A new one-dimensional aluminum fluorophosphate, AlP2O5（OH）3F·0.5[H2dien] （dien=diethylenetriamine）, was solvothermally synthesized by using organic amine as the structure directing agent, and its structure was determined by single-crystal X-ray diffraction. The complex inorganic architecture consists of trans-corner-sharing AlO4F2 octahedra chain decorated by phosphate tetrahedra along both sides of the -F-Al-F-Al-F- backbone displaying a series of Al2P three-membered rings, which will represent a new fundamental structural type in metal phosphates. The results of CHN elemental analysis, EDS, and TGA are also presented. Crystal data： C4H18Al2F2N3O16P4, monoclinic, space group P21/c with a=6.9107（14）, b=15.749（3）, c=8.9741（18） , β=109.829（2）o, V=918.8（3） 3, Z=2, Mr=580.05, Dc=2.097 g/cm3, μ=0.618 mm-1, S=1.022, F（000）=590, the final R=0.0510 and wR=0.1284 for 1607 observed reflections （I 〉 2σ（I））.
Two novel compounds, {[Co2（epda）2（4,4＇-bpy）（H20）z]＇3H20}n 1 and {[Co2（epda）2（bpe）（HzO）z]＇3HzO}n 2 （H2epda = 5-ethyl-pyridine-2,3-dicarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine and bpe = 1,2-di（4-pyridyl）ethylene） were solvothermally synthesized and charac- terized by elemental analysis, IR spectroscopy, thermogravimetric analysis （TGA）, and single- crystal X-ray diffraction. Complex 1 is ofmonoclinic system, space group P21/c with a = 13.344（5）, b = 14.724（5）, c = 8.267（3） A, fl = 105.840（4）~, V= 1562.5（10） A3, Dc = 1.480 g/cm3, Mr = 375.19, Z = 4, F（000） = 712, gl = 1.121 mm-1, the final R = 0.0512 and wR = 0.1260 for 2890 observed reflections with I 〉 2σ（I）. 2 belongs to the monoclinic system, space group P21/c with a = 14.224（4）, b = 14.726（4）, c = 8.287（2） A,β = 99.696（4）°, V= 1711.1（9） A3, Dc = 1.402 g/cm3, Mr = 388.21, Z = 4, F（000） = 740, kt = 1.027 mm-1, the final R = 0.0354 and wR = 0.0862 for 12237 observed reflections with I 〉 2a（/）. Both complexes present intimately related structures featuring infinite Co-carboxylate layers of [Con（epda）（H20）]n pillared by 4,4＇-bpy （or bpe） molecule to produce the microporous frameworks, Unambiguously indicating that pore dimensions of the framework are regulated by the N,N＇-donor pillars.
A novel compound, {[Cu2（nbdc）2（4,4＇-bpy）2（H2O）2]·2H2O}n（H2nbdc = 4-nitrobenzene-1,2-dicarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine）, was hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis（TGA）, and single-crystal X-ray diffraction. The complex is of orthorhombic system, space group Pbcn with a = 32.222（7）, b = 7.8503（16）, c = 28.389（6）, V = 7181（3）3, Dc = 1.720 g/cm3, Mr = 929.74, Z = 8, F（000） = 3792, μ = 1.273 mm-1, the final R = 0.0591 and wR = 0.1378 for 4548 observed reflections with I 〉 2σ（I）. The compound exhibits a 3D self-penetrating framework with bcu net topology, in which the（46·48）-networks are joined by the H2nbdc and 4,4＇-bpy linkers.
