Hydrogen-bonding functionalities of selected azole drugs in multicom­ponent crystals with tri­thio­cyanuric acid The supra­molecular architectures of five azole active pharmaceutical ingredients (econazole, luliconazole, isavuconazole, voriconazole and posaconazole) with tri­thio­cyanuric acid have been characterized, with particular emphasis on their hy­dro­gen-bonding functionalities. Four-mol­ecule assemblies formed via N—H⋯N/S hy­dro­gen bonds are analyzed using QTAIM and pairwise inter­action energy calculations to elucidate their stability and energetics.

Ben et al.: Hydrogen-bonding functionalities of selected azole drugs in multicom­ponent crystals with tri­thio­cyanuric acid #CrystalStructure #Imidazole #Triazole ... #IUCr https://journals.iucr.org/paper?S2053229626003219

Nucleophilic substitution of a phthalimidyl group with morpholine in an N1-methyl-1,2,3-triazole: crystallographic evidence for migration of the methyl­ene bridge X-ray crystallography revealed that the reaction of 2-{[4-(4-bromo­phen­yl)-1H-1,2,3-triazol-1-yl]meth­yl}phthalimide with morpholine led to substitution of the phthalimide group, including migration of the substituent from N1 to N2 on the 1,2,3-triazole ring.

Palme et al.: Nucleophilic substitution of a phthalimidyl group with morpholine in an N1-methyl-1,2,3-triazole: crystallographic evidence for migration of the methyl­ene bridge #DipolarCycloaddition #ClickChemistry ... #IUCr https://journals.iucr.org/paper?S2053229626002810

Towards the design of ionic traps incorporating thermo­labile units: structural characterization of copper(II), palladium(II) and rhodium(II) com­plexes with the amino­alcohol ligand 2-(pyridin-2-yl­amino)­ethanol Single-crystal X-ray diffraction studies of Cu, Pd and Rh com­plexes with 2-(pyridin-2-yl­amino)­ethanol (L1) revealed how ligand flexibility governs coordination geometry, supra­molecular organization and crystallization behaviour. These results provide valuable structural insights for the rational design of thermo­labile ionic traps incorporating thermosensitive moieties.

M​ateja-Pluta et al.: Towards the design of ionic traps incorporating thermo­labile units: structural characterization of copper(II), palladium(II) and rhodium(II) com­plexes with t... #IUCr https://journals.iucr.org/paper?S2053229626002676

A new nickel coordination polymer electrode material for hybrid supercapacitors A new nickel coordination polymer electrode material for hybrid supercapacitors, Ni–mba–K(Na) (where H2mba is 2-mercapto­benzoic acid), has been prepared successfully. As a hybrid capacitor electrode material, Ni–mba–K(Na) exhibits the characteristics of battery-type electrode materials but demonstrates a capacitor-level power density and cycling stability. This structure and performance have rarely been investigated.

Wu et al.: A new nickel coordination polymer electrode material for hybrid supercapacitors #CrystalStructure #NickelCoordinationPolymer #ElectrodeMaterial ... #IUCr https://journals.iucr.org/paper?S205322962600207X

Preparation and powder X-ray diffraction study of tecovirimat hydrate solid forms Methods for the reproducible preparation of three hydrated solid forms of the anti­viral com­pound tecovirimat (forms I, III and V) are presented and their phase purity was verified by powder X-ray diffraction using Rietveld refinement. Two previously unknown crystal structures (forms I and V) were determined. A com­parative analysis was made of the hy­dro­gen-bonding motifs and packing architectures.

Ivlev et al.: Preparation and powder X-ray diffraction study of tecovirimat hydrate solid forms #CrystalStructure #CrystalPolymorphism #Tecovirimat ... #IUCr https://journals.iucr.org/paper?S2053229626001154

March issue @actacrystc.iucr.org The cover article reports the effects of protonation in salt forms of a thioamide @UniStrathclyde @StrathScience @UniStrathLibIT #pharmaceutical #salt #protonation #protonated #thioamide #carbocation #crystallography #openaccess journals.iucr.org/c/issues/202...

Room-tem­per­a­ture crystal structures of [CH(NH2)2]3Sb2X9 (X = Br and I) Two new vacancy-ordered formamidinium anti­mony halide triple-per­ov­skites, FA3Sb2X9 {FA = [CH(NH2)2]+; X = Br and I}, measured by single-crystal X-ray diffraction are described.

Bhatt et al.: Room-tem­per­a­ture crystal structures of [CH(NH2)2]3Sb2X9 (X = Br and I) #CrystalStructure #HalidePerovskite #Crystallography ... #IUCr https://journals.iucr.org/paper?S2053229626000811

Salt forms of a thio­amide: protonation of 1-(2,6-di­methyl­phen­yl)thio­urea Treating the thio­amide 1-(2,6-di­methyl­phen­yl)thio­urea (DMPT) with concentrated aqueous strong acids gave three salt forms with protonation at the thio­amide S atom. Protonation causes lengthening of the C&z-dbnd;S bond and shortening of the C—N bonds in effects similar to those seen when amides are pro­ton­ated at the O atom.

D​onnachie et al.: Salt forms of a thio­amide: protonation of 1-(2,6-di­methyl­phen­yl)thio­urea #CrystalStructure #Pharmaceutical #SaltSelection ... #IUCr https://journals.iucr.org/paper?S2053229626001804

Chiral three-dimensional cadmium(II)-based coordination polymer constructed from a lactic acid derivative: synthesis, structure and properties In the presence of pyrazine (pyr), the self-assembly reaction of (R)-5-(1-carb­oxy­eth­oxy)isophthalic acid, (R)-H3cia, with CdII ions constructed a three-dimensional framework [Cd3{(R)-cia}2(pyr)(H2O)4] (HU32-R) with SHG activity.

Yin et al.: Chiral three-dimensional cadmium(II)-based coordination polymer constructed from a lactic acid derivative: synthesis, structure and properties #ChiralCoordinationPolymer #LacticAcidDerivative ... #IUCr https://journals.iucr.org/paper?S2053229626001671

Structural and biological aspects of (tert-but­oxy­carbonyl­amino)­propyl­phospho­nate derivatives Three derivatives of (tert-but­oxy­carbonyl­amino)­propyl­phospho­nate were analyzed in terms of pharmacokinetic, structural and anti­bacterial activity.

Olczak et al.: Structural and biological aspects of (tert-but­oxy­carbonyl­amino)­propyl­phospho­nate derivatives #TertButoxycarbonylaminoPropylphos­pho­nate #AntibacterialActivity #Enantiomer ... #IUCr https://journals.iucr.org/paper?S2053229626001440

Structure and optical properties of a trimetallic cobalt–molybdenum–sodium metal–organic framework The structure of a trimetallic MOF synthesized under solvothermal conditions has been determined using 3D electron diffraction with bulk sample purity assessed by Rietveld analysis of high-resolution powder X-ray diffraction. The 3D connected structure con­tains tetra­hedral MoVI, five-coordinate CoII and six- and seven-coordinate Na, connected by benzene-1,3,5-tri­carboxyl­ate, and shows a UV–Vis spectrum consistent with the trigonal bipyramidal cobalt(II) centre.

M​oore et al.: Structure and optical properties of a trimetallic cobalt–molybdenum–sodium metal–organic framework #CrystalStructure #DED #MetalorganicFramework ... #IUCr https://journals.iucr.org/paper?S205322962600077X

February issue @actacrystc.iucr.org The cover article reports the effect of bromine substitution on the aromatic ring and enone connectivity of a series of ferrocenyl chalcones @UPR_Oficial @NatsciUPR @procoretech #ferrocene #ClaisenSchmidt @IUCr #crystallography journals.iucr.org/c/issues/202...

Cocrystals of cyan­uric acid with di(pyridin-4-yl)sulfane and 1,2-di(pyridin-4-yl)disulfane obtained from 4-mer­cap­to­pyridine under controlled illumination conditions Crystallization of 4-mer­cap­to­pyridine with cyan­uric acid under controlled illumination conditions yields three co­crys­tals and reveals how UV irradiation alters solution speciation and the resulting solid forms.

Książkiewicz et al.: Cocrystals of cyan­uric acid with di(pyridin-4-yl)sulfane and 1,2-di(pyridin-4-yl)disulfane obtained from 4-mer­cap­to­pyridine under controlled illumination conditions... #IUCr https://journals.iucr.org/paper?S2053229626000665

Crystal structures, cytotoxicity studies and inter­actions with DNA of novel in situ-formed com­plexes containing N-scorpionate ligands and nitrate ions Three com­plexes were synthesized in an efficient one-pot synthesis. They show potent anti­proliferative activity combined with their great selectivity towards cancer cells.

Adach et al.: Crystal structures, cytotoxicity studies and inter­actions with DNA of novel in situ-formed com­plexes containing N-scorpionate ligands and nitrate ions #NScorpionateCobaltIIComplexe #OnePotSynthesis ... #IUCr https://journals.iucr.org/paper?S2053229626000525

Comprehensive structural analysis of bromine-substituted ferro­cen­yl chalcones Three novel crystal structures for bromine-substituted ferro­cen­yl chalcones are reported, as well as an in-depth structural study that includes five structures within the series of com­pounds. The effect of bromine substitution on the aromatic ring and enone connectivity of the ferro­cen­yl chalcones was evaluated over crystal structure and supra­molecular features. A Hirshfeld surface analysis is also developed.

Burgos-Suazo et al.: Comprehensive structural analysis of bromine-substituted ferro­cen­yl chalcones #Ferrocene #BromineSubstitutedFerrocenylChalcones #Bromine ... #IUCr https://journals.iucr.org/paper?S2053229625011647

Synthesis, structure and characterization of a new glycolate: sodium glycolate–glycolic acid (1/1) Sodium glycolate–glycolic acid (SGGA), Na(C2H3O3)(C2H4O3), was synthesized to investigate the role of Na+ in the `A′ site of A(C2H3O3)(C2H4O3) glycolates. SGGA crystallizes in the chiral ortho­rhom­bic space group P212121, despite lacking chiral C atoms. The bonding behaviour of glycolic acid and the structural function of Na+ have been clarified, offering insights for the discovery of new minerals.

Hu and Lian: Synthesis, structure and characterization of a new glycolate: sodium glycolate–glycolic acid (1/1) #CrystalStructure #SodiumGlycolateGlycolicAcid #PotassiumGlycolateGlycolicAcid ... #IUCr https://journals.iucr.org/paper?S2053229625011635

Two different products from the reaction between 2-formyl­phenyl­boronic acid and benzhydrazide: benzoyl hydrazone versus dimer After the reaction between 2-formyl­phenyl­boronic acid and benzhydrazide, one of the two products was isolated. The reaction outcome is modulated by solvent choice; performing the reaction in water gives a benzoyl hydrazone and conducting the reaction in ethanol leads to the isolation of a dimer product. These findings are supported using a combination of X-ray crystallography and NMR and high-resolution mass spectrometry (HRMS) data.

Chakiris et al.: Two different products from the reaction between 2-formyl­phenyl­boronic acid and benzhydrazide: benzoyl hydrazone versus dimer #CrystalStructure #Diazaborine #Hydrazone ... #IUCr https://journals.iucr.org/paper?S2053229625011167

A new combination to form a solid solution: a solid solution consisting of a stabilized phenoxyl radical and its meth­oxy analogue The 2,4,6-tris­(4-tert-butyl­phen­yl)phenoxyl radical formed two solid solutions with its meth­oxy analogue. According to single-crystal X-ray analysis, the crystal structure of each solid solution is thought to be dominated by the characters of the main com­ponents.

Xinwen et al.: A new combination to form a solid solution: a solid solution consisting of a stabilized phenoxyl radical and its meth­oxy analogue #CrystalStructure #PolymorphicSolidSolution #DFTCalculations ... #IUCr https://journals.iucr.org/paper?S2053229625011441

Methyl-group effect on the photoluminescence property of a spiro­[fluorene-9,9'-xanthene] derivative: a structural and spectroscopic study The structural and photoluminescent properties of 1′,3′,6′,8′-tetra­methyl­spiro­[fluorene-9,9′-xanthene] were explored, emphasizing the importance of methyl groups in enhancing fluorescence. Single-crystal X-ray diffraction revealed a unique 90° crossover between the fluorene and xanthene segments.

Lu et al.: Methyl-group effect on the photoluminescence property of a spiro­[fluorene-9,9'-xanthene] derivative: a structural and spectroscopic study #CrystalStructure #PpiroFluorene99Xanthene #OrganicMolecule ... #IUCr https://journals.iucr.org/paper?S2053229625011246

Charge-enhanced pyri­dyl tri­fluoro­borate organocatalysts: crystal structures and reactivity An examination of the relationship between the solid-state features of the crystal structures of eleven 3- and 4-pyrdiyl tri­fluoro­borate organocatalysts and their solution-state reactivity is reported.

Lovstedt et al.: Charge-enhanced pyri­dyl tri­fluoro­borate organocatalysts: crystal structures and reactivity #Organocatalysts #CrystalStructure #ChargeEnhancedReactivity ... #IUCr https://journals.iucr.org/paper?S2053229625010629

Two isotypical disodium salts of the anti­hypertensive agent valsartan The crystal structures of two isotypical disodium salts of the antihypertensive agent valsartan were characterized using powder and single-crystal X-ray diffraction.

Buikin et al.: Two isotypical disodium salts of the anti­hypertensive agent valsartan #PowderDiffraction #ActivePharmaceuticalIngredient #API ... #IUCr https://journals.iucr.org/paper?S2053229625010216

December issue @actacrystc.iucr.org The cover article reports the catalytic properties of a lithium complex towards the ring-opening polymerization of e-caprolactone #diimine #azaallyl #lithium #DFT #ROP #polydispersityindex #PDI #IUCr #crystallography journals.iucr.org/c/issues/202...

Crystal structures, thermal properties and inter­molecular inter­actions of new benzamide-based derivatives The supra­molecular assemblies in two benzamide-based derivatives are stabilized by inter­molecular hy­dro­gen bonding between the amide groups. Strong directional connectivity provided by hy­dro­gen bonds joins mol­ecules into one-dimensional chains. Thermal analysis allowed us to propose a mechanism for the transformations of one of the derivatives on heating, including exothermic polymerization, amide-group abstraction and partial benzene abstraction.

Rajakumar et al.: Crystal structures, thermal properties and inter­molecular inter­actions of new benzamide-based derivatives #CrystalStructure #HydrogenBonding #SingleCrystal ... #IUCr https://journals.iucr.org/paper?S2053229625010083

Chloride salts of the antibacterial agent pazufloxacin: (H3O)2(Pzfx)5Cl7·10H2O and (Pzfx)Cl·1.75H2O·0.5C2H5OH By recrystallization of pazufloxacinium mesylate from HCl solutions, two pazufloxacinium chlorides have been obtained and characterized by means of X-ray diffraction.

Tselukovskaya et al.: Chloride salts of the antibacterial agent pazufloxacin: (H3O)2(Pzfx)5Cl7·10H2O and (Pzfx)Cl·1.75H2O·0.5C2H5OH #Pazufloxacine #ActivePharmaceuticalIngredient #API ... #IUCr https://journals.iucr.org/paper?S2053229625010423

Structures and electronic properties of cobalt(II) selone coordination com­plexes The structures of a cyclic seleno­urea ligand and two distorted tetra­hedral cobalt(II) chloride com­plexes are disclosed, along with their com­puted electronic properties and thermochemistry.

Purcell et al.: Structures and electronic properties of cobalt(II) selone coordination com­plexes #SelenoureaLigand #CobaltIIComplex #CoordinationChemistry ... #IUCr https://journals.iucr.org/paper?S2053229625010101

Single-crystal X-ray diffraction analysis and mechanistic implications of (2R*,3R*)-2-(2-phen­oxy­eth­yl)tetra­hydro­furan-3-yl acetate To unambiguously determine the stereochemical outcome of a highly stereospecific rearrangement of epoxides into tetra­hydro­furans, single crystals of one of the products, (2R*,3R*)-2-(2-phen­oxy­eth­yl)tetra­hydro­furan-3-yl acetate, were grown and analyzed. Based on the crystal structure data, we were able to show that the contiguous stereocenters of this mol­ecule are in a syn configuration, and we now suggest with confidence a plausible mechanism for the rearrangement reaction.

Kelley et al.: Single-crystal X-ray diffraction analysis and mechanistic implications of (2R*,3R*)-2-(2-phen­oxy­eth­yl)tetra­hydro­furan-3-yl acetate #Epoxide #Rearrangement #Tetrahydrofuran ... #IUCr https://journals.iucr.org/paper?S2053229625010150

A binuclear lithium com­plex based on an ansa-bis­(1-aza­all­yl) ligand: synthesis, structure and catalysis for ring-opening polymerization of ɛ-cap­ro­lac­tone A binuclear ansa-bis­(1-aza­all­yl) lithium com­plex was prepared by treating the di­imine [(2,6-Me2C6H3)N&z-dbnd;C(Ph)CH2]2SiPh2 with lithium diiso­propyl­amide and was characterized by X-ray diffraction techniques. Density functional theory calculations were used to investigate the catalytic properties of the binuclear com­plex towards the ring-opening polymerization of ɛ-cap­ro­lac­tone and the com­plex showed good catalytic activity.

Xue et al.: A binuclear lithium com­plex based on an ansa-bis­(1-aza­all­yl) ligand: synthesis, structure and catalysis for ring-opening polymerization of ɛ-cap­ro­lac­tone #Diimine #AnsaBis1Azaallyl #Lithium ... #IUCr https://journals.iucr.org/paper?S2053229625009933

Crystal structure, supra­molecular architecture and spectroscopic characterization of the Knoevenagel-type indole derivative (2E)-2-(1H-indol-3-yl­methyl­idene)-4,4-dimethyl-3-oxo­penta­nenitrile The crystal structure of a Knoevenagel-type indole derivative reveals a supra­molecular framework stabilized by N—H⋯O hy­dro­gen bonds, π–π stacking and C&z-tbnd;N⋯H inter­actions. Complementary Hirshfeld surface analysis, inter­action energy calculations and spectroscopic studies provide a com­prehensive description of its structural and electronic features.

D​íaz et al.: Crystal structure, supra­molecular architecture and spectroscopic characterization of the Knoevenagel-type indole derivative (2E)-2-(1H-indol-3-yl­methyl­idene)-4,4-dimethyl-3-oxo­penta­nenitrile ... #IUCr https://journals.iucr.org/paper?S2053229625009945

Weak hy­dro­gen bonding in the structures of three double-acyl­ated amino­anti­pyrines The structures of three doubly-acyl­ated 4-amino­anti­pyrine com­pounds where the aryl substituent is varied are reported and analysed in terms of their relative conformation, inter­molecular inter­actions and overall packing. The com­pounds were crystallized using the encapsulated nanodroplet crystallization (ENaCt) protocol.

M​ardiana et al.: Weak hy­dro­gen bonding in the structures of three double-acyl­ated amino­anti­pyrines #CrystalStructure #Arylation #CrystalPacking ... #IUCr https://journals.iucr.org/paper?S2053229625009581

Effect of the size of halide ligands on the crystal structures of halide-bibridged polymers of HgX2 with 4-ethyl­pyridine Three pyridine-based halide-bibridged polymers have been synthesized and their structures determined. The effect of the size of the halides on the crystal structures has been investigated.

B. M. Parveen Beebeejaun-Boodoo: Effect of the size of halide ligands on the crystal structures of halide-bibridged polymers of HgX2 with 4-ethyl­pyridine #HalideBibridgedPolymers #CrystalStructure ... #IUCr https://journals.iucr.org/paper?S2053229625009702