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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H15 Cl2 N3 Pd Se'
_chemical_formula_sum            'C16 H15 Cl2 N3 Pd Se '
_chemical_formula_weight         505.57

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'
Se Se -0.0929 2.2259 '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)
_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'

_cell_length_a                   8.8269(19)
_cell_length_b                   9.289(2)
_cell_length_c                   20.716(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1698.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4205
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      23.63

_exptl_crystal_description       Rods
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.227
_exptl_crystal_density_meas      1.977
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984.0
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.036
_exptl_absorpt_correction_T_max  0.072
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_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  '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            16232
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2998
_reflns_number_gt                2826
_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)+(0.0337P)²+0.8040P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(15)
_refine_ls_number_reflns         2998
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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
C4 C 0.7675(9) 0.0271(8) 0.1819(4) 0.058(2) Uani 1 1 d . . .
H4 H 0.8500 -0.0349 0.1849 0.070 Uiso 1 1 calc R . .
C5 C 0.7498(8) 0.1104(7) 0.1270(3) 0.0487(17) Uani 1 1 d . . .
H5 H 0.8182 0.1024 0.0931 0.058 Uiso 1 1 calc R . .
C1 C 0.5283(7) 0.2098(8) 0.1732(3) 0.0508(18) Uani 1 1 d . . .
H1 H 0.4453 0.2712 0.1706 0.061 Uiso 1 1 calc R . .
C11 C 0.2049(6) 0.9741(6) 0.1510(3) 0.0359(14) Uani 1 1 d . . .
C6 C 0.6307(7) 0.2050(6) 0.1230(3) 0.0386(14) Uani 1 1 d . . .
C16 C 0.1673(7) 1.1179(6) 0.1459(3) 0.0409(15) Uani 1 1 d . . .
H16 H 0.1715 1.1649 0.1063 0.049 Uiso 1 1 calc R . .
C12 C 0.1987(7) 0.9032(7) 0.2082(3) 0.0458(16) Uani 1 1 d . . .
H12 H 0.2219 0.8056 0.2102 0.055 Uiso 1 1 calc R . .
C7 C 0.6115(8) 0.2891(7) 0.0615(3) 0.0454(16) Uani 1 1 d . . .
H7A H 0.7106 0.3075 0.0430 0.054 Uiso 1 1 calc R . .
H7B H 0.5547 0.2314 0.0308 0.054 Uiso 1 1 calc R . .
N2 N 0.3809(5) 0.4325(5) 0.0667(3) 0.0392(11) Uani 1 1 d . . .
N1 N 0.5324(5) 0.4279(5) 0.0710(3) 0.0428(12) Uani 1 1 d . . .
C8 C 0.5953(6) 0.5541(6) 0.0855(3) 0.0366(15) Uani 1 1 d . . .
H8 H 0.6975 0.5749 0.0912 0.044 Uiso 1 1 calc R . .
Pd1 Pd 0.13857(4) 0.65645(4) 0.07276(2) 0.02957(13) Uani 1 1 d . . .
Se1 Se 0.26923(6) 0.87925(6) 0.07207(3) 0.03745(16) Uani 1 1 d . . .
Cl2 Cl 0.00876(17) 0.44003(16) 0.07008(9) 0.0478(4) Uani 1 1 d . . .
Cl1 Cl -0.08234(16) 0.78258(16) 0.06545(8) 0.0430(4) Uani 1 1 d . . .
C10 C 0.4674(7) 0.8036(7) 0.1020(3) 0.0448(16) Uani 1 1 d . . .
H10A H 0.5490 0.8512 0.0790 0.054 Uiso 1 1 calc R . .
H10B H 0.4797 0.8228 0.1478 0.054 Uiso 1 1 calc R . .
N3 N 0.3446(5) 0.5674(5) 0.0807(2) 0.0368(11) Uani 1 1 d . . .
C9 C 0.4739(6) 0.6468(7) 0.0902(3) 0.0350(14) Uani 1 1 d . . .
C13 C 0.1578(7) 0.9766(8) 0.2638(3) 0.0486(17) Uani 1 1 d . . .
H13 H 0.1560 0.9300 0.3035 0.058 Uiso 1 1 calc R . .
C3 C 0.6664(9) 0.0341(8) 0.2316(4) 0.060(2) Uani 1 1 d . . .
H3 H 0.6791 -0.0228 0.2682 0.072 Uiso 1 1 calc R . .
C15 C 0.1234(8) 1.1901(8) 0.2010(4) 0.0563(19) Uani 1 1 d . . .
H15 H 0.0961 1.2867 0.1989 0.068 Uiso 1 1 calc R . .
C2 C 0.5470(8) 0.1255(9) 0.2269(4) 0.062(2) Uani 1 1 d . . .
H2 H 0.4772 0.1309 0.2604 0.074 Uiso 1 1 calc R . .
C14 C 0.1202(8) 1.1184(8) 0.2591(4) 0.0571(19) Uani 1 1 d . . .
H14 H 0.0915 1.1681 0.2961 0.068 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
C4 C3 1.365(10) . ?
C4 C5 1.384(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(9) . ?
C5 H5 0.9300 . ?
C1 C2 1.369(10) . ?
C1 C6 1.378(8) . ?
C1 H1 0.9300 . ?
C11 C12 1.357(9) . ?
C11 C16 1.381(8) . ?
C11 Se1 1.942(6) . ?
C6 C7 1.506(8) . ?
C16 C15 1.380(9) . ?
C16 H16 0.9300 . ?
C12 C13 1.386(9) . ?
C12 H12 0.9300 . ?
C7 N1 1.479(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N2 N3 1.326(6) . ?
N2 N1 1.340(6) . ?
N1 C8 1.331(7) . ?
C8 C9 1.378(8) . ?
C8 H8 0.9300 . ?
Pd1 N3 2.005(4) . ?
Pd1 Cl1 2.2799(15) . ?
Pd1 Cl2 2.3146(16) . ?
Pd1 Se1 2.3693(8) . ?
Se1 C10 1.985(6) . ?
C10 C9 1.478(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N3 C9 1.373(7) . ?
C13 C14 1.362(10) . ?
C13 H13 0.9300 . ?
C3 C2 1.356(10) . ?
C3 H3 0.9300 . ?
C15 C14 1.375(10) . ?
C15 H15 0.9300 . ?
C2 H2 0.9300 . ?
C14 H14 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
C3 C4 C5 121.3(7) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.6(7) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C2 C1 C6 121.0(6) . . ?
C2 C1 H1 119.5 . . ?
C6 C1 H1 119.5 . . ?
C12 C11 C16 121.8(6) . . ?
C12 C11 Se1 121.8(5) . . ?
C16 C11 Se1 116.4(5) . . ?
C5 C6 C1 118.5(6) . . ?
C5 C6 C7 118.0(6) . . ?
C1 C6 C7 123.3(6) . . ?
C11 C16 C15 118.3(6) . . ?
C11 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C11 C12 C13 119.8(6) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
N1 C7 C6 113.1(5) . . ?
N1 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
N1 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N3 N2 N1 104.9(4) . . ?
C8 N1 N2 113.7(5) . . ?
C8 N1 C7 126.9(5) . . ?
N2 N1 C7 119.3(5) . . ?
N1 C8 C9 104.0(5) . . ?
N1 C8 H8 128.0 . . ?
C9 C8 H8 128.0 . . ?
N3 Pd1 Cl1 173.41(14) . . ?
N3 Pd1 Cl2 95.32(14) . . ?
Cl1 Pd1 Cl2 91.22(6) . . ?
N3 Pd1 Se1 85.37(13) . . ?
Cl1 Pd1 Se1 88.11(4) . . ?
Cl2 Pd1 Se1 178.20(5) . . ?
C11 Se1 C10 98.9(3) . . ?
C11 Se1 Pd1 104.41(17) . . ?
C10 Se1 Pd1 96.77(19) . . ?
C9 C10 Se1 109.3(4) . . ?
C9 C10 H10A 109.8 . . ?
Se1 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
Se1 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
N2 N3 C9 109.8(5) . . ?
N2 N3 Pd1 126.3(4) . . ?
C9 N3 Pd1 123.0(4) . . ?
N3 C9 C8 107.5(5) . . ?
N3 C9 C10 121.4(5) . . ?
C8 C9 C10 131.1(5) . . ?
C14 C13 C12 118.7(7) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C2 C3 C4 118.9(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C15 C16 119.7(7) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C3 C2 C1 120.7(7) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C13 C14 C15 121.7(7) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?

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
C3 C4 C5 C6 1.8(11) . . . . ?
C4 C5 C6 C1 -2.5(9) . . . . ?
C4 C5 C6 C7 -177.5(6) . . . . ?
C2 C1 C6 C5 1.9(10) . . . . ?
C2 C1 C6 C7 176.6(6) . . . . ?
C12 C11 C16 C15 0.4(9) . . . . ?
Se1 C11 C16 C15 -179.0(5) . . . . ?
C16 C11 C12 C13 -1.8(10) . . . . ?
Se1 C11 C12 C13 177.5(5) . . . . ?
C5 C6 C7 N1 -153.5(5) . . . . ?
C1 C6 C7 N1 31.7(9) . . . . ?
N3 N2 N1 C8 -1.5(8) . . . . ?
N3 N2 N1 C7 176.9(5) . . . . ?
C6 C7 N1 C8 88.7(8) . . . . ?
C6 C7 N1 N2 -89.4(8) . . . . ?
N2 N1 C8 C9 -0.6(7) . . . . ?
C7 N1 C8 C9 -178.8(6) . . . . ?
C12 C11 Se1 C10 -54.2(5) . . . . ?
C16 C11 Se1 C10 125.2(5) . . . . ?
C12 C11 Se1 Pd1 45.2(5) . . . . ?
C16 C11 Se1 Pd1 -135.4(4) . . . . ?
N3 Pd1 Se1 C11 -114.7(2) . . . . ?
Cl1 Pd1 Se1 C11 64.35(19) . . . . ?
Cl2 Pd1 Se1 C11 132.7(15) . . . . ?
N3 Pd1 Se1 C10 -13.7(2) . . . . ?
Cl1 Pd1 Se1 C10 165.39(19) . . . . ?
Cl2 Pd1 Se1 C10 -126.3(15) . . . . ?
C11 Se1 C10 C9 125.9(4) . . . . ?
Pd1 Se1 C10 C9 20.1(4) . . . . ?
N1 N2 N3 C9 3.1(7) . . . . ?
N1 N2 N3 Pd1 171.9(4) . . . . ?
Cl1 Pd1 N3 N2 -168.3(10) . . . . ?
Cl2 Pd1 N3 N2 18.5(5) . . . . ?
Se1 Pd1 N3 N2 -159.9(5) . . . . ?
Cl1 Pd1 N3 C9 -0.9(17) . . . . ?
Cl2 Pd1 N3 C9 -174.1(4) . . . . ?
Se1 Pd1 N3 C9 7.5(4) . . . . ?
N2 N3 C9 C8 -3.6(6) . . . . ?
Pd1 N3 C9 C8 -172.8(4) . . . . ?
N2 N3 C9 C10 175.6(5) . . . . ?
Pd1 N3 C9 C10 6.4(7) . . . . ?
N1 C8 C9 N3 2.5(6) . . . . ?
N1 C8 C9 C10 -176.6(6) . . . . ?
Se1 C10 C9 N3 -19.3(7) . . . . ?
Se1 C10 C9 C8 159.6(5) . . . . ?
C11 C12 C13 C14 1.9(10) . . . . ?
C5 C4 C3 C2 -0.4(11) . . . . ?
C11 C16 C15 C14 0.9(10) . . . . ?
C4 C3 C2 C1 -0.3(11) . . . . ?
C6 C1 C2 C3 -0.5(11) . . . . ?
C12 C13 C14 C15 -0.7(11) . . . . ?
C16 C15 C14 C13 -0.7(11) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 1013860'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H15 Cl2 N3 Pd S'
_chemical_formula_sum            'C16 H15 Cl2 N3 Pd S'
_chemical_formula_weight         458.68

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'
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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.482(3)
_cell_length_b                   11.062(4)
_cell_length_c                   18.913(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.849(6)
_cell_angle_gamma                90.00
_cell_volume                     1772.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5055
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.52

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      1.719
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912.0
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_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  '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            16478
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3116
_reflns_number_gt                2981
_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)+(0.0280P)²+3.7294P] 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         3116
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_restrained_S_all      1.276
_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 0.9847(7) 0.4522(6) 0.2303(3) 0.0615(16) Uani 1 1 d . . .
H1 H 1.0335 0.3916 0.2053 0.074 Uiso 1 1 calc R . .
C2 C 1.0000(10) 0.4538(7) 0.3028(4) 0.084(2) Uani 1 1 d . . .
H2 H 1.0603 0.3949 0.3266 0.101 Uiso 1 1 calc R . .
C3 C 0.9279(10) 0.5407(8) 0.3402(4) 0.084(2) Uani 1 1 d . . .
H3 H 0.9398 0.5417 0.3893 0.100 Uiso 1 1 calc R . .
C4 C 0.8385(10) 0.6259(7) 0.3059(4) 0.083(2) Uani 1 1 d . . .
H4 H 0.7877 0.6845 0.3317 0.099 Uiso 1 1 calc R . .
C5 C 0.8224(7) 0.6263(5) 0.2324(4) 0.0625(16) Uani 1 1 d . . .
H5 H 0.7609 0.6850 0.2091 0.075 Uiso 1 1 calc R . .
C6 C 0.8975(6) 0.5398(4) 0.1940(3) 0.0412(12) Uani 1 1 d . . .
C7 C 0.8874(6) 0.5426(5) 0.1146(3) 0.0439(12) Uani 1 1 d . . .
H7A H 0.8306 0.6148 0.0992 0.053 Uiso 1 1 calc R . .
H7B H 0.9934 0.5483 0.0978 0.053 Uiso 1 1 calc R . .
C8 C 0.8753(6) 0.3388(5) 0.0537(3) 0.0448(12) Uani 1 1 d . . .
H8 H 0.9825 0.3229 0.0512 0.054 Uiso 1 1 calc R . .
C9 C 0.7543(5) 0.2691(4) 0.0299(3) 0.0374(11) Uani 1 1 d . . .
C10 C 0.7438(6) 0.1491(5) -0.0056(3) 0.0500(13) Uani 1 1 d . . .
H10A H 0.7641 0.0858 0.0292 0.060 Uiso 1 1 calc R . .
H10B H 0.8237 0.1437 -0.0404 0.060 Uiso 1 1 calc R . .
C11 C 0.5724(6) 0.1911(5) -0.1345(3) 0.0428(12) Uani 1 1 d . . .
C12 C 0.6244(8) 0.3069(6) -0.1435(3) 0.0658(17) Uani 1 1 d . . .
H12 H 0.6436 0.3574 -0.1047 0.079 Uiso 1 1 calc R . .
C13 C 0.6480(9) 0.3475(7) -0.2112(3) 0.079(2) Uani 1 1 d . . .
H13 H 0.6881 0.4247 -0.2179 0.095 Uiso 1 1 calc R . .
C14 C 0.6131(9) 0.2754(7) -0.2685(3) 0.078(2) Uani 1 1 d . . .
H14 H 0.6285 0.3038 -0.3139 0.094 Uiso 1 1 calc R . .
C15 C 0.5552(9) 0.1613(7) -0.2591(3) 0.076(2) Uani 1 1 d . . .
H15 H 0.5285 0.1128 -0.2980 0.091 Uiso 1 1 calc R . .
C16 C 0.5369(8) 0.1190(6) -0.1920(3) 0.0598(16) Uani 1 1 d . . .
H16 H 0.5001 0.0408 -0.1854 0.072 Uiso 1 1 calc R . .
Cl1 Cl 0.18040(15) 0.16507(12) -0.02721(7) 0.0480(3) Uani 1 1 d . . .
Cl2 Cl 0.27359(14) 0.39916(12) 0.07803(7) 0.0447(3) Uani 1 1 d . . .
N1 N 0.8083(4) 0.4358(4) 0.0817(2) 0.0364(9) Uani 1 1 d . . .
N2 N 0.6524(4) 0.4318(4) 0.07642(19) 0.0361(9) Uani 1 1 d . . .
N3 N 0.6186(4) 0.3287(3) 0.04497(19) 0.0336(9) Uani 1 1 d . . .
Pd1 Pd 0.40789(4) 0.26035(3) 0.013332(18) 0.03216(13) Uani 1 1 d . . .
S1 S 0.54900(15) 0.12637(11) -0.04912(7) 0.0408(3) 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 C2 1.371(9) . ?
C1 C6 1.381(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.355(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.499(7) . ?
C7 N1 1.481(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N1 1.336(6) . ?
C8 C9 1.343(7) . ?
C8 H8 0.9300 . ?
C9 N3 1.368(6) . ?
C9 C10 1.489(7) . ?
C10 S1 1.826(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.368(8) . ?
C11 C16 1.370(7) . ?
C11 S1 1.786(5) . ?
C12 C13 1.381(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.369(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.368(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
Cl1 Pd1 2.2968(14) . ?
Cl2 Pd1 2.3003(13) . ?
N1 N2 1.322(5) . ?
N2 N3 1.312(5) . ?
N3 Pd1 2.005(4) . ?
Pd1 S1 2.2727(14) . ?

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
C2 C1 C6 120.7(6) . . ?
C2 C1 H1 119.6 . . ?
C6 C1 H1 119.6 . . ?
C3 C2 C1 120.5(7) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.0(6) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.3(7) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 118.4(5) . . ?
C5 C6 C7 120.6(5) . . ?
C1 C6 C7 121.0(5) . . ?
N1 C7 C6 114.0(4) . . ?
N1 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N1 C8 C9 105.1(4) . . ?
N1 C8 H8 127.4 . . ?
C9 C8 H8 127.4 . . ?
C8 C9 N3 106.9(4) . . ?
C8 C9 C10 133.7(5) . . ?
N3 C9 C10 119.4(4) . . ?
C9 C10 S1 111.0(3) . . ?
C9 C10 H10A 109.4 . . ?
S1 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
S1 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C16 120.3(5) . . ?
C12 C11 S1 122.7(4) . . ?
C16 C11 S1 117.0(4) . . ?
C11 C12 C13 118.9(6) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 120.6(7) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 120.0(6) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 119.6(6) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C11 120.4(6) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
N2 N1 C8 112.7(4) . . ?
N2 N1 C7 119.3(4) . . ?
C8 N1 C7 128.0(4) . . ?
N3 N2 N1 105.0(4) . . ?
N2 N3 C9 110.3(4) . . ?
N2 N3 Pd1 129.4(3) . . ?
C9 N3 Pd1 120.2(3) . . ?
N3 Pd1 S1 85.18(11) . . ?
N3 Pd1 Cl1 174.04(11) . . ?
S1 Pd1 Cl1 89.01(5) . . ?
N3 Pd1 Cl2 92.72(11) . . ?
S1 Pd1 Cl2 177.91(5) . . ?
Cl1 Pd1 Cl2 93.09(5) . . ?
C11 S1 C10 102.3(3) . . ?
C11 S1 Pd1 107.07(17) . . ?
C10 S1 Pd1 99.45(17) . . ?

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(11) . . . . ?
C1 C2 C3 C4 0.7(12) . . . . ?
C2 C3 C4 C5 -1.1(12) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C4 C5 C6 C1 1.5(9) . . . . ?
C4 C5 C6 C7 -177.1(5) . . . . ?
C2 C1 C6 C5 -2.0(9) . . . . ?
C2 C1 C6 C7 176.6(6) . . . . ?
C5 C6 C7 N1 -117.1(5) . . . . ?
C1 C6 C7 N1 64.3(7) . . . . ?
N1 C8 C9 N3 0.0(5) . . . . ?
N1 C8 C9 C10 -179.0(5) . . . . ?
C8 C9 C10 S1 -161.8(5) . . . . ?
N3 C9 C10 S1 19.3(6) . . . . ?
C16 C11 C12 C13 -3.3(10) . . . . ?
S1 C11 C12 C13 176.2(5) . . . . ?
C11 C12 C13 C14 3.0(11) . . . . ?
C12 C13 C14 C15 -0.5(12) . . . . ?
C13 C14 C15 C16 -1.8(12) . . . . ?
C14 C15 C16 C11 1.6(11) . . . . ?
C12 C11 C16 C15 1.0(10) . . . . ?
S1 C11 C16 C15 -178.6(5) . . . . ?
C9 C8 N1 N2 -0.5(6) . . . . ?
C9 C8 N1 C7 -179.0(4) . . . . ?
C6 C7 N1 N2 81.5(5) . . . . ?
C6 C7 N1 C8 -100.1(6) . . . . ?
C8 N1 N2 N3 0.8(5) . . . . ?
C7 N1 N2 N3 179.4(4) . . . . ?
N1 N2 N3 C9 -0.7(5) . . . . ?
N1 N2 N3 Pd1 -176.3(3) . . . . ?
C8 C9 N3 N2 0.4(5) . . . . ?
C10 C9 N3 N2 179.6(4) . . . . ?
C8 C9 N3 Pd1 176.5(3) . . . . ?
C10 C9 N3 Pd1 -4.3(6) . . . . ?
N2 N3 Pd1 S1 166.0(4) . . . . ?
C9 N3 Pd1 S1 -9.2(3) . . . . ?
N2 N3 Pd1 Cl1 179(27) . . . . ?
C9 N3 Pd1 Cl1 3.9(13) . . . . ?
N2 N3 Pd1 Cl2 -14.0(4) . . . . ?
C9 N3 Pd1 Cl2 170.8(3) . . . . ?
C12 C11 S1 C10 -54.5(6) . . . . ?
C16 C11 S1 C10 125.0(5) . . . . ?
C12 C11 S1 Pd1 49.5(5) . . . . ?
C16 C11 S1 Pd1 -131.0(4) . . . . ?
C9 C10 S1 C11 87.9(4) . . . . ?
C9 C10 S1 Pd1 -22.0(4) . . . . ?
N3 Pd1 S1 C11 -90.3(2) . . . . ?
Cl1 Pd1 S1 C11 91.00(18) . . . . ?
Cl2 Pd1 S1 C11 -90.4(14) . . . . ?
N3 Pd1 S1 C10 15.8(2) . . . . ?
Cl1 Pd1 S1 C10 -162.9(2) . . . . ?
Cl2 Pd1 S1 C10 15.7(14) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 1013861'
