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|Title:||Convenient route to niobium in lower oxidation states: Synthesis and crystal structure of K4[Nb(C2O4)4]·4H 2O·1/2H2C2O4|
|Authors:||Ooi, B.-L. |
|Citation:||Ooi, B.-L.,Shihabara, T.,Sakane, G.,Mok, K.-F. (1997-12-01). Convenient route to niobium in lower oxidation states: Synthesis and crystal structure of K4[Nb(C2O4)4]·4H 2O·1/2H2C2O4. Inorganica Chimica Acta 266 (1) : 103-107. ScholarBank@NUS Repository.|
|Abstract:||A convenient preparative route to an Nb(IV) complex, K4[Nb(C2O4)4]·4H 2O·1/2H2C2O4, is obtained by zinc reduction of concentrated hydrochloric acid-ethanol solutions of niobium pentachloride followed by in situ complexation with oxalate. This direct method of synthesis of an Nb(IV) complex may serve to open up a new avenue to the aqueous solution chemistry of niobium in lower oxidation states. The structure of the complex, as determined by X-ray crystallography, is a square-antiprism tetrakis-chelate arrangement of the oxalate ligand coordinated to an Nb(IV) center. The brown complex crystallizes in the triclinic space groupP1̄, with Z=2, a= 11.219(4), b= 12.931 (5), c = 9.257(4) Å, α= 110.79(3), β= 114.15(2), γ= 88.56(3)°, V= 1134.4(9) Å3, Mr = 718.46, Dcalc = 2.10 g cm-3, R = 0.029 and Rw = 0.0049. © 1997 Elsevier Science S.A.|
|Source Title:||Inorganica Chimica Acta|
|Appears in Collections:||Staff Publications|
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