#------------------------------------------------------------------------------
#$Date: 2024-08-01 05:19:28 +0300 (Thu, 01 Aug 2024) $
#$Revision: 293619 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023217.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_2023217
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 (C6 H7 N)]'
_chemical_formula_moiety         'C6 H7 Au Br3 N'
_chemical_formula_sum            'C6 H7 Au Br3 N'
_chemical_formula_weight         529.82
_chemical_name_systematic
;
Tribromido(3-methylpyridine-κN)gold(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 118.887(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6763(6)
_cell_length_b                   6.78409(14)
_cell_length_c                   18.4807(5)
_cell_measurement_reflns_used    7609
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2190
_cell_measurement_theta_min      2.4970
_cell_volume                     2050.19(12)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.36.28 (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 0.996
_diffrn_measured_fraction_theta_max 0.957
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40540
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.990
_diffrn_reflns_theta_min         2.491
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.985
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.014
_refine_diff_density_min         -1.714
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0263
_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)+(0.0194P)²+10.7877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                2563
_reflns_number_total             3120
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5729.cif
_cod_data_source_block           3
_cod_original_cell_volume        2050.18(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2023217
_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   0.147
_shelx_estimated_absorpt_t_max   0.625
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.25213(2) 0.25929(2) 0.37416(2) 0.01140(5) Uani d 1 . .
Br Br1 0.10545(3) 0.26127(7) 0.29684(3) 0.01921(10) Uani d 1 . .
Br Br2 0.25822(3) 0.55197(7) 0.30223(3) 0.01973(11) Uani d 1 . .
Br Br3 0.24913(3) -0.02193(7) 0.45387(3) 0.01697(10) Uani d 1 . .
N N11 0.3782(2) 0.2527(5) 0.4343(2) 0.0120(7) Uani d 1 . .
C C12 0.4162(3) 0.2409(6) 0.3884(3) 0.0135(8) Uani d 1 . .
H H12 0.384098 0.233363 0.329940 0.016 Uiso calc 1 . .
C C13 0.4998(3) 0.2393(6) 0.4233(3) 0.0142(9) Uani d 1 . .
C C14 0.5454(3) 0.2506(6) 0.5089(3) 0.0151(9) Uani d 1 . .
H H14 0.603448 0.250258 0.534980 0.018 Uiso calc 1 . .
C C15 0.5065(3) 0.2623(6) 0.5564(3) 0.0150(9) Uani d 1 . .
H H15 0.537267 0.269624 0.614938 0.018 Uiso calc 1 . .
C C16 0.4220(3) 0.2631(6) 0.5169(3) 0.0141(9) Uani d 1 . .
H H16 0.394516 0.271021 0.548698 0.017 Uiso calc 1 . .
C C17 0.5387(3) 0.2290(7) 0.3688(3) 0.0205(10) Uani d 1 . .
H H17A 0.503831 0.151818 0.319215 0.031 Uiso calc 1 . .
H H17B 0.592426 0.165859 0.398891 0.031 Uiso calc 1 . .
H H17C 0.545228 0.362545 0.352579 0.031 Uiso calc 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 Br1 . . 176.62(10) y
N11 Au1 Br2 . . 88.25(10) y
Br1 Au1 Br2 . . 90.649(17) y
N11 Au1 Br3 . . 90.63(10) y
Br1 Au1 Br3 . . 90.653(17) y
Br2 Au1 Br3 . . 176.494(17) y
C16 N11 C12 . . 120.3(4) y
C16 N11 Au1 . . 121.4(3) ?
C12 N11 Au1 . . 118.3(3) ?
N11 C12 C13 . . 122.1(4) ?
N11 C12 H12 . . 119.0 ?
C13 C12 H12 . . 119.0 ?
C12 C13 C14 . . 117.8(4) ?
C12 C13 C17 . . 119.6(4) ?
C14 C13 C17 . . 122.5(4) ?
C15 C14 C13 . . 120.3(4) ?
C15 C14 H14 . . 119.9 ?
C13 C14 H14 . . 119.9 ?
C16 C15 C14 . . 118.7(4) ?
C16 C15 H15 . . 120.7 ?
C14 C15 H15 . . 120.7 ?
N11 C16 C15 . . 120.9(4) ?
N11 C16 H16 . . 119.5 ?
C15 C16 H16 . . 119.5 ?
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 ?
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 . 2.062(4) y
Au1 Br1 . 2.4009(5) y
Au1 Br2 . 2.4225(5) y
Au1 Br3 . 2.4276(5) y
N11 C16 . 1.341(6) y
N11 C12 . 1.346(6) y
C12 C13 . 1.372(6) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.391(6) ?
C13 C17 . 1.501(6) ?
C14 C15 . 1.386(6) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.382(6) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 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
C15 H15 Br1 8_556 0.95 2.97 3.905(5) 167.8 yes
C16 H16 Br1 7_556 0.95 2.86 3.721(5) 150.7 yes
C12 H12 Br2 4_545 0.95 2.88 3.684(4) 143.6 yes
C14 H14 Br3 5_656 0.95 3.08 3.880(5) 143.1 yes
C17 H17B Br3 5_656 0.98 3.06 3.984(5) 158.6 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
Br2 Au1 N11 C16 . . . . 120.5(3) y
Br3 Au1 N11 C16 . . . . -56.1(3) y
Br2 Au1 N11 C12 . . . . -58.4(3) y
Br3 Au1 N11 C12 . . . . 124.9(3) y
C16 N11 C12 C13 . . . . -0.1(6) ?
Au1 N11 C12 C13 . . . . 178.8(3) ?
N11 C12 C13 C14 . . . . 0.0(6) ?
N11 C12 C13 C17 . . . . -179.1(4) ?
C12 C13 C14 C15 . . . . 0.2(6) ?
C17 C13 C14 C15 . . . . 179.2(4) ?
C13 C14 C15 C16 . . . . -0.2(6) ?
C12 N11 C16 C15 . . . . 0.2(6) ?
Au1 N11 C16 C15 . . . . -178.8(3) ?
C14 C15 C16 N11 . . . . 0.0(6) ?
