A complex of gallium with a Schiff base - bis(orthoquinone) ligand

1999 ◽  
Vol 77 (4) ◽  
pp. 502-510 ◽  
Author(s):  
Martyn A Brown ◽  
Jesus A Castro ◽  
Bruce R McGarvey ◽  
Dennis G Tuck
Keyword(s):  
Schiff Base ◽  
Liquid Ammonia ◽  
Aqueous Ammonia ◽  
Tridentate Ligand ◽  
Triclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Spin Resonance ◽  
Aerial Oxidation ◽  
A Cell

The electrochemical oxidation of gallium in a cell containing a solution of 3,5-di-tert-butylcatechol (H2dbc) in a mixture of liquid ammonia and diethyl ether gives rise to the complex Ga(dbqdi)2, where dbqdi is a tridentate ligand formed by the condensation of two molecules of H2dbc and ammonia. The same paramagnetic molecule can be prepared by treating GaCl3 with H2dbc in ethanol with concentrated aqueous ammonia, with subsequent aerial oxidation. The crystal parameters are triclinic, space group P[Formula: see text], a = 11.6140(8), b = 12.3415(9), c = 20.765(1) Å, α = 89.491(1)°, β = 74.287(1)°, γ = 75.748(1)°, Z = 2, and R = 0.0542 for 7578 unique reflections. The structure, which is based on a GaO4N2 kernel, is discussed on the basis of crystallographic and ESR results.Key words: gallium, electrochemical synthesis, electron spin resonance, X-ray crystallography.

"A-frame" vs. "open-book" geometries in binuclear complexes bridged by diphosphines and mercaptothiazolinate ligands. Unusual examples involving a bridging bis(diphenylphosphino)ethane group

1993 ◽  
Vol 71 (5) ◽  
pp. 726-737 ◽  
Author(s):  
Jianliang Xiao ◽  
Martin Cowie
Keyword(s):  
Monoclinic Space Group ◽  
Stable Form ◽  
Binuclear Complexes ◽  
Open Book ◽  
Solid Reaction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
A Cell

Reaction of the tetracarbonyl species [M(CO)2(µ-mtz)]2 (M = Rh, Ir; mtz = 2-mercaptothiazolinate) with 1 equivalent of the diphosphines (Ph2P(CH2)nPPh2; n = 1 (dppm), 2 (dppe)) yields the compounds [M2(CO)2(µ-L)(µ-mtz)2] (M = Rh, L = dppm (1), dppe (3); M = Ir, L = dppm (2)), which readily undergo oxidative addition of iodine to give [M2I2(CO)2(µ-L)(µ-mtz)2] (M = Rh, L = dppm (4), dppe (6); M = Ir, L = dppm (5)). When 2 equivalents of dppm are used, the A-frame compounds [M2(CO)2(η1-mtz)(µ-mtz)(dppm)2] (M = Rh (7), Ir (8)) are afforded. In solution the dangling mtz group of 7 undergoes exchange with both the free mtz anion and the bridging mtz ligand. Compounds 7 and 8 are also produced by treatment of trans-[MCl(CO)(dppm)]2 (M = Rh, Ir) with 2 equivalents of the mtz anion. Reaction of these dppm-bridged dichloro species with 1 equivalent of the mtz anion yields [M2Cl(CO)2(µ-mtz)(dppm)2] (M = Rh (9a), Ir (10)). Compound 9a undergoes reversible Cl− dissociation to give [Rh2(CO)2(µ-mtz)(dppm)2][Cl] (9b), which is also the stable form in the solid. Reaction of 9 with CO gives the carbonyl-bridged species [Rh2(CO)2(µ-CO)(µ-mtz)(dppm)2][Cl]. The structures of 6 and 9b have been determined by X-ray crystallography. Compound 6 crystallizes in the triclinic space group [Formula: see text] with one-half equivalent of THF per asymmetric unit in a cell having a = 9.856(3) Å, b = 14.078(6) Å, c = 16.245(5) Å, α = 103.66(3)°, β = 93.21(3)°, γ = 92.91(3)°, V = 2182(1) Å3, and Z = 2, and has refined to R = 0.045 and Rw = 0.057 on the basis of 433 parameters varied. Compound 9b crystallizes with one equivalent of CH2Cl2 in the monoclinic space group P21/n with a = 11.400(1) Å, b = 21.944(2) Å, c = 22.134(1) Å, β = 92.494(7)°, V = 5532(1) Å3, and Z = 4, and has refined to R = 0.062 and Rw = 0.082 on the basis of 613 parameters varied.

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

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 4-vinylpyridine derivatives: Protonation, methylation and silver(I) coordination chemistry

2021 ◽  
pp. 174751982198965
Author(s):  
Guoqi Zhang
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Coordination Chemistry ◽  
Elemental Analysis ◽  
Silver Complex ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Moiety ◽  
New Compounds

( E)-4-[2-(Pyridin-4-yl)vinyl]benzaldehyde, containing both a 4-vinylpyridine and an aldehyde functionality, is utilized to develop new, highly conjugated chalcone compounds and a bis-Schiff base azine compound. The chalcone-containing compounds are further explored for their protonation, methylation and silver(I) coordination chemistry using the pyridine moiety. In parallel, a cyano-containing analogue, ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile is also synthesized and studied for its silver(I) coordination chemistry. These new compounds are fully characterized by mass spectrometry, elemental analysis and spectroscopic techniques. The methylated product of ( E)-1-(9-anthryl)-3-{4-[2-(pyridin-4-yl)vinyl]phenyl}prop-2-en-1-one and a silver complex of ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile are structurally determined by X-ray crystallography.

scholarly journals Structural Characterization of Heterodinuclear ZnII-LnIII Complexes (Ln = Pr, Nd) with a Ring-Contracted H2valdien-Derived Schiff Base Ligand

2021 ◽  
Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Structural Characterization ◽  
Schiff Base Ligand ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Imidazoline Ring

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

The direct electrochemical synthesis of some metal derivatives of lapachol

1997 ◽  
Vol 75 (5) ◽  
pp. 499-506 ◽  
Author(s):  
E.H. De Oliveira ◽  
G.E.A. Medeiros ◽  
C. Peppe ◽  
Martyn A. Brown ◽  
Dennis G. Tuck
Keyword(s):  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
Acetonitrile Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Anode ◽  
X Ray Crystallography ◽  
Metal Derivatives ◽  
Derivatives Of

The electrochemical oxidation of a sacrificial metal anode (M = Zn, Cd, Cu) in an acetonitrile solution of 2-hydroxy-3-(3-methyl-2-butenyl)-1,4-naphthoquinone, lapachol, C15H14O3 (=HL) gives ML2. The results are in keeping with earlier work on direct electrochemical synthesis in related systems. Adducts with 2,2′-bipyridine (bpy) and N,N,N′,N′-tetramethylethanediamine (tmen) have also been prepared. The structure of the 2,2′-bipyridine adduct of Cu(lapacholate)2 has been established by X-ray crystallography. The parameters are triclinic, space group [Formula: see text], a = 12.748(59) Å, b = 13.859(49) Å, c = 11.770(59) Å, α = 108.30(4)°, β = 108.08(3)°, γ = 68.94(3)°, Z = 2, R = 0.059 for 2256 unique reflections. The copper atom is in a distorted CuN2O2O2′ environment. The mechanism of the formation of this Cu(lapacholate)2 is discussed. Keywords: electrochemical synthesis, lapachol, X-ray crystallography, copper(II) complex.

scholarly journals Synthesis and structural peculiarities of gallium Complexes with novel paullone derivatives

2008 ◽  
Vol 6 (3) ◽  
pp. 340-346 ◽  
Author(s):  
Werner Ginzinger ◽  
Vladimir Arion ◽  
Gerald Giester ◽  
Markus Galanski ◽  
Bernhard Keppler
Keyword(s):  
Schiff Base ◽  
Tridentate Ligand ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gallium Chloride ◽  
Structural Peculiarities ◽  
Gallium Complex ◽  
Gallium Complexes

Abstract9-Bromo-7,12-dihydroindolo[3,2-d][1]benzazepin-6-ylhydrazine was reacted with 2-acetylpyridine to give a Schiff base as a potential tridentate ligand. The reaction of this ligand with gallium chloride afforded complexes of 1:1 and 2:1 stoichiometry. The results of X-ray diffraction studies of the ligand and both gallium complexes are reported and compared with the data for a related gallium complex with a Schiff base obtained from 9-bromo-7,12-dihydroindolo[3,2-d][1]benzazepin-6-ylhydrazine and 2-hydroxybenzaldehyde.

Electrical property and Schottky behavior of a flexible Schiff-base compound: X-ray structure and stabilization of 1D water chain

2018 ◽  
Vol 20 (38) ◽  
pp. 24744-24749 ◽  
Author(s):  
Basudeb Dutta ◽  
Joydeep Datta ◽  
Suvendu Maity ◽  
Chittaranjan Sinha ◽  
Di Sun ◽  
...  
Keyword(s):  
Schiff Base ◽  
Electrical Property ◽  
Impedance Spectroscopy ◽  
Schottky Diode ◽  
X Ray ◽  
X Ray Crystallography ◽  
Water Chain ◽  
Schiff Base Compound ◽  
Base Compound

A flexible Schiff-base compound has been synthesized and structurally confirmed by X-ray crystallography. The compound behaves as a Schottky diode, as supported by the impedance spectroscopy.

The Structures of the Decaphenylmetallocenium Cations of Chromium and Cobalt

1997 ◽  
Vol 50 (11) ◽  
pp. 1035 ◽  
Author(s):  
Leslie D. Field ◽  
Trevor W. Hambley ◽  
Taian He, ◽  
Anthony F. Masters ◽  
Peter Turner
Keyword(s):  
Methylene Chloride ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography

Decaphenylchromocenium and decaphenylcobaltocenium cations [M(η5-C5Ph5)2]+, M = Cr and Co, were synthesized by oxidation of the corresponding neutral decaphenylchromocene and decaphenylcobaltocene respectively with nitrosyl tetrafluoroborate. The complexes are air-stable and were fully characterized; decaphenylchromocenium tetrafluoroborate (1) and decaphenylcobaltocenium tetrafluoroborate (2) were structurally characterized by X-ray crystallography. Crystals of (1) (as a water/methylene chloride solvate), C70·5H50BClCrF4O0·5, M 1079·42, are triclinic, space group P -1 (No. 2), a 13·634(5), b 17·424(5), c 13·298(4) Å, α 106·45(2), β 101·83(3), γ 74·56(2)°, Z 2. Crystals of (2) (as a water/methylene chloride solvate), C70·5H50BClCoF4O0·5, M 1086·36, are triclinic, space group P-1 (No. 2), a 13·633(2), b 17·683(3), c 13·255(3) Å, α 107·95(1), β 102·71(1), γ 73·23(1)°, Z2.

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