Acta Crystallographica Section E: Crystallographic Communications最新文献

Redetermination of the crystal structure of BiF₅ was undertaken to a much higher precision and quantum chemical calculations for an assignment of the Raman and IR bands.

The crystal structure of bis­muth penta­fluoride, BiF₅, was rerefined from single-crystal data. BiF₅ crystallizes in the α-UF₅ structure type in the form of colorless needles. In comparison with the previously reported crystal-structure model [Hebecker (1971#). Z. Anorg. Allg. Chem.384, 111–114], the lattice parameters and fractional atomic coordinates were determined to much higher precision and all atoms were refined anisotropically, leading to a significantly improved structure model. The Bi atom (site symmetry 4/m..) is surrounded by six F atoms in a distorted octa­hedral coordination environment. The [BiF₆] octa­hedra are corner-linked to form infinite straight chains extending parallel to [001]. Density functional theory (DFT) calculations at the PBE0/TZVP level of theory were performed on the crystal structure of BiF₅ to calculate its IR and Raman spectra. These are compared with experimental data.

The complex 2-[(4-phenyl-1H-1,2,3-triazol-1-yl)meth­yl]pyridin-1-ium hexa­kis­(nitrato-O,O′)thorate was synthesized from layered solutions of Th(NO₃)₄·5H₂O and 2-[(4-phenyl-1H-1,2,3-triazol-1-yl)meth­yl]pyridine (L).

Reaction of thorium(IV) nitrate with 2-[(4-phenyl-1H-1,2,3-triazol-1-yl)meth­yl]pyridine (L) yielded (LH)₂[Th(NO₃)₆] or (C₁₄H₁₃N₄)₂[Th(NO₃)₆] (1), instead of the expected mixed-ligand complex [Th(NO₃)₄L₂], which was detected in the mass spectrum of 1. In the structure, the [Th(NO₃)₆]²⁻ anions display an icosa­hedral coordination geometry and are connected by LH⁺ cations through C—H⋯O hydrogen bonds. The LH⁺ cations inter­act via N—H⋯N hydrogen bonds. Hirshfeld surface analysis indicates that the most important inter­actions are O⋯H/H⋯O hydrogen-bonding inter­actions, which represent a 55.2% contribution.

The Mo—Mo bond in the dinuclear mol­ecular title compound is 3.2323 (3) Å, in good agreement with related dinuclear molybdenum(I) compounds with cyclo­penta­dienyl (Cp) ligands.

The dinuclear mol­ecule of the title compound, [Mo₂(C₉H₁₃)₂(CO)₆] or [Mo(^tBuCp)(CO)₃]₂ where ^tBu and Cp are tert-butyl and cyclo­penta­dienyl, is centrosymmetric and is characterized by an Mo—Mo bond length of 3.2323 (3) Å. Imposed by inversion symmetry, the ^tBuCp and the carbonyl ligands are in a transoid arrangement to each other. In the crystal, inter­molecular C—H⋯O contacts lead to the formation of layers parallel to the bc plane.

Mol­ecules of the aryl diester, 2-methyl-1,4-phenyl­ene bis­(3,5-di­bromo­benzoate), crystallized out from the melt (m.p. = 502 K/DSC). The crystal structure consists of a C—H⋯Br hydrogen-bonded network and weaker, offset π–π inter­actions.

The aryl diester compound, 2-methyl-1,4-phenyl­ene bis­(3,5-di­bromo­benzoate), C₂₁H₁₂Br₄O₄, was synthesized by esterification of methyl hydro­quinone with 3,5-di­bromo­benzoic acid. A crystalline sample was obtained by cooling a sample of the melt (m.p. = 502 K/DSC) to room temperature. The mol­ecular structure consists of a central benzene ring with anti-3,5-di­bromo­benzoate groups symmetrically attached at the 1 and 4 positions and a methyl group attached at the 2 position of the central ring. In the crystal structure (space group P

The title mol­ecule is centrosymmetric, with a pyrazine ligand bridging two {Cu₁₀Ir₃} cluster units that are arranged in an unusual shape containing 13 vertices, 22 faces, and 32 sides.

Single crystals of the mol­ecular compound, {Cu₂₀Ir₆Cl₈(C₂₁H₂₄N₂)₆(C₄H₄N₂)₃]·3.18CH₃OH or [({Cu₁₀Ir₃}Cl₄(IMes)₃(pyrazine))₂(pyrazine)]·3.18CH₃OH [where IMes is 1,3-bis­(2,4,6-trimethylphen­yl)imidazol-2-yl­idene], with a unique heterometallic cluster have been prepared and the structure revealed using single-crystal X-ray diffraction. The mol­ecule is centrosymmetric with two {Cu₁₀Ir₃} cores bridged by a pyrazine ligand. The polymetallic cluster contains three stabilizing N-heterocyclic carbenes, four Cl ligands, and a non-bridging pyrazine ligand. Notably, the Cu—Ir core is arranged in an unusual shape containing 13 vertices, 22 faces, and 32 sides. The atoms within the trideca­metallic cluster are arranged in four planes, with 2, 4, 4, 3 metals in each plane. Ir atoms are present in alternate planes with an Ir atom featuring in the peripheral bimetallic plane, and two Ir atoms featuring on opposite sides of the non-adjacent tetra­metallic plane. The crystal contains two disordered methanol solvent mol­ecules with an additional region of non-modelled electron density corrected for using the SQUEEZE routine in PLATON [Spek (2015#). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unmodelled methanol solvent mol­ecule(s).

Two inter­mediates, 4-amino-3,5-di­fluoro­benzo­nitrile, C₇H₄F₂N₂ (I), and ethyl 4-amino-3,5-di­fluoro­benzoate, C₉H₉F₂NO₂ (II), along with a visible-light-responsive azo­benzene derivative, diethyl 4,4′-(diazene-1,2-di­yl)bis­(3,5-di­fluoro­benzoate), C₁₈H₁₄F₄N₂O₄ (III), obtained by four-step synthetic procedure, were studied using single-crystal X-ray diffraction. In the crystals of I and II, the mol­ecules are connected by N—H⋯N, N—H⋯F and N—H⋯O hydrogen bonds, C—H⋯F short contacts, and π-stacking inter­actions. In the crystal of III, only stacking inter­actions between the mol­ecules are found.

The crystal structures of two inter­mediates, 4-amino-3,5-di­fluoro­benzo­nitrile, C₇H₄F₂N₂ (I), and ethyl 4-amino-3,5-di­fluoro­benzoate, C₉H₉F₂NO₂ (II), along with a visible-light-responsive azo­benzene derivative, diethyl 4,4′-(diazene-1,2-di­yl)bis­(3,5-di­fluoro­benzoate), C₁₈H₁₄F₄N₂O₄ (III), obtained by four-step synthetic procedure, were studied using single-crystal X-ray diffraction. The mol­ecules of I and II demonstrate the quinoid character of phenyl rings accompanied by the distortion of bond angles related to the presence of fluorine substituents in the 3 and 5 (ortho) positions. In the crystals of I and II, the mol­ecules are connected by N—H⋯N, N—H⋯F and N—H⋯O hydrogen bonds, C—H⋯F short contacts, and π-stacking inter­actions. In crystal of III, only stacking inter­actions between the mol­ecules are found.

The title mol­ecule has a twisted conformation and is connected with its neighbours by C—H⋯O and C—H⋯N hydrogen bonds, π–π and Br–π inter­actions.

The title compound, C₁₇H₁₃BrN₄O₅, was synthesized by a Cu₂Br₂-catalysed Meldal–Sharpless reaction between 4-nitro­phen­oxy­acetic acid propargyl ether and para-bromo­phenyl­azide, and characterized by X-ray structure determination and ¹H NMR spectroscopy. The mol­ecules, with a near-perpendicular orientation of the bromo­phenyl-triazole and nitro­phen­oxy­acetate fragments, are connected into a three-dimensional network by inter­molecular C—H⋯O and C—H⋯N hydrogen bonds (confirmed by Hirshfeld surface analysis), π–π and Br–π inter­actions.

The crystal structures of two 1H-indole derivatives are described and the inter­molecular contacts in the crystals are assessed and analysed using Hirshfeld surface analysis and two-dimensional fingerprint plots.

Two new [1-(phenyl­sulfon­yl)-1H-indol-2-yl]methanamine derivatives, namely, N-(3-meth­oxy­phen­yl)-N-{[1-(phenyl­sulfon­yl)-1H-indol-2-yl]meth­yl}acetamide, C₂₄H₂₂N₂O₄S, (I), and N-(2,5-di­meth­oxy­phen­yl)-N-{[1-(phenyl­sulfon­yl)-1H-indol-2-yl]meth­yl}benzene­sulfonamide, C₂₉H₂₆N₂O₆S₂, (II), reveal a nearly orthogonal orientation of their indole ring systems and sulfonyl-bound phenyl rings. The sulfonyl moieties adopt the anti-periplanar conformation. For both compounds, the crystal packing is dominated by C—H⋯O bonding [C⋯O = 3.312 (4)–3.788 (8) Å], with the structure of II exhibiting a larger number, but weaker bonds of this type. Slipped π–π inter­actions of anti­parallel indole systems are specific for I, whereas the structure of II delivers two kinds of C—H⋯π inter­actions at both axial sides of the indole moiety. These findings agree with the results of Hirshfeld surface analysis. The primary contributions to the surface areas are associated with the contacts involving H atoms. Although II manifests a larger fraction of the O⋯H/H⋯O contacts (25.8 versus 22.4%), most of them are relatively distal and agree with the corresponding van der Waals separations.

The asymmetric unit of the title compound consists of two independent ion pairs of 4-(di­methyl­amino)­pyridin-1-ium quinolin-8-ol-5-sulfonate (HDMAP⁺·HqSA⁻) and neutral N,N-di­methyl­pyridin-4-amine (DMAP), forming a 1:1:1 cation:anion:neutral mol­ecule co-crystal. The compound has a layered structure, including cation layers of HDMAP⁺ with DMAP and anion layers of HqSA⁻ in the crystal. The cation and anion layers are linked by inter­molecular C—H⋯O hydrogen bonds and C—H⋯π inter­actions.

The asymmetric unit of the title compound is composed of two independent ion pairs of 4-(di­methyl­amino)­pyridin-1-ium 8-hy­droxy­quinoline-5-sulfonate (HDMAP⁺·HqSA⁻, C₇H₁₁N₂⁺·C₉H₆NO₄S⁻) and neutral N,N-di­methyl­pyridin-4-amine mol­ecules (DMAP, C₇H₁₀N₂), co-crystallized as a 1:1:1 HDMAP⁺:HqSA⁻:DMAP adduct in the monoclinic system, space group Pc. The compound has a layered structure, including cation layers of HDMAP⁺ with DMAP and anion layers of HqSA⁻ in the crystal. In the cation layer, there are inter­molecular N—H⋯N hydrogen bonds between the protonated HDMAP⁺ mol­ecule and the neutral DMAP mol­ecule. In the anion layer, each HqSA⁻ is surrounded by other six HqSA⁻, where the planar network structure is formed by inter­molecular O—H⋯O and C—H⋯O hydrogen bonds. The cation and anion layers are linked by inter­molecular C—H⋯O hydrogen bonds and C—H⋯π inter­actions.