An approach towards the synthesis of lithium and beryllium diphenylphosphinites

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Chantsalmaa Berthold ◽  
Lewis R. Thomas-Hargreaves ◽  
Sergei I. Ivlev ◽  
Magnus R. Buchner
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Diphenylphosphine Oxide ◽  
Reaction Conditions ◽  
Solid State Structure ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy

Abstract The diphenylphosphinites [(THF)Li(OPPh2)]4 and [(THF)2Be(OPPh2)2] have been synthesized via direct deprotonation of diphenylphosphine oxide with n BuLi and BePh2, respectively, as well as via salt metathesis. These compounds were characterized by multinuclear NMR spectroscopy, and the side-products of the reactions obtained under various reaction conditions have been identified. The beryllium derivative could not be isolated and decomposed into diphosphine oxide Ph2PP(O)Ph2. The solid-state structure of this final product together with that of [(THF)Li(OPPh2)]4 have been determined by single-crystal X-ray diffraction.

Synthesis and structure of the λ 6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Isabelle Georg ◽  
Michael Bolte ◽  
Matthias Wagner ◽  
Hans-Wolfram Lerner
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

Abstract The λ 6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) was synthesized by treatment of Si2Cl6 with Cs[OSO2CH3] in the presence of 18-crown-6. Compound 1 is the first example of a λ 6Si-silicate with a methanesulfonate ligand. It was characterized by NMR spectroscopy and by single-crystal X-ray diffraction. The solid-state structure of 1 consists of discrete [Si(OSO2CH3)6]2– anions and two [Cs(18-crown-6)]+ cations (triclinic space group, P 1 ¯ $P\overline{1}$ , Z = 1).

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Synthesis of Diferrocenylethyne by Molybdenum-Catalyzed Metathesis of 1-Ferrocenylprop-1-yne

2003 ◽  
Vol 68 (10) ◽  
pp. 1897-1903 ◽  
Author(s):  
Martin Kotora ◽  
David Nečas ◽  
Petr Štěpnička
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Catalytic Systems ◽  
Solid State Structure ◽  
X Ray

Diferrocenylethyne (1) was synthesized by metathesis of 1-ferrocenylprop-1-yne using various catalytic systems based on [Mo(CO)6] (5 mole %) and a chlorophenol (30 mole %) in toluene. The yields varied for different chlorophenols; the best conversions were obtained with 2,5-dichlorophenol (66%) and 4-chlorophenol (55%). Alkyne 1 was further reduced to the known (E)-1,2-diferrocenylethene and 1,2-diferrocenylethane, and its solid-state structure determined by single-crystal X-ray diffraction.

scholarly journals Investigating Differences and Similarities between Betaxolol Polymorphs

Crystals ◽  
2019 ◽  
Vol 9 (10) ◽  
pp. 509 ◽  
Author(s):  
Patrizia Rossi ◽  
Paola Paoli ◽  
Stella Milazzo ◽  
Laura Chelazzi ◽  
Andrea Ienco ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Blocking Agent ◽  
Rotational Isomer ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Β Blocker ◽  
Adrenergic Blocking

Betaxolol belongs to the class of β1-adrenergic blocking agent. Several polymorphs of racemic betaxolol have been reported in the literature, but only one of them (BE_I) had the crystal structure determined from single-crystal X-ray diffraction. Here, we present a new crystalline phase of betaxolol (BE_IV). Its solid-state structure has been obtained from single-crystal X-ray diffraction data. The molecular and crystal arrangements of betaxolol in BE_IV have been further investigated by molecular modelling, by Cambridge Structural Database (CSD) surveys and by Hirshfeld surface analysis. A comparison with the solid-state structure of BE_I have been carried out. In the two polymorphs the 2-hydroxy-3-(isopropylamino)-propoxy chain, which is common to other β-blocker drugs, adopts a different conformation. In addition, the rotational isomer found in BE_IV is different with respect to the four already observed in the solid-state structure of analogous compounds. In both the polymorphs, the most significant interaction is due to the H-bonds involving the OH group as donor and the NH as acceptor, while the interaction where OH works as acceptor (NH acts as donor) is definitely less important. The resulting H-bond patterns are however different: Alternate R2,2(10) a > a (OH donors) and R2,2(10) b > b (OH acceptors) in BE_I vs. alternate R4,4 (8) a > b > a > b (OH donors) and R2,2 (10) b > b (OH acceptor) in BE_IV.

Phosphine chalcogenide complexes of antimony(III) halides

2015 ◽  
Vol 93 (3) ◽  
pp. 375-379 ◽  
Author(s):  
Karlee L. Bamford ◽  
Alasdair P.M. Robertson ◽  
Hilary A. Jenkins ◽  
Brian O. Patrick ◽  
Neil Burford
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Phosphine Oxide ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Derivatives Of

Three series of phosphine chalcogenide complexes of the antimony(III) halides SbX3 (X = F, Cl, Br, or I) have been synthesized and characterized by spectroscopic and crystallographic methods. Complexes of the generic formulae (Cy3PO)SbX3 (X = F (1a), Cl (1b), or Br (1c)), (Cy3PO)2SbX3 (X = F (2a), Cl (2b), or Br (2c)), and (Cy3PS)SbX3 (X = Cl (3b), Br (3c), or I (3d)) were synthesized via the treatment of solutions of SbX3 with OPCy3 and SPCy3, respectively. Derivatives of (Cy3PO)SbX3 were characterized by single crystal X-ray diffraction for 1a and 1b and crystallize as dimers through symmetry related intermolecular Sb–X interactions, providing the first structurally characterized examples of this class of complex. Derivatives of (Cy3PS)SbX3 (3b–3c) adopt analogous dimeric structures in the solid state. The solid-state structure of (Cy3PO)2SbCl3 (2b) is consistent with the previously reported structures of bis-phosphine oxide complexes of antimony(III), with a square pyramidal Sb center and cis-configured OPCy3 ligands. The phosphine chalcogenide complexes of SbX3 display configurations that are consistent with the perceived trans-labilizing properties of the ligands/substituents.

Dimesitylborane monomer-dimer equilibrium in solution, and the solid-state structure of the dimer by single crystal neutron and X-ray diffraction

2003 ◽  
Vol 680 (1-2) ◽  
pp. 165-172 ◽  
Author(s):  
Christopher D Entwistle ◽  
Todd B Marder ◽  
Philip S Smith ◽  
Judith A.K Howard ◽  
Mark A Fox ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray

Solid-State Structure and Tautomerism of 2-Aminotroponimines Studied by X-ray Crystallography and Multinuclear NMR Spectroscopy

2004 ◽  
Vol 2004 (21) ◽  
pp. 4452-4466 ◽  
Author(s):  
Rosa M. Claramunt ◽  
Dionisia Sanz ◽  
Marta Pérez-Torralba ◽  
Elena Pinilla ◽  
M. Rosario Torres ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
Multinuclear Nmr ◽  
X Ray Crystallography ◽  
Multinuclear Nmr Spectroscopy

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

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