#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:00:57 +0100 (jue 07 de nov de 2019) $
#$Revision: 224163 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/84/7048476.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_7048476
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, Cl'
_chemical_formula_sum            'C12 H8 Au Cl3 N2'
_chemical_formula_weight         483.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-09-18 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2927(17)
_cell_length_b                   17.827(3)
_cell_length_c                   6.4414(8)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.61
_cell_volume                     1296.8(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-2018/3 (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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0934
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16820
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         3.608
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    11.943
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.477
_exptl_crystal_description       tablet
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.863
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0362
_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)+(0.0297P)²+21.4312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                782
_reflns_number_total             857
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04960b2.cif
_cod_data_source_block           m18128
_cod_depositor_comments
'Adding full bibliography for 7048474--7048479.cif.'
_cod_original_cell_volume        1296.7(3)
_cod_database_code               7048476
_shelx_shelxl_version_number     2018/3
_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   0.448
_shelx_estimated_absorpt_t_max   0.716
_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. 
;
_shelx_res_file
; 
TITL m18128.res in Cmcm 
    m18128.res 
    created by SHELXL-2018/3 at 11:08:26 on 27-Jun-2018 
CELL  0.71073  11.2927  17.8268   6.4414   90.000   90.000   90.000 
ZERR    4.000   0.0017   0.0026   0.0008    0.000    0.000    0.000 
LATT  7 
SYMM -X, -Y, 1/2+Z 
SYMM -X, Y, 1/2-Z 
SYMM X, -Y, -Z 
SFAC C H AU CL N 
UNIT 48 32 4 12 8 
TEMP -183 
SIZE 0.08 0.04 0.03 
REM COLR yellow 
REM FORM tablet 
REM The crystal was not single.  There were at least three slightly 
REM mis-aligned pieces. 
OMIT 1 1 0 
L.S. 10 
BOND $H 
LIST 4 
ACTA 
CONF 
HTAB 
FMAP 2 
PLAN 5 
WGHT    0.029700   21.431200 
FVAR       0.13381 
AU1   3    0.500000    0.758663    0.750000    10.25000    0.03057    0.02863 = 
         0.02833    0.00000    0.00000    0.00000 
C1    1    0.262763    0.675399    0.750000    10.50000    0.02247    0.03507 = 
         0.02824    0.00000    0.00000    0.00133 
AFIX  43 
H1    2    0.224384    0.722821    0.750000    10.50000   -1.20000 
AFIX   0 
CL1   4    0.642009    0.848031    0.750000    10.50000    0.04429    0.03278 = 
         0.03634    0.00000    0.00000   -0.00889 
N1    5    0.380721    0.671626    0.750000    10.50000    0.01997    0.02716 = 
         0.03655    0.00000    0.00000   -0.00636 
CL2   4    0.500000    0.726890    0.250000    10.25000    0.02408    0.03149 = 
         0.03328    0.00000    0.00000    0.00000 
C2    1    0.196723    0.610543    0.750000    10.50000    0.01720    0.04551 = 
         0.02623    0.00000    0.00000    0.00251 
AFIX  43 
H2    2    0.112779    0.614046    0.750000    10.50000   -1.20000 
AFIX   0 
C3    1    0.248194    0.541523    0.750000    10.50000    0.03124    0.03348 = 
         0.03343    0.00000    0.00000   -0.00393 
AFIX  43 
H3    2    0.200964    0.497424    0.750000    10.50000   -1.20000 
AFIX   0 
C5    1    0.437680    0.603866    0.750000    10.50000    0.02405    0.03444 = 
         0.02258    0.00000    0.00000    0.00354 
C4    1    0.375732    0.536447    0.750000    10.50000    0.02451    0.03009 = 
         0.02346    0.00000    0.00000   -0.00214 
C6    1    0.439782    0.467681    0.750000    10.50000    0.02744    0.02748 = 
         0.03066    0.00000    0.00000   -0.00704 
AFIX  43 
H6    2    0.398065    0.421404    0.750000    10.50000   -1.20000 
AFIX   0 
HKLF 4 
 
 
 
 
REM  m18128.res in Cmcm 
REM wR2 = 0.0899, GooF = S = 1.162, Restrained GooF = 1.162 for all data 
REM R1 = 0.0362 for 782 Fo > 4sig(Fo) and 0.0424 for all 857 data 
REM 57 parameters refined using 0 restraints 
 
END 
 
WGHT      0.0297     21.4314 
 
REM Instructions for potential hydrogen bonds 
EQIV $1 -x+1, y, -z+3/2 
HTAB C1 Cl1_$1 
EQIV $2 -x+1/2, -y+3/2, -z+1 
HTAB C1 Cl2_$2 
 
REM Highest difference peak  1.863,  deepest hole -1.278,  1-sigma level  0.226 
Q1    1   0.1339  0.6925  0.7500  10.50000  0.05    1.86 
Q2    1   0.4394  0.3851  0.7500  10.50000  0.05    1.53 
Q3    1   0.5866  0.8054  0.7500  10.50000  0.05    1.43 
Q4    1   0.4005  0.7209  0.7500  10.50000  0.05    1.41 
Q5    1   0.5000  0.7632  0.8880  10.50000  0.05    1.33 
;
_shelx_res_checksum              57655
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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
Au1 Au 0.500000 0.75866(3) 0.750000 0.0292(2) Uani 1 4 d S T P
C1 C 0.2628(9) 0.6754(5) 0.750000 0.029(2) Uani 1 2 d S T P
H1 H 0.224384 0.722821 0.750000 0.034 Uiso 1 2 calc R U P
Cl1 Cl 0.6420(3) 0.84803(13) 0.750000 0.0378(6) Uani 1 2 d S T P
N1 N 0.3807(7) 0.6716(4) 0.750000 0.0279(17) Uani 1 2 d S T P
Cl2 Cl 0.500000 0.72689(18) 0.250000 0.0296(7) Uani 1 4 d S T P
C2 C 0.1967(9) 0.6105(6) 0.750000 0.030(2) Uani 1 2 d S T P
H2 H 0.112779 0.614046 0.750000 0.036 Uiso 1 2 calc R U P
C3 C 0.2482(10) 0.5415(6) 0.750000 0.033(2) Uani 1 2 d S T P
H3 H 0.200964 0.497424 0.750000 0.039 Uiso 1 2 calc R U P
C5 C 0.4377(8) 0.6039(5) 0.750000 0.0270(19) Uani 1 2 d S T P
C4 C 0.3757(8) 0.5364(5) 0.750000 0.0260(19) Uani 1 2 d S T P
C6 C 0.4398(9) 0.4677(5) 0.750000 0.029(2) Uani 1 2 d S T P
H6 H 0.398065 0.421404 0.750000 0.034 Uiso 1 2 calc R U P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0306(3) 0.0286(3) 0.0283(3) 0.000 0.000 0.000
C1 0.022(5) 0.035(5) 0.028(5) 0.000 0.000 0.001(4)
Cl1 0.0443(16) 0.0328(12) 0.0363(13) 0.000 0.000 -0.0089(10)
N1 0.020(4) 0.027(4) 0.037(4) 0.000 0.000 -0.006(3)
Cl2 0.0241(16) 0.0315(15) 0.0333(17) 0.000 0.000 0.000
C2 0.017(5) 0.046(5) 0.026(5) 0.000 0.000 0.003(4)
C3 0.031(5) 0.033(5) 0.033(5) 0.000 0.000 -0.004(4)
C5 0.024(5) 0.034(5) 0.023(5) 0.000 0.000 0.004(4)
C4 0.025(5) 0.030(4) 0.023(4) 0.000 0.000 -0.002(4)
C6 0.027(5) 0.027(4) 0.031(5) 0.000 0.000 -0.007(4)
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
N1 Au1 N1 81.9(5) . 3_656
N1 Au1 Cl1 93.8(2) . 3_656
N1 Au1 Cl1 175.8(2) 3_656 3_656
N1 Au1 Cl1 175.8(2) . .
N1 Au1 Cl1 93.9(2) 3_656 .
Cl1 Au1 Cl1 90.38(15) 3_656 .
N1 C1 C2 119.9(9) . .
N1 C1 H1 120.0 . .
C2 C1 H1 120.0 . .
C1 N1 C5 120.9(8) . .
C1 N1 Au1 128.1(7) . .
C5 N1 Au1 111.0(6) . .
C3 C2 C1 121.9(10) . .
C3 C2 H2 119.1 . .
C1 C2 H2 119.1 . .
C2 C3 C4 118.9(9) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
N1 C5 C4 121.8(9) . .
N1 C5 C5 118.0(5) . 3_656
C4 C5 C5 120.2(6) . 3_656
C5 C4 C6 119.3(9) . .
C5 C4 C3 116.6(9) . .
C6 C4 C3 124.1(9) . .
C6 C6 C4 120.5(5) 3_656 .
C6 C6 H6 119.7 3_656 .
C4 C6 H6 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 N1 2.055(7) .
Au1 N1 2.055(7) 3_656
Au1 Cl1 2.260(3) 3_656
Au1 Cl1 2.260(3) .
C1 N1 1.334(12) .
C1 C2 1.376(14) .
C1 H1 0.9500 .
N1 C5 1.369(12) .
C2 C3 1.361(14) .
C2 H2 0.9500 .
C3 C4 1.443(14) .
C3 H3 0.9500 .
C5 C4 1.391(13) .
C5 C5 1.407(19) 3_656
C4 C6 1.423(13) .
C6 C6 1.36(2) 3_656
C6 H6 0.9500 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 N1 C5 0.0 . .
C2 C1 N1 Au1 180.0 . .
N1 C1 C2 C3 0.0 . .
C1 C2 C3 C4 0.0 . .
C1 N1 C5 C4 0.0 . .
Au1 N1 C5 C4 180.0 . .
C1 N1 C5 C5 180.0 . 3_656
Au1 N1 C5 C5 0.0 . 3_656
N1 C5 C4 C6 180.0 . .
C5 C5 C4 C6 0.0 3_656 .
N1 C5 C4 C3 0.0 . .
C5 C5 C4 C3 180.0 3_656 .
C2 C3 C4 C5 0.0 . .
C2 C3 C4 C6 180.0 . .
C5 C4 C6 C6 0.0 . 3_656
C3 C4 C6 C6 180.0 . 3_656
