#------------------------------------------------------------------------------
#$Date: 2024-10-01 05:15:35 +0300 (Tue, 01 Oct 2024) $
#$Revision: 294951 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023269.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_2023269
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 Br4]'
_chemical_formula_moiety         'C24 H54 Au P2 S2 +, Au Br4 -'
_chemical_formula_sum            'C24 H54 Au2 Br4 P2 S2'
_chemical_formula_weight         1182.30
_chemical_name_common
;
Bis(tri-tert-butylphosphane sulfide)gold(I) tetrabromidoaurate(III)
;
_chemical_name_systematic
;
Bis(tri-tert-butylphosphane sulfide)gold(I) tetrabromidoaurate(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                105.533(4)
_cell_angle_beta                 97.476(4)
_cell_angle_gamma                99.318(4)
_cell_formula_units_Z            1
_cell_length_a                   8.4858(4)
_cell_length_b                   9.3738(4)
_cell_length_c                   11.9910(5)
_cell_measurement_reflns_used    18685
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6703
_cell_measurement_theta_min      2.2998
_cell_volume                     891.63(7)
_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 0.984
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0192
_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            47038
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.739
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            'dichroic red / orange'
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.707
_refine_ls_extinction_coef       0.00106(8)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0116P)²+0.5840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0325
_reflns_number_gt                4754
_reflns_number_total             5273
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5733.cif
_cod_data_source_block           5a
_cod_database_code               2023269
_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   0.306
_shelx_estimated_absorpt_t_max   0.425
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 0.500000 0.500000 0.01767(3) Uani d 1 . .
P P1 0.23519(6) 0.62570(6) 0.31823(4) 0.01195(9) Uani d 1 . .
S S1 0.32147(7) 0.65725(6) 0.49172(4) 0.01907(11) Uani d 1 . .
C C1 0.1193(3) 0.7846(2) 0.32673(19) 0.0179(4) Uani d 1 . .
C C2 0.0947(2) 0.4340(2) 0.25201(18) 0.0161(4) Uani d 1 . .
C C3 0.4086(2) 0.6476(2) 0.23441(18) 0.0148(4) Uani d 1 . .
C C11 0.0041(3) 0.7651(3) 0.2107(2) 0.0229(5) Uani d 1 . .
H H11A -0.046051 0.853518 0.218391 0.034 Uiso calc 1 . .
H H11B -0.080684 0.673822 0.193650 0.034 Uiso calc 1 . .
H H11C 0.065876 0.755553 0.146441 0.034 Uiso calc 1 . .
C C12 0.2391(3) 0.9378(2) 0.3589(2) 0.0242(5) Uani d 1 . .
H H12A 0.294987 0.942582 0.293034 0.036 Uiso calc 1 . .
H H12B 0.319085 0.948369 0.428893 0.036 Uiso calc 1 . .
H H12C 0.179396 1.020062 0.375282 0.036 Uiso calc 1 . .
C C13 0.0190(3) 0.7956(3) 0.4264(2) 0.0255(5) Uani d 1 . .
H H13A 0.092498 0.822098 0.502309 0.038 Uiso calc 1 . .
H H13B -0.054057 0.697986 0.413248 0.038 Uiso calc 1 . .
H H13C -0.045101 0.873804 0.426810 0.038 Uiso calc 1 . .
C C21 0.0490(3) 0.3926(3) 0.11710(18) 0.0214(4) Uani d 1 . .
H H21A -0.032059 0.297666 0.087433 0.032 Uiso calc 1 . .
H H21B 0.146181 0.380317 0.082385 0.032 Uiso calc 1 . .
H H21C 0.003949 0.473460 0.095605 0.032 Uiso calc 1 . .
C C22 -0.0621(3) 0.4321(3) 0.3032(2) 0.0249(5) Uani d 1 . .
H H22A -0.124008 0.499729 0.275828 0.037 Uiso calc 1 . .
H H22B -0.034697 0.466349 0.389330 0.037 Uiso calc 1 . .
H H22C -0.127572 0.328918 0.276980 0.037 Uiso calc 1 . .
C C23 0.1708(3) 0.3088(2) 0.2847(2) 0.0214(4) Uani d 1 . .
H H23A 0.189478 0.328889 0.370358 0.032 Uiso calc 1 . .
H H23B 0.274437 0.307373 0.257067 0.032 Uiso calc 1 . .
H H23C 0.096941 0.210579 0.247410 0.032 Uiso calc 1 . .
C C31 0.3558(3) 0.6877(3) 0.12054(19) 0.0202(4) Uani d 1 . .
H H31A 0.446562 0.692699 0.077889 0.030 Uiso calc 1 . .
H H31B 0.323728 0.785957 0.140472 0.030 Uiso calc 1 . .
H H31C 0.263619 0.609826 0.070876 0.030 Uiso calc 1 . .
C C32 0.5513(3) 0.7717(3) 0.3137(2) 0.0215(4) Uani d 1 . .
H H32A 0.588570 0.743513 0.384194 0.032 Uiso calc 1 . .
H H32B 0.515439 0.867910 0.337020 0.032 Uiso calc 1 . .
H H32C 0.640651 0.782509 0.270440 0.032 Uiso calc 1 . .
C C33 0.4739(3) 0.5008(2) 0.20084(19) 0.0192(4) Uani d 1 . .
H H33A 0.567617 0.516960 0.162526 0.029 Uiso calc 1 . .
H H33B 0.388545 0.419573 0.146635 0.029 Uiso calc 1 . .
H H33C 0.506945 0.472478 0.271985 0.029 Uiso calc 1 . .
Au Au2 0.500000 1.000000 1.000000 0.01376(3) Uani d 1 . .
Br Br1 0.43975(3) 0.87358(2) 0.78998(2) 0.02087(5) Uani d 1 . .
Br Br2 0.77780(3) 0.96487(3) 1.00751(2) 0.02657(5) 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'
Br Br -0.2901 2.4595 '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_666 . 180.0 y
C2 P1 C3 . . 111.22(9) ?
C2 P1 C1 . . 111.27(10) ?
C3 P1 C1 . . 111.39(9) ?
C2 P1 S1 . . 110.08(7) ?
C3 P1 S1 . . 110.94(7) ?
C1 P1 S1 . . 101.58(7) y
P1 S1 Au1 . . 107.15(3) y
C12 C1 C11 . . 108.38(18) ?
C12 C1 C13 . . 106.10(18) ?
C11 C1 C13 . . 108.66(18) ?
C12 C1 P1 . . 110.09(14) ?
C11 C1 P1 . . 113.07(15) ?
C13 C1 P1 . . 110.28(14) ?
C22 C2 C21 . . 108.46(18) ?
C22 C2 C23 . . 105.66(17) ?
C21 C2 C23 . . 109.05(17) ?
C22 C2 P1 . . 109.93(15) ?
C21 C2 P1 . . 112.27(14) ?
C23 C2 P1 . . 111.23(14) ?
C33 C3 C31 . . 108.08(17) ?
C33 C3 C32 . . 106.56(17) ?
C31 C3 C32 . . 109.51(16) ?
C33 C3 P1 . . 110.98(14) ?
C31 C3 P1 . . 111.94(14) ?
C32 C3 P1 . . 109.63(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 ?
Br1 Au2 Br1 . 2_677 180.0 y
Br1 Au2 Br2 . 2_677 89.687(9) y
Br1 Au2 Br2 2_677 2_677 90.313(9) ?
Br1 Au2 Br2 . . 90.312(9) y
Br1 Au2 Br2 2_677 . 89.687(9) ?
Br2 Au2 Br2 2_677 . 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_666 2.2891(5) ?
Au1 S1 . 2.2891(5) y
P1 C2 . 1.892(2) ?
P1 C3 . 1.901(2) ?
P1 C1 . 1.901(2) ?
P1 S1 . 2.0384(7) y
C1 C12 . 1.540(3) ?
C1 C11 . 1.541(3) ?
C1 C13 . 1.546(3) ?
C2 C22 . 1.535(3) ?
C2 C21 . 1.539(3) ?
C2 C23 . 1.540(3) ?
C3 C33 . 1.539(3) ?
C3 C31 . 1.541(3) ?
C3 C32 . 1.541(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 Br1 . 2.4245(2) y
Au2 Br1 2_677 2.4245(2) ?
Au2 Br2 2_677 2.4260(2) ?
Au2 Br2 . 2.4260(2) y
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
C33 H33C Au1 . 0.98 2.69 3.567(2) 149.8 yes
C23 H23A Au1 . 0.98 2.86 3.421(2) 117.5 yes
C22 H22C Br1 2_566 0.98 2.88 3.756(2) 150.0 yes
C12 H12A Br1 2_676 0.98 3.05 3.890(2) 145.2 yes
C32 H32A S1 . 0.98 2.86 3.338(2) 110.9 yes
C23 H23A S1 . 0.98 2.98 3.456(2) 110.8 yes
C13 H13A S1 . 0.98 2.67 3.160(2) 111.5 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 . . . . 71.01(7) ?
C3 P1 S1 Au1 . . . . -52.53(7) ?
C1 P1 S1 Au1 . . . . -171.01(7) y
C2 P1 C1 C12 . . . . -169.51(14) ?
C3 P1 C1 C12 . . . . -44.79(17) ?
S1 P1 C1 C12 . . . . 73.37(15) ?
C2 P1 C1 C11 . . . . -48.13(18) ?
C3 P1 C1 C11 . . . . 76.59(17) ?
S1 P1 C1 C11 . . . . -165.24(14) ?
C2 P1 C1 C13 . . . . 73.75(17) ?
C3 P1 C1 C13 . . . . -161.53(15) ?
S1 P1 C1 C13 . . . . -43.37(16) ?
C3 P1 C2 C22 . . . . -167.67(14) ?
C1 P1 C2 C22 . . . . -42.86(17) ?
S1 P1 C2 C22 . . . . 68.96(15) ?
C3 P1 C2 C21 . . . . -46.85(17) ?
C1 P1 C2 C21 . . . . 77.96(17) ?
S1 P1 C2 C21 . . . . -170.22(13) ?
C3 P1 C2 C23 . . . . 75.67(16) ?
C1 P1 C2 C23 . . . . -159.52(14) ?
S1 P1 C2 C23 . . . . -47.70(16) ?
C2 P1 C3 C33 . . . . -40.99(17) ?
C1 P1 C3 C33 . . . . -165.73(14) ?
S1 P1 C3 C33 . . . . 81.89(15) ?
C2 P1 C3 C31 . . . . 79.86(16) ?
C1 P1 C3 C31 . . . . -44.89(17) ?
S1 P1 C3 C31 . . . . -157.27(13) ?
C2 P1 C3 C32 . . . . -158.42(13) ?
C1 P1 C3 C32 . . . . 76.83(15) ?
S1 P1 C3 C32 . . . . -35.55(15) ?
