Preparation and properties of molybdenum and tungsten dinitrogen complexes. XLII. Preparation and characterization of W(V) diazoalkane complexes mer,trans- (X=Br, I; R=Me, Ph) and hydrazido(2-) complex . X-ray structure of mer,trans-<WBr3(NN=...

Article abstract of DOI:10.1016/0022-328X(93)83272-W

Reactions of W(IV) diazoalkane complexes cis,mer- (X=Br, I; R=Me, Ph) and hydrazido(2-) complex cis,mer- with five equivalents of CH2X2 in toluene at 80 deg C gave paramagnetic W(V) complexes, mer,trans- and respectively.The latter complex was also obtained upon hydrolysis of a W(V) disilylhydrazido(2-) complex and was converted into mer,trans- by the subsequent condensation with RMeC=O.The structure of mer,trans- (6d) was determined by X-ray analysis.Crystal data for 6d are as follows: monoclinic, space group P2₁/n with a=9.900(3) Angstroem, b=21.029(4) Angstroem, c=13.950(2) Angstroem, β=96.80(2)^o, V=2883.9(11) Angstroem³, Z=4 and R=0.060 for 4567 reflections.