21205-91-4Relevant articles and documents
Europium(II) and Ytterbium(II) Cyclic Organohydroborates: An Europium(II) Complex with an Agostic Interaction
Chen, Xuenian,Lim, Soyoung,Plecnik, Christine E.,Liu, Shengming,Du, Bin,Meyers, Edward A.,Shore, Sheldon G.
, p. 692 - 698 (2004)
Lanthanide bis((cyclooctane-1,5-diyl)dihydroborate) complexes (THF) 4Ln{(μ-H)2BC8H14}2 (Ln = Eu, 1; Yb, 2) were synthesized by a metathesis reaction between (THF) xLnCl2 and K[H2BC8H14] in THF in a 1:2 molar ratio. Attempts to prepare the monosubstituted lanthanide cyclic organohydroborates (THF)xLnCl{(μ-H)2BC 8H14} were unsuccessful. On the basis of the molecular structure and IR spectrum of 1, there is an agostic interaction between Eu(II) and one of the α-C-H hydrogens from the {(μ-H)2BC 8H14} unit. No such interaction was observed for 2. The coordinated THF in 1 and 2 can be removed under dynamic vacuum, but the solvent ligands remain bound to Yb when 2 is directly dissolved in Et2O or toluene. In strong Lewis basic solvents, such as pyridine or CH3CN, attack of the Yb-H-B bridge bonds results. Decomposition of 2 to the 9-BBN dimer in CD2Cl2 was observed by 11B and 1H NMR spectroscopies. Compound 2 was reacted with 2 equiv of the hydride ion abstracting reagent B(C6F5)3 to afford the solvent-separated ion pair [Yb(THF)6][HB(C 6F5)3]2 (3). Complexes 1, 2, and 3 were characterized by single-crystal X-ray diffraction analysis. Crystal data: 1 is orthorhombic, Pna21, a = 21.975(1) A, b = 9.310(1) A, c = 16.816(1) A, Z = 4; 2 is triclinic, P1, a = 9.862(1) A, b = 10.227(1) A, c = 10.476(1) A, α = 69.87(1)°, β = 76.63(1)°, γ = 66.12(1)°, γ = 1; 3.Et2O is triclinic, P1, a = 13.708(1) A, b =14.946(1) A, c = 17.177(1) A, α = 81.01(1)°, β = 88.32(1)°, γ = 88.54(1)°, Z = 2.
Braun et al.
, p. 2388 (1971)
Brown et al.
, p. 7765,7768 (1974)
Synthesis and x-ray and neutron structures of Zr{(μ-H) 2BC8H14}4
Ding, Errun,Du, Bin,Meyers, Edward A.,Shore, Sheldon G.,Yousufuddin, Muhammed,Bau, Robert,McIntyre, Garry J.
, p. 2459 - 2464 (2005)
The complex Zr(9-BBN)4 [9-BBN = (μ-H)2BC 8H14] has been synthesized via the reaction of K(9-BBN) with ZrCl4 in diethyl ether. The structure of the title compound has been determined by X-ray and neutron single-crystal diffraction techniques. Each 9-BBN ligand is coordinated to the Zr atom via two B-H-Zr bridges, and these metal-ligand bonding interactions are further augmented by three prominent C-H...Zr agostic interactions. Average molecular parameters derived from the neutron analysis: Zr-H = 2.051(8) A, B-H = 1.286(7) A, Zr...B = 2.409(6) A, Zr-H-B = 87.7(4)°, H-Zr-H = 58.9(3)°. The Zr...H distances corresponding to the three C-H...Zr agostic interactions are 2.424(7), 2.663(8), and 2.551(7) A. The fourth potential C-H...Zr interaction has a Zr...H distance [3.146(7) A] that is too long to be considered in the agostic range. Single-crystal X-ray diffraction data were collected on an Enraf-Nonius Kappa CCD diffraction system, and neutron diffraction data were collected on the quasi-Laue diffractometer VIVALDI at the Institut Laue-Langevin; the final agreement factor for the neutron analysis is 6.52% for 2557 reflections with I > 2σ(I).
9 - boron bicyclo [3.3.1] nonane dimer synthesis method
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Paragraph 0040, (2017/02/09)
The invention relates to a synthesis method of a 9-borabicyclo[3.3.1]nonane dimer. The synthesis method is used for synthesizing the 9-borabicyclo[3.3.1]nonane dimer by performing a hydroboration reaction on a hydroboron, an oxidizing agent and 1,5-cyclooctadiene as the raw materials in a solvent selected from ethers, aromatic hydrocarbons, aliphatic hydrocarbons and the like under the protection of an inert gas. The synthesis method is simple and convenient to operate, mild in conditions, low in cost, high in product yield and product purity, and suitable for certain scale industrial production.
Tris(2,6-diisopropylphenolato)titanium(IV) dihydridodiorganylborates: Synthesis and structures
Knizek, Joerg,Noeth, Heinrich
, p. 1888 - 1900 (2011/06/26)
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-iPr 2C6H3O)3Ti(H2BR 2) 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)3TiH 2BC8H14 and the corresponding titanium dihydridobis(cyclohexyl)borate.