# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_HK121F1
_database_code_depnum_ccdc_archive 'CCDC 2422633'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2025-02-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 14 novembre 2022                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
"[1,3]dithiolo[4',5':5,6][1,4]dithiino[2,3-b]pyrazine-2-thione"
_chemical_formula_moiety         'C7 H2 N2 S5'
_chemical_formula_sum            'C7 H2 N2 S5'
_chemical_formula_weight         274.41
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, y, -z-1/2'

_cell_length_a                   23.107(3)
_cell_length_b                   10.6201(13)
_cell_length_c                   3.9168(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     961.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5765
_cell_measurement_theta_min      2.6050
_cell_measurement_theta_max      27.6542
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.1553707
_diffrn_orient_matrix_UB_21      -0.1928973
_diffrn_orient_matrix_UB_31      0.0619144
_diffrn_orient_matrix_UB_12      -0.0154549
_diffrn_orient_matrix_UB_22      0.0394403
_diffrn_orient_matrix_UB_32      0.0840948
_diffrn_orient_matrix_UB_13      -0.0335976
_diffrn_orient_matrix_UB_23      0.0217982
_diffrn_orient_matrix_UB_33      -0.0163979


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       stick
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             552
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_T_max  0.977

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.1-1        #
# Number of scans            :        5                                        #
# Total number of frames [*] :      291                                        #
# Total length of scans  [*] :   291.00 (deg.)                                 #
# Rotation speed         [*] :    50.00 sec./deg.                              #
# Total exposition time  [*] :      4 h     2 min.                             #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     5.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    5.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   50.0  1.00    34.0    97   97.0    0.1    2.7  144.0  -44.5 150.0 #
#  4 Omega   50.0  1.00    34.0    97   97.0    0.1   99.7   72.0  -44.5 150.0 #
#  5 Omega   50.0  1.00    34.0    97   97.0    0.1    2.7  288.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0455
_diffrn_reflns_av_r_equivalents  0.0638
_diffrn_reflns_number            9822
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         2.605
_diffrn_reflns_theta_max         27.655
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             1175
_reflns_number_gt                1082
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.

;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+0.9502P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         1175
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.255

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.25407(11) 0.250000 0.5528(8) 0.0188(6) Uani 1 2 d S T P . .
C2 C 0.35167(7) 0.31325(19) 0.8359(5) 0.0146(4) Uani 1 1 d . . . . .
C3 C 0.46719(7) 0.31619(17) 0.8392(5) 0.0133(4) Uani 1 1 d . . . . .
N4 N 0.51286(7) 0.38174(16) 0.7345(5) 0.0165(3) Uani 1 1 d . . . . .
C5 C 0.55835(8) 0.31489(19) 0.6268(5) 0.0183(4) Uani 1 1 d . . . . .
H5 H 0.591730 0.358205 0.547724 0.022 Uiso 1 1 calc R U . . .
S1 S 0.18922(3) 0.250000 0.3801(2) 0.0279(2) Uani 1 2 d S T P . .
S2 S 0.29190(2) 0.38657(5) 0.65192(13) 0.01785(16) Uani 1 1 d . . . . .
S3 S 0.40819(2) 0.40687(5) 0.99377(13) 0.01620(16) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 S1 1.644(3) . ?
C1 S2 1.7373(15) . ?
C1 S2 1.7373(15) 7_565 ?
C2 C2 1.343(4) 7_565 ?
C2 S2 1.7417(18) . ?
C2 S3 1.7541(19) . ?
C3 N4 1.329(2) . ?
C3 C3 1.406(4) 7_565 ?
C3 S3 1.7755(18) . ?
N4 C5 1.337(2) . ?
C5 C5 1.378(4) 7_565 ?
C5 H5 0.9500 . ?

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
S1 C1 S2 123.40(7) . . ?
S1 C1 S2 123.40(7) . 7_565 ?
S2 C1 S2 113.20(15) . 7_565 ?
C2 C2 S2 116.55(7) 7_565 . ?
C2 C2 S3 124.53(6) 7_565 . ?
S2 C2 S3 118.88(12) . . ?
N4 C3 C3 121.59(11) . 7_565 ?
N4 C3 S3 115.52(14) . . ?
C3 C3 S3 122.85(6) 7_565 . ?
C3 N4 C5 116.33(17) . . ?
N4 C5 C5 122.08(11) . 7_565 ?
N4 C5 H5 119.0 . . ?
C5 C5 H5 119.0 7_565 . ?
C1 S2 C2 96.78(10) . . ?
C2 S3 C3 98.29(9) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C3 N4 C5 0.6(2) 7_565 . . . ?
S3 C3 N4 C5 178.08(14) . . . . ?
C3 N4 C5 C5 -0.6(2) . . . 7_565 ?
S1 C1 S2 C2 177.16(19) . . . . ?
S2 C1 S2 C2 -3.26(18) 7_565 . . . ?
C2 C2 S2 C1 2.00(11) 7_565 . . . ?
S3 C2 S2 C1 179.90(13) . . . . ?
C2 C2 S3 C3 40.05(8) 7_565 . . . ?
S2 C2 S3 C3 -137.67(12) . . . . ?
N4 C3 S3 C2 143.46(15) . . . . ?
C3 C3 S3 C2 -39.12(8) 7_565 . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR HK121F1                                                #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_chemical_melting_point          463
####################################################################### 
# 
# 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_HK317_2
_database_code_depnum_ccdc_archive 'CCDC 2422635'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2025-02-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 23 fevrier 2024                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
(tetraethylammonium)[bis([1,4]dithiino[2,3-b]pyrazine-2,3-bis(thiolate))nickelate]
_chemical_formula_moiety         'C12 H4 N4 Ni S8, C8 H20 N'
_chemical_formula_sum            'C20 H24 N5 Ni S8'
_chemical_formula_weight         649.63
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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'

_cell_length_a                   21.976(2)
_cell_length_b                   8.3085(8)
_cell_length_c                   16.7017(17)
_cell_angle_alpha                90
_cell_angle_beta                 119.994(3)
_cell_angle_gamma                90
_cell_volume                     2641.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.5466
_cell_measurement_theta_max      27.5162
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0149202
_diffrn_orient_matrix_UB_21      0.0013934
_diffrn_orient_matrix_UB_31      -0.0503581
_diffrn_orient_matrix_UB_12      -0.0371525
_diffrn_orient_matrix_UB_22      -0.1136028
_diffrn_orient_matrix_UB_32      -0.0141511
_diffrn_orient_matrix_UB_13      -0.0445388
_diffrn_orient_matrix_UB_23      0.0206301
_diffrn_orient_matrix_UB_33      -0.0486826


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1340
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_T_max  0.870

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.10-0       #
# Total number of scans:        5                                              #
#                                                                              #
# ....[fast scans included]:                                                   #
#    . Total number of frames :      942                                       #
#    . Total length of scans  :   651.00 (deg.)                                #
#    . Mean rotation speed    :    10.65 sec./deg.                             #
#    . Total exposition time  :      1 h 29 min. [89 min.]                     #
#                                                                              #
#                                                                              #
# ....[fast scans excluded]:                                                   #
#    . Total number of frames :      582                                       #
#    . Total length of scans  :   291.00 (deg.)                                #
#    . Mean rotation speed    :    16.00 sec./deg.                             #
#    . Total exposition time  :      1 h 17 min. [77 min.]                     #
#                                                                              #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     2.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    2.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega    8.0  0.50    34.0   194   97.0    0.1    2.7    0.0  -44.5 150.0 #
#  4 Omega    8.0  0.50    34.0   194   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  5 Omega    8.0  0.50    34.0   194   97.0    0.1    2.7  216.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0191
_diffrn_reflns_av_r_equivalents  0.0262
_diffrn_reflns_number            15252
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.675
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             3026
_reflns_number_gt                2822
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0373P)²+1.9565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         3026
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.054

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Ni Ni 0.3393 1.1124 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ni1 Ni 0.500000 0.000000 0.500000 0.02684(9) Uani 1 2 d S . P . .
S1 S 0.61039(2) -0.03193(5) 0.59756(3) 0.03304(10) Uani 1 1 d . . . . .
S2 S 0.51464(2) 0.25035(5) 0.48173(3) 0.02978(10) Uani 1 1 d . . . . .
S3 S 0.73554(2) 0.18337(5) 0.68642(3) 0.03614(11) Uani 1 1 d . . . . .
S4 S 0.63234(2) 0.48424(4) 0.57034(3) 0.03238(10) Uani 1 1 d . . . . .
C1 C 0.64439(7) 0.16013(19) 0.60995(10) 0.0293(3) Uani 1 1 d . . . . .
C2 C 0.60214(8) 0.28407(18) 0.56050(10) 0.0281(3) Uani 1 1 d . . . . .
C3 C 0.75628(8) 0.31836(18) 0.62149(11) 0.0300(3) Uani 1 1 d . . . . .
C4 C 0.71262(8) 0.44913(18) 0.57373(10) 0.0293(3) Uani 1 1 d . . . . .
N5 N 0.73011(7) 0.55607(16) 0.52946(10) 0.0348(3) Uani 1 1 d . . . . .
C6 C 0.79094(9) 0.5310(2) 0.53174(13) 0.0385(4) Uani 1 1 d . . . . .
H6 H 0.805662 0.604816 0.501375 0.046 Uiso 1 1 calc R U . . .
C7 C 0.83293(9) 0.4006(2) 0.57705(12) 0.0370(4) Uani 1 1 d . . . . .
H7 H 0.875430 0.386701 0.575974 0.044 Uiso 1 1 calc R U . . .
N8 N 0.81628(7) 0.29295(16) 0.62241(10) 0.0343(3) Uani 1 1 d . . . . .
N21 N 0.500000 0.3653(2) 0.750000 0.0311(4) Uani 1 2 d S T P . .
C23 C 0.500000 0.6718(3) 0.750000 0.0622(9) Uani 1 2 d S T P . .
H23A H 0.504537 0.768669 0.786046 0.075 Uiso 0.5 1 calc R U P A .
H23B H 0.536943 0.671194 0.733429 0.075 Uiso 0.5 1 calc R U P . .
H23C H 0.453871 0.671193 0.693591 0.075 Uiso 0.5 1 calc R U P . .
C22 C 0.5077(2) 0.5142(3) 0.8108(2) 0.0350(7) Uani 0.5 1 d . . P A -1
H22A H 0.554071 0.513246 0.868087 0.042 Uiso 0.5 1 calc R U P A -1
H22B H 0.470619 0.513245 0.828066 0.042 Uiso 0.5 1 calc R U P A -1
C24 C 0.51387(18) 0.2241(4) 0.8180(2) 0.0328(6) Uani 0.5 1 d . . P A -1
H24A H 0.562369 0.233104 0.870823 0.039 Uiso 0.5 1 calc R U P A -1
H24B H 0.481250 0.233418 0.842468 0.039 Uiso 0.5 1 calc R U P A -1
C25 C 0.5048(3) 0.0616(4) 0.7741(2) 0.0405(9) Uani 0.5 1 d . . P A -1
H25A H 0.514134 -0.022419 0.820053 0.049 Uiso 0.5 1 calc R U P A -1
H25B H 0.456501 0.050656 0.722593 0.049 Uiso 0.5 1 calc R U P A -1
H25C H 0.537667 0.050341 0.750964 0.049 Uiso 0.5 1 calc R U P A -1
C26 C 0.42386(18) 0.3561(4) 0.6719(2) 0.0360(7) Uani 0.5 1 d . . P A -1
H26A H 0.413829 0.454404 0.633884 0.043 Uiso 0.5 1 calc R U P A -1
H26B H 0.419843 0.263546 0.632217 0.043 Uiso 0.5 1 calc R U P A -1
C27 C 0.3675(6) 0.3394(12) 0.6966(7) 0.049(2) Uani 0.5 1 d . . P A -1
H27A H 0.321559 0.334935 0.639958 0.059 Uiso 0.5 1 calc R U P A -1
H27B H 0.375002 0.240256 0.732153 0.059 Uiso 0.5 1 calc R U P A -1
H27C H 0.368958 0.432035 0.733828 0.059 Uiso 0.5 1 calc R U P A -1
C28 C 0.54772(18) 0.3670(4) 0.7147(2) 0.0352(7) Uani 0.5 1 d . . P A -1
H28A H 0.535387 0.459225 0.671724 0.042 Uiso 0.5 1 calc R U P A -1
H28B H 0.540233 0.267621 0.678192 0.042 Uiso 0.5 1 calc R U P A -1
C29 C 0.6250(6) 0.3787(12) 0.7859(7) 0.0444(18) Uani 0.5 1 d . . P A -1
H29A H 0.652664 0.378951 0.754641 0.053 Uiso 0.5 1 calc R U P A -1
H29B H 0.633699 0.478435 0.821317 0.053 Uiso 0.5 1 calc R U P A -1
H29C H 0.638559 0.286257 0.827804 0.053 Uiso 0.5 1 calc R U P A -1



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
Ni1 S2 2.1497(4) 5_656 ?
Ni1 S2 2.1497(4) . ?
Ni1 S1 2.1583(4) . ?
Ni1 S1 2.1584(4) 5_656 ?
S1 C1 1.7300(16) . ?
S2 C2 1.7256(15) . ?
S3 C1 1.7673(15) . ?
S3 C3 1.7707(16) . ?
S4 C4 1.7611(15) . ?
S4 C2 1.7675(16) . ?
C1 C2 1.356(2) . ?
C3 N8 1.328(2) . ?
C3 C4 1.404(2) . ?
C4 N5 1.330(2) . ?
N5 C6 1.335(2) . ?
C6 C7 1.378(3) . ?
C6 H6 0.9500 . ?
C7 N8 1.336(2) . ?
C7 H7 0.9500 . ?
N21 C28 1.438(3) . ?
N21 C26 1.525(3) . ?
N21 C24 1.553(3) . ?
N21 C22 1.555(3) . ?
C23 C22 1.613(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23A 0.9800 2_656 ?
C23 H23B 0.9800 2_656 ?
C23 H23C 0.9800 2_656 ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 C25 1.501(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.494(13) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.512(12) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

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
S2 Ni1 S2 180.0 5_656 . ?
S2 Ni1 S1 88.019(14) 5_656 . ?
S2 Ni1 S1 91.982(14) . . ?
S2 Ni1 S1 91.981(14) 5_656 5_656 ?
S2 Ni1 S1 88.019(14) . 5_656 ?
S1 Ni1 S1 180.00(2) . 5_656 ?
C1 S1 Ni1 103.42(5) . . ?
C2 S2 Ni1 103.75(5) . . ?
C1 S3 C3 99.93(7) . . ?
C4 S4 C2 99.82(7) . . ?
C2 C1 S1 120.30(12) . . ?
C2 C1 S3 122.74(12) . . ?
S1 C1 S3 116.93(9) . . ?
C1 C2 S2 120.26(12) . . ?
C1 C2 S4 123.17(12) . . ?
S2 C2 S4 116.56(8) . . ?
N8 C3 C4 121.47(14) . . ?
N8 C3 S3 116.76(12) . . ?
C4 C3 S3 121.74(12) . . ?
N5 C4 C3 121.85(14) . . ?
N5 C4 S4 115.77(12) . . ?
C3 C4 S4 122.37(12) . . ?
C4 N5 C6 116.32(14) . . ?
N5 C6 C7 121.65(16) . . ?
N5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
N8 C7 C6 122.64(15) . . ?
N8 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C3 N8 C7 116.03(14) . . ?
C28 N21 C26 111.31(18) . . ?
C28 N21 C24 113.0(2) . . ?
C26 N21 C24 108.50(19) . . ?
C28 N21 C22 113.4(2) . . ?
C26 N21 C22 108.2(2) . . ?
C24 N21 C22 101.88(17) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 179.01(12) . 2_656 ?
H23A C23 H23A 69.5 . 2_656 ?
H23B C23 H23A 71.0 . 2_656 ?
H23C C23 H23A 71.0 . 2_656 ?
C22 C23 H23B 70.04(14) . 2_656 ?
H23A C23 H23B 71.0 . 2_656 ?
H23B C23 H23B 179.4 . 2_656 ?
H23C C23 H23B 70.5 . 2_656 ?
H23A C23 H23B 109.5 2_656 2_656 ?
C22 C23 H23C 70.04(14) . 2_656 ?
H23A C23 H23C 71.0 . 2_656 ?
H23B C23 H23C 70.5 . 2_656 ?
H23C C23 H23C 179.4 . 2_656 ?
H23A C23 H23C 109.5 2_656 2_656 ?
H23B C23 H23C 109.5 2_656 2_656 ?
N21 C22 C23 106.9(2) . . ?
N21 C22 H22A 110.3 . . ?
C23 C22 H22A 110.3 . . ?
N21 C22 H22B 110.3 . . ?
C23 C22 H22B 110.3 . . ?
H22A C22 H22B 108.6 . . ?
N21 C22 H23B 120.9(2) . 2_656 ?
C23 C22 H23B 35.76(8) . 2_656 ?
H22A C22 H23B 123.9 . 2_656 ?
H22B C22 H23B 74.6 . 2_656 ?
N21 C22 H23C 120.9(2) . 2_656 ?
C23 C22 H23C 35.76(8) . 2_656 ?
H22A C22 H23C 74.6 . 2_656 ?
H22B C22 H23C 123.9 . 2_656 ?
H23B C22 H23C 61.0 2_656 2_656 ?
C25 C24 N21 113.1(2) . . ?
C25 C24 H24A 109.0 . . ?
N21 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
N21 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N21 118.4(5) . . ?
C27 C26 H26A 107.7 . . ?
N21 C26 H26A 107.7 . . ?
C27 C26 H26B 107.7 . . ?
N21 C26 H26B 107.7 . . ?
H26A C26 H26B 107.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N21 C28 C29 116.1(4) . . ?
N21 C28 H28A 108.3 . . ?
C29 C28 H28A 108.3 . . ?
N21 C28 H28B 108.3 . . ?
C29 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C1 C2 -1.85(14) . . . . ?
Ni1 S1 C1 S3 179.85(7) . . . . ?
C3 S3 C1 C2 -39.44(15) . . . . ?
C3 S3 C1 S1 138.81(9) . . . . ?
S1 C1 C2 S2 -2.25(19) . . . . ?
S3 C1 C2 S2 175.94(8) . . . . ?
S1 C1 C2 S4 178.99(8) . . . . ?
S3 C1 C2 S4 -2.8(2) . . . . ?
Ni1 S2 C2 C1 5.09(14) . . . . ?
Ni1 S2 C2 S4 -176.08(7) . . . . ?
C4 S4 C2 C1 42.43(15) . . . . ?
C4 S4 C2 S2 -136.37(9) . . . . ?
C1 S3 C3 N8 -139.98(12) . . . . ?
C1 S3 C3 C4 42.02(14) . . . . ?
N8 C3 C4 N5 -2.0(2) . . . . ?
S3 C3 C4 N5 175.95(12) . . . . ?
N8 C3 C4 S4 179.27(12) . . . . ?
S3 C3 C4 S4 -2.83(19) . . . . ?
C2 S4 C4 N5 142.33(12) . . . . ?
C2 S4 C4 C3 -38.82(14) . . . . ?
C3 C4 N5 C6 1.0(2) . . . . ?
S4 C4 N5 C6 179.83(12) . . . . ?
C4 N5 C6 C7 0.4(2) . . . . ?
N5 C6 C7 N8 -1.0(3) . . . . ?
C4 C3 N8 C7 1.3(2) . . . . ?
S3 C3 N8 C7 -176.67(12) . . . . ?
C6 C7 N8 C3 0.1(2) . . . . ?
C28 N21 C22 C23 54.2(3) . . . . ?
C26 N21 C22 C23 -69.9(3) . . . . ?
C24 N21 C22 C23 175.9(2) . . . . ?
C28 N21 C24 C25 -61.9(3) . . . . ?
C26 N21 C24 C25 62.0(3) . . . . ?
C22 N21 C24 C25 176.1(3) . . . . ?
C28 N21 C26 C27 175.0(5) . . . . ?
C24 N21 C26 C27 50.1(5) . . . . ?
C22 N21 C26 C27 -59.7(5) . . . . ?
C26 N21 C28 C29 179.1(5) . . . . ?
C24 N21 C28 C29 -58.5(5) . . . . ?
C22 N21 C28 C29 56.8(5) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: test3.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: test3.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR HK317_2                                                #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_chemical_name_common            (Et4N)[Ni(pzdtdt)2]
_chemical_melting_point          513
####################################################################### 
# 
# 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_HK130
_database_code_depnum_ccdc_archive 'CCDC 2422634'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2025-02-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 15 novembre 2022                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
"[1,3]dithiolo[4',5':5,6][1,4]dithiino[2,3-b]pyrazin-2-one"
_chemical_formula_moiety         'C7 H2 N2 O S4'
_chemical_formula_sum            'C7 H2 N2 O S4'
_chemical_formula_weight         258.35
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
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                   12.5503(10)
_cell_length_b                   3.8827(3)
_cell_length_c                   19.3569(17)
_cell_angle_alpha                90
_cell_angle_beta                 101.122(3)
_cell_angle_gamma                90
_cell_volume                     925.53(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9839
_cell_measurement_theta_min      3.8925
_cell_measurement_theta_max      27.4422
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0538582
_diffrn_orient_matrix_UB_21      -0.0187483
_diffrn_orient_matrix_UB_31      -0.0578099
_diffrn_orient_matrix_UB_12      0.1912877
_diffrn_orient_matrix_UB_22      -0.0824822
_diffrn_orient_matrix_UB_32      -0.1514622
_diffrn_orient_matrix_UB_13      -0.0115000
_diffrn_orient_matrix_UB_23      -0.0498095
_diffrn_orient_matrix_UB_33      0.0126011


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             520
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.933

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.1-1        #
# Number of scans            :        3                                        #
# Total number of frames [*] :      626                                        #
# Total length of scans  [*] :   313.00 (deg.)                                 #
# Rotation speed         [*] :    30.00 sec./deg.                              #
# Total exposition time  [*] :      2 h    36 min.                             #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     3.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Phi     15.0  0.50    34.0   432  216.0    0.1  270.3  324.0   24.0 150.0 #
#  3 Omega   15.0  0.50    34.0   194   97.0    0.1    2.7   72.0  -44.5 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0235
_diffrn_reflns_av_r_equivalents  0.0276
_diffrn_reflns_number            9875
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.309
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             2059
_reflns_number_gt                1996
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.

;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0281P)²+0.5260P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         2059
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0582
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.43367(10) 0.8416(3) 0.71957(6) 0.0158(2) Uani 1 1 d . . . . .
N2 N 0.45334(10) 0.7384(3) 0.78639(6) 0.0202(2) Uani 1 1 d . . . . .
C3 C 0.55177(12) 0.6034(4) 0.81062(7) 0.0242(3) Uani 1 1 d . . . . .
H3 H 0.569357 0.527480 0.858118 0.029 Uiso 1 1 calc R U . . .
C4 C 0.62860(12) 0.5715(4) 0.76826(8) 0.0261(3) Uani 1 1 d . . . . .
H4 H 0.697764 0.477951 0.787884 0.031 Uiso 1 1 calc R U . . .
N5 N 0.60845(10) 0.6686(3) 0.70046(6) 0.0235(2) Uani 1 1 d . . . . .
C6 C 0.51088(10) 0.8035(3) 0.67640(6) 0.0169(3) Uani 1 1 d . . . . .
C7 C 0.27577(10) 0.8752(3) 0.60520(6) 0.0152(2) Uani 1 1 d . . . . .
C8 C 0.34829(10) 0.8367(3) 0.56309(6) 0.0159(2) Uani 1 1 d . . . . .
C9 C 0.16763(11) 0.5674(4) 0.49416(7) 0.0208(3) Uani 1 1 d . . . . .
O10 O 0.09982(9) 0.4279(3) 0.45068(5) 0.0315(3) Uani 1 1 d . . . . .
S1 S 0.30721(2) 1.04725(8) 0.69040(2) 0.01642(9) Uani 1 1 d . . . . .
S2 S 0.48562(3) 0.95221(9) 0.58812(2) 0.01931(10) Uani 1 1 d . . . . .
S3 S 0.30312(3) 0.63830(9) 0.48189(2) 0.01946(10) Uani 1 1 d . . . . .
S4 S 0.14452(2) 0.71877(9) 0.57648(2) 0.01865(10) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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
C1 N2 1.3310(16) . ?
C1 C6 1.4041(18) . ?
C1 S1 1.7691(13) . ?
N2 C3 1.3406(18) . ?
C3 C4 1.387(2) . ?
C3 H3 0.9500 . ?
C4 N5 1.3417(19) . ?
C4 H4 0.9500 . ?
N5 C6 1.3308(17) . ?
C6 S2 1.7733(13) . ?
C7 C8 1.3421(18) . ?
C7 S4 1.7431(13) . ?
C7 S1 1.7523(13) . ?
C8 S3 1.7439(13) . ?
C8 S2 1.7562(13) . ?
C9 O10 1.2040(17) . ?
C9 S4 1.7741(14) . ?
C9 S3 1.7831(14) . ?

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
N2 C1 C6 121.79(12) . . ?
N2 C1 S1 115.65(10) . . ?
C6 C1 S1 122.50(9) . . ?
C1 N2 C3 116.32(12) . . ?
N2 C3 C4 121.80(13) . . ?
N2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
N5 C4 C3 122.14(13) . . ?
N5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C6 N5 C4 116.11(12) . . ?
N5 C6 C1 121.82(12) . . ?
N5 C6 S2 116.54(10) . . ?
C1 C6 S2 121.57(10) . . ?
C8 C7 S4 118.51(10) . . ?
C8 C7 S1 123.93(10) . . ?
S4 C7 S1 117.41(7) . . ?
C7 C8 S3 117.13(10) . . ?
C7 C8 S2 123.26(10) . . ?
S3 C8 S2 119.50(7) . . ?
O10 C9 S4 124.12(11) . . ?
O10 C9 S3 122.69(11) . . ?
S4 C9 S3 113.19(7) . . ?
C7 S1 C1 98.83(6) . . ?
C8 S2 C6 99.56(6) . . ?
C8 S3 C9 95.78(6) . . ?
C7 S4 C9 95.38(6) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 N2 C3 1.47(19) . . . . ?
S1 C1 N2 C3 -175.60(10) . . . . ?
C1 N2 C3 C4 -0.3(2) . . . . ?
N2 C3 C4 N5 -1.1(2) . . . . ?
C3 C4 N5 C6 1.2(2) . . . . ?
C4 N5 C6 C1 0.0(2) . . . . ?
C4 N5 C6 S2 177.01(11) . . . . ?
N2 C1 C6 N5 -1.4(2) . . . . ?
S1 C1 C6 N5 175.51(10) . . . . ?
N2 C1 C6 S2 -178.25(10) . . . . ?
S1 C1 C6 S2 -1.38(16) . . . . ?
S4 C7 C8 S3 1.17(15) . . . . ?
S1 C7 C8 S3 176.53(7) . . . . ?
S4 C7 C8 S2 -175.00(7) . . . . ?
S1 C7 C8 S2 0.35(18) . . . . ?
C8 C7 S1 C1 -41.51(13) . . . . ?
S4 C7 S1 C1 133.90(8) . . . . ?
N2 C1 S1 C7 -141.72(10) . . . . ?
C6 C1 S1 C7 41.23(12) . . . . ?
C7 C8 S2 C6 40.84(13) . . . . ?
S3 C8 S2 C6 -135.25(8) . . . . ?
N5 C6 S2 C8 143.55(11) . . . . ?
C1 C6 S2 C8 -39.41(12) . . . . ?
C7 C8 S3 C9 -0.61(12) . . . . ?
S2 C8 S3 C9 175.71(8) . . . . ?
O10 C9 S3 C8 -179.54(13) . . . . ?
S4 C9 S3 C8 -0.11(9) . . . . ?
C8 C7 S4 C9 -1.06(12) . . . . ?
S1 C7 S4 C9 -176.72(8) . . . . ?
O10 C9 S4 C7 180.00(13) . . . . ?
S3 C9 S4 C7 0.58(8) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR HK130                                                  #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_chemical_melting_point          462
####################################################################### 
# 
# 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_HK142
_database_code_depnum_ccdc_archive 'CCDC 2422637'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2025-02-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 07 decembre 2022                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
(tetraphenylphosphonium)[bis([1,4]dithiino[2,3-b]pyrazine-2,3-bis(thiolate))aurate)
_chemical_formula_moiety         '        C12 H4 Au N4 S8, C24 H20 P'
_chemical_formula_sum            'C36 H24 Au N4 P S8'
_chemical_formula_weight         997.01
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4285(8)
_cell_length_b                   11.7655(11)
_cell_length_c                   19.481(2)
_cell_angle_alpha                104.095(4)
_cell_angle_beta                 99.229(4)
_cell_angle_gamma                90.809(4)
_cell_volume                     1846.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9893
_cell_measurement_theta_min      2.1872
_cell_measurement_theta_max      27.4801
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.1196584
_diffrn_orient_matrix_UB_21      -0.0108368
_diffrn_orient_matrix_UB_31      -0.0075733
_diffrn_orient_matrix_UB_12      0.0013781
_diffrn_orient_matrix_UB_22      -0.0083134
_diffrn_orient_matrix_UB_32      -0.0873624
_diffrn_orient_matrix_UB_13      -0.0037999
_diffrn_orient_matrix_UB_23      -0.0528902
_diffrn_orient_matrix_UB_33      -0.0084616


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             980
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_T_max  0.798

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.1-1        #
# Number of scans            :        5                                        #
# Total number of frames [*] :      582                                        #
# Total length of scans  [*] :   291.00 (deg.)                                 #
# Rotation speed         [*] :    20.00 sec./deg.                              #
# Total exposition time  [*] :      1 h    37 min.                             #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     2.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@    2.0  1.00    34.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   10.0  0.50    34.0   194   97.0    0.1    2.7  144.0  -44.5 150.0 #
#  4 Omega   10.0  0.50    34.0   194   97.0    0.1    2.7  288.0  -44.5 150.0 #
#  5 Omega   10.0  0.50    34.0   194   97.0    0.1    2.7    0.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0393
_diffrn_reflns_av_r_equivalents  0.0284
_diffrn_reflns_number            21288
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.456
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_reflns_number_total             8370
_reflns_number_gt                7390
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.

;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²+0.9466P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         8370
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.122

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Au Au -2.0133 8.8022 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.500000 0.000000 0.000000 0.02803(6) Uani 1 2 d S . P . .
S1 S 0.56132(11) 0.07128(8) 0.12324(4) 0.03869(19) Uani 1 1 d . . . . .
S2 S 0.64927(11) -0.16070(8) 0.00799(4) 0.0397(2) Uani 1 1 d . . . . .
S3 S 0.64503(10) -0.04578(9) 0.23922(5) 0.0408(2) Uani 1 1 d . . . . .
S4 S 0.73047(9) -0.28037(7) 0.12369(5) 0.03503(18) Uani 1 1 d . . . . .
C1 C 0.6259(3) -0.0569(3) 0.14679(16) 0.0290(6) Uani 1 1 d . . . . .
C2 C 0.6623(3) -0.1517(3) 0.09977(17) 0.0282(6) Uani 1 1 d . . . . .
C3 C 0.8584(3) -0.2199(3) 0.20622(17) 0.0291(6) Uani 1 1 d . . . . .
N4 N 0.9859(3) -0.2812(3) 0.22127(18) 0.0352(6) Uani 1 1 d . . . . .
C5 C 1.0774(4) -0.2378(3) 0.2862(2) 0.0396(8) Uani 1 1 d . . . . .
H5 H 1.168036 -0.279218 0.300112 0.048 Uiso 1 1 calc R U . . .
C6 C 1.0456(4) -0.1366(3) 0.3331(2) 0.0424(8) Uani 1 1 d . . . . .
H6 H 1.116289 -0.109179 0.377568 0.051 Uiso 1 1 calc R U . . .
N7 N 0.9172(3) -0.0752(3) 0.31784(16) 0.0411(7) Uani 1 1 d . . . . .
C8 C 0.8241(3) -0.1188(3) 0.25479(17) 0.0306(6) Uani 1 1 d . . . . .
Au2 Au 0.500000 0.500000 0.500000 0.02148(5) Uani 1 2 d S . P . .
S11 S 0.28793(8) 0.36004(6) 0.45780(4) 0.02726(15) Uani 1 1 d . . . . .
S12 S 0.59831(8) 0.40938(6) 0.58967(4) 0.02712(15) Uani 1 1 d . . . . .
S13 S 0.15470(8) 0.18018(7) 0.51722(5) 0.03012(17) Uani 1 1 d . . . . .
S14 S 0.46618(9) 0.22381(7) 0.64516(4) 0.03091(16) Uani 1 1 d . . . . .
C11 C 0.4388(3) 0.3063(2) 0.57998(17) 0.0256(6) Uani 1 1 d . . . . .
C12 C 0.3124(3) 0.2863(2) 0.52650(17) 0.0250(6) Uani 1 1 d . . . . .
C13 C 0.2659(3) 0.0633(2) 0.53770(16) 0.0255(6) Uani 1 1 d . . . . .
N14 N 0.2078(3) -0.0444(2) 0.50262(14) 0.0296(5) Uani 1 1 d . . . . .
C15 C 0.2904(4) -0.1324(3) 0.51921(18) 0.0327(7) Uani 1 1 d . . . . .
H15 H 0.251236 -0.210713 0.496132 0.039 Uiso 1 1 calc R U . . .
C16 C 0.4305(4) -0.1139(3) 0.56860(18) 0.0321(7) Uani 1 1 d . . . . .
H16 H 0.487046 -0.179697 0.577216 0.039 Uiso 1 1 calc R U . . .
N17 N 0.4896(3) -0.0056(2) 0.60494(14) 0.0297(5) Uani 1 1 d . . . . .
C18 C 0.4048(3) 0.0819(2) 0.59036(16) 0.0249(6) Uani 1 1 d . . . . .
P1 P 0.92115(8) 0.70055(6) 0.81239(4) 0.02312(15) Uani 1 1 d . . . . .
C21 C 0.8787(3) 0.8525(3) 0.82428(17) 0.0270(6) Uani 1 1 d . . . . .
C22 C 0.8005(3) 0.8903(3) 0.76544(17) 0.0291(6) Uani 1 1 d . . . . .
H22 H 0.773834 0.836562 0.719677 0.035 Uiso 1 1 calc R U . . .
C23 C 0.7623(4) 1.0059(3) 0.77421(19) 0.0329(7) Uani 1 1 d . . . . .
H23 H 0.707163 1.031650 0.734727 0.039 Uiso 1 1 calc R U . . .
C24 C 0.8042(5) 1.0839(3) 0.8403(2) 0.0450(9) Uani 1 1 d . . . . .
H24 H 0.778269 1.163641 0.846280 0.054 Uiso 1 1 calc R U . . .
C25 C 0.8832(6) 1.0471(3) 0.8978(2) 0.0561(11) Uani 1 1 d . . . . .
H25 H 0.912012 1.101956 0.943078 0.067 Uiso 1 1 calc R U . . .
C26 C 0.9216(5) 0.9308(3) 0.8906(2) 0.0436(9) Uani 1 1 d . . . . .
H26 H 0.976272 0.905639 0.930410 0.052 Uiso 1 1 calc R U . . .
C27 C 1.0495(3) 0.6748(2) 0.88919(17) 0.0262(6) Uani 1 1 d . . . . .
C28 C 0.9858(4) 0.6664(3) 0.95008(17) 0.0296(6) Uani 1 1 d . . . . .
H28 H 0.874853 0.677492 0.951544 0.036 Uiso 1 1 calc R U . . .
C29 C 1.0850(4) 0.6418(3) 1.00830(18) 0.0355(7) Uani 1 1 d . . . . .
H29 H 1.042829 0.637472 1.050047 0.043 Uiso 1 1 calc R U . . .
C30 C 1.2464(4) 0.6235(4) 1.0049(2) 0.0467(9) Uani 1 1 d . . . . .
H30 H 1.314020 0.604850 1.044121 0.056 Uiso 1 1 calc R U . . .
C31 C 1.3089(4) 0.6322(4) 0.9456(2) 0.0563(11) Uani 1 1 d . . . . .
H31 H 1.419643 0.620219 0.944127 0.068 Uiso 1 1 calc R U . . .
C32 C 1.2118(4) 0.6583(4) 0.8876(2) 0.0438(9) Uani 1 1 d . . . . .
H32 H 1.256202 0.664998 0.846821 0.053 Uiso 1 1 calc R U . . .
C33 C 1.0131(3) 0.6590(3) 0.73325(17) 0.0287(6) Uani 1 1 d . . . . .
C34 C 1.0941(4) 0.7438(3) 0.7112(2) 0.0407(8) Uani 1 1 d . . . . .
H34 H 1.106522 0.822806 0.739112 0.049 Uiso 1 1 calc R U . . .
C35 C 1.1571(5) 0.7117(4) 0.6475(2) 0.0572(12) Uani 1 1 d . . . . .
H35 H 1.209734 0.769392 0.631113 0.069 Uiso 1 1 calc R U . . .
C36 C 1.1429(5) 0.5968(5) 0.6087(2) 0.0559(12) Uani 1 1 d . . . . .
H36 H 1.186398 0.575346 0.565522 0.067 Uiso 1 1 calc R U . . .
C37 C 1.0660(4) 0.5120(4) 0.6316(2) 0.0493(10) Uani 1 1 d . . . . .
H37 H 1.059006 0.432407 0.604798 0.059 Uiso 1 1 calc R U . . .
C38 C 0.9993(3) 0.5427(3) 0.69353(18) 0.0356(7) Uani 1 1 d . . . . .
H38 H 0.944340 0.484734 0.708844 0.043 Uiso 1 1 calc R U . . .
C39 C 0.7397(3) 0.6106(2) 0.79943(15) 0.0233(5) Uani 1 1 d . . . . .
C40 C 0.7469(3) 0.5002(2) 0.81370(17) 0.0274(6) Uani 1 1 d . . . . .
H40 H 0.847592 0.473649 0.831327 0.033 Uiso 1 1 calc R U . . .
C41 C 0.6084(4) 0.4291(3) 0.80238(18) 0.0321(6) Uani 1 1 d . . . . .
H41 H 0.612995 0.354878 0.813572 0.038 Uiso 1 1 calc R U . . .
C42 C 0.4620(4) 0.4672(3) 0.77441(19) 0.0350(7) Uani 1 1 d . . . . .
H42 H 0.366335 0.418780 0.766362 0.042 Uiso 1 1 calc R U . . .
C43 C 0.4554(3) 0.5744(3) 0.7585(2) 0.0371(7) Uani 1 1 d . . . . .
H43 H 0.355368 0.598450 0.738147 0.045 Uiso 1 1 calc R U . . .
C44 C 0.5926(3) 0.6484(3) 0.77152(17) 0.0292(6) Uani 1 1 d . . . . .
H44 H 0.586336 0.723497 0.761604 0.035 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 S2 2.3085(8) . ?
Au1 S2 2.3086(8) 2_655 ?
Au1 S1 2.3116(9) . ?
Au1 S1 2.3117(9) 2_655 ?
S1 C1 1.750(3) . ?
S2 C2 1.751(3) . ?
S3 C1 1.754(3) . ?
S3 C8 1.768(3) . ?
S4 C3 1.766(3) . ?
S4 C2 1.766(3) . ?
C1 C2 1.334(4) . ?
C3 N4 1.336(4) . ?
C3 C8 1.394(5) . ?
N4 C5 1.348(5) . ?
C5 C6 1.372(6) . ?
C5 H5 0.9500 . ?
C6 N7 1.343(4) . ?
C6 H6 0.9500 . ?
N7 C8 1.327(4) . ?
Au2 S12 2.3113(8) 2_666 ?
Au2 S12 2.3114(8) . ?
Au2 S11 2.3170(7) . ?
Au2 S11 2.3171(7) 2_666 ?
S11 C12 1.751(3) . ?
S12 C11 1.754(3) . ?
S13 C13 1.764(3) . ?
S13 C12 1.768(3) . ?
S14 C11 1.766(3) . ?
S14 C18 1.768(3) . ?
C11 C12 1.339(4) . ?
C13 N14 1.329(4) . ?
C13 C18 1.404(4) . ?
N14 C15 1.331(4) . ?
C15 C16 1.376(5) . ?
C15 H15 0.9500 . ?
C16 N17 1.342(4) . ?
C16 H16 0.9500 . ?
N17 C18 1.323(4) . ?
P1 C27 1.792(3) . ?
P1 C21 1.794(3) . ?
P1 C39 1.795(3) . ?
P1 C33 1.801(3) . ?
C21 C26 1.382(5) . ?
C21 C22 1.401(4) . ?
C22 C23 1.377(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.388(4) . ?
C27 C28 1.402(4) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.370(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.389(5) . ?
C33 C38 1.392(5) . ?
C34 C35 1.397(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.372(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.384(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.393(4) . ?
C39 C44 1.395(4) . ?
C40 C41 1.383(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.393(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.369(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?

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
S2 Au1 S2 180.0 . 2_655 ?
S2 Au1 S1 89.85(3) . . ?
S2 Au1 S1 90.15(3) 2_655 . ?
S2 Au1 S1 90.15(3) . 2_655 ?
S2 Au1 S1 89.85(3) 2_655 2_655 ?
S1 Au1 S1 180.0 . 2_655 ?
C1 S1 Au1 99.43(11) . . ?
C2 S2 Au1 99.60(10) . . ?
C1 S3 C8 101.13(14) . . ?
C3 S4 C2 100.95(15) . . ?
C2 C1 S1 123.6(2) . . ?
C2 C1 S3 123.5(2) . . ?
S1 C1 S3 112.92(18) . . ?
C1 C2 S2 123.3(2) . . ?
C1 C2 S4 123.6(2) . . ?
S2 C2 S4 113.09(17) . . ?
N4 C3 C8 121.8(3) . . ?
N4 C3 S4 115.6(3) . . ?
C8 C3 S4 122.5(2) . . ?
C3 N4 C5 115.1(3) . . ?
N4 C5 C6 123.0(3) . . ?
N4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
N7 C6 C5 121.8(3) . . ?
N7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C8 N7 C6 115.7(3) . . ?
N7 C8 C3 122.7(3) . . ?
N7 C8 S3 115.2(3) . . ?
C3 C8 S3 122.0(2) . . ?
S12 Au2 S12 180.00(3) 2_666 . ?
S12 Au2 S11 89.23(3) 2_666 . ?
S12 Au2 S11 90.77(3) . . ?
S12 Au2 S11 90.77(3) 2_666 2_666 ?
S12 Au2 S11 89.23(3) . 2_666 ?
S11 Au2 S11 180.0 . 2_666 ?
C12 S11 Au2 100.17(9) . . ?
C11 S12 Au2 100.11(10) . . ?
C13 S13 C12 100.42(13) . . ?
C11 S14 C18 100.20(14) . . ?
C12 C11 S12 124.1(2) . . ?
C12 C11 S14 122.6(2) . . ?
S12 C11 S14 113.27(16) . . ?
C11 C12 S11 123.7(2) . . ?
C11 C12 S13 123.1(2) . . ?
S11 C12 S13 113.11(16) . . ?
N14 C13 C18 121.2(3) . . ?
N14 C13 S13 116.5(2) . . ?
C18 C13 S13 122.2(2) . . ?
C13 N14 C15 116.3(3) . . ?
N14 C15 C16 122.3(3) . . ?
N14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
N17 C16 C15 121.9(3) . . ?
N17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C18 N17 C16 115.9(3) . . ?
N17 C18 C13 122.2(3) . . ?
N17 C18 S14 116.7(2) . . ?
C13 C18 S14 121.0(2) . . ?
C27 P1 C21 111.92(14) . . ?
C27 P1 C39 106.70(13) . . ?
C21 P1 C39 111.04(13) . . ?
C27 P1 C33 111.13(13) . . ?
C21 P1 C33 107.07(15) . . ?
C39 P1 C33 108.99(14) . . ?
C26 C21 C22 120.5(3) . . ?
C26 C21 P1 120.5(2) . . ?
C22 C21 P1 119.0(2) . . ?
C23 C22 C21 119.7(3) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.9(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 118.6(3) . . ?
C21 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
C32 C27 C28 119.5(3) . . ?
C32 C27 P1 120.1(3) . . ?
C28 C27 P1 120.3(2) . . ?
C29 C28 C27 120.0(3) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.4(3) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C31 C30 C29 120.6(3) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 120.5(3) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 119.9(3) . . ?
C31 C32 H32 120.0 . . ?
C27 C32 H32 120.0 . . ?
C34 C33 C38 120.3(3) . . ?
C34 C33 P1 119.8(3) . . ?
C38 C33 P1 119.8(2) . . ?
C33 C34 C35 119.2(4) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C36 C35 C34 120.0(4) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C37 120.7(4) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C36 C37 C38 120.1(4) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C37 C38 C33 119.6(4) . . ?
C37 C38 H38 120.2 . . ?
C33 C38 H38 120.2 . . ?
C40 C39 C44 119.9(3) . . ?
C40 C39 P1 119.9(2) . . ?
C44 C39 P1 120.2(2) . . ?
C41 C40 C39 120.4(3) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C42 119.4(3) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C43 C42 C41 120.2(3) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C44 121.1(3) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C43 C44 C39 118.9(3) . . ?
C43 C44 H44 120.5 . . ?
C39 C44 H44 120.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Au1 S1 C1 C2 14.5(3) . . . . ?
Au1 S1 C1 S3 -167.66(14) . . . . ?
C8 S3 C1 C2 38.1(3) . . . . ?
C8 S3 C1 S1 -139.73(18) . . . . ?
S1 C1 C2 S2 -0.3(4) . . . . ?
S3 C1 C2 S2 -177.86(17) . . . . ?
S1 C1 C2 S4 179.00(17) . . . . ?
S3 C1 C2 S4 1.4(4) . . . . ?
Au1 S2 C2 C1 -14.2(3) . . . . ?
Au1 S2 C2 S4 166.47(13) . . . . ?
C3 S4 C2 C1 -39.1(3) . . . . ?
C3 S4 C2 S2 140.25(17) . . . . ?
C2 S4 C3 N4 -147.6(2) . . . . ?
C2 S4 C3 C8 36.2(3) . . . . ?
C8 C3 N4 C5 -0.1(5) . . . . ?
S4 C3 N4 C5 -176.3(3) . . . . ?
C3 N4 C5 C6 -1.6(5) . . . . ?
N4 C5 C6 N7 1.8(6) . . . . ?
C5 C6 N7 C8 -0.1(5) . . . . ?
C6 N7 C8 C3 -1.7(5) . . . . ?
C6 N7 C8 S3 173.9(2) . . . . ?
N4 C3 C8 N7 1.8(5) . . . . ?
S4 C3 C8 N7 177.8(3) . . . . ?
N4 C3 C8 S3 -173.4(2) . . . . ?
S4 C3 C8 S3 2.6(4) . . . . ?
C1 S3 C8 N7 144.8(3) . . . . ?
C1 S3 C8 C3 -39.6(3) . . . . ?
Au2 S12 C11 C12 7.2(3) . . . . ?
Au2 S12 C11 S14 -176.33(13) . . . . ?
C18 S14 C11 C12 40.2(3) . . . . ?
C18 S14 C11 S12 -136.30(16) . . . . ?
S12 C11 C12 S11 0.3(4) . . . . ?
S14 C11 C12 S11 -175.81(16) . . . . ?
S12 C11 C12 S13 178.96(16) . . . . ?
S14 C11 C12 S13 2.9(4) . . . . ?
Au2 S11 C12 C11 -7.6(3) . . . . ?
Au2 S11 C12 S13 173.59(13) . . . . ?
C13 S13 C12 C11 -42.1(3) . . . . ?
C13 S13 C12 S11 136.69(16) . . . . ?
C12 S13 C13 N14 -145.9(2) . . . . ?
C12 S13 C13 C18 36.7(3) . . . . ?
C18 C13 N14 C15 -1.4(4) . . . . ?
S13 C13 N14 C15 -178.8(2) . . . . ?
C13 N14 C15 C16 -1.5(4) . . . . ?
N14 C15 C16 N17 2.3(5) . . . . ?
C15 C16 N17 C18 0.1(4) . . . . ?
C16 N17 C18 C13 -3.0(4) . . . . ?
C16 N17 C18 S14 172.5(2) . . . . ?
N14 C13 C18 N17 3.8(4) . . . . ?
S13 C13 C18 N17 -178.9(2) . . . . ?
N14 C13 C18 S14 -171.4(2) . . . . ?
S13 C13 C18 S14 5.8(3) . . . . ?
C11 S14 C18 N17 140.3(2) . . . . ?
C11 S14 C18 C13 -44.2(3) . . . . ?
C27 P1 C21 C26 -9.9(3) . . . . ?
C39 P1 C21 C26 109.2(3) . . . . ?
C33 P1 C21 C26 -131.9(3) . . . . ?
C27 P1 C21 C22 170.5(2) . . . . ?
C39 P1 C21 C22 -70.4(3) . . . . ?
C33 P1 C21 C22 48.5(3) . . . . ?
C26 C21 C22 C23 -1.7(5) . . . . ?
P1 C21 C22 C23 177.9(2) . . . . ?
C21 C22 C23 C24 1.3(5) . . . . ?
C22 C23 C24 C25 -0.3(6) . . . . ?
C23 C24 C25 C26 -0.4(7) . . . . ?
C22 C21 C26 C25 1.0(6) . . . . ?
P1 C21 C26 C25 -178.6(3) . . . . ?
C24 C25 C26 C21 0.0(7) . . . . ?
C21 P1 C27 C32 -102.7(3) . . . . ?
C39 P1 C27 C32 135.6(3) . . . . ?
C33 P1 C27 C32 16.9(3) . . . . ?
C21 P1 C27 C28 79.8(3) . . . . ?
C39 P1 C27 C28 -41.8(3) . . . . ?
C33 P1 C27 C28 -160.5(2) . . . . ?
C32 C27 C28 C29 0.0(5) . . . . ?
P1 C27 C28 C29 177.5(2) . . . . ?
C27 C28 C29 C30 -1.2(5) . . . . ?
C28 C29 C30 C31 1.5(6) . . . . ?
C29 C30 C31 C32 -0.6(7) . . . . ?
C30 C31 C32 C27 -0.6(7) . . . . ?
C28 C27 C32 C31 0.9(6) . . . . ?
P1 C27 C32 C31 -176.6(3) . . . . ?
C27 P1 C33 C34 -97.3(3) . . . . ?
C21 P1 C33 C34 25.2(3) . . . . ?
C39 P1 C33 C34 145.4(3) . . . . ?
C27 P1 C33 C38 84.2(3) . . . . ?
C21 P1 C33 C38 -153.3(2) . . . . ?
C39 P1 C33 C38 -33.1(3) . . . . ?
C38 C33 C34 C35 2.0(5) . . . . ?
P1 C33 C34 C35 -176.4(3) . . . . ?
C33 C34 C35 C36 -2.0(6) . . . . ?
C34 C35 C36 C37 0.3(6) . . . . ?
C35 C36 C37 C38 1.4(6) . . . . ?
C36 C37 C38 C33 -1.3(5) . . . . ?
C34 C33 C38 C37 -0.4(5) . . . . ?
P1 C33 C38 C37 178.1(3) . . . . ?
C27 P1 C39 C40 -35.7(3) . . . . ?
C21 P1 C39 C40 -157.9(2) . . . . ?
C33 P1 C39 C40 84.4(3) . . . . ?
C27 P1 C39 C44 147.7(2) . . . . ?
C21 P1 C39 C44 25.5(3) . . . . ?
C33 P1 C39 C44 -92.2(3) . . . . ?
C44 C39 C40 C41 -1.9(5) . . . . ?
P1 C39 C40 C41 -178.5(2) . . . . ?
C39 C40 C41 C42 2.0(5) . . . . ?
C40 C41 C42 C43 -0.2(5) . . . . ?
C41 C42 C43 C44 -1.8(5) . . . . ?
C42 C43 C44 C39 1.9(5) . . . . ?
C40 C39 C44 C43 0.0(5) . . . . ?
P1 C39 C44 C43 176.6(2) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR HK142                                                  #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
_chemical_name_common            (Ph4P)[Au(pzdtdt)2]
_chemical_melting_point          '> 523'
####################################################################### 
# 
# 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_HKC161
_database_code_depnum_ccdc_archive 'CCDC 2422636'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;CDIFX ISCR CNRS Univ Rennes
France
;
_audit_update_record             
;
2025-02-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 04 mars 2024                                             #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H4 Au N4 S8'
_chemical_formula_sum            'C12 H4 Au N4 S8'
_chemical_formula_weight         657.64
_chemical_compound_source        'synthesis as described'

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
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                   3.7034(5)
_cell_length_b                   30.203(4)
_cell_length_c                   7.5483(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.492(5)
_cell_angle_gamma                90
_cell_volume                     835.05(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7147
_cell_measurement_theta_min      2.6975
_cell_measurement_theta_max      27.5094
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0804183
_diffrn_orient_matrix_UB_21      0.2545670
_diffrn_orient_matrix_UB_31      -0.0571338
_diffrn_orient_matrix_UB_12      -0.0288335
_diffrn_orient_matrix_UB_22      -0.0116572
_diffrn_orient_matrix_UB_32      -0.0113558
_diffrn_orient_matrix_UB_13      -0.0579560
_diffrn_orient_matrix_UB_23      0.0292033
_diffrn_orient_matrix_UB_33      0.1171774


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       stick
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.025
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.615
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             622
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    9.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.782

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.10-0       #
# Total number of scans:        5                                              #
#                                                                              #
# ....[fast scans included]:                                                   #
#    . Total number of frames :      942                                       #
#    . Total length of scans  :   651.00 (deg.)                                #
#    . Mean rotation speed    :    77.96 sec./deg.                             #
#    . Total exposition time  :     10 h 42 min. [642 min.]                    #
#                                                                              #
#                                                                              #
# ....[fast scans excluded]:                                                   #
#    . Total number of frames :      582                                       #
#    . Total length of scans  :   291.00 (deg.)                                #
#    . Mean rotation speed    :   120.00 sec./deg.                             #
#    . Total exposition time  :      9 h 42 min. [582 min.]                    #
#                                                                              #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast    10.0  1.00    37.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Fast@   10.0  1.00    37.0   180  180.0    0.0    0.0  180.0   54.7 150.0 #
#  3 Omega   60.0  0.50    34.0   194   97.0    0.1    2.7    0.0  -44.5 150.0 #
#  4 Omega   60.0  0.50    34.0   194   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  5 Omega   60.0  0.50    34.0   194   97.0    0.1    2.7  216.0  -44.5 150.0 #
#                                                                              #
#  @: attenuated beam                                                          #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0279
_diffrn_reflns_av_r_equivalents  0.0308
_diffrn_reflns_number            7629
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.698
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             1914
_reflns_number_gt                1848
_reflns_threshold_expression     >2sigma(I)

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal class for the
calculation of statistics and refinement.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+13.2011P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         1914
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.534
_refine_ls_restrained_S_all      1.534
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.208

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
N N 0.0061 0.0033 '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'

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 0.000000 0.500000 0.000000 0.01768(15) Uani 1 2 d S . P . .
S1 S 0.0571(7) 0.57447(7) -0.0572(3) 0.0193(4) Uani 1 1 d . . . . .
S2 S 0.1608(7) 0.51324(7) 0.3002(3) 0.0188(4) Uani 1 1 d . . . . .
S3 S 0.3675(7) 0.65002(8) 0.1483(3) 0.0211(5) Uani 1 1 d . . . . .
S4 S 0.4629(6) 0.58696(7) 0.5165(3) 0.0181(4) Uani 1 1 d . . . . .
C1 C 0.234(2) 0.5940(3) 0.1525(13) 0.0186(18) Uani 1 1 d . . . . .
C2 C 0.275(2) 0.5686(3) 0.3017(12) 0.0190(18) Uani 1 1 d . . . . .
C3 C 0.279(2) 0.6691(3) 0.3580(13) 0.0200(18) Uani 1 1 d . . . . .
C4 C 0.312(2) 0.6425(3) 0.5128(12) 0.0162(17) Uani 1 1 d . . . . .
N5 N 0.253(2) 0.6582(3) 0.6698(11) 0.0241(17) Uani 1 1 d . . . . .
C6 C 0.165(3) 0.7010(3) 0.6746(15) 0.026(2) Uani 1 1 d . . . . .
H6 H 0.117218 0.713588 0.784166 0.031 Uiso 1 1 calc R U . . .
C7 C 0.142(3) 0.7273(3) 0.5243(15) 0.030(2) Uani 1 1 d . . . . .
H7 H 0.084847 0.757819 0.534362 0.036 Uiso 1 1 calc R U . . .
N8 N 0.197(2) 0.7117(3) 0.3647(12) 0.0271(19) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 S2 2.291(2) 3_565 ?
Au1 S2 2.291(2) . ?
Au1 S1 2.306(2) . ?
Au1 S1 2.306(2) 3_565 ?
S1 C1 1.725(10) . ?
S2 C2 1.723(9) . ?
S3 C3 1.760(10) . ?
S3 C1 1.764(9) . ?
S4 C2 1.758(9) . ?
S4 C4 1.768(9) . ?
C1 C2 1.354(13) . ?
C3 N8 1.325(12) . ?
C3 C4 1.407(13) . ?
C4 N5 1.324(12) . ?
N5 C6 1.334(12) . ?
C6 C7 1.379(15) . ?
C6 H6 0.9500 . ?
C7 N8 1.337(14) . ?
C7 H7 0.9500 . ?

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
S2 Au1 S2 180.00(11) 3_565 . ?
S2 Au1 S1 90.15(8) 3_565 . ?
S2 Au1 S1 89.85(8) . . ?
S2 Au1 S1 89.85(8) 3_565 3_565 ?
S2 Au1 S1 90.15(8) . 3_565 ?
S1 Au1 S1 180.0 . 3_565 ?
C1 S1 Au1 101.2(3) . . ?
C2 S2 Au1 101.7(3) . . ?
C3 S3 C1 102.0(4) . . ?
C2 S4 C4 101.8(4) . . ?
C2 C1 S1 123.3(7) . . ?
C2 C1 S3 124.2(7) . . ?
S1 C1 S3 112.4(5) . . ?
C1 C2 S2 123.2(7) . . ?
C1 C2 S4 124.6(7) . . ?
S2 C2 S4 112.1(5) . . ?
N8 C3 C4 121.0(9) . . ?
N8 C3 S3 115.2(8) . . ?
C4 C3 S3 123.7(7) . . ?
N5 C4 C3 122.2(8) . . ?
N5 C4 S4 114.8(7) . . ?
C3 C4 S4 122.9(7) . . ?
C4 N5 C6 116.4(9) . . ?
N5 C6 C7 121.5(10) . . ?
N5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
N8 C7 C6 122.6(9) . . ?
N8 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C3 N8 C7 116.4(9) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Au1 S1 C1 C2 -6.0(8) . . . . ?
Au1 S1 C1 S3 172.1(4) . . . . ?
C3 S3 C1 C2 -34.6(9) . . . . ?
C3 S3 C1 S1 147.4(5) . . . . ?
S1 C1 C2 S2 0.8(12) . . . . ?
S3 C1 C2 S2 -177.0(5) . . . . ?
S1 C1 C2 S4 178.6(5) . . . . ?
S3 C1 C2 S4 0.7(12) . . . . ?
Au1 S2 C2 C1 4.9(8) . . . . ?
Au1 S2 C2 S4 -173.1(4) . . . . ?
C4 S4 C2 C1 34.3(9) . . . . ?
C4 S4 C2 S2 -147.7(5) . . . . ?
C1 S3 C3 N8 -151.3(7) . . . . ?
C1 S3 C3 C4 32.5(8) . . . . ?
N8 C3 C4 N5 2.1(13) . . . . ?
S3 C3 C4 N5 178.1(7) . . . . ?
N8 C3 C4 S4 -173.7(7) . . . . ?
S3 C3 C4 S4 2.3(11) . . . . ?
C2 S4 C4 N5 148.5(7) . . . . ?
C2 S4 C4 C3 -35.4(8) . . . . ?
C3 C4 N5 C6 -1.0(13) . . . . ?
S4 C4 N5 C6 175.1(7) . . . . ?
C4 N5 C6 C7 -0.8(15) . . . . ?
N5 C6 C7 N8 1.6(17) . . . . ?
C4 C3 N8 C7 -1.2(14) . . . . ?
S3 C3 N8 C7 -177.5(8) . . . . ?
C6 C7 N8 C3 -0.5(16) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................



# ............... End of .RES file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .HKL SHELXL file: job.hkl
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR HKC161                                                 #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
