#------------------------------------------------------------------------------
#$Date: 2024-10-01 05:15:35 +0300 (Tue, 01 Oct 2024) $
#$Revision: 294951 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023270.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_2023270
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 Se1)2] [Au Br4]'
_chemical_formula_moiety         'C24 H54 Au P2 Se2 +, Au Br4 -'
_chemical_formula_sum            'C24 H54 Au2 Br4 P2 Se2'
_chemical_formula_weight         1276.10
_chemical_name_common
;
Bis(tri-tert-butylphosphane selenide)gold(I) tetrabromidoaurate(III)
;
_chemical_name_systematic
;
Bis(tri-tert-butylphosphane selenide-κSe)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                106.172(4)
_cell_angle_beta                 101.100(4)
_cell_angle_gamma                97.485(4)
_cell_formula_units_Z            1
_cell_length_a                   8.4403(4)
_cell_length_b                   9.2135(4)
_cell_length_c                   12.6496(5)
_cell_measurement_reflns_used    14356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7830
_cell_measurement_theta_min      2.3420
_cell_volume                     909.28(8)
_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 0.988
_diffrn_measured_fraction_theta_max 0.944
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0244
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48315
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.852
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            'dichroic red / orange'
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.875
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0204
_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/[σ²(Fo²)+(0.0130P)²+0.5218P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0344
_refine_ls_wR_factor_ref         0.0358
_reflns_number_gt                4704
_reflns_number_total             5398
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5733.cif
_cod_data_source_block           5b
_cod_original_cell_volume        909.28(7)
_cod_database_code               2023270
_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   0.274
_shelx_estimated_absorpt_t_max   0.594
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 0.01861(4) Uani d 1 . .
P P1 0.23823(7) 0.64599(7) 0.31359(5) 0.01078(12) Uani d 1 . .
Se Se1 0.33995(3) 0.69690(3) 0.49665(2) 0.01875(6) Uani d 1 . .
C C1 0.1452(3) 0.8210(3) 0.3065(2) 0.0149(5) Uani d 1 . .
C C2 0.0740(3) 0.4642(3) 0.2605(2) 0.0157(5) Uani d 1 . .
C C3 0.4077(3) 0.6294(3) 0.2335(2) 0.0149(5) Uani d 1 . .
C C11 0.0226(3) 0.7960(3) 0.1928(2) 0.0187(5) Uani d 1 . .
H H11A -0.012248 0.893101 0.191675 0.028 Uiso calc 1 . .
H H11B -0.073718 0.717803 0.183909 0.028 Uiso calc 1 . .
H H11C 0.075797 0.761303 0.130341 0.028 Uiso calc 1 . .
C C12 0.2828(3) 0.9601(3) 0.3281(2) 0.0211(6) Uani d 1 . .
H H12A 0.335033 0.943442 0.264003 0.032 Uiso calc 1 . .
H H12B 0.365231 0.972203 0.397672 0.032 Uiso calc 1 . .
H H12C 0.236033 1.053424 0.336352 0.032 Uiso calc 1 . .
C C13 0.0553(3) 0.8691(3) 0.4026(2) 0.0236(6) Uani d 1 . .
H H13A 0.133672 0.894224 0.476149 0.035 Uiso calc 1 . .
H H13B -0.033236 0.783986 0.394871 0.035 Uiso calc 1 . .
H H13C 0.008642 0.959636 0.397541 0.035 Uiso calc 1 . .
C C21 0.0156(3) 0.4067(3) 0.1300(2) 0.0240(6) Uani d 1 . .
H H21A -0.077729 0.320043 0.106641 0.036 Uiso calc 1 . .
H H21B 0.105937 0.373030 0.097288 0.036 Uiso calc 1 . .
H H21C -0.018463 0.490517 0.103187 0.036 Uiso calc 1 . .
C C22 -0.0744(3) 0.4956(3) 0.3114(3) 0.0247(6) Uani d 1 . .
H H22A -0.125847 0.570296 0.281828 0.037 Uiso calc 1 . .
H H22B -0.037130 0.537331 0.394132 0.037 Uiso calc 1 . .
H H22C -0.154595 0.399274 0.290525 0.037 Uiso calc 1 . .
C C23 0.1345(3) 0.3327(3) 0.2995(2) 0.0213(6) Uani d 1 . .
H H23A 0.165564 0.364689 0.382498 0.032 Uiso calc 1 . .
H H23B 0.230240 0.308679 0.269764 0.032 Uiso calc 1 . .
H H23C 0.046253 0.241134 0.270923 0.032 Uiso calc 1 . .
C C31 0.3563(3) 0.6577(3) 0.1182(2) 0.0222(6) Uani d 1 . .
H H31A 0.445177 0.645911 0.078661 0.033 Uiso calc 1 . .
H H31B 0.334466 0.762354 0.130622 0.033 Uiso calc 1 . .
H H31C 0.256479 0.582947 0.072048 0.033 Uiso calc 1 . .
C C32 0.5661(3) 0.7457(3) 0.3056(2) 0.0218(6) Uani d 1 . .
H H32A 0.603830 0.722334 0.376128 0.033 Uiso calc 1 . .
H H32B 0.543344 0.850345 0.323377 0.033 Uiso calc 1 . .
H H32C 0.651798 0.738455 0.262964 0.033 Uiso calc 1 . .
C C33 0.4516(3) 0.4686(3) 0.2097(2) 0.0196(5) Uani d 1 . .
H H33A 0.543109 0.465501 0.172319 0.029 Uiso calc 1 . .
H H33B 0.355681 0.391299 0.160333 0.029 Uiso calc 1 . .
H H33C 0.483986 0.446471 0.281408 0.029 Uiso calc 1 . .
Au Au2 0.500000 1.000000 1.000000 0.01304(3) Uani d 1 . .
Br Br1 0.38051(3) 0.89229(3) 0.79758(2) 0.02139(6) Uani d 1 . .
Br Br2 0.77027(3) 0.96169(3) 0.97214(2) 0.02058(6) 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'
Se Se -0.0929 2.2259 '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
Se1 Au1 Se1 . 2_666 180.0 ?
C2 P1 C1 . . 111.15(11) ?
C2 P1 C3 . . 111.98(11) ?
C1 P1 C3 . . 110.57(11) ?
C2 P1 Se1 . . 109.06(8) ?
C1 P1 Se1 . . 102.74(8) y
C3 P1 Se1 . . 110.96(8) ?
P1 Se1 Au1 . . 101.806(19) y
C12 C1 C11 . . 109.1(2) ?
C12 C1 C13 . . 105.1(2) ?
C11 C1 C13 . . 108.1(2) ?
C12 C1 P1 . . 109.79(17) ?
C11 C1 P1 . . 113.56(17) ?
C13 C1 P1 . . 110.76(17) ?
C22 C2 C23 . . 106.1(2) ?
C22 C2 C21 . . 109.1(2) ?
C23 C2 C21 . . 108.2(2) ?
C22 C2 P1 . . 109.27(17) ?
C23 C2 P1 . . 111.81(16) ?
C21 C2 P1 . . 112.14(17) ?
C33 C3 C32 . . 106.7(2) ?
C33 C3 C31 . . 107.3(2) ?
C32 C3 C31 . . 109.5(2) ?
C33 C3 P1 . . 111.40(17) ?
C32 C3 P1 . . 109.97(17) ?
C31 C3 P1 . . 111.73(17) ?
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 . 89.101(10) ?
Br1 Au2 Br2 . . 90.899(10) y
Br1 Au2 Br2 2_677 2_677 90.898(10) ?
Br1 Au2 Br2 . 2_677 89.102(10) y
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 Se1 . 2.4036(3) y
Au1 Se1 2_666 2.4036(3) ?
P1 C2 . 1.895(2) ?
P1 C1 . 1.900(2) ?
P1 C3 . 1.904(2) ?
P1 Se1 . 2.2009(6) y
C1 C12 . 1.537(3) ?
C1 C11 . 1.541(3) ?
C1 C13 . 1.547(3) ?
C2 C22 . 1.538(4) ?
C2 C23 . 1.538(3) ?
C2 C21 . 1.543(4) ?
C3 C33 . 1.537(3) ?
C3 C32 . 1.543(3) ?
C3 C31 . 1.543(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_677 2.4265(3) ?
Au2 Br1 . 2.4265(3) y
Au2 Br2 . 2.4295(3) y
Au2 Br2 2_677 2.4295(3) ?
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 2.64 3.540(3) 152.3 yes
C23 H23A Au1 . 0.98 2.86 3.449(3) 119.6 yes
C22 H22C Br1 2_566 0.98 2.88 3.851(3) 172.9 yes
C12 H12A Br1 2_676 0.98 3.02 3.793(3) 137.2 yes
C32 H32A Se1 . 0.98 2.95 3.442(3) 112.1 yes
C23 H23A Se1 . 0.98 3.03 3.556(3) 115.1 yes
C13 H13A Se1 . 0.98 2.70 3.263(3) 116.6 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 Se1 Au1 . . . . 72.38(9) ?
C1 P1 Se1 Au1 . . . . -169.62(8) y
C3 P1 Se1 Au1 . . . . -51.43(8) ?
C2 P1 C1 C12 . . . . -169.27(17) ?
C3 P1 C1 C12 . . . . -44.3(2) ?
Se1 P1 C1 C12 . . . . 74.22(17) ?
C2 P1 C1 C11 . . . . -46.8(2) ?
C3 P1 C1 C11 . . . . 78.21(19) ?
Se1 P1 C1 C11 . . . . -163.33(16) ?
C2 P1 C1 C13 . . . . 75.1(2) ?
C3 P1 C1 C13 . . . . -159.92(17) ?
Se1 P1 C1 C13 . . . . -41.45(18) ?
C1 P1 C2 C22 . . . . -44.8(2) ?
C3 P1 C2 C22 . . . . -168.98(17) ?
Se1 P1 C2 C22 . . . . 67.81(18) ?
C1 P1 C2 C23 . . . . -161.96(18) ?
C3 P1 C2 C23 . . . . 73.8(2) ?
Se1 P1 C2 C23 . . . . -49.39(19) ?
C1 P1 C2 C21 . . . . 76.3(2) ?
C3 P1 C2 C21 . . . . -47.9(2) ?
Se1 P1 C2 C21 . . . . -171.13(16) ?
C2 P1 C3 C33 . . . . -39.8(2) ?
C1 P1 C3 C33 . . . . -164.31(17) ?
Se1 P1 C3 C33 . . . . 82.36(17) ?
C2 P1 C3 C32 . . . . -157.89(17) ?
C1 P1 C3 C32 . . . . 77.56(19) ?
Se1 P1 C3 C32 . . . . -35.76(18) ?
C2 P1 C3 C31 . . . . 80.3(2) ?
C1 P1 C3 C31 . . . . -44.3(2) ?
Se1 P1 C3 C31 . . . . -157.59(16) ?
