Studies on Aromatic Trichromophore Systems Incorporating Anthracene Moieties. II. Crystal Structures of 2-(9-Anthryl)-1-(9-anthrylmethyl)ethyl 2-(9-Phenanthryl)-ethyl Succinate (A2PHEN) and 2-(9-Anthryl)-1-(9-anthrylmethyl)ethyl Methyl Succinate (A2SC) and Their Fluorescence in the Solid State

1994 ◽  
Vol 47 (3) ◽  
pp. 423 ◽  
Author(s):  
M Cotrait ◽  
P Marsau ◽  
L Kessab ◽  
S Grelier ◽  
A Nourmamode ◽  
...  
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Intermolecular Interactions ◽  
Intramolecular Interactions ◽  
Van Der Waals Interactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ethyl Methyl ◽  
Molecular Fluorescence ◽  
Ester Chain

The structures of 2-(9-anthryl)-1-(9-anthrylmethyl)ethyl 2-(9-phenanthryl)ethyl succinate (A2PHEN) and 2-(9-anthryl)-1-(9-anthrylmethyl)ethyl methyl succinate (A2SC) have been determined by X-ray diffraction, and the molecular fluorescence of the crystals has been established. The two crystals are monoclinic. A2PHEN: C 2/c, a 39.47(1), b 9.718(2), c 19.924(8) Ǻ; β 97.81(3)°; R 0.036 for 2903 unique reflections. A2SC: P 21/c, a 16.248(2), b 10.325(2), c 18.052(2) Ǻ. β 114.20(3)°; R 0.044 for 2586 unique reflections. For both structures, the bisanthracene moiety and a large part of the ester chain show similar conformations. The crystal cohesion is due to intermolecular π overlapping between one of the anthracene components of the bichromophore moiety and to numerous van der Waals interactions. No intramolecular interactions between the phenanthrene and the anthracene moieties are observed in A2PHEN. The fluorescence emissions of A2PHEN and A2SC are of excimer type, and correlate well with the intermolecular interactions between the anthracene rings.

Studies on Aromatic Trichromophore Systems Incorporating Anthracene Moieties. III. Crystal Structures of 2-(9-Anthryl)-1-(9-anthrylmethyl)ethyl 2-(9-Anthryl)ethyl Succinate (A2A) and 2-(9-Anthryl)ethyl Acetate (AM) and Their Fluorescence in the Solid State

1996 ◽  
Vol 49 (1) ◽  
pp. 13 ◽  
Author(s):  
M Cotrait ◽  
H Allouchi ◽  
P Marsau ◽  
A Nourmamode ◽  
S Grelier ◽  
...  
Keyword(s):  
Solid State ◽  
Ethyl Acetate ◽  
Fluorescence Emission ◽  
Intramolecular Interactions ◽  
Van Der Waals Interactions ◽  
Dilute Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Fluorescence ◽  
Ester Chain

The structures of 2-(9-anthryl)-1-(9-anthrylmethyl)ethyl 2-(9 anthryl )ethyl succinate (A2A) and 2-(9-anthryl)ethyl acetate (AM) have been determined by X-ray diffraction, and the molecular fluorescence of the crystals has been established. The A2A crystal is triclinic while the AM crystal is monoclinic. A2A: Pī , a 18.514(5), b 11.802(3), c 10.836(3) Ǻ; α 99.63(2), β 85.75(2), γ 79.67(2)°, R 0.053 for 3547 observed reflections. AM: P21/c, a 12.566(2), b 12.991(2), c 8.805(2) Ǻ, β 97.84(1)°, R 0.040 for 1519 observed reflections. For the A2A molecule as for the previously studied A2PHEN and A2SC (see Part II), the bisanthracene moiety and a large part of the ester chain show similar conformations. The crystal cohesion is due to numerous van der Waals interactions in both compounds and to π intermolecular overlap between the anthracene moieties of neighbouring molecules of AM. The fluorescence emission of the AM crystal is of excimer type and correlates with the intermolecular stacking of the anthracene rings. In contrast, the emission from the A2A crystal was found to be very weak and with some similarity with the emission of the dilute solution. This is probably due to defects, not accounted for by the X-ray determination, permitting intramolecular interactions in the solid.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

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)◦.

Crystal structures of some eriostyl/nitrobenzoate derivatives

1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations

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.

Supramolecular architectures in two 1:1 cocrystals of 5-fluorouracil with 5-bromothiophene-2-carboxylic acid and thiophene-2-carboxylic acid

2017 ◽  
Vol 73 (6) ◽  
pp. 481-485 ◽  
Author(s):  
Marimuthu Mohana ◽  
Packianathan Thomas Muthiah ◽  
Colin D. McMillen
Keyword(s):  
Solid State ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Base Pairs ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Acid Acid ◽  
Carboxylic Acid Dimer

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.

Intermolecular interactions and electronic properties in phosphino-(oligothiophene) palladium(II) and platinum(II) complexes

2007 ◽  
Vol 85 (5) ◽  
pp. 383-391 ◽  
Author(s):  
Tracey L Stott ◽  
Michael O Wolf ◽  
Brian O Patrick
Keyword(s):  
Solid State ◽  
Metal Complexes ◽  
Electronic Properties ◽  
Crystal Structures ◽  
Structural Properties ◽  
Absorption Spectra ◽  
Intermolecular Interactions ◽  
Electronic Spectra ◽  
X Ray ◽  
Π Stacking

A series of Pt(II) and Pd(II) complexes containing diphenylphosphino-substituted oligothiophene ligands ranging from 1 to 3 thiophene rings in length have been prepared. Crystal structures of four of these complexes were determined via single X-ray crystal diffraction and the solid-state packing arrangements found to vary with both the metal and the thiophene-containing ligand. In some cases, π-stacking between thiophene rings are found for the oligothiophene ligands. Solution and solid-state absorption spectra of these complexes are reported.Key words: oligothiophenes, metal complexes, structural properties, electronic spectra.

Structure and conformational analysis of a bidentate pro-ligand, C21H34N2S2, from powder synchrotron diffraction data and solid-state DFTB calculations

2009 ◽  
Vol 65 (5) ◽  
pp. 639-646 ◽  
Author(s):  
Edward E. Ávila ◽  
Asiloé J. Mora ◽  
Gerzon E. Delgado ◽  
Ricardo R. Contreras ◽  
Luis Rincón ◽  
...  
Keyword(s):  
Solid State ◽  
Diffraction Data ◽  
Density Functional ◽  
Simulated Annealing Algorithm ◽  
Theoretical Calculations ◽  
Tight Binding ◽  
Van Der Waals Interactions ◽  
Am1 Calculations ◽  
X Ray Diffraction ◽  
X Ray

The molecular and crystalline structure of ethyl 1′,2′,3′,4′,4a′,5′,6′,7′-octahydrodispiro[cyclohexane-1,2′-quinazoline-4′,1′′-cyclohexane]-8′-carbodithioate (I) was solved and refined from powder synchrotron X-ray diffraction data. The initial model for the structural solution in direct space using the simulated annealing algorithm implemented in DASH [David et al. (2006). J. Appl. Cryst. 39, 910–915] was obtained performing a conformational study on the fused six-membered rings of the octahydroquinazoline system and the two spiran cyclohexane rings of (I). The best model was chosen using experimental evidence from 1H and 13C NMR [Contreras et al. (2001). J. Heterocycl. Chem. 38, 1223–1225] in combination with semi-empirical AM1 calculations. In the refined structure the two spiran rings have the chair conformation, while both of the fused rings in the octahydroquinazoline system have half-chair conformations compared with in-vacuum density-functional theory (DFT) B3LYP/6-311G*, DFTB (density-functional tight-binding) theoretical calculations in the solid state and other related structures from X-ray diffraction data. Compound (I) presents weak intramolecular hydrogen bonds of the type N—H...S and C—H...S, which produce delocalization of the electron density in the generated rings described by graph symbols S(6) and S(5). Packing of the molecules is dominated by van der Waals interactions.

Crystal Structures of New Compounds Na0.5Sm4.5Ti4O15 and Na0.5Eu4.5Ti4O15

2011 ◽  
Vol 415-417 ◽  
pp. 468-471
Author(s):  
Qiao Hong Yu ◽  
Zheng Fa Li ◽  
Yong Xiang Li ◽  
Ping Zhan Si ◽  
Jiang Ying Wang ◽  
...  
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ordinary Temperature ◽  
Europium Titanate ◽  
New Compounds

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.

Crystal Structures of Cyclosporin Derivatives: O-Acetyl-(4R)-4-(E-2-butyl)-4,N-dimethyl-L-threonyl-cyclosporin A and O-Acetyl-(4R)-4-[E-2-(4-bromobutyl)]-4,N-dimethyl-L-threonyl-cyclosporin A

1999 ◽  
Vol 64 (1) ◽  
pp. 89-98 ◽  
Author(s):  
Bohumil Kratochvíl ◽  
Alexandr Jegorov ◽  
Svetlana Pakhomova ◽  
Michal Hušák ◽  
Petr Bulej ◽  
...  
Keyword(s):  
Solid State ◽  
Cyclosporin A ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

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.

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