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Mild Hydrothermal Synthesis and Structural Determination of Two Layered, Structurally Related Inorganic–Organic Hybrid Vanadates with Nickel(II) and Tris(2‐aminoethyl)amine
Author(s) -
Larrea Edurne S.,
Mesa José L.,
Pizarro José L.,
RodríguezFernández Jesús,
Arriortua María I.,
Rojo Teófilo
Publication year - 2009
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.200900145
Subject(s) - chemistry , hydrothermal circulation , crystallite , crystallography , stacking , nickel , dehydration , crystal structure , octahedron , hydrothermal synthesis , infrared spectroscopy , single crystal , phase (matter) , chemical engineering , organic chemistry , biochemistry , engineering
2D Ni 2 (C 6 H 19 N 4 ) 2 (V 6 O 18 ) · 2H 2 O ( 1) and Ni 2 (C 6 H 19 N 4 ) 2 (V 6 O 18 ) · H 2 O ( 2 ) are inorganic–organic hybrid compounds that have been synthesised under hydrothermal conditions. Crystalline aggregates composed of both compounds were obtained and structural characterisation was subsequently carried out using single crystalline fragments of these aggregates. Optimisation of the synthetic conditions allowed us to obtain 1 as a polycrystalline powder. The crystal structures of 1 and 2 were solved using single‐crystal X‐ray diffraction data. Both compounds are structurally related, as the layers from which they are built have the same composition and connectivity in both structures. The main differences between them are the layer stacking and water contents. UV/Vis spectroscopy of 1 shows the characteristic features of the Ni II d 8 cation in slightly distorted octahedral symmetry. From the temperature‐dependent magnetic susceptibility measurements the parameter D / hc = –3.75 cm –1 was obtained. Phase 1 undergoes a reversible structural transformation at approximately 60 °C as a result of the dehydration process. This dehydration gives rise to a decrease in the unit cell volume.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)