scholarly journals Synthesis and photophysical properties of novel benzophospholo[3,2-b]indole derivatives

2017 ◽  
Vol 13 ◽  
pp. 2304-2309 ◽  
Author(s):  
Mio Matsumura ◽  
Mizuki Yamada ◽  
Atsuya Muranaka ◽  
Misae Kanai ◽  
Naoki Kakusawa ◽  
...  
Keyword(s):  
Structure Analysis ◽  
Phosphine Oxide ◽  
Photophysical Properties ◽  
Starting Material ◽  
Indole Derivatives ◽  
X Ray

The parent benzophospholo[3,2-b]indole was prepared by the reaction of dichlorophenylphosphine with a dilithium intermediate, which was prepared in two steps from 2-ethynyl-N,N-dimethylaniline. Using the obtained benzophosphole-fused indole as a common starting material, simple modifications were carried out at the phosphorus center of the phosphole, synthesizing various functionalized analogs. The X-ray structure analysis of trivalent phosphole and phosphine oxide showed that the fused tetracyclic moieties are planar. The benzophosphole-fused indoles, such as phosphine oxide, phospholium salt, and borane complex, exhibited strong photoluminescence in dichloromethane (Φ = 67–75%).

The Stability and Conformation of the 1,3,6,8-Tetraazatricyclo[4.4.1.13,8]dodecane System: the Structure of the Condensation Product of 1,2-Diaminocyclohexane and Formaldehyde

1975 ◽  
Vol 53 (13) ◽  
pp. 1933-1935 ◽  
Author(s):  
P. Murray-Rust ◽  
F. G. Riddell
Keyword(s):  
Structure Analysis ◽  
Condensation Product ◽  
Optically Active ◽  
Starting Material ◽  
Analogous Reaction ◽  
X Ray ◽  
The Stability

The condensation of d,1-trans-1,2-diaminocyclohexane with formaldehyde gives a pentacyclic molecule based on the 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane nucleus. This was shown to have S4 symmetry by 1H n.m.r. and an X-ray analysis showed crystals to be orthorhombic, Fddd, a = 12.02, b = 19.25, c = 12.90 Å. The symmetry of the compound in the crystal was D2d due to a disordered arrangement and structure analysis was carried out to R = 0.166. When optically active diamine was used as starting material, the analogous reaction did not occur and this was attributed to strain in the tricyclic system. The conformation of the molecule is related to those of similar compounds as found by X-ray analysis.

scholarly journals Pyridinium Pentachloridooxomolybdate(V), (PyH)2[MoOCl5], Revisited: Single-Crystal X-ray Structure Determination

Molbank ◽  
10.3390/m1249 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1249
Author(s):  
Jaka Šturm ◽  
Barbara Modec
Keyword(s):  
Coordination Chemistry ◽  
Single Crystal ◽  
Structure Analysis ◽  
Structure Determination ◽  
Structural Characteristics ◽  
Starting Material ◽  
X Ray

(PyH)2[MoOCl5] was obtained in the form of emerald green crystals unintentionally from (PyH)5[MoOCl4(H2O)]3Cl2 in acetonitrile. (PyH)2[MoOCl5] has been used as a starting material in molybdenum(V) coordination chemistry for decades, yet its true identity has not been known until now. The X-ray structure analysis has undoubtedly confirmed the existence of this compound. The [MoOCl5]2− ion displays the usual structural characteristics of the mononuclear MoO3+-containing compounds.

Preparation and Characterisation of Iodo-functionalised Azobenzene Derivatives of the Type I–p-C6H4–N=N–p-C6H4–X

2008 ◽  
Vol 63 (12) ◽  
pp. 1395-1401 ◽  
Author(s):  
Ulrich Siemeling ◽  
Clemens Bruhn ◽  
Mario Meier ◽  
Christian Schirrmacher
Keyword(s):  
Single Crystal ◽  
Structure Analysis ◽  
General Type ◽  
Starting Material ◽  
Type I ◽  
X Ray Diffraction ◽  
Ferrocene Derivative ◽  
X Ray ◽  
Derivatives Of ◽  
Azobenzene Derivatives

A broad range of azobenzene derivates of the general type I-p-C6H4-N=N-p-C6H4-X (1) have been prepared. In the case of X = Ph (b), C≡C-Fc (e, Fc = ferrocenyl), OMe (g), Oi-Pr (i), and NMe2 (m), these compounds have been characterised by single-crystal X-ray structure analysis. In addition, the closely related 4-dimethylamino-1-(4-iodophenylazo)naphthalene 2 and 8-(4-iodophenylazo) quinoline 3 have also been prepared. Furthermore, the ferrocene derivative Fc-C≡C-p-C6H4- NH2 (4), which served as a starting material for the synthesis of I-p-C6H4-N=N-p-C6H4-p-C6H4- C≡C-Fc (1e), was prepared and structurally characterised by X-ray diffraction.

scholarly journals Hybrid Layered Crystal Comprising Polyoxometalate and Surfactant Synthesized from Reduced Mo-Blue Species

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Keisuke Mikurube ◽  
Kimiko Hasegawa ◽  
Haruo Naruke ◽  
Takeru Ito
Keyword(s):  
Structure Analysis ◽  
Single Phase ◽  
Proton Conductor ◽  
Starting Material ◽  
Layered Crystal ◽  
Two Dimensional ◽  
X Ray ◽  
New Class ◽  
Layered Crystals ◽  
Inorganic Layers

A hybrid layered crystal containing polyoxomolybdate was successfully synthesized from reduced Mo-blue species as starting material. The hybrid crystal, [C5H5N(C16H33)]2[β-H2Mo8O26]·2C2H5OH (C16py-H2Mo8), was obtained as a single phase by the gradual oxidation of hexadecylpyridinium-Mo-blue (C16py-Mo-blue) hybrid. The X-ray structure analysis revealed that C16py-H2Mo8comprisedβ-type octamolybdate anion with two protons (β-H2Mo8). Theβ-H2Mo8anions and ethanol molecules of crystallization formed two-dimensional anionic layers. The pyridine rings of C16py did not attend to form the two-dimensional inorganic layers, and the interdigitated C16py bilayers were sandwiched by theβ-H2Mo8anionic layers with periodicity of 18.2 Å. These C16py-H2Mo8hybrid layered crystals possibly work as a new class of proton conductor.

scholarly journals Synthesis, structural characterization, and optical properties of benzo[f]naphtho[2,3-b]phosphoindoles

2021 ◽  
Vol 17 ◽  
pp. 671-677
Author(s):  
Mio Matsumura ◽  
Takahiro Teramoto ◽  
Masato Kawakubo ◽  
Masatoshi Kawahata ◽  
Yuki Murata ◽  
...  
Keyword(s):  
Optical Properties ◽  
Fluorescence Spectroscopy ◽  
Single Crystal ◽  
Functional Groups ◽  
Phosphine Oxide ◽  
Structural Characterization ◽  
Phosphorus Atom ◽  
Starting Material ◽  
Spectroscopy Data ◽  
X Ray

Phosphole-fused π-conjugated acenes have been attracting interest because of the attractive features of the phosphole moiety, such as fluorescence and chemically modifiable properties. Herein, 6-phenyl-6H-benzo[f]naphtho[2,3-b]phosphoindole was prepared by reacting dichlorophenylphosphine with a dilithium intermediate derived from 3,3′-dibromo-2,2′-binaphthyl. Various derivatives, such as a phospholium salt and a borane–phosphole complex with functional groups on the phosphorus atom were synthesized using the obtained phosphole as a common starting material. Single-crystal X-ray analysis of the parent benzo[f]naphtho[2,3-b]phosphoindole revealed that the pentacyclic ring is almost planar. Fluorescence spectroscopy data showed that the phosphole derivatives, such as phosphine oxide and the phospholium salt and borane complex exhibited photoluminescence in chloroform.

Absolute Stereochemistry of (-)-Wieland-Miescher Ketone as Established by the X-ray Crystallographic and CD Exciton Chirality Methods

1992 ◽  
Vol 57 (7) ◽  
pp. 1459-1465 ◽  
Author(s):  
Nobuyuki Harada ◽  
Tatsuo Sugioka ◽  
Hisashi Uda ◽  
Takeo Kuriki
Keyword(s):  
Structure Analysis ◽  
Absolute Configuration ◽  
X Ray ◽  
The Absolute ◽  
Absolute Stereochemistry

The 8aR absolute stereochemistry of Wieland-Miescher ketone (-)-I was established by the X-ray structure analysis of its bis(4-bromobenzoate) derivatives (1R,6R,8aR)-(+)-IV and (1R,6S,8aR)-(-)-V. The absolute configuration of (-)-I was corroborated further by the application of the CD exciton chirality method to bis(4-bromobenzoates) (+)-IV and (-)-V.

Synthesis of 1,2,3-Triazole-Fused Indole Derivatives via Copper-Catalyzed Cascade Reaction

Synthesis ◽  
2021 ◽  
Author(s):  
Fengtao Zhou ◽  
Qiuyu Zhang ◽  
Kashif Majeed ◽  
Bangjie Liu
Keyword(s):  
Quantum Efficiency ◽  
Photophysical Properties ◽  
Cascade Reaction ◽  
Tandem Reaction ◽  
Indole Derivatives ◽  
Wide Range

AbstractA copper-catalyzed tandem reaction has been developed for the synthesis of 1,2,3-triazole-fused indole derivatives. This protocol allowed us to access a wide range of 1,2,3-triazole-fused indole derivatives in moderate to excellent yields. The 1,2,3-triazole-fused indole derivatives emit blue and greenish light when excited at 365 nm. The products were further explored for their quantum efficiency and photophysical properties.

scholarly journals Preparative-scale HPLC Resolution of Metallacyclic η3-Allyltricarbonyliron Complexes and Determination of the Absolute Configuration by X-Ray Crystal Structure Analysis

1999 ◽  
Vol 23 (9) ◽  
pp. 578-579
Author(s):  
Rainer Schobert ◽  
Hermann Pfab ◽  
Jutta Böhmer ◽  
Frank Hampel ◽  
Andreas Werner
Keyword(s):  
Crystal Structure ◽  
Silica Gel ◽  
Structure Analysis ◽  
Absolute Configuration ◽  
Crystal Structure Analysis ◽  
Preparative Scale ◽  
X Ray ◽  
The Absolute

Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.

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