[VCl3(NPPh3)(OPPh3)], ein Phosphaniminato‐Komplex von Vanadium(IV)

Rübenstahl, T.; Dehnicke, Kurt; Krautscheid, Harald

doi:10.1002/zaac.19936190612

Cited by 5 publications

(8 citation statements)

References 17 publications

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“…31 P NMR δ: 54.3 (∆ν 1/2 ) 511 Hz). 13 C NMR δ: 143.9, 143.1, 129.5, 128.9, 127.1, 124.6, 122.8, 41.8, 41.5 (d, tBu, 1 J P-C ) 31.5 Hz), 29.7, 29.0, 25.0.…”

Section: Synthesis Of Vcl(n(sime 3 ) 2 )(Nph)(nptbu 3 ) (14)mentioning

confidence: 99%

“…[9][10][11] In addition, several groups have reported related vanadium(IV)-and vanadium(III)-phosphinimide derivatives. [12][13][14][15][16][17] In this paper, we describe our efforts to prepare and characterize V(V)-phosphinimide derivatives. A series of vanadium-imide-phosphinimide complexes are reported.…”

Section: Introductionmentioning

confidence: 99%

“…19 All organic reagents were purified by conventional methods. 1 H and 13 C{ 1 H} NMR spectra were recorded on Bruker Avance-300 and 500 spectrometers. All spectra were recorded in C 6 D 6 at ambient temperatures unless otherwise noted.…”

Section: Introductionmentioning

confidence: 99%

“…31 P NMR δ: 62.4 (∆ν 1/2 ) 732 Hz). 13 13). Alkylation and arylation reactions were performed in a similar manner using MeLi or PhMgBr and the appropriate vanadium dichloride precursor; thus, only one preparation is detailed.…”

Section: Introductionmentioning

confidence: 99%

“…J H-H ) 8 Hz),6.71 (t, 1H, Np-Ph,3 J H-H ) 7 Hz), 1.05 (d, 27H, tBu,3 J P-H ) 14 Hz) 31. P NMR δ: 64.4 (∆ν 1/2 ) 625 Hz) 13. C NMR δ: 128.7, 125.2, 123.1, 42.1 (d, tBu, 1 J P-C ) 40 Hz), 29.7. ν N-P : 1122 cm -1 .…”

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Synthesis and Characterization of Vanadium(V)−Phosphinimide Complexes

Hawkeswood

Stephan

2003

Inorg. Chem.

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Synthetic routes to vanadium(V)-phosphinimide derivatives are addressed. Initial synthetic efforts afforded the known compound formulated as VCl(2)(NPPh(3))(3) which was crystallographically determined to be the salt [VCl(NPPh(3))(3)]Cl (1). Reactions of the vanadium-imide precursors VCl(3)(NAr) (Ar = Ph, C(6)H(3)-2,6-iPr(2)) with R(3)PNSiMe(3) (R = Ph, iPr, tBu) afforded VCl(2)(NPh)(NPPh(3)) (4), VCl(2)(NPh)(NPiPr(3)) (5), VCl(2)(NPh)(NPtBu(3)) (6), VCl(2)(NC(6)H(3)-2,6-iPr(2))(NPPh(3)) (7), VCl(2)(NC(6)H(3)-2,6-iPr(2))(NPiPr(3)) (8), and VCl(2)(NC(6)H(3)-2,6-iPr(2))(NPtBu(3)) (9) in yields ranging from 72% to 84%. Subsequent alkylation or arylation reactions resulted in VMe(2)(NC(6)H(3)-2,6-iPr(2))(NPtBu(3)) (10), VPh(2)(NPh)(NPtBu(3)) (11), VPh(2)(NC(6)H(3)-2,6-iPr(2))(NPiPr(3)) (12), and VPh(2)(NC(6)H(3)-2,6-iPr(2))(NPtBu(3)) (13) while substitution reactions with Li[N(SiMe(3))(2)] and Li[SBn] gave VCl(N(SiMe(3))(2))(NPh)(NPtBu(3)) (14) and V(SBn)(2)(NC(6)H(3)-2,6-iPr(2))(NPtBu(3)) (15) in yields ranging from 40% to 49% yield. Polarization of the N-P phosphinimide bond and V-N multiple bond character are evidenced by crystallographic data.

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“…31 P NMR δ: 54.3 (∆ν 1/2 ) 511 Hz). 13 C NMR δ: 143.9, 143.1, 129.5, 128.9, 127.1, 124.6, 122.8, 41.8, 41.5 (d, tBu, 1 J P-C ) 31.5 Hz), 29.7, 29.0, 25.0.…”

Section: Synthesis Of Vcl(n(sime 3 ) 2 )(Nph)(nptbu 3 ) (14)mentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Synthesis and Characterization of Vanadium(V)−Phosphinimide Complexes

Hawkeswood

Stephan

2003

Inorg. Chem.

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Phosphaniminato‐Komplexe des Vanadiums Die Kristallstruktur von [V₃Cl₆(NPMe₃)₅⁺]₂[V₄O₄Cl₈(NPMe₃)₂²⁻] ·; 6 CH₃CN

Rübenstahl

Dehnicke

Magull

1995

Zeitschrift anorg allge chemie

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Professor Dietrich Babel zum 65. Geburtstag gewidmet Inhaltsiibersicht. Vanadiumtetrachlorid reagiert in CC14-Lijsung rnit MesSiNPMe3 unter Bildung des Donor-Akzeptorkomplexes [VCL,(Me,SiNPMe,)], der sich in siedendem Acetonitril rnit weiterem Me3SiNPMe3 zu dem Phosphaniminatokomplex [V3C16(NPMe,),] 'C1-umsetzt. Durch partielle Hydrolyse in Acetonitrillosung entstehen hieraus schwarze Einkristalle[V3C16(NPMe3)5+]2[V404Cls(NPMe3)~-] * 6CH3CN, die wir rontgenographisch charakterisiert haben. Raumgruppe P2, /c, Z = 2, Strukturlosung mit 3 008 unabhangigen beobachteten Reflexen, R = 0,090. Gitterkonstanten bei -70°C: a = 1379,O; b = 1915,8; c = 2278 pm, / 3 = 102,79". In dem komplexen Kation bilden die drei Vanadiumatome rnit zwei p3-NPMe3-Gruppen eine trigonale Bipyramide, die drei ubrigen NPMe,-Gruppen und die Chloratome sind terminal gebunden. In dem Anion [V404C18(NPMe,)2]2-sind die Vanadiumatome iiber p2-0-Atome zu einem Rechteck verknupft; zusatzlich fungieren die beiden Phosphaniminatoliganden als p2-N-Brucken. Phosphoraneiminato Complexes of Vanadiun i. The Crystal Structure of [V,CI,(NPMe,),fl,[V,O,CI,(NPMe,)~-] -6 CH ,CN Abstract. Vanadiumtetrachloride reacts in CC1, solution with Me3SiNPMe3 to form the donor acceptor complex [VC14(Me3SiNPMe3)], which reacts with excess Me,SiNPMe, in boiling acetonitrile to form the phosphoraneiminato complex [V,C&(NPMe& + Cl-. Partial hydrolysis in acetonitrile solution leads to black single crystals of [V3Cl6(NPMe3),+],-[V404Cls(NPMe3)?-] . 6CH3CN, which are characterized by a crystal structure determination. Space group P2,/c, Z = 2, structure solution with 3 008 observed unique reflections, R = 0.090. Lattice dimensions at -70°C: a = 1379.0, b = 1915.8, c = 2278 pm, p = 102,79". In the complex cation the three vanadium atoms form a trigonal bipyramid with two p3-NPMe3 groups; the residual NPMe,-groups and the chlorine atoms are in terminal functions. In the anion [V404C18(NPMe3)2]2-the vanadium atoms are linked by p2-0 atoms to form a rectangle; in addition the two phosphoraneiminato ligands form p2-N bridges.

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