Tris(pyrazolyl)borate Copper Hydroxide Complexes Featuring Tunable Intramolecular H-bonding

Author(s):  
Evan Gardner ◽  
Caitlyn Cobb ◽  
Jeffery A. Bertke ◽  
Timothy H. Warren

A modular synthesis provides access to a series of new tris(pyrazolyl)borate ligands <sup>XpyMe</sup>TpK that possess a single functionalized pendant pyridyl (py) or pyrimidyl (pyd) arm designed to engage in tunable intramolecular H-bonding to metal–bound functionalities. To illustrate such H-bonding interactions, a series of [<sup>XpyMe</sup>TpCu]<sub>2</sub>(𝜇–OH)<sub>2</sub>(<b>6a</b><b>–6e</b>) complexes were synthesized from the corresponding <sup>XpyMe</sup>TpCu–OAc (<b>5a–5e</b>) complexes. Single crystal X-ray structures of three new dinuclear [<sup>XpyMe</sup>TpCu]<sub>2</sub>(𝜇–OH)<sub>2</sub>complexes reveal H-bonding between the pendant heterocycle and bridging hydroxide ligands while the donor arm engages the copper center in an unusual monomeric <sup>DMAPMe</sup>TpCu–OH complex. Vibrational studies (IR) of each bridging hydroxide complex reveal reduced 𝜈<sub>OH </sub>frequencies that tracks with the H-bond accepting ability of the pendant arm.

2019 ◽  
Author(s):  
Evan Gardner ◽  
Caitlyn Cobb ◽  
Jeffery A. Bertke ◽  
Timothy H. Warren

A modular synthesis provides access to a series of new tris(pyrazolyl)borate ligands <sup>XpyMe</sup>TpK that possess a single functionalized pendant pyridyl (py) or pyrimidyl (pyd) arm designed to engage in tunable intramolecular H-bonding to metal–bound functionalities. To illustrate such H-bonding interactions, a series of [<sup>XpyMe</sup>TpCu]<sub>2</sub>(𝜇–OH)<sub>2</sub>(<b>6a</b><b>–6e</b>) complexes were synthesized from the corresponding <sup>XpyMe</sup>TpCu–OAc (<b>5a–5e</b>) complexes. Single crystal X-ray structures of three new dinuclear [<sup>XpyMe</sup>TpCu]<sub>2</sub>(𝜇–OH)<sub>2</sub>complexes reveal H-bonding between the pendant heterocycle and bridging hydroxide ligands while the donor arm engages the copper center in an unusual monomeric <sup>DMAPMe</sup>TpCu–OH complex. Vibrational studies (IR) of each bridging hydroxide complex reveal reduced 𝜈<sub>OH </sub>frequencies that tracks with the H-bond accepting ability of the pendant arm.


Author(s):  
J. M. Galbraith ◽  
L. E. Murr ◽  
A. L. Stevens

Uniaxial compression tests and hydrostatic tests at pressures up to 27 kbars have been performed to determine operating slip systems in single crystal and polycrystal1ine beryllium. A recent study has been made of wave propagation in single crystal beryllium by shock loading to selectively activate various slip systems, and this has been followed by a study of wave propagation and spallation in textured, polycrystal1ine beryllium. An alteration in the X-ray diffraction pattern has been noted after shock loading, but this alteration has not yet been correlated with any structural change occurring during shock loading of polycrystal1ine beryllium.This study is being conducted in an effort to characterize the effects of shock loading on textured, polycrystal1ine beryllium. Samples were fabricated from a billet of Kawecki-Berylco hot pressed HP-10 beryllium.


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


2019 ◽  
Author(s):  
Swaraj Sengupta ◽  
Sahanwaj Khan ◽  
Shyamal K. Chattopadhyay ◽  
Indrani Banerjee ◽  
Tarun K. Panda ◽  
...  

Synthesis and characterisation of one trinuclear copper complex, ([Cu<sub>3</sub>L<sub>3</sub>O]ClO<sub>4</sub>) (<b>1</b>) and one nickel complex ([Ni(L'H)<sub>2</sub>(dmso)<sub>2</sub>](ClO<sub>4</sub>)<sub>2</sub>) (<b>2</b>) with Schiff base ligands: (3Z)-3-((Z)-(1-(thiophen-2-yl)ethylidene)hydrazono)butan-2-one oxime (LH) and 1-(pyridin-2-yl)ethylidene)hydrazono)butan-2-one oxime (L<sup>'</sup>H). <b>1</b> shows high catecholase activity and has also been tested as a catalyst for the synthesis of benzylimine. <b>2 </b> shows phenoxazinone synthase activity.


Sign in / Sign up

Export Citation Format

Share Document