Bis(carbonyl-κC)(N,N-dimethylthiocarbamoyl-κ2 C,S)(pyridine-2-thiolato-κ2 N,S)(triphenylphosphine-κP)molybdenum(II)

There are two independent molecules with similar configurations in the title complex, [Mo(C3H6NS)(C5H4NS)(C18H15P)(CO)2]. The geometry around the metal atom is that of a capped octahedron. The thiocabamoyl and pyridine-2-thiolate ligands coordinate to the molybdenum metal center through the C and S atoms, and N and S atoms, respectively. NMR, IR and MS analyses are in agreement with the structure of the title compound.

There are two independent molecules with similar configurations in the title complex, [Mo(C 3 H 6 NS)(C 5 H 4 NS)(C 18 H 15 P)-(CO) 2 ]. The geometry around the metal atom is that of a capped octahedron. The thiocabamoyl and pyridine-2-thiolate ligands coordinate to the molybdenum metal center through the C and S atoms, and N and S atoms, respectively. NMR, IR and MS analyses are in agreement with the structure of the title compound.

Ilsley
To synthesis of seven coordinated and NS-coordinated metal compound, complex [Mo(CO) 2 (SCNMe 2 )(PPh 3 ) 2 Cl] was used to react with C 5 H 4 NSH in dichloromethane at room temperature. As a result, a chloride and triphenylphosphine displaced complex [Mo(CO) 2 (SNC 5 H 4 )(SCNMe 2 )(PPh 3 )] was isolated with 82% yield. The X-ray crystal structure analysis has been carried out to provide structural parameters.
In the 1 H NMR spectrum of (I), three protons of the SNC 5 H 4 ligand exhibits one doublet resonance at δ 6.21 and two triplet resonances at δ 6.46, 6.88 with ratio of 1:1:1. Two methyl resonances at δ 3.55 and δ 3.78 of the SCNMe 2 ligand are observed in the 1 H NMR spectra of complex (I), consistent with hindered rotation about the partially multiple C-N bond.
In the 13 C{ 1 H} NMR spectrum of (I), two singlet resonances appear at δ 45.2, δ 50.4 for the carbon atoms of N-methyl groups, respectively. Three singlet resonances appear at δ 176.8, 235.1 and 248.0 for the carbon atom of the NCS, CO and Me 2 NCS groups, respectively. The 31 P{ 1 H} NMR spectrum of (I) shows one resonance at δ 48.5.
It is also noted the IR spectrum of the title complex (I) shows five stretching bands at 1921 and 1824 cm -1 for C=O, at 1563 cm -1 for C=N, at 1481 and 1434 cm -1 for C=S groups. In the FAB mass spectra, base peak with the typical Mo isotope distribution is in agreement with the [M + ] molecular mass of (I).

Experimental
The synthesis of the title compound (I) was carried out as follows. CH 2 Cl 2 (10 ml) was added to a flask (100 ml) containing C 5 H 4 NSH (0.111 g, 1.0 mmol) and [Mo(CO) 2 (SCNMe 2 )(PPh 3 ) 2 Cl] (0.800 g, 1.0 mmol). The solution was stirred for 10 min at room temperature. The solution is concentrated under vacuum and MeOH (10 ml) was added to initiate precipitation. The orange solids were isolated by filtration (G4), washed with diethyl ether (2 x 10 ml) and subsequently drying under vacuum yielding [Mo(CO) 2 (SNC 5 H 4 )(SCNMe 2 )(PPh 3 )] (0.501 g, 82%). Further purification was accomplished by recrystallization from 1/10 CH 2 Cl 2 /n-hexane. The orange crystals of (I) for X-ray structure analysis were obtained by slow diffusion of n-hexane into the CH 2 Cl 2 solution of the title compound at room temperature for 3 days.  Fig. 1. The molecular structure of (I), showing two independent molecules and the 50% probability displacement ellipsoids.