METALLOCENE DERIVATIVES OF EARLY TRANSITION ELEMENTS. PART 4. SYNTHESIS AND CRYSTAL STRUCTURES OF A SERIES OF ZIRCONOCENE(IV) HALIDES (X = Cl OR Br) AND 2X2> ( X =F, Br, OR I)

DOI: 10.1039/DT9870001463

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1463 - 1472 (1987)

Update date:2022-08-16

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Authors:

Antinolo, Antonio

Lappert, Michael F.

Singh, Anirudh

Winterborn, Duncan J. W.

Engelhardt, Lutz M.

et al. et al.

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Article abstract of DOI:10.1039/DT9870001463

A series of zirconocene(IV) halides, and 2X2> , has been prepared, either by (i) substitutive procedures from ZrCl4 , or (ii), for complexes (3), (5), or (6), by oxidative addition to 2(CO)2>.The only v_asym(ZrX2) vibration to be assigned with confidence is for X = F at 563 cm^-1, (1)H and (13)C n.m.r.data are unexceptional.X-Ray structure determinations of complexes (1)-(5) have been carried out.Their molecular symmetry is close to 2, or crystallographically imposed 2 in (3), with the stereochemistry about the metal centre best described as distorted tetrahedral.The angle X-Zr-X is 93.70(7), 94.2(1), 100.5(3), 100.25(5), and 100.37(4)deg for the halides (1)-(5), respectively; and the corresponding centroid-Zr-centroid angles are 129.1, 128.2, 131.4, 131.4, and 131.8 deg.Metalhalogen distances in (1) <2.505(2) and 2.476(2) Angstroem> and (3) <2.212(6) Angstroem> are significantly longer than in the parent zirconocene(IV) halides (cf. 2.44 Angstroem for X = Cl and 1.98 Angstroem for X = F) as are the metal-centroid distances in (3)-(5).

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