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  • 1
    ISSN: 1434-1948
    Keywords: Platinum ; Nickel ; Stannyl complexes ; Oxidative addition ; Tin ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of Ni(COD)2 (COD = 1,5-cyclooctadiene) with two equivalents of Ph2PCH2CH2SnPh3 or of (Ph3P)2Pt(C2H4) with two equivalents of Ph2PCH2CH2SnR3 (R = Ph, Me, Bu) results in the immediate formation of the complexes (R3SnCH2CH2Ph2P)M[PPh2CH2CH2SnPh2(M-Sn)](R) (M = Ni, Pt) with a cis arrangement of the two phosphorus atoms. The structure of (Me3SnCH2CH2Ph2P)Pt[PPh2CH2-CH2SnMe2(Pt-Sn)](Me) was confirmed by an X-ray structure analysis. In the presence of PPh3, this complex shows dynamic behavior in solution due to Ph2PCH2CH2SnMe3/PPh3 exchange. When the phosphanylalkylstannanes Ph2PCH2CH2SnPh3-xMex (x = 1, 2) are employed in the reaction with Ni(COD)2 or (Ph3P)2Pt(C2H4), the Sn-Ph groups are more prone to oxidative addition than the Sn-Me groups. When Ni(COD)2 is treated with one equivalent of Ph2PCH2CH2SnPh3 and PR′3 (PCy3 or PMe2Ph) each, the complexes (R′3P)M(PPh2CH2CH2SnPh2)(Ph)(M-Sn) are formed. Heating of (Ph3SnCH2CH2Ph2P)Ni[PPh2-CH2CH2SnPh2(Ni-Sn)](Ph) to 70 °C induces the oxidative addition of a Sn-Ph group of the dangling ligand, and cis-Ni[PPh2CH2CH2SnPh2(Ni-Sn)]2 is obtained. The same complex is formed upon reaction of Ni(COD)2 with Ph2PCH2CH2SnPh2H. Reaction of Ni(COD)2 with Ph2PCH2CH2SnMe3 results in the immediate formation of trans-Ni[(PPh2CH2CH2SnMe2(Ni-Sn)]2.
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  • 2
    ISSN: 0009-2940
    Keywords: Stannyl complexes ; Oxidative addition of Sn - C bonds ; Phosphinoalkylstannanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Stannyl Complexes, 4.  -  Palladium and Platinum Complexes with Chelatting Phosphinoalkylstannyl Ligands by Oxidative Addition of Sn - C BondsReaction of (Ph3P)4Pd with two equivalents of Ph2PCH2CH2-SnR3 (R = Ph, Me) gives the Pd(II) stannyl complexes trans-Pd(PPh2CH2CH2SnR2)2 (2) by oxidative addition of two Sn - R groups and elimination of R - R. Products corresponding to earlier steps of the reaction are obtained by the reaction of (Ph3P)2Pt(C2H4) with Ph2P(CH2)nSnR3 (n = 2, 3). The phenylderivatives Ph2P[CH2]nSnPh3 afford the Pt(II) complexes (Ph3P)(Ph)PtPPh2[CH2]nSnPh2 (3), in which the two phosphorus atoms are cis-configurated, while Ph2PCH2CH2SnMe3 gives the Pt(IV) complex cis,cis,cis-(Me)2Pt(PPh2CH2CH2SnMe2)2 (3) as stable product.
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  • 3
    ISSN: 0009-2940
    Keywords: Metal hydrides ; Iron complexes ; Silyl complexes ; Stannyl complexes ; Three-center bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The complexes FeH3(PPh2R')3ER3 (R' = nBu: ER3 = SnPh3, SiMePh2; R' = Et: ER3 = SnPh3) were prepared by reaction of Fe(H)2(H2)(PPh2R')3 with HSnPn3 or HSiMePh2. The heavy-atom skeleton of FeH3(PPh2Et)3SnPh3 shows an approximate C3 symmetry in the crystalline state and a nearly tetrahedral FeP3Sn core. However, the NMR spectra indicate the presence of Fe,H,Si(Sn) three-center two-electron bonds at low temperature in solution.
    Additional Material: 1 Ill.
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  • 4
    ISSN: 0009-2940
    Keywords: Anionic complexes ; Chromium complexes ; Manganese complexes ; Stannyl complexes ; Hydrido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Stannyl Complexes, 9[1]. - Substitution Reactions of the Anionic Hydrido Complexes [(π-MeC5H4)-(CO)2MnH]- and [(π-Arene)(CO)2CrH]-The anionic hydrido complexes K[(π-MeC5H4)(CO)2MnH] (2c) and K[(π-arene)(CO)2CrH] (π-arene = C6H6, C6H5Me, 1,2,3-C6H3Me3, C6Me6, C6H5Ph, indan) (5a-f) are spontaneously formed on stirring THF solutions of the dianionic complexes K2 [(π-MeC5H4)(CO)2Mn] (1) or K2[(π-arene)(CO)2Cr] (4) at - 78°C. The dianionic complexes are obtained by potassium naphthalenide reduction of (π-MeC5H4)(CO)2MnL or (π-arene)(CO)2CrL (L = pyridine or THF). Reaction of 2c with Me3SnCl or Ph2SnCl2 yields the bis(stannyl) complexes Cp*(CO)2Mn(SnR3)2 (SnR3 = SnMe3, SnPh2Cl), while reactions with the „smaller“ stannanes Me2SnCl2 or Et2SnCl2 results in the SnR2-bridged complexes [Cp′(CO)2Mn]2(μ-SnR2)((Mn-Mn). The bis(stannyl) complexes (π-arene)(CO)2Cr(SnR2Cl)2 (R = Me, Ph) are obtained from 5 and R2SnCl2. However, the reaction is strongly influenced by steric effects: with Me2SnCl2, bis(stannyl) complexes are obtained for π-arene = C6H6, C6H5Me, 1,2,3-C6H3Me3, or C6Me6, with Ph2SnCl2 only for π-arene = C6H6 and C6H5Me. Reaction of the sterically demanding complexes K[(π-C6H5Ph)(CO)2CrH] or K[(π-indan)(CO)2CrH] with Ph2SnCl2 stops at the stage of the anionic stannyl complexes K[(π-arene)(CO)2Cr-SnPh2Cl].
    Additional Material: 1 Ill.
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  • 5
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Stannyl complexes ; Chromium complexes ; Anionic complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition Metal Stannyl Complexes, 7[1]. - Preparation of Carbene Complexes (π1-Arene)(CO)2CrCR2 by the Reaction of the Anionic Stannyl Complexes [(π1-Arene)(CO)2CrSnPh3]- with R2CX2 or [R2CX]YCarbene complexes (π1-arene)(CO)2Cr=CR2 are formed in substitution/elimination reactions from the anionic stannyl complexes K[(π1-arene)(CO)2CrSnPh3] [π1-arene=C6H6 (1a), 1,3,5-Me3C6H3 (1b), 1,2,4,5-Me4C6H2 (1c)] C6Me6 (1d) and organic dihalides R2CX2 containing activated C - X bonds or ionic halides [R2CX]Y. Bis(stannyl) complexes (π1-arene)(CO)2Cr(SnPh3)2 (3) and hydrido(stannyl)complexes (π1-arene)(CO)2Cr(H)SnPh3 are formed as byproducts due to the reaction of the eliminated Ph3SnCl with the anionic starting complexes or electron transfer reactions, respectively. The portion and ratio of the byproducts is largely influenced by the steric properties of both the (π1-arene)(CO)2Cr fragment and the organic halide. Pyridinylidene complexes 2) are only obtained from 2-chloro-N1-methylpyridinium tetrafluoroborat with 1a - c, but not with 1d. With the sterically less demanding halides [R2N=C(H)Cl]Cl [NR2=NMe2, (n=3, 4)] or 3,3-dichloro-1,2-diphenylcyclopropene the carbene complexes (π1-arene)(CO)2Cr=C(H)NR2 or are obtained with all employed π1-arene ligands.
    Additional Material: 2 Ill.
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  • 6
    ISSN: 0009-2940
    Keywords: Stannyl complexes ; Hydride complexes ; Three-center bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition-Metal Stannyl Complexes, 3. - Metal, Hydrogen, Tin Three-Center Bonding in Group VI Hydrido Stannyl ComplexesThe hydrido stannyl complex (π-1,3,5-Me3C6H3)(CO)2Cr(H)-SnPh3 (1) is prepared by photochemical reaction of (π-1,3,5-Me3C6H3)(CO)3Cr with HSnPh3. The 119SnHCr coupling constant (327.6 Hz) and an X-ray structure analysis [Sn - H 202(4), Cr - H 159(4), Cr - Sn 270.16(6) pm] show that the Sn - H bond is coordinated in an η2 fashion. The complexes (CO)4(R3P)-W(H)SnPh3 (R3P=Ph3P, MePh2P) (2) and (CO)3(dppe)M(H)-SnR3 (M=Cr, SnR3=SnPh3; M=Mo, SnR3=SnMe3, SnPh3; M=W, SnR3=SnMe3, SnPh2Me, SnPh3) (4 - 6) are obtained either by thermal reaction of (CO)4(R3P)W(THF) or (CO)3(dppe)ML (L=THF, acetone) with HSiR3, or by photochemical reaction of (CO)4(dppe)M with HSnPh3. Reaction of (CO)4(Ph3P)W(THF) with HSnMe3 yields (CO)4(Ph3P)W(Sn-Me3)2 (3). The Sn,M,H coupling constants in the complexes 2 and (CO)3(dppe)M(H)SnR3 (M=Cr, Mo) are in the range of 250 - 315 Hz and therefore these complexes seem to contain an η2-coordinated stannane. Contrary to this, the SnWH coupling constants in (CO)3(dppe)W(H)SnR3 are considerably lower (70 - 90 Hz), suggesting complete oxidative addition of the H - Sn bond. The complexes (CO)3(dppe)M(H)SnPh3 decompose in benzene solution at room temperature to give, inter alia, hexaphenyldistannane. Ph6Sn2 · 2 C6H6 crystallizes in the space group \documentclass{article}\pagestyle{empty}\begin{document}$ R\bar 3 $\end{document} (Z=1); in the crystal lattice the benzene molecules are perpendicular to the three-fold axis of symmetry of the distannane molecule.
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  • 7
    ISSN: 0009-2940
    Keywords: Stannyl complexes ; Plumbyl complexes ; Tungsten complexes ; Molybdenum complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition-Metal Stannyl Complexes, 10 - Molybdocen and Wolframocen Derivatives with Two Different Main-Group-4 LigandsReactions of Li[Cp2MSnPh3] (M = Mo, W) with CH3I, BuBr, PhCH2Br, PhC(O)Cl or Br(CH2)nBr (n = 4,5) yield Cp2M(R)SnPh3 [R = CH3, Bu, CH2Ph, C(O)Ph, (CH2)nBr], while tBuBr or CH3C(O)Cl give the hydrido complexes Cp2M(H)SnPh3. A silyl stannyl complex is only obtained from Li[Cp2WSnPh3] and Me3SiOSO2CF3, but not with Me3SiCl or from the anionic Mo complex. In contrast, the reactions of chlorostannanes provide the bis(stannyl) complexes Cp2M(SnR′3)SnPh3 or Cp2M(SnR′2Cl)SnPh3. R/Cl exchange at the tin atom is observed when an excess of the chlorostannane is used. Upon reaction of Li[Cp2MSnPh3] with Ph3PbCl only Cp2M(PbPh3)SnPh3 is formed, while a mixture of Cp2M(PbMe3)SnPh3 and Cp2M(PbMe2Cl)SnPh3 is obtained with Me3PbCl due to redistribution reactions. The structures of Cp2W(SnPh3)C(O)Ph, Cp2W(SnPh3)SntBu2Cl and Cp2W(SnPh3)PbMe2Cl were determined by X-ray structure analyses.
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