Quinones and quinone methides. X. The crystal structure of a dimeric oxidation product from 2,4-Bis(1,1-dimethylethyl)-6-[(4-methoxyphenyl)methyl]phenol

1984 ◽  
Vol 37 (12) ◽  
pp. 2593
Author(s):  
RY Wong ◽  
L Jurd
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Oxidation Product ◽  
Crystallographic Analysis ◽  
Quinone Methides ◽  
X Ray ◽  
A Minor

The molecular structure of a minor oxidation product of the insect sterilant 2,4-bis(1,1-dimethylethyl) 6-[(4-methoxyphenyl)methyl]phenol has been established as (�)-cis-1,3,6,8-tetrakis(1,1-dimethyl-ethyl)-4b,9b-bis(4-methoxyphenyl)-4b,9b-dihydrobenzofuro[3,2-b]benzofuran by means of X-ray crystallographic analysis.

The Meisenheimer rearrangement in heterocyclic synthesis. II. Synthesis and X-ray crystal structure of a tetrahydro-1H-2,3-benzoxazocine and preparation of a hexahydro-2,3-benzoxazonine

1980 ◽  
Vol 33 (6) ◽  
pp. 1323 ◽  
Author(s):  
JB Bremner ◽  
EJ Browne ◽  
PE Davies ◽  
CLWAH Raston
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Acetic Acid ◽  
Crystal And Molecular Structure ◽  
Phosphorus Oxychloride ◽  
Crystallographic Analysis ◽  
Heterocyclic Synthesis ◽  
Reaction Conditions ◽  
X Ray ◽  
Heterocyclic Derivatives

The heterocyclic derivatives, 8,9-dimethoxy-3-methyl-1-phenyl-3,4,5,6- tetrahydro-1H-2,3-benzoxazocine(3a) and 9,10-dimethoxy-3-methyl-1- phenyl-1,3,4,5,6,7-hexahydro-2,3-benzoxazonine (3b),examples of two new ring systems, have been prepared by Meisenheimer rearrangement of the corresponding 2-benzazepine and 2-benzazocine N-oxide derivatives (2a) and (2b). The Bischler-Napieralski-type cyclization reaction was used in the preparation of the tertiary amine precursors of these N-oxides reaction conditions for the cyclization were critical and phosphorus oxychloride in refluxing butanenitrile was found to give the best yields of the seven- or eight-membered cyclic imine intermediates. Reductive cleavage of the benzoxazocine derivative (3a) with zinc in acetic acid followed by N-methylation gave the expected product, [2-{3- (dimethylamino)propyl}-4,5-di-methoxyphenyl]phenylmethanol (12). The crystal and molecular structure of (3a) has been determined by X-ray crystallographic analysis.

Quinones and quinone methides. IX. Oxidation of 2,4-Bis(1,1-dimethylethyl)-6-(4-methoxyphenylmethyl)phenol in alcoholic solvents: Monomeric products and the crystal structure of an unusual dimes, 2-[3,5-Bis(1,1-dimethylethyl)-2-{methoxy-(4-methoxyphenyl)methoxy} phenoxyl-1,5-bis(1,1-dimethylethyl)-3-[methoxy-(4-methoxyphenyl)methyl]benzene

1981 ◽  
Vol 34 (8) ◽  
pp. 1645 ◽  
Author(s):  
L Jurd ◽  
RY Wong
Keyword(s):  
Crystal Structure ◽  
Silver Oxide ◽  
Crystallographic Analysis ◽  
Quinone Methides ◽  
X Ray ◽  
High Yields ◽  
Methyl Benzene

Oxidation of the title benzylphenol (1) with silver oxide in alcoholic media forms benzylic ethers of type (5) in high yields; e.g. oxidation in methanol yields 2,4-bis(1,1-dimethylethyl)-6-[methoxy(4- methoxyphenyl)methyl]phenol(5a) together with an unusual dimer, the structure of which was shown by X-ray crystallographic analysis to be 2-[3,5-bis(1,1-dimethylethyl)-2-{methoxy(4-methoxyphenyl)- methoxy}phenoxy]-1,5-bis(1,1-dimethylethy)-3-[methoxy(4- methoxyphenyl)methyl]benzene (6). The benzylic ethers (5) are convenient intermediates for the syntheses of a variety of compounds related to (1).

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Chalkogenolat-Ionen und ihre Derivate, V Kristall- und Molekülstruktur von 2.8-Dimethyldibenzo [c.g] [1.2.5.6] tetrathiacyclooktadien, einem Oxidationsprodukt von 4-Methylbenzol-1.2-dithiol/Chalcogenolates and their Derivatives, V Crystal and Molecular Structure of 2.8-Dimethyldibenzo[c,g][1,2,5,6]tetrathiaocin, an Oxidation Product of 4-Methylbenzene-1,2-dithiol

1979 ◽  
Vol 34 (1) ◽  
pp. 48-51 ◽  
Author(s):  
Jürgen Kopf ◽  
Klaus von Deuten ◽  
Bahman Nakhdjavan ◽  
Günter Klar
Keyword(s):  
Molecular Structure ◽  
Dihedral Angle ◽  
Oxidation Product ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
The Mean ◽  
Ray Methods ◽  
Anti Form

Abstract The structure of 2,8-dimethyldibenzo[c,g][1,2,5,6]tetrathiaocin (1b) has been determined by X-ray methods and discussed in connection with the preferred conformations of diaryl disulfides. The compound has the anti-form I. The SS-distance is 205.8 pm, the mean CSS-angle 104.1°, and the CSS/SSC-dihedral angle 111.1°.

A Novel Alkali-Metal Hydrido-tris(pyrazolyl)borate (Tp*) Complex. Isolation and Crystal Structure of [(Me2CO)3(NaTp*)2]

2014 ◽  
Vol 69 (7) ◽  
pp. 793-798
Author(s):  
Laurent Plasseraud ◽  
Hélène Cattey
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Sodium Hydroxide ◽  
Title Compound ◽  
Room Temperature ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Large Excess ◽  
X Ray ◽  
Acetone Water

The title compound was isolated from the treatment of Tp*Sn(Cl)2Bu (1) with a large excess of sodium hydroxide in a mixture of acetone-water at room temperature. [(Me2CO)3(NaTp*)2] (2) crystallizes at 4 °C as prismatic colorless crystals, in the monoclinic space group P21/c with Z = 4, a = 12.2837(6), b = 24.3197(12), c = 16.9547(8) Å, β = 110.017(1)°, and V = 4759.0(4) Å3. The X-ray crystallographic analysis revealed a dinuclear unit in which two Tp*Na moieties are held together by three bridging acetone molecules acting as oxygen-based donors.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

Molecular structure and reactivity of the 1,2-dihydrocarbazol-4(3H)-one: X-ray crystal structure of N-methyl and N-(p-methylbenzenesulfonyl) derivatives

1995 ◽  
Vol 25 (5) ◽  
pp. 249-257 ◽  
Author(s):  
José Gonzalo Rodríguez ◽  
Celestina del Valle ◽  
Carmen Esteban-Calderón ◽  
Martín Martinez-Ripoll
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
X Ray

Synthese und Eigenschaften einiger Silylethinylsilane; Molekülstruktur von Tetrakis(trimethylsilylethinyl)silan / Synthesis and Properties of Some Silylethynylsilane; Molecular Structure of Tetrakis(trimethylsilylethynyl)silane

1988 ◽  
Vol 43 (1) ◽  
pp. 49-52 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Jan Ebenhöch
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Silicon Atom ◽  
Grignard Reagent ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Nmr Data

Abstract Trimethylsilylethine (1) has been prepared from C2H2, sodium and Me3SiCl in anisole. The product can be converted into a Grignard reagent Me3SiC≡CMgCl using iPrMgCl. This reagent yields the compounds Me3SiC≡CSiH3, (Me3SiC≡C)2SiH2, (Me3SiC≡C)3SiH, and (Me3SiC≡C)4Si (2-5) when treated with equivalent amounts of H3SiBr, H2SiBr2, HSiCl3, or SiCl4. respectively. The new silanes have been characterized by NMR data. The crystal structure of (Me3SiC≡C)4Si has been determined by single crystal X-ray diffraction. It shows the expected tetrahedral geometry at he central silicon atom with four linear SiC≡CSi linkages.

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