# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014



data_new



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C16 H16 N4 O2 '

_chemical_formula_sum            'C16 H16 N4 O2'



_chemical_formula_weight         296.33



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'



_symmetry_cell_setting           Monoclinic

_symmetry_space_group_name_H-M   P2(1)/n

_symmetry_space_group_name_Hall  '-P 2yn'


loop_

_symmetry_equiv_pos_as_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                   9.1945(6)

_cell_length_b                   8.2633(5)

_cell_length_c                   9.9539(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 107.528(2)

_cell_angle_gamma                90.00

_cell_volume                     721.15(8)

_cell_formula_units_Z            2

_cell_measurement_temperature    298(2)

_cell_measurement_reflns_used    1775

_cell_measurement_theta_min      2.65

_cell_measurement_theta_max      29.44



_exptl_crystal_description       Hexagonal

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.20

_exptl_crystal_size_min          0.15

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.365

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             312.0

_exptl_absorpt_coefficient_mu    0.094

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9695

_exptl_absorpt_correction_T_max  0.9815

_exptl_absorpt_process_details   'SADABS (Bruker,2004)'



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      298(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 APEXII CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            4185

_diffrn_reflns_av_R_equivalents  0.0213

_diffrn_reflns_av_sigmaI/netI    0.0208

_diffrn_reflns_limit_h_min       -9

_diffrn_reflns_limit_h_max       10

_diffrn_reflns_limit_k_min       -9

_diffrn_reflns_limit_k_max       9

_diffrn_reflns_limit_l_min       -11

_diffrn_reflns_limit_l_max       11

_diffrn_reflns_theta_min         2.65

_diffrn_reflns_theta_max         25.00

_reflns_number_total             1211

_reflns_number_gt                1006

_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'APEXII, Bruker,2004'
_computing_cell_refinement       'APEXII/SAINT, Bruker,2004'
_computing_data_reduction        'SAINT PLUS/XPREP, Bruker,2004'
_computing_structure_solution    'SHELXS-97  (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97  (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3   (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97  (Sheldrick, 2008)'



_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     SHELXL

_refine_ls_extinction_coef       0.094(16)

_refine_ls_extinction_expression 
Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^

_refine_ls_number_reflns         1211

_refine_ls_number_parameters     101

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0466

_refine_ls_R_factor_gt           0.0367

_refine_ls_wR_factor_ref         0.1378

_refine_ls_wR_factor_gt          0.1259

_refine_ls_goodness_of_fit_ref   1.068

_refine_ls_restrained_S_all      1.068

_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_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group



















C1 C 0.59223(17) 0.2205(2) 0.40234(15) 0.0415(5) Uani 1 1 d . . .
H1 H 0.5282 0.2887 0.3362 0.050 Uiso 1 1 calc R . .
C2 C 0.5890(2) 0.2197(2) 0.54064(17) 0.0502(5) Uani 1 1 d . . .
H2 H 0.5212 0.2890 0.5648 0.060 Uiso 1 1 calc R . .
C3 C 0.7725(2) 0.0281(2) 0.60233(16) 0.0527(5) Uani 1 1 d . . .
H3 H 0.8347 -0.0396 0.6703 0.063 Uiso 1 1 calc R . .
C4 C 0.78512(19) 0.02116(18) 0.46801(15) 0.0420(5) Uani 1 1 d . . .
H4 H 0.8552 -0.0480 0.4472 0.050 Uiso 1 1 calc R . .
C5 C 0.69165(17) 0.11882(17) 0.36450(14) 0.0321(5) Uani 1 1 d . . .
C6 C 0.71437(18) 0.11741(17) 0.22088(14) 0.0336(5) Uani 1 1 d . . .
C7 C 0.60485(18) 0.10757(18) -0.03545(14) 0.0360(5) Uani 1 1 d . . .
H7A H 0.7092 0.1337 -0.0305 0.043 Uiso 1 1 calc R . .
H7B H 0.5392 0.1920 -0.0890 0.043 Uiso 1 1 calc R . .
C8 C 0.43882(16) 0.05291(19) 0.10929(14) 0.0357(5) Uani 1 1 d . . .
H8A H 0.3652 0.1347 0.0627 0.043 Uiso 1 1 calc R . .
H8B H 0.4372 0.0439 0.2060 0.043 Uiso 1 1 calc R . .
N1 N 0.67727(19) 0.12546(19) 0.64106(15) 0.0546(5) Uani 1 1 d . . .
N2 N 0.59056(14) 0.10160(14) 0.10744(11) 0.0339(4) Uani 1 1 d . . .
O1 O 0.84355(13) 0.13381(17) 0.21237(11) 0.0579(5) Uani 1 1 d . . .






_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





















C1 C5 1.375(2) . ?
C1 C2 1.386(2) . ?
C1 H1 0.9300 . ?
C2 N1 1.333(2) . ?
C2 H2 0.9300 . ?
C3 N1 1.329(2) . ?
C3 C4 1.378(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.5058(19) . ?
C6 O1 1.2234(18) . ?
C6 N2 1.3467(18) . ?
C7 N2 1.4681(16) . ?
C7 C8 1.511(2) 3_655 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.4575(19) . ?
C8 C7 1.511(2) 3_655 ?
C8 H8A 0.9700 . ?
C8 H8B 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


































C5 C1 C2 118.96(15) . . ?
C5 C1 H1 120.5 . . ?
C2 C1 H1 120.5 . . ?
N1 C2 C1 123.86(16) . . ?
N1 C2 H2 118.1 . . ?
C1 C2 H2 118.1 . . ?
N1 C3 C4 124.22(16) . . ?
N1 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
C3 C4 C5 118.88(16) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C1 C5 C4 117.84(14) . . ?
C1 C5 C6 123.96(13) . . ?
C4 C5 C6 117.99(13) . . ?
O1 C6 N2 123.08(13) . . ?
O1 C6 C5 118.69(13) . . ?
N2 C6 C5 118.22(13) . . ?
N2 C7 C8 110.71(11) . 3_655 ?
N2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 3_655 . ?
N2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 3_655 . ?
H7A C7 H7B 108.1 . . ?
N2 C8 C7 110.57(12) . 3_655 ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 3_655 . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 3_655 . ?
H8A C8 H8B 108.1 . . ?
C3 N1 C2 116.23(14) . . ?
C6 N2 C8 125.93(12) . . ?
C6 N2 C7 120.62(12) . . ?
C8 N2 C7 112.76(11) . . ?



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




















C5 C1 C2 N1 0.0(3) . . . . ?
N1 C3 C4 C5 -1.2(3) . . . . ?
C2 C1 C5 C4 -0.6(2) . . . . ?
C2 C1 C5 C6 -175.19(13) . . . . ?
C3 C4 C5 C1 1.1(2) . . . . ?
C3 C4 C5 C6 176.06(13) . . . . ?
C1 C5 C6 O1 125.49(17) . . . . ?
C4 C5 C6 O1 -49.11(19) . . . . ?
C1 C5 C6 N2 -53.09(19) . . . . ?
C4 C5 C6 N2 132.31(15) . . . . ?
C4 C3 N1 C2 0.6(3) . . . . ?
C1 C2 N1 C3 0.0(3) . . . . ?
O1 C6 N2 C8 168.20(15) . . . . ?
C5 C6 N2 C8 -13.3(2) . . . . ?
O1 C6 N2 C7 -1.6(2) . . . . ?
C5 C6 N2 C7 176.93(11) . . . . ?
C7 C8 N2 C6 -115.02(15) 3_655 . . . ?
C7 C8 N2 C7 55.45(17) 3_655 . . . ?
C8 C7 N2 C6 115.51(15) 3_655 . . . ?
C8 C7 N2 C8 -55.53(19) 3_655 . . . ?



_diffrn_measured_fraction_theta_max 0.957

_diffrn_reflns_theta_full        25.00

_diffrn_measured_fraction_theta_full 0.957

_refine_diff_density_max         0.184

_refine_diff_density_min         -0.148

_refine_diff_density_rms         0.032

_database_code_depnum_ccdc_archive 'CCDC 952097'

data_new

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 N12 O4 Pd2, 4(Cl O4), 3(O)'
_chemical_formula_sum            'C36 H48 Cl4 N12 O23 Pd2'
_chemical_formula_weight         1371.46

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmc2(1)
_symmetry_space_group_name_Hall  'C 2c -2 '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, 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'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   18.8926(6)
_cell_length_b                   17.6085(6)
_cell_length_c                   17.0599(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5675.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8296
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      27.56

_exptl_crystal_description       Block
_exptl_crystal_colour            metallic
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2768
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7421
_exptl_absorpt_correction_T_max  0.7985
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32532
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5142
_reflns_number_gt                4677
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       APEXII,Bruker,2004
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'


_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)+(0.0955P)²+4.2899P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_number_reflns         5142
_refine_ls_number_parameters     369
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1244
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9624(4) 0.3300(6) 0.3473(6) 0.109(4) Uani 1 1 d . . .
H1A H 0.9465 0.2783 0.3562 0.130 Uiso 1 1 calc R . .
H1B H 0.9465 0.3446 0.2954 0.130 Uiso 1 1 calc R . .
C2 C 0.8929(5) 0.5555(5) 0.4986(6) 0.095(3) Uani 1 1 d . . .
H2 H 0.9153 0.5802 0.4573 0.114 Uiso 1 1 calc R . .
C3 C 0.8338(5) 0.5875(5) 0.5278(7) 0.097(3) Uani 1 1 d . . .
H3 H 0.8146 0.6302 0.5038 0.117 Uiso 1 1 calc R . .
C4 C 0.8025(3) 0.5579(3) 0.5914(4) 0.0529(14) Uani 1 1 d . . .
C5 C 0.8336(6) 0.4952(7) 0.6208(7) 0.110(4) Uani 1 1 d . . .
H5 H 0.8152 0.4723 0.6655 0.132 Uiso 1 1 calc R . .
C6 C 0.8922(5) 0.4650(5) 0.5851(5) 0.091(3) Uani 1 1 d . . .
H6 H 0.9123 0.4216 0.6067 0.109 Uiso 1 1 calc R . .
C7 C 0.7351(3) 0.5896(4) 0.6261(4) 0.0600(16) Uani 1 1 d . . .
C8 C 0.8032(3) 0.6777(4) 0.7103(4) 0.0613(18) Uani 1 1 d . . .
H8A H 0.8446 0.6538 0.6873 0.074 Uiso 1 1 calc R . .
H8B H 0.8030 0.6663 0.7659 0.074 Uiso 1 1 calc R . .
C9 C 0.8073(4) 0.7603(5) 0.6991(5) 0.063(2) Uani 1 1 d . . .
H9A H 0.8141 0.7715 0.6439 0.076 Uiso 1 1 calc R . .
H9B H 0.8476 0.7802 0.7277 0.076 Uiso 1 1 calc R . .
C10 C 0.6777(4) 0.7668(5) 0.6912(5) 0.066(2) Uani 1 1 d . . .
H10A H 0.6782 0.7774 0.6354 0.079 Uiso 1 1 calc R . .
H10B H 0.6364 0.7912 0.7136 0.079 Uiso 1 1 calc R . .
C11 C 0.6733(3) 0.6825(5) 0.7042(5) 0.068(2) Uani 1 1 d . . .
H11A H 0.6681 0.6719 0.7597 0.082 Uiso 1 1 calc R . .
H11B H 0.6324 0.6621 0.6770 0.082 Uiso 1 1 calc R . .
C12 C 0.7378(3) 0.8518(4) 0.7804(5) 0.0592(18) Uani 1 1 d . . .
C13 C 0.8065(3) 0.8794(3) 0.8186(4) 0.0490(13) Uani 1 1 d . . .
C14 C 0.8418(4) 0.9419(4) 0.7890(4) 0.0564(16) Uani 1 1 d . . .
H14 H 0.8268 0.9650 0.7428 0.068 Uiso 1 1 calc R . .
C15 C 0.8996(3) 0.9696(4) 0.8291(4) 0.0556(14) Uani 1 1 d . . .
H15 H 0.9243 1.0106 0.8084 0.067 Uiso 1 1 calc R . .
C16 C 0.8875(4) 0.8791(3) 0.9236(4) 0.0569(15) Uani 1 1 d . . .
H16 H 0.9029 0.8571 0.9701 0.068 Uiso 1 1 calc R . .
C17 C 0.8301(3) 0.8475(3) 0.8850(4) 0.0562(15) Uani 1 1 d . . .
H17 H 0.8080 0.8044 0.9051 0.067 Uiso 1 1 calc R . .
C18 C 1.0359(4) 1.0668(8) 1.1007(5) 0.125(4) Uani 1 1 d D . .
H18A H 1.0516 1.0413 1.1480 0.149 Uiso 1 1 calc R . .
H18B H 1.0516 1.1192 1.1044 0.149 Uiso 1 1 calc R . .
Cl1 Cl 1.0000 0.71222(18) 0.62473(17) 0.0735(7) Uani 1 2 d S . .
Cl2 Cl 0.5000 0.74220(14) 0.58604(14) 0.0545(5) Uani 1 2 d S . .
Cl3 Cl 0.72101(9) 0.65834(11) 0.95958(17) 0.0840(5) Uani 1 1 d . . .
N1 N 0.9281(3) 0.3778(3) 0.4029(4) 0.0602(14) Uani 1 1 d D . .
N2 N 0.9210(3) 0.4933(3) 0.5235(3) 0.0509(11) Uani 1 1 d . . .
N3 N 0.7390(3) 0.6464(3) 0.6740(4) 0.0606(15) Uani 1 1 d . . .
N4 N 0.7415(3) 0.7975(3) 0.7272(3) 0.0574(13) Uani 1 1 d . . .
N5 N 0.9214(2) 0.9396(2) 0.8964(3) 0.0412(10) Uani 1 1 d . . .
N6 N 1.0714(3) 1.0332(3) 1.0366(3) 0.0548(12) Uani 1 1 d D . .
H6A H 1.1015 0.9974 1.0541 0.066 Uiso 1 1 calc R . .
H6B H 1.0967 1.0686 1.0109 0.066 Uiso 1 1 calc R . .
O1 O 0.6792(3) 0.5595(4) 0.6082(5) 0.102(3) Uani 1 1 d . . .
O2 O 0.6835(2) 0.8814(3) 0.8022(5) 0.100(2) Uani 1 1 d . . .
O3 O 1.0000 0.6382(7) 0.6536(12) 0.216(9) Uani 1 2 d S . .
O4 O 1.0000 0.7634(7) 0.6897(7) 0.141(5) Uani 1 2 d S . .
O5 O 0.9426(5) 0.7274(6) 0.5789(7) 0.147(4) Uani 1 1 d . . .
O6 O 0.6966(9) 0.5981(8) 0.9193(9) 0.215(6) Uani 1 1 d . . .
O7 O 0.7876(5) 0.6710(6) 0.9476(12) 0.217(8) Uani 1 1 d . . .
O8 O 0.6945(9) 0.7269(6) 0.9303(12) 0.213(8) Uani 1 1 d . . .
O9 O 0.6924(12) 0.6508(11) 1.0270(10) 0.328(14) Uani 1 1 d . . .
O10 O 0.5000 0.7714(9) 0.6605(7) 0.132(6) Uani 1 2 d S . .
O11 O 0.4369(3) 0.7652(4) 0.5459(4) 0.0912(19) Uani 1 1 d . . .
O12 O 0.5000 0.6614(5) 0.5875(8) 0.111(3) Uani 1 2 d S . .
O13 O 0.6821(6) 0.0302(5) 0.8352(10) 0.169(5) Uani 1 1 d . . .
O14 O 0.0000 0.1156(10) 0.782(2) 0.321(19) Uani 1 2 d S . .
Pd1 Pd 1.0000 0.43840(3) 0.46588(4) 0.04408(17) Uani 1 2 d S . .
Pd2 Pd 1.0000 0.98562(2) 0.96263(3) 0.03370(15) Uani 1 2 d S . .
H3N H 0.916(3) 0.417(2) 0.367(3) 0.041(16) Uiso 1 1 d D . .
H4N H 0.8837(19) 0.370(5) 0.427(5) 0.13(4) Uiso 1 1 d D . .


_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
C1 C1 1.420(14) 3_755 ?
C1 N1 1.425(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.289(10) . ?
C2 C3 1.348(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.340(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.348(12) . ?
C4 C7 1.512(9) . ?
C5 C6 1.372(12) . ?
C5 H5 0.9300 . ?
C6 N2 1.282(9) . ?
C6 H6 0.9300 . ?
C7 O1 1.220(8) . ?
C7 N3 1.294(8) . ?
C8 N3 1.469(8) . ?
C8 C9 1.469(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N4 1.486(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N4 1.456(8) . ?
C10 C11 1.503(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.487(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.209(8) . ?
C12 N4 1.320(9) . ?
C12 C13 1.532(8) . ?
C13 C17 1.342(9) . ?
C13 C14 1.384(9) . ?
C14 C15 1.378(9) . ?
C14 H14 0.9300 . ?
C15 N5 1.328(8) . ?
C15 H15 0.9300 . ?
C16 N5 1.327(7) . ?
C16 C17 1.386(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C18 1.358(17) 3_755 ?
C18 N6 1.412(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
Cl1 O5 1.363(9) 3_755 ?
Cl1 O5 1.363(9) . ?
Cl1 O3 1.393(13) . ?
Cl1 O4 1.428(14) . ?
Cl2 O10 1.370(10) . ?
Cl2 O12 1.422(9) . ?
Cl2 O11 1.433(6) . ?
Cl2 O11 1.434(6) 3_655 ?
Cl3 O9 1.277(13) . ?
Cl3 O7 1.295(8) . ?
Cl3 O6 1.345(10) . ?
Cl3 O8 1.400(12) . ?
N1 Pd1 2.033(5) . ?
N1 H3N 0.950(2) . ?
N1 H4N 0.950(2) . ?
N2 Pd1 2.031(5) . ?
N5 Pd2 2.034(4) . ?
N6 Pd2 2.028(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
Pd1 N2 2.031(5) 3_755 ?
Pd1 N1 2.033(5) 3_755 ?
Pd2 N6 2.028(5) 3_755 ?
Pd2 N5 2.034(4) 3_755 ?

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 C1 N1 117.0(4) 3_755 . ?
C1 C1 H1A 108.0 3_755 . ?
N1 C1 H1A 108.0 . . ?
C1 C1 H1B 108.0 3_755 . ?
N1 C1 H1B 108.0 . . ?
H1A C1 H1B 107.3 . . ?
N2 C2 C3 125.1(8) . . ?
N2 C2 H2 117.4 . . ?
C3 C2 H2 117.4 . . ?
C4 C3 C2 120.1(8) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 115.4(7) . . ?
C3 C4 C7 123.0(7) . . ?
C5 C4 C7 121.6(7) . . ?
C4 C5 C6 120.2(8) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
N2 C6 C5 123.8(7) . . ?
N2 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
O1 C7 N3 122.9(6) . . ?
O1 C7 C4 118.2(6) . . ?
N3 C7 C4 119.0(5) . . ?
N3 C8 C9 111.1(6) . . ?
N3 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N3 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 N4 110.5(6) . . ?
C8 C9 H9A 109.6 . . ?
N4 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
N4 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N4 C10 C11 110.5(6) . . ?
N4 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N3 C11 C10 108.9(6) . . ?
N3 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O2 C12 N4 124.7(6) . . ?
O2 C12 C13 116.8(6) . . ?
N4 C12 C13 118.5(5) . . ?
C17 C13 C14 118.8(5) . . ?
C17 C13 C12 120.5(5) . . ?
C14 C13 C12 120.4(6) . . ?
C15 C14 C13 118.8(6) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N5 C15 C14 122.3(5) . . ?
N5 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N5 C16 C17 122.3(6) . . ?
N5 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C13 C17 C16 119.5(5) . . ?
C13 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C18 C18 N6 118.3(4) 3_755 . ?
C18 C18 H18A 107.7 3_755 . ?
N6 C18 H18A 107.7 . . ?
C18 C18 H18B 107.7 3_755 . ?
N6 C18 H18B 107.7 . . ?
H18A C18 H18B 107.1 . . ?
O5 Cl1 O5 105.3(10) 3_755 . ?
O5 Cl1 O3 112.7(7) 3_755 . ?
O5 Cl1 O3 112.7(7) . . ?
O5 Cl1 O4 108.8(6) 3_755 . ?
O5 Cl1 O4 108.8(6) . . ?
O3 Cl1 O4 108.5(10) . . ?
O10 Cl2 O12 111.0(9) . . ?
O10 Cl2 O11 109.7(5) . . ?
O12 Cl2 O11 106.9(4) . . ?
O10 Cl2 O11 109.7(5) . 3_655 ?
O12 Cl2 O11 106.9(4) . 3_655 ?
O11 Cl2 O11 112.6(6) . 3_655 ?
O9 Cl3 O7 124.9(16) . . ?
O9 Cl3 O6 103.5(9) . . ?
O7 Cl3 O6 112.8(10) . . ?
O9 Cl3 O8 105.0(14) . . ?
O7 Cl3 O8 98.2(9) . . ?
O6 Cl3 O8 112.0(11) . . ?
C1 N1 Pd1 111.0(4) . . ?
C1 N1 H3N 97(4) . . ?
Pd1 N1 H3N 97(4) . . ?
C1 N1 H4N 127(7) . . ?
Pd1 N1 H4N 116(7) . . ?
H3N N1 H4N 100.3(19) . . ?
C6 N2 C2 115.1(6) . . ?
C6 N2 Pd1 121.6(5) . . ?
C2 N2 Pd1 123.1(5) . . ?
C7 N3 C8 127.1(5) . . ?
C7 N3 C11 120.1(5) . . ?
C8 N3 C11 112.5(5) . . ?
C12 N4 C10 121.0(5) . . ?
C12 N4 C9 125.9(5) . . ?
C10 N4 C9 113.1(5) . . ?
C16 N5 C15 118.1(5) . . ?
C16 N5 Pd2 118.5(4) . . ?
C15 N5 Pd2 123.2(4) . . ?
C18 N6 Pd2 109.9(5) . . ?
C18 N6 H6A 109.7 . . ?
Pd2 N6 H6A 109.7 . . ?
C18 N6 H6B 109.7 . . ?
Pd2 N6 H6B 109.7 . . ?
H6A N6 H6B 108.2 . . ?
N2 Pd1 N2 94.5(3) 3_755 . ?
N2 Pd1 N1 174.6(2) 3_755 . ?
N2 Pd1 N1 90.9(2) . . ?
N2 Pd1 N1 90.9(2) 3_755 3_755 ?
N2 Pd1 N1 174.6(2) . 3_755 ?
N1 Pd1 N1 83.8(3) . 3_755 ?
N6 Pd2 N6 83.4(3) . 3_755 ?
N6 Pd2 N5 174.60(19) . . ?
N6 Pd2 N5 91.43(19) 3_755 . ?
N6 Pd2 N5 91.43(19) . 3_755 ?
N6 Pd2 N5 174.60(19) 3_755 3_755 ?
N5 Pd2 N5 93.7(3) . 3_755 ?

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
N2 C2 C3 C4 5.4(18) . . . . ?
C2 C3 C4 C5 -1.3(15) . . . . ?
C2 C3 C4 C7 -178.4(8) . . . . ?
C3 C4 C5 C6 -1.2(17) . . . . ?
C7 C4 C5 C6 175.8(10) . . . . ?
C4 C5 C6 N2 0(2) . . . . ?
C3 C4 C7 O1 97.1(10) . . . . ?
C5 C4 C7 O1 -79.7(12) . . . . ?
C3 C4 C7 N3 -83.9(10) . . . . ?
C5 C4 C7 N3 99.3(11) . . . . ?
N3 C8 C9 N4 53.8(8) . . . . ?
N4 C10 C11 N3 -55.7(9) . . . . ?
O2 C12 C13 C17 87.9(9) . . . . ?
N4 C12 C13 C17 -91.4(9) . . . . ?
O2 C12 C13 C14 -86.2(10) . . . . ?
N4 C12 C13 C14 94.5(8) . . . . ?
C17 C13 C14 C15 -0.4(9) . . . . ?
C12 C13 C14 C15 173.8(6) . . . . ?
C13 C14 C15 N5 -2.0(10) . . . . ?
C14 C13 C17 C16 1.9(10) . . . . ?
C12 C13 C17 C16 -172.3(6) . . . . ?
N5 C16 C17 C13 -1.2(11) . . . . ?
C1 C1 N1 Pd1 2.5(7) 3_755 . . . ?
C5 C6 N2 C2 3.2(15) . . . . ?
C5 C6 N2 Pd1 -172.2(10) . . . . ?
C3 C2 N2 C6 -6.1(15) . . . . ?
C3 C2 N2 Pd1 169.2(9) . . . . ?
O1 C7 N3 C8 167.9(9) . . . . ?
C4 C7 N3 C8 -11.0(12) . . . . ?
O1 C7 N3 C11 -5.7(13) . . . . ?
C4 C7 N3 C11 175.3(7) . . . . ?
C9 C8 N3 C7 129.1(8) . . . . ?
C9 C8 N3 C11 -56.9(8) . . . . ?
C10 C11 N3 C7 -128.6(7) . . . . ?
C10 C11 N3 C8 56.9(9) . . . . ?
O2 C12 N4 C10 -1.8(13) . . . . ?
C13 C12 N4 C10 177.5(7) . . . . ?
O2 C12 N4 C9 179.8(9) . . . . ?
C13 C12 N4 C9 -1.0(11) . . . . ?
C11 C10 N4 C12 -122.4(7) . . . . ?
C11 C10 N4 C9 56.2(9) . . . . ?
C8 C9 N4 C12 123.5(7) . . . . ?
C8 C9 N4 C10 -55.0(8) . . . . ?
C17 C16 N5 C15 -1.1(10) . . . . ?
C17 C16 N5 Pd2 175.2(5) . . . . ?
C14 C15 N5 C16 2.7(9) . . . . ?
C14 C15 N5 Pd2 -173.5(5) . . . . ?
C18 C18 N6 Pd2 -4.1(7) 3_755 . . . ?
C6 N2 Pd1 N2 -93.9(7) . . . 3_755 ?
C2 N2 Pd1 N2 91.0(7) . . . 3_755 ?
C6 N2 Pd1 N1 85.8(7) . . . . ?
C2 N2 Pd1 N1 -89.2(7) . . . . ?
C6 N2 Pd1 N1 84(3) . . . 3_755 ?
C2 N2 Pd1 N1 -91(3) . . . 3_755 ?
C1 N1 Pd1 N2 -5(3) . . . 3_755 ?
C1 N1 Pd1 N2 177.2(7) . . . . ?
C1 N1 Pd1 N1 -3.0(8) . . . 3_755 ?
C18 N6 Pd2 N6 4.8(8) . . . 3_755 ?
C18 N6 Pd2 N5 -10(3) . . . . ?
C18 N6 Pd2 N5 -173.8(7) . . . 3_755 ?
C16 N5 Pd2 N6 -61(2) . . . . ?
C15 N5 Pd2 N6 116(2) . . . . ?
C16 N5 Pd2 N6 -75.6(5) . . . 3_755 ?
C15 N5 Pd2 N6 100.6(5) . . . 3_755 ?
C16 N5 Pd2 N5 102.9(5) . . . 3_755 ?
C15 N5 Pd2 N5 -80.9(5) . . . 3_755 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.115
_database_code_depnum_ccdc_archive 'CCDC 967775'
