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包含氰基桥联镧系（III）和过渡金属的异金属一维阵列

Heterometallic One-Dimensional Arrays Containing Cyanide-Bridged Lanthanide(III) and Transition Metals.

作者信息

Knoeppel David W., Liu Jianping, Meyers Edward A., Shore Sheldon G.

机构信息

Department of Chemistry, The Ohio State University, Columbus, Ohio 43210.

出版信息

Inorg Chem. 1998 Sep 21;37(19):4828-4837. doi: 10.1021/ic980449h.

DOI:10.1021/ic980449h
PMID:11670646
Abstract

One-dimensional arrays having the general formula {(DMF)(10)Ln(2)M(CN)(4)}(infinity) [Ln = Sm, Eu, Er, Yb and M = Ni, Pd, Pt] were prepared from the reactions of 2:3 molar ratios of LnCl(3) with K(2)[M(CN)(4)] in DMF (DMF = N,N-dimethylformamide). Under similar conditions using 1:1 molar ratios of SmCl(3) and K(2)[Ni(CN)(4)] in DMF or YbCl(3) and K(2)[Ni(CN)(4)] in DMA (DMA = N,N-dimethylacetamide), the one-dimensional arrays {(DMF)(5)Sm[Ni(CN)(4)]Cl}(infinity), 8, and {(DMA)(4)Yb[Ni(CN)(4)]Cl}(infinity), 9, were prepared. An earlier study of {(DMF)(10)YbNi(CN)(4)}(infinity), 3, and {(DMF)(10)Yb(2)Pt(CN)(4)}(infinity), 7, showed that two different yet related one-dimensional arrays can be adopted. In the present study, X-ray crystal structures of {(DMF)(10)Sm(2)Ni(CN)(4)}(infinity), 1, and {(DMF)(10)Er(2)Ni(CN)(4)}(infinity), 2, are shown to be isomorphous with {(DMF)(10)Yb(2)Ni(CN)(4)}(infinity), 3, while {(DMF)(10)Sm(2)Pd(CN)(4)}(infinity), 4, {(DMF)(10)Eu(2)Pd(CN)(4)}(infinity), 5, and {(DMF)(10)Yb(2)Pd(CN)(4)}(infinity), 6, are isomorphous with {(DMF)(10)Yb(2)Pt(CN)(4)}(infinity), 7. Single-crystal X-ray crystal structure determinations reveal that arrays 1, 2, and 3 consist of cyanide-bridged "diamond"-shaped Ln(2)Ni(2) metal cores. These metal cores are linked together in an infinite array through cyanide bridges by Ni(CN)(4)(-) anions generating a single-strand chain. Crystal data for 1: triclinic space group P&onemacr;, a = 10.442(5) Å, b = 10.923(2) Å, c = 15.168(3) Å, alpha = 74.02(2) degrees, beta = 83.81(3) degrees, gamma = 82.91(2) degrees, Z = 2. Crystal data for 2: triclinic space group P&onemacr;, a = 10.172(1) Å, b = 11.111(3) Å, c = 15.369(2) Å, alpha = 73.17(2) degrees, beta = 85.15(1) degrees, gamma = 83.48(2) degrees, Z = 2. Arrays 4, 5, 6, and 7 consist of two parallel zigzag chains that are linked together through bridging M(CN)(4)(-) anions. Crystal data for 4: triclinic space group P&onemacr;, a = 9.304(2) Å, b = 11.351(3) Å, c = 16.257(5) Å, alpha = 81.62(2) degrees, beta = 77.51(2) degrees, gamma = 82.47(2) degrees, Z = 2. Crystal data for 5: triclinic space group P&onemacr;, a = 9.300(3) Å, b = 11.353(4) Å, c = 16.279(3) Å, alpha = 81.58(2) degrees, beta = 77.37(2) degrees, gamma = 81.58(2) degrees, Z = 2. Crystal data for 6: triclinic space group P&onemacr;, a = 9.164(2) Å, b = 11.718(3) Å, c = 16.122(3) Å, alpha = 79.88(2) degrees, beta = 74.43(2) degrees, gamma = 80.50(2) degrees, Z = 2. Electrical conductance, NMR, and infrared studies of DMF solutions of 1-7 reveal that these arrays are partially ionized in solution. Single-crystal X-ray analyses of the one-dimensional arrays 8 and 9 show that these complexes adopt the commonly observed zigzag chain structure. Crystal data for 8: monoclinic space group P2(1)/n, a =7.783(2) Å, b = 17.748(8) Å, c = 21.236(5) Å, beta = 92.87(2) degrees, Z = 4. Crystal data for 9: monoclinic space group P2(1)/n, a = 10.022(2) Å, b = 19.505(4) Å, c = 15.742(3) Å, beta = 105.94(2) degrees, Z = 4. Studies of 8 and 9 in DMF and DMA, respectively, indicate that 8 is partially ionized and 9 is almost completely ionized.

摘要

通式为{(DMF)(10)Ln(2)M(CN)(4)}(∞) [Ln = Sm、Eu、Er、Yb，M = Ni、Pd、Pt]的一维阵列是由LnCl(3)与K(2)[M(CN)(4)]以2:3的摩尔比在N,N - 二甲基甲酰胺（DMF）中反应制备而成。在相似条件下，使用SmCl(3)与K(2)[Ni(CN)(4)]以1:1的摩尔比在DMF中反应，或者YbCl(3)与K(2)[Ni(CN)(4)]以1:1的摩尔比在N,N - 二甲基乙酰胺（DMA）中反应，制备出了一维阵列{(DMF)(5)Sm[Ni(CN)(4)]Cl}(∞)（8）和{(DMA)(4)Yb[Ni(CN)(4)]Cl}(∞)（9）。早期对{(DMF)(10)YbNi(CN)(4)}(∞)（3）和{(DMF)(10)Yb(2)Pt(CN)(4)}(∞)（7）的研究表明，可以采用两种不同但相关的一维阵列。在本研究中，{(DMF)(10)Sm(2)Ni(CN)(4)}(∞)（1）和{(DMF)(10)Er(2)Ni(CN)(4)}(∞)（2）的X射线晶体结构显示与{(DMF)(10)Yb(2)Ni(CN)(4)}(∞)（3）同构，而{(DMF)(10)Sm(2)Pd(CN)(4)}(∞)（4）、{(DMF)(10)Eu(2)Pd(CN)(4)}(∞)（5）和{(DMF)(10)Yb(2)Pd(CN)(4)}(∞)（6）与{(DMF)(10)Yb(2)Pt(CN)(4)}(∞)（7）同构。单晶X射线晶体结构测定表明，阵列1、2和3由氰基桥连的“菱形”Ln(2)Ni(2)金属核组成。这些金属核通过[Ni(CN)(4)]²⁻阴离子通过氰基桥在无限阵列中连接在一起，形成单链链。1的晶体数据：三斜晶系空间群P&onemacr;，a = 10.442(5) Å，b = 10.923(2) Å，c = 15.168(3) Å，α = 74.02(2)°，β = 83.81(3)°，γ = 82.91(2)°，Z = 2。2的晶体数据：三斜晶系空间群P&onemacr;，a = 10.172(1) Å，b = 11.111(3) Å，c = 15.369(2) Å，α = 73.17(2)°，β = 85.15(1)°，γ = 83.48(2)°，Z = 2。阵列4、5、6和7由两条平行的之字形链组成，它们通过桥连的[M(CN)(4)]²⁻阴离子连接在一起。4的晶体数据：三斜晶系空间群P&onemacr;，a = 9.304(2) Å，b = 11.351(3) Å，c = 16.257(5) Å，α = 81.62(2)°，β = 77.51(2)°，γ = 82.47(2)°，Z = 2。5的晶体数据：三斜晶系空间群P&onemacr;，a = 9.300(3) Å，b = 11.353(4) Å，c = 16.279(3) Å，α = 81.58(2)°，β = 77.37(2)°，γ = 81.58(2)°，Z = 2。6的晶体数据：三斜晶系空间群P&onemacr;，a = 9.164(2) Å，b = 11.718(3) Å，c = 16.122(3) Å，α = 79.88(2)°，β = 74.43(2)°，γ = 80.50(2)°，Z = 2。对1 - 7的DMF溶液进行的电导率、核磁共振和红外研究表明，这些阵列在溶液中部分电离。对一维阵列8和9的单晶X射线分析表明，这些配合物采用常见的之字形链结构。8的晶体数据：单斜晶系空间群P2(1)/n，a =7.783(2) Å，b = 17.748(8) Å，c = 21.236(5) Å，β = 92.87(2)°，Z = 4。9的晶体数据：单斜晶系空间群P2(1)/n，a = 10.022(2) Å，b = 19.505(4) Å，c = 15.742(3) Å，β = 105.94(2)°，Z = 4。分别在DMF和DMA中对8和9的研究表明，8部分电离，9几乎完全电离。

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