Skip to main content
OSTI.GOVU.S. Department of Energy Office of Scientific and Technical Information
U.S. Department of Energy
Office of Scientific and Technical Information
 

Structural characterization of paramagnetic, triangulo niobium clusters, Cp'/sub 3/Nb/sub 3/Cl/sub 3/(/mu//sub 2/-Cl)/sub 3/(/mu//sub 3/-O)(/mu//sub 3/-X) (X = OH, Cl)

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00291a026· OSTI ID:5762095
;

The Nb(III) complex (Cp'Nb(CO)/sub 2/Cl/sub 2/)/sub 2/ (1, Cp' = C/sub 5/H/sub 4/Me) undergoes decarbonylation in refluxing THF to give a dark brown paramagnetic compound believed to be Cp'/sub 3/Nb/sub 3/Cl/sub 6/(/mu//sub 3/-O) (2). Compound 2 reacts with atmospheric oxygen to produce Cp'/sub 3/Nb/sub 3/Cl/sub 3/(/mu//sub 2/-Cl)/sub 3/(/mu//sub 3/-O)(/mu//sub 3/-OH) (3) and with chlorinated hydrocarbons to form Cp'/sub 3/Nb/sub 3/Cl/sub 3/(/mu//sub 2/-Cl)/sub 3/(/mu//sub 3/-O)(/mu//sub 3/-Cl) (4). Compounds 3 and 4 are paramagnetic. X-ray structure determinations show that each of these clusters has one short Nb-Nb distance of ca. 2.92 /angstrom/ corresponding to a Nb-Nb bond and two long Nb/center dot//center dot//center dot/Nb distances near 3.28 (3) or 3.39 /angstrom/ (4). The Nb/sub 3/ triangle is bridged by Cl atoms along each edge and is capped by a /mu//sub 3/-oxo ligand and a /mu//sub 3/-hydroxo (3) or /mu//sub 3/-chloro ligand (4) on opposite sides of the Nb/sub 3/ plane. Terminal Cp and Cl ligands complete the coordination sphere about each Nb atom. Crystal data: for 3, a = 7.210 (2) /angstrom/, b = 26.097 (7) /angstrom/, c = 12.518 (3) /angstrom/, /beta/ = 94.18 (2)/degree/, space group P2/sub 1//n, Z = 4, V = 2349 /angstrom//sup 3/, /rho//sub calcd/ = 2.06 g/mL, R = 0.039 and R/sub w/ = 0.054 on 2551 reflections with I > 3/sigma/(I); for 4, a = 7.620 (1) /angstrom/, b = 15.108 (4) /angstrom/, c = 21.670 (6) /angstrom/, /alpha/ = 87.45 (2)/degree/, /beta/ = 93.68 (2)/degree/, /gamma/ = 104.01 (2)/degree/, space group P1, Z = 4, V = 2414 (1) /angstrom//sup 3/, /rho//sub calcd/ = 2.01 g/mL, R = 0.065 and R/sub w/ = 0.055 on 2424 reflections with I > 3/sigma/(I). 6 references, 3 figures, 4 tables.

Research Organization:
Univ. of Michigan, Ann Arbor (USA)
OSTI ID:
5762095
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 27:18; ISSN INOCA
Country of Publication:
United States
Language:
English

Similar Records

Diphosphine- and CO-Induced Fragmentation of Chloride-bridged Dinuclear Complex and Cp*Ir(mu-Cl)(3)Re(CO)(3) and Attempted Synthesis of Cp*Ir(mu-Cl)(3)Mn(CO)(3): Spectroscopic Data and X-ray Diffraction Structures of the Pentamethylcyclopentadienyl Compounds [Cp*IrCl{(Z)-Ph2PCH = CHPPh2}][Cl]center dot 2CHCl(3) and Cp*Ir(CO)Cl-2
Journal Article · Thu Dec 31 23:00:00 EST 2009 · Journal of Chemical Crystallography · OSTI ID:986820
Metal-metal-bonded compounds of lower-valent niobium and tantalum. Compounds containing the [Nb[sub 2]Cl[sub 7](PR[sub 3])[sub 2]][sup [minus]] and [Nb[sub 3]Cl[sub 10](PR[sub 3])[sub 3]][sup [minus]] ions and some clues as to how higher-nuclearity clusters are formed
Journal Article · Tue Mar 16 23:00:00 EST 1993 · Inorganic Chemistry; (United States) · OSTI ID:6623931
Synthesis and structure of the cationic tert-butoxide complexes Y sub 3 (OR) sub 7 Cl(THF) sub 3 sup + , Y sub 2 (OR) sub 4 Cl(THF) sub 4 sup + , and Y(OR)Cl(THF) sub 5 sup + : Representatives of a new class of yttrium alkoxides
Journal Article · Tue Mar 13 23:00:00 EST 1990 · Journal of the American Chemical Society; (USA) · OSTI ID:6428846

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
400202 -- Isotope Effects
Isotope Exchange
& Isotope Separation
ALKANES
CARBONYLS
CHLORIDES
CHLORINE COMPOUNDS
CRYSTAL STRUCTURE
CYCLOALKANES
DATA
EXPERIMENTAL DATA
HALIDES
HALOGEN COMPOUNDS
HYDROCARBONS
HYDROGEN COMPOUNDS
HYDROXIDES
INFORMATION
MAGNETISM
MOLECULAR STRUCTURE
NIOBIUM CHLORIDES
NIOBIUM COMPOUNDS
NUMERICAL DATA
ORGANIC COMPOUNDS
OXYGEN COMPOUNDS
PARAMAGNETISM
REFRACTORY METAL COMPOUNDS
TRANSITION ELEMENT COMPOUNDS