The crystal structure of π-cyclopentadienyltricarbonyl-σ-phenyltungsten

Semion, V. A.; Chapovskii, Yu. A.; Struchkov, Yu. T.; Nesmeyanov, A. N.

doi:10.1039/c19680000666

Cited by 7 publications

(3 citation statements)

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“…There is a plane of symmetry passing through C(1)−W−C(11). The molecule is a conventional piano stool structure, the structural features of the W(CO) 3 Cp group being unexceptional and closely similar to those found in WPh(CO) 3 Cp and {W(CO) 3 Cp} 2 (μ-C 2 ), for example. The important feature is the coordination of the diynyl ligand.…”

Section: Resultsmentioning

confidence: 58%

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)

Bruce

Low

et al. 1998

Organometallics

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Reactions of buta-1,3-diyne with appropriate metal halides, carried out in the presence of CuI in NHEt2, have given high yields of M(C⋮CC⋮CH)(CO) n Cp [M = W (1-W), Mo (1-Mo), n = 3; M = Fe, n = 2 (2)]. Complex 1-W was metalated with LiNPri 2; subsequent reactions with SiClMe3 or PClPh2 gave W(C⋮CC⋮CR)(CO)3Cp [R = SiMe3 (3) or P(O)Ph2 (4)] in modest to high yield. Coupling of 1 with iodoarenes, catalyzed by a mixed CuI−Pd0 catalyst, gave M(C⋮CC⋮CAr) (CO)3Cp [M = W, Ar = Ph (5-W), tol (6), C6H4OMe-4 (7), C6H4CO2Me-4 (8); M = Mo, Ar = Ph (5-Mo)]. Oxidative coupling of 1 (CuCl-tmed-O2) gave {M(CO)3Cp}2(μ-C8) [M = W (9-W), Mo (9-Mo)]. Addition of tetracyanoethene to 1-W occurred at the C⋮C triple bond further from the metal atom, to give W{C⋮CC[=C(CN)2]CHC(CN)2}(CO)3Cp (10). Substitution of CO by PPh3 was difficult, but the Me3NO-induced reaction with 5-W afforded cis-W(C⋮CC⋮CPh)(CO)2(PPh3)Cp (11) in low yield. The X-ray crystal structures of 3 and 10, together with that of cis-W(C⋮CPh)(CO)2(PPh3)Cp (12), are reported.

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Section: Resultsmentioning

confidence: 58%

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)

Bruce

Low

et al. 1998

Organometallics

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“…Encouraged by these results but acknowledging that the covalent radius of tungsten is particularly ill-defined, we can similarly derive a value of 1.59 Å for the covalent radius of W(0) in an octahedral environment on the basis of the average W−N distance (2.29 Å) found in (Tps Me 2 )W(CO) 3 . It is interesting to note that values of 1.57 and 1.58 Å have been estimated before for r cov (W) based on the X-ray structure analysis of CpW(CO) 3 Ph …”

Section: Resultsmentioning

confidence: 92%

Syntheses and Structures of Methyltris(pyrazolyl)silane Complexes of the Group 6 Metals

Pullen¹,

Rabinovich²,

Incarvito³

et al. 2000

Inorg. Chem.

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The methyltris(3,5-dimethylpyrazolyl)silane ligand, TpsMe2, was readily prepared by the metathesis reaction of methyltrichlorosilane with 3 equiv of lithium 3,5-dimethylpyrazolate. The octahedral tricarbonyl complexes (TpsMe2)M(CO)3 were synthesized either by ligand exchange with the labile nitrile adducts M(CO)3(NCR)3 (M = Cr, Mo, R = Me; M = W, R = Et) or thermally by direct substitution on the hexacarbonyls M(CO)6 (M = Cr, Mo). The three new complexes were characterized by a combination of analytical and spectroscopic techniques, including electrospray ionization mass spectrometry and single-crystal X-ray diffraction. They are all isostructural and display in the solid state the expected distorted octahedral geometries with facially coordinated tris(pyrazolyl)silane ligands. Crystallographic data were used to calculate the ligand cone angles (251-264 degrees) in (TpsMe2)M(CO)3 and also to estimate a value of 1.59 A for the covalent radius of octahedral W(0).

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“…The structure of t r icar bony1 x-cyclopentadienyl-o-phenyltungsten(I1) has been determined by X-ray crystallography ; the W-C(pheny1) bond-length is 2-32 A. 283 The structure of trans-acetyldicarbonyl-x-cyclopentadienyltriphenylphosphinemolybdenum(rr) has been determined by X-ray crystallography; the Mo-C(acety1) bond-length is 2.26 A.284 o-Phenacyl complexes c f molybdenum and iron are formed by the reactions of [Mo(x-C~H~)(CO)~]and [Fe(n-CsHs)(CO)z]-with phenacyl chloride. 285 The reactions of NaM(C0)5, (M = Mn or Re) with substituted phenacyl chlorides286 and isopht haloy 1 c hlor ide287 yield o-ar omat ic derivatives of M (CO)5.…”

Section: J a Mcginnety And M J Maysmentioning

confidence: 99%

Chapter 13. Transition-metal carbonyls and organometallic complexes

McGinnety¹,

Mays²

1968

Annu. Rep. Prog. Chem., Sect. A. Gen. Phys and Inorg. Chem.

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THE pattern of this year's review has not been changed from that adopted last year. The task of the reviewers in selecting reference becomes, however more difficult from year to year as the volume of published work increases. We hope we have included most of the more striking advances but there is certainly much interesting work which we have had to omit through lack of space. The most notable increase in effort has been in the field of platinum metal chemistry, and this has undoubtedly been stimulated by the ability of many of these complexes to act as homogenous catalysts in organic reactions. Although, as predicted last year, several new complexes of molecular nitrogen have been prepared, the problem of the catalytic fixation of nitrogen under mild conditions remains unsolved.Among the topics which have been reviewed are: metal carbony1s;l kinetics and mechanism of substitution reactions of metal carbonyls;2 the activation of molecular iiitrogen;3 the chemistry of the rarer platinum metal^;^ metal-metal bonds in transition-metal compounds ;5 organometallic derivatives from metal carbonyls and acetylene compounds;6 catalysis by cobalt carbonyl~;~ and mass spectra of organometallic compounds.* Volume 4 of the 'Annual Surveys of Organoinetallic Chemistry' has appeared,g also a useful comprehensive text book.lO Carbonyls and Hydridocarbony1s.-(a) Mononuclear. The electronic spectra of several neutral and ionic metal hexacarbonyls in the vapour and solution states have been recorded at room temperature. Some of the solution spectra have also been recorded at 7 7 " ~. Calculated molecular orbitals have been used for the purpose of transition assignments and also for a discussion of

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The crystal structure of π-cyclopentadienyltricarbonyl-σ-phenyltungsten

Cited by 7 publications

References 0 publications

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)

Syntheses and Structures of Methyltris(pyrazolyl)silane Complexes of the Group 6 Metals

Chapter 13. Transition-metal carbonyls and organometallic complexes

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The crystal structure of π-cyclopentadienyltricarbonyl-σ-phenyltungsten

Cited by 7 publications

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Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)3(η-C5H5) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe3)(CO)3(η-C5H5), W{C⋮CC[CH=C(CN)2]=C(CN)2}(CO)3(η-C5H5), andcis-W(C⋮CPh)(CO)2(PPh3)(η-C5H5)

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)3(η-C5H5) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe3)(CO)3(η-C5H5), W{C⋮CC[CH=C(CN)2]=C(CN)2}(CO)3(η-C5H5), andcis-W(C⋮CPh)(CO)2(PPh3)(η-C5H5)

Syntheses and Structures of Methyltris(pyrazolyl)silane Complexes of the Group 6 Metals

Chapter 13. Transition-metal carbonyls and organometallic complexes

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Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)

Syntheses and Chemistry of the Diynyl Complexes M(C⋮CC⋮CH)(CO)₃(η-C₅H₅) (M = Mo, W): Crystal Structures of W(C⋮CC⋮CSiMe₃)(CO)₃(η-C₅H₅), W{C⋮CC[CH=C(CN)₂]=C(CN)₂}(CO)₃(η-C₅H₅), andcis-W(C⋮CPh)(CO)₂(PPh₃)(η-C₅H₅)