# Electronic Supplementary Material (ESI) for RSC Advances.
# 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 2132932'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;University of Sfax
Tunisia
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pd, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Br4 N2 Pd'
_chemical_formula_weight         518.23

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'
Pd Pd -0.9988 1.0072 '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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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                   18.182(2)
_cell_length_b                   7.2741(7)
_cell_length_c                   9.8478(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.340(4)
_cell_angle_gamma                90
_cell_volume                     1302.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3364
_cell_measurement_theta_min      3.6428
_cell_measurement_theta_max      27.5025

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.644
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    13.657
_shelx_estimated_absorpt_T_min   0.081
_shelx_estimated_absorpt_T_max   0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            1503
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1503
_reflns_number_gt                1360
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+104.1012P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         1503
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1377
_refine_ls_wR_factor_gt          0.1287
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5782(7) 0.2497(18) 0.6433(10) 0.029(2) Uani 1 1 d . . . . .
H1A H 0.605638 0.217300 0.726717 0.043 Uiso 1 1 calc R U . . .
H1B H 0.558278 0.374305 0.651751 0.043 Uiso 1 1 calc R U . . .
H1C H 0.537642 0.162523 0.628807 0.043 Uiso 1 1 calc R U . . .
N2 N 0.6274(5) 0.2422(14) 0.5277(9) 0.0244(19) Uani 1 1 d . . . . .
H2A H 0.646529 0.126892 0.522337 0.029 Uiso 1 1 calc R U . . .
H2B H 0.665468 0.321251 0.543394 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5919(7) 0.2887(17) 0.3957(11) 0.031(3) Uani 1 1 d . . . . .
H3A H 0.628205 0.280626 0.323946 0.046 Uiso 1 1 calc R U . . .
H3B H 0.551676 0.202277 0.376380 0.046 Uiso 1 1 calc R U . . .
H3C H 0.572312 0.414058 0.399325 0.046 Uiso 1 1 calc R U . . .
Pd1 Pd 0.750000 0.750000 0.500000 0.0135(3) Uani 1 2 d S . P . .
Br1 Br 0.61652(5) 0.77330(15) 0.52367(10) 0.0199(3) Uani 1 1 d . . . . .
Br2 Br 0.75488(5) 0.51209(14) 0.67475(9) 0.0185(3) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.029(6) 0.041(7) 0.016(5) -0.002(4) 0.007(4) 0.006(5)
N2 0.023(5) 0.030(5) 0.020(4) -0.006(4) 0.001(4) -0.002(4)
C3 0.039(7) 0.032(6) 0.021(5) 0.004(5) 0.007(5) -0.004(5)
Pd1 0.0166(5) 0.0132(5) 0.0106(4) 0.0004(3) 0.0000(3) -0.0005(4)
Br1 0.0166(5) 0.0253(5) 0.0178(5) 0.0036(4) 0.0007(3) -0.0005(4)
Br2 0.0227(5) 0.0166(5) 0.0160(4) 0.0047(3) 0.0002(3) -0.0007(4)

_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 1.466(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N2 C3 1.476(14) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
Pd1 Br2 2.4407(9) . ?
Pd1 Br2 2.4407(9) 7_666 ?
Pd1 Br1 2.4493(10) 7_666 ?
Pd1 Br1 2.4494(10) . ?

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 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 N2 C3 114.4(9) . . ?
C1 N2 H2A 108.7 . . ?
C3 N2 H2A 108.7 . . ?
C1 N2 H2B 108.7 . . ?
C3 N2 H2B 108.7 . . ?
H2A N2 H2B 107.6 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Br2 Pd1 Br2 180.0 . 7_666 ?
Br2 Pd1 Br1 89.90(3) . 7_666 ?
Br2 Pd1 Br1 90.10(3) 7_666 7_666 ?
Br2 Pd1 Br1 90.10(3) . . ?
Br2 Pd1 Br1 89.90(3) 7_666 . ?
Br1 Pd1 Br1 180.0 7_666 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A Br1 0.98 2.93 3.798(11) 148.5 6_566
C1 H1A Br2 0.98 3.08 3.893(12) 141.3 4_646
N2 H2A Br1 0.91 2.63 3.417(10) 145.3 1_545
N2 H2A Br2 0.91 2.86 3.489(9) 127.7 7_656
N2 H2B Br2 0.91 2.48 3.341(9) 158.3 .
C3 H3A Br1 0.98 2.99 3.729(11) 133.5 6_565
C3 H3A Br2 0.98 3.01 3.622(13) 121.8 7_656
C3 H3A Br2 0.98 3.15 3.989(12) 145.2 6_565
C3 H3C Br1 0.98 2.99 3.767(13) 137.2 .

_refine_diff_density_max         1.871
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.364

_shelx_res_file                  
;
TITL job [Space group= C2/c]
    shelx.res
    created by SHELXL-2016/6 at 15:11:29 on 06-Jan-2022
CELL  0.71073  18.1816   7.2741   9.8478   90.000   91.340   90.000
ZERR     4.00   0.0020   0.0007   0.0010    0.000    0.004    0.000
LATT   7
SYMM  - X,   Y, 1/2 - Z
SFAC  C    H    N    PD   BR
UNIT  16   64   8    4    16
MERG   2
FMAP   2
PLAN   20
SIZE     0.04   0.12   0.37
ACTA
BOND   $H
HTAB
EQIV $2 x, -y+1, z+1/2
HTAB C1 Br1_$2
EQIV $3 -x+3/2, y-1/2, -z+3/2
HTAB C1 Br2_$3
EQIV $4 x, y-1, z
HTAB N2 Br1_$4
EQIV $5 -x+3/2, -y+1/2, -z+1
HTAB N2 Br2_$5
HTAB N2 Br2
EQIV $6 x, -y+1, z-1/2
HTAB C3 Br1_$6
HTAB C3 Br2_$5
HTAB C3 Br2_$6
HTAB C3 Br1
CONF
LIST   4
WPDB  -2
L.S.   14
TEMP  -123.00
WGHT    0.035200  104.101196
FVAR       0.19626
mole 1
C1    1    0.578160    0.249707    0.643325    11.00000    0.02934    0.04130 =
         0.01563   -0.00246    0.00658    0.00592
AFIX  33
H1A   2    0.605638    0.217300    0.726717    11.00000   -1.50000
H1B   2    0.558278    0.374305    0.651751    11.00000   -1.50000
H1C   2    0.537642    0.162523    0.628807    11.00000   -1.50000
AFIX   0
N2    3    0.627417    0.242218    0.527667    11.00000    0.02292    0.02994 =
         0.02028   -0.00626    0.00090   -0.00241
AFIX  23
H2A   2    0.646529    0.126892    0.522337    11.00000   -1.20000
H2B   2    0.665468    0.321251    0.543394    11.00000   -1.20000
AFIX   0
C3    1    0.591919    0.288702    0.395742    11.00000    0.03929    0.03171 =
         0.02089    0.00362    0.00729   -0.00407
AFIX  33
H3A   2    0.628205    0.280626    0.323946    11.00000   -1.50000
H3B   2    0.551676    0.202277    0.376380    11.00000   -1.50000
H3C   2    0.572312    0.414058    0.399325    11.00000   -1.50000
AFIX   0
mole 2
PD1   4    0.750000    0.750000    0.500000    10.50000    0.01659    0.01323 =
         0.01057    0.00042    0.00000   -0.00045
BR1   5    0.616519    0.773300    0.523672    11.00000    0.01656    0.02528 =
         0.01779    0.00358    0.00066   -0.00054
BR2   5    0.754878    0.512095    0.674754    11.00000    0.02274    0.01661 =
         0.01601    0.00466    0.00017   -0.00068
HKLF    4




REM  job [Space group= C2/c]
REM R1 =  0.0535 for    1360 Fo > 4sig(Fo)  and  0.0646 for all    1503 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.0299     96.6595

REM Instructions for potential hydrogen bonds
HTAB C1 Br1_$2
HTAB C1 Br2_$3
HTAB N2 Br1_$4
HTAB N2 Br2_$5
HTAB N2 Br2
HTAB C3 Br1_$6
HTAB C3 Br2_$5
HTAB C3 Br1

REM Highest difference peak  1.871,  deepest hole -1.497,  1-sigma level  0.364
Q1    1   0.7072  0.7624  0.5618  11.00000  0.05    1.87
Q2    1   0.6617  0.7771  0.4177  11.00000  0.05    1.60
Q3    1   0.7083  0.5010  0.7074  11.00000  0.05    1.34
Q4    1   0.6760  0.6619  0.5739  11.00000  0.05    1.25
Q5    1   0.7010  0.6470  0.4594  11.00000  0.05    1.17
Q6    1   0.6774  0.8705  0.5527  11.00000  0.05    1.13
Q7    1   0.6086  0.0060  0.7797  11.00000  0.05    1.13
Q8    1   0.6602  0.0539  0.7534  11.00000  0.05    1.06
Q9    1   0.6533  0.5298  0.5403  11.00000  0.05    1.03
Q10   1   0.5653  0.7252  0.5764  11.00000  0.05    1.03
Q11   1   0.5625  0.7752  0.4706  11.00000  0.05    0.99
Q12   1   0.6786  0.1018  0.6119  11.00000  0.05    0.98
Q13   1   0.8019  0.6657  0.5612  11.00000  0.05    0.95
Q14   1   0.8005  0.5656  0.6512  11.00000  0.05    0.94
Q15   1   0.4873  0.1728  0.6787  11.00000  0.05    0.93
Q16   1   0.6628  0.0995  0.2129  11.00000  0.05    0.91
Q17   1   0.6387  0.3450  0.3791  11.00000  0.05    0.91
Q18   1   0.7986  0.6212  0.7038  11.00000  0.05    0.90
Q19   1   0.6564 -0.0075  0.5535  11.00000  0.05    0.90
Q20   1   0.4842  0.3179  0.6816  11.00000  0.05    0.89
;
_shelx_res_checksum              69876
