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CRYSTALLOGRAPHIC
COMMUNICATIONS

Volume 79| Part 9

ISSN: 2056-9890

September 2023 issue

Cover illustration: A tennimide macrocycle resides on a twofold axis and adopts an alternate (syn/anti)₂ conformation with no inner cavity (niche), unlike all previously reported (syn)₄ tennimide conformations. A partial occupancy water molecule (with 0.167 site occupancy) at hydrogen-bonding distances to two symmetry-related carbonyl O atoms (as O—H⋯O=C) resides on the twofold axis in a molecular niche between two of the pyridine rings. Macrocycle aggregation occurs as one-dimensional chains along the (010) direction. See Mocilac, Pohl & Gallagher [Acta Cryst. (2023). E78, 837–841].

modern approaches and tools for teaching crystallography

Foreword to the special virtual issue on Modern approaches and tools for teaching crystallography

G. Díaz de Delgado and S. Parkin

A compilation of articles with a strong teaching element published since 2018 is presented alongside an overview of the articles in the special issue on this topic.

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research communications

Diastereotopic groups in two new single-enantiomer structures (R₂)P(O)[NH-(+)CH(C₂H₅)(C₆H₅)] (R = OC₆H₅ and C₆H₅)

F. Eslami, M. Pourayoubi, F. Sabbaghi, E. Skořepová, M. Dušek and S. Baniyaghoob

Two new single-enantiomer phosphorus structures were studied. Their geometries, conformations and NMR features are discussed.

CCDC references: 2283048; 2283049

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Crystal structure and Hirshfeld surface analysis of 7-[(6-hydroxy-5,5,8a-trimethyl-2-methylenedecahydronaphthalen-1-yl)methoxy]-2H-chromen-2-one

E. G. Karimli, V. N. Khrustalev, M. Akkurt, A. N. Khalilov, A. Bhattarai, A. N. Aleskerova and İ. G. Mamedov

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Crystal structure of bis(3,5-dichloro-2-hydroxybenzyl)(2-methoxyethyl)amine

B. M. Wile, C. L. Griffith and A. R. Johnson

The title compound was prepared via a modified Mannich reaction between 2-methoxyethylamine, 2,4-dichlorophenol, and aqueous formaldehyde. The resulting amine bis(phenol) provides an interesting comparison to related species as a result of the electron-withdrawing substituents on the phenol rings, in combination with similar steric parameters.

CCDC reference: 2067395

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Structures of rac-2,4:3,5-dimethylene xylitol derivatives

M. Satlow and P. G. Williard

The crystal structures of three xylitol derivatives prepared directly from commercially available xylitol by treatment with formalin and acid followed by subsequent derivatization of the primary hydroxyl group of the bis-methylene ketal with mesyl chloride, benzyl bromide or phenyl isocyanate are reported.

CCDC references: 2284876; 2284877; 2284878

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A nickel(II) complex with an unsymmetrical tetradentate chelating ligand derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol

F. K. Al-Zeidaneen, C. E. Anson and A. K. Powell

[(2-{[6-(1,3-Benzothiazol-2-yl)pyridin-2-yl]carbonylazanidyl}phenyl)sulfanido]nickel(II) crystallizes in the centrosymmetric monoclinic space group P2₁/n. Both arms of the expected bis-Schiff base ligand based on pyridine-2,6-dicarbaldehyde and 2-aminothiophenol had oxidized; one by cyclization to a benzothiazole, the other by oxidation of its imine linkage to the corresponding amide.

CCDC reference: 2285993

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Synthesis, crystal structure and Hirshfeld surface analysis of 5-[2-(dicyanomethylidene)hydrazin-1-yl]-2,4,6-triiodoisophthalic acid ethanol monosolvate

F. S. Aliyeva, G. Z. Mammadova, M. Akkurt, S. T. Çelikesir and A. Bhattarai

In the crystal, pairs of molecules are linked by O—H⋯O and N—H⋯O hydrogen bonds forming dimers with $[R_{2}^{2}]$ (14) motifs. These dimers are connected by O—H⋯O hydrogen bonds into chains along the a-axis direction, forming $[R_{2}^{2}]$ (16) ring motifs. Further O—H⋯O interactions involving the ethanol solvent molecule connect the chains into a three-dimensional network.

CCDC reference: 2286318

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Crystal structure of a (carboxymethyl)triethylazanium bromide–2-(triethylazaniumyl)acetate (1/1) hydrogen-bonded dimer

F. M. Carlson, R. J. Staples and S. M. Biros

The crystal structure of a hydrogen-bonded dimer of (triethylazaniumyl)acetic acid and (triethylazaniumyl)acetate bromide features a carboxylic acid hydrogen atom that is engaged in an asymmetric hydrogen bond with the carboxylate oxygen. The crystal also features intramolecular C—H hydrogen bonds and a layer of bromide ions that is surrounded by alkyl groups.

CCDC reference: 2286618

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Synthesis, crystal structure and Hirshfeld surface analysis of a copper(II) complex involving 3-methylbenzoate and 2,2′-bipyridine ligands

A. Qadir

A new copper(II) complex with 3-methylbenzoate and 2,2′-bipyridine synthesized displays chains of hydrogen-bonded complex units along the b axis. Hirshfeld surface analysis indicates that H⋯H and H⋯C/C⋯H contacts are the most important interactions.

CCDC reference: 2117143

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Crystal structure and Hirshfeld surface analysis of 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium chloride monohydrate

E. Z. Huseynov, M. Akkurt, I. Brito, A. Bhattarai, F. N. Naghiyev, K. A. Asadov and A. M. Maharramov

In the crystal, the 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium cations are linked by O—H⋯Cl, N—H⋯Cl, N—H⋯O, N—H⋯S and C—H⋯S hydrogen bonds, forming a tri-periodic network.

CCDC reference: 2288159

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Crystal structure and Hirshfeld surface analysis of 3-(bromomethyl)-2-[1,2-dibromo-2-(6-nitrobenzo[d][1,3]dioxol-5-yl)ethyl]-1-(phenylsulfonyl)-1H-indole chloroform 0.585-solvate

N. Achyuta, S. Kanagasabai, P. Vinayagam, A. K. Mohanakrishnan, N. Gautham and K. Gunasekaran

The title indole derivative crystallizes with a partial occupancy [0.585 (4)] CHCl₃ solvent molecule. The dihedral angles between the indole ring system and pendant nitrobenzodioxolane rings system and phenylsulfonyl ring are 4.81 (14) and 72.24 (19)°, respectively. In the crystal, the indole molecules are linked to each other and to the chloroform molecule by weak C—H⋯O, C—H⋯Cl, C—H⋯π, C—Br⋯π and C—Cl⋯π and aromatic π–π stacking interactions.

CCDC reference: 2279852

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Crystal structure of 2-{[5-(methylsulfanyl)-4-phenyl-4H-1,2,4-triazol-3-yl]methyl}benzo[d]thiazole

R. A. Azzam, G. H. Elgemeie, H. A. Elboshi and P. G. Jones

In the crystal structure of the title compound, the triazole ring exhibits interplanar angles of ca 64 and 77° with the phenyl and benzothiazole planes, respectively. The packing involves three borderline C—H⋯N contacts and a pairing of the triazole rings across an inversion centre.

CCDC reference: 2287438

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Crystal structures of the complexes containing macrocyclic cations [M(cyclam)]²⁺ (M = Ni, Zn) and tetraiodidocadmate(2–) anion

I. L. Andriichuk, S. Shova and Y. D. Lampeka

The isostructural compounds I and II are composed of planar macrocyclic cations [M(cyclam)]²⁺ and the tetrahedral anion [CdI₄]²⁻, which plays a purely charge-compensation function in the Ni^II complex I and is axially coordinated via the iodide atom in the Zn^II complex II. In both complexes, as a result of N–H⋯I hydrogen bonding, the alternating cations and anions form chains running along the b-axis direction that are arranged into di-periodic sheets oriented parallel to the (101) and ( $[\overline{1}]$ 01) planes.

CCDC references: 2281090; 2281091

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Crystal structure studies and Hirshfeld surface analysis of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at 90 K

H. G. Anil Kumar, T. M. Mohan Kumar, T. R. Divakara, D. Geetha, H. S. Yathirajan and S. Parkin

The low-temperature (90 K) crystal structure of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate is presented along with a Hirshfeld surface analysis of the organic cation.

CCDC reference: 2289098

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Spectroscopic, crystallographic, and Hirshfeld surface characterization of nine-membered-ring-containing 9-methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and its parent tetrahydrocarbazole

M. J. Flores, B. Mai and J. M. Tanski

9-Methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and 6-methoxy-1,2,3,4-tetrahydrocarbazole represent the structures of a benzoazonine that contains a nine-membered ring and its parent tetrahydrocarbazole. The molecules of the former pack together via strong amide N—H⋯O hydrogen bonding and weak C—H⋯O interactions, whereas the parent tetrahydrocarbazole packs with C/N—H⋯π interactions, as visualized by Hirshfeld surface characterization.

CCDC references: 2289217; 2289218

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The unusual (syn-/anti-)₂ conformation of a dimethoxypyrimidyl-based tennimide

P. Mocilac, F. Pohl and J. F. Gallagher

The tennimide macrocycle (I) resides on a twofold axis and adopts an alternate (syn/anti)₂ conformation with no inner cavity (niche), unlike all previously reported (syn)₄ tennimide conformations. A partial occupancy water molecule (with 0.167 site occupancy) at hydrogen-bonding distances to two symmetry-related carbonyl O atoms (as O—H⋯O=C) resides on the twofold axis in a molecular niche between two of the pyridine rings. Macrocycle aggregation occurs as one-dimensional chains along the (010) direction.

CCDC reference: 2286597

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Synthesis, characterization and crystal structure of methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate

H. V. P. Hollauer, R. C. Vilas Novas, G. P. Guedes, C. D. Buarque and L. B. L. Escobar

A new coumarin derivative, methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate, has been synthesized and characterized.

CCDC reference: 2289922

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Crystal structure and Hirshfeld surface analysis of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one

M. Akkurt, F. N. Naghiyev, V. N. Khrustalev, K. A. Asadov, A. N. Khalilov, A. Bhattarai and İ. G. Mamedov

In the crystal of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one, the molecules are linked into chains by weak C—H⋯O interactions along the b axis. Successive chains form a zigzag structure along the c axis, and these chains are connected to each other by face-to-face π–π stacking interactions along the a axis, forming layers parallel to the (001) plane. The crystal structure maintains its stability via van der Waals interactions between the layers.

CCDC reference: 2290092

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Crystal structure of the nucleoside 2′-deoxyguanosine dimethyl sulfoxide disolvate

B. Spingler

The first high-quality crystal structure of unmodified 2′-deoxyguanosine is reported. The isolated crystals are the dimethyl sulfoxide disolvate.

CCDC reference: 2290127

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Crystal structure and Hirshfeld surface analysis of 8-azaniumylquinolinium tetrachloridozincate(II)

G. A. Umirova, K. K. Turaev, B. K. Alimnazarov, S. A. Kasimov, A. T. Djalilov, B. T. Ibragimov and J. M. Ashurov

The organic–inorganic hybride salt (C₉H₁₀N₂)[ZnCl₄] consists of a planar 8-azaniumylquinolinium dication and a tetrahedral tetrachloridozincate(II) dianion, held together by N—H⋯Cl and C—H⋯Cl hydrogen bonds, and π—π interactions.

CCDC reference: 2290822

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Synthesis, structure and Hirshfeld surface analysis of a coordination compound of cadmium acetate with 2-aminobenzoxazole

S. Razzoqova, A. Ibragimov, B. Torambetov, S. Kadirova, T. Holczbauer, J. Ashurov and B. Ibragimov

The molecular and crystal structures of a cadmium acetate coordination compound with 2-aminobenzoxazole were studied, and the Hirshfeld surfaces and fingerprint plots were generated to investigate various intermolecular interactions.

CCDC reference: 2290113

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issue contents

September 2023 issue

modern approaches and tools for teaching crystallography

Foreword to the special virtual issue on Modern approaches and tools for teaching crystallography

research communications

Diastereotopic groups in two new single-enantiomer structures (R₂)P(O)[NH-(+)CH(C₂H₅)(C₆H₅)] (R = OC₆H₅ and C₆H₅)

Crystal structure and Hirshfeld surface analysis of 7-[(6-hydroxy-5,5,8a-trimethyl-2-methylenedecahydronaphthalen-1-yl)methoxy]-2H-chromen-2-one

Crystal structure of bis(3,5-dichloro-2-hydroxybenzyl)(2-methoxyethyl)amine

Structures of rac-2,4:3,5-dimethylene xylitol derivatives

A nickel(II) complex with an unsymmetrical tetradentate chelating ligand derived from pyridine-2,6-dicarbaldehyde and 2-aminothiophenol

Synthesis, crystal structure and Hirshfeld surface analysis of 5-[2-(dicyanomethylidene)hydrazin-1-yl]-2,4,6-triiodoisophthalic acid ethanol monosolvate

Crystal structure of a (carboxymethyl)triethylazanium bromide–2-(triethylazaniumyl)acetate (1/1) hydrogen-bonded dimer

Synthesis, crystal structure and Hirshfeld surface analysis of a copper(II) complex involving 3-methylbenzoate and 2,2′-bipyridine ligands

Crystal structure and Hirshfeld surface analysis of 2-amino-5-{(1E)-1-[(carbamothioylamino)imino]ethyl}-4-methyl-1,3-thiazol-3-ium chloride monohydrate

Crystal structure and Hirshfeld surface analysis of 3-(bromomethyl)-2-[1,2-dibromo-2-(6-nitrobenzo[d][1,3]dioxol-5-yl)ethyl]-1-(phenylsulfonyl)-1H-indole chloroform 0.585-solvate

Crystal structure of 2-{[5-(methylsulfanyl)-4-phenyl-4H-1,2,4-triazol-3-yl]methyl}benzo[d]thiazole

Crystal structures of the complexes containing macrocyclic cations [M(cyclam)]²⁺ (M = Ni, Zn) and tetraiodidocadmate(2–) anion

Crystal structure studies and Hirshfeld surface analysis of 4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at 90 K

Spectroscopic, crystallographic, and Hirshfeld surface characterization of nine-membered-ring-containing 9-methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and its parent tetrahydrocarbazole

The unusual (syn-/anti-)₂ conformation of a dimethoxypyrimidyl-based tennimide

Synthesis, characterization and crystal structure of methyl 2-(2-oxo-2H-chromen-4-ylamino)benzoate

Crystal structure and Hirshfeld surface analysis of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one

Crystal structure of the nucleoside 2′-deoxyguanosine dimethyl sulfoxide disolvate

Crystal structure and Hirshfeld surface analysis of 8-azaniumylquinolinium tetrachloridozincate(II)

Synthesis, structure and Hirshfeld surface analysis of a coordination compound of cadmium acetate with 2-aminobenzoxazole

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