合成了无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3],并采用元素分析、红外光谱表征和单晶X射线衍射分析和热重分析研究.红外光谱分析表明SCN-采用1,3-μ模式.结构分析表明,相邻的Cd(II)原子通过三个1,3-μ-SCN- 阴离子桥连形成无限的[Cd(SCN)-3]∞之字链结构,固体结构中[C12H11N2O2]+阳离子和[Cd(SCN)-3]∞配阴离子形成了分离柱状堆积.该晶体属于单斜晶系P2(1)/c空间群,晶胞参数分别为:a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3 , T = 293(2) K, μ = 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)]. 热分析结果在180-305 ℃化合物失去一个有机分子,305 ℃以上伴随着镉升华失去三个SCN-阴离子.
A new inorganic-organic hybrid compound [NO2BzPy][Cd(SCN)3], where [NO2BzPy]+ = 1-(4' -nitro-benzyl)pyridinium, was synthesized and characterized by elemental analysis, IR spectroscopy, TG analysis and single-crystal X-ray diffraction. The results of IR analysis show that the SCN- anions are coordinated in a di-1,3-μ bridge mode. Adjacent Cd(II) atoms are linked by three 1,3-μ-SCN- anions forming infinite [Cd(SCN)-3]∞ zigzag polymeric chains. In the crystal structure of the title compound, cations and ations form completely segregated stacking column along the direction of c-axis. Crystal data: monoclinic, space group P2(1)/c with a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3, T= 293(2) K, μ= 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)].Thermogravimentric analysis reveal the organic molecule is lost in the range of 180-305 ℃ and three SCN- anions are lost after 305 ℃ accompanying the sublimation of cadmium.
参考文献
| [1] | Hollingsworth M D .Crystal Engineering:from Structure to Function[J].Science,2002,295:2410-2413. |
| [2] | Sun, AW;Lauher, JW;Goroff, NS .Preparation of poly(diiododiacetylene), an ordered conjugated polymer of carbon and iodine[J].Science,2006(5776):1030-1034. |
| [3] | Zhang H;Wang XM;Teo BK .MOLECULAR DESIGN AND CRYSTAL ENGINEERING OF A NEW SERIES OF INORGANIC POLYMERS SEPARATED BY ORGANIC SPACERS - STRUCTURES OF [(18C6)K][CD(SCN)(3)] AND [(18C6)(2)NA-2(H2O)(2)](1/2)[CD(SCN)(3)][J].Journal of the American Chemical Society,1996(47):11813-11821. |
| [4] | Zhang H.;Price GE.;Teo BK.;Zelmon DE. .Wide spectral range nonlinear optical crystals of one-dimensional coordination solids [Et4N][Cd(SCN)(3)] and [Et4N][Cd(SeCN)(3)] and the general design criteria for [R4N][Cd(XCN)(3)] (where R = alkyl and X = S, Se, Te) as NLO crystals[J].Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics,2000(9):1868-1873. |
| [5] | Miller J S;Epstein A J .Organic and Organometallic Molecular Magnetic Materials-Designer Magnets[J].Angewandte Chemie International Edition,1994,33(04):385-415. |
| [6] | Dongbin Dang;Chunlin Ni;Yan Bai;Zhengfang Tian;Zhaoping Ni;Lili Wen;Qingjin Meng;Song Gao .Peculiar Magnetic Transition Behaviour Around 208 K in One-dimensional Nickel(III) Chain Complex [l-(4'-Vinylbenzyl)pyridinium][Ni(mnt)2] (mnt~(2-) = Maleonitriledithiolate)[J].Chemistry Letters,2005(5):680-681. |
| [7] | Dang DB;Bai Y;Wen LL;Tian ZF;Li YZ;Meng QJ .Crystal and molecular structures of two nickel maleonitriledithiolate complexes containing 1-methyl-3-(2 '-nitryl-4 '-bromo-benzyl)-imidazolium cations[J].Journal of Molecular Structure,2005(1/3):99-103. |
| [8] | Dan DD;Ni CL;Bai Y;Tian ZF;Wen LL;Meng QJ;Gao S .Synthesis, crystal structure and magnetic properties of a nickel(III) maleonitriledithiolate complex using 1-methyl-3-benzylbenzimidazolium cation[J].Journal of Molecular Structure,2005(1/3):197-200. |
| [9] | Bulgarevich S B;Bren D V;Movshovic D Y et al.Conformational Investigation of N-aralkylpyridinium Ions by Cotton-mouten Effect Method[J].Journal of Molecular Structure,1994,317:147-155. |
| [10] | Sheldrick G.M .SHELXL,Structure Determination Software Program[CP].Bruker Analytical X-ray System Inc.,Madison,Wisconsin,USA,1997. |
| [11] | Banerjee S.;Drew MGB.;Ghosh A. .Construction of coordination polymers of cadmium(II) with mixed hexamethylenetetramine and terephthalate or thiocyanate ligands[J].Polyhedron: The International Journal for Inorganic and Organometallic Chemistry,2003(21):2933-2941. |
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