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Lewis-base adducts of Group 1B metal(I) compounds. Part 17. Synthesis and crystal structures of adducts of copper(I) cyanide with nitrogen bases

机译:1B族金属(I)化合物的路易斯碱加合物。第17部分。氰化亚铜与氮碱的加合物的合成和晶体结构

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摘要

Compounds of the type [Cu(CN) L,] [L = diethylamine, (1 ), triethylamine, (2), 4-methylpyridine, (3), or 1 ,1 0-phenanthroline, (4)] have been synthesized by recrystallization of copper(i) cyanide from (or with) the parent base and their crystal structures have been determined by single-crystal X-ray diffraction methods; n = 1 except in the case of (3) where n = 1.5. Crystals of (1) are monoclinic, space group P2,/n, with a = 15.1 08(7), b = 7.321 (5), c = 13.699(6) A, p = 103.00(4)", and Z = 8; R was 0.044 for No = 871 independent 'observed' reflections. For (2), crystals are orthorhombic, space group Pnma, with a = 9.501 (4), b = 8.921 (4), c = 11.279(5) A, and Z = 4; R = 0.039, No = 369. For (3), crystals are monoclinic, space group Cc,with a = 9.587(3), b = 16.326(4), c = 14.022(4) A, p = 109.38(2)", and Z = 4; R = 0.031, No = 1 070. For (4), crystals are trigonal, space group P3,, with a = 9.1 75(5), c = 11.753(8) A, and Z = 3; R = 0.041, No = 81 2. All complexes are one-dimensional polymers, that in (2) being disposed completely in a mirror plane except for the substituent alkyl groups. Copper atoms in (1 ) and (2) are trigonally planar co-ordinated by C,N(cyanide) and N(base), as is one of the two copper atoms in (3);the other copper atom in (3) is unusual, being four-co-ordinated pseudo-tetrahedrally by C,N(cyanide) and two N(base). A similar copper environment is found in (4).
机译:已合成[Cu(CN)L,]类型的化合物[L =二乙胺,(1),三乙胺,(2),4-甲基吡啶,(3)或1,1 0-菲咯啉,(4)]用单晶X射线衍射法测定了从(或与之)母体碱中氰化亚铜(i)的重结晶。 n = 1,但(3)中n = 1.5时除外。 (1)的晶体是单斜晶体,空间群P2,/ n,a = 15.1 08(7),b = 7.321(5),c = 13.699(6)A,p = 103.00(4)“,Z = 8;对于No = 871的独立“观察”反射,R为0.044。对于(2),晶体是正交晶体,空间群Pnma,a = 9.501(4),b = 8.921(4),c = 11.279(5)A对于(3),晶体是单斜晶体,空间群Cc,其中a = 9.587(3),b = 16.326(4),c = 14.022(4)A,并且Z = 4; R = 0.039,No = 369。 p = 109.38(2)“,Z = 4; R = 0.031,No = 1070。对于(4),晶体是三角形的,空间群P3,其中a = 9.1 75(5),c = 11.753(8)A,Z = 3; n = 1。 R = 0.041,No = 81 2.所有配合物均为一维聚合物,在(2)中,除取代基烷基外,全部完全位于镜面。 (1)和(2)中的铜原子与C,N(氰化物)和N(碱)呈三角形平面配位,与(3)中的两个铜原子之一相同;(3)中的另一个铜原子是不寻常的,由C,N(氰化物)和两个N(基数)伪四面体四配位。在(4)中发现了类似的铜环境。

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