# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2223894'
loop_
_audit_author_name
_audit_author_address
'Horacio Sandoval'
;
Mexico
;
_audit_update_record             
;
2022-12-01 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;

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

_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_chemical_formula_sum            'C16 H26 Br Cu N6 O8 S2'
_chemical_formula_weight         638

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   14.7154(18)
_cell_length_b                   12.7433(12)
_cell_length_c                   12.6692(15)
_cell_angle_alpha                90
_cell_angle_beta                 99.767(11)
_cell_angle_gamma                90
_cell_volume                     2341.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1656
_cell_measurement_theta_min      3.752
_cell_measurement_theta_max      28.822

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

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.81
_exptl_crystal_F_000             1296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
20 1 2 0.0366
-20 -1 -2 0.0366
-4 16 7 0.2418
4 -16 -7 0.2418
-1 10 15 0.2065
1 -10 -15 0.2065
5 16 -8 0.1929
-5 -16 8 0.1929


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

_exptl_absorpt_coefficient_mu    2.874
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
     model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_T_max  0.794
_shelx_estimated_absorpt_T_min   0.339
_shelx_estimated_absorpt_T_max   0.824

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

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.4685
_diffrn_orient_matrix_ub_11      0.0022327
_diffrn_orient_matrix_ub_12      0.0218265
_diffrn_orient_matrix_ub_13      -0.0508688
_diffrn_orient_matrix_ub_21      -0.0480525
_diffrn_orient_matrix_ub_22      0.0107043
_diffrn_orient_matrix_ub_23      -0.0075094
_diffrn_orient_matrix_ub_31      0.0093542
_diffrn_orient_matrix_ub_32      0.0500768
_diffrn_orient_matrix_ub_33      0.0238962
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_number            5110
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.691
_diffrn_reflns_theta_max         29.379
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.847
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.847
_reflns_Friedel_coverage         0
_reflns_number_total             2732
_reflns_number_gt                2211
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'

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

_atom_sites_solution_hydrogens   geom

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2732
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.126

#----------------------------------------------------------------------------#
#                   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'
O O 0.0106 0.006 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Br1 Br 0.75 0.67653(3) 0.5 0.02305(15) Uani 1 2 d S T P . .
Cu1 Cu 0.75 0.48301(4) 0.5 0.01533(15) Uani 1 2 d S T P . .
S8 S 0.45094(5) 0.13902(6) 0.40884(5) 0.01370(18) Uani 1 1 d . . . . .
O3 O 0.48571(15) 0.21025(17) 0.49458(15) 0.0191(5) Uani 1 1 d . . . . .
O4 O 0.51685(15) 0.06848(16) 0.37375(16) 0.0196(5) Uani 1 1 d . . . . .
O1 O 0.37425(17) 0.57592(17) 0.33134(18) 0.0240(5) Uani 1 1 d . . . . .
N1 N 0.63232(18) 0.44310(19) 0.41474(19) 0.0141(5) Uani 1 1 d . . . . .
O2 O 0.34264(17) 0.43541(18) 0.23411(19) 0.0272(6) Uani 1 1 d . . . . .
N3 N 0.51973(17) 0.35673(19) 0.31090(18) 0.0129(5) Uani 1 1 d . . . . .
N4 N 0.39512(19) 0.4900(2) 0.2976(2) 0.0193(6) Uani 1 1 d . . . . .
C5 C 0.5555(2) 0.5053(2) 0.3992(2) 0.0141(6) Uani 1 1 d . . . . .
H5 H 0.55141 0.573749 0.427675 0.017 Uiso 1 1 calc R U . . .
C2 C 0.6089(2) 0.3538(2) 0.3613(2) 0.0137(6) Uani 1 1 d . . . . .
C4 C 0.4859(2) 0.4533(2) 0.3364(2) 0.0141(6) Uani 1 1 d . . . . .
C7 C 0.3991(2) 0.2148(2) 0.2966(2) 0.0147(6) Uani 1 1 d . . . . .
H7A H 0.362056 0.168137 0.243379 0.018 Uiso 1 1 calc R U . . .
H7B H 0.356892 0.267042 0.320113 0.018 Uiso 1 1 calc R U . . .
C9 C 0.3583(2) 0.0657(2) 0.4438(2) 0.0169(7) Uani 1 1 d . . . . .
H9A H 0.372673 0.047708 0.520858 0.02 Uiso 1 1 calc R U . . .
H9B H 0.302136 0.109784 0.432675 0.02 Uiso 1 1 calc R U . . .
C6 C 0.4709(2) 0.2712(2) 0.2444(2) 0.0155(6) Uani 1 1 d . . . . .
H6A H 0.516977 0.219368 0.228751 0.019 Uiso 1 1 calc R U . . .
H6B H 0.440398 0.301134 0.175328 0.019 Uiso 1 1 calc R U . . .
C11 C 0.6727(2) 0.2645(2) 0.3583(3) 0.0198(7) Uani 1 1 d . . . . .
H11A H 0.735923 0.286971 0.386187 0.03 Uiso 1 1 calc R U . . .
H11B H 0.668977 0.240332 0.28421 0.03 Uiso 1 1 calc R U . . .
H11C H 0.655532 0.207055 0.402386 0.03 Uiso 1 1 calc R U . . .
C10 C 0.3387(2) -0.0352(3) 0.3790(3) 0.0222(7) Uani 1 1 d . . . . .
H10A H 0.326044 -0.018246 0.302506 0.033 Uiso 1 1 calc R U . . .
H10B H 0.285077 -0.070504 0.399286 0.033 Uiso 1 1 calc R U . . .
H10C H 0.392495 -0.081605 0.393757 0.033 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
Br1 Cu1 2.4661(7) . ?
Cu1 N1 1.947(3) . ?
Cu1 N1 1.947(3) 2_656 ?
S8 O3 1.441(2) . ?
S8 O4 1.447(2) . ?
S8 C9 1.770(3) . ?
S8 C7 1.780(3) . ?
O1 N4 1.233(3) . ?
N1 C2 1.339(4) . ?
N1 C5 1.368(4) . ?
O2 N4 1.231(3) . ?
N3 C2 1.359(4) . ?
N3 C4 1.386(4) . ?
N3 C6 1.486(4) . ?
N4 C4 1.422(4) . ?
C5 C4 1.358(4) . ?
C5 H5 0.95 . ?
C2 C11 1.481(4) . ?
C7 C6 1.520(4) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C9 C10 1.526(4) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 149.71(15) . 2_656 ?
N1 Cu1 Br1 105.14(7) . . ?
N1 Cu1 Br1 105.14(7) 2_656 . ?
O3 S8 O4 116.89(13) . . ?
O3 S8 C9 109.51(14) . . ?
O4 S8 C9 109.49(14) . . ?
O3 S8 C7 108.05(14) . . ?
O4 S8 C7 108.10(13) . . ?
C9 S8 C7 104.02(15) . . ?
C2 N1 C5 106.5(3) . . ?
C2 N1 Cu1 129.1(2) . . ?
C5 N1 Cu1 124.4(2) . . ?
C2 N3 C4 105.7(2) . . ?
C2 N3 C6 125.6(2) . . ?
C4 N3 C6 128.7(3) . . ?
O2 N4 O1 124.2(3) . . ?
O2 N4 C4 119.3(3) . . ?
O1 N4 C4 116.5(3) . . ?
C4 C5 N1 109.0(3) . . ?
C4 C5 H5 125.5 . . ?
N1 C5 H5 125.5 . . ?
N1 C2 N3 111.1(3) . . ?
N1 C2 C11 123.8(3) . . ?
N3 C2 C11 125.1(3) . . ?
C5 C4 N3 107.7(3) . . ?
C5 C4 N4 127.8(3) . . ?
N3 C4 N4 124.4(3) . . ?
C6 C7 S8 111.6(2) . . ?
C6 C7 H7A 109.3 . . ?
S8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
S8 C7 H7B 109.3 . . ?
H7A C7 H7B 108 . . ?
C10 C9 S8 113.2(2) . . ?
C10 C9 H9A 108.9 . . ?
S8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
S8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
N3 C6 C7 113.9(2) . . ?
N3 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
N3 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C2 C11 H11A 109.5 . . ?
C2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
C2 N1 C5 C4 0.0(3) . . . . ?
Cu1 N1 C5 C4 -179.7(2) . . . . ?
C5 N1 C2 N3 0.6(3) . . . . ?
Cu1 N1 C2 N3 -179.68(18) . . . . ?
C5 N1 C2 C11 -179.5(3) . . . . ?
Cu1 N1 C2 C11 0.3(4) . . . . ?
C4 N3 C2 N1 -0.9(3) . . . . ?
C6 N3 C2 N1 180.0(2) . . . . ?
C4 N3 C2 C11 179.1(3) . . . . ?
C6 N3 C2 C11 0.0(4) . . . . ?
N1 C5 C4 N3 -0.6(3) . . . . ?
N1 C5 C4 N4 -177.8(3) . . . . ?
C2 N3 C4 C5 0.9(3) . . . . ?
C6 N3 C4 C5 179.9(3) . . . . ?
C2 N3 C4 N4 178.2(3) . . . . ?
C6 N3 C4 N4 -2.8(4) . . . . ?
O2 N4 C4 C5 174.1(3) . . . . ?
O1 N4 C4 C5 -6.2(4) . . . . ?
O2 N4 C4 N3 -2.6(4) . . . . ?
O1 N4 C4 N3 177.0(3) . . . . ?
O3 S8 C7 C6 72.3(2) . . . . ?
O4 S8 C7 C6 -55.0(2) . . . . ?
C9 S8 C7 C6 -171.4(2) . . . . ?
O3 S8 C9 C10 -160.1(2) . . . . ?
O4 S8 C9 C10 -30.8(3) . . . . ?
C7 S8 C9 C10 84.6(2) . . . . ?
C2 N3 C6 C7 108.4(3) . . . . ?
C4 N3 C6 C7 -70.4(4) . . . . ?
S8 C7 C6 N3 -69.0(3) . . . . ?



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