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Journal of Structural Chemistry

2011 year, number 2


D. P. Domonov, N. V. Kuratieva, S. I. Pechenyuk
Keywords: double complex salts, cobalt, iron, cuprum, single crystal X-ray diffraction, intermetallic compounds, thermal decomposition, ligands, ammonia, methane
Pages: 365-371


Double complex salts (DCSs) [Co(NH3)6][Fe(CN)6] (I) and [Co(NH3)6]2[Cu(C2O4)2]3 (II) and complex [Co(NH3)6]2(C2O4)3·4H2O (III) are synthesized and investigated by single crystal XRD, crystal optics, and elemental analysis. The crystalline phases of I, II, and III (R-3, P21/c, and Pnnm space groups respectively) have the following crystallographic characteristics: a = 10.9804(2) Å, b = 10.9804(2) Å, c = 10.8224(3) Å, V = 1130.03(4) Å3, Z = 3, dx = 1.65 g/cm3 (I); a = 9.6370(2) Å, b = 10.2452(2) Å, c = 13.2108(3) Å, V = 1932.90(9) Å3, Z = 2, dx= 1.97 g/cm3 (II), and a = 11.7658(3) Å, b = 11.7254(3) Å, c = 14.1913(4) Å, V = 1304.34(5) Å3, Z = 2, dx = 1.68 g/cm3 (III). This paper investigates the products of DCS thermolysis in a hydrogen atmosphere: the intermetallic compound CoFe with the bcc parameter а = 2.852 Å for I and a heterogeneous mixture of Co and Cu in the decomposition of II. The coordinated CN- and groups then turn into NH3, hydrocarbons, and CO2. The dominant hydrocarbon is methane.