Synthesis and X-ray structure of 1,2,2,2-tetrakis(3-methoxyphenyl)ethanone

2000 ◽  
Vol 78 (12) ◽  
pp. 1647-1650
Author(s):  
LeRoy H Klemm ◽  
Timothy JR Weakley
Keyword(s):  
Carbon Atom ◽  
Chemical Bonding ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Reductive Dimerization ◽  
X Ray Crystallography ◽  
H Nmr

Photochemical reductive dimerization of 3,3'-dimethoxybenzophenone (1b) gave the symmetrical benzopinacol 1,1,2,2-tetrakis(3-methoxyphenyl)ethane-1,2-diol (2b), which was rearranged to the benzopinacolone 1,2,2,2-tetrakis(3-methoxyphenyl)ethanone (3b) by means of I2 in boiling glacial HOAc. The structure of 3b was indicated by 1H NMR and determined definitively by X-ray crystallography. The crystals are monoclinic, space group P21/c, a = 12.250(2), b = 9.6997(12), c = 20.866(2) Å, β = 95.319(11)°, Z = 4, R = 0.053 for 4523 independent reflections. The structure establishes that the migrating 3-methoxyphenyl group retains bonding through its number 1' carbon atom to the parent C2-unit during the rearrangement process.Key words: X-ray structure, pinacol-pinacolone rearrangement, chemical bonding.

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 and characterization of [MII(bqb)] (M = Co, Ni, Cu), [N(n-Bu)4][CoIII(bqb)(CN)2], and [N(n-Bu)4][CoIII(bqb)(N3)2] containing deprotonated N,N'-bis(2-quinolinecarboxamide)-1,2-benzene (bqb) – X-ray crystal structures of [NiII(bqb)] and [N(n-Bu)4][CoIII(bqb)(N3)2]

2006 ◽  
Vol 84 (7) ◽  
pp. 971-978 ◽  
Author(s):  
Soria Meghdadi ◽  
Mehdi Amirnasr ◽  
Vratislav Langer ◽  
Alison Zamanpoor
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Elemental Analyses

Cobalt(II), nickel(II), copper(II), and two cobalt(III) complexes of a new dianionic ligand, bqb, [H2bqb = N,N'-bis(2-quinolinecarboxamide)-1,2-benzene] have been synthesized and characterized by elemental analyses, IR, and 1H NMR spectroscopy. The crystal and molecular structures of the [Ni(bqb)] (2) and [N(n-Bu)4][CoIII(bqb)(N3)2] (5) complexes were determined by X-ray crystallography. Complex 2 crystallizes in the monoclinic space group C2/c with a distorted square-planar structure including two short Ni–N (1.848 Å) and two long Ni–N (1.958 Å) bonds. The structure consists of sheets formed in the plane parallel to the b axis and diagonal to vectors a and c by intermolecular hydrogen bonds. Complex 5 crystallizes in the monoclinic space group C2 with a distorted octahedral structure. The [N(n-Bu)4]+ ion is disordered at the C3A and C4A atoms of one Bu. The IR and 1H NMR spectra of the complexes are also discussed.Key words: N4-dianionic amido ligand (bqb), (bqb) complexes of Co(II), Ni(II), Cu(II), and Co(III), azide, cyanide, X-ray crystal structures.

Synthesis, crystal structure and biological activity of 2-[2-(quinolin-2-yl)vinyl]-8-hydroxyquinoline and 2-[2-(quinolin-4-yl)vinyl]-8-hydroxyquinoline

2007 ◽  
Vol 40 (3) ◽  
pp. 471-475 ◽  
Author(s):  
He-Ping Zeng ◽  
Ting-Ting Wang ◽  
Dan-Feng Xu ◽  
Yue-Peng Cai ◽  
Dong-Feng Chen
Keyword(s):  
Biological Activities ◽  
Monoclinic Space Group ◽  
Flow Cytometry Analysis ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Diphenyltetrazolium Bromide ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Two new isomeric 8-hydroxyquinoline derivatives with quinoline groups have been synthesized by Perkin condensation. Their structures were characterized by EI-MS,1H NMR spectroscopy, elemental analysis and FT–IR spectroscopy; crystal structures were determined by X-ray crystallography. 2-[2-(Quinolin-2-yl)vinyl]-8-hydroxyquinoline crystallizes in the tetragonal space groupI41/aand 2-[2-(quinolin-4-yl)vinyl]-8-hydroxyquinoline crystallizes in the monoclinic space groupP21/n. Hydrogen bonds and intermolecular interactions are observed in the compounds and stabilize their structures. The biological activities were investigated by MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay and flow cytometry analysis, and the results revealed that the two compounds had effects on the proliferation of rat mesenchymal stem cells.

Crystallographic characterization of three cathinone hydrochlorides new on the NPS market: 1-(4-methylphenyl)-2-(pyrrolidin-1-yl)hexan-1-one (4-MPHP), 4-methyl-1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one (α-PiHP) and 2-(methylamino)-1-(4-methylphenyl)pentan-1-one (4-MPD)

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
Marcin Rojkiewicz ◽  
Piotr Kuś ◽  
Maria Książek ◽  
Joachim Kusz
Keyword(s):  
Chemical Structure ◽  
Crystallographic Data ◽  
New Psychoactive Substances ◽  
Monoclinic Space Group ◽  
Psychoactive Substances ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Analytical Laboratories

Cathinones belong to a group of compounds of great interest in the new psychoactive substances (NPS) market. Constant changes to the chemical structure made by the producers of these compounds require a quick reaction from analytical laboratories in ascertaining their characteristics. In this article, three cathinone derivatives were characterized by X-ray crystallography. The investigated compounds were confirmed as: 1-[1-(4-methylphenyl)-1-oxohexan-2-yl]pyrrolidin-1-ium chloride (1, C17H26NO+·Cl−, the hydrochloride of 4-MPHP), 1-(4-methyl-1-oxo-1-phenylpentan-2-yl)pyrrolidin-1-ium chloride (2; C16H24NO+·Cl−, the hydrochloride of α-PiHP) and methyl[1-(4-methylphenyl)-1-oxopentan-2-yl]azanium chloride (3; C13H20NO+·Cl−, the hydrochloride of 4-MPD). All the salts crystallize in a monoclinic space group: 1 and 2 in P21/c, and 3 in P21/n. To the best of our knowledge, this study provides the first detailed and comprehensive crystallographic data on salts 1–3.

scholarly journals Chemie polyfunktioneller Moleküle, 114 [1]. Synthese und Struktur eines ionischen und nichtionischen, cyclischen Carbaphosphazens und eines Cobalt(III)phosphazen-Komplexes / Chemistry of Polyfunctional Molecules, 114 [1]. Synthesis and Structure of an Ionic and Non Ionic Cyclic Carbaphosphazene and of a Cobalt(III)phosphazene Complex

1994 ◽  
Vol 49 (12) ◽  
pp. 1763-1773 ◽  
Author(s):  
Jochen Ellermann ◽  
Jörg Sutter ◽  
Falk A. Knoch ◽  
Matthias Moll ◽  
Walter Bauer
Keyword(s):  
Mass Spectra ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr

Reaction of (1) in CH2Cl2 with benzimidazole yields . The salt [4]+BPh4- has been prepared in THF by metathesis of [4]+Cl- with NaBPh4. Deprotonation of the cationic ring in [4]+BPh4- was accomplished using 1,8-diazabicyclo[5.4.01,7]undec-7-ene and resulted in the six-membered carbacyclophosphazene (6). Treating 1 with 8 -hydroxyquinoline in CH2Cl2 yields the octahedral cis-complex = 8-oxyquinolinate group). The com pounds [4]+BPh4-, 6 and 7 are characterized by their IR, Raman, 31P{1H} NMR, 13C{1H} NMR, 1H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4- and 7×0.5 CH2Cl2. The colourless plates of [4]+BPh4- crystallize in the triclinic space group P1̄, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; α = 100.79(2), β = 103.71(3), γ = 108.18(2)°. The black blocks of 7×0.5 CH2Cl2 crystallize in the monoclinic space group P 21/c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; β = 105.86(5)°.

The preparation and X-ray crystal structure of Te(N3)3SbF6 containing the triazidotellurium(IV) cation, Te(N3)3+

1989 ◽  
Vol 67 (11) ◽  
pp. 1687-1692 ◽  
Author(s):  
James P. Johnson ◽  
Gregory K. MacLean ◽  
Jack Passmore ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Average Bond

The crystal structure of Te(N3)3SbF6 containing the first binary tellurium–nitrogen cation, triazidotellurium(IV) (Te(N3)3+), has been determined by X-ray crystallography. Single crystals of Te(N3)3SbF6 are monoclinic, space group P21/c with a = 9.201(6), b = 8.445(4), c = 13.582(7) Å, β = 100.36(5)°, Z = 4, final R1 = 0.036 for 1286 observed reflections. The structure consists of discrete Te(N3)3+ cations and distorted octahedral SbF6− anions, with some cation–anion interactions. The average Te—Nα—Nβ—Nγ bond distances in Te(N3)3+ are Te—Nα, 1.994(7); Nα—Nβ, 1.237(11); and Nβ—Nγ, 1.116(12) Å. The average bond angles about the Te, Nα, and Nβ atoms are 94.1(3)°, 116.5(6)°, and 173.7(9)°. Structural correlations with other TeX3+ species have yielded an estimate of the electronegativity of the N3− group to be 3.1 ± 0.1. Keywords: tetratellurium (2+) cation, triazidotellurium(IV) cation, electronegativity, azide.

Metal-selenolate chemistry: stereochemistry of adamantane-type clusters of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd)

1992 ◽  
Vol 70 (3) ◽  
pp. 792-801 ◽  
Author(s):  
Jagadese J. Vittal ◽  
Philip A. W. Dean ◽  
Nicholas C. Payne
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Space Groups ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Minimum Number

The structures of three tetramethylammonium salts containing anions of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd) were determined by single crystal X-ray diffraction techniques. The Zn salt crystallizes in different space groups depending upon the solvent combination used in the synthesis. Thus crystals of (Me4N)2[Zn4(SePh)10], 1, grown from a mixture of methanol, acetonitrile, and acetone are triclinic, space group [Formula: see text] with cell dimensions a = 13.214(2), b = 23.859(2), c = 13.072(1) Å, α = 91.134(8), β = 113.350(8), γ = 79.865(9)°, and Z = 2. In the absence of acetone, a solvated crystal (Me4N)2[Zn4(SePh)10]•CH3CN, 2, is formed, which belongs to the monoclinic space group P21/n with a = 14.248(1), b = 39.722(2), c = 13.408(1) Å, β = 97.132(5)°, and Z = 4. The Cd salt (Me4N)2[Cd4(SePh)10], 3, crystallizes in the monoclinic space group P21/c, with a = 20.830(2), b = 14.282(1), c = 25.872(1) Å, β = 99.626(6)°, and Z = 4. These three salts are the first examples of homoleptic, tetranuclear selenolatometal(II) anions with (μ-Se)6M4 cages of adamantane-type stereochemistry. In each case the phenyl substituents of the bridging ligands adopt the configuration [aae, aae, aee, aee], which has the minimum number of two 1,3-axial–axial non-bonding substituent interactions. Keywords: selenolate complexes, synthesis, X-ray crystallography, isomerism, adamantane stereochemistry.

Structure and conformation of the N-β-propionic acids of cyclohexan[b]indole and cyclooctan[b]indole

1986 ◽  
Vol 64 (9) ◽  
pp. 1829-1835 ◽  
Author(s):  
Carmen Esteban-Calderon ◽  
Martín Martinez-Ripoll ◽  
Severino García-Blanco ◽  
Fernando Temprano ◽  
José Gonzalo Rodriguez
Keyword(s):  
Propionic Acid ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Ray Methods

The structures of cyclohexan[b]indole N-β-propionic acid (1) and cyclooctan[b]indole N-β-propionic acid (2) have been determined by X-ray methods. The conformational populations of their N-β-propionic chains have been determined in solution by 1H nmr analyses. Crystals of 1 are triclinic, space group [Formula: see text] with a = 12.3562(4), b = 11.0727(3), c = 10.2050(4) Å, α = 108.519(3), β = 83.941(3), γ = 104.826(3)°, and Z = 4. Crystals of 2 are monoclinic, space group P21/c, with a = 5.636(1), b = 18.937(3), c = 13.976(4) Å, β = 98.84(3)°, and Z = 4. In both structures, the molecules are linked forming dimers through centrosymmetric H bonds. In solution the trans conformation of the chain is the preferred one in both compounds and increases with dilution until a constant value is reached.

Synthese Und Kristallstrukturen Von Chlorometallaten [M = V(III), Mo(V)]

2001 ◽  
Vol 56 (8) ◽  
pp. 759-764 ◽  
Author(s):  
Soheila Chitsaz ◽  
Effat Iravani ◽  
Jochen Pauls ◽  
Bernhard Neumüller
Keyword(s):  
Ir Spectroscopy ◽  
Membered Ring ◽  
Dinuclear Complex ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Independent Molecules ◽  
Triclinic Form

[(THF)2LiCl2VCl2(THF)2] (1) and [Li(THF)4][OMoCl4(THF)] (2) can be prepared by the reactions of VCI3 with LiCl in THF and of Li(H)PtBu with OM0 CI4 in THF, respectively. 1 and 2 were characterized by IR spectroscopy, MS spectrometry (2) and X-ray crystallography. 1 can be obtained in two modifications depending on the temperature of crystallization. At -30 °C a triclinic form, 1a, was isolated from THF solution with one unique molecule per asymmetric unit. However, at 20 °C, 1b crystallized in the monoclinic space group P2/c. It possesses four independent molecules per asymmetric unit. According to the structure analyses 1 consists of a dinuclear complex with a planar LiCl2V four-membered ring while 2 consists of seperate ions [Li(THF)4]+ and [OMoCl4(THF)]-

Synthesis and Structure of an Aluminum Bis(3-chloropentanedionate) Isopropoxide: [Al(μ-OiPr)(3-Clacac)2]2

2014 ◽  
Vol 69 (7) ◽  
pp. 799-803 ◽  
Author(s):  
Kiran Gupta ◽  
Peter Mayer ◽  
Ashutosh Pandey
Keyword(s):  
Ir Spectroscopy ◽  
Ambient Temperature ◽  
Single Crystal ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Elemental Analyses

1A[Al(OiPr)3]4 was reacted at ambient temperature with 3-chloropentanedione (3-ClacacH) in 1 : 1 molar ratio in toluene, to obtain the mono-substituted product. However, the bis-substituted dinuclear tetrakis(3-chloropentanedionato)-di-m-isopropoxy-dialuminum(III) [Al(μ-OiPr)(3-Clacac)2]2 () was isolated in 46% yield upon aging of the reaction mixture at −10 °C. The supernatant upon aging yielded a crop of tris-3-chloroacetylacetonate Al(3-Clacac)3·H2O (1) in 13% yield. Complexes 1A (monoclinic, space group P21/c with Z = 2) and 1(cubic, space group P43n with Z = 8) were characterized by elemental analyses, NMR and IR spectroscopy and single-crystal X-ray crystallography.

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