CRYSTAL-STRUCTURE AND SOLUTION-STATE NMR-SPECTRA OF 1,1'-(1,4,10-TRIOXA-7,13-DIAZACYCLOPENTADECANE-7,13-DIYLDICARBONYL)FERROCENE HYDRATE

The crystal structure of the ferrocene-containing cryptand l,1ʹ-(l,4,10-trioxa-7,13-diazacyclopentadecane-7,13-diyldicarbonyI)ferrocene hydrate has been determined by X-ray crystallography. Crystals are orthorhombic, with a = 8.575 (6) Å, b = 13.512 (9) Å, c = 17.734 (11) Å, space group P212121, and d(calcd, Z = 4) = 1.53 g cm-3. The structure was solved from the Patterson function and refined by least squares; RF = 0.056 (Rw = 0.058). The cyclopentadienyl rings are almost parallel, the dihedral angle between their least-squares planes being 3.2 (6)°, with an inter-ring separation of 3.28 (2) Å. The ferrocene rings are rotated from the eclipsed conformation by only ca. 0.3°. The orientation of the carbonyls is trans, with substitution at the cyclopentadienyl rings staggered by ca. 71.7°. The amide π-bonding systems exhibit only slight distortions from planarity. The proposed structure in solution as determined by 2-D homo-and heteronuclear NMR techniques is consistent with the X-ray structure. © 1990, American Chemical Society. All rights reserved.