Synthesis and absolute structure of (R)-2-(benzyl­selan­yl)-1-phenyl­ethanaminium hydrogen sulfate monohydrate: crystal structure and Hirshfeld surface analyses

A hydrogen sulfate salt, [BnSeCH₂CH(Ph)NH₃⁺](HSO₄⁻), of a chiral selenated amine (R)-2-(benzyl­selan­yl)-1-phenyl­ethanamine (BnSeCH₂CH(Ph)NH₂) has been synthesized and characterized by elemental analysis,¹H and ¹³C{¹H} NMR, FT–IR analysis, and single-crystal X-ray diffraction studies. This selenated salt crystallizes as a monohydrate. In the crystal, several O—H⋯O and N—H⋯O hydrogen bonds and C–H⋯π and Se⋯O weak inter­actions result in a complex two-dimensional sheet-like supra­molecular architecture.

Synthesis, crystal structure and Hirshfeld surface analysis of (4-methyl­phen­yl)[1-(penta­fluoro­phen­yl)-5-(tri­fluoro­meth­yl)-1H-1,2,3-triazol-4-yl]methanone

The title compound was obtained via the reaction of 1-azido-2,3,4,5,6-penta­fluoro­benzene with 4,4,4-tri­fluoro-1-(p-tol­yl)butane-1,3-dione using tri­ethyl­amine as a base catalyst and solvent. In the crystal, the mol­ecules are linked by C—H⋯F and C—H⋯O hydrogen bonds as well as by aromatic π–π stacking inter­actions into a three-dimensional network.

Crystal structure and Hirshfeld surface analysis of (3aSR,6RS,6aSR,7RS,11bSR,11cRS)-2,2-di­benzyl-2,3,6a,11c-tetra­hydro-1H,6H,7H-3a,6:7,11b-di­epoxy­dibenzo[de,h]isoquinolin-2-ium tri­fluoro­methane­sulfonate

In the crystal, dimeric C—H⋯O hydrogen bonds connect pairs of cations, producing two (6) ring motifs parallel to the (001) plane. Inter­molecular C—H⋯O hydrogen connections connect the cations and anions, producing a three-dimensional network.

Crystal structure of methyl 1,3-benzoxazole-2-carboxyl­ate

The herringbone structure of methyl 1,3-benzoxazole-2-carboxyl­ate is characterized by strong C—H⋯N and weak C—H⋯O hydrogen bonds, and further stabilized by C—O⋯π and π–π inter­actions.

Synthesis and crystal structure of di­aqua­bis­(hexa­methyl­enetramine-κN)bis­(thio­cyanato-κN)cobalt(II)–hexa­methyl­ene­tetra­mine–aceto­nitrile (1/2/2)

The crystal structure of the title compound consists of discrete neutral complexes in which the cobalt cations are octa­hedrally coordinated by two N-bonded thio­cyanate anions, two hexa­methyl­ene­tetra­amine ligands and two water mol­ecules with additional aceto­nitrile and hexa­methyl­ene­tetra­mine solvate mol­ecules, which are hydrogen bonded to the complexes.

Crystal structure and Hirshfeld surface analysis of (Z)-2-{[(2,4-di­methyl­phen­yl)imino]­meth­yl}-4-methyl­phenol

The title Schiff base exists in the enol–imine tautomeric form and adopts a Z configuration. In the crystal, the mol­ecules are linked by weak C—H⋯π hydrogen bonds and very weak π–π stacking inter­actions.

Crystal structure of 2-oxo-1,2-di­phenyl­ethyl diiso­propyl­carbamate

The title compound, C₂₁H₂₅NO₃, crystallizes as a racemic twin in the chiral space group P2₁. Both R- and S-enanti­omers are connected into infinite helical chains by weak C—H⋯O hydrogen bonds between the phenyl ring of the benzoyl group and the carbamate carbonyl group.

Crystal structures of two alanyl­piperidine analogues

The crystal structures of ethyl 1-[N-(4-methyl­phen­yl)-N-(methyl­sulfon­yl)alan­yl]piperidine-4-carboxyl­ate and 1-[N-(4-methyl­phen­yl)-N-(methyl­sulfon­yl)alan­yl]piperidine-4-carb­oxy­lic acid, two analogues studied as potentiators of Ubiquitin C-terminal hydro­lase-L1 (UCH-L1), have been determined. Despite being analogues, different crystal packings are observed. A polymorph risk assessment was carried out to study inter­actions in the second compound.

Formation of a macrocycle from di­chloro­dimethyl­silane and a pyridoxalimine Schiff base ligand

The reaction of di­chloro­dimethyl­silane with a polydentate Schiff base ligand derived from pyridoxal and 2-ethano­lamine yielded a macrocyclic silicon compound.

Hydrogen-bonding landscape of the carbamoyl­cyano­nitro­somethanide anion in the crystal structure of its ammonium salt

The structure of the title salt, ammonium carbamoyl­cyano­nitro­somethanide, NH₄⁺·C₃H₂N₃O₂⁻, features the co-existence of different hydrogen-bonding patterns, which are specific to each of the three functional groups (nitroso, carbamoyl and cyano) of the methanide anion. The relatively simple scheme of these inter­actions allows the delineation of the supra­molecular synthons, which may be applicable to crystal engineering of hydrogen-bonded solids containing polyfunctional methanide anions.

Isostructural rubidium and caesium 4-(3,5-di­nitro­pyrazol-4-yl)-3,5-di­nitro­pyrazolates: crystal engineering with polynitro energetic species

In the structures of the title salts, two independent cations (Rb, Cs) are situated on a crystallographic twofold axis and on a center of inversion, respectively. Mutual inter­molecular hydrogen bonding between the conjugate 3,5-dinito­pyrazole NH-donor and 3,5-di­nitro­pyrazolate N-acceptor sites of the anions governs the self-assembly of the translation-related anions in a predictable fashion. The anionic chains are further linked by multiple ion–dipole inter­actions involving the 12-coordinate cations bonded to two pyrazole N-atoms and all of the eight nitro O-atoms. The resulting ionic networks follow the CsCl topological archetype, with either metal or organic ions residing in an environment of eight counter-ions. Weak lone pair–π-hole inter­actions are also relevant to the packing.

Synthesis and crystal structure of a new chiral α-amino­oxime nickel(II) complex

The reaction of a nickel precursor with an enanti­omerically pure amino-oxime issued from (R)-limonene led to the formation of bis­[κ³N,N,N-(amino­oxime)-μ-chlorido]­dichloro­dinickel as a new dinuclear nickel complex.

Comparison of the crystal structures of the low- and high-temperature forms of bis­[4-(di­methyl­amino)­pyridine]­dithio­cyanato­cobalt(II)

The crystal structures of the low-temperature and the already published high-temperature forms of Co(NCS)₂(DMAP)₂ (DMAP = 4-di­methyl­amino­pyridine) were determined at 100 K, indicating that these two forms represent an exception from the Kitaigorodskii density rule.

Crystal structure and Hirshfeld surface analysis of bis­[(eth­oxy­methane­thio­yl)sulfanido](N,N,N′,N′-tetra­methyl­ethane-1,2-di­amine)­mercury(II)

In the crystal, mol­ecules are linked by weak C—H⋯S hydrogen bonds, forming a two-dimensional supra­molecular architecture.

Synthesis and crystal structure of a solvated Co^III complex with 2-hy­droxy-3-meth­oxy­benzaldehyde thio­semicarbazone ligands

The synthesis, crystal structure and spectroscopic characterization of the novel and, according to our knowledge the first to be obtained in crystalline form, Co^III complex with a multidentate NSO-containing mixed-ligand − 2-hy­droxy-3-meth­oxy­benzaldehyde thio­semicarbazone – is reported.

Crystal structure studies of 4-ethyl­piperazin-1-ium 3,5-di­nitro­benzoate, 4-methyl­piperazin-1-ium 3,5-di­nitro­benzoate and 4-methyl­piperazin-1-ium 4-iodo­benzoate

Three novel piperazinium salts are described. Their crystal structure is based on layers formed by hydrogen bonding, halogen bonding and other weak inter­actions. One exhibits an asymmetric unit containing a 1-ethyl­piperazinium cation and a 3,5-di­nitro­benzoate anion while the other two salts have asymmetric units containing 1-methyl­piperazinium as a common cation and a 3,5-di­nitro­benzoate anion or a 4-iodo­benzoate anion.

Crystal structure of [{[Ni(C₁₀H₂₄N₄)][Ni(CN)₄]}·2H₂O]_n, a one-dimensional coordination polymer formed from the [Ni(cyclam)]²⁺ cation and the [Ni(CN)₄]^2– anion

The title coordination polymer consists of parallel linear chains built up of macrocyclic cations possessing a slightly tetra­gonally distorted NiN₆ octa­hedral coordination geometry formed by four N atoms of the aza­macrocyclic ligand in the equatorial plane and two trans N atoms of the cyanide groups of the bridging tetra­cyano­nickelate anion in the axial positions. In the crystal, two independent [10] polymeric chains are cross-linked by N—H⋯O_w (w = water) and O_w—H⋯N_c (c = cyanide) hydrogen bonds into a three-dimensional network.

Role of pK_a in establishing the crystal structures of six hydrogen-bonded compounds of 4-methyl­quinoline with different isomers of chloro- and nitro-substituted benzoic acids

The structures of the six hydrogen-bonded 1:1 compounds of 4-methyl­quinoline with 2-chloro-4-nitro­benzoic acid, 2-chloro-5-nitro­benzoic acid, 2-chloro-6-nitro­benzoic acid, 3-chloro-2-nitro­benzoic acid, 4-chloro-2-nitro­benzoic acid and 5-chloro-2-nitro­benzoic acid have been determined at 185–190 K. In each crystal, the acid and base mol­ecules are linked by a short hydrogen bond between a carb­oxy/carboxyl­ate O atom and an N atom of the base.

Crystal structure and Hirshfeld surface analysis of di-μ-chlorido-bis­[(aceto­nitrile-κN)chlorido­(ethyl 5-methyl-1H-pyrazole-3-carboxyl­ate-κ²N²,O)copper(II)]

The title compound, [Cu₂Cl₄(C₅H₁₀N₂O₂)₂(CH₃CN)₂] or [Cu₂(μ₂-Cl)₂(CH₃—Pz-COOCH₂CH₃)₂Cl₂(CH₃CN)₂], was synthesized using an one-pot reaction of copper powder, copper(II) chloride dihydrate and ethyl 5-methyl-1H-pyrazole-3-carboxyl­ate (CH₃—Pz-COOCH₂CH₃) in aceto­nitrile under ambient conditions. This complex consists of discrete binuclear mol­ecules with a {Cu₂(μ₂-Cl)₂} core.

Crystal structure and Hirshfeld surface analysis of (E)-1-[2,2-di­chloro-1-(4-fluoro­phen­yl)ethen­yl]-2-(2,4-di­chloro­phen­yl)diazene

In the crystal, C—H⋯N, C—Cl⋯π inter­actions and face-to-face π–π stacking inter­actions connect the mol­ecules, forming ribbons along the a-axis direction.

Crystal structure, Hirshfeld surface analysis and DFT studies of tetra­kis­(μ-3-nitro­benzoato-κ²O¹:O^1′)bis­[(N,N-di­methyl­formamide-κO)copper(II)] di­methyl­formamide disolvate

The title compound, [Cu₂(C₇H₄NO₄)₄(C₃H₇NO)₂]·(C₃H₇NO)₂, is a binuclear copper(II) complex located on an inversion center midway between the two copper(II) cations. The asymmetric unit consists of one Cu^II cation, two 3-nitro­benzoato ligands, and two di­methyl­formamide (DMF) mol­ecules, one of which coordinates to the Cu^II cation and one is a solvate mol­ecule. The carboxyl­ate groups of the ligands bridge two Cu^II cations, completing a distorted octa­hedral O₅Cu coordination environment.

Crystal structure, Hirshfeld surface and frontier mol­ecular orbital analysis of 9-(3-bromo-4-hy­droxy-5-meth­oxy­phen­yl)-3,3,6,6-tetra­methyl-3,4,5,6,7,9-hexa­hydro-1H-xanthene-1,8(2H)-dione

In the xanthene moiety of the title compound, the central ring adopts a flattened-boat conformation whereas the cyclo­hexenone rings adopt envelope conformations. In the crystal, mol­ecules are linked by pairs of O—H⋯O hydrogen bonds, forming inversion dimers with an (20) ring motif.

Crystal structure of trans-di­aqua­(1,4,8,11-tetra­aza­undeca­ne)nickel(II) bis­(pyridine-2,6-di­carboxyl­ato)nickel(II)

The coordination polyhedra of the nickel(II) ions of the title compound in the complex cation and the anion, viz., trans-NiN₄O₂ and trans-NiO₄N₂, are distorted octa­hedra. In the crystal, the donor groups of the tetra­amine and the coordinated water mol­ecules and the carboxyl­ate groups of the pyridine-2,6-di­carboxyl­ate anions are involved in numerous N—H⋯O and O—H⋯O hydrogen bonds, thereby forming sheets of ions lying parallel to the (001) plane.

Syntheses and crystal structures of two copper(I)–halide π,σ-coordination compounds based on 2-[(prop-2-en-1-yl)sulfan­yl]pyridine

The title compounds, di-μ-chlorido-bis­({2-[(η-2,3)-(prop-2-en-1-yl)sulfan­yl]pyridine-κN}copper(I)) and di-μ-bromido-bis­({2-[(η-2,3)-(prop-2-en-1-yl)sulfan­yl]pyridine-κN}copper(I)) were obtained by alternating-current electrochemical synthesis starting from an ethano­lic solution of 2-[(prop-2-en-1-yl)sulfan­yl]pyridine (Psup) and the copper(II) halide. The isostructural crystals are built up from centrosymmetric [Cu₂Hal₂(Psup)₂] dimers, which are formed due to the π,σ-chelating behavior of the organic ligand.

Crystal structures of Zn(cyclam)I₂ (second monoclinic polymorph) and Zn(cyclam)I(I₃)

The crystal of the first title compound contains five-coordinate [Zn(L)I]⁺ (L = cyclam) cations and non-coordinated iodide anions; the extended structure is consolidated by N—H⋯I and N—H⋯(I,I) hydrogen bonds. The crystals of the second title compound consist of chains of [Zn(L)I]⁺ units and triiodide counter-ions but without significant hydrogen-bonding inter­actions.