Soluble Pyridine Complexes Of The Ternary Gallium(III) Chalcogenide Halides (GaEX)3, With E = S, Se And X = Cl, Br

2001 ◽  
Vol 56 (8) ◽  
pp. 711-718 ◽  
Author(s):  
Stefan D. Nogai ◽  
Annette Schier ◽  
Hubert Schmidbaur
Keyword(s):  
Single Crystal ◽  
Molecular Complexes ◽  
Membered Ring ◽  
New Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Ligands ◽  
Ring Molecules ◽  
Gallium Metal ◽  
Convenient Preparation

The four ternary gallium(III) chalcogenide halides GaEX with E = S, Se and X = Cl, Br can be prepared a) from the binary gallium(III) chalcogenides Ga2E3 and halides Ga2X6, b) from gallium(I) tetrahalogallates(III) GafGaX4] and the chalcogen E, and c) from gallium metal and the dichalcogen dihalides E2X2. The new method c) was shown to be the most convenient preparation. The products are readily soluble in pyridine to give trinuclear molecular complexes [GaEX·Py]3 which are not volatile without decomposition, but can be purified by crystallization. The structures have been determined by single crystal X-ray diffraction techniques. The two chlorides are isostructural and show twisted tub-form six-membered ring molecules with the pyridine donors in axial positions. The two bromides are also isostructural, but with the pyridine ligands in two axial and one equatorial positions

Conformational Comparisons Between Phenoxyacetic Acid Derivatives in Adducts and in the Free Form

1999 ◽  
Vol 52 (7) ◽  
pp. 695 ◽  
Author(s):  
Graham Smith ◽  
Catherine J. Cooper ◽  
Veena Chauhan ◽  
Daniel E. Lynch ◽  
Simon Parsons ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Single Crystal ◽  
Free Acid ◽  
Molecular Complexes ◽  
The Other ◽  
Free Form ◽  
Phenoxyacetic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dichlorophenoxy Acetic Acid

Six molecular complexes containing the herbicidally active (2,4-dichlorophenoxy)acetic acid (2,4-d) and (2,4,5-trichlorophenoxy)acetic acid (2,4,5-t) have been prepared and studied by using single-crystal X-ray diffraction techniques. These adduct structures are 2,4-d with 4,4′-dipyridine (2 : 1 complex), and 2,4,5-t with respectively 5-nitroquinoline (1 : 1), 4,4′-dipyridine (2 : 1), 2-amino-2-thiazoline (1 : 1), 2-aminobenzothiazole (1 : 1) and 2-amino-5-ethyl-1,3,4-thiadiazole (1 : 1). The conformations of the phenoxyacetic acid molecules were found to be either synclinal (in three cases) or antiperiplanar (in the other three cases). A general review is also made about the conformational aspects of previously reported adducts of phenoxyacetic acid derivatives and how they compare to their free acid structures.

Synthesis of an Oxaspirolactone Intermediate for the Synthesis of Spirolides

2000 ◽  
Vol 53 (10) ◽  
pp. 845 ◽  
Author(s):  
Margaret A. Brimble ◽  
Fares A. Fares ◽  
Peter Turner
Keyword(s):  
Carboxylic Acid ◽  
Single Crystal ◽  
Building Block ◽  
New Method ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

A new method has been established for the preparation of C 2-oxidized 5,5-spiroacetals, which are key intermediates for the synthesis of the bis-spiroacetal moiety of the spirolides. A bridged orthoester was used as a masked carboxylic acid in the preparation of these bicyclic oxaspirolactones. The synthesis of chiral lactone (12), a building block for the synthesis of the spirolides, is also reported. The two chiral centres in lactone (12) were assembled by addition of a chiral crotyl borane to an aldehyde. The structure of lactone (12) was determined by single-crystal X-ray diffraction; orthorhombic space group P212121 (No. 19), a 12.437(2), b 23.881(4), c 7.545(1) Å, V 2240.9(5) Å3, R(F) 0.0460, and Rw(F) 0.0458.

Crystal structure of zerumbone [(E,E,E)-2,6,9,9-Tetramethylcycloundeca-2,6,10-trien-1-one]

1981 ◽  
Vol 34 (10) ◽  
pp. 2243 ◽  
Author(s):  
SR Hall ◽  
S Nimgirawath ◽  
CL Raston ◽  
A Sittatrakul ◽  
S Thadaniti ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Zingiber Zerumbet ◽  
Space Group ◽  
X Ray ◽  
Considerable Distortion

The crystal structure of zerumbone, C15H22O, extracted from the rhizomes of Zingiber zerumbet Smith, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.051 for 925 'observed' reflections. Crystals are monoclinic, space group P21/c, a 9.036(3), b 9.712(5), c 15.643(6) �, β 97.19(3)�, Z = 4. Although the molecule has no chiral centre, the presence of the three trans double bonds confers considerable distortion and rigidity on the eleven-membered ring and renders the whole molecule chiral and potentially resolvable.

scholarly journals A pyridyl-substituted cyclodisilazane [(Apy)2(μ-SiMe)2] (ApyH2 = 2-aminopyridine)

IUCrData ◽  
2017 ◽  
Vol 2 (3) ◽  
Author(s):  
Rui Li ◽  
Xin-E Duan ◽  
Wei Cao ◽  
Xue-Hong Wei
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Title Compound ◽  
Membered Ring ◽  
Side Product ◽  
Inversion Center ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compound C

The title compound, C14H20N4Si2 or [(Apy)2(μ-SiMe)2], systematic name 2-[2,2,4,4-tetramethyl-3-(pyridin-2-yl)-1,3,2,4-diazadisiletidin-1-yl]pyridine, was obtained as a side product from the reaction of 2-amino-pyridine with LiBu n followed by the addition of Me2NMe2SiCl in hexane. The compound was characterized by single-crystal X-ray diffraction analysis and NMR spectroscopy. The title compound lies about an inversion center at the centroid of the cyclodisilazane ring. The four-membered Si2N2 core is strictly planar with the two pyridyl rings placed centrosymmetrically on either side of the Si2N2 plane and are almost coplanar with the central four-membered ring.

Combined Single-Crystal X-ray Diffraction and FTIR Study of Morpholinium−Water Molecular Complexes Embedded in a Chabasite Network

2003 ◽  
Vol 107 (36) ◽  
pp. 9655-9661 ◽  
Author(s):  
Annalisa Martucci ◽  
Alberto Alberti ◽  
Giuseppe Cruciani ◽  
Alberto Frache ◽  
Salvatore Coluccia ◽  
...  
Keyword(s):  
Single Crystal ◽  
Molecular Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ftir Study

Arene–perfluoroarene interactions in crystal engineering. Part 14. 1:1 Complexes of octafluoronaphthalene with fluorene and 9,10-dihydrophenanthrene

2006 ◽  
Vol 84 (2) ◽  
pp. 238-242 ◽  
Author(s):  
Jonathan C Collings ◽  
Andrei S Batsanov ◽  
Judith AK Howard ◽  
Todd B Marder
Keyword(s):  
Single Crystal ◽  
Key Words ◽  
Crystal Engineering ◽  
Molecular Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Face To Face ◽  
Π Stacking

The 1:1 molecular complexes of octafluoronaphthalene (OFN) with fluorene (1) and with 9,10-dihydrophenanthrene (2) were prepared by cocrystallization of the components and characterized by single-crystal X-ray diffraction. The structure of 1 can be described as a mixed-stack or a laminar checkerboard motif of alternating OFN and fluorene molecules, whilst slanted mixed-stack, herringbone, and face-to-face heteromolecular dimer motifs can all be recognised in 2.Key words: single crystal, X-ray structure, π stacking, fluoroarene.

scholarly journals Crystal Structures of Two Macrocyclic Bischalcones Possessing 26-Membered Rings

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Rina Mondal ◽  
Nayim Sepay ◽  
Debajyoti Ghoshal ◽  
Asok K. Mallik
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Single crystal X-ray diffraction of two macrocyclic bischalcones, namely, (2E,25E)-11,17,33,37-tetraoxapentacyclo[36.4.0.05,10.018,23.027,32]dotetraconta-1(42),2,5,7,9,18,20,22,25,27,29,31,38,40-tetradecaene-4,24-dione(1) and (2E,24E)-11,16,32,37-tetraoxapentacyclo[36.4.0.05,10.017,22.026,31]dotetraconta-1(42),2,5,7,9,17,19,21,24,26,28,30,38,40-tetradecaene-4,23-dione(2), each containing a 26-membered ring, has been studied. Compound 1 belongs to the monoclinic system, space group C2/c with a = 34.3615(9) Å, b = 12.7995(3) Å, c = 14.6231(3) Å, β = 96.912(2)°,  V = 6,384.6(3) Å3, and Z = 8. Compound 2 is triclinic, space group P-1 with a = 10.066(2) Å, b = 10.670(3) Å, c = 16.590(3) Å, α = 85.95(2), β = 89.244(14), γ = 62.211(13), V = 1572.0(6) Å3, and Z = 2. Intermolecular C–H⋯O hydrogen bonding interactions are present in both compounds.

scholarly journals Self-assembly of metallosupramolecular rhombi from chiral concave 9,9’-spirobifluorene-derived bis(pyridine) ligands

2014 ◽  
Vol 10 ◽  
pp. 432-441 ◽  
Author(s):  
Rainer Hovorka ◽  
Sophie Hytteballe ◽  
Torsten Piehler ◽  
Georg Meyer-Eppler ◽  
Filip Topić ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Self Assembly ◽  
The Self ◽  
Assembly Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Ligands ◽  
Racemic Form

Two new 9,9’-spirobifluorene-based bis(4-pyridines) were synthesised in enantiopure and one also in racemic form. These ligands act as concave templates and form metallosupramolecular [(dppp)2M2L2] rhombi with cis-protected [(dppp)Pd]2+ and [(dppp)Pt]2+ ions. The self-assembly process of the racemic ligand preferably occurs in a narcissistic self-recognising manner. Hence, a mixture of all three possible stereoisomers [(dppp)2M2{(R)-L}2](OTf)4, [(dppp)2M2{(S)-L}2](OTf)4, and [(dppp)2M2{(R)-L}{(S)-L}](OTf)4 was obtained in an approximate 1.5:1.5:1 ratio which corresponds to an amplification of the homochiral assemblies by a factor of approximately three as evidenced by NMR spectroscopy and mass spectrometry. The racemic homochiral assemblies could also be characterised by single crystal X-ray diffraction.

scholarly journals Determining hydrogen positions in crystal engineered organic molecular complexes by joint neutron powder and single crystal X-ray diffraction

CrystEngComm ◽  
2014 ◽  
Vol 16 (7) ◽  
pp. 1232-1236 ◽  
Author(s):  
Marc Schmidtmann ◽  
Paul Coster ◽  
Paul F. Henry ◽  
Valeska P. Ting ◽  
Mark T. Weller ◽  
...  
Keyword(s):  
Single Crystal ◽  
Molecular Complexes ◽  
X Ray Diffraction ◽  
X Ray
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