Two　copper　helical　coordination　polymers,　[Cu(2-pc)(3-pc)](n)　1　and　[Cu(2-pc)(4-pc)](n)　2　(2-pc　=　2-pyridine　carboxylate,　3-pc　=　3-pyridine　carboxylate,　4-pc　=　4-pyridine　carboxylate)　have　been　hydrothermally　synthesized　directly　from　pyridine　carboxylic　acids　and　copper　nitrate.　The　crystal　structure　were　determined　by　single-crystal　X-ray　diffraction　with　the　following　data:　compound　1,　orthorhombic,　P2(1)2(1)2(1),　a　=　6.591(3)angstrom,　b　=　8.692(5)angstrom,　c　=　20.548(9)angstrom,　V　=　1177.2(9)angstrom(3),　Z　=　4;　compound　2,　orthorhombic,　Pna2(1),　a　=　21.160(10)angstrom,　b　=　9.095(5)angstrom,　c　=　6.401(3)angstrom,　V　=　1231.9(11)angstrom(3),　Z　=　4.　The　acentric　three-dimensional　(3D)　framework　of　I　is　constructed　from　right-handed　helical　Cu(2-pc)　chains　and　left-handed　Cu(3-pe)　helices.　As　for　2,　Cu(2-pc)　helical　chains,　in　which　left-　and　right-handed　helices　are　coexisting,　and　Cu(4-pc)　zigzag　chains　combined　together　to　form　acentric　3D　architecture　of　2　as　well.　Additionally,　besides　general　spectral　characterization,　we　first　introduce　generalized　2D　correlation　spectroscopy　to　explore　the　coordination　polymers　and　ascertain　the　stretching　vibration　location　of　carboxylate　groups　of　compounds　1　and　2.　(C)　2007　Elsevier　Inc.　All　rights　reserved.