Distibylation of Acetylenes with Ph2Sb–SbPh2: Synthesis, Crystal Structures and Phosphorescence Properties of Bis(diphenylstibyl)ethenes

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1181-1187
Author(s):  
Joji Ohshita ◽  
Toshiyuki Tsuchida ◽  
Kazuya Murakami ◽  
Yousuke Ooyama ◽  
Takayuki Nakanishi ◽  
...  

Abstract Treatment of tetraphenyldistibine (1) with terminal arylacetylenes, XC6H5C≡CH (2a-c, X=H, F, OMe), gave the corresponding anti-addition products (E)-aryl-1,2-bis(diphenylstibyl)ethenes 3a-c in 11 - 17% yields. A similar reaction of 1 with 1,4-diphenylbutadiyne provided (E)-1,4-diphenyl- 1,2-bis(diphenylstibyl)but-1-en-3-yne (3d) in 28% yield. X-Ray diffraction studies on crystals of 3a, 3b and 3d revealed a congested configuration around the ethylene core. The optical properties of the adducts 3a-d were examined by measuring UV absorption and photoluminescence spectra. Interestingly, 3d showed phosphorescence in the solid state, which was enhanced at low temperature.

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.


2014 ◽  
Vol 6 (2) ◽  
pp. 217-231 ◽  
Author(s):  
F. Khatun ◽  
M. A. Gafur ◽  
M. S. Ali ◽  
M. S. Islam ◽  
M. A. R. Sarker

The lithium-cobalt oxide LixCoO2 is a promising candidate as highly active cathode material of lithium ion rechargeable batteries. The crystalline-layered lithium cobaltite has attracted increased attention due to recent discoveries of some extraordinary properties such as unconventional transport and magnetic properties. Due to layered crystal structure, Li contents (x) in LixCoO2 might play an important role on its interesting properties. LiCoO2 crystalline cathode material was prepared by using solid-state reaction synthesis, and then LixCoO2 (x<1) has been synthesized by deintercalation of produced single-phase powders. Structure and morphology of the synthesized powders were investigated by X-ray diffraction (XRD), Infrared spectroscopy, Impedance analyzer etc. The influence of lithium composition (x) on structural, electronic and optical properties of lithium cobaltite was studied. Temperature dependent electrical resistivity was measured using four-probe technique. While LixCoO2 with x = 0.9 is a semiconductor, the highly Li-deficient phase (0.75 ? x ? 0.5) exhibits metallic conductivity. The ionic conductivity of LixCoO2 (x = 0.5 – 1.15) was measured using impedance spectroscopy and maximum conductivity of Li0.5CoO2 was found to be 6.5×10-6 S/cm at 273 K. The properties that are important for applications, such as ionic conductivity, charge capacity, and optical absorption are observed to increase with Li deficiency. Keywords: Calcination; Characterization; Inorganic compounds; Solid-State reaction; X-ray diffraction. © 2014 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.doi: http://dx.doi.org/10.3329/jsr.v6i2.17900 J. Sci. Res. 6 (2), 217-231 (2014)  


1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.


2017 ◽  
Vol 73 (6) ◽  
pp. 481-485 ◽  
Author(s):  
Marimuthu Mohana ◽  
Packianathan Thomas Muthiah ◽  
Colin D. McMillen

In solid-state engineering, cocrystallization is a strategy actively pursued for pharmaceuticals. Two 1:1 cocrystals of 5-fluorouracil (5FU; systematic name: 5-fluoro-1,3-dihydropyrimidine-2,4-dione), namely 5-fluorouracil–5-bromothiophene-2-carboxylic acid (1/1), C5H3BrO2S·C4H3FN2O2, (I), and 5-fluorouracil–thiophene-2-carboxylic acid (1/1), C4H3FN2O2·C5H4O2S, (II), have been synthesized and characterized by single-crystal X-ray diffraction studies. In both cocrystals, carboxylic acid molecules are linked through an acid–acid R 2 2(8) homosynthon (O—H...O) to form a carboxylic acid dimer and 5FU molecules are connected through two types of base pairs [homosynthon, R 2 2(8) motif] via a pair of N—H...O hydrogen bonds. The crystal structures are further stabilized by C—H...O interactions in (II) and C—Br...O interactions in (I). In both crystal structures, π–π stacking and C—F...π interactions are also observed.


2011 ◽  
Vol 415-417 ◽  
pp. 468-471
Author(s):  
Qiao Hong Yu ◽  
Zheng Fa Li ◽  
Yong Xiang Li ◽  
Ping Zhan Si ◽  
Jiang Ying Wang ◽  
...  

New compounds of sodium samarium titanate Na0.5Sm4.5Ti4O15and sodium europium titanate Na0.5Eu4.5Ti4O15were synthesized successfully by solid state reaction at 1300 oC and 1200 oC, respectively. The lattice parameters of Na0.5Sm4.5Ti4O15and Na0.5Eu4.5Ti4O15were determined at ordinary temperature by using X-ray powder diffraction method. Their Lattice types were determined, and their patterns were indexed. Polycrystalline X-ray diffraction data of sodium samarium titanate were listed. Differences of their crystal structures were analyzed and discussed.


1999 ◽  
Vol 64 (1) ◽  
pp. 89-98 ◽  
Author(s):  
Bohumil Kratochvíl ◽  
Alexandr Jegorov ◽  
Svetlana Pakhomova ◽  
Michal Hušák ◽  
Petr Bulej ◽  
...  

The structures of O-acetyl-(4R)-4-(E-2-butyl)-4,N-dimethyl-L-threonyl-cyclosporin A (1) and O-acetyl-(4R)-4-[E-2-(4-bromobutyl)]-4,N-dimethyl-L-threonyl-cyclosporin A (2) were determined by X-ray diffraction methods and compared with the structure of related cyclosporins. In contrast to expectation, neither the acetylation nor the subsequent bromination of 1 affects the conformation and packing of cyclosporins in the solid state. Both compounds are isomorphous and crystallize in the orthorhombic space group P212121 with a = 12.936(2) Å, b = 15.590(2) Å, c = 36.280(3) Å, and a = 12.916(3) Å, b = 15.675(4) Å, c = 36.715(7) Å, for 1 and 2, respectively.


2021 ◽  
Vol 904 ◽  
pp. 329-333
Author(s):  
Qun Si Wang ◽  
Jun Feng Ma ◽  
Tian Qing Cui ◽  
Dong Bin Tang ◽  
Qi Zhou

M2SiO4: Tb3+, Mn2+, Nd3+ (M = Mg2+, Ca2+, Sr2+, and Ba2+) phosphors suitable for near-ultraviolet-violet radiation excitation were successfully prepared at 1400 °C in N2 atmosphere by a high-temperature solid-state reaction, and their phase compositions and luminescent performance were also studied by X-ray diffraction (XRD), photoluminescence spectra. Results show that their emission intensity increases in the order of Ca2SiO4 > Mg2SiO4 > Sr2SiO4 > Ba2SiO4 matrix phosphor. Ca1.94SiO4: 0.02Tb3 +, 0.02Mn2+, 0.02Nd2+ phosphor exhibits the best luminescence performance.


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