# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_complex_3
_database_code_depnum_ccdc_archive 'CCDC 2117260'
loop_
_audit_author_name
_audit_author_address
'Jose Perez Perez'
;Technical University of Cartagena
Spain
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-01-10 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         ?
_chemical_formula_sum            'C31 H48 N4 O12 Pd S2'
_chemical_formula_weight         839.25

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'
O O 0.0106 0.0060 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_symmetry_space_group_name_H-M   'P c a b'
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_Int_Tables_number      61

_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+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'

_cell_length_a                   14.7548(7)
_cell_length_b                   14.9919(8)
_cell_length_c                   33.9400(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7507.6(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9478
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      30.44

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             3488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.669
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7043
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            158800
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         2.027
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11463
_reflns_number_gt                9683
_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       'APEX3 2019.1_0 (Bruker AXS Inc.)'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0420P)²+28.0205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11463
_refine_ls_number_parameters     474
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1407
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.210
_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
O3 O 0.52973(17) 0.45787(16) 0.18931(7) 0.0222(5) Uani 1 1 d . . . . .
O4 O 0.51374(17) 0.42876(18) 0.10421(7) 0.0243(5) Uani 1 1 d . . . . .
O2 O 0.6806(2) 0.70851(19) 0.15448(9) 0.0328(6) Uani 1 1 d . . . . .
O1 O 0.65945(19) 0.63094(18) 0.09216(8) 0.0276(6) Uani 1 1 d . . . . .
N1 N 0.63333(19) 0.54612(19) 0.15634(8) 0.0184(5) Uani 1 1 d . . . . .
C8 C 0.7193(2) 0.4632(2) 0.05851(10) 0.0202(6) Uani 1 1 d . . . . .
O5 O 0.59041(19) 0.28628(17) 0.09622(8) 0.0285(6) Uani 1 1 d . . . . .
O6 O 0.79117(18) 0.50300(18) 0.05556(8) 0.0259(5) Uani 1 1 d . . . . .
N2 N 0.68507(19) 0.42823(19) 0.09274(8) 0.0183(5) Uani 1 1 d . . . . .
C1 C 0.5484(2) 0.5244(2) 0.16949(10) 0.0191(6) Uani 1 1 d . . . . .
N4 N 0.8354(2) 0.3564(2) 0.14345(9) 0.0250(6) Uani 1 1 d . . . . .
N3 N 0.7922(2) 0.4841(2) 0.20309(9) 0.0248(6) Uani 1 1 d . . . . .
C20 C 0.7299(3) 0.4642(3) 0.23653(12) 0.0319(8) Uani 1 1 d . . . . .
H20A H 0.676626 0.501471 0.233461 0.038 Uiso 1 1 calc R U . . .
H20B H 0.759850 0.482904 0.260596 0.038 Uiso 1 1 calc R U . . .
C23 C 0.7862(3) 0.2722(2) 0.13265(12) 0.0270(7) Uani 1 1 d . . . . .
H23A H 0.751125 0.284409 0.109100 0.032 Uiso 1 1 calc R U . . .
H23B H 0.743361 0.259584 0.153584 0.032 Uiso 1 1 calc R U . . .
C17 C 0.8133(3) 0.5822(3) 0.20406(11) 0.0264(7) Uani 1 1 d . . . . .
H17A H 0.756465 0.614590 0.202791 0.032 Uiso 1 1 calc R U . . .
H17B H 0.847184 0.596794 0.180422 0.032 Uiso 1 1 calc R U . . .
C16 C 0.8751(3) 0.3467(3) 0.18411(12) 0.0303(8) Uani 1 1 d . . . . .
H16A H 0.838316 0.305416 0.199233 0.036 Uiso 1 1 calc R U . . .
H16B H 0.935584 0.321674 0.182031 0.036 Uiso 1 1 calc R U . . .
C15 C 0.8800(3) 0.4343(3) 0.20550(12) 0.0307(8) Uani 1 1 d . . . . .
H15A H 0.894919 0.423656 0.232935 0.037 Uiso 1 1 calc R U . . .
H15B H 0.927929 0.470393 0.194139 0.037 Uiso 1 1 calc R U . . .
C26 C 0.9066(3) 0.3723(3) 0.11284(13) 0.0316(8) Uani 1 1 d . . . . .
H26A H 0.877440 0.371638 0.087231 0.038 Uiso 1 1 calc R U . . .
H26B H 0.948530 0.322501 0.113523 0.038 Uiso 1 1 calc R U . . .
O9 O 0.8920(2) 0.1658(2) 0.15921(9) 0.0331(6) Uani 1 1 d . . . . .
O10 O 0.9069(2) 0.5363(2) 0.11815(10) 0.0367(7) Uani 1 1 d . . . . .
O8 O 0.6552(2) 0.3319(2) 0.20818(10) 0.0369(7) Uani 1 1 d . . . . .
O7 O 0.8064(2) 0.6256(3) 0.27271(10) 0.0490(9) Uani 1 1 d D . . . .
24 C 0.8400(3) 0.1876(3) 0.12521(12) 0.0291(8) Uani 1 1 d . . . . .
H24 H 0.881178 0.197649 0.103008 0.035 Uiso 1 1 calc R U . . .
C27 C 0.9616(3) 0.4580(3) 0.11600(14) 0.0347(9) Uani 1 1 d . . . . .
H27 H 0.998751 0.454829 0.139893 0.042 Uiso 1 1 calc R U . . .
C18 C 0.8667(3) 0.6172(3) 0.23952(11) 0.0308(8) Uani 1 1 d . . . . .
H18 H 0.915199 0.575078 0.246013 0.037 Uiso 1 1 calc R U . . .
C25 C 0.7747(3) 0.1135(3) 0.11455(15) 0.0408(10) Uani 1 1 d . . . . .
H25A H 0.740745 0.130330 0.091584 0.061 Uiso 1 1 calc R U . . .
H25B H 0.808011 0.059900 0.109204 0.061 Uiso 1 1 calc R U . . .
H25C H 0.733826 0.103401 0.136114 0.061 Uiso 1 1 calc R U . . .
C21 C 0.6980(3) 0.3697(3) 0.24240(14) 0.0401(11) Uani 1 1 d . . . . .
H21 H 0.750892 0.332962 0.248879 0.048 Uiso 1 1 calc R U . . .
C19 C 0.9077(3) 0.7066(3) 0.22901(13) 0.0350(9) Uani 1 1 d . . . . .
H19A H 0.947620 0.699660 0.206878 0.052 Uiso 1 1 calc R U . . .
H19B H 0.860316 0.747831 0.222377 0.052 Uiso 1 1 calc R U . . .
H19C H 0.941301 0.729122 0.251111 0.052 Uiso 1 1 calc R U . . .
C28 C 1.0247(4) 0.4633(4) 0.08051(17) 0.0494(13) Uani 1 1 d . . . . .
H28A H 1.061168 0.410343 0.079314 0.074 Uiso 1 1 calc R U . . .
H28B H 0.989316 0.468212 0.056856 0.074 Uiso 1 1 calc R U . . .
H28C H 1.063184 0.514560 0.082992 0.074 Uiso 1 1 calc R U . . .
C22 C 0.6336(3) 0.3679(4) 0.27765(15) 0.0537(15) Uani 1 1 d . . . . .
H22A H 0.663254 0.393349 0.300178 0.081 Uiso 1 1 calc R U . . .
H22B H 0.580240 0.401879 0.271597 0.081 Uiso 1 1 calc R U . . .
H22C H 0.616869 0.307372 0.283311 0.081 Uiso 1 1 calc R U . . .
O11 O 0.8159(3) 0.2531(4) 0.03293(11) 0.0667(12) Uani 1 1 d . . . . .
C29 C 0.7901(4) 0.2589(3) -0.00095(14) 0.0415(11) Uani 1 1 d . . . . .
C31 C 0.7047(4) 0.2143(3) -0.01445(16) 0.0473(12) Uani 1 1 d . . . . .
H31A H 0.695435 0.226323 -0.041945 0.071 Uiso 1 1 calc R U . . .
H31B H 0.709615 0.151107 -0.010455 0.071 Uiso 1 1 calc R U . . .
H31C H 0.654291 0.236943 0.000382 0.071 Uiso 1 1 calc R U . . .
C30 C 0.8426(4) 0.3098(4) -0.03083(17) 0.0550(14) Uani 1 1 d . . . . .
H30A H 0.811979 0.307030 -0.055753 0.082 Uiso 1 1 calc R U . . .
H30B H 0.847667 0.370933 -0.022647 0.082 Uiso 1 1 calc R U . . .
H30C H 0.902035 0.284433 -0.033368 0.082 Uiso 1 1 calc R U . . .
Pd1 Pd 0.73634(2) 0.45465(2) 0.14826(2) 0.01819(7) Uani 1 1 d . . . . .
S2 S 0.58645(6) 0.37893(6) 0.08617(2) 0.01929(16) Uani 1 1 d . . . . .
S1 S 0.63256(6) 0.64232(6) 0.13262(3) 0.01983(16) Uani 1 1 d . . . . .
C14 C 0.5830(2) 0.3957(2) 0.03515(10) 0.0223(7) Uani 1 1 d . . . . .
C4 C 0.3329(3) 0.6528(3) 0.14662(12) 0.0298(8) Uani 1 1 d . . . . .
H4 H 0.270316 0.650205 0.149545 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3859(2) 0.5856(3) 0.16290(11) 0.0248(7) Uani 1 1 d . . . . .
H3 H 0.359992 0.539200 0.177159 0.030 Uiso 1 1 calc R U . . .
C9 C 0.6581(3) 0.4434(2) 0.02426(10) 0.0222(7) Uani 1 1 d . . . . .
C7 C 0.5156(2) 0.6603(2) 0.13619(10) 0.0186(6) Uani 1 1 d . . . . .
C6 C 0.4647(3) 0.7290(2) 0.12084(11) 0.0244(7) Uani 1 1 d . . . . .
H6 H 0.491380 0.776640 0.107649 0.029 Uiso 1 1 calc R U . . .
C2 C 0.4786(2) 0.5904(2) 0.15714(10) 0.0189(6) Uani 1 1 d . . . . .
C11 C 0.6014(3) 0.4470(3) -0.04130(11) 0.0336(9) Uani 1 1 d . . . . .
H11 H 0.606996 0.464303 -0.067499 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5258(3) 0.3984(3) -0.02979(12) 0.0343(9) Uani 1 1 d . . . . .
H12 H 0.481899 0.383632 -0.048348 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3709(3) 0.7237(3) 0.12608(12) 0.0293(8) Uani 1 1 d . . . . .
H5 H 0.333685 0.767932 0.115735 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6691(3) 0.4705(3) -0.01460(11) 0.0287(8) Uani 1 1 d . . . . .
H10 H 0.719679 0.503057 -0.022474 0.034 Uiso 1 1 calc R U . . .
C13 C 0.5149(3) 0.3717(3) 0.00905(11) 0.0273(8) Uani 1 1 d . . . . .
H13 H 0.464454 0.339298 0.017178 0.033 Uiso 1 1 calc R U . . .
O12 O 0.6107(3) 0.1443(3) 0.2130(2) 0.0818(17) Uani 1 1 d D . . . .
H32A H 0.601(6) 0.193(4) 0.198(2) 0.123 Uiso 1 1 d D U . . .
H32B H 0.6703(17) 0.137(4) 0.2193(17) 0.055(17) Uiso 1 1 d D . . . .
H8A H 0.610(5) 0.374(5) 0.201(2) 0.07(2) Uiso 1 1 d . . . . .
H7A H 0.836(5) 0.642(6) 0.2954(15) 0.12(3) Uiso 1 1 d D . . . .
H9A H 0.950(6) 0.129(6) 0.151(3) 0.13(3) Uiso 1 1 d . . . . .
H10A H 0.877(4) 0.536(4) 0.0945(16) 0.040(15) Uiso 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
O3 C1 1.234(4) . ?
O4 S2 1.444(3) . ?
O2 S1 1.427(3) . ?
O1 S1 1.439(3) . ?
N1 C1 1.370(4) . ?
N1 S1 1.652(3) . ?
N1 Pd1 2.065(3) . ?
C8 O6 1.221(4) . ?
C8 N2 1.371(4) . ?
C8 C9 1.502(5) . ?
O5 S2 1.431(3) . ?
N2 S2 1.647(3) . ?
N2 Pd1 2.069(3) . ?
C1 C2 1.488(5) . ?
N4 C26 1.497(5) . ?
N4 C23 1.502(5) . ?
N4 C16 1.507(5) . ?
N4 Pd1 2.081(3) . ?
N3 C20 1.491(5) . ?
N3 C15 1.498(5) . ?
N3 C17 1.504(5) . ?
N3 Pd1 2.083(3) . ?
C20 C21 1.506(7) . ?
C23 24 1.516(5) . ?
C17 C18 1.531(5) . ?
C16 C15 1.503(6) . ?
C26 C27 1.523(6) . ?
O9 24 1.424(5) . ?
O10 C27 1.426(5) . ?
O8 C21 1.438(6) . ?
O7 C18 1.441(5) . ?
24 C25 1.514(6) . ?
C27 C28 1.524(6) . ?
C18 C19 1.514(6) . ?
C21 C22 1.528(7) . ?
O11 C29 1.214(6) . ?
C29 C30 1.487(8) . ?
C29 C31 1.498(8) . ?
S2 C14 1.751(4) . ?
S1 C7 1.751(3) . ?
C14 C9 1.370(5) . ?
C14 C13 1.387(5) . ?
C4 C3 1.389(5) . ?
C4 C5 1.390(6) . ?
C3 C2 1.384(5) . ?
C9 C10 1.389(5) . ?
C7 C6 1.377(5) . ?
C7 C2 1.380(5) . ?
C6 C5 1.397(5) . ?
C11 C12 1.388(7) . ?
C11 C10 1.395(6) . ?
C12 C13 1.387(6) . ?

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
C1 N1 S1 111.1(2) . . ?
C1 N1 Pd1 123.9(2) . . ?
S1 N1 Pd1 121.34(16) . . ?
O6 C8 N2 125.2(3) . . ?
O6 C8 C9 123.7(3) . . ?
N2 C8 C9 111.0(3) . . ?
C8 N2 S2 112.5(2) . . ?
C8 N2 Pd1 124.3(2) . . ?
S2 N2 Pd1 122.16(16) . . ?
O3 C1 N1 125.1(3) . . ?
O3 C1 C2 122.4(3) . . ?
N1 C1 C2 112.5(3) . . ?
C26 N4 C23 107.7(3) . . ?
C26 N4 C16 112.2(3) . . ?
C23 N4 C16 109.2(3) . . ?
C26 N4 Pd1 115.8(2) . . ?
C23 N4 Pd1 106.0(2) . . ?
C16 N4 Pd1 105.7(2) . . ?
C20 N3 C15 113.1(3) . . ?
C20 N3 C17 107.9(3) . . ?
C15 N3 C17 107.9(3) . . ?
C20 N3 Pd1 113.2(2) . . ?
C15 N3 Pd1 106.6(2) . . ?
C17 N3 Pd1 108.0(2) . . ?
N3 C20 C21 118.8(4) . . ?
N4 C23 24 119.4(3) . . ?
N3 C17 C18 117.3(3) . . ?
C15 C16 N4 112.1(3) . . ?
N3 C15 C16 111.6(3) . . ?
N4 C26 C27 117.3(3) . . ?
O9 24 C25 111.6(3) . . ?
O9 24 C23 109.8(3) . . ?
C25 24 C23 108.7(3) . . ?
O10 C27 C26 113.3(3) . . ?
O10 C27 C28 110.1(4) . . ?
C26 C27 C28 108.2(4) . . ?
O7 C18 C19 110.8(4) . . ?
O7 C18 C17 109.1(3) . . ?
C19 C18 C17 108.9(3) . . ?
O8 C21 C20 113.7(3) . . ?
O8 C21 C22 110.6(4) . . ?
C20 C21 C22 108.3(5) . . ?
O11 C29 C30 121.2(6) . . ?
O11 C29 C31 121.5(5) . . ?
C30 C29 C31 117.3(5) . . ?
N1 Pd1 N2 88.79(11) . . ?
N1 Pd1 N4 175.58(12) . . ?
N2 Pd1 N4 92.85(12) . . ?
N1 Pd1 N3 91.81(12) . . ?
N2 Pd1 N3 177.68(12) . . ?
N4 Pd1 N3 86.70(12) . . ?
O5 S2 O4 115.56(17) . . ?
O5 S2 N2 111.53(16) . . ?
O4 S2 N2 111.52(15) . . ?
O5 S2 C14 112.09(17) . . ?
O4 S2 C14 108.88(16) . . ?
N2 S2 C14 95.49(16) . . ?
O2 S1 O1 116.20(18) . . ?
O2 S1 N1 110.49(17) . . ?
O1 S1 N1 111.07(15) . . ?
O2 S1 C7 110.23(17) . . ?
O1 S1 C7 110.87(17) . . ?
N1 S1 C7 96.18(16) . . ?
C9 C14 C13 123.3(3) . . ?
C9 C14 S2 108.5(3) . . ?
C13 C14 S2 128.0(3) . . ?
C3 C4 C5 121.8(4) . . ?
C2 C3 C4 117.6(4) . . ?
C14 C9 C10 120.3(4) . . ?
C14 C9 C8 112.4(3) . . ?
C10 C9 C8 127.3(4) . . ?
C6 C7 C2 123.2(3) . . ?
C6 C7 S1 128.8(3) . . ?
C2 C7 S1 107.9(2) . . ?
C7 C6 C5 116.7(3) . . ?
C7 C2 C3 120.2(3) . . ?
C7 C2 C1 112.2(3) . . ?
C3 C2 C1 127.6(3) . . ?
C12 C11 C10 121.7(4) . . ?
C13 C12 C11 120.8(4) . . ?
C4 C5 C6 120.5(4) . . ?
C9 C10 C11 117.3(4) . . ?
C14 C13 C12 116.6(4) . . ?

_refine_diff_density_max         1.689
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.107



####################################################################### 
# 
# 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_complex_1
_database_code_depnum_ccdc_archive 'CCDC 2117261'
loop_
_audit_author_name
_audit_author_address
'Jose Perez Perez'
;Technical University of Cartagena
Spain
;
_audit_update_record             
;
2022-01-06 deposited with the CCDC.	2022-01-10 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         ?
_chemical_formula_sum            'C14 H32 Cl2 N2 O4 Pd'
_chemical_formula_weight         469.71

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.0082(5)
_cell_length_b                   11.6508(8)
_cell_length_c                   18.8174(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.478(3)
_cell_angle_gamma                90
_cell_volume                     1974.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9455
_cell_measurement_theta_min      4.15
_cell_measurement_theta_max      74.66

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_F_000             968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.229
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4674
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37191
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.056
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4040
_reflns_number_gt                3418
_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       'APEX3 2019.1_0 (Bruker AXS Inc.)'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0718P)²+6.6809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4040
_refine_ls_number_parameters     255
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1474
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002

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 0.22781(4) 0.15825(4) 0.78045(2) 0.03020(16) Uani 1 1 d . . . . .
Cl1 Cl 0.26542(16) 0.27116(14) 0.68223(8) 0.0432(3) Uani 1 1 d . . . . .
Cl2 Cl 0.39123(16) 0.27066(16) 0.84643(9) 0.0482(4) Uani 1 1 d . . . . .
N1 N 0.0787(5) 0.0515(4) 0.7256(2) 0.0333(10) Uani 1 1 d D . . . .
N2 N 0.1791(5) 0.0564(5) 0.8698(3) 0.0381(11) Uani 1 1 d . . . . .
C3 C 0.1296(6) 0.0184(5) 0.6530(3) 0.0363(12) Uani 1 1 d . . . . .
H3A H 0.126415 0.086006 0.622948 0.044 Uiso 1 1 calc R U . . .
H3B H 0.059708 -0.036703 0.633391 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2840(6) -0.0328(6) 0.6492(3) 0.0398(13) Uani 1 1 d . . . . .
H4 H 0.346558 0.002624 0.685970 0.048 Uiso 1 1 calc R U . . .
C6 C -0.0627(6) 0.1198(5) 0.7197(3) 0.0377(12) Uani 1 1 d . U . . .
H6AA H -0.051657 0.174598 0.681327 0.045 Uiso 0.6 1 calc R U P A 1
H6AB H -0.074108 0.163342 0.763274 0.045 Uiso 0.6 1 calc R U P A 1
H6BC H -0.040584 0.190549 0.694792 0.045 Uiso 0.4 1 calc R U P B 2
H6BD H -0.092845 0.140541 0.767395 0.045 Uiso 0.4 1 calc R U P B 2
C2 C 0.0475(6) -0.0157(6) 0.8480(3) 0.0388(12) Uani 1 1 d . . . . .
H2A H 0.041865 -0.083129 0.878104 0.047 Uiso 1 1 calc R U . . .
H2B H -0.043204 0.028102 0.853769 0.047 Uiso 1 1 calc R U . . .
C1 C 0.0632(6) -0.0514(5) 0.7719(3) 0.0384(12) Uani 1 1 d . . . . .
H1A H 0.149846 -0.100060 0.767025 0.046 Uiso 1 1 calc R U . . .
H1B H -0.023386 -0.095130 0.757271 0.046 Uiso 1 1 calc R U . . .
C10 C 0.0467(7) 0.2310(6) 0.9226(3) 0.0452(14) Uani 1 1 d . . . . .
H10 H 0.077301 0.269818 0.878886 0.054 Uiso 1 1 calc R U . . .
C13 C 0.3135(8) -0.0990(7) 0.9452(4) 0.0496(15) Uani 1 1 d . . . . .
H13 H 0.299950 -0.053383 0.988392 0.059 Uiso 0.563(14) 1 calc R U P C 1
H13A H 0.242484 -0.159085 0.931776 0.059 Uiso 0.437(14) 1 calc R U P C 2
C12 C 0.3154(7) -0.0157(7) 0.8833(3) 0.0469(15) Uani 1 1 d . . . . .
H12A H 0.398620 0.035932 0.890434 0.056 Uiso 1 1 calc R U . . .
H12B H 0.334866 -0.059386 0.840538 0.056 Uiso 1 1 calc R U . . .
C9 C 0.1433(7) 0.1267(6) 0.9335(3) 0.0455(15) Uani 1 1 d . . . . .
H9A H 0.236145 0.151760 0.954820 0.055 Uiso 1 1 calc R U . . .
H9B H 0.094904 0.077105 0.967599 0.055 Uiso 1 1 calc R U . . .
C7 C -0.2050(12) 0.0526(13) 0.7067(7) 0.044(2) Uani 0.6 1 d D U P D 1
H7 H -0.224580 -0.000583 0.745882 0.053 Uiso 0.6 1 calc R U P D 1
C14 C 0.4622(8) -0.1586(7) 0.9523(4) 0.0563(18) Uani 1 1 d . . . . .
H14A H 0.540018 -0.102311 0.953043 0.084 Uiso 1 1 calc R U . . .
H14B H 0.464971 -0.201928 0.995706 0.084 Uiso 1 1 calc R U . . .
H14C H 0.475916 -0.209379 0.912733 0.084 Uiso 1 1 calc R U . . .
C5 C 0.3532(7) -0.0108(7) 0.5767(3) 0.0498(16) Uani 1 1 d . . . . .
H5A H 0.359218 0.070394 0.568437 0.075 Uiso 1 1 calc R U . . .
H5B H 0.451074 -0.043355 0.575654 0.075 Uiso 1 1 calc R U . . .
H5C H 0.292909 -0.045577 0.540294 0.075 Uiso 1 1 calc R U . . .
C11 C 0.0661(11) 0.3132(8) 0.9842(4) 0.069(2) Uani 1 1 d . . . . .
H11A H 0.168534 0.335195 0.988108 0.104 Uiso 1 1 calc R U . . .
H11B H 0.006196 0.380138 0.976184 0.104 Uiso 1 1 calc R U . . .
H11C H 0.035917 0.276281 1.027324 0.104 Uiso 1 1 calc R U . . .
O1 O 0.2736(5) -0.1540(4) 0.6630(3) 0.0457(10) Uani 1 1 d . . . . .
H1 H 0.356513 -0.182812 0.661050 0.069 Uiso 1 1 calc R U . . .
O3 O -0.1053(5) 0.1956(5) 0.9147(3) 0.0536(12) Uani 1 1 d . . . . .
H3 H -0.158039 0.252283 0.908804 0.080 Uiso 1 1 calc R U . . .
O4B O 0.2025(10) -0.1816(9) 0.9442(5) 0.056(3) Uani 0.563(14) 1 d . . P C 1
H4B H 0.137538 -0.163611 0.972380 0.084 Uiso 0.563(14) 1 calc R U P C 1
O2 O -0.1927(12) -0.0084(13) 0.6395(7) 0.066(3) Uani 0.46 1 d D U P D 1
H2 H -0.255200 0.016090 0.611400 0.099 Uiso 0.46 1 calc R U P D 1
O4 O 0.2618(17) -0.0535(10) 1.0091(7) 0.066(4) Uani 0.437(14) 1 d . . P C 2
H4A H 0.223372 -0.104609 1.032624 0.099 Uiso 0.437(14) 1 calc R U P C 2
C8 C -0.333(2) 0.1373(19) 0.6964(12) 0.065(5) Uani 0.6 1 d D U P D 1
H8A H -0.343746 0.183204 0.738480 0.098 Uiso 0.6 1 calc R U P D 1
H8B H -0.423705 0.095655 0.687789 0.098 Uiso 0.6 1 calc R U P D 1
H8C H -0.313245 0.186220 0.656602 0.098 Uiso 0.6 1 calc R U P D 1
O5 O -0.277(4) 0.027(3) 0.7762(18) 0.049(7) Uiso 0.14 1 d . . P E 3
H5 H -0.279247 -0.038783 0.795666 0.073 Uiso 0.14 1 d R U P E 3
C8A C -0.338(3) 0.111(3) 0.7143(15) 0.057(6) Uani 0.4 1 d D U P D 2
H8AA H -0.344289 0.191724 0.703941 0.086 Uiso 0.4 1 calc R U P D 2
H8AB H -0.335499 0.100077 0.764828 0.086 Uiso 0.4 1 calc R U P D 2
H8AC H -0.422285 0.072379 0.694335 0.086 Uiso 0.4 1 calc R U P D 2
C7A C -0.1964(18) 0.0627(19) 0.6822(10) 0.045(4) Uani 0.4 1 d D U P D 2
H7A H -0.193098 -0.019856 0.692139 0.054 Uiso 0.4 1 calc R U P D 2
O2A O -0.1871(14) 0.0783(13) 0.6069(6) 0.054(3) Uani 0.4 1 d D . P D 2
H2AA H -0.226024 0.139422 0.595835 0.081 Uiso 0.4 1 calc R U P D 2


_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 N1 2.096(5) . ?
Pd1 N2 2.107(5) . ?
Pd1 Cl1 2.2960(15) . ?
Pd1 Cl2 2.3224(15) . ?
N1 C1 1.490(8) . ?
N1 C3 1.495(7) . ?
N1 C6 1.505(7) . ?
N2 C9 1.488(8) . ?
N2 C2 1.507(7) . ?
N2 C12 1.508(8) . ?
C3 C4 1.515(8) . ?
C4 O1 1.439(8) . ?
C4 C5 1.527(8) . ?
C6 C7 1.520(14) . ?
C6 C7A 1.543(18) . ?
C2 C1 1.499(8) . ?
C10 O3 1.437(8) . ?
C10 C9 1.508(10) . ?
C10 C11 1.512(10) . ?
C13 O4B 1.387(12) . ?
C13 O4 1.399(15) . ?
C13 C14 1.513(10) . ?
C13 C12 1.515(10) . ?
C7 O2 1.456(16) . ?
C7 C8 1.532(15) . ?
C8A C7A 1.522(18) . ?
C7A O2A 1.431(19) . ?

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 Pd1 N2 85.54(19) . . ?
N1 Pd1 Cl1 92.38(14) . . ?
N2 Pd1 Cl1 176.45(14) . . ?
N1 Pd1 Cl2 177.04(14) . . ?
N2 Pd1 Cl2 91.50(14) . . ?
Cl1 Pd1 Cl2 90.58(6) . . ?
C1 N1 C3 111.0(5) . . ?
C1 N1 C6 112.6(4) . . ?
C3 N1 C6 109.6(4) . . ?
C1 N1 Pd1 104.6(3) . . ?
C3 N1 Pd1 113.8(3) . . ?
C6 N1 Pd1 105.1(3) . . ?
C9 N2 C2 110.5(5) . . ?
C9 N2 C12 110.6(5) . . ?
C2 N2 C12 111.9(5) . . ?
C9 N2 Pd1 112.4(4) . . ?
C2 N2 Pd1 105.4(3) . . ?
C12 N2 Pd1 105.9(4) . . ?
N1 C3 C4 115.7(4) . . ?
O1 C4 C3 108.5(5) . . ?
O1 C4 C5 110.7(5) . . ?
C3 C4 C5 111.0(5) . . ?
N1 C6 C7 116.8(7) . . ?
N1 C6 C7A 117.6(8) . . ?
C1 C2 N2 109.5(5) . . ?
N1 C1 C2 110.3(5) . . ?
O3 C10 C9 109.3(6) . . ?
O3 C10 C11 111.4(6) . . ?
C9 C10 C11 110.1(6) . . ?
O4B C13 C14 108.7(7) . . ?
O4 C13 C14 113.5(8) . . ?
O4B C13 C12 116.5(7) . . ?
O4 C13 C12 115.1(8) . . ?
C14 C13 C12 110.3(6) . . ?
N2 C12 C13 118.2(5) . . ?
N2 C9 C10 117.6(5) . . ?
O2 C7 C6 108.7(10) . . ?
O2 C7 C8 105.5(12) . . ?
C6 C7 C8 108.8(14) . . ?
O2A C7A C8A 113.7(17) . . ?
O2A C7A C6 110.3(14) . . ?
C8A C7A C6 108.0(19) . . ?

_refine_diff_density_max         2.051
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.130



