# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2168350'
loop_
_audit_author_name
_audit_author_address
'Dr. Shobhana Krishnaswamy '
;Department of Chemistry, IIT Madras
India
;
_audit_update_record             
;
2022-04-23 deposited with the CCDC.	2022-06-28 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            'C28 H42 N14 O16 Pd2'
_chemical_formula_weight         1043.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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                   7.7499(9)
_cell_length_b                   10.4043(12)
_cell_length_c                   12.9225(15)
_cell_angle_alpha                87.015(5)
_cell_angle_beta                 74.757(5)
_cell_angle_gamma                75.488(5)
_cell_volume                     973.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9867
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      72.91

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    8.245
_shelx_estimated_absorpt_T_min   0.289
_shelx_estimated_absorpt_T_max   0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_process_details   'SADABS, Bruker 2016'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro focus sealed tube'
_diffrn_measurement_device_type  
'Bruker axs kappa apex3 PHOTON II Diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15644
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.545
_diffrn_reflns_theta_max         67.478
_diffrn_reflns_theta_full        67.478
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             3460
_reflns_number_gt                2854
_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(Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_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)+(0.2000P)²] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0041(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3460
_refine_ls_number_parameters     290
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0990
_refine_ls_wR_factor_ref         0.3024
_refine_ls_wR_factor_gt          0.2860
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_restrained_S_all      1.256
_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 0.21010(9) 0.07070(7) 0.23767(5) 0.0559(5) Uani 1 1 d . . . . .
C1 C -0.0710(15) 0.3318(11) 0.2402(9) 0.061(3) Uani 1 1 d . . . . .
C2 C -0.1463(14) 0.3815(10) 0.3440(9) 0.060(2) Uani 1 1 d . . . . .
H2 H -0.182832 0.324389 0.400867 0.072 Uiso 1 1 calc R U . . .
C3 C -0.1682(15) 0.5147(11) 0.3648(8) 0.061(2) Uani 1 1 d . . . . .
C4 C -0.1129(16) 0.5973(12) 0.2815(9) 0.069(3) Uani 1 1 d . . . . .
H4 H -0.127926 0.688645 0.295923 0.083 Uiso 1 1 calc R U . . .
C5 C -0.0365(17) 0.5483(12) 0.1781(9) 0.071(3) Uani 1 1 d . . . . .
H5 H 0.000723 0.605839 0.121676 0.085 Uiso 1 1 calc R U . . .
C6 C -0.0135(15) 0.4132(11) 0.1560(8) 0.064(3) Uani 1 1 d . . . . .
H6 H 0.040073 0.378270 0.085131 0.077 Uiso 1 1 calc R U . . .
C7 C -0.3073(14) 0.5141(11) 0.5612(9) 0.060(2) Uani 1 1 d . . . . .
C8 C -0.2822(14) 0.7020(11) 0.6667(8) 0.059(2) Uani 1 1 d . . . . .
H8 H -0.194457 0.722338 0.605560 0.071 Uiso 1 1 calc R U . . .
C9 C -0.3583(13) 0.5979(10) 0.6603(8) 0.057(2) Uani 1 1 d . . . . .
C10 C -0.4844(15) 0.5675(11) 0.7522(9) 0.062(2) Uani 1 1 d . . . . .
H10 H -0.537634 0.494703 0.751861 0.074 Uiso 1 1 calc R U . . .
C11 C -0.5295(16) 0.6458(12) 0.8435(8) 0.067(3) Uani 1 1 d . . . . .
H11 H -0.616388 0.628655 0.906327 0.080 Uiso 1 1 calc R U . . .
C12 C -0.4486(15) 0.7465(11) 0.8421(9) 0.065(3) Uani 1 1 d . . . . .
H12 H -0.479880 0.798717 0.905527 0.078 Uiso 1 1 calc R U . . .
C13 C 0.4325(18) -0.1941(12) 0.2422(11) 0.070(3) Uani 1 1 d . . . . .
H13A H 0.391110 -0.230730 0.314131 0.084 Uiso 1 1 calc R U . . .
H13B H 0.556489 -0.249117 0.206988 0.084 Uiso 1 1 calc R U . . .
C14 C 0.2987(18) -0.2001(12) 0.1760(10) 0.072(3) Uani 1 1 d . . . . .
H14A H 0.349520 -0.179371 0.100093 0.086 Uiso 1 1 calc R U . . .
H14B H 0.275566 -0.289754 0.178983 0.086 Uiso 1 1 calc R U . . .
N1 N -0.0378(13) 0.1934(9) 0.2196(8) 0.059(2) Uani 1 1 d . . . . .
H1A H -0.043433 0.183088 0.151124 0.071 Uiso 1 1 calc R U . . .
H1B H -0.131727 0.163716 0.263868 0.071 Uiso 1 1 calc R U . . .
N2 N 0.4429(14) -0.0587(10) 0.2533(9) 0.064(2) Uani 1 1 d D . . . .
H2A H 0.471(18) -0.041(14) 0.312(6) 0.077 Uiso 1 1 d D U . . .
H2B H 0.537(12) -0.047(13) 0.202(7) 0.077 Uiso 1 1 d D U . . .
N3 N 0.1213(15) -0.0972(11) 0.2249(9) 0.066(2) Uani 1 1 d . . . . .
H3A H 0.075(18) -0.140(14) 0.288(12) 0.079 Uiso 1 1 d . U . . .
H3B H 0.036(18) -0.081(13) 0.185(10) 0.079 Uiso 1 1 d . U . . .
N4 N -0.2376(13) 0.5725(9) 0.4685(7) 0.064(2) Uani 1 1 d . . . . .
H4N H -0.235368 0.656050 0.473747 0.076 Uiso 1 1 calc R U . . .
N5 N -0.3277(11) 0.7768(9) 0.7569(7) 0.0530(18) Uani 1 1 d . . . . .
N6 N 0.3790(15) 0.8863(9) 0.5385(8) 0.070(2) Uani 1 1 d . . . . .
N7 N 0.8500(14) -0.1092(10) 0.0517(7) 0.070(2) Uani 1 1 d . . . . .
O1 O -0.3222(14) 0.4000(9) 0.5668(7) 0.087(3) Uani 1 1 d . . . . .
O2 O 0.3566(13) 0.8852(9) 0.6372(7) 0.079(2) Uani 1 1 d . . . . .
O3 O 0.2398(12) 0.9191(9) 0.5003(7) 0.077(2) Uani 1 1 d . . . . .
O4 O 0.5372(11) 0.8534(8) 0.4752(7) 0.074(2) Uani 1 1 d . . . . .
O5 O 1.0169(12) -0.1670(9) 0.0111(7) 0.080(2) Uani 1 1 d . . . . .
O6 O 0.7288(15) -0.1184(14) 0.0122(8) 0.109(4) Uani 1 1 d . . . . .
O7 O 0.8075(13) -0.0449(10) 0.1372(7) 0.085(3) Uani 1 1 d . . . . .
O8 O 0.0398(12) 1.1827(9) 0.5563(7) 0.076(2) Uani 1 1 d D . . . .
H8A H 0.088(19) 1.102(5) 0.538(12) 0.114 Uiso 1 1 d D U . . .
H8B H -0.047(15) 1.216(12) 0.528(11) 0.114 Uiso 1 1 d D 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 N2 2.014(10) . ?
Pd1 N5 2.031(8) 2_566 ?
Pd1 N3 2.060(10) . ?
Pd1 N1 2.086(9) . ?
C1 C2 1.385(16) . ?
C1 C6 1.392(15) . ?
C1 N1 1.424(14) . ?
C2 C3 1.384(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(15) . ?
C3 N4 1.411(13) . ?
C4 C5 1.378(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(17) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O1 1.218(13) . ?
C7 N4 1.358(14) . ?
C7 C9 1.494(15) . ?
C8 N5 1.353(13) . ?
C8 C9 1.372(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(15) . ?
C10 C11 1.384(15) . ?
C10 H10 0.9500 . ?
C11 C12 1.346(15) . ?
C11 H11 0.9500 . ?
C12 N5 1.326(13) . ?
C12 H12 0.9500 . ?
C13 N2 1.447(15) . ?
C13 C14 1.522(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N3 1.521(17) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 H2A 0.88(2) . ?
N2 H2B 0.88(2) . ?
N3 H3A 0.93(15) . ?
N3 H3B 0.91(13) . ?
N4 H4N 0.8800 . ?
N6 O2 1.241(13) . ?
N6 O4 1.257(13) . ?
N6 O3 1.266(12) . ?
N7 O6 1.206(12) . ?
N7 O7 1.246(12) . ?
N7 O5 1.263(12) . ?
O8 H8A 0.85(2) . ?
O8 H8B 0.84(2) . ?

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 Pd1 N5 89.6(4) . 2_566 ?
N2 Pd1 N3 84.5(4) . . ?
N5 Pd1 N3 173.4(3) 2_566 . ?
N2 Pd1 N1 176.0(3) . . ?
N5 Pd1 N1 94.3(3) 2_566 . ?
N3 Pd1 N1 91.5(4) . . ?
C2 C1 C6 121.0(10) . . ?
C2 C1 N1 120.0(10) . . ?
C6 C1 N1 118.9(10) . . ?
C3 C2 C1 119.8(10) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.8(10) . . ?
C2 C3 N4 123.6(10) . . ?
C4 C3 N4 116.6(9) . . ?
C5 C4 C3 120.7(11) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.0(11) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 118.6(10) . . ?
C1 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
O1 C7 N4 124.0(10) . . ?
O1 C7 C9 120.7(10) . . ?
N4 C7 C9 115.3(9) . . ?
N5 C8 C9 122.3(9) . . ?
N5 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 118.0(9) . . ?
C8 C9 C7 122.6(9) . . ?
C10 C9 C7 119.4(9) . . ?
C11 C10 C9 118.7(10) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C12 C11 C10 119.2(10) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N5 C12 C11 123.6(10) . . ?
N5 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
N2 C13 C14 110.8(10) . . ?
N2 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N3 C14 C13 106.3(9) . . ?
N3 C14 H14A 110.5 . . ?
C13 C14 H14A 110.5 . . ?
N3 C14 H14B 110.5 . . ?
C13 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
C1 N1 Pd1 117.6(7) . . ?
C1 N1 H1A 107.9 . . ?
Pd1 N1 H1A 107.9 . . ?
C1 N1 H1B 107.9 . . ?
Pd1 N1 H1B 107.9 . . ?
H1A N1 H1B 107.2 . . ?
C13 N2 Pd1 110.8(7) . . ?
C13 N2 H2A 116(10) . . ?
Pd1 N2 H2A 111(9) . . ?
C13 N2 H2B 106(9) . . ?
Pd1 N2 H2B 110(9) . . ?
H2A N2 H2B 103(10) . . ?
C14 N3 Pd1 103.5(7) . . ?
C14 N3 H3A 101(8) . . ?
Pd1 N3 H3A 118(9) . . ?
C14 N3 H3B 115(8) . . ?
Pd1 N3 H3B 111(8) . . ?
H3A N3 H3B 109(10) . . ?
C7 N4 C3 127.5(9) . . ?
C7 N4 H4N 116.3 . . ?
C3 N4 H4N 116.3 . . ?
C12 N5 C8 118.3(9) . . ?
C12 N5 Pd1 121.0(7) . 2_566 ?
C8 N5 Pd1 120.7(7) . 2_566 ?
O2 N6 O4 121.4(10) . . ?
O2 N6 O3 119.5(11) . . ?
O4 N6 O3 119.0(10) . . ?
O6 N7 O7 118.7(11) . . ?
O6 N7 O5 121.8(10) . . ?
O7 N7 O5 119.5(9) . . ?
H8A O8 H8B 111(4) . . ?

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
C6 C1 C2 C3 1.2(16) . . . . ?
N1 C1 C2 C3 176.1(9) . . . . ?
C1 C2 C3 C4 -0.6(16) . . . . ?
C1 C2 C3 N4 -177.7(10) . . . . ?
C2 C3 C4 C5 0.1(16) . . . . ?
N4 C3 C4 C5 177.3(11) . . . . ?
C3 C4 C5 C6 -0.1(18) . . . . ?
C2 C1 C6 C5 -1.1(16) . . . . ?
N1 C1 C6 C5 -176.2(10) . . . . ?
C4 C5 C6 C1 0.6(17) . . . . ?
N5 C8 C9 C10 -1.5(15) . . . . ?
N5 C8 C9 C7 -179.3(9) . . . . ?
O1 C7 C9 C8 154.0(11) . . . . ?
N4 C7 C9 C8 -23.3(14) . . . . ?
O1 C7 C9 C10 -23.8(15) . . . . ?
N4 C7 C9 C10 158.9(10) . . . . ?
C8 C9 C10 C11 1.8(15) . . . . ?
C7 C9 C10 C11 179.7(10) . . . . ?
C9 C10 C11 C12 -1.4(17) . . . . ?
C10 C11 C12 N5 0.7(18) . . . . ?
N2 C13 C14 N3 -50.4(14) . . . . ?
C2 C1 N1 Pd1 -84.9(11) . . . . ?
C6 C1 N1 Pd1 90.1(10) . . . . ?
C14 C13 N2 Pd1 25.1(13) . . . . ?
C13 C14 N3 Pd1 49.2(11) . . . . ?
O1 C7 N4 C3 -1.2(18) . . . . ?
C9 C7 N4 C3 175.9(10) . . . . ?
C2 C3 N4 C7 -6.1(17) . . . . ?
C4 C3 N4 C7 176.8(10) . . . . ?
C11 C12 N5 C8 -0.4(17) . . . . ?
C11 C12 N5 Pd1 -179.3(9) . . . 2_566 ?
C9 C8 N5 C12 0.8(15) . . . . ?
C9 C8 N5 Pd1 179.7(7) . . . 2_566 ?

_refine_diff_density_max         1.153
_refine_diff_density_min         -2.096
_refine_diff_density_rms         0.193



# start Validation Reply Form
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Pd1       1.68 eA-3  
RESPONSE: The electron density does not correspond to any unaccounted atom
types and PLATON does not suggest the presence of twinning in the 
structure. This alert is possibly due to Fourier truncation error. 
;
# end Validation Reply Form
