Crystal structure of 3-chlorobenzo[b]thiophene-2-carbonyl chloride

2009 ◽  
Vol 2009 (7) ◽  
pp. 437-439 ◽  
Author(s):  
Sara Tarighi ◽  
Alireza Abbasi ◽  
Sara Zamanian ◽  
Alireza Badiei ◽  
Mahmood Ghoranneviss
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cinnamic Acid ◽  
Thionyl Chloride ◽  
Structure Determination ◽  
X Ray ◽  
Packing Structure ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
C Nmr

3-Chlorobenzo[b]thiophene-2-carbonyl chloride was synthesised from cinnamic acid and thionyl chloride. The single crystal X-ray structure determination confirmed the earlier proposed structure and the product was further characterised by 1H NMR, 13C NMR and mass spectrometry. The X-ray structure determination revealed two sets of symmetry related molecules along the b-axis that are loosely connected by relatively weak CH…π ( 3.626, 3.628 Å) interactions, giving rise to two infinite chains. The packing structure is dominated by Van der Waals forces between these chains. No significant π–π interactions are found in the crystal structure.

Synthesis and Single Crystal X-Ray Structure of Ethyl 2-(1,3-Benzoxazol- 2-yl)-5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate

2007 ◽  
Vol 62 (5) ◽  
pp. 705-710 ◽  
Author(s):  
Ali Souldozi ◽  
Jabbar Khalafy ◽  
Ahmad Poursattar Marjani ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Structure Determination ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
X Ray ◽  
C Nmr

Abstract Ethyl 5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate was prepared from the reaction of diethyl 2-(4-toluidinocarbothioyl)malonate with hydroxylamine. Its reaction with 2- chlorobenzoxazole gave the corresponding N-substituted isoxazolone. The structure of the final product 4 was confirmed by IR, 1H and 13C NMR spectroscopy and mass spectrometry, and by X-ray single crystal structure determination.

Syntheses, Spectroscopy And Crystal Structures Of (R)-N-(1-Aryl-Ethyl)Salicylaldimines And [Rh{(R)-N-(1-Aryl-Ethyl)Salicylaldiminato}(η4-Cod)] Complexes

2007 ◽  
Vol 62 (6) ◽  
pp. 807-817 ◽  
Author(s):  
Mohammed Enamullah ◽  
A.K.M. Royhan Uddin ◽  
Anne-Christine Chamayou ◽  
Christoph Janiak
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Schiff Bases ◽  
Structure Determination ◽  
Chelate Ring ◽  
Optical Rotation ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Chiral Schiff Base ◽  
C Nmr

Condensation of salicylaldehyde with enantiopure (R)-(1-aryl-ethyl)amines yields the enantiopure Schiff bases (R)-N-(1-aryl-ethyl)salicylaldimine (HSB*; aryl = phenyl, 2-methoxyphenyl, 3- methoxyphenyl, 4-methoxyphenyl (4), 4-bromophenyl (5), 2-naphthyl). These Schiff bases readily react with dinuclear (acetato)(η4-cycloocta-1,5-diene)rhodium(I), [Rh(μ-O2CMe)(η4-cod)]2, to afford the mononuclear complexes, cyclooctadiene-((R)-N-(1-aryl-ethyl)salicylaldiminato-κ2N,O)- rhodium(I), [Rh(SB∗)(η4-cod)] (SB* = deprotonated chiral Schiff base = salicylaldiminate; aryl = phenyl (7), 2-methoxyphenyl, 4-methoxyphenyl, 4-bromophenyl, 2-naphthyl). The complexes have been characterized by IR, UV/vis, 1H/13C NMR and mass spectrometry, optical rotation as well as by single-crystal X-ray structure determination for 4, 5 and 7. The structure of 5 shows C-Br· · ·π contacts. Compound 7 is only the second example of a Rh(η4-cod) complex with a six-membered Rh-N,O-chelate ring

On Attempts to Synthesize Lanthanide Complexes of the Dianionic Fluorenyl-alkoxo Ligand [C13H8-cyclo-C6H10-O]2-. Crystal Structure of (C13H9-cyclo-C6H10-O)LaI2(DME)2

2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectra ◽  
Single Crystal ◽  
Lanthanide Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.

Synthesis and X-Ray Crystal Structure of Two Novel Ester Ferrocenophanes

2007 ◽  
Vol 62 (4) ◽  
pp. 605-609 ◽  
Author(s):  
Li Tao ◽  
Yang Bingqin ◽  
Gao Bo
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Elemental Analysis ◽  
3D Structure ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
Tof Ms

Two novel ester ferrocenophanes have been prepared by esterification of 1,1′-ferrocenedi(carbonyl chloride) with glycol and 1,4-butanediol, respectively. Both of them have been characterized by IR, elemental analysis, MALDI-TOF MS and 1H NMR spectroscopic methods, and their structures have been elucidated by X-ray diffraction. The intermolecular associations based on C-H···O hydrogen bonds have also been discussed. These molecules are assembled into chains, and the chains are further assembled into a 3D structure through several hydrogen bonds.

Gilded Chalices: Tetra-aurated Calix[4]arenes

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1061-1072 ◽  
Author(s):  
Ulf H. Strasser ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Raphael J. F. Berger ◽  
Norbert W. Mitzela
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Quantum Chemical ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Elemental Analyses ◽  
One Step ◽  
Energy Of Formation

Abstract 5,11,17,23-Tetrakis(trimethylsilylethynyl)-25,26,27,28-tetra-n-propoxycalix[4]arene (1) was synthesised in two steps starting from 25,26,27,28-tetra-n-propoxycalix[4]arene, and the structure of 1 was determined by X-ray diffraction. Compound 1 was desilylated (K2CO3) to give 5,11,17,23- tetrakis(ethynyl)-25,26,27,28-tetra-n-propoxycalix[4]arene (2), which was tetra-aurated under basic conditions (NaOEt, THF) with a series of phosphane-gold chlorides (o-Tol3PAuCl, Ph3PAuCl, Ph2MePAuCl, PhMe2PAuCl, Me3PAuCl, Cy3PAuCl, t-Bu3PAuCl) to afford in good to excellent yields the tetra-aurated tetraethynylcalix[4]arene species 3-9 in one step [with phosphane ligands o-Tol3P (3), Ph3P (4), Ph2MeP (5), PhMe2P (6), Me3P (7), Cy3P (8), t-Bu3P (9)]. All compounds were characterised by 1H NMR and infrared spectroscopy, mass spectrometry and by elemental analyses, additionally 3, 4, 5, 8 and 9 by 13C{1H}, and 3-6, 8 and 9 by 31P{1H} NMR spectroscopy. The molecular structures of complexes 3 and 9 were determined by X-ray diffraction and show pinched-cone conformations, but neither intra- nor intermolecular attractive aurophilic Au···Au contacts. The acceptor ability of complexes 3 and 9 was investigated by complexation attempts with various phosphane-gold chlorides and xenon gas under pressure, but interactions could not be determined experimentally. The formation of a complex between xenon and gilded calix[4]arene could, however, be predicted for fluorine-substituted species and with very small phosphane ligands (PH3) on the basis of quantum-chemical calculations; the energy of formation is 9:6 kJ mol-1. The crystal structure of Ph2MePAuCl was also determined and shows Au···Au-bonded dimers.

Kristallstruktur und spektroskopische Untersuchung von Mg(GeMe3)2 · 2 DME / Crystal Structure and Spectroscopic Study of Mg(GeMe3)2 · 2 DME

1984 ◽  
Vol 39 (7) ◽  
pp. 855-860 ◽  
Author(s):  
Lutz Rösch ◽  
Carl Krüger ◽  
A .-P. Chiang
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Study ◽  
Nmr Spectra ◽  
X Ray ◽  
H Nmr ◽  
Magnesium Compound ◽  
C Nmr

Mg(GeMe3)2 · 2 DME is synthesized by reaction of Hg(GeMe3)2 with magnesium in 1 ,2 -- dimethoxyethane. The X-ray structure, IR, Raman, 1H NMR , and 13C NMR spectra of this first organogermyl magnesium compound are reported.

Dihydride formation versus H2-elimination in the protonation of the heterobimetallic FePt complex (CO)3Fe(μ-H)(μ-PCy2)Pt(PEt3)2

1990 ◽  
Vol 68 (6) ◽  
pp. 869-874 ◽  
Author(s):  
Hilary A. Jenkins ◽  
Stephen J. Loeb ◽  
David G. Dick ◽  
Douglas W. Stephan
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Structure Determination ◽  
Reductive Elimination ◽  
Space Group ◽  
X Ray ◽  
Hydride Complex ◽  
H Nmr ◽  
H2 Elimination ◽  
Hydride Ligands

The reaction of Li[Fe(CO)4(PCy2)] with trans-PtCl(H)(PEt3)2 results in the formation of the hydride complex (CO)3Fe((μ-H)((μ-PCy2)Pt(PEt3)2, 1. This heterobimetallic, phosphido-bridged complex reacts with one equivalent of HBF4•Et2O to give the complex [(CO)3Fe(μ-H)2((μ-PCy2)Pt(PEt3)2][BF4], 2, which contains two bridging hydride ligands. This species is isolated and fully characterized by 31P{1H} and 1H NMR and infrared spectroscopy. In contrast, 1 reacts with one equivalent of HCl•DMA (DMA = dimethylacetamide) to give the complex (CO)3ClFe(μ-PCy2)Pt(PEt3)2, 3. This species is the result of oxidative addition of HCl with subsequent reductive elimination of H2(g). This complex is fully characterized by 31P{1H} and 1H NMR, infrared spectroscopy and an X-ray crystal structure determination. 3 crystallizes in the space group [Formula: see text] with a = 10.037(4) Å, b = 10.644(3) Å, c = 17.137(9) Å, α = 102.80(3)°, β = 76.74(3)°, γ = 103.99(3)°, V = 1702(1) Å3, and Z = 2. The structure was refined to R = 2.54% and Rw = 2.73% for 4056 reflections with Fo2 > 3σ(Fo2). Keywords: heterobimetallic, hydride, phosphide, protonation.

scholarly journals Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
L. A. Saghatforoush ◽  
L. Valencia ◽  
F. Chalabian ◽  
Sh. Ghammamy
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Antibacterial Activities ◽  
Tridentate Ligand ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Biological Studies ◽  
C Nmr

A new Cd(II) complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy), [Cd(Cltpy)(I)2], has been synthesized and characterized by CHN elemental analysis,1H-NMR,13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria.

Synthesis, crystal structure determination, and spectroscopic analyses of 1-chloro-2-(2,6-diisopropylphenyl)-4,4-dimethyl-2-azaspiro[5.5]undecane-3,5-dione: an unyielding precursor to a cyclic (alkyl)(amido)carbene

2021 ◽  
Vol 77 (7) ◽  
Author(s):  
Todd W. Hudnall ◽  
Eric W. Reinheimer ◽  
Christopher L. Dorsey
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Close Inspection ◽  
Precursor Molecule ◽  
X Ray ◽  
Spectroscopic Analyses ◽  
C Nmr

The synthesis, single-crystal X-ray structure, and 1H and 13C NMR spectrocopic analyses of an unyielding precursor molecule to a cyclic (alkyl)(amido)carbene, 1-chloro-2-(2,6-diisopropylphenyl)-4,4-dimethyl-2-azaspiro[5.5]undecane-3,5-dione, C24H34ClNO2 (1), is reported. Despite the use of several bases, 1 could not be deprotonated to afford the corresponding carbene. The crystal structure of 1 was compared to the crystal structures of two structurally similar HCl adducts of stable carbenes (compounds 4 and 5), which revealed no significant differences in the geometries about the `carbene' C atoms. To better understand the reactivity differences observed for 1 when compared to 4 and 5, modified percent buried volume (%V bur) calculations were performed. These calculations revealed that the H atom bound to the carbene C atom is the most sterically hindered in compound 1 when compared to 4 and 5 (%V bur = 84.9, 81.3, and 79.3% for 1, 4, and 5, respectively). Finally, close inspection of the quadrant-specific %V bur values indicated that the approach of a deprotonating base to the H atom bound to the carbene C atom is significantly blocked in 1 (69.9%) when compared to 4 and 5 (50.4 and 56.5%, respectively).

Novel hole transport materials based on N,N′-disubstituted-dihydrophenazine derivatives for electroluminescent diodes

2014 ◽  
Vol 2 (46) ◽  
pp. 9858-9865 ◽  
Author(s):  
Zhiwen Zheng ◽  
Qingchen Dong ◽  
Liao Gou ◽  
Jian-Hua Su ◽  
Jinhai Huang
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Crystal Structure Analysis ◽  
Hole Transport ◽  
Organic Light Emitting Diodes ◽  
Light Emitting ◽  
H Nmr ◽  
Organic Light ◽  
Single Crystal Structure Analysis ◽  
C Nmr

A series of novel hole transport materials for organic light-emitting diodes (OLEDs) based on 9,14-diphenyl-9,14-dihydrodibenzo[a,c]phenazine were synthesized and characterized by 1H NMR and 13C NMR, mass spectrometry and single crystal structure analysis methodologies.

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