Two Fe₃(μ₃-S)₂(CO)₈ clusters with terminal N-heterocyclic carbenes

Two Fe₃(CO)₈(μ₃-S)₂ clusters with terminal N-heterocyclic carbenes have been synthesized. Of the eight carbonyl ligands, one deviates significantly from linearity. In one cluster, N—H⋯S and C—H⋯O hydrogen bonds combine the mol­ecules into [101] sheets, while in the other cluster, N—H⋯S and C—H⋯O inter­actions link the mol­ecules into [111] chains.

Redetermination of NaGdS₂, NaLuS₂ and NaYS₂

The title structures have been redetermined in order to improve the structural data of the rhombohedral series of group 1 rare earth sulfides. The observed dependence of the fractional coordinate z(S²⁻) on the identity of the rare earth element in the newly determined structures is in agreement with the known structures of the potassium and rubidium analogues.

(8RS)-4-Amino-6-(4-chloro­phenyl)-8-(2,4-di­chloro­thia­zol-5-yl)-8,9-di­hydro-7H-pyrimido[4,5-b][1,4]diazepine N,N-di­methyl­formamide mono­solvate: sheets built from N—H⋯N and C—H⋯O hydrogen bonds

The molecular components of a solvated 7H-pyrimido[4,5-b][1,4]diazepine derivative are linked by hydrogen bonds to form sheets containing four types of hydrogen-bonded ring.

Two nickel(II) bis­[(pyridin-2-yl)meth­yl]amine complexes with homophthalic and benzene-1,2,4,5-tetra­carb­oxy­lic acids

Two new Ni^II complexes are presented, i.e. a one-dimensional polymeric complex incorporating homophthalate, where the anion acts as the bridging ligand, and a complex incorporating benzene-1,2,4,5-tetra­carboxyl­ate, with two independent Ni centres in different environments, one of them a centrosymmetric 4− dinuclear complex and the other a 2+ mononuclear unit, appearing in a 1:2 ratio. The supra­molecular structure is supported by a profuse hydrogen-bonding network.

2,2′-Bi[benzo[b]thio­phene]: an unexpected isolation of the benzo[b]thio­phene dimer

The cross-coupling reaction of (benzo[b]thiophen-2-yl)tributylstannane and 2-chloro-3-methylpyridine using a palladium catalyst gave the desired product in excellent yield, but resulted in the unexpected isolation of the benzo[b]thiophene dimer present in trace quantities (2–3 mol%) during recrystallization. Two independent half-molecules of this dimer comprise the symmetric unit, and the dimers exhibit ring disorder.

A new semiconducting quaternary mixed halogenide: penta­thallium dimercury penta­bromide tetra­iodide, Tl₅Hg₂Br₅I₄

A novel semiconducting quaternary mixed halogenide, Tl₅Hg₂Br₅I₄, represents a new series of composite structures described by the general formula nTlBr*mTl₂[HgBr₂I₂].

Folded conformations due to arene inter­actions in dissymmetric and symmetric butyl­idene-linker models based on pyrazolo­[3,4-d]pyrimidine, purine and 7-de­aza­purine

Three butyl­idene-linker models have been designed and synthesized. They show intra­molecular folding in solution and also, more importantly, in the solid state. These folded conformations in the solid are mainly stabilized by inter­actions between arene groups.

A novel dinuclear bis­muth(III) coordination compound: bis­(μ-pyridine-2,6-di­carboxyl­ato)-κ⁴O²,N,O⁶:O^6′;κ⁴O²:O^2′,N,O⁶-bis­[(azido-κN)(1,10-phenanthroline-κ²N,N′)bis­muth(III)] tetra­hydrate

In the centrosymmetric dimeric fragment of the title compound, each Bi^III centre is seven-coordinated by three O atoms and four N atoms in a distorted penta­gonal–bipyramidal geometry. The three-dimensional supra­molecular structure is assembled via O—H⋯O hydrogen bonds and two types of π–π stacking inter­actions.

Mol­ecular and supra­molecular ionic aggregates H_xO_y^z in organic and organometallic crystalline hydrates

Fully developed supra­molecular aggregates H_xO_y^z exhibit three modes of hydrogen bonding with characteristic contiguous O⋯O distances. These distances can be used to identify hydrate species and to guide H-atom placement.

Substituent effects in trans-p,p′-di­substituted azo­benzenes: X-ray structures at 100 K and DFT-calculated structures

The crystal and mol­ecular structures of two para-substituted azo­benzenes with π-electron-donating –NEt₂ and π-electron-withdrawing –COOEt groups are reported, along with the effects of the substituents on the aromaticity of the benzene ring. Density functional theory (DFT) calculations were performed to analyse the differences in the geometry and aromaticity of the studied compounds in the crystalline state and for the isolated mol­ecules.

Hydrogen ADPs with Cu Kα data? Invariom and Hirshfeld atom modelling of fluconazole

For the structure of fluconazole monohydrate, a case study on different model refinements is reported, based on single-crystal X-ray diffraction data measured at 100 K with Cu Kα radiation to a resolution of sin θ/λ of 0.6 Å⁻¹. The structure, anisotropic displacement parameters (ADPs) and figures of merit from the independent atom model are compared to `invariom' and `Hirshfeld atom' refinements.

A novel alkaline earth strontium(II) coordination polymer: poly[hexa­aqua­tetra­kis­(μ₅-pyridine-2,6-di­carboxyl­ato)bis­(μ₄-pyridine-2,6-di­carboxyl­ato)(μ₇-sulfato)­hepta­strontium(II)]

The title compound has been synthesized by an ionothermal method. The compound not only exhibits a three-dimensional structure with a unique coordination mode of the sulfate anion, but also features the first example of a hepta­nuclear strontium(II) coordination polymer.

Preparation and X-ray analysis of potassium (2,3-di­chloro­phen­yl)glucosinolate

Crystals of biologically active potassium (2,3-di­chloro­phen­yl)glucosinolate were obtained as a dual solvate, containing one methanol and one ethanol mol­ecule of crystallization. The three-dimensional polymeric network consists of chains containing the potassium ions coordinated and bridged by sugar O atoms, which run parallel to the a axis and are further crosslinked through the sugar molecules.

Fe^III in a low-spin state in caesium bis­[3-ethoxysalicylaldehyde 4-methyl­thiosemicarbazonato(2–)-κ³O²,N¹,S]ferrate(III) methanol monosolvate

The Fe^IIIS₂N₂O₂ chromophore contains two O,N,S-donating dianionic 3-ethoxysalicylaldehyde 4-methyl­thiosemicarbazonate(2−) ligands in perpendicular planes, with the O and S atoms in cis positions and the N atoms in trans positions. The Fe^III cation is in the low-spin state at 100 K.

A copper(I) coordination polymer incorporation the corrosion inhibitor 1H-benzotriazole: poly[μ₃-benzotriazolato-κ³N¹:N²:N³-copper(I)]

1H-Benzotriazole (BTAH) has been used for the first time as a ligand to construct a copper(I) coordination polymer, viz. [Cu(BTA)]_n. [Cu₂(BTA)₂]₂ secondary building units form a one-dimensional chain along the c axis.

An organic–inorganic hybrid compound containing imidazolium cations and a one-dimensional lithium hexa­cyanido­cobaltate-based anionic framework

In an organic–inorganic hybrid compound, neighbouring [Co(CN)₆]³⁻ anionic units are linked by Li⁺ cations through the cyanide groups in a trans mode, forming a one-dimensional zigzag chain structure extending along the c axis. A three-dimensional supra­molecular network is formed through hydrogen-bonding inter­actions and is further stabilized by weak CN⋯π inter­actions between the cyanide groups and the imidazolium cations.

Two-dimensional coordination polymeric structures in caesium complexes with ring-substituted phen­oxy­acetic acids

Two-dimensional coordination polymeric structures have been found in the Cs salts of the 4-fluoro-, 3-chloro-2-methyl- and 2,4-dichloro- ring-substituted phenoxyacetic acids. These complexes exhibit irregular CsO₆ to CsO₈ coordination geometries and, in the case of the (2,4-dichlorophenoxy)acetate analogue, provide an example of a CsO₈Cl geometry involving a hydrogen bis(phenoxyacetate) ligand species.

A new three-dimensional coordination polymer of Sr^II based on dipicolinic acid, with different coordination environments for Sr^II

The reaction of dipicolinic acid with strontium yields a three-dimensional coordination polymer consisting of two independent Sr centres, two independent dipicolinate ligands (one doubly deprotonated and the other singly deprotonated) and two water mol­ecules. The dipicolinate ligands adopt μ₃- and μ₄-bridging modes, linking the alkaline earth metal centres into a three-dimensional coordination framework.

Octyl 1-(5-tert-butyl-1H-pyrazol-3-yl)-2-(4-chloro­phenyl)-1H-benzimid­azole-5-carboxyl­ate: complex sheets built from N—H⋯N, C—H⋯N and C—H⋯O hydrogen bonds

Hydrogen bonds link mol­ecules of the title compound into tripartite sheets, with the hydrogen bonds in the central layer and the hydro­carbyl substituents on the exterior.

The Ce₂Li_0.39Ni_1.61Si₂ structure as a new derivative of the AlB₂ family

A quaternary inter­metallic dicerium lithium/nickel disilicide, Ce₂Li_0.39Ni_1.61Si₂, is compared with parent binary AlB₂ and RE–T–Si (RE = rare earth and T = transition metal) ternary phase compounds. The calculated electronic structure indicates metallic bonding is dominant within Ce₂Li_0.39Ni_1.61Si₂.

An ethanol-solvated centrosymmetric dimer of bis­muth(III) and thiosaccharinate resulting from `semicoordination' contacts

In an ethanol-solvated centrosymmetric dimer of bismuth(III) and thiosaccharinate, the Bi³⁺ cation is coordinated by three thio­saccharinate ligands, all of them acting as bidentate chelates through the N and exocyclic S atoms (in a κ²N,S mode). Centrosymmetric dimers result from the association of molecules via π–π interactions.

Formation of lithium, sodium and potassium complexes with 1,3,5-tri­amino-1,3,5-tri­deoxy-cis-inositol (taci)

The Li complex of 1,3,5-tri­amino-1,3,5-tri­deoxy-cis-inositol (taci) crystallizes as a dication, [Li(Htaci)(taci)]²⁺, whereas the Na and K complexes are simple bis-complexes, viz. [Na(taci)₂]⁺ and [K(taci)₂]⁺. All three complexes were isolated as iodide salts, with the additional inclusion of two water mol­ecules in the Li complex. Extended hydrogen bonding constitutes characteristic supra­molecular patterns in the solid state.