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First examples of metal cyclohexylphosphonates: Influence of the choice of synthetic route on the product

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Title First examples of metal cyclohexylphosphonates: Influence of the choice of synthetic route on the product
 
Creator MURUGAVEL, R
DAVIS, P
WALAWALKAR, MG
 
Subject structural-characterization
zirconium-phosphate
pyrazole ligands
phosphonates
cage
intercalation
cobalt
model
ions
aluminophosphonate
cobalt
phosphorus
phosphonate complexes
inclusion compounds
 
Description The first divalent metal cyclohexylphosphonate derivative, [CO(O3PCy)-H2O](n) (1) has been synthesized using four different synthetic methodologies in the presence of added amines. The new phosphonates have been characterized with the aid of analytical, thermoanalytical, spectroscopic, and powder XRD studies. The nature and particle size of the product formed is highly dependent on the method employed (viz. (a) room temperature synthesis, (b) hydrothermal synthesis, (c) microwave assisted synthesis, and (d) a biphasic reaction) as revealed by SEM and TEM studies. While in most cases the metal phosphonates were isolated as insoluble crystalline powders directly from the reaction mixture, the use of 3,5-dimethylpyrazole (DMP) as co-ligand leads to the isolation of soluble compound [{Co(H2O)(4)(DMP)(2)} {CYPO3H}(2)](n) (2) as single crystals. The X-ray diffraction studies on 2 reveal a hydrogenbonded polymeric structure for this compound. Crystal data: C22H48CoN4O10P2, monoclinic, P2(1)/c, a = 12.147(2), b = 11.607(2), c = 11.872(2) angstrom, beta = 104.00(3)degrees, V = 1624.2(5) angstrom(3), Z = 2, R1 (all data) = 0.050, wR2 (all data) = 0.145.
 
Publisher WILEY-V C H VERLAG GMBH
 
Date 2011-09-01T16:49:04Z
2011-12-26T12:59:43Z
2011-12-27T05:52:27Z
2011-09-01T16:49:04Z
2011-12-26T12:59:43Z
2011-12-27T05:52:27Z
2005
 
Type Article
 
Identifier ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 631(13-14), 2806-2811
0044-2313
http://dx.doi.org/10.1002/zaac.200500156
http://dspace.library.iitb.ac.in/xmlui/handle/10054/12824
http://hdl.handle.net/10054/12824
 
Language en