issue contents

CRYSTALLOGRAPHIC
COMMUNICATIONS

Volume 79| Part 7

ISSN: 2056-9890

July 2023 issue

Cover illustration: In their article, Chiara Massera and John Helliwell take us on a tour of important moments in crystallography through ten seminal papers or `golden oldies' that present different fundamental concepts in our field. They reformulate the title of each paper to emphasize the importance of that concept and how it is perceived and applied today. They also include a short biographical sketch on the authors, which helps us to get a broader perspective of the people behind those papers. We may have our own list of `golden oldies', or we may decide we need more than ten. In any case, Massera and Helliwell's contribution will be a necessary reference to all crystallographers, especially those who follow the history of crystallography and those who put their best effort in teaching the new generations. We would certainly welcome more papers like this. See: Massera & Helliwell [Acta Cryst. (2023). E78, 580–591].

modern approaches and tools for teaching crystallography

Golden oldies: ten crystallography articles that we think must be read

C. Massera and J. R. Helliwell

We have selected a set of ten diverse crystallography articles to illustrate important moments in the development of our field of science. They are a mixture of `science pull and technology push'. Ten is an arbitrary number and our choice is personal, so many others might have been chosen.

Read article

research communications

Structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole, another ostensible by-product in the synthesis of geminal-dimethyl hydrodipyrrins

H. C. Sample, B. Twamley and M. O. Senge

The crystal structure of a by-product in the synthesis of geminal-dimethyl hydrodipyrrins is reported; (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole (1, C₂₆H₂₄N₄O₈S₂Br₂). Generated through a nitronate-mediated dimerization, this compound presents unforeseen enantiomeric resolution, something previously not noted in its singular prior report. This crystal adds to the ever-growing library of by-products arising from these syntheses.

CCDC reference: 2265533

Read article

Crystal structure and Hirshfeld surface analysis of (1H-imidazole-κN³)[N-(2-oxidobenzylidene)tyrosinato-κ³O,N,O′]copper(II)

S. Suzuki, Y. Akiyama, D. Nakane and T. Akitsu

The amino acid Schiff base copper(II) title complex consists of a tridentate ligand synthesized from L-tyrosine and salicylaldehyde. One imidazole molecule is additionally coordinating to the copper(II) ion. The crystal structure features N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds.

CCDC reference: 2266335

Read article

Crystal structure of Ag₃Dy₂(NO₃)₉ and quantitative comparison to isotypic compounds

W. Klein

The crystal structure of the title compound and its particular relation to isotypic compounds is considered.

CCDC reference: 2266445

Read article

Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of the 1,1′-(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)

S. I. Tirkasheva, O. E. Ziyadullaev, A. G. Eshimbetov, B. T. Ibragimov and J. M. Ashurov

The two crystallographically non-equivalent molecules in the title compound have C₂ and C_i symmetries. The crystal structure features strong intermolecular O—H⋯O hydrogen bonds, which form eight-membered rings with $[R_{4}^{4}]$ (8) graph-set motifs, linking the molecules into layers.

CCDC reference: 2189423

Read article

Crystal structure and Hirshfeld-surface analysis of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime at 90 K

D. Geetha, C. N. Kavitha, T. R. Divakara, Y. B. Basavaraju, H. S. Yathirajan and S. Parkin

The synthesis and crystal structure of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime, C₁₃H₁₁ClN₂O, are presented along with a comparison to a previously determined triclinic form.

CCDC reference: 2265648

Read article

Metal halide coordination compounds with quinazolin-4(3H)-one

K. K. Turgunov and U. Englert

The cadmium(II) and mercury (II) coordination compounds with composition [CdBr₂(quinoz)] and [HgCl₂(quinoz)], respectively, where quinoz = quinazolin-4(3H)-one, are chain polymers with bridging halogen atoms. The structure of [CdI₂(quinoz)₂] was re-determined at 100 K, modeling minor disorder.

CCDC references: 2267121; 2267120; 2267119

Read article

Crystal structures of two Sm^III complexes with dipicolinate [DPA]²⁻ ligands: comparison of luminescent properties of products obtained at different pH values

S. S. Mortensen and T. J. Sørensen

Crystallization of the title compounds, synthesized from Sm(CF₃SO₃)₃ and dipicolinic acid solution, was found to change as a function of pH.

CCDC references: 2246127; 2246128

Read article

Cyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(η⁴-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(η⁴-tetraphenylcyclopentadienone)iron acetone hemisolvate

A. Bütikofer and P. Chen

Cyclopentadienone triisocyanide iron complexes were isolated and fully characterized for the first time. Two of the twelve isolated complexes could be crystallographically characterized.

CCDC references: 2248733; 2260413

Read article

Crystal structure of 1-(4-bromophenyl)but-3-yn-1-one

S. K. Siddiqui, C. V. Ramana and R. G. Gonnade

The title compound crystallizes in the monoclinic crystal system in the centrosymmetric space group P2₁/n. The crystal structure features C—H⋯O hydrogen bonding and a short C=O⋯C≡C (acetylene) contacts.

CCDC reference: 2268276

Read article

Crystal structures and Hirshfeld surface analyses of (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-phenyldiazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methylphenyl)diazene, (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(4-methoxyphenyl)diazene and (E)-1-[1-(4-tert-butylphenyl)-2,2-dichloroethenyl]-2-(3-methylphenyl)diazene

A. Maharramov, N. Q. Shikhaliyev, A. Qajar, G. T. Atakishiyeva, A. Niyazova, V. N. Khrustalev, M. Akkurt, S. Ö. Yıldırım and A. Bhattarai

C—H⋯π and C—Cl⋯π interactions are the most important intermolecular interactions in the crystal structures of the title compounds.

CCDC references: 2268431; 2268430; 2268429; 2268428

Read article

Synthesis, crystal structure and Hirshfeld surface analysis of bis(caffeinium) hexachloridoplatinum(IV) in comparison with some related compounds

K. A. Zagidullin, A. P. Novikov, D. A. Zelenina, M. S. Grigoriev and K. E. German

In the crystal, the cations and anions form a layered structure via strong N—H⋯Cl, weak C—H⋯Cl and C—H⋯O hydrogen bonds and π-stacking interactions.

CCDC reference: 2268577

Read article

3,5-Lutidine pentaaqua sulfate complexes of first-row transition metals: [M(3,5-lutidine)(H₂O)₅]SO₄, with M = Mn, Co, Ni, and Zn

J. A. Golen and D. R. Manke

The structures of four metal 3,5-lutidine pentaaqua sulfates (Mn, Co, Ni, Zn) are presented and are shown to be isostructural.

CCDC references: 2269315; 2269314; 2269313; 2269312

Read article

Crystal structure of 5-(β-D-glucopyranosylthio)-N-(4-methylphenyl)-1,3,4-thiadiazol-2-amine

M. A. Abu-Zaied, A. M. S. Hebishy, G. H. Elgemeie, H. T. Salama and P. G. Jones

In the title compound, the angle between the tolyl and thiadiazole rings is 9.2 (1)°. The hydrogen bonding is a combination of a ribbon involving hydrogen bonds of the sugar residues, and a layer based on N—H⋯O and O—H⋯N hydrogen bonds.

CCDC reference: 2269285

Read article

catena-Poly[[bis(diaqualithium)]-μ₄-3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diido]: a new moisture-insensitive alkali-metal energetic salt with a well-defined network structure

K. V. Domasevitch, G. A. Senchyk and H. Krautscheid

In the title salt, the 3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diide dianion [{TNBPz}²⁻] is situated across the twofold axis. The distorted coordination octahedra around Li⁺ involve four short bonds with two pyrazolate N atoms and two aqua ligands and two longer contacts with nitro-O atoms. When combined with μ₄-{TNBPz}²⁻, this generates a mono-periodic polymeric structure incorporating discrete centrosymmeric [(H₂O)₂Li–(dinitropyrazolato)₂–Li(H₂O)₂] units. The three-dimensional stack of mutually orthogonal coordination chains is reminiscent of a Lincoln log pattern.

CCDC reference: 2269963

Read article

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

E. Pehlivanlar, S. Ö. Yıldırım, R. Şimşek, M. Akkurt, R. J. Butcher and A. Bhattarai

In the crystal, molecules are connected via N—H⋯O and C—H⋯O hydrogen bonds and C—H⋯π interactions, forming layers parallel to the (100) plane. van der Waals forces and C—H⋯F interactions connect these layers, consolidating the crystal structure.

CCDC reference: 2271384

Read article

Crystal structure and Hirshfeld surface analysis of bis{(Z)-N′-[(E)-(furan-2-yl)methylidene]carbamohydrazonothioato}nickel(II) methanol disolvate

A. N. Azizova, G. Z. Mammadova, S. T. Çelikesir, M. Akkurt and A. Bhattarai

In the title complex, the Ni^II atom is coordinated by the S and N atoms of two N′-[(Z)-(furan-2-yl)methylidene]carbamohydrazonothioic acid ligands in a distorted square-planar geometry.

CCDC reference: 2269284

Read article

The synthesis, crystal structure and spectroscopic analysis of (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one

Vinaya, A. S. Richard, S. M. Murthy, Y. B. Basavaraju, H. S. Yathirajan and S. Parkin

The synthesis, crystal structure and some spectroscopic details for (E)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-(4-chlorophenyl)prop-2-en-1-one are presented.

CCDC reference: 2272334

Read article

Crystallographic and spectroscopic characterization of two 1-phenyl-1H-imidazoles: 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazole

I. F. McClements, C. R. Wiesler and J. M. Tanski

Two 1-phenyl-1H-imidazoles, 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazole, differ in the substituent para to the imidazole group on the arene ring. Both molecules pack with different motifs via similar weak C—H⋯N/O interactions and differ with respect to the angles between the mean planes of the imidazole and arene rings.

CCDC references: 2267421; 2267419

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

July 2023 issue

modern approaches and tools for teaching crystallography

Golden oldies: ten crystallography articles that we think must be read

research communications

Structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole, another ostensible by-product in the synthesis of geminal-dimethyl hydrodipyrrins

Crystal structure and Hirshfeld surface analysis of (1H-imidazole-κN³)[N-(2-oxidobenzylidene)tyrosinato-κ³O,N,O′]copper(II)

Crystal structure of Ag₃Dy₂(NO₃)₉ and quantitative comparison to isotypic compounds

Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of the 1,1′-(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)

Crystal structure and Hirshfeld-surface analysis of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime at 90 K

Metal halide coordination compounds with quinazolin-4(3H)-one

Crystal structures of two Sm^III complexes with dipicolinate [DPA]²⁻ ligands: comparison of luminescent properties of products obtained at different pH values

Cyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(η⁴-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(η⁴-tetraphenylcyclopentadienone)iron acetone hemisolvate

Crystal structure of 1-(4-bromophenyl)but-3-yn-1-one

Synthesis, crystal structure and Hirshfeld surface analysis of bis(caffeinium) hexachloridoplatinum(IV) in comparison with some related compounds

3,5-Lutidine pentaaqua sulfate complexes of first-row transition metals: [M(3,5-lutidine)(H₂O)₅]SO₄, with M = Mn, Co, Ni, and Zn

Crystal structure of 5-(β-D-glucopyranosylthio)-N-(4-methylphenyl)-1,3,4-thiadiazol-2-amine

catena-Poly[[bis(diaqualithium)]-μ₄-3,3′,5,5′-tetranitro-4,4′-bipyrazole-1,1′-diido]: a new moisture-insensitive alkali-metal energetic salt with a well-defined network structure

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

Crystal structure and Hirshfeld surface analysis of bis{(Z)-N′-[(E)-(furan-2-yl)methylidene]carbamohydrazonothioato}nickel(II) methanol disolvate

The synthesis, crystal structure and spectroscopic analysis of (E)-3-(4-chlorophenyl)-1-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)prop-2-en-1-one

Crystallographic and spectroscopic characterization of two 1-phenyl-1H-imidazoles: 4-(1H-imidazol-1-yl)benzaldehyde and 1-(4-methoxyphenyl)-1H-imidazole

Special issues

Research communications

Explore

Emerging Sources Citation Index

Editorial Advisory Board

News and jobs