The crystal and molecular structures of ethoxido-oxo-bis(1,5,9,13-tetrathiacyclohexadecane)-μ-oxodimolybdenum-(IV)trifluoromethanesuIfonate hydrate are reported. The complex crystallizes in the orthohombic space group Pn21 a with four molecules per unit cell of dimensions a = 16.149(2)Å, b = 20.477(4)Å, c = 15.217(2)Å and V = 5381 (2)Å3. Full matrix least squares refinement gave final discrepancy factors of R1=. 076 and R2 =. 094 for 3147 data having F2 >2.5σ(F2), The molecular structure is highlighted by a linearO-Mo=O—Mo=O unit. The two macrocycles coordinate each Mo atom in a “planar” tetradentate mode, and are staggered ∼43° relative to one another. © 1979, Taylor & Francis Group, LLC. All rights reserved.