Michael W. Bishop
University of Sussex
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Journal of Organometallic Chemistry | 1981
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Bryan D. Neaves; Phillip L. Dahlstrom; Jeffery Hyde; Jon Zubieta
Abstract The nitrido complexes [MoN(S 2 CNR 2 ) 3 ] (R 2 Me 2 , Et 2 ) and [ReN)S 2 CNR 2)2 -(PMe 2 Ph) n ] (R 2 Me 2 ; Et 2 ; n 0, 1) react with halides R′X (R′ PhCO, PhSO 2 , 2,4-(NO 2)2 C 6 H 3 , 2,4-(NO 2)2 C 6 H 3 S; X Cl, R′ Me, X I), [R′3 O ]BF 4 (R′ Me, Et) or [Ph 3 C]BF 4 to give the imido complexes [Mo(NR′)(S 2 CNR 2 ) 3 ]+ and [Re(NR′)(S 2 CNR 2 ) 2 (PME 2 Ph) n ] (R′ Me, Et, Ph 3 C + , PhSO 2 , PhCO, 2,4(O 2 N) 2 -C 6 H 3 , 2,4-(O 2 N) 2 C 6 H 3 S); the X-ray crystal structures of [Mo(NCPh 3 )(S 2 -CNMe 2 )3]BF 4 and [Mo(NSO 2 Ph)(S 2 CNMe 2 )3]PF 6 have been determined. Both complexes have approximately pentagonal bipyramidal geometries although the NSO 2 Ph complex is more distorted. The NCPh 3 and NSO 2 Ph complexes have MoNC and MoNS angles of 175.1(5) ° and 161.3(13)° and MoN distances of 1.731(2) and 1.70(2)A, respectively.
Journal of The Less Common Metals | 1977
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; M.B Hursthouse; M Motevalle
Abstract Molybdenum(IV), (V) and (VI) nitrido complexes are prepared using trimethylsilylazide; the complexes [MoN(S 2 CNR 2 ) 3 ] ( R 2 = Me 2 , Et 2 , ( CH 2 ) 5 ) are precursors for the preparation of thionitrosyl and imido complexes and a trimeric species with two bridging nitride ligands. The X-ray crystal structures of [MoN(S 2 CNEt 2 ) 3 ], [MoN(S 2 CNMe 2 ) 3 ] and the trimeric complex [{MoN(S 2 CNEt 2 ) 3 } 2 Mo(S 2 CNEt 2 ) 3 ] [PF 6 ] 3 are reported. The preparation of mono- and bis-hydrazido(2-) complexes from molybdenum(IV) bis-oxo complexes and N,N-disubstituted hydrazines is also reported and their structures are compared with other analogous complexes.
Journal of The Chemical Society-dalton Transactions | 1979
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Michael B. Hursthouse; Majid Motevalli
The oxo-complexes [MoO2L2][L = oxinate, S2CNMe2, S2CNEt2, S2CN(CH2)5, or S2CNPh2] react with the hydrazines R2NNH2[R2= Me2, (CH2)5, or Ph2] to give the hydrazido(2–)-complexes [Mo(NNR2)OL2]. The crystal and molecular structure of [Mo(NNMe2)O(S2CNMe2)2] has been determined by single-crystal X-ray diffraction methods. The complex crystallises in the monoclinic system, space group P21/c with a= 7.897, b= 13.854, c= 15.517 A, β= 103.1°, and Z= 4. The molecule has a distorted octahedral configuration with the hydrazido-ligand bonded linearly in a position cis to the oxo-group. The Mo–N and N–N distances of 1.799 and 1.288 A are consistent with a mode of bonding closer to the representation [graphic omitted][graphic omitted]N[graphic omitted]R2 than Mo[graphic omitted]N–NR2.
Journal of The Chemical Society-dalton Transactions | 1979
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Michael B. Hursthouse; S. Amarasiri A. Jayaweera; Andrew Quick
The molybdenum(IV) oxo-complexes [MoOCl2(PR″3)3](PR″3= PMe2Ph or PEt2Ph) react with the substituted hydrazines RCONHNHR′(R = Ph, p-ClC6H4, p-MeC6H4, p-MeOC6H4, Et, Prn, Pri, or CH2Ph; R′= Ph, p-ClC6H4,p-MeOC6H4, 1-C10H7, or Me) to give the imido-complexes [MoCl2(NR′)(R′N2COR)(PR″3)]. The crystal and molecular structure of the title complex has been determined from single-crystal X-ray diffractometer data. The crystals are monoclinic with a= 8.995, b= 19.090, c= 17.860 A, β= 104.15°, space group P21/c, and Z= 4. The structure has been solved by Patterson and Fourier methods, and least-squares refinement using 2 279 independent observed reflections has reached R= 0.066. The co-ordination geometry is distorted octahedral. The metal–diazene chelate system is quite planar and bond lengths indicate considerable delocalisation within the chelate ring. In particular, the Mo–N length [1.984(8)A] is shorter than the Mo–O length [2.110(7)A] and this is taken to indicate partial double-bond character in the Mo–N bond. The remaining metal–ligand distances are Mo–N(imido) 1.726(9), Mo–Cl 2.393(4)(trans to P) and 2.406(3)(trans to N in chelate ring), and Mo–P 2.528(4)A.
Journal of The Chemical Society, Chemical Communications | 1976
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Michael B. Hursthouse; Majid Motevalli
The reaction of [MoN(S2CNEt2)3] with hydroxylamine-O-sulphonic acid and NaBF4 in methanol gives the title compound, the structure of which has been determined by X-ray diffraction.
Journal of The Chemical Society-dalton Transactions | 1979
Michael W. Bishop; Graham Butler; Joseph Chatt; Jonathan R. Dilworth; G. Jeffery Leigh
We describe a series of complexes [Mo(N2Q)(S2CNMe2)3](Q = alkyl, aryl, or alkoxycarbonyl) and [Mo(N2Q)2(S2CNMe2)2] prepared from [MoO2(S2CNMe2)2] and the appropriate hydrazine. Representative members of the former class of compounds can be protonated, alkylated, and arylated at the diazenido-nitrogen remote from the metal. The latter compounds are formed via intermediates which are probably [Mo(N2H2Q)(N2Q)(S2CNMe2)2]. The electrochemical properties of the new complexes are discussed.
Journal of The Chemical Society, Chemical Communications | 1977
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Gerald Kaufman; Stephen. Kim; Jon Zubieta
The product of the reaction between [MoO2(S2CNEt2)2] and benzoylhydrazine hydrochloride is shown by X-ray crystallography to be an asymmetric dinuclear complex [Mo2O(PhCON2)2(S2CNEt2)2], with bridging benzoyldiazenido-ligands.
Journal of The Chemical Society-dalton Transactions | 1979
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth
The molybdenum nitrido-complexes [MoN(S2CNR2)3] react with elemental sulphur or propylene sulphide to give the thionitrosyl complexes [Mo(NS)(S2CNR2)3] in high yield. The rhenium nitrido-complexes [ReX2N(PR3)3](PR3= PMe2Ph, PEt2Ph, or PMePh2; X = Cl or Br) react with half an equivalent of S2Cl2 to give the pink thionitrosyl complexes [ReCl(X)(NS)(PR3)3] in yields of 60–70%. Use of an excess of S2Cl2 gives the purple complexes [ReCl2X(NS)(PR3)2] in good yields. The five-co-ordinate nitrido-complexes [ReCl2N(PRPh2)2](R = Ph or Prn) also give [ReCl3(NS)(PRPh2)2] on reaction with half an equivalent of S2Cl2. The osmium nitrido-complexes [OsX3NL2][L = AsPh3, PMe2Ph, ½ bipy (2,2′-bipyridyl), or py (pyridine); X = Cl or Br] react analogously with S2Cl2 to give [OsClX2(NS)L2]. ν(N–S) appears in the i.r. spectra in the range 1 120–1 280 cm–1, and the 1H n.m.r. spectra of the diamagnetic complexes show the phosphines to be mer in [ReCl2(NS)(PR3)3] and trans in [OsCl3(NS)(PMe2Ph)2]. Treatment of the thionitrosyls with tertiary phosphines regenerates the parent nitrido-complexes in high yields.
Journal of The Chemical Society-dalton Transactions | 1979
Michael W. Bishop; Joseph Chatt; Jonathan R. Dilworth; Michael B. Hursthouse; Majid Motevalli
The complexes [MoCl(O)(P–P)2][MoCl3O(RCON2Ph)](R = Ph, p-ClC6H4,p-MeOC6H4, or Me; P–P = Ph2PCH2CH2PPh2 or Ph2PCHCHPPh2) have been prepared by reactions of the hydrazines RCONHNHPh with [{MoCl2O(P–P)}2] or [MoCl3O(P-P)] in refluxing methanol. The crystal and molecular structure of [MoCl(O)(Ph2PCH2CH2PPh2)2][MoCl3O(p-ClC6H4CON2Ph)] has been determined by single-crystal X-ray diffraction methods. The complex crystallises in the triclinic system, space group P with a= 14.87(1), b= 11.84(1), c= 18.37(1)A, α= 96.1(1), β= 98.8(1), γ= 97.2(1)°, and Z= 2. The geometry of the oxo(diazene) anion is distorted octahedral with the chloride atoms in a mer configuration and the oxygen atom of the diazene ligand is trans to the oxo-function. The Mo–Cl distances are 2.410(6), 2.412(6), and 2.334(7)A. The MoO terminal distance is 1.620(14)A and the bond lengths within the diazene ligand indicate considerable delocalisation.
Journal of The Chemical Society-dalton Transactions | 1978
Edward O. Bishop; Graham Butler; Joseph Chatt; Jonathan R. Dilworth; G. Jeffery Leigh; David Orchard; Michael W. Bishop
The rate of N-methyl exchange in a series of aryldiazenidomolybdenum complexes has been studied by 1H n.m.r. spectroscopy as a function of temperature and of substitution in the aromatic ring. The results indicate a fluxional rearrangement characterised by a single first-order rate constant. The aromatic-substituent effect shows a better Hammett correlation with σ than with σ+ values. The ρ factor is –0.64. Implications for the geometry of the system are discussed.