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

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

data_Shehata
_audit_block_doi                 10.5517/ccdc.csd.cc27sbp2
_database_code_depnum_ccdc_archive 'CCDC 2078974'
loop_
_audit_author_name
_audit_author_address
'ElSayed Shalaby'
;National Research Centre in Egypt
Egypt
;
_audit_update_record             
;
2021-04-20 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H24 N4 Pd, Cl4 Pd'
_chemical_formula_sum            'C10 H24 Cl4 N4 Pd2'
_chemical_formula_weight         554.93

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.5750(2)
_cell_length_b                   9.0820(4)
_cell_length_c                   12.9300(4)
_cell_angle_alpha                76.030(2)
_cell_angle_beta                 83.160(2)
_cell_angle_gamma                69.500(2)
_cell_volume                     914.64(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    571(2)
_cell_measurement_reflns_used    5066
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.545
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_diffrn_ambient_temperature      571(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker AXS, KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            8524
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.961
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        25.241
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4148
_reflns_number_gt                3046
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'CrystaMaker X (CrystalMaker Software ltd., 2020)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0215P)²] 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         4148
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_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
Pd1 Pd 0.500000 0.500000 0.000000 0.02967(12) Uani 1 2 d S . P . .
Cl22 Cl 0.74369(13) 0.28249(14) 0.00575(8) 0.0442(3) Uani 1 1 d . . . . .
Cl23 Cl 0.62123(13) 0.61207(14) 0.09547(8) 0.0422(3) Uani 1 1 d . . . . .
Pd2 Pd 0.33333(3) 0.29662(4) 0.25570(2) 0.02879(10) Uani 1 1 d . . . . .
N8 N 0.1086(4) 0.4444(4) 0.3029(2) 0.0347(8) Uani 1 1 d . . . . .
N9 N 0.1531(4) 0.2363(4) 0.2014(2) 0.0330(8) Uani 1 1 d . . . . .
N13 N 0.4858(4) 0.3948(5) 0.3056(2) 0.0435(9) Uani 1 1 d . . . . .
H13A H 0.559641 0.315647 0.348064 0.052 Uiso 1 1 calc R U . . .
H13B H 0.542511 0.429642 0.248445 0.052 Uiso 1 1 calc R U . . .
N14 N 0.5411(4) 0.1240(4) 0.2092(2) 0.0422(9) Uani 1 1 d . . . . .
H14A H 0.608960 0.173781 0.171453 0.051 Uiso 1 1 calc R U . . .
H14B H 0.593502 0.061607 0.267815 0.051 Uiso 1 1 calc R U . . .
C10 C 0.1056(6) 0.5631(6) 0.3641(3) 0.0501(12) Uani 1 1 d . . . . .
H10A H 0.119566 0.510509 0.438883 0.060 Uiso 1 1 calc R U . . .
H10B H -0.002339 0.647308 0.357863 0.060 Uiso 1 1 calc R U . . .
C11 C 0.2391(7) 0.6379(6) 0.3271(3) 0.0588(14) Uani 1 1 d . . . . .
H11A H 0.210819 0.735240 0.354052 0.071 Uiso 1 1 calc R U . . .
H11B H 0.241222 0.668343 0.249841 0.071 Uiso 1 1 calc R U . . .
C12 C 0.4111(6) 0.5285(6) 0.3625(3) 0.0575(14) Uani 1 1 d . . . . .
H12A H 0.484042 0.592272 0.351685 0.069 Uiso 1 1 calc R U . . .
H12B H 0.404700 0.483321 0.438354 0.069 Uiso 1 1 calc R U . . .
C15 C 0.2031(6) 0.1070(6) 0.1406(3) 0.0519(12) Uani 1 1 d . . . . .
H15A H 0.217319 0.152991 0.065684 0.062 Uiso 1 1 calc R U . . .
H15B H 0.114739 0.061200 0.147715 0.062 Uiso 1 1 calc R U . . .
C16 C 0.3629(6) -0.0253(6) 0.1784(4) 0.0540(13) Uani 1 1 d . . . . .
H16A H 0.355498 -0.056307 0.255550 0.065 Uiso 1 1 calc R U . . .
H16B H 0.372920 -0.118337 0.150436 0.065 Uiso 1 1 calc R U . . .
C17 C 0.5179(6) 0.0184(6) 0.1463(3) 0.0546(13) Uani 1 1 d . . . . .
H17A H 0.613699 -0.079544 0.154234 0.066 Uiso 1 1 calc R U . . .
H17B H 0.513449 0.071921 0.071578 0.066 Uiso 1 1 calc R U . . .
C18 C 0.0280(5) 0.3253(6) 0.3645(3) 0.0434(11) Uani 1 1 d . . . . .
H18A H -0.089297 0.380129 0.378368 0.052 Uiso 1 1 calc R U . . .
H18B H 0.080444 0.272715 0.432303 0.052 Uiso 1 1 calc R U . . .
C19 C 0.0481(5) 0.2016(6) 0.2987(3) 0.0430(11) Uani 1 1 d . . . . .
H19A H 0.101227 0.093979 0.339830 0.052 Uiso 1 1 calc R U . . .
H19B H -0.060070 0.208423 0.278565 0.052 Uiso 1 1 calc R U . . .
C20 C 0.0563(5) 0.3936(5) 0.1353(3) 0.0401(11) Uani 1 1 d . . . . .
H20A H -0.046850 0.388290 0.115399 0.048 Uiso 1 1 calc R U . . .
H20B H 0.120102 0.419814 0.070682 0.048 Uiso 1 1 calc R U . . .
C21 C 0.0189(5) 0.5221(5) 0.2009(3) 0.0432(11) Uani 1 1 d . . . . .
H21A H 0.056693 0.609696 0.161751 0.052 Uiso 1 1 calc R U . . .
H21B H -0.100116 0.565308 0.215737 0.052 Uiso 1 1 calc R U . . .
Pd3 Pd 0.500000 0.000000 0.500000 0.03863(14) Uani 1 2 d S . P . .
Cl24 Cl 0.72321(14) 0.09315(17) 0.47452(9) 0.0606(4) Uani 1 1 d . . . . .
Cl25 Cl 0.34769(16) 0.20299(16) 0.58660(9) 0.0602(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl23 2.3008(11) 2_665 ?
Pd1 Cl23 2.3008(11) . yes
Pd1 Cl22 2.3128(11) 2_665 ?
Pd1 Cl22 2.3128(11) . yes
Pd2 N8 2.047(3) . yes
Pd2 N13 2.054(3) . yes
Pd2 N9 2.054(3) . yes
Pd2 N14 2.058(3) . yes
N8 C10 1.476(5) . ?
N8 C21 1.498(4) . ?
N8 C18 1.502(5) . ?
N9 C15 1.481(5) . ?
N9 C20 1.486(5) . ?
N9 C19 1.494(4) . ?
N13 C12 1.483(6) . ?
N13 H13A 0.8900 . ?
N13 H13B 0.8900 . ?
N14 C17 1.473(6) . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
C10 C11 1.502(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.512(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C15 C16 1.511(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.502(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.519(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.528(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
Pd3 Cl25 2.3066(13) 2_656 ?
Pd3 Cl25 2.3066(13) . ?
Pd3 Cl24 2.3102(12) 2_656 ?
Pd3 Cl24 2.3102(12) . ?

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
Cl23 Pd1 Cl23 180.00(5) 2_665 . ?
Cl23 Pd1 Cl22 89.73(4) 2_665 2_665 ?
Cl23 Pd1 Cl22 90.27(4) . 2_665 ?
Cl23 Pd1 Cl22 90.27(4) 2_665 . ?
Cl23 Pd1 Cl22 89.73(4) . . ?
Cl22 Pd1 Cl22 180.0 2_665 . ?
N8 Pd2 N13 98.61(14) . . ?
N8 Pd2 N9 73.44(13) . . ?
N13 Pd2 N9 170.55(14) . . ?
N8 Pd2 N14 171.44(14) . . ?
N13 Pd2 N14 89.30(14) . . ?
N9 Pd2 N14 98.96(14) . . ?
C10 N8 C21 112.3(3) . . ?
C10 N8 C18 112.1(3) . . ?
C21 N8 C18 106.7(3) . . ?
C10 N8 Pd2 119.1(3) . . ?
C21 N8 Pd2 103.4(2) . . ?
C18 N8 Pd2 102.0(2) . . ?
C15 N9 C20 111.4(3) . . ?
C15 N9 C19 112.0(3) . . ?
C20 N9 C19 107.6(3) . . ?
C15 N9 Pd2 119.5(3) . . ?
C20 N9 Pd2 101.0(2) . . ?
C19 N9 Pd2 104.2(2) . . ?
C12 N13 Pd2 119.2(3) . . ?
C12 N13 H13A 107.5 . . ?
Pd2 N13 H13A 107.5 . . ?
C12 N13 H13B 107.5 . . ?
Pd2 N13 H13B 107.5 . . ?
H13A N13 H13B 107.0 . . ?
C17 N14 Pd2 118.3(3) . . ?
C17 N14 H14A 107.7 . . ?
Pd2 N14 H14A 107.7 . . ?
C17 N14 H14B 107.7 . . ?
Pd2 N14 H14B 107.7 . . ?
H14A N14 H14B 107.1 . . ?
N8 C10 C11 112.9(3) . . ?
N8 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N8 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 C12 113.7(4) . . ?
C10 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N13 C12 C11 114.0(4) . . ?
N13 C12 H12A 108.8 . . ?
C11 C12 H12A 108.8 . . ?
N13 C12 H12B 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.6 . . ?
N9 C15 C16 112.5(3) . . ?
N9 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N9 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 114.8(4) . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
N14 C17 C16 113.5(3) . . ?
N14 C17 H17A 108.9 . . ?
C16 C17 H17A 108.9 . . ?
N14 C17 H17B 108.9 . . ?
C16 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
N8 C18 C19 108.3(3) . . ?
N8 C18 H18A 110.0 . . ?
C19 C18 H18A 110.0 . . ?
N8 C18 H18B 110.0 . . ?
C19 C18 H18B 110.0 . . ?
H18A C18 H18B 108.4 . . ?
N9 C19 C18 107.8(3) . . ?
N9 C19 H19A 110.1 . . ?
C18 C19 H19A 110.1 . . ?
N9 C19 H19B 110.1 . . ?
C18 C19 H19B 110.1 . . ?
H19A C19 H19B 108.5 . . ?
N9 C20 C21 108.2(3) . . ?
N9 C20 H20A 110.1 . . ?
C21 C20 H20A 110.1 . . ?
N9 C20 H20B 110.1 . . ?
C21 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
N8 C21 C20 107.7(3) . . ?
N8 C21 H21A 110.2 . . ?
C20 C21 H21A 110.2 . . ?
N8 C21 H21B 110.2 . . ?
C20 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
Cl25 Pd3 Cl25 180.00(5) 2_656 . ?
Cl25 Pd3 Cl24 90.77(5) 2_656 2_656 ?
Cl25 Pd3 Cl24 89.23(5) . 2_656 ?
Cl25 Pd3 Cl24 89.23(5) 2_656 . ?
Cl25 Pd3 Cl24 90.77(5) . . ?
Cl24 Pd3 Cl24 180.0 2_656 . ?

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
C21 N8 C10 C11 -83.1(4) . . . . ?
C18 N8 C10 C11 156.8(4) . . . . ?
Pd2 N8 C10 C11 37.9(5) . . . . ?
N8 C10 C11 C12 -75.7(5) . . . . ?
Pd2 N13 C12 C11 -32.4(5) . . . . ?
C10 C11 C12 N13 72.7(5) . . . . ?
C20 N9 C15 C16 151.3(4) . . . . ?
C19 N9 C15 C16 -88.2(4) . . . . ?
Pd2 N9 C15 C16 34.1(5) . . . . ?
N9 C15 C16 C17 -73.8(5) . . . . ?
Pd2 N14 C17 C16 -36.2(5) . . . . ?
C15 C16 C17 N14 75.7(5) . . . . ?
C10 N8 C18 C19 -175.9(3) . . . . ?
C21 N8 C18 C19 60.7(4) . . . . ?
Pd2 N8 C18 C19 -47.4(3) . . . . ?
C15 N9 C19 C18 170.7(3) . . . . ?
C20 N9 C19 C18 -66.6(4) . . . . ?
Pd2 N9 C19 C18 40.1(4) . . . . ?
N8 C18 C19 N9 4.7(4) . . . . ?
C15 N9 C20 C21 -176.5(3) . . . . ?
C19 N9 C20 C21 60.4(4) . . . . ?
Pd2 N9 C20 C21 -48.6(3) . . . . ?
C10 N8 C21 C20 169.9(3) . . . . ?
C18 N8 C21 C20 -66.8(4) . . . . ?
Pd2 N8 C21 C20 40.2(3) . . . . ?
N9 C20 C21 N8 5.7(4) . . . . ?

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
_geom_hbond_publ_flag
N13 H13A Cl24 0.89 2.39 3.268(3) 171.6 . yes
N13 H13B Cl23 0.89 2.45 3.300(3) 160.2 . yes
N14 H14A Cl22 0.89 2.47 3.294(3) 154.6 . yes
N14 H14B Cl25 0.89 2.60 3.395(3) 149.0 2_656 yes
C10 H10B Cl25 0.97 2.88 3.783(5) 155.8 2_566 yes
C12 H12B Cl25 0.97 2.95 3.747(5) 140.5 . yes
C16 H16B Cl23 0.97 2.80 3.596(5) 139.4 1_545 yes
C19 H19A Cl24 0.97 2.83 3.676(4) 146.1 2_656 yes
C20 H20A Cl22 0.97 2.94 3.846(4) 156.2 1_455 yes
C20 H20A Cl23 0.97 2.86 3.592(4) 133.1 1_455 yes
C20 H20B Cl23 0.97 2.89 3.816(4) 160.7 2_665 yes
C21 H21A Cl22 0.97 2.80 3.658(4) 147.6 2_665 yes
C21 H21B Cl23 0.97 2.86 3.573(4) 131.4 1_455 yes

_refine_diff_density_max         0.865
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.129

