# Supplementary Information (SI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2360175'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Florence
Italy
;
_audit_update_record             
;
2024-06-17 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;

_publ_section_title_             
;
A combined solid state, solution and DFT study of 
a dimethyl-cyclen-Pd(II) complex
;


_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            'C22 H32 Cl2 N4 O14 Pd'
_chemical_formula_weight         753.81

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'
Cl Cl 0.3639 0.7018 '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      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                   19.6006(9)
_cell_length_b                   9.2491(4)
_cell_length_c                   17.4562(12)
_cell_angle_alpha                90
_cell_angle_beta                 119.8500(10)
_cell_angle_gamma                90
_cell_volume                     2744.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9627
_cell_measurement_theta_min      5.31
_cell_measurement_theta_max      71.80

_exptl_crystal_description       prism'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    7.961
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_process_details   'SADABS-2016/2, Sheldrick 2015'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21120
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         5.203
_diffrn_reflns_theta_max         72.482
_diffrn_reflns_theta_full        67.679
_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             2719
_reflns_number_gt                2698
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SR/2014 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0554P)²+22.9716P] 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         2719
_refine_ls_number_parameters     198
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1111
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Cl1 Cl 0.64735(5) 0.17783(9) 0.15259(5) 0.0135(2) Uani 1 1 d . . . . .
O11 O 0.70986(19) 0.1607(4) 0.24248(19) 0.0286(7) Uani 1 1 d . . . . .
O12 O 0.57206(18) 0.1702(3) 0.1490(2) 0.0255(7) Uani 1 1 d . . . . .
O13 O 0.65587(19) 0.3146(3) 0.1188(2) 0.0228(6) Uani 1 1 d . . . . .
O14 O 0.65167(17) 0.0624(3) 0.09896(18) 0.0192(6) Uani 1 1 d . . . . .
Pd1 Pd 0.500000 0.68982(3) 0.250000 0.01057(14) Uani 1 2 d S T P . .
O1 O 0.59067(16) 0.3856(3) 0.27027(17) 0.0185(6) Uani 1 1 d D . . . .
H1O H 0.572(3) 0.306(3) 0.247(3) 0.028 Uiso 1 1 d D U . . .
O2 O 0.58731(19) 0.1381(3) 0.3541(2) 0.0271(7) Uani 1 1 d . . . . .
O3 O 0.69977(15) 0.4931(3) 0.49907(16) 0.0166(5) Uani 1 1 d . . . . .
N1 N 0.61614(16) 0.7364(3) 0.33953(18) 0.0098(6) Uani 1 1 d . . . . .
N2 N 0.47520(16) 0.7279(3) 0.34880(18) 0.0097(6) Uani 1 1 d . . . . .
C1 C 0.6920(2) 0.3733(5) 0.5389(3) 0.0215(8) Uani 1 1 d . . . . .
H1 H 0.714588 0.374417 0.601336 0.026 Uiso 1 1 calc R U . . .
C2 C 0.6542(2) 0.2538(4) 0.4953(3) 0.0211(8) Uani 1 1 d . . . . .
H2 H 0.650656 0.173432 0.527027 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6186(2) 0.2457(4) 0.3998(3) 0.0185(8) Uani 1 1 d . . . . .
C4 C 0.6243(2) 0.3790(4) 0.3592(2) 0.0138(7) Uani 1 1 d . . . . .
C5 C 0.6651(2) 0.4934(4) 0.4082(2) 0.0131(7) Uani 1 1 d . . . . .
C6 C 0.6807(2) 0.6262(4) 0.3715(2) 0.0129(7) Uani 1 1 d . . . . .
H6A H 0.688638 0.598490 0.321659 0.015 Uiso 1 1 calc R U . . .
H6B H 0.730110 0.670796 0.417537 0.015 Uiso 1 1 calc R U . . .
C7 C 0.6145(2) 0.8044(4) 0.4169(2) 0.0136(7) Uani 1 1 d . . . . .
H7A H 0.649496 0.889964 0.436772 0.016 Uiso 1 1 calc R U . . .
H7B H 0.634947 0.734418 0.466316 0.016 Uiso 1 1 calc R U . . .
C8 C 0.5320(2) 0.8502(4) 0.3936(2) 0.0128(7) Uani 1 1 d . . . . .
H8A H 0.531454 0.878144 0.448043 0.015 Uiso 1 1 calc R U . . .
H8B H 0.515852 0.935152 0.353920 0.015 Uiso 1 1 calc R U . . .
C9 C 0.6310(2) 0.8470(4) 0.2854(2) 0.0123(7) Uani 1 1 d . . . . .
H9A H 0.687263 0.874341 0.316436 0.015 Uiso 1 1 calc R U . . .
H9B H 0.599558 0.935156 0.277943 0.015 Uiso 1 1 calc R U . . .
C10 C 0.3919(2) 0.7834(4) 0.3049(2) 0.0124(7) Uani 1 1 d . . . . .
H10A H 0.387262 0.858588 0.342452 0.015 Uiso 1 1 calc R U . . .
H10B H 0.355725 0.703323 0.297878 0.015 Uiso 1 1 calc R U . . .
C11 C 0.4857(2) 0.6115(4) 0.4121(2) 0.0151(7) Uani 1 1 d . . . . .
H11A H 0.447972 0.533686 0.380967 0.023 Uiso 1 1 calc R U . . .
H11B H 0.539372 0.573187 0.438637 0.023 Uiso 1 1 calc R U . . .
H11C H 0.476828 0.650528 0.458595 0.023 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
Cl1 O13 1.440(3) . ?
Cl1 O11 1.440(3) . ?
Cl1 O12 1.447(3) . ?
Cl1 O14 1.450(3) . ?
Pd1 N2 2.042(3) . ?
Pd1 N2 2.042(3) 2_655 ?
Pd1 N1 2.066(3) 2_655 ?
Pd1 N1 2.066(3) . ?
O1 C4 1.353(4) . ?
O1 H1O 0.837(10) . ?
O2 C3 1.232(5) . ?
O3 C1 1.357(5) . ?
O3 C5 1.379(4) . ?
N1 C6 1.500(4) . ?
N1 C7 1.504(4) . ?
N1 C9 1.516(4) . ?
N2 C11 1.482(4) . ?
N2 C8 1.505(4) . ?
N2 C10 1.507(4) . ?
C1 C2 1.337(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.453(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.454(5) . ?
C4 C5 1.345(5) . ?
C5 C6 1.486(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.518(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.526(5) 2_655 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
O13 Cl1 O11 109.50(19) . . ?
O13 Cl1 O12 110.40(19) . . ?
O11 Cl1 O12 109.77(19) . . ?
O13 Cl1 O14 109.05(17) . . ?
O11 Cl1 O14 109.32(18) . . ?
O12 Cl1 O14 108.77(17) . . ?
N2 Pd1 N2 160.13(16) . 2_655 ?
N2 Pd1 N1 88.12(11) . 2_655 ?
N2 Pd1 N1 87.76(11) 2_655 2_655 ?
N2 Pd1 N1 87.76(11) . . ?
N2 Pd1 N1 88.12(11) 2_655 . ?
N1 Pd1 N1 155.94(16) 2_655 . ?
C4 O1 H1O 111(4) . . ?
C1 O3 C5 118.3(3) . . ?
C6 N1 C7 110.0(3) . . ?
C6 N1 C9 107.6(3) . . ?
C7 N1 C9 111.9(3) . . ?
C6 N1 Pd1 123.2(2) . . ?
C7 N1 Pd1 105.0(2) . . ?
C9 N1 Pd1 98.62(19) . . ?
C11 N2 C8 111.5(3) . . ?
C11 N2 C10 109.9(3) . . ?
C8 N2 C10 110.0(3) . . ?
C11 N2 Pd1 120.1(2) . . ?
C8 N2 Pd1 98.22(19) . . ?
C10 N2 Pd1 106.4(2) . . ?
C2 C1 O3 123.7(4) . . ?
C2 C1 H1 118.2 . . ?
O3 C1 H1 118.2 . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
O2 C3 C2 125.9(4) . . ?
O2 C3 C4 120.2(4) . . ?
C2 C3 C4 113.9(3) . . ?
C5 C4 O1 119.4(3) . . ?
C5 C4 C3 121.5(3) . . ?
O1 C4 C3 119.1(3) . . ?
C4 C5 O3 121.8(3) . . ?
C4 C5 C6 124.0(3) . . ?
O3 C5 C6 114.1(3) . . ?
C5 C6 N1 113.9(3) . . ?
C5 C6 H6A 108.8 . . ?
N1 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
N1 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
N1 C7 C8 111.9(3) . . ?
N1 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N2 C8 C7 110.1(3) . . ?
N2 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
N1 C9 C10 109.6(3) . 2_655 ?
N1 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 2_655 . ?
N1 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 2_655 . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 110.1(3) . 2_655 ?
N2 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 2_655 . ?
N2 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 2_655 . ?
H10A C10 H10B 108.2 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         0.698
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.142


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
