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First Examples of Metal Cyclohexylphosphonates: Influence of the Choice of Synthetic Route on the Product
Author(s) -
Murugavel Ramaswamy,
Davis Paul,
Walawalkar Mrinalini G.
Publication year - 2005
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200500156
Subject(s) - monoclinic crystal system , metal , hydrothermal synthesis , crystallography , derivative (finance) , crystal structure , single crystal , materials science , ligand (biochemistry) , chemistry , nuclear chemistry , hydrothermal circulation , organic chemistry , chemical engineering , biochemistry , receptor , financial economics , economics , engineering
The first divalent metal cyclohexylphosphonate derivative, [Co(O 3 PCy)·H 2 O] 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(H 2 O) 4 (DMP) 2 }{CyPO 3 H} 2 ] n ( 2 ) as single crystals. The X‐ray diffraction studies on 2 reveal a hydrogen‐bonded polymeric structure for this compound. Crystal data: C 22 H 48 CoN 4 O 10 P 2 , monoclinic, P2 1 /c, a = 12.147(2), b = 11.607(2), c = 11.872(2) Å, β = 104.00(3)°, V = 1624.2(5) Å 3 , Z = 2, R1(all data) = 0.050, wR2 (all data) = 0.145.