Isolation and structural characterization of the first homoleptic lanthanide-zirconium oxoisopropoxide, La2Zr3O(OPri)16. Combination of an [M4O] tetrahedron with an [MO6] octahedron - A new structure type for pentanuclear alkoxide complexes

Inorganic Chemistry Communications

Volumn 10, Issue 3, 2007, Pages 352-354

  Turova, N Ya ^a   Kessler, V G ^b   Turevskaya, E P ^a   Yanovsky, A I ^c  

^a MOSCOW STATE UNIVERSITY   (Russian Federation)

^b SWEDISH UNIVERSITY OF AGRICULTURAL SCIENCES   (Sweden)

^c A N NESMEYANOV INSTITUTE OF ORGANOELEMENT COMPOUNDS   (Russian Federation)

Author keywords

Crystal and molecular structure; Lanthanum; Oxoalkoxides; Precursor; Sol gel; Zirconium

Indexed keywords

EID: 33846895031     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.inoche.2006.12.002     Document Type: Article

References (24)

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11. +.
12. 3, M = 1512.86, Monoclinic, Space Group C2/c, a = 21.976(8), b = 15.835(5), c = 20.722(6) Å, β = 113.805(12)°. 2964 independent reflections [R(int) = 0.0803] were collected to 2θ ≤ 40.00° using SMART CCD 1k diffractometer (Mo Kα radiation, λ = 0.71073 Å) at 25 °C. The structure was solved by direct methods. Metal atom coordinates were extracted from the initial solution and all other non-hydrogen atoms were located in subsequent difference Fourier syntheses. All non-hydrogen atoms were refined by full-matrix technique first in isotropic and then in anisotropic approximation. Geometrical restraints have been put on all carbon atoms to diminish the effects caused by disorder in the structure, three carbon atoms C(42), C(71) and C(92) were refined with the ISOR restraints to reduce the elongation of the thermal ellipsoids caused by disorder. The hydrogen atom coordinates were calculated geometrically using a riding model and included in the final refinement in isotropic approximation. All calculations were performed using SHELXTL program package on an IBM PC [13]. Final discrepancy factors were R1 = 0.0709, wR2 = 0.1462 [I > 2sigma(I)].
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