#------------------------------------------------------------------------------
#$Date: 2024-10-01 05:15:35 +0300 (Tue, 01 Oct 2024) $
#$Revision: 294951 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023266.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_2023266
loop_
_publ_author_name
'Upmann, Daniel'
'Bockfeld, Dirk'
'Jones, Peter G.'
'Târcoveanu, Eliza'
_publ_section_title
;
 Crystal structures of seven mixed-valence gold compounds of the form [(R
 1 R 2 R 3PE)2AuI]+[AuIII X 4]− (R = tert-butyl or isopropyl, E = S
 or Se, and X = Cl or Br)
;
_journal_coeditor_code           WM5733
_journal_issue                   10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1087
_journal_page_last               1096
_journal_paper_doi               10.1107/S2056989024009095
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Au (C12 H27 P1 S1)2] [Au Cl4]'
_chemical_formula_moiety         'C24 H54 Au P2 S2 +, Au Cl4 -'
_chemical_formula_sum            'C24 H54 Au2 Cl4 P2 S2'
_chemical_formula_weight         1004.46
_chemical_name_common
;
Bis(tri-tert-butylphosphane sulfide)gold(I) tetrachloridoaurate(III)
;
_chemical_name_systematic
;
Bis(tri-tert-butylphosphane sulfide-κS)gold(I)
tetrachloridoaurate(III)
;
_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                107.427(3)
_cell_angle_beta                 97.511(3)
_cell_angle_gamma                102.841(3)
_cell_formula_units_Z            1
_cell_length_a                   8.5541(2)
_cell_length_b                   9.1550(3)
_cell_length_c                   12.0421(4)
_cell_measurement_reflns_used    64231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7560
_cell_measurement_theta_min      2.4090
_cell_volume                     857.31(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
XP (Bruker, 1998)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.946
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            166022
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         31.083
_diffrn_reflns_theta_min         2.426
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.379
_refine_ls_extinction_coef       0.00495(18)
_refine_ls_extinction_expression
;Fc^*^ =
 kFc[1+0.001×Fc²λ³/sin(2θ)]^-1/4^
;
_refine_ls_extinction_method
;
SHELXL2019/3 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         5209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0185P)²+0.7041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0382
_reflns_number_gt                4622
_reflns_number_total             5209
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5733.cif
_cod_data_source_block           3
_cod_original_cell_volume        857.30(5)
_cod_database_code               2023266
_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   0.264
_shelx_estimated_absorpt_t_max   0.343
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 0.500000 0.000000 0.500000 0.01381(4) Uani d 1 . .
P P1 0.23333(6) 0.11351(5) 0.31699(4) 0.01003(9) Uani d 1 . .
S S1 0.32514(6) 0.15468(6) 0.49180(4) 0.01576(9) Uani d 1 . .
C C1 0.1171(2) 0.2704(2) 0.32846(16) 0.0142(3) Uani d 1 . .
C C2 0.0891(2) -0.0945(2) 0.24486(16) 0.0132(3) Uani d 1 . .
C C3 0.4057(2) 0.1460(2) 0.23434(15) 0.0129(3) Uani d 1 . .
C C11 -0.0022(3) 0.2404(2) 0.21169(18) 0.0187(4) Uani d 1 . .
H H11A -0.048072 0.331055 0.219483 0.028 Uiso calc 1 . .
H H11B -0.091156 0.143334 0.194725 0.028 Uiso calc 1 . .
H H11C 0.056734 0.227528 0.146391 0.028 Uiso calc 1 . .
C C12 0.2395(3) 0.4356(2) 0.36375(18) 0.0192(4) Uani d 1 . .
H H12A 0.294950 0.441402 0.298285 0.029 Uiso calc 1 . .
H H12B 0.321044 0.453291 0.435083 0.029 Uiso calc 1 . .
H H12C 0.180728 0.517607 0.380378 0.029 Uiso calc 1 . .
C C13 0.0194(3) 0.2785(2) 0.42887(18) 0.0200(4) Uani d 1 . .
H H13A 0.095897 0.310702 0.505547 0.030 Uiso calc 1 . .
H H13B -0.055894 0.173395 0.413300 0.030 Uiso calc 1 . .
H H13C -0.043387 0.356352 0.431261 0.030 Uiso calc 1 . .
C C21 0.0403(2) -0.1412(2) 0.10879(16) 0.0168(4) Uani d 1 . .
H H21A -0.044660 -0.243312 0.076309 0.025 Uiso calc 1 . .
H H21B 0.136711 -0.151025 0.074283 0.025 Uiso calc 1 . .
H H21C -0.002069 -0.058982 0.089049 0.025 Uiso calc 1 . .
C C22 -0.0668(3) -0.1054(2) 0.29582(19) 0.0202(4) Uani d 1 . .
H H22A -0.134025 -0.216395 0.266777 0.030 Uiso calc 1 . .
H H22B -0.129498 -0.039380 0.270205 0.030 Uiso calc 1 . .
H H22C -0.036434 -0.067401 0.382994 0.030 Uiso calc 1 . .
C C23 0.1666(3) -0.2184(2) 0.27418(17) 0.0169(4) Uani d 1 . .
H H23A 0.191786 -0.193494 0.360662 0.025 Uiso calc 1 . .
H H23B 0.267939 -0.215856 0.244147 0.025 Uiso calc 1 . .
H H23C 0.089573 -0.324714 0.236401 0.025 Uiso calc 1 . .
C C31 0.3485(3) 0.1787(2) 0.11975(16) 0.0163(4) Uani d 1 . .
H H31A 0.439144 0.190646 0.078153 0.024 Uiso calc 1 . .
H H31B 0.313906 0.276878 0.140200 0.024 Uiso calc 1 . .
H H31C 0.256104 0.089492 0.067927 0.024 Uiso calc 1 . .
C C32 0.5508(2) 0.2864(2) 0.31569(18) 0.0174(4) Uani d 1 . .
H H32A 0.590922 0.263261 0.386809 0.026 Uiso calc 1 . .
H H32B 0.514561 0.383441 0.339413 0.026 Uiso calc 1 . .
H H32C 0.639240 0.301838 0.272617 0.026 Uiso calc 1 . .
C C33 0.4723(2) -0.0006(2) 0.20037(17) 0.0156(4) Uani d 1 . .
H H33A 0.567529 0.022387 0.164807 0.023 Uiso calc 1 . .
H H33B 0.386675 -0.091506 0.142802 0.023 Uiso calc 1 . .
H H33C 0.505082 -0.026062 0.271857 0.023 Uiso calc 1 . .
Au Au2 0.500000 0.500000 1.000000 0.01173(3) Uani d 1 . .
Cl Cl1 0.47385(6) 0.37675(5) 0.80089(4) 0.01857(9) Uani d 1 . .
Cl Cl2 0.26132(6) 0.56585(6) 0.96144(5) 0.02260(10) 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
S1 Au1 S1 . 2_656 180.0 y
C2 P1 C3 . . 111.14(8) ?
C2 P1 C1 . . 111.01(9) ?
C3 P1 C1 . . 111.40(8) ?
C2 P1 S1 . . 110.51(6) ?
C3 P1 S1 . . 110.85(6) ?
C1 P1 S1 . . 101.57(6) y
P1 S1 Au1 . . 107.87(2) y
C12 C1 C11 . . 108.62(15) ?
C12 C1 C13 . . 106.15(15) ?
C11 C1 C13 . . 108.74(16) ?
C12 C1 P1 . . 109.58(13) ?
C11 C1 P1 . . 112.97(12) ?
C13 C1 P1 . . 110.54(12) ?
C22 C2 C21 . . 108.92(16) ?
C22 C2 C23 . . 105.94(15) ?
C21 C2 C23 . . 108.80(15) ?
C22 C2 P1 . . 109.76(13) ?
C21 C2 P1 . . 112.22(12) ?
C23 C2 P1 . . 110.98(13) ?
C33 C3 C31 . . 108.25(14) ?
C33 C3 C32 . . 106.34(16) ?
C31 C3 C32 . . 109.41(15) ?
C33 C3 P1 . . 110.79(12) ?
C31 C3 P1 . . 111.87(13) ?
C32 C3 P1 . . 110.02(12) ?
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 ?
Cl1 Au2 Cl1 2_667 . 180.0 y
Cl1 Au2 Cl2 2_667 . 90.336(18) ?
Cl1 Au2 Cl2 . . 89.664(18) y
Cl1 Au2 Cl2 2_667 2_667 89.664(18) ?
Cl1 Au2 Cl2 . 2_667 90.336(18) y
Cl2 Au2 Cl2 . 2_667 180.0 y
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 . 2.2889(5) y
Au1 S1 2_656 2.2889(5) ?
P1 C2 . 1.8939(19) ?
P1 C3 . 1.9024(19) ?
P1 C1 . 1.9036(18) ?
P1 S1 . 2.0374(6) y
C1 C12 . 1.536(3) ?
C1 C11 . 1.537(3) ?
C1 C13 . 1.550(3) ?
C2 C22 . 1.535(3) ?
C2 C21 . 1.538(2) ?
C2 C23 . 1.538(2) ?
C3 C33 . 1.538(2) ?
C3 C31 . 1.539(2) ?
C3 C32 . 1.540(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 ?
Au2 Cl1 2_667 2.2802(5) ?
Au2 Cl1 . 2.2802(5) y
Au2 Cl2 . 2.2836(5) y
Au2 Cl2 2_667 2.2836(5) ?
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 2.81 3.421(2) 121.2 yes
C33 H33C Au1 . 0.98 2.69 3.5832(19) 151.3 yes
C13 H13A S1 . 0.98 2.66 3.164(2) 111.9 yes
C32 H32A S1 . 0.98 2.87 3.353(2) 111.1 yes
C12 H12A Cl1 2_666 0.98 2.91 3.786(2) 149.6 yes
C22 H22A Cl1 2_556 0.98 2.83 3.607(2) 136.3 yes
C23 H23B Cl1 2_656 0.98 2.94 3.782(2) 145.1 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
C2 P1 S1 Au1 . . . . 69.57(7) ?
C3 P1 S1 Au1 . . . . -54.11(6) ?
C1 P1 S1 Au1 . . . . -172.57(6) y
C2 P1 C1 C12 . . . . -168.83(12) ?
C3 P1 C1 C12 . . . . -44.40(15) ?
S1 P1 C1 C12 . . . . 73.67(13) ?
C2 P1 C1 C11 . . . . -47.57(16) ?
C3 P1 C1 C11 . . . . 76.86(15) ?
S1 P1 C1 C11 . . . . -165.08(13) ?
C2 P1 C1 C13 . . . . 74.52(15) ?
C3 P1 C1 C13 . . . . -161.04(13) ?
S1 P1 C1 C13 . . . . -42.98(14) ?
C3 P1 C2 C22 . . . . -167.85(12) ?
C1 P1 C2 C22 . . . . -43.27(15) ?
S1 P1 C2 C22 . . . . 68.64(13) ?
C3 P1 C2 C21 . . . . -46.59(15) ?
C1 P1 C2 C21 . . . . 77.99(15) ?
S1 P1 C2 C21 . . . . -170.10(11) ?
C3 P1 C2 C23 . . . . 75.38(14) ?
C1 P1 C2 C23 . . . . -160.04(12) ?
S1 P1 C2 C23 . . . . -48.13(14) ?
C2 P1 C3 C33 . . . . -42.58(15) ?
C1 P1 C3 C33 . . . . -166.94(12) ?
S1 P1 C3 C33 . . . . 80.74(13) ?
C2 P1 C3 C31 . . . . 78.30(14) ?
C1 P1 C3 C31 . . . . -46.06(14) ?
S1 P1 C3 C31 . . . . -158.38(11) ?
C2 P1 C3 C32 . . . . -159.88(12) ?
C1 P1 C3 C32 . . . . 75.76(14) ?
S1 P1 C3 C32 . . . . -36.56(13) ?
