Ruthenium carbonyl complexes. III. Peparations, properties and structures of Dicarbonyl- and Monocarbonyl-(2,2':6',2''-terpyridyl)ruthenium(II) complexes

1984 ◽  
Vol 37 (5) ◽  
pp. 929 ◽  
Author(s):  
GB Deacon ◽  
JM Patrick ◽  
BW Skelton ◽  
NC Thomas ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Room Temperature ◽  
Chloro Complex ◽  
Carbonyl Complexes ◽  
X Ray ◽  
X Ray Crystallography ◽  
Ruthenium Carbonyl

Reaction of 2,2':6',2''-terpyridyl (tpy) with ruthenium dicarbonyl dihalides yields the complexes Ru(CO)2X2(tpy) (X = Br or Cl), which can be protonated giving [Ru(CO)2X2(tpyH)]ClO4. Crystal structures of the two forms (red and yellow) of Ru(CO)2Br2(tpy) show each to have octahedral stereo-chemistry with cis-carbonyls, trans-bromines, and bidentate tpy. Treatment of Ru(CO)2X2(tpy) complexes with trimethylamine N-oxide in dichloromethane at room temperature gives cis-Ru(CO)X2(tpy) complexes. The presence of cis halogens and tridentate terpyridyl in the chloro complex has been established by X-ray crystallography. Reaction of terpyridyl with ruthenium trichloride in dimethylformamide yields trans-Ru(CO)Cl2(tpy), the crystal structure of which has been determined.

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.

Cyclometallated Compounds. IX. Reactions of 2-Benzoylpyridine With Rhodium(III) Trichloride

1995 ◽  
Vol 48 (9) ◽  
pp. 1573 ◽  
Author(s):  
DJ Degeest ◽  
PJ Steel
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Reaction Conditions ◽  
Initial Product ◽  
X Ray ◽  
X Ray Crystallography

X-Ray crystallography and n.m.r. spectroscopy have been used to study the products of reactions between rhodium(III) trichloride and 2-benzoylpyridine under various reaction conditions. X-Ray crystal structures have shown that the initial product of reaction in refluxing ethanol is a centrosymmetric isomer, as previously proposed, but that this undergoes aqueous hydrolysis to a C2-symmetric isomer, rather than the previously proposed C2v isomer. Reaction in refluxing 2-methoxyethanol produces an unusual complex with one C-N cyclometallated ligand and one N-O coordinated ligand. In Me2SO, the non-cyclometallated ligand of this latter compound undergoes solvolysis to produce a complex containing two Me2SO molecules, one coordinated through oxygen and the other through sulfur. The X-ray crystal structure of this compound is also reported.

Synthesis of the cyclopropa[c]benzofuran system of mycorrhizin A and of gilmicolin from a benzofuranol. Crystal structure of a 5,8-Methanocyclopropa-[c]naphtho[2,3-b]furan derivative

1982 ◽  
Vol 35 (8) ◽  
pp. 1665 ◽  
Author(s):  
RFC Brown ◽  
GD Fallon ◽  
BM Gatehouse ◽  
CM Jones ◽  
ID Rae
Keyword(s):  
Crystal Structure ◽  
Ultraviolet Irradiation ◽  
Room Temperature ◽  
Cyclopropane Ring ◽  
Structural Features ◽  
Side Chain ◽  
Furan Derivative ◽  
Methoxy Derivative ◽  
X Ray ◽  
X Ray Crystallography

The cyclopropa[c]benzofuran derivative (17), which contains the structural features of methyl ethers of mycorrhizin A and gilmicolin save for the C3 side chain, has been synthesized from the benzofuranol (4) through the benzofuran-4,7-dione (5) and the 7a-methoxy derivative (8). The cyclopropane ring of (17) was introduced by ultraviolet irradiation of a 1-pyrazoline (13) at -78�; irradiation at room temperature gave mainly a profoundly rearranged acidic product for which the methanoindenone structure (18) is proposed. The stereochemistry of the penultimate cyclopropane (16) has been established by X-ray crystallography.

A topochemical rearrangement with multiple inversions of configuration

2001 ◽  
Vol 79 (8) ◽  
pp. 1272-1277 ◽  
Author(s):  
Saul Wolfe ◽  
Yih-Huang Hsieh ◽  
Raymond J Batchelor ◽  
Frederick WB Einstein ◽  
Ian D Gay
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Room Temperature ◽  
The Other ◽  
X Ray ◽  
Controlled Processes ◽  
X Ray Crystallography ◽  
Intramolecular Process ◽  
C Nmr ◽  
The Ideal

Crystalline 2-benzyloxypyridine-1-oxide rearranges slowly at room temperature to crystalline 1-benzyloxy-2-pyridone. No intermediates are detected when the process is followed by solid-state 13C NMR. The crystal structure of the pyridine-1-oxide strongly suggests that a topochemically controlled intramolecular process, in which the benzyl group migrates with retention of configuration, is not feasible. On the other hand, although somewhat disfavoured by initial solid-state O···C···O angles significantly less than the ideal 180°, intermolecular topochemically controlled processes can be envisaged that lead, with multiple inversions of configuration, either to net retention of configuration or to net inversion of configuration in the benzyl group. In contrast to the 50–80% inversion observed in solution, in the solid state only inversion is observed experimentally when chirally labelled α-deuteriobenzyloxypyridine-1-oxide is allowed to rearrange.Key words: X-ray crystallography, solid-state 13C NMR, benzyl-α-D-alcohol, 2-benzyloxypyridine-1-oxide, 1-benzyloxy-2-pyridone.

Synthesis, spectral data, and crystal structure of two novel substitution patterns in dithiaporphyrins

2007 ◽  
Vol 11 (01) ◽  
pp. 1-8 ◽  
Author(s):  
Youngjae You ◽  
Thalia S. Daniels ◽  
Paulina M. Dominiak ◽  
Michael R. Detty
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Spectral Data ◽  
X Ray ◽  
X Ray Crystallography

The syntheses, characterizations and crystal structures of 5-(4-tert-butylphenyl)-15,20-diphenyl-10-(4-methoxy)phenyl-21,23-dithiaporphyrin (1b) and 2,3-dimethoxy-10,15-diphenyl-21,23-dithiaporphyrin (2) are described. The cyclization of 2-[1-(4-methoxyphenyl)-1-pyrrolomethyl]-5-(1-phenyl-1-pyrrolomethyl)thiophene and 2-[1-(4-t-butylphenyl)-1-hydroxymethyl]-5-(1-phenyl-1-hydroxymethyl)thiophene gave predominantly the cis-regioisomer, which was characterized by X-ray crystallography.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Synthesis, structural characterization and catalytic activity of chlororuthenium(II) complexes with substituted Schiff base/phosphine ancillary ligands

2020 ◽  
Vol 75 (9-10) ◽  
pp. 851-857
Author(s):  
Chong Chen ◽  
Fule Wu ◽  
Jiao Ji ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Schiff Base ◽  
Catalytic Activity ◽  
Structural Characterization ◽  
Room Temperature ◽  
Molecular Structures ◽  
Cationic Complex ◽  
Neutral Complex ◽  
Ancillary Ligands ◽  
X Ray ◽  
X Ray Crystallography

AbstractTreatment of [(η6-p-cymene)RuCl2]2 with one equivalent of chlorodiphenylphosphine in tetrahydrofuran at reflux afforded a neutral complex [(η6-p-cymene)RuCl2(κ1-P-PPh2OH)] (1). Similarly, the reaction of [Ru(bpy)2Cl2·2H2O] (bpy = 2,2′-bipyridine) and chlorodiphenylphosphine in methanol gave a cationic complex [Ru(bpy)2Cl(κ1-P-PPh2OCH3)](PF6) (2), while treatment of [RuCl2(PPh3)3] with [2-(C5H4N)CH=N(CH2)2N(CH3)2] (L1) in tetrahydrofuran at room temperature afforded a ruthenium(II) complex [Ru(PPh3)Cl2(κ3-N,N,N-L1)] (3). Interaction of the chloro-bridged complex [Ru(CO)2Cl2]n with one equivalent of [Ph2P(o-C6H4)CH=N(CH2)2N(CH3)2] (L2) led to the isolation of [Ru(CO)Cl2(κ3-P,N,N-L2)] (4). The molecular structures of the ruthenium(II) complexes 1–4 have been determined by single-crystal X-ray crystallography. The properties of the ruthenium(II) complex 4 as a hydrogenation catalyst for acetophenone were also tested.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

scholarly journals A mixed chirality α-helix in a stapled bicyclic and a linear antimicrobial peptide revealed by X-ray crystallography

2021 ◽  
Author(s):  
Stéphane Baeriswyl ◽  
Hippolyte Personne ◽  
Ivan Di Bonaventura ◽  
Thilo Köhler ◽  
Christian van Delden ◽  
...  
Keyword(s):  
Antimicrobial Peptides ◽  
Antimicrobial Peptide ◽  
Crystal Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Α Helix

We report the first X-ray crystal structures of mixed chirality α-helices comprising only natural residues as the example of bicyclic and linear membrane disruptive amphiphilic antimicrobial peptides containing seven l- and four d-residues.

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