scholarly journals Structural Chemistry of Halide including Thallides A8Tl11X1−n (A = K, Rb, Cs; X = Cl, Br; n = 0.1–0.9)

Crystals ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 319 ◽  
Author(s):  
Stefanie Gärtner ◽  
Susanne Tiefenthaler ◽  
Nikolaus Korber ◽  
Sabine Stempfhuber ◽  
Birgit Hischa
Keyword(s):  
Alkali Metal ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Moisture Sensitivity ◽  
Metal Compounds ◽  
X Ray ◽  
Extra Electron ◽  
Alkali Metal Compounds ◽  
New Compounds ◽  
Insight Into

A8Tl11 (A = alkali metal) compounds have been known since the investigations of Corbett et al. in 1995 and are still a matter of current discussions as the compound includes one extra electron referred to the charge of the Tl117− cluster. Attempts to substitute this additional electron by incorporation of a halide atom succeeded in the preparation of single crystals for the lightest triel homologue of the group, Cs8Ga11Cl, and powder diffraction experiments for the heavier homologues also suggested the formation of analogous compounds. However, X-Ray single crystal studies on A8Tl11X to prove this substitution and to provide a deeper insight into the influence on the thallide substructure have not yet been performed, probably due to severe absorption combined with air and moisture sensitivity for this class of compounds. Here, we present single crystal X-Ray structure analyses of the new compounds Cs8Tl11Cl0.8, Cs8Tl11Br0.9, Cs5Rb3Tl11Cl0.5, Cs5.7K2.3Tl11Cl0.6 and K4Rb4Tl11Cl0.1. It is shown that a (partial) incorporation of halide can also be indirectly determined by examination of the Tl-Tl distances, thereby the newly introduced cdd/cdav ratio allows to evaluate the degree of distortion of Tl117− clusters.

scholarly journals Single Crystal X-ray Structure Analyses of Thallides: Halide Incorporation and Mixed Alkali Sites in A8Tl11X (A = K, Rb, Cs; X = Cl, Br)

Proceedings ◽  
2018 ◽  
Vol 2 (14) ◽  
pp. 1124
Author(s):  
Stefanie Gärtner ◽  
Susanne Tiefenthaler
Keyword(s):  
Single Crystal ◽  
Alkali Metals ◽  
Data Sets ◽  
Moisture Sensitivity ◽  
Metal Compounds ◽  
X Ray ◽  
Mixed Alkali ◽  
Extra Electron ◽  
Alkali Metal Compounds ◽  
New Compounds

A8Tl11 (A = alkali metal) compounds have been known since the investigations of Corbett et al. in 1995 and still are matter of current discussions as the compound includes one extra electron referred to the charge of the Tl117− cluster. Attempts to substitute the charge by incorporation of a halide atom succeeded for the lightest homologue of the group, Cs8Ga11Cl, and powder diffraction experiments for the heavier homologues also suggested the formation of analogous compounds. However, X-ray single crystal studies on A8Tl11X to prove this substitution and to provide a deeper insight into the influence on the thallide substructure have not yet been performed, probably due to severe absorption combined with air and moisture sensitivity for this class of compounds. In our contribution we present single crystal X-ray analyses of the new compounds Cs8Tl11Cl0.8, Cs8Tl11Br0.9 and Cs5Rb3Tl11Cl0.5. It is shown that a (partial) incorporation of halide can also be indirectly determined by examination of the Tl-Tl distances for low resolved data sets, e.g., for Cs5.7K2.3Tl11Cl?. Mixed occupied sites by two different alkali metals indicate a dependence on the cesium content, the systems K/Rb–Tl–Br and K/Rb–Tl–Cl only gave rise to the formation of the higher reduced (K/Rb)8Tl11 and the less reduced by-product (K/Rb)15Tl27. We have not been able to prove the formation of halide including thallides in the absence of cesium.

Synthesis and Reactivity of Novel Alkali Metal Stannides

2004 ◽  
Vol 59 (11-12) ◽  
pp. 1462-1470 ◽  
Author(s):  
Thorsten Schollmeier ◽  
Ulrich Englich ◽  
Roland Fischer ◽  
Ingo Prass ◽  
Karin Ruhlandt ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Alkali Metal ◽  
Synthesis And Characterization ◽  
Metal Compounds ◽  
X Ray ◽  
X Ray Crystallography ◽  
Multinuclear Nmr Spectroscopy ◽  
Alkali Metal Compounds ◽  
Potassium Hydride

Reactivity and side products of reactions of diorganodihydridostannanes (R2SnH2, R = Me, nBu, tBu)) with various alkali metal compounds have been discussed. Alternatively, the synthesis and characterization of a family of novel potassium stannides are described as well. The compounds of type (RR’2Si)R”2SnK (R, R’= Me, Ph; R”= , Me, tBu, Ph) 4 - 9 were synthesized by reaction of potassium hydride with bis(silyl)stannides ((RR’2Si)2SnR”2). All compounds were characterized by multinuclear NMR spectroscopy. In addition, the tri-tert-butyltin compound 3 (LiSntBu3) and the unsymmetrical silyl substituted stannane 10 were characterized by X-ray crystallography.

New results on the x-ray structure of trans-(CH) x and its alkali metal compounds

1991 ◽  
Vol 41 (1-2) ◽  
pp. 33-38 ◽  
Author(s):  
J.E. Fischer ◽  
P.A. Heiney ◽  
J. Ma
Keyword(s):  
Alkali Metal ◽  
Metal Compounds ◽  
X Ray ◽  
Alkali Metal Compounds

About alkali metal dicyanamides: syntheses, single-crystal structure determination, DSC/TG and vibrational spectra of KCs[N(CN)2]2 and NaRb2[N(CN)2]3 · H2O

2015 ◽  
Vol 70 (6) ◽  
pp. 365-372 ◽  
Author(s):  
Olaf Reckeweg ◽  
Ryo H. Wakabayashi ◽  
Francis J. DiSalvo ◽  
Armin Schulz ◽  
Christof Schneck ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

AbstractTransparent colorless crystals of KCs[N(CN)2]2 and NaRb2[N(CN)2]3 · H2O were obtained by blending aqueous solutions of Na[N(CN)2] and RbF or KF, respectively. After evaporation of the water, the remaining solid was extracted with absolute ethanol and the solvent was allowed to evaporate at r. t.. KCs[N(CN)2]2 crystallizes in the space group C2/c (no. 15) with the cell parameters a = 1382.7(2), b = 998.1(1) and c = 1455.4(2) pm, and β = 118.085(4) °. The structure of NaRb2[N(CN)2]3 · H2O is exhibiting the space group P63/m (no. 176) with the cell parameters a = 705.98(7) and c = 1462.89(12) pm. Single-crystalline α-K[N(CN)2] was obtained while attempting to synthesize ‘NaK2[N(CN)2]3’, corroborating the results of previous X-ray powder diffraction experiments. Vibrational spectra and DSC/TGA analyses complete our results.

The crystal structures of solvent-free alkali-metal squarates from powder diffraction data

2005 ◽  
Vol 220 (11) ◽  
Author(s):  
Robert E. Dinnebier ◽  
Hanne Nuss ◽  
Martin Jansen
Keyword(s):  
High Resolution ◽  
Alkali Metal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Room Temperature ◽  
Solvent Free ◽  
Crystallographic Data ◽  
Powder Diffraction Data ◽  
X Ray

AbstractThe crystal structures of solvent-free lithium, sodium, rubidium, and cesium squarates have been determined from high resolution synchrotron and X-ray laboratory powder patterns. Crystallographic data at room temperature of Li

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