Laboratoire de l'Etat Solide, Département de Chimie, Université de Sfax, BP 1171, 3000 Sfax, Tunisia.
Dalton Trans. 2011 Nov 21;40(43):11613-20. doi: 10.1039/c1dt11030f. Epub 2011 Sep 29.
A series of novel organically templated metal sulfates, [C(5)H(14)N(2)]M(II)(H(2)O)(6)(2) with (M(II) = Mn (1), Fe (2), Co (3) and Ni (4)), have been successfully synthesized by slow evaporation and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, thermogravimetric analysis and magnetic measurements. All compounds were prepared using a racemic source of the 2-methylpiperazine and they crystallized in the monoclinic systems, P2(1)/n for (1, 3) and P2(1)/c for (2,4). Crystal data are as follows: [C(5)H(14)N(2)]Mn(H(2)O)(6)(2), a = 6.6385(10) Å, b = 11.0448(2) Å, c = 12.6418(2) Å, β = 101.903(10)°, V = 906.98(3) Å(3), Z = 2; [C(5)H(14)N(2)]Fe(H(2)O)(6)(2), a = 10.9273(2) Å, b = 7.8620(10) Å, c = 11.7845(3) Å, β = 116.733(10)°, V = 904.20(3) Å(3), Z = 2; [C(5)H(14)N(2)]Co(H(2)O)(6)(2), a = 6.5710(2) Å, b = 10.9078(3) Å, c = 12.5518(3) Å, β = 101.547(2)°, V = 881.44(4) Å(3), Z = 2; [C(5)H(14)N(2)]Ni(H(2)O)(6)(2), a = 10.8328(2) Å, b = 7.8443(10) Å, c = 11.6790(2) Å, β = 116.826(10)°, V = 885.63(2) Å(3), Z = 2. The three-dimensional structure networks for these compounds consist of isolated M(II)(H(2)O)(6) and C(5)H(14)N(2) cations and (SO(4))(2-) anions linked by hydrogen-bonds only. The use of racemic 2-methylpiperazine results in crystallographic disorder of the amines and creation of inversion centers. The magnetic measurements indicate that the Mn complex (1) is paramagnetic, while compounds 2, 3 and 4, (M(II) = Fe, Co, Ni respectively) exhibit single ion anisotropy.
一系列新型有机模板金属硫酸盐[C(5)H(14)N(2)]M(II)(H(2)O)(6)(2)（其中 M(II) = Mn(1)、Fe(2)、Co(3)和 Ni(4))，通过缓慢蒸发成功合成，并通过单晶 X 射线衍射、红外光谱、热重分析和磁性测量进行了表征。所有化合物均使用 2-甲基哌嗪的外消旋源制备，它们在单斜晶系 P2(1)/n 中结晶(1,3)和 P2(1)/c(2,4)。晶体数据如下：[C(5)H(14)N(2)]Mn(H(2)O)(6)(2)，a = 6.6385(10)Å，b = 11.0448(2)Å，c = 12.6418(2)Å，β = 101.903(10)°，V = 906.98(3)Å(3)，Z = 2；[C(5)H(14)N(2)]Fe(H(2)O)(6)(2)，a = 10.9273(2)Å，b = 7.8620(10)Å，c = 11.7845(3)Å，β = 116.733(10)°，V = 904.20(3)Å(3)，Z = 2；[C(5)H(14)N(2)]Co(H(2)O)(6)(2)，a = 6.5710(2)Å，b = 10.9078(3)Å，c = 12.5518(3)Å，β = 101.547(2)°，V = 881.44(4)Å(3)，Z = 2；[C(5)H(14)N(2)]Ni(H(2)O)(6)(2)，a = 10.8328(2)Å，b = 7.8443(10)Å，c = 11.6790(2)Å，β = 116.826(10)°，V = 885.63(2)Å(3)，Z = 2。这些化合物的三维结构网络由孤立的M(II)(H(2)O)(6)和C(5)H(14)N(2)阳离子和(SO(4))(2-)阴离子通过氢键连接而成。使用外消旋 2-甲基哌嗪导致胺的结晶无序和反演中心的形成。磁性测量表明，Mn 配合物(1)是顺磁性的，而化合物 2、3 和 4(分别为 M(II) = Fe、Co、Ni)则表现出单离子各向异性。
