Two new organo-inorganic hybrid compounds, aluminum nitrilotris(methylene)t
rismonohydrogenphosphonate hydrate, Al[(HO3PCH2)(3)N]H2O, and tricopper(II)
bis-nitrilobis(methylene)diphosphonate, Cu-3[(O3PCH2)(2)NH2](2), have been
synthesized. The crystal structures have been determined ab initio from po
wder diffraction data and refined by the Rietveld method. Al[(HO3PCH2)(3)N]
H2O is monoclinic, space group P2(1)/n, with a = 12.1945(3) Angstrom, b = 9
.1129(3) Angstrom, c = 8.5495(2) Angstrom, beta = 94.317(2)degrees, Z = 4,
and the X-ray powder diffraction pattern has been refined to R-wP = 8.7%. C
u-3[(O3PCH2)(2)NH2](2) is orthorhombic, space group Pbca, with a = 16.1209(
6) Angstrom, b = 9.4890(4) Angstrom, c = 9.4113(4) Angstrom, Z = 4 and its
pattern was refined to R-wP = 13.5%. The crystal structure of aluminum phos
phonate contains a close packing of inorganic chains, formed by alternating
AlO6 octahedra and O3PC tetrahedra. These chains are covalently interconne
cted by the organic groups to give the 3D framework. The structure of coppe
r phosphonate has two distinct copper environments, one a tetragonally elon
gated tetrahedron and the other a distorted square plane. These structural
units are linked by the organic phosphonate. Thermal and infrared data are
discussed. (C) 2001 Academic Press.