#------------------------------------------------------------------------------
#$Date: 2024-02-05 13:07:49 +0100 (Mon, 05 Feb 2024) $
#$Revision: 289690 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022967.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_2022967
loop_
_publ_author_name
'Upmann, Daniel'
'Jones, Peter G.'
'Bockfeld, Dirk'
'Târcoveanu, Eliza'
_publ_section_title
;
Crystal structures of sixteen phosphane chalcogenide complexes of gold(I)
chloride, bromide and iodide.
;
_journal_coeditor_code YZ2044
_journal_issue 'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 34
_journal_page_last 49
_journal_paper_doi 10.1107/S2056989023010459
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Au Cl (C12 H27 P S)]'
_chemical_formula_moiety 'C12 H27 Au Cl P S'
_chemical_formula_sum 'C12 H27 Au Cl P S'
_chemical_formula_weight 466.78
_chemical_name_systematic
;
Chlorido(tri-tert-butylphosphane sulfide-\kS)gold
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 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 93.583(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.45319(17)
_cell_length_b 10.9040(3)
_cell_length_c 8.7166(2)
_cell_measurement_reflns_used 9477
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.7049
_cell_measurement_theta_min 2.3364
_cell_volume 801.87(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
Bruker XP (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 0.990
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0358
_diffrn_reflns_av_unetI/netI 0.0307
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 22238
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.774
_diffrn_reflns_theta_min 2.341
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 9.546
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.70708
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.933
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 452
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.618
_refine_diff_density_min -0.750
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.493(8)
_refine_ls_extinction_coef 0.00088(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/3 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 156
_refine_ls_number_reflns 4617
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0214
_refine_ls_R_factor_gt 0.0188
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0324
_refine_ls_wR_factor_ref 0.0332
_reflns_number_gt 4382
_reflns_number_total 4617
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2044sup1.cif
_cod_data_source_block 4a
_cod_depositor_comments
'Adding full bibliography for 2022965--2022980.cif.'
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2022967
_cod_database_fobs_code 2022967
_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 0.394
_shelx_estimated_absorpt_t_max 0.701
_shelx_hkl_file
;
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0 -14 -2 1902.93 334.960 12
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-10 4 3 5004.75 497.635 5
10 4 -3 4226.14 467.835 15
10 4 -3 4643.28 501.941 7
-10 4 2 468.180 211.255 10
-10 4 2 287.087 191.633 5
10 4 -2 589.055 245.021 15
10 4 -2 755.751 257.906 7
-10 4 1 6054.38 518.864 5
-10 4 1 5932.16 517.791 10
10 4 -1 6268.70 572.522 15
10 4 -1 6864.77 599.652 7
-10 4 0 2845.24 369.476 10
-10 4 0 3172.29 373.068 5
-10 4 0 3039.32 332.072 8
10 4 0 3055.66 425.155 15
10 4 0 3412.87 453.256 7
-10 4 -1 582.957 185.682 10
-10 4 -1 377.936 178.711 5
-10 4 -1 163.617 142.989 8
10 4 1 369.604 196.423 15
10 4 1 1054.28 289.717 7
-10 4 -2 13117.9 761.124 5
-10 4 -2 13290.7 796.675 10
-10 4 -2 13466.8 739.904 8
10 4 2 14003.1 877.221 15
10 4 2 13398.8 865.256 7
-10 4 -3 4981.97 471.388 11
-10 4 -3 5159.12 510.230 10
-10 4 -3 4393.72 450.711 5
-10 4 -3 4598.36 445.264 8
10 4 3 3942.14 477.333 15
10 4 3 4603.61 512.558 7
-10 4 -3 4522.80 469.077 3
-10 4 -4 742.381 228.484 11
-10 4 -4 477.517 217.180 3
-10 4 -4 164.303 155.653 10
-10 4 -4 647.949 209.994 5
-10 4 -4 205.480 143.877 8
10 4 4 497.805 239.721 15
10 4 4 774.969 262.648 7
-10 4 -5 2959.17 409.386 11
-10 4 -5 2277.62 351.308 5
-10 5 6 1717.63 352.441 10
-10 5 5 7026.44 624.314 10
-10 5 5 6252.36 602.961 5
10 5 -5 7427.31 610.475 15
10 5 -5 8391.03 679.515 7
-10 5 4 615.954 223.629 10
-10 5 4 400.576 205.040 5
10 5 -4 117.761 177.044 15
10 5 -4 319.936 242.938 7
-10 5 3 4486.31 467.398 10
-10 5 3 3879.19 446.465 5
10 5 -3 4538.10 496.625 15
10 5 -3 4775.22 519.683 7
-10 5 2 11483.8 750.673 5
-10 5 2 11185.0 726.096 10
10 5 -2 11600.3 789.109 15
10 5 -2 12985.1 856.651 7
-10 5 1 1063.78 253.790 10
-10 5 1 954.880 225.900 5
10 5 -1 549.472 216.727 15
10 5 -1 1246.20 319.331 7
-10 5 0 1997.43 322.427 10
-10 5 0 2068.43 318.693 5
10 5 0 2117.12 367.478 15
10 5 0 2126.69 358.555 7
-10 5 -1 11460.3 724.145 5
-10 5 -1 9811.58 670.332 10
10 5 1 10377.6 769.395 15
10 5 1 9682.12 747.364 7
-10 5 -2 637.048 192.049 10
-10 5 -2 924.589 238.164 5
10 5 2 653.363 256.644 15
10 5 2 842.654 265.636 7
-10 5 -3 6577.67 567.720 5
-10 5 -3 6504.48 570.704 10
10 5 3 6052.17 604.847 15
10 5 3 6602.63 623.139 7
-10 5 -3 6386.55 544.644 11
-10 5 -4 2503.74 371.460 11
-10 5 -4 2630.93 384.641 10
-10 5 -4 3068.49 406.254 5
-10 5 -5 252.114 175.057 5
10 6 -5-80.4529 179.232 7
-10 6 4 6114.14 554.086 10
-10 6 4 5579.23 554.782 5
10 6 -4 5043.40 530.826 15
10 6 -4 5494.77 583.097 7
-10 6 3 3854.55 433.115 10
-10 6 3 4734.39 513.153 5
10 6 -3 4924.09 529.013 15
10 6 -3 5826.34 593.660 7
-10 6 2 440.156 196.760 10
-10 6 2 569.355 235.301 5
10 6 -2 796.512 256.414 15
10 6 -2 1153.79 287.383 7
-10 6 1 5957.75 547.632 5
-10 6 1 5107.30 476.685 10
10 6 -1 6361.65 612.183 15
10 6 -1 6175.28 605.823 7
-10 6 0 4299.91 439.842 10
-10 6 0 3128.04 398.820 5
10 6 0 4086.51 491.673 15
10 6 0 3156.47 457.818 7
-10 6 -1 672.568 219.444 10
-10 6 -1 599.660 212.904 5
10 6 1 1747.63 364.353 15
10 6 1 1038.12 283.696 7
-10 6 -2 13229.4 811.057 5
-10 6 -2 11031.7 724.751 10
10 6 2 11605.2 852.338 7
-10 6 -3 3777.52 437.040 10
-10 6 -3 4002.81 466.471 5
-10 6 -4 742.150 230.981 10
-10 6 -4 157.090 150.792 11
10 7 -4 707.416 258.563 15
10 7 -3 4180.60 505.968 15
-10 7 2 10557.7 748.505 5
10 7 -2 10408.6 790.243 15
-10 7 1 586.830 211.754 5
10 7 -1 595.566 249.007 15
-10 7 0 1863.15 326.660 5
-10 7 -1 7274.75 618.515 5
-10 7 -1 7249.93 571.378 10
-10 7 -2 268.448 148.512 10
-10 7 -3 4584.47 472.616 10
-11 -6 3 3136.94 423.890 14
11 -6 -3 3315.92 440.194 12
-11 -5 3 2703.03 390.123 14
11 -4 -5 2339.79 365.199 7
-11 -4 4 15.2651 151.983 14
11 -4 -4 284.577 221.382 7
-11 -4 3 7282.43 606.370 14
11 -4 -3 8283.24 666.493 7
11 -4 -2 9231.76 715.845 7
11 -3 -5 1716.64 304.743 7
11 -3 -4 6407.11 591.932 15
11 -3 -4 6862.83 597.942 7
-11 -3 4 5786.32 563.091 14
11 -3 -3 3874.23 465.663 15
-11 -3 3 3245.43 417.570 14
11 -3 -3 4401.52 501.698 7
-11 -3 2 1930.14 366.392 10
-11 -3 2 2329.21 372.640 8
11 -3 -2 2196.03 372.555 15
11 -3 -2 2203.01 348.033 7
-11 -3 1 10261.6 758.419 10
-11 -3 1 10717.1 753.112 8
11 -3 -1 10553.0 768.225 15
11 -3 -1 10650.5 762.505 7
-11 -3 0 77.4393 151.387 10
11 -3 0-49.3898 181.450 15
11 -3 0 472.723 239.359 7
11 -2 -5 1866.00 333.618 15
11 -2 -5 1868.16 338.028 7
11 -2 -4-70.6122 159.451 15
-11 -2 4 345.888 224.519 14
11 -2 -4-195.697 183.410 7
-11 -2 3 7192.25 628.154 8
11 -2 -3 6577.05 587.735 15
-11 -2 3 6418.42 560.896 14
11 -2 -3 6257.23 572.240 7
-11 -2 2 9978.98 746.124 10
-11 -2 2 10315.6 740.891 8
11 -2 -2 9613.41 717.411 15
11 -2 -2 10905.5 766.736 7
-11 -2 2 9859.69 664.315 14
-11 -2 1 211.500 178.730 10
-11 -2 1 182.638 177.532 8
11 -2 -1 26.6865 182.242 15
11 -2 -1-101.253 208.281 7
-11 -2 0 8064.86 649.143 10
-11 -2 0 7477.85 628.952 8
11 -2 0 6882.76 620.257 15
11 -2 0 7591.50 642.912 7
-11 -2 -1 6177.19 575.361 10
-11 -2 -1 6348.78 585.425 8
11 -2 1 4619.10 513.181 15
11 -2 1 4929.77 528.265 7
11 -1 -5 2417.56 366.712 15
11 -1 -5 1983.98 338.377 7
-11 -1 4 3808.40 479.888 8
11 -1 -4 3323.05 426.168 15
-11 -1 4 3535.39 438.448 14
11 -1 -4 3624.88 434.005 7
-11 -1 3 3682.74 471.282 10
-11 -1 3 2248.95 367.482 8
11 -1 -3 2334.75 356.619 15
-11 -1 3 2258.53 355.268 14
11 -1 -3 2514.75 375.353 7
-11 -1 2 1995.82 345.171 10
-11 -1 2 1455.80 305.211 8
11 -1 -2 2152.77 354.473 15
-11 -1 2 1653.61 289.398 14
11 -1 -2 1316.31 311.390 7
-11 -1 1 6647.45 602.999 10
-11 -1 1 6843.34 585.020 8
11 -1 -1 6988.14 606.817 15
11 -1 -1 7161.29 617.223 7
-11 -1 0 480.487 216.142 10
-11 -1 0 336.642 198.940 8
11 -1 0 551.134 241.726 15
11 -1 0 195.773 178.454 7
-11 -1 -1 4167.05 485.861 10
-11 -1 -1 3053.90 395.766 8
11 -1 1 2811.32 411.333 15
11 -1 1 3407.15 427.309 7
-11 -1 -2 9544.84 718.959 8
11 -1 2 9855.45 742.573 15
-11 0 5 1522.77 325.446 8
11 0 -5 1841.91 322.381 15
11 0 -5 1121.47 255.147 7
-11 0 4-107.431 165.342 8
11 0 -4 331.658 218.297 15
-11 0 4 100.979 147.529 14
11 0 -4-76.8123 152.681 7
-11 0 3 6518.08 608.445 10
-11 0 3 5791.69 556.054 8
11 0 -3 6028.95 562.666 15
11 0 -3 6368.82 579.287 7
-11 0 3 6683.60 578.564 14
-11 0 2 4950.53 528.721 10
-11 0 2 5040.42 504.757 8
11 0 -2 5444.83 541.806 15
11 0 -2 5267.27 531.454 7
-11 0 1 204.344 201.320 10
-11 0 1 125.792 175.422 8
11 0 -1 361.162 210.776 15
11 0 -1-221.786 207.049 7
-11 0 0 4872.67 513.062 10
-11 0 0 4722.73 485.610 8
11 0 0 5605.58 556.144 15
11 0 0 4681.07 508.591 7
-11 0 -1 4689.84 511.401 10
-11 0 -1 6015.62 546.084 8
11 0 1 5092.11 532.362 15
11 0 1 6111.79 569.727 7
-11 0 -2 210.072 172.160 8
11 0 2-185.033 211.410 15
11 0 2-331.770 205.164 7
-11 0 -3 4348.99 442.017 3
-11 0 -3 4324.56 486.639 8
-11 0 -4 3168.56 405.305 3
-11 1 5 2242.76 381.989 8
11 1 -5 2372.98 365.689 15
11 1 -5 2392.83 364.701 7
-11 1 4 3679.69 449.529 8
11 1 -4 3801.83 444.991 15
11 1 -4 4098.42 483.404 7
-11 1 3 2449.37 384.022 10
-11 1 3 2783.44 390.254 8
11 1 -3 2558.98 379.287 15
11 1 -3 3051.12 416.383 7
-11 1 2 1928.27 353.786 10
-11 1 2 1710.52 292.500 8
11 1 -2 1370.41 305.285 15
11 1 -2 1672.55 339.706 7
-11 1 1 7638.19 628.195 10
-11 1 1 6791.58 566.076 8
11 1 -1 7493.85 629.284 15
11 1 -1 8380.65 676.732 7
-11 1 0 106.687 167.109 10
-11 1 0 466.175 219.233 8
11 1 0 197.565 181.460 15
11 1 0 213.878 180.669 7
-11 1 -1 3398.63 437.192 10
-11 1 -1 2848.49 379.421 8
11 1 1 3036.51 430.575 15
11 1 1 3197.77 427.631 7
-11 1 -2 8895.33 693.535 10
-11 1 -2 9838.98 696.978 8
-11 1 -3 587.526 195.907 3
-11 1 -3 1015.49 257.044 8
-11 1 -4 1113.92 264.466 3
-11 2 5 1954.61 333.639 5
-11 2 5 2232.46 375.993 8
11 2 -5 2216.78 351.748 15
11 2 -5 3002.65 423.136 7
-11 2 4 35.7729 133.731 5
-11 2 4 103.322 170.929 8
11 2 -4-114.010 189.419 15
11 2 -4-71.8983 194.364 7
-11 2 3 6912.79 618.867 10
-11 2 3 6032.60 539.935 8
11 2 -3 8415.71 668.357 15
11 2 -3 6987.55 623.950 7
-11 2 2 9665.99 717.876 10
-11 2 2 9884.56 680.142 8
11 2 -2 10382.5 745.744 15
11 2 -2 10525.7 764.768 7
-11 2 1-42.6255 172.230 10
-11 2 1-114.106 160.142 8
11 2 -1-170.037 202.290 15
11 2 -1-131.344 198.331 7
-11 2 0 7686.03 633.831 10
-11 2 0 7557.22 587.252 8
11 2 0 7943.74 665.886 15
11 2 0 7611.13 653.873 7
-11 2 -1 6423.92 584.711 10
-11 2 -1 5567.85 517.626 8
11 2 1 5210.42 544.758 15
11 2 1 6220.65 602.183 7
-11 2 -2 511.664 204.072 10
-11 2 -2 654.506 231.523 8
-11 2 -3 3632.05 432.876 8
-11 2 -3 4191.90 460.571 3
-11 3 5 2195.12 375.614 5
11 3 -5 1517.56 298.400 15
11 3 -5 1645.28 317.170 7
-11 3 4 6327.66 574.903 5
11 3 -4 6889.09 610.988 15
11 3 -4 6302.12 612.821 7
-11 3 3 3608.64 455.460 10
-11 3 3 4144.73 452.105 5
11 3 -3 2677.70 400.964 15
11 3 -3 4312.83 502.219 7
-11 3 2 2583.40 385.293 10
-11 3 2 1409.45 272.399 5
11 3 -2 1533.09 334.138 15
11 3 -2 2551.57 403.476 7
-11 3 1 10434.4 686.992 5
-11 3 1 10399.3 733.902 10
-11 3 1 10338.7 675.374 8
11 3 -1 10604.2 769.050 15
11 3 -1 10869.6 793.507 7
-11 3 0 118.649 156.156 10
-11 3 0 201.124 165.009 8
11 3 0 142.697 179.965 15
11 3 0 333.691 235.258 7
-11 3 -1 4579.21 486.108 10
-11 3 -1 4089.76 426.859 8
-11 3 -2 8605.07 626.121 8
-11 3 -3 535.346 210.227 8
-11 4 4-266.676 195.325 5
11 4 -4-174.928 178.715 15
-11 4 3 8033.17 638.369 5
-11 4 3 6535.90 598.704 10
11 4 -3 7969.22 670.870 15
-11 4 2 9625.36 689.577 5
-11 4 2 9286.74 698.617 10
11 4 -2 10296.6 767.645 15
-11 4 1 44.4776 163.169 10
-11 4 1 377.984 198.958 5
-11 4 0 5229.73 518.654 10
-11 4 0 5382.79 504.378 5
-11 4 -1 4153.22 467.657 10
-11 4 -1 4648.64 471.567 5
-11 4 -2 157.598 144.969 5
-11 5 3 2312.88 366.283 10
-11 5 3 2783.24 412.681 5
-11 5 2 1510.86 314.173 10
-11 5 2 1479.07 295.647 5
-11 5 1 7027.12 602.522 5
-11 5 1 5808.58 549.971 10
-11 5 0 207.716 145.848 10
-11 5 0 422.585 211.548 5
-11 5 -1 2873.04 391.097 10
-11 5 -1 3481.89 421.856 5
-11 5 -2 7940.35 637.712 5
-11 6 2 5369.40 520.488 10
-11 6 1 97.4143 149.128 10
-11 6 0 4436.60 467.041 10
-11 6 -1 2594.19 376.532 10
-12 2 2 5571.71 539.804 8
-12 2 1 1304.69 290.739 8
-12 2 0-56.8350 159.199 8
;
_shelx_hkl_checksum 36263
_shelx_res_file
;
TITL Strauss in P2(1)
shelx.res
created by SHELXL-2019/3 at 09:59:20 on 16-Oct-2023
CELL 0.71073 8.453185 10.904012 8.716638 90.0000 93.5829 90.0000
ZERR 2.00 0.00017 0.00026 0.00021 0.0000 0.0022 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H P S Cl Au
UNIT 24.00 54.00 2.00 2.00 2.00 2.00
L.S. 6
FMAP 2
PLAN 10
SIZE 0.12 0.04 0.04
TEMP -173
ACTA 60
CONF 2.3
BOND $H
EQIV $1 1+x, y, 1+z
EQIV $2 1+x, y, z
HTAB C11 Cl1_$1
HTAB C21 Cl1_$2
HTAB C23 Au1
HTAB C33 Au1
HTAB C13 S1
HTAB C32 S1
TWIN
WGHT 0.011000
EXTI 0.000877
BASF 0.49341
FVAR 1.69148
AU1 6 0.312011 0.564149 0.170746 11.00000 0.01100 0.01472 =
0.01674 -0.00056 0.00179 0.00010
CL1 5 0.162214 0.569870 -0.056195 11.00000 0.01940 0.02003 =
0.01694 -0.00033 -0.00075 -0.00103
P1 3 0.687676 0.556987 0.348866 11.00000 0.01201 0.01134 =
0.01016 -0.00028 0.00038 -0.00184
S1 4 0.454450 0.552495 0.399728 11.00000 0.01403 0.01950 =
0.01488 -0.00020 0.00380 -0.00119
C1 1 0.794647 0.570548 0.546509 11.00000 0.01778 0.01809 =
0.01093 -0.00177 -0.00201 -0.00384
C2 1 0.739919 0.406874 0.252890 11.00000 0.01621 0.00631 =
0.00947 -0.00010 -0.00027 0.00144
C3 1 0.730533 0.693984 0.224782 11.00000 0.01393 0.00877 =
0.01542 -0.00409 0.00359 0.00245
C11 1 0.972237 0.539867 0.543268 11.00000 0.02183 0.02688 =
0.01558 0.00317 -0.00705 -0.00611
AFIX 137
H11A 2 1.025548 0.558348 0.643676 11.00000 -1.50000
H11B 2 1.019336 0.589148 0.463893 11.00000 -1.50000
H11C 2 0.984837 0.452582 0.520174 11.00000 -1.50000
AFIX 0
C12 1 0.776304 0.702187 0.609880 11.00000 0.02595 0.02248 =
0.01651 -0.00530 0.00074 -0.00490
AFIX 137
H12A 2 0.828416 0.760500 0.543936 11.00000 -1.50000
H12B 2 0.825412 0.706776 0.714582 11.00000 -1.50000
H12C 2 0.663482 0.722555 0.611207 11.00000 -1.50000
AFIX 0
C13 1 0.720381 0.485552 0.663334 11.00000 0.02795 0.02888 =
0.01046 -0.00032 -0.00041 -0.00615
AFIX 137
H13A 2 0.784327 0.487915 0.761022 11.00000 -1.50000
H13B 2 0.717121 0.401449 0.623621 11.00000 -1.50000
H13C 2 0.612418 0.513184 0.679729 11.00000 -1.50000
AFIX 0
C21 1 0.905114 0.411839 0.187461 11.00000 0.01556 0.01260 =
0.01927 0.00246 -0.00056 0.00207
AFIX 137
H21A 2 0.905982 0.475338 0.107954 11.00000 -1.50000
H21B 2 0.929363 0.332133 0.142587 11.00000 -1.50000
H21C 2 0.984985 0.431201 0.270260 11.00000 -1.50000
AFIX 0
C22 1 0.733442 0.301403 0.368934 11.00000 0.02221 0.01300 =
0.02089 0.00078 0.00054 -0.00087
AFIX 137
H22A 2 0.739656 0.222865 0.314982 11.00000 -1.50000
H22B 2 0.633712 0.305586 0.420296 11.00000 -1.50000
H22C 2 0.822823 0.308415 0.445620 11.00000 -1.50000
AFIX 0
C23 1 0.617857 0.375748 0.120895 11.00000 0.01903 0.01584 =
0.01887 -0.00612 -0.00010 0.00149
AFIX 137
H23A 2 0.648524 0.299347 0.071520 11.00000 -1.50000
H23B 2 0.613931 0.442353 0.045267 11.00000 -1.50000
H23C 2 0.513170 0.365667 0.161610 11.00000 -1.50000
AFIX 0
C31 1 0.907925 0.732176 0.238675 11.00000 0.01900 0.01393 =
0.01385 0.00025 0.00269 -0.00135
AFIX 137
H31A 2 0.938675 0.752911 0.345808 11.00000 -1.50000
H31B 2 0.923658 0.803689 0.173256 11.00000 -1.50000
H31C 2 0.973333 0.664016 0.205725 11.00000 -1.50000
AFIX 0
C32 1 0.627622 0.804598 0.270111 11.00000 0.02365 0.01157 =
0.01914 0.00326 0.00419 0.00242
AFIX 137
H32A 2 0.653075 0.876203 0.208330 11.00000 -1.50000
H32B 2 0.649634 0.823282 0.379334 11.00000 -1.50000
H32C 2 0.515199 0.784127 0.251279 11.00000 -1.50000
AFIX 0
C33 1 0.688968 0.670141 0.052892 11.00000 0.01659 0.01652 =
0.01493 0.00287 0.00065 0.00164
AFIX 137
H33A 2 0.759057 0.606472 0.015972 11.00000 -1.50000
H33B 2 0.702814 0.745915 -0.005224 11.00000 -1.50000
H33C 2 0.578575 0.642859 0.038511 11.00000 -1.50000
AFIX 0
HKLF 4
REM Strauss in P2(1)
REM wR2 = 0.0332, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0188 for 4382 Fo > 4sig(Fo) and 0.0214 for all 4617 data
REM 156 parameters refined using 1 restraints
END
WGHT 0.0110 0.0000
REM Highest difference peak 0.618, deepest hole -0.750, 1-sigma level 0.106
Q1 1 0.8678 0.5617 0.5429 11.00000 0.05 0.62
Q2 1 0.3244 0.5624 0.3001 11.00000 0.05 0.61
Q3 1 0.4252 0.5627 0.4785 11.00000 0.05 0.53
Q4 1 0.2387 0.5635 0.1589 11.00000 0.05 0.52
Q5 1 0.2564 0.5483 0.0446 11.00000 0.05 0.50
Q6 1 0.4064 0.6181 0.2823 11.00000 0.05 0.47
Q7 1 0.2934 0.5656 -0.0411 11.00000 0.05 0.45
Q8 1 0.6184 0.5636 0.4145 11.00000 0.05 0.42
Q9 1 0.2330 0.5194 0.2501 11.00000 0.05 0.42
Q10 1 0.6787 0.2587 0.4218 11.00000 0.05 0.41
;
_shelx_res_checksum 52216
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au1 0.31201(2) 0.56415(4) 0.17075(2) 0.01412(5) Uani d 1 . .
Cl Cl1 0.16221(10) 0.5699(4) -0.05619(10) 0.0189(2) Uani d 1 . .
P P1 0.68768(10) 0.5570(4) 0.34887(10) 0.0112(3) Uani d 1 . .
S S1 0.45445(11) 0.5525(4) 0.39973(11) 0.0160(4) Uani d 1 . .
C C1 0.7946(4) 0.5705(10) 0.5465(4) 0.0157(8) Uani d 1 . .
C C2 0.7399(9) 0.4069(6) 0.2529(8) 0.0107(13) Uani d 1 . .
C C3 0.7305(9) 0.6940(6) 0.2248(8) 0.0126(14) Uani d 1 . .
C C11 0.9722(5) 0.5399(5) 0.5433(5) 0.0218(14) Uani d 1 . .
H H11A 1.025548 0.558348 0.643676 0.033 Uiso calc 1 . .
H H11B 1.019336 0.589148 0.463893 0.033 Uiso calc 1 . .
H H11C 0.984837 0.452582 0.520174 0.033 Uiso calc 1 . .
C C12 0.7763(6) 0.7022(5) 0.6099(5) 0.0217(10) Uani d 1 . .
H H12A 0.828416 0.760500 0.543936 0.033 Uiso calc 1 . .
H H12B 0.825412 0.706776 0.714582 0.033 Uiso calc 1 . .
H H12C 0.663482 0.722555 0.611207 0.033 Uiso calc 1 . .
C C13 0.7204(6) 0.4856(5) 0.6633(5) 0.0225(10) Uani d 1 . .
H H13A 0.784327 0.487915 0.761022 0.034 Uiso calc 1 . .
H H13B 0.717121 0.401449 0.623621 0.034 Uiso calc 1 . .
H H13C 0.612418 0.513184 0.679729 0.034 Uiso calc 1 . .
C C21 0.9051(8) 0.4118(6) 0.1875(6) 0.0159(13) Uani d 1 . .
H H21A 0.905982 0.475338 0.107954 0.024 Uiso calc 1 . .
H H21B 0.929363 0.332133 0.142587 0.024 Uiso calc 1 . .
H H21C 0.984985 0.431201 0.270260 0.024 Uiso calc 1 . .
C C22 0.7334(5) 0.3014(4) 0.3689(5) 0.0187(9) Uani d 1 . .
H H22A 0.739656 0.222865 0.314982 0.028 Uiso calc 1 . .
H H22B 0.633712 0.305586 0.420296 0.028 Uiso calc 1 . .
H H22C 0.822823 0.308415 0.445620 0.028 Uiso calc 1 . .
C C23 0.6179(5) 0.3757(4) 0.1209(5) 0.0180(9) Uani d 1 . .
H H23A 0.648524 0.299347 0.071520 0.027 Uiso calc 1 . .
H H23B 0.613931 0.442353 0.045267 0.027 Uiso calc 1 . .
H H23C 0.513170 0.365667 0.161610 0.027 Uiso calc 1 . .
C C31 0.9079(9) 0.7322(6) 0.2387(6) 0.0155(13) Uani d 1 . .
H H31A 0.938675 0.752911 0.345808 0.023 Uiso calc 1 . .
H H31B 0.923658 0.803689 0.173256 0.023 Uiso calc 1 . .
H H31C 0.973333 0.664016 0.205725 0.023 Uiso calc 1 . .
C C32 0.6276(5) 0.8046(4) 0.2701(5) 0.0180(9) Uani d 1 . .
H H32A 0.653075 0.876203 0.208330 0.027 Uiso calc 1 . .
H H32B 0.649634 0.823282 0.379334 0.027 Uiso calc 1 . .
H H32C 0.515199 0.784127 0.251279 0.027 Uiso calc 1 . .
C C33 0.6890(5) 0.6701(4) 0.0529(5) 0.0160(9) Uani d 1 . .
H H33A 0.759057 0.606472 0.015972 0.024 Uiso calc 1 . .
H H33B 0.702814 0.745915 -0.005224 0.024 Uiso calc 1 . .
H H33C 0.578575 0.642859 0.038511 0.024 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 0.01100(6) 0.01472(8) 0.01674(7) 0.00010(15) 0.00179(4) -0.00056(16)
Cl1 0.0194(4) 0.0200(7) 0.0169(4) -0.0010(11) -0.0007(3) -0.0003(11)
P1 0.0120(3) 0.0113(9) 0.0102(4) -0.0018(8) 0.0004(3) -0.0003(9)
S1 0.0140(4) 0.0195(13) 0.0149(4) -0.0012(7) 0.0038(3) -0.0002(7)
C1 0.0178(15) 0.018(2) 0.0109(15) -0.004(4) -0.0020(12) -0.002(4)
C2 0.016(3) 0.006(3) 0.009(3) 0.001(2) 0.000(2) 0.000(2)
C3 0.014(3) 0.009(3) 0.015(3) 0.002(2) 0.004(2) -0.004(2)
C11 0.0218(19) 0.027(4) 0.0156(19) -0.006(2) -0.0070(15) 0.0032(19)
C12 0.026(2) 0.022(3) 0.017(2) -0.005(2) 0.001(2) -0.005(2)
C13 0.028(3) 0.029(3) 0.010(2) -0.006(2) -0.0004(19) 0.000(2)
C21 0.016(2) 0.013(3) 0.019(3) 0.002(2) -0.001(3) 0.002(2)
C22 0.022(2) 0.013(2) 0.021(2) -0.0009(18) 0.0005(18) 0.0008(18)
C23 0.019(2) 0.016(2) 0.019(2) 0.0015(18) -0.0001(18) -0.0061(19)
C31 0.019(2) 0.014(3) 0.014(3) -0.001(2) 0.003(2) 0.000(2)
C32 0.024(2) 0.012(2) 0.019(2) 0.0024(18) 0.0042(18) 0.0033(18)
C33 0.017(2) 0.017(2) 0.015(2) 0.0016(18) 0.0007(17) 0.0029(18)
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S1 Au1 Cl1 . . 177.70(15) y
C3 P1 C1 . . 111.1(4) y
C3 P1 C2 . . 111.7(2) y
C1 P1 C2 . . 110.8(4) y
C3 P1 S1 . . 111.3(3) y
C1 P1 S1 . . 102.45(12) y
C2 P1 S1 . . 109.1(3) y
P1 S1 Au1 . . 105.86(5) y
C13 C1 C11 . . 108.6(6) ?
C13 C1 C12 . . 105.5(4) ?
C11 C1 C12 . . 109.1(5) ?
C13 C1 P1 . . 111.2(4) ?
C11 C1 P1 . . 112.1(3) ?
C12 C1 P1 . . 110.0(5) ?
C23 C2 C22 . . 106.2(5) ?
C23 C2 C21 . . 108.2(5) ?
C22 C2 C21 . . 109.9(5) ?
C23 C2 P1 . . 110.9(4) ?
C22 C2 P1 . . 109.6(4) ?
C21 C2 P1 . . 111.9(4) ?
C33 C3 C32 . . 106.3(5) ?
C33 C3 C31 . . 106.4(5) ?
C32 C3 C31 . . 109.0(5) ?
C33 C3 P1 . . 112.5(4) ?
C32 C3 P1 . . 109.7(5) ?
C31 C3 P1 . . 112.7(5) ?
C1 C11 H11A . . 109.5 ?
C1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C1 C12 H12A . . 109.5 ?
C1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C1 C13 H13A . . 109.5 ?
C1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C2 C21 H21A . . 109.5 ?
C2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C2 C22 H22A . . 109.5 ?
C2 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C2 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C2 C23 H23A . . 109.5 ?
C2 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C2 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C3 C31 H31A . . 109.5 ?
C3 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C3 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C3 C32 H32A . . 109.5 ?
C3 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C3 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C3 C33 H33A . . 109.5 ?
C3 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C3 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 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 S1 . 2.2692(10) y
Au1 Cl1 . 2.2820(8) y
P1 C3 . 1.892(8) ?
P1 C1 . 1.901(4) ?
P1 C2 . 1.903(8) ?
P1 S1 . 2.0482(12) y
C1 C13 . 1.539(8) ?
C1 C11 . 1.540(6) ?
C1 C12 . 1.549(11) ?
C2 C23 . 1.535(8) ?
C2 C22 . 1.535(7) ?
C2 C21 . 1.542(10) ?
C3 C33 . 1.540(8) ?
C3 C32 . 1.553(8) ?
C3 C31 . 1.554(10) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C33 H33A . 0.9800 ?
C33 H33B . 0.9800 ?
C33 H33C . 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
C11 H11A Cl1 1_656 0.98 2.80 3.765(4) 170.1 yes
C21 H21A Cl1 1_655 0.98 2.86 3.575(7) 130.3 yes
C23 H23C Au1 . 0.98 2.76 3.352(4) 119.7 yes
C33 H33C Au1 . 0.98 2.73 3.599(4) 147.7 yes
C13 H13C S1 . 0.98 2.74 3.197(5) 108.9 yes
C32 H32C S1 . 0.98 2.90 3.344(6) 108.7 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
C3 P1 S1 Au1 . . . . 53.2(3) y
C1 P1 S1 Au1 . . . . 172.0(4) y
C2 P1 S1 Au1 . . . . -70.5(3) y
C3 P1 C1 C13 . . . . 161.2(5) ?
C2 P1 C1 C13 . . . . -74.0(5) ?
S1 P1 C1 C13 . . . . 42.3(6) ?
C3 P1 C1 C11 . . . . -76.9(7) ?
C2 P1 C1 C11 . . . . 47.8(7) ?
S1 P1 C1 C11 . . . . 164.1(6) ?
C3 P1 C1 C12 . . . . 44.6(4) ?
C2 P1 C1 C12 . . . . 169.4(4) ?
S1 P1 C1 C12 . . . . -74.3(4) ?
C3 P1 C2 C23 . . . . -73.8(4) ?
C1 P1 C2 C23 . . . . 161.8(4) ?
S1 P1 C2 C23 . . . . 49.7(5) ?
C3 P1 C2 C22 . . . . 169.3(5) ?
C1 P1 C2 C22 . . . . 44.9(5) ?
S1 P1 C2 C22 . . . . -67.2(5) ?
C3 P1 C2 C21 . . . . 47.1(4) ?
C1 P1 C2 C21 . . . . -77.3(5) ?
S1 P1 C2 C21 . . . . 170.6(3) ?
C1 P1 C3 C33 . . . . 163.0(4) ?
C2 P1 C3 C33 . . . . 38.7(4) ?
S1 P1 C3 C33 . . . . -83.5(5) ?
C1 P1 C3 C32 . . . . -78.8(5) ?
C2 P1 C3 C32 . . . . 156.9(5) ?
S1 P1 C3 C32 . . . . 34.6(5) ?
C1 P1 C3 C31 . . . . 42.8(5) ?
C2 P1 C3 C31 . . . . -81.5(5) ?
S1 P1 C3 C31 . . . . 156.2(4) ?