#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:00:57 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/84/7048474.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7048474
loop_
_publ_author_name
'Mertens, R. Tyler'
'Kim, Jong Hyun'
'Jennings, Will C.'
'Parkin, Sean'
'Awuah, Samuel G.'
_publ_section_title
;
 Revisiting the reactivity of tetrachloroauric acid with N,N-bidentate
 ligands: structural and spectroscopic insights.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2093
_journal_page_last               2099
_journal_paper_doi               10.1039/c8dt04960b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H8 Au Cl2 N2, 0.5(Au Cl4), 0.5(Au Cl2)'
_chemical_formula_sum            'C12 H8 Au2 Cl5 N2'
_chemical_formula_weight         751.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2017 and CIFFIX/1'
_audit_update_record
;
2018-09-18 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                84.463(1)
_cell_angle_beta                 77.729(1)
_cell_angle_gamma                87.429(1)
_cell_formula_units_Z            2
_cell_length_a                   7.4092(2)
_cell_length_b                   7.7822(2)
_cell_length_c                   14.3986(3)
_cell_measurement_reflns_used    9150
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.81
_cell_volume                     807.22(3)
_computing_cell_refinement       'APEX3 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELX (Sheldrick, 2008) and CIFFIX (Parkin, 2013)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21007
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.814
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    18.972
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_description       'small block cut from needle'
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00121(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0122
_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/[σ²(Fo²)+0.8980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0254
_refine_ls_wR_factor_ref         0.0257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3541
_reflns_number_total             3691
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04960b2.cif
_cod_data_source_block           m17109
_cod_depositor_comments
'Adding full bibliography for 7048474--7048479.cif.'
_cod_database_code               7048474
_shelx_shelxl_version_number     2017/1
_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   0.396
_shelx_estimated_absorpt_t_max   0.451
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Au3 Au 1.000000 0.500000 0.500000 0.01097(4) Uani 1 2 d S . P
Cl4 Cl 0.69036(9) 0.52575(8) 0.55898(5) 0.02032(14) Uani 1 1 d . . .
Cl5 Cl 1.02626(9) 0.79288(7) 0.48048(5) 0.01716(13) Uani 1 1 d . . .
Au1 Au 0.38824(2) 0.47040(2) 0.77466(2) 0.01446(3) Uani 1 1 d . . .
Cl1 Cl 0.3651(1) 0.70674(8) 0.85622(5) 0.02362(14) Uani 1 1 d . . .
Cl2 Cl 0.14303(10) 0.56819(9) 0.71270(5) 0.02218(14) Uani 1 1 d . . .
N1 N 0.6197(3) 0.3739(3) 0.81905(16) 0.0168(5) Uani 1 1 d . . .
N2 N 0.4182(3) 0.2473(3) 0.70860(15) 0.0147(4) Uani 1 1 d . . .
C1 C 0.7089(4) 0.4378(4) 0.8780(2) 0.0216(6) Uani 1 1 d . . .
H1 H 0.668737 0.544940 0.902840 0.026 Uiso 1 1 calc R U .
C2 C 0.8609(4) 0.3494(4) 0.9039(2) 0.0243(6) Uani 1 1 d . . .
H2 H 0.924355 0.397372 0.945734 0.029 Uiso 1 1 calc R U .
C3 C 0.9195(4) 0.1942(4) 0.8696(2) 0.0229(6) Uani 1 1 d . . .
H3 H 1.021737 0.133544 0.888575 0.028 Uiso 1 1 calc R U .
C4 C 0.8282(4) 0.1246(4) 0.80625(19) 0.0180(5) Uani 1 1 d . . .
C5 C 0.6760(4) 0.2188(3) 0.78314(18) 0.0156(5) Uani 1 1 d . . .
C6 C 0.5706(4) 0.1523(3) 0.72496(18) 0.0145(5) Uani 1 1 d . . .
C7 C 0.6177(4) -0.0067(3) 0.68717(18) 0.0162(5) Uani 1 1 d . . .
C8 C 0.5030(4) -0.0641(3) 0.63148(19) 0.0184(5) Uani 1 1 d . . .
H8 H 0.531639 -0.170259 0.603437 0.022 Uiso 1 1 calc R U .
C9 C 0.3501(4) 0.0309(3) 0.61701(19) 0.0189(6) Uani 1 1 d . . .
H9 H 0.271103 -0.010258 0.580446 0.023 Uiso 1 1 calc R U .
C10 C 0.3109(4) 0.1893(3) 0.65652(19) 0.0177(5) Uani 1 1 d . . .
H10 H 0.205674 0.256099 0.645740 0.021 Uiso 1 1 calc R U .
C11 C 0.8753(4) -0.0385(4) 0.76779(19) 0.0202(6) Uani 1 1 d . . .
H11 H 0.978181 -0.104094 0.782810 0.024 Uiso 1 1 calc R U .
C12 C 0.7758(4) -0.1003(3) 0.71058(19) 0.0190(6) Uani 1 1 d . . .
H12 H 0.811074 -0.207965 0.685255 0.023 Uiso 1 1 calc R U .
Au2 Au 0.500000 0.000000 1.000000 0.01622(4) Uani 1 2 d S . P
Cl3 Cl 0.27884(9) 0.20559(9) 0.98335(5) 0.02108(14) Uani 1 1 d . . .
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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl4 Au3 Cl4 180.0 2_766 .
Cl4 Au3 Cl5 91.18(2) 2_766 2_766
Cl4 Au3 Cl5 88.82(2) . 2_766
Cl4 Au3 Cl5 88.82(2) 2_766 .
Cl4 Au3 Cl5 91.19(2) . .
Cl5 Au3 Cl5 180.0 2_766 .
N2 Au1 N1 81.98(9) . .
N2 Au1 Cl1 175.72(6) . .
N1 Au1 Cl1 94.29(7) . .
N2 Au1 Cl2 94.01(6) . .
N1 Au1 Cl2 174.85(6) . .
Cl1 Au1 Cl2 89.84(3) . .
C1 N1 C5 120.1(2) . .
C1 N1 Au1 128.58(19) . .
C5 N1 Au1 111.26(17) . .
C10 N2 C6 120.2(2) . .
C10 N2 Au1 128.26(18) . .
C6 N2 Au1 111.50(17) . .
N1 C1 C2 120.7(3) . .
N1 C1 H1 119.7 . .
C2 C1 H1 119.7 . .
C3 C2 C1 120.5(3) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C2 C3 C4 119.9(3) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 117.0(3) . .
C5 C4 C11 118.4(2) . .
C3 C4 C11 124.5(3) . .
N1 C5 C4 121.8(2) . .
N1 C5 C6 117.8(2) . .
C4 C5 C6 120.3(2) . .
N2 C6 C7 121.5(2) . .
N2 C6 C5 117.4(2) . .
C7 C6 C5 121.0(2) . .
C8 C7 C6 117.1(2) . .
C8 C7 C12 125.1(2) . .
C6 C7 C12 117.8(2) . .
C9 C8 C7 120.7(2) . .
C9 C8 H8 119.7 . .
C7 C8 H8 119.7 . .
C8 C9 C10 119.4(3) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C10 C9 121.0(2) . .
N2 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
C12 C11 C4 121.0(2) . .
C12 C11 H11 119.5 . .
C4 C11 H11 119.5 . .
C11 C12 C7 121.4(3) . .
C11 C12 H12 119.3 . .
C7 C12 H12 119.3 . .
Cl3 Au2 Cl3 180.0 . 2_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au3 Cl4 2.2777(6) 2_766
Au3 Cl4 2.2777(6) .
Au3 Cl5 2.2814(6) 2_766
Au3 Cl5 2.2814(6) .
Au1 N2 2.040(2) .
Au1 N1 2.042(2) .
Au1 Cl1 2.2570(7) .
Au1 Cl2 2.2605(7) .
N1 C1 1.324(4) .
N1 C5 1.372(3) .
N2 C10 1.322(3) .
N2 C6 1.372(3) .
C1 C2 1.393(4) .
C1 H1 0.9500 .
C2 C3 1.366(4) .
C2 H2 0.9500 .
C3 C4 1.405(4) .
C3 H3 0.9500 .
C4 C5 1.399(4) .
C4 C11 1.433(4) .
C5 C6 1.406(4) .
C6 C7 1.400(4) .
C7 C8 1.399(4) .
C7 C12 1.435(4) .
C8 C9 1.367(4) .
C8 H8 0.9500 .
C9 C10 1.400(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.349(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
Au2 Cl3 2.2716(7) .
Au2 Cl3 2.2716(7) 2_657
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
C5 N1 C1 C2 0.3(4)
Au1 N1 C1 C2 177.0(2)
N1 C1 C2 C3 -0.7(4)
C1 C2 C3 C4 1.3(4)
C2 C3 C4 C5 -1.5(4)
C2 C3 C4 C11 -178.5(3)
C1 N1 C5 C4 -0.6(4)
Au1 N1 C5 C4 -177.8(2)
C1 N1 C5 C6 176.7(2)
Au1 N1 C5 C6 -0.5(3)
C3 C4 C5 N1 1.2(4)
C11 C4 C5 N1 178.4(2)
C3 C4 C5 C6 -176.0(2)
C11 C4 C5 C6 1.2(4)
C10 N2 C6 C7 0.3(4)
Au1 N2 C6 C7 179.50(19)
C10 N2 C6 C5 -178.2(2)
Au1 N2 C6 C5 0.9(3)
N1 C5 C6 N2 -0.3(3)
C4 C5 C6 N2 177.0(2)
N1 C5 C6 C7 -178.9(2)
C4 C5 C6 C7 -1.5(4)
N2 C6 C7 C8 0.3(4)
C5 C6 C7 C8 178.9(2)
N2 C6 C7 C12 -177.9(2)
C5 C6 C7 C12 0.6(4)
C6 C7 C8 C9 -1.3(4)
C12 C7 C8 C9 176.8(3)
C7 C8 C9 C10 1.6(4)
C6 N2 C10 C9 -0.1(4)
Au1 N2 C10 C9 -179.09(19)
C8 C9 C10 N2 -0.9(4)
C5 C4 C11 C12 0.0(4)
C3 C4 C11 C12 177.0(3)
C4 C11 C12 C7 -0.9(4)
C8 C7 C12 C11 -177.5(3)
C6 C7 C12 C11 0.6(4)
