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)
Upmann, Daniel; Bockfeld, Dirk; Jones, Peter G.; Târcoveanu, Eliza; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1087–1096; doi:10.1107/S2056989024009095

data_2023269
_publ_section_title
;
 Crystal structures of seven mixed-valence gold compounds of the form [(R
 1 R 2 R 3PE)2AuI]+[AuIII X 4]&#x2212; (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-<i>tert</i>-butylphosphane sulfide)gold(I) tetrabromidoaurate(III)
;
_chemical_name_systematic
;
Bis(tri-<i>tert</i>-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
;
<i>SHELXL2019/3</i> (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       '\w 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
;<i>F</i>~c~^*^ =
 <i>kF</i>~c~[1+0.001\\times<i>F</i>~c~^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_extinction_method
;
<i>SHELXL2019/3</i> (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/[\s^2^(Fo^2^)+(0.0116P)^2^+0.5840P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            wm5733.cif
_cod_data_source_block           5a
_cod_database_code               2023269
_shelx_estimated_absorpt_t_min   0.306
_shelx_estimated_absorpt_t_max   0.425
_shelx_hkl_checksum              66123
_shelx_res_checksum              60032