Synthesis and Characterization of 3-Chloropropyl-substituted o- Carboranes: Crystal Structures of 1,2-(1,3-Propanediyl)-o-carborane, 1-(3-Chloropropyl)-o-carborane and 1,2-Bis(3-chloropropyl)-ocarborane

2013 ◽  
Vol 68 (7) ◽  
pp. 804-810 ◽  
Author(s):  
Deqian Bian ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Ping Lu
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Main Product ◽  
Total Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reactions of the lithio-o-carborane Li2C2B10H10 with ClCH2CH2CH2Br were studied under various conditions. While the main product is the known exo-polyhedrally cyclized 1,2- (1,3-propanediyl)-o-carborane (2), the expected 3-chloropropyl-substituted carborane products 1- (ClCH2CH2CH2)C2B10H11 (3) and 1,2-(ClCH2CH2CH2)2C2B10H10 (4) can be obtained in a total yield of 22%. In the presence of CuCl, the same reaction proceeded rather slowly and gave compound 3and bis(o-carborane) (5) in small yields, with the recovery of the starting o-C2B10H12. Compounds 2- 4were characterized by means of IR and NMR spectroscopy and mass spectrometry, as well as by single-crystal X-ray diffraction.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

Incremental iodination of the eight-vertex closo monocarborane anion [closo-1-CB7H8]–: Preparation and characterization of [closo-1-CB7H5-6,7,8-I3]– and [closo-1-CB7H2-2,3,4,6,7,8-I6]–, and the synthesis of the first eight-vertex C-methylated carborane anion [1-CH3-closo-1-CB7H4-6,7,8-I3]–

2010 ◽  
Vol 75 (9) ◽  
pp. 931-947 ◽  
Author(s):  
Radim Dostál ◽  
Michael G. S. Londesborough ◽  
Magdalena Kvíčalová ◽  
Jan Macháček ◽  
Ivana Císařová ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Electrophilic Substitution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Behavior ◽  
Elemental Iodine ◽  
Insight Into

Iodination of [closo-1-CB7H8]– (anion 1) with elemental iodine under various controlled conditions yields a continuum from mono- to hexaiodinated derivatives including the previously unknown [closo-1-CB7H5-6,7,8-I3]– (anion 5) and [closo-1-CB7H2-2,3,4,6,7,8-I6]– (anion 8). These species, characterized by mass spectrometry and NMR spectroscopy, and, in the case of 8, by single-crystal X-ray diffraction, provide insight into the fluxional molecular behavior of anion 1 in solution. Investigation of direct electrophilic substitution on the carbon-vertex of anion 1 using standard conditions and reagents (deprotonation by BuLi followed by addition of electrophile) proved futile, but the same conditions when using the new triiodo-deravitive anion 5 resulted in the formation of the first eight-vertex C-methylated carborane anion [1-CH3-closo-1-CB7H4-6,7,8-I3]– (anion 9), in 60% yield.

Synthesis and Characterization of o-Carboranylthioether Derivatives

2011 ◽  
Vol 66 (9) ◽  
pp. 947-952
Author(s):  
Meiling Xu ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Bin Peng ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Single Crystal ◽  
Uv Light ◽  
Chloroform Solution ◽  
Alkyl Halides ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

The reactions of the dithiolato-o-carborane salt (Et3NH)2(S2C2B10H10) (2) with alkyl halides BrCH2CH=CH2, BrCH2CH2CH2Cl and C6H5CH2Cl, afford the o-carboranyl-bisthioether derivatives 3a - c, which have been characterized by IR and NMR (1H, 13C, 11B) spectroscopy, mass spectrometry, and single-crystal X-ray diffraction (3c). The photoluminescent properties of the known compound 3c has been investigated. It exhibits a violet (chloroform solution) or blue (solid state) emission when excited with UV light.

Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

Synthesis and characterization of Cu(II)-halide 1-methylimidazole complexes

2016 ◽  
Vol 71 (2) ◽  
pp. 105-112 ◽  
Author(s):  
Michael Hörmannsdorfer ◽  
Ulrike Kahl ◽  
Tom Nilges
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Thermal Analyses ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

AbstractThree new complexes of Cu(II) halides (Cl, Br) with 1-methylimidazole (MIm), [Cu(MIm)4]Br2 (1), [Cu(MIm)4Br]Br · H2O (2), and [Cu(MIm)6]Cl2 · 2H2O (3) have been synthesized in ethanol. Their crystal structures have been determined by single-crystal X-ray diffraction. FT-IR spectroscopy, mass spectrometry, and thermal analyses were applied to characterize the compounds.

Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter
Keyword(s):  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

Synthesis and characterization of the pentazolate anion cyclo-N5ˉ in (N5)6(H3O)3(NH4)4Cl

Science ◽  
2017 ◽  
Vol 355 (6323) ◽  
pp. 374-376 ◽  
Author(s):  
Chong Zhang ◽  
Chengguo Sun ◽  
Bingcheng Hu ◽  
Chuanming Yu ◽  
Ming Lu
Keyword(s):  
Thermal Analysis ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Decomposition Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Onset Decomposition Temperature ◽  
The Stability

Pentazole (HN5), an unstable molecular ring comprising five nitrogen atoms, has been of great interest to researchers for the better part of a century. We report the synthesis and characterization of the pentazolate anion stabilized in a (N5)6(H3O)3(NH4)4Cl salt. The anion was generated by direct cleavage of the C–N bond in a multisubstituted arylpentazole using m-chloroperbenzoic acid and ferrous bisglycinate. The structure was confirmed by single-crystal x-ray diffraction analysis, which highlighted stabilization of the cyclo-N5ˉ ring by chloride, ammonium, and hydronium. Thermal analysis indicated the stability of the salt below 117°C on the basis of thermogravimetry-measured onset decomposition temperature.

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