issue contents

CRYSTALLOGRAPHIC
COMMUNICATIONS

Volume 79| Part 12

ISSN: 2056-9890

December 2023 issue

Cover illustration: 2-(2-Hydroxyphenyl)benzimidazoles are a class of photoluminescent ligands, the properties of which can be tuned through complexation to different metal centres. The present study discusses the synthesis and structural characterization of two new bi-nuclear complexes of Mn and Co with benzimidazole derivatives, stemming from a longstanding collaboration between the Laboratoire de Chimie de Coordination Organique (LCCO), University of Dakar, Senegal, and the National Crystallography Service (NCS), School of Chemistry, University of Southampton, UK. This collaboration is one of the many successful programmes (such as the IUCr Crystallography in Africa Initiative or the IUCr–UNESCO OpenLab network) to foster and promote crystallography throughout the African continent. The paper is also included in a special collection celebrating the recent founding of the African Crystallographic Association. See Orton, Diouf, Gueye, Gaye, Thiam & Coles [Acta Cryst. (2023). E78, 1109–1114].

research communications

Synthesis and crystal structures of two related Co and Mn complexes: a celebration of collaboration between the universities of Dakar and Southampton

J. B. Orton, N. Diouf, R. S. Gueye, M. Gaye, I. E. Thiam and S. J. Coles

The synthesis and structures are reported of two transition-metal complexes involving 2-(2-hydroxyphenyl)benzimidazole with cobalt and manganese, arising from a UK–Africa collaboration.

CCDC references: 2306731; 2306730

Read article

Crystal structure and Hirshfeld surface analysis of a new mononuclear copper(II) complex: [bis(pyridin-2-yl-κN)amine](formato-κO)(m-hydroxybenzoato-κ²O,O′)copper(II)

W. Chaisuriya, K. Chainok and N. Wannarit

The molecular structure of the ternary mononuclear copper(II) title complex shows a slightly distorted square-pyramidal coordination environment of the Cu^II atom with an [N₂O₃] coordination set.

CCDC reference: 2302393

Read article

Crystal structure of CaSiF₆·2H₂O(mP2) and reevaluation of the Si^IV–F bond-valence parameter R₀

K. Motaln and M. Lozinšek

The crystal structure of a second polymorph of CaSiF₆·2H₂O featuring a layered structure connected by hydrogen bonds is presented.

CCDC reference: 2303630

Read article

Crystal structure and Hirshfeld surface analysis of 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic acid dimethyl sulfoxide-d₆ monosolvate

G. Z. Mammadova, E. D. Yakovleva, P. P. Erokhin, M. S. Grigoriev, Z. Atioğlu, A. N. Azizova, M. Akkurt and A. Bhattarai

In the crystal, molecules are connected by pairs of intermolecular C—H⋯O hydrogen bonds, forming dimers with $[R_{2}^{2}]$ (8) motifs. These dimers form a three-dimensional network through O—H⋯O, O—H⋯S and C—H⋯O hydrogen bonds with each other directly and through solvent molecules.

CCDC reference: 2305649

Read article

Synthesis, characterization, crystal structure and Hirshfeld surface analysis of isobutyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate

S. Ö. Yıldırım, M. Akkurt, G. Çetin, R. Şimşek, R. J. Butcher and A. Bhattarai

In the crystal, the molecules are linked by N—H⋯O and C—H⋯O interactions, forming supramolecular chains parallel to the a axis. These chains pack with C—H⋯π interactions between them, forming layers parallel to the (010) plane.

CCDC reference: 2305562

Read article

Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and of its bis-chelated nickel(II) complex

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

A bis-chelated mononuclear nickel(II) complex with a dithiocarbazate ligand bearing a long saturated alkyl chain exhibits a distorted cis square planar coordination of the metal with two ligands conformationally different from the proligand.

CCDC references: 2254903; 2254853

Read article

Crystal structure and Hirshfeld surface analysis of (2Z)-3-oxo-N-phenyl-2-[(1H-pyrrol-2-yl)methylidene]butanamide monohydrate

A. S. Safarova, A. N. Khalilov, M. Akkurt, I. Brito, A. Bhattarai, F. N. Naghiyev and I. G. Mamedov

In the title compound, the molecules are connected by C—H⋯O hydrogen bonds in layers parallel to the (020) plane. C—H⋯π and π–π interactions further link the molecules into chains extending in the [ $[\overline{1}]$ 01] direction.

CCDC reference: 2306713

Read article

Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-one

S. K. Phillips, S. G. Brancato, S. N. MacMillan, M. J. Snider, A. J. Roering and K. A. Hicks

The synthesis of the title compound as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization are described.

CCDC reference: 2306392

Read article

Crystal structure of polymeric bis(3-amino-1H-pyrazole)cadmium dibromide

I. S. Kuzevanova, O. S. Vynohradov, V. A. Pavlenko, S. O. Malinkin, S. Shova, I. O. Fritsky and M. Seredyuk

The title compound {[CdBr₂(3-apz)₂]}_n consists of a Cd²⁺ cation, bromide anions balancing the charge and bridging 3-aminopyrazole (3-apz) molecules. The Cd²⁺ cations are coordinated by two bromide anions and two 3-apz ligands, generating trans-CdN₄Br₂ octahedra, and are linked into chains by pairs of the bridging ligands. In the crystal, the 3-apz ligands and bromide anions of neighboring chains are linked through interchain hydrogen bonding into a two-dimensional supramolecular network.

CCDC reference: 2306409

Read article

Crystal structure reinvestigation and spectroscopic analysis of tricadmium orthophosphate

F.-Z. Cherif, M. Taibi, A. Boukhari, A. Assani, M. Saadi and L. El Ammari

The transition-metal orthophosphate, β-Cd₃(PO₄)₂, was synthesized by a solid-state reaction and characterized by single-crystal X-ray diffraction and EDS spectroscopy. It crystallizes in the monoclinic system, space group P2₁/n.

CCDC reference: 2306650

Read article

Crystal structures of the isotypic complexes bis(morpholine)gold(I) chloride and bis(morpholine)gold(I) bromide

C. Döring and P. G. Jones

In the title compounds, the gold atoms lie on inversion centres and are linearly coordinated by two morpholine ligands. The halide anions lie on twofold axes. Hydrogen bonds and Au⋯halide contacts lead to a layer structure.

CCDC references: 2113955; 2113954

Read article

Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-κ²N²,S)palladium(II) ethanol monosolvate

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

The synthesis, crystal structure and Hirshfeld analysis of the first complex with the (R,S)-fixolide 4-methylthiosemicarbazonato ligand is reported. A hydrogen-bonded macrocyclic environment type is observed for the Pd^II homoleptic complex. In the crystal, the complexes and the ethanol solvate molecules are linked by H⋯S and H⋯O interactions, forming mono-periodic hydrogen-bonded ribbons along [011].

CCDC reference: 2308228

Read article

Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)

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

In the crystal structure of the title compound, Fe(NCS)(Cl)(3-cyanopyridine)₄ (3-cyanopyridine = pyridine-3-carbonitrile) the Fe^II cations are octahedrally coordinated by one terminal N-bonding thiocyanate anion, one chloride anion and four 3-cyanopyridine coligands that coordinate with the pyridine N atom to the iron centers. Upon heating the 3-cyanopyridine coligands are emitted in two separate steps, leading to the formation of an intermediate compound with the composition Fe(NCS)(Cl)(3-cyanopyridine)₂.

CCDC reference: 2307914

Read article

Synthesis, structure and Hirshfeld surface analysis of 1,3-bis[(1-octyl-1H-1,2,3-triazol-4-yl)methyl]-1H-benzo[d]imidazol-2(3H)-one

M. Zouhair, L. El Ghayati, H. El Monfalouti, H. Abchihi, T. Hökelek, M. Ahmed, J. T. Mague and N. K. Sebbar

The title molecule adopts a conformation resembling a two-bladed fan with the octyl chains in fully extended conformations. In the crystal, the molecules are linked by C—H⋯O and C—H⋯N hydrogen bonds and C—H⋯π interactions.

CCDC reference: 2307930

Read article

Crystal structure, Hirshfeld surface analysis, intermolecular interaction energies, energy frameworks and DFT calculations of 4-amino-1-(prop-2-yn-1-yl)pyrimidin-2(1H)-one

M. Lahyaoui, A. Haoudi, B. E. Kartah, A. Mazzah, T. Hökelek, J. T. Mague, Y. Kandri Rodi and N. K. Sebbar

The molecular structure of the title compound comprises an essentially planar pyrimidine ring from which the propynyl group is rotated by 15.31 (4)°. In the crystal, a tri-periodic network is formed by N—H⋯O, N—H⋯N and C—H⋯O hydrogen-bonding and slipped π–π stacking interactions, leading to narrow channels extending parallel to the c axis.

CCDC reference: 2308262

Read article

Synthesis, crystal structure and Hirshfeld surface analysis of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine

J. Suyunov, B. Torambetov, K. Turaev, S. Kadirova, B. Alimnazarov and J. Ashurov

The molecular and crystal structure of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine was studied and Hirshfeld surfaces and fingerprint plots were generated to investigate the various intermolecular interactions.

CCDC reference: 2257108

Read article

Crystal structure and antimycobacterial evaluation of 2-(cyclohexylmethyl)-7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-one

A. Richter, R. Goddard, P. Imming and R. W. Seidel

The crystal structure of the title compound features centrosymmetric dimers formed through C—H⋯O weak hydrogen bonds between a C—H group of the electron-deficient benzene ring and the benzothiazolinone carbonyl O atom with an $[R_{2}^{2}]$ (10) motif.

CCDC reference: 2309724

Read article

An octanuclear nickel(II) pyrazolate cluster with a cubic Ni₈ core and its methyl- and n-octyl-functionalized derivatives

W. A. Al Isawi, M. Zeller and G. Mezei

The molecular and crystal structure of a discrete [Ni₈(μ₄-OH)₆(μ-4-Rpz)₁₂]²⁻ (R = H; pz = pyrazolato anion) cluster with an unprecedented, perfectly cubic arrangement of its eight Ni centers is reported, along with its lower-symmetry alkyl-functionalized (R = methyl and n-octyl) derivatives.

CCDC references: 2309528; 2309527; 2309526

Read article

Synthesis and redetermination of the crystal structure of NbF₅

M. Möbs and F. Kraus

NbF₅ was synthesized in high purity by direct fluorination. IR and Raman spectroscopy confirms the high purity. The crystal structure was redetermined at 100 K with higher precision.

CCDC references: 2309973; 2289431

Read article

Synthesis, crystal structure and computational analysis of 2,7-bis(4-chlorophenyl)-3,3-dimethyl-1,4-diazepan-5-one

S. Akila, T. Vidhyasagar, J. P. Winfred Jebaraj, A. A. Thiruvalluvar and K. Rajeswari

The seven-membered 1,4-diazepane ring adopts a chair conformation with the 4-chlorophenyl groups in equatorial orientations. The title compound possesses a docking score of −8.9 kcal mol⁻¹ with the human oestrogen receptor 3ERT protein.

CCDC reference: 2166707

Read article

Synthesis, crystal structure and Hirshfeld surface analysis of the tetrakis complex NaNdPyr₄(i-PrOH)₂·i-PrOH with a carbacylamidophosphate of the amide type

N. S. Kariaka, V. V. Dyakonenko, K. O. Znovjyak, S. V. Shishkina and V. M. Amirkhanov

The crystal structure of neodymium tetrakis complex based on bis(N,N-tetramethylene)(trichloroacetyl)phosphoric acid triamide is reported and discussed.

CCDC reference: 2309129

Read article

Dimorphism of [Bi₂O₂(OH)](NO₃) – the ordered Pna2₁ structure at 100 K

M. Weil, O. P. Missen and S. J. Mills

A structural phase transition occurs for [Bi₂O₂(OH)](NO₃) between 173 K (space group Cmc2₁; previous single-crystal X-ray data) and 100 K (space group Pna2₁; current single-crystal X-ray data).

CCDC reference: 2310821

Read article

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text
		Text

issue contents

December 2023 issue

research communications

Synthesis and crystal structures of two related Co and Mn complexes: a celebration of collaboration between the universities of Dakar and Southampton

Crystal structure and Hirshfeld surface analysis of a new mononuclear copper(II) complex: [bis(pyridin-2-yl-κN)amine](formato-κO)(m-hydroxybenzoato-κ²O,O′)copper(II)

Crystal structure of CaSiF₆·2H₂O(mP2) and reevaluation of the Si^IV–F bond-valence parameter R₀

Crystal structure and Hirshfeld surface analysis of 10-hydroxy-2-(4-methoxyphenyl)-3-oxo-2,3,3a,4,10,10a-hexahydro-1H-9-thia-2-azacyclopenta[b]fluorene-4-carboxylic acid dimethyl sulfoxide-d₆ monosolvate

Synthesis, characterization, crystal structure and Hirshfeld surface analysis of isobutyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate

Crystal structure of S-n-octyl 3-(1-phenylethylidene)dithiocarbazate and of its bis-chelated nickel(II) complex

Crystal structure and Hirshfeld surface analysis of (2Z)-3-oxo-N-phenyl-2-[(1H-pyrrol-2-yl)methylidene]butanamide monohydrate

Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-one

Crystal structure of polymeric bis(3-amino-1H-pyrazole)cadmium dibromide

Crystal structure reinvestigation and spectroscopic analysis of tricadmium orthophosphate

Crystal structures of the isotypic complexes bis(morpholine)gold(I) chloride and bis(morpholine)gold(I) bromide

Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-κ²N²,S)palladium(II) ethanol monosolvate

Synthesis, crystal structure and properties of chloridotetrakis(pyridine-3-carbonitrile)thiocyanatoiron(II)

Synthesis, structure and Hirshfeld surface analysis of 1,3-bis[(1-octyl-1H-1,2,3-triazol-4-yl)methyl]-1H-benzo[d]imidazol-2(3H)-one

Crystal structure, Hirshfeld surface analysis, intermolecular interaction energies, energy frameworks and DFT calculations of 4-amino-1-(prop-2-yn-1-yl)pyrimidin-2(1H)-one

Synthesis, crystal structure and Hirshfeld surface analysis of a cadmium complex of naphthalene-1,5-disulfonate and o-phenylenediamine

Crystal structure and antimycobacterial evaluation of 2-(cyclohexylmethyl)-7-nitro-5-(trifluoromethyl)benzo[d]isothiazol-3(2H)-one

An octanuclear nickel(II) pyrazolate cluster with a cubic Ni₈ core and its methyl- and n-octyl-functionalized derivatives

Synthesis and redetermination of the crystal structure of NbF₅

Synthesis, crystal structure and computational analysis of 2,7-bis(4-chlorophenyl)-3,3-dimethyl-1,4-diazepan-5-one

Synthesis, crystal structure and Hirshfeld surface analysis of the tetrakis complex NaNdPyr₄(i-PrOH)₂·i-PrOH with a carbacylamidophosphate of the amide type

Dimorphism of [Bi₂O₂(OH)](NO₃) – the ordered Pna2₁ structure at 100 K

Special issues

Research communications

Explore

Emerging Sources Citation Index

Editorial Advisory Board

News and jobs