Inorganic-organic hybrid compounds:: hydrothermal synthesis and characterization of a new three-dimensional metal tetraphosphonate Mn[(HO3PCH2)N(H)(CH2)4(H)N(CH2PO3H)2]

The new manganese tetraphosphonate. Mn[(HO3PCH2)(2)N(H)(CH2)(4)(H)N(CH2PO3)(2)] (1) was hydrothermally synthesized from MnCl2 and N,N,N',N'-tetrametylphospliono-1,4-diaminobutane, (H2O3PCH2)(2)N-(CH2)(4)-N(CH2PO3H2)(2). The structure was determined from single-crystal X-ray diffraction data (Mn[(HO3PCH2)(2)N(H)(CH2)(4)(H)N(CH2PO3)(2)], monoclinic, P2(1)/a, with a = 9.6663(1), b = 9.2249(2), c = 10.5452(1) pin, beta = 105.676(1)degrees, V = 905.35(3) x 10(6) pm, Z = 2, R-1 = 0.051, wR(2) = 0.109 (all data). The structure contains the zwitter ions [(HO3PCH2)(2)N(H)-(CH2)(4)-(H)N(CH2PO3)(2)](2-) and is built from alternating corner-linked [MnO6] and [PO3C] polyhedra forming a two-dimensional net of eight-rings. These layers are connected to a pillared structure by the diaminobutane groups. Magnetic susceptibility data confirms the presence of Mn2+ ions. Thermogravimetric measurements show a stability of 1 up to similar to 290degreesC. Between 290degreesC and 345degreesC a one-step loss of similar to 7.0% is observed, and above 345degreesC the continuous decomposition of the organic part of the structures takes place. (C) 2003 Elsevier Inc. All rights reserved.