -8 4 3 9999.37 1058.13 10 -8 4 4 20350.9 1890.38 6 -8 4 4 19822.5 1616.51 10 -8 -4 4 20752.2 1717.03 4 -8 -4 4 19312.8 1541.91 12 -8 4 4 19753.3 1746.08 12 -8 -4 5 4684.05 711.219 12 -8 -4 5 4614.85 817.812 4 -8 4 5 5793.26 937.235 10 -8 4 5 4310.16 873.825 6 -8 4 5 4529.95 817.128 12 -8 4 6 11941.1 1442.18 4 -8 -4 6 13834.1 1363.47 4 -8 4 6 13799.1 1529.57 10 -8 4 6 14960.1 1363.58 12 -8 -4 6 14616.1 1201.54 12 -8 4 7 4052.02 766.035 7 -8 4 7 5749.46 1108.55 10 -8 4 7 3833.59 826.167 4 -8 -4 7 4111.91 748.573 4 -8 -4 8 17447.3 1575.72 4 -8 4 8 22102.7 1926.93 7 -8 4 8 18466.4 1663.79 4 -8 4 8 20787.0 2063.77 10 -8 4 9 2187.77 578.630 4 -8 -4 9 2508.42 583.418 4 -8 4 9 2799.57 851.351 7 -8 4 9 2810.69 894.055 10 -8 -4 10 29161.7 2046.81 4 -8 4 10 29816.8 2580.70 7 -8 4 10 25770.9 2600.36 10 -8 4 11 10328.7 1617.19 7 -8 -4 11 10357.8 1202.09 4 -8 -6 -4 17720.8 1882.53 1 -8 6 -3 7492.28 1268.01 6 -8 -6 -2 31274.7 2224.17 4 -8 6 -2 34404.9 2617.64 6 -8 -6 -2 36764.1 2691.86 12 -8 6 -2 31659.2 2551.92 12 -8 -6 -1 16965.1 1622.74 4 -8 6 -1 17710.0 1874.18 6 -8 6 -1 18281.3 1909.48 12 -8 -6 -1 20645.4 1935.50 12 -8 -6 0 58816.7 3348.54 12 -8 -6 0 63657.2 3245.78 4 -8 6 0 66068.4 3667.00 6 -8 6 0 63386.7 3554.12 12 -8 -6 1 25888.6 1945.91 4 -8 6 1 26259.0 2190.92 6 -8 -6 1 22198.7 1902.17 12 -8 6 1 23840.0 2059.42 12 -8 -6 2 54912.7 2956.12 4 -8 -6 2 56873.6 3013.09 12 -8 6 2 54531.5 3160.02 12 -8 6 2 54878.5 3256.14 6 -8 6 3 16840.6 1773.28 6 -8 6 3 17198.5 1672.48 12 -8 -6 3 19753.9 1623.11 12 -8 6 3 19690.5 1508.57 10 -8 -6 3 17494.9 1576.58 4 -8 6 4 35728.1 2584.56 6 -8 -6 4 38928.0 2261.35 12 -8 -6 4 37009.7 2328.50 4 -8 6 4 41612.2 2395.46 10 -8 6 4 41340.6 2560.68 12 -8 6 5 13670.0 1389.86 12 -8 6 5 11532.7 1429.93 6 -8 -6 5 11656.4 1114.63 12 -8 6 5 12913.8 1383.62 10 -8 -6 5 11636.6 1259.04 4 -8 6 6 20323.5 1875.15 6 -8 -6 6 19592.7 1416.59 12 -8 6 6 18112.3 1753.33 10 -8 -6 6 16600.8 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434.860 8 3 -3 -9 610.135 362.210 8 3 -3 -9 1406.32 400.581 1 3 3 -9 1162.66 481.778 11 3 -3 -9 467.902 384.096 11 3 3 -8 38940.1 1646.36 1 3 3 -8 37974.6 1946.81 8 3 -3 -8 38217.0 2002.02 8 3 -3 -8 38606.4 1747.13 1 3 3 -8 34961.4 2137.90 11 3 -3 -8 36148.1 2083.02 11 3 3 -7 624.628 281.087 8 3 -3 -7 673.683 326.427 8 3 3 -7 586.912 209.156 1 3 3 -7 338.256 292.139 11 3 -3 -7 970.220 411.012 11 3 -3 -7 1039.75 286.630 1 3 3 -6 92475.5 3203.18 8 3 -3 -6 95398.8 3253.35 8 3 3 -6 99489.3 2719.77 1 3 -3 -6 98995.8 2945.17 1 3 3 -6 99984.9 2465.34 12 3 3 -6 96639.2 3651.55 11 3 -3 -6 100983. 3480.34 11 3 3 -5 16504.6 1032.75 8 3 -3 -5 15346.0 994.726 8 3 3 -5 16822.7 661.350 1 3 -3 -5 15607.0 817.510 1 3 3 -5 17141.6 694.477 12 3 3 -5 16175.3 1229.81 11 3 -3 -5 17225.8 1131.56 11 3 -3 -4 269803. 6408.40 1 3 3 -4 260722. 5934.11 1 3 3 -4 266098. 6897.13 8 3 -3 -4 280391. 6824.12 8 3 3 -4 290823. 6365.33 12 3 3 -4 249963. 7383.45 11 3 -3 -4 286816. 7040.83 11 3 3 -3 24067.2 1303.82 8 3 -3 -3 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567.719 9 3 -3 3 4317.25 637.662 5 3 3 3 4200.25 683.396 5 3 3 3 4564.90 433.802 7 3 3 3 3762.24 575.493 14 3 -3 3 4440.52 511.392 14 3 3 3 3737.92 496.717 13 3 -3 3 3868.69 598.157 13 3 -3 3 4776.65 667.181 2 3 -3 4 52943.5 2464.24 5 3 3 4 54178.5 2546.09 5 3 3 4 54586.3 2440.42 14 3 -3 4 54701.5 2090.90 14 3 -3 4 53086.2 2503.39 13 3 3 4 56727.1 2002.46 7 3 3 4 53807.0 2109.12 13 3 -3 4 55584.9 2586.73 2 3 3 4 61773.1 2238.10 10 3 3 4 53040.1 1650.29 9 3 -3 4 56114.0 2236.98 9 3 -3 5 3678.47 500.241 9 3 -3 5 3396.21 651.051 5 3 3 5 2981.20 593.730 5 3 -3 5 3885.55 532.566 14 3 3 5 4263.77 699.358 14 3 3 5 3775.88 516.855 13 3 -3 5 3701.85 654.178 13 3 3 5 3939.69 513.545 7 3 -3 5 3807.92 732.620 2 3 3 5 3834.40 498.328 10 3 3 6 52018.0 2562.64 14 3 3 6 51595.1 2174.54 7 3 3 6 52800.6 2241.52 13 3 -3 6 48996.0 2520.80 13 3 -3 6 52229.5 2079.96 9 3 -3 6 47530.4 2543.90 5 3 3 6 46186.3 2575.78 5 3 -3 7 1528.63 554.154 5 3 3 7 831.076 453.870 5 3 3 7 1832.87 521.204 14 3 3 7 1633.36 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8 9 9 -4 14703.0 1763.95 3 9 9 -4 17810.9 2138.55 11 9 -9 -3 6719.31 1157.91 8 9 9 -3 8413.64 1457.04 5 9 9 -3 5600.44 1188.30 14 9 9 -3 4970.28 1051.86 3 9 -9 -3 5970.78 1208.10 13 9 9 -3 5611.09 1349.02 11 9 -9 -2 11559.8 1583.26 9 9 -9 -2 10170.1 1344.74 5 9 9 -2 7164.48 1270.94 5 9 9 -2 11684.1 1700.54 14 9 -9 -2 9058.75 1412.72 13 9 -9 -1 8651.33 1209.14 5 9 9 -1 6506.37 1288.05 5 9 11 -7 19725.4 2388.88 8 9 -11 -7 21230.3 2113.04 8 9 -11 -7 22000.8 2112.36 11 9 11 -6 4142.03 1084.47 8 9 -11 -6 5373.32 1129.44 8 9 11 -5 11961.3 1793.99 8 9 11 -5 11513.7 1690.47 3 9 11 -4 1123.05 704.248 3 9 11 -3 9042.17 1538.39 5 9 11 -3 6945.68 1232.92 3 9 11 -2 4006.91 1008.89 5 9 13 -4 7498.25 1452.10 5 9 13 -3 16410.4 2085.33 5 10 0 -7-964.266 649.971 11 10 0 -6 64783.1 4293.44 8 10 0 -6 74089.9 4263.24 11 10 0 -5-159.702 533.176 8 10 0 -5-386.529 501.888 11 10 0 -4 47620.2 3472.08 8 10 0 -4 48230.9 3267.36 11 10 0 -3 64.5628 484.108 8 10 0 -3 238.101 407.418 11 10 0 -2 27643.1 2380.69 11 10 0 -1 60.3304 484.120 13 10 0 -1-364.716 548.375 11 10 -2 -7 1106.82 763.671 11 10 2 -6 49884.1 3756.35 8 10 -2 -6 48896.3 3694.80 8 10 2 -6 59574.3 3805.65 11 10 -2 -6 58295.3 3711.02 11 10 2 -5 168.806 583.852 8 10 -2 -5 858.783 629.197 8 10 2 -5 1147.04 727.184 11 10 -2 -5 352.115 468.552 11 10 2 -4 43668.3 3322.69 8 10 -2 -4 41890.2 3226.54 8 10 2 -4 43485.6 3141.06 11 10 -2 -4 43189.6 3029.59 11 10 2 -3-374.430 520.017 8 10 -2 -3-104.827 491.197 8 10 2 -3 260.514 480.717 11 10 -2 -3 400.546 495.731 11 10 -2 -2 17944.9 1938.94 5 10 -2 -2 18714.6 2019.07 13 10 2 -2 21228.8 2115.56 11 10 -2 -2 17868.1 1861.18 11 10 2 -1-108.866 490.751 13 10 -2 0 6726.94 1090.80 14 10 2 0 6541.73 1140.88 13 10 -4 -7 6501.97 1317.08 11 10 -4 -6 33862.8 3013.48 8 10 -4 -6 39718.6 2984.54 11 10 4 -5 8158.23 1567.73 8 10 -4 -5 4442.33 1122.97 8 10 4 -5 5737.07 1101.82 3 10 4 -5 6695.50 1285.98 11 10 -4 -5 5611.31 1136.77 11 10 -4 -4 22415.9 2302.73 8 10 4 -4 21447.1 2232.01 11 10 -4 -4 17022.8 1850.10 11 10 -4 -3 4730.19 1074.05 8 10 4 -3 5705.78 1244.61 11 10 -4 -3 4673.90 926.685 11 10 -4 -2 10684.8 1500.04 5 10 -6 -6 31962.1 2873.72 8 10 6 -6 34483.8 2783.34 3 10 -6 -6 33977.8 2725.35 11 10 -6 -5 11598.3 1704.61 8 10 6 -5 15681.4 1776.36 3 10 -6 -5 11845.7 1596.70 11 10 -6 -4 33979.1 2838.47 8 10 -6 -4 33550.8 2587.92 11 10 -6 -3 7905.65 1347.78 8 10 -6 -3 8344.15 1352.04 5 10 -6 -2 14106.8 1670.39 5 10 -8 -6 26789.9 2355.55 11 10 -8 -5 16329.2 2058.76 8 10 8 -5 19924.9 2066.67 3 10 -8 -4 16436.2 1924.00 8 10 -8 -3 9054.48 1408.19 8 10 -8 -3 7419.21 1281.82 5 0 0 0 0.00 0.00 0 TITL Bath in Cc REM Cc (#9 in standard setting) CELL 0.71073 7.624028 15.935992 9.253792 90.0000 112.3331 90.0000 ZERR 4.00 0.000164 0.000278 0.000191 0.0000 0.0024 0.0000 LATT -7 SYMM x,-y, z+1/2 SFAC C H N Cl Au UNIT 28.00 40.00 4.00 16.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 56447 _shelx_res_file ; TITL Bath in C2/c shelx.res created by SHELXL-2019/3 at 09:38:52 on 11-Jun-2024 CELL 0.71073 7.6240 15.9360 9.2538 90.000 112.333 90.000 ZERR 4 0.0003 0.0006 0.0004 0.000 0.005 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N Cl Au UNIT 28 36 4 12 4 L.S. 6 FMAP 2 PLAN 10 SIZE 0.20 0.12 0.04 TEMP -173 ACTA 60 BOND $H CONF 2.3 OMIT 1 1 3 EQIV $1 -x+1, -y+1, -z+1 EQIV $2 x, -y+1, z+1/2 EQIV $3 x-1/2, y+1/2, z EQIV $4 -x+3/2, y+1/2, -z+3/2 EQIV $5 -x+2, y, -z+3/2 HTAB C12 Cl1_$1 HTAB C17 Cl1_$1 HTAB C14 Cl2_$3 HTAB C14 Cl2_$4 RTAB DIST Au1 Cl2_$1 RTAB DIST Au1 Cl2_$2 RTAB DIST Cl1 Cl2_$1 RTAB ANGL Au1 Cl1 Cl2_$1 RTAB DIST Cl1 Cl2_$2 RTAB ANGL Au1 Cl1 Cl2_$2 RTAB DIST Cl2 CL2_$1 RTAB ANGL Au1 Cl2 Cl2_$1 RTAB DIST Cl2 Cl2_$5 RTAB ANGL Au1 Cl2 Cl2_$5 WGHT 0.014400 1.585700 FVAR 1.84453 AU1 5 0.500000 0.514477 0.750000 10.50000 0.01446 0.00766 = 0.00989 0.00000 0.00535 0.00000 CL1 4 0.500000 0.371931 0.750000 10.50000 0.03106 0.00914 = 0.01465 0.00000 0.01110 0.00000 CL2 4 0.748319 0.515032 0.668828 11.00000 0.01887 0.01402 = 0.02224 0.00121 0.01281 0.00270 N11 3 0.500000 0.642328 0.750000 10.50000 0.01343 0.01006 = 0.01169 0.00000 0.00391 0.00000 C12 1 0.496595 0.684103 0.621798 11.00000 0.01570 0.01213 = 0.01213 0.00062 0.00614 -0.00035 AFIX 43 H12 2 0.493575 0.653448 0.532835 11.00000 -1.20000 AFIX 0 C13 1 0.497451 0.771074 0.618416 11.00000 0.01340 0.01373 = 0.01736 0.00440 0.00609 0.00063 C14 1 0.500000 0.814239 0.750000 10.50000 0.01286 0.00991 = 0.02103 0.00000 0.00456 0.00000 AFIX 43 H14 2 0.500001 0.873853 0.750001 10.50000 -1.20000 AFIX 0 C17 1 0.497795 0.816919 0.475518 11.00000 0.02388 0.01670 = 0.02178 0.00534 0.00979 0.00029 AFIX 137 H17A 2 0.626920 0.818020 0.476847 11.00000 -1.50000 H17B 2 0.452929 0.874520 0.475849 11.00000 -1.50000 H17C 2 0.413758 0.787938 0.381216 11.00000 -1.50000 AFIX 0 HKLF 4 REM Bath in C2/c REM wR2 = 0.0322, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0144 for 1496 Fo > 4sig(Fo) and 0.0161 for all 1563 data REM 58 parameters refined using 0 restraints END WGHT 0.0144 1.5857 REM Highest difference peak 1.261, deepest hole -0.880, 1-sigma level 0.139 Q1 1 0.6330 0.5190 0.7186 11.00000 0.05 1.26 Q2 1 0.5227 0.5110 0.8526 11.00000 0.05 1.09 Q3 1 0.5987 0.5128 0.7799 11.00000 0.05 0.72 Q4 1 0.5847 0.5750 0.7787 11.00000 0.05 0.63 Q5 1 0.4814 0.7908 0.5404 11.00000 0.05 0.53 Q6 1 0.4865 0.7893 0.6790 11.00000 0.05 0.49 Q7 1 0.7582 0.4376 0.5199 11.00000 0.05 0.48 Q8 1 0.4549 0.4838 0.5582 11.00000 0.05 0.47 Q9 1 0.7973 0.5189 0.7809 11.00000 0.05 0.45 Q10 1 0.4979 0.5582 0.5790 11.00000 0.05 0.44 ; _shelx_res_checksum 57487 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au Au1 0.500000 0.51448(2) 0.750000 0.01045(4) Uani d 1 . . Cl Cl1 0.500000 0.37193(5) 0.750000 0.01757(16) Uani d 1 . . Cl Cl2 0.74832(9) 0.51503(3) 0.66883(7) 0.01690(12) Uani d 1 . . N N11 0.500000 0.64233(17) 0.750000 0.0120(5) Uani d 1 . . C C12 0.4966(3) 0.68410(14) 0.6218(3) 0.0131(4) Uani d 1 . . H H12 0.493575 0.653448 0.532835 0.016 Uiso calc 1 . . C C13 0.4975(3) 0.77107(15) 0.6184(3) 0.0148(4) Uani d 1 . . C C14 0.500000 0.8142(2) 0.750000 0.0152(6) Uani d 1 . . H H14 0.500001 0.873853 0.750001 0.018 Uiso calc 1 . . C C17 0.4978(4) 0.81692(16) 0.4755(3) 0.0205(5) Uani d 1 . . H H17A 0.626920 0.818020 0.476847 0.031 Uiso calc 1 . . H H17B 0.452929 0.874520 0.475849 0.031 Uiso calc 1 . . H H17C 0.413758 0.787938 0.381216 0.031 Uiso calc 1 . . 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 0.01446(7) 0.00766(7) 0.00989(6) 0.000 0.00535(5) 0.000 Cl1 0.0311(5) 0.0091(3) 0.0146(4) 0.000 0.0111(3) 0.000 Cl2 0.0189(3) 0.0140(3) 0.0222(3) 0.00270(19) 0.0128(2) 0.0012(2) N11 0.0134(13) 0.0101(13) 0.0117(13) 0.000 0.0039(10) 0.000 C12 0.0157(11) 0.0121(10) 0.0121(10) -0.0004(8) 0.0061(9) 0.0006(8) C13 0.0134(11) 0.0137(11) 0.0174(11) 0.0006(8) 0.0061(9) 0.0044(9) C14 0.0129(15) 0.0099(14) 0.0210(17) 0.000 0.0046(13) 0.000 C17 0.0239(13) 0.0167(12) 0.0218(13) 0.0003(9) 0.0098(11) 0.0053(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 N11 Au1 Cl1 . . 180.0 y N11 Au1 Cl2 . . 89.779(14) y Cl1 Au1 Cl2 . . 90.221(14) y N11 Au1 Cl2 . 2_656 89.779(14) ? Cl1 Au1 Cl2 . 2_656 90.221(14) ? Cl2 Au1 Cl2 . 2_656 179.56(3) y C12 N11 C12 . 2_656 121.0(3) y C12 N11 Au1 . . 119.50(14) ? C12 N11 Au1 2_656 . 119.50(14) ? N11 C12 C13 . . 120.9(2) ? N11 C12 H12 . . 119.6 ? C13 C12 H12 . . 119.6 ? C12 C13 C14 . . 118.2(2) ? C12 C13 C17 . . 120.3(2) ? C14 C13 C17 . . 121.5(2) ? C13 C14 C13 . 2_656 120.8(3) ? C13 C14 H14 . . 119.6 ? C13 C14 H14 2_656 . 119.6 ? C13 C17 H17A . . 109.5 ? C13 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C13 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? 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 N11 . 2.037(3) y Au1 Cl1 . 2.2716(8) y Au1 Cl2 . 2.2867(6) y Au1 Cl2 2_656 2.2867(6) ? N11 C12 . 1.352(3) y N11 C12 2_656 1.352(3) ? C12 C13 . 1.386(3) ? C12 H12 . 0.9500 ? C13 C14 . 1.392(3) ? C13 C17 . 1.512(3) ? C14 H14 . 0.9500 ? C17 H17A . 0.9800 ? C17 H17B . 0.9800 ? C17 H17C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C12 H12 Cl1 5_666 0.95 2.67 3.564(2) 157.7 yes C17 H17C Cl1 5_666 0.98 3.00 3.666(3) 126.2 ? C14 H14 Cl2 3_455 0.95 2.87 3.659(3) 141.7 yes C14 H14 Cl2 4_656 0.95 2.87 3.659(3) 141.7 yes 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 Cl2 Au1 N11 C12 . . . . 51.15(11) y Cl2 Au1 N11 C12 2_656 . . . -128.85(11) ? Cl2 Au1 N11 C12 . . . 2_656 -128.85(11) y Cl2 Au1 N11 C12 2_656 . . 2_656 51.15(11) ? C12 N11 C12 C13 2_656 . . . 0.32(16) ? Au1 N11 C12 C13 . . . . -179.68(16) ? N11 C12 C13 C14 . . . . -0.6(3) ? N11 C12 C13 C17 . . . . 178.70(19) ? C12 C13 C14 C13 . . . 2_656 0.31(15) ? C17 C13 C14 C13 . . . 2_656 -179.0(3) ?