A novel complex [Na(NIT-1'-MeBzIm)3]ClO4 (NIT-1'-MeBzIm = 2-{2'-[(l'- 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 P 3 and Z = 2. Crystal data: C45H57ClN12NaO10, Mr = 984.47, a = 13.9411(8), b = 13.9411(8), c = 14.8622(16), γ = 120°, V = 2501.5(3)3, Dc = 1.307 g/cm3, 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'-MeBzIm 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.
A new complex [Zn(NIT-1'-MeBzIm)Cl2(H2O)] (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. 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) , β = 103.904(2)°, V = 1919.6(5) 3, Dc = 1.528 g/cm3, μ(MoKα) = 1.579 mm1, 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.
The self-assembly of Co(OAc)·4H2O with H2tbip and bipy (H2tbip = 5-tert-butyl isophthalic acid, bipy = 4,4'-bipyridine) generates one new complex, [Co3(tbip)2(Htbip)2(bipy)]n, which has been characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. Single-crystal X-ray analysis reveals that it crystallizes in the triclinic space group P1 with a = 9.471(6), b = 12.597(8), c = 12.899(8), α = 84.660(7), β = 70.548(7), γ = 81.965(7)o, V = 1435.1(15)3, Mr = 1215.85, Dc = 1.407 g/cm3, Z = 1, F(000) = 629, μ(MoKα) = 0.926 mm-1, the final R = 0.0623 and wR = 0.1724. The complex consists of a tbip bridged trinuclear cobalt() unit and is further linked by 4,4'-bipyridine molecule to form a 2D supramolecular network.
A new oxalato-bridged dinickel(Ⅱ) complex [Ni2(NIT-MeImz)4(C2O4)](Ac)2·8H2O has been synthesized and characterized structurally as well as magnetically.It crystallizes in monoclinic,space group C2/c with a=24.608(4),b=21.399(3),c=17.992(3),β=131.680(2)°,V=7076(2)3,C50H86N16Ni2O24,Mr=1412.77,Z=4,Dc=1.326 g/cm3,μ(MoKα)=0.614 mm-1,F(000)=2984,R=0.0751 and wR=0.1791 for 2956 observed reflections with Ⅰ>2σ(Ⅰ).X-ray analysis reveals that the crystal structure consists of [Ni2(NIT-MeImz)4(C2O4)]2+ moiety and two Ac-anions.Each nickel(Ⅱ) ion is six-coordinated with a distorted octahedral geometry:two nitrogen atoms and two oxygen atoms from NIT-MeImz together with two other oxygen atoms from the oxalato ion.The 2-D net structure is formed and arranged through intermolecular H-bonding interactions.Magnetic measurements show antiferromagnetic interactions for this complex.
A new one-dimensional dicyanamide bridged zinc(II) complex containing nitronyl nitroxide radicals Zn(NO3)(NIT-1'-MeBzIm)(dca)n·(H2O)n(NIT-1'-MeBzIm = 2-{2'-(l'-me-thyl)benzimidazolyl}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, dca = dicyanamide anion) has been prepared and structurally characterized by single-crystal X-ray diffraction.The complex crystallizes in triclinic, space group P1, with a = 7.428(3), b = 9.839(3), c = 16.708(6), α = 93.270(4), β = 101.642(4), γ = 100.632(4)°, C17.5H21N8O5.5Zn, Mr = 496.79, V = 1169.7(7) 3, Dc = 1.411 g/cm3, μ(MoKα) = 1.096 mm-1, Z = 2, F(000) = 512, R = 0.0583 and wR = 0.1663 for 4295 observed reflections with I > 2σ(I).X-ray analysis reveals that the zinc(II) ion is six-coordinated with a distorted octahedral geometry.These units develop as 1D species where dicyanamide ligands bridge zinc(II) ions.In addition, molecules are linked by π-π piling interactions to form 1-D double-chains.Magnetic investigation indicates that the weak intramolecular interactions are antiferromagnetic with J =-0.27 cm?1, where the spin Hamitonian is defined as H =-2∑i,jJi,jSiS within the complex.
Two new coordination polymers,{[Co(O2N-Hbtb)(phen)(H2O)3]·2H2O}n 1 and {[Cu3(O2N-btb)2(bipy)2(H2O)4]·4H2O}n 2(O2N-H3btb=5-nitro-1,2,3-benzenetricarboxylic acid,phen=1,10-phenanthroline,bipy=2,2'-bipyridine),were prepared through hydrothermal reactions of Co(Ⅱ) or Cu(Ⅱ) salt with O2N-H3btb in the presence of different auxiliary N-donor ligands.Their crystal structures were determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectroscopy.In the two complexes,O2N-H3btb ligand acts as monodentate and bis-monodentate modes,respectively.Complex 1 displays a two-dimensional layered structure through the inter-and intramolecular hydrogen bonding interactions while complex 2 has an O2N-btb bridged one-dimensional chain which is extended into a three-dimensional network by hydrogen bonding interactions.The magnetic properties of complex 2 are investigated over the temperature range of 2～300 K and ferromagnetic interactions are observed.
Three new coordination networks based on a versatile and unsymmetric building block 3-(sulfonyl-glycine)benzoic acid (H3L) 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.
