Das LiPH<sub>2</sub> ·1 Monoglym

Schäfer, H.; Fritz, G.; Hölderich, Wolfgang F.

doi:10.1002/zaac.19774280127

Cited by 71 publications

(30 citation statements)

References 9 publications

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“…NMR spectra were recorded on a Jeol Eclipse-400 spectrometer operating at 400. [18], KP(H)SiiPr 3 [19], KPHSi(tBu) 3 [19], HP(SiiPr 3 ) 2 [11]; (thf)W(CO) 5 was prepared by UV-irradiation of W(CO) 6 in THF solution [8].…”

Section: Experimental General Remarksmentioning

confidence: 99%

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Rotter¹,

Karaghiosoff²,

Mayer³

et al. 2005

Heteroatom Chemistry

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Section: Experimental General Remarksmentioning

confidence: 99%

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Rotter¹,

Karaghiosoff²,

Mayer³

et al. 2005

Heteroatom Chemistry

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“…[7] (4.12 g, 31.71 mmol) in THF (100 mL) at 0 8C. The reaction mixture was subsequently warmed to 22 8C and stirred for 16 h, resulting in a clear solution.…”

mentioning

confidence: 99%

Synthesis of Macrocyclic Aluminum–Phosphorus and Gallium–Phosphorus Compounds

Hänisch¹,

Stahl²

2006

Angew Chem Int Ed

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Compounds of the type R 2 Al À PR' 2 and R 2 Ga À PR' 2 show a strong tendency to form cyclic s-donor-s-acceptor species [R 2 MÀPR' 2 ] n (M = Al, Ga; n = 2, 3). [1,2] These compounds usually feature four-or six-membered rings (I or II). Monomeric compounds are only isolated when the substituents R and R' are sterically very demanding.[3] Recently, we obtained the first evidence that larger cycles can also be synthesized. The reaction of the diphosphanylsilane iPr 2 Si(PH 2 ) 2 with MEt 3 (M = Al, Ga, In) leads to the compounds [iPr 2 Si{P(H)MEt 2 } 2 ] 2 .[4] The products feature an eight-membered M 4 P 4 ring, in which the two pairs of opposing phosphorus atoms are bridged by iPr 2 Si groups, resulting in an M 4 P 4 Si 2 adamantoid cage (III).By varying the bridging units between the phosphorus atoms, it should be possible to obtain polycyclic compounds with new structural motifs. For this reason, we synthesized the diphosphanyldisiloxane O(SiiPr 2 PH 2 ) 2 (1). The eight-membered ring compound [O(SiiPr 2 ) 2 PH] 2 (2) was isolated as a byproduct. Both 1 and 2 were obtained from the reaction of the dichlorodisiloxane O(SiiPr 2 Cl) 2 with two equivalents of [LiPH 2 (dme)] (dme = dimethoxyethane) in THF [Eq. (1)]. Compound 1 can be isolated in a pure form by distillation, and 2 can subsequently be obtained by recrystallization of the distillation residue.In the 31 P NMR spectrum of 1, a triplet of higher order at d = À261.8 ppm represents the AA' part of an AA'X 2 X' 2 spin system. The 1 H NMR spectrum shows a doublet of higher order at d = 1.32 ppm, with a 1 J P,H coupling constant of 185 Hz, that is assigned to the phosphanyl groups (X 2 X' 2 part), as well as a multiplet at d = 1.13 ppm that is assigned to the isopropyl groups. In the 29 Si{ 1 H} NMR spectrum, the X part of an ABX spin system is observed, with 1 J Si,P and 3 J Si,P coupling constants of 24.3 and 0.12 Hz. Silicon satellites corresponding to the AB part of the spin system are detected in the 31 P{ 1 H} NMR spectrum. In the 13 C{ 1 H} NMR spectrum, a multiplet assigned to the tertiary carbon atoms, as well as two multiplets assigned to the diastereotopic methyl groups are observed. In the electron ionization (EI) mass spectrum of 1, the molecular-ion (

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“…The monomeric complexes 1 {±100 ± 3°C; a = 1391.1(4); b = 809.8 (2); c = 1249.1(3) pm; b = 102.84(2)°}, 2 {±100 ± 3°C; a = 1398.3(4); b = 819.8(3); c = 1258.5(4) pm; b = 103.35(2)°} and 3 {±100 ± 3°C; a = 1308.4(2); b = 788.2(1); c = 1195. 6(1) pm; b = 95.…”

Section: Professor Hartmut Ba èRnighausen Zum 65 Geburtstag Gewidmetmentioning

confidence: 99%

“…Ebenso unerwartet fielen bei Reaktionen von 1-Chlor-2,2-bis(trimethylsilyl)-1k 3 -phosphaethen mit (1,2-Dimethoxyethan-O,O')lithium-bis(trimethylsilyl)stibanid bzw. von 2,3,4, 3 -phosphol-3-id mit x-Bromstyrol in 1,2-Dimethoxyethan das analog zusammengesetzte Chlorid 3 und Bromid 4 an. Die monomeren Komplexe 1 {±100 ± 3°C; a = 1391,1 (4) Abstract.…”

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“…Halogenid-Anionen a È quatoriale Positionen {Li±P 260,4(4); Li±As 269,8 (6); Li±Cl 238,6(7); Li±Br 256,3(10) pm}, wa È hrend die Chelatliganden a È quatoriale und axiale Lagen u È berbru È cken {Li±O eq 205,4(4) bis 207,4(4); Li±O ax 208,9(3) bis 215,5(2) pm}. Die Koordination im (dme) 2 Li-Fragment, die Li±X-Absta È nde (X = P, As, Cl, Br), die Struktur der Chelatringe und die Packung der Neutralkomplexe werden im Detail diskutiert. Abstract.…”

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Bis(1,2-dimethoxyethan-O,O′)lithium-phosphanid, -arsanid und -chlorid – drei neue Vertreter des Bis(1,2-dimethoxyethan-O,O′)lithium-bromid-Typs

Becker¹,

Eschbach²,

Mündt³

et al. 1998

Z. anorg. allg. Chem.

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Bei Versuchen zur Isolierung des thermisch instabilen Lithium‐silylphosphanids schieden sich bei –60 °C aus 1,2‐Dimethoxyethan Einkristalle des bisher unbekannten Dismutierungsproduktes Bis(1,2‐dimethoxyethan‐O,O′)lithium‐phosphanid (1) ab. Das homologe Arsanid 2 kristallisierte aus, nachdem eine bei –78 °C eingefrorene Lösung von Arsan im selben Lösungsmittel mit Lithium‐n‐butanid behandelt worden war. Ebenso unerwartet fielen bei Reaktionen von 1‐Chlor‐2,2‐bis(trimethylsilyl)‐1λ3‐phosphaethen mit (1,2‐Dimethoxyethan‐O,O′)lithium‐bis(trimethylsilyl)stibanid bzw. von Lithium‐1,2,3,4,5‐pentaphenyl‐2,3‐dihydro‐1λ3‐phosphol‐3‐id mit ω‐Bromstyrol in 1,2‐Dimethoxyethan das analog zusammengesetzte Chlorid 3 und Bromid 4 an. Die monomeren Komplexe 1 {–100 ± 3 °C; a = 1391,1(4); b = 809,8(2); c = 1249,1(3) pm; β = 102,84(2)°}, 2 {–100 ± 3 °C; a = 1398,3(4); b = 819,8(3); c = 1258,5(4) pm; β = 103,35(2)°} und 3 {–100 ± 3 °C; a = 1308,4(2); b = 788,2(1); c = 1195,6(1) pm; β = 95,35(1)°} kristallisieren in der monoklinen Raumgruppe C2/c mit vier solvatisierten Ionenpaaren in der Elementarzelle und sind isotyp zum bereits von Rogers u. a. [13] bei Zimmertemperatur untersuchten Bis(1,2‐dimethoxyethan‐O,O′)lithium‐bromid (4) {–73 ± 2 °C; a = 1319,0(2); b = 794,1(1); c = 1214,3(2) pm; β = 96,22(1)°}. In den trigonal‐bipyramidal koordinierten Neutralkomplexen der Symmetrie C2 besetzen die Pnikogenanid‐ bzw. Halogenid‐Anionen äquatoriale Positionen {Li–P 260,4(4); Li–As 269,8(6); Li–Cl 238,6(7); Li–Br 256,3(10) pm}, während die Chelatliganden äquatoriale und axiale Lagen überbrücken {Li–Oeq 205,4(4) bis 207,4(4); Li–Oax 208,9(3) bis 215,5(2) pm}. Die Koordination im (dme)2Li‐Fragment, die Li–X‐Abstände (X = P, As, Cl, Br), die Struktur der Chelatringe und die Packung der Neutralkomplexe werden im Detail diskutiert.

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Das LiPH₂ ·1 Monoglym

Cited by 71 publications

References 9 publications

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Synthesis of Macrocyclic Aluminum–Phosphorus and Gallium–Phosphorus Compounds

Bis(1,2-dimethoxyethan-O,O′)lithium-phosphanid, -arsanid und -chlorid – drei neue Vertreter des Bis(1,2-dimethoxyethan-O,O′)lithium-bromid-Typs

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Das LiPH2 ·1 Monoglym

Cited by 71 publications

References 9 publications

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Coordination of phosphanide and trialkylsilylphosphanide ligands at pentacarbonyltungsten fragments: An NMR spectroscopic and structural investigation

Synthesis of Macrocyclic Aluminum–Phosphorus and Gallium–Phosphorus Compounds

Bis(1,2-dimethoxyethan-O,O′)lithium-phosphanid, -arsanid und -chlorid – drei neue Vertreter des Bis(1,2-dimethoxyethan-O,O′)lithium-bromid-Typs

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Das LiPH₂ ·1 Monoglym