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Synthesis and molecular structures of niobocene derivatives containing an Nb-Sn-Nb metallic chain

Journal Article · · Sov. J. Coordinat. Chem.; (United States)
OSTI ID:6509443
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The complex (Cp/sub 2/Nb(CO))/sub 2/SnCl/sub 2/ (I) has been synthesized in the form of golden brown crystals by reacting Cp/sub 2/Nb(CO)H with SnCl/sub 4/ in THF (it has also been obtained by a back synthesis from Cp/sub 2/Nb(CO)H and Cp/sub 2/Nb(COSnCl/sub 3/). The more soluble methylcyclopentadienyl analog ((CH/sub 3/C/sub 5/H/sub 4/)/sub 2/Nb(CO))/sub 2/SnCl/sub 2/ (II) has been isolated in the form of reddish orange crystals following the reaction of (CH/sub 3/C/sub 5/H/sub 4/)/sub 2/Nb(CO)H with SnCl/sub 2/ in THF in the presence of Et/sub 3/N. According to the data from x-ray diffraction analysis, complex II contains an Nb-Sn-Nb metallic chain with short, probably partially multiple Nb-Sn bonds (2.840(2) A) and a 140.69(5)/sup 0/ angle between them. The tin atom has a very distorted tetrahedral environment (the NbSnCl angles are equal to 107.6(1), and the ClSnCl angle equals 92.0(6)/sup 0/), the Sn-Cl bonds being strongly elongated (2.518(6) A) due to the partial double character of the Nb-Sn bonds. A structure of a similar type is observed for the complex (Cp/sub 2/NbH)/sub 2/Sn(Cl)Et (III), which is unexpectedly formed as a result of the successive addition of triethylamine, butyllithium, and Et/sub 2/SnCl/sub 2/ to a solution of Cp/sub 2/NbBH/sub 4/ in THF. In complex III each Cp/sub 2/Nb fragment is joined to a terminal hydride atom (Nb-H = 1.66(1) and 1.69(1) A) and forms a shortened bond with the tin atom (Nb-Sn = 2.868(1) and 2.856(1) A, and the NbSnNb angle equals 129.44(5)/sup 0/), which has a pseudotetrahedral environment (NbSnCl = 101.01(9), NbSnC(Et) = 113.25(5), and ClSnC(Et) 89.84(5)/sup 0/) with strongly elongated Sn-Cl (2.600(4) A) and Sn-C(Et) (2.25(2) A) bonds.
OSTI ID:
6509443
Journal Information:
Sov. J. Coordinat. Chem.; (United States), Journal Name: Sov. J. Coordinat. Chem.; (United States) Vol. 11:8; ISSN SJCCD
Country of Publication:
United States
Language:
English

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Related Subjects

36 MATERIALS SCIENCE
360602 -- Other Materials-- Structure & Phase Studies
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
BOND ANGLE
BOND LENGTHS
CARBONYLS
CHEMICAL BONDS
CHLORIDES
CHLORINE COMPOUNDS
COHERENT SCATTERING
COMPLEXES
COORDINATION VALENCES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
CRYSTALLIZATION
DIAMAGNETISM
DIFFRACTION
DIMENSIONS
DISTANCE
FURANS
HALIDES
HALOGEN COMPOUNDS
HETEROCYCLIC COMPOUNDS
INTERATOMIC DISTANCES
LATTICE PARAMETERS
LENGTH
MAGNETISM
MOLECULAR STRUCTURE
MONOCLINIC LATTICES
NIOBIUM COMPLEXES
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORTHORHOMBIC LATTICES
PHASE TRANSFORMATIONS
SCATTERING
SPACE GROUPS
SUPERCONDUCTORS
SYNTHESIS
TETRAHYDROFURAN
TIN CHLORIDES
TIN COMPOUNDS
TIN HALIDES
TRANSITION ELEMENT COMPLEXES
VALENCE
X-RAY DIFFRACTION