Hydrothermal synthesis and crystal structure of the Ni{sub 2}(C{sub 4}H{sub 4}N{sub 2})(V{sub 4}O{sub 12})(H{sub 2}O){sub 2} and Ni{sub 3}(C{sub 4}H{sub 4}N{sub 2}){sub 3}(V{sub 8}O{sub 23}) inorganic-organic hybrid compounds. Thermal, spectroscopic and magnetic studies of the hydrated phase
- Dpto. de Quimica Inorganica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao (Spain)
- Dpto. de Mineralogia y Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco, Apdo. 644, E-48080 Bilbao (Spain)
Ni{sub 2}(C{sub 4}H{sub 4}N{sub 2})(V{sub 4}O{sub 12})(H{sub 2}O){sub 2}, 1, and Ni{sub 3}(C{sub 4}H{sub 4}N{sub 2}){sub 3}(V{sub 8}O{sub 23}), 2, have been synthesized using mild hydrothermal conditions at 170 deg. C under autogenous pressure. Both phases crystallize in the P-1 triclinic space group, with the unit-cell parameters, a=7.437(7), b=7.571(3), c=7.564(4) A, {alpha}=65.64(4), {beta}=76.09(4), {gamma}=86.25(3){sup o} for 1 and a=8.566(2), b=9.117(2), c=12.619(3) A, {alpha}=71.05(2), {beta}=83.48(4), {gamma}=61.32(3){sup o} for 2, being Z=2 for both compounds. The crystal structure of the three-dimensional 1 is constructed from layers linked between them through the pyrazine molecules. The sheets are formed by edge-shared [Ni{sub 2}O{sub 6}(H{sub 2}O){sub 2}N{sub 2}] nickel(II) dimers octahedra and rings composed by four [V{sub 4}O{sub 12}] vanadium(V) tetrahedra linked through vertices. The crystal structure of 2 is formed from vertex shared [VO{sub 4}] tetrahedra that give rise to twelve member rings. [NiO{sub 4}(C{sub 4}H{sub 4}N{sub 2}){sub 2}]{sub {infinity}} chains, resulting from [NiO{sub 4}N{sub 2}] octahedra and pyrazine molecules, give rise to a 3D skeleton when connecting to [VO{sub 4}] tetrahedra. Diffuse reflectance measurements of 1 indicate a slightly distorted octahedral geometry with values of Dq=880, B=980 and C=2700 cm{sup -1}. Magnetic measurements of 1, carried out in the 5.0-300 K range, indicate the existence of antiferromagnetic couplings with a Neel temperature near to 38 K. - Graphical abstract: Crystal structure of a sheet of Ni{sub 2}(C{sub 4}H{sub 4}N{sub 2})(V{sub 4}O{sub 12})(H{sub 2}O){sub 2}.
- OSTI ID:
- 21015758
- Journal Information:
- Journal of Solid State Chemistry, Vol. 180, Issue 3; Other Information: DOI: 10.1016/j.jssc.2006.12.037; PII: S0022-4596(07)00018-7; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
- Country of Publication:
- United States
- Language:
- English
Similar Records
Metal phosphonates based on aminomethylenediphosphonate: Syntheses and characterization of Na{sub 4}Zn{l_brace}NH{sub 3}CH(PO{sub 3}){sub 2}{r_brace}{sub 2}.4H{sub 2}O, Ni{l_brace}NH{sub 3}CH(PO{sub 3}H){sub 2}{r_brace}{sub 2}.xH{sub 2}O and NaNi{sub 2}{l_brace}NH{sub 3}CH(PO{sub 3})(PO{sub 3}H{sub 0.5}){r_brace}{sub 2}(H{sub 2}O){sub 2}.2H{sub 2}O
Hydrothermal synthesis and crystal structure of [Ni(H[sub 2]O)[sub 4]][VO(PO[sub 4])][sub 2], a nickel(II) vanadyl(IV) phosphate