#------------------------------------------------------------------------------
#$Date: 2024-05-06 07:23:16 +0300 (Mon, 06 May 2024) $
#$Revision: 291733 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023055.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_2023055
loop_
_publ_author_name
'Upmann, Daniel'
'Bockfeld, Dirk'
'Jones, Peter G.'
'Târcoveanu, Eliza'
_publ_section_title
;
 Crystal structures of ten phosphane chalcogenide complexes of gold(III)
 chloride and bromide.
;
_journal_coeditor_code           YZ2051
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              355
_journal_page_last               369
_journal_paper_doi               10.1107/S2056989024002032
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Au Cl3 (C12 H27 P S)], C H2 Cl2'
_chemical_formula_moiety         'C12 H27 Au Cl3 P S, C H2 Cl2'
_chemical_formula_sum            'C13 H29 Au Cl5 P S'
_chemical_formula_weight         622.61
_chemical_name_systematic
;
Trichlorido(tri-tert-butylphosphane sulfide-κS)gold(III)
dichloromethane monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                98.398(3)
_cell_angle_beta                 101.174(3)
_cell_angle_gamma                95.991(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4202(3)
_cell_length_b                   11.2194(4)
_cell_length_c                   11.8355(4)
_cell_measurement_reflns_used    47731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6240
_cell_measurement_theta_min      2.7670
_cell_volume                     1074.95(7)
_computing_cell_refinement
;
CrysAlisPro, Version  1.171.38.43 (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro, Version  1.171.38.43 (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro, Version  1.171.38.43 (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 0.993
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            157605
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.123
_diffrn_reflns_theta_min         2.340
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.012
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         6558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0205
_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/[σ²(Fo²)+(0.0147P)²+0.9642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0373
_reflns_number_gt                6124
_reflns_number_total             6558
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yz2051.cif
_cod_data_source_block           12a
_cod_depositor_comments
'Adding full bibliography for 2023050--2023062.cif.'
_cod_database_code               2023055
_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   0.516
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au1 0.53561(2) 0.65489(2) 0.29756(2) 0.01423(3) Uani d 1 . .
P P1 0.63223(6) 0.33330(4) 0.26499(4) 0.01110(9) Uani d 1 . .
S S1 0.55574(6) 0.47197(4) 0.36749(4) 0.01588(10) Uani d 1 . .
Cl Cl1 0.51329(8) 0.84355(5) 0.24639(6) 0.03068(13) Uani d 1 . .
Cl Cl2 0.78232(7) 0.73160(5) 0.41951(5) 0.02751(12) Uani d 1 . .
Cl Cl3 0.28358(6) 0.58666(4) 0.18025(5) 0.01819(10) Uani d 1 . .
C C1 0.6853(2) 0.23096(17) 0.37810(18) 0.0147(4) Uani d 1 . .
C C2 0.8182(2) 0.38937(18) 0.21024(18) 0.0156(4) Uani d 1 . .
C C3 0.4579(2) 0.25575(17) 0.14205(18) 0.0152(4) Uani d 1 . .
C C11 0.7890(3) 0.13553(18) 0.3356(2) 0.0189(4) Uani d 1 . .
H H11A 0.896288 0.176237 0.332015 0.028 Uiso calc 1 . .
H H11B 0.733736 0.091959 0.257732 0.028 Uiso calc 1 . .
H H11C 0.803183 0.077662 0.390133 0.028 Uiso calc 1 . .
C C12 0.5282(3) 0.16507(19) 0.4010(2) 0.0187(4) Uani d 1 . .
H H12A 0.556046 0.121650 0.466725 0.028 Uiso calc 1 . .
H H12B 0.472365 0.106869 0.331072 0.028 Uiso calc 1 . .
H H12C 0.456061 0.224697 0.419971 0.028 Uiso calc 1 . .
C C13 0.7792(3) 0.3055(2) 0.49633(19) 0.0204(4) Uani d 1 . .
H H13A 0.806888 0.250522 0.552104 0.031 Uiso calc 1 . .
H H13B 0.710742 0.362704 0.526409 0.031 Uiso calc 1 . .
H H13C 0.879701 0.350796 0.485668 0.031 Uiso calc 1 . .
C C21 0.8590(3) 0.2910(2) 0.1190(2) 0.0210(4) Uani d 1 . .
H H21A 0.959839 0.320758 0.096282 0.031 Uiso calc 1 . .
H H21B 0.769214 0.272475 0.049961 0.031 Uiso calc 1 . .
H H21C 0.873861 0.217124 0.152734 0.031 Uiso calc 1 . .
C C22 0.9645(3) 0.4278(2) 0.3140(2) 0.0217(4) Uani d 1 . .
H H22A 1.055508 0.469794 0.288068 0.033 Uiso calc 1 . .
H H22B 0.998283 0.355582 0.344279 0.033 Uiso calc 1 . .
H H22C 0.933090 0.482692 0.375708 0.033 Uiso calc 1 . .
C C23 0.7922(3) 0.50296(19) 0.1537(2) 0.0198(4) Uani d 1 . .
H H23A 0.785061 0.571139 0.213648 0.030 Uiso calc 1 . .
H H23B 0.690694 0.486182 0.093839 0.030 Uiso calc 1 . .
H H23C 0.884367 0.523857 0.117485 0.030 Uiso calc 1 . .
C C31 0.4816(3) 0.12534(18) 0.0939(2) 0.0209(4) Uani d 1 . .
H H31A 0.392796 0.091382 0.026551 0.031 Uiso calc 1 . .
H H31B 0.480460 0.074977 0.154879 0.031 Uiso calc 1 . .
H H31C 0.586512 0.126580 0.069678 0.031 Uiso calc 1 . .
C C32 0.2951(2) 0.25318(19) 0.1836(2) 0.0186(4) Uani d 1 . .
H H32A 0.277011 0.336554 0.210355 0.028 Uiso calc 1 . .
H H32B 0.299746 0.207114 0.248201 0.028 Uiso calc 1 . .
H H32C 0.205260 0.214234 0.118818 0.028 Uiso calc 1 . .
C C33 0.4420(3) 0.32898(19) 0.04080(19) 0.0191(4) Uani d 1 . .
H H33A 0.538213 0.325449 0.005922 0.029 Uiso calc 1 . .
H H33B 0.434062 0.413848 0.070728 0.029 Uiso calc 1 . .
H H33C 0.343501 0.294182 -0.018603 0.029 Uiso calc 1 . .
C C99 1.0588(4) 0.8679(2) 0.2453(2) 0.0322(6) Uani d 1 . .
H H99A 0.963855 0.820052 0.262990 0.039 Uiso calc 1 . .
H H99B 1.141490 0.813027 0.234783 0.039 Uiso calc 1 . .
Cl Cl4 1.14230(7) 0.98659(5) 0.36326(5) 0.02400(11) Uani d 1 . .
Cl Cl5 0.99590(10) 0.92468(7) 0.11422(6) 0.04378(17) Uani d 1 . .
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
Cl3 Au1 Cl2 . . 176.996(18) y
Cl3 Au1 Cl1 . . 88.53(2) y
Cl2 Au1 Cl1 . . 89.55(2) y
Cl3 Au1 S1 . . 93.402(18) y
Cl2 Au1 S1 . . 88.30(2) y
Cl1 Au1 S1 . . 174.441(19) y
C3 P1 C2 . . 112.33(9) y
C3 P1 C1 . . 111.29(9) y
C2 P1 C1 . . 111.38(9) y
C3 P1 S1 . . 110.17(6) y
C2 P1 S1 . . 111.66(6) y
C1 P1 S1 . . 99.33(6) y
P1 S1 Au1 . . 117.50(3) y
C12 C1 C11 . . 108.93(16) ?
C12 C1 C13 . . 106.51(17) ?
C11 C1 C13 . . 109.07(17) ?
C12 C1 P1 . . 110.11(14) ?
C11 C1 P1 . . 110.82(14) ?
C13 C1 P1 . . 111.28(13) ?
C22 C2 C23 . . 106.45(17) ?
C22 C2 C21 . . 110.01(17) ?
C23 C2 C21 . . 108.11(17) ?
C22 C2 P1 . . 109.39(14) ?
C23 C2 P1 . . 111.29(13) ?
C21 C2 P1 . . 111.46(14) ?
C31 C3 C33 . . 108.18(17) ?
C31 C3 C32 . . 109.39(16) ?
C33 C3 C32 . . 106.69(17) ?
C31 C3 P1 . . 112.55(14) ?
C33 C3 P1 . . 109.73(13) ?
C32 C3 P1 . . 110.12(14) ?
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 ?
Cl4 C99 Cl5 . . 111.42(13) ?
Cl4 C99 H99A . . 109.3 ?
Cl5 C99 H99A . . 109.3 ?
Cl4 C99 H99B . . 109.3 ?
Cl5 C99 H99B . . 109.3 ?
H99A C99 H99B . . 108.0 ?
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 Cl3 . 2.2860(5) y
Au1 Cl2 . 2.2894(6) y
Au1 Cl1 . 2.3013(5) y
Au1 S1 . 2.3323(5) y
P1 C3 . 1.888(2) y
P1 C2 . 1.8906(19) y
P1 C1 . 1.906(2) y
P1 S1 . 2.0658(6) y
C1 C12 . 1.537(3) ?
C1 C11 . 1.540(3) ?
C1 C13 . 1.541(3) ?
C2 C22 . 1.536(3) ?
C2 C23 . 1.540(3) ?
C2 C21 . 1.542(3) ?
C3 C31 . 1.538(3) ?
C3 C33 . 1.542(3) ?
C3 C32 . 1.542(3) ?
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 ?
C99 Cl4 . 1.760(3) ?
C99 Cl5 . 1.770(3) ?
C99 H99A . 0.9900 ?
C99 H99B . 0.9900 ?
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
C23 H23A Au1 . 0.98 2.69 3.438(2) 133.6 yes
C13 H13B S1 . 0.98 2.61 3.131(2) 113.6 yes
C32 H32A S1 . 0.98 2.83 3.323(2) 111.9 yes
C23 H23A Cl2 . 0.98 2.82 3.778(2) 167.5 yes
C32 H32A Cl3 . 0.98 2.88 3.759(2) 150.3 yes
C33 H33B Cl3 . 0.98 2.73 3.623(2) 151.5 yes
C99 H99A Cl2 . 0.99 2.84 3.749(3) 152.7 yes
C99 H99B Cl3 1_655 0.99 2.96 3.903(3) 159.9 yes
C22 H22A Cl3 1_655 0.98 2.82 3.791(2) 171.2 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 . . . . -78.75(7) y
C2 P1 S1 Au1 . . . . 46.80(8) y
C1 P1 S1 Au1 . . . . 164.36(6) y
Cl3 Au1 S1 P1 . . . . 82.19(3) y
Cl2 Au1 S1 P1 . . . . -100.28(3) y
C3 P1 C1 C12 . . . . -41.56(16) ?
C2 P1 C1 C12 . . . . -167.75(13) ?
S1 P1 C1 C12 . . . . 74.48(14) ?
C3 P1 C1 C11 . . . . 79.02(16) ?
C2 P1 C1 C11 . . . . -47.17(16) ?
S1 P1 C1 C11 . . . . -164.93(13) ?
C3 P1 C1 C13 . . . . -159.43(13) ?
C2 P1 C1 C13 . . . . 74.39(16) ?
S1 P1 C1 C13 . . . . -43.38(14) ?
C3 P1 C2 C22 . . . . -168.80(13) ?
C1 P1 C2 C22 . . . . -43.18(16) ?
S1 P1 C2 C22 . . . . 66.86(15) ?
C3 P1 C2 C23 . . . . 73.86(16) ?
C1 P1 C2 C23 . . . . -160.53(14) ?
S1 P1 C2 C23 . . . . -50.49(16) ?
C3 P1 C2 C21 . . . . -46.91(17) ?
C1 P1 C2 C21 . . . . 78.70(17) ?
S1 P1 C2 C21 . . . . -171.26(13) ?
C2 P1 C3 C31 . . . . 77.86(17) ?
C1 P1 C3 C31 . . . . -47.81(17) ?
S1 P1 C3 C31 . . . . -156.98(13) ?
C2 P1 C3 C33 . . . . -42.66(16) ?
C1 P1 C3 C33 . . . . -168.32(13) ?
S1 P1 C3 C33 . . . . 82.51(13) ?
C2 P1 C3 C32 . . . . -159.80(13) ?
C1 P1 C3 C32 . . . . 74.54(15) ?
S1 P1 C3 C32 . . . . -34.64(15) ?
