Hydridoborates and hydridoborato metallates

Knizek, Jörg; Nöth, Heinrich

doi:10.1016/s0022-328x(00)00688-4

Cited by 65 publications

(52 citation statements)

References 26 publications

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“…No reaction was observed on treating 1 with lithium 2-dihydro-2-boratafluorene [20] in diethyl ether as expected for a reaction according to Equation (15). However, when the ether was replaced by THF a 11 B NMR signal at δ = 7.6 ppm suggested the formation of the corresponding titanium(IV) diorganyldihydridoborate.…”

Section: Resultsmentioning

confidence: 58%

“…The homogeneous reaction of 1 with lithium bis(cyclohexyl)dihydridoborate [20] in diethyl ether yielded the titanium(IV) bis(cyclohexyl)dihydridoborate 16 within 4 hours almost quantitatively; see Equation (13). 1 H and 13 C NMR signals for compound 16 and one 11 B NMR signal at δ = 15.0 ppm were observed both at room temperature and at -80°C.…”

Section: Resultsmentioning

confidence: 99%

“…Unexpected was the heterogeneous reaction of 1 with K[H 2 B(C 5 H 10 ) 2 ] [19,20] in pentane (T = -110 to 20°C). This reaction led to a single 11 B NMR signal at 7.3 ppm, which we assigned to compound 10; see Equation (7).…”

Section: Resultsmentioning

confidence: 99%

“…This result contrasts the easy preparation and crystal structure determination of bis-(cyclopentadienyl)zirconium(IV) dihydridoborinate. [4,19] The reaction of 1 with [K(H 2 -9-BBN)] [20] in hexane is much less complicated. Yields of up to 70 % of compound 11 (δ B = 11.1 ppm) were obtained; see Equation (9).…”

Section: Resultsmentioning

confidence: 99%

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Tris(2,6‐diisopropylphenolato)titanium(IV) Dihydridodiorganylborates: Synthesis and Structures

Knizek

Nöth

2011

Eur J Inorg Chem

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The reactions of tris(2,6‐diisopropylphenolato)titanium(IV) chloride with alkali‐metal dihydridodiorganylborates M(H2BR2) (M = Li, K; R = Me, C6H11, CMe3; BR2 = BC5H10, BC8H14) led to the corresponding titanium dihydridodiorganylborates. However, in almost all cases byproducts such as (2,6‐diisopropylphenolato)diorganylboranes, triorganylboranes, diorganylboranes, diborane and tetrakis(2,6‐diisopropylphenolato)titanium(IV) were also generated. (2,6‐iPr2C6H3O)3Ti(H2BR2) compounds also resulted from the interaction of methyltris(2,6‐diisopropylphenolato)titanium, for example, with catecholborane. In addition to the formation of tris(2,6‐diisopropylphenolato)catecholboratotitanium(IV), B‐methylcatecholborane was also formed The reaction of potassium dihydro‐9‐cyclooctylborate with 2,6‐bis(2,2‐di‐tert‐butyl‐2‐hydroxyethyl)pyridinetitanium dichloride (LTiCl2) led to the complex LTi(H2BC8H14)2. This compound showed no agostic C–H···Ti interaction in contrast to (2,6‐iPr2C6H3O)3TiH2BC8H14 and the corresponding titanium dihydridobis(cyclohexyl)borate.

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Section: Resultsmentioning

confidence: 58%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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Tris(2,6‐diisopropylphenolato)titanium(IV) Dihydridodiorganylborates: Synthesis and Structures

Knizek

Nöth

2011

Eur J Inorg Chem

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“…Thiols were attractive, as B À S bonds are weaker than analogous B À O bonds and the acidity of the SH moiety could aid the reaction. On the basis of DFT calculations for the gas phase, coupled with experimental data or estimates of the heats of vaporization, benzenedithiol was predicted to be a better reagent than thiophenol for the reaction with borazine, a computational surrogate for PB, where the products are presumed to retain the B À H bond ( [14] suggesting that [NH 4 ][B(C 6 H 4 S 2 ) 2 ] is formed (this assignment is consistent with the calculated NMR spectrum, see the Supporting Information). Attempts to make this product independently from (C 6 H 4 S 2 )BÀH·(NH 3 ) and benzenedithiol failed to produce a pure material even under driving conditions (heat and gas removal by freezepump-thaw cycles).…”

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Efficient Regeneration of Partially Spent Ammonia Borane Fuel

et al. 2009

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Synthesis and Structures of Amino(triphenylgermyl) Boranes and Trihydro(triphenylgermyl) Borates

Habereder¹,

Nöth²

2001

Z. anorg. allg. Chem.

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The B-(triphenylgermyl)borazines 4 a and 4 b, the 1,2-bis(dimethylamino)-1,2-bis(triphenylgermyl)-diborane(4), 5, and the (2,2,6,6-tetramethylpiperidino)(triphenylgermyl)-boranes 6 and 7 were prepared by allowing LiGePh 3 to react with the corresponding B-bromoborazines and aminochloroboranes, respectively. BH 3 dissolved in thf readily adds to LiGePh 3 generating Li(H 3 BGePh 3 ), 8 a, in thf solution. Addition of N-bases to the solution of 8 a produced (tment hf)Li(H 3 BGePh 3 ), 8 b, and dimeric (py) 2 Li(H 3 BGePh 3 ), 8 c. The borazine ring in 4 b is distorted into a boat shape. In 5 the NBGe planes are twisted against each other by 85°.Comparison with analogous (triphenylstannyl)boranes points to a more pronounced steric effect of the Ph 3 Ge group over the Ph 3 Sn group due to the shorter B±Ge bond. A fairly short B±Ge bond is found for the (triphenylgermyl)trihydroborates. The molecular structure of (Et 2 O) 3 LiGePh 3 shows compressed C±Ge±C bond angles. Its molecular parameters fit well into the series L n LiEPh 3 (E = Si, Sn, Pb). Synthese und Strukturen von Amino(triphenylgermyl)boranen und Trihydro(triphenylgermyl)boratenInhaltsu È bersicht. Die B-(Triphenylgermyl)borazine 4 a und 4 b, das 1,2-Bis(dimethylamino)-1,2-bis(triphenyl-germyl)diboran(4) 5 und die (2,2,6,6-Tetramethylpiperidino)(triphenylgermyl)borane 6 und 7 wurden durch Umsetzung von LiGePh 3 mit den entsprechenden B-Bromoborazinen bzw. Aminochloroboranen dargestellt. In thf gelo È stes BH 3 addiert sich an LiGePh 3 zu Li(H 3 BGePh 3 ), 8 a. Zugabe von N-Basen zu dessen Lo È sung ergibt (tmen)(thf)Li(H 3 BGePh 3 ), 8 b, und dimeres (py) 2 Li(H 3 BGePh 3 ), 8 c. Der Borazinring in 4 b ist zu einer Bootkonformation verzerrt. In 5 sind die NBGeEbenen um 85°gegeneinander verdrillt. Der Vergleich mit den entspechenden (Triphenylstannyl)boranen weist auf einen ausgepra È gteren sterischen Effekt de Phe 3 Ge-Gruppe gegenu È ber der Ph 3 Sn-Gruppe als Folge der ku È rzeren B±Ge-Bindung hin. In den (Triphenylgermyl)hydroboraten liegen ziemlich kurze B±Ge-Bindungen vor. Die Moleku È lstruktur von (Et 2 O) 3 LiGePh 3 weist kleine C±Ge±C-Winkel auf. Sie passen sehr gut in die Reihe der L n LiEPh 3 -Verbindungen (E = Si, Sn, Pb).

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Hydridoborates and hydridoborato metallates

Cited by 65 publications

References 26 publications

Tris(2,6‐diisopropylphenolato)titanium(IV) Dihydridodiorganylborates: Synthesis and Structures

Tris(2,6‐diisopropylphenolato)titanium(IV) Dihydridodiorganylborates: Synthesis and Structures

Efficient Regeneration of Partially Spent Ammonia Borane Fuel

Synthesis and Structures of Amino(triphenylgermyl) Boranes and Trihydro(triphenylgermyl) Borates

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