Tubular metal-organic complex (C2H9N2)2(C2H10N2)0.5[MoO2(OC6H4O)2] has been synthesized. The title complex crystallizes in the tetragonal system, space group P4(2)/n with a = 25.214(8), c = 7.484(4) ?, and Z = 8. The X-ray structural analysis of the complex reveals tube-like framework which is stabilized by hydrogen bond. Chiral anions [Mo(V)O2(OC6H4O)2]3? of the complex have two types of isomers(λ /δ configuration). Helical nanostructure of this metal-organic complex was formed using a sonochemical method. Sonocation may lead to the transformation from the bulk tubular complex to the helical nanostructure. The as-synthesized nanohelices were all double-stranded and left- and right-handed nanohelices were both formed. The helical nanostructure is a new morphology of inorganic-organic hybrid materials on the nanoscale level and the exact formation mechanism of these helices still needs further investigation. The title complex crystallizes in the tetragonal system, space group P4 (2) / n with a = 25.214 (8), c (c) = 7.484 (4) ?, and Z = 8. The X-ray structural analysis of the complex reveals tube-like framework which is stabilized by hydrogen bond. Chiral anions [Mo (V) O2 (OC6H4O) 2] 3? Of the Complex have two types of isomers (λ / δ configuration). Helical nanostructure of this metal-organic complex was formed using a sonochemical method. Sonocation may lead to the transformation from the bulk tubular complex to the helical nanostructure. The as-synthesized nanohelices were all double-stranded and left- and right-handed nanohelices were both formed. The helical nanostructure is a new morphology of inorganic-organic hybrid materials on the nanoscale level and the exact formation mechanism of these helices still needs further investigation.