Articles

Journal of Cluster Science

, Volume 6, Issue 1, pp 93-106

First online:

Synthesis and structural characterization of [SiMe2(C5H4)2][(C5Me5) Zr(μ-S)]2. a dinuclear zirconocenophane complex with a skewed dimethylsilyl-bridged bis(cyclopentadienyl) ligand

  • Linda M. BurstynowiczAffiliated withDepartment of Chemistry, West Virginia University
  • , Jeffrey L. PetersenAffiliated withDepartment of Chemistry, West Virginia University

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Abstract

The reaction of [SiMe2(C5H4)2][(C5Me5)ZrMe2]2 with H2S at 110°C proceeds with the formation of [SiMe2(C5H4)2][(C5Me5)Zr(μ-S)]2]2. The molecular structure of this dinuclear zirconocenophane compound features a non-planar four-membered Zr2(μ-S)2 2 ring with two symmetrically-bridging sulfido groups. The bridging dimethylsilyl-bridged bis(cyclopentadienyl) ligand adopts a skewed orientation to accommodate the long Zr ... Zr separation of 3.611(1) Å. This compound crystallizes in the centrosymmetric space group P1 with refined lattice parameters ofa = 10.905(1) Å,b = 10.939(2) Å,c = 14.621(2) Å,α = 106.32(1)°,β = 91.25(1)°,γ = 111.25(1)°,V = 1545.1(8) Å3, ρcalc. = 1.512g/cm3,Z=2. Full-matrix refinement converged with final discrepancy indices of R(F o = 0.045 andR(F o) = 0.079 with GOF= 1.60 for 4403 data withF o > 3σ(F o).

Key Words

Zirconium sulfide