One-pot synthesis of fac-[Mn(CO)3(PP)Cl] from Mn2(CO)10, [PP] and chlorinated solvents: [PP] = 1,2-bis(diethylphosphino)ethane (depe), 1,2-bis(diphenylphosphino)ethane (dppe) or 1,3-bis(diphenylphosphino)propane (dppp). The X-ray crystal structure of fac-[Mn(CO)3(depe)Cl]
作者:Guang Qing Li、Julian Feldman、Jeanette A. Krause、Milton Orchin
DOI:10.1016/s0277-5387(96)00523-2
日期:1997.4
Abstract In a one-pot reaction, the three titled manganese chloride complexes were prepared by refluxing Mn2(CO)10 with (PP) in 2-chloroethanol for two hours. The new compounds were characterized by IR, 1H NMR, mass spectra and microanalyses. The X-ray crystal structure of fac-Mn(CO)3(depe)Cl is also reported.
The preparation and reactions of the azides of fac-Mn(CO)3(P-P)N3. The X-ray crystal structures of fac-[Mn(CO)3(P-P)(OH2)]BF4, fac-Mn(CO)3(P-P)() [(P-P)=dppe and depe], and fac-[Mn(CO)3(depe)(PPh3)]BF4
作者:Thomas M. Becker、Jeanette A. Krause-Bauer、Craig L. Homrighausen、Milton Orchin
DOI:10.1016/s0277-5387(99)00161-8
日期:1999.8
A simple three-step, high-yield synthesis of the titled azides from Mn-2(CO)(10) and P-P is described involving the intermediate aqua complexes, fac-[Mn(CO)(3)(P-P)(H2O)]BF4, 3a,b. The aqua ligand is very labile; it is easily exchanged for D2O, PPh3, and NO2-. Crystal structures of the two titled aqua complexes and fac-[Mn(CO)(3)(depe)(PPh3)]BF4, 6a, are reported. The aqua complexes react instantaneously with aqueous NaN3 to give quantitative yields of the corresponding covalent azides which undergo the expected 1,3-dipolar additions with CF3CN to give the corresponding tetrazoles whose crystal structures are also reported. (C) 1999 Elsevier Science Ltd. All rights reserved.
Conversion of a manganese-carbon-bonded complex to a manganese-oxygen-bonded complex, some reactions of manganese carbonato complexes
作者:Guang Qing Li、Robert M. Burns、Santosh K. Mandal、Jeanette Krause Bauer、Milton Orchin
DOI:10.1016/s0022-328x(97)00486-5
日期:1997.12
Stirring a solution of the manganese carboxylate, (dppe)(CO)(3)Mn-C(O)OCH3, 1, in dichloromethane saturated with water converts it to the bridging carbonato complex, (dppe)(CO)(3)Mn-OC(O)O-Mn(CO)(3)(dppe), 2. This multi-step con vers ion involves the in-situ transformation of a Mn-C bonded complex to a Mn-O bonded one. When 2 is stirred with HCl, it is converted quantitatively to the covalent chloride (dppe)(CO)(3)Mn-Cl, 11, with evolution of carbon dioxide. Similar HCl treatment of the manganese carboxylate 1 gives three compounds: the same covalent chloride, 11; the ionic chloride, [(dppe)(CO)(4)Mn]Cl-+(-), 12, and the hydride, (dppe)(CO)(3)Mn-H, 5. Reasonable schemes for these conversions are suggested. Heating the ionic chloride complex to its melting point converts it to the covalent chloride complex; the same transformation is accomplished by refluxing the ionic chloride in acetonitrile. (C) 1997 Elsevier Science S.A.