# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_kv
_database_code_depnum_ccdc_archive 'CCDC 1040304'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H38 Cl2 N4 O4 Pd2'
_chemical_formula_sum            'C47 H38 Cl2 N4 O4 Pd2'
_chemical_formula_weight         1006.51

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

loop_
_symmetry_equiv_pos_as_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                   18.0741(4)
_cell_length_b                   16.5018(4)
_cell_length_c                   15.3290(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.5910(10)
_cell_angle_gamma                90.00
_cell_volume                     4157.28(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.65

_exptl_crystal_description       needles
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34962
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         30.57
_reflns_number_total             6333
_reflns_number_gt                5122
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0482P)²+1.2171P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00107(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6333
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.009
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.969640(9) 1.099819(9) 0.145020(11) 0.03199(7) Uani 1 1 d . . .
Cl1 Cl 0.06240(11) 0.43691(7) 0.21650(15) 0.1448(6) Uani 1 1 d . . .
O2 O 0.89461(10) 1.18857(9) 0.17120(12) 0.0423(4) Uani 1 1 d . . .
O1 O 1.05742(10) 1.18562(10) 0.16826(11) 0.0435(4) Uani 1 1 d . . .
N2 N 0.92790(10) 0.93178(10) 0.11337(12) 0.0338(3) Uani 1 1 d . . .
N1 N 0.89187(10) 1.00538(10) 0.11265(12) 0.0335(3) Uani 1 1 d . . .
C3 C 0.81585(12) 0.98949(13) 0.10128(15) 0.0368(4) Uani 1 1 d . . .
C2 C 0.80433(15) 0.90581(13) 0.0975(2) 0.0449(5) Uani 1 1 d . . .
H2 H 0.7573 0.8790 0.0920 0.054 Uiso 1 1 calc R . .
C1 C 0.87482(13) 0.87029(13) 0.10346(16) 0.0385(4) Uani 1 1 d . . .
C10 C 1.00949(12) 0.93695(13) 0.12327(14) 0.0348(4) Uani 1 1 d . . .
C15 C 1.05679(14) 0.87006(15) 0.12525(18) 0.0454(5) Uani 1 1 d . . .
H15 H 1.0369 0.8178 0.1234 0.055 Uiso 1 1 calc R . .
C14 C 1.13408(15) 0.88270(17) 0.1300(2) 0.0520(6) Uani 1 1 d . . .
H14 H 1.1662 0.8385 0.1307 0.062 Uiso 1 1 calc R . .
C13 C 1.16376(15) 0.95949(18) 0.13381(19) 0.0515(6) Uani 1 1 d . . .
H13 H 1.2155 0.9671 0.1360 0.062 Uiso 1 1 calc R . .
C12 C 1.11736(14) 1.02584(15) 0.13438(17) 0.0441(5) Uani 1 1 d . . .
H12 H 1.1384 1.0777 0.1376 0.053 Uiso 1 1 calc R . .
C11 C 1.03953(12) 1.01581(13) 0.13013(15) 0.0354(4) Uani 1 1 d . . .
C16 C 0.88809(14) 0.78270(13) 0.09617(17) 0.0415(5) Uani 1 1 d . . .
C4 C 0.75252(12) 1.05089(13) 0.08495(16) 0.0378(4) Uani 1 1 d . . .
C9 C 0.74482(14) 1.11739(14) 0.02638(17) 0.0417(5) Uani 1 1 d . . .
H9 H 0.7835 1.1264 0.0022 0.050 Uiso 1 1 calc R . .
C8 C 0.68022(15) 1.17032(15) 0.00370(18) 0.0488(5) Uani 1 1 d . . .
H8 H 0.6755 1.2144 -0.0361 0.059 Uiso 1 1 calc R . .
C7 C 0.62271(16) 1.15820(17) 0.0397(2) 0.0570(7) Uani 1 1 d . . .
H7 H 0.5795 1.1941 0.0247 0.068 Uiso 1 1 calc R . .
C6 C 0.62992(18) 1.09230(18) 0.0981(2) 0.0597(7) Uani 1 1 d . . .
H6 H 0.5911 1.0836 0.1221 0.072 Uiso 1 1 calc R . .
C5 C 0.69462(15) 1.03894(16) 0.12125(19) 0.0503(6) Uani 1 1 d . . .
H5 H 0.6992 0.9950 0.1612 0.060 Uiso 1 1 calc R . .
C17 C 0.90461(15) 0.75032(15) 0.02313(19) 0.0497(6) Uani 1 1 d . . .
H17 H 0.9108 0.7844 -0.0217 0.060 Uiso 1 1 calc R . .
C21 C 0.8773(2) 0.73062(16) 0.1606(2) 0.0625(7) Uani 1 1 d . . .
H21 H 0.8651 0.7513 0.2095 0.075 Uiso 1 1 calc R . .
C18 C 0.91207(17) 0.66735(17) 0.0163(2) 0.0604(7) Uani 1 1 d . . .
H18 H 0.9239 0.6461 -0.0326 0.072 Uiso 1 1 calc R . .
C19 C 0.9023(2) 0.61634(17) 0.0810(3) 0.0708(9) Uani 1 1 d . . .
H19 H 0.9077 0.5606 0.0764 0.085 Uiso 1 1 calc R . .
C20 C 0.8845(3) 0.64771(18) 0.1525(3) 0.0821(11) Uani 1 1 d . . .
H20 H 0.8773 0.6131 0.1962 0.099 Uiso 1 1 calc R . .
C22 C 0.89174(13) 1.20545(12) 0.24864(16) 0.0377(4) Uani 1 1 d . . .
C23 C 0.81962(17) 1.25381(18) 0.2441(2) 0.0611(7) Uani 1 1 d . . .
H23A H 0.8067 1.2946 0.1954 0.092 Uiso 1 1 calc R . .
H23B H 0.8324 1.2792 0.3050 0.092 Uiso 1 1 calc R . .
H23C H 0.7738 1.2185 0.2290 0.092 Uiso 1 1 calc R . .
C24 C 0.0000 0.3785(3) 0.2500 0.0910(17) Uani 1 2 d S . .
H24A H -0.0330 0.3440 0.1968 0.109 Uiso 0.50 1 calc PR . .
H24B H 0.0330 0.3440 0.3032 0.109 Uiso 0.50 1 calc PR . .


_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 C11 1.952(2) . ?
Pd1 N1 2.0175(17) . ?
Pd1 O1 2.0440(15) . ?
Pd1 O2 2.1443(15) . ?
Pd1 Pd1 2.9365(3) 2_755 ?
Cl1 C24 1.716(3) . ?
O2 C22 1.241(3) . ?
O1 C22 1.265(3) 2_755 ?
N2 C1 1.361(3) . ?
N2 N1 1.376(2) . ?
N2 C10 1.421(3) . ?
N1 C3 1.337(3) . ?
C3 C2 1.394(3) . ?
C3 C4 1.470(3) . ?
C2 C1 1.370(3) . ?
C2 H2 0.9300 . ?
C1 C16 1.477(3) . ?
C10 C15 1.389(3) . ?
C10 C11 1.397(3) . ?
C15 C14 1.384(3) . ?
C15 H15 0.9300 . ?
C14 C13 1.368(4) . ?
C14 H14 0.9300 . ?
C13 C12 1.381(3) . ?
C13 H13 0.9300 . ?
C12 C11 1.391(3) . ?
C12 H12 0.9300 . ?
C16 C17 1.381(3) . ?
C16 C21 1.383(4) . ?
C4 C9 1.388(3) . ?
C4 C5 1.389(3) . ?
C9 C8 1.382(3) . ?
C9 H9 0.9300 . ?
C8 C7 1.379(4) . ?
C8 H8 0.9300 . ?
C7 C6 1.380(4) . ?
C7 H7 0.9300 . ?
C6 C5 1.387(4) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C17 C18 1.384(4) . ?
C17 H17 0.9300 . ?
C21 C20 1.385(4) . ?
C21 H21 0.9300 . ?
C18 C19 1.367(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.366(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C22 O1 1.265(3) 2_755 ?
C22 C23 1.505(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 Cl1 1.716(3) 2 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?

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
C11 Pd1 N1 80.86(8) . . ?
C11 Pd1 O1 91.10(8) . . ?
N1 Pd1 O1 171.39(7) . . ?
C11 Pd1 O2 175.94(7) . . ?
N1 Pd1 O2 98.25(7) . . ?
O1 Pd1 O2 89.98(7) . . ?
C11 Pd1 Pd1 99.40(6) . 2_755 ?
N1 Pd1 Pd1 100.02(5) . 2_755 ?
O1 Pd1 Pd1 84.26(5) . 2_755 ?
O2 Pd1 Pd1 76.82(4) . 2_755 ?
C22 O2 Pd1 127.85(14) . . ?
C22 O1 Pd1 122.73(14) 2_755 . ?
C1 N2 N1 110.36(17) . . ?
C1 N2 C10 135.15(18) . . ?
N1 N2 C10 114.50(16) . . ?
C3 N1 N2 106.57(16) . . ?
C3 N1 Pd1 139.17(14) . . ?
N2 N1 Pd1 113.63(12) . . ?
N1 C3 C2 109.11(19) . . ?
N1 C3 C4 124.89(19) . . ?
C2 C3 C4 125.7(2) . . ?
C1 C2 C3 107.6(2) . . ?
C1 C2 H2 126.2 . . ?
C3 C2 H2 126.2 . . ?
N2 C1 C2 106.33(19) . . ?
N2 C1 C16 127.5(2) . . ?
C2 C1 C16 126.1(2) . . ?
C15 C10 C11 121.5(2) . . ?
C15 C10 N2 123.8(2) . . ?
C11 C10 N2 114.68(17) . . ?
C14 C15 C10 118.7(2) . . ?
C14 C15 H15 120.7 . . ?
C10 C15 H15 120.7 . . ?
C13 C14 C15 120.8(2) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C12 C11 120.7(2) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C11 C10 117.9(2) . . ?
C12 C11 Pd1 126.96(17) . . ?
C10 C11 Pd1 114.85(14) . . ?
C17 C16 C21 118.8(2) . . ?
C17 C16 C1 122.5(2) . . ?
C21 C16 C1 118.6(2) . . ?
C9 C4 C5 118.8(2) . . ?
C9 C4 C3 121.1(2) . . ?
C5 C4 C3 119.8(2) . . ?
C8 C9 C4 120.6(2) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C7 C8 C9 120.4(2) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C5 C4 120.2(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C16 C21 C20 120.2(3) . . ?
C16 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
O2 C22 O1 127.1(2) . 2_755 ?
O2 C22 C23 117.0(2) . . ?
O1 C22 C23 115.9(2) 2_755 . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Cl1 C24 Cl1 111.7(3) 2 . ?
Cl1 C24 H24A 109.3 2 . ?
Cl1 C24 H24A 109.3 . . ?
Cl1 C24 H24B 109.3 2 . ?
Cl1 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.134
