# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_2248jbc7
_database_code_depnum_ccdc_archive 'CCDC 2204793'
loop_
_audit_author_name
_audit_author_address
'Paul Bernhardt'
;The University of Queensland
Australia
;
_audit_update_record             
;
2022-09-01 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_2248jbc7            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: theta limit of dual source diffractometer reached.
;
# Added during the CSD deposition process: Thursday 01 September 2022 12:53 PM
# end Validation Reply Form


_audit_creation_date             2022-07-14T17:20:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_formula_sum            'C21 H21 Cu N4 S4'
_chemical_formula_weight         521.2

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_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                   23.8933(4)
_cell_length_b                   8.90930(10)
_cell_length_c                   10.5529(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.058(2)
_cell_angle_gamma                90
_cell_volume                     2218.41(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    3828
_cell_measurement_theta_min      5.29
_cell_measurement_theta_max      61.43
_cell_measurement_wavelength     1.54184

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

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072

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

_exptl_absorpt_coefficient_mu    5.039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.238
_shelx_estimated_absorpt_T_max   0.824

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

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_orient_matrix_ub_11      0.02505
_diffrn_orient_matrix_ub_12      0.140522
_diffrn_orient_matrix_ub_13      -0.055042
_diffrn_orient_matrix_ub_21      0.005127
_diffrn_orient_matrix_ub_22      -0.086857
_diffrn_orient_matrix_ub_23      -0.123836
_diffrn_orient_matrix_ub_31      -0.060092
_diffrn_orient_matrix_ub_32      0.051292
_diffrn_orient_matrix_ub_33      -0.058878
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  
'Agilent Technologies Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_number            5249
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.747
_diffrn_reflns_theta_max         61.567
_diffrn_reflns_theta_full        61.567
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             1720
_reflns_number_gt                1638
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom

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

_shelx_SHELXL_version_number     2018/1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+9.6077P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1720
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1677
_refine_ls_wR_factor_gt          0.1658
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.124

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 0.5 0.8582(7) 0.75 0.0519(17) Uani 1 2 d S T P . .
H1 H 0.499999 0.964788 0.749997 0.062 Uiso 1 2 calc R U P . .
C2 C 0.53396(17) 0.7902(5) 0.6691(5) 0.0507(12) Uani 1 1 d . . . . .
C3 C 0.5658(2) 0.8895(5) 0.5895(6) 0.0627(15) Uani 1 1 d . . . . .
H3A H 0.60661 0.880565 0.619863 0.094 Uiso 1 1 calc R U . . .
H3B H 0.554054 0.994015 0.597369 0.094 Uiso 1 1 calc R U . . .
H3C H 0.557546 0.858549 0.499335 0.094 Uiso 1 1 calc R U . . .
C4 C 0.58150(18) 0.4473(6) 0.5824(5) 0.0474(11) Uani 1 1 d . . . . .
C5 C 0.6667(2) 0.5094(6) 0.4349(4) 0.0504(12) Uani 1 1 d . . . . .
H5A H 0.678989 0.481426 0.352715 0.06 Uiso 1 1 calc R U . . .
H5B H 0.642827 0.600342 0.419398 0.06 Uiso 1 1 calc R U . . .
C6 C 0.71803(18) 0.5461(5) 0.5307(4) 0.0381(9) Uani 1 1 d . . . . .
C7 C 0.71681(19) 0.6625(5) 0.6183(4) 0.0419(10) Uani 1 1 d . . . . .
H7 H 0.682848 0.717849 0.618466 0.05 Uiso 1 1 calc R U . . .
C8 C 0.7645(2) 0.6982(5) 0.7051(4) 0.0449(10) Uani 1 1 d . . . . .
H8 H 0.7634 0.778291 0.764026 0.054 Uiso 1 1 calc R U . . .
C9 C 0.8136(2) 0.6178(6) 0.7059(4) 0.0499(11) Uani 1 1 d . . . . .
H9 H 0.846233 0.641451 0.766231 0.06 Uiso 1 1 calc R U . . .
C10 C 0.8155(2) 0.5025(5) 0.6192(5) 0.0493(12) Uani 1 1 d . . . . .
H10 H 0.849542 0.447211 0.619718 0.059 Uiso 1 1 calc R U . . .
C11 C 0.76827(19) 0.4676(5) 0.5322(4) 0.0444(10) Uani 1 1 d . . . . .
H11 H 0.770036 0.388799 0.472343 0.053 Uiso 1 1 calc R U . . .
Cu1 Cu 0.5 0.50093(9) 0.75 0.0408(4) Uani 1 2 d S T P . .
N1 N 0.53915(15) 0.6414(4) 0.6620(4) 0.0492(10) Uani 1 1 d . . . . .
N2 N 0.57673(15) 0.5919(4) 0.5844(4) 0.0480(10) Uani 1 1 d . . . . .
S1 S 0.54721(7) 0.32525(14) 0.67214(19) 0.0795(6) Uani 1 1 d . . . . .
S2 S 0.62404(5) 0.35705(14) 0.48496(13) 0.0539(4) 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 C2 1.404(6) 2_656 ?
C1 C2 1.404(6) . ?
C2 N1 1.335(6) . ?
C2 C3 1.507(7) . ?
C4 N2 1.294(6) . ?
C4 S1 1.730(5) . ?
C4 S2 1.751(5) . ?
C5 C6 1.497(6) . ?
C5 S2 1.825(5) . ?
C6 C11 1.387(6) . ?
C6 C7 1.393(6) . ?
C7 C8 1.383(6) . ?
C8 C9 1.372(7) . ?
C9 C10 1.382(7) . ?
C10 C11 1.373(7) . ?
Cu1 N1 1.891(4) . ?
Cu1 N1 1.891(4) 2_656 ?
Cu1 S1 2.1655(15) . ?
Cu1 S1 2.1655(15) 2_656 ?
N1 N2 1.380(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C2 128.9(6) 2_656 . ?
N1 C2 C1 122.0(5) . . ?
N1 C2 C3 119.5(4) . . ?
C1 C2 C3 118.5(4) . . ?
N2 C4 S1 124.5(4) . . ?
N2 C4 S2 121.8(4) . . ?
S1 C4 S2 113.7(3) . . ?
C6 C5 S2 113.7(3) . . ?
C11 C6 C7 118.4(4) . . ?
C11 C6 C5 120.9(4) . . ?
C7 C6 C5 120.7(4) . . ?
C8 C7 C6 120.6(4) . . ?
C9 C8 C7 119.9(4) . . ?
C8 C9 C10 120.1(5) . . ?
C11 C10 C9 120.1(5) . . ?
C10 C11 C6 120.8(4) . . ?
N1 Cu1 N1 97.1(2) . 2_656 ?
N1 Cu1 S1 87.97(12) . . ?
N1 Cu1 S1 172.76(14) 2_656 . ?
N1 Cu1 S1 172.76(14) . 2_656 ?
N1 Cu1 S1 87.97(12) 2_656 2_656 ?
S1 Cu1 S1 87.43(8) . 2_656 ?
C2 N1 N2 115.2(4) . . ?
C2 N1 Cu1 124.9(3) . . ?
N2 N1 Cu1 119.9(3) . . ?
C4 N2 N1 113.2(4) . . ?
C4 S1 Cu1 94.19(17) . . ?
C4 S2 C5 103.4(2) . . ?



# END of CIF
####################################################################### 
# 
# 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_PB1_Pnma
_database_code_depnum_ccdc_archive 'CCDC 2204794'
loop_
_audit_author_name
_audit_author_address
'Paul Bernhardt'
;The University of Queensland
Australia
;
_audit_update_record             
;
2022-09-01 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;

_audit_creation_date             2022-08-05T10:35:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_formula_sum            'C9 H14 Cu N4 S4'
_chemical_formula_weight         370.02

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_Int_Tables_number      62
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   46.877(9)
_cell_length_b                   6.9630(14)
_cell_length_c                   8.8140(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2876.9(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6678
_cell_measurement_theta_min      3.85
_cell_measurement_theta_max      30.27
_cell_measurement_wavelength     0.7108


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

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512

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

_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_diffrn_source                   Synchrotron
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_T_max  1

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

_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7108
_diffrn_radiation_type           synchrotron
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.02
_diffrn_orient_matrix_ub_11      -0.016045
_diffrn_orient_matrix_ub_12      -0.045568
_diffrn_orient_matrix_ub_13      0.037321
_diffrn_orient_matrix_ub_21      0.098656
_diffrn_orient_matrix_ub_22      -0.017447
_diffrn_orient_matrix_ub_23      -0.007141
_diffrn_orient_matrix_ub_31      0.028609
_diffrn_orient_matrix_ub_32      0.034575
_diffrn_orient_matrix_ub_33      0.04552
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Dectris Eiger 9M'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_number            35983
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         0.869
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.244
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.939
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.939
_reflns_Friedel_coverage         0
_reflns_number_total             3366
_reflns_number_gt                2636
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom

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

_shelx_SHELXL_version_number     2018/1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0601P)²+2.4243P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3366
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.087

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   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 0 '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'
Cu Cu 0.3201 1.2651 '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
C1A C 0.09469(10) 0.25 0.3935(5) 0.0402(11) Uani 1 2 d S T P . .
H1A1 H 0.09578 0.363792 0.326377 0.048 Uiso 0.5 1 calc R U P . .
H1A2 H 0.09578 0.136208 0.326377 0.048 Uiso 0.5 1 calc R U P . .
C2A C 0.12180(10) 0.25 0.4852(5) 0.0373(10) Uani 1 2 d S T P . .
C3A C 0.14880(10) 0.25 0.3933(6) 0.0437(12) Uani 1 2 d S T P . .
H3A1 H 0.144039 0.25 0.285029 0.066 Uiso 1 2 calc R U P . .
H3A2 H 0.15998 0.364917 0.417456 0.066 Uiso 0.5 1 calc R U P . .
H3A3 H 0.15998 0.135083 0.417456 0.066 Uiso 0.5 1 calc R U P . .
C4A C 0.14981(10) 0.25 0.8387(5) 0.0373(10) Uani 1 2 d S T P . .
C5A C 0.06536(10) 0.25 0.4584(5) 0.0391(11) Uani 1 2 d S T P . .
C6A C 0.04190(11) 0.25 0.3431(5) 0.0484(13) Uani 1 2 d S T P . .
H6A1 H 0.050151 0.25 0.24097 0.073 Uiso 1 2 calc R U P . .
H6A2 H 0.03009 0.135083 0.356471 0.073 Uiso 0.5 1 calc R U P . .
H6A3 H 0.03009 0.364917 0.356471 0.073 Uiso 0.5 1 calc R U P . .
C7A C 0.02597(10) 0.25 0.7834(5) 0.0338(10) Uani 1 2 d S T P . .
C8A C 0.20721(11) 0.25 0.7731(6) 0.0485(13) Uani 1 2 d S T P . .
H8A1 H 0.226864 0.25 0.810975 0.073 Uiso 1 2 calc R U P . .
H8A2 H 0.204011 0.135083 0.711211 0.073 Uiso 0.5 1 calc R U P . .
H8A3 H 0.204012 0.364917 0.711211 0.073 Uiso 0.5 1 calc R U P . .
C9A C -0.01134(11) 0.25 1.0326(5) 0.0444(12) Uani 1 2 d S T P . .
H9A1 H -0.031192 0.25 1.067488 0.067 Uiso 1 2 calc R U P . .
H9A2 H -0.001633 0.135083 1.070745 0.067 Uiso 0.5 1 calc R U P . .
H9A3 H -0.001633 0.364917 1.070745 0.067 Uiso 0.5 1 calc R U P . .
N1A N 0.12177(8) 0.25 0.6309(4) 0.0384(9) Uani 1 2 d S T P . .
N2A N 0.14938(8) 0.25 0.6932(4) 0.0388(9) Uani 1 2 d S T P . .
N3A N 0.06023(8) 0.25 0.6014(4) 0.0336(8) Uani 1 2 d S T P . .
N4A N 0.03086(8) 0.25 0.6390(4) 0.0386(9) Uani 1 2 d S T P . .
Cu1A Cu 0.08867(2) 0.25 0.76692(6) 0.03496(17) Uani 1 2 d S T P . .
S1A S 0.12016(3) 0.25 0.95959(13) 0.0424(3) Uani 1 2 d S T P . .
S2A S 0.18258(3) 0.25 0.93269(14) 0.0424(3) Uani 1 2 d S T P . .
S3A S 0.05141(3) 0.25 0.92654(13) 0.0453(3) Uani 1 2 d S T P . .
S4A S -0.01054(3) 0.25 0.82774(14) 0.0391(3) Uani 1 2 d S T P . .
C1B C -0.14420(10) 0.25 -0.0373(5) 0.0405(11) Uani 1 2 d S T P . .
H1B1 H -0.141907 0.13632 -0.103608 0.049 Uiso 0.5 1 calc R U P . .
H1B2 H -0.141907 0.36368 -0.103608 0.049 Uiso 0.5 1 calc R U P . .
C2B C -0.11929(11) 0.25 0.0637(5) 0.0392(11) Uani 1 2 d S T P . .
C3B C -0.09073(11) 0.25 -0.0137(6) 0.0446(12) Uani 1 2 d S T P . .
H3B1 H -0.093465 0.25 -0.123905 0.067 Uiso 1 2 calc R U P . .
H3B2 H -0.080044 0.364917 0.016203 0.067 Uiso 0.5 1 calc R U P . .
H3B3 H -0.080044 0.135083 0.016203 0.067 Uiso 0.5 1 calc R U P . .
C4B C -0.09749(10) 0.25 0.4341(5) 0.0343(10) Uani 1 2 d S T P . .
C5B C -0.17458(11) 0.25 0.0105(5) 0.0382(11) Uani 1 2 d S T P . .
C6B C -0.19599(12) 0.25 -0.1151(5) 0.0488(13) Uani 1 2 d S T P . .
H6B1 H -0.186062 0.25 -0.212927 0.073 Uiso 1 2 calc R U P . .
H6B2 H -0.207967 0.135083 -0.107319 0.073 Uiso 0.5 1 calc R U P . .
H6B3 H -0.207967 0.364917 -0.107319 0.073 Uiso 0.5 1 calc R U P . .
C7B C -0.21959(10) 0.25 0.3113(5) 0.0380(11) Uani 1 2 d S T P . .
C8B C -0.03815(10) 0.25 0.4151(5) 0.0430(11) Uani 1 2 d S T P . .
H8B1 H -0.019956 0.25 0.469834 0.065 Uiso 1 2 calc R U P . .
H8B2 H -0.039359 0.135083 0.351188 0.065 Uiso 0.5 1 calc R U P . .
H8B3 H -0.039359 0.364917 0.351189 0.065 Uiso 0.5 1 calc R U P . .
C9B C -0.27167(12) 0.25 0.1681(7) 0.0638(17) Uani 1 2 d S T P . .
H9B1 H -0.292508 0.25 0.177304 0.096 Uiso 1 2 calc R U P . .
H9B2 H -0.265546 0.364917 0.112786 0.096 Uiso 0.5 1 calc R U P . .
H9B3 H -0.265546 0.135083 0.112786 0.096 Uiso 0.5 1 calc R U P . .
N1B N -0.12135(8) 0.25 0.2115(4) 0.0366(9) Uani 1 2 d S T P . .
N2B N -0.09480(8) 0.25 0.2875(4) 0.0401(10) Uani 1 2 d S T P . .
N3B N -0.18200(9) 0.25 0.1518(4) 0.0385(9) Uani 1 2 d S T P . .
N4B N -0.21181(8) 0.25 0.1720(5) 0.0389(9) Uani 1 2 d S T P . .
Cu1B Cu -0.15701(2) 0.25 0.33047(6) 0.03462(17) Uani 1 2 d S T P . .
S1B S -0.12887(3) 0.25 0.53686(13) 0.0388(3) Uani 1 2 d S T P . .
S2B S -0.06690(3) 0.25 0.54804(13) 0.0398(3) Uani 1 2 d S T P . .
S3B S -0.19727(3) 0.25 0.46919(13) 0.0453(3) Uani 1 2 d S T P . .
S4B S -0.25590(3) 0.25 0.35454(16) 0.0510(4) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   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
C1A C5A 1.489(7) . ?
C1A C2A 1.506(7) . ?
C2A N1A 1.284(6) . ?
C2A C3A 1.503(6) . ?
C4A N2A 1.283(6) . ?
C4A S2A 1.745(5) . ?
C4A S1A 1.751(5) . ?
C5A N3A 1.283(6) . ?
C5A C6A 1.498(6) . ?
C7A N4A 1.293(6) . ?
C7A S3A 1.736(5) . ?
C7A S4A 1.756(5) . ?
C8A S2A 1.820(5) . ?
C9A S4A 1.806(5) . ?
N1A N2A 1.406(5) . ?
N1A Cu1A 1.961(4) . ?
N3A N4A 1.416(5) . ?
N3A Cu1A 1.976(4) . ?
Cu1A S3A 2.2427(14) . ?
Cu1A S1A 2.2503(13) . ?
C1B C2B 1.468(7) . ?
C1B C5B 1.485(7) . ?
C2B N1B 1.306(6) . ?
C2B C3B 1.502(6) . ?
C4B N2B 1.299(6) . ?
C4B S1B 1.727(5) . ?
C4B S2B 1.750(4) . ?
C5B N3B 1.293(6) . ?
C5B C6B 1.494(7) . ?
C7B N4B 1.281(6) . ?
C7B S3B 1.741(5) . ?
C7B S4B 1.744(5) . ?
C8B S2B 1.786(5) . ?
C9B S4B 1.802(6) . ?
N1B N2B 1.414(5) . ?
N1B Cu1B 1.973(4) . ?
N3B N4B 1.409(6) . ?
N3B Cu1B 1.963(4) . ?
Cu1B S1B 2.2471(13) . ?
Cu1B S3B 2.2487(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
C5A C1A C2A 124.9(4) . . ?
N1A C2A C3A 122.7(5) . . ?
N1A C2A C1A 122.4(4) . . ?
C3A C2A C1A 114.9(4) . . ?
N2A C4A S2A 119.2(4) . . ?
N2A C4A S1A 126.6(4) . . ?
S2A C4A S1A 114.2(3) . . ?
N3A C5A C1A 123.4(4) . . ?
N3A C5A C6A 121.9(4) . . ?
C1A C5A C6A 114.7(4) . . ?
N4A C7A S3A 126.4(4) . . ?
N4A C7A S4A 113.1(3) . . ?
S3A C7A S4A 120.5(3) . . ?
C2A N1A N2A 112.9(4) . . ?
C2A N1A Cu1A 127.8(3) . . ?
N2A N1A Cu1A 119.3(3) . . ?
C4A N2A N1A 113.9(4) . . ?
C5A N3A N4A 114.3(4) . . ?
C5A N3A Cu1A 126.8(3) . . ?
N4A N3A Cu1A 118.9(3) . . ?
C7A N4A N3A 113.7(4) . . ?
N1A Cu1A N3A 94.73(16) . . ?
N1A Cu1A S3A 178.84(12) . . ?
N3A Cu1A S3A 86.43(11) . . ?
N1A Cu1A S1A 86.69(12) . . ?
N3A Cu1A S1A 178.59(11) . . ?
S3A Cu1A S1A 92.15(5) . . ?
C4A S1A Cu1A 93.53(16) . . ?
C4A S2A C8A 101.1(2) . . ?
C7A S3A Cu1A 94.54(16) . . ?
C7A S4A C9A 104.0(2) . . ?
C2B C1B C5B 126.2(4) . . ?
N1B C2B C1B 123.0(4) . . ?
N1B C2B C3B 121.3(4) . . ?
C1B C2B C3B 115.7(4) . . ?
N2B C4B S1B 127.2(4) . . ?
N2B C4B S2B 119.4(3) . . ?
S1B C4B S2B 113.4(2) . . ?
N3B C5B C1B 122.1(4) . . ?
N3B C5B C6B 122.2(5) . . ?
C1B C5B C6B 115.7(4) . . ?
N4B C7B S3B 126.5(4) . . ?
N4B C7B S4B 119.2(4) . . ?
S3B C7B S4B 114.3(3) . . ?
C2B N1B N2B 114.0(4) . . ?
C2B N1B Cu1B 126.4(3) . . ?
N2B N1B Cu1B 119.6(3) . . ?
C4B N2B N1B 112.7(4) . . ?
C5B N3B N4B 112.9(4) . . ?
C5B N3B Cu1B 127.8(4) . . ?
N4B N3B Cu1B 119.4(3) . . ?
C7B N4B N3B 113.8(4) . . ?
N3B Cu1B N1B 94.54(16) . . ?
N3B Cu1B S1B 179.31(12) . . ?
N1B Cu1B S1B 86.15(11) . . ?
N3B Cu1B S3B 86.30(12) . . ?
N1B Cu1B S3B 179.17(11) . . ?
S1B Cu1B S3B 93.01(5) . . ?
C4B S1B Cu1B 94.34(15) . . ?
C4B S2B C8B 104.0(2) . . ?
C7B S3B Cu1B 94.00(17) . . ?
C7B S4B C9B 101.6(3) . . ?



# END of CIF
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
