Inner-sphere hydrolysis of ethyl isothiocyanate in MoCl4{[N(Et)C(S)](2)Cl}: Crystal structure of the product of hydrolysis, ethylammonium aquatetrachlorooxomolybdate(V) (NH3Et)[MoOCl4(H2O)]

The product of insertion MoCl4{[N(Et)C(S)](2)Cl} (I) was obtained by reacting MoCl5 with EtNCS in dichloroethane. The hydrolysis of this complex gave single crystals of (NH3Et)[MoOCl4(H2O)] (II), which were characterized by X-ray crystallography. The crystals of II consist of complex anions [(MoOCl4)-O-V(H2O)](-) and ethylammonium cations united by an extended network of interionic contacts N-H...Cl N-H...O, and C-H...O. The bond lengths in the coordination octahedron MoO2Cl4: Mo=O(oxo), 1.67 Angstrom; Mo-O(H2O)(trans), 2.381 Angstrom, and Mo-Cl-cis, 2.365 Angstrom. On the basis of the X-ray diffraction data, the assignment of the frequencies in the IR spectra of II was performed. The results of the X-ray diffraction study and IR spectroscopy for I allowed us to conclude that the addition of ethyl isothiocyanate to pentachloromolybdenum(V) is stereospecific.