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

  
data_kns21m 
  
  
_audit_creation_method            SHELXL-97
_publ_contact_author_name          'joshi hemant and Singh A. K.'
_publ_contact_author_address     
; 
      Department of Chemistry 
      Indian Institute of Technology
      Hauz Khas, New Delhi 110016
      India
; 
_publ_contact_author_email     'aksingh@chemistry.iitd.ac.in'
_publ_contact_author_fax     '+91-11-26582277'
_publ_contact_author_phone     '+91-11-26591507'
_chemical_name_systematic  
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety         'C15 H16 Cl2 O Pd S2' 
_chemical_formula_sum 
 'C15 H16 Cl2 O Pd S2' 
_chemical_formula_weight          453.72 
  
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 '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    'P b c a'
_symmetry_space_group_name_Hall   '-P 2ac 2ab'  
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z-1/2' 
 '-x-1/2, y-1/2, z' 
  
_cell_length_a                    8.117(3) 
_cell_length_b                    20.123(8) 
_cell_length_c                    20.541(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3355(2) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     8442 
_cell_measurement_theta_min       2.25 
_cell_measurement_theta_max       27.33 
  
_exptl_crystal_description        rod 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.32 
_exptl_crystal_size_mid           0.26 
_exptl_crystal_size_min           0.21 
_exptl_crystal_density_meas       1.796 
_exptl_crystal_density_diffrn     1.796 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1808.0 
_exptl_absorpt_coefficient_mu     1.668 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.597 
_exptl_absorpt_correction_T_max   0.707 
_exptl_absorpt_process_details    '(SADABS; Sheldrick, 1996)'
  
_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   '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             28910 
_diffrn_reflns_av_R_equivalents   0.0589 
_diffrn_reflns_av_sigmaI/netI     0.0254 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -23 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          1.98 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              2959 
_reflns_number_gt                 2395 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_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)+(0.0640P)²+6.5338P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2959 
_refine_ls_number_parameters      191 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0547 
_refine_ls_R_factor_gt            0.0426 
_refine_ls_wR_factor_ref          0.1191 
_refine_ls_wR_factor_gt           0.1124 
_refine_ls_goodness_of_fit_ref    1.068 
_refine_ls_restrained_S_all       1.068 
_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 
Pd1 Pd -0.11989(4) 0.036876(18) 0.59977(2) 0.04116(17) Uani 1 1 d . . . 
S1 S 0.02896(15) 0.11382(6) 0.65591(7) 0.0459(3) Uani 1 1 d . . . 
S2 S 0.07631(16) -0.04232(6) 0.58311(7) 0.0429(3) Uani 1 1 d . . . 
Cl1 Cl -0.33568(17) 0.11059(7) 0.61512(11) 0.0768(6) Uani 1 1 d . . . 
Cl2 Cl -0.29248(17) -0.03841(7) 0.54920(8) 0.0608(4) Uani 1 1 d . . . 
O1 O 0.4434(6) 0.0167(3) 0.7019(3) 0.0826(14) Uani 1 1 d . . . 
H1 H 0.4382 0.0069 0.7406 0.124 Uiso 1 1 calc R . . 
C1 C 0.0341(6) 0.1875(2) 0.6078(2) 0.0387(11) Uani 1 1 d . . . 
C2 C -0.0494(6) 0.2421(2) 0.6325(3) 0.0437(11) Uani 1 1 d . . . 
H2 H -0.1041 0.2389 0.6721 0.052 Uiso 1 1 calc R . . 
C3 C -0.0515(7) 0.3010(3) 0.5982(3) 0.0516(13) Uani 1 1 d . . . 
H3 H -0.1080 0.3375 0.6147 0.062 Uiso 1 1 calc R . . 
C4 C 0.0295(7) 0.3058(3) 0.5400(3) 0.0509(13) Uani 1 1 d . . . 
H4 H 0.0290 0.3458 0.5174 0.061 Uiso 1 1 calc R . . 
C5 C 0.1114(6) 0.2522(3) 0.5149(3) 0.0515(13) Uani 1 1 d . . . 
H5 H 0.1656 0.2560 0.4752 0.062 Uiso 1 1 calc R . . 
C6 C 0.1144(6) 0.1922(3) 0.5481(3) 0.0488(13) Uani 1 1 d . . . 
H6 H 0.1691 0.1556 0.5307 0.059 Uiso 1 1 calc R . . 
C7 C 0.2478(7) 0.0947(3) 0.6613(3) 0.0645(17) Uani 1 1 d . . . 
H7A H 0.2999 0.1063 0.6203 0.077 Uiso 1 1 calc R . . 
H7B H 0.2966 0.1221 0.6950 0.077 Uiso 1 1 calc R . . 
C8 C 0.2855(6) 0.0213(3) 0.6765(3) 0.0517(14) Uani 1 1 d . . . 
H8 H 0.2059 0.0044 0.7083 0.062 Uiso 1 1 calc R . . 
C9 C 0.2788(6) -0.0209(3) 0.6155(3) 0.0543(14) Uani 1 1 d . . . 
H9A H 0.3373 -0.0620 0.6242 0.065 Uiso 1 1 calc R . . 
H9B H 0.3392 0.0022 0.5816 0.065 Uiso 1 1 calc R . . 
C10 C 0.0185(6) -0.1096(2) 0.6357(2) 0.0388(11) Uani 1 1 d . . . 
C12 C 0.0242(9) -0.2265(3) 0.6534(4) 0.073(2) Uani 1 1 d . . . 
H12 H 0.0581 -0.2687 0.6406 0.087 Uiso 1 1 calc R . . 
C13 C -0.0665(9) -0.2194(3) 0.7079(4) 0.0679(18) Uani 1 1 d . . . 
H13 H -0.0959 -0.2565 0.7323 0.081 Uiso 1 1 calc R . . 
C14 C -0.1152(8) -0.1574(3) 0.7273(3) 0.0704(19) Uani 1 1 d . . . 
H14 H -0.1781 -0.1526 0.7649 0.084 Uiso 1 1 calc R . . 
C15 C -0.0714(7) -0.1018(3) 0.6914(3) 0.0539(14) Uani 1 1 d . . . 
H15 H -0.1031 -0.0596 0.7050 0.065 Uiso 1 1 calc R . . 
C11 C 0.0675(7) -0.1719(3) 0.6164(3) 0.0549(14) Uani 1 1 d . . . 
H11 H 0.1293 -0.1772 0.5787 0.066 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 S1 2.2775(15) . ? 
Pd1 S2 2.2788(14) . ? 
Pd1 Cl2 2.3102(15) . ? 
Pd1 Cl1 2.3168(16) . ? 
S1 C1 1.782(5) . ? 
S1 C7 1.821(6) . ? 
S2 C10 1.794(5) . ? 
S2 C9 1.825(6) . ? 
O1 C8 1.387(7) . ? 
O1 H1 0.8200 . ? 
C1 C2 1.386(7) . ? 
C1 C6 1.392(7) . ? 
C2 C3 1.379(7) . ? 
C2 H2 0.9300 . ? 
C3 C4 1.367(8) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.368(8) . ? 
C4 H4 0.9300 . ? 
C5 C6 1.387(8) . ? 
C5 H5 0.9300 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.540(7) . ? 
C7 H7A 0.9700 . ? 
C7 H7B 0.9700 . ? 
C8 C9 1.514(8) . ? 
C8 H8 0.9800 . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C10 C15 1.365(7) . ? 
C10 C11 1.374(7) . ? 
C12 C13 1.347(10) . ? 
C12 C11 1.383(9) . ? 
C12 H12 0.9300 . ? 
C13 C14 1.367(9) . ? 
C13 H13 0.9300 . ? 
C14 C15 1.388(8) . ? 
C14 H14 0.9300 . ? 
C15 H15 0.9300 . ? 
C11 H11 0.9300 . ? 
  
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 
S1 Pd1 S2 100.41(5) . . ? 
S1 Pd1 Cl2 174.40(6) . . ? 
S2 Pd1 Cl2 84.12(6) . . ? 
S1 Pd1 Cl1 84.08(6) . . ? 
S2 Pd1 Cl1 175.22(5) . . ? 
Cl2 Pd1 Cl1 91.30(7) . . ? 
C1 S1 C7 100.8(2) . . ? 
C1 S1 Pd1 107.29(16) . . ? 
C7 S1 Pd1 113.9(2) . . ? 
C10 S2 C9 101.2(2) . . ? 
C10 S2 Pd1 104.73(16) . . ? 
C9 S2 Pd1 114.18(19) . . ? 
C8 O1 H1 109.5 . . ? 
C2 C1 C6 119.8(5) . . ? 
C2 C1 S1 116.4(4) . . ? 
C6 C1 S1 123.7(4) . . ? 
C3 C2 C1 120.0(5) . . ? 
C3 C2 H2 120.0 . . ? 
C1 C2 H2 120.0 . . ? 
C4 C3 C2 120.1(5) . . ? 
C4 C3 H3 120.0 . . ? 
C2 C3 H3 120.0 . . ? 
C3 C4 C5 120.4(5) . . ? 
C3 C4 H4 119.8 . . ? 
C5 C4 H4 119.8 . . ? 
C4 C5 C6 120.7(5) . . ? 
C4 C5 H5 119.6 . . ? 
C6 C5 H5 119.6 . . ? 
C5 C6 C1 118.9(5) . . ? 
C5 C6 H6 120.6 . . ? 
C1 C6 H6 120.6 . . ? 
C8 C7 S1 114.1(4) . . ? 
C8 C7 H7A 108.7 . . ? 
S1 C7 H7A 108.7 . . ? 
C8 C7 H7B 108.7 . . ? 
S1 C7 H7B 108.7 . . ? 
H7A C7 H7B 107.6 . . ? 
O1 C8 C9 107.9(5) . . ? 
O1 C8 C7 108.9(4) . . ? 
C9 C8 C7 111.3(5) . . ? 
O1 C8 H8 109.6 . . ? 
C9 C8 H8 109.6 . . ? 
C7 C8 H8 109.6 . . ? 
C8 C9 S2 117.8(4) . . ? 
C8 C9 H9A 107.9 . . ? 
S2 C9 H9A 107.9 . . ? 
C8 C9 H9B 107.9 . . ? 
S2 C9 H9B 107.9 . . ? 
H9A C9 H9B 107.2 . . ? 
C15 C10 C11 120.1(5) . . ? 
C15 C10 S2 123.9(4) . . ? 
C11 C10 S2 116.0(4) . . ? 
C13 C12 C11 120.7(6) . . ? 
C13 C12 H12 119.6 . . ? 
C11 C12 H12 119.6 . . ? 
C12 C13 C14 119.8(6) . . ? 
C12 C13 H13 120.1 . . ? 
C14 C13 H13 120.1 . . ? 
C13 C14 C15 120.5(6) . . ? 
C13 C14 H14 119.8 . . ? 
C15 C14 H14 119.8 . . ? 
C10 C15 C14 119.3(5) . . ? 
C10 C15 H15 120.4 . . ? 
C14 C15 H15 120.4 . . ? 
C10 C11 C12 119.6(6) . . ? 
C10 C11 H11 120.2 . . ? 
C12 C11 H11 120.2 . . ? 
  
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 
S2 Pd1 S1 C1 117.15(17) . . . . ? 
Cl2 Pd1 S1 C1 -99.0(5) . . . . ? 
Cl1 Pd1 S1 C1 -64.49(18) . . . . ? 
S2 Pd1 S1 C7 6.6(2) . . . . ? 
Cl2 Pd1 S1 C7 150.4(5) . . . . ? 
Cl1 Pd1 S1 C7 -175.1(2) . . . . ? 
S1 Pd1 S2 C10 108.42(17) . . . . ? 
Cl2 Pd1 S2 C10 -68.26(17) . . . . ? 
Cl1 Pd1 S2 C10 -51.5(8) . . . . ? 
S1 Pd1 S2 C9 -1.3(2) . . . . ? 
Cl2 Pd1 S2 C9 -178.0(2) . . . . ? 
Cl1 Pd1 S2 C9 -161.3(8) . . . . ? 
C7 S1 C1 C2 -127.8(4) . . . . ? 
Pd1 S1 C1 C2 112.8(4) . . . . ? 
C7 S1 C1 C6 52.9(5) . . . . ? 
Pd1 S1 C1 C6 -66.5(4) . . . . ? 
C6 C1 C2 C3 -0.7(7) . . . . ? 
S1 C1 C2 C3 180.0(4) . . . . ? 
C1 C2 C3 C4 -0.3(8) . . . . ? 
C2 C3 C4 C5 0.8(8) . . . . ? 
C3 C4 C5 C6 -0.3(8) . . . . ? 
C4 C5 C6 C1 -0.7(8) . . . . ? 
C2 C1 C6 C5 1.1(7) . . . . ? 
S1 C1 C6 C5 -179.6(4) . . . . ? 
C1 S1 C7 C8 -157.6(5) . . . . ? 
Pd1 S1 C7 C8 -43.1(5) . . . . ? 
S1 C7 C8 O1 -159.0(5) . . . . ? 
S1 C7 C8 C9 82.2(6) . . . . ? 
O1 C8 C9 S2 164.3(4) . . . . ? 
C7 C8 C9 S2 -76.3(5) . . . . ? 
C10 S2 C9 C8 -79.6(4) . . . . ? 
Pd1 S2 C9 C8 32.3(5) . . . . ? 
C9 S2 C10 C15 92.9(5) . . . . ? 
Pd1 S2 C10 C15 -26.0(5) . . . . ? 
C9 S2 C10 C11 -88.4(5) . . . . ? 
Pd1 S2 C10 C11 152.7(4) . . . . ? 
C11 C12 C13 C14 -0.6(10) . . . . ? 
C12 C13 C14 C15 -0.2(10) . . . . ? 
C11 C10 C15 C14 -1.2(8) . . . . ? 
S2 C10 C15 C14 177.5(4) . . . . ? 
C13 C14 C15 C10 1.1(9) . . . . ? 
C15 C10 C11 C12 0.4(8) . . . . ? 
S2 C10 C11 C12 -178.4(5) . . . . ? 
C13 C12 C11 C10 0.5(9) . . . . ? 
  
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    1.476 
_refine_diff_density_min   -0.639 
_refine_diff_density_rms    0.122 
