#------------------------------------------------------------------------------
#$Date: 2024-08-01 05:19:28 +0300 (Thu, 01 Aug 2024) $
#$Revision: 293619 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023220.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_2023220
loop_
_publ_author_name
'Döring, Cindy'
'Jones, Peter G.'
_publ_section_title
;
 Crystal structures of seven gold(III) complexes of the form LAuX 3 (L =
 substituted pyridine, X = Cl or Br)
;
_journal_coeditor_code           WM5729
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              894
_journal_page_last               909
_journal_paper_doi               10.1107/S2056989024007266
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Au Br3 (C7 H9 N)]'
_chemical_formula_moiety         'C7 H9 Au Br3 N'
_chemical_formula_sum            'C7 H9 Au Br3 N'
_chemical_formula_weight         543.85
_chemical_name_systematic
;
Tribromido(3,5-dimethylpyridine-κN)gold(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                113.828(4)
_cell_angle_beta                 103.543(4)
_cell_angle_gamma                98.368(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2506(3)
_cell_length_b                   8.4726(4)
_cell_length_c                   9.4210(4)
_cell_measurement_reflns_used    9505
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4990
_cell_measurement_theta_min      2.4850
_cell_volume                     563.93(5)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
Bruker XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL-2019/3 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL-2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.938
_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  0.0712
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30785
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.098
_diffrn_reflns_theta_min         2.498
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.622
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0271
_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)+(0.0212P)²+1.2689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                3017
_reflns_number_total             3392
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5729.cif
_cod_data_source_block           6
_cod_database_code               2023220
_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   0.081
_shelx_estimated_absorpt_t_max   0.698
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 0.12370(2) 0.25661(2) 0.49051(2) 0.01349(6) Uani d 1 . .
Br Br1 0.03437(6) 0.14810(6) 0.19990(6) 0.01893(10) Uani d 1 . .
Br Br2 0.40986(6) 0.22579(7) 0.48839(6) 0.02386(11) Uani d 1 . .
Br Br3 -0.16592(6) 0.28402(6) 0.48783(6) 0.01976(10) Uani d 1 . .
N N11 0.2017(4) 0.3438(5) 0.7424(5) 0.0147(7) Uani d 1 . .
C C12 0.2688(6) 0.2381(6) 0.8004(6) 0.0168(9) Uani d 1 . .
H H12 0.279048 0.126752 0.726372 0.020 Uiso calc 1 . .
C C13 0.3231(5) 0.2900(6) 0.9669(6) 0.0158(9) Uani d 1 . .
C C14 0.3052(6) 0.4523(6) 1.0705(6) 0.0190(9) Uani d 1 . .
H H14 0.340733 0.489516 1.185204 0.023 Uiso calc 1 . .
C C15 0.2367(6) 0.5623(6) 1.0112(6) 0.0151(8) Uani d 1 . .
C C16 0.1850(6) 0.5024(6) 0.8425(6) 0.0166(9) Uani d 1 . .
H H16 0.137385 0.574253 0.797647 0.020 Uiso calc 1 . .
C C17 0.4003(6) 0.1710(7) 1.0302(6) 0.0214(10) Uani d 1 . .
H H17A 0.521624 0.232331 1.097981 0.032 Uiso calc 1 . .
H H17B 0.394076 0.059044 0.937453 0.032 Uiso calc 1 . .
H H17C 0.335545 0.144135 1.096319 0.032 Uiso calc 1 . .
C C18 0.2204(7) 0.7414(6) 1.1209(6) 0.0214(10) Uani d 1 . .
H H18A 0.124462 0.770022 1.061149 0.032 Uiso calc 0.5 . .
H H18B 0.328297 0.833284 1.156030 0.032 Uiso calc 0.5 . .
H H18C 0.197840 0.737961 1.217411 0.032 Uiso calc 0.5 . .
H H18D 0.309270 0.790823 1.228578 0.032 Uiso calc 0.5 . .
H H18E 0.105436 0.727561 1.133697 0.032 Uiso calc 0.5 . .
H H18F 0.235893 0.822884 1.072316 0.032 Uiso calc 0.5 . .
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0082
0 0 -1 0.0082
1 0 0 0.0680
-1 0 0 0.0663
-1 5 -2 0.1145
0 -5 3 0.0804
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 Br1 . . 178.39(10) y
N11 Au1 Br2 . . 90.03(10) y
Br1 Au1 Br2 . . 89.437(17) y
N11 Au1 Br3 . . 90.85(10) y
Br1 Au1 Br3 . . 89.674(17) y
Br2 Au1 Br3 . . 179.045(17) y
C16 N11 C12 . . 121.8(4) y
C16 N11 Au1 . . 120.0(3) ?
C12 N11 Au1 . . 118.2(3) ?
N11 C12 C13 . . 120.5(4) ?
N11 C12 H12 . . 119.7 ?
C13 C12 H12 . . 119.7 ?
C14 C13 C12 . . 118.0(4) ?
C14 C13 C17 . . 122.1(4) ?
C12 C13 C17 . . 119.9(4) ?
C13 C14 C15 . . 121.6(5) ?
C13 C14 H14 . . 119.2 ?
C15 C14 H14 . . 119.2 ?
C14 C15 C16 . . 117.5(4) ?
C14 C15 C18 . . 122.9(4) ?
C16 C15 C18 . . 119.7(4) ?
N11 C16 C15 . . 120.5(4) ?
N11 C16 H16 . . 119.7 ?
C15 C16 H16 . . 119.7 ?
C13 C17 H17A . . 109.5 ?
C13 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C13 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C15 C18 H18A . . 109.5 ?
C15 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C15 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C15 C18 H18D . . 109.5 ?
H18A C18 H18D . . 141.1 ?
H18B C18 H18D . . 56.3 ?
H18C C18 H18D . . 56.3 ?
C15 C18 H18E . . 109.5 ?
H18A C18 H18E . . 56.3 ?
H18B C18 H18E . . 141.1 ?
H18C C18 H18E . . 56.3 ?
H18D C18 H18E . . 109.5 ?
C15 C18 H18F . . 109.5 ?
H18A C18 H18F . . 56.3 ?
H18B C18 H18F . . 56.3 ?
H18C C18 H18F . . 141.1 ?
H18D C18 H18F . . 109.5 ?
H18E C18 H18F . . 109.5 ?
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 . 2.078(4) y
Au1 Br1 . 2.3892(5) y
Au1 Br2 . 2.4167(5) y
Au1 Br3 . 2.4295(4) y
N11 C16 . 1.344(6) y
N11 C12 . 1.344(6) ?
C12 C13 . 1.382(7) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.381(6) ?
C13 C17 . 1.508(6) ?
C14 C15 . 1.388(6) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.391(6) ?
C15 C18 . 1.499(6) ?
C16 H16 . 0.9500 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 H18A . 0.9800 ?
C18 H18B . 0.9800 ?
C18 H18C . 0.9800 ?
C18 H18D . 0.9800 ?
C18 H18E . 0.9800 ?
C18 H18F . 0.9800 ?
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
C16 H16 Br1 2_566 0.95 2.91 3.792(4) 154.4 yes
C17 H17C Br1 1_556 0.98 2.87 3.749(5) 149.0 yes
C18 H18A Br1 2_566 0.98 2.89 3.784(5) 151.3 yes
C18 H18C Br3 2_567 0.98 2.93 3.902(5) 173.7 yes
C14 H14 Br2 2_667 0.95 3.02 3.826(5) 143.8 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
Br2 Au1 N11 C16 . . . . 124.0(3) y
Br3 Au1 N11 C16 . . . . -56.3(3) y
Br2 Au1 N11 C12 . . . . -55.8(3) y
Br3 Au1 N11 C12 . . . . 123.9(3) y
C16 N11 C12 C13 . . . . 0.1(6) ?
Au1 N11 C12 C13 . . . . 179.9(3) ?
N11 C12 C13 C14 . . . . 0.4(6) ?
N11 C12 C13 C17 . . . . -179.2(4) ?
C12 C13 C14 C15 . . . . -0.6(7) ?
C17 C13 C14 C15 . . . . 178.9(4) ?
C13 C14 C15 C16 . . . . 0.5(6) ?
C13 C14 C15 C18 . . . . -178.2(4) ?
C12 N11 C16 C15 . . . . -0.2(6) ?
Au1 N11 C16 C15 . . . . 180.0(3) ?
C14 C15 C16 N11 . . . . -0.1(6) ?
C18 C15 C16 N11 . . . . 178.7(4) ?
