Synthesis and characterization of molybdenum–tin complexes derived from the molybdenum tricarbonyl anion, [MeGapz 3 ]Mo(CO) 3 − , and organotin chlorides. X-ray crystal structure of [MeGapz 3 ]Mo(CO) 3 SnPh 3 (where pz = pyrazolyl, N 2 C 3 H 3 )

• Published in: Canadian journal of chemistry 1986-02, Vol.64 (2), p.321-327
• Main Authors: Onyiriuka, Emmanuel C., Rettig, Steven J., Storr, Alan
• Format: Article
• Language: English
• ISSN: 0008-4042; 1480-3291
• DOI: 10.1139/v86-054

The reaction of the molybdenum tricarbonyl anion, [MeGapz 3 ]Mo(CO) 3 − , with the organotin chlorides, Ph 3 SnCl, Me 3 SnCl, and Me 2 SnCl 2 , has yielded a series of complexes in which direct Mo—Sn single bonds are featured. The [MeGapz 3 ]Mo(CO) 3 SnMe 2 Cl complex shows an interesting solution behavior in which a transition from a 3:4, or piano stool structure, to a 3:3:1, or capped octahedral arrangement, is thought to occur. The 3:3:1 structure has been demonstrated in the solid state for the [MeGapz 3 ]Mo(CO) 3 SnPh 3 compound by means of a crystal structure determination. Crystals of [methyltris(1-pyrazolyl)gallato-N,N,N](triphenylstannyl)tricarbonylmolybdenum are monoclinic, a = 11.4439(8), b = 19.5116(8), c = 15.2686(12) Å β = 111.370(3)°, Z = 4, space group P2 1 /c. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.025 and R w  = 0.031 for 5259 reflections with I ≥ 3σ(I). Important bond lengths include: Mo—Sn = 2.8579(3), Mo—N = 2.239(2)–2.244(2), Mo—C = 1.967(3)–2.000(3), Sn—C = 2.151(3)–2.166(3), Ga—N = 1.920(3)–1.931(3), and Ga—C = 1.943(4) Å.