Journal
CRYSTAL GROWTH & DESIGN
Volume 5, Issue 2, Pages 623-629Publisher
AMER CHEMICAL SOC
DOI: 10.1021/cg049838e
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Pyridine-2,6-dicarboxylic acid (pdcH(2)) and 4,4'-bipyridyl (4,4'-bpy) reacts under hydrothermal condition with Co(II)- or Ni(II)-nitrate to form very similar 2-D metal-organic framework (MOF) structures with the empirical formula [M(pdc)(4,4'-bpy)] - 1/2MeOH (M = Co(II), 1 and Ni(II), 2). Compound 1 crystallizes in the monoclinic space group P2(1)/n with a = 11.419(3) angstrom, b = 10.290(2) angstrom, c = 15.695(5) angstrom, beta = 96.052(5)degrees, V = 1833.9(13) angstrom(3), Z = 4, R1 = 0.046, WR2 = 0.125, and S = 1.059. Compound 2 also crystallizes in the monoclinic space group P2(1)/n with a = 11.249(5) angstrom, b = 10.277(2) angstrom, c = 15.607(5) angstrom, beta = 97.916(5)degrees, V = 1787.1(13) angstrom(3), Z = 4, R1 = 0.058, WR2 = 0.155, and S = 0.99. Rectangular voids of approximate dimension 8.9 x 5.5 angstrom formed in these two structures remain empty. Each 2-D sheet thus formed is stacked on top of each other with an intricate array of hydrogen bonding, showing a perpendicular distance of similar to 8.1 and 7.8 angstrom in 1 and 2, respectively. When 1,2-di(4-pyridyl)ethylene is used in place of 4,4'-bipyridyl to construct the MOFs, only Ni(II)-nitrate affords crystals whose structure differs greatly from that of 1 or 2. Here, 1,2-di(4-pyridyl)ethylene is not bonded to the metal but exists in the lattice in diprotonated form, and a hydrogen-bonded 3-D structure of discrete (dpeH(2))[Ni(pdc)2]center dot 5H(2)O (3) units is formed. Compound 3 crystallizes in the monoclinic space group P2(1)/n with a = 8.915(2) angstrom, b = 19.844(6) angstrom, c = 15.799(5) angstrom, beta = 96.083(5)degrees, V = 2779.2(19) angstrom(3), Z = 4, R1 = 0.0391, WR2 = 0.0998, and S = 1.096. Interestingly, in 3, an acyclic trimeric water cluster is hydrogen bonded to the spacer and a free carboxylate O atom.
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