Chalkogen-Derivate der Halbsandwich-Wolfram(V)-Komplexe CpWCl4 und CpWCl4(PMe3). Röntgen-Kristallstrukturanalysen vonanti-[CpW(Se)(μ-Se)]2 und CpW(S)2(OMe) (original) (raw)
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Journal of Organometallic Chemistry, 1993
Starting from the halfsandwich compound Cp*Re(O)Cl 2, the chalcogen-bridged binuclear complexes CP*2Re2(/x-E4)2 (E = S, Se), CP*2Re202(/z-E)(/x-E2) (E = S, Se) and CP*2Re202(/I,-E)2 (E = Se, Te) have been prepared by reaction with oligochalcogenides and subsequent chalcogen abstraction using tertiary phosphanes, PR 3. The molecular structures in the crystalline state of three selenium compounds have been determined by X-ray structure analyses" in contrast to the oxo complexes, the oxygen-free ' o . . compounds CP*ERe2(/.t-E4) 2 are disting.uished by a strong intramolecular Re-Re interaction (d(Re=Re) 2.692(1) A m Cp 2Re2(/.t-Se4)2, d(Re "-Re) 4.32 A and 3.77 A in CP*EReEO2(/,i,-Se) (~-Se 2) and CP*2ReEO2(P,-Se)2, respectively). The reactions of Cp*Re(O)Cl 2 with either NaES 4 or (NEt4)2Se 6 lead initially to the mononuclear cyclo-tetrachalcogenide compounds Cp*Re(O)(E 4) (E = S, Se), which can then be converted into the binuclear complexes. However, Cp*2ReEOE(/X-Te)2 was directly formed in the reaction between Cp*Re(O)Cl 2 and (NnBu4)2Tes.
Zeitschrift für Naturforschung B, 1994
Mn(SPh)Cl3]2-, [Mn(SPh)3CI]2-, [Mn2(SPh)6]2-und [Mn4(SPh)6Br4]2": Synthese, Struktur und ausgewählte Eigenschaften einiger neuer Chalkogenolatkomplexe des zweiwertigen Mangans [M n(SPh)C l3]2-, [M n(SPh)3Cl]2~, [M n2(SPh)6]2-and [M n4(SPh)6B r4]2': Synthesis, S tructure and Selected Properties of Som e New C halkogenolate C om plexes of D ivalent M anganese H ans-O scar S tep h an 3, Klaus G riesarb, W olfgang H aa seb, G erald H e n k e l3 *
Zeitschrift für Naturforschung B, 1991
Pentalithium Octa(ter/-butoxy)samarat(III), Synthesis, X-Ray [Li(tmed)]3[Sm (CH3)6] reacts with te/7-butanol in diethyl ether to give [Li5S m (0-r-C 4 H 9)8] (1), the structure o f which has been elucidated by X-ray structure analysis. 1 crystallizes tetragonally with a = 1703(4) and c-3178(1) pm, space group P 4,2,2, Z = 8. The structure was refined to R = 0.042 for 4082 observed reflections (F0 > 6 er(F0)).
Zeitschrift für Naturforschung B, 2005
Reactions of L-tert-Leucine (tert-butylglycine), tert-leucine methyl ester, GlyValOMe, and Leu- AlaOMe with the chloro-bridged complexes [Cp*IrCl2]2, [(p-cymene)RuCl2]2 or [(C6Me6)RuCl2]2 in the presence of NaOMe give the complexes [Cp*Ir(Cl)NH2CH(R)CO2] (1), [(p-cymene)Ru(Cl)- NH2CH(R)CO2] (2), Cp*Ir(Cl2)[NH2CH(R)CO2Me] (5), {(C6Me6)Ru(Cl)[NH2CH2CONHCH(R)- CO2Me]}+Cl− (6), [Cp*Ir(Cl)NH2CH2CONCH(R)CO2Me] (7), [Cp*Ir(Cl)NH2CH(CH2CHMe2)- CONCH(R)CO2Me)] (8), and Cp*Ir(Cl2)[NH2CH2CONHCH(R)CO2Me) (9). With pentaglycine the complexes [Cp*Ir(Cl2)(pentaglycinate+Na+)] (10) and [(C6Me6)Ru(pentaglycineOMe- H+)] (11) could be isolated. Coordination of one equivalent of the S-protected tripeptide glutathione to [Cp*Ir(Cl)] and to [(C6Me6)Ru(Cl)] was observed. Some in situ prepared (p-cymene)Ru complexes with deprotonated dipeptide esters were tested as catalysts and the complex [(p-cymene)Ru(Cl)(NH2CH(CHMeEt)NCH (CHMe2)CO2tert-Bu)] gave a yield of 73% and moderate entantiomeric excess (36% ee)...
Zeitschrift für anorganische und allgemeine Chemie, 2008
Single crystals of the mixed ligand complexes [Be(OSMe 2) 3 (H 2 O)]Cl 2 (2) and [Be(OSMe 2) 2 (H 2 O) 2 ]Cl 2 (3) were obtained from saturated solutions of [Be(OSMe 2) 4 ]Cl 2 (1) in acetonitrile and dichloromethane, respectively, in the presence of traces of water, while single crystals of 1 were available by reaction of the carbodiphosphorane complex [BeCl 2 {C(PPh 3) 2 }] with DMSO/toluene solution. All complexes are characterized by X-ray diffraction and IR spectroscopy. 1: Space group Pbca, Z ϭ 8, lattice dimensions at 193 K: a ϭ 962.4(1), b ϭ 1888.8(2), c ϭ 2115.8(2) pm, R 1 ϭ 0.0344. 1 consists of [Be(OSMe 2) 4 ] 2ϩ cations with distorted tetrahedral coordination of the oxygen atoms of the DMSO molecules with BeϪO distances of 161.9 pm on average, and chloride ions.
Zeitschrift für Naturforschung. B, A journal of chemical sciences, 2005
AlaOMe with the chloro-bridged complexes [Cp * IrCl 2 ] 2 , [(p-cymene)RuCl 2 ] 2 or [(C 6 Me 6)RuCl 2 ] 2 in the presence of NaOMe give the complexes [Cp * Ir(Cl)NH 2 CH(R)CO 2 ] (1), [(p-cymene)Ru(Cl)-NH 2 CH(R)CO 2 ] (2), Cp * Ir(Cl 2)[NH 2 CH(R)CO 2 Me] (5), {(C 6 Me 6)Ru(Cl)[NH 2 CH 2 CONHCH(R)-CO 2 Me]} + Cl − (6), [Cp * Ir(Cl)NH 2 CH 2 CONCH(R)CO 2 Me] (7), [Cp * Ir(Cl)NH 2 CH(CH 2 CHMe 2)-CONCH(R)CO 2 Me)] (8), and Cp * Ir(Cl 2)[NH 2 CH 2 CONHCH(R)CO 2 Me) (9). With pentaglycine the complexes [Cp * Ir(Cl 2)(pentaglycinate + Na +)] (10) and [(C 6 Me 6)Ru(penta-glycineOMe-H +)] (11) could be isolated. Coordination of one equivalent of the S-protected tripeptide glutathione to [Cp * Ir(Cl)] and to [(C 6 Me 6)Ru(Cl)] was observed. Some in situ prepared (p-cymene)Ru complexes with deprotonated dipeptide esters were tested as catalysts and the complex [(p-cymene)Ru(Cl)(NH 2 CH(CHMeEt)NCH (CHMe 2)CO 2 tert-Bu)] gave a yield of 73% and moderate entantiomeric excess (36% ee) in the transfer hydrogenation of acetophenone to 2-propanol.