Nitro­sonium complexation by the tetra­phospho­nate cavitand 5,11,17,23-tetra­methyl-6,10:12,16:18,22:24,4-tetra­kis­(phenyl­phospho­nato-κ²O,O)resorcin(4)arene

Resorcinarene-based tetra­phospho­nate cavitands are versatile mol­ecular receptors which combine a π-basic aromatic cavity with hydrogen-bond acceptor groups at their upper rim. Their complexation properties span from neutral mol­ecules to cationic species, and have been extensively studied both in solution and in the solid state. In this paper, we report the NMR solution studies and the crystal structure of a new supra­molecular complex between a tetra­phospho­nate cavitand and the nitrosyl cation NO⁺. The cation is disordered over two equivalent positions, and inter­acts with two adjacent P=O groups at the upper rim of the cavitand through a dipole–charge inter­action.

Crystal structure of the Ba^II-based Co^II-containing one-dimensional coordination polymer poly[[aqua{μ₄-2,2′-[(4,10-di­methyl-1,4,7,10-tetra­aza­cyclo­dodecane-1,7-di­yl)bis­(methyl­idene)]bis­(4-oxo-4H-pyran-3-olato)}­perchloratocobaltbarium] perchlorate]

A barium-μ₂-oxygen motif develops along the a axis, connecting symmetry-related dinuclear Ba^II–Co^II cationic fragments in a wave-like chain, forming a one-dimensional metal coordination polymer. Non-coordinating ClO₄⁻ anions are located in the space between the chains in this first example of a macrocyclic ligand forming a Ba^II-based one-dimensional coordination polymer, containing Co^II ions surrounded by a N₄O₂ donor set.

Crystal structure and Hirshfeld surface analysis of (2E,2′E)-3,3′-(1,4-phenyl­ene)bis­[1-(2,4-di­fluoro­phen­yl)prop-2-en-1-one]

The asymmetric unit of the title compound consists of one and a half bis­chalcone mol­ecules. In the crystal, mol­ecules are linked into a three-dimensional network by C—H⋯F and C—H⋯O hydrogen bonds, some of the C—H⋯F links being unusually short (< 2.20 Å). Hirshfeld surface analyses are presented and discussed.

Crystal structure of di­ethyl 3,3′-[(2,4-di­chloro­phen­yl)methyl­idene]bis­(1H-indole-2-carboxyl­ate)

In the title compound, the two indole ring systems are approximately perpendicular to one another, making a dihedral angle of 80.9 (5)°. In the crystal, pairs of N—H⋯O hydrogen bonds link the mol­ecules into inversion dimers and these are further linked by N—H⋯O and hydrogen bonds and short Cl—Cl contacts into supra­molecular chains.

Crystal structure of N-[6-amino-5-(benzo[d]thia­zol-2-yl)-3-cyano-4-methyl­sulfanyl-2-oxo-1,2-di­hydro­pyridin-1-yl]-4-methyl­benzene­sulfonamide di­methyl­formamide monosolvate

In the title compound, the toluene­sulfonamide ring and the combined ring system involving the pyridone and benzo­thia­zole rings subtend an inter­planar angle of 39.86 (4)°. The pyridone and benzo­thiazyl rings are linked by an intra­molecular N—H_amine⋯N_thia­zole hydrogen bond. The mol­ecules are linked by hydrogen bonds and an S⋯O contact to form layers parallel to the bc plane.

Crystal structure of the formal 20 electron zirconocene penta­fulvene complex Cp₂Zr(η⁵,η¹-adamantyl­idene­penta­fulvene):toluene:n-hexane = 1:0.125:0.125

The mol­ecular and crystal structure of a formal 20 electron zirconium(IV) complex bearing two cyclo­penta­dienyl and one sterically demanding penta­fulvene ligand is reported in which the penta­fulvene is bound in an η⁵:η¹ manner. The complex crystallizes together with toluene and n-hexane in a ratio of 1:0.125:0.125.

Crystal structure of (1S,2R)-2-hy­droxy-1,2-di­phenyl­ethan-1-aminium (S)-2-aza­niumyl­butane­dioate monohydrate

The title diastereomeric salt, formed between 2-amino-1,2-di­phenyl­ethanol (ADE) and aspartic acid (ASP), crystallizes as a monohydrate. In the crystal, the ASP anions are linked via N—H⋯O hydrogen bonds to form a 2₁ helix along the b-axis direction.

Synthesis and crystal structure of a new pyridinium bromide salt: 4-methyl-1-(3-phen­oxy­prop­yl)pyridinium bromide

The simple synthesis and crystal structure of a new pyridinium bromide salt, 4-methyl-1-(3-phen­oxy prop­yl)pyridinium bromide, are reported. The C–H⋯Br⁻ inter­actions have an effect on the NMR signals of the ortho- and meta-pyridinium protons.

Crystal structures of (E)-1-{3-[(5-fluoro-2-hy­droxy­benzyl­idene)amino]­phen­yl}ethanone and of a fourth polymorph of (E)-1-{3-[(2-hy­droxy-3-meth­oxy­benzyl­idene)amino]­phen­yl}ethanone

The mol­ecules of the title compounds are effectively planar, apart from the methyl H atoms. In the crystals, C—H⋯O hydrogen bonds link the mol­ecules into chains in one compound and into sheets in the other.

Crystal structures of two 1:2 dihydrate compounds of chloranilic acid with 2-carb­oxy­pyridine and 2-carb­oxy­quinoline

Crystal structures of hydrogen-bonded 1:2 dihydrate compounds of chloranilic acid with 2-carb­oxy­pyridine (I) and 2-carb­oxy­quinoline (II) have been determined at 180 and 200 K, respectively. The base mol­ecule in (I) is disordered over cationic and twitterionic states, while that in (II) is in a twitterionic form. In each crystal, the three components are linked by O—H⋯O and N—H⋯O hydrogen bonds, forming a layer structure.

Crystal structures of 1-hy­droxy-4-prop­yloxy-9,10-anthra­quinone and its acetyl derivative

The title compounds were synthesized from the commercially available dye quinizarin. In both compounds, the anthra­quinone frameworks are close to planarity but there is a large difference in the conformation of the prop­yloxy group.

Crystal structures of two (Z)-2-(4-oxo-1,3-thia­zolidin-2-yl­idene)acetamides

The crystal structures of two (oxo­thia­zolidin-2-yl­idene)acetamides, namely (Z)-2-[2-(morpholin-4-yl)-2-oxo­ethyl­idene]thia­zolidin-4-one and (Z)-N-(4-meth­oxy­phen­yl)-2-(4-oxo­thia­zolidin-2-yl­idene)acetamide are described and compared with a related structure.

Crystal structure of BaMn₂(AsO₄)₂ containing discrete [Mn₄O₁₈]²⁸⁻ units

BaMn₂(AsO₄)₂ was isolated from a high-temperature halide flux. Its crystal structure is characterized by infinite sheets made up of AsO₄ units and distorted MnO₆ octa­hedra while barium cations inter­leave successive sheets. The layered framework comprises weakly inter­acting [Mn₄O₁₈]²⁸⁻ tetra­meric units. These units in the neighboring layer are separated from each other by 6.614 (2) Å (Mn⋯Mn distance).

Crystal structure of (1S,4S)-2,5-diazo­niabi­cyclo[2.2.1]heptane dibromide

The mol­ecular structure of the 2,5-di­aza­bicyclo­[2.2.1]heptane parent ring has been characterized for the first time. The asymmetric unit contains two crystallographically independent cages of 2,5-di­aza­bicyclo­[2.2.1]heptane, each cage being protonated at the two nitro­gen sites. The overall charge balance is maintained by four crystallogrphically independent bromide ions. In the crystal, the components of the structure are linked via a complex three-dimensional network of N—H⋯Br hydrogen bonds.

Crystal structure of r-1,c-2-di­benzoyl-t-3,t-4-bis­(2-nitro­phen­yl)cyclo­butane

The title mol­ecule is a tetra­substituted truxinic-type cyclo­butane derivative with a central ring that is almost planar despite of being placed in a general position. The mol­ecular structure of the dimer shows that the four benzene rings of the substituents are oriented in such a way that potential steric hindrance is minimized, whilst allowing some degree of inter­molecular π–π inter­actions for crystal stabilization.

A one-dimensional Hg^II coordination polymer based on bis­(pyridin-3-ylmeth­yl)sulfane

The reaction of Hg^II with the bridging ligand bis­(pyridin-3-ylmeth­yl)sulfane afforded a one-dimensional zigzag chain polymeric structure, with the charge balanced by two coordinated chloride anions. C—H⋯Cl hydrogen bonds and Hg—Cl⋯π inter­actions, together with C—H⋯π hydrogen bonds, stabilize the crystal structure.

Crystal structure of aqua­(1H-pyrazole-κN²)(pyridine-2,6-di­carboxyl­ato-κ³O²,N,O⁶)copper(II) dihydrate

The synthesis and crystal structure of tridentate pyridine-2,6-di­carboxyl­ate Cu^II complex with a heterocyclic pyrazole ligand, a potential candidate for metal catalysts, are reported. The Cu^II atom is coordinated by three O atoms and two N atoms, provided by a tridentate pyridine-2,6-di­carboxyl­ate, one pyrazole and one water ligand, forming a slightly distorted square-pyramidal geometry.

Crystal structures of salen-type ligands 2-[(1E)-({1-(3-chloro­phen­yl)-2-[(E)-(2-hy­droxy­benzyl­idene)amino]­prop­yl}imino)­meth­yl]phenol and 2-[(1E)-({1-(4-chloro­phen­yl)-2-[(E)-(2-hy­droxy­benzyl­idene)amino]­prop­yl}imino)­meth­yl]phenol

The title compounds are differing only by the position of the chlorine atom in the benzene ring. The mol­ecular structures are very similar, except for the relative position of the hy­droxy­phenyl rings.

Crystal structure of a zigzag Co^II coordination polymer: catena-poly[[di­chlorido­bis­(methanol-κO)cobalt(II)]-μ-bis­(pyridin-3-ylmeth­yl)sulfane-κ²N:N′]

In the title compound, each Co^II ion is coordinated by two pyridine N atoms from two individual dipyridyl ligands, two methanol O atoms and two chloride anions in an elongated octa­hedral geometry. Each dipyridyl ligand links two Co^II ions, forming infinite zigzag chains.

Stoichiometric and polymorphic salt of imidazolium picrate monohydrate

An aqueous 1:1 co-crystal salt formed from imidazole and picric acid was obtained in methanol solution. A three-dimensional hydrogen-bonded network is formed in the crystal by N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds and is further consolidated by π–π stacking inter­actions between pairs of imidazolium cations and picrate anions.

A new monoclinic polymorph of N-(3-methyl­phen­yl)eth­oxy­carbo­thio­amide: crystal structure and Hirshfeld surface analysis

Two mol­ecules comprise the asymmetric unit in the title thio­amide mol­ecule, each of which exists as the thioamide–thione tautomer. In the crystal, the mol­ecules assemble via an eight-membered thio­amide {⋯SCNH}₂ synthon to form dimeric aggregates.

Crystal structure of poly[[μ₃-(S)-2-amino-3-hy­droxy­propano­ato]-cis-di-μ-chlorido-caesium­palladium(II)]

This compound was previously shown to have anti­cancer activity in rodent test systems and recently found to have anti­fungal activity. The Pd centre is in a square-planar coordination environment with two chlorine atoms in cis positions and the remaining two coordination sites being coordinated by N and O atoms from deprotonated L-serine. Each of the Cs cations shows ninefold coordination with six chlorine and three O atoms resulting in a coordination environment that is similar to the well known Cs₂SO₄ structure.

Deca­chloro­cyclo­penta­silanes coordinated by pairs of chloride anions, with different cations, but the same solvent mol­ecules

The planar deca­chloro­cyclo­penta­silane rings in the title compounds are coordinated by two chloride ions to generate inverse-sandwich complexes.

Buthalital and methitural – 5,5-substituted derivatives of 2-thio­barbituric acid forming the same type of hydrogen-bonded chain

In the title structures, each mol­ecules is connected to two other mol­ecules via four N—H⋯O hydrogen bonds, resulting in a chain with a sequence of (8) rings.

Crystal structures of 2,6-di­bromo-4-methyl­benzo­nitrile and 2,6-di­bromo-4-methyl­phenyl isocyanide

The title crystals are isomorphous, with tetra­meric Br⋯Br contacts as the principal packing inter­action. No CN⋯Br or NC⋯Br contacts are observed.

Crystal structure of cis-1-phenyl-8-(pyridin-2-ylmeth­yl)dibenzo[1,2-c:2,1-h]-2,14-dioxa-8-aza-1-borabi­cyclo­[4.4.0]deca-3,8-diene

The present work describes the synthesis and crystal structure of the new B-phenyl­oxaza­borocine, C₂₆H₂₃BN₂O₂. The title compound adopts a zwitterionic form with a significant intra­molecular N→B dative bond and inter­molecular C—H⋯O inter­actions connecting mol­ecules parallel to the b axis.

Formation and structural characterization of a europium(II) mono(scorpionate) complex and a sterically crowded pyraza­bole

Reaction of EuI₂(THF)₂ with K[HB(3,5-^iPr2pz)] (= KTp^iPr2, pz = pyrazol­yl) afforded the new europium(II) scorpionate complex (KTp^iPr2)(3,5-^iPr2pzH)₂Eu^III (1) in addition to the sterically crowded pyraza­bole derivative trans-{(3,5-^iPr2pz)HB(μ-3,5-^iPr2pz)}₂ (2) which were both structurally characterized through X-ray diffraction.

Crystal structure of poly[[di-μ₃-acetato-tetra­aqua­bis­(μ₂-cyclo­hexane-1,4-di­carboxyl­ato)dilanth­anum(III)] dihydrate]

The title compound is a binuclear lanthanum(III) complex having each metal ion in deca­coordination with oxygen atoms from 1,4-chdc²⁻ ligands, acetate groups and coordinated water mol­ecules to form a distorted bicapped square anti­prismatic geometry. The strong inter­molecular O–H⋯O and weak C–H⋯O inter­actions lead to the construction of a three-dimensional supra­molecular architecture.

Crystal structure of 3,6,6-tri­methyl-4-oxo-1-(pyridin-2-yl)-4,5,6,7-tetra­hydro-1H-indazol-7-aminium chloride and its monohydrate

In the title compounds 1 and 2, the organic moieties adopt flattened conformations stabilized by an intra­molecular N—H⋯N hydrogen bonds formed by the protonated amino group and the N atom of the pyridyl substituent. In 1, the organic moieties are linked with two N—H⋯Cl⁻-type hydrogen bonds, forming a C(4) graph-set. In its monohydrate, 2, the Cl⁻ anion and a water mol­ecule assemble the moieties into infinite bands showing hydrogen-bond patterns with graph sets C(6), (12) and (8). Both crystals display π–π stacked supra­molecular structures running along the b axis.

Crystal structure, thermal and fluorescence properties of 2,2′:6′,2′′-terpyridine-1,1′,1′′-triium tetra­chlorido­nickelate(II) chloride

The synthesis, and structural determination of 2,2′:6′,2′′-terpyridine-1,1′,1′′-triium tetra­chlorido­nickelate(II) chloride are reported. The crystal structure features N—H⋯Cl and C—H⋯Cl hydrogen bonds and Ni—Cl⋯π ring inter­actions.

Crystal structure of a di­aryl carbonate: 1,3-phenyl­ene bis­(phenyl carbonate)

The whole mol­ecule of the title di­aryl­carbonate is generated by mirror symmetry, the mirror bis­ecting the central benzene ring, and the carbonate groups adopt an s-cis-s-cis conformation. In the crystal, there are only weak C—H⋯O hydrogen bonds and offset π–π inter­actions present.

Crystal structures of three ortho-substituted N-acyl­hydrazone derivatives

The effect of the nature of substitutions on the structural parameters and hydrogen-bonding inter­actions in N-acyl­hydrazone derivatives has been studied by synthesizing and determining the crystal structures of three ortho-substituted N-acyl­hydrazone derivatives, namely (E)-N-{2-[2-(2-chloro­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (I), (E)-N-{2-[2-(2-methyl­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (II) and (E)-N-{2-[2-(2-nitro­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (III).

Crystal structure of mer-tris­{2,6-di­fluoro-3-[5-(2-fluoro­phen­yl)pyridin-2-yl-κN]pyridin-4-yl-κC⁴}iridium(III) di­chloro­methane hemisolvate n-hexane hemisolvate

Iridium(III) complexes based on 2,3′-bi­pyridine ligands are known to exhibit strong emission from blue to green that makes them of inter­est for organic light-emitting diodes and organic lighting uses. In the title compound, the Ir^III ion adopts a distorted octa­hedral coordination environment defined by three C,N-chelating 2,6-di­fluoro-3-[5-(2-fluoro­phen­yl)pyridin-2-yl]pyridin-4-yl ligands in a meridional manner. In the crystal, inter­molecular C—H⋯F and C—H⋯π hydrogen bonds, as well as inter­molecular C—F⋯π inter­actions, are present, leading to a two-dimensional network.

Crystal structure of di­ethyl 3,3′-[(4-nitro­phen­yl)methyl­ene]bis­(1H-indole-2-carboxyl­ate)

In the title compound, the two indole ring systems are approximately perpendicular to one another, making a dihedral angle of 89.7 (5)°. In the crystal, pairs of N—H⋯O hydrogen bonds link the mol­ecules into the inversion dimers, which are further linked into supra­molecular chains.

Crystal structure of bis­{μ₂-2,2′-[(4,10-di­methyl-1,4,7,10-tetra­aza­cyclo­dodecane-1,7-di­yl)bis­(meth­ylene)]bis­(4-oxo-4H-pyran-3-olato)}dicobalt­calcium bis­(perchlorate) 1.36-hydrate

The title compound is a new heterotrinuclear Co^II–Ca^II–Co^II dimer of L1. L1 undergoes a cobalt-driven preorganization, leading to the formation of an electron-rich area able to host a hard metal ion such as Ca^II. In the dimer, two neutral [Co(H_–2L1)] moieties, held together by the Ca^II ion, are rotated by 90°. The trinuclear complexes form layers perpendicular to the c axis; the perchlorate anions are located between the layers and inter­act with the complexes, as well as the lattice water mol­ecules.

Crystal structure and Hirshfeld surface analysis of hexa­kis­(μ-benzoato-κ²O:O′)bis­(pyridine-3-carbo­nitrile-κN¹)trizinc(II)

The asymmetric unit of the title complex contains one half of the complex mol­ecule, one and a half Zn^II cations, three benzoate (Bnz) and one pyridine-3-carbo­nitrile (CPy) mol­ecule; the Bnz anions act as bidentate ligands through the carboxyl­ate O atoms, while the Cpy anion acts as a monodentate N(pyridine)-bonding ligand. The complete centrosymmetric trinuclear complex thus comprises a linear array of three Zn^II cations. In the crystal, the Bnz anions link to the Cpy N atoms via weak C—H⋯N hydrogen bonds, forming a two-dimensional network. The Hirshfeld surface analysis confirms the role of H-atom contacts in establishing the packing.

Crystal structure of methyl 2-[5-(2-hy­droxy­phen­yl)-2H-tetra­zol-2-yl]acetate

The title compound, methyl 2-[5-(2-hy­droxy­phen­yl)-2H-tetra­zol-2-yl]acetate, is the major product from the reaction between 2-(2H-tetra­zol-5-yl)phenol and methyl 2-bromo­acetate in the presence of potassium carbonate, which gave three isomeric products.

Crystal structure of 3-(4,4-di­fluoro-5,7-di­methyl-4-bora-3a,4a-di­aza-s-indacen-3-yl)propanoic acid

The crystal structure of the title compound has been determined at 100 K. In the crystal, O—H⋯O, C—H⋯On and C—H⋯F hydrogen bonds, and C—H⋯π and π–π inter­actions connect neighbouring mol­ecules.

Crystal structure of catena-poly[[[tetra­aqua­iron(II)]-trans-μ-1,2-bis­(pyridin-4-yl)ethene-κ²N:N′] bis­(p-toluene­sulfonate) methanol disolvate]

The 1,2-bis­(pyridin-4-yl)ethene mol­ecules bridge Fe^II cations to form polymeric chains running along the a axis.