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Control of donor-acceptor interactions in organoalkaline-earth-transition-metal complexes. Crystallographic characterization of (Me{sub 5}C{sub 5}){sub 2}HfCl({mu}-Cl)Ca(Me{sub 5}C{sub 5}){sub 2}

Journal Article · · Organometallics
; ;  [1]
  1. Vanderbilt Univ., Nashville, TN (United States)

The problem of ligand exchange or loss in the formation of organometallic alkaline-earth-transition-metal complexes can be minimized by ensuring that any exchange would be degenerate or would require an unfavorable transfer of ligands. This approach is illustrated in the formation of chloride-bridged calcium-group 4 dimers and in an isocarbonyl-linked calcium-chromium dimer. Bis(pentamethylcyclopentadienyl)calcium Cp*{sub 2}Ca, reacts with Cp*{sub 2}ZrCl{sub 2}, Cp*{sub 2}HfCl{sub 2}, and Cp*{sub 2}ThCl{sub 2} in toluene to yield 1:1 adducts. Orange-yellow crystals of Cp*{sub 2}HfCl({mu}-Cl)CaCp* grown from toluene are triclinic, space group P{bar 1}, with a = 11.146 (4) {angstrom}, b = 16.942 (6) {angstrom}, c = 11.109 (3) {angstrom}, {alpha} = 103.34 (3){degrees}, {beta} = 94.89 (3){degrees}, {gamma} = 102.50 (3){degrees}, and D(calcd) = 1.398 g cm{sup -3} for Z = 2. The structure consists of two bent metallocene units with a single {mu}-Cl and a terminal Cl on hafnium: Ca-{mu}-Cl = 2.864 (3) {angstrom}, Hf-{mu}-Cl = 2.463 (3) {angstrom}, Hf-Cl(t) = 2.383 (3) {angstrom}, and Ca-Cl-Hf = 161.3 (1){degrees}. Cp*{sub 2}Ca reacts with Cp*{sub 2}Zr(CO){sub 2} and mesitylene chromium tricarbonyl in toluene in yield 1:1 adducts. In the solid state, the calcium-chromium adduct exists as a tetranuclear species, constructed around a 12-membered ring consisting of two Ca and Cr atoms and four carbonyl groups. 39 refs., 2 figs., 4 figs.

Sponsoring Organization:
USDOE
OSTI ID:
567348
Journal Information:
Organometallics, Journal Name: Organometallics Journal Issue: 7 Vol. 11; ISSN 0276-7333; ISSN ORGND7
Country of Publication:
United States
Language:
English