Utilizing N-[(4-carboxyphenyl)-sulfonyl]glycine (abbreviated as cbsglyH3),a new cobalt complex [Co(cbsglyH)(bipy)2]3H2O (bipy = 2,2'-bipyridine) has been synthesized under mild conditions and characterized by IR,elemental analysis,thermogravimetric analysis and X-ray diffraction analysis. It crystallizes in the monoclinic system,space group C2/c with a = 34.978(3),b = 12.0437(11),c = 20.0041(19) ,β = 122.2990(10)°,V = 7123.0(11) 3,Z = 8,C29H28CoN5O9S,Mr = 681.55,μ = 0.593 mm-1,Dc = 1.271 Kg/m3,F(000) = 2816,the final R = 0.0434 and wR = 0.1351. The title complex is a monomeric compound which is further assembled by intermolecular hydrogen bonds into a 3-D supramolecular network. Thermogravimetric analysis illustrates that this complex begins decomposing at 100 ℃ and decompounding completely at 560 ℃.
A new complex [Co(NIT-1′-MeBzIm)2Cl2](NIT-1′-MeBzIm = 2-{2′-[(l′-methyl)-benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method.The complex crystallizes in the monoclinic system,space group C2/c,Z = 4.Crystal data:C30H38Cl2CoN8O4,Mr = 704.51,a = 17.074(3),b = 21.350(3),c = 11.6962(19),β = 108.879(2)°,V = 4034.3(11)3,Dc = 1.160 g/cm3,μ(MoKα) = 0.597 mm-1,F(000) = 1468,R = 0.0422 and wR = 0.1141 for 2577 observed reflections with I 2σ(I).X-ray analysis reveals that the Co(Ⅱ) ion is six-coordinated with a distorted octahedral geometry.Temperature dependence of susceptibility measurements shows the existence of antiferromagnetic interactions between the Co(Ⅱ) ion and the radicals(J =-52.88 cm-1).
A novel two-dimensional self-assembly network formulated as [K(TSSB)]n (TSSB= taurine-salicylaldehyde Schiff base) has been synthesized via the reaction of salicylaldehyde with taurine at the presence of potassium hydroxide in water-methanol solution,and was structurally characterized by elemental analysis,IR,UV-VIS spectra and X-ray diffraction.It crystallizes in the monoclinic system,space group P21/c with a=20.245(3),b=7.2905(9),c=7.5458(10),β= 94.1920(10)o,V=1110.8(2)3,Mr=267.34,Z=4,Dc=1.599 g/cm3,μ(MoKα)=0.663 mm-1 and F(000)=552.The units of K[TSSB] are linked into a one-dimensional double chain structure via the sulfonic groups from the taurine-salicylaldelyde Schiff base,and such chains are further extended through O-K-O bond interactions resulting in a two-dimensional supramolecular architecture.In the complex,the K(I) ion displays a slightly distorted dodecahedral geometry with an eight-coordination number.
A novel dicyanamido-bridged 3D polymeric complex {[Zn2(bpa)2(dca)]dca}n (1) (dca = dicyanamide anion,bpa = 1,2-bis(4-pyridyl)ethane) has been synthesized by reacting 1,2-bis(4-pyridyl)ethane with zinc salt in the presence of sodium dicyanamide,and characterized by elemental analysis,IR spectra and X-ray diffraction. It crystallizes in the monoclinic system,space group C2/c with a = 18.587(3),b = 20.070(3),c = 8.7957(13) ,β = 100.611(2)o,V = 3225.0(8) 3,Mr = 539.92,μ = 0.789 mm-1,F(000) = 1116,Z = 4,ρ = 1.112 (g/cm3),R = 0.0582 and wR = 0.1762. Complex 1 forms a 3D porous framework through the bpa and dca ligands,and gives 1-D coordination channels encapsulated by the guest dca molecules. Complex 1 also displays strong photo-luminescent properties in the solid state at room temperature.
Reaction of 3,5-pyridine-dicarboxylic acid(3,5-PydcH2) with iron salt in hydrothermal condition results in the formation of a three-dimensional self-assembly network formulated as [C14H14Fe2N2O12]n,and it has been structurally characterized by elemental analysis,IR spectra and X-ray diffraction.It crystallizes in the monoclinic system,space group C2/c with a=9.9633(15),b=12.0942(18),c=7.4297(11)A and β=105.822o.The units of Fe2(pydc)2·2H2O are linked into a one-dimensional structure via the chelate carboxylate groups from the 3,5-pyridine-dicarboxylate.The interlayer hydrogen bonding interactions result in a three-dimensional supramolecular architecture.In the complex,the Fe(Ⅲ) ion displays a slightly distorted pentagonal bipyramidal geometry with seven coordination numbers.Cyclic-voltammetry measurement reveals the oxidation and reduction processes for the complex are quasi-reversible in nature.
A novel azide-bridged copper(Ⅱ) coordination polymer, [Cu3(NITpPy)4(N3)6]n (NITpPy = 4-pyridyl-4,4,5,5-tetramethylimidazline-3-oxide-1-oxyl), was structurally and magnetically characterized. It crystallizes in the triclinic space group P with a = 7.6932(10), b = 14.5556(19), c = 16.122(2) , α = 108.443(2), β = 95.251(2), γ = 104.236(2)°, V = 1631.7(4) 3, C48H64Cu3N30O8, Mr = 1379.87, Z = 1, Dc = 1.404 g/cm3, μ(MoKα) = 1.041 mm-1, F(000) = 713, the R = 0.0510 and wR = 0.1185 for 4285 observed reflections with I 2σ(I). X-ray analysis reveals that the Cu(Ⅱ) ions are linked by nitrogen atom of μ1,1 azido ligands to form a Cu-Cu-Cu unit. The units are linked by μ1,3 azido ligands through a bridging style to form a one-dimensional coordination polymer. The variable-temperature magnetic susceptibility data of the complex show ferromagnetic interactions in the complex.
Making use of N-P-acetamidobenzenesulfonyl-glycine acid (abbreviated as abglyH2),two transitional metal complexes [Zn(abglyH)(phen)2]ClO4·H2O (1) and Co(abglyH)2(bipy)2(H2O)2 (2) (phen = 1,10-phenanthroline,bipy = 4,4'-bipyridine) have been synthesized under mild conditions and characterized by IR,elemental analysis and X-ray diffraction analysis. Complex 1 is a monomeric compound which is further assembled by intermolecular hydrogen bonds and π-π interaction into a 2-D supramolecular network. Complex 2 is also a monomeric compound and further connected by intermolecular hydrogen bonds to form a 2-D supramolecular network. Fluorescent analysis shows that complex 1 has an emissive maximum at 364 nm in the solution state at room temperature.