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 Manipulating the Conformation of 3,2′:6′,3″-Terpyridine in [Cu2(μ-OAc)4(3,2′:6′,3″-tpy)]n 1D-Polymers

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 182-198
Author(s):  
Dalila Rocco ◽  
Samantha Novak ◽  
Alessandro Prescimone ◽  
Edwin C. Constable ◽  
Catherine E. Housecroft
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Metal Binding ◽  
Polymer Chains ◽  
X Ray Diffraction ◽  
Face To Face ◽  
Single Crystal Structures ◽  
Π Stacking ◽  
Metal Binding Domain ◽  
Packing Interactions

We report the preparation and characterization of 4′-([1,1′-biphenyl]-4-yl)-3,2′:6′,3″-terpyridine (1), 4′-(4′-fluoro-[1,1′-biphenyl]-4-yl)-3,2′:6′,3″-terpyridine (2), 4′-(4′-chloro-[1,1′-biphenyl]-4-yl)-3,2′:6′,3″-terpyridine (3), 4′-(4′-bromo-[1,1′-biphenyl]-4-yl)-3,2′:6′,3″-terpyridine (4), and 4′-(4′-methyl-[1,1′-biphenyl]-4-yl)-3,2′:6′,3″-terpyridine (5), and their reactions with copper(II) acetate. Single-crystal structures of the [Cu2(μ-OAc)4L]n 1D-coordination polymers with L = 1–5 have been determined, and powder X-ray diffraction confirms that the single crystal structures are representative of the bulk samples. [Cu2(μ-OAc)4(1)]n and [Cu2(μ-OAc)4(2)]n are isostructural, and zigzag polymer chains are present which engage in π-stacking interactions between [1,1′-biphenyl]pyridine units. 1D-chains nest into one another to give 2D-sheets; replacing the peripheral H in 1 by an F substituent in 2 has no effect on the solid-state structure, indicating that bifurcated contacts (H...H for 1 or H...F for 2) are only secondary packing interactions. Upon going from [Cu2(μ-OAc)4(1)]n and [Cu2(μ-OAc)4(2)]n to [Cu2(μ-OAc)4(3)]n, [Cu2(μ-OAc)4(4)]n, and [Cu2(μ-OAc)4(5)]n·nMeOH, the increased steric demands of the Cl, Br, or Me substituent induces a switch in the conformation of the 3,2′:6′,3″-tpy metal-binding domain, and a concomitant change in dominant packing interactions to py–py and py–biphenyl face-to-face π-stacking. The study underlines how the 3,2′:6′,3″-tpy domain can adapt to different steric demands of substituents through its conformational flexibility.

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.

scholarly journals High pressure studies of L-Serine-L-Ascorbic acid co-crystal

2014 ◽  
Vol 70 (a1) ◽  
pp. C988-C988
Author(s):  
Sergey Arkhipov ◽  
Boris Zakharov ◽  
Elena Boldyreva
Keyword(s):  
High Pressure ◽  
Ascorbic Acid ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Crystal Engineering ◽  
Mixed Crystals ◽  
Study Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range

"Experiments for studying crystalline materials under extreme conditions are a powerful tool for investigating ""structure-property"" relationships. They also give information on the behavior of hydrogen bonds and are important both for materials science and crystal engineering. In addition, many processes in the living organisms are also related to mechanical stress. One of the most interesting tasks is to identify factors which influence the stability of a structure, or a part of the structure, at high pressure. Experiments on the systematic study of compounds in a wide range of pressures allow us to accumulate data that can be used to solve this problem. For a more complete picture, the mixed crystals of the selected compound are studied. Investigation of mixed crystals and cocrystals of interest can be compared with the crystals of individual compounds. We have chosen the structure of L-serine - L-ascorbic acid to be compared with those of L-serine and L-ascorbic acids for such a study. Phase transitions were previously reported to be induced by increasing pressure in both L-serine [1] and L-ascorbic acid [2]; moreover, the structure of L-serine was followed at multiple pressures by single-crystal and powder X-ray diffraction[3]. L-serine – L-ascorbic acid co-crystal was studied in the pressure range 0-5.4 GPa (at multiple points at every 0.5-0.7 GPa) by single-crystal X-ray diffraction and Raman spectroscopy. A phase transition has been detected and some rearrangement in the network of hydrogen bonds was observed. The high pressure data were compared with those for the individual structures of the L-serine and L-ascorbic acid. This work was supported by RFBR (grants 12–03-31541, 14-03-31866, 13-03-92704, 14-03-00902 ), Ministry of Science and Education of Russia and Russian Academy of Sciences."

The Syntheses and Structures of Two New Zn(II) Complexes Based on 3-Nitrobenzoato Ligand

2013 ◽  
Vol 807-809 ◽  
pp. 2671-2674
Author(s):  
Ying Bing Lu ◽  
Fang Mei Jian ◽  
Shuang Jin
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Face To Face ◽  
Π Interactions ◽  
Carboxylate Groups ◽  
Supramolecular Chain ◽  
Supramolecular Layer

Two new Zn (II) coordination polymers with 3-nitrobenzoato ligands have been prepared, and their structures have been characterized by single-crystal X-ray diffraction techniques. The structure of [Zn (3-nbz)2(μ-4,4'-bpy)]n(1) (3-nbz = 3-nitrobenzoato, 4,4'-bpy = 4,4'-bipyridine) shows 1-D chains originating from terminal 3-nbz ligands andμ-4,4'-bpy molecules. The chains are further connected through face-to-face π stacking interactions to genenate a 2-D supramolecular layer. In Zn (3-nbz)2(2,2'-bpy) (2) (2,2'-bpy = 2,2'-bipyridine), carboxylate groups exhibit chelated bidentate to give discrete mononuclear units, which are linked by face-to-face π-π and C-H···π interactions to produce a 1-D supramolecular chain.

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

A clothes-peg-shaped binucleartrans-bis(2-aminotroponato)palladium(II) complex bearing pentamethylene spacers

2013 ◽  
Vol 69 (5) ◽  
pp. 503-505 ◽  
Author(s):  
Naruyoshi Komiya ◽  
Takeharu Kageyama ◽  
Masaya Naito ◽  
Takeshi Naota
Keyword(s):  
Single Crystal ◽  
Mass Spectroscopy ◽  
Crystalline State ◽  
Palladium Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Π Stacking ◽  
Ft Ir ◽  
Molecular Unit

rac-Bis{μ-trans-2,2′-[pentane-1,5-diylbis(azanediyl)]ditroponato}dipalladium(II), [Pd2(C19H20N2O2)2], has been synthesized and fully characterized using single-crystal X-ray diffraction,1H NMR, FT–IR and mass spectroscopy. Thetranscoordination, vaulted structure andanticonformation have been unequivocally established from the X-ray diffraction studies. This is the first example of a bis(aminotroponato)palladium complex. In the crystalline state, the molecule has twofold symmetry and each molecular unit undergoes intermolecular offset π-stacking of the tropone rings to afford heterochiral interpenetrating dimers that are aligned in a lamellar manner with a herringbone packing motif.

Eindimensionale Kupfer(II)-Koordinationspolymere: Kristall-Engineering durch variable Verknüpfungsmuster [1] / One Dimensional Copper(II) Coordination Polymers: Crystal Engineering through Variable Types of Linkage [1]

1997 ◽  
Vol 52 (1) ◽  
pp. 125-134 ◽  
Author(s):  
Rolf W. Saalfrank ◽  
Roland Harbig ◽  
Oliver Struck ◽  
Frank Hampel ◽  
Eva Maria Peters ◽  
...  
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Crystal Engineering ◽  
Coordination Compounds ◽  
Acetate Solution ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
1D Coordination Polymer

Reaction of a methanolic copper(II) acetate solution with tetrazolyl enol derivatives 2a or 2b leads to the formation of the corresponding lD-coordination polymer 1∞[CuL2] 3a and pseudo 1D-coordination polymer [CuL2]2 3b, respectively. On the contrary, reaction of 2c with methanolic copper(II) acetate solution yields OH-bridged 1D-coordination polymer 1∞[CuL2(MeOH)2 3c. Single-crystal X-ray diffraction of the supramolecular species 3 established unequivocally the structures of the stairlike coordination compounds. Reaction of a methanolic copper(II) acetate solution with amidotetrazole derivative 6 leads to the formation of the lD-coordination polymer 1∞ [CuL2] 7. The structure of 7 has been established by X-ray structure analysis

Bifunctional bis(oxazolines) as potential ligands in catalytic asymmetric reactions

2004 ◽  
Vol 82 (2) ◽  
pp. 306-313 ◽  
Author(s):  
Stephen Hanessian ◽  
Eric Jnoff ◽  
Noemy Bernstein ◽  
Michel Simard
Keyword(s):  
Single Crystal ◽  
Key Words ◽  
Enantiomeric Excess ◽  
Asymmetric Reactions ◽  
Potential Utility ◽  
X Ray Diffraction ◽  
Asymmetric Addition ◽  
X Ray ◽  
Oxazoline Ligands ◽  
Cu Complexes

C2-symmetrical bis(oxazoline) ligands bearing pendant alkylthio ether groups were synthesized, and the structures of Cu complexes were determined by single crystal X-ray diffraction. The potential utility in catalysis was shown in the asymmetric addition of methyllithium to an aromatic aldimine, which resulted in a mixture of products with an enantiomeric excess of 68%.Key words: two-center catalysis, bis(oxazoline), aldimine, imine alkylation.

scholarly journals A 1:1 energetic co-crystal formed between trinitrotoluene and 2,3-diaminotoluene

2018 ◽  
Vol 37 (1) ◽  
pp. 61 ◽  
Author(s):  
Nilgun Sen
Keyword(s):  
Single Crystal ◽  
Intermolecular Interactions ◽  
Crystal Packing ◽  
Main Mechanism ◽  
Oxygen Balance ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fingerprint Plots ◽  
Hirshfeld Surfaces ◽  
Π Stacking

A 1:1 co-crystal of trinitrotoluene (TNT) and 2,3-diaminotoluene was prepared by solvent evapo- ration, and the structure of the co-crystal was determined by single-crystal and powder X-ray diffraction. The results indicate that the main mechanism of co-crystallization originates from the intermolecular hy- drogen bonding (amino-nitro) and π-π stacking. We also examined the Hirshfeld surfaces and associated fingerprint plots of the co-crystal and reveal that the structures are stabilized by H…H, O–H, O…O and C…C (π-π) intermolecular interactions. We analyzed the crystal packing and show its influence upon im- pact sensitivity. The results highlight that co-crystallization is an effective way to modify the sensitivity, oxygen balance and density of explosives. 

scholarly journals Synthesis, characterization and crystal structure of platinum(II) complexes with thiourea derivative ligands

2018 ◽  
Vol 9 (4) ◽  
pp. 360-368
Author(s):  
Ebru Keskin ◽  
Ummuhan Solmaz ◽  
Gun Binzet ◽  
Ilkay Gumus ◽  
Hakan Arslan
Keyword(s):  
Single Crystal ◽  
Weak Interactions ◽  
Platinum Complexes ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Thiourea Derivatives ◽  
X Ray ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
In Cis

Thiourea derivatives [N-(di-n-propylcarbamothioyl)-4-fluorobenzamide (HL1) and N-(di-n-propylcarbamothioyl)-4-bromobenzamide (HL2)] and their platinum complexes have been successfully synthesized and structurally characterized by spectroscopic 1H NMR, 13C NMR, COSY, HMQC, and FT-IR techniques. The structure of both complexes was also confirmed by single crystal X-ray diffraction studies. The study of X-ray single crystal diffraction shows that the supramolecular aggregation of the complexes is stabilized via weak interactions as well as stacking interactions such as C-H···π and π···π. The cis-[Pt(L1-S,O)2 showed C–H···π and π···π stacking interactions, whereas only C–H···π stacking interaction was observed in cis-[Pt(L2-S,O)2]. In addition, the strong classical and non-classical intermolecular hydrogen bonds are not found in the prepared complexes. Therefore, it can be said that the C–H···π and π···π stacking interactions play an important role in the formation of supramolecular structures of the complexes.

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