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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Bipy, phen, and P(C6H4CH2NMe2-2)(3) in the synthesis of cationic silver(I) complexes; the solid-state structures of [P(C6H4CH2NMe2-2)(3)]AgOTf and [Ag(phen)(2)]OTf [German]
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Bipy, phen, and P(C6H4CH2NMe2-2)(3) in the synthesis of cationic silver(I) complexes; the solid-state structures of [P(C6H4CH2NMe2-2)(3)]AgOTf and [Ag(phen)(2)]OTf [German]

机译：Bipy，phen和P（C6H4CH2NMe2-2）（3）在阳离子银（I）配合物的合成中; [P（C6H4CH2NMe2-2）（3）] AgOTf和[Ag（phen）（2）] OTf的固态结构[德语]

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摘要

The reaction of [P(C6H4CH2NMe2-2)(3)]AgX (1a, X = OTf, 1b, X = OClO3) with equimolar amounts of (LL)-L-boolean AND (2a, (LL)-L-boolean AND = 2,2'-bipyridine, bipy; 2b, (LL)-L-boolean AND = 4,4'-dimethyl-2,2'-bipyridine, bipy'; 2c, (LL)-L-boolean AND = 1,10-phenanthroline, phen) leads to the formation of the cationic complexes {[P(C6H4CH2NMe2-2)(3)]Ag((LL)-L-boolean AND)}X-+(-) = bipy: 3a, X = OTf, 3b, X = ClO4; (LL)-L-boolean AND = bipy': 3c, X = OTf, 3d, X = ClO4; ((LL)-L-boolean AND = phen: 3e, X = OTf, 3f, X = ClO4) in which the building blocks (LL)-L-boolean AND and P(C6H4CH2NMe2-2)(3) act as bidentate chelating ligands and are datively-bound to the silver atom. Spectroscopic studies reveal that on the NMR time-scale the phosphane group is dynamic with exchanging the respective Me2NCH2 built-in arms. While complex 3e is stable in the solid-state, it appeared that solutions of 3e start to decompose upon precipitation of colloidal silver when they are heated or irradiated with light, respectively. Appropriate work-up of the reaction mixture allows the isolation of the phosphane P(C6H4CH2NMe2-2)(3) (5) along with [Ag(phen)(2)]OTf (4). The solid-state structures of neutral la and cationic 4 are reported. Mononuclear la crystallizes in the monoclinic space group P2(1)/c with the cell parameters a = 16.7763(2), b = 14.7892(2), c = 25.44130(10) Angstrom, beta = 106.1260(10), V = 6063.83(11) Angstrom(3) and Z = 4 with 8132 observed unique reflections (R-1 = 0.0712), while 4 crystallizes in the monoclinic space group C2/c with the cell parameters a = 26.749(3), b = 7.1550(10), c = 26.077(3) Angstrom, beta = 113.503(2), V = 4576.8(10) Angstrom(3) and Z = 4 with 6209 observed unique reflections (R-1 = 0.0481). The unit cell of 1a consists of two independent molecules. In both molecules the silver atom possesses a distorted tetrahedral coordination sphere and a boat-like conformation for the six-membered AgPNCH2C2/phenyl cycles is found. In 4, as typical for 1a, the silver atom possesses the coordination number 4. The two phen ligands are tilted by 40.63degrees. The OTf group is acting as non-coordinating counter ion. [References: 27]
机译：[P（C6H4CH2NMe2-2）（3）] AgX（1a，X = OTf，1b，X = OClO3）与等摩尔量的（LL）-L-布尔AND和（2a，（LL）-L-布尔）的反应AND = 2,2'-联吡啶，Bipy; 2b，（LL）-L-布尔AND = 4,4'-二甲基-2,2'-联吡啶，Bipy'; 2c，（LL）-L-布尔AND = 1,10-菲咯啉（phen）导致形成阳离子络合物{[P（C6H4CH2NMe2-2）（3）] Ag（（LL）-L-布尔AND）} X-+（-）= bipy：3a ，X = OTf，3b，X = ClO4; （LL）-L-布尔AND = bipy'：3c，X = OTf，3d，X = ClO4; （（LL）-L-布尔AND = phen：3e，X = OTf，3f，X = ClO4）其中，构建基（LL）-L-布尔AND和P（C6H4CH2NMe2-2）（3）充当双齿螯合配体，并与银原子键合。光谱研究表明，在NMR时标上，膦基是动态的，可以交换各自的Me2NCH2内置臂。尽管配合物3e在固态中是稳定的，但似乎当分别加热或照射光时，3e的溶液在胶态银沉淀时开始分解。对反应混合物进行适当的后处理可以分离出膦P（C6H4CH2NMe2-2）（3）（5）和[Ag（phen）（2）] OTf（4）。报道了中性1a和阳离子4的固态结构。单核la在单元参数a = 16.7763（2），b = 14.7892（2），c = 25.44130（10）埃，β= 106.1260（10），V = 6063.83的单斜空间群P2（1）/ c中结晶（11）Angstrom（3）和Z = 4，观察到8132次独特反射（R-1 = 0.0712），而4在单斜空间群C2 / c中结晶，单元参数a = 26.749（3），b = 7.1550（ 10），c = 26.077（3）埃，beta = 113.503（2），V = 4576.8（10）埃（3），Z = 4，有6209个观察到的独特反射（R-1 = 0.0481）。 1a的晶胞由两个独立的分子组成。在两个分子中，银原子均具有扭曲的四面体配位球，并发现了六元AgPNCH2C2 /苯基循环的船形构象。在4中，如典型的1a所示，银原子的配位数为4。两个phen配体倾斜40.63度。 OTf基团充当非配位抗衡离子。 [参考：27]

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