The application of TOCSY to boron chemistry

Donohoe, David J.; Reed, David; Welch, Alan J.

doi:10.1016/0277-5387(94)00485-w

Cited by 7 publications

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“…Finally, we report the experimental 11 B NMR spectrum of monophenylcarborane and its complete assignment via 11 B{ 1 H}/ 11 B{ 1 H} (COSY), 1 H{ 11 B selective } and 1 H{ 11 B}/ 1 H{ 11 B} (COSY) spectroscopy. These complement results of an 11 B{ 1 H}/ 11 B{ 1 H} (TOCSY; total correlation spectroscopy) experiment on 1-Ph-1,2- closo -C 2 B 10 H 11 reported recently …”

Section: Introductionsupporting

confidence: 84%

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

Brain¹,

Cowie²,

Donohoe³

et al. 1996

Inorg. Chem.

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The compound 1-phenyl-1,2-dicarba-closo-dodecaborane(12), 1-C(6)H(5)-1,2-closo-C(2)B(10)H(11) (1), has been synthesized and characterized by a complete assignment of its (11)B NMR spectrum via (11)B{(1)H}/(11)B{(1)H} (COSY), (1)H{(11)B(selective)} and (1)H{(11)B}/(1)H{(11)B} (COSY) spectroscopy. An electron- and X-ray diffraction investigation of 1, complemented by ab initio calculations, has been undertaken. The gas-phase electron-diffraction (GED) data can be fitted by several models describing conformations which differ in the position of the phenyl ring with respect to the carborane cage. Local symmetries ofC(2)(v)() and D(6)(h)() for the 1,2-C(2)B(10) and C(6) moieties, respectively, were adopted in the GED model in order to simplify the problem. In addition, constraints among the close-lying C-C and B-B bonds were employed. However, even though such simplifications led to satisfactory refinements (R(G) = 0.069-0.071), a unique, definitive solution could not be gained. The (C-C)(mean), (C-B)(mean) and (B-B)(mean) bond lengths,r(a), are ca. 1.44, 1.72, and 1.78 Å, respectively. The C(6) hexagon, with r(a)(C-C) = ca. 1.394 Å, either eclipses the C(1)-C(2) vector (overall C(s)() symmetry) or more or less eclipses the C(1)-B(4) cluster bond (overall C(1) symmetry). In contrast, in the solid at 199 K, the ring lies at a position intermediate between the two GED positions, as determined by X-ray crystallography [C(8)H(16)B(10), monoclinic P2(1)/a: a = 12.047(3) Å, b = 18.627(4) Å, c = 12.332(5) Å, beta = 110.09(4) degrees, Z = 8]. The C-B distances span the range 1.681(6)-1.743(5) Å, and B-B lengths lie between 1.756(6) and 1.795(6) Å. A similar conformation was found for the theoretical (RHF/6-31G level) structure which was fully optimized in C(1) symmetry. The r(e) distances are consistent with the dimensions derived in the experimental studies. IGLO calculations of the (11)B chemical shifts, in addition to SCF single-point energies of the GED structures, further support these observations.

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Section: Introductionsupporting

confidence: 84%

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

Brain¹,

Cowie²,

Donohoe³

et al. 1996

Inorg. Chem.

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Boron NMR

Reed¹

2007

Encyclopedia of Magnetic Resonance

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The use of low mixing time TOCSY experiments to provide phase-sensitive 11B cosy data

Reed

1996

Polyhedron

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The application of TOCSY to boron chemistry

Cited by 7 publications

References 5 publications

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

Boron NMR

The use of low mixing time TOCSY experiments to provide phase-sensitive 11B cosy data

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The application of TOCSY to boron chemistry

Cited by 7 publications

References 5 publications

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C2B10H11. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C2B10H11. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

Boron NMR

The use of low mixing time TOCSY experiments to provide phase-sensitive 11B cosy data

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Product

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About

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations

1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C₂B₁₀H₁₁. Synthesis, Characterization, and Structure As Determined in the Gas Phase by Electron Diffraction, in the Crystalline Phase at 199 K by X-ray Diffraction, and by ab Initio Computations