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The synthesis of the heterobimetallic hafnium(IV)-nickel(0) complexes {[Hf](μ-σ ,π- C≡CR) 2 }Ni(CO) ( 3a , [Hf] = (η 5 -C 5 H 5 ) 2 Hf, R = Ph;  3b , [Hf] = (η 5 -C 5 H 4 SiMe 3 ) 2 Hf, R =  t Bu) in which an early (Hf) and a late (Ni) transition metal atom are bridged by σ - and π-bound alkynyl groups succeeds by treatment of [Hf](C≡CR) 2  ( 1a , [Hf] = (η 5 -C 5 H 5 ) 2 Hf, R = Ph;  1b , [Hf] = (η 5 -C 5 H 4 SiMe 3 ) 2 Hf, R =  t Bu) with equimolar amounts of Ni(CO) 4  ( 2 ). The reaction chemistry of  1 and  3 towards different substrates is discussed. Treatment of  3b with P(OMe)3 ( 4a ) affords the mononuclear nickel monocarbonyl complex Ni(CO)[P(OMe) 3 ] 3  ( 5 ), while the reaction of  1a or  1b with MCl 2  ( 6a , M = Fe;  6b , M = Ni;  6c , M = Co) produces by an cyclopentadienyl transfer from hafnium to M the sandwich compounds (η 5 -C 5 H 4 R’) 2 M (M = Fe:  7a , R’ = H;  7b , R’ = SiMe 3 ; M = Ni:  7c , R’ = H;  7d , R’ = SiMe 3 ; M = Co:  7e , R’ = H). Addition of KOH to  1b  or  3b , respectively, affords the homobimetallic hafnium complex {[Hf](C≡CR)} 2 O ( 8 ) in which two [Hf](C≡CR) fragments are bridged by an oxygen atom. Possible reaction mechanisms for the formation of  5 ,  7 and  8 by starting from  1 or  3 will be given. The result of the X-ray structure analysis of  8 is reported. Complex  8 crystallises in the monoclinic space group C2/c with the cell parameters a = 24.437(8), b = 14.655(5), c = 14.123(4) Å, β = 101.67(2)◦, V = 4953(3) Å 3 , Z = 4 and D = 1.454 g cm−3. Complex  8 contains a linear Hf-O-Hf unit with pseudo-tetrahedral coordinated hafnium atoms.

zeitschrift für naturforschung b

Synthese und Reaktionsverhalten von {[Hf](μ-σ,π-C≡CR) 2  }Ni(CO); die Röntgenstrukturanalyse von [(η 5 -C 5 H 4 SiMe 3 ) 2 Hf(C≡C t Bu)] 2 O / Synthesis and Reaction Behaviour of {[Hf](μ −σ ,π -C≡CR) 2 }Ni(CO); the Solid-State Structure of [(η 5 –C 5 H 4 SiMe 3 )2Hf(C≡C t Bu)] 2 O