Dichloromethane is a coordinating solvent
Dichloromethane is a coordinating solvent
复制标题
二氯甲烷是配位溶剂
DOI：
10.1021/ja00192a052
复制
发表时间：
1989
影响因子：
15
通讯作者：
S. Strauss
中科院分区：
文献类型：
--
作者：
T. D. Newbound;Mark R. Colsman;M. Miller;G. Wulfsberg;O. P. Anderson;S. Strauss
2AgCl+ Ag2 (CH2Cl2) 4Pd (OTeF5) 4(1)过量PdCl2的存在；未形成Pd (OTeF5) 2。通过过滤将AgCl从反应混合物中除去后，将浓缩的二氯甲烷溶液缓慢冷却至20℃，生长出I的琥珀晶体。这些极吸湿的晶体在25℃时很容易在充满氮气的手套箱中脱落（由于二氯甲烷的损失）。两个对称相关的Ag (CH2Cl2) 2+基团由中心对称的Pd (OTeF5) 42”核心桥接，该核心包含一个平面Pd04阵列。在实验误差范围内，两种双齿二氯甲烷配体不受二氯甲烷气相结构的干扰：结合c - clv = 1.76 (2) A, cl - c - clv = 110.4 (6)；游离C-Cl= 1.7724 (5) Á， Cl-C-Cl= 111.78(2). 17含Cl的配体与Ag (I)离子结合更强（Ag- clv = 2.793 (3) Á）比配体con-(8)(a) Cook, p.m.；达尔，l.f.；迪克霍夫，DW J. Am。化学。社会科学学报，1992,9(4):531 - 531。(b)库克，p.m.论文，威斯康星大学，麦迪逊，1972年。
2AgCl+ Ag2 (CH2Cl2) 4Pd (OTeF5) 4 (1) the presence of excess PdCl2; no Pd (OTeF5) 2 was formed. After removing AgCl from the reaction mixture by filtration, amber crystals of I were grown by slowly cooling a concentrated dichloromethane solution to-20 C. These extremely hygroscopic crystals readily effloresce (by loss of dichloromethane) in a N2-filled glovebox at 25 C. Nevertheless, crystals of I were isolated, examined, and mounted on the diffractometer without allowing the crystals to warm to above-20 C. 5 Two symmetry-related Ag (CH2Cl2) 2+ moieties are bridged by the centrosymmetric Pd (OTeF5) 42" core, which contains a planar Pd04 array. To within experimentalerror, the two bidentate dichloromethane ligands are unperturbed from the gas-phase structure of dichloromethane: bound C-Clav= 1.76 (2) A, Cl-C-Clav= 110.4 (6); free C-Cl= 1.7724 (5) Á, Cl-C-Cl= 111.78 (2). 17 The ligand containing Cl is bound more strongly to the Ag (I) ion (Ag-Clav= 2.793 (3) Á) than the ligand con-(8)(a) Cook, P. M.; Dahl, L. F.; Dickerhoof, DW J. Am. Chem. Soc. 1972, 94, 5511.(b) Cook, P. M. Thesis, University of Wisconsin, Madison, 1972.