A one-dimensional chain organic-inorganic heteropoly compounds As(phen)AsMoO7 has been synthesized by the hydrothermal reaction and structurally characterized by single crystal X-ray diffraction analysis.The crystal data are as follows:triclinic,space group P-1,a=8.5202(9)(A),b=8.6607(9)(A),c=11.1796(12)(A),a=111.7710(10)°,β3=90.1210(10)°,γ=110.5220(10)°,V=709.16(13)(A)3,Z=2,R1=0.0295,wR2=0.0864,S=1.067.The structrure of the title compound is composed of [As(phen)] 3+complex cation and [AsMoO7]3-anion.A [As2Mo2O14]6-cluster is polymerized by two [AsMoO7]3-anion.The structure consists of the [As2Mo2O14]6-cluster which is connected by [As(phen)] 3+ complex cation.forms one-dimensional chain.Meanwhile,the phen rings of [As(phen)]3+ are parallel to each other and cause significant π-π stacking.The interplanar distances between the phen planes are 3.389(A).The organic-inorganic heteropoly compound forms a two-dimensional supermolecule layer structure through the ineterchain π-π stacking.