Crystal structure of bis[S-hexyl 3-(4-methylbenzylidene)dithiocarbazato-κ2 N 3,S]palladium(II)

The whole molecule of the title complex, [Pd(C15H21N2S2)2], is generated by twofold rotational symmetry. The palladium(II) atom exhibits a square-planar coordination geometry, and is located on the crystallographic twofold axis that induces a cis configuration of the N,S chelating ligands. In the crystal, molecules stack along the c-axis direction and there are no significant intermolecular interactions present. The structure was refined as an inversion twin with a final BASF parameter of 0.34 (2).


S2. Refinement
Crystal data, data collection and structure refinement details are summarized in Table 1. All H atoms were fixed geometrically (C-H = 0.95 -0.99 Å) and refined as riding, with U iso (H) =1.2 U eq (C). The rather high R factor is affected by the small crystal dimensions and consequently by low diffraction at high θ angles. The collected data were cut at a resolution of 0.85 Å. The structure was refined as an inversion twin with a final BASF parameter = 0.34 (2).
In the crystal, there are no significant intermolecular interactions present. The molecules pack along the c axis direction  A view of the molecular structure of the title complex, with atom labelling (symmetry code: (i) -x + 1, y, -z).
Displacement ellipsoids are drawn at the 50% probability level.

Figure 2
Crystal packing of the title complex viewed along the b axis.

Bis[S-hexyl 3-(4-methylbenzylidene)dithiocarbazato-κ 2 N 3 ,S]palladium(II)
Crystal data [Pd(C 15  where P = (F o 2 + 2F c 2 )/3 (Δ/σ) max < 0.001 Δρ max = 2.07 e Å −3 Δρ min = −1.31 e Å −3 Absolute structure: Flack (1983), 1218 Friedel pairs Absolute structure parameter: 0.34 (2) Special details Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > 2σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.