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Orphenadrinium dihydrogen citrate.

ABSTRACT: In the title salt, C(18)H(24)NO(+)·C(6)H(7)O(7) (-), the dihedral angle between the benzene rings in the cation is 74.2?(5)°. In the crystal, anion-anion O-H?O hydrogen bonds and weak O-H?O inter-actions form infinite chains along [100]. Between these chains, cation-anion N-H-O hydrogen bonds are observed, forming an alternate pattern of cation and anion layers and leading to a two-dimensional network parallel to (100).

SUBMITTER: Kaur M

PROVIDER: S-EPMC3569781 | biostudies-literature | 2013 Feb

REPOSITORIES: biostudies-literature

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Orphenadrinium dihydrogen citrate.

Kaur Manpreet M Jasinski Jerry P JP Keeley Amanda C AC Yathirajan H S HS Siddaraju B P BP

Acta crystallographica. Section E, Structure reports online 20130119 Pt 2

In the title salt, C(18)H(24)NO(+)·C(6)H(7)O(7) (-), the dihedral angle between the benzene rings in the cation is 74.2 (5)°. In the crystal, anion-anion O-H⋯O hydrogen bonds and weak O-H⋯O inter-actions form infinite chains along [100]. Between these chains, cation-anion N-H-O hydrogen bonds are observed, forming an alternate pattern of cation and anion layers and leading to a two-dimensional network parallel to (100). ...[more]

PMID: 23424527

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Project description:The titanocene sulfido complex Cp*(2)Ti(S)py (1, Cp* = pentamethylcyclopentadienyl; py = pyridine) is synthesized by addition of a suspension of S(8) to a toluene solution of Cp*(2)Ti-(CH(2)CH(2)) (2) and py. The rate of rotation of the pyridine ligand in solution was determined by (1)H NMR spectroscopy, and the structure of 1 was determined by X-ray crystallography. Complex 1 reacts reversibly with dihydrogen to give Cp*(2)Ti(H)SH (6) and py. Reaction of 1 with HD gives an equilibrium mixture of Cp*(2)Ti(D)SH and Cp*(2)Ti(H)SD; H(2) and D(2) are not formed in this reaction. 1D (1)H NMR magnetization transfer spectra and 2D EXSY (1)H NMR spectra of 6 in the presence of H(2) show that in solution the H(2), hydride, and hydrosulfido hydrogen atoms exchange. A four-center mechanism for this exchange is proposed. The EXSY studies show that the Ti-H and S-H hydrogens exchange with each other more rapidly than either of those hydrogens exchanges with external H(2). A transient dihydrogen complex intermediate is proposed to explain this observation. The infrared spectrum of 6 shows an absorption assigned to the Ti-H stretching mode at 1591 cm(-1) that shifts upon deuteration to 1154 cm(-1). Reaction of 1 with trimethylsilane, diethylsilane, or dimethylsilane gives Cp*(2)-Ti(H)SSiMe(3) (7), Cp*(2)Ti(H)SSiHEt(2) (8), or Cp*(2)Ti(H)SSiHMe(2) (9), respectively. The isotope effect for the reaction producing 7 has been measured, and a mechanism is proposed. Treatment of 1 with an additional equivalent of S(8) results in the formation of the disulfide Cp*(2)Ti(S(2)) (4). Acetylene inserts into the Ti-S bond of 4 to produce the vinyl disulfide complex 5. The structures of 4 and 5 have been determined by X-ray diffraction. Compound 4 reacts with 2 in the presence of py to produce 1. Phosphines react with 4 in the presence of H(2) to provide 6 and the corresponding phosphine sulfide. Reaction of hydrogen with 4 gives Cp*(2)-Ti(SH)(2) (3). The reactions of 1 and 4 with dihydrogen provide a model for possible mechanisms of H(2) activation by metal-sulfide hydrodesulfurization catalysts.

Dataset Information

Orphenadrinium dihydrogen citrate.

Publications

Orphenadrinium dihydrogen citrate.

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