Bis‐(trimethylsilyl)‐amino‐halogenoborane

Geymayer, Peter; Rochow, Eugene G.; Wannagat, U.

doi:10.1002/ange.19640761117

Cited by 44 publications

(13 citation statements)

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“…The two-step procedure starts with a modified Brellochs reaction [47] yielding salts of the 10-vertex carborate anion [6-Ph-6-nido-CB 9 H 11 ] À , [48] followed by boron insertion using BH 3 3À , which underwent boron insertion reactions with Cl 2 BNA C H T U N G T R E N N U N G (SiMe 3 ) 2 [50] to produce the respective NA C H T U N G T R E N N U N G (SiMe 3 ) 2 -substituted 12-vertex carba-closododecaborates. These silylated intermediates were neither characterized spectroscopically nor isolated.…”

Section: Salts Of the [1-h 2 N-closo-cb 11 H 11 ]mentioning

confidence: 99%

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Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)

Finze

2009

Chemistry A European J

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The first primary 2-aminocarba-closo-dodecaborates [1-R-2-H(2)N-closo-CB(11)H(10)](-) (R=H (1), Ph (2)) have been synthesized by insertion reactions of (Me(3)Si)(2)NBCl(2) into the trianions [7-R-7-nido-CB(10)H(10)](3-). The difunctionalized species [1,2-(H(2)N)(2)-closo-CB(11)H(10)] (3) and 1-CyHN-2-H(3)N-closo-CB(11)H(10) (H-4) have been prepared analogously from (Me(3)Si)(2)NBCl(2) and 7-H(3)N-7-nido-CB(10)H(12). In addition, the preparation of [Et(4)N][1-H(2)N-2-Ph-closo-CB(11)H(10)] ([Et(4)N]-5) starting from PhBCl(2) and 7-H(3)N-7-nido-CB(10)H(12) is described. Methylation of the [1-Ph-2-H(2)N-closo-CB(11)H(10)](-) ion (2) to produce 1-Ph-2-Me(3)N-closo-CB(11)H(10) (6) is reported. The crystal structures of [Et(4)N]-2, [Et(4)N]-5, and 6 were determined and the geometric parameters were compared to theoretical values derived from DFT and ab initio calculations. All new compounds were studied by NMR, IR, and Raman spectroscopy, MALDI mass spectrometry, and elemental analysis. The discussion of the experimental NMR chemical shifts and of selected vibrational band positions is supported by theoretical data. The thermal properties were investigated by differential scanning calorimetry (DSC). The pK(a) values of 2-H(3)N-closo-CB(11)H(11) (H-1), 1-H(3)N-closo-CB(11)H(10) (H-7), and 1,2-(H(3)N)(2)-closo-CB(11)H(10) (H(2)-3) were determined by potentiometric titration and by NMR studies. The experimental results are compared to theoretical data (DFT and ab initio). The basicities of the aminocarba-closo-dodecaborates agree well with the spectroscopic and structural properties.

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Section: Salts Of the [1-h 2 N-closo-cb 11 H 11 ]mentioning

confidence: 99%

“…(Me 3 Si) 2 NBCl 2 was synthesized according to a known procedure. [50] 7-H 3 N-7-nido-CB 10 H 12 , [10] 7-CyH 2 N-7-nido-CB 10 H 12 , [45] [84] 1-H 3 N-closo-CB 10 H 11 (H-7) [9] and Cs[7-nido-CB 10 H 13 ] [44] were prepared according to known procedures.…”

mentioning

confidence: 99%

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)

Finze

2009

Chemistry A European J

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“…[36] Compound 3 can be isolated by distillation at 89°C/11 Torr. Single-crystals, obtained from a hexane solution at -78°C, were found to melt at 5-7°C.…”

Section: 46-trihaloborazines and Their Structuresmentioning

confidence: 99%

“…At -78°C stirring was started and a solution of (HN=BCl) 3 [69] (0.68 g, 3.7 mmol), dissolved in toluene (25 mL), was drop wise added to the suspension. After warming to ambient temperature the reaction was followed by 11 B NMR spectroscopy: the signal of (HN=BCl) 3 [Bis(trimethylsilyl)amino]dichloroborane (3): [36] a) A 250 mL threenecked round-bottomed flask fitted with a dry-ice reflux condenser was charged with a solution of N(SiMe 3 ) 3 (5.95 g, 25.5 mmol) in hexane (50 mL). BCl 3 (43.0 g, 30.0 mL), condensed in a dry-ice cooled dropping funnel, was then diluted with hexane (50 mL).…”

Section: 46-trifluoroborazine (1)mentioning

confidence: 99%

Structural Chemistry of Borazines

Anand¹,

Nöth²,

Schwenk‐Kircher³

et al. 2008

Eur J Inorg Chem

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Keywords: Borazines / Ring distortionThe solid-state structure of (HN=BF) 3 has been redetermined. It is characterised by a stacking of the molecules, similar to hexagonal boron nitride. In contrast, (F 3 CH 2 N=BF) 3 shows no intermolecular interactions between the planar borazine rings. In (Cl 2 BN=BCl) 3 , the Cl 2 B groups are almost perpendicularly oriented to the planar borazine ring and its B-Cl bonds are shorter than the Cl-B bonds to the ring boron atoms. Reactions of (Cl 2 BN=BCl) 3 with Me 3 SiNMe 2 allows a successive Cl/Me 2 N exchange. Depending on the molar ratio, the compounds [Cl

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“…Hexakis(trimethylsilyl)-2,4-diamino-1,3,2, 4-diazadiboretidin wurde zuerst yon Geymayer, Rochow & Wannagat (1964) und yon Russ & McDiarmid (1964) beschrieben. Die Verbindung enth~dt einen Vierring aus alternierenden B-und N-Atomen, die aber im Gegensatz zu den entsprechenden Atomen in den Cycloborazanen dreibindig sind, ferner sind an die B-Atome je ein exocyclisches N-Atom gebunden.…”

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Strukturbestimmungen an Bor–Stickstoff-Verbindungen. IV. Die Kristall- und Molekularstruktur von Hexakis(trimethylsilyl)-2,4-diamino-1,3,2,4-diazadiboretidin

Hess¹

1969

Acta Crystallogr Sect B

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The title compound, a four-membered boron-nitrogen ring system, was investigated by X-ray methods.The crystals are monoclinic, space group P21/a with a=22.11, b= 14.96, c= 10.93/~, ~= 108"6 °, and four molecules in the unit cell. The structure determination is based on 3449 reflexion values, which were mainly obtained with the aid of an automatic diffractometer. Three-dimensional Patterson and Fourier syntheses were used for the structure determination. The structure was refined by least squares. The proposed structure could be confirmed. The four-membered.ring is planar, within the limits of accuracy of the determination, and the substituents on the N atoms are also arranged in a plane. The Si atoms attached to the exocyclic N atoms lie, however, not in the plane of the four-membered ring, but almost perpendicular to it. This can be attributed to steric factors. The following average bond lengths were found: B-N 1.45, N-Si 1.75, Si-C 1.87/~. The shortness of the exocyclic B-N bond is surprising since the substituent on the B and N atoms are arranged nearly perpendicularly to one another, not allowing the formation of a classical n-bond.

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Bis‐(trimethylsilyl)‐amino‐halogenoborane

Abstract: entsteht unter den gleichen Bedingungen 2(C2H&O,HSnCI3 (SS,-H = -1 l,8 ppm).In ihrem chemischen Verhalten unterscheiden sich die Atherate der Trihalogengermane stark von den (1917).Uns gelang nunniehr auch die Darstellung von Verbindungen mit der Gruppierung >B-N(Si<)2.

Cited by 44 publications

References 4 publications

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)

Structural Chemistry of Borazines

Strukturbestimmungen an Bor–Stickstoff-Verbindungen. IV. Die Kristall- und Molekularstruktur von Hexakis(trimethylsilyl)-2,4-diamino-1,3,2,4-diazadiboretidin

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Bis‐(trimethylsilyl)‐amino‐halogenoborane

Abstract: entsteht unter den gleichen Bedingungen 2(C2H&O,HSnCI3 (SS,-H = -1 l,8 ppm).In ihrem chemischen Verhalten unterscheiden sich die Atherate der Trihalogengermane stark von den (1917).Uns gelang nunniehr auch die Darstellung von Verbindungen mit der Gruppierung >B-N(Si<)2.

Cited by 44 publications

References 4 publications

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H2N‐closo‐CB11H10] (R=H, Ph, H2N, CyHN)

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H2N‐closo‐CB11H10] (R=H, Ph, H2N, CyHN)

Structural Chemistry of Borazines

Strukturbestimmungen an Bor–Stickstoff-Verbindungen. IV. Die Kristall- und Molekularstruktur von Hexakis(trimethylsilyl)-2,4-diamino-1,3,2,4-diazadiboretidin

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Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)

Synthesis and Characterization of 2‐Mono‐ and 1,2‐Diaminocarba‐closo‐dodecaborates M[1‐R‐2‐H₂N‐closo‐CB₁₁H₁₀] (R=H, Ph, H₂N, CyHN)