A new coordination polymer, {[Ni2(CH3O-ip)2(1,6-bih)2]}n(1), (CH3O-H2ip = 5-methoxyisophthalic acid, 1,6-bih = 1,6-bis(imidazol-1-yl)hexane), has been obtained under hydrothermal conditions. Complex 1 was determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectroscopy. Complex 1 shows a two-dimensional corrugated layer with (3,5)-connected (42.6)(42.67.8) topology. Furthermore, thermogravimetric property of 1 was also investigated. Supplemental materials are available for this article. Go to the publisher's online edition ofSynthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistryto view the supplemental file. [ABSTRACT FROM AUTHOR]