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

  
data_shelxl 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C30 H24 Cl11 N2 P Pd' 
_chemical_formula_weight          939.83 
  
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' 
 'P'  'P'   0.1023   0.0942 
 '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    P2(1)2(1)2(1) 
  
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' 
  
_cell_length_a                    19.497(4) 
_cell_length_b                    10.517(2) 
_cell_length_c                    18.232(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3738.5(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.670 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1864 
_exptl_absorpt_coefficient_mu     1.351 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
  
_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 P4' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7986 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0309 
_diffrn_reflns_limit_h_min        -25 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          3.14 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              7986 
_reflns_number_gt                 6804 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_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)+(0.0718P)²+4.0043P] 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    0.51(4) 
_refine_ls_number_reflns          7986 
_refine_ls_number_parameters      406 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0605 
_refine_ls_R_factor_gt            0.0483 
_refine_ls_wR_factor_ref          0.1343 
_refine_ls_wR_factor_gt           0.1242 
_refine_ls_goodness_of_fit_ref    1.060 
_refine_ls_restrained_S_all       1.060 
_refine_ls_shift/su_max           2.281 
_refine_ls_shift/su_mean          0.138 
  
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 0.406414(17) 0.61455(3) 1.07223(3) 0.04052(10) Uani 1 1 d . . . 
P1 P 0.46751(7) 0.86812(12) 0.98838(8) 0.0421(3) Uani 1 1 d . . . 
Cl1 Cl 0.35531(8) 0.48244(14) 1.15581(8) 0.0572(3) Uani 1 1 d . . . 
N2 N 0.3949(3) 0.4896(4) 0.9879(3) 0.0510(10) Uani 1 1 d . . . 
C1 C 0.3589(4) 0.3835(6) 0.9875(5) 0.0677(17) Uani 1 1 d . . . 
H1A H 0.3272 0.3691 1.0247 0.081 Uiso 1 1 calc R . . 
Cl2 Cl 0.43790(9) 0.74766(14) 1.16456(8) 0.0568(3) Uani 1 1 d . . . 
N1 N 0.4544(2) 0.7159(4) 0.9903(3) 0.0458(10) Uani 1 1 d . . . 
C2 C 0.3673(5) 0.2916(7) 0.9321(5) 0.082(2) Uani 1 1 d . . . 
H2A H 0.3401 0.2189 0.9319 0.098 Uiso 1 1 calc R . . 
C3 C 0.4150(5) 0.3093(7) 0.8792(5) 0.087(3) Uani 1 1 d . . . 
H3A H 0.4212 0.2477 0.8431 0.104 Uiso 1 1 calc R . . 
Cl3 Cl 0.56910(19) 0.4180(3) 0.05096(18) 0.1309(10) Uani 1 1 d . . . 
C4 C 0.4560(4) 0.4225(6) 0.8784(4) 0.0636(16) Uani 1 1 d . . . 
Cl4 Cl 0.61544(16) 0.5314(3) 0.1832(2) 0.1208(10) Uani 1 1 d . . . 
C5 C 0.4418(3) 0.5129(5) 0.9331(3) 0.0507(12) Uani 1 1 d . . . 
Cl5 Cl 0.5476(2) 0.2876(2) 0.1872(2) 0.1218(10) Uani 1 1 d . . . 
C6 C 0.4780(3) 0.6314(5) 0.9356(3) 0.0493(12) Uani 1 1 d . . . 
Cl6 Cl 0.6557(2) 0.2088(4) 0.8720(2) 0.1498(14) Uani 1 1 d . . . 
C7 C 0.5295(4) 0.6497(7) 0.8868(4) 0.0640(16) Uani 1 1 d . . . 
H7A H 0.5556 0.7237 0.8887 0.077 Uiso 1 1 calc R . . 
Cl7 Cl 0.7259(2) 0.4351(4) 0.8502(4) 0.184(2) Uani 1 1 d . . . 
C8 C 0.5435(4) 0.5565(8) 0.8332(4) 0.0744(19) Uani 1 1 d . . . 
H8A H 0.5789 0.5714 0.8002 0.089 Uiso 1 1 calc R . . 
Cl8 Cl 0.7525(2) 0.2286(6) 0.7580(3) 0.192(2) Uani 1 1 d . . . 
C9 C 0.5084(4) 0.4487(8) 0.8275(4) 0.077(2) Uani 1 1 d . . . 
H9A H 0.5184 0.3911 0.7903 0.092 Uiso 1 1 calc R . . 
Cl9 Cl 0.7193(4) 0.8515(7) 0.9200(3) 0.211(3) Uani 1 1 d . . . 
C10 C 0.5518(4) 0.4369(9) 0.1449(6) 0.092(3) Uani 1 1 d . . . 
H10A H 0.5075 0.4797 0.1506 0.110 Uiso 1 1 calc R . . 
Cl10 Cl 0.7229(5) 0.7411(6) 0.7745(4) 0.275(5) Uani 1 1 d . . . 
C11 C 0.4661(3) 0.9265(5) 0.8946(3) 0.0475(11) Uani 1 1 d . . . 
Cl11 Cl 0.8163(4) 0.8617(11) 0.8321(8) 0.346(6) Uani 1 1 d . . . 
C12 C 0.4044(3) 0.9326(7) 0.8569(4) 0.0564(14) Uani 1 1 d . . . 
H12A H 0.3642 0.9086 0.8806 0.068 Uiso 1 1 calc R . . 
C13 C 0.4013(4) 0.9726(7) 0.7867(4) 0.0682(17) Uani 1 1 d . . . 
H13A H 0.3594 0.9735 0.7623 0.082 Uiso 1 1 calc R . . 
C14 C 0.4607(4) 1.0129(7) 0.7503(4) 0.0679(17) Uani 1 1 d . . . 
H14A H 0.4584 1.0416 0.7021 0.081 Uiso 1 1 calc R . . 
C15 C 0.5227(4) 1.0095(7) 0.7870(4) 0.076(2) Uani 1 1 d . . . 
H15A H 0.5626 1.0357 0.7635 0.091 Uiso 1 1 calc R . . 
C16 C 0.5253(4) 0.9667(6) 0.8593(4) 0.0639(16) Uani 1 1 d . . . 
H16A H 0.5670 0.9652 0.8840 0.077 Uiso 1 1 calc R . . 
C20 C 0.6903(5) 0.3049(11) 0.8070(6) 0.104(3) Uani 1 1 d . . . 
H20A H 0.6541 0.3335 0.7736 0.124 Uiso 1 1 calc R . . 
C21 C 0.5478(3) 0.9135(5) 1.0278(3) 0.0492(12) Uani 1 1 d . . . 
C22 C 0.5875(3) 0.8190(6) 1.0613(4) 0.0573(16) Uani 1 1 d . . . 
H22A H 0.5715 0.7358 1.0630 0.069 Uiso 1 1 calc R . . 
C23 C 0.6505(4) 0.8491(9) 1.0917(4) 0.076(2) Uani 1 1 d . . . 
H23A H 0.6770 0.7859 1.1132 0.091 Uiso 1 1 calc R . . 
C24 C 0.6737(4) 0.9717(9) 1.0901(4) 0.080(2) Uani 1 1 d . . . 
H24A H 0.7155 0.9915 1.1118 0.096 Uiso 1 1 calc R . . 
C25 C 0.6365(4) 1.0652(8) 1.0574(5) 0.078(2) Uani 1 1 d . . . 
H25A H 0.6529 1.1483 1.0568 0.093 Uiso 1 1 calc R . . 
C26 C 0.5734(3) 1.0362(6) 1.0247(4) 0.0622(15) Uani 1 1 d . . . 
H26A H 0.5486 1.0994 1.0008 0.075 Uiso 1 1 calc R . . 
C31 C 0.3978(3) 0.9459(5) 1.0351(3) 0.0479(11) Uani 1 1 d . . . 
C32 C 0.3318(3) 0.9025(6) 1.0245(4) 0.0626(15) Uani 1 1 d . . . 
H32A H 0.3242 0.8296 0.9968 0.075 Uiso 1 1 calc R . . 
C33 C 0.2774(4) 0.9667(8) 1.0549(5) 0.079(2) Uani 1 1 d . . . 
H33A H 0.2327 0.9389 1.0466 0.095 Uiso 1 1 calc R . . 
C34 C 0.2893(4) 1.0723(8) 1.0974(5) 0.086(2) Uani 1 1 d . . . 
H34A H 0.2525 1.1141 1.1192 0.103 Uiso 1 1 calc R . . 
C35 C 0.3548(4) 1.1171(6) 1.1081(5) 0.073(2) Uani 1 1 d . . . 
H35A H 0.3621 1.1902 1.1357 0.087 Uiso 1 1 calc R . . 
C36 C 0.4091(3) 1.0535(5) 1.0780(6) 0.0644(15) Uani 1 1 d . . . 
H36A H 0.4536 1.0821 1.0861 0.077 Uiso 1 1 calc R . . 
C30 C 0.7364(7) 0.8651(13) 0.8347(10) 0.139(5) Uani 1 1 d . . . 
H30 H 0.7186 0.9452 0.8149 0.166 Uiso 1 1 calc R . . 
  
  
_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 N2 2.034(5) . ? 
Pd1 N1 2.060(5) . ? 
Pd1 Cl2 2.2738(15) . ? 
Pd1 Cl1 2.2903(15) . ? 
P1 N1 1.622(5) . ? 
P1 C21 1.788(6) . ? 
P1 C31 1.801(5) . ? 
P1 C11 1.817(6) . ? 
N2 C1 1.319(8) . ? 
N2 C5 1.376(8) . ? 
C1 C2 1.407(10) . ? 
N1 C6 1.412(7) . ? 
C2 C3 1.353(13) . ? 
C3 C4 1.435(12) . ? 
Cl3 C10 1.756(11) . ? 
C4 C9 1.406(11) . ? 
C4 C5 1.406(8) . ? 
Cl4 C10 1.737(11) . ? 
C5 C6 1.432(8) . ? 
Cl5 C10 1.752(9) . ? 
C6 C7 1.355(9) . ? 
Cl6 C20 1.698(10) . ? 
C7 C8 1.411(10) . ? 
Cl7 C20 1.725(13) . ? 
C8 C9 1.329(12) . ? 
Cl8 C20 1.707(13) . ? 
Cl9 C30 1.597(18) . ? 
Cl10 C30 1.724(17) . ? 
C11 C12 1.387(8) . ? 
C11 C16 1.387(9) . ? 
Cl11 C30 1.559(16) . ? 
C12 C13 1.349(9) . ? 
C13 C14 1.400(11) . ? 
C14 C15 1.382(11) . ? 
C15 C16 1.394(10) . ? 
C21 C26 1.384(8) . ? 
C21 C22 1.399(8) . ? 
C22 C23 1.383(10) . ? 
C23 C24 1.366(12) . ? 
C24 C25 1.359(12) . ? 
C25 C26 1.401(10) . ? 
C31 C32 1.379(9) . ? 
C31 C36 1.393(10) . ? 
C32 C33 1.375(10) . ? 
C33 C34 1.374(12) . ? 
C34 C35 1.375(12) . ? 
C35 C36 1.368(10) . ? 
  
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 
N2 Pd1 N1 80.5(2) . . ? 
N2 Pd1 Cl2 170.63(15) . . ? 
N1 Pd1 Cl2 95.51(13) . . ? 
N2 Pd1 Cl1 93.62(15) . . ? 
N1 Pd1 Cl1 173.73(14) . . ? 
Cl2 Pd1 Cl1 89.91(6) . . ? 
N1 P1 C21 113.2(3) . . ? 
N1 P1 C31 108.6(2) . . ? 
C21 P1 C31 110.5(3) . . ? 
N1 P1 C11 110.6(3) . . ? 
C21 P1 C11 107.5(3) . . ? 
C31 P1 C11 106.3(3) . . ? 
C1 N2 C5 120.0(5) . . ? 
C1 N2 Pd1 127.5(5) . . ? 
C5 N2 Pd1 111.1(4) . . ? 
N2 C1 C2 121.6(8) . . ? 
C6 N1 P1 123.7(4) . . ? 
C6 N1 Pd1 109.5(4) . . ? 
P1 N1 Pd1 126.7(3) . . ? 
C3 C2 C1 119.8(7) . . ? 
C2 C3 C4 120.3(6) . . ? 
C9 C4 C5 118.6(7) . . ? 
C9 C4 C3 125.0(7) . . ? 
C5 C4 C3 116.4(7) . . ? 
N2 C5 C4 121.7(6) . . ? 
N2 C5 C6 117.3(5) . . ? 
C4 C5 C6 120.9(6) . . ? 
C7 C6 N1 128.0(6) . . ? 
C7 C6 C5 117.9(6) . . ? 
N1 C6 C5 114.1(5) . . ? 
C6 C7 C8 119.9(7) . . ? 
C9 C8 C7 123.2(7) . . ? 
C8 C9 C4 119.3(6) . . ? 
Cl4 C10 Cl5 111.7(5) . . ? 
Cl4 C10 Cl3 108.6(5) . . ? 
Cl5 C10 Cl3 109.7(6) . . ? 
C12 C11 C16 118.5(6) . . ? 
C12 C11 P1 119.7(4) . . ? 
C16 C11 P1 121.9(5) . . ? 
C13 C12 C11 121.6(6) . . ? 
C12 C13 C14 120.5(6) . . ? 
C15 C14 C13 119.1(6) . . ? 
C14 C15 C16 119.9(7) . . ? 
C11 C16 C15 120.5(7) . . ? 
Cl6 C20 Cl8 111.6(7) . . ? 
Cl6 C20 Cl7 108.3(7) . . ? 
Cl8 C20 Cl7 109.1(6) . . ? 
C26 C21 C22 118.7(6) . . ? 
C26 C21 P1 123.2(5) . . ? 
C22 C21 P1 118.1(4) . . ? 
C23 C22 C21 120.2(6) . . ? 
C24 C23 C22 120.1(7) . . ? 
C25 C24 C23 121.1(7) . . ? 
C24 C25 C26 119.8(7) . . ? 
C21 C26 C25 120.1(7) . . ? 
C32 C31 C36 119.7(5) . . ? 
C32 C31 P1 119.1(5) . . ? 
C36 C31 P1 121.0(4) . . ? 
C33 C32 C31 120.1(7) . . ? 
C34 C33 C32 119.6(7) . . ? 
C35 C34 C33 120.9(6) . . ? 
C36 C35 C34 119.7(7) . . ? 
C35 C36 C31 120.0(6) . . ? 
Cl11 C30 Cl9 103.6(12) . . ? 
Cl11 C30 Cl10 96.7(10) . . ? 
Cl9 C30 Cl10 121.4(9) . . ? 
  
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.669 
_refine_diff_density_min   -0.578 
_refine_diff_density_rms    0.081 
