 
data_shelxl 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          '(C42 H50 Cl2 N6 Pd).2(C2 H3 N)' 
_chemical_formula_sum 
 'C46 H56 Cl2 N8 Pd' 
_chemical_formula_weight          898.29 
 
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' 
 '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            tetragonal 
_symmetry_space_group_name_H-M    I41/acd 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y+1/2, z' 
 'x, -y, -z+1/2' 
 '-x+1/2, y, -z' 
 '-y+1/4, -x+1/4, -z+1/4' 
 'y+3/4, x+1/4, -z+1/4' 
 'y+1/4, -x+1/4, z+3/4' 
 '-y+1/4, x+3/4, z+1/4' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, -y+1, z+1/2' 
 'x+1/2, -y+1/2, -z+1' 
 '-x+1, y+1/2, -z+1/2' 
 '-y+3/4, -x+3/4, -z+3/4' 
 'y+5/4, x+3/4, -z+3/4' 
 'y+3/4, -x+3/4, z+5/4' 
 '-y+3/4, x+5/4, z+3/4' 
 '-x, -y, -z' 
 'x, y-1/2, -z' 
 '-x, y, z-1/2' 
 'x-1/2, -y, z' 
 'y-1/4, x-1/4, z-1/4' 
 '-y-3/4, -x-1/4, z-1/4' 
 '-y-1/4, x-1/4, -z-3/4' 
 'y-1/4, -x-3/4, -z-1/4' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x+1/2, y, -z+1/2' 
 '-x+1/2, y+1/2, z' 
 'x, -y+1/2, z+1/2' 
 'y+1/4, x+1/4, z+1/4' 
 '-y-1/4, -x+1/4, z+1/4' 
 '-y+1/4, x+1/4, -z-1/4' 
 'y+1/4, -x-1/4, -z+1/4' 
 
_cell_length_a                    14.7337(4) 
_cell_length_b                    14.7337(4) 
_cell_length_c                    43.098(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      9355.9(7) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     5040 
_cell_measurement_theta_min       2.8 
_cell_measurement_theta_max       26.1 
 
_exptl_crystal_description        block
_exptl_crystal_colour             'pale yellow' 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.275 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3744 
_exptl_absorpt_coefficient_mu     0.550 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.822
_exptl_absorpt_correction_T_max   0.914 
_exptl_absorpt_process_details    'SADABS (Bruker, 1999)' 
 
_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 axs kappa apex2 CCD Diffractometer' 
_diffrn_measurement_method        'ω and φ scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             39193 
_diffrn_reflns_av_R_equivalents   0.0481 
_diffrn_reflns_av_sigmaI/netI     0.0168 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -49 
_diffrn_reflns_limit_l_max        51 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              2072 
_reflns_number_gt                 1595 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'APEX2 (Bruker, 2004)'
_computing_cell_refinement        'APEX2/SAINT (Bruker, 2004)' 
_computing_data_reduction         'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution     'SIR92 (Altornare et al., 1993)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_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)+(0.0269P)²+66.1200P] 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        0.00028(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2072 
_refine_ls_number_parameters      138 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0762 
_refine_ls_R_factor_gt            0.0599 
_refine_ls_wR_factor_ref          0.1459 
_refine_ls_wR_factor_gt           0.1366 
_refine_ls_goodness_of_fit_ref    1.329 
_refine_ls_restrained_S_all       1.333 
_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 0.4488(4) 0.4116(4) 0.31579(13) 0.0501(14) Uani 1 1 d . . . 
C2 C 0.3627(4) 0.4250(4) 0.32824(14) 0.0489(14) Uani 1 1 d . A . 
C3 C 0.3389(4) 0.5127(4) 0.33679(15) 0.0614(17) Uani 1 1 d . . . 
H3 H 0.2817 0.5228 0.3452 0.074 Uiso 1 1 calc R A . 
C4 C 0.3968(5) 0.5850(4) 0.33330(17) 0.0628(17) Uani 1 1 d . A . 
C5 C 0.4812(5) 0.5686(4) 0.32045(16) 0.0647(18) Uani 1 1 d . . . 
H5 H 0.5208 0.6171 0.3177 0.078 Uiso 1 1 calc R A . 
C6 C 0.5089(4) 0.4832(4) 0.31157(13) 0.0490(14) Uani 1 1 d . A . 
C7 C 0.6025(5) 0.4678(5) 0.29870(17) 0.073(2) Uani 1 1 d . . . 
H7A H 0.5980 0.4423 0.2783 0.109 Uiso 1 1 calc R A . 
H7B H 0.6350 0.4268 0.3119 0.109 Uiso 1 1 calc R . . 
H7C H 0.6343 0.5246 0.2977 0.109 Uiso 1 1 calc R . . 
C8 C 0.3697(6) 0.6793(5) 0.3430(2) 0.105(3) Uani 1 1 d . . . 
H8A H 0.4208 0.7092 0.3523 0.157 Uiso 1 1 calc R A . 
H8B H 0.3210 0.6759 0.3577 0.157 Uiso 1 1 calc R . . 
H8C H 0.3502 0.7129 0.3251 0.157 Uiso 1 1 calc R . . 
C9 C 0.2971(4) 0.3484(4) 0.33252(17) 0.0658(18) Uani 1 1 d . . . 
H9A H 0.2957 0.3119 0.3141 0.099 Uiso 1 1 calc R A . 
H9B H 0.2377 0.3723 0.3365 0.099 Uiso 1 1 calc R . . 
H9C H 0.3160 0.3117 0.3498 0.099 Uiso 1 1 calc R . . 
N2 N 0.4873(4) 0.2926(4) 0.27864(11) 0.0713(17) Uani 1 1 d . . . 
C12 C 0.4655(13) 0.3228(11) 0.2489(3) 0.095(6) Uani 0.50 1 d P A . 
H12A H 0.4471 0.3852 0.2498 0.143 Uiso 0.50 1 calc PR . . 
H12B H 0.4168 0.2868 0.2407 0.143 Uiso 0.50 1 calc PR . . 
H12C H 0.5177 0.3172 0.2357 0.143 Uiso 0.50 1 calc PR . . 
C10 C 0.5000 0.2500 0.32818(15) 0.0411(15) Uani 1 2 d S . . 
N1 N 0.4784(4) 0.3195(4) 0.30843(11) 0.0479(13) Uani 0.50 1 d P A 1 
C11 C 0.4784(4) 0.3195(4) 0.30843(11) 0.0479(13) Uani 0.50 1 d P A 2 
Cl1 Cl 0.61142(10) 0.36142(10) 0.3750 0.0568(5) Uani 1 2 d S . . 
Pd1 Pd 0.5000 0.2500 0.3750 0.0400(3) Uani 1 4 d S . . 
N3 N 0.3118(16) 0.4494(14) 0.2470(7) 0.186(10) Uiso 0.50 1 d PD . . 
C13 C 0.2861(19) 0.3743(17) 0.2462(7) 0.161(10) Uiso 0.50 1 d PD . . 
C14 C 0.252(3) 0.2852(18) 0.2475(10) 0.188(12) Uiso 0.50 1 d PD . . 
 
 
_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 C6 1.389(8) . ? 
C1 C2 1.392(8) . ? 
C1 N1 1.461(8) . ? 
C2 C3 1.389(9) . ? 
C2 C9 1.497(8) . ? 
C3 C4 1.372(9) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.383(10) . ? 
C4 C8 1.505(9) . ? 
C5 C6 1.376(9) . ? 
C5 H5 0.9300 . ? 
C6 C7 1.504(9) . ? 
C7 H7A 0.9600 . ? 
C7 H7B 0.9600 . ? 
C7 H7C 0.9600 . ? 
C8 H8A 0.9600 . ? 
C8 H8B 0.9600 . ? 
C8 H8C 0.9600 . ? 
C9 H9A 0.9600 . ? 
C9 H9B 0.9600 . ? 
C9 H9C 0.9600 . ? 
N2 N2 1.310(12) 2_655 ? 
N2 N1 1.350(7) . ? 
N2 C12 1.396(14) . ? 
C12 H12A 0.9600 . ? 
C12 H12B 0.9600 . ? 
C12 H12C 0.9600 . ? 
C10 C11 1.369(6) 2_655 ? 
C10 N1 1.369(6) 2_655 ? 
C10 N1 1.369(6) . ? 
C10 Pd1 2.018(6) . ? 
Cl1 Pd1 2.322(2) . ? 
Pd1 C10 2.018(6) 13 ? 
Pd1 Cl1 2.322(2) 2_655 ? 
N3 C13 1.169(17) . ? 
N3 N3 1.51(4) 3_565 ? 
C13 C14 1.408(18) . ? 
C14 C14 1.06(5) 25 ? 
 
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 
C6 C1 C2 121.6(6) . . ? 
C6 C1 N1 119.2(5) . . ? 
C2 C1 N1 119.1(5) . . ? 
C3 C2 C1 117.6(5) . . ? 
C3 C2 C9 120.4(6) . . ? 
C1 C2 C9 122.0(6) . . ? 
C4 C3 C2 122.4(6) . . ? 
C4 C3 H3 118.8 . . ? 
C2 C3 H3 118.8 . . ? 
C3 C4 C5 117.8(6) . . ? 
C3 C4 C8 121.5(7) . . ? 
C5 C4 C8 120.7(7) . . ? 
C6 C5 C4 122.5(6) . . ? 
C6 C5 H5 118.7 . . ? 
C4 C5 H5 118.7 . . ? 
C5 C6 C1 118.0(6) . . ? 
C5 C6 C7 120.8(6) . . ? 
C1 C6 C7 121.2(6) . . ? 
C6 C7 H7A 109.5 . . ? 
C6 C7 H7B 109.5 . . ? 
H7A C7 H7B 109.5 . . ? 
C6 C7 H7C 109.5 . . ? 
H7A C7 H7C 109.5 . . ? 
H7B C7 H7C 109.5 . . ? 
C4 C8 H8A 109.5 . . ? 
C4 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
C4 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
C2 C9 H9A 109.5 . . ? 
C2 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
C2 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
N2 N2 N1 108.0(3) 2_655 . ? 
N2 N2 C12 111.8(7) 2_655 . ? 
N1 N2 C12 139.3(9) . . ? 
N2 C12 H12A 109.5 . . ? 
N2 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
N2 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
C11 C10 N1 0.0(4) 2_655 2_655 ? 
C11 C10 N1 103.1(6) 2_655 . ? 
N1 C10 N1 103.1(6) 2_655 . ? 
C11 C10 Pd1 128.4(3) 2_655 . ? 
N1 C10 Pd1 128.4(3) 2_655 . ? 
N1 C10 Pd1 128.4(3) . . ? 
N2 N1 C10 110.4(5) . . ? 
N2 N1 C1 120.5(5) . . ? 
C10 N1 C1 129.0(5) . . ? 
C10 Pd1 C10 180.0 13 . ? 
C10 Pd1 Cl1 90.000(1) 13 . ? 
C10 Pd1 Cl1 90.000(1) . . ? 
C10 Pd1 Cl1 90.003(1) 13 2_655 ? 
C10 Pd1 Cl1 89.997(1) . 2_655 ? 
Cl1 Pd1 Cl1 180.0 . 2_655 ? 
C13 N3 N3 159(3) . 3_565 ? 
N3 C13 C14 175(4) . . ? 
C14 C14 C13 160(6) 25 . ? 
 
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 
C6 C1 C2 C3 -0.9(9) . . . . ? 
N1 C1 C2 C3 176.0(5) . . . . ? 
C6 C1 C2 C9 179.3(6) . . . . ? 
N1 C1 C2 C9 -3.8(9) . . . . ? 
C1 C2 C3 C4 0.2(9) . . . . ? 
C9 C2 C3 C4 180.0(6) . . . . ? 
C2 C3 C4 C5 0.7(10) . . . . ? 
C2 C3 C4 C8 -179.5(7) . . . . ? 
C3 C4 C5 C6 -0.8(10) . . . . ? 
C8 C4 C5 C6 179.4(7) . . . . ? 
C4 C5 C6 C1 0.1(9) . . . . ? 
C4 C5 C6 C7 -177.9(6) . . . . ? 
C2 C1 C6 C5 0.8(9) . . . . ? 
N1 C1 C6 C5 -176.1(5) . . . . ? 
C2 C1 C6 C7 178.8(6) . . . . ? 
N1 C1 C6 C7 1.8(9) . . . . ? 
N2 N2 N1 C10 0.9(9) 2_655 . . . ? 
C12 N2 N1 C10 168.7(13) . . . . ? 
N2 N2 N1 C1 -178.8(7) 2_655 . . . ? 
C12 N2 N1 C1 -11.0(16) . . . . ? 
C11 C10 N1 N2 -0.3(3) 2_655 . . . ? 
N1 C10 N1 N2 -0.3(3) 2_655 . . . ? 
Pd1 C10 N1 N2 179.7(3) . . . . ? 
C11 C10 N1 C1 179.4(7) 2_655 . . . ? 
N1 C10 N1 C1 179.4(7) 2_655 . . . ? 
Pd1 C10 N1 C1 -0.6(7) . . . . ? 
C6 C1 N1 N2 -73.7(8) . . . . ? 
C2 C1 N1 N2 109.3(7) . . . . ? 
C6 C1 N1 C10 106.7(6) . . . . ? 
C2 C1 N1 C10 -70.4(8) . . . . ? 
C11 C10 Pd1 C10 73(13) 2_655 . . 13 ? 
N1 C10 Pd1 C10 73(13) 2_655 . . 13 ? 
N1 C10 Pd1 C10 -107(13) . . . 13 ? 
C11 C10 Pd1 Cl1 117.7(3) 2_655 . . . ? 
N1 C10 Pd1 Cl1 117.7(3) 2_655 . . . ? 
N1 C10 Pd1 Cl1 -62.3(3) . . . . ? 
C11 C10 Pd1 Cl1 -62.3(3) 2_655 . . 2_655 ? 
N1 C10 Pd1 Cl1 -62.3(3) 2_655 . . 2_655 ? 
N1 C10 Pd1 Cl1 117.7(3) . . . 2_655 ? 
N3 N3 C13 C14 -38(58) 3_565 . . . ? 
N3 C13 C14 C14 -89(55) . . . 25 ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.392 
_refine_diff_density_min   -0.502 
_refine_diff_density_rms    0.070 
