Synthesis and crystal structure of a new homoleptic tetraarylruthenium(IV) complex Ru(2,4,5-Me3C6H2)4

2017 ◽  
Vol 72 (7) ◽  
pp. 523-525
Author(s):  
Chang-Jiu Wang ◽  
Xiu-Li Wu ◽  
Xiu-Fang Ma ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Column Chromatography ◽  
Proton Nmr ◽  
Proton Nmr Spectroscopy ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Moderate Yield

AbstractTreatment of [Ru(acac)3] (acac−=acetylacetonate) with (2,4,5-Me3C6H2)MgBr, followed by column chromatography in air, afforded the homoleptic tetraaryl-ruthenium(IV) complex [Ru(2,4,5-Me3C6H2)4] (1) in moderate yield. The product was characterized by proton NMR spectroscopy and microanalyses. Its crystal structure has also been established by X-ray crystallography.

Conformation of two 4'-thio-2'-deoxynucleoside analogs studied by 5000-MHz proton NMR spectroscopy and x-ray crystallography.

1992 ◽  
Vol 114 (25) ◽  
pp. 9936-9943 ◽  
Author(s):  
Leo H. Koole ◽  
Janez Plavec ◽  
Hongying Liu ◽  
Beverly R. Vincent ◽  
Michael R. Dyson ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Proton Nmr ◽  
Proton Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography

Synthesis and Crystal Structure of Lead(II) Thenoyltrifluoroacetonate Complexes with Substituted 2,2' -Bipyridines: Interplay of Intermolecular Interactions in Crystals

2010 ◽  
Vol 65 (2) ◽  
pp. 128-134 ◽  
Author(s):  
Farzin Marandi ◽  
Zahra Nikpey ◽  
Jia Hao Goh ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Nmr Spectroscopy ◽  
Intermolecular Interactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Three substituted 2,2'-bipyridine adducts of lead(II) thenoyltrifluoroacetonate, [Pb(4,4'-dm-2,2’- bpy)(ttfa)2]2, 1, [Pb(5,5' -dm-2,2’-bpy)(ttfa)2]2, 2, and [Pb(4,4'-dmo-2,2’-bpy)(ttfa)2], 3, (4,4’ -dm- 2,2’-bpy, 5,5’-dm-2,2’-bpy, 4,4’-dmo-2,2’-bpy and ttfa are the abbreviations for 4,4’-dimethyl-, 5,5’-dimethyl-, and 4,4’-dimethoxy-2,2’-bipyridine, and thenoyltrifluoroacetonate, respectively) have been synthesized, characterized by elemental and thermal analysis, IR and 1H- and 13C-NMR spectroscopy, and studied by X-ray crystallography. The supramolecular features in these complexes are guided/controlled by weak directional intermolecular interactions.

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.

Crystal-Structure Determination of Powdered Paramagnetic Lanthanide Complexes by Proton NMR Spectroscopy

2009 ◽  
Vol 121 (17) ◽  
pp. 3128-3132 ◽  
Author(s):  
Gwendal Kervern ◽  
Anthony D'Aléo ◽  
Loïc Toupet ◽  
Olivier Maury ◽  
Lyndon Emsley ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Lanthanide Complexes ◽  
Proton Nmr ◽  
Crystal Structure Determination ◽  
Proton Nmr Spectroscopy

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

Synthese und Kristallstruktur des Komplexsalzes [Au(tBu2PH)2][HCl2] / Synthesis and Crystal Structure of the Complex Salt [Au(tBu2PH)2][HCl2]

2012 ◽  
Vol 67 (6) ◽  
pp. 543-548 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Complex Salt ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Large Complex

The synthesis and the characterization of the complex salt [Au(tBu2PH)2][HCl2] (2) resulting from the reaction of hydrogen tetrachloridoaurate(III) hydrate with tBu2PH in dichloromethane at room temperature is reported. Single crystals of 2 have been analyzed by X-ray crystallography: monoclinic, P21=c, Z = 12, a = 12:0805(3), b = 12:3729(4), c = 46:7506(13) Å ; ß = 90:948(2)°; V = 6986:9(3) Å3; T = 173(2) K. The hydrogen bihalide anions [HCl2]- fill the interstices between the large complex cations [Au(tBu2PH)2]+ in the crystal.

scholarly journals Structure of the interleukin-2 tyrosine kinase Src homology 2 domain; comparison between X-ray and NMR-derived structures

2012 ◽  
Vol 68 (2) ◽  
pp. 145-153 ◽  
Author(s):  
Raji E. Joseph ◽  
Nathaniel D. Ginder ◽  
Julie A. Hoy ◽  
Jay C. Nix ◽  
D. Bruce Fulton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Tyrosine Kinase ◽  
Interleukin 2 ◽  
Crystal Form ◽  
X Ray ◽  
Proline Isomerization ◽  
Sh2 Domains ◽  
X Ray Crystallography ◽  
Src Homology

The crystal structure of the interleukin-2 tyrosine kinase Src homology domain (Itk SH2) is described and it is found that unlike in studies of this domain using NMR spectroscopy,cis–trans-prolyl isomerization is not readily detected in the crystal structure. Based on similarities between the Itk SH2 crystal form and thecisform of the Itk SH2 NMR structure, it is concluded that it is likely that the prolyl imide bond at least in part adopts thecisconformation in the crystal form. However, the lack of high-resolution data and the dynamic nature of the proline-containing loop mean that the precise imide-bond conformation cannot be determined and prolylcis–transisomerization in the crystal cannot be ruled out. Given the preponderance of structures that have been solved by X-ray crystallography in the Protein Data Bank, this result supports the notion that prolyl isomerization in folded proteins has been underestimated among known structures. Interestingly, while the precise status of the proline residue is ambiguous, Itk SH2 crystallizes as a domain-swapped dimer. The domain-swapped structure of Itk SH2 is similar to the domain-swapped SH2 domains of Grb2 and Nck, with domain swapping occurring at the β-meander region of all three SH2 domains. Thus, for Itk SH2 structural analysis by NMR spectroscopy and X-ray crystallography revealed very different structural features: proline isomerizationversusdomain-swapped dimerization, respectively.

scholarly journals Molecular recognition of polar neutral molecules by metallomacrocycles: synthesis, proton NMR spectroscopy, x-ray structure, electrochemistry, and ab initio calculations

1991 ◽  
Vol 56 (21) ◽  
pp. 6083-6094 ◽  
Author(s):  
Arie R. Van Doorn ◽  
Robert Schaafstra ◽  
Martinus Bos ◽  
Sybolt Harkema ◽  
Johan Van Eerden ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Molecular Recognition ◽  
Ab Initio Calculations ◽  
Ab Initio ◽  
Proton Nmr ◽  
Proton Nmr Spectroscopy ◽  
X Ray

Notizen: Synthesis and Crystal Structure of the Hydrogen Bonded Complex of Tri-paratoluidylphosphazenyl Oxide with Ethyl Alcohol

1976 ◽  
Vol 31 (9) ◽  
pp. 1295-1296 ◽  
Author(s):  
T. Stanley Cameron ◽  
M. Gerard Magee ◽  
Samuel Mclean
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Oxygen Atom ◽  
Ethyl Alcohol ◽  
Title Compound ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Bond Lengths ◽  
X Ray Crystallography ◽  
Phosphoryl Oxygen

The title compound was synthesised and its structure determined by X-ray crystallography. The structure contains a hydrogen bond between the OH group of the alcohol and the phosphoryl oxygen atom. The P–N bond lengths are significantly different and the differences can be attributed to varying ρπ—dπ interactions along the bonds.

New polysubstituted monoterpenic thiazolidinones: synthesis, spectroscopic and crystal structure studies

2018 ◽  
Vol 74 (12) ◽  
pp. 1629-1634 ◽  
Author(s):  
Abdellah N'ait Ousidi ◽  
Moulay Youssef Ait Itto ◽  
Aziz Auhmani ◽  
Abdelkhalek Riahi ◽  
Anthony Robert ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
2D Nmr ◽  
Asymmetric Unit ◽  
2D Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography ◽  
Naturally Occurring ◽  
Spectroscopic Analyses ◽  
Graph Set

The synthesis of three new polysubstituted monoterpenic thiazolidin-4-ones, namely (Z)-3-methyl-2-{(E)-[(1R,4R)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene]hydrazinylidene}thiazolidin-4-one, C14H21N3OS (2), (2Z,5Z)-5-[(dimethylamino)methylidene]-2-{(E)-[(1R,4R)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene]hydrazinylidene}thiazolidin-4-one, C16H24N4OS (3), and (2Z,5Z)-5-[(dimethylamino)methylidene]-3-methyl-2-{(E)-[(1R,4R)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene]hydrazinylidene}thiazolidin-4-one, C17H26N4OS (4), is reported, starting from the corresponding thiosemicarbazones obtained from naturally occurring (R)-camphor. All the newly obtained thiazolidin-4-ones have been fully characterized by HRMS and 1H and 13C (1D and 2D) NMR spectroscopy. Two of them, i.e. 2 and 3, were identified by single-crystal X-ray crystallography, confirming the synthetic pathway and the spectroscopic analyses. In 3, there are two roughly identical molecules within the asymmetric unit with the same absolute configuration. These two molecules are linked through N—H...O hydrogen bonds, building an R 2 2(8) graph-set motif.

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