The crystal structures, Hirshfeld surface analyses and energy frameworks of two hexa­thia­pyrazino­phane regioisomers; 2,5,8,11,14,17-hexa­thia-[9.9](2,6,3,5)-pyrazino­phane and 2,5,8,11,14,17-hexa­thia-[9.9](2,5,3,6)-pyrazino­phane

The title hexa­thia­pyrazino­phanes are regioisomers, having a central tetra-2,3,5,6-methyl­ene­pyrazine unit with two –S—CH₂—CH₂—S—CH₂—CH₂—S– chains linking the methyl­ene C atoms at positions 2 and 6 and 3 and 5 in the m-bis regioisomer, but linking the methyl­ene C atoms at positions 2 and 5 and 3 and 6 in the p-bis regioisomer.

Crystal structures of [(μ₂-L1)di­bromidodicopper(II)] dibromide and poly[[(μ₂-L1)di­iodido­dicopper(I)]-di-μ-iodido-dicopper(I)], where L1 is 2,5,8,11,14,17-hexa­thia-[9.9](2,6,3,5)-pyrazino­phane

The reaction of the hexa­thia­pyrazino­phane ligand, 2,5,8,11,14,17-hexa­thia-[9.9](2,6,3,5)-pyrazino­phane, with copper(II) dibromide lead to the formation of a binuclear complex. Reaction with copper(I) iodide also gave a binuclear complex, which is bridged by a Cu₂I₂ unit to form a two-dimensional coordination polymer.

4-[(1E)-({[(Benzyl­sulfan­yl)methane­thio­yl]amino}­imino)­meth­yl]benzene-1,3-diol chloro­form hemisolvate: crystal structure, Hirshfeld surface analysis and computational study

The title hydrazine carbodi­thio­ate chloro­form hemi-solvate features approximately planar mol­ecules with splayed phenyl groups. Supra­molecular tapes are formed in the crystal through a combination of N—H⋯S, hydroxyl-O—H⋯O(hydrox­yl) and hydroxyl-O—H⋯π(phen­yl) inter­actions.

Synthesis and crystal structure of [Zn₆Br₄(C₉H₁₈NO)₄(OH)₄]·2C₃H₆O₂

The complete mol­ecule of the hexa­metallic title complex, namely, tetra­bromido­tetra-μ-hydroxido-hexa­kis­[μ-2-methyl-3-(pyrrolidin-1-yl)propan-2-olato]hexa­zinc(II) acetone disolvate, is generated by a crystallographic centre of symmetry. Two of the unique zinc atoms adopt distorted ZnO₂NBr tetra­hedral coordination geometries and the other adopts a ZnO₃N tetra­hedral arrangement. Both unique alkoxide ligands are N,O-chelating and both hydroxide ions are μ² bridging.

Crystal structure of (1,4-di­phenyl-4H-1,2,4-triazol-3-yl)phenyl­amine di­fluoro­phosphate, and a survey of the di­fluoro­phosphate anion (PO₂F₂⁻)

The title compound represents the di­fluoro­phosphate salt of Nitron, an analytical reagent used for gravimetrical analysis of nitrate ions. An analysis of the bond–length distribution and average bond lengths in PO₂F₂ tetra­hedra is given.

Crystal structure and Hirshfeld surface analysis of 1-(2-fluoro­phen­yl)-1H-tetra­zole-5(4H)-thione

In the crystal, mol­ecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an (8) ring motif. The dimers are linked by the offset face-to-face π–π stacking inter­actions.

Crystal structures of three platinacyclic complexes bearing iso­propyl eugenoxyacetate and pyridine derivatives

Three new platinum(II) complexes bearing an isopropyl eugenoxyacetate and pyridine derivatives have been synthesized and further characterized by single-crystal X-ray diffraction.

Crystal structure of N,N-diiso­propyl-4-methyl­benzene­sulfonamide

The synthesis and crystal structure of a diisopropyl-substituted p-tolunesulfonamide is discussed. This structure features C—H⋯O hydrogen bonds (both intra- and inter­molecular) and inter­molecular C—H⋯π inter­actions.

Crystal structure of SrCo₄(OH)(PO₄)₃, a new hy­droxy­phosphate

Three [CoO₆] octa­hedra, one [CoO₄] tetra­hedron and three PO₄ tetra­hedra are linked into a three-dimensional framework structure exhibiting channels parallel to [100] in which the eleven-coordinate strontium cations are located.

Crystal structure, Hirshfeld surface analysis and computational study of a rhodamine B–salicyl­aldehyde Schiff base derivative

The mol­ecular structure of the title compound comprises two parts, xanthene and iso­indole, sharing a central quaternary carbon atom. Both the xanthene and iso­indole moieties are nearly planar and are almost perpendicular.

Crystal structure and Hirshfeld surface analysis of 4-{2,2-di­chloro-1-[(E)-(4-chloro­phen­yl)diazen­yl]ethen­yl}-N,N-di­methyl­aniline

The asymmetric unit of the title compound comprises three independent mol­ecules of similar geometry. The crystal structure is stabilized by inter­molecular C—H⋯N and C—H⋯Cl hydrogen bonds in addition to C—Cl⋯π inter­actions.

Crystal structure and Hirshfeld surface analysis of one-dimensional copper(II) coordination polymer incorporating succinate and tetra­methyl­ethylene­diamine ligands

The title compound, {[Cu(succ)(tmeda)]·4H₂O}_n, consists of one-dimensional polymeric chains in which the central metal atom is coordinated in a distorted square-planar geometry by one oxygen atom each from two succ ligands and two TMEDA ligand nitro­gen atoms.

Comparison of two Mn^IVMn^IV-bis-μ-oxo complexes {[Mn^IV(N₄(6-Me-DPEN))]₂(μ-O)₂}²⁺ and {[Mn^IV(N₄(6-Me-DPPN))]₂(μ-O)₂}²⁺

The addition of tert-butyl hydro­peroxide (^tBuOOH) to two Mn^II complexes, differing by a small synthetic alteration from an ethyl to a propyl linker in the ligand scaffold, results in the formation of the high-valent bis-oxo complexes {[Mn^IV(N₄(6-Me-DPEN))]₂(μ-O)₂}²⁺ (1) and {[Mn^IV(N₄(6-Me-DPPN))]₂(μ-O)₂}²⁺ (2).

Reductive cleavage of N,N′-di-tert-butyl­carbodi­imide generates tert-butyl­cyanamide ligands, (Me₃CNCN)⁻, that bind potassium both end-on and side-on in the same single crystal

The crystal structure is reported of a single crystal containing potassium salts of two different tert-butyl­cyanamide anions that co-crystallized with one equivalent of 1,3-di-tert-butyl urea.

Methyl 3-[(1-benzyl-4-phenyl-1H-1,2,3-triazol-5-yl)formamido]­propano­ate: crystal structure, Hirshfeld surface analysis and computational chemistry

The title compound is constructed about a tri-substituted 1,2,3-triazole ring, with the substituent at the C atom flanked by the C and N atoms being a substituted amide group, and with the adjacent C and N atoms bearing phenyl and benzyl groups, respectively. In the crystal, pairwise amide-N—H⋯O(carbon­yl) hydrogen bonds give rise to a centrosymmetric dimer.

Two N-{[4-(3-aryl-4-sydnonyl­idene­amino)-5-sulfan­ylidene-1H-1,2,4-triazol-3-yl]meth­yl}benzamides as disordered ethanol monosolvates

In each of the title newly synthesized and closely related N-{[4-(3-aryl-4-sydnonyl­idene­amino)-5-sulfanyl­idene-1H-1,2,4-triazol-3-yl]meth­yl}benzamides, which crystallized as ethanol monosolvates, the independent components are linked by hydrogen bonds to form centrosymmetric four-mol­ecule aggregates.

Phenol hemihydrate: redetermination of the crystal structure by neutron powder diffraction, Hirshfeld surface analysis and characterization of the thermal expansion

The existing crystal structure of phenol hemihydrate is shown to be incorrect and a new model, refined from high-resolution neutron powder diffraction data, is reported.

Crystal structure of 4-methyl-N-propyl­benzene­sulfonamide

The title compound comprises two mol­ecules in the asymmetric unit. Inter­molecular C—H⋯O and N—H⋯O hydrogen bonds lead to a three-dimensional network structure.

Crystal structure, Hirshfeld surface analysis and DFT studies of (E)-4-methyl-2-{[(4-methyl­phen­yl)imino]­meth­yl}phenol

The title compound, C₁₅H₁₅NO, shows an intra­molecular O—H⋯N hydrogen bond and the aromatic rings are tilted by 45.73 (2)°.

4-Nitro­benzyl 3,4-bis­(acet­yloxy)-2-(4-meth­oxy­phen­yl)pyrrolidine-1-carboxyl­ate: crystal structure, Hirshfeld surface analysis and computational chemistry

The title compound, containing a tetra-substituted pyrrolidine ring, has an N-bound (equatorial) 4-nitro­phen­yl)ethyl­carboxyl­ate group with an adjacent C-bound 4-meth­oxy­phenyl (bis­ectional) and then two acet­yloxy subtituents in equatorial and axial positions, respectively. The five-membered ring is twisted about the bond bearing the acet­yloxy subtituents.

Crystal structure of {μ₂-1,2-bis­[(4-methyl­phenyl­sulfan­yl]-3-oxoprop-1-ene-1,3-diyl-1:2κ²C³:C¹}dicarbonyl-1κ²C-[μ₂-methyl­enebis(di­phenyl­phos­phane)-1:2κ²P:P′](tri­phenyl­phosphane-2κP)iron­platinum(Fe—Pt), [(OC)₂Fe(μ-dppm){μ-C(=O)C(4-MeC₆H₄SCH₂)=CCH₂SC₆H₄Me-4}Pt(PPh₃)]

The title compound represents the first example of a diphosphane-bridged heterobimetallic Fe—Pt dimetalla­cyclo­pentenone complex resulting from a bimetallic activation of metal-coordinated carbonyl ligand with an inter­nal alkyne, namely 1,4-bis­(p-tolyl­thio)­but-2-yne. The bridging μ₂-C(= O)C(CH₂SC₆H₄Me-4)=CCH₂SC₆H₄Me-4 unit (stemming from a carbon–carbon coupling reaction between CO and the triple bond of the alkyne di­thio­ether) forms a five-membered dimetalla­cyclo­pentenone ring, in which the C=C bond is π-coordinated to the Fe center.

Crystal structure and Hirshfeld surface analysis of 4-{[(E)-4-(hept­yloxy)benzyl­idene]amino}-N-(naphthalen-2-yl)-1,3-thia­zol-2-amine

Charge-assisted C—H⋯π hydrogen bonds along with π–π inter­actions stabilize the crystalline state. Inter­molecular inter­actions are qu­anti­fied by Hirshfeld surface analysis.

Crystal structure of 5-[(benzo­yloxy)meth­yl]-5,6-dihy­droxy-4-oxo­cyclo­hex-2-en-1-yl benzoate

The crystal structure 5-[(benzo­yloxy)meth­yl]-5,6-dihy­droxy-4-oxo­cyclo­hex-2-en-1-yl benzoate a natural product from Pipers griffithii leaves known as zeylenone has been determined.

The crystal structure, Hirshfeld surface analysis and energy frameworks of 2-[2-(meth­oxy­carbon­yl)-3,6-bis­(meth­oxy­meth­oxy)phen­yl]acetic acid

The title compound, 2-(2-(meth­oxy­carbon­yl)-3,6-bis­(meth­oxy­meth­oxy)phen­yl)acetic acid, was synthesized as an inter­mediate for a possible total synthesis of the isocoumarin 3-methyl-3,5,8-trihy­droxy-3,4-di­hydro­isocoumarin.

Crystal structures and Hirshfeld surface analyses of 6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one and 5-bromo-6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one chloro­form monosolvate

Bromination of 6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one resulted in the formation of the 5-bromo derivative, 5-bromo-6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one. The two mol­ecules differ essentially in the orientation of the meth­oxy group on position 6 of the isocoumarin ring system.

Crystal structure and Hirshfeld surface analysis of the ortho­rhom­bic polymorph of a Zn^II complex with 3,5-di­nitro­benzoic acid and ethyl­enedi­amine

During systematic investigations of the biological action enhancement of well known compounds, a new metal complex, (ethane-1,2-di­amine)­bis­(3,5-di­nitro­benzoato)zinc(II), was synthesized and the structure of its ortho­rhom­bic form has determined. The zinc ion has a distorted tetra­hedral environment formed by two monodentate 3,5-di­nitro­benzoato anions and chelating ethyl­enedi­amine mol­ecule.

Syntheses and crystal structures of the quaternary thio­germanates Cu₄FeGe₂S₇ and Cu₄CoGe₂S₇

The isostructural crystal structures of Cu₄FeGe₂S₇ and Cu₄CoGe₂S₇ were solved and refined. All the metal cations form MS₄ tetra­hedra and share corners to create a three-dimensional, non-centrosymmetric structure.

Crystal structure and Hirshfeld surface analysis of 4-{2,2-di­chloro-1-[(E)-2-(4-methyl­phen­yl)diazen-1-yl]ethen­yl}-N,N-di­methyl­aniline

In the title compound, the benzene rings make a dihedral angle of 62.73 (9)° with each other. In the crystal, mol­ecules are linked by a pair of C—Cl⋯π inter­actions, forming an inversion dimer. A short HL⋯·HL contact links the dimers, forming a ribbon propagating along the c-axis.

Polymorphism of bis­(1,3-benzo­thia­zol-2-yl) tri­thio­carbonate

Bis(benzo­thia­zol-2-yl)tri­thio­carbonate, C₁₅H₈N₂S₅, crystallizes in two visually distinguishable polymorphs, each containing a different conformer of the title compound and featuring different kinds of intra- and inter­molecular S⋯S, S⋯N and π–π inter­actions.

Crystal structure of the [(THF)Cs(μ-η⁵:η⁵-Cp′)₃Yb]_n oligomer

Reduction of (C₅H₄SiMe₃)₃Yb^III in THF using excess Cs metal forms the oligomeric complex [(THF)Cs(μ-η⁵:η⁵-Cp′)₃Yb^II]_n. The complex has hexa­gonal layers of Cs₃Yb₃ with THF ligands and Me₃Si groups in between the layers.

Crystal structure of posnjakite formed in the first crystal water-cooling line of the ANSTO Melbourne Australian Synchrotron MX1 Double Crystal Monochromator

Exceptionally large crystals of posnjakite, Cu₄SO₄(OH)₆(H₂O), formed during corrosion of a Swagelock(tm) Snubber copper gasket within the MX1 beamline at the ANSTO-Melbourne, Australian Synchrotron. The crystal structure was solved using synchrotron radiation and revealed a structure based upon [Cu₄(OH)₆(H₂O)O] sheets, which contain Jahn–Teller-distorted Cu octa­hedra.

Selective synthesis and crystal structures of manganese(I) complexes with a bi- or tridentate terpyridine ligand

The structural comparison of two Mn carbonyl complexes comprising a terpyridine derivative engaged in bidentate or tridentate coordination of the central Mn^I atom is reported.

Crystallographic and spectroscopic characterization of racemic Mosher's Acid

Mosher's Acid (systematic name: 3,3,3-tri­fluoro-2-meth­oxy-2-phenyl­propanoic acid) is a carb­oxy­lic acid that when resolved can be employed as a chiral derivatizing agent. The two independent mol­ecules in the asymmetric unit form a non-centrosymmetric homochiral dimer via inter­molecularly hydrogen-bonded head-to-tail dimers with graph-set notation (8).

Crystal structure and Hirshfeld surface analysis of 2-{[(4-iodo­phen­yl)imino]­meth­yl}-4-nitro­phenol

In the title Schiff base compound, C₁₃H₉IN₂O₃, the hy­droxy group forms a intra­molecular hydrogen bond to the imine N atom and generates an S(6) ring motif. The 4-iodo­benzene ring is inclined to the phenol ring by 39.1 (2)°. The configuration about the C=N bonds is E. The crystal structure features C—H⋯O hydrogen-bonding inter­actions.

2,2′-(Disulfanedi­yl)di­benzoic acid N,N-di­methyl­formamide monosolvate: crystal structure, Hirshfeld surface analysis and computational study

In the title 1:1 solvate, 2,2′-di­thiodi­benzoic acid (DTBA):di­methyl­formamide (DMF), the DTBA mol­ecule is twisted [C—S—S—C = −88.57 (6)°]. Four-mol­ecule aggregates are formed in the crystal via DTBA-O—H⋯O(DMF) and DTBA-O—H⋯O(DTBA) hydrogen bonding. These are connected in three-dimensions by benzene-C—H⋯O(DTBA), DTBA-C=O⋯π(benzene) and benzene-C—H⋯π(benzene) inter­actions.

Synthesis and crystal structures of 3-hy­droxy-2,4-di­methyl-2H-thio­phen-5-one and 3-hy­droxy-4-methyl-2H-thio­phen-5-one

The structures of two hy­droxy-thio­phenone derivatives related to the anti­biotic thiol­actomycin are presented. The main structural feature of both compounds is C(6) hydrogen-bonded chains formed between the OH and C=O groups.

Synthesis and crystal structures of 2-(ferrocenyl­carbon­yl)benzoic acid and 3-ferrocenylphthalide

2-Ferrocenyl­carbonyl­benzoic acid (C₁₈H₁₄FeO₃) was synthesized from the Friedel–Crafts acyl­ation of ferrocene with phthalic anhydride, and the product was reduced to 3-ferrocenylphthalide (C₁₈H₁₄FeO₂) using Zn(Cu) in aqueous sodium hydroxide. Both compounds were characterized using IR, NMR, and single-crystal X-ray analysis.

Crystal structure and Hirshfeld surface analysis of 1-methyl-4-(2-methyl-10H-benzo[b]thieno[2,3-e][1,4]diazepin-4-yl)piperazin-1-ium 2,5-di­hydroxy­benzoate propan-2-ol monosolvate

The asymmetric unit of the title salt consists of an olanzapinium cation, an independent 2,5 di­hydroxy­benzoate anion and a solvent isopropyl alcohol mol­ecule. The central seven-membered heterocycle is in a boat conformation, while the piperazine ring displays a distorted chair conformation. The dihedral angle between the benzene and thiene rings flanking the diazepine ring is 52.58 (19)°. In the crystal, the anions and cations are connected by N—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network.