Five new metal complexes, [Zn3(L1)2(BTC)2]·6H2O (1), [Zn3(L1)(BTC)2] (2), [Cd3(L1)(BTC)2] (3), [Cd3(L2)(BTC)2]·4H2O (4), and [Cd3(L2)(BTC)2(H2O)2] (5), have been successfully synthesized by solvothermal reactions of corresponding metal salts with 1,3,5-benzenetricarboxylic acid (H3BTC) and imidazole-containing ligands 1,3,5-tris(imidazol-1-ylmethyl)benzene (L1) and 3,3′,5,5′-tetra(imidazol-1-yl)-1,1′-biphenyl (L2). The structures of the complexes were determined by single crystal X-ray diffraction analysis. Complexes 1 and 2 obtained at different reaction temperatures show different structures: 1 is a three-dimensional (3D) net with Zn-BTC3– layers pillared by L1 ligands, while 2 has a 3D structure with a Zn-BTC3– framework and Zn-L1 chain. Complexes 2 and 3, which contain different metal centers, have similar framework structures but different coordination modes of carboxylate groups. 4 and 5 that were prepared from different solvents show different 3D structures. The thermal stability, photoluminescence...

Zinc(II) and Cadmium(II) Complexes with 1,3,5-Benzenetricarboxylate and Imidazole-Containing Ligands: Structural Variation via Reaction Temperature and Solvent

Solvothermal reactions of LnCl3·6H2O (Ln = Nd, Eu, Yb) with equimolar amounts of 5,11,17,23-tetrakis[(m-carboxyphenyl)azo]-25,26,27,28-tetrahydroxycalix[4]arene (H4L) at 90 or 140 °C gave rise to a set of six lanthanide(III) coordination polymers {[Nd2ClL(HCOO)(DMF)3(H2O)]·0.5DMF·MeCN·1.5H2O}n (1), {[Ln2ClL(HCOO)(DMF)]·sol}n (2: Ln = Eu, sol =0.5MeCN·1.5H2O; 3: Ln = Yb, sol = 1.5H2O), and {[H3O][LnL(H2O)]·DMF·MeCN·H2O}n (4: Ln = Nd; 5: Ln = Eu; 6: Ln = Yb). Complexes 1–6 were characterized by elemental analysis, IR, powder X-ray diffraction, and single-crystal X-ray diffraction. Compounds 1–3 have two-dimensional (2D) networks in which [Nd6Cl4L2(DMF)12(H2O)2] units (1) or [Ln6Cl4L2(DMF)2] (Ln = Eu (2), Yb (3)) are interlinked by the carboxyl groups of formates. Compounds 4–6 exhibit 2-fold interpenetrating 2D networks in which each [Ln4L(H2O)4] “four-flier pinwheel” unit works as a planar eight-connecting node to connect its eight equivalents via four L ligands. The formation of 1–6 provided an interestin...

Temperature-Driven Assembly of Ln(III) (Ln = Nd, Eu, Yb) Coordination Polymers of a Flexible Azo Calix[4]arene Polycarboxylate Ligand

Solvothermal reactions of 2,2′-biphenyldicarboxylate (H2dpa) and 4,4′-azobispyridine (azpy) in the presence of transition metal ions produce six new complexes, namely, [Co(dpa)(bphy)]n (1), [Co(dpa)(azpy)(H2O)]n·0.5nH2O (2), [Zn(dpa)(bphy)]n (3), [Zn(dpa)(azpy)(H2O)]n (4), [Mn(dpa)(azpy)(H2O)]n·0.5nH2O (5), and [Mn(dpa)(azpy)]n·nH2O·nMeOH (6) (bphy = 1,2-bis(4-pyridyl)hydrazine). The crystal structure analyses reveal that complexes 1 and 3 are isostructural which features a plywood-like structure, while complex 4 exhibits a parallel chains array. Complexes 2 and 5 afford a two-dimensional chiral (4,4) network, and complex 6 shows a (4,4) network. It was noteworthy that the in situ reduction of azpy to bphy was found in complexes 1 and 3, which were confirmed by single-crystal structures and LC-MS analyses. However, this in situ reduction was not found at a low reaction temperature in the syntheses of complexes 2, 4, and 5. The second-harmonic-generation (SHG) properties of 1 and 3 and the solid circular d...

Temperature-Dependent in Situ Reduction of 4,4′-Azobispyridine via Solvothermal Reaction

A series of nine coordination polymers {[Cd(L)(2)(solvent)(x)](solvent)(y)}(n) have been prepared from Cd(NO(3))(2) and 5-bromonicotinic acid (HL) in different solvents through a layered diffusion method. By using CH(3)OH/H(2)O at different volume ratios of 1:1 and 1:3, a one-dimensional (1D) coordination species (1a) and a three-dimensional (3D) (3,6)-connected framework (2a·g(1)) can be obtained. A similar self-assembly process in C(2)H(5)OH/H(2)O or H(2)O/1,4-dioxane gives 2a·g(2) or 2a·g(3), which are isomorphic to 2a·g(1) but with different lattice solvents. Replacement of the mixed solvents with DMF/H(2)O (v/v 1:1 or 1:3) also gives a 1D chain complex (1b) or a 3D microporous framework (2b·g(1)). Similarly, MOF 2b·g(2) can be assembled from CH(3)CN/H(2)O as an isomorphic solvate of 2b·g(1). Significantly, the 3D MOF families of 2a·g(n) and 2b·g(n) are supramolecular isomers even though they are topologically equivalent. Also, if a mixture of CH(3)OH/CH(2)Cl(2) (v/v 1:1 or 3:1) is used, a pair of distinct MOFs (3a·g) and (3b) are generated as pseudo-polymorphs that show a two-dimensional (2D) sheet and a 3D coordination framework, respectively. Furthermore, mutual solvent-induced conversions were realized between 1a and 1b and between 2a·g(1), 2a·g(2), and 2a·g(3) following the size-dependent rule of the solvent. These results are of great significance in recognizing the solvent effect upon coordination assemblies and their crystal transformations.

Exceptional crystallization diversity and solid-state conversions of Cd(II) coordination frameworks with 5-bromonicotinate directed by solvent media.

Four similar Mn(II) metal–organic frameworks (MOFs), {[Mn2(nbtc)(H2O)2(S)]·S·0.5H2O}n [S = DMF (1), DMA (2), NMP (3), DEF (4)] (DMF = N,N′-dimethylformamide, DMA = N,N′-dimethylacetamide, NMP = N-methyl-2-pyrrolidinone, DEF = N,N′-diethylformamide), have been assembled solvothermally from the nitro and carboxyl doubly functionalized ligand 6,6′-dinitro-2,2′,4,4′-biphenyl tetracarboxylic acid (H4nbtc) and characterized by single-crystal X-ray diffraction, elemental analyses, infrared spectroscopy, thermogravimetric analyses, and powder X-ray diffraction. All MOFs exhibit unique three-dimensional double-walled open-frameworks with one-dimensional parallelogram channels and have guest/coordinated water and carbonyl solvent molecules, reasonably providing a good example of the competitive behavior of water and carbonyl solvent molecules and an excellent candidate for studying the single crystal coordinated solvent exchange transformations. Interestingly, because of the different steric hindrance of the series...

Effect of Coordinated Solvent Molecules on Metal Coordination Sphere and Solvent-Induced Transformations

The self-assembly properties of the proximal p-tert-butylcalix[4]dihydroquinone compound have been studied to investigate the role played by crystallization conditions in driving the formation of a previously reported cubic porous framework. In chloroform and anhydrous ethyl acetate, the mutual inclusion of the tert-butyl groups is favored, leading to the cubic porous structure; otherwise, in the presence of a higher water amount, the OH groups provide H-bonds with bridging water molecules and a new triclinic crystal structure is obtained, in which the calixarene molecules include chloroform inside their cavities. By exposing a cubic/triclinic powder mixture to acetonitrile vapors, a new monoclinic chiral crystal structure is obtained by supramolecular assembly of calixarene, acetonitrile, and water molecules with the formation of single handed helices.

Solvent Induced Pseudopolymorphism in a Calixarene-Based Porous Host Framework

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Solvent Induced Pseudopolymorphism in a Calixarene-Based Porous Host Framework