# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_[Pd(H-2L2)](H2O)6
_database_code_depnum_ccdc_archive 'CCDC 2045688'
loop_
_audit_author_name
_audit_author_address
'Patrizia Rossi'
;University of Firenze
Italy
;
_audit_update_record             
;
2021-05-27 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT417_PdH-2L2H2O6         
;
PROBLEM: Short Inter D-H..H-D H4W2 ..H5W2 . 2.05 Ang.
RESPONSE: The molecules to which H4W2 and H5w2 belong are part
 of a net of  water molecules connected by H-bonds
;



_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            'C24 H34 N2 O12 Pd'
_chemical_formula_weight         648.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   13.8990(5)
_cell_length_b                   9.2755(5)
_cell_length_c                   20.2093(19)
_cell_angle_alpha                90
_cell_angle_beta                 100.880(5)
_cell_angle_gamma                90
_cell_volume                     2558.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6400
_cell_measurement_theta_min      4.4320
_cell_measurement_theta_max      72.2660

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    6.468
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.28586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            19062
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.264
_diffrn_reflns_theta_max         72.480
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5059
_reflns_number_gt                3738
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2004, (Burla, 2005)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'PARST97 (Nardelli, 1995)'
_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)+(0.0593P)²+10.0468P] 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         5059
_refine_ls_number_parameters     388
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1498
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.061
_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
Pd1 Pd 0.36393(4) 0.18120(5) 0.69205(2) 0.02159(16) Uani 1 1 d . . . . .
O1 O 0.4248(3) 0.2557(4) 0.7836(2) 0.0264(10) Uani 1 1 d . . . . .
O2 O 0.3459(3) 0.0159(4) 0.9067(2) 0.0254(10) Uani 1 1 d . . . . .
O3 O 0.4847(4) 0.4011(5) 0.8974(2) 0.0334(12) Uani 1 1 d . . . . .
O4 O 0.3884(3) 0.3772(4) 0.6557(2) 0.0239(10) Uani 1 1 d . . . . .
O5 O 0.3590(3) 0.3365(4) 0.4738(2) 0.0254(10) Uani 1 1 d . . . . .
O6 O 0.4202(4) 0.6496(4) 0.6174(2) 0.0296(11) Uani 1 1 d . . . . .
N1 N 0.3453(4) -0.0183(5) 0.7300(2) 0.0203(11) Uani 1 1 d . . . . .
N2 N 0.3018(4) 0.1024(5) 0.6000(2) 0.0217(12) Uani 1 1 d . . . . .
C1 C 0.2789(5) -0.0981(6) 0.6748(3) 0.0277(16) Uani 1 1 d . . . . .
H1A H 0.286686 -0.203216 0.682378 0.033 Uiso 1 1 calc R U . . .
H1B H 0.209863 -0.072479 0.675165 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3007(5) -0.0141(7) 0.7898(3) 0.0261(15) Uani 1 1 d . . . . .
H2A H 0.294313 -0.113840 0.805858 0.031 Uiso 1 1 calc R U . . .
H2B H 0.234005 0.027049 0.777448 0.031 Uiso 1 1 calc R U . . .
C3 C 0.3587(5) 0.0737(7) 0.8463(3) 0.0261(15) Uani 1 1 d . . . . .
C4 C 0.4076(5) 0.1976(6) 0.8407(3) 0.0236(14) Uani 1 1 d . . . . .
C5 C 0.4455(5) 0.2825(6) 0.9018(3) 0.0255(15) Uani 1 1 d . . . . .
C6 C 0.4273(5) 0.2222(6) 0.9645(3) 0.0226(14) Uani 1 1 d . . . . .
C7 C 0.4540(5) 0.2943(7) 1.0262(3) 0.0249(14) Uani 1 1 d . . . . .
H7 H 0.485424 0.385528 1.027281 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4358(5) 0.2360(7) 1.0848(3) 0.0306(16) Uani 1 1 d . . . . .
H8 H 0.453177 0.287446 1.125994 0.037 Uiso 1 1 calc R U . . .
C9 C 0.3916(5) 0.1003(8) 1.0838(3) 0.0297(16) Uani 1 1 d . . . . .
H9 H 0.381256 0.058482 1.124846 0.036 Uiso 1 1 calc R U . . .
C10 C 0.3628(5) 0.0268(7) 1.0245(3) 0.0291(16) Uani 1 1 d . . . . .
H10 H 0.331552 -0.064420 1.023810 0.035 Uiso 1 1 calc R U . . .
C11 C 0.3808(5) 0.0895(6) 0.9650(3) 0.0256(15) Uani 1 1 d . . . . .
C12 C 0.4435(5) -0.0924(7) 0.7459(3) 0.0310(16) Uani 1 1 d . . . . .
H12A H 0.472800 -0.094638 0.705418 0.046 Uiso 1 1 calc R U . . .
H12B H 0.486748 -0.039567 0.781681 0.046 Uiso 1 1 calc R U . . .
H12C H 0.434866 -0.191233 0.760899 0.046 Uiso 1 1 calc R U . . .
C13 C 0.3039(5) -0.0592(7) 0.6081(3) 0.0265(15) Uani 1 1 d . . . . .
H13A H 0.256124 -0.103948 0.571302 0.032 Uiso 1 1 calc R U . . .
H13B H 0.369952 -0.096181 0.605535 0.032 Uiso 1 1 calc R U . . .
C14 C 0.3609(5) 0.1436(6) 0.5494(3) 0.0253(15) Uani 1 1 d . . . . .
H14A H 0.331916 0.099655 0.505542 0.030 Uiso 1 1 calc R U . . .
H14B H 0.428058 0.104987 0.563315 0.030 Uiso 1 1 calc R U . . .
C15 C 0.3659(5) 0.3042(7) 0.5412(3) 0.0245(14) Uani 1 1 d . . . . .
C16 C 0.3835(5) 0.4058(7) 0.5906(3) 0.0262(15) Uani 1 1 d . . . . .
C17 C 0.3977(5) 0.5558(6) 0.5735(3) 0.0253(15) Uani 1 1 d . . . . .
C18 C 0.3875(5) 0.5864(6) 0.5012(3) 0.0225(14) Uani 1 1 d . . . . .
C19 C 0.3968(5) 0.7266(7) 0.4766(3) 0.0264(15) Uani 1 1 d . . . . .
H19 H 0.411340 0.804414 0.507416 0.032 Uiso 1 1 calc R U . . .
C20 C 0.3852(5) 0.7523(7) 0.4088(3) 0.0291(16) Uani 1 1 d . . . . .
H20 H 0.389582 0.847793 0.392685 0.035 Uiso 1 1 calc R U . . .
C21 C 0.3668(5) 0.6372(7) 0.3634(3) 0.0288(16) Uani 1 1 d . . . . .
H21 H 0.360363 0.654852 0.316482 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3581(5) 0.5003(7) 0.3857(3) 0.0267(15) Uani 1 1 d . . . . .
H22 H 0.344973 0.422729 0.354646 0.032 Uiso 1 1 calc R U . . .
C23 C 0.3687(5) 0.4755(7) 0.4542(3) 0.0245(14) Uani 1 1 d . . . . .
C24 C 0.1976(5) 0.1513(7) 0.5786(3) 0.0283(16) Uani 1 1 d . . . . .
H24A H 0.159762 0.122961 0.612802 0.042 Uiso 1 1 calc R U . . .
H24B H 0.195962 0.256408 0.573666 0.042 Uiso 1 1 calc R U . . .
H24C H 0.169188 0.106444 0.535459 0.042 Uiso 1 1 calc R U . . .
O1W O 0.6326(4) 1.2226(6) 0.8087(3) 0.0470(14) Uani 1 1 d D . . . .
H1W1 H 0.639(5) 1.149(6) 0.786(4) 0.056 Uiso 1 1 d D U . . .
H1W2 H 0.5712(10) 1.225(9) 0.798(4) 0.056 Uiso 1 1 d D U . . .
O2W O 0.4775(4) 0.5561(5) 0.7671(2) 0.0328(12) Uani 1 1 d D . . . .
H2W1 H 0.470(6) 0.527(6) 0.7275(10) 0.039 Uiso 1 1 d D U . . .
H2W2 H 0.486(6) 0.475(3) 0.785(3) 0.039 Uiso 1 1 d D U . . .
O3W O 0.7601(4) 0.9232(6) 0.6053(3) 0.0441(14) Uani 1 1 d D . . . .
H3W1 H 0.785(5) 0.992(5) 0.630(3) 0.053 Uiso 1 1 d D U . . .
H3W2 H 0.800(5) 0.861(5) 0.624(4) 0.053 Uiso 1 1 d D U . . .
O4W O 0.6729(4) 0.9537(7) 0.7495(3) 0.0474(14) Uani 1 1 d D . . . .
H4W1 H 0.708(5) 0.991(9) 0.724(3) 0.057 Uiso 1 1 d D U . . .
H4W2 H 0.637(5) 0.909(8) 0.718(2) 0.057 Uiso 1 1 d D U . . .
O5W O 0.6737(4) 0.6287(6) 0.7811(3) 0.0417(13) Uani 1 1 d D . . . .
H5W1 H 0.6123(12) 0.617(7) 0.776(4) 0.050 Uiso 1 1 d D U . . .
H5W2 H 0.668(5) 0.713(4) 0.764(4) 0.050 Uiso 1 1 d D U . . .
O6W O 0.5632(4) 0.8840(6) 0.6193(3) 0.0419(13) Uani 1 1 d D . . . .
H6W1 H 0.545(5) 0.797(3) 0.616(4) 0.050 Uiso 1 1 d D U . . .
H6W2 H 0.620(2) 0.868(7) 0.612(4) 0.050 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 O1 2.006(4) . ?
Pd1 O4 2.014(4) . ?
Pd1 N2 2.033(5) . ?
Pd1 N1 2.038(5) . ?
O1 C4 1.336(8) . ?
O2 C11 1.370(7) . ?
O2 C3 1.375(8) . ?
O3 C5 1.237(8) . ?
O4 C16 1.331(8) . ?
O5 C23 1.363(7) . ?
O5 C15 1.381(7) . ?
O6 C17 1.240(7) . ?
N1 C2 1.460(8) . ?
N1 C1 1.501(7) . ?
N1 C12 1.508(8) . ?
N2 C14 1.477(9) . ?
N2 C24 1.500(8) . ?
N2 C13 1.508(8) . ?
C1 C13 1.499(9) . ?
C2 C3 1.506(8) . ?
C3 C4 1.351(9) . ?
C4 C5 1.475(8) . ?
C5 C6 1.450(9) . ?
C6 C11 1.391(9) . ?
C6 C7 1.402(8) . ?
C7 C8 1.370(9) . ?
C8 C9 1.400(10) . ?
C9 C10 1.371(9) . ?
C10 C11 1.400(9) . ?
C14 C15 1.502(8) . ?
C15 C16 1.361(9) . ?
C16 C17 1.456(9) . ?
C17 C18 1.468(9) . ?
C18 C23 1.392(8) . ?
C18 C19 1.407(9) . ?
C19 C20 1.370(9) . ?
C20 C21 1.399(9) . ?
C21 C22 1.360(9) . ?
C22 C23 1.382(8) . ?

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
O1 Pd1 O4 87.40(17) . . ?
O1 Pd1 N2 179.02(19) . . ?
O4 Pd1 N2 93.58(18) . . ?
O1 Pd1 N1 91.58(18) . . ?
O4 Pd1 N1 177.6(2) . . ?
N2 Pd1 N1 87.44(19) . . ?
C4 O1 Pd1 123.0(4) . . ?
C11 O2 C3 119.0(5) . . ?
C16 O4 Pd1 124.1(4) . . ?
C23 O5 C15 120.0(5) . . ?
C2 N1 C1 109.3(5) . . ?
C2 N1 C12 110.1(5) . . ?
C1 N1 C12 109.8(5) . . ?
C2 N1 Pd1 113.0(4) . . ?
C1 N1 Pd1 105.8(3) . . ?
C12 N1 Pd1 108.7(4) . . ?
C14 N2 C24 110.8(5) . . ?
C14 N2 C13 109.3(5) . . ?
C24 N2 C13 109.3(5) . . ?
C14 N2 Pd1 110.1(4) . . ?
C24 N2 Pd1 112.0(4) . . ?
C13 N2 Pd1 105.2(4) . . ?
C13 C1 N1 109.6(5) . . ?
N1 C2 C3 113.1(6) . . ?
C4 C3 O2 123.9(5) . . ?
C4 C3 C2 127.0(6) . . ?
O2 C3 C2 108.8(5) . . ?
O1 C4 C3 126.2(5) . . ?
O1 C4 C5 114.5(5) . . ?
C3 C4 C5 119.3(6) . . ?
O3 C5 C6 123.8(5) . . ?
O3 C5 C4 120.5(6) . . ?
C6 C5 C4 115.6(5) . . ?
C11 C6 C7 117.4(6) . . ?
C11 C6 C5 120.4(5) . . ?
C7 C6 C5 122.1(6) . . ?
C8 C7 C6 121.3(6) . . ?
C7 C8 C9 119.7(6) . . ?
C10 C9 C8 120.9(6) . . ?
C9 C10 C11 118.3(6) . . ?
O2 C11 C6 121.6(6) . . ?
O2 C11 C10 116.1(6) . . ?
C6 C11 C10 122.2(6) . . ?
C1 C13 N2 109.5(5) . . ?
N2 C14 C15 112.1(5) . . ?
C16 C15 O5 122.9(6) . . ?
C16 C15 C14 127.7(6) . . ?
O5 C15 C14 109.2(5) . . ?
O4 C16 C15 123.7(6) . . ?
O4 C16 C17 116.2(5) . . ?
C15 C16 C17 120.1(6) . . ?
O6 C17 C16 121.9(6) . . ?
O6 C17 C18 122.7(6) . . ?
C16 C17 C18 115.4(5) . . ?
C23 C18 C19 117.4(6) . . ?
C23 C18 C17 120.5(6) . . ?
C19 C18 C17 122.2(6) . . ?
C20 C19 C18 120.9(6) . . ?
C19 C20 C21 119.7(6) . . ?
C22 C21 C20 120.8(6) . . ?
C21 C22 C23 119.2(6) . . ?
O5 C23 C22 116.8(6) . . ?
O5 C23 C18 121.1(5) . . ?
C22 C23 C18 122.1(6) . . ?

_refine_diff_density_max         0.943
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.144

