The diethyl ether adducts of molybdenum(IV) and tungsten(IV) chloride, MCl4(Et2O)2, are broadly useful precursors for synthetic inorganic and organometallic chemistry, and the lability of the coordinated ethers allows for facile ligand substitution. The adducts are fragile at room temperature and reduced pressure, and the ether ligands are readily displaced in other coordinating solvents. Our group has recently developed novel synthetic protocols for the preparation and crystallization of trans-MCl4(Et2O)2 (M = Mo, W). We report our experimental approach and provide a discussion of relevant crystallographic metrical parameters. Additionally, we report an alternative approach for the preparation of 1,2-dimethoxyethane adducts, cis-MCl4(dme) (M =Mo, W), and provide spectroscopic analysis of the cis and trans isomers of these d2 octahedral systems.

Synthesis and structural confirmation of elusive molybdenum(IV) and tungsten(IV) reagents

ACS Fall 2021

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