Synthesis of 12-Hydroxy and 12-Dioxane Derivatives of the closo-1-Carbadodecaborate(1-) Ion. Variations on the Plešek's Cobalt Bis(dicarbollide) Pattern

2002 ◽  
Vol 67 (7) ◽  
pp. 953-964 ◽  
Author(s):  
Bohumír Grüner ◽  
Ivana Císařová ◽  
Josef Čáslavský ◽  
Bernard Bonnetot ◽  
David Cornu
Keyword(s):  
Molecular Structure ◽  
High Field ◽  
Dimethyl Sulfate ◽  
High Yield ◽  
X Ray Diffraction ◽  
Melting Points ◽  
X Ray ◽  
Derivatives Of ◽  
Moderate Yield ◽  
Dioxane Ring

Synthesis of two new B(12) substituted derivatives of the closo-[1-CB11H12]- anion (1) is reported. The zwitterionic derivative containing dioxane ring {12-[O(CH2CH2)2O]+-1-CB11H11-}0 (2) was obtained in moderate yield using reaction of anion 1 with dioxane as solvent, induced by dimethyl sulfate. The anion [12-(HO)-1-CB11H11]- (3) was obtained in high yield upon treatment of the parent anion with 80% H2SO4 at high temperature. Both compounds containing reactive functionalities were designed to serve as useful synthons for a variety of synthetic purposes. The compounds were characterized by 11B and 1H high-field NMR, IR spectroscopy, mass spectrometry, melting points and TLC. Molecular structure of compound 2 was determined by single crystal X-ray diffraction analysis.

The Meisenheimer Rearrangement in Heterocyclic Synthesis. IV. Derivatives of the 2H,6H-1,5,4-Benzodioxazocine and 7H-1,6,5-Benzodioxazonine Ring Systems: X-Ray Crystal Structure of 10-Methoxy-5-methyl-7-phenyl-2,3,4,5-tetrahydro-7H-1,6,5-benzodioxazonine

1988 ◽  
Vol 41 (3) ◽  
pp. 293 ◽  
Author(s):  
JB Bremner ◽  
EJ Browne ◽  
LM Engelhardt ◽  
IWK Gunawardana ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Ring System ◽  
Heterocyclic Synthesis ◽  
Rearrangement Product ◽  
Ring Systems ◽  
X Ray ◽  
Derivatives Of ◽  
Moderate Yield

Meisenheimer rearrangement of the N-oxides (4) derived from a series of 5-aryl-4-methyl-2,3,4,5-tetrahydro-1,4-benzoxazepines (3) gave rise to eight derivatives (5) of the new 2H,6H-1,5,4-benzodioxazocine ring system. Reaction of 9-methoxy-5-methyl-6-phenyl-3,4,5,6- tetrahydro-2H-1,5-benzoxazocine (6) with 3-chloroperoxybenzoic acid gave an unstable N-oxide (7). A Meisenheimer rearrangement product from (7), 10-methoxy-5-methyl-7-phenyl-2,3,4,5-tetrahydro-7 H-1,6,5- benzodioxazonine (8), the first example of this ring system, was isolated directly in moderate yield on oxidation of (6) with cooling. The crystal and molecular structure of (8) has been determined by X-ray crystallographic methods.

ChemInform Abstract: Crystal and Molecular Structure of Methylsulfinyl Derivatives of Furan and Thiophene by X-Ray Diffraction.

ChemInform ◽  
2010 ◽  
Vol 22 (37) ◽  
pp. no-no
Author(s):  
U. FOLLI ◽  
D. IAROSSI ◽  
A. MUCCI ◽  
A. MUSATTI ◽  
M. NARDELLI ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Derivatives Of

Crystal and molecular structure of methylsulphinyl derivatives of furan and thiophene by X-ray diffraction

1991 ◽  
Vol 246 (1-2) ◽  
pp. 99-111 ◽  
Author(s):  
Ugo Folli ◽  
Dario Iarossi ◽  
Adele Mucci ◽  
Amos Musatti ◽  
Mario Nardelli ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Derivatives Of

Derivatives of the Triaminoguanidinium Ion, 2. Prototropic Tautomerism, Crystal and Molecular Structure of N,N´,N´´-Tris(propan- 2-iminyl)guanidine [1, 2]

2013 ◽  
Vol 68 (3) ◽  
pp. 207-213 ◽  
Author(s):  
Jan Szabo ◽  
Gerhard Maas
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Prototropic Tautomerism ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray ◽  
H Nmr ◽  
Compound C ◽  
Crystallographic Symmetry ◽  
Derivatives Of

The title compound, C10H20N6 (2), was prepared from N,N´,N´´-triaminoguanidinium chloride. Solvent- and temperature-dependent 1H NMR spectra indicating prototropic tautomerism were observed in solution. The crystal and molecular structure was determined by X-ray diffraction analysis. The compound crystallizes in the hexagonal space group P63/m. The molecules lie on crystallographic mirror planes parallel to the a,b plane, which are separated from each other by 3:37 Å . The threefold crystallographic symmetry of the molecules is due to disorder with positional averaging of individual molecules.

Synthesis, Infrared and X-Ray Studies of Diphenyltellurium(IV) Nitrosocarbamylcyanmethanides. X-Ray Evidence for Stability of a Tritelluroxane Fragment -Ph2Te-O-Ph2Te-O-Ph2Te-

1996 ◽  
Vol 51 (6) ◽  
pp. 832-837 ◽  
Author(s):  
Konstantin V. Domasevitch ◽  
Victor V. Skopenko ◽  
Eduard B. Rusanov
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Spectroscopic Data ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Nitroso Group ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic ◽  
Derivatives Of

Abstract Diphenyltellurium(IV) derivatives of the types Ph2Te{ACO}2 (1), Ph4Te2O{ACO}2 (2) and Ph6Te3O2{ACO} (3) (ACO = nitrosocarbamylcyanmethanide -ONC(CN)C(O)NH2) have been prepared. The IR spectroscopic data reveal that the ambidentate ligands are coordinated to the tellurium(IV) atom in a monodentate manner via the nitroso oxygen atom. The crystal and molecular structure of 3 has been determined from X-ray diffraction data (triclinic, space group P1̅ with a = 12.382(2), 6=13.100(2), c = 14.944(3) Å, a = 87.74( 1), β = 85.04(2), 7 = 66.29( 1)°, V = 2211.0 A , Z = 2, R = 0.040). The structure is made up of unsymmetric molecules, in which the tellurium atoms are linked by oxo bridges to form chains Te-O-Te-O-Te (d(Te-O) ca. 1.94-2.09 A). The Te-0 (nitroso group) bond lengths are in the range 2.33 - 2.36 Å

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

scholarly journals Synthesis of Bis(Carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) and Attempt of Synthesis of Gadolinium Bis(Dicarbollide)

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1321
Author(s):  
Yasunobu Asawa ◽  
Aleksandra V. Arsent’eva ◽  
Sergey A. Anufriev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
X Ray Diffraction ◽  
Stable Conformation ◽  
Acyl Chlorides ◽  
X Ray ◽  
Cesium Fluoride ◽  
The Stability

Bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) were prepared by the reactions of the corresponding carboranyl acyl chlorides with ethylenediamine. Crystal molecular structure of 1,1′-μ-(CH2NH(O)C-1,2-C2B10H11)2 was determined by single crystal X-ray diffraction. Treatment of bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 with ammonium or cesium fluoride results in partial deboronation of the ortho-carborane cages to the nido-carborane ones with formation of [7,7′(8′)-μ-(CH2NH(O)C(CH2)n-7,8-C2B9H11)2]2−. The attempted reaction of [7,7′(8′)-μ-(CH2NH(O)CCH2-7,8-C2B9H11)2]2− with GdCl3 in 1,2-dimethoxy- ethane did not give the expected metallacarborane. The stability of different conformations of Gd-containing metallacarboranes has been estimated by quantum-chemical calculations using [3,3-μ-DME-3,3′-Gd(1,2-C2B9H11)2]− as a model. It was found that in the most stable conformation the CH groups of the dicarbollide ligands are in anti,anti-orientation with respect to the DME ligand, while any rotation of the dicarbollide ligand reduces the stability of the system. This makes it possible to rationalize the design of carborane ligands for the synthesis of gadolinium metallacarboranes on their base.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

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