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CRYSTALLOGRAPHIC
COMMUNICATIONS

Volume 79| Part 11

ISSN: 2056-9890

November 2023 issue

Cover illustration: High levels of greenhouse gas emissions, in particular carbon dioxide, are considered the primary source of the global warming that our planet is experiencing. Among several strategies being explored for the mitigation and control of these emissions are processes that separate, capture and store CO₂ through the so-called carbon capture and sequestration materials (CCS). The stored gases can then be used in reactions leading to materials useful in other different processes such as the synthesis of catalysts or pharmaceutical compounds. This article presents the structure of a novel Cu-carbamato complex, bis[N-(5-methyl-1H-pyrazol-3-yl-κN²)carbamato-κO]copper(II) tetrahydrate, obtained in a reaction driven by absorption of CO₂ present in the environment. See Sirenko, Kuzevanova, Vynohradov, Naumova & Shova [Acta Cryst. (2023). E78, 988–992].

research communications

Synthesis, crystal structure and reactivity of bis(μ-2-methylpyridine N-oxide-κ²O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvate

C. Näther and I. Jess

The crystal structure of the title compound consists of dinuclear complexes, in which the Co^II cations are fivefold coordinated and linked by centrosymmetric pairs of μ-1,1(O,O)-bridging 2-methylpyridine N-oxide coligands.

CCDC reference: 2295983

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Crystal structure of bis(3-carboxy-1-methylpyridinium) octabromide

V. Y. Sirenko, D. D. Naumova, I. A. Golenya, S. Shova and I. A. Gural'skiy

The structure of the title compound is composed of rare Z-shaped octabromide anions embedded within N-methylnicotinic acid cations.

CCDC reference: 2297637

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Unusual reaction of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol with triphenylborane: crystal structures and optical properties

H. Le Thi Hong, T. Le Phuong, T. Van Pham, H. Minh Thi Nguyen and L. Van Meervelt

The molecular and crystal structure of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol and its reaction product with triphenylborane are described. In compound Et₂N-Bz, one of the ethyl groups and the benzothiazole ring are disordered over two sets of atomic sites with major occupancy components of 0.822 (5) and 0.843 (2), respectively.

CCDC references: 2297768; 2297767

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Carbon dioxide capture from air leading to bis[N-(5-methyl-1H-pyrazol-3-yl-κN²)carbamato-κO]copper(II) tetrahydrate

V. Y. Sirenko, I. S. Kuzevanova, O. S. Vynohradov, D. D. Naumova and S. Shova

A mononuclear square-planar Cu^II complex was synthesized by reacting 5-methyl-3-pyrazolamine and copper(II) acetate in water under ambient conditions. Diethanolamine was added to facilitate carbon dioxide adsorption, creating an alkaline environment. Structural analysis revealed that the complex crystallizes in the P2₁/c space group of the monoclinic crystal system, with the central copper(II) atom in a square-planar coordination environment N₂O₂. Co-crystallized water molecules are present, forming O—H⋯O hydrogen bonds with the Cu^II mononuclear complex. Hirshfeld surface analysis highlighted the importance of various interactions, including H⋯O/O⋯H, H⋯C/C⋯H, and H⋯N/N⋯H, in providing crystal structure packing.

CCDC reference: 2298123

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Synthesis, crystal structure and Hirshfeld analysis of trans-bis{(2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamidato-κ²N¹,S}palladium(II)

A. P. L. de Melo, B. B. Martins, L. Bresolin, B. Tirloni and A. B. de Oliveira

The synthesis, crystal structure and Hirshfeld surface analysis of a new Pd^II cinnamaldehyde 4-thiosemicarbazone homoleptic complex is reported. As a result of H⋯S intramolecular interactions, graph-set motif S(5), the coordination sphere resembles a hydrogen-bonded macrocyclic environment-type. In the crystal, the molecules are linked by H⋯S interactions, with graph-set motifs $[R_{2}^{2}]$ (8), forming a mono-periodic hydrogen-bonded polymer along [001].

CCDC reference: 2163054

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Synthesis, crystal structure and in vitro anti-proliferative activity of 2-[(4-acetylphenyl)carbamoyl]phenyl acetate

R. A. Mohamed-Ezzat, B. M. Kariuki and A. M. Srour

2-[(4-Acetylphenyl)carbamoyl]phenyl acetate, a derivative of aspirin, has been structurally characterized revealing a structure based on intermolecular N—H⋯O hydrogen bonds and π–π interactions.

CCDC reference: 2087303

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Crystal structure of dibenzylammonium hydrogen (4-aminophenyl)arsonate monohydrate

B. Traoré, W. Diallo, M. Sidibé, L. Diop, L. Plasseraud and H. Cattey

The title salt consists of three components, comprising one dibenzylammonium cation, [(C₆H₅CH₂)₂NH₂]⁺, one hydrogen (4-aminophenyl)arsonate anion, [H₂NC₆H₄As(OH)O₂]⁻, and one molecule of water. In the crystal, these components are organized in infinite zigzag chains via intermolecular hydrogen bonds. Weak interactions between the chains lead to a three-dimensional network.

CCDC reference: 2297206

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Crystal structure of Cs₂GdNb₆Cl₁₅O₃ in the structural evolution of niobium oxychlorides with octahedral Nb₆-cluster units

S. Silaban, M. E. Haryani, F. Gulo and C. Perrin

Cs₂GdNb₆Cl₁₅O₃ is an octahedral Nb-cluster compound containing three inner ligands of oxygen atoms. Individual Nb₆ clusters are linked to each other via Gd^III and Cs^I atoms, which exhibit a coordination number of 9 (three O and six Cl ligands) and 12 (twelve Cl ligands).

CCDC reference: 2299097

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Synthesis and crystal structure of 2-(anthracen-9-yl)-1-(tert-butyldimethylsilyl)-3,6-dihydro-1λ⁴,2λ⁴-azaborinine

P. J. Gliese, Y. Appiarius, T. Scheele, E. Lork, T. Neudecker and A. Staubitz

A modification of a B—Cl 1,2–azaborinine precursor with anthracenyl lithium generates an air-stable analog of cyclohexadiene. In the crystal packing, van der Waals interactions are dominant.

CCDC reference: 2297014

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Crystal structures of five halido gold complexes involving piperidine or pyrrolidine as ligands or (protonated) as cations

C. Döring and P. G. Jones

The structures of five gold complexes involving piperidine or pyrrolidine, either as neutral ligands or protonated counter-cations, are presented.

CCDC references: 2113940; 2113939; 2113938; 2113937; 2297985

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Synthesis, crystal structure and thermal properties of poly[[μ-1,2-bis(pyridin-4-yl)ethene-κ²N:N′-μ-bromido-copper(I)] 1,2-bis(pyridin-4-yl)ethene 0.25-solvate]

C. Näther, A. Müller-Meinhard and I. Jess

In the crystal structure of the title compound, the copper(I) cations are tetrahededrally coordinated and linked by pairs of bromide anions into dinuclear units that are further connected into layers by the 1,2-bis(pyridin-4-yl)ethene (4-bpe) coligands. The layers are stacked so that cavities are formed in which disordered 4-bpe molecules are embedded.

CCDC reference: 2300129

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Synthesis, crystal structure and Hirshfeld surface analysis of 1-(12-bromododecyl)indoline-2,3-dione

N. Rharmili, O. Abdellaoui, A. Haoudi, J. T. Mague, T. Hökelek, F. Ouazzani Chahdi, Y. Kandri Rodi, A. Mazzah and N. K. Sebbar

The pendant dodecyl chain in the title compound adopts an all-trans conformation apart from the gauche terminal C—C—C—Br moiety.

CCDC reference: 2301451

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Crystal structure, Hirshfeld surface and crystal void analysis, intermolecular interaction energies, DFT calculations and energy frameworks of 2H-benzo[b][1,4]thiazin-3(4H)-one 1,1-dioxide

E. Irrou, Y. Ait Elmachkouri, A. Mazzah, T. Hökelek, A. Haoudi, J. T. Mague, M. L. Taha and N. K. Sebbar

In the title compound, the thiazine ring exhibits a screw-boat conformation. In the crystal, corrugated layers of molecules parallel to the ab plane are formed by N—H⋯O and C—H⋯O hydrogen bonds together with C—H⋯π(ring) and S=O⋯π(ring) interactions. The layers are connected by additional C—H⋯O hydrogen bonds and π-stacking interactions.

CCDC reference: 2298958

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Crystal structure and supramolecular features of a bis-urea-functionalized pillar[5]arene

M. Vinodh, F. H. Alipour and T. F. Al-Azemi

The crystal structure and supramolecular features are reported of a dimeric bis-urea-functionalized pillar[5]arene macrocycle, which functions as a receptor system to the DMF guest molecule.

CCDC reference: 2285344

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Synthesis, crystal structure and Hirshfeld surface analysis of diacetatobis[4-(2-aminoethyl)morpholine]cadmium tetrahydrate

B. Chidambaranathan, S. Sivaraj, P. Vijayamathubalan and S. Selvakumar

In the title coordination compound, the Cd atom is octahedrally coordinated by two N,N′-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a centre of inversion, whereas the morpholine and four water molecules are adjacent to the acetate moieties. In the crystal, neighboring metal complexes and uncoordinated water molecules are linked via N—H⋯O and O—H⋯O hydrogen-bonding interactions.

CCDC reference: 2299387

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Crystal structure of (μ-hydrogen disulfato)-μ-oxido-bis[(4,4′-di-tert-butyl-2,2′-bipyridine)oxidovanadium(IV/V)] acetonitrile monosolvate

S. Kodama, T. Hashiguchi and A. Nomoto

The crystal structure of a dinuclear oxidovanadium(IV/V) complex [V₂O₂(μ-O)(μ-H(SO₄)₂)(4,4′-^tBubpy)₂] acetonitrile monosolvate has been determined.

CCDC reference: 2301351

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Crystal structure and Hirshfeld surface analysis of poly[[tetraaqua(μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.1^3,17.1^8,12]tetracosane-5,6,14,15,20,21-hexaonato)iron(IV)dilithium] tetrahydrate]

M. O. Plutenko, S. Shova, V. A. Pavlenko, I. A. Golenya and I. O. Fritsky

The title compound was obtained as a result of a template reaction between oxalohydrazide, formaldehyde and iron(III) chloride in the presence of atmospheric O₂. The complex anion of the title compound reveals clathrochelate topology and includes an Fe^IV metal centre. In the crystal, the complex anions are connected through two Li cations into dimers, which are connected by Li—O bonds, forming infinite chains along the b-axis direction.

CCDC reference: 2298136

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Synthesis and crystal structure of bis(9-mesityl-9,10-dihydro-10-aza-9-borabenzo[h]quinolinato-κ²N¹,N¹⁰)zinc(II)

Y. Appiarius, P. Puylaert and A. Staubitz

The NH-deprotonation of a 10-aza-9-borabenzo[h]quinoline yields a bidentate ligand that was used for the synthesis of a 2:1 coordination complex with zinc. Its crystal packing is dominated by intense intra- and intermolecular π–π stacking interactions.

CCDC reference: 2302109

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Synthesis and crystal structures of two solvates of 1-{[2,6-bis(hydroxymethyl)-4-methylphenoxy]methyl}-3,5-bis{[(4,6-dimethylpyridin-2-yl)amino]methyl}-2,4,6-triethylbenzene

M. Stapf, U. Schmidt, W. Seichter and M. Mazik

In the crystal structures of the formamide monosolvate (1a) and the n-propanol/water solvate/hydrate (1b), the host molecules adopt similar geometries with an alternating arrangement of the substituents above and below the plane of the central arene ring.

CCDC references: 2301884; 2301883

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Redetermination of the crystal structure of yttrium chromium tetraboride, YCrB₄, from single-crystal X-ray diffraction data

M. Tokuda, K. Yubuta, T. Shishido and K. Sugiyama

The structural parameters of yttrium chromium tetraboride YCrB₄ were refined based on single-crystal X-ray diffraction data. The present study successfully refined all the positional and atomic displacement parameters of the Y, Cr, and B atoms.

CCDC reference: 2300781

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Crystal structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrile

T. T. T. Bui, D. H. Mac, P. Quang Trung and C. T. Pham

The structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrile, prepared by a three-component one-pot reaction, is based on dimers connected by N—H⋯O hydrogen bonds, which also interact through π–π contacts.

CCDC reference: 2302104

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Crystal structure of 1-(2,6-diisopropylphenyl)-1H-imidazole

N. Dudeja, B. C. Arreaga, J. P. Brannon and S. C. E. Stieber

At 106 (2) K, the title molecule has monoclinic P2₁/c symmetry with four molecules in the unit cell. The imidazole ring is rotated 80.7 (1)° relative to the phenyl ring. Intermolecular stabilization primarily results from close contacts between the N-atom at the 3-position on the imidazole ring and the C—H bond at the 4-position on the neighboring ^DippIm.

CCDC reference: 2302037

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Synthesis, crystal structure and Hirshfeld surface analysis of diaquabis(o-phenylenediamine-κ²N,N′)nickel(II) naphthalene-1,5-disulfonate

J. R. Suyunov, K. K. Turaev, B. K. Alimnazarov, Y. E. Nazarov, I. J. Mengnorov, B. T. Ibragimov and J. M. Ashurov

In the title salt, [Ni(C₆H₈N₂)₂(H₂O)₂]·(C₁₀H₆O₆S₂), the Ni^II atom exhibits a slightly tetragonally distorted {O₂N₄} octahedral coordination environment, with two pairs of equatorial Ni—N bonds and a pair of longer axial Ni—O bonds.

CCDC reference: 2303464

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Crystal structure of 2-methyl-1H-imidazol-3-ium 3,5-dicarboxybenzoate

S. Baletska, S. Techert and J. de J. Velazquez-Garcia

The structure of a 2-methyl-1H-imidazol-3-ium trimesate compound was determined by single-crystal X-ray diffraction. The compound is composed of protonated 2-methylimidazole and singly deprotonated trimesic acid molecules.

CCDC reference: 2302266

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Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate

C. Näther, A. Müller-Meinhard and I. Jess

Two complexes, 1 and 2, based on Fe(NCS)₂ and 3-cyanopyridine as coligand were synthesized, structurally characterized and investigated for their thermal behavior. In both compounds the Fe^II cations are octahedrally coordinated by two N-bonded thiocyanate anions in trans-position as well as four 3-cyanopyridine coligands for compound 1 and two 3-cyanopyridine ligands and two water molecules for compound 2. Upon heating, both complexes transform into an intermediate with bridging anionic ligands that is isotypic to its Cd(NCS)₂ and Mn(NCS)₂ analogs.

CCDC references: 2301450; 2301449

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Crystal structure and Hirshfeld surface analysis of bis(3-aminopyrazole-κN¹)bis(3-aminopyrazole-κN²)bis(nitrato-κO)copper(II)

O. I. Kucheriv, I. A. Golenya, O. Prysiazhna, S. V. Partsevska and I. A. Gural'skiy

The title molecular coordination compound exhibits a central Cu^II atom with a distorted octahedral [N₄O₂] coordination environment. The axial positions are occupied by two O atoms from nitrate anions and equatorial positions occupied by pyridine-like N atoms from four 3-aminopyrazole ligands.

CCDC reference: 2302897

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Crystal structure and Hirshfeld surface analysis of triazatriborinotris[1,3,2]benzodiazaborole acetone disolvate

C. Streeter, K. A. Wheeler and A. N. Lamm

The title compound, alternatively known as benzodiazaborole trimer, C₁₈H₁₅B₃N₆·2C₃H₆O, at 100 K crystallizes in the triclinic system, space group P $[\overline{1}]$ . The structure displays N—H⋯O hydrogen bonding connecting the main molecule with the crystallization solvent.

CCDC reference: 2303332

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issue contents

November 2023 issue

research communications

Synthesis, crystal structure and reactivity of bis(μ-2-methylpyridine N-oxide-κ²O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvate

Crystal structure of bis(3-carboxy-1-methylpyridinium) octabromide

Unusual reaction of (E)-2-[(benzo[d]thiazol-2-ylimino)methyl]-5-(diethylamino)phenol with triphenylborane: crystal structures and optical properties

Carbon dioxide capture from air leading to bis[N-(5-methyl-1H-pyrazol-3-yl-κN²)carbamato-κO]copper(II) tetrahydrate

Synthesis, crystal structure and Hirshfeld analysis of trans-bis{(2E)-N-phenyl-2-[(2E)-3-phenyl-2-propen-1-ylidene]hydrazinecarbothioamidato-κ²N¹,S}palladium(II)

Synthesis, crystal structure and in vitro anti-proliferative activity of 2-[(4-acetylphenyl)carbamoyl]phenyl acetate

Crystal structure of dibenzylammonium hydrogen (4-aminophenyl)arsonate monohydrate

Crystal structure of Cs₂GdNb₆Cl₁₅O₃ in the structural evolution of niobium oxychlorides with octahedral Nb₆-cluster units

Synthesis and crystal structure of 2-(anthracen-9-yl)-1-(tert-butyldimethylsilyl)-3,6-dihydro-1λ⁴,2λ⁴-azaborinine

Crystal structures of five halido gold complexes involving piperidine or pyrrolidine as ligands or (protonated) as cations

Synthesis, crystal structure and thermal properties of poly[[μ-1,2-bis(pyridin-4-yl)ethene-κ²N:N′-μ-bromido-copper(I)] 1,2-bis(pyridin-4-yl)ethene 0.25-solvate]

Synthesis, crystal structure and Hirshfeld surface analysis of 1-(12-bromododecyl)indoline-2,3-dione

Crystal structure, Hirshfeld surface and crystal void analysis, intermolecular interaction energies, DFT calculations and energy frameworks of 2H-benzo[b][1,4]thiazin-3(4H)-one 1,1-dioxide

Crystal structure and supramolecular features of a bis-urea-functionalized pillar[5]arene

Synthesis, crystal structure and Hirshfeld surface analysis of diacetatobis[4-(2-aminoethyl)morpholine]cadmium tetrahydrate

Crystal structure of (μ-hydrogen disulfato)-μ-oxido-bis[(4,4′-di-tert-butyl-2,2′-bipyridine)oxidovanadium(IV/V)] acetonitrile monosolvate

Crystal structure and Hirshfeld surface analysis of poly[[tetraaqua(μ-1,3,4,7,8,10,12,13,16,17,19,22-dodecaazatetracyclo[8.8.4.1^3,17.1^8,12]tetracosane-5,6,14,15,20,21-hexaonato)iron(IV)dilithium] tetrahydrate]

Synthesis and crystal structure of bis(9-mesityl-9,10-dihydro-10-aza-9-borabenzo[h]quinolinato-κ²N¹,N¹⁰)zinc(II)

Synthesis and crystal structures of two solvates of 1-{[2,6-bis(hydroxymethyl)-4-methylphenoxy]methyl}-3,5-bis{[(4,6-dimethylpyridin-2-yl)amino]methyl}-2,4,6-triethylbenzene

Redetermination of the crystal structure of yttrium chromium tetraboride, YCrB₄, from single-crystal X-ray diffraction data

Crystal structure of 4-(naphthalen-2-yl)-2-oxo-6-phenyl-1,2-dihydropyridine-3-carbonitrile

Crystal structure of 1-(2,6-diisopropylphenyl)-1H-imidazole

Synthesis, crystal structure and Hirshfeld surface analysis of diaquabis(o-phenylenediamine-κ²N,N′)nickel(II) naphthalene-1,5-disulfonate

Crystal structure of 2-methyl-1H-imidazol-3-ium 3,5-dicarboxybenzoate

Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate

Crystal structure and Hirshfeld surface analysis of bis(3-aminopyrazole-κN¹)bis(3-aminopyrazole-κN²)bis(nitrato-κO)copper(II)

Crystal structure and Hirshfeld surface analysis of triazatriborinotris[1,3,2]benzodiazaborole acetone disolvate

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