# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_3pcdcl
_database_code_depnum_ccdc_archive 'CCDC 2331639'
loop_
_audit_author_name
_audit_author_address
'Houcine Naili'
;University of Sfax
Tunisia
;
_audit_update_record             
;
2024-02-07 deposited with the CCDC.	2024-05-19 downloaded from the CCDC.
;
_audit_creation_date             2021-09-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Pd, 2(H2 O), 2(C6 H10 N2)'
_chemical_formula_sum            'C12 H24 Cl6 N4 O2 Pd'
_chemical_formula_weight         575.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H24 Cl6 N4 O2 Pd1'
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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.7207(8)
_cell_length_b                   7.7941(8)
_cell_length_c                   9.5977(9)
_cell_angle_alpha                81.799(8)
_cell_angle_beta                 83.134(8)
_cell_angle_gamma                66.739(10)
_cell_volume                     523.91(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7068
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2550
_cell_measurement_theta_min      3.4110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 2 10 0.1438
2 -3 -12 0.1716
-8 2 -7 0.1051
8 -2 6 0.0396
0 -6 -12 0.1586
-7 4 0 0.1755
9 2 8 0.0708
-9 -2 -8 0.1044
-10 -4 2 0.1197
-10 -6 -7 0.1346
3 -2 -12 0.1923
9 6 8 0.1321
5 11 0 0.1789
1 1 13 0.1088
-3 -8 8 0.1001
-1 0 -13 0.1546
-5 -11 -2 0.1666

_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.157
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.4242 2.2522 9.8106 0.0976 0.7292 0.6773
1.6343 -3.4465 -12.3720 -0.0579 -0.4246 -0.9035
-7.9285 1.5413 -7.2370 0.5184 0.6770 -0.5224
8.0287 -2.1966 5.9521 -0.5513 -0.7196 0.4222
0.2391 -5.5939 -11.7895 -0.2457 -0.3171 -0.9160
-7.3698 4.4911 -0.1068 0.6087 0.7929 0.0281
8.9136 1.8702 8.4277 -0.2441 -0.6931 0.6783
-8.8939 -1.8890 -8.4750 0.2430 0.6900 -0.6817
-10.3907 -3.8138 2.4583 -0.1820 0.9831 0.0184
-9.7171 -5.7016 -7.2119 -0.1355 0.7241 -0.6763
2.6610 -1.6712 -12.4253 0.0896 -0.4940 -0.8648
9.4529 5.7175 7.7774 0.1290 -0.6887 0.7134
5.2686 10.7972 -0.0584 0.9136 -0.3233 0.2467
1.2928 0.6781 13.4789 -0.3053 0.1101 0.9459
-3.3346 -7.9650 7.7800 -0.8821 0.3133 0.3519
-1.0384 -0.1664 -13.4154 0.3468 -0.1247 -0.9296
-5.4884 -10.9038 -2.2921 -0.8594 0.3037 -0.4114

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_min         2.860
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00  14.00   1.00    1.00    --  -10.24 -37.00  30.00   99
  2  ω    -38.00  63.00   1.00    1.00    --  -10.24  57.00 150.00  101
  3  ω    -43.00  39.00   1.00    1.00    --  -10.24  77.00-150.00   82
  4  ω    -21.00  39.00   1.00    1.00    --   11.34  77.00  60.00   60
  5  ω      1.00  52.00   1.00    1.00    --   11.34 -99.00 -60.00   51
  6  ω    -37.00  66.00   1.00    1.00    --  -10.24  31.00  45.00  103
  7  ω    -21.00  39.00   1.00    1.00    --   11.34  77.00-150.00   60
  8  ω      1.00  52.00   1.00    1.00    --   11.34 -99.00  60.00   51
  9  ω    -13.00  86.00   1.00    1.00    --   11.34  37.00 -30.00   99
 10  ω    -21.00  39.00   1.00    1.00    --   11.34  77.00 -30.00   60
 11  ω    -43.00  39.00   1.00    1.00    --  -10.24  77.00 -60.00   82
 12  ω    -43.00 -18.00   1.00    1.00    --  -10.24  77.00 -30.00   25
 13  ω      1.00  52.00   1.00    1.00    --   11.34 -99.00-120.00   51
 14  ω      1.00  52.00   1.00    1.00    --   11.34 -99.00 150.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0237053000
_diffrn_orient_matrix_UB_12      0.0960443000
_diffrn_orient_matrix_UB_13      -0.0252074000
_diffrn_orient_matrix_UB_21      -0.0971307000
_diffrn_orient_matrix_UB_22      0.0175473000
_diffrn_orient_matrix_UB_23      0.0165989000
_diffrn_orient_matrix_UB_31      0.0072005000
_diffrn_orient_matrix_UB_32      0.0197067000
_diffrn_orient_matrix_UB_33      0.0684925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2179
_reflns_number_total             2682
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.250
_refine_ls_extinction_coef       0.068(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+3.4193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1587
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1B,H1C)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C5(H5)
2.d Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.0188(2) Uani 1 2 d S . P . .
Cl1 Cl 0.5989(2) 0.1667(2) 0.16336(15) 0.0234(3) Uani 1 1 d . . . . .
Cl2 Cl 0.8469(2) 0.4208(2) -0.10702(16) 0.0254(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5626(2) 0.6671(2) 0.19765(15) 0.0243(3) Uani 1 1 d . . . . .
O1 O 0.4126(8) 0.4135(7) 0.4230(5) 0.0339(11) Uani 1 1 d G . . . .
H1B H 0.419646 0.335648 0.366778 0.051 Uiso 1 1 d G U . . .
H1C H 0.451761 0.495714 0.379361 0.051 Uiso 1 1 d G U . . .
N1 N 1.0931(9) 0.6614(8) 0.5422(7) 0.0363(14) Uani 1 1 d . . . . .
H1 H 1.195044 0.568668 0.520605 0.044 Uiso 1 1 calc R U . . .
N2 N 0.7719(8) 0.8463(8) 0.9536(5) 0.0264(11) Uani 1 1 d . . . . .
H2A H 0.671036 0.851305 0.914336 0.032 Uiso 1 1 calc R U . . .
H2B H 0.734906 0.907607 1.030144 0.032 Uiso 1 1 calc R U . . .
H2C H 0.844982 0.726966 0.977739 0.032 Uiso 1 1 calc R U . . .
C1 C 0.9656(11) 0.7461(10) 0.4445(7) 0.0360(16) Uani 1 1 d . . . . .
H1A H 0.988196 0.704263 0.355550 0.043 Uiso 1 1 calc R U . . .
C2 C 0.8041(11) 0.8928(11) 0.4768(7) 0.0373(16) Uani 1 1 d . . . . .
H2 H 0.714951 0.950581 0.410130 0.045 Uiso 1 1 calc R U . . .
C3 C 0.7717(9) 0.9564(9) 0.6075(7) 0.0279(13) Uani 1 1 d . . . . .
H3 H 0.661721 1.057848 0.629390 0.034 Uiso 1 1 calc R U . . .
C4 C 0.9059(8) 0.8667(9) 0.7071(6) 0.0243(12) Uani 1 1 d . . . . .
C5 C 1.0668(9) 0.7162(9) 0.6717(7) 0.0286(13) Uani 1 1 d . . . . .
H5 H 1.156551 0.653105 0.737265 0.034 Uiso 1 1 calc R U . . .
C6 C 0.8804(9) 0.9348(9) 0.8508(7) 0.0263(13) Uani 1 1 d . . . . .
H6A H 1.003357 0.905024 0.884953 0.032 Uiso 1 1 calc R U . . .
H6B H 0.813984 1.070196 0.842977 0.032 Uiso 1 1 calc R U . . .


_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 Cl1 2.7106(14) 2_665 ?
Pd1 Cl1 2.7106(14) . ?
Pd1 Cl2 2.6130(15) . ?
Pd1 Cl2 2.6130(15) 2_665 ?
Pd1 Cl3 2.6363(14) 2_665 ?
Pd1 Cl3 2.6364(14) . ?
O1 H1B 0.8499 . ?
O1 H1C 0.8508 . ?
N1 H1 0.8600 . ?
N1 C1 1.347(10) . ?
N1 C5 1.338(9) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C6 1.488(8) . ?
C1 H1A 0.9300 . ?
C1 C2 1.357(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.373(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.396(9) . ?
C4 C5 1.377(9) . ?
C4 C6 1.512(9) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
Cl1 Pd1 Cl1 180.0 2_665 . ?
Cl2 Pd1 Cl1 91.98(5) . . ?
Cl2 Pd1 Cl1 88.02(5) . 2_665 ?
Cl2 Pd1 Cl1 91.98(5) 2_665 2_665 ?
Cl2 Pd1 Cl1 88.02(5) 2_665 . ?
Cl2 Pd1 Cl2 180.0 . 2_665 ?
Cl2 Pd1 Cl3 90.06(5) 2_665 2_665 ?
Cl2 Pd1 Cl3 89.94(5) 2_665 . ?
Cl2 Pd1 Cl3 89.94(5) . 2_665 ?
Cl2 Pd1 Cl3 90.06(5) . . ?
Cl3 Pd1 Cl1 87.66(4) 2_665 . ?
Cl3 Pd1 Cl1 87.66(4) . 2_665 ?
Cl3 Pd1 Cl1 92.34(4) . . ?
Cl3 Pd1 Cl1 92.34(4) 2_665 2_665 ?
Cl3 Pd1 Cl3 180.0 2_665 . ?
H1B O1 H1C 109.4 . . ?
C1 N1 H1 118.8 . . ?
C5 N1 H1 118.8 . . ?
C5 N1 C1 122.4(6) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
N1 C1 H1A 120.2 . . ?
N1 C1 C2 119.5(6) . . ?
C2 C1 H1A 120.2 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.3(7) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.1(6) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C6 121.4(6) . . ?
C5 C4 C3 119.0(6) . . ?
C5 C4 C6 119.6(6) . . ?
N1 C5 C4 119.5(6) . . ?
N1 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
N2 C6 C4 111.2(5) . . ?
N2 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
C4 C6 H6A 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?

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
N1 H1 O1 0.86 1.87 2.706(8) 162.8 1_655 yes

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
N1 C1 C2 C3 0.9(10) . . . . ?
C1 N1 C5 C4 -1.2(10) . . . . ?
C1 C2 C3 C4 -0.8(10) . . . . ?
C2 C3 C4 C5 -0.3(9) . . . . ?
C2 C3 C4 C6 178.0(6) . . . . ?
C3 C4 C5 N1 1.3(9) . . . . ?
C3 C4 C6 N2 88.2(7) . . . . ?
C5 N1 C1 C2 0.1(10) . . . . ?
C5 C4 C6 N2 -93.5(7) . . . . ?
C6 C4 C5 N1 -177.0(5) . . . . ?

_olex2_date_sample_data_collection 2021-09-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id 3PCdCl
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.759
