scholarly journals Bis(diphenylphosphino)methane Dioxide Complexes of Lanthanide Trichlorides: Synthesis, Structures and Spectroscopy

Chemistry ◽  
2020 ◽  
Vol 2 (4) ◽  
pp. 947-959
Author(s):  
Robert D. Bannister ◽  
William Levason ◽  
Gillian Reid

Bis(diphenylphosphino)methane dioxide (dppmO2) forms eight-coordinate cations [M(dppmO2)4]Cl3 (M = La, Ce, Pr, Nd, Sm, Eu, Gd) on reaction in a 4:1 molar ratio with the appropriate LnCl3 in ethanol. Similar reaction in a 3:1 ratio produced seven-coordinate [M(dppmO2)3Cl]Cl2 (M = Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb), whilst LuCl3 alone produced six-coordinate [Lu(dppmO2)2Cl2]Cl. The complexes have been characterised by IR, 1H and 31P{1H}-NMR spectroscopy. X-ray structures show that [M(dppmO2)4]Cl3 (M = Ce, Sm, Gd) contain square antiprismatic cations, whilst [M(dppmO2)3Cl]Cl2 (M = Yb, Dy, Lu) have distorted pentagonal bipyramidal structures with apical Cl. The [Lu(dppmO2)2Cl2]Cl has a cis octahedral cation. The structure of [Yb(dppmO2)3(H2O)]Cl3·dppmO2 is also reported. The change in coordination numbers and geometry along the series is driven by the decreasing lanthanide cation radii, but the chloride counter anions also play a role.

Molbank ◽  
10.3390/m1077 ◽  
2019 ◽  
Vol 2019 (3) ◽  
pp. M1077
Author(s):  
Lan ◽  
Zheng ◽  
Wang

The compound 2-(3,5-dimethyl-1H-pyrazol-1-yl)thiazolo[4,5-b]pyridine (1) was synthesized with a yield of 71% by the reaction of 1-(thiazolo[4,5-b]pyridine-2-yl)hydrazine and acetylacetone. The structure was characterized by a single-crystal X-ray structure determination as well as 1H and 13C{1H} NMR spectroscopy. X-ray crystallography on 1 confirms the molecule consists of a pyridine–thiazole moiety and the pyrazole ring, and all non-hydrogen atoms are planar.


2005 ◽  
Vol 58 (3) ◽  
pp. 199 ◽  
Author(s):  
Ethan D. Goddard-Borger ◽  
Brian W. Skelton ◽  
Robert V. Stick ◽  
Allan H. White

The use of 1H NMR spectroscopy, in tandem with X-ray crystallography, has cast light on the conformation of the 1,6-disulfide-bridged derivatives of d-gluco-, d-manno-, d-allo-, d-galacto-, and d-talo-pyranose. A similar investigation was performed on the thiosulfinate derived from the d-gluco disulfide. Single-crystal X-ray structure determinations are reported for (1S,5S,6S,7S,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, (1S,5S,6S,7R,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, and (1S,2S,5S,6S,7S,8R)-6,7,8-triacetoxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane 2-oxide.


CrystEngComm ◽  
2022 ◽  
Author(s):  
Zenghui Zhang ◽  
Rui-Lian Lin ◽  
Xiangyun Yu ◽  
Li-Xia Chen ◽  
Zhu Tao ◽  
...  

The binding interactions of cucurbit[8]uril (Q[8]) with L-Valine, D-Leucine, and D-Methionine, both in aqueous solution and solid state, have been studied by 1H NMR spectroscopy and X-ray crystallography. 1H NMR...


2007 ◽  
Vol 360 (6) ◽  
pp. 2071-2082 ◽  
Author(s):  
Antonio de Leon ◽  
Josefina Pons ◽  
Jordi García-Antón ◽  
Xavier Solans ◽  
Mercè Font-Bardia ◽  
...  

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