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CRYSTALLOGRAPHIC
COMMUNICATIONS

Volume 79| Part 8

ISSN: 2056-9890

August 2023 issue

Cover illustration: Three new Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamine have been synthesized and structurally characterized. They exist as enamine tautomers that contain nearly planar amino-methylene-pentane-2,4-dione cores. The main structural differences between the compounds arise from conformational aspects regarding the orientation of the CH₂Ph, CH(CH₃)Ph and C(CH₃)₃ moieties. In order to obtain some insight into how the observed conformations are influenced by the crystal packing, the gas-phase molecular structures of these compounds were optimized by DFT methods. See: Halz, Hentsch, Wagner & Merzweiler [Acta Cryst. (2023). E78, 707–713].

research communications

Co-crystallization of N′-benzylidenepyridine-4-carbohydrazide and benzoic acid via autoxidation of benzaldehyde

I. B. Setshedi, A. Lemmerer and M. G. Smith

The 1:1 co-crystal N′-[(2-methylphenyl)methylidene]pyridine-4-carbohydrazide–benzoic acid (1/1) formed unexpectedly after autoxidation of benzaldehyde during the slow evaporation process of a solution of isoniazid in benzaldehyde. The original intent of the synthesis was to modify isoniazid with benzaldehyde and crystallize the product in order to improve efficacy against Mycobacteria species, but benzoic acid formed spontaneously and co-crystallized with the intended product, N′-benzylidenepyridine-4-carbohydrazide.

CCDC reference: 2250754

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Synthesis, crystal structure and Hirshfeld surface analysis of naphthalene-2,3-diyl bis(3-benzyloxy)benzoate

H. Anil Kumar, S. Selvanandan, H. T. Srinivasa, G. Venkateshappa and B. S. Palakshamurthy

In the title compound, C₃₈H₂₈O₆, the dihedral angles between the naphthalene ring system and its pendant benzyloxy rings A and B are 88.05 (7) and 80.84 (7)°, respectively. The dihedral angles between the A and B rings and their attached phenyl rings are 49.15 (8) and 80.78 (8)°, respectively. In the extended structure, the molecules are linked by weak C—H⋯O and C—H⋯π bonds and π–π stacking interactions, which variously generate C(11) chains and $[R_{2}^{2}]$ (12) loops as part of a three-dimensional network. The Hirshfeld surface [fingerprint contributions = H⋯H (42.3%), C⋯H/H⋯C (40.3%) and O⋯H/H⋯O (15.7%)] and intermolecular interaction energies are reported, with dispersion, E_dis at −428.6 kJ mol⁻¹ being the major contributor.

CCDC reference: 2271880

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Crystal structures and Hirshfeld surface analyses of N,N-dimethylacetamide–1-(dimethyl-λ⁴-azanylidene)ethan-1-ol tribromide (1/1), N,N-dimethylacetamide–1-(dimethyl-λ⁴-azanylidene)ethan-1-ol dibromidoiodate (1/1) and N,N-dimethylacetamide–1-(dimethyl-λ⁴-azanylidene)ethan-1-ol dichloridoiodate (1/1)

G. Z. Mammadova, D. F. Mertsalov, D. M. Shchevnikov, M. S. Grigoriev, M. Akkurt, S. Ö. Yıldırım and A. Bhattarai

In all three title crystals, the cations are linked by O—H⋯O and/or C—H⋯O hydrogen bonds. The three-dimensional packing is further consolidated by strong halogen–hydrogen and weak van der Waals interactions.

CCDC references: 2271693; 2271692; 2271691

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Synthesis and crystal structure of a bench-stable pyridinium ketene hemiaminal: 1-(1-ethoxyethenyl)-2-[methyl(phenyl)amino]pyridin-1-ium trifluoromethanesulfonate

Z. A. Krevlin, I. C. Bote, M. C. F. Crespo, C. C. Lam, C. D. McMillen and M. M. Majireck

The N-quaternized ketene N,O-acetal, 1-(1-ethoxyvinyl)-2-(methyl(phenyl)amino)pyridin-1-ium trifluoromethanesulfonate was synthesized and its structure determined, making it a rare example of this class of compounds to be structurally characterized.

CCDC reference: 2278022

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(NH₄)₂[UO₂Cl₄]·2H₂O, a new uranyl tetrachloride with ammonium charge-balancing cations

T. A. Kohlgruber and R. G. Surbella III

While several actinyl tetrahalides have been synthesized and their structures reported, (NH₄)₂(UO₂Cl₄)·2H₂O represents a new uranyl tetrachloride salt synthesized in a slow evaporation from a 2 M hydrochloric acid solution. Its optical properties were measured by diffuse reflectance and luminescence spectroscopies, while powder X-ray diffraction confirmed an ammonium chloride impurity phase.

CCDC reference: 2278035

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Synthesis and crystal structures of three Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamine

J. H. Halz, A. Hentsch, C. Wagner and K. Merzweiler

The crystal structures of three Schiff bases synthesized from 3-formylaceylacetone and different primary amines were determined and compared with simulated gas phase structures based on DFT calculations.

CCDC references: 2279192; 2279191; 2279190

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Crystal structure of bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-κ²N³,S}nickel(II)

S. S. Khan, M. B. H. Howlader, M. C. Sheikh, R. Miyatake and E. Zangrando

The mononuclear nickel(II) complex is bis-chelated by dithiocarbazato ligands bearing a thienyl ring and an n-octyl alkyl chain.

CCDC reference: 2254902

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Crystal structure of K₆[Zn(CO₃)₄]

F. Eder and M. Weil

The crystal structure of the title compound comprises a tetracarbonatozincate(II) anion, [Zn(CO₃)₄]⁶⁻, with point-group symmetry 2 where the Zn^II atom is surrounded in a distorted tetrahedral manner by four monodentate carbonate groups.

CCDC reference: 2280530

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Crystal structure and luminescence spectrum of a one-dimensional nickel(II) coordination polymer incorporating 1,4-bis[(2-methylimidazol-1-yl)methyl]benzene and adamantane-1,3-dicarboxylate co-ligands

Y. Zhang, H. Qin and B. Wu

The title one-dimensional coordination polymer features alternating 26- and 16-membered rings.

CCDC reference: 2280450

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Crystal structure of poly[(acetonitrile-κN)(μ₃-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-κ⁴N,O:O′:O′′)sodium]

K. Kubono, R. Tanaka, Y. Kashiwagi, K. Tani and K. Yokoi

In the title compound, the Na^I atom has a distorted square-pyramidal coordination environment. The molecular structure exhibits an intramolecular bifurcated O—H⋯[N(tertiary amine), N(pyridyl)] hydrogen bond. In the crystal, the molecules are linked by the bridging Na—O(sulfonato) coordination bonds and the intermolecular C—H⋯O hydrogen bonds, forming a three-dimensional network structure.

CCDC reference: 2279961

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Crystal structures of four organic salts of trihexyphenidyl at 90 K

Vinaya, Y. B. Basavaraju, H. S. Yathirajan and S. Parkin

The low-temperature crystal structures of four organic salts of the anti-spasmodic drug trihexyphenidyl are presented.

CCDC references: 2280174; 2280173; 2280172; 2280171

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Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-one

A. N. Khalilov, V. N. Khrustalev, A. I. Samigullina, M. Akkurt, R. M. Rzayev, A. Bhattarai and İ. G. Mamedov

In the crystal, pairs of molecules are linked by C—H⋯O hydrogen bonds, forming dimers with $[R_{2}^{2}]$ (14) ring motifs. Molecules are connected via C—H⋯π interactions forming a three-dimensional network.

CCDC reference: 2280559

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Crystal-structure determination and Hirshfeld surface analysis of two new thiophene derivatives: (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}benzenesulfonamide and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}-N-(but-2-yn-1-yl)benzenesulfonamide

S. Madhan, M. NizamMohideen, V. Pavunkumar and A. K. MohanaKrishnan

The crystal structures of two benzothiophene derivatives are described and the intermolecular contacts in the crystals analysed using Hirshfeld surface analysis and two-dimensional fingerprint plots.

CCDC references: 2280606; 2280605

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Crystal structure and Hirshfeld surface analysis of 4-cyano-N-[(4-cyanophenyl)sulfonyl]-N-[2-(5-methylfuran-2-yl)phenyl]benzenesulfonamide

G. Z. Mammadova, E. D. Yakovleva, G. M. Burkin, V. N. Khrustalev, M. Akkurt, S. T. Çelikesir and A. Bhattarai

The crystal structure features C—H⋯O and C—H⋯N hydrogen bonds, which link the molecules into layers parallel to the (100) plane. IC—H⋯π interactions and weak van der Waals interactions occur between the layers.

CCDC reference: 2282070

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N-Cyclohexyltryptamine: freebase, bromide and fumarate

M. Naeem, A. N. Le, B. E. Bauer, A. R. Chadeayne, J. A. Golen and D. R. Manke

The crystal structure of the freebase of the monoalkyl tryptamine N-cyclohexyltryptamine is presented, along with those of its bromide and fumarate salts.

CCDC references: 2281772; 2281771; 2281770

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Synthesis, optical properties and crystal structure of (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene

H. Watanabe, T. Sato, M. Sumita, M. Shiroyama, D. Sugawara, T. Tokuyama, Y. Okuda, K. Wakamatsu, H. Akashi and A. Orita

A dehydrobenzannulene, (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene, was stereoselectively synthesized, and its crystal structure and UV-Vis absorption and photoluminescence optical properties were determined.

CCDC reference: 2252157

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Synthesis and crystal structures of (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine

T. Nasr, B. M. Kariuki, M. M. Elansary, R. Elhaggar and W. Zaghary

Two benzylidenehydrazinederivatives have been synthesized and structurally characterized.

CCDC references: 2235324; 2235323

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issue contents

August 2023 issue

research communications

Co-crystallization of N′-benzylidenepyridine-4-carbohydrazide and benzoic acid via autoxidation of benzaldehyde

Synthesis, crystal structure and Hirshfeld surface analysis of naphthalene-2,3-diyl bis(3-benzyloxy)benzoate

Synthesis and crystal structure of a bench-stable pyridinium ketene hemiaminal: 1-(1-ethoxyethenyl)-2-[methyl(phenyl)amino]pyridin-1-ium trifluoromethanesulfonate

(NH₄)₂[UO₂Cl₄]·2H₂O, a new uranyl tetrachloride with ammonium charge-balancing cations

Synthesis and crystal structures of three Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamine

Crystal structure of bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-κ²N³,S}nickel(II)

Crystal structure of K₆[Zn(CO₃)₄]

Crystal structure and luminescence spectrum of a one-dimensional nickel(II) coordination polymer incorporating 1,4-bis[(2-methylimidazol-1-yl)methyl]benzene and adamantane-1,3-dicarboxylate co-ligands

Crystal structure of poly[(acetonitrile-κN)(μ₃-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-κ⁴N,O:O′:O′′)sodium]

Crystal structures of four organic salts of trihexyphenidyl at 90 K

Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-one

Crystal-structure determination and Hirshfeld surface analysis of two new thiophene derivatives: (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}benzenesulfonamide and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}-N-(but-2-yn-1-yl)benzenesulfonamide

Crystal structure and Hirshfeld surface analysis of 4-cyano-N-[(4-cyanophenyl)sulfonyl]-N-[2-(5-methylfuran-2-yl)phenyl]benzenesulfonamide

N-Cyclohexyltryptamine: freebase, bromide and fumarate

Synthesis, optical properties and crystal structure of (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene

Synthesis and crystal structures of (E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine

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