# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_mo_jva181026Pd1
_database_code_depnum_ccdc_archive 'CCDC 2241934'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2023-02-14 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;

_audit_creation_method           'APEX3 v2016.5-0'
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H36 N4 O6 Pd2'
_chemical_formula_sum            'C26 H36 N4 O6 Pd2'
_chemical_formula_weight         713.39

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'
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           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                   18.3312(13)
_cell_length_b                   11.1332(7)
_cell_length_c                   15.7306(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.275(2)
_cell_angle_gamma                90
_cell_volume                     2991.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    39827
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       ' plate'
_exptl_crystal_colour            'fluorescent yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.615
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            38675
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.184
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3447
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_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)+(0.0202P)²+6.5133P] 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         3447
_refine_ls_number_parameters     180
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0533
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_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 0.42363(2) 0.77914(2) 0.67529(2) 0.01430(6) Uani 1 1 d . . . . .
O1 O 0.31738(11) 0.65562(19) 0.94513(13) 0.0308(5) Uani 1 1 d . . . . .
N1 N 0.42884(12) 0.6642(2) 0.57463(14) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.37104(14) 0.6411(2) 0.70609(17) 0.0175(5) Uani 1 1 d . . . . .
O2 O 0.39786(10) 0.89319(16) 0.76367(12) 0.0190(4) Uani 1 1 d . . . . .
H2 H 0.2068(18) 0.493(3) 0.813(2) 0.022(8) Uiso 1 1 d . . . . .
N2 N 0.24353(13) 0.5364(2) 0.82895(16) 0.0222(5) Uani 1 1 d . . . . .
C2 C 0.38173(15) 0.5330(2) 0.66688(18) 0.0208(5) Uani 1 1 d . . . . .
C3 C 0.34755(17) 0.4280(2) 0.6820(2) 0.0279(6) Uani 1 1 d . . . . .
H3 H 0.354152 0.355081 0.654206 0.034 Uiso 1 1 calc R U . . .
O3 O 0.51877(10) 0.92340(16) 0.86626(12) 0.0216(4) Uani 1 1 d . . . . .
C4 C 0.30378(16) 0.4294(2) 0.73768(19) 0.0268(6) Uani 1 1 d . . . . .
H4 H 0.281482 0.357084 0.749342 0.032 Uiso 1 1 calc R U . . .
C5 C 0.29257(14) 0.5366(2) 0.77638(17) 0.0199(5) Uani 1 1 d . . . . .
C6 C 0.32598(14) 0.6422(2) 0.76045(17) 0.0175(5) Uani 1 1 d . . . . .
H6 H 0.317951 0.715400 0.786845 0.021 Uiso 1 1 calc R U . . .
C9 C 0.49592(16) 0.6840(3) 0.54452(19) 0.0258(6) Uani 1 1 d . . . . .
H9A H 0.493998 0.624938 0.497553 0.039 Uiso 1 1 calc R U . . .
H9B H 0.545098 0.674896 0.596751 0.039 Uiso 1 1 calc R U . . .
H9C H 0.492926 0.765177 0.519398 0.039 Uiso 1 1 calc R U . . .
C8 C 0.35506(16) 0.6809(3) 0.49452(18) 0.0263(6) Uani 1 1 d . . . . .
H8A H 0.355427 0.628060 0.444840 0.039 Uiso 1 1 calc R U . . .
H8B H 0.350958 0.764676 0.474214 0.039 Uiso 1 1 calc R U . . .
H8C H 0.310217 0.660900 0.511743 0.039 Uiso 1 1 calc R U . . .
C7 C 0.43256(16) 0.5386(2) 0.61037(18) 0.0227(6) Uani 1 1 d . . . . .
H7A H 0.487222 0.517500 0.648158 0.027 Uiso 1 1 calc R U . . .
H7B H 0.413533 0.480924 0.559072 0.027 Uiso 1 1 calc R U . . .
C10 C 0.25800(15) 0.5960(2) 0.90865(18) 0.0226(6) Uani 1 1 d . . . . .
C11 C 0.19649(17) 0.5808(3) 0.9508(2) 0.0305(7) Uani 1 1 d . . . . .
H11A H 0.184836 0.659044 0.971462 0.046 Uiso 1 1 calc R U . . .
H11B H 0.215992 0.525978 1.002962 0.046 Uiso 1 1 calc R U . . .
H11C H 0.148737 0.547530 0.905363 0.046 Uiso 1 1 calc R U . . .
C12 C 0.44702(14) 0.9437(2) 0.83324(17) 0.0191(5) Uani 1 1 d . . . . .
C13 C 0.41451(19) 1.0371(3) 0.8792(2) 0.0458(9) Uani 1 1 d . . . . .
H13A H 0.422603 1.117223 0.858316 0.069 Uiso 1 1 calc R U . . .
H13B H 0.441412 1.031664 0.945426 0.069 Uiso 1 1 calc R U . . .
H13C H 0.358366 1.023171 0.863608 0.069 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 C1 1.966(2) . ?
Pd1 O2 2.0603(17) . ?
Pd1 N1 2.065(2) . ?
Pd1 O3 2.1500(17) 2_656 ?
Pd1 Pd1 2.9304(4) 2_656 ?
O1 C10 1.226(3) . ?
N1 C9 1.486(3) . ?
N1 C8 1.488(3) . ?
N1 C7 1.500(3) . ?
C1 C6 1.388(3) . ?
C1 C2 1.398(4) . ?
O2 C12 1.269(3) . ?
N2 C10 1.356(3) . ?
N2 C5 1.425(3) . ?
N2 H2 0.79(3) . ?
C2 C3 1.387(4) . ?
C2 C7 1.504(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
O3 C12 1.247(3) . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C6 H6 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C10 C11 1.511(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.507(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
C1 Pd1 O2 93.59(9) . . ?
C1 Pd1 N1 82.40(9) . . ?
O2 Pd1 N1 170.10(7) . . ?
C1 Pd1 O3 176.12(9) . 2_656 ?
O2 Pd1 O3 90.17(7) . 2_656 ?
N1 Pd1 O3 93.74(8) . 2_656 ?
C1 Pd1 Pd1 102.33(7) . 2_656 ?
O2 Pd1 Pd1 81.09(5) . 2_656 ?
N1 Pd1 Pd1 108.58(6) . 2_656 ?
O3 Pd1 Pd1 79.18(5) 2_656 2_656 ?
C9 N1 C8 108.3(2) . . ?
C9 N1 C7 109.1(2) . . ?
C8 N1 C7 109.7(2) . . ?
C9 N1 Pd1 115.25(16) . . ?
C8 N1 Pd1 106.95(16) . . ?
C7 N1 Pd1 107.39(15) . . ?
C6 C1 C2 119.3(2) . . ?
C6 C1 Pd1 126.81(19) . . ?
C2 C1 Pd1 113.85(18) . . ?
C12 O2 Pd1 126.17(16) . . ?
C10 N2 C5 125.6(2) . . ?
C10 N2 H2 117(2) . . ?
C5 N2 H2 117(2) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 C7 123.5(2) . . ?
C1 C2 C7 116.2(2) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C12 O3 Pd1 124.68(16) . 2_656 ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 N2 118.6(2) . . ?
C6 C5 N2 121.2(2) . . ?
C1 C6 C5 120.2(2) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C7 C2 107.8(2) . . ?
N1 C7 H7A 110.1 . . ?
C2 C7 H7A 110.1 . . ?
N1 C7 H7B 110.1 . . ?
C2 C7 H7B 110.1 . . ?
H7A C7 H7B 108.5 . . ?
O1 C10 N2 122.7(2) . . ?
O1 C10 C11 122.2(3) . . ?
N2 C10 C11 115.1(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 O2 126.2(2) . . ?
O3 C12 C13 117.8(2) . . ?
O2 C12 C13 116.0(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

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
N2 H2 O2 0.79(3) 2.17(3) 2.940(3) 166(3) 4_546

_refine_diff_density_max         0.720
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_jva210408Pd1
_database_code_depnum_ccdc_archive 'CCDC 2241935'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2023-02-14 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H28 F12 N4 O10 Pd4, 3(C4 H10 O)'
_chemical_formula_sum            'C42 H58 F12 N4 O13 Pd4'
_chemical_formula_weight         1480.52

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'
F F 0.0171 0.0103 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   22.9077(10)
_cell_length_b                   22.9077(10)
_cell_length_c                   23.8452(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10836.6(11)
_cell_formula_units_Z            9
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    58065
_cell_measurement_theta_min      1
_cell_measurement_theta_max      26.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_F_000             6606
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.135
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6399
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.857
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            47233
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.224
_diffrn_reflns_theta_max         26.486
_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             4987
_reflns_number_gt                3833
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_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)+(0.0596P)²+81.8462P] 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         4987
_refine_ls_number_parameters     274
_refine_ls_number_restraints     339
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1213
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.002
_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 0.58554(2) 0.64667(2) 0.59143(2) 0.02408(13) Uani 1 1 d . . . . .
H1 H 0.446(2) 0.4636(14) 0.664(2) 0.041(17) Uiso 1 1 d D . . . .
O1 O 0.56686(19) 0.60565(18) 0.66737(14) 0.0349(9) Uani 1 1 d . . . . .
N1 N 0.4731(2) 0.5051(2) 0.64863(17) 0.0300(10) Uani 1 1 d D . . . .
C1 C 0.4994(3) 0.5748(2) 0.5627(2) 0.0256(10) Uani 1 1 d . . . . .
Pd2 Pd 0.32089(2) 0.39234(2) 0.46382(2) 0.02757(13) Uani 1 1 d . . . . .
O2 O 0.68072(17) 0.72482(17) 0.62517(14) 0.0277(8) Uani 1 1 d . . . . .
N2 N 0.3312(2) 0.4734(2) 0.41796(19) 0.0365(11) Uani 1 1 d . . . . .
C2 C 0.4602(2) 0.5154(3) 0.5919(2) 0.0248(10) Uani 1 1 d . . . . .
C3 C 0.4044(3) 0.4593(3) 0.5665(2) 0.0260(10) Uani 1 1 d . . . . .
H3 H 0.378750 0.418580 0.586767 0.031 Uiso 1 1 calc R U . . .
O3 O 0.74932(19) 0.6877(2) 0.59288(16) 0.0369(9) Uani 1 1 d . . . . .
O4 O 0.30881(18) 0.31571(18) 0.51624(15) 0.0315(8) Uani 1 1 d . . . . .
C4 C 0.3878(3) 0.4648(3) 0.5112(2) 0.0264(10) Uani 1 1 d . . . . .
C5 C 0.4245(3) 0.5262(3) 0.4840(2) 0.0280(11) Uani 1 1 d . . . . .
O5 O 0.38823(17) 0.29535(18) 0.48085(14) 0.0284(8) Uani 1 1 d . . . . .
C6 C 0.4790(3) 0.5796(3) 0.5082(2) 0.0279(11) Uani 1 1 d . . . . .
H6 H 0.503530 0.620514 0.487887 0.033 Uiso 1 1 calc R U . . .
C7 C 0.5208(3) 0.5482(3) 0.6827(2) 0.0303(11) Uani 1 1 d . . . . .
C8 C 0.5210(3) 0.5289(3) 0.7417(2) 0.0431(15) Uani 1 1 d . . . . .
H8A H 0.494087 0.479761 0.745313 0.065 Uiso 1 1 calc R U . . .
H8B H 0.501765 0.549895 0.765494 0.065 Uiso 1 1 calc R U . . .
H8C H 0.567468 0.544180 0.753520 0.065 Uiso 1 1 calc R U . . .
C9 C 0.4032(3) 0.5269(3) 0.4240(2) 0.0332(12) Uani 1 1 d . . . . .
H9A H 0.408588 0.571549 0.414944 0.040 Uiso 1 1 calc R U . . .
H9B H 0.431687 0.518283 0.397924 0.040 Uiso 1 1 calc R U . . .
C10 C 0.2867(4) 0.4967(4) 0.4413(3) 0.0534(17) Uani 1 1 d . . . . .
H10A H 0.291668 0.535147 0.419358 0.080 Uiso 1 1 calc R U . . .
H10B H 0.299186 0.510576 0.480385 0.080 Uiso 1 1 calc R U . . .
H10C H 0.239783 0.460049 0.439625 0.080 Uiso 1 1 calc R U . . .
C11 C 0.3158(4) 0.4568(4) 0.3577(2) 0.0493(16) Uani 1 1 d . . . . .
H11A H 0.327645 0.498031 0.336658 0.074 Uiso 1 1 calc R U . . .
H11B H 0.267557 0.424657 0.353159 0.074 Uiso 1 1 calc R U . . .
H11C H 0.341937 0.436783 0.343415 0.074 Uiso 1 1 calc R U . . .
C13 C 0.7955(3) 0.7888(3) 0.6432(3) 0.0564(15) Uani 1 1 d D . . . .
C12 C 0.7361(3) 0.7267(3) 0.6180(2) 0.0327(11) Uani 1 1 d . . . . .
C15 C 0.3172(3) 0.2266(3) 0.5520(2) 0.0519(15) Uani 1 1 d D . . . .
C14 C 0.3412(3) 0.2855(3) 0.5125(2) 0.0287(11) Uani 1 1 d . . . . .
F1 F 0.8558(4) 0.7943(5) 0.6388(4) 0.0607(10) Uani 0.584(10) 1 d D U P A 1
F2 F 0.8016(4) 0.8457(3) 0.6262(4) 0.0607(10) Uani 0.584(10) 1 d D U P A 1
F3 F 0.7801(4) 0.7892(5) 0.7004(3) 0.0607(10) Uani 0.584(10) 1 d D U P A 1
F4 F 0.3579(6) 0.2004(6) 0.5537(5) 0.0715(11) Uani 0.399(5) 1 d D . P B 1
F5 F 0.2585(5) 0.1739(5) 0.5327(4) 0.0715(11) Uani 0.399(5) 1 d D . P B 1
F6 F 0.3100(7) 0.2422(6) 0.6042(4) 0.0715(11) Uani 0.399(5) 1 d D . P B 1
F1A F 0.8470(5) 0.7778(6) 0.6523(6) 0.0607(10) Uani 0.416(10) 1 d D U P A 2
F2A F 0.8145(5) 0.8391(5) 0.6026(5) 0.0607(10) Uani 0.416(10) 1 d D U P A 2
F3A F 0.7899(6) 0.8192(6) 0.6867(5) 0.0607(10) Uani 0.416(10) 1 d D U P A 2
F4A F 0.3259(5) 0.1778(4) 0.5327(3) 0.0715(11) Uani 0.601(5) 1 d D . P B 2
F5A F 0.2530(4) 0.2000(4) 0.5673(3) 0.0715(11) Uani 0.601(5) 1 d D . P B 2
F6A F 0.3512(4) 0.2448(4) 0.6010(3) 0.0715(11) Uani 0.601(5) 1 d D . P B 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 C1 1.956(5) . ?
Pd1 O1 1.986(4) . ?
Pd1 O5 2.073(3) 10_666 ?
Pd1 O2 2.169(3) . ?
Pd1 Pd2 3.0074(5) 10_666 ?
O1 C7 1.261(6) . ?
N1 C7 1.323(7) . ?
N1 C2 1.429(6) . ?
N1 H1 0.916(10) . ?
C1 C2 1.387(7) . ?
C1 C6 1.403(7) . ?
Pd2 C4 1.960(5) . ?
Pd2 O4 2.058(4) . ?
Pd2 N2 2.064(5) . ?
Pd2 O3 2.197(4) 10_666 ?
O2 C12 1.260(6) . ?
N2 C10 1.476(8) . ?
N2 C11 1.483(7) . ?
N2 C9 1.492(7) . ?
C2 C3 1.417(7) . ?
C3 C4 1.395(7) . ?
C3 H3 0.9500 . ?
O3 C12 1.233(6) . ?
O4 C14 1.244(6) . ?
C4 C5 1.386(7) . ?
C5 C6 1.365(7) . ?
C5 C9 1.513(7) . ?
O5 C14 1.241(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.476(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 F1 1.326(8) . ?
C13 F3A 1.292(8) . ?
C13 F2 1.305(7) . ?
C13 F1A 1.340(9) . ?
C13 F2A 1.399(8) . ?
C13 F3 1.410(7) . ?
C13 C12 1.516(8) . ?
C15 F4A 1.313(7) . ?
C15 F6 1.328(8) . ?
C15 F5A 1.330(7) . ?
C15 F4 1.338(8) . ?
C15 F6A 1.349(7) . ?
C15 F5 1.361(8) . ?
C15 C14 1.508(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
C1 Pd1 O1 91.91(18) . . ?
C1 Pd1 O5 95.46(18) . 10_666 ?
O1 Pd1 O5 170.47(14) . 10_666 ?
C1 Pd1 O2 178.55(18) . . ?
O1 Pd1 O2 86.68(14) . . ?
O5 Pd1 O2 85.98(13) 10_666 . ?
C1 Pd1 Pd2 99.53(14) . 10_666 ?
O1 Pd1 Pd2 106.01(12) . 10_666 ?
O5 Pd1 Pd2 78.75(10) 10_666 10_666 ?
O2 Pd1 Pd2 80.56(9) . 10_666 ?
C7 O1 Pd1 128.9(3) . . ?
C7 N1 C2 128.3(4) . . ?
C7 N1 H1 114(4) . . ?
C2 N1 H1 118(4) . . ?
C2 C1 C6 117.6(5) . . ?
C2 C1 Pd1 122.4(4) . . ?
C6 C1 Pd1 119.6(4) . . ?
C4 Pd2 O4 95.00(18) . . ?
C4 Pd2 N2 81.6(2) . . ?
O4 Pd2 N2 174.40(16) . . ?
C4 Pd2 O3 176.60(18) . 10_666 ?
O4 Pd2 O3 86.09(15) . 10_666 ?
N2 Pd2 O3 97.54(17) . 10_666 ?
C4 Pd2 Pd1 97.62(14) . 10_666 ?
O4 Pd2 Pd1 79.89(10) . 10_666 ?
N2 Pd2 Pd1 104.92(14) . 10_666 ?
O3 Pd2 Pd1 79.38(10) 10_666 10_666 ?
C12 O2 Pd1 123.9(3) . . ?
C10 N2 C11 109.8(5) . . ?
C10 N2 C9 110.2(5) . . ?
C11 N2 C9 109.1(5) . . ?
C10 N2 Pd2 109.7(4) . . ?
C11 N2 Pd2 112.2(4) . . ?
C9 N2 Pd2 105.7(3) . . ?
C1 C2 C3 121.5(5) . . ?
C1 C2 N1 123.5(5) . . ?
C3 C2 N1 115.0(4) . . ?
C4 C3 C2 119.0(5) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C12 O3 Pd2 124.2(3) . 10_666 ?
C14 O4 Pd2 124.5(3) . . ?
C5 C4 C3 118.7(5) . . ?
C5 C4 Pd2 114.2(4) . . ?
C3 C4 Pd2 127.0(4) . . ?
C6 C5 C4 121.9(5) . . ?
C6 C5 C9 123.0(5) . . ?
C4 C5 C9 114.8(5) . . ?
C14 O5 Pd1 124.7(3) . 10_666 ?
C5 C6 C1 120.9(5) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O1 C7 N1 123.3(5) . . ?
O1 C7 C8 117.6(5) . . ?
N1 C7 C8 119.2(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C5 108.1(4) . . ?
N2 C9 H9A 110.1 . . ?
C5 C9 H9A 110.1 . . ?
N2 C9 H9B 110.1 . . ?
C5 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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 . . ?
F1 C13 F2 107.2(7) . . ?
F3A C13 F1A 107.9(9) . . ?
F3A C13 F2A 100.6(8) . . ?
F1A C13 F2A 109.1(8) . . ?
F1 C13 F3 109.2(7) . . ?
F2 C13 F3 101.2(6) . . ?
F1 C13 C12 117.5(6) . . ?
F3A C13 C12 122.6(7) . . ?
F2 C13 C12 114.3(6) . . ?
F1A C13 C12 110.5(7) . . ?
F2A C13 C12 105.2(6) . . ?
F3 C13 C12 106.3(6) . . ?
O3 C12 O2 130.4(5) . . ?
O3 C12 C13 116.3(5) . . ?
O2 C12 C13 113.3(5) . . ?
F4A C15 F5A 108.1(7) . . ?
F6 C15 F4 107.5(9) . . ?
F4A C15 F6A 104.9(7) . . ?
F5A C15 F6A 103.8(6) . . ?
F6 C15 F5 110.9(8) . . ?
F4 C15 F5 102.3(9) . . ?
F4A C15 C14 113.6(5) . . ?
F6 C15 C14 112.5(7) . . ?
F5A C15 C14 114.0(5) . . ?
F4 C15 C14 113.4(6) . . ?
F6A C15 C14 111.6(6) . . ?
F5 C15 C14 109.8(6) . . ?
O5 C14 O4 130.4(5) . . ?
O5 C14 C15 115.9(5) . . ?
O4 C14 C15 113.6(5) . . ?

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 O2 0.916(10) 2.021(14) 2.932(5) 173(6) 14_456 yes
N1 H1 F3A^b 0.916(10) 2.91(5) 3.418(11) 116(4) 14_456 yes

_refine_diff_density_max         1.474
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.135



