#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:06:04 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293998 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023168.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_2023168
loop_
_publ_author_name
'Döring, Cindy'
'Jones, Peter G.'
_publ_section_title
;
 Crystal structures of four gold(I) complexes [AuL
 ₂]⁺[AuX ₂]⁻ and a
 by-product
 (L·LH⁺)[AuBr₂]⁻
 (L = substituted pyridine, X = Cl or Br).
;
_journal_coeditor_code           YZ2055
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              729
_journal_page_last               737
_journal_paper_doi               10.1107/S2056989024005437
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Au (C6 H7 N)2] [Au Br2]'
_chemical_formula_moiety         'C12 H14 Au N2 +, Au Br2 -'
_chemical_formula_sum            'C12 H14 Au2 Br2 N2'
_chemical_formula_weight         740.00
_chemical_name_systematic
;
Bis(3-methylpyridine)gold(I) dibromidoaurate(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 120.415(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7380(6)
_cell_length_b                   6.44097(13)
_cell_length_c                   8.1923(3)
_cell_measurement_reflns_used    11080
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6520
_cell_measurement_theta_min      2.8270
_cell_volume                     761.66(6)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2014)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2014)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2014)
;
_computing_molecular_graphics
;
Bruker XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.966
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25258
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.906
_diffrn_reflns_theta_min         2.822
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.930
_refine_ls_extinction_coef       0.00089(6)
_refine_ls_extinction_expression
'Fc^*^ = kFc[1 + 0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method
;
SHELXL2019/3 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1255
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0128
_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)+(0.0135P)²+1.2949P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0283
_refine_ls_wR_factor_ref         0.0293
_reflns_number_gt                1162
_reflns_number_total             1255
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yz2055.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2023167--2023171.cif.'
_cod_original_cell_volume        761.65(5)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2023168
_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   0.120
_shelx_estimated_absorpt_t_max   0.193
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.000000 0.000000 0.000000 0.01689(5) Uani d 1 . .
Au Au2 0.000000 0.500000 0.000000 0.01495(5) Uani d 1 . .
Br Br1 0.04670(2) 0.500000 0.32827(5) 0.02509(8) Uani d 1 . .
N N11 0.11729(18) 0.000000 -0.0135(4) 0.0162(5) Uani d 1 . .
C C12 0.1127(2) 0.000000 -0.1827(4) 0.0169(6) Uani d 1 . .
H H12 0.053400 0.000000 -0.294313 0.020 Uiso calc 1 . .
C C13 0.1909(2) 0.000000 -0.2013(4) 0.0162(6) Uani d 1 . .
C C14 0.2766(2) 0.000000 -0.0343(5) 0.0172(6) Uani d 1 . .
H H14 0.331892 0.000000 -0.040186 0.021 Uiso calc 1 . .
C C15 0.2820(2) 0.000000 0.1388(5) 0.0192(6) Uani d 1 . .
H H15 0.340530 0.000000 0.252323 0.023 Uiso calc 1 . .
C C16 0.2012(2) 0.000000 0.1456(5) 0.0185(6) Uani d 1 . .
H H16 0.204838 0.000000 0.265147 0.022 Uiso calc 1 . .
C C17 0.1818(2) 0.000000 -0.3930(5) 0.0236(7) Uani d 1 . .
H H17A 0.153(2) 0.125(5) -0.465(5) 0.052(10) Uiso d 1 . .
H H17B 0.243(3) 0.000000 -0.380(8) 0.059(16) Uiso 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'
N N 0.0061 0.0033 '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
N11 Au1 N11 . 5 180.0 y
N11 Au1 Au2 . . 90.0 ?
N11 Au1 Au2 5 . 90.0 ?
N11 Au1 Au2 . 1_545 90.0 ?
N11 Au1 Au2 5 1_545 90.0 ?
Au2 Au1 Au2 . 1_545 180.0 y
Br1 Au2 Br1 5_565 . 180.0 y
Br1 Au2 Au1 5_565 . 90.0 ?
Br1 Au2 Au1 . . 90.0 y
Br1 Au2 Au1 5_565 1_565 90.0 ?
Br1 Au2 Au1 . 1_565 90.0 ?
Au1 Au2 Au1 . 1_565 180.0 y
C16 N11 C12 . . 118.9(3) y
C16 N11 Au1 . . 120.8(2) ?
C12 N11 Au1 . . 120.3(2) ?
N11 C12 C13 . . 123.0(3) ?
N11 C12 H12 . . 118.5 ?
C13 C12 H12 . . 118.5 ?
C12 C13 C14 . . 116.8(3) ?
C12 C13 C17 . . 120.8(3) ?
C14 C13 C17 . . 122.4(3) ?
C15 C14 C13 . . 120.6(3) ?
C15 C14 H14 . . 119.7 ?
C13 C14 H14 . . 119.7 ?
C14 C15 C16 . . 119.2(3) ?
C14 C15 H15 . . 120.4 ?
C16 C15 H15 . . 120.4 ?
N11 C16 C15 . . 121.5(3) ?
N11 C16 H16 . . 119.2 ?
C15 C16 H16 . . 119.2 ?
C13 C17 H17A . . 113(2) ?
C13 C17 H17B . . 110(3) ?
H17A C17 H17B . . 104(3) ?
C13 C17 H17A . 6 113(2) ?
H17A C17 H17A . 6 112(4) ?
H17B C17 H17A . 6 104(3) ?
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 N11 . 2.021(3) y
Au1 N11 5 2.021(3) ?
Au1 Au2 . 3.22048(6) y
Au1 Au2 1_545 3.22048(6) ?
Au2 Br1 5_565 2.3906(3) ?
Au2 Br1 . 2.3906(3) y
N11 C16 . 1.348(4) ?
N11 C12 . 1.349(4) ?
C12 C13 . 1.391(4) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.394(4) ?
C13 C17 . 1.499(5) ?
C14 C15 . 1.375(5) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.381(5) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
C17 H17A . 0.97(3) ?
C17 H17B . 0.98(3) ?
C17 H17A 6 0.97(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
C15 H15 Br1 7_556 0.95 2.97 3.822(3) 150.5 yes
C14 H14 Au2 3_545 0.95 2.66 3.604(3) 171.4 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
N11 Au1 Au2 Br1 . . . . -106.73(8) y
N11 Au1 Au2 Br1 5 . . . 73.27(8) y
C16 N11 C12 C13 . . . . 0.000000 ?
Au1 N11 C12 C13 . . . . 180.000000 ?
N11 C12 C13 C14 . . . . 0.000000 ?
N11 C12 C13 C17 . . . . 180.0000(10) ?
C12 C13 C14 C15 . . . . 0.000000 ?
C17 C13 C14 C15 . . . . 180.0000(10) ?
C13 C14 C15 C16 . . . . 0.000000 ?
C12 N11 C16 C15 . . . . 0.000000 ?
Au1 N11 C16 C15 . . . . 180.000000 ?
C14 C15 C16 N11 . . . . 0.000000 ?
