Three new coordination networks based on a versatile and unsymmetric building block 3-(sulfonyl-glycine)benzoic acid (HAL) ligand and inorganic Co(Ⅱ) salt, [Co(HL)(bipy)2]. ClO4·1.5H2O (1), [Co3(L)2(H2O)6]·4H2O (2) and [Co(HL)(bpp)(H2O)2]·2H2O (3) (bipy = 2,2-bipyridine, bpp = 1,3-bi(4-pyridyl)propane), have been synthesized in aqueous media and structurally characterized by single-crystal X-ray diffraction. Reaction of Co salt with H3L afforded a neutral 1D alternating chain, which shows a 3-D supramolecular network through hydrogen bonds. When the auxiliary 2,2-bipyridine is used, a mononuclear unit is constructed; if using auxiliary ligand bpp, a neutral 1-D uniform chain is obtained and further extended into a 3-D supramolecular structure through versatile hydrogen bonds. The H3L ligand in 1 adopts a bidentate chelating coordination mode while that in 2 and 3 assumes a pentadentate bridging and a bis-monodentate bridging modes, respectively. This work and our previous work evidently demonstrate that the structures vary with altering the second ligands.
A new Cd(Ⅱ) complex([Cd(H2PIDC)2]n) with singly deprotonated 2-propyl-imidazole-4,5-dicarboxylate as bridging ligand was synthesized and characterized by X-ray diffraction method.Crystal data:monoclinic,space group P21/c,with a=8.2547(11),b=10.7071(15),c=13.9131(14)A,β=126.164(5)o,V=992.8(2)A^3,C16H18N4O8Cd,Mr=506.74,Z=2,Dc=1.695g/cm^3,F(000)=508,μ=1.151 mm^-1,R=0.0296 and wR=0.0812 for 1581 observed reflections.Singly deprotonated ligands(H2PIDC-) act as μ3-bridge and join the Cd(Ⅱ) atoms into a 2-D layer structure.The 2-D layers are further linked by intermolecular hydrogen bonds into a 3D network.The luminescent property of the complex was also investigated.
A novel complex [Na(NIT-1'-MeBzIm)3]ClO4 (NIT-1'-MeBzIm = 2-{2'-[(1'- methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by elemental analysis, IR spectra and X-ray diffraction methods. The title complex crystallizes in trigonal, space group P3 and Z = 2. Crystal data: C45H57ClN12NaO10, Mr = 984.47, a = 13.9411(8), b = 13.9411(8), c = 14.8622(16) A, γ= 120°, V= 2501.5(3) A^3, Dc = 1.307 g/cm^3, μ(MoKα) = 0.152 mm^-1, F(000) = 1038, R = 0.0637 and wR = 0.1813 for 1957 observed reflections with I 〉 2σ(I). X-ray analysis reveals that the Na(I) ion is six-coordinated with three NIT-1'-MeBzlm radicals. As we know, three radicals coordinating to the Na(I) ion in the main group by a chelate way is the first example. The Na(I) ion resides in a distorted octahedron with a facial configuration. Meanwhile, the intermolecular weak interactions result in a 2-D double layer conformation where the uncoordinated perchlorate anions are inserted in the packing space and take part in the H-bond interactions, and each complex is connected with six neighboring complexes and three perchlorate anions.
Spinel structure ferrites MFe2O4(M = Co,Ni,Mn,Zn) nano-octahedrons have been fabricated by a simple hydrothermal route under mild conditions,using sodium citrate as addition agent.The products were characterized in detail by XRD,TEM and ED.The growth process was also monitored by NaOH concentration,temperature and citrate-dependent observations.It was found that the reaction temperature had no obvious influence on the morphology of the products,while NaOH concentration had great effect on the morphology of the final products.The edge size of octahedral ferrites was estimated to 100-200 nm at the hydrothermal temperature of 180 ℃.Vibrating sample magnetometer was used to characterize magnetic properties of octahedral ferrites at room temperature.Magnetic measurements showed that these ferrites exhibited obvious ferromagnetic behaviors.
A new complex [Zn(NIT-1′-MeBzlm)Cl2(H2O)] (NIT-1′-MeBzlm = 2-{2′-[(1′- methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method. Crystal data: monoclinic, space group P21/n, Z = 4, C15H21Cl2N4O3Zn, Mr = 441.63, a = 7.2225(10), b = 30.849(4), c = 8.8758(13)A, β = 103.904(2)°, V = 1919.6(5)A^3, Dc = 1.528 g/cm^3, μ(MoKα) = 1.579 mm^-1, F(000) = 908, R = 0.0436 and wR = 0.1029 for 2456 observed reflections with I〉 2σ(I). X-ray analysis reveals that the Zn(Ⅱ) ion is four-coordinated with a distorted tetrahedron. There also exist H-bonds, π-π piling interactions and weak intermolecular contacts between the NO groups which form a mutual stagger 3-D network configuration. Magnetic investigation reveals that there exists intermolecular antiferro- and ferromagnetic interactions in the title complex.