#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:38:50 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232142 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/70/4347049.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_4347049
loop_
_publ_author_name
'Corbo, Robert'
'Ryan, Gemma F.'
'Haghighatbin, Mohammad A.'
'Hogan, Conor F.'
'Wilson, David J. D.'
'Hulett, Mark D.'
'Barnard, Peter J.'
'Dutton, Jason L.'
_publ_section_title
;
 Access to the Parent Tetrakis(pyridine)gold(III) Trication, Facile
 Formation of Rare Au(III) Terminal Hydroxides, and Preliminary Studies of
 Biological Properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2830
_journal_page_last               2839
_journal_paper_doi               10.1021/acs.inorgchem.5b02667
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C26 H28 Au F6 N6 O6 S2'
_chemical_formula_weight         895.63
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.340(3)
_cell_length_b                   12.963(3)
_cell_length_c                   19.695(4)
_cell_measurement_reflns_used    10920
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0940
_cell_measurement_theta_min      3.7630
_cell_volume                     3661.1(14)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    SHELXP
_computing_publication_material  SHELXP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27459
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  0.5525
_exptl_absorpt_correction_T_min  0.3651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²+5.8962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                3102
_reflns_number_total             3504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02667_si_002.cif
_cod_data_source_block           8bipy
_cod_original_cell_volume        3661.0(13)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4347049
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au1 Au 0.969057(16) 0.2500 0.619240(11) 0.03333(11) Uani 1 2 d S
S2 S 0.48308(13) -0.2500 0.29907(9) 0.0509(5) Uani 1 2 d S
S1 S 0.33272(11) -0.2500 0.60027(9) 0.0386(4) Uani 1 2 d S
N1 N 1.0758(3) 0.1485(3) 0.62331(17) 0.0342(8) Uani 1 1 d .
N2 N 0.8682(3) 0.1441(3) 0.61591(17) 0.0354(8) Uani 1 1 d .
O22 O 0.5800(4) -0.2500 0.2923(3) 0.0725(18) Uani 1 2 d S
O32 O 0.3804(2) -0.1561(3) 0.58437(18) 0.0531(9) Uani 1 1 d .
O31 O 0.2343(3) -0.2500 0.5836(3) 0.0482(12) Uani 1 2 d S
F31 F 0.2889(3) -0.1682(3) 0.71745(16) 0.0723(10) Uani 1 1 d .
C41 C 0.3318(5) -0.2500 0.6920(4) 0.0446(16) Uani 1 2 d S
C24 C 0.7560(3) 0.0419(4) 0.6731(2) 0.0433(11) Uani 1 1 d .
H24A H 0.7318 0.0162 0.7147 0.052 Uiso 1 1 calc R
C12 C 1.0682(4) 0.0461(4) 0.6198(2) 0.0426(11) Uani 1 1 d .
H12A H 1.0083 0.0158 0.6145 0.051 Uiso 1 1 calc R
C13 C 1.1449(4) -0.0162(4) 0.6236(2) 0.0515(13) Uani 1 1 d .
H13A H 1.1384 -0.0890 0.6212 0.062 Uiso 1 1 calc R
C23 C 0.7144(3) 0.0124(4) 0.6110(2) 0.0420(11) Uani 1 1 d .
F21 F 0.3714(5) -0.2500 0.4019(4) 0.117(3) Uani 1 2 d S
C15 C 1.2395(4) 0.1333(4) 0.6350(2) 0.0456(12) Uani 1 1 d .
H15A H 1.2989 0.1645 0.6408 0.055 Uiso 1 1 calc R
C25 C 0.8294(3) 0.1062(4) 0.6738(2) 0.0417(11) Uani 1 1 d .
H25A H 0.8552 0.1258 0.7163 0.050 Uiso 1 1 calc R
C14 C 1.2318(4) 0.0276(4) 0.6309(2) 0.0489(13) Uani 1 1 d .
H14A H 1.2858 -0.0147 0.6331 0.059 Uiso 1 1 calc R
C31 C 0.4601(7) -0.2500 0.3879(4) 0.068(3) Uani 1 2 d S
O21 O 0.4403(5) -0.1577(5) 0.2748(3) 0.123(2) Uani 1 1 d .
C21 C 0.8290(3) 0.1183(5) 0.5559(2) 0.0514(13) Uani 1 1 d .
H21A H 0.8546 0.1458 0.5152 0.062 Uiso 1 1 calc R
C22 C 0.7551(4) 0.0549(5) 0.5518(2) 0.0549(14) Uani 1 1 d .
H22A H 0.7297 0.0385 0.5085 0.066 Uiso 1 1 calc R
F32 F 0.4180(3) -0.2500 0.7168(2) 0.0710(13) Uani 1 2 d S
N22 N 0.6406(3) -0.0508(4) 0.6081(2) 0.0522(11) Uani 1 1 d .
C16 C 1.1603(3) 0.1938(3) 0.6306(2) 0.0336(10) Uani 1 1 d .
C27 C 0.5972(4) -0.0909(5) 0.6700(3) 0.0647(16) Uani 1 1 d .
H27A H 0.6292 -0.0624 0.7097 0.097 Uiso 1 1 calc R
H27B H 0.6021 -0.1663 0.6705 0.097 Uiso 1 1 calc R
H27C H 0.5314 -0.0709 0.6710 0.097 Uiso 1 1 calc R
F22 F 0.4945(4) -0.1656(5) 0.4150(3) 0.144(2) Uani 1 1 d .
C26 C 0.6017(5) -0.0829(6) 0.5421(3) 0.080(2) Uani 1 1 d .
H26A H 0.6373 -0.0505 0.5053 0.120 Uiso 1 1 calc R
H26B H 0.5363 -0.0615 0.5392 0.120 Uiso 1 1 calc R
H26C H 0.6058 -0.1581 0.5378 0.120 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Au1 N2 87.0(2) . 7_565
N2 Au1 N1 95.88(18) . .
N2 Au1 N1 177.15(15) 7_565 .
N2 Au1 N1 177.15(15) . 7_565
N2 Au1 N1 95.88(18) 7_565 7_565
N1 Au1 N1 81.3(2) . 7_565
O22 S2 O21 113.3(3) . 7
O22 S2 O21 113.3(3) . .
O21 S2 O21 113.9(7) 7 .
O22 S2 C31 106.1(4) . .
O21 S2 C31 104.5(3) 7 .
O21 S2 C31 104.5(3) . .
O32 S1 O32 116.6(3) . 7
O32 S1 O31 114.55(18) . .
O32 S1 O31 114.55(18) 7 .
O32 S1 C41 102.9(2) . .
O32 S1 C41 102.9(2) 7 .
O31 S1 C41 102.7(3) . .
C12 N1 C16 120.6(4) . .
C12 N1 Au1 125.8(4) . .
C16 N1 Au1 113.6(3) . .
C21 N2 C25 118.2(4) . .
C21 N2 Au1 120.1(3) . .
C25 N2 Au1 121.2(3) . .
F31 C41 F31 106.4(6) . 7
F31 C41 F32 107.1(4) . .
F31 C41 F32 107.1(4) 7 .
F31 C41 S1 112.4(4) . .
F31 C41 S1 112.4(4) 7 .
F32 C41 S1 111.1(5) . .
C25 C24 C23 120.6(4) . .
N1 C12 C13 121.3(5) . .
C12 C13 C14 119.4(5) . .
N22 C23 C24 122.5(4) . .
N22 C23 C22 121.8(4) . .
C24 C23 C22 115.7(5) . .
C14 C15 C16 119.6(5) . .
C24 C25 N2 122.4(4) . .
C13 C14 C15 119.3(5) . .
F21 C31 F22 106.2(6) . .
F21 C31 F22 106.2(6) . 7
F22 C31 F22 112.8(9) . 7
F21 C31 S2 112.9(7) . .
F22 C31 S2 109.3(5) . .
F22 C31 S2 109.3(5) 7 .
C22 C21 N2 122.2(5) . .
C21 C22 C23 120.9(5) . .
C23 N22 C27 121.1(4) . .
C23 N22 C26 120.7(4) . .
C27 N22 C26 118.3(5) . .
N1 C16 C15 119.7(4) . .
N1 C16 C16 115.7(3) . 7_565
C15 C16 C16 124.6(3) . 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 N2 1.994(4) .
Au1 N2 1.994(4) 7_565
Au1 N1 2.019(4) .
Au1 N1 2.019(4) 7_565
S2 O22 1.396(6) .
S2 O21 1.427(5) 7
S2 O21 1.427(5) .
S2 C31 1.779(9) .
S1 O32 1.430(4) .
S1 O32 1.430(4) 7
S1 O31 1.449(5) .
S1 C41 1.808(7) .
N1 C12 1.334(6) .
N1 C16 1.355(6) .
N2 C21 1.351(6) .
N2 C25 1.361(6) .
F31 C41 1.324(5) .
C41 F31 1.324(5) 7
C41 F32 1.329(8) .
C24 C25 1.343(7) .
C24 C23 1.413(7) .
C12 C13 1.367(8) .
C13 C14 1.376(8) .
C23 N22 1.340(7) .
C23 C22 1.417(7) .
F21 C31 1.302(11) .
C15 C14 1.377(8) .
C15 C16 1.383(7) .
C31 F22 1.314(7) .
C31 F22 1.314(7) 7
C21 C22 1.343(7) .
N22 C27 1.464(7) .
N22 C26 1.474(7) .
C16 C16 1.457(9) 7_565
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
N2 Au1 N1 C12 3.7(4) . .
N2 Au1 N1 C12 177(100) 7_565 .
N1 Au1 N1 C12 -176.6(3) 7_565 .
N2 Au1 N1 C16 -176.0(3) . .
N2 Au1 N1 C16 -2(3) 7_565 .
N1 Au1 N1 C16 3.7(3) 7_565 .
N2 Au1 N2 C21 81.1(4) 7_565 .
N1 Au1 N2 C21 -99.2(4) . .
N1 Au1 N2 C21 -105(3) 7_565 .
N2 Au1 N2 C25 -90.5(4) 7_565 .
N1 Au1 N2 C25 89.2(4) . .
N1 Au1 N2 C25 83(3) 7_565 .
O32 S1 C41 F31 59.2(5) . .
O32 S1 C41 F31 -179.3(4) 7 .
O31 S1 C41 F31 -60.0(4) . .
O32 S1 C41 F31 179.3(4) . 7
O32 S1 C41 F31 -59.2(5) 7 7
O31 S1 C41 F31 60.0(4) . 7
O32 S1 C41 F32 -60.77(17) . .
O32 S1 C41 F32 60.77(17) 7 .
O31 S1 C41 F32 180.0 . .
C16 N1 C12 C13 0.2(7) . .
Au1 N1 C12 C13 -179.5(3) . .
N1 C12 C13 C14 -0.3(7) . .
C25 C24 C23 N22 -179.4(5) . .
C25 C24 C23 C22 -0.2(8) . .
C23 C24 C25 N2 -1.2(8) . .
C21 N2 C25 C24 2.1(8) . .
Au1 N2 C25 C24 173.9(4) . .
C12 C13 C14 C15 0.7(7) . .
C16 C15 C14 C13 -1.1(8) . .
O22 S2 C31 F21 180.0 . .
O21 S2 C31 F21 -60.0(4) 7 .
O21 S2 C31 F21 60.0(4) . .
O22 S2 C31 F22 62.0(6) . .
O21 S2 C31 F22 -178.0(6) 7 .
O21 S2 C31 F22 -58.1(7) . .
O22 S2 C31 F22 -62.0(6) . 7
O21 S2 C31 F22 58.1(7) 7 7
O21 S2 C31 F22 178.0(6) . 7
C25 N2 C21 C22 -1.6(8) . .
Au1 N2 C21 C22 -173.5(5) . .
N2 C21 C22 C23 0.2(9) . .
N22 C23 C22 C21 179.9(6) . .
C24 C23 C22 C21 0.7(9) . .
C24 C23 N22 C27 1.6(8) . .
C22 C23 N22 C27 -177.6(6) . .
C24 C23 N22 C26 -177.6(6) . .
C22 C23 N22 C26 3.3(9) . .
C12 N1 C16 C15 -0.5(6) . .
Au1 N1 C16 C15 179.2(3) . .
C12 N1 C16 C16 177.2(3) . 7_565
Au1 N1 C16 C16 -3.1(3) . 7_565
C14 C15 C16 N1 1.0(7) . .
C14 C15 C16 C16 -176.5(3) . 7_565
