ChemInform Abstract: Enhanced Nucleophilicity of Tris-(2,6-dimethoxyphenyl)bismuthane as Studied by X-Ray Crystallography, 17O NMR Spectroscopy and Theoretical Calculations. X-Ray Molecular Structure of Tris-(2,6-dimethoxyphenyl) bismuthane and of Trimesi

ChemInform ◽  
2010 ◽  
Vol 26 (20) ◽  
pp. no-no
Author(s):  
T. OGAWA ◽  
T. IKEGAMI ◽  
T. HIKASA ◽  
N. ONO ◽  
H. SUZUKI
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Theoretical Calculations ◽  
17O Nmr ◽  
X Ray ◽  
X Ray Crystallography ◽  
17O Nmr Spectroscopy

Molecular structure and dynamics of C-1-adamantyl substituted N-unsubstituted pyrazoles studied by solid state NMR spectroscopy and X-ray crystallography

1997 ◽  
pp. 1867-1876 ◽  
Author(s):  
Rosa María Claramunt ◽  
María Dolores Santa María ◽  
Isabelle Forfar ◽  
Francisco Aguilar-Parrilla ◽  
María Minguet-Bonvehí ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
X Ray ◽  
Solid State Nmr Spectroscopy ◽  
X Ray Crystallography ◽  
Structure And Dynamics

Atropisomerism and conformational aspects of meso-tetraarylporphyrins and related compounds

2011 ◽  
Vol 15 (01) ◽  
pp. 1-28 ◽  
Author(s):  
Augusto C. Tomé ◽  
Artur M.S. Silva ◽  
Ibon Alkorta ◽  
José Elguero
Keyword(s):  
Nmr Spectroscopy ◽  
Theoretical Calculations ◽  
Comprehensive Description ◽  
Aryl Ring ◽  
X Ray ◽  
Conformationally Restricted ◽  
X Ray Crystallography ◽  
Picket Fence ◽  
Related Compounds

This review provides a comprehensive description of the atropisomerism of meso-di- and tetraarylporphyrins with substituents in ortho-positions of the aryl ring, as well as in corroles and in conveniently substituted phthalocyanines. Different methods of study were examined: X-ray crystallography, NMR spectroscopy (both static and dynamic aspects), classical kinetics, HPLC and theoretical calculations. Then the four atropisomers, the tautomerism of the inner protons, the 'picket fence' concept, conformationally restricted meso-tetraarylporphyrins and the influence of the metal on the conformation were discussed based on 250 references.

Coordination Behavior of tBu2PH towards [{Rh(μ-Cl)(coe)2}2] (coe = cis-cyclooctene): Crystal and Molecular Structure of [{Rh(μ-Cl)(tBu2PH)2}2]

2008 ◽  
Vol 63 (9) ◽  
pp. 1035-1039 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Crystal And Molecular Structure ◽  
Molar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Molar Ratios ◽  
H Nmr ◽  
Coordination Behavior ◽  
Independent Synthesis

The reaction of [{Rh(μ-Cl)(coe)2}2] (coe = cis-cyclooctene) with tBu2PH in different solvents in various molar ratios was investigated. Working with a molar ratio of Rh to P = 1 : 2 in heptane overnight afforded [{Rh(μ-Cl)(tBu2PH)2}2] (1) in nearly quantitative yield. Upon tuning the molar ratio (Rh/P) in the range from 1 : 2 to 1 : 0.5, 31P{1H} NMR spectroscopy indicated the formation of [(tBu2PH)2Rh(μ-Cl)2Rh(coe)2] (3) besides the complexes [{Rh(μ-Cl)(coe)(tBu2PH)}2] (cis, 2a; trans, 2b). The constitution of 3 was established by an independent synthesis mixing 1 with [{Rh(μ- Cl)(coe)2}2] or [{Rh(μ-Cl)(cod)}2] (cod = 1.4-cyclooctadiene), respectively, which also yielded [(tBu2PH)2Rh(μ-Cl)2Rh(cod)] (4). Single crystals of 1 have been analyzed by X-ray crystallography (monoclinic, Cc, Z = 8, a = 32.7375(3), b = 11.1294(1), c = 24.5134(3)Å ; β = 106.7228(4)◦; V = 8553.70(15) Å3; T = 200 (2) K).

Bis(di-tert-butylphosphino)ethan-nickel(0)-Komplexe / Bis(di-tert-butylphosphino)ethane-nickel(0) Complexes

1993 ◽  
Vol 48 (5) ◽  
pp. 608-626 ◽  
Author(s):  
Klaus-Richard Pörschke ◽  
Christian Pluta ◽  
Bernd Proft ◽  
Frank Lutz ◽  
Carl Krüger
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
Screw Axis ◽  
Open Chain ◽  
X Ray ◽  
X Ray Crystallography ◽  
Rapid Exchange ◽  
Displacement Reactions ◽  
Diene Ligands

Ni(cdt) reacts with tBu2Bu2PC2H4P4P'Bu2 in pentane at 20°C to yield brownish crystals of (tBu2Bu2PC2H4P4P'Bu2)Ni(η2-C12H18) (1). The molecular structure of 1, as established by X-ray crystallography, exhibits a trigonal-planar coordination geometry of the nickel center with a η2bonded cdt ligand. In the crystal 1 exists as two enantiomers, which are determined by the leftor right-handed screw axis of the cdt ligand. The cdt ligand in 1 resists most typical displacement reactions but 1 reacts with CO at – 78°C to afford the colorless 18e complex (tBu2Bu2PC2H4P4P'Bu2)Ni(CO)2 (2). From the reaction of Ni(cod)2 with tBu2Bu2PC2H4P4P'Bu2 yellow needles of (tBu2Bu2PC2H4P4P'Bu2)Ni(η2-cod) (3) are obtained. Low temperature NMR spectroscopy established that only one diene C=C bond is coordinated to nickel(0). At higher temperatures a rapid exchange of the coordinated and unbound C=C bonds is induced. When solutions of 3 are kept at 20°C for several days the dinuclear, almost insoluble yellow complex {(tBu2PC2H4P4P'Bu2)Ni}2(μ-η2,η2-cod) (4) precipitates. The reaction of Ni(C2H4)3 and tBu2Bu2PC2H4P4P'Bu2 affords orange (tBu2Bu2PC2H4P4P'Bu2)Ni(C2H4) (5). From Ni(1,5-hexadiene)2 and tBu2Bu2PC2H4P4P'Bu2 in 1,5-hexadiene the yellow-greenish complex (tBu2Bu2PC2H4P4P'Bu2)Ni(η2-C6H10) (6) is obtained. As for 3, only one diene C=C bond is coordinated to nickel(0), but the structure is fluxional with exchange of the coordinated and unbound C=C bonds (NMR at 20°C). From a solution of 6 in pentane the dinuclear, diastereomeric compounds rac/meso-{(tBu2PC2H4P4P'Bu2)Ni}2(μ-η2,η2-C6H10) (7a,b) separate in large yellow crystals. In similar reactions the 1,6-heptadiene complexes (tBu2Bu2PC2H4PtBu2)Ni(η2-C7H12) (8) and rac/meso-{(tBu2Bu2PC2H4PtBu2)Ni}2(µ-η2μ-η2,η2-C7H12) (9a,b) are also obtained. In 6, 7a,b, 8, and 9a,b the open-chain diene ligands can easily be displaced, e.g., by ethene to afford 5. Thus, complexes 6, 7a,b, 8, 9a, b are the most reactive. These complexes react readily (the ethene derivative 5 also reacts but very slowly) with butadiene to yield large yellow cubes of (tBu2Bu2PC2H4P4P'Bu2)Ni(η72-C4H6) (10), which is also fluxional. The alkene complexes 5, 6, 7a, b, 8, 9a,b, 10 react with ethyne to yield yellow-brownish crystalline (tBu2tBu2PC2H4P4P'Bu2)Ni(C2H2) (11).

scholarly journals Synthesis of Six and Seven-membered Heterocyclic Molecules Containing an Adamantyl Fragment and an X-ray Crystal Structure of (E)-N-(adamantan-1-yl)-1-(3-nitrophenyl)methanimine

2020 ◽  
Vol 17 (1(Suppl.)) ◽  
pp. 0272
Author(s):  
Ahmed Shukkur
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Good Yield ◽  
1H Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography ◽  
Heterocyclic Molecules ◽  
Citraconic Anhydride

       Our work included a synthesis of three new imine derivatives—1,3-thiazinan-4-one, 1,3-oxazinan-6-one and 1,3-oxazepin-4,7-dione—which contained an adamantyl fragment. These were produced via the condensation of the Schiff`s base (E)-N-(adamantan-1-yl)-1-(3-aryl)methanimine with 3-mercaptopropanoic acid; 3-chloropropanoic acid; and maleic, citraconic anhydride, respectively. These new imines were prepared via the condensation of adamantan-1-ylamine and 3-nitro-, 3-bromobenzaldehyde in n-BuOH. We obtained a good yield of products. FTIR, 1H NMR spectroscopy and C.H.N.S analysis were used to diagnostic the products. The molecular structure of (E)-N-(adamantan-1-yl)-1-(3-nitrophenyl)methanimine was confirmed by X-ray crystallography analysis.  

Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

2017 ◽  
Vol 72 (10) ◽  
pp. 759-762 ◽  
Author(s):  
Marion Graf ◽  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Title Complex ◽  
Dinuclear Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diruthenium Complex

AbstractTreatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]4+ (1) besides small amounts of the species [Ru(tppz)2]2+. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF6)4 has been established by X-ray crystallography.

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