Hydrocarbon-soluble molecular silicophosphonate [RSi(OH){OP(O)(H)(OH)}]2O (R = (2,6-i-Pr2C6H3)NSiMe3) (1) which contains two Si-O-H, two P-O-H, one Si-O-Si, and two Si- O-P linkages is obtained in 35% yield from a direct reaction between RSi(OH)3 and the λ3-cyclotriphosphazane [EtNPCl]3 in the presence of Et3N. The silicophosphonate 1 has been characterized with the aid of IR and NMR (1H, 31P, and 29Si) spectroscopy. A single-crystal X-ray diffraction study reveals that the molecule is built around a HO-P-O-Si(OH)-O-Si(OH)-O-P-OH inorganic backbone. The preliminary investigations indicate that 1 could serve as a useful precursor for the preparation molecular metallosilicophosphonates.