Supramolecular Assemblies of (±-2,2''''-Dihydroxy-1,1''''-binaphthyl with 2,2''''-Bipyridine and Naphthodiazine

Introduction Optically active 1,1'-bi-2-naphthol (BINOL) and its derivatives have been widely used as chiral ligands of catalysts for asymmetric reactions and effective host compounds for the isolation or optical resolution of a wide range of organic guest molecules through the for-mation of crystalline inclusion complexes.1,2 The wide-ranging and important applications of these com-pounds in organic synthesis have stimulated great inter-est in developing efficient methods for their prepara-…     

Two Co(Ⅱ) Coordination Polymers Based on 3,5-Di(4H-1,2,4-triazole-4-yl)benzoic Acid Ligand: Syntheses,Structures and Magnetic Property

Two Co(Ⅱ) coordination polymers, namely [Co(L)Cl]_n(1) and [Co(L)(CH_3 COO)]_n(2), {HL = 3,5-di(4 H-1,2,4-triazole-4-yl)benzoic acid}, were synthesized under hydrothermal conditions. Compound 1 crystallizes in orthorhombic system, space group Pmma with a = 7.032(5), b = 11.555(8), c = 8.185(5) ?, V = 665.1(7) ?~3, Z = 2, Dc = 1.746 g/cm3~, F(000) = 350, Mr = 349.61, μ = 1.504 mm~(-1), the final R = 0.0568 and w R = 0.1739 for 2312 observed reflections with I 2σ(I). Compound 2 crystallizes in orthorhombic system, space group Pmma with a = 7.7505(17), b = 11.391(3), c = 8.0298(18) ?, V = 708.9(3) ?~3, Z = 2, Dc = 1.748 g/cm~3, F(000) = 378, Mr = 373.20, μ = 1.245 mm-1, the final R = 0.0350 and w R = 0.0873 for 5239 observed reflections with I 2σ(I). Single-crystal X-ray analyses revealed that complexes 1 and 2 exhibit similar 2 D layer structures with uncoordinated carboxyl as dangling arms. The neighboring layers are further connected by these arms, leading to interest 2 D → 3 D polythreading frameworks. Moreover, the magnetic susceptibility study indicates compound 1 exhibits antiferromagnetic behavior.     

Two Nickel（Ⅱ） Complexes Constructed by Novel Bis（3-methoxy-2-pyridyl）ether-6,6′-dicarboxylic Acid Ligand： Lattice Water Control of Structure

Under given conditions, two complexes of [Ni（H20）2BEDA]·2H2O 1 and [Ni（Py）2- BEDA]·6H2O 2 （BEDA = bis（3-methoxy-2-pyridyl）ether-6,6′-dicarboxylic acid） have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Crystal data for 1： C14H18NiN2O11, monoelinic C2/c, a = 14.3844（17）, b = 12.9900（15）, c = 9.6309（11） A, β = 104.3350（10）°, V= 1743.5（4） A3, Z = 4, Dc= 1.711 g/cm^3, F（000） = 928, μ = 1.179 mm^-1, Mr= 449.01, the final R = 0.0228 and wR = 0.0625. Crystal data for 2： C24H32NiN4O13, triclinic P1, a = 9.423（2）, b = 11.863（3）, c = 13.089（3） A, α = 91.511（3）, β = 92.465（3）, γ = 100.696（2）°, V = 1435.6（6） A^3, Z = 2, Dc= 1.488 g/cm^3, F（000） = 672, μ = 0.748 mm^-1, Mr= 643.25, the final R = 0.0400 and wR = 0.0975. Interestingly, in the two complexes, lattice water molecules dominate its crystal structures. Therefore, extensive intermolecular hydrogen bonds assemble 1 and 2 into 2D extended sheets and a 3D open framework, respectively. Furthermore, water molecules present in 2 are associated to form water clusters.     

Crystal Structure and Spectroscopic Properties of[Ni（phen）3]Pic2.2CH3CN

1　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｔｈｅｐｒｏｃｅｓｓｏｆｔｈｅｐｒｅｐａｒａｔｉｏｎｏｆＮｉ(Ｐｉｃ) 2 Ｌ(Ｌ =1 ,3 ｂｉｓ (2 ｆｏｒｍｙｌｐｈｅｎｏｘｙ) 2 ｈｙｄｒｏｘｙｌ ｐｒｏｐａｎｅｔｈｉｏｓｅｍｉｃａｒｂａｚｏｎｅ )ｍｉｘｅｄｃｏｍｐｌｅｘｗｉｔｈｐｈｅｎ,ａｒｅｄｃｒｙｓｔａｌｗａｓｏｂｔａｉｎｅｄｉｎａｃｅｔｏｎｉｔｒｉｌｅｓｏｌｕｔｉｏｎ .Ｈｏｗｅｖｅｒ,ｔｈｅｅｌｅｍｅｎｔａｌａｎａｌｙｓｉｓｒｅｓｕｌｔｓｏｆｔｈｅｒｅｄｃｒｙｓｔａｌｉｎｄｉｃａｔｅｄｔｈａｔｉｔｉｓｎｏｔｔｈｅ…     

1-{[2-(1,3-二苯基-1H-萘[1,2-e][1,3]-2-噁嗪基)环己氨基]-苯基-甲基}-2-萘酚的合成与晶体学表征

具有光学活性的1,2-二氨基环己烷及其衍生物作为手性辅剂或手性配体被广泛地用在催化不对称合成中[1-3].最近,我们在无溶剂的条件下,利用(1R,2R)-1,2-二氨基环己烷与2-萘酚、苯甲醛反应一锅法合成手性配体1的过程中,没有得到目标化合物1,得到了一种新的1,2-二氨基环己烷衍生物2.经元素分析,IR,1H NMR,13C NMR,MS以及X射线单晶衍射,确定了2的结构,结果表明2中含有五个手性中心.本文报道2的合成与晶体学表征(Scheme 1).     

Synthesis and Crystal Structure of 3,3＇-Bis（2-benzimidazolyl）-2,2＇-dipyridine with Hydrated Zinc（Ⅱ） Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(II) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr = 1259.38) belongs to the monoclinic system, space group C2/c with a = 20.874(2), b = 14.9953(16), c = 20.462(3) , β = 101.553(2)°, V = 6274.8(13) 3, Z = 4, Dc = 1.333 g/cm3, F (000) = 2608, μ(MoKα) = 0.548 mm–1, R = 0.0682 and wR = 0.1931 for 4984 observed reflections with I > 2σ(I). The Zn(II) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2+ cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

两个基于半刚性双甲基苯并咪唑配体的螺旋型镉配位聚合物

以1,4-双（2-甲基苯并咪唑-1-亚甲基）苯（bmb）为主配体与Cd（NO₃）₂反应,通过改变辅助双羧酸配体2个羧基间的连接基团,得到了2个配位聚合物{[Cd（bmb）（tba）]·DMF}_n（1）和[Cd（bmb）（ada）]_n（2）（H₂tda=5-叔丁基间苯二甲酸,H₂ada=1,3-金刚烷二乙酸）。结构分析表明聚合物1显示二维三明治结构,带有交替的左手和右手螺旋链。聚合物2也显示了二维三明治结构,带有meso-螺旋和微孔。聚合物1和2都显示了强的荧光发射和高的热稳定性。     

两个基于柔性双苯并咪唑配体的锌配位聚合物的合成、晶体结构和荧光性质

以1,4-双(2-甲基苯并咪唑-1-亚甲基)苯(bmb)和2个芳香多羧酸1,2,4,5-均苯四酸(H4btec)、4-(3,4-二羧基苯甲酰)邻苯二甲酸(H4dcbp)为配体,在水热条件下合成了2个锌配位聚合物{[Zn(bmb)_(0.5)(btec)_(0.5)(H_2O)]·H_2O}_n(1)和{[Zn_2(bmb)_2(dcbp)]·5H_2O}_n(2),并用X射线单晶衍射、红外光谱、元素分析和粉末衍射对其结构进行了表征。晶体结构测试表明2个聚合物均为复杂的三维框架结构,配体bmb在2个配合物中均为μ_2-η~1∶η~1的配位模式。此外还研究了2个配合物的荧光性质和热稳定性。