Formation and decomposition of the Sb(III)/Li cage [{Sb(P-t-Bu)3}2Li6·6THF]

2002 ◽  
Vol 80 (11) ◽  
pp. 1421-1427 ◽  
Author(s):  
Alan Bashall ◽  
Felipe García ◽  
Gavin T Lawson ◽  
Mary McPartlin ◽  
Alexander Rothenberger ◽  
...  
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Initial Formation ◽  
X Ray ◽  
Cage Complex ◽  
Reaction Solution

The heterometallic Sb(III)/Li cage complex [{Sb(P-t-Bu)3}2Li6·6THF] (1) is obtained by the low-temperature (<0°C) reaction of Sb(NMe2)3 with t-BuPHLi (1:3 equiv) in THF. Thermolysis of this reaction solution leads to the formation of the bicyclic distibane [(t-BuP)3Sb]2 (2). 31P NMR spectroscopic studies reveal that this process involves initial formation of [(t-BuP)3Sb]– and [t-Bu(H)PP-t-Bu]– anions. Complexes 1 and 2 have been characterized in the solid state by X-ray diffraction studies.Key words: antimony, lithium, cage.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.

Ni/GeSn solid-state reaction monitored by combined X-ray diffraction analyses: focus on the Ni-rich phase

2018 ◽  
Vol 51 (4) ◽  
pp. 1133-1140 ◽  
Author(s):  
Andrea Quintero ◽  
Patrice Gergaud ◽  
Joris Aubin ◽  
Jean-Michel Hartmann ◽  
Vincent Reboud ◽  
...  
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Solid State Reaction ◽  
Metastable Phase ◽  
Hexagonal Structure ◽  
X Ray Diffraction ◽  
Rich Phase ◽  
X Ray ◽  
Pole Figures

The Ni/Ge0.9Sn0.1 solid-state reaction was monitored by combining in situ X-ray diffraction, in-plane reciprocal space map measurements and in-plane pole figures. A sequential growth was shown, in which the first phase formed was an Ni-rich phase. Then, at 518 K, the mono-stanogermanide phase Ni(Ge0.9Sn0.1) was observed. This phase was stable up to 873 K. Special attention has been given to the nature and the crystallographic orientation of the Ni-rich phase obtained at low temperature. It is demonstrated, with in-plane pole figure measurements and simulation, that it was the ∊-Ni5(Ge0.9Sn0.1)3 metastable phase with a hexagonal structure.

Preparative and Vibrational Spectroscopic Studies of Anilinium Salts Containing the [Hg2Cl6]2-, [Hg2Cl4X2]2-, [CdHgI6]2-, [CdHgI4Br2]2- and [CdHgBr4I2]2- Ions (X = Br, I)

1991 ◽  
Vol 46 (11) ◽  
pp. 1532-1538 ◽  
Author(s):  
Theodoros F. Zafiropoulos ◽  
John C. Plakatouras ◽  
S. P. Perlepes
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Raman Spectra ◽  
Spectroscopic Studies ◽  
Ir And Raman Spectra ◽  
X Ray ◽  
Ir And Raman ◽  
Complex Anions

Synthetic procedures are described that allow access to anilinium salts containing the complex anions [Hg2Cl62-, [Hg2Cl4X2]2- (X = Br, I), [CdHgI6]2-, [CdHgI4Br2]2- and [CdHgBr4I2]2--. Isolated dimeric structures are proposed for the new complexes in the solid state, using X-ray powder patterns, Far-IR and Raman spectra. The spectral detail is greatly enhanced in measurements at low temperature (∼100 K).

Low-temperature single-crystal X-Ray diffraction,1H and13C solid-state NMR and14N NQR studies of 1,8-bis(dimethyl-amino)naphthalene

1995 ◽  
Vol 91 (21) ◽  
pp. 3925-3932 ◽  
Author(s):  
Krzysztof Woźniak ◽  
Heyong He ◽  
Jacek Klinowski ◽  
Bolesław Nogaj ◽  
Dariusz Lemański ◽  
...  
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Single Crystal ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray
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