# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c292
_database_code_depnum_ccdc_archive 'CCDC 2083080'
loop_
_audit_author_name
_audit_author_address
'M. Concepcion Gimeno'
;Instituto de Sintesis Quimica y Catalisis Homogenea
Spain
;
_audit_update_record             
;
2021-05-11 deposited with the CCDC.	2021-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17.60 H24 F9.60 N1.60 P1.60 S4.80 Tl1.60'
_chemical_formula_weight         970.81

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.9876(4)
_cell_length_b                   15.7182(4)
_cell_length_c                   16.7412(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3417.58(18)
_cell_formula_units_Z            5
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5304
_cell_measurement_theta_min      4.1724
_cell_measurement_theta_max      28.8174

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_F_000             2288
_exptl_transmission_factor_min   0.22949
_exptl_transmission_factor_max   1.00000
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    9.965
_shelx_estimated_absorpt_T_min   0.503
_shelx_estimated_absorpt_T_max   0.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w rotations'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            17326
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.181
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3172
_reflns_number_gt                2637
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+18.5164P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3172
_refine_ls_number_parameters     208
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.53174(2) 0.00870(2) 0.16444(2) 0.02507(13) Uani 1 1 d . . . . .
S1 S 0.57528(15) -0.02164(12) 0.35059(11) 0.0280(4) Uani 1 1 d . . . . .
S2 S 0.71659(15) 0.01089(12) 0.05668(11) 0.0276(4) Uani 1 1 d . . . . .
S3 S 0.68057(13) -0.13860(11) 0.20422(10) 0.0231(4) Uani 1 1 d . . . . .
N1 N 0.6968(4) 0.1003(3) 0.2257(3) 0.0213(12) Uani 1 1 d . . . . .
C1 C 0.6164(6) 0.0883(5) 0.3587(4) 0.0323(18) Uani 1 1 d . . . . .
H1A H 0.557283 0.125538 0.345770 0.039 Uiso 1 1 calc R U . . .
H1B H 0.636212 0.099606 0.414774 0.039 Uiso 1 1 calc R U . . .
C2 C 0.7063(6) 0.1123(4) 0.3048(4) 0.0233(15) Uani 1 1 d . . . . .
C3 C 0.7942(6) 0.1476(4) 0.3391(5) 0.0314(18) Uani 1 1 d . . . . .
H3 H 0.798680 0.154679 0.395369 0.038 Uiso 1 1 calc R U . . .
C4 C 0.8733(6) 0.1718(5) 0.2912(5) 0.0354(19) Uani 1 1 d . . . . .
H4 H 0.933822 0.195941 0.313590 0.042 Uiso 1 1 calc R U . . .
C5 C 0.8648(6) 0.1608(5) 0.2097(5) 0.0314(17) Uani 1 1 d . . . . .
H5 H 0.918974 0.177250 0.174833 0.038 Uiso 1 1 calc R U . . .
C6 C 0.7735(6) 0.1246(4) 0.1796(4) 0.0268(16) Uani 1 1 d . . . . .
C7 C 0.7645(6) 0.1137(5) 0.0904(4) 0.0363(19) Uani 1 1 d . . . . .
H7A H 0.833271 0.123076 0.066463 0.044 Uiso 1 1 calc R U . . .
H7B H 0.718190 0.158530 0.069616 0.044 Uiso 1 1 calc R U . . .
C8 C 0.8135(6) -0.0609(6) 0.0948(5) 0.040(2) Uani 1 1 d . . . . .
H8A H 0.862740 -0.073361 0.051184 0.048 Uiso 1 1 calc R U . . .
H8B H 0.852011 -0.031290 0.137539 0.048 Uiso 1 1 calc R U . . .
C9 C 0.7766(9) -0.1394(7) 0.1257(7) 0.067(3) Uani 1 1 d . U . . .
H9A H 0.836848 -0.171493 0.145882 0.080 Uiso 1 1 calc R U . . .
H9B H 0.747970 -0.172299 0.080445 0.080 Uiso 1 1 calc R U . . .
C10 C 0.7559(9) -0.0956(7) 0.2858(6) 0.070(3) Uani 1 1 d . U . . .
H10A H 0.813292 -0.135160 0.297630 0.084 Uiso 1 1 calc R U . . .
H10B H 0.786286 -0.040767 0.268822 0.084 Uiso 1 1 calc R U . . .
C11 C 0.6940(6) -0.0816(5) 0.3613(5) 0.0325(17) Uani 1 1 d . . . . .
H11A H 0.738355 -0.051649 0.400377 0.039 Uiso 1 1 calc R U . . .
H11B H 0.677015 -0.137890 0.384282 0.039 Uiso 1 1 calc R U . . .
P1 P 0.98319(15) 0.71677(12) 0.98769(11) 0.0271(4) Uani 1 1 d . . . . .
F1 F 0.9546(4) 0.7387(4) 1.0774(3) 0.0509(14) Uani 1 1 d . . . . .
F2 F 1.0028(4) 0.6201(3) 1.0113(3) 0.0531(14) Uani 1 1 d . . . . .
F3 F 1.0134(4) 0.6951(3) 0.8972(3) 0.0499(13) Uani 1 1 d . . . . .
F4 F 1.1010(3) 0.7372(3) 1.0072(3) 0.0446(12) Uani 1 1 d . . . . .
F5 F 0.8670(4) 0.6973(4) 0.9681(3) 0.0651(16) Uani 1 1 d . . . . .
F6 F 0.9690(4) 0.8141(3) 0.9635(3) 0.0491(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 N1 2.778(5) . ?
Tl1 S2 3.0032(19) . ?
Tl1 S3 3.0888(17) . ?
S1 C1 1.813(8) . ?
S1 C11 1.816(8) . ?
S2 C8 1.806(8) . ?
S2 C7 1.821(8) . ?
S3 C10 1.811(11) . ?
S3 C9 1.812(11) . ?
N1 C6 1.318(9) . ?
N1 C2 1.342(9) . ?
C1 C2 1.523(10) . ?
C2 C3 1.393(10) . ?
C3 C4 1.357(11) . ?
C4 C5 1.381(11) . ?
C5 C6 1.409(10) . ?
C6 C7 1.506(10) . ?
C8 C9 1.422(13) . ?
C10 C11 1.514(13) . ?
P1 F5 1.574(5) . ?
P1 F1 1.584(5) . ?
P1 F2 1.591(5) . ?
P1 F6 1.594(5) . ?
P1 F4 1.596(5) . ?
P1 F3 1.602(5) . ?

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
_geom_angle_publ_flag
N1 Tl1 S2 66.37(12) . . ?
N1 Tl1 S3 79.98(12) . . ?
S2 Tl1 S3 68.77(5) . . ?
C1 S1 C11 103.7(4) . . ?
C8 S2 C7 101.9(4) . . ?
C8 S2 Tl1 109.7(3) . . ?
C7 S2 Tl1 95.6(3) . . ?
C10 S3 C9 100.2(6) . . ?
C10 S3 Tl1 102.8(4) . . ?
C9 S3 Tl1 106.2(4) . . ?
C6 N1 C2 117.9(6) . . ?
C6 N1 Tl1 121.1(5) . . ?
C2 N1 Tl1 120.6(4) . . ?
C2 C1 S1 114.7(5) . . ?
N1 C2 C3 122.6(7) . . ?
N1 C2 C1 118.6(6) . . ?
C3 C2 C1 118.8(6) . . ?
C4 C3 C2 119.2(7) . . ?
C3 C4 C5 119.2(7) . . ?
C4 C5 C6 118.2(7) . . ?
N1 C6 C5 122.9(7) . . ?
N1 C6 C7 119.3(6) . . ?
C5 C6 C7 117.7(7) . . ?
C6 C7 S2 115.7(5) . . ?
C9 C8 S2 115.9(7) . . ?
C8 C9 S3 119.3(8) . . ?
C11 C10 S3 113.4(8) . . ?
C10 C11 S1 116.3(6) . . ?
F5 P1 F1 90.9(3) . . ?
F5 P1 F2 91.1(3) . . ?
F1 P1 F2 90.5(3) . . ?
F5 P1 F6 91.3(3) . . ?
F1 P1 F6 90.3(3) . . ?
F2 P1 F6 177.4(3) . . ?
F5 P1 F4 179.6(3) . . ?
F1 P1 F4 89.3(3) . . ?
F2 P1 F4 89.3(3) . . ?
F6 P1 F4 88.3(3) . . ?
F5 P1 F3 89.8(3) . . ?
F1 P1 F3 179.3(3) . . ?
F2 P1 F3 89.6(3) . . ?
F6 P1 F3 89.6(3) . . ?
F4 P1 F3 90.1(3) . . ?

_refine_diff_density_max         2.948
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.182



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c313
_database_code_depnum_ccdc_archive 'CCDC 2083082'
loop_
_audit_author_name
_audit_author_address
'M. Concepcion Gimeno'
;Instituto de Sintesis Quimica y Catalisis Homogenea
Spain
;
_audit_update_record             
;
2021-05-11 deposited with the CCDC.	2021-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H15 Au2 F20 N S3 Tl2'
_chemical_formula_weight         1728.33

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'
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'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.4455(2)
_cell_length_b                   12.42490(10)
_cell_length_c                   20.2617(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.5410(10)
_cell_angle_gamma                90
_cell_volume                     3876.19(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    24106
_cell_measurement_theta_min      4.1675
_cell_measurement_theta_max      28.8159

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.962
_exptl_crystal_F_000             3120
_exptl_transmission_factor_min   0.37236
_exptl_transmission_factor_max   1.00000
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    16.125
_shelx_estimated_absorpt_T_min   0.089
_shelx_estimated_absorpt_T_max   0.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w rotations'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            43489
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.215
_diffrn_reflns_theta_max         28.861
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9282
_reflns_number_gt                8510
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+3.7516P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9282
_refine_ls_number_parameters     568
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0524
_refine_ls_wR_factor_gt          0.0510
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.47317(2) 0.87270(2) 0.30845(2) 0.01586(4) Uani 1 1 d . . . . .
Au2 Au 0.23556(2) 0.56955(2) 0.23017(2) 0.01213(4) Uani 1 1 d . . . . .
Tl1 Tl 0.44842(2) 0.60733(2) 0.27934(2) 0.01346(4) Uani 1 1 d . . . . .
Tl2 Tl 0.28387(2) 0.82703(2) 0.26574(2) 0.01688(4) Uani 1 1 d . . . . .
C1 C 0.4232(3) 0.9177(3) 0.3948(2) 0.0165(8) Uani 1 1 d . . . . .
C2 C 0.4307(3) 1.0235(3) 0.4154(2) 0.0184(9) Uani 1 1 d . . . . .
C3 C 0.4021(3) 1.0611(3) 0.4749(2) 0.0193(9) Uani 1 1 d . . . . .
C4 C 0.3664(3) 0.9901(4) 0.5162(2) 0.0234(10) Uani 1 1 d . . . . .
C5 C 0.3576(3) 0.8824(4) 0.4982(2) 0.0236(10) Uani 1 1 d . . . . .
C6 C 0.3843(3) 0.8504(3) 0.4383(2) 0.0193(9) Uani 1 1 d . . . . .
C11 C 0.5332(3) 0.8390(3) 0.2241(2) 0.0165(9) Uani 1 1 d . . . . .
C12 C 0.6227(3) 0.8335(3) 0.2244(2) 0.0189(9) Uani 1 1 d . . . . .
C13 C 0.6666(3) 0.8178(3) 0.1685(2) 0.0215(10) Uani 1 1 d . . . . .
C14 C 0.6206(3) 0.8030(3) 0.1082(2) 0.0208(9) Uani 1 1 d . . . . .
C15 C 0.5312(3) 0.8057(3) 0.1047(2) 0.0184(9) Uani 1 1 d . . . . .
C16 C 0.4908(3) 0.8242(3) 0.1617(2) 0.0166(8) Uani 1 1 d . . . . .
F1 F 0.46705(18) 1.09727(19) 0.37758(13) 0.0260(6) Uani 1 1 d . . . . .
F2 F 0.41058(18) 1.1653(2) 0.49171(13) 0.0286(6) Uani 1 1 d . . . . .
F3 F 0.33860(17) 1.0244(2) 0.57430(13) 0.0324(7) Uani 1 1 d . . . . .
F4 F 0.32213(19) 0.8131(2) 0.53952(15) 0.0366(7) Uani 1 1 d . . . . .
F5 F 0.37172(18) 0.74436(19) 0.42239(14) 0.0315(6) Uani 1 1 d . . . . .
F6 F 0.67189(17) 0.8430(2) 0.28246(13) 0.0263(6) Uani 1 1 d . . . . .
F7 F 0.75408(16) 0.8138(2) 0.17177(15) 0.0327(7) Uani 1 1 d . . . . .
F8 F 0.66224(17) 0.7837(2) 0.05406(14) 0.0304(6) Uani 1 1 d . . . . .
F9 F 0.48547(16) 0.7906(2) 0.04625(12) 0.0259(6) Uani 1 1 d . . . . .
F10 F 0.40183(15) 0.82540(19) 0.15507(12) 0.0195(5) Uani 1 1 d . . . . .
S1 S 0.45743(7) 0.36787(8) 0.30639(5) 0.0144(2) Uani 1 1 d . . . . .
S2 S 0.52250(7) 0.48375(8) 0.16474(5) 0.0158(2) Uani 1 1 d . . . . .
S3 S 0.52846(7) 0.56809(8) 0.41690(5) 0.0145(2) Uani 1 1 d . . . . .
N1 N 0.6309(2) 0.5876(2) 0.28699(16) 0.0122(7) Uani 1 1 d . . . . .
C17 C 0.5517(3) 0.3262(3) 0.2647(2) 0.0159(8) Uani 1 1 d . . . . .
H17A H 0.603095 0.368079 0.282124 0.019 Uiso 1 1 calc R U . . .
H17B H 0.563636 0.249095 0.273717 0.019 Uiso 1 1 calc R U . . .
C18 C 0.5361(3) 0.3441(3) 0.1903(2) 0.0181(9) Uani 1 1 d . . . . .
H18A H 0.483519 0.303542 0.174064 0.022 Uiso 1 1 calc R U . . .
H18B H 0.585777 0.313392 0.168616 0.022 Uiso 1 1 calc R U . . .
C19 C 0.6324(3) 0.5327(3) 0.1695(2) 0.0191(9) Uani 1 1 d . . . . .
H19A H 0.668370 0.477079 0.149851 0.023 Uiso 1 1 calc R U . . .
H19B H 0.633382 0.597032 0.140767 0.023 Uiso 1 1 calc R U . . .
C20 C 0.6774(3) 0.5627(3) 0.2362(2) 0.0133(8) Uani 1 1 d . . . . .
C21 C 0.7675(3) 0.5671(3) 0.2406(2) 0.0163(8) Uani 1 1 d . . . . .
H21 H 0.798612 0.552583 0.202993 0.020 Uiso 1 1 calc R U . . .
C22 C 0.8107(3) 0.5928(3) 0.3002(2) 0.0177(9) Uani 1 1 d . . . . .
H22 H 0.872411 0.593773 0.304740 0.021 Uiso 1 1 calc R U . . .
C23 C 0.7641(3) 0.6172(3) 0.3535(2) 0.0155(8) Uani 1 1 d . . . . .
H23 H 0.793168 0.635479 0.395068 0.019 Uiso 1 1 calc R U . . .
C24 C 0.6736(3) 0.6145(3) 0.3455(2) 0.0135(8) Uani 1 1 d . . . . .
C25 C 0.6227(3) 0.6490(3) 0.4019(2) 0.0153(8) Uani 1 1 d . . . . .
H25A H 0.603157 0.724080 0.393677 0.018 Uiso 1 1 calc R U . . .
H25B H 0.662300 0.649289 0.442798 0.018 Uiso 1 1 calc R U . . .
C26 C 0.5696(3) 0.4318(3) 0.4168(2) 0.0158(8) Uani 1 1 d . . . . .
H26A H 0.618250 0.427630 0.387876 0.019 Uiso 1 1 calc R U . . .
H26B H 0.591993 0.411586 0.462189 0.019 Uiso 1 1 calc R U . . .
C27 C 0.4983(3) 0.3534(3) 0.3920(2) 0.0175(9) Uani 1 1 d . . . . .
H27A H 0.449038 0.361671 0.419979 0.021 Uiso 1 1 calc R U . . .
H27B H 0.520917 0.279301 0.398514 0.021 Uiso 1 1 calc R U . . .
C31 C 0.1903(3) 0.5615(3) 0.32228(19) 0.0127(8) Uani 1 1 d . . . . .
C32 C 0.1044(3) 0.5824(3) 0.3319(2) 0.0133(8) Uani 1 1 d . . . . .
C33 C 0.0693(3) 0.5742(3) 0.3928(2) 0.0145(8) Uani 1 1 d . . . . .
C34 C 0.1225(3) 0.5427(3) 0.4478(2) 0.0162(8) Uani 1 1 d . . . . .
C35 C 0.2088(3) 0.5248(3) 0.44092(19) 0.0145(8) Uani 1 1 d . . . . .
C36 C 0.2399(2) 0.5334(3) 0.37944(19) 0.0129(8) Uani 1 1 d . . . . .
C41 C 0.2770(2) 0.5808(3) 0.13691(19) 0.0126(8) Uani 1 1 d . . . . .
C42 C 0.3175(3) 0.5003(3) 0.1037(2) 0.0153(8) Uani 1 1 d . . . . .
C43 C 0.3495(3) 0.5115(3) 0.0423(2) 0.0172(9) Uani 1 1 d . . . . .
C44 C 0.3421(3) 0.6095(3) 0.0109(2) 0.0179(9) Uani 1 1 d . . . . .
C45 C 0.3010(3) 0.6925(3) 0.0408(2) 0.0161(8) Uani 1 1 d . . . . .
C46 C 0.2696(2) 0.6765(3) 0.10168(19) 0.0129(8) Uani 1 1 d . . . . .
F11 F 0.04804(16) 0.61104(19) 0.28016(12) 0.0196(5) Uani 1 1 d . . . . .
F12 F -0.01565(15) 0.5951(2) 0.39894(13) 0.0237(6) Uani 1 1 d . . . . .
F13 F 0.08986(15) 0.5296(2) 0.50647(11) 0.0210(5) Uani 1 1 d . . . . .
F14 F 0.26148(15) 0.4988(2) 0.49457(11) 0.0200(5) Uani 1 1 d . . . . .
F15 F 0.32571(14) 0.5103(2) 0.37644(12) 0.0198(5) Uani 1 1 d . . . . .
F16 F 0.32893(16) 0.40090(19) 0.13252(13) 0.0224(6) Uani 1 1 d . . . . .
F17 F 0.38852(18) 0.4288(2) 0.01327(13) 0.0270(6) Uani 1 1 d . . . . .
F18 F 0.37331(19) 0.6251(2) -0.04804(13) 0.0285(6) Uani 1 1 d . . . . .
F19 F 0.29345(17) 0.7885(2) 0.01035(12) 0.0233(6) Uani 1 1 d . . . . .
F20 F 0.22868(15) 0.76233(18) 0.12763(12) 0.0191(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 2.045(4) . ?
Au1 C11 2.051(4) . ?
Au1 Tl2 3.0363(2) . ?
Au1 Tl1 3.3660(2) . ?
Au2 C31 2.047(4) . ?
Au2 C41 2.047(4) . ?
Au2 Tl2 3.0299(2) 2_545 ?
Au2 Tl2 3.3505(2) . ?
Au2 Tl1 3.3917(2) . ?
Tl1 N1 2.821(3) . ?
Tl1 S3 2.9981(10) . ?
Tl1 S1 3.0266(10) . ?
Tl1 S2 3.0787(10) . ?
Tl1 Tl2 3.7251(2) . ?
C1 C2 1.382(6) . ?
C1 C6 1.386(6) . ?
C2 F1 1.345(5) . ?
C2 C3 1.397(6) . ?
C3 F2 1.342(5) . ?
C3 C4 1.362(6) . ?
C4 F3 1.354(5) . ?
C4 C5 1.390(7) . ?
C5 F4 1.347(5) . ?
C5 C6 1.372(6) . ?
C6 F5 1.367(5) . ?
C11 C12 1.383(6) . ?
C11 C16 1.390(6) . ?
C12 F6 1.355(5) . ?
C12 C13 1.379(6) . ?
C13 F7 1.349(5) . ?
C13 C14 1.376(6) . ?
C14 F8 1.336(5) . ?
C14 C15 1.378(6) . ?
C15 F9 1.342(5) . ?
C15 C16 1.376(6) . ?
C16 F10 1.370(4) . ?
S1 C27 1.807(4) . ?
S1 C17 1.815(4) . ?
S2 C19 1.799(4) . ?
S2 C18 1.819(4) . ?
S3 C26 1.808(4) . ?
S3 C25 1.815(4) . ?
N1 C20 1.336(5) . ?
N1 C24 1.352(5) . ?
C17 C18 1.524(6) . ?
C19 C20 1.516(5) . ?
C20 C21 1.389(6) . ?
C21 C22 1.370(6) . ?
C22 C23 1.379(6) . ?
C23 C24 1.395(6) . ?
C24 C25 1.499(6) . ?
C26 C27 1.525(6) . ?
C31 C32 1.381(6) . ?
C31 C36 1.382(5) . ?
C32 F11 1.355(4) . ?
C32 C33 1.391(6) . ?
C33 F12 1.353(5) . ?
C33 C34 1.386(6) . ?
C34 F13 1.338(5) . ?
C34 C35 1.371(6) . ?
C35 F14 1.344(4) . ?
C35 C36 1.374(5) . ?
C36 F15 1.362(4) . ?
C41 C42 1.381(6) . ?
C41 C46 1.386(5) . ?
C42 F16 1.372(5) . ?
C42 C43 1.383(6) . ?
C43 F17 1.350(5) . ?
C43 C44 1.374(6) . ?
C44 F18 1.337(5) . ?
C44 C45 1.376(6) . ?
C45 F19 1.344(5) . ?
C45 C46 1.375(5) . ?
C46 F20 1.367(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
_geom_angle_publ_flag
C1 Au1 C11 174.10(16) . . ?
C1 Au1 Tl2 82.79(11) . . ?
C11 Au1 Tl2 102.31(11) . . ?
C1 Au1 Tl1 111.87(12) . . ?
C11 Au1 Tl1 72.93(11) . . ?
Tl2 Au1 Tl1 70.947(5) . . ?
C31 Au2 C41 177.92(15) . . ?
C31 Au2 Tl2 83.40(10) . 2_545 ?
C41 Au2 Tl2 97.59(11) . 2_545 ?
C31 Au2 Tl2 86.37(10) . . ?
C41 Au2 Tl2 93.02(11) . . ?
Tl2 Au2 Tl2 164.700(5) 2_545 . ?
C31 Au2 Tl1 97.60(11) . . ?
C41 Au2 Tl1 83.97(11) . . ?
Tl2 Au2 Tl1 103.027(6) 2_545 . ?
Tl2 Au2 Tl1 67.076(5) . . ?
N1 Tl1 S3 66.31(7) . . ?
N1 Tl1 S1 82.73(7) . . ?
S3 Tl1 S1 70.25(3) . . ?
N1 Tl1 S2 64.46(7) . . ?
S3 Tl1 S2 118.00(3) . . ?
S1 Tl1 S2 68.39(3) . . ?
N1 Tl1 Au1 88.64(6) . . ?
S3 Tl1 Au1 87.915(19) . . ?
S1 Tl1 Au1 158.17(2) . . ?
S2 Tl1 Au1 125.23(2) . . ?
N1 Tl1 Au2 160.94(6) . . ?
S3 Tl1 Au2 124.70(2) . . ?
S1 Tl1 Au2 86.945(19) . . ?
S2 Tl1 Au2 96.832(19) . . ?
Au1 Tl1 Au2 106.323(5) . . ?
N1 Tl1 Tl2 137.77(6) . . ?
S3 Tl1 Tl2 114.62(2) . . ?
S1 Tl1 Tl2 139.03(2) . . ?
S2 Tl1 Tl2 127.001(19) . . ?
Au1 Tl1 Tl2 50.393(4) . . ?
Au2 Tl1 Tl2 55.935(4) . . ?
Au2 Tl2 Au1 84.351(6) 2 . ?
Au2 Tl2 Au2 159.167(6) 2 . ?
Au1 Tl2 Au2 115.643(6) . . ?
Au2 Tl2 Tl1 142.674(6) 2 . ?
Au1 Tl2 Tl1 58.660(5) . . ?
Au2 Tl2 Tl1 56.990(4) . . ?
C2 C1 C6 114.3(4) . . ?
C2 C1 Au1 119.4(3) . . ?
C6 C1 Au1 126.2(3) . . ?
F1 C2 C1 120.3(4) . . ?
F1 C2 C3 116.0(4) . . ?
C1 C2 C3 123.6(4) . . ?
F2 C3 C4 120.4(4) . . ?
F2 C3 C2 120.6(4) . . ?
C4 C3 C2 119.0(4) . . ?
F3 C4 C3 120.1(4) . . ?
F3 C4 C5 119.9(4) . . ?
C3 C4 C5 119.9(4) . . ?
F4 C5 C6 122.0(4) . . ?
F4 C5 C4 119.3(4) . . ?
C6 C5 C4 118.7(4) . . ?
F5 C6 C5 116.2(4) . . ?
F5 C6 C1 119.5(4) . . ?
C5 C6 C1 124.3(4) . . ?
C12 C11 C16 113.3(4) . . ?
C12 C11 Au1 121.7(3) . . ?
C16 C11 Au1 125.0(3) . . ?
F6 C12 C13 116.6(4) . . ?
F6 C12 C11 119.3(4) . . ?
C13 C12 C11 124.1(4) . . ?
F7 C13 C14 118.9(4) . . ?
F7 C13 C12 121.4(4) . . ?
C14 C13 C12 119.7(4) . . ?
F8 C14 C13 120.3(4) . . ?
F8 C14 C15 120.5(4) . . ?
C13 C14 C15 119.2(4) . . ?
F9 C15 C16 121.5(4) . . ?
F9 C15 C14 119.8(4) . . ?
C16 C15 C14 118.7(4) . . ?
F10 C16 C15 115.9(4) . . ?
F10 C16 C11 119.1(4) . . ?
C15 C16 C11 125.0(4) . . ?
C27 S1 C17 100.7(2) . . ?
C27 S1 Tl1 106.20(13) . . ?
C17 S1 Tl1 102.89(13) . . ?
C19 S2 C18 102.7(2) . . ?
C19 S2 Tl1 101.31(14) . . ?
C18 S2 Tl1 107.61(14) . . ?
C26 S3 C25 103.43(19) . . ?
C26 S3 Tl1 105.66(14) . . ?
C25 S3 Tl1 91.81(13) . . ?
C20 N1 C24 118.6(3) . . ?
C20 N1 Tl1 124.9(2) . . ?
C24 N1 Tl1 116.2(3) . . ?
C18 C17 S1 110.4(3) . . ?
C17 C18 S2 115.2(3) . . ?
C20 C19 S2 119.7(3) . . ?
N1 C20 C21 122.6(4) . . ?
N1 C20 C19 120.5(4) . . ?
C21 C20 C19 116.9(4) . . ?
C22 C21 C20 118.8(4) . . ?
C21 C22 C23 119.6(4) . . ?
C22 C23 C24 119.0(4) . . ?
N1 C24 C23 121.4(4) . . ?
N1 C24 C25 119.4(4) . . ?
C23 C24 C25 119.1(4) . . ?
C24 C25 S3 116.4(3) . . ?
C27 C26 S3 110.8(3) . . ?
C26 C27 S1 116.2(3) . . ?
C32 C31 C36 113.9(4) . . ?
C32 C31 Au2 121.4(3) . . ?
C36 C31 Au2 124.7(3) . . ?
F11 C32 C31 120.4(4) . . ?
F11 C32 C33 115.8(3) . . ?
C31 C32 C33 123.9(4) . . ?
F12 C33 C34 119.9(4) . . ?
F12 C33 C32 121.0(3) . . ?
C34 C33 C32 119.1(4) . . ?
F13 C34 C35 120.5(4) . . ?
F13 C34 C33 120.5(4) . . ?
C35 C34 C33 119.0(4) . . ?
F14 C35 C34 119.3(4) . . ?
F14 C35 C36 121.3(4) . . ?
C34 C35 C36 119.4(4) . . ?
F15 C36 C35 115.8(3) . . ?
F15 C36 C31 119.5(4) . . ?
C35 C36 C31 124.7(4) . . ?
C42 C41 C46 113.1(4) . . ?
C42 C41 Au2 125.9(3) . . ?
C46 C41 Au2 121.0(3) . . ?
F16 C42 C41 119.5(4) . . ?
F16 C42 C43 115.5(4) . . ?
C41 C42 C43 125.0(4) . . ?
F17 C43 C44 119.8(4) . . ?
F17 C43 C42 121.3(4) . . ?
C44 C43 C42 118.9(4) . . ?
F18 C44 C43 121.3(4) . . ?
F18 C44 C45 119.7(4) . . ?
C43 C44 C45 119.0(4) . . ?
F19 C45 C46 121.1(4) . . ?
F19 C45 C44 119.3(4) . . ?
C46 C45 C44 119.6(4) . . ?
F20 C46 C45 116.0(3) . . ?
F20 C46 C41 119.5(3) . . ?
C45 C46 C41 124.5(4) . . ?

_refine_diff_density_max         1.707
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.177



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c277
_database_code_depnum_ccdc_archive 'CCDC 2083081'
loop_
_audit_author_name
_audit_author_address
'M. Concepcion Gimeno'
;Instituto de Sintesis Quimica y Catalisis Homogenea
Spain
;
_audit_update_record             
;
2021-05-11 deposited with the CCDC.	2021-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H17 Au2 Cl2 F10 N S3'
_chemical_formula_weight         1070.40

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'
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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.4729(4)
_cell_length_b                   11.9047(3)
_cell_length_c                   21.1631(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.996(4)
_cell_angle_gamma                90
_cell_volume                     2792.05(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11102
_cell_measurement_theta_min      4.2462
_cell_measurement_theta_max      28.1029

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.546
_exptl_crystal_F_000             1992
_exptl_transmission_factor_min   0.35369
_exptl_transmission_factor_max   1.00000
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_exptl_absorpt_coefficient_mu    10.999
_shelx_estimated_absorpt_T_min   0.110
_shelx_estimated_absorpt_T_max   0.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w rotations'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            22231
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.255
_diffrn_reflns_theta_max         28.165
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6071
_reflns_number_gt                5415
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²+16.3482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6071
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.66407(2) 0.91517(2) 0.71451(2) 0.01454(7) Uani 1 1 d . . . . .
Au2 Au 0.30833(2) 0.77887(2) 0.32464(2) 0.01561(7) Uani 1 1 d . . . . .
C1 C 0.5644(5) 0.9274(5) 0.7805(3) 0.0144(11) Uani 1 1 d . . . . .
C2 C 0.6120(5) 0.9576(4) 0.8452(3) 0.0153(11) Uani 1 1 d . . . . .
C3 C 0.5481(6) 0.9532(5) 0.8923(3) 0.0229(13) Uani 1 1 d . . . . .
C4 C 0.4301(6) 0.9175(5) 0.8748(3) 0.0233(13) Uani 1 1 d . . . . .
C5 C 0.3782(5) 0.8867(5) 0.8109(3) 0.0210(12) Uani 1 1 d . . . . .
C6 C 0.4459(5) 0.8928(5) 0.7650(3) 0.0183(12) Uani 1 1 d . . . . .
F1 F 0.7282(3) 0.9919(3) 0.86563(16) 0.0209(7) Uani 1 1 d . . . . .
F2 F 0.5991(4) 0.9831(4) 0.95405(17) 0.0355(10) Uani 1 1 d . . . . .
F3 F 0.3648(4) 0.9123(4) 0.91869(19) 0.0377(10) Uani 1 1 d . . . . .
F4 F 0.2636(3) 0.8490(3) 0.79331(18) 0.0285(8) Uani 1 1 d . . . . .
F5 F 0.3906(3) 0.8573(3) 0.70399(16) 0.0246(8) Uani 1 1 d . . . . .
S1 S 0.77327(12) 0.88675(11) 0.63806(7) 0.0147(3) Uani 1 1 d . . . . .
C7 C 0.6959(5) 0.9611(5) 0.5637(3) 0.0138(11) Uani 1 1 d . . . . .
H7A H 0.611896 0.933528 0.548615 0.017 Uiso 1 1 calc R U . . .
H7B H 0.693158 1.042340 0.573184 0.017 Uiso 1 1 calc R U . . .
C8 C 0.7600(5) 0.9437(5) 0.5097(3) 0.0151(11) Uani 1 1 d . . . . .
H8A H 0.768236 0.862336 0.502257 0.018 Uiso 1 1 calc R U . . .
H8B H 0.841949 0.976681 0.523179 0.018 Uiso 1 1 calc R U . . .
S2 S 0.67537(13) 1.00948(12) 0.43466(7) 0.0178(3) Uani 1 1 d . . . . .
C9 C 0.5615(5) 0.9037(5) 0.4032(3) 0.0181(12) Uani 1 1 d . . . . .
H9A H 0.533115 0.872189 0.439880 0.022 Uiso 1 1 calc R U . . .
H9B H 0.491575 0.939525 0.372328 0.022 Uiso 1 1 calc R U . . .
C10 C 0.6085(5) 0.8085(5) 0.3682(3) 0.0190(12) Uani 1 1 d . . . . .
H10A H 0.678633 0.773267 0.399233 0.023 Uiso 1 1 calc R U . . .
H10B H 0.637147 0.840520 0.331766 0.023 Uiso 1 1 calc R U . . .
C11 C 0.1411(5) 0.8424(4) 0.3166(3) 0.0145(11) Uani 1 1 d . . . . .
C12 C 0.0702(5) 0.8872(5) 0.2595(3) 0.0165(11) Uani 1 1 d . . . . .
C13 C -0.0480(5) 0.9180(5) 0.2509(3) 0.0166(12) Uani 1 1 d . . . . .
C14 C -0.0992(5) 0.9098(5) 0.3030(3) 0.0201(12) Uani 1 1 d . . . . .
C15 C -0.0316(5) 0.8690(5) 0.3620(3) 0.0185(12) Uani 1 1 d . . . . .
C16 C 0.0857(5) 0.8367(5) 0.3672(3) 0.0169(11) Uani 1 1 d . . . . .
F6 F 0.1166(3) 0.9008(3) 0.20708(16) 0.0209(7) Uani 1 1 d . . . . .
F7 F -0.1163(3) 0.9550(3) 0.19274(16) 0.0247(8) Uani 1 1 d . . . . .
F8 F -0.2143(3) 0.9426(3) 0.29608(18) 0.0286(8) Uani 1 1 d . . . . .
F9 F -0.0811(3) 0.8596(3) 0.41255(17) 0.0297(9) Uani 1 1 d . . . . .
F10 F 0.1470(3) 0.7946(3) 0.42612(16) 0.0210(7) Uani 1 1 d . . . . .
S3 S 0.49687(13) 0.70003(12) 0.33574(7) 0.0176(3) Uani 1 1 d . . . . .
C17 C 0.5217(6) 0.5999(5) 0.4032(3) 0.0223(13) Uani 1 1 d . . . . .
H17A H 0.460733 0.539495 0.390862 0.027 Uiso 1 1 calc R U . . .
H17B H 0.601946 0.565120 0.408349 0.027 Uiso 1 1 calc R U . . .
C18 C 0.5160(5) 0.6461(4) 0.4683(3) 0.0163(11) Uani 1 1 d . . . . .
C19 C 0.4062(6) 0.6569(5) 0.4848(3) 0.0208(12) Uani 1 1 d . . . . .
H19 H 0.332699 0.634811 0.455021 0.025 Uiso 1 1 calc R U . . .
C20 C 0.4074(5) 0.7005(5) 0.5454(3) 0.0183(12) Uani 1 1 d . . . . .
H20 H 0.334140 0.710402 0.557799 0.022 Uiso 1 1 calc R U . . .
C21 C 0.5173(5) 0.7297(4) 0.5883(3) 0.0156(11) Uani 1 1 d . . . . .
H21 H 0.520304 0.758760 0.630469 0.019 Uiso 1 1 calc R U . . .
C22 C 0.6221(5) 0.7157(4) 0.5682(3) 0.0139(11) Uani 1 1 d . . . . .
C23 C 0.7460(5) 0.7399(5) 0.6122(3) 0.0146(11) Uani 1 1 d . . . . .
H23A H 0.807038 0.717473 0.589059 0.018 Uiso 1 1 calc R U . . .
H23B H 0.758172 0.692380 0.651760 0.018 Uiso 1 1 calc R U . . .
N1 N 0.6227(4) 0.6758(4) 0.5091(2) 0.0151(10) Uani 1 1 d . . . . .
Cl1 Cl 0.4272(3) 0.19497(19) 0.81453(11) 0.0700(8) Uani 1 1 d . . . . .
Cl2 Cl 0.4421(2) 0.2937(3) 0.94129(11) 0.0690(8) Uani 1 1 d . . . . .
C24 C 0.4018(8) 0.3139(7) 0.8569(4) 0.0445(19) Uani 1 1 d . . . . .
H24A H 0.448848 0.377468 0.846066 0.053 Uiso 1 1 calc R U . . .
H24B H 0.315265 0.334145 0.842544 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 2.027(5) . ?
Au1 S1 2.3131(13) . ?
Au2 C11 2.028(5) . ?
Au2 S3 2.3134(14) . ?
C1 C6 1.377(8) . ?
C1 C2 1.385(8) . ?
C2 F1 1.354(6) . ?
C2 C3 1.382(8) . ?
C3 F2 1.335(7) . ?
C3 C4 1.376(9) . ?
C4 F3 1.338(7) . ?
C4 C5 1.377(9) . ?
C5 F4 1.347(7) . ?
C5 C6 1.393(8) . ?
C6 F5 1.351(7) . ?
S1 C7 1.824(5) . ?
S1 C23 1.834(6) . ?
C7 C8 1.524(7) . ?
C8 S2 1.811(6) . ?
S2 C9 1.813(6) . ?
C9 C10 1.527(8) . ?
C10 S3 1.823(6) . ?
C11 C12 1.377(8) . ?
C11 C16 1.381(8) . ?
C12 F6 1.359(6) . ?
C12 C13 1.371(8) . ?
C13 F7 1.350(6) . ?
C13 C14 1.380(8) . ?
C14 F8 1.348(7) . ?
C14 C15 1.376(8) . ?
C15 F9 1.340(6) . ?
C15 C16 1.376(8) . ?
C16 F10 1.359(6) . ?
S3 C17 1.824(6) . ?
C17 C18 1.501(8) . ?
C18 N1 1.349(7) . ?
C18 C19 1.396(8) . ?
C19 C20 1.382(8) . ?
C20 C21 1.393(8) . ?
C21 C22 1.385(8) . ?
C22 N1 1.341(7) . ?
C22 C23 1.511(8) . ?
Cl1 C24 1.741(8) . ?
Cl2 C24 1.741(9) . ?

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
_geom_angle_publ_flag
C1 Au1 S1 175.56(16) . . ?
C11 Au2 S3 177.70(16) . . ?
C6 C1 C2 115.2(5) . . ?
C6 C1 Au1 120.9(4) . . ?
C2 C1 Au1 123.5(4) . . ?
F1 C2 C3 116.4(5) . . ?
F1 C2 C1 119.8(5) . . ?
C3 C2 C1 123.8(5) . . ?
F2 C3 C4 119.8(5) . . ?
F2 C3 C2 121.0(5) . . ?
C4 C3 C2 119.1(5) . . ?
F3 C4 C3 121.1(6) . . ?
F3 C4 C5 119.4(6) . . ?
C3 C4 C5 119.5(5) . . ?
F4 C5 C4 120.2(5) . . ?
F4 C5 C6 120.3(5) . . ?
C4 C5 C6 119.5(6) . . ?
F5 C6 C1 120.7(5) . . ?
F5 C6 C5 116.2(5) . . ?
C1 C6 C5 122.9(5) . . ?
C7 S1 C23 101.4(3) . . ?
C7 S1 Au1 107.60(18) . . ?
C23 S1 Au1 105.45(18) . . ?
C8 C7 S1 111.1(4) . . ?
C7 C8 S2 110.2(4) . . ?
C8 S2 C9 101.2(3) . . ?
C10 C9 S2 112.5(4) . . ?
C9 C10 S3 114.0(4) . . ?
C12 C11 C16 114.4(5) . . ?
C12 C11 Au2 123.3(4) . . ?
C16 C11 Au2 122.1(4) . . ?
F6 C12 C13 116.2(5) . . ?
F6 C12 C11 119.7(5) . . ?
C13 C12 C11 124.1(5) . . ?
F7 C13 C12 122.0(5) . . ?
F7 C13 C14 119.0(5) . . ?
C12 C13 C14 119.0(5) . . ?
F8 C14 C15 120.5(5) . . ?
F8 C14 C13 120.0(5) . . ?
C15 C14 C13 119.5(5) . . ?
F9 C15 C16 121.4(5) . . ?
F9 C15 C14 119.9(5) . . ?
C16 C15 C14 118.8(5) . . ?
F10 C16 C15 116.1(5) . . ?
F10 C16 C11 119.8(5) . . ?
C15 C16 C11 124.1(5) . . ?
C10 S3 C17 102.4(3) . . ?
C10 S3 Au2 107.36(19) . . ?
C17 S3 Au2 107.3(2) . . ?
C18 C17 S3 116.4(4) . . ?
N1 C18 C19 123.0(5) . . ?
N1 C18 C17 115.7(5) . . ?
C19 C18 C17 121.3(5) . . ?
C20 C19 C18 118.3(5) . . ?
C19 C20 C21 119.2(5) . . ?
C22 C21 C20 118.8(5) . . ?
N1 C22 C21 122.9(5) . . ?
N1 C22 C23 114.3(5) . . ?
C21 C22 C23 122.7(5) . . ?
C22 C23 S1 115.2(4) . . ?
C22 N1 C18 117.8(5) . . ?
Cl2 C24 Cl1 112.4(5) . . ?

_refine_diff_density_max         1.870
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.192



